Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Mike Ward' 'Harry Adams' 'Giusseppe Calgero' 'Stephen Faulkner' 'Theodore Lazarides' 'Daniel Sykes' _publ_contact_author_name 'Mike Ward' _publ_contact_author_address ; Department of Chemistry University of Sheffield Dainton Building Sheffield S3 7HF UNITED KINGDOM ; _publ_contact_author_email M.D.WARD@SHEFFIELD.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Heteronuclear bipyrimidine-bridged Ru-Ln and Os-Ln dyads: low-energy 3MLCT states as energy-donors to Yb(III) and Nd(III) ; data_prwnt4m _database_code_depnum_ccdc_archive 'CCDC 661953' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H51 Cl2 F18 N6 Nd O7 Ru' _chemical_formula_weight 1482.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.036(3) _cell_length_b 14.384(3) _cell_length_c 16.284(3) _cell_angle_alpha 75.965(4) _cell_angle_beta 84.187(4) _cell_angle_gamma 84.216(4) _cell_volume 2937.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4744 _cell_measurement_theta_min 4.467 _cell_measurement_theta_max 52.719 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1474 _exptl_absorpt_coefficient_mu 1.331 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6909 _exptl_absorpt_correction_T_max 0.9244 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 34073 _diffrn_reflns_av_R_equivalents 0.1047 _diffrn_reflns_av_sigmaI/netI 0.1432 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.57 _reflns_number_total 13204 _reflns_number_gt 8137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0954P)^2^+2.2816P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13204 _refine_ls_number_parameters 713 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1301 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.2036 _refine_ls_wR_factor_gt 0.1750 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.042 _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 Nd1 Nd 0.06395(3) 0.30318(3) 0.36555(2) 0.01836(14) Uani 1 1 d . . . Ru1 Ru -0.03208(5) 0.08989(4) 0.74183(4) 0.01673(16) Uani 1 1 d . . . Cl1 Cl -0.15871(16) 0.04834(14) 0.66062(12) 0.0237(4) Uani 1 1 d . . . Cl2 Cl 0.00310(16) -0.07360(14) 0.82081(11) 0.0224(4) Uani 1 1 d . . . O1 O 0.1954(4) 0.3639(4) 0.4344(3) 0.0239(13) Uani 1 1 d . . . O2 O 0.2341(4) 0.2381(4) 0.3228(3) 0.0243(13) Uani 1 1 d . . . O3 O -0.0350(4) 0.4585(4) 0.3512(3) 0.0226(13) Uani 1 1 d . . . O4 O -0.1226(4) 0.2782(4) 0.3945(3) 0.0226(12) Uani 1 1 d . . . O5 O -0.0169(4) 0.3259(4) 0.2330(3) 0.0228(13) Uani 1 1 d . . . O6 O 0.1506(4) 0.4253(4) 0.2539(3) 0.0265(13) Uani 1 1 d . . . O7 O 0.0419(4) 0.1512(4) 0.3313(3) 0.0253(13) Uani 1 1 d D . . H1W H 0.0390 0.1557 0.2785 0.030 Uiso 1 1 d RD . . H2W H 0.0418 0.0917 0.3551 0.030 Uiso 1 1 d RD . . N1 N -0.1365(5) 0.1130(5) 0.8388(4) 0.0191(14) Uani 1 1 d . . . N2 N 0.0615(5) 0.1271(4) 0.8192(4) 0.0190(14) Uani 1 1 d . . . N3 N -0.0510(5) 0.2221(4) 0.6676(4) 0.0176(14) Uani 1 1 d . . . N4 N 0.0728(5) 0.0770(5) 0.6409(4) 0.0208(15) Uani 1 1 d . . . N5 N -0.0141(5) 0.3128(5) 0.5253(4) 0.0204(15) Uani 1 1 d . . . N6 N 0.1131(5) 0.1549(4) 0.4963(4) 0.0168(14) Uani 1 1 d . . . F1 F 0.4384(4) 0.4269(5) 0.4596(4) 0.0562(17) Uani 1 1 d . . . F2 F 0.3399(5) 0.3551(5) 0.5627(4) 0.066(2) Uani 1 1 d . . . F3 F 0.2885(5) 0.4930(5) 0.4890(4) 0.0617(19) Uani 1 1 d . . . F4 F 0.4994(5) 0.2210(7) 0.2775(6) 0.105(3) Uani 1 1 d . . . F5 F 0.3898(5) 0.2641(7) 0.1854(5) 0.092(3) Uani 1 1 d . . . F6 F 0.3883(5) 0.1250(7) 0.2689(6) 0.095(3) Uani 1 1 d . . . F7 F -0.0714(5) 0.6281(4) 0.2326(4) 0.0527(16) Uani 1 1 d . . . F8 F -0.2341(5) 0.6233(4) 0.2642(4) 0.0536(17) Uani 1 1 d . . . F9 F -0.1344(4) 0.6432(4) 0.3541(3) 0.0394(13) Uani 1 1 d . . . F10 F -0.3816(5) 0.3381(5) 0.3601(7) 0.101(3) Uani 1 1 d . . . F11 F -0.3166(6) 0.2318(6) 0.4603(6) 0.102(3) Uani 1 1 d . . . F12 F -0.2898(5) 0.2130(5) 0.3377(5) 0.0645(19) Uani 1 1 d . . . F13 F -0.1965(5) 0.3572(5) 0.1621(4) 0.069(2) Uani 1 1 d . . . F14 F -0.0881(5) 0.3230(5) 0.0682(4) 0.0596(18) Uani 1 1 d . . . F15 F -0.1416(7) 0.4679(5) 0.0660(5) 0.087(3) Uani 1 1 d . . . F16 F 0.2553(5) 0.5276(5) 0.0843(4) 0.070(2) Uani 1 1 d . . . F17 F 0.1421(6) 0.6379(5) 0.1057(4) 0.071(2) Uani 1 1 d . . . F18 F 0.2520(5) 0.5795(4) 0.1952(3) 0.0467(15) Uani 1 1 d . . . C1 C -0.2386(7) 0.1136(6) 0.8418(5) 0.0245(19) Uani 1 1 d . . . H1 H -0.2681 0.1057 0.7932 0.029 Uiso 1 1 calc R . . C2 C -0.3042(6) 0.1249(6) 0.9102(5) 0.0262(19) Uani 1 1 d . . . H2 H -0.3769 0.1285 0.9073 0.031 Uiso 1 1 calc R . . C3 C -0.2621(6) 0.1312(6) 0.9860(4) 0.0215(18) Uani 1 1 d . . . C4 C -0.1557(6) 0.1311(5) 0.9823(5) 0.0201(17) Uani 1 1 d . . . H4 H -0.1240 0.1354 1.0311 0.024 Uiso 1 1 calc R . . C5 C -0.0945(6) 0.1248(6) 0.9092(4) 0.0193(17) Uani 1 1 d . . . C6 C -0.3361(7) 0.1439(6) 1.0631(5) 0.0255(19) Uani 1 1 d . . . C7 C -0.3846(7) 0.2464(7) 1.0424(6) 0.039(2) Uani 1 1 d . . . H7A H -0.4318 0.2574 1.0904 0.046 Uiso 1 1 calc R . . H7B H -0.4231 0.2568 0.9919 0.046 Uiso 1 1 calc R . . H7C H -0.3301 0.2911 1.0314 0.046 Uiso 1 1 calc R . . C8 C -0.4191(7) 0.0730(7) 1.0821(5) 0.037(2) Uani 1 1 d . . . H8A H -0.4645 0.0827 1.1316 0.045 Uiso 1 1 calc R . . H8B H -0.3864 0.0072 1.0941 0.045 Uiso 1 1 calc R . . H8C H -0.4599 0.0832 1.0329 0.045 Uiso 1 1 calc R . . C9 C -0.2786(7) 0.1267(7) 1.1432(5) 0.033(2) Uani 1 1 d . . . H9A H -0.2470 0.0606 1.1563 0.049 Uiso 1 1 calc R . . H9B H -0.3273 0.1368 1.1907 0.049 Uiso 1 1 calc R . . H9C H -0.2245 0.1716 1.1340 0.049 Uiso 1 1 calc R . . C10 C 0.0186(6) 0.1373(5) 0.8957(5) 0.0193(17) Uani 1 1 d . . . C11 C 0.0739(6) 0.1625(6) 0.9541(5) 0.0218(18) Uani 1 1 d . . . H11 H 0.0409 0.1671 1.0079 0.026 Uiso 1 1 calc R . . C12 C 0.1776(6) 0.1814(6) 0.9350(5) 0.0207(17) Uani 1 1 d . . . C13 C 0.2213(6) 0.1697(6) 0.8556(5) 0.0208(17) Uani 1 1 d . . . H13 H 0.2919 0.1806 0.8391 0.025 Uiso 1 1 calc R . . C14 C 0.1621(6) 0.1426(5) 0.8013(5) 0.0191(17) Uani 1 1 d . . . H14 H 0.1941 0.1343 0.7483 0.023 Uiso 1 1 calc R . . C15 C 0.2394(7) 0.2135(6) 0.9969(5) 0.0271(19) Uani 1 1 d . . . C16 C 0.1712(8) 0.2825(7) 1.0405(7) 0.045(3) Uani 1 1 d . . . H16A H 0.2109 0.3026 1.0803 0.054 Uiso 1 1 calc R . . H16B H 0.1112 0.2503 1.0715 0.054 Uiso 1 1 calc R . . H16C H 0.1475 0.3391 0.9977 0.054 Uiso 1 1 calc R . . C17 C 0.2707(8) 0.1224(7) 1.0663(6) 0.041(2) Uani 1 1 d . . . H17A H 0.3147 0.0767 1.0397 0.049 Uiso 1 1 calc R . . H17B H 0.2083 0.0923 1.0948 0.049 Uiso 1 1 calc R . . H17C H 0.3088 0.1409 1.1080 0.049 Uiso 1 1 calc R . . C18 C 0.3359(8) 0.2592(8) 0.9539(6) 0.051(3) Uani 1 1 d . . . H18A H 0.3792 0.2138 0.9264 0.061 Uiso 1 1 calc R . . H18B H 0.3744 0.2760 0.9962 0.061 Uiso 1 1 calc R . . H18C H 0.3168 0.3174 0.9110 0.061 Uiso 1 1 calc R . . C19 C -0.1074(6) 0.2990(6) 0.6849(5) 0.0212(18) Uani 1 1 d . . . H19 H -0.1399 0.2944 0.7405 0.025 Uiso 1 1 calc R . . C20 C -0.1202(6) 0.3850(6) 0.6250(5) 0.0224(18) Uani 1 1 d . . . H20 H -0.1594 0.4395 0.6385 0.027 Uiso 1 1 calc R . . C21 C -0.0730(6) 0.3878(6) 0.5445(5) 0.0210(17) Uani 1 1 d . . . H21 H -0.0826 0.4448 0.5012 0.025 Uiso 1 1 calc R . . C22 C -0.0046(6) 0.2333(6) 0.5869(4) 0.0184(17) Uani 1 1 d . . . C23 C 0.0642(6) 0.1512(6) 0.5722(4) 0.0202(17) Uani 1 1 d . . . C24 C 0.1377(6) 0.0002(6) 0.6313(5) 0.0233(18) Uani 1 1 d . . . H24 H 0.1454 -0.0539 0.6778 0.028 Uiso 1 1 calc R . . C25 C 0.1923(6) -0.0001(6) 0.5550(5) 0.0218(18) Uani 1 1 d . . . H25 H 0.2391 -0.0532 0.5482 0.026 Uiso 1 1 calc R . . C26 C 0.1773(6) 0.0801(5) 0.4869(5) 0.0195(17) Uani 1 1 d . . . H26 H 0.2138 0.0807 0.4333 0.023 Uiso 1 1 calc R . . C27 C 0.3410(8) 0.4101(8) 0.4843(6) 0.041(2) Uani 1 1 d . . . C28 C 0.2928(6) 0.3591(6) 0.4266(5) 0.0236(18) Uani 1 1 d . . . C29 C 0.3577(7) 0.3129(7) 0.3757(6) 0.033(2) Uani 1 1 d . . . H29 H 0.4298 0.3192 0.3742 0.040 Uiso 1 1 calc R . . C30 C 0.3251(7) 0.2568(7) 0.3257(5) 0.032(2) Uani 1 1 d . . . C31 C 0.4030(8) 0.2143(10) 0.2658(8) 0.058(4) Uani 1 1 d . . . C32 C -0.1445(7) 0.5937(7) 0.2964(5) 0.033(2) Uani 1 1 d . . . C33 C -0.1243(8) 0.4875(7) 0.3289(6) 0.039(2) Uani 1 1 d . . . C34 C -0.2079(8) 0.4329(7) 0.3357(6) 0.038(2) Uani 1 1 d . . . H34 H -0.2724 0.4637 0.3176 0.045 Uiso 1 1 calc R . . C35 C -0.1988(8) 0.3298(7) 0.3700(6) 0.038(2) Uani 1 1 d . . . C36 C -0.2980(8) 0.2813(7) 0.3856(8) 0.048(3) Uani 1 1 d . . . C37 C -0.1132(8) 0.3871(7) 0.1149(5) 0.032(2) Uani 1 1 d . . . C38 C -0.0263(8) 0.3927(7) 0.1687(6) 0.040(2) Uani 1 1 d . . . C39 C 0.0383(8) 0.4690(7) 0.1413(6) 0.036(2) Uani 1 1 d . . . H39 H 0.0254 0.5158 0.0905 0.044 Uiso 1 1 calc R . . C40 C 0.1203(7) 0.4778(7) 0.1862(6) 0.039(2) Uani 1 1 d . . . C41 C 0.1939(8) 0.5555(7) 0.1426(5) 0.037(2) Uani 1 1 d . . . C50 C 0.525(2) 0.9626(19) 0.4247(17) 0.235(7) Uiso 1 1 d DU . . H50A H 0.4632 0.9477 0.4641 0.282 Uiso 1 1 calc R . . H50B H 0.5167 1.0297 0.3929 0.282 Uiso 1 1 calc R . . H50C H 0.5860 0.9525 0.4568 0.282 Uiso 1 1 calc R . . C51 C 0.537(2) 0.8961(18) 0.3624(17) 0.209(6) Uiso 1 1 d DU . . H51A H 0.6043 0.8618 0.3777 0.251 Uiso 1 1 calc R . . H51B H 0.5537 0.9440 0.3091 0.251 Uiso 1 1 calc R . . C52 C 0.494(2) 0.8207(17) 0.3248(17) 0.202(5) Uiso 1 1 d DU . . H52A H 0.4670 0.8646 0.2733 0.242 Uiso 1 1 calc R . . H52B H 0.5602 0.7919 0.3036 0.242 Uiso 1 1 calc R . . C53 C 0.4269(19) 0.7365(16) 0.3308(16) 0.193(5) Uiso 1 1 d DU . . H53A H 0.4320 0.6964 0.3891 0.231 Uiso 1 1 calc R . . H53B H 0.3548 0.7656 0.3286 0.231 Uiso 1 1 calc R . . C54 C 0.4356(19) 0.6648(16) 0.2735(16) 0.185(5) Uiso 1 1 d DU . . H54A H 0.3653 0.6419 0.2821 0.222 Uiso 1 1 calc R . . H54B H 0.4389 0.7078 0.2159 0.222 Uiso 1 1 calc R . . C55 C 0.5036(19) 0.5752(16) 0.2597(15) 0.184(5) Uiso 1 1 d DU . . H55A H 0.4805 0.5242 0.3089 0.220 Uiso 1 1 calc R . . H55B H 0.5730 0.5882 0.2720 0.220 Uiso 1 1 calc R . . C56 C 0.5284(19) 0.5211(17) 0.1884(15) 0.191(7) Uiso 1 1 d DU . . H56A H 0.5871 0.4735 0.2022 0.229 Uiso 1 1 calc R . . H56B H 0.5459 0.5669 0.1347 0.229 Uiso 1 1 calc R . . H56C H 0.4679 0.4885 0.1827 0.229 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 Nd1 0.0221(3) 0.0227(2) 0.0086(2) 0.00051(16) -0.00396(16) -0.00096(18) Ru1 0.0208(4) 0.0214(3) 0.0062(3) 0.0007(2) -0.0033(2) -0.0002(3) Cl1 0.0296(11) 0.0276(11) 0.0142(9) -0.0031(8) -0.0082(8) -0.0017(9) Cl2 0.0327(11) 0.0231(10) 0.0089(8) 0.0024(7) -0.0064(8) -0.0011(9) O1 0.021(3) 0.034(3) 0.015(3) -0.003(2) -0.004(2) -0.001(3) O2 0.021(3) 0.038(4) 0.015(3) -0.009(2) -0.002(2) 0.000(3) O3 0.026(3) 0.033(3) 0.009(3) -0.001(2) -0.007(2) -0.002(3) O4 0.020(3) 0.026(3) 0.017(3) 0.001(2) -0.002(2) 0.001(3) O5 0.035(3) 0.021(3) 0.009(3) 0.002(2) -0.005(2) 0.001(3) O6 0.030(3) 0.034(3) 0.011(3) 0.005(2) -0.005(2) -0.008(3) O7 0.040(4) 0.024(3) 0.011(3) 0.000(2) -0.011(2) -0.002(3) N1 0.019(4) 0.023(4) 0.014(3) 0.002(3) -0.005(3) -0.007(3) N2 0.024(4) 0.020(3) 0.009(3) 0.002(3) 0.001(3) 0.003(3) N3 0.027(4) 0.017(3) 0.008(3) 0.000(3) -0.003(3) -0.001(3) N4 0.023(4) 0.021(4) 0.018(3) 0.001(3) -0.011(3) 0.000(3) N5 0.024(4) 0.021(4) 0.015(3) 0.001(3) -0.006(3) -0.002(3) N6 0.019(3) 0.018(3) 0.012(3) -0.001(3) -0.003(3) 0.000(3) F1 0.031(3) 0.089(5) 0.064(4) -0.045(4) -0.001(3) -0.012(3) F2 0.070(5) 0.102(6) 0.029(3) -0.015(3) -0.028(3) -0.004(4) F3 0.055(4) 0.062(4) 0.087(5) -0.051(4) -0.032(4) 0.012(3) F4 0.027(4) 0.207(10) 0.127(7) -0.136(7) 0.006(4) -0.003(5) F5 0.056(5) 0.190(9) 0.050(4) -0.067(5) 0.022(4) -0.037(5) F6 0.044(4) 0.128(7) 0.145(8) -0.107(7) 0.002(5) 0.012(4) F7 0.055(4) 0.054(4) 0.036(3) 0.007(3) 0.004(3) 0.006(3) F8 0.048(4) 0.035(3) 0.079(5) -0.001(3) -0.043(3) 0.002(3) F9 0.043(3) 0.035(3) 0.044(3) -0.015(3) -0.005(3) -0.003(3) F10 0.029(4) 0.045(4) 0.221(11) -0.015(5) -0.014(5) 0.005(3) F11 0.078(6) 0.086(6) 0.121(7) -0.006(5) 0.058(5) -0.021(5) F12 0.059(4) 0.057(4) 0.082(5) -0.012(4) -0.030(4) -0.011(3) F13 0.051(4) 0.110(6) 0.052(4) -0.028(4) -0.010(3) -0.016(4) F14 0.057(4) 0.091(5) 0.047(4) -0.046(4) -0.017(3) 0.008(4) F15 0.119(7) 0.059(5) 0.079(5) 0.010(4) -0.067(5) 0.001(4) F16 0.073(5) 0.110(6) 0.035(4) -0.037(4) 0.021(3) -0.031(4) F17 0.081(5) 0.051(4) 0.069(5) 0.031(3) -0.032(4) -0.027(4) F18 0.059(4) 0.060(4) 0.025(3) -0.006(3) -0.010(3) -0.023(3) C1 0.033(5) 0.031(5) 0.011(4) 0.000(3) -0.012(3) -0.008(4) C2 0.016(4) 0.044(5) 0.017(4) -0.003(4) -0.006(3) -0.006(4) C3 0.021(4) 0.034(5) 0.007(3) 0.001(3) 0.001(3) -0.003(4) C4 0.028(5) 0.021(4) 0.010(4) -0.002(3) -0.001(3) 0.001(4) C5 0.023(4) 0.025(4) 0.006(3) 0.001(3) -0.002(3) 0.004(3) C6 0.031(5) 0.032(5) 0.010(4) -0.002(3) 0.004(3) 0.001(4) C7 0.037(6) 0.054(6) 0.020(5) -0.004(4) 0.006(4) 0.006(5) C8 0.027(5) 0.065(7) 0.018(4) -0.010(4) 0.006(4) -0.005(5) C9 0.031(5) 0.056(6) 0.010(4) -0.010(4) 0.002(3) 0.004(4) C10 0.023(4) 0.020(4) 0.013(4) -0.004(3) 0.000(3) 0.006(3) C11 0.031(5) 0.024(4) 0.007(4) 0.004(3) -0.003(3) -0.004(4) C12 0.022(4) 0.021(4) 0.017(4) 0.004(3) -0.012(3) -0.001(3) C13 0.018(4) 0.031(5) 0.010(4) 0.002(3) -0.004(3) -0.002(4) C14 0.022(4) 0.022(4) 0.010(4) 0.000(3) 0.001(3) 0.000(3) C15 0.027(5) 0.039(5) 0.016(4) -0.005(4) -0.005(3) -0.010(4) C16 0.040(6) 0.044(6) 0.056(7) -0.014(5) -0.021(5) -0.002(5) C17 0.046(6) 0.044(6) 0.034(5) -0.008(5) -0.023(5) 0.004(5) C18 0.050(7) 0.073(8) 0.033(6) -0.007(5) -0.004(5) -0.037(6) C19 0.030(5) 0.026(4) 0.007(3) -0.002(3) -0.002(3) 0.001(4) C20 0.032(5) 0.019(4) 0.016(4) -0.005(3) -0.001(3) 0.000(4) C21 0.028(5) 0.021(4) 0.011(4) 0.003(3) -0.008(3) 0.001(4) C22 0.019(4) 0.026(4) 0.010(4) 0.002(3) -0.006(3) -0.009(3) C23 0.026(4) 0.026(4) 0.007(3) 0.000(3) -0.006(3) -0.001(4) C24 0.034(5) 0.024(4) 0.011(4) -0.002(3) -0.008(3) -0.001(4) C25 0.030(5) 0.021(4) 0.014(4) -0.006(3) -0.003(3) 0.007(4) C26 0.026(4) 0.025(4) 0.009(4) -0.007(3) 0.000(3) -0.003(4) C27 0.030(6) 0.056(7) 0.040(6) -0.015(5) -0.012(4) -0.001(5) C28 0.019(4) 0.033(5) 0.019(4) -0.004(4) -0.004(3) -0.006(4) C29 0.018(5) 0.050(6) 0.035(5) -0.015(5) -0.005(4) -0.001(4) C30 0.034(5) 0.042(6) 0.023(5) -0.012(4) 0.001(4) -0.004(4) C31 0.022(6) 0.105(11) 0.067(8) -0.058(8) 0.000(5) -0.012(6) C32 0.040(6) 0.038(5) 0.014(4) 0.000(4) -0.001(4) 0.008(4) C33 0.056(7) 0.044(6) 0.021(5) -0.009(4) -0.013(4) -0.006(5) C34 0.033(5) 0.046(6) 0.032(5) -0.008(5) -0.003(4) 0.001(5) C35 0.036(6) 0.049(6) 0.022(5) 0.000(4) 0.007(4) -0.008(5) C36 0.035(6) 0.032(6) 0.074(8) -0.012(6) 0.009(6) 0.003(5) C37 0.045(6) 0.034(5) 0.013(4) 0.003(4) -0.013(4) -0.001(4) C38 0.058(7) 0.039(6) 0.021(5) -0.005(4) -0.006(4) 0.006(5) C39 0.051(6) 0.031(5) 0.022(5) 0.002(4) -0.006(4) 0.002(5) C40 0.033(6) 0.052(6) 0.023(5) 0.006(4) -0.001(4) -0.007(5) C41 0.061(7) 0.038(6) 0.012(4) 0.000(4) -0.003(4) -0.010(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 Nd1 O2 2.422(5) . ? Nd1 O7 2.433(5) . ? Nd1 O5 2.435(5) . ? Nd1 O3 2.436(6) . ? Nd1 O6 2.469(5) . ? Nd1 O1 2.474(5) . ? Nd1 O4 2.476(5) . ? Nd1 N6 2.701(6) . ? Nd1 N5 2.725(6) . ? Ru1 N3 1.997(6) . ? Ru1 N2 2.033(7) . ? Ru1 N1 2.046(6) . ? Ru1 N4 2.060(7) . ? Ru1 Cl2 2.414(2) . ? Ru1 Cl1 2.420(2) . ? O1 C28 1.259(9) . ? O2 C30 1.251(10) . ? O3 C33 1.255(11) . ? O4 C35 1.218(11) . ? O5 C38 1.245(10) . ? O6 C40 1.251(10) . ? O7 H1W 0.8500 . ? O7 H2W 0.8500 . ? N1 C1 1.326(10) . ? N1 C5 1.373(9) . ? N2 C14 1.343(10) . ? N2 C10 1.347(9) . ? N3 C19 1.338(10) . ? N3 C22 1.370(9) . ? N4 C23 1.351(9) . ? N4 C24 1.353(10) . ? N5 C22 1.330(9) . ? N5 C21 1.341(10) . ? N6 C23 1.323(9) . ? N6 C26 1.325(10) . ? F1 C27 1.321(11) . ? F2 C27 1.329(11) . ? F3 C27 1.328(11) . ? F4 C31 1.305(11) . ? F5 C31 1.350(15) . ? F6 C31 1.308(14) . ? F7 C32 1.370(10) . ? F8 C32 1.317(10) . ? F9 C32 1.333(10) . ? F10 C36 1.333(12) . ? F11 C36 1.266(13) . ? F12 C36 1.385(12) . ? F13 C37 1.312(11) . ? F14 C37 1.327(10) . ? F15 C37 1.283(10) . ? F16 C41 1.292(11) . ? F17 C41 1.342(11) . ? F18 C41 1.324(11) . ? C1 C2 1.365(11) . ? C1 H1 0.9500 . ? C2 C3 1.427(11) . ? C2 H2 0.9500 . ? C3 C4 1.381(11) . ? C3 C6 1.540(10) . ? C4 C5 1.381(10) . ? C4 H4 0.9500 . ? C5 C10 1.491(11) . ? C6 C7 1.516(12) . ? C6 C8 1.519(12) . ? C6 C9 1.526(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.385(11) . ? C11 C12 1.394(11) . ? C11 H11 0.9500 . ? C12 C13 1.402(10) . ? C12 C15 1.531(11) . ? C13 C14 1.377(11) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C18 1.507(12) . ? C15 C16 1.521(13) . ? C15 C17 1.558(12) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.384(11) . ? C19 H19 0.9500 . ? C20 C21 1.385(10) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.461(11) . ? C24 C25 1.368(10) . ? C24 H24 0.9500 . ? C25 C26 1.406(11) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.538(12) . ? C28 C29 1.362(12) . ? C29 C30 1.398(12) . ? C29 H29 0.9500 . ? C30 C31 1.522(13) . ? C32 C33 1.496(13) . ? C33 C34 1.386(13) . ? C34 C35 1.450(13) . ? C34 H34 0.9500 . ? C35 C36 1.501(14) . ? C37 C38 1.520(13) . ? C38 C39 1.409(13) . ? C39 C40 1.387(13) . ? C39 H39 0.9500 . ? C40 C41 1.539(13) . ? C50 C51 1.541(2) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.541(2) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.541(2) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.539(2) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.539(2) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.540(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? 