# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1719 data_erk_987 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54.50 H57 Cl N2 O2 P2 Ru' _chemical_formula_weight 970.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 'triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.511(1) _cell_length_b 13.315(1) _cell_length_c 18.735(2) _cell_angle_alpha 70.27(1) _cell_angle_beta 73.87(1) _cell_angle_gamma 72.15(1) _cell_volume 2523.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 8.27 _cell_measurement_theta_max 10.91 _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1010 _exptl_absorpt_coefficient_mu 0.468 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.8534 _exptl_absorpt_correction_T_max 0.9770 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Nonius MACH3' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 13.3 _diffrn_reflns_number 6996 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.1597 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6601 _reflns_number_gt 4263 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Express (Nonius B.V., 1994)' _computing_cell_refinement 'Express (Nonius B.V., 1994)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL-92 (Keller, 1992)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Toluene is refined with restraints. Hydrogens at N from Fourier, but fixed to the nitrogen atoms. ; _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^)+(0.1758P)^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 'refined as riding atoms (see above)' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6601 _refine_ls_number_parameters 554 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1582 _refine_ls_R_factor_gt 0.0864 _refine_ls_wR_factor_ref 0.2369 _refine_ls_wR_factor_gt 0.2214 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.960 _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 0.12983(7) 0.50193(6) 0.29743(4) 0.0280(3) Uani 1 1 d . . . Cl Cl 0.3092(2) 0.5821(2) 0.24212(15) 0.0461(7) Uani 1 1 d . . . C1 C 0.2326(9) 0.3652(8) 0.4650(5) 0.035(2) Uani 1 1 d . . . O1 O 0.3266(7) 0.3947(5) 0.4628(4) 0.0445(18) Uani 1 1 d . . . N1 N 0.2182(8) 0.2605(6) 0.5051(4) 0.037(2) Uani 1 1 d . . . H1 H 0.1471 0.2458 0.5050 0.045 Uiso 1 1 d R . . C11 C 0.3052(9) 0.1707(7) 0.5480(5) 0.035(2) Uani 1 1 d . . . C12 C 0.3129(12) 0.1954(10) 0.6196(7) 0.059(3) Uani 1 1 d . . . H12A H 0.3301 0.2673 0.6053 0.088 Uiso 1 1 calc R . . H12B H 0.3792 0.1403 0.6432 0.088 Uiso 1 1 calc R . . H12C H 0.2345 0.1944 0.6560 0.088 Uiso 1 1 calc R . . C13 C 0.2514(12) 0.0695(8) 0.5707(7) 0.061(3) Uani 1 1 d . . . H13A H 0.1736 0.0793 0.6075 0.091 Uiso 1 1 calc R . . H13B H 0.3100 0.0047 0.5939 0.091 Uiso 1 1 calc R . . H13C H 0.2366 0.0604 0.5250 0.091 Uiso 1 1 calc R . . C14 C 0.4364(9) 0.1506(8) 0.4970(6) 0.046(3) Uani 1 1 d . . . H14A H 0.4319 0.1329 0.4518 0.068 Uiso 1 1 calc R . . H14B H 0.4918 0.0901 0.5264 0.068 Uiso 1 1 calc R . . H14C H 0.4677 0.2163 0.4807 0.068 Uiso 1 1 calc R . . C2 C 0.1238(9) 0.6412(7) 0.4203(5) 0.030(2) Uani 1 1 d . . . O2 O 0.0445(6) 0.7336(5) 0.4170(4) 0.0411(17) Uani 1 1 d . . . N2 N 0.2328(8) 0.6185(7) 0.4330(5) 0.043(2) Uani 1 1 d . . . H2 H 0.2752 0.5479 0.4400 0.052 Uiso 1 1 d R . . C21 C 0.2991(10) 0.6963(9) 0.4383(7) 0.048(3) Uani 1 1 d . . . C22 C 0.4242(14) 0.6265(12) 0.4524(12) 0.103(6) Uani 1 1 d . . . H22A H 0.4152 0.5746 0.5033 0.154 Uiso 1 1 calc R . . H22B H 0.4769 0.6727 0.4497 0.154 Uiso 1 1 calc R . . H22C H 0.4616 0.5869 0.4135 0.154 Uiso 1 1 calc R . . C23 C 0.2220(14) 0.7488(11) 0.5031(8) 0.071(4) Uani 1 1 d . . . H23A H 0.2378 0.6985 0.5526 0.107 Uiso 1 1 calc R . . H23B H 0.1343 0.7647 0.5021 0.107 Uiso 1 1 calc R . . H23C H 0.2451 0.8164 0.4956 0.107 Uiso 1 1 calc R . . C24 C 0.3126(13) 0.7836(9) 0.3591(8) 0.066(4) Uani 1 1 d . . . H24A H 0.3630 0.8302 0.3589 0.099 Uiso 1 1 calc R . . H24B H 0.2310 0.8279 0.3501 0.099 Uiso 1 1 calc R . . H24C H 0.3524 0.7473 0.3185 0.099 Uiso 1 1 calc R . . C3 C 0.1320(9) 0.4337(7) 0.4239(5) 0.030(2) Uani 1 1 d . . . C4 C 0.0830(9) 0.5513(7) 0.4080(5) 0.032(2) Uani 1 1 d . . . C5 C -0.0261(8) 0.5778(8) 0.3776(5) 0.030(2) Uani 1 1 d . . . H5 H -0.0768 0.6485 0.3622 0.036 Uiso 1 1 calc R . . C6 C -0.0455(9) 0.4797(8) 0.3745(5) 0.034(2) Uani 1 1 d . . . H6 H -0.1102 0.4730 0.3562 0.041 Uiso 1 1 calc R . . C7 C 0.0485(9) 0.3961(8) 0.4034(5) 0.032(2) Uani 1 1 d . . . H7 H 0.0559 0.3217 0.4088 0.039 Uiso 1 1 calc R . . P1 P 0.2326(3) 0.3529(2) 0.24664(15) 0.0374(7) Uani 1 1 d . . . P2 P 0.0414(3) 0.6239(2) 0.19209(14) 0.0378(7) Uani 1 1 d . . . C31 C 0.2544(12) 0.3596(10) 0.1452(6) 0.053(3) Uani 1 1 d . . . C32 C 0.3362(13) 0.4177(11) 0.0926(7) 0.070(4) Uani 1 1 d . . . H32 H 0.3740 0.4568 0.1093 0.084 Uiso 1 1 calc R . . C33 C 0.3645(17) 0.4201(16) 0.0152(9) 0.095(5) Uani 1 1 d . . . H33 H 0.4185 0.4629 -0.0202 0.114 Uiso 1 1 calc R . . C34 C 0.316(2) 0.3619(16) -0.0092(10) 0.116(8) Uani 1 1 d . . . H34 H 0.3425 0.3583 -0.0607 0.139 Uiso 1 1 calc R . . C35 C 0.223(2) 0.3044(16) 0.0412(11) 0.119(8) Uani 1 1 d . . . H35 H 0.1825 0.2700 0.0222 0.143 Uiso 1 1 calc R . . C36 C 0.1944(14) 0.3017(11) 0.1201(8) 0.072(4) Uani 1 1 d . . . H36 H 0.1370 0.2624 0.1555 0.086 Uiso 1 1 calc R . . C41 C 0.3934(11) 0.2907(9) 0.2562(6) 0.047(3) Uani 1 1 d . . . C42 C 0.4527(11) 0.3199(10) 0.2989(6) 0.051(3) Uani 1 1 d . . . H42 H 0.4085 0.3755 0.3233 0.061 Uiso 1 1 calc R . . C43 C 0.5731(12) 0.2702(11) 0.3065(7) 0.061(4) Uani 1 1 d . . . H43 H 0.6098 0.2937 0.3351 0.073 Uiso 1 1 calc R . . C44 C 0.6415(12) 0.1881(11) 0.2741(7) 0.067(4) Uani 1 1 d . . . H44 H 0.7243 0.1541 0.2798 0.080 Uiso 1 1 calc R . . C45 C 0.5828(13) 0.1565(11) 0.2315(8) 0.067(4) Uani 1 1 d . . . H45 H 0.6262 0.0992 0.2086 0.081 Uiso 1 1 calc R . . C46 C 0.4654(12) 0.2072(10) 0.2233(7) 0.061(3) Uani 1 1 d . . . H46 H 0.4298 0.1849 0.1935 0.074 Uiso 1 1 calc R . . C51 C 0.1618(10) 0.2338(8) 0.2976(6) 0.041(3) Uani 1 1 d . . . C52 C 0.2210(12) 0.1398(9) 0.3443(7) 0.054(3) Uani 1 1 d . . . H52 H 0.3031 0.1325 0.3479 0.065 Uiso 1 1 calc R . . C53 C 0.1625(17) 0.0545(11) 0.3868(8) 0.079(4) Uani 1 1 d . . . H53 H 0.2048 -0.0095 0.4187 0.094 Uiso 1 1 calc R . . C54 C 0.0411(17) 0.0646(12) 0.3816(9) 0.081(5) Uani 1 1 d . . . H54 H 0.0023 0.0061 0.4087 0.097 Uiso 1 1 calc R . . C55 C -0.0214(14) 0.1576(12) 0.3380(8) 0.073(4) Uani 1 1 d . . . H55 H -0.1042 0.1650 0.3355 0.088 Uiso 1 1 calc R . . C56 C 0.0388(13) 0.2433(10) 0.2964(8) 0.064(3) Uani 1 1 d . . . H56 H -0.0055 0.3088 0.2670 0.076 Uiso 1 1 calc R . . C61 C -0.1104(9) 0.6035(10) 0.2007(5) 0.046(3) Uani 1 1 d . . . C62 C -0.2217(11) 0.6714(12) 0.2288(7) 