#-----------------------------------------------------------------------------80 # Subsequently are contained the CIF's of one structure # 1 = compound (9) # separated by #===END #-----------------------------------------------------------------------------80 data_global _publ_contact_author ; Dr. Enrique O\~nate Rodr\'iguez Departamento de Qu\'imica Inorg\'anica - I.C.M.A. Facultad de Ciencias Universidad de Zaragoza - C.S.I.C. 50009 Zaragoza, Spain ; _publ_contact_author_email enriqueo@posta.unizar.es #-----------------------------------------------------------------------------80 #Publication details loop_ _publ_author_name 'Bola\~no, S.' 'Rodr\'iguez-Rocha, M. Mar' 'Bravo, J.' 'Castro, J.' 'O\~nate, E.' 'Peruzzini, M.' _publ_requested_journal 'Organometallics' _journal_name_full ; Organometallics ; _publ_section_title ; Reactivity of [TpRuCl(PTA)(PPh3)] with Alkynes and Propargylic Alcohols: The Occurrence of Structurally Related Cationic vs Neutral Allenylidene Complexes with the HydridoTris(pyrazolylborate)ruthenium Moiety ; _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year 2009 #-----------------------------------------------------------------------------80 # Data for compound 9 (local labelling mae409as) data_mae409as _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H59 B F6 N12 P4 Ru' _chemical_formula_weight 1225.89 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0938(14) _cell_length_b 14.2160(16) _cell_length_c 17.962(2) _cell_angle_alpha 72.991(2) _cell_angle_beta 70.925(2) _cell_angle_gamma 67.592(2) _cell_volume 2647.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5952 _cell_measurement_theta_min 2 _cell_measurement_theta_max 24 _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.490 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details ; Absorption correction performed with SADABS program. This is based on the method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33. SADABS: Area-Detector Absorption Correction. Bruker-AXS within SAINT+ package, v. 6.1 (2000). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 25159 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 28.85 _reflns_number_total 12370 _reflns_number_gt 9887 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.625 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.1 (Bruker AXS, 2000)' _computing_data_reduction 'SAINT+ v. 6.1 (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.1 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.1 (Bruker, 2000)' _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^)+(0.0520P)^2^+0.5908P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12370 _refine_ls_number_parameters 706 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 Ru Ru 0.70268(2) 0.852567(19) 0.742035(13) 0.01307(7) Uani 1 1 d . . . P1 P 0.59501(7) 0.78002(6) 0.86496(4) 0.01699(16) Uani 1 1 d . . . P2 P 0.87249(7) 0.84010(6) 0.78345(4) 0.01521(16) Uani 1 1 d . . . P3 P 0.76966(7) 0.69315(6) 0.60883(4) 0.01503(16) Uani 1 1 d . . . P4 P 0.83600(8) 0.22647(7) 0.64980(5) 0.02526(19) Uani 1 1 d . . . F1 F 0.8294(2) 0.11518(16) 0.65363(12) 0.0358(5) Uani 1 1 d . . . F2 F 0.89250(19) 0.23821(18) 0.55430(11) 0.0379(5) Uani 1 1 d . . . F3 F 0.70102(19) 0.28055(18) 0.63591(13) 0.0440(6) Uani 1 1 d . . . F4 F 0.8464(2) 0.33694(16) 0.64605(14) 0.0443(6) Uani 1 1 d . . . F5 F 0.7827(2) 0.21379(17) 0.74495(11) 0.0376(5) Uani 1 1 d . . . F6 F 0.97388(18) 0.17270(16) 0.66220(12) 0.0346(5) Uani 1 1 d . . . N1 N 0.6109(2) 1.0065(2) 0.76729(14) 0.0185(5) Uani 1 1 d . . . N2 N 0.5620(2) 1.0826(2) 0.70917(15) 0.0190(5) Uani 1 1 d . . . N3 N 0.7779(2) 0.92428(19) 0.62258(14) 0.0149(5) Uani 1 1 d . . . N4 N 0.7038(2) 1.01377(19) 0.58669(14) 0.0165(5) Uani 1 1 d . . . N5 N 0.5478(2) 0.88165(19) 0.69629(14) 0.0156(5) Uani 1 1 d . . . N6 N 0.5057(2) 0.97597(19) 0.64982(14) 0.0171(5) Uani 1 1 d . . . N7 N 1.0659(2) 0.7351(2) 0.86079(15) 0.0204(6) Uani 1 1 d . . . N8 N 1.1128(2) 0.8514(2) 0.73121(14) 0.0176(5) Uani 1 1 d . . . N9 N 0.9819(2) 0.9252(2) 0.85111(14) 0.0191(5) Uani 1 1 d . . . N10 N 0.6858(2) 0.76088(19) 0.47413(15) 0.0180(5) Uani 1 1 d . . . N11 N 0.6661(2) 0.5938(2) 0.55693(15) 0.0199(5) Uani 1 1 d . . . N12 N 0.8698(2) 0.6073(2) 0.47455(15) 0.0196(5) Uani 1 1 d . . . B B 0.5694(3) 1.0592(3) 0.6297(2) 0.0183(7) Uani 1 1 d . . . H1 H 0.523(3) 1.128(3) 0.5925(19) 0.022 Uiso 1 1 d . . . C1 C 0.8019(3) 0.7151(2) 0.69293(16) 0.0163(6) Uani 1 1 d . . . C2 C 0.9011(3) 0.6375(2) 0.70631(16) 0.0166(6) Uani 1 1 d . . . C3 C 0.9968(3) 0.5569(2) 0.72163(17) 0.0177(6) Uani 1 1 d . . . C4 C 0.9739(3) 0.4623(2) 0.78097(18) 0.0204(6) Uani 1 1 d . . . C5 C 0.9792(3) 0.3782(3) 0.75454(19) 0.0264(7) Uani 1 1 d . . . H5 H 0.9969 0.3804 0.6997 0.032 Uiso 1 1 calc R . . C6 C 0.9585(4) 0.2906(3) 0.8084(2) 0.0329(8) Uani 1 1 d . . . H6 H 0.9635 0.2343 0.7898 0.039 Uiso 1 1 calc R . . C7 C 0.9305(3) 0.2873(3) 0.8899(2) 0.0286(8) Uani 1 1 d . . . H7 H 0.9166 0.2287 0.9262 0.034 Uiso 1 1 calc R . . C8 C 0.9231(3) 0.3706(3) 0.91744(19) 0.0256(7) Uani 1 1 d . . . H8 H 0.9030 0.3687 0.9723 0.031 Uiso 1 1 calc R . . C9 C 0.9458(3) 0.4578(3) 0.86332(18) 0.0235(7) Uani 