# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1933 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 crystal structure in the paper 'Switching of the inter-component photoinduced...' by Susana Encinas, et al, submitted to Dalton Transactions for publication. ; #=============================================================== data_boxes _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C58.50 H70 F18 N10 O6.50 P3 Ru' _chemical_formula_weight 1553.22 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7188(14) _cell_length_b 13.5675(13) _cell_length_c 22.289(3) _cell_angle_alpha 77.372(10) _cell_angle_beta 85.719(10) _cell_angle_gamma 62.299(7) _cell_volume 3321.4(7) _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 block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method ? _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 0.417 _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.88 _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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33735 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14970 _reflns_number_observed 10706 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+0.1793P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14970 _refine_ls_number_parameters 883 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_obs 0.0561 _refine_ls_wR_factor_all 0.1724 _refine_ls_wR_factor_obs 0.1555 _refine_ls_goodness_of_fit_all 1.041 _refine_ls_goodness_of_fit_obs 1.120 _refine_ls_restrained_S_all 1.041 _refine_ls_restrained_S_obs 1.119 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.72700(2) -0.43316(2) 0.347815(13) 0.03079(10) Uani 1 d . . O1 O 0.1599(2) 0.1289(2) 0.23391(12) 0.0442(6) Uani 1 d . . N111 N 0.7890(2) -0.3733(3) 0.40716(14) 0.0361(7) Uani 1 d . . C112 C 0.7218(3) -0.3458(3) 0.4568(2) 0.0396(8) Uani 1 d . . C113 C 0.7587(4) -0.3148(4) 0.5031(2) 0.0599(12) Uani 1 d . . H11A H 0.7115(4) -0.2963(4) 0.5380(2) 0.072 Uiso 1 calc R . C114 C 0.8660(5) -0.3115(6) 0.4976(3) 0.086(2) Uani 1 d . . H11B H 0.8934(5) -0.2915(6) 0.5293(3) 0.103 Uiso 1 calc R . C115 C 0.9327(4) -0.3367(5) 0.4472(2) 0.0655(14) Uani 1 d . . H11C H 1.0055(4) -0.3325(5) 0.4426(2) 0.079 Uiso 1 calc R . C116 C 0.8921(3) -0.3681(4) 0.4032(2) 0.0455(9) Uani 1 d . . H11D H 0.9390(3) -0.3870(4) 0.3683(2) 0.055 Uiso 1 calc R . N121 N 0.5976(2) -0.4009(2) 0.41266(13) 0.0340(6) Uani 1 d . . C122 C 0.6097(3) -0.3540(3) 0.4583(2) 0.0357(8) Uani 1 d . . C123 C 0.5226(3) -0.3171(3) 0.5010(2) 0.0413(8) Uani 1 d . . H12A H 0.5335(3) -0.2850(3) 0.5324(2) 0.050 Uiso 1 calc R . C124 C 0.4200(3) -0.3269(3) 0.4980(2) 0.0440(9) Uani 1 d . . H12B H 0.3596(3) -0.3016(3) 0.5269(2) 0.053 Uiso 1 calc R . C125 C 0.4071(3) -0.3744(3) 0.4519(2) 0.0426(9) Uani 1 d . . H12C H 0.3376(3) -0.3825(3) 0.4488(2) 0.051 Uiso 1 calc R . C126 C 0.4964(3) -0.4100(3) 0.4106(2) 0.0380(8) Uani 1 d . . H12D H 0.4864(3) -0.4424(3) 0.3791(2) 0.046 Uiso 1 calc R . N211 N 0.8630(2) -0.4656(2) 0.28625(13) 0.0314(6) Uani 1 d . . C212 C 0.9519(3) -0.5757(3) 0.2971(2) 0.0312(7) Uani 1 d . . C213 C 1.0445(3) -0.6103(3) 0.2568(2) 0.0377(8) Uani 1 d . . H21A