0.065(4) Uani 1 1 d . . . H62 H -0.2200 0.7369 0.2368 0.078 Uiso 1 1 calc R . . C63 C -0.3352(13) 0.6423(16) 0.2450(9) 0.091(5) Uani 1 1 d . . . H63 H -0.4090 0.6880 0.2643 0.109 Uiso 1 1 calc R . . C64 C -0.3397(13) 0.5477(15) 0.2328(7) 0.077(4) Uani 1 1 d . . . H64 H -0.4166 0.5292 0.2435 0.092 Uiso 1 1 calc R . . C65 C -0.2347(13) 0.4811(14) 0.2055(8) 0.073(4) Uani 1 1 d . . . H65 H -0.2396 0.4167 0.1974 0.088 Uiso 1 1 calc R . . C66 C -0.1222(11) 0.5047(10) 0.1895(6) 0.050(3) Uani 1 1 d . . . H66 H -0.0505 0.4563 0.1709 0.060 Uiso 1 1 calc R . . C71 C 0.1128(10) 0.6390(9) 0.0891(5) 0.044(3) Uani 1 1 d . . . C72 C 0.0605(13) 0.6227(11) 0.0380(6) 0.063(4) Uani 1 1 d . . . H72 H -0.0099 0.5929 0.0568 0.076 Uiso 1 1 calc R . . C73 C 0.1092(17) 0.6492(13) -0.0414(7) 0.088(5) Uani 1 1 d . . . H73 H 0.0701 0.6423 -0.0768 0.106 Uiso 1 1 calc R . . C74 C 0.2190(15) 0.6864(12) -0.0656(8) 0.082(5) Uani 1 1 d . . . H74 H 0.2590 0.6985 -0.1179 0.098 Uiso 1 1 calc R . . C75 C 0.2688(14) 0.7054(12) -0.0150(8) 0.077(4) Uani 1 1 d . . . H75 H 0.3388 0.7359 -0.0338 0.092 Uiso 1 1 calc R . . C76 C 0.2202(12) 0.6814(11) 0.0623(7) 0.062(3) Uani 1 1 d . . . H76 H 0.2573 0.6929 0.0969 0.074 Uiso 1 1 calc R . . C81 C 0.0054(10) 0.7724(9) 0.1866(6) 0.045(3) Uani 1 1 d . . . C82 C -0.0531(13) 0.8469(10) 0.1310(8) 0.072(4) Uani 1 1 d . . . H82 H -0.0738 0.8230 0.0953 0.086 Uiso 1 1 calc R . . C83 C -0.0840(18) 0.9599(13) 0.1247(10) 0.102(6) Uani 1 1 d . . . H83 H -0.1281 1.0113 0.0871 0.122 Uiso 1 1 calc R . . C84 C -0.0464(16) 0.9931(10) 0.1772(10) 0.092(6) Uani 1 1 d . . . H84 H -0.0655 1.0676 0.1756 0.110 Uiso 1 1 calc R . . C85 C 0.0179(14) 0.9154(10) 0.2302(8) 0.072(4) Uani 1 1 d . . . H85 H 0.0452 0.9379 0.2639 0.086 Uiso 1 1 calc R . . C86 C 0.0446(11) 0.8047(9) 0.2364(7) 0.053(3) Uani 1 1 d . . . H86 H 0.0886 0.7527 0.2739 0.063 Uiso 1 1 calc R . . C91 C 0.566(4) 0.152(3) -0.085(2) 0.18(2) Uiso 0.50 1 d PGD . . H91 H 0.5537 0.2051 -0.0590 0.212 Uiso 0.50 1 calc PR . . C92 C 0.473(3) 0.153(3) -0.119(3) 0.24(3) Uiso 0.50 1 d PG . . H92 H 0.3971 0.2067 -0.1161 0.294 Uiso 0.50 1 calc PR . . C93 C 0.491(4) 0.076(4) -0.158(2) 0.20(3) Uiso 0.50 1 d PG . . H93 H 0.4275 0.0762 -0.1808 0.246 Uiso 0.50 1 calc PR . . C94 C 0.602(4) -0.003(3) -0.162(2) 0.23(3) Uiso 0.50 1 d PG . . H94 H 0.6146 -0.0559 -0.1885 0.272 Uiso 0.50 1 calc PR . . C95 C 0.696(3) -0.004(3) -0.128(2) 0.146(16) Uiso 0.50 1 d PGD . . H95 H 0.7712 -0.0576 -0.1314 0.175 Uiso 0.50 1 calc PR . . C96 C 0.678(3) 0.074(3) -0.0897(19) 0.163(19) Uiso 0.50 1 d PGD . . C97 C 0.757(6) 0.046(6) -0.028(4) 0.35(5) Uiso 0.50 1 d PD . . H97A H 0.7036 0.0611 0.0193 0.522 Uiso 0.50 1 calc PR . . H97B H 0.8174 0.0915 -0.0471 0.522 Uiso 0.50 1 calc PR . . H97C H 0.8006 -0.0305 -0.0173 0.522 Uiso 0.50 1 calc PR . . 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 0.0273(5) 0.0341(5) 0.0241(4) -0.0085(3) 0.0001(3) -0.0133(3) Cl 0.0374(15) 0.0558(16) 0.0463(15) -0.0115(13) 0.0025(12) -0.0253(13) C1 0.034(6) 0.033(6) 0.033(5) -0.011(4) -0.008(5) 0.002(5) O1 0.039(4) 0.041(4) 0.057(5) -0.008(3) -0.009(4) -0.020(4) N1 0.047(5) 0.031(5) 0.034(4) 0.001(4) -0.008(4) -0.020(4) C11 0.042(6) 0.020(5) 0.040(6) -0.003(4) -0.012(5) -0.004(4) C12 0.058(8) 0.063(8) 0.050(7) -0.018(6) -0.013(6) -0.002(6) C13 0.075(9) 0.026(6) 0.071(8) -0.004(5) -0.013(7) -0.010(6) C14 0.034(6) 0.036(6) 0.056(7) -0.014(5) -0.006(5) 0.004(5) C2 0.031(6) 0.030(5) 0.034(5) -0.006(4) -0.008(4) -0.015(5) O2 0.041(4) 0.032(4) 0.049(4) -0.015(3) 0.000(3) -0.010(3) N2 0.045(6) 0.036(5) 0.056(6) -0.012(4) -0.006(5) -0.024(4) C21 0.040(7) 0.049(6) 0.065(7) -0.018(6) -0.011(6) -0.022(5) C22 0.065(10) 0.070(10) 0.20(2) -0.041(11) -0.057(12) -0.023(8) C23 0.099(11) 0.071(9) 0.067(8) -0.024(7) -0.012(8) -0.051(8) C24 0.072(9) 0.046(7) 0.077(9) -0.012(6) 0.002(7) -0.028(7) C3 0.028(5) 0.032(5) 0.025(5) -0.001(4) 0.004(4) -0.015(4) C4 0.040(6) 0.027(5) 0.022(5) -0.004(4) 0.011(4) -0.015(4) C5 0.022(5) 0.034(5) 0.024(5) -0.002(4) -0.001(4) -0.004(4) C6 0.029(6) 0.051(6) 0.024(5) -0.013(5) -0.001(4) -0.013(5) C7 0.039(6) 0.036(5) 0.019(5) 0.003(4) 0.000(4) -0.022(5) P1 0.0397(17) 0.0422(15) 0.0322(14) -0.0149(12) -0.0027(12) -0.0110(13) P2 0.0397(17) 0.0467(16) 0.0247(13) -0.0083(12) 0.0000(12) -0.0140(13) C31 0.062(8) 0.067(8) 0.026(6) -0.020(5) -0.006(6) -0.005(6) C32 0.077(10) 0.082(9) 0.037(7) -0.022(7) 0.000(7) -0.003(8) C33 0.100(13) 0.115(14) 0.062(10) -0.039(10) -0.014(9) 0.000(11) C34 0.16(2) 0.098(14) 0.043(9) -0.018(9) -0.002(11) 0.017(13) C35 0.17(2) 0.112(14) 0.098(14) -0.073(13) -0.076(15) 0.037(14) C36 0.091(11) 0.077(9) 0.058(8) -0.028(7) -0.021(8) -0.018(8) C41 0.053(7) 0.049(6) 0.029(5) -0.007(5) 0.009(5) -0.021(6) C42 0.051(8) 0.059(7) 0.035(6) -0.007(5) 0.001(5) -0.019(6) C43 0.059(9) 0.085(9) 0.040(7) 0.007(7) -0.014(6) -0.039(8) C44 0.044(8) 0.077(9) 0.051(8) 0.001(7) 0.000(6) -0.004(7) C45 0.058(9) 0.059(8) 0.065(8) -0.020(7) 0.005(7) 0.001(7) C46 0.054(9) 0.053(7) 0.067(8) -0.016(6) -0.009(7) 0.000(6) C51 0.044(7) 0.040(6) 0.048(6) -0.025(5) 0.004(5) -0.021(5) C52 0.065(8) 0.035(6) 0.061(7) -0.015(6) -0.010(6) -0.013(6) C53 0.131(15) 0.049(8) 0.073(9) -0.016(7) -0.019(9) -0.045(9) C54 0.117(14) 0.060(9) 0.088(11) -0.016(8) -0.018(10) -0.058(9) C55 0.074(10) 0.079(10) 0.087(10) -0.027(9) -0.012(8) -0.044(8) C56 0.066(9) 0.052(7) 0.083(9) -0.024(7) -0.022(7) -0.016(7) C61 0.028(6) 0.077(8) 0.022(5) -0.010(5) -0.004(4) -0.003(6) C62 0.040(8) 0.096(10) 0.067(8) -0.039(8) -0.015(6) -0.005(7) C63 0.039(9) 0.146(16) 0.089(11) -0.065(11) 0.016(7) -0.013(9) C64 0.049(9) 0.141(14) 0.043(7) -0.016(8) -0.004(6) -0.041(9) C65 0.058(10) 0.119(12) 0.060(8) -0.030(8) -0.004(7) -0.045(9) C66 0.051(8) 0.059(7) 0.037(6) -0.011(5) -0.006(5) -0.013(6) C71 0.049(7) 0.053(7) 0.023(5) -0.007(5) 0.001(5) -0.011(6) C72 0.076(9) 0.087(9) 0.036(7) -0.018(6) -0.003(6) -0.037(8) C73 0.138(15) 0.107(12) 0.032(7) -0.013(7) -0.004(8) -0.063(11) C74 0.095(12) 0.094(11) 0.035(7) 0.000(7) 0.003(8) -0.025(9) C75 0.066(10) 0.092(10) 0.059(9) -0.012(8) 0.017(7) -0.038(8) C76 0.063(9) 0.085(9) 0.040(7) -0.020(6) 0.010(6) -0.034(7) C81 0.049(7) 0.047(6) 0.035(6) -0.007(5) -0.008(5) -0.009(5) C82 0.084(11) 0.052(8) 0.071(9) -0.017(7) -0.017(8) -0.002(7) C83 0.127(16) 0.067(10) 0.088(12) -0.005(9) -0.037(11) 0.007(10) C84 0.111(13) 0.031(7) 0.098(12) -0.018(8) 0.008(10) 0.008(8) C85 0.088(11) 0.049(8) 0.070(9) -0.020(7) 0.007(8) -0.021(7) C86 0.062(8) 0.052(7) 0.046(7) -0.009(5) 0.003(6) -0.032(6) _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 C7 2.166(8) . ? Ru C6 2.169(9) . ? Ru C5 2.217(9) . ? Ru C3 2.238(9) . ? Ru C4 2.257(9) . ? Ru