# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1129 data_global #================================================================= # SUBMISSION DETAILS _publ_contact_author ; Dr. Michael Ward School of Chemistry University of Bristol Cantock's Close BS8 1TS Bristol UK ; _publ_contact_author_phone '0117 9287655' _publ_contact_author_fax '0117 9290509' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the two crystal structures in the paper 'A stepwise synthetic strategy for the preparation of trinuclear complexes of bis-terpyridyl bridging ligands containing aza-crown macrocyclic spacer groups' by K. L Bushell, S. M. Couchman, J. C. Jeffery, L. H. Rees and M. D. Ward submitted to Dalton Transactions for publication. ; #================================================================= data_structure1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H71 Cl2 F6 N10 O14 P Ru' _chemical_formula_weight 1437.18 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'F' 'F' 0.0171 0.0103 '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 8.357(4) _cell_length_b 17.697(5) _cell_length_c 22.442(8) _cell_angle_alpha 76.16(3) _cell_angle_beta 87.85(2) _cell_angle_gamma 81.87(2) _cell_volume 3190(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 0.443 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _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 16835 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.1011 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 20.00 _reflns_number_total 5931 _reflns_number_gt 3891 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.2005P)^2^+22.0741P] 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 5931 _refine_ls_number_parameters 840 _refine_ls_number_restraints 270 _refine_ls_R_factor_all 0.1476 _refine_ls_R_factor_gt 0.1044 _refine_ls_wR_factor_ref 0.3185 _refine_ls_wR_factor_gt 0.2820 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 1.458 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.02123(8) -0.13752(4) -0.15486(3) 0.0310(2) Uani 1 1 d U . . P1 P 0.2024(3) 0.29782(16) -0.20961(13) 0.0579(9) Uani 1 1 d U . . F1 F 0.3317(8) 0.3547(4) -0.2250(3) 0.104(2) Uani 1 1 d U . . F2 F 0.1468(12) 0.3334(5) -0.1518(3) 0.136(3) Uani 1 1 d U . . F3 F 0.3279(10) 0.2365(4) -0.1656(4) 0.142(3) Uani 1 1 d U . . F4 F 0.2606(9) 0.2573(4) -0.2618(4) 0.124(2) Uani 1 1 d U . . F5 F 0.0829(10) 0.3550(5) -0.2519(4) 0.140(3) Uani 1 1 d U . . F6 F 0.0765(8) 0.2390(4) -0.1877(3) 0.109(2) Uani 1 1 d U . . Cl1 Cl 0.6942(4) -0.45688(17) -0.12979(13) 0.0853(11) Uani 1 1 d U . . O11 O 0.7692(12) -0.5311(5) -0.1398(5) 0.129(3) Uani 1 1 d U . . O12 O 0.8250(13) -0.4059(6) -0.1512(7) 0.168(4) Uani 1 1 d U . . O13 O 0.6018(14) -0.4704(9) -0.0750(4) 0.188(5) Uani 1 1 d U . . O14 O 0.5817(10) -0.4285(5) -0.1808(3) 0.088(3) Uani 1 1 d U . . Cl2 Cl -0.2492(3) 0.63098(13) -0.51620(11) 0.0156(7) Uani 0.70 1 d PU . . O21 O -0.2042(9) 0.7050(4) -0.5261(4) 0.048(2) Uani 0.70 1 d PU . . O22 O -0.1194(8) 0.5748(4) -0.4869(3) 0.034(2) Uani 0.70 1 d PU . . O23 O -0.2819(11) 0.6141(6) -0.5705(4) 0.071(3) Uani 0.70 1 d PU . . O24 O -0.3882(9) 0.6284(4) -0.4763(4) 0.038(2) Uani 0.70 1 d PU . . O1 O 0.1404(13) 0.5053(5) -0.1807(5) 0.128(4) Uani 1 1 d . . . C4 C 0.6988(16) 0.2836(6) -0.1570(6) 0.096(4) Uani 1 1 d U . . H4A H 0.7995 0.3004 -0.1759 0.144 Uiso 1 1 calc R . . H4B H 0.6715 0.3070 -0.1219 0.144 Uiso 1 1 calc R . . H4C H 0.6114 0.3007 -0.1872 0.144 Uiso 1 1 calc R . . C5 C 0.7191(13) 0.2002(6) -0.1367(5) 0.075(4) Uani 1 1 d U . . N6 N 0.7324(14) 0.1344(6) -0.1237(6) 0.120(5) Uani 1 1 d U . . C7 C 0.347(2) 0.3910(8) -0.0443(6) 0.159(8) Uani 1 1 d U . . H7A H 0.3121 0.4269 -0.0178 0.238 Uiso 1 1 calc R . . H7B H 0.2595 0.3922 -0.0726 0.238 Uiso 1 1 calc R . . H7C H 0.4425 0.4072 -0.0678 0.238 Uiso 1 1 calc R . . C8 C 0.3858(19) 0.3133(7) -0.0076(6) 0.113(5) Uani 1 1 d U . . N9 N 0.4080(17) 0.2518(7) 0.0212(6) 0.131(5) Uani 1 1 d U . . N11 N -0.0600(8) -0.1194(4) -0.0706(3) 0.0352(16) Uani 1 1 d U . . C12 C -0.1294(10) -0.0531(5) -0.0575(4) 0.044(2) Uani 1 1 d U . . H12A H -0.1471 -0.0066 -0.0893 0.053 Uiso 1 1 calc R . . C13 C -0.1768(12) -0.0509(6) 0.0022(4) 0.060(3) Uani 1 1 d U . . H13 H -0.2283 -0.0029 0.0103 0.073 Uiso 1 1 calc R . . C14 C -0.1509(13) -0.1159(6) 0.0492(5) 0.071(3) Uani 1 1 d U . . H14A H -0.1811 -0.1138 0.0901 0.085 Uiso 1 1 calc R . . C15 C -0.0787(13) -0.1854(6) 0.0355(4) 0.064(3) Uani 1 1 d U . . H15A H -0.0628 -0.2326 0.0668 0.077 Uiso 1 1 calc R . . C16 C -0.0312(11) -0.1853(5) -0.0229(4) 0.046(2) Uani 1 1 d U . . N21 N 0.0881(9) -0.2451(4) -0.1010(3) 0.0399(17) Uani 1 1 d U . . C22 C 0.0546(12) -0.2561(5) -0.0416(4) 0.050(2) Uani 1 1 d U . . C23 C 0.1033(15) -0.3294(6) -0.0034(5) 0.080(4) Uani 1 1 d U . . H23A H 0.0829 -0.3399 0.0395 0.095 Uiso 1 1 calc R . . C24 C 0.1851(15) -0.3877(6) -0.0315(5) 0.085(4) Uani 1 1 d U . . H24A H 0.2206 -0.4384 -0.0066 0.102 Uiso 1 1 calc R . . C25 C 0.2139(14) -0.3737(5) -0.0923(5) 0.074(3) Uani 1 1 d U . . H25 H 0.2681 -0.4142 -0.1098 0.089 Uiso 1 1 calc R . . C26 C 0.1652(10) -0.3013(5) -0.1285(4) 0.042(2) Uani 1 1 d U . . N31 N 0.1192(8) -0.1999(4) -0.2182(3) 0.0369(16) Uani 1 1 d U . . C32 C 0.1806(10) -0.2749(5) -0.1949(4) 0.043(2) Uani 1 1 d U . . C33 C 0.2498(11) -0.3218(5) -0.2344(4) 0.056(2) Uani 1 1 d U . . H33A H 0.2932 -0.3749 -0.2177 0.067 Uiso 1 1 calc R . . C34 C 0.2550(12) -0.2926(6) -0.2947(5) 0.067(3) Uani 1 1 d U . . H34A H 0.3025 -0.3244 -0.3210 0.080 Uiso 1 1 calc R . . C35 C 0.1920(11) -0.2172(5) -0.3179(4) 0.058(3) Uani 1 1 d U . . H35A H 0.1943 -0.1963 -0.3610 0.069 Uiso 1 1 calc R . . C36 C 0.1243(11) -0.1702(5) -0.2803(4) 0.048(2) Uani 1 1 d U . . H36A H 0.0811 -0.1171 -0.2974 0.057 Uiso 1 1 calc R . . N41 N -0.2008(8) -0.1498(4) -0.1851(3) 0.0343(15) Uani 1 1 d U . . C42 C -0.2754(10) -0.2140(5) -0.1732(4) 0.044(2) Uani 1 1 d U . . H42A H -0.2300 -0.2589 -0.1434 0.052 Uiso 1 1 calc R . . C43 C -0.4135(11) -0.2173(5) -0.2020(4) 0.054(3) Uani 1 1 d U . . H43 H -0.4625 -0.2640 -0.1922 0.065 Uiso 1 1 calc R . . C44 C -0.4827(12) -0.1534(5) -0.2452(4) 0.059(3) Uani 1 1 d U . . H44 H -0.5788 -0.1559 -0.2656 0.071 Uiso 1 1 calc R . . C45 C -0.4103(10) -0.0850(5) -0.2589(4) 0.049(2) Uani 1 1 d U . . H45A H -0.4541 -0.0402 -0.2892 0.059 Uiso 1 1 calc R . . C46 C -0.2740(10) -0.0847(5) -0.2273(4) 0.037(2) Uani 1 1 d U . . N51 N -0.0397(8) -0.0308(3) -0.2080(3) 0.0305(15) Uani 1 1 d U . . C52 C -0.1868(10) -0.0153(5) -0.2362(4) 0.038(2) Uani 1 1 d U . . C53 C -0.2367(11) 0.0607(5) -0.2721(4) 0.041(2) Uani 1 1 d U . . H53A H -0.3368 