1 1 d . . . H9 H 0.9422 0.5135 0.8823 0.028 Uiso 1 1 calc R . . C10 C 1.1274(3) 0.5552(2) 0.68373(18) 0.0193(6) Uani 1 1 d . . . C11 C 1.1575(3) 0.6267(2) 0.61493(17) 0.0189(6) Uani 1 1 d . . . H11 H 1.0951 0.6758 0.5917 0.023 Uiso 1 1 calc R . . C12 C 1.2780(3) 0.6260(3) 0.58051(19) 0.0222(7) Uani 1 1 d . . . H12 H 1.2957 0.6747 0.5348 0.027 Uiso 1 1 calc R . . C13 C 1.3724(3) 0.5533(3) 0.6138(2) 0.0273(7) Uani 1 1 d . . . H13 H 1.4535 0.5530 0.5910 0.033 Uiso 1 1 calc R . . C14 C 1.3446(3) 0.4809(3) 0.6815(2) 0.0306(8) Uani 1 1 d . . . H14 H 1.4073 0.4318 0.7044 0.037 Uiso 1 1 calc R . . C15 C 1.2233(3) 0.4809(3) 0.7155(2) 0.0272(7) Uani 1 1 d . . . H15 H 1.2062 0.4306 0.7601 0.033 Uiso 1 1 calc R . . C16 C 0.5852(3) 1.0540(3) 0.82828(18) 0.0218(7) Uani 1 1 d . . . H16 H 0.6066 1.0206 0.8769 0.026 Uiso 1 1 calc R . . C17 C 0.5235(3) 1.1583(3) 0.8100(2) 0.0274(7) Uani 1 1 d . . . H17 H 0.4967 1.2075 0.8420 0.033 Uiso 1 1 calc R . . C18 C 0.5103(3) 1.1735(3) 0.7336(2) 0.0240(7) Uani 1 1 d . . . H18 H 0.4718 1.2364 0.7040 0.029 Uiso 1 1 calc R . . C19 C 0.8832(3) 0.8986(2) 0.56635(17) 0.0165(6) Uani 1 1 d . . . H19 H 0.9507 0.8404 0.5743 0.020 Uiso 1 1 calc R . . C20 C 0.8786(3) 0.9700(3) 0.49464(17) 0.0206(7) Uani 1 1 d . . . H20 H 0.9395 0.9690 0.4469 0.025 Uiso 1 1 calc R . . C21 C 0.7636(3) 1.0425(2) 0.51013(17) 0.0193(6) Uani 1 1 d . . . H21 H 0.7323 1.1013 0.4740 0.023 Uiso 1 1 calc R . . C22 C 0.4703(3) 0.8307(2) 0.70458(16) 0.0162(6) Uani 1 1 d . . . H22 H 0.4767 0.7638 0.7339 0.019 Uiso 1 1 calc R . . C23 C 0.3789(3) 0.8906(2) 0.66383(17) 0.0196(6) Uani 1 1 d . . . H23 H 0.3146 0.8728 0.6603 0.023 Uiso 1 1 calc R . . C24 C 0.4050(3) 0.9826(2) 0.62965(18) 0.0190(6) Uani 1 1 d . . . H24 H 0.3605 1.0395 0.5981 0.023 Uiso 1 1 calc R . . C25 C 0.9575(3) 0.7239(2) 0.84730(17) 0.0186(6) Uani 1 1 d . . . H25A H 0.9014 0.7101 0.8989 0.022 Uiso 1 1 calc R . . H25B H 0.9847 0.6645 0.8221 0.022 Uiso 1 1 calc R . . C26 C 1.0103(3) 0.8553(2) 0.70248(16) 0.0163(6) Uani 1 1 d . . . H26A H 1.0390 0.8008 0.6719 0.020 Uiso 1 1 calc R . . H26B H 0.9863 0.9211 0.6664 0.020 Uiso 1 1 calc R . . C27 C 0.8636(3) 0.9387(2) 0.83610(17) 0.0189(6) Uani 1 1 d . . . H27A H 0.8356 1.0071 0.8041 0.023 Uiso 1 1 calc R . . H27B H 0.8029 0.9351 0.8870 0.023 Uiso 1 1 calc R . . C28 C 1.1557(3) 0.7525(2) 0.78432(18) 0.0204(6) Uani 1 1 d . . . H28A H 1.2303 0.7492 0.7956 0.024 Uiso 1 1 calc R . . H28B H 1.1767 0.6967 0.7564 0.024 Uiso 1 1 calc R . . C29 C 1.0755(3) 0.9353(2) 0.77543(17) 0.0193(6) Uani 1 1 d . . . H29A H 1.1478 0.9366 0.7869 0.023 Uiso 1 1 calc R . . H29B H 1.0435 1.0010 0.7414 0.023 Uiso 1 1 calc R . . C30 C 1.0290(3) 0.8229(3) 0.90033(17) 0.0228(7) Uani 1 1 d . . . H30A H 1.0995 0.8215 0.9157 0.027 Uiso 1 1 calc R . . H30B H 0.9656 0.8140 0.9491 0.027 Uiso 1 1 calc R . . C31 C 0.6969(3) 0.8019(2) 0.53684(17) 0.0166(6) Uani 1 1 d . . . H31A H 0.6159 0.8410 0.5642 0.020 Uiso 1 1 calc R . . H31B H 0.7466 0.8480 0.5127 0.020 Uiso 1 1 calc R . . C32 C 0.6768(3) 0.6071(2) 0.63231(18) 0.0188(6) Uani 1 1 d . . . H32A H 0.7157 0.5403 0.6624 0.023 Uiso 1 1 calc R . . H32B H 0.5955 0.6368 0.6649 0.023 Uiso 1 1 calc R . . C33 C 0.9064(3) 0.6250(2) 0.53871(17) 0.0196(6) Uani 1 1 d . . . H33A H 0.9621 0.6660 0.5152 0.023 Uiso 1 1 calc R . . H33B H 0.9496 0.5590 0.5676 0.023 Uiso 1 1 calc R . . C34 C 0.6089(3) 0.6927(2) 0.50875(18) 0.0200(6) Uani 1 1 d . . . H34A H 0.5319 0.7287 0.5422 0.024 Uiso 1 1 calc R . . H34B H 0.5895 0.6788 0.4655 0.024 Uiso 1 1 calc R . . C35 C 0.8062(3) 0.7050(2) 0.42809(17) 0.0198(6) Uani 1 1 d . . . H35A H 0.7947 0.6905 0.3821 0.024 Uiso 1 1 calc R . . H35B H 0.8580 0.7493 0.4081 0.024 Uiso 1 1 calc R . . C36 C 0.7874(3) 0.5431(2) 0.50799(19) 0.0220(7) Uani 1 1 d . . . H36A H 0.8275 0.4794 0.5408 0.026 Uiso 1 1 calc R . . H36B H 0.7752 0.5245 0.4641 0.026 Uiso 1 1 calc R . . C37 C 0.5525(3) 0.6672(2) 0.86724(17) 0.0186(6) Uani 1 1 d . . . C38 C 0.6447(3) 0.5803(2) 0.84120(18) 0.0216(7) Uani 1 1 d . . . H38 H 0.7259 0.5807 0.8232 0.026 Uiso 1 1 calc R . . C39 C 0.6193(3) 0.4929(3) 0.8412(2) 0.0275(7) Uani 1 1 d . . . H39 H 0.6827 0.4352 0.8246 0.033 Uiso 1 1 calc R . . C40 C 0.4984(3) 0.4928(3) 0.8662(2) 0.0294(8) Uani 1 1 d . . . H40 H 0.4799 0.4352 0.8660 0.035 Uiso 1 1 calc R . . C41 C 0.4051(3) 0.5787(3) 0.8916(2) 0.0288(8) Uani 1 1 d . . . H41 H 0.3238 0.5784 0.9083 0.035 Uiso 1 1 calc R . . C42 C 0.4309(3) 0.6653(3) 0.89254(19) 0.0236(7) Uani 1 1 d . . . H42 H 0.3672 0.7223 0.9101 0.028 Uiso 1 1 calc R . . C43 C 0.4414(3) 0.8632(3) 0.91114(18) 0.0207(7) Uani 1 1 d . . . C44 C 0.3685(3) 0.9440(3) 0.86512(18) 0.0220(7) Uani 1 1 d . . . H44 H 0.4014 0.9635 0.8106 0.026 Uiso 1 1 calc R . . C45 C 0.2470(3) 0.9961(3) 0.8995(2) 0.0267(7) Uani 1 1 d . . . H45 H 0.1989 1.0494 0.8677 0.032 Uiso 1 1 calc R . . C46 C 0.1973(3) 0.9690(3) 0.9810(2) 0.0323(8) Uani 1 1 d . . . H46 H 0.1161 1.0039 1.0040 0.039 Uiso 1 1 calc R . . C47 C 0.2689(3) 0.8899(3) 1.0278(2) 0.0312(8) Uani 1 1 d . . . H47 H 0.2364 0.8720 1.0826 0.037 Uiso 1 1 calc R . . C48 C 0.3889(3) 0.8373(3) 0.99334(19) 0.0259(7) Uani 1 1 d . . . H48 H 0.4360 0.7835 1.0253 0.031 Uiso 1 1 calc R . . C49 