# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1899 data_biptef _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H46 Co F12 N6 O P2' _chemical_formula_weight 1191.88 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 22.6852(17) _cell_length_b 16.9553(13) _cell_length_c 16.2765(12) _cell_angle_alpha 90.00 _cell_angle_beta 120.6580(10) _cell_angle_gamma 90.00 _cell_volume 5385.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2888 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description blocks _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2436 _exptl_absorpt_coefficient_mu 0.467 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.34 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Systematic absences indicated either space group Cc or C2/c. The former was chosen for structure solution and shown to be correct by successful refinement. Inspection of the final structure did not reveal any additional symmetry. The structure was solved by direct methods using SHELXS (Sheldrick, 1990) (TREF) with additional light atoms found by Fourier methods, including one lattice molecule of tetra-hydro furan. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 times the equivalent isotropic displacement parameter of the atom to which they are attached. The absolute structure of the individual crystal chosen was checked by refinement of a delta-f" multiplier. Absolute structure parameter x = 0.10(4). This gives a rather weak indication that the absolute structure is correct. Floating origin constraints were generated automatically. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 10476 _diffrn_reflns_av_R_equivalents 0.1499 _diffrn_reflns_av_sigmaI/netI 0.1929 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5068 _reflns_number_gt 2517 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PC (Siemens, 1994)' _computing_publication_material 'SHELXTL PC (Siemens, 1994)' _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^)+(0.0730P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(4) _refine_ls_number_reflns 5068 _refine_ls_number_parameters 721 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1714 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.1958 _refine_ls_wR_factor_gt 0.1555 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.004 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 Co1 Co 0.26948(13) 0.75202(13) 0.18853(17) 0.0477(6) Uani 1 1 d . . . N11 N 0.2025(7) 0.7891(8) 0.2190(9) 0.049(4) Uani 1 1 d . . . C12 C 0.1680(8) 0.7490(10) 0.2515(11) 0.056(4) Uani 1 1 d . . . H12A H 0.1772 0.6953 0.2629 0.068 Uiso 1 1 calc R . . C13 C 0.1200(10) 0.7802(11) 0.2697(13) 0.065(5) Uani 1 1 d . . . H13A H 0.0983 0.7490 0.2934 0.078 Uiso 1 1 calc R . . C14 C 0.1048(10) 0.8607(11) 0.2512(13) 0.070(5) Uani 1 1 d . . . H14A H 0.0724 0.8844 0.2620 0.084 Uiso 1 1 calc R . . C15 C 0.1386(9) 0.9031(9) 0.2173(11) 0.055(5) Uani 1 1 d . . . H15A H 0.1297 0.9567 0.2056 0.066 Uiso 1 1 calc R . . C16 C 0.1852(8) 0.8685(9) 0.2002(10) 0.042(4) Uani 1 1 d . . . C17 C 0.2273(8) 0.9098(8) 0.1685(10) 0.040(4) Uani 1 1 d . . . N18 N 0.2689(7) 0.8603(6) 0.1596(9) 0.041(4) Uani 1 1 d . . . C19 C 0.3139(9) 0.8853(10) 0.1360(11) 0.049(4) Uani 1 1 d . . . C110 C 0.3195(8) 0.9667(8) 0.1214(10) 0.043(4) Uani 1 1 d . . . H11A H 0.3537 0.9849 0.1109 0.052 Uiso 1 1 calc R . . C111 C 0.2740(8) 1.0178(9) 0.1231(11) 0.041(4) Uani 1 1 d . . . C112 C 0.2279(9) 0.9892(9) 0.1509(10) 0.050(5) Uani 1 1 d . . . H11B H 0.1985 1.0235 0.1572 0.060 Uiso 1 1 calc R . . C113 C 0.3555(8) 0.8222(9) 0.1308(10) 0.042(4) Uani 1 1 d . . . N114 N 0.3381(6) 0.7501(8) 0.1490(8) 0.038(3) Uani 1 1 d . . . C115 C 0.3749(9) 0.6900(10) 0.1503(11) 0.053(5) Uani 1 1 d . . . H11C H 0.3645 0.6412 0.1660 0.063 Uiso 1 1 calc R . . C116 C 0.4260(11) 0.6915(11) 0.1313(15) 0.082(6) Uani 1 1 d . . . H11D H 0.4498 0.6463 0.1331 0.098 Uiso 1 1 calc R . . C117 C 0.4411(10) 0.7648(12) 0.1088(13) 0.074(6) Uani 1 1 d . . . H11E H 0.4750 0.7691 0.0931 0.089 Uiso 1 1 calc R . . C118 C 0.4066(9) 0.8309(10) 0.1096(12) 0.063(5) Uani 1 1 d . . . H11F H 0.4174 0.8803 0.0961 0.075 Uiso 1 1 calc R . . C119 C 0.2797(8) 1.1034(8) 0.1109(12) 0.043(4) Uani 1 1 d . . . C120 C 0.3408(8) 1.1386(9) 0.1311(12) 0.053(5) Uani 1 1 d . . . H12B H 0.3803 1.1080 0.1573 0.063 Uiso 1 1 calc R . . C121 C 0.3451(9) 1.2168(9) 0.1139(12) 0.053(5) Uani 1 1 d . . . H12C H 0.3874 1.2378 0.1293 0.064 Uiso 1 1 calc R . . C122 C 0.2904(9) 1.2635(10) 0.0759(12) 0.049(5) Uani 1 1 d . . . C123 C 0.2261(10) 1.2308(10) 0.0540(13) 0.067(6) Uani 1 1 d . . . H12D H 0.1875 1.2629 0.0282 0.081 Uiso 1 1 calc R . . C124 C 0.2203(10) 1.1497(9) 0.0711(12) 0.065(6) Uani 1 1 d . . . H12F H 0.1783 1.1280 0.0562 0.078 Uiso 1 1 calc R . . C125 C 0.2931(8) 1.3504(8) 0.0559(11) 0.036(4) Uani 1 1 d . . . C126 C 0.3505(10) 1.3931(9) 0.1102(12) 0.061(5) Uani 1 1 d . . . H12E H 0.3880 1.3688 0.1614 0.073 Uiso 1 1 calc R . . C127 C 0.3552(10) 1.4729(9) 0.0916(14) 0.062(5) Uani 1 1 d . . . H12I H 0.3944 1.5016 0.1323 0.075 Uiso 1 1 calc R . . C128 C 0.3028(11) 1.5079(10) 0.0144(13) 0.060(5) Uani 1 1 d . . . H12J H 0.3065 1.5605 0.0015 0.072 Uiso 1 1 calc R . . C129 C 0.2450(10) 1.4673(9) -0.0445(12) 0.062(6) Uani 1 1 d . . . H12K H 0.2096 1.4919 -0.0981 0.075 Uiso 1 1 calc R . . C130 C 0.2380(10) 1.3880(10) -0.0249(12) 0.067(5) Uani 1 1 d . . . H13B H 0.1978 1.3605 -0.0644 0.081 Uiso 1 1 calc R . . N21 N 0.3439(6) 0.7540(8) 0.3190(7) 0.042(4) Uani 1 1 d U . . C22 C 0.3819(9) 0.8170(10) 0.3692(13) 0.051(5) Uani 1 1 d . . . H22A H 0.3683 0.8660 0.3398 0.062 Uiso 1 1 calc R . . C23 C 0.4385(11) 0.8155(10) 0.4592(14) 0.072(6) Uani 1 1 d . . . H23A H 0.4620 0.8616 0.4888 0.086 Uiso 1 1 calc R . . C24 C 0.4598(11) 0.7433(13) 0.5050(13) 0.080(7) Uani 1 1 d . . . H24A H 0.4987 0.7390 0.5653 0.096 Uiso 1 1 calc R . . C25 C 0.4195(9) 0.6758(10) 0.4558(12) 0.052(5) Uani 1 1 d . . . H25A H 0.4301 0.6266 0.4852 0.062 Uiso 1 1 calc R . . C26 C 0.3661(9) 0.6843(9) 0.3661(13) 0.048(4) Uani 1 1 d . . . C27 C 0.3217(9) 0.6177(9) 0.3054(12) 0.048(5) Uani 1 1 d . . . N28 N 0.2731(7) 0.6452(6) 0.2201(10) 0.035(3) Uani 1 1 d . . . C29 C 0.2298(8) 0.5933(8) 0.1539(10) 0.031(4) Uani 1 1 d . . . C210 C 0.2323(8) 0.5134(8) 0.1753(13) 0.048(5) Uani 1 1 d . . . H21A H 0.2009 0.4789 0.1295 0.058 Uiso 1 1 calc R . . C211 C 0.2791(9) 0.4863(9) 0.2602(12) 0.042(4) Uani 1 1 d . . . C212 C 0.3266(8) 0.5388(8) 0.3273(11) 0.037(4) Uani 1 1 d . . . H21B H 0.3612 0.5206 0.3863 0.045 Uiso 1 1 calc R . . C213 C 0.1827(8) 0.6339(9) 0.0641(12) 0.044(4) Uani 1 1 d . . . N214 N 0.1963(7) 0.7131(7) 0.0637(9) 0.045(4) Uani 1 1 d . . . C215 C 0.1545(9) 0.7562(9) -0.0121(12) 0.052(5) Uani 1 1 d . . . H21C H 0.1606 0.8105 -0.0108 0.062 Uiso 1 1 calc R . . C216 C 0.1014(11) 0.7208(11) -0.0936(14) 0.069(6) Uani 1 1 d . . . H21D H 0.0734 0.7518 -0.1465 0.083 Uiso 1 1 calc R . . C217 C 0.0898(10) 0.6423(11) -0.0974(15) 0.075(6) Uani 1 1 d . . . H21E H 0.0554 0.6185 -0.1527 0.090 Uiso 1 1 calc R . . C218 C 0.1308(9) 0.5986(9) -0.0158(14) 0.055(4) Uani 1 1 d . . . H21F H 0.1231 0.5448 -0.0154 0.066 Uiso 1 1 calc R . . C219 C 0.2826(9) 0.4015(8) 0.2860(12) 0.043(4) Uani 1 1 d . . . C220 C 0.3450(9) 0.3606(9) 0.3371(11) 0.053(5) Uani 1 1 d . . . H22B H 0.3858 0.3878 0.3571 0.064 Uiso 1 1 calc R . . C221 C 0.3478(11) 0.2807(9) 0.3588(13) 0.065(6) Uani 1 1 d . . . H22C H 0.3898 0.2549 0.3914 0.078 Uiso 1 1 calc R . . C222 C 0.2872(9) 0.2394(8) 0.3314(10) 0.037(4) Uani 1 1 d . . . C223 C 0.2286(10) 0.2813(10) 0.2866(15) 0.075(6) Uani 1 1 d . . . H22D H 0.1879 0.2554 0.2704 0.090 Uiso 1 1 calc R . . C224 C 0.2250(11) 0.3623(11) 0.2628(13) 0.071(6) Uani 1 1 d . . . H22E H 0.1829 0.3880 0.2312 0.085 Uiso 1 1 calc R . . C225 C 0.2913(9) 0.1554(9) 0.3553(11) 0.043(4) Uani 1 1 d . . . C226 C 0.3450(10) 0.1105(10) 0.3710(11) 0.059(5) Uani 1 1 d . . . H22F H 0.3799 0.1340 0.3658 0.071 Uiso 1 1 calc R . . C227 C 0.3511(12) 0.0302(11) 0.3948(13) 0.077(6) Uani 1 1 d . . . H22G H 0.3887 0.0004 0.4050 0.093 Uiso 1 1 calc R . . C228 C 0.2967(12) -0.0032(11) 0.4025(12) 0.071(6) Uani 1 1 d . . . H22H H 0.2987 -0.0562 0.4186 0.085 Uiso 1 1 calc R . . C229 C 0.2412(10) 0.0411(10) 0.3867(13) 0.065(5) Uani 1 1 d . . . H22I H 0.2056 0.0187 0.3913 0.078 Uiso 1 1 calc R . . C230 C 0.2396(11) 0.1202(10) 0.3636(13) 0.076(6) Uani 1 1 d . . . H23C H 0.2024 0.1506 0.3533 0.091 Uiso 1 1 calc R . . P1 P 0.5411(3) 1.0335(3) 0.1856(4) 0.0650(15) Uani 1 1 d . . . F11 F 0.5947(10) 1.0616(11) 0.2847(12) 0.209(8) Uani 1 1 d . . . F12 F 0.4779(8) 1.0109(8) 0.0942(11) 0.182(8) Uani 1 1 d . . . F13 F 0.5022(11) 1.0106(8) 0.2373(16) 0.189(9) Uani 1 1 d . . . F14 F 0.5784(13) 1.0536(10) 0.138(2) 0.262(13) Uani 1 1 d . . . F15 F 0.5137(8) 1.1193(6) 0.1719(8) 0.139(6) Uani 1 1 d . . . F16 F 0.5681(8) 0.9475(7) 0.2021(9) 0.141(5) Uani 1 1 d . . . P2 P 0.0361(3) 0.0353(3) 0.3826(4) 0.0766(17) Uani 1 1 d . . . F21 F -0.0208(8) 0.0960(10) 0.3288(11) 0.180(7) Uani 1 1 d . . . F22 F 0.0937(7) -0.0279(9) 0.4291(14) 0.188(7) Uani 1 1 d . . . F23 F -0.0026(9) -0.0018(9) 0.4270(17) 0.195(8) Uani 1 1 d . . . F24 F 0.0818(11) 0.0767(11) 0.3521(19) 0.239(11) Uani 1 1 d . . . F25 F 0.0053(10) -0.0182(12) 0.3015(13) 0.279(15) Uani 1 1 d . . . F26 F 0.0674(8) 0.0893(9) 0.4702(11) 0.174(6) Uani 1 1 d . . . C002 C 1.0076(15) 0.692(3) 0.359(3) 0.157(14) Uani 1 1 d . . . H00A H 0.9592 0.6823 0.3156 0.189 Uiso 1 1 calc R . . H00B H 1.0318 0.6828 0.3251 0.189 Uiso 1 1 calc R . . C004 C 1.0610(18) 0.691(4) 0.535(2) 0.24(4) Uani 1 1 d . . . H00C H 1.1087 0.6795 0.5808 0.293 Uiso 1 1 calc R . . H00D H 1.0344 0.6813 0.5657 0.293 Uiso 1 1 calc R . . O001 O 1.0185(14) 0.7765(18) 0.395(3) 0.194(11) Uani 1 1 d . . . C003 C 1.0521(19) 0.784(3) 0.499(3) 0.25(3) Uani 1 1 d . . . H00E H 1.0239 0.8132 0.5172 0.303 Uiso 1 1 calc R . . H00F H 1.0963 0.8094 0.5254 0.303 Uiso 1 1 calc R . . C001 C 1.0341(17) 0.6384(17) 0.443(5) 0.19(2) Uani 1 1 d . . . H00G H 1.0711 0.6063 0.4475 0.224 Uiso 1 1 calc R . . H00H H 0.9979 0.6037 0.4361 0.224 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0635(14) 0.0334(11) 0.0581(13) -0.0053(11) 0.0397(12) -0.0078(12) N11 0.050(9) 0.042(9) 0.045(9) -0.007(7) 0.018(8) 0.001(8) C12 0.062(12) 0.041(10) 0.077(12) -0.015(10) 0.043(11) -0.002(10) C13 0.084(15) 0.050(12) 0.084(15) -0.005(10) 0.060(14) -0.013(11) C14 0.086(15) 0.063(13) 0.092(14) -0.006(11) 0.068(13) 0.007(12) C15 0.082(13) 0.038(10) 0.062(11) 0.006(8) 0.049(11) 0.005(10) C16 0.045(10) 0.047(11) 0.040(10) -0.021(8) 0.026(9) -0.005(9) C17 0.040(11) 0.030(10) 0.052(11) 0.015(8) 0.025(10) 0.011(8) N18 0.053(9) 0.021(7) 0.056(10) -0.006(6) 0.032(8) 0.001(8) C19 0.059(12) 0.049(12) 0.063(11) 0.005(9) 0.050(11) -0.009(9) C110 0.053(11) 0.032(9) 0.063(11) -0.004(8) 0.043(10) -0.009(9) C111 0.045(11) 0.028(9) 0.066(12) -0.004(8) 0.039(10) -0.020(8) C112 0.081(13) 0.033(10) 0.040(10) 0.016(8) 0.033(10) 0.007(9) C113 0.037(10) 0.029(10) 0.061(11) -0.014(8) 0.027(9) -0.020(8) N114 0.040(8) 0.032(7) 0.052(8) -0.014(7) 0.030(7) 0.017(7) C115 0.045(11) 0.053(12) 0.063(12) -0.022(9) 0.031(10) -0.027(10) C116 0.087(16) 0.052(13) 0.123(17) 0.032(12) 0.066(15) 0.014(12) C117 0.086(15) 0.083(16) 0.100(15) 0.012(12) 0.081(14) -0.006(13) C118 0.069(14) 0.042(12) 0.097(14) 0.010(10) 0.058(13) -0.001(10) C119 0.050(12) 0.013(8) 0.068(12) 0.007(8) 0.032(10) 0.003(8) C120 0.039(11) 0.024(9) 0.101(15) 0.003(9) 0.040(11) 0.002(8) C121 0.041(11) 0.042(11) 0.086(13) 0.007(9) 0.040(11) 0.013(9) C122 0.051(12) 0.047(12) 0.063(12) -0.008(10) 0.040(11) -0.016(10) C123 0.075(15) 0.056(13) 0.091(15) 0.011(10) 0.058(13) 0.017(11) C124 0.098(17) 0.038(11) 0.071(13) 0.008(9) 0.052(13) 0.006(11) C125 0.049(12) 0.010(8) 0.056(11) -0.005(8) 0.032(10) -0.007(8) C126 0.095(15) 0.042(11) 0.076(13) -0.012(9) 0.066(13) -0.022(11) C127 0.084(15) 0.044(11) 0.084(15) -0.016(10) 0.060(14) -0.026(11) C128 0.087(15) 0.040(10) 0.043(11) 0.004(10) 0.026(11) 0.009(12) C129 0.106(17) 0.029(11) 0.048(11) 0.000(9) 0.036(12) -0.002(11) C130 0.094(16) 0.059(13) 0.067(13) 0.000(10) 0.055(13) 0.017(12) N21 0.069(9) 0.038(7) 0.017(7) -0.024(7) 0.021(6) -0.017(8) C22 0.049(12) 0.055(12) 0.050(12) -0.006(10) 0.025(11) -0.006(10) C23 0.104(18) 0.035(11) 0.067(15) -0.001(11) 0.036(15) -0.001(12) C24 0.078(15) 0.089(16) 0.056(13) -0.042(14) 0.022(12) -0.033(15) C25 0.057(13) 0.068(13) 0.030(11) 0.004(10) 0.022(11) 0.007(11) C26 0.062(12) 0.029(10) 0.057(13) 0.022(10) 0.034(11) 0.009(10) C27 0.079(14) 0.039(11) 0.043(11) 0.006(9) 0.044(11) 0.019(10) N28 0.053(9) 0.013(6) 0.047(10) 0.000(7) 0.031(8) 0.011(7) C29 0.044(11) 0.023(9) 0.037(9) 0.015(8) 0.028(9) 0.012(8) C210 0.061(13) 0.017(9) 0.084(14) -0.018(9) 0.050(12) -0.025(8) C211 0.051(12) 0.034(10) 0.044(11) 0.013(9) 0.026(10) 0.015(10) C212 0.037(10) 0.027(9) 0.057(11) 0.025(8) 0.030(10) 0.016(8) C213 0.039(11) 0.040(10) 0.055(12) -0.014(10) 0.025(10) -0.003(9) N214 0.052(9) 0.033(8) 0.067(11) -0.011(8) 0.043(9) -0.001(7) C215 0.083(14) 0.024(9) 0.064(12) 0.029(10) 0.049(12) 0.018(10) C216 0.095(17) 0.047(12) 0.058(13) -0.032(10) 0.035(13) -0.021(11) C217 0.071(15) 0.057(13) 0.090(16) -0.008(13) 0.036(14) 0.005(12) C218 0.057(12) 0.025(9) 0.087(13) -0.005(11) 0.039(12) -0.005(10) C219 0.056(12) 0.022(9) 0.058(11) 0.002(9) 0.035(10) 0.011(9) C220 0.056(13) 0.045(11) 0.065(12) 0.001(9) 0.037(11) 0.010(9) C221 0.096(16) 0.030(10) 0.096(15) 0.044(9) 0.067(14) 0.032(10) C222 0.047(11) 0.021(9) 0.043(10) 0.010(7) 0.022(10) 0.010(9) C223 0.067(15) 0.032(11) 0.124(18) 0.003(11) 0.047(15) -0.011(11) C224 0.067(15) 0.055(13) 0.073(14) 0.005(10) 0.023(13) -0.002(11) C225 0.045(11) 0.037(10) 0.051(11) -0.012(8) 0.027(10) -0.016(10) C226 0.072(13) 0.045(12) 0.058(12) 0.009(9) 0.031(11) 0.006(10) C227 0.111(18) 0.040(12) 0.092(15) 0.001(10) 0.060(15) 0.002(12) C228 0.096(17) 0.042(12) 0.053(12) -0.003(9) 0.022(13) -0.016(12) C229 0.088(16) 0.040(12) 0.083(14) 0.012(10) 0.055(13) -0.015(11) C230 0.109(18) 0.039(12) 0.082(14) -0.020(10) 0.049(14) -0.009(11) P1 0.069(4) 0.058(3) 0.072(4) 0.015(3) 0.039(4) 0.002(3) F11 0.162(16) 0.212(18) 0.136(14) -0.024(13) -0.009(13) 0.027(14) F12 0.155(15) 0.094(10) 0.150(13) 0.007(9) -0.028(13) -0.015(10) F13 0.29(2) 0.099(11) 0.30(2) 0.061(13) 0.24(2) 0.042(13) F14 0.37(3) 0.156(15) 0.51(4) 0.033(19) 0.40(3) 0.004(17) F15 0.248(16) 0.061(7) 0.096(8) 0.022(6) 0.078(10) 0.016(9) F16 0.204(14) 0.121(10) 0.147(11) 0.056(9) 0.125(12) 0.107(10) P2 0.055(4) 0.069(4) 0.095(4) -0.007(3) 0.031(4) 0.001(3) F21 0.164(14) 0.246(16) 0.163(13) 0.076(12) 0.107(13) 0.144(13) F22 0.121(12) 0.139(12) 0.29(2) 0.082(13) 0.098(14) 0.087(10) F23 0.188(17) 0.133(12) 0.36(2) 0.046(16) 0.206(19) 0.004(11) F24 0.26(2) 0.168(17) 0.43(3) 0.085(19) 0.29(3) 0.066(16) F25 0.159(17) 0.28(2) 0.193(18) -0.161(17) -0.062(14) 0.117(16) F26 0.136(12) 0.198(15) 0.140(12) -0.050(12) 0.035(11) -0.043(11) C002 0.11(3) 0.19(3) 0.26(5) -0.07(4) 0.16(3) -0.05(3) C004 0.07(2) 0.61(11) 0.09(2) 0.17(4) 0.06(2) 0.07(4) O001 0.17(2) 0.19(2) 0.30(4) 0.07(2) 0.18(3) 0.033(18) C003 0.11(3) 0.52(9) 0.21(4) -0.26(5) 0.14(3) -0.17(4) C001 0.10(3) 0.12(2) 0.41(6) 0.10(4) 0.18(4) 0.05(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N28 1.873(11) . Y Co1 N18 1.894(11) . Y Co1 N21 1.925(11) . Y Co1 N11 1.928(14) . Y Co1 N114 1.966(12) . Y Co1 N214 1.971(13) . Y N11 C12 1.334(19) . ? N11 C16 1.392(17) . ? C12 C13 1.37(2) . ? C13 C14 1.40(2) . ? C14 C15 1.36(2) . ? C15 C16 1.36(2) . ? C16 C17 1.474(19) . ? C17 N18 1.324(17) . ? C17 C112 1.377(18) . ? N18 C19 1.330(18) . ? C19 C110 1.417(19) . ? C19 C113 1.46(2) . ? C110 C111 1.359(19) . ? C111 C112 1.42(2) . ? C111 C119 1.479(18) . ? C113 N114 1.363(16) . ? C113 C118 1.38(2) . ? N114 C115 1.309(18) . ? C115 C116 1.35(2) . ? C116 C117 1.39(2) . ? C117 C118 1.37(2) . ? C119 C120 1.385(19) . ? C119 C124 1.40(2) . ? C120 C121 1.368(19) . ? C121 C122 1.33(2) . ? C122 C123 1.43(2) . ? C122 C125 1.52(2) . ? C123 C124 1.42(2) . ? C125 C126 1.35(2) . ? C125 C130 1.42(2) . ? C126 C127 1.40(2) . ? C127 C128 1.35(2) . ? C128 C129 1.35(2) . ? C129 C130 1.41(2) . ? N21 C22 1.354(18) . ? N21 C26 1.359(17) . ? C22 C23 1.37(2) . ? C23 C24 1.38(2) . ? C24 C25 1.43(2) . ? C25 C26 1.347(18) . ? C26 C27 1.50(2) . ? C27 N28 1.342(17) . ? C27 C212 1.374(18) . ? N28 C29 1.349(16) . ? C29 C210 1.392(18) . ? C29 C213 1.468(19) . ? C210 C211 1.32(2) . ? C211 C212 1.395(19) . ? C211 C219 1.49(2) . ? C213 C218 1.37(2) . ? C213 N214 1.378(16) . ? N214 C215 1.327(17) . ? C215 C216 1.39(2) . ? C216 C217 1.35(2) . ? C217 C218 1.38(2) . ? C219 C224 1.34(2) . ? C219 C220 1.41(2) . ? C220 C221 1.394(19) . ? C221 C222 1.40(2) . ? C222 C223 1.35(2) . ? C222 C225 1.47(2) . ? C223 C224 1.42(2) . ? C225 C226 1.35(2) . ? C225 C230 1.38(2) . ? C226 C227 1.40(2) . ? C227 C228 1.42(3) . ? C228 C229 1.37(2) . ? C229 C230 1.39(2) . ? P1 F14 1.453(16) . ? P1 F12 1.497(13) . ? P1 F11 1.519(17) . ? P1 F13 1.547(15) . ? P1 F16 1.551(11) . ? P1 F15 1.553(11) . ? P2 F25 1.453(14) . ? P2 F24 1.529(18) . ? P2 F21 1.529(13) . ? P2 F23 1.529(16) . ? P2 F26 1.531(15) . ? P2 F22 1.554(12) . ? C002 C001 1.49(4) . ? C002 O001 1.52(4) . ? C004 C001 1.58(6) . ? C004 C003 1.65(7) . ? O001 C003 1.46(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 N28 Co1 N18 178.1(7) . . ? N28 Co1 N21 79.8(6) . . ? N18 Co1 N21 98.5(6) . . ? N28 Co1 N11 100.1(6) . . ? N18 Co1 N11 80.9(6) . . ? N21 Co1 N11 94.2(5) . . ? N28 Co1 N114 98.2(6) . . ? N18 Co1 N114 80.9(6) . . ? N21 Co1 N114 88.0(5) . . ? N11 Co1 N114 161.7(6) . . ? N28 Co1 N214 81.7(6) . . ? N18 Co1 N214 100.0(6) . . ? N21 Co1 N214 161.4(6) . . ? N11 Co1 N214 90.8(5) . . ? N114 Co1 N214 92.8(5) . . ? C12 N11 C16 115.1(15) . . ? C12 N11 Co1 129.4(12) . . ? C16 N11 Co1 115.4(12) . . ? N11 C12 C13 125.4(17) . . ? C12 C13 C14 117.7(18) . . ? C15 C14 C13 118.3(18) . . ? C14 C15 C16 121.1(16) . . ? C15 C16 N11 122.3(16) . . ? C15 C16 C17 125.4(16) . . ? N11 C16 C17 112.1(14) . . ? N18 C17 C112 120.9(14) . . ? N18 C17 C16 111.2(13) . . ? C112 C17 C16 127.8(15) . . ? C17 N18 C19 121.6(13) . . ? C17 N18 Co1 120.1(11) . . ? C19 N18 Co1 118.1(11) . . ? N18 C19 C110 120.3(15) . . ? N18 C19 C113 113.5(14) . . ? C110 C19 C113 126.2(15) . . ? C111 C110 C19 119.0(14) . . ? C110 C111 C112 118.6(13) . . ? C110 C111 C119 120.3(14) . . ? C112 C111 C119 120.5(15) . . ? C17 C112 C111 119.1(15) . . ? N114 C113 C118 121.6(14) . . ? N114 C113 C19 112.3(14) . . ? C118 C113 C19 126.1(15) . . ? C115 N114 C113 116.8(13) . . ? C115 N114 Co1 127.7(12) . . ? C113 N114 Co1 114.9(10) . . ? N114 C115 C116 126.6(17) . . ? C115 C116 C117 115.9(19) . . ? C118 C117 C116 120.8(17) . . ? C117 C118 C113 118.2(15) . . ? C120 C119 C124 118.6(14) . . ? C120 C119 C111 122.5(14) . . ? C124 C119 C111 118.8(14) . . ? C121 C120 C119 122.4(14) . . ? C122 C121 C120 121.7(16) . . ? C121 C122 C123 118.6(16) . . ? C121 C122 C125 123.3(15) . . ? C123 C122 C125 118.2(16) . . ? C122 C123 C124 120.8(17) . . ? C119 C124 C123 118.0(17) . . ? C126 C125 C130 117.7(14) . . ? C126 C125 C122 120.7(15) . . ? C130 C125 C122 121.4(15) . . ? C125 C126 C127 122.0(17) . . ? C128 C127 C126 119.8(17) . . ? C127 C128 C129 120.8(17) . . ? C128 C129 C130 120.3(17) . . ? C129 C130 C125 119.3(17) . . ? C22 N21 C26 114.0(14) . . ? C22 N21 Co1 127.6(12) . . ? C26 N21 Co1 118.1(11) . . ? N21 C22 C23 126.3(16) . . ? C22 C23 C24 118.1(17) . . ? C23 C24 C25 117.3(17) . . ? C26 C25 C24 119.1(16) . . ? C25 C26 N21 125.1(16) . . ? C25 C26 C27 124.3(15) . . ? N21 C26 C27 110.6(15) . . ? N28 C27 C212 121.4(15) . . ? N28 C27 C26 110.0(13) . . ? C212 C27 C26 128.6(16) . . ? C27 N28 C29 118.7(12) . . ? C27 N28 Co1 121.2(11) . . ? C29 N28 Co1 119.9(10) . . ? N28 C29 C210 120.9(13) . . ? N28 C29 C213 110.7(12) . . ? C210 C29 C213 128.4(15) . . ? C211 C210 C29 120.6(14) . . ? C210 C211 C212 118.9(14) . . ? C210 C211 C219 122.0(16) . . ? C212 C211 C219 119.1(14) . . ? C27 C212 C211 119.3(14) . . ? C218 C213 N214 120.4(15) . . ? C218 C213 C29 125.3(15) . . ? N214 C213 C29 114.3(14) . . ? C215 N214 C213 119.1(14) . . ? C215 N214 Co1 127.0(12) . . ? C213 N214 Co1 113.2(11) . . ? N214 C215 C216 120.6(16) . . ? C217 C216 C215 121(2) . . ? C216 C217 C218 117.5(19) . . ? C213 C218 C217 120.7(15) . . ? C224 C219 C220 117.8(15) . . ? C224 C219 C211 119.8(16) . . ? C220 C219 C211 122.4(16) . . ? C221 C220 C219 122.1(16) . . ? C220 C221 C222 119.7(16) . . ? C223 C222 C221 116.6(15) . . ? C223 C222 C225 124.4(17) . . ? C221 C222 C225 118.9(15) . . ? C222 C223 C224 124.1(18) . . ? C219 C224 C223 119.5(18) . . ? C226 C225 C230 117.8(16) . . ? C226 C225 C222 121.8(16) . . ? C230 C225 C222 120.3(17) . . ? C225 C226 C227 123.7(18) . . ? C226 C227 C228 116.3(19) . . ? C229 C228 C227 121.3(18) . . ? C228 C229 C230 118.3(18) . . ? C225 C230 C229 122.6(19) . . ? F14 P1 F12 93.0(14) . . ? F14 P1 F11 97.2(14) . . ? F12 P1 F11 168.0(13) . . ? F14 P1 F13 178.9(11) . . ? F12 P1 F13 87.3(11) . . ? F11 P1 F13 82.6(12) . . ? F14 P1 F16 91.6(9) . . ? F12 P1 F16 91.5(8) . . ? F11 P1 F16 94.5(9) . . ? F13 P1 F16 87.4(7) . . ? F14 P1 F15 90.2(9) . . ? F12 P1 F15 89.2(8) . . ? F11 P1 F15 84.4(9) . . ? F13 P1 F15 90.8(8) . . ? F16 P1 F15 178.1(8) . . ? F25 P2 F24 94.8(15) . . ? F25 P2 F21 91.4(9) . . ? F24 P2 F21 91.1(10) . . ? F25 P2 F23 92.7(14) . . ? F24 P2 F23 172.0(14) . . ? F21 P2 F23 91.6(9) . . ? F25 P2 F26 177.4(15) . . ? F24 P2 F26 87.7(12) . . ? F21 P2 F26 89.2(9) . . ? F23 P2 F26 84.8(11) . . ? F25 P2 F22 84.8(10) . . ? F24 P2 F22 86.2(9) . . ? F21 P2 F22 175.1(10) . . ? F23 P2 F22 91.6(9) . . ? F26 P2 F22 94.7(10) . . ? C001 C002 O001 108(3) . . ? C001 C004 C003 106(2) . . ? C003 O001 C002 114(3) . . ? O001 C003 C004 103(3) . . ? C002 C001 C004 108(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.394 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.069 data_mh009 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56.50 H47.50 B2 F8 N8.50 O6 Ru' _chemical_formula_weight 1216.22 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' 'Ru' 'Ru' -1.2594 0.8363 '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' 'B' 'B' 0.0013 0.0007 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.9750(10) _cell_length_b 16.9820(10) _cell_length_c 20.3260(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.400(10) _cell_angle_gamma 90.00 _cell_volume 5504.