# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _publ_contact_author_name 'Jay Siegel' _publ_contact_author_address ; Institute of Organic Chemistry University of Zurich Winterthurerstrasse 190 Zurich CH-8057 ; _publ_contact_author_email JSS@OCI.UNIZH.CH _publ_section_title ; Synthesis of Arhiral and Racemic Catenanes Based on Terpyridine and a Directionalized Terpyridine Mimic, Pyridyl-Phenanthroline ; loop_ _publ_author_name 'Jay Siegel' 'Peter Gantzel' 'Jon Loren' # End of CIF ============================================================ data_sad _database_code_depnum_ccdc_archive 'CCDC 270917' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C172.23 H106 Cl3.11 F12 N6 O15 P2 Ru' _chemical_formula_weight 3000.59 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' Cl Cl 0.1484 0.1585 '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 16.1362(14) _cell_length_b 17.4816(16) _cell_length_c 30.711(3) _cell_angle_alpha 77.635(2) _cell_angle_beta 75.632(2) _cell_angle_gamma 65.267(2) _cell_volume 7562.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description box _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 0.260 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9522 _exptl_absorpt_correction_T_max 0.9596 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41159 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 22.57 _reflns_number_total 19541 _reflns_number_gt 12817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19541 _refine_ls_number_parameters 1116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1317 _refine_ls_R_factor_gt 0.0980 _refine_ls_wR_factor_ref 0.3071 _refine_ls_wR_factor_gt 0.2824 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.833 _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 C1W C 0.4552(8) -0.3740(8) 0.0228(3) 0.149(3) Uiso 1 1 d G . . C2W C 0.4100(9) -0.4273(7) 0.0461(4) 0.149(3) Uiso 1 1 d G . . C3W C 0.3709(8) -0.4221(7) 0.0918(4) 0.149(3) Uiso 1 1 d G . . C4W C 0.3771(8) -0.3637(8) 0.1140(3) 0.149(3) Uiso 1 1 d G . . C5W C 0.4223(8) -0.3105(7) 0.0906(4) 0.149(3) Uiso 1 1 d G . . C6W C 0.4614(8) -0.3156(7) 0.0450(4) 0.149(3) Uiso 1 1 d G . . C1X C 0.6209(13) -0.0541(11) 0.3889(4) 0.150(4) Uiso 0.743(11) 1 d PG A 1 C2X C 0.6711(8) -0.1132(10) 0.4207(6) 0.150(4) Uiso 0.743(11) 1 d PG A 1 C3X C 0.6252(12) -0.1333(9) 0.4635(6) 0.150(4) Uiso 0.743(11) 1 d PG A 1 C4X C 0.5291(13) -0.0943(11) 0.4745(5) 0.150(4) Uiso 0.743(11) 1 d PG A 1 C5X C 0.4789(8) -0.0353(10) 0.4427(6) 0.150(4) Uiso 0.743(11) 1 d PG A 1 C6X C 0.5248(13) -0.0152(10) 0.3999(6) 0.150(4) Uiso 0.743(11) 1 d PG A 1 C1XA C 0.534(6) -0.0562(15) 0.4518(13) 0.188(9) Uiso 0.257(11) 1 d PG A 2 Cl1X Cl 0.5508(17) -0.1542(11) 0.4354(8) 0.188(9) Uiso 0.257(11) 1 d PG A 2 Cl2X Cl 0.4963(17) 0.0310(11) 0.4091(8) 0.188(9) Uiso 0.257(11) 1 d PG A 2 C1T C 0.0479(8) 0.6083(6) 0.0759(4) 0.090(2) Uiso 0.728(8) 1 d PG B 1 C2T C 0.1170(6) 0.6405(7) 0.0663(4) 0.090(2) Uiso 0.728(8) 1 d PG B 1 C3T C 0.1019(7) 0.7130(7) 0.0842(4) 0.090(2) Uiso 0.728(8) 1 d PG B 1 C4T C 0.0178(8) 0.7531(6) 0.1117(4) 0.090(2) Uiso 0.728(8) 1 d PG B 1 C5T C -0.0513(6) 0.7209(6) 0.1213(3) 0.090(2) Uiso 0.728(8) 1 d PG B 1 C6T C -0.0362(7) 0.6485(7) 0.1034(4) 0.090(2) Uiso 0.728(8) 1 d PG B 1 C1TA C 0.1321(17) 0.651(2) 0.0572(13) 0.097(4) Uiso 0.272(8) 1 d PG B 2 Cl1A Cl 0.1480(7) 0.7338(7) 0.0749(4) 0.097(4) Uiso 0.272(8) 1 d PG B 2 Cl2A Cl 0.0251(7) 0.6418(7) 0.0849(4) 0.097(4) Uiso 0.272(8) 1 d PG B 2 F1 F 0.0432(4) 0.1086(3) 0.61329(16) 0.0746(15) Uani 1 1 d . C . F4 F 0.0677(4) 0.0274(4) 0.71485(16) 0.0837(17) Uani 1 1 d . C . F2A F 0.0921(12) 0.1407(9) 0.6635(6) 0.068(4) Uiso 0.415(9) 1 d P C 1 F3A F 0.1673(9) 0.0312(14) 0.6530(4) 0.058(4) Uiso 0.415(9) 1 d P C 1 F5A F 0.0546(17) -0.0161(9) 0.6537(5) 0.060(4) Uiso 0.415(9) 1 d P C 1 F6A F -0.0470(9) 0.1392(9) 0.6767(4) 0.053(3) Uiso 0.415(9) 1 d P C 1 F2B F 0.0562(18) 0.1537(9) 0.6792(6) 0.072(5) Uiso 0.415(9) 1 d P C 3 F3B F 0.1547(10) 0.0039(9) 0.6450(5) 0.067(4) Uiso 0.415(9) 1 d P C 3 F5B F 0.0102(12) 0.0026(10) 0.6620(5) 0.062(4) Uiso 0.415(9) 1 d P C 3 F6B F -0.0538(9) 0.1034(16) 0.6816(5) 0.063(4) Uiso 0.415(9) 1 d P C 3 P1 P 0.05542(16) 0.06859(15) 0.66407(7) 0.0561(6) Uani 1 1 d G . . F23 F 0.1504(16) 0.077(3) 0.6495(9) 0.083(9) Uiso 0.170(18) 1 d PG C 2 F35 F 0.099(3) -0.0187(8) 0.6463(9) 0.083(9) Uiso 0.170(18) 1 d PG C 2 F56 F -0.0396(16) 0.060(3) 0.6786(9) 0.083(9) Uiso 0.170(18) 1 d PG C 2 F62 F 0.012(3) 0.1558(8) 0.6818(9) 0.083(9) Uiso 0.170(18) 1 d PG C 2 F7 F 0.7586(4) 0.5885(3) 0.11609(17) 0.0814(16) Uani 1 1 d . D . F10 F 0.6117(4) 0.6260(4) 0.20847(17) 0.0847(17) Uani 1 1 d . D . F8 F 0.7232(8) 0.6738(6) 0.1661(2) 0.079(4) Uani 0.75(2) 1 d P D 1 F9 F 0.7634(7) 0.5391(8) 0.1911(3) 0.104(4) Uani 0.75(2) 1 d P D 1 F11 F 0.6550(12) 0.5340(8) 0.1589(3) 0.118(5) Uani 0.75(2) 1 d P D 1 F12 F 0.6140(6) 0.6745(9) 0.1332(3) 0.103(4) Uani 0.75(2) 1 d P D 1 P2 P 0.68551(19) 0.60520(15) 0.16248(8) 0.0608(7) Uani 1 1 d G . . F23A F 0.7636(10) 0.5861(15) 0.1887(7) 0.083(6) Uiso 0.25(2) 1 d PG D 2 F35A F 0.7084(17) 0.5091(4) 0.1664(7) 0.083(6) Uiso 0.25(2) 1 d PG D 2 F56A F 0.6075(10) 0.6242(15) 0.1362(7) 0.083(6) Uiso 0.25(2) 1 d PG D 2 F62A F 0.6626(17) 0.7013(4) 0.1585(7) 0.083(6) Uiso 0.25(2) 1 d PG D 2 C1Y C 0.3017(10) -0.6523(8) 0.5780(5) 0.110(4) Uiso 1 1 d . . . Cl1 Cl 0.3512(6) -0.5919(5) 0.5397(2) 0.255(4) Uani 1 1 d . . . Cl2 Cl 0.1817(5) -0.6131(5) 0.5735(2) 0.223(3) Uani 1 1 d . . . O1Z O 0.3982(6) -0.0522(5) 0.2115(3) 0.101(2) Uani 1 1 d . . . C2Z C 0.3388(6) -0.1647(5) 0.2519(3) 0.056(2) Uani 1 1 d . . . C3Z C 0.3969(9) -0.1214(8) 0.2094(4) 0.094(4) Uiso 1 1 d . . . C4Z C 0.4510(7) -0.1444(13) 0.1718(4) 0.163(8) Uani 1 1 d . . . O1ZA O -0.0093(7) 0.0231(9) 0.4552(4) 0.151(4) Uani 1 1 d . . . C2ZA C -0.0033(8) 0.0808(9) 0.4733(5) 0.090(4) Uani 1 1 d . . . C3ZA C 0.0059(8) 0.0656(9) 0.5176(4) 0.095(4) Uani 1 1 d . . . O1ZB O 0.0452(5) 0.4804(4) 0.2637(2) 0.0774(19) Uani 1 1 d . . . C2ZB C -0.0199(7) 0.5468(6) 0.2626(4) 0.067(3) Uani 1 1 d . . . C3ZB C -0.0709(8) 0.5917(8) 0.3036(5) 0.104(4) Uani 1 1 d . . . C4ZB C -0.0593(9) 0.5914(10) 0.2205(5) 0.123(5) Uani 1 1 d . . . O7 O 0.7157(4) 0.4322(4) 0.03312(17) 0.0606(16) Uani 1 1 d . . . O8 O 0.7749(4) 0.5539(3) -0.03003(18) 0.0563(15) Uani 1 1 d . . . O9 O -0.2922(3) 0.5493(3) 0.34033(16) 0.0442(13) Uani 1 1 d . . . O10 O -0.3775(4) 0.7313(3) 0.32750(17) 0.0492(14) Uani 1 1 d . . . C1H C 0.7828(5) -0.1039(3) 0.51984(18) 0.063(3) Uani 1 1 d G . . C2H C 0.7657(5) -0.1250(3) 0.56673(17) 0.066(3) Uani 1 1 d G . . H2H H 0.7366 -0.0810 0.5861 0.079 Uiso 1 1 d G . . C3H C 0.7909(5) -0.2099(3) 0.58541(13) 0.069(3) Uani 1 1 d G . . H3H H 0.7792 -0.2244 0.6177 0.083 Uiso 1 1 d G . . C4H C 0.8333(5) -0.2738(2) 0.55721(17) 0.049(2) Uani 1 1 d G . . C5H C 0.8503(7) -0.2527(3) 0.51033(16) 0.166(9) Uani 1 1 d G . . H5H H 0.8795 -0.2967 0.4909 0.200 Uiso 1 1 d G . . C6H C 0.8251(7) -0.1678(4) 0.49163(13) 0.164(9) Uani 1 1 d G . . H6H H 0.8369 -0.1533 0.4594 0.197 Uiso 1 1 d G . . C1I C 0.9048(4) -0.5377(2) 0.60883(18) 0.057(2) Uani 1 1 d G . . C2I C 0.8732(4) -0.4776(3) 0.63885(13) 0.054(2) Uani 1 1 d G . . H2I H 0.8668 -0.4953 0.6709 0.065 Uiso 1 1 d G . . C3I C 0.8512(4) -0.3920(3) 0.62228(15) 0.054(2) Uani 1 1 d G . . H3I H 0.8295 -0.3506 0.6429 0.064 Uiso 1 1 d G . . C4I C 0.8606(4) -0.3664(2) 0.57567(16) 0.047(2) Uani 1 1 d G . . C5I C 0.8921(5) -0.4264(3) 0.54567(12) 0.069(3) Uani 1 1 d G . . H5I H 0.8986 -0.4088 0.5136 0.083 Uiso 1 1 d G . . C6I C 0.9142(5) -0.5121(3) 0.56224(16) 0.082(3) Uani 1 1 d G . . H6I H 0.9359 -0.5534 0.5416 0.099 Uiso 1 1 d G . . C1Q C -0.0945(5) 0.9941(4) 0.12336(16) 0.069(3) Uani 1 1 d G . . C2Q C -0.0934(4) 0.9913(4) 0.16896(19) 0.053(2) Uani 1 1 d G . . H2Q H -0.0608 1.0193 0.1774 0.063 Uiso 1 1 d G . . C3Q C -0.1398(4) 0.9478(4) 0.20230(14) 0.053(2) Uani 1 1 d G . . H3Q H -0.1390 0.9459 0.2337 0.063 Uiso 1 1 d G . . C4Q C -0.1872(4) 0.9071(4) 0.19002(17) 0.051(2) Uani 1 1 d G . . C5Q C -0.1882(6) 0.9099(5) 0.1444(2) 0.158(8) Uani 1 1 d G . . H5Q H -0.2208 0.8819 0.1360 0.189 Uiso 1 1 d G . . C6Q C -0.1419(6) 0.9534(6) 0.11108(14) 0.163(8) Uani 1 1 d G . . H6Q H -0.1427 0.9553 0.0797 0.196 Uiso 1 1 d G . . C1R C -0.3316(3) 0.7717(3) 0.29254(14) 0.0424(19) Uani 1 1 d G . . C2R C -0.3325(3) 0.7760(3) 0.24676(16) 0.0418(18) Uani 1 1 d G . . H2R H -0.3656 0.7491 0.2378 0.050 Uiso 1 1 d G . . C3R C -0.2852(3) 0.8194(3) 0.21402(11) 0.0435(19) Uani 1 1 d G . . H3R H -0.2858 0.8224 0.1825 0.052 Uiso 1 1 d G . . C4R C -0.2371(3) 0.8585(3) 0.22706(14) 0.0431(19) Uani 1 1 d G . . C5R C -0.2362(4) 0.8542(3) 0.27283(16) 0.056(2) Uani 1 1 d G . . H5R H -0.2031 0.8811 0.2818 0.067 Uiso 1 1 d G . . C6R C -0.2835(4) 0.8108(3) 0.30558(12) 0.057(2) Uani 1 1 d G . . H6R H -0.2829 0.8078 0.3371 0.068 Uiso 1 1 d G . . O11 O -0.0469(5) 1.0328(5) 0.0894(2) 0.080(2) Uani 1 1 d . . . O12 O 0.3369(4) 1.1341(3) -0.10629(17) 0.0553(15) Uani 1 1 d . . . C11 C 0.7181(6) 0.5037(5) 0.0473(3) 0.055(2) Uiso 1 1 d . . . H11A H 0.7297 0.4900 0.0788 0.066 Uiso 1 1 calc R . . H11B H 0.6582 0.5527 0.0461 0.066 Uiso 1 1 calc R . . C12 C 0.7951(6) 0.5239(5) 0.0155(3) 0.055(2) Uiso 1 1 d . . . H12A H 0.8049 0.5680 0.0267 0.066 Uiso 1 1 calc R . . H12B H 0.8531 0.4725 0.0148 0.066 Uiso 1 1 calc R . . C13 C -0.3349(5) 0.5960(5) 0.3028(3) 0.0430(19) Uiso 1 1 d . . . H13A H -0.3600 0.5622 0.2919 0.052 Uiso 1 1 calc R . . H13B H -0.2889 0.6094 0.2779 0.052 Uiso 1 1 calc R . . C14 C -0.4109(6) 0.6755(5) 0.3172(3) 0.049(2) Uiso 1 1 d . . . H14A H -0.4474 0.7045 0.2926 0.059 Uiso 1 1 calc R . . H14B H -0.4527 0.6613 0.3442 0.059 Uiso 1 1 calc R . . C15 C 0.0055(10) 1.0631(9) 0.0989(5) 0.115(5) Uani 1 1 d . . . H15A H 0.0477 1.0193 0.1184 0.138 Uiso 1 1 calc R . . H15B H -0.0333 1.1120 0.1160 0.138 Uiso 1 1 calc R . . C16 C 0.0636(9) 1.0921(9) 0.0555(5) 0.109(4) Uani 1 1 d . . . C17 C 0.1099(8) 1.1096(8) 0.0215(5) 0.126(6) Uani 1 1 d . . . C18 C 0.1661(7) 1.1412(6) -0.0131(4) 0.080(3) Uani 1 1 d . . . C19 C 0.2185(6) 1.1653(6) -0.0400(3) 0.059(2) Uani 1 1 d . . . C20 C 0.2838(6) 1.1931(5) -0.0733(3) 0.054(2) Uani 1 1 d . . . H20A H 0.3269 1.1999 -0.0579 0.065 Uiso 1 1 calc R . . H20B H 0.2499 1.2493 -0.0893 0.065 Uiso 1 1 calc R . . N1J N 0.3639(4) 0.1026(3) 0.27153(19) 0.0338(14) Uiso 1 1 d . . . C2J C 0.4572(5) 0.0586(4) 0.2601(2) 0.0354(17) Uiso 1 1 d . . . C3J C 0.4975(6) -0.0233(5) 0.2809(3) 0.0451(19) Uiso 1 1 d . . . H3JA H 0.5624 -0.0544 0.2736 0.054 Uiso 1 1 calc R . . C4J C 0.4421(5) -0.0597(5) 0.3126(3) 0.049(2) Uiso 1 1 d . . . H4JA H 0.4692 -0.1163 0.3265 0.059 Uiso 1 1 calc R . . C5J C 0.3467(5) -0.0136(5) 0.3243(3) 0.0444(19) Uiso 1 1 d . . . H5JA H 0.3089 -0.0381 0.3463 0.053 Uiso 1 1 calc R . . C6J C 0.3083(5) 0.0684(4) 0.3032(2) 0.0357(17) Uiso 1 1 d . . . C1K C 0.5023(5) 0.1076(4) 0.2256(2) 0.0371(17) Uiso 1 1 d . . . C2K C 0.5966(5) 0.0803(5) 0.2096(2) 0.0404(18) Uiso 1 1 d . . . H2KA H 0.6364 0.0252 0.2203 0.048 Uiso 1 1 calc R . . C3K C 0.6337(5) 0.1324(4) 0.1780(2) 0.0420(18) Uiso 1 1 d . . . H3KA H 0.6987 0.1131 0.1674 0.050 Uiso 1 1 calc R . . C4K C 0.5753(5) 0.2135(5) 0.1618(3) 0.0446(19) Uiso 1 1 d . . . C5K C 0.4806(5) 0.2368(4) 0.1791(2) 0.0368(17) Uiso 1 1 d . . . H5KA H 0.4393 0.2913 0.1683 0.044 Uiso 1 1 calc R . . N6K N 0.4447(4) 0.1869(3) 0.20993(19) 0.0346(14) Uiso 1 1 d . . . C1L C 0.2117(5) 0.1289(4) 0.3111(2) 0.0361(17) Uiso 1 1 d . . . C2L C 0.1396(5) 0.1097(5) 0.3388(3) 0.0437(19) Uiso 1 1 d . . . H2LA H 0.1510 0.0541 0.3544 0.052 Uiso 1 1 calc R . . C3L C 0.0500(5) 0.1720(5) 0.3438(3) 0.0462(19) Uiso 1 1 d . . . H3LA H -0.0006 0.1587 0.3616 0.055 Uiso 1 1 calc R . . C4L C 0.0356(5) 0.2539(4) 0.3222(2) 0.0361(17) Uiso 1 1 d . . . C5L C 0.1104(5) 0.2693(4) 0.2942(2) 0.0376(17) Uiso 1 1 d . . . H5LA H 0.1006 0.3251 0.2792 0.045 Uiso 1 1 calc R . . N6L N 0.1961(4) 0.2089(3) 0.28737(19) 0.0338(14) Uiso 1 1 d . . . C1M C -0.0566(3) 0.3285(2) 0.32703(14) 0.0376(17) Uiso 1 1 d G . . C2M C -0.0960(3) 0.3715(3) 0.28885(11) 0.0387(17) Uiso 1 1 d G . . C3M C -0.1763(3) 0.4449(3) 0.29233(12) 0.0409(18) Uiso 1 1 d G . . H3MA H -0.2033 0.4742 0.2663 0.049 Uiso 1 1 calc R . . C4M C -0.2171(3) 0.4755(2) 0.33403(14) 0.0415(18) Uiso 1 1 d G . . C5M C -0.1777(3) 0.4325(3) 0.37220(11) 0.0413(18) Uiso 1 1 d G . . H5MA H -0.2055 0.4534 0.4007 0.050 Uiso 1 1 calc R . . C6M C -0.0974(3) 0.3591(3) 0.36869(12) 0.0409(18) Uiso 1 1 d G . . C7M C -0.0555(6) 0.3168(5) 0.4114(3) 0.050(2) Uiso 1 1 d . . . H7MA H -0.0764 0.2707 0.4260 0.075 Uiso 1 1 calc R . . H7MB H -0.0756 0.3589 0.4324 0.075 Uiso 1 1 calc R . . H7MC H 0.0123 0.2938 0.4033 0.075 Uiso 1 1 calc R . . C8M C -0.0550(6) 0.3415(5) 0.2422(3) 0.051(2) Uiso 1 1 d . . . H8MA H -0.1037 0.3638 0.2238 0.077 Uiso 1 1 calc R . . H8MB H -0.0292 0.2794 0.2455 0.077 Uiso 1 1 calc R . . H8MC H -0.0058 0.3623 0.2274 0.077 Uiso 1 1 calc R . . C1N C 0.6081(4) 0.2738(3) 0.12740(15) 0.0440(19) Uiso 1 1 d G . . C2N C 0.6638(4) 0.2477(2) 0.08649(17) 0.051(2) Uiso 1 1 d G . . C3N C 0.6973(4) 0.3030(3) 0.05508(14) 0.054(2) Uiso 1 1 d G . . H3NA H 0.7353 0.2852 0.0271 0.064 Uiso 1 1 calc R . . C4N C 0.6751(4) 0.3844(3) 0.06457(15) 0.053(2) Uiso 1 1 d G . . C5N C 0.6194(4) 0.4105(2) 0.10548(17) 0.052(2) Uiso 1 1 d G . . H5NB H 0.6043 0.4660 0.1120 0.062 Uiso 1 1 calc R . . C6N C 0.5859(3) 0.3552(3) 0.13690(13) 0.049(2) Uiso 1 1 d G . . C7N C 0.5250(6) 0.3900(5) 0.1806(3) 0.054(2) Uiso 1 1 d . . . H7NA H 0.4596 0.4085 0.1786 0.080 Uiso 1 1 calc R . . H7NB H 0.5366 0.4383 0.1849 0.080 Uiso 1 1 calc R . . H7NC H 0.5396 0.3455 0.2063 0.080 Uiso 1 1 calc R . . C8N C 0.6868(6) 0.1621(5) 0.0715(3) 0.064(2) Uiso 1 1 d . . . H8NA H 0.7031 0.1663 0.0384 0.096 Uiso 1 1 calc R . . H8NB H 0.6327 0.1465 0.0817 0.096 Uiso 1 1 calc R . . H8NC H 0.7393 0.1187 0.0848 0.096 Uiso 1 1 calc R . . C1O C 0.7120(3) 0.6363(2) -0.03673(18) 0.048(2) Uiso 1 1 d G . . C2O C 0.6481(4) 0.6514(3) -0.06396(18) 0.055(2) Uiso 1 1 d G . . H2OA H 0.6468 0.6055 -0.0752 0.066 Uiso 1 1 calc R . . C3O C 0.5863(3) 0.7338(3) -0.07470(18) 0.053(2) Uiso 1 1 d G . . H3OA H 0.5427 0.7441 -0.0933 0.063 Uiso 1 1 calc R . . C4O C 0.5883(3) 0.8011(2) -0.05821(18) 0.047(2) Uiso 1 1 d G . . C5O C 0.6522(4) 0.7860(3) -0.03100(19) 0.059(2) Uiso 1 1 d G . . H5OA H 0.6535 0.8319 -0.0197 0.071 Uiso 1 1 calc R . . C6O C 0.7140(3) 0.7036(3) -0.02024(18) 0.058(2) Uiso 1 1 d G . . H6OA H 0.7576 0.6933 -0.0017 0.070 Uiso 1 1 calc R . . C1P C 0.5213(3) 0.8911(2) -0.06971(16) 0.0448(19) Uiso 1 1 d G . . C2P C 0.4716(4) 0.9434(3) -0.03591(12) 0.050(2) Uiso 1 1 d G . . H2PA H 0.4801 0.9230 -0.0054 0.060 Uiso 1 1 calc R . . C3P C 0.4095(3) 1.0256(3) -0.04681(14) 0.049(2) Uiso 1 1 d G . . H3PA H 0.3756 1.0613 -0.0237 0.059 Uiso 1 1 calc R . . C4P C 0.3971(3) 1.0555(2) -0.09147(16) 0.048(2) Uiso 1 1 d G . . C5P C 0.4468(4) 1.0031(3) -0.12525(12) 0.053(2) Uiso 1 1 d G . . H5PA H 0.4384 1.0235 -0.1557 0.063 Uiso 1 1 calc R . . C6P C 0.5089(3) 0.9209(3) -0.11439(14) 0.050(2) Uiso 1 1 d G . . H6PA H 0.5428 0.8852 -0.1375 0.060 Uiso 1 1 calc R . . O1 O 0.6624(4) 0.1507(4) 0.46093(18) 0.0587(15) Uani 1 1 d . . . O2 O 0.7540(4) -0.0184(3) 0.50525(19) 0.0683(18) Uani 1 1 d . . . O3 O 0.1646(5) -0.1829(4) 0.1618(3) 0.086(2) Uani 1 1 d . . . O4 O 0.2476(5) -0.3227(4) 0.2222(3) 0.088(2) Uani 1 1 d . . . O5 O 0.6119(5) -0.5913(4) 0.4643(2) 0.083(2) Uani 1 1 d . . . O6 O 0.9239(5) -0.6206(4) 0.6289(2) 0.0721(19) Uani 1 1 d . . . C1 C 0.7550(6) 0.0959(6) 0.4496(3) 0.065(3) Uani 1 1 d . . . H1A H 0.7925 0.1044 0.4678 0.078 Uiso 1 1 calc R . . H1B H 0.7780 0.1113 0.4173 0.078 Uiso 1 1 calc R . . C2 C 0.7696(8) 0.0060(6) 0.4568(3) 0.080(3) Uani 1 1 d . . . H2A H 0.7256 -0.0028 0.4428 0.097 Uiso 1 1 calc R . . H2B H 0.8336 -0.0285 0.4431 0.097 Uiso 1 1 calc R . . C3 C 0.1131(8) -0.2160(7) 0.1975(5) 0.106(5) Uani 1 1 d . . . H3A H 0.0535 -0.1692 0.2067 0.128 Uiso 1 1 calc R . . H3B H 0.0986 -0.2573 0.1864 0.128 Uiso 1 1 calc R . . C4 C 0.1519(8) -0.2554(10) 0.2353(4) 0.110(4) Uani 1 1 d . . . H4A H 0.1119 -0.2820 0.2569 0.132 Uiso 1 1 calc R . . H4B H 0.1567 -0.2130 0.2503 0.132 Uiso 1 1 calc R . . C5 C 0.9637(8) -0.6862(6) 0.5996(4) 0.082(3) Uani 1 1 d . . . H5A H 0.9848 -0.7422 0.6183 0.098 Uiso 1 1 calc R . . H5B H 1.0189 -0.6801 0.5788 0.098 Uiso 1 1 calc R . . C6 C 0.9004(8) -0.6844(6) 0.5732(4) 0.068(3) Uani 1 1 d . . . C7 C 0.8512(9) -0.6844(6) 0.5511(4) 0.069(3) Uani 1 1 d . . . C8 C 0.7945(10) -0.6809(6) 0.5228(4) 0.078(4) Uani 1 1 d . . . C9 C 0.7452(9) -0.6756(6) 0.4969(4) 0.072(3) Uani 1 1 d . . . C10 C 0.6930(8) -0.6663(6) 0.4614(4) 0.079(3) Uani 1 1 d . . . H10A H 0.7322 -0.6637 0.4311 0.095 Uiso 1 1 calc R . . H10B H 0.6761 -0.7160 0.4655 0.095 Uiso 1 1 calc R . . N1A N 0.2566(4) 0.3378(4) 0.2127(2) 0.0378(14) Uiso 1 1 d . . . C2A C 0.2687(5) 0.3988(4) 0.2274(2) 0.0403(18) Uiso 1 1 d . . . C3A C 0.2373(5) 0.4822(5) 0.2054(3) 0.049(2) Uiso 1 1 d . . . H3AE H 0.2448 0.5261 0.2156 0.059 Uiso 1 1 calc R . . C4A C 0.1951(6) 0.4985(5) 0.1686(3) 0.052(2) Uiso 1 1 d . . . H4AA H 0.1736 0.5545 0.1532 0.062 Uiso 1 1 calc R . . C5A C 0.1835(6) 0.4348(5) 0.1537(3) 0.052(2) Uiso 1 1 d . . . H5AE H 0.1537 0.4474 0.1285 0.062 Uiso 1 1 calc R . . C6A C 0.2160(5) 0.3518(5) 0.1758(3) 0.0415(18) Uiso 1 1 d . . . C1B C 0.2127(5) 0.2768(5) 0.1659(2) 0.0407(18) Uiso 1 1 d . . . N2B N 0.2557(4) 0.2030(4) 0.1924(2) 0.0383(14) Uiso 1 1 d . . . C3B C 0.2507(5) 0.1310(5) 0.1865(2) 0.0408(18) Uiso 1 1 d . . . H3BE H 0.2828 0.0801 0.2042 0.049 Uiso 1 1 calc R . . C4B C 0.2024(5) 0.1258(5) 0.1567(3) 0.0439(19) Uiso 1 1 d . . . C5B C 0.1618(6) 0.2006(5) 0.1289(3) 0.054(2) Uiso 1 1 d . . . H5BC H 0.1304 0.2002 0.1066 0.065 Uiso 1 1 calc R . . C6B C 0.1672(6) 0.2756(5) 0.1337(3) 0.051(2) Uiso 1 1 d . . . H6BE H 0.1393 0.3262 0.1147 0.062 Uiso 1 1 calc R . . C1C C 0.3178(5) 0.3679(5) 0.2660(2) 0.0404(18) Uiso 1 1 d . . . N2C N 0.3410(4) 0.2830(3) 0.28126(19) 0.0353(14) Uiso 1 1 d . . . C3C C 0.3900(5) 0.2488(5) 0.3144(2) 0.0395(18) Uiso 1 1 d . . . H3CA H 0.4043 0.1904 0.3252 0.047 Uiso 1 1 calc R . . C4C C 0.4216(5) 0.2933(5) 0.3343(3) 0.0434(19) Uiso 1 1 d . . . C5C C 0.3939(6) 0.3803(5) 0.3199(3) 0.053(2) Uiso 1 1 d . . . H5CA H 0.4112 0.4142 0.3334 0.063 Uiso 1 1 calc R . . C6C C 0.3419(5) 0.4166(5) 0.2864(3) 0.048(2) Uiso 1 1 d . . . H6CA H 0.3223 0.4760 0.2772 0.058 Uiso 1 1 calc R . . C1D C 0.4835(3) 0.2507(3) 0.36816(15) 0.0449(19) Uiso 1 1 d G . . C2D C 0.4588(3) 0.2786(3) 0.41047(16) 0.047(2) Uiso 1 1 d G . . C3D C 0.5203(3) 0.2427(3) 0.44082(13) 0.052(2) Uiso 1 1 d G . . H3DA H 0.5035 0.2618 0.4697 0.063 Uiso 1 1 calc R . . C4D C 0.6065(3) 0.1789(3) 0.42889(15) 0.050(2) Uiso 1 1 d G . . C5D C 0.6312(3) 0.1510(3) 0.38660(16) 0.049(2) Uiso 1 1 d G . . H5DA H 0.6900 0.1074 0.3785 0.058 Uiso 1 1 calc R . . C6D C 0.5697(3) 0.1869(3) 0.35622(13) 0.050(2) Uiso 1 1 d G . . C7D C 0.6016(6) 0.1537(5) 0.3108(3) 0.056(2) Uiso 1 1 d . . . H7DA H 0.6688 0.1215 0.3061 0.084 Uiso 1 1 calc R . . H7DB H 0.5863 0.2015 0.2867 0.084 Uiso 1 1 calc R . . H7DC H 0.5703 0.1166 0.3101 0.084 Uiso 1 1 calc R . . C8D C 0.3682(6) 0.3488(5) 0.4256(3) 0.061(2) Uiso 1 1 d . . . H8DA H 0.3428 0.3327 0.4570 0.091 Uiso 1 1 calc R . . H8DB H 0.3243 0.3583 0.4060 0.091 Uiso 1 1 calc R . . H8DC H 0.3783 0.4010 0.4236 0.091 Uiso 1 1 calc R . . C1E C 0.1907(4) 0.0450(3) 0.15746(18) 0.051(2) Uiso 1 1 d G . . C2E C 0.1324(4) 0.0211(3) 0.19423(16) 0.051(2) Uiso 1 1 d G . . C3E C 0.1220(4) -0.0550(3) 0.19706(17) 0.064(2) Uiso 1 1 d G . . H3EA H 0.0821 -0.0713 0.2222 0.077 Uiso 1 1 calc R . . C4E C 0.1699(4) -0.1073(3) 0.1631(2) 0.068(3) Uiso 1 1 d G . . C5E C 0.2282(4) -0.0833(3) 0.12628(17) 0.068(3) Uiso 1 1 d G . . H5EA H 0.2609 -0.1189 0.1031 0.082 Uiso 1 1 calc R . . C6E C 0.2386(4) -0.0072(3) 0.12347(16) 0.056(2) Uiso 1 1 d G . . C7E C 0.3073(7) 0.0130(6) 0.0844(3) 0.077(3) Uiso 1 1 d . . . H7EA H 0.3598 0.0111 0.0958 0.116 Uiso 1 1 calc R . . H7EB H 0.2770 0.0698 0.0688 0.116 Uiso 1 1 calc R . . H7EC H 0.3297 -0.0289 0.0631 0.116 Uiso 1 1 calc R . . C8E C 0.0799(7) 0.0765(6) 0.2317(3) 0.074(3) Uiso 1 1 d . . . H8EA H 0.1232 0.0737 0.2500 0.111 Uiso 1 1 calc R . . H8EB H 0.0329 0.0564 0.2510 0.111 Uiso 1 1 calc R . . H8EC H 0.0496 0.1353 0.2185 0.111 Uiso 1 1 calc R . . C1F C 0.2967(4) -0.3549(4) 0.25684(17) 0.070(3) Uiso 1 1 d G . . C2F C 0.3925(4) -0.3931(4) 0.24404(14) 0.066(2) Uiso 1 1 d G . . H2FA H 0.4199 -0.3932 0.2129 0.079 Uiso 1 1 calc R . . C3F C 0.4483(3) -0.4313(3) 0.27696(18) 0.059(2) Uiso 1 1 d G . . H3FA H 0.5137 -0.4573 0.2682 0.071 Uiso 1 1 calc R . . C4F C 0.4083(4) -0.4313(4) 0.32266(16) 0.058(2) Uiso 1 1 d G . . C5F C 0.3125(4) -0.3931(4) 0.33542(14) 0.064(2) Uiso 1 1 d G . . H5FA H 0.2852 -0.3930 0.3666 0.077 Uiso 1 1 calc R . . C6F C 0.2567(3) -0.3549(4) 0.30252(19) 0.064(2) Uiso 1 1 d G . . H6FA H 0.1913 -0.3288 0.3113 0.077 Uiso 1 1 calc R . . C1G C 0.4657(4) -0.4746(4) 0.35877(17) 0.061(2) Uiso 1 1 d G . . C2G C 0.5448(4) -0.5483(4) 0.35231(15) 0.063(2) Uiso 1 1 d G . . H2GA H 0.5643 -0.5704 0.3242 0.075 Uiso 1 1 calc R . . C3G C 0.5953(3) -0.5897(3) 0.38712(19) 0.063(2) Uiso 1 1 d G . . H3GA H 0.6493 -0.6400 0.3827 0.076 Uiso 1 1 calc R . . C4G C 0.5667(4) -0.5573(4) 0.42835(17) 0.065(2) Uiso 1 1 d G . . C5G C 0.4876(4) -0.4836(4) 0.43481(16) 0.075(3) Uiso 1 1 d G . . H5GA H 0.4681 -0.4614 0.4630 0.090 Uiso 1 1 calc R . . C6G C 0.4371(4) -0.4422(3) 0.4000(2) 0.073(3) Uiso 1 1 d G . . H6GA H 0.3832 -0.3919 0.4044 0.087 Uiso 1 1 calc R . . Ru1 Ru 0.30883(4) 0.22007(3) 0.242489(19) 0.0340(2) Uani 1 1 d . . . C1S C 0.3404(3) -0.2213(3) 0.36868(18) 0.063(2) Uiso 1 1 d G . . C2S C 0.3763(3) -0.2042(3) 0.4006(2) 0.059(2) Uiso 1 1 d G . . C3S C 0.3183(4) -0.1458(4) 0.43043(17) 0.060(2) Uiso 1 1 d G . . C4S C 0.2243(3) -0.1045(3) 0.42845(18) 0.061(2) Uiso 1 1 d G . . C5S C 0.1883(3) -0.1216(3) 0.39661(19) 0.058(2) Uiso 1 1 d G . . C6S C 0.2464(4) -0.1800(4) 0.36672(17) 0.059(2) Uiso 1 1 d G . . C1U C 0.0215(6) 1.3526(8) 0.0314(2) 0.151(8) Uani 1 1 d G . . C2U C -0.0317(8) 1.3039(6) 0.0485(4) 0.149(7) Uani 1 1 d G . . C3U C -0.0916(7) 1.3166(5) 0.0900(4) 0.113(4) Uani 1 1 d G . . C4U C -0.0981(5) 1.3781(6) 0.1143(2) 0.085(3) Uani 1 1 d G . . C5U C -0.0449(6) 1.4268(5) 0.0972(3) 0.095(4) Uani 1 1 d G . . C6U C 0.0149(5) 1.4141(7) 0.0557(3) 0.119(6) Uani 1 1 d G . . C1V C -0.2061(5) 0.2209(5) 0.20408(19) 0.070(3) Uani 1 1 d G . . C2V C -0.1740(5) 0.1649(3) 0.2415(3) 0.094(4) Uani 1 1 d G . . C3V C -0.1944(5) 0.1945(4) 0.2831(2) 0.078(3) Uani 1 1 d G . . C4V C -0.2468(5) 0.2800(4) 0.28720(18) 0.070(3) Uani 1 1 d G . . C5V C -0.2789(4) 0.3360(3) 0.2498(2) 0.077(3) Uani 1 1 d G . . C6V C -0.2586(5) 0.3064(5) 0.2082(2) 0.079(3) Uani 1 1 d G . . 