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 O2 Nd1 O7 72.96(19) . . ? O2 Nd1 O5 99.23(18) . . ? O7 Nd1 O5 67.81(17) . . ? O2 Nd1 O3 139.01(19) . . ? O7 Nd1 O3 135.95(18) . . ? O5 Nd1 O3 76.01(17) . . ? O2 Nd1 O6 70.06(19) . . ? O7 Nd1 O6 117.05(18) . . ? O5 Nd1 O6 70.15(18) . . ? O3 Nd1 O6 70.14(18) . . ? O2 Nd1 O1 70.83(18) . . ? O7 Nd1 O1 135.17(18) . . ? O5 Nd1 O1 143.47(18) . . ? O3 Nd1 O1 88.86(18) . . ? O6 Nd1 O1 73.47(18) . . ? O2 Nd1 O4 146.61(19) . . ? O7 Nd1 O4 73.71(18) . . ? O5 Nd1 O4 69.66(18) . . ? O3 Nd1 O4 70.69(18) . . ? O6 Nd1 O4 128.97(18) . . ? O1 Nd1 O4 136.23(18) . . ? O2 Nd1 N6 74.87(18) . . ? O7 Nd1 N6 69.77(18) . . ? O5 Nd1 N6 136.94(18) . . ? O3 Nd1 N6 135.41(17) . . ? O6 Nd1 N6 139.23(19) . . ? O1 Nd1 N6 75.93(18) . . ? O4 Nd1 N6 91.80(18) . . ? O2 Nd1 N5 127.59(18) . . ? O7 Nd1 N5 113.60(18) . . ? O5 Nd1 N5 132.30(19) . . ? O3 Nd1 N5 73.82(18) . . ? O6 Nd1 N5 129.35(19) . . ? O1 Nd1 N5 71.41(18) . . ? O4 Nd1 N5 65.92(18) . . ? N6 Nd1 N5 61.63(19) . . ? N3 Ru1 N2 94.8(2) . . ? N3 Ru1 N1 96.4(2) . . ? N2 Ru1 N1 78.9(2) . . ? N3 Ru1 N4 79.7(2) . . ? N2 Ru1 N4 100.3(2) . . ? N1 Ru1 N4 175.9(2) . . ? N3 Ru1 Cl2 174.35(18) . . ? N2 Ru1 Cl2 86.24(18) . . ? N1 Ru1 Cl2 89.29(18) . . ? N4 Ru1 Cl2 94.63(18) . . ? N3 Ru1 Cl1 85.62(19) . . ? N2 Ru1 Cl1 173.85(18) . . ? N1 Ru1 Cl1 94.98(18) . . ? N4 Ru1 Cl1 85.83(18) . . ? Cl2 Ru1 Cl1 93.90(7) . . ? C28 O1 Nd1 133.6(5) . . ? C30 O2 Nd1 135.7(5) . . ? C33 O3 Nd1 132.3(6) . . ? C35 O4 Nd1 131.1(6) . . ? C38 O5 Nd1 135.2(6) . . ? C40 O6 Nd1 131.4(6) . . ? Nd1 O7 H1W 113.6 . . ? Nd1 O7 H2W 139.8 . . ? H1W O7 H2W 106.3 . . ? C1 N1 C5 117.5(7) . . ? C1 N1 Ru1 127.1(5) . . ? C5 N1 Ru1 115.4(5) . . ? C14 N2 C10 116.9(7) . . ? C14 N2 Ru1 126.1(5) . . ? C10 N2 Ru1 117.0(5) . . ? C19 N3 C22 116.2(6) . . ? C19 N3 Ru1 128.5(5) . . ? C22 N3 Ru1 115.2(5) . . ? C23 N4 C24 117.0(7) . . ? C23 N4 Ru1 113.8(5) . . ? C24 N4 Ru1 128.5(5) . . ? C22 N5 C21 117.1(7) . . ? C22 N5 Nd1 117.7(5) . . ? C21 N5 Nd1 124.6(5) . . ? C23 N6 C26 117.4(6) . . ? C23 N6 Nd1 119.3(5) . . ? C26 N6 Nd1 123.0(5) . . ? N1 C1 C2 124.4(7) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C1 C2 C3 119.2(7) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 116.1(7) . . ? C4 C3 C6 124.7(7) . . ? C2 C3 C6 119.1(7) . . ? C5 C4 C3 121.5(7) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? N1 C5 C4 121.2(7) . . ? N1 C5 C10 113.6(6) . . ? C4 C5 C10 125.0(7) . . ? C7 C6 C8 110.6(8) . . ? C7 C6 C9 109.6(7) . . ? C8 C6 C9 106.7(7) . . ? C7 C6 C3 107.1(6) . . ? C8 C6 C3 111.6(7) . . ? C9 C6 C3 111.4(7) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 122.6(7) . . ? N2 C10 C5 114.0(7) . . ? C11 C10 C5 123.3(7) . . ? C10 C11 C12 120.9(7) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C13 115.9(7) . . ? C11 C12 C15 122.0(7) . . ? C13 C12 C15 122.2(7) . . ? C14 C13 C12 120.1(7) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? N2 C14 C13 123.7(7) . . ? N2 C14 H14 118.2 . . ? C13 C14 H14 118.2 . . ? C18 C15 C16 110.4(8) . . ? C18 C15 C12 112.3(7) . . ? C16 C15 C12 109.7(7) . . ? C18 C15 C17 108.9(8) . . ? C16 C15 C17 108.0(7) . . ? C12 C15 C17 107.4(7) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 122.6(7) . . ? N3 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C19 C20 C21 116.6(7) . . ? C19 C20 H20 121.7 . . ? C21 C20 H20 121.7 . . ? N5 C21 C20 122.4(7) . . ? N5 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? N5 C22 N3 125.1(7) . . ? N5 C22 C23 120.0(7) . . ? N3 C22 C23 114.9(6) . . ? N6 C23 N4 125.7(7) . . ? N6 C23 C22 119.6(7) . . ? N4 C23 C22 114.7(6) . . ? N4 C24 C25 120.4(7) . . ? N4 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 118.4(7) . . ? C24 C25 H25 120.8 . . ? C26 C25 H25 120.8 . . ? N6 C26 C25 121.0(7) . . ? N6 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? F1 C27 F3 108.3(9) . . ? F1 C27 F2 106.9(8) . . ? F3 C27 F2 107.1(8) . . ? F1 C27 C28 112.7(8) . . ? F3 C27 C28 112.1(8) . . ? F2 C27 C28 109.6(8) . . ? O1 C28 C29 127.8(8) . . ? O1 C28 C27 114.1(7) . . ? C29 C28 C27 118.0(8) . . ? C28 C29 C30 124.2(8) . . ? C28 C29 H29 117.9 . . ? C30 C29 H29 117.9 . . ? O2 C30 C29 126.1(8) . . ? O2 C30 C31 113.8(8) . . ? C29 C30 C31 120.1(9) . . ? F4 C31 F6 109.7(11) . . ? F4 C31 F5 105.7(10) . . ? F6 C31 F5 106.5(9) . . ? F4 C31 C30 114.1(9) . . ? F6 C31 C30 111.9(10) . . ? F5 C31 C30 108.5(10) . . ? F8 C32 F9 107.7(7) . . ? F8 C32 F7 105.2(7) . . ? F9 C32 F7 103.1(8) . . ? F8 C32 C33 116.3(8) . . ? F9 C32 C33 113.1(7) . . ? F7 C32 C33 110.5(8) . . ? O3 C33 C34 127.3(9) . . ? O3 C33 C32 116.2(9) . . ? C34 C33 C32 116.3(9) . . ? C33 C34 C35 121.3(9) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? O4 C35 C34 128.6(9) . . ? O4 C35 C36 115.1(9) . . ? C34 C35 C36 115.9(9) . . ? F11 C36 F10 110.0(10) . . ? F11 C36 F12 102.6(9) . . ? F10 C36 F12 104.1(10) . . ? F11 C36 C35 115.4(11) . . ? F10 C36 C35 115.2(9) . . ? F12 C36 C35 108.1(8) . . ? F15 C37 F13 105.9(9) . . ? F15 C37 F14 108.8(8) . . ? F13 C37 F14 104.6(8) . . ? F15 C37 C38 113.8(8) . . ? F13 C37 C38 111.6(7) . . ? F14 C37 C38 111.6(8) . . ? O5 C38 C39 125.6(9) . . ? O5 C38 C37 115.5(9) . . ? C39 C38 C37 118.8(8) . . ? C40 C39 C38 122.0(9) . . ? C40 C39 H39 119.0 . . ? C38 C39 H39 119.0 . . ? O6 C40 C39 129.5(9) . . ? O6 C40 C41 113.6(8) . . ? C39 C40 C41 116.5(8) . . ? F16 C41 F18 107.5(9) . . ? F16 C41 F17 107.5(8) . . ? F18 C41 F17 105.0(8) . . ? F16 C41 C40 110.8(8) . . ? F18 C41 C40 113.9(7) . . ? F17 C41 C40 111.7(9) . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C50 C51 C52 150(3) . . ? C50 C51 H51A 99.1 . . ? C52 C51 H51A 99.1 . . ? C50 C51 H51B 99.1 . . ? C52 C51 H51B 99.1 . . ? H51A C51 H51B 104.0 . . ? C53 C52 C51 153(2) . . ? C53 C52 H52A 98.4 . . ? C51 C52 H52A 98.4 . . ? C53 C52 H52B 98.4 . . ? C51 C52 H52B 98.4 . . ? H52A C52 H52B 103.8 . . ? C54 C53 C52 128(2) . . ? C54 C53 H53A 105.2 . . ? C52 C53 H53A 105.2 . . ? C54 C53 H53B 105.2 . . ? C52 C53 H53B 105.2 . . ? H53A C53 H53B 105.9 . . ? C55 C54 C53 139(2) . . ? C55 C54 H54A 102.3 . . ? C53 C54 H54A 102.3 . . ? C55 C54 H54B 102.3 . . ? C53 C54 H54B 102.3 . . ? H54A C54 H54B 104.8 . . ? C54 C55 C56 137(2) . . ? C54 C55 H55A 102.9 . . ? C56 C55 H55A 102.9 . . ? C54 C55 H55B 102.9 . . ? C56 C55 H55B 102.9 . . ? H55A C55 H55B 105.1 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? 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 O2 Nd1 O1 C28 8.1(7) . . . . ? O7 Nd1 O1 C28 46.0(8) . . . . ? O5 Nd1 O1 C28 -71.3(8) . . . . ? O3 Nd1 O1 C28 -135.6(7) . . . . ? O6 Nd1 O1 C28 -66.0(7) . . . . ? O4 Nd1 O1 C28 164.3(6) . . . . ? N6 Nd1 O1 C28 86.7(7) . . . . ? N5 Nd1 O1 C28 151.1(7) . . . . ? O7 Nd1 O2 C30 -168.4(8) . . . . ? O5 Nd1 O2 C30 128.4(8) . . . . ? O3 Nd1 O2 C30 49.1(9) . . . . ? O6 Nd1 O2 C30 63.5(8) . . . . ? O1 Nd1 O2 C30 -15.3(8) . . . . ? O4 Nd1 O2 C30 -164.8(7) . . . . ? N6 Nd1 O2 C30 -95.3(8) . . . . ? N5 Nd1 O2 C30 -61.4(8) . . . . ? O2 Nd1 O3 C33 130.7(7) . . . . ? O7 Nd1 O3 C33 7.5(8) . . . . ? O5 Nd1 O3 C33 42.6(7) . . . . ? O6 Nd1 O3 C33 116.3(7) . . . . ? O1 Nd1 O3 C33 -170.9(7) . . . . ? O4 Nd1 O3 C33 -30.4(7) . . . . ? N6 Nd1 O3 C33 -102.4(7) . . . . ? N5 Nd1 O3 C33 -100.0(7) . . . . ? O2 Nd1 O4 C35 -130.5(8) . . . . ? O7 Nd1 O4 C35 -126.9(8) . . . . ? O5 Nd1 O4 C35 -55.1(8) . . . . ? O3 Nd1 O4 C35 26.7(8) . . . . ? O6 Nd1 O4 C35 -15.0(9) . . . . ? O1 Nd1 O4 C35 93.3(8) . . . . ? N6 Nd1 O4 C35 164.8(8) . . . . ? N5 Nd1 O4 C35 107.1(8) . . . . ? O2 Nd1 O5 C38 -90.7(8) . . . . ? O7 Nd1 O5 C38 -157.9(9) . . . . ? O3 Nd1 O5 C38 47.7(8) . . . . ? O6 Nd1 O5 C38 -25.9(8) . . . . ? O1 Nd1 O5 C38 -20.5(10) . . . . ? O4 Nd1 O5 C38 122.0(9) . . . . ? N6 Nd1 O5 C38 -168.4(8) . . . . ? N5 Nd1 O5 C38 99.7(8) . . . . ? O2 Nd1 O6 C40 130.6(8) . . . . ? O7 Nd1 O6 C40 73.0(8) . . . . ? O5 Nd1 O6 C40 22.4(8) . . . . ? O3 Nd1 O6 C40 -59.4(8) . . . . ? O1 Nd1 O6 C40 -154.3(8) . . . . ? O4 Nd1 O6 C40 -17.5(9) . . . . ? N6 Nd1 O6 C40 162.8(8) . . . . ? N5 Nd1 O6 C40 -106.6(8) . . . . ? N3 Ru1 N1 C1 79.3(7) . . . . ? N2 Ru1 N1 C1 173.0(7) . . . . ? N4 Ru1 N1 C1 94(3) . . . . ? Cl2 Ru1 N1 C1 -100.7(6) . . . . ? Cl1 Ru1 N1 C1 -6.8(7) . . . . ? N3 Ru1 N1 C5 -103.7(5) . . . . ? N2 Ru1 N1 C5 -10.0(5) . . . . ? N4 Ru1 N1 C5 -89(3) . . . . ? Cl2 Ru1 N1 C5 76.3(5) . . . . ? Cl1 Ru1 N1 C5 170.1(5) . . . . ? N3 Ru1 N2 C14 -77.2(6) . . . . ? N1 Ru1 N2 C14 -172.8(7) . . . . ? N4 Ru1 N2 C14 3.2(7) . . . . ? Cl2 Ru1 N2 C14 97.2(6) . . . . ? Cl1 Ru1 N2 C14 -171.2(13) . . . . ? N3 Ru1 N2 C10 102.8(5) . . . . ? N1 Ru1 N2 C10 7.2(5) . . . . ? N4 Ru1 N2 C10 -176.8(5) . . . . ? Cl2 Ru1 N2 C10 -82.8(5) . . . . ? Cl1 Ru1 N2 C10 9(2) . . . . ? N2 Ru1 N3 C19 -73.4(7) . . . . ? N1 Ru1 N3 C19 5.9(7) . . . . ? N4 Ru1 N3 C19 -173.0(7) . . . . ? Cl2 Ru1 N3 C19 -174.2(15) . . . . ? Cl1 Ru1 N3 C19 100.5(7) . . . . ? N2 Ru1 N3 C22 110.7(5) . . . . ? N1 Ru1 N3 C22 -170.0(5) . . . . ? N4 Ru1 N3 C22 11.1(5) . . . . ? Cl2 Ru1 N3 C22 10(2) . . . . ? Cl1 Ru1 N3 C22 -75.5(5) . . . . ? N3 Ru1 N4 C23 -11.5(5) . . . . ? N2 Ru1 N4 C23 -104.6(6) . . . . ? N1 Ru1 N4 C23 -27(4) . . . . ? Cl2 Ru1 N4 C23 168.4(5) . . . . ? Cl1 Ru1 N4 C23 74.8(5) . . . . ? N3 Ru1 N4 C24 178.0(7) . . . . ? N2 Ru1 N4 C24 84.9(7) . . . . ? N1 Ru1 N4 C24 163(3) . . . . ? Cl2 Ru1 N4 C24 -2.1(7) . . . . ? Cl1 Ru1 N4 C24 -95.7(7) . . . . ? O2 Nd1 N5 C22 -49.2(6) . . . . ? O7 Nd1 N5 C22 36.9(6) . . . . ? O5 Nd1 N5 C22 117.8(5) . . . . ? O3 Nd1 N5 C22 170.6(6) . . . . ? O6 Nd1 N5 C22 -143.5(5) . . . . ? O1 Nd1 N5 C22 -95.1(6) . . . . ? O4 Nd1 N5 C22 94.9(6) . . . . ? N6 Nd1 N5 C22 -11.4(5) . . . . ? O2 Nd1 N5 C21 139.9(6) . . . . ? O7 Nd1 N5 C21 -134.0(6) . . . . ? O5 Nd1 N5 C21 -53.2(7) . . . . ? O3 Nd1 N5 C21 -0.4(6) . . . . ? O6 Nd1 N5 C21 45.6(7) . . . . ? O1 Nd1 N5 C21 94.0(6) . . . . ? O4 Nd1 N5 C21 -76.0(6) . . . . ? N6 Nd1 N5 C21 177.7(7) . . . . ? O2 Nd1 N6 C23 159.8(6) . . . . ? O7 Nd1 N6 C23 -123.2(6) . . . . ? O5 Nd1 N6 C23 -112.8(6) . . . . ? O3 Nd1 N6 C23 12.7(7) . . . . ? O6 Nd1 N6 C23 128.5(5) . . . . ? O1 Nd1 N6 C23 86.2(6) . . . . ? O4 Nd1 N6 C23 -51.3(6) . . . . ? N5 Nd1 N6 C23 10.0(5) . . . . ? O2 Nd1 N6 C26 -26.8(6) . . . . ? O7 Nd1 N6 C26 50.3(6) . . . . ? O5 Nd1 N6 C26 60.6(7) . . . . ? O3 Nd1 N6 C26 -173.9(5) . . . . ? O6 Nd1 N6 C26 -58.1(7) . . . . ? O1 Nd1 N6 C26 -100.3(6) . . . . ? O4 Nd1 N6 C26 122.2(6) . . . . ? N5 Nd1 N6 C26 -176.6(6) . . . . ? C5 N1 C1 C2 -0.2(12) . . . . ? Ru1 N1 C1 C2 176.7(6) . . . . ? N1 C1 C2 C3 -3.7(13) . . . . ? C1 C2 C3 C4 3.8(12) . . . . ? C1 C2 C3 C6 -180.0(8) . . . . ? C2 C3 C4 C5 -0.2(12) . . . . ? C6 C3 C4 C5 -176.2(7) . . . . ? C1 N1 C5 C4 4.0(11) . . . . ? Ru1 N1 C5 C4 -173.3(6) . . . . ? C1 N1 C5 C10 -171.7(7) . . . . ? Ru1 N1 C5 C10 11.1(8) . . . . ? C3 C4 C5 N1 -3.7(12) . . . . ? C3 C4 C5 C10 171.4(7) . . . . ? C4 C3 C6 C7 102.9(9) . . . . ? C2 C3 C6 C7 -73.0(10) . . . . ? C4 C3 C6 C8 -136.0(9) . . . . ? C2 C3 C6 C8 48.1(10) . . . . ? C4 C3 C6 C9 -16.9(11) . . . . ? C2 C3 C6 C9 167.2(8) . . . . ? C14 N2 C10 C11 0.1(11) . . . . ? Ru1 N2 C10 C11 -179.9(6) . . . . ? C14 N2 C10 C5 176.6(7) . . . . ? Ru1 N2 C10 C5 -3.4(8) . . . . ? N1 C5 C10 N2 -5.0(10) . . . . ? C4 C5 C10 N2 179.5(7) . . . . ? N1 C5 C10 C11 171.4(7) . . . . ? C4 C5 C10 C11 -4.0(12) . . . . ? N2 C10 C11 C12 1.8(12) . . . . ? C5 C10 C11 C12 -174.4(7) . . . . ? C10 C11 C12 C13 -2.2(11) . . . . ? C10 C11 C12 C15 177.4(7) . . . . ? C11 C12 C13 C14 0.8(11) . . . . ? C15 C12 C13 C14 -178.7(7) . . . . ? C10 N2 C14 C13 -1.5(11) . . . . ? Ru1 N2 C14 C13 178.5(6) . . . . ? C12 C13 C14 N2 1.0(12) . . . . ? C11 C12 C15 C18 -161.8(8) . . . . ? C13 C12 C15 C18 17.7(12) . . . . ? C11 C12 C15 C16 -38.6(11) . . . . ? C13 C12 C15 C16 140.9(8) . . . . ? C11 C12 C15 C17 78.5(10) . . . . ? C13 C12 C15 C17 -102.0(9) . . . . ? C22 N3 C19 C20 1.0(12) . . . . ? Ru1 N3 C19 C20 -174.9(6) . . . . ? N3 C19 C20 C21 1.2(12) . . . . ? C22 N5 C21 C20 1.7(12) . . . . ? Nd1 N5 C21 C20 172.7(6) . . . . ? C19 C20 C21 N5 -2.6(12) . . . . ? C21 N5 C22 N3 0.8(11) . . . . ? Nd1 N5 C22 N3 -170.9(6) . . . . ? C21 N5 C22 C23 -175.6(7) . . . . ? Nd1 N5 C22 C23 12.7(9) . . . . ? C19 N3 C22 N5 -2.1(11) . . . . ? Ru1 N3 C22 N5 174.4(6) . . . . ? C19 N3 C22 C23 174.5(7) . . . . ? Ru1 N3 C22 C23 -9.0(8) . . . . ? C26 N6 C23 N4 -1.1(12) . . . . ? Nd1 N6 C23 N4 172.7(6) . . . . ? C26 N6 C23 C22 177.8(7) . . . . ? Nd1 N6 C23 C22 -8.4(9) . . . . ? C24 N4 C23 N6 0.5(12) . . . . ? Ru1 N4 C23 N6 -171.1(6) . . . . ? C24 N4 C23 C22 -178.4(7) . . . . ? Ru1 N4 C23 C22 10.0(9) . . . . ? N5 C22 C23 N6 -3.1(11) . . . . ? N3 C22 C23 N6 -179.9(7) . . . . ? N5 C22 C23 N4 175.9(7) . . . . ? N3 C22 C23 N4 -0.9(10) . . . . ? C23 N4 C24 C25 0.8(11) . . . . ? Ru1 N4 C24 C25 171.0(6) . . . . ? N4 C24 C25 C26 -1.5(12) . . . . ? C23 N6 C26 C25 0.3(11) . . . . ? Nd1 N6 C26 C25 -173.2(6) . . . . ? C24 C25 C26 N6 0.9(12) . . . . ? Nd1 O1 C28 C29 -2.4(14) . . . . ? Nd1 O1 C28 C27 179.5(5) . . . . ? F1 C27 C28 O1 -162.8(8) . . . . ? F3 C27 C28 O1 -40.3(11) . . . . ? F2 C27 C28 O1 78.4(10) . . . . ? F1 C27 C28 C29 18.9(13) . . . . ? F3 C27 C28 C29 141.3(9) . . . . ? F2 C27 C28 C29 -100.0(10) . . . . ? O1 C28 C29 C30 -3.8(16) . . . . ? C27 C28 C29 C30 174.3(9) . . . . ? Nd1 O2 C30 C29 16.5(15) . . . . ? Nd1 O2 C30 C31 -161.9(7) . . . . ? C28 C29 C30 O2 -3.0(16) . . . . ? C28 C29 C30 C31 175.3(10) . . . . ? O2 C30 C31 F4 -170.1(11) . . . . ? C29 C30 C31 F4 11.3(17) . . . . ? O2 C30 C31 F6 -44.9(14) . . . . ? C29 C30 C31 F6 136.6(10) . . . . ? O2 C30 C31 F5 72.4(12) . . . . ? C29 C30 C31 F5 -106.2(10) . . . . ? Nd1 O3 C33 C34 26.6(14) . . . . ? Nd1 O3 C33 C32 -157.6(5) . . . . ? F8 C32 C33 O3 172.7(7) . . . . ? F9 C32 C33 O3 -62.0(11) . . . . ? F7 C32 C33 O3 52.9(10) . . . . ? F8 C32 C33 C34 -11.0(12) . . . . ? F9 C32 C33 C34 114.3(9) . . . . ? F7 C32 C33 C34 -130.8(9) . . . . ? O3 C33 C34 C35 -1.4(15) . . . . ? C32 C33 C34 C35 -177.2(8) . . . . ? Nd1 O4 C35 C34 -19.6(14) . . . . ? Nd1 O4 C35 C36 167.0(6) . . . . ? C33 C34 C35 O4 -1.8(15) . . . . ? C33 C34 C35 C36 171.5(9) . . . . ? O4 C35 C36 F11 49.1(13) . . . . ? C34 C35 C36 F11 -125.1(10) . . . . ? O4 C35 C36 F10 179.0(10) . . . . ? C34 C35 C36 F10 4.8(14) . . . . ? O4 C35 C36 F12 -65.0(12) . . . . ? C34 C35 C36 F12 120.8(9) . . . . ? Nd1 O5 C38 C39 22.5(15) . . . . ? Nd1 O5 C38 C37 -160.0(6) . . . . ? F15 C37 C38 O5 159.7(9) . . . . ? F13 C37 C38 O5 40.0(12) . . . . ? F14 C37 C38 O5 -76.7(10) . . . . ? F15 C37 C38 C39 -22.6(13) . . . . ? F13 C37 C38 C39 -142.4(9) . . . . ? F14 C37 C38 C39 100.9(10) . . . . ? O5 C38 C39 C40 -1.4(16) . . . . ? C37 C38 C39 C40 -178.7(9) . . . . ? Nd1 O6 C40 C39 -17.5(16) . . . . ? Nd1 O6 C40 C41 170.6(5) . . . . ? C38 C39 C40 O6 -0.4(17) . . . . ? C38 C39 C40 C41 171.3(9) . . . . ? O6 C40 C41 F16 96.5(10) . . . . ? C39 C40 C41 F16 -76.5(11) . . . . ? O6 C40 C41 F18 -24.8(13) . . . . ? C39 C40 C41 F18 162.1(9) . . . . ? O6 C40 C41 F17 -143.6(8) . . . . ? C39 C40 C41 F17 43.4(12) . . . . ? C50 C51 C52 C53 -29(10) . . . . ? C51 C52 C53 C54 -161(5) . . . . ? C52 C53 C54 C55 77(5) . . . . ? C53 C54 C55 C56 -160(3) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.942 _refine_diff_density_min -1.868 _refine_diff_density_rms 0.201 #===END data_imw286m _database_code_depnum_ccdc_archive 'CCDC 661954' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H39 Cl2 F18 N8 Nd O8 Ru S2' _chemical_formula_weight 1530.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 20.802(11) _cell_length_b 12.338(7) _cell_length_c 24.436(13) _cell_angle_alpha 90.00 _cell_angle_beta 107.040(9) _cell_angle_gamma 90.00 _cell_volume 5996(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1018 _cell_measurement_theta_min 5.261 _cell_measurement_theta_max 52.840 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3020 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6090 _exptl_absorpt_correction_T_max 0.8979 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 65561 _diffrn_reflns_av_R_equivalents 0.0825 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.58 _reflns_number_total 13614 _reflns_number_gt 8913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+27.8313P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13614 _refine_ls_number_parameters 754 _refine_ls_number_restraints 137 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1391 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.005 _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 Nd1 Nd 0.170514(17) 0.25088(3) 0.462198(13) 0.02450(10) Uani 1 1 d . . . Ru1 Ru 0.42057(2) 0.45539(4) 0.644281(19) 0.01923(12) Uani 1 1 d . . . S1 S 0.60176(10) 0.71111(17) 0.66223(8) 0.0417(5) Uani 1 1 d . . . S2 S 0.56006(10) 0.23477(14) 0.56323(8) 0.0370(4) Uani 1 1 d . . . F1 F 0.2173(4) 0.6453(5) 0.5037(3) 0.111(3) Uani 1 1 d . . . F2 F 0.1188(6) 0.7030(6) 0.5025(4) 0.152(4) Uani 1 1 d . . . F3 F 0.1387(4) 0.6543(4) 0.4268(3) 0.091(2) Uani 1 1 d . . . F4 F 0.0283(5) 0.2722(6) 0.5968(5) 0.085(3) Uiso 0.547(11) 1 d PDU A 1 F5 F 0.0112(5) 0.4446(7) 0.5954(4) 0.072(3) Uiso 0.547(11) 1 d PDU A 1 F6 F 0.1068(4) 0.3792(10) 0.6444(4) 0.085(3) Uiso 0.547(11) 1 d PDU A 1 F6' F 0.0964(6) 0.3136(10) 0.6400(4) 0.081(3) Uiso 0.453(11) 1 d PDU A 2 F4' F 0.0021(5) 0.3094(10) 0.5732(5) 0.082(4) Uiso 0.453(11) 1 d PDU A 2 F5' F 0.0380(6) 0.4597(7) 0.6162(5) 0.086(4) Uiso 0.453(11) 1 d PDU A 2 F7 F 0.1504(3) -0.1068(5) 0.5761(2) 0.0692(15) Uani 1 1 d . B . F8 F 0.0453(2) -0.1126(4) 0.53186(19) 0.0526(12) Uani 1 1 d . B . F9 F 0.0863(3) 0.0240(4) 0.5837(2) 0.0741(17) Uani 1 1 d . B . F10 F 0.0365(4) -0.1182(7) 0.3349(4) 0.049(2) Uiso 0.520(15) 1 d PDU B 1 F11 F 0.0778(5) 0.0098(6) 0.2953(3) 0.054(3) Uiso 0.520(15) 1 d PDU B 1 F12 F 0.1416(4) -0.1203(8) 0.3392(4) 0.063(3) Uiso 0.520(15) 1 d PDU B 1 F10' F 0.0581(5) -0.1489(6) 0.3420(4) 0.045(2) Uiso 0.480(15) 1 d PDU B 2 F12' F 0.1442(4) -0.0784(9) 0.3232(5) 0.060(3) Uiso 0.480(15) 1 d PDU B 2 F11' F 0.0498(5) 0.0078(7) 0.3012(4) 0.059(3) Uiso 0.480(15) 1 d PDU B 2 C37 C 0.1522(4) 0.3625(6) 0.2748(4) 0.052(3) Uiso 0.583(7) 1 d PDU C 1 F13 F 0.1125(4) 0.4322(7) 0.2384(4) 0.066(2) Uiso 0.583(7) 1 d PDU C 1 F14 F 0.2125(4) 0.4097(8) 0.2925(4) 0.081(3) Uiso 0.583(7) 1 d PDU C 1 F15 F 0.1595(5) 0.2777(7) 0.2433(5) 0.096(3) Uiso 0.583(7) 1 d PDU C 1 C37' C 0.1504(5) 0.3820(9) 0.2781(4) 0.052(3) Uiso 0.417(7) 1 d PDU C 2 F13' F 0.1097(5) 0.3742(11) 0.2247(5) 0.074(3) Uiso 0.417(7) 1 d PDU C 2 F14' F 0.1586(7) 0.4880(10) 0.2890(6) 0.100(4) Uiso 0.417(7) 1 d PDU C 2 F15' F 0.2101(5) 0.3455(10) 0.2762(5) 0.064(3) Uiso 