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 0.371 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9129 _exptl_absorpt_correction_T_max 0.9464 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32250 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.45 _reflns_number_total 12528 _reflns_number_gt 10005 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+9.0890P] 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 12528 _refine_ls_number_parameters 751 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1667 _refine_ls_wR_factor_gt 0.1566 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.987928(18) 0.480784(14) 0.241726(14) 0.02257(10) Uani 1 1 d . . . C2A C 1.1178(2) 0.4284(2) 0.35112(19) 0.0328(8) Uani 1 1 d . . . H2A H 1.0986 0.3763 0.3425 0.039 Uiso 1 1 calc R . . C2B C 0.8677(2) 0.5416(2) 0.34322(19) 0.0303(8) Uani 1 1 d . . . H2B H 0.8862 0.5929 0.3325 0.036 Uiso 1 1 calc R . . C3A C 1.1798(3) 0.4397(2) 0.3999(2) 0.0389(9) Uani 1 1 d . . . H3A H 1.2036 0.3963 0.4238 0.047 Uiso 1 1 calc R . . C3B C 0.8092(3) 0.5339(2) 0.3900(2) 0.0376(9) Uani 1 1 d . . . H3B H 0.7874 0.5791 0.4106 0.045 Uiso 1 1 calc R . . C4A C 1.2070(3) 0.5157(2) 0.4135(2) 0.0368(9) Uani 1 1 d . . . H4A H 1.2501 0.5251 0.4469 0.044 Uiso 1 1 calc R . . C4B C 0.7828(3) 0.4593(2) 0.40622(19) 0.0346(8) Uani 1 1 d . . . H4B H 0.7420 0.4526 0.4379 0.042 Uiso 1 1 calc R . . C5A C 1.1712(2) 0.5777(2) 0.37819(18) 0.0306(8) Uani 1 1 d . . . H5A H 1.1883 0.6303 0.3877 0.037 Uiso 1 1 calc R . . C5B C 0.8163(2) 0.3945(2) 0.37601(17) 0.0293(8) Uani 1 1 d . . . H5B H 0.8002 0.3428 0.3879 0.035 Uiso 1 1 calc R . . C6A C 1.1103(2) 0.56258(19) 0.32887(17) 0.0253(7) Uani 1 1 d . . . C6B C 0.8734(2) 0.40569(19) 0.32842(16) 0.0232(7) Uani 1 1 d . . . C7A C 1.0685(2) 0.62418(18) 0.28739(16) 0.0218(7) Uani 1 1 d . . . C7B C 0.9088(2) 0.34135(18) 0.29003(16) 0.0220(7) Uani 1 1 d . . . C9A C 0.9667(2) 0.64309(18) 0.19977(16) 0.0229(7) Uani 1 1 d . . . C9B C 0.9959(2) 0.31693(19) 0.20258(17) 0.0240(7) Uani 1 1 d . . . C10A C 0.9801(2) 0.72390(19) 0.20165(17) 0.0253(7) Uani 1 1 d . . . H10A H 0.9499 0.7574 0.1713 0.030 Uiso 1 1 calc R . . C10B C 0.9760(2) 0.23741(19) 0.20302(18) 0.0267(7) Uani 1 1 d . . . H10B H 0.9987 0.2026 0.1721 0.032 Uiso 1 1 calc R . . C11A C 1.0384(2) 0.75567(19) 0.24853(17) 0.0245(7) Uani 1 1 d . . . C11B C 0.9221(2) 0.20886(19) 0.24937(18) 0.0260(7) Uani 1 1 d . . . C12A C 1.0821(2) 0.70456(19) 0.29230(17) 0.0253(7) Uani 1 1 d . . . H12A H 1.1209 0.7249 0.3252 0.030 Uiso 1 1 calc R . . C12B C 0.8900(2) 0.26180(19) 0.29442(17) 0.0252(7) Uani 1 1 d . . . H12B H 0.8556 0.2434 0.3277 0.030 Uiso 1 1 calc R . . C13A C 0.9039(2) 0.59987(19) 0.15822(16) 0.0237(7) Uani 1 1 d . . . C13B C 1.0560(2) 0.35669(19) 0.16096(17) 0.0259(7) Uani 1 1 d . . . C15A C 0.8429(2) 0.4774(2) 0.13492(18) 0.0301(8) Uani 1 1 d . . . H15A H 0.8420 0.4221 0.1416 0.036 Uiso 1 1 calc R . . C15B C 1.1232(3) 0.4744(2) 0.1392(2) 0.0407(10) Uani 1 1 d . . . H15B H 1.1308 0.5291 0.1471 0.049 Uiso 1 1 calc R . . C16A C 0.7845(3) 0.5103(2) 0.09042(19) 0.0372(9) Uani 1 1 d . . . H16A H 0.7432 0.4783 0.0680 0.045 Uiso 1 1 calc R . . C16B C 1.1714(3) 0.4384(3) 0.0941(2) 0.0523(12) Uani 1 1 d . . . H16B H 1.2116 0.4677 0.0717 0.063 Uiso 1 1 calc R . . C17A C 0.7870(3) 0.5904(2) 0.07899(18) 0.0345(8) Uani 1 1 d . . . H17A H 0.7475 0.6142 0.0483 0.041 Uiso 1 1 calc R . . C17B C 1.1605(3) 0.3593(3) 0.0817(2) 0.0480(11) Uani 1 1 d . . . H17B H 1.1930 0.3333 0.0507 0.058 Uiso 1 1 calc R . . C18A C 0.8476(2) 0.6358(2) 0.11268(18) 0.0298(8) Uani 1 1 d . . . H18A H 0.8508 0.6908 0.1048 0.036 Uiso 1 1 calc R . . C18B C 1.1014(3) 0.3182(2) 0.11507(19) 0.0357(9) Uani 1 1 d . . . H18B H 1.0922 0.2638 0.1064 0.043 Uiso 1 1 calc R . . C19A C 1.0559(2) 0.84131(19) 0.25271(18) 0.0270(7) Uani 1 1 d . . . C19B C 0.8982(2) 0.12453(19) 0.25094(19) 0.0289(8) Uani 1 1 d . . . C20A C 1.0561(2) 0.8880(2) 0.19650(19) 0.0321(8) Uani 1 1 d . . . H20A H 1.0410 0.8654 0.1547 0.038 Uiso 1 1 calc R . . C20B C 0.8870(3) 0.0866(2) 0.3104(2) 0.0353(9) Uani 1 1 d . . . H20B H 0.8938 0.1152 0.3506 0.042 Uiso 1 1 calc R . . C21A C 1.0780(3) 0.9669(2) 0.2005(2) 0.0335(8) Uani 1 1 d . . . H21A H 1.0788 0.9974 0.1613 0.040 Uiso 1 1 calc R . . C21B C 0.8659(3) 0.0075(2) 0.3115(2) 0.0366(9) Uani 1 1 d . . . H21B H 0.8601 -0.0177 0.3527 0.044 Uiso 1 1 calc R . . C22A C 1.0987(2) 1.0019(2) 0.2614(2) 0.0306(8) Uani 1 1 d . . . C22B C 0.8531(2) -0.0361(2) 0.2537(2) 0.0334(9) Uani 1 1 d . . . C23A C 1.0959(2) 0.9555(2) 0.31772(19) 0.0330(8) Uani 1 1 d . . . H23A H 1.1082 0.9786 0.3598 0.040 Uiso 1 1 calc R . . C23B C 0.8640(3) 0.0020(2) 0.1944(2) 0.0353(9) Uani 1 1 d . . . H23B H 0.8561 -0.0264 0.1542 0.042 Uiso 1 1 calc R . . C24A C 1.0755(2) 0.8765(2) 0.31356(19) 0.0318(8) Uani 1 1 d . . . H24A H 1.0749 0.8459 0.3526 0.038 Uiso 1 1 calc R . . C24B C 0.8863(3) 0.0813(2) 0.1929(2) 0.0336(8) Uani 1 1 d . . . H24B H 0.8935 0.1062 0.1517 0.040 Uiso 1 1 calc R . . C25A C 1.1253(2) 1.0860(2) 0.2662(2) 0.0315(8) Uani 1 1 d . . . C25B C 0.8265(2) -0.1206(2) 0.2559(2) 0.0342(9) Uani 1 1 d . . . C26A C 1.1694(3) 1.1206(2) 0.2171(2) 0.0374(9) Uani 1 1 d . . . H26A H 1.1804 1.0911 0.1788 0.045 Uiso 1 1 calc R . . C26B C 0.8467(3) -0.1669(2) 0.3113(2) 0.0398(10) Uani 1 1 d . . . H26B H 0.8794 -0.1450 0.3474 0.048 Uiso 1 1 calc R . . C27A C 1.1977(3) 1.1977(2) 0.2230(2) 0.0422(10) Uani 1 1 d . . . H27A H 1.2283 1.2202 0.1890 0.051 Uiso 1 1 calc R . . C27B C 0.8199(3) -0.2445(2) 0.3146(2) 0.0433(11) Uani 1 1 d . . . H27B H 0.8337 -0.2751 0.3528 0.052 Uiso 1 1 calc R . . C28A C 1.1820(3) 1.2417(2) 0.2776(2) 0.0430(10) Uani 1 1 d . . . H28A H 1.2017 1.2943 0.2814 0.052 Uiso 1 1 calc R . . C28B C 0.7728(3) -0.2775(2) 0.2618(2) 0.0437(11) Uani 1 1 d . . . H28B H 0.7543 -0.3305 0.2636 0.052 Uiso 1 1 calc R . . C29A C 1.1373(3) 1.2090(2) 0.3270(2) 0.0406(10) Uani 1 1 d . . . H29A H 1.1259 1.2393 0.3647 0.049 Uiso 1 1 calc R . . C29B C 0.7534(3) -0.2324(2) 0.2070(2) 0.0426(10) Uani 1 1 d . . . H29B H 0.7211 -0.2546 0.1709 0.051 Uiso 1 1 calc R . . C30A C 1.1091(2) 1.1314(2) 0.3212(2) 0.0348(9) Uani 1 1 d . . . H30A H 1.0783 1.1092 0.3552 0.042 Uiso 1 1 calc R . . C30B C 0.7802(2) -0.1552(2) 0.2036(2) 0.0377(9) Uani 1 1 d . . . H30B H 0.7667 -0.1253 0.1649 0.045 Uiso 1 1 calc R . . N1A N 1.08275(19) 0.48734(16) 0.31498(14) 0.0258(6) Uani 1 1 d . . . N1B N 0.89993(18) 0.47978(15) 0.31207(14) 0.0238(6) Uani 1 1 d . . . N8A N 1.01199(17) 0.59513(16) 0.24178(13) 0.0219(6) Uani 1 1 d . . . N8B N 0.96121(18) 0.36713(15) 0.24473(13) 0.0222(6) Uani 1 1 d . . . N14A N 0.90127(19) 0.52022(16) 0.16930(14) 0.0247(6) Uani 1 1 d . . . N14B N 1.06608(19) 0.43574(16) 0.17254(14) 0.0281(6) Uani 1 1 d . . . B1 B 0.3335(5) 0.6566(3) 0.0192(3) 0.0586(16) Uani 1 1 d . . . B2 B 0.2626(4) 0.2603(3) 0.5063(3) 0.0528(14) Uani 1 1 d . . . F1 F 0.3023(3) 0.58640(19) 0.04055(15) 0.0936(13) Uani 1 1 d . . . F2 F 0.3454(3) 0.6505(2) -0.04650(18) 0.1104(16) Uani 1 1 d . . . F3 F 0.2762(3) 0.7166(2) 0.0296(2) 0.0925(12) Uani 1 1 d . . . F4 F 0.4055(2) 0.6753(3) 0.0559(2) 0.1046(14) Uani 1 1 d . . . F5 F 0.2356(3) 0.18145(18) 0.50370(18) 0.0892(12) Uani 1 1 d . . . F6 F 0.1959(2) 0.30579(19) 0.51593(16) 0.0746(9) Uani 1 1 d . . . F7 F 0.2990(2) 0.28066(17) 0.44692(13) 0.0632(8) Uani 1 1 d . . . F8 F 0.3218(3) 0.2659(3) 0.55820(17) 0.0967(13) Uani 1 1 d . . . C40 C 0.5282(4) 0.5338(5) -0.0073(3) 0.098(2) Uani 0.50 1 d P . 5 H40A H 0.5634 0.5468 0.0323 0.148 Uiso 0.50 1 calc PR . 5 H40B H 0.4941 0.5796 -0.0208 0.148 Uiso 0.50 1 calc PR . 5 H40C H 0.5639 0.5191 -0.0429 0.148 Uiso 0.50 1 calc PR . 5 N41 N 0.5282(4) 0.5338(5) -0.0073(3) 0.098(2) Uani 0.50 1 d P . . O42 O 0.5851(6) 0.5654(6) 0.0369(5) 0.086(3) Uani 0.50 1 d P . . O43 O 0.5199(9) 0.5772(8) -0.0618(4) 0.116(4) Uani 0.50 1 d P . . C50A C 1.0114(15) 0.2214(8) 0.5064(11) 0.159(9) Uiso 0.50 1 d PD A 1 H50A H 0.9551 0.1983 0.5033 0.239 Uiso 0.50 1 calc PR A 1 H50B H 1.0414 0.2038 0.5472 0.239 Uiso 0.50 1 calc PR A 1 H50C H 1.0421 0.2045 0.4685 0.239 Uiso 0.50 1 calc PR A 1 N51A N 1.0048(7) 0.3069(6) 0.5066(4) 0.079(2) Uiso 0.50 1 d PD A 1 O52A O 1.0006(5) 0.3341(5) 0.4518(4) 0.149(2) Uiso 0.50 1 d PD A 1 O53A O 1.0087(5) 0.3402(5) 0.5588(4) 0.157(3) Uiso 0.50 1 d PD A 1 C50B C 0.9979(12) 0.4537(7) 0.4998(9) 0.125(6) Uiso 0.50 1 d PD B 2 H50D H 0.9852 0.4757 0.5426 0.187 Uiso 0.50 1 calc PR B 2 H50E H 0.9545 0.4700 0.4664 0.187 Uiso 0.50 1 calc PR B 2 H50F H 1.0526 0.4730 0.4874 0.187 Uiso 0.50 1 calc PR B 2 N51B N 0.9997(7) 0.3700(6) 0.5039(4) 0.079(2) Uiso 0.50 1 d PD B 2 O52B O 1.0006(5) 0.3341(5) 0.4518(4) 0.149(2) Uiso 0.50 1 d PD B 2 O53B O 1.0087(5) 0.3402(5) 0.5588(4) 0.157(3) Uiso 0.50 1 d PD B 2 O60 O 0.531(2) 0.414(2) 0.5050(7) 0.196(13) Uani 0.33 1 d P . . O61 O 0.5738(16) 0.490(3) 0.4912(11) 0.212(18) Uani 0.33 1 d P . . O62 O 0.5000 0.5000 0.5000 0.172(19) Uani 0.33 2 d SP . . O70A O 0.1328(11) 0.7164(10) -0.0798(9) 0.168(4) Uiso 0.50 1 d PD C 3 N71A N 0.1048(13) 0.7485(11) -0.0332(9) 0.143(7) Uiso 0.50 1 d PD C 3 O72A O 0.1224(12) 0.8182(11) -0.0277(9) 0.179(6) Uiso 0.50 1 d PD C 3 C73A C 0.0796(17) 0.7248(18) 0.0317(10) 0.150(8) Uiso 0.50 1 d PD C 3 H73A H 0.0901 0.7681 0.0629 0.226 Uiso 0.50 1 calc PR C 3 H73B H 0.1120 0.6785 0.0467 0.226 Uiso 0.50 1 calc PR C 3 H73C H 0.0197 0.7118 0.0290 0.226 Uiso 0.50 1 calc PR C 3 O70B O 0.0735(11) 0.6192(10) -0.0190(8) 0.168(4) Uiso 0.50 1 d PD D 4 N71B N 0.0799(9) 0.6740(8) 0.0187(8) 0.101(4) Uiso 0.50 1 d PD D 4 O72B O 0.0775(17) 0.6468(15) 0.0740(9) 0.264(11) Uiso 0.50 1 d PD D 4 C73B C 0.0906(11) 0.7569(7) 0.0046(10) 0.090(4) Uiso 0.50 1 d PD D 4 H73D H 0.0357 0.7809 -0.0060 0.135 Uiso 0.50 1 calc PR D 4 H73E H 0.1258 0.7628 -0.0330 0.135 Uiso 0.50 1 calc PR D 4 H73F H 0.1176 0.7830 0.0433 0.135 Uiso 0.50 1 calc PR D 4 O80 O -0.004(4) 0.5025(14) -0.007(3) 0.168(14) Uiso 0.17 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02905(16) 0.01221(14) 0.02661(15) 0.00108(10) 0.00296(11) -0.00137(10) C2A 0.040(2) 0.0195(17) 0.039(2) 0.0082(15) 0.0035(17) 0.0057(15) C2B 0.038(2) 0.0159(16) 0.038(2) -0.0023(14) 0.0051(16) 0.0003(14) C3A 0.048(2) 0.030(2) 0.038(2) 0.0118(17) -0.0014(18) 0.0092(17) C3B 0.048(2) 0.0260(19) 0.040(2) -0.0090(16) 0.0102(19) 0.0052(16) C4A 0.036(2) 0.040(2) 0.034(2) 0.0050(17) -0.0033(17) 0.0054(17) C4B 0.038(2) 0.036(2) 0.0317(19) -0.0048(16) 0.0101(17) -0.0027(16) C5A 0.034(2) 0.0288(19) 0.0287(18) -0.0023(14) 0.0018(15) -0.0010(15) C5B 0.037(2) 0.0211(17) 0.0301(18) -0.0003(14) 0.0012(15) -0.0041(14) C6A 0.0307(18) 0.0185(16) 0.0275(17) 0.0004(13) 0.0074(14) 0.0007(13) C6B 0.0276(17) 0.0161(15) 0.0255(16) -0.0006(12) -0.0007(14) -0.0019(13) C7A 0.0237(17) 0.0178(15) 0.0240(16) 0.0010(12) 0.0023(13) 0.0006(12) C7B 0.0249(17) 0.0162(15) 0.0247(16) 0.0014(12) 0.0004(13) -0.0003(12) C9A 0.0258(17) 0.0164(15) 0.0267(16) 0.0001(13) 0.0033(14) -0.0023(12) C9B 0.0275(17) 0.0166(15) 0.0278(17) 0.0020(13) 0.0019(14) 0.0019(12) C10A 0.0291(18) 0.0177(16) 0.0293(18) 0.0029(13) 0.0027(14) 0.0013(13) C10B 0.0316(19) 0.0161(16) 0.0328(18) -0.0032(13) 0.0047(15) 0.0013(13) C11A 0.0272(18) 0.0157(15) 0.0311(17) 0.0001(13) 0.0058(14) -0.0011(13) C11B 0.0284(18) 0.0146(15) 0.0351(19) 0.0012(13) 0.0012(15) -0.0002(13) C12A 0.0278(18) 0.0186(16) 0.0293(17) -0.0018(13) 0.0014(14) -0.0024(13) C12B 0.0278(18) 0.0164(15) 0.0316(18) 0.0025(13) 0.0033(14) -0.0011(13) C13A 0.0277(18) 0.0182(16) 0.0255(16) 0.0005(13) 0.0044(14) -0.0034(13) C13B 0.0302(18) 0.0176(16) 0.0300(17) 0.0018(13) 0.0036(15) -0.0019(13) C15A 0.039(2) 0.0210(17) 0.0297(18) -0.0007(14) 0.0000(16) -0.0082(15) C15B 0.052(3) 0.027(2) 0.045(2) 0.0011(17) 0.018(2) -0.0109(17) C16A 0.042(2) 0.038(2) 0.031(2) -0.0023(16) -0.0047(17) -0.0131(17) C16B 0.065(3) 0.039(2) 0.057(3) 0.002(2) 0.034(2) -0.012(2) C17A 0.037(2) 0.037(2) 0.0281(18) 0.0039(16) -0.0052(16) -0.0026(16) C17B 0.060(3) 0.037(2) 0.051(3) -0.0030(19) 0.029(2) -0.002(2) C18A 0.035(2) 0.0240(17) 0.0306(18) 0.0054(14) 0.0009(15) -0.0011(14) C18B 0.046(2) 0.0246(19) 0.038(2) -0.0020(15) 0.0149(18) -0.0009(16) C19A 0.0264(18) 0.0157(16) 0.0387(19) -0.0005(14) 0.0021(15) 0.0005(13) C19B 0.0305(19) 0.0144(16) 0.042(2) 0.0003(14) 0.0075(16) -0.0016(13) C20A 0.041(2) 0.0192(17) 0.0352(19) -0.0011(14) -0.0015(17) -0.0027(15) C20B 0.049(2) 0.0168(17) 0.041(2) -0.0012(15) 0.0123(18) -0.0007(15) C21A 0.041(2) 0.0186(17) 0.040(2) 0.0069(15) 0.0000(17) -0.0024(15) C21B 0.051(2) 0.0187(17) 0.042(2) 0.0035(15) 0.0158(19) -0.0049(16) C22A 0.032(2) 0.0142(15) 0.046(2) -0.0018(14) -0.0007(17) -0.0003(13) C22B 0.035(2) 0.0161(16) 0.050(2) 0.0003(15) 0.0122(18) -0.0004(14) C23A 0.040(2) 0.0200(17) 0.038(2) -0.0053(15) -0.0010(17) -0.0036(15) C23B 0.044(2) 0.0184(17) 0.044(2) -0.0019(15) 0.0053(18) -0.0066(15) C24A 0.042(2) 0.0185(17) 0.0348(19) 0.0005(14) 0.0049(17) -0.0021(15) C24B 0.042(2) 0.0167(17) 0.042(2) 0.0017(15) 0.0046(18) -0.0027(15) C25A 0.0283(19) 0.0156(16) 0.050(2) 0.0008(15) -0.0046(17) -0.0006(13) C25B 0.034(2) 0.0181(17) 0.053(2) -0.0016(16) 0.0200(18) -0.0017(14) C26A 0.036(2) 0.0229(18) 0.053(2) -0.0003(17) 0.0022(18) -0.0010(15) C26B 0.046(2) 0.0212(18) 0.054(2) -0.0011(17) 0.018(2) -0.0008(16) C27A 0.035(2) 0.0221(18) 0.070(3) 0.0107(19) 0.002(2) -0.0044(16) C27B 0.049(3) 0.0192(18) 0.065(3) 0.0070(18) 0.027(2) 0.0046(17) C28A 0.038(2) 0.0166(18) 0.073(3) -0.0015(19) -0.009(2) -0.0025(15) C28B 0.040(2) 0.0179(17) 0.075(3) 0.0002(19) 0.025(2) -0.0042(16) C29A 0.038(2) 0.0200(18) 0.062(3) -0.0055(18) -0.011(2) 0.0026(16) C29B 0.036(2) 0.0235(19) 0.070(3) -0.0068(19) 0.017(2) -0.0043(16) C30A 0.036(2) 0.0185(17) 0.048(2) -0.0007(15) -0.0059(18) 0.0002(14) C30B 0.035(2) 0.0218(18) 0.058(3) -0.0017(17) 0.0144(19) -0.0017(15) N1A 0.0316(16) 0.0169(14) 0.0295(15) 0.0015(11) 0.0061(13) 0.0015(11) N1B 0.0292(15) 0.0162(13) 0.0260(14) -0.0005(11) 0.0018(12) 0.0018(11) N8A 0.0255(14) 0.0151(13) 0.0253(14) 0.0014(10) 0.0046(12) 0.0005(10) N8B 0.0277(15) 0.0139(13) 0.0249(14) 0.0002(10) 0.0012(12) -0.0006(11) N14A 0.0297(15) 0.0173(14) 0.0272(14) 0.0016(11) 0.0023(12) -0.0025(11) N14B 0.0353(17) 0.0194(14) 0.0300(15) 0.0024(12) 0.0059(13) -0.0032(12) B1 0.090(5) 0.029(3) 0.055(3) -0.011(2) -0.006(3) -0.011(3) B2 0.077(4) 0.042(3) 0.038(3) -0.001(2) -0.002(3) 0.022(3) F1 0.178(4) 0.0459(18) 0.0548(18) 0.0036(14) -0.009(2) -0.032(2) F2 0.210(5) 0.061(2) 0.062(2) -0.0017(17) 0.028(3) -0.037(3) F3 0.092(3) 0.057(2) 0.126(3) -0.019(2) -0.020(2) 0.0095(18) F4 0.074(2) 0.112(3) 0.127(3) -0.053(3) -0.009(2) 0.000(2) F5 0.149(4) 0.0421(18) 0.077(2) -0.0019(16) 0.012(2) 0.0046(19) F6 0.093(2) 0.0570(19) 0.076(2) 0.0137(16) 0.0239(19) 0.0230(17) F7 0.096(2) 0.0491(16) 0.0458(15) -0.0017(12) 0.0110(15) 0.0194(15) F8 0.106(3) 0.120(3) 0.060(2) 0.022(2) -0.028(2) -0.025(2) C40 0.077(4) 0.149(7) 0.071(4) -0.002(4) 0.013(3) 0.006(4) N41 0.077(4) 0.149(7) 0.071(4) -0.002(4) 0.013(3) 0.006(4) O42 0.067(5) 0.090(7) 0.099(7) -0.030(5) -0.016(5) -0.002(5) O43 0.154(10) 0.147(11) 0.049(5) 0.004(6) 0.020(6) -0.030(8) O60 0.31(3) 0.26(3) 0.023(7) 0.029(12) 0.048(12) 0.10(3) O61 0.114(18) 0.45(5) 0.075(13) 0.14(2) 0.015(12) -0.01(2) O62 0.31(6) 0.18(3) 0.043(13) 0.006(18) 0.09(3) -0.04(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N8B 1.978(3) . ? Ru1 N8A 1.980(3) . ? Ru1 N1A 2.063(3) . ? Ru1 N1B 2.064(3) . ? Ru1 N14A 2.071(3) . ? Ru1 N14B 2.081(3) . ? C2A N1A 1.343(4) . ? C2A C3A 1.373(6) . ? C2B N1B 1.344(4) . ? C2B C3B 1.378(5) . ? C3A C4A 1.384(6) . ? C3B C4B 1.381(5) . ? C4A C5A 1.380(5) . ? C4B C5B 1.383(5) . ? C5A C6A 1.380(5) . ? C5B C6B 1.381(5) . ? C6A N1A 1.375(4) . ? C6A C7A 1.478(5) . ? C6B N1B 1.375(4) . ? C6B C7B 1.475(4) . ? C7A N8A 1.348(4) . ? C7A C12A 1.385(5) . ? C7B N8B 1.353(4) . ? C7B C12B 1.388(4) . ? C9A N8A 1.357(4) . ? C9A C10A 1.389(5) . ? C9A C13A 1.469(5) . ? C9B N8B 1.351(4) . ? C9B C10B 1.388(5) . ? C9B C13B 1.480(5) . ? C10A C11A 1.400(5) . ? C10B C11B 1.400(5) . ? C11A C12A 1.399(5) . ? C11A C19A 1.482(4) . ? C11B C12B 1.402(5) . ? C11B C19B 1.483(4) . ? C13A N14A 1.372(4) . ? C13A C18A 1.392(5) . ? C13B N14B 1.371(4) . ? C13B C18B 1.380(5) . ? C15A N14A 1.345(5) . ? C15A C16A 1.379(6) . ? C15B N14B 1.340(5) . ? C15B C16B 1.375(6) . ? C16A C17A 1.381(5) . ? C16B C17B 1.375(6) . ? C17A C18A 1.387(5) . ? C17B C18B 1.383(6) . ? C19A C20A 1.391(5) . ? C19A C24A 1.393(5) . ? C19B C20B 1.391(5) . ? C19B C24B 1.393(5) . ? C20A C21A 1.386(5) . ? C20B C21B 1.386(5) . ? C21A C22A 1.396(6) . ? C21B C22B 1.393(6) . ? C22A C23A 1.393(5) . ? C22A C25A 1.492(5) . ? C22B C23B 1.389(6) . ? C22B C25B 1.497(5) . ? C23A C24A 1.381(5) . ? C23B C24B 1.395(5) . ? C25A C26A 1.386(6) . ? C25A C30A 1.395(6) . ? C25B C30B 1.389(6) . ? C25B C26B 1.396(6) . ? C26A C27A 1.388(5) . ? C26B C27B 1.389(5) . ? C27A C28A 1.374(6) . ? C27B C28B 1.391(7) . ? C28A C29A 1.381(6) . ? C28B C29B 1.371(7) . ? C29A C30A 1.396(5) . ? C29B C30B 1.383(5) . ? B1 F2 1.365(7) . ? B1 F4 1.370(7) . ? B1 F1 1.373(6) . ? B1 F3 1.393(7) . ? B2 F6 1.340(6) . ? B2 F8 1.376(7) . ? B2 F5 1.408(7) . ? B2 F7 1.414(6) . ? C40 N41 1.499(15) 3_665 ? C50A N51A 1.456(9) . ? N51A O53A 1.201(8) . ? N51A O52A 1.204(8) . ? C50B N51B 1.424(9) . ? O60 O61 1.50(5) . ? O60 O62 1.55(3) . ? O61 O62 1.21(3) . ? O62 O61 1.21(3) 3_666 ? O62 O60 1.55(3) 3_666 ? O70A N71A 1.201(9) . ? N71A O72A 1.220(9) . ? N71A C73A 1.459(10) . ? O70B N71B 1.206(9) . ? N71B O72B 1.219(10) . ? N71B C73B 1.448(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8B Ru1 N8A 177.74(11) . . ? N8B Ru1 N1A 100.42(11) . . ? N8A Ru1 N1A 79.19(11) . . ? N8B Ru1 N1B 79.25(11) . . ? N8A Ru1 N1B 98.51(11) . . ? N1A Ru1 N1B 90.09(11) . . ? N8B Ru1 N14A 101.60(11) . . ? N8A Ru1 N14A 78.74(11) . . ? N1A Ru1 N14A 157.92(11) . . ? N1B Ru1 N14A 92.35(11) . . ? N8B Ru1 N14B 78.55(11) . . ? N8A Ru1 N14B 103.69(11) . . ? N1A Ru1 N14B 93.63(12) . . ? N1B Ru1 N14B 157.80(11) . . ? N14A Ru1 N14B 92.35(12) . . ? N1A C2A C3A 123.4(3) . . ? N1B C2B C3B 123.1(3) . . ? C2A C3A C4A 118.6(3) . . ? C2B C3B C4B 118.8(3) . . ? C5A C4A C3A 119.5(4) . . ? C3B C4B C5B 119.4(4) . . ? C4A C5A C6A 119.2(4) . . ? C6B C5B C4B 119.4(3) . . ? N1A C6A C5A 121.7(3) . . ? N1A C6A C7A 114.4(3) . . ? C5A C6A C7A 123.9(3) . . ? N1B C6B C5B 121.4(3) . . ? N1B C6B C7B 114.6(3) . . ? C5B C6B C7B 124.0(3) . . ? N8A C7A C12A 120.4(3) . . ? N8A C7A C6A 113.2(3) . . ? C12A C7A C6A 126.4(3) . . ? N8B C7B C12B 120.3(3) . . ? N8B C7B C6B 113.1(3) . . ? C12B C7B C6B 126.5(3) . . ? N8A C9A C10A 120.0(3) . . ? N8A C9A C13A 112.5(3) . . ? C10A C9A C13A 127.5(3) . . ? N8B C9B C10B 120.5(3) . . ? N8B C9B C13B 112.3(3) . . ? C10B C9B C13B 127.2(3) . . ? C9A C10A C11A 119.6(3) . . ? C9B C10B C11B 119.5(3) . . ? C12A C11A C10A 118.7(3) . . ? C12A C11A C19A 119.1(3) . . ? C10A C11A C19A 122.2(3) . . ? C10B C11B C12B 118.7(3) . . ? C10B C11B C19B 121.2(3) . . ? C12B C11B C19B 120.0(3) . . ? C7A C12A C11A 119.7(3) . . ? C7B C12B C11B 119.5(3) . . ? N14A C13A C18A 121.1(3) . . ? N14A C13A C9A 115.1(3) . . ? C18A C13A C9A 123.7(3) . . ? N14B C13B C18B 121.3(3) . . ? N14B C13B C9B 115.0(3) . . ? C18B C13B C9B 123.7(3) . . ? N14A C15A C16A 122.9(3) . . ? N14B C15B C16B 123.0(4) . . ? C15A C16A C17A 119.0(4) . . ? C15B C16B C17B 119.1(4) . . ? C16A C17A C18A 119.4(4) . . ? C16B C17B C18B 119.1(4) . . ? C17A C18A C13A 119.3(3) . . ? C13B C18B C17B 119.5(4) . . ? C20A C19A C24A 118.3(3) . . ? C20A C19A C11A 121.4(3) . . ? C24A C19A C11A 120.3(3) . . ? C20B C19B C24B 118.4(3) . . ? C20B C19B C11B 120.8(3) . . ? C24B C19B C11B 120.8(3) . . ? C21A C20A C19A 121.1(3) . . ? C21B C20B C19B 120.4(4) . . ? C20A C21A C22A 120.6(4) . . ? C20B C21B C22B 121.8(4) . . ? C23A C22A C21A 118.1(3) . . ? C23A C22A C25A 120.7(3) . . ? C21A C22A C25A 121.2(3) . . ? C23B C22B C21B 117.7(3) . . ? C23B C22B C25B 121.5(4) . . ? C21B C22B C25B 120.8(4) . . ? C24A C23A C22A 121.2(4) . . ? C22B C23B C24B 121.0(4) . . ? C23A C24A C19A 120.7(3) . . ? C19B C24B C23B 120.8(4) . . ? C26A C25A C30A 118.0(3) . . ? C26A C25A C22A 120.9(4) . . ? C30A C25A C22A 121.1(4) . . ? C30B C25B C26B 117.8(3) . . ? C30B C25B C22B 121.5(4) . . ? C26B C25B C22B 120.7(4) . . ? C25A C26A C27A 120.9(4) . . ? C27B C26B C25B 121.1(4) . . ? C28A C27A C26A 120.5(4) . . ? C26B C27B C28B 119.9(4) . . ? C27A C28A C29A 119.8(4) . . ? C29B C28B C27B 119.2(4) . . ? C28A C29A C30A 119.7(4) . . ? C28B C29B C30B 121.0(4) . . ? C25A C30A C29A 121.0(4) . . ? C29B C30B C25B 121.0(4) . . ? C2A N1A C6A 117.5(3) . . ? C2A N1A Ru1 128.2(3) . . ? C6A N1A Ru1 114.2(2) . . ? C2B N1B C6B 117.9(3) . . ? C2B N1B Ru1 128.0(2) . . ? C6B N1B Ru1 114.1(2) . . ? C7A N8A C9A 121.5(3) . . ? C7A N8A Ru1 118.8(2) . . ? C9A N8A Ru1 119.5(2) . . ? C9B N8B C7B 121.4(3) . . ? C9B N8B Ru1 119.9(2) . . ? C7B N8B Ru1 118.7(2) . . ? C15A N14A C13A 118.3(3) . . ? C15A N14A Ru1 127.4(2) . . ? C13A N14A Ru1 114.2(2) . . ? C15B N14B C13B 118.0(3) . . ? C15B N14B Ru1 128.0(3) . . ? C13B N14B Ru1 114.0(2) . . ? F2 B1 F4 112.8(6) . . ? F2 B1 F1 108.4(4) . . ? F4 B1 F1 109.8(5) . . ? F2 B1 F3 109.6(5) . . ? F4 B1 F3 106.7(4) . . ? F1 B1 F3 109.5(6) . . ? F6 B2 F8 111.4(4) . . ? F6 B2 F5 108.0(5) . . ? F8 B2 F5 106.9(4) . . ? F6 B2 F7 110.8(4) . . ? F8 B2 F7 109.8(5) . . ? F5 B2 F7 109.9(4) . . ? O53A N51A O52A 129.4(10) . . ? O53A N51A C50A 118.2(12) . . ? O52A N51A C50A 112.3(12) . . ? O61 O60 O62 46.8(18) . . ? O62 O61 O60 68.8(16) . . ? O61 O62 O61 180.000(5) . 3_666 ? O61 O62 O60 116(2) . 3_666 ? O61 O62 O60 64(2) 3_666 3_666 ? O61 O62 O60 64(2) . . ? O61 O62 O60 116(2) 3_666 . ? O60 O62 O60 180.000(9) 3_666 . ? O70A N71A O72A 115(2) . . ? O70A N71A C73A 136(2) . . ? O72A N71A C73A 105(2) . . ? O70B N71B O72B 106.7(18) . . ? O70B N71B C73B 129.1(17) . . ? O72B N71B C73B 124(2) . . ? 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 N1A C2A C3A C4A 1.1(6) . . . . ? N1B C2B C3B C4B 0.7(6) . . . . ? C2A C3A C4A C5A 0.3(6) . . . . ? C2B C3B C4B C5B 0.8(6) . . . . ? C3A C4A C5A C6A -1.5(6) . . . . ? C3B C4B C5B C6B -2.3(6) . . . . ? C4A C5A C6A N1A 1.6(5) . . . . ? C4A C5A C6A C7A -179.2(3) . . . . ? C4B C5B C6B N1B 2.3(5) . . . . ? C4B C5B C6B C7B -175.9(3) . . . . ? N1A C6A C7A N8A -1.7(4) . . . . ? C5A C6A C7A N8A 179.0(3) . . . . ? N1A C6A C7A C12A 177.8(3) . . . . ? C5A C6A C7A C12A -1.5(6) . . . . ? N1B C6B C7B N8B -0.5(4) . . . . ? C5B C6B C7B N8B 177.8(3) . . . . ? N1B C6B C7B C12B -177.0(3) . . . . ? C5B C6B C7B C12B 1.3(6) . . . . ? N8A C9A C10A C11A -2.2(5) . . . . ? C13A C9A C10A C11A 174.6(3) . . . . ? N8B C9B C10B C11B -2.6(5) . . . . ? C13B C9B C10B C11B 175.2(3) . . . . ? C9A C10A C11A C12A 0.3(5) . . . . ? C9A C10A C11A C19A 179.6(3) . . . . ? C9B C10B C11B C12B -0.3(5) . . . . ? C9B C10B C11B C19B 179.1(3) . . . . ? N8A C7A C12A C11A -1.6(5) . . . . ? C6A C7A C12A C11A 179.0(3) . . . . ? C10A C11A C12A C7A 1.6(5) . . . . ? C19A C11A C12A C7A -177.7(3) . . . . ? N8B C7B C12B C11B -3.3(5) . . . . ? C6B C7B C12B C11B 173.0(3) . . . . ? C10B C11B C12B C7B 3.1(5) . . . . ? C19B C11B C12B C7B -176.2(3) . . . . ? N8A C9A C13A N14A 0.7(4) . . . . ? C10A C9A C13A N14A -176.3(3) . . . . ? N8A C9A C13A C18A 177.8(3) . . . . ? C10A C9A C13A C18A 0.8(6) . . . . ? N8B C9B C13B N14B 0.4(4) . . . . ? C10B C9B C13B N14B -177.6(3) . . . . ? N8B C9B C13B C18B 178.4(3) . . . . ? C10B C9B C13B C18B 0.5(6) . . . . ? N14A C15A C16A C17A 1.8(6) . . . . ? N14B C15B C16B C17B 0.6(8) . . . . ? C15A C16A C17A C18A -0.4(6) . . . . ? C15B C16B C17B C18B -0.1(8) . . . . ? C16A C17A C18A C13A -1.1(6) . . . . ? N14A C13A C18A C17A 1.3(5) . . . . ? C9A C13A C18A C17A -175.7(3) . . . . ? N14B C13B C18B C17B 2.4(6) . . . . ? C9B C13B C18B C17B -175.5(4) . . . . ? C16B C17B C18B C13B -1.4(7) . . . . ? C12A C11A C19A C20A 143.2(4) . . . . ? C10A C11A C19A C20A -36.1(5) . . . . ? C12A C11A C19A C24A -34.5(5) . . . . ? C10A C11A C19A C24A 146.2(4) . . . . ? C10B C11B C19B C20B 144.3(4) . . . . ? C12B C11B C19B C20B -36.4(5) . . . . ? C10B C11B C19B C24B -35.9(5) . . . . ? C12B C11B C19B C24B 143.5(4) . . . . ? C24A C19A C20A C21A 2.1(6) . . . . ? C11A C19A C20A C21A -175.6(4) . . . . ? C24B C19B C20B C21B 1.1(6) . . . . ? C11B C19B C20B C21B -179.0(4) . . . . ? C19A C20A C21A C22A -1.3(6) . . . . ? C19B C20B C21B C22B -1.8(6) . . . . ? C20A C21A C22A C23A -0.6(6) . . . . ? C20A C21A C22A C25A 177.8(4) . . . . ? C20B C21B C22B C23B 1.4(6) . . . . ? C20B C21B C22B C25B -177.1(4) . . . . ? C21A C22A C23A C24A 1.8(6) . . . . ? C25A C22A C23A C24A -176.6(4) . . . . ? C21B C22B C23B C24B -0.5(6) . . . . ? C25B C22B C23B C24B 178.1(4) . . . . ? C22A C23A C24A C19A -1.1(6) . . . . ? C20A C19A C24A C23A -0.9(6) . . . . ? C11A C19A C24A C23A 176.8(4) . . . . ? C20B C19B C24B C23B -0.2(6) . . . . ? C11B C19B C24B C23B 179.9(4) . . . . ? C22B C23B C24B C19B -0.1(6) . . . . ? C23A C22A C25A C26A 146.1(4) . . . . ? C21A C22A C25A C26A -32.3(6) . . . . ? C23A C22A C25A C30A -31.8(5) . . . . ? C21A C22A C25A C30A 149.8(4) . . . . ? C23B C22B C25B C30B -26.4(6) . . . . ? C21B C22B C25B C30B 152.1(4) . . . . ? C23B C22B C25B C26B 154.5(4) . . . . ? C21B C22B C25B C26B -27.0(6) . . . . ? C30A C25A C26A C27A 1.1(6) . . . . ? C22A C25A C26A C27A -176.8(4) . . . . ? C30B C25B C26B C27B -1.3(6) . . . . ? C22B C25B C26B C27B 177.8(4) . . . . ? C25A C26A C27A C28A -0.6(6) . . . . ? C25B C26B C27B C28B 0.6(6) . . . . ? C26A C27A C28A C29A -0.2(6) . . . . ? C26B C27B C28B C29B -0.1(6) . . . . ? C27A C28A C29A C30A 0.5(6) . . . . ? C27B C28B C29B C30B 0.2(6) . . . . ? C26A C25A C30A C29A -0.8(6) . . . . ? C22A C25A C30A C29A 177.1(4) . . . . ? C28A C29A C30A C25A 0.0(6) . . . . ? C28B C29B C30B C25B -0.9(6) . . . . ? C26B C25B C30B C29B 1.5(6) . . . . ? C22B C25B C30B C29B -177.7(4) . . . . ? C3A C2A N1A C6A -1.1(5) . . . . ? C3A C2A N1A Ru1 -178.6(3) . . . . ? C5A C6A N1A C2A -0.3(5) . . . . ? C7A C6A N1A C2A -179.6(3) . . . . ? C5A C6A N1A Ru1 177.6(3) . . . . ? C7A C6A N1A Ru1 -1.7(4) . . . . ? N8B Ru1 N1A C2A 3.1(3) . . . . ? N8A Ru1 N1A C2A -179.2(3) . . . . ? N1B Ru1 N1A C2A 82.1(3) . . . . ? N14A Ru1 N1A C2A 178.6(3) . . . . ? N14B Ru1 N1A C2A -76.0(3) . . . . ? N8B Ru1 N1A C6A -174.6(2) . . . . ? N8A Ru1 N1A C6A 3.2(2) . . . . ? N1B Ru1 N1A C6A -95.5(2) . . . . ? N14A Ru1 N1A C6A 1.0(4) . . . . ? N14B Ru1 N1A C6A 106.4(2) . . . . ? C3B C2B N1B C6B -0.6(6) . . . . ? C3B C2B N1B Ru1 -179.6(3) . . . . ? C5B C6B N1B C2B -0.9(5) . . . . ? C7B C6B N1B C2B 177.5(3) . . . . ? C5B C6B N1B Ru1 178.2(3) . . . . ? C7B C6B N1B Ru1 -3.4(4) . . . . ? N8B Ru1 N1B C2B -176.5(3) . . . . ? N8A Ru1 N1B C2B 3.8(3) . . . . ? N1A Ru1 N1B C2B 82.9(3) . . . . ? N14A Ru1 N1B C2B -75.2(3) . . . . ? N14B Ru1 N1B C2B -177.3(3) . . . . ? N8B Ru1 N1B C6B 4.4(2) . . . . ? N8A Ru1 N1B C6B -175.2(2) . . . . ? N1A Ru1 N1B C6B -96.2(2) . . . . ? N14A Ru1 N1B C6B 105.8(2) . . . . ? N14B Ru1 N1B C6B 3.7(5) . . . . ? C12A C7A N8A C9A -0.3(5) . . . . ? C6A C7A N8A C9A 179.2(3) . . . . ? C12A C7A N8A Ru1 -174.9(2) . . . . ? C6A C7A N8A Ru1 4.6(4) . . . . ? C10A C9A N8A C7A 2.2(5) . . . . ? C13A C9A N8A C7A -175.0(3) . . . . ? C10A C9A N8A Ru1 176.8(2) . . . . ? C13A C9A N8A Ru1 -0.5(4) . . . . ? N8B Ru1 N8A C7A 76(3) . . . . ? N1A Ru1 N8A C7A -4.4(2) . . . . ? N1B Ru1 N8A C7A 84.1(2) . . . . ? N14A Ru1 N8A C7A 174.8(3) . . . . ? N14B Ru1 N8A C7A -95.5(2) . . . . ? N8B Ru1 N8A C9A -99(3) . . . . ? N1A Ru1 N8A C9A -179.0(3) . . . . ? N1B Ru1 N8A C9A -90.6(3) . . . . ? N14A Ru1 N8A C9A 0.2(2) . . . . ? N14B Ru1 N8A C9A 89.8(3) . . . . ? C10B C9B N8B C7B 2.5(5) . . . . ? C13B C9B N8B C7B -175.5(3) . . . . ? C10B C9B N8B Ru1 -178.3(3) . . . . ? C13B C9B N8B Ru1 3.6(4) . . . . ? C12B C7B N8B C9B 0.4(5) . . . . ? C6B C7B N8B C9B -176.3(3) . . . . ? C12B C7B N8B Ru1 -178.7(2) . . . . ? C6B C7B N8B Ru1 4.5(4) . . . . ? N8A Ru1 N8B C9B -176(35) . . . . ? N1A Ru1 N8B C9B -96.1(3) . . . . ? N1B Ru1 N8B C9B 175.8(3) . . . . ? N14A Ru1 N8B C9B 85.6(3) . . . . ? N14B Ru1 N8B C9B -4.4(3) . . . . ? N8A Ru1 N8B C7B 3(3) . . . . ? N1A Ru1 N8B C7B 83.1(3) . . . . ? N1B Ru1 N8B C7B -5.0(2) . . . . ? N14A Ru1 N8B C7B -95.2(3) . . . . ? N14B Ru1 N8B C7B 174.8(3) . . . . ? C16A C15A N14A C13A -1.7(5) . . . . ? C16A C15A N14A Ru1 175.8(3) . . . . ? C18A C13A N14A C15A 0.1(5) . . . . ? C9A C13A N14A C15A 177.3(3) . . . . ? C18A C13A N14A Ru1 -177.7(3) . . . . ? C9A C13A N14A Ru1 -0.6(4) . . . . ? N8B Ru1 N14A C15A 0.3(3) . . . . ? N8A Ru1 N14A C15A -177.4(3) . . . . ? N1A Ru1 N14A C15A -175.2(3) . . . . ? N1B Ru1 N14A C15A -79.2(3) . . . . ? N14B Ru1 N14A C15A 79.1(3) . . . . ? N8B Ru1 N14A C13A 178.0(2) . . . . ? N8A Ru1 N14A C13A 0.2(2) . . . . ? N1A Ru1 N14A C13A 2.4(4) . . . . ? N1B Ru1 N14A C13A 98.4(2) . . . . ? N14B Ru1 N14A C13A -103.3(2) . . . . ? C16B C15B N14B C13B 0.4(7) . . . . ? C16B C15B N14B Ru1 -179.6(4) . . . . ? C18B C13B N14B C15B -1.9(6) . . . . ? C9B C13B N14B C15B 176.2(3) . . . . ? C18B C13B N14B Ru1 178.1(3) . . . . ? C9B C13B N14B Ru1 -3.8(4) . . . . ? N8B Ru1 N14B C15B -175.6(4) . . . . ? N8A Ru1 N14B C15B 4.0(4) . . . . ? N1A Ru1 N14B C15B -75.7(4) . . . . ? N1B Ru1 N14B C15B -174.9(3) . . . . ? N14A Ru1 N14B C15B 83.0(4) . . . . ? N8B Ru1 N14B C13B 4.3(2) . . . . ? N8A Ru1 N14B C13B -176.0(2) . . . . ? N1A Ru1 N14B C13B 104.2(3) . . . . ? N1B Ru1 N14B C13B 5.1(5) . . . . ? N14A Ru1 N14B C13B -97.0(3) . . . . ? O60 O61 O62 O61 -16(100) . . . 3_666 ? O60 O61 O62 O60 180.000(3) . . . 3_666 ? O61 O60 O62 O61 180.000(5) . . . 