C 0.6641(3) 0.7341(3) 0.95134(17) 0.0228(7) Uani 1 1 d . . . C50 C 0.7167(3) 0.6303(3) 0.98272(19) 0.0272(8) Uani 1 1 d . . . H50 H 0.7116 0.5788 0.9629 0.033 Uiso 1 1 calc R . . C51 C 0.7774(3) 0.6029(3) 1.0442(2) 0.0360(9) Uani 1 1 d . . . H51 H 0.8135 0.5335 1.0646 0.043 Uiso 1 1 calc R . . C52 C 0.7834(3) 0.6793(4) 1.07420(19) 0.0368(10) Uani 1 1 d . . . H52 H 0.8251 0.6610 1.1142 0.044 Uiso 1 1 calc R . . C53 C 0.7286(3) 0.7816(3) 1.04557(19) 0.0334(9) Uani 1 1 d . . . H53 H 0.7315 0.8326 1.0669 0.040 Uiso 1 1 calc R . . C54 C 0.6690(3) 0.8092(3) 0.98490(17) 0.0265(8) Uani 1 1 d . . . H54 H 0.6314 0.8789 0.9661 0.032 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 Ru 0.01028(11) 0.01809(13) 0.01129(11) 0.00072(9) -0.00240(8) -0.00777(9) P1 0.0138(4) 0.0241(4) 0.0139(3) 0.0005(3) -0.0028(3) -0.0104(3) P2 0.0130(4) 0.0204(4) 0.0132(3) 0.0007(3) -0.0034(3) -0.0091(3) P3 0.0132(4) 0.0157(4) 0.0158(3) 0.0005(3) -0.0041(3) -0.0063(3) P4 0.0263(5) 0.0274(5) 0.0218(4) 0.0040(4) -0.0056(3) -0.0150(4) F1 0.0476(13) 0.0336(12) 0.0359(11) 0.0007(10) -0.0141(10) -0.0253(10) F2 0.0386(12) 0.0526(14) 0.0209(10) 0.0056(10) -0.0048(9) -0.0240(11) F3 0.0283(12) 0.0523(15) 0.0417(12) 0.0056(11) -0.0113(10) -0.0108(11) F4 0.0600(16) 0.0261(12) 0.0502(14) 0.0053(10) -0.0209(12) -0.0204(11) F5 0.0426(13) 0.0467(14) 0.0226(10) -0.0035(10) -0.0014(9) -0.0212(11) F6 0.0289(11) 0.0400(13) 0.0358(11) 0.0039(10) -0.0117(9) -0.0168(10) N1 0.0157(13) 0.0245(14) 0.0182(12) -0.0018(11) -0.0037(10) -0.0113(11) N2 0.0171(13) 0.0185(13) 0.0212(13) -0.0018(11) -0.0052(10) -0.0063(11) N3 0.0147(12) 0.0172(13) 0.0145(11) 0.0010(10) -0.0054(9) -0.0083(10) N4 0.0191(13) 0.0166(13) 0.0148(11) 0.0018(10) -0.0070(10) -0.0081(11) N5 0.0141(12) 0.0178(13) 0.0155(11) 0.0006(10) -0.0049(10) -0.0073(10) N6 0.0138(12) 0.0180(13) 0.0178(12) -0.0012(10) -0.0056(10) -0.0035(10) N7 0.0172(13) 0.0287(15) 0.0178(12) 0.0013(11) -0.0064(10) -0.0124(12) N8 0.0131(12) 0.0247(14) 0.0167(12) -0.0013(11) -0.0035(10) -0.0099(11) N9 0.0156(13) 0.0281(15) 0.0157(12) -0.0007(11) -0.0054(10) -0.0106(11) N10 0.0188(13) 0.0178(13) 0.0204(12) -0.0022(11) -0.0065(10) -0.0087(11) N11 0.0193(13) 0.0183(13) 0.0235(13) -0.0028(11) -0.0055(11) -0.0082(11) N12 0.0175(13) 0.0212(14) 0.0193(12) -0.0028(11) -0.0040(10) -0.0063(11) B 0.0156(16) 0.0188(17) 0.0201(16) 0.0013(14) -0.0055(13) -0.0077(14) C1 0.0154(14) 0.0218(16) 0.0141(13) 0.0044(12) -0.0050(11) -0.0130(12) C2 0.0178(15) 0.0218(16) 0.0120(13) 0.0006(12) -0.0029(11) -0.0117(13) C3 0.0163(15) 0.0237(16) 0.0143(13) 0.0016(12) -0.0054(11) -0.0103(13) C4 0.0102(14) 0.0222(16) 0.0237(15) 0.0027(13) -0.0053(12) -0.0039(12) C5 0.0301(18) 0.0276(18) 0.0220(15) -0.0001(14) -0.0066(14) -0.0131(15) C6 0.042(2) 0.0284(19) 0.0346(19) 0.0013(16) -0.0132(17) -0.0203(17) C7 0.0299(19) 0.0296(19) 0.0264(17) 0.0124(15) -0.0120(14) -0.0186(16) C8 0.0244(17) 0.0290(19) 0.0196(15) 0.0039(14) -0.0045(13) -0.0113(15) C9 0.0215(16) 0.0226(17) 0.0216(15) -0.0010(13) -0.0037(13) -0.0055(13) C10 0.0161(15) 0.0211(16) 0.0217(15) -0.0008(13) -0.0059(12) -0.0084(13) C11 0.0188(15) 0.0189(16) 0.0184(14) -0.0018(12) -0.0061(12) -0.0055(13) C12 0.0213(16) 0.0243(17) 0.0232(15) -0.0049(13) -0.0003(13) -0.0135(14) C13 0.0158(16) 0.0300(19) 0.0355(18) -0.0055(15) -0.0027(14) -0.0102(14) C14 0.0173(16) 0.0291(19) 0.0388(19) 0.0047(16) -0.0126(15) -0.0038(14) C15 0.0218(17) 0.0274(18) 0.0273(17) 0.0049(14) -0.0071(14) -0.0089(14) C16 0.0184(15) 0.0303(18) 0.0205(15) -0.0075(14) -0.0012(12) -0.0128(14) C17 0.0262(18) 0.0310(19) 0.0275(17) -0.0114(15) -0.0003(14) -0.0126(15) C18 0.0219(16) 0.0186(16) 0.0308(17) -0.0045(14) -0.0066(14) -0.0058(13) C19 0.0139(14) 0.0203(15) 0.0182(14) -0.0019(12) -0.0059(11) -0.0083(12) C20 0.0241(16) 0.0284(17) 0.0141(13) -0.0010(13) -0.0039(12) -0.0163(14) C21 0.0237(16) 0.0196(16) 0.0176(14) 0.0049(12) -0.0088(12) -0.0131(13) C22 0.0139(14) 0.0193(15) 0.0148(13) -0.0012(12) -0.0018(11) -0.0075(12) C23 0.0141(14) 0.0262(17) 0.0185(14) -0.0038(13) -0.0038(12) -0.0070(13) C24 0.0128(14) 0.0233(16) 0.0202(14) -0.0023(13) -0.0075(12) -0.0034(12) C25 0.0161(15) 0.0246(16) 0.0158(13) 0.0026(12) -0.0068(11) -0.0097(13) C26 0.0153(14) 0.0209(16) 0.0141(13) 0.0005(12) -0.0031(11) -0.0105(12) C27 0.0153(15) 0.0265(17) 0.0166(14) -0.0019(13) -0.0035(11) -0.0103(13) C28 0.0132(14) 0.0266(17) 0.0230(15) -0.0033(13) -0.0060(12) -0.0078(13) C29 0.0169(15) 0.0271(17) 0.0173(14) -0.0022(13) -0.0027(12) -0.0134(13) C30 0.0208(16) 0.0358(19) 0.0147(14) -0.0001(13) -0.0061(12) -0.0139(14) C31 0.0185(15) 0.0177(15) 0.0158(13) -0.0008(12) -0.0063(11) -0.0082(12) C32 0.0171(15) 0.0173(15) 0.0218(15) -0.0014(12) -0.0025(12) -0.0088(12) C33 0.0152(15) 0.0223(16) 0.0200(14) -0.0035(13) -0.0047(12) -0.0046(13) C34 0.0197(16) 0.0222(16) 0.0215(15) -0.0020(13) -0.0071(12) -0.0100(13) C35 0.0234(16) 0.0217(16) 0.0169(14) -0.0015(13) -0.0064(12) -0.0104(13) C36 0.0246(17) 0.0192(16) 0.0237(15) -0.0044(13) -0.0064(13) -0.0079(13) C37 0.0168(15) 0.0228(16) 0.0145(13) 0.0053(12) -0.0037(11) -0.0111(13) C38 0.0193(16) 0.0226(17) 0.0201(15) 0.0073(13) -0.0057(12) -0.0115(13) C39 0.0261(18) 0.0213(17) 