H 1.1053(3) -0.6869(3) 0.2644(2) 0.045 Uiso 1 calc R . C214 C 1.0485(3) -0.5337(3) 0.2058(2) 0.0448(9) Uani 1 d . . H21B H 1.1112(3) -0.5569(3) 0.1778(2) 0.054 Uiso 1 calc R . C215 C 0.9600(3) -0.4228(4) 0.1962(2) 0.0460(9) Uani 1 d . . H21C H 0.9617(3) -0.3679(4) 0.1619(2) 0.055 Uiso 1 calc R . C216 C 0.8688(3) -0.3925(3) 0.2369(2) 0.0386(8) Uani 1 d . . H21D H 0.8074(3) -0.3162(3) 0.2294(2) 0.046 Uiso 1 calc R . N221 N 0.8481(2) -0.5958(2) 0.38897(13) 0.0331(6) Uani 1 d . . C222 C 0.9423(3) -0.6487(3) 0.3545(2) 0.0326(7) Uani 1 d . . C223 C 1.0241(3) -0.7629(3) 0.3748(2) 0.0405(8) Uani 1 d . . H22A H 1.0880(3) -0.8001(3) 0.3497(2) 0.049 Uiso 1 calc R . C224 C 1.0115(3) -0.8209(3) 0.4311(2) 0.0453(9) Uani 1 d . . H22B H 1.0657(3) -0.8990(3) 0.4451(2) 0.054 Uiso 1 calc R . C225 C 0.9190(3) -0.7649(3) 0.4674(2) 0.0446(9) Uani 1 d . . H22C H 0.9104(3) -0.8030(3) 0.5071(2) 0.054 Uiso 1 calc R . C226 C 0.8396(3) -0.6528(3) 0.4450(2) 0.0398(8) Uani 1 d . . H22D H 0.7763(3) -0.6144(3) 0.4701(2) 0.048 Uiso 1 calc R . N311 N 0.6436(2) -0.4831(2) 0.29382(13) 0.0322(6) Uani 1 d . . C312 C 0.5575(3) -0.3978(3) 0.2541(2) 0.0350(8) Uani 1 d . . C313 C 0.4890(3) -0.4200(3) 0.2182(2) 0.0408(8) Uani 1 d . . H31A H 0.4296(3) -0.3597(3) 0.1902(2) 0.049 Uiso 1 calc R . C314 C 0.5085(4) -0.5304(4) 0.2238(2) 0.0487(10) Uani 1 d . . H31B H 0.4627(4) -0.5468(4) 0.1995(2) 0.058 Uiso 1 calc R . C315 C 0.5952(4) -0.6178(3) 0.2652(2) 0.0459(9) Uani 1 d . . H31C H 0.6086(4) -0.6941(3) 0.2703(2) 0.055 Uiso 1 calc R . C316 C 0.6610(3) -0.5905(3) 0.2986(2) 0.0387(8) Uani 1 d . . H31D H 0.7216(3) -0.6501(3) 0.3263(2) 0.046 Uiso 1 calc R . N321 N 0.6128(2) -0.2792(2) 0.29497(14) 0.0343(6) Uani 1 d . . C322 C 0.5415(3) -0.2828(3) 0.2541(2) 0.0340(8) Uani 1 d . . C323 C 0.4604(3) -0.1834(3) 0.2160(2) 0.0414(9) Uani 1 d . . H32A H 0.4102(3) -0.1865(3) 0.1878(2) 0.050 Uiso 1 calc R . C324 C 0.4537(3) -0.0802(3) 0.2198(2) 0.0448(9) Uani 1 d . . H32B H 0.3988(3) -0.0119(3) 0.1940(2) 0.054 Uiso 1 calc R . C325 C 0.5269(3) -0.0763(3) 0.2611(2) 0.0430(9) Uani 1 d . . C326 C 0.6048(3) -0.1777(3) 0.2977(2) 0.0383(8) Uani 1 d . . H32C H 0.6552(3) -0.1759(3) 0.3263(2) 0.046 Uiso 1 calc R . C410 C 0.5282(3) 0.0345(3) 0.2637(3) 0.0561(12) Uani 1 d . . H41A H 0.5759(3) 0.0219(3) 0.3003(3) 0.067 Uiso 1 calc R . H41B H 0.5672(3) 0.0565(3) 0.2268(3) 0.067 Uiso 1 calc R . N411 N 0.4074(3) 0.1289(3) 0.2666(2) 0.0552(10) Uani 1 d . . C412 C 0.3945(4) 0.2345(4) 0.2242(3) 0.081(2) Uani 1 d . . H41C H 0.3213(4) 0.2994(4) 0.2339(3) 0.097 Uiso 1 calc R . H41D H 0.4626(4) 0.2474(4) 0.2313(3) 0.097 Uiso 1 calc R . C413 C 0.3885(5) 0.2324(4) 0.1586(3) 0.083(2) Uani 1 d . . H41E H 0.3821(5) 0.3044(4) 0.1327(3) 0.100 Uiso 1 calc R . H41F H 0.4620(5) 0.1688(4) 0.1480(3) 0.100 Uiso 1 calc R . O414 O 0.2881(3) 0.2185(3) 0.1466(2) 0.0762(10) Uani 1 d . . C415 C 0.2821(7) 0.2046(8) 0.0845(3) 0.115(3) Uani 1 d . . H41G H 0.3593(7) 0.1450(8) 0.0742(3) 0.139 Uiso 1 calc R . H41H H 0.2642(7) 0.2768(8) 0.0548(3) 0.139 Uiso 1 calc R . C416 C 0.1837(7) 0.1705(6) 0.0805(3) 0.116(3) Uani 1 d . . H41I H 0.1115(7) 0.2191(6) 0.1005(3) 0.140 Uiso 1 calc R . H41J