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 F1 0.093(4) 0.068(3) 0.044(3) 0.003(2) -0.014(3) -0.017(3) F4 0.101(4) 0.128(5) 0.042(3) 0.009(3) -0.022(3) -0.067(4) P1 0.0540(14) 0.0697(15) 0.0404(13) -0.0025(11) -0.0093(11) -0.0214(12) F7 0.111(5) 0.084(4) 0.053(3) -0.015(3) 0.000(3) -0.047(3) F10 0.104(4) 0.118(5) 0.049(3) -0.006(3) -0.004(3) -0.066(4) F8 0.114(9) 0.090(6) 0.055(5) -0.022(4) 0.007(4) -0.068(6) F9 0.123(7) 0.096(8) 0.062(5) 0.021(5) -0.031(5) -0.018(5) F11 0.194(12) 0.141(9) 0.086(6) -0.015(6) 0.003(7) -0.144(9) F12 0.098(6) 0.125(9) 0.061(5) 0.015(5) -0.032(5) -0.023(6) P2 0.0864(18) 0.0605(15) 0.0451(14) 0.0015(11) -0.0153(13) -0.0396(14) Cl1 0.394(10) 0.308(8) 0.147(4) -0.121(5) 0.103(6) -0.258(8) Cl2 0.235(6) 0.341(9) 0.183(5) -0.111(6) 0.005(5) -0.184(6) O1Z 0.113(6) 0.081(5) 0.113(6) 0.000(5) -0.023(5) -0.046(5) C2Z 0.070(6) 0.065(6) 0.052(5) -0.015(4) -0.001(4) -0.046(5) C4Z 0.034(6) 0.34(2) 0.063(8) 0.000(11) 0.012(5) -0.041(9) O1ZA 0.118(8) 0.185(12) 0.104(8) 0.014(8) -0.027(6) -0.027(8) C2ZA 0.071(7) 0.103(10) 0.095(10) -0.014(8) -0.012(7) -0.034(7) C3ZA 0.091(8) 0.121(10) 0.067(8) -0.001(7) -0.018(6) -0.037(7) O1ZB 0.059(4) 0.069(4) 0.091(5) -0.004(4) -0.004(4) -0.019(4) C2ZB 0.048(6) 0.052(6) 0.091(8) 0.009(5) -0.019(5) -0.016(5) C3ZB 0.066(7) 0.097(9) 0.147(12) -0.055(8) -0.008(7) -0.016(6) C4ZB 0.075(8) 0.159(13) 0.099(10) 0.032(9) -0.024(7) -0.028(8) O7 0.082(4) 0.084(4) 0.034(3) 0.002(3) 0.002(3) -0.060(4) O8 0.060(4) 0.058(3) 0.043(3) 0.008(3) -0.010(3) -0.023(3) O9 0.041(3) 0.038(3) 0.041(3) -0.004(2) -0.006(2) -0.004(2) O10 0.054(3) 0.040(3) 0.040(3) 0.000(2) -0.004(3) -0.010(3) C1H 0.078(6) 0.042(5) 0.051(6) -0.001(4) -0.007(5) -0.010(5) C2H 0.096(7) 0.052(5) 0.042(5) -0.012(4) -0.005(5) -0.024(5) C3H 0.100(8) 0.050(5) 0.040(5) -0.007(4) 0.003(5) -0.020(5) C4H 0.048(5) 0.056(5) 0.039(5) -0.010(4) -0.004(4) -0.017(4) C5H 0.31(2) 0.042(6) 0.060(8) -0.003(6) -0.023(10) 0.013(9) C6H 0.31(2) 0.049(7) 0.041(6) 0.005(5) -0.007(9) 0.003(9) C1I 0.049(5) 0.052(5) 0.062(6) -0.008(5) 0.012(4) -0.023(4) C2I 0.057(5) 0.058(5) 0.046(5) -0.003(4) -0.012(4) -0.021(4) C3I 0.063(6) 0.057(5) 0.039(5) -0.004(4) -0.016(4) -0.019(4) C4I 0.045(5) 0.046(5) 0.046(5) 0.001(4) -0.004(4) -0.019(4) C5I 0.103(8) 0.061(6) 0.042(5) -0.015(5) 0.015(5) -0.042(6) C6I 0.115(9) 0.060(6) 0.054(6) -0.014(5) 0.035(6) -0.041(6) C1Q 0.073(7) 0.081(7) 0.062(6) -0.011(5) -0.002(5) -0.045(6) C2Q 0.046(5) 0.062(5) 0.055(6) -0.014(4) -0.012(4) -0.022(4) C3Q 0.049(5) 0.062(5) 0.049(5) -0.005(4) -0.010(4) -0.023(4) C4Q 0.054(5) 0.059(5) 0.050(5) -0.013(4) -0.008(4) -0.028(4) C5Q 0.259(19) 0.28(2) 0.055(7) -0.037(10) 0.027(9) -0.241(18) C6Q 0.26(2) 0.28(2) 0.074(9) -0.025(11) -0.006(10) -0.244(19) C1R 0.039(4) 0.030(4) 0.041(5) -0.006(3) -0.006(4) 0.003(3) C2R 0.037(4) 0.037(4) 0.047(5) -0.007(4) -0.011(4) -0.008(3) C3R 0.050(5) 0.032(4) 0.041(5) -0.003(3) -0.008(4) -0.010(4) C4R 0.048(5) 0.041(4) 0.041(5) -0.008(4) -0.007(4) -0.017(4) C5R 0.065(6) 0.068(6) 0.045(5) -0.011(4) -0.012(4) -0.032(5) C6R 0.069(6) 0.054(5) 0.049(5) -0.004(4) -0.020(5) -0.022(5) O11 0.091(5) 0.114(6) 0.072(5) -0.011(4) -0.003(4) -0.082(5) O12 0.072(4) 0.049(3) 0.039(3) -0.002(3) -0.006(3) -0.021(3) C15 0.096(10) 0.125(11) 0.097(10) 0.008(8) 0.003(8) -0.041(9) C16 0.092(9) 0.132(11) 0.102(10) 0.020(8) -0.025(8) -0.055(8) C17 0.061(7) 0.123(10) 0.141(12) 0.068(9) 0.002(8) -0.037(7) C18 0.066(7) 0.066(7) 0.088(8) 0.013(6) -0.013(6) -0.017(6) C19 0.060(6) 0.058(6) 0.047(5) 0.009(4) -0.004(5) -0.021(5) C20 0.068(6) 0.050(5) 0.044(5) -0.001(4) -0.011(4) -0.023(4) O1 0.066(4) 0.064(4) 0.047(3) 0.000(3) -0.026(3) -0.021(3) O2 0.091(5) 0.048(3) 0.044(3) 0.001(3) -0.009(3) -0.011(3) O3 0.085(5) 0.058(4) 0.124(6) -0.001(4) -0.010(4) -0.046(4) O4 0.066(4) 0.082(5) 0.097(5) 0.008(4) 0.007(4) -0.031(4) O5 0.102(5) 0.059(4) 0.067(4) -0.017(3) 0.010(4) -0.022(4) O6 0.079(4) 0.053(4) 0.068(4) -0.001(3) 0.017(3) -0.031(3) C1 0.063(6) 0.062(6) 0.054(6) 0.008(5) -0.020(5) -0.009(5) C2 0.103(8) 0.069(7) 0.036(5) 0.002(5) -0.005(5) -0.009(6) C3 0.073(8) 0.070(7) 0.147(13) 0.005(8) 0.013(8) -0.028(6) C4 0.073(8) 0.173(13) 0.077(8) 0.002(9) 0.012(7) -0.066(9) C5 0.071(7) 0.057(6) 0.108(9) -0.027(6) 0.012(7) -0.023(5) C6 0.075(8) 0.052(6) 0.070(7) -0.015(5) 0.017(6) -0.033(6) C7 0.086(9) 0.053(6) 0.065(7) -0.020(6) 0.031(6) -0.041(6) C8 0.109(10) 0.049(6) 0.060(8) -0.017(6) 0.037(7) -0.041(7) C9 0.092(9) 0.062(6) 0.057(7) -0.016(6) 0.029(6) -0.044(6) C10 0.091(8) 0.054(6) 0.086(8) -0.028(6) 0.023(6) -0.033(6) Ru1 0.0357(4) 0.0335(4) 0.0264(3) 0.0042(2) -0.0036(2) -0.0121(3) C1U 0.073(10) 0.22(2) 0.105(13) 0.045(13) -0.043(9) -0.023(11) C2U 0.144(15) 0.169(16) 0.080(10) -0.029(11) -0.051(10) 0.015(12) C3U 0.134(12) 0.081(9) 0.101(11) 0.005(7) -0.038(9) -0.018(8) C4U 0.074(7) 0.099(9) 0.068(7) 0.017(6) -0.026(6) -0.026(7) C5U 0.063(7) 0.131(10) 0.082(8) 0.024(7) -0.038(6) -0.032(7) C6U 0.069(8) 0.190(15) 0.076(9) 0.059(9) -0.039(7) -0.052(9) C1V 0.073(7) 0.082(7) 0.064(7) -0.012(6) -0.004(5) -0.041(6) C2V 0.090(8) 0.108(9) 0.096(9) -0.039(8) 0.020(7) -0.057(7) C3V 0.080(7) 0.080(7) 0.077(7) -0.011(6) 0.012(6) -0.047(6) C4V 0.080(7) 0.063(6) 0.069(7) -0.014(5) -0.007(5) -0.031(5) C5V 0.066(6) 0.087(7) 0.073(7) -0.012(6) 0.003(6) -0.032(6) C6V 0.064(6) 0.095(8) 0.084(8) -0.012(6) -0.004(6) -0.041(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 C1W C6W 1.3915 . ? C1W C2W 1.3922 . ? C2W C3W 1.3917 . ? C3W C4W 1.3917 . ? C4W C5W 1.3913 . ? C5W C6W 1.3915 . ? C1X C2X 1.3916 . ? C1X C6X 1.3917 . ? C2X C3X 1.3917 . ? C3X C4X 1.3918 . ? C4X C5X 1.3914 . ? C5X C6X 1.3915 . ? C1XA Cl1X 1.7813 . ? C1XA Cl2X 1.7814 . ? C1T C6T 1.3917 . ? C1T C2T 1.3927 . ? C2T C3T 1.3916 . ? C3T C4T 1.3918 . ? C4T C5T 1.3915 . ? C5T C6T 1.3917 . ? C1TA Cl2A 1.7811 . ? C1TA Cl1A 1.7814 . ? F1 P1 1.591(5) . ? F4 P1 1.595(5) . ? F2A P1 1.597(14) . ? F3A P1 1.614(13) . ? F5A P1 1.585(13) . ? F6A P1 1.608(12) . ? F2B P1 1.658(15) . ? F3B P1 1.578(13) . ? F5B P1 1.621(13) . ? F5B F6B 1.78(2) . ? F6B P1 1.593(13) . ? P1 F62 1.5450 . ? P1 F23 1.5450 . ? P1 F56 1.5450 . ? P1 F35 1.5450 . ? F7 P2 1.600(6) . ? F10 P2 1.602(6) . ? F8 P2 1.588(7) . ? F9 P2 1.608(8) . ? F11 P2 1.551(8) . ? F12 P2 1.577(8) . ? P2 F56A 1.5450 . ? P2 F35A 1.5450 . ? P2 F62A 1.5450 . ? P2 F23A 1.5450 . ? C1Y Cl1 1.687(15) . ? C1Y Cl2 1.795(15) . ? O1Z C3Z 1.235(13) . ? C2Z C3Z 1.648(15) . ? C3Z C4Z 1.290(16) . ? O1ZA C2ZA 1.299(15) . ? O1ZA C3ZA 1.581(17) 2_556 ? C2ZA C3ZA 1.362(17) . ? C3ZA O1ZA 1.581(17) 2_556 ? O1ZB C2ZB 1.196(10) . ? C2ZB C4ZB 1.499(15) . ? C2ZB C3ZB 1.500(15) . ? O7 C4N 1.364(6) . ? O7 C11 1.425(9) . ? O8 C1O 1.378(6) . ? O8 C12 1.450(10) . ? O9 C4M 1.362(5) . ? O9 C13 1.409(9) . ? O10 C1R 1.385(6) . ? O10 C14 1.414(9) . ? C1H O2 1.373(7) . ? C1H C2H 1.3949 . ? C1H C6H 1.3953 . ? C2H C3H 1.3950 . ? C3H C4H 1.3953 . ? C4H C5H 1.3949 . ? C4H C4I 1.506(5) . ? C5H C6H 1.3949 . ? C1I O6 1.382(7) . ? C1I C6I 1.3950 . ? C1I C2I 1.3951 . ? C2I C3I 1.3950 . ? C3I C4I 1.3953 . ? C4I C5I 1.3946 . ? C5I C6I 1.3950 . ? C1Q O11 1.368(7) . ? C1Q C2Q 1.3953 . ? C1Q C6Q 1.3954 . ? C2Q C3Q 1.3950 . ? C3Q C4Q 1.3952 . ? C4Q C5Q 1.3953 . ? C4Q C4R 1.539(5) . ? C5Q C6Q 1.3950 . ? C1R C2R 1.3949 . ? C1R C6R 1.3951 . ? C2R C3R 1.3949 . ? C3R C4R 1.3952 . ? C4R C5R 1.3946 . ? C5R C6R 1.3952 . ? O11 C15 1.281(16) . ? O12 C4P 1.369(6) . ? O12 C20 1.450(9) . ? C11 C12 1.498(11) . ? C13 C14 1.482(10) . ? C15 C16 1.548(17) . ? C16 C17 1.188(16) . ? C17 C18 1.394(16) . ? C18 C19 1.175(13) . ? C19 C20 1.441(12) . ? N1J C2J 1.366(9) . ? N1J C6J 1.369(9) . ? N1J Ru1 1.971(5) . ? C2J C3J 1.385(10) . ? C2J C1K 1.462(10) . ? C3J C4J 1.389(11) . ? C4J C5J 1.400(10) . ? C5J C6J 1.385(10) . ? C6J C1L 1.467(10) . ? C1K N6K 1.369(9) . ? C1K C2K 1.380(10) . ? C2K C3K 1.384(10) . ? C3K C4K 1.398(10) . ? C4K C5K 1.397(10) . ? C4K C1N 1.491(8) . ? C5K N6K 1.339(9) . ? N6K Ru1 2.060(6) . ? C1L C2L 1.380(10) . ? C1L N6L 1.382(9) . ? C2L C3L 1.394(10) . ? C3L C4L 1.391(10) . ? C4L C5L 1.389(10) . ? C4L C1M 1.512(7) . ? C5L N6L 1.341(9) . ? N6L Ru1 2.046(6) . ? C1M C6M 1.3913 . ? C1M C2M 1.3918 . ? C2M C3M 1.3914 . ? C2M C8M 1.524(8) . ? C3M C4M 1.3924 . ? C4M C5M 1.3918 . ? C5M C6M 1.3916 . ? C6M C7M 1.527(8) . ? C1N C2N 1.3916 . ? C1N C6N 1.3920 . ? C2N C3N 1.3913 . ? C2N C8N 1.528(9) . ? C3N C4N 1.3920 . ? C4N C5N 1.3916 . ? C5N C6N 1.3920 . ? C6N C7N 1.526(8) . ? C1O C2O 1.3917 . ? C1O C6O 1.3917 . ? C2O C3O 1.3916 . ? C3O C4O 1.3919 . ? C4O C5O 1.3909 . ? C4O C1P 1.515(5) . ? C5O C6O 1.3914 . ? C1P C2P 1.3917 . ? C1P C6P 1.3920 . ? C2P C3P 1.3914 . ? C3P C4P 1.3916 . ? C4P C5P 1.3914 . ? C5P C6P 1.3916 . ? O1 C4D 1.373(6) . ? O1 C1 1.399(10) . ? O2 C2 1.446(10) . ? O3 C4E 1.370(7) . ? O3 C3 1.381(13) . ? O4 C1F 1.365(9) . ? O4 C4 1.518(14) . ? O5 C4G 1.363(8) . ? O5 C10 1.413(11) . ? O6 C5 1.441(11) . ? C1 C2 1.464(13) . ? C3 C4 1.366(17) . ? C5 C6 1.441(17) . ? C6 C7 1.166(16) . ? C7 C8 1.39(2) . ? C8 C9 1.221(17) . ? C9 C10 1.482(17) . ? N1A C2A 1.342(9) . ? N1A C6A 1.376(9) . ? N1A Ru1 1.976(6) . ? C2A C3A 1.403(10) . ? C2A C1C 1.470(10) . ? C3A C4A 1.379(11) . ? C4A C5A 1.387(11) . ? C5A C6A 1.399(10) . ? C6A C1B 1.432(10) . ? C1B N2B 1.374(9) . ? C1B C6B 1.380(11) . ? N2B C3B 1.346(9) . ? N2B Ru1 2.062(6) . ? C3B C4B 1.380(10) . ? C4B C5B 1.397(11) . ? C4B C1E 1.496(8) . ? C5B C6B 1.390(11) . ? C1C N2C 1.374(9) . ? C1C C6C 1.378(11) . ? N2C C3C 1.329(9) . ? N2C Ru1 2.059(6) . ? C3C C4C 1.389(10) . ? C4C C5C 1.396(11) . ? C4C C1D 1.480(8) . ? C5C C6C 1.366(11) . ? C1D C6D 1.3916 . ? C1D C2D 1.3919 . ? C2D C3D 1.3907 . ? C2D C8D 1.505(9) . ? C3D C4D 1.3920 . ? C4D C5D 1.3914 . ? C5D C6D 1.3916 . ? C6D C7D 1.513(9) . ? C1E C2E 1.3914 . ? C1E C6E 1.3919 . ? C2E C3E 1.3914 . ? C2E C8E 1.513(10) . ? C3E C4E 1.3920 . ? C4E C5E 1.3918 . ? C5E C6E 1.3919 . ? C6E C7E 1.510(10) . ? C1F C6F 1.3914 . ? C1F C2F 1.3920 . ? C2F C3F 1.3917 . ? C3F C4F 1.3919 . ? C4F C5F 1.3913 . ? C4F C1G 1.492(6) . ? C5F C6F 1.3913 . ? C1G C6G 1.3910 . ? C1G C2G 1.3918 . ? C2G C3G 1.3921 . ? C3G C4G 1.3913 . ? C4G C5G 1.3913 . ? C5G C6G 1.3919 . ? C1S C2S 1.3913 . ? C1S C6S 1.3919 . ? C2S C3S 1.3917 . ? C3S C4S 1.3918 . ? C4S C5S 1.3906 . ? C5S C6S 1.3920 . ? C1U C6U 1.3913 . ? C1U C2U 1.3915 . ? C2U C3U 1.3915 . ? C3U C4U 1.3920 . ? C4U C5U 1.3913 . ? C5U C6U 1.3917 . ? C1V C6V 1.3920 . ? C1V C2V 1.3923 . ? C2V C3V 1.3919 . ? C3V C4V 1.3916 . ? C4V C5V 1.3912 . ? C5V C6V 1.3911 . ? 