# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Eric McInnes' _publ_contact_author_address ; School of Chemistry University of Manchester Oxford Road Manchester M13 9PL UNITED KINGDOM ; _publ_contact_author_email ERIC.MCINNES@MANCHESTER.AC.UK _publ_section_title ; Large spin, magnetically anisotropic, octametallic vanadium(III) clusters with strong ferromagnetic interactions ; loop_ _publ_author_name 'E. McInnes' 'Anne-Laure Barra' 'D. Collison' 'Rachel Shaw' 'Floriana Tuna' 'Wolfgang Wernsdorfer' # Attachment '1.cif' data_sad1 _database_code_depnum_ccdc_archive 'CCDC 654038' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H168 Cl6 N26 O16 V8' _chemical_formula_weight 2802.98 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.4394(5) _cell_length_b 20.0945(7) _cell_length_c 22.9242(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.395(3) _cell_angle_gamma 90.00 _cell_volume 6610.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15694 _cell_measurement_theta_min 2.6758 _cell_measurement_theta_max 31.9592 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.4134 _exptl_crystal_size_mid 0.2967 _exptl_crystal_size_min 0.2140 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.635 _exptl_absorpt_correction_T_max 0.773 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalliber 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43757 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 24.72 _reflns_number_total 11239 _reflns_number_gt 7499 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. Data was processed to a resolution of 0.8 angstroms. All non hydrogen atoms were refined anisotropically. The pivalate methyl groups C8, C9 and C10 are disordered over two sites. Displacement and geometrical restraints were applied to the thermal parameters of C7, C8, C9 and C10. The butyl chains of the tetrabutylammonium group show some disorder, carbons C66, C67 and C75 are disordered over two sites. Displacement and geometrical restraints were applied to the thermal parameters of C66 and C67. Displacement and geometrical restraints were applied to O1S, C1S, C2S, C3S, C4S, O2S, C5S, C6S, C7S and C8S of the two tetrahydrofuran molecules. All hydrogens were included in calculated positions using the riding model. 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^)+(0.1104P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11239 _refine_ls_number_parameters 847 _refine_ls_number_restraints 175 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1637 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 1.005 _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 V1 V 0.44254(5) 0.92976(3) 0.01071(3) 0.01578(18) Uani 1 1 d . . 1 V2 V 0.36025(5) 0.77886(4) -0.03507(3) 0.01926(19) Uani 1 1 d . A 1 V3 V 0.32225(5) 0.83242(3) 0.09700(3) 0.01755(18) Uani 1 1 d . A 1 V4 V 0.67432(5) 0.93824(4) 0.05068(3) 0.01849(19) Uani 1 1 d . A 1 Cl1 Cl 0.35402(8) 0.70401(6) -0.11480(5) 0.0283(3) Uani 1 1 d . A 1 Cl2 Cl 0.26347(7) 0.83373(6) 0.18853(4) 0.0259(3) Uani 1 1 d . A 1 Cl3 Cl 0.81163(7) 0.88646(6) 0.09367(5) 0.0273(3) Uani 1 1 d . A 1 O1 O 0.56772(18) 0.97633(13) 0.01898(11) 0.0173(6) Uani 1 1 d . . 1 O2 O 0.37230(18) 0.84378(13) 0.02453(11) 0.0167(6) Uani 1 1 d . A 1 O3 O 0.3917(2) 0.70342(16) 0.02087(15) 0.0350(8) Uani 1 1 d . A 1 O4 O 0.3737(2) 0.73947(15) 0.10844(14) 0.0288(7) Uani 1 1 d . A 1 O5 O 0.2238(2) 0.76428(16) -0.03088(13) 0.0278(7) Uani 1 1 d . A 1 O6 O 0.2013(2) 0.79334(15) 0.05984(12) 0.0260(7) Uani 1 1 d . A 1 N21 N 0.5044(2) 0.79650(17) -0.03897(14) 0.0189(8) Uani 1 1 d . A 1 N22 N 0.5353(2) 0.85465(18) -0.01615(15) 0.0204(8) Uani 1 1 d . A 1 N23 N 0.6273(2) 0.85541(18) -0.00346(14) 0.0195(8) Uani 1 1 d . A 1 N31 N 0.4521(2) 0.87073(16) 0.13441(14) 0.0171(8) Uani 1 1 d . A 1 N32 N 0.5011(2) 0.90092(17) 0.09696(14) 0.0166(8) Uani 1 1 d . A 1 N33 N 0.5916(2) 0.90505(17) 0.11658(14) 0.0203(8) Uani 1 1 d . A 1 N41 N 0.3252(2) 0.86090(18) -0.09143(14) 0.0192(8) Uani 1 1 d . A 1 N42 N 0.3522(2) 0.91940(17) -0.06973(15) 0.0186(8) Uani 1 1 d . . 1 N43 N 0.6978(2) 1.03060(17) 0.09560(14) 0.0186(8) Uani 1 1 d . . 1 N51 N 0.2691(2) 0.92940(17) 0.07782(15) 0.0200(8) Uani 1 1 d . . 1 N52 N 0.3154(2) 0.96464(17) 0.04210(14) 0.0178(8) Uani 1 1 d . . 1 N53 N 0.7333(2) 0.98304(17) -0.02042(15) 0.0200(8) Uani 1 1 d . . 1 C1 C 0.3912(3) 0.6954(3) 0.0735(2) 0.0353(12) Uani 1 1 d . A 1 C2 C 0.4055(3) 0.6254(2) 0.0991(2) 0.0330(12) Uani 1 1 d . A 1 C3 C 0.3078(4) 0.5948(3) 0.0953(3) 0.0607(18) Uani 1 1 d . A 1 H3A H 0.3124 0.5491 0.1075 0.091 Uiso 1 1 calc R A 1 H3B H 0.2789 0.5972 0.0555 0.091 Uiso 1 1 calc R A 1 H3C H 0.2708 0.6189 0.1205 0.091 Uiso 1 1 calc R A 1 C4 C 0.4499(4) 0.6252(3) 0.1608(2) 0.0528(16) Uani 1 1 d . A 1 H4A H 0.5119 0.6427 0.1622 0.079 Uiso 1 1 calc R A 1 H4B H 0.4524 0.5805 0.1755 0.079 Uiso 1 1 calc R A 1 H4C H 0.4140 0.6523 0.1844 0.079 Uiso 1 1 calc R A 1 C5 C 0.4647(5) 0.5839(3) 0.0592(3) 0.0597(17) Uani 1 1 d . A 1 H5A H 0.5275 0.6003 0.0632 0.090 Uiso 1 1 calc R A 1 H5B H 0.4383 0.5880 0.0190 0.090 Uiso 1 1 calc R A 1 H5C H 0.4645 0.5380 0.0707 0.090 Uiso 1 1 calc R A 1 C6 C 0.1749(3) 0.7689(2) 0.0106(2) 0.0257(10) Uani 1 1 d . A 1 C7 C 0.0756(3) 0.7412(3) 0.0009(2) 0.0350(10) Uani 1 1 d U A 1 C8X C 0.0794(7) 0.6730(5) 0.0283(5) 0.0506(18) Uani 0.608(8) 1 d PU A 1 H8A H 0.1079 0.6759 0.0681 0.076 Uiso 0.608(8) 1 calc PR A 1 H8B H 0.1154 0.6439 0.0064 0.076 Uiso 0.608(8) 1 calc PR A 1 H8C H 0.0173 0.6558 0.0278 0.076 Uiso 0.608(8) 1 calc PR A 1 C9X C 0.0136(6) 0.7863(5) 0.0387(4) 0.0416(18) Uani 0.608(8) 1 d PU A 1 H9A H -0.0478 0.7676 0.0374 0.062 Uiso 0.608(8) 1 calc PR A 1 H9B H 0.0096 0.8305 0.0229 0.062 Uiso 0.608(8) 1 calc PR A 1 H9C H 0.0418 0.7877 0.0787 0.062 Uiso 0.608(8) 1 calc PR A 1 C10X C 0.0376(8) 0.7450(6) -0.0610(5) 0.047(2) Uani 0.608(8) 1 d PU A 1 H10A H -0.0237 0.7260 -0.0658 0.071 Uiso 0.608(8) 1 calc PR A 1 H10B H 0.0773 0.7208 -0.0844 0.071 Uiso 0.608(8) 1 calc PR A 1 H10C H 0.0344 0.7907 -0.0732 0.071 Uiso 0.608(8) 1 calc PR A 1 C8Y C 0.0838(10) 0.6650(7) -0.0195(8) 0.049(3) Uani 0.392(8) 1 d PU A 2 H8D H 0.1186 0.6400 0.0113 0.074 Uiso 0.392(8) 1 calc PR A 2 H8E H 0.1152 0.6631 -0.0542 0.074 Uiso 0.392(8) 1 calc PR A 2 H8F H 0.0226 0.6462 -0.0276 0.074 Uiso 0.392(8) 1 calc