0.0286(17) 0.0023(14) -0.0021(14) -0.0098(14) C40 0.0279(19) 0.0248(18) 0.0366(19) 0.0017(15) -0.0075(15) -0.0155(15) C41 0.0220(17) 0.0289(19) 0.0360(19) 0.0036(15) -0.0066(15) -0.0162(15) C42 0.0183(16) 0.0259(18) 0.0258(16) 0.0016(14) -0.0061(13) -0.0105(14) C43 0.0159(15) 0.0293(18) 0.0206(15) -0.0076(13) -0.0005(12) -0.0124(13) C44 0.0191(16) 0.0287(18) 0.0213(15) -0.0093(14) 0.0005(12) -0.0123(14) C45 0.0194(16) 0.0271(18) 0.0360(18) -0.0105(15) -0.0038(14) -0.0092(14) C46 0.0203(17) 0.040(2) 0.039(2) -0.0226(18) 0.0058(15) -0.0126(16) C47 0.0300(19) 0.043(2) 0.0248(17) -0.0134(16) 0.0087(14) -0.0246(17) C48 0.0268(18) 0.036(2) 0.0203(15) -0.0056(14) -0.0027(13) -0.0178(15) C49 0.0174(15) 0.038(2) 0.0154(14) 0.0034(14) -0.0031(12) -0.0182(14) C50 0.0234(17) 0.040(2) 0.0200(15) 0.0051(15) -0.0047(13) -0.0200(16) C51 0.0289(19) 0.052(3) 0.0225(17) 0.0166(17) -0.0083(15) -0.0237(18) C52 0.0275(19) 0.072(3) 0.0169(15) 0.0053(18) -0.0052(14) -0.032(2) C53 0.0304(19) 0.061(3) 0.0171(15) -0.0027(17) -0.0012(14) -0.0303(19) C54 0.0213(17) 0.044(2) 0.0139(14) 0.0004(14) 0.0005(12) -0.0182(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 Ru C1 2.137(3) . ? Ru N5 2.138(2) . ? Ru N3 2.150(2) . ? Ru N1 2.151(3) . ? Ru P2 2.3337(8) . ? Ru P1 2.3338(8) . ? P1 C49 1.836(3) . ? P1 C37 1.848(3) . ? P1 C43 1.852(3) . ? P2 C26 1.856(3) . ? P2 C27 1.861(3) . ? P2 C25 1.862(3) . ? P3 C1 1.812(3) . ? P3 C32 1.836(3) . ? P3 C31 1.836(3) . ? P3 C33 1.841(3) . ? P4 F3 1.586(2) . ? P4 F1 1.595(2) . ? P4 F5 1.599(2) . ? P4 F4 1.603(2) . ? P4 F6 1.608(2) . ? P4 F2 1.610(2) . ? N1 C16 1.343(4) . ? N1 N2 1.365(3) . ? N2 C18 1.337(4) . ? N2 B 1.526(4) . ? N3 C19 1.340(4) . ? N3 N4 1.366(3) . ? N4 C21 1.352(4) . ? N4 B 1.526(4) . ? N5 C22 1.338(4) . ? N5 N6 1.363(3) . ? N6 C24 1.343(4) . ? N6 B 1.545(4) . ? N7 C30 1.465(4) . ? N7 C28 1.469(4) . ? N7 C25 1.481(4) . ? N8 C28 1.463(4) . ? N8 C26 1.468(4) . ? N8 C29 1.471(4) . ? N9 C29 1.468(4) . ? N9 C27 1.472(4) . ? N9 C30 1.473(4) . ? N10 C34 1.466(4) . ? N10 C35 1.466(4) . ? N10 C31 1.473(4) . ? N11 C34 1.464(4) . ? N11 C36 1.472(4) . ? N11 C32 1.473(4) . ? N12 C35 1.464(4) . ? N12 C36 1.472(4) . ? N12 C33 1.475(4) . ? B H1 1.08(3) . ? C1 C2 1.318(4) . ? C2 C3 1.320(4) . ? C3 C10 1.496(4) . ? C3 C4 1.508(4) . ? C4 C5 1.382(5) . ? C4 C9 1.393(4) . ? C5 C6 1.388(5) . ? C5 H5 0.9300 . ? C6 C7 1.380(5) . ? C6 H6 0.9300 . ? C7 C8 1.375(5) . ? C7 H7 0.9300 . ? C8 C9 1.392(4) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C15 1.390(4) . ? C10 C11 1.395(4) . ? C11 C12 1.382(4) . ? C11 H11 0.9300 . ? C12 C13 1.384(5) . ? C12 H12 0.9300 . ? C13 C14 1.384(5) . ? C13 H13 0.9300 . ? C14 C15 1.393(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.377(5) . ? C16 H16 0.9300 . ? C17 C18 1.377(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.390(4) . ? C19 H19 0.9300 . ? C20 C21 1.377(4) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.388(4) . ? C22 H22 0.9300 . ? C23 C24 1.380(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.391(4) . ? C37 C42 1.398(4) . ? C38 C39 1.389(5) . ? C38 H38 0.9300 . ? C39 C40 1.382(4) . ? C39 H39 0.9300 . ? C40 C41 1.383(5) . ? C40 H40 0.9300 . ? C41 C42 1.386(5) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.389(4) . ? C43 C48 1.402(4) . ? C44 C45 1.390(4) . ? C44 H44 0.9300 . ? C45 C46 1.388(5) . ? C45 H45 0.9300 . ? C46 C47 1.379(5) . ? C46 H46 0.9300 . ? C47 C48 1.380(5) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.391(5) . ? C49 C54 1.397(5) . ? C50 C51 1.403(5) . ? C50 H50 0.9300 . ? C51 C52 1.380(6) . ? C51 H51 0.9300 . ? C52 C53 1.367(6) . ? C52 H52 0.9300 . ? C53 C54 1.382(5) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru N5 92.09(10) . . ? C1 Ru N3 81.99(10) . . ? N5 Ru N3 84.24(9) . . ? C1 Ru N1 168.70(10) . . ? N5 Ru N1 84.71(9) . . ? N3 Ru N1 86.90(9) . . ? C1 Ru P2 91.56(8) . . ? N5 Ru P2 173.27(7) . . ? N3 Ru P2 90.67(7) . . ? N1 Ru P2 90.64(7) . . ? C1 Ru P1 98.66(8) . . ? N5 Ru P1 87.21(7) . . ? N3 Ru P1 171.45(7) . . ? N1 Ru P1 92.02(7) . . ? P2 Ru P1 97.83(3) . . ? C49 P1 C37 101.72(14) . . ? C49 P1 C43 99.06(14) . . ? C37 P1 C43 99.11(14) . . ? C49 P1 Ru 118.71(10) . . ? C37 P1 Ru 117.27(10) . . ? C43 P1 Ru 117.49(11) . . ? C26 P2 C27 95.65(13) . . ? C26 P2 C25 96.06(13) . . ? C27 P2 C25 97.17(14) . . ? C26 P2 Ru 116.16(9) . . ? C27 P2 Ru 120.50(10) . . ? C25 P2 Ru 125.04(10) . . ? C1 P3 C32 116.80(13) . . ? C1 P3 C31 121.20(14) . . ? C32 P3 C31 101.87(14) . . ? C1 P3 C33 114.68(14) . . ? C32 P3 C33 99.15(14) . . ? C31 P3 C33 99.60(14) . . ? F3 P4 F1 90.94(13) . . ? F3 P4 F5 91.15(12) . . ? F1 P4 F5 90.11(12) . . ? F3 P4 F4 90.58(13) . . ? F1 P4 F4 178.47(13) . . ? F5 P4 F4 90.02(12) . . ? F3 P4 F6 178.92(13) . . ? F1 P4 F6 89.50(12) . . ? F5 P4 F6 89.84(12) . . ? F4 P4 F6 88.98(12) . . ? F3 P4 F2 90.04(12) . . ? F1 P4 F2 89.92(12) . . ? F5 P4 F2 178.82(13) . . ? F4 P4 F2 89.92(13) . . ? F6 P4 F2 88.98(11) . . ? C16 N1 N2 105.0(3) . . ? C16 N1 Ru 137.3(2) . . ? N2 N1 Ru 117.72(18) . . ? C18 N2 N1 110.3(3) . . ? C18 N2 B 128.4(3) . . ? N1 N2 B 121.4(3) . . ? C19 N3 N4 105.6(2) . . ? C19 N3 Ru 135.5(2) . . ? N4 N3 Ru 118.58(17) . . ? C21 N4 N3 