0.417(7) 1 d PDU C 2 F16 F -0.0807(4) 0.2894(8) 0.2805(3) 0.073(2) Uiso 0.666(16) 1 d PDU C 1 F17 F -0.0803(4) 0.3082(7) 0.3687(3) 0.060(2) Uiso 0.666(16) 1 d PDU C 1 F18 F -0.0582(4) 0.1523(4) 0.3380(4) 0.057(2) Uiso 0.666(16) 1 d PDU C 1 F18' F -0.0681(8) 0.1615(8) 0.3119(7) 0.077(4) Uiso 0.334(16) 1 d PDU C 2 F16' F -0.0794(6) 0.3336(11) 0.2951(6) 0.052(4) Uiso 0.334(16) 1 d PDU C 2 F17' F -0.0739(7) 0.2718(13) 0.3790(4) 0.055(4) Uiso 0.334(16) 1 d PDU C 2 O1 O 0.1509(3) 0.4467(4) 0.4601(2) 0.0436(13) Uani 1 1 d . . . O2 O 0.1079(2) 0.3026(4) 0.5291(2) 0.0393(12) Uani 1 1 d . . . O3 O 0.1508(2) 0.0914(4) 0.51154(18) 0.0352(11) Uani 1 1 d . . . O4 O 0.1454(2) 0.0883(4) 0.39755(19) 0.0369(12) Uani 1 1 d . . . O5 O 0.1709(2) 0.3109(4) 0.36890(18) 0.0319(11) Uani 1 1 d . C . O6 O 0.0554(2) 0.2596(4) 0.40415(19) 0.0403(12) Uani 1 1 d . C . O7 O 0.2751(2) 0.1559(4) 0.45860(18) 0.0331(11) Uani 1 1 d . . . H4W H 0.2736 0.0966 0.4406 0.040 Uiso 1 1 d R . . H3W H 0.3132 0.1839 0.4613 0.040 Uiso 1 1 d R . . N1 N 0.4653(2) 0.4377(4) 0.7301(2) 0.0209(10) Uani 1 1 d . . . N2 N 0.3708(3) 0.5685(4) 0.6776(2) 0.0217(11) Uani 1 1 d . . . N3 N 0.3693(2) 0.4670(4) 0.5582(2) 0.0213(10) Uani 1 1 d . . . N4 N 0.3468(2) 0.3454(4) 0.63829(19) 0.0194(10) Uani 1 1 d . . . N5 N 0.2809(3) 0.3814(4) 0.4863(2) 0.0236(11) Uani 1 1 d . . . N6 N 0.2506(2) 0.2638(4) 0.57168(19) 0.0212(11) Uani 1 1 d . . . N7 N 0.4924(3) 0.5699(4) 0.6453(2) 0.0261(12) Uani 1 1 d . . . N8 N 0.4787(3) 0.3443(4) 0.6182(2) 0.0247(11) Uani 1 1 d . . . C1 C 0.3174(3) 0.6271(5) 0.6477(3) 0.0259(14) Uani 1 1 d . . . H1 H 0.2981 0.6111 0.6082 0.031 Uiso 1 1 calc R . . C2 C 0.2894(3) 0.7083(5) 0.6713(3) 0.0281(14) Uani 1 1 d . . . H2 H 0.2519 0.7473 0.6481 0.034 Uiso 1 1 calc R . . C3 C 0.3158(3) 0.7344(5) 0.7293(3) 0.0263(14) Uani 1 1 d . . . C4 C 0.3699(3) 0.6717(5) 0.7604(2) 0.0220(12) Uani 1 1 d . . . H4 H 0.3891 0.6852 0.8001 0.026 Uiso 1 1 calc R . . C5 C 0.3965(3) 0.5899(5) 0.7346(2) 0.0202(12) Uani 1 1 d . . . C6 C 0.4515(3) 0.5165(5) 0.7644(2) 0.0187(12) Uani 1 1 d . . . C7 C 0.4872(3) 0.5202(5) 0.8220(2) 0.0198(12) Uani 1 1 d . . . H7 H 0.4776 0.5759 0.8453 0.024 Uiso 1 1 calc R . . C8 C 0.5366(3) 0.4442(5) 0.8466(2) 0.0211(12) Uani 1 1 d . . . C9 C 0.5457(3) 0.3622(5) 0.8107(3) 0.0244(13) Uani 1 1 d . . . H9 H 0.5771 0.3059 0.8257 0.029 Uiso 1 1 calc R . . C10 C 0.5103(3) 0.3614(5) 0.7539(2) 0.0243(13) Uani 1 1 d . . . H10 H 0.5179 0.3042 0.7305 0.029 Uiso 1 1 calc R . . C11 C 0.2870(3) 0.8264(5) 0.7561(3) 0.0324(15) Uani 1 1 d . . . C12 C 0.2355(6) 0.8930(9) 0.7106(4) 0.085(4) Uani 1 1 d . . . H12A H 0.2579 0.9270 0.6848 0.127 Uiso 1 1 calc R . . H12B H 0.2163 0.9492 0.7294 0.127 Uiso 1 1 calc R . . H12C H 0.1996 0.8452 0.6886 0.127 Uiso 1 1 calc R . . C13 C 0.2523(6) 0.7757(8) 0.7975(5) 0.086(4) Uani 1 1 d . . . H13A H 0.2157 0.7284 0.7761 0.129 Uiso 1 1 calc R . . H13B H 0.2341 0.8332 0.8162 0.129 Uiso 1 1 calc R . . H13C H 0.2851 0.7331 0.8265 0.129 Uiso 1 1 calc R . . C14 C 0.3420(4) 0.9021(7) 0.7895(4) 0.060(3) Uani 1 1 d . . . H14A H 0.3724 0.8627 0.8215 0.090 Uiso 1 1 calc R . . H14B H 0.3217 0.9630 0.8043 0.090 Uiso 1 1 calc R . . H14C H 0.3672 0.9296 0.7643 0.090 Uiso 1 1 calc R . . C15 C 0.5794(3) 0.4524(5) 0.9084(2) 0.0261(13) Uani 1 1 d . . . C16 C 0.5358(4) 0.4695(7) 0.9475(3) 0.052(2) Uani 1 1 d . . . H16A H 0.5064 0.5321 0.9343 0.078 Uiso 1 1 calc R . . H16B H 0.5645 0.4827 0.9866 0.078 Uiso 1 1 calc R . . H16C H 0.5084 0.4047 0.9470 0.078 Uiso 1 1 calc R . . C17 C 0.6236(5) 0.5533(8) 0.9124(4) 0.069(3) Uani 1 1 d . . . H17A H 0.6574 0.5396 0.8924 0.103 Uiso 1 1 calc R . . H17B H 0.6462 0.5697 0.9527 0.103 Uiso 1 1 calc R . . H17C H 0.5955 0.6149 0.8946 0.103 Uiso 1 1 calc R . . C18 C 0.6228(5) 0.3535(7) 0.9287(3) 0.060(3) Uani 1 1 d . . . H18A H 0.5941 0.2892 0.9250 0.089 Uiso 1 1 calc R . . H18B H 0.6489 0.3630 0.9689 0.089 Uiso 1 1 calc R . . H18C H 0.6535 0.3441 0.9054 0.089 Uiso 1 1 calc R . . C19 C 0.3845(3) 0.5285(5) 0.5176(3) 0.0278(14) Uani 1 1 d . . . H19 H 0.4197 0.5803 0.5285 0.033 Uiso 1 1 calc R . . C20 C 0.3493(4) 0.5164(6) 0.4609(3) 0.0351(16) Uani 1 1 d . . . H20 H 0.3609 0.5572 0.4323 0.042 Uiso 1 1 calc R . . C21 C 0.2962(3) 0.4431(5) 0.4464(3) 0.0322(15) Uani 1 1 d . . . H21 H 0.2703 0.4363 0.4074 0.039 Uiso 1 1 calc R . . C22 C 0.3183(3) 0.3960(5) 0.5400(2) 0.0208(12) Uani 1 1 d . . . C23 C 0.3038(3) 0.3298(5) 0.5847(2) 0.0194(12) Uani 1 1 d . . . C24 C 0.2381(3) 0.2081(5) 0.6146(3) 0.0251(13) Uani 1 1 d . . . H24 H 0.2001 0.1616 0.6067 0.030 Uiso 1 1 calc R . . C25 C 0.2800(3) 0.2174(5) 0.6705(3) 0.0260(14) Uani 1 1 d . . . H25 H 0.2716 0.1769 0.7007 0.031 Uiso 1 1 calc R . . C26 C 0.3338(3) 0.2865(5) 0.6806(2) 0.0228(13) Uani 1 1 d . . . H26 H 0.3629 0.2934 0.7185 0.027 Uiso 1 1 calc R . . C27 C 0.1504(7) 0.6312(8) 0.4806(5) 0.076(3) Uani 1 1 d . . . C28 C 0.1322(4) 0.5136(7) 0.4904(4) 0.052(2) Uani 1 1 d . . . C29 C 0.1013(5) 0.4931(8) 0.5333(4) 0.065(3) Uani 1 1 d . . . H29 H 0.0875 0.5519 0.5524 0.079 Uiso 1 1 calc R . . C30 C 0.0907(4) 0.3868(8) 0.5481(3) 0.048(2) Uani 1 1 d . A . C31 C 0.0567(3) 0.3685(5) 0.5963(3) 0.070(3) Uani 1 1 d D . . C32 C 0.0905(2) -0.0559(4) 0.3406(3) 0.0446(19) Uani 1 1 d D . . C33 C 0.1101(3) 0.0070(5) 0.3975(3) 0.0312(15) Uani 1 1 d . B . C34 C 0.0907(4) -0.0355(5) 0.4433(3) 0.0320(15) Uani 1 1 d . . . H34 H 0.0609 -0.0957 0.4372 0.038 Uiso 1 1 calc R B . C35 C 0.1141(4) 0.0088(6) 0.4970(3) 0.0329(15) Uani 1 1 d . B . C36 C 0.0982(4) -0.0474(6) 0.5476(3) 0.0420(18) Uani 1 1 d . . . C38 C 0.1251(4) 0.3279(6) 0.3233(3) 0.0347(16) Uani 1 1 d . . . C39 C 0.0564(4) 0.3162(7) 0.3119(3) 0.0406(18) Uani 1 1 d . C . H39 H 0.0284 0.3326 0.2746 0.049 Uiso 1 1 calc R . . C40 C 0.0268(4) 0.2816(6) 0.3527(3) 0.0371(17) Uani 1 1 d . . . C41 C -0.0493(4) 0.2595(4) 0.33445(19) 0.058(3) Uani 1 1 d D C . C42 C 0.5124(3) 0.2999(5) 0.5956(2) 0.0234(13) Uani 1 1 d . . . C43 C 0.5378(3) 0.6282(5) 0.6525(2) 0.0264(14) Uani 1 1 d . . . O8 O 0.3986(3) 0.2392(5) 0.4697(2) 0.0495(14) Uani 1 1 d . . . H1W H 0.3953 0.2437 0.4343 0.059 Uiso 1 1 d R . . H2W H 0.4389 0.2321 0.4908 0.059 Uiso 1 1 d R . . C44 C 0.2605(6) 0.0850(8) 0.3143(5) 0.072(3) Uani 1 1 d . . . H44A H 0.2792 0.1591 0.3160 0.087 Uiso 1 1 calc R . . H44B H 0.2188 0.0891 0.3259 0.087 Uiso 1 1 calc R . . Cl1 Cl 0.24071(17) 0.0368(2) 0.24315(13) 0.0873(9) Uani 1 1 d . . . Cl2 Cl 0.31791(15) 0.0028(2) 0.36198(13) 0.0823(8) Uani 1 1 d . . . 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 Nd1 0.02556(18) 0.02840(19) 0.01689(16) 0.00062(14) 0.00209(12) -0.00799(15) Ru1 0.0218(2) 0.0199(2) 0.0147(2) -0.00271(18) 0.00329(18) -0.0038(2) S1 0.0401(11) 0.0497(11) 0.0346(9) -0.0031(8) 0.0099(8) -0.0246(9) S2 0.0454(11) 0.0287(9) 0.0448(10) -0.0076(8) 0.0256(9) -0.0012(8) F1 0.114(6) 0.061(4) 0.128(6) 0.004(4) -0.012(5) -0.031(4) F2 0.273(12) 0.045(4) 0.180(8) 0.003(5) 0.131(9) 0.039(6) F3 0.118(5) 0.049(3) 0.105(5) 0.035(3) 0.031(4) 0.013(3) F7 0.067(3) 0.079(4) 0.051(3) 0.032(3) 0.000(3) -0.010(3) F8 0.061(3) 0.048(3) 0.053(3) 0.000(2) 0.024(2) -0.026(2) F9 0.129(5) 0.059(3) 0.055(3) -0.014(3) 0.058(3) -0.034(3) O1 0.042(3) 0.036(3) 0.055(3) 0.007(3) 0.019(3) 0.005(2) O2 0.037(3) 0.047(3) 0.036(3) -0.001(2) 0.013(2) 0.006(2) O3 0.048(3) 0.034(3) 0.022(2) -0.003(2) 0.007(2) -0.019(2) O4 0.044(3) 0.040(3) 0.026(2) -0.009(2) 0.010(2) -0.019(2) O5 0.032(3) 0.038(3) 0.023(2) 0.004(2) 0.004(2) -0.010(2) O6 0.027(3) 0.063(4) 0.025(2) 0.007(2) 0.000(2) -0.008(2) O7 0.035(3) 0.033(3) 0.030(2) -0.002(2) 0.008(2) 0.000(2) N1 0.018(2) 0.023(3) 0.019(2) -0.004(2) 0.001(2) 0.000(2) N2 0.026(3) 0.017(3) 0.023(2) -0.002(2) 0.008(2) -0.005(2) N3 0.023(3) 0.022(3) 0.019(2) -0.002(2) 0.006(2) -0.002(2) N4 0.025(3) 0.020(3) 0.012(2) -0.0011(19) 0.0044(19) -0.002(2) N5 0.029(3) 0.021(3) 0.018(2) 0.001(2) 0.002(2) -0.009(2) N6 0.022(3) 0.025(3) 0.014(2) -0.002(2) 0.0020(19) -0.008(2) N7 0.027(3) 0.026(3) 0.023(3) -0.001(2) 0.003(2) -0.002(2) N8 0.027(3) 0.025(3) 0.022(3) -0.003(2) 0.006(2) -0.002(2) C1 0.029(3) 0.023(3) 0.020(3) 0.003(2) 0.000(3) -0.003(3) C2 0.023(3) 0.029(3) 0.027(3) 0.001(3) 0.000(3) -0.004(3) C3 0.021(3) 0.022(3) 0.035(3) 0.001(3) 0.006(3) -0.001(3) C4 0.026(3) 0.021(3) 0.019(3) -0.002(2) 0.005(2) -0.003(3) C5 0.019(3) 0.022(3) 0.020(3) 0.004(2) 0.005(2) 0.000(2) C6 0.020(3) 0.017(3) 0.020(3) 0.000(2) 0.006(2) -0.001(2) C7 0.021(3) 0.019(3) 0.019(3) -0.003(2) 0.005(2) 0.001(2) C8 0.019(3) 0.026(3) 0.019(3) -0.002(2) 0.007(2) -0.002(3) C9 0.024(3) 0.022(3) 0.026(3) -0.001(3) 0.004(3) 0.008(3) C10 0.023(3) 0.029(3) 0.019(3) -0.007(2) 0.003(2) 0.005(3) C11 0.027(4) 0.027(3) 0.041(4) -0.007(3) 0.005(3) 0.006(3) C12 0.093(8) 0.078(7) 0.067(7) -0.021(6) -0.003(6) 0.052(7) C13 0.104(9) 0.063(7) 0.126(10) -0.010(6) 0.088(9) 0.010(6) C14 0.048(5) 0.055(6) 0.068(6) -0.029(5) 0.001(4) 0.016(4) C15 0.033(4) 0.030(3) 0.013(3) 0.000(2) 0.003(2) 0.004(3) C16 0.070(6) 0.068(6) 0.025(4) 0.012(4) 0.024(4) 0.034(5) C17 0.070(6) 0.083(7) 0.038(5) 0.000(5) -0.009(4) -0.041(6) C18 0.080(6) 0.064(6) 0.021(4) -0.006(4) -0.006(4) 0.040(5) C19 0.032(4) 0.029(3) 0.022(3) -0.001(3) 0.007(3) -0.011(3) C20 0.045(4) 0.037(4) 0.023(3) 0.004(3) 0.009(3) -0.015(3) C21 0.038(4) 0.035(4) 0.021(3) 0.006(3) 0.003(3) -0.012(3) C22 0.025(3) 0.019(3) 0.018(3) 0.002(2) 0.005(2) -0.005(2) C23 0.020(3) 0.020(3) 0.016(3) 0.000(2) 0.001(2) 0.001(2) C24 0.024(3) 0.026(3) 0.023(3) -0.002(3) 0.004(3) -0.008(3) C25 0.032(4) 0.027(3) 0.019(3) 0.002(2) 0.007(3) -0.011(3) C26 0.030(3) 0.023(3) 0.015(3) -0.001(2) 0.005(2) -0.001(3) C27 0.109(10) 0.042(6) 0.080(8) 0.012(5) 0.033(7) 0.012(6) C28 0.050(5) 0.044(5) 0.057(5) 0.005(4) 0.008(4) 0.016(4) C29 0.080(7) 0.055(6) 0.068(6) -0.007(5) 0.031(6) 0.024(5) C30 0.039(5) 0.064(6) 0.039(4) 0.003(4) 0.011(4) 0.012(4) C31 0.069(7) 0.090(8) 0.057(6) -0.018(5) 0.029(5) 0.027(6) C32 0.045(5) 0.044(5) 0.043(4) -0.007(4) 0.011(4) -0.015(4) C33 0.034(4) 0.028(3) 0.030(3) -0.006(3) 0.007(3) -0.006(3) C34 0.038(4) 0.028(4) 0.029(3) -0.004(3) 0.008(3) -0.013(3) C35 0.040(4) 0.027(4) 0.033(4) 0.004(3) 0.013(3) -0.001(3) C36 0.049(5) 0.038(4) 0.040(4) 0.000(3) 0.014(4) -0.013(4) C38 0.040(4) 0.037(4) 0.023(3) 0.011(3) 0.004(3) -0.009(3) C39 0.030(4) 0.057(5) 0.028(4) 0.014(3) -0.002(3) -0.008(4) C40 0.031(4) 0.045(4) 0.032(4) 0.010(3) 0.004(3) -0.005(3) C41 0.036(4) 0.092(7) 0.040(4) 0.029(5) 0.001(4) 0.005(5) C42 0.028(3) 0.024(3) 0.016(3) -0.001(2) 0.002(3) -0.009(3) C43 0.032(4) 0.034(4) 0.015(3) -0.002(3) 0.010(3) -0.004(3) O8 0.036(3) 0.080(4) 0.033(3) 0.005(3) 0.011(2) -0.001(3) C44 0.086(8) 0.053(6) 0.087(8) -0.008(5) 0.040(6) -0.010(6) Cl1 0.109(2) 0.0799(19) 0.0840(19) 0.0162(16) 0.0460(18) 0.0220(17) Cl2 0.0801(19) 0.0830(19) 0.0835(19) -0.0258(15) 0.0234(15) 0.0103(16) _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 Nd1 O5 2.400(4) . ? Nd1 O6 2.402(5) . ? Nd1 O3 2.404(5) . ? Nd1 O1 2.449(5) . ? Nd1 O2 2.453(5) . ? Nd1 O7 2.495(5) . ? Nd1 O4 2.511(5) . ? Nd1 N6 2.710(5) . ? Nd1 N5 2.724(5) . ? Ru1 N4 2.022(5) . ? Ru1 N1 2.041(5) . ? Ru1 N2 2.044(5) . ? Ru1 N8 2.049(5) . ? Ru1 N7 2.051(5) . ? Ru1 N3 2.066(5) . ? S1 C43 1.639(7) . ? S2 C42 1.647(7) . ? F1 C27 1.351(14) . ? F2 C27 1.309(12) . ? F3 C27 1.297(12) . ? F4 C31 1.328(5) . ? F5 C31 1.329(5) . ? F6 C31 1.329(5) . ? F6' C31 1.328(5) . ? F4' C31 1.329(5) . ? F5' C31 1.328(5) . ? F7 C36 1.326(9) . ? F8 C36 1.327(8) . ? F9 C36 1.322(9) . ? F10 C32 1.335(4) . ? F11 C32 1.335(4) . ? F12 C32 1.335(4) . ? F10' C32 1.335(4) . ? F12' C32 1.335(4) . ? F11' C32 1.336(4) . ? C37 F15 1.334(5) . ? C37 F13 1.334(5) . ? C37 F14 1.335(5) . ? C37 C38 1.515(12) . ? C37' F13' 1.334(5) . ? C37' F14' 1.335(5) . ? C37' F15' 1.335(5) . ? C37' C38 1.512(13) . ? F16 C41 1.339(5) . ? F17 C41 1.338(5) . ? F18 C41 1.342(5) . ? F18' C41 1.339(5) . ? F16' C41 1.342(5) . ? F17' C41 1.341(5) . ? O1 C28 1.244(10) . ? O2 C30 1.234(10) . ? O3 C35 1.261(8) . ? O4 C33 1.242(8) . ? O5 C38 1.255(8) . ? O6 C40 1.253(8) . ? O7 H4W 0.8499 . ? O7 H3W 0.8498 . ? N1 C10 1.336(8) . ? N1 C6 1.368(7) . ? N2 C1 1.348(8) . ? N2 C5 1.363(7) . ? N3 C22 1.348(7) . ? N3 C19 1.357(8) . ? N4 C26 1.355(7) . ? N4 C23 1.365(7) . ? N5 C22 1.328(7) . ? N5 C21 1.346(8) . ? N6 C23 1.335(7) . ? N6 C24 1.340(8) . ? N7 C43 1.160(8) . ? N8 C42 1.151(8) . ? C1 C2 1.367(9) . ? C1 H1 0.9500 . ? C2 C3 1.400(9) . ? C2 H2 0.9500 . ? C3 C4 1.394(8) . ? C3 C11 1.518(9) . ? C4 C5 1.388(8) . ? C4 H4 0.9500 . ? C5 C6 1.472(8) . ? C6 C7 1.388(8) . ? C7 C8 1.392(8) . ? C7 H7 0.9500 . ? C8 C9 1.388(8) . ? C8 C15 1.515(8) . ? C9 C10 1.366(8) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C14 1.516(11) . ? C11 C12 1.536(11) . ? C11 C13 1.537(12) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.512(9) . ? C15 C18 1.513(10) . ? C15 C17 1.533(11) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.371(9) . ? C19 H19 0.9500 . ? C20 C21 1.390(9) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.464(8) . ? C24 C25 1.394(8) . ? C24 H24 0.9500 . ? C25 C26 1.370(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.537(13) . ? C28 C29 1.404(13) . ? C29 C30 1.395(13) . ? C29 H29 0.9500 . ? C30 C31 1.558(12) . ? C32 C33 1.539(10) . ? C33 C34 1.400(9) . ? C34 C35 1.373(9) . ? C34 H34 0.9500 . ? C35 C36 1.535(10) . ? C38 C39 1.380(10) . ? C39 C40 1.384(10) . ? C39 H39 0.9500 . ? C40 C41 1.538(11) . ? O8 H1W 0.8501 . ? O8 H2W 0.8499 . ? C44 Cl2 1.731(11) . ? C44 Cl1 1.769(11) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? 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 O5 Nd1 O6 72.89(16) . . ? O5 Nd1 O3 141.04(15) . . ? O6 Nd1 O3 92.64(17) . . ? O5 Nd1 O1 73.91(17) . . ? O6 Nd1 O1 79.17(18) . . ? O3 Nd1 O1 139.99(17) . . ? O5 Nd1 O2 134.67(17) . . ? O6 Nd1 O2 75.51(17) . . ? O3 Nd1 O2 71.17(17) . . ? O1 Nd1 O2 68.86(17) . . ? O5 Nd1 O7 82.27(15) . . ? O6 Nd1 O7 136.81(16) . . ? O3 Nd1 O7 84.92(17) . . ? O1 Nd1 O7 127.21(16) . . ? O2 Nd1 O7 141.61(15) . . ? O5 Nd1 O4 72.96(16) . . ? O6 Nd1 O4 71.13(18) . . ? O3 Nd1 O4 68.12(15) . . ? O1 Nd1 O4 140.57(17) . . ? O2 Nd1 O4 124.98(17) . . ? O7 Nd1 O4 68.02(16) . . ? O5 Nd1 N6 138.35(15) . . ? O6 Nd1 N6 142.97(16) . . ? O3 Nd1 N6 72.47(15) . . ? O1 Nd1 N6 90.73(16) . . ? O2 Nd1 N6 67.65(16) . . ? O7 Nd1 N6 76.84(15) . . ? O4 Nd1 N6 128.49(16) . . ? O5 Nd1 N5 77.58(15) . . ? O6 Nd1 N5 137.10(16) . . ? O3 Nd1 N5 129.21(15) . . ? O1 Nd1 N5 62.99(17) . . ? O2 Nd1 N5 106.30(17) . . ? O7 Nd1 N5 66.23(16) . . ? O4 Nd1 N5 127.95(16) . . ? N6 Nd1 N5 61.10(14) . . ? N4 Ru1 N1 96.33(19) . . ? N4 Ru1 N2 91.4(2) . . ? N1 Ru1 N2 78.18(19) . . ? N4 Ru1 N8 91.9(2) . . ? N1 Ru1 N8 96.6(2) . . ? N2 Ru1 N8 174.1(2) . . ? N4 Ru1 N7 176.44(19) . . ? N1 Ru1 N7 87.2(2) . . ? N2 Ru1 N7 88.7(2) . . ? N8 Ru1 N7 88.3(2) . . ? N4 Ru1 N3 79.54(19) . . ? N1 Ru1 N3 175.8(2) . . ? N2 Ru1 N3 100.8(2) . . ? N8 Ru1 N3 84.5(2) . . ? N7 Ru1 N3 96.94(19) . . ? F15 C37 F13 106.0(5) . . ? F15 C37 F14 105.9(5) . . ? F13 C37 F14 105.9(5) . . ? F15 C37 C38 111.2(8) . . ? F13 C37 C38 113.8(7) . . ? F14 C37 C38 113.6(8) . . ? F13' C37' F14' 105.9(5) . . ? F13' C37' F15' 105.8(5) . . ? F14' C37' F15' 105.8(5) . . ? F13' C37' C38 115.1(9) . . ? F14' C37' C38 109.7(10) . . ? F15' C37' C38 113.8(9) . . ? C28 O1 Nd1 136.1(5) . . ? C30 O2 Nd1 137.7(5) . . ? C35 O3 Nd1 134.3(4) . . ? C33 O4 Nd1 131.3(4) . . ? C38 O5 Nd1 133.0(4) . . ? C40 O6 Nd1 134.5(5) . . ? Nd1 O7 H4W 121.5 . . ? Nd1 O7 H3W 127.5 . . ? H4W O7 H3W 106.4 . . ? C10 N1 C6 118.7(5) . . ? C10 N1 Ru1 125.0(4) . . ? C6 N1 Ru1 116.0(4) . . ? C1 N2 C5 117.7(5) . . ? C1 N2 Ru1 125.7(4) . . ? C5 N2 Ru1 116.5(4) . . ? C22 N3 C19 116.8(5) . . ? C22 N3 Ru1 114.3(4) . . ? C19 N3 Ru1 128.5(4) . . ? C26 N4 C23 115.8(5) . . ? C26 N4 Ru1 128.4(4) . . ? C23 N4 Ru1 115.7(4) . . ? C22 N5 C21 116.5(5) . . ? C22 N5 Nd1 120.4(4) . . ? C21 N5 Nd1 122.8(4) . . ? C23 N6 C24 117.6(5) . . ? C23 N6 Nd1 119.9(4) . . ? C24 N6 Nd1 122.5(4) . . ? C43 N7 Ru1 170.9(5) . . ? C42 N8 Ru1 165.0(5) . . ? N2 C1 C2 123.4(6) . . ? N2 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 120.4(6) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 116.0(6) . . ? C4 C3 C11 122.5(6) . . ? C2 C3 C11 121.5(6) . . ? C5 C4 C3 121.5(5) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? N2 C5 C4 121.0(5) . . ? N2 C5 C6 113.7(5) . . ? C4 C5 C6 125.2(5) . . ? N1 C6 C7 119.9(5) . . ? N1 C6 C5 113.9(5) . . ? C7 C6 C5 126.1(5) . . ? C6 C7 C8 121.6(5) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C9 C8 C7 116.0(5) . . ? C9 C8 C15 122.0(5) . . ? C7 C8 C15 121.9(5) . . ? C10 C9 C8 120.9(6) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? N1 C10 C9 122.6(5) . . ? N1 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C14 C11 C3 111.3(6) . . ? C14 C11 C12 108.4(7) . . ? C3 C11 C12 111.5(6) . . ? C14 C11 C13 108.8(8) . . ? C3 C11 C13 107.5(6) . . ? C12 C11 C13 109.4(8) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C18 108.4(6) . . ? C16 C15 C8 110.7(6) . . ? C18 C15 C8 113.1(5) . . ? C16 C15 C17 107.8(7) . . ? C18 C15 C17 110.2(7) . . ? C8 C15 C17 106.5(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 120.5(6) . . ? N3 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C21 118.6(6) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? N5 C21 C20 121.4(6) . . ? N5 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? N5 C22 N3 126.2(5) . . ? N5 C22 C23 118.3(5) . . ? N3 C22 C23 115.5(5) . . ? N6 C23 N4 125.4(5) . . ? N6 C23 C22 119.9(5) . . ? N4 C23 C22 114.6(5) . . ? N6 C24 C25 121.0(6) . . ? N6 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 118.1(5) . . ? C26 C25 H25 120.9 . . ? C24 C25 H25 120.9 . . ? N4 C26 C25 122.0(5) . . ? N4 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? F3 C27 F2 107.4(9) . . ? F3 C27 F1 105.1(10) . . ? F2 C27 F1 108.8(11) . . ? F3 C27 C28 112.6(9) . . ? F2 C27 C28 113.5(10) . . ? F1 C27 C28 109.1(9) . . ? O1 C28 C29 