# 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_imw1729p21c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H39 Co N9, 2(B F4), C H Cl3, O H2' _chemical_formula_sum 'C46 H42 B2 Cl3 Co F8 N9 O' _chemical_formula_weight 1075.79 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' O O 0.0106 0.0060 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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 12.2347(3) _cell_length_b 31.6797(9) _cell_length_c 13.5802(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.6540(10) _cell_angle_gamma 90.00 _cell_volume 4744.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9139 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.36 _exptl_crystal_description block _exptl_crystal_colour 'light orange' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2188 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7925 _exptl_absorpt_correction_T_max 0.8625 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 85055 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.61 _reflns_number_total 10912 _reflns_number_gt 7940 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. Both of the BF4 anions were located, although one of them was disordered. The oxygen atom of a water molecule was located, however the hydrogen atoms could not be located from the data. 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^)+(0.0516P)^2^+15.0672P] 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 10912 _refine_ls_number_parameters 619 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1655 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Co1 Co 0.19129(4) 0.117791(14) 0.84174(4) 0.01991(12) Uani 1 1 d . . . N11A N 0.1680(2) 0.17981(9) 0.8936(2) 0.0219(6) Uani 1 1 d . . . C12A C 0.1084(3) 0.20724(11) 0.8116(3) 0.0246(7) Uani 1 1 d . . . C13A C 0.1004(3) 0.24999(11) 0.8300(3) 0.0312(8) Uani 1 1 d . . . H13A H 0.0589 0.2686 0.7705 0.037 Uiso 1 1 calc R . . C14A C 0.1534(4) 0.26516(12) 0.9358(4) 0.0353(9) Uani 1 1 d . . . H14A H 0.1503 0.2944 0.9502 0.042 Uiso 1 1 calc R . . C15A C 0.2110(4) 0.23707(12) 1.0200(3) 0.0338(9) Uani 1 1 d . . . H15A H 0.2458 0.2465 1.0937 0.041 Uiso 1 1 calc R . . C16A C 0.2175(3) 0.19494(11) 0.9959(3) 0.0272(7) Uani 1 1 d . . . H16A H 0.2589 0.1759 1.0544 0.033 Uiso 1 1 calc R . . N21A N 0.0169(3) 0.14103(10) 0.5809(2) 0.0300(7) Uani 1 1 d . . . N22A N 0.0711(3) 0.14773(9) 0.6904(2) 0.0239(6) Uani 1 1 d . . . C23A C 0.0544(3) 0.18900(11) 0.7021(3) 0.0257(7) Uani 1 1 d . . . C24A C -0.0122(4) 0.20833(13) 0.6011(3) 0.0372(9) Uani 1 1 d . . . H24A H -0.0373 0.2370 0.5874 0.045 Uiso 1 1 calc R . . C25A C -0.0331(4) 0.17675(13) 0.5265(3) 0.0377(9) Uani 1 1 d . . . H25A H -0.0757 0.1795 0.4494 0.045 Uiso 1 1 calc R . . C26A C 0.0089(4) 0.09901(13) 0.5334(3) 0.0346(9) Uani 1 1 d . . . H26A H 0.0841 0.0832 0.5777 0.041 Uiso 1 1 calc R . . H26B H 0.0033 0.1020 0.4588 0.041 Uiso 1 1 calc R . . C31A C -0.0988(4) 0.07387(12) 0.5276(3) 0.0311(8) Uani 1 1 d . . . C32A C -0.2123(4) 0.09203(13) 0.4937(3) 0.0334(8) Uani 1 1 d . . . H32A H -0.2236 0.1211 0.4752 0.040 Uiso 1 1 calc R . . C33A C -0.3102(4) 0.06754(15) 0.4868(3) 0.0434(10) Uani 1 1 d . . . H33A H -0.3880 0.0800 0.4642 0.052 Uiso 1 1 calc R . . C34A C -0.2934(5) 0.02511(16) 0.5131(4) 0.0510(13) Uani 1 1 d . . . H34A H -0.3600 0.0083 0.5077 0.061 Uiso 1 1 calc R . . C35A C -0.1815(5) 0.00738(15) 0.5468(4) 0.0524(13) Uani 1 1 d . . . H35A H -0.1703 -0.0218 0.5651 0.063 Uiso 1 1 calc R . . C36A C -0.0844(4) 0.03155(14) 0.5543(3) 0.0432(10) Uani 1 1 d . . . H36A H -0.0067 0.0189 0.5782 0.052 Uiso 1 1 calc R . . N11B N 0.3444(2) 0.14366(9) 0.8209(2) 0.0208(6) Uani 1 1 d . . . C12B C 0.4498(3) 0.14551(10) 0.9130(3) 0.0226(7) Uani 1 1 d . . . C13B C 0.5541(3) 0.16369(11) 0.9150(3) 0.0295(8) Uani 1 1 d . . . H13B H 0.6269 0.1645 0.9807 0.035 Uiso 1 1 calc R . . C14B C 0.5501(3) 0.18058(12) 0.8196(3) 0.0327(8) Uani 1 1 d . . . H14B H 0.6200 0.1934 0.8190 0.039 Uiso 1 1 calc R . . C15B C 0.4437(3) 0.17850(11) 0.7258(3) 0.0292(8) Uani 1 1 d . . . H15B H 0.4393 0.1896 0.6592 0.035 Uiso 1 1 calc R . . C16B C 0.3425(3) 0.15991(11) 0.7295(3) 0.0268(7) Uani 1 1 d . . . H16B H 0.2692 0.1587 0.6643 0.032 Uiso 1 1 calc R . . N21B N 0.3706(3) 0.09273(9) 1.1020(2) 0.0264(6) Uani 1 1 d . . . N22B N 0.3459(3) 0.10661(9) 1.0004(2) 0.0220(6) Uani 1 1 d . . . C23B C 0.4475(3) 0.12620(10) 1.0105(3) 0.0232(7) Uani 1 1 d . . . C24B C 0.5371(4) 0.12467(13) 1.1175(3) 0.0357(9) Uani 1 1 d . . . H24B H 0.6165 0.1362 1.1456 0.043 Uiso 1 1 calc R . . C25B C 0.4847(4) 0.10277(13) 1.1733(3) 0.0366(9) Uani 1 1 d . . . H25B H 0.5223 0.0959 1.2489 0.044 Uiso 1 1 calc R . . C26B C 0.2869(3) 0.06648(11) 1.1257(3) 0.0276(8) Uani 1 1 d . . . H26C H 0.2059 0.0672 1.0627 0.033 Uiso 1 1 calc R . . H26D H 0.2788 0.0781 1.1900 0.033 Uiso 1 1 calc R . . C31B C 0.3303(3) 0.02130(11) 1.1485(3) 0.0241(7) Uani 1 1 d . . . C32B C 0.3479(3) -0.00252(12) 1.0702(3) 0.0285(8) Uani 1 1 d . . . H32B H 0.3349 0.0100 1.0025 0.034 Uiso 1 1 calc R . . C33B C 0.3843(3) -0.04432(13) 1.0904(3) 0.0337(8) Uani 1 1 d . . . H33B H 0.3948 -0.0605 1.0362 0.040 Uiso 1 1 calc R . . C34B C 0.4052(3) -0.06230(12) 1.1896(3) 0.0335(8) Uani 1 1 d . . . H34B H 0.4296 -0.0910 1.2034 0.040 Uiso 1 1 calc R . . C35B C 0.3908(3) -0.03888(12) 1.2683(3) 0.0323(8) Uani 1 1 d . . . H35B H 0.4070 -0.0513 1.3369 0.039 Uiso 1 1 calc R . . C36B C 0.3529(3) 0.00280(11) 1.2480(3) 0.0274(7) Uani 1 1 d . . . H36B H 0.3423 0.0187 1.3025 0.033 Uiso 1 1 calc R . . N11C N 0.2097(2) 0.05542(9) 0.7911(2) 0.0217(6) Uani 1 1 d . . . C12C C 0.1377(3) 0.02564(11) 0.8045(3) 0.0227(7) Uani 1 1 d . . . C13C C 0.1489(3) -0.01701(11) 0.7867(3) 0.0278(8) Uani 1 1 d . . . H13C H 0.0964 -0.0372 0.7955 0.033 Uiso 1 1 calc R . . C14C C 0.2379(3) -0.02946(12) 0.7558(3) 0.0303(8) Uani 1 1 d . . . H14C H 0.2479 -0.0585 0.7439 0.036 Uiso 1 1 calc R . . C15C C 0.3122(3) 0.00063(12) 0.7425(3) 0.0304(8) Uani 1 1 d . . . H15C H 0.3739 -0.0073 0.7215 0.037 Uiso 1 1 calc R . . C16C C 0.2948(3) 0.04276(11) 0.7603(3) 0.0262(7) Uani 1 1 d . . . H16C H 0.3453 0.0634 0.7502 0.031 Uiso 1 1 calc R . . N21C N -0.0266(3) 0.08735(9) 0.9101(2) 0.0248(6) Uani 1 1 d . . . N22C N 0.0566(2) 0.08271(9) 0.8699(2) 0.0219(6) Uani 1 1 d . . . C23C C 0.0517(3) 0.04148(11) 0.8436(3) 0.0229(7) Uani 1 1 d . . . C24C C -0.0354(3) 0.02033(12) 0.8647(3) 0.0304(8) Uani 1 1 d . . . H24C H -0.0572 -0.0086 0.8522 0.036 Uiso 1 1 calc R . . C25C C -0.0829(3) 0.05051(12) 0.9074(3) 0.0314(8) Uani 1 1 d . . . H25C H -0.1447 0.0462 0.9310 0.038 Uiso 1 1 calc R . . C26C C -0.0503(3) 0.12767(12) 0.9475(3) 0.0287(8) Uani 1 1 d . . . H26E H 0.0282 0.1409 0.9954 0.034 Uiso 1 1 calc R . . H26F H -0.0951 0.1227 0.9921 0.034 Uiso 1 1 calc R . . C31C C -0.1217(3) 0.15804(11) 0.8573(3) 0.0257(7) Uani 1 1 d . . . C32C C -0.1203(3) 0.20052(12) 0.8822(4) 0.0349(9) Uani 1 1 d . . . H32C H -0.0752 0.2098 0.9553 0.042 Uiso 1 1 calc R . . C33C C -0.1839(4) 0.22933(13) 0.8019(4) 0.0429(11) Uani 1 1 d . . . H33C H -0.1815 0.2584 0.8200 0.051 Uiso 1 1 calc R . . C34C C -0.2512(4) 0.21649(14) 0.6952(4) 0.0423(10) Uani 1 1 d . . . H34C H -0.2939 0.2366 0.6398 0.051 Uiso 1 1 calc R . . C35C C -0.2555(4) 0.17407(14) 0.6701(4) 0.0396(9) Uani 1 1 d . . . H35C H -0.3029 0.1649 0.5973 0.048 Uiso 1 1 calc R . . C36C C -0.1913(4) 0.14484(12) 0.7504(3) 0.0329(8) Uani 1 1 d . . . H36C H -0.1949 0.1157 0.7324 0.039 Uiso 1 1 calc R . . O1S O 0.0893(3) 0.08100(11) 0.2255(3) 0.0622(10) Uani 1 1 d . . . C1S C 0.4596(4) 0.30653(15) 0.8895(4) 0.0460(11) Uani 1 1 d . . . H1S H 0.4777 0.3304 0.9424 0.055 Uiso 1 1 calc R . . Cl1S Cl 0.44880(13) 0.26036(4) 0.95523(12) 0.0576(3) Uani 1 1 d . . . Cl2S Cl 0.32068(14) 0.31742(5) 0.77682(10) 0.0674(4) Uani 1 1 d . . . Cl3S Cl 0.57973(15) 0.30299(5) 0.85134(14) 0.0713(4) Uani 1 1 d . . . B11 B 0.3482(5) 0.10462(15) 0.4977(4) 0.0385(11) Uani 1 1 d . . . F11 F 0.3337(3) 0.07873(9) 0.5725(2) 0.0569(7) Uani 1 1 d . . . F12 F 0.4675(3) 0.11840(9) 0.5398(2) 0.0583(7) Uani 1 1 d . . . F13 F 0.3224(3) 0.08213(9) 0.4024(2) 0.0661(9) Uani 1 1 d . . . F14 F 0.2729(3) 0.13886(10) 0.4760(2) 0.0644(8) Uani 1 1 d . . . B1 B 0.8674(4) 0.15780(16) 0.1949(4) 0.0377(10) Uiso 1 1 d . . . F1 F 0.8271(2) 0.12116(8) 0.1335(2) 0.0469(6) Uiso 1 1 d . A . F2 F 0.7938(5) 0.16931(17) 0.2486(4) 0.0565(14) Uiso 0.629(8) 1 d P A 1 F3 F 0.9835(4) 0.15397(14) 0.2815(4) 0.0527(15) Uiso 0.629(8) 1 d P A 1 F4 F 0.8708(6) 0.19052(17) 0.1304(4) 0.0650(16) Uiso 0.629(8) 1 d P A 1 F2X F 0.9861(9) 0.1617(3) 0.2078(9) 0.079(3) Uiso 0.371(8) 1 d P A 2 F3X F 0.8061(9) 0.1908(3) 0.1279(7) 0.060(3) Uiso 0.371(8) 1 d P A 2 F4X F 0.8463(12) 0.1516(4) 0.2793(10) 0.092(4) Uiso 0.371(8) 1 d P A 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 Co1 0.0180(2) 0.0204(2) 0.0214(2) 0.00039(17) 0.00868(17) -0.00029(17) N11A 0.0218(14) 0.0192(14) 0.0251(14) 0.0008(11) 0.0105(12) 0.0002(11) C12A 0.0179(16) 0.0252(18) 0.0330(19) 0.0043(14) 0.0133(14) 0.0009(13) C13A 0.0280(19) 0.0231(18) 0.045(2) 0.0069(15) 0.0182(17) 0.0032(14) C14A 0.033(2) 0.0230(19) 0.054(3) -0.0045(17) 0.0222(19) -0.0015(15) C15A 0.035(2) 0.029(2) 0.037(2) -0.0084(16) 0.0144(17) -0.0020(16) C16A 0.0268(18) 0.0260(18) 0.0290(18) -0.0018(14) 0.0122(15) 0.0006(14) N21A 0.0277(16) 0.0399(18) 0.0212(15) 0.0036(13) 0.0094(13) -0.0018(13) N22A 0.0200(14) 0.0297(16) 0.0218(14) 0.0029(11) 0.0089(12) 0.0002(11) C23A 0.0220(17) 0.0270(18) 0.0291(18) 0.0065(14) 0.0120(15) -0.0001(13) C24A 0.038(2) 0.032(2) 0.037(2) 0.0124(17) 0.0122(18) -0.0019(17) C25A 0.039(2) 0.043(2) 0.0245(19) 0.0133(17) 0.0071(17) -0.0045(18) C26A 0.035(2) 0.046(2) 0.0236(18) -0.0055(16) 0.0132(16) 0.0002(17) C31A 0.038(2) 0.035(2) 0.0171(16) -0.0019(14) 0.0096(15) 0.0007(16) C32A 0.039(2) 0.032(2) 0.032(2) -0.0045(15) 0.0173(17) -0.0016(16) C33A 0.043(2) 0.056(3) 0.037(2) -0.015(2) 0.022(2) -0.011(2) C34A 0.070(3) 0.055(3) 0.033(2) -0.011(2) 0.027(2) -0.030(3) C35A 0.078(4) 0.032(2) 0.033(2) 0.0002(18) 0.011(2) -0.011(2) C36A 0.054(3) 0.038(2) 0.0232(19) -0.0028(16) 0.0035(18) 0.003(2) N11B 0.0196(14) 0.0194(14) 0.0246(14) 0.0001(11) 0.0107(12) -0.0013(10) C12B 0.0200(16) 0.0204(16) 0.0294(18) -0.0026(13) 0.0125(14) 0.0003(12) C13B 0.0243(18) 0.0246(18) 0.041(2) -0.0046(15) 0.0149(16) -0.0030(14) C14B 0.031(2) 0.0243(18) 0.053(2) -0.0004(16) 0.0276(19) -0.0036(15) C15B 0.037(2) 0.0213(17) 0.039(2) 0.0020(15) 0.0255(18) 0.0004(15) C16B 0.0293(19) 0.0282(18) 0.0258(17) 0.0015(14) 0.0147(15) 0.0006(14) N21B 0.0273(15) 0.0289(16) 0.0216(14) 0.0035(12) 0.0094(12) 0.0014(12) N22B 0.0224(14) 0.0212(14) 0.0225(14) 0.0022(11) 0.0098(12) 0.0024(11) C23B 0.0209(16) 0.0216(17) 0.0246(17) -0.0012(13) 0.0074(14) 0.0008(12) C24B 0.030(2) 0.036(2) 0.032(2) 0.0009(16) 0.0054(16) -0.0071(16) C25B 0.035(2) 0.041(2) 0.0240(18) 0.0013(16) 0.0039(16) -0.0029(17) C26B 0.0309(19) 0.0290(19) 0.0271(18) 0.0070(14) 0.0165(15) 0.0054(15) C31B 0.0213(17) 0.0258(18) 0.0253(17) 0.0016(13) 0.0101(14) 0.0022(13) C32B 0.0258(18) 0.035(2) 0.0235(17) 0.0006(14) 0.0095(15) 0.0021(15) C33B 0.030(2) 0.034(2) 0.037(2) -0.0063(16) 0.0156(17) 0.0031(16) C34B 0.032(2) 0.0227(18) 0.047(2) 0.0004(16) 0.0182(18) 0.0020(15) C35B 0.033(2) 0.031(2) 0.036(2) 0.0073(16) 0.0174(17) 0.0022(15) C36B 0.0305(19) 0.0286(19) 0.0255(18) 0.0017(14) 0.0143(15) 0.0004(15) N11C 0.0186(13) 0.0232(14) 0.0225(14) 0.0013(11) 0.0082(11) -0.0005(11) C12C 0.0204(16) 0.0252(17) 0.0192(16) 0.0004(13) 0.0055(13) -0.0010(13) C13C 0.0286(18) 0.0235(18) 0.0275(18) 0.0006(14) 0.0086(15) -0.0027(14) C14C 0.034(2) 0.0253(18) 0.0257(18) -0.0048(14) 0.0073(16) 0.0035(15) C15C 0.0317(19) 0.032(2) 0.0293(19) -0.0038(15) 0.0150(16) 0.0033(15) C16C 0.0248(18) 0.0281(18) 0.0271(18) 0.0000(14) 0.0125(15) 0.0021(14) N21C 0.0234(15) 0.0276(15) 0.0262(15) 0.0014(12) 0.0134(12) 0.0010(12) N22C 0.0179(13) 0.0262(15) 0.0237(14) 0.0005(11) 0.0109(11) -0.0029(11) C23C 0.0210(16) 0.0228(17) 0.0232(16) 0.0028(13) 0.0080(14) -0.0004(13) C24C 0.0256(18) 0.0259(18) 0.041(2) 0.0033(15) 0.0157(16) -0.0024(14) C25C 0.0268(19) 0.033(2) 0.038(2) 0.0062(16) 0.0177(17) -0.0023(15) C26C 0.0259(18) 0.034(2) 0.0289(18) -0.0065(15) 0.0146(15) -0.0023(14) C31C 0.0212(17) 0.0274(18) 0.0338(19) -0.0030(14) 0.0168(15) -0.0022(13) C32C 0.0252(19) 0.030(2) 0.050(2) -0.0124(17) 0.0169(18) -0.0055(15) C33C 0.032(2) 0.0207(19) 0.085(3) -0.002(2) 0.034(2) -0.0018(16) C34C 0.038(2) 0.036(2) 0.062(3) 0.018(2) 0.031(2) 0.0073(18) C35C 0.046(2) 0.040(2) 0.036(2) 0.0048(17) 0.0198(19) 0.0067(19) C36C 0.037(2) 0.0267(19) 0.036(2) 0.0009(15) 0.0160(17) 0.0011(15) O1S 0.056(2) 0.044(2) 0.098(3) -0.0103(19) 0.045(2) -0.0014(16) C1S 0.060(3) 0.041(2) 0.043(2) -0.0054(19) 0.027(2) -0.002(2) Cl1S 0.0650(8) 0.0464(7) 0.0763(9) 0.0094(6) 0.0443(7) 0.0089(6) Cl2S 0.0733(9) 0.0863(10) 0.0367(6) 0.0027(6) 0.0182(6) -0.0045(8) Cl3S 0.0790(10) 0.0723(9) 0.0865(10) -0.0064(8) 0.0584(9) -0.0099(8) B11 0.049(3) 0.030(2) 0.038(2) -0.0015(18) 0.021(2) 0.001(2) F11 0.075(2) 0.0485(16) 0.0479(16) 0.0058(12) 0.0279(15) -0.0144(14) F12 0.0517(17) 0.0574(18) 0.0665(19) 0.0069(14) 0.0263(15) -0.0072(14) F13 0.108(3) 0.0468(17) 0.0474(16) -0.0099(13) 0.0369(17) 0.0030(16) F14 0.074(2) 0.0655(19) 0.0481(16) 0.0036(14) 0.0218(15) 0.0345(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 Co1 N11C 2.136(3) . ? Co1 N11A 2.147(3) . ? Co1 N22C 2.154(3) . ? Co1 N22A 2.161(3) . ? Co1 N11B 2.173(3) . ? Co1 N22B 2.195(3) . ? N11A C16A 1.341(4) . ? N11A C12A 1.350(4) . ? C12A C13A 1.388(5) . ? C12A C23A 1.460(5) . ? C13A C14A 1.381(6) . ? C13A H13A 0.9500 . ? C14A C15A 1.378(6) . ? C14A H14A 0.9500 . ? C15A C16A 1.385(5) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? N21A C25A 1.345(5) . ? N21A N22A 1.357(4) . ? N21A C26A 1.464(5) . ? N22A C23A 1.343(5) . ? C23A C24A 1.398(5) . ? C24A C25A 1.367(6) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? C26A C31A 1.513(6) . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? C31A C36A 1.380(6) . ? C31A C32A 1.385(6) . ? C32A C33A 1.396(6) . ? C32A H32A 0.9500 . ? C33A C34A 1.383(7) . ? C33A H33A 0.9500 . ? C34A C35A 1.363(8) . ? C34A H34A 0.9500 . ? C35A C36A 1.379(7) . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? N11B C16B 1.335(4) . ? N11B C12B 1.354(4) . ? C12B C13B 1.389(5) . ? C12B C23B 1.471(5) . ? C13B C14B 1.382(6) . ? C13B H13B 0.9500 . ? C14B C15B 1.374(6) . ? C14B H14B 0.9500 . ? C15B C16B 1.391(5) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? N21B C25B 1.348(5) . ? N21B N22B 1.351(4) . ? N21B C26B 1.460(5) . ? N22B C23B 1.342(4) . ? C23B C24B 1.391(5) . ? C24B C25B 1.373(6) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? C26B C31B 1.511(5) . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? C31B C36B 1.387(5) . ? C31B C32B 1.395(5) . ? C32B C33B 1.386(5) . ? C32B H32B 0.9500 . ? C33B C34B 1.380(6) . ? C33B H33B 0.9500 . ? C34B C35B 1.374(6) . ? C34B H34B 0.9500 . ? C35B C36B 1.387(5) . ? C35B H35B 0.9500 . ? C36B H36B 0.9500 . ? N11C C16C 1.341(4) . ? N11C C12C 1.356(4) . ? C12C C13C 1.390(5) . ? C12C C23C 1.457(5) . ? C13C C14C 1.383(5) . ? C13C H13C 0.9500 . ? C14C C15C 1.382(5) . ? C14C H14C 0.9500 . ? C15C C16C 1.389(5) . ? C15C H15C 0.9500 . ? C16C H16C 0.9500 . ? N21C C25C 1.348(5) . ? N21C N22C 1.356(4) . ? N21C C26C 1.449(5) . ? N22C C23C 1.349(4) . ? C23C C24C 1.390(5) . ? C24C C25C 1.371(5) . ? C24C H24C 0.9500 . ? C25C H25C 0.9500 . ? C26C C31C 1.505(5) . ? C26C H26E 0.9900 . ? C26C H26F 0.9900 . ? C31C C32C 1.386(5) . ? C31C C36C 1.392(5) . ? C32C C33C 1.376(6) . ? C32C H32C 0.9500 . ? C33C C34C 1.382(7) . ? C33C H33C 0.9500 . ? C34C C35C 1.382(6) . ? C34C H34C 0.9500 . ? C35C C36C 1.386(5) . ? C35C H35C 0.9500 . ? C36C H36C 0.9500 . ? C1S Cl1S 1.748(5) . ? C1S Cl2S 1.760(5) . ? C1S Cl3S 1.761(5) . ? C1S H1S 1.0000 . ? B11 F14 1.370(6) . ? B11 F11 1.376(5) . ? B11 F12 1.387(6) . ? B11 F13 1.389(5) . ? B1 F4X 1.295(12) . ? B1 F4 1.369(7) . ? B1 F3X 1.375(10) . ? B1 F1 1.389(5) . ? B1 F2X 1.391(11) . ? B1 F3 1.404(7) . ? B1 F2 1.430(7) . ? 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 N11C Co1 N11A 178.17(11) . . ? N11C Co1 N22C 77.01(11) . . ? N11A Co1 N22C 101.16(11) . . ? N11C Co1 N22A 102.90(11) . . ? N11A Co1 N22A 77.16(11) . . ? N22C Co1 N22A 97.90(11) . . ? N11C Co1 N11B 95.17(10) . . ? N11A Co1 N11B 86.66(10) . . ? N22C Co1 N11B 170.58(11) . . ? N22A Co1 N11B 88.90(11) . . ? N11C Co1 N22B 90.03(10) . . ? N11A Co1 N22B 90.36(10) . . ? N22C Co1 N22B 98.20(11) . . ? N22A Co1 N22B 161.26(11) . . ? N11B Co1 N22B 76.32(10) . . ? C16A N11A C12A 117.7(3) . . ? C16A N11A Co1 127.0(2) . . ? C12A N11A Co1 114.8(2) . . ? N11A C12A C13A 122.3(3) . . ? N11A C12A C23A 115.4(3) . . ? C13A C12A C23A 122.2(3) . . ? C14A C13A C12A 119.2(4) . . ? C14A C13A H13A 120.4 . . ? C12A C13A H13A 120.4 . . ? C15A C14A C13A 118.7(4) . . ? C15A C14A H14A 120.7 . . ? C13A C14A H14A 120.7 . . ? C14A C15A C16A 119.2(4) . . ? C14A C15A H15A 120.4 . . ? C16A C15A H15A 120.4 . . ? N11A C16A C15A 122.9(3) . . ? N11A C16A H16A 118.6 . . ? C15A C16A H16A 118.6 . . ? C25A N21A N22A 111.1(3) . . ? C25A N21A C26A 126.5(3) . . ? N22A N21A C26A 122.2(3) . . ? C23A N22A N21A 104.8(3) . . ? C23A N22A Co1 113.0(2) . . ? N21A N22A Co1 141.4(2) . . ? N22A C23A C24A 111.3(3) . . ? N22A C23A C12A 118.8(3) . . ? C24A C23A C12A 129.9(3) . . ? C25A C24A C23A 104.4(4) . . ? C25A C24A H24A 127.8 . . ? C23A C24A H24A 127.8 . . ? N21A C25A C24A 108.3(3) . . ? N21A C25A H25A 125.8 . . ? C24A C25A H25A 125.8 . . ? N21A C26A C31A 113.1(3) . . ? N21A C26A H26A 109.0 . . ? C31A C26A H26A 109.0 . . ? N21A C26A H26B 109.0 . . ? C31A C26A H26B 109.0 . . ? H26A C26A H26B 107.8 . . ? C36A C31A C32A 119.1(4) . . ? C36A C31A C26A 119.2(4) . . ? C32A C31A C26A 121.6(4) . . ? C31A C32A C33A 119.9(4) . . ? C31A C32A H32A 120.0 . . ? C33A C32A H32A 120.0 . . ? C34A C33A C32A 119.7(4) . . ? C34A C33A H33A 120.1 . . ? C32A C33A H33A 120.1 . . ? C35A C34A C33A 120.2(4) . . ? C35A C34A H34A 119.9 . . ? C33A C34A H34A 119.9 . . ? C34A C35A C36A 120.2(4) . . ? C34A C35A H35A 119.9 . . ? C36A C35A H35A 119.9 . . ? C35A C36A C31A 120.8(5) . . ? C35A C36A H36A 119.6 . . ? C31A C36A H36A 119.6 . . ? C16B N11B C12B 117.9(3) . . ? C16B N11B Co1 126.7(2) . . ? C12B N11B Co1 115.2(2) . . ? N11B C12B C13B 122.4(3) . . ? N11B C12B C23B 115.6(3) . . ? C13B C12B C23B 122.1(3) . . ? C14B C13B C12B 118.9(4) . . ? C14B C13B H13B 120.6 . . ? C12B C13B H13B 120.6 . . ? C15B C14B C13B 119.0(3) . . ? C15B C14B H14B 120.5 . . ? C13B C14B H14B 120.5 . . ? C14B C15B C16B 119.2(3) . . ? C14B C15B H15B 120.4 . . ? C16B C15B H15B 120.4 . . ? N11B C16B C15B 122.7(3) . . ? N11B C16B H16B 118.7 . . ? C15B C16B H16B 118.7 . . ? C25B N21B N22B 111.2(3) . . ? C25B N21B C26B 125.7(3) . . ? N22B N21B C26B 122.9(3) . . ? C23B N22B N21B 104.9(3) . . ? C23B N22B Co1 113.1(2) . . ? N21B N22B Co1 140.5(2) . . ? N22B C23B C24B 111.5(3) . . ? N22B C23B C12B 118.6(3) . . ? C24B C23B C12B 129.9(3) . . ? C25B C24B C23B 104.4(3) . . ? C25B C24B H24B 127.8 . . ? C23B C24B H24B 127.8 . . ? N21B C25B C24B 107.9(3) . . ? N21B C25B H25B 126.0 . . ? C24B C25B H25B 126.0 . . ? N21B C26B C31B 111.5(3) . . ? N21B C26B H26C 109.3 . . ? C31B C26B H26C 109.3 . . ? N21B C26B H26D 109.3 . . ? C31B C26B H26D 109.3 . . ? H26C C26B H26D 108.0 . . ? C36B C31B C32B 118.9(3) . . ? C36B C31B C26B 120.2(3) . . ? C32B C31B C26B 120.9(3) . . ? C33B C32B C31B 120.6(3) . . ? C33B C32B H32B 119.7 . . ? C31B C32B H32B 119.7 . . ? C34B C33B C32B 119.7(4) . . ? C34B C33B H33B 120.2 . . ? C32B C33B H33B 120.2 . . ? C35B C34B C33B 120.3(4) . . ? C35B C34B H34B 119.9 . . ? C33B C34B H34B 119.8 . . ? C34B C35B C36B 120.3(4) . . ? C34B C35B H35B 119.9 . . ? C36B C35B H35B 119.9 . . ? C35B C36B C31B 120.3(3) . . ? C35B C36B H36B 119.9 . . ? C31B C36B H36B 119.9 . . ? C16C N11C C12C 118.1(3) . . ? C16C N11C Co1 125.6(2) . . ? C12C N11C Co1 115.8(2) . . ? N11C C12C C13C 122.3(3) . . ? N11C C12C C23C 115.0(3) . . ? C13C C12C C23C 122.6(3) . . ? C14C C13C C12C 118.7(3) . . ? C14C C13C H13C 120.7 . . ? C12C C13C H13C 120.7 . . ? C15C C14C C13C 119.5(3) . . ? C15C C14C H14C 120.3 . . ? C13C C14C H14C 120.3 . . ? C14C C15C C16C 118.8(3) . . ? C14C C15C H15C 120.6 . . ? C16C C15C H15C 120.6 . . ? N11C C16C C15C 122.7(3) . . ? N11C C16C H16C 118.7 . . ? C15C C16C H16C 118.7 . . ? C25C N21C N22C 111.1(3) . . ? C25C N21C C26C 126.6(3) . . ? N22C N21C C26C 122.4(3) . . ? C23C N22C N21C 104.9(3) . . ? C23C N22C Co1 113.7(2) . . ? N21C N22C Co1 141.4(2) . . ? N22C C23C C24C 111.2(3) . . ? N22C C23C C12C 118.3(3) . . ? C24C C23C C12C 130.4(3) . . ? C25C C24C C23C 104.7(3) . . ? C25C C24C H24C 127.6 . . ? C23C C24C H24C 127.6 . . ? N21C C25C C24C 108.1(3) . . ? N21C C25C H25C 126.0 . . ? C24C C25C H25C 126.0 . . ? N21C C26C C31C 114.3(3) . . ? N21C C26C H26E 108.7 . . ? C31C C26C H26E 108.7 . . ? N21C C26C H26F 108.7 . . ? C31C C26C H26F 108.7 . . ? H26E C26C H26F 107.6 . . ? C32C C31C C36C 118.9(4) . . ? C32C C31C C26C 118.7(3) . . ? C36C C31C C26C 122.3(3) . . ? C33C C32C C31C 120.5(4) . . ? C33C C32C H32C 119.7 . . ? C31C C32C H32C 119.7 . . ? C32C C33C C34C 120.8(4) . . ? C32C C33C H33C 119.6 . . ? C34C C33C H33C 119.6 . . ? C35C C34C C33C 119.1(4) . . ? C35C C34C H34C 120.4 . . ? C33C C34C H34C 120.4 . . ? C34C C35C C36C 120.5(4) . . ? C34C C35C H35C 119.7 . . ? C36C C35C H35C 119.7 . . ? C35C C36C C31C 120.1(4) . . ? C35C C36C H36C 119.9 . . ? C31C C36C H36C 119.9 . . ? Cl1S C1S Cl2S 110.5(3) . . ? Cl1S C1S Cl3S 110.7(3) . . ? Cl2S C1S Cl3S 111.8(3) . . ? Cl1S C1S H1S 107.9 . . ? Cl2S C1S H1S 107.9 . . ? Cl3S C1S H1S 107.9 . . ? F14 B11 F11 109.9(4) . . ? F14 B11 F12 109.2(4) . . ? F11 B11 F12 109.4(4) . . ? F14 B11 F13 110.2(4) . . ? F11 B11 F13 109.4(4) . . ? F12 B11 F13 108.6(4) . . ? F4X B1 F4 139.0(7) . . ? F4X B1 F3X 116.1(8) . . ? F4 B1 F3X 32.9(4) . . ? F4X B1 F1 104.4(6) . . ? F4 B1 F1 110.5(4) . . ? F3X B1 F1 106.7(5) . . ? F4X B1 F2X 120.0(8) . . ? F4 B1 F2X 72.2(5) . . ? F3X B1 F2X 104.9(7) . . ? F1 B1 F2X 103.3(5) . . ? F4X B1 F3 76.2(7) . . ? F4 B1 F3 107.5(5) . . ? F3X B1 F3 133.2(6) . . ? F1 B1 F3 113.5(4) . . ? F2X B1 F3 43.9(4) . . ? F4X B1 F2 34.5(6) . . ? F4 B1 F2 109.5(5) . . ? F3X B1 F2 81.9(5) . . ? F1 B1 F2 112.4(4) . . ? F2X B1 F2 140.1(6) . . ? F3 B1 F2 103.1(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11C Co1 N11A C16A 88(3) . . . . ? N22C Co1 N11A C16A 84.2(3) . . . . ? N22A Co1 N11A C16A 179.9(3) . . . . ? N11B Co1 N11A C16A -90.5(3) . . . . ? N22B Co1 N11A C16A -14.2(3) . . . . ? N11C Co1 N11A C12A -100(3) . . . . ? N22C Co1 N11A C12A -104.0(2) . . . . ? N22A Co1 N11A C12A -8.3(2) . . . . ? N11B Co1 N11A C12A 81.3(2) . . . . ? N22B Co1 N11A C12A 157.6(2) . . . . ? C16A N11A C12A C13A 1.9(5) . . . . ? Co1 N11A C12A C13A -170.7(3) . . . . ? C16A N11A C12A C23A -179.0(3) . . . . ? Co1 N11A C12A C23A 8.4(4) . . . . ? N11A C12A C13A C14A -1.0(5) . . . . ? C23A C12A C13A C14A 179.9(3) . . . . ? C12A C13A C14A C15A -1.1(6) . . . . ? C13A C14A C15A C16A 2.2(6) . . . . ? C12A N11A C16A C15A -0.7(5) . . . . ? Co1 N11A C16A C15A 170.8(3) . . . . ? C14A C15A C16A N11A -1.3(6) . . . . ? C25A N21A N22A C23A -0.8(4) . . . . ? C26A N21A N22A C23A -176.6(3) . . . . ? C25A N21A N22A Co1 -168.7(3) . . . . ? C26A N21A N22A Co1 15.4(5) . . . . ? N11C Co1 N22A C23A -175.0(2) . . . . ? N11A Co1 N22A C23A 6.9(2) . . . . ? N22C Co1 N22A C23A 106.6(2) . . . . ? N11B Co1 N22A C23A -80.0(2) . . . . ? N22B Co1 N22A C23A -42.4(5) . . . . ? N11C Co1 N22A N21A -7.7(4) . . . . ? N11A Co1 N22A N21A 174.2(4) . . . . ? N22C Co1 N22A N21A -86.1(4) . . . . ? N11B Co1 N22A N21A 87.4(4) . . . . ? N22B Co1 N22A N21A 124.9(4) . . . . ? N21A N22A C23A C24A 1.3(4) . . . . ? Co1 N22A C23A C24A 173.2(2) . . . . ? N21A N22A C23A C12A -176.7(3) . . . . ? Co1 N22A C23A C12A -4.8(4) . . . . ? N11A C12A C23A N22A -2.4(5) . . . . ? C13A C12A C23A N22A 176.8(3) . . . . ? N11A C12A C23A C24A -179.9(4) . . . . ? C13A C12A C23A C24A -0.8(6) . . . . ? N22A C23A C24A C25A -1.3(4) . . . . ? C12A C23A C24A C25A 176.4(4) . . . . ? N22A N21A C25A C24A 0.0(5) . . . . ? C26A N21A C25A C24A 175.6(4) . . . . ? C23A C24A C25A N21A 0.8(5) . . . . ? C25A N21A C26A C31A -90.2(5) . . . . ? N22A N21A C26A C31A 85.0(4) . . . . ? N21A C26A C31A C36A -138.3(4) . . . . ? N21A C26A C31A C32A 43.2(5) . . . . ? C36A C31A C32A C33A -0.1(6) . . . . ? C26A C31A C32A C33A 178.4(3) . . . . ? C31A C32A C33A C34A -0.5(6) . . . . ? C32A C33A C34A C35A 0.7(6) . . . . ? C33A C34A C35A C36A -0.3(7) . . . . ? C34A C35A C36A C31A -0.3(7) . . . . ? C32A C31A C36A C35A 0.5(6) . . . . ? C26A C31A C36A C35A -178.0(4) . . . . ? N11C Co1 N11B C16B 87.5(3) . . . . ? N11A Co1 N11B C16B -92.5(3) . . . . ? N22C Co1 N11B C16B 121.0(6) . . . . ? N22A Co1 N11B C16B -15.3(3) . . . . ? N22B Co1 N11B C16B 176.3(3) . . . . ? N11C Co1 N11B C12B -96.9(2) . . . . ? N11A Co1 N11B C12B 83.1(2) . . . . ? N22C Co1 N11B C12B -63.4(7) . . . . ? N22A Co1 N11B C12B 160.3(2) . . . . ? N22B Co1 N11B C12B -8.1(2) . . . . ? C16B N11B C12B C13B 0.3(5) . . . . ? Co1 N11B C12B C13B -175.8(3) . . . . ? C16B N11B C12B C23B -178.5(3) . . . . ? Co1 N11B C12B C23B 5.5(4) . . . . ? N11B C12B C13B C14B 0.1(5) . . . . ? C23B C12B C13B C14B 178.9(3) . . . . ? C12B C13B C14B C15B -0.6(5) . . . . ? C13B C14B C15B C16B 0.7(5) . . . . ? C12B N11B C16B C15B -0.2(5) . . . . ? Co1 N11B C16B C15B 175.3(3) . . . . ? C14B C15B C16B N11B -0.3(5) . . . . ? C25B N21B N22B C23B -0.8(4) . . . . ? C26B N21B N22B C23B -174.8(3) . . . . ? C25B N21B N22B Co1 -164.9(3) . . . . ? C26B N21B N22B Co1 21.1(5) . . . . ? N11C Co1 N22B C23B 105.0(2) . . . . ? N11A Co1 N22B C23B -76.8(2) . . . . ? N22C Co1 N22B C23B -178.1(2) . . . . ? N22A Co1 N22B C23B -29.1(5) . . . . ? N11B Co1 N22B C23B 9.7(2) . . . . ? N11C Co1 N22B N21B -91.7(4) . . . . ? N11A Co1 N22B N21B 86.5(4) . . . . ? N22C Co1 N22B N21B -14.8(4) . . . . ? N22A Co1 N22B N21B 134.2(4) . . . . ? N11B Co1 N22B N21B 173.0(4) . . . . ? N21B N22B C23B C24B 0.4(4) . . . . ? Co1 N22B C23B C24B 169.5(3) . . . . ? N21B N22B C23B C12B -179.4(3) . . . . ? Co1 N22B C23B C12B -10.4(4) . . . . ? N11B C12B C23B N22B 3.5(5) . . . . ? C13B C12B C23B N22B -175.3(3) . . . . ? N11B C12B C23B C24B -176.3(4) . . . . ? C13B C12B C23B C24B 4.9(6) . . . . ? N22B C23B C24B C25B 0.1(4) . . . . ? C12B C23B C24B C25B 180.0(4) . . . . ? N22B N21B C25B C24B 0.9(5) . . . . ? C26B N21B C25B C24B 174.7(3) . . . . ? C23B C24B C25B N21B -0.6(5) . . . . ? C25B N21B C26B C31B -66.6(5) . . . . ? N22B N21B C26B C31B 106.5(4) . . . . ? N21B C26B C31B C36B 120.6(4) . . . . ? N21B C26B C31B C32B -59.7(4) . . . . ? C36B C31B C32B C33B 1.7(5) . . . . ? C26B C31B C32B C33B -178.1(3) . . . . ? C31B C32B C33B C34B -1.1(6) . . . . ? C32B C33B C34B C35B -0.4(6) . . . . ? C33B C34B C35B C36B 1.3(6) . . . . ? C34B C35B C36B C31B -0.7(6) . . . . ? C32B C31B C36B C35B -0.8(5) . . . . ? C26B C31B C36B C35B 178.9(3) . . . . ? N11A Co1 N11C C16C -178(100) . . . . ? N22C Co1 N11C C16C -174.3(3) . . . . ? N22A Co1 N11C C16C 90.4(3) . . . . ? N11B Co1 N11C C16C 0.3(3) . . . . ? N22B Co1 N11C C16C -75.9(3) . . . . ? N11A Co1 N11C C12C -6(4) . . . . ? N22C Co1 N11C C12C -2.7(2) . . . . ? N22A Co1 N11C C12C -98.0(2) . . . . ? N11B Co1 N11C C12C 172.0(2) . . . . ? N22B Co1 N11C C12C 95.7(2) . . . . ? C16C N11C C12C C13C -0.5(5) . . . . ? Co1 N11C C12C C13C -172.8(3) . . . . ? C16C N11C C12C C23C 176.9(3) . . . . ? Co1 N11C C12C C23C 4.7(4) . . . . ? N11C C12C C13C C14C 1.1(5) . . . . ? C23C C12C C13C C14C -176.2(3) . . . . ? C12C C13C C14C C15C -0.7(5) . . . . ? C13C C14C C15C C16C -0.2(5) . . . . ? C12C N11C C16C C15C -0.4(5) . . . . ? Co1 N11C C16C C15C 171.0(3) . . . . ? C14C C15C C16C N11C 0.8(5) . . . . ? C25C N21C N22C C23C -0.9(4) . . . . ? C26C N21C N22C C23C -179.5(3) . . . . ? C25C N21C N22C Co1 -178.0(3) . . . . ? C26C N21C N22C Co1 3.4(5) . . . . ? N11C Co1 N22C C23C 0.2(2) . . . . ? N11A Co1 N22C C23C -179.9(2) . . . . ? N22A Co1 N22C C23C 101.7(2) . . . . ? N11B Co1 N22C C23C -34.2(8) . . . . ? N22B Co1 N22C C23C -87.9(2) . . . . ? N11C Co1 N22C N21C 177.1(4) . . . . ? N11A Co1 N22C N21C -3.0(4) . . . . ? N22A Co1 N22C N21C -81.4(4) . . . . ? N11B Co1 N22C N21C 142.7(6) . . . . ? N22B Co1 N22C N21C 89.0(4) . . . . ? N21C N22C C23C C24C 1.2(4) . . . . ? Co1 N22C C23C C24C 179.2(2) . . . . ? N21C N22C C23C C12C -175.8(3) . . . . ? Co1 N22C C23C C12C 2.2(4) . . . . ? N11C C12C C23C N22C -4.6(4) . . . . ? C13C C12C C23C N22C 172.8(3) . . . . ? N11C C12C C23C C24C 179.1(3) . . . . ? C13C C12C C23C C24C -3.5(6) . . . . ? N22C C23C C24C C25C -1.0(4) . . . . ? C12C C23C C24C C25C 175.5(3) . . . . ? N22C N21C C25C C24C 0.3(4) . . . . ? C26C N21C C25C C24C 178.9(3) . . . . ? C23C C24C C25C N21C 0.4(4) . . . . ? C25C N21C C26C C31C -104.0(4) . . . . ? N22C N21C C26C C31C 74.5(4) . . . . ? N21C C26C C31C C32C -162.0(3) . . . . ? N21C C26C C31C C36C 19.5(5) . . . . ? C36C C31C C32C C33C -1.9(6) . . . . ? C26C C31C C32C C33C 179.6(3) . . . . ? C31C C32C C33C C34C 0.6(6) . . . . ? C32C C33C C34C C35C 1.0(6) . . . . ? C33C C34C C35C C36C -1.3(6) . . . . ? C34C C35C C36C C31C 0.0(6) . . . . ? C32C C31C C36C C35C 1.6(6) . . . . ? C26C C31C C36C C35C -180.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.388 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.090 _database_code_depnum_ccdc_archive 'CCDC 959996' ####################################################################### # # 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_1547p-1bak _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H21 N9 Ru, 2(F6 P), 2(C2 H3 N)' _chemical_formula_sum 'C28 H27 F12 N11 P2 Ru' _chemical_formula_weight 908.62 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' 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/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 14.3036(9) _cell_length_b 13.2235(8) _cell_length_c 23.5081(16) _cell_angle_alpha 90.00 _cell_angle_beta 121.776(4) _cell_angle_gamma 90.00 _cell_volume 3779.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1852 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 20.38 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7965 _exptl_absorpt_correction_T_max 0.8653 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20044 _diffrn_reflns_av_R_equivalents 0.0944 _diffrn_reflns_av_sigmaI/netI 0.0963 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 23.26 _reflns_number_total 5413 _reflns_number_gt 3162 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _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. Solved by direct methods. Global restraints were applied to the carbon and nitrogen atoms to bring the thermal parameters in line. One complex cation, two acetonitrile molecules and two PF6 anions occupy the asymmetric unit, with one full PF6 molecule and two at half occupancy. The space group was changed from P1 to P1/2c in platon. ; _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^)+(0.1733P)^2^+8.1971P] 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 5413 _refine_ls_number_parameters 491 _refine_ls_number_restraints 327 _refine_ls_R_factor_all 0.1437 _refine_ls_R_factor_gt 0.0858 _refine_ls_wR_factor_ref 0.2955 _refine_ls_wR_factor_gt 0.2479 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.029 _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 0.32966(7) 0.48576(6) 0.16787(4) 0.0496(4) Uani 1 1 d . . . N11A N 0.3511(8) 0.3517(7) 0.1316(5) 0.056(2) Uani 1 1 d U . . N21A N 0.1559(9) 0.3959(8) 0.1977(5) 0.066(3) Uani 1 1 d U . . H21A H 0.1462 0.4505 0.2138 0.080 Uiso 1 1 d R . . N22A N 0.2241(8) 0.3891(6) 0.1759(4) 0.048(2) Uani 1 1 d U . . N31A N 0.2832(7) 0.6162(6) 0.1966(4) 0.050(2) Uani 1 1 d U . . N41A N 0.1481(8) 0.5110(7) 0.0143(5) 0.067(3) Uani 1 1 d U . . H41A H 0.1639 0.4572 0.0007 0.080 Uiso 1 1 d R . . N42A N 0.2008(7) 0.5409(7) 0.0789(4) 0.050(2) Uani 1 1 d U . . N51A N 0.4648(9) 0.4499(7) 0.2587(5) 0.071(3) Uani 1 1 d U . . N61A N 0.4578(10) 0.6178(8) 0.1210(6) 0.080(3) Uani 1 1 d U . . H61A H 0.4002 0.6368 0.0843 0.096 Uiso 1 1 d R . . N62A N 0.4543(8) 0.5596(8) 0.1665(6) 0.065(3) Uani 1 1 d U . . C12A C 0.2859(10) 0.2727(8) 0.1283(6) 0.060(3) Uani 1 1 d U . . C13A C 0.2934(11) 0.1762(10) 0.1046(6) 0.072(3) Uani 1 1 d U . . H13A H 0.2510 0.1208 0.1045 0.086 Uiso 1 1 calc R . . C14A C 0.3612(12) 0.1657(11) 0.0828(7) 0.077(4) Uani 1 1 d U . . H14A H 0.3636 0.1028 0.0641 0.093 Uiso 1 1 calc R . . C15A C 0.4227(10) 0.2364(9) 0.0860(6) 0.059(3) Uani 1 1 d U . . H15A H 0.4715 0.2257 0.0707 0.071 Uiso 1 1 calc R . . C16A C 0.4197(10) 0.3312(9) 0.1121(6) 0.058(3) Uani 1 1 d U . . H16A H 0.4692 0.3823 0.1157 0.070 Uiso 1 1 calc R . . C23A C 0.2155(10) 0.2946(9) 0.1526(6) 0.061(3) Uani 1 1 d U . . C24A C 0.1325(11) 0.2354(10) 0.1606(6) 0.075(4) Uani 1 1 d U . . H24A H 0.1077 0.1677 0.1482 0.090 Uiso 1 1 calc R . . C25A C 0.1024(11) 0.3086(10) 0.1915(6) 0.068(3) Uani 1 1 d U . . H25A H 0.0521 0.2982 0.2058 0.082 Uiso 1 1 calc R . . C32A C 0.1983(8) 0.6688(7) 0.1467(5) 0.046(3) Uani 1 1 d U . . C33A C 0.1544(9) 0.7545(8) 0.1591(6) 0.053(3) Uani 1 1 d U . . H33A H 0.0931 0.7888 0.1235 0.063 Uiso 1 1 calc R . . C34A C 0.2014(9) 0.7873(9) 0.2232(6) 0.056(3) Uani 1 1 d U . . H34A H 0.1748 0.8464 0.2331 0.067 Uiso 1 1 calc R . . C35A C 0.2888(10) 0.7334(9) 0.2739(6) 0.061(3) Uani 1 1 d U . . H35A H 0.3216 0.7554 0.3190 0.073 Uiso 1 1 calc R . . C36A C 0.3277(9) 0.6505(8) 0.2603(6) 0.051(3) Uani 1 1 d U . . H36A H 0.3877 0.6149 0.2960 0.061 Uiso 1 1 calc R . . C43A C 0.1545(8) 0.6253(8) 0.0808(5) 0.047(3) Uani 1 1 d U . . C44A C 0.0691(10) 0.6514(9) 0.0154(6) 0.066(3) Uani 1 1 d U . . H44A H 0.0215 0.7082 0.0026 0.079 Uiso 1 1 calc R . . C45A C 0.0692(11) 0.5762(9) -0.0264(6) 0.077(4) Uani 1 1 d U . . H45A H 0.0231 0.5722 -0.0737 0.092 Uiso 1 1 calc R . . C52A C 0.5636(11) 0.4775(10) 0.2677(7) 0.078(3) Uani 1 1 d U . . C53A C 0.6664(13) 0.4511(12) 0.3233(8) 0.103(5) Uani 1 1 d U . . H53A H 0.7341 0.4695 0.3276 0.124 Uiso 1 1 calc R . . C54A C 0.6607(15) 0.3970(13) 0.3702(9) 0.108(5) Uani 1 1 d U . . H54A H 0.7278 0.3744 0.4080 0.130 Uiso 1 1 calc R . . C55A C 0.5664(13) 0.3731(10) 0.3668(7) 0.089(5) Uani 1 1 d U . . H55A H 0.5681 0.3395 0.4031 0.106 Uiso 1 1 calc R . . C56A C 0.4680(11) 0.3976(9) 0.3105(6) 0.078(4) Uani 1 1 d U . . H56A H 0.4012 0.3783 0.3071 0.094 Uiso 1 1 calc R . . C63A C 0.5564(10) 0.5383(10) 0.2175(8) 0.071(3) Uani 1 1 d U . . C64A C 0.6329(12) 0.5917(12) 0.1997(8) 0.094(4) Uani 1 1 d U . . H64A H 0.7110 0.5912 0.2235 0.112 Uiso 1 1 calc R . . C65A C 0.5574(14) 0.6423(12) 0.1384(9) 0.092(4) Uani 1 1 d U . . H65A H 0.5769 0.6864 0.1144 0.110 Uiso 1 1 calc R . . P11 P 0.0375(3) 0.0516(3) 0.27264(18) 0.0673(10) Uani 1 1 d . . . F12 F -0.0856(7) 0.0120(6) 0.2273(4) 0.092(3) Uani 1 1 d . . . F13 F 0.0804(11) -0.0607(8) 0.2934(6) 0.138(4) Uani 1 1 d . . . F14 F 0.1572(8) 0.0974(10) 0.3185(5) 0.128(4) Uani 1 1 d . . . F15 F 0.0206(7) 0.0549(6) 0.3346(4) 0.080(2) Uani 1 1 d . . . F16 F -0.0031(8) 0.1653(6) 0.2549(5) 0.102(3) Uani 1 1 d . . . F17 F 0.0536(10) 0.0496(8) 0.2106(5) 0.125(4) Uani 1 1 d . . . P31 P 0.5000 0.5000 0.5000 0.093(2) Uani 1 2 d S . . F32 F 0.4429(8) 0.5407(8) 0.4265(5) 0.115(3) Uani 1 1 d . . . F33 F 0.6130(9) 0.4926(8) 0.5030(7) 0.133(4) Uani 1 1 d . . . F34 F 0.4736(11) 0.3866(8) 0.4765(6) 0.138(4) Uani 1 1 d . . . P21 P 0.0000 0.5000 0.5000 0.0479(11) Uani 1 2 d S . . F22 F 0.1015(9) 0.5292(12) 0.4960(5) 0.171(6) Uani 1 1 d . . . F23 F -0.0725(6) 0.5009(5) 0.4201(3) 0.073(2) Uani 1 1 d . . . F24 F 0.0243(11) 0.3874(7) 0.4969(4) 0.149(5) Uani 1 1 d . . . N13S N 0.7113(14) 0.2852(11) 0.0024(8) 0.131(6) Uani 1 1 d U . . C11S C 0.8088(14) 0.1584(16) 0.0946(8) 0.120(6) Uani 1 1 d U . . H11A H 0.8361 0.1095 0.0798 0.144 Uiso 1 1 d R . . H11B H 0.8631 0.1921 0.1350 0.144 Uiso 1 1 d R . . H11C H 0.7634 0.1278 0.1058 0.144 Uiso 1 1 d R . . C12S C 0.7532(15) 0.2288(14) 0.0463(8) 0.100(5) Uani 1 1 d U . . N43S N 0.1607(10) 0.1861(9) 0.4630(5) 0.081(4) Uani 1 1 d U . . C41S C 0.1389(13) 0.3423(11) 0.3911(7) 0.083(4) Uani 1 1 d U . . H41E H 0.1316 0.4029 0.4125 0.124 Uiso 1 1 calc R . . H41F H 0.0720 0.3334 0.3470 0.124 Uiso 1 1 calc R . . H41G H 0.2023 0.3499 0.3861 0.124 Uiso 1 1 calc R . . C42S C 0.1548(13) 0.2546(11) 0.4323(7) 0.081(4) Uani 1 1 d U . . 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 0.0362(6) 0.0281(5) 0.0465(6) -0.0102(4) -0.0043(4) 0.0037(4) N11A 0.037(5) 0.042(5) 0.055(5) -0.001(4) 0.001(4) 0.011(4) N21A 0.072(6) 0.052(5) 0.053(6) -0.003(4) 0.018(5) 0.000(5) N22A 0.048(5) 0.036(4) 0.041(5) -0.001(4) 0.009(4) -0.007(4) N31A 0.033(4) 0.031(4) 0.051(5) -0.011(4) -0.002(4) -0.010(4) N41A 0.060(6) 0.043(5) 0.054(5) -0.013(4) 0.000(5) 0.006(4) N42A 0.040(5) 0.035(5) 0.045(5) -0.012(4) 0.002(4) 0.001(4) N51A 0.055(5) 0.039(5) 0.062(6) -0.020(4) -0.009(5) 0.012(4) N61A 0.068(6) 0.061(7) 0.091(7) -0.024(5) 0.028(6) -0.010(5) N62A 0.042(5) 0.047(6) 0.083(7) -0.024(5) 0.017(5) 0.001(4) C12A 0.054(6) 0.032(5) 0.045(6) 0.002(4) -0.009(4) 0.003(4) C13A 0.062(7) 0.047(6) 0.055(7) -0.001(5) -0.004(5) 0.007(5) C14A 0.061(8) 0.066(7) 0.066(7) -0.012(6) 0.006(6) 0.013(6) C15A 0.056(7) 0.046(6) 0.052(6) -0.007(5) 0.011(5) 0.016(5) C16A 0.037(6) 0.046(6) 0.052(6) -0.001(5) -0.003(5) 0.000(5) C23A 0.051(6) 0.043(5) 0.043(5) -0.004(4) -0.008(4) 0.003(5) C24A 0.070(7) 0.044(6) 0.057(7) 0.003(5) -0.004(5) -0.007(5) C25A 0.062(7) 0.070(7) 0.061(7) 0.004(6) 0.024(5) -0.007(6) C32A 0.033(5) 0.028(5) 0.052(5) -0.005(4) 0.005(4) -0.004(4) C33A 0.043(6) 0.037(6) 0.062(6) -0.004(5) 0.018(5) 0.000(4) C34A 0.043(6) 0.044(6) 0.069(6) -0.015(5) 0.022(5) -0.002(5) C35A 0.055(6) 0.044(6) 0.061(6) -0.013(5) 0.016(5) -0.010(5) C36A 0.041(5) 0.034(5) 0.054(6) -0.013(5) 0.008(5) -0.014(4) C43A 0.036(5) 0.034(5) 0.050(5) -0.004(4) 0.009(4) 0.004(4) C44A 0.050(6) 0.047(6) 0.060(6) 0.001(5) 0.002(5) 0.018(5) C45A 0.065(7) 0.055(7) 0.055(6) 0.002(5) -0.007(6) 0.019(5) C52A 0.045(5) 0.056(6) 0.078(7) -0.030(5) -0.006(5) 0.022(5) C53A 0.073(7) 0.073(8) 0.090(8) -0.032(6) -0.007(7) 0.028(7) C54A 0.088(8) 0.077(9) 0.081(8) -0.028(6) -0.009(8) 0.024(7) C55A 0.082(8) 0.046(7) 0.058(7) -0.008(5) -0.019(6) 0.015(6) C56A 0.070(7) 0.044(6) 0.055(6) -0.011(5) -0.012(5) 0.008(6) C63A 0.040(5) 0.061(6) 0.092(7) -0.040(5) 0.021(5) 0.008(5) C64A 0.050(7) 0.100(8) 0.116(9) -0.055(7) 0.033(6) -0.005(6) C65A 0.084(8) 0.091(8) 0.107(8) -0.034(7) 0.054(7) -0.026(7) P11 0.078(3) 0.068(2) 0.058(2) -0.0069(17) 0.037(2) -0.0089(19) F12 0.091(6) 0.090(6) 0.064(5) 0.002(4) 0.020(4) -0.038(5) F13 0.197(12) 0.100(8) 0.183(11) 0.044(8) 0.145(10) 0.058(8) F14 0.082(6) 0.202(12) 0.101(7) -0.016(7) 0.049(6) -0.048(7) F15 0.093(6) 0.090(6) 0.059(5) -0.021(4) 0.040(4) -0.034(5) F16 0.135(8) 0.069(6) 0.124(7) -0.005(5) 0.084(7) -0.025(5) F17 0.215(12) 0.105(7) 0.115(8) -0.019(6) 0.129(9) -0.031(7) P31 0.092(5) 0.083(5) 0.124(6) 0.043(4) 0.071(4) 0.021(3) F32 0.100(7) 0.122(8) 0.126(8) 0.052(7) 0.062(7) 0.013(6) F33 0.113(8) 0.155(10) 0.171(11) 0.058(8) 0.103(9) 0.030(7) F34 0.215(13) 0.089(8) 0.154(10) 0.015(7) 0.128(10) -0.007(8) P21 0.046(3) 0.027(2) 0.046(2) 0.0011(16) 0.008(2) -0.0008(17) F22 0.084(7) 0.35(2) 0.077(7) -0.047(9) 0.044(6) -0.103(10) F23 0.078(5) 0.060(5) 0.051(4) 0.003(3) 0.013(4) -0.001(4) F24 0.225(13) 0.062(6) 0.069(6) -0.002(4) 0.015(7) 0.048(7) N13S 0.144(13) 0.082(10) 0.087(10) -0.014(7) 0.007(9) -0.040(9) C11S 0.100(13) 0.148(15) 0.072(11) 0.017(9) 0.018(9) -0.016(11) C12S 0.101(12) 0.091(12) 0.058(9) -0.012(7) 0.007(9) -0.021(9) N43S 0.099(9) 0.051(7) 0.058(7) 0.001(5) 0.019(6) -0.005(6) C41S 0.107(11) 0.070(9) 0.071(9) 0.023(7) 0.047(8) -0.003(8) C42S 0.105(10) 0.052(8) 0.069(9) 0.003(6) 0.033(8) 0.005(7) _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 N51A 2.042(10) . ? Ru1 N62A 2.048(11) . ? Ru1 N11A 2.059(10) . ? Ru1 N42A 2.060(9) . ? Ru1 N22A 2.062(10) . ? Ru1 N31A 2.085(9) . ? N11A C16A 1.311(15) . ? N11A C12A 1.376(15) . ? N21A N22A 1.320(13) . ? N21A C25A 1.351(16) . ? N21A H21A 0.8598 . ? N22A C23A 1.344(14) . ? N31A C32A 1.356(13) . ? N31A C36A 1.359(13) . ? N41A C45A 1.340(14) . ? N41A N42A 1.350(13) . ? N41A H41A 0.8574 . ? N42A C43A 1.310(13) . ? N51A C52A 1.364(19) . ? N51A C56A 1.382(18) . ? N61A C65A 1.299(18) . ? N61A N62A 1.339(15) . ? N61A H61A 0.8592 . ? N62A C63A 1.343(16) . ? C12A C13A 1.419(17) . ? C12A C23A 1.424(18) . ? C13A C14A 1.322(19) . ? C13A H13A 0.9500 . ? C14A C15A 1.258(18) . ? C14A H14A 0.9500 . ? C15A C16A 1.406(16) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C23A C24A 1.514(19) . ? C24A C25A 1.407(19) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? C32A C33A 1.399(15) . ? C32A C43A 1.450(15) . ? C33A C34A 1.358(16) . ? C33A H33A 0.9500 . ? C34A C35A 1.388(16) . ? C34A H34A 0.9500 . ? C35A C36A 1.342(16) . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? C43A C44A 1.412(15) . ? C44A C45A 1.399(17) . ? C44A H44A 0.9500 . ? C45A H45A 0.9500 . ? C52A C63A 1.39(2) . ? C52A C53A 1.403(18) . ? C53A C54A 1.35(3) . ? C53A H53A 0.9500 . ? C54A C55A 1.35(2) . ? C54A H54A 0.9500 . ? C55A C56A 1.369(17) . ? C55A H55A 0.9500 . ? C56A H56A 0.9500 . ? C63A C64A 1.53(2) . ? C64A C65A 1.43(2) . ? C64A H64A 0.9500 . ? C65A H65A 0.9500 . ? P11 F13 1.583(10) . ? P11 F16 1.587(10) . ? P11 F14 1.587(10) . ? P11 F12 1.591(9) . ? P11 F17 1.593(9) . ? P11 F15 1.597(8) . ? P31 F32 1.567(9) 3_666 ? P31 F32 1.567(9) . ? P31 F34 1.574(11) . ? P31 F34 1.574(11) 3_666 ? P31 F33 1.583(10) . ? P31 F33 1.584(10) 3_666 ? P21 F24 1.539(9) . ? P21 F24 1.540(9) 3_566 ? P21 F22 1.552(9) . ? P21 F22 1.552(9) 3_566 ? P21 F23 1.598(7) . ? P21 F23 1.598(7) 3_566 ? N13S C12S 1.15(2) . ? C11S C12S 1.36(2) . ? C11S H11A 0.9124 . ? C11S H11B 0.9628 . ? C11S H11C 0.9145 . ? N43S C42S 1.134(16) . ? C41S C42S 1.450(19) . ? C41S H41E 0.9800 . ? C41S H41F 0.9800 . ? C41S H41G 0.9800 . ? 