H 0.1631(7) 0.1799(6) 0.0370(3) 0.140 Uiso 1 calc R . O417 O 0.2265(4) 0.0575(5) 0.1104(2) 0.1015(14) Uani 1 d . . C418 C 0.1631(6) 0.0066(6) 0.0941(3) 0.093(2) Uani 1 d . . H41K H 0.2085(6) -0.0768(6) 0.1086(3) 0.112 Uiso 1 calc R . H41L H 0.1559(6) 0.0224(6) 0.0486(3) 0.112 Uiso 1 calc R . C419 C 0.0420(4) 0.0462(5) 0.1195(2) 0.073(2) Uani 1 d . . H41M H 0.0042(4) 0.0041(5) 0.1070(2) 0.088 Uiso 1 calc R . H41N H -0.0064(4) 0.1279(5) 0.1011(2) 0.088 Uiso 1 calc R . N420 N 0.0400(3) 0.0305(3) 0.1897(2) 0.0522(9) Uani 1 d . . C421 C 0.0920(5) -0.0939(4) 0.2190(3) 0.0678(14) Uani 1 d . . H42A H 0.0426(5) -0.1253(4) 0.2065(3) 0.081 Uiso 1 calc R . H42B H 0.1726(5) -0.1341(4) 0.2033(3) 0.081 Uiso 1 calc R . C422 C 0.1001(4) -0.1174(4) 0.2880(3) 0.0702(14) Uani 1 d . . H42C H 0.0217(4) -0.0721(4) 0.3044(3) 0.084 Uiso 1 calc R . H42D H 0.1248(4) -0.1991(4) 0.3051(3) 0.084 Uiso 1 calc R . O423 O 0.1847(3) -0.0875(3) 0.30491(14) 0.0556(7) Uani 1 d . . C424 C 0.1908(4) -0.0964(5) 0.3685(2) 0.0674(14) Uani 1 d . . H42E H 0.1983(4) -0.1712(5) 0.3906(2) 0.081 Uiso 1 calc R . H42F H 0.1171(4) -0.0362(5) 0.3815(2) 0.081 Uiso 1 calc R . C425 C 0.2962(4) -0.0839(4) 0.3841(2) 0.0621(13) Uani 1 d . . H42G H 0.3016(4) -0.0910(4) 0.4291(2) 0.075 Uiso 1 calc R . H42H H 0.3698(4) -0.1451(4) 0.3718(2) 0.075 Uiso 1 calc R . O426 O 0.2846(3) 0.0242(3) 0.35284(14) 0.0552(8) Uani 1 d . . C427 C 0.3727(4) 0.0483(5) 0.3725(2) 0.071(2) Uani 1 d . . H42I H 0.4513(4) -0.0195(5) 0.3750(2) 0.085 Uiso 1 calc R . H42J H 0.3545(4) 0.0656(5) 0.4141(2) 0.085 Uiso 1 calc R . C428 C 0.3774(4) 0.1476(4) 0.3289(3) 0.072(2) Uani 1 d . . H42K H 0.2991(4) 0.2155(4) 0.3276(3) 0.086 Uiso 1 calc R . H42L H 0.4370(4) 0.1637(4) 0.3449(3) 0.086 Uiso 1 calc R . C429 C -0.0855(4) 0.0949(4) 0.2115(2) 0.0605(12) Uani 1 d . . H42M H -0.1304(4) 0.0531(4) 0.2080(2) 0.073 Uiso 1 calc R . H42N H -0.0809(4) 0.0955(4) 0.2555(2) 0.073 Uiso 1 calc R . N511 N -0.3152(4) 0.3556(4) 0.1072(2) 0.0659(11) Uani 1 d . . C512 C -0.2487(4) 0.2464(4) 0.1377(2) 0.0610(12) Uani 1 d . . H51B H -0.2683(4) 0.1894(4) 0.1322(2) 0.073 Uiso 1 calc R . C513 C -0.1533(4) 0.2152(4) 0.1767(2) 0.0510(10) Uani 1 d . . C514 C -0.1276(4) 0.3010(4) 0.1842(2) 0.0564(11) Uani 1 d . . H51C H -0.0635(4) 0.2830(4) 0.2109(2) 0.068 Uiso 1 calc R . C515 C -0.1936(4) 0.4103(3) 0.1538(2) 0.0473(10) Uani 1 d . . H51D H -0.1756(4) 0.4684(3) 0.1591(2) 0.057 Uiso 1 calc R . C516 C -0.2865(4) 0.4358(4) 0.1155(2) 0.0498(10) Uani 1 d . . N521 N -0.3419(4) 0.6381(4) 0.0992(2) 0.0717(12) Uani 1 d . . C522 C -0.4151(5) 0.7491(4) 0.0714(3) 0.0702(14) Uani 1 d . . H52B H -0.4032(5) 0.8078(4) 0.0813(3) 0.084 Uiso 1 calc R . C523 C -0.5037(5) 0.7784(5) 0.0304(3) 0.078(2) Uani 1 d . . H52C H -0.5540(5) 0.8559(5) 0.0126(3) 0.093 Uiso 1 calc R . C524 C -0.5186(5) 0.6935(6) 0.0154(3) 0.081(2) Uani 1 d . . H52D H -0.5790(5) 0.7124(6) -0.0139(3) 0.097 Uiso 1 calc R . C525 C -0.4480(4) 0.5806(4) 0.0419(2) 0.0560(11) Uani 1 d . . H52E H -0.4593(4) 0.5220(4) 0.0312(2) 0.067 Uiso 1 calc R . C526 C -0.3607(4) 0.5551(4) 0.0841(2) 0.0505(10) Uani 1 d . . P1 P 0.23550(10) 0.52009(10) 0.33705(6) 0.0530(3) Uani 