128.0(8) . . ? O1 C28 C27 113.5(8) . . ? C29 C28 C27 118.4(8) . . ? C30 C29 C28 120.3(8) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? O2 C30 C29 127.5(8) . . ? O2 C30 C31 114.2(7) . . ? C29 C30 C31 118.2(7) . . ? F4 C31 F5' 125.2(10) . . ? F4 C31 F6' 73.1(6) . . ? F5' C31 F6' 108.5(5) . . ? F4 C31 F5 108.4(5) . . ? F5' C31 F5 28.8(5) . . ? F6' C31 F5 130.2(9) . . ? F4 C31 F6 108.4(5) . . ? F5' C31 F6 80.2(6) . . ? F6' C31 F6 36.7(5) . . ? F5 C31 F6 108.3(5) . . ? F4 C31 F4' 35.5(5) . . ? F5' C31 F4' 108.4(5) . . ? F6' C31 F4' 108.3(5) . . ? F5 C31 F4' 82.3(6) . . ? F6 C31 F4' 141.4(9) . . ? F4 C31 C30 116.0(8) . . ? F5' C31 C30 113.6(8) . . ? F6' C31 C30 111.6(7) . . ? F5 C31 C30 111.4(7) . . ? F6 C31 C30 104.0(8) . . ? F4' C31 C30 106.2(8) . . ? F10 C32 F11 107.9(4) . . ? F10 C32 F12' 127.2(7) . . ? F11 C32 F12' 81.0(5) . . ? F10 C32 F10' 24.8(4) . . ? F11 C32 F10' 124.4(7) . . ? F12' C32 F10' 107.8(4) . . ? F10 C32 F12 107.9(4) . . ? F11 C32 F12 107.8(4) . . ? F12' C32 F12 28.6(4) . . ? F10' C32 F12 84.4(5) . . ? F10 C32 F11' 85.8(5) . . ? F11 C32 F11' 27.7(4) . . ? F12' C32 F11' 107.8(4) . . ? F10' C32 F11' 107.8(4) . . ? F12 C32 F11' 132.4(7) . . ? F10 C32 C33 112.1(6) . . ? F11 C32 C33 112.2(6) . . ? F12' C32 C33 111.5(6) . . ? F10' C32 C33 114.3(6) . . ? F12 C32 C33 108.7(6) . . ? F11' C32 C33 107.3(6) . . ? O4 C33 C34 127.6(6) . . ? O4 C33 C32 114.1(5) . . ? C34 C33 C32 118.1(5) . . ? C35 C34 C33 120.7(6) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? O3 C35 C34 127.4(6) . . ? O3 C35 C36 113.2(6) . . ? C34 C35 C36 119.3(6) . . ? F9 C36 F7 107.6(7) . . ? F9 C36 F8 107.1(6) . . ? F7 C36 F8 107.4(6) . . ? F9 C36 C35 111.3(6) . . ? F7 C36 C35 109.6(6) . . ? F8 C36 C35 113.4(6) . . ? O5 C38 C39 129.3(6) . . ? O5 C38 C37' 112.7(6) . . ? C39 C38 C37' 117.5(6) . . ? O5 C38 C37 112.4(6) . . ? C39 C38 C37 118.3(6) . . ? C37' C38 C37 9.8(4) . . ? C38 C39 C40 122.8(6) . . ? C38 C39 H39 118.6 . . ? C40 C39 H39 118.6 . . ? O6 C40 C39 127.4(7) . . ? O6 C40 C41 113.5(6) . . ? C39 C40 C41 118.9(6) . . ? F17 C41 F18' 121.8(10) . . ? F17 C41 F16 107.8(4) . . ? F18' C41 F16 81.1(7) . . ? F17 C41 F17' 22.1(6) . . ? F18' C41 F17' 107.6(4) . . ? F16 C41 F17' 125.2(9) . . ? F17 C41 F16' 86.2(6) . . ? F18' C41 F16' 107.6(4) . . ? F16 C41 F16' 27.9(6) . . ? F17' C41 F16' 107.3(4) . . ? F17 C41 F18 107.5(4) . . ? F18' C41 F18 26.8(6) . . ? F16 C41 F18 107.4(4) . . ? F17' C41 F18 88.1(7) . . ? F16' C41 F18 132.4(8) . . ? F17 C41 C40 112.4(6) . . ? F18' C41 C40 115.5(8) . . ? F16 C41 C40 113.6(6) . . ? F17' C41 C40 110.4(8) . . ? F16' C41 C40 108.1(8) . . ? F18 C41 C40 107.8(6) . . ? N8 C42 S2 179.2(6) . . ? N7 C43 S1 179.5(7) . . ? H1W O8 H2W 113.1 . . ? Cl2 C44 Cl1 112.4(6) . . ? Cl2 C44 H44A 109.1 . . ? Cl1 C44 H44A 109.1 . . ? Cl2 C44 H44B 109.1 . . ? Cl1 C44 H44B 109.1 . . ? H44A C44 H44B 107.9 . . ? 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 O5 Nd1 O1 C28 167.3(8) . . . . ? O6 Nd1 O1 C28 92.2(8) . . . . ? O3 Nd1 O1 C28 11.1(9) . . . . ? O2 Nd1 O1 C28 13.7(8) . . . . ? O7 Nd1 O1 C28 -125.9(7) . . . . ? O4 Nd1 O1 C28 133.5(7) . . . . ? N6 Nd1 O1 C28 -52.0(8) . . . . ? N5 Nd1 O1 C28 -108.7(8) . . . . ? O5 Nd1 O2 C30 -44.9(8) . . . . ? O6 Nd1 O2 C30 -91.8(7) . . . . ? O3 Nd1 O2 C30 170.2(8) . . . . ? O1 Nd1 O2 C30 -8.0(7) . . . . ? O7 Nd1 O2 C30 115.7(7) . . . . ? O4 Nd1 O2 C30 -145.8(7) . . . . ? N6 Nd1 O2 C30 92.0(7) . . . . ? N5 Nd1 O2 C30 43.6(8) . . . . ? O5 Nd1 O3 C35 -29.8(8) . . . . ? O6 Nd1 O3 C35 35.9(6) . . . . ? O1 Nd1 O3 C35 112.2(6) . . . . ? O2 Nd1 O3 C35 109.6(7) . . . . ? O7 Nd1 O3 C35 -100.9(6) . . . . ? O4 Nd1 O3 C35 -32.5(6) . . . . ? N6 Nd1 O3 C35 -178.6(7) . . . . ? N5 Nd1 O3 C35 -154.4(6) . . . . ? O5 Nd1 O4 C33 -147.8(6) . . . . ? O6 Nd1 O4 C33 -70.5(6) . . . . ? O3 Nd1 O4 C33 30.4(6) . . . . ? O1 Nd1 O4 C33 -113.8(6) . . . . ? O2 Nd1 O4 C33 -14.7(7) . . . . ? O7 Nd1 O4 C33 123.8(6) . . . . ? N6 Nd1 O4 C33 73.2(6) . . . . ? N5 Nd1 O4 C33 153.9(6) . . . . ? O6 Nd1 O5 C38 -0.7(6) . . . . ? O3 Nd1 O5 C38 71.6(7) . . . . ? O1 Nd1 O5 C38 -84.0(6) . . . . ? O2 Nd1 O5 C38 -48.4(7) . . . . ? O7 Nd1 O5 C38 143.6(6) . . . . ? O4 Nd1 O5 C38 74.3(6) . . . . ? N6 Nd1 O5 C38 -156.3(6) . . . . ? N5 Nd1 O5 C38 -149.2(6) . . . . ? O5 Nd1 O6 C40 3.0(7) . . . . ? O3 Nd1 O6 C40 -140.2(7) . . . . ? O1 Nd1 O6 C40 79.3(7) . . . . ? O2 Nd1 O6 C40 150.0(7) . . . . ? O7 Nd1 O6 C40 -54.8(8) . . . . ? O4 Nd1 O6 C40 -74.4(7) . . . . ? N6 Nd1 O6 C40 155.9(6) . . . . ? N5 Nd1 O6 C40 51.5(8) . . . . ? N4 Ru1 N1 C10 84.0(5) . . . . ? N2 Ru1 N1 C10 174.2(5) . . . . ? N8 Ru1 N1 C10 -8.6(5) . . . . ? N7 Ru1 N1 C10 -96.6(5) . . . . ? N3 Ru1 N1 C10 97(3) . . . . ? N4 Ru1 N1 C6 -101.8(4) . . . . ? N2 Ru1 N1 C6 -11.6(4) . . . . ? N8 Ru1 N1 C6 165.6(4) . . . . ? N7 Ru1 N1 C6 77.6(4) . . . . ? N3 Ru1 N1 C6 -89(3) . . . . ? N4 Ru1 N2 C1 -77.0(5) . . . . ? N1 Ru1 N2 C1 -173.2(5) . . . . ? N8 Ru1 N2 C1 158.5(17) . . . . ? N7 Ru1 N2 C1 99.4(5) . . . . ? N3 Ru1 N2 C1 2.6(5) . . . . ? N4 Ru1 N2 C5 106.5(4) . . . . ? N1 Ru1 N2 C5 10.4(4) . . . . ? N8 Ru1 N2 C5 -18(2) . . . . ? N7 Ru1 N2 C5 -77.0(4) . . . . ? N3 Ru1 N2 C5 -173.8(4) . . . . ? N4 Ru1 N3 C22 -4.1(4) . . . . ? N1 Ru1 N3 C22 -18(3) . . . . ? N2 Ru1 N3 C22 -93.6(4) . . . . ? N8 Ru1 N3 C22 88.8(4) . . . . ? N7 Ru1 N3 C22 176.4(4) . . . . ? N4 Ru1 N3 C19 -177.2(6) . . . . ? N1 Ru1 N3 C19 169(2) . . . . ? N2 Ru1 N3 C19 93.4(5) . . . . ? N8 Ru1 N3 C19 -84.2(5) . . . . ? N7 Ru1 N3 C19 3.4(6) . . . . ? N1 Ru1 N4 C26 2.4(5) . . . . ? N2 Ru1 N4 C26 -75.9(5) . . . . ? N8 Ru1 N4 C26 99.3(5) . . . . ? N7 Ru1 N4 C26 -168(3) . . . . ? N3 Ru1 N4 C26 -176.7(5) . . . . ? N1 Ru1 N4 C23 -178.8(4) . . . . ? N2 Ru1 N4 C23 103.0(4) . . . . ? N8 Ru1 N4 C23 -81.9(4) . . . . ? N7 Ru1 N4 C23 11(3) . . . . ? N3 Ru1 N4 C23 2.2(4) . . . . ? O5 Nd1 N5 C22 -179.7(5) . . . . ? O6 Nd1 N5 C22 133.1(4) . . . . ? O3 Nd1 N5 C22 -31.7(5) . . . . ? O1 Nd1 N5 C22 102.2(5) . . . . ? O2 Nd1 N5 C22 47.0(5) . . . . ? O7 Nd1 N5 C22 -92.8(5) . . . . ? O4 Nd1 N5 C22 -123.2(4) . . . . ? N6 Nd1 N5 C22 -5.1(4) . . . . ? O5 Nd1 N5 C21 7.8(5) . . . . ? O6 Nd1 N5 C21 -39.4(6) . . . . ? O3 Nd1 N5 C21 155.8(5) . . . . ? O1 Nd1 N5 C21 -70.3(5) . . . . ? O2 Nd1 N5 C21 -125.5(5) . . . . ? O7 Nd1 N5 C21 94.8(5) . . . . ? O4 Nd1 N5 C21 64.3(6) . . . . ? N6 Nd1 N5 C21 -177.6(6) . . . . ? O5 Nd1 N6 C23 10.0(5) . . . . ? O6 Nd1 N6 C23 -129.1(4) . . . . ? O3 Nd1 N6 C23 160.7(5) . . . . ? O1 Nd1 N6 C23 -56.3(4) . . . . ? O2 Nd1 N6 C23 -123.0(5) . . . . ? O7 Nd1 N6 C23 71.9(4) . . . . ? O4 Nd1 N6 C23 119.3(4) . . . . ? N5 Nd1 N6 C23 2.0(4) . . . . ? O5 Nd1 N6 C24 -171.8(4) . . . . ? O6 Nd1 N6 C24 49.1(6) . . . . ? O3 Nd1 N6 C24 -21.1(5) . . . . ? O1 Nd1 N6 C24 121.9(5) . . . . ? O2 Nd1 N6 C24 55.2(5) . . . . ? O7 Nd1 N6 C24 -109.9(5) . . . . ? O4 Nd1 N6 C24 -62.5(5) . . . . ? N5 Nd1 N6 C24 -179.8(5) . . . . ? N4 Ru1 N7 C43 -170(3) . . . . ? N1 Ru1 N7 C43 20(3) . . . . ? N2 Ru1 N7 C43 98(3) . . . . ? N8 Ru1 N7 C43 -77(3) . . . . ? N3 Ru1 N7 C43 -161(3) . . . . ? N4 Ru1 N8 C42 131.0(19) . . . . ? N1 Ru1 N8 C42 -132.4(19) . . . . ? N2 Ru1 N8 C42 -104(2) . . . . ? N7 Ru1 N8 C42 -45.4(19) . . . . ? N3 Ru1 N8 C42 51.7(19) . . . . ? C5 N2 C1 C2 2.2(9) . . . . ? Ru1 N2 C1 C2 -174.3(5) . . . . ? N2 C1 C2 C3 -0.4(10) . . . . ? C1 C2 C3 C4 -1.3(9) . . . . ? C1 C2 C3 C11 178.1(6) . . . . ? C2 C3 C4 C5 1.2(9) . . . . ? C11 C3 C4 C5 -178.2(6) . . . . ? C1 N2 C5 C4 -2.2(8) . . . . ? Ru1 N2 C5 C4 174.5(4) . . . . ? C1 N2 C5 C6 175.7(5) . . . . ? Ru1 N2 C5 C6 -7.5(6) . . . . ? C3 C4 C5 N2 0.6(9) . . . . ? C3 C4 C5 C6 -177.1(6) . . . . ? C10 N1 C6 C7 4.2(8) . . . . ? Ru1 N1 C6 C7 -170.4(4) . . . . ? C10 N1 C6 C5 -174.3(5) . . . . ? Ru1 N1 C6 C5 11.1(6) . . . . ? N2 C5 C6 N1 -2.3(7) . . . . ? C4 C5 C6 N1 175.5(5) . . . . ? N2 C5 C6 C7 179.3(5) . . . . ? C4 C5 C6 C7 -2.9(10) . . . . ? N1 C6 C7 C8 -0.9(9) . . . . ? C5 C6 C7 C8 177.5(6) . . . . ? C6 C7 C8 C9 -2.9(9) . . . . ? C6 C7 C8 C15 175.3(5) . . . . ? C7 C8 C9 C10 3.6(9) . . . . ? C15 C8 C9 C10 -174.7(6) . . . . ? C6 N1 C10 C9 -3.6(9) . . . . ? Ru1 N1 C10 C9 170.4(5) . . . . ? C8 C9 C10 N1 -0.3(10) . . . . ? C4 C3 C11 C14 49.8(9) . . . . ? C2 C3 C11 C14 -129.7(7) . . . . ? C4 C3 C11 C12 170.9(8) . . . . ? C2 C3 C11 C12 -8.5(10) . . . . ? C4 C3 C11 C13 -69.2(9) . . . . ? C2 C3 C11 C13 111.4(8) . . . . ? C9 C8 C15 C16 -132.1(7) . . . . ? C7 C8 C15 C16 49.7(8) . . . . ? C9 C8 C15 C18 -10.2(9) . . . . ? C7 C8 C15 C18 171.7(7) . . . . ? C9 C8 C15 C17 111.0(8) . . . . ? C7 C8 C15 C17 -67.2(8) . . . . ? C22 N3 C19 C20 -0.8(9) . . . . ? Ru1 N3 C19 C20 172.1(5) . . . . ? N3 C19 C20 C21 2.5(11) . . . . ? C22 N5 C21 C20 1.2(10) . . . . ? Nd1 N5 C21 C20 173.9(5) . . . . ? C19 C20 C21 N5 -2.7(11) . . . . ? C21 N5 C22 N3 0.7(10) . . . . ? Nd1 N5 C22 N3 -172.2(5) . . . . ? C21 N5 C22 C23 -179.3(6) . . . . ? Nd1 N5 C22 C23 7.7(7) . . . . ? C19 N3 C22 N5 -0.9(9) . . . . ? Ru1 N3 C22 N5 -174.8(5) . . . . ? C19 N3 C22 C23 179.2(5) . . . . ? Ru1 N3 C22 C23 5.3(7) . . . . ? C24 N6 C23 N4 0.0(9) . . . . ? Nd1 N6 C23 N4 178.2(4) . . . . ? C24 N6 C23 C22 -177.5(5) . . . . ? Nd1 N6 C23 C22 0.8(7) . . . . ? C26 N4 C23 N6 1.3(9) . . . . ? Ru1 N4 C23 N6 -177.7(5) . . . . ? C26 N4 C23 C22 178.9(5) . . . . ? Ru1 N4 C23 C22 -0.1(6) . . . . ? N5 C22 C23 N6 -5.7(9) . . . . ? N3 C22 C23 N6 174.3(5) . . . . ? N5 C22 C23 N4 176.6(5) . . . . ? N3 C22 C23 N4 -3.5(8) . . . . ? C23 N6 C24 C25 -1.2(9) . . . . ? Nd1 N6 C24 C25 -179.4(5) . . . . ? N6 C24 C25 C26 1.1(10) . . . . ? C23 N4 C26 C25 -1.4(9) . . . . ? Ru1 N4 C26 C25 177.5(5) . . . . ? C24 C25 C26 N4 0.2(10) . . . . ? Nd1 O1 C28 C29 -14.9(15) . . . . ? Nd1 O1 C28 C27 161.0(7) . . . . ? F3 C27 C28 O1 43.7(13) . . . . ? F2 C27 C28 O1 165.9(10) . . . . ? F1 C27 C28 O1 -72.6(11) . . . . ? F3 C27 C28 C29 -140.1(10) . . . . ? F2 C27 C28 C29 -17.8(15) . . . . ? F1 C27 C28 C29 103.7(11) . . . . ? O1 C28 C29 C30 2.8(16) . . . . ? C27 C28 C29 C30 -172.8(9) . . . . ? Nd1 O2 C30 C29 3.1(14) . . . . ? Nd1 O2 C30 C31 -173.6(4) . . . . ? C28 C29 C30 O2 3.0(15) . . . . ? C28 C29 C30 C31 179.6(8) . . . . ? O2 C30 C31 F4 -23.8(9) . . . . ? C29 C30 C31 F4 159.2(8) . . . . ? O2 C30 C31 F5' -179.6(8) . . . . ? C29 C30 C31 F5' 3.4(10) . . . . ? O2 C30 C31 F6' 57.3(10) . . . . ? C29 C30 C31 F6' -119.7(9) . . . . ? O2 C30 C31 F5 -148.4(7) . . . . ? C29 C30 C31 F5 34.5(10) . . . . ? O2 C30 C31 F6 95.1(8) . . . . ? C29 C30 C31 F6 -81.9(9) . . . . ? O2 C30 C31 F4' -60.5(9) . . . . ? C29 C30 C31 F4' 122.4(9) . . . . ? Nd1 O4 C33 C34 -22.2(11) . . . . ? Nd1 O4 C33 C32 162.1(4) . . . . ? F10 C32 C33 O4 -159.1(7) . . . . ? F11 C32 C33 O4 -37.5(8) . . . . ? F12' C32 C33 O4 51.3(8) . . . . ? F10' C32 C33 O4 173.9(7) . . . . ? F12 C32 C33 O4 81.7(8) . . . . ? F11' C32 C33 O4 -66.5(8) . . . . ? F10 C32 C33 C34 24.7(8) . . . . ? F11 C32 C33 C34 146.4(7) . . . . ? F12' C32 C33 C34 -124.8(8) . . . . ? F10' C32 C33 C34 -2.2(9) . . . . ? F12 C32 C33 C34 -94.5(8) . . . . ? F11' C32 C33 C34 117.3(8) . . . . ? O4 C33 C34 C35 -4.3(12) . . . . ? C32 C33 C34 C35 171.3(6) . . . . ? Nd1 O3 C35 C34 25.5(12) . . . . ? Nd1 O3 C35 C36 -157.2(5) . . . . ? C33 C34 C35 O3 3.9(12) . . . . ? C33 C34 C35 C36 -173.2(7) . . . . ? O3 C35 C36 F9 40.2(9) . . . . ? C34 C35 C36 F9 -142.3(7) . . . . ? O3 C35 C36 F7 -78.8(8) . . . . ? C34 C35 C36 F7 98.8(8) . . . . ? O3 C35 C36 F8 161.1(6) . . . . ? C34 C35 C36 F8 -21.3(10) . . . . ? Nd1 O5 C38 C39 -0.4(12) . . . . ? Nd1 O5 C38 C37' 171.2(5) . . . . ? Nd1 O5 C38 C37 -178.2(4) . . . . ? F13' C37' C38 O5 161.6(7) . . . . ? F14' C37' C38 O5 -79.2(8) . . . . ? F15' C37' C38 O5 39.2(9) . . . . ? F13' C37' C38 C39 -25.8(10) . . . . ? F14' C37' C38 C39 93.5(8) . . . . ? F15' C37' C38 C39 -148.2(8) . . . . ? F13' C37' C38 C37 71(3) . . . . ? F14' C37' C38 C37 -170(3) . . . . ? F15' C37' C38 C37 -51(3) . . . . ? F15 C37 C38 O5 93.8(7) . . . . ? F13 C37 C38 O5 -146.7(6) . . . . ? F14 C37 C38 O5 -25.4(8) . . . . ? F15 C37 C38 C39 -84.3(8) . . . . ? F13 C37 C38 C39 35.3(9) . . . . ? F14 C37 C38 C39 156.5(7) . . . . ? F15 C37 C38 C37' -173(3) . . . . ? F13 C37 C38 C37' -53(3) . . . . ? F14 C37 C38 C37' 68(3) . . . . ? O5 C38 C39 C40 0.2(14) . . . . ? C37' C38 C39 C40 -171.0(8) . . . . ? C37 C38 C39 C40 177.9(7) . . . . ? Nd1 O6 C40 C39 -4.3(13) . . . . ? Nd1 O6 C40 C41 171.7(4) . . . . ? C38 C39 C40 O6 2.2(14) . . . . ? C38 C39 C40 C41 -173.6(7) . . . . ? O6 C40 C41 F17 53.2(8) . . . . ? C39 C40 C41 F17 -130.4(7) . . . . ? O6 C40 C41 F18' -92.8(11) . . . . ? C39 C40 C41 F18' 83.5(11) . . . . ? O6 C40 C41 F16 176.0(7) . . . . ? C39 C40 C41 F16 -7.6(9) . . . . ? O6 C40 C41 F17' 29.5(10) . . . . ? C39 C40 C41 F17' -154.1(10) . . . . ? O6 C40 C41 F16' 146.6(10) . . . . ? C39 C40 C41 F16' -37.0(11) . . . . ? O6 C40 C41 F18 -65.2(8) . . . . ? C39 C40 C41 F18 111.2(8) . . . . ? Ru1 N8 C42 S2 -146(48) . . . . ? Ru1 N7 C43 S1 171(100) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H4W Cl2 0.85 2.63 3.342(5) 142.2 . O7 H3W O8 0.85 1.86 2.706(7) 177.0 . O8 H2W S2 0.85 2.62 3.465(6) 171.9 . O8 H1W S1 0.85 2.44 3.280(6) 169.0 3_666 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.045 _refine_diff_density_min -1.021 _refine_diff_density_rms 0.153 #===END data_imw627m _database_code_depnum_ccdc_archive 'CCDC 661955' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H64 F30 Gd N8 O9.50 P2 Ru' _chemical_formula_weight 1927.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 25.1174(15) _cell_length_b 11.2557(6) _cell_length_c 30.1564(18) _cell_angle_alpha 90.00 _cell_angle_beta 105.252(3) _cell_angle_gamma 90.00 _cell_volume 8225.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9117 _cell_measurement_theta_min 4.576 _cell_measurement_theta_max 57.963 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3832 _exptl_absorpt_coefficient_mu 1.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6773 _exptl_absorpt_correction_T_max 0.8846 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 243062 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 0.84 _diffrn_reflns_theta_max 29.74 _reflns_number_total 22522 _reflns_number_gt 17724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+28.7584P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22522 _refine_ls_number_parameters 982 _refine_ls_number_restraints 89 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _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 Gd1 Gd 0.182642(7) 0.644873(16) 0.168825(6) 0.02251(6) Uani 1 1 d . . . Ru1 Ru 0.268360(11) 0.79008(2) 0.001134(10) 0.01877(7) Uani 1 1 d . . . P1 P 0.12004(6) 0.31803(11) 0.01313(4) 0.0385(3) Uani 1 1 d . . . F1 F 0.07939(19) 0.2082(4) 0.00625(16) 0.0832(13) Uani 1 1 d . . . F2 F 0.10638(19) 0.3388(4) -0.04049(11) 0.0724(11) Uani 1 1 d . . . F3 F 0.16957(17) 0.2339(3) 0.01223(14) 0.0703(10) Uani 1 1 d . . . F4 F 0.13206(17) 0.3028(3) 0.06757(11) 0.0636(9) Uani 1 1 d . . . F5 F 0.06963(16) 0.4048(4) 0.01499(14) 0.0726(10) Uani 1 1 d . . . F6 F 0.15952(16) 0.4311(3) 0.02142(13) 0.0654(9) Uani 1 1 d . . . F9 F 0.46075(8) 0.2868(2) 0.01631(10) 0.0390(6) Uani 1 1 d D . . P2 P 0.40039(8) 0.2673(2) 0.02514(11) 0.0243(6) Uiso 0.526(7) 1 d PDU A 1 F7 F 0.3995(3) 0.1306(4) 0.0120(2) 0.0363(15) Uiso 0.526(7) 1 d PDU A 1 F8 F 0.3742(3) 0.3187(6) -0.0258(2) 0.0490(15) Uiso 0.526(7) 1 d PDU A 1 F10 F 0.4272(2) 0.2171(6) 0.07511(15) 0.0439(14) Uiso 0.526(7) 1 d PDU A 1 F11 F 0.33945(17) 0.2429(5) 0.0301(2) 0.0368(13) Uiso 0.526(7) 1 d PDU A 1 F12 F 0.4001(2) 0.3993(4) 0.0444(2) 0.0429(14) Uiso 0.526(7) 1 d PDU A 1 P2' P 0.39713(9) 0.2824(2) 0.01438(12) 0.0235(6) Uiso 0.474(7) 1 d PDU A 2 F7' F 0.3981(3) 0.1459(4) 0.0000(2) 0.0306(15) Uiso 0.474(7) 1 d PDU A 2 F8' F 0.3793(2) 0.2956(5) -0.03982(17) 0.0348(14) Uiso 0.474(7) 1 d PDU A 2 F10' F 0.4150(3) 0.2676(7) 0.06902(16) 0.0510(16) Uiso 0.474(7) 1 d PDU A 2 F11' F 0.33376(17) 0.2802(6) 0.0152(2) 0.0341(13) Uiso 0.474(7) 1 d PDU A 2 F12' F 0.3989(2) 0.4223(4) 0.0219(2) 0.0389(15) Uiso 0.474(7) 1 d PDU A 2 C45 C 0.3411(5) 0.8875(13) 0.2167(2) 0.063(2) Uiso 0.549(6) 1 d PDU B 1 F13 F 0.3479(3) 0.8948(7) 0.1748(2) 0.0707(19) Uiso 0.549(6) 1 d PDU B 1 F14 F 0.3911(3) 0.8751(7) 0.2458(2) 0.0641(18) Uiso 0.549(6) 1 d PDU B 1 F15 F 0.3191(4) 0.9881(8) 0.2261(3) 0.104(3) Uiso 0.549(6) 1 d PDU B 1 C45' C 0.3459(7) 0.8680(14) 0.2088(3) 0.068(3) Uiso 0.451(6) 1 d PDU B 2 F13' F 0.3781(4) 0.8122(10) 0.1862(3) 0.100(3) Uiso 0.451(6) 1 d PDU B 2 F14' F 0.3781(4) 0.9181(8) 0.2470(3) 0.070(2) Uiso 0.451(6) 1 d PDU B 2 F15' F 0.3194(4) 0.9559(9) 0.1816(3) 0.097(3) Uiso 0.451(6) 1 d PDU B 2 F16 F 0.24732(17) 0.5811(6) 0.33483(14) 0.1058(19) Uani 1 1 d . . . F17 F 0.33052(17) 0.6418(3) 0.35082(11) 0.0678(11) Uani 1 1 d . . . F18 F 0.3092(2) 0.4736(4) 0.32041(15) 0.0921(15) Uani 1 1 d . . . F19 F 0.00336(18) 0.8554(5) 0.09519(14) 0.0905(16) Uani 1 1 d . . . F20 F -0.01705(15) 0.7170(4) 0.1344(2) 0.118(2) Uani 1 1 d . . . F21 F -0.02079(14) 0.8989(3) 0.15495(13) 0.0614(9) Uani 1 1 d . . . F25 F 0.1704(3) 0.1380(7) 0.1944(3) 0.087(2) Uiso 0.485(10) 1 d PDU C 1 F26 F 0.2188(3) 0.2156(6) 0.1533(2) 0.0461(16) Uiso 0.485(10) 1 d PDU C 1 F27 F 0.2474(3) 0.2190(8) 0.2265(2) 0.069(2) Uiso 0.485(10) 1 d PDU C 1 F25' F 0.1608(3) 0.1578(7) 0.1682(3) 0.073(2) Uiso 0.515(10) 1 d PDU C 2 F26' F 0.2393(3) 0.2283(6) 0.1664(2) 0.0540(17) Uiso 0.515(10) 1 d PDU C 2 F27' F 0.2244(3) 0.1770(7) 0.2307(2) 0.069(2) Uiso 0.515(10) 1 d PDU C 2 F28 F 0.05677(13) 0.3663(3) 0.26419(11) 0.0527(8) Uani 1 1 d . C . F29 F 0.09952(14) 0.5200(3) 0.29749(10) 0.0530(8) Uani 1 1 d . C . F30 F 0.03128(13) 0.5394(4) 0.23796(13) 0.0711(11) Uani 1 1 d . C . O1 O 0.19466(12) 0.4342(3) 0.17290(10) 0.0296(6) Uani 1 1 d . . . O2 O 0.12183(12) 0.5688(3) 0.20950(10) 0.0314(6) Uani 1 1 d . . . O3 O 0.09673(12) 0.7508(3) 0.14442(10) 0.0321(6) Uani 1 1 d . . . O4 O 0.17915(14) 0.8007(3) 0.22159(12) 0.0411(8) Uani 1 1 d . D . O5 O 0.26926(13) 