0.0727 -0.2933 0.049 Uiso 1 1 calc R . . C54 C -0.1382(11) 0.1166(5) -0.2758(4) 0.039(2) Uani 1 1 d U . . C55 C 0.0108(11) 0.0998(5) -0.2478(4) 0.041(2) Uani 1 1 d U . . H55 H 0.0792 0.1393 -0.2521 0.050 Uiso 1 1 calc R . . C56 C 0.0603(10) 0.0234(4) -0.2130(3) 0.0280(19) Uani 1 1 d U . . N61 N 0.2180(7) -0.0838(3) -0.1456(3) 0.0282(15) Uani 1 1 d U . . C62 C 0.2079(9) -0.0051(4) -0.1780(3) 0.0293(19) Uani 1 1 d U . . C63 C 0.3261(10) 0.0384(5) -0.1744(4) 0.037(2) Uani 1 1 d U . . H63A H 0.3173 0.0912 -0.1977 0.044 Uiso 1 1 calc R . . C64 C 0.4598(11) 0.0076(5) -0.1373(4) 0.046(2) Uani 1 1 d U . . H64 H 0.5422 0.0388 -0.1352 0.055 Uiso 1 1 calc R . . C65 C 0.4714(10) -0.0701(5) -0.1032(4) 0.041(2) Uani 1 1 d U . . H65A H 0.5597 -0.0927 -0.0763 0.050 Uiso 1 1 calc R . . C66 C 0.3488(10) -0.1133(5) -0.1099(3) 0.036(2) Uani 1 1 d U . . H66A H 0.3581 -0.1668 -0.0879 0.043 Uiso 1 1 calc R . . C71 C -0.1915(11) 0.2009(5) -0.3095(4) 0.042(2) Uani 1 1 d U . . C72 C -0.3524(11) 0.2324(5) -0.3069(4) 0.041(2) Uani 1 1 d U . . H72 H -0.4285 0.2008 -0.2850 0.050 Uiso 1 1 calc R . . C73 C -0.4029(11) 0.3114(5) -0.3370(4) 0.041(2) Uani 1 1 d U . . H73A H -0.5127 0.3335 -0.3347 0.049 Uiso 1 1 calc R . . C74 C -0.2927(11) 0.3565(5) -0.3696(4) 0.041(2) Uani 1 1 d U . . C75 C -0.1314(11) 0.3242(5) -0.3733(4) 0.043(2) Uani 1 1 d U . . H75A H -0.0562 0.3552 -0.3965 0.052 Uiso 1 1 calc R . . C76 C -0.0812(11) 0.2476(5) -0.3437(4) 0.043(2) Uani 1 1 d U . . H76 H 0.0289 0.2260 -0.3463 0.052 Uiso 1 1 calc R . . C77 C -0.3484(11) 0.4436(4) -0.4014(4) 0.040(2) Uani 1 1 d U . . H77A H -0.2795 0.4593 -0.4379 0.048 Uiso 1 1 calc R . . H77B H -0.4611 0.4491 -0.4157 0.048 Uiso 1 1 calc R . . N81 N -0.3397(8) 0.4987(4) -0.3588(3) 0.0372(17) Uani 1 1 d U . . H81A H -0.3619 0.5497 -0.3825 0.045 Uiso 1 1 calc R . . C82 C -0.4624(10) 0.4898(5) -0.3086(4) 0.043(2) Uani 1 1 d U . . H82A H -0.4511 0.5272 -0.2830 0.052 Uiso 1 1 calc R . . H82B H -0.4421 0.4360 -0.2820 0.052 Uiso 1 1 calc R . . C83 C -0.6352(10) 0.5047(5) -0.3335(4) 0.039(2) Uani 1 1 d U . . H83A H -0.6574 0.4604 -0.3503 0.046 Uiso 1 1 calc R . . H83B H -0.7146 0.5107 -0.3006 0.046 Uiso 1 1 calc R . . O84 O -0.6455(7) 0.5744(3) -0.3801(2) 0.0383(16) Uani 1 1 d U . . C85 C -0.8016(11) 0.5892(5) -0.4093(4) 0.050(3) Uani 1 1 d U . . H85A H -0.8876 0.6034 -0.3808 0.059 Uiso 1 1 calc R . . H85B H -0.8250 0.5418 -0.4217 0.059 Uiso 1 1 calc R . . C86 C -0.7933(11) 0.6577(5) -0.4660(4) 0.046(3) Uani 1 1 d U . . H86A H -0.6979 0.6450 -0.4911 0.055 Uiso 1 1 calc R . . H86B H -0.8910 0.6639 -0.4913 0.055 Uiso 1 1 calc R . . O87 O -0.7827(7) 0.7294(3) -0.4498(3) 0.0473(18) Uani 1 1 d U . . C88 C -0.8062(13) 0.7958(6) -0.5004(4) 0.059(3) Uani 1 1 d U . . H88A H -0.8392 0.8434 -0.4846 0.071 Uiso 1 1 calc R . . H88B H -0.8960 0.7898 -0.5257 0.071 Uiso 1 1 calc R . . C89 C -0.6652(15) 0.8076(6) -0.5392(5) 0.079(3) Uani 1 1 d U . . H89A H -0.6846 0.8597 -0.5683 0.095 Uiso 1 1 calc R . . H89B H -0.6480 0.7672 -0.5634 0.095 Uiso 1 1 calc R . . N90 N -0.5179(11) 0.8032(5) -0.5030(4) 0.075(2) Uani 1 1 d U . . H90A H -0.4369 0.7648 -0.4997 0.091 Uiso 1 1 calc R . . C91 C -0.5193(14) 0.8698(6) -0.4725(6) 0.087(3) Uani 1 1 d U . . H91A H -0.6143 0.8718 -0.4449 0.104 Uiso 1 1 calc R . . H91B H -0.5272 0.9201 -0.5039 0.104 Uiso 1 1 calc R . . C92 C -0.3626(14) 0.8582(6) -0.4352(6) 0.091(3) Uani 1 1 d U . . H92A H -0.2674 0.8577 -0.4628 0.109 Uiso 1 1 calc R . . H92B H -0.3628 0.9019 -0.4146 0.109 Uiso 1 1 calc R . . O93 O -0.3546(8) 0.7846(4) -0.3901(3) 0.073(2) Uani 1 1 d U . . C94 C -0.2029(14) 0.7651(6) -0.3587(6) 0.084(3) Uani 1 1 d U . . H94A H -0.1856 0.8073 -0.3385 0.101 Uiso 1 1 calc R . . H94B H -0.1136 0.7597 -0.3883 0.101 Uiso 1 1 calc R . . C95 C -0.2045(14) 0.6900(6) -0.3121(5) 0.075(3) Uani 1 1 d U . . H95A H -0.1115 0.6814 -0.2841 0.090 Uiso 1 1 calc R . . H95B H -0.3050 0.6923 -0.2875 0.090 Uiso 1 1 calc R . . O96 O -0.1954(8) 0.6266(3) -0.3421(3) 0.0551(19) Uani 1 1 d U . . C97 C -0.1551(13) 0.5509(6) -0.3031(4) 0.061(3) Uani 1 1 d U . . H97A H -0.2263 0.5452 -0.2665 0.073 Uiso 1 1 calc R . . H97B H -0.0420 0.5445 -0.2891 0.073 Uiso 1 1 calc R . . C98 C -0.1739(11) 0.4895(5) -0.3356(4) 0.048(2) Uani 1 1 d U . . H98A H -0.0967 0.4927 -0.3704 0.058 Uiso 1 1 calc R . . H98B H -0.1485 0.4371 -0.3074 0.058 Uiso 1 1 calc R . . C101 C -1.0556(10) 0.0017(8) -0.3934(9) 0.189(6) Uani 1 1 d DU . . C102 C -0.8755(8) 0.0144(3) -0.4064(3) 0.0344(17) Uani 1 1 d DU . . C104 C -0.6973(7) 0.0547(3) -0.3783(2) 0.0227(16) Uani 1 1 d DU . . O103 O -0.8580(8) 0.1003(4) -0.4081(5) 0.106(3) Uani 0.50 1 d PDU . . C105 C -0.6293(14) 0.1069(7) -0.3410(6) 0.111(3) Uani 0.50 1 d PDU . . O107 O -0.7751(10) -0.0163(7) -0.3475(5) 0.143(3) Uani 0.50 1 d PDU . . C106 C -0.5201(11) 0.0300(8) -0.3961(7) 0.047(4) Uani 0.50 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0324(4) 0.0245(3) 0.0385(4) -0.0154(3) -0.0012(3) 0.0023(3) P1 0.0531(16) 0.0558(16) 0.0613(16) -0.0075(13) -0.0034(14) -0.0061(13) F1 0.100(3) 0.078(3) 0.130(5) -0.007(3) -0.002(3) -0.030(3) F2 0.202(6) 0.120(4) 0.104(3) -0.053(3) 0.031(4) -0.051(4) F3 0.127(4) 0.086(4) 0.184(5) 0.031(4) -0.059(4) -0.009(3) F4 0.109(5) 0.143(4) 0.149(3) -0.079(3) 0.050(3) -0.052(3) F5 0.121(4) 0.129(5) 0.151(5) -0.007(4) -0.068(4) 0.022(4) F6 0.102(3) 0.126(4) 0.117(4) -0.051(3) 0.032(3) -0.047(3) Cl1 0.117(2) 0.0645(17) 0.0578(16) -0.0015(15) 0.0019(16) 0.0192(17) O11 0.142(7) 0.060(3) 0.177(7) -0.044(4) -0.024(5) 0.043(4) O12 0.099(4) 0.109(5) 0.308(12) -0.062(6) -0.024(5) -0.022(4) O13 0.151(7) 0.290(12) 0.064(4) 0.005(6) 0.021(4) 0.083(7) O14 0.087(4) 0.106(5) 0.064(4) -0.019(4) -0.015(3) 0.016(4) Cl2 0.0052(12) 0.0133(12) 0.0298(13) -0.0103(11) 0.0063(11) 0.0008(10) O21 0.018(4) 0.017(3) 0.102(6) -0.006(3) 0.034(4) 0.004(3) O22 0.013(3) 0.030(4) 0.050(4) 0.002(4) -0.003(3) 0.007(3) O23 0.045(5) 0.129(6) 0.046(3) -0.031(4) -0.013(3) -0.010(5) O24 0.019(3) 0.024(4) 0.054(4) 0.016(4) 0.014(3) 0.009(3) O1 0.146(8) 0.099(6) 0.147(8) -0.035(6) -0.037(6) -0.028(6) C4 0.097(9) 0.058(4) 0.138(10) -0.032(7) -0.033(8) -0.003(7) C5 0.064(7) 0.060(4) 0.105(8) -0.030(6) -0.028(6) 0.000(6) N6 0.108(8) 0.063(4) 0.189(11) -0.016(7) -0.037(8) -0.018(6) C7 0.31(2) 0.073(5) 0.091(9) -0.002(6) -0.070(12) -0.016(11) C8 0.175(13) 0.059(5) 0.102(8) -0.023(5) -0.062(9) 0.015(8) N9 0.163(11) 0.077(5) 0.135(9) 0.004(6) -0.056(9) 0.014(8) N11 0.031(4) 0.042(3) 0.039(2) -0.022(2) 0.003(2) -0.005(3) C12 0.031(5) 0.051(4) 0.060(3) -0.037(3) -0.003(4) 0.002(4) C13 0.068(7) 0.059(4) 0.069(4) -0.046(3) 0.008(5) -0.003(5) C14 