P1 2.335(3) . ? Ru P2 2.347(3) . ? Ru Cl 2.427(3) . ? C1 O1 1.245(12) . ? C1 N1 1.378(12) . ? C1 C3 1.463(13) . ? N1 C11 1.464(12) . ? C11 C12 1.515(14) . ? C11 C13 1.536(14) . ? C11 C14 1.545(14) . ? C2 N2 1.269(12) . ? C2 O2 1.281(11) . ? C2 C4 1.516(13) . ? N2 C21 1.503(13) . ? C21 C22 1.493(17) . ? C21 C23 1.532(17) . ? C21 C24 1.548(16) . ? C3 C7 1.398(13) . ? C3 C4 1.447(13) . ? C4 C5 1.420(13) . ? C5 C6 1.413(13) . ? C6 C7 1.372(14) . ? P1 C41 1.813(12) . ? P1 C31 1.822(10) . ? P1 C51 1.851(10) . ? P2 C61 1.805(11) . ? P2 C71 1.843(10) . ? P2 C81 1.864(11) . ? C31 C32 1.368(18) . ? C31 C36 1.430(17) . ? C32 C33 1.387(19) . ? C33 C34 1.33(3) . ? C34 C35 1.44(3) . ? C35 C36 1.41(2) . ? C41 C46 1.384(15) . ? C41 C42 1.390(16) . ? C42 C43 1.365(17) . ? C43 C44 1.356(18) . ? C44 C45 1.404(19) . ? C45 C46 1.338(18) . ? C51 C52 1.367(15) . ? C51 C56 1.389(16) . ? C52 C53 1.392(17) . ? C53 C54 1.39(2) . ? C54 C55 1.35(2) . ? C55 C56 1.405(18) . ? C61 C62 1.404(16) . ? C61 C66 1.450(16) . ? C62 C63 1.40(2) . ? C63 C64 1.37(2) . ? C64 C65 1.35(2) . ? C65 C66 1.356(17) . ? C71 C72 1.366(16) . ? C71 C76 1.411(16) . ? C72 C73 1.399(17) . ? C73 C74 1.40(2) . ? C74 C75 1.36(2) . ? C75 C76 1.364(17) . ? C81 C82 1.344(17) . ? C81 C86 1.373(15) . ? C82 C83 1.41(2) . ? C83 C84 1.41(2) . ? C84 C85 1.36(2) . ? C85 C86 1.380(16) . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C95 C96 1.3900 . ? C96 C97 1.554(9) . ? 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 C7 Ru C6 36.9(4) . . ? C7 Ru C5 61.3(4) . . ? C6 Ru C5 37.6(3) . . ? C7 Ru C3 37.0(3) . . ? C6 Ru C3 63.0(3) . . ? C5 Ru C3 62.6(3) . . ? C7 Ru C4 61.2(3) . . ? C6 Ru C4 62.5(3) . . ? C5 Ru C4 37.0(3) . . ? C3 Ru C4 37.6(3) . . ? C7 Ru P1 91.3(3) . . ? C6 Ru P1 112.3(3) . . ? C5 Ru P1 149.5(3) . . ? C3 Ru P1 104.3(2) . . ? C4 Ru P1 141.4(2) . . ? C7 Ru P2 130.5(3) . . ? C6 Ru P2 95.7(3) . . ? C5 Ru P2 89.9(2) . . ? C3 Ru P2 152.6(2) . . ? C4 Ru P2 118.6(2) . . ? P1 Ru P2 99.68(9) . . ? C7 Ru Cl 140.8(3) . . ? C6 Ru Cl 155.6(3) . . ? C5 Ru Cl 118.5(3) . . ? C3 Ru Cl 105.1(2) . . ? C4 Ru Cl 94.8(2) . . ? P1 Ru Cl 90.94(10) . . ? P2 Ru Cl 87.45(10) . . ? O1 C1 N1 121.3(9) . . ? O1 C1 C3 124.5(9) . . ? N1 C1 C3 114.1(9) . . ? C1 N1 C11 127.5(8) . . ? N1 C11 C12 110.6(8) . . ? N1 C11 C13 105.2(8) . . ? C12 C11 C13 110.4(9) . . ? N1 C11 C14 111.1(8) . . ? C12 C11 C14 109.4(9) . . ? C13 C11 C14 110.1(8) . . ? N2 C2 O2 125.8(9) . . ? N2 C2 C4 117.4(9) . . ? O2 C2 C4 116.8(8) . . ? C2 N2 C21 127.3(9) . . ? C22 C21 N2 104.4(9) . . ? C22 C21 C23 114.3(12) . . ? N2 C21 C23 108.4(9) . . ? C22 C21 C24 110.1(12) . . ? N2 C21 C24 107.7(9) . . ? C23 C21 C24 111.4(10) . . ? C7 C3 C4 104.7(8) . . ? C7 C3 C1 126.0(8) . . ? C4 C3 C1 128.4(9) . . ? C7 C3 Ru 68.7(5) . . ? C4 C3 Ru 71.9(5) . . ? C1 C3 Ru 131.2(6) . . ? C5 C4 C3 107.7(8) . . ? C5 C4 C2 119.7(8) . . ? C3 C4 C2 132.6(9) . . ? C5 C4 Ru 70.0(5) . . ? C3 C4 Ru 70.5(5) . . ? C2 C4 Ru 126.4(6) . . ? C6 C5 C4 108.3(8) . . ? C6 C5 Ru 69.4(5) . . ? C4 C5 Ru 73.0(5) . . ? C7 C6 C5 106.7(9) . . ? C7 C6 Ru 71.4(5) . . ? C5 C6 Ru 73.0(5) . . ? C6 C7 C3 112.6(9) . . ? C6 C7 Ru 71.7(5) . . ? C3 C7 Ru 74.3(5) . . ? C41 P1 C31 96.8(5) . . ? C41 P1 C51 100.8(5) . . ? C31 P1 C51 103.1(5) . . ? C41 P1 Ru 117.4(4) . . ? C31 P1 Ru 123.7(4) . . ? C51 P1 Ru 111.6(3) . . ? C61 P2 C71 104.2(5) . . ? C61 P2 C81 102.1(5) . . ? C71 P2 C81 96.2(5) . . ? C61 P2 Ru 109.5(3) . . ? C71 P2 Ru 126.1(4) . . ? C81 P2 Ru 115.7(3) . . ? C32 C31 C36 119.8(11) . . ? C32 C31 P1 118.0(10) . . ? C36 C31 P1 122.1(10) . . ? C31 C32 C33 121.4(15) . . ? C34 C33 C32 120.3(19) . . ? C33 C34 C35 121.7(16) . . ? C36 C35 C34 117.6(18) . . ? C35 C36 C31 118.9(16) . . ? C46 C41 C42 114.8(11) . . ? C46 C41 P1 122.1(9) . . ? C42 C41 P1 123.1(9) . . ? C43 C42 C41 122.0(12) . . ? C44 C43 C42 122.1(12) . . ? C43 C44 C45 116.8(12) . . ? C46 C45 C44 120.5(12) . . ? C45 C46 C41 123.9(13) . . ? C52 C51 C56 117.4(10) . . ? C52 C51 P1 122.5(9) . . ? C56 C51 P1 119.7(9) . . ? C51 C52 C53 121.6(13) . . ? C54 C53 C52 119.5(14) . . ? C55 C54 C53 120.5(13) . . ? C54 C55 C56 119.1(14) . . ? C51 C56 C55 121.8(12) . . ? C62 C61 C66 115.9(11) . . ? C62 C61 P2 123.2(10) . . ? C66 C61 P2 120.3(8) . . ? C63 C62 C61 120.5(13) . . ? C64 C63 C62 120.6(13) . . ? C65 C64 C63 120.4(13) . . ? C64 C65 C66 121.6(14) . . ? C65 C66 C61 121.1(12) . . ? C72 C71 C76 120.0(10) . . ? C72 C71 P2 123.7(9) . . ? C76 C71 P2 115.9(8) . . ? C71 C72 C73 121.7(13) . . ? C72 C73 C74 116.8(13) . . ? C75 C74 C73 121.2(12) . . ? C74 C75 C76 121.9(14) . . ? C75 C76 C71 118.2(12) . . ? C82 C81 C86 120.8(11) . . ? C82 C81 P2 119.2(9) . . ? C86 C81 P2 119.9(8) . . ? C81 C82 C83 121.6(14) . . ? C82 C83 C84 117.5(14) . . ? C85 C84 C83 118.8(13) . . ? C84 C85 C86 122.6(14) . . ? C81 C86 C85 118.4(12) . . ? C92 C91 C96 120.0 . . ? C93 C92 C91 120.0 . . ? C92 C93 C94 120.0 . . ? C95 C94 C93 120.0 . . ? C94 C95 C96 120.0 . . ? C95 C96 C91 120.0 . . ? C95 C96 C97 118.1(9) . . ? C91 C96 C97 118.0(9) . . ? 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 O1 C1 N1 C11 -1.3(15) . . . . ? C3 C1 N1 C11 176.1(8) . . . . ? C1 N1 C11 C12 68.9(13) . . . . ? C1 N1 C11 C13 -171.9(9) . . . . ? C1 N1 C11 C14 -52.8(12) . . . . ? O2 C2 N2 C21 -7.5(17) . . . . ? C4 C2 N2 C21 172.8(9) . . . . ? C2 N2 C21 C22 -178.9(12) . . . . ? C2 N2 C21 C23 58.8(14) . . . . ? C2 N2 C21 C24 -61.9(14) . . . . ? O1 C1 C3 C7 157.4(9) . . . . ? N1 C1 C3 C7 -19.9(13) . . . . ? O1 C1 C3 C4 -34.6(15) . . . . ? N1 C1 C3 C4 148.1(9) . . . . ? O1 C1 C3 Ru 65.1(13) . . . . ? N1 C1 C3 Ru -112.2(9) . . . . ? C6 Ru C3 C7 35.3(6) . . . . ? C5 Ru C3 C7 77.8(6) . . . . ? C4 Ru C3 C7 114.4(8) . . . . ? P1 Ru C3 C7 -72.6(6) . . . . ? P2 Ru C3 C7 77.5(7) . . . . ? Cl Ru C3 C7 -167.6(5) . . . . ? C7 Ru C3 C4 -114.4(8) . . . . ? C6 Ru C3 C4 -79.1(6) . . . . ? C5 Ru C3 C4 -36.7(5) . . . . ? P1 Ru C3 C4 172.9(5) . . . . ? P2 Ru C3 C4 -36.9(8) . . . . ? Cl Ru C3 C4 78.0(5) . . . . ? C7 Ru C3 C1 119.9(11) . . . . ? C6 Ru C3 C1 155.2(10) . . . . ? C5 Ru C3 C1 -162.4(10) . . . . ? C4 Ru C3 C1 -125.7(11) . . . . ? P1 Ru C3 C1 47.2(9) . . . . ? P2 Ru C3 C1 -162.6(6) . . . . ? Cl Ru C3 C1 -47.7(9) . . . . ? C7 C3 C4 C5 -1.0(9) . . . . ? C1 C3 C4 C5 -171.0(9) . . . . ? Ru C3 C4 C5 60.3(6) . . . . ? C7 C3 C4 C2 176.7(9) . . . . ? C1 C3 C4 C2 6.7(16) . . . . ? Ru C3 C4 C2 -122.0(10) . . . . ? C7 C3 C4 Ru -61.3(6) . . . . ? C1 C3 C4 Ru 128.7(10) . . . . ? N2 C2 C4 C5 -166.7(9) . . . . ? O2 C2 C4 C5 13.5(12) . . . . ? N2 C2 C4 C3 15.8(15) . . . . ? O2 C2 C4 C3 -164.0(9) . . . . ? N2 C2 C4 Ru -80.7(11) . . . . ? O2 C2 C4 Ru 99.5(9) . . . . ? C7 Ru C4 C5 -79.5(6) . . . . ? C6 