0.7468(3) 0.18388(11) 0.0415(8) Uani 1 1 d . B . O6 O 0.24001(13) 0.5883(3) 0.24331(10) 0.0359(7) Uani 1 1 d . B . O7 O 0.12137(12) 0.5585(3) 0.10156(10) 0.0350(7) Uani 1 1 d . . . O8 O 0.0450(2) 0.6747(5) 0.03511(16) 0.0851(16) Uani 1 1 d . . . N1 N 0.34708(13) 0.8388(3) 0.03681(10) 0.0206(6) Uani 1 1 d . . . N2 N 0.31490(12) 0.7122(3) -0.03721(10) 0.0209(6) Uani 1 1 d . . . N3 N 0.25423(12) 0.9340(3) -0.04173(10) 0.0211(6) Uani 1 1 d . . . N4 N 0.19116(12) 0.7528(3) -0.04090(11) 0.0217(6) Uani 1 1 d . . . N5 N 0.22666(13) 0.8596(3) 0.04541(11) 0.0220(6) Uani 1 1 d . . . N6 N 0.27151(12) 0.6494(3) 0.04551(11) 0.0206(6) Uani 1 1 d . . . N7 N 0.18750(13) 0.8053(3) 0.10645(11) 0.0247(6) Uani 1 1 d . . . N8 N 0.23924(13) 0.5863(3) 0.10952(11) 0.0236(6) Uani 1 1 d . . . C1 C 0.36005(16) 0.9079(3) 0.07423(13) 0.0258(7) Uani 1 1 d . . . H1 H 0.3311 0.9342 0.0868 0.031 Uiso 1 1 calc R . . C2 C 0.41335(17) 0.9429(4) 0.09548(13) 0.0279(8) Uani 1 1 d . . . H2 H 0.4203 0.9925 0.1219 0.034 Uiso 1 1 calc R . . C3 C 0.45686(15) 0.9061(3) 0.07847(13) 0.0238(7) Uani 1 1 d . . . C4 C 0.44334(15) 0.8322(3) 0.03966(13) 0.0233(7) Uani 1 1 d . . . H4 H 0.4718 0.8037 0.0270 0.028 Uiso 1 1 calc R . . C5 C 0.38911(15) 0.8003(3) 0.01952(12) 0.0206(7) Uani 1 1 d . . . C6 C 0.37082(15) 0.7265(3) -0.02219(12) 0.0207(7) Uani 1 1 d . . . C7 C 0.40592(15) 0.6741(3) -0.04504(13) 0.0225(7) Uani 1 1 d . . . H7 H 0.4446 0.6855 -0.0338 0.027 Uiso 1 1 calc R . . C8 C 0.38551(15) 0.6049(3) -0.08422(12) 0.0220(7) Uani 1 1 d . . . C9 C 0.32826(16) 0.5932(3) -0.09913(14) 0.0261(8) Uani 1 1 d . . . H9 H 0.3121 0.5476 -0.1258 0.031 Uiso 1 1 calc R . . C10 C 0.29516(15) 0.6476(3) -0.07533(13) 0.0241(7) Uani 1 1 d . . . H10 H 0.2563 0.6388 -0.0865 0.029 Uiso 1 1 calc R . . C11 C 0.51660(16) 0.9448(3) 0.10023(14) 0.0275(8) Uani 1 1 d . . . C12 C 0.5215(2) 1.0195(4) 0.14359(16) 0.0392(10) Uani 1 1 d . . . H12A H 0.5602 1.0423 0.1565 0.059 Uiso 1 1 calc R . . H12B H 0.5088 0.9728 0.1662 0.059 Uiso 1 1 calc R . . H12C H 0.4988 1.0911 0.1357 0.059 Uiso 1 1 calc R . . C13 C 0.53665(18) 1.0197(4) 0.06526(16) 0.0356(9) Uani 1 1 d . . . H13A H 0.5748 1.0447 0.0788 0.053 Uiso 1 1 calc R . . H13B H 0.5131 1.0899 0.0570 0.053 Uiso 1 1 calc R . . H13C H 0.5348 0.9722 0.0377 0.053 Uiso 1 1 calc R . . C14 C 0.5530(2) 0.8345(4) 0.1129(2) 0.0477(13) Uani 1 1 d . . . H14A H 0.5912 0.8589 0.1268 0.072 Uiso 1 1 calc R . . H14B H 0.5513 0.7879 0.0851 0.072 Uiso 1 1 calc R . . H14C H 0.5398 0.7861 0.1348 0.072 Uiso 1 1 calc R . . C15 C 0.42459(16) 0.5487(3) -0.10936(13) 0.0258(7) Uani 1 1 d . . . C16 C 0.45159(19) 0.6489(4) -0.13012(16) 0.0343(9) Uani 1 1 d . . . H16A H 0.4770 0.6148 -0.1464 0.051 Uiso 1 1 calc R . . H16B H 0.4721 0.7012 -0.1055 0.051 Uiso 1 1 calc R . . H16C H 0.4230 0.6948 -0.1517 0.051 Uiso 1 1 calc R . . C17 C 0.46929(17) 0.4775(4) -0.07480(15) 0.0309(8) Uani 1 1 d . . . H17A H 0.4945 0.4413 -0.0908 0.046 Uiso 1 1 calc R . . H17B H 0.4518 0.4150 -0.0609 0.046 Uiso 1 1 calc R . . H17C H 0.4900 0.5308 -0.0507 0.046 Uiso 1 1 calc R . . C18 C 0.39379(19) 0.4647(4) -0.14749(15) 0.0359(9) Uani 1 1 d . . . H18A H 0.4199 0.4300 -0.1629 0.054 Uiso 1 1 calc R . . H18B H 0.3654 0.5092 -0.1698 0.054 Uiso 1 1 calc R . . H18C H 0.3763 0.4012 -0.1341 0.054 Uiso 1 1 calc R . . C19 C 0.29100(15) 1.0200(3) -0.04293(13) 0.0253(7) Uani 1 1 d . . . H19 H 0.3282 1.0100 -0.0255 0.030 Uiso 1 1 calc R . . C20 C 0.27678(16) 1.1219(3) -0.06854(14) 0.0281(8) Uani 1 1 d . . . H20 H 0.3043 1.1794 -0.0691 0.034 Uiso 1 1 calc R . . C21 C 0.22243(17) 1.1417(3) -0.09375(13) 0.0253(7) Uani 1 1 d . . . C22 C 0.18513(16) 1.0503(3) -0.09369(13) 0.0244(7) Uani 1 1 d . . . H22 H 0.1479 1.0583 -0.1111 0.029 Uiso 1 1 calc R . . C23 C 0.20178(14) 0.9478(3) -0.06847(12) 0.0211(7) Uani 1 1 d . . . C24 C 0.16587(15) 0.8439(3) -0.06809(13) 0.0226(7) Uani 1 1 d . . . C25 C 0.11125(16) 0.8361(4) -0.09346(14) 0.0291(8) Uani 1 1 d . . . H25 H 0.0945 0.9014 -0.1119 0.035 Uiso 1 1 calc R . . C26 C 0.08046(17) 0.7329(4) -0.09223(15) 0.0324(9) Uani 1 1 d . . . C27 C 0.10760(18) 0.6403(4) -0.06591(15) 0.0330(9) Uani 1 1 d . . . H27 H 0.0888 0.5674 -0.0650 0.040 Uiso 1 1 calc R . . C28 C 0.16176(16) 0.6524(3) -0.04086(15) 0.0276(8) Uani 1 1 d . . . H28 H 0.1792 0.5872 -0.0228 0.033 Uiso 1 1 calc R . . C29 C 0.20734(18) 1.2588(4) -0.11962(16) 0.0328(9) Uani 1 1 d . . . C30 C 0.2247(2) 1.3625(4) -0.0857(2) 0.0448(12) Uani 1 1 d . . . H30A H 0.2152 1.4379 -0.1021 0.067 Uiso 1 1 calc R . . H30B H 0.2647 1.3592 -0.0719 0.067 Uiso 1 1 calc R . . H30C H 0.2054 1.3563 -0.0615 0.067 Uiso 1 1 calc R . . C31 C 0.2382(3) 1.2658(5) -0.15723(19) 0.0525(14) Uani 1 1 d . . . H31A H 0.2290 1.3406 -0.1742 0.079 Uiso 1 1 calc R . . H31B H 0.2273 1.1988 -0.1784 0.079 Uiso 1 1 calc R . . H31C H 0.2781 1.2626 -0.1431 0.079 Uiso 1 1 calc R . . C32 C 0.1452(2) 1.2688(4) -0.1408(2) 0.0474(13) Uani 1 1 d . . . H32A H 0.1369 1.3447 -0.1571 0.071 Uiso 1 1 calc R . . H32B H 0.1260 1.2649 -0.1165 0.071 Uiso 1 1 calc R . . H32C H 0.1328 1.2033 -0.1625 0.071 Uiso 1 1 calc R . . C33 C 0.01912(19) 0.7285(5) -0.11824(18) 0.0471(13) Uani 1 1 d . . . C34 C -0.0115(2) 0.8172(7) -0.0939(3) 0.0683(18) Uani 1 1 d . . . H34A H -0.0071 0.7919 -0.0621 0.102 Uiso 1 1 calc R . . H34B H -0.0508 0.8187 -0.1101 0.102 Uiso 1 1 calc R . . H34C H 0.0041 0.8969 -0.0942 0.102 Uiso 1 1 calc R . . C35 C -0.0050(3) 0.6059(7) -0.1168(3) 0.077(2) Uani 1 1 d . . . H35A H 0.0003 0.5813 -0.0848 0.115 Uiso 1 1 calc R . . H35B H 0.0135 0.5494 -0.1325 0.115 Uiso 1 1 calc R . . H35C H -0.0446 0.6074 -0.1323 0.115 Uiso 1 1 calc R . . C36 C 0.0115(2) 0.7699(6) -0.16726(19) 0.0569(16) Uani 1 1 d . . . H36A H 0.0272 0.8496 -0.1672 0.085 Uiso 1 1 calc R . . H36B H -0.0280 0.7721 -0.1830 0.085 Uiso 1 1 calc R . . H36C H 0.0302 0.7148 -0.1833 0.085 Uiso 1 1 calc R . . C37 C 0.20502(17) 0.9693(3) 0.04527(14) 0.0285(8) Uani 1 1 d . . . H37 H 0.2106 1.0263 0.0237 0.034 Uiso 1 1 calc R . . C38 C 0.17507(19) 1.0007(4) 0.07568(16) 0.0351(9) Uani 1 1 d . . . H38 H 0.1606 1.0786 0.0759 0.042 Uiso 1 1 calc R . . C39 C 0.16687(18) 0.9149(4) 0.10589(15) 0.0315(9) Uani 1 1 d . . . H39 H 0.1459 0.9343 0.1269 0.038 Uiso 1 1 calc R . . C40 C 0.21721(14) 0.7829(3) 0.07703(12) 0.0207(7) Uani 1 1 d . . . C41 C 0.24360(14) 0.6657(3) 0.07791(12) 0.0203(7) Uani 1 1 d . . . C42 C 0.26461(18) 0.4821(4) 0.10895(15) 0.0318(9) Uani 1 1 d . . . H42 H 0.2621 0.4230 0.1308 0.038 Uiso 1 1 calc R . . C43 C 0.29451(19) 0.4579(4) 0.07742(15) 0.0334(9) Uani 1 1 d . . . H43 H 0.3127 0.3838 0.0776 0.040 Uiso 1 1 calc R . . C44 C 0.29715(16) 0.5442(4) 0.04581(14) 0.0284(8) Uani 1 1 d . . . H44 H 0.3174 0.5294 0.0238 0.034 Uiso 1 1 calc R . . C46 C 0.3043(2) 0.7759(5) 0.21971(17) 0.0477(13) Uani 1 1 d . . . C47 C 0.3122(2) 0.7298(5) 0.26370(17) 0.0469(12) Uani 1 1 d . B . H47 H 0.3402 0.7616 0.2884 0.056 Uiso 1 1 calc R . . C48 C 0.27926(19) 0.6374(4) 0.27160(15) 0.0351(9) Uani 1 1 d . . . C49 C 0.2910(2) 0.5852(5) 0.31989(18) 0.0500(13) Uani 1 1 d . B . C50 C 0.0077(2) 0.8187(6) 0.1382(2) 0.0550(14) Uani 1 1 d . . . C51 C 0.06794(19) 0.8074(4) 0.16540(17) 0.0358(9) Uani 1 1 d . . . C52 C 0.0853(2) 0.8567(5) 0.2090(2) 0.0493(13) Uani 1 1 d . D . H52 H 0.0595 0.8958 0.2221 0.059 Uiso 1 1 calc R . . C53 C 0.1398(2) 0.8488(5) 0.2330(2) 0.0494(13) Uani 1 1 d D . . C54 C 0.1566(4) 0.9176(9) 0.2792(3) 0.070(3) Uiso 0.377(7) 1 d PDU D 1 F22 F 0.2088(4) 0.9272(11) 0.2998(4) 0.077(3) Uiso 0.377(7) 1 d PDU D 1 F23 F 0.1365(5) 1.0245(11) 0.2757(4) 0.092(3) Uiso 0.377(7) 1 d PDU D 1 F24 F 0.1348(5) 0.8624(12) 0.3081(5) 0.108(3) Uiso 0.377(7) 1 d PDU D 1 C54' C 0.1572(3) 0.8926(6) 0.2838(3) 0.072(2) Uiso 0.623(7) 1 d PDU D 2 F22' F 0.2013(3) 0.9639(7) 0.2873(3) 0.094(2) Uiso 0.623(7) 1 d PDU D 2 F23' F 0.1718(3) 0.8048(7) 0.3150(3) 0.103(3) Uiso 0.623(7) 1 d PDU D 2 F24' F 0.1176(3) 0.9568(7) 0.2956(3) 0.092(2) Uiso 0.623(7) 1 d PDU D 2 C55 C 0.20199(16) 0.2306(4) 0.19107(12) 0.0432(11) Uani 1 1 d D . . C56 C 0.17818(18) 0.3543(4) 0.19465(14) 0.0300(8) Uani 1 1 d . C . C57 C 0.14047(18) 0.3633(4) 0.22135(15) 0.0323(9) Uani 1 1 d . . . H57 H 0.1318 0.2947 0.2365 0.039 Uiso 1 1 calc R C . C58 C 0.11554(16) 0.4705(4) 0.22612(13) 0.0291(8) Uani 1 1 d . C . C59 C 0.07461(19) 0.4738(5) 0.25624(17) 0.0407(11) Uani 1 1 d . . . O3W O 0.4116(7) 0.6477(14) 0.1432(6) 0.127(5) Uiso 0.50 1 d P . . O2W O 0.3865(11) 1.228(2) 0.1737(9) 0.212(10) Uiso 0.50 1 d P . . O1W O 0.3856(11) 0.494(3) 0.2037(9) 0.224(11) Uiso 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 Gd1 0.02399(10) 0.02272(9) 0.02339(9) -0.00187(7) 0.01080(7) -0.00188(7) Ru1 0.01858(13) 0.01730(13) 0.02178(14) 0.00115(10) 0.00769(10) -0.00110(10) P1 0.0539(7) 0.0288(5) 0.0351(6) -0.0014(5) 0.0156(5) -0.0030(5) F1 0.098(3) 0.065(2) 0.093(3) -0.025(2) 0.039(3) -0.042(2) F2 0.104(3) 0.076(3) 0.0367(17) 0.0009(16) 0.0187(19) 0.014(2) F3 0.085(3) 0.0494(19) 0.090(3) 0.0157(18) 0.047(2) 0.0247(18) F4 0.091(3) 0.064(2) 0.0380(16) 0.0086(15) 0.0209(17) 0.0003(19) F5 0.069(2) 0.077(3) 0.071(2) -0.012(2) 0.0159(19) 0.021(2) F6 0.077(2) 0.0385(17) 0.078(2) 0.0094(16) 0.0149(19) -0.0178(16) F9 0.0199(11) 0.0399(14) 0.0561(16) -0.0076(12) 0.0083(11) -0.0051(10) F16 0.058(2) 0.205(6) 0.054(2) 0.056(3) 0.0149(18) -0.007(3) F17 0.078(2) 0.078(3) 0.0344(16) 0.0059(15) -0.0087(16) -0.0234(19) F18 0.130(4) 0.057(2) 0.069(2) 0.020(2) -0.009(3) 0.004(2) F19 0.068(3) 0.144(4) 0.058(2) 0.003(2) 0.0150(19) 0.054(3) F20 0.0328(19) 0.067(3) 0.234(7) -0.019(3) -0.003(3) 0.0019(18) F21 0.0519(18) 0.067(2) 0.073(2) 0.0061(18) 0.0309(17) 0.0313(17) F28 0.0533(18) 0.065(2) 0.0478(17) -0.0016(14) 0.0281(14) -0.0256(15) F29 0.0638(19) 0.066(2) 0.0382(15) -0.0146(14) 0.0295(14) -0.0150(16) F30 0.0423(17) 0.107(3) 0.076(2) 0.033(2) 0.0376(17) 0.0235(19) O1 0.0366(15) 0.0261(14) 0.0306(14) 0.0006(11) 0.0169(12) -0.0001(12) O2 0.0307(15) 0.0345(15) 0.0324(15) -0.0017(12) 0.0144(12) -0.0028(12) O3 0.0303(15) 0.0352(15) 0.0344(15) -0.0030(12) 0.0150(12) 0.0040(12) O4 0.0393(18) 0.0377(17) 0.0465(19) -0.0176(15) 0.0114(15) -0.0064(14) O5 0.0347(16) 0.062(2) 0.0282(15) 0.0011(14) 0.0082(13) -0.0194(16) O6 0.0349(16) 0.0359(16) 0.0338(16) 0.0026(13) 0.0034(13) -0.0064(13) O7 0.0290(15) 0.0405(17) 0.0342(15) -0.0120(13) 0.0062(12) 0.0002(13) O8 0.085(4) 0.106(4) 0.054(3) -0.002(3) -0.001(2) 0.042(3) N1 0.0220(14) 0.0207(14) 0.0206(14) -0.0004(11) 0.0082(11) -0.0030(11) N2 0.0194(14) 0.0217(14) 0.0217(14) -0.0005(11) 0.0056(11) -0.0037(11) N3 0.0209(14) 0.0193(14) 0.0239(14) -0.0001(11) 0.0077(12) -0.0043(11) N4 0.0199(14) 0.0187(14) 0.0287(16) 0.0006(12) 0.0104(12) -0.0034(11) N5 0.0217(15) 0.0188(14) 0.0263(15) 0.0003(11) 0.0078(12) 0.0000(11) N6 0.0180(14) 0.0195(14) 0.0261(15) 0.0027(11) 0.0092(12) 0.0017(11) N7 0.0258(16) 0.0220(15) 0.0283(16) -0.0029(12) 0.0110(13) 0.0006(12) N8 0.0256(15) 0.0216(15) 0.0262(15) 0.0036(12) 0.0113(12) 0.0020(12) C1 0.0267(18) 0.0269(18) 0.0245(18) -0.0033(15) 0.0079(14) 0.0002(15) C2 0.034(2) 0.0251(18) 0.0238(18) -0.0058(14) 0.0067(15) -0.0025(16) C3 0.0255(18) 0.0212(17) 0.0230(17) 0.0012(14) 0.0033(14) -0.0011(14) C4 0.0201(17) 0.0244(17) 0.0245(17) -0.0028(14) 0.0044(14) -0.0012(14) C5 0.0229(17) 0.0173(16) 0.0214(16) 0.0005(13) 0.0055(13) -0.0006(13) C6 0.0202(16) 0.0186(16) 0.0228(16) 0.0001(13) 0.0047(13) -0.0028(13) C7 0.0185(16) 0.0232(17) 0.0262(18) -0.0025(14) 0.0064(14) -0.0040(13) C8 0.0229(17) 0.0208(16) 0.0243(17) -0.0013(13) 0.0096(14) -0.0018(13) C9 0.0235(18) 0.0268(19) 0.0285(18) -0.0077(15) 0.0076(15) -0.0061(15) C10 0.0199(17) 0.0246(18) 0.0275(18) -0.0046(14) 0.0059(14) -0.0061(14) C11 0.0267(19) 0.0245(18) 0.0279(19) -0.0055(15) 0.0011(15) -0.0031(15) C12 0.037(2) 0.044(3) 0.033(2) -0.0123(19) 0.0036(18) -0.010(2) C13 0.028(2) 0.041(2) 0.037(2) -0.0057(19) 0.0077(17) -0.0094(18) C14 0.035(2) 0.033(2) 0.060(3) -0.007(2) -0.014(2) 0.0033(19) C15 0.0247(18) 0.0249(18) 0.0290(19) -0.0061(15) 0.0092(15) -0.0012(14) C16 0.032(2) 0.040(2) 0.035(2) 0.0003(18) 0.0161(18) -0.0019(18) C17 0.030(2) 0.0253(19) 0.037(2) -0.0048(16) 0.0076(17) 0.0029(15) C18 0.035(2) 0.039(2) 0.035(2) -0.0147(18) 0.0122(18) -0.0004(18) C19 0.0205(17) 0.0240(18) 0.0302(19) 0.0023(15) 0.0047(14) -0.0064(14) C20 0.0262(19) 0.0236(18) 0.034(2) 0.0040(15) 0.0065(16) -0.0081(15) C21 0.0298(19) 0.0207(17) 0.0249(18) 0.0012(14) 0.0062(15) -0.0054(14) C22 0.0237(17) 0.0241(18) 0.0258(18) 0.0020(14) 0.0072(14) -0.0036(14) C23 0.0205(16) 0.0224(17) 0.0217(16) 0.0001(13) 0.0077(13) -0.0035(13) C24 0.0224(17) 0.0234(17) 0.0240(17) 0.0014(13) 0.0096(14) -0.0039(14) C25 0.0239(18) 0.033(2) 0.0284(19) 0.0057(16) 0.0039(15) -0.0076(16) C26 0.0246(19) 0.038(2) 0.034(2) 0.0031(17) 0.0052(16) -0.0140(17) C27 0.030(2) 0.032(2) 0.037(2) 0.0007(17) 0.0089(17) -0.0144(17) C28 0.0254(19) 0.0221(18) 0.037(2) 0.0033(15) 0.0116(16) -0.0053(14) C29 0.031(2) 0.0246(19) 0.041(2) 0.0121(17) 0.0066(17) -0.0016(16) C30 0.043(3) 0.024(2) 0.064(3) 0.000(2) 0.010(2) -0.0031(18) C31 0.067(4) 0.046(3) 0.049(3) 0.025(2) 0.025(3) 0.010(3) C32 0.038(3) 0.032(2) 0.063(3) 0.016(2) -0.003(2) 0.0003(19) C33 0.029(2) 0.059(3) 0.047(3) 0.017(2) -0.002(2) -0.022(2) C34 0.026(2) 0.101(5) 0.078(4) 0.011(4) 0.014(3) 0.001(3) C35 0.048(3) 0.076(4) 0.090(5) 0.025(4) -0.013(3) -0.039(3) C36 0.040(3) 0.074(4) 0.046(3) 0.016(3) -0.008(2) -0.026(3) C37 0.034(2) 0.0214(17) 0.032(2) 0.0029(15) 0.0133(16) 0.0026(15) C38 0.044(2) 0.0216(18) 0.045(2) 0.0005(17) 0.021(2) 0.0071(17) C39 0.039(2) 0.0240(19) 0.038(2) -0.0033(16) 0.0206(18) 0.0042(16) C40 0.0192(16) 0.0178(15) 0.0251(17) -0.0004(13) 0.0056(13) 0.0003(13) C41 0.0188(16) 0.0197(16) 0.0230(16) -0.0004(13) 0.0063(13) -0.0015(13) C42 0.038(2) 0.0263(19) 0.036(2) 0.0103(16) 0.0184(18) 0.0091(17) C43 0.044(2) 0.0220(18) 0.042(2) 0.0084(17) 0.025(2) 0.0116(17) C44 0.0287(19) 0.0263(19) 0.035(2) 0.0055(16) 0.0180(16) 0.0082(15) C46 0.042(3) 0.066(3) 0.035(2) -0.001(2) 0.011(2) -0.025(2) C47 0.041(3) 0.063(3) 0.034(2) -0.002(2) 0.005(2) -0.020(2) C48 0.032(2) 0.041(2) 0.032(2) 0.0014(18) 0.0074(17) -0.0028(18) C49 0.047(3) 0.060(3) 0.038(3) 0.011(2) 0.002(2) -0.012(3) C50 0.041(3) 0.058(3) 0.071(4) -0.008(3) 0.022(3) 0.017(3) C51 0.035(2) 0.031(2) 0.048(3) -0.0033(19) 0.021(2) 0.0032(17) C52 0.045(3) 0.046(3) 0.064(3) -0.024(2) 0.027(3) 0.002(2) C53 0.056(3) 0.043(3) 0.054(3) -0.024(2) 0.022(3) -0.005(2) C55 0.056(3) 0.029(2) 0.048(3) 0.007(2) 0.021(2) 0.001(2) C56 0.034(2) 0.0257(19) 0.030(2) -0.0024(15) 0.0086(16) -0.0030(16) C57 0.032(2) 0.036(2) 0.030(2) 0.0050(16) 0.0100(17) -0.0070(17) C58 0.0249(18) 0.041(2) 0.0218(17) -0.0007(16) 0.0071(14) -0.0105(16) C59 0.034(2) 0.055(3) 0.039(2) 0.004(2) 0.0195(19) -0.005(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 Gd1 O2 2.357(3) . ? Gd1 O4 2.385(3) . ? Gd1 O1 2.389(3) . ? Gd1 O5 2.395(3) . ? Gd1 O7 2.406(3) . ? Gd1 O3 2.405(3) . ? Gd1 O6 2.413(3) . ? Gd1 N7 2.633(3) . ? Gd1 N8 2.644(3) . ? Ru1 N3 2.044(3) . ? Ru1 N2 2.045(3) . ? Ru1 N5 2.056(3) . ? Ru1 N1 2.061(3) . ? Ru1 N4 2.062(3) . ? Ru1 N6 2.061(3) . ? P1 F3 1.569(4) . ? P1 F2 1.580(4) . ? P1 F1 1.582(4) . ? P1 F6 1.592(3) . ? P1 F4 1.598(3) . ? P1 F5 1.611(4) . ? F9 P2' 1.584(3) . ? F9 P2 1.622(3) . ? P2 F10 1.584(4) . ? P2 F7 1.588(4) . ? P2 F12 1.597(4) . ? P2 F11 1.601(3) . ? P2 F8 1.610(4) . ? P2' F8' 1.584(4) . ? P2' F12' 1.590(4) . ? P2' F7' 1.598(4) . ? P2' F11' 1.599(4) . ? P2' F10' 1.599(4) . ? C45 F15 1.323(9) . ? C45 F13 1.324(9) . ? C45 F14 1.336(9) . ? C45 C46 1.576(18) . ? C45' F13' 1.342(11) . ? C45' F14' 1.344(11) . ? C45' F15' 1.344(11) . ? C45' C46 1.57(2) . ? F16 C49 1.291(7) . ? F17 C49 1.332(6) . ? F18 C49 1.336(7) . ? F19 C50 1.339(8) . ? F20 C50 1.293(8) . ? F21 C50 1.330(6) . ? F25 C55 1.330(6) . ? F26 C55 1.325(6) . ? F27 C55 1.348(6) . ? F25' C55 1.357(6) . ? F26' C55 1.340(6) . ? F27' C55 1.325(6) . ? F28 C59 1.333(6) . ? F29 C59 1.341(6) . ? F30 C59 1.310(6) . ? O1 C56 1.247(5) . ? O2 C58 1.241(5) . ? O3 C51 1.253(5) . ? O4 C53 1.252(6) . ? O5 C46 1.244(6) . ? O6 C48 1.250(5) . ? N1 C1 1.338(5) . ? N1 C5 1.365(5) . ? N2 C10 1.340(5) . ? N2 C6 1.367(5) . ? N3 C19 1.345(5) . ? N3 C23 1.360(5) . ? N4 C28 1.350(5) . ? N4 C24 1.361(5) . ? N5 C37 1.349(5) . ? N5 C40 1.353(5) . ? N6 C44 1.347(5) . ? N6 C41 1.357(5) . ? N7 C40 1.325(5) . ? N7 C39 1.337(5) . ? N8 C41 1.333(5) . ? N8 C42 1.337(5) . ? C1 C2 1.381(5) . ? C1 H1 0.9500 . ? C2 C3 1.387(6) . ? C2 H2 0.9500 . ? C3 C4 1.403(5) . ? C3 C11 1.534(5) . ? C4 C5 1.385(5) . ? C4 H4 0.9500 . ? C5 C6 1.476(5) . ? C6 C7 1.385(5) . ? C7 C8 1.395(5) . ? C7 H7 0.9500 . ? C8 C9 1.395(5) . ? C8 C15 1.527(5) . ? C9 C10 1.377(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C14 1.529(6) . ? C11 C13 1.535(6) . ? C11 C12 1.532(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C18 1.531(6) . ? C15 C16 1.532(6) . ? C15 C17 1.540(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.377(5) . ? C19 H19 0.9500 . ? C20 C21 1.395(6) . ? C20 H20 0.9500 . ? C21 C22 1.392(5) . ? C21 C29 1.527(5) . ? C22 C23 1.385(5) . ? C22 H22 0.9500 . ? C23 C24 1.479(5) . ? C24 C25 1.387(5) . ? C25 C26 1.401(5) . ? C25 H25 0.9500 . ? C26 C27 1.377(6) . ? C26 C33 1.535(6) . ? C27 C28 1.378(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C32 1.528(6) . ? C29 C31 1.536(7) . ? C29 C30 1.538(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C36 1.513(7) . ? C33 C35 1.513(8) . ? C33 C34 1.557(9) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.376(6) . ? C37 H37 0.9500 . ? C38 C39 1.380(6) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.473(5) . ? C42 C43 1.385(6) . ? C42 H42 0.9500 . ? C43 C44 1.375(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C46 C47 1.389(7) . ? C47 C48 1.389(7) . ? C47 H47 0.9500 . ? C48 C49 1.525(7) . ? C50 C51 1.525(7) . ? C51 C52 1.386(7) . ? C52 C53 1.374(8) . ? C52 H52 0.9500 . ? C53 C54 1.552(10) . ? C53 C54' 1.558(10) . ? C54 F23 1.298(9) . ? C54 F22 1.299(9) . ? C54 F24 1.302(9) . ? C54' F23' 1.347(7) . ? C54' F22' 1.350(7) . ? C54' F24' 1.352(7) . ? C55 C56 1.530(6) . ? C56 C57 1.399(6) . ? C57 C58 1.385(6) . ? C57 H57 0.9500 . ? C58 C59 1.541(6) . ? 