data_publication_text ##=========================================================================== ##== This CIF corresponds to a manuscript being submitted to ##== Organometallics ##=========================================================================== ##== Crystal structure deposit codes CCDC 833091-833092 _publ_requested_journal 'Chemistry: Organometallics' _publ_contact_author_name 'Pedro Valerga' _publ_contact_author_address ; Departamento de CMIM y Qu\'imica Inorg\'anica Universidad de C\'adiz Facultad de Ciencias Campus Universitario del R\'io San Pedro 11510. Puerto Real. SPAIN. ; _publ_contact_author_email pedro.valerga@uca.es _publ_contact_author_phone '34 (956) 016340' _publ_contact_author_fax '34 (956) 016288' loop_ _publ_author_name _publ_author_address 'Fern\'andez, Francys E.' ; Departamento de CMIM y Qu\'imica Inorg\'anica Universidad de C\'adiz Facultad de Ciencias Campus Universitario del R\'io San Pedro 11510. Puerto Real. SPAIN. ; 'Puerta, M.Carmen' ; Departamento de CMIM y Qu\'imica Inorg\'anica Universidad de C\'adiz Facultad de Ciencias Campus Universitario del R\'io San Pedro 11510. Puerto Real. SPAIN. ; 'Valerga, Pedro' ; Departamento de CMIM y Qu\'imica Inorg\'anica Universidad de C\'adiz Facultad de Ciencias Campus Universitario del R\'io San Pedro 11510. Puerto Real. SPAIN. ; _publ_contact_letter ; Please consider this CIF submission for publication in Organometallics Title: New Half-Sandwich Ruthenium (II) Picolyl-NHC Complexes: Synthesis, Characterization and Catalytic Activity in Transfer Hydrogenation Reactions Authors:Francys E. Fern\'andez, M. Carmen Puerta, Pedro Valerga. Yours sincerely, Pedro Valerga July, 2011 ; ##============================================================ ##=== 2 CIFs follow corresponding to ##=== data_pv0925 ==== CCDC 833091 == (Compound 2a in the text) ##=== data_pv1018 ==== CCDC 833092 == (Compound 3b in the text) ##============================================================ ##=== data_pv0925 ==== CCDC 833091 == (Compound 2a in the text) data_pv0925 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Acetonitrile- {3-(methyl)-1-(pyrid-2-ylmethyl)-2,3-dihydro-imidazole-2-ylidene-\k^2^ C,N} (pentahapto-pentamethyl-cyclopentadienyl)-ruthenium (II) tetrakis{3,5-bis(trifluoromethyl)phenyl}borate ; _chemical_name_common ? _chemical_formula_moiety 'C32 H12 B F24, C22 H29 N4 Ru' _chemical_formula_sum 'C54 H41 B F24 N4 Ru' _chemical_melting_point ? _exptl_crystal_description plate _exptl_crystal_colour orange _diffrn_ambient_temperature 100(2) _chemical_formula_weight 1313.79 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' B B 0.0013 0.0007 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.427(3) _cell_length_b 12.814(3) _cell_length_c 17.884(4) _cell_angle_alpha 91.85(3) _cell_angle_beta 100.30(3) _cell_angle_gamma 104.44(3) _cell_volume 2704.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2888 _cell_measurement_theta_min 2.257 _cell_measurement_theta_max 22.577 _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _exptl_special_details ; Bruker SMART APEX 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. A hemisphere of the reciprocal space up to theta(max) = 25.09 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 10 sec per frame, 1700 frames were recorded using program SMART (Bruker). Frame data evaluation and integration were done with program SAINT+(Bruker); Lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections with program SAINT + (Bruker). Correction for absorption and crystal decay (insignificant) were applied by semi-empirical method from equivalents using program SADABS (G.M. Sheldrick, version of 2001, Univ. of Goettingen, Germany). Data reduction was done with program XPREP (BRUKER). ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '1700 omega scan frames, 0.3 deg, 10 sec' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.0026 _diffrn_reflns_number 18176 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.09 _reflns_number_total 9179 _reflns_number_gt 7324 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 vers. 1.08 (Farrugia, 2005)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.1054P)^2^+2.8168P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary vecmap _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 9179 _refine_ls_number_parameters 784 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1783 _refine_ls_wR_factor_gt 0.1670 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.97063(3) 0.77412(3) 0.66406(2) 0.02568(15) Uani 1 1 d . . . N1 N 0.8290(4) 0.7438(4) 0.5743(3) 0.0391(11) Uani 1 1 d . . . N2 N 0.8175(4) 0.9223(4) 0.6769(3) 0.0397(11) Uani 1 1 d . . . N3 N 0.8783(4) 0.8801(4) 0.7888(3) 0.0467(13) Uani 1 1 d . . . N4 N 0.8939(4) 0.6486(4) 0.7203(3) 0.0422(12) Uani 1 1 d . . . C1 C 1.1420(4) 0.8654(4) 0.7136(3) 0.0274(11) Uani 1 1 d . . . C2 C 1.1115(4) 0.8939(4) 0.6374(3) 0.0243(10) Uani 1 1 d . . . C3 C 1.0914(4) 0.7994(4) 0.5868(3) 0.0272(11) Uani 1 1 d . . . C4 C 1.1080(4) 0.7113(4) 0.6314(3) 0.0268(11) Uani 1 1 d . . . C5 C 1.1382(4) 0.7530(4) 0.7094(3) 0.0304(11) Uani 1 1 d . . . C6 C 1.1804(4) 0.9436(4) 0.7829(3) 0.0359(13) Uani 1 1 d . . . H6A H 1.1836 0.9037 0.8287 0.054 Uiso 1 1 calc R . . H6B H 1.1269 0.9883 0.7833 0.054 Uiso 1 1 calc R . . H6C H 1.2558 0.9901 0.7820 0.054 Uiso 1 1 calc R . . C7 C 1.1176(4) 1.0074(4) 0.6154(3) 0.0354(13) Uani 1 1 d . . . H7A H 1.1971 1.0472 0.6197 0.053 Uiso 1 1 calc R . . H7B H 1.0824 1.0437 0.6496 0.053 Uiso 1 1 calc R . . H7C H 1.0775 1.0050 0.5627 0.053 Uiso 1 1 calc R . . C8 C 1.0625(4) 0.7950(4) 0.5018(3) 0.0335(12) Uani 1 1 d . . . H8A H 1.0137 0.8431 0.4866 0.050 Uiso 1 1 calc R . . H8B H 1.0227 0.7207 0.4814 0.050 Uiso 1 1 calc R . . H8C H 1.1323 0.8181 0.4815 0.050 Uiso 1 1 calc R . . C9 C 1.1048(5) 0.6008(4) 0.6011(3) 0.0399(13) Uani 1 1 d . . . H9A H 1.0610 0.5865 0.5489 0.060 Uiso 1 1 calc R . . H9B H 1.0692 0.5475 0.6333 0.060 Uiso 1 1 calc R . . H9C H 1.1822 0.5956 0.6012 0.060 Uiso 1 1 calc R . . C10 C 1.1683(5) 0.6881(5) 0.7747(3) 0.0391(13) Uani 1 1 d . . . H10A H 1.2472 0.6852 0.7792 0.059 Uiso 1 1 calc R . . H10B H 1.1185 0.6145 0.7654 0.059 Uiso 1 1 calc R . . H10C H 1.1586 0.7221 0.8220 0.059 Uiso 1 1 calc R . . C11 C 0.8695(5) 0.5783(6) 0.7558(4) 0.0530(17) Uani 1 1 d . . . C12 C 0.8412(6) 0.4980(6) 0.8104(5) 0.078(3) Uani 1 1 d . . . H12A H 0.8365 0.5346 0.8582 0.117 Uiso 1 1 calc R . . H12B H 0.9001 0.4589 0.8202 0.117 Uiso 1 1 calc R . . H12C H 0.7681 0.4469 0.7894 0.117 Uiso 1 1 calc R . . C13 C 0.7969(5) 0.6523(5) 0.5314(3) 0.0439(15) Uani 1 1 d . . . H13 H 0.8379 0.6002 0.5455 0.053 Uiso 1 1 calc R . . C14 C 0.7111(6) 0.6231(6) 0.4686(4) 0.0522(16) Uani 1 1 d . . . H14 H 0.6941 0.5552 0.4402 0.063 Uiso 1 1 calc R . . C15 C 0.6522(5) 0.6974(5) 0.4498(4) 0.0509(16) Uani 1 1 d . . . H15 H 0.5923 0.6816 0.4065 0.061 Uiso 1 1 calc R . . C16 C 0.6769(5) 0.7960(5) 0.4919(3) 0.0428(14) Uani 1 1 d . . . H16 H 0.6328 0.8458 0.4788 0.051 Uiso 1 1 calc R . . C17 C 0.7663(4) 0.8209(5) 0.5533(3) 0.0383(13) Uani 1 1 d . . . C18 C 0.8029(5) 0.9293(5) 0.5960(3) 0.0415(14) Uani 1 1 d . . . H18A H 0.8754 0.9700 0.5833 0.050 Uiso 1 1 calc R . . H18B H 0.7457 0.9698 0.5798 0.050 Uiso 1 1 calc R . . C19 C 0.8850(4) 0.8662(4) 0.7145(3) 0.0328(12) Uani 1 1 d . . . C20 C 0.8028(6) 0.9450(6) 0.7966(4) 0.0614(19) Uani 1 1 d . . . H20 H 0.7827 0.9658 0.8426 0.074 Uiso 1 1 calc R . . C21 C 0.7657(5) 0.9711(6) 0.7269(4) 0.0558(18) Uani 1 1 d . . . H21 H 0.7143 1.0143 0.7136 0.067 Uiso 1 1 calc R . . C22 C 0.9331(6) 0.8331(6) 0.8520(4) 0.065(2) Uani 1 1 d . . . H22A H 0.8787 0.7703 0.8653 0.098 Uiso 1 1 calc R . . H22B H 0.9611 0.8868 0.8959 0.098 Uiso 1 1 calc R . . H22C H 0.9967 0.8102 0.8376 0.098 Uiso 1 1 calc R . . F1 F 0.7036(4) 0.3749(3) 0.5242(2) 0.0684(12) Uani 1 1 d . . . F2 F 0.6987(4) 0.2304(3) 0.5779(3) 0.0752(14) Uani 1 1 d . . . F3 F 0.8296(3) 0.3742(4) 0.6199(3) 0.0850(15) Uani 1 1 d . . . F4 F 0.4389(4) 0.6034(3) 0.6995(3) 0.0909(17) Uani 1 1 d . . . F5 F 0.5624(6) 0.6562(4) 0.6331(4) 0.128(3) Uani 1 1 d . . . F6 F 0.6035(5) 0.6698(4) 0.7492(4) 0.124(2) Uani 1 1 d . . . F7A F 0.9432(7) 0.2579(11) 1.0289(3) 0.117(4) Uani 0.731(6) 1 d P A 1 F8A F 0.9740(5) 0.3354(7) 0.9312(7) 0.103(3) Uani 0.731(6) 1 d P A 1 F9A F 0.8869(4) 0.1748(5) 0.9195(5) 0.086(3) Uani 0.731(6) 1 d P A 1 F10 F 0.5625(4) 0.4553(3) 1.0809(2) 0.0556(10) Uani 1 1 d . B 1 F11 F 0.6695(3) 0.5770(3) 1.0324(2) 0.0602(10) Uani 1 1 d . B 1 F12 F 0.7403(4) 0.4962(4) 1.1228(2) 0.101(2) Uani 1 1 d . B 1 F13 F 0.2181(3) 0.0368(3) 0.9745(2) 0.0518(9) Uani 1 1 d . C 1 F14 F 0.0766(3) 0.1035(4) 0.9603(2) 0.0723(13) Uani 1 1 d . C 1 F15 F 0.2346(4) 0.1910(3) 1.0274(2) 0.0736(12) Uani 1 1 d . C 1 F16 F 0.0593(3) 0.3718(3) 0.7482(2) 0.0620(11) Uani 1 1 d . D 1 F17 F -0.0001(3) 0.2124(3) 0.6948(2) 0.0576(10) Uani 1 1 d . D 1 F18 F 0.1321(3) 0.3249(4) 0.6581(2) 0.0738(13) Uani 1 1 d . D 1 F19A F 0.5528(5) -0.0948(3) 0.9525(3) 0.0542(13) Uani 0.832(6) 1 d P E 1 F20A F 0.3804(4) -0.1610(5) 0.9164(3) 0.0733(18) Uani 0.832(6) 1 d P E 1 F21A F 0.4904(8) -0.2370(4) 0.8729(3) 0.095(3) Uani 0.832(6) 1 d P E 1 F22 F 0.5124(3) -0.0741(3) 0.58417(18) 0.0496(9) Uani 1 1 d . . . F23 F 0.3700(3) -0.1971(2) 0.60239(18) 0.0446(8) Uani 1 1 d . . . F24 F 0.3477(3) -0.0454(2) 0.56587(16) 0.0389(7) Uani 1 1 d . . . F7B F 0.8848(17) 0.173(3) 0.9826(11) 0.117(4) Uani 0.269(6) 1 d P A 2 F8B F 0.9783(16) 0.3274(18) 1.007(2) 0.103(3) Uani 0.269(6) 1 d P A 2 F9B F 0.9289(15) 0.274(2) 0.8986(14) 0.086(3) Uani 0.269(6) 1 d P A 2 F19B F 0.5894(19) -0.1816(18) 0.8890(12) 0.0542(13) Uani 0.168(6) 1 d P E 2 F20B F 0.492(3) -0.106(3) 0.949(2) 0.0733(18) Uani 0.168(6) 1 d P E 2 F21B F 0.407(4) -0.224(2) 0.8819(15) 0.095(3) Uani 0.168(6) 1 d P E 2 C23 C 0.5405(4) 0.3198(4) 0.7451(3) 0.0207(10) Uani 1 1 d . . . C24 C 0.6071(4) 0.2955(4) 0.6945(3) 0.0231(10) Uani 1 1 d . . . H24 H 0.6249 0.2276 0.6954 0.028 Uiso 1 1 