PR A 2 C9Y C 0.0273(10) 0.7403(9) 0.0507(7) 0.046(2) Uani 0.392(8) 1 d PU A 2 H9D H -0.0376 0.7319 0.0390 0.069 Uiso 0.392(8) 1 calc PR A 2 H9E H 0.0342 0.7825 0.0703 0.069 Uiso 0.392(8) 1 calc PR A 2 H9F H 0.0521 0.7057 0.0768 0.069 Uiso 0.392(8) 1 calc PR A 2 C10Y C 0.0239(12) 0.7786(8) -0.0543(7) 0.041(3) Uani 0.392(8) 1 d PU A 2 H10D H -0.0358 0.7584 -0.0649 0.062 Uiso 0.392(8) 1 calc PR A 2 H10E H 0.0606 0.7754 -0.0866 0.062 Uiso 0.392(8) 1 calc PR A 2 H10F H 0.0157 0.8246 -0.0447 0.062 Uiso 0.392(8) 1 calc PR A 2 C21 C 0.5811(3) 0.7577(2) -0.04280(18) 0.0217(10) Uani 1 1 d . . . C22 C 0.5897(3) 0.6926(2) -0.06187(19) 0.0276(11) Uani 1 1 d . A . H22 H 0.5379 0.6673 -0.0755 0.033 Uiso 1 1 calc R . . C23 C 0.6783(3) 0.6675(3) -0.0596(2) 0.0367(12) Uani 1 1 d . . . H23 H 0.6868 0.6240 -0.0718 0.044 Uiso 1 1 calc R A . C24 C 0.7569(3) 0.7062(3) -0.0391(2) 0.0359(12) Uani 1 1 d . A . H24 H 0.8160 0.6878 -0.0393 0.043 Uiso 1 1 calc R . . C25 C 0.7492(3) 0.7695(2) -0.0191(2) 0.0300(11) Uani 1 1 d . . . H25 H 0.8013 0.7943 -0.0048 0.036 Uiso 1 1 calc R A . C26 C 0.6591(3) 0.7954(2) -0.02120(18) 0.0224(10) Uani 1 1 d . A . C31 C 0.5131(3) 0.8557(2) 0.18292(18) 0.0205(9) Uani 1 1 d . . . C32 C 0.4992(3) 0.8242(2) 0.23561(18) 0.0247(10) Uani 1 1 d . A . H32 H 0.4411 0.8084 0.2429 0.030 Uiso 1 1 calc R . . C33 C 0.5758(3) 0.8181(2) 0.2756(2) 0.0328(12) Uani 1 1 d . . . H33 H 0.5693 0.7980 0.3114 0.039 Uiso 1 1 calc R A . C34 C 0.6647(3) 0.8412(2) 0.2647(2) 0.0341(12) Uani 1 1 d . A . H34 H 0.7147 0.8360 0.2936 0.041 Uiso 1 1 calc R . . C35 C 0.6794(3) 0.8708(2) 0.2130(2) 0.0289(11) Uani 1 1 d . . . H35 H 0.7380 0.8857 0.2057 0.035 Uiso 1 1 calc R A . C36 C 0.6011(3) 0.8774(2) 0.17124(18) 0.0209(10) Uani 1 1 d . A . C41 C 0.2550(3) 0.8726(2) -0.13530(17) 0.0223(10) Uani 1 1 d . . . C42 C 0.2006(3) 0.8287(2) -0.17262(19) 0.0300(11) Uani 1 1 d . A . H42 H 0.2093 0.7828 -0.1707 0.036 Uiso 1 1 calc R . . C43 C 0.1338(3) 0.8573(3) -0.2122(2) 0.0337(12) Uani 1 1 d . . . H43 H 0.0964 0.8300 -0.2377 0.040 Uiso 1 1 calc R A . C44 C 0.7597(3) 1.0584(2) 0.13787(17) 0.0195(9) Uani 1 1 d . . . C45 C 0.8284(3) 1.0307(2) 0.17902(18) 0.0268(11) Uani 1 1 d . . . H45 H 0.8381 0.9849 0.1814 0.032 Uiso 1 1 calc R . . C46 C 0.8799(3) 1.0736(3) 0.2152(2) 0.0345(12) Uani 1 1 d . . . H46 H 0.9258 1.0566 0.2429 0.041 Uiso 1 1 calc R . . C51 C 0.8140(3) 1.0397(2) -0.08078(18) 0.0196(9) Uani 1 1 d . . . C52 C 0.8910(3) 1.0559(2) -0.1107(2) 0.0277(11) Uani 1 1 d . . . H52 H 0.8906 1.0931 -0.1348 0.033 Uiso 1 1 calc R . . C53 C 0.9655(3) 1.0151(3) -0.1028(2) 0.0345(12) Uani 1 1 d . . . H53 H 1.0175 1.0248 -0.1218 0.041 Uiso 1 1 calc R . . C54 C 0.9669(3) 0.9580(2) -0.0666(2) 0.0351(12) Uani 1 1 d . . . H54 H 1.0195 0.9310 -0.0628 0.042 Uiso 1 1 calc R . . C55 C 0.8932(3) 0.9417(2) -0.0372(2) 0.0292(11) Uani 1 1 d . . . H55 H 0.8938 0.9040 -0.0136 0.035 Uiso 1 1 calc R . . C56 C 0.8166(3) 0.9846(2) -0.04437(18) 0.0210(10) Uani 1 1 d . . . N60 N 0.0031(3) 0.7153(2) 0.24364(19) 0.0399(11) Uani 1 1 d . . . C60 C -0.0577(4) 0.7073(3) 0.1855(3) 0.0499(15) Uani 1 1 d . . . H60A H -0.0388 0.7403 0.1583 0.060 Uiso 1 1 calc R . . H60B H -0.0457 0.6638 0.1697 0.060 Uiso 1 1 calc R . . C61 C -0.1615(4) 0.7141(3) 0.1880(3) 0.0601(17) Uani 1 1 d . . . H61A H -0.1827 0.6800 0.2134 0.072 Uiso 1 1 calc R . . H61B H -0.1753 0.7572 0.2039 0.072 Uiso 1 1 calc R . . C62 C -0.2111(5) 0.7068(4) 0.1271(3) 0.069(2) Uani 1 1 d . . . H62A H -0.1906 0.6659 0.1100 0.083 Uiso 1 1 calc R . . H62B H -0.1932 0.7434 0.1032 0.083 Uiso 1 1 calc R . . C63 C -0.3159(5) 0.7055(4) 0.1247(3) 0.077(2) Uani 1 1 d . . . H63A H -0.3343 0.6713 0.1503 0.115 Uiso 1 1 calc R . . H63B H -0.3426 0.6966 0.0852 0.115 Uiso 1 1 calc R . . H63C H -0.3376 0.7479 0.1370 0.115 Uiso 1 1 calc R . . C64 C -0.0276(4) 0.6675(3) 0.2892(3) 0.0458(14) Uani 1 1 d . C . H64A H 0.0154 0.6716 0.3247 0.055 Uiso 1 1 calc R . . H64B H -0.0885 0.6813 0.2987 0.055 Uiso 1 1 calc R . . C65 C -0.0331(5) 0.5954(3) 0.2721(3) 0.071(2) Uani 1 1 d . . . H65A H -0.0965 0.5861 0.2554 0.085 Uiso 1 1 calc R B 1 H65B H 0.0068 0.5885 0.2412 0.085 Uiso 1 1 calc R B 1 C66X C -0.0072(7) 0.5464(4) 0.3185(4) 0.0428(19) Uani 0.671(10) 1 d PU C 1 H66A H -0.0593 0.5433 0.3416 0.051 Uiso 0.671(10) 1 calc PR C 1 H66B H -0.0025 0.5037 0.2993 0.051 Uiso 0.671(10) 1 calc PR C 1 C67X C 0.0692(8) 0.5531(5) 0.3562(5) 0.063(2) Uani 0.671(10) 1 d PU C 1 H67A H 0.1220 0.5364 0.3388 0.094 Uiso 0.671(10) 1 calc PR C 1 H67B H 0.0620 0.5285 0.3913 0.094 Uiso 0.671(10) 1 calc PR C 1 H67C H 0.0787 0.5993 0.3658 0.094 Uiso 0.671(10) 1 calc PR C 1 C66Y C 0.0264(16) 0.5532(9) 0.2926(9) 0.052(2) Uani 0.329(10) 1 d PU C 2 H66C H 0.0413 0.5310 0.2573 0.062 Uiso 0.329(10) 1 calc PR C 2 H66D H -0.0121 0.5217 0.3111 0.062 Uiso 0.329(10) 1 calc PR C 2 C67Y C 0.1133(15) 0.5485(9) 0.3298(8) 0.050(3) Uani 0.329(10) 1 d PU C 2 H67D H 0.1638 0.5474 0.3059 0.075 Uiso 0.329(10) 1 calc PR C 2 H67E H 0.1138 0.5086 0.3528 0.075 Uiso 0.329(10) 1 calc PR C 2 H67F H 0.1201 0.5864 0.3554 0.075 Uiso 0.329(10) 1 calc PR C 2 C68 C 0.1028(4) 0.7023(3) 0.2324(3) 0.0432(14) Uani 1 1 d . . . H68A H 0.1070 0.6565 0.2195 0.052 Uiso 1 1 calc R . . H68B H 0.1166 0.7305 0.2002 0.052 Uiso 1 1 calc R . . C69 C 0.1770(4) 0.7132(3) 0.2827(2) 0.0404(13) Uani 1 1 d . . . H69A H 0.1572 0.6943 0.3182 0.048 Uiso 1 1 calc R . . H69B H 0.1866 0.7606 0.2890 0.048 Uiso 1 1 calc R . . C70 C 0.2681(4) 0.6807(3) 0.2698(3) 0.0486(15) Uani 1 1 d . . . H70A H 0.2584 0.6332 0.2648 0.058 Uiso 1 1 calc R . . H70B H 0.2860 0.6984 0.2334 0.058 Uiso 1 1 calc R . . C71 C 0.3466(4) 0.6926(3) 0.3186(3) 0.0589(17) Uani 1 1 d . . . H71A H 0.3594 0.7394 0.3218 0.088 Uiso 1 1 calc R . . H71B H 0.4015 0.6695 0.3096 0.088 Uiso 1 1 calc R . . H71C H 0.3285 0.6764 0.3550 0.088 Uiso 1 1 calc R . . C72 C -0.0068(4) 0.7851(2) 0.2677(2) 0.0401(13) Uani 1 1 d . . . H72A H -0.0698 0.7903 0.2778 0.048 Uiso 1 1 calc R . . H72B H 0.0351 0.7893 0.3036 0.048 Uiso 1 1 calc R . . C73 C 0.0131(4) 0.8411(2) 0.2269(3) 0.0451(14) Uani 1 1 d . D . H73A H -0.0346 0.8421 0.1936 0.054 Uiso 1 1 calc R . . H73B H 0.0727 0.8336 0.2123 0.054 Uiso 1 1 calc R . . C74 C 0.0150(7) 0.9078(3) 0.2590(4) 0.073(2) Uani 1 1 d . . . C75X C 0.0865(9) 0.9159(5) 0.2961(5) 0.067(4) Uani 0.643(11) 