0.084(8) 0.078(5) 0.061(4) -0.034(3) 0.012(5) -0.018(5) C15 0.090(8) 0.060(4) 0.043(4) -0.008(3) 0.015(5) -0.017(5) C16 0.059(6) 0.047(3) 0.036(3) -0.011(3) 0.001(4) -0.021(4) N21 0.050(4) 0.026(2) 0.042(3) -0.007(2) -0.013(3) 0.002(3) C22 0.062(6) 0.043(3) 0.043(3) -0.007(3) -0.012(4) -0.010(4) C23 0.144(10) 0.050(4) 0.040(4) -0.002(3) -0.038(5) 0.000(5) C24 0.116(9) 0.054(5) 0.077(4) -0.010(4) -0.036(6) 0.012(5) C25 0.114(9) 0.031(4) 0.078(4) -0.024(3) -0.039(5) 0.018(5) C26 0.034(5) 0.021(3) 0.071(3) -0.017(3) -0.012(4) 0.006(4) N31 0.033(4) 0.037(3) 0.048(2) -0.028(2) -0.001(3) 0.000(3) C32 0.035(5) 0.032(3) 0.070(3) -0.031(3) -0.009(4) 0.005(4) C33 0.043(6) 0.051(4) 0.087(4) -0.045(3) -0.003(4) -0.001(4) C34 0.060(7) 0.076(4) 0.086(4) -0.061(4) 0.015(5) -0.014(4) C35 0.055(6) 0.070(4) 0.064(4) -0.043(3) 0.018(4) -0.021(4) C36 0.047(6) 0.059(4) 0.045(3) -0.029(3) -0.002(4) -0.006(4) N41 0.030(3) 0.035(3) 0.046(3) -0.029(3) 0.001(2) -0.001(2) C42 0.034(4) 0.040(4) 0.066(5) -0.033(4) 0.011(3) -0.005(3) C43 0.037(4) 0.056(4) 0.086(6) -0.045(4) 0.011(4) -0.020(4) C44 0.043(5) 0.078(4) 0.074(5) -0.054(4) -0.003(4) -0.004(3) C45 0.026(4) 0.062(4) 0.066(5) -0.036(4) -0.009(3) 0.014(3) C46 0.021(3) 0.041(3) 0.054(5) -0.026(3) 0.000(3) 0.007(3) N51 0.032(3) 0.027(2) 0.035(3) -0.015(2) -0.009(3) 0.005(2) C52 0.027(3) 0.041(3) 0.043(5) -0.012(3) -0.003(3) 0.009(3) C53 0.041(4) 0.038(3) 0.043(5) -0.019(3) -0.011(4) 0.017(3) C54 0.043(4) 0.034(3) 0.031(4) -0.006(3) 0.001(3) 0.015(3) C55 0.052(4) 0.023(3) 0.050(5) -0.017(3) -0.005(4) 0.008(3) C56 0.031(3) 0.025(3) 0.028(4) -0.015(3) -0.001(3) 0.008(3) N61 0.029(3) 0.024(3) 0.032(3) -0.013(2) 0.000(2) 0.004(2) C62 0.029(3) 0.030(3) 0.032(4) -0.014(3) 0.002(3) -0.002(3) C63 0.032(4) 0.025(4) 0.057(5) -0.018(4) 0.002(3) -0.003(3) C64 0.040(4) 0.049(4) 0.056(5) -0.024(4) -0.004(4) -0.013(4) C65 0.033(4) 0.043(4) 0.051(5) -0.020(4) -0.007(4) 0.002(3) C66 0.043(4) 0.032(4) 0.034(4) -0.015(3) -0.006(3) 0.004(3) C71 0.047(4) 0.040(3) 0.030(4) -0.007(3) 0.001(4) 0.020(3) C72 0.049(4) 0.032(4) 0.036(5) -0.008(4) 0.000(4) 0.018(3) C73 0.047(4) 0.031(4) 0.036(5) -0.007(3) 0.009(4) 0.021(3) C74 0.047(4) 0.034(3) 0.034(5) -0.005(3) -0.002(4) 0.016(3) C75 0.045(4) 0.038(4) 0.043(5) -0.014(4) 0.001(4) 0.014(3) C76 0.049(4) 0.031(4) 0.045(5) -0.012(4) 0.006(4) 0.016(3) C77 0.040(5) 0.033(3) 0.044(4) -0.011(3) -0.003(3) 0.008(3) N81 0.033(3) 0.033(3) 0.042(3) -0.012(3) -0.003(3) 0.016(3) C82 0.046(3) 0.035(5) 0.046(4) -0.013(4) 0.002(3) 0.006(4) C83 0.041(4) 0.037(4) 0.034(4) -0.006(3) 0.009(3) 0.001(4) O84 0.047(3) 0.025(3) 0.040(3) -0.007(2) 0.006(2) 0.000(3) C85 0.049(5) 0.045(4) 0.051(5) -0.007(4) -0.009(4) -0.001(4) C86 0.046(6) 0.044(3) 0.049(5) -0.013(3) -0.004(4) -0.002(4) O87 0.058(4) 0.037(3) 0.046(3) -0.015(2) -0.006(3) 0.005(3) C88 0.081(4) 0.046(4) 0.048(5) -0.011(4) -0.018(4) 0.009(5) C89 0.120(5) 0.058(6) 0.043(5) -0.005(4) 0.014(3) 0.021(5) N90 0.071(4) 0.044(4) 0.110(5) -0.028(3) 0.038(4) 0.006(4) C91 0.078(6) 0.055(5) 0.131(7) -0.038(4) 0.032(4) -0.001(5) C92 0.075(6) 0.047(5) 0.158(8) -0.038(4) 0.032(4) -0.015(5) O93 0.065(4) 0.051(3) 0.118(5) -0.048(3) 0.027(3) -0.014(3) C94 0.067(6) 0.064(4) 0.144(7) -0.070(4) 0.015(5) -0.015(5) C95 0.070(7) 0.083(4) 0.097(6) -0.065(3) 0.011(5) -0.016(5) O96 0.060(4) 0.052(2) 0.061(4) -0.030(3) 0.003(3) -0.005(3) C97 0.060(6) 0.072(4) 0.053(5) -0.017(3) -0.013(4) -0.009(5) C98 0.039(4) 0.049(4) 0.054(5) -0.012(4) -0.010(4) 0.005(4) C101 0.090(4) 0.306(10) 0.196(15) -0.093(14) 0.035(6) -0.062(5) C102 0.061(3) 0.005(3) 0.024(3) -0.001(3) 0.025(3) 0.027(3) C104 0.042(3) 0.000(3) 0.000(3) 0.028(2) 0.024(2) 0.032(2) O103 0.126(4) 0.037(3) 0.169(8) -0.082(4) -0.108(5) 0.076(4) C105 0.013(6) 0.150(5) 0.201(8) -0.143(5) -0.039(5) 0.074(4) O107 0.158(5) 0.152(4) 0.080(6) 0.104(5) -0.035(4) -0.103(4) C106 0.070(4) 0.023(8) 0.027(8) 0.009(6) 0.020(6) 0.030(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N51 1.986(6) . ? Ru1 N21 2.011(6) . ? Ru1 N61 2.052(7) . ? Ru1 N41 2.057(7) . ? Ru1 N11 2.068(7) . ? Ru1 N31 2.078(7) . ? P1 F5 1.499(8) . ? P1 F4 1.543(8) . ? P1 F1 1.553(8) . ? P1 F6 1.568(8) . ? P1 F3 1.580(8) . ? P1 F2 1.600(9) . ? Cl1 O13 1.416(10) . ? Cl1 O11 1.437(9) . ? Cl1 O14 1.456(8) . ? Cl1 O12 1.508(11) . ? Cl2 O23 1.367(10) . ? Cl2 O21 1.379(8) . ? Cl2 O22 1.426(7) . ? Cl2 O24 1.439(8) . ? C4 C5 1.424(14) . ? C5 N6 1.121(14) . ? C7 C8 1.424(17) . ? C8 N9 1.118(15) . ? N11 C12 1.325(10) . ? N11 C16 1.381(10) . ? C12 C13 1.392(13) . ? C13 C14 1.360(13) . ? C14 C15 1.390(15) . ? C15 C16 1.354(13) . ? C16 C22 1.496(13) . ? N21 C22 1.325(11) . ? N21 C26 1.367(11) . ? C22 C23 1.388(12) . ? C23 C24 1.418(16) . ? C24 C25 1.346(15) . ? C25 C26 1.359(12) . ? C26 C32 1.458(12) . ? N31 C32 1.340(10) . ? N31 C36 1.367(10) . ? C32 C33 1.409(13) . ? C33 C34 1.328(13) . ? C34 C35 1.348(13) . ? C35 C36 1.376(13) . ? N41 C42 1.339(10) . ? N41 C46 1.385(9) . ? C42 C43 1.360(13) . ? C43 C44 1.373(12) . ? C44 C45 1.394(13) . ? C45 C46 1.366(12) . ? C46 C52 1.484(12) . ? N51 C56 1.342(10) . ? N51 C52 1.367(10) . ? C52 C53 1.407(11) . ? C53 C54 1.360(13) . ? C54 C55 1.377(12) . ? C54 C71 1.515(11) . ? C55 C56 1.404(10) . ? C56 C62 1.448(11) . ? N61 C66 1.348(10) . ? N61 C62 1.402(9) . ? C62 C63 1.351(12) . ? C63 C64 1.384(12) . ? C64 C65 1.397(11) . ? C65 C66 1.395(12) . ? C71 C72 1.386(12) . ? C71 C76 1.407(12) . ? C72 C73 1.411(11) . ? C73 C74 1.378(12) . ? C74 C75 1.396(12) . ? C74 C77 1.548(11) . ? C75 C76 1.372(11) . ? C77 N81 1.531(11) . ? N81 C98 1.472(11) . ? N81 C82 1.490(11) . ? C82 C83 1.534(12) . ? C83 O84 1.408(9) . ? O84 C85 1.443(11) . ? C85 C86 1.541(12) . ? C86 O87 1.417(11) . ? O87 C88 1.422(10) . ? C88 C89 1.447(15) . ? C89 N90 1.483(15) . ? N90 C91 1.497(15) . ? C91 C92 1.544(17) . ? C92 O93 1.440(12) . ? O93 C94 1.432(13) . ? C94 C95 1.482(14) . ? C95 O96 1.432(12) . ? O96 C97 1.418(10) . ? C97 C98 1.475(14) . ? C101 C102 1.559(10) . ? C102 O107 1.535(11) . ? C102 O103 1.539(9) . ? C102 C104 1.927(10) . ? C104 O107 1.505(10) . ? C104 C106 1.549(11) . ? C104 O103 1.550(8) . ? C104 C105 1.559(13) . ? 