3_666 ? O61 O60 O62 O60 -160(100) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.164 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.096 data_mh002 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58.50 H46 Cu F12 N7 O2.50 P2' _chemical_formula_weight 1240.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.304(2) _cell_length_b 17.2230(10) _cell_length_c 16.6490(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.910(10) _cell_angle_gamma 90.00 _cell_volume 11475.8(11) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5064 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8798 _exptl_absorpt_correction_T_max 0.8798 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32236 _diffrn_reflns_av_R_equivalents 0.1248 _diffrn_reflns_av_sigmaI/netI 0.1806 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.83 _reflns_number_total 13541 _reflns_number_gt 6103 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 13541 _refine_ls_number_parameters 701 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.2670 _refine_ls_R_factor_gt 0.1542 _refine_ls_wR_factor_ref 0.4410 _refine_ls_wR_factor_gt 0.3900 _refine_ls_goodness_of_fit_ref 1.274 _refine_ls_restrained_S_all 1.377 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.86706(3) -0.24025(6) -0.14545(7) 0.0359(4) Uani 1 1 d . . . P1 P -1.0000 0.0000 0.0000 0.0341(8) Uani 1 2 d S . . P2 P -1.0000 -0.5000 -0.5000 0.0388(9) Uani 1 2 d S . . F1 F -0.96386(14) 0.0218(3) -0.0059(4) 0.0496(15) Uani 1 1 d . . . F2 F -0.98518(15) -0.0783(3) 0.0492(4) 0.0549(16) Uani 1 1 d . . . F3 F -1.00866(17) -0.0451(4) -0.0873(4) 0.0616(18) Uani 1 1 d . . . F4 F -0.96391(15) -0.5208(4) -0.4325(4) 0.0582(17) Uani 1 1 d . . . F5 F -1.00574(17) -0.4370(4) -0.4366(4) 0.0608(18) Uani 1 1 d . . . F6 F -0.98305(16) -0.4354(4) -0.5412(4) 0.0604(17) Uani 1 1 d . . . N1A N -0.8261(2) -0.2924(5) -0.0348(6) 0.053(2) Uani 1 1 d . . . N1B N -0.83409(19) -0.1976(4) -0.2024(5) 0.0377(19) Uani 1 1 d . . . N8A N -0.86842(18) -0.3538(4) -0.1733(5) 0.0310(17) Uani 1 1 d . . . N8B N -0.86789(17) -0.1315(4) -0.1223(5) 0.0313(17) Uani 1 1 d . . . N14A N -0.90777(19) -0.2476(4) -0.2742(5) 0.0360(18) Uani 1 1 d . . . N14B N -0.9019(2) -0.2393(4) -0.0819(5) 0.0371(18) Uani 1 1 d . . . C2A C -0.8066(4) -0.2555(7) 0.0359(9) 0.076(4) Uani 1 1 d . . . H2A H -0.8092 -0.2013 0.0421 0.091 Uiso 1 1 calc R . . C2B C -0.8187(3) -0.2382(6) -0.2488(7) 0.048(3) Uani 1 1 d . . . H2B H -0.8217 -0.2929 -0.2528 0.057 Uiso 1 1 calc R . . C3A C -0.7831(4) -0.2958(8) 0.0985(9) 0.091(5) Uani 1 1 d . . . H3A H -0.7685 -0.2688 0.1458 0.109 Uiso 1 1 calc R . . C3B C -0.7988(3) -0.2035(6) -0.2908(8) 0.053(3) Uani 1 1 d . . . H3B H -0.7887 -0.2337 -0.3235 0.063 Uiso 1 1 calc R . . C4A C -0.7806(4) -0.3770(8) 0.0930(8) 0.092(5) Uani 1 1 d . . . H4A H -0.7649 -0.4061 0.1364 0.110 Uiso 1 1 calc R . . C4B C -0.7942(3) -0.1251(6) -0.2838(7) 0.048(3) Uani 1 1 d . . . H4B H -0.7808 -0.0996 -0.3120 0.058 Uiso 1 1 calc R . . C5A C -0.8018(3) -0.4123(6) 0.0225(7) 0.067(4) Uani 1 1 d . . . H5A H -0.8012 -0.4671 0.0167 0.081 Uiso 1 1 calc R . . C5B C -0.8094(2) -0.0824(6) -0.2343(6) 0.040(2) Uani 1 1 d . . . H5B H -0.8061 -0.0280 -0.2278 0.047 Uiso 1 1 calc R . . C6A C -0.8242(3) -0.3680(6) -0.0411(6) 0.046(3) Uani 1 1 d . . . C6B C -0.8291(2) -0.1199(5) -0.1957(5) 0.032(2) Uani 1 1 d . . . C7A C -0.8476(2) -0.4040(5) -0.1197(6) 0.033(2) Uani 1 1 d . . . C7B C -0.8487(2) -0.0813(5) -0.1485(6) 0.033(2) Uani 1 1 d . . . C9A C -0.8911(2) -0.3807(5) -0.2449(5) 0.032(2) Uani 1 1 d . . . C9B C -0.8897(2) -0.1035(5) -0.0846(6) 0.033(2) Uani 1 1 d . . . C10A C -0.8934(2) -0.4593(5) -0.2657(6) 0.033(2) Uani 1 1 d . . . H10A H -0.9095 -0.4772 -0.3166 0.040 Uiso 1 1 calc R . . C10B C -0.8921(2) -0.0247(5) -0.0695(6) 0.035(2) Uani 1 1 d . . . H10B H -0.9079 -0.0065 -0.0444 0.042 Uiso 1 1 calc R . . C11A C -0.8716(2) -0.5112(5) -0.2103(6) 0.035(2) Uani 1 1 d . . . C11B C -0.8712(2) 0.0271(5) -0.0913(6) 0.035(2) Uani 1 1 d . . . C12A C -0.8488(2) -0.4824(5) -0.1377(6) 0.038(2) Uani 1 1 d . . . H12A H -0.8337 -0.5169 -0.0994 0.045 Uiso 1 1 calc R . . C12B C -0.8491(2) -0.0021(5) -0.1309(6) 0.036(2) Uani 1 1 d . . . H12B H -0.8343 0.0322 -0.1458 0.043 Uiso 1 1 calc R . . C13A C -0.9122(2) -0.3210(5) -0.3020(6) 0.032(2) Uani 1 1 d . . . C13B C -0.9089(2) -0.1675(5) -0.0607(6) 0.036(2) Uani 1 1 d . . . C15A C -0.9267(3) -0.1927(6) -0.3223(7) 0.048(3) Uani 1 1 d . . . H15A H -0.9241 -0.1409 -0.3016 0.057 Uiso 1 1 calc R . . C15B C -0.9179(3) -0.2989(6) -0.0624(7) 0.049(3) Uani 1 1 d . . . H15B H -0.9129 -0.3496 -0.0773 0.059 Uiso 1 1 calc R . . C16A C -0.9499(3) -0.2070(6) -0.4009(7) 0.059(3) Uani 1 1 d . . . H16A H -0.9625 -0.1657 -0.4339 0.070 Uiso 1 1 calc R . . C16B C -0.9411(3) -0.2911(6) -0.0216(7) 0.054(3) Uani 1 1 d . . . H16B H -0.9522 -0.3354 -0.0097 0.065 Uiso 1 1 calc R . . C17A C -0.9543(3) -0.2810(7) -0.4305(7) 0.059(3) Uani 1 1 d . . . H17A H -0.9706 -0.2925 -0.4837 0.071 Uiso 1 1 calc R . . C17B C -0.9480(3) -0.2194(6) 0.0011(7) 0.048(3) Uani 1 1 d . . . H17B H -0.9633 -0.2129 0.0315 0.057 Uiso 1 1 calc R . . C18A C -0.9346(3) -0.3402(6) -0.3813(6) 0.049(3) Uani 1 1 d . . . H18A H -0.9364 -0.3921 -0.4016 0.059 Uiso 1 1 calc R . . C18B C -0.9325(2) -0.1548(6) -0.0202(7) 0.043(2) Uani 1 1 d . . . H18B H -0.9378 -0.1037 -0.0075 0.052 Uiso 1 1 calc R . . C19A C -0.8743(2) -0.5942(5) -0.2310(6) 0.035(2) Uani 1 1 d . . . C19B C -0.8722(2) 0.1109(5) -0.0736(6) 0.037(2) Uani 1 1 d . . . C20A C -0.9051(2) -0.6310(6) -0.2678(6) 0.042(2) Uani 1 1 d . . . H20A H -0.9252 -0.6020 -0.2798 0.051 Uiso 1 1 calc R . . C20B C -0.9023(3) 0.1468(6) -0.0799(8) 0.052(3) Uani 1 1 d . . . H20B H -0.9225 0.1178 -0.0991 0.062 Uiso 1 1 calc R . . C21A C -0.9066(3) -0.7098(6) -0.2871(7) 0.046(3) Uani 1 1 d . . . H21A H -0.9278 -0.7343 -0.3093 0.055 Uiso 1 1 calc R . . C21B C -0.9034(3) 0.2231(6) -0.0588(9) 0.060(3) Uani 1 1 d . . . H21B H -0.9243 0.2452 -0.0615 0.072 Uiso 1 1 calc R . . C22A C -0.8778(2) -0.7532(5) -0.2746(6) 0.041(2) Uani 1 1 d . . . C22B C -0.8748(3) 0.2701(6) -0.0335(7) 0.047(3) Uani 1 1 d . . . C23A C -0.8470(3) -0.7175(6) -0.2392(7) 0.046(3) Uani 1 1 d . . . H23A H -0.8272 -0.7470 -0.2303 0.055 Uiso 1 1 calc R . . C23B C -0.8442(3) 0.2330(5) -0.0283(7) 0.043(2) Uani 1 1 d . . . H23B H -0.8240 0.2620 -0.0111 0.052 Uiso 1 1 calc R . . C24A C -0.8446(3) -0.6399(5) -0.2164(6) 0.043(2) Uani 1 1 d . . . H24A H -0.8233 -0.6169 -0.1912 0.051 Uiso 1 1 calc R . . C24B C -0.8434(2) 0.1562(5) -0.0478(6) 0.039(2) Uani 1 1 d . . . H24B H -0.8225 0.1329 -0.0437 0.047 Uiso 1 1 calc R . . C25A C -0.8799(3) -0.8372(6) -0.2989(7) 0.050(3) Uani 1 1 d . . . C25B C -0.8760(3) 0.3531(6) -0.0103(7) 0.053(3) Uani 1 1 d . . . C26A C -0.9070(3) -0.8822(6) -0.2968(6) 0.048(3) Uani 1 1 d . . . H26A H -0.9240 -0.8599 -0.2780 0.057 Uiso 1 1 calc R . . C26B C -0.9042(3) 0.3986(6) -0.0502(8) 0.058(3) Uani 1 1 d . . . H26B H -0.9221 0.3771 -0.0951 0.070 Uiso 1 1 calc R . . C27A C -0.9095(3) -0.9597(6) -0.3221(7) 0.057(3) Uani 1 1 d . . . H27A H -0.9274 -0.9908 -0.3177 0.068 Uiso 1 1 calc R . . C27B C -0.9064(4) 0.4740(6) -0.0250(10) 0.070(4) Uani 1 1 d . . . H27B H -0.9254 0.5047 -0.0532 0.084 Uiso 1 1 calc R . . C28A C -0.8855(3) -0.9917(6) -0.3542(7) 0.059(3) Uani 1 1 d . . . H28A H -0.8876 -1.0438 -0.3737 0.070 Uiso 1 1 calc R . . C28B C -0.8800(4) 0.5052(6) 0.0433(9) 0.075(4) Uani 1 1 d . . . H28B H -0.8814 0.5569 0.0618 0.090 Uiso 1 1 calc R . . C29A C -0.8587(3) -0.9469(6) -0.3571(7) 0.053(3) Uani 1 1 d . . . H29A H -0.8422 -0.9684 -0.3779 0.064 Uiso 1 1 calc R . . C29B C -0.8526(4) 0.4603(7) 0.0827(8) 0.065(3) Uani 1 1 d . . . H29B H -0.8347 0.4815 0.1278 0.078 Uiso 1 1 calc R . . C30A C -0.8564(3) -0.8712(6) -0.3298(7) 0.050(3) Uani 1 1 d . . . H30A H -0.8379 -0.8409 -0.3321 0.060 Uiso 1 1 calc R . . C30B C -0.85084(9) 0.3855(2) 0.0575(3) 0.062(3) Uani 1 1 d . . . H30B H -0.8320 0.3547 0.0870 0.075 Uiso 1 1 calc R . . O100 O -0.97192(9) -0.0501(2) -0.2201(3) 0.181(5) Uani 1 1 d R . . N101 N -1.00000(9) -0.0862(2) -0.2500(3) 0.110(6) Uani 1 2 d SR . . C102 C -1.00000(9) -0.1657(2) -0.2500(3) 0.139(7) Uani 1 2 d SR . . H10C H -0.9997 -0.1847 -0.1943 0.208 Uiso 0.50 1 calc PR . . H10D H -0.9801 -0.1847 -0.2620 0.208 Uiso 0.50 1 calc PR . . H10E H -1.0201 -0.1847 -0.2938 0.208 Uiso 0.50 1 calc PR . . O200 O -0.97991(9) -0.3716(2) -0.2339(3) 0.181(5) Uani 1 1 d RD . . N201 N -1.00000(9) -0.4055(2) -0.2500(3) 0.110(6) Uani 1 2 d SRD . . C202 C -1.00000(9) -0.4852(2) -0.2500(3) 0.139(7) Uani 1 2 d SR . . H20C H -0.9773 -0.5042 -0.2208 0.208 Uiso 0.50 1 calc PR . . H20D H -1.0075 -0.5042 -0.3087 0.208 Uiso 0.50 1 calc PR . . H20E H -1.0151 -0.5042 -0.2206 0.208 Uiso 0.50 1 calc PR . . C300 C -0.99702(9) 0.1517(2) -0.2091(3) 0.095(5) Uani 1 1 d RD . . H300 H -0.9912 0.1051 -0.1771 0.114 Uiso 1 1 calc R . . C301 C -0.99922(9) 0.2180(2) -0.1719(3) 0.087(5) Uani 1 1 d RD . . H301 H -1.0005 0.2137 -0.1161 0.105 Uiso 1 1 calc R . . C302 C -0.99998(9) 0.2910(2) -0.2014(3) 0.111(7) Uani 1 1 d RD . . H302 H -1.0004 0.3364 -0.1694 0.133 Uiso 1 1 calc R . . P3 P -0.74410(9) 0.0727(2) -0.3043(3) 0.187(4) Uani 1 1 d RD . . F13 F -0.74950(9) 0.0203(2) -0.2349(3) 0.246(10) Uani 1 1 d R . . F14 F -0.77923(9) 0.0522(2) -0.3536(3) 0.288(14) Uani 1 1 d R . . F15 F -0.73834(9) 0.1204(2) -0.3798(3) 0.305(14) Uani 1 1 d R . . F16 F -0.71450(9) 0.1115(2) -0.2252(3) 0.40(2) Uani 1 1 d R . . F17 F -0.73153(9) -0.0048(2) -0.3425(3) 0.49(3) Uani 1 1 d R . . F18 F -0.75764(9) 0.1512(2) -0.2779(3) 0.180(9) Uani 0.65 1 d PRD . . F19 F -0.75440(9) 0.1069(2) -0.2000(3) 0.078(6) Uani 0.35 1 d PRD . . C600 C -0.74331(9) -0.1956(2) -0.4396(3) 0.139(7) Uani 0.50 1 d PR . . H60A H -0.7291 -0.1675 -0.3898 0.208 Uiso 0.50 1 calc PR . . H60B H -0.7664 -0.1769 -0.4541 0.208 Uiso 0.50 1 calc PR . . H60C H -0.7351 -0.1867 -0.4876 0.208 Uiso 0.50 1 calc PR . . O601 O -0.74235(9) -0.2696(2) -0.4227(3) 0.181(5) Uani 0.50 1 d PR . . H601 H -0.7270 -0.2785 -0.3769 0.272 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0422(8) 0.0220(6) 0.0461(7) -0.0059(5) 0.0180(6) -0.0018(5) P1 0.037(2) 0.0245(18) 0.0417(19) -0.0022(15) 0.0149(16) 0.0004(14) P2 0.045(2) 0.031(2) 0.0382(19) -0.0014(16) 0.0106(17) 0.0036(16) F1 0.047(4) 0.037(3) 0.069(4) 0.002(3) 0.025(3) -0.006(3) F2 0.058(4) 0.037(3) 0.072(4) 0.020(3) 0.025(3) 0.013(3) F3 0.082(5) 0.053(4) 0.053(4) -0.014(3) 0.028(3) -0.014(3) F4 0.047(4) 0.050(4) 0.067(4) 0.003(3) 0.004(3) 0.006(3) F5 0.082(5) 0.046(4) 0.055(4) -0.014(3) 0.022(3) 0.014(3) F6 0.068(4) 0.052(4) 0.061(4) 0.013(3) 0.020(3) -0.010(3) N1A 0.048(6) 0.038(5) 0.059(5) -0.012(5) -0.003(4) 0.008(4) N1B 0.038(5) 0.028(4) 0.048(5) -0.010(4) 0.016(4) -0.003(3) N8A 0.032(4) 0.027(4) 0.035(4) 0.004(3) 0.012(3) 0.002(3) N8B 0.033(4) 0.027(4) 0.039(4) 0.002(3) 0.018(3) -0.001(3) N14A 0.035(5) 0.017(4) 0.052(5) 0.001(3) 0.009(4) 0.002(3) N14B 0.046(5) 0.018(4) 0.046(5) -0.007(3) 0.013(4) -0.010(3) C2A 0.079(10) 0.050(8) 0.072(9) -0.028(7) -0.012(7) -0.001(7) C2B 0.055(7) 0.030(6) 0.063(7) -0.010(5) 0.027(6) -0.002(5) C3A 0.118(13) 0.047(8) 0.068(8) -0.016(7) -0.027(8) -0.014(8) C3B 0.043(7) 0.042(6) 0.081(8) -0.021(6) 0.032(6) 0.002(5) C4A 0.134(13) 0.052(8) 0.051(7) 0.000(7) -0.024(8) -0.008(8) C4B 0.046(7) 0.034(6) 0.072(7) -0.007(5) 0.028(6) -0.006(5) C5A 0.081(9) 0.030(6) 0.057(7) 0.003(5) -0.024(6) -0.015(6) C5B 0.037(6) 0.026(5) 0.056(6) -0.009(5) 0.015(5) -0.008(4) C6A 0.049(7) 0.032(6) 0.047(6) -0.012(5) 0.005(5) -0.007(5) C6B 0.034(5) 0.021(5) 0.037(5) -0.003(4) 0.008(4) 0.006(4) C7A 0.039(6) 0.019(5) 0.041(5) 0.000(4) 0.013(4) 0.000(4) C7B 0.025(5) 0.025(5) 0.046(5) 0.000(4) 0.006(4) 0.000(4) C9A 0.042(6) 0.021(5) 0.035(5) 0.002(4) 0.013(4) 0.001(4) C9B 0.027(5) 0.027(5) 0.043(5) 0.000(4) 0.008(4) 0.000(4) C10A 0.034(5) 0.022(5) 0.042(5) -0.003(4) 0.008(4) -0.001(4) C10B 0.043(6) 0.022(5) 0.043(5) -0.006(4) 0.021(5) 0.002(4) C11A 0.046(6) 0.019(5) 0.042(5) -0.004(4) 0.016(5) -0.001(4) C11B 0.035(5) 0.027(5) 0.040(5) -0.001(4) 0.009(4) -0.001(4) C12A 0.048(6) 0.027(5) 0.035(5) 0.006(4) 0.009(4) 0.002(4) C12B 0.043(6) 0.025(5) 0.043(5) -0.006(4) 0.017(5) -0.004(4) C13A 0.030(5) 0.030(5) 0.037(5) 0.001(4) 0.011(4) -0.001(4) C13B 0.037(6) 0.028(5) 0.039(5) -0.009(4) 0.009(4) 0.003(4) C15A 0.049(7) 0.028(5) 0.067(7) 0.011(5) 0.018(6) 0.006(5) C15B 0.066(8) 0.025(5) 0.062(7) -0.004(5) 0.028(6) -0.009(5) C16A 0.078(9) 0.032(6) 0.061(7) 0.010(5) 0.014(7) 0.013(6) C16B 0.059(8) 0.034(6) 0.069(7) -0.005(6) 0.022(6) -0.015(5) C17A 0.070(9) 0.040(7) 0.046(6) 0.010(5) -0.010(6) 0.012(6) C17B 0.052(7) 0.041(6) 0.057(6) -0.004(5) 0.028(5) -0.011(5) C18A 0.066(8) 0.019(5) 0.052(6) -0.006(4) 0.006(6) 0.003(5) C18B 0.044(6) 0.027(5) 0.064(7) -0.008(5) 0.023(5) -0.004(4) C19A 0.031(5) 0.036(5) 0.032(5) 0.000(4) 0.003(4) 0.004(4) C19B 0.032(5) 0.028(5) 0.057(6) -0.006(5) 0.023(5) -0.003(4) C20A 0.030(5) 0.032(5) 0.057(6) -0.004(5) 0.002(5) 0.001(4) C20B 0.045(7) 0.025(5) 0.095(9) -0.003(6) 0.034(6) -0.006(4) C21A 0.032(6) 0.030(5) 0.060(6) -0.002(5) -0.008(5) -0.001(4) C21B 0.045(7) 0.035(6) 0.114(10) -0.009(6) 0.045(7) -0.003(5) C22A 0.038(6) 0.029(5) 0.044(6) -0.007(4) -0.003(4) -0.005(4) C22B 0.056(7) 0.025(5) 0.074(7) -0.004(5) 0.039(6) -0.003(5) C23A 0.042(6) 0.028(5) 0.062(7) -0.004(5) 0.009(5) 0.012(4) C23B 0.047(6) 0.029(5) 0.055(6) -0.014(5) 0.019(5) -0.013(4) C24A 0.040(6) 0.024(5) 0.055(6) -0.002(4) 0.001(5) -0.004(4) C24B 0.039(6) 0.024(5) 0.062(6) -0.002(4) 0.024(5) 0.007(4) C25A 0.051(7) 0.023(5) 0.063(7) -0.013(5) -0.001(5) 0.010(5) C25B 0.084(9) 0.026(5) 0.071(7) -0.007(5) 0.058(7) 0.002(5) C26A 0.046(7) 0.028(5) 0.051(6) 0.000(5) -0.009(5) -0.002(5) C26B 0.077(9) 0.029(6) 0.085(8) 0.001(6) 0.049(7) 0.001(5) C27A 0.061(8) 0.029(6) 0.057(7) 0.002(5) -0.014(6) -0.009(5) C27B 0.088(10) 0.027(6) 0.121(12) -0.001(7) 0.070(9) 0.011(6) C28A 0.076(9) 0.020(5) 0.057(7) -0.010(5) -0.010(6) 0.009(5) C28B 0.151(14) 0.017(5) 0.089(9) -0.002(6) 0.083(10) 0.014(7) C29A 0.050(7) 0.031(6) 0.064(7) -0.008(5) -0.001(6) 0.010(5) C29B 0.111(11) 0.037(7) 0.055(7) -0.001(6) 0.037(7) -0.009(7) C30A 0.052(7) 0.022(5) 0.063(7) -0.011(5) 0.000(5) -0.004(5) C30B 0.083(9) 0.028(6) 0.084(8) -0.017(6) 0.038(7) -0.001(6) O100 0.145(9) 0.324(16) 0.090(6) -0.032(7) 0.059(6) -0.070(9) N101 0.094(12) 0.178(18) 0.066(8) 0.000 0.037(8) 0.000 C102 0.19(2) 0.134(17) 0.118(13) 0.000 0.086(13) 0.000 O200 0.145(9) 0.324(16) 0.090(6) -0.032(7) 0.059(6) -0.070(9) N201 0.094(12) 0.178(18) 0.066(8) 0.000 0.037(8) 0.000 C202 0.19(2) 0.134(17) 0.118(13) 0.000 0.086(13) 0.000 C300 0.053(9) 0.163(17) 0.074(8) -0.021(9) 0.027(8) 0.004(9) C301 0.112(13) 0.096(12) 0.058(8) -0.013(9) 0.033(8) -0.021(10) C302 0.036(8) 0.130(14) 0.161(16) -0.081(12) 0.025(10) -0.024(9) P3 0.091(4) 0.106(5) 0.355(12) 0.116(6) 0.062(6) 0.011(3) F13 0.215(17) 0.124(12) 0.35(2) 0.126(14) 0.026(16) -0.079(11) F14 0.063(8) 0.34(2) 0.39(3) 0.24(2) -0.014(11) -0.028(11) F15 0.31(2) 0.139(13) 0.61(4) 0.124(19) 0.35(3) 0.012(13) F16 0.240(19) 0.232(19) 0.54(4) 0.21(2) -0.12(2) -0.198(17) F17 0.226(19) 0.111(14) 1.16(9) 0.23(3) 0.26(4) 0.064(13) F18 0.190(19) 0.081(12) 0.25(2) 0.115(15) 0.047(17) 0.014(11) F19 0.038(11) 0.044(12) 0.14(2) 0.000(12) 0.019(12) 0.003(9) C600 0.19(2) 0.134(17) 0.118(13) 0.000 0.086(13) 0.000 O601 0.145(9) 0.324(16) 0.090(6) -0.032(7) 0.059(6) -0.070(9) _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 Cu1 N8B 1.915(7) . ? Cu1 N8A 2.006(7) . ? Cu1 N1B 2.060(8) . ? Cu1 N14B 2.075(8) . ? Cu1 N1A 2.266(9) . ? Cu1 N14A 2.276(8) . ? P1 F3 1.583(6) . ? P1 F3 1.583(6) 5_355 ? P1 F2 1.597(5) 5_355 ? P1 F2 1.597(5) . ? P1 F1 1.608(5) . ? P1 F1 1.608(5) 5_355 ? P2 F5 1.587(6) 5_344 ? P2 F5 1.587(6) . ? P2 F6 1.593(6) . ? P2 F6 1.593(6) 5_344 ? P2 F4 1.615(6) 5_344 ? P2 F4 1.615(6) . ? N1A C6A 1.311(12) . ? N1A C2A 1.356(14) . ? N1B C2B 1.353(12) . ? N1B C6B 1.353(11) . ? N8A C7A 1.346(11) . ? N8A C9A 1.347(11) . ? N8B C7B 1.352(11) . ? N8B C9B 1.362(11) . ? N14A C15A 1.327(12) . ? N14A C13A 1.339(11) . ? N14B C15B 1.325(12) . ? N14B C13B 1.344(11) . ? C2A C3A 1.374(18) . ? C2B C3B 1.392(15) . ? C3A C4A 1.408(18) . ? C3B C4B 1.364(14) . ? C4A C5A 1.366(16) . ? C4B C5B 1.406(13) . ? C5A C6A 1.399(14) . ? C5B C6B 1.368(13) . ? C6A C7A 1.494(13) . ? C6B C7B 1.472(12) . ? C7A C12A 1.382(12) . ? C7B C12B 1.397(12) . ? C9A C10A 1.393(12) . ? C9A C13A 1.485(12) . ? C9B C10B 1.389(12) . ? C9B C13B 1.498(13) . ? C10A C11A 1.396(12) . ? C10B C11B 1.386(12) . ? C11A C12A 1.371(13) . ? C11A C19A 1.466(12) . ? C11B C12B 1.400(12) . ? C11B C19B 1.477(12) . ? C13A C18A 1.393(13) . ? C13B C18B 1.389(13) . ? C15A C16A 1.379(16) . ? C15B C16B 1.371(15) . ? C16A C17A 1.357(16) . ? C16B C17B 1.352(15) . ? C17A C18A 1.402(14) . ? C17B C18B 1.395(13) . ? C19A C20A 1.398(12) . ? C19A C24A 1.436(13) . ? C19B C20B 1.389(13) . ? C19B C24B 1.394(13) . ? C20A C21A 1.390(13) . ? C20B C21B 1.365(14) . ? C21A C22A 1.387(14) . ? C21B C22B 1.401(15) . ? C22A C23A 1.386(14) . ? C22A C25A 1.497(13) . ? C22B C23B 1.424(14) . ? C22B C25B 1.487(13) . ? C23A C24A 1.384(13) . ? C23B C24B 1.364(12) . ? C25A C30A 1.391(15) . ? C25A C26A 1.394(15) . ? C25B C30B 1.392(13) . ? C25B C26B 1.402(16) . ? C26A C27A 1.394(14) . ? C26B C27B 1.376(15) . ? C27A C28A 1.403(17) . ? C27B C28B 1.414(19) . ? C28A C29A 1.383(16) . ? C28B C29B 1.371(18) . ? C29A C30A 1.375(13) . ? C29B C30B 1.364(12) . ? O100 N101 1.2893 . ? N101 O100 1.289(6) 2_354 ? N101 C102 1.3692 . ? O200 N201 0.9937 . ? O200 O200 1.608(7) 2_354 ? N201 O200 0.994(6) 2_354 ? N201 C202 1.3720 . ? C300 C300 1.303(9) 2_354 ? C300 C301 1.3166 . ? C301 C302 1.3465 . ? C302 C302 1.618(9) 2_354 ? P3 F14 1.4884 . ? P3 F13 1.5409 . ? P3 F15 1.5853 . ? P3 F18 1.5861 . ? P3 F16 1.6378 . ? P3 F17 1.6387 . ? P3 F19 2.0115 . ? F13 F19 1.6384 . ? F18 F19 1.4730 . ? C600 O601 1.3041 . ? 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 N8B Cu1 N8A 177.3(3) . . ? N8B Cu1 N1B 78.7(3) . . ? N8A Cu1 N1B 102.4(3) . . ? N8B Cu1 N14B 80.0(3) . . ? N8A Cu1 N14B 98.9(3) . . ? N1B Cu1 N14B 158.6(3) . . ? N8B Cu1 N1A 106.4(3) . . ? N8A Cu1 N1A 76.1(3) . . ? N1B Cu1 N1A 93.5(3) . . ? N14B Cu1 N1A 94.1(3) . . ? N8B Cu1 N14A 100.7(3) . . ? N8A Cu1 N14A 76.8(3) . . ? N1B Cu1 N14A 90.3(3) . . ? N14B Cu1 N14A 92.0(3) . . ? N1A Cu1 N14A 152.8(3) . . ? F3 P1 F3 180.0(4) . 5_355 ? F3 P1 F2 90.5(3) . 5_355 ? F3 P1 F2 89.5(3) 5_355 5_355 ? F3 P1 F2 89.5(3) . . ? F3 P1 F2 90.5(3) 5_355 . ? F2 P1 F2 180.0(2) 5_355 . ? F3 P1 F1 90.0(3) . . ? F3 P1 F1 90.0(3) 5_355 . ? F2 P1 F1 89.7(3) 5_355 . ? F2 P1 F1 90.3(3) . . ? F3 P1 F1 90.0(3) . 5_355 ? F3 P1 F1 90.0(3) 5_355 5_355 ? F2 P1 F1 90.3(3) 5_355 5_355 ? F2 P1 F1 89.7(3) . 5_355 ? F1 P1 F1 179.999(1) . 5_355 ? F5 P2 F5 179.995(5) 5_344 . ? F5 P2 F6 90.2(3) 5_344 . ? F5 P2 F6 89.8(3) . . ? F5 P2 F6 89.8(3) 5_344 5_344 ? F5 P2 F6 90.2(3) . 5_344 ? F6 P2 F6 179.996(2) . 5_344 ? F5 P2 F4 90.2(3) 5_344 5_344 ? F5 P2 F4 89.8(3) . 5_344 ? F6 P2 F4 90.1(3) . 5_344 ? F6 P2 F4 89.9(3) 5_344 5_344 ? F5 P2 F4 89.8(3) 5_344 . ? F5 P2 F4 90.2(3) . . ? F6 P2 F4 89.9(3) . . ? F6 P2 F4 90.1(3) 5_344 . ? F4 P2 F4 179.996(2) 5_344 . ? C6A N1A C2A 120.0(10) . . ? C6A N1A Cu1 112.2(7) . . ? C2A N1A Cu1 127.6(8) . . ? C2B N1B C6B 117.8(8) . . ? C2B N1B Cu1 126.9(7) . . ? C6B N1B Cu1 115.2(6) . . ? C7A N8A C9A 119.4(8) . . ? C7A N8A Cu1 120.6(6) . . ? C9A N8A Cu1 119.9(6) . . ? C7B N8B C9B 119.4(8) . . ? C7B N8B Cu1 120.5(6) . . ? C9B N8B Cu1 119.9(6) . . ? C15A N14A C13A 118.3(9) . . ? C15A N14A Cu1 130.8(7) . . ? C13A N14A Cu1 110.9(6) . . ? C15B N14B C13B 118.3(9) . . ? C15B N14B Cu1 128.4(7) . . ? C13B N14B Cu1 113.2(6) . . ? N1A C2A C3A 120.6(11) . . ? N1B C2B C3B 123.1(9) . . ? C2A C3A C4A 120.2(11) . . ? C4B C3B C2B 118.4(9) . . ? C5A C4A C3A 117.1(12) . . ? C3B C4B C5B 119.1(10) . . ? C4A C5A C6A 120.2(11) . . ? C6B C5B C4B 119.6(9) . . ? N1A C6A C5A 121.7(9) . . ? N1A C6A C7A 116.3(9) . . ? C5A C6A C7A 122.0(9) . . ? N1B C6B C5B 122.0(8) . . ? N1B C6B C7B 113.0(8) . . ? C5B C6B C7B 124.8(8) . . ? N8A C7A C12A 120.9(8) . . ? N8A C7A C6A 114.8(8) . . ? C12A C7A C6A 124.4(8) . . ? N8B C7B C12B 120.5(8) . . ? N8B C7B C6B 112.6(8) . . ? C12B C7B C6B 126.9(8) . . ? N8A C9A C10A 121.8(8) . . ? N8A C9A C13A 115.8(8) . . ? C10A C9A C13A 122.3(8) . . ? N8B C9B C10B 121.9(8) . . ? N8B C9B C13B 111.6(8) . . ? C10B C9B C13B 126.5(8) . . ? C9A C10A C11A 118.6(8) . . ? C11B C10B C9B 119.5(8) . . ? C12A C11A C10A 118.5(8) . . ? C12A C11A C19A 122.6(8) . . ? C10A C11A C19A 119.0(8) . . ? C10B C11B C12B 118.2(8) . . ? C10B C11B C19B 121.0(8) . . ? C12B C11B C19B 120.9(8) . . ? C11A C12A C7A 120.8(9) . . ? C7B C12B C11B 120.3(9) . . ? N14A C13A C18A 121.9(9) . . ? N14A C13A C9A 116.4(8) . . ? C18A C13A C9A 121.7(8) . . ? N14B C13B C18B 121.7(9) . . ? N14B C13B C9B 115.0(8) . . ? C18B C13B C9B 123.2(8) . . ? N14A C15A C16A 123.4(10) . . ? N14B C15B C16B 123.4(10) . . ? C17A C16A C15A 118.9(10) . . ? C17B C16B C15B 118.8(10) . . ? C16A C17A C18A 119.0(10) . . ? C16B C17B C18B 119.7(10) . . ? C13A C18A C17A 118.3(9) . . ? C13B C18B C17B 118.0(9) . . ? C20A C19A C24A 117.6(9) . . ? C20A C19A C11A 122.4(8) . . ? C24A C19A C11A 119.9(8) . . ? C20B C19B C24B 117.7(9) . . ? C20B C19B C11B 120.4(8) . . ? C24B C19B C11B 121.9(8) . . ? C21A C20A C19A 120.8(9) . . ? C21B C20B C19B 121.0(10) . . ? C22A C21A C20A 121.2(9) . . ? C20B C21B C22B 122.4(10) . . ? C23A C22A C21A 118.9(9) . . ? C23A C22A C25A 120.6(9) . . ? C21A C22A C25A 120.5(9) . . ? C21B C22B C23B 116.1(9) . . ? C21B C22B C25B 122.4(10) . . ? C23B C22B C25B 121.5(9) . . ? C24A C23A C22A 121.3(9) . . ? C24B C23B C22B 120.9(9) . . ? C23A C24A C19A 120.0(9) . . ? C23B C24B C19B 121.9(9) . . ? C30A C25A C26A 118.0(9) . . ? C30A C25A C22A 121.3(10) . . ? C26A C25A C22A 120.6(10) . . ? C30B C25B C26B 118.1(9) . . ? C30B C25B C22B 121.0(10) . . ? C26B C25B C22B 120.6(11) . . ? C27A C26A C25A 120.4(11) . . ? C27B C26B C25B 120.8(12) . . ? C26A C27A C28A 119.9(11) . . ? C26B C27B C28B 119.4(12) . . ? C29A C28A C27A 119.8(10) . . ? C29B C28B C27B 119.6(11) . . ? C30A C29A C28A 119.3(11) . . ? C30B C29B C28B 120.5(11) . . ? C29A C30A C25A 122.5(11) . . ? C29B C30B C25B 121.5(8) . . ? O100 N101 O100 122.33(15) 2_354 . ? O100 N101 C102 118.83(15) 2_354 . ? O100 N101 C102 118.8 . . ? N201 O200 O200 36.0 . 2_354 ? O200 N201 O200 108.0(2) 2_354 . ? O200 N201 C202 126.0(2) 2_354 . ? O200 N201 C202 126.0 . . ? C300 C300 C301 118.21(6) 2_354 . ? C300 C301 C302 129.4 . . ? C301 C302 C302 110.9 . 2_354 ? F14 P3 F13 84.9 . . ? F14 P3 F15 93.9 . . ? F13 P3 F15 175.4 . . ? F14 P3 F18 88.2 . . ? F13 P3 F18 97.9 . . ? F15 P3 F18 86.5 . . ? F14 P3 F16 155.0 . . ? F13 P3 F16 84.0 . . ? F15 P3 F16 98.7 . . ? F18 P3 F16 71.3 . . ? F14 P3 F17 89.2 . . ? F13 P3 F17 87.7 . . ? F15 P3 F17 87.8 . . ? F18 P3 F17 173.6 . . ? F16 P3 F17 112.6 . . ? F14 P3 F19 95.1 . . ? F13 P3 F19 52.9 . . ? F15 P3 F19 131.6 . . ? F18 P3 F19 46.5 . . ? F16 P3 F19 60.6 . . ? F17 P3 F19 139.6 . . ? P3 F13 F19 78.4 . . ? F19 F18 P3 82.1 . . ? F18 F19 F13 98.4 . . ? F18 F19 P3 51.4 . . ? F13 F19 P3 48.6 . . ? 