1 d P D 1 H75A H 0.0819 0.9578 0.3157 0.101 Uiso 0.643(11) 1 calc PR D 1 H75B H 0.1415 0.9157 0.2761 0.101 Uiso 0.643(11) 1 calc PR D 1 H75C H 0.0899 0.8805 0.3243 0.101 Uiso 0.643(11) 1 calc PR D 1 C75Y C -0.0452(11) 0.9267(7) 0.2979(7) 0.042(5) Uani 0.357(11) 1 d P D 2 H75D H -0.0515 0.8913 0.3253 0.063 Uiso 0.357(11) 1 calc PR D 2 H75E H -0.1050 0.9366 0.2770 0.063 Uiso 0.357(11) 1 calc PR D 2 H75F H -0.0214 0.9656 0.3188 0.063 Uiso 0.357(11) 1 calc PR D 2 O1S O 0.8520(5) 0.5408(5) 0.1330(4) 0.173(2) Uani 1 1 d DU . . C1S C 0.8228(8) 0.5185(7) 0.0703(5) 0.174(2) Uani 1 1 d DU . . H1S1 H 0.8239 0.5551 0.0428 0.209 Uiso 1 1 calc R . . H1S2 H 0.8620 0.4828 0.0588 0.209 Uiso 1 1 calc R . . C2S C 0.7293(8) 0.4960(7) 0.0747(5) 0.174(2) Uani 1 1 d DU . . H2S1 H 0.6860 0.5275 0.0546 0.209 Uiso 1 1 calc R . . H2S2 H 0.7203 0.4536 0.0547 0.209 Uiso 1 1 calc R . . C3S C 0.7092(7) 0.4890(7) 0.1280(6) 0.174(2) Uani 1 1 d DU . . H3S1 H 0.6986 0.4424 0.1361 0.209 Uiso 1 1 calc R . . H3S2 H 0.6529 0.5136 0.1332 0.209 Uiso 1 1 calc R . . C4S C 0.7853(9) 0.5138(8) 0.1671(5) 0.173(2) Uani 1 1 d DU . . H4S1 H 0.7637 0.5478 0.1923 0.208 Uiso 1 1 calc R . . H4S2 H 0.8130 0.4780 0.1915 0.208 Uiso 1 1 calc R . . O2S O 0.8639(8) 0.5709(4) 0.9092(4) 0.188(3) Uani 1 1 d DU . . C5S C 0.8635(10) 0.5922(5) 0.8500(5) 0.148(5) Uani 1 1 d D . . H5S1 H 0.8050 0.6142 0.8370 0.178 Uiso 1 1 calc R . . H5S2 H 0.9137 0.6237 0.8470 0.178 Uiso 1 1 calc R . . C6S C 0.8751(11) 0.5361(5) 0.8141(4) 0.187(3) Uani 1 1 d DU . . H6S1 H 0.9239 0.5447 0.7892 0.225 Uiso 1 1 calc R . . H6S2 H 0.8177 0.5274 0.7890 0.225 Uiso 1 1 calc R . . C7S C 0.8990(10) 0.4800(5) 0.8502(5) 0.182(3) Uani 1 1 d DU . . H7S1 H 0.9586 0.4614 0.8427 0.218 Uiso 1 1 calc R . . H7S2 H 0.8516 0.4457 0.8446 0.218 Uiso 1 1 calc R . . C8S C 0.9041(11) 0.5096(6) 0.9105(6) 0.191(3) Uani 1 1 d DU . . H8S1 H 0.8726 0.4805 0.9357 0.229 Uiso 1 1 calc R . . H8S2 H 0.9688 0.5132 0.9268 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 V1 0.0132(4) 0.0209(4) 0.0132(4) 0.0047(3) 0.0012(3) 0.0001(3) V2 0.0181(4) 0.0234(4) 0.0161(4) -0.0007(3) 0.0013(3) -0.0001(3) V3 0.0185(4) 0.0203(4) 0.0142(4) 0.0019(3) 0.0035(3) -0.0025(3) V4 0.0130(4) 0.0236(4) 0.0185(4) 0.0069(3) 0.0003(3) 0.0010(3) Cl1 0.0277(6) 0.0325(6) 0.0238(6) -0.0082(5) -0.0008(5) 0.0030(5) Cl2 0.0283(6) 0.0328(6) 0.0178(5) 0.0036(5) 0.0083(5) -0.0026(5) Cl3 0.0177(5) 0.0326(6) 0.0303(6) 0.0084(5) -0.0024(5) 0.0032(5) O1 0.0135(14) 0.0203(15) 0.0179(14) 0.0036(12) 0.0014(12) -0.0008(12) O2 0.0159(15) 0.0196(15) 0.0145(14) 0.0016(12) 0.0015(12) -0.0011(12) O3 0.041(2) 0.0295(19) 0.033(2) 0.0099(16) -0.0028(16) -0.0032(16) O4 0.0299(18) 0.0253(18) 0.0320(18) -0.0025(15) 0.0067(15) 0.0016(14) O5 0.0210(17) 0.0367(19) 0.0264(17) -0.0038(15) 0.0055(14) -0.0041(14) O6 0.0239(17) 0.0340(18) 0.0198(16) -0.0013(14) 0.0007(13) -0.0067(14) N21 0.0168(18) 0.024(2) 0.0169(18) -0.0002(15) 0.0046(15) -0.0009(16) N22 0.0163(19) 0.028(2) 0.0168(18) 0.0055(16) 0.0015(15) 0.0001(16) N23 0.0154(19) 0.025(2) 0.0182(18) 0.0077(15) 0.0032(15) 0.0015(15) N31 0.0192(19) 0.0201(19) 0.0120(17) 0.0024(15) 0.0017(15) -0.0012(15) N32 0.0133(18) 0.0208(19) 0.0155(17) 0.0028(15) 0.0002(14) -0.0013(15) N33 0.021(2) 0.023(2) 0.0161(18) 0.0074(15) -0.0010(15) -0.0014(16) N41 0.0158(18) 0.026(2) 0.0149(18) 0.0000(16) -0.0003(15) 0.0002(15) N42 0.0159(18) 0.025(2) 0.0153(18) 0.0061(15) 0.0029(14) -0.0016(15) N43 0.0150(18) 0.025(2) 0.0155(17) 0.0064(16) 0.0006(15) 0.0023(15) N51 0.0202(19) 0.025(2) 0.0156(18) 0.0015(15) 0.0061(15) -0.0042(16) N52 0.0172(18) 0.0199(19) 0.0166(18) 0.0027(15) 0.0032(15) -0.0007(15) N53 0.0151(18) 0.025(2) 0.0192(18) 0.0052(16) -0.0005(15) -0.0006(15) C1 0.023(3) 0.041(3) 0.041(3) 0.004(3) 0.000(2) -0.006(2) C2 0.030(3) 0.031(3) 0.036(3) 0.008(2) -0.006(2) 0.002(2) C3 0.066(4) 0.045(4) 0.069(4) 0.012(3) -0.005(4) -0.010(3) C4 0.065(4) 0.048(4) 0.044(3) 0.009(3) -0.002(3) 0.012(3) C5 0.070(4) 0.055(4) 0.054(4) 0.002(3) 0.007(3) 0.024(3) C6 0.023(2) 0.026(3) 0.027(3) 0.005(2) 0.000(2) -0.002(2) C7 0.020(2) 0.043(2) 0.042(2) 0.001(2) 0.0032(18) -0.0065(19) C8X 0.045(4) 0.042(3) 0.065(4) 0.004(3) 0.007(4) -0.011(3) C9X 0.020(4) 0.059(4) 0.045(4) -0.007(4) -0.003(3) 0.000(3) C10X 0.033(4) 0.066(5) 0.042(2) -0.006(3) 0.001(3) -0.010(5) C8Y 0.037(5) 0.044(5) 0.066(6) 0.001(5) 0.002(5) -0.012(5) C9Y 0.033(4) 0.052(5) 0.052(5) -0.002(5) 0.004(4) -0.013(4) C10Y 0.027(5) 0.049(6) 0.048(5) 0.002(5) 0.002(5) -0.003(5) C21 0.021(2) 0.029(3) 0.015(2) 0.0035(19) 0.0029(18) 0.0059(19) C22 0.025(3) 0.034(3) 0.023(2) -0.007(2) 0.001(2) 0.001(2) C23 0.035(3) 0.035(3) 0.040(3) -0.009(2) 0.002(2) 0.008(2) C24 0.023(3) 0.041(3) 0.044(3) -0.001(3) 0.003(2) 0.009(2) C25 0.022(2) 0.029(3) 0.039(3) 0.006(2) 0.005(2) 0.003(2) C26 0.021(2) 0.027(2) 0.019(2) 0.0034(19) 0.0039(18) 0.002(2) C31 0.025(2) 0.020(2) 0.016(2) 0.0019(18) -0.0003(18) 0.0014(19) C32 0.027(2) 0.030(3) 0.018(2) 0.0083(19) 0.0052(19) -0.001(2) C33 0.038(3) 0.038(3) 0.022(2) 0.016(2) 0.001(2) 0.001(2) C34 0.032(3) 0.044(3) 0.024(2) 0.010(2) -0.008(2) 0.003(2) C35 0.025(3) 0.032(3) 0.028(3) 0.009(2) -0.005(2) -0.005(2) C36 0.023(2) 0.024(2) 0.016(2) 0.0038(18) 0.0014(18) 0.0000(19) C41 0.021(2) 0.034(3) 0.012(2) 0.0012(19) 0.0025(18) 0.005(2) C42 0.030(3) 0.035(3) 0.023(2) -0.006(2) -0.003(2) 0.007(2) C43 0.032(3) 0.042(3) 0.025(3) -0.012(2) -0.010(2) 0.009(2) C44 0.014(2) 0.030(3) 0.014(2) 0.0028(18) -0.0007(17) 0.0020(19) C45 0.023(2) 0.035(3) 0.021(2) 0.003(2) 0.000(2) 0.009(2) C46 0.027(3) 0.052(3) 0.021(2) -0.003(2) -0.011(2) 0.009(2) C51 0.021(2) 0.020(2) 0.018(2) -0.0007(18) 0.0036(18) -0.0017(18) C52 0.024(2) 0.031(3) 0.031(3) 0.002(2) 0.012(2) -0.001(2) C53 0.024(3) 0.043(3) 0.039(3) 0.003(2) 0.016(2) -0.004(2) C54 0.018(2) 0.036(3) 0.052(3) 0.006(3) 0.011(2) 0.006(2) C55 0.021(2) 0.030(3) 0.036(3) 0.008(2) 0.003(2) 0.002(2) C56 0.015(2) 0.027(2) 0.021(2) 0.0012(19) 0.0037(18) -0.0005(18) N60 0.048(3) 0.030(2) 0.043(3) 0.008(2) 0.010(2) -0.001(2) C60 0.056(4) 0.038(3) 0.055(4) 0.009(3) 0.003(3) -0.003(3) C61 0.062(4) 0.047(4) 0.069(4) 0.013(3) -0.003(3) 0.009(3) C62 0.064(5) 0.062(4) 0.076(5) 0.027(4) -0.018(4) -0.011(4) C63 0.082(6) 0.064(5) 0.079(5) 0.015(4) -0.014(4) 0.000(4) C64 0.055(4) 0.031(3) 0.051(3) 