110.0(2) . . ? C21 N4 B 129.2(3) . . ? N3 N4 B 120.4(2) . . ? C22 N5 N6 105.6(2) . . ? C22 N5 Ru 136.0(2) . . ? N6 N5 Ru 118.30(18) . . ? C24 N6 N5 110.3(2) . . ? C24 N6 B 128.8(3) . . ? N5 N6 B 120.9(2) . . ? C30 N7 C28 108.3(2) . . ? C30 N7 C25 110.8(2) . . ? C28 N7 C25 110.7(2) . . ? C28 N8 C26 111.4(2) . . ? C28 N8 C29 108.3(2) . . ? C26 N8 C29 110.9(2) . . ? C29 N9 C27 110.9(2) . . ? C29 N9 C30 108.1(2) . . ? C27 N9 C30 111.5(2) . . ? C34 N10 C35 109.4(2) . . ? C34 N10 C31 111.0(2) . . ? C35 N10 C31 112.3(2) . . ? C34 N11 C36 108.6(2) . . ? C34 N11 C32 112.0(2) . . ? C36 N11 C32 111.3(2) . . ? C35 N12 C36 108.2(2) . . ? C35 N12 C33 111.6(2) . . ? C36 N12 C33 111.0(2) . . ? N2 B N4 110.0(2) . . ? N2 B N6 107.2(2) . . ? N4 B N6 107.9(3) . . ? N2 B H1 110.5(17) . . ? N4 B H1 111.2(17) . . ? N6 B H1 109.9(18) . . ? C2 C1 P3 105.2(2) . . ? C2 C1 Ru 131.9(2) . . ? P3 C1 Ru 122.56(16) . . ? C1 C2 C3 177.1(3) . . ? C2 C3 C10 123.1(3) . . ? C2 C3 C4 118.6(3) . . ? C10 C3 C4 118.2(3) . . ? C5 C4 C9 118.5(3) . . ? C5 C4 C3 120.5(3) . . ? C9 C4 C3 121.0(3) . . ? C4 C5 C6 121.1(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 119.8(3) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C8 C7 C6 120.0(3) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.1(3) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C4 120.4(3) . . ? C8 C9 H9 119.8 . . ? C4 C9 H9 119.8 . . ? C15 C10 C11 117.8(3) . . ? C15 C10 C3 120.8(3) . . ? C11 C10 C3 121.4(3) . . ? C12 C11 C10 121.5(3) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 119.1(3) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 120.5(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C10 C15 C14 120.8(3) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? N1 C16 C17 111.6(3) . . ? N1 C16 H16 124.2 . . ? C17 C16 H16 124.2 . . ? C16 C17 C18 104.4(3) . . ? C16 C17 H17 127.8 . . ? C18 C17 H17 127.8 . . ? N2 C18 C17 108.6(3) . . ? N2 C18 H18 125.7 . . ? C17 C18 H18 125.7 . . ? N3 C19 C20 111.4(3) . . ? N3 C19 H19 124.3 . . ? C20 C19 H19 124.3 . . ? C21 C20 C19 104.5(3) . . ? C21 C20 H20 127.7 . . ? C19 C20 H20 127.7 . . ? N4 C21 C20 108.5(3) . . ? N4 C21 H21 125.8 . . ? C20 C21 H21 125.8 . . ? N5 C22 C23 111.2(3) . . ? N5 C22 H22 124.4 . . ? C23 C22 H22 124.4 . . ? C24 C23 C22 104.5(3) . . ? C24 C23 H23 127.7 . . ? C22 C23 H23 127.7 . . ? N6 C24 C23 108.3(3) . . ? N6 C24 H24 125.8 . . ? C23 C24 H24 125.8 . . ? N7 C25 P2 113.7(2) . . ? N7 C25 H25A 108.8 . . ? P2 C25 H25A 108.8 . . ? N7 C25 H25B 108.8 . . ? P2 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? N8 C26 P2 114.22(19) . . ? N8 C26 H26A 108.7 . . ? P2 C26 H26A 108.7 . . ? N8 C26 H26B 108.7 . . ? P2 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? N9 C27 P2 113.6(2) . . ? N9 C27 H27A 108.9 . . ? P2 C27 H27A 108.9 . . ? N9 C27 H27B 108.9 . . ? P2 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? N8 C28 N7 114.4(2) . . ? N8 C28 H28A 108.7 . . ? N7 C28 H28A 108.7 . . ? N8 C28 H28B 108.7 . . ? N7 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? N9 C29 N8 114.0(2) . . ? N9 C29 H29A 108.8 . . ? N8 C29 H29A 108.8 . . ? N9 C29 H29B 108.8 . . ? N8 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? N7 C30 N9 114.7(2) . . ? N7 C30 H30A 108.6 . . ? N9 C30 H30A 108.6 . . ? N7 C30 H30B 108.6 . . ? N9 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? N10 C31 P3 109.0(2) . . ? N10 C31 H31A 109.9 . . ? P3 C31 H31A 109.9 . . ? N10 C31 H31B 109.9 . . ? P3 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? N11 C32 P3 109.16(19) . . ? N11 C32 H32A 109.8 . . ? P3 C32 H32A 109.8 . . ? N11 C32 H32B 109.8 . . ? P3 C32 H32B 109.8 . . ? H32A C32 H32B 108.3 . . ? N12 C33 P3 110.4(2) . . ? N12 C33 H33A 109.6 . . ? P3 C33 H33A 109.6 . . ? N12 C33 H33B 109.6 . . ? P3 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? N11 C34 N10 114.1(2) . . ? N11 C34 H34A 108.7 . . ? N10 C34 H34A 108.7 . . ? N11 C34 H34B 108.7 . . ? N10 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? N12 C35 N10 113.7(2) . . ? N12 C35 H35A 108.8 . . ? N10 C35 H35A 108.8 . . ? N12 C35 H35B 108.8 . . ? N10 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N12 C36 N11 114.2(3) . . ? N12 C36 H36A 108.7 . . ? N11 C36 H36A 108.7 . . ? N12 C36 H36B 108.7 . . ? N11 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C38 C37 C42 117.8(3) . . ? C38 C37 P1 119.0(2) . . ? C42 C37 P1 123.2(2) . . ? C39 C38 C37 122.1(3) . . ? C39 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? C40 C39 C38 119.1(3) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 119.9(3) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C40 C41 C42 120.8(3) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C41 C42 C37 120.3(3) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? C44 C43 C48 117.7(3) . . ? C44 C43 P1 121.8(2) . . ? C48 C43 P1 120.0(3) . . ? C43 C44 C45 120.9(3) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C46 C45 C44 120.2(3) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C47 C46 C45 119.7(3) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C46 C47 C48 120.0(3) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C43 121.5(3) . . ? C47 C48 H48 119.3 . . ? C43 C48 H48 119.3 . . ? C50 C49 C54 118.3(3) . . ? C50 C49 P1 124.3(3) . . ? C54 C49 P1 117.3(3) . . ? C49 C50 C51 120.1(3) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C52 C51 C50 119.9(4) . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C53 C52 C51 120.4(3) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C52 C53 C54 120.0(4) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C53 C54 C49 121.2(4) . . ? C53 C54 H54 119.4 . . ? C49 C54 H54 119.4 . . ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.095 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.096 #===END data_pat # Data for compound 2 _audit_creation_method SHELXL-97 _chemical_name_systematic _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H42 B N9 P2 Ru' _chemical_formula_weight 834.66 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.180(2) _cell_length_b 10.678(2) _cell_length_c 19.582(4) _cell_angle_alpha 81.850(5) _cell_angle_beta 79.352(4) _cell_angle_gamma 67.111(4) _cell_volume 1921.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1353 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.57 _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 0.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.609 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details ; Sheldrick, G. M. SADABS, An empirical absorption correction program for area detector data. University of Gottingen, Germany, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12226 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.2136 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 28.15 _reflns_number_total 8751 _reflns_number_gt 3228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farrugia L.J., 1997)' _computing_publication_material ? _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.119(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8751 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2400 _refine_ls_R_factor_gt 0.1207 _refine_ls_wR_factor_ref 0.3737 _refine_ls_wR_factor_gt 0.2803 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _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 Ru Ru 0.62920(10) 0.64797(11) 0.72054(5) 0.0551(5) Uani 1 1 d . . . P1 P 0.8295(3) 0.5574(4) 0.77802(17) 0.0642(9) Uani 1 1 d . . . C11 C 0.8047(15) 0.4779(17) 0.8655(8) 0.082(4) Uani 1 1 d . . . C12 C 0.7139(19) 0.567(2) 0.9165(8) 0.098(5) Uani 1 1 d . . . H12 H 0.6754 0.6603 0.9046 0.117 Uiso 1 1 calc R . . C13 C 0.681(2) 0.515(3) 0.9856(8) 0.133(9) Uani 1 1 d . . . H13 H 0.6248 0.5752 1.0193 0.160 Uiso 1 1 calc R . . C14 C 0.731(3) 0.381(3) 1.0024(12) 0.169(12) Uani 1 1 d . . . H14 H 0.6967 0.3450 1.0449 0.203 Uiso 1 1 calc R . . C15 C 0.839(3) 0.292(3) 0.9537(13) 0.191(14) Uani 1 1 d . . . H15 H 0.8901 0.2014 0.9680 0.229 Uiso 1 1 calc R . . C16 C 0.8652(19) 0.340(2) 0.8865(9) 0.124(8) Uani 1 1 d . . . H16 H 0.9253 0.2798 0.8539 0.149 Uiso 1 1 calc R . . C21 C 0.9713(14) 0.4205(15) 0.7303(7) 0.071(4) Uani 1 1 d . . . C22 C 1.0962(14) 0.4266(15) 0.6917(7) 0.071(4) Uani 1 1 d . . . H22 H 1.1188 0.5024 0.6935 0.085 Uiso 1 1 calc R . . C23 C 1.1884(15) 0.3258(17) 0.6509(8) 0.082(4) Uani 1 1 d . . . H23 H 1.2715 0.3342 0.6253 0.099 Uiso 1 1 calc R . . C24 C 1.1589(15) 0.2117(17) 0.6474(9) 0.087(4) Uani 1 1 d . . . H24 H 1.2238 0.1419 0.6207 0.104 Uiso 1 1 calc R . . C25 C 1.0378(18) 0.2007(16) 0.6822(9) 0.093(5) Uani 1 1 d . . . H25 H 1.0195 0.1232 0.6787 0.111 Uiso 1 1 calc R . . C26 C 0.9342(16) 0.3052(16) 0.7251(9) 0.089(5) Uani 1 1 d . . . H26 H 0.8484 0.2985 0.7481 0.107 Uiso 1 1 calc R . . C31 C 0.9160(14) 0.6668(16) 0.7975(7) 0.070(4) Uani 1 1 d . . . C32 C 0.8409(16) 0.8010(17) 0.8052(7) 0.076(4) Uani 1 1 d . . . H32 H 0.7437 0.8358 0.8003 0.092 Uiso 1 1 calc R . . C33 C 0.899(2) 0.890(2) 0.8200(8) 0.099(5) Uani 1 1 d . . . H33 H 0.8450 0.9828 0.8231 0.119 Uiso 1 1 calc R . . C34 C 1.045(3) 0.832(3) 0.8300(10) 0.126(8) Uani 1 1 d . . . H34 H 1.0886 0.8882 0.8402 0.152 Uiso 1 1 calc R . . C35 C 1.125(2) 0.696(3) 0.8253(9) 0.109(7) Uani 1 1 d . . . H35 H 1.2215 0.6593 0.8317 0.131 Uiso 1 1 calc R . . C36 C 1.0590(17) 0.614(2) 0.8108(8) 0.097(5) Uani 1 1 d . . . H36 H 1.1109 0.5208 0.8097 0.116 Uiso 1 1 calc R . . C1 C 0.5199(14) 0.7696(15) 0.7951(6) 0.064(3) Uani 1 1 d . . . C2 C 0.4487(18) 0.8591(17) 0.8360(8) 0.084(4) Uani 1 1 d . . . C3 C 0.3686(17) 0.9536(19) 0.8874(8) 0.083(4) Uani 1 1 d . . . C4 C 0.2830(19) 1.087(2) 0.8698(11) 0.106(6) Uani 1 1 d . . . H4 H 0.2671 1.1145 0.8239 0.128 Uiso 1 1 calc R . . C5 C 0.222(2) 1.176(2) 0.9193(15) 0.132(8) Uani 1 1 d . . . H5 H 0.1714 1.2669 0.9056 0.158 Uiso 1 1 calc R . . C6 C 0.231(4) 1.143(4) 0.9854(18) 0.191(15) Uani 1 1 d . . . H6 H 0.1807 1.2058 1.0183 0.229 Uiso 1 1 calc R . . C7 C 0.309(4) 1.021(4) 1.0041(15) 0.24(2) Uani 1 1 d . . . H7 H 0.3231 0.9971 1.0505 0.287 Uiso 1 1 calc R . . C8 C 0.375(3) 0.924(3) 0.9549(11) 0.198(15) Uani 1 1 d . . . H8 H 0.4263 0.8344 0.9704 0.238 Uiso 1 1 calc R . . P2 P 0.6868(3) 0.8179(3) 0.65519(16) 0.0559(8) Uani 1 1 d . . . N51 N 0.8814(13) 0.9304(13) 0.5833(6) 0.076(3) Uani 1 1 d . . . N52 N 0.6766(11) 0.9572(11) 0.5241(5) 0.064(3) Uani 1 1 d . . . N53 N 0.6378(13) 1.0911(11) 0.6231(6) 