1 d . . F11 F 0.2113(3) 0.5518(3) 0.40406(15) 0.0869(10) Uani 1 d . . F12 F 0.3607(2) 0.4179(3) 0.36203(15) 0.0834(9) Uani 1 d . . F13 F 0.1089(2) 0.6240(2) 0.3127(2) 0.0787(9) Uani 1 d . . F14 F 0.1745(3) 0.4384(2) 0.35741(14) 0.0718(8) Uani 1 d . . F15 F 0.2602(2) 0.4885(3) 0.27124(13) 0.0703(8) Uani 1 d . . F16 F 0.2957(2) 0.6028(3) 0.31777(15) 0.0740(8) Uani 1 d . . P2 P -1.23032(12) 0.92955(11) -0.89456(6) 0.0568(3) Uani 1 d . . F21 F -1.3125(4) 0.9549(4) -0.9500(2) 0.131(2) Uani 1 d . . F22 F -1.2810(3) 0.8543(3) -0.8514(2) 0.0987(11) Uani 1 d . . F23 F -1.1412(4) 0.8206(4) -0.9182(2) 0.139(2) Uani 1 d . . F24 F -1.3161(6) 1.0369(4) -0.8726(3) 0.184(3) Uani 1 d . . F25 F -1.1414(5) 0.9003(6) -0.8422(2) 0.177(3) Uani 1 d . . F26 F -1.1748(4) 1.0024(4) -0.9368(2) 0.123(2) Uani 1 d . . P3 P -0.76946(12) 0.94611(11) -0.39816(6) 0.0610(3) Uani 1 d . . F31 F -0.8945(4) 1.0512(4) -0.4102(2) 0.140(2) Uani 1 d . . F32 F -0.8378(4) 0.8767(4) -0.3648(2) 0.134(2) Uani 1 d . . F33 F -0.7846(5) 0.9226(5) -0.4615(2) 0.162(2) Uani 1 d . . F34 F -0.6475(5) 0.8405(5) -0.3900(3) 0.198(3) Uani 1 d . . F35 F -0.7543(5) 0.9564(7) -0.3338(2) 0.207(3) Uani 1 d . . F36 F -0.7077(5) 1.0146(5) -0.4270(4) 0.225(4) Uani 1 d . . C1 C 0.2493(10) 0.5730(9) 0.1014(5) 0.172(5) Uani 1 d . . H1A H 0.2961(10) 0.5359(9) 0.1401(5) 0.258 Uiso 1 calc R . H1B H 0.2962(10) 0.5378(9) 0.0680(5) 0.258 Uiso 1 calc R . H1C H 0.1767(10) 0.5640(9) 0.1052(5) 0.258 Uiso 1 calc R . C2 C 0.2173(7) 0.6952(8) 0.0875(3) 0.111(3) Uani 1 d . . O2 O 0.2526(6) 0.7420(5) 0.1189(3) 0.148(2) Uani 1 d . . C3 C 0.1451(7) 0.7661(8) 0.0296(3) 0.131(3) Uani 1 d . . H3A H 0.1296(7) 0.8452(8) 0.0255(3) 0.196 Uiso 1 calc R . H3B H 0.0695(7) 0.7630(8) 0.0314(3) 0.196 Uiso 1 calc R . H3C H 0.1889(7) 0.7367(8) -0.0058(3) 0.196 Uiso 1 calc R . C60 C 0.1374(27) 0.5387(32) 0.0576(12) 0.344(27) Uani 0.50 d PDU . C61 C 0.0585(29) 0.5338(29) 0.0075(12) 0.248(17) Uani 0.50 d PDU . C62 C 0.0383(19) 0.4667(17) -0.0373(7) 0.254(7) Uani 1 d DU . 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 0.02303(14) 0.0310(2) 0.0382(2) -0.01223(11) 0.00148(10) -0.01026(11) O1 0.0428(15) 0.0380(14) 0.053(2) -0.0157(12) 0.0019(12) -0.0169(12) N111 0.0288(14) 0.036(2) 0.044(2) -0.0141(13) 0.0005(12) -0.0128(13) C112 0.035(2) 0.047(2) 0.042(2) -0.014(2) 0.002(2) -0.022(2) C113 0.062(3) 0.095(4) 0.053(3) -0.040(3) 0.017(2) -0.054(3) C114 0.081(4) 0.157(6) 0.072(3) -0.062(4) 0.017(3) -0.084(4) C115 0.054(3) 0.101(4) 0.071(3) -0.035(3) 0.007(2) -0.053(3) C116 0.034(2) 0.058(3) 0.054(2) -0.022(2) 0.003(2) -0.025(2) N121 0.0268(14) 0.036(2) 0.040(2) -0.0116(13) 0.0010(12) -0.0138(12) C122 0.032(2) 0.034(2) 0.040(2) -0.009(2) -0.0011(14) -0.0133(15) C123 0.040(2) 0.047(2) 0.042(2) -0.018(2) 0.005(2) -0.021(2) C124 0.036(2) 0.048(2) 0.044(2) -0.014(2) 0.010(2) -0.016(2) C125 0.029(2) 0.049(2) 0.051(2) -0.011(2) 0.002(2) -0.019(2) C126 0.029(2) 0.043(2) 0.044(2) -0.013(2) 0.0024(15) -0.017(2) N211 0.0261(14) 0.0307(15) 0.037(2) -0.0092(12) -0.0011(11) -0.0119(12) C212 0.025(2) 0.033(2) 0.037(2) -0.0138(14) -0.0004(13) -0.0113(14) C213 0.031(2) 0.036(2) 0.043(2) -0.016(2) 