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 N8B Cu1 N1A C6A 176.5(8) . . . . ? N8A Cu1 N1A C6A -2.4(8) . . . . ? N1B Cu1 N1A C6A -104.2(8) . . . . ? N14B Cu1 N1A C6A 95.7(8) . . . . ? N14A Cu1 N1A C6A -6.7(13) . . . . ? N8B Cu1 N1A C2A 2.3(12) . . . . ? N8A Cu1 N1A C2A -176.6(12) . . . . ? N1B Cu1 N1A C2A 81.5(12) . . . . ? N14B Cu1 N1A C2A -78.5(12) . . . . ? N14A Cu1 N1A C2A 179.0(10) . . . . ? N8B Cu1 N1B C2B -175.6(9) . . . . ? N8A Cu1 N1B C2B 1.9(9) . . . . ? N14B Cu1 N1B C2B -170.8(9) . . . . ? N1A Cu1 N1B C2B 78.4(9) . . . . ? N14A Cu1 N1B C2B -74.7(9) . . . . ? N8B Cu1 N1B C6B 0.6(6) . . . . ? N8A Cu1 N1B C6B 178.1(6) . . . . ? N14B Cu1 N1B C6B 5.4(13) . . . . ? N1A Cu1 N1B C6B -105.4(7) . . . . ? N14A Cu1 N1B C6B 101.5(7) . . . . ? N8B Cu1 N8A C7A -156(6) . . . . ? N1B Cu1 N8A C7A 92.0(7) . . . . ? N14B Cu1 N8A C7A -90.6(7) . . . . ? N1A Cu1 N8A C7A 1.4(7) . . . . ? N14A Cu1 N8A C7A 179.4(7) . . . . ? N8B Cu1 N8A C9A 22(7) . . . . ? N1B Cu1 N8A C9A -90.1(7) . . . . ? N14B Cu1 N8A C9A 87.2(7) . . . . ? N1A Cu1 N8A C9A 179.2(7) . . . . ? N14A Cu1 N8A C9A -2.8(6) . . . . ? N8A Cu1 N8B C7B -114(6) . . . . ? N1B Cu1 N8B C7B -1.0(7) . . . . ? N14B Cu1 N8B C7B -179.2(7) . . . . ? N1A Cu1 N8B C7B 89.4(7) . . . . ? N14A Cu1 N8B C7B -89.1(7) . . . . ? N8A Cu1 N8B C9B 61(6) . . . . ? N1B Cu1 N8B C9B 174.1(7) . . . . ? N14B Cu1 N8B C9B -4.1(7) . . . . ? N1A Cu1 N8B C9B -95.5(7) . . . . ? N14A Cu1 N8B C9B 86.0(7) . . . . ? N8B Cu1 N14A C15A 1.4(9) . . . . ? N8A Cu1 N14A C15A -179.7(9) . . . . ? N1B Cu1 N14A C15A -77.1(9) . . . . ? N14B Cu1 N14A C15A 81.7(9) . . . . ? N1A Cu1 N14A C15A -175.4(9) . . . . ? N8B Cu1 N14A C13A -178.2(6) . . . . ? N8A Cu1 N14A C13A 0.6(6) . . . . ? N1B Cu1 N14A C13A 103.3(6) . . . . ? N14B Cu1 N14A C13A -98.0(6) . . . . ? N1A Cu1 N14A C13A 5.0(11) . . . . ? N8B Cu1 N14B C15B -178.5(9) . . . . ? N8A Cu1 N14B C15B 4.0(9) . . . . ? N1B Cu1 N14B C15B 176.8(9) . . . . ? N1A Cu1 N14B C15B -72.5(9) . . . . ? N14A Cu1 N14B C15B 81.0(9) . . . . ? N8B Cu1 N14B C13B 3.0(6) . . . . ? N8A Cu1 N14B C13B -174.5(6) . . . . ? N1B Cu1 N14B C13B -1.7(13) . . . . ? N1A Cu1 N14B C13B 109.0(7) . . . . ? N14A Cu1 N14B C13B -97.5(7) . . . . ? C6A N1A C2A C3A 5(2) . . . . ? Cu1 N1A C2A C3A 178.7(12) . . . . ? C6B N1B C2B C3B -1.4(15) . . . . ? Cu1 N1B C2B C3B 174.7(8) . . . . ? N1A C2A C3A C4A -5(3) . . . . ? N1B C2B C3B C4B 1.0(17) . . . . ? C2A C3A C4A C5A 2(3) . . . . ? C2B C3B C4B C5B 0.4(16) . . . . ? C3A C4A C5A C6A 1(2) . . . . ? C3B C4B C5B C6B -1.3(15) . . . . ? C2A N1A C6A C5A -2.0(19) . . . . ? Cu1 N1A C6A C5A -176.8(10) . . . . ? C2A N1A C6A C7A 177.7(11) . . . . ? Cu1 N1A C6A C7A 2.9(12) . . . . ? C4A C5A C6A N1A -1(2) . . . . ? C4A C5A C6A C7A 179.3(13) . . . . ? C2B N1B C6B C5B 0.3(14) . . . . ? Cu1 N1B C6B C5B -176.2(7) . . . . ? C2B N1B C6B C7B 176.3(8) . . . . ? Cu1 N1B C6B C7B -0.2(10) . . . . ? C4B C5B C6B N1B 1.0(14) . . . . ? C4B C5B C6B C7B -174.5(9) . . . . ? C9A N8A C7A C12A 0.9(13) . . . . ? Cu1 N8A C7A C12A 178.8(7) . . . . ? C9A N8A C7A C6A -178.2(8) . . . . ? Cu1 N8A C7A C6A -0.4(11) . . . . ? N1A C6A C7A N8A -1.9(14) . . . . ? C5A C6A C7A N8A 177.8(10) . . . . ? N1A C6A C7A C12A 179.0(10) . . . . ? C5A C6A C7A C12A -1.3(17) . . . . ? C9B N8B C7B C12B 5.5(13) . . . . ? Cu1 N8B C7B C12B -179.4(7) . . . . ? C9B N8B C7B C6B -173.9(8) . . . . ? Cu1 N8B C7B C6B 1.2(10) . . . . ? N1B C6B C7B N8B -0.6(11) . . . . ? C5B C6B C7B N8B 175.3(9) . . . . ? N1B C6B C7B C12B -180.0(9) . . . . ? C5B C6B C7B C12B -4.1(15) . . . . ? C7A N8A C9A C10A -0.6(13) . . . . ? Cu1 N8A C9A C10A -178.5(7) . . . . ? C7A N8A C9A C13A -177.7(7) . . . . ? Cu1 N8A C9A C13A 4.4(10) . . . . ? C7B N8B C9B C10B -2.4(13) . . . . ? Cu1 N8B C9B C10B -177.5(7) . . . . ? C7B N8B C9B C13B 179.5(8) . . . . ? Cu1 N8B C9B C13B 4.3(10) . . . . ? N8A C9A C10A C11A 0.2(14) . . . . ? C13A C9A C10A C11A 177.2(8) . . . . ? N8B C9B C10B C11B -1.5(14) . . . . ? C13B C9B C10B C11B 176.3(9) . . . . ? C9A C10A C11A C12A -0.1(13) . . . . ? C9A C10A C11A C19A 178.9(8) . . . . ? C9B C10B C11B C12B 2.2(13) . . . . ? C9B C10B C11B C19B -178.0(8) . . . . ? C10A C11A C12A C7A 0.4(14) . . . . ? C19A C11A C12A C7A -178.6(9) . . . . ? N8A C7A C12A C11A -0.8(14) . . . . ? C6A C7A C12A C11A 178.2(9) . . . . ? N8B C7B C12B C11B -4.8(14) . . . . ? C6B C7B C12B C11B 174.6(8) . . . . ? C10B C11B C12B C7B 0.8(14) . . . . ? C19B C11B C12B C7B -179.0(9) . . . . ? C15A N14A C13A C18A 3.5(14) . . . . ? Cu1 N14A C13A C18A -176.8(8) . . . . ? C15A N14A C13A C9A -178.4(8) . . . . ? Cu1 N14A C13A C9A 1.3(9) . . . . ? N8A C9A C13A N14A -3.6(12) . . . . ? C10A C9A C13A N14A 179.2(8) . . . . ? N8A C9A C13A C18A 174.5(9) . . . . ? C10A C9A C13A C18A -2.6(14) . . . . ? C15B N14B C13B C18B -0.7(14) . . . . ? Cu1 N14B C13B C18B 177.9(8) . . . . ? C15B N14B C13B C9B 179.7(8) . . . . ? Cu1 N14B C13B C9B -1.6(10) . . . . ? N8B C9B C13B N14B -1.5(11) . . . . ? C10B C9B C13B N14B -179.5(9) . . . . ? N8B C9B C13B C18B 179.0(9) . . . . ? C10B C9B C13B C18B 1.0(15) . . . . ? C13A N14A C15A C16A -2.3(16) . . . . ? Cu1 N14A C15A C16A 178.0(9) . . . . ? C13B N14B C15B C16B 0.0(16) . . . . ? Cu1 N14B C15B C16B -178.4(8) . . . . ? N14A C15A C16A C17A 1.5(18) . . . . ? N14B C15B C16B C17B -1.0(17) . . . . ? C15A C16A C17A C18A -1.9(19) . . . . ? C15B C16B C17B C18B 2.7(16) . . . . ? N14A C13A C18A C17A -3.9(16) . . . . ? C9A C13A C18A C17A 178.1(10) . . . . ? C16A C17A C18A C13A 3.0(18) . . . . ? N14B C13B C18B C17B 2.4(15) . . . . ? C9B C13B C18B C17B -178.1(9) . . . . ? C16B C17B C18B C13B -3.4(16) . . . . ? C12A C11A C19A C20A 140.8(10) . . . . ? C10A C11A C19A C20A -38.3(13) . . . . ? C12A C11A C19A C24A -41.7(14) . . . . ? C10A C11A C19A C24A 139.3(9) . . . . ? C10B C11B C19B C20B -35.5(14) . . . . ? C12B C11B C19B C20B 144.3(10) . . . . ? C10B C11B C19B C24B 142.6(10) . . . . ? C12B C11B C19B C24B -37.7(14) . . . . ? C24A C19A C20A C21A 1.9(14) . . . . ? C11A C19A C20A C21A 179.5(10) . . . . ? C24B C19B C20B C21B -2.1(17) . . . . ? C11B C19B C20B C21B 176.1(11) . . . . ? C19A C20A C21A C22A -3.4(16) . . . . ? C19B C20B C21B C22B 3(2) . . . . ? C20A C21A C22A C23A 2.5(16) . . . . ? C20A C21A C22A C25A -177.6(10) . . . . ? C20B C21B C22B C23B -1.9(18) . . . . ? C20B C21B C22B C25B -179.8(12) . . . . ? C21A C22A C23A C24A -0.2(16) . . . . ? C25A C22A C23A C24A 179.9(10) . . . . ? C21B C22B C23B C24B 0.5(16) . . . . ? C25B C22B C23B C24B 178.4(10) . . . . ? C22A C23A C24A C19A -1.2(16) . . . . ? C20A C19A C24A C23A 0.4(14) . . . . ? C11A C19A C24A C23A -177.3(9) . . . . ? C22B C23B C24B C19B 0.1(16) . . . . ? C20B C19B C24B C23B 0.7(15) . . . . ? C11B C19B C24B C23B -177.5(9) . . . . ? C23A C22A C25A C30A -34.4(15) . . . . ? C21A C22A C25A C30A 145.7(11) . . . . ? C23A C22A C25A C26A 150.2(10) . . . . ? C21A C22A C25A C26A -29.7(16) . . . . ? C21B C22B C25B C30B 140.3(11) . . . . ? C23B C22B C25B C30B -37.5(14) . . . . ? C21B C22B C25B C26B -32.6(16) . . . . ? C23B C22B C25B C26B 149.6(11) . . . . ? C30A C25A C26A C27A 2.3(15) . . . . ? C22A C25A C26A C27A 177.9(9) . . . . ? C30B C25B C26B C27B 2.5(15) . . . . ? C22B C25B C26B C27B 175.6(10) . . . . ? C25A C26A C27A C28A -3.3(16) . . . . ? C25B C26B C27B C28B -1.5(17) . . . . ? C26A C27A C28A C29A 2.7(16) . . . . ? C26B C27B C28B C29B 0.8(18) . . . . ? C27A C28A C29A C30A -1.0(16) . . . . ? C27B C28B C29B C30B -1.3(17) . . . . ? C28A C29A C30A C25A 0.0(17) . . . . ? C26A C25A C30A C29A -0.6(16) . . . . ? C22A C25A C30A C29A -176.2(10) . . . . ? C28B C29B C30B C25B 2.4(14) . . . . ? C26B C25B C30B C29B -3.0(12) . . . . ? C22B C25B C30B C29B -176.0(9) . . . . ? O200 O200 N201 C202 180.0(5) 2_354 . . . ? C300 C300 C301 C302 -15.6(3) 2_354 . . . ? C300 C301 C302 C302 3.5(3) . . . 2_354 ? F14 P3 F13 F19 -100.3 . . . . ? F15 P3 F13 F19 -175(100) . . . . ? F18 P3 F13 F19 -12.8 . . . . ? F16 P3 F13 F19 57.3 . . . . ? F17 P3 F13 F19 170.3 . . . . ? F14 P3 F18 F19 98.7 . . . . ? F13 P3 F18 F19 14.1 . . . . ? F15 P3 F18 F19 -167.3 . . . . ? F16 P3 F18 F19 -66.8 . . . . ? F17 P3 F18 F19 164.5 . . . . ? P3 F18 F19 F13 -13.3 . . . . ? P3 F13 F19 F18 13.8 . . . . ? F14 P3 F19 F18 -82.7 . . . . ? F13 P3 F19 F18 -162.4 . . . . ? F15 P3 F19 F18 17.1 . . . . ? F16 P3 F19 F18 91.6 . . . . ? F17 P3 F19 F18 -177.4 . . . . ? F14 P3 F19 F13 79.7 . . . . ? F15 P3 F19 F13 179.5 . . . . ? F18 P3 F19 F13 162.4 . . . . ? F16 P3 F19 F13 -106.1 . . . . ? F17 P3 F19 F13 -15.0 . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.750 _refine_diff_density_min -1.037 _refine_diff_density_rms 0.174 data_nibptp _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H38 F12 N6 Ni O P2' _chemical_formula_weight 1135.55 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, -z' 'x-1/2, -y-1/2, -z' _cell_length_a 16.5047(4) _cell_length_b 17.1444(4) _cell_length_c 20.3835(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5767.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4981 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description plates _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 0.472 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 21595 _diffrn_reflns_av_R_equivalents 0.1410 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 22.00 _reflns_number_total 3642 _reflns_number_gt 2356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 3642 _refine_ls_number_parameters 402 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1760 _refine_ls_R_factor_gt 0.1243 _refine_ls_wR_factor_ref 0.3072 _refine_ls_wR_factor_gt 0.2877 _refine_ls_goodness_of_fit_ref 1.770 _refine_ls_restrained_S_all 1.778 _refine_ls_shift/su_max 0.227 _refine_ls_shift/su_mean 0.012 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 Ni1 Ni 0.0000 0.0000 0.23819(8) 0.0392(7) Uani 1 2 d S . . N11 N 0.0916(5) 0.0072(4) 0.3089(4) 0.039(2) Uani 1 1 d . . . C12 C 0.1271(7) -0.0523(6) 0.3432(5) 0.055(3) Uani 1 1 d . . . H12A H 0.1102 -0.1042 0.3339 0.066 Uiso 1 1 calc R . . C13 C 0.1845(7) -0.0417(7) 0.3894(5) 0.057(3) Uani 1 1 d . . . H13A H 0.2066 -0.0853 0.4120 0.068 Uiso 1 1 calc R . . C14 C 0.2110(8) 0.0325(7) 0.4038(5) 0.060(3) Uani 1 1 d . . . H14A H 0.2511 0.0412 0.4364 0.072 Uiso 1 1 calc R . . C15 C 0.1771(7) 0.0944(6) 0.3690(5) 0.049(3) Uani 1 1 d . . . H15A H 0.1950 0.1462 0.3767 0.059 Uiso 1 1 calc R . . C16 C 0.1176(6) 0.0798(5) 0.3234(5) 0.039(3) Uani 1 1 d . . . N17 N 0.0235(5) 0.1135(4) 0.2396(4) 0.041(2) Uani 1 1 d . . . C18 C 0.0761(7) 0.1409(6) 0.2823(5) 0.044(3) Uani 1 1 d . . . C19 C 0.0933(7) 0.2200(5) 0.2865(5) 0.046(3) Uani 1 1 d . . . H19A H 0.1308 0.2387 0.3181 0.055 Uiso 1 1 calc R . . C110 C 0.0552(7) 0.2715(5) 0.2441(4) 0.043(3) Uani 1 1 d . . . C111 C -0.0001(7) 0.2400(6) 0.1994(5) 0.050(3) Uani 1 1 d . . . H11A H -0.0263 0.2732 0.1687 0.060 Uiso 1 1 calc R . . C112 C -0.0167(6) 0.1623(5) 0.1996(5) 0.041(3) Uani 1 1 d . . . N113 N -0.0818(5) 0.0431(4) 0.1676(4) 0.040(2) Uani 1 1 d . . . C114 C -0.1375(7) 0.0040(7) 0.1342(5) 0.049(3) Uani 1 1 d . . . H11B H -0.1390 -0.0511 0.1392 0.059 Uiso 1 1 calc R . . C115 C -0.1921(8) 0.0369(7) 0.0935(6) 0.069(4) Uani 1 1 d . . . H11C H -0.2306 0.0058 0.0706 0.082 Uiso 1 1 calc R . . C116 C -0.1907(8) 0.1174(7) 0.0859(5) 0.070(4) Uani 1 1 d . . . H11D H -0.2295 0.1429 0.0590 0.084 Uiso 1 1 calc R . . C117 C -0.1325(8) 0.1592(7) 0.1179(5) 0.065(4) Uani 1 1 d . . . H11E H -0.1295 0.2141 0.1123 0.078 Uiso 1 1 calc R . . C118 C -0.0777(7) 0.1215(6) 0.1586(5) 0.049(3) Uani 1 1 d . . . C119 C 0.0752(7) 0.3553(5) 0.2453(5) 0.049(3) Uani 1 1 d . . . C120 C 0.0927(7) 0.3921(6) 0.3050(5) 0.053(3) Uani 1 1 d . . . H12B H 0.0899 0.3631 0.3446 0.064 Uiso 1 1 calc R . . C121 C 0.1138(7) 0.4695(6) 0.3070(6) 0.057(3) Uani 1 1 d . . . H12C H 0.1246 0.4926 0.3485 0.068 Uiso 1 1 calc R . . C122 C 0.1202(7) 0.5150(6) 0.2523(6) 0.060(3) Uani 1 1 d . . . C123 C 0.1047(7) 0.4771(6) 0.1911(6) 0.060(4) Uani 1 1 d . . . H12D H 0.1104 0.5057 0.1514 0.072 Uiso 1 1 calc R . . C124 C 0.0815(7) 0.3992(6) 0.1884(5) 0.058(3) Uani 1 1 d . . . H12E H 0.0698 0.3759 0.1472 0.070 Uiso 1 1 calc R . . C125 C 0.1464(8) 0.5965(7) 0.2541(7) 0.069(4) Uani 1 1 d . . . C126 C 0.1287(8) 0.6444(6) 0.3076(6) 0.067(4) Uani 1 1 d . . . H12F H 0.0966 0.6237 0.3421 0.080 Uiso 1 1 calc R . . C127 C 0.1549(9) 0.7181(7) 0.3126(8) 0.085(5) Uani 1 1 d . . . H12G H 0.1394 0.7490 0.3492 0.102 Uiso 1 1 calc R . . C128 C 0.2037(11) 0.7486(8) 0.2653(9) 0.097(5) Uani 1 1 d . . . H12H H 0.2219 0.8010 0.2695 0.117 Uiso 1 1 calc R . . C129 C 0.2274(9) 0.7049(8) 0.2109(8) 0.092(5) Uani 1 1 d . . . H12I H 0.2624 0.7262 0.1785 0.110 Uiso 1 1 calc R . . C130 C 0.1975(8) 0.6271(6) 0.2056(7) 0.072(4) Uani 1 1 d . . . H13B H 0.2123 0.5958 0.1691 0.087 Uiso 1 1 calc R . . P1 P 0.2983(4) -0.2172(3) 0.5000 0.0748(17) Uani 1 2 d SD . . F11 F 0.2872(9) -0.3077(5) 0.5000 0.143(6) Uani 1 2 d SD A . F12 F 0.3095(7) -0.1244(5) 0.5000 0.117(4) Uani 1 2 d SD A . F13A F 0.3694(9) -0.2212(6) 0.5505(6) 0.136(7) Uani 0.81(2) 1 d PD A 1 F14A F 0.2395(10) -0.2144(7) 0.5602(9) 0.193(11) Uani 0.81(2) 1 d PD A 1 F13B F 0.3001(16) -0.2148(10) 0.5750(6) 0.024(11) Uiso 0.19(2) 1 d PD A 2 F14B F 0.2064(9) -0.2019(12) 0.5000 0.105(17) Uiso 0.38(4) 2 d SPD A 2 P2 P -0.3342(7) -0.1430(4) 0.0000 0.151(4) Uani 1 2 d SD . . F21 F -0.3288(18) -0.2329(8) 0.0000 0.323(17) Uani 1 2 d SD . . F22 F -0.3283(19) -0.0537(9) 0.0000 0.35(2) Uani 1 2 d SD . . F23 F -0.2621(10) -0.1426(9) 0.0549(6) 0.256(8) Uani 1 1 d D . . F24 F -0.3989(7) -0.1456(7) 0.0549(6) 0.174(5) Uani 1 1 d D . . C022 C -0.500(4) -0.030(3) 0.0000 0.127(19) Uiso 0.50 2 d SP . . C024 C -0.3572(18) -0.0133(18) 0.0000 0.113(9) Uiso 1 2 d S . . O001 O -0.1195(7) -0.2173(6) 0.0000 0.056(3) Uani 1 2 d S . . C003 C 0.007(3) -0.141(3) 0.5000 0.122(17) Uiso 0.50 2 d SP . . C002 C -0.083(2) -0.272(2) 0.0473(16) 0.115(11) Uiso 0.50 1 d P . . C001 C -0.056(3) -0.137(3) 0.0000 0.105(14) Uiso 0.50 2 d SP . . C004 C 0.427(4) 0.042(4) 0.5000 0.17(2) Uiso 0.50 2 d SP . . C005 C 0.0000 0.0000 0.5000 0.17(4) Uiso 0.50 4 d SP . . C006 C -0.200(4) -0.256(3) 0.0000 0.136(19) Uiso 0.50 2 d SP . . C007 C 0.049(4) -0.321(3) 0.5000 0.15(2) Uiso 0.50 2 d SP . . C008 C -0.064(2) -0.203(2) 0.0543(19) 0.133(13) Uiso 0.50 1 d P . . C009 C -0.004(3) -0.069(4) 0.5000 0.132(18) Uiso 0.50 2 d SP . . C010 C -0.165(3) -0.178(2) -0.068(2) 0.148(15) Uiso 0.50 1 d P . . C011 C -0.424(3) -0.059(3) 0.0000 0.098(14) Uiso 0.50 2 d SP . . 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 Ni1 0.0689(14) 0.0120(10) 0.0367(11) 0.000 0.000 -0.0004(10) N11 0.061(6) 0.008(4) 0.047(5) -0.005(4) 0.005(4) 0.001(4) C12 0.092(10) 0.023(6) 0.050(7) 0.010(5) -0.006(7) 0.005(6) C13 0.073(9) 0.041(8) 0.055(8) 0.013(6) -0.019(7) 0.010(6) C14 0.083(10) 0.044(8) 0.052(8) -0.002(6) -0.011(7) 0.007(7) C15 0.089(9) 0.019(6) 0.039(6) -0.001(5) -0.015(6) 0.000(6) C16 0.065(8) 0.017(6) 0.035(6) 0.003(4) 0.004(6) 0.000(5) N17 0.067(7) 0.023(5) 0.033(5) -0.005(4) -0.009(5) -0.003(4) C18 0.064(8) 0.023(7) 0.044(7) 0.002(5) 0.006(6) -0.001(5) C19 0.080(8) 0.020(6) 0.038(6) -0.005(5) 0.003(6) -0.002(6) C110 0.083(9) 0.020(6) 0.027(6) 0.007(5) -0.002(6) 0.009(6) C111 0.088(9) 0.026(6) 0.035(6) 0.004(5) -0.022(7) 0.000(6) C112 0.070(8) 0.011(6) 0.042(6) 0.005(5) -0.019(6) 0.000(5) N113 0.060(6) 0.017(5) 0.042(5) -0.001(4) -0.001(5) -0.001(4) C114 0.061(8) 0.037(7) 0.049(7) 0.000(6) -0.004(6) -0.008(7) C115 0.097(11) 0.054(9) 0.055(8) -0.008(6) -0.023(8) -0.008(8) C116 0.103(11) 0.055(9) 0.052(8) 0.007(6) -0.044(8) -0.008(8) C117 0.114(11) 0.037(7) 0.043(7) -0.004(6) -0.013(7) 0.001(8) C118 0.093(9) 0.020(6) 0.035(6) 0.006(5) -0.007(6) 0.005(6) C119 0.072(8) 0.014(6) 0.060(8) 0.003(6) -0.002(6) -0.001(5) C120 0.089(10) 0.019(6) 0.052(8) 0.005(5) -0.007(6) 0.008(6) C121 0.092(10) 0.023(7) 0.056(8) -0.010(5) -0.005(7) -0.001(6) C122 0.070(9) 0.020(7) 0.091(10) -0.003(6) -0.001(7) 0.003(5) C123 0.092(10) 0.018(7) 0.071(9) 0.010(5) 0.014(7) -0.002(6) C124 0.104(10) 0.018(6) 0.052(7) 0.005(5) 0.000(6) 0.004(6) C125 0.066(9) 0.031(7) 0.111(12) -0.004(8) -0.019(8) 0.004(6) C126 0.085(10) 0.017(7) 0.098(10) -0.012(6) -0.022(8) 0.001(6) C127 0.103(12) 0.021(8) 0.131(13) -0.006(7) 0.010(10) 0.002(7) C128 0.106(13) 0.030(9) 0.156(16) -0.015(10) -0.050(12) 0.023(9) C129 0.091(11) 0.034(9) 0.151(15) 0.028(9) 0.002(10) -0.012(8) C130 0.077(10) 0.022(7) 0.119(11) 0.005(7) -0.001(9) 0.007(6) P1 0.113(5) 0.041(3) 0.070(4) 0.000 0.000 0.028(3) F11 0.322(19) 0.041(7) 0.065(7) 0.000 0.000 0.061(9) F12 0.154(12) 0.050(7) 0.147(10) 0.000 0.000 0.001(7) F13A 0.186(17) 0.101(10) 0.122(9) 0.028(7) -0.075(10) -0.003(8) F14A 0.186(18) 0.098(10) 0.29(3) -0.085(11) 0.166(17) -0.031(10) P2 0.240(12) 0.071(6) 0.142(7) 0.000 0.000 -0.007(6) F21 0.59(5) 0.060(13) 0.32(3) 0.000 0.000 -0.01(2) F22 0.40(5) 0.078(17) 0.57(5) 0.000 0.000 0.03(2) F23 0.34(2) 0.278(19) 0.147(10) -0.066(11) -0.125(13) 0.026(15) F24 0.147(10) 0.168(12) 0.209(12) 0.003(9) 0.053(9) -0.022(8) O001 0.082(9) 0.038(7) 0.049(7) 0.000 0.000 -0.015(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 Ni1 N17 1.984(8) 2 ? Ni1 N17 1.984(8) . y Ni1 N11 2.092(8) 2 ? Ni1 N11 2.092(8) . y Ni1 N113 2.107(8) 2 ? Ni1 N113 2.107(8) . y N11 C16 1.349(11) . ? N11 C12 1.368(12) . ? C12 C13 1.349(14) . ? C13 C14 1.377(15) . ? C14 C15 1.393(14) . ? C15 C16 1.375(13) . ? C16 C18 1.506(13) . ? N17 C18 1.316(12) . ? N17 C112 1.346(11) . ? C18 C19 1.387(13) . ? C19 C110 1.386(13) . ? C110 C111 1.398(13) . ? C110 C119 1.475(13) . ? C111 C112 1.360(13) . ? C112 C118 1.483(14) . ? N113 C114 1.327(12) . ? N113 C118 1.357(11) . ? C114 C115 1.349(15) . ? C115 C116 1.389(15) . ? C116 C117 1.365(15) . ? C117 C118 1.388(15) . ? C119 C124 1.386(13) . ? C119 C120 1.401(13) . ? C120 C121 1.373(13) . ? C121 C122 1.364(14) . ? C122 C123 1.430(15) . ? C122 C125 1.462(15) . ? C123 C124 1.390(13) . ? C125 C126 1.396(16) . ? C125 C130 1.400(16) . ? C126 C127 1.340(15) . ? C127 C128 1.36(2) . ? C128 C129 1.40(2) . ? C129 C130 1.427(16) . ? P1 F13B 1.529(13) 6_556 ? P1 F13B 1.529(13) . ? P1 F14B 1.540(15) . ? P1 F11 1.563(9) . ? P1 F13A 1.562(9) . ? P1 F13A 1.562(9) 6_556 ? P1 F14A 1.566(11) 6_556 ? P1 F14A 1.566(11) . ? P1 F12 1.601(9) . ? P2 F22 1.534(15) . ? P2 F21 1.543(13) . ? P2 F24 1.548(10) 6 ? P2 F24 1.548(10) . ? P2 F23 1.633(12) 6 ? P2 F23 1.633(12) . ? P2 C011 2.06(6) . ? P2 C024 2.26(3) . ? F22 C024 0.84(3) . ? F22 C011 1.57(6) . ? F23 C010 1.74(4) 6 ? C022 C022 1.04(9) 5_455 ? C022 C011 1.35(6) . ? C022 C011 1.98(9) 5_455 ? C024 C011 1.34(5) . ? O001 C008 1.46(4) 6 ? O001 C008 1.46(4) . ? O001 C006 1.48(6) . ? O001 C002 1.47(3) 6 ? O001 C002 1.47(3) . ? O001 C010 1.71(4) . ? O001 C010 1.71(4) 6 ? O001 C001 1.74(5) . ? C003 C009 1.24(6) . ? C002 C008 1.24(4) . ? C002 C002 1.93(6) 6 ? C001 C008 1.59(5) 6 ? C001 C008 1.59(5) . ? C005 C009 1.19(6) . ? C005 C009 1.19(6) 5_556 ? C006 C010 2.01(6) . ? C006 C010 2.01(6) 6 ? C008 C010 1.74(5) 6 ? C010 C008 1.74(5) 6 ? C010 F23 1.74(4) 6 ? C011 C022 1.98(9) 5_455 ? 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 N17 Ni1 N17 178.3(4) 2 . y N17 Ni1 N11 77.9(3) 2 2 ? N17 Ni1 N11 100.9(3) . 2 y N17 Ni1 N11 100.9(3) 2 . ? N17 Ni1 N11 77.9(3) . . y N11 Ni1 N11 92.9(4) 2 . y N17 Ni1 N113 78.0(3) 2 2 ? N17 Ni1 N113 103.2(3) . 2 y N11 Ni1 N113 155.9(3) 2 2 ? N11 Ni1 N113 91.6(3) . 2 y N17 Ni1 N113 103.2(3) 2 . ? N17 Ni1 N113 78.0(3) . . y N11 Ni1 N113 91.6(3) 2 . ? N11 Ni1 N113 155.9(3) . . y N113 Ni1 N113 93.9(4) 2 . y C16 N11 C12 116.1(9) . . ? C16 N11 Ni1 115.8(6) . . ? C12 N11 Ni1 128.1(7) . . ? C13 C12 N11 123.8(10) . . ? C12 C13 C14 119.8(10) . . ? C13 C14 C15 117.9(11) . . ? C16 C15 C14 119.5(10) . . ? N11 C16 C15 122.9(9) . . ? N11 C16 C18 112.1(9) . . ? C15 C16 C18 125.0(9) . . ? C18 N17 C112 120.3(8) . . ? C18 N17 Ni1 119.3(7) . . ? C112 N17 Ni1 120.3(6) . . ? N17 C18 C19 121.6(9) . . ? N17 C18 C16 114.7(9) . . ? C19 C18 C16 123.6(10) . . ? C110 C19 C18 119.5(10) . . ? C19 C110 C111 117.2(9) . . ? C19 C110 C119 120.6(10) . . ? C111 C110 C119 122.2(9) . . ? C112 C111 C110 120.5(9) . . ? N17 C112 C111 120.8(9) . . ? N17 C112 C118 112.5(8) . . ? C111 C112 C118 126.7(9) . . ? C114 N113 C118 117.8(9) . . ? C114 N113 Ni1 128.1(7) . . ? C118 N113 Ni1 114.0(7) . . ? N113 C114 C115 124.6(11) . . ? C114 C115 C116 118.2(11) . . ? C117 C116 C115 118.7(11) . . ? C116 C117 C118 120.0(11) . . ? N113 C118 C117 120.6(10) . . ? N113 C118 C112 115.2(9) . . ? C117 C118 C112 124.0(9) . . ? C124 C119 C120 117.8(9) . . ? C124 C119 C110 122.2(9) . . ? C120 C119 C110 119.9(9) . . ? C121 C120 C119 120.9(10) . . ? C122 C121 C120 123.3(11) . . ? C121 C122 C123 116.1(10) . . ? C121 C122 C125 123.3(11) . . ? C123 C122 C125 120.6(11) . . ? C124 C123 C122 121.3(10) . . ? C119 C124 C123 120.6(11) . . ? C126 C125 C130 117.2(12) . . ? C126 C125 C122 121.3(13) . . ? C130 C125 C122 121.2(12) . . ? C127 C126 C125 123.2(14) . . ? C126 C127 C128 120.0(15) . . ? C127 C128 C129 121.5(15) . . ? C128 C129 C130 117.7(14) . . ? C125 C130 C129 120.4(13) . . ? F13B P1 F13B 176.2(16) 6_556 . ? F13B P1 F14B 90.8(10) 6_556 . ? F13B P1 F14B 90.8(10) . . ? F13B P1 F11 91.7(7) 6_556 . ? F13B P1 F11 91.7(7) . . ? F14B P1 F11 93.1(9) . . ? F13B P1 F13A 130.3(14) 6_556 . ? F13B P1 F13A 47.8(9) . . ? F14B P1 F13A 138.3(6) . . ? F11 P1 F13A 92.5(6) . . ? F13B P1 F13A 47.8(9) 6_556 6_556 ? F13B P1 F13A 130.3(14) . 6_556 ? F14B P1 F13A 138.3(6) . 6_556 ? F11 P1 F13A 92.5(6) . 6_556 ? F13A P1 F13A 82.5(12) . 6_556 ? F13B P1 F14A 39.4(9) 6_556 6_556 ? F13B P1 F14A 142.6(16) . 6_556 ? F14B P1 F14A 52.0(8) . 6_556 ? F11 P1 F14A 87.6(6) . 6_556 ? F13A P1 F14A 169.6(12) . 6_556 ? F13A P1 F14A 87.1(8) 6_556 6_556 ? F13B P1 F14A 142.6(16) 6_556 . ? F13B P1 F14A 39.4(9) . . ? F14B P1 F14A 52.0(8) . . ? F11 P1 F14A 87.6(6) . . ? F13A P1 F14A 87.1(8) . . ? F13A P1 F14A 169.6(12) 6_556 . ? F14A P1 F14A 103.3(16) 6_556 . ? F13B P1 F12 88.3(7) 6_556 . ? F13B P1 F12 88.3(7) . . ? F14B P1 F12 86.8(8) . . ? F11 P1 F12 179.9(8) . . ? F13A P1 F12 87.6(5) . . ? F13A P1 F12 87.6(5) 6_556 . ? F14A P1 F12 92.4(5) 6_556 . ? F14A P1 F12 92.4(5) . . ? F22 P2 F21 173.1(17) . . ? F22 P2 F24 94.1(9) . 6 ? F21 P2 F24 90.6(9) . 6 ? F22 P2 F24 94.1(9) . . ? F21 P2 F24 90.6(9) . . ? F24 P2 F24 92.7(12) 6 . ? F22 P2 F23 87.1(9) . 6 ? F21 P2 F23 87.9(9) . 6 ? F24 P2 F23 90.4(7) 6 6 ? F24 P2 F23 176.6(10) . 6 ? F22 P2 F23 87.1(9) . . ? F21 P2 F23 87.9(9) . . ? F24 P2 F23 176.6(10) 6 . ? F24 P2 F23 90.4(7) . . ? F23 P2 F23 86.4(13) 6 . ? F22 P2 C011 49.2(17) . . ? F21 P2 C011 137.7(19) . . ? F24 P2 C011 61.8(10) 6 . ? F24 P2 C011 61.8(10) . . ? F23 P2 C011 121.1(10) 6 . ? F23 P2 C011 121.1(10) . . ? F22 P2 C024 13.3(14) . . ? F21 P2 C024 173.6(14) . . ? F24 P2 C024 85.0(8) 6 . ? F24 P2 C024 85.0(8) . . ? F23 P2 C024 96.7(8) 6 . ? F23 P2 C024 96.7(8) . . ? C011 P2 C024 35.9(15) . . ? C024 F22 P2 142(4) . . ? C024 F22 C011 59(3) . . ? P2 F22 C011 83(2) . . ? P2 F23 C010 141.0(17) . 6 ? C022 C022 C011 111(9) 5_455 . ? C022 C022 C011 39(6) 5_455 5_455 ? C011 C022 C011 151(4) . 5_455 ? F22 C024 C011 89(4) . . ? F22 C024 P2 25(3) . . ? C011 C024 P2 64(3) . . ? C008 O001 C008 99(3) 6 . ? C008 O001 C006 129.6(17) 6 . ? C008 O001 C006 129.6(17) . . ? C008 O001 C002 50.0(17) 6 6 ? C008 O001 C002 111(2) . 6 ? C006 O001 C002 95(2) . 6 ? C008 O001 C002 111(2) 6 . ? C008 O001 C002 50.0(17) . . ? C006 O001 C002 95(2) . . ? C002 O001 C002 82(3) 6 . ? C008 O001 C010 65.8(19) 6 . ? C008 O001 C010 145(2) . . ? C006 O001 C010 77.6(19) . . ? C002 O001 C010 84.1(19) 6 . ? C002 O001 C010 163(2) . . ? C008 O001 C010 145(2) 6 6 ? C008 O001 C010 65.8(19) . 6 ? C006 O001 C010 77.6(19) . 6 ? C002 O001 C010 163(2) 6 6 ? C002 O001 C010 84.1(19) . 6 ? C010 O001 C010 108(3) . 6 ? C008 O001 C001 58.9(18) 6 . ? C008 O001 C001 58.9(18) . . ? C006 O001 C001 154(3) . . ? C002 O001 C001 105.1(19) 6 . ? C002 O001 C001 105.1(19) . . ? C010 O001 C001 87.2(17) . . ? C010 O001 C001 87.2(17) 6 . ? C008 C002 O001 64(3) . . ? C008 C002 C002 97(3) . 6 ? O001 C002 C002 49.1(13) . 6 ? C008 C001 C008 88(4) 6 . ? C008 C001 O001 52(2) 6 . ? C008 C001 O001 52(2) . . ? C009 C005 C009 179.993(9) . 5_556 ? O001 C006 C010 56(2) . . ? O001 C006 C010 56(2) . 6 ? C010 C006 C010 87(3) . 6 ? C002 C008 O001 66(3) . . ? C002 C008 C001 129(4) . . ? O001 C008 C001 69(2) . . ? C002 C008 C010 91(3) . 6 ? O001 C008 C010 64(2) . 6 ? C001 C008 C010 91(3) . 6 ? C005 C009 C003 169(6) . . ? O001 C010 C008 49.9(18) . 6 ? O001 C010 F23 115(3) . 6 ? C008 C010 F23 161(3) 6 6 ? O001 C010 C006 46.0(19) . . ? C008 C010 C006 90(3) 6 . ? F23 C010 C006 82(3) 6 . ? C022 C011 C024 123(5) . . ? C022 C011 F22 156(5) . . ? C024 C011 F22 32.3(19) . . ? C022 C011 C022 29(4) . 5_455 ? C024 C011 C022 94(3) . 5_455 ? F22 C011 C022 126(3) . 5_455 ? C022 C011 P2 157(4) . . ? C024 C011 P2 80(3) . . ? F22 C011 P2 47.6(16) . . ? C022 C011 P2 174(4) 5_455 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.771 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.120 data_mh008 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H45 B2 F8 N8 O0.50 Zn' _chemical_formula_weight 1101.01 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2890(10) _cell_length_b 13.6880(10) _cell_length_c 20.2780(10) _cell_angle_alpha 97.010(10) _cell_angle_beta 99.500(10) _cell_angle_gamma 93.070(10) _cell_volume 2516.