0.014(3) 0.005(3) -0.007(3) C65 0.105(6) 0.031(3) 0.067(4) 0.013(3) -0.040(4) -0.019(4) C66X 0.078(6) 0.027(3) 0.029(4) 0.006(3) 0.034(3) -0.001(4) C67X 0.096(6) 0.041(4) 0.052(5) 0.011(4) 0.011(3) 0.008(4) C66Y 0.084(6) 0.034(4) 0.041(5) 0.007(4) 0.022(4) 0.004(5) C67Y 0.083(7) 0.033(5) 0.037(7) 0.012(6) 0.025(5) 0.013(6) C68 0.051(3) 0.027(3) 0.053(3) -0.001(3) 0.015(3) 0.001(3) C69 0.053(3) 0.036(3) 0.034(3) 0.010(2) 0.014(3) -0.002(3) C70 0.057(4) 0.043(3) 0.048(3) 0.010(3) 0.016(3) 0.007(3) C71 0.063(4) 0.069(4) 0.046(4) 0.014(3) 0.009(3) 0.004(3) C72 0.048(3) 0.029(3) 0.047(3) 0.008(2) 0.021(3) 0.001(2) C73 0.058(4) 0.028(3) 0.054(4) 0.012(3) 0.029(3) 0.003(3) C74 0.128(7) 0.028(3) 0.075(5) 0.002(3) 0.063(5) 0.008(4) C75X 0.119(11) 0.031(5) 0.048(6) 0.000(5) -0.007(7) 0.006(6) C75Y 0.061(11) 0.021(8) 0.047(10) 0.022(7) 0.020(8) -0.003(7) O1S 0.134(4) 0.224(5) 0.152(5) -0.059(5) -0.021(4) 0.000(4) C1S 0.136(4) 0.225(5) 0.153(5) -0.059(5) -0.022(4) 0.000(4) C2S 0.136(4) 0.225(5) 0.153(5) -0.059(5) -0.022(4) 0.000(4) C3S 0.135(4) 0.224(5) 0.153(5) -0.058(5) -0.023(4) -0.001(4) C4S 0.135(4) 0.224(5) 0.153(5) -0.058(5) -0.022(4) -0.001(4) O2S 0.280(8) 0.110(5) 0.191(6) 0.021(5) 0.104(6) 0.046(5) C5S 0.233(14) 0.122(9) 0.108(8) 0.037(7) 0.100(9) 0.012(9) C6S 0.285(8) 0.103(5) 0.199(6) 0.045(5) 0.140(7) 0.069(6) C7S 0.271(8) 0.102(5) 0.198(6) 0.046(4) 0.142(6) 0.064(5) C8S 0.278(8) 0.116(5) 0.198(6) 0.037(5) 0.111(6) 0.053(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 V1 O1 2.006(3) 3_675 ? V1 O1 2.025(3) . ? V1 O2 2.046(3) . ? V1 N32 2.142(3) . ? V1 N42 2.147(3) . ? V1 N22 2.153(4) . ? V1 N52 2.161(3) . ? V2 O2 1.883(3) . ? V2 O5 2.004(3) . ? V2 O3 2.005(3) . ? V2 N41 2.121(4) . ? V2 N21 2.123(3) . ? V2 Cl1 2.3611(13) . ? V3 O2 1.898(3) . ? V3 O6 2.015(3) . ? V3 O4 2.017(3) . ? V3 N31 2.117(3) . ? V3 N51 2.123(4) . ? V3 Cl2 2.3495(12) . ? V4 O1 1.798(3) . ? V4 N53 2.121(3) . ? V4 N43 2.131(4) . ? V4 N33 2.134(3) . ? V4 N23 2.141(4) . ? V4 Cl3 2.3558(12) . ? O1 V1 2.006(3) 3_675 ? O3 C1 1.218(6) . ? O4 C1 1.239(6) . ? O5 C6 1.250(5) . ? O6 C6 1.251(5) . ? N21 N22 1.336(5) . ? N21 C21 1.365(5) . ? N22 N23 1.328(5) . ? N23 C26 1.369(5) . ? N31 N32 1.320(4) . ? N31 C31 1.374(5) . ? N32 N33 1.336(5) . ? N33 C36 1.363(5) . ? N41 N42 1.318(5) . ? N41 C41 1.367(5) . ? N42 N43 1.336(5) 3_675 ? N43 N42 1.337(5) 3_675 ? N43 C44 1.363(5) . ? N51 N52 1.320(5) . ? N51 C51 1.360(5) 3_675 ? N52 N53 1.330(5) 3_675 ? N53 N52 1.330(5) 3_675 ? N53 C56 1.378(5) . ? C1 C2 1.530(7) . ? C2 C4 1.485(7) . ? C2 C3 1.533(7) . ? C2 C5 1.561(7) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.531(6) . ? C7 C9Y 1.404(15) . ? C7 C10X 1.463(11) . ? C7 C8X 1.506(10) . ? C7 C10Y 1.583(16) . ? C7 C9X 1.596(10) . ? C7 C8Y 1.610(15) . ? C8X H8A 0.9600 . ? C8X H8B 0.9600 . ? C8X H8C 0.9600 . ? C9X H9A 0.9600 . ? C9X H9B 0.9600 . ? C9X H9C 0.9600 . ? C10X H10A 0.9600 . ? C10X H10B 0.9600 . ? C10X H10C 0.9600 . ? C8Y H8D 0.9600 . ? C8Y H8E 0.9600 . ? C8Y H8F 0.9600 . ? C9Y H9D 0.9600 . ? C9Y H9E 0.9600 . ? C9Y H9F 0.9600 . ? C10Y H10D 0.9600 . ? C10Y H10E 0.9600 . ? C10Y H10F 0.9600 . ? C21 C22 1.390(6) . ? C21 C26 1.400(6) . ? C22 C23 1.371(7) . ? C22 H22 0.9300 . ? C23 C24 1.413(7) . ? C23 H23 0.9300 . ? C24 C25 1.361(7) . ? C24 H24 0.9300 . ? C25 C26 1.397(6) . ? C25 H25 0.9300 . ? C31 C36 1.397(6) . ? C31 C32 1.397(6) . ? C32 C33 1.361(6) . ? C32 H32 0.9300 . ? C33 C34 1.413(7) . ? C33 H33 0.9300 . ? C34 C35 1.364(6) . ? C34 H34 0.9300 . ? C35 C36 1.404(6) . ? C35 H35 0.9300 . ? C41 C44 1.402(6) 3_675 ? C41 C42 1.407(6) . ? C42 C43 1.374(6) . ? C42 H42 0.9300 . ? C43 C46 1.402(7) 3_675 ? C43 H43 0.9300 . ? C44 C41 1.402(6) 3_675 ? C44 C45 1.406(6) . ? C45 C46 1.360(6) . ? C45 H45 0.9300 . ? C46 C43 1.402(7) 3_675 ? C46 H46 0.9300 . ? C51 N51 1.359(5) 3_675 ? C51 C56 1.384(6) . ? C51 C52 1.408(6) . ? C52 C53 1.347(7) . ? C52 H52 0.9300 . ? C53 C54 1.415(7) . ? C53 H53 0.9300 . ? C54 C55 1.361(6) . ? C54 H54 0.9300 . ? C55 C56 1.397(6) . ? C55 H55 0.9300 . ? N60 C68 1.513(7) . ? N60 C72 1.518(6) . ? N60 C60 1.520(7) . ? N60 C64 1.521(6) . ? C60 C61 1.512(8) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.504(9) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.508(9) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 C65 1.501(8) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C66Y 1.26(2) . ? C65 C66X 1.467(10) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66X C67X 1.331(13) . ? C66X H66A 0.9700 . ? C66X H66B 0.9700 . ? C67X H67A 0.9600 . ? C67X H67B 0.9600 . ? C67X H67C 0.9600 . ? C66Y C67Y 1.44(3) . ? C66Y H66C 0.9700 . ? C66Y H66D 0.9700 . ? C67Y H67D 0.9600 . ? C67Y H67E 0.9600 . ? C67Y H67F 0.9600 . ? C68 C69 1.501(7) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.526(7) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.519(8) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 C73 1.511(7) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C74 1.527(8) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75X 1.272(12) . ? C74 C75Y 1.367(16) . ? C75X H75A 0.9600 . ? C75X H75B 0.9600 . ? C75X H75C 0.9600 . ? C75Y H75D 0.9600 . ? C75Y H75E 0.9600 . ? C75Y H75F 0.9600 . ? O1S C4S 1.413(12) . ? O1S C1S 1.520(11) . ? C1S C2S 1.438(12) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S C3S 1.293(12) . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C3S C4S 1.429(12) . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C4S H4S1 0.9700 . ? C4S H4S2 0.9700 . ? O2S C8S 1.359(11) . ? O2S C5S 1.423(10) . ? C5S C6S 1.417(11) . ? C5S H5S1 0.9700 . ? C5S H5S2 0.9700 . ? C6S C7S 1.419(11) . ? C6S H6S1 0.9700 . ? C6S H6S2 0.9700 . ? C7S C8S 1.498(13) . ? C7S H7S1 0.9700 . ? C7S H7S2 0.9700 . ? C8S H8S1 0.9700 . ? C8S H8S2 0.9700 . ? 