0.0022(15) -0.011(2) C214 0.036(2) 0.048(2) 0.046(2) -0.012(2) 0.008(2) -0.015(2) C215 0.043(2) 0.048(2) 0.045(2) -0.005(2) 0.008(2) -0.022(2) C216 0.037(2) 0.029(2) 0.045(2) -0.007(2) 0.000(2) -0.012(2) N221 0.0275(14) 0.034(2) 0.039(2) -0.0085(13) 0.0006(12) -0.0150(12) C222 0.026(2) 0.033(2) 0.040(2) -0.0107(15) -0.0020(14) -0.0132(14) C223 0.037(2) 0.034(2) 0.044(2) -0.011(2) 0.000(2) -0.011(2) C224 0.042(2) 0.036(2) 0.054(2) -0.006(2) -0.008(2) -0.016(2) C225 0.043(2) 0.047(2) 0.045(2) 0.001(2) -0.005(2) -0.025(2) C226 0.032(2) 0.046(2) 0.041(2) -0.008(2) 0.0024(15) -0.019(2) N311 0.0275(14) 0.031(2) 0.040(2) -0.0128(12) 0.0034(12) -0.0128(12) C312 0.025(2) 0.038(2) 0.042(2) -0.015(2) 0.0053(14) -0.0129(15) C313 0.033(2) 0.044(2) 0.047(2) -0.016(2) -0.003(2) -0.017(2) C314 0.043(2) 0.053(3) 0.062(3) -0.025(2) 0.002(2) -0.027(2) C315 0.047(2) 0.041(2) 0.060(2) -0.021(2) 0.009(2) -0.025(2) C316 0.037(2) 0.037(2) 0.043(2) -0.011(2) 0.002(2) -0.016(2) N321 0.0251(14) 0.032(2) 0.045(2) -0.0171(13) 0.0029(12) -0.0095(12) C322 0.022(2) 0.037(2) 0.041(2) -0.017(2) 0.0047(13) -0.0089(14) C323 0.029(2) 0.037(2) 0.053(2) -0.014(2) -0.002(2) -0.008(2) C324 0.032(2) 0.035(2) 0.059(2) -0.011(2) -0.001(2) -0.008(2) C325 0.029(2) 0.032(2) 0.067(3) -0.019(2) 0.006(2) -0.010(2) C326 0.027(2) 0.036(2) 0.055(2) -0.020(2) 0.002(2) -0.0121(15) C410 0.035(2) 0.034(2) 0.100(4) -0.019(2) -0.006(2) -0.012(2) N411 0.037(2) 0.032(2) 0.098(3) -0.025(2) -0.005(2) -0.0105(14) C412 0.046(3) 0.027(2) 0.167(6) -0.013(3) -0.011(3) -0.016(2) C413 0.051(3) 0.046(3) 0.137(6) 0.009(3) 0.007(3) -0.022(2) O414 0.062(2) 0.079(3) 0.080(2) 0.000(2) 0.008(2) -0.033(2) C415 0.104(5) 0.159(8) 0.059(4) 0.014(4) 0.014(4) -0.058(5) C416 0.141(7) 0.076(4) 0.081(4) -0.027(4) -0.043(5) 0.004(4) O417 0.103(3) 0.135(4) 0.071(3) -0.032(3) 0.009(2) -0.055(3) C418 0.085(4) 0.122(6) 0.069(4) -0.045(4) 0.005(3) -0.035(4) C419 0.056(3) 0.097(4) 0.069(3) -0.043(3) -0.007(2) -0.025(3) N420 0.043(2) 0.050(2) 0.066(2) -0.027(2) 0.002(2) -0.017(2) C421 0.060(3) 0.047(3) 0.100(4) -0.031(3) -0.006(3) -0.020(2) C422 0.055(3) 0.046(3) 0.109(4) -0.005(3) 0.000(3) -0.027(2) O423 0.055(2) 0.053(2) 0.061(2) -0.0085(15) 0.0062(15) -0.029(2) C424 0.059(3) 0.068(3) 0.054(3) 0.003(2) 0.011(2) -0.021(3) C425 0.051(3) 0.064(3) 0.046(2) -0.005(2) 0.004(2) -0.008(2) O426 0.045(2) 0.053(2) 0.054(2) -0.0179(14) -0.0050(13) -0.0082(14) C427 0.047(3) 0.081(4) 0.072(3) -0.047(3) -0.011(2) -0.004(2) C428 0.044(2) 0.050(3) 0.124(5) -0.051(3) -0.015(3) -0.008(2) C429 0.049(3) 0.052(3) 0.080(3) -0.021(2) 0.008(2) -0.022(2) N511 0.057(2) 0.067(3) 0.077(3) -0.032(2) -0.010(2) -0.022(2) C512 0.053(3) 0.059(3) 0.080(3) -0.034(3) -0.001(2) -0.024(2) C513 0.043(2) 0.049(2) 0.062(3) -0.021(2) 0.002(2) -0.018(2) C514 0.054(3) 0.057(3) 0.063(3) -0.020(2) -0.007(2) -0.026(2) C515 0.048(2) 0.042(2) 0.059(2) -0.012(2) -0.009(2) -0.024(2) C516 0.048(2) 0.054(3) 0.049(2) -0.021(2) 0.000(2) -0.021(2) N521 0.084(3) 0.066(3) 0.071(3) -0.010(2) -0.007(2) -0.040(2) C522 0.081(4) 0.054(3) 0.077(3) -0.007(3) 0.008(3) -0.037(3) C523 0.058(3) 0.069(4) 0.077(4) 0.017(3) 0.000(3) -0.019(3) C524 