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1130 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8045 _exptl_absorpt_correction_T_max 0.9559 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17830 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.1179 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11395 _reflns_number_gt 7274 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+3.4983P] 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 11395 _refine_ls_number_parameters 785 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1332 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.1566 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.05972(4) 0.44580(3) 0.22880(2) 0.02602(13) Uani 1 1 d . . . C2A C -0.0777(4) 0.6462(3) 0.20423(19) 0.0314(9) Uani 1 1 d . . . H2A H -0.0358 0.6671 0.2501 0.038 Uiso 1 1 calc R . . C2B C 0.3700(4) 0.5023(3) 0.19197(19) 0.0324(9) Uani 1 1 d . . . H2B H 0.3329 0.4638 0.1498 0.039 Uiso 1 1 calc R . . C3A C -0.1649(4) 0.7083(3) 0.1697(2) 0.0343(9) Uani 1 1 d . . . H3A H -0.1844 0.7704 0.1916 0.041 Uiso 1 1 calc R . . C3B C 0.5123(4) 0.5451(3) 0.2030(2) 0.0356(9) Uani 1 1 d . . . H3B H 0.5715 0.5367 0.1690 0.043 Uiso 1 1 calc R . . C4A C -0.2231(4) 0.6789(3) 0.1029(2) 0.0393(10) Uani 1 1 d . . . H4A H -0.2822 0.7209 0.0779 0.047 Uiso 1 1 calc R . . C4B C 0.5654(4) 0.6003(3) 0.2647(2) 0.0368(9) Uani 1 1 d . . . H4B H 0.6622 0.6307 0.2736 0.044 Uiso 1 1 calc R . . C5A C -0.1948(4) 0.5876(3) 0.07243(19) 0.0317(9) Uani 1 1 d . . . H5A H -0.2345 0.5658 0.0264 0.038 Uiso 1 1 calc R . . C5B C 0.4774(4) 0.6114(3) 0.31358(19) 0.0322(9) Uani 1 1 d . . . H5B H 0.5132 0.6485 0.3564 0.039 Uiso 1 1 calc R . . C6A C -0.1074(4) 0.5284(3) 0.11040(17) 0.0254(8) Uani 1 1 d . . . C6B C 0.3348(4) 0.5668(3) 0.29869(17) 0.0264(8) Uani 1 1 d . . . C7A C -0.0729(4) 0.4272(3) 0.08359(17) 0.0246(8) Uani 1 1 d . . . C7B C 0.2299(4) 0.5766(3) 0.34639(17) 0.0259(8) Uani 1 1 d . . . C9A C 0.0405(4) 0.2875(3) 0.11233(17) 0.0256(8) Uani 1 1 d . . . C9B C -0.0018(4) 0.5235(3) 0.36377(17) 0.0242(8) Uani 1 1 d . . . C10A C -0.0027(4) 0.2387(3) 0.04731(18) 0.0289(8) Uani 1 1 d . . . H10A H 0.0226 0.1731 0.0363 0.035 Uiso 1 1 calc R . . C10B C 0.0154(4) 0.5855(3) 0.42437(17) 0.0284(8) Uani 1 1 d . . . H10B H -0.0608 0.5870 0.4504 0.034 Uiso 1 1 calc R . . C11A C -0.0838(4) 0.2867(3) -0.00194(17) 0.0269(8) Uani 1 1 d . . . C11B C 0.1448(4) 0.6461(3) 0.44745(17) 0.0280(8) Uani 1 1 d . . . C12A C -0.1169(4) 0.3833(3) 0.01759(18) 0.0281(8) Uani 1 1 d . . . H12A H -0.1697 0.4190 -0.0146 0.034 Uiso 1 1 calc R . . C12B C 0.2534(4) 0.6396(3) 0.40646(18) 0.0309(9) Uani 1 1 d . . . H12B H 0.3434 0.6787 0.4202 0.037 Uiso 1 1 calc R . . C13A C 0.1297(4) 0.2453(3) 0.16877(17) 0.0270(8) Uani 1 1 d . . . C13B C -0.1359(4) 0.4579(3) 0.33369(18) 0.0259(8) Uani 1 1 d . . . C15A C 0.2255(4) 0.2703(3) 0.28317(18) 0.0304(8) Uani 1 1 d . . . H15A H 0.2368 0.3101 0.3258 0.036 Uiso 1 1 calc R . . C15B C -0.2538(4) 0.3544(3) 0.23955(19) 0.0304(8) Uani 1 1 d . . . H15B H -0.2550 0.3244 0.1947 0.036 Uiso 1 1 calc R . . C16A C 0.2924(4) 0.1822(3) 0.27858(19) 0.0353(9) Uani 1 1 d . . . H16A H 0.3473 0.1611 0.3174 0.042 Uiso 1 1 calc R . . C16B C -0.3744(4) 0.3359(3) 0.2704(2) 0.0375(10) Uani 1 1 d . . . H16B H -0.4560 0.2934 0.2473 0.045 Uiso 1 1 calc R . . C17A C 0.2774(4) 0.1260(3) 0.2166(2) 0.0392(10) Uani 1 1 d . . . H17A H 0.3243 0.0661 0.2121 0.047 Uiso 1 1 calc R . . C17B C -0.3720(4) 0.3808(3) 0.3351(2) 0.0357(9) Uani 1 1 d . . . H17B H -0.4519 0.3686 0.3576 0.043 Uiso 1 1 calc R . . C18A C 0.1937(4) 0.1565(3) 0.1605(2) 0.0379(10) Uani 1 1 d . . . H18A H 0.1807 0.1175 0.1175 0.045 Uiso 1 1 calc R . . C18B C -0.2528(4) 0.4437(3) 0.36738(19) 0.0315(9) Uani 1 1 d . . . H18B H -0.2507 0.4766 0.4116 0.038 Uiso 1 1 calc R . . C19A C -0.1302(4) 0.2390(3) -0.07270(17) 0.0283(8) Uani 1 1 d . . . C19B C 0.1643(4) 0.7164(3) 0.51021(17) 0.0291(8) Uani 1 1 d . . . C20A C -0.0647(4) 0.1560(3) -0.09784(18) 0.0305(8) Uani 1 1 d . . . H20A H 0.0068 0.1272 -0.0687 0.037 Uiso 1 1 calc R . . C20B C 0.2901(4) 0.7801(3) 0.53212(19) 0.0363(9) Uani 1 1 d . . . H20B H 0.3646 0.7800 0.5052 0.044 Uiso 1 1 calc R . . C21A C -0.1029(4) 0.1156(3) -0.16471(18) 0.0320(9) Uani 1 1 d . . . H21A H -0.0572 0.0590 -0.1804 0.038 Uiso 1 1 calc R . . C21B C 0.3089(4) 0.8432(3) 0.59212(19) 0.0349(9) Uani 1 1 d . . . H21B H 0.3959 0.8857 0.6052 0.042 Uiso 1 1 calc R . . C22A C -0.2068(4) 0.1552(3) -0.21028(18) 0.0302(8) Uani 1 1 d . . . C22B C 0.2039(4) 0.8463(3) 0.63389(18) 0.0311(8) Uani 1 1 d . . . C23A C -0.2743(4) 0.2365(3) -0.18387(19) 0.0359(9) Uani 1 1 d . . . H23A H -0.3470 0.2647 -0.2128 0.043 Uiso 1 1 calc R . . C23B C 0.0768(4) 0.7837(3) 0.61153(19) 0.0359(9) Uani 1 1 d . . . H23B H 0.0013 0.7850 0.6380 0.043 Uiso 1 1 calc R . . C24A C -0.2380(4) 0.2770(3) -0.11684(19) 0.0345(9) Uani 1 1 d . . . H24A H -0.2873 0.3315 -0.1006 0.041 Uiso 1 1 calc R . . C24B C 0.0583(4) 0.7200(3) 0.55184(19) 0.0368(9) Uani 1 1 d . . . H24B H -0.0288 0.6777 0.5388 0.044 Uiso 1 1 calc R . . C25A C -0.2419(4) 0.1138(3) -0.28262(18) 0.0345(9) Uani 1 1 d . . . C25B C 0.2279(4) 0.9104(3) 0.69985(18) 0.0311(9) Uani 1 1 d . . . C26A C -0.1486(6) 0.0519(4) -0.3123(2) 0.0540(12) Uani 1 1 d . . . H26A H -0.0587 0.0387 -0.2863 0.065 Uiso 1 1 calc R . . C26B C 0.3167(5) 0.9974(3) 0.7118(2) 0.0424(10) Uani 1 1 d . . . H26B H 0.3628 1.0173 0.6766 0.051 Uiso 1 1 calc R . . C27A C -0.1851(7) 0.0095(4) -0.3791(2) 0.0650(15) Uani 1 1 d . . . H27A H -0.1220 -0.0342 -0.3979 0.078 Uiso 1 1 calc R . . C27B C 0.3399(5) 1.0564(3) 0.7737(2) 0.0466(11) Uani 1 1 d . . . H27B H 0.4002 1.1163 0.7804 0.056 Uiso 1 1 calc R . . C28A C -0.3134(6) 0.0306(4) -0.4183(2) 0.0628(15) Uani 1 1 d . . . H28A H -0.3378 0.0023 -0.4642 0.075 Uiso 1 1 calc R . . C28B C 0.2755(4) 1.0281(3) 0.8258(2) 0.0390(10) Uani 1 1 d . . . H28B H 0.2923 1.0679 0.8685 0.047 Uiso 1 1 calc R . . C29A C -0.4043(5) 0.0921(4) -0.3907(2) 0.0521(12) Uani 1 1 d . . . H29A H -0.4920 0.1070 -0.4177 0.062 Uiso 1 1 calc R . . C29B C 0.1863(4) 0.9416(3) 0.8152(2) 0.0384(10) Uani 1 1 d . . . H29B H 0.1412 0.9218 0.8507 0.046 Uiso 1 1 calc R . . C30A C -0.3700(5) 0.1331(3) -0.32362(19) 0.0415(10) Uani 1 1 d . . . H30A H -0.4354 0.1754 -0.3052 0.050 Uiso 1 1 calc R . . C30B C 0.1628(4) 0.8840(3) 0.7530(2) 0.0376(9) Uani 1 1 d . . . H30B H 0.1007 0.8249 0.7462 0.045 Uiso 1 1 calc R . . N1A N -0.0501(3) 0.5578(2) 0.17534(14) 0.0268(7) Uani 1 1 d . . . N1B N 0.2832(3) 0.5132(2) 0.23839(14) 0.0272(7) Uani 1 1 d . . . N8A N 0.0044(3) 0.3793(2) 0.12943(14) 0.0250(6) Uani 1 1 d . . . N8B N 0.1038(3) 0.5200(2) 0.32580(14) 0.0260(7) Uani 1 1 d . . . N14A N 0.1455(3) 0.3012(2) 0.22950(14) 0.0268(7) Uani 1 1 d . . . N14B N -0.1372(3) 0.4129(2) 0.27104(14) 0.0264(7) Uani 1 1 d . . . N40 N 0.1747(5) 1.0043(3) -0.0184(2) 0.0587(11) Uani 1 1 d . . . C41 C 0.2754(5) 0.9881(3) 0.0179(2) 0.0422(10) Uani 1 1 d . . . C42 C 0.4010(5) 0.9684(4) 0.0648(2) 0.0547(12) Uani 1 1 d . . . H42A H 0.4561 0.9191 0.0426 0.082 Uiso 1 1 calc R . . H42B H 0.3686 0.9433 0.1036 0.082 Uiso 1 1 calc R . . H42C H 0.4637 1.0295 0.0802 0.082 Uiso 1 1 calc R . . N43 N -0.1592(6) 0.7725(4) 0.3386(2) 0.0901(17) Uani 1 1 d . . . C44 C -0.1437(6) 0.8226(4) 0.3879(3) 0.0577(13) Uani 1 1 d . . . C45 C -0.1247(6) 0.8859(4) 0.4514(2) 0.0689(15) Uani 1 1 d . . . H45A H -0.1614 0.9501 0.4440 0.103 Uiso 1 1 calc R . . H45B H -0.0205 0.8948 0.4713 0.103 Uiso 1 1 calc R . . H45C H -0.1793 0.8556 0.4821 0.103 Uiso 1 1 calc R . . B1 B 0.3495(4) 0.3120(5) 0.4815(2) 0.068(4) Uani 0.583(12) 1 d PD A 1 F1 F 0.4603(7) 0.3547(6) 0.4540(4) 0.103(4) Uani 0.583(12) 1 d PD A 1 F2 F 0.2640(8) 0.2433(5) 0.4329(3) 0.076(3) Uani 0.583(12) 1 d PD A 1 F3 F 0.4099(6) 0.2655(7) 0.5353(3) 0.094(4) Uani 0.583(12) 1 d PD A 1 F4 F 0.2635(6) 0.3844(5) 0.5037(5) 0.111(5) Uani 0.583(12) 1 d PD A 1 B1B B 0.3486(6) 0.3418(5) 0.4763(3) 0.050(5) Uani 0.417(12) 1 d PD A 2 F1B F 0.3248(13) 0.3312(7) 0.5408(3) 0.091(4) Uani 0.417(12) 1 d PD A 2 F2B F 0.2468(7) 0.4012(6) 0.4471(6) 0.088(4) Uani 0.417(12) 1 d PD A 2 F3B F 0.4883(6) 0.3850(8) 0.4796(6) 0.081(4) Uani 0.417(12) 1 d PD A 2 F4B F 0.3343(13) 0.2499(6) 0.4377(5) 0.096(4) Uani 0.417(12) 1 d PD A 2 B2 B 0.4843(3) 0.2862(2) 0.06272(14) 0.0594(17) Uani 0.764(5) 1 d PD B 3 F5 F 0.5802(4) 0.3700(3) 0.0774(3) 0.1062(18) Uani 0.764(5) 1 d PD B 3 F6 F 0.5194(5) 0.2242(3) 0.1111(2) 0.133(3) Uani 0.764(5) 1 d PD B 3 F7 F 0.4949(5) 0.2379(4) -0.00020(18) 0.138(3) Uani 0.764(5) 1 d PD B 3 F8 F 0.3427(3) 0.3130(3) 0.0626(2) 0.0953(15) Uani 0.764(5) 1 d PD B 3 B2B B 0.4993(7) 0.2769(6) 0.0520(4) 0.0594(17) Uani 0.236(5) 1 d PD B 4 F5B F 0.5339(12) 0.3448(8) 0.0107(6) 0.107(6) Uani 0.236(5) 1 d PD B 4 F6B F 0.6259(9) 0.2377(8) 0.0803(6) 0.082(5) Uani 0.236(5) 1 d PD B 4 F7B F 0.4035(11) 0.2018(7) 0.0144(6) 0.068(5) Uani 0.236(5) 1 d PD B 4 F8B F 0.4341(12) 0.3233(9) 0.1028(5) 0.0953(15) Uani 0.236(5) 1 d PD B 4 O1 O -0.4337(8) 0.4594(6) -0.0445(4) 0.083(2) 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 Zn1 0.0268(2) 0.0291(2) 0.0203(2) -0.00308(17) 0.00359(15) 0.00115(17) C2A 0.033(2) 0.030(2) 0.029(2) -0.0058(17) 0.0065(16) 0.0006(16) C2B 0.040(2) 0.033(2) 0.024(2) -0.0015(16) 0.0089(16) 0.0053(17) C3A 0.040(2) 0.026(2) 0.037(2) -0.0022(17) 0.0111(17) 0.0034(17) C3B 0.032(2) 0.043(2) 0.036(2) 0.0071(19) 0.0145(17) 0.0069(18) C4A 0.047(2) 0.033(2) 0.037(2) 0.0030(19) 0.0054(18) 0.0123(18) C4B 0.0244(19) 0.043(2) 0.044(2) 0.009(2) 0.0080(17) -0.0004(17) C5A 0.040(2) 0.030(2) 0.023(2) 0.0017(16) 0.0022(16) 0.0047(17) C5B 0.0247(18) 0.039(2) 0.031(2) 0.0002(17) 0.0026(15) 0.0000(16) C6A 0.0285(18) 0.025(2) 0.0221(19) 0.0004(15) 0.0056(14) 0.0003(15) C6B 0.0283(18) 0.030(2) 0.0208(18) 0.0030(15) 0.0018(14) 0.0053(15) C7A 0.0237(17) 0.0245(19) 0.0252(19) 0.0012(15) 0.0057(14) -0.0001(14) C7B 0.0257(18) 0.031(2) 0.0188(18) 0.0001(15) -0.0004(14) 0.0021(15) C9A 0.0271(18) 0.025(2) 0.0235(19) -0.0013(15) 0.0050(14) 0.0025(15) C9B 0.0252(18) 0.028(2) 0.0192(18) 0.0032(15) 0.0041(14) 0.0038(15) C10A 0.034(2) 0.026(2) 0.026(2) -0.0008(16) 0.0054(15) 0.0040(16) C10B 0.0292(19) 0.032(2) 0.0227(19) -0.0001(16) 0.0052(15) 0.0004(16) C11A 0.0281(18) 0.033(2) 0.0174(18) -0.0030(15) 0.0035(14) 0.0010(16) C11B 0.0310(19) 0.032(2) 0.0195(18) -0.0007(16) 0.0012(14) 0.0042(16) C12A 0.0319(19) 0.029(2) 0.0227(19) 0.0035(16) 0.0027(15) 0.0038(16) C12B 0.0261(18) 0.037(2) 0.027(2) -0.0024(17) 0.0011(15) 0.0014(16) C13A 0.0278(18) 0.028(2) 0.0240(19) 0.0002(16) 0.0051(14) -0.0011(15) C13B 0.0267(18) 0.025(2) 0.0257(19) 0.0018(15) 0.0037(14) 0.0032(15) C15A 0.0306(19) 0.036(2) 0.023(2) 0.0040(17) 0.0013(15) -0.0005(16) C15B 0.031(2) 0.031(2) 0.026(2) -0.0016(16) 0.0019(15) -0.0016(16) C16A 0.038(2) 0.036(2) 0.029(2) 0.0070(18) -0.0018(16) 0.0014(18) C16B 0.031(2) 0.035(2) 0.044(3) 0.0006(19) 0.0033(17) -0.0020(17) C17A 0.049(2) 0.031(2) 0.036(2) 0.0050(18) -0.0009(18) 0.0110(18) C17B 0.0274(19) 0.044(3) 0.038(2) 0.0063(19) 0.0111(16) 0.0021(17) C18A 0.049(2) 0.034(2) 0.029(2) -0.0025(18) 0.0028(17) 0.0095(19) C18B 0.0306(19) 0.037(2) 0.027(2) 0.0000(17) 0.0067(15) 0.0033(16) C19A 0.0318(19) 0.029(2) 0.0219(19) -0.0015(15) 0.0029(15) -0.0020(16) C19B 0.0296(19) 0.034(2) 0.0211(19) -0.0019(16) 0.0010(15) 0.0035(16) C20A 0.032(2) 0.033(2) 0.025(2) 0.0004(16) 0.0016(15) 0.0055(16) C20B 0.040(2) 0.042(2) 0.026(2) -0.0039(18) 0.0110(16) -0.0017(18) C21A 0.037(2) 0.029(2) 0.028(2) -0.0063(16) 0.0048(16) 0.0036(16) C21B 0.038(2) 0.039(2) 0.026(2) -0.0027(17) 0.0059(16) -0.0052(18) C22A 0.041(2) 0.026(2) 0.0219(19) -0.0011(16) 0.0047(16) -0.0049(16) C22B 0.037(2) 0.029(2) 0.026(2) 0.0002(16) 0.0036(16) 0.0078(16) C23A 0.049(2) 0.032(2) 0.023(2) 0.0006(17) -0.0029(17) 0.0093(18) C23B 0.033(2) 0.046(3) 0.026(2) -0.0079(18) 0.0072(16) 0.0022(18) C24A 0.047(2) 0.026(2) 0.027(2) -0.0038(16) -0.0002(17) 0.0099(17) C24B 0.030(2) 0.045(3) 0.031(2) -0.0079(18) 0.0039(16) -0.0026(17) C25A 0.052(2) 0.029(2) 0.022(2) 0.0035(16) 0.0086(17) -0.0089(18) C25B 0.034(2) 0.035(2) 0.023(2) -0.0022(16) 0.0023(15) 0.0115(17) C26A 0.077(3) 0.056(3) 0.030(2) 0.001(2) 0.014(2) 0.011(3) C26B 0.054(3) 0.040(3) 0.032(2) -0.0013(19) 0.0099(19) -0.004(2) C27A 0.105(4) 0.061(3) 0.031(3) -0.008(2) 0.022(3) 0.015(3) C27B 0.052(3) 0.037(3) 0.047(3) -0.008(2) 0.008(2) -0.006(2) C28A 0.095(4) 0.066(4) 0.021(2) -0.011(2) 0.012(2) -0.013(3) C28B 0.042(2) 0.042(3) 0.028(2) -0.0087(19) -0.0004(17) 0.0064(19) C29A 0.063(3) 0.059(3) 0.028(2) 0.000(2) 0.001(2) -0.012(2) C29B 0.042(2) 0.044(3) 0.028(2) -0.0023(18) 0.0054(17) 0.0090(19) C30A 0.053(3) 0.043(3) 0.026(2) -0.0024(18) 0.0084(18) -0.007(2) C30B 0.041(2) 0.035(2) 0.034(2) -0.0036(18) 0.0048(17) 0.0024(18) N1A 0.0288(16) 0.0258(17) 0.0243(16) -0.0031(13) 0.0059(12) -0.0009(13) N1B 0.0295(16) 0.0294(17) 0.0219(16) -0.0017(13) 0.0060(12) 0.0028(13) N8A 0.0272(15) 0.0246(17) 0.0224(16) 0.0003(13) 0.0040(12) 0.0018(13) N8B 0.0243(15) 0.0317(18) 0.0211(16) 0.0023(13) 0.0015(12) 0.0035(13) N14A 0.0275(15) 0.0317(18) 0.0196(15) -0.0005(13) 0.0036(12) -0.0013(13) N14B 0.0279(15) 0.0262(17) 0.0230(16) -0.0024(13) 0.0034(12) 0.0003(13) N40 0.060(3) 0.075(3) 0.044(2) 0.013(2) 0.011(2) 0.018(2) C41 0.049(3) 0.043(3) 0.038(3) 0.001(2) 0.016(2) 0.009(2) C42 0.047(3) 0.066(3) 0.052(3) 0.012(2) 0.005(2) 0.010(2) N43 0.139(5) 0.069(3) 0.054(3) -0.022(3) 0.018(3) -0.006(3) C44 0.078(3) 0.047(3) 0.045(3) -0.003(2) 0.009(2) 0.005(3) C45 0.098(4) 0.057(3) 0.043(3) -0.015(3) 0.002(3) 0.008(3) B1 0.031(7) 0.132(12) 0.038(9) -0.014(8) 0.011(6) 0.016(6) F1 0.083(6) 0.140(8) 0.112(7) 0.043(6) 0.068(5) 0.029(5) F2 0.071(5) 0.101(5) 0.042(3) -0.023(3) -0.017(3) 0.033(4) F3 0.051(4) 0.188(10) 0.039(3) 0.029(4) -0.002(2) -0.026(4) F4 0.049(4) 0.131(8) 0.136(10) -0.083(7) 0.047(5) -0.014(4) B1B 0.040(11) 0.073(10) 0.030(10) -0.008(8) -0.006(8) -0.003(7) F1B 0.110(10) 0.131(10) 0.028(4) 0.005(5) 0.010(5) -0.006(8) F2B 0.056(5) 0.076(6) 0.129(10) 0.035(6) -0.012(5) 0.006(4) F3B 0.035(4) 0.113(8) 0.103(9) 0.032(7) 0.015(4) 0.020(4) F4B 0.084(9) 0.120(9) 0.059(6) -0.045(6) -0.020(6) 0.027(6) B2 0.073(4) 0.062(4) 0.037(4) -0.008(3) 0.001(3) 0.016(4) F5 0.096(4) 0.099(4) 0.119(5) 0.009(3) 0.020(3) -0.025(3) F6 0.170(6) 0.100(4) 0.107(5) 0.048(4) -0.055(4) -0.025(4) F7 0.148(6) 0.174(8) 0.072(4) -0.048(4) -0.020(4) 0.099(6) F8 0.070(3) 0.142(4) 0.069(3) -0.008(3) 0.009(2) 0.016(3) B2B 0.073(4) 0.062(4) 0.037(4) -0.008(3) 0.001(3) 0.016(4) F5B 0.058(9) 0.163(19) 0.099(14) 0.009(13) 0.022(9) -0.009(10) F6B 0.063(9) 0.096(12) 0.071(10) -0.002(8) -0.020(7) -0.002(8) F7B 0.082(10) 0.032(6) 0.073(10) 0.010(6) -0.038(8) 0.008(7) F8B 0.070(3) 0.142(4) 0.069(3) -0.008(3) 0.009(2) 0.016(3) O1 0.076(5) 0.101(6) 0.067(5) 0.006(5) 0.000(4) 0.004(4) _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 Zn1 N8B 2.066(3) . ? Zn1 N8A 2.077(3) . ? Zn1 N14A 2.174(3) . ? Zn1 N1A 2.185(3) . ? Zn1 N14B 2.192(3) . ? Zn1 N1B 2.194(3) . ? C2A N1A 1.336(4) . ? C2A C3A 1.379(5) . ? C2B N1B 1.338(4) . ? C2B C3B 1.388(5) . ? C3A C4A 1.375(5) . ? C3B C4B 1.381(5) . ? C4A C5A 1.383(5) . ? C4B C5B 1.385(5) . ? C5A C6A 1.387(5) . ? C5B C6B 1.397(5) . ? C6A N1A 1.340(4) . ? C6A C7A 1.496(5) . ? C6B N1B 1.347(4) . ? C6B C7B 1.482(5) . ? C7A N8A 1.338(4) . ? C7A C12A 1.384(5) . ? C7B N8B 1.345(4) . ? C7B C12B 1.382(5) . ? C9A N8A 1.337(4) . ? C9A C10A 1.388(5) . ? C9A C13A 1.493(5) . ? C9B N8B 1.343(4) . ? C9B C10B 1.386(5) . ? C9B C13B 1.492(5) . ? C10A C11A 1.400(5) . ? C10B C11B 1.402(5) . ? C11A C12A 1.399(5) . ? C11A C19A 1.486(5) . ? C11B C12B 1.409(5) . ? C11B C19B 1.478(5) . ? C13A N14A 1.349(4) . ? C13A C18A 1.386(5) . ? C13B N14B 1.340(4) . ? C13B C18B 1.392(5) . ? C15A N14A 1.340(4) . ? C15A C16A 1.386(5) . ? C15B N14B 1.333(4) . ? C15B C16B 1.396(5) . ? C16A C17A 1.373(5) . ? C16B C17B 1.376(5) . ? C17A C18A 1.391(5) . ? C17B C18B 1.385(5) . ? C19A C24A 1.395(5) . ? C19A C20A 1.398(5) . ? C19B C20B 1.395(5) . ? C19B C24B 1.399(5) . ? C20A C21A 1.381(5) . ? C20B C21B 1.384(5) . ? C21A C22A 1.401(5) . ? C21B C22B 1.392(5) . ? C22A C23A 1.399(5) . ? C22A C25A 1.483(5) . ? C22B C23B 1.398(5) . ? C22B C25B 1.484(5) . ? C23A C24A 1.383(5) . ? C23B C24B 1.383(5) . ? C25A C30A 1.392(6) . ? C25A C26A 1.400(6) . ? C25B C26B 1.384(5) . ? C25B C30B 1.394(5) . ? C26A C27A 1.385(6) . ? C26B C27B 1.386(5) . ? C27A C28A 1.385(7) . ? C27B C28B 1.380(6) . ? C28A C29A 1.361(7) . ? C28B C29B 1.382(6) . ? C29A C30A 1.385(5) . ? C29B C30B 1.383(5) . ? N40 C41 1.140(5) . ? C41 C42 1.439(6) . ? N43 C44 1.124(6) . ? C44 C45 1.441(6) . ? B1 F1 1.3849(9) . ? B1 F3 1.3850(9) . ? B1 F4 1.3851(9) . ? B1 F2 1.3852(9) . ? B1B F3B 1.3850(9) . ? B1B F1B 1.3850(9) . ? B1B F4B 1.3851(9) . ? B1B F2B 1.3851(9) . ? B2 F7 1.3845(9) . ? B2 F6 1.3845(9) . ? B2 F8 1.3851(9) . ? B2 F5 1.3854(9) . ? B2B F7B 1.3850(9) . ? B2B F6B 1.3851(9) . ? B2B F8B 1.3852(9) . ? B2B F5B 1.3852(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8B Zn1 N8A 175.65(12) . . ? N8B Zn1 N14A 108.72(11) . . ? N8A Zn1 N14A 75.51(11) . . ? N8B Zn1 N1A 100.23(11) . . ? N8A Zn1 N1A 75.57(11) . . ? N14A Zn1 N1A 151.04(11) . . ? N8B Zn1 N14B 75.61(11) . . ? N8A Zn1 N14B 103.07(11) . . ? N14A Zn1 N14B 97.57(11) . . ? N1A Zn1 N14B 90.37(11) . . ? N8B Zn1 N1B 75.91(11) . . ? N8A Zn1 N1B 105.48(11) . . ? N14A Zn1 N1B 89.70(11) . . ? N1A Zn1 N1B 96.52(11) . . ? N14B Zn1 N1B 151.45(11) . . ? N1A C2A C3A 122.2(3) . . ? N1B C2B C3B 122.7(3) . . ? C4A C3A C2A 118.8(4) . . ? C4B C3B C2B 118.1(3) . . ? C3A C4A C5A 119.5(4) . . ? C3B C4B C5B 120.0(3) . . ? C4A C5A C6A 118.7(4) . . ? C4B C5B C6B 118.7(3) . . ? N1A C6A C5A 121.6(3) . . ? N1A C6A C7A 114.8(3) . . ? C5A C6A C7A 123.5(3) . . ? N1B C6B C5B 121.2(3) . . ? N1B C6B C7B 115.6(3) . . ? C5B C6B C7B 123.2(3) . . ? N8A C7A C12A 120.9(3) . . ? N8A C7A C6A 114.4(3) . . ? C12A C7A C6A 124.6(3) . . ? N8B C7B C12B 121.1(3) . . ? N8B C7B C6B 114.3(3) . . ? C12B C7B C6B 124.6(3) . . ? N8A C9A C10A 121.4(3) . . ? N8A C9A C13A 113.9(3) . . ? C10A C9A C13A 124.8(3) . . ? N8B C9B C10B 121.2(3) . . ? N8B C9B C13B 113.9(3) . . ? C10B C9B C13B 124.8(3) . . ? C9A C10A C11A 119.7(3) . . ? C9B C10B C11B 120.3(3) . . ? C12A C11A C10A 117.2(3) . . ? C12A C11A C19A 120.7(3) . . ? C10A C11A C19A 122.1(3) . . ? C10B C11B C12B 116.7(3) . . ? C10B C11B C19B 121.8(3) . . ? C12B C11B C19B 121.5(3) . . ? C7A C12A C11A 120.3(3) . . ? C7B C12B C11B 120.4(3) . . ? N14A C13A C18A 121.7(3) . . ? N14A C13A C9A 114.8(3) . . ? C18A C13A C9A 123.5(3) . . ? N14B C13B C18B 121.6(3) . . ? N14B C13B C9B 115.3(3) . . ? C18B C13B C9B 123.2(3) . . ? N14A C15A C16A 122.1(3) . . ? N14B C15B C16B 122.1(3) . . ? C17A C16A C15A 118.5(3) . . ? C17B C16B C15B 118.4(3) . . ? C16A C17A C18A 120.1(4) . . ? C16B C17B C18B 119.7(3) . . ? C13A C18A C17A 118.3(4) . . ? C17B C18B C13B 118.7(3) . . ? C24A C19A C20A 117.7(3) . . ? C24A C19A C11A 121.2(3) . . ? C20A C19A C11A 121.1(3) . . ? C20B C19B C24B 116.6(3) . . ? C20B C19B C11B 122.3(3) . . ? C24B C19B C11B 121.1(3) . . ? C21A C20A C19A 120.6(3) . . ? C21B C20B C19B 121.6(3) . . ? C20A C21A C22A 122.3(3) . . ? C20B C21B C22B 121.8(4) . . ? C23A C22A C21A 116.3(3) . . ? C23A C22A C25A 122.0(3) . . ? C21A C22A C25A 121.7(3) . . ? C21B C22B C23B 116.6(3) . . ? C21B C22B C25B 121.7(3) . . ? C23B C22B C25B 121.7(3) . . ? C24A C23A C22A 121.9(4) . . ? C24B C23B C22B 121.6(3) . . ? C23A C24A C19A 121.1(3) . . ? C23B C24B C19B 121.7(3) . . ? C30A C25A C26A 117.1(4) . . ? C30A C25A C22A 121.6(4) . . ? C26A C25A C22A 121.3(4) . . ? C26B C25B C30B 117.2(3) . . ? C26B C25B C22B 122.0(3) . . ? C30B C25B C22B 120.8(4) . . ? C27A C26A C25A 121.1(5) . . ? C25B C26B C27B 121.7(4) . . ? C28A C27A C26A 120.1(5) . . ? C28B C27B C26B 120.0(4) . . ? C29A C28A C27A 119.7(4) . . ? C27B C28B C29B 119.5(4) . . ? C28A C29A C30A 120.5(5) . . ? C28B C29B C30B 119.9(4) . . ? C29A C30A C25A 121.4(4) . . ? C29B C30B C25B 121.6(4) . . ? C2A N1A C6A 119.2(3) . . ? C2A N1A Zn1 125.0(2) . . ? C6A N1A Zn1 115.3(2) . . ? C2B N1B C6B 119.3(3) . . ? C2B N1B Zn1 126.3(2) . . ? C6B N1B Zn1 114.3(2) . . ? C9A N8A C7A 120.5(3) . . ? C9A N8A Zn1 120.0(2) . . ? C7A N8A Zn1 119.5(2) . . ? C9B N8B C7B 120.2(3) . . ? C9B N8B Zn1 119.7(2) . . ? C7B N8B Zn1 119.3(2) . . ? C15A N14A C13A 119.3(3) . . ? C15A N14A Zn1 124.8(2) . . ? C13A N14A Zn1 115.5(2) . . ? C15B N14B C13B 119.5(3) . . ? C15B N14B Zn1 125.6(2) . . ? C13B N14B Zn1 114.9(2) . . ? N40 C41 C42 178.8(5) . . ? N43 C44 C45 179.3(6) . . ? F1 B1 F3 109.53(9) . . ? F1 B1 F4 109.44(9) . . ? F3 B1 F4 109.50(9) . . ? F1 B1 F2 109.49(9) . . ? F3 B1 F2 109.41(9) . . ? F4 B1 F2 109.46(9) . . ? F3B B1B F1B 109.48(9) . . ? F3B B1B F4B 109.50(9) . . ? F1B B1B F4B 109.45(9) . . ? F3B B1B F2B 109.46(9) . . ? F1B B1B F2B 109.48(9) . . ? F4B B1B F2B 109.46(9) . . ? F7 B2 F6 109.64(9) . . ? F7 B2 F8 109.45(9) . . ? F6 B2 F8 109.51(9) . . ? F7 B2 F5 109.50(9) . . ? F6 B2 F5 109.41(9) . . ? F8 B2 F5 109.31(9) . . ? F7B B2B F6B 109.52(9) . . ? F7B B2B F8B 109.45(9) . . ? F6B B2B F8B 109.46(9) . . ? F7B B2B F5B 109.47(9) . . ? F6B B2B F5B 109.45(9) . . ? F8B B2B F5B 109.47(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A C2A C3A C4A -1.2(6) . . . . ? N1B C2B C3B C4B 0.5(6) . . . . ? C2A C3A C4A C5A 1.0(6) . . . . ? C2B C3B C4B C5B 0.2(6) . . . . ? C3A C4A C5A C6A -0.3(6) . . . . ? C3B C4B C5B C6B -0.7(6) . . . . ? C4A C5A C6A N1A -0.1(5) . . . . ? C4A C5A C6A C7A 178.1(3) . . . . ? C4B C5B C6B N1B 0.6(6) . . . . ? C4B C5B C6B C7B -177.9(4) . . . . ? N1A C6A C7A N8A 3.0(4) . . . . ? C5A C6A C7A N8A -175.4(3) . . . . ? N1A C6A C7A C12A -178.0(3) . . . . ? C5A C6A C7A C12A 3.7(5) . . . . ? N1B C6B C7B N8B 8.1(5) . . . . ? C5B C6B C7B N8B -173.3(3) . . . . ? N1B C6B C7B C12B -170.2(3) . . . . ? C5B C6B C7B C12B 8.5(6) . . . . ? N8A C9A C10A C11A 1.0(5) . . . . ? C13A C9A C10A C11A -178.6(3) . . . . ? N8B C9B C10B C11B -0.2(5) . . . . ? C13B C9B C10B C11B -178.5(3) . . . . ? C9A C10A C11A C12A 0.2(5) . . . . ? C9A C10A C11A C19A 178.6(3) . . . . ? C9B C10B C11B C12B -0.4(5) . . . . ? C9B C10B C11B C19B 177.2(3) . . . . ? N8A C7A C12A C11A 1.5(5) . . . . ? C6A C7A C12A C11A -177.5(3) . . . . ? C10A C11A C12A C7A -1.4(5) . . . . ? C19A C11A C12A C7A -179.8(3) . . . . ? N8B C7B C12B C11B -0.3(6) . . . . ? C6B C7B C12B C11B 177.8(3) . . . . ? C10B C11B C12B C7B 0.6(5) . . . . ? C19B C11B C12B C7B -177.0(3) . . . . ? N8A C9A C13A N14A 7.3(4) . . . . ? C10A C9A C13A N14A -173.0(3) . . . . ? N8A C9A C13A C18A -172.0(3) . . . . ? C10A C9A C13A C18A 7.7(6) . . . . ? N8B C9B C13B N14B -6.2(4) . . . . ? C10B C9B C13B N14B 172.2(3) . . . . ? N8B C9B C13B C18B 174.1(3) . . . . ? C10B C9B C13B C18B -7.5(6) . . . . ? N14A C15A C16A C17A 1.1(6) . . . . ? N14B C15B C16B C17B 0.7(6) . . . . ? C15A C16A C17A C18A -1.5(6) . . . . ? C15B C16B C17B C18B 1.1(6) . . . . ? N14A C13A C18A C17A -0.8(6) . . . . ? C9A C13A C18A C17A 178.5(3) . . . . ? C16A C17A C18A C13A 1.4(6) . . . . ? C16B C17B C18B C13B -1.7(6) . . . . ? N14B C13B C18B C17B 0.6(6) . . . . ? C9B C13B C18B C17B -179.7(3) . . . . ? C12A C11A C19A C24A -16.9(5) . . . . ? C10A C11A C19A C24A 164.8(4) . . . . ? C12A C11A C19A C20A 161.5(3) . . . . ? C10A C11A C19A C20A -16.8(5) . . . . ? C10B C11B C19B C20B -177.2(4) . . . . ? C12B C11B C19B C20B 0.3(6) . . . . ? C10B C11B C19B C24B 4.8(6) . . . . ? C12B C11B C19B C24B -177.7(4) . . . . ? C24A C19A C20A C21A 2.1(5) . . . . ? C11A C19A C20A C21A -176.4(3) . . . . ? C24B C19B C20B C21B 0.2(6) . . . . ? C11B C19B C20B C21B -177.9(4) . . . . ? C19A C20A C21A C22A 0.4(6) . . . . ? C19B C20B C21B C22B 0.3(6) . . . . ? C20A C21A C22A C23A -2.2(6) . . . . ? C20A C21A C22A C25A 177.2(3) . . . . ? C20B C21B C22B C23B -1.3(6) . . . . ? C20B C21B C22B C25B 176.8(4) . . . . ? C21A C22A C23A C24A 1.4(6) . . . . ? C25A C22A C23A C24A -177.9(4) . . . . ? C21B C22B C23B C24B 1.7(6) . . . . ? C25B C22B C23B C24B -176.3(4) . . . . ? C22A C23A C24A C19A 1.0(6) . . . . ? C20A C19A C24A C23A -2.8(6) . . . . ? C11A C19A C24A C23A 175.7(4) . . . . ? C22B C23B C24B C19B -1.3(6) . . . . ? C20B C19B C24B C23B 0.2(6) . . . . ? C11B C19B C24B C23B 178.4(4) . . . . ? C23A C22A C25A C30A -18.9(6) . . . . ? C21A C22A C25A C30A 161.7(4) . . . . ? C23A C22A C25A C26A 162.2(4) . . . . ? C21A C22A C25A C26A -17.1(6) . . . . ? C21B C22B C25B C26B 28.3(6) . . . . ? C23B C22B C25B C26B -153.7(4) . . . . ? C21B C22B C25B C30B -150.7(4) . . . . ? C23B C22B C25B C30B 27.2(5) . . . . ? C30A C25A C26A C27A -2.0(7) . . . . ? C22A C25A C26A C27A 176.8(4) . . . . ? C30B C25B C26B C27B -0.2(6) . . . . ? C22B C25B C26B C27B -179.3(4) . . . . ? C25A C26A C27A C28A 2.2(8) . . . . ? C25B C26B C27B C28B 0.9(7) . . . . ? C26A C27A C28A C29A -0.9(8) . . . . ? C26B C27B C28B C29B -0.9(6) . . . . ? C27A C28A C29A C30A -0.5(8) . . . . ? C27B C28B C29B C30B 0.2(6) . . . . ? C28A C29A C30A C25A 0.6(7) . . . . ? C26A C25A C30A C29A 0.6(6) . . . . ? C22A C25A C30A C29A -178.2(4) . . . . ? C28B C29B C30B C25B 0.5(6) . . . . ? C26B C25B C30B C29B -0.5(6) . . . . ? C22B C25B C30B C29B 178.6(3) . . . . ? C3A C2A N1A C6A 0.8(5) . . . . ? C3A C2A N1A Zn1 -170.8(3) . . . . ? C5A C6A N1A C2A -0.1(5) . . . . ? C7A C6A N1A C2A -178.5(3) . . . . ? C5A C6A N1A Zn1 172.3(3) . . . . ? C7A C6A N1A Zn1 -6.1(4) . . . . ? N8B Zn1 N1A C2A -1.6(3) . . . . ? N8A Zn1 N1A C2A 177.3(3) . . . . ? N14A Zn1 N1A C2A -179.7(2) . . . . ? N14B Zn1 N1A C2A 73.9(3) . . . . ? N1B Zn1 N1A C2A -78.4(3) . . . . ? N8B Zn1 N1A C6A -173.5(2) . . . . ? N8A Zn1 N1A C6A 5.4(2) . . . . ? N14A Zn1 N1A C6A 8.5(4) . . . . ? N14B Zn1 N1A C6A -98.0(2) . . . . ? N1B Zn1 N1A C6A 109.7(2) . . . . ? C3B C2B N1B C6B -0.7(6) . . . . ? C3B C2B N1B Zn1 -177.8(3) . . . . ? C5B C6B N1B C2B 0.1(5) . . . . ? C7B C6B N1B C2B 178.7(3) . . . . ? C5B C6B N1B Zn1 177.6(3) . . . . ? C7B C6B N1B Zn1 -3.8(4) . . . . ? N8B Zn1 N1B C2B 176.8(3) . . . . ? N8A Zn1 N1B C2B -7.5(3) . . . . ? N14A Zn1 N1B C2B 67.4(3) . . . . ? N1A Zn1 N1B C2B -84.3(3) . . . . ? N14B Zn1 N1B C2B 172.8(3) . . . . ? N8B Zn1 N1B C6B -0.5(2) . . . . ? N8A Zn1 N1B C6B 175.2(2) . . . . ? N14A Zn1 N1B C6B -109.9(2) . . . . ? N1A Zn1 N1B C6B 98.5(2) . . . . ? N14B Zn1 N1B C6B -4.5(4) . . . . ? C10A C9A N8A C7A -1.1(5) . . . . ? C13A C9A N8A C7A 178.6(3) . . . . ? C10A C9A N8A Zn1 175.9(2) . . . . ? C13A C9A N8A Zn1 -4.3(4) . . . . ? C12A C7A N8A C9A -0.2(5) . . . . ? C6A C7A N8A C9A 178.9(3) . . . . ? C12A C7A N8A Zn1 -177.2(2) . . . . ? C6A C7A N8A Zn1 1.9(4) . . . . ? N8B Zn1 N8A C9A -165.7(14) . . . . ? N14A Zn1 N8A C9A 0.7(2) . . . . ? N1A Zn1 N8A C9A 179.1(3) . . . . ? N14B Zn1 N8A C9A -93.9(3) . . . . ? N1B Zn1 N8A C9A 86.2(3) . . . . ? N8B Zn1 N8A C7A 11.4(17) . . . . ? N14A Zn1 N8A C7A 177.7(3) . . . . ? N1A Zn1 N8A C7A -3.8(2) . . . . ? N14B Zn1 N8A C7A 83.2(3) . . . . ? N1B Zn1 N8A C7A -96.7(3) . . . . ? C10B C9B N8B C7B 0.5(5) . . . . ? C13B C9B N8B C7B 179.0(3) . . . . ? C10B C9B N8B Zn1 -169.2(3) . . . . ? C13B C9B N8B Zn1 9.3(4) . . . . ? C12B C7B N8B C9B -0.3(5) . . . . ? C6B C7B N8B C9B -178.6(3) . . . . ? C12B C7B N8B Zn1 169.5(3) . . . . ? C6B C7B N8B Zn1 -8.8(4) . . . . ? N8A Zn1 N8B C9B 65.9(16) . . . . ? N14A Zn1 N8B C9B -100.1(3) . . . . ? N1A Zn1 N8B C9B 80.9(3) . . . . ? N14B Zn1 N8B C9B -6.9(3) . . . . ? N1B Zn1 N8B C9B 175.1(3) . . . . ? N8A Zn1 N8B C7B -103.9(15) . . . . ? N14A Zn1 N8B C7B 90.1(3) . . . . ? N1A Zn1 N8B C7B -88.9(3) . . . . ? N14B Zn1 N8B C7B -176.7(3) . . . . ? N1B Zn1 N8B C7B 5.3(3) . . . . ? C16A C15A N14A C13A -0.4(5) . . . . ? C16A C15A N14A Zn1 -171.8(3) . . . . ? C18A C13A N14A C15A 0.3(5) . . . . ? C9A C13A N14A C15A -179.0(3) . . . . ? C18A C13A N14A Zn1 172.5(3) . . . . ? C9A C13A N14A Zn1 -6.8(4) . . . . ? N8B Zn1 N14A C15A -5.8(3) . . . . ? N8A Zn1 N14A C15A 175.3(3) . . . . ? N1A Zn1 N14A C15A 172.2(2) . . . . ? N14B Zn1 N14A C15A -83.1(3) . . . . ? N1B Zn1 N14A C15A 69.2(3) . . . . ? N8B Zn1 N14A C13A -177.5(2) . . . . ? N8A Zn1 N14A C13A 3.6(2) . . . . ? N1A Zn1 N14A C13A 0.5(4) . . . . ? N14B Zn1 N14A C13A 105.2(2) . . . . ? N1B Zn1 N14A C13A -102.5(2) . . . . ? C16B C15B N14B C13B -1.8(5) . . . . ? C16B C15B N14B Zn1 179.0(3) . . . . ? C18B C13B N14B C15B 1.2(5) . . . . ? C9B C13B N14B C15B -178.6(3) . . . . ? C18B C13B N14B Zn1 -179.6(3) . . . . ? C9B C13B N14B Zn1 0.7(4) . . . . ? N8B Zn1 N14B C15B -177.8(3) . . . . ? N8A Zn1 N14B C15B 6.5(3) . . . . ? N14A Zn1 N14B C15B -70.3(3) . . . . ? N1A Zn1 N14B C15B 81.7(3) . . . . ? N1B Zn1 N14B C15B -173.8(3) . . . . ? N8B Zn1 N14B C13B 3.0(2) . . . . ? N8A Zn1 N14B C13B -172.7(2) . . . . ? N14A Zn1 N14B C13B 110.5(2) . . . . ? N1A Zn1 N14B C13B -97.5(2) . . . . ? N1B Zn1 N14B C13B 7.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.894 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.070 data_mh001 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C115 H85 Cd2 F24 N13 O2 P4' _chemical_formula_weight 2485.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8640(10) _cell_length_b 18.7200(10) _cell_length_c 21.8500(10) _cell_angle_alpha 98.350(10) _cell_angle_beta 98.920(10) _cell_angle_gamma 107.120(10) _cell_volume 5243.