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 N51A Ru1 N62A 77.0(5) . . ? N51A Ru1 N11A 88.2(4) . . ? N62A Ru1 N11A 94.8(4) . . ? N51A Ru1 N42A 172.6(4) . . ? N62A Ru1 N42A 97.8(4) . . ? N11A Ru1 N42A 97.6(3) . . ? N51A Ru1 N22A 95.5(4) . . ? N62A Ru1 N22A 169.4(4) . . ? N11A Ru1 N22A 77.3(4) . . ? N42A Ru1 N22A 90.3(4) . . ? N51A Ru1 N31A 98.1(4) . . ? N62A Ru1 N31A 92.3(4) . . ? N11A Ru1 N31A 171.5(3) . . ? N42A Ru1 N31A 76.6(3) . . ? N22A Ru1 N31A 96.3(4) . . ? C16A N11A C12A 115.7(11) . . ? C16A N11A Ru1 128.7(8) . . ? C12A N11A Ru1 115.6(9) . . ? N22A N21A C25A 113.1(11) . . ? N22A N21A H21A 123.5 . . ? C25A N21A H21A 123.4 . . ? N21A N22A C23A 107.1(10) . . ? N21A N22A Ru1 136.0(8) . . ? C23A N22A Ru1 116.9(9) . . ? C32A N31A C36A 118.0(9) . . ? C32A N31A Ru1 115.9(7) . . ? C36A N31A Ru1 126.1(7) . . ? C45A N41A N42A 112.1(10) . . ? C45A N41A H41A 123.7 . . ? N42A N41A H41A 124.2 . . ? C43A N42A N41A 107.1(9) . . ? C43A N42A Ru1 117.7(7) . . ? N41A N42A Ru1 135.1(7) . . ? C52A N51A C56A 116.5(11) . . ? C52A N51A Ru1 115.7(11) . . ? C56A N51A Ru1 127.7(10) . . ? C65A N61A N62A 112.8(14) . . ? C65A N61A H61A 123.7 . . ? N62A N61A H61A 123.5 . . ? N61A N62A C63A 110.7(12) . . ? N61A N62A Ru1 133.2(9) . . ? C63A N62A Ru1 115.6(11) . . ? N11A C12A C13A 121.0(14) . . ? N11A C12A C23A 115.2(11) . . ? C13A C12A C23A 123.8(13) . . ? C14A C13A C12A 118.0(14) . . ? C14A C13A H13A 121.0 . . ? C12A C13A H13A 121.0 . . ? C15A C14A C13A 122.1(15) . . ? C15A C14A H14A 118.9 . . ? C13A C14A H14A 118.9 . . ? C14A C15A C16A 120.4(15) . . ? C14A C15A H15A 119.8 . . ? C16A C15A H15A 119.8 . . ? N11A C16A C15A 122.5(12) . . ? N11A C16A H16A 118.7 . . ? C15A C16A H16A 118.7 . . ? N22A C23A C12A 114.9(12) . . ? N22A C23A C24A 109.9(12) . . ? C12A C23A C24A 135.3(11) . . ? C25A C24A C23A 100.4(11) . . ? C25A C24A H24A 129.8 . . ? C23A C24A H24A 129.8 . . ? N21A C25A C24A 109.5(13) . . ? N21A C25A H25A 125.3 . . ? C24A C25A H25A 125.3 . . ? N31A C32A C33A 122.1(10) . . ? N31A C32A C43A 114.1(9) . . ? C33A C32A C43A 123.8(10) . . ? C34A C33A C32A 118.4(11) . . ? C34A C33A H33A 120.8 . . ? C32A C33A H33A 120.8 . . ? C33A C34A C35A 119.0(11) . . ? C33A C34A H34A 120.5 . . ? C35A C34A H34A 120.5 . . ? C36A C35A C34A 120.9(12) . . ? C36A C35A H35A 119.5 . . ? C34A C35A H35A 119.5 . . ? C35A C36A N31A 121.6(11) . . ? C35A C36A H36A 119.2 . . ? N31A C36A H36A 119.2 . . ? N42A C43A C44A 109.5(10) . . ? N42A C43A C32A 115.6(9) . . ? C44A C43A C32A 134.8(10) . . ? C45A C44A C43A 105.7(10) . . ? C45A C44A H44A 127.2 . . ? C43A C44A H44A 127.2 . . ? N41A C45A C44A 105.5(11) . . ? N41A C45A H45A 127.3 . . ? C44A C45A H45A 127.3 . . ? N51A C52A C63A 114.6(11) . . ? N51A C52A C53A 124.8(18) . . ? C63A C52A C53A 120.6(17) . . ? C54A C53A C52A 114.1(19) . . ? C54A C53A H53A 123.0 . . ? C52A C53A H53A 123.0 . . ? C55A C54A C53A 124.4(17) . . ? C55A C54A H54A 117.8 . . ? C53A C54A H54A 117.8 . . ? C54A C55A C56A 119.2(18) . . ? C54A C55A H55A 120.4 . . ? C56A C55A H55A 120.4 . . ? C55A C56A N51A 120.8(16) . . ? C55A C56A H56A 119.6 . . ? N51A C56A H56A 119.6 . . ? N62A C63A C52A 116.1(13) . . ? N62A C63A C64A 104.9(14) . . ? C52A C63A C64A 139.0(13) . . ? C65A C64A C63A 102.7(12) . . ? C65A C64A H64A 128.6 . . ? C63A C64A H64A 128.6 . . ? N61A C65A C64A 108.7(16) . . ? N61A C65A H65A 125.6 . . ? C64A C65A H65A 125.6 . . ? F13 P11 F16 177.7(6) . . ? F13 P11 F14 92.5(8) . . ? F16 P11 F14 86.0(6) . . ? F13 P11 F12 90.6(6) . . ? F16 P11 F12 90.8(5) . . ? F14 P11 F12 176.4(7) . . ? F13 P11 F17 92.7(6) . . ? F16 P11 F17 89.1(5) . . ? F14 P11 F17 90.2(6) . . ? F12 P11 F17 91.3(6) . . ? F13 P11 F15 88.0(5) . . ? F16 P11 F15 90.2(5) . . ? F14 P11 F15 89.8(5) . . ? F12 P11 F15 88.6(5) . . ? F17 P11 F15 179.3(6) . . ? F32 P31 F32 179.999(3) 3_666 . ? F32 P31 F34 87.1(6) 3_666 . ? F32 P31 F34 92.9(6) . . ? F32 P31 F34 92.9(6) 3_666 3_666 ? F32 P31 F34 87.1(6) . 3_666 ? F34 P31 F34 180.0(10) . 3_666 ? F32 P31 F33 90.2(6) 3_666 . ? F32 P31 F33 89.8(5) . . ? F34 P31 F33 90.4(6) . . ? F34 P31 F33 89.6(6) 3_666 . ? F32 P31 F33 89.8(6) 3_666 3_666 ? F32 P31 F33 90.2(5) . 3_666 ? F34 P31 F33 89.6(6) . 3_666 ? F34 P31 F33 90.4(6) 3_666 3_666 ? F33 P31 F33 180.00(6) . 3_666 ? F24 P21 F24 179.998(5) . 3_566 ? F24 P21 F22 89.8(8) . . ? F24 P21 F22 90.2(8) 3_566 . ? F24 P21 F22 90.2(8) . 3_566 ? F24 P21 F22 89.8(8) 3_566 3_566 ? F22 P21 F22 179.998(3) . 3_566 ? F24 P21 F23 88.5(4) . . ? F24 P21 F23 91.5(4) 3_566 . ? F22 P21 F23 88.6(5) . . ? F22 P21 F23 91.4(5) 3_566 . ? F24 P21 F23 91.5(4) . 3_566 ? F24 P21 F23 88.5(4) 3_566 3_566 ? F22 P21 F23 91.4(5) . 3_566 ? F22 P21 F23 88.6(5) 3_566 3_566 ? F23 P21 F23 179.997(2) . 3_566 ? C12S C11S H11A 110.4 . . ? C12S C11S H11B 108.7 . . ? H11A C11S H11B 114.8 . . ? C12S C11S H11C 110.7 . . ? H11A C11S H11C 107.9 . . ? H11B C11S H11C 104.3 . . ? N13S C12S C11S 173(2) . . ? C42S C41S H41E 109.5 . . ? C42S C41S H41F 109.5 . . ? H41E C41S H41F 109.5 . . ? C42S C41S H41G 109.5 . . ? H41E C41S H41G 109.5 . . ? H41F C41S H41G 109.5 . . ? N43S C42S C41S 175.9(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N51A Ru1 N11A C16A -80.2(10) . . . . ? N62A Ru1 N11A C16A -3.4(10) . . . . ? N42A Ru1 N11A C16A 95.1(10) . . . . ? N22A Ru1 N11A C16A -176.2(10) . . . . ? N31A Ru1 N11A C16A 142(2) . . . . ? N51A Ru1 N11A C12A 98.7(8) . . . . ? N62A Ru1 N11A C12A 175.5(8) . . . . ? N42A Ru1 N11A C12A -86.0(8) . . . . ? N22A Ru1 N11A C12A 2.6(7) . . . . ? N31A Ru1 N11A C12A -39(3) . . . . ? C25A N21A N22A C23A 1.4(13) . . . . ? C25A N21A N22A Ru1 179.2(8) . . . . ? N51A Ru1 N22A N21A 92.3(10) . . . . ? N62A Ru1 N22A N21A 137(2) . . . . ? N11A Ru1 N22A N21A 179.1(11) . . . . ? N42A Ru1 N22A N21A -83.1(10) . . . . ? N31A Ru1 N22A N21A -6.5(11) . . . . ? N51A Ru1 N22A C23A -90.0(8) . . . . ? N62A Ru1 N22A C23A -46(2) . . . . ? N11A Ru1 N22A C23A -3.2(7) . . . . ? N42A Ru1 N22A C23A 94.6(8) . . . . ? N31A Ru1 N22A C23A 171.2(8) . . . . ? N51A Ru1 N31A C32A 174.5(8) . . . . ? N62A Ru1 N31A C32A 97.3(8) . . . . ? N11A Ru1 N31A C32A -48(3) . . . . ? N42A Ru1 N31A C32A -0.2(8) . . . . ? N22A Ru1 N31A C32A -89.0(8) . . . . ? N51A Ru1 N31A C36A -7.8(10) . . . . ? N62A Ru1 N31A C36A -84.9(9) . . . . ? N11A Ru1 N31A C36A 129(2) . . . . ? N42A Ru1 N31A C36A 177.6(10) . . . . ? N22A Ru1 N31A C36A 88.7(9) . . . . ? C45A N41A N42A C43A 1.4(15) . . . . ? C45A N41A N42A Ru1 -178.1(10) . . . . ? N51A Ru1 N42A C43A -44(4) . . . . ? N62A Ru1 N42A C43A -89.4(9) . . . . ? N11A Ru1 N42A C43A 174.7(9) . . . . ? N22A Ru1 N42A C43A 97.4(9) . . . . ? N31A Ru1 N42A C43A 1.0(9) . . . . ? N51A Ru1 N42A N41A 135(3) . . . . ? N62A Ru1 N42A N41A 90.1(12) . . . . ? N11A Ru1 N42A N41A -5.8(12) . . . . ? N22A Ru1 N42A N41A -83.1(12) . . . . ? N31A Ru1 N42A N41A -179.4(12) . . . . ? N62A Ru1 N51A C52A -9.1(8) . . . . ? N11A Ru1 N51A C52A 86.2(9) . . . . ? N42A Ru1 N51A C52A -55(4) . . . . ? N22A Ru1 N51A C52A 163.3(8) . . . . ? N31A Ru1 N51A C52A -99.6(8) . . . . ? N62A Ru1 N51A C56A 173.9(11) . . . . ? N11A Ru1 N51A C56A -90.8(10) . . . . ? N42A Ru1 N51A C56A 128(3) . . . . ? N22A Ru1 N51A C56A -13.7(10) . . . . ? N31A Ru1 N51A C56A 83.4(10) . . . . ? C65A N61A N62A C63A -2.5(15) . . . . ? C65A N61A N62A Ru1 -174.0(9) . . . . ? N51A Ru1 N62A N61A 179.4(11) . . . . ? N11A Ru1 N62A N61A 92.4(11) . . . . ? N42A Ru1 N62A N61A -6.0(11) . . . . ? N22A Ru1 N62A N61A 134(2) . . . . ? N31A Ru1 N62A N61A -82.8(11) . . . . ? N51A Ru1 N62A C63A 8.3(8) . . . . ? N11A Ru1 N62A C63A -78.7(8) . . . . ? N42A Ru1 N62A C63A -177.1(8) . . . . ? N22A Ru1 N62A C63A -37(3) . . . . ? N31A Ru1 N62A C63A 106.1(8) . . . . ? C16A N11A C12A C13A -0.5(15) . . . . ? Ru1 N11A C12A C13A -179.6(8) . . . . ? C16A N11A C12A C23A 177.2(10) . . . . ? Ru1 N11A C12A C23A -1.9(12) . . . . ? N11A C12A C13A C14A -3.1(17) . . . . ? C23A C12A C13A C14A 179.4(11) . . . . ? C12A C13A C14A C15A 4(2) . . . . ? C13A C14A C15A C16A -1(2) . . . . ? C12A N11A C16A C15A 3.4(16) . . . . ? Ru1 N11A C16A C15A -177.7(8) . . . . ? C14A C15A C16A N11A -2.7(18) . . . . ? N21A N22A C23A C12A -178.5(9) . . . . ? Ru1 N22A C23A C12A 3.1(12) . . . . ? N21A N22A C23A C24A 0.0(12) . . . . ? Ru1 N22A C23A C24A -178.3(7) . . . . ? N11A C12A C23A N22A -0.8(14) . . . . ? C13A C12A C23A N22A 176.8(10) . . . . ? N11A C12A C23A C24A -178.8(11) . . . . ? C13A C12A C23A C24A -1(2) . . . . ? N22A C23A C24A C25A -1.2(12) . . . . ? C12A C23A C24A C25A 176.9(13) . . . . ? N22A N21A C25A C24A -2.3(14) . . . . ? C23A C24A C25A N21A 2.0(13) . . . . ? C36A N31A C32A C33A -1.7(16) . . . . ? Ru1 N31A C32A C33A 176.3(8) . . . . ? C36A N31A C32A C43A -178.6(9) . . . . ? Ru1 N31A C32A C43A -0.6(12) . . . . ? N31A C32A C33A C34A 2.4(17) . . . . ? C43A C32A C33A C34A 178.9(11) . . . . ? C32A C33A C34A C35A -1.8(18) . . . . ? C33A C34A C35A C36A 0.7(19) . . . . ? C34A C35A C36A N31A -0.1(19) . . . . ? C32A N31A C36A C35A 0.5(16) . . . . ? Ru1 N31A C36A C35A -177.2(9) . . . . ? N41A N42A C43A C44A -0.2(14) . . . . ? Ru1 N42A C43A C44A 179.5(8) . . . . ? N41A N42A C43A C32A 178.7(10) . . . . ? Ru1 N42A C43A C32A -1.7(14) . . . . ? N31A C32A C43A N42A 1.5(15) . . . . ? C33A C32A C43A N42A -175.3(11) . . . . ? N31A C32A C43A C44A 179.9(13) . . . . ? C33A C32A C43A C44A 3(2) . . . . ? N42A C43A C44A C45A -1.1(15) . . . . ? C32A C43A C44A C45A -179.6(13) . . . . ? N42A N41A C45A C44A -2.0(16) . . . . ? C43A C44A C45A N41A 1.8(16) . . . . ? C56A N51A C52A C63A -174.0(11) . . . . ? Ru1 N51A C52A C63A 8.7(14) . . . . ? C56A N51A C52A C53A 4.2(18) . . . . ? Ru1 N51A C52A C53A -173.1(10) . . . . ? N51A C52A C53A C54A -2(2) . . . . ? C63A C52A C53A C54A 176.0(13) . . . . ? C52A C53A C54A C55A -3(2) . . . . ? C53A C54A C55A C56A 5(2) . . . . ? C54A C55A C56A N51A -3(2) . . . . ? C52A N51A C56A C55A -1.7(17) . . . . ? Ru1 N51A C56A C55A 175.2(9) . . . . ? N61A N62A C63A C52A -179.4(10) . . . . ? Ru1 N62A C63A C52A -6.3(14) . . . . ? N61A N62A C63A C64A -0.2(13) . . . . ? Ru1 N62A C63A C64A 172.9(7) . . . . ? N51A C52A C63A N62A -1.5(16) . . . . ? C53A C52A C63A N62A -179.8(11) . . . . ? N51A C52A C63A C64A 179.6(13) . . . . ? C53A C52A C63A C64A 1(2) . . . . ? N62A C63A C64A C65A 2.5(13) . . . . ? C52A C63A C64A C65A -178.6(15) . . . . ? N62A N61A C65A C64A 4.2(16) . . . . ? C63A C64A C65A N61A -4.0(15) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.145 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.154 _database_code_depnum_ccdc_archive 'CCDC 959997' ####################################################################### # # 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_imw1546p-34thmarch _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H21 N9 Ru, C24 H18 N9 Ru, F6 P, 3(C7 H8)' _chemical_formula_sum 'C34.50 H31.50 F3 N9 P0.50 Ru' _chemical_formula_weight 745.74 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 Trigonal _symmetry_space_group_name_H-M 'P-3 ' _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 14.1604(10) _cell_length_b 14.1604(10) _cell_length_c 19.0761(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3312.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1353 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 22.36 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9836 _exptl_absorpt_correction_T_max 0.9890 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12287 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 27.54 _reflns_number_total 5090 _reflns_number_gt 3485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _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. Solved by direct methods. One third each of the protonated complex cation along with one third of the tris-deprotonated complex are present in the asymmetric unit, along with one sixth each of two PF6 anions. The occupancy of the PF6 anions indicate that one PF6 anion is shared between the two complexes in order to balance the charge. A whole toluene solvent molecule is also present. ; _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^)+(0.0701P)^2^+1.1150P] 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 5090 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1218 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 0.3333 0.6667 0.08122(3) 0.01554(17) Uani 1 3 d S . . N11A N 0.3625(3) 0.5603(3) 0.02259(19) 0.0213(8) Uani 1 1 d . . . C12A C 0.3037(4) 0.4522(4) 0.0413(2) 0.0213(10) Uani 1 1 d . . . C13A C 0.3053(4) 0.3712(4) 0.0004(3) 0.0305(11) Uani 1 1 d . . . H13A H 0.2626 0.2966 0.0134 0.037 Uiso 1 1 calc R . . C14A C 0.3699(5) 0.4006(5) -0.0593(3) 0.0364(13) Uani 1 1 d . . . H14A H 0.3719 0.3463 -0.0876 0.044 Uiso 1 1 calc R . . C15A C 0.4315(4) 0.5100(5) -0.0774(3) 0.0346(12) Uani 1 1 d . . . H15A H 0.4771 0.5317 -0.1176 0.042 Uiso 1 1 calc R . . C16A C 0.4256(4) 0.5860(4) -0.0362(2) 0.0266(11) Uani 1 1 d . . . H16A H 0.4677 0.6606 -0.0492 0.032 Uiso 1 1 calc R . . N21A N 0.1785(3) 0.4864(3) 0.19124(19) 0.0194(8) Uani 1 1 d . . . H21A H 0.1660 0.5279 0.2196 0.09(3) Uiso 1 1 calc R . . N22A N 0.2428(3) 0.5214(3) 0.13426(19) 0.0172(8) Uani 1 1 d . . . C23A C 0.2401(4) 0.4326(4) 0.1045(2) 0.0199(9) Uani 1 1 d . . . C24A C 0.1719(4) 0.3399(4) 0.1439(3) 0.0244(10) Uani 1 1 d . . . H24A H 0.1543 0.2668 0.1351 0.029 Uiso 1 1 calc R . . C25A C 0.1360(4) 0.3776(4) 0.1984(3) 0.0236(10) Uani 1 1 d . . . H25A H 0.0889 0.3341 0.2350 0.028 Uiso 1 1 calc R . . Ru2 Ru 0.3333 0.6667 0.38397(3) 0.01390(17) Uani 1 3 d S . . N11B N 0.2184(3) 0.5329(3) 0.44042(19) 0.0172(8) Uani 1 1 d . . . C12B C 0.2021(3) 0.4334(3) 0.4191(2) 0.0186(9) Uani 1 1 d . . . C13B C 0.1278(4) 0.3375(4) 0.4534(3) 0.0234(10) Uani 1 1 d . . . H13B H 0.1167 0.2691 0.4376 0.028 Uiso 1 1 calc R . . C14B C 0.0708(4) 0.3428(4) 0.5102(3) 0.0297(11) Uani 1 1 d . . . H14B H 0.0211 0.2783 0.5346 0.036 Uiso 1 1 calc R . . C15B C 0.0867(4) 0.4442(4) 0.5316(3) 0.0285(11) Uani 1 1 d . . . H15B H 0.0479 0.4495 0.5706 0.034 Uiso 1 1 calc R . . C16B C 0.1597(4) 0.5363(4) 0.4954(2) 0.0232(10) Uani 1 1 d . . . H16B H 0.1691 0.6048 0.5095 0.028 Uiso 1 1 calc R . . N21B N 0.3912(3) 0.5310(3) 0.27941(19) 0.0178(8) Uani 1 1 d . . . N22B N 0.3330(3) 0.5391(3) 0.33226(18) 0.0157(7) Uani 1 1 d . . . C23B C 0.2696(3) 0.4390(3) 0.3601(2) 0.0166(9) Uani 1 1 d . . . C24B C 0.2869(4) 0.3630(4) 0.3241(2) 0.0223(10) Uani 1 1 d . . . H24B H 0.2534 0.2867 0.3320 0.027 Uiso 1 1 calc R . . C25B C 0.3643(4) 0.4250(4) 0.2741(2) 0.0226(10) Uani 1 1 d . . . H25B H 0.3942 0.3972 0.2409 0.027 Uiso 1 1 calc R . . P1 P 1.0000 1.0000 0.5000 0.0209(6) Uani 1 6 d S . . F1 F 0.9619(3) 0.8960(3) 0.45183(19) 0.0545(10) Uani 1 1 d . . . P2 P 0.0000 0.0000 0.0000 0.0310(7) Uani 1 6 d S . . F2 F 0.0914(5) 0.0881(6) 0.0447(4) 0.161(3) Uani 1 1 d . . . C1S C 0.7602(5) 0.6163(6) 0.2915(4) 0.0518(17) Uani 1 1 d . . . C2S C 0.8098(5) 0.7172(6) 0.3225(3) 0.0501(17) Uani 1 1 d . . . H2S H 0.7968 0.7221 0.3709 0.060 Uiso 1 1 calc R . . C3S C 0.8774(5) 0.8116(6) 0.2866(4) 0.0569(18) Uani 1 1 d . . . H3S H 0.9090 0.8801 0.3098 0.068 Uiso 1 1 calc R . . C4S C 0.8986(5) 0.8061(6) 0.2182(4) 0.0552(18) Uani 1 1 d . . . H4S H 0.9456 0.8709 0.1932 0.066 Uiso 1 1 calc R . . C5S C 0.8527(5) 0.7078(7) 0.1849(4) 0.058(2) Uani 1 1 d . . . H5S H 0.8680 0.7046 0.1367 0.070 Uiso 1 1 calc R . . C6S C 0.7834(5) 0.6116(6) 0.2211(4) 0.0555(18) Uani 1 1 d . . . H6S H 0.7522 0.5433 0.1977 0.067 Uiso 1 1 calc R . . C7S C 0.6827(7) 0.5137(7) 0.3306(5) 0.095(3) Uani 1 1 d . . . H7S1 H 0.7219 0.5012 0.3685 0.143 Uiso 1 1 calc R . . H7S2 H 0.6527 0.4516 0.2982 0.143 Uiso 1 1 calc R . . H7S3 H 0.6231 0.5215 0.3503 0.143 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0163(2) 0.0163(2) 0.0140(3) 0.000 0.000 0.00815(11) N11A 0.022(2) 0.029(2) 0.0150(19) -0.0039(16) -0.0015(15) 0.0143(17) C12A 0.023(2) 0.021(2) 0.023(2) -0.0052(19) -0.0056(19) 0.014(2) C13A 0.031(3) 0.029(3) 0.033(3) -0.009(2) -0.007(2) 0.017(2) C14A 0.044(3) 0.044(3) 0.032(3) -0.015(3) -0.007(3) 0.030(3) C15A 0.037(3) 0.047(3) 0.025(3) -0.003(2) 0.007(2) 0.025(3) C16A 0.027(3) 0.029(3) 0.024(3) 0.000(2) 0.003(2) 0.014(2) N21A 0.0171(19) 0.0227(19) 0.0165(19) 0.0012(16) -0.0011(15) 0.0085(16) N22A 0.0150(18) 0.0179(19) 0.0177(19) -0.0019(15) -0.0024(15) 0.0074(15) C23A 0.020(2) 0.019(2) 0.022(2) -0.0028(18) -0.0064(19) 0.0109(19) C24A 0.025(2) 0.017(2) 0.030(3) -0.002(2) -0.006(2) 0.010(2) C25A 0.022(2) 0.020(2) 0.025(3) 0.0020(19) -0.007(2) 0.007(2) Ru2 0.0135(2) 0.0135(2) 0.0147(3) 0.000 0.000 0.00676(11) N11B 0.0144(17) 0.0154(18) 0.0192(19) 0.0019(15) -0.0021(15) 0.0055(15) C12B 0.018(2) 0.015(2) 0.020(2) 0.0031(17) -0.0058(18) 0.0056(18) C13B 0.017(2) 0.017(2) 0.030(3) 0.0027(19) -0.004(2) 0.0047(18) C14B 0.022(2) 0.025(3) 0.035(3) 0.014(2) 0.009(2) 0.006(2) C15B 0.025(3) 0.034(3) 0.028(3) 0.008(2) 0.009(2) 0.016(2) C16B 0.019(2) 0.026(2) 0.025(2) 0.003(2) 0.0046(19) 0.011(2) N21B 0.0219(19) 0.0207(19) 0.0177(18) -0.0040(15) -0.0013(15) 0.0158(16) N22B 0.0197(18) 0.0177(18) 0.0130(18) -0.0011(14) -0.0030(15) 0.0118(15) C23B 0.021(2) 0.015(2) 0.016(2) -0.0006(17) -0.0032(18) 0.0101(18) C24B 0.027(2) 0.018(2) 0.024(2) -0.0023(19) -0.009(2) 0.013(2) C25B 0.031(3) 0.023(2) 0.022(2) -0.0005(19) 0.000(2) 0.020(2) P1 0.0185(9) 0.0185(9) 0.0259(16) 0.000 0.000 0.0092(4) F1 0.070(3) 0.0352(19) 0.055(2) -0.0209(17) -0.008(2) 0.0240(19) P2 0.0328(11) 0.0328(11) 0.0274(17) 0.000 0.000 0.0164(5) F2 0.143(6) 0.135(6) 0.171(6) -0.078(5) -0.095(5) 0.043(4) C1S 0.040(4) 0.067(5) 0.058(4) 0.022(4) 0.002(3) 0.034(3) C2S 0.048(4) 0.086(5) 0.040(4) -0.008(4) -0.007(3) 0.051(4) C3S 0.044(4) 0.058(4) 0.076(5) -0.008(4) -0.014(4) 0.031(4) C4S 0.034(3) 0.058(4) 0.070(5) 0.014(4) -0.004(3) 0.020(3) C5S 0.048(4) 0.106(6) 0.040(4) 0.008(4) 0.005(3) 0.052(4) C6S 0.048(4) 0.058(4) 0.072(5) -0.020(4) -0.021(4) 0.035(4) C7S 0.067(5) 0.090(6) 0.120(8) 0.062(6) 0.003(5) 0.033(5) _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 N22A 2.065(4) . ? Ru1 N22A 2.065(4) 3_565 ? Ru1 N22A 2.065(4) 2_665 ? Ru1 N11A 2.077(4) 3_565 ? Ru1 N11A 2.077(4) 2_665 ? Ru1 N11A 2.077(4) . ? N11A C16A 1.365(6) . ? N11A C12A 1.374(6) . ? C12A C13A 1.396(6) . ? C12A C23A 1.446(6) . ? C13A C14A 1.388(7) . ? C13A H13A 0.9500 . ? C14A C15A 1.389(8) . ? C14A H14A 0.9500 . ? C15A C16A 1.369(7) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? N21A N22A 1.343(5) . ? N21A C25A 1.352(6) . ? N21A H21A 0.8800 . ? N22A C23A 1.362(5) . ? C23A C24A 1.398(6) . ? C24A C25A 1.376(7) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? Ru2 N22B 2.057(3) . ? Ru2 N22B 2.057(3) 3_565 ? Ru2 N22B 2.057(3) 2_665 ? Ru2 N11B 2.077(3) 2_665 ? Ru2 N11B 2.077(3) . ? Ru2 N11B 2.077(3) 3_565 ? N11B C16B 1.355(6) . ? N11B C12B 1.370(5) . ? C12B C13B 1.396(6) . ? C12B C23B 1.452(6) . ? C13B C14B 1.376(7) . ? C13B H13B 0.9500 . ? C14B C15B 1.398(7) . ? C14B H14B 0.9500 . ? C15B C16B 1.377(6) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? N21B N22B 1.342(5) . ? N21B C25B 1.356(5) . ? N22B C23B 1.351(5) . ? C23B C24B 1.398(6) . ? C24B C25B 1.385(7) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? P1 F1 1.584(3) 4_776 ? P1 F1 1.584(3) 6_656 ? P1 F1 1.584(3) 3_675 ? P1 F1 1.584(3) 2_765 ? P1 F1 1.584(3) 5_566 ? P1 F1 1.584(3) . ? P2 F2 1.531(5) . ? P2 F2 1.531(5) 4 ? P2 F2 1.531(5) 5 ? P2 F2 1.531(5) 2 ? P2 F2 1.531(5) 6 ? P2 F2 1.531(5) 3 ? C1S C2S 1.372(9) . ? C1S C6S 1.391(9) . ? C1S C7S 1.510(9) . ? C2S C3S 1.376(10) . ? C2S H2S 0.9500 . ? C3S C4S 1.350(10) . ? C3S H3S 0.9500 . ? C4S C5S 1.364(10) . ? C4S H4S 0.9500 . ? C5S C6S 1.400(10) . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? 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 N22A Ru1 N22A 98.03(13) . 3_565 ? N22A Ru1 N22A 98.03(13) . 2_665 ? N22A Ru1 N22A 98.03(13) 3_565 2_665 ? N22A Ru1 N11A 90.84(14) . 3_565 ? N22A Ru1 N11A 77.89(14) 3_565 3_565 ? N22A Ru1 N11A 170.72(14) 2_665 3_565 ? N22A Ru1 N11A 170.72(14) . 