Ru C4 C5 -37.5(5) . . . . ? C3 Ru C4 C5 -118.2(8) . . . . ? P1 Ru C4 C5 -129.3(5) . . . . ? P2 Ru C4 C5 43.4(6) . . . . ? Cl Ru C4 C5 133.1(5) . . . . ? C7 Ru C4 C3 38.7(5) . . . . ? C6 Ru C4 C3 80.7(6) . . . . ? C5 Ru C4 C3 118.2(8) . . . . ? P1 Ru C4 C3 -11.0(7) . . . . ? P2 Ru C4 C3 161.6(4) . . . . ? Cl Ru C4 C3 -108.6(5) . . . . ? C7 Ru C4 C2 167.8(10) . . . . ? C6 Ru C4 C2 -150.2(9) . . . . ? C5 Ru C4 C2 -112.7(10) . . . . ? C3 Ru C4 C2 129.1(11) . . . . ? P1 Ru C4 C2 118.0(7) . . . . ? P2 Ru C4 C2 -69.3(9) . . . . ? Cl Ru C4 C2 20.5(8) . . . . ? C3 C4 C5 C6 0.1(10) . . . . ? C2 C4 C5 C6 -178.0(7) . . . . ? Ru C4 C5 C6 60.8(6) . . . . ? C3 C4 C5 Ru -60.7(6) . . . . ? C2 C4 C5 Ru 121.3(8) . . . . ? C7 Ru C5 C6 -38.4(5) . . . . ? C3 Ru C5 C6 -80.5(6) . . . . ? C4 Ru C5 C6 -117.7(8) . . . . ? P1 Ru C5 C6 -9.9(8) . . . . ? P2 Ru C5 C6 99.4(5) . . . . ? Cl Ru C5 C6 -173.5(5) . . . . ? C7 Ru C5 C4 79.3(6) . . . . ? C6 Ru C5 C4 117.7(8) . . . . ? C3 Ru C5 C4 37.2(5) . . . . ? P1 Ru C5 C4 107.9(6) . . . . ? P2 Ru C5 C4 -142.9(5) . . . . ? Cl Ru C5 C4 -55.8(5) . . . . ? C4 C5 C6 C7 0.9(10) . . . . ? Ru C5 C6 C7 64.0(6) . . . . ? C4 C5 C6 Ru -63.1(6) . . . . ? C5 Ru C6 C7 -114.8(8) . . . . ? C3 Ru C6 C7 -35.4(5) . . . . ? C4 Ru C6 C7 -77.9(6) . . . . ? P1 Ru C6 C7 59.8(6) . . . . ? P2 Ru C6 C7 162.7(5) . . . . ? Cl Ru C6 C7 -101.0(8) . . . . ? C7 Ru C6 C5 114.8(8) . . . . ? C3 Ru C6 C5 79.4(6) . . . . ? C4 Ru C6 C5 36.9(5) . . . . ? P1 Ru C6 C5 174.6(4) . . . . ? P2 Ru C6 C5 -82.5(5) . . . . ? Cl Ru C6 C5 13.8(10) . . . . ? C5 C6 C7 C3 -1.5(10) . . . . ? Ru C6 C7 C3 63.5(7) . . . . ? C5 C6 C7 Ru -65.0(6) . . . . ? C4 C3 C7 C6 1.6(10) . . . . ? C1 C3 C7 C6 171.9(9) . . . . ? Ru C3 C7 C6 -61.9(6) . . . . ? C4 C3 C7 Ru 63.5(6) . . . . ? C1 C3 C7 Ru -126.2(9) . . . . ? C5 Ru C7 C6 39.1(5) . . . . ? C3 Ru C7 C6 120.9(8) . . . . ? C4 Ru C7 C6 81.6(6) . . . . ? P1 Ru C7 C6 -126.8(5) . . . . ? P2 Ru C7 C6 -22.9(7) . . . . ? Cl Ru C7 C6 140.0(5) . . . . ? C6 Ru C7 C3 -120.9(8) . . . . ? C5 Ru C7 C3 -81.7(6) . . . . ? C4 Ru C7 C3 -39.3(6) . . . . ? P1 Ru C7 C3 112.3(5) . . . . ? P2 Ru C7 C3 -143.7(5) . . . . ? Cl Ru C7 C3 19.2(8) . . . . ? C7 Ru P1 C41 -96.5(4) . . . . ? C6 Ru P1 C41 -127.8(5) . . . . ? C5 Ru P1 C41 -121.3(6) . . . . ? C3 Ru P1 C41 -61.5(4) . . . . ? C4 Ru P1 C41 -54.5(6) . . . . ? P2 Ru P1 C41 132.0(4) . . . . ? Cl Ru P1 C41 44.4(4) . . . . ? C7 Ru P1 C31 143.0(6) . . . . ? C6 Ru P1 C31 111.7(6) . . . . ? C5 Ru P1 C31 118.2(7) . . . . ? C3 Ru P1 C31 178.0(6) . . . . ? C4 Ru P1 C31 -175.0(6) . . . . ? P2 Ru P1 C31 11.5(5) . . . . ? Cl Ru P1 C31 -76.1(5) . . . . ? C7 Ru P1 C51 19.2(5) . . . . ? C6 Ru P1 C51 -12.1(5) . . . . ? C5 Ru P1 C51 -5.6(6) . . . . ? C3 Ru P1 C51 54.2(5) . . . . ? C4 Ru P1 C51 61.1(6) . . . . ? P2 Ru P1 C51 -112.4(4) . . . . ? Cl Ru P1 C51 160.1(4) . . . . ? C7 Ru P2 C61 -10.4(5) . . . . ? C6 Ru P2 C61 -24.0(5) . . . . ? C5 Ru P2 C61 -61.1(5) . . . . ? C3 Ru P2 C61 -60.9(7) . . . . ? C4 Ru P2 C61 -85.6(5) . . . . ? P1 Ru P2 C61 89.8(4) . . . . ? Cl Ru P2 C61 -179.7(4) . . . . ? C7 Ru P2 C71 -135.9(6) . . . . ? C6 Ru P2 C71 -149.5(5) . . . . ? C5 Ru P2 C71 173.4(5) . . . . ? C3 Ru P2 C71 173.6(7) . . . . ? C4 Ru P2 C71 148.9(5) . . . . ? P1 Ru P2 C71 -35.7(5) . . . . ? Cl Ru P2 C71 54.8(5) . . . . ? C7 Ru P2 C81 104.3(5) . . . . ? C6 Ru P2 C81 90.7(5) . . . . ? C5 Ru P2 C81 53.5(5) . . . . ? C3 Ru P2 C81 53.7(7) . . . . ? C4 Ru P2 C81 29.1(5) . . . . ? P1 Ru P2 C81 -155.5(4) . . . . ? Cl Ru P2 C81 -65.0(4) . . . . ? C41 P1 C31 C32 -58.8(11) . . . . ? C51 P1 C31 C32 -161.6(10) . . . . ? Ru P1 C31 C32 70.9(11) . . . . ? C41 P1 C31 C36 117.7(11) . . . . ? C51 P1 C31 C36 14.9(11) . . . . ? Ru P1 C31 C36 -112.7(10) . . . . ? C36 C31 C32 C33 -1(2) . . . . ? P1 C31 C32 C33 175.3(11) . . . . ? C31 C32 C33 C34 -3(2) . . . . ? C32 C33 C34 C35 7(3) . . . . ? C33 C34 C35 C36 -7(3) . . . . ? C34 C35 C36 C31 3(2) . . . . ? C32 C31 C36 C35 1(2) . . . . ? P1 C31 C36 C35 -175.4(11) . . . . ? C31 P1 C41 C46 -41.4(10) . . . . ? C51 P1 C41 C46 63.3(10) . . . . ? Ru P1 C41 C46 -175.2(8) . . . . ? C31 P1 C41 C42 140.7(9) . . . . ? C51 P1 C41 C42 -114.5(9) . . . . ? Ru P1 C41 C42 6.9(10) . . . . ? C46 C41 C42 C43 0.7(15) . . . . ? P1 C41 C42 C43 178.7(8) . . . . ? C41 C42 C43 C44 -1.2(17) . . . . ? C42 C43 C44 C45 0.4(18) . . . . ? C43 C44 C45 C46 0.9(19) . . . . ? C44 C45 C46 C41 -1(2) . . . . ? C42 C41 C46 C45 0.6(17) . . . . ? P1 C41 C46 C45 -177.4(10) . . . . ? C41 P1 C51 C52 14.9(10) . . . . ? C31 P1 C51 C52 114.6(9) . . . . ? Ru P1 C51 C52 -110.6(8) . . . . ? C41 P1 C51 C56 -173.0(9) . . . . ? C31 P1 C51 C56 -73.2(10) . . . . ? Ru P1 C51 C56 61.6(9) . . . . ? C56 C51 C52 C53 2.7(16) . . . . ? P1 C51 C52 C53 175.0(9) . . . . ? C51 C52 C53 C54 0.2(19) . . . . ? C52 C53 C54 C55 -2(2) . . . . ? C53 C54 C55 C56 2(2) . . . . ? C52 C51 C56 C55 -3.5(17) . . . . ? P1 C51 C56 C55 -176.1(10) . . . . ? C54 C55 C56 C51 1(2) . . . . ? C71 P2 C61 C62 -122.8(10) . . . . ? C81 P2 C61 C62 -23.1(11) . . . . ? Ru P2 C61 C62 100.0(10) . . . . ? C71 P2 C61 C66 66.7(9) . . . . ? C81 P2 C61 C66 166.3(8) . . . . ? Ru P2 C61 C66 -70.6(8) . . . . ? C66 C61 C62 C63 0.5(17) . . . . ? P2 C61 C62 C63 -170.4(11) . . . . ? C61 C62 C63 C64 -1(2) . . . . ? C62 C63 C64 C65 0(2) . . . . ? C63 C64 C65 C66 0(2) . . . . ? C64 C65 C66 C61 -0.4(19) . . . . ? C62 C61 C66 C65 0.1(16) . . . . ? P2 C61 C66 C65 171.3(9) . . . . ? C61 P2 C71 C72 -7.3(12) . . . . ? C81 P2 C71 C72 -111.5(11) . . . . ? Ru P2 C71 C72 120.4(10) . . . . ? C61 P2 C71 C76 165.6(9) . . . . ? C81 P2 C71 C76 61.4(10) . . . . ? Ru P2 C71 C76 -66.7(10) . . . . ? C76 C71 C72 C73 -1(2) . . . . ? P2 C71 C72 C73 171.3(11) . . . . ? C71 C72 C73 C74 4(2) . . . . ? C72 C73 C74 C75 -6(2) . . . . ? C73 C74 C75 C76 5(2) . . . . ? C74 C75 C76 C71 -2(2) . . . . ? C72 C71 C76 C75 0.2(19) . . . . ? P2 C71 C76 C75 -173.0(10) . . . . ? C61 P2 C81 C82 -56.7(11) . . . . ? C71 P2 C81 C82 49.3(11) . . . . ? Ru P2 C81 C82 -175.5(9) . . . . ? C61 P2 C81 C86 126.8(9) . . . . ? C71 P2 C81 C86 -127.2(10) . . . . ? Ru P2 C81 C86 8.0(11) . . . . ? C86 C81 C82 C83 -4(2) . . . . ? P2 C81 C82 C83 179.1(13) . . . . ? C81 C82 C83 C84 3(3) . . . . ? C82 C83 C84 C85 0(3) . . . . ? C83 C84 C85 C86 -2(2) . . . . ? C82 C81 C86 C85 2.7(18) . . . . ? P2 C81 C86 C85 179.2(9) . . . . ? C84 C85 C86 C81 1(2) . . . . ? C96 C91 C92 C93 0.0 . . . . ? C91 C92 C93 C94 0.0 . . . . ? C92 C93 C94 C95 0.0 . . . . ? C93 C94 C95 C96 0.0 . . . . ? C94 C95 C96 C91 0.0 . . . . ? C94 C95 C96 C97 157(4) . . . . ? C92 C91 C96 C95 0.0 . . . . ? C92 C91 C96 C97 -157(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.099 _refine_diff_density_min -2.145 _refine_diff_density_rms 0.181 data_erk_954 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H52 N4 O4 Ru' _chemical_formula_weight 705.89 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' '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' '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 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.458(4) _cell_length_b 15.758(3) _cell_length_c 18.019(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.61(2) _cell_angle_gamma 90.00 _cell_volume 3513.