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 N51 Ru1 N21 178.7(3) . . ? N51 Ru1 N61 78.3(2) . . ? N21 Ru1 N61 100.4(3) . . ? N51 Ru1 N41 79.9(3) . . ? N21 Ru1 N41 101.4(3) . . ? N61 Ru1 N41 158.2(2) . . ? N51 Ru1 N11 100.5(3) . . ? N21 Ru1 N11 79.7(3) . . ? N61 Ru1 N11 88.4(3) . . ? N41 Ru1 N11 95.7(3) . . ? N51 Ru1 N31 101.8(2) . . ? N21 Ru1 N31 78.0(3) . . ? N61 Ru1 N31 98.1(3) . . ? N41 Ru1 N31 86.2(3) . . ? N11 Ru1 N31 157.6(2) . . ? F5 P1 F4 90.6(5) . . ? F5 P1 F1 91.4(4) . . ? F4 P1 F1 92.5(4) . . ? F5 P1 F6 92.4(5) . . ? F4 P1 F6 91.1(4) . . ? F1 P1 F6 174.7(4) . . ? F5 P1 F3 179.1(6) . . ? F4 P1 F3 88.7(5) . . ? F1 P1 F3 89.2(4) . . ? F6 P1 F3 87.1(4) . . ? F5 P1 F2 93.5(5) . . ? F4 P1 F2 175.5(4) . . ? F1 P1 F2 89.3(5) . . ? F6 P1 F2 86.8(4) . . ? F3 P1 F2 87.2(5) . . ? O13 Cl1 O11 109.0(8) . . ? O13 Cl1 O14 107.6(6) . . ? O11 Cl1 O14 102.7(6) . . ? O13 Cl1 O12 132.0(9) . . ? O11 Cl1 O12 101.5(6) . . ? O14 Cl1 O12 100.6(6) . . ? O23 Cl2 O21 110.8(6) . . ? O23 Cl2 O22 108.6(5) . . ? O21 Cl2 O22 108.7(5) . . ? O23 Cl2 O24 111.4(5) . . ? O21 Cl2 O24 107.8(5) . . ? O22 Cl2 O24 109.4(4) . . ? N6 C5 C4 176.3(14) . . ? N9 C8 C7 176.4(19) . . ? C12 N11 C16 118.1(7) . . ? C12 N11 Ru1 128.1(5) . . ? C16 N11 Ru1 113.8(5) . . ? N11 C12 C13 120.8(8) . . ? C14 C13 C12 121.3(9) . . ? C13 C14 C15 117.8(10) . . ? C16 C15 C14 119.3(9) . . ? C15 C16 N11 122.5(8) . . ? C15 C16 C22 123.4(8) . . ? N11 C16 C22 114.1(7) . . ? C22 N21 C26 124.9(7) . . ? C22 N21 Ru1 117.7(6) . . ? C26 N21 Ru1 117.4(5) . . ? N21 C22 C23 118.6(9) . . ? N21 C22 C16 114.7(7) . . ? C23 C22 C16 126.7(8) . . ? C22 C23 C24 116.8(9) . . ? C25 C24 C23 122.2(9) . . ? C24 C25 C26 119.7(10) . . ? C25 C26 N21 117.8(8) . . ? C25 C26 C32 128.2(9) . . ? N21 C26 C32 114.0(7) . . ? C32 N31 C36 119.1(7) . . ? C32 N31 Ru1 115.8(6) . . ? C36 N31 Ru1 125.1(5) . . ? N31 C32 C33 119.8(8) . . ? N31 C32 C26 114.7(7) . . ? C33 C32 C26 125.5(7) . . ? C34 C33 C32 120.9(8) . . ? C33 C34 C35 119.2(10) . . ? C34 C35 C36 121.1(9) . . ? N31 C36 C35 120.0(8) . . ? C42 N41 C46 116.8(7) . . ? C42 N41 Ru1 128.3(5) . . ? C46 N41 Ru1 114.6(5) . . ? N41 C42 C43 122.5(8) . . ? C42 C43 C44 120.4(9) . . ? C43 C44 C45 119.3(9) . . ? C46 C45 C44 117.5(8) . . ? C45 C46 N41 123.4(8) . . ? C45 C46 C52 123.2(7) . . ? N41 C46 C52 113.4(7) . . ? C56 N51 C52 122.9(6) . . ? C56 N51 Ru1 119.5(5) . . ? C52 N51 Ru1 117.5(5) . . ? N51 C52 C53 119.0(8) . . ? N51 C52 C46 114.0(7) . . ? C53 C52 C46 127.0(8) . . ? C54 C53 C52 118.5(8) . . ? C53 C54 C55 121.8(7) . . ? C53 C54 C71 120.7(8) . . ? C55 C54 C71 117.4(8) . . ? C54 C55 C56 119.1(8) . . ? N51 C56 C55 118.6(7) . . ? N51 C56 C62 113.8(6) . . ? C55 C56 C62 127.5(8) . . ? C66 N61 C62 116.9(7) . . ? C66 N61 Ru1 128.2(5) . . ? C62 N61 Ru1 114.8(5) . . ? C63 C62 N61 121.2(7) . . ? C63 C62 C56 125.2(7) . . ? N61 C62 C56 113.6(7) . . ? C62 C63 C64 121.4(7) . . ? C63 C64 C65 118.8(8) . . ? C66 C65 C64 117.7(8) . . ? N61 C66 C65 123.9(7) . . ? C72 C71 C76 119.5(7) . . ? C72 C71 C54 119.2(8) . . ? C76 C71 C54 121.4(8) . . ? C71 C72 C73 119.7(8) . . ? C74 C73 C72 120.0(8) . . ? C73 C74 C75 120.2(7) . . ? C73 C74 C77 119.6(8) . . ? C75 C74 C77 120.2(8) . . ? C76 C75 C74 120.1(8) . . ? C75 C76 C71 120.5(8) . . ? N81 C77 C74 112.4(6) . . ? C98 N81 C82 112.6(6) . . ? C98 N81 C77 109.8(6) . . ? C82 N81 C77 113.3(7) . . ? N81 C82 C83 112.0(7) . . ? O84 C83 C82 106.4(7) . . ? C83 O84 C85 109.6(6) . . ? O84 C85 C86 106.4(7) . . ? O87 C86 C85 112.2(7) . . ? C86 O87 C88 113.1(7) . . ? O87 C88 C89 114.3(8) . . ? C88 C89 N90 112.0(8) . . ? C89 N90 C91 113.9(8) . . ? N90 C91 C92 109.5(9) . . ? O93 C92 C91 108.4(9) . . ? C94 O93 C92 111.6(8) . . ? O93 C94 C95 108.7(9) . . ? O96 C95 C94 109.5(9) . . ? C97 O96 C95 114.7(7) . . ? O96 C97 C98 110.6(8) . . ? N81 C98 C97 111.0(7) . . ? O107 C102 O103 92.2(7) . . ? O107 C102 C101 110.5(8) . . ? O103 C102 C101 109.2(7) . . ? O107 C102 C104 50.0(4) . . ? O103 C102 C104 51.7(3) . . ? C101 C102 C104 143.7(9) . . ? O107 C104 C106 110.5(7) . . ? O107 C104 O103 93.0(5) . . ? C106 C104 O103 140.4(8) . . ? O107 C104 C105 121.9(8) . . ? C106 C104 C105 87.1(8) . . ? O103 C104 C105 107.6(6) . . ? O107 C104 C102 51.4(4) . . ? C106 C104 C102 121.9(7) . . ? O103 C104 C102 51.2(3) . . ? C105 C104 C102 151.0(6) . . ? C102 O103 C104 77.2(5) . . ? C104 O107 C102 78.7(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.156 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.167 #=END data_structure2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74.22 H77.60 F16.17 N12 O5.81 P2.70 Ru' _chemical_formula_weight 1722.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ru' 'Ru' -1.2594 0.8363 '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' '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' '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' 'F' 'F' 0.0171 0.0103 '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 11.417(4) _cell_length_b 18.318(9) _cell_length_c 20.444(9) _cell_angle_alpha 76.40(3) _cell_angle_beta 88.87(5) _cell_angle_gamma 81.32(4) _cell_volume 4108(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1767 _exptl_absorpt_coefficient_mu 0.336 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ? _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 ? _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 27122 _diffrn_reflns_av_R_equivalents 0.1034 _diffrn_reflns_av_sigmaI/netI 0.1488 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 22.50 _reflns_number_total 10660 _reflns_number_gt 4796 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.2726P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10660 _refine_ls_number_parameters 1047 _refine_ls_number_restraints 1123 _refine_ls_R_factor_all 0.2390 _refine_ls_R_factor_gt 0.1329 _refine_ls_wR_factor_ref 0.4290 _refine_ls_wR_factor_gt 0.3461 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.173 _refine_ls_shift/su_mean 0.019 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 1.20750(7) -0.07319(5) 0.80919(4) 0.0705(3) Uani 1 1 d U . . N111 N 1.3048(6) -0.0901(6) 0.8974(4) 0.0939(19) Uani 1 1 d DU . . C112 C 1.3288(6) -0.1613(8) 0.9300(4) 0.109(2) Uani 1 1 d DU . . C113 C 1.3894(7) -0.1891(7) 0.9930(4) 0.138(3) Uani 1 1 d DU . . H11A H 1.4073 -0.2400 1.0154 0.166 Uiso 1 1 calc R . . C114 C 1.4182(10) -0.1266(5) 1.0160(7) 0.173(3) Uani 1 1 d DU . . H11C H 1.4603 -0.1399 1.0566 0.208 Uiso 1 1 calc R . . C115 C 1.3937(11) -0.0473(7) 0.9877(5) 0.175(4) Uani 1 1 d DU . . H115 H 1.4124 -0.0095 1.0074 0.210 Uiso 1 1 calc R . . C116 C 1.3366(8) -0.0351(8) 0.9248(4) 0.132(3) Uani 1 1 d DU . . H11D H 1.3192 0.0148 0.8999 0.159 Uiso 1 1 calc R . . N121 N 1.2228(6) -0.1825(5) 0.8429(4) 0.0769(18) Uani 1 1 d DU . . C122 C 1.2880(7) -0.2192(8) 0.9010(5) 0.094(2) Uani 1 1 d DU . . C123 C 1.2975(9) -0.2985(8) 0.9220(6) 0.119(3) Uani 1 1 d DU . . H12A H 1.3407 -0.3242 0.9608 0.143 Uiso 1 1 calc R . . C124 C 1.2448(12) -0.3377(8) 0.8864(7) 0.127(4) Uani 1 1 d DU . . H12B H 1.2542 -0.3903 0.9017 0.152 Uiso 1 1 calc R . . C125 C 1.1783(10) -0.3056(6) 