2_665 ? N22A Ru1 N11A 90.84(14) 3_565 2_665 ? N22A Ru1 N11A 77.89(14) 2_665 2_665 ? N11A Ru1 N11A 93.73(14) 3_565 2_665 ? N22A Ru1 N11A 77.90(14) . . ? N22A Ru1 N11A 170.72(14) 3_565 . ? N22A Ru1 N11A 90.84(14) 2_665 . ? N11A Ru1 N11A 93.73(14) 3_565 . ? N11A Ru1 N11A 93.73(14) 2_665 . ? C16A N11A C12A 117.5(4) . . ? C16A N11A Ru1 126.1(3) . . ? C12A N11A Ru1 116.0(3) . . ? N11A C12A C13A 121.4(4) . . ? N11A C12A C23A 113.7(4) . . ? C13A C12A C23A 124.9(4) . . ? C14A C13A C12A 119.4(5) . . ? C14A C13A H13A 120.3 . . ? C12A C13A H13A 120.3 . . ? C13A C14A C15A 119.4(5) . . ? C13A C14A H14A 120.3 . . ? C15A C14A H14A 120.3 . . ? C16A C15A C14A 118.9(5) . . ? C16A C15A H15A 120.5 . . ? C14A C15A H15A 120.5 . . ? N11A C16A C15A 123.4(5) . . ? N11A C16A H16A 118.3 . . ? C15A C16A H16A 118.3 . . ? N22A N21A C25A 109.6(4) . . ? N22A N21A H21A 125.2 . . ? C25A N21A H21A 125.2 . . ? N21A N22A C23A 107.2(4) . . ? N21A N22A Ru1 137.1(3) . . ? C23A N22A Ru1 115.6(3) . . ? N22A C23A C24A 109.3(4) . . ? N22A C23A C12A 116.3(4) . . ? C24A C23A C12A 134.4(4) . . ? C25A C24A C23A 104.9(4) . . ? C25A C24A H24A 127.6 . . ? C23A C24A H24A 127.6 . . ? N21A C25A C24A 109.0(4) . . ? N21A C25A H25A 125.5 . . ? C24A C25A H25A 125.5 . . ? N22B Ru2 N22B 98.92(12) . 3_565 ? N22B Ru2 N22B 98.92(12) . 2_665 ? N22B Ru2 N22B 98.92(12) 3_565 2_665 ? N22B Ru2 N11B 87.86(14) . 2_665 ? N22B Ru2 N11B 172.94(14) 3_565 2_665 ? N22B Ru2 N11B 77.93(14) 2_665 2_665 ? N22B Ru2 N11B 77.93(14) . . ? N22B Ru2 N11B 87.86(14) 3_565 . ? N22B Ru2 N11B 172.94(14) 2_665 . ? N11B Ru2 N11B 95.56(13) 2_665 . ? N22B Ru2 N11B 172.94(14) . 3_565 ? N22B Ru2 N11B 77.93(14) 3_565 3_565 ? N22B Ru2 N11B 87.86(14) 2_665 3_565 ? N11B Ru2 N11B 95.56(13) 2_665 3_565 ? N11B Ru2 N11B 95.56(13) . 3_565 ? C16B N11B C12B 118.4(4) . . ? C16B N11B Ru2 125.7(3) . . ? C12B N11B Ru2 115.9(3) . . ? N11B C12B C13B 121.3(4) . . ? N11B C12B C23B 113.9(4) . . ? C13B C12B C23B 124.8(4) . . ? C14B C13B C12B 119.6(4) . . ? C14B C13B H13B 120.2 . . ? C12B C13B H13B 120.2 . . ? C13B C14B C15B 119.2(4) . . ? C13B C14B H14B 120.4 . . ? C15B C14B H14B 120.4 . . ? C16B C15B C14B 119.0(5) . . ? C16B C15B H15B 120.5 . . ? C14B C15B H15B 120.5 . . ? N11B C16B C15B 122.5(4) . . ? N11B C16B H16B 118.7 . . ? C15B C16B H16B 118.7 . . ? N22B N21B C25B 107.7(4) . . ? N21B N22B C23B 108.7(3) . . ? N21B N22B Ru2 134.7(3) . . ? C23B N22B Ru2 116.2(3) . . ? N22B C23B C24B 109.5(4) . . ? N22B C23B C12B 115.9(4) . . ? C24B C23B C12B 134.7(4) . . ? C25B C24B C23B 103.8(4) . . ? C25B C24B H24B 128.1 . . ? C23B C24B H24B 128.1 . . ? N21B C25B C24B 110.3(4) . . ? N21B C25B H25B 124.9 . . ? C24B C25B H25B 124.9 . . ? F1 P1 F1 89.73(19) 4_776 6_656 ? F1 P1 F1 90.27(19) 4_776 3_675 ? F1 P1 F1 180.000(1) 6_656 3_675 ? F1 P1 F1 90.27(19) 4_776 2_765 ? F1 P1 F1 90.27(19) 6_656 2_765 ? F1 P1 F1 89.73(19) 3_675 2_765 ? F1 P1 F1 89.73(19) 4_776 5_566 ? F1 P1 F1 89.73(19) 6_656 5_566 ? F1 P1 F1 90.27(19) 3_675 5_566 ? F1 P1 F1 180.000(1) 2_765 5_566 ? F1 P1 F1 179.999(1) 4_776 . ? F1 P1 F1 90.27(19) 6_656 . ? F1 P1 F1 89.73(19) 3_675 . ? F1 P1 F1 89.73(19) 2_765 . ? F1 P1 F1 90.27(19) 5_566 . ? F2 P2 F2 179.998(1) . 4 ? F2 P2 F2 88.0(4) . 5 ? F2 P2 F2 92.0(4) 4 5 ? F2 P2 F2 92.0(4) . 2 ? F2 P2 F2 88.0(4) 4 2 ? F2 P2 F2 180.0(6) 5 2 ? F2 P2 F2 88.0(4) . 6 ? F2 P2 F2 92.0(4) 4 6 ? F2 P2 F2 92.0(4) 5 6 ? F2 P2 F2 88.0(4) 2 6 ? F2 P2 F2 92.0(4) . 3 ? F2 P2 F2 88.0(4) 4 3 ? F2 P2 F2 88.0(4) 5 3 ? F2 P2 F2 92.0(4) 2 3 ? F2 P2 F2 180.0(6) 6 3 ? C2S C1S C6S 117.2(6) . . ? C2S C1S C7S 122.4(7) . . ? C6S C1S C7S 120.4(8) . . ? C1S C2S C3S 122.8(7) . . ? C1S C2S H2S 118.6 . . ? C3S C2S H2S 118.6 . . ? C4S C3S C2S 119.5(7) . . ? C4S C3S H3S 120.3 . . ? C2S C3S H3S 120.3 . . ? C3S C4S C5S 120.2(7) . . ? C3S C4S H4S 119.9 . . ? C5S C4S H4S 119.9 . . ? C4S C5S C6S 120.5(6) . . ? C4S C5S H5S 119.8 . . ? C6S C5S H5S 119.8 . . ? C1S C6S C5S 119.8(6) . . ? C1S C6S H6S 120.1 . . ? C5S C6S H6S 120.1 . . ? C1S C7S H7S1 109.5 . . ? C1S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C1S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N22A Ru1 N11A C16A 179.3(4) . . . . ? N22A Ru1 N11A C16A 114.5(9) 3_565 . . . ? N22A Ru1 N11A C16A -82.7(4) 2_665 . . . ? N11A Ru1 N11A C16A 89.3(3) 3_565 . . . ? N11A Ru1 N11A C16A -4.7(4) 2_665 . . . ? N22A Ru1 N11A C12A 6.1(3) . . . . ? N22A Ru1 N11A C12A -58.6(10) 3_565 . . . ? N22A Ru1 N11A C12A 104.2(3) 2_665 . . . ? N11A Ru1 N11A C12A -83.9(4) 3_565 . . . ? N11A Ru1 N11A C12A -177.9(3) 2_665 . . . ? C16A N11A C12A C13A -2.2(6) . . . . ? Ru1 N11A C12A C13A 171.6(3) . . . . ? C16A N11A C12A C23A 179.4(4) . . . . ? Ru1 N11A C12A C23A -6.8(5) . . . . ? N11A C12A C13A C14A 1.8(7) . . . . ? C23A C12A C13A C14A 179.9(5) . . . . ? C12A C13A C14A C15A -0.1(8) . . . . ? C13A C14A C15A C16A -1.0(8) . . . . ? C12A N11A C16A C15A 1.1(7) . . . . ? Ru1 N11A C16A C15A -172.0(4) . . . . ? C14A C15A C16A N11A 0.5(8) . . . . ? C25A N21A N22A C23A 0.5(5) . . . . ? C25A N21A N22A Ru1 176.9(3) . . . . ? N22A Ru1 N22A N21A -9.0(4) 3_565 . . . ? N22A Ru1 N22A N21A 90.3(3) 2_665 . . . ? N11A Ru1 N22A N21A -86.9(4) 3_565 . . . ? N11A Ru1 N22A N21A 153.6(8) 2_665 . . . ? N11A Ru1 N22A N21A 179.5(4) . . . . ? N22A Ru1 N22A C23A 167.1(3) 3_565 . . . ? N22A Ru1 N22A C23A -93.5(4) 2_665 . . . ? N11A Ru1 N22A C23A 89.3(3) 3_565 . . . ? N11A Ru1 N22A C23A -30.2(10) 2_665 . . . ? N11A Ru1 N22A C23A -4.4(3) . . . . ? N21A N22A C23A C24A 0.1(5) . . . . ? Ru1 N22A C23A C24A -177.1(3) . . . . ? N21A N22A C23A C12A 179.4(4) . . . . ? Ru1 N22A C23A C12A 2.2(5) . . . . ? N11A C12A C23A N22A 3.0(6) . . . . ? C13A C12A C23A N22A -175.2(4) . . . . ? N11A C12A C23A C24A -177.9(5) . . . . ? C13A C12A C23A C24A 3.8(8) . . . . ? N22A C23A C24A C25A -0.7(5) . . . . ? C12A C23A C24A C25A -179.8(5) . . . . ? N22A N21A C25A C24A -1.0(5) . . . . ? C23A C24A C25A N21A 1.1(5) . . . . ? N22B Ru2 N11B C16B -178.1(4) . . . . ? N22B Ru2 N11B C16B -78.5(4) 3_565 . . . ? N22B Ru2 N11B C16B 117.8(11) 2_665 . . . ? N11B Ru2 N11B C16B 95.3(3) 2_665 . . . ? N11B Ru2 N11B C16B -0.9(4) 3_565 . . . ? N22B Ru2 N11B C12B 1.9(3) . . . . ? N22B Ru2 N11B C12B 101.5(3) 3_565 . . . ? N22B Ru2 N11B C12B -62.2(12) 2_665 . . . ? N11B Ru2 N11B C12B -84.7(4) 2_665 . . . ? N11B Ru2 N11B C12B 179.1(3) 3_565 . . . ? C16B N11B C12B C13B -0.7(6) . . . . ? Ru2 N11B C12B C13B 179.3(3) . . . . ? C16B N11B C12B C23B -179.6(4) . . . . ? Ru2 N11B C12B C23B 0.4(5) . . . . ? N11B C12B C13B C14B -0.9(7) . . . . ? C23B C12B C13B C14B 178.0(4) . . . . ? C12B C13B C14B C15B 1.3(7) . . . . ? C13B C14B C15B C16B -0.3(7) . . . . ? C12B N11B C16B C15B 1.8(7) . . . . ? Ru2 N11B C16B C15B -178.2(3) . . . . ? C14B C15B C16B N11B -1.3(7) . . . . ? C25B N21B N22B C23B -0.2(5) . . . . ? C25B N21B N22B Ru2 171.7(3) . . . . ? N22B Ru2 N22B N21B 98.7(3) 3_565 . . . ? N22B Ru2 N22B N21B -1.9(4) 2_665 . . . ? N11B Ru2 N22B N21B -79.3(4) 2_665 . . . ? N11B Ru2 N22B N21B -175.4(4) . . . . ? N11B Ru2 N22B N21B 161.6(10) 3_565 . . . ? N22B Ru2 N22B C23B -89.9(4) 3_565 . . . ? N22B Ru2 N22B C23B 169.5(3) 2_665 . . . ? N11B Ru2 N22B C23B 92.1(3) 2_665 . . . ? N11B Ru2 N22B C23B -4.1(3) . . . . ? N11B Ru2 N22B C23B -27.0(13) 3_565 . . . ? N21B N22B C23B C24B -0.1(5) . . . . ? Ru2 N22B C23B C24B -173.6(3) . . . . ? N21B N22B C23B C12B 179.1(3) . . . . ? Ru2 N22B C23B C12B 5.5(5) . . . . ? N11B C12B C23B N22B -3.8(5) . . . . ? C13B C12B C23B N22B 177.3(4) . . . . ? N11B C12B C23B C24B 175.0(5) . . . . ? C13B C12B C23B C24B -3.9(8) . . . . ? N22B C23B C24B C25B 0.3(5) . . . . ? C12B C23B C24B C25B -178.6(5) . . . . ? N22B N21B C25B C24B 0.4(5) . . . . ? C23B C24B C25B N21B -0.4(5) . . . . ? C6S C1S C2S C3S 1.9(9) . . . . ? C7S C1S C2S C3S -177.6(6) . . . . ? C1S C2S C3S C4S -1.3(10) . . . . ? C2S C3S C4S C5S 0.4(10) . . . . ? C3S C4S C5S C6S 0.0(10) . . . . ? C2S C1S C6S C5S -1.5(9) . . . . ? C7S C1S C6S C5S 178.0(6) . . . . ? C4S C5S C6S C1S 0.6(10) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.807 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.143 _database_code_depnum_ccdc_archive 'CCDC 959998' ####################################################################### # # 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_imw1768 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H39 N9 Ru, 2(F6 P), 2(C3 H6 O)' _chemical_formula_sum 'C51 H51 F12 N9 O2 P2 Ru' _chemical_formula_weight 1213.02 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1447(2) _cell_length_b 12.2542(3) _cell_length_c 20.6452(4) _cell_angle_alpha 93.7290(10) _cell_angle_beta 95.9190(10) _cell_angle_gamma 111.0040(10) _cell_volume 2602.28(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9976 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 30.82 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8040 _exptl_absorpt_correction_T_max 0.9143 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43754 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0264 _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 -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11756 _reflns_number_gt 10299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0720P)^2^+4.6317P] 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 11756 _refine_ls_number_parameters 698 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.35116(2) 0.283572(17) 0.267880(10) 0.01837(8) Uani 1 1 d . . . N11A N 0.3556(2) 0.4470(2) 0.24563(11) 0.0209(5) Uani 1 1 d . . . C12A C 0.2951(3) 0.5000(2) 0.28325(13) 0.0217(5) Uani 1 1 d . . . C13A C 0.2890(3) 0.6086(3) 0.27217(15) 0.0282(6) Uani 1 1 d . . . H13A H 0.2461 0.6442 0.2991 0.034 Uiso 1 1 calc R . . C14A C 0.3473(4) 0.6638(3) 0.22072(16) 0.0342(7) Uani 1 1 d . . . H14A H 0.3447 0.7381 0.2121 0.041 Uiso 1 1 calc R . . C15A C 0.4089(4) 0.6104(3) 0.18231(16) 0.0365(8) Uani 1 1 d . . . H15A H 0.4493 0.6475 0.1471 0.044 Uiso 1 1 calc R . . C16A C 0.4111(3) 0.5024(3) 0.19578(15) 0.0294(6) Uani 1 1 d . . . H16A H 0.4533 0.4655 0.1690 0.035 Uiso 1 1 calc R . . N21A N 0.1874(2) 0.2810(2) 0.38827(11) 0.0233(5) Uani 1 1 d . . . N22A N 0.2516(2) 0.32842(19) 0.33878(11) 0.0197(4) Uani 1 1 d . . . C23A C 0.2376(3) 0.4330(2) 0.33530(13) 0.0210(5) Uani 1 1 d . . . C24A C 0.1645(3) 0.4522(2) 0.38296(14) 0.0241(6) Uani 1 1 d . . . H24A H 0.1406 0.5185 0.3907 0.029 Uiso 1 1 calc R . . C25A C 0.1348(3) 0.3545(3) 0.41591(14) 0.0259(6) Uani 1 1 d . . . H25A H 0.0862 0.3404 0.4517 0.031 Uiso 1 1 calc R . . C26A C 0.2013(3) 0.1788(2) 0.41550(13) 0.0238(6) Uani 1 1 d . . . H26C H 0.2003 0.1213 0.3793 0.029 Uiso 1 1 calc R . . H26D H 0.1263 0.1408 0.4388 0.029 Uiso 1 1 calc R . . C31A C 0.3255(3) 0.2103(3) 0.46251(14) 0.0254(6) Uani 1 1 d . . . C32A C 0.3742(3) 0.1237(3) 0.47708(17) 0.0331(7) Uani 1 1 d . . . H32A H 0.3297 0.0453 0.4572 0.040 Uiso 1 1 calc R . . C33A C 0.4866(4) 0.1503(3) 0.52021(17) 0.0379(8) Uani 1 1 d . . . H33A H 0.5190 0.0902 0.5294 0.046 Uiso 1 1 calc R . . C34A C 0.5524(3) 0.2640(3) 0.55025(16) 0.0361(7) Uani 1 1 d . . . H34A H 0.6298 0.2822 0.5799 0.043 Uiso 1 1 calc R . . C35A C 0.5044(3) 0.3495(3) 0.53654(17) 0.0379(8) Uani 1 1 d . . . H35A H 0.5483 0.4274 0.5573 0.045 Uiso 1 1 calc R . . C36A C 0.3923(3) 0.3237(3) 0.49271(16) 0.0321(7) Uani 1 1 d . . . H36A H 0.3609 0.3843 0.4833 0.038 Uiso 1 1 calc R . . N11B N 0.5195(2) 0.3463(2) 0.33407(11) 0.0222(5) Uani 1 1 d . . . C12B C 0.5649(3) 0.2639(3) 0.35629(13) 0.0243(6) Uani 1 1 d . . . C13B C 0.6805(3) 0.2944(3) 0.39850(15) 0.0309(6) Uani 1 1 d . . . H13B H 0.7096 0.2353 0.4135 0.037 Uiso 1 1 calc R . . C14B C 0.7521(3) 0.4118(3) 0.41813(15) 0.0335(7) Uani 1 1 d . . . H14B H 0.8315 0.4347 0.4468 0.040 Uiso 1 1 calc R . . C15B C 0.7069(3) 0.4953(3) 0.39563(15) 0.0314(7) Uani 1 1 d . . . H15B H 0.7553 0.5765 0.4084 0.038 Uiso 1 1 calc R . . C16B C 0.5903(3) 0.4603(3) 0.35421(15) 0.0263(6) Uani 1 1 d . . . H16B H 0.5595 0.5186 0.3396 0.032 Uiso 1 1 calc R . . N21B N 0.2988(3) 0.0119(2) 0.28738(12) 0.0256(5) Uani 1 1 d . . . N22B N 0.3659(2) 0.12964(19) 0.29822(11) 0.0214(5) Uani 1 1 d . . . C23B C 0.4797(3) 0.1434(3) 0.33369(14) 0.0250(6) Uani 1 1 d . . . C24B C 0.4863(4) 0.0341(3) 0.34462(16) 0.0335(7) Uani 1 1 d . . . H24B H 0.5562 0.0191 0.3675 0.040 Uiso 1 1 calc R . . C25B C 0.3700(4) -0.0463(3) 0.31503(16) 0.0332(7) Uani 1 1 d . . . H25B H 0.3435 -0.1293 0.3140 0.040 Uiso 1 1 calc R . . C26B C 0.1663(3) -0.0382(2) 0.25415(15) 0.0268(6) Uani 1 1 d . . . H26A H 0.1289 0.0239 0.2547 0.032 Uiso 1 1 calc R . . H26B H 0.1146 -0.1006 0.2791 0.032 Uiso 1 1 calc R . . C31B C 0.1527(3) -0.0899(2) 0.18385(15) 0.0261(6) Uani 1 1 d . . . C32B C 0.0270(3) -0.1424(3) 0.15015(18) 0.0354(7) Uani 1 1 d . . . H32B H -0.0453 -0.1450 0.1716 0.043 Uiso 1 1 calc R . . C33B C 0.0077(4) -0.1905(3) 0.08582(19) 0.0453(9) Uani 1 1 d . . . H33B H -0.0778 -0.2258 0.0630 0.054 Uiso 1 1 calc R . . C34B C 0.1122(5) -0.1875(3) 0.05448(18) 0.0491(10) Uani 1 1 d . . . H34B H 0.0984 -0.2211 0.0103 0.059 Uiso 1 1 calc R . . C35B C 0.2376(4) -0.1356(3) 0.08736(17) 0.0417(8) Uani 1 1 d . . . H35B H 0.3095 -0.1334 0.0657 0.050 Uiso 1 1 calc R . . C36B C 0.2576(3) -0.0866(3) 0.15266(15) 0.0304(6) Uani 1 1 d . . . H36B H 0.3431 -0.0511 0.1754 0.036 Uiso 1 1 calc R . . N11C N 0.4494(2) 0.2576(2) 0.19144(11) 0.0214(5) Uani 1 1 d . . . C12C C 0.3750(3) 0.2058(2) 0.13344(14) 0.0219(5) Uani 1 1 d . . . C13C C 0.4271(3) 0.1783(3) 0.07946(15) 0.0285(6) Uani 1 1 d . . . H13C H 0.3726 0.1416 0.0396 0.034 Uiso 1 1 calc R . . C14C C 0.5595(3) 0.2049(3) 0.08440(15) 0.0313(7) Uani 1 1 d . . . H14C H 0.5972 0.1857 0.0482 0.038 Uiso 1 1 calc R . . C15C C 0.6360(3) 0.2598(3) 0.14291(16) 0.0316(7) Uani 1 1 d . . . H15C H 0.7274 0.2802 0.1472 0.038 Uiso 1 1 calc R . . C16C C 0.5784(3) 0.2846(3) 0.19484(15) 0.0269(6) Uani 1 1 d . . . H16C H 0.6319 0.3225 0.2348 0.032 Uiso 1 1 calc R . . N21C N 0.0699(2) 0.1781(2) 0.17768(12) 0.0233(5) Uani 1 1 d . . . N22C N 0.2009(2) 0.21095(19) 0.18979(11) 0.0208(5) Uani 1 1 d . . . C23C C 0.2373(3) 0.1816(2) 0.13327(14) 0.0224(5) Uani 1 1 d . . . C24C C 0.1304(3) 0.1302(3) 0.08470(14) 0.0268(6) Uani 1 1 d . . . H24C H 0.1301 0.1020 0.0407 0.032 Uiso 1 1 calc R . . C25C C 0.0266(3) 0.1296(3) 0.11469(15) 0.0279(6) Uani 1 1 d . . . H25C H -0.0613 0.1002 0.0948 0.034 Uiso 1 1 calc R . . C26C C -0.0042(3) 0.2114(3) 0.22386(15) 0.0256(6) Uani 1 1 d . . . H26E H 0.0377 0.2143 0.2690 0.031 Uiso 1 1 calc R . . H26F H -0.0924 0.1501 0.2189 0.031 Uiso 1 1 calc R . . C31C C -0.0156(3) 0.3294(3) 0.21484(15) 0.0259(6) Uani 1 1 d . . . C32C C 0.0286(3) 0.3941(3) 0.16346(16) 0.0317(7) Uani 1 1 d . . . H32C H 0.0690 0.3653 0.1317 0.038 Uiso 1 1 calc R . . C33C C 0.0134(4) 0.5010(3) 0.15880(19) 0.0405(8) Uani 1 1 d . . . H33C H 0.0427 0.5446 0.1234 0.049 Uiso 1 1 calc R . . C34C C -0.0440(4) 0.5449(3) 0.2052(2) 0.0429(8) Uani 1 1 d . . . H34C H -0.0528 0.6187 0.2019 0.051 Uiso 1 1 calc R . . C35C C -0.0881(3) 0.4813(3) 0.25617(18) 0.0382(8) Uani 1 1 d . . . H35C H -0.1274 0.5110 0.2881 0.046 Uiso 1 1 calc R . . C36C C -0.0750(3) 0.3739(3) 0.26063(16) 0.0319(7) Uani 1 1 d . . . H36C H -0.1069 0.3297 0.2954 0.038 Uiso 1 1 calc R . . P1 P 0.64219(10) 0.90112(10) 0.11237(5) 0.0440(2) Uani 1 1 d . . . F1 F 0.5713(3) 0.9633(2) 0.06322(15) 0.0680(7) Uani 1 1 d . . . F2 F 0.5377(3) 0.8862(3) 0.16133(14) 0.0656(7) Uani 1 1 d . . . F3 F 0.5500(2) 0.7795(2) 0.07111(12) 0.0534(6) Uani 1 1 d . . . F4 F 0.7295(3) 1.0228(3) 0.15095(18) 0.1153(16) Uani 1 1 d . . . F5 F 0.7478(2) 0.9121(3) 0.06339(11) 0.0602(7) Uani 1 1 d . . . F6 F 0.7064(4) 0.8308(5) 0.15656(15) 0.1113(16) Uani 1 1 d . . . P2 P 0.06901(8) 0.76910(7) 0.42392(4) 0.02873(17) Uani 1 1 d . . . F7 F 0.1646(2) 0.7406(2) 0.37890(13) 0.0539(6) Uani 1 1 d . . . F8 F 0.1104(2) 0.89889(16) 0.40301(10) 0.0388(5) Uani 1 1 d . . . F9 F -0.0326(3) 0.7923(3) 0.46543(15) 0.0713(9) Uani 1 1 d . . . F10 F 0.1796(3) 0.8129(2) 0.48404(13) 0.0682(8) Uani 1 1 d . . . F11 F 0.0276(2) 0.63893(19) 0.44555(14) 0.0584(7) Uani 1 1 d . . . F12 F -0.0416(3) 0.7243(2) 0.36196(14) 0.0657(7) Uani 1 1 d . . . C2S C 0.2831(5) 0.4682(4) 1.0003(2) 0.0616(12) Uani 1 1 d . . . C3S C 0.2302(6) 0.5617(5) 1.0073(3) 0.0755(15) Uani 1 1 d . . . H3S1 H 0.1950 0.5598 1.0490 0.113 Uiso 1 1 calc R . . H3S2 H 0.1611 0.5493 0.9710 0.113 Uiso 1 1 calc R . . H3S3 H 0.2994 0.6383 1.0066 0.113 Uiso 1 1 calc R . . C1S C 0.3499(6) 0.4602(5) 0.9421(3) 0.0790(16) Uani 1 1 d . . . H1S1 H 0.3790 0.3937 0.9436 0.118 Uiso 1 1 calc R . . H1S2 H 0.4250 0.5331 0.9426 0.118 Uiso 1 1 calc R . . H1S3 H 0.2895 0.4484 0.9020 0.118 Uiso 1 1 calc R . . O1S O 0.2793(6) 0.4020(3) 1.0421(2) 0.1083(17) Uani 1 1 d . . . C11S C 0.7384(7) 0.8212(6) 0.3116(3) 0.097(2) Uani 1 1 d . . . H11A H 0.6613 0.8288 0.2881 0.146 Uiso 1 1 calc R . . H11B H 0.7150 0.7793 0.3500 0.146 Uiso 1 1 calc R . . H11C H 0.7732 0.7770 0.2824 0.146 Uiso 1 1 calc R . . C12S C 0.8373(4) 0.9388(5) 0.3328(2) 0.0588(12) Uani 1 1 d . . . C13S C 0.8317(6) 0.9901(7) 0.4004(4) 0.100(2) Uani 1 1 d . . . H13D H 0.8893 0.9703 0.4327 0.150 Uiso 1 1 calc R . . H13E H 0.7425 0.9576 0.4107 0.150 Uiso 1 1 calc R . . H13F H 0.8595 1.0758 0.4018 0.150 Uiso 1 1 calc R . . O11S O 0.9217(4) 0.9879(4) 0.3029(2) 0.0900(14) 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 0.01838(12) 0.01517(11) 0.01981(12) 0.00285(8) 0.00367(8) 0.00361(8) N11A 0.0227(12) 0.0183(10) 0.0191(11) 0.0045(8) 0.0034(9) 0.0040(9) C12A 0.0229(13) 0.0178(12) 0.0199(12) 0.0010(10) -0.0004(10) 0.0032(10) C13A 0.0354(17) 0.0224(13) 0.0286(15) 0.0039(11) 0.0048(12) 0.0122(12) C14A 0.048(2) 0.0243(14) 0.0326(16) 0.0079(12) 0.0098(14) 0.0138(14) C15A 0.051(2) 0.0289(16) 0.0308(16) 0.0126(13) 0.0141(15) 0.0117(15) C16A 0.0357(17) 0.0252(14) 0.0261(14) 0.0077(11) 0.0100(12) 0.0072(12) N21A 0.0246(12) 0.0238(11) 0.0204(11) 0.0062(9) 0.0052(9) 0.0062(10) N22A 0.0185(11) 0.0193(10) 0.0197(10) 0.0056(8) 0.0036(8) 0.0041(9) C23A 0.0209(13) 0.0192(12) 0.0208(12) 0.0023(10) 0.0014(10) 0.0053(10) C24A 0.0240(14) 0.0242(13) 0.0244(13) 0.0020(11) 0.0033(11) 0.0094(11) C25A 0.0254(15) 0.0277(14) 0.0237(13) 0.0018(11) 0.0037(11) 0.0090(12) C26A 0.0277(15) 0.0206(13) 0.0214(13) 0.0051(10) 0.0061(11) 0.0056(11) C31A 0.0302(15) 0.0236(13) 0.0220(13) 0.0054(10) 0.0073(11) 0.0080(12) C32A 0.0366(17) 0.0235(14) 0.0380(17) 0.0079(12) 0.0040(14) 0.0092(13) C33A 0.042(2) 0.0364(17) 0.0385(18) 0.0117(14) 0.0019(15) 0.0183(15) C34A 0.0349(18) 0.0443(19) 0.0281(15) 0.0036(13) -0.0015(13) 0.0149(15) C35A 0.0357(18) 0.0337(17) 0.0394(18) -0.0058(14) -0.0044(14) 0.0111(14) C36A 0.0349(17) 0.0274(15) 0.0333(16) 0.0004(12) -0.0009(13) 0.0129(13) N11B 0.0210(11) 0.0225(11) 0.0205(11) 0.0037(9) 0.0051(9) 0.0040(9) C12B 0.0245(14) 0.0267(14) 0.0212(13) 0.0039(11) 0.0043(11) 0.0083(11) C13B 0.0280(16) 0.0386(17) 0.0264(14) 0.0039(12) 0.0010(12) 0.0133(13) C14B 0.0238(15) 0.0441(18) 0.0270(15) 0.0018(13) 0.0000(12) 0.0070(13) C15B 0.0253(15) 0.0292(15) 0.0298(15) -0.0003(12) 0.0022(12) -0.0009(12) C16B 0.0239(14) 0.0227(13) 0.0292(14) 0.0031(11) 0.0044(11) 0.0047(11) N21B 0.0326(14) 0.0158(10) 0.0257(12) 0.0032(9) 0.0049(10) 0.0054(10) N22B 0.0245(12) 0.0172(10) 0.0210(11) 0.0030(8) 0.0055(9) 0.0051(9) C23B 0.0276(15) 0.0261(14) 0.0214(13) 0.0038(11) 0.0027(11) 0.0099(12) C24B 0.0421(19) 0.0295(15) 0.0317(16) 0.0060(12) 0.0000(14) 0.0176(14) C25B 0.0457(19) 0.0212(14) 0.0340(16) 0.0058(12) 0.0027(14) 0.0143(13) C26B 0.0271(15) 0.0186(13) 0.0317(15) 0.0035(11) 0.0094(12) 0.0033(11) C31B 0.0312(16) 0.0157(12) 0.0307(15) 0.0051(11) 0.0038(12) 0.0074(11) C32B 0.0348(18) 0.0247(15) 0.0433(18) 0.0049(13) -0.0001(14) 0.0080(13) C33B 0.052(2) 0.0312(17) 0.045(2) -0.0014(15) -0.0148(17) 0.0129(16) C34B 0.078(3) 0.042(2) 0.0299(17) -0.0034(15) -0.0067(18) 0.029(2) C35B 0.061(2) 0.0423(19) 0.0321(17) 0.0054(14) 0.0117(16) 0.0296(18) C36B 0.0380(17) 0.0267(14) 0.0305(15) 0.0058(12) 0.0056(13) 0.0159(13) N11C 0.0213(12) 0.0189(10) 0.0233(11) 0.0042(9) 0.0052(9) 0.0058(9) C12C 0.0230(14) 0.0169(12) 0.0248(13) 0.0046(10) 0.0038(11) 0.0057(10) C13C 0.0306(16) 0.0276(14) 0.0259(14) 0.0009(11) 0.0055(12) 0.0091(12) C14C 0.0339(17) 0.0346(16) 0.0281(15) 0.0022(12) 0.0106(13) 0.0145(14) C15C 0.0243(15) 0.0386(17) 0.0336(16) 0.0044(13) 0.0076(12) 0.0125(13) C16C 0.0227(14) 0.0312(15) 0.0261(14) 0.0045(11) 0.0040(11) 0.0086(12) N21C 0.0183(11) 0.0225(11) 0.0260(12) 0.0021(9) 0.0002(9) 0.0047(9) N22C 0.0200(11) 0.0167(10) 0.0238(11) 0.0027(8) 0.0036(9) 0.0043(9) C23C 0.0242(14) 0.0186(12) 0.0238(13) 0.0046(10) 0.0043(11) 0.0064(10) C24C 0.0286(15) 0.0239(13) 0.0241(14) 0.0002(11) 0.0008(11) 0.0062(12) C25C 0.0246(15) 0.0270(14) 0.0270(14) 0.0007(11) -0.0017(11) 0.0051(12) C26C 0.0195(13) 0.0263(14) 0.0286(14) 0.0032(11) 0.0048(11) 0.0052(11) C31C 0.0182(13) 0.0272(14) 0.0290(14) -0.0007(11) -0.0009(11) 0.0060(11) C32C 0.0286(16) 0.0326(16) 0.0340(16) 0.0044(13) 0.0048(13) 0.0109(13) C33C 0.0391(19) 0.0380(18) 0.0444(19) 0.0124(15) 0.0043(15) 0.0133(15) C34C 0.0371(19) 0.0324(17) 0.060(2) -0.0001(16) -0.0012(17) 0.0166(15) C35C 0.0289(17) 0.0413(18) 0.0443(19) -0.0063(15) 0.0023(14) 0.0156(14) C36C 0.0231(15) 0.0391(17) 0.0315(16) 0.0003(13) 0.0015(12) 0.0102(13) P1 0.0313(5) 0.0577(6) 0.0373(5) 0.0027(4) 0.0084(4) 0.0091(4) F1 0.082(2) 0.0511(15) 0.0779(19) 0.0170(13) 0.0134(15) 0.0300(14) F2 0.0574(16) 0.0723(17) 0.0671(17) 0.0009(13) 0.0340(13) 0.0181(13) F3 0.0536(14) 0.0488(13) 0.0522(13) 0.0137(11) 0.0146(11) 0.0090(11) F4 0.070(2) 0.117(3) 0.093(2) -0.059(2) 0.0305(18) -0.037(2) F5 0.0332(12) 0.0852(18) 0.0429(12) -0.0096(12) 0.0094(10) 0.0006(12) F6 0.096(3) 0.235(5) 0.0505(17) 0.040(2) 0.0143(17) 0.111(3) P2 0.0285(4) 0.0241(4) 0.0355(4) 0.0088(3) 0.0117(3) 0.0091(3) F7 0.0572(15) 0.0527(13) 0.0645(15) 0.0145(11) 0.0308(12) 0.0280(12) F8 0.0420(11) 0.0267(9) 0.0436(11) 0.0112(8) 0.0053(9) 0.0067(8) F9 0.094(2) 0.0783(18) 0.0871(19) 0.0535(16) 0.0665(17) 0.0638(17) F10 0.088(2) 0.0542(15) 0.0541(15) 0.0032(12) -0.0281(14) 0.0277(14) F11 0.0608(15) 0.0322(11) 0.0943(19) 0.0281(12) 0.0369(14) 0.0212(11) F12 0.0528(15) 0.0513(14) 0.0745(18) -0.0026(12) -0.0178(13) 0.0056(12) C2S 0.078(3) 0.047(2) 0.050(2) 0.0089(19) 0.009(2) 0.011(2) C3S 0.083(4) 0.093(4) 0.064(3) 0.017(3) 0.026(3) 0.043(3) C1S 0.103(5) 0.074(3) 0.073(3) 0.008(3) 0.028(3) 0.043(3) O1S 0.189(5) 0.056(2) 0.073(3) 0.023(2) 0.024(3) 0.032(3) C11S 0.107(5) 0.088(4) 0.084(4) 0.021(3) -0.022(4) 0.027(4) C12S 0.045(2) 0.076(3) 0.064(3) 0.033(2) 0.017(2) 0.026(2) C13S 0.070(4) 0.132(6) 0.109(5) -0.009(4) 0.020(4) 0.052(4) O11S 0.072(2) 0.133(4) 0.095(3) 0.073(3) 0.044(2) 0.055(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 N11A 2.068(2) . ? Ru1 N11B 2.069(2) . ? Ru1 N11C 2.081(2) . ? Ru1 N22B 2.081(2) . ? Ru1 N22A 2.084(2) . ? Ru1 N22C 2.094(2) . ? N11A C16A 1.351(4) . ? N11A C12A 1.355(4) . ? C12A C13A 1.389(4) . ? C12A C23A 1.456(4) . ? C13A C14A 1.389(4) . ? C13A H13A 0.9500 . ? C14A C15A 1.376(5) . ? C14A H14A 0.9500 . ? C15A C16A 1.379(4) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? N21A N22A 1.350(3) . ? N21A C25A 1.364(4) . ? N21A C26A 1.456(4) . ? N22A C23A 1.351(4) . ? C23A C24A 1.400(4) . ? C24A C25A 1.369(4) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? C26A C31A 1.516(4) . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? C31A C36A 1.388(4) . ? C31A C32A 1.390(4) . ? C32A C33A 1.381(5) . ? C32A H32A 0.9500 . ? C33A C34A 1.388(5) . ? C33A H33A 0.9500 . ? C34A C35A 1.370(5) . ? C34A H34A 0.9500 . ? C35A C36A 1.388(5) . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? N11B C16B 1.347(4) . ? N11B C12B 1.365(4) . ? C12B C13B 1.393(4) . ? C12B C23B 1.454(4) . ? C13B C14B 1.380(5) . ? C13B H13B 0.9500 . ? C14B C15B 1.379(5) . ? C14B H14B 0.9500 . ? C15B C16B 1.388(4) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? N21B C25B 1.352(4) . ? N21B N22B 1.357(3) . ? N21B C26B 1.455(4) . ? N22B C23B 1.346(4) . ? C23B C24B 1.399(4) . ? C24B C25B 1.367(5) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? C26B C31B 1.516(4) . ? C26B H26A 0.9900 . ? C26B H26B 0.9900 . ? C31B C36B 1.381(4) . ? C31B C32B 1.398(4) . ? C32B C33B 1.380(5) . ? C32B H32B 0.9500 . ? C33B C34B 1.380(6) . ? C33B H33B 0.9500 . ? C34B C35B 1.389(6) . ? C34B H34B 0.9500 . ? C35B C36B 1.402(5) . ? C35B H35B 0.9500 . ? C36B H36B 0.9500 . ? N11C C16C 1.348(4) . ? N11C C12C 1.358(4) . ? C12C C13C 1.384(4) . ? C12C C23C 1.455(4) . ? C13C C14C 1.384(5) . ? C13C H13C 0.9500 . ? C14C C15C 1.382(5) . ? C14C H14C 0.9500 . ? C15C C16C 1.376(4) . ? C15C H15C 0.9500 . ? C16C H16C 0.9500 . ? N21C N22C 1.358(3) . ? N21C C25C 1.357(4) . ? N21C C26C 1.453(4) . ? N22C C23C 1.343(4) . ? C23C C24C 1.398(4) . ? C24C C25C 1.366(4) . ? C24C H24C 0.9500 . ? C25C H25C 0.9500 . ? C26C C31C 1.518(4) . ? C26C H26E 0.9900 . ? C26C H26F 0.9900 . ? C31C C32C 1.391(4) . ? C31C C36C 1.397(4) . ? C32C C33C 1.387(5) . ? C32C H32C 0.9500 . ? C33C C34C 1.387(5) . ? C33C H33C 0.9500 . ? C34C C35C 1.376(6) . ? C34C H34C 0.9500 . ? C35C C36C 1.383(5) . ? C35C H35C 0.9500 . ? C36C H36C 0.9500 . ? P1 F4 1.565(3) . ? P1 F6 1.580(4) . ? P1 F2 1.589(3) . ? P1 F3 1.600(3) . ? P1 F5 1.605(2) . ? P1 F1 1.613(3) . ? P2 F10 1.572(3) . ? P2 F9 1.580(2) . ? P2 F8 1.5916(19) . ? P2 F7 1.597(2) . ? P2 F12 1.599(3) . ? P2 F11 1.601(2) . ? C2S O1S 1.215(6) . ? C2S C3S 1.470(7) . ? C2S C1S 1.492(7) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C11S C12S 1.471(8) . ? C11S H11A 0.9800 . ? C11S H11B 0.9800 . ? C11S H11C 0.9800 . ? C12S O11S 1.179(5) . ? C12S C13S 1.511(8) . ? C13S H13D 0.9800 . ? C13S H13E 0.9800 . ? C13S H13F 0.9800 . ? 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 N11A Ru1 N11B 95.77(9) . . ? N11A Ru1 N11C 95.08(9) . . ? N11B Ru1 N11C 92.35(9) . . ? N11A Ru1 N22B 173.28(9) . . ? N11B Ru1 N22B 77.52(9) . . ? N11C Ru1 N22B 85.70(9) . . ? N11A Ru1 N22A 77.60(9) . . ? N11B Ru1 N22A 89.62(9) . . ? N11C Ru1 N22A 172.58(9) . . ? N22B Ru1 N22A 101.71(9) . . ? N11A Ru1 N22C 87.27(9) . . ? N11B Ru1 N22C 169.73(9) . . ? N11C Ru1 N22C 77.58(9) . . ? N22B Ru1 N22C 99.41(9) . . ? N22A Ru1 N22C 100.63(9) . . ? C16A N11A C12A 118.3(2) . . ? C16A N11A Ru1 124.8(2) . . ? C12A N11A Ru1 116.84(17) . . ? N11A C12A C13A 122.2(3) . . ? N11A C12A C23A 114.1(2) . . ? C13A C12A C23A 123.7(3) . . ? C12A C13A C14A 118.3(3) . . ? C12A C13A H13A 120.8 . . ? C14A C13A H13A 120.8 . . ? C15A C14A C13A 119.8(3) . . ? C15A C14A H14A 120.1 . . ? C13A C14A H14A 120.1 . . ? C14A C15A C16A 119.0(3) . . ? C14A C15A H15A 120.5 . . ? C16A C15A H15A 120.5 . . ? N11A C16A C15A 122.4(3) . . ? N11A C16A H16A 118.8 . . ? C15A C16A H16A 118.8 . . ? N22A N21A C25A 110.8(2) . . ? N22A N21A C26A 121.6(2) . . ? C25A N21A C26A 126.2(2) . . ? N21A N22A C23A 105.5(2) . . ? N21A N22A Ru1 139.00(18) . . ? C23A N22A Ru1 115.44(17) . . ? N22A C23A C24A 110.9(2) . . ? N22A C23A C12A 116.0(2) . . ? C24A C23A C12A 133.1(3) . . ? C25A C24A C23A 104.9(3) . . ? C25A C24A H24A 127.6 . . ? C23A C24A H24A 127.6 . . ? N21A C25A C24A 108.0(3) . . ? N21A C25A H25A 126.0 . . ? C24A C25A H25A 126.0 . . ? N21A C26A C31A 112.5(2) . . ? N21A C26A H26C 109.1 . . ? C31A C26A H26C 109.1 . . ? N21A C26A H26D 109.1 . . ? C31A C26A H26D 109.1 . . ? H26C C26A H26D 107.8 . . ? C36A C31A C32A 118.3(3) . . ? C36A C31A C26A 121.9(3) . . ? C32A C31A C26A 119.8(3) . . ? C33A C32A C31A 120.7(3) . . ? C33A C32A H32A 119.6 . . ? C31A C32A H32A 119.6 . . ? C32A C33A C34A 120.5(3) . . ? C32A C33A H33A 119.8 . . ? C34A C33A H33A 119.8 . . ? C35A C34A C33A 119.1(3) . . ? C35A C34A H34A 120.5 . . ? C33A C34A H34A 120.5 . . ? C34A C35A C36A 120.7(3) . . ? C34A C35A H35A 119.6 . . ? C36A C35A H35A 119.6 . . ? C35A C36A C31A 120.7(3) . . ? C35A C36A H36A 119.7 . . ? C31A C36A H36A 119.7 . . ? C16B N11B C12B 118.0(3) . . ? C16B N11B Ru1 125.8(2) . . ? C12B N11B Ru1 116.20(18) . . ? N11B C12B C13B 122.2(3) . . ? N11B C12B C23B 113.9(3) . . ? C13B C12B C23B 124.0(3) . . ? C14B C13B C12B 119.0(3) . . ? C14B C13B H13B 120.5 . . ? C12B C13B H13B 120.5 . . ? C15B C14B C13B 119.1(3) . . ? C15B C14B H14B 120.5 . . ? C13B C14B H14B 120.5 . . ? C14B C15B C16B 119.8(3) . . ? C14B C15B H15B 120.1 . . ? C16B C15B H15B 120.1 . . ? N11B C16B C15B 122.1(3) . . ? N11B C16B H16B 119.0 . . ? C15B C16B H16B 119.0 . . ? C25B N21B N22B 110.2(3) . . ? C25B N21B C26B 127.4(2) . . ? N22B N21B C26B 122.3(2) . . ? C23B N22B N21B 105.8(2) . . ? C23B N22B Ru1 115.03(18) . . ? N21B N22B Ru1 138.71(19) . . ? N22B C23B C24B 110.6(3) . . ? N22B C23B C12B 116.0(3) . . ? C24B C23B C12B 133.2(3) . . ? C25B C24B C23B 104.7(3) . . ? C25B C24B H24B 127.6 . . ? C23B C24B H24B 127.6 . . ? N21B C25B C24B 108.6(3) . . ? N21B C25B H25B 125.7 . . ? C24B C25B H25B 125.7 . . ? N21B C26B C31B 114.7(2) . . ? N21B C26B H26A 108.6 . . ? C31B C26B H26A 108.6 . . ? N21B C26B H26B 108.6 . . ? C31B C26B H26B 108.6 . . ? H26A C26B H26B 107.6 . . ? C36B C31B C32B 119.8(3) . . ? C36B C31B C26B 123.1(3) . . ? C32B C31B C26B 117.1(3) . . ? C33B C32B C31B 120.1(4) . . ? C33B C32B H32B 119.9 . . ? C31B C32B H32B 119.9 . . ? C34B C33B C32B 120.3(4) . . ? C34B C33B H33B 119.9 . . ? C32B C33B H33B 119.9 . . ? C33B C34B C35B 120.2(3) . . ? C33B C34B H34B 119.9 . . ? C35B C34B H34B 119.9 . . ? C34B C35B C36B 119.7(4) . . ? C34B C35B H35B 120.2 . . ? C36B C35B H35B 120.2 . . ? C31B C36B C35B 119.9(3) . . ? C31B C36B H36B 120.1 . . ? C35B C36B H36B 120.1 . . ? C16C N11C C12C 117.6(2) . . ? C16C N11C Ru1 126.1(2) . . ? C12C N11C Ru1 116.28(19) . . ? N11C C12C C13C 122.3(3) . . ? N11C C12C C23C 114.3(2) . . ? C13C C12C C23C 123.4(3) . . ? C14C C13C C12C 119.1(3) . . ? C14C C13C H13C 120.4 . . ? C12C C13C H13C 120.4 . . ? C13C C14C C15C 118.8(3) . . ? C13C C14C H14C 120.6 . . ? C15C C14C H14C 120.6 . . ? C16C C15C C14C 119.2(3) . . ? C16C C15C H15C 120.4 . . ? C14C C15C H15C 120.4 . . ? N11C C16C C15C 122.9(3) . . ? N11C C16C H16C 118.6 . . ? C15C C16C H16C 118.6 . . ? N22C N21C C25C 110.2(2) . . ? N22C N21C C26C 122.2(2) . . ? C25C N21C C26C 126.8(3) . . ? C23C N22C N21C 105.5(2) . . ? C23C N22C Ru1 115.15(19) . . ? N21C N22C Ru1 139.29(18) . . ? N22C C23C C24C 111.2(3) . . ? N22C C23C C12C 116.6(2) . . ? C24C C23C C12C 132.2(3) . . ? C25C C24C C23C 104.6(3) . . ? C25C C24C H24C 127.7 . . ? C23C C24C H24C 127.7 . . ? N21C C25C C24C 108.6(3) . . ? N21C C25C H25C 125.7 . . ? C24C C25C H25C 125.7 . . ? N21C C26C C31C 113.4(2) . . ? N21C C26C H26E 108.9 . . ? C31C C26C H26E 108.9 . . ? N21C C26C H26F 108.9 . . ? C31C C26C H26F 108.9 . . ? H26E C26C H26F 107.7 . . ? C32C C31C C36C 118.8(3) . . ? C32C C31C C26C 123.6(3) . . ? C36C C31C C26C 117.6(3) . . ? C33C C32C C31C 119.7(3) . . ? C33C C32C H32C 120.1 . . ? C31C C32C H32C 120.1 . . ? C34C C33C C32C 120.8(3) . . ? C34C C33C H33C 119.6 . . ? C32C C33C H33C 119.6 . . ? C35C C34C C33C 119.8(3) . . ? C35C C34C H34C 120.1 . . ? C33C C34C H34C 120.1 . . ? C34C C35C C36C 119.7(3) . . ? C34C C35C H35C 120.1 . . ? C36C C35C H35C 120.1 . . ? C35C C36C C31C 121.1(3) . . ? C35C C36C H36C 119.4 . . ? C31C C36C H36C 119.4 . . ? F4 P1 F6 93.2(3) . . ? F4 P1 F2 90.22(16) . . ? F6 P1 F2 89.18(17) . . ? F4 P1 F3 177.6(2) . . ? F6 P1 F3 89.2(2) . . ? F2 P1 F3 89.73(14) . . ? F4 P1 F5 90.90(16) . . ? F6 P1 F5 89.28(17) . . ? F2 P1 F5 178.15(18) . . ? F3 P1 F5 89.21(13) . . ? F4 P1 F1 91.3(2) . . ? F6 P1 F1 175.4(2) . . ? F2 P1 F1 91.81(17) . . ? F3 P1 F1 86.32(15) . . ? F5 P1 F1 89.64(16) . . ? F10 P2 F9 92.41(18) . . ? F10 P2 F8 90.52(13) . . ? F9 P2 F8 90.32(13) . . ? F10 P2 F7 90.82(16) . . ? F9 P2 F7 176.57(18) . . ? F8 P2 F7 90.79(12) . . ? F10 P2 F12 178.97(18) . . ? F9 P2 F12 88.62(18) . . ? F8 P2 F12 89.39(13) . . ? F7 P2 F12 88.15(16) . . ? F10 P2 F11 89.13(15) . . ? F9 P2 F11 89.42(13) . . ? F8 P2 F11 179.55(14) . . ? F7 P2 F11 89.49(13) . . ? F12 P2 F11 90.97(15) . . ? O1S C2S C3S 121.7(5) . . ? O1S C2S C1S 119.8(5) . . ? C3S C2S C1S 118.4(4) . . ? C2S C3S H3S1 109.5 . . ? C2S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C2S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C12S C11S H11A 109.5 . . ? C12S C11S H11B 109.5 . . ? H11A C11S H11B 109.5 . . ? C12S C11S H11C 109.5 . . ? H11A C11S H11C 109.5 . . ? H11B C11S H11C 109.5 . . ? O11S C12S C11S 124.4(6) . . ? O11S C12S C13S 120.7(6) . . ? C11S C12S C13S 114.7(5) . . ? C12S C13S H13D 109.5 . . ? C12S C13S H13E 109.5 . . ? H13D C13S H13E 109.5 . . ? C12S C13S H13F 109.5 . . ? H13D C13S H13F 109.5 . . ? H13E C13S H13F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11B Ru1 N11A C16A 92.2(2) . . . . ? N11C Ru1 N11A C16A -0.7(3) . . . . ? N22B Ru1 N11A C16A 95.7(8) . . . . ? N22A Ru1 N11A C16A -179.5(3) . . . . ? N22C Ru1 N11A C16A -78.0(2) . . . . ? N11B Ru1 N11A C12A -89.6(2) . . . . ? N11C Ru1 N11A C12A 177.5(2) . . . . ? N22B Ru1 N11A C12A -86.0(8) . . . . ? N22A Ru1 N11A C12A -1.22(19) . . . . ? N22C Ru1 N11A C12A 100.3(2) . . . . ? C16A N11A C12A C13A -0.2(4) . . . . ? Ru1 N11A C12A C13A -178.6(2) . . . . ? C16A N11A C12A C23A 179.6(3) . . . . ? Ru1 N11A C12A C23A 1.2(3) . . . . ? N11A C12A C13A C14A 0.0(5) . . . . ? C23A C12A C13A C14A -179.8(3) . . . . ? C12A C13A C14A C15A 0.0(5) . . . . ? C13A C14A C15A C16A 0.2(5) . . . . ? C12A N11A C16A C15A 0.4(5) . . . . ? Ru1 N11A C16A C15A 178.6(3) . . . . ? C14A C15A C16A N11A -0.4(5) . . . . ? C25A N21A N22A C23A -0.5(3) . . . . ? C26A N21A N22A C23A -167.8(2) . . . . ? C25A N21A N22A Ru1 -176.4(2) . . . . ? C26A N21A N22A Ru1 16.3(4) . . . . ? N11A Ru1 N22A N21A 176.7(3) . . . . ? N11B Ru1 N22A N21A -87.3(3) . . . . ? N11C Ru1 N22A N21A 167.2(6) . . . . ? N22B Ru1 N22A N21A -10.2(3) . . . . ? N22C Ru1 N22A N21A 91.9(3) . . . . ? N11A Ru1 N22A C23A 1.02(19) . . . . ? N11B Ru1 N22A C23A 97.0(2) . . . . ? N11C Ru1 N22A C23A -8.5(8) . . . . ? N22B Ru1 N22A C23A 174.18(19) . . . . ? N22C Ru1 N22A C23A -83.8(2) . . . . ? N21A N22A C23A C24A 0.2(3) . . . . ? Ru1 N22A C23A C24A 177.22(18) . . . . ? N21A N22A C23A C12A -177.7(2) . . . . ? Ru1 N22A C23A C12A -0.7(3) . . . . ? N11A C12A C23A N22A -0.3(4) . . . . ? C13A C12A C23A N22A 179.5(3) . . . . ? N11A C12A C23A C24A -177.7(3) . . . . ? C13A C12A C23A C24A 2.1(5) . . . . ? N22A C23A C24A C25A 0.2(3) . . . . ? C12A C23A C24A C25A 177.7(3) . . . . ? N22A N21A C25A C24A 0.7(3) . . . . ? C26A N21A C25A C24A 167.3(3) . . . . ? C23A C24A C25A N21A -0.5(3) . . . . ? N22A N21A C26A C31A 78.9(3) . . . . ? C25A N21A C26A C31A -86.4(3) . . . . ? N21A C26A C31A C36A 20.8(4) . . . . ? N21A C26A C31A C32A -160.2(3) . . . . ? C36A C31A C32A C33A -0.4(5) . . . . ? C26A C31A C32A C33A -179.4(3) . . . . ? C31A C32A C33A C34A 0.5(5) . . . . ? C32A C33A C34A C35A 0.0(5) . . . . ? C33A C34A C35A C36A -0.7(6) . . . . ? C34A C35A C36A C31A 0.9(5) . . . . ? C32A C31A C36A C35A -0.3(5) . . . . ? C26A C31A C36A C35A 178.7(3) . . . . ? N11A Ru1 N11B C16B 4.6(2) . . . . ? N11C Ru1 N11B C16B 100.0(2) . . . . ? N22B Ru1 N11B C16B -174.9(2) . . . . ? N22A Ru1 N11B C16B -72.9(2) . . . . ? N22C Ru1 N11B C16B 111.5(5) . . . . ? N11A Ru1 N11B C12B -171.9(2) . . . . ? N11C Ru1 N11B C12B -76.6(2) . . . . ? N22B Ru1 N11B C12B 8.52(19) . . . . ? N22A Ru1 N11B C12B 110.6(2) . . . . ? N22C Ru1 N11B C12B -65.1(6) . . . . ? C16B N11B C12B C13B 0.0(4) . . . . ? Ru1 N11B C12B C13B 176.8(2) . . . . ? C16B N11B C12B C23B 178.0(3) . . . . ? Ru1 N11B C12B C23B -5.2(3) . . . . ? N11B C12B C13B C14B -0.5(5) . . . . ? C23B C12B C13B C14B -178.3(3) . . . . ? C12B C13B C14B C15B 0.3(5) . . . . ? C13B C14B C15B C16B 0.5(5) . . . . ? C12B N11B C16B C15B 0.8(4) . . . . ? Ru1 N11B C16B C15B -175.7(2) . . . . ? C14B C15B C16B N11B -1.0(5) . . . . ? C25B N21B N22B C23B -0.5(3) . . . . ? C26B N21B N22B C23B 175.7(3) . . . . ? C25B N21B N22B Ru1 170.6(2) . . . . ? C26B N21B N22B Ru1 -13.1(4) . . . . ? N11A Ru1 N22B C23B -14.3(9) . . . . ? N11B Ru1 N22B C23B -10.7(2) . . . . ? N11C Ru1 N22B C23B 82.6(2) . . . . ? N22A Ru1 N22B C23B -97.7(2) . . . . ? N22C Ru1 N22B C23B 159.3(2) . . . . ? N11A Ru1 N22B N21B 175.1(7) . . . . ? N11B Ru1 N22B N21B 178.7(3) . . . . ? N11C Ru1 N22B N21B -87.9(3) . . . . ? N22A Ru1 N22B N21B 91.7(3) . . . . ? N22C Ru1 N22B N21B -11.3(3) . . . . ? N21B N22B C23B C24B 1.0(3) . . . . ? Ru1 N22B C23B C24B -172.6(2) . . . . ? N21B N22B C23B C12B -175.0(2) . . . . ? Ru1 N22B C23B C12B 11.4(3) . . . . ? N11B C12B C23B N22B -4.2(4) . . . . ? C13B C12B C23B N22B 173.8(3) . . . . ? N11B C12B C23B C24B -179.1(3) . . . . ? C13B C12B C23B C24B -1.1(5) . . . . ? N22B C23B C24B C25B -1.1(4) . . . . ? C12B C23B C24B C25B 174.0(3) . . . . ? N22B N21B C25B C24B -0.1(4) . . . . ? C26B N21B C25B C24B -176.1(3) . . . . ? C23B C24B C25B N21B 0.7(4) . . . . ? C25B N21B C26B C31B -80.3(4) . . . . ? N22B N21B C26B C31B 104.1(3) . . . . ? N21B C26B C31B C36B -2.1(4) . . . . ? N21B C26B C31B C32B 178.2(2) . . . . ? C36B C31B C32B C33B -0.2(5) . . . . ? C26B C31B C32B C33B 179.5(3) . . . . ? C31B C32B C33B C34B 0.3(5) . . . . ? C32B C33B C34B C35B -0.3(6) . . . . ? C33B C34B C35B C36B 0.2(5) . . . . ? C32B C31B C36B C35B 0.1(4) . . . . ? C26B C31B C36B C35B -179.6(3) . . . . ? C34B C35B C36B C31B -0.1(5) . . . . ? N11A Ru1 N11C C16C 93.1(2) . . . . ? N11B Ru1 N11C C16C -2.9(2) . . . . ? N22B Ru1 N11C C16C -80.2(2) . . . . ? N22A Ru1 N11C C16C 102.5(7) . . . . ? N22C Ru1 N11C C16C 179.2(2) . . . . ? N11A Ru1 N11C C12C -88.7(2) . . . . ? N11B Ru1 N11C C12C 175.28(19) . . . . ? N22B Ru1 N11C C12C 98.0(2) . . . . ? N22A Ru1 N11C C12C -79.4(7) . . . . ? N22C Ru1 N11C C12C -2.64(18) . . . . ? C16C N11C C12C C13C 1.4(4) . . . . ? Ru1 N11C C12C C13C -176.9(2) . . . . ? C16C N11C C12C C23C -178.8(2) . . . . ? Ru1 N11C C12C C23C 2.9(3) . . . . ? N11C C12C C13C C14C -0.3(4) . . . . ? C23C C12C C13C C14C 180.0(3) . . . . ? C12C C13C C14C C15C -1.0(5) . . . . ? C13C C14C C15C C16C 1.1(5) . . . . ? C12C N11C C16C C15C -1.3(4) . . . . ? Ru1 N11C C16C C15C 176.8(2) . . . . ? C14C C15C C16C N11C 0.0(5) . . . . ? C25C N21C N22C C23C -0.2(3) . . . . ? C26C N21C N22C C23C -170.3(2) . . . . ? C25C N21C N22C Ru1 -177.1(2) . . . . ? C26C N21C N22C Ru1 12.8(4) . . . . ? N11A Ru1 N22C C23C 97.78(19) . . . . ? N11B Ru1 N22C C23C -9.8(6) . . . . ? N11C Ru1 N22C C23C 1.96(18) . . . . ? N22B Ru1 N22C C23C -81.5(2) . . . . ? N22A Ru1 N22C C23C 174.62(18) . . . . ? N11A Ru1 N22C N21C -85.5(3) . . . . ? N11B Ru1 N22C N21C 166.9(4) . . . . ? N11C Ru1 N22C N21C 178.6(3) . . . . ? N22B Ru1 N22C N21C 95.2(3) . . . . ? N22A Ru1 N22C N21C -8.7(3) . . . . ? N21C N22C C23C C24C 0.2(3) . . . . ? Ru1 N22C C23C C24C 177.94(18) . . . . ? N21C N22C C23C C12C -178.8(2) . . . . ? Ru1 N22C C23C C12C -1.1(3) . . . . ? N11C C12C C23C N22C -1.2(4) . . . . ? C13C C12C C23C N22C 178.6(3) . . . . ? N11C C12C C23C C24C -179.9(3) . . . . ? C13C C12C C23C C24C -0.2(5) . . . . ? N22C C23C C24C C25C -0.1(3) . . . . ? C12C C23C C24C C25C 178.7(3) . . . . ? N22C N21C C25C C24C 0.1(3) . . . . ? C26C N21C C25C C24C 169.7(3) . . . . ? C23C C24C C25C N21C 0.0(3) . . . . ? N22C N21C C26C C31C 87.8(3) . . . . ? C25C N21C C26C C31C -80.6(3) . . . . ? N21C C26C C31C C32C 6.3(4) . . . . ? N21C C26C C31C C36C -174.3(2) . . . . ? C36C C31C C32C C33C 0.2(5) . . . . ? C26C C31C C32C C33C 179.6(3) . . . . ? C31C C32C C33C C34C 0.8(5) . . . . ? C32C C33C C34C C35C -0.9(6) . . . . ? C33C C34C C35C C36C -0.1(5) . . . . ? C34C C35C C36C C31C 1.1(5) . . . . ? C32C C31C C36C C35C -1.1(5) . . . . ? C26C C31C C36C C35C 179.