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 8.49 _cell_measurement_theta_max 11.29 _exptl_crystal_description 'needle' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.8284 _exptl_absorpt_correction_T_max 0.9760 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 3.2 _diffrn_reflns_number 3194 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.2538 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3090 _reflns_number_gt 1799 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Express (Nonius B.V., 1994)' _computing_cell_refinement 'Express (Nonius B.V., 1994)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL-92 (Keller, 1992)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically, at N from Diff.-Fourier' _refine_ls_hydrogen_treatment 'refined as riding atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3090 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1716 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1261 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _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 0.0000 0.07078(5) 0.2500 0.0228(2) Uani 1 2 d S . . C1 C 0.0287(5) 0.1285(4) 0.1440(3) 0.0282(15) Uani 1 1 d . . . H1 H -0.0111 0.1743 0.1215 0.034 Uiso 1 1 calc R . . C2 C 0.1235(5) 0.1358(4) 0.1947(3) 0.0288(15) Uani 1 1 d . . . H2 H 0.1570 0.1865 0.2124 0.035 Uiso 1 1 calc R . . C3 C 0.1589(5) 0.0525(4) 0.2140(3) 0.0325(16) Uani 1 1 d . . . H3 H 0.2210 0.0382 0.2462 0.039 Uiso 1 1 calc R . . C4 C 0.0839(5) -0.0064(4) 0.1760(3) 0.0264(15) Uani 1 1 d . . . C5 C 0.0028(5) 0.0420(3) 0.1324(3) 0.0207(13) Uani 1 1 d . . . C6 C -0.0948(5) 0.0150(3) 0.0809(3) 0.0245(14) Uani 1 1 d . . . O6 O -0.1161(3) 0.0534(2) 0.0216(2) 0.0366(11) Uani 1 1 d . . . N7 N -0.1533(4) -0.0503(3) 0.1025(3) 0.0295(13) Uani 1 1 d . . . H7 H -0.135(4) -0.065(4) 0.144(3) 0.035 Uiso 1 1 d . . . C8 C -0.2535(4) -0.0827(4) 0.0607(3) 0.0284(14) Uani 1 1 d . . . C81 C -0.3387(5) -0.0135(5) 0.0527(4) 0.064(2) Uani 1 1 d . . . H81A H -0.3482 0.0090 0.1017 0.096 Uiso 1 1 calc R . . H81B H -0.4067 -0.0369 0.0299 0.096 Uiso 1 1 calc R . . H81C H -0.3159 0.0317 0.0215 0.096 Uiso 1 1 calc R . . C82 C -0.2908(6) -0.1566(5) 0.1060(4) 0.055(2) Uani 1 1 d . . . H82A H -0.2360 -0.2006 0.1102 0.083 Uiso 1 1 calc R . . H82B H -0.3578 -0.1793 0.0811 0.083 Uiso 1 1 calc R . . H82C H -0.3021 -0.1369 0.1555 0.083 Uiso 1 1 calc R . . C83 C -0.2301(5) -0.1141(4) -0.0157(3) 0.0484(19) Uani 1 1 d . . . H83A H -0.2067 -0.0669 -0.0444 0.073 Uiso 1 1 calc R . . H83B H -0.2952 -0.1387 -0.0419 0.073 Uiso 1 1 calc R . . H83C H -0.1736 -0.1567 -0.0095 0.073 Uiso 1 1 calc R . . C9 C 0.1009(5) -0.1007(4) 0.1829(3) 0.0279(15) Uani 1 1 d . . . O9 O 0.1296(4) -0.1327(3) 0.2446(2) 0.0525(14) Uani 1 1 d . . . N10 N 0.0897(4) -0.1427(3) 0.1186(3) 0.0275(12) Uani 1 1 d . . . H10 H 0.071(5) -0.120(4) 0.079(3) 0.033 Uiso 1 1 d . . . C11 C 0.1056(5) -0.2346(4) 0.1092(3) 0.0327(16) Uani 1 1 d . . . C111 C 0.0784(6) -0.2547(4) 0.0272(4) 0.059(2) Uani 1 1 d . . . H11A H 0.0937 -0.3140 0.0186 0.089 Uiso 1 1 calc R . . H11B H 0.1218 -0.2194 -0.0019 0.089 Uiso 1 1 calc R . . H11C H 0.0024 -0.2435 0.0124 0.089 Uiso 1 1 calc R . . C112 C 0.0342(9) -0.2837(5) 0.1535(5) 0.113(4) Uani 1 1 d . . . H11D H 0.0691 -0.2906 0.2041 0.169 Uiso 1 1 calc R . . H11E H 0.0203 -0.3391 0.1309 0.169 Uiso 1 1 calc R . . H11F H -0.0336 -0.2537 0.1545 0.169 Uiso 1 1 calc R . . C113 C 0.2232(7) -0.2561(5) 0.1310(5) 0.092(3) Uani 1 1 d . . . H11G H 0.2444 -0.2384 0.1822 0.139 Uiso 1 1 calc R . . H11H H 0.2672 -0.2269 0.0981 0.139 Uiso 1 1 calc R . . H11I H 0.2334 -0.3169 0.1269 0.139 Uiso 1 1 calc R . . C21 C 0.4606(8) 0.0037(7) 0.2239(12) 0.167(12) Uani 1 1 d . . . H21 H 0.4287 0.0554 0.2073 0.201 Uiso 1 1 calc R . . C22 C 0.4235(9) -0.0683(8) 0.1930(7) 0.129(4) Uani 1 1 d . . . H22 H 0.3716 -0.0678 0.1508 0.155 Uiso 1 1 calc R . . C23 C 0.4639(8) -0.1470(6) 0.2250(8) 0.112(6) Uani 1 1 d . . . H23 H 0.4338 -0.1986 0.2067 0.135 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 0.0310(4) 0.0215(4) 0.0161(4) 0.000 0.0030(3) 0.000 C1 0.046(4) 0.027(4) 0.011(3) 0.011(3) 0.003(3) -0.001(3) C2 0.032(4) 0.027(4) 0.028(4) -0.005(3) 0.006(3) -0.014(3) C3 0.038(4) 0.042(5) 0.018(3) 0.002(3) 0.005(3) 0.005(3) C4 0.037(4) 0.024(3) 0.021(4) -0.005(3) 0.013(3) 0.003(3) C5 0.030(3) 0.021(3) 0.012(3) 0.002(2) 0.007(2) -0.003(3) C6 0.039(4) 0.022(3) 0.012(3) -0.003(3) -0.001(3) 0.003(3) O6 0.047(3) 0.037(3) 0.023(2) 0.009(2) -0.0090(19) -0.008(2) N7 0.041(3) 0.030(3) 0.017(3) 0.003(2) -0.002(2) -0.008(2) C8 0.030(3) 0.031(4) 0.024(3) -0.005(3) -0.001(3) -0.006(3) C81 0.038(4) 0.069(6) 0.084(6) -0.013(5) -0.004(4) 0.005(4) C82 0.054(5) 0.066(5) 0.044(5) -0.002(4) 0.004(4) -0.029(4) C83 0.052(5) 0.061(5) 0.032(4) -0.015(4) 0.004(3) -0.015(4) C9 0.034(4) 0.032(4) 0.019(3) 0.006(3) 0.005(3) 0.008(3) O9 0.092(4) 0.044(3) 0.021(3) 0.006(2) 0.002(2) 0.029(3) N10 0.042(3) 0.027(3) 0.013(3) 0.002(2) 0.003(2) 0.007(2) C11 0.052(5) 0.022(3) 0.025(3) 0.002(3) 0.012(3) 0.007(3) C111 0.103(6) 0.030(4) 0.041(4) -0.013(3) -0.006(4) 0.016(4) C112 0.212(12) 0.034(5) 0.115(8) -0.009(5) 0.115(8) -0.034(6) C113 0.102(8) 0.080(7) 0.086(7) -0.028(5) -0.028(6) 0.055(6) C21 0.105(14) 0.059(6) 0.37(4) 0.080(13) 0.17(2) 0.035(7) C22 0.119(9) 0.088(8) 0.197(13) 0.019(12) 0.087(8) 0.014(9) C23 0.084(12) 0.078(7) 0.19(2) -0.047(9) 0.082(11) -0.032(6) _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 C4 2.160(6) . ? Ru C4 2.160(6) 2 ? Ru C5 2.172(5) . ? Ru C5 2.172(5) 2 ? Ru C3 2.172(6) . ? Ru C3 2.172(6) 2 ? Ru C1 2.182(5) 2 ? Ru C1 2.182(5) . ? Ru C2 2.182(6) . ? Ru C2 2.182(6) 2 ? C1 C5 1.411(7) . ? C1 C2 1.412(8) . ? C2 C3 1.415(8) . ? C3 C4 1.433(8) . ? C4 C5 1.428(7) . ? C4 C9 1.505(8) . ? C5 C6 1.503(7) . ? C6 O6 1.230(6) . ? C6 N7 1.344(7) . ? N7 C8 1.473(7) . ? C8 C81 1.517(9) . ? C8 C83 1.523(7) . ? C8 C82 1.525(8) . ? C9 O9 1.236(6) . ? C9 N10 1.328(7) . ? N10 C11 1.475(7) . ? C11 C112 1.480(9) . ? C11 C111 1.510(8) . ? C11 C113 1.511(9) . ? C21 C21 1.28(4) 2_655 ? C21 C22 1.323(17) . ? C22 C23 1.434(14) . ? C23 C23 1.20(2) 2_655 ? 