calc R . . C25 C 0.6473(4) 0.3665(4) 0.6438(3) 0.0281(11) Uani 1 1 d . . . C26 C 0.6247(4) 0.4670(4) 0.6404(3) 0.0304(11) Uani 1 1 d . . . H26 H 0.6510 0.5153 0.6045 0.036 Uiso 1 1 calc R . . C27 C 0.5624(4) 0.4944(4) 0.6913(3) 0.0272(11) Uani 1 1 d . . . C28 C 0.5217(4) 0.4233(4) 0.7424(3) 0.0260(11) Uani 1 1 d . . . H28 H 0.4798 0.4452 0.7767 0.031 Uiso 1 1 calc R . . C29 C 0.7187(5) 0.3361(5) 0.5921(3) 0.0410(14) Uani 1 1 d . . . C30 C 0.5398(5) 0.6044(4) 0.6905(4) 0.0446(15) Uani 1 1 d . . . C31 C 0.5948(4) 0.2828(4) 0.8860(3) 0.0221(10) Uani 1 1 d . . . C32 C 0.6991(4) 0.2555(4) 0.8937(3) 0.0249(10) Uani 1 1 d . . . H32 H 0.7092 0.2058 0.8566 0.030 Uiso 1 1 calc R . . C33 C 0.7869(4) 0.2995(4) 0.9542(3) 0.0320(12) Uani 1 1 d . A . C34 C 0.7767(4) 0.3721(4) 1.0091(3) 0.0309(12) Uani 1 1 d . . . H34 H 0.8373 0.4020 1.0506 0.037 Uiso 1 1 calc R . . C35 C 0.6748(4) 0.4000(4) 1.0018(3) 0.0308(12) Uani 1 1 d . B . C36 C 0.5864(4) 0.3564(4) 0.9418(3) 0.0272(11) Uani 1 1 d . . . H36 H 0.5177 0.3773 0.9387 0.033 Uiso 1 1 calc R . . C37 C 0.8943(5) 0.2681(6) 0.9596(4) 0.0458(15) Uani 1 1 d . . . C38 C 0.6626(5) 0.4815(5) 1.0597(3) 0.0427(15) Uani 1 1 d . . . C39 C 0.3706(4) 0.2384(4) 0.8212(3) 0.0208(10) Uani 1 1 d . . . C40 C 0.3319(4) 0.1939(4) 0.8851(3) 0.0228(10) Uani 1 1 d . . . H40 H 0.3842 0.1735 0.9236 0.027 Uiso 1 1 calc R . . C41 C 0.2207(4) 0.1783(4) 0.8946(3) 0.0253(10) Uani 1 1 d . C . C42 C 0.1428(4) 0.2108(4) 0.8401(3) 0.0273(11) Uani 1 1 d . . . H42 H 0.0669 0.2018 0.8465 0.033 Uiso 1 1 calc R . . C43 C 0.1777(4) 0.2559(4) 0.7773(3) 0.0245(10) Uani 1 1 d . D . C44 C 0.2891(4) 0.2677(4) 0.7669(3) 0.0235(10) Uani 1 1 d . . . H44 H 0.3102 0.2964 0.7218 0.028 Uiso 1 1 calc R . . C45 C 0.1868(4) 0.1292(5) 0.9633(3) 0.0393(13) Uani 1 1 d . . . C46 C 0.0943(4) 0.2917(5) 0.7198(3) 0.0344(12) Uani 1 1 d . . . C47 C 0.4878(4) 0.1108(4) 0.7850(3) 0.0213(10) Uani 1 1 d . . . C48 C 0.4986(4) 0.0394(4) 0.8425(3) 0.0230(10) Uani 1 1 d . . . H48 H 0.5212 0.0677 0.8942 0.028 Uiso 1 1 calc R . . C49 C 0.4772(4) -0.0706(4) 0.8255(3) 0.0253(10) Uani 1 1 d . E . C50 C 0.4497(4) -0.1154(4) 0.7511(3) 0.0259(11) Uani 1 1 d . . . H50 H 0.4384 -0.1908 0.7399 0.031 Uiso 1 1 calc R . . C51 C 0.4392(4) -0.0474(4) 0.6938(3) 0.0236(10) Uani 1 1 d . . . C52 C 0.4563(4) 0.0630(4) 0.7108(3) 0.0212(10) Uani 1 1 d . . . H52 H 0.4461 0.1075 0.6700 0.025 Uiso 1 1 calc R . . C53 C 0.4817(5) -0.1415(5) 0.8895(4) 0.0418(14) Uani 1 1 d . . . C54 C 0.4167(4) -0.0908(4) 0.6127(3) 0.0300(11) Uani 1 1 d . . . B1 B 0.4972(4) 0.2381(4) 0.8084(3) 0.0212(11) 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 0.0189(2) 0.0309(3) 0.0274(2) 0.00190(16) 0.00621(15) 0.00546(16) N1 0.022(2) 0.059(3) 0.031(3) 0.000(2) 0.0065(18) 0.001(2) N2 0.024(2) 0.045(3) 0.052(3) 0.002(2) 0.008(2) 0.011(2) N3 0.046(3) 0.051(3) 0.049(3) -0.001(2) 0.024(2) 0.013(2) N4 0.024(2) 0.036(3) 0.065(3) 0.020(3) 0.014(2) 0.001(2) C1 0.015(2) 0.030(3) 0.037(3) 0.000(2) 0.004(2) 0.006(2) C2 0.019(2) 0.026(3) 0.027(3) 0.005(2) 0.0071(19) 0.0021(19) C3 0.016(2) 0.033(3) 0.033(3) 0.005(2) 0.009(2) 0.006(2) C4 0.017(2) 0.024(3) 0.039(3) -0.002(2) 0.005(2) 0.005(2) C5 0.019(2) 0.032(3) 0.040(3) 0.002(2) 0.010(2) 0.004(2) C6 0.024(3) 0.045(3) 0.034(3) -0.005(2) 0.004(2) 0.002(2) C7 0.028(3) 0.030(3) 0.051(3) 0.002(2) 0.012(2) 0.010(2) C8 0.030(3) 0.042(3) 0.030(3) 0.005(2) 0.006(2) 0.011(2) C9 0.040(3) 0.034(3) 0.052(4) 0.004(3) 0.016(3) 0.015(3) C10 0.035(3) 0.043(3) 0.037(3) 0.015(3) 0.002(2) 0.010(3) C11 0.030(3) 0.062(4) 0.053(4) 0.022(3) -0.003(3) -0.009(3) C12 0.044(4) 0.058(5) 0.106(6) 0.053(4) -0.016(4) -0.017(3) C13 0.044(3) 0.040(3) 0.045(4) 0.004(3) 0.023(3) -0.002(3) C14 0.056(4) 0.057(4) 0.044(4) 0.010(3) 0.012(3) 0.012(3) C15 0.045(4) 0.058(4) 0.049(4) 0.011(3) 0.014(3) 0.007(3) C16 0.037(3) 0.052(4) 0.041(3) 0.014(3) 0.009(3) 0.014(3) C17 0.025(3) 0.058(4) 0.036(3) 0.015(3) 0.009(2) 0.013(3) C18 0.029(3) 0.038(3) 0.056(4) 0.002(3) 0.005(3) 0.009(2) C19 0.019(3) 0.032(3) 0.046(3) 0.004(2) 0.009(2) 0.003(2) C20 0.057(4) 0.071(5) 0.063(5) -0.004(4) 0.026(4) 0.019(4) C21 0.031(3) 0.062(4) 0.080(5) -0.014(4) 0.018(3) 0.018(3) C22 0.064(5) 0.078(5) 0.063(5) 0.011(4) 0.027(4) 0.024(4) F1 0.104(3) 0.069(3) 0.051(2) 0.0118(19) 0.052(2) 0.030(2) F2 0.115(4) 0.033(2) 0.102(3) 0.007(2) 0.085(3) 0.019(2) F3 0.040(2) 0.131(4) 0.088(3) -0.030(3) 0.029(2) 0.021(2) F4 0.065(3) 0.043(2) 0.194(5) 0.043(3) 0.065(3) 0.036(2) F5 0.230(7) 0.079(3) 0.157(5) 0.087(4) 0.149(5) 0.105(4) F6 0.131(5) 0.041(3) 0.185(6) -0.036(3) -0.026(4) 0.037(3) F7A 0.083(5) 0.279(12) 0.032(3) 0.011(4) -0.003(3) 0.135(7) F8A 0.039(3) 0.103(5) 0.190(10) 0.047(7) 0.061(5) 0.027(3) F9A 0.031(3) 0.080(4) 0.143(7) -0.048(4) -0.015(3) 0.035(3) F10 0.088(3) 0.042(2) 0.046(2) -0.0029(16) 0.0262(19) 0.0250(19) F11 0.073(3) 0.0242(18) 0.085(3) -0.0063(18) 0.021(2) 0.0121(17) F12 0.112(4) 0.116(4) 0.070(3) -0.065(3) -0.058(3) 0.084(3) F13 0.052(2) 0.063(2) 0.054(2) 0.0325(18) 0.0266(17) 0.0252(18) F14 0.033(2) 0.124(4) 0.076(3) 0.061(3) 0.0295(18) 0.030(2) F15 0.103(3) 0.081(3) 0.036(2) 0.004(2) 0.032(2) 0.009(2) F16 0.070(3) 0.063(2) 0.061(2) -0.0050(19) -0.0119(19) 0.048(2) F17 0.0364(19) 0.056(2) 0.068(2) 0.0083(18) -0.0176(17) 0.0083(17) F18 0.045(2) 0.142(4) 0.049(2) 0.052(2) 0.0133(18) 0.043(2) F19A 0.059(3) 0.043(2) 0.044(2) 0.0180(18) -0.023(2) 0.005(2) F20A 0.053(3) 0.102(4) 0.064(3) 0.057(3) 0.015(2) 0.011(3) F21A 0.229(10) 0.033(3) 0.048(3) 0.020(2) 0.042(4) 0.070(4) F22 0.0322(17) 0.074(2) 0.0430(19) -0.0092(17) 0.0172(14) 0.0090(16) F23 0.063(2) 0.0249(17) 0.0399(18) -0.0066(13) 0.0061(16) 0.0047(15) F24 0.0452(18) 0.0402(18) 0.0318(17) -0.0006(13) 0.0004(14) 0.0176(15) F7B 0.083(5) 0.279(12) 0.032(3) 0.011(4) -0.003(3) 0.135(7) F8B 0.039(3) 0.103(5) 0.190(10) 0.047(7) 0.061(5) 0.027(3) F9B 0.031(3) 0.080(4) 0.143(7) -0.048(4) -0.015(3) 0.035(3) F19B 0.059(3) 0.043(2) 0.044(2) 0.0180(18) -0.023(2) 0.005(2) F20B 0.053(3) 0.102(4) 0.064(3) 0.057(3) 0.015(2) 0.011(3) F21B 0.229(10) 0.033(3) 0.048(3) 0.020(2) 0.042(4) 0.070(4) C23 0.018(2) 0.019(2) 0.024(2) 0.0015(19) 0.0067(18) 0.0023(18) C24 0.018(2) 0.023(2) 0.029(3) -0.001(2) 0.0052(19) 0.0078(19) C25 0.032(3) 0.028(3) 0.026(3) -0.002(2) 0.011(2) 0.005(2) C26 0.032(3) 0.028(3) 0.032(3) 0.008(2) 0.013(2) 0.003(2) C27 0.027(3) 0.019(2) 0.039(3) 0.008(2) 0.014(2) 0.005(2) C28 0.024(3) 0.025(3) 0.032(3) 0.001(2) 0.011(2) 0.007(2) C29 0.045(4) 0.035(3) 0.048(4) 0.004(3) 0.028(3) 0.006(3) C30 0.053(4) 0.026(3) 0.065(4) 0.011(3) 0.034(3) 0.012(3) C31 0.023(2) 0.021(2) 0.022(2) 0.0033(19) 0.0035(19) 0.0065(19) C32 0.021(2) 0.027(3) 0.029(3) 0.002(2) 0.008(2) 0.008(2) C33 0.022(3) 0.035(3) 0.037(3) 0.004(2) 0.005(2) 0.004(2) C34 0.023(3) 0.029(3) 0.035(3) 0.002(2) -0.006(2) 0.004(2) C35 0.033(3) 0.027(3) 0.030(3) -0.001(2) -0.003(2) 0.010(2) C36 0.023(3) 0.027(3) 0.034(3) 0.004(2) 0.004(2) 0.011(2) C37 0.027(3) 0.063(4) 0.050(4) 0.002(3) 0.000(3) 0.022(3) C38 0.046(4) 0.037(3) 0.040(3) -0.009(3) -0.011(3) 0.017(3) C39 0.020(2) 0.019(2) 0.022(2) -0.0045(19) 0.0019(18) 0.0047(19) C40 0.022(2) 0.025(3) 0.020(2) 0.0002(19) 0.0015(18) 0.007(2) C41 0.024(2) 0.026(3) 0.029(3) 0.003(2) 0.011(2) 0.008(2) C42 0.020(2) 0.034(3) 0.031(3) 0.000(2) 0.008(2) 0.010(2) C43 0.024(2) 0.024(3) 0.024(3) -0.004(2) 0.0008(19) 0.007(2) C44 0.027(3) 0.022(2) 0.023(2) 0.0037(19) 0.0081(19) 0.007(2) C45 0.026(3) 0.056(4) 0.041(3) 0.009(3) 0.013(2) 0.015(3) C46 0.026(3) 0.045(3) 0.036(3) 0.011(3) 0.009(2) 0.014(2) C47 0.014(2) 0.022(2) 0.031(3) 0.007(2) 0.0096(18) 0.0050(18) C48 0.020(2) 0.023(3) 0.026(3) 0.004(2) 0.0053(19) 0.0043(19) C49 0.020(2) 0.028(3) 0.028(3) 0.007(2) 0.0024(19) 0.007(2) C50 0.024(3) 0.017(2) 0.038(3) 0.005(2) 0.007(2) 0.0054(19) C51 0.015(2) 0.024(3) 0.031(3) -0.003(2) 0.0052(19) 0.0039(19) C52 0.015(2) 0.023(2) 0.027(3) 0.003(2) 0.0067(18) 0.0050(18) C53 0.045(4) 0.032(3) 0.039(4) 0.010(3) -0.002(3) -0.001(3) C54 0.026(3) 0.030(3) 0.033(3) -0.002(2) 0.006(2) 0.006(2) B1 0.019(3) 0.024(3) 0.022(3) 0.000(2) 0.006(2) 0.006(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 N4 2.047(5) . ? Ru1 C19 2.059(5) . ? Ru1 N1 2.106(4) . ? Ru1 C2 2.157(5) . ? Ru1 C1 2.169(5) . ? Ru1 C5 2.182(5) . ? Ru1 C3 2.189(5) . ? Ru1 C4 2.217(5) . ? N1 C13 1.312(7) . ? N1 C17 1.424(7) . ? N2 C19 1.343(7) . ? N2 C21 1.405(7) . ? N2 C18 1.434(8) . ? N3 C19 1.356(7) . ? N3 C20 1.421(8) . ? N3 C22 1.441(9) . ? N4 C11 1.128(7) . ? C1 C5 1.429(7) . ? C1 C2 1.431(7) . ? C1 C6 1.496(7) . ? C2 C3 1.430(7) . ? C2 C7 1.505(7) . ? C3 C4 1.438(7) . ? C3 C8 1.494(7) . ? C4 C5 1.428(7) . ? C4 C9 1.488(7) . ? C5 C10 1.502(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.465(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.373(9) . ? C13 H13 0.9500 . ? C14 C15 1.355(9) . ? C14 H14 0.9500 . ? C15 C16 1.386(9) . ? C15 H15 0.9500 . ? C16 C17 1.381(8) . ? C16 H16 0.9500 . ? C17 C18 1.486(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C20 C21 1.333(10) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? F1 C29 1.327(7) . ? F2 C29 1.323(6) . ? F3 C29 1.337(7) . ? F4 C30 1.289(7) . ? F5 C30 1.275(7) . ? F6 C30 1.322(8) . ? F7A C37 1.304(9) . ? F8A C37 1.328(10) . ? F9A C37 1.349(9) . ? F10 C38 1.331(7) . ? F11 C38 1.321(7) . ? F12 C38 1.321(6) . ? F13 C45 1.345(7) . ? F14 C45 1.317(6) . ? F15 C45 1.325(7) . ? F16 C46 1.329(6) . ? F17 C46 1.340(6) . ? F18 C46 1.318(6) . ? F19A C53 1.320(7) . ? F20A C53 1.394(8) . ? F21A C53 1.285(8) . ? F22 C54 1.348(6) . ? F23 C54 1.333(6) . ? F24 C54 1.341(6) . ? F7B C37 1.28(3) . ? F8B C37 1.27(3) . ? F9B C37 1.24(3) . ? F19B C53 1.55(2) . ? F20B C53 1.12(4) . ? F21B C53 1.20(4) . ? C23 C28 1.404(7) . ? C23 C24 1.407(6) . ? C23 B1 1.638(7) . ? C24 C25 1.374(7) . ? C24 H24 0.9500 . ? C25 C26 1.385(7) . ? C25 C29 1.495(7) . ? C26 C27 1.385(7) . ? C26 H26 0.9500 . ? C27 C28 1.382(7) . ? C27 C30 1.504(7) . ? C28 H28 0.9500 . ? C31 C36 1.386(7) . ? C31 C32 1.409(6) . ? C31 B1 1.650(7) . ? C32 