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 O2 Gd1 O4 77.14(11) . . ? O2 Gd1 O1 72.73(10) . . ? O4 Gd1 O1 136.20(11) . . ? O2 Gd1 O5 139.11(10) . . ? O4 Gd1 O5 73.27(12) . . ? O1 Gd1 O5 111.69(12) . . ? O2 Gd1 O7 86.19(11) . . ? O4 Gd1 O7 137.07(11) . . ? O1 Gd1 O7 71.72(11) . . ? O5 Gd1 O7 134.53(11) . . ? O2 Gd1 O3 71.77(10) . . ? O4 Gd1 O3 69.64(11) . . ? O1 Gd1 O3 126.78(10) . . ? O5 Gd1 O3 121.18(12) . . ? O7 Gd1 O3 67.60(10) . . ? O2 Gd1 O6 74.33(10) . . ? O4 Gd1 O6 71.98(12) . . ? O1 Gd1 O6 69.76(10) . . ? O5 Gd1 O6 70.10(11) . . ? O7 Gd1 O6 140.46(11) . . ? O3 Gd1 O6 133.12(11) . . ? O2 Gd1 N7 141.17(10) . . ? O4 Gd1 N7 89.37(12) . . ? O1 Gd1 N7 133.49(9) . . ? O5 Gd1 N7 66.20(11) . . ? O7 Gd1 N7 79.30(11) . . ? O3 Gd1 N7 69.39(10) . . ? O6 Gd1 N7 135.82(10) . . ? O2 Gd1 N8 142.99(10) . . ? O4 Gd1 N8 139.05(11) . . ? O1 Gd1 N8 72.79(9) . . ? O5 Gd1 N8 67.95(11) . . ? O7 Gd1 N8 70.57(10) . . ? O3 Gd1 N8 121.03(10) . . ? O6 Gd1 N8 105.55(10) . . ? N7 Gd1 N8 63.50(10) . . ? N3 Ru1 N2 90.68(12) . . ? N3 Ru1 N5 94.34(12) . . ? N2 Ru1 N5 174.14(12) . . ? N3 Ru1 N1 95.88(12) . . ? N2 Ru1 N1 78.26(12) . . ? N5 Ru1 N1 98.18(12) . . ? N3 Ru1 N4 78.10(12) . . ? N2 Ru1 N4 98.64(12) . . ? N5 Ru1 N4 85.38(12) . . ? N1 Ru1 N4 173.28(12) . . ? N3 Ru1 N6 171.82(12) . . ? N2 Ru1 N6 96.19(12) . . ? N5 Ru1 N6 79.05(12) . . ? N1 Ru1 N6 89.88(12) . . ? N4 Ru1 N6 96.42(12) . . ? F3 P1 F2 91.8(2) . . ? F3 P1 F1 90.8(2) . . ? F2 P1 F1 91.3(2) . . ? F3 P1 F6 91.2(2) . . ? F2 P1 F6 90.1(2) . . ? F1 P1 F6 177.6(2) . . ? F3 P1 F4 90.9(2) . . ? F2 P1 F4 177.1(2) . . ? F1 P1 F4 89.5(2) . . ? F6 P1 F4 89.0(2) . . ? F3 P1 F5 179.0(2) . . ? F2 P1 F5 89.1(2) . . ? F1 P1 F5 89.6(2) . . ? F6 P1 F5 88.4(2) . . ? F4 P1 F5 88.1(2) . . ? P2' F9 P2 12.69(11) . . ? F10 P2 F7 82.4(3) . . ? F10 P2 F12 91.6(3) . . ? F7 P2 F12 172.8(4) . . ? F10 P2 F11 91.6(3) . . ? F7 P2 F11 84.7(3) . . ? F12 P2 F11 91.7(3) . . ? F10 P2 F8 179.0(3) . . ? F7 P2 F8 97.7(4) . . ? F12 P2 F8 88.4(4) . . ? F11 P2 F8 89.4(3) . . ? F10 P2 F9 91.3(3) . . ? F7 P2 F9 92.4(3) . . ? F12 P2 F9 91.6(2) . . ? F11 P2 F9 175.6(3) . . ? F8 P2 F9 87.7(3) . . ? F8' P2' F9 92.5(3) . . ? F8' P2' F12' 92.5(4) . . ? F9 P2' F12' 88.5(3) . . ? F8' P2' F7' 80.3(4) . . ? F9 P2' F7' 87.3(3) . . ? F12' P2' F7' 171.4(4) . . ? F8' P2' F11' 90.2(3) . . ? F9 P2' F11' 177.0(3) . . ? F12' P2' F11' 90.2(3) . . ? F7' P2' F11' 94.4(3) . . ? F8' P2' F10' 179.4(4) . . ? F9 P2' F10' 87.6(3) . . ? F12' P2' F10' 88.1(4) . . ? F7' P2' F10' 99.2(4) . . ? F11' P2' F10' 89.6(4) . . ? F15 C45 F13 108.5(8) . . ? F15 C45 F14 108.9(8) . . ? F13 C45 F14 107.3(8) . . ? F15 C45 C46 112.7(10) . . ? F13 C45 C46 109.2(9) . . ? F14 C45 C46 110.1(9) . . ? F13' C45' F14' 108.9(11) . . ? F13' C45' F15' 107.6(10) . . ? F14' C45' F15' 107.6(10) . . ? F13' C45' C46 108.8(12) . . ? F14' C45' C46 112.5(11) . . ? F15' C45' C46 111.3(12) . . ? C56 O1 Gd1 133.5(3) . . ? C58 O2 Gd1 134.6(3) . . ? C51 O3 Gd1 133.5(3) . . ? C53 O4 Gd1 132.2(3) . . ? C46 O5 Gd1 133.6(3) . . ? C48 O6 Gd1 133.6(3) . . ? C1 N1 C5 117.7(3) . . ? C1 N1 Ru1 125.6(3) . . ? C5 N1 Ru1 116.6(2) . . ? C10 N2 C6 117.6(3) . . ? C10 N2 Ru1 125.4(2) . . ? C6 N2 Ru1 116.9(2) . . ? C19 N3 C23 117.8(3) . . ? C19 N3 Ru1 125.5(3) . . ? C23 N3 Ru1 116.5(2) . . ? C28 N4 C24 117.5(3) . . ? C28 N4 Ru1 126.6(3) . . ? C24 N4 Ru1 115.5(2) . . ? C37 N5 C40 116.2(3) . . ? C37 N5 Ru1 128.3(3) . . ? C40 N5 Ru1 115.4(2) . . ? C44 N6 C41 116.8(3) . . ? C44 N6 Ru1 128.1(3) . . ? C41 N6 Ru1 115.1(2) . . ? C40 N7 C39 116.8(3) . . ? C40 N7 Gd1 119.2(2) . . ? C39 N7 Gd1 123.5(3) . . ? C41 N8 C42 116.8(3) . . ? C41 N8 Gd1 118.4(2) . . ? C42 N8 Gd1 124.8(2) . . ? N1 C1 C2 123.3(4) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 120.3(3) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C2 C3 C4 116.4(3) . . ? C2 C3 C11 122.3(3) . . ? C4 C3 C11 121.3(3) . . ? C5 C4 C3 120.9(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? N1 C5 C4 121.4(3) . . ? N1 C5 C6 113.9(3) . . ? C4 C5 C6 124.7(3) . . ? N2 C6 C7 121.2(3) . . ? N2 C6 C5 114.3(3) . . ? C7 C6 C5 124.6(3) . . ? C6 C7 C8 121.2(3) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C7 C8 C9 116.3(3) . . ? C7 C8 C15 120.7(3) . . ? C9 C8 C15 122.9(3) . . ? C10 C9 C8 120.2(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? N2 C10 C9 123.4(3) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? C14 C11 C13 109.5(4) . . ? C14 C11 C12 108.9(4) . . ? C13 C11 C12 108.5(3) . . ? C14 C11 C3 109.3(3) . . ? C13 C11 C3 108.8(3) . . ? C12 C11 C3 111.8(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C8 C15 C18 111.4(3) . . ? C8 C15 C16 108.0(3) . . ? C18 C15 C16 109.8(3) . . ? C8 C15 C17 109.2(3) . . ? C18 C15 C17 108.7(3) . . ? C16 C15 C17 109.7(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 122.4(3) . . ? N3 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 C21 120.8(3) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 116.3(3) . . ? C22 C21 C29 124.2(4) . . ? C20 C21 C29 119.5(3) . . ? C23 C22 C21 120.7(3) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? N3 C23 C22 121.8(3) . . ? N3 C23 C24 113.7(3) . . ? C22 C23 C24 124.5(3) . . ? N4 C24 C25 121.4(3) . . ? N4 C24 C23 114.3(3) . . ? C25 C24 C23 124.2(3) . . ? C24 C25 C26 120.7(4) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 116.7(4) . . ? C27 C26 C33 123.3(4) . . ? C25 C26 C33 120.0(4) . . ? C26 C27 C28 120.6(4) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? N4 C28 C27 122.9(4) . . ? N4 C28 H28 118.5 . . ? C27 C28 H28 118.5 . . ? C21 C29 C32 111.5(3) . . ? C21 C29 C31 108.4(4) . . ? C32 C29 C31 110.2(4) . . ? C21 C29 C30 109.0(4) . . ? C32 C29 C30 107.6(4) . . ? C31 C29 C30 110.0(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C33 C35 111.1(5) . . ? C36 C33 C26 110.0(4) . . ? C35 C33 C26 111.8(5) . . ? C36 C33 C34 108.2(5) . . ? C35 C33 C34 108.7(5) . . ? C26 C33 C34 107.0(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 C38 121.5(4) . . ? N5 C37 H37 119.2 . . ? C38 C37 H37 119.2 . . ? C37 C38 C39 117.6(4) . . ? C37 C38 H38 121.2 . . ? C39 C38 H38 121.2 . . ? N7 C39 C38 122.0(4) . . ? N7 C39 H39 119.0 . . ? C38 C39 H39 119.0 . . ? N7 C40 N5 125.8(3) . . ? N7 C40 C41 119.2(3) . . ? N5 C40 C41 115.0(3) . . ? N8 C41 N6 125.4(3) . . ? N8 C41 C40 119.5(3) . . ? N6 C41 C40 115.1(3) . . ? N8 C42 C43 121.8(4) . . ? N8 C42 H42 119.1 . . ? C43 C42 H42 119.1 . . ? C44 C43 C42 118.1(4) . . ? C44 C43 H43 120.9 . . ? C42 C43 H43 120.9 . . ? N6 C44 C43 121.0(4) . . ? N6 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? O5 C46 C47 128.5(5) . . ? O5 C46 C45' 110.5(5) . . ? C47 C46 C45' 120.8(5) . . ? O5 C46 C45 116.9(4) . . ? C47 C46 C45 114.4(4) . . ? C45' C46 C45 13.5(4) . . ? C48 C47 C46 120.1(4) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? O6 C48 C47 127.8(4) . . ? O6 C48 C49 113.7(4) . . ? C47 C48 C49 118.6(4) . . ? F16 C49 F17 108.5(5) . . ? F16 C49 F18 106.4(5) . . ? F17 C49 F18 104.5(5) . . ? F16 C49 C48 112.2(4) . . ? F17 C49 C48 113.9(4) . . ? F18 C49 C48 110.6(5) . . ? F20 C50 F21 109.9(5) . . ? F20 C50 F19 105.8(6) . . ? F21 C50 F19 104.1(5) . . ? F20 C50 C51 111.1(5) . . ? F21 C50 C51 114.2(5) . . ? F19 C50 C51 111.3(5) . . ? O3 C51 C52 127.1(5) . . ? O3 C51 C50 113.2(4) . . ? C52 C51 C50 119.7(4) . . ? C53 C52 C51 119.7(4) . . ? C53 C52 H52 120.2 . . ? C51 C52 H52 120.2 . . ? O4 C53 C52 129.2(5) . . ? O4 C53 C54 114.5(6) . . ? C52 C53 C54 116.1(5) . . ? O4 C53 C54' 111.7(5) . . ? C52 C53 C54' 118.8(5) . . ? C54 C53 C54' 11.6(4) . . ? F23 C54 F22 106.5(6) . . ? F23 C54 F24 105.9(6) . . ? F22 C54 F24 105.6(6) . . ? F23 C54 C53 112.4(9) . . ? F22 C54 C53 118.2(10) . . ? F24 C54 C53 107.4(10) . . ? F23' C54' F22' 108.3(5) . . ? F23' C54' F24' 107.0(5) . . ? F22' C54' F24' 107.9(5) . . ? F23' C54' C53 114.2(7) . . ? F22' C54' C53 106.1(7) . . ? F24' C54' C53 113.1(6) . . ? F27' C55 F26 124.3(5) . . ? F27' C55 F25 72.3(4) . . ? F26 C55 F25 107.2(4) . . ? F27' C55 F26' 107.4(4) . . ? F26 C55 F26' 25.1(3) . . ? F25 C55 F26' 123.0(6) . . ? F27' C55 F27 34.1(3) . . ? F26 C55 F27 105.9(4) . . ? F25 C55 F27 105.2(4) . . ? F26' C55 F27 82.4(4) . . ? F27' C55 F25' 105.7(4) . . ? F26 C55 F25' 81.9(4) . . ? F25 C55 F25' 34.4(4) . . ? F26' C55 F25' 104.9(4) . . ? F27 C55 F25' 135.8(5) . . ? F27' C55 C56 115.5(5) . . ? F26 C55 C56 113.2(4) . . ? F25 C55 C56 117.1(5) . . ? F26' C55 C56 113.6(4) . . ? F27 C55 C56 107.3(5) . . ? F25' C55 C56 109.0(5) . . ? O1 C56 C57 128.3(4) . . ? O1 C56 C55 115.4(4) . . ? C57 C56 C55 116.3(4) . . ? C58 C57 C56 121.0(4) . . ? C58 C57 H57 119.5 . . ? C56 C57 H57 119.5 . . ? O2 C58 C57 128.7(4) . . ? O2 C58 C59 113.1(4) . . ? C57 C58 C59 118.2(4) . . ? F30 C59 F28 107.8(4) . . ? F30 C59 F29 107.8(4) . . ? F28 C59 F29 106.3(4) . . ? F30 C59 C58 112.0(4) . . ? F28 C59 C58 113.1(4) . . ? F29 C59 C58 109.6(4) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.500 _refine_diff_density_min -1.256 _refine_diff_density_rms 0.144 #===END data_imw661 _database_code_depnum_ccdc_archive 'CCDC 661956' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H65 F30 N8 Nd O10 Os P2' _chemical_formula_weight 2012.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 25.213(2) _cell_length_b 11.2690(10) _cell_length_c 30.304(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.428(5) _cell_angle_gamma 90.00 _cell_volume 8299.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8641 _cell_measurement_theta_min 4.565 _cell_measurement_theta_max 54.582 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3964 _exptl_absorpt_coefficient_mu 2.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4589 _exptl_absorpt_correction_T_max 0.9340 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 173473 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.59 _reflns_number_total 19136 _reflns_number_gt 14687 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+57.6499P] 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 SHELXL _refine_ls_extinction_coef 0.00030(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 19136 _refine_ls_number_parameters 1005 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1606 _refine_ls_wR_factor_gt 0.1459 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.002 _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 Nd1 Nd 0.184076(16) 0.35859(3) 0.671862(13) 0.02875(10) Uani 1 1 d . . . Os1 Os 0.269950(10) 0.21236(2) 0.503575(8) 0.02185(8) Uani 1 1 d . . . P1 P 0.39763(18) 0.7186(4) 0.5151(2) 0.0247(10) Uiso 0.483(10) 1 d PU A 1 F1 F 0.3990(4) 0.5802(9) 0.5230(4) 0.044(2) Uiso 0.483(10) 1 d PU A 1 F2 F 0.3343(4) 0.7217(9) 0.5168(4) 0.037(2) Uiso 0.483(10) 1 d PU A 1 F3 F 0.3799(4) 0.7072(9) 0.4623(4) 0.038(2) Uiso 0.483(10) 1 d PU A 1 F4 F 0.4598(5) 0.7113(10) 0.5120(4) 0.027(2) Uiso 0.483(10) 1 d PU A 1 F5 F 0.4164(5) 0.7315(12) 0.5707(4) 0.055(2) Uiso 0.483(10) 1 d PU A 1 F6 F 0.3987(4) 0.8585(9) 0.5009(4) 0.033(2) Uiso 0.483(10) 1 d PU A 1 P1' P 0.40097(17) 0.7351(4) 0.52698(19) 0.0243(10) Uiso 0.517(10) 1 d PU A 2 F1' F 0.4013(4) 0.6052(9) 0.5469(4) 0.047(2) Uiso 0.517(10) 1 d PU A 2 F2' F 0.3406(4) 0.7604(9) 0.5322(3) 0.039(2) Uiso 0.517(10) 1 d PU A 2 F3' F 0.3730(5) 0.6804(10) 0.4752(4) 0.052(3) Uiso 0.517(10) 1 d PU A 2 F4' F 0.4617(5) 0.7173(11) 0.5224(4) 0.035(3) Uiso 0.517(10) 1 d PU A 2 F5' F 0.4277(4) 0.7849(10) 0.5746(3) 0.044(2) Uiso 0.517(10) 1 d PU A 2 F6' F 0.3996(4) 0.8666(9) 0.5142(4) 0.038(2) Uiso 0.517(10) 1 d PU A 2 P2 P 0.12453(12) 0.6861(2) 0.51527(8) 0.0508(6) Uani 1 1 d . . . F7 F 0.1616(3) 0.5716(5) 0.5230(3) 0.087(2) Uani 1 1 d . . . F8 F 0.0736(3) 0.6005(7) 0.5173(3) 0.095(2) Uani 1 1 d . . . F9 F 0.1363(3) 0.6997(6) 0.5687(2) 0.088(2) Uani 1 1 d . . . F10 F 0.1737(3) 0.7670(6) 0.5141(3) 0.096(2) Uani 1 1 d . . . F11 F 0.1094(3) 0.6659(7) 0.4622(2) 0.095(2) Uani 1 1 d . . . F12 F 0.0857(4) 0.7973(7) 0.5100(3) 0.125(3) Uani 1 1 d . . . F13 F 0.2195(5) 0.7893(9) 0.6562(3) 0.053(3) Uiso 0.502(14) 1 d PDU B 1 F14 F 0.2410(4) 0.7979(11) 0.7293(3) 0.072(3) Uiso 0.502(14) 1 d PDU B 1 F15 F 0.1646(5) 0.8702(10) 0.6903(5) 0.084(3) Uiso 0.502(14) 1 d PDU B 1 F13' F 0.2380(4) 0.7826(9) 0.6701(4) 0.054(3) Uiso 0.498(14) 1 d PDU B 2 F14' F 0.2178(5) 0.8369(11) 0.7314(3) 0.077(3) Uiso 0.498(14) 1 d PDU B 2 F15' F 0.1570(4) 0.8447(11) 0.6672(4) 0.074(3) Uiso 0.498(14) 1 d PDU B 2 F16 F 0.0312(2) 0.4672(7) 0.7400(2) 0.083(2) Uani 1 1 d . B . F17 F 0.0564(2) 0.6391(5) 0.76619(19) 0.0652(16) Uani 1 1 d . B . F18 F 0.0997(2) 0.4869(5) 0.79934(17) 0.0612(14) Uani 1 1 d . B . F19 F 0.2483(3) 0.4054(9) 0.8392(2) 0.111(3) Uani 1 1 d . . . F20 F 0.3082(3) 0.5214(6) 0.8264(2) 0.095(2) Uani 1 1 d . . . F21 F 0.3328(3) 0.3529(6) 0.85491(18) 0.0714(17) Uani 1 1 d . . . F22 F 0.3510(4) 0.1105(8) 0.6794(2) 0.131(4) Uani 1 1 d . . . F23 F 0.3171(5) 0.0144(7) 0.7246(5) 0.164(5) Uani 1 1 d . . . F24 F 0.3878(4) 0.1074(9) 0.7483(3) 0.125(4) Uani 1 1 d . . . F25 F 0.0069(4) 0.1340(13) 0.5967(3) 0.164(5) Uani 1 1 d . . . F26 F -0.0189(3) 0.0969(6) 0.6547(2) 0.0803(19) Uani 1 1 d . . . F27 F -0.0160(3) 0.2747(8) 0.6362(6) 0.218(9) Uani 1 1 d . . . C59 C 0.1571(4) 0.1029(10) 0.7863(5) 0.081(4) Uiso 0.570(11) 1 d PDU C 1 F28 F 0.2000(5) 0.0324(12) 0.7882(5) 0.099(4) Uiso 0.570(11) 1 d PDU C 1 F29 F 0.1727(6) 0.1869(10) 0.8179(5) 0.109(4) Uiso 0.570(11) 1 d PDU C 1 F30 F 0.1181(5) 0.0387(12) 0.7971(5) 0.099(3) Uiso 0.570(11) 1 d PDU C 1 C59' C 0.1579(5) 0.0799(12) 0.7822(5) 0.082(4) Uiso 0.430(11) 1 d PDU C 2 F28' F 0.2114(5) 0.0634(15) 0.8008(6) 0.092(4) Uiso 0.430(11) 1 d PDU C 2 F29' F 0.1387(7) 0.1462(15) 0.8108(6) 0.111(4) Uiso 0.430(11) 1 d PDU C 2 F30' F 0.1331(6) -0.0251(13) 0.7784(6) 0.091(4) Uiso 0.430(11) 1 d PDU C 2 O1 O 0.1949(2) 0.5736(4) 0.67646(17) 0.0365(11) Uani 1 1 d . . . O2 O 0.1224(2) 0.4370(5) 0.71306(17) 0.0377(12) Uani 1 1 d . . . O3 O 0.2431(2) 0.4133(5) 0.74751(18) 0.0411(12) Uani 1 1 d . . . O4 O 0.2719(2) 0.2525(5) 0.68799(18) 0.0452(14) Uani 1 1 d . . . O5 O 0.0972(2) 0.2496(5) 0.64711(18) 0.0402(12) Uani 1 1 d . . . O6 O 0.1791(2) 0.1987(5) 0.7250(2) 0.0468(14) Uani 1 1 d . C . O7 O 0.1205(2) 0.4454(5) 0.60270(19) 0.0443(13) Uani 1 1 d . . . N1 N 0.3163(2) 0.2905(4) 0.46527(18) 0.0238(11) Uani 1 1 d . . . N2 N 0.3490(2) 0.1629(4) 0.53837(17) 0.0229(11) Uani 1 1 d . . . N3 N 0.2549(2) 0.0685(5) 0.46046(17) 0.0232(11) Uani 1 1 d . . . N4 N 0.1926(2) 0.2494(5) 0.46172(19) 0.0261(11) Uani 1 1 d . D . N5 N 0.2730(2) 0.3517(5) 0.54781(18) 0.0236(11) Uani 1 1 d . . . N6 N 0.2290(2) 0.1440(5) 0.54757(18) 0.0240(11) Uani 1 1 d . . . N7 N 0.1896(2) 0.1963(5) 0.6087(2) 0.0291(12) Uani 1 1 d . . . N8 N 0.2407(2) 0.4168(5) 0.61108(19) 0.0276(12) Uani 1 1 d . . . C1 C 0.2965(3) 0.3561(6) 0.4277(2) 0.0287(14) Uani 1 1 d . . . H1 H 0.2577 0.3655 0.4169 0.034 Uiso 1 1 calc R . . C2 C 0.3292(3) 0.4106(6) 0.4038(2) 0.0284(14) Uani 1 1 d . . . H2 H 0.3128 0.4573 0.3776 0.034 Uiso 1 1 calc R . . C3 C 0.3860(3) 0.3974(5) 0.4179(2) 0.0235(13) Uani 1 1 d . . . C4 C 0.4067(3) 0.3271(6) 0.4569(2) 0.0247(13) Uani 1 1 d . . . H4 H 0.4453 0.3153 0.4678 0.030 Uiso 1 1 calc R . . C5 C 0.3719(3) 0.2745(5) 0.4797(2) 0.0218(12) Uani 1 1 d . . . C6 C 0.3906(3) 0.2005(5) 0.5212(2) 0.0222(12) Uani 1 1 d . . . C7 C 0.4441(3) 0.1680(6) 0.5406(2) 0.0268(13) Uani 1 1 d . . . H7 H 0.4722 0.1958 0.5276 0.032 Uiso 1 1 calc R . . C8 C 0.4584(3) 0.0944(6) 0.5793(2) 0.0258(13) Uani 1 1 d . . . C9 C 0.4152(3) 0.0585(6) 0.5965(2) 0.0301(14) Uani 1 1 d . . . H9 H 0.4223 0.0093 0.6229 0.036 Uiso 1 1 calc R . . C10 C 0.3616(3) 0.0940(6) 0.5754(2) 0.0290(14) Uani 1 1 d . . . H10 H 0.3328 0.0681 0.5880 0.035 Uiso 1 1 calc R . . C11 C 0.4251(3) 0.4534(6) 0.3924(2) 0.0291(14) Uani 1 1 d . . . C12 C 0.3932(3) 0.5371(7) 0.3543(3) 0.0383(17) Uani 1 1 d . . . H12A H 0.3764 0.6011 0.3679 0.057 Uiso 1 1 calc R . . H12B H 0.3644 0.4924 0.3326 0.057 Uiso 1 1 calc R . . H12C H 0.4186 0.5711 0.3382 0.057 Uiso 1 1 calc R . . C13 C 0.4690(3) 0.5246(6) 0.4264(3) 0.0346(16) Uani 1 1 d . . . H13A H 0.4515 0.5884 0.4394 0.052 Uiso 1 1 calc R . . H13B H 0.4947 0.5589 0.4106 0.052 Uiso 1 1 calc R . . H13C H 0.4892 0.4722 0.4510 0.052 Uiso 1 1 calc R . . C14 C 0.4514(3) 0.3540(6) 0.3716(2) 0.0344(16) Uani 1 1 d . . . H14A H 0.4227 0.3092 0.3498 0.052 Uiso 1 1 calc R . . H14B H 0.4715 0.3008 0.3959 0.052 Uiso 1 1 calc R . . H14C H 0.4770 0.3880 0.3556 0.052 Uiso 1 1 calc R . . C15 C 0.5174(3) 0.0550(6) 0.6004(2) 0.0308(14) Uani 1 1 d . . . C16 C 0.5371(3) -0.0198(7) 0.5649(3) 0.0376(17) Uani 1 1 d . . . H16A H 0.5751 -0.0455 0.5782 0.056 Uiso 1 1 calc R . . H16B H 0.5352 0.0283 0.5376 0.056 Uiso 1 1 calc R . . H16C H 0.5133 -0.0896 0.5564 0.056 Uiso 1 1 calc R . . C17 C 0.5541(3) 0.1655(7) 0.6132(3) 0.050(2) Uani 1 1 d . . . H17A H 0.5922 0.1409 0.6268 0.075 Uiso 1 1 calc R . . H17B H 0.5413 0.2137 0.6352 0.075 Uiso 1 1 calc R . . H17C H 0.5522 0.2124 0.5855 0.075 Uiso 1 1 calc R . . C18 C 0.5228(3) -0.0207(7) 0.6438(3) 0.0426(18) Uani 1 1 d . . . H18A H 0.5613 -0.0441 0.6563 0.064 Uiso 1 1 calc R . . H18B H 0.4999 -0.0918 0.6359 0.064 Uiso 1 1 calc R . . H18C H 0.5107 0.0258 0.6666 0.064 Uiso 1 1 calc R . . C19 C 0.2913(3) -0.0190(6) 0.4595(2) 0.0305(14) Uani 1 1 d . . . H19 H 0.3283 -0.0104 0.4774 0.037 Uiso 1 1 calc R . . C20 C 0.2767(3) -0.1196(6) 0.4337(2) 0.0330(15) Uani 1 1 d . . . H20 H 0.3040 -0.1774 0.4332 0.040 Uiso 1 1 calc R . . C21 C 0.2229(3) -0.1387(6) 0.4081(2) 0.0287(14) Uani 1 1 d . . . C22 C 0.1860(3) -0.0471(6) 0.4080(2) 0.0289(14) Uani 1 1 d . . . H22 H 0.1489 -0.0547 0.3904 0.035 Uiso 1 1 calc R . . C23 C 0.2026(3) 0.0556(6) 0.4333(2) 0.0246(13) Uani 1 1 d . . . C24 C 0.1675(3) 0.1599(6) 0.4336(2) 