0.059(3) 0.109(5) 0.063(3) 0.006(3) -0.019(3) -0.036(3) C525 0.048(2) 0.068(3) 0.050(2) -0.010(2) -0.010(2) -0.024(2) C526 0.049(2) 0.061(3) 0.046(2) -0.011(2) 0.002(2) -0.029(2) P1 0.0394(6) 0.0569(7) 0.0713(8) -0.0272(6) 0.0040(5) -0.0236(5) F11 0.076(2) 0.131(3) 0.095(2) -0.070(2) 0.029(2) -0.066(2) F12 0.053(2) 0.087(2) 0.090(2) -0.015(2) -0.010(2) -0.015(2) F13 0.0381(14) 0.066(2) 0.127(3) -0.019(2) 0.0035(15) -0.0209(13) F14 0.078(2) 0.075(2) 0.081(2) -0.019(2) -0.004(2) -0.049(2) F15 0.066(2) 0.085(2) 0.071(2) -0.032(2) 0.0060(14) -0.037(2) F16 0.054(2) 0.080(2) 0.112(2) -0.040(2) 0.017(2) -0.043(2) P2 0.0643(7) 0.0568(7) 0.0559(7) -0.0100(6) -0.0022(6) -0.0335(6) F21 0.149(4) 0.116(3) 0.138(3) 0.045(3) -0.085(3) -0.086(3) F22 0.109(3) 0.101(3) 0.096(2) 0.006(2) 0.004(2) -0.068(2) F23 0.159(4) 0.096(3) 0.109(3) -0.022(2) 0.040(3) -0.021(3) F24 0.224(6) 0.101(4) 0.224(6) -0.082(4) 0.125(5) -0.068(4) F25 0.228(6) 0.267(7) 0.108(3) 0.024(4) -0.077(4) -0.190(6) F26 0.181(4) 0.151(4) 0.095(3) -0.005(2) 0.009(3) -0.135(4) P3 0.0581(7) 0.0550(7) 0.0679(8) -0.0165(6) 0.0019(6) -0.0228(6) F31 0.088(3) 0.096(3) 0.175(4) -0.002(3) 0.023(3) -0.006(2) F32 0.169(4) 0.150(4) 0.119(3) 0.016(3) -0.018(3) -0.119(4) F33 0.169(5) 0.215(6) 0.093(3) -0.067(3) 0.018(3) -0.068(4) F34 0.129(4) 0.161(5) 0.147(4) -0.007(4) 0.002(3) 0.053(3) F35 0.203(6) 0.423(11) 0.135(4) -0.152(6) 0.051(4) -0.226(7) F36 0.154(5) 0.160(5) 0.357(10) 0.018(6) 0.078(6) -0.109(4) C1 0.197(11) 0.137(9) 0.177(10) 0.052(7) -0.041(9) -0.103(8) C2 0.095(5) 0.128(7) 0.077(4) -0.020(5) -0.004(4) -0.023(5) O2 0.147(5) 0.139(5) 0.101(4) -0.047(4) -0.011(4) -0.008(4) C3 0.126(7) 0.164(8) 0.074(4) -0.001(5) -0.014(4) -0.050(6) C60 0.225(30) 0.395(43) 0.098(16) 0.011(23) 0.091(18) 0.076(29) C61 0.255(30) 0.270(28) 0.085(14) -0.045(17) 0.079(19) -0.017(23) C62 0.283(20) 0.292(19) 0.180(14) -0.012(13) -0.022(14) -0.137(17) _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 N321 2.054(3) . ? Ru1 N121 2.059(3) . ? Ru1 N311 2.061(3) . ? Ru1 N221 2.061(3) . ? Ru1 N111 2.062(3) . ? Ru1 N211 2.067(3) . ? N111 C116 1.341(5) . ? N111 C112 1.354(5) . ? C112 C113 1.382(5) . ? C112 C122 1.479(5) . ? C113 C114 1.381(6) . ? C114 C115 1.364(7) . ? C115 C116 1.368(6) . ? N121 C126 1.354(4) . ? N121 C122 1.365(4) . ? C122 C123 1.384(5) . ? C123 C124 1.379(5) . ? C124 C125 1.382(5) . ? C125 C126 1.378(5) . ? N211 C216 1.333(4) . ? N211 C212 1.372(4) . ? C212 C213 1.389(5) . ? C212 C222 1.473(5) . ? C213 C214 1.377(5) . ? C214 C215 1.378(5) . ? C215 C216 1.378(5) . ? N221 C226 1.344(5) . ? N221 C222 1.357(4) . ? C222 C223 1.398(5) . ? C223 C224 1.370(6) . ? C224 C225 1.382(6) . ? C225 C226 1.377(5) . ? N311 C316 1.348(5) . ? N311 C312 1.358(4) . ? C312 C313 1.393(5) . ? C312 C322 1.476(5) . ? C313 C314 1.378(5) . ? C314 C315 1.389(6) . ? C315 C316 1.376(5) . ? N321 C326 1.347(4) . ? N321 C322 1.357(4) . ? C322 C323 1.392(5) . ? C323 C324 1.384(5) . ? C324 C325 1.382(5) . ? C325 C326 1.380(5) . ? C325 C410 1.525(5) . ? C410 N411 1.482(5) . ? N411 C428 1.459(7) . ? N411 C412 1.478(6) . ? C412 C413 1.477(9) . ? C413 O414 1.426(6) . ? O414 C415 