C33 1.383(7) . ? C32 H32 0.9500 . ? C33 C34 1.375(7) . ? C33 C37 1.476(8) . ? C34 C35 1.384(7) . ? C34 H34 0.9500 . ? C35 C36 1.380(7) . ? C35 C38 1.500(8) . ? C36 H36 0.9500 . ? C39 C40 1.400(7) . ? C39 C44 1.404(6) . ? C39 B1 1.631(7) . ? C40 C41 1.388(6) . ? C40 H40 0.9500 . ? C41 C42 1.397(7) . ? C41 C45 1.479(7) . ? C42 C43 1.369(7) . ? C42 H42 0.9500 . ? C43 C44 1.401(7) . ? C43 C46 1.492(7) . ? C44 H44 0.9500 . ? C47 C52 1.390(7) . ? C47 C48 1.409(6) . ? C47 B1 1.641(7) . ? C48 C49 1.381(7) . ? C48 H48 0.9500 . ? C49 C50 1.381(7) . ? C49 C53 1.486(7) . ? C50 C51 1.377(7) . ? C50 H50 0.9500 . ? C51 C52 1.392(6) . ? C51 C54 1.488(7) . ? C52 H52 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ru1 C19 86.9(2) . . ? N4 Ru1 N1 91.84(19) . . ? C19 Ru1 N1 84.3(2) . . ? N4 Ru1 C2 155.57(19) . . ? C19 Ru1 C2 102.84(19) . . ? N1 Ru1 C2 111.21(18) . . ? N4 Ru1 C1 118.42(19) . . ? C19 Ru1 C1 98.31(19) . . ? N1 Ru1 C1 149.69(19) . . ? C2 Ru1 C1 38.64(18) . . ? N4 Ru1 C5 91.90(19) . . ? C19 Ru1 C5 126.8(2) . . ? N1 Ru1 C5 148.84(19) . . ? C2 Ru1 C5 64.25(19) . . ? C1 Ru1 C5 38.33(18) . . ? N4 Ru1 C3 136.49(19) . . ? C19 Ru1 C3 136.6(2) . . ? N1 Ru1 C3 93.31(17) . . ? C2 Ru1 C3 38.41(18) . . ? C1 Ru1 C3 64.12(19) . . ? C5 Ru1 C3 63.58(19) . . ? N4 Ru1 C4 100.64(19) . . ? C19 Ru1 C4 162.35(18) . . ? N1 Ru1 C4 111.16(18) . . ? C2 Ru1 C4 64.29(18) . . ? C1 Ru1 C4 64.06(18) . . ? C5 Ru1 C4 37.88(19) . . ? C3 Ru1 C4 38.10(18) . . ? C13 N1 C17 115.9(5) . . ? C13 N1 Ru1 120.6(4) . . ? C17 N1 Ru1 123.4(4) . . ? C19 N2 C21 111.2(5) . . ? C19 N2 C18 122.6(5) . . ? C21 N2 C18 126.2(5) . . ? C19 N3 C20 110.0(5) . . ? C19 N3 C22 126.8(5) . . ? C20 N3 C22 123.1(6) . . ? C11 N4 Ru1 168.5(5) . . ? C5 C1 C2 107.6(4) . . ? C5 C1 C6 127.4(5) . . ? C2 C1 C6 124.8(5) . . ? C5 C1 Ru1 71.3(3) . . ? C2 C1 Ru1 70.2(3) . . ? C6 C1 Ru1 127.8(3) . . ? C3 C2 C1 107.9(4) . . ? C3 C2 C7 126.7(4) . . ? C1 C2 C7 124.7(4) . . ? C3 C2 Ru1 72.0(3) . . ? C1 C2 Ru1 71.1(3) . . ? C7 C2 Ru1 129.4(3) . . ? C2 C3 C4 108.5(4) . . ? C2 C3 C8 125.4(5) . . ? C4 C3 C8 126.1(4) . . ? C2 C3 Ru1 69.6(3) . . ? C4 C3 Ru1 72.0(3) . . ? C8 C3 Ru1 126.1(3) . . ? C5 C4 C3 106.9(4) . . ? C5 C4 C9 126.7(5) . . ? C3 C4 C9 126.2(5) . . ? C5 C4 Ru1 69.7(3) . . ? C3 C4 Ru1 69.9(3) . . ? C9 C4 Ru1 129.6(3) . . ? C4 C5 C1 109.1(5) . . ? C4 C5 C10 124.0(5) . . ? C1 C5 C10 126.8(5) . . ? C4 C5 Ru1 72.4(3) . . ? C1 C5 Ru1 70.4(3) . . ? C10 C5 Ru1 126.5(4) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 C12 172.4(8) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 127.5(6) . . ? N1 C13 H13 116.2 . . ? C14 C13 H13 116.2 . . ? C15 C14 C13 115.7(6) . . ? C15 C14 H14 122.1 . . ? C13 C14 H14 122.1 . . ? C14 C15 C16 121.8(6) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C17 C16 C15 119.3(6) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 N1 119.8(5) . . ? C16 C17 C18 121.4(5) . . ? N1 C17 C18 118.8(5) . . ? N2 C18 C17 112.1(5) . . ? N2 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? N2 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N2 C19 N3 105.3(5) . . ? N2 C19 Ru1 125.0(4) . . ? N3 C19 Ru1 129.6(4) . . ? C21 C20 N3 106.7(6) . . ? C21 C20 H20 126.6 . . ? N3 C20 H20 126.6 . . ? C20 C21 N2 106.7(6) . . ? C20 C21 H21 126.6 . . ? N2 C21 H21 126.6 . . ? N3 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 115.3(4) . . ? C28 C23 B1 121.7(4) . . ? C24 C23 B1 122.7(4) . . ? C25 C24 C23 122.4(4) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C24 C25 C26 121.3(4) . . ? C24 C25 C29 119.7(5) . . ? C26 C25 C29 119.1(5) . . ? C27 C26 C25 117.6(5) . . ? C27 C26 H26 121.2 . . ? C25 C26 H26 121.2 . . ? C28 C27 C26 121.4(5) . . ? C28 C27 C30 120.0(4) . . ? C26 C27 C30 118.6(5) . . ? C27 C28 C23 122.0(4) . . ? C27 C28 H28 119.0 . . ? C23 C28 H28 119.0 . . ? F2 C29 F1 105.3(5) . . ? F2 C29 F3 107.2(5) . . ? F1 C29 F3 104.4(5) . . ? F2 C29 C25 113.0(4) . . ? F1 C29 C25 113.6(5) . . ? F3 C29 C25 112.6(5) . . ? F5 C30 F4 109.9(6) . . ? F5 C30 F6 103.5(6) . . ? F4 C30 F6 102.2(6) . . ? F5 C30 C27 115.1(5) . . ? F4 C30 C27 113.3(5) . . ? F6 C30 C27 111.6(5) . . ? C36 C31 C32 116.2(4) . . ? C36 C31 B1 123.9(4) . . ? C32 C31 B1 119.5(4) . . ? C33 C32 C31 121.2(4) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C34 C33 C32 121.6(5) . . ? C34 C33 C37 119.3(5) . . ? C32 C33 C37 119.1(5) . . ? C33 C34 C35 117.6(4) . . ? C33 C34 H34 121.2 . . ? C35 C34 H34 121.2 . . ? C36 C35 C34 121.3(5) . . ? C36 C35 C38 120.0(5) . . ? C34 C35 C38 118.7(4) . . ? C35 C36 C31 122.0(4) . . ? C35 C36 H36 119.0 . . ? C31 C36 H36 119.0 . . ? F9B C37 F8B 102.9(15) . . ? F9B C37 F7B 110.3(14) . . ? F8B C37 F7B 104.2(15) . . ? F7A C37 F8A 104.7(7) . . ? F7A C37 F9A 105.4(7) . . ? F8A C37 F9A 100.4(7) . . ? F9B C37 C33 112.3(9) . . ? F8B C37 C33 115.6(11) . . ? F7B C37 C33 111.0(9) . . ? F7A C37 C33 114.6(6) . . ? F8A C37 C33 115.1(6) . . ? F9A C37 C33 115.1(5) . . ? F11 C38 F12 107.0(5) . . ? F11 C38 F10 104.8(5) . . ? F12 C38 F10 106.5(6) . . ? F11 C38 C35 111.6(5) . . ? F12 C38 C35 113.2(5) . . ? F10 C38 C35 113.1(5) . . ? C40 C39 C44 115.4(4) . . ? C40 C39 B1 119.8(4) . . ? C44 C39 B1 124.2(4) . . ? C41 C40 C39 123.0(4) . . ? C41 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? C40 C41 C42 119.8(4) . . ? C40 C41 C45 119.4(4) . . ? C42 C41 C45 120.8(4) . . ? C43 C42 C41 118.9(4) . . ? C43 C42 H42 120.6 . . ? C41 C42 H42 120.6 . . ? C42 C43 C44 120.8(4) . . ? C42 C43 C46 118.5(4) . . ? C44 C43 C46 120.7(4) . . ? C43 C44 C39 122.0(4) . . ? C43 C44 H44 119.0 . . ? C39 C44 H44 119.0 . . ? F14 C45 F15 107.3(5) . . ? F14 C45 F13 105.5(5) . . ? F15 C45 F13 104.3(5) . . ? F14 C45 C41 113.5(5) . . ? F15 C45 C41 113.6(5) . . ? F13 C45 C41 112.0(4) . . ? F18 C46 F16 106.6(5) . . ? F18 C46 F17 105.4(5) . . ? F16 C46 F17 105.2(4) . . ? F18 C46 C43 114.4(4) . . ? F16 C46 C43 112.5(4) . . ? F17 C46 C43 112.2(4) . . ? C52 C47 C48 115.3(4) . . ? C52 C47 B1 124.4(4) . . ? C48 C47 B1 119.8(4) . . ? C49 C48 C47 121.8(4) . . ? C49 C48 H48 119.1 . . ? C47 C48 H48 119.1 . . ? C50 C49 C48 121.6(4) . . ? C50 C49 C53 119.9(5) . . ? C48 C49 C53 118.5(5) . . ? C51 C50 C49 117.9(4) . . ? C51 C50 H50 121.1 . . ? C49 C50 H50 121.1 . . ? C50 C51 C52 120.6(4) . . ? C50 C51 C54 119.9(4) . . ? C52 C51 C54 119.4(4) . . ? C47 C52 C51 122.7(4) . . ? C47 C52 H52 118.6 . . ? C51 C52 H52 118.6 . . ? F20B C53 F21B 107(2) . . ? F21A C53 F19A 112.3(6) . . ? F21A C53 F20A 103.2(6) . . ? F19A C53 F20A 99.4(6) . . ? F20B C53 C49 119.5(16) . . ? F21B C53 C49 116.0(14) . . ? F21A C53 C49 116.0(5) . . ? F19A C53 C49 114.2(5) . . ? F20A C53 C49 109.7(5) . . ? F20B C53 F19B 105.0(18) . . ? F21B C53 F19B 103(2) . . ? C49 C53 F19B 104.7(9) . . ? F23 C54 F24 106.1(4) . . ? F23 C54 F22 105.7(4) . . ? F24 C54 F22 105.4(4) . . ? F23 C54 C51 113.3(4) . . ? F24 C54 C51 113.7(4) . . ? F22 C54 C51 112.0(4) . . ? C39 B1 C23 112.9(4) . . ? C39 B1 C47 104.3(4) . . ? C23 B1 C47 113.6(4) . . ? C39 B1 C31 112.5(4) . . ? C23 B1 C31 103.4(4) . . ? C47 B1 C31 110.5(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 N4 Ru1 N1 C13 -63.3(4) . . . . ? C19 Ru1 N1 C13 -149.9(4) . . . . ? C2 Ru1 N1 C13 108.5(4) . . . . ? C1 Ru1 N1 C13 113.4(5) . . . . ? C5 Ru1 N1 C13 33.5(6) . . . . ? C3 Ru1 N1 C13 73.5(4) . . . . ? C4 Ru1 N1 C13 38.9(5) . . . . ? N4 Ru1 N1 C17 120.3(4) . . . . ? C19 Ru1 N1 C17 33.6(4) . . . . ? C2 Ru1 N1 C17 -68.0(4) . . . . ? C1 Ru1 N1 C17 -63.1(6) . . . . ? C5 Ru1 N1 C17 -143.0(4) . . . . ? C3 Ru1 N1 C17 -102.9(4) . . . . ? C4 Ru1 N1 C17 -137.6(4) . . . . ? C19 Ru1 N4 C11 -126(3) . . . . ? N1 Ru1 N4 C11 150(3) . . . . ? C2 Ru1 N4 C11 -11(3) . . . . ? C1 Ru1 N4 C11 -28(3) . . . . ? C5 Ru1 N4 C11 1(3) . . . . ? C3 Ru1 N4 C11 53(3) . . . . ? C4 Ru1 N4 C11 38(3) . . . . ? N4 Ru1 C1 C5 51.4(4) . . . . ? C19 Ru1 C1 C5 142.4(3) . . . . ? N1 Ru1 C1 C5 -124.8(4) . . . . ? C2 Ru1 C1 C5 -117.4(4) . . . . ? C3 Ru1 C1 C5 -79.4(3) . . . . ? C4 Ru1 C1 C5 -36.9(3) . . . . ? N4 Ru1 C1 C2 168.8(3) . . . . ? C19 Ru1 C1 C2 -100.2(3) . . . . ? N1 Ru1 C1 C2 -7.4(5) . . . . ? C5 Ru1 C1 C2 117.4(4) . . . . ? C3 Ru1 C1 C2 38.0(3) . . . . ? C4 Ru1 C1 C2 80.6(3) . . . . ? N4 Ru1 C1 C6 -71.9(5) . . . . ? C19 Ru1 C1 C6 19.1(5) . . . . ? N1 Ru1 C1 C6 111.9(5) . . . . ? C2 Ru1 C1 C6 119.3(6) . . . . ? C5 Ru1 C1 C6 -123.3(6) . . . . ? C3 Ru1 C1 C6 157.3(5) . . . . ? C4 Ru1 C1 C6 -160.2(5) . . . . ? C5 C1 C2 C3 -1.1(5) . . . . ? C6 C1 C2 C3 174.0(4) . . . . ? Ru1 C1 C2 C3 -63.0(3) . . . . ? C5 C1 C2 C7 -172.7(4) . . . . ? C6 C1 C2 C7 2.4(7) . . . . ? Ru1 C1 C2 C7 125.4(5) . . . . ? C5 C1 C2 Ru1 61.9(3) . . . . ? C6 C1 C2 Ru1 -123.0(5) . . . . ? N4 Ru1 C2 C3 92.6(5) . . . . ? C19 Ru1 C2 C3 -155.8(3) . . . . ? N1 Ru1 C2 C3 -67.1(3) . . . . ? C1 Ru1 C2 C3 116.9(4) . . . . ? C5 Ru1 C2 C3 79.2(3) . . . . ? C4 Ru1 C2 C3 37.0(3) . . . . ? N4 Ru1 C2 C1 -24.3(6) . . . . ? C19 Ru1 C2 C1 87.3(3) . . . . ? N1 Ru1 C2 C1 176.0(3) . . . . ? C5 Ru1 C2 C1 -37.7(3) . . . . ? C3 Ru1 C2 C1 -116.9(4) . . . . ? C4 Ru1 C2 C1 -79.9(3) . . . . ? N4 Ru1 C2 C7 -144.2(5) . . . . ? C19 Ru1 C2 C7 -32.7(5) . . . . ? N1 Ru1 C2 C7 56.1(5) . . . . ? C1 Ru1 C2 C7 -119.9(6) . . . . ? C5 Ru1 C2 C7 -157.6(5) . . . . ? C3 Ru1 C2 C7 123.2(6) . . . . ? C4 Ru1 C2 C7 160.2(5) . . . . ? C1 C2 C3 C4 0.7(5) . . . . ? C7 C2 C3 C4 172.0(4) . . . . ? Ru1 C2 C3 C4 -61.8(3) . . . . ? C1 C2 C3 C8 -177.1(4) . . . . ? C7 C2 C3 C8 -5.7(8) . . . . ? Ru1 C2 C3 C8 120.5(5) . . . . ? C1 C2 C3 Ru1 62.5(3) . . . . ? C7 C2 C3 Ru1 -126.2(5) . . . . ? N4 Ru1 C3 C2 -143.1(3) . . . . ? C19 Ru1 C3 C2 35.5(4) . . . . ? N1 Ru1 C3 C2 120.7(3) . . . . ? C1 Ru1 C3 C2 -38.2(3) . . . . ? C5 Ru1 C3 C2 -81.1(3) . . . . ? C4 Ru1 C3 C2 -118.5(4) . . . . ? N4 Ru1 C3 C4 -24.6(4) . . . . ? C19 Ru1 C3 C4 154.0(3) . . . . ? N1 Ru1 C3 C4 -120.8(3) . . . . ? C2 Ru1 C3 C4 118.5(4) . . . . ? C1 Ru1 C3 C4 80.3(3) . . . . ? C5 Ru1 C3 C4 37.4(3) . . . . ? N4 Ru1 C3 C8 97.3(5) . . . . ? C19 Ru1 C3 C8 -84.0(5) . . . . ? N1 Ru1 C3 C8 1.1(5) . . . . ? C2 Ru1 C3 C8 -119.5(6) . . . . ? C1 