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 C6W C1W C2W 120.0 . . ? C3W C2W C1W 120.0 . . ? C4W C3W C2W 120.0 . . ? C5W C4W C3W 120.0 . . ? C4W C5W C6W 120.0 . . ? C5W C6W C1W 120.0 . . ? C2X C1X C6X 120.0 . . ? C1X C2X C3X 120.0 . . ? C2X C3X C4X 120.0 . . ? C5X C4X C3X 120.0 . . ? C4X C5X C6X 120.0 . . ? C5X C6X C1X 120.0 . . ? Cl1X C1XA Cl2X 112.4 . . ? C6T C1T C2T 120.0 . . ? C3T C2T C1T 120.0 . . ? C2T C3T C4T 120.0 . . ? C5T C4T C3T 120.0 . . ? C4T C5T C6T 120.0 . . ? C5T C6T C1T 120.0 . . ? Cl2A C1TA Cl1A 112.4 . . ? P1 F5B F6B 55.7(6) . . ? P1 F6B F5B 57.2(7) . . ? F62 P1 F23 90.0 . . ? F62 P1 F56 90.0 . . ? F23 P1 F56 180.0 . . ? F62 P1 F35 180.0 . . ? F23 P1 F35 90.0 . . ? F56 P1 F35 90.0 . . ? F62 P1 F3B 138.0(15) . . ? F23 P1 F3B 48.5(15) . . ? F56 P1 F3B 131.5(15) . . ? F35 P1 F3B 42.0(15) . . ? F62 P1 F5A 155.1(12) . . ? F23 P1 F5A 114.9(12) . . ? F56 P1 F5A 65.1(12) . . ? F35 P1 F5A 24.9(12) . . ? F3B P1 F5A 66.7(9) . . ? F62 P1 F1 93.7(11) . . ? F23 P1 F1 84.3(11) . . ? F56 P1 F1 95.7(11) . . ? F35 P1 F1 86.3(11) . . ? F3B P1 F1 88.5(6) . . ? F5A P1 F1 88.9(5) . . ? F62 P1 F6B 64.4(12) . . ? F23 P1 F6B 154.0(12) . . ? F56 P1 F6B 26.0(12) . . ? F35 P1 F6B 115.5(12) . . ? F3B P1 F6B 157.4(9) . . ? F5A P1 F6B 90.8(8) . . ? F1 P1 F6B 92.2(6) . . ? F62 P1 F4 86.9(11) . . ? F23 P1 F4 96.0(11) . . ? F56 P1 F4 84.0(11) . . ? F35 P1 F4 93.1(11) . . ? F3B P1 F4 91.2(6) . . ? F5A P1 F4 90.4(5) . . ? F1 P1 F4 179.3(4) . . ? F6B P1 F4 87.8(6) . . ? F62 P1 F2A 45.3(15) . . ? F23 P1 F2A 44.9(16) . . ? F56 P1 F2A 135.1(16) . . ? F35 P1 F2A 134.7(15) . . ? F3B P1 F2A 93.4(8) . . ? F5A P1 F2A 159.4(9) . . ? F1 P1 F2A 85.3(6) . . ? F6B P1 F2A 109.2(9) . . ? F4 P1 F2A 95.4(6) . . ? F62 P1 F6A 43.2(15) . . ? F23 P1 F6A 130.4(16) . . ? F56 P1 F6A 49.6(16) . . ? F35 P1 F6A 136.8(15) . . ? F3B P1 F6A 172.5(7) . . ? F5A P1 F6A 112.9(8) . . ? F1 P1 F6A 84.0(5) . . ? F6B P1 F6A 23.8(7) . . ? F4 P1 F6A 96.3(5) . . ? F2A P1 F6A 86.2(7) . . ? F62 P1 F3A 113.2(13) . . ? F23 P1 F3A 26.2(13) . . ? F56 P1 F3A 153.8(13) . . ? F35 P1 F3A 66.8(13) . . ? F3B P1 F3A 25.2(6) . . ? F5A P1 F3A 91.2(7) . . ? F1 P1 F3A 94.8(5) . . ? F6B P1 F3A 172.7(7) . . ? F4 P1 F3A 85.2(5) . . ? F2A P1 F3A 69.7(8) . . ? F6A P1 F3A 155.9(8) . . ? F56A P2 F35A 90.0 . . ? F56A P2 F62A 90.0 . . ? F35A P2 F62A 180.0 . . ? F56A P2 F23A 180.0 . . ? F35A P2 F23A 90.0 . . ? F62A P2 F23A 90.0 . . ? F56A P2 F11 59.3(7) . . ? F35A P2 F11 32.0(7) . . ? F62A P2 F11 148.0(7) . . ? F23A P2 F11 120.7(7) . . ? F56A P2 F12 34.0(7) . . ? F35A P2 F12 123.3(6) . . ? F62A P2 F12 56.7(6) . . ? F23A P2 F12 146.0(7) . . ? F11 P2 F12 93.3(6) . . ? F56A P2 F8 123.7(7) . . ? F35A P2 F8 144.5(7) . . ? F62A P2 F8 35.5(7) . . ? F23A P2 F8 56.3(7) . . ? F11 P2 F8 176.4(6) . . ? F12 P2 F8 89.7(5) . . ? F56A P2 F7 89.0(8) . . ? F35A P2 F7 83.3(8) . . ? F62A P2 F7 96.7(8) . . ? F23A P2 F7 91.0(8) . . ? F11 P2 F7 92.0(5) . . ? F12 P2 F7 86.9(4) . . ? F8 P2 F7 86.2(4) . . ? F56A P2 F10 91.0(8) . . ? F35A P2 F10 99.1(8) . . ? F62A P2 F10 80.9(8) . . ? F23A P2 F10 89.1(8) . . ? F11 P2 F10 90.0(5) . . ? F12 P2 F10 91.8(4) . . ? F8 P2 F10 91.9(4) . . ? F7 P2 F10 177.6(3) . . ? F56A P2 F9 150.3(7) . . ? F35A P2 F9 60.5(7) . . ? F62A P2 F9 119.5(7) . . ? F23A P2 F9 29.7(7) . . ? F11 P2 F9 91.0(6) . . ? F12 P2 F9 175.3(5) . . ? F8 P2 F9 86.0(5) . . ? F7 P2 F9 91.0(4) . . ? F10 P2 F9 90.2(4) . . ? Cl1 C1Y Cl2 108.3(9) . . ? O1Z C3Z C4Z 104.5(15) . . ? O1Z C3Z C2Z 119.9(10) . . ? C4Z C3Z C2Z 135.4(14) . . ? C2ZA O1ZA C3ZA 122.8(11) . 2_556 ? O1ZA C2ZA C3ZA 119.5(13) . . ? C2ZA C3ZA O1ZA 117.8(11) . 2_556 ? O1ZB C2ZB C4ZB 123.2(11) . . ? O1ZB C2ZB C3ZB 122.8(10) . . ? C4ZB C2ZB C3ZB 113.9(10) . . ? C4N O7 C11 117.1(5) . . ? C1O O8 C12 115.7(6) . . ? C4M O9 C13 118.2(5) . . ? C1R O10 C14 118.9(5) . . ? O2 C1H C2H 114.9(4) . . ? O2 C1H C6H 125.0(4) . . ? C2H C1H C6H 120.0 . . ? C1H C2H C3H 120.0 . . ? C2H C3H C4H 120.0 . . ? C5H C4H C3H 120.0 . . ? C5H C4H C4I 118.0(4) . . ? C3H C4H C4I 122.0(4) . . ? C4H C5H C6H 120.0 . . ? C5H C6H C1H 120.0 . . ? O6 C1I C6I 124.8(4) . . ? O6 C1I C2I 115.2(4) . . ? C6I C1I C2I 120.0 . . ? C3I C2I C1I 120.0 . . ? C2I C3I C4I 120.0 . . ? C5I C4I C3I 120.0 . . ? C5I C4I C4H 119.2(4) . . ? C3I C4I C4H 120.7(4) . . ? C4I C5I C6I 120.0 . . ? C5I C6I C1I 120.0 . . ? O11 C1Q C2Q 122.1(5) . . ? O11 C1Q C6Q 117.8(5) . . ? C2Q C1Q C6Q 120.0 . . ? C3Q C2Q C1Q 120.0 . . ? C2Q C3Q C4Q 120.0 . . ? C3Q C4Q C5Q 120.0 . . ? C3Q C4Q C4R 119.5(4) . . ? C5Q C4Q C4R 120.5(4) . . ? C6Q C5Q C4Q 120.0 . . ? C5Q C6Q C1Q 120.0 . . ? O10 C1R C2R 124.3(4) . . ? O10 C1R C6R 115.7(4) . . ? C2R C1R C6R 120.0 . . ? C1R C2R C3R 120.0 . . ? C2R C3R C4R 120.0 . . ? C5R C4R C3R 120.0 . . ? C5R C4R C4Q 121.5(4) . . ? C3R C4R C4Q 118.5(4) . . ? C4R C5R C6R 120.0 . . ? C1R C6R C5R 120.0 . . ? C15 O11 C1Q 120.0(8) . . ? C4P O12 C20 117.9(5) . . ? O7 C11 C12 106.7(6) . . ? O8 C12 C11 111.8(7) . . ? O9 C13 C14 108.5(6) . . ? O10 C14 C13 112.4(7) . . ? O11 C15 C16 111.6(12) . . ? C17 C16 C15 176.1(16) . . ? C16 C17 C18 168.1(19) . . ? C19 C18 C17 174.7(12) . . ? C18 C19 C20 178.8(11) . . ? C19 C20 O12 112.3(7) . . ? C2J N1J C6J 122.1(6) . . ? C2J N1J Ru1 118.6(5) . . ? C6J N1J Ru1 119.3(4) . . ? N1J C2J C3J 119.4(6) . . ? N1J C2J C1K 112.5(6) . . ? C3J C2J C1K 128.1(7) . . ? C2J C3J C4J 119.4(7) . . ? C3J C4J C5J 120.6(7) . . ? C6J C5J C4J 118.8(7) . . ? N1J C6J C5J 119.7(6) . . ? N1J C6J C1L 112.1(6) . . ? C5J C6J C1L 128.2(7) . . ? N6K C1K C2K 119.7(7) . . ? N6K C1K C2J 115.6(6) . . ? C2K C1K C2J 124.7(6) . . ? C1K C2K C3K 120.7(7) . . ? C2K C3K C4K 120.0(7) . . ? C5K C4K C3K 116.4(7) . . ? C5K C4K C1N 119.4(6) . . ? C3K C4K C1N 124.1(7) . . ? N6K C5K C4K 123.7(7) . . ? C5K N6K C1K 119.5(6) . . ? C5K N6K Ru1 126.6(5) . . ? C1K N6K Ru1 113.7(4) . . ? C2L C1L N6L 120.9(6) . . ? C2L C1L C6J 124.5(6) . . ? N6L C1L C6J 114.6(6) . . ? C1L C2L C3L 119.8(7) . . ? C4L C3L C2L 119.1(7) . . ? C5L C4L C3L 118.5(7) . . ? C5L C4L C1M 116.9(6) . . ? C3L C4L C1M 124.6(6) . . ? N6L C5L C4L 122.9(7) . . ? C5L N6L C1L 118.6(6) . . ? C5L N6L Ru1 126.8(5) . . ? C1L N6L Ru1 114.6(4) . . ? C6M C1M C2M 120.0 . . ? C6M C1M C4L 120.0(4) . . ? C2M C1M C4L 119.7(4) . . ? C3M C2M C1M 120.0 . . ? C3M C2M C8M 117.2(4) . . ? C1M C2M C8M 122.7(4) . . ? C2M C3M C4M 120.0 . . ? O9 C4M C5M 115.6(3) . . ? O9 C4M C3M 124.3(3) . . ? C5M C4M C3M 120.0 . . ? C6M C5M C4M 120.0 . . ? C1M C6M C5M 120.0 . . ? C1M C6M C7M 122.5(4) . . ? C5M C6M C7M 117.4(4) . . ? C2N C1N C6N 120.0 . . ? C2N C1N C4K 120.0(4) . . ? C6N C1N C4K 119.9(4) . . ? C3N C2N C1N 120.0 . . ? C3N C2N C8N 115.8(5) . . ? C1N C2N C8N 124.0(5) . . ? C2N C3N C4N 120.0 . . ? O7 C4N C5N 124.0(4) . . ? O7 C4N C3N 115.9(4) . . ? C5N C4N C3N 120.0 . . ? C4N C5N C6N 120.0 . . ? C5N C6N C1N 120.0 . . ? C5N C6N C7N 116.0(4) . . ? C1N C6N C7N 124.0(4) . . ? O8 C1O C2O 116.6(4) . . ? O8 C1O C6O 123.3(4) . . ? C2O C1O C6O 120.0 . . ? C3O C2O C1O 120.0 . . ? C2O C3O C4O 120.0 . . ? C5O C4O C3O 120.0 . . ? C5O C4O C1P 119.6(4) . . ? C3O C4O C1P 120.5(4) . . ? C4O C5O C6O 120.0 . . ? C5O C6O C1O 120.0 . . ? C2P C1P C6P 120.0 . . ? C2P C1P C4O 120.5(4) . . ? C6P C1P C4O 119.5(4) . . ? C3P C2P C1P 120.0 . . ? C2P C3P C4P 120.0 . . ? O12 C4P C5P 114.4(4) . . ? O12 C4P C3P 125.6(4) . . ? C5P C4P C3P 120.0 . . ? C4P C5P C6P 120.0 . . ? C5P C6P C1P 120.0 . . ? C4D O1 C1 118.9(6) . . ? C1H O2 C2 116.5(6) . . ? C4E O3 C3 120.2(9) . . ? C1F O4 C4 113.2(8) . . ? C4G O5 C10 119.7(7) . . ? C1I O6 C5 117.7(7) . . ? O1 C1 C2 114.1(9) . . ? O2 C2 C1 106.9(8) . . ? C4 C3 O3 117.3(12) . . ? C3 C4 O4 109.9(10) . . ? O6 C5 C6 113.5(9) . . ? C7 C6 C5 178.2(11) . . ? C6 C7 C8 176.4(11) . . ? C9 C8 C7 177.9(11) . . ? C8 C9 C10 173.4(10) . . ? O5 C10 C9 109.5(8) . . ? C2A N1A C6A 123.3(6) . . ? C2A N1A Ru1 118.4(5) . . ? C6A N1A Ru1 118.1(5) . . ? N1A C2A C3A 120.1(7) . . ? N1A C2A C1C 113.5(6) . . ? C3A C2A C1C 126.4(7) . . ? C4A C3A C2A 118.0(8) . . ? C3A C4A C5A 121.4(8) . . ? C4A C5A C6A 119.8(8) . . ? N1A C6A C5A 117.5(7) . . ? N1A C6A C1B 113.2(6) . . ? C5A C6A C1B 129.3(7) . . ? N2B C1B C6B 119.9(7) . . ? N2B C1B C6A 115.6(6) . . ? C6B C1B C6A 124.5(7) . . ? C3B N2B C1B 118.5(6) . . ? C3B N2B Ru1 127.2(5) . . ? C1B N2B Ru1 113.9(5) . . ? N2B C3B C4B 124.8(7) . . ? C3B C4B C5B 116.1(7) . . ? C3B C4B C1E 120.2(7) . . ? C5B C4B C1E 123.6(7) . . ? C6B C5B C4B 120.2(8) . . ? C1B C6B C5B 120.4(8) . . ? N2C C1C C6C 119.9(7) . . ? N2C C1C C2A 114.8(6) . . ? C6C C1C C2A 125.2(7) . . ? C3C N2C C1C 118.7(6) . . ? C3C N2C Ru1 127.2(5) . . ? C1C N2C Ru1 113.5(5) . . ? N2C C3C C4C 124.0(7) . . ? C3C C4C C5C 116.4(7) . . ? C3C C4C C1D 122.0(6) . . ? C5C C4C C1D 121.6(7) . . ? C6C C5C C4C 120.1(8) . . ? C5C C6C C1C 120.5(8) . . ? C6D C1D C2D 120.0 . . ? C6D C1D C4C 119.6(4) . . ? C2D C1D C4C 120.2(4) . . ? C3D C2D C1D 120.0 . . ? C3D C2D C8D 116.6(5) . . ? C1D C2D C8D 123.4(5) . . ? C2D C3D C4D 120.0 . . ? O1 C4D C5D 125.3(4) . . ? O1 C4D C3D 114.7(4) . . ? C5D C4D C3D 120.0 . . ? C4D C5D C6D 120.0 . . ? C5D C6D C1D 120.0 . . ? C5D C6D C7D 117.0(4) . . ? C1D C6D C7D 123.0(4) . . ? C2E C1E C6E 120.0 . . ? C2E C1E C4B 118.2(4) . . ? C6E C1E C4B 121.8(4) . . ? C3E C2E C1E 120.1 . . ? C3E C2E C8E 119.0(5) . . ? C1E C2E C8E 121.0(5) . . ? C2E C3E C4E 120.0 . . ? O3 C4E C5E 114.6(5) . . ? O3 C4E C3E 125.4(5) . . ? C5E C4E C3E 120.0 . . ? C4E C5E C6E 120.0 . . ? C1E C6E C5E 120.0 . . ? C1E C6E C7E 122.1(5) . . ? C5E C6E C7E 117.7(5) . . ? O4 C1F C6F 124.2(5) . . ? O4 C1F C2F 115.7(5) . . ? C6F C1F C2F 120.0 . . ? C3F C2F C1F 120.0 . . ? C2F C3F C4F 120.0 . . ? C5F C4F C3F 120.0 . . ? C5F C4F C1G 118.6(4) . . ? C3F C4F C1G 121.3(4) . . ? C6F C5F C4F 120.0 . . ? C5F C6F