0.073(3) Uani 1 1 d . . . C51 C 0.8723(14) 0.8166(14) 0.6313(6) 0.064(3) Uani 1 1 d . . . H51A H 0.9089 0.8183 0.6734 0.077 Uiso 1 1 calc R . . H51B H 0.9336 0.7323 0.6104 0.077 Uiso 1 1 calc R . . C52 C 0.6448(13) 0.8464(13) 0.5663(6) 0.062(3) Uani 1 1 d . . . H52A H 0.6983 0.7631 0.5431 0.074 Uiso 1 1 calc R . . H52B H 0.5431 0.8646 0.5683 0.074 Uiso 1 1 calc R . . C53 C 0.5977(15) 0.9962(15) 0.6768(7) 0.073(4) Uani 1 1 d . . . H53A H 0.4942 1.0210 0.6827 0.087 Uiso 1 1 calc R . . H53B H 0.6230 1.0050 0.7208 0.087 Uiso 1 1 calc R . . C54 C 0.8369(15) 0.9289(17) 0.5171(7) 0.080(4) Uani 1 1 d . . . H54A H 0.8913 0.8406 0.4988 0.096 Uiso 1 1 calc R . . H54B H 0.8590 0.9973 0.4841 0.096 Uiso 1 1 calc R . . C55 C 0.5971(16) 1.0860(14) 0.5552(7) 0.075(4) Uani 1 1 d . . . H55A H 0.4950 1.1029 0.5615 0.090 Uiso 1 1 calc R . . H55B H 0.6129 1.1587 0.5233 0.090 Uiso 1 1 calc R . . C56 C 0.7904(15) 1.0606(16) 0.6126(8) 0.080(4) Uani 1 1 d . . . H56A H 0.8191 1.0612 0.6571 0.097 Uiso 1 1 calc R . . H56B H 0.8092 1.1332 0.5818 0.097 Uiso 1 1 calc R . . B B 0.4903(18) 0.4845(18) 0.6491(8) 0.070(4) Uani 1 1 d . . . H0 H 0.4464 0.4359 0.6275 0.084 Uiso 1 1 calc R . . N41 N 0.5477(10) 0.4912(11) 0.7682(5) 0.060(3) Uani 1 1 d . . . N42 N 0.5065(11) 0.4283(11) 0.7238(5) 0.065(3) Uani 1 1 d . . . N43 N 0.7258(10) 0.5229(10) 0.6312(5) 0.056(2) Uani 1 1 d . . . N44 N 0.6404(11) 0.4709(11) 0.6077(6) 0.063(3) Uani 1 1 d . . . N45 N 0.4334(11) 0.7205(10) 0.6780(5) 0.058(2) Uani 1 1 d . . . N46 N 0.3972(11) 0.6352(12) 0.6488(5) 0.063(3) Uani 1 1 d . . . C41 C 0.4639(16) 0.3314(15) 0.7623(9) 0.083(4) Uani 1 1 d . . . H41 H 0.4317 0.2732 0.7452 0.099 Uiso 1 1 calc R . . C42 C 0.4756(18) 0.3334(18) 0.8287(8) 0.094(5) Uani 1 1 d . . . H42 H 0.4505 0.2798 0.8665 0.112 Uiso 1 1 calc R . . C43 C 0.5326(15) 0.4315(16) 0.8301(7) 0.074(4) Uani 1 1 d . . . H43 H 0.5566 0.4517 0.8697 0.088 Uiso 1 1 calc R . . C44 C 0.6999(15) 0.4208(15) 0.5460(7) 0.074(4) Uani 1 1 d . . . H44 H 0.6598 0.3849 0.5185 0.089 Uiso 1 1 calc R . . C45 C 0.8328(15) 0.4323(14) 0.5307(7) 0.073(4) Uani 1 1 d . . . H45 H 0.9031 0.4023 0.4925 0.088 Uiso 1 1 calc R . . C46 C 0.8373(14) 0.4988(15) 0.5852(6) 0.067(3) Uani 1 1 d . . . H46 H 0.9139 0.5237 0.5881 0.081 Uiso 1 1 calc R . . C47 C 0.2643(14) 0.7024(16) 0.6275(7) 0.069(3) Uani 1 1 d . . . H47 H 0.2186 0.6647 0.6041 0.083 Uiso 1 1 calc R . . C48 C 0.2110(14) 0.8316(17) 0.6460(7) 0.075(4) Uani 1 1 d . . . H48 H 0.1218 0.8994 0.6402 0.090 Uiso 1 1 calc R . . C49 C 0.3235(13) 0.8396(14) 0.6766(7) 0.065(3) Uani 1 1 d . . . H49 H 0.3206 0.9179 0.6935 0.078 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 Ru 0.0534(7) 0.0530(7) 0.0560(6) -0.0005(4) -0.0025(4) -0.0203(5) P1 0.0531(19) 0.073(3) 0.0601(19) 0.0042(17) -0.0059(14) -0.0205(18) C11 0.064(9) 0.086(12) 0.081(9) 0.020(9) -0.012(7) -0.019(8) C12 0.111(13) 0.101(14) 0.081(11) 0.004(10) -0.014(9) -0.044(12) C13 0.139(17) 0.22(3) 0.052(9) 0.006(13) -0.003(10) -0.087(19) C14 0.17(2) 0.19(3) 0.096(16) 0.066(18) -0.029(15) -0.03(2) C15 0.17(2) 0.17(3) 0.126(19) 0.062(18) 0.008(17) 0.02(2) C16 0.096(13) 0.116(17) 0.096(12) 0.044(11) -0.004(9) 0.007(12) C21 0.066(8) 0.064(9) 0.083(9) 0.000(7) -0.017(7) -0.023(7) C22 0.056(8) 0.063(9) 0.087(9) -0.007(7) -0.002(7) -0.019(7) C23 0.056(8) 0.083(12) 0.101(11) -0.015(9) -0.005(7) -0.018(8) C24 0.056(9) 0.077(12) 0.114(12) -0.014(9) -0.007(8) -0.010(8) C25 0.092(12) 0.053(10) 0.129(14) 0.006(9) -0.022(10) -0.025(9) C26 0.066(9) 0.060(10) 0.139(14) -0.004(10) -0.021(9) -0.019(8) C31 0.054(8) 0.079(11) 0.067(8) 0.002(7) -0.007(6) -0.017(8) C32 0.077(10) 0.089(12) 0.065(8) -0.009(8) -0.007(7) -0.034(9) C33 0.115(14) 0.115(15) 0.090(11) -0.021(10) -0.020(10) -0.059(13) C34 0.18(2) 0.15(2) 0.092(13) -0.025(14) -0.018(14) -0.10(2) C35 0.108(14) 0.15(2) 0.099(12) -0.036(14) -0.025(10) -0.073(15) C36 0.091(11) 0.116(15) 0.086(10) -0.018(10) -0.025(8) -0.033(11) C1 0.072(8) 0.072(10) 0.061(7) 0.004(7) -0.012(6) -0.042(8) C2 0.112(12) 0.077(11) 0.077(9) -0.027(8) -0.003(8) -0.048(10) C3 0.089(11) 0.088(13) 0.071(9) -0.024(9) 0.008(8) -0.034(10) C4 0.089(12) 0.079(13) 0.134(15) -0.030(12) 0.018(11) -0.020(11) C5 0.126(17) 0.089(15) 0.17(2) -0.066(16) 0.027(16) -0.033(13) C6 0.24(4) 0.15(3) 0.14(2) -0.10(2) 0.05(2) -0.03(2) C7 0.29(4) 0.19(3) 0.12(2) -0.08(2) 0.01(2) 0.04(3) C8 0.25(3) 0.16(3) 0.081(14) -0.041(16) -0.015(16) 0.04(2) P2 0.0580(18) 0.053(2) 0.0569(17) -0.0020(14) -0.0022(13) -0.0244(16) N51 0.084(8) 0.069(8) 0.082(8) 0.014(6) -0.012(6) -0.043(7) N52 0.066(7) 0.046(6) 0.078(7) 0.003(5) -0.012(5) -0.020(5) N53 0.084(8) 0.049(7) 0.092(8) 0.004(6) -0.022(6) -0.029(6) C51 0.078(8) 0.062(9) 0.058(7) 0.009(6) -0.011(6) -0.037(7) C52 0.051(7) 0.051(8) 0.078(8) -0.001(6) -0.005(6) -0.016(6) C53 0.086(10) 0.078(10) 0.064(8) -0.005(7) -0.012(7) -0.042(8) C54 0.081(10) 0.101(13) 0.065(8) 0.015(8) -0.011(7) -0.047(9) C55 0.092(10) 0.052(9) 0.086(9) 0.015(7) -0.035(8) -0.029(8) C56 0.075(9) 0.072(11) 0.103(11) 0.020(8) -0.027(8) -0.039(9) B 0.083(11) 0.066(11) 0.072(10) -0.014(8) -0.008(8) -0.038(9) N41 0.049(6) 0.068(7) 0.055(6) -0.003(5) 0.003(4) -0.019(5) N42 0.069(7) 0.058(7) 0.070(7) 