Ru1 C3 C8 -157.8(5) . . . . ? C5 Ru1 C3 C8 159.3(5) . . . . ? C4 Ru1 C3 C8 122.0(5) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C8 C3 C4 C5 177.8(4) . . . . ? Ru1 C3 C4 C5 -60.2(3) . . . . ? C2 C3 C4 C9 -174.7(5) . . . . ? C8 C3 C4 C9 3.0(8) . . . . ? Ru1 C3 C4 C9 125.0(5) . . . . ? C2 C3 C4 Ru1 60.3(3) . . . . ? C8 C3 C4 Ru1 -122.0(5) . . . . ? N4 Ru1 C4 C5 -79.3(3) . . . . ? C19 Ru1 C4 C5 34.8(8) . . . . ? N1 Ru1 C4 C5 -175.4(3) . . . . ? C2 Ru1 C4 C5 80.4(3) . . . . ? C1 Ru1 C4 C5 37.3(3) . . . . ? C3 Ru1 C4 C5 117.7(4) . . . . ? N4 Ru1 C4 C3 163.0(3) . . . . ? C19 Ru1 C4 C3 -82.9(7) . . . . ? N1 Ru1 C4 C3 66.8(3) . . . . ? C2 Ru1 C4 C3 -37.3(3) . . . . ? C1 Ru1 C4 C3 -80.4(3) . . . . ? C5 Ru1 C4 C3 -117.7(4) . . . . ? N4 Ru1 C4 C9 42.1(5) . . . . ? C19 Ru1 C4 C9 156.2(6) . . . . ? N1 Ru1 C4 C9 -54.1(5) . . . . ? C2 Ru1 C4 C9 -158.2(5) . . . . ? C1 Ru1 C4 C9 158.7(5) . . . . ? C5 Ru1 C4 C9 121.4(6) . . . . ? C3 Ru1 C4 C9 -120.9(6) . . . . ? C3 C4 C5 C1 -0.8(5) . . . . ? C9 C4 C5 C1 174.0(5) . . . . ? Ru1 C4 C5 C1 -61.1(3) . . . . ? C3 C4 C5 C10 -177.1(4) . . . . ? C9 C4 C5 C10 -2.3(8) . . . . ? Ru1 C4 C5 C10 122.6(5) . . . . ? C3 C4 C5 Ru1 60.3(3) . . . . ? C9 C4 C5 Ru1 -124.9(5) . . . . ? C2 C1 C5 C4 1.2(5) . . . . ? C6 C1 C5 C4 -173.8(4) . . . . ? Ru1 C1 C5 C4 62.4(3) . . . . ? C2 C1 C5 C10 177.3(5) . . . . ? C6 C1 C5 C10 2.4(8) . . . . ? Ru1 C1 C5 C10 -121.5(5) . . . . ? C2 C1 C5 Ru1 -61.2(3) . . . . ? C6 C1 C5 Ru1 123.8(5) . . . . ? N4 Ru1 C5 C4 105.0(3) . . . . ? C19 Ru1 C5 C4 -167.5(3) . . . . ? N1 Ru1 C5 C4 8.2(5) . . . . ? C2 Ru1 C5 C4 -80.5(3) . . . . ? C1 Ru1 C5 C4 -118.5(4) . . . . ? C3 Ru1 C5 C4 -37.6(3) . . . . ? N4 Ru1 C5 C1 -136.5(3) . . . . ? C19 Ru1 C5 C1 -49.0(4) . . . . ? N1 Ru1 C5 C1 126.8(4) . . . . ? C2 Ru1 C5 C1 38.0(3) . . . . ? C3 Ru1 C5 C1 80.9(3) . . . . ? C4 Ru1 C5 C1 118.5(4) . . . . ? N4 Ru1 C5 C10 -14.7(5) . . . . ? C19 Ru1 C5 C10 72.9(5) . . . . ? N1 Ru1 C5 C10 -111.4(5) . . . . ? C2 Ru1 C5 C10 159.8(5) . . . . ? C1 Ru1 C5 C10 121.8(6) . . . . ? C3 Ru1 C5 C10 -157.2(5) . . . . ? C4 Ru1 C5 C10 -119.6(6) . . . . ? C17 N1 C13 C14 0.7(9) . . . . ? Ru1 N1 C13 C14 -176.0(5) . . . . ? N1 C13 C14 C15 -1.0(10) . . . . ? C13 C14 C15 C16 -0.6(9) . . . . ? C14 C15 C16 C17 2.2(9) . . . . ? C15 C16 C17 N1 -2.4(8) . . . . ? C15 C16 C17 C18 174.3(5) . . . . ? C13 N1 C17 C16 1.0(7) . . . . ? Ru1 N1 C17 C16 177.7(4) . . . . ? C13 N1 C17 C18 -175.8(5) . . . . ? Ru1 N1 C17 C18 0.8(7) . . . . ? C19 N2 C18 C17 54.8(7) . . . . ? C21 N2 C18 C17 -125.4(6) . . . . ? C16 C17 C18 N2 132.0(5) . . . . ? N1 C17 C18 N2 -51.3(6) . . . . ? C21 N2 C19 N3 -0.8(6) . . . . ? C18 N2 C19 N3 179.0(5) . . . . ? C21 N2 C19 Ru1 176.2(4) . . . . ? C18 N2 C19 Ru1 -4.0(7) . . . . ? C20 N3 C19 N2 1.0(6) . . . . ? C22 N3 C19 N2 178.0(6) . . . . ? C20 N3 C19 Ru1 -175.8(4) . . . . ? C22 N3 C19 Ru1 1.2(9) . . . . ? N4 Ru1 C19 N2 -125.5(5) . . . . ? N1 Ru1 C19 N2 -33.3(4) . . . . ? C2 Ru1 C19 N2 77.2(5) . . . . ? C1 Ru1 C19 N2 116.3(4) . . . . ? C5 Ru1 C19 N2 144.5(4) . . . . ? C3 Ru1 C19 N2 55.5(5) . . . . ? C4 Ru1 C19 N2 118.5(7) . . . . ? N4 Ru1 C19 N3 50.8(5) . . . . ? N1 Ru1 C19 N3 143.0(5) . . . . ? C2 Ru1 C19 N3 -106.5(5) . . . . ? C1 Ru1 C19 N3 -67.5(5) . . . . ? C5 Ru1 C19 N3 -39.2(6) . . . . ? C3 Ru1 C19 N3 -128.3(5) . . . . ? C4 Ru1 C19 N3 -65.2(9) . . . . ? C19 N3 C20 C21 -0.8(7) . . . . ? C22 N3 C20 C21 -177.9(6) . . . . ? N3 C20 C21 N2 0.3(7) . . . . ? C19 N2 C21 C20 0.4(7) . . . . ? C18 N2 C21 C20 -179.5(6) . . . . ? C28 C23 C24 C25 -2.5(7) . . . . ? B1 C23 C24 C25 -177.0(4) . . . . ? C23 C24 C25 C26 0.5(7) . . . . ? C23 C24 C25 C29 179.3(5) . . . . ? C24 C25 C26 C27 1.5(8) . . . . ? C29 C25 C26 C27 -177.3(5) . . . . ? C25 C26 C27 C28 -1.5(8) . . . . ? C25 C26 C27 C30 178.1(5) . . . . ? C26 C27 C28 C23 -0.5(8) . . . . ? C30 C27 C28 C23 179.9(5) . . . . ? C24 C23 C28 C27 2.5(7) . . . . ? B1 C23 C28 C27 177.1(4) . . . . ? C24 C25 C29 F2 26.4(8) . . . . ? C26 C25 C29 F2 -154.8(5) . . . . ? C24 C25 C29 F1 146.2(5) . . . . ? C26 C25 C29 F1 -35.0(7) . . . . ? C24 C25 C29 F3 -95.3(6) . . . . ? C26 C25 C29 F3 83.5(7) . . . . ? C28 C27 C30 F5 -167.9(6) . . . . ? C26 C27 C30 F5 12.5(9) . . . . ? C28 C27 C30 F4 -40.1(8) . . . . ? C26 C27 C30 F4 140.3(6) . . . . ? C28 C27 C30 F6 74.6(7) . . . . ? C26 C27 C30 F6 -105.0(7) . . . . ? C36 C31 C32 C33 0.5(7) . . . . ? B1 C31 C32 C33 173.8(5) . . . . ? C31 C32 C33 C34 -0.3(8) . . . . ? C31 C32 C33 C37 180.0(5) . . . . ? C32 C33 C34 C35 0.0(8) . . . . ? C37 C33 C34 C35 179.7(5) . . . . ? C33 C34 C35 C36 0.3(8) . . . . ? C33 C34 C35 C38 -178.3(5) . . . . ? C34 C35 C36 C31 -0.1(8) . . . . ? C38 C35 C36 C31 178.4(5) . . . . ? C32 C31 C36 C35 -0.3(7) . . . . ? B1 C31 C36 C35 -173.3(5) . . . . ? C34 C33 C37 F9B -131.4(13) . . . . ? C32 C33 C37 F9B 48.3(14) . . . . ? C34 C33 C37 F8B -13.8(18) . . . . ? C32 C33 C37 F8B 165.9(16) . . . . ? C34 C33 C37 F7B 104.5(12) . . . . ? C32 C33 C37 F7B -75.8(13) . . . . ? C34 C33 C37 F7A 37.7(11) . . . . ? C32 C33 C37 F7A -142.6(9) . . . . ? C34 C33 C37 F8A -83.8(9) . . . . ? C32 C33 C37 F8A 96.0(9) . . . . ? C34 C33 C37 F9A 160.2(7) . . . . ? C32 C33 C37 F9A -20.1(9) . . . . ? C36 C35 C38 F11 -74.9(7) . . . . ? C34 C35 C38 F11 103.6(6) . . . . ? C36 C35 C38 F12 164.2(6) . . . . ? C34 C35 C38 F12 -17.2(8) . . . . ? C36 C35 C38 F10 42.9(7) . . . . ? C34 C35 C38 F10 -138.5(5) . . . . ? C44 C39 C40 C41 0.7(7) . . . . ? B1 C39 C40 C41 -171.2(4) . . . . ? C39 C40 C41 C42 -2.2(7) . . . . ? C39 C40 C41 C45 179.1(5) . . . . ? C40 C41 C42 C43 1.3(7) . . . . ? C45 C41 C42 C43 -180.0(5) . . . . ? C41 C42 C43 C44 1.0(7) . . . . ? C41 C42 C43 C46 -179.2(4) . . . . ? C42 C43 C44 C39 -2.6(7) . . . . ? C46 C43 C44 C39 177.7(4) . . . . ? C40 C39 C44 C43 1.7(6) . . . . ? B1 C39 C44 C43 173.2(4) . . . . ? C40 C41 C45 F14 -170.2(5) . . . . ? C42 C41 C45 F14 11.1(8) . . . . ? C40 C41 C45 F15 67.0(6) . . . . ? C42 C41 C45 F15 -111.8(6) . . . . ? C40 C41 C45 F13 -50.9(7) . . . . ? C42 C41 C45 F13 130.4(5) . . . . ? C42 C43 C46 F18 -174.1(5) . . . . ? C44 C43 C46 F18 5.6(7) . . . . ? C42 C43 C46 F16 64.2(6) . . . . ? C44 C43 C46 F16 -116.1(5) . . . . ? C42 C43 C46 F17 -54.1(6) . . . . ? C44 C43 C46 F17 125.6(5) . . . . ? C52 C47 C48 C49 -1.1(6) . . . . ? B1 C47 C48 C49 171.6(4) . . . . ? C47 C48 C49 C50 3.3(7) . . . . ? C47 C48 C49 C53 -175.3(4) . . . . ? C48 C49 C50 C51 -2.8(7) . . . . ? C53 C49 C50 C51 175.8(5) . . . . ? C49 C50 C51 C52 0.2(7) . . . . ? C49 C50 C51 C54 176.2(4) . . . . ? C48 C47 C52 C51 -1.5(6) . . . . ? B1 C47 C52 C51 -173.9(4) . . . . ? C50 C51 C52 C47 2.0(7) . . . . ? C54 C51 C52 C47 -174.0(4) . . . . ? C50 C49 C53 F20B -171.2(19) . . . . ? C48 C49 C53 F20B 7(2) . . . . ? C50 C49 C53 F21B -42(2) . . . . ? C48 C49 C53 F21B 137(2) . . . . ? C50 C49 C53 F21A 18.6(9) . . . . ? C48 C49 C53 F21A -162.8(6) . . . . ? C50 C49 C53 F19A 151.6(6) . . . . ? C48 C49 C53 F19A -29.8(8) . . . . ? C50 C49 C53 F20A -97.8(6) . . . . ? C48 C49 C53 F20A 80.8(6) . . . . ? C50 C49 C53 F19B 71.6(10) . . . . ? C48 C49 C53 F19B -109.7(10) . . . . ? C50 C51 C54 F23 22.4(6) . . . . ? C52 C51 C54 F23 -161.6(4) . . . . ? C50 C51 C54 F24 143.6(4) . . . . ? C52 C51 C54 F24 -40.4(6) . . . . ? C50 C51 C54 F22 -97.1(5) . . . . ? C52 C51 C54 F22 79.0(6) . . . . ? C40 C39 B1 C23 -164.9(4) . . . . ? C44 C39 B1 C23 24.0(6) . . . . ? C40 C39 B1 C47 71.4(5) . . . . ? C44 C39 B1 C47 -99.7(5) . . . . ? C40 C39 B1 C31 -48.3(6) . . . . ? C44 C39 B1 C31 140.5(4) . . . . ? C28 C23 B1 C39 41.9(6) . . . . ? C24 C23 B1 C39 -143.9(4) . . . . ? C28 C23 B1 C47 160.3(4) . . . . ? C24 C23 B1 C47 -25.4(6) . . . . ? C28 C23 B1 C31 -80.0(5) . . . . ? C24 C23 B1 C31 94.3(5) . . . . ? C52 C47 B1 C39 88.9(5) . . . . ? C48 C47 B1 C39 -83.1(5) . . . . ? C52 C47 B1 C23 -34.4(6) . . . . ? C48 C47 B1 C23 153.6(4) . . . . ? C52 C47 B1 C31 -150.0(4) . . . . ? C48 C47 B1 C31 38.0(5) . . . . ? C36 C31 B1 C39 -28.2(6) . . . . ? C32 C31 B1 C39 159.0(4) . . . . ? C36 C31 B1 C23 93.9(5) . . . . ? C32 C31 B1 C23 -78.9(5) . . . . ? C36 C31 B1 C47 -144.3(5) . . . . ? C32 C31 B1 C47 42.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.341 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.113 ##=== END OF CIF ##=== data_pv1018 ==== CCDC 833092 == (Compound 3b in the text) data_pv1018 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (\h^2^-dioxygen)-{\k^2^ C,N-3-isopropyl-1-(pyrid-2-ylmethyl)-2,3-dihydro- imidazole-2-ylidene}-(\h^5^-pentamethylcyclopentadienyl)-ruthenium(II) tetrakis{3,5-bis(trifluoromethyl)phenyl}borate dichloromethane diethylether solvates ; _chemical_name_common ? _chemical_formula_moiety 'C22 H30 N3 O2 Ru, C32 H12 B F24, 0.56(C H2 Cl2), 0.44(C4 H10 O)' _chemical_formula_sum 'C56.32 H47.53 B Cl1.12 F24 N3 O2.44 Ru' _chemical_melting_point ? _exptl_crystal_description plate _exptl_crystal_colour red _diffrn_ambient_temperature 100(2) _chemical_formula_weight 1412.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _symmetry_space_group_name_Hall '-P2ybc' 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 12.498(3) _cell_length_b 17.896(4) _cell_length_c 26.458(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.67(3) _cell_angle_gamma 90.00 _cell_volume 5917(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6017 _cell_measurement_theta_min 2.124 _cell_measurement_theta_max 24.963 _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2840.8 _exptl_absorpt_coefficient_mu 0.436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _exptl_special_details ; Bruker SMART APEX 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. A hemisphere of the reciprocal space up to theta(max) = 25.04 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 10 sec per frame, 1700 frames were recorded using program SMART (Bruker). Frame data evaluation and integration were done with program SAINT+(Bruker); Lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections with program SAINT + (Bruker). Correction for crystal decay (insignificant) was applied. ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '1700 omega scan frames, 0.3 deg, 10 sec' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.0026 _diffrn_reflns_number 39232 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.04 _reflns_number_total 10356 _reflns_number_gt 9256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2001)' _computing_molecular_graphics 'ORTEP-3 vers. 1.08 (Farrugia, 2005)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0608P)^2^+8.9880P] 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 10356 _refine_ls_number_parameters 876 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.086 _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 0.57000(2) 0.354524(14) 0.581234(9) 0.02307(10) Uani 1 1 d . . . O1 O 0.4993(2) 0.39018(16) 0.51770(9) 0.0409(6) Uani 1 1 d . . . O2 O 0.4209(2) 0.37280(15) 0.55267(10) 0.0384(6) Uani 1 1 d . . . N1 N 0.5573(2) 0.19358(16) 0.61351(12) 0.0339(7) Uani 1 1 d . . . N2 N 0.4086(2) 0.24531(15) 0.63122(10) 0.0281(6) Uani 1 1 d . . . N3 N 0.6482(2) 0.27731(18) 0.53124(11) 0.0346(7) Uani 1 1 d . . . C1 C 0.5811(3) 0.4180(2) 0.65155(12) 0.0292(8) Uani 1 1 d . . . C2 C 0.6783(3) 0.3757(2) 0.64639(12) 0.0291(8) Uani 1 1 d . . . C3 C 0.7329(3) 0.40254(19) 0.60306(12) 0.0267(7) Uani 1 1 d . . . C4 C 0.6700(3) 0.45993(18) 0.58063(12) 0.0267(7) Uani 1 1 d . . . C5 C 0.5759(3) 0.46937(19) 0.61021(13) 0.0287(7) Uani 1 1 d . . . C6 C 0.5100(3) 0.4169(2) 0.69653(14) 0.0399(9) Uani 1 1 d . . . H6A H 0.5034 0.3656 0.7090 0.060 Uiso 1 1 calc R . . H6B H 0.4391 0.4359 0.6869 0.060 Uiso 1 1 calc R . . H6C H 0.5409 0.4485 0.7232 0.060 Uiso 1 1 calc R . . C7 C 0.7235(3) 0.3252(2) 0.68625(14) 0.0414(9) Uani 1 1 d . . . H7A H 0.7422 0.3545 0.7163 0.062 Uiso 1 1 calc R . . H7B H 0.7877 0.3005 0.6735 0.062 Uiso 1 1 calc R . . H7C H 0.6701 0.2874 0.6951 0.062 Uiso 1 1 calc R . . C8 C 0.8395(3) 0.3756(2) 0.58469(14) 0.0359(8) Uani 1 1 d . . . H8A H 0.8387 0.3741 0.5477 0.054 Uiso 1 1 calc R . . H8B H 0.8535 0.3254 0.5980 0.054 Uiso 1 1 calc R . . H8C H 0.8958 0.4098 0.5964 0.054 Uiso 1 1 calc R . . C9 C 0.6963(3) 0.5041(2) 0.53434(14) 0.0361(8) Uani 1 1 d . . . H9A H 0.7181 0.5547 0.5442 0.054 Uiso 1 1 calc R . . H9B H 0.6331 0.5068 0.5121 0.054 Uiso 1 1 calc R . . H9C H 0.7550 0.4797 0.5164 0.054 Uiso 1 1 calc R . . C10 C 0.4901(3) 0.5252(2) 0.59993(15) 0.0378(9) Uani 1 1 d . . . H10A H 0.5129 0.5743 0.6125 0.057 Uiso 1 1 calc R . . H10B H 0.4245 0.5100 0.6171 0.057 Uiso 1 1 calc R . . H10C H 0.4763 0.5281 0.5634 0.057 Uiso 1 1 calc R . . C11 C 0.5062(3) 0.26000(19) 0.61269(12) 0.0263(7) Uani 1 1 d . . . C12 C 0.4915(3) 0.1378(2) 0.63140(17) 0.0440(10) Uani 1 1 d . . . H12 H 0.5090 0.0864 0.6350 0.053 Uiso 1 1 calc R . . C13 C 0.3988(3) 0.1700(2) 0.64255(16) 0.0403(9) Uani 1 1 d . . . H13 H 0.3374 0.1459 0.6558 0.048 Uiso 1 1 calc R . . C14 C 0.3194(3) 0.2990(2) 0.63842(13) 0.0304(8) Uani 1 1 d . . . H14 H 0.3479 0.3506 0.6331 0.037 Uiso 1 1 calc R . . C15 C 0.2784(3) 0.2941(2) 0.69218(15) 0.0431(10) Uani 1 1 d . . . H15A H 0.2403 0.2468 0.6967 0.065 Uiso 1 1 calc R . . H15B H 0.2295 0.3358 0.6985 0.065 Uiso 1 1 calc R . . H15C H 0.3389 0.2966 0.7160 0.065 Uiso 1 1 calc R . . C16 C 0.2316(3) 0.2854(2) 0.59993(16) 0.0448(10) Uani 1 1 d . . . H16A H 0.2611 0.2887 0.5658 0.067 Uiso 1 1 calc R . . H16B H 0.1755 0.3231 0.6038 0.067 Uiso 1 1 calc R . . H16C H 0.2012 0.2356 0.6051 0.067 Uiso 1 1 calc R . . C17 C 0.6676(3) 0.1835(2) 0.59735(16) 0.0413(9) Uani 1 1 d . . . H17A H 0.6861 0.1298 0.5996 0.050 Uiso 1 1 calc R . . H17B H 0.7157 0.2110 0.6208 0.050 Uiso 1 1 calc R . . C18 C 0.6871(3) 0.2101(2) 0.54454(16) 0.0392(9) Uani 1 1 d . . . C19 C 0.7501(3) 0.1682(3) 0.5125(2) 0.0576(13) Uani 1 1 d . . . H19 H 0.7766 0.1208 0.5228 0.069 Uiso 1 1 calc R . . C20 C 0.7739(4) 0.1962(4) 0.4653(2) 0.0679(17) Uani 1 1 d . . . H20 H 0.8178 0.1686 0.4429 0.081 Uiso 1 1 calc R . . C21 C 0.7335(4) 0.2642(4) 0.45119(17) 0.0614(14) Uani 1 1 d . . . H21 H 0.7487 0.2845 0.4189 0.074 Uiso 1 1 calc R . . C22 C 0.6700(3) 0.3030(3) 0.48473(14) 0.0467(11) Uani 1 1 d . . . H22 H 0.6407 0.3497 0.4745 0.056 Uiso 1 1 calc R . . F1 F -0.08572(19) 1.06646(12) 0.82472(9) 0.0472(6) Uani 1 1 d . . . F2 F -0.09695(19) 0.95935(14) 0.86077(8) 0.0480(6) Uani 1 1 d . . . F3 F 0.05038(16) 0.99331(12) 0.82707(7) 0.0365(5) Uani 1 1 d . . . F4 F -0.32835(18) 0.98563(15) 0.63948(8) 0.0492(6) Uani 1 1 d . . . F5 F -0.38738(17) 1.01621(13) 0.71227(9) 0.0457(6) Uani 1 1 d . . . F6 F -0.40166(17) 0.90355(13) 0.68664(10) 0.0480(6) Uani 1 1 d . . . F7A F 0.3891(9) 0.9899(6) 0.6741(4) 0.058(3) Uani 0.64(5) 1 d P A 1 F8A F 0.2487(14) 1.0066(8) 0.6303(5) 0.046(2) Uani 0.64(5) 1 d P A 1 F9A F 0.3806(19) 0.9456(10) 0.6007(9) 0.079(5) Uani 0.64(5) 1 d P A 1 F10A F 0.3449(7) 0.6287(5) 0.6845(5) 0.063(3) Uani 0.63(2) 1 d P B 1 F11A F 0.4766(6) 0.6987(4) 0.6768(6) 0.067(3) Uani 0.63(2) 1 d P B 1 F12A F 0.3990(15) 0.6836(8) 0.7487(3) 0.106(5) Uani 0.63(2) 1 d P B 1 F7B F 0.368(3) 0.9960(12) 0.6769(6) 0.084(7) Uani 0.36(5) 1 d P A 2 F8B F 0.253(3) 0.994(2) 0.618(2) 0.094(10) Uani 0.36(5) 1 d P A 2 F9B F 0.4002(17) 0.9467(18) 0.6081(13) 0.051(6) Uani 0.36(5) 1 d P A 2 F10B F 0.378(3) 0.6438(14) 0.6697(10) 0.109(9) Uani 0.37(2) 1 d P B 2 F11B F 0.4806(8) 0.7184(9) 0.7113(10) 0.072(6) Uani 0.37(2) 1 d P B 2 F12B F 0.3551(12) 0.6658(9) 0.7431(7) 0.077(6) Uani 0.37(2) 1 d P B 2 F13 F -0.05358(19) 0.60293(12) 0.48737(8) 0.0429(5) Uani 1 1 d . . . F14 F -0.06979(19) 0.56556(11) 0.56432(8) 0.0424(5) Uani 1 1 d . . . F15 F 0.08499(17) 0.59223(12) 0.53583(8) 0.0427(5) Uani 1 1 d . . . F16 F -0.1374(2) 0.94240(13) 0.52333(9) 0.0535(6) Uani 1 1 d . . . F17 F -0.1418(2) 0.86615(14) 0.46111(9) 0.0592(7) Uani 1 1 d . . . F18 F 0.0060(2) 0.91545(14) 0.48429(10) 0.0590(7) Uani 1 1 d . . . F19 F -0.35123(17) 0.60084(13) 0.73840(9) 0.0471(6) Uani 1 1 d . . . F20 F -0.25140(17) 0.50406(11) 0.73225(9) 0.0426(5) Uani 1 1 d . . . F21 F -0.2736(2) 0.57585(15) 0.66851(9) 0.0580(7) Uani 1 1 d . . . F22 F 0.0354(2) 0.68521(14) 0.87449(8) 0.0531(6) Uani 1 1 d . . . F23 F 0.14024(19) 0.61712(15) 0.83192(9) 0.0529(6) Uani 1 1 d . . . F24 F 0.0017(2) 0.56878(15) 0.86528(9) 0.0616(7) Uani 1 1 d . . . C23 C -0.0686(2) 0.86676(17) 0.70621(12) 0.0210(7) Uani 1 1 d . . . C24 C -0.0319(2) 0.90541(17) 0.74899(11) 0.0212(6) Uani 1 1 d . . . H24 H 0.0368 0.8937 0.7626 0.025 Uiso 1 1 calc R . . C25 C -0.0924(3) 0.96014(17) 0.77212(12) 0.0225(7) Uani 1 1 d . . . C26 C -0.1918(3) 0.98076(18) 0.75265(12) 0.0248(7) Uani 1 1 d . . . H26 H -0.2327 1.0191 0.7680 0.030 Uiso 1 1 calc R . . C27 C -0.2293(3) 0.94354(18) 0.70999(12) 0.0243(7) Uani 1 1 d . . . C28 C -0.1699(2) 0.88709(18) 0.68787(12) 0.0223(7) Uani 1 1 d . . . H28 H -0.1989 0.8615 0.6594 0.027 Uiso 1 1 calc R . . C29 C -0.0560(3) 0.99463(18) 0.82081(13) 0.0287(7) Uani 1 1 d . . . C30 C -0.3357(3) 0.9623(2) 0.68748(14) 0.0320(8) Uani 1 1 d . . . C31 C 0.1267(2) 0.80677(17) 0.68457(11) 0.0213(7) Uani 1 1 d . . . C32 C 0.1712(3) 0.87482(18) 0.66844(11) 0.0224(7) Uani 1 1 d . . . H32 H 0.1250 0.9160 0.6621 0.027 Uiso 1 1 calc R . . C33 C 0.2799(3) 0.88385(18) 0.66153(12) 0.0245(7) Uani 1 1 d . A . C34 C 0.3508(3) 0.82580(19) 0.67178(12) 0.0264(7) Uani 1 1 d . . . H34 H 0.4257 0.8322 0.6677 0.032 Uiso 1 1 calc R . . C35 C 0.3096(3) 0.75888(19) 0.68802(12) 0.0271(7) Uani 1 1 d . B . C36 C 0.1994(2) 0.74914(18) 0.69367(12) 0.0234(7) Uani 1 1 d . . . H36 H 0.1732 0.7018 0.7040 0.028 Uiso 1 1 calc R . . C37 C 0.3235(3) 0.9554(2) 0.64138(14) 0.0314(8) Uani 1 1 d . . . C38 C 0.3832(3) 0.6947(2) 0.70051(16) 0.0393(9) Uani 1 1 d . . . C39 C -0.0288(2) 0.77963(18) 0.62343(11) 0.0206(6) Uani 1 1 d . . . C40 C -0.0177(2) 0.70797(18) 0.60315(12) 0.0236(7) Uani 1 1 d . . . H40 H -0.0003 0.6679 0.6253 0.028 Uiso 1 1 calc R . . C41 C -0.0309(3) 0.69301(18) 0.55196(12) 0.0253(7) Uani 1 1 d . . . C42 C -0.0551(3) 0.7502(2) 0.51827(12) 0.0287(7) Uani 1 1 d . . . H42 H -0.0652 0.7402 0.4833 0.034 Uiso 1 1 calc R . . C43 C -0.0642(3) 0.82250(19) 0.53702(12) 0.0271(7) Uani 1 1 d . . . C44 C -0.0509(2) 0.83642(18) 0.58855(12) 0.0239(7) Uani 1 1 d . . . H44 H -0.0570 0.8863 0.6004 0.029 Uiso 1 1 calc R . . C45 C -0.0180(3) 0.6140(2) 0.53446(13) 0.0310(8) Uani 1 1 d . . . C46 C -0.0853(3) 0.8857(2) 0.50171(13) 0.0365(9) Uani 1 1 d . . . C47 C -0.0422(2) 0.72457(17) 0.71864(11) 0.0210(6) Uani 1 1 d . . . C48 C -0.1316(3) 0.68073(18) 0.70546(12) 0.0242(7) Uani 1 1 d . . . H48 H -0.1706 0.6922 0.6754 0.029 Uiso 1 1 calc R . . C49 C -0.1646(3) 0.62118(18) 0.73499(12) 0.0246(7) Uani 1 1 d . . . C50 C -0.1114(3) 0.60273(18) 0.77921(12) 0.0267(7) Uani 1 1 d . . . H50 H -0.1332 0.5612 0.7989 0.032 Uiso 1 1 calc R . . C51 C -0.0256(3) 0.64631(18) 0.79398(12) 0.0268(7) Uani 1 1 d . . . C52 C 0.0074(3) 0.70648(17) 0.76422(12) 0.0230(7) Uani 1 1 d . . . H52 H 0.0660 0.7361 0.7756 0.028 Uiso 1 1 calc R . . C53 C -0.2597(3) 0.5759(2) 0.71849(14) 0.0334(8) Uani 1 1 d . . . C54 C 0.0359(3) 0.6291(2) 0.84121(14) 0.0356(8) Uani 1 1 d . . . B1 B -0.0036(3) 0.79486(19) 0.68355(13) 0.0204(7) Uani 1 1 d . . . Cl1 Cl 0.3275(3) 0.2787(2) 0.41158(13) 0.0974(15) Uani 0.559(6) 1 d PD C 1 Cl2 Cl 0.4551(4) 0.1646(2) 0.4643(3) 0.176(3) Uani 0.559(6) 1 d PD C 1 C55 C 0.387(3) 0.2409(14) 0.4597(9) 0.259(16) Uiso 0.559(6) 1 d PD C 1 H55A H 0.3296 0.2356 0.4852 0.311 Uiso 0.559(6) 1 calc PR C 1 H55B H 0.4350 0.2803 0.4729 0.311 Uiso 0.559(6) 1 calc PR C 1 O3A O 0.4008(7) 0.1737(4) 0.4918(3) 0.0277(19) Uiso 0.308(4) 1 d PD C 2 C56 C 0.4252(14) -0.0039(9) 0.4814(7) 0.113(4) Uiso 0.441(6) 1 d PD C 2 H56A H 0.3676 -0.0304 0.4988 0.169 Uiso 0.441(6) 1 calc PR C 2 H56B H 0.4934 -0.0293 0.4881 0.169 Uiso 0.441(6) 1 calc PR C 2 H56C H 0.4104 -0.0036 0.4450 0.169 Uiso 0.441(6) 1 calc PR C 2 C57 C 0.4323(15) 0.0840(8) 0.5027(7) 0.113(4) Uiso 0.441(6) 1 d PD C 2 H57A H 0.5104 0.0885 0.5086 0.135 Uiso 0.441(6) 1 calc PR C 2 H57B H 0.4025 0.0776 0.5369 0.135 Uiso 0.441(6) 