C1F 120.0 . . ? C6G C1G C2G 120.0 . . ? C6G C1G C4F 119.1(4) . . ? C2G C1G C4F 120.9(4) . . ? C1G C2G C3G 120.0 . . ? C4G C3G C2G 120.0 . . ? O5 C4G C3G 125.0(5) . . ? O5 C4G C5G 115.0(5) . . ? C3G C4G C5G 120.0 . . ? C4G C5G C6G 120.0 . . ? C1G C6G C5G 120.0 . . ? N1J Ru1 N1A 178.6(2) . . ? N1J Ru1 N6L 79.1(2) . . ? N1A Ru1 N6L 102.2(2) . . ? N1J Ru1 N2C 100.0(2) . . ? N1A Ru1 N2C 79.5(2) . . ? N6L Ru1 N2C 96.6(2) . . ? N1J Ru1 N6K 79.5(2) . . ? N1A Ru1 N6K 99.2(2) . . ? N6L Ru1 N6K 158.5(2) . . ? N2C Ru1 N6K 85.6(2) . . ? N1J Ru1 N2B 101.4(2) . . ? N1A Ru1 N2B 79.0(2) . . ? N6L Ru1 N2B 87.7(2) . . ? N2C Ru1 N2B 158.5(2) . . ? N6K Ru1 N2B 98.2(2) . . ? C2S C1S C6S 120.0 . . ? C1S C2S C3S 120.0 . . ? C2S C3S C4S 120.0 . . ? C5S C4S C3S 120.0 . . ? C4S C5S C6S 120.0 . . ? C1S C6S C5S 120.0 . . ? C6U C1U C2U 120.0 . . ? C1U C2U C3U 120.0 . . ? C2U C3U C4U 120.0 . . ? C5U C4U C3U 120.0 . . ? C4U C5U C6U 120.0 . . ? C1U C6U C5U 120.0 . . ? C6V C1V C2V 119.9 . . ? C3V C2V C1V 120.0 . . ? C4V C3V C2V 120.0 . . ? C5V C4V C3V 120.0 . . ? C6V C5V C4V 120.0 . . ? C5V C6V C1V 120.0 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 22.57 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.308 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.114 data_SG0306 _database_code_depnum_ccdc_archive 'CCDC 274362' _audit_creation_method SHELXL-97 _audit_creation_date 03-02-26 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C66 H62 Fe N6 O4 2+, 2(F6 P 1-), H2 O' _chemical_formula_sum 'C66 H64 F12 Fe N6 O5 P2' _chemical_formula_weight 1367.02 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 264 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 256 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Fe Fe 4 0.3463 0.8444 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 24 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 20 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 23.3906(5) _cell_length_b 11.4829(2) _cell_length_c 23.2945(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6256.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 110335 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 0.384 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_T_max 0.994 _exptl_special_details ; Solvent used: dichloromethane / benzene Cooling Device: Oxford Cryosystems Cryostream 700Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.929(2) Frames collected: 439 Seconds exposure per frame: 90 Degrees rotation per frame: 1.0 Crystal-Detector distance (mm): 35.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 75497 _diffrn_reflns_av_R_equivalents 0.1679 _diffrn_reflns_av_sigmaI/netI 0.0814 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 24.99 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 5489 _reflns_number_gt 3041 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2002)' _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 'w=1/[\s^2^(Fo^2^)+(0.1189P)^2^+8.3355P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5489 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1491 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2337 _refine_ls_wR_factor_gt 0.1913 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.252 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.089 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 1.0000 0.17935(9) 0.2500 0.0368(3) Uani 1 2 d S . . O1 O 0.6991(2) -0.3210(4) 0.1831(2) 0.0844(15) Uani 1 1 d . . . O2 O 1.01219(18) 0.7366(3) 0.54360(15) 0.0550(11) Uani 1 1 d . . . N1 N 0.97380(19) 0.0535(4) 0.19855(17) 0.0389(11) Uani 1 1 d . . . N2 N 1.06173(19) 0.1785(3) 0.19836(16) 0.0372(10) Uani 1 1 d . . . N3 N 1.04744(18) 0.3044(3) 0.28485(17) 0.0372(10) Uani 1 1 d . . . C2 C 0.9249(2) -0.0075(4) 0.2021(2) 0.0401(13) Uani 1 1 d . . . H2 H 0.8969 0.0166 0.2292 0.048 Uiso 1 1 calc R . . C3 C 0.9131(2) -0.1046(4) 0.1679(2) 0.0410(13) Uani 1 1 d . . . C4 C 0.9541(3) -0.1385(5) 0.1289(2) 0.0504(15) Uani 1 1 d . . . H4 H 0.9477 -0.2044 0.1052 0.060 Uiso 1 1 calc R . . C5 C 1.0042(3) -0.0772(5) 0.1243(2) 0.0491(15) Uani 1 1 d . . . H5 H 1.0326 -0.1016 0.0978 0.059 Uiso 1 1 calc R . . C6 C 1.0135(2) 0.0204(4) 0.1583(2) 0.0401(13) Uani 1 1 d . . . C7 C 1.0637(2) 0.0964(4) 0.1562(2) 0.0420(13) Uani 1 1 d . . . C8 C 1.1083(3) 0.0934(6) 0.1180(2) 0.0549(16) Uani 1 1 d . . . H8 H 1.1096 0.0354 0.0889 0.066 Uiso 1 1 calc R . . C9 C 1.1513(3) 0.1761(6) 0.1223(3) 0.0623(17) Uani 1 1 d . . . H9 H 1.1820 0.1761 0.0957 0.075 Uiso 1 1 calc R . . C10 C 1.1491(3) 0.2591(5) 0.1657(2) 0.0551(16) Uani 1 1 d . . . H10 H 1.1784 0.3159 0.1692 0.066 Uiso 1 1 calc R . . C11 C 1.1042(2) 0.2579(5) 0.2036(2) 0.0443(14) Uani 1 1 d . . . C12 C 1.0940(2) 0.3339(4) 0.2524(2) 0.0431(13) Uani 1 1 d . . . C13 C 1.1276(2) 0.4313(5) 0.2670(2) 0.0467(14) Uani 1 1 d . . . H13 H 1.1595 0.4524 0.2441 0.056 Uiso 1 1 calc R . . C14 C 1.1138(2) 0.4953(5) 0.3146(2) 0.0486(15) Uani 1 1 d . . . H14 H 1.1358 0.5621 0.3239 0.058 Uiso 1 1 calc R . . C15 C 1.0681(2) 0.4642(4) 0.3495(2) 0.0424(13) Uani 1 1 d . . . C16 C 1.0364(2) 0.3672(5) 0.3317(2) 0.0411(13) Uani 1 1 d . . . H16 H 1.0047 0.3446 0.3546 0.049 Uiso 1 1 calc R . . C17 C 0.8577(3) -0.1632(5) 0.1728(2) 0.0484(15) Uani 1 1 d . . . C18 C 0.8413(3) -0.2146(5) 0.2231(3) 0.0597(17) Uani 1 1 d . . . C19 C 0.7857(3) -0.2678(6) 0.2257(3) 0.073(2) Uani 1 1 d . . . H19 H 0.7717 -0.3022 0.2600 0.088 Uiso 1 1 calc R . . C20 C 0.7530(2) -0.2669(5) 0.1751(3) 0.0494(14) Uani 1 1 d . . . C21 C 0.7697(3) -0.2162(6) 0.1260(3) 0.0675(19) Uani 1 1 d . . . H21 H 0.7450 -0.2170 0.0937 0.081 Uiso 1 1 calc R . . C22 C 0.8211(3) -0.1644(5) 0.1221(3) 0.0654(18) Uani 1 1 d . . . C23 C 0.8790(4) -0.2180(6) 0.2750(3) 0.086(2) Uani 1 1 d . . . H231 H 0.9177 -0.2407 0.2637 0.129 Uiso 1 1 calc R . . H232 H 0.8639 -0.2748 0.3025 0.129 Uiso 1 1 calc R . . H233 H 0.8800 -0.1407 0.2929 0.129 Uiso 1 1 calc R . . C24 C 0.6632(4) -0.3214(8) 0.1323(3) 0.096(3) Uani 1 1 d . . . H241 H 0.6566 -0.2412 0.1197 0.144 Uiso 1 1 calc R . . H242 H 0.6266 -0.3584 0.1413 0.144 Uiso 1 1 calc R . . H243 H 0.6823 -0.3651 0.1016 0.144 Uiso 1 1 calc R . . C25 C 0.8396(3) -0.1126(6) 0.0645(3) 0.075(2) Uani 1 1 d . . . H251 H 0.8621 -0.1702 0.0433 0.113 Uiso 1 1 calc R . . H252 H 0.8628 -0.0429 0.0713 0.113 Uiso 1 1 calc R . . H253 H 0.8056 -0.0915 0.0422 0.113 Uiso 1 1 calc R . . C26 C 1.0519(2) 0.5311(4) 0.4019(2) 0.0412(13) Uani 1 1 d . . . C27 C 0.9955(2) 0.5713(5) 0.4091(2) 0.0441(14) Uani 1 1 d . . . C28 C 0.9811(2) 0.6396(4) 0.4567(2) 0.0424(13) Uani 1 1 d . . . H28 H 0.9430 0.6666 0.4615 0.051 Uiso 1 1 calc R . . C29 C 1.0222(3) 0.6676(4) 0.4966(2) 0.0429(14) Uani 1 1 d . . . C30 C 1.0773(3) 0.6263(5) 0.4909(2) 0.0467(14) Uani 1 1 d . . . H30 H 1.1049 0.6445 0.5194 0.056 Uiso 1 1 calc R . . C31 C 1.0931(2) 0.5589(5) 0.4442(2) 0.0458(14) Uani 1 1 d . . . C32 C 0.9475(3) 0.5468(6) 0.3665(2) 0.0600(17) Uani 1 1 d . . . H321 H 0.9631 0.5449 0.3275 0.090 Uiso 1 1 calc R . . H322 H 0.9186 0.6082 0.3693 0.090 Uiso 1 1 calc R . . H323 H 0.9300 0.4714 0.3755 0.090 Uiso 1 1 calc R . . C33 C 0.9574(3) 0.7900(5) 0.5458(2) 0.0581(17) Uani 1 1 d . . . H331 H 0.9520 0.8390 0.5118 0.087 Uiso 1 1 calc R . . H332 H 0.9545 0.8381 0.5804 0.087 Uiso 1 1 calc R . . H333 H 0.9277 0.7296 0.5467 0.087 Uiso 1 1 calc R . . C34 C 1.1544(3) 0.5149(5) 0.4417(3) 0.0567(16) Uani 1 1 d . . . H341 H 1.1770 0.5658 0.4168 0.085 Uiso 1 1 calc R . . H342 H 1.1548 0.4354 0.4264 0.085 Uiso 1 1 calc R . . H343 H 1.1708 0.5151 0.4805 0.085 Uiso 1 1 calc R . . P1 P 0.80461(8) 0.80783(15) 0.44489(7) 0.0592(5) Uani 1 1 d . . . F1A F 0.8659(12) 0.823(2) 0.4280(13) 0.134(10) Uani 0.54(4) 1 d P A 1 F2A F 0.7381(14) 0.783(3) 0.4710(12) 0.089(7) Uani 0.54(4) 1 d P A 1 F3A F 0.7971(6) 0.9470(12) 0.4506(10) 0.077(4) Uani 0.54(4) 1 d P A 1 F4A F 0.8236(7) 0.807(3) 0.5122(6) 0.103(6) Uani 0.54(4) 1 d P A 1 F5A F 0.8107(9) 0.6739(17) 0.4455(11) 0.113(7) Uani 0.54(4) 1 d P A 1 F6A F 0.7803(7) 0.8096(18) 0.3839(8) 0.077(6) Uani 0.54(4) 1 d P A 1 F1B F 0.8702(9) 0.8176(15) 0.4185(8) 0.047(5) Uani 0.46(4) 1 d P A 2 F2B F 0.7445(16) 0.810(4) 0.4645(16) 0.092(9) Uani 0.46(4) 1 d P A 2 F3B F 0.818(2) 0.920(3) 0.4754(13) 0.136(12) Uani 0.46(4) 1 d P A 2 F4B F 0.8275(7) 0.737(3) 0.4978(9) 0.099(7) Uani 0.46(4) 1 d P A 2 F5B F 0.7988(10) 0.686(2) 0.4121(17) 0.118(12) Uani 0.46(4) 1 d P A 2 F6B F 0.7880(14) 0.871(4) 0.3886(13) 0.142(13) Uani 0.46(4) 1 d P A 2 O3 O 0.7183(4) 0.0260(7) 0.3390(4) 0.077(3) Uani 0.50 1 d P . . 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 0.0460(7) 0.0327(6) 0.0316(6) 0.000 0.0050(5) 0.000 O1 0.071(3) 0.081(4) 0.101(4) 0.004(3) 0.006(3) -0.007(3) O2 0.075(3) 0.049(2) 0.042(2) -0.0085(18) -0.004(2) -0.002(2) N1 0.050(3) 0.034(2) 0.032(2) -0.0026(18) -0.004(2) 0.004(2) N2 0.050(3) 0.032(2) 0.030(2) 0.0020(19) 0.0017(19) 0.005(2) N3 0.045(3) 0.036(2) 0.031(2) 0.0039(19) 0.0052(19) -0.001(2) C2 0.048(4) 0.038(3) 0.034(3) -0.001(2) 0.001(2) 0.005(3) C3 0.048(3) 0.035(3) 0.040(3) -0.004(2) -0.011(3) 0.005(3) C4 0.061(4) 0.042(3) 0.048(4) -0.012(3) -0.012(3) 0.007(3) C5 0.060(4) 0.047(3) 0.040(3) -0.006(3) 0.008(3) 0.014(3) C6 0.048(3) 0.037(3) 0.035(3) -0.002(2) 0.000(2) 0.009(3) C7 0.052(4) 0.036(3) 0.037(3) 0.003(2) 0.005(3) 0.013(3) C8 0.058(4) 0.061(4) 0.046(3) -0.005(3) 0.014(3) 0.011(3) C9 0.061(4) 0.063(4) 0.063(4) 0.001(3) 0.023(3) 0.005(4) C10 0.055(4) 0.053(4) 0.058(4) 0.002(3) 0.016(3) -0.001(3) C11 0.051(4) 0.040(3) 0.042(3) 0.009(3) 0.010(3) 0.007(3) C12 0.048(3) 0.038(3) 0.043(3) 0.005(3) 0.005(3) 0.001(3) C13 0.048(4) 0.047(3) 0.045(3) 0.008(3) 0.007(3) -0.005(3) C14 0.054(4) 0.038(3) 0.054(4) 0.007(3) 0.000(3) -0.010(3) C15 0.051(3) 0.036(3) 0.041(3) 0.003(2) -0.004(3) -0.004(3) C16 0.046(3) 0.040(3) 0.038(3) 0.006(2) 0.002(3) -0.003(3) C17 0.053(4) 0.043(3) 0.048(4) -0.015(3) -0.005(3) 0.012(3) C18 0.061(4) 0.047(4) 0.071(4) -0.021(3) 0.003(4) -0.003(3) C19 0.092(6) 0.071(5) 0.057(4) -0.001(4) 0.020(4) 0.025(4) C20 0.045(3) 0.043(3) 0.060(4) -0.002(3) 0.002(3) -0.006(3) C21 0.077(5) 0.063(4) 0.062(4) -0.001(3) 0.011(4) -0.001(4) C22 0.055(4) 0.046(4) 0.096(5) -0.023(4) 0.001(4) -0.007(3) C23 0.130(7) 0.063(5) 0.064(5) 0.014(4) 0.017(5) -0.005(5) C24 0.088(6) 0.109(7) 0.092(6) 0.009(5) -0.011(5) -0.030(5) C25 0.086(5) 0.084(5) 0.057(4) 0.003(4) -0.018(4) -0.011(4) C26 0.052(4) 0.031(3) 0.042(3) 0.004(2) 0.000(3) -0.007(3) C27 0.056(4) 0.041(3) 0.036(3) 0.000(2) -0.006(3) -0.002(3) C28 0.050(4) 0.035(3) 0.042(3) 0.004(2) 0.003(3) -0.006(2) C29 0.063(4) 0.035(3) 0.031(3) 0.002(2) 0.001(3) -0.008(3) C30 0.063(4) 0.036(3) 0.040(3) 0.003(3) -0.012(3) -0.013(3) C31 0.055(4) 0.032(3) 0.050(3) 0.004(3) -0.003(3) -0.010(3) C32 0.054(4) 0.070(4) 