0.8292(6) 0.100(3) Uani 1 1 d DU . . H12C H 1.1410 -0.3333 0.8053 0.120 Uiso 1 1 calc R . . C126 C 1.1722(8) -0.2245(6) 0.8099(5) 0.071(2) Uani 1 1 d DU . . N131 N 1.1117(5) -0.1009(4) 0.7353(3) 0.0552(17) Uani 1 1 d DU . . C132 C 1.1059(7) -0.1766(5) 0.7486(4) 0.063(2) Uani 1 1 d DU . . C133 C 1.0421(8) -0.2051(5) 0.7047(5) 0.074(3) Uani 1 1 d DU . . H13A H 1.0374 -0.2567 0.7130 0.089 Uiso 1 1 calc R . . C134 C 0.9864(9) -0.1550(6) 0.6489(5) 0.084(3) Uani 1 1 d DU . . H13B H 0.9440 -0.1729 0.6192 0.101 Uiso 1 1 calc R . . C135 C 0.9932(8) -0.0796(6) 0.6372(5) 0.073(3) Uani 1 1 d DU . . H13C H 0.9560 -0.0458 0.5996 0.088 Uiso 1 1 calc R . . C136 C 1.0570(8) -0.0539(6) 0.6826(4) 0.068(3) Uani 1 1 d DU . . H13D H 1.0609 -0.0023 0.6752 0.081 Uiso 1 1 calc R . . N211 N 1.3541(6) -0.0654(5) 0.7471(3) 0.0714(19) Uani 1 1 d DU . . C212 C 1.3593(8) 0.0082(6) 0.7123(4) 0.074(2) Uani 1 1 d DU . . C213 C 1.4515(8) 0.0207(6) 0.6679(4) 0.073(3) Uani 1 1 d DU . . H21A H 1.4578 0.0701 0.6447 0.088 Uiso 1 1 calc R . . C214 C 1.5335(9) -0.0379(7) 0.6572(5) 0.084(3) Uani 1 1 d DU . . H21C H 1.5937 -0.0287 0.6265 0.100 Uiso 1 1 calc R . . C215 C 1.5254(8) -0.1098(6) 0.6923(4) 0.073(3) Uani 1 1 d DU . . H21D H 1.5817 -0.1499 0.6863 0.088 Uiso 1 1 calc R . . C216 C 1.4344(8) -0.1238(6) 0.7370(4) 0.073(3) Uani 1 1 d DU . . H21E H 1.4283 -0.1733 0.7600 0.088 Uiso 1 1 calc R . . N221 N 1.1922(7) 0.0395(5) 0.7713(4) 0.0748(19) Uani 1 1 d DU . . C222 C 1.2671(8) 0.0672(6) 0.7254(4) 0.078(2) Uani 1 1 d DU . . C223 C 1.2503(9) 0.1448(6) 0.6955(5) 0.083(3) Uani 1 1 d DU . . H22A H 1.3029 0.1653 0.6635 0.100 Uiso 1 1 calc R . . C224 C 1.1521(11) 0.1919(7) 0.7145(5) 0.093(3) Uani 1 1 d DU . . C225 C 1.0783(10) 0.1580(7) 0.7636(5) 0.087(3) Uani 1 1 d DU . . H22B H 1.0138 0.1881 0.7772 0.104 Uiso 1 1 calc R . . C226 C 1.0971(9) 0.0848(6) 0.7914(5) 0.079(2) Uani 1 1 d DU . . N231 N 1.0551(6) -0.0325(5) 0.8574(4) 0.0696(19) Uani 1 1 d DU . . C232 C 1.0289(8) 0.0446(7) 0.8425(5) 0.089(3) Uani 1 1 d DU . . C233 C 0.9383(9) 0.0786(8) 0.8775(5) 0.103(3) Uani 1 1 d DU . . H23A H 0.9204 0.1313 0.8676 0.123 Uiso 1 1 calc R . . C234 C 0.8763(11) 0.0373(8) 0.9252(6) 0.123(4) Uani 1 1 d DU . . H23B H 0.8178 0.0616 0.9483 0.147 Uiso 1 1 calc R . . C235 C 0.8993(9) -0.0420(8) 0.9401(6) 0.102(3) Uani 1 1 d DU . . H23C H 0.8544 -0.0712 0.9713 0.122 Uiso 1 1 calc R . . C236 C 0.9944(8) -0.0767(7) 0.9057(5) 0.084(3) Uani 1 1 d DU . . H23D H 1.0150 -0.1293 0.9160 0.100 Uiso 1 1 calc R . . C241 C 1.1319(11) 0.2738(7) 0.6813(6) 0.114(4) Uani 1 1 d DU . . C242 C 1.0454(10) 0.3259(7) 0.7087(6) 0.125(4) Uani 1 1 d DU . . H24A H 1.0073 0.3075 0.7485 0.150 Uiso 1 1 calc R . . C243 C 1.0186(12) 0.4037(8) 0.6761(6) 0.131(4) Uani 1 1 d DU . . H24B H 0.9637 0.4356 0.6948 0.157 Uiso 1 1 calc R . . C244 C 1.0710(14) 0.4321(9) 0.6187(6) 0.129(4) Uani 1 1 d DU . . C245 C 1.1608(16) 0.3841(8) 0.5909(7) 0.146(5) Uani 1 1 d DU . . H24C H 1.2034 0.4034 0.5532 0.176 Uiso 1 1 calc R . . C246 C 1.1802(15) 0.3083(8) 0.6231(6) 0.137(5) Uani 1 1 d DU . . H24D H 1.2326 0.2770 0.6026 0.165 Uiso 1 1 calc R . . C247 C 1.0365(17) 0.5137(8) 0.5819(6) 0.147(5) Uani 1 1 d U . . H24E H 1.0909 0.5274 0.5456 0.176 Uiso 1 1 calc R . . H24F H 0.9571 0.5215 0.5629 0.176 Uiso 1 1 calc R . . N250 N 1.0410(7) 0.5612(6) 0.6315(5) 0.164(3) Uani 1 1 d DU . . C251 C 1.1604(10) 0.5585(9) 0.6539(5) 0.217(6) Uani 1 1 d DU . . H25A H 1.1999 0.5072 0.6564 0.260 Uiso 1 1 calc R . . H25B H 1.1977 0.5913 0.6179 0.260 Uiso 1 1 calc R . . C252 C 1.1897(9) 0.5768(9) 0.7134(5) 0.166(6) Uani 1 1 d DU . . H25C H 1.1976 0.6303 0.7037 0.200 Uiso 1 1 calc R . . H25D H 1.2660 0.5479 0.7298 0.200 Uiso 1 1 calc R . . O253 O 1.1072(8) 0.5625(4) 0.7637(3) 0.129(3) Uiso 1 1 d DU . . C254 C 1.1194(10) 0.4910(5) 0.8063(4) 0.120(4) Uani 1 1 d DU . . H25E H 1.2026 0.4694 0.8115 0.144 Uiso 1 1 calc R . . H25J H 1.0784 0.4581 0.7871 0.144 Uiso 1 1 calc R . . C255 C 1.0715(9) 0.4950(9) 0.8708(5) 0.181(7) Uani 1 1 d DU . . H25K H 1.0845 0.4446 0.9004 0.217 Uiso 1 1 calc R . . H25L H 1.1139 0.5274 0.8898 0.217 Uiso 1 1 calc R . . O256 O 0.9541(6) 0.5224(7) 0.8684(5) 0.198(5) Uani 1 1 d DU . . C257 C 0.8782(8) 0.5153(6) 0.9232(6) 0.146(5) Uani 1 1 d DU . . H25F H 0.9030 0.5412 0.9555 0.176 Uiso 1 1 calc R . . H25G H 0.8799 0.4621 0.9453 0.176 Uiso 1 1 calc R . . C258 C 0.7587(9) 0.5489(6) 0.8982(7) 0.142(4) Uani 1 1 d DU . . H25H H 0.7357 0.5203 0.8675 0.171 Uiso 1 1 calc R . . H25I H 0.7058 0.5416 0.9361 0.171 Uiso 1 1 calc R . . N259 N 0.7379(6) 0.6282(4) 0.8643(5) 0.100(3) Uani 1 1 d DU . . C260 C 0.6118(8) 0.6523(7) 0.8488(4) 0.129(4) Uani 1 1 d DU . . H26A H 0.5679 0.6366 0.8894 0.154 Uiso 1 1 calc R . . H26B H 0.5971 0.7074 0.8356 0.154 Uiso 1 1 calc R . . C261 C 0.5655(10) 0.6229(8) 0.7959(5) 0.165(5) Uani 1 1 d DU . . H26C H 0.5821 0.5679 0.8068 0.198 Uiso 1 1 calc R . . H26D H 0.4803 0.6381 0.7912 0.198 Uiso 1 1 calc R . . O262 O 0.6207(9) 0.6528(5) 0.7361(3) 0.137(3) Uani 1 1 d DU . . C263 C 0.6045(9) 0.6229(8) 0.6807(5) 0.199(5) Uani 1 1 d DU . . H26E H 0.5210 0.6330 0.6682 0.239 Uiso 1 1 calc R . . H26F H 0.6279 0.5682 0.6931 0.239 Uiso 1 1 calc R . . C264 C 0.6712(11) 0.6543(11) 0.6245(5) 0.238(8) Uani 1 1 d DU . . H26G H 0.6489 0.6377 0.5855 0.286 Uiso 1 1 calc R . . H26H H 0.6532 0.7093 0.6145 0.286 Uiso 1 1 calc R . . O265 O 0.7941(6) 0.6319(5) 0.6373(4) 0.167(3) Uani 1 1 d DU . . C266 C 0.8649(9) 0.6508(8) 0.5792(6) 0.203(5) Uani 1 1 d DU . . H26I H 0.8435 0.7040 0.5571 0.243 Uiso 1 1 calc R . . H26J H 0.8515 0.6207 0.5476 0.243 Uiso 1 1 calc R . . C267 C 0.9878(9) 0.6355(7) 0.6000(8) 0.219(5) Uani 1 1 d DU . . H26K H 1.0336 0.6526 0.5604 0.263 Uiso 1 1 calc R . . H26L H 0.9975 0.6677 0.6305 0.263 Uiso 1 1 calc R . . C270 C 0.7816(10) 0.6749(6) 0.9094(6) 0.093(3) Uani 1 1 d U . . H27A H 0.7436 0.6638 0.9527 0.111 Uiso 1 1 calc R . . H27B H 0.8664 0.6601 0.9169 0.111 Uiso 1 1 calc R . . C271 C 0.7566(8) 0.7560(6) 0.8799(5) 0.072(3) Uani 1 1 d DU . . C272 C 0.6852(7) 0.8052(6) 0.9134(5) 0.078(3) Uani 1 1 d DU . . H27C H 0.6527 0.7846 0.9544 0.093 Uiso 1 1 calc R . . C273 C 0.6624(7) 0.8809(6) 0.8882(5) 0.075(3) Uani 1 1 d DU . . H27D H 0.6158 0.9114 0.9122 0.090 Uiso 1 1 calc R . . C274 C 0.7087(8) 0.9138(6) 0.8260(5) 0.067(2) Uani 1 1 d DU . . C275 C 0.7786(8) 0.8664(6) 0.7923(5) 0.075(3) Uani 1 1 d DU . . H27E H 0.8095 0.8866 0.7507 0.090 Uiso 1 1 calc R . . C276 C 0.8018(9) 0.7920(6) 0.8193(5) 0.080(3) Uani 1 1 d DU . . H27F H 0.8515 0.7622 0.7960 0.096 Uiso 1 1 calc R . . N281 N 0.8850(7) 1.1097(5) 0.6435(4) 0.092(3) Uani 1 1 d DU . . C282 