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2508 _exptl_absorpt_coefficient_mu 0.570 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7638 _exptl_absorpt_correction_T_max 0.8477 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61863 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.1118 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 30.49 _reflns_number_total 31793 _reflns_number_gt 16339 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+2.5922P] 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 31793 _refine_ls_number_parameters 1436 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1478 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.235340(18) 0.490279(13) -0.245270(12) 0.03576(7) Uani 1 1 d . . . Cd2 Cd 0.212087(18) 0.000041(13) -0.258797(12) 0.03604(7) Uani 1 1 d . . . P1 P -0.19169(7) -0.00609(5) -0.24553(4) 0.0347(2) Uani 1 1 d . . . P2 P -0.16536(8) 0.51013(6) -0.23619(5) 0.0480(2) Uani 1 1 d . . . P3 P 0.48381(8) 0.30129(5) -0.13121(4) 0.0415(2) Uani 1 1 d . . . P4 P 0.02842(16) -0.23816(11) -0.48982(6) 0.1244(8) Uani 1 1 d . . . F1 F -0.25421(16) -0.03493(11) -0.31693(9) 0.0501(5) Uani 1 1 d . . . F2 F -0.29287(15) -0.04718(12) -0.22144(10) 0.0531(5) Uani 1 1 d . . . F3 F -0.22380(17) 0.06919(11) -0.24185(11) 0.0575(6) Uani 1 1 d . . . F4 F -0.08968(16) 0.03438(11) -0.26867(11) 0.0581(6) Uani 1 1 d . . . F5 F -0.12956(15) 0.02308(12) -0.17388(10) 0.0537(5) Uani 1 1 d . . . F6 F -0.16108(16) -0.08186(11) -0.24906(10) 0.0499(5) Uani 1 1 d . . . F7 F -0.23236(18) 0.46504(13) -0.30390(10) 0.0611(6) Uani 1 1 d . . . F8 F -0.24904(17) 0.45914(13) -0.20430(11) 0.0616(6) Uani 1 1 d . . . F9 F -0.22815(17) 0.56980(12) -0.23764(11) 0.0613(6) Uani 1 1 d . . . F10 F -0.0830(2) 0.56106(14) -0.26834(14) 0.0850(8) Uani 1 1 d . . . F11 F -0.10227(18) 0.45206(14) -0.23485(11) 0.0695(7) Uani 1 1 d . . . F12 F -0.09976(19) 0.55608(18) -0.16831(13) 0.0987(11) Uani 1 1 d . . . F13 F 0.36323(18) 0.25682(14) -0.13923(12) 0.0737(7) Uani 1 1 d . . . F14 F 0.5037(2) 0.27323(13) -0.06600(11) 0.0758(8) Uani 1 1 d . . . F15 F 0.4603(2) 0.32891(12) -0.19536(10) 0.0667(7) Uani 1 1 d . . . F16 F 0.4714(2) 0.37569(12) -0.09223(11) 0.0727(7) Uani 1 1 d . . . F17 F 0.49619(19) 0.22702(12) -0.16888(11) 0.0661(7) Uani 1 1 d . . . F18 F 0.60238(18) 0.34565(15) -0.12235(13) 0.0818(8) Uani 1 1 d . . . F19 F -0.0830(3) -0.2383(2) -0.49322(14) 0.1250(14) Uani 1 1 d . . . F20 F 0.0534(3) -0.2217(2) -0.41592(12) 0.1281(15) Uani 1 1 d . . . F21 F 0.0131(3) -0.2469(2) -0.56327(13) 0.1554(19) Uani 1 1 d . . . F22 F 0.0617(3) -0.1434(2) -0.48448(15) 0.1340(14) Uani 1 1 d . . . F23 F 0.0024(4) -0.3270(2) -0.49485(17) 0.1524(17) Uani 1 1 d . . . F24 F 0.1455(4) -0.2319(3) -0.48714(17) 0.180(2) Uani 1 1 d . . . N1A N 0.3560(2) 0.45597(14) -0.29789(12) 0.0351(6) Uani 1 1 d . . . N1B N 0.1390(2) 0.36429(15) -0.24983(13) 0.0365(6) Uani 1 1 d . . . N1C N 0.3290(2) -0.03940(15) -0.31211(13) 0.0386(7) Uani 1 1 d . . . N1D N 0.1069(2) -0.12061(15) -0.25257(13) 0.0398(7) Uani 1 1 d . . . N8A N 0.38659(19) 0.51506(13) -0.17451(12) 0.0294(6) Uani 1 1 d . . . N8B N 0.08319(19) 0.46094(14) -0.31500(12) 0.0309(6) Uani 1 1 d . . . N8C N 0.3717(2) 0.03968(14) -0.19318(13) 0.0336(6) Uani 1 1 d . . . N8D N 0.06265(19) -0.03338(14) -0.33211(12) 0.0299(6) Uani 1 1 d . . . N14A N 0.2202(2) 0.54419(15) -0.14569(13) 0.0368(6) Uani 1 1 d . . . N14B N 0.2314(2) 0.59690(15) -0.28899(13) 0.0382(7) Uani 1 1 d . . . N14C N 0.2028(2) 0.05598(15) -0.15729(13) 0.0358(6) Uani 1 1 d . . . N14D N 0.2107(2) 0.10172(14) -0.30872(12) 0.0343(6) Uani 1 1 d . . . C2A C 0.3355(3) 0.42370(18) -0.35954(16) 0.0417(8) Uani 1 1 d . . . H2A H 0.2693 0.4161 -0.3843 0.050 Uiso 1 1 calc R . . C2B C 0.1714(3) 0.3186(2) -0.21568(17) 0.0447(9) Uani 1 1 d . . . H2B H 0.2376 0.3383 -0.1883 0.054 Uiso 1 1 calc R . . C2C C 0.3029(3) -0.0814(2) -0.37111(17) 0.0486(9) Uani 1 1 d . . . H2C H 0.2323 -0.0999 -0.3919 0.058 Uiso 1 1 calc R . . C2D C 0.1320(3) -0.1624(2) -0.21164(18) 0.0506(10) Uani 1 1 d . . . H2D H 0.1975 -0.1424 -0.1835 0.061 Uiso 1 1 calc R . . C3A C 0.4056(3) 0.4012(2) -0.38835(17) 0.0494(10) Uani 1 1 d . . . H3A H 0.3886 0.3790 -0.4322 0.059 Uiso 1 1 calc R . . C3B C 0.1128(3) 0.2447(2) -0.21869(17) 0.0478(9) Uani 1 1 d . . . H3B H 0.1380 0.2136 -0.1941 0.057 Uiso 1 1 calc R . . C3C C 0.3739(3) -0.0987(2) -0.40266(18) 0.0546(10) Uani 1 1 d . . . H3C H 0.3526 -0.1304 -0.4437 0.066 Uiso 1 1 calc R . . C3D C 0.0682(3) -0.2323(2) -0.20838(18) 0.0523(10) Uani 1 1 d . . . H3D H 0.0889 -0.2603 -0.1789 0.063 Uiso 1 1 calc R . . C4A C 0.5008(3) 0.41146(19) -0.35272(17) 0.0481(9) Uani 1 1 d . . . H4A H 0.5513 0.3970 -0.3716 0.058 Uiso 1 1 calc R . . C4B C 0.0174(3) 0.2165(2) -0.25776(19) 0.0543(10) Uani 1 1 d . . . H4B H -0.0252 0.1656 -0.2602 0.065 Uiso 1 1 calc R . . C4C C 0.4759(3) -0.0693(2) -0.37363(19) 0.0578(11) Uani 1 1 d . . . H4C H 0.5270 -0.0789 -0.3948 0.069 Uiso 1 1 calc R . . C4D C -0.0262(3) -0.2608(2) -0.2486(2) 0.0631(12) Uani 1 1 d . . . H4D H -0.0729 -0.3090 -0.2474 0.076 Uiso 1 1 calc R . . C5A C 0.5225(3) 0.44297(18) -0.28914(17) 0.0408(8) Uani 1 1 d . . . H5A H 0.5875 0.4490 -0.2635 0.049 Uiso 1 1 calc R . . C5B C -0.0168(3) 0.2628(2) -0.29380(18) 0.0488(9) Uani 1 1 d . . . H5B H -0.0826 0.2437 -0.3216 0.059 Uiso 1 1 calc R . . C5C C 0.5040(3) -0.0255(2) -0.31337(18) 0.0527(10) Uani 1 1 d . . . H5C H 0.5747 -0.0044 -0.2930 0.063 Uiso 1 1 calc R . . C5D C -0.0525(3) -0.2187(2) -0.29100(19) 0.0547(10) Uani 1 1 d . . . H5D H -0.1178 -0.2379 -0.3194 0.066 Uiso 1 1 calc R . . C6A C 0.4488(2) 0.46582(16) -0.26281(15) 0.0320(7) Uani 1 1 d . . . C6B C 0.0455(2) 0.33684(18) -0.28890(15) 0.0342(7) Uani 1 1 d . . . C6C C 0.4291(3) -0.01248(19) -0.28274(16) 0.0379(8) Uani 1 1 d . . . C6D C 0.0153(3) -0.14914(17) -0.29236(15) 0.0333(7) Uani 1 1 d . . . C7A C 0.4677(2) 0.50179(16) -0.19444(15) 0.0304(7) Uani 1 1 d . . . C7B C 0.0146(2) 0.39002(17) -0.32627(15) 0.0319(7) Uani 1 1 d . . . C7C C 0.4520(2) 0.02835(18) -0.21570(16) 0.0357(8) Uani 1 1 d . . . C7D C -0.0095(2) -0.10056(17) -0.33736(15) 0.0312(7) Uani 1 1 d . . . C9A C 0.3956(2) 0.54604(16) -0.11385(15) 0.0294(7) Uani 1 1 d . . . C9B C 0.0632(2) 0.51300(17) -0.34682(15) 0.0320(7) Uani 1 1 d . . . C9C C 0.3848(2) 0.07283(17) -0.13293(16) 0.0335(7) Uani 1 1 d . . . C9D C 0.0462(2) 0.01546(16) -0.36839(14) 0.0296(7) Uani 1 1 d . . . C10A C 0.4874(2) 0.56488(17) -0.07026(15) 0.0316(7) Uani 1 1 d . . . H10A H 0.4913 0.5844 -0.0270 0.038 Uiso 1 1 calc R . . C10B C -0.0258(2) 0.49514(18) -0.39221(15) 0.0351(7) Uani 1 1 d . . . H10B H -0.0379 0.5324 -0.4149 0.042 Uiso 1 1 calc R . . C10C C 0.4795(2) 0.09469(18) -0.09146(16) 0.0377(8) Uani 1 1 d . . . H10C H 0.4869 0.1175 -0.0485 0.045 Uiso 1 1 calc R . . C10D C -0.0450(2) -0.00342(17) -0.41288(15) 0.0332(7) Uani 1 1 d . . . H10D H -0.0548 0.0311 -0.4392 0.040 Uiso 1 1 calc R . . C11A C 0.5745(2) 0.55494(16) -0.09033(15) 0.0306(7) Uani 1 1 d . . . C11B C -0.0980(2) 0.42231(18) -0.40473(15) 0.0357(8) Uani 1 1 d . . . C11C C 0.5637(3) 0.08292(19) -0.11340(17) 0.0413(8) Uani 1 1 d . . . C11D C -0.1220(2) -0.07283(17) -0.41905(15) 0.0330(7) Uani 1 1 d . . . C12A C 0.5631(2) 0.52237(16) -0.15398(15) 0.0313(7) Uani 1 1 d . . . H12A H 0.6204 0.5144 -0.1693 0.038 Uiso 1 1 calc R . . C12B C -0.0765(2) 0.36968(18) -0.37034(15) 0.0345(7) Uani 1 1 d . . . H12B H -0.1247 0.3198 -0.3773 0.041 Uiso 1 1 calc R . . C12C C 0.5494(3) 0.05011(19) -0.17662(17) 0.0411(8) Uani 1 1 d . . . H12C H 0.6059 0.0425 -0.1932 0.049 Uiso 1 1 calc R . . C12D C -0.1026(2) -0.12183(17) -0.38010(15) 0.0340(7) Uani 1 1 d . . . H12D H -0.1532 -0.1698 -0.3829 0.041 Uiso 1 1 calc R . . C13A C 0.3015(2) 0.56140(17) -0.09765(15) 0.0306(7) Uani 1 1 d . . . C13B C 0.1442(2) 0.59018(18) -0.32939(15) 0.0349(7) Uani 1 1 d . . . C13C C 0.2902(2) 0.08367(17) -0.11305(16) 0.0332(7) Uani 1 1 d . . . C13D C 0.1293(2) 0.09078(17) -0.35583(15) 0.0316(7) Uani 1 1 d . . . C15A C 0.1354(3) 0.55965(19) -0.13439(18) 0.0438(9) Uani 1 1 d . . . H15A H 0.0776 0.5467 -0.1684 0.053 Uiso 1 1 calc R . . C15B C 0.3075(3) 0.66408(19) -0.27411(18) 0.0496(10) Uani 1 1 d . . . H15B H 0.3687 0.6689 -0.2451 0.060 Uiso 1 1 calc R . . C15C C 0.1155(3) 0.06354(19) -0.14232(18) 0.0439(9) Uani 1 1 d . . . H15C H 0.0538 0.0441 -0.1739 0.053 Uiso 1 1 calc R . . C15D C 0.2847(3) 0.16978(19) -0.29263(16) 0.0406(8) Uani 1 1 d . . . H15D H 0.3420 0.1771 -0.2595 0.049 Uiso 1 1 calc R . . C16A C 0.1283(3) 0.59333(19) -0.07585(18) 0.0440(9) Uani 1 1 d . . . H16A H 0.0673 0.6040 -0.0695 0.053 Uiso 1 1 calc R . . C16B C 0.3013(3) 0.7265(2) -0.29890(19) 0.0554(11) Uani 1 1 d . . . H16B H 0.3575 0.7729 -0.2883 0.067 Uiso 1 1 calc R . . C16C C 0.1116(3) 0.09799(19) -0.08358(18) 0.0466(9) Uani 1 1 d . . . H16C H 0.0482 0.1016 -0.0744 0.056 Uiso 1 1 calc R . . C16D C 0.2817(3) 0.22945(19) -0.32181(17) 0.0431(8) Uani 1 1 d . . . H16D H 0.3350 0.2774 -0.3087 0.052 Uiso 1 1 calc R . . C17A C 0.2120(3) 0.61118(19) -0.02653(18) 0.0430(9) Uani 1 1 d . . . H17A H 0.2095 0.6347 0.0145 0.052 Uiso 1 1 calc R . . C17B C 0.2112(3) 0.7198(2) -0.3393(2) 0.0595(11) Uani 1 1 d . . . H17B H 0.2040 0.7620 -0.3569 0.071 Uiso 1 1 calc R . . C17C C 0.2007(3) 0.1272(2) -0.03839(19) 0.0500(10) Uani 1 1 d . . . H17C H 0.2004 0.1523 0.0026 0.060 Uiso 1 1 calc R . . C17D C 0.1998(3) 0.21800(19) -0.37047(17) 0.0454(9) Uani 1 1 d . . . H17D H 0.1960 0.2580 -0.3920 0.055 Uiso 1 1 calc R . . C18A C 0.2995(3) 0.59467(18) -0.03717(16) 0.0377(8) Uani 1 1 d . . . H18A H 0.3575 0.6060 -0.0035 0.045 Uiso 1 1 calc R . . C18B C 0.1316(3) 0.65154(19) -0.35420(18) 0.0478(9) Uani 1 1 d . . . H18B H 0.0684 0.6466 -0.3813 0.057 Uiso 1 1 calc R . . C18C C 0.2910(3) 0.1199(2) -0.05291(18) 0.0478(9) Uani 1 1 d . . . H18C H 0.3534 0.1395 -0.0219 0.057 Uiso 1 1 calc R . . C18D C 0.1230(3) 0.14810(19) -0.38782(16) 0.0425(8) Uani 1 1 d . . . H18D H 0.0661 0.1395 -0.4216 0.051 Uiso 1 1 calc R . . C19A C 0.6752(2) 0.57902(17) -0.04612(15) 0.0314(7) Uani 1 1 d . . . C19B C -0.1949(2) 0.39988(18) -0.45347(15) 0.0344(7) Uani 1 1 d . . . C19C C 0.6656(3) 0.10385(19) -0.07045(17) 0.0399(8) Uani 1 1 d . . . C19D C -0.2225(2) -0.09442(17) -0.46380(15) 0.0336(7) Uani 1 1 d . . . C20A C 0.7026(2) 0.64131(18) 0.00430(15) 0.0359(8) Uani 1 1 d . . . H20A H 0.6540 0.6664 0.0119 0.043 Uiso 1 1 calc R . . C20B C -0.1993(3) 0.4332(2) -0.50651(17) 0.0439(9) Uani 1 1 d . . . H20B H -0.1399 0.4716 -0.5110 0.053 Uiso 1 1 calc R . . C20C C 0.7058(3) 0.17345(19) -0.02808(17) 0.0422(8) Uani 1 1 d . . . H20C H 0.6672 0.2078 -0.0262 0.051 Uiso 1 1 calc R . . C20D C -0.2660(3) -0.03984(19) -0.47994(18) 0.0482(9) Uani 1 1 d . . . H20D H -0.2306 0.0125 -0.4619 0.058 Uiso 1 1 calc R . . C21A C 0.7990(2) 0.66669(18) 0.04308(15) 0.0366(8) Uani 1 1 d . . . H21A H 0.8158 0.7094 0.0768 0.044 Uiso 1 1 calc R . . C21B C -0.2883(3) 0.41145(19) -0.55252(17) 0.0428(8) Uani 1 1 d . . . H21B H -0.2894 0.4356 -0.5878 0.051 Uiso 1 1 calc R . . C21C C 0.8020(3) 0.19304(19) 0.01153(17) 0.0421(8) Uani 1 1 d . . . H21C H 0.8282 0.2408 0.0403 0.050 Uiso 1 1 calc R . . C21D C -0.3594(3) -0.06029(19) -0.52158(18) 0.0469(9) Uani 1 1 d . . . H21D H -0.3869 -0.0216 -0.5317 0.056 Uiso 1 1 calc R . . C22A C 0.8730(2) 0.63146(17) 0.03420(15) 0.0318(7) Uani 1 1 d . . . C22B C -0.3768(2) 0.35465(17) -0.54820(16) 0.0356(8) Uani 1 1 d . . . C22C C 0.8610(2) 0.14435(19) 0.01015(16) 0.0374(8) Uani 1 1 d . . . C22D C -0.4149(2) -0.13635(18) -0.54937(15) 0.0361(8) Uani 1 1 d . . . C23A C 0.8451(2) 0.56848(17) -0.01527(15) 0.0328(7) Uani 1 1 d . . . H23A H 0.8934 0.5427 -0.0220 0.039 Uiso 1 1 calc R . . C23B C -0.3727(3) 0.32263(19) -0.49481(17) 0.0436(9) Uani 1 1 d . . . H23B H -0.4323 0.2845 -0.4901 0.052 Uiso 1 1 calc R . . C23C C 0.8194(3) 0.07446(19) -0.03271(17) 0.0447(9) Uani 1 1 d . . . H23C H 0.8577 0.0400 -0.0346 0.054 Uiso 1 1 calc R . . C23D C -0.3708(3) -0.19050(18) -0.53297(16) 0.0407(8) Uani 1 1 d . . . H23D H -0.4062 -0.2429 -0.5510 0.049 Uiso 1 1 calc R . . C24A C 0.7482(2) 0.54269(17) -0.05481(16) 0.0354(8) Uani 1 1 d . . . H24A H 0.7312 0.4997 -0.0883 0.043 Uiso 1 1 calc R . . C24B C -0.2837(3) 0.3450(2) -0.44821(17) 0.0440(9) Uani 1 1 d . . . H24B H -0.2835 0.3224 -0.4120 0.053 Uiso 1 1 calc R . . C24C C 0.7236(3) 0.0545(2) -0.07243(18) 0.0444(9) Uani 1 1 d . . . H24C H 0.6972 0.0067 -0.1013 0.053 Uiso 1 1 calc R . . C24D C -0.2770(3) -0.17017(18) -0.49119(17) 0.0412(8) Uani 1 1 d . . . H24D H -0.2493 -0.2088 -0.4811 0.049 Uiso 1 1 calc R . . C25A C 0.9795(2) 0.66220(18) 0.07413(15) 0.0329(7) Uani 1 1 d . . . C25B C -0.4708(3) 0.32814(18) -0.59958(16) 0.0396(8) Uani 1 1 d . . . C25C C 0.9651(3) 0.16767(19) 0.05121(16) 0.0376(8) Uani 1 1 d . . . C25D C -0.5131(3) -0.15785(19) -0.59604(16) 0.0383(8) Uani 1 1 d . . . C26A C 1.0262(3) 0.74035(19) 0.09588(16) 0.0406(8) Uani 1 1 d . . . H26A H 0.9885 0.7739 0.0870 0.049 Uiso 1 1 calc R . . C26B C -0.4969(3) 0.3755(2) -0.63780(18) 0.0505(10) Uani 1 1 d . . . H26B H -0.4539 0.4272 -0.6307 0.061 Uiso 1 1 calc R . . C26C C 1.0286(3) 0.2429(2) 0.06532(16) 0.0414(8) Uani 1 1 d . . . H26C H 1.0053 0.2798 0.0476 0.050 Uiso 1 1 calc R . . C26D C -0.5842(3) -0.1195(2) -0.59014(18) 0.0501(9) Uani 1 1 d . . . H26D H -0.5708 -0.0798 -0.5544 0.060 Uiso 1 1 calc R . . C27A C 1.1265(3) 0.7699(2) 0.13012(17) 0.0471(9) Uani 1 1 d . . . H27A H 1.1573 0.8234 0.1445 0.056 Uiso 1 1 calc R . . C27B C -0.5840(3) 0.3493(2) -0.68590(19) 0.0590(11) Uani 1 1 d . . . H27B H -0.6000 0.3828 -0.7116 0.071 Uiso 1 1 calc R . . C27C C 1.1250(3) 0.2657(2) 0.10443(17) 0.0516(10) Uani 1 1 d . . . H27C H 1.1667 0.3179 0.1140 0.062 Uiso 1 1 calc R . . C27D C -0.6739(3) -0.1378(3) -0.6351(2) 0.0637(12) Uani 1 1 d . . . H27D H -0.7209 -0.1104 -0.6304 0.076 Uiso 1 1 calc R . . C28A C 1.1821(3) 0.7218(2) 0.14352(16) 0.0491(10) Uani 1 1 d . . . H28A H 1.2514 0.7422 0.1667 0.059 Uiso 1 1 calc R . . C28B C -0.6471(3) 0.2755(2) -0.69646(19) 0.0610(11) Uani 1 1 d . . . H28B H -0.7077 0.2577 -0.7290 0.073 Uiso 1 1 calc R . . C28C C 1.1603(3) 0.2132(3) 0.12942(19) 0.0626(12) Uani 1 1 d . . . H28C H 1.2264 0.2289 0.1567 0.075 Uiso 1 1 calc R . . C28D C -0.6953(3) -0.1957(2) -0.68682(19) 0.0584(11) Uani 1 1 d . . . H28D H -0.7566 -0.2079 -0.7181 0.070 Uiso 1 1 calc R . . C29A C 1.1364(3) 0.6442(2) 0.12311(18) 0.0503(10) Uani 1 1 d . . . H29A H 1.1740 0.6109 0.1328 0.060 Uiso 1 1 calc R . . C29B C -0.6225(3) 0.2273(2) -0.6599(2) 0.0656(12) Uani 1 1 d . . . H29B H -0.6657 0.1756 -0.6674 0.079 Uiso 1 1 calc R . . C29C C 1.1005(3) 0.1379(3) 0.11522(19) 0.0619(12) Uani 1 1 d . . . H29C H 1.1260 0.1012 0.1319 0.074 Uiso 1 1 calc R . . C29D C -0.6275(3) -0.2359(2) -0.69297(19) 0.0622(11) Uani 1 1 d . . . H29D H -0.6427 -0.2768 -0.7280 0.075 Uiso 1 1 calc R . . C30A C 1.0365(3) 0.6146(2) 0.08871(16) 0.0416(8) Uani 1 1 d . . . H30A H 1.0059 0.5609 0.0747 0.050 Uiso 1 1 calc R . . C30B C -0.5354(3) 0.2533(2) -0.61233(19) 0.0522(10) Uani 1 1 d . . . H30B H -0.5191 0.2190 -0.5876 0.063 Uiso 1 1 calc R . . C30C C 1.0025(3) 0.1148(2) 0.07642(18) 0.0502(10) Uani 1 1 d . . . H30C H 0.9611 0.0626 0.0672 0.060 Uiso 1 1 calc R . . C30D C -0.5375(3) -0.2167(2) -0.64819(18) 0.0527(10) Uani 1 1 d . . . H30D H -0.4910 -0.2445 -0.6532 0.063 Uiso 1 1 calc R . . C100 C 0.5155(3) 0.8535(2) -0.1734(2) 0.0590(11) Uani 1 1 d . . . H100 H 0.5321 0.8845 -0.2035 0.071 Uiso 1 1 calc R . . C101 C 0.4384(4) 0.8549(3) -0.1462(3) 0.0878(16) Uani 1 1 d . . . H101 H 0.4004 0.8880 -0.1559 0.105 Uiso 1 1 calc R . . C102 C 0.5713(4) 0.8085(3) -0.1590(2) 0.0822(15) Uani 1 1 d . . . H102 H 0.6279 0.8085 -0.1785 0.099 Uiso 1 1 calc R . . C103 C 0.4674(5) 0.7628(3) -0.0884(2) 0.0947(19) Uani 1 1 d . . . H103 H 0.4503 0.7313 -0.0587 0.114 Uiso 1 1 calc R . . C104 C 0.5480(5) 0.7628(3) -0.1168(3) 0.0935(18) Uani 1 1 d . . . H104 H 0.5879 0.7309 -0.1072 0.112 Uiso 1 1 calc R . . C105 C 0.4116(5) 0.8094(4) -0.1040(3) 0.115(2) Uani 1 1 d . . . H105 H 0.3543 0.8101 -0.0853 0.138 Uiso 1 1 calc R . . O1 O 0.3033(4) 0.3458(3) -0.5466(2) 0.128(4) Uiso 0.519(6) 1 d PD A 1 N200 N 0.3287(6) 0.4100(3) -0.5575(4) 0.088(3) Uiso 0.519(6) 1 d PD A 1 C201 C 0.2618(8) 0.4224(7) -0.6035(5) 0.100(4) Uiso 0.519(6) 1 d PD A 1 H20E H 0.2853 0.4763 -0.6065 0.150 Uiso 0.519(6) 1 calc PR A 1 H20F H 0.1931 0.4094 -0.5933 0.150 Uiso 0.519(6) 1 calc PR A 1 H20G H 0.2585 0.3905 -0.6440 0.150 Uiso 0.519(6) 1 calc PR A 1 O3 O 0.4059(5) 0.4621(4) -0.5290(4) 0.106(3) Uiso 0.519(6) 1 d PD A 1 O2 O 0.3033(4) 0.3458(3) -0.5466(2) 0.128(3) Uiso 0.481(6) 1 d PD A 2 N202 N 0.2610(7) 0.3905(5) -0.5635(5) 0.103(3) Uiso 0.481(6) 1 d PD A 2 C203 C 0.3229(12) 0.4584(7) -0.5702(9) 0.164(7) Uiso 0.481(6) 1 d PD A 2 H20H H 0.3278 0.4560 -0.6147 0.245 Uiso 0.481(6) 1 calc PR A 2 H20I H 0.3919 0.4698 -0.5441 0.245 Uiso 0.481(6) 1 calc PR A 2 H20J H 0.2940 0.4985 -0.5568 0.245 Uiso 0.481(6) 1 calc PR A 2 O4 O 0.1807(7) 0.3824(6) -0.5999(4) 0.138(4) Uiso 0.481(6) 1 d PD A 2 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 Cd1 0.02784(14) 0.03622(13) 0.03654(15) 0.00460(10) -0.00616(11) 0.00833(10) Cd2 0.02654(13) 0.04051(14) 0.03881(15) 0.00969(11) -0.00081(11) 0.01063(11) P1 0.0267(5) 0.0333(4) 0.0436(5) 0.0054(4) 0.0094(4) 0.0092(4) P2 0.0372(6) 0.0653(6) 0.0452(6) 0.0036(5) 0.0115(5) 0.0245(5) P3 0.0431(6) 0.0362(5) 0.0377(5) 0.0063(4) 0.0007(4) 0.0060(4) P4 0.1938(19) 0.1893(19) 0.0405(7) -0.0102(9) -0.0106(9) 0.1706(17) F1 0.0505(13) 0.0546(12) 0.0432(12) 0.0059(10) 0.0034(10) 0.0193(10) F2 0.0331(12) 0.0606(13) 0.0597(14) 0.0085(11) 0.0183(11) 0.0039(10) F3 0.0606(15) 0.0426(12) 0.0724(16) 0.0045(11) 0.0090(12) 0.0272(11) F4 0.0435(13) 0.0519(13) 0.0736(16) 0.0088(11) 0.0274(12) 0.0016(10) F5 0.0370(12) 0.0685(14) 0.0479(13) -0.0068(11) 0.0013(10) 0.0188(11) F6 0.0576(14) 0.0460(12) 0.0546(13) 0.0108(10) 0.0141(11) 0.0281(10) F7 0.0622(16) 0.0753(15) 0.0435(13) 0.0053(11) 0.0029(11) 0.0262(12) F8 0.0571(15) 0.0894(17) 0.0634(15) 0.0349(13) 0.0275(12) 0.0441(13) F9 0.0543(14) 0.0641(14) 0.0747(17) 0.0117(12) 0.0187(13) 0.0313(12) F10 0.0678(18) 0.0752(17) 0.118(2) 0.0113(16) 0.0532(17) 0.0186(14) F11 0.0649(16) 0.1019(19) 0.0658(16) 0.0162(14) 0.0224(13) 0.0585(15) F12 0.0469(16) 0.162(3) 0.0687(18) -0.0422(18) -0.0115(13) 0.0498(17) F13 0.0476(15) 0.0768(16) 0.0804(18) 0.0167(14) 0.0075(13) -0.0016(12) F14 0.105(2) 0.0593(14) 0.0448(14) 0.0177(11) -0.0131(14) 0.0100(14) F15 0.0938(19) 0.0551(14) 0.0449(13) 0.0187(11) 0.0006(13) 0.0180(13) F16 0.108(2) 0.0460(13) 0.0680(17) 0.0074(11) 0.0360(16) 0.0237(13) F17 0.0828(18) 0.0510(13) 0.0640(16) 0.0040(11) 0.0073(13) 0.0288(13) F18 0.0443(15) 0.0909(19) 0.0836(19) 0.0029(15) 0.0081(14) -0.0078(13) F19 0.150(3) 0.165(3) 0.080(2) -0.010(2) -0.017(2) 0.119(3) F20 0.194(4) 0.188(3) 0.0495(17) -0.0021(19) -0.004(2) 0.160(3) F21 0.253(5) 0.222(4) 0.0489(18) -0.007(2) -0.008(2) 0.200(4) F22 0.162(4) 0.172(3) 0.086(2) -0.010(2) -0.009(2) 0.114(3) F23 0.244(5) 0.153(3) 0.093(3) 0.000(2) 0.008(3) 0.137(4) F24 0.218(5) 0.310(6) 0.090(3) 0.013(3) 0.017(3) 0.223(5) N1A 0.0385(17) 0.0276(13) 0.0345(16) 0.0058(11) 0.0016(13) 0.0071(12) N1B 0.0342(16) 0.0365(15) 0.0387(16) 0.0127(12) 0.0039(13) 0.0109(12) N1C 0.0343(17) 0.0436(16) 0.0397(17) 0.0115(13) 0.0048(14) 0.0154(13) N1D 0.0380(17) 0.0416(16) 0.0405(17) 0.0142(13) 0.0029(14) 0.0136(13) N8A 0.0235(14) 0.0308(13) 0.0330(15) 0.0057(11) 0.0057(12) 0.0080(11) N8B 0.0235(14) 0.0341(14) 0.0317(15) 0.0033(11) 0.0010(12) 0.0084(11) N8C 0.0270(15) 0.0359(15) 0.0399(17) 0.0085(12) 0.0060(13) 0.0131(12) N8D 0.0281(14) 0.0305(14) 0.0287(14) 0.0045(11) 0.0026(12) 0.0083(11) N14A 0.0256(15) 0.0393(15) 0.0410(17) 0.0025(13) 0.0011(13) 0.0097(12) N14B 0.0320(16) 0.0344(15) 0.0394(17) 0.0042(12) -0.0066(13) 0.0064(12) N14C 0.0238(14) 0.0398(15) 0.0450(17) 0.0114(13) 0.0061(13) 0.0112(12) N14D 0.0274(15) 0.0332(14) 0.0366(16) 0.0069(12) 0.0003(13) 0.0046(12) C2A 0.050(2) 0.0358(18) 0.0330(19) 0.0041(15) -0.0035(17) 0.0118(16) C2B 0.042(2) 0.048(2) 0.042(2) 0.0149(17) 0.0028(18) 0.0134(17) C2C 0.052(2) 0.054(2) 0.041(2) 0.0099(18) 0.0066(19) 0.0203(19) C2D 0.045(2) 0.057(2) 0.053(2) 0.0215(19) 0.0042(19) 0.0198(19) C3A 0.074(3) 0.041(2) 0.032(2) 0.0057(16) 0.009(2) 0.019(2) C3B 0.059(3) 0.046(2) 0.045(2) 0.0219(18) 0.013(2) 0.0193(19) C3C 0.072(3) 0.060(2) 0.039(2) 0.0113(19) 0.013(2) 0.030(2) C3D 0.064(3) 0.052(2) 0.051(2) 0.0270(19) 0.015(2) 0.025(2) C4A 0.055(3) 0.044(2) 0.046(2) 0.0028(17) 0.018(2) 0.0168(18) C4B 0.056(3) 0.041(2) 0.061(3) 0.0185(19) 0.012(2) 0.0040(19) C4C 0.063(3) 0.075(3) 0.050(3) 0.018(2) 0.023(2) 0.036(2) C4D 0.069(3) 0.049(2) 0.067(3) 0.030(2) 0.010(2) 0.006(2) C5A 0.039(2) 0.0386(19) 0.044(2) 0.0054(16) 0.0095(17) 0.0125(16) C5B 0.038(2) 0.046(2) 0.056(3) 0.0142(18) 0.0073(19) 0.0038(17) C5C 0.050(2) 0.070(3) 0.050(2) 0.015(2) 0.017(2) 0.031(2) C5D 0.050(2) 0.047(2) 0.057(3) 0.0209(19) -0.001(2) 0.0012(18) C6A 0.0311(18) 0.0264(16) 0.0343(18) 0.0051(13) 0.0052(15) 0.0043(13) C6B 0.0278(18) 0.0371(18) 0.0360(19) 0.0057(14) 0.0081(15) 0.0080(14) C6C 0.035(2) 0.0440(19) 0.041(2) 0.0144(16) 0.0089(16) 0.0195(16) C6D 0.0352(19) 0.0330(17) 0.0324(18) 0.0066(14) 0.0073(15) 0.0121(14) C7A 0.0282(17) 0.0278(16) 0.0325(18) 0.0053(13) 0.0063(14) 0.0058(13) C7B 0.0244(17) 0.0358(17) 0.0344(18) 0.0026(14) 0.0057(14) 0.0105(14) C7C 0.0295(18) 0.0380(18) 0.043(2) 0.0110(15) 0.0070(16) 0.0150(15) C7D 0.0266(17) 0.0320(17) 0.0319(18) 0.0016(13) 0.0053(14) 0.0076(14) C9A 0.0239(16) 0.0281(16) 0.0339(18) 0.0061(13) 0.0034(14) 0.0063(13) C9B 0.0280(17) 0.0375(18) 0.0305(18) 0.0046(14) 0.0042(14) 0.0130(14) C9C 0.0266(17) 0.0333(17) 0.042(2) 0.0091(14) 0.0068(15) 0.0109(14) C9D 0.0243(16) 0.0303(16) 0.0309(17) 0.0023(13) 0.0010(14) 0.0082(13) C10A 0.0245(17) 0.0345(17) 0.0321(18) 0.0037(13) 0.0006(14) 0.0083(13) C10B 0.0276(18) 0.0420(19) 0.0355(19) 0.0053(15) 0.0015(15) 0.0150(15) C10C 0.0296(18) 0.0401(19) 0.041(2) 0.0024(15) 0.0016(16) 0.0129(15) C10D 0.0344(19) 0.0295(16) 0.0320(18) 0.0047(13) 0.0014(15) 0.0087(14) C11A 0.0229(16) 0.0304(16) 0.0362(18) 0.0054(14) 0.0026(14) 0.0077(13) C11B 0.0263(18) 0.0413(19) 0.0373(19) 0.0021(15) 0.0025(15) 0.0127(15) C11C 0.0287(19) 0.0421(19) 0.051(2) 0.0053(17) 0.0009(17) 0.0137(15) C11D 0.0292(18) 0.0345(17) 0.0298(18) -0.0002(14) 0.0009(15) 0.0082(14) C12A 0.0255(17) 0.0322(16) 0.0341(18) 0.0025(13) 0.0027(14) 0.0101(13) C12B 0.0256(17) 0.0347(17) 0.0379(19) 0.0006(14) 0.0049(15) 0.0059(14) C12C 0.0259(18) 0.047(2) 0.052(2) 0.0082(17) 0.0088(17) 0.0140(15) C12D 0.0285(18) 0.0314(17) 0.0335(18) 0.0007(14) 0.0019(15) 0.0021(14) C13A 0.0229(16) 0.0315(16) 0.0345(18) 0.0067(14) 0.0021(14) 0.0065(13) C13B 0.0304(18) 0.0359(18) 0.0340(19) 0.0026(14) 0.0001(15) 0.0097(14) C13C 0.0246(17) 0.0314(17) 0.042(2) 0.0079(14) 0.0054(15) 0.0081(13) C13D 0.0279(17) 0.0334(17) 0.0304(18) 0.0079(14) 0.0034(14) 0.0063(14) C15A 0.0256(18) 0.049(2) 0.054(2) 0.0051(18) 0.0020(17) 0.0143(16) C15B 0.040(2) 0.042(2) 0.052(2) 0.0056(17) -0.0096(18) 0.0027(17) C15C 0.0272(19) 0.048(2) 0.058(2) 0.0128(18) 0.0079(18) 0.0127(16) C15D 0.0327(19) 0.043(2) 0.040(2) 0.0088(16) -0.0031(16) 0.0084(16) C16A 0.0264(19) 0.044(2) 0.062(3) 0.0055(18) 0.0096(18) 0.0135(16) C16B 0.054(3) 0.034(2) 0.062(3) 0.0061(18) -0.004(2) -0.0003(18) C16C 0.037(2) 0.044(2) 0.063(3) 0.0105(19) 0.018(2) 0.0165(17) C16D 0.037(2) 0.0409(19) 0.044(2) 0.0098(16) 0.0035(17) 0.0038(16) C17A 0.038(2) 0.0406(19) 0.050(2) 0.0053(16) 0.0152(18) 0.0098(16) C17B 0.060(3) 0.039(2) 0.067(3) 0.0122(19) -0.012(2) 0.0105(19) C17C 0.045(2) 0.050(2) 0.056(3) 0.0016(18) 0.020(2) 0.0172(18) C17D 0.042(2) 0.0382(19) 0.048(2) 0.0193(17) -0.0027(18) 0.0022(16) C18A 0.0281(18) 0.0406(19) 0.038(2) 0.0020(15) 0.0021(15) 0.0060(15) C18B 0.042(2) 0.038(2) 0.058(2) 0.0115(17) -0.0077(19) 0.0140(17) C18C 0.031(2) 0.056(2) 0.049(2) -0.0033(18) 0.0065(18) 0.0112(17) C18D 0.038(2) 0.043(2) 0.038(2) 0.0131(16) -0.0052(16) 0.0048(16) C19A 0.0229(16) 0.0327(16) 0.0341(18) 0.0034(14) -0.0016(14) 0.0079(13) C19B 0.0227(17) 0.0400(18) 0.0368(19) 0.0000(15) 0.0017(15) 0.0109(14) C19C 0.0245(17) 0.046(2) 0.046(2) 0.0038(16) 0.0033(16) 0.0113(15) C19D 0.0312(18) 0.0350(17) 0.0298(18) 0.0036(14) 0.0021(15) 0.0071(14) C20A 0.0266(18) 0.0425(19) 0.0358(19) -0.0005(15) 0.0011(15) 0.0141(15) C20B 0.0298(19) 0.045(2) 0.046(2) 0.0032(17) 0.0018(17) 0.0026(16) C20C 0.0290(19) 0.0413(19) 0.053(2) 0.0007(17) 0.0020(17) 0.0148(15) C20D 0.042(2) 0.0320(18) 0.059(2) 0.0032(17) -0.0081(19) 0.0067(16) C21A 0.0315(19) 0.0395(18) 0.0342(19) -0.0024(14) 0.0014(15) 0.0122(15) C21B 0.0299(19) 0.050(2) 0.041(2) 0.0101(16) 0.0004(16) 0.0048(16) C21C 0.035(2) 0.0397(19) 0.048(2) 0.0011(16) 0.0022(17) 0.0141(16) C21D 0.040(2) 0.0363(19) 0.056(2) 0.0069(17) -0.0096(18) 0.0117(16) C22A 0.0228(16) 0.0359(17) 0.0358(18) 0.0123(14) 0.0017(14) 0.0078(13) C22B 0.0266(18) 0.0336(17) 0.040(2) -0.0013(15) -0.0035(15) 0.0097(14) C22C 0.0273(18) 0.0434(19) 0.040(2) 0.0090(16) 0.0023(15) 0.0118(15) C22D 0.0274(18) 0.0416(19) 0.0339(19) 0.0061(15) 0.0012(15) 0.0067(15) C23A 0.0261(17) 0.0301(16) 0.042(2) 0.0056(14) 0.0032(15) 0.0121(13) C23B 0.0279(19) 0.045(2) 0.050(2) 0.0109(17) -0.0020(17) 0.0052(15) C23C 0.034(2) 0.043(2) 0.058(2) 0.0073(18) 0.0034(18) 0.0191(16) C23D 0.0336(19) 0.0319(17) 0.045(2) 0.0017(15) -0.0049(17) 0.0036(15) C24A 0.0297(18) 0.0294(16) 0.043(2) 0.0009(14) 0.0002(16) 0.0097(14) C24B 0.034(2) 0.051(2) 0.044(2) 0.0172(17) 0.0020(17) 0.0103(17) C24C 0.0310(19) 0.043(2) 0.054(2) -0.0018(17) 0.0024(18) 0.0136(16) C24D 0.039(2) 0.0320(18) 0.047(2) 0.0064(15) -0.0034(17) 0.0102(15) C25A 0.0240(17) 0.0426(19) 0.0311(18) 0.0090(14) 0.0025(14) 0.0103(14) C25B 0.0311(19) 0.0386(19) 0.042(2) 0.0003(15) -0.0004(16) 0.0081(15) C25C 0.0302(19) 0.050(2) 0.0346(19) 0.0116(16) 0.0028(15) 0.0159(16) C25D 0.0281(18) 0.047(2) 0.0342(19) 0.0107(16) -0.0008(15) 0.0057(15) C26A 0.0307(19) 0.045(2) 0.041(2) -0.0002(16) 0.0001(16) 0.0138(16) C26B 0.034(2) 0.048(2) 0.060(3) 0.0116(19) -0.0045(19) 0.0047(17) C26C 0.0307(19) 0.054(2) 0.038(2) 0.0130(16) 0.0032(16) 0.0124(16) C26D 0.041(2) 0.058(2) 0.046(2) 0.0030(18) -0.0026(18) 0.0182(19) C27A 0.034(2) 0.054(2) 0.042(2) -0.0006(17) -0.0020(17) 0.0076(17) C27B 0.042(2) 0.073(3) 0.055(3) 0.023(2) -0.004(2) 0.011(2) C27C 0.036(2) 0.067(3) 0.043(2) 0.0080(19) -0.0004(18) 0.0089(19) C27D 0.041(2) 