1 calc PR C 2 C58 C 0.3676(8) 0.2437(5) 0.4653(3) 0.0344(16) Uiso 0.441(6) 1 d PD C 2 H58A H 0.4024 0.2854 0.4838 0.041 Uiso 0.441(6) 1 calc PR C 2 H58B H 0.2897 0.2490 0.4707 0.041 Uiso 0.441(6) 1 calc PR C 2 C59 C 0.3883(9) 0.2600(5) 0.4018(3) 0.0344(16) Uiso 0.441(6) 1 d PD C 2 H59A H 0.4609 0.2445 0.3930 0.052 Uiso 0.441(6) 1 calc PR C 2 H59B H 0.3795 0.3134 0.3947 0.052 Uiso 0.441(6) 1 calc PR C 2 H59C H 0.3362 0.2314 0.3817 0.052 Uiso 0.441(6) 1 calc PR C 2 O3B O 0.3847(17) 0.1655(11) 0.4568(7) 0.032(4) Uiso 0.1322(18) 1 d P C 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02664(16) 0.02115(16) 0.02141(15) 0.00066(10) 0.00080(10) -0.00412(11) O1 0.0508(17) 0.0437(16) 0.0281(13) 0.0078(11) -0.0086(12) -0.0061(13) O2 0.0363(14) 0.0361(15) 0.0425(15) 0.0113(12) -0.0118(11) -0.0073(12) N1 0.0309(16) 0.0204(15) 0.0505(19) 0.0061(13) 0.0072(13) 0.0047(12) N2 0.0295(16) 0.0213(15) 0.0336(15) 0.0013(12) 0.0047(12) -0.0020(12) N3 0.0301(16) 0.0389(19) 0.0349(16) -0.0122(14) 0.0074(13) -0.0105(14) C1 0.0288(18) 0.033(2) 0.0258(16) -0.0073(14) -0.0010(14) -0.0099(15) C2 0.0318(19) 0.0305(19) 0.0249(17) 0.0011(14) -0.0064(14) -0.0086(15) C3 0.0264(18) 0.0264(18) 0.0274(17) -0.0047(14) -0.0031(13) -0.0056(14) C4 0.0288(18) 0.0233(18) 0.0280(17) -0.0026(13) -0.0011(14) -0.0071(14) C5 0.0322(19) 0.0212(17) 0.0328(18) -0.0063(14) -0.0014(14) -0.0042(14) C6 0.038(2) 0.050(2) 0.0315(19) -0.0120(17) 0.0050(16) -0.0145(18) C7 0.049(2) 0.042(2) 0.033(2) 0.0074(17) -0.0083(17) -0.0067(19) C8 0.0278(19) 0.040(2) 0.040(2) -0.0012(16) -0.0004(15) -0.0020(16) C9 0.038(2) 0.031(2) 0.039(2) 0.0093(16) -0.0009(16) -0.0066(16) C10 0.039(2) 0.029(2) 0.045(2) -0.0053(16) 0.0009(17) 0.0011(16) C11 0.0273(18) 0.0237(18) 0.0281(17) 0.0016(13) 0.0008(13) 0.0005(14) C12 0.046(2) 0.022(2) 0.065(3) 0.0106(18) 0.008(2) 0.0004(17) C13 0.041(2) 0.0242(19) 0.055(2) 0.0068(17) 0.0107(18) -0.0053(17) C14 0.0259(18) 0.0231(18) 0.042(2) -0.0045(15) 0.0035(15) -0.0011(14) C15 0.040(2) 0.039(2) 0.051(2) -0.0109(18) 0.0167(18) -0.0099(18) C16 0.035(2) 0.044(2) 0.056(3) -0.0069(19) -0.0061(18) -0.0026(18) C17 0.032(2) 0.027(2) 0.064(3) -0.0029(18) 0.0044(18) 0.0070(16) C18 0.0239(19) 0.039(2) 0.055(2) -0.0178(18) 0.0059(16) -0.0044(16) C19 0.030(2) 0.062(3) 0.080(3) -0.038(3) 0.004(2) -0.001(2) C20 0.037(3) 0.104(5) 0.063(3) -0.055(3) 0.012(2) -0.014(3) C21 0.042(3) 0.103(4) 0.040(2) -0.029(3) 0.0107(19) -0.022(3) C22 0.044(2) 0.065(3) 0.031(2) -0.0127(19) 0.0077(17) -0.020(2) F1 0.0583(15) 0.0258(12) 0.0572(14) -0.0184(10) -0.0156(11) 0.0072(10) F2 0.0621(15) 0.0560(15) 0.0260(11) -0.0046(10) 0.0092(10) -0.0225(12) F3 0.0305(11) 0.0419(13) 0.0371(11) -0.0090(9) -0.0061(9) -0.0032(9) F4 0.0409(13) 0.0666(16) 0.0401(13) 0.0101(11) -0.0030(10) 0.0176(12) F5 0.0328(12) 0.0479(14) 0.0563(14) -0.0140(11) -0.0051(10) 0.0189(10) F6 0.0264(11) 0.0408(14) 0.0765(16) -0.0037(12) -0.0124(10) -0.0032(10) F7A 0.045(5) 0.040(4) 0.088(7) 0.019(4) -0.032(4) -0.026(3) F8A 0.031(3) 0.031(3) 0.077(5) 0.015(4) 0.012(3) -0.002(2) F9A 0.131(12) 0.039(5) 0.068(6) -0.008(4) 0.070(8) -0.015(7) F10A 0.040(3) 0.022(3) 0.126(9) -0.004(4) 0.003(3) 0.004(2) F11A 0.031(3) 0.041(3) 0.131(9) 0.022(4) 0.030(4) 0.013(2) F12A 0.158(12) 0.118(8) 0.043(4) -0.023(4) -0.036(6) 0.108(8) F7B 0.160(18) 0.054(9) 0.039(7) -0.031(7) 0.049(11) -0.070(10) F8B 0.037(9) 0.060(14) 0.19(3) 0.087(15) -0.013(14) -0.011(9) F9B 0.030(8) 0.048(10) 0.077(13) 0.021(9) 0.034(6) 0.002(4) F10B 0.14(2) 0.091(15) 0.093(12) -0.060(11) -0.036(12) 0.090(14) F11B 0.026(4) 0.065(7) 0.125(14) 0.035(8) -0.020(6) 0.006(4) F12B 0.058(7) 0.060(7) 0.113(13) 0.063(9) 0.017(7) 0.029(5) F13 0.0583(14) 0.0368(13) 0.0335(11) -0.0130(9) -0.0047(10) -0.0013(11) F14 0.0585(14) 0.0246(11) 0.0444(12) -0.0055(9) 0.0104(10) -0.0117(10) F15 0.0418(13) 0.0342(12) 0.0522(13) -0.0106(10) 0.0042(10) 0.0067(10) F16 0.0805(18) 0.0385(13) 0.0416(13) 0.0107(10) 0.0051(12) 0.0190(13) F17 0.092(2) 0.0414(14) 0.0435(14) 0.0088(11) -0.0293(13) -0.0070(13) F18 0.0644(17) 0.0477(15) 0.0652(16) 0.0236(12) 0.0150(13) -0.0086(12) F19 0.0274(12) 0.0393(13) 0.0745(16) 0.0010(12) 0.0026(11) -0.0040(10) F20 0.0402(12) 0.0232(11) 0.0645(15) -0.0005(10) 0.0044(10) -0.0135(9) F21 0.0707(17) 0.0614(16) 0.0417(13) -0.0011(11) -0.0107(11) -0.0448(14) F22 0.0782(18) 0.0492(15) 0.0313(12) -0.0075(10) -0.0141(11) 0.0049(13) F23 0.0478(15) 0.0679(17) 0.0428(13) 0.0045(12) -0.0123(11) 0.0136(12) F24 0.088(2) 0.0508(16) 0.0454(14) 0.0258(12) -0.0204(13) -0.0238(14) C23 0.0197(16) 0.0166(16) 0.0267(16) 0.0015(12) 0.0046(12) -0.0052(12) C24 0.0193(16) 0.0179(16) 0.0264(16) 0.0027(12) 0.0002(12) -0.0026(12) C25 0.0268(17) 0.0138(15) 0.0272(16) 0.0016(12) 0.0028(13) -0.0059(13) C26 0.0257(17) 0.0171(16) 0.0318(17) -0.0006(13) 0.0073(13) 0.0004(13) C27 0.0213(16) 0.0223(17) 0.0294(17) 0.0031(13) 0.0023(13) -0.0023(13) C28 0.0228(16) 0.0192(16) 0.0249(16) -0.0004(13) 0.0011(12) -0.0045(13) C29 0.0331(19) 0.0199(17) 0.0331(18) -0.0034(14) 0.0041(14) -0.0023(14) C30 0.0278(19) 0.0297(19) 0.039(2) -0.0027(15) -0.0005(15) 0.0034(15) C31 0.0233(16) 0.0203(17) 0.0205(15) -0.0047(12) 0.0008(12) -0.0020(13) C32 0.0227(16) 0.0212(17) 0.0233(16) -0.0025(12) 0.0026(12) 0.0001(13) C33 0.0263(17) 0.0226(17) 0.0246(16) -0.0057(13) 0.0040(13) -0.0037(14) C34 0.0176(16) 0.0293(18) 0.0322(17) -0.0067(14) 0.0035(13) -0.0040(14) C35 0.0237(17) 0.0272(18) 0.0304(17) -0.0048(14) 0.0015(13) 0.0010(14) C36 0.0255(17) 0.0195(16) 0.0253(16) -0.0039(13) 0.0025(13) -0.0036(13) C37 0.0272(19) 0.0269(19) 0.040(2) 0.0000(16) 0.0073(16) -0.0023(15) C38 0.028(2) 0.032(2) 0.057(3) -0.0010(19) 0.0026(18) 0.0081(16) C39 0.0151(15) 0.0226(17) 0.0241(15) -0.0023(13) 0.0018(12) -0.0035(12) C40 0.0206(16) 0.0231(17) 0.0272(16) 0.0016(13) 0.0030(13) -0.0035(13) C41 0.0223(17) 0.0244(18) 0.0294(17) -0.0037(14) 0.0020(13) -0.0036(13) C42 0.0279(18) 0.034(2) 0.0238(16) -0.0054(14) 0.0017(13) -0.0071(15) C43 0.0254(17) 0.0274(18) 0.0287(17) 0.0034(14) 0.0023(13) -0.0056(14) C44 0.0219(16) 0.0194(16) 0.0305(17) -0.0016(13) 0.0017(13) -0.0049(13) C45 0.032(2) 0.032(2) 0.0291(18) -0.0051(15) 0.0043(14) -0.0057(16) C46 0.046(2) 0.034(2) 0.0293(19) -0.0001(16) 0.0002(16) -0.0047(18) C47 0.0227(16) 0.0166(16) 0.0238(15) -0.0039(12) 0.0069(12) 0.0011(12) C48 0.0228(17) 0.0228(17) 0.0271(16) 0.0001(13) 0.0032(13) 0.0000(13) C49 0.0241(17) 0.0182(16) 0.0316(17) -0.0040(13) 0.0054(13) -0.0025(13) C50 0.0330(19) 0.0195(17) 0.0280(17) 0.0026(13) 0.0079(14) -0.0032(14) C51 0.0332(19) 0.0219(17) 0.0252(16) -0.0011(13) 0.0036(14) 0.0006(14) C52 0.0220(16) 0.0202(16) 0.0270(16) -0.0049(13) 0.0027(13) -0.0028(13) C53 0.035(2) 0.029(2) 0.0362(19) 0.0022(15) 0.0018(15) -0.0094(16) C54 0.042(2) 0.029(2) 0.036(2) 0.0035(15) -0.0007(16) -0.0024(16) B1 0.0204(18) 0.0163(17) 0.0244(18) -0.0009(14) -0.0006(14) -0.0008(14) Cl1 0.091(3) 0.099(2) 0.101(2) 0.0223(18) -0.047(2) -0.0214(19) Cl2 0.100(3) 0.094(3) 0.329(8) -0.113(4) -0.104(4) 0.041(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 O1 1.995(2) . ? Ru1 O2 2.029(3) . ? Ru1 C11 2.051(3) . ? Ru1 N3 2.155(3) . ? Ru1 C1 2.183(3) . ? Ru1 C5 2.195(3) . ? Ru1 C2 2.212(3) . ? Ru1 C4 2.263(3) . ? Ru1 C3 2.278(3) . ? O1 O2 1.390(4) . ? N1 C11 1.349(4) . ? N1 C12 1.381(5) . ? N1 C17 1.459(5) . ? N2 C11 1.347(4) . ? N2 C13 1.387(5) . ? N2 C14 1.485(4) . ? N3 C18 1.342(5) . ? N3 C22 1.345(5) . ? C1 C5 1.430(5) . ? C1 C2 1.439(5) . ? C1 C6 1.494(5) . ? C2 C3 1.425(5) . ? C2 C7 1.495(5) . ? C3 C4 1.419(5) . ? C3 C8 1.502(5) . ? C4 C5 1.431(5) . ? C4 C9 1.497(5) . ? C5 C10 1.488(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 C13 1.330(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C16 1.508(5) . ? C14 C15 1.520(5) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.499(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.385(6) . ? C19 C20 1.381(8) . ? C19 H19 0.9500 . ? C20 C21 1.368(8) . ? C20 H20 0.9500 . ? C21 C22 1.384(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? F1 C29 1.342(4) . ? F2 C29 1.338(4) . ? F3 C29 1.338(4) . ? F4 C30 1.341(4) . ? F5 C30 1.337(4) . ? F6 C30 1.336(4) . ? F7A C37 1.336(9) . ? F8A C37 1.339(17) . ? F9A C37 1.309(17) . ? F10A C38 1.340(10) . ? F11A C38 1.333(7) . ? F12A C38 1.303(9) . ? F7B C37 1.308(17) . ? F8B C37 1.28(3) . ? F9B C37 1.32(3) . ? F10B C38 1.223(17) . ? F11B C38 1.317(10) . ? F12B C38 1.293(15) . ? F13 C45 1.333(4) . ? F14 C45 1.344(4) . ? F15 C45 1.345(4) . ? F16 C46 1.338(4) . ? F17 C46 1.325(4) . ? F18 C46 1.346(4) . ? F19 C53 1.342(4) . ? F20 C53 1.340(4) . ? F21 C53 1.332(4) . ? F22 C54 1.336(4) . ? F23 C54 1.347(4) . ? F24 C54 1.327(4) . ? C23 C24 1.399(4) . ? C23 C28 1.400(5) . ? C23 B1 1.639(5) . ? C24 C25 1.385(4) . ? C24 H24 0.9500 . ? C25 C26 1.389(5) . ? C25 C29 1.495(5) . ? C26 C27 1.387(5) . ? C26 H26 0.9500 . ? C27 C28 1.387(5) . ? C27 C30 1.489(5) . ? C28 H28 0.9500 . ? C31 C36 1.394(5) . ? C31 C32 1.407(4) . ? C31 B1 1.642(5) . ? C32 C33 1.382(4) . ? C32 H32 0.9500 . ? C33 C34 1.390(5) . ? C33 C37 1.493(5) . ? C34 C35 1.375(5) . ? C34 H34 0.9500 . ? C35 C36 1.398(4) . ? C35 C38 1.506(5) . ? C36 H36 0.9500 . ? C39 C40 1.398(4) . ? C39 C44 1.398(5) . ? C39 B1 1.641(4) . ? C40 C41 1.389(4) . ? C40 H40 0.9500 . ? C41 C42 1.388(5) . ? C41 C45 1.498(5) . ? C42 C43 1.391(5) . ? C42 H42 0.9500 . ? C43 C44 1.394(5) . ? C43 C46 1.488(5) . ? C44 H44 0.9500 . ? C47 C52 1.388(5) . ? C47 C48 1.406(5) . ? C47 B1 1.639(5) . ? C48 C49 1.387(5) . ? C48 H48 0.9500 . ? C49 C50 1.379(5) . ? C49 C53 1.499(5) . ? C50 C51 1.379(5) . ? C50 H50 0.9500 . ? C51 C52 1.399(5) . ? C51 C54 1.491(5) . ? C52 H52 0.9500 . ? Cl1 C55 1.613(17) . ? Cl2 C55 1.616(17) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? O3A C58 1.491(10) . ? O3A C57 1.677(14) . ? C56 C57 1.673(15) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.730(11) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 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 O1 Ru1 O2 