C 0.7995(7) 1.1522(6) 0.6704(5) 0.078(3) Uani 1 1 d DU . . C283 C 0.7832(10) 1.2295(7) 0.6480(6) 0.107(4) Uani 1 1 d DU . . H28B H 0.7225 1.2583 0.6660 0.128 Uiso 1 1 calc R . . C284 C 0.8539(12) 1.2665(8) 0.5992(7) 0.129(4) Uani 1 1 d DU . . H28C H 0.8449 1.3192 0.5864 0.155 Uiso 1 1 calc R . . C285 C 0.9383(11) 1.2219(7) 0.5705(6) 0.107(4) Uani 1 1 d DU . . H28D H 0.9853 1.2438 0.5360 0.129 Uiso 1 1 calc R . . C286 C 0.9511(9) 1.1450(6) 0.5940(5) 0.090(3) Uani 1 1 d DU . . H28E H 1.0085 1.1151 0.5748 0.108 Uiso 1 1 calc R . . N291 N 0.6305(6) 1.1547(5) 0.7413(4) 0.071(2) Uani 1 1 d DU . . C292 C 0.7270(7) 1.1117(6) 0.7219(4) 0.073(3) Uani 1 1 d DU . . C293 C 0.7549(7) 1.0356(5) 0.7483(4) 0.063(3) Uani 1 1 d DU . . H29B H 0.8225 1.0085 0.7343 0.076 Uiso 1 1 calc R . . C294 C 0.6819(7) 0.9985(6) 0.7961(4) 0.063(2) Uani 1 1 d DU . . C295 C 0.5829(7) 1.0451(6) 0.8139(5) 0.068(3) Uani 1 1 d DU . . H29C H 0.5301 1.0234 0.8450 0.082 Uiso 1 1 calc R . . C296 C 0.5630(8) 1.1190(6) 0.7874(5) 0.071(3) Uani 1 1 d DU . . N301 N 0.3895(7) 1.1343(6) 0.8569(4) 0.096(3) Uani 1 1 d DU . . C302 C 0.4558(7) 1.1705(6) 0.8067(4) 0.076(3) Uani 1 1 d DU . . C303 C 0.4377(9) 1.2451(7) 0.7764(6) 0.107(4) Uani 1 1 d DU . . H30B H 0.4866 1.2655 0.7422 0.129 Uiso 1 1 calc R . . C304 C 0.3393(10) 1.2923(7) 0.7989(7) 0.121(4) Uani 1 1 d DU . . H30A H 0.3221 1.3442 0.7802 0.145 Uiso 1 1 calc R . . C305 C 0.2710(10) 1.2551(8) 0.8508(7) 0.120(4) Uani 1 1 d DU . . H30E H 0.2071 1.2830 0.8672 0.144 Uiso 1 1 calc R . . C306 C 0.2968(10) 1.1795(8) 0.8771(6) 0.109(4) Uani 1 1 d DU . . H30F H 0.2487 1.1571 0.9108 0.131 Uiso 1 1 calc R . . P2 P 0.2763(3) 0.11038(19) 0.49721(13) 0.0836(10) Uani 1 1 d U . . F21 F 0.3178(8) 0.1609(4) 0.4275(3) 0.133(3) Uani 1 1 d U . . F22 F 0.1524(7) 0.1618(5) 0.4849(3) 0.157(3) Uani 1 1 d U . . F23 F 0.3169(9) 0.1691(4) 0.5359(3) 0.138(2) Uani 1 1 d U . . F24 F 0.2384(6) 0.0528(4) 0.4586(3) 0.1149(19) Uani 1 1 d U . . F25 F 0.4046(5) 0.0641(4) 0.5084(3) 0.100(2) Uani 1 1 d U . . F26 F 0.2357(5) 0.0617(4) 0.5672(3) 0.0858(18) Uani 1 1 d U . . P3 P 0.4427(3) 0.4202(2) 0.9208(2) 0.1095(13) Uani 1 1 d U . . F31 F 0.4708(14) 0.3340(6) 0.9198(8) 0.272(4) Uani 1 1 d U . . F32 F 0.4308(13) 0.5034(5) 0.9241(7) 0.245(4) Uani 1 1 d U . . F33 F 0.3083(8) 0.4211(9) 0.9310(6) 0.270(5) Uani 1 1 d U . . F34 F 0.4604(7) 0.3916(6) 0.9982(4) 0.181(3) Uani 1 1 d U . . F35 F 0.5786(7) 0.4194(6) 0.9147(5) 0.176(3) Uani 1 1 d U . . F36 F 0.4233(9) 0.4498(7) 0.8426(5) 0.204(4) Uani 1 1 d U . . P1 P 0.9722(3) 0.26491(19) 0.9642(2) 0.0743(13) Uani 0.686(4) 1 d PDU A 1 F11 F 1.0775(6) 0.1919(4) 0.9699(5) 0.094(3) Uani 0.686(4) 1 d PDU A 1 F12 F 1.0731(8) 0.3167(5) 0.9602(5) 0.122(3) Uani 0.686(4) 1 d PDU A 1 F13 F 0.9736(7) 0.2532(4) 1.0433(4) 0.084(2) Uani 0.686(4) 1 d PDU A 1 F14 F 0.8593(8) 0.3334(4) 0.9498(5) 0.121(3) Uani 0.686(4) 1 d PDU A 1 F15 F 0.9718(9) 0.2791(6) 0.8837(4) 0.113(3) Uani 0.686(4) 1 d PDU A 1 F16 F 0.8722(5) 0.2060(3) 0.9674(3) 0.0573(18) Uani 0.686(4) 1 d PDU A 1 C1 C 0.743(2) 0.3706(9) 0.7879(16) 0.095(10) Uani 0.314(4) 1 d PDU A 2 C2 C 0.7093(14) 0.2918(11) 0.8319(15) 0.077(8) Uani 0.314(4) 1 d PDU A 2 C3 C 0.910(2) 0.2609(13) 0.9172(10) 0.060 Uiso 0.314(4) 1 d PDU A 2 C4 C 1.0313(17) 0.2039(15) 0.9102(12) 0.060 Uiso 0.314(4) 1 d PDU A 2 O O 0.8499(11) 0.2493(10) 0.8473(7) 0.077(6) Uani 0.314(4) 1 d PDU A 2 O1 O 0.8824(7) 0.6435(5) 0.7527(4) 0.104(3) Uani 1 1 d U . . N400 N 0.3221(11) 0.7532(7) 0.6431(7) 0.158(5) Uani 1 1 d U . . C401 C 0.3236(13) 0.8096(9) 0.6019(8) 0.123(5) Uani 1 1 d U . . C402 C 0.3216(13) 0.8778(9) 0.5510(8) 0.133(5) Uani 1 1 d U . . O2 O 0.519(3) 0.288(2) 0.5453(17) 0.273(15) Uani 0.50 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0313(4) 0.1279(7) 0.0598(4) -0.0397(4) 0.0114(3) -0.0092(4) N111 0.036(4) 0.204(4) 0.056(3) -0.047(3) 0.020(3) -0.039(4) C112 0.031(5) 0.233(4) 0.058(4) -0.019(4) 0.007(4) -0.025(6) C113 0.034(5) 0.313(6) 0.059(5) -0.021(5) 0.013(4) -0.036(7) C114 0.040(6) 0.393(6) 0.114(7) -0.097(5) 0.016(6) -0.066(8) C115 0.101(8) 0.377(6) 0.106(6) -0.120(7) 0.040(6) -0.130(9) C116 0.064(5) 0.297(6) 0.091(5) -0.104(5) 0.051(4) -0.117(6) N121 0.025(4) 0.135(3) 0.065(4) -0.023(3) 0.009(3) 0.002(3) C122 0.032(5) 0.170(4) 0.062(5) -0.015(4) 0.013(4) 0.019(5) C123 0.051(6) 0.174(5) 0.094(7) -0.001(5) 0.006(5) 0.052(6) C124 0.106(9) 0.123(6) 0.114(8) 0.007(5) 0.004(6) 0.048(6) C125 0.092(7) 0.090(4) 0.100(6) -0.031(5) 0.011(5) 0.052(5) C126 0.038(5) 0.096(4) 0.070(5) -0.021(4) 0.019(3) 0.018(4) N131 0.032(3) 0.074(3) 0.060(3) -0.025(3) 0.004(3) 0.006(3) C132 0.042(5) 0.074(4) 0.075(4) -0.034(3) 0.011(3) 0.012(4) C133 0.062(6) 0.069(4) 0.096(5) -0.050(4) 0.004(4) 0.019(4) C134 0.066(6) 0.102(5) 0.089(6) -0.046(5) 0.000(5) 0.010(5) C135 0.046(5) 0.092(5) 0.080(5) -0.030(5) -0.007(4) 0.014(5) C136 0.052(5) 0.095(5) 0.052(4) -0.021(4) 0.006(4) 0.006(5) N211 0.039(3) 0.134(4) 0.047(3) -0.032(3) 0.010(3) -0.015(3) C212 0.049(4) 0.133(4) 0.049(5) -0.034(4) 0.005(3) -0.020(4) C213 0.050(5) 0.127(5) 0.049(5) -0.028(5) 0.003(4) -0.021(4) C214 0.051(5) 0.148(6) 0.057(5) -0.035(5) 0.015(4) -0.018(5) C215 0.046(5) 0.133(5) 0.047(5) -0.041(5) -0.001(4) -0.004(5) C216 0.041(4) 0.136(5) 0.049(5) -0.036(5) 0.001(3) -0.007(4) N221 0.055(4) 0.119(3) 0.069(4) -0.051(3) 0.015(3) -0.028(3) C222 0.054(5) 0.128(4) 0.059(5) -0.035(4) 0.012(4) -0.020(4) C223 0.066(5) 0.135(4) 0.056(5) -0.032(5) 0.004(4) -0.024(4) C224 0.106(7) 0.132(4) 0.049(5) -0.042(4) 0.005(5) -0.012(5) C225 0.070(6) 0.128(5) 0.069(6) -0.044(4) 0.010(4) -0.001(5) C226 0.070(5) 0.114(4) 0.078(5) -0.065(4) 0.024(4) -0.029(4) N231 0.037(3) 0.118(4) 0.067(4) -0.045(3) 0.013(3) -0.020(3) C232 0.057(5) 0.125(5) 0.090(6) -0.045(4) 0.024(4) -0.002(5) C233 0.060(6) 0.157(6) 0.089(6) -0.050(5) 0.015(4) 0.025(5) C234 0.080(7) 0.191(6) 0.114(7) -0.080(6) 0.040(5) -0.009(6) C235 0.041(5) 0.189(6) 0.083(6) -0.049(6) 0.021(4) -0.017(6) C236 0.037(5) 0.147(6) 0.076(6) -0.039(5) 0.016(4) -0.024(5) C241 0.140(10) 0.135(5) 0.075(6) -0.044(4) 0.025(6) -0.017(5) C242 0.120(9) 0.145(6) 0.102(7) -0.032(5) 0.018(6) 0.008(7) C243 0.136(10) 0.143(6) 0.106(7) -0.034(5) 0.008(6) 0.009(7) C244 0.148(10) 0.162(5) 0.069(6) -0.033(5) -0.012(6) 0.008(6) C245 0.222(12) 0.134(6) 0.087(7) -0.041(5) 0.041(7) -0.020(7) C246 0.187(12) 0.144(6) 0.080(7) -0.031(5) 0.036(6) -0.020(8) C247 0.218(12) 0.143(5) 0.083(6) -0.046(4) 0.012(7) -0.006(7) N250 0.197(6) 0.198(5) 0.115(6) -0.087(5) 0.017(6) -0.009(7) C251 0.205(7) 0.301(15) 0.191(9) -0.106(8) 0.050(8) -0.120(9) C252 0.130(11) 0.217(14) 0.144(8) -0.041(7) 