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 O1 V1 O1 68.19(12) 3_675 . ? O1 V1 O2 145.88(11) 3_675 . ? O1 V1 O2 145.92(11) . . ? O1 V1 N32 125.05(12) 3_675 . ? O1 V1 N32 77.41(12) . . ? O2 V1 N32 77.30(12) . . ? O1 V1 N42 77.59(12) 3_675 . ? O1 V1 N42 125.16(12) . . ? O2 V1 N42 77.69(12) . . ? N32 V1 N42 154.99(13) . . ? O1 V1 N22 125.97(12) 3_675 . ? O1 V1 N22 76.92(12) . . ? O2 V1 N22 77.71(12) . . ? N32 V1 N22 83.12(13) . . ? N42 V1 N22 91.39(13) . . ? O1 V1 N52 76.97(12) 3_675 . ? O1 V1 N52 126.94(12) . . ? O2 V1 N52 76.60(12) . . ? N32 V1 N52 92.47(12) . . ? N42 V1 N52 81.95(13) . . ? N22 V1 N52 154.28(13) . . ? O2 V2 O5 94.50(12) . . ? O2 V2 O3 93.65(13) . . ? O5 V2 O3 90.73(14) . . ? O2 V2 N41 84.26(12) . . ? O5 V2 N41 88.50(13) . . ? O3 V2 N41 177.71(14) . . ? O2 V2 N21 84.44(12) . . ? O5 V2 N21 178.76(14) . . ? O3 V2 N21 89.98(14) . . ? N41 V2 N21 90.75(13) . . ? O2 V2 Cl1 174.56(9) . . ? O5 V2 Cl1 89.48(9) . . ? O3 V2 Cl1 89.99(11) . . ? N41 V2 Cl1 92.16(10) . . ? N21 V2 Cl1 91.53(10) . . ? O2 V3 O6 94.22(12) . . ? O2 V3 O4 93.13(12) . . ? O6 V3 O4 89.07(13) . . ? O2 V3 N31 84.52(12) . . ? O6 V3 N31 177.85(13) . . ? O4 V3 N31 89.26(13) . . ? O2 V3 N51 82.67(12) . . ? O6 V3 N51 89.64(13) . . ? O4 V3 N51 175.50(13) . . ? N31 V3 N51 91.93(13) . . ? O2 V3 Cl2 172.32(9) . . ? O6 V3 Cl2 89.97(9) . . ? O4 V3 Cl2 93.37(10) . . ? N31 V3 Cl2 91.48(9) . . ? N51 V3 Cl2 90.94(10) . . ? O1 V4 N53 84.69(12) . . ? O1 V4 N43 84.69(12) . . ? N53 V4 N43 86.89(13) . . ? O1 V4 N33 84.13(12) . . ? N53 V4 N33 168.65(13) . . ? N43 V4 N33 90.08(13) . . ? O1 V4 N23 83.95(13) . . ? N53 V4 N23 90.76(13) . . ? N43 V4 N23 168.57(13) . . ? N33 V4 N23 90.05(13) . . ? O1 V4 Cl3 178.47(10) . . ? N53 V4 Cl3 96.77(10) . . ? N43 V4 Cl3 95.81(9) . . ? N33 V4 Cl3 94.42(10) . . ? N23 V4 Cl3 95.57(10) . . ? V4 O1 V1 124.41(14) . 3_675 ? V4 O1 V1 123.77(14) . . ? V1 O1 V1 111.81(12) 3_675 . ? V2 O2 V3 122.57(14) . . ? V2 O2 V1 118.68(13) . . ? V3 O2 V1 118.75(13) . . ? C1 O3 V2 135.0(4) . . ? C1 O4 V3 132.6(3) . . ? C6 O5 V2 131.9(3) . . ? C6 O6 V3 134.2(3) . . ? N22 N21 C21 106.6(3) . . ? N22 N21 V2 114.5(2) . . ? C21 N21 V2 135.6(3) . . ? N23 N22 N21 112.2(3) . . ? N23 N22 V1 124.6(3) . . ? N21 N22 V1 122.3(3) . . ? N22 N23 C26 106.6(3) . . ? N22 N23 V4 112.4(3) . . ? C26 N23 V4 139.6(3) . . ? N32 N31 C31 106.6(3) . . ? N32 N31 V3 114.8(2) . . ? C31 N31 V3 135.0(3) . . ? N31 N32 N33 112.7(3) . . ? N31 N32 V1 122.6(2) . . ? N33 N32 V1 124.4(2) . . ? N32 N33 C36 106.1(3) . . ? N32 N33 V4 112.6(2) . . ? C36 N33 V4 140.5(3) . . ? N42 N41 C41 106.7(3) . . ? N42 N41 V2 115.0(2) . . ? C41 N41 V2 133.6(3) . . ? N41 N42 N43 112.4(3) . 3_675 ? N41 N42 V1 122.4(3) . . ? N43 N42 V1 123.7(3) 3_675 . ? N42 N43 C44 106.6(3) 3_675 . ? N42 N43 V4 113.0(2) 3_675 . ? C44 N43 V4 139.2(3) . . ? N52 N51 C51 107.3(3) . 3_675 ? N52 N51 V3 115.1(3) . . ? C51 N51 V3 135.3(3) 3_675 . ? N51 N52 N53 111.9(3) . 3_675 ? N51 N52 V1 122.7(3) . . ? N53 N52 V1 124.4(2) 3_675 . ? N52 N53 C56 106.4(3) 3_675 . ? N52 N53 V4 112.5(2) 3_675 . ? C56 N53 V4 139.4(3) . . ? O3 C1 O4 124.7(5) . . ? O3 C1 C2 119.1(5) . . ? O4 C1 C2 116.0(4) . . ? C4 C2 C1 113.1(4) . . ? C4 C2 C3 110.5(5) . . ? C1 C2 C3 105.2(4) . . ? C4 C2 C5 110.6(4) . . ? C1 C2 C5 109.0(4) . . ? C3 C2 C5 108.3(5) . . ? O5 C6 O6 125.1(4) . . ? O5 C6 C7 117.5(4) . . ? O6 C6 C7 117.4(4) . . ? C9Y C7 C10X 128.5(8) . . ? C9Y C7 C8X 69.3(8) . . ? C10X C7 C8X 116.3(7) . . ? C9Y C7 C6 115.4(7) . . ? C10X C7 C6 111.5(6) . . ? C8X C7 C6 106.3(5) . . ? C9Y C7 C10Y 115.0(9) . . ? C10X C7 C10Y 27.2(6) . . ? C8X C7 C10Y 139.1(8) . . ? C6 C7 C10Y 107.1(7) . . ? C9Y C7 C9X 37.4(7) . . ? C10X C7 C9X 109.0(6) . . ? C8X C7 C9X 106.6(6) . . ? C6 C7 C9X 106.7(5) . . ? C10Y C7 C9X 85.6(7) . . ? C9Y C7 C8Y 106.3(9) . . ? C10X C7 C8Y 78.5(8) . . ? C8X C7 C8Y 41.8(6) . . ? C6 C7 C8Y 106.9(6) . . ? C10Y C7 C8Y 105.3(9) . . ? C9X C7 C8Y 139.5(7) . . ? H8D C8Y H8E 109.5 . . ? H8D C8Y H8F 109.5 . . ? H8E C8Y H8F 109.5 . . ? H9D C9Y H9E 109.5 . . ? H9D C9Y H9F 109.5 . . ? H9E C9Y H9F 109.5 . . ? H10D C10Y H10E 109.5 . . ? H10D C10Y H10F 109.5 . . ? H10E C10Y H10F 109.5 . . ? N21 C21 C22 131.2(4) . . ? N21 C21 C26 107.2(4) . . ? C22 C21 C26 121.5(4) . . ? C23 C22 C21 116.8(4) . . ? C23 C22 H22 121.6 . . ? C21 C22 H22 121.6 . . ? C22 C23 C24 121.5(5) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C25 C24 C23 122.3(5) . . ? C25 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? C24 C25 C26 116.5(4) . . ? C24 C25 H25 121.7 . . ? C26 C25 H25 121.7 . . ? N23 C26 C25 131.3(4) . . ? N23 C26 C21 107.3(4) . . ? C25 C26 C21 121.4(4) . . ? N31 C31 C36 106.9(3) . . ? N31 C31 C32 131.2(4) . . ? C36 C31 C32 121.9(4) . . ? C33 C32 C31 116.0(4) . . ? C33 C32 H32 122.0 . . ? C31 C32 H32 122.0 . . ? C32 C33 C34 122.5(4) . . ? C32 C33 H33 118.8 . . ? C34 C33 H33 118.8 . . ? C35 C34 C33 122.0(4) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? C34 C35 C36 116.2(4) . . ? C34 C35 H35 121.9 . . ? C36 C35 H35 121.9 . . ? N33 C36 C31 107.7(4) . . ? N33 C36 C35 131.0(4) . . ? C31 C36 C35 121.3(4) . . ? N41 C41 C44 107.3(4) . 3_675 ? N41 C41 C42 131.1(4) . . ? C44 C41 C42 121.6(4) 3_675 . ? C43 C42 C41 116.2(4) . . ? C43 C42 H42 121.9 . . ? C41 C42 H42 121.9 . . ? C42 C43 C46 122.1(4) . 3_675 ? C42 C43 H43 118.9 . . ? C46 C43 H43 118.9 3_675 . ? N43 C44 C41 106.9(4) . 3_675 ? N43 C44 C45 132.2(4) . . ? C41 C44 C45 120.8(4) 3_675 . ? C46 C45 C44 117.0(4) . . ? C46 C45 H45 121.5 . . ? C44 C45 H45 121.5 . . ? C45 C46 C43 122.3(4) . 3_675 ? C45 C46 H46 118.9 . . ? C43 C46 H46 118.9 3_675 . ? N51 C51 C56 107.5(4) 3_675 . ? N51 C51 C52 131.9(4) 3_675 . ? C56 C51 C52 120.6(4) . . ? C53 C52 C51 117.1(4) . . ? C53 C52 H52 121.5 . . ? C51 C52 H52 121.5 . . ? C52 C53 C54 122.1(4) . . ? C52 C53 H53 119.0 . . ? C54 C53 H53 119.0 . . ? C55 C54 C53 121.6(4) . . ? C55 C54 H54 119.2 . . ? C53 C54 H54 119.2 . . ? C54 C55 C56 116.4(4) . . ? C54 C55 H55 121.8 . . ? C56 C55 H55 121.8 . . ? N53 C56 C51 107.0(4) . . ? N53 C56 C55 130.9(4) . . ? C51 C56 C55 122.1(4) . . ? C68 N60 C72 110.6(4) . . ? C68 N60 C60 107.4(4) . . ? C72 N60 C60 110.3(4) . . ? C68 N60 C64 111.3(4) . . ? C72 N60 C64 106.7(4) . . ? C60 N60 C64 110.5(4) . . ? C61 C60 N60 115.8(5) . . ? C61 C60 H60A 108.3 . . ? N60 C60 H60A 108.3 . . ? C61 C60 H60B 108.3 . . ? N60 C60 H60B 108.3 . . ? H60A C60 H60B 107.4 . . ? C62 C61 C60 109.1(6) . . ? C62 C61 H61A 109.9 . . ? C60 C61 H61A 109.9 . . ? C62 C61 H61B 109.9 . . ? C60 C61 H61B 109.9 . . ? H61A C61 H61B 108.3 . . ? C61 C62 C63 114.1(7) . . ? C61 C62 H62A 108.7 . . ? C63 C62 H62A 108.7 . . ? C61 C62 H62B 108.7 . . ? C63 C62 H62B 108.7 . . ? H62A C62 H62B 107.6 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 N60 116.2(5) . . ? C65 C64 H64A 108.2 . . ? N60 C64 H64A 108.2 . . ? C65 C64 H64B 108.2 . . ? N60 C64 H64B 108.2 . . ? H64A C64 H64B 107.4 . . ? C66Y C65 C66X 33.8(10) . . ? C66Y C65 C64 122.5(11) . . ? C66X C65 C64 117.1(6) . . ? C66Y C65 H65A 126.3 . . ? C66X C65 H65A 108.0 . . ? C64 C65 H65A 108.0 . . ? C66Y C65 H65B 75.1 . . ? C66X C65 H65B 108.0 . . ? C64 C65 H65B 108.0 . . ? H65A C65 H65B 107.3 . . ? C67X C66X C65 122.0(8) . . ? C67X C66X H66A 106.8 . . ? C65 C66X H66A 106.8 . . ? C67X C66X H66B 106.8 . . ? C65 C66X H66B 106.8 . . ? H66A C66X H66B 106.7 . . ? C65 C66Y C67Y 141.1(17) . . ? C65 C66Y H66C 101.7 . . ? C67Y C66Y H66C 101.7 . . ? C65 C66Y H66D 101.7 . . ? C67Y C66Y H66D 101.7 . . ? H66C C66Y H66D 104.7 . . ? C66Y C67Y H67D 109.5 . . ? C66Y C67Y H67E 109.5 . . ? H67D C67Y H67E 109.5 . . ? C66Y C67Y H67F 109.5 . . ? H67D C67Y H67F 109.5 . . ? H67E C67Y H67F 109.5 . . ? C69 C68 N60 117.1(4) . . ? C69 C68 H68A 108.0 . . ? N60 C68 H68A 108.0 . . ? C69 C68 H68B 108.0 . . ? N60 C68 H68B 108.0 . . ? H68A C68 H68B 107.3 . . ? C68 C69 C70 110.2(4) . . ? C68 C69 H69A 109.6 . . ? C70 C69 H69A 109.6 . . ? C68 C69 H69B 109.6 . . ? C70 C69 H69B 109.6 . . ? H69A C69 H69B 108.1 . . ? C71 C70 C69 112.3(5) . . ? C71 C70 H70A 109.1 . . ? C69 C70 H70A 109.1 . . ? C71 C70 H70B 109.1 . . ? C69 C70 H70B 109.1 . . ? H70A C70 H70B 107.9 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C73 C72 N60 115.6(4) . . ? C73 C72 H72A 108.4 . . ? N60 C72 H72A 108.4 . . ? C73 C72 H72B 108.4 . . ? N60 C72 H72B 108.4 . . ? H72A C72 H72B 107.5 . . ? C72 C73 C74 110.5(5) . . ? C72 C73 H73A 109.5 . . ? C74 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? C74 C73 H73B 109.5 . . ? H73A C73 H73B 108.1 . . ? C75X C74 C75Y 93.2(10) . . ? C75X C74 C73 113.9(8) . . ? C75Y C74 C73 125.4(8) . . ? C74 C75X H75A 109.5 . . ? C74 C75X H75B 109.5 . . ? C74 C75X H75C 109.5 . . ? C74 C75Y H75D 109.5 . . ? C74 C75Y H75E 109.5 . . ? H75D C75Y H75E 109.5 . . ? C74 C75Y H75F 109.5 . . ? H75D C75Y H75F 109.5 . . ? H75E C75Y H75F 109.5 . . ? C4S O1S C1S 105.9(8) . . ? C2S C1S O1S 101.0(9) . . ? C2S C1S H1S1 111.6 . . ? O1S C1S H1S1 111.6 . . ? C2S C1S H1S2 111.6 . . ? O1S C1S H1S2 111.6 . . ? H1S1 C1S H1S2 109.4 . . ? C3S C2S C1S 114.3(9) . . ? C3S C2S H2S1 108.7 . . ? C1S C2S H2S1 108.7 . . ? C3S C2S H2S2 108.7 . . ? C1S C2S H2S2 108.7 . . ? H2S1 C2S H2S2 107.6 . . ? C2S C3S C4S 108.4(9) . . ? C2S C3S H3S1 110.0 . . ? C4S C3S H3S1 110.0 . . ? C2S C3S H3S2 110.0 . . ? C4S C3S H3S2 110.0 . . ? H3S1 C3S H3S2 108.4 . . ? O1S C4S C3S 108.2(9) . . ? O1S C4S H4S1 110.1 . . ? C3S C4S H4S1 110.1 . . ? O1S C4S H4S2 110.1 . . ? C3S C4S H4S2 110.1 . . ? H4S1 C4S H4S2 108.4 . . ? C8S O2S C5S 104.5(8) . . ? C6S C5S O2S 109.0(8) . . ? C6S C5S H5S1 109.9 . . ? O2S C5S H5S1 109.9 . . ? C6S C5S H5S2 109.9 . . ? O2S C5S H5S2 109.9 . . ? H5S1 C5S H5S2 108.3 . . ? C5S C6S C7S 109.3(8) . . ? C5S C6S H6S1 109.8 . . ? C7S C6S H6S1 109.8 . . ? C5S C6S H6S2 109.8 . . ? C7S C6S H6S2 109.8 . . ? H6S1 C6S H6S2 108.3 . . ? C6S C7S C8S 101.9(7) . . ? C6S C7S H7S1 111.4 . . ? C8S C7S H7S1 111.4 . . ? C6S C7S H7S2 111.4 . . ? C8S C7S H7S2 111.4 . . ? H7S1 C7S H7S2 109.3 . . ? O2S C8S C7S 111.3(10) . . ? O2S C8S H8S1 109.4 . . ? C7S C8S H8S1 109.4 . . ? O2S C8S H8S2 109.4 . . ? C7S C8S H8S2 109.4 . . ? H8S1 C8S H8S2 108.0 . . ? 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 N53 V4 O1 V1 -44.41(18) . . . 3_675 ? N43 V4 O1 V1 42.95(17) . . . 3_675 ? N33 V4 O1 V1 133.59(18) . . . 3_675 ? N23 V4 O1 V1 -135.74(18) . . . 3_675 ? Cl3 V4 O1 V1 152(4) . . . 3_675 ? N53 V4 O1 V1 137.05(18) . . . . ? N43 V4 O1 V1 -135.59(18) . . . . ? N33 V4 O1 V1 -44.95(17) . . . . ? N23 V4 O1 V1 45.72(17) . . . . ? Cl3 V4 O1 V1 -26(4) . . . . ? O1 V1 O1 V4 178.7(3) 3_675 . . . ? O2 V1 O1 V4 -0.5(3) . . . . ? N32 V1 O1 V4 42.39(17) . . . . ? N42 V1 O1 V4 -125.71(18) . . . . ? N22 V1 O1 V4 -43.36(17) . . . . ? N52 V1 O1 V4 125.91(17) . . . . ? O1 V1 O1 V1 -0.004(1) 3_675 . . 3_675 ? O2 V1 O1 V1 -179.25(15) . . . 3_675 ? N32 V1 O1 V1 -136.31(16) . . . 3_675 ? N42 V1 O1 V1 55.59(19) . . . 3_675 ? N22 V1 O1 V1 137.94(15) . . . 3_675 ? N52 V1 O1 V1 -52.79(19) . . . 3_675 ? O5 V2 O2 V3 46.92(18) . . . . ? O3 V2 O2 V3 -44.11(18) . . . . ? N41 V2 O2 V3 134.94(18) . . . . ? N21 V2 O2 V3 -133.74(18) . . . . ? Cl1 V2 O2 V3 -176.1(8) . . . . ? O5 V2 O2 V1 -133.32(15) . . . . ? O3 V2 O2 V1 135.65(16) . . . . ? N41 V2 O2 V1 -45.29(15) . . . . ? N21 V2 O2 V1 46.02(16) . . . . ? Cl1 V2 O2 V1 3.7(11) . . . . ? O6 V3 O2 V2 -42.27(18) . . . . ? O4 V3 O2 V2 47.02(17) . . . . ? N31 V3 O2 V2 135.98(18) . . . . ? N51 V3 O2 V2 -131.36(18) . . . . ? Cl2 V3 O2 V2 -165.2(6) . . . . ? O6 V3 O2 V1 137.97(15) . . . . ? O4 V3 O2 V1 -132.74(15) . . . . ? N31 V3 O2 V1 -43.78(15) . . . . ? N51 V3 O2 V1 48.88(15) . . . . ? Cl2 V3 O2 V1 15.0(8) . . . . ? O1 V1 O2 V2 91.3(2) 3_675 . . . ? O1 V1 O2 V2 -90.0(2) . . . . ? N32 V1 O2 V2 -132.93(17) . . . . ? N42 V1 O2 V2 46.86(15) . . . . ? N22 V1 O2 V2 -47.33(15) . . . . ? N52 V1 O2 V2 131.38(17) . . . . ? O1 V1 O2 V3 -89.0(2) 3_675 . . . ? O1 V1 O2 V3 89.8(2) . . . . ? N32 V1 O2 V3 46.84(15) . . . . ? N42 V1 O2 V3 -133.37(17) . . . . ? N22 V1 O2 V3 132.44(17) . . . . ? N52 V1 O2 V3 -48.85(15) . . . . ? O2 V2 O3 C1 20.2(5) . . . . ? O5 V2 O3 C1 -74.4(5) . . . . ? N41 V2 O3 C1 -4(4) . . . . ? N21 V2 O3 C1 104.6(5) . . . . ? Cl1 V2 O3 C1 -163.9(5) . . . . ? O2 V3 O4 C1 -29.2(4) . . . . ? O6 V3 O4 C1 65.0(4) . . . . ? N31 V3 O4 C1 -113.7(4) . . . . ? N51 V3 O4 C1 -8.3(19) . . . . ? Cl2 V3 O4 C1 154.9(4) . . . . ? O2 V2 O5 C6 -30.1(4) . . . . ? O3 V2 O5 C6 63.6(4) . . . . ? N41 V2 O5 C6 -114.3(4) . . . . ? N21 V2 O5 C6 -62(6) . . . . ? Cl1 V2 O5 C6 153.6(4) . . . . ? O2 V3 O6 C6 16.2(4) . . . . ? O4 V3 O6 C6 -76.8(4) . . . . ? N31 V3 O6 C6 -38(4) . . . . ? N51 V3 O6 C6 98.9(4) . . . . ? Cl2 V3 O6 C6 -170.2(4) . . . . ? O2 V2 N21 N22 -20.3(3) . . . . ? O5 V2 N21 N22 11(6) . . . . ? O3 V2 N21 N22 -113.9(3) . . . . ? N41 V2 N21 N22 63.9(3) . . . . ? Cl1 V2 N21 N22 156.1(3) . . . . ? O2 V2 N21 C21 136.0(4) . . . . ? O5 V2 N21 C21 168(43) . . . . ? O3 V2 N21 C21 42.3(4) . . . . ? N41 V2 N21 C21 -139.9(4) . . . . ? Cl1 V2 N21 C21 -47.7(4) . . . . ? C21 N21 N22 N23 -1.7(4) . . . . ? V2 N21 N22 N23 161.2(2) . . . . ? C21 N21 N22 V1 -171.3(3) . . . . ? V2 N21 N22 V1 -8.4(4) . . . . ? O1 V1 