40.41(11) . . ? O1 Ru1 C11 115.81(12) . . ? O2 Ru1 C11 85.68(12) . . ? O1 Ru1 N3 83.54(12) . . ? O2 Ru1 N3 107.20(11) . . ? C11 Ru1 N3 84.33(12) . . ? O1 Ru1 C1 125.10(13) . . ? O2 Ru1 C1 106.42(12) . . ? C11 Ru1 C1 95.99(13) . . ? N3 Ru1 C1 146.30(13) . . ? O1 Ru1 C5 90.43(12) . . ? O2 Ru1 C5 90.34(12) . . ? C11 Ru1 C5 129.97(13) . . ? N3 Ru1 C5 143.27(12) . . ? C1 Ru1 C5 38.14(13) . . ? O1 Ru1 C2 149.66(12) . . ? O2 Ru1 C2 144.44(13) . . ? C11 Ru1 C2 93.56(13) . . ? N3 Ru1 C2 108.09(13) . . ? C1 Ru1 C2 38.21(13) . . ? C5 Ru1 C2 63.24(13) . . ? O1 Ru1 C4 88.10(12) . . ? O2 Ru1 C4 111.59(11) . . ? C11 Ru1 C4 155.20(12) . . ? N3 Ru1 C4 106.00(12) . . ? C1 Ru1 C4 62.80(12) . . ? C5 Ru1 C4 37.42(12) . . ? C2 Ru1 C4 61.95(12) . . ? O1 Ru1 C3 118.61(12) . . ? O2 Ru1 C3 147.96(12) . . ? C11 Ru1 C3 123.97(13) . . ? N3 Ru1 C3 89.26(12) . . ? C1 Ru1 C3 62.61(12) . . ? C5 Ru1 C3 62.10(13) . . ? C2 Ru1 C3 36.97(12) . . ? C4 Ru1 C3 36.41(12) . . ? O2 O1 Ru1 71.11(14) . . ? O1 O2 Ru1 68.47(15) . . ? C11 N1 C12 111.0(3) . . ? C11 N1 C17 123.5(3) . . ? C12 N1 C17 125.5(3) . . ? C11 N2 C13 110.5(3) . . ? C11 N2 C14 127.2(3) . . ? C13 N2 C14 122.2(3) . . ? C18 N3 C22 118.0(3) . . ? C18 N3 Ru1 125.4(2) . . ? C22 N3 Ru1 116.1(3) . . ? C5 C1 C2 107.3(3) . . ? C5 C1 C6 126.5(3) . . ? C2 C1 C6 125.4(3) . . ? C5 C1 Ru1 71.39(18) . . ? C2 C1 Ru1 72.00(19) . . ? C6 C1 Ru1 129.8(2) . . ? C3 C2 C1 108.2(3) . . ? C3 C2 C7 126.2(3) . . ? C1 C2 C7 124.3(3) . . ? C3 C2 Ru1 74.05(19) . . ? C1 C2 Ru1 69.79(18) . . ? C7 C2 Ru1 132.0(3) . . ? C4 C3 C2 108.2(3) . . ? C4 C3 C8 125.8(3) . . ? C2 C3 C8 126.0(3) . . ? C4 C3 Ru1 71.22(18) . . ? C2 C3 Ru1 68.99(19) . . ? C8 C3 Ru1 126.2(2) . . ? C3 C4 C5 108.2(3) . . ? C3 C4 C9 126.8(3) . . ? C5 C4 C9 125.1(3) . . ? C3 C4 Ru1 72.37(19) . . ? C5 C4 Ru1 68.69(18) . . ? C9 C4 Ru1 124.9(2) . . ? C1 C5 C4 108.2(3) . . ? C1 C5 C10 126.7(3) . . ? C4 C5 C10 125.1(3) . . ? C1 C5 Ru1 70.48(19) . . ? C4 C5 Ru1 73.90(19) . . ? C10 C5 Ru1 122.9(2) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 N1 104.6(3) . . ? N2 C11 Ru1 131.8(2) . . ? N1 C11 Ru1 123.2(2) . . ? C13 C12 N1 106.7(3) . . ? C13 C12 H12 126.6 . . ? N1 C12 H12 126.6 . . ? C12 C13 N2 107.1(3) . . ? C12 C13 H13 126.5 . . ? N2 C13 H13 126.5 . . ? N2 C14 C16 110.5(3) . . ? N2 C14 C15 110.1(3) . . ? C16 C14 C15 111.8(3) . . ? N2 C14 H14 108.1 . . ? C16 C14 H14 108.1 . . ? C15 C14 H14 108.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 113.5(3) . . ? N1 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? N1 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N3 C18 C19 122.1(4) . . ? N3 C18 C17 117.8(3) . . ? C19 C18 C17 119.9(4) . . ? C20 C19 C18 119.2(5) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C21 C20 C19 119.1(4) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 119.0(5) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? N3 C22 C21 122.6(5) . . ? N3 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? C24 C23 C28 116.0(3) . . ? C24 C23 B1 121.7(3) . . ? C28 C23 B1 121.8(3) . . ? C25 C24 C23 122.1(3) . . ? C25 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? C24 C25 C26 121.0(3) . . ? C24 C25 C29 120.7(3) . . ? C26 C25 C29 118.2(3) . . ? C27 C26 C25 117.8(3) . . ? C27 C26 H26 121.1 . . ? C25 C26 H26 121.1 . . ? C28 C27 C26 121.0(3) . . ? C28 C27 C30 118.4(3) . . ? C26 C27 C30 120.6(3) . . ? C27 C28 C23 122.0(3) . . ? C27 C28 H28 119.0 . . ? C23 C28 H28 119.0 . . ? F2 C29 F3 106.4(3) . . ? F2 C29 F1 106.4(3) . . ? F3 C29 F1 106.4(3) . . ? F2 C29 C25 111.8(3) . . ? F3 C29 C25 113.0(3) . . ? F1 C29 C25 112.4(3) . . ? F6 C30 F5 105.9(3) . . ? F6 C30 F4 106.2(3) . . ? F5 C30 F4 106.2(3) . . ? F6 C30 C27 112.1(3) . . ? F5 C30 C27 113.6(3) . . ? F4 C30 C27 112.2(3) . . ? C36 C31 C32 115.7(3) . . ? C36 C31 B1 123.4(3) . . ? C32 C31 B1 120.2(3) . . ? C33 C32 C31 122.3(3) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C32 C33 C34 120.8(3) . . ? C32 C33 C37 120.7(3) . . ? C34 C33 C37 118.4(3) . . ? C35 C34 C33 118.1(3) . . ? C35 C34 H34 120.9 . . ? C33 C34 H34 120.9 . . ? C34 C35 C36 121.0(3) . . ? C34 C35 C38 120.2(3) . . ? C36 C35 C38 118.8(3) . . ? C31 C36 C35 122.0(3) . . ? C31 C36 H36 119.0 . . ? C35 C36 H36 119.0 . . ? F8B C37 F7B 109(2) . . ? F8B C37 F9A 93(2) . . ? F7B C37 F9A 115.6(11) . . ? F8B C37 F9B 104(2) . . ? F7B C37 F9B 103.7(17) . . ? F8B C37 F7A 119(2) . . ? F9A C37 F7A 104.9(10) . . ? F9B C37 F7A 92.4(14) . . ? F7B C37 F8A 94.0(16) . . ? F9A C37 F8A 107.3(12) . . ? F9B C37 F8A 116.4(14) . . ? F7A C37 F8A 104.3(8) . . ? F8B C37 C33 112.9(15) . . ? F7B C37 C33 112.0(9) . . ? F9A C37 C33 112.5(9) . . ? F9B C37 C33 114.1(14) . . ? F7A C37 C33 112.9(5) . . ? F8A C37 C33 114.2(8) . . ? F10B C38 F12B 105.8(16) . . ? F10B C38 F12A 123.1(13) . . ? F10B C38 F11B 115.1(11) . . ? F12B C38 F11B 101.6(9) . . ? F12A C38 F11B 73.1(7) . . ? F10B C38 F11A 76.4(14) . . ? F12B C38 F11A 132.9(7) . . ? F12A C38 F11A 110.2(6) . . ? F12B C38 F10A 79.9(10) . . ? F12A C38 F10A 103.0(9) . . ? F11B C38 F10A 132.6(10) . . ? F11A C38 F10A 102.1(6) . . ? F10B C38 C35 113.2(10) . . ? F12B C38 C35 108.9(7) . . ? F12A C38 C35 114.6(5) . . ? F11B C38 C35 111.3(7) . . ? F11A C38 C35 113.0(4) . . ? F10A C38 C35 112.8(6) . . ? C40 C39 C44 115.7(3) . . ? C40 C39 B1 120.4(3) . . ? C44 C39 B1 123.6(3) . . ? C41 C40 C39 122.7(3) . . ? C41 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? C42 C41 C40 120.4(3) . . ? C42 C41 C45 121.4(3) . . ? C40 C41 C45 118.1(3) . . ? C41 C42 C43 118.4(3) . . ? C41 C42 H42 120.8 . . ? C43 C42 H42 120.8 . . ? C42 C43 C44 120.4(3) . . ? C42 C43 C46 119.8(3) . . ? C44 C43 C46 119.8(3) . . ? C43 C44 C39 122.4(3) . . ? C43 C44 H44 118.8 . . ? C39 C44 H44 118.8 . . ? F13 C45 F14 107.3(3) . . ? F13 C45 F15 106.9(3) . . ? F14 C45 F15 105.4(3) . . ? F13 C45 C41 113.1(3) . . ? F14 C45 C41 111.9(3) . . ? F15 C45 C41 111.8(3) . . ? F17 C46 F16 106.8(3) . . ? F17 C46 F18 105.8(3) . . ? F16 C46 F18 105.4(3) . . ? F17 C46 C43 113.4(3) . . ? F16 C46 C43 113.1(3) . . ? F18 C46 C43 111.8(3) . . ? C52 C47 C48 115.5(3) . . ? C52 C47 B1 122.7(3) . . ? C48 C47 B1 121.8(3) . . ? C49 C48 C47 122.0(3) . . ? C49 C48 H48 119.0 . . ? C47 C48 H48 119.0 . . ? C50 C49 C48 121.2(3) . . ? C50 C49 C53 119.4(3) . . ? C48 C49 C53 119.4(3) . . ? C51 C50 C49 118.1(3) . . ? C51 C50 H50 121.0 . . ? C49 C50 H50 121.0 . . ? C50 C51 C52 120.6(3) . . ? C50 C51 C54 120.8(3) . . ? C52 C51 C54 118.6(3) . . ? C47 C52 C51 122.5(3) . . ? C47 C52 H52 118.8 . . ? C51 C52 H52 118.8 . . ? F21 C53 F20 106.1(3) . . ? F21 C53 F19 106.7(3) . . ? F20 C53 F19 106.0(3) . . ? F21 C53 C49 112.6(3) . . ? F20 C53 C49 112.4(3) . . ? F19 C53 C49 112.5(3) . . ? F24 C54 F22 106.9(3) . . ? F24 C54 F23 106.1(3) . . ? F22 C54 F23 104.6(3) . . ? F24 C54 C51 113.8(3) . . ? F22 C54 C51 113.0(3) . . ? F23 C54 C51 111.7(3) . . ? C23 B1 C47 104.2(2) . . ? C23 B1 C39 113.2(3) . . ? C47 B1 C39 111.5(3) . . ? C23 B1 C31 112.8(3) . . ? C47 B1 C31 112.9(3) . . ? C39 B1 C31 102.5(2) . . ? Cl1 C55 Cl2 130.7(17) . . ? Cl1 C55 H55A 104.6 . . ? Cl2 C55 H55A 104.6 . . ? Cl1 C55 H55B 104.6 . . ? Cl2 C55 H55B 104.6 . . ? H55A C55 H55B 105.7 . . ? C58 O3A C57 161.3(9) . . ? C57 C56 H56A 109.5 . . ? C57 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C57 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C56 C57 O3A 146.3(14) . . ? C56 C57 H57A 100.3 . . ? O3A C57 H57A 100.3 . . ? C56 C57 H57B 100.3 . . ? O3A C57 H57B 100.3 . . ? H57A C57 H57B 104.2 . . ? O3A C58 C59 123.7(7) . . ? O3A C58 H58A 106.4 . . ? C59 C58 H58A 106.4 . . ? O3A C58 H58B 106.4 . . ? C59 C58 H58B 106.4 . . ? H58A C58 H58B 106.5 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 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 C11 Ru1 O1 O2 45.8(2) . . . . ? N3 Ru1 O1 O2 126.30(17) . . . . ? C1 Ru1 O1 O2 -73.0(2) . . . . ? C5 Ru1 O1 O2 -90.02(18) . . . . ? C2 Ru1 O1 O2 -118.5(3) . . . . ? C4 Ru1 O1 O2 -127.37(18) . . . . ? C3 Ru1 O1 O2 -148.09(16) . . . . ? C11 Ru1 O2 O1 -139.66(18) . . . . ? N3 Ru1 O2 O1 -56.96(19) . . . . ? C1 Ru1 O2 O1 125.35(18) . . . . ? C5 Ru1 O2 O1 90.27(18) . . . . ? C2 Ru1 O2 O1 130.3(2) . . . . ? C4 Ru1 O2 O1 58.68(19) . . . . ? C3 Ru1 O2 O1 61.0(3) . . . . ? O1 Ru1 N3 C18 -154.0(3) . . . . ? O2 Ru1 N3 C18 -120.8(3) . . . . ? C11 Ru1 N3 C18 -37.1(3) . . . . ? C1 Ru1 N3 C18 55.2(4) . . . . ? C5 Ru1 N3 C18 124.0(3) . . . . ? C2 Ru1 N3 C18 54.8(3) . . . . ? C4 Ru1 N3 C18 119.9(3) . . . . ? C3 Ru1 N3 C18 87.1(3) . . . . ? O1 Ru1 N3 C22 34.1(3) . . . . ? O2 Ru1 N3 C22 67.3(3) . . . . ? C11 Ru1 N3 C22 151.0(3) . . . . ? C1 Ru1 N3 C22 -116.7(3) . . . . ? C5 Ru1 N3 C22 -47.9(4) . . . . ? C2 Ru1 N3 C22 -117.1(3) . . . . ? C4 Ru1 N3 C22 -52.0(3) . . . . ? C3 Ru1 N3 C22 -84.8(3) . . . . ? O1 Ru1 C1 C5 -28.3(2) . . . . ? O2 Ru1 C1 C5 -68.6(2) . . . . ? C11 Ru1 C1 C5 -155.8(2) . . . . ? N3 Ru1 C1 C5 115.4(3) . . . . ? C2 Ru1 C1 C5 116.0(3) . . . . ? C4 Ru1 C1 C5 37.68(19) . . . . ? C3 Ru1 C1 C5 78.8(2) . . . . ? O1 Ru1 C1 C2 -144.35(19) . . . . ? O2 Ru1 C1 C2 175.39(18) . . . . ? C11 Ru1 C1 C2 88.1(2) . . . . ? N3 Ru1 C1 C2 -0.6(3) . . . . ? C5 Ru1 C1 C2 -116.0(3) . . . . ? C4 Ru1 C1 C2 -78.4(2) . . . . ? C3 Ru1 C1 C2 -37.19(19) . . . . ? O1 Ru1 C1 C6 94.2(4) . . . . ? O2 Ru1 C1 C6 53.9(4) . . . . ? C11 Ru1 C1 C6 -33.3(4) . . . . ? N3 Ru1 C1 C6 -122.1(3) . . . . ? C5 Ru1 C1 C6 122.5(4) . . . . ? C2 Ru1 C1 C6 -121.5(4) . . . . ? C4 Ru1 C1 C6 160.1(4) . . . . ? C3 Ru1 C1 C6 -158.7(4) . . . . ? C5 C1 C2 C3 1.5(4) . . . . ? C6 C1 C2 C3 -168.9(3) . . . . ? Ru1 C1 C2 C3 64.6(2) . . . . ? C5 C1 C2 C7 169.2(3) . . . . ? C6 C1 C2 C7 -1.2(5) . . . . ? Ru1 C1 C2 C7 -127.7(3) . . . . ? C5 C1 C2 Ru1 -63.1(2) . . . . ? C6 C1 C2 Ru1 126.5(3) . . . . ? O1 Ru1 C2 C3 -46.1(3) . . . . ? O2 Ru1 C2 C3 -124.4(2) . . . . ? C11 Ru1 C2 C3 148.0(2) . . . . ? N3 Ru1 C2 C3 62.8(2) . . . . ? C1 Ru1 C2 C3 -116.8(3) . . . . ? C5 Ru1 C2 C3 -78.4(2) . . . . ? C4 Ru1 C2 C3 -36.1(2) . . . . ? O1 Ru1 C2 C1 70.7(3) . . . . ? O2 Ru1 C2 C1 -7.6(3) . . . . ? C11 