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 C4 Ru C4 111.5(3) . 2 ? C4 Ru C5 38.5(2) . . ? C4 Ru C5 123.2(2) 2 . ? C4 Ru C5 123.2(2) . 2 ? C4 Ru C5 38.5(2) 2 2 ? C5 Ru C5 155.9(3) . 2 ? C4 Ru C3 38.6(2) . . ? C4 Ru C3 129.2(2) 2 . ? C5 Ru C3 64.1(2) . . ? C5 Ru C3 112.4(2) 2 . ? C4 Ru C3 129.2(2) . 2 ? C4 Ru C3 38.6(2) 2 2 ? C5 Ru C3 112.4(2) . 2 ? C5 Ru C3 64.1(2) 2 2 ? C3 Ru C3 164.8(3) . 2 ? C4 Ru C1 156.1(2) . 2 ? C4 Ru C1 63.6(2) 2 2 ? C5 Ru C1 164.6(2) . 2 ? C5 Ru C1 37.8(2) 2 2 ? C3 Ru C1 124.3(2) . 2 ? C3 Ru C1 63.1(2) 2 2 ? C4 Ru C1 63.6(2) . . ? C4 Ru C1 156.1(2) 2 . ? C5 Ru C1 37.8(2) . . ? C5 Ru C1 164.6(2) 2 . ? C3 Ru C1 63.1(2) . . ? C3 Ru C1 124.3(2) 2 . ? C1 Ru C1 130.7(3) 2 . ? C4 Ru C2 64.3(2) . . ? C4 Ru C2 164.2(2) 2 . ? C5 Ru C2 64.0(2) . . ? C5 Ru C2 129.4(2) 2 . ? C3 Ru C2 37.9(2) . . ? C3 Ru C2 156.0(2) 2 . ? C1 Ru C2 113.5(2) 2 . ? C1 Ru C2 37.8(2) . . ? C4 Ru C2 164.2(2) . 2 ? C4 Ru C2 64.3(2) 2 2 ? C5 Ru C2 129.4(2) . 2 ? C5 Ru C2 64.0(2) 2 2 ? C3 Ru C2 156.0(2) . 2 ? C3 Ru C2 37.9(2) 2 2 ? C1 Ru C2 37.8(2) 2 2 ? C1 Ru C2 113.5(2) . 2 ? C2 Ru C2 124.0(3) . 2 ? C5 C1 C2 109.5(5) . . ? C5 C1 Ru 70.7(3) . . ? C2 C1 Ru 71.1(3) . . ? C1 C2 C3 107.3(5) . . ? C1 C2 Ru 71.1(3) . . ? C3 C2 Ru 70.6(3) . . ? C2 C3 C4 108.4(5) . . ? C2 C3 Ru 71.4(3) . . ? C4 C3 Ru 70.3(3) . . ? C5 C4 C3 107.4(5) . . ? C5 C4 C9 131.1(6) . . ? C3 C4 C9 121.5(5) . . ? C5 C4 Ru 71.2(3) . . ? C3 C4 Ru 71.1(3) . . ? C9 C4 Ru 125.4(4) . . ? C1 C5 C4 107.4(5) . . ? C1 C5 C6 121.4(5) . . ? C4 C5 C6 131.2(5) . . ? C1 C5 Ru 71.5(3) . . ? C4 C5 Ru 70.3(3) . . ? C6 C5 Ru 123.9(4) . . ? O6 C6 N7 123.9(5) . . ? O6 C6 C5 118.3(5) . . ? N7 C6 C5 117.8(5) . . ? C6 N7 C8 125.0(5) . . ? N7 C8 C81 110.0(5) . . ? N7 C8 C83 109.6(5) . . ? C81 C8 C83 110.7(5) . . ? N7 C8 C82 106.4(5) . . ? C81 C8 C82 110.3(5) . . ? C83 C8 C82 109.7(5) . . ? O9 C9 N10 124.9(6) . . ? O9 C9 C4 120.1(5) . . ? N10 C9 C4 114.9(5) . . ? C9 N10 C11 126.0(5) . . ? N10 C11 C112 110.8(5) . . ? N10 C11 C111 107.4(5) . . ? C112 C11 C111 109.7(6) . . ? N10 C11 C113 109.2(6) . . ? C112 C11 C113 111.6(7) . . ? C111 C11 C113 108.0(6) . . ? C21 C21 C22 120.7(8) 2_655 . ? C21 C22 C23 118.8(13) . . ? C23 C23 C22 120.1(7) 2_655 . ? 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 C4 Ru C1 C5 38.2(3) . . . . ? C4 Ru C1 C5 -45.4(7) 2 . . . ? C5 Ru C1 C5 158.2(6) 2 . . . ? C3 Ru C1 C5 81.7(4) . . . . ? C3 Ru C1 C5 -82.8(4) 2 . . . ? C1 Ru C1 C5 -164.9(4) 2 . . . ? C2 Ru C1 C5 119.6(5) . . . . ? C2 Ru C1 C5 -124.6(4) 2 . . . ? C4 Ru C1 C2 -81.4(4) . . . . ? C4 Ru C1 C2 -165.0(5) 2 . . . ? C5 Ru C1 C2 -119.6(5) . . . . ? C5 Ru C1 C2 38.6(10) 2 . . . ? C3 Ru C1 C2 -37.9(3) . . . . ? C3 Ru C1 C2 157.6(4) 2 . . . ? C1 Ru C1 C2 75.5(3) 2 . . . ? C2 Ru C1 C2 115.8(4) 2 . . . ? C5 C1 C2 C3 1.2(7) . . . . ? Ru C1 C2 C3 61.7(4) . . . . ? C5 C1 C2 Ru -60.6(4) . . . . ? C4 Ru C2 C1 79.4(4) . . . . ? C4 Ru C2 C1 157.4(7) 2 . . . ? C5 Ru C2 C1 36.4(3) . . . . ? C5 Ru C2 C1 -167.6(3) 2 . . . ? C3 Ru C2 C1 117.0(5) . . . . ? C3 Ru C2 C1 -50.5(7) 2 . . . ? C1 Ru C2 C1 -126.8(4) 2 . . . ? C2 Ru C2 C1 -85.1(3) 2 . . . ? C4 Ru C2 C3 -37.6(3) . . . . ? C4 Ru C2 C3 40.4(10) 2 . . . ? C5 Ru C2 C3 -80.6(4) . . . . ? C5 Ru C2 C3 75.4(4) 2 . . . ? C3 Ru C2 C3 -167.5(3) 2 . . . ? C1 Ru C2 C3 116.2(4) 2 . . . ? C1 Ru C2 C3 -117.0(5) . . . . ? C2 Ru C2 C3 157.9(4) 2 . . . ? C1 C2 C3 C4 -1.2(6) . . . . ? Ru C2 C3 C4 60.8(4) . . . . ? C1 C2 C3 Ru -62.0(4) . . . . ? C4 Ru C3 C2 118.3(5) . . . . ? C4 Ru C3 C2 -166.9(3) 2 . . . ? C5 Ru C3 C2 80.2(3) . . . . ? C5 Ru C3 C2 -126.0(3) 2 . . . ? C3 Ru C3 C2 160.4(3) 2 . . . ? C1 Ru C3 C2 -84.9(4) 2 . . . ? C1 Ru C3 C2 37.8(3) . . . . ? C2 Ru C3 C2 -49.9(8) 2 . . . ? C4 Ru C3 C4 74.8(5) 2 . . . ? C5 Ru C3 C4 -38.2(3) . . . . ? C5 Ru C3 C4 115.7(4) 2 . . . ? C3 Ru C3 C4 42.1(3) 2 . . . ? C1 Ru C3 C4 156.8(3) 2 . . . ? C1 Ru C3 C4 -80.6(4) . . . . ? C2 Ru C3 C4 -118.3(5) . . . . ? C2 Ru C3 C4 -168.2(5) 2 . . . ? C2 C3 C4 C5 0.8(6) . . . . ? Ru C3 C4 C5 62.3(4) . . . . ? C2 C3 C4 C9 177.9(5) . . . . ? Ru C3 C4 C9 -120.5(6) . . . . ? C2 C3 C4 Ru -61.6(4) . . . . ? C4 Ru C4 C5 116.8(4) 2 . . . ? C5 Ru C4 C5 158.4(3) 2 . . . ? C3 Ru C4 C5 -116.7(5) . . . . ? C3 Ru C4 C5 76.4(4) 2 . . . ? C1 Ru C4 C5 -170.1(5) 2 . . . ? C1 Ru C4 C5 -37.6(3) . . . . ? C2 Ru C4 C5 -79.8(4) . . . . ? C2 Ru C4 C5 45.5(10) 2 . . . ? C4 Ru C4 C3 -126.5(4) 2 . . . ? C5 Ru C4 C3 116.7(5) . . . . ? C5 Ru C4 C3 -84.9(4) 2 . . . ? C3 Ru C4 C3 -166.8(3) 2 . . . ? C1 Ru C4 C3 -53.4(7) 2 . . . ? C1 Ru C4 C3 79.1(4) . . . . ? C2 Ru C4 C3 36.9(3) . . . . ? C2 Ru C4 C3 162.2(8) 2 . . . ? C4 Ru C4 C9 -10.8(4) 2 . . . ? C5 Ru C4 C9 -127.6(7) . . . . ? C5 Ru C4 C9 30.8(6) 2 . . . ? C3 Ru C4 C9 115.7(7) . . . . ? C3 Ru C4 C9 -51.1(6) 2 . . . ? C1 Ru C4 C9 62.3(8) 2 . . . ? C1 Ru C4 C9 -165.1(6) . . . . ? C2 Ru C4 C9 152.6(6) . . . . ? C2 Ru C4 C9 -82.0(10) 2 . . . ? C2 C1 C5 C4 -0.7(7) . . . . ? Ru C1 C5 C4 -61.5(4) . . . . ? C2 C1 C5 C6 179.9(5) . . . . ? Ru C1 C5 C6 119.0(5) . . . . ? C2 C1 C5 Ru 60.8(4) . . . . ? C3 C4 C5 C1 0.0(6) . . . . ? C9 C4 C5 C1 -176.8(6) . . . . ? Ru C4 C5 C1 62.3(4) . . . . ? C3 C4 C5 C6 179.3(5) . . . . ? C9 C4 C5 C6 2.6(10) . . . . ? Ru C4 C5 C6 -118.4(6) . . . . ? C3 C4 C5 Ru -62.3(4) . . . . ? C9 C4 C5 Ru 120.9(7) . . . . ? C4 Ru C5 C1 -117.0(5) . . . . ? C4 Ru C5 C1 159.8(3) 2 . . . ? C5 Ru C5 C1 -166.0(4) 2 . . . ? C3 Ru C5 C1 -78.7(4) . . . . ? C3 Ru C5 C1 117.6(4) 2 . . . ? C1 Ru C5 C1 47.9(12) 2 . . . ? C2 Ru C5 C1 -36.3(4) . . . . ? C2 Ru C5 C1 77.5(4) 2 . . . ? C4 Ru C5 C4 -83.1(5) 2 . . . ? C5 Ru C5 C4 -49.0(3) 2 . . . ? C3 Ru C5 C4 38.3(3) . . . . ? C3 Ru C5 C4 -125.4(4) 2 . . . ? C1 Ru C5 C4 164.9(8) 2 . . . ? C1 Ru C5 C4 117.0(5) . . . . ? C2 Ru C5 C4 80.7(4) . . . . ? C2 Ru C5 C4 -165.5(3) 2 . . . ? C4 Ru C5 C6 127.1(6) . . . . ? C4 Ru C5 C6 44.0(5) 2 . . . ? C5 Ru C5 C6 78.1(4) 2 . . . ? C3 Ru C5 C6 165.4(5) . . . . ? C3 Ru C5 C6 1.7(5) 2 . . . ? C1 Ru C5 C6 -68.0(10) 2 . . . ? C1 Ru C5 C6 -115.9(6) . . . . ? C2 Ru C5 C6 -152.2(5) . . . . ? C2 Ru C5 C6 -38.4(5) 2 . . . ? C1 C5 C6 O6 40.6(8) . . . . ? C4 C5 C6 O6 -138.6(6) . . . . ? Ru C5 C6 O6 128.5(5) . . . . ? C1 C5 C6 N7 -139.8(6) . . . . ? C4 C5 C6 N7 40.9(9) . . . . ? Ru C5 C6 N7 -52.0(7) . . . . ? O6 C6 N7 C8 -3.2(9) . . . . ? C5 C6 N7 C8 177.2(5) . . . . ? C6 N7 C8 C81 -60.6(7) . . . . ? C6 N7 C8 C83 61.3(7) . . . . ? C6 N7 C8 C82 179.9(5) . . . . ? C5 C4 C9 O9 -139.7(6) . . . . ? C3 C4 C9 O9 43.9(9) . . . . ? Ru C4 C9 O9 -44.3(8) . . . . ? C5 C4 C9 N10 44.5(9) . . . . ? C3 C4 C9 N10 -131.9(6) . . . . ? Ru C4 C9 N10 139.9(5) . . . . ? O9 C9 N10 C11 2.2(10) . . . . ? C4 C9 N10 C11 177.8(5) . . . . ? C9 N10 C11 C112 57.2(9) . . . . ? C9 N10 C11 C111 177.0(6) . . . . ? C9 N10 C11 C113 -66.0(8) . . . . ? C21 C21 C22 C23 8(3) 2_655 . . . ? C21 C22 C23 C23 -6(2) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.480 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.110 data_erk1128 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H46 Fe N4 O4' _chemical_formula_weight 582.