0.056(4) -0.022(3) -0.007(3) 0.013(3) C33 0.077(5) 0.051(4) 0.047(4) -0.014(3) -0.004(3) 0.008(3) C34 0.057(4) 0.052(4) 0.061(4) 0.002(3) -0.005(3) -0.005(3) P1 0.0616(13) 0.0594(12) 0.0565(10) 0.0027(9) -0.0064(9) -0.0114(9) F1A 0.073(13) 0.163(19) 0.17(2) 0.060(14) -0.002(12) -0.017(12) F2A 0.077(11) 0.123(18) 0.067(7) 0.007(8) 0.012(8) -0.052(9) F3A 0.091(8) 0.054(6) 0.085(10) 0.009(6) 0.019(6) 0.002(5) F4A 0.134(9) 0.112(15) 0.062(6) -0.002(8) -0.029(6) -0.036(9) F5A 0.162(12) 0.058(7) 0.120(16) 0.028(10) 0.008(11) -0.005(7) F6A 0.059(6) 0.122(15) 0.049(6) -0.015(9) -0.004(4) 0.003(8) F1B 0.034(8) 0.052(8) 0.055(7) -0.004(6) 0.001(5) -0.009(6) F2B 0.072(11) 0.092(15) 0.113(17) -0.020(13) 0.049(9) -0.037(11) F3B 0.25(3) 0.079(14) 0.083(15) -0.030(11) 0.058(17) -0.048(15) F4B 0.135(10) 0.108(18) 0.053(10) 0.021(10) -0.010(7) -0.017(10) F5B 0.115(13) 0.075(16) 0.16(2) -0.059(16) 0.041(14) -0.049(11) F6B 0.120(17) 0.20(3) 0.103(18) 0.068(19) 0.004(13) 0.066(19) O3 0.095(7) 0.054(5) 0.080(6) 0.011(5) -0.044(5) -0.020(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 Fe N2 1.879(4) . ? Fe N2 1.879(4) 4_755 ? Fe N1 1.975(4) 4_755 ? Fe N1 1.975(4) . ? Fe N3 1.988(4) . ? Fe N3 1.988(4) 4_755 ? O1 C20 1.418(7) . ? O1 C24 1.450(8) . ? O2 C29 1.372(6) . ? O2 C33 1.422(7) . ? N1 C2 1.344(7) . ? N1 C6 1.373(6) . ? N2 C11 1.354(7) . ? N2 C7 1.362(6) . ? N3 C16 1.334(6) . ? N3 C12 1.369(7) . ? C2 C3 1.398(7) . ? C2 H2 0.9500 . ? C3 C4 1.377(8) . ? C3 C17 1.464(8) . ? C4 C5 1.370(8) . ? C4 H4 0.9500 . ? C5 C6 1.390(7) . ? C5 H5 0.9500 . ? C6 C7 1.463(7) . ? C7 C8 1.372(7) . ? C8 C9 1.387(8) . ? C8 H8 0.9500 . ? C9 C10 1.391(8) . ? C9 H9 0.9500 . ? C10 C11 1.371(7) . ? C10 H10 0.9500 . ? C11 C12 1.453(7) . ? C12 C13 1.408(8) . ? C13 C14 1.369(8) . ? C13 H13 0.9500 . ? C14 C15 1.389(7) . ? C14 H14 0.9500 . ? C15 C16 1.402(7) . ? C15 C26 1.491(7) . ? C16 H16 0.9500 . ? C17 C18 1.368(8) . ? C17 C22 1.457(9) . ? C18 C19 1.437(9) . ? C18 C23 1.498(10) . ? C19 C20 1.405(9) . ? C19 H19 0.9500 . ? C20 C21 1.341(8) . ? C21 C22 1.343(9) . ? C21 H21 0.9500 . ? C22 C25 1.530(9) . ? C23 H231 0.9800 . ? C23 H232 0.9800 . ? C23 H233 0.9800 . ? C24 H241 0.9800 . ? C24 H242 0.9800 . ? C24 H243 0.9800 . ? C25 H251 0.9800 . ? C25 H252 0.9800 . ? C25 H253 0.9800 . ? C26 C27 1.407(8) . ? C26 C31 1.416(7) . ? C27 C28 1.401(7) . ? C27 C32 1.523(7) . ? C28 C29 1.375(8) . ? C28 H28 0.9500 . ? C29 C30 1.379(8) . ? C30 C31 1.386(8) . ? C30 H30 0.9500 . ? C31 C34 1.520(8) . ? C32 H321 0.9800 . ? C32 H322 0.9800 . ? C32 H323 0.9800 . ? C33 H331 0.9800 . ? C33 H332 0.9800 . ? C33 H333 0.9800 . ? C34 H341 0.9800 . ? C34 H342 0.9800 . ? C34 H343 0.9800 . ? P1 F1A 1.50(3) . ? P1 F2A 1.69(3) . ? P1 F3A 1.613(14) . ? P1 F4A 1.629(13) . ? P1 F5A 1.544(19) . ? P1 F6A 1.531(18) . ? P1 F1B 1.66(2) . ? P1 F2B 1.48(4) . ? P1 F3B 1.499(18) . ? P1 F4B 1.570(14) . ? P1 F5B 1.597(17) . ? P1 F6B 1.55(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 N2 Fe N2 179.4(3) . 4_755 ? N2 Fe N1 98.41(17) . 4_755 ? N2 Fe N1 81.16(18) 4_755 4_755 ? N2 Fe N1 81.16(18) . . ? N2 Fe N1 98.41(18) 4_755 . ? N1 Fe N1 85.9(2) 4_755 . ? N2 Fe N3 80.57(17) . . ? N2 Fe N3 99.86(16) 4_755 . ? N1 Fe N3 96.17(16) 4_755 . ? N1 Fe N3 161.72(17) . . ? N2 Fe N3 99.86(16) . 4_755 ? N2 Fe N3 80.57(17) 4_755 4_755 ? N1 Fe N3 161.72(17) 4_755 4_755 ? N1 Fe N3 96.16(16) . 4_755 ? N3 Fe N3 87.5(2) . 4_755 ? C20 O1 C24 114.1(5) . . ? C29 O2 C33 115.6(4) . . ? C2 N1 C6 118.3(4) . . ? C2 N1 Fe 127.5(3) . . ? C6 N1 Fe 114.0(3) . . ? C11 N2 C7 120.4(5) . . ? C11 N2 Fe 120.2(3) . . ? C7 N2 Fe 119.4(4) . . ? C16 N3 C12 118.2(4) . . ? C16 N3 Fe 128.1(4) . . ? C12 N3 Fe 113.4(3) . . ? N1 C2 C3 123.3(5) . . ? N1 C2 H2 118.3 . . ? C3 C2 H2 118.3 . . ? C4 C3 C2 117.6(5) . . ? C4 C3 C17 122.5(5) . . ? C2 C3 C17 119.8(5) . . ? C5 C4 C3 120.2(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.2(5) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? N1 C6 C5 120.4(5) . . ? N1 C6 C7 113.6(4) . . ? C5 C6 C7 126.0(5) . . ? N2 C7 C8 120.7(5) . . ? N2 C7 C6 111.2(4) . . ? C8 C7 C6 128.0(5) . . ? C7 C8 C9 119.2(6) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C8 C9 C10 119.7(6) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 119.3(6) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? N2 C11 C10 120.7(5) . . ? N2 C11 C12 110.7(5) . . ? C10 C11 C12 128.5(6) . . ? N3 C12 C13 120.5(5) . . ? N3 C12 C11 114.4(5) . . ? C13 C12 C11 125.1(5) . . ? C14 C13 C12 119.4(5) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 121.2(5) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 116.0(5) . . ? C14 C15 C26 122.9(5) . . ? C16 C15 C26 121.1(5) . . ? N3 C16 C15 124.7(5) . . ? N3 C16 H16 117.6 . . ? C15 C16 H16 117.6 . . ? C18 C17 C22 121.6(6) . . ? C18 C17 C3 120.9(5) . . ? C22 C17 C3 117.5(5) . . ? C17 C18 C19 118.2(6) . . ? C17 C18 C23 122.6(6) . . ? C19 C18 C23 119.2(7) . . ? C20 C19 C18 117.0(6) . . ? C20 C19 H19 121.5 . . ? C18 C19 H19 121.5 . . ? C21 C20 C19 123.9(6) . . ? C21 C20 O1 124.2(6) . . ? C19 C20 O1 111.8(6) . . ? C20 C21 C22 120.7(7) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C17 118.4(7) . . ? C21 C22 C25 118.9(6) . . ? C17 C22 C25 122.7(6) . . ? C18 C23 H231 109.5 . . ? C18 C23 H232 109.5 . . ? H231 C23 H232 109.5 . . ? C18 C23 H233 109.5 . . ? H231 C23 H233 109.5 . . ? H232 C23 H233 109.5 . . ? O1 C24 H241 109.5 . . ? O1 C24 H242 109.5 . . ? H241 C24 H242 109.5 . . ? O1 C24 H243 109.5 . . ? H241 C24 H243 109.5 . . ? H242 C24 H243 109.5 . . ? C22 C25 H251 109.5 . . ? C22 C25 H252 109.5 . . ? H251 C25 H252 109.5 . . ? C22 C25 H253 109.5 . . ? H251 C25 H253 109.5 . . ? H252 C25 H253 109.5 . . ? C27 C26 C31 118.9(5) . . ? C27 C26 C15 120.4(5) . . ? C31 C26 C15 120.7(5) . . ? C28 C27 C26 120.2(5) . . ? C28 C27 C32 116.2(5) . . ? C26 C27 C32 123.5(5) . . ? C29 C28 C27 119.9(5) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? O2 C29 C28 123.7(5) . . ? O2 C29 C30 115.8(5) . . ? C28 C29 C30 120.5(5) . . ? C29 C30 C31 121.2(5) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C30 C31 C26 119.3(5) . . ? C30 C31 C34 117.9(5) . . ? C26 C31 C34 122.8(5) . . ? C27 C32 H321 109.5 . . ? C27 C32 H322 109.5 . . ? H321 C32 H322 109.5 . . ? C27 C32 H323 109.5 . . ? H321 C32 H323 109.5 . . ? H322 C32 H323 109.5 . . ? O2 C33 H331 109.5 . . ? O2 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? O2 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C31 C34 H341 109.5 . . ? C31 C34 H342 109.5 . . ? H341 C34 H342 109.5 . . ? C31 C34 H343 109.5 . . ? H341 C34 H343 109.5 . . ? H342 C34 H343 109.5 . . ? F2B P1 F3B 91.7(19) . . ? F1A P1 F6A 96.4(13) . . ? F1A P1 F5A 91.9(13) . . ? F6A P1 F5A 93.3(8) . . ? F2B P1 F6B 90.8(19) . . ? F3B P1 F6B 93.0(11) . . ? F2B P1 F4B 95.3(18) . . ? F3B P1 F4B 90.2(10) . . ? F6B P1 F4B 173.0(12) . . ? F2B P1 F5B 94.9(16) . . ? F3B P1 F5B 173.2(16) . . ? F6B P1 F5B 88.9(11) . . ? F4B P1 F5B 87.2(9) . . ? F1A P1 F3A 90.4(12) . . ? F6A P1 F3A 91.4(7) . . ? F5A P1 F3A 174.6(7) . . ? F1A P1 F4A 89.5(12) . . ? F6A P1 F4A 174.0(10) . . ? F5A P1 F4A 87.8(7) . . ? F3A P1 F4A 87.3(7) . . ? F2B P1 F1B 173.7(19) . . ? F3B P1 F1B 86.0(14) . . ? F6B P1 F1B 83.5(14) . . ? F4B P1 F1B 90.6(9) . . ? F5B P1 F1B 87.7(8) . . ? F1A P1 F2A 173.4(16) . . ? F6A P1 F2A 89.7(11) . . ? F5A P1 F2A 85.2(15) . . ? F3A P1 F2A 92.0(14) . . ? F4A P1 F2A 84.5(11) . . ? 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 N2 Fe N1 C2 -178.9(4) . . . . ? N2 Fe N1 C2 1.5(4) 4_755 . . . ? N1 Fe N1 C2 81.9(4) 4_755 . . . ? N3 Fe N1 C2 179.3(5) . . . . ? N3 Fe N1 C2 -79.8(4) 4_755 . . . ? N2 Fe N1 C6 7.2(3) . . . . ? N2 Fe N1 C6 -172.4(3) 4_755 . . . ? N1 Fe N1 C6 -91.9(4) 4_755 . . . ? N3 Fe N1 C6 5.4(7) . . . . ? N3 Fe N1 C6 106.3(3) 4_755 . . . ? N2 Fe N2 C11 -141.9(3) 4_755 . . . ? N1 Fe N2 C11 -99.2(4) 4_755 . . . ? N1 Fe N2 C11 176.3(4) . . . . ? N3 Fe N2 C11 -4.3(4) . . . . ? N3 Fe N2 C11 81.5(4) 4_755 . . . ? N2 Fe N2 C7 37.2(5) 4_755 . . . ? N1 Fe N2 C7 79.9(4) 4_755 . . . ? N1 Fe N2 C7 -4.6(4) . . . . ? N3 Fe N2 C7 174.8(4) . . . . ? N3 Fe N2 C7 -99.4(4) 4_755 . . . ? N2 Fe N3 C16 -179.7(4) . . . . ? N2 Fe N3 C16 -0.1(4) 4_755 . . . ? N1 Fe N3 C16 -82.2(4) 4_755 . . . ? N1 Fe N3 C16 -177.9(5) . . . . ? N3 Fe N3 C16 79.9(4) 4_755 . . . ? N2 Fe N3 C12 6.9(3) . . . . ? N2 Fe N3 C12 -173.5(3) 4_755 . . . ? N1 Fe N3 C12 104.4(4) 4_755 . . . ? N1 Fe N3 C12 8.7(7) . . . . ? N3 Fe N3 C12 -93.5(4) 4_755 . . . ? C6 N1 C2 C3 1.7(7) . . . . ? Fe N1 C2 C3 -171.9(4) . . . . ? N1 C2 C3 C4 0.1(8) . . . . ? N1 C2 C3 C17 -177.4(5) . . . . ? C2 C3 C4 C5 -0.5(8) . . . . ? C17 C3 C4 C5 177.0(5) . . . . ? C3 C4 C5 C6 -0.9(8) . . . . ? C2 N1 C6 C5 -3.2(7) . . . . ? Fe N1 C6 C5 171.3(4) . . . . ? C2 N1 C6 C7 177.0(4) . . . . ? Fe N1 C6 C7 -8.5(5) . . . . ? C4 C5 C6 N1 2.8(8) . . . . ? C4 C5 C6 C7 -177.3(5) . . . . ? C11 N2 C7 C8 -0.8(7) . . . . ? Fe N2 C7 C8 -179.9(4) . . . . ? C11 N2 C7 C6 -179.7(4) . . . . ? Fe N2 C7 C6 1.3(5) . . . . ? N1 C6 C7 N2 4.9(6) . . . . ? C5 C6 C7 N2 -175.0(5) . . . . ? N1 C6 C7 C8 -173.9(5) . . . . ? C5 C6 C7 C8 6.2(9) . . . . ? N2 C7 C8 C9 -0.7(8) . . . . ? C6 C7 C8 C9 178.0(5) . . . . ? C7 C8 C9 C10 1.2(9) . . . . ? C8 C9 C10 C11 -0.2(9) . . . . ? C7 N2 C11 C10 1.8(8) . . . . ? Fe N2 C11 C10 -179.2(4) . . . . ? C7 N2 C11 C12 -178.2(4) . . . . ? Fe N2 C11 C12 0.9(6) . . . . ? C9 C10 C11 N2 -1.3(9) . . . . ? C9 C10 C11 C12 178.7(6) . . . . ? C16 N3 C12 C13 -2.7(7) . . . . ? Fe N3 C12 C13 171.4(4) . . . . ? C16 N3 C12 C11 177.5(4) . . . . ? Fe N3 C12 C11 -8.4(6) . . . . ? N2 C11 C12 N3 5.1(6) . . . . ? C10 C11 C12 N3 -174.9(5) . . . . ? N2 C11 C12 C13 -174.7(5) . . . . ? C10 C11 C12 C13 5.4(9) . . . . ? N3 C12 C13 C14 1.0(8) . . . . ? C11 C12 C13 C14 -179.2(5) . . . . ? C12 C13 C14 C15 1.6(8) . . . . ? C13 C14 C15 C16 -2.4(8) . . . . ? C13 C14 C15 C26 179.7(5) . . . . ? C12 N3 C16 C15 1.9(8) . . . . ? Fe N3 C16 C15 -171.2(4) . . . . ? C14 C15 C16 N3 0.6(8) . . . . ? C26 C15 C16 N3 178.6(5) . . . . ? C4 C3 C17 C18 120.1(6) . . . . ? C2 C3 C17 C18 -62.4(7) . . . . ? C4 C3 C17 C22 -59.9(7) . . . . ? C2 C3 C17 C22 117.5(6) . . . . ? C22 C17 C18 C19 -1.7(9) . . . . ? C3 C17 C18 C19 178.3(5) . . . . ? C22 C17 C18 C23 177.8(6) . . . . ? C3 C17 C18 C23 -2.2(9) . . . . ? C17 C18 C19 C20 2.3(9) . . . . ? C23 C18 C19 C20 -177.2(6) . . . . ? C18 C19 C20 C21 -2.4(9) . . . . ? C18 C19 C20 O1 -179.5(5) . . . . ? C24 O1 C20 C21 2.3(9) . . . . ? C24 O1 C20 C19 179.4(6) . . . . ? C19 C20 C21 C22 1.7(10) . . . . ? O1 C20 C21 C22 178.5(6) . . . . ? C20 C21 C22 C17 -0.9(9) . . . . ? C20 C21 C22 C25 177.3(6) . . . . ? C18 C17 C22 C21 1.0(9) . . . . ? C3 C17 C22 C21 -179.0(5) . . . . ? C18 C17 C22 C25 -177.1(6) . . . . ? C3 C17 C22 C25 2.9(8) . . . . ? C14 C15 C26 C27 