1.449(8) . ? C415 C416 1.537(10) . ? C416 O417 1.386(8) . ? O417 C418 1.391(7) . ? C418 C419 1.488(8) . ? C419 N420 1.533(6) . ? N420 C421 1.503(6) . ? N420 C429 1.523(5) . ? C421 C422 1.502(8) . ? C422 O423 1.414(5) . ? O423 C424 1.402(6) . ? C424 C425 1.501(7) . ? C425 O426 1.423(6) . ? O426 C427 1.426(5) . ? C427 C428 1.501(8) . ? C429 C513 1.499(6) . ? N511 C516 1.349(6) . ? N511 C512 1.361(6) . ? C512 C513 1.387(6) . ? C513 C514 1.391(6) . ? C514 C515 1.360(6) . ? C515 C516 1.373(5) . ? C516 C526 1.478(6) . ? N521 C526 1.368(6) . ? N521 C522 1.376(6) . ? C522 C523 1.357(7) . ? C523 C524 1.361(8) . ? C524 C525 1.381(7) . ? C525 C526 1.375(6) . ? P1 F12 1.584(3) . ? P1 F15 1.586(3) . ? P1 F13 1.600(3) . ? P1 F14 1.602(3) . ? P1 F16 1.603(3) . ? P1 F11 1.613(3) . ? P2 F24 1.519(4) . ? P2 F25 1.541(4) . ? P2 F21 1.553(4) . ? P2 F23 1.562(4) . ? P2 F22 1.573(3) . ? P2 F26 1.583(4) . ? P3 F36 1.496(5) . ? P3 F35 1.506(5) . ? P3 F34 1.534(4) . ? P3 F31 1.557(4) . ? P3 F33 1.558(5) . ? P3 F32 1.598(4) . ? C1 C2 1.476(12) . ? C2 O2 1.266(10) . ? C2 C3 1.498(9) . ? C60 C61 1.59(3) . ? C61 C62 1.36(3) 2_565 ? C61 C62 1.60(2) . ? C62 C61 1.36(3) 2_565 ? C62 C62 2.03(4) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N321 Ru1 N121 86.70(11) . . ? N321 Ru1 N311 78.87(11) . . ? N121 Ru1 N311 93.83(11) . . ? N321 Ru1 N221 171.65(11) . . ? N121 Ru1 N221 99.90(11) . . ? N311 Ru1 N221 95.49(11) . . ? N321 Ru1 N111 98.24(11) . . ? N121 Ru1 N111 78.95(11) . . ? N311 Ru1 N111 172.42(11) . . ? N221 Ru1 N111 88.10(11) . . ? N321 Ru1 N211 94.78(11) . . ? N121 Ru1 N211 176.83(10) . . ? N311 Ru1 N211 89.20(11) . . ? N221 Ru1 N211 78.88(11) . . ? N111 Ru1 N211 98.06(11) . . ? C116 N111 C112 118.5(3) . . ? C116 N111 Ru1 126.0(3) . . ? C112 N111 Ru1 115.3(2) . . ? N111 C112 C113 121.3(3) . . ? N111 C112 C122 115.7(3) . . ? C113 C112 C122 123.0(4) . . ? C114 C113 C112 118.4(4) . . ? C115 C114 C113 120.5(4) . . ? C114 C115 C116 118.2(4) . . ? N111 C116 C115 122.9(4) . . ? C126 N121 C122 117.2(3) . . ? C126 N121 Ru1 126.4(2) . . ? C122 N121 Ru1 116.0(2) . . ? N121 C122 C123 121.7(3) . . ? N121 C122 C112 113.8(3) . . ? C123 C122 C112 124.5(3) . . ? C124 C123 C122 120.1(3) . . ? C123 C124 C125 118.5(4) . . ? C126 C125 C124 119.2(3) . . ? N121 C126 C125 123.2(3) . . ? C216 N211 C212 118.5(3) . . ? C216 N211 Ru1 126.6(2) . . ? C212 N211 Ru1 114.8(2) . . ? N211 C212 C213 120.5(3) . . ? N211 C212 C222 114.9(3) . . ? C213 C212 C222 124.6(3) . . ? C214 C213 C212 120.1(3) . . ? C213 C214 C215 118.8(4) . . ? C216 C215 C214 119.1(4) . . ? N211 C216 C215 123.0(3) . . ? C226 N221 C222 118.7(3) . . ? C226 N221 Ru1 125.8(2) . . ? C222 N221 Ru1 115.4(2) . . ? N221 C222 C223 120.8(3) . . ? N221 C222 C212 114.9(3) . . ? C223 C222 C212 124.2(3) . . ? C224 C223 C222 119.6(4) . . ? C223 C224 C225 119.3(4) . . ? C226 C225 C224 118.9(4) . . ? N221 C226 C225 122.5(4) . . ? C316 N311 C312 118.6(3) . . ? C316 N311 Ru1 125.5(2) . . ? C312 N311 Ru1 115.7(2) . . ? N311 C312 C313 121.1(3) . . ? N311 C312 C322 114.7(3) . . ? C313 C312 C322 124.2(3) . . ? C314 C313 C312 119.3(4) . . ? C313 C314 C315 119.8(4) . . ? C316 C315 C314 