0.089(3) 0.062(3) 0.012(2) -0.002(2) 0.030(2) C28A 0.0268(19) 0.078(3) 0.032(2) 0.0058(18) -0.0048(16) 0.0102(19) C28B 0.040(2) 0.078(3) 0.041(2) 0.000(2) -0.0116(19) -0.001(2) C28C 0.040(2) 0.098(3) 0.042(2) 0.004(2) -0.0093(19) 0.023(2) C28D 0.037(2) 0.084(3) 0.045(2) 0.009(2) -0.0049(19) 0.015(2) C29A 0.035(2) 0.071(3) 0.049(2) 0.022(2) -0.0004(18) 0.024(2) C29B 0.053(3) 0.050(2) 0.063(3) -0.007(2) -0.013(2) -0.007(2) C29C 0.063(3) 0.089(3) 0.048(3) 0.023(2) 0.002(2) 0.045(3) C29D 0.052(3) 0.077(3) 0.043(2) -0.003(2) -0.007(2) 0.016(2) C30A 0.034(2) 0.048(2) 0.044(2) 0.0170(17) 0.0008(17) 0.0152(16) C30B 0.046(2) 0.037(2) 0.059(3) 0.0027(18) -0.006(2) 0.0042(17) C30C 0.047(2) 0.058(2) 0.049(2) 0.0142(19) 0.006(2) 0.0227(19) C30D 0.040(2) 0.064(3) 0.048(2) 0.0004(19) -0.0029(19) 0.0183(19) C100 0.044(2) 0.065(3) 0.069(3) 0.028(2) 0.015(2) 0.012(2) C101 0.070(4) 0.126(5) 0.092(4) 0.047(4) 0.031(3) 0.048(3) C102 0.082(4) 0.104(4) 0.092(4) 0.049(3) 0.042(3) 0.051(3) C103 0.115(5) 0.081(4) 0.055(3) 0.028(3) 0.012(3) -0.021(3) C104 0.123(5) 0.072(3) 0.098(4) 0.030(3) 0.020(4) 0.046(3) C105 0.074(4) 0.186(7) 0.092(5) 0.046(5) 0.043(4) 0.030(4) _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 Cd1 N8B 2.270(2) . ? Cd1 N8A 2.284(2) . ? Cd1 N1B 2.322(3) . ? Cd1 N14A 2.329(3) . ? Cd1 N14B 2.345(3) . ? Cd1 N1A 2.355(3) . ? Cd2 N8D 2.273(3) . ? Cd2 N8C 2.290(3) . ? Cd2 N14D 2.331(3) . ? Cd2 N1D 2.336(3) . ? Cd2 N14C 2.351(3) . ? Cd2 N1C 2.360(3) . ? P1 F6 1.5908(19) . ? P1 F4 1.591(2) . ? P1 F1 1.593(2) . ? P1 F3 1.593(2) . ? P1 F5 1.596(2) . ? P1 F2 1.596(2) . ? P2 F11 1.584(2) . ? P2 F10 1.584(3) . ? P2 F7 1.585(2) . ? P2 F12 1.587(3) . ? P2 F8 1.592(2) . ? P2 F9 1.607(2) . ? P3 F18 1.575(2) . ? P3 F17 1.579(2) . ? P3 F15 1.583(2) . ? P3 F16 1.593(2) . ? P3 F14 1.601(2) . ? P3 F13 1.602(2) . ? P4 F19 1.534(4) . ? P4 F20 1.563(3) . ? P4 F21 1.564(3) . ? P4 F23 1.578(4) . ? P4 F24 1.585(4) . ? P4 F22 1.677(4) . ? N1A C6A 1.338(4) . ? N1A C2A 1.343(4) . ? N1B C2B 1.340(4) . ? N1B C6B 1.346(4) . ? N1C C2C 1.343(4) . ? N1C C6C 1.345(4) . ? N1D C6D 1.333(4) . ? N1D C2D 1.342(4) . ? N8A C9A 1.338(4) . ? N8A C7A 1.342(4) . ? N8B C9B 1.344(4) . ? N8B C7B 1.348(4) . ? N8C C9C 1.332(4) . ? N8C C7C 1.343(4) . ? N8D C7D 1.333(4) . ? N8D C9D 1.339(4) . ? N14A C15A 1.340(4) . ? N14A C13A 1.341(4) . ? N14B C15B 1.339(4) . ? N14B C13B 1.344(4) . ? N14C C13C 1.339(4) . ? N14C C15C 1.342(4) . ? N14D C15D 1.337(4) . ? N14D C13D 1.348(4) . ? C2A C3A 1.368(5) . ? C2B C3B 1.370(5) . ? C2C C3C 1.372(5) . ? C2D C3D 1.365(5) . ? C3A C4A 1.369(5) . ? C3B C4B 1.366(5) . ? C3C C4C 1.366(6) . ? C3D C4D 1.366(6) . ? C4A C5A 1.377(5) . ? C4B C5B 1.385(5) . ? C4C C5C 1.377(5) . ? C4D C5D 1.374(5) . ? C5A C6A 1.389(4) . ? C5B C6B 1.379(5) . ? C5C C6C 1.379(5) . ? C5D C6D 1.371(5) . ? C6A C7A 1.495(4) . ? C6B C7B 1.490(4) . ? C6C C7C 1.489(5) . ? C6D C7D 1.500(4) . ? C7A C12A 1.384(4) . ? C7B C12B 1.379(4) . ? C7C C12C 1.391(5) . ? C7D C12D 1.383(4) . ? C9A C10A 1.383(4) . ? C9A C13A 1.497(4) . ? C9B C10B 1.379(4) . ? C9B C13B 1.498(4) . ? C9C C10C 1.386(4) . ? C9C C13C 1.502(4) . ? C9D C10D 1.387(4) . ? C9D C13D 1.491(4) . ? C10A C11A 1.400(4) . ? C10B C11B 1.393(4) . ? C10C C11C 1.392(4) . ? C10D C11D 1.391(4) . ? C11A C12A 1.400(4) . ? C11A C19A 1.473(4) . ? C11B C12B 1.394(4) . ? C11B C19B 1.487(4) . ? C11C C12C 1.386(5) . ? C11C C19C 1.478(5) . ? C11D C12D 1.393(4) . ? C11D C19D 1.481(4) . ? C13A C18A 1.385(4) . ? C13B C18B 1.383(4) . ? C13C C18C 1.385(5) . ? C13D C18D 1.379(4) . ? C15A C16A 1.373(5) . ? C15B C16B 1.377(5) . ? C15C C16C 1.367(5) . ? C15D C16D 1.372(5) . ? C16A C17A 1.378(5) . ? C16B C17B 1.374(5) . ? C16C C17C 1.366(5) . ? C16D C17D 1.372(5) . ? C17A C18A 1.382(4) . ? C17B C18B 1.377(5) . ? C17C C18C 1.378(5) . ? C17D C18D 1.378(5) . ? C19A C24A 1.396(4) . ? C19A C20A 1.398(4) . ? C19B C24B 1.384(5) . ? C19B C20B 1.395(5) . ? C19C C20C 1.388(5) . ? C19C C24C 1.393(4) . ? C19D C24D 1.386(4) . ? C19D C20D 1.390(4) . ? C20A C21A 1.374(4) . ? C20B C21B 1.378(5) . ? C20C C21C 1.387(5) . ? C20D C21D 1.376(5) . ? C21A C22A 1.395(4) . ? C21B C22B 1.393(5) . ? C21C C22C 1.393(4) . ? C21D C22D 1.395(4) . ? C22A C23A 1.393(4) . ? C22A C25A 1.493(4) . ? C22B C23B 1.388(5) . ? C22B C25B 1.486(4) . ? C22C C23C 1.398(5) . ? C22C C25C 1.481(4) . ? C22D C23D 1.390(4) . ? C22D C25D 1.477(4) . ? C23A C24A 1.387(4) . ? C23B C24B 1.385(5) . ? C23C C24C 1.383(5) . ? C23D C24D 1.382(5) . ? C25A C26A 1.389(4) . ? C25A C30A 1.391(4) . ? C25B C30B 1.383(5) . ? C25B C26B 1.388(5) . ? C25C C26C 1.384(5) . ? C25C C30C 1.387(5) . ? C25D C30D 1.387(5) . ? C25D C26D 1.391(5) . ? C26A C27A 1.379(5) . ? C26B C27B 1.383(5) . ? C26C C27C 1.379(5) . ? C26D C27D 1.378(5) . ? C27A C28A 1.379(5) . ? C27B C28B 1.364(5) . ? C27C C28C 1.364(5) . ? C27D C28D 1.375(6) . ? C28A C29A 1.376(5) . ? C28B C29B 1.371(6) . ? C28C C29C 1.370(6) . ? C28D C29D 1.377(5) . ? C29A C30A 1.377(5) . ? C29B C30B 1.376(5) . ? C29C C30C 1.394(5) . ? C29D C30D 1.378(5) . ? C100 C101 1.307(6) . ? C100 C102 1.339(6) . ? C101 C105 1.364(7) . ? C102 C104 1.357(6) . ? C103 C104 1.359(7) . ? C103 C105 1.372(8) . ? O1 N200 1.2207(10) . ? N200 O3 1.2200(10) . ? N200 C201 1.3515(10) . ? N202 O4 1.2207(10) . ? N202 C203 1.3514(10) . ? 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 N8B Cd1 N8A 177.79(9) . . ? N8B Cd1 N1B 71.12(9) . . ? N8A Cd1 N1B 106.67(9) . . ? N8B Cd1 N14A 109.63(9) . . ? N8A Cd1 N14A 70.58(9) . . ? N1B Cd1 N14A 99.14(10) . . ? N8B Cd1 N14B 70.87(9) . . ? N8A Cd1 N14B 111.34(9) . . ? N1B Cd1 N14B 141.97(9) . . ? N14A Cd1 N14B 94.38(9) . . ? N8B Cd1 N1A 109.30(9) . . ? N8A Cd1 N1A 70.52(9) . . ? N1B Cd1 N1A 93.26(9) . . ? N14A Cd1 N1A 141.07(9) . . ? N14B Cd1 N1A 98.17(9) . . ? N8D Cd2 N8C 173.59(9) . . ? N8D Cd2 N14D 70.79(9) . . ? N8C Cd2 N14D 104.44(9) . . ? N8D Cd2 N1D 70.89(9) . . ? N8C Cd2 N1D 114.10(9) . . ? N14D Cd2 N1D 141.42(9) . . ? N8D Cd2 N14C 114.32(9) . . ? N8C Cd2 N14C 70.15(9) . . ? N14D Cd2 N14C 98.48(9) . . ? N1D Cd2 N14C 93.14(9) . . ? N8D Cd2 N1C 105.47(9) . . ? N8C Cd2 N1C 70.38(9) . . ? N14D Cd2 N1C 96.30(9) . . ? N1D Cd2 N1C 97.91(9) . . ? N14C Cd2 N1C 140.15(9) . . ? F6 P1 F4 89.66(11) . . ? F6 P1 F1 90.26(11) . . ? F4 P1 F1 90.50(12) . . ? F6 P1 F3 179.24(13) . . ? F4 P1 F3 91.09(12) . . ? F1 P1 F3 89.61(12) . . ? F6 P1 F5 90.05(11) . . ? F4 P1 F5 89.71(12) . . ? F1 P1 F5 179.62(12) . . ? F3 P1 F5 90.07(12) . . ? F6 P1 F2 89.68(11) . . ? F4 P1 F2 179.01(14) . . ? F1 P1 F2 90.24(12) . . ? F3 P1 F2 89.57(12) . . ? F5 P1 F2 89.55(12) . . ? F11 P2 F10 89.16(14) . . ? F11 P2 F7 90.99(13) . . ? F10 P2 F7 90.05(15) . . ? F11 P2 F12 90.04(14) . . ? F10 P2 F12 90.20(17) . . ? F7 P2 F12 178.95(14) . . ? F11 P2 F8 91.31(13) . . ? F10 P2 F8 179.42(16) . . ? F7 P2 F8 89.60(13) . . ? F12 P2 F8 90.14(16) . . ? F11 P2 F9 179.31(15) . . ? F10 P2 F9 90.20(14) . . ? F7 P2 F9 89.24(13) . . ? F12 P2 F9 89.73(14) . . ? F8 P2 F9 89.34(12) . . ? F18 P3 F17 91.33(14) . . ? F18 P3 F15 90.60(15) . . ? F17 P3 F15 90.13(13) . . ? F18 P3 F16 88.80(15) . . ? F17 P3 F16 179.10(14) . . ? F15 P3 F16 90.76(13) . . ? F18 P3 F14 91.09(15) . . ? F17 P3 F14 90.75(13) . . ? F15 P3 F14 178.07(16) . . ? F16 P3 F14 88.36(14) . . ? F18 P3 F13 179.17(16) . . ? F17 P3 F13 89.34(14) . . ? F15 P3 F13 89.88(14) . . ? F16 P3 F13 90.52(14) . . ? F14 P3 F13 88.42(14) . . ? F19 P4 F20 92.88(19) . . ? F19 P4 F21 90.4(2) . . ? F20 P4 F21 174.0(3) . . ? F19 P4 F23 95.6(3) . . ? F20 P4 F23 92.8(2) . . ? F21 P4 F23 91.9(2) . . ? F19 P4 F24 175.9(3) . . ? F20 P4 F24 87.8(2) . . ? F21 P4 F24 88.6(2) . . ? F23 P4 F24 88.4(2) . . ? F19 P4 F22 87.02(19) . . ? F20 P4 F22 87.17(19) . . ? F21 P4 F22 88.0(2) . . ? F23 P4 F22 177.4(3) . . ? F24 P4 F22 89.0(3) . . ? C6A N1A C2A 118.5(3) . . ? C6A N1A Cd1 117.2(2) . . ? C2A N1A Cd1 124.2(2) . . ? C2B N1B C6B 119.2(3) . . ? C2B N1B Cd1 123.6(2) . . ? C6B N1B Cd1 117.2(2) . . ? C2C N1C C6C 118.8(3) . . ? C2C N1C Cd2 124.2(2) . . ? C6C N1C Cd2 116.8(2) . . ? C6D N1D C2D 118.2(3) . . ? C6D N1D Cd2 117.2(2) . . ? C2D N1D Cd2 124.6(2) . . ? C9A N8A C7A 120.2(3) . . ? C9A N8A Cd1 119.90(19) . . ? C7A N8A Cd1 119.9(2) . . ? C9B N8B C7B 120.1(3) . . ? C9B N8B Cd1 120.2(2) . . ? C7B N8B Cd1 119.6(2) . . ? C9C N8C C7C 120.2(3) . . ? C9C N8C Cd2 120.3(2) . . ? C7C N8C Cd2 119.5(2) . . ? C7D N8D C9D 120.4(3) . . ? C7D N8D Cd2 119.7(2) . . ? C9D N8D Cd2 119.86(19) . . ? C15A N14A C13A 118.8(3) . . ? C15A N14A Cd1 123.4(2) . . ? C13A N14A Cd1 117.8(2) . . ? C15B N14B C13B 118.6(3) . . ? C15B N14B Cd1 124.6(2) . . ? C13B N14B Cd1 116.7(2) . . ? C13C N14C C15C 118.8(3) . . ? C13C N14C Cd2 117.8(2) . . ? C15C N14C Cd2 123.4(2) . . ? C15D N14D C13D 118.8(3) . . ? C15D N14D Cd2 123.8(2) . . ? C13D N14D Cd2 117.38(19) . . ? N1A C2A C3A 123.1(3) . . ? N1B C2B C3B 122.5(3) . . ? N1C C2C C3C 122.9(4) . . ? N1D C2D C3D 123.4(4) . . ? C2A C3A C4A 118.6(3) . . ? C4B C3B C2B 118.7(3) . . ? C4C C3C C2C 118.3(4) . . ? C2D C3D C4D 118.3(3) . . ? C3A C4A C5A 119.2(3) . . ? C3B C4B C5B 119.4(3) . . ? C3C C4C C5C 119.5(4) . . ? C3D C4D C5D 118.9(4) . . ? C4A C5A C6A 119.5(3) . . ? C6B C5B C4B 119.4(4) . . ? C4C C5C C6C 119.8(4) . . ? C6D C5D C4D 120.1(4) . . ? N1A C6A C5A 121.1(3) . . ? N1A C6A C7A 116.5(3) . . ? C5A C6A C7A 122.4(3) . . ? N1B C6B C5B 120.7(3) . . ? N1B C6B C7B 116.6(3) . . ? C5B C6B C7B 122.7(3) . . ? N1C C6C C5C 120.6(3) . . ? N1C C6C C7C 116.1(3) . . ? C5C C6C C7C 123.2(3) . . ? N1D C6D C5D 121.2(3) . . ? N1D C6D C7D 116.4(3) . . ? C5D C6D C7D 122.4(3) . . ? N8A C7A C12A 121.4(3) . . ? N8A C7A C6A 115.8(3) . . ? C12A C7A C6A 122.9(3) . . ? N8B C7B C12B 120.9(3) . . ? N8B C7B C6B 115.4(3) . . ? C12B C7B C6B 123.7(3) . . ? N8C C7C C12C 120.8(3) . . ? N8C C7C C6C 116.3(3) . . ? C12C C7C C6C 122.7(3) . . ? N8D C7D C12D 121.3(3) . . ? N8D C7D C6D 115.8(3) . . ? C12D C7D C6D 122.8(3) . . ? N8A C9A C10A 121.5(3) . . ? N8A C9A C13A 115.5(3) . . ? C10A C9A C13A 123.0(3) . . ? N8B C9B C10B 121.3(3) . . ? N8B C9B C13B 115.2(3) . . ? C10B C9B C13B 123.4(3) . . ? N8C C9C C10C 121.7(3) . . ? N8C C9C C13C 115.7(3) . . ? C10C C9C C13C 122.6(3) . . ? N8D C9D C10D 120.8(3) . . ? N8D C9D C13D 115.8(3) . . ? C10D C9D C13D 123.3(3) . . ? C9A C10A C11A 119.6(3) . . ? C9B C10B C11B 119.8(3) . . ? C9C C10C C11C 119.3(3) . . ? C9D C10D C11D 120.1(3) . . ? C12A C11A C10A 117.8(3) . . ? C12A C11A C19A 121.2(3) . . ? C10A C11A C19A 121.1(3) . . ? C10B C11B C12B 117.9(3) . . ? C10B C11B C19B 122.0(3) . . ? C12B C11B C19B 120.1(3) . . ? C12C C11C C10C 118.2(3) . . ? C12C C11C C19C 120.7(3) . . ? C10C C11C C19C 121.1(3) . . ? C10D C11D C12D 117.5(3) . . ? C10D C11D C19D 122.3(3) . . ? C12D C11D C19D 120.2(3) . . ? C7A C12A C11A 119.6(3) . . ? C7B C12B C11B 120.0(3) . . ? C11C C12C C7C 119.7(3) . . ? C7D C12D C11D 119.9(3) . . ? N14A C13A C18A 121.5(3) . . ? N14A C13A C9A 116.2(3) . . ? C18A C13A C9A 122.2(3) . . ? N14B C13B C18B 121.1(3) . . ? N14B C13B C9B 116.6(3) . . ? C18B C13B C9B 122.3(3) . . ? N14C C13C C18C 120.8(3) . . ? N14C C13C C9C 116.0(3) . . ? C18C C13C C9C 123.2(3) . . ? N14D C13D C18D 120.8(3) . . ? N14D C13D C9D 116.0(3) . . ? C18D C13D C9D 123.1(3) . . ? N14A C15A C16A 123.0(3) . . ? N14B C15B C16B 123.1(3) . . ? N14C C15C C16C 122.9(3) . . ? N14D C15D C16D 123.0(3) . . ? C15A C16A C17A 118.2(3) . . ? C17B C16B C15B 118.0(3) . . ? C17C C16C C15C 118.7(3) . . ? C15D C16D C17D 118.2(3) . . ? C16A C17A C18A 119.5(3) . . ? C16B C17B C18B 119.5(3) . . ? C16C C17C C18C 119.3(4) . . ? C16D C17D C18D 119.5(3) . . ? C17A C18A C13A 119.0(3) . . ? C17B C18B C13B 119.6(3) . . ? C17C C18C C13C 119.6(3) . . ? C17D C18D C13D 119.6(3) . . ? C24A C19A C20A 117.8(3) . . ? C24A C19A C11A 121.2(3) . . ? C20A C19A C11A 121.0(3) . . ? C24B C19B C20B 117.6(3) . . ? C24B C19B C11B 121.4(3) . . ? C20B C19B C11B 121.0(3) . . ? C20C C19C C24C 118.8(3) . . ? C20C C19C C11C 120.6(3) . . ? C24C C19C C11C 120.5(3) . . ? C24D C19D C20D 117.4(3) . . ? C24D C19D C11D 121.0(3) . . ? C20D C19D C11D 121.5(3) . . ? C21A C20A C19A 120.9(3) . . ? C21B C20B C19B 121.2(3) . . ? C21C C20C C19C 120.3(3) . . ? C21D C20D C19D 121.2(3) . . ? C20A C21A C22A 121.7(3) . . ? C20B C21B C22B 121.2(3) . . ? C20C C21C C22C 121.6(3) . . ? C20D C21D C22D 121.8(3) . . ? C23A C22A C21A 117.5(3) . . ? C23A C22A C25A 121.1(3) . . ? C21A C22A C25A 121.4(3) . . ? C23B C22B C21B 117.4(3) . . ? C23B C22B C25B 121.4(3) . . ? C21B C22B C25B 121.2(3) . . ? C21C C22C C23C 117.4(3) . . ? C21C C22C C25C 120.7(3) . . ? C23C C22C C25C 121.9(3) . . ? C23D C22D C21D 116.6(3) . . ? C23D C22D C25D 121.7(3) . . ? C21D C22D C25D 121.6(3) . . ? C24A C23A C22A 121.2(3) . . ? C24B C23B C22B 121.4(3) . . ? C24C C23C C22C 121.4(3) . . ? C24D C23D C22D 121.8(3) . . ? C23A C24A C19A 120.9(3) . . ? C19B C24B C23B 121.1(3) . . ? C23C C24C C19C 120.5(3) . . ? C23D C24D C19D 121.2(3) . . ? C26A C25A C30A 118.0(3) . . ? C26A C25A C22A 120.2(3) . . ? C30A C25A C22A 121.7(3) . . ? C30B C25B C26B 116.9(3) . . ? C30B C25B C22B 120.6(3) . . ? C26B C25B C22B 122.5(3) . . ? C26C C25C C30C 117.8(3) . . ? C26C C25C C22C 121.0(3) . . ? C30C C25C C22C 121.1(3) . . ? C30D C25D C26D 117.1(3) . . ? C30D C25D C22D 121.2(3) . . ? C26D C25D C22D 121.7(3) . . ? C27A C26A C25A 120.9(3) . . ? C27B C26B C25B 121.5(3) . . ? C27C C26C C25C 121.6(3) . . ? C27D C26D C25D 121.4(4) . . ? C26A C27A C28A 120.2(3) . . ? C28B C27B C26B 120.1(4) . . ? C28C C27C C26C 119.9(4) . . ? C28D C27D C26D 120.1(4) . . ? C29A C28A C27A 119.5(3) . . ? C27B C28B C29B 119.6(4) . . ? C27C C28C C29C 120.0(4) . . ? C27D C28D C29D 119.6(4) . . ? C28A C29A C30A 120.4(3) . . ? C28B C29B C30B 120.2(4) . . ? C28C C29C C30C 120.2(4) . . ? C28D C29D C30D 119.9(4) . . ? C29A C30A C25A 120.9(3) . . ? C29B C30B C25B 121.7(4) . . ? C25C C30C C29C 120.3(4) . . ? C29D C30D C25D 121.7(4) . . ? C101 C100 C102 120.2(4) . . ? C100 C101 C105 120.9(5) . . ? C100 C102 C104 120.9(5) . . ? C104 C103 C105 118.1(5) . . ? C102 C104 C103 119.9(5) . . ? C101 C105 C103 120.0(5) . . ? O3 N200 O1 124.9(7) . . ? O3 N200 C201 119.9(8) . . ? O1 N200 C201 115.2(8) . . ? O4 N202 C203 102.3(10) . . ? 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 N8B Cd1 N1A C6A -176.7(2) . . . . ? N8A Cd1 N1A C6A 1.0(2) . . . . ? N1B Cd1 N1A C6A -105.5(2) . . . . ? N14A Cd1 N1A C6A 3.3(3) . . . . ? N14B Cd1 N1A C6A 110.8(2) . . . . ? N8B Cd1 N1A C2A -0.4(3) . . . . ? N8A Cd1 N1A C2A 177.3(3) . . . . ? N1B Cd1 N1A C2A 70.7(2) . . . . ? N14A Cd1 N1A C2A 179.6(2) . . . . ? N14B Cd1 N1A C2A -72.9(2) . . . . ? N8B Cd1 N1B C2B -179.8(3) . . . . ? N8A Cd1 N1B C2B 0.2(3) . . . . ? N14A Cd1 N1B C2B -72.1(3) . . . . ? N14B Cd1 N1B C2B 178.5(2) . . . . ? N1A Cd1 N1B C2B 70.9(3) . . . . ? N8B Cd1 N1B C6B -0.3(2) . . . . ? N8A Cd1 N1B C6B 179.8(2) . . . . ? N14A Cd1 N1B C6B 107.5(2) . . . . ? N14B Cd1 N1B C6B -1.9(3) . . . . ? N1A Cd1 N1B C6B -109.6(2) . . . . ? N8D Cd2 N1C C2C -7.6(3) . . . . ? N8C Cd2 N1C C2C 177.5(3) . . . . ? N14D Cd2 N1C C2C -79.4(3) . . . . ? N1D Cd2 N1C C2C 64.6(3) . . . . ? N14C Cd2 N1C C2C 169.3(2) . . . . ? N8D Cd2 N1C C6C 166.9(2) . . . . ? N8C Cd2 N1C C6C -8.0(2) . . . . ? N14D Cd2 N1C C6C 95.1(2) . . . . ? N1D Cd2 N1C C6C -120.8(2) . . . . ? N14C Cd2 N1C C6C -16.2(3) . . . . ? N8D Cd2 N1D C6D -0.3(2) . . . . ? N8C Cd2 N1D C6D -176.0(2) . . . . ? N14D Cd2 N1D C6D 6.6(3) . . . . ? N14C Cd2 N1D C6D 114.4(2) . . . . ? N1C Cd2 N1D C6D -104.0(2) . . . . ? N8D Cd2 N1D C2D -179.7(3) . . . . ? N8C Cd2 N1D C2D 4.6(3) . . . . ? N14D Cd2 N1D C2D -172.8(2) . . . . ? N14C Cd2 N1D C2D -65.0(3) . . . . ? N1C Cd2 N1D C2D 76.6(3) . . . . ? N8B Cd1 N8A C9A -96(2) . . . . ? N1B Cd1 N8A C9A -93.7(2) . . . . ? N14A Cd1 N8A C9A 0.3(2) . . . . ? N14B Cd1 N8A C9A 87.4(2) . . . . ? N1A Cd1 N8A C9A 178.7(2) . . . . ? N8B Cd1 N8A C7A 87(2) . . . . ? N1B Cd1 N8A C7A 89.3(2) . . . . ? N14A Cd1 N8A C7A -176.6(2) . . . . ? N14B Cd1 N8A C7A -89.6(2) . . . . ? N1A Cd1 N8A C7A 1.8(2) . . . . ? N8A Cd1 N8B C9B -176(17) . . . . ? N1B Cd1 N8B C9B -178.2(2) . . . . ? N14A Cd1 N8B C9B 88.5(2) . . . . ? N14B Cd1 N8B C9B 0.7(2) . . . . ? N1A Cd1 N8B C9B -91.5(2) . . . . ? N8A Cd1 N8B C7B 1(2) . . . . ? N1B Cd1 N8B C7B -0.9(2) . . . . ? N14A Cd1 N8B C7B -94.2(2) . . . . ? N14B Cd1 N8B C7B 178.0(2) . . . . ? N1A Cd1 N8B C7B 85.9(2) . . . . ? N8D Cd2 N8C C9C 135.6(7) . . . . ? N14D Cd2 N8C C9C 94.3(2) . . . . ? N1D Cd2 N8C C9C -84.0(2) . . . . ? N14C Cd2 N8C C9C 0.4(2) . . . . ? N1C Cd2 N8C C9C -174.0(2) . . . . ? N8D Cd2 N8C C7C -45.3(9) . . . . ? N14D Cd2 N8C C7C -86.5(2) . . . . ? N1D Cd2 N8C C7C 95.1(2) . . . . ? N14C Cd2 N8C C7C 179.5(2) . . . . ? N1C Cd2 N8C C7C 5.1(2) . . . . ? N8C Cd2 N8D C7D 141.8(7) . . . . ? N14D Cd2 N8D C7D -175.6(2) . . . . ? N1D Cd2 N8D C7D -0.2(2) . . . . ? N14C Cd2 N8D C7D -84.8(2) . . . . ? N1C Cd2 N8D C7D 93.0(2) . . . . ? N8C Cd2 N8D C9D -40.3(9) . . . . ? N14D Cd2 N8D C9D 2.3(2) . . . . ? N1D Cd2 N8D C9D 177.7(2) . . . . ? N14C Cd2 N8D C9D 93.1(2) . . . . ? N1C Cd2 N8D C9D -89.1(2) . . . . ? N8B Cd1 N14A C15A -4.4(3) . . . . ? N8A Cd1 N14A C15A 177.9(3) . . . . ? N1B Cd1 N14A C15A -77.5(3) . . . . ? N14B Cd1 N14A C15A 66.8(3) . . . . ? N1A Cd1 N14A C15A 175.6(2) . . . . ? N8B Cd1 N14A C13A 176.5(2) . . . . ? N8A Cd1 N14A C13A -1.1(2) . . . . ? N1B Cd1 N14A C13A 103.4(2) . . . . ? N14B Cd1 N14A C13A -112.2(2) . . . . ? N1A Cd1 N14A C13A -3.5(3) . . . . ? N8B Cd1 N14B C15B 179.5(3) . . . . ? N8A Cd1 N14B C15B -0.6(3) . . . . ? N1B Cd1 N14B C15B -178.8(3) . . . . ? N14A Cd1 N14B C15B 70.3(3) . . . . ? N1A Cd1 N14B C15B -72.8(3) . . . . ? N8B Cd1 N14B C13B 2.9(2) . . . . ? N8A Cd1 N14B C13B -177.2(2) . . . . ? N1B Cd1 N14B C13B 4.5(3) . . . . ? N14A Cd1 N14B C13B -106.4(2) . . . . ? N1A Cd1 N14B C13B 110.6(2) . . . . ? N8D Cd2 N14C C13C -173.9(2) . . . . ? N8C Cd2 N14C C13C 1.2(2) . . . . ? N14D Cd2 N14C C13C -101.2(2) . . . . ? N1D Cd2 N14C C13C 115.7(2) . . . . ? N1C Cd2 N14C C13C 9.4(3) . . . . ? N8D Cd2 N14C C15C 4.0(3) . . . . ? N8C Cd2 N14C C15C 179.0(3) . . . . ? N14D Cd2 N14C C15C 76.6(3) . . . . ? N1D Cd2 N14C C15C -66.5(3) . . . . ? N1C Cd2 N14C C15C -172.8(2) . . . . ? N8D Cd2 N14D C15D 176.2(3) . . . . ? N8C Cd2 N14D C15D -8.3(3) . . . . ? N1D Cd2 N14D C15D 169.3(2) . . . . ? N14C Cd2 N14D C15D 63.3(3) . . . . ? N1C Cd2 N14D C15D -79.6(3) . . . . ? N8D Cd2 N14D C13D -2.8(2) . . . . ? N8C Cd2 N14D C13D 172.7(2) . . . . ? N1D Cd2 N14D C13D -9.7(3) . . . . ? N14C Cd2 N14D C13D -115.7(2) . . . . ? N1C Cd2 N14D C13D 101.4(2) . . . . ? C6A N1A C2A C3A -0.8(5) . . . . ? Cd1 N1A C2A C3A -177.0(2) . . . . ? C6B N1B C2B C3B -0.2(5) . . . . ? Cd1 N1B C2B C3B 179.3(3) . . . . ? C6C N1C C2C C3C 0.6(5) . . . . ? Cd2 N1C C2C C3C 175.0(3) . . . . ? C6D N1D C2D C3D -0.5(5) . . . . ? Cd2 N1D C2D C3D 178.9(3) . . . . ? N1A C2A C3A C4A 0.6(5) . . . . ? N1B C2B C3B C4B -0.4(6) . . . . ? N1C C2C C3C C4C -2.8(6) . . . . ? N1D C2D C3D C4D -0.4(6) . . . . ? C2A C3A C4A C5A 0.8(5) . . . . ? C2B C3B C4B C5B 0.9(6) . . . . ? C2C C3C C4C C5C 2.0(6) . . . . ? C2D C3D C4D C5D 0.7(6) . . . . ? C3A C4A C5A C6A -1.9(5) . . . . ? C3B C4B C5B C6B -0.9(6) . . . . ? C3C C4C C5C C6C 0.6(6) . . . . ? C3D C4D C5D C6D -0.2(6) . . . . ? C2A N1A C6A C5A -0.3(4) . . . . ? Cd1 N1A C6A C5A 176.2(2) . . . . ? C2A N1A C6A C7A -179.8(3) . . . . ? Cd1 N1A C6A C7A -3.4(3) . . . . ? C4A C5A C6A N1A 1.7(5) . . . . ? C4A C5A C6A C7A -178.8(3) . . . . ? C2B N1B C6B C5B 0.2(5) . . . . ? Cd1 N1B C6B C5B -179.4(3) . . . . ? C2B N1B C6B C7B -179.1(3) . . . . ? Cd1 N1B C6B C7B 1.3(4) . . . . ? C4B C5B C6B N1B 0.4(5) . . . . ? C4B C5B C6B C7B 179.6(3) . . . . ? C2C N1C C6C C5C 2.2(5) . . . . ? Cd2 N1C C6C C5C -172.6(3) . . . . ? C2C N1C C6C C7C -175.3(3) . . . . ? Cd2 N1C C6C C7C 9.9(4) . . . . ? C4C C5C C6C N1C -2.8(5) . . . . ? C4C C5C C6C C7C 174.5(3) . . . . ? C2D N1D C6D C5D 1.1(5) . . . . ? Cd2 N1D C6D C5D -178.4(3) . . . . ? C2D N1D C6D C7D -179.9(3) . . . . ? Cd2 N1D C6D C7D 0.7(4) . . . . ? C4D C5D C6D N1D -0.8(6) . . . . ? C4D C5D C6D C7D -179.7(4) . . . . ? C9A N8A C7A C12A -2.7(4) . . . . ? Cd1 N8A C7A C12A 174.2(2) . . . . ? C9A N8A C7A C6A 179.0(3) . . . . ? Cd1 N8A C7A C6A -4.1(3) . . . . ? N1A C6A C7A N8A 4.9(4) . . . . ? C5A C6A C7A N8A -174.6(3) . . . . ? N1A C6A C7A C12A -173.4(3) . . . . ? C5A C6A C7A C12A 7.1(5) . . . . ? C9B N8B C7B C12B 0.0(4) . . . . ? Cd1 N8B C7B C12B -177.3(2) . . . . ? C9B N8B C7B C6B 179.2(3) . . . . ? Cd1 N8B C7B C6B 1.9(3) . . . . ? N1B C6B C7B N8B -2.1(4) . . . . ? C5B C6B C7B N8B 178.6(3) . . . . ? N1B C6B C7B C12B 177.0(3) . . . . ? C5B C6B C7B C12B -2.3(5) . . . . ? C9C N8C C7C C12C 0.7(5) . . . . ? Cd2 N8C C7C C12C -178.4(2) . . . . ? C9C N8C C7C C6C 177.1(3) . . . . ? Cd2 N8C C7C C6C -2.0(4) . . . . ? N1C C6C C7C N8C -5.4(4) . . . . ? C5C C6C C7C N8C 177.2(3) . . . . ? N1C C6C C7C C12C 170.9(3) . . . . ? C5C C6C C7C C12C -6.5(5) . . . . ? C9D N8D C7D C12D 0.2(4) . . . . ? Cd2 N8D C7D C12D 178.0(2) . . . . ? C9D N8D C7D C6D -177.3(3) . . . . ? Cd2 N8D C7D C6D 0.6(3) . . . . ? N1D C6D C7D N8D -0.8(4) . . . . ? C5D C6D C7D N8D 178.2(3) . . . . ? N1D C6D C7D C12D -178.2(3) . . . . ? C5D C6D C7D C12D 0.8(5) . . . . ? C7A N8A C9A C10A -0.2(4) . . . . ? Cd1 N8A C9A C10A -177.2(2) . . . . ? C7A N8A C9A C13A 177.4(3) . . . . ? Cd1 N8A C9A C13A 0.5(3) . . . . ? C7B N8B C9B C10B -1.3(4) . . . . ? Cd1 N8B C9B C10B 176.0(2) . . . . ? C7B N8B C9B C13B 178.9(3) . . . . ? Cd1 N8B C9B C13B -3.8(4) . . . . ? C7C N8C C9C C10C -1.7(5) . . . . ? Cd2 N8C C9C C10C 177.4(2) . . . . ? C7C N8C C9C C13C 179.2(3) . . . . ? Cd2 N8C C9C C13C -1.7(4) . . . . ? C7D N8D C9D C10D -1.3(4) . . . . ? Cd2 N8D C9D C10D -179.2(2) . . . . ? C7D N8D C9D C13D 176.4(3) . . . . ? Cd2 N8D C9D C13D -1.5(3) . . . . ? N8A C9A C10A C11A 3.2(4) . . . . ? C13A C9A C10A C11A -174.3(3) . . . . ? N8B C9B C10B C11B 1.3(5) . . . . ? C13B C9B C10B C11B -178.8(3) . . . . ? N8C C9C C10C C11C 1.1(5) . . . . ? C13C C9C C10C C11C -179.9(3) . . . . ? N8D C9D C10D C11D 1.9(5) . . . . ? C13D C9D C10D C11D -175.7(3) . . . . ? C9A C10A C11A C12A -3.1(4) . . . . ? C9A C10A C11A C19A 176.0(3) . . . . ? C9B C10B C11B C12B -0.2(5) . . . . ? C9B C10B C11B C19B -179.5(3) . . . . ? C9C C10C C11C C12C 0.6(5) . . . . ? C9C C10C C11C C19C -178.7(3) . . . . ? C9D C10D C11D C12D -1.2(4) . . . . ? C9D C10D C11D C19D 177.3(3) . . . . ? N8A C7A C12A C11A 2.6(4) . . . . ? C6A C7A C12A C11A -179.2(3) . . . . ? C10A C11A C12A C7A 0.4(4) . . . . ? C19A C11A C12A C7A -178.7(3) . . . . ? N8B C7B C12B C11B 1.1(5) . . . . ? C6B C7B C12B C11B -178.0(3) . . . . ? C10B C11B C12B C7B -1.0(5) . . . . ? C19B C11B C12B C7B 178.4(3) . . . . ? C10C C11C C12C C7C -1.5(5) . . . . ? C19C C11C C12C C7C 177.7(3) . . . . ? N8C C7C C12C C11C 0.9(5) . . . . ? C6C C7C C12C C11C -175.3(3) . . . . ? N8D C7D C12D C11D 0.5(5) . . . . ? C6D C7D C12D C11D 177.8(3) . . . . ? C10D C11D C12D C7D 0.1(4) . . . . ? C19D C11D C12D C7D -178.5(3) . . . . ? C15A N14A C13A C18A -0.1(5) . . . . ? Cd1 N14A C13A C18A 179.0(2) . . . . ? C15A N14A C13A C9A -177.3(3) . . . . ? Cd1 N14A C13A C9A 1.8(3) . . . . ? N8A C9A C13A N14A -1.5(4) . . . . ? C10A C9A C13A N14A 176.1(3) . . . . ? N8A C9A C13A C18A -178.7(3) . . . . ? C10A C9A C13A C18A -1.1(5) . . . . ? C15B N14B C13B C18B -1.4(5) . . . . ? Cd1 N14B C13B C18B 175.4(3) . . . . ? C15B N14B C13B C9B 177.3(3) . . . . ? Cd1 N14B C13B C9B -5.8(4) . . . . ? N8B C9B C13B N14B 6.4(4) . . . . ? C10B C9B C13B N14B -173.5(3) . . . . ? N8B C9B C13B C18B -174.9(3) . . . . ? C10B C9B C13B C18B 5.3(5) . . . . ? C15C N14C C13C C18C -0.3(5) . . . . ? Cd2 N14C C13C C18C 177.6(2) . . . . ? C15C N14C C13C C9C 179.7(3) . . . . ? Cd2 N14C C13C C9C -2.4(3) . . . . ? N8C C9C C13C N14C 2.7(4) . . . . ? C10C C9C C13C N14C -176.4(3) . . . . ? N8C C9C C13C C18C -177.3(3) . . . . ? C10C C9C C13C C18C 3.6(5) . . . . ? C15D N14D C13D C18D 1.1(5) . . . . ? Cd2 N14D C13D C18D -179.8(2) . . . . ? C15D N14D C13D C9D -176.0(3) . . . . ? Cd2 N14D C13D C9D 3.1(3) . . . . ? N8D C9D C13D N14D -1.1(4) . . . . ? C10D C9D C13D N14D 176.5(3) . . . . ? N8D C9D C13D C18D -178.2(3) . . . . ? C10D C9D C13D C18D -0.5(5) . . . . ? C13A N14A C15A C16A 0.9(5) . . . . ? Cd1 N14A C15A C16A -178.2(3) . . . . ? C13B N14B C15B C16B -0.9(6) . . . . ? Cd1 N14B C15B C16B -177.5(3) . . . . ? C13C N14C C15C C16C -0.4(5) . . . . ? Cd2 N14C C15C C16C -178.2(3) . . . . ? C13D N14D C15D C16D 0.2(5) . . . . ? Cd2 N14D C15D C16D -178.8(3) . . . . ? N14A C15A C16A C17A -0.7(5) . . . . ? N14B C15B C16B C17B 2.0(6) . . . . ? N14C C15C C16C C17C 1.1(5) . . . . ? N14D C15D C16D C17D -1.2(5) . . . . ? C15A C16A C17A C18A -0.2(5) . . . . ? C15B C16B C17B C18B -0.7(6) . . . . ? C15C C16C C17C C18C -1.2(5) . . . . ? C15D C16D C17D C18D 0.9(5) . . . . ? C16A C17A C18A C13A 0.9(5) . . . . ? N14A C13A C18A C17A -0.8(5) . . . . ? C9A C13A C18A C17A 176.3(3) . . . . ? C16B C17B C18B C13B -1.5(6) . . . . ? N14B C13B C18B C17B 2.6(6) . . . . ? C9B C13B C18B C17B -176.1(3) . . . . ? C16C C17C C18C C13C 0.5(6) . . . . ? N14C C13C C18C C17C 0.3(5) . . . . ? C9C C13C C18C C17C -179.7(3) . . . . ? C16D C17D C18D C13D 0.3(6) . . . . ? N14D C13D C18D C17D -1.4(5) . . . . ? C9D C13D C18D C17D 175.5(3) . . . . ? C12A C11A C19A C24A -29.0(5) . . . . ? C10A C11A C19A C24A 151.9(3) . . . . ? C12A C11A C19A C20A 148.0(3) . . . . ? C10A C11A C19A C20A -31.1(5) . . . . ? C10B C11B C19B C24B -150.9(3) . . . . ? C12B C11B C19B C24B 29.8(5) . . . . ? C10B C11B C19B C20B 29.5(5) . . . . ? C12B C11B C19B C20B -149.8(3) . . . . ? C12C C11C C19C C20C 135.8(4) . . . . ? C10C C11C C19C C20C -45.0(5) . . . . ? C12C C11C C19C C24C -43.3(5) . . . . ? C10C C11C C19C C24C 135.9(4) . . . . ? C10D C11D C19D C24D 149.9(3) . . . . ? C12D C11D C19D C24D -31.7(5) . . . . ? C10D C11D C19D C20D -30.2(5) . . . . ? C12D C11D C19D C20D 148.3(3) . . . . ? C24A C19A C20A C21A 1.3(5) . . . . ? C11A C19A C20A C21A -175.8(3) . . . . ? C24B C19B C20B C21B -1.0(5) . . . . ? C11B C19B C20B C21B 178.6(3) . . . . ? C24C C19C C20C C21C -0.1(5) . . . . ? C11C C19C C20C C21C -179.2(3) . . . . ? C24D C19D C20D C21D -0.1(5) . . . . ? C11D C19D C20D C21D 180.0(3) . . . . ? C19A C20A C21A C22A -0.4(5) . . . . ? C19B C20B C21B C22B -0.9(5) . . . . ? C19C C20C C21C C22C 0.2(6) . . . . ? C19D C20D C21D C22D 0.2(6) . . . . ? C20A C21A C22A C23A -0.8(5) . . . . ? C20A C21A C22A C25A 176.3(3) . . . . ? C20B C21B C22B C23B 2.0(5) . . . . ? C20B C21B C22B C25B -176.5(3) . . . . ? C20C C21C C22C C23C -0.2(5) . . . . ? C20C C21C C22C C25C 177.7(3) . . . . ? C20D C21D C22D C23D -0.2(5) . . . . ? C20D C21D C22D C25D -177.5(4) . . . . ? C21A C22A C23A C24A 1.1(5) . . . . ? C25A C22A C23A C24A -176.0(3) . . . . ? C21B C22B C23B C24B -1.3(5) . . . . ? C25B C22B C23B C24B 177.2(3) . . . . ? C21C C22C C23C C24C 0.3(5) . . . . ? C25C C22C C23C C24C -177.6(3) . . . . ? C21D C22D C23D C24D 0.1(5) . . . . ? C25D C22D C23D C24D 177.4(3) . . . . ? C22A C23A C24A C19A -0.2(5) . . . . ? C20A C19A C24A C23A -1.0(5) . . . . ? C11A C19A C24A C23A 176.1(3) . . . . ? C20B C19B C24B C23B 1.7(5) . . . . ? C11B C19B C24B C23B -177.9(3) . . . . ? C22B C23B C24B C19B -0.6(5) . . . . ? C22C C23C C24C C19C -0.3(6) . . . . ? C20C C19C C24C C23C 0.2(6) . . . . ? C11C C19C C24C C23C 179.3(3) . . . . ? C22D C23D C24D C19D -0.1(6) . . . . ? C20D C19D C24D C23D 0.0(5) . . . . ? C11D C19D C24D C23D 180.0(3) . . . . ? C23A C22A C25A C26A 143.2(3) . . . . ? C21A C22A C25A C26A -33.8(5) . . . . ? C23A C22A C25A C30A -34.3(5) . . . . ? C21A C22A C25A C30A 148.6(3) . . . . ? C23B C22B C25B C30B -30.4(5) . . . . ? C21B C22B C25B C30B 148.1(4) . . . . ? C23B C22B C25B C26B 151.3(4) . . . . ? C21B C22B C25B C26B -30.3(5) . . . . ? C21C C22C C25C C26C -34.5(5) . . . . ? C23C C22C C25C C26C 143.4(4) . . . . ? C21C C22C C25C C30C 146.0(4) . . . . ? C23C C22C C25C C30C -36.2(5) . . . . ? C23D C22D C25D C30D -35.6(5) . . . . ? C21D C22D C25D C30D 141.6(4) . . . . ? C23D C22D C25D C26D 145.3(4) . . . . ? C21D C22D C25D C26D -37.6(5) . . . . ? C30A C25A C26A C27A 0.9(5) . . . . ? C22A C25A C26A C27A -176.7(3) . . . . ? C30B C25B C26B C27B 0.7(6) . . . . ? C22B C25B C26B C27B 179.1(3) . . . . ? C30C C25C C26C C27C -1.7(5) . . . . ? C22C C25C C26C C27C 178.8(3) . . . . ? C30D C25D C26D C27D -1.7(6) . . . . ? C22D C25D C26D C27D 177.4(4) . . . . ? C25A C26A C27A C28A -0.2(6) . . . . ? C25B C26B C27B C28B 0.5(6) . . . . ? C25C C26C C27C C28C 1.0(6) . . . . ? C25D C26D C27D C28D 0.8(7) . . . . ? C26A C27A C28A C29A -0.8(6) . . . . ? C26B C27B C28B C29B -1.2(7) . . . . ? C26C C27C C28C C29C 0.6(6) . . . . ? C26D C27D C28D C29D 0.9(7) . . . . ? C27A C28A C29A C30A 1.0(6) . . . . ? C27B C28B C29B C30B 0.8(7) . . . . ? C27C C28C C29C C30C -1.5(6) . . . . ? C27D C28D C29D C30D -1.6(7) . . . . ? C28A C29A C30A C25A -0.3(6) . . . . ? C26A C25A C30A C29A -0.6(5) . . . . ? C22A C25A C30A C29A 176.9(3) . . . . ? C28B C29B C30B C25B 0.5(7) . . . . ? C26B C25B C30B C29B -1.2(6) . . . . ? C22B C25B C30B C29B -179.6(4) . . . . ? C26C C25C C30C C29C 0.7(5) . . . . ? C22C C25C C30C C29C -179.7(3) . . . . ? C28C C29C C30C C25C 0.8(6) . . . . ? C28D C29D C30D C25D 0.6(7) . . . . ? C26D C25D C30D C29D 1.0(6) . . . . ? C22D C25D C30D C29D -178.2(4) . . . . ? C102 C100 C101 C105 -1.6(9) . . . . ? C101 C100 C102 C104 1.0(8) . . . . ? C100 C102 C104 C103 -0.3(9) . . . . ? C105 C103 C104 C102 0.3(9) . . . . ? C100 C101 C105 C103 1.5(10) . . . . ? C104 C103 C105 C101 -0.