126.5(6) . . . . ? C16 C15 C26 C27 -51.3(7) . . . . ? C14 C15 C26 C31 -51.2(7) . . . . ? C16 C15 C26 C31 131.0(5) . . . . ? C31 C26 C27 C28 1.3(8) . . . . ? C15 C26 C27 C28 -176.4(5) . . . . ? C31 C26 C27 C32 -179.9(5) . . . . ? C15 C26 C27 C32 2.4(8) . . . . ? C26 C27 C28 C29 0.1(8) . . . . ? C32 C27 C28 C29 -178.8(5) . . . . ? C33 O2 C29 C28 -6.9(7) . . . . ? C33 O2 C29 C30 172.9(5) . . . . ? C27 C28 C29 O2 178.1(5) . . . . ? C27 C28 C29 C30 -1.7(8) . . . . ? O2 C29 C30 C31 -177.9(5) . . . . ? C28 C29 C30 C31 1.9(8) . . . . ? C29 C30 C31 C26 -0.5(8) . . . . ? C29 C30 C31 C34 -178.8(5) . . . . ? C27 C26 C31 C30 -1.1(7) . . . . ? C15 C26 C31 C30 176.6(5) . . . . ? C27 C26 C31 C34 177.1(5) . . . . ? C15 C26 C31 C34 -5.2(8) . . . . ? data_SG0305 _database_code_depnum_ccdc_archive 'CCDC 274363' _audit_creation_method SHELXL-97 _audit_creation_date 03-02-26 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C66 H62 N6 O4 Ru 2+,2(P F6 1-), H2 O' _chemical_formula_sum 'C66 H64 F12 N6 O5 P2 Ru' _chemical_formula_weight 1412.20 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 264 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 256 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; F F 48 0.0171 0.0103 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 24 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 20 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 8 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Ru Ru 4 -1.2594 0.8363 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 23.1733(3) _cell_length_b 11.96030(10) _cell_length_c 22.8083(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6321.54(13) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 63075 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description tablet _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 0.390 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 0.975 _exptl_special_details ; Solvent used: dichloromethane / benzene Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.505(1) Frames collected: 360 Seconds exposure per frame: 96 Degrees rotation per frame: 1.6 Crystal-Detector distance (mm): 35.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 101070 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 5577 _reflns_number_gt 3965 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2002)' _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 'w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+9.8096P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5577 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1664 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.308 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.081 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 1.0000 0.18124(4) 0.2500 0.0460(2) Uani 1 2 d S . . O1 O 0.7041(2) -0.3224(4) 0.1826(3) 0.1080(16) Uani 1 1 d . . . O2 O 1.01549(17) 0.7242(3) 0.54499(15) 0.0677(10) Uani 1 1 d . . . N1 N 0.97449(17) 0.0546(3) 0.19430(14) 0.0483(9) Uani 1 1 d . . . N2 N 1.06489(17) 0.1797(3) 0.19406(15) 0.0515(9) Uani 1 1 d . . . N3 N 1.05123(17) 0.3072(3) 0.28400(15) 0.0505(9) Uani 1 1 d . . . C2 C 0.9270(2) -0.0074(4) 0.19771(18) 0.0518(11) Uani 1 1 d . . . H2 H 0.8987 0.0132 0.2259 0.062 Uiso 1 1 calc R . . C3 C 0.9157(2) -0.1013(4) 0.16239(18) 0.0544(12) Uani 1 1 d . . . C4 C 0.9583(2) -0.1307(4) 0.1232(2) 0.0622(13) Uani 1 1 d . . . H4 H 0.9534 -0.1950 0.0993 0.075 Uiso 1 1 calc R . . C5 C 1.0073(2) -0.0683(5) 0.1185(2) 0.0649(14) Uani 1 1 d . . . H5 H 1.0361 -0.0891 0.0910 0.078 Uiso 1 1 calc R . . C6 C 1.0156(2) 0.0254(4) 0.15364(18) 0.0548(12) Uani 1 1 d . . . C7 C 1.0658(2) 0.0993(4) 0.15167(19) 0.0566(12) Uani 1 1 d . . . C8 C 1.1112(2) 0.0967(6) 0.1120(2) 0.0763(16) Uani 1 1 d . . . H8 H 1.1121 0.0423 0.0817 0.092 Uiso 1 1 calc R . . C9 C 1.1550(3) 0.1740(6) 0.1173(3) 0.0847(19) Uani 1 1 d . . . H9 H 1.1863 0.1721 0.0905 0.102 Uiso 1 1 calc R . . C10 C 1.1543(2) 0.2540(5) 0.1606(2) 0.0752(16) Uani 1 1 d . . . H10 H 1.1847 0.3068 0.1641 0.090 Uiso 1 1 calc R . . C11 C 1.1076(2) 0.2555(4) 0.1992(2) 0.0611(13) Uani 1 1 d . . . C12 C 1.0987(2) 0.3305(4) 0.24947(19) 0.0576(12) Uani 1 1 d . . . C13 C 1.1332(3) 0.4233(5) 0.2630(2) 0.0697(15) Uani 1 1 d . . . H13 H 1.1655 0.4410 0.2391 0.084 Uiso 1 1 calc R . . C14 C 1.1203(2) 0.4894(4) 0.3110(2) 0.0696(14) Uani 1 1 d . . . H14 H 1.1435 0.5528 0.3195 0.083 Uiso 1 1 calc R . . C15 C 1.0736(2) 0.4639(4) 0.3469(2) 0.0551(12) Uani 1 1 d . . . C16 C 1.0406(2) 0.3717(4) 0.33093(19) 0.0529(11) Uani 1 1 d . . . H16 H 1.0083 0.3531 0.3548 0.063 Uiso 1 1 calc R . . C17 C 0.8608(2) -0.1614(4) 0.1678(2) 0.0551(12) Uani 1 1 d . . . C18 C 0.8460(2) -0.2124(4) 0.2204(2) 0.0671(14) Uani 1 1 d . . . C19 C 0.7913(3) -0.2652(5) 0.2234(3) 0.0861(18) Uani 1 1 d . . . H19 H 0.7785 -0.2990 0.2588 0.103 Uiso 1 1 calc R . . C20 C 0.7557(2) -0.2669(4) 0.1724(2) 0.0662(13) Uani 1 1 d . . . C21 C 0.7733(3) -0.2185(5) 0.1219(3) 0.0746(15) Uani 1 1 d . . . H21 H 0.7488 -0.2216 0.0886 0.089 Uiso 1 1 calc R . . C22 C 0.8247(2) -0.1659(4) 0.1174(3) 0.0662(14) Uani 1 1 d . . . C23 C 0.8866(3) -0.2127(6) 0.2737(3) 0.094(2) Uani 1 1 d . . . H231 H 0.9259 -0.2306 0.2609 0.141 Uiso 1 1 calc R . . H232 H 0.8735 -0.2690 0.3020 0.141 Uiso 1 1 calc R . . H233 H 0.8862 -0.1388 0.2923 0.141 Uiso 1 1 calc R . . C24 C 0.6669(4) -0.3249(7) 0.1293(4) 0.125(3) Uani 1 1 d . . . H241 H 0.6587 -0.2482 0.1166 0.188 Uiso 1 1 calc R . . H242 H 0.6306 -0.3631 0.1384 0.188 Uiso 1 1 calc R . . H243 H 0.6869 -0.3650 0.0978 0.188 Uiso 1 1 calc R . . C25 C 0.8403(3) -0.1148(5) 0.0596(2) 0.0807(17) Uani 1 1 d . . . H251 H 0.8605 -0.1702 0.0355 0.121 Uiso 1 1 calc R . . H252 H 0.8656 -0.0502 0.0660 0.121 Uiso 1 1 calc R . . H253 H 0.8051 -0.0905 0.0394 0.121 Uiso 1 1 calc R . . C26 C 1.0570(2) 0.5314(4) 0.3993(2) 0.0578(12) Uani 1 1 d . . . C27 C 1.0004(2) 0.5713(4) 0.4054(2) 0.0566(12) Uani 1 1 d . . . C28 C 0.9854(2) 0.6350(4) 0.4542(2) 0.0584(13) Uani 1 1 d . . . H28 H 0.9470 0.6617 0.4587 0.070 Uiso 1 1 calc R . . C29 C 1.0266(3) 0.6590(4) 0.4962(2) 0.0591(13) Uani 1 1 d . . . C30 C 1.0824(2) 0.6190(4) 0.4909(2) 0.0613(13) Uani 1 1 d . . . H30 H 1.1099 0.6354 0.5205 0.074 Uiso 1 1 calc R . . C31 C 1.0987(2) 0.5558(4) 0.4431(2) 0.0585(12) Uani 1 1 d . . . C32 C 0.9525(3) 0.5496(5) 0.3614(2) 0.0758(16) Uani 1 1 d . . . H321 H 0.9684 0.5516 0.3216 0.114 Uiso 1 1 calc R . . H322 H 0.9227 0.6073 0.3654 0.114 Uiso 1 1 calc R . . H323 H 0.9355 0.4759 0.3689 0.114 Uiso 1 1 calc R . . C33 C 0.9600(3) 0.7765(5) 0.5470(2) 0.0767(16) Uani 1 1 d . . . H331 H 0.9564 0.8292 0.5143 0.115 Uiso 1 1 calc R . . H332 H 0.9558 0.8167 0.5842 0.115 Uiso 1 1 calc R . . H333 H 0.9299 0.7193 0.5439 0.115 Uiso 1 1 calc R . . C34 C 1.1597(2) 0.5137(5) 0.4406(3) 0.0774(16) Uani 1 1 d . . . H341 H 1.1830 0.5643 0.4165 0.116 Uiso 1 1 calc R . . H342 H 1.1602 0.4387 0.4234 0.116 Uiso 1 1 calc R . . H343 H 1.1757 0.5109 0.4804 0.116 Uiso 1 1 calc R . . P1 P 0.80919(7) 0.80699(13) 0.44412(8) 0.0772(5) Uani 1 1 d . . . F1A F 0.8726(6) 0.8199(10) 0.4238(6) 0.085(5) Uani 0.448(16) 1 d P A 1 F2A F 0.7433(7) 0.7902(14) 0.4714(6) 0.095(5) Uani 0.448(16) 1 d P A 1 F3A F 0.7955(6) 0.9406(9) 0.4524(7) 0.108(5) Uani 0.448(16) 1 d P A 1 F4A F 0.8258(5) 0.8074(18) 0.5157(5) 0.134(6) Uani 0.448(16) 1 d P A 1 F5A F 0.8114(8) 0.6830(8) 0.4447(9) 0.159(7) Uani 0.448(16) 1 d P A 1 F6A F 0.7823(4) 0.8148(19) 0.3852(5) 0.103(6) Uani 0.448(16) 1 d P A 1 F1B F 0.8709(6) 0.7998(17) 0.4156(7) 0.172(9) Uani 0.552(16) 1 d P A 2 F2B F 0.7494(8) 0.818(2) 0.4644(9) 0.201(9) Uani 0.552(16) 1 d P A 2 F3B F 0.8344(9) 0.9028(9) 0.4799(4) 0.142(6) Uani 0.552(16) 1 d P A 2 F4B F 0.8298(4) 0.7232(9) 0.4919(5) 0.110(4) Uani 0.552(16) 1 d P A 2 F5B F 0.7955(4) 0.7044(12) 0.3999(6) 0.118(5) Uani 0.552(16) 1 d P A 2 F6B F 0.7967(8) 0.8859(15) 0.3884(7) 0.158(6) Uani 0.552(16) 1 d P A 2 O3 O 0.7115(9) 0.0207(9) 0.3497(8) 0.263(12) Uani 0.50 1 d P . . 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 0.0654(4) 0.0430(3) 0.0297(3) 0.000 0.0126(2) 0.000 O1 0.099(3) 0.090(3) 0.135(4) -0.009(3) 0.031(3) -0.021(3) O2 0.095(3) 0.059(2) 0.048(2) -0.0030(16) -0.0040(18) -0.0165(19) N1 0.066(2) 0.047(2) 0.0316(18) 0.0001(15) 0.0009(17) 0.0109(19) N2 0.066(2) 0.054(2) 0.034(2) 0.0088(16) 0.0100(17) 0.0082(19) N3 0.068(2) 0.048(2) 0.037(2) 0.0081(16) 0.0127(17) -0.0066(17) C2 0.068(3) 0.053(3) 0.035(2) -0.0079(19) -0.001(2) 0.013(2) C3 0.078(3) 0.053(3) 0.033(2) -0.0079(19) -0.013(2) 0.020(2) C4 0.078(3) 0.066(3) 0.043(3) -0.019(2) -0.009(2) 0.025(3) C5 0.082(4) 0.078(3) 0.035(2) -0.013(2) 0.000(2) 0.031(3) C6 0.068(3) 0.067(3) 0.029(2) -0.003(2) 0.003(2) 0.023(2) C7 0.068(3) 0.067(3) 0.034(2) 0.005(2) 0.010(2) 0.019(2) C8 0.074(4) 0.112(5) 0.043(3) -0.008(3) 0.014(3) 0.021(4) C9 0.080(4) 0.124(5) 0.050(3) -0.003(3) 0.027(3) 0.001(4) C10 0.070(3) 0.099(4) 0.057(3) 0.011(3) 0.020(3) -0.006(3) C11 0.074(3) 0.069(3) 0.040(3) 0.011(2) 0.015(2) 0.007(3) C12 0.072(3) 0.057(3) 0.043(3) 0.015(2) 0.016(2) -0.005(2) C13 0.079(4) 0.072(3) 0.059(3) 0.017(3) 0.021(3) -0.017(3) C14 0.089(4) 0.058(3) 0.062(3) 0.014(3) 0.005(3) -0.026(3) C15 0.078(3) 0.042(2) 0.045(3) 0.007(2) 0.003(2) -0.011(2) C16 0.071(3) 0.044(2) 0.043(2) 0.006(2) 0.009(2) -0.008(2) C17 0.071(3) 0.050(2) 0.045(3) -0.016(2) -0.011(2) 0.016(2) C18 0.079(4) 0.057(3) 0.065(4) -0.023(3) 0.003(3) 0.007(3) C19 0.116(5) 0.062(3) 0.081(4) -0.009(3) 0.033(4) 0.011(3) C20 0.068(3) 0.061(3) 0.070(3) -0.012(3) 0.002(3) -0.002(3) C21 0.089(4) 0.065(3) 0.070(4) 0.001(3) 0.002(3) 0.001(3) C22 0.073(4) 0.053(3) 0.073(4) -0.008(2) -0.008(3) 0.002(3) C23 0.142(6) 0.079(4) 0.061(4) 0.012(3) -0.011(4) -0.002(4) C24 0.116(6) 0.140(7) 0.119(7) 0.002(5) -0.005(5) -0.059(5) C25 0.100(4) 0.085(4) 0.057(3) 0.003(3) -0.022(3) -0.001(3) C26 0.083(4) 0.039(2) 0.051(3) 0.008(2) 0.004(2) -0.017(2) C27 0.085(4) 0.041(2) 0.044(3) 0.0062(19) -0.007(2) -0.014(2) C28 0.086(4) 0.040(2) 0.049(3) 0.006(2) -0.001(2) -0.017(2) C29 0.099(4) 0.039(2) 0.039(3) 0.0053(19) -0.002(3) -0.020(3) C30 0.078(4) 0.048(3) 0.058(3) 0.007(2) -0.003(3) -0.023(3) C31 0.077(3) 0.043(2) 0.055(3) 0.005(2) 0.001(2) -0.022(2) C32 0.097(4) 0.071(3) 0.059(3) -0.016(3) -0.015(3) 0.013(3) C33 0.118(5) 0.061(3) 0.051(3) -0.001(3) -0.007(3) -0.008(3) C34 0.084(4) 0.067(3) 0.082(4) 0.000(3) -0.006(3) -0.024(3) P1 0.0772(11) 0.0781(10) 0.0763(11) -0.0109(8) -0.0030(8) -0.0185(8) F1A 0.064(7) 0.092(6) 0.098(9) 0.058(6) -0.039(6) -0.046(5) F2A 0.095(8) 0.121(8) 0.071(6) -0.032(5) 0.035(5) -0.073(7) F3A 0.122(9) 0.081(6) 0.121(11) -0.019(6) 0.041(7) -0.004(6) F4A 0.132(9) 0.188(17) 0.083(7) 0.010(9) -0.015(6) -0.034(9) F5A 0.244(17) 0.054(6) 0.178(19) -0.006(8) 