N22 N23 69.3(3) 3_675 . . . ? O1 V1 N22 N23 19.0(3) . . . . ? O2 V1 N22 N23 -138.0(3) . . . . ? N32 V1 N22 N23 -59.6(3) . . . . ? N42 V1 N22 N23 144.9(3) . . . . ? N52 V1 N22 N23 -140.9(3) . . . . ? O1 V1 N22 N21 -122.5(3) 3_675 . . . ? O1 V1 N22 N21 -172.7(3) . . . . ? O2 V1 N22 N21 30.2(3) . . . . ? N32 V1 N22 N21 108.7(3) . . . . ? N42 V1 N22 N21 -46.8(3) . . . . ? N52 V1 N22 N21 27.4(5) . . . . ? N21 N22 N23 C26 2.6(4) . . . . ? V1 N22 N23 C26 171.9(3) . . . . ? N21 N22 N23 V4 -166.7(2) . . . . ? V1 N22 N23 V4 2.6(4) . . . . ? O1 V4 N23 N22 -24.9(3) . . . . ? N53 V4 N23 N22 -109.5(3) . . . . ? N43 V4 N23 N22 -31.5(8) . . . . ? N33 V4 N23 N22 59.2(3) . . . . ? Cl3 V4 N23 N22 153.6(2) . . . . ? O1 V4 N23 C26 171.0(4) . . . . ? N53 V4 N23 C26 86.4(4) . . . . ? N43 V4 N23 C26 164.4(6) . . . . ? N33 V4 N23 C26 -105.0(4) . . . . ? Cl3 V4 N23 C26 -10.5(4) . . . . ? O2 V3 N31 N32 16.0(3) . . . . ? O6 V3 N31 N32 70(4) . . . . ? O4 V3 N31 N32 109.2(3) . . . . ? N51 V3 N31 N32 -66.4(3) . . . . ? Cl2 V3 N31 N32 -157.4(3) . . . . ? O2 V3 N31 C31 -138.8(4) . . . . ? O6 V3 N31 C31 -85(3) . . . . ? O4 V3 N31 C31 -45.6(4) . . . . ? N51 V3 N31 C31 138.7(4) . . . . ? Cl2 V3 N31 C31 47.7(4) . . . . ? C31 N31 N32 N33 2.0(4) . . . . ? V3 N31 N32 N33 -159.7(3) . . . . ? C31 N31 N32 V1 175.7(3) . . . . ? V3 N31 N32 V1 14.0(4) . . . . ? O1 V1 N32 N31 117.5(3) 3_675 . . . ? O1 V1 N32 N31 169.1(3) . . . . ? O2 V1 N32 N31 -33.9(3) . . . . ? N42 V1 N32 N31 -34.4(5) . . . . ? N22 V1 N32 N31 -112.8(3) . . . . ? N52 V1 N32 N31 41.7(3) . . . . ? O1 V1 N32 N33 -69.6(3) 3_675 . . . ? O1 V1 N32 N33 -18.0(3) . . . . ? O2 V1 N32 N33 139.0(3) . . . . ? N42 V1 N32 N33 138.5(3) . . . . ? N22 V1 N32 N33 60.1(3) . . . . ? N52 V1 N32 N33 -145.3(3) . . . . ? N31 N32 N33 C36 -2.0(5) . . . . ? V1 N32 N33 C36 -175.5(3) . . . . ? N31 N32 N33 V4 170.0(2) . . . . ? V1 N32 N33 V4 -3.5(4) . . . . ? O1 V4 N33 N32 25.2(3) . . . . ? N53 V4 N33 N32 35.4(8) . . . . ? N43 V4 N33 N32 109.8(3) . . . . ? N23 V4 N33 N32 -58.7(3) . . . . ? Cl3 V4 N33 N32 -154.3(3) . . . . ? O1 V4 N33 C36 -167.0(5) . . . . ? N53 V4 N33 C36 -156.8(6) . . . . ? N43 V4 N33 C36 -82.3(5) . . . . ? N23 V4 N33 C36 109.1(5) . . . . ? Cl3 V4 N33 C36 13.5(5) . . . . ? O2 V2 N41 N42 19.7(3) . . . . ? O5 V2 N41 N42 114.4(3) . . . . ? O3 V2 N41 N42 44(4) . . . . ? N21 V2 N41 N42 -64.6(3) . . . . ? Cl1 V2 N41 N42 -156.2(3) . . . . ? O2 V2 N41 C41 -132.2(4) . . . . ? O5 V2 N41 C41 -37.6(4) . . . . ? O3 V2 N41 C41 -108(3) . . . . ? N21 V2 N41 C41 143.4(4) . . . . ? Cl1 V2 N41 C41 51.9(4) . . . . ? C41 N41 N42 N43 1.7(4) . . . 3_675 ? V2 N41 N42 N43 -157.5(2) . . . 3_675 ? C41 N41 N42 V1 168.1(3) . . . . ? V2 N41 N42 V1 9.0(4) . . . . ? O1 V1 N42 N41 173.2(3) 3_675 . . . ? O1 V1 N42 N41 121.6(3) . . . . ? O2 V1 N42 N41 -30.5(3) . . . . ? N32 V1 N42 N41 -30.0(5) . . . . ? N22 V1 N42 N41 46.6(3) . . . . ? N52 V1 N42 N41 -108.4(3) . . . . ? O1 V1 N42 N43 -21.8(3) 3_675 . . 3_675 ? O1 V1 N42 N43 -73.5(3) . . . 3_675 ? O2 V1 N42 N43 134.5(3) . . . 3_675 ? N32 V1 N42 N43 134.9(3) . . . 3_675 ? N22 V1 N42 N43 -148.4(3) . . . 3_675 ? N52 V1 N42 N43 56.5(3) . . . 3_675 ? O1 V4 N43 N42 -20.5(3) . . . 3_675 ? N53 V4 N43 N42 64.5(3) . . . 3_675 ? N33 V4 N43 N42 -104.6(3) . . . 3_675 ? N23 V4 N43 N42 -13.9(8) . . . 3_675 ? Cl3 V4 N43 N42 161.0(2) . . . 3_675 ? O1 V4 N43 C44 174.0(4) . . . . ? N53 V4 N43 C44 -101.1(4) . . . . ? N33 V4 N43 C44 89.9(4) . . . . ? N23 V4 N43 C44 -179(45) . . . . ? Cl3 V4 N43 C44 -4.6(4) . . . . ? O2 V3 N51 N52 -23.7(3) . . . . ? O6 V3 N51 N52 -118.0(3) . . . . ? O4 V3 N51 N52 -44.7(18) . . . . ? N31 V3 N51 N52 60.5(3) . . . . ? Cl2 V3 N51 N52 152.0(3) . . . . ? O2 V3 N51 C51 136.2(4) . . . 3_675 ? O6 V3 N51 C51 41.9(4) . . . 3_675 ? O4 V3 N51 C51 115.1(16) . . . 3_675 ? N31 V3 N51 C51 -139.6(4) . . . 3_675 ? Cl2 V3 N51 C51 -48.1(4) . . . 3_675 ? C51 N51 N52 N53 -1.0(4) 3_675 . . 3_675 ? V3 N51 N52 N53 164.3(2) . . . 3_675 ? C51 N51 N52 V1 -170.0(3) 3_675 . . . ? V3 N51 N52 V1 -4.7(4) . . . . ? O1 V1 N52 N51 -173.2(3) 3_675 . . . ? O1 V1 N52 N51 -123.8(3) . . . . ? O2 V1 N52 N51 28.6(3) . . . . ? N32 V1 N52 N51 -47.7(3) . . . . ? N42 V1 N52 N51 107.8(3) . . . . ? N22 V1 N52 N51 31.5(5) . . . . ? O1 V1 N52 N53 19.2(3) 3_675 . . 3_675 ? O1 V1 N52 N53 68.6(3) . . . 3_675 ? O2 V1 N52 N53 -139.0(3) . . . 3_675 ? N32 V1 N52 N53 144.7(3) . . . 3_675 ? N42 V1 N52 N53 -59.8(3) . . . 3_675 ? N22 V1 N52 N53 -136.1(3) . . . 3_675 ? O1 V4 N53 N52 23.3(3) . . . 3_675 ? N43 V4 N53 N52 -61.7(3) . . . 3_675 ? N33 V4 N53 N52 13.1(9) . . . 3_675 ? N23 V4 N53 N52 107.1(3) . . . 3_675 ? Cl3 V4 N53 N52 -157.2(2) . . . 3_675 ? O1 V4 N53 C56 -174.8(4) . . . . ? N43 V4 N53 C56 100.2(4) . . . . ? N33 V4 N53 C56 175.0(6) . . . . ? N23 V4 N53 C56 -91.0(4) . . . . ? Cl3 V4 N53 C56 4.7(4) . . . . ? V2 O3 C1 O4 -4.9(8) . . . . ? V2 O3 C1 C2 170.1(3) . . . . ? V3 O4 C1 O3 10.7(7) . . . . ? V3 O4 C1 C2 -164.4(3) . . . . ? O3 C1 C2 C4 150.9(5) . . . . ? O4 C1 C2 C4 -33.6(6) . . . . ? O3 C1 C2 C3 -88.4(6) . . . . ? O4 C1 C2 C3 87.1(5) . . . . ? O3 C1 C2 C5 27.5(6) . . . . ? O4 C1 C2 C5 -157.0(4) . . . . ? V2 O5 C6 O6 10.0(7) . . . . ? V2 O5 C6 C7 -168.6(3) . . . . ? V3 O6 C6 O5 -1.4(7) . . . . ? V3 O6 C6 C7 177.2(3) . . . . ? O5 C6 C7 C9Y 172.6(9) . . . . ? O6 C6 C7 C9Y -6.1(10) . . . . ? O5 C6 C7 C10X -29.4(8) . . . . ? O6 C6 C7 C10X 151.9(7) . . . . ? O5 C6 C7 C8X 98.3(6) . . . . ? O6 C6 C7 C8X -80.4(7) . . . . ? O5 C6 C7 C10Y -57.8(8) . . . . ? O6 C6 C7 C10Y 123.5(8) . . . . ? O5 C6 C7 C9X -148.3(5) . . . . ? O6 C6 C7 C9X 33.0(7) . . . . ? O5 C6 C7 C8Y 54.6(8) . . . . ? O6 C6 C7 C8Y -124.1(8) . . . . ? N22 N21 C21 C22 178.3(4) . . . . ? V2 N21 C21 C22 20.8(7) . . . . ? N22 N21 C21 C26 0.0(4) . . . . ? V2 N21 C21 C26 -157.5(3) . . . . ? N21 C21 C22 C23 -179.3(4) . . . . ? C26 C21 C22 C23 -1.2(7) . . . . ? C21 C22 C23 C24 -0.3(7) . . . . ? C22 C23 C24 C25 1.8(8) . . . . ? C23 C24 C25 C26 -1.6(7) . . . . ? N22 N23 C26 C25 179.3(5) . . . . ? V4 N23 C26 C25 -16.0(8) . . . . ? N22 N23 C26 C21 -2.5(4) . . . . ? V4 N23 C26 C21 162.2(3) . . . . ? C24 C25 C26 N23 178.0(4) . . . . ? C24 C25 C26 C21 0.0(7) . . . . ? N21 C21 C26 N23 1.5(5) . . . . ? C22 C21 C26 N23 -177.0(4) . . . . ? N21 C21 C26 C25 179.9(4) . . . . ? C22 C21 C26 C25 1.5(7) . . . . ? N32 N31 C31 C36 -1.3(4) . . . . ? V3 N31 C31 C36 155.0(3) . . . . ? N32 N31 C31 C32 179.6(5) . . . . ? V3 N31 C31 C32 -24.2(7) . . . . ? N31 C31 C32 C33 -178.9(4) . . . . ? C36 C31 C32 C33 2.1(7) . . . . ? C31 C32 C33 C34 -0.8(7) . . . . ? C32 C33 C34 C35 -0.4(8) . . . . ? C33 C34 C35 C36 0.4(7) . . . . ? N32 N33 C36 C31 1.0(5) . . . . ? V4 N33 C36 C31 -167.3(3) . . . . ? N32 N33 C36 C35 -177.1(5) . . . . ? V4 N33 C36 C35 14.6(8) . . . . ? N31 C31 C36 N33 0.1(5) . . . . ? C32 C31 C36 N33 179.4(4) . . . . ? N31 C31 C36 C35 178.5(4) . . . . ? C32 C31 C36 C35 -2.2(7) . . . . ? C34 C35 C36 N33 178.9(5) . . . . ? C34 C35 C36 C31 0.9(7) . . . . ? N42 N41 C41 C44 -1.1(4) . . . 