118.1(4) . . ? N311 C316 C315 123.1(3) . . ? C326 N321 C322 118.8(3) . . ? C326 N321 Ru1 125.3(2) . . ? C322 N321 Ru1 115.8(2) . . ? N321 C322 C323 120.7(3) . . ? N321 C322 C312 114.9(3) . . ? C323 C322 C312 124.4(3) . . ? C324 C323 C322 119.4(3) . . ? C325 C324 C323 120.0(4) . . ? C326 C325 C324 117.7(3) . . ? C326 C325 C410 120.4(3) . . ? C324 C325 C410 121.7(4) . . ? N321 C326 C325 123.3(3) . . ? N411 C410 C325 112.7(3) . . ? C428 N411 C412 110.9(4) . . ? C428 N411 C410 112.4(4) . . ? C412 N411 C410 110.6(4) . . ? C413 C412 N411 113.6(4) . . ? O414 C413 C412 110.0(5) . . ? C413 O414 C415 113.5(5) . . ? O414 C415 C416 108.4(5) . . ? O417 C416 C415 107.5(6) . . ? C416 O417 C418 112.7(6) . . ? O417 C418 C419 113.9(5) . . ? C418 C419 N420 114.2(4) . . ? C421 N420 C429 110.5(4) . . ? C421 N420 C419 109.9(4) . . ? C429 N420 C419 111.4(4) . . ? C422 C421 N420 113.5(4) . . ? O423 C422 C421 108.1(4) . . ? C424 O423 C422 112.4(4) . . ? O423 C424 C425 109.2(4) . . ? O426 C425 C424 109.8(4) . . ? C425 O426 C427 112.6(4) . . ? O426 C427 C428 111.2(4) . . ? N411 C428 C427 113.5(4) . . ? C513 C429 N420 114.6(4) . . ? C516 N511 C512 118.2(4) . . ? N511 C512 C513 122.5(4) . . ? C512 C513 C514 117.2(4) . . ? C512 C513 C429 120.8(4) . . ? C514 C513 C429 121.9(4) . . ? C515 C514 C513 120.6(4) . . ? C514 C515 C516 119.5(4) . . ? N511 C516 C515 121.9(4) . . ? N511 C516 C526 118.5(4) . . ? C515 C516 C526 119.6(4) . . ? C526 N521 C522 117.4(4) . . ? C523 C522 N521 122.9(5) . . ? C522 C523 C524 118.1(5) . . ? C523 C524 C525 121.6(5) . . ? C526 C525 C524 118.2(5) . . ? N521 C526 C525 121.6(4) . . ? N521 C526 C516 118.3(4) . . ? C525 C526 C516 120.1(4) . . ? F12 P1 F15 90.3(2) . . ? F12 P1 F13 179.2(2) . . ? F15 P1 F13 90.5(2) . . ? F12 P1 F14 90.4(2) . . ? F15 P1 F14 90.8(2) . . ? F13 P1 F14 89.8(2) . . ? F12 P1 F16 89.8(2) . . ? F15 P1 F16 90.3(2) . . ? F13 P1 F16 90.0(2) . . ? F14 P1 F16 179.0(2) . . ? F12 P1 F11 89.4(2) . . ? F15 P1 F11 179.6(2) . . ? F13 P1 F11 89.8(2) . . ? F14 P1 F11 89.4(2) . . ? F16 P1 F11 89.6(2) . . ? F24 P2 F25 89.9(4) . . ? F24 P2 F21 93.4(4) . . ? F25 P2 F21 176.1(3) . . ? F24 P2 F23 178.9(3) . . ? F25 P2 F23 90.2(3) . . ? F21 P2 F23 86.4(3) . . ? F24 P2 F22 93.2(3) . . ? F25 P2 F22 88.5(2) . . ? F21 P2 F22 93.3(2) . . ? F23 P2 F22 87.9(2) . . ? F24 P2 F26 87.8(3) . . ? F25 P2 F26 89.7(2) . . ? F21 P2 F26 88.4(2) . . ? F23 P2 F26 91.1(3) . . ? F22 P2 F26 177.9(2) . . ? F36 P3 F35 94.0(4) . . ? F36 P3 F34 87.7(4) . . ? F35 P3 F34 88.6(4) . . ? F36 P3 F31 92.8(3) . . ? F35 P3 F31 95.0(4) . . ? F34 P3 F31 176.3(3) . . ? F36 P3 F33 91.4(4) . . ? F35 P3 F33 173.7(4) . . ? F34 P3 F33 88.5(3) . . ? F31 P3 F33 87.9(3) . . ? F36 P3 F32 177.1(4) . . ? F35 P3 F32 83.5(3) . . ? F34 P3 F32 93.8(4) . . ? F31 P3 F32 85.9(3) . . ? F33 P3 F32 91.1(3) . . ? O2 C2 C1 124.5(8) . . ? O2 C2 C3 118.2(9) . . ? C1 C2 C3 117.1(9) . . ? C62 C61 C60 105.7(22) 2_565 . ? C62 C61 C62 86.6(25) 2_565 . ? C60 C61 C62 150.2(27) . . ? C61 C62 C61 93.4(25) 2_565 . ? C61 C62 C62 51.7(16) 2_565 2_565 ? C61 C62 C62 41.8(13) . 2_565 ? _refine_diff_density_max 1.135 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.085