0.0253(13) Uani 1 1 d . . . C25 C 0.1138(3) 0.1703(7) 0.4076(3) 0.0391(18) Uani 1 1 d . D . H25 H 0.0969 0.1057 0.3890 0.047 Uiso 1 1 calc R . . C26 C 0.0839(3) 0.2740(8) 0.4082(3) 0.047(2) Uani 1 1 d . . . C27 C 0.1112(3) 0.3652(7) 0.4355(3) 0.0434(19) Uani 1 1 d . D . H27 H 0.0929 0.4385 0.4364 0.052 Uiso 1 1 calc R . . C28 C 0.1640(3) 0.3512(6) 0.4613(3) 0.0321(15) Uani 1 1 d . . . H28 H 0.1815 0.4156 0.4797 0.039 Uiso 1 1 calc R D . C29 C 0.2073(3) -0.2555(7) 0.3821(3) 0.0393(17) Uani 1 1 d . . . C30 C 0.1452(4) -0.2663(8) 0.3629(4) 0.057(3) Uani 1 1 d . . . H30A H 0.1364 -0.3418 0.3465 0.085 Uiso 1 1 calc R . . H30B H 0.1316 -0.2005 0.3418 0.085 Uiso 1 1 calc R . . H30C H 0.1276 -0.2637 0.3881 0.085 Uiso 1 1 calc R . . C31 C 0.2261(4) -0.3599(7) 0.4155(3) 0.054(2) Uani 1 1 d . . . H31A H 0.2162 -0.4351 0.3991 0.081 Uiso 1 1 calc R . . H31B H 0.2079 -0.3547 0.4403 0.081 Uiso 1 1 calc R . . H31C H 0.2661 -0.3563 0.4284 0.081 Uiso 1 1 calc R . . C32 C 0.2367(5) -0.2610(9) 0.3438(3) 0.064(3) Uani 1 1 d . . . H32A H 0.2272 -0.3353 0.3268 0.096 Uiso 1 1 calc R . . H32B H 0.2766 -0.2575 0.3573 0.096 Uiso 1 1 calc R . . H32C H 0.2251 -0.1937 0.3230 0.096 Uiso 1 1 calc R . . C33 C 0.0210(6) 0.2707(14) 0.3837(5) 0.048(2) Uiso 0.651(13) 1 d PU D 1 C34 C -0.0095(7) 0.1856(15) 0.4072(5) 0.058(3) Uiso 0.651(13) 1 d PU D 1 H34A H 0.0053 0.1053 0.4067 0.087 Uiso 0.651(13) 1 calc PR D 1 H34B H -0.0487 0.1857 0.3910 0.087 Uiso 0.651(13) 1 calc PR D 1 H34C H -0.0048 0.2107 0.4389 0.087 Uiso 0.651(13) 1 calc PR D 1 C35 C -0.0034(7) 0.3908(14) 0.3855(5) 0.059(3) Uiso 0.651(13) 1 d PU D 1 H35A H 0.0039 0.4165 0.4175 0.088 Uiso 0.651(13) 1 calc PR D 1 H35B H -0.0432 0.3873 0.3718 0.088 Uiso 0.651(13) 1 calc PR D 1 H35C H 0.0132 0.4473 0.3685 0.088 Uiso 0.651(13) 1 calc PR D 1 C36 C 0.0107(7) 0.2222(14) 0.3358(5) 0.048(3) Uiso 0.651(13) 1 d PU D 1 H36A H 0.0270 0.1430 0.3369 0.072 Uiso 0.651(13) 1 calc PR D 1 H36B H 0.0273 0.2751 0.3175 0.072 Uiso 0.651(13) 1 calc PR D 1 H36C H -0.0291 0.2170 0.3218 0.072 Uiso 0.651(13) 1 calc PR D 1 C33' C 0.0287(12) 0.308(3) 0.3732(10) 0.049(3) Uiso 0.349(13) 1 d PU D 2 C34' C -0.0096(13) 0.256(3) 0.3989(10) 0.059(3) Uiso 0.349(13) 1 d PU D 2 H34D H -0.0028 0.2943 0.4290 0.088 Uiso 0.349(13) 1 calc PR D 2 H34E H -0.0031 0.1708 0.4029 0.088 Uiso 0.349(13) 1 calc PR D 2 H34F H -0.0478 0.2704 0.3815 0.088 Uiso 0.349(13) 1 calc PR D 2 C35' C 0.0141(12) 0.434(3) 0.3654(10) 0.060(4) Uiso 0.349(13) 1 d PU D 2 H35D H 0.0173 0.4730 0.3949 0.089 Uiso 0.349(13) 1 calc PR D 2 H35E H -0.0238 0.4405 0.3463 0.089 Uiso 0.349(13) 1 calc PR D 2 H35F H 0.0392 0.4716 0.3499 0.089 Uiso 0.349(13) 1 calc PR D 2 C36' C 0.0210(12) 0.255(3) 0.3278(9) 0.044(4) Uiso 0.349(13) 1 d PU D 2 H36D H 0.0301 0.1703 0.3311 0.067 Uiso 0.349(13) 1 calc PR D 2 H36E H 0.0451 0.2946 0.3118 0.067 Uiso 0.349(13) 1 calc PR D 2 H36F H -0.0175 0.2644 0.3102 0.067 Uiso 0.349(13) 1 calc PR D 2 C37 C 0.2988(3) 0.4582(6) 0.5479(2) 0.0305(15) Uani 1 1 d . . . H37 H 0.3192 0.4727 0.5262 0.037 Uiso 1 1 calc R . . C38 C 0.2954(3) 0.5452(6) 0.5790(3) 0.0366(17) Uani 1 1 d . . . H38 H 0.3132 0.6194 0.5792 0.044 Uiso 1 1 calc R . . C39 C 0.2653(3) 0.5213(6) 0.6100(2) 0.0328(15) Uani 1 1 d . . . H39 H 0.2621 0.5810 0.6312 0.039 Uiso 1 1 calc R . . C40 C 0.2451(2) 0.3376(5) 0.5796(2) 0.0212(12) Uani 1 1 d . . . C41 C 0.2190(3) 0.2198(5) 0.5791(2) 0.0250(13) Uani 1 1 d . . . C42 C 0.2086(3) 0.0332(6) 0.5482(2) 0.0310(15) Uani 1 1 d . . . H42 H 0.2151 -0.0240 0.5272 0.037 Uiso 1 1 calc R . . C43 C 0.1788(3) 0.0007(6) 0.5782(3) 0.0399(18) Uani 1 1 d . . . H43 H 0.1650 -0.0776 0.5784 0.048 Uiso 1 1 calc R . . C44 C 0.1698(3) 0.0866(6) 0.6081(3) 0.0382(17) Uani 1 1 d . . . H44 H 0.1488 0.0666 0.6288 0.046 Uiso 1 1 calc R . . C45 C 0.1986(3) 0.7782(7) 0.69219(18) 0.051(2) Uani 1 1 d D . . C46 C 0.1768(3) 0.6530(7) 0.6965(2) 0.0368(16) Uani 1 1 d . B . C47 C 0.1390(3) 0.6439(7) 0.7226(3) 0.0376(17) Uani 1 1 d . . . H47 H 0.1294 0.7131 0.7367 0.045 Uiso 1 1 calc R B . C48 C 0.1149(3) 0.5353(7) 0.7286(2) 0.0359(16) Uani 1 1 d . B . C49 C 0.0746(4) 0.5332(9) 0.7585(3) 0.050(2) Uani 1 1 d . . . C50 C 0.2928(4) 0.4077(9) 0.8251(3) 0.056(2) Uani 1 1 d . . . C51 C 0.2814(3) 0.3614(7) 0.7757(3) 0.0398(17) Uani 1 1 d . . . C52 C 0.3131(4) 0.2671(8) 0.7678(3) 0.048(2) Uani 1 1 d . . . H52 H 0.3403 0.2336 0.7926 0.058 Uiso 1 1 calc R . . C53 C 0.3057(4) 0.2212(8) 0.7238(3) 0.047(2) Uani 1 1 d . . . C54 C 0.3413(5) 0.1156(11) 0.7179(4) 0.066(3) Uani 1 1 d . . . C55 C 0.0081(5) 0.1784(14) 0.6397(5) 0.087(4) Uani 1 1 d . . . C56 C 0.0685(4) 0.1908(8) 0.6672(3) 0.051(2) Uani 1 1 d . . . C57 C 0.0856(4) 0.1410(9) 0.7106(4) 0.061(3) Uani 1 1 d . C . H57 H 0.0598 0.1016 0.7233 0.073 Uiso 1 1 calc R . . C58 C 0.1402(4) 0.1486(8) 0.7354(4) 0.059(3) Uani 1 1 d D . . O3W O 0.3875(6) 0.7762(8) 0.6742(4) 0.051(3) Uani 0.50 1 d P . . O2W O 0.4152(5) 0.3465(8) 0.6409(4) 0.043(3) Uani 0.50 1 d P . . O4W O 0.3479(5) 0.6267(12) 0.7375(4) 0.054(3) Uani 0.50 1 d P . . O1W O 0.5200(6) -0.0278(19) 0.7841(5) 0.092(6) Uani 0.50 1 d P . . O8 O 0.0408(5) 0.3341(12) 0.5345(4) 0.083(3) Uiso 0.677(13) 1 d PU E 1 O8' O 0.0718(11) 0.267(2) 0.5229(9) 0.081(4) Uiso 0.323(13) 1 d PU E 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 Nd1 0.0350(2) 0.02466(18) 0.0328(2) 0.00393(14) 0.01979(16) 0.00405(15) Os1 0.02212(13) 0.01918(12) 0.02614(13) 0.00019(9) 0.00970(9) 0.00112(9) P2 0.0757(17) 0.0334(11) 0.0483(13) 0.0026(9) 0.0251(12) 0.0069(11) F7 0.087(5) 0.047(3) 0.116(5) -0.021(3) 0.010(4) 0.023(3) F8 0.087(5) 0.100(5) 0.104(5) 0.008(4) 0.036(4) -0.025(4) F9 0.136(6) 0.080(5) 0.059(4) -0.015(3) 0.043(4) -0.011(4) F10 0.122(6) 0.072(4) 0.120(6) -0.030(4) 0.076(5) -0.045(4) F11 0.128(6) 0.100(5) 0.052(4) 0.000(4) 0.015(4) -0.014(5) F12 0.154(8) 0.080(5) 0.157(8) 0.036(5) 0.068(7) 0.066(5) F16 0.051(3) 0.123(6) 0.089(4) -0.043(4) 0.044(3) -0.026(4) F17 0.065(3) 0.080(4) 0.062(3) -0.006(3) 0.036(3) 0.030(3) F18 0.073(4) 0.072(4) 0.050(3) 0.012(3) 0.036(3) 0.012(3) F19 0.066(4) 0.213(9) 0.060(4) -0.051(5) 0.024(3) -0.004(5) F20 0.138(6) 0.058(4) 0.073(4) -0.025(3) 0.000(4) -0.002(4) F21 0.083(4) 0.077(4) 0.043(3) -0.007(3) -0.005(3) 0.015(3) F22 0.177(8) 0.164(8) 0.065(4) 0.027(5) 0.057(5) 0.134(7) F23 0.168(10) 0.055(5) 0.301(15) -0.006(7) 0.117(10) 0.026(6) F24 0.112(6) 0.168(8) 0.082(5) -0.019(5) 0.001(4) 0.098(6) F25 0.117(7) 0.283(16) 0.092(6) -0.013(8) 0.029(5) -0.110(9) F26 0.065(4) 0.081(4) 0.105(5) -0.012(4) 0.040(4) -0.033(3) F27 0.041(4) 0.072(6) 0.48(2) 0.041(9) -0.032(8) -0.006(4) O1 0.046(3) 0.031(3) 0.038(3) 0.002(2) 0.022(2) 0.003(2) O2 0.040(3) 0.038(3) 0.042(3) 0.000(2) 0.024(2) 0.005(2) O3 0.046(3) 0.035(3) 0.043(3) -0.002(2) 0.012(2) 0.007(2) O4 0.050(3) 0.057(3) 0.033(3) 0.005(2) 0.018(3) 0.021(3) O5 0.041(3) 0.047(3) 0.041(3) 0.002(2) 0.023(2) -0.006(2) O6 0.048(3) 0.040(3) 0.058(4) 0.017(3) 0.023(3) 0.006(3) O7 0.035(3) 0.047(3) 0.050(3) 0.019(3) 0.009(2) -0.001(2) N1 0.027(3) 0.020(2) 0.027(3) 0.001(2) 0.012(2) 0.005(2) N2 0.027(3) 0.018(2) 0.025(3) 0.001(2) 0.009(2) 0.002(2) N3 0.025(3) 0.021(3) 0.022(2) 0.001(2) 0.004(2) 0.004(2) N4 0.021(3) 0.025(3) 0.036(3) -0.004(2) 0.013(2) 0.002(2) N5 0.023(3) 0.024(3) 0.026(3) 0.000(2) 0.010(2) 0.001(2) N6 0.024(3) 0.022(3) 0.026(3) 0.000(2) 0.006(2) 0.000(2) N7 0.034(3) 0.022(3) 0.038(3) 0.002(2) 0.022(3) 0.001(2) N8 0.030(3) 0.025(3) 0.032(3) -0.001(2) 0.016(2) -0.002(2) C1 0.023(3) 0.027(3) 0.037(4) 0.007(3) 0.009(3) 0.006(3) C2 0.026(3) 0.028(3) 0.033(3) 0.012(3) 0.010(3) 0.008(3) C3 0.028(3) 0.018(3) 0.026(3) 0.000(2) 0.011(3) 0.005(2) C4 0.021(3) 0.024(3) 0.028(3) 0.002(2) 0.005(3) 0.005(2) C5 0.022(3) 0.020(3) 0.022(3) 0.000(2) 0.005(2) 0.001(2) C6 0.023(3) 0.018(3) 0.025(3) 0.000(2) 0.005(2) 0.001(2) C7 0.029(4) 0.024(3) 0.027(3) 0.001(3) 0.006(3) 0.003(3) C8 0.027(3) 0.024(3) 0.025(3) -0.001(2) 0.004(3) 0.003(3) C9 0.036(4) 0.027(3) 0.025(3) 0.004(3) 0.004(3) 0.000(3) C10 0.030(4) 0.027(3) 0.031(3) 0.003(3) 0.010(3) -0.002(3) C11 0.029(4) 0.028(3) 0.032(3) 0.009(3) 0.013(3) 0.002(3) C12 0.035(4) 0.042(4) 0.040(4) 0.015(3) 0.012(3) 0.006(3) C13 0.034(4) 0.027(3) 0.043(4) 0.008(3) 0.012(3) 0.002(3) C14 0.041(4) 0.033(4) 0.034(4) -0.001(3) 0.019(3) 0.002(3) C15 0.031(4) 0.027(3) 0.030(3) 0.004(3) -0.001(3) -0.002(3) C16 0.028(4) 0.044(4) 0.042(4) 0.005(3) 0.011(3) 0.007(3) C17 0.043(5) 0.032(4) 0.058(5) 0.009(4) -0.015(4) -0.005(4) C18 0.042(5) 0.044(4) 0.038(4) 0.013(3) 0.005(3) 0.009(4) C19 0.024(3) 0.031(4) 0.034(4) -0.001(3) 0.003(3) 0.006(3) C20 0.038(4) 0.023(3) 0.036(4) -0.006(3) 0.008(3) 0.011(3) C21 0.036(4) 0.022(3) 0.026(3) 0.001(3) 0.005(3) 0.002(3) C22 0.029(4) 0.026(3) 0.032(3) 0.000(3) 0.008(3) 0.002(3) C23 0.022(3) 0.027(3) 0.025(3) 0.001(3) 0.007(2) 0.004(3) C24 0.027(3) 0.028(3) 0.022(3) 0.000(2) 0.007(3) 0.002(3) C25 0.030(4) 0.046(4) 0.039(4) -0.013(3) 0.006(3) 0.011(3) C26 0.029(4) 0.061(5) 0.046(4) -0.013(4) 0.004(3) 0.022(4) C27 0.035(4) 0.045(4) 0.051(5) -0.009(4) 0.013(4) 0.018(4) C28 0.029(4) 0.026(3) 0.045(4) -0.002(3) 0.017(3) 0.005(3) C29 0.042(4) 0.028(4) 0.044(4) -0.009(3) 0.005(3) -0.001(3) C30 0.050(5) 0.035(5) 0.073(6) -0.017(4) -0.007(5) -0.001(4) C31 0.055(5) 0.022(4) 0.080(7) -0.005(4) 0.009(5) 0.003(4) C32 0.081(7) 0.063(6) 0.056(6) -0.028(5) 0.031(5) -0.022(5) C37 0.030(4) 0.028(3) 0.038(4) -0.004(3) 0.018(3) -0.007(3) C38 0.044(4) 0.027(3) 0.048(4) -0.006(3) 0.028(4) -0.010(3) C39 0.043(4) 0.024(3) 0.039(4) -0.007(3) 0.023(3) -0.004(3) C40 0.019(3) 0.021(3) 0.024(3) 0.002(2) 0.006(2) 0.001(2) C41 0.021(3) 0.021(3) 0.034(3) 0.005(3) 0.011(3) 0.002(3) C42 0.039(4) 0.021(3) 0.035(4) -0.004(3) 0.013(3) -0.004(3) C43 0.050(5) 0.021(3) 0.055(5) 0.002(3) 0.027(4) -0.008(3) C44 0.043(4) 0.031(4) 0.050(4) 0.005(3) 0.028(4) -0.003(3) C45 0.072(6) 0.031(4) 0.052(5) 0.000(4) 0.020(5) 0.006(4) C46 0.048(5) 0.033(4) 0.029(4) 0.001(3) 0.010(3) 0.008(3) C47 0.041(4) 0.035(4) 0.039(4) -0.008(3) 0.013(3) 0.008(3) C48 0.032(4) 0.048(4) 0.028(3) 0.003(3) 0.008(3) 0.012(3) C49 0.038(5) 0.063(6) 0.053(5) -0.009(4) 0.020(4) 0.005(4) C50 0.060(6) 0.059(6) 0.042(5) -0.005(4) 0.003(4) 0.006(5) C51 0.038(4) 0.043(4) 0.039(4) 0.003(3) 0.010(3) 0.003(3) C52 0.047(5) 0.061(5) 0.036(4) 0.008(4) 0.011(4) 0.018(4) C53 0.045(5) 0.059(5) 0.041(4) 0.008(4) 0.020(4) 0.016(4) C54 0.069(7) 0.075(7) 0.057(6) 0.003(5) 0.019(5) 0.033(6) C55 0.063(8) 0.116(11) 0.091(9) 0.011(8) 0.036(7) -0.034(8) C56 0.046(5) 0.050(5) 0.066(6) 0.012(4) 0.031(4) -0.004(4) C57 0.057(6) 0.061(6) 0.076(7) 0.029(5) 0.038(5) 0.003(5) C58 0.064(6) 0.049(5) 0.074(6) 0.032(5) 0.036(5) 0.011(5) O3W 0.103(10) 0.016(5) 0.047(6) 0.003(4) 0.040(7) -0.011(5) O2W 0.060(7) 0.021(5) 0.038(6) -0.016(4) -0.003(5) 0.003(5) O4W 0.061(8) 0.067(8) 0.039(6) 0.022(6) 0.024(6) 0.009(6) O1W 0.057(9) 0.167(18) 0.059(9) 0.041(10) 0.029(7) 0.033(10) _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 Nd1 O2 2.406(5) . ? Nd1 O1 2.439(5) . ? Nd1 O6 2.442(5) . ? Nd1 O4 2.448(5) . ? Nd1 O5 2.448(5) . ? Nd1 O3 2.457(5) . ? Nd1 O7 2.476(5) . ? Nd1 N7 2.676(6) . ? Nd1 N8 2.695(5) . ? Os1 N6 2.042(5) . ? Os1 N1 2.052(5) . ? Os1 N5 2.052(5) . ? Os1 N3 2.054(5) . ? Os1 N4 2.065(6) . ? Os1 N2 2.067(5) . ? P1 F3 1.549(11) . ? P1 F1 1.577(11) . ? P1 F4 1.598(12) . ? P1 F2 1.611(10) . ? P1 F5 1.630(13) . ? P1 F6 1.637(11) . ? P1' F5' 1.529(11) . ? P1' F6' 1.530(11) . ? P1' F1' 1.582(10) . ? P1' F4' 1.586(12) . ? P1' F2' 1.597(10) . ? P1' F3' 1.657(12) . ? P2 F10 1.548(7) . ? P2 F11 1.569(7) . ? P2 F12 1.572(7) . ? P2 F7 1.573(6) . ? P2 F9 1.573(6) . ? P2 F8 1.621(7) . ? F13 C45 1.337(6) . ? F14 C45 1.348(6) . ? F15 C45 1.337(6) . ? F13' C45 1.338(6) . ? F14' C45 1.334(6) . ? F15' C45 1.347(6) . ? F16 C49 1.319(11) . ? F17 C49 1.322(10) . ? F18 C49 1.338(10) . ? F19 C50 1.304(12) . ? F20 C50 1.336(12) . ? F21 C50 1.314(11) . ? F22 C54 1.255(11) . ? F23 C54 1.334(15) . ? F24 C54 1.287(13) . ? F25 C55 1.389(16) . ? F26 C55 1.295(13) . ? F27 C55 1.235(17) . ? C59 F29 1.329(7) . ? C59 F28 1.330(7) . ? C59 F30 1.330(7) . ? C59 C58 1.574(16) . ? C59' F30' 1.329(8) . ? C59' F28' 1.329(8) . ? C59' F29' 1.330(8) . ? C59' C58 1.571(16) . ? O1 C46 1.235(8) . ? O2 C48 1.237(9) . ? O3 C51 1.250(9) . ? O4 C53 1.240(10) . ? O5 C56 1.252(9) . ? O6 C58 1.243(10) . ? N1 C1 1.338(8) . ? N1 C5 1.365(8) . ? N2 C10 1.332(8) . ? N2 C6 1.358(8) . ? N3 C19 1.352(8) . ? N3 C23 1.364(8) . ? N4 C28 1.353(8) . ? N4 C24 1.363(8) . ? N5 C40 1.346(8) . ? N5 C37 1.365(8) . ? N6 C42 1.352(8) . ? N6 C41 1.354(8) . ? N7 C44 1.331(9) . ? N7 C41 1.334(8) . ? N8 C40 1.332(8) . ? N8 C39 1.335(9) . ? C1 C2 1.378(9) . ? C1 H1 0.9500 . ? C2 C3 1.391(9) . ? C2 H2 0.9500 . ? C3 C4 1.402(9) . ? C3 C11 1.539(9) . ? C4 C5 1.385(9) . ? C4 H4 0.9500 . ? C5 C6 1.478(8) . ? C6 C7 1.371(9) . ? C7 C8 1.403(9) . ? C7 H7 0.9500 . ? C8 C9 1.386(9) . ? C8 C15 1.521(9) . ? C9 C10 1.391(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C14 1.523(9) . ? C11 C13 1.525(10) . ? C11 C12 1.540(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.538(10) . ? C15 C18 1.541(10) . ? C15 C16 1.550(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.371(9) . ? C19 H19 0.9500 . ? C20 C21 1.390(10) . ? C20 H20 0.9500 . ? C21 C22 1.388(9) . ? C21 C29 1.531(10) . ? C22 C23 1.390(9) . ? C22 H22 0.9500 . ? C23 C24 1.473(9) . ? C24 C25 1.378(10) . ? C25 C26 1.394(10) . ? C25 H25 0.9500 . ? C26 C27 1.383(12) . ? C26 C33' 1.56(3) . ? C26 C33 1.562(17) . ? C27 C28 1.362(11) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.524(12) . ? C29 C32 1.533(12) . ? C29 C31 1.543(12) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.49(2) . ? C33 C36 1.51(2) . ? C33 C34 1.52(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C33' C36' 1.47(4) . ? C33' C35' 1.47(4) . ? C33' C34' 1.51(4) . ? C34' H34D 0.9800 . ? C34' H34E 0.9800 . ? C34' H34F 0.9800 . ? C35' H35D 0.9800 . ? C35' H35E 0.9800 . ? C35' H35F 0.9800 . ? C36' H36D 0.9800 . ? C36' H36E 0.9800 . ? C36' H36F 0.9800 . ? C37 C38 1.379(9) . ? C37 H37 0.9500 . ? C38 C39 1.380(9) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.481(9) . ? C42 C43 1.373(10) . ? C42 H42 0.9500 . ? C43 C44 1.385(10) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.532(11) . ? C46 C47 1.396(10) . ? C47 C48 1.399(11) . ? C47 H47 0.9500 . ? C48 C49 1.531(10) . ? C50 C51 1.538(12) . ? C51 C52 1.390(11) . ? C52 C53 1.394(12) . ? C52 H52 0.9500 . ? C53 C54 1.531(12) . ? C55 C56 1.535(16) . ? C56 C57 1.389(13) . ? C57 C58 1.384(14) . ? C57 H57 0.9500 . ? 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 O2 Nd1 O1 71.54(17) . . ? O2 Nd1 O6 77.01(18) . . ? O1 Nd1 O6 136.09(19) . . ? O2 Nd1 O4 138.64(18) . . ? O1 Nd1 O4 113.1(2) . . ? O6 Nd1 O4 73.17(19) . . ? O2 Nd1 O5 72.20(18) . . ? O1 Nd1 O5 126.42(18) . . ? O6 Nd1 O5 68.45(19) . . ? O4 Nd1 O5 120.3(2) . . ? O2 Nd1 O3 74.85(18) . . ? O1 Nd1 O3 70.51(17) . . ? O6 Nd1 O3 72.2(2) . . ? O4 Nd1 O3 69.20(18) . . ? O5 Nd1 O3 133.04(17) . . ? O2 Nd1 O7 86.09(19) . . ? O1 Nd1 O7 72.14(18) . . ? O6 Nd1 O7 135.58(19) . . ? O4 Nd1 O7 135.18(18) . . ? O5 Nd1 O7 67.30(18) . . ? O3 Nd1 O7 141.79(19) . . ? O2 Nd1 N7 141.78(18) . . ? O1 Nd1 N7 133.90(16) . . ? O6 Nd1 N7 89.35(19) . . ? O4 Nd1 N7 65.96(19) . . ? O5 Nd1 N7 69.58(17) . . ? O3 Nd1 N7 134.77(18) . . ? O7 Nd1 N7 79.06(19) . . ? O2 Nd1 N8 142.95(17) . . ? O1 Nd1 N8 74.05(16) . . ? O6 Nd1 N8 139.47(18) . . ? O4 Nd1 N8 68.91(18) . . ? O5 Nd1 N8 120.42(17) . . ? O3 Nd1 N8 106.07(18) . . ? O7 Nd1 N8 70.52(17) . . ? N7 Nd1 N8 62.61(16) . . ? N6 Os1 N1 173.9(2) . . ? N6 Os1 N5 78.5(2) . . ? N1 Os1 N5 96.5(2) . . ? N6 Os1 N3 94.4(2) . . ? N1 Os1 N3 90.9(2) . . ? N5 Os1 N3 171.1(2) . . ? N6 Os1 N4 85.3(2) . . ? N1 Os1 N4 98.8(2) . . ? N5 Os1 N4 96.4(2) . . ? N3 Os1 N4 77.5(2) . . ? N6 Os1 N2 98.7(2) . . ? N1 Os1 N2 77.7(2) . . ? N5 Os1 N2 90.5(2) . . ? N3 Os1 N2 95.8(2) . . ? N4 Os1 N2 172.6(2) . . ? F3 P1 F1 93.6(6) . . ? F3 P1 F4 87.3(6) . . ? F1 P1 F4 88.6(6) . . ? F3 P1 F2 91.1(6) . . ? F1 P1 F2 89.9(5) . . ? F4 P1 F2 177.7(7) . . ? F3 P1 F5 179.6(8) . . ? F1 P1 F5 86.7(6) . . ? F4 P1 F5 92.6(6) . . ? F2 P1 F5 89.1(6) . . ? F3 P1 F6 80.2(6) . . ? F1 P1 F6 172.6(6) . . ? F4 P1 F6 87.0(6) . . ? F2 P1 F6 94.2(5) . . ? F5 P1 F6 99.5(7) . . ? F5' P1' F6' 81.9(6) . . ? F5' P1' F1' 91.4(6) . . ? F6' P1' F1' 172.0(6) . . ? F5' P1' F4' 86.4(6) . . ? F6' P1' F4' 93.3(6) . . ? F1' P1' F4' 90.5(6) . . ? F5' P1' F2' 91.8(6) . . ? F6' P1' F2' 83.9(6) . . ? F1' P1' F2' 92.1(5) . . ? F4' P1' F2' 176.9(6) . . ? F5' P1' F3' 179.0(6) . . ? F6' P1' F3' 98.3(6) . . ? F1' P1' F3' 88.5(6) . . ? F4' P1' F3' 92.7(6) . . ? F2' P1' F3' 89.1(6) . . ? F10 P2 F11 92.3(4) . . ? F10 P2 F12 90.5(5) . . ? F11 P2 F12 92.1(5) . . ? F10 P2 F7 92.2(4) . . ? F11 P2 F7 90.4(4) . . ? F12 P2 F7 176.2(5) . . ? F10 P2 F9 91.9(4) . . ? F11 P2 F9 175.8(4) . . ? F12 P2 F9 88.2(5) . . ? F7 P2 F9 89.1(4) . . ? F10 P2 F8 179.1(5) . . ? F11 P2 F8 88.5(4) . . ? F12 P2 F8 90.0(5) . . ? F7 P2 F8 87.2(4) . . ? F9 P2 F8 87.3(4) . . ? F29 C59 F28 108.3(7) . . ? F29 C59 F30 108.0(7) . . ? F28 C59 F30 108.1(7) . . ? F29 C59 C58 115.0(12) . . ? F28 C59 C58 104.0(11) . . ? F30 C59 C58 113.1(11) . . ? F30' C59' F28' 108.2(8) . . ? F30' C59' F29' 108.2(8) . . ? F28' C59' F29' 107.9(7) . . ? F30' C59' C58 110.3(12) . . ? F28' C59' C58 117.6(13) . . ? F29' C59' C58 104.2(13) . . ? C46 O1 Nd1 134.2(5) . . ? C48 O2 Nd1 135.3(5) . . ? C51 O3 Nd1 133.3(5) . . ? C53 O4 Nd1 133.5(5) . . ? C56 O5 Nd1 134.6(6) . . ? C58 O6 Nd1 133.3(6) . . ? C1 N1 C5 117.7(5) . . ? C1 N1 Os1 125.3(4) . . ? C5 N1 Os1 117.0(4) . . ? C10 N2 C6 118.0(5) . . ? C10 N2 Os1 124.7(4) . . ? C6 N2 Os1 117.3(4) . . ? C19 N3 C23 117.5(6) . . ? C19 N3 Os1 125.3(4) . . ? C23 N3 Os1 117.0(4) . . ? C28 N4 C24 117.6(6) . . ? C28 N4 Os1 126.2(5) . . ? C24 N4 Os1 116.1(4) . . ? C40 N5 C37 116.2(5) . . ? C40 N5 Os1 116.2(4) . . ? C37 N5 Os1 127.5(4) . . ? C42 N6 C41 