0.009(7) -0.002(10) C254 0.133(9) 0.091(8) 0.138(7) -0.051(6) -0.031(6) 0.014(7) C255 0.163(6) 0.218(17) 0.126(8) 0.013(11) -0.002(7) -0.001(11) O256 0.205(6) 0.149(9) 0.181(8) 0.026(8) 0.056(6) 0.047(8) C257 0.195(7) 0.071(8) 0.138(9) 0.028(8) 0.031(6) 0.001(7) C258 0.182(6) 0.096(5) 0.144(11) -0.031(6) 0.018(8) 0.000(7) N259 0.090(5) 0.085(4) 0.126(7) -0.030(4) 0.010(5) -0.008(5) C260 0.077(5) 0.161(10) 0.148(6) -0.038(6) 0.009(6) -0.017(6) C261 0.124(9) 0.185(13) 0.192(6) -0.051(7) -0.024(6) -0.034(9) O262 0.149(8) 0.112(6) 0.145(4) -0.035(5) -0.054(5) 0.008(6) C263 0.224(8) 0.197(13) 0.204(6) -0.099(7) -0.062(7) -0.025(11) C264 0.289(6) 0.26(2) 0.154(7) -0.070(11) -0.048(7) 0.033(15) O265 0.274(5) 0.112(7) 0.101(6) -0.025(6) -0.011(5) 0.016(8) C266 0.366(6) 0.115(11) 0.083(8) -0.010(8) 0.026(6) 0.076(10) C267 0.328(6) 0.165(7) 0.169(13) -0.082(7) 0.102(8) 0.003(10) C270 0.075(6) 0.106(4) 0.098(7) -0.021(4) 0.025(5) -0.025(5) C271 0.049(5) 0.095(4) 0.077(5) -0.023(4) 0.004(4) -0.020(4) C272 0.057(6) 0.109(5) 0.078(5) -0.034(4) 0.025(4) -0.033(5) C273 0.049(5) 0.102(5) 0.086(5) -0.038(4) 0.026(4) -0.030(5) C274 0.038(5) 0.101(4) 0.066(5) -0.027(4) 0.004(4) -0.007(4) C275 0.046(5) 0.107(5) 0.065(5) -0.015(4) 0.012(4) 0.005(5) C276 0.057(6) 0.105(5) 0.075(5) -0.027(4) 0.018(5) 0.005(5) N281 0.064(5) 0.105(5) 0.083(5) 0.004(4) 0.032(4) 0.017(4) C282 0.039(4) 0.101(5) 0.080(6) -0.006(4) 0.012(4) 0.010(4) C283 0.075(7) 0.103(5) 0.123(8) -0.008(6) 0.027(5) 0.014(6) C284 0.121(9) 0.101(6) 0.122(9) 0.021(6) 0.049(7) 0.039(6) C285 0.095(7) 0.096(5) 0.098(8) 0.017(6) 0.026(6) 0.025(6) C286 0.063(6) 0.095(5) 0.083(6) 0.012(6) 0.032(5) 0.027(5) N291 0.047(4) 0.100(5) 0.060(4) -0.024(4) 0.009(3) 0.016(4) C292 0.037(4) 0.095(5) 0.071(6) -0.010(4) 0.008(4) 0.029(4) C293 0.031(4) 0.082(4) 0.071(6) -0.018(4) 0.004(4) 0.010(4) C294 0.031(4) 0.109(4) 0.048(5) -0.023(4) -0.008(4) 0.004(4) C295 0.026(4) 0.112(4) 0.069(6) -0.029(5) 0.002(4) -0.007(4) C296 0.036(4) 0.113(5) 0.060(5) -0.026(5) 0.002(3) 0.008(4) N301 0.041(4) 0.176(6) 0.064(5) -0.036(4) 0.006(3) 0.016(4) C302 0.035(4) 0.126(5) 0.082(5) -0.057(5) 0.001(3) -0.003(4) C303 0.050(6) 0.120(5) 0.166(9) -0.071(5) 0.031(5) -0.002(5) C304 0.066(7) 0.139(6) 0.177(10) -0.089(5) 0.036(6) 0.002(5) C305 0.043(6) 0.187(6) 0.146(9) -0.083(7) 0.014(5) 0.002(6) C306 0.044(5) 0.194(7) 0.087(7) -0.053(6) 0.006(5) 0.019(6) P2 0.0710(18) 0.114(2) 0.0538(15) -0.0242(15) 0.0049(14) 0.0292(17) F21 0.179(6) 0.136(5) 0.059(3) -0.007(3) 0.033(4) 0.029(4) F22 0.129(4) 0.224(6) 0.067(4) -0.019(4) -0.004(3) 0.113(4) F23 0.209(6) 0.133(4) 0.077(4) -0.036(3) 0.033(4) -0.027(4) F24 0.082(4) 0.176(4) 0.089(3) -0.053(3) -0.010(3) 0.009(4) F25 0.044(3) 0.165(5) 0.078(4) -0.024(3) 0.005(3) 0.021(3) F26 0.050(3) 0.131(4) 0.062(3) -0.012(3) 0.007(3) 0.012(3) P3 0.081(2) 0.104(2) 0.130(3) -0.007(2) 0.008(2) -0.006(2) F31 0.353(9) 0.125(4) 0.362(9) -0.086(5) -0.050(11) -0.059(5) F32 0.293(9) 0.113(4) 0.307(8) -0.064(4) -0.061(10) 0.072(5) F33 0.078(4) 0.444(10) 0.190(7) 0.120(9) -0.017(4) -0.036(5) F34 0.095(5) 0.273(8) 0.129(4) 0.000(5) -0.001(4) 0.047(6) F35 0.090(4) 0.221(7) 0.216(7) -0.046(7) 0.032(4) -0.034(4) F36 0.179(7) 0.303(8) 0.127(4) -0.003(5) 0.012(4) -0.099(8) P1 0.061(2) 0.046(2) 0.103(3) 0.000(2) 0.048(2) -0.0030(17) F11 0.048(4) 0.086(4) 0.138(6) -0.025(4) 0.035(4) 0.009(3) F12 0.155(5) 0.105(5) 0.120(6) -0.026(5) 0.029(5) -0.062(4) F13 0.064(5) 0.082(5) 0.116(4) -0.040(4) 0.026(4) -0.020(4) F14 0.153(5) 0.036(4) 0.135(6) 0.020(4) 0.092(5) 0.036(4) F15 0.089(6) 0.150(8) 0.096(4) -0.030(4) 0.011(4) -0.001(5) F16 0.042(3) 0.055(3) 0.070(4) -0.022(3) 0.016(3) 0.022(3) C1 0.055(17) 0.089(10) 0.13(2) -0.029(11) 0.021(15) 0.013(9) C2 0.041(9) 0.074(12) 0.13(2) -0.054(12) -0.018(15) -0.012(10) O 0.069(9) 0.120(12) 0.034(9) -0.032(9) 0.005(9) 0.028(10) O1 0.102(6) 0.115(6) 0.093(5) -0.023(5) 0.010(5) -0.013(5) N400 0.105(9) 0.134(7) 0.201(12) -0.007(6) 0.028(9) 0.031(8) C401 0.091(9) 0.139(8) 0.125(10) -0.025(6) 0.004(8) 0.019(9) C402 0.100(10) 0.151(9) 0.131(11) -0.011(7) -0.006(9) -0.005(9) O2 0.18(2) 0.38(3) 0.25(2) -0.10(2) -0.097(19) 0.03(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N121 1.941(9) . ? Ru1 N221 2.009(8) . ? Ru1 N111 2.073(8) . ? Ru1 N131 2.081(7) . ? Ru1 N211 2.082(7) . ? Ru1 N231 2.108(7) . ? N111 C112 1.307(15) . ? N111 C116 1.357(15) . ? C112 C113 1.420(10) . ? C112 C122 1.467(18) . ? C113 C114 1.419(12) . ? C114 C115 1.419(12) . ? C115 C116 1.409(11) . ? N121 C126 1.332(13) . ? N121 C122 1.387(11) . ? C122 C123 1.403(18) . ? C123 C124 1.34(2) . ? C124 C125 1.366(17) . ? C125 C126 1.437(15) . ? C126 C132 1.494(12) . ? N131 C136 1.312(10) . ? N131 C132 1.361(11) . ? C132 C133 1.402(14) . ? C133 C134 1.382(13) . ? C134 C135 1.358(14) . ? C135 C136 1.396(14) . ? N211 C216 1.352(12) . ? N211 C212 1.378(13) . ? C212 C213 1.386(12) . ? C212 C222 1.458(14) . ? C213 C214 1.369(14) . ? C214 C215 1.359(14) . ? C215 C216 1.383(13) . ? N221 C222 1.321(12) . ? N221 C226 1.382(13) . ? C222 C223 1.394(14) . ? C223 C224 1.415(15) . ? C224 C225 1.390(15) . ? C224 C241 1.479(16) . ? C225 C226 1.313(14) . ? C226 C232 1.421(14) . ? N231 C236 1.370(12) . ? N231 C232 1.359(13) . ? C232 C233 1.399(14) . ? C233 C234 1.346(17) . ? C234 C235 1.397(19) . ? C235 C236 1.433(15) . ? C241 C246 1.358(17) . ? C241 C242 1.465(17) . ? C242 C243 1.414(17) . ? C243 C244 1.336(18) . ? C244 C245 1.44(2) . ? C244 C247 1.503(18) . ? C245 C246 1.376(18) . ? C247 N250 1.488(17) . ? N250 C267 1.411(12) . ? N250 C251 1.437(12) . ? C251 C252 1.396(12) . ? C252 O253 1.387(10) . ? O253 C254 1.381(9) . ? C254 C255 1.430(11) . ? C255 O256 1.355(10) . ? O256 C257 1.396(11) . ? C257 C258 1.459(11) . ? C258 N259 1.441(10) . ? N259 C260 1.460(10) . ? N259 C270 1.532(15) . ? C260 C261 1.456(12) . ? C261 O262 1.396(11) . ? O262 C263 1.396(11) . ? C263 C264 1.422(13) . ? C264 O265 1.413(13) . ? O265 C266 1.428(12) . ? C266 C267 1.441(12) . ? C270 C271 1.452(14) . ? C271 C276 1.389(13) . ? C271 C272 1.412(14) . ? C272 C273 1.347(13) . ? C273 C274 1.404(13) . ? C274 C275 1.383(13) . ? C274 C294 1.514(13) . ? C275 C276 1.333(14) . ? N281 C282 1.346(12) . ? N281 C286 1.349(13) . ? C282 C283 1.368(15) . ? C282 C292 1.458(13) . ? C283 C284 1.385(17) . ? C284 C285 1.380(17) . ? C285 C286 1.365(15) . ? N291 C296 1.321(12) . ? N291 C292 1.363(11) . ? C292 C293 1.361(12) . ? C293 C294 1.394(12) . ? C294 C295 1.406(13) . ? C295 C296 1.321(14) . ? C296 C302 1.533(13) . ? N301 C302 1.366(12) . ? N301 C306 1.362(14) . ? C302 C303 1.347(14) . ? C303 C304 1.448(16) . ? C304 C305 1.408(18) . ? C305 C306 1.352(18) . ? P2 F22 1.567(7) . ? P2 F24 1.571(8) . ? P2 F25 1.569(6) . ? P2 F26 1.599(6) . ? P2 F23 1.601(9) . ? P2 F21 1.611(7) . ? P3 F32 1.526(10) . ? P3 F33 1.542(10) . ? P3 F35 1.553(9) . ? P3 F34 1.553(9) . ? P3 F36 1.572(10) . ? P3 F31 1.568(11) . ? P1 F13 1.579(8) . ? P1 F12 1.588(9) . ? P1 F15 1.605(8) . ? P1 F14 1.635(7) . ? P1 F11 1.642(7) . ? P1 F16 1.675(7) . ? C1 C2 1.61(2) . ? C2 O 1.677(18) . ? C3 C4 1.63(2) . ? C3 O 1.67(2) . ? N400 C401 1.172(18) . ? C401 C402 1.423(19) . ? 