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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 6.793(1) _cell_length_b 10.902(1) _cell_length_c 11.208(1) _cell_angle_alpha 92.05(1) _cell_angle_beta 99.78(1) _cell_angle_gamma 107.58(1) _cell_volume 776.41(15) _cell_formula_units_Z 1 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow-orange' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 312 _exptl_absorpt_coefficient_mu 0.524 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.8377 _exptl_absorpt_correction_T_max 0.9494 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6015 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.55 _reflns_number_total 3538 _reflns_number_gt 3309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL-92 (Keller, 1992)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.3959P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically, at N from Diff.-Fourier' _refine_ls_hydrogen_treatment 'refined as riding atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3538 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Fe Fe 0.0000 0.0000 0.0000 0.02325(11) Uani 1 2 d S . . C1 C 0.2884(2) 0.07236(15) -0.04440(13) 0.0242(3) Uani 1 1 d . . . C2 C 0.2249(2) -0.06720(15) -0.05167(14) 0.0244(3) Uani 1 1 d . . . C3 C 0.1925(2) -0.10384(17) 0.06664(14) 0.0275(3) Uani 1 1 d . . . H3 H 0.1501 -0.1900 0.0885 0.033 Uiso 1 1 calc R . . C4 C 0.2335(2) 0.00852(18) 0.14568(14) 0.0294(3) Uani 1 1 d . . . H4 H 0.2223 0.0109 0.2290 0.035 Uiso 1 1 calc R . . C5 C 0.2944(2) 0.11717(17) 0.07854(14) 0.0274(3) Uani 1 1 d . . . H5 H 0.3328 0.2050 0.1098 0.033 Uiso 1 1 calc R . . C10 C 0.3302(2) 0.15925(16) -0.14363(14) 0.0261(3) Uani 1 1 d . . . O11 O 0.2317(2) 0.12735(12) -0.24944(10) 0.0353(3) Uani 1 1 d . . . N12 N 0.4775(2) 0.27405(14) -0.10779(12) 0.0277(3) Uani 1 1 d . . . H12 H 0.553(3) 0.281(2) -0.039(2) 0.033 Uiso 1 1 d . . . C13 C 0.5455(3) 0.37617(17) -0.18908(16) 0.0365(4) Uani 1 1 d . . . C14 C 0.3600(4) 0.4209(2) -0.2430(2) 0.0567(6) Uani 1 1 d . . . H14A H 0.2466 0.3473 -0.2884 0.085 Uiso 1 1 calc R . . H14B H 0.4050 0.4875 -0.2980 0.085 Uiso 1 1 calc R . . H14C H 0.3092 0.4568 -0.1774 0.085 Uiso 1 1 calc R . . C15 C 0.6348(4) 0.3261(2) -0.2902(2) 0.0553(6) Uani 1 1 d . . . H15A H 0.7587 0.3024 -0.2544 0.083 Uiso 1 1 calc R . . H15B H 0.6752 0.3939 -0.3447 0.083 Uiso 1 1 calc R . . H15C H 0.5279 0.2501 -0.3364 0.083 Uiso 1 1 calc R . . C16 C 0.7158(4) 0.4876(2) -0.11011(19) 0.0511(5) Uani 1 1 d . . . H16A H 0.6574 0.5190 -0.0456 0.077 Uiso 1 1 calc R . . H16B H 0.7670 0.5578 -0.1603 0.077 Uiso 1 1 calc R . . H16C H 0.8326 0.4575 -0.0737 0.077 Uiso 1 1 calc R . . C20 C 0.2016(2) -0.16858(16) -0.15186(14) 0.0260(3) Uani 1 1 d . . . O21 O 0.2144(2) -0.27546(12) -0.12443(11) 0.0332(3) Uani 1 1 d . . . N22 N 0.1685(2) -0.13576(15) -0.26554(12) 0.0317(3) Uani 1 1 d . . . H22 H 0.167(3) -0.057(2) -0.2747(19) 0.038 Uiso 1 1 d . . . C23 C 0.1535(3) -0.21761(18) -0.37716(15) 0.0345(4) Uani 1 1 d . . . C24 C 0.3595(4) -0.2473(2) -0.37502(18) 0.0510(5) Uani 1 1 d . . . H24A H 0.4735 -0.1666 -0.3746 0.076 Uiso 1 1 calc R . . H24B H 0.3464 -0.3046 -0.4473 0.076 Uiso 1 1 calc R . . H24C H 0.3908 -0.2898 -0.3018 0.076 Uiso 1 1 calc R . . C25 C 0.1165(5) -0.1386(2) -0.48307(18) 0.0583(6) Uani 1 1 d . . . H25A H -0.0177 -0.1216 -0.4856 0.087 Uiso 1 1 calc R . . H25B H 0.1125 -0.1870 -0.5593 0.087 Uiso 1 1 calc R . . H25C H 0.2309 -0.0565 -0.4725 0.087 Uiso 1 1 calc R . . C26 C -0.0282(4) -0.3425(2) -0.3879(2) 0.0594(6) Uani 1 1 d . . . H26A H -0.0003 -0.3932 -0.3203 0.089 Uiso 1 1 calc R . . H26B H -0.0427 -0.3925 -0.4651 0.089 Uiso 1 1 calc R . . H26C H -0.1585 -0.3223 -0.3853 0.089 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 Fe 0.01935(16) 0.02829(18) 0.02375(16) 0.00156(11) 0.00438(11) 0.00979(12) C1 0.0182(7) 0.0276(8) 0.0268(7) 0.0010(6) 0.0042(5) 0.0074(6) C2 0.0204(7) 0.0283(8) 0.0274(7) 0.0043(6) 0.0050(5) 0.0113(6) C3 0.0235(7) 0.0342(9) 0.0286(7) 0.0074(6) 0.0056(6) 0.0138(6) C4 0.0240(7) 0.0413(10) 0.0238(7) 0.0035(6) 0.0026(6) 0.0127(7) C5 0.0213(7) 0.0335(9) 0.0263(7) -0.0016(6) 0.0022(6) 0.0085(6) C10 0.0269(8) 0.0268(8) 0.0274(7) 0.0031(6) 0.0060(6) 0.0119(6) O11 0.0437(7) 0.0306(7) 0.0269(6) 0.0018(5) -0.0018(5) 0.0092(5) N12 0.0294(7) 0.0281(7) 0.0251(6) 0.0043(5) 0.0049(5) 0.0082(5) C13 0.0507(11) 0.0269(9) 0.0305(8) 0.0050(7) 0.0110(7) 0.0082(7) C14 0.0824(17) 0.0404(12) 0.0485(12) 0.0120(9) -0.0007(11) 0.0274(12) C15 0.0831(17) 0.0429(12) 0.0425(11) 0.0081(9) 0.0344(11) 0.0108(11) C16 0.0608(13) 0.0371(11) 0.0426(11) 0.0023(8) 0.0153(9) -0.0062(9) C20 0.0216(7) 0.0267(8) 0.0302(8) 0.0024(6) 0.0055(6) 0.0080(6) O21 0.0400(7) 0.0264(6) 0.0333(6) 0.0038(5) 0.0060(5) 0.0109(5) N22 0.0424(8) 0.0284(8) 0.0276(7) 0.0009(6) 0.0044(6) 0.0173(6) C23 0.0461(10) 0.0307(9) 0.0260(8) -0.0014(6) 0.0027(7) 0.0136(7) C24 0.0637(14) 0.0636(15) 0.0346(10) -0.0055(9) 0.0096(9) 0.0341(12) C25 0.0997(19) 0.0516(14) 0.0296(9) 0.0028(9) 0.0022(10) 0.0379(13) C26 0.0627(15) 0.0498(14) 0.0479(12) -0.0107(10) 0.0010(10) -0.0019(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C1 2.0332(15) 2 ? Fe C1 2.0332(15) . ? Fe C2 2.0381(15) . ? Fe C2 2.0381(15) 2 ? Fe C3 2.0426(15) . ? Fe C3 2.0426(15) 2 ? Fe C5 2.0455(16) . ? Fe C5 2.0455(16) 2 ? Fe C4 2.0521(15) 2 ? Fe C4 2.0521(15) . ? C1 C5 1.435(2) . ? C1 C2 1.446(2) . ? C1 C10 1.495(2) . ? C2 C3 1.432(2) . ? C2 C20 1.501(2) . ? C3 C4 1.413(2) . ? C4 C5 1.419(2) . ? C10 O11 1.2393(19) . ? C10 N12 1.341(2) . ? N12 C13 1.479(2) . ? C13 C14 1.525(3) . ? C13 C16 1.524(3) . ? C13 C15 1.530(3) . ? C20 O21 1.240(2) . ? C20 N22 1.336(2) . ? N22 C23 1.481(2) . ? C23 C25 1.522(3) . ? C23 C26 1.521(3) . ? C23 C24 1.525(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe C1 180.00(8) 2 . ? C1 Fe C2 138.40(6) 2 . ? C1 Fe C2 41.60(6) . . ? C1 Fe C2 41.60(6) 2 2 ? C1 Fe C2 138.40(6) . 2 ? C2 Fe C2 180.00(8) . 2 ? C1 Fe C3 110.82(6) 2 . ? C1 Fe C3 69.18(6) . . ? C2 Fe C3 41.08(6) . . ? C2 Fe C3 138.92(6) 2 . ? C1 Fe C3 69.18(6) 2 2 ? C1 Fe C3 110.82(6) . 2 ? C2 Fe C3 138.92(6) . 2 ? C2 Fe C3 41.08(6) 2 2 ? C3 Fe C3 180.00(10) . 