115.4(5) . . ? C42 N6 Os1 128.2(4) . . ? C41 N6 Os1 116.4(4) . . ? C44 N7 C41 116.5(6) . . ? C44 N7 Nd1 123.7(4) . . ? C41 N7 Nd1 119.4(4) . . ? C40 N8 C39 116.4(5) . . ? C40 N8 Nd1 119.1(4) . . ? C39 N8 Nd1 124.5(4) . . ? N1 C1 C2 123.6(6) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 120.1(6) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C2 C3 C4 116.3(6) . . ? C2 C3 C11 123.1(6) . . ? C4 C3 C11 120.7(6) . . ? C5 C4 C3 121.2(6) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? N1 C5 C4 121.2(6) . . ? N1 C5 C6 114.4(5) . . ? C4 C5 C6 124.4(6) . . ? N2 C6 C7 121.7(6) . . ? N2 C6 C5 113.5(5) . . ? C7 C6 C5 124.8(6) . . ? C6 C7 C8 121.4(6) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C9 C8 C7 115.8(6) . . ? C9 C8 C15 122.3(6) . . ? C7 C8 C15 121.9(6) . . ? C8 C9 C10 120.5(6) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? N2 C10 C9 122.7(6) . . ? N2 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C14 C11 C13 110.3(6) . . ? C14 C11 C3 108.3(5) . . ? C13 C11 C3 108.9(5) . . ? C14 C11 C12 109.7(6) . . ? C13 C11 C12 108.9(6) . . ? C3 C11 C12 110.6(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C8 C15 C17 109.0(6) . . ? C8 C15 C18 112.1(6) . . ? C17 C15 C18 108.9(6) . . ? C8 C15 C16 108.9(5) . . ? C17 C15 C16 109.4(7) . . ? C18 C15 C16 108.6(6) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 122.3(6) . . ? N3 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C19 C20 C21 121.3(6) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C22 C21 C20 116.1(6) . . ? C22 C21 C29 124.0(6) . . ? C20 C21 C29 119.9(6) . . ? C21 C22 C23 121.0(6) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? N3 C23 C22 121.5(6) . . ? N3 C23 C24 113.4(6) . . ? C22 C23 C24 125.1(6) . . ? N4 C24 C25 121.1(6) . . ? N4 C24 C23 114.5(6) . . ? C25 C24 C23 124.4(6) . . ? C24 C25 C26 121.1(7) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C26 C25 116.5(7) . . ? C27 C26 C33' 116.0(13) . . ? C25 C26 C33' 125.9(12) . . ? C27 C26 C33 125.7(8) . . ? C25 C26 C33 117.3(9) . . ? C33' C26 C33 21.8(10) . . ? C28 C27 C26 120.8(7) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? N4 C28 C27 122.8(7) . . ? N4 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? C30 C29 C21 111.2(6) . . ? C30 C29 C32 111.3(8) . . ? C21 C29 C32 108.3(7) . . ? C30 C29 C31 107.1(7) . . ? C21 C29 C31 109.0(6) . . ? C32 C29 C31 109.9(8) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C33 C36 113.3(13) . . ? C35 C33 C34 106.9(13) . . ? C36 C33 C34 104.0(12) . . ? C35 C33 C26 109.7(12) . . ? C36 C33 C26 111.1(12) . . ? C34 C33 C26 111.7(12) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C36' C33' C35' 106(2) . . ? C36' C33' C34' 113(2) . . ? C35' C33' C34' 107(2) . . ? C36' C33' C26 114(2) . . ? C35' C33' C26 119(2) . . ? C34' C33' C26 98(2) . . ? C33' C34' H34D 109.5 . . ? C33' C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C33' C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C33' C35' H35D 109.5 . . ? C33' C35' H35E 109.5 . . ? H35D C35' H35E 109.5 . . ? C33' C35' H35F 109.5 . . ? H35D C35' H35F 109.5 . . ? H35E C35' H35F 109.5 . . ? C33' C36' H36D 109.5 . . ? C33' C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C33' C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? N5 C37 C38 120.7(6) . . ? N5 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C37 C38 C39 118.2(6) . . ? C37 C38 H38 120.9 . . ? C39 C38 H38 120.9 . . ? N8 C39 C38 122.2(6) . . ? N8 C39 H39 118.9 . . ? C38 C39 H39 118.9 . . ? N8 C40 N5 126.4(6) . . ? N8 C40 C41 119.2(5) . . ? N5 C40 C41 114.4(5) . . ? N7 C41 N6 126.3(6) . . ? N7 C41 C40 119.7(6) . . ? N6 C41 C40 114.1(5) . . ? N6 C42 C43 122.2(6) . . ? N6 C42 H42 118.9 . . ? C43 C42 H42 118.9 . . ? C42 C43 C44 117.3(6) . . ? C42 C43 H43 121.3 . . ? C44 C43 H43 121.3 . . ? N7 C44 C43 122.2(6) . . ? N7 C44 H44 118.9 . . ? C43 C44 H44 118.9 . . ? F14' C45 F15 74.3(6) . . ? F14' C45 F13 123.5(9) . . ? F15 C45 F13 106.3(5) . . ? F14' C45 F13' 106.6(5) . . ? F15 C45 F13' 120.2(9) . . ? F13 C45 F13' 23.5(5) . . ? F14' C45 F15' 105.6(5) . . ? F15 C45 F15' 31.8(5) . . ? F13 C45 F15' 84.6(6) . . ? F13' C45 F15' 105.6(5) . . ? F14' C45 F14 32.4(5) . . ? F15 C45 F14 105.4(5) . . ? F13 C45 F14 105.5(5) . . ? F13' C45 F14 83.2(6) . . ? F15' C45 F14 134.8(9) . . ? F14' C45 C46 115.7(8) . . ? F15 C45 C46 118.6(8) . . ? F13 C45 C46 112.6(7) . . ? F13' C45 C46 114.0(7) . . ? F15' C45 C46 108.5(8) . . ? F14 C45 C46 107.6(7) . . ? O1 C46 C47 128.6(7) . . ? O1 C46 C45 115.9(6) . . ? C47 C46 C45 115.5(6) . . ? C46 C47 C48 121.5(7) . . ? C46 C47 H47 119.2 . . ? C48 C47 H47 119.2 . . ? O2 C48 C47 128.2(7) . . ? O2 C48 C49 113.8(7) . . ? C47 C48 C49 118.0(7) . . ? F16 C49 F17 107.2(7) . . ? F16 C49 F18 107.9(8) . . ? F17 C49 F18 106.8(7) . . ? F16 C49 C48 111.4(7) . . ? F17 C49 C48 114.0(8) . . ? F18 C49 C48 109.2(7) . . ? F19 C50 F21 109.5(9) . . ? F19 C50 F20 106.0(9) . . ? F21 C50 F20 105.5(8) . . ? F19 C50 C51 111.0(8) . . ? F21 C50 C51 114.9(8) . . ? F20 C50 C51 109.4(8) . . ? O3 C51 C52 127.9(8) . . ? O3 C51 C50 114.7(7) . . ? C52 C51 C50 117.4(7) . . ? C51 C52 C53 120.7(8) . . ? C51 C52 H52 119.6 . . ? C53 C52 H52 119.6 . . ? O4 C53 C52 128.2(8) . . ? O4 C53 C54 114.0(8) . . ? C52 C53 C54 117.8(8) . . ? F22 C54 F24 107.2(10) . . ? F22 C54 F23 108.2(12) . . ? F24 C54 F23 101.4(11) . . ? F22 C54 C53 114.2(9) . . ? F24 C54 C53 115.1(9) . . ? F23 C54 C53 109.8(9) . . ? F27 C55 F26 111.1(12) . . ? F27 C55 F25 110.4(15) . . ? F26 C55 F25 101.0(12) . . ? F27 C55 C56 111.2(12) . . ? F26 C55 C56 114.3(11) . . ? F25 C55 C56 108.3(10) . . ? O5 C56 C57 126.9(9) . . ? O5 C56 C55 113.7(9) . . ? C57 C56 C55 119.4(8) . . ? C58 C57 C56 120.3(8) . . ? C58 C57 H57 119.9 . . ? C56 C57 H57 119.9 . . ? O6 C58 C57 128.8(9) . . ? O6 C58 C59' 113.6(9) . . ? C57 C58 C59' 117.6(8) . . ? O6 C58 C59 111.8(9) . . ? C57 C58 C59 119.0(8) . . ? C59' C58 C59 10.6(7) . . ? 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 O2 Nd1 O1 C46 6.9(7) . . . . ? O6 Nd1 O1 C46 -39.6(8) . . . . ? O4 Nd1 O1 C46 -128.9(7) . . . . ? O5 Nd1 O1 C46 56.6(7) . . . . ? O3 Nd1 O1 C46 -73.0(7) . . . . ? O7 Nd1 O1 C46 98.8(7) . . . . ? N7 Nd1 O1 C46 152.8(6) . . . . ? N8 Nd1 O1 C46 173.0(7) . . . . ? O1 Nd1 O2 C48 -8.2(7) . . . . ? O6 Nd1 O2 C48 140.7(7) . . . . ? O4 Nd1 O2 C48 96.1(7) . . . . ? O5 Nd1 O2 C48 -148.1(7) . . . . ? O3 Nd1 O2 C48 65.9(7) . . . . ? O7 Nd1 O2 C48 -80.7(7) . . . . ? N7 Nd1 O2 C48 -147.5(6) . . . . ? N8 Nd1 O2 C48 -30.8(8) . . . . ? O2 Nd1 O3 C51 133.5(7) . . . . ? O1 Nd1 O3 C51 -151.1(7) . . . . ? O6 Nd1 O3 C51 52.6(7) . . . . ? O4 Nd1 O3 C51 -25.7(7) . . . . ? O5 Nd1 O3 C51 86.8(7) . . . . ? O7 Nd1 O3 C51 -163.8(6) . . . . ? N7 Nd1 O3 C51 -17.9(8) . . . . ? N8 Nd1 O3 C51 -85.0(7) . . . . ? O2 Nd1 O4 C53 -4.6(10) . . . . ? O1 Nd1 O4 C53 83.3(8) . . . . ? O6 Nd1 O4 C53 -50.2(8) . . . . ? O5 Nd1 O4 C53 -101.9(8) . . . . ? O3 Nd1 O4 C53 26.7(8) . . . . ? O7 Nd1 O4 C53 170.8(8) . . . . ? N7 Nd1 O4 C53 -147.2(9) . . . . ? N8 Nd1 O4 C53 144.3(9) . . . . ? O2 Nd1 O5 C56 -55.9(8) . . . . ? O1 Nd1 O5 C56 -105.3(8) . . . . ? O6 Nd1 O5 C56 26.8(8) . . . . ? O4 Nd1 O5 C56 80.6(8) . . . . ? O3 Nd1 O5 C56 -8.3(9) . . . . ? O7 Nd1 O5 C56 -149.1(8) . . . . ? N7 Nd1 O5 C56 124.5(8) . . . . ? N8 Nd1 O5 C56 162.5(8) . . . . ? O2 Nd1 O6 C58 48.1(9) . . . . ? O1 Nd1 O6 C58 93.0(9) . . . . ? O4 Nd1 O6 C58 -160.9(9) . . . . ? O5 Nd1 O6 C58 -27.6(9) . . . . ? O3 Nd1 O6 C58 126.1(9) . . . . ? O7 Nd1 O6 C58 -22.3(10) . . . . ? N7 Nd1 O6 C58 -95.9(9) . . . . ? N8 Nd1 O6 C58 -139.7(8) . . . . ? N6 Os1 N1 C1 -124.7(18) . . . . ? N5 Os1 N1 C1 -90.7(5) . . . . ? N3 Os1 N1 C1 84.4(5) . . . . ? N4 Os1 N1 C1 6.9(6) . . . . ? N2 Os1 N1 C1 -179.8(6) . . . . ? N6 Os1 N1 C5 55(2) . . . . ? N5 Os1 N1 C5 89.0(4) . . . . ? N3 Os1 N1 C5 -95.9(4) . . . . ? N4 Os1 N1 C5 -173.5(4) . . . . ? N2 Os1 N1 C5 -0.1(4) . . . . ? N6 Os1 N2 C10 6.8(5) . . . . ? N1 Os1 N2 C10 -178.3(6) . . . . ? N5 Os1 N2 C10 85.2(5) . . . . ? N3 Os1 N2 C10 -88.6(5) . . . . ? N4 Os1 N2 C10 -115.8(16) . . . . ? N6 Os1 N2 C6 -175.5(4) . . . . ? N1 Os1 N2 C6 -0.5(4) . . . . ? N5 Os1 N2 C6 -97.0(4) . . . . ? N3 Os1 N2 C6 89.1(4) . . . . ? N4 Os1 N2 C6 62.0(17) . . . . ? N6 Os1 N3 C19 -101.2(5) . . . . ? N1 Os1 N3 C19 75.8(5) . . . . ? N5 Os1 N3 C19 -137.6(12) . . . . ? N4 Os1 N3 C19 174.6(6) . . . . ? N2 Os1 N3 C19 -2.0(6) . . . . ? N6 Os1 N3 C23 73.2(5) . . . . ? N1 Os1 N3 C23 -109.8(5) . . . . ? N5 Os1 N3 C23 36.7(15) . . . . ? N4 Os1 N3 C23 -11.0(4) . . . . ? N2 Os1 N3 C23 172.4(4) . . . . ? N6 Os1 N4 C28 91.0(6) . . . . ? N1 Os1 N4 C28 -84.4(6) . . . . ? N5 Os1 N4 C28 13.2(6) . . . . ? N3 Os1 N4 C28 -173.4(6) . . . . ? N2 Os1 N4 C28 -145.8(14) . . . . ? N6 Os1 N4 C24 -85.7(5) . . . . ? N1 Os1 N4 C24 98.9(5) . . . . ? N5 Os1 N4 C24 -163.5(5) . . . . ? N3 Os1 N4 C24 9.9(4) . . . . ? N2 Os1 N4 C24 37.6(18) . . . . ? N6 Os1 N5 C40 -5.1(4) . . . . ? N1 Os1 N5 C40 178.4(4) . . . . ? N3 Os1 N5 C40 32.1(16) . . . . ? N4 Os1 N5 C40 78.8(5) . . . . ? N2 Os1 N5 C40 -103.9(5) . . . . ? N6 Os1 N5 C37 177.0(6) . . . . ? N1 Os1 N5 C37 0.5(6) . . . . ? N3 Os1 N5 C37 -145.9(12) . . . . ? N4 Os1 N5 C37 -99.1(6) . . . . ? N2 Os1 N5 C37 78.2(6) . . . . ? N1 Os1 N6 C42 -141.8(17) . . . . ? N5 Os1 N6 C42 -176.4(6) . . . . ? N3 Os1 N6 C42 8.9(6) . . . . ? N4 Os1 N6 C42 86.0(6) . . . . ? N2 Os1 N6 C42 -87.7(6) . . . . ? N1 Os1 N6 C41 41(2) . . . . ? N5 Os1 N6 C41 6.3(4) . . . . ? N3 Os1 N6 C41 -168.3(5) . . . . ? N4 Os1 N6 C41 -91.2(5) . . . . ? N2 Os1 N6 C41 95.1(5) . . . . ? O2 Nd1 N7 C44 -42.7(7) . . . . ? O1 Nd1 N7 C44 -163.5(5) . . . . ? O6 Nd1 N7 C44 25.1(6) . . . . ? O4 Nd1 N7 C44 96.9(6) . . . . ? O5 Nd1 N7 C44 -42.1(6) . . . . ? O3 Nd1 N7 C44 88.9(6) . . . . ? O7 Nd1 N7 C44 -111.8(6) . . . . ? N8 Nd1 N7 C44 174.6(6) . . . . ? O2 Nd1 N7 C41 145.1(5) . . . . ? O1 Nd1 N7 C41 24.4(6) . . . . ? O6 Nd1 N7 C41 -147.1(5) . . . . ? O4 Nd1 N7 C41 -75.2(5) . . . . ? O5 Nd1 N7 C41 145.8(5) . . . . ? O3 Nd1 N7 C41 -83.2(5) . . . . ? O7 Nd1 N7 C41 76.1(5) . . . . ? N8 Nd1 N7 C41 2.5(5) . . . . ? O2 Nd1 N8 C40 -142.6(4) . . . . ? O1 Nd1 N8 C40 -164.9(5) . . . . ? O6 Nd1 N8 C40 50.1(6) . . . . ? O4 Nd1 N8 C40 71.9(5) . . . . ? O5 Nd1 N8 C40 -41.7(5) . . . . ? O3 Nd1 N8 C40 131.4(5) . . . . ? O7 Nd1 N8 C40 -88.6(5) . . . . ? N7 Nd1 N8 C40 -1.1(4) . . . . ? O2 Nd1 N8 C39 37.5(7) . . . . ? O1 Nd1 N8 C39 15.2(6) . . . . ? O6 Nd1 N8 C39 -129.7(6) . . . . ? O4 Nd1 N8 C39 -108.0(6) . . . . ? O5 Nd1 N8 C39 138.5(5) . . . . ? O3 Nd1 N8 C39 -48.5(6) . . . . ? O7 Nd1 N8 C39 91.5(6) . . . . ? N7 Nd1 N8 C39 179.0(6) . . . . ? C5 N1 C1 C2 -2.0(10) . . . . ? Os1 N1 C1 C2 177.6(5) . . . . ? N1 C1 C2 C3 1.1(11) . . . . ? C1 C2 C3 C4 0.0(10) . . . . ? C1 C2 C3 C11 178.7(6) . . . . ? C2 C3 C4 C5 -0.1(9) . . . . ? C11 C3 C4 C5 -178.9(6) . . . . ? C1 N1 C5 C4 1.8(9) . . . . ? Os1 N1 C5 C4 -177.9(5) . . . . ? C1 N1 C5 C6 -179.6(5) . . . . ? Os1 N1 C5 C6 0.7(7) . . . . ? C3 C4 C5 N1 -0.8(9) . . . . ? C3 C4 C5 C6 -179.2(6) . . . . ? C10 N2 C6 C7 0.9(9) . . . . ? Os1 N2 C6 C7 -177.0(5) . . . . ? C10 N2 C6 C5 179.0(5) . . . . ? Os1 N2 C6 C5 1.1(7) . . . . ? N1 C5 C6 N2 -1.1(8) . . . . ? C4 C5 C6 N2 177.4(6) . . . . ? N1 C5 C6 C7 176.8(6) . . . . ? C4 C5 C6 C7 -4.6(10) . . . . ? N2 C6 C7 C8 -0.2(10) . . . . ? C5 C6 C7 C8 -178.0(6) . . . . ? C6 C7 C8 C9 -0.7(9) . . . . ? C6 C7 C8 C15 178.4(6) . . . . ? C7 C8 C9 C10 0.7(10) . . . . ? C15 C8 C9 C10 -178.3(6) . . . . ? C6 N2 C10 C9 -0.8(10) . . . . ? Os1 N2 C10 C9 176.9(5) . . . . ? C8 C9 C10 N2 0.0(10) . . . . ? C2 C3 C11 C14 -112.7(7) . . . . ? C4 C3 C11 C14 65.9(8) . . . . ? C2 C3 C11 C13 127.2(7) . . . . ? C4 C3 C11 C13 -54.1(8) . . . . ? C2 C3 C11 C12 7.6(9) . . . . ? C4 C3 C11 C12 -173.7(6) . . . . ? C9 C8 C15 C17 -124.1(7) . . . . ? C7 C8 C15 C17 56.9(9) . . . . ? C9 C8 C15 C18 -3.5(9) . . . . ? C7 C8 C15 C18 177.5(6) . . . . ? C9 C8 C15 C16 116.7(7) . . . . ? C7 C8 C15 C16 -62.4(8) . . . . ? C23 N3 C19 C20 -2.1(10) . . . . ? Os1 N3 C19 C20 172.2(5) . . . . ? N3 C19 C20 C21 -2.2(11) . . . . ? C19 C20 C21 C22 4.1(10) . . . . ? C19 C20 C21 C29 -176.1(7) . . . . ? C20 C21 C22 C23 -1.8(10) . . . . ? C29 C21 C22 C23 178.4(6) . . . . ? C19 N3 C23 C22 4.4(9) . . . . ? Os1 N3 C23 C22 -170.4(5) . . . . ? C19 N3 C23 C24 -174.8(6) . . . . ? Os1 N3 C23 C24 10.3(7) . . . . ? C21 C22 C23 N3 -2.5(10) . . . . ? C21 C22 C23 C24 176.7(6) . . . . ? C28 N4 C24 C25 -3.6(10) . . . . ? Os1 N4 C24 C25 173.4(5) . . . . ? C28 N4 C24 C23 175.6(6) . . . . ? Os1 N4 C24 C23 -7.5(7) . . . . ? N3 C23 C24 N4 -1.8(8) . . . . ? C22 C23 C24 N4 179.0(6) . . . . ? N3 C23 C24 C25 177.4(7) . . . . ? C22 C23 C24 C25 -1.9(11) . . . . ? N4 C24 C25 C26 1.9(12) . . . . ? C23 C24 C25 C26 -177.2(7) . . . . ? C24 C25 C26 C27 0.9(13) . . . . ? C24 C25 C26 C33' 165.5(16) . . . . ? C24 C25 C26 C33 -170.8(9) . . . . ? C25 C26 C27 C28 -1.9(13) . . . . ? C33' C26 C27 C28 -168.1(14) . . . . ? C33 C26 C27 C28 169.1(10) . . . . ? C24 N4 C28 C27 2.7(10) . . . . ? Os1 N4 C28 C27 -174.0(6) . . . . ? C26 C27 C28 N4 0.1(13) . . . . ? C22 C21 C29 C30 -9.4(11) . . . . ? C20 C21 C29 C30 170.8(7) . . . . ? C22 C21 C29 C32 113.2(9) . . . . ? C20 C21 C29 C32 -66.6(9) . . . . ? C22 C21 C29 C31 -127.3(8) . . . . ? C20 C21 C29 C31 52.9(9) . . . . ? C27 C26 C33 C35 12.4(17) . . . . ? C25 C26 C33 C35 -176.7(10) . . . . ? C33' C26 C33 C35 -58(3) . . . . ? C27 C26 C33 C36 138.4(12) . . . . ? C25 C26 C33 C36 -50.7(15) . . . . ? C33' C26 C33 C36 68(3) . . . . ? C27 C26 C33 C34 -105.9(14) . . . . ? C25 C26 C33 C34 65.0(14) . . . . ? C33' C26 C33 C34 -176(4) . . . . ? C27 C26 C33' C36' 137.7(19) . . . . ? C25 C26 C33' C36' -27(3) . . . . ? C33 C26 C33' C36' -100(4) . . . . ? C27 C26 C33' C35' 11(3) . . . . ? C25 C26 C33' C35' -154(2) . . . . ? C33 C26 C33' C35' 133(5) . . . . ? C27 C26 C33' C34' -103.3(19) . . . . ? C25 C26 C33' C34' 92(2) . . . . ? C33 C26 C33' C34' 19(3) . . . . ? C40 N5 C37 C38 -0.4(10) . . . . ? Os1 N5 C37 C38 177.6(6) . . . . ? N5 C37 C38 C39 0.0(11) . . . . ? C40 N8 C39 C38 -2.0(11) . . . . ? Nd1 N8 C39 C38 177.8(6) . . . . ? C37 C38 C39 N8 1.3(12) . . . . ? C39 N8 C40 N5 1.7(10) . . . . ? Nd1 N8 C40 N5 -178.2(5) . . . . ? C39 N8 C40 C41 179.8(6) . . . . ? Nd1 N8 C40 C41 -0.1(8) . . . . ? C37 N5 C40 N8 -0.5(9) . . . . ? Os1 N5 C40 N8 -178.7(5) . . . . ? C37 N5 C40 C41 -178.6(6) . . . . ? Os1 N5 C40 C41 3.2(7) . . . . ? C44 N7 C41 N6 2.1(10) . . . . ? Nd1 N7 C41 N6 174.8(5) . . . . ? C44 N7 C41 C40 -176.4(6) . . . . ? Nd1 N7 C41 C40 -3.7(8) . . . . ? C42 N6 C41 N7 -2.7(10) . . . . ? Os1 N6 C41 N7 174.9(5) . . . . ? C42 N6 C41 C40 175.9(6) . . . . ? Os1 N6 C41 C40 -6.5(7) . . . . ? N8 C40 C41 N7 2.6(9) . . . . ? N5 C40 C41 N7 -179.2(6) . . . . ? N8 C40 C41 N6 -176.1(6) . . . . ? N5 C40 C41 N6 2.2(8) . . . . ? C41 N6 C42 C43 1.2(10) . . . . ? Os1 N6 C42 C43 -176.0(6) . . . . ? N6 C42 C43 C44 0.5(12) . . . . ? C41 N7 C44 C43 -0.1(11) . . . . ? Nd1 N7 C44 C43 -172.5(6) . . . . ? C42 C43 C44 N7 -1.1(12) . . . . ? Nd1 O1 C46 C47 -4.6(13) . . . . ? Nd1 O1 C46 C45 175.6(4) . . . . ? F14' C45 C46 O1 -129.4(8) . . . . ? F15 C45 C46 O1 145.2(8) . . . . ? F13 C45 C46 O1 20.3(9) . . . . ? F13' C45 C46 O1 -5.2(9) . . . . ? F15' C45 C46 O1 112.1(8) . . . . ? F14 C45 C46 O1 -95.5(9) . . . . ? F14' C45 C46 C47 50.8(10) . . . . ? F15 C45 C46 C47 -34.7(10) . . . . ? F13 C45 C46 C47 -159.5(8) . . . . ? F13' C45 C46 C47 174.9(8) . . . . ? F15' C45 C46 C47 -67.7(9) . . . . ? F14 C45 C46 C47 84.6(9) . . . . ? O1 C46 C47 C48 -1.3(13) . . . . ? C45 C46 C47 C48 178.5(6) . . . . ? Nd1 O2 C48 C47 7.1(12) . . . . ? Nd1 O2 C48 C49 -171.7(5) . . . . ? C46 C47 C48 O2 0.1(13) . . . . ? C46 C47 C48 C49 178.9(7) . . . . ? O2 C48 C49 F16 -43.4(10) . . . . ? C47 C48 C49 F16 137.7(8) . . . . ? O2 C48 C49 F17 -164.9(7) . . . . ? C47 C48 C49 F17 16.2(11) . . . . ? O2 C48 C49 F18 75.7(9) . . . . ? C47 C48 C49 F18 -103.3(9) . . . . ? Nd1 O3 C51 C52 19.6(13) . . . . ? Nd1 O3 C51 C50 -158.9(6) . . . . ? F19 C50 C51 O3 54.7(11) . . . . ? F21 C50 C51 O3 179.6(8) . . . . ? F20 C50 C51 O3 -61.9(11) . . . . ? F19 C50 C51 C52 -124.0(10) . . . . ? F21 C50 C51 C52 0.9(13) . . . . ? F20 C50 C51 C52 119.3(9) . . . . ? O3 C51 C52 C53 2.3(15) . . . . ? C50 C51 C52 C53 -179.2(9) . . . . ? Nd1 O4 C53 C52 -21.7(15) . . . . ? Nd1 O4 C53 C54 155.8(7) . . . . ? C51 C52 C53 O4 -1.3(16) . . . . ? C51 C52 C53 C54 -178.7(9) . . . . ? O4 C53 C54 F22 31.6(15) . . . . ? C52 C53 C54 F22 -150.7(11) . . . . ? O4 C53 C54 F24 156.2(10) . . . . ? C52 C53 C54 F24 -26.0(15) . . . . ? O4 C53 C54 F23 -90.1(12) . . . . ? C52 C53 C54 F23 87.6(13) . . . . ? Nd1 O5 C56 C57 -19.8(15) . . . . ? Nd1 O5 C56 C55 158.6(8) . . . . ? F27 C55 C56 O5 -68.2(16) . . . . ? F26 C55 C56 O5 165.0(10) . . . . ? F25 C55 C56 O5 53.2(15) . . . . ? F27 C55 C56 C57 110.3(15) . . . . ? F26 C55 C56 C57 -16.5(18) . . . . ? F25 C55 C56 C57 -128.3(12) . . . . ? O5 C56 C57 C58 -3.4(17) . . . . ? C55 C56 C57 C58 178.3(11) . . . . ? Nd1 O6 C58 C57 22.4(17) . . . . ? Nd1 O6 C58 C59' -161.3(7) . . . . ? Nd1 O6 C58 C59 -149.9(6) . . . . ? C56 C57 C58 O6 2.0(18) . . . . ? C56 C57 C58 C59' -174.2(10) . . . . ? C56 C57 C58 C59 173.8(9) . . . . ? F30' C59' C58 O6 -137.0(10) . . . . ? F28' C59' C58 O6 -12.2(14) . . . . ? F29' C59' C58 O6 107.1(11) . . . . ? F30' C59' C58 C57 39.8(13) . . . . ? F28' C59' C58 C57 164.5(11) . . . . ? F29' C59' C58 C57 -76.1(12) . . . . ? F30' C59' C58 C59 140(4) . . . . ? F28' C59' C58 C59 -95(3) . . . . ? F29' C59' C58 C59 24(3) . . . . ? F29 C59 C58 O6 61.6(11) . . . . ? F28 C59 C58 O6 -56.7(10) . . . . ? F30 C59 C58 O6 -173.7(8) . . . . ? F29 C59 C58 C57 -111.6(11) . . . . ? F28 C59 C58 C57 130.2(10) . . . . ? F30 C59 C58 C57 13.1(13) . . . . ? F29 C59 C58 C59' 163(4) . . . . ? F28 C59 C58 C59' 45(3) . . . . ? F30 C59 C58 C59' -72(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.913 _refine_diff_density_min -1.260 _refine_diff_density_rms 0.177 #===END