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.678 _refine_diff_density_min -0.787 _refine_diff_density_rms 0.098 _database_code_depnum_ccdc_archive 'CCDC 959999' ####################################################################### # # 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_imw1781p-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H39 N9 Ru, 2(F6 P), C3 H6 O' _chemical_formula_sum 'C48 H45 F12 N9 O P2 Ru' _chemical_formula_weight 1154.94 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7741(3) _cell_length_b 12.1017(3) _cell_length_c 17.9981(4) _cell_angle_alpha 99.8650(10) _cell_angle_beta 96.3270(10) _cell_angle_gamma 107.5040(10) _cell_volume 2373.61(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9964 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 0.494 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8659 _exptl_absorpt_correction_T_max 0.9431 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37534 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.52 _reflns_number_total 10838 _reflns_number_gt 10362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _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. The structure was solved by direct methods. There were no particular problems encountered in the structure refinement. The asymmetric unit contains a full complex cation, two PF6 anions and an acetone solvent molecule. ; _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^)+(0.0331P)^2^+1.3024P] 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 10838 _refine_ls_number_parameters 660 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.002 _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 0.140797(9) 0.436292(9) 0.275654(6) 0.01749(4) Uani 1 1 d . . . N11A N 0.15366(11) 0.41560(11) 0.38782(7) 0.0212(2) Uani 1 1 d . . . C12A C 0.04806(14) 0.38801(12) 0.41573(8) 0.0225(3) Uani 1 1 d . . . C13A C 0.04361(16) 0.36891(14) 0.48939(9) 0.0282(3) Uani 1 1 d . . . H13A H -0.0312 0.3495 0.5075 0.034 Uiso 1 1 calc R . . C14A C 0.14859(17) 0.37826(14) 0.53600(9) 0.0308(3) Uani 1 1 d . . . H14A H 0.1471 0.3657 0.5866 0.037 Uiso 1 1 calc R . . C15A C 0.25663(16) 0.40639(15) 0.50791(9) 0.0301(3) Uani 1 1 d . . . H15A H 0.3301 0.4131 0.5390 0.036 Uiso 1 1 calc R . . C16A C 0.25577(15) 0.42443(14) 0.43401(9) 0.0265(3) Uani 1 1 d . . . H16A H 0.3299 0.4438 0.4151 0.032 Uiso 1 1 calc R . . N21A N -0.14664(11) 0.37627(11) 0.24964(8) 0.0242(3) Uani 1 1 d . . . N22A N -0.03736(11) 0.39024(10) 0.29025(7) 0.0211(2) Uani 1 1 d . . . C23A C -0.05703(14) 0.37643(12) 0.36100(9) 0.0233(3) Uani 1 1 d . . . C24A C -0.18009(14) 0.35265(14) 0.36532(10) 0.0297(3) Uani 1 1 d . . . H24A H -0.2179 0.3396 0.4085 0.036 Uiso 1 1 calc R . . C25A C -0.23362(14) 0.35236(14) 0.29405(10) 0.0299(3) Uani 1 1 d . . . H25A H -0.3174 0.3379 0.2781 0.036 Uiso 1 1 calc R . . C26A C -0.16684(14) 0.36156(13) 0.16709(9) 0.0269(3) Uani 1 1 d . . . H26A H -0.0959 0.4154 0.1520 0.032 Uiso 1 1 calc R . . H26B H -0.2380 0.3849 0.1512 0.032 Uiso 1 1 calc R . . C31A C -0.18771(14) 0.23544(14) 0.12514(9) 0.0261(3) Uani 1 1 d . . . C32A C -0.20255(15) 0.14264(14) 0.16315(10) 0.0286(3) Uani 1 1 d . . . H32A H -0.1948 0.1582 0.2174 0.034 Uiso 1 1 calc R . . C33A C -0.22869(16) 0.02713(15) 0.12218(11) 0.0351(4) Uani 1 1 d . . . H33A H -0.2385 -0.0359 0.1485 0.042 Uiso 1 1 calc R . . C34A C -0.24048(17) 0.00363(17) 0.04322(12) 0.0401(4) Uani 1 1 d . . . H34A H -0.2588 -0.0755 0.0153 0.048 Uiso 1 1 calc R . . C35A C -0.22548(18) 0.09592(19) 0.00492(11) 0.0425(4) Uani 1 1 d . . . H35A H -0.2337 0.0801 -0.0493 0.051 Uiso 1 1 calc R . . C36A C -0.19844(17) 0.21131(17) 0.04590(10) 0.0359(4) Uani 1 1 d . . . H36A H -0.1872 0.2744 0.0196 0.043 Uiso 1 1 calc R . . N11B N 0.10917(11) 0.25797(11) 0.22854(7) 0.0223(2) Uani 1 1 d . . . C12B C 0.10536(14) 0.22888(13) 0.15166(9) 0.0246(3) Uani 1 1 d . . . C13B C 0.08439(16) 0.11312(15) 0.11313(10) 0.0307(3) Uani 1 1 d . . . H13B H 0.0843 0.0953 0.0596 0.037 Uiso 1 1 calc R . . C14B C 0.06356(17) 0.02396(15) 0.15397(11) 0.0343(4) Uani 1 1 d . . . H14B H 0.0486 -0.0560 0.1288 0.041 Uiso 1 1 calc R . . C15B C 0.06477(16) 0.05272(15) 0.23174(11) 0.0331(4) Uani 1 1 d . . . H15B H 0.0495 -0.0075 0.2605 0.040 Uiso 1 1 calc R . . C16B C 0.08838(14) 0.16960(14) 0.26731(10) 0.0273(3) Uani 1 1 d . . . H16B H 0.0901 0.1887 0.3210 0.033 Uiso 1 1 calc R . . N21B N 0.13306(12) 0.50927(11) 0.11171(7) 0.0244(3) Uani 1 1 d . . . N22B N 0.12592(11) 0.43191(11) 0.15879(7) 0.0208(2) Uani 1 1 d . . . C23B C 0.12090(14) 0.32878(13) 0.11426(9) 0.0236(3) Uani 1 1 d . . . C24B C 0.12714(15) 0.34001(15) 0.03841(9) 0.0293(3) Uani 1 1 d . . . H24B H 0.1263 0.2808 -0.0040 0.035 Uiso 1 1 calc R . . C25B C 0.13471(15) 0.45551(15) 0.03917(9) 0.0297(3) Uani 1 1 d . . . H25B H 0.1402 0.4918 -0.0037 0.036 Uiso 1 1 calc R . . C26B C 0.12654(14) 0.62767(13) 0.13726(9) 0.0244(3) Uani 1 1 d . . . H26C H 0.0812 0.6268 0.1804 0.029 Uiso 1 1 calc R . . H26D H 0.0798 0.6468 0.0950 0.029 Uiso 1 1 calc R . . C31B C 0.24723(14) 0.72564(13) 0.16258(8) 0.0236(3) Uani 1 1 d . . . C32B C 0.24480(15) 0.83670(14) 0.19763(9) 0.0287(3) Uani 1 1 d . . . H32B H 0.1697 0.8473 0.2047 0.034 Uiso 1 1 calc R . . C33B C 0.35081(17) 0.93179(15) 0.22220(10) 0.0354(4) Uani 1 1 d . . . H33B H 0.3485 1.0072 0.2461 0.042 Uiso 1 1 calc R . . C34B C 0.46043(17) 0.91627(17) 0.21167(11) 0.0384(4) Uani 1 1 d . . . H34B H 0.5333 0.9814 0.2280 0.046 Uiso 1 1 calc R . . C35B C 0.46378(16) 0.80636(17) 0.17748(11) 0.0369(4) Uani 1 1 d . . . H35B H 0.5391 0.7958 0.1709 0.044 Uiso 1 1 calc R . . C36B C 0.35656(15) 0.71049(15) 0.15247(10) 0.0297(3) Uani 1 1 d . . . H36B H 0.3590 0.6351 0.1286 0.036 Uiso 1 1 calc R . . N11C N 0.17598(11) 0.61650(11) 0.32071(7) 0.0195(2) Uani 1 1 d . . . C12C C 0.29489(13) 0.68455(13) 0.34036(8) 0.0216(3) Uani 1 1 d . . . C13C C 0.33160(15) 0.80285(14) 0.37711(9) 0.0269(3) Uani 1 1 d . . . H13C H 0.4151 0.8477 0.3909 0.032 Uiso 1 1 calc R . . C14C C 0.24462(16) 0.85509(14) 0.39350(9) 0.0301(3) Uani 1 1 d . . . H14C H 0.2676 0.9361 0.4189 0.036 Uiso 1 1 calc R . . C15C C 0.12366(15) 0.78701(14) 0.37221(9) 0.0284(3) Uani 1 1 d . . . H15C H 0.0626 0.8212 0.3821 0.034 Uiso 1 1 calc R . . C16C C 0.09253(14) 0.66874(13) 0.33636(8) 0.0234(3) Uani 1 1 d . . . H16C H 0.0094 0.6227 0.3223 0.028 Uiso 1 1 calc R . . N21C N 0.42019(12) 0.46616(12) 0.26923(8) 0.0265(3) Uani 1 1 d . . . N22C N 0.32706(11) 0.50546(11) 0.28535(7) 0.0215(2) Uani 1 1 d . . . C23C C 0.37751(13) 0.62120(13) 0.31851(8) 0.0230(3) Uani 1 1 d . . . C24C C 0.50330(14) 0.65633(16) 0.32336(9) 0.0301(3) Uani 1 1 d . . . H24C H 0.5601 0.7331 0.3441 0.036 Uiso 1 1 calc R . . C25C C 0.52650(14) 0.55624(17) 0.29190(10) 0.0322(4) Uani 1 1 d . . . H25C H 0.6041 0.5506 0.2867 0.039 Uiso 1 1 calc R . . C26C C 0.40450(15) 0.34103(15) 0.24251(10) 0.0299(3) Uani 1 1 d . . . H26E H 0.3181 0.2946 0.2383 0.036 Uiso 1 1 calc R . . H26F H 0.4514 0.3157 0.2814 0.036 Uiso 1 1 calc R . . C31C C 0.44324(14) 0.31117(14) 0.16629(9) 0.0276(3) Uani 1 1 d . . . C32C C 0.43892(18) 0.37556(18) 0.10990(11) 0.0394(4) Uani 1 1 d . . . H32C H 0.4143 0.4438 0.1190 0.047 Uiso 1 1 calc R . . C33C C 0.4710(2) 0.3393(2) 0.03991(12) 0.0498(5) Uani 1 1 d . . . H33C H 0.4680 0.3831 0.0011 0.060 Uiso 1 1 calc R . . C34C C 0.5070(2) 0.2405(2) 0.02645(11) 0.0469(5) Uani 1 1 d . . . H34C H 0.5293 0.2168 -0.0214 0.056 Uiso 1 1 calc R . . C35C C 0.51088(17) 0.17597(17) 0.08225(11) 0.0400(4) Uani 1 1 d . . . H35C H 0.5352 0.1075 0.0729 0.048 Uiso 1 1 calc R . . C36C C 0.47907(15) 0.21154(15) 0.15216(10) 0.0319(3) Uani 1 1 d . . . H36C H 0.4819 0.1672 0.1907 0.038 Uiso 1 1 calc R . . P1 P 0.80404(4) 0.70003(3) 0.18616(2) 0.02480(8) Uani 1 1 d . . . F1 F 0.80133(10) 0.62375(10) 0.25130(6) 0.0402(2) Uani 1 1 d . . . F2 F 0.84277(12) 0.60443(10) 0.13051(7) 0.0480(3) Uani 1 1 d . . . F3 F 0.76626(13) 0.79580(12) 0.24094(7) 0.0523(3) Uani 1 1 d . . . F4 F 0.80915(11) 0.77567(9) 0.12119(6) 0.0408(3) Uani 1 1 d . . . F5 F 0.94356(10) 0.77130(11) 0.21921(8) 0.0504(3) Uani 1 1 d . . . F6 F 0.66614(11) 0.62842(13) 0.15321(7) 0.0545(3) Uani 1 1 d . . . P2 P 0.48833(4) 0.21675(4) 0.42692(2) 0.02655(9) Uani 1 1 d . . . F7 F 0.62420(9) 0.26552(10) 0.47249(6) 0.0387(2) Uani 1 1 d . . . F8 F 0.35300(9) 0.16930(11) 0.38013(7) 0.0454(3) Uani 1 1 d . . . F9 F 0.49678(12) 0.34850(10) 0.41890(7) 0.0474(3) Uani 1 1 d . . . F10 F 0.48043(12) 0.08567(11) 0.43456(8) 0.0520(3) Uani 1 1 d . . . F11 F 0.43919(11) 0.23659(14) 0.50556(7) 0.0556(3) Uani 1 1 d . . . F12 F 0.53770(10) 0.19668(10) 0.34757(6) 0.0378(2) Uani 1 1 d . . . C1S C 0.7310(3) 1.0229(2) 0.37071(16) 0.0632(7) Uani 1 1 d . . . H1S1 H 0.7500 1.0951 0.3502 0.095 Uiso 1 1 calc R . . H1S2 H 0.6807 1.0292 0.4101 0.095 Uiso 1 1 calc R . . H1S3 H 0.6870 0.9541 0.3293 0.095 Uiso 1 1 calc R . . C2S C 0.84509(19) 1.00819(17) 0.40485(11) 0.0431(4) Uani 1 1 d . . . C3S C 0.83293(19) 0.89950(18) 0.43636(12) 0.0441(4) Uani 1 1 d . . . H3S1 H 0.8091 0.8297 0.3941 0.066 Uiso 1 1 calc R . . H3S2 H 0.7712 0.8906 0.4693 0.066 Uiso 1 1 calc R . . H3S3 H 0.9105 0.9069 0.4664 0.066 Uiso 1 1 calc R . . O4S O 0.94251(19) 1.0791(2) 0.40523(13) 0.0893(7) 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 0.01734(6) 0.01764(6) 0.01847(6) 0.00570(4) 0.00605(4) 0.00510(4) N11A 0.0243(6) 0.0194(6) 0.0220(6) 0.0068(5) 0.0082(5) 0.0075(5) C12A 0.0280(7) 0.0153(6) 0.0252(7) 0.0041(5) 0.0115(6) 0.0061(5) C13A 0.0372(8) 0.0230(7) 0.0268(7) 0.0069(6) 0.0165(6) 0.0085(6) C14A 0.0471(10) 0.0266(8) 0.0225(7) 0.0089(6) 0.0122(7) 0.0134(7) C15A 0.0372(9) 0.0314(8) 0.0250(7) 0.0088(6) 0.0049(6) 0.0146(7) C16A 0.0280(8) 0.0293(8) 0.0256(7) 0.0092(6) 0.0077(6) 0.0114(6) N21A 0.0187(6) 0.0184(6) 0.0339(7) 0.0041(5) 0.0046(5) 0.0046(5) N22A 0.0188(6) 0.0159(5) 0.0278(6) 0.0044(5) 0.0061(5) 0.0043(4) C23A 0.0246(7) 0.0160(6) 0.0284(7) 0.0030(5) 0.0107(6) 0.0043(5) C24A 0.0246(8) 0.0244(7) 0.0377(9) 0.0023(6) 0.0148(6) 0.0037(6) C25A 0.0199(7) 0.0239(7) 0.0440(9) 0.0021(7) 0.0105(6) 0.0053(6) C26A 0.0237(7) 0.0219(7) 0.0342(8) 0.0092(6) 0.0017(6) 0.0057(6) C31A 0.0203(7) 0.0249(7) 0.0311(8) 0.0067(6) 0.0032(6) 0.0045(6) C32A 0.0292(8) 0.0248(7) 0.0321(8) 0.0073(6) 0.0057(6) 0.0086(6) C33A 0.0323(9) 0.0249(8) 0.0478(10) 0.0072(7) 0.0091(7) 0.0085(7) C34A 0.0334(9) 0.0324(9) 0.0468(11) -0.0064(8) 0.0064(8) 0.0081(7) C35A 0.0416(10) 0.0496(11) 0.0310(9) -0.0016(8) 0.0069(8) 0.0126(9) C36A 0.0355(9) 0.0392(9) 0.0342(9) 0.0133(7) 0.0085(7) 0.0101(7) N11B 0.0219(6) 0.0217(6) 0.0261(6) 0.0073(5) 0.0082(5) 0.0085(5) C12B 0.0251(7) 0.0236(7) 0.0269(7) 0.0058(6) 0.0077(6) 0.0094(6) C13B 0.0353(9) 0.0272(8) 0.0302(8) 0.0015(6) 0.0074(7) 0.0132(7) C14B 0.0387(9) 0.0214(7) 0.0429(10) 0.0038(7) 0.0068(7) 0.0118(7) C15B 0.0370(9) 0.0240(8) 0.0428(9) 0.0126(7) 0.0110(7) 0.0119(7) C16B 0.0290(8) 0.0256(7) 0.0322(8) 0.0117(6) 0.0103(6) 0.0114(6) N21B 0.0279(6) 0.0234(6) 0.0220(6) 0.0086(5) 0.0052(5) 0.0061(5) N22B 0.0211(6) 0.0210(6) 0.0209(6) 0.0071(5) 0.0051(5) 0.0057(5) C23B 0.0239(7) 0.0229(7) 0.0234(7) 0.0044(6) 0.0058(6) 0.0067(6) C24B 0.0340(8) 0.0302(8) 0.0216(7) 0.0030(6) 0.0067(6) 0.0084(7) C25B 0.0351(9) 0.0315(8) 0.0215(7) 0.0083(6) 0.0061(6) 0.0074(7) C26B 0.0259(7) 0.0238(7) 0.0246(7) 0.0083(6) 0.0040(6) 0.0083(6) C31B 0.0268(7) 0.0245(7) 0.0200(7) 0.0100(5) 0.0031(5) 0.0065(6) C32B 0.0316(8) 0.0284(8) 0.0278(8) 0.0101(6) 0.0067(6) 0.0094(6) C33B 0.0426(10) 0.0266(8) 0.0324(9) 0.0076(7) 0.0044(7) 0.0046(7) C34B 0.0337(9) 0.0355(9) 0.0375(9) 0.0135(7) -0.0027(7) -0.0009(7) C35B 0.0260(8) 0.0448(10) 0.0424(10) 0.0182(8) 0.0050(7) 0.0105(7) C36B 0.0303(8) 0.0298(8) 0.0319(8) 0.0111(6) 0.0067(6) 0.0111(6) N11C 0.0207(6) 0.0204(6) 0.0175(5) 0.0069(4) 0.0052(4) 0.0044(5) C12C 0.0222(7) 0.0248(7) 0.0167(6) 0.0080(5) 0.0033(5) 0.0041(5) C13C 0.0274(7) 0.0254(7) 0.0222(7) 0.0064(6) 0.0007(6) 0.0009(6) C14C 0.0400(9) 0.0211(7) 0.0252(7) 0.0035(6) 0.0047(7) 0.0055(6) C15C 0.0340(8) 0.0244(7) 0.0292(8) 0.0068(6) 0.0101(6) 0.0108(6) C16C 0.0238(7) 0.0229(7) 0.0243(7) 0.0073(6) 0.0072(6) 0.0065(6) N21C 0.0206(6) 0.0355(7) 0.0280(6) 0.0115(5) 0.0101(5) 0.0112(5) N22C 0.0188(6) 0.0282(6) 0.0209(6) 0.0099(5) 0.0068(5) 0.0089(5) C23C 0.0210(7) 0.0284(7) 0.0180(6) 0.0085(5) 0.0035(5) 0.0039(6) C24C 0.0210(7) 0.0380(9) 0.0271(8) 0.0096(7) 0.0035(6) 0.0022(6) C25C 0.0184(7) 0.0462(10) 0.0332(8) 0.0137(7) 0.0072(6) 0.0085(7) C26C 0.0290(8) 0.0344(8) 0.0372(9) 0.0179(7) 0.0162(7) 0.0167(7) C31C 0.0221(7) 0.0301(8) 0.0282(8) 0.0074(6) 0.0034(6) 0.0047(6) C32C 0.0465(11) 0.0406(10) 0.0368(9) 0.0156(8) 0.0110(8) 0.0170(8) C33C 0.0614(13) 0.0542(12) 0.0339(10) 0.0183(9) 0.0129(9) 0.0129(10) C34C 0.0474(11) 0.0514(12) 0.0324(9) -0.0024(8) 0.0107(8) 0.0071(9) C35C 0.0357(9) 0.0380(10) 0.0394(10) -0.0042(8) 0.0031(8) 0.0100(8) C36C 0.0258(8) 0.0334(8) 0.0342(9) 0.0062(7) 0.0022(6) 0.0078(6) P1 0.02499(19) 0.02315(18) 0.0288(2) 0.00706(15) 0.00824(15) 0.00954(15) F1 0.0365(6) 0.0487(6) 0.0434(6) 0.0262(5) 0.0121(5) 0.0147(5) F2 0.0745(8) 0.0330(6) 0.0514(7) 0.0134(5) 0.0306(6) 0.0299(6) F3 0.0746(9) 0.0623(8) 0.0367(6) 0.0050(5) 0.0170(6) 0.0470(7) F4 0.0626(7) 0.0346(5) 0.0366(6) 0.0153(4) 0.0174(5) 0.0250(5) F5 0.0288(5) 0.0440(6) 0.0714(8) 0.0204(6) 0.0003(5) 0.0000(5) F6 0.0316(6) 0.0679(8) 0.0527(7) 0.0175(6) -0.0035(5) 0.0010(6) P2 0.02267(19) 0.0312(2) 0.02478(19) 0.00785(16) 0.00446(15) 0.00623(15) F7 0.0261(5) 0.0545(7) 0.0309(5) 0.0156(5) -0.0002(4) 0.0045(4) F8 0.0242(5) 0.0614(7) 0.0441(6) 0.0090(5) -0.0004(4) 0.0078(5) F9 0.0590(7) 0.0335(6) 0.0476(7) 0.0051(5) -0.0024(6) 0.0180(5) F10 0.0502(7) 0.0379(6) 0.0681(8) 0.0262(6) 0.0060(6) 0.0079(5) F11 0.0443(7) 0.0945(10) 0.0328(6) 0.0155(6) 0.0169(5) 0.0254(7) F12 0.0361(5) 0.0520(6) 0.0275(5) 0.0078(4) 0.0077(4) 0.0171(5) C1S 0.0756(17) 0.0473(13) 0.0693(16) 0.0106(11) -0.0071(13) 0.0320(12) C2S 0.0453(11) 0.0354(10) 0.0370(10) 0.0061(8) -0.0014(8) 0.0001(8) C3S 0.0391(10) 0.0433(11) 0.0492(11) 0.0157(9) 0.0010(8) 0.0115(8) O4S 0.0638(12) 0.0861(15) 0.0863(14) 0.0419(12) -0.0093(10) -0.0269(11) _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 N22A 2.0611(12) . ? Ru1 N11A 2.0711(12) . ? Ru1 N22C 2.0741(12) . ? Ru1 N22B 2.0814(12) . ? Ru1 N11B 2.0820(12) . ? Ru1 N11C 2.0885(12) . ? N11A C16A 1.349(2) . ? N11A C12A 1.3620(18) . ? C12A C13A 1.388(2) . ? C12A C23A 1.449(2) . ? C13A C14A 1.378(3) . ? C13A H13A 0.9500 . ? C14A C15A 1.389(2) . ? C14A H14A 0.9500 . ? C15A C16A 1.384(2) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? N21A N22A 1.3556(18) . ? N21A C25A 1.361(2) . ? N21A C26A 1.450(2) . ? N22A C23A 1.3482(19) . ? C23A C24A 1.404(2) . ? C24A C25A 1.364(3) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? C26A C31A 1.516(2) . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? C31A C36A 1.390(2) . ? C31A C32A 1.390(2) . ? C32A C33A 1.389(2) . ? C32A H32A 0.9500 . ? C33A C34A 1.383(3) . ? C33A H33A 0.9500 . ? C34A C35A 1.388(3) . ? C34A H34A 0.9500 . ? C35A C36A 1.387(3) . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? N11B C16B 1.3515(19) . ? N11B C12B 1.360(2) . ? C12B C13B 1.388(2) . ? C12B C23B 1.456(2) . ? C13B C14B 1.384(2) . ? C13B H13B 0.9500 . ? C14B C15B 1.381(3) . ? C14B H14B 0.9500 . ? C15B C16B 1.379(2) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? N21B N22B 1.3572(17) . ? N21B C25B 1.360(2) . ? N21B C26B 1.4554(19) . ? N22B C23B 1.3439(19) . ? C23B C24B 1.403(2) . ? C24B C25B 1.371(2) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? C26B C31B 1.514(2) . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? C31B C36B 1.381(2) . ? C31B C32B 1.393(2) . ? C32B C33B 1.385(2) . ? C32B H32B 0.9500 . ? C33B C34B 1.387(3) . ? C33B H33B 0.9500 . ? C34B C35B 1.380(3) . ? C34B H34B 0.9500 . ? C35B C36B 1.399(2) . ? C35B H35B 0.9500 . ? C36B H36B 0.9500 . ? N11C C16C 1.3484(19) . ? N11C C12C 1.3641(18) . ? C12C C13C 1.384(2) . ? C12C C23C 1.455(2) . ? C13C C14C 1.388(2) . ? C13C H13C 0.9500 . ? C14C C15C 1.386(2) . ? C14C H14C 0.9500 . ? C15C C16C 1.384(2) . ? C15C H15C 0.9500 . ? C16C H16C 0.9500 . ? N21C C25C 1.355(2) . ? N21C N22C 1.3599(17) . ? N21C C26C 1.456(2) . ? N22C C23C 1.344(2) . ? C23C C24C 1.401(2) . ? C24C C25C 1.364(3) . ? C24C H24C 0.9500 . ? C25C H25C 0.9500 . ? C26C C31C 1.512(2) . ? C26C H26E 0.9900 . ? C26C H26F 0.9900 . ? C31C C36C 1.386(2) . ? C31C C32C 1.387(2) . ? C32C C33C 1.392(3) . ? C32C H32C 0.9500 . ? C33C C34C 1.378(3) . ? C33C H33C 0.9500 . ? C34C C35C 1.379(3) . ? C34C H34C 0.9500 . ? C35C C36C 1.387(3) . ? C35C H35C 0.9500 . ? C36C H36C 0.9500 . ? P1 F6 1.5825(12) . ? P1 F3 1.5901(11) . ? P1 F5 1.5977(12) . ? P1 F4 1.5994(11) . ? P1 F2 1.6032(11) . ? P1 F1 1.6090(11) . ? P2 F10 1.5915(12) . ? P2 F11 1.5948(12) . ? P2 F7 1.5991(10) . ? P2 F9 1.5997(12) . ? P2 F8 1.6019(11) . ? P2 F12 1.6079(10) . ? C1S C2S 1.488(3) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S O4S 1.207(3) . ? C2S C3S 1.494(3) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? 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 N22A Ru1 N11A 78.02(5) . . ? N22A Ru1 N22C 167.24(5) . . ? N11A Ru1 N22C 92.28(5) . . ? N22A Ru1 N22B 102.08(5) . . ? N11A Ru1 N22B 171.89(5) . . ? N22C Ru1 N22B 88.70(5) . . ? N22A Ru1 N11B 87.76(5) . . ? N11A Ru1 N11B 94.67(5) . . ? N22C Ru1 N11B 101.43(5) . . ? N22B Ru1 N11B 77.26(5) . . ? N22A Ru1 N11C 93.61(5) . . ? N11A Ru1 N11C 86.55(5) . . ? N22C Ru1 N11C 77.37(5) . . ? N22B Ru1 N11C 101.51(5) . . ? N11B Ru1 N11C 178.34(4) . . ? C16A N11A C12A 118.14(13) . . ? C16A N11A Ru1 125.85(10) . . ? C12A N11A Ru1 115.99(10) . . ? N11A C12A C13A 121.82(15) . . ? N11A C12A C23A 114.00(13) . . ? C13A C12A C23A 124.14(14) . . ? C14A C13A C12A 119.46(15) . . ? C14A C13A H13A 120.3 . . ? C12A C13A H13A 120.3 . . ? C13A C14A C15A 119.03(14) . . ? C13A C14A H14A 120.5 . . ? C15A C14A H14A 120.5 . . ? C16A C15A C14A 119.06(16) . . ? C16A C15A H15A 120.5 . . ? C14A C15A H15A 120.5 . . ? N11A C16A C15A 122.49(15) . . ? N11A C16A H16A 118.8 . . ? C15A C16A H16A 118.8 . . ? N22A N21A C25A 110.17(13) . . ? N22A N21A C26A 122.15(12) . . ? C25A N21A C26A 126.15(14) . . ? C23A N22A N21A 105.98(12) . . ? C23A N22A Ru1 115.57(10) . . ? N21A N22A Ru1 138.26(10) . . ? N22A C23A C24A 110.41(14) . . ? N22A C23A C12A 116.29(13) . . ? C24A C23A C12A 133.30(14) . . ? C25A C24A C23A 105.01(14) . . ? C25A C24A H24A 127.5 . . ? C23A C24A H24A 127.5 . . ? N21A C25A C24A 108.43(14) . . ? N21A C25A H25A 125.8 . . ? C24A C25A H25A 125.8 . . ? N21A C26A C31A 112.98(12) . . ? N21A C26A H26A 109.0 . . ? C31A C26A H26A 109.0 . . ? N21A C26A H26B 109.0 . . ? C31A C26A H26B 109.0 . . ? H26A C26A H26B 107.8 . . ? C36A C31A C32A 119.19(15) . . ? C36A C31A C26A 118.78(15) . . ? C32A C31A C26A 121.95(14) . . ? C33A C32A C31A 120.25(16) . . ? C33A C32A H32A 119.9 . . ? C31A C32A H32A 119.9 . . ? C34A C33A C32A 120.23(17) . . ? C34A C33A H33A 119.9 . . ? C32A C33A H33A 119.9 . . ? C33A C34A C35A 119.82(17) . . ? C33A C34A H34A 120.1 . . ? C35A C34A H34A 120.1 . . ? C36A C35A C34A 119.92(17) . . ? C36A C35A H35A 120.0 . . ? C34A C35A H35A 120.0 . . ? C35A C36A C31A 120.59(17) . . ? C35A C36A H36A 119.7 . . ? C31A C36A H36A 119.7 . . ? C16B N11B C12B 118.02(13) . . ? C16B N11B Ru1 125.57(11) . . ? C12B N11B Ru1 116.36(10) . . ? N11B C12B C13B 122.12(14) . . ? N11B C12B C23B 113.94(13) . . ? C13B C12B C23B 123.91(14) . . ? C14B C13B C12B 118.90(15) . . ? C14B C13B H13B 120.6 . . ? C12B C13B H13B 120.6 . . ? C15B C14B C13B 119.17(15) . . ? C15B C14B H14B 120.4 . . ? C13B C14B H14B 120.4 . . ? C16B C15B C14B 119.44(15) . . ? C16B C15B H15B 120.3 . . ? C14B C15B H15B 120.3 . . ? N11B C16B C15B 122.31(15) . . ? N11B C16B H16B 118.8 . . ? C15B C16B H16B 118.8 . . ? N22B N21B C25B 110.24(13) . . ? N22B N21B C26B 122.24(12) . . ? C25B N21B C26B 127.22(13) . . ? C23B N22B N21B 105.80(12) . . ? C23B N22B Ru1 115.62(10) . . ? N21B N22B Ru1 138.06(10) . . ? N22B C23B C24B 110.97(13) . . ? N22B C23B C12B 115.93(13) . . ? C24B C23B C12B 133.03(14) . . ? C25B C24B C23B 104.55(14) . . ? C25B C24B H24B 127.7 . . ? C23B C24B H24B 127.7 . . ? N21B C25B C24B 108.42(14) . . ? N21B C25B H25B 125.8 . . ? C24B C25B H25B 125.8 . . ? N21B C26B C31B 115.29(13) . . ? N21B C26B H26C 108.5 . . ? C31B C26B H26C 108.5 . . ? N21B C26B H26D 108.5 . . ? C31B C26B H26D 108.5 . . ? H26C C26B H26D 107.5 . . ? C36B C31B C32B 119.53(15) . . ? C36B C31B C26B 123.82(14) . . ? C32B C31B C26B 116.64(14) . . ? C33B C32B C31B 120.65(16) . . ? C33B C32B H32B 119.7 . . ? C31B C32B H32B 119.7 . . ? C32B C33B C34B 119.62(17) . . ? C32B C33B H33B 120.2 . . ? C34B C33B H33B 120.2 . . ? C35B C34B C33B 120.12(17) . . ? C35B C34B H34B 119.9 . . ? C33B C34B H34B 119.9 . . ? C34B C35B C36B 120.17(17) . . ? C34B C35B H35B 119.9 . . ? C36B C35B H35B 119.9 . . ? C31B C36B C35B 119.89(16) . . ? C31B C36B H36B 120.1 . . ? C35B C36B H36B 120.1 . . ? C16C N11C C12C 117.93(13) . . ? C16C N11C Ru1 125.81(10) . . ? C12C N11C Ru1 116.11(10) . . ? N11C C12C C13C 122.32(14) . . ? N11C C12C C23C 113.70(13) . . ? C13C C12C C23C 123.97(14) . . ? C12C C13C C14C 119.06(15) . . ? C12C C13C H13C 120.5 . . ? C14C C13C H13C 120.5 . . ? C15C C14C C13C 118.84(15) . . ? C15C C14C H14C 120.6 . . ? C13C C14C H14C 120.6 . . ? C16C C15C C14C 119.45(15) . . ? C16C C15C H15C 120.3 . . ? C14C C15C H15C 120.3 . . ? N11C C16C C15C 122.38(14) . . ? N11C C16C H16C 118.8 . . ? C15C C16C H16C 118.8 . . ? C25C N21C N22C 110.10(14) . . ? C25C N21C C26C 126.63(14) . . ? N22C N21C C26C 122.63(13) . . ? C23C N22C N21C 105.87(12) . . ? C23C N22C Ru1 116.03(10) . . ? N21C N22C Ru1 138.07(10) . . ? N22C C23C C24C 110.53(14) . . ? N22C C23C C12C 116.37(13) . . ? C24C C23C C12C 133.08(15) . . ? C25C C24C C23C 104.98(15) . . ? C25C C24C H24C 127.5 . . ? C23C C24C H24C 127.5 . . ? N21C C25C C24C 108.51(14) . . ? N21C C25C H25C 125.7 . . ? C24C C25C H25C 125.7 . . ? N21C C26C C31C 114.72(13) . . ? N21C C26C H26E 108.6 . . ? C31C C26C H26E 108.6 . . ? N21C C26C H26F 108.6 . . ? C31C C26C H26F 108.6 . . ? H26E C26C H26F 107.6 . . ? C36C C31C C32C 119.62(16) . . ? C36C C31C C26C 117.43(14) . . ? C32C C31C C26C 122.88(16) . . ? C31C C32C C33C 119.48(19) . . ? C31C C32C H32C 120.3 . . ? C33C C32C H32C 120.3 . . ? C34C C33C C32C 120.53(19) . . ? C34C C33C H33C 119.7 . . ? C32C C33C H33C 119.7 . . ? C33C C34C C35C 120.15(18) . . ? C33C C34C H34C 119.9 . . ? C35C C34C H34C 119.9 . . ? C34C C35C C36C 119.65(18) . . ? C34C C35C H35C 120.2 . . ? C36C C35C H35C 120.2 . . ? C31C C36C C35C 120.57(17) . . ? C31C C36C H36C 119.7 . . ? C35C C36C H36C 119.7 . . ? F6 P1 F3 90.12(8) . . ? F6 P1 F5 179.50(8) . . ? F3 P1 F5 90.34(8) . . ? F6 P1 F4 90.47(7) . . ? F3 P1 F4 90.08(6) . . ? F5 P1 F4 89.72(7) . . ? F6 P1 F2 90.12(8) . . ? F3 P1 F2 179.45(7) . . ? F5 P1 F2 89.42(7) . . ? F4 P1 F2 89.43(6) . . ? F6 P1 F1 90.33(7) . . ? F3 P1 F1 90.63(6) . . ? F5 P1 F1 89.47(6) . . ? F4 P1 F1 178.93(6) . . ? F2 P1 F1 89.86(6) . . ? F10 P2 F11 89.99(8) . . ? F10 P2 F7 89.99(7) . . ? F11 P2 F7 90.22(6) . . ? F10 P2 F9 179.68(8) . . ? F11 P2 F9 90.31(8) . . ? F7 P2 F9 89.91(6) . . ? F10 P2 F8 90.74(7) . . ? F11 P2 F8 90.54(7) . . ? F7 P2 F8 178.95(7) . . ? F9 P2 F8 89.36(7) . . ? F10 P2 F12 90.01(7) . . ? F11 P2 F12 179.92(7) . . ? F7 P2 F12 89.85(6) . . ? F9 P2 F12 89.69(6) . . ? F8 P2 F12 89.39(6) . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O4S C2S C1S 121.5(2) . . ? O4S C2S C3S 121.9(2) . . ? C1S C2S C3S 116.60(19) . . ? C2S C3S H3S1 109.5 . . ? C2S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C2S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N22A Ru1 N11A C16A 176.40(13) . . . . ? N22C Ru1 N11A C16A -11.97(13) . . . . ? N22B Ru1 N11A C16A 84.8(4) . . . . ? N11B Ru1 N11A C16A 89.69(12) . . . . ? N11C Ru1 N11A C16A -89.16(12) . . . . ? N22A Ru1 N11A C12A -2.04(10) . . . . ? N22C Ru1 N11A C12A 169.59(10) . . . . ? N22B Ru1 N11A C12A -93.6(3) . . . . ? N11B Ru1 N11A C12A -88.74(10) . . . . ? N11C Ru1 N11A C12A 92.40(10) . . . . ? C16A N11A C12A C13A -0.1(2) . . . . ? Ru1 N11A C12A C13A 178.42(11) . . . . ? C16A N11A C12A C23A -177.92(13) . . . . ? Ru1 N11A C12A C23A 0.64(15) . . . . ? N11A C12A C13A C14A 0.2(2) . . . . ? C23A C12A C13A C14A 177.72(14) . . . . ? C12A C13A C14A C15A -0.2(2) . . . . ? C13A C14A C15A C16A 0.1(2) . . . . ? C12A N11A C16A C15A 0.1(2) . . . . ? Ru1 N11A C16A C15A -178.30(12) . . . . ? C14A C15A C16A N11A -0.1(2) . . . . ? C25A N21A N22A C23A -0.87(16) . . . . ? C26A N21A N22A C23A -167.54(12) . . . . ? C25A N21A N22A Ru1 -175.29(11) . . . . ? C26A N21A N22A Ru1 18.0(2) . . . . ? N11A Ru1 N22A C23A 3.21(10) . . . . ? N22C Ru1 N22A C23A -38.0(3) . . . . ? N22B Ru1 N22A C23A 174.92(10) . . . . ? N11B Ru1 N22A C23A 98.46(10) . . . . ? N11C Ru1 N22A C23A -82.49(10) . . . . ? N11A Ru1 N22A N21A 177.26(15) . . . . ? N22C Ru1 N22A N21A 136.1(2) . . . . ? N22B Ru1 N22A N21A -11.03(15) . . . . ? N11B Ru1 N22A N21A -87.49(14) . . . . ? N11C Ru1 N22A N21A 91.56(14) . . . . ? N21A N22A C23A C24A 0.40(16) . . . . ? Ru1 N22A C23A C24A 176.28(10) . . . . ? N21A N22A C23A C12A -179.79(12) . . . . ? Ru1 N22A C23A C12A -3.91(16) . . . . ? N11A C12A C23A N22A 2.14(18) . . . . ? C13A C12A C23A N22A -175.57(13) . . . . ? N11A C12A C23A C24A -178.10(15) . . . . ? C13A C12A C23A C24A 4.2(3) . . . . ? N22A C23A C24A C25A 0.20(17) . . . . ? C12A C23A C24A C25A -179.57(15) . . . . ? N22A N21A C25A C24A 1.02(17) . . . . ? C26A N21A C25A C24A 167.03(14) . . . . ? C23A C24A C25A N21A -0.73(17) . . . . ? N22A N21A C26A C31A 81.24(17) . . . . ? C25A N21A C26A C31A -83.21(18) . . . . ? N21A C26A C31A C36A -174.83(14) . . . . ? N21A C26A C31A C32A 8.5(2) . . . . ? C36A C31A C32A C33A -0.5(2) . . . . ? C26A C31A C32A C33A 176.14(15) . . . . ? C31A C32A C33A C34A -0.2(3) . . . . ? C32A C33A C34A C35A 0.3(3) . . . . ? C33A C34A C35A C36A 0.2(3) . . . . ? C34A C35A C36A C31A -0.8(3) . . . . ? C32A C31A C36A C35A 1.0(3) . . . . ? C26A C31A C36A C35A -175.73(16) . . . . ? N22A Ru1 N11B C16B -69.40(13) . . . . ? N11A Ru1 N11B C16B 8.39(13) . . . . ? N22C Ru1 N11B C16B 101.67(12) . . . . ? N22B Ru1 N11B C16B -172.32(13) . . . . ? N11C Ru1 N11B C16B 145.2(16) . . . . ? N22A Ru1 N11B C12B 108.25(11) . . . . ? N11A Ru1 N11B C12B -173.96(11) . . . . ? N22C Ru1 N11B C12B -80.68(11) . . . . ? N22B Ru1 N11B C12B 5.33(10) . . . . ? N11C Ru1 N11B C12B -37.2(17) . . . . ? C16B N11B C12B C13B -1.8(2) . . . . ? Ru1 N11B C12B C13B -179.67(12) . . . . ? C16B N11B C12B C23B 176.14(13) . . . . ? Ru1 N11B C12B C23B -1.69(17) . . . . ? N11B C12B C13B C14B 1.7(2) . . . . ? C23B C12B C13B C14B -176.05(15) . . . . ? C12B C13B C14B C15B -0.3(3) . . . . ? C13B C14B C15B C16B -0.9(3) . . . . ? C12B N11B C16B C15B 0.5(2) . . . . ? Ru1 N11B C16B C15B 178.15(12) . . . . ? C14B C15B C16B N11B 0.8(3) . . . . ? C25B N21B N22B C23B -1.11(17) . . . . ? C26B N21B N22B C23B 173.01(13) . . . . ? C25B N21B N22B Ru1 169.84(12) . . . . ? C26B N21B N22B Ru1 -16.0(2) . . . . ? N22A Ru1 N22B C23B -93.32(11) . . . . ? N11A Ru1 N22B C23B -3.5(4) . . . . ? N22C Ru1 N22B C23B 93.57(11) . . . . ? N11B Ru1 N22B C23B -8.46(10) . . . . ? N11C Ru1 N22B C23B 170.40(10) . . . . ? N22A Ru1 N22B N21B 96.33(14) . . . . ? N11A Ru1 N22B N21B -173.8(3) . . . . ? N22C Ru1 N22B N21B -76.77(14) . . . . ? N11B Ru1 N22B N21B -178.80(15) . . . . ? N11C Ru1 N22B N21B 0.05(15) . . . . ? N21B N22B C23B C24B 1.14(17) . . . . ? Ru1 N22B C23B C24B -172.17(10) . . . . ? N21B N22B C23B C12B -176.41(13) . . . . ? Ru1 N22B C23B C12B 10.28(17) . . . . ? N11B C12B C23B N22B -5.7(2) . . . . ? C13B C12B C23B N22B 172.28(15) . . . . ? N11B C12B C23B C24B 177.49(16) . . . . ? C13B C12B C23B C24B -4.6(3) . . . . ? N22B C23B C24B C25B -0.74(19) . . . . ? C12B C23B C24B C25B 176.24(17) . . . . ? N22B N21B C25B C24B 0.68(19) . . . . ? C26B N21B C25B C24B -173.08(15) . . . . ? C23B C24B C25B N21B 0.03(19) . . . . ? N22B N21B C26B C31B 96.31(16) . . . . ? C25B N21B C26B C31B -90.62(19) . . . . ? N21B C26B C31B C36B 9.3(2) . . . . ? N21B C26B C31B C32B -170.99(13) . . . . ? C36B C31B C32B C33B 0.1(2) . . . . ? C26B C31B C32B C33B -179.58(14) . . . . ? C31B C32B C33B C34B 0.1(3) . . . . ? C32B C33B C34B C35B -0.6(3) . . . . ? C33B C34B C35B C36B 0.8(3) . . . . ? C32B C31B C36B C35B 0.1(2) . . . . ? C26B C31B C36B C35B 179.76(15) . . . . ? C34B C35B C36B C31B -0.5(3) . . . . ? N22A Ru1 N11C C16C -10.54(12) . . . . ? N11A Ru1 N11C C16C -88.29(12) . . . . ? N22C Ru1 N11C C16C 178.59(12) . . . . ? N22B Ru1 N11C C16C 92.58(12) . . . . ? N11B Ru1 N11C C16C 134.8(17) . . . . ? N22A Ru1 N11C C12C 164.91(10) . . . . ? N11A Ru1 N11C C12C 87.16(10) . . . . ? N22C Ru1 N11C C12C -5.96(9) . . . . ? N22B Ru1 N11C C12C -91.97(10) . . . . ? N11B Ru1 N11C C12C -49.7(17) . . . . ? C16C N11C C12C C13C 1.7(2) . . . . ? Ru1 N11C C12C C13C -174.07(11) . . . . ? C16C N11C C12C C23C -177.80(12) . . . . ? Ru1 N11C C12C C23C 6.37(15) . . . . ? N11C C12C C13C C14C -1.2(2) . . . . ? C23C C12C C13C C14C 178.35(14) . . . . ? C12C C13C C14C C15C -0.2(2) . . . . ? C13C C14C C15C C16C 1.0(2) . . . . ? C12C N11C C16C C15C -1.0(2) . . . . ? Ru1 N11C C16C C15C 174.40(11) . . . . ? C14C C15C C16C N11C -0.4(2) . . . . ? C25C N21C N22C C23C -0.14(16) . . . . ? C26C N21C N22C C23C 171.25(13) . . . . ? C25C N21C N22C Ru1 -177.84(11) . . . . ? C26C N21C N22C Ru1 -6.5(2) . . . . ? N22A Ru1 N22C C23C -41.3(3) . . . . ? N11A Ru1 N22C C23C -81.43(10) . . . . ? N22B Ru1 N22C C23C 106.62(10) . . . . ? N11B Ru1 N22C C23C -176.66(10) . . . . ? N11C Ru1 N22C C23C 4.52(10) . . . . ? N22A Ru1 N22C N21C 136.3(2) . . . . ? N11A Ru1 N22C N21C 96.11(14) . . . . ? N22B Ru1 N22C N21C -75.84(14) . . . . ? N11B Ru1 N22C N21C 0.88(15) . . . . ? N11C Ru1 N22C N21C -177.94(15) . . . . ? N21C N22C C23C C24C 0.25(16) . . . . ? Ru1 N22C C23C C24C 178.54(10) . . . . ? N21C N22C C23C C12C 179.12(12) . . . . ? Ru1 N22C C23C C12C -2.59(16) . . . . ? N11C C12C C23C N22C -2.50(18) . . . . ? C13C C12C C23C N22C 177.96(13) . . . . ? N11C C12C C23C C24C 176.06(15) . . . . ? C13C C12C C23C C24C -3.5(3) . . . . ? N22C C23C C24C C25C -0.26(17) . . . . ? C12C C23C C24C C25C -178.88(15) . . . . ? N22C N21C C25C C24C -0.02(18) . . . . ? C26C N21C C25C C24C -170.98(14) . . . . ? C23C C24C C25C N21C 0.17(18) . . . . ? C25C N21C C26C C31C -67.8(2) . . . . ? N22C N21C C26C C31C 122.32(15) . . . . ? N21C C26C C31C C36C 153.65(15) . . . . ? N21C C26C C31C C32C -29.3(2) . . . . ? C36C C31C C32C C33C -0.2(3) . . . . ? C26C C31C C32C C33C -177.12(18) . . . . ? C31C C32C C33C C34C -0.1(3) . . . . ? C32C C33C C34C C35C 0.4(3) . . . . ? C33C C34C C35C C36C -0.4(3) . . . . ? C32C C31C C36C C35C 0.2(3) . . . . ? C26C C31C C36C C35C 177.27(16) . . . . ? C34C C35C C36C C31C 0.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.538 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.079 _database_code_depnum_ccdc_archive 'CCDC 960000' ####################################################################### # # 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_imw1774p3c1try2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H27 N9 Ru, 2(F6 P)' _chemical_formula_sum 'C27 H27 F12 N9 P2 Ru' _chemical_formula_weight 868.59 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 Trigonal _symmetry_space_group_name_H-M 'P3c1 ' _symmetry_space_group_name_Hall 'P 3 -2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' _cell_length_a 10.3032(3) _cell_length_b 10.3032(3) _cell_length_c 17.0022(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1563.08(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9965 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.52 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8416 _exptl_absorpt_correction_T_max 0.8822 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26517 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0117 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.52 _reflns_number_total 2421 _reflns_number_gt 2305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _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. The structure was solved by direct methods. One third of the complex cation and each anion is found in the asymmetric unit, which grows to the full complex. The space group P-3c1 was suggested, but this did not allow a solvable solution of the dataset. The space group P3c1 instead gave a sensible solution. There is a large amount of residual density located near the ruthenium atom, due to the diffuse electron density around the metal centre. ; _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^)+(0.0965P)^2^+1.6743P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.20(5) _refine_ls_number_reflns 2421 _refine_ls_number_parameters 156 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.6667 0.3333 0.41845(4) 0.01714(16) Uani 1 3 d S . . N11 N 0.8624(5) 0.4305(4) 0.4854(3) 0.0196(9) Uani 1 1 d . . . C12 C 0.4243(4) 0.3878(5) 0.4672(2) 0.0215(7) Uani 1 1 d . . . C13 C 0.3411(4) 0.4296(4) 0.5141(2) 0.0246(7) Uani 1 1 d . . . H13 H 0.2396 0.3983 0.5020 0.030 Uiso 1 1 calc R . . C14 C 0.4106(5) 0.5181(5) 0.5790(2) 0.0281(7) Uani 1 1 d . . . H14 H 0.3540 0.5425 0.6140 0.034 Uiso 1 1 calc R . . C15 C 1.0110(4) 0.4392(5) 0.5942(2) 0.0271(8) Uani 1 1 d . . . H15 H 1.0285 0.3904 0.6369 0.033 Uiso 1 1 calc R . . C16 C 0.8892(4) 0.3625(4) 0.5458(2) 0.0245(7) Uani 1 1 d . . . H16 H 0.8223 0.2590 0.5551 0.029 Uiso 1 1 calc R . . N21 N 0.4627(5) 0.2574(5) 0.3624(2) 0.0207(6) Uani 1 1 d . . . N22 N 0.3865(5) 0.1763(4) 0.2988(3) 0.0281(8) Uani 1 1 d . . . C23 C 0.2441(5) 0.1590(5) 0.2942(2) 0.0290(8) Uani 1 1 d . . . H23 H 0.1697 0.1055 0.2555 0.035 Uiso 1 1 calc R . . C24 C 0.2336(4) 0.2356(5) 0.3575(2) 0.0259(7) Uani 1 1 d . . . H24 H 0.1501 0.2464 0.3711 0.031 Uiso 1 1 calc R . . C25 C 0.3685(4) 0.2943(4) 0.3979(2) 0.0216(7) Uani 1 1 d . . . C31 C 0.4488(5) 0.1079(5) 0.2478(2) 0.0299(8) Uani 1 1 d . . . H31A H 0.5402 0.1865 0.2227 0.045 Uiso 1 1 calc R . . H31B H 0.3754 0.0485 0.2072 0.045 Uiso 1 1 calc R . . H31C H 0.4728 0.0427 0.2790 0.045 Uiso 1 1 calc R . . P1 P 1.0000 0.0000 0.57284(17) 0.0300(5) Uani 1 3 d S . . F1 F 0.8635(4) -0.0233(5) 0.62888(18) 0.0534(8) Uani 1 1 d . . . F2 F 0.9790(4) 0.1153(3) 0.51959(16) 0.0421(7) Uani 1 1 d . . . P2 P 0.3333 0.6667 0.80402(14) 0.0251(5) Uani 1 3 d S . . F3 F 0.4676(3) 0.6830(4) 0.74874(15) 0.0372(6) Uani 1 1 d . . . F4 F 0.4519(3) 0.8006(3) 0.85791(14) 0.0348(6) 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 0.01218(18) 0.01218(18) 0.0271(3) 0.000 0.000 0.00609(9) N11 0.0116(19) 0.0204(17) 0.0275(17) 0.0057(12) 0.0002(16) 0.0084(12) C12 0.0253(18) 0.0265(18) 0.0176(14) 0.0020(12) -0.0012(13) 0.0167(15) C13 0.0268(18) 0.0288(18) 0.0263(16) 0.0033(14) 0.0017(14) 0.0200(16) C14 0.0261(19) 0.036(2) 0.0272(18) 0.0037(17) 0.0022(16) 0.0194(18) C15 0.0227(18) 0.0290(19) 0.0283(18) 0.0009(14) 0.0000(14) 0.0119(15) C16 0.0256(18) 0.0245(17) 0.0260(17) 0.0046(14) 0.0014(14) 0.0145(14) N21 0.0169(17) 0.0261(16) 0.0152(13) -0.0077(14) -0.0028(12) 0.0078(15) N22 0.0191(18) 0.0212(15) 0.0372(19) -0.0092(14) -0.0033(15) 0.0049(13) C23 0.032(2) 0.028(2) 0.0266(18) -0.0026(17) -0.0037(15) 0.0141(18) C24 0.0183(17) 0.035(2) 0.0268(17) -0.0044(15) -0.0049(13) 0.0148(15) C25 0.0145(15) 0.0253(17) 0.0234(16) -0.0004(13) -0.0006(12) 0.0088(13) C31 0.0298(19) 0.0310(19) 0.0307(18) -0.0088(16) -0.0039(15) 0.0165(16) P1 0.0339(8) 0.0339(8) 0.0221(10) 0.000 0.000 0.0170(4) F1 0.053(2) 0.071(2) 0.0392(15) -0.0137(16) 0.0091(14) 0.033(2) F2 0.0541(19) 0.0391(15) 0.0426(15) -0.0060(12) -0.0153(14) 0.0304(15) P2 0.0290(7) 0.0290(7) 0.0174(9) 0.000 0.000 0.0145(4) F3 0.0369(14) 0.0477(17) 0.0301(12) -0.0042(11) 0.0039(10) 0.0235(13) F4 0.0363(14) 0.0348(14) 0.0287(12) -0.0052(10) -0.0023(10) 0.0144(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N21 2.071(4) 2_655 ? Ru1 N21 2.071(4) 3_665 ? Ru1 N21 2.071(4) . ? Ru1 N11 2.085(4) . ? Ru1 N11 2.085(4) 3_665 ? Ru1 N11 2.085(4) 2_655 ? N11 C16 1.347(5) . ? N11 C12 1.364(5) 3_665 ? C12 N11 1.364(5) 2_655 ? C12 C13 1.388(5) . ? C12 C25 1.446(5) . ? C13 C14 1.382(6) . ? C13 H13 0.9500 . ? C14 C15 1.382(6) 2_655 ? C14 H14 0.9500 . ? C15 C16 1.373(5) . ? C15 C14 1.382(6) 3_665 ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 C25 1.349(6) . ? N21 N22 1.353(5) . ? N22 C23 1.389(6) . ? N22 C31 1.453(5) . ? C23 C24 1.370(6) . ? C23 H23 0.9500 . ? C24 C25 1.388(5) . ? C24 H24 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? P1 F2 1.592(3) 2_645 ? P1 F2 1.592(3) 3_765 ? P1 F2 1.592(3) . ? P1 F1 1.614(4) 3_765 ? P1 F1 1.614(4) 2_645 ? P1 F1 1.614(4) . ? P2 F4 1.597(3) 2_665 ? P2 F4 1.597(3) . ? P2 F4 1.597(3) 3_565 ? P2 F3 1.611(3) 2_665 ? P2 F3 1.611(3) . ? P2 F3 1.611(3) 3_565 ? 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 N21 Ru1 N21 100.54(13) 2_655 3_665 ? N21 Ru1 N21 100.54(13) 2_655 . ? N21 Ru1 N21 100.54(13) 3_665 . ? N21 Ru1 N11 88.51(13) 2_655 . ? N21 Ru1 N11 77.97(15) 3_665 . ? N21 Ru1 N11 170.94(14) . . ? N21 Ru1 N11 77.97(15) 2_655 3_665 ? N21 Ru1 N11 170.94(14) 3_665 3_665 ? N21 Ru1 N11 88.51(13) . 3_665 ? N11 Ru1 N11 93.03(16) . 3_665 ? N21 Ru1 N11 170.94(14) 2_655 2_655 ? N21 Ru1 N11 88.50(13) 3_665 2_655 ? N21 Ru1 N11 77.97(15) . 2_655 ? N11 Ru1 N11 93.03(16) . 2_655 ? N11 Ru1 N11 93.03(16) 3_665 2_655 ? C16 N11 C12 120.0(4) . 3_665 ? C16 N11 Ru1 124.6(3) . . ? C12 N11 Ru1 115.3(3) 3_665 . ? N11 C12 C13 120.7(4) 2_655 . ? N11 C12 C25 114.3(4) 2_655 . ? C13 C12 C25 125.0(3) . . ? C14 C13 C12 117.9(4) . . ? C14 C13 H13 121.1 . . ? C12 C13 H13 121.1 . . ? C13 C14 C15 121.3(4) . 2_655 ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 2_655 . ? C16 C15 C14 118.1(4) . 3_665 ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 3_665 . ? N11 C16 C15 121.6(4) . . ? N11 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C25 N21 N22 104.7(4) . . ? C25 N21 Ru1 115.2(3) . . ? N22 N21 Ru1 140.1(3) . . ? N21 N22 C23 111.9(4) . . ? N21 N22 C31 121.1(4) . . ? C23 N22 C31 126.8(4) . . ? C24 C23 N22 105.4(4) . . ? C24 C23 H23 127.3 . . ? N22 C23 H23 127.3 . . ? C23 C24 C25 106.9(4) . . ? C23 C24 H24 126.6 . . ? C25 C24 H24 126.6 . . ? N21 C25 C24 111.1(3) . . ? N21 C25 C12 116.7(3) . . ? C24 C25 C12 132.2(4) . . ? N22 C31 H31A 109.5 . . ? N22 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N22 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? F2 P1 F2 90.85(18) 2_645 3_765 ? F2 P1 F2 90.85(18) 2_645 . ? F2 P1 F2 90.86(19) 3_765 . ? F2 P1 F1 178.3(2) 2_645 3_765 ? F2 P1 F1 90.77(18) 3_765 3_765 ? F2 P1 F1 89.67(16) . 3_765 ? F2 P1 F1 90.77(18) 2_645 2_645 ? F2 P1 F1 89.67(16) 3_765 2_645 ? F2 P1 F1 178.3(2) . 2_645 ? F1 P1 F1 88.7(2) 3_765 2_645 ? F2 P1 F1 89.66(16) 2_645 . ? F2 P1 F1 178.3(2) 3_765 . ? F2 P1 F1 90.77(18) . . ? F1 P1 F1 88.7(2) 3_765 . ? F1 P1 F1 88.7(2) 2_645 . ? F4 P2 F4 90.36(16) 2_665 . ? F4 P2 F4 90.36(16) 2_665 3_565 ? F4 P2 F4 90.36(16) . 3_565 ? F4 P2 F3 89.91(14) 2_665 2_665 ? F4 P2 F3 90.36(14) . 2_665 ? F4 P2 F3 179.2(2) 3_565 2_665 ? F4 P2 F3 179.2(2) 2_665 . ? F4 P2 F3 89.90(14) . . ? F4 P2 F3 90.35(14) 3_565 . ? F3 P2 F3 89.37(16) 2_665 . ? F4 P2 F3 90.36(14) 2_665 3_565 ? F4 P2 F3 179.2(2) . 3_565 ? F4 P2 F3 89.90(14) 3_565 3_565 ? F3 P2 F3 89.38(16) 2_665 3_565 ? F3 P2 F3 89.37(16) . 3_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N21 Ru1 N11 C16 -75.5(3) 2_655 . . . ? N21 Ru1 N11 C16 -176.6(3) 3_665 . . . ? N21 Ru1 N11 C16 102.0(10) . . . . ? N11 Ru1 N11 C16 2.4(4) 3_665 . . . ? N11 Ru1 N11 C16 95.6(3) 2_655 . . . ? N21 Ru1 N11 C12 108.1(3) 2_655 . . 3_665 ? N21 Ru1 N11 C12 7.0(3) 3_665 . . 3_665 ? N21 Ru1 N11 C12 -74.5(13) . . . 3_665 ? N11 Ru1 N11 C12 -174.0(3) 3_665 . . 3_665 ? N11 Ru1 N11 C12 -80.8(4) 2_655 . . 3_665 ? N11 C12 C13 C14 0.6(6) 2_655 . . . ? C25 C12 C13 C14 179.2(4) . . . . ? C12 C13 C14 C15 4.2(6) . . . 2_655 ? C12 N11 C16 C15 5.3(6) 3_665 . . . ? Ru1 N11 C16 C15 -171.0(3) . . . . ? C14 C15 C16 N11 -0.5(6) 3_665 . . . ? N21 Ru1 N21 C25 165.5(3) 2_655 . . . ? N21 Ru1 N21 C25 -91.6(4) 3_665 . . . ? N11 Ru1 N21 C25 -11.9(13) . . . . ? N11 Ru1 N21 C25 88.0(3) 3_665 . . . ? N11 Ru1 N21 C25 -5.4(3) 2_655 . . . ? N21 Ru1 N21 N22 -13.2(5) 2_655 . . . ? N21 Ru1 N21 N22 89.7(4) 3_665 . . . ? N11 Ru1 N21 N22 169.4(8) . . . . ? N11 Ru1 N21 N22 -90.7(5) 3_665 . . . ? N11 Ru1 N21 N22 175.9(5) 2_655 . . . ? C25 N21 N22 C23 -1.1(5) . . . . ? Ru1 N21 N22 C23 177.7(4) . . . . ? C25 N21 N22 C31 -176.1(4) . . . . ? Ru1 N21 N22 C31 2.6(7) . . . . ? N21 N22 C23 C24 1.1(5) . . . . ? C31 N22 C23 C24 175.8(4) . . . . ? N22 C23 C24 C25 -0.6(5) . . . . ? N22 N21 C25 C24 0.7(5) . . . . ? Ru1 N21 C25 C24 -178.4(3) . . . . ? N22 N21 C25 C12 -177.6(3) . . . . ? Ru1 N21 C25 C12 3.2(4) . . . . ? C23 C24 C25 N21 -0.1(5) . . . . ? C23 C24 C25 C12 177.9(4) . . . . ? N11 C12 C25 N21 2.7(4) 2_655 . . . ? C13 C12 C25 N21 -175.9(4) . . . . ? N11 C12 C25 C24 -175.1(4) 2_655 . . . ? C13 C12 C25 C24 6.3(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.962 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.127 _database_code_depnum_ccdc_archive 'CCDC 960001' ####################################################################### # # 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_imw1775p-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H27 N9 Ru, 2(F6 P)' _chemical_formula_sum 'C27 H27 F12 N9 P2 Ru' _chemical_formula_weight 868.59 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' 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 'P2(1)/C ' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.8161(5) _cell_length_b 13.2773(5) _cell_length_c 20.7149(7) _cell_angle_alpha 90.00 _cell_angle_beta 117.692(2) _cell_angle_gamma 90.00 _cell_volume 3364.