2 ? C1 Fe C5 138.80(6) 2 . ? C1 Fe C5 41.20(6) . . ? C2 Fe C5 69.19(6) . . ? C2 Fe C5 110.81(6) 2 . ? C3 Fe C5 68.11(7) . . ? C3 Fe C5 111.89(7) 2 . ? C1 Fe C5 41.20(6) 2 2 ? C1 Fe C5 138.80(6) . 2 ? C2 Fe C5 110.81(6) . 2 ? C2 Fe C5 69.19(6) 2 2 ? C3 Fe C5 111.89(7) . 2 ? C3 Fe C5 68.11(7) 2 2 ? C5 Fe C5 180.00(6) . 2 ? C1 Fe C4 69.20(6) 2 2 ? C1 Fe C4 110.80(6) . 2 ? C2 Fe C4 110.95(6) . 2 ? C2 Fe C4 69.05(6) 2 2 ? C3 Fe C4 139.64(7) . 2 ? C3 Fe C4 40.36(7) 2 2 ? C5 Fe C4 139.47(7) . 2 ? C5 Fe C4 40.53(7) 2 2 ? C1 Fe C4 110.80(6) 2 . ? C1 Fe C4 69.20(6) . . ? C2 Fe C4 69.05(6) . . ? C2 Fe C4 110.95(6) 2 . ? C3 Fe C4 40.36(7) . . ? C3 Fe C4 139.64(7) 2 . ? C5 Fe C4 40.53(7) . . ? C5 Fe C4 139.47(7) 2 . ? C4 Fe C4 180.00(11) 2 . ? C5 C1 C2 107.18(14) . . ? C5 C1 C10 123.93(14) . . ? C2 C1 C10 128.81(13) . . ? C5 C1 Fe 69.86(9) . . ? C2 C1 Fe 69.38(8) . . ? C10 C1 Fe 123.36(10) . . ? C3 C2 C1 107.03(13) . . ? C3 C2 C20 120.02(14) . . ? C1 C2 C20 132.86(14) . . ? C3 C2 Fe 69.63(9) . . ? C1 C2 Fe 69.02(8) . . ? C20 C2 Fe 128.80(11) . . ? C4 C3 C2 109.17(15) . . ? C4 C3 Fe 70.18(9) . . ? C2 C3 Fe 69.29(9) . . ? C3 C4 C5 107.88(14) . . ? C3 C4 Fe 69.46(9) . . ? C5 C4 Fe 69.49(9) . . ? C4 C5 C1 108.73(14) . . ? C4 C5 Fe 69.99(9) . . ? C1 C5 Fe 68.94(9) . . ? O11 C10 N12 123.52(15) . . ? O11 C10 C1 121.85(14) . . ? N12 C10 C1 114.61(13) . . ? C10 N12 C13 124.60(14) . . ? N12 C13 C14 109.69(17) . . ? N12 C13 C16 106.38(14) . . ? C14 C13 C16 109.86(18) . . ? N12 C13 C15 110.39(15) . . ? C14 C13 C15 110.45(18) . . ? C16 C13 C15 110.00(18) . . ? O21 C20 N22 124.69(15) . . ? O21 C20 C2 118.65(14) . . ? N22 C20 C2 116.66(14) . . ? C20 N22 C23 125.66(15) . . ? N22 C23 C25 106.18(15) . . ? N22 C23 C26 110.49(17) . . ? C25 C23 C26 110.48(19) . . ? N22 C23 C24 109.85(15) . . ? C25 C23 C24 109.59(19) . . ? C26 C23 C24 110.17(19) . . ? 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 C1 Fe C1 C5 76(100) 2 . . . ? C2 Fe C1 C5 -118.30(13) . . . . ? C2 Fe C1 C5 61.70(13) 2 . . . ? C3 Fe C1 C5 -80.14(10) . . . . ? C3 Fe C1 C5 99.86(10) 2 . . . ? C5 Fe C1 C5 180.0 2 . . . ? C4 Fe C1 C5 143.17(10) 2 . . . ? C4 Fe C1 C5 -36.83(10) . . . . ? C1 Fe C1 C2 -165(100) 2 . . . ? C2 Fe C1 C2 180.0 2 . . . ? C3 Fe C1 C2 38.17(9) . . . . ? C3 Fe C1 C2 -141.83(9) 2 . . . ? C5 Fe C1 C2 118.30(13) . . . . ? C5 Fe C1 C2 -61.70(13) 2 . . . ? C4 Fe C1 C2 -98.52(10) 2 . . . ? C4 Fe C1 C2 81.48(10) . . . . ? C1 Fe C1 C10 -42(100) 2 . . . ? C2 Fe C1 C10 123.64(16) . . . . ? C2 Fe C1 C10 -56.36(16) 2 . . . ? C3 Fe C1 C10 161.80(14) . . . . ? C3 Fe C1 C10 -18.20(14) 2 . . . ? C5 Fe C1 C10 -118.06(17) . . . . ? C5 Fe C1 C10 61.94(17) 2 . . . ? C4 Fe C1 C10 25.12(14) 2 . . . ? C4 Fe C1 C10 -154.88(14) . . . . ? C5 C1 C2 C3 0.40(16) . . . . ? C10 C1 C2 C3 -176.34(14) . . . . ? Fe C1 C2 C3 -59.51(10) . . . . ? C5 C1 C2 C20 -176.07(15) . . . . ? C10 C1 C2 C20 7.2(3) . . . . ? Fe C1 C2 C20 124.03(17) . . . . ? C5 C1 C2 Fe 59.90(10) . . . . ? C10 C1 C2 Fe -116.83(15) . . . . ? C1 Fe C2 C3 -61.51(13) 2 . . . ? C1 Fe C2 C3 118.49(13) . . . . ? C2 Fe C2 C3 -160(100) 2 . . . ? C3 Fe C2 C3 180.0 2 . . . ? C5 Fe C2 C3 80.14(10) . . . . ? C5 Fe C2 C3 -99.86(10) 2 . . . ? C4 Fe C2 C3 -143.37(10) 2 . . . ? C4 Fe C2 C3 36.63(10) . . . . ? C1 Fe C2 C1 180.0 2 . . . ? C2 Fe C2 C1 82(100) 2 . . . ? C3 Fe C2 C1 -118.49(13) . . . . ? C3 Fe C2 C1 61.51(13) 2 . . . ? C5 Fe C2 C1 -38.35(9) . . . . ? C5 Fe C2 C1 141.65(9) 2 . . . ? C4 Fe C2 C1 98.14(10) 2 . . . ? C4 Fe C2 C1 -81.86(10) . . . . ? C1 Fe C2 C20 51.22(18) 2 . . . ? C1 Fe C2 C20 -128.78(18) . . . . ? C2 Fe C2 C20 -47(100) 2 . . . ? C3 Fe C2 C20 112.72(18) . . . . ? C3 Fe C2 C20 -67.28(18) 2 . . . ? C5 Fe C2 C20 -167.13(16) . . . . ? C5 Fe C2 C20 12.87(16) 2 . . . ? C4 Fe C2 C20 -30.64(16) 2 . . . ? C4 Fe C2 C20 149.36(16) . . . . ? C1 C2 C3 C4 0.13(17) . . . . ? C20 C2 C3 C4 177.14(13) . . . . ? Fe C2 C3 C4 -58.99(11) . . . . ? C1 C2 C3 Fe 59.12(10) . . . . ? C20 C2 C3 Fe -123.87(13) . . . . ? C1 Fe C3 C4 -98.00(10) 2 . . . ? C1 Fe C3 C4 82.00(10) . . . . ? C2 Fe C3 C4 120.63(14) . . . . ? C2 Fe C3 C4 -59.37(14) 2 . . . ? C3 Fe C3 C4 75(100) 2 . . . ? C5 Fe C3 C4 37.61(9) . . . . ? C5 Fe C3 C4 -142.39(9) 2 . . . ? C4 Fe C3 C4 180.0 2 . . . ? C1 Fe C3 C2 141.37(9) 2 . . . ? C1 Fe C3 C2 -38.63(9) . . . . ? C2 Fe C3 C2 180.0 2 . . . ? C3 Fe C3 C2 -46(100) 2 . . . ? C5 Fe C3 C2 -83.01(10) . . . . ? C5 Fe C3 C2 96.99(10) 2 . . . ? C4 Fe C3 C2 59.37(14) 2 . . . ? C4 Fe C3 C2 -120.63(14) . . . . ? C2 C3 C4 C5 -0.62(17) . . . . ? Fe C3 C4 C5 -59.06(11) . . . . ? C2 C3 C4 Fe 58.45(11) . . . . ? C1 Fe C4 C3 98.06(10) 2 . . . ? C1 Fe C4 C3 -81.94(10) . . . . ? C2 Fe C4 C3 -37.27(9) . . . . ? C2 Fe C4 C3 142.73(9) 2 . . . ? C3 Fe C4 C3 180.0 2 . . . ? C5 Fe C4 C3 -119.36(13) . . . . ? C5 Fe C4 C3 60.64(13) 2 . . . ? C4 Fe C4 C3 11(100) 2 . . . ? C1 Fe C4 C5 -142.58(9) 2 . . . ? C1 Fe C4 C5 37.42(9) . . . . ? C2 Fe C4 C5 82.10(10) . . . . ? C2 Fe C4 C5 -97.90(10) 2 . . . ? C3 Fe C4 C5 119.36(13) . . . . ? C3 Fe C4 C5 -60.64(13) 2 . . . ? C5 Fe C4 C5 180.0 2 . . . ? C4 Fe C4 C5 130(100) 2 . . . ? C3 C4 C5 C1 0.87(17) . . . . ? Fe C4 C5 C1 -58.18(10) . . . . ? C3 C4 C5 Fe 59.04(11) . . . . ? C2 C1 C5 C4 -0.78(17) . . . . ? C10 C1 C5 C4 176.15(13) . . . . ? Fe C1 C5 C4 58.82(11) . . . . ? C2 C1 C5 Fe -59.60(10) . . . . ? C10 C1 C5 Fe 117.33(14) . . . . ? C1 Fe C5 C4 59.58(13) 2 . . . ? C1 Fe C5 C4 -120.42(13) . . . . ? C2 Fe C5 C4 -81.71(10) . . . . ? C2 Fe C5 C4 98.29(10) 2 . . . ? C3 Fe C5 C4 -37.46(9) . . . . ? C3 Fe C5 C4 142.54(9) 2 . . . ? C5 Fe C5 C4 177(100) 2 . . . ? C4 Fe C5 C4 180.0 2 . . . ? C1 Fe C5 C1 180.0 2 . . . ? C2 Fe C5 C1 38.71(9) . . . . ? C2 Fe C5 C1 -141.29(9) 2 . . . ? C3 Fe C5 C1 82.96(10) . . . . ? C3 Fe C5 C1 -97.04(10) 2 . . . ? C5 Fe C5 C1 -62(81) 2 . . . ? C4 Fe C5 C1 -59.58(13) 2 . . . ? C4 Fe C5 C1 120.42(13) . . . . ? C5 C1 C10 O11 -143.03(16) . . . . ? C2 C1 C10 O11 33.2(2) . . . . ? Fe C1 C10 O11 -56.1(2) . . . . ? C5 C1 C10 N12 35.3(2) . . . . ? C2 C1 C10 N12 -148.42(15) . . . . ? Fe C1 C10 N12 122.25(13) . . . . ? O11 C10 N12 C13 -1.5(3) . . . . ? C1 C10 N12 C13 -179.83(14) . . . . ? C10 N12 C13 C14 61.9(2) . . . . ? C10 N12 C13 C16 -179.30(17) . . . . ? C10 N12 C13 C15 -60.0(2) . . . . ? C3 C2 C20 O21 -20.4(2) . . . . ? C1 C2 C20 O21 155.70(16) . . . . ? Fe C2 C20 O21 -107.46(16) . . . . ? C3 C2 C20 N22 159.72(15) . . . . ? C1 C2 C20 N22 -24.2(2) . . . . ? Fe C2 C20 N22 72.66(19) . . . . ? O21 C20 N22 C23 -3.6(3) . . . . ? C2 C20 N22 C23 176.24(15) . . . . ? C20 N22 C23 C25 -179.70(19) . . . . ? C20 N22 C23 C26 60.5(2) . . . . ? C20 N22 C23 C24 -61.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.610 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.051