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 N121 Ru1 N221 178.2(3) . . ? N121 Ru1 N111 78.0(4) . . ? N221 Ru1 N111 103.4(4) . . ? N121 Ru1 N131 79.9(3) . . ? N221 Ru1 N131 98.7(3) . . ? N111 Ru1 N131 157.8(4) . . ? N121 Ru1 N211 100.4(3) . . ? N221 Ru1 N211 78.4(3) . . ? N111 Ru1 N211 94.5(3) . . ? N131 Ru1 N211 90.8(3) . . ? N121 Ru1 N231 103.3(3) . . ? N221 Ru1 N231 77.9(3) . . ? N111 Ru1 N231 89.7(3) . . ? N131 Ru1 N231 94.0(3) . . ? N211 Ru1 N231 156.3(3) . . ? C112 N111 C116 119.6(9) . . ? C112 N111 Ru1 114.0(8) . . ? C116 N111 Ru1 126.3(7) . . ? N111 C112 C113 126.2(11) . . ? N111 C112 C122 118.5(8) . . ? C113 C112 C122 115.3(11) . . ? C114 C113 C112 108.8(11) . . ? C113 C114 C115 131.0(11) . . ? C116 C115 C114 108.8(12) . . ? N111 C116 C115 125.5(11) . . ? C126 N121 C122 118.3(10) . . ? C126 N121 Ru1 120.4(6) . . ? C122 N121 Ru1 121.3(8) . . ? N121 C122 C123 118.4(12) . . ? N121 C122 C112 108.1(10) . . ? C123 C122 C112 133.4(10) . . ? C124 C123 C122 120.5(11) . . ? C123 C124 C125 124.4(14) . . ? C124 C125 C126 112.7(12) . . ? N121 C126 C125 125.7(9) . . ? N121 C126 C132 111.6(9) . . ? C125 C126 C132 122.7(10) . . ? C136 N131 C132 121.0(8) . . ? C136 N131 Ru1 127.1(7) . . ? C132 N131 Ru1 111.9(5) . . ? N131 C132 C133 119.6(8) . . ? N131 C132 C126 116.1(9) . . ? C133 C132 C126 124.3(9) . . ? C134 C133 C132 118.7(9) . . ? C135 C134 C133 120.4(11) . . ? C134 C135 C136 118.8(9) . . ? N131 C136 C135 121.5(10) . . ? C216 N211 C212 121.2(8) . . ? C216 N211 Ru1 126.5(7) . . ? C212 N211 Ru1 112.2(6) . . ? N211 C212 C213 117.8(9) . . ? N211 C212 C222 117.2(8) . . ? C213 C212 C222 125.0(10) . . ? C214 C213 C212 121.7(10) . . ? C215 C214 C213 118.9(9) . . ? C214 C215 C216 120.6(10) . . ? N211 C216 C215 119.9(10) . . ? C222 N221 C226 122.3(9) . . ? C222 N221 Ru1 119.9(7) . . ? C226 N221 Ru1 117.7(7) . . ? N221 C222 C223 119.5(9) . . ? N221 C222 C212 112.1(9) . . ? C223 C222 C212 128.4(9) . . ? C222 C223 C224 118.9(10) . . ? C225 C224 C223 117.7(11) . . ? C225 C224 C241 123.2(11) . . ? C223 C224 C241 119.1(10) . . ? C226 C225 C224 122.0(11) . . ? C225 C226 N221 119.5(10) . . ? C225 C226 C232 126.8(10) . . ? N221 C226 C232 113.7(9) . . ? C236 N231 C232 121.2(8) . . ? C236 N231 Ru1 124.7(7) . . ? C232 N231 Ru1 113.6(6) . . ? N231 C232 C233 118.8(10) . . ? N231 C232 C226 116.5(9) . . ? C233 C232 C226 124.7(11) . . ? C234 C233 C232 121.9(13) . . ? C233 C234 C235 120.3(12) . . ? C234 C235 C236 117.7(11) . . ? N231 C236 C235 120.0(11) . . ? C246 C241 C242 113.0(12) . . ? C246 C241 C224 127.0(12) . . ? C242 C241 C224 119.9(11) . . ? C243 C242 C241 121.4(12) . . ? C244 C243 C242 120.9(14) . . ? C243 C244 C245 120.0(14) . . ? C243 C244 C247 120.6(14) . . ? C245 C244 C247 119.3(12) . . ? C246 C245 C244 116.5(14) . . ? C241 C246 C245 127.9(15) . . ? N250 C247 C244 107.5(10) . . ? C267 N250 C251 112.4(11) . . ? C267 N250 C247 107.0(10) . . ? C251 N250 C247 111.4(11) . . ? C252 C251 N250 124.0(10) . . ? C251 C252 O253 113.7(10) . . ? C254 O253 C252 118.2(10) . . ? O253 C254 C255 110.4(9) . . ? O256 C255 C254 113.4(9) . . ? C255 O256 C257 125.9(9) . . ? O256 C257 C258 108.2(9) . . ? N259 C258 C257 118.3(9) . . ? C258 N259 C260 109.8(8) . . ? C258 N259 C270 109.3(9) . . ? C260 N259 C270 110.6(8) . . ? C261 C260 N259 115.4(9) . . ? O262 C261 C260 107.5(9) . . ? C261 O262 C263 117.6(10) . . ? O262 C263 C264 112.2(11) . . ? O265 C264 C263 111.1(10) . . ? C264 O265 C266 113.7(8) . . ? O265 C266 C267 108.6(10) . . ? N250 C267 C266 120.6(11) . . ? C271 C270 N259 112.1(9) . . ? C276 C271 C272 114.6(9) . . ? C276 C271 C270 124.5(10) . . ? C272 C271 C270 120.9(9) . . ? C273 C272 C271 122.5(9) . . ? C272 C273 C274 120.3(10) . . ? C275 C274 C273 118.0(9) . . ? C275 C274 C294 120.9(8) . . ? C273 C274 C294 121.1(9) . . ? C276 C275 C274 120.3(9) . . ? C275 C276 C271 124.3(10) . . ? C282 N281 C286 118.7(9) . . ? N281 C282 C283 119.5(9) . . ? N281 C282 C292 117.0(9) . . ? C283 C282 C292 123.5(9) . . ? C282 C283 C284 122.3(11) . . ? C285 C284 C283 117.3(12) . . ? C286 C285 C284 118.5(11) . . ? N281 C286 C285 123.6(10) . . ? C296 N291 C292 116.9(8) . . ? C293 C292 N291 122.8(8) . . ? C293 C292 C282 121.4(8) . . ? N291 C292 C282 115.9(8) . . ? C292 C293 C294 119.8(8) . . ? C293 C294 C295 115.3(9) . . ? C293 C294 C274 121.5(8) . . ? C295 C294 C274 123.3(8) . . ? C296 C295 C294 121.6(9) . . ? N291 C296 C295 123.7(9) . . ? N291 C296 C302 114.2(9) . . ? C295 C296 C302 122.1(9) . . ? C302 N301 C306 115.4(10) . . ? N301 C302 C303 126.3(9) . . ? N301 C302 C296 114.1(9) . . ? C303 C302 C296 119.5(9) . . ? C302 C303 C304 117.6(11) . . ? C305 C304 C303 116.2(12) . . ? C306 C305 C304 121.2(12) . . ? C305 C306 N301 123.4(12) . . ? F22 P2 F24 92.5(5) . . ? F22 P2 F25 176.0(5) . . ? F24 P2 F25 90.5(4) . . ? F22 P2 F26 92.0(4) . . ? F24 P2 F26 91.2(4) . . ? F25 P2 F26 90.6(3) . . ? F22 P2 F23 88.1(5) . . ? F24 P2 F23 179.1(5) . . ? F25 P2 F23 88.9(5) . . ? F26 P2 F23 89.5(4) . . ? F22 P2 F21 87.8(4) . . ? F24 P2 F21 90.1(4) . . ? F25 P2 F21 89.5(4) . . ? F26 P2 F21 178.7(5) . . ? F23 P2 F21 89.2(4) . . ? F32 P3 F33 90.8(8) . . ? F32 P3 F35 88.2(7) . . ? F33 P3 F35 176.8(7) . . ? F32 P3 F34 92.6(7) . . ? F33 P3 F34 88.4(6) . . ? F35 P3 F34 88.6(5) . . ? F32 P3 F36 86.9(7) . . ? F33 P3 F36 91.0(6) . . ? F35 P3 F36 92.0(6) . . ? F34 P3 F36 179.2(7) . . ? F32 P3 F31 173.2(8) . . ? F33 P3 F31 95.5(9) . . ? F35 P3 F31 85.4(7) . . ? F34 P3 F31 85.1(7) . . ? F36 P3 F31 95.5(8) . . ? F13 P1 F12 88.9(5) . . ? F13 P1 F15 178.4(6) . . ? F12 P1 F15 89.7(6) . . ? F13 P1 F14 96.0(5) . . ? F12 P1 F14 97.3(5) . . ? F15 P1 F14 83.3(5) . . ? F13 P1 F11 90.5(5) . . ? F12 P1 F11 87.8(5) . . ? F15 P1 F11 90.2(5) . . ? F14 P1 F11 171.7(6) . . ? F13 P1 F16 92.1(4) . . ? F12 P1 F16 176.4(5) . . ? F15 P1 F16 89.3(5) . . ? F14 P1 F16 86.0(4) . . ? F11 P1 F16 88.7(4) . . ? C1 C2 O 95.3(12) . . ? C4 C3 O 93.0(13) . . ? C2 O C3 114.5(16) . . ? N400 C401 C402 178.0(18) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.218 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.153