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8010 _exptl_absorpt_correction_T_max 0.9676 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 59514 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.54 _reflns_number_total 7735 _reflns_number_gt 6869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _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. The structure was solved by direct methods. Hydrogens were added in calculated positions. One of the PF6 anions was disordered over two sites, and global restraints were used in order to bring the thermal parameters in line. Two of the rings were fixed using geometric restraints, and the nitrogen-methyl bond on the same pyrazolyl ring was fixed at a reasonable distance. ; _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^)+(0.0424P)^2^+17.6466P] 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 7735 _refine_ls_number_parameters 503 _refine_ls_number_restraints 391 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1495 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.117 _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 0.71222(3) 0.24242(3) 0.294661(18) 0.02737(11) Uani 1 1 d . . . N11A N 0.5534(3) 0.2771(3) 0.2716(2) 0.0361(8) Uani 1 1 d U . . C12A C 0.5127(4) 0.2241(4) 0.3102(3) 0.0374(10) Uani 1 1 d U . . C13A C 0.4047(4) 0.2372(5) 0.2964(3) 0.0479(12) Uani 1 1 d U . . H13A H 0.3768 0.1997 0.3232 0.057 Uiso 1 1 calc R . . C14A C 0.3387(5) 0.3043(5) 0.2441(4) 0.0584(15) Uani 1 1 d U . . H14A H 0.2650 0.3135 0.2343 0.070 Uiso 1 1 calc R . . C15A C 0.3806(5) 0.3582(6) 0.2057(4) 0.0603(16) Uani 1 1 d U . . H15A H 0.3363 0.4048 0.1691 0.072 Uiso 1 1 calc R . . C16A C 0.4874(4) 0.3429(5) 0.2216(3) 0.0488(13) Uani 1 1 d U . . H16A H 0.5162 0.3811 0.1957 0.059 Uiso 1 1 calc R . . N21A N 0.7456(4) 0.0802(3) 0.4163(2) 0.0406(9) Uani 1 1 d U . . N22A N 0.6878(3) 0.1495(3) 0.3649(2) 0.0341(8) Uani 1 1 d U . . C23A C 0.5887(4) 0.1534(4) 0.3620(3) 0.0376(10) Uani 1 1 d U . . C24A C 0.5828(5) 0.0850(4) 0.4116(3) 0.0495(13) Uani 1 1 d U . . H24A H 0.5222 0.0724 0.4203 0.059 Uiso 1 1 calc R . . C25A C 0.6836(5) 0.0406(4) 0.4446(3) 0.0515(13) Uani 1 1 d U . . H25A H 0.7063 -0.0097 0.4814 0.062 Uiso 1 1 calc R . . C26A C 0.8586(5) 0.0550(5) 0.4361(3) 0.0522(14) Uani 1 1 d U . . H26A H 0.8624 0.0263 0.3937 0.078 Uiso 1 1 calc R . . H26B H 0.8859 0.0056 0.4758 0.078 Uiso 1 1 calc R . . H26C H 0.9036 0.1160 0.4521 0.078 Uiso 1 1 calc R . . N11B N 0.7612(3) 0.3653(3) 0.3653(2) 0.0323(8) Uani 1 1 d U . . C12B C 0.7729(4) 0.4537(4) 0.3369(3) 0.0352(10) Uani 1 1 d U . . C13B C 0.8001(5) 0.5424(4) 0.3768(3) 0.0464(12) Uani 1 1 d U . . H13B H 0.8085 0.6033 0.3558 0.056 Uiso 1 1 calc R . . C14B C 0.8148(6) 0.5411(4) 0.4473(3) 0.0595(15) Uani 1 1 d U . . H14B H 0.8320 0.6014 0.4751 0.071 Uiso 1 1 calc R . . C15B C 0.8042(6) 0.4517(4) 0.4771(3) 0.0581(15) Uani 1 1 d U . . H15B H 0.8152 0.4491 0.5258 0.070 Uiso 1 1 calc R . . C16B C 0.7775(5) 0.3657(4) 0.4345(3) 0.0459(12) Uani 1 1 d U . . H16B H 0.7702 0.3040 0.4552 0.055 Uiso 1 1 calc R . . N21B N 0.7169(3) 0.3657(4) 0.1638(2) 0.0419(10) Uani 1 1 d U . . N22B N 0.7253(3) 0.3547(3) 0.2308(2) 0.0327(8) Uani 1 1 d U . . C23B C 0.7566(4) 0.4459(4) 0.2629(3) 0.0347(9) Uani 1 1 d U . . C24B C 0.7683(5) 0.5142(4) 0.2151(3) 0.0449(12) Uani 1 1 d U . . H24B H 0.7892 0.5830 0.2239 0.054 Uiso 1 1 calc R . . C25B C 0.7431(5) 0.4604(5) 0.1536(3) 0.0491(13) Uani 1 1 d U . . H25B H 0.7439 0.4850 0.1107 0.059 Uiso 1 1 calc R . . C26B C 0.6876(5) 0.2817(5) 0.1129(3) 0.0533(15) Uani 1 1 d U . . H26D H 0.7479 0.2331 0.1304 0.080 Uiso 1 1 calc R . . H26E H 0.6734 0.3067 0.0648 0.080 Uiso 1 1 calc R . . H26F H 0.6218 0.2487 0.1093 0.080 Uiso 1 1 calc R . . N11C N 0.6681(3) 0.1246(2) 0.22259(18) 0.0479(11) Uani 1 1 d GU . . C12C C 0.7519(3) 0.0715(3) 0.2187(2) 0.0575(14) Uani 1 1 d GU . . C13C C 0.7273(4) -0.0067(3) 0.1688(3) 0.077(2) Uani 1 1 d GU . . H13C H 0.7846 -0.0430 0.1661 0.092 Uiso 1 1 calc R . . C14C C 0.6190(5) -0.0317(3) 0.1229(3) 0.096(2) Uani 1 1 d GU . . H14C H 0.6022 -0.0851 0.0888 0.115 Uiso 1 1 calc R . . C15C C 0.5352(4) 0.0214(4) 0.1268(2) 0.094(2) Uani 1 1 d GU . . H15C H 0.4611 0.0044 0.0955 0.113 Uiso 1 1 calc R . . C16C C 0.5597(3) 0.0996(3) 0.1767(2) 0.080(2) Uani 1 1 d GU . . H16C H 0.5025 0.1359 0.1794 0.096 Uiso 1 1 calc R . . N21C N 0.9728(3) 0.2147(3) 0.3495(2) 0.0658(14) Uani 1 1 d GDU . . N22C N 0.8604(3) 0.1901(2) 0.3080(2) 0.0443(10) Uani 1 1 d GU . . C23C C 0.8524(3) 0.1045(3) 0.2646(2) 0.0571(14) Uani 1 1 d GU . . C24C C 0.9598(4) 0.0762(3) 0.2794(3) 0.0666(17) Uani 1 1 d GU . . H24C H 0.9783 0.0213 0.2578 0.080 Uiso 1 1 calc R . . C25C C 1.0324(7) 0.1415(5) 0.3300(4) 0.0702(18) Uani 1 1 d GU . . H25C H 1.1096 0.1391 0.3493 0.084 Uiso 1 1 calc R . . C26C C 1.0084(6) 0.3055(4) 0.3940(4) 0.081(2) Uani 1 1 d DU . . H26G H 1.0884 0.3085 0.4189 0.122 Uiso 1 1 calc R . . H26H H 0.9815 0.3043 0.4302 0.122 Uiso 1 1 calc R . . H26I H 0.9792 0.3649 0.3627 0.122 Uiso 1 1 calc R . . P1 P 0.35552(15) 0.22798(12) 0.48386(8) 0.0519(4) Uani 1 1 d . . . F1 F 0.2456(6) 0.1774(8) 0.4835(4) 0.0576(19) Uani 0.684(9) 1 d PU A 1 F2 F 0.4162(6) 0.2214(8) 0.5664(3) 0.089(3) Uani 0.684(9) 1 d PU A 1 F3 F 0.3035(7) 0.3343(5) 0.4827(5) 0.086(2) Uani 0.684(9) 1 d PU A 1 F4 F 0.4464(9) 0.2767(13) 0.4725(9) 0.064(3) Uani 0.684(9) 1 d PU A 1 F5 F 0.3957(7) 0.1180(5) 0.4778(6) 0.081(3) Uani 0.684(9) 1 d PU A 1 F6 F 0.2844(5) 0.2281(7) 0.3950(3) 0.077(2) Uani 0.684(9) 1 d PU A 1 F1A F 0.4546(15) 0.1554(14) 0.5488(10) 0.091(5) Uani 0.316(9) 1 d PU A 2 F2A F 0.4065(15) 0.3144(14) 0.5481(10) 0.103(6) Uani 0.316(9) 1 d PU A 2 F3A F 0.2862(12) 0.2994(16) 0.4278(11) 0.093(6) Uani 0.316(9) 1 d PU A 2 F4A F 0.3406(18) 0.1411(16) 0.4356(11) 0.091(5) Uani 0.316(9) 1 d PU A 2 F5A F 0.2833(16) 0.1945(18) 0.5134(10) 0.068(4) Uani 0.316(9) 1 d PU A 2 F6A F 0.4753(18) 0.266(2) 0.4826(18) 0.053(5) Uani 0.316(9) 1 d PU A 2 P2 P 0.00962(12) 0.78157(11) 0.36567(8) 0.0430(3) Uani 1 1 d . . . F21 F -0.0930(3) 0.7182(3) 0.30895(19) 0.0556(8) Uani 1 1 d . . . F22 F -0.0677(3) 0.8759(3) 0.3537(2) 0.0701(11) Uani 1 1 d . . . F23 F 0.0331(3) 0.8182(3) 0.30113(17) 0.0506(8) Uani 1 1 d . . . F24 F 0.1131(3) 0.8426(4) 0.4223(2) 0.0871(15) Uani 1 1 d . . . F25 F 0.0849(3) 0.6846(3) 0.3765(2) 0.0702(11) Uani 1 1 d . . . F26 F -0.0126(4) 0.7426(4) 0.4313(2) 0.0752(12) 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 0.02778(18) 0.03039(19) 0.02301(17) -0.00523(13) 0.01103(13) -0.00039(14) N11A 0.036(2) 0.044(2) 0.0304(19) 0.0018(16) 0.0169(16) 0.0019(17) C12A 0.039(2) 0.047(3) 0.032(2) -0.0071(19) 0.0217(19) -0.003(2) C13A 0.039(3) 0.062(3) 0.049(3) -0.006(2) 0.026(2) -0.006(2) C14A 0.036(3) 0.075(4) 0.063(4) -0.006(3) 0.022(3) 0.000(3) C15A 0.040(3) 0.079(4) 0.054(3) 0.012(3) 0.015(3) 0.015(3) C16A 0.039(3) 0.064(3) 0.040(3) 0.010(2) 0.016(2) 0.008(2) N21A 0.054(2) 0.033(2) 0.0304(19) -0.0001(16) 0.0161(18) 0.0036(18) N22A 0.041(2) 0.0309(19) 0.0278(18) -0.0025(15) 0.0144(16) 0.0032(16) C23A 0.047(3) 0.038(2) 0.032(2) -0.0065(18) 0.022(2) -0.008(2) C24A 0.067(3) 0.046(3) 0.044(3) -0.001(2) 0.033(3) -0.006(3) C25A 0.077(4) 0.041(3) 0.036(3) 0.001(2) 0.026(3) -0.001(3) C26A 0.063(4) 0.047(3) 0.041(3) 0.002(2) 0.020(3) 0.023(3) N11B 0.041(2) 0.0279(18) 0.0251(17) -0.0017(14) 0.0131(16) 0.0044(16) C12B 0.040(2) 0.031(2) 0.037(2) -0.0001(18) 0.020(2) 0.0046(18) C13B 0.064(3) 0.032(2) 0.048(3) -0.003(2) 0.029(3) -0.002(2) C14B 0.089(4) 0.037(3) 0.055(3) -0.013(2) 0.035(3) -0.002(3) C15B 0.097(4) 0.045(3) 0.033(3) -0.011(2) 0.030(3) -0.004(3) C16B 0.069(3) 0.036(2) 0.030(2) -0.0020(19) 0.021(2) 0.002(2) N21B 0.040(2) 0.061(3) 0.0286(19) -0.0024(18) 0.0185(17) -0.004(2) N22B 0.0303(18) 0.042(2) 0.0274(18) 0.0017(15) 0.0150(15) 0.0011(16) C23B 0.035(2) 0.037(2) 0.034(2) 0.0019(18) 0.0171(19) 0.0026(19) C24B 0.048(3) 0.044(3) 0.048(3) 0.007(2) 0.027(2) 0.000(2) C25B 0.050(3) 0.062(3) 0.041(3) 0.012(2) 0.027(2) -0.002(3) C26B 0.056(3) 0.077(4) 0.033(3) -0.014(3) 0.026(3) -0.024(3) N11C 0.068(3) 0.047(2) 0.043(2) -0.0208(19) 0.037(2) -0.029(2) C12C 0.096(4) 0.035(3) 0.069(3) -0.009(2) 0.062(3) -0.009(3) C13C 0.145(6) 0.044(3) 0.072(4) -0.020(3) 0.076(4) -0.005(4) C14C 0.129(6) 0.080(5) 0.107(6) -0.022(5) 0.080(5) -0.018(5) C15C 0.117(6) 0.089(5) 0.072(5) -0.029(4) 0.040(4) -0.044(5) C16C 0.105(5) 0.088(5) 0.042(3) -0.019(3) 0.029(3) -0.053(4) N21C 0.053(3) 0.059(3) 0.085(4) 0.022(3) 0.031(3) 0.004(2) N22C 0.034(2) 0.036(2) 0.065(3) 0.008(2) 0.024(2) 0.0003(17) C23C 0.085(4) 0.041(3) 0.079(4) 0.018(3) 0.066(3) 0.021(3) C24C 0.087(4) 0.055(3) 0.090(4) 0.019(3) 0.069(4) 0.026(3) C25C 0.093(5) 0.061(4) 0.090(5) 0.025(3) 0.070(4) 0.032(3) C26C 0.057(4) 0.082(5) 0.089(6) -0.007(4) 0.021(4) 0.002(4) P1 0.0699(10) 0.0529(9) 0.0411(8) 0.0009(6) 0.0327(8) 0.0015(7) F1 0.042(4) 0.079(5) 0.051(4) 0.020(4) 0.022(3) 0.005(3) F2 0.086(5) 0.139(8) 0.031(3) 0.001(4) 0.018(3) -0.020(5) F3 0.102(6) 0.053(4) 0.132(7) -0.002(4) 0.078(6) 0.011(3) F4 0.030(6) 0.088(7) 0.052(5) 0.014(4) -0.001(5) 0.004(4) F5 0.087(6) 0.055(4) 0.132(8) 0.004(5) 0.075(6) 0.009(4) F6 0.063(4) 0.135(7) 0.037(3) -0.006(4) 0.026(3) -0.030(4) F1A 0.110(11) 0.083(10) 0.083(10) 0.038(8) 0.048(9) 0.014(9) F2A 0.104(11) 0.085(10) 0.105(11) -0.046(9) 0.038(9) -0.010(9) F3A 0.064(8) 0.098(12) 0.096(12) 0.053(10) 0.019(9) -0.017(8) F4A 0.113(13) 0.093(12) 0.082(11) -0.040(9) 0.058(9) -0.015(10) F5A 0.064(11) 0.080(10) 0.066(11) 0.018(10) 0.037(8) 0.001(9) F6A 0.023(10) 0.058(8) 0.056(10) 0.041(6) -0.001(9) 0.001(8) P2 0.0411(7) 0.0514(8) 0.0389(7) -0.0052(6) 0.0205(6) -0.0033(6) F21 0.055(2) 0.0510(19) 0.060(2) -0.0095(16) 0.0264(17) -0.0118(16) F22 0.075(3) 0.050(2) 0.103(3) -0.012(2) 0.056(2) 0.0021(19) F23 0.061(2) 0.0524(19) 0.0439(17) -0.0024(14) 0.0289(16) -0.0086(16) F24 0.061(2) 0.146(4) 0.060(2) -0.050(3) 0.033(2) -0.044(3) F25 0.065(2) 0.087(3) 0.062(2) 0.022(2) 0.0322(19) 0.030(2) F26 0.080(3) 0.104(3) 0.056(2) 0.007(2) 0.044(2) -0.002(2) _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 N11C 2.050(3) . ? Ru1 N22A 2.052(4) . ? Ru1 N22B 2.056(4) . ? Ru1 N22C 2.056(3) . ? Ru1 N11A 2.069(4) . ? Ru1 N11B 2.084(4) . ? N11A C16A 1.338(7) . ? N11A C12A 1.367(6) . ? C12A C13A 1.394(7) . ? C12A C23A 1.444(7) . ? C13A C14A 1.371(9) . ? C13A H13A 0.9500 . ? C14A C15A 1.381(9) . ? C14A H14A 0.9500 . ? C15A C16A 1.368(8) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? N21A C25A 1.350(7) . ? N21A N22A 1.352(5) . ? N21A C26A 1.457(7) . ? N22A C23A 1.344(6) . ? C23A C24A 1.401(7) . ? C24A C25A 1.368(9) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? N11B C16B 1.344(6) . ? N11B C12B 1.355(6) . ? C12B C13B 1.388(7) . ? C12B C23B 1.445(6) . ? C13B C14B 1.377(8) . ? C13B H13B 0.9500 . ? C14B C15B 1.377(8) . ? C14B H14B 0.9500 . ? C15B C16B 1.384(7) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? N21B N22B 1.346(5) . ? N21B C25B 1.352(7) . ? N21B C26B 1.458(7) . ? N22B C23B 1.352(6) . ? C23B C24B 1.407(7) . ? C24B C25B 1.358(8) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? N11C C12C 1.3900 . ? N11C C16C 1.3900 . ? C12C C23C 1.341(5) . ? C12C C13C 1.3900 . ? C13C C14C 1.3900 . ? C13C H13C 0.9500 . ? C14C C15C 1.3900 . ? C14C H14C 0.9500 . ? C15C C16C 1.3900 . ? C15C H15C 0.9500 . ? C16C H16C 0.9500 . ? N21C N22C 1.4200 . ? N21C C25C 1.446(7) . ? N21C C26C 1.4580(10) . ? N22C C23C 1.4200 . ? C23C C24C 1.4200 . ? C24C C25C 1.372(10) . ? C24C H24C 0.9500 . ? C25C H25C 0.9500 . ? C26C H26G 0.9800 . ? C26C H26H 0.9800 . ? C26C H26I 0.9800 . ? P1 F3A 1.460(14) . ? P1 F5A 1.46(2) . ? P1 F4A 1.477(16) . ? P1 F2 1.518(6) . ? P1 F4 1.525(15) . ? P1 F3 1.580(6) . ? P1 F5 1.588(7) . ? P1 F6 1.635(6) . ? P1 F2A 1.646(15) . ? P1 F1 1.658(9) . ? P1 F1A 1.703(15) . ? P1 F6A 1.74(2) . ? P2 F24 1.587(4) . ? P2 F22 1.589(4) . ? P2 F23 1.592(3) . ? P2 F21 1.597(4) . ? P2 F25 1.604(4) . ? P2 F26 1.611(4) . ? 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 N11C Ru1 N22A 88.05(14) . . ? N11C Ru1 N22B 99.81(15) . . ? N22A Ru1 N22B 170.04(15) . . ? N11C Ru1 N22C 77.32(14) . . ? N22A Ru1 N22C 100.54(15) . . ? N22B Ru1 N22C 87.25(15) . . ? N11C Ru1 N11A 94.40(15) . . ? N22A Ru1 N11A 77.96(16) . . ? N22B Ru1 N11A 95.21(15) . . ? N22C Ru1 N11A 171.66(15) . . ? N11C Ru1 N11B 177.13(15) . . ? N22A Ru1 N11B 94.60(15) . . ? N22B Ru1 N11B 77.67(15) . . ? N22C Ru1 N11B 101.08(15) . . ? N11A Ru1 N11B 87.23(16) . . ? C16A N11A C12A 118.1(5) . . ? C16A N11A Ru1 126.3(4) . . ? C12A N11A Ru1 115.5(3) . . ? N11A C12A C13A 120.5(5) . . ? N11A C12A C23A 114.5(4) . . ? C13A C12A C23A 125.0(5) . . ? C14A C13A C12A 119.9(5) . . ? C14A C13A H13A 120.0 . . ? C12A C13A H13A 120.0 . . ? C13A C14A C15A 119.3(5) . . ? C13A C14A H14A 120.4 . . ? C15A C14A H14A 120.4 . . ? C16A C15A C14A 118.5(6) . . ? C16A C15A H15A 120.7 . . ? C14A C15A H15A 120.7 . . ? N11A C16A C15A 123.6(6) . . ? N11A C16A H16A 118.2 . . ? C15A C16A H16A 118.2 . . ? C25A N21A N22A 110.2(5) . . ? C25A N21A C26A 127.0(5) . . ? N22A N21A C26A 122.8(4) . . ? C23A N22A N21A 106.2(4) . . ? C23A N22A Ru1 116.4(3) . . ? N21A N22A Ru1 137.4(3) . . ? N22A C23A C24A 110.3(5) . . ? N22A C23A C12A 115.6(4) . . ? C24A C23A C12A 134.1(5) . . ? C25A C24A C23A 104.7(5) . . ? C25A C24A H24A 127.7 . . ? C23A C24A H24A 127.7 . . ? N21A C25A C24A 108.6(5) . . ? N21A C25A H25A 125.7 . . ? C24A C25A H25A 125.7 . . ? N21A C26A H26A 109.5 . . ? N21A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? N21A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C16B N11B C12B 117.8(4) . . ? C16B N11B Ru1 126.2(3) . . ? C12B N11B Ru1 116.0(3) . . ? N11B C12B C13B 122.0(4) . . ? N11B C12B C23B 114.0(4) . . ? C13B C12B C23B 123.9(5) . . ? C14B C13B C12B 119.1(5) . . ? C14B C13B H13B 120.4 . . ? C12B C13B H13B 120.4 . . ? C15B C14B C13B 119.4(5) . . ? C15B C14B H14B 120.3 . . ? C13B C14B H14B 120.3 . . ? C14B C15B C16B 118.6(5) . . ? C14B C15B H15B 120.7 . . ? C16B C15B H15B 120.7 . . ? N11B C16B C15B 123.0(5) . . ? N11B C16B H16B 118.5 . . ? C15B C16B H16B 118.5 . . ? N22B N21B C25B 111.2(4) . . ? N22B N21B C26B 121.7(4) . . ? C25B N21B C26B 127.1(4) . . ? N21B N22B C23B 105.3(4) . . ? N21B N22B Ru1 138.7(3) . . ? C23B N22B Ru1 115.9(3) . . ? N22B C23B C24B 110.2(4) . . ? N22B C23B C12B 116.2(4) . . ? C24B C23B C12B 133.5(5) . . ? C25B C24B C23B 105.0(5) . . ? C25B C24B H24B 127.5 . . ? C23B C24B H24B 127.5 . . ? N21B C25B C24B 108.2(5) . . ? N21B C25B H25B 125.9 . . ? C24B C25B H25B 125.9 . . ? N21B C26B H26D 109.5 . . ? N21B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? N21B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C12C N11C C16C 120.0 . . ? C12C N11C Ru1 117.1(2) . . ? C16C N11C Ru1 122.8(2) . . ? C23C C12C C13C 125.9(3) . . ? C23C C12C N11C 114.1(3) . . ? C13C C12C N11C 120.0 . . ? C12C C13C C14C 120.0 . . ? C12C C13C H13C 120.0 . . ? C14C C13C H13C 120.0 . . ? C15C C14C C13C 120.0 . . ? C15C C14C H14C 120.0 . . ? C13C C14C H14C 120.0 . . ? C16C C15C C14C 120.0 . . ? C16C C15C H15C 120.0 . . ? C14C C15C H15C 120.0 . . ? C15C C16C N11C 120.0 . . ? C15C C16C H16C 120.0 . . ? N11C C16C H16C 120.0 . . ? N22C N21C C25C 106.3(4) . . ? N22C N21C C26C 121.7(4) . . ? C25C N21C C26C 131.6(5) . . ? N21C N22C C23C 108.0 . . ? N21C N22C Ru1 138.1(2) . . ? C23C N22C Ru1 113.9(2) . . ? C12C C23C C24C 134.4(3) . . ? C12C C23C N22C 117.5(3) . . ? C24C C23C N22C 108.0 . . ? C23C C24C C25C 108.4(3) . . ? C23C C24C H24C 125.8 . . ? C25C C24C H24C 125.8 . . ? C24C C25C N21C 109.2(6) . . ? C24C C25C H25C 125.4 . . ? N21C C25C H25C 125.4 . . ? N21C C26C H26G 109.5 . . ? N21C C26C H26H 109.5 . . ? H26G C26C H26H 109.5 . . ? N21C C26C H26I 109.5 . . ? H26G C26C H26I 109.5 . . ? H26H C26C H26I 109.5 . . ? F3A P1 F5A 102.0(11) . . ? F3A P1 F4A 97.8(13) . . ? F5A P1 F4A 97.9(12) . . ? F3A P1 F2 138.5(12) . . ? F5A P1 F2 68.8(8) . . ? F4A P1 F2 123.2(10) . . ? F3A P1 F4 83.4(7) . . ? F5A P1 F4 164.8(11) . . ? F4A P1 F4 95.3(11) . . ? F2 P1 F4 97.8(6) . . ? F3A P1 F3 44.1(10) . . ? F5A P1 F3 83.3(10) . . ? F4A P1 F3 140.3(10) . . ? F2 P1 F3 94.4(6) . . ? F4 P1 F3 91.1(7) . . ? F3A P1 F5 131.2(11) . . ? F5A P1 F5 94.9(10) . . ? F4A P1 F5 34.1(8) . . ? F2 P1 F5 90.4(5) . . ? F4 P1 F5 92.0(7) . . ? F3 P1 F5 173.9(5) . . ? F3A P1 F6 43.5(10) . . ? F5A P1 F6 107.6(8) . . ? F4A P1 F6 54.3(9) . . ? F2 P1 F6 175.7(4) . . ? F4 P1 F6 86.2(6) . . ? F3 P1 F6 87.2(5) . . ? F5 P1 F6 87.8(5) . . ? F3A P1 F2A 93.8(12) . . ? F5A P1 F2A 89.6(11) . . ? F4A P1 F2A 164.6(11) . . ? F2 P1 F2A 47.5(8) . . ? F4 P1 F2A 75.8(10) . . ? F3 P1 F2A 53.8(7) . . ? F5 P1 F2A 132.1(8) . . ? F6 P1 F2A 135.8(9) . . ? F3A P1 F1 90.0(6) . . ? F5A P1 F1 22.5(7) . . ? F4A P1 F1 80.8(8) . . ? F2 P1 F1 90.4(4) . . ? F4 P1 F1 171.8(6) . . ? F3 P1 F1 87.3(4) . . ? F5 P1 F1 88.9(5) . . ? F6 P1 F1 85.7(4) . . ? F2A P1 F1 109.4(8) . . ? F3A P1 F1A 170.1(8) . . ? F5A P1 F1A 87.2(10) . . ? F4A P1 F1A 84.3(11) . . ? F2 P1 F1A 42.0(7) . . ? F4 P1 F1A 86.8(7) . . ? F3 P1 F1A 135.3(9) . . ? F5 P1 F1A 50.2(7) . . ? F6 P1 F1A 137.0(8) . . ? F2A P1 F1A 82.6(10) . . ? F1 P1 F1A 99.9(6) . . ? F3A P1 F6A 94.5(9) . . ? F5A P1 F6A 158.9(13) . . ? F4A P1 F6A 92.9(16) . . ? F2 P1 F6A 90.1(11) . . ? F4 P1 F6A 11.1(11) . . ? F3 P1 F6A 99.9(11) . . ? F5 P1 F6A 83.9(12) . . ? F6 P1 F6A 93.5(11) . . ? F2A P1 F6A 76.0(15) . . ? F1 P1 F6A 172.8(12) . . ? F1A P1 F6A 75.8(9) . . ? F24 P2 F22 91.3(3) . . ? F24 P2 F23 89.9(2) . . ? F22 P2 F23 90.7(2) . . ? F24 P2 F21 178.8(3) . . ? F22 P2 F21 89.9(2) . . ? F23 P2 F21 90.07(19) . . ? F24 P2 F25 90.2(3) . . ? F22 P2 F25 178.5(3) . . ? F23 P2 F25 89.5(2) . . ? F21 P2 F25 88.6(2) . . ? F24 P2 F26 90.0(2) . . ? F22 P2 F26 90.4(2) . . ? F23 P2 F26 178.9(2) . . ? F21 P2 F26 90.0(2) . . ? F25 P2 F26 89.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11C Ru1 N11A C16A -91.7(5) . . . . ? N22A Ru1 N11A C16A -178.8(5) . . . . ? N22B Ru1 N11A C16A 8.6(5) . . . . ? N22C Ru1 N11A C16A -98.3(12) . . . . ? N11B Ru1 N11A C16A 85.9(5) . . . . ? N11C Ru1 N11A C12A 86.0(4) . . . . ? N22A Ru1 N11A C12A -1.1(3) . . . . ? N22B Ru1 N11A C12A -173.7(3) . . . . ? N22C Ru1 N11A C12A 79.4(11) . . . . ? N11B Ru1 N11A C12A -96.4(4) . . . . ? C16A N11A C12A C13A 1.4(7) . . . . ? Ru1 N11A C12A C13A -176.5(4) . . . . ? C16A N11A C12A C23A 178.9(5) . . . . ? Ru1 N11A C12A C23A 1.0(5) . . . . ? N11A C12A C13A C14A -0.6(8) . . . . ? C23A C12A C13A C14A -177.7(5) . . . . ? C12A C13A C14A C15A 0.0(10) . . . . ? C13A C14A C15A C16A -0.3(10) . . . . ? C12A N11A C16A C15A -1.8(9) . . . . ? Ru1 N11A C16A C15A 175.9(5) . . . . ? C14A C15A C16A N11A 1.2(10) . . . . ? C25A N21A N22A C23A 0.7(5) . . . . ? C26A N21A N22A C23A -179.4(4) . . . . ? C25A N21A N22A Ru1 -178.8(4) . . . . ? C26A N21A N22A Ru1 1.2(7) . . . . ? N11C Ru1 N22A C23A -93.9(3) . . . . ? N22B Ru1 N22A C23A 48.4(10) . . . . ? N22C Ru1 N22A C23A -170.6(3) . . . . ? N11A Ru1 N22A C23A 1.0(3) . . . . ? N11B Ru1 N22A C23A 87.2(3) . . . . ? N11C Ru1 N22A N21A 85.5(4) . . . . ? N22B Ru1 N22A N21A -132.2(8) . . . . ? N22C Ru1 N22A N21A 8.8(5) . . . . ? N11A Ru1 N22A N21A -179.6(5) . . . . ? N11B Ru1 N22A N21A -93.4(4) . . . . ? N21A N22A C23A C24A -0.7(5) . . . . ? Ru1 N22A C23A C24A 178.9(3) . . . . ? N21A N22A C23A C12A 179.6(4) . . . . ? Ru1 N22A C23A C12A -0.9(5) . . . . ? N11A C12A C23A N22A -0.1(6) . . . . ? C13A C12A C23A N22A 177.2(5) . . . . ? N11A C12A C23A C24A -179.7(5) . . . . ? C13A C12A C23A C24A -2.4(9) . . . . ? N22A C23A C24A C25A 0.5(6) . . . . ? C12A C23A C24A C25A -179.9(5) . . . . ? N22A N21A C25A C24A -0.4(6) . . . . ? C26A N21A C25A C24A 179.6(5) . . . . ? C23A C24A C25A N21A 0.0(6) . . . . ? N11C Ru1 N11B C16B -152(3) . . . . ? N22A Ru1 N11B C16B 5.8(5) . . . . ? N22B Ru1 N11B C16B 179.4(5) . . . . ? N22C Ru1 N11B C16B -95.9(4) . . . . ? N11A Ru1 N11B C16B 83.4(4) . . . . ? N11C Ru1 N11B C12B 31(3) . . . . ? N22A Ru1 N11B C12B -171.3(3) . . . . ? N22B Ru1 N11B C12B 2.4(3) . . . . ? N22C Ru1 N11B C12B 87.0(4) . . . . ? N11A Ru1 N11B C12B -93.6(4) . . . . ? C16B N11B C12B C13B -0.4(7) . . . . ? Ru1 N11B C12B C13B 176.9(4) . . . . ? C16B N11B C12B C23B 178.6(5) . . . . ? Ru1 N11B C12B C23B -4.1(5) . . . . ? N11B C12B C13B C14B -0.6(9) . . . . ? C23B C12B C13B C14B -179.4(6) . . . . ? C12B C13B C14B C15B 1.2(10) . . . . ? C13B C14B C15B C16B -1.0(11) . . . . ? C12B N11B C16B C15B 0.7(9) . . . . ? Ru1 N11B C16B C15B -176.3(5) . . . . ? C14B C15B C16B N11B 0.0(10) . . . . ? C25B N21B N22B C23B 0.7(5) . . . . ? C26B N21B N22B C23B 178.1(5) . . . . ? C25B N21B N22B Ru1 -175.3(4) . . . . ? C26B N21B N22B Ru1 2.2(8) . . . . ? N11C Ru1 N22B N21B -2.9(5) . . . . ? N22A Ru1 N22B N21B -144.6(8) . . . . ? N22C Ru1 N22B N21B 73.7(5) . . . . ? N11A Ru1 N22B N21B -98.3(5) . . . . ? N11B Ru1 N22B N21B 175.7(5) . . . . ? N11C Ru1 N22B C23B -178.6(3) . . . . ? N22A Ru1 N22B C23B 39.7(10) . . . . ? N22C Ru1 N22B C23B -102.0(3) . . . . ? N11A Ru1 N22B C23B 86.0(3) . . . . ? N11B Ru1 N22B C23B 0.0(3) . . . . ? N21B N22B C23B C24B -0.3(5) . . . . ? Ru1 N22B C23B C24B 176.7(3) . . . . ? N21B N22B C23B C12B -179.2(4) . . . . ? Ru1 N22B C23B C12B -2.2(5) . . . . ? N11B C12B C23B N22B 4.2(6) . . . . ? C13B C12B C23B N22B -176.9(5) . . . . ? N11B C12B C23B C24B -174.5(5) . . . . ? C13B C12B C23B C24B 4.5(9) . . . . ? N22B C23B C24B C25B -0.2(6) . . . . ? C12B C23B C24B C25B 178.5(5) . . . . ? N22B N21B C25B C24B -0.8(6) . . . . ? C26B N21B C25B C24B -178.1(5) . . . . ? C23B C24B C25B N21B 0.6(6) . . . . ? N22A Ru1 N11C C12C -100.9(2) . . . . ? N22B Ru1 N11C C12C 85.3(2) . . . . ? N22C Ru1 N11C C12C 0.4(2) . . . . ? N11A Ru1 N11C C12C -178.6(2) . . . . ? N11B Ru1 N11C C12C 57(3) . . . . ? N22A Ru1 N11C C16C 81.8(3) . . . . ? N22B Ru1 N11C C16C -92.0(2) . . . . ? N22C Ru1 N11C C16C -176.9(3) . . . . ? N11A Ru1 N11C C16C 4.0(3) . . . . ? N11B Ru1 N11C C16C -121(3) . . . . ? C16C N11C C12C C23C 178.6(4) . . . . ? Ru1 N11C C12C C23C 1.1(4) . . . . ? C16C N11C C12C C13C 0.0 . . . . ? Ru1 N11C C12C C13C -177.4(3) . . . . ? C23C C12C C13C C14C -178.4(5) . . . . ? N11C C12C C13C C14C 0.0 . . . . ? C12C C13C C14C C15C 0.0 . . . . ? C13C C14C C15C C16C 0.0 . . . . ? C14C C15C C16C N11C 0.0 . . . . ? C12C N11C C16C C15C 0.0 . . . . ? Ru1 N11C C16C C15C 177.3(3) . . . . ? C25C N21C N22C C23C 0.0(4) . . . . ? C26C N21C N22C C23C 173.4(6) . . . . ? C25C N21C N22C Ru1 179.6(4) . . . . ? C26C N21C N22C Ru1 -7.0(8) . . . . ? N11C Ru1 N22C N21C 178.6(4) . . . . ? N22A Ru1 N22C N21C -95.8(4) . . . . ? N22B Ru1 N22C N21C 77.9(4) . . . . ? N11A Ru1 N22C N21C -174.7(10) . . . . ? N11B Ru1 N22C N21C 1.0(4) . . . . ? N11C Ru1 N22C C23C -1.8(2) . . . . ? N22A Ru1 N22C C23C 83.8(2) . . . . ? N22B Ru1 N22C C23C -102.5(2) . . . . ? N11A Ru1 N22C C23C 4.9(12) . . . . ? N11B Ru1 N22C C23C -179.3(2) . . . . ? C13C C12C C23C C24C -0.5(7) . . . . ? N11C C12C C23C C24C -179.0(4) . . . . ? C13C C12C C23C N22C 175.7(3) . . . . ? N11C C12C C23C N22C -2.7(4) . . . . ? N21C N22C C23C C12C -177.2(5) . . . . ? Ru1 N22C C23C C12C 3.1(4) . . . . ? N21C N22C C23C C24C 0.0 . . . . ? Ru1 N22C C23C C24C -179.7(3) . . . . ? C12C C23C C24C C25C 176.5(6) . . . . ? N22C C23C C24C C25C 0.0(4) . . . . ? C23C C24C C25C N21C -0.1(7) . . . . ? N22C N21C C25C C24C 0.1(7) . . . . ? C26C N21C C25C C24C -172.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.858 _refine_diff_density_min -1.737 _refine_diff_density_rms 0.111 #===END _database_code_depnum_ccdc_archive 'CCDC 960002'