Ru1 C2 C1 -95.2(2) . . . . ? N3 Ru1 C2 C1 179.64(19) . . . . ? C5 Ru1 C2 C1 38.4(2) . . . . ? C4 Ru1 C2 C1 80.8(2) . . . . ? C3 Ru1 C2 C1 116.8(3) . . . . ? O1 Ru1 C2 C7 -170.8(3) . . . . ? O2 Ru1 C2 C7 110.8(4) . . . . ? C11 Ru1 C2 C7 23.3(4) . . . . ? N3 Ru1 C2 C7 -61.9(4) . . . . ? C1 Ru1 C2 C7 118.5(4) . . . . ? C5 Ru1 C2 C7 156.9(4) . . . . ? C4 Ru1 C2 C7 -160.8(4) . . . . ? C3 Ru1 C2 C7 -124.7(4) . . . . ? C1 C2 C3 C4 -1.1(4) . . . . ? C7 C2 C3 C4 -168.5(3) . . . . ? Ru1 C2 C3 C4 60.7(2) . . . . ? C1 C2 C3 C8 178.0(3) . . . . ? C7 C2 C3 C8 10.6(6) . . . . ? Ru1 C2 C3 C8 -120.2(3) . . . . ? C1 C2 C3 Ru1 -61.8(2) . . . . ? C7 C2 C3 Ru1 130.8(4) . . . . ? O1 Ru1 C3 C4 36.6(2) . . . . ? O2 Ru1 C3 C4 -3.7(3) . . . . ? C11 Ru1 C3 C4 -158.54(19) . . . . ? N3 Ru1 C3 C4 118.8(2) . . . . ? C1 Ru1 C3 C4 -80.5(2) . . . . ? C5 Ru1 C3 C4 -37.23(19) . . . . ? C2 Ru1 C3 C4 -119.0(3) . . . . ? O1 Ru1 C3 C2 155.5(2) . . . . ? O2 Ru1 C3 C2 115.3(3) . . . . ? C11 Ru1 C3 C2 -39.6(3) . . . . ? N3 Ru1 C3 C2 -122.2(2) . . . . ? C1 Ru1 C3 C2 38.4(2) . . . . ? C5 Ru1 C3 C2 81.7(2) . . . . ? C4 Ru1 C3 C2 119.0(3) . . . . ? O1 Ru1 C3 C8 -84.6(3) . . . . ? O2 Ru1 C3 C8 -124.8(3) . . . . ? C11 Ru1 C3 C8 80.3(3) . . . . ? N3 Ru1 C3 C8 -2.4(3) . . . . ? C1 Ru1 C3 C8 158.3(3) . . . . ? C5 Ru1 C3 C8 -158.4(3) . . . . ? C2 Ru1 C3 C8 119.9(4) . . . . ? C4 Ru1 C3 C8 -121.2(4) . . . . ? C2 C3 C4 C5 0.3(4) . . . . ? C8 C3 C4 C5 -178.8(3) . . . . ? Ru1 C3 C4 C5 59.6(2) . . . . ? C2 C3 C4 C9 179.9(3) . . . . ? C8 C3 C4 C9 0.8(5) . . . . ? Ru1 C3 C4 C9 -120.8(3) . . . . ? C2 C3 C4 Ru1 -59.3(2) . . . . ? C8 C3 C4 Ru1 121.6(3) . . . . ? O1 Ru1 C4 C3 -148.4(2) . . . . ? O2 Ru1 C4 C3 177.91(18) . . . . ? C11 Ru1 C4 C3 46.3(4) . . . . ? N3 Ru1 C4 C3 -65.7(2) . . . . ? C1 Ru1 C4 C3 80.0(2) . . . . ? C5 Ru1 C4 C3 118.4(3) . . . . ? C2 Ru1 C4 C3 36.60(19) . . . . ? O1 Ru1 C4 C5 93.2(2) . . . . ? O2 Ru1 C4 C5 59.5(2) . . . . ? C11 Ru1 C4 C5 -72.0(4) . . . . ? N3 Ru1 C4 C5 175.9(2) . . . . ? C1 Ru1 C4 C5 -38.4(2) . . . . ? C2 Ru1 C4 C5 -81.8(2) . . . . ? C3 Ru1 C4 C5 -118.4(3) . . . . ? O1 Ru1 C4 C9 -25.5(3) . . . . ? O2 Ru1 C4 C9 -59.1(3) . . . . ? C11 Ru1 C4 C9 169.3(3) . . . . ? N3 Ru1 C4 C9 57.2(3) . . . . ? C1 Ru1 C4 C9 -157.1(3) . . . . ? C5 Ru1 C4 C9 -118.7(4) . . . . ? C2 Ru1 C4 C9 159.5(3) . . . . ? C3 Ru1 C4 C9 122.9(4) . . . . ? C2 C1 C5 C4 -1.3(4) . . . . ? C6 C1 C5 C4 169.0(3) . . . . ? Ru1 C1 C5 C4 -64.8(2) . . . . ? C2 C1 C5 C10 -179.4(3) . . . . ? C6 C1 C5 C10 -9.1(6) . . . . ? Ru1 C1 C5 C10 117.1(3) . . . . ? C2 C1 C5 Ru1 63.5(2) . . . . ? C6 C1 C5 Ru1 -126.2(3) . . . . ? C3 C4 C5 C1 0.6(4) . . . . ? C9 C4 C5 C1 -179.0(3) . . . . ? Ru1 C4 C5 C1 62.6(2) . . . . ? C3 C4 C5 C10 178.8(3) . . . . ? C9 C4 C5 C10 -0.8(5) . . . . ? Ru1 C4 C5 C10 -119.3(3) . . . . ? C3 C4 C5 Ru1 -62.0(2) . . . . ? C9 C4 C5 Ru1 118.5(3) . . . . ? O1 Ru1 C5 C1 157.2(2) . . . . ? O2 Ru1 C5 C1 116.8(2) . . . . ? C11 Ru1 C5 C1 32.1(3) . . . . ? N3 Ru1 C5 C1 -123.1(2) . . . . ? C2 Ru1 C5 C1 -38.5(2) . . . . ? C4 Ru1 C5 C1 -116.5(3) . . . . ? C3 Ru1 C5 C1 -80.3(2) . . . . ? O1 Ru1 C5 C4 -86.3(2) . . . . ? O2 Ru1 C5 C4 -126.7(2) . . . . ? C11 Ru1 C5 C4 148.6(2) . . . . ? N3 Ru1 C5 C4 -6.6(3) . . . . ? C1 Ru1 C5 C4 116.5(3) . . . . ? C2 Ru1 C5 C4 78.0(2) . . . . ? C3 Ru1 C5 C4 36.23(19) . . . . ? O1 Ru1 C5 C10 35.4(3) . . . . ? O2 Ru1 C5 C10 -5.0(3) . . . . ? C11 Ru1 C5 C10 -89.7(3) . . . . ? N3 Ru1 C5 C10 115.1(3) . . . . ? C1 Ru1 C5 C10 -121.8(4) . . . . ? C2 Ru1 C5 C10 -160.3(3) . . . . ? C4 Ru1 C5 C10 121.7(4) . . . . ? C3 Ru1 C5 C10 157.9(3) . . . . ? C13 N2 C11 N1 -1.1(4) . . . . ? C14 N2 C11 N1 -179.8(3) . . . . ? C13 N2 C11 Ru1 172.2(3) . . . . ? C14 N2 C11 Ru1 -6.5(5) . . . . ? C12 N1 C11 N2 1.2(4) . . . . ? C17 N1 C11 N2 -178.9(3) . . . . ? C12 N1 C11 Ru1 -172.8(3) . . . . ? C17 N1 C11 Ru1 7.1(5) . . . . ? O1 Ru1 C11 N2 -61.9(3) . . . . ? O2 Ru1 C11 N2 -34.1(3) . . . . ? N3 Ru1 C11 N2 -141.9(3) . . . . ? C1 Ru1 C11 N2 72.0(3) . . . . ? C5 Ru1 C11 N2 52.7(4) . . . . ? C2 Ru1 C11 N2 110.2(3) . . . . ? C4 Ru1 C11 N2 101.6(4) . . . . ? C3 Ru1 C11 N2 132.8(3) . . . . ? O1 Ru1 C11 N1 110.3(3) . . . . ? O2 Ru1 C11 N1 138.1(3) . . . . ? N3 Ru1 C11 N1 30.3(3) . . . . ? C1 Ru1 C11 N1 -115.8(3) . . . . ? C5 Ru1 C11 N1 -135.1(3) . . . . ? C2 Ru1 C11 N1 -77.5(3) . . . . ? C4 Ru1 C11 N1 -86.1(4) . . . . ? C3 Ru1 C11 N1 -54.9(3) . . . . ? C11 N1 C12 C13 -0.9(5) . . . . ? C17 N1 C12 C13 179.2(4) . . . . ? N1 C12 C13 N2 0.2(5) . . . . ? C11 N2 C13 C12 0.6(5) . . . . ? C14 N2 C13 C12 179.3(3) . . . . ? C11 N2 C14 C16 107.9(4) . . . . ? C13 N2 C14 C16 -70.6(4) . . . . ? C11 N2 C14 C15 -128.1(4) . . . . ? C13 N2 C14 C15 53.4(4) . . . . ? C11 N1 C17 C18 -55.5(5) . . . . ? C12 N1 C17 C18 124.4(4) . . . . ? C22 N3 C18 C19 1.5(5) . . . . ? Ru1 N3 C18 C19 -170.3(3) . . . . ? C22 N3 C18 C17 176.8(3) . . . . ? Ru1 N3 C18 C17 5.0(5) . . . . ? N1 C17 C18 N3 46.3(5) . . . . ? N1 C17 C18 C19 -138.3(4) . . . . ? N3 C18 C19 C20 0.0(6) . . . . ? C17 C18 C19 C20 -175.1(4) . . . . ? C18 C19 C20 C21 -0.9(6) . . . . ? C19 C20 C21 C22 0.2(7) . . . . ? C18 N3 C22 C21 -2.3(6) . . . . ? Ru1 N3 C22 C21 170.3(3) . . . . ? C20 C21 C22 N3 1.4(6) . . . . ? C28 C23 C24 C25 0.5(4) . . . . ? B1 C23 C24 C25 -171.9(3) . . . . ? C23 C24 C25 C26 -2.0(5) . . . . ? C23 C24 C25 C29 173.5(3) . . . . ? C24 C25 C26 C27 1.4(5) . . . . ? C29 C25 C26 C27 -174.2(3) . . . . ? C25 C26 C27 C28 0.6(5) . . . . ? C25 C26 C27 C30 179.4(3) . . . . ? C26 C27 C28 C23 -2.2(5) . . . . ? C30 C27 C28 C23 179.0(3) . . . . ? C24 C23 C28 C27 1.6(4) . . . . ? B1 C23 C28 C27 174.0(3) . . . . ? C24 C25 C29 F2 -93.0(4) . . . . ? C26 C25 C29 F2 82.6(4) . . . . ? C24 C25 C29 F3 27.0(4) . . . . ? C26 C25 C29 F3 -157.4(3) . . . . ? C24 C25 C29 F1 147.5(3) . . . . ? C26 C25 C29 F1 -36.9(4) . . . . ? C28 C27 C30 F6 58.5(4) . . . . ? C26 C27 C30 F6 -120.3(3) . . . . ? C28 C27 C30 F5 178.6(3) . . . . ? C26 C27 C30 F5 -0.2(5) . . . . ? C28 C27 C30 F4 -60.9(4) . . . . ? C26 C27 C30 F4 120.3(3) . . . . ? C36 C31 C32 C33 0.7(4) . . . . ? B1 C31 C32 C33 -170.3(3) . . . . ? C31 C32 C33 C34 -1.9(5) . . . . ? C31 C32 C33 C37 176.2(3) . . . . ? C32 C33 C34 C35 1.2(5) . . . . ? C37 C33 C34 C35 -176.9(3) . . . . ? C33 C34 C35 C36 0.5(5) . . . . ? C33 C34 C35 C38 -178.9(3) . . . . ? C32 C31 C36 C35 1.1(4) . . . . ? B1 C31 C36 C35 171.8(3) . . . . ? C34 C35 C36 C31 -1.8(5) . . . . ? C38 C35 C36 C31 177.7(3) . . . . ? C32 C33 C37 F8B -20(3) . . . . ? C34 C33 C37 F8B 158(3) . . . . ? C32 C33 C37 F7B 103.9(17) . . . . ? C34 C33 C37 F7B -78.0(17) . . . . ? C32 C33 C37 F9A -124.0(14) . . . . ? C34 C33 C37 F9A 54.2(14) . . . . ? C32 C33 C37 F9B -138.7(15) . . . . ? C34 C33 C37 F9B 39.5(15) . . . . ? C32 C33 C37 F7A 117.6(7) . . . . ? C34 C33 C37 F7A -64.3(8) . . . . ? C32 C33 C37 F8A -1.4(8) . . . . ? C34 C33 C37 F8A 176.8(7) . . . . ? C34 C35 C38 F10B -109(2) . . . . ? C36 C35 C38 F10B 72(2) . . . . ? C34 C35 C38 F12B 133.7(11) . . . . ? C36 C35 C38 F12B -45.8(11) . . . . ? C34 C35 C38 F12A 102.9(11) . . . . ? C36 C35 C38 F12A -76.5(11) . . . . ? C34 C35 C38 F11B 22.5(14) . . . . ? C36 C35 C38 F11B -157.0(14) . . . . ? C34 C35 C38 F11A -24.4(9) . . . . ? C36 C35 C38 F11A 156.1(8) . . . . ? C34 C35 C38 F10A -139.6(6) . . . . ? C36 C35 C38 F10A 40.9(7) . . . . ? C44 C39 C40 C41 -2.0(4) . . . . ? B1 C39 C40 C41 -175.5(3) . . . . ? C39 C40 C41 C42 0.7(5) . . . . ? C39 C40 C41 C45 -179.5(3) . . . . ? C40 C41 C42 C43 0.8(5) . . . . ? C45 C41 C42 C43 -178.9(3) . . . . ? C41 C42 C43 C44 -1.0(5) . . . . ? C41 C42 C43 C46 177.3(3) . . . . ? C42 C43 C44 C39 -0.4(5) . . . . ? C46 C43 C44 C39 -178.7(3) . . . . ? C40 C39 C44 C43 1.9(5) . . . . ? B1 C39 C44 C43 175.1(3) . . . . ? C42 C41 C45 F13 -13.3(5) . . . . ? C40 C41 C45 F13 166.9(3) . . . . ? C42 C41 C45 F14 -134.6(3) . . . . ? C40 C41 C45 F14 45.6(4) . . . . ? C42 C41 C45 F15 107.5(4) . . . . ? C40 C41 C45 F15 -72.3(4) . . . . ? C42 C43 C46 F17 30.3(5) . . . . ? C44 C43 C46 F17 -151.3(3) . . . . ? C42 C43 C46 F16 152.1(3) . . . . ? C44 C43 C46 F16 -29.6(5) . . . . ? C42 C43 C46 F18 -89.2(4) . . . . ? C44 C43 C46 F18 89.2(4) . . . . ? C52 C47 C48 C49 -3.0(4) . . . . ? B1 C47 C48 C49 179.9(3) . . . . ? C47 C48 C49 C50 0.7(5) . . . . ? C47 C48 C49 C53 -179.1(3) . . . . ? C48 C49 C50 C51 1.5(5) . . . . ? C53 C49 C50 C51 -178.7(3) . . . . ? C49 C50 C51 C52 -1.3(5) . . . . ? C49 C50 C51 C54 -179.6(3) . . . . ? C48 C47 C52 C51 3.1(4) . . . . ? B1 C47 C52 C51 -179.8(3) . . . . ? C50 C51 C52 C47 -1.1(5) . . . . ? C54 C51 C52 C47 177.2(3) . . . . ? C50 C49 C53 F21 -151.9(3) . . . . ? C48 C49 C53 F21 27.9(5) . . . . ? C50 C49 C53 F20 -32.2(4) . . . . ? C48 C49 C53 F20 147.7(3) . . . . ? C50 C49 C53 F19 87.4(4) . . . . ? C48 C49 C53 F19 -92.7(4) . . . . ? C50 C51 C54 F24 1.7(5) . . . . ? C52 C51 C54 F24 -176.7(3) . . . . ? C50 C51 C54 F22 -120.6(4) . . . . ? C52 C51 C54 F22 61.1(4) . . . . ? C50 C51 C54 F23 121.8(4) . . . . ? C52 C51 C54 F23 -56.6(4) . . . . ? C24 C23 B1 C47 82.2(3) . . . . ? C28 C23 B1 C47 -89.7(3) . . . . ? C24 C23 B1 C39 -156.4(3) . . . . ? C28 C23 B1 C39 31.7(4) . . . . ? C24 C23 B1 C31 -40.5(4) . . . . ? C28 C23 B1 C31 147.6(3) . . . . ? C52 C47 B1 C23 -86.6(3) . . . . ? C48 C47 B1 C23 90.3(3) . . . . ? C52 C47 B1 C39 150.9(3) . . . . ? C48 C47 B1 C39 -32.2(4) . . . . ? C52 C47 B1 C31 36.1(4) . . . . ? C48 C47 B1 C31 -147.0(3) . . . . ? C40 C39 B1 C23 -154.1(3) . . . . ? C44 C39 B1 C23 33.0(4) . . . . ? C40 C39 B1 C47 -37.0(4) . . . . ? C44 C39 B1 C47 150.1(3) . . . . ? C40 C39 B1 C31 84.0(3) . . . . ? C44 C39 B1 C31 -88.9(3) . . . . ? C36 C31 B1 C23 144.9(3) . . . . ? C32 C31 B1 C23 -44.9(4) . . . . ? C36 C31 B1 C47 27.1(4) . . . . ? C32 C31 B1 C47 -162.7(3) . . . . ? C36 C31 B1 C39 -93.0(3) . . . . ? C32 C31 B1 C39 77.2(3) . . . . ? C58 O3A C57 C56 -17(5) . . . . ? C57 O3A C58 C59 -28(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.110 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.088 ##=== END OF CIF ##=== END OF GLOBAL CIF