0.003(5) -0.007(5) -0.030(6) N43 0.049(5) 0.048(6) 0.067(6) 0.000(5) 0.001(4) -0.018(5) N44 0.057(6) 0.052(7) 0.076(7) -0.004(5) -0.003(5) -0.019(5) N45 0.059(6) 0.046(6) 0.064(6) -0.015(5) 0.009(5) -0.020(5) N46 0.054(6) 0.061(7) 0.067(6) 0.002(5) -0.003(5) -0.017(6) C41 0.089(11) 0.060(9) 0.107(12) 0.002(8) 0.003(9) -0.048(8) C42 0.113(13) 0.114(14) 0.070(9) 0.019(9) 0.004(8) -0.075(12) C43 0.077(9) 0.090(11) 0.065(8) 0.002(7) -0.003(6) -0.050(9) C44 0.077(9) 0.086(11) 0.059(8) -0.015(7) 0.008(7) -0.035(8) C45 0.077(9) 0.065(9) 0.063(8) -0.008(7) 0.007(7) -0.017(8) C46 0.063(8) 0.077(10) 0.061(7) -0.002(7) 0.000(6) -0.029(7) C47 0.061(8) 0.075(10) 0.073(8) -0.005(7) -0.010(6) -0.027(8) C48 0.055(8) 0.080(11) 0.079(9) 0.008(8) -0.014(6) -0.014(8) C49 0.057(8) 0.052(8) 0.077(8) 0.004(6) -0.005(6) -0.017(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 Ru C1 1.967(14) . ? Ru N45 2.121(11) . ? Ru N41 2.170(10) . ? Ru N43 2.195(10) . ? Ru P2 2.273(3) . ? Ru P1 2.317(3) . ? P1 C11 1.821(15) . ? P1 C31 1.826(15) . ? P1 C21 1.828(15) . ? C11 C16 1.39(2) . ? C11 C12 1.41(2) . ? C12 C13 1.42(2) . ? C13 C14 1.34(3) . ? C14 C15 1.44(3) . ? C15 C16 1.36(3) . ? C21 C22 1.374(18) . ? C21 C26 1.442(19) . ? C22 C23 1.363(19) . ? C23 C24 1.38(2) . ? C24 C25 1.33(2) . ? C25 C26 1.44(2) . ? C31 C32 1.35(2) . ? C31 C36 1.402(19) . ? C32 C33 1.39(2) . ? C33 C34 1.41(3) . ? C34 C35 1.37(3) . ? C35 C36 1.37(2) . ? C1 C2 1.242(18) . ? C2 C3 1.43(2) . ? C3 C8 1.32(2) . ? C3 C4 1.38(2) . ? C4 C5 1.35(2) . ? C5 C6 1.30(4) . ? C6 C7 1.27(4) . ? C7 C8 1.40(3) . ? P2 C52 1.825(13) . ? P2 C53 1.836(15) . ? P2 C51 1.855(12) . ? N51 C51 1.449(15) . ? N51 C54 1.454(17) . ? N51 C56 1.466(18) . ? N52 C52 1.451(15) . ? N52 C55 1.452(17) . ? N52 C54 1.523(16) . ? N53 C56 1.438(16) . ? N53 C53 1.470(16) . ? N53 C55 1.477(16) . ? B N42 1.513(19) . ? B N46 1.52(2) . ? B N44 1.555(18) . ? N41 C43 1.300(16) . ? N41 N42 1.380(14) . ? N42 C41 1.354(16) . ? N43 C46 1.275(14) . ? N43 N44 1.368(13) . ? N44 C44 1.331(15) . ? N45 C49 1.328(15) . ? N45 N46 1.333(14) . ? N46 C47 1.373(16) . ? C41 C42 1.33(2) . ? C42 C43 1.387(19) . ? C44 C45 1.380(18) . ? C45 C46 1.380(18) . ? C47 C48 1.348(19) . ? C48 C49 1.423(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru N45 85.8(4) . . ? C1 Ru N41 92.3(4) . . ? N45 Ru N41 81.1(4) . . ? C1 Ru N43 172.7(4) . . ? N45 Ru N43 86.9(4) . . ? N41 Ru N43 86.9(4) . . ? C1 Ru P2 91.2(4) . . ? N45 Ru P2 88.8(3) . . ? N41 Ru P2 169.1(3) . . ? N43 Ru P2 88.3(3) . . ? C1 Ru P1 91.3(4) . . ? N45 Ru P1 173.2(3) . . ? N41 Ru P1 92.9(3) . . ? N43 Ru P1 96.0(3) . . ? P2 Ru P1 97.36(13) . . ? C11 P1 C31 98.1(7) . . ? C11 P1 C21 103.9(7) . . ? C31 P1 C21 106.1(6) . . ? C11 P1 Ru 116.4(5) . . ? C31 P1 Ru 120.6(5) . . ? C21 P1 Ru 109.9(4) . . ? C16 C11 C12 117.6(15) . . ? C16 C11 P1 126.6(14) . . ? C12 C11 P1 115.8(12) . . ? C11 C12 C13 121(2) . . ? C14 C13 C12 120(2) . . ? C13 C14 C15 119(2) . . ? C16 C15 C14 120(2) . . ? C15 C16 C11 122(2) . . ? C22 C21 C26 118.4(14) . . ? C22 C21 P1 126.3(12) . . ? C26 C21 P1 114.6(11) . . ? C23 C22 C21 122.5(14) . . ? C22 C23 C24 120.3(14) . . ? C25 C24 C23 120.3(16) . . ? C24 C25 C26 122.1(16) . . ? C21 C26 C25 116.3(14) . . ? C32 C31 C36 116.9(15) . . ? C32 C31 P1 121.1(11) . . ? C36 C31 P1 121.8(13) . . ? C31 C32 C33 124.4(16) . . ? C32 C33 C34 116.0(19) . . ? C35 C34 C33 122.1(19) . . ? C34 C35 C36 118.3(19) . . ? C35 C36 C31 122.2(19) . . ? C2 C1 Ru 172.3(12) . . ? C1 C2 C3 175.4(17) . . ? C8 C3 C4 114.4(18) . . ? C8 C3 C2 123.4(19) . . ? C4 C3 C2 122.1(16) . . ? C5 C4 C3 120(2) . . ? C6 C5 C4 123(3) . . ? C7 C6 C5 119(3) . . ? C6 C7 C8 120(3) . . ? C3 C8 C7 123(3) . . ? C52 P2 C53 96.7(6) . . ? C52 P2 C51 96.1(5) . . ? C53 P2 C51 97.3(6) . . ? C52 P2 Ru 114.3(4) . . ? C53 P2 Ru 121.8(4) . . ? C51 P2 Ru 124.6(4) . . ? C51 N51 C54 111.7(11) . . ? C51 N51 C56 111.0(11) . . ? C54 N51 C56 108.2(12) . . ? C52 N52 C55 111.3(10) . . ? C52 N52 C54 109.9(10) . . ? C55 N52 C54 108.4(11) . . ? C56 N53 C53 111.7(11) . . ? C56 N53 C55 107.4(12) . . ? C53 N53 C55 111.6(10) . . ? N51 C51 P2 113.6(9) . . ? N52 C52 P2 115.3(8) . . ? N53 C53 P2 112.7(9) . . ? N51 C54 N52 112.2(11) . . ? N52 C55 N53 113.8(11) . . ? N53 C56 N51 115.9(11) . . ? N42 B N46 108.5(11) . . ? N42 B N44 109.5(12) . . ? N46 B N44 107.5(11) . . ? C43 N41 N42 107.0(11) . . ? C43 N41 Ru 136.5(10) . . ? N42 N41 Ru 116.4(7) . . ? C41 N42 N41 107.8(11) . . ? C41 N42 B 129.9(12) . . ? N41 N42 B 121.4(10) . . ? C46 N43 N44 105.0(10) . . ? C46 N43 Ru 137.1(9) . . ? N44 N43 Ru 116.8(7) . . ? C44 N44 N43 110.9(10) . . ? C44 N44 B 128.4(11) . . ? N43 N44 B 120.5(10) . . ? C49 N45 N46 106.3(11) . . ? C49 N45 Ru 133.6(9) . . ? N46 N45 Ru 120.0(8) . . ? N45 N46 C47 110.0(11) . . ? N45 N46 B 120.8(11) . . ? C47 N46 B 128.8(12) . . ? C42 C41 N42 108.7(13) . . ? C41 C42 C43 106.2(13) . . ? N41 C43 C42 110.2(13) . . ? N44 C44 C45 106.7(12) . . ? C46 C45 C44 103.9(11) . . ? N43 C46 C45 113.3(12) . . ? C48 C47 N46 109.0(12) . . ? C47 C48 C49 103.5(12) . . ? N45 C49 C48 111.1(13) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.425 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.267 #===END