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.814 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.083 data_mh003 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H30 Cl2 N6 O10.50 Ru' _chemical_formula_weight 958.69 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8240(10) _cell_length_b 20.4730(10) _cell_length_c 24.0870(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.340(10) _cell_angle_gamma 90.00 _cell_volume 4344.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8104 _exptl_absorpt_correction_T_max 0.8982 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14854 _diffrn_reflns_av_R_equivalents 0.0948 _diffrn_reflns_av_sigmaI/netI 0.2299 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.87 _reflns_number_total 9866 _reflns_number_gt 4172 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1157P)^2^+25.4222P] 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 9866 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2577 _refine_ls_R_factor_gt 0.1134 _refine_ls_wR_factor_ref 0.3122 _refine_ls_wR_factor_gt 0.2394 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.37612(9) 0.16438(4) 0.65877(4) 0.0332(3) Uani 1 1 d . . . C29B C 0.1860(17) 0.0941(8) 0.1371(6) 0.071(4) Uani 1 1 d . . . H29B H 0.1306 0.1237 0.1133 0.086 Uiso 1 1 calc R . . N14B N 0.5886(8) 0.1239(4) 0.6481(4) 0.0310(19) Uani 1 1 d . . . N14A N 0.4681(8) 0.2575(4) 0.6537(3) 0.0320(19) Uani 1 1 d . . . N8B N 0.3581(8) 0.1411(4) 0.5793(3) 0.0319(19) Uani 1 1 d . . . C13B C 0.6060(10) 0.1015(5) 0.5955(5) 0.036(3) Uani 1 1 d . . . N1B N 0.1579(9) 0.1972(4) 0.6371(3) 0.035(2) Uani 1 1 d . . . N1A N 0.2884(9) 0.0830(4) 0.6950(4) 0.040(2) Uani 1 1 d . . . C11B C 0.3365(10) 0.1123(5) 0.4661(4) 0.036(2) Uani 1 1 d . . . C9B C 0.4771(10) 0.1133(5) 0.5548(4) 0.031(2) Uani 1 1 d . . . N8A N 0.3994(9) 0.1889(4) 0.7376(4) 0.039(2) Uani 1 1 d . . . C3B C -0.0782(11) 0.2492(6) 0.6493(5) 0.049(3) Uani 1 1 d . . . H3B H -0.1445 0.2704 0.6732 0.058 Uiso 1 1 calc R . . C13A C 0.5031(11) 0.2851(5) 0.7034(4) 0.038(3) Uani 1 1 d . . . C12B C 0.2153(11) 0.1401(5) 0.4935(4) 0.035(2) Uani 1 1 d . . . H12B H 0.1221 0.1485 0.4730 0.042 Uiso 1 1 calc R . . C10B C 0.4670(10) 0.0984(5) 0.4981(4) 0.036(2) Uani 1 1 d . . . H10B H 0.5507 0.0786 0.4816 0.044 Uiso 1 1 calc R . . C19B C 0.3234(11) 0.1007(5) 0.4062(4) 0.036(2) Uani 1 1 d . . . C5B C -0.0257(10) 0.2100(5) 0.5602(4) 0.039(3) Uani 1 1 d . . . H5B H -0.0544 0.2038 0.5219 0.047 Uiso 1 1 calc R . . C17B C 0.8567(11) 0.0630(6) 0.6221(5) 0.046(3) Uani 1 1 d . . . H17B H 0.9483 0.0419 0.6135 0.055 Uiso 1 1 calc R . . C7B C 0.2285(11) 0.1553(5) 0.5486(4) 0.039(3) Uani 1 1 d . . . C18B C 0.7408(11) 0.0711(5) 0.5819(5) 0.042(3) Uani 1 1 d . . . H18B H 0.7525 0.0561 0.5451 0.050 Uiso 1 1 calc R . . C22B C 0.2941(12) 0.0749(5) 0.2896(4) 0.041(3) Uani 1 1 d . . . C6B C 0.1175(11) 0.1873(5) 0.5824(5) 0.038(3) Uani 1 1 d . . . C24B C 0.1988(12) 0.1213(6) 0.3723(5) 0.053(3) Uani 1 1 d . . . H24B H 0.1203 0.1449 0.3888 0.064 Uiso 1 1 calc R . . C23B C 0.1842(11) 0.1091(6) 0.3157(5) 0.045(3) Uani 1 1 d . . . H23B H 0.0971 0.1245 0.2946 0.054 Uiso 1 1 calc R . . C30B C 0.1977(13) 0.1048(6) 0.1928(5) 0.049(3) Uani 1 1 d . . . H30B H 0.1513 0.1423 0.2077 0.058 Uiso 1 1 calc R . . C5A C 0.2200(15) 0.0363(7) 0.7824(6) 0.068(4) Uani 1 1 d . . . H5A H 0.2139 0.0402 0.8215 0.081 Uiso 1 1 calc R . . C4B C -0.1210(11) 0.2405(6) 0.5939(5) 0.046(3) Uani 1 1 d . . . H4B H -0.2169 0.2559 0.5794 0.055 Uiso 1 1 calc R . . C10A C 0.4750(15) 0.2659(7) 0.8075(5) 0.063(4) Uani 1 1 d . . . H10A H 0.5137 0.3077 0.8178 0.076 Uiso 1 1 calc R . . C17A C 0.5975(14) 0.3797(7) 0.6579(6) 0.060(3) Uani 1 1 d . . . H17A H 0.6424 0.4219 0.6591 0.071 Uiso 1 1 calc R . . C21B C 0.4186(12) 0.0529(6) 0.3215(4) 0.043(3) Uani 1 1 d . . . H21B H 0.4952 0.0288 0.3044 0.052 Uiso 1 1 calc R . . C9A C 0.4636(12) 0.2471(6) 0.7521(4) 0.044(3) Uani 1 1 d . . . C15A C 0.4907(11) 0.2895(5) 0.6072(5) 0.039(3) Uani 1 1 d . . . H15A H 0.4621 0.2699 0.5724 0.046 Uiso 1 1 calc R . . C16B C 0.8377(11) 0.0863(6) 0.6752(5) 0.044(3) Uani 1 1 d . . . H16B H 0.9169 0.0818 0.7034 0.053 Uiso 1 1 calc R . . C20B C 0.4338(12) 0.0656(5) 0.3789(5) 0.046(3) Uani 1 1 d . . . H20B H 0.5210 0.0501 0.3997 0.055 Uiso 1 1 calc R . . C28B C 0.253(2) 0.0414(9) 0.1154(6) 0.092(6) Uani 1 1 d . . . H28B H 0.2480 0.0347 0.0763 0.110 Uiso 1 1 calc R . . C18A C 0.5738(12) 0.3462(6) 0.7066(6) 0.053(3) Uani 1 1 d . . . H18A H 0.6051 0.3645 0.7417 0.063 Uiso 1 1 calc R . . C15B C 0.7024(11) 0.1161(5) 0.6870(5) 0.040(3) Uani 1 1 d . . . H15B H 0.6899 0.1316 0.7236 0.048 Uiso 1 1 calc R . . C2A C 0.2356(10) 0.0288(5) 0.6688(6) 0.048(3) Uani 1 1 d . . . H2A H 0.2423 0.0251 0.6297 0.058 Uiso 1 1 calc R . . C12A C 0.3602(17) 0.1630(9) 0.8316(6) 0.088(5) Uani 1 1 d . . . H12A H 0.3219 0.1349 0.8589 0.105 Uiso 1 1 calc R . . C2B C 0.0616(10) 0.2268(5) 0.6699(4) 0.037(2) Uani 1 1 d . . . H2B H 0.0901 0.2326 0.7083 0.044 Uiso 1 1 calc R . . C16A C 0.5556(13) 0.3514(6) 0.6082(5) 0.055(3) Uani 1 1 d . . . H16A H 0.5707 0.3739 0.5745 0.066 Uiso 1 1 calc R . . C26B C 0.3436(17) 0.0074(6) 0.2059(5) 0.062(4) Uani 1 1 d . . . H26B H 0.3995 -0.0228 0.2289 0.075 Uiso 1 1 calc R . . C25B C 0.2770(12) 0.0613(5) 0.2283(5) 0.045(3) Uani 1 1 d . . . C27B C 0.327(2) -0.0015(8) 0.1493(6) 0.092(5) Uani 1 1 d . . . H27B H 0.3696 -0.0394 0.1336 0.111 Uiso 1 1 calc R . . C6A C 0.2858(12) 0.0864(6) 0.7509(5) 0.053(3) Uani 1 1 d . . . C3A C 0.1715(13) -0.0217(6) 0.6978(6) 0.065(4) Uani 1 1 d . . . H3A H 0.1317 -0.0589 0.6785 0.078 Uiso 1 1 calc R . . C11A C 0.4302(19) 0.2237(9) 0.8466(6) 0.092(5) Uani 1 1 d . . . H11A H 0.4458 0.2348 0.8848 0.111 Uiso 1 1 calc R . . C4A C 0.1657(16) -0.0179(7) 0.7543(7) 0.075(4) Uani 1 1 d . . . H4A H 0.1239 -0.0530 0.7742 0.090 Uiso 1 1 calc R . . C7A C 0.3507(14) 0.1470(6) 0.7770(5) 0.054(3) Uani 1 1 d . . . Cl1 Cl 0.8657(6) 0.0328(3) 0.4551(2) 0.1177(18) Uani 1 1 d . . . Cl2 Cl -0.1117(6) 0.2654(5) 0.80003(19) 0.200(4) Uani 1 1 d . . . O1 O 0.2471(14) 0.0440(7) 0.9441(5) 0.094(4) Uiso 1 1 d . . . O2 O 0.6420(11) 0.2300(5) 0.9770(4) 0.081(3) Uiso 1 1 d . . . O3 O -0.1973(10) 0.1653(5) 0.4214(4) 0.051(2) Uiso 1 1 d . . . O4 O -0.0382(14) 0.1600(7) 0.8004(5) 0.117(4) Uiso 1 1 d . . . O5 O 0.3003(12) 0.2997(6) 0.4777(5) 0.098(3) Uiso 1 1 d . . . O6 O 0.536(3) 0.4146(12) 0.4682(9) 0.084(7) Uiso 0.50 1 d P . . O7 O 0.279(3) -0.0010(13) 0.9291(10) 0.096(7) Uiso 0.50 1 d P . . O8 O 0.053(2) 0.2777(11) 0.4195(10) 0.096(7) Uiso 0.50 1 d P . . O9 O 0.159(2) 0.0620(10) 0.9500(8) 0.073(6) Uiso 0.50 1 d P . . O10 O 0.734(5) 0.170(2) 0.8731(18) 0.118(14) Uiso 0.30 1 d P . . O11 O -0.107(5) 0.148(2) 0.9064(19) 0.121(14) Uiso 0.30 1 d P . . O12 O 0.013(6) 0.045(3) 0.876(2) 0.121(17) Uiso 0.25 1 d P . . O13 O 0.520(3) 0.3695(16) 0.4753(12) 0.041(7) Uiso 0.25 1 d P . . O14 O 0.613(3) 0.4305(14) 0.4783(12) 0.037(7) Uiso 0.25 1 d P . . O15 O -0.256(6) 0.175(3) 0.408(2) 0.107(19) Uiso 0.25 1 d P . . O16 O 0.727(4) 0.360(2) 0.4638(16) 0.079(11) Uiso 0.25 1 d P . . O17 O -0.039(6) 0.085(3) 0.848(2) 0.094(17) Uiso 0.20 1 d P . . O18 O 0.965(6) 0.470(2) 0.505(2) 0.093(17) Uiso 0.20 1 d P . . O19 O 0.166(5) 0.127(2) 0.9797(19) 0.100(14) Uiso 0.25 1 d P . . O20 O 0.104(7) 0.289(3) 0.363(3) 0.16(2) Uiso 0.25 1 d P . . O21 O 0.886(3) 0.3991(13) 0.5146(11) 0.120(8) Uiso 0.50 1 d P . . O22 O 0.960(6) 0.359(3) 0.471(2) 0.132(19) Uiso 0.25 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 Ru1 0.0246(4) 0.0350(5) 0.0396(5) -0.0019(5) -0.0015(3) 0.0025(4) C29B 0.086(10) 0.078(11) 0.048(9) -0.003(8) -0.012(8) -0.011(8) N14B 0.026(4) 0.020(4) 0.047(5) -0.003(4) 0.004(4) 0.001(3) N14A 0.028(4) 0.040(5) 0.029(5) -0.004(4) 0.009(4) 0.009(4) N8B 0.016(4) 0.041(5) 0.039(5) 0.002(4) 0.000(4) 0.000(3) C13B 0.018(5) 0.036(6) 0.055(7) -0.012(5) 0.009(5) 0.002(4) N1B 0.033(4) 0.040(5) 0.030(5) 0.001(4) -0.002(4) -0.006(4) N1A 0.033(5) 0.043(6) 0.041(6) 0.002(4) -0.012(4) -0.002(4) C11B 0.026(5) 0.040(6) 0.042(6) -0.011(5) 0.002(5) -0.003(5) C9B 0.027(5) 0.033(6) 0.033(6) 0.001(5) 0.001(4) -0.003(4) N8A 0.030(4) 0.046(6) 0.041(5) 0.005(4) -0.007(4) 0.001(4) C3B 0.029(6) 0.054(8) 0.063(8) -0.010(6) 0.007(6) 0.011(5) C13A 0.039(6) 0.035(6) 0.039(6) -0.013(5) 0.004(5) 0.008(5) C12B 0.030(5) 0.031(5) 0.045(7) -0.004(5) 0.001(5) -0.001(4) C10B 0.024(5) 0.039(6) 0.047(7) -0.001(5) 0.010(5) -0.003(4) C19B 0.038(6) 0.034(6) 0.036(6) -0.001(5) -0.001(5) -0.003(5) C5B 0.021(5) 0.061(8) 0.035(6) -0.001(5) 0.001(4) 0.013(5) C17B 0.024(5) 0.047(7) 0.067(8) 0.009(6) 0.003(5) 0.008(5) C7B 0.031(5) 0.044(7) 0.042(6) 0.005(5) 0.004(5) 0.007(5) C18B 0.032(6) 0.037(6) 0.058(7) 0.001(5) 0.009(5) 0.003(5) C22B 0.050(6) 0.038(6) 0.037(6) -0.009(5) 0.010(5) -0.006(5) C6B 0.037(6) 0.028(5) 0.050(7) -0.001(5) 0.001(5) 0.003(4) C24B 0.037(6) 0.066(9) 0.057(8) -0.027(7) 0.009(6) 0.003(6) C23B 0.031(6) 0.062(8) 0.040(7) -0.005(6) -0.009(5) 0.003(5) C30B 0.050(7) 0.049(7) 0.047(7) 0.002(6) -0.001(6) -0.013(6) C5A 0.076(9) 0.062(9) 0.063(9) 0.025(7) -0.019(7) -0.029(8) C4B 0.028(5) 0.067(8) 0.043(7) -0.003(6) 0.005(5) 0.010(5) C10A 0.074(9) 0.060(9) 0.053(8) 0.005(7) -0.016(7) -0.011(7) C17A 0.062(8) 0.050(8) 0.069(10) 0.010(7) 0.015(7) -0.008(6) C21B 0.045(6) 0.050(7) 0.035(6) -0.005(5) 0.008(5) 0.011(5) C9A 0.037(6) 0.061(8) 0.031(6) -0.008(6) -0.013(5) -0.002(6) C15A 0.044(6) 0.035(6) 0.038(6) -0.011(5) 0.007(5) 0.002(5) C16B 0.031(6) 0.049(7) 0.052(7) 0.002(6) -0.010(5) 0.006(5) C20B 0.041(6) 0.045(7) 0.052(7) -0.004(6) 0.005(5) 0.012(5) C28B 0.151(16) 0.091(13) 0.032(8) -0.014(8) -0.010(9) -0.006(12) C18A 0.045(6) 0.047(8) 0.066(8) -0.013(7) -0.003(6) -0.001(6) C15B 0.027(5) 0.042(7) 0.050(7) 0.002(5) -0.010(5) 0.004(5) C2A 0.018(5) 0.036(7) 0.088(9) 0.004(6) -0.009(5) -0.002(5) C12A 0.081(10) 0.134(15) 0.046(8) 0.027(10) -0.011(7) -0.042(11) C2B 0.028(5) 0.047(7) 0.036(6) 0.002(5) 0.011(5) 0.007(5) C16A 0.059(8) 0.051(8) 0.056(8) -0.005(6) 0.008(6) 0.002(6) C26B 0.115(11) 0.033(7) 0.039(7) -0.005(6) 0.013(7) -0.006(7) C25B 0.051(7) 0.038(7) 0.048(7) 0.001(6) 0.017(6) -0.018(5) C27B 0.158(16) 0.079(11) 0.041(9) -0.015(8) 0.009(9) 0.025(11) C6A 0.039(6) 0.053(8) 0.065(9) 0.017(7) -0.020(6) -0.001(6) C3A 0.047(7) 0.054(8) 0.090(11) 0.031(8) -0.022(7) -0.017(6) C11A 0.116(13) 0.124(15) 0.033(8) -0.012(9) -0.019(8) -0.027(12) C4A 0.074(9) 0.056(9) 0.094(12) 0.037(9) -0.005(9) -0.018(7) C7A 0.068(8) 0.061(9) 0.029(6) 0.011(6) -0.012(6) -0.017(6) Cl1 0.101(3) 0.164(5) 0.089(3) -0.032(3) 0.011(3) -0.004(3) Cl2 0.086(3) 0.452(13) 0.063(3) -0.062(5) 0.023(2) -0.115(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N8A 1.964(9) . ? Ru1 N8B 1.970(8) . ? Ru1 N1A 2.052(9) . ? Ru1 N1B 2.077(8) . ? Ru1 N14A 2.079(9) . ? Ru1 N14B 2.080(7) . ? C29B C28B 1.35(2) . ? C29B C30B 1.358(16) . ? N14B C15B 1.342(12) . ? N14B C13B 1.366(13) . ? N14A C15A 1.323(13) . ? N14A C13A 1.343(12) . ? N8B C7B 1.356(12) . ? N8B C9B 1.359(12) . ? C13B C18B 1.399(13) . ? C13B C9B 1.478(13) . ? N1B C2B 1.339(12) . ? N1B C6B 1.360(13) . ? N1A C2A 1.346(13) . ? N1A C6A 1.349(15) . ? C11B C10B 1.378(14) . ? C11B C12B 1.409(13) . ? C11B C19B 1.460(14) . ? C9B C10B 1.395(14) . ? N8A C9A 1.355(14) . ? N8A C7A 1.368(14) . ? C3B C4B 1.377(15) . ? C3B C2B 1.381(14) . ? C13A C18A 1.398(15) . ? C13A C9A 1.468(15) . ? C12B C7B 1.362(14) . ? C19B C24B 1.396(15) . ? C19B C20B 1.405(14) . ? C5B C4B 1.356(14) . ? C5B C6B 1.422(13) . ? C17B C18B 1.377(14) . ? C17B C16B 1.384(15) . ? C7B C6B 1.464(14) . ? C22B C23B 1.377(14) . ? C22B C21B 1.378(14) . ? C22B C25B 1.502(15) . ? C24B C23B 1.383(15) . ? C30B C25B 1.395(15) . ? C5A C4A 1.372(18) . ? C5A C6A 1.419(17) . ? C10A C11A 1.354(19) . ? C10A C9A 1.385(16) . ? C17A C16A 1.360(17) . ? C17A C18A 1.386(17) . ? C21B C20B 1.406(15) . ? C15A C16A 1.390(15) . ? C16B C15B 1.385(14) . ? C28B C27B 1.34(2) . ? C2A C3A 1.388(16) . ? C12A C7A 1.353(18) . ? C12A C11A 1.43(2) . ? C26B C25B 1.375(16) . ? C26B C27B 1.376(17) . ? C6A C7A 1.492(16) . ? C3A C4A 1.366(19) . ? O1 O9 0.88(2) . ? O1 O7 1.03(2) . ? O3 O15 0.62(5) . ? O6 O14 0.78(3) . ? O6 O13 0.95(3) . ? O7 O9 1.76(3) . ? O8 O20 1.48(7) . ? O9 O19 1.52(5) . ? O10 O11 1.63(6) 1_655 ? O11 O10 1.64(6) 1_455 ? O11 O22 1.64(7) 4_466 ? O12 O17 1.14(6) . ? O13 O14 1.49(4) . ? O14 O16 1.81(5) . ? O18 O18 1.39(10) 3_766 ? O18 O21 1.63(5) . ? O21 O22 1.51(6) . ? O22 O11 1.64(6) 4_665 ? 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 N8A Ru1 N8B 178.4(3) . . ? N8A Ru1 N1A 79.5(4) . . ? N8B Ru1 N1A 101.9(3) . . ? N8A Ru1 N1B 101.7(3) . . ? N8B Ru1 N1B 79.2(3) . . ? N1A Ru1 N1B 90.1(3) . . ? N8A Ru1 N14A 78.6(4) . . ? N8B Ru1 N14A 100.0(3) . . ? N1A Ru1 N14A 158.1(3) . . ? N1B Ru1 N14A 92.7(3) . . ? N8A Ru1 N14B 100.2(3) . . ? N8B Ru1 N14B 78.8(3) . . ? N1A Ru1 N14B 95.4(3) . . ? N1B Ru1 N14B 158.0(3) . . ? N14A Ru1 N14B 90.1(3) . . ? C28B C29B C30B 120.1(14) . . ? C15B N14B C13B 119.2(8) . . ? C15B N14B Ru1 127.2(7) . . ? C13B N14B Ru1 113.5(6) . . ? C15A N14A C13A 120.5(9) . . ? C15A N14A Ru1 125.7(7) . . ? C13A N14A Ru1 113.8(7) . . ? C7B N8B C9B 120.1(9) . . ? C7B N8B Ru1 119.7(7) . . ? C9B N8B Ru1 120.2(6) . . ? N14B C13B C18B 120.6(9) . . ? N14B C13B C9B 115.9(8) . . ? C18B C13B C9B 123.4(10) . . ? C2B N1B C6B 120.0(8) . . ? C2B N1B Ru1 127.6(7) . . ? C6B N1B Ru1 112.4(7) . . ? C2A N1A C6A 118.9(10) . . ? C2A N1A Ru1 126.8(8) . . ? C6A N1A Ru1 114.3(7) . . ? C10B C11B C12B 116.9(9) . . ? C10B C11B C19B 122.4(9) . . ? C12B C11B C19B 120.7(9) . . ? N8B C9B C10B 120.6(8) . . ? N8B C9B C13B 111.4(8) . . ? C10B C9B C13B 128.0(9) . . ? C9A N8A C7A 121.0(10) . . ? C9A N8A Ru1 119.6(7) . . ? C7A N8A Ru1 119.4(7) . . ? C4B C3B C2B 119.7(10) . . ? N14A C13A C18A 120.3(11) . . ? N14A C13A C9A 115.9(9) . . ? C18A C13A C9A 123.8(10) . . ? C7B C12B C11B 121.6(9) . . ? C11B C10B C9B 120.4(9) . . ? C24B C19B C20B 115.1(10) . . ? C24B C19B C11B 122.9(10) . . ? C20B C19B C11B 121.9(9) . . ? C4B C5B C6B 119.6(10) . . ? C18B C17B C16B 118.9(10) . . ? N8B C7B C12B 120.2(9) . . ? N8B C7B C6B 111.3(9) . . ? C12B C7B C6B 128.5(9) . . ? C17B C18B C13B 119.7(11) . . ? C23B C22B C21B 118.2(10) . . ? C23B C22B C25B 120.6(10) . . ? C21B C22B C25B 121.2(10) . . ? N1B C6B C5B 119.6(9) . . ? N1B C6B C7B 117.4(9) . . ? C5B C6B C7B 123.0(10) . . ? C23B C24B C19B 123.1(10) . . ? C22B C23B C24B 120.9(10) . . ? C29B C30B C25B 120.7(13) . . ? C4A C5A C6A 117.5(13) . . ? C5B C4B C3B 119.7(10) . . ? C11A C10A C9A 119.0(13) . . ? C16A C17A C18A 119.2(12) . . ? C22B C21B C20B 120.9(10) . . ? N8A C9A C10A 119.9(11) . . ? N8A C9A C13A 112.0(9) . . ? C10A C9A C13A 128.0(11) . . ? N14A C15A C16A 121.2(10) . . ? C17B C16B C15B 119.6(10) . . ? C19B C20B C21B 121.8(10) . . ? C27B C28B C29B 119.8(13) . . ? C17A C18A C13A 118.9(11) . . ? N14B C15B C16B 121.9(10) . . ? N1A C2A C3A 121.3(13) . . ? C7A C12A C11A 117.2(13) . . ? N1B C2B C3B 121.5(10) . . ? C17A C16A C15A 119.6(12) . . ? C25B C26B C27B 118.2(13) . . ? C26B C25B C30B 118.8(11) . . ? C26B C25B C22B 120.9(11) . . ? C30B C25B C22B 120.3(11) . . ? C28B C27B C26B 122.4(15) . . ? N1A C6A C5A 121.9(12) . . ? N1A C6A C7A 115.8(10) . . ? C5A C6A C7A 122.2(12) . . ? C4A C3A C2A 119.9(13) . . ? C10A C11A C12A 121.3(13) . . ? C3A C4A C5A 120.3(13) . . ? C12A C7A N8A 121.3(12) . . ? C12A C7A C6A 127.8(12) . . ? N8A C7A C6A 110.9(10) . . ? O9 O1 O7 133(3) . . ? O14 O6 O13 118(4) . . ? O1 O7 O9 21.2(13) . . ? O1 O9 O19 116(3) . . ? O1 O9 O7 25.3(15) . . ? O19 O9 O7 141(2) . . ? O10 O11 O22 138(4) 1_455 4_466 ? O6 O13 O14 27(2) . . ? O6 O14 O13 34(3) . . ? O6 O14 O16 95(4) . . ? O13 O14 O16 68(2) . . ? O18 O18 O21 179(7) 3_766 . ? O22 O21 O18 100(3) . . ? O21 O22 O11 124(4) . 4_665 ? 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 N8A Ru1 N14B C15B 2.1(9) . . . . ? N8B Ru1 N14B C15B -179.2(9) . . . . ? N1A Ru1 N14B C15B -78.1(8) . . . . ? N1B Ru1 N14B C15B 178.1(8) . . . . ? N14A Ru1 N14B C15B 80.6(8) . . . . ? N8A Ru1 N14B C13B 179.8(7) . . . . ? N8B Ru1 N14B C13B -1.6(7) . . . . ? N1A Ru1 N14B C13B 99.5(7) . . . . ? N1B Ru1 N14B C13B -4.3(12) . . . . ? N14A Ru1 N14B C13B -101.8(7) . . . . ? N8A Ru1 N14A C15A -175.9(8) . . . . ? N8B Ru1 N14A C15A 5.0(8) . . . . ? N1A Ru1 N14A C15A -171.6(8) . . . . ? N1B Ru1 N14A C15A -74.5(8) . . . . ? N14B Ru1 N14A C15A 83.7(8) . . . . ? N8A Ru1 N14A C13A 3.2(6) . . . . ? N8B Ru1 N14A C13A -175.9(6) . . . . ? N1A Ru1 N14A C13A 7.5(12) . . . . ? N1B Ru1 N14A C13A 104.6(7) . . . . ? N14B Ru1 N14A C13A -97.2(7) . . . . ? N8A Ru1 N8B C7B -124(12) . . . . ? N1A Ru1 N8B C7B 88.4(8) . . . . ? N1B Ru1 N8B C7B 0.6(7) . . . . ? N14A Ru1 N8B C7B -90.3(8) . . . . ? N14B Ru1 N8B C7B -178.4(8) . . . . ? N8A Ru1 N8B C9B 53(13) . . . . ? N1A Ru1 N8B C9B -94.1(7) . . . . ? N1B Ru1 N8B C9B 178.1(8) . . . . ? N14A Ru1 N8B C9B 87.1(7) . . . . ? N14B Ru1 N8B C9B -0.9(7) . . . . ? C15B N14B C13B C18B -0.3(15) . . . . ? Ru1 N14B C13B C18B -178.1(8) . . . . ? C15B N14B C13B C9B -178.5(9) . . . . ? Ru1 N14B C13B C9B 3.7(11) . . . . ? N8A Ru1 N1B C2B -0.3(9) . . . . ? N8B Ru1 N1B C2B -178.9(9) . . . . ? N1A Ru1 N1B C2B 79.0(9) . . . . ? N14A Ru1 N1B C2B -79.3(9) . . . . ? N14B Ru1 N1B C2B -176.3(8) . . . . ? N8A Ru1 N1B C6B 177.8(7) . . . . ? N8B Ru1 N1B C6B -0.8(7) . . . . ? N1A Ru1 N1B C6B -102.9(7) . . . . ? N14A Ru1 N1B C6B 98.9(7) . . . . ? N14B Ru1 N1B C6B 1.9(13) . . . . ? N8A Ru1 N1A C2A -178.4(8) . . . . ? N8B Ru1 N1A C2A 0.7(8) . . . . ? N1B Ru1 N1A C2A 79.7(8) . . . . ? N14A Ru1 N1A C2A 177.4(7) . . . . ? N14B Ru1 N1A C2A -79.0(8) . . . . ? N8A Ru1 N1A C6A 1.6(7) . . . . ? N8B Ru1 N1A C6A -179.3(7) . . . . ? N1B Ru1 N1A C6A -100.3(8) . . . . ? N14A Ru1 N1A C6A -2.7(13) . . . . ? N14B Ru1 N1A C6A 101.0(7) . . . . ? C7B N8B C9B C10B -0.6(14) . . . . ? Ru1 N8B C9B C10B -178.1(7) . . . . ? C7B N8B C9B C13B -179.5(9) . . . . ? Ru1 N8B C9B C13B 3.0(11) . . . . ? N14B C13B C9B N8B -4.3(13) . . . . ? C18B C13B C9B N8B 177.5(10) . . . . ? N14B C13B C9B C10B 176.9(10) . . . . ? C18B C13B C9B C10B -1.2(17) . . . . ? N8B Ru1 N8A C9A 31(13) . . . . ? N1A Ru1 N8A C9A 178.9(8) . . . . ? N1B Ru1 N8A C9A -93.2(8) . . . . ? N14A Ru1 N8A C9A -2.8(7) . . . . ? N14B Ru1 N8A C9A 85.2(8) . . . . ? N8B Ru1 N8A C7A -148(12) . . . . ? N1A Ru1 N8A C7A -1.1(8) . . . . ? N1B Ru1 N8A C7A 86.8(9) . . . . ? N14A Ru1 N8A C7A 177.3(9) . . . . ? N14B Ru1 N8A C7A -94.7(8) . . . . ? C15A N14A C13A C18A -4.4(14) . . . . ? Ru1 N14A C13A C18A 176.4(8) . . . . ? C15A N14A C13A C9A 175.9(9) . . . . ? Ru1 N14A C13A C9A -3.2(11) . . . . ? C10B C11B C12B C7B 2.8(15) . . . . ? C19B C11B C12B C7B -175.6(10) . . . . ? C12B C11B C10B C9B -1.6(15) . . . . ? C19B C11B C10B C9B 176.7(9) . . . . ? N8B C9B C10B C11B 0.6(15) . . . . ? C13B C9B C10B C11B 179.2(10) . . . . ? C10B C11B C19B C24B -172.5(11) . . . . ? C12B C11B C19B C24B 5.8(16) . . . . ? C10B C11B C19B C20B 10.1(16) . . . . ? C12B C11B C19B C20B -171.7(10) . . . . ? C9B N8B C7B C12B 1.8(15) . . . . ? Ru1 N8B C7B C12B 179.3(8) . . . . ? C9B N8B C7B C6B -177.7(9) . . . . ? Ru1 N8B C7B C6B -0.2(12) . . . . ? C11B C12B C7B N8B -2.9(16) . . . . ? C11B C12B C7B C6B 176.5(10) . . . . ? C16B C17B C18B C13B -1.0(16) . . . . ? N14B C13B C18B C17B 0.7(16) . . . . ? C9B C13B C18B C17B 178.8(10) . . . . ? C2B N1B C6B C5B 1.4(15) . . . . ? Ru1 N1B C6B C5B -176.8(8) . . . . ? C2B N1B C6B C7B 179.3(9) . . . . ? Ru1 N1B C6B C7B 1.0(12) . . . . ? C4B C5B C6B N1B -0.7(16) . . . . ? C4B C5B C6B C7B -178.4(11) . . . . ? N8B C7B C6B N1B -0.5(14) . . . . ? C12B C7B C6B N1B 180.0(10) . . . . ? N8B C7B C6B C5B 177.2(10) . . . . ? C12B C7B C6B C5B -2.3(18) . . . . ? C20B C19B C24B C23B -0.7(17) . . . . ? C11B C19B C24B C23B -178.3(11) . . . . ? C21B C22B C23B C24B 0.3(17) . . . . ? C25B C22B C23B C24B 179.6(10) . . . . ? C19B C24B C23B C22B 0.4(19) . . . . ? C28B C29B C30B C25B -1(2) . . . . ? C6B C5B C4B C3B -0.1(18) . . . . ? C2B C3B C4B C5B 0.2(18) . . . . ? C23B C22B C21B C20B -0.6(17) . . . . ? C25B C22B C21B C20B -179.9(10) . . . . ? C7A N8A C9A C10A -2.6(16) . . . . ? Ru1 N8A C9A C10A 177.5(9) . . . . ? C7A N8A C9A C13A -178.2(10) . . . . ? Ru1 N8A C9A C13A 1.8(11) . . . . ? C11A C10A C9A N8A 4.1(19) . . . . ? C11A C10A C9A C13A 179.0(13) . . . . ? N14A C13A C9A N8A 1.1(13) . . . . ? C18A C13A C9A N8A -178.5(9) . . . . ? N14A C13A C9A C10A -174.1(11) . . . . ? C18A C13A C9A C10A 6.3(18) . . . . ? C13A N14A C15A C16A 2.1(15) . . . . ? Ru1 N14A C15A C16A -178.8(8) . . . . ? C18B C17B C16B C15B 0.9(17) . . . . ? C24B C19B C20B C21B 0.4(16) . . . . ? C11B C19B C20B C21B 178.0(10) . . . . ? C22B C21B C20B C19B 0.3(18) . . . . ? C30B C29B C28B C27B 2(3) . . . . ? C16A C17A C18A C13A -2.0(18) . . . . ? N14A C13A C18A C17A 4.4(16) . . . . ? C9A C13A C18A C17A -176.1(11) . . . . ? C13B N14B C15B C16B 0.3(15) . . . . ? Ru1 N14B C15B C16B 177.8(8) . . . . ? C17B C16B C15B N14B -0.6(17) . . . . ? C6A N1A C2A C3A 3.5(14) . . . . ? Ru1 N1A C2A C3A -176.6(8) . . . . ? C6B N1B C2B C3B -1.4(16) . . . . ? Ru1 N1B C2B C3B 176.6(8) . . . . ? C4B C3B C2B N1B 0.5(17) . . . . ? C18A C17A C16A C15A -0.3(18) . . . . ? N14A C15A C16A C17A 0.3(17) . . . . ? C27B C26B C25B C30B -0.8(19) . . . . ? C27B C26B C25B C22B -178.4(13) . . . . ? C29B C30B C25B C26B 0.2(17) . . . . ? C29B C30B C25B C22B 177.7(11) . . . . ? C23B C22B C25B C26B -152.3(12) . . . . ? C21B C22B C25B C26B 26.9(16) . . . . ? C23B C22B C25B C30B 30.1(16) . . . . ? C21B C22B C25B C30B -150.6(11) . . . . ? C29B C28B C27B C26B -3(3) . . . . ? C25B C26B C27B C28B 2(3) . . . . ? C2A N1A C6A C5A -4.2(16) . . . . ? Ru1 N1A C6A C5A 175.9(9) . . . . ? C2A N1A C6A C7A 178.1(9) . . . . ? Ru1 N1A C6A C7A -1.8(12) . . . . ? C4A C5A C6A N1A 3.4(19) . . . . ? C4A C5A C6A C7A -179.0(12) . . . . ? N1A C2A C3A C4A -2.2(17) . . . . ? C9A C10A C11A C12A -5(2) . . . . ? C7A C12A C11A C10A 5(2) . . . . ? C2A C3A C4A C5A 1(2) . . . . ? C6A C5A C4A C3A -2(2) . . . . ? C11A C12A C7A N8A -3(2) . . . . ? C11A C12A C7A C6A 178.8(13) . . . . ? C9A N8A C7A C12A 2.2(18) . . . . ? Ru1 N8A C7A C12A -177.9(11) . . . . ? C9A N8A C7A C6A -179.5(9) . . . . ? Ru1 N8A C7A C6A 0.4(13) . . . . ? N1A C6A C7A C12A 179.1(13) . . . . ? C5A C6A C7A C12A 1(2) . . . . ? N1A C6A C7A N8A 0.9(14) . . . . ? C5A C6A C7A N8A -176.7(11) . . . . ? O7 O1 O9 O19 173(3) . . . . ? O1 O7 O9 O19 -10(4) . . . . ? O13 O6 O14 O16 37(5) . . . . ? O6 O13 O14 O16 -140(5) . . . . ? O18 O18 O21 O22 0(100) 3_766 . . . ? O18 O21 O22 O11 -89(5) . . . 4_665 ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.402 _refine_diff_density_min -1.489 _refine_diff_density_rms 0.159