0.017(16) -0.021(7) F6A 0.050(5) 0.203(18) 0.056(5) -0.007(9) -0.001(3) 0.020(8) F1B 0.061(7) 0.35(2) 0.105(8) -0.075(10) 0.010(6) -0.036(8) F2B 0.134(12) 0.25(2) 0.215(16) 0.005(13) 0.078(11) 0.063(12) F3B 0.269(17) 0.083(6) 0.075(6) -0.025(5) 0.014(7) -0.067(8) F4B 0.149(7) 0.088(7) 0.094(8) 0.027(6) 0.006(5) -0.038(5) F5B 0.082(6) 0.164(11) 0.109(8) -0.072(8) 0.009(5) -0.051(6) F6B 0.204(15) 0.164(12) 0.106(8) 0.017(9) -0.004(9) 0.046(10) O3 0.43(3) 0.074(7) 0.285(18) -0.019(9) -0.30(2) 0.018(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 Ru N2 1.972(4) . ? Ru N1 2.064(4) . ? Ru N3 2.069(4) . ? O1 C20 1.387(7) . ? O1 C24 1.493(9) . ? O2 C29 1.383(6) . ? O2 C33 1.430(7) . ? N1 C2 1.330(6) . ? N1 C6 1.374(6) . ? N2 C11 1.348(6) . ? N2 C7 1.363(6) . ? N3 C16 1.342(6) . ? N3 C12 1.382(6) . ? C2 C3 1.407(6) . ? C2 H2 0.9500 . ? C3 C4 1.376(7) . ? C3 C17 1.467(7) . ? C4 C5 1.364(8) . ? C4 H4 0.9500 . ? C5 C6 1.391(7) . ? C5 H5 0.9500 . ? C6 C7 1.463(7) . ? C7 C8 1.387(7) . ? C8 C9 1.378(8) . ? C8 H8 0.9500 . ? C9 C10 1.375(8) . ? C9 H9 0.9500 . ? C10 C11 1.395(7) . ? C10 H10 0.9500 . ? C11 C12 1.469(7) . ? C12 C13 1.402(7) . ? C13 C14 1.383(8) . ? C13 H13 0.9500 . ? C14 C15 1.390(7) . ? C14 H14 0.9500 . ? C15 C16 1.392(6) . ? C15 C26 1.494(6) . ? C16 H16 0.9500 . ? C17 C18 1.389(7) . ? C17 C22 1.423(7) . ? C18 C19 1.418(8) . ? C18 C23 1.537(8) . ? C19 C20 1.426(9) . ? C19 H19 0.9500 . ? C20 C21 1.351(8) . ? C21 C22 1.349(8) . ? C21 H21 0.9500 . ? C22 C25 1.499(8) . ? C23 H231 0.9800 . ? C23 H232 0.9800 . ? C23 H233 0.9800 . ? C24 H241 0.9800 . ? C24 H242 0.9800 . ? C24 H243 0.9800 . ? C25 H251 0.9800 . ? C25 H252 0.9800 . ? C25 H253 0.9800 . ? C26 C27 1.402(7) . ? C26 C31 1.419(7) . ? C27 C28 1.393(7) . ? C27 C32 1.518(7) . ? C28 C29 1.382(7) . ? C28 H28 0.9500 . ? C29 C30 1.386(8) . ? C30 C31 1.380(7) . ? C30 H30 0.9500 . ? C31 C34 1.502(7) . ? C32 H321 0.9800 . ? C32 H322 0.9800 . ? C32 H323 0.9800 . ? C33 H331 0.9800 . ? C33 H332 0.9800 . ? C33 H333 0.9800 . ? C34 H341 0.9800 . ? C34 H342 0.9800 . ? C34 H343 0.9800 . ? P1 F1A 1.549(13) . ? P1 F2A 1.662(14) . ? P1 F3A 1.640(10) . ? P1 F4A 1.678(11) . ? P1 F5A 1.484(10) . ? P1 F6A 1.483(11) . ? P1 F1B 1.574(14) . ? P1 F2B 1.466(17) . ? P1 F3B 1.523(8) . ? P1 F4B 1.555(8) . ? P1 F5B 1.620(8) . ? P1 F6B 1.609(15) . ? 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 N2 Ru N2 178.9(2) . 4_755 ? N2 Ru N1 99.96(15) . 4_755 ? N2 Ru N1 79.22(16) . . ? N1 Ru N1 85.53(19) . 4_755 ? N2 Ru N3 79.17(15) . . ? N1 Ru N3 158.39(15) . . ? N2 Ru N3 101.65(14) . 4_755 ? N1 Ru N3 98.03(14) . 4_755 ? N3 Ru N3 86.5(2) . 4_755 ? C20 O1 C24 111.8(5) . . ? C29 O2 C33 116.0(4) . . ? C2 N1 C6 118.2(4) . . ? C2 N1 Ru 127.6(3) . . ? C6 N1 Ru 113.8(3) . . ? C11 N2 C7 121.7(4) . . ? C11 N2 Ru 119.8(3) . . ? C7 N2 Ru 118.5(3) . . ? C16 N3 C12 119.1(4) . . ? C16 N3 Ru 127.7(3) . . ? C12 N3 Ru 113.0(3) . . ? N1 C2 C3 124.4(4) . . ? N1 C2 H2 117.8 . . ? C3 C2 H2 117.8 . . ? C4 C3 C2 116.3(5) . . ? C4 C3 C17 123.4(4) . . ? C2 C3 C17 120.2(4) . . ? C5 C4 C3 120.5(5) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.8(5) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? N1 C6 C5 119.8(5) . . ? N1 C6 C7 114.8(4) . . ? C5 C6 C7 125.4(4) . . ? N2 C7 C8 119.4(5) . . ? N2 C7 C6 113.0(4) . . ? C8 C7 C6 127.5(5) . . ? C9 C8 C7 119.0(5) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C10 C9 C8 121.4(5) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 118.1(6) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? N2 C11 C10 120.4(5) . . ? N2 C11 C12 112.1(4) . . ? C10 C11 C12 127.5(5) . . ? N3 C12 C13 119.2(4) . . ? N3 C12 C11 115.7(4) . . ? C13 C12 C11 125.1(5) . . ? C14 C13 C12 120.2(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.7(5) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 116.6(4) . . ? C14 C15 C26 123.7(4) . . ? C16 C15 C26 119.7(4) . . ? N3 C16 C15 124.2(4) . . ? N3 C16 H16 117.9 . . ? C15 C16 H16 117.9 . . ? C18 C17 C22 122.4(5) . . ? C18 C17 C3 120.2(4) . . ? C22 C17 C3 117.4(5) . . ? C17 C18 C19 117.3(5) . . ? C17 C18 C23 122.2(5) . . ? C19 C18 C23 120.5(6) . . ? C18 C19 C20 118.9(6) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C21 C20 O1 127.5(6) . . ? C21 C20 C19 121.0(5) . . ? O1 C20 C19 111.5(5) . . ? C22 C21 C20 122.0(6) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C17 118.4(6) . . ? C21 C22 C25 118.0(5) . . ? C17 C22 C25 123.6(5) . . ? C18 C23 H231 109.5 . . ? C18 C23 H232 109.5 . . ? H231 C23 H232 109.5 . . ? C18 C23 H233 109.5 . . ? H231 C23 H233 109.5 . . ? H232 C23 H233 109.5 . . ? O1 C24 H241 109.5 . . ? O1 C24 H242 109.5 . . ? H241 C24 H242 109.5 . . ? O1 C24 H243 109.5 . . ? H241 C24 H243 109.5 . . ? H242 C24 H243 109.5 . . ? C22 C25 H251 109.5 . . ? C22 C25 H252 109.5 . . ? H251 C25 H252 109.5 . . ? C22 C25 H253 109.5 . . ? H251 C25 H253 109.5 . . ? H252 C25 H253 109.5 . . ? C27 C26 C31 119.9(5) . . ? C27 C26 C15 120.3(4) . . ? C31 C26 C15 119.8(5) . . ? C28 C27 C26 119.9(5) . . ? C28 C27 C32 116.0(5) . . ? C26 C27 C32 124.1(4) . . ? C29 C28 C27 119.7(5) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 O2 123.1(5) . . ? C28 C29 C30 120.9(5) . . ? O2 C29 C30 116.0(5) . . ? C31 C30 C29 120.9(5) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C26 118.8(5) . . ? C30 C31 C34 118.0(5) . . ? C26 C31 C34 123.1(5) . . ? C27 C32 H321 109.5 . . ? C27 C32 H322 109.5 . . ? H321 C32 H322 109.5 . . ? C27 C32 H323 109.5 . . ? H321 C32 H323 109.5 . . ? H322 C32 H323 109.5 . . ? O2 C33 H331 109.5 . . ? O2 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? O2 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C31 C34 H341 109.5 . . ? C31 C34 H342 109.5 . . ? H341 C34 H342 109.5 . . ? C31 C34 H343 109.5 . . ? H341 C34 H343 109.5 . . ? H342 C34 H343 109.5 . . ? F6A P1 F5A 94.9(9) . . ? F2B P1 F3B 97.1(10) . . ? F6A P1 F1A 97.0(6) . . ? F5A P1 F1A 94.0(8) . . ? F2B P1 F4B 97.3(10) . . ? F3B P1 F4B 89.5(6) . . ? F2B P1 F1B 173.7(11) . . ? F3B P1 F1B 85.0(8) . . ? F4B P1 F1B 88.6(8) . . ? F2B P1 F6B 91.5(11) . . ? F3B P1 F6B 92.9(7) . . ? F4B P1 F6B 170.5(7) . . ? F1B P1 F6B 82.5(9) . . ? F2B P1 F5B 94.7(9) . . ? F3B P1 F5B 168.1(8) . . ? F4B P1 F5B 90.5(7) . . ? F1B P1 F5B 83.1(8) . . ? F6B P1 F5B 85.3(7) . . ? F6A P1 F3A 87.8(9) . . ? F5A P1 F3A 168.3(7) . . ? F1A P1 F3A 96.9(6) . . ? F6A P1 F2A 87.8(7) . . ? F5A P1 F2A 84.7(9) . . ? F1A P1 F2A 175.2(7) . . ? F3A P1 F2A 84.1(7) . . ? F6A P1 F4A 167.8(6) . . ? F5A P1 F4A 89.3(10) . . ? F1A P1 F4A 94.2(6) . . ? F3A P1 F4A 85.9(7) . . ? F2A P1 F4A 81.1(6) . . ? 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 N2 Ru N1 C2 179.3(4) . . . . ? N2 Ru N1 C2 0.1(4) 4_755 . . . ? N1 Ru N1 C2 78.3(4) 4_755 . . . ? N3 Ru N1 C2 178.8(4) . . . . ? N3 Ru N1 C2 -80.3(4) 4_755 . . . ? N2 Ru N1 C6 7.1(3) . . . . ? N2 Ru N1 C6 -172.1(3) 4_755 . . . ? N1 Ru N1 C6 -93.9(3) 4_755 . . . ? N3 Ru N1 C6 6.6(5) . . . . ? N3 Ru N1 C6 107.5(3) 4_755 . . . ? N2 Ru N2 C11 -141.4(3) 4_755 . . . ? N1 Ru N2 C11 -99.7(3) 4_755 . . . ? N1 Ru N2 C11 176.8(4) . . . . ? N3 Ru N2 C11 -3.3(3) . . . . ? N3 Ru N2 C11 80.8(4) 4_755 . . . ? N2 Ru N2 C7 37.1(3) 4_755 . . . ? N1 Ru N2 C7 78.8(3) 4_755 . . . ? N1 Ru N2 C7 -4.6(3) . . . . ? N3 Ru N2 C7 175.2(3) . . . . ? N3 Ru N2 C7 -100.7(3) 4_755 . . . ? N2 Ru N3 C16 178.8(4) . . . . ? N2 Ru N3 C16 -1.9(4) 4_755 . . . ? N1 Ru N3 C16 -82.5(4) 4_755 . . . ? N1 Ru N3 C16 179.3(4) . . . . ? N3 Ru N3 C16 76.2(4) 4_755 . . . ? N2 Ru N3 C12 5.0(3) . . . . ? N2 Ru N3 C12 -175.7(3) 4_755 . . . ? N1 Ru N3 C12 103.7(3) 4_755 . . . ? N1 Ru N3 C12 5.5(6) . . . . ? N3 Ru N3 C12 -97.5(3) 4_755 . . . ? C6 N1 C2 C3 0.0(6) . . . . ? Ru N1 C2 C3 -171.9(3) . . . . ? N1 C2 C3 C4 1.8(7) . . . . ? N1 C2 C3 C17 -177.4(4) . . . . ? C2 C3 C4 C5 -2.2(7) . . . . ? C17 C3 C4 C5 177.0(4) . . . . ? C3 C4 C5 C6 0.8(7) . . . . ? C2 N1 C6 C5 -1.5(6) . . . . ? Ru N1 C6 C5 171.5(3) . . . . ? C2 N1 C6 C7 178.5(4) . . . . ? Ru N1 C6 C7 -8.5(5) . . . . ? C4 C5 C6 N1 1.2(7) . . . . ? C4 C5 C6 C7 -178.9(5) . . . . ? C11 N2 C7 C8 -1.3(7) . . . . ? Ru N2 C7 C8 -179.8(4) . . . . ? C11 N2 C7 C6 179.9(4) . . . . ? Ru N2 C7 C6 1.4(5) . . . . ? N1 C6 C7 N2 4.8(6) . . . . ? C5 C6 C7 N2 -175.1(4) . . . . ? N1 C6 C7 C8 -173.8(5) . . . . ? C5 C6 C7 C8 6.3(8) . . . . ? N2 C7 C8 C9 1.4(8) . . . . ? C6 C7 C8 C9 180.0(5) . . . . ? C7 C8 C9 C10 -0.6(9) . . . . ? C8 C9 C10 C11 -0.4(9) . . . . ? C7 N2 C11 C10 0.3(7) . . . . ? Ru N2 C11 C10 178.8(4) . . . . ? C7 N2 C11 C12 -177.5(4) . . . . ? Ru N2 C11 C12 1.0(5) . . . . ? C9 C10 C11 N2 0.5(8) . . . . ? C9 C10 C11 C12 178.0(5) . . . . ? C16 N3 C12 C13 -2.5(7) . . . . ? Ru N3 C12 C13 171.8(4) . . . . ? C16 N3 C12 C11 179.5(4) . . . . ? Ru N3 C12 C11 -6.1(5) . . . . ? N2 C11 C12 N3 3.5(6) . . . . ? C10 C11 C12 N3 -174.1(5) . . . . ? N2 C11 C12 C13 -174.3(5) . . . . ? C10 C11 C12 C13 8.1(9) . . . . ? N3 C12 C13 C14 1.2(8) . . . . ? C11 C12 C13 C14 179.0(5) . . . . ? C12 C13 C14 C15 0.9(8) . . . . ? C13 C14 C15 C16 -1.7(8) . . . . ? C13 C14 C15 C26 -179.8(5) . . . . ? C12 N3 C16 C15 1.8(7) . . . . ? Ru N3 C16 C15 -171.7(3) . . . . ? C14 C15 C16 N3 0.4(7) . . . . ? C26 C15 C16 N3 178.5(4) . . . . ? C4 C3 C17 C18 118.9(5) . . . . ? C2 C3 C17 C18 -61.9(6) . . . . ? C4 C3 C17 C22 -60.4(6) . . . . ? C2 C3 C17 C22 118.8(5) . . . . ? C22 C17 C18 C19 -3.1(7) . . . . ? C3 C17 C18 C19 177.6(4) . . . . ? C22 C17 C18 C23 176.7(5) . . . . ? C3 C17 C18 C23 -2.6(7) . . . . ? C17 C18 C19 C20 2.2(7) . . . . ? C23 C18 C19 C20 -177.6(5) . . . . ? C24 O1 C20 C21 0.3(9) . . . . ? C24 O1 C20 C19 -179.7(6) . . . . ? C18 C19 C20 C21 -0.5(8) . . . . ? C18 C19 C20 O1 179.6(5) . . . . ? O1 C20 C21 C22 179.5(5) . . . . ? C19 C20 C21 C22 -0.5(9) . . . . ? C20 C21 C22 C17 -0.3(8) . . . . ? C20 C21 C22 C25 180.0(5) . . . . ? C18 C17 C22 C21 2.2(7) . . . . ? C3 C17 C22 C21 -178.5(5) . . . . ? C18 C17 C22 C25 -178.1(5) . . . . ? C3 C17 C22 C25 1.2(7) . . . . ? C14 C15 C26 C27 126.9(5) . . . . ? C16 C15 C26 C27 -51.2(6) . . . . ? C14 C15 C26 C31 -52.9(6) . . . . ? C16 C15 C26 C31 129.1(5) . . . . ? C31 C26 C27 C28 0.3(6) . . . . ? C15 C26 C27 C28 -179.5(4) . . . . ? C31 C26 C27 C32 -179.7(4) . . . . ? C15 C26 C27 C32 0.6(7) . . . . ? C26 C27 C28 C29 0.4(6) . . . . ? C32 C27 C28 C29 -179.6(4) . . . . ? C27 C28 C29 O2 178.2(4) . . . . ? C27 C28 C29 C30 -1.1(6) . . . . ? C33 O2 C29 C28 -6.5(6) . . . . ? C33 O2 C29 C30 172.8(4) . . . . ? C28 C29 C30 C31 1.1(7) . . . . ? O2 C29 C30 C31 -178.2(4) . . . . ? C29 C30 C31 C26 -0.4(6) . . . . ? C29 C30 C31 C34 -179.1(4) . . . . ? C27 C26 C31 C30 -0.3(6) . . . . ? C15 C26 C31 C30 179.5(4) . . . . ? C27 C26 C31 C34 178.4(4) . . . . ? C15 C26 C31 C34 -1.9(6) . . . . ? # End of CIF ============================================================