3_675 ? V2 N41 C41 C44 152.5(3) . . . 3_675 ? N42 N41 C41 C42 -179.3(4) . . . . ? V2 N41 C41 C42 -25.8(7) . . . . ? N41 C41 C42 C43 179.1(4) . . . . ? C44 C41 C42 C43 1.1(7) 3_675 . . . ? C41 C42 C43 C46 -0.2(7) . . . 3_675 ? N42 N43 C44 C41 -0.8(4) 3_675 . . 3_675 ? V4 N43 C44 C41 165.3(3) . . . 3_675 ? N42 N43 C44 C45 179.1(4) 3_675 . . . ? V4 N43 C44 C45 -14.7(7) . . . . ? N43 C44 C45 C46 179.3(4) . . . . ? C41 C44 C45 C46 -0.8(6) 3_675 . . . ? C44 C45 C46 C43 -0.1(7) . . . 3_675 ? N51 C51 C52 C53 177.8(5) 3_675 . . . ? C56 C51 C52 C53 1.0(7) . . . . ? C51 C52 C53 C54 0.5(7) . . . . ? C52 C53 C54 C55 -0.7(8) . . . . ? C53 C54 C55 C56 -0.5(7) . . . . ? N52 N53 C56 C51 -0.1(4) 3_675 . . . ? V4 N53 C56 C51 -162.7(3) . . . . ? N52 N53 C56 C55 -179.5(5) 3_675 . . . ? V4 N53 C56 C55 17.9(8) . . . . ? N51 C51 C56 N53 0.7(5) 3_675 . . . ? C52 C51 C56 N53 178.2(4) . . . . ? N51 C51 C56 C55 -179.8(4) 3_675 . . . ? C52 C51 C56 C55 -2.3(7) . . . . ? C54 C55 C56 N53 -178.7(5) . . . . ? C54 C55 C56 C51 2.0(7) . . . . ? C68 N60 C60 C61 176.3(5) . . . . ? C72 N60 C60 C61 -63.1(6) . . . . ? C64 N60 C60 C61 54.7(6) . . . . ? N60 C60 C61 C62 178.4(5) . . . . ? C60 C61 C62 C63 174.0(5) . . . . ? C68 N60 C64 C65 -65.4(6) . . . . ? C72 N60 C64 C65 173.9(5) . . . . ? C60 N60 C64 C65 53.9(6) . . . . ? N60 C64 C65 C66Y 105.9(14) . . . . ? N60 C64 C65 C66X 144.5(7) . . . . ? C66Y C65 C66X C67X 63(2) . . . . ? C64 C65 C66X C67X -45.9(12) . . . . ? C66X C65 C66Y C67Y -96(3) . . . . ? C64 C65 C66Y C67Y -5(4) . . . . ? C72 N60 C68 C69 54.3(6) . . . . ? C60 N60 C68 C69 174.8(4) . . . . ? C64 N60 C68 C69 -64.1(6) . . . . ? N60 C68 C69 C70 164.8(4) . . . . ? C68 C69 C70 C71 177.9(5) . . . . ? C68 N60 C72 C73 63.4(6) . . . . ? C60 N60 C72 C73 -55.3(6) . . . . ? C64 N60 C72 C73 -175.4(5) . . . . ? N60 C72 C73 C74 -171.6(6) . . . . ? C72 C73 C74 C75X 72.1(9) . . . . ? C72 C73 C74 C75Y -40.8(13) . . . . ? C4S O1S C1S C2S 14.4(15) . . . . ? O1S C1S C2S C3S -13.2(19) . . . . ? C1S C2S C3S C4S 7(2) . . . . ? C1S O1S C4S C3S -11.7(16) . . . . ? C2S C3S C4S O1S 3.8(19) . . . . ? C8S O2S C5S C6S 18.7(17) . . . . ? O2S C5S C6S C7S -10.0(18) . . . . ? C5S C6S C7S C8S -2.2(17) . . . . ? C5S O2S C8S C7S -20.5(17) . . . . ? C6S C7S C8S O2S 14.5(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.878 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.099 data_rsv39_1 _database_code_depnum_ccdc_archive 'CCDC 654039' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H134 Cl6 N26 O14 V8' _chemical_formula_weight 2736.71 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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 13.2856(8) _cell_length_b 14.7996(7) _cell_length_c 18.4967(9) _cell_angle_alpha 66.701(5) _cell_angle_beta 77.315(5) _cell_angle_gamma 80.523(5) _cell_volume 3246.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6787 _cell_measurement_theta_min 2.6595 _cell_measurement_theta_max 31.9333 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1410 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8083 _exptl_absorpt_correction_T_max 0.8660 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalliber 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19141 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 23.26 _reflns_number_total 9300 _reflns_number_gt 5853 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. Data was processed to a resolution of 0.90 angstroms. All non hydrogen atoms were refined anisotropically. The butyl chains of the tetrabutylammonium group show some disorder, carbons C60, C61, C62, C65, C66, C67, C72, C73 and C74 are disordered over two sites. Displacement and geometric restraints were applied to the thermal parameters of N60 and C60 to C75. Displacement and geometrical restraints were applied to O1S, C1S, C2S, C3S, C4S, O2S, C6S, C7S and C8S of the two tetrahydrofuran molecules. There are short H-H contacts between H68B-H73B,H64A-H72A, H69B-H72B, H34-H74C, this is due to disorder within the tetra butyl ammonium chains. There is a deviating X-C-H bond angle on C63 again due to disorder in the butyl chains. All hydrogens were included in calculated positions using the riding model. 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^)+(0.1753P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9300 _refine_ls_number_parameters 898 _refine_ls_number_restraints 405 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2469 _refine_ls_wR_factor_gt 0.2254 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N60 N 0.7170(8) 0.4739(6) 0.7322(6) 0.090(2) Uani 1 1 d DU . . V1 V 0.56628(9) 0.01416(9) 0.40859(7) 0.0152(3) Uani 1 1 d . . . V2 V 0.59300(10) 0.12197(9) 0.20677(7) 0.0203(3) Uani 1 1 d . . . V3 V 0.77635(10) -0.04666(9) 0.28918(8) 0.0216(4) Uani 1 1 d . . . V4 V 0.60782(9) 0.15590(9) 0.50176(7) 0.0164(3) Uani 1 1 d . . . Cl1 Cl 0.51436(16) 0.24150(15) 0.10199(12) 0.0324(5) Uani 1 1 d . . . Cl2 Cl 0.93375(15) -0.14700(17) 0.28999(14) 0.0386(6) Uani 1 1 d . . . Cl3 Cl 0.69215(14) 0.28102(13) 0.50638(12) 0.0238(5) Uani 1 1 d . . . O1 O 0.5412(4) 0.0608(3) 0.5002(3) 0.0171(11) Uani 1 1 d . . . O2 O 0.6477(4) 0.0307(3) 0.2969(3) 0.0185(11) Uani 1 1 d . . . O3 O 0.7320(4) 0.1781(4) 0.1526(3) 0.0287(13) Uani 1 1 d . . . O4 O 0.8505(4) 0.0660(5) 0.2088(4) 0.0372(15) Uani 1 1 d . . . O5 O 0.6183(4) 0.0241(4) 0.1527(3) 0.0306(13) Uani 1 1 d . . . O6 O 0.7401(4) -0.0844(4) 0.2062(3) 0.0359(14) Uani 1 1 d . . . N21 N 0.5686(5) 0.2177(4) 0.2704(4) 0.0214(14) Uani 1 1 d . . . N22 N 0.5658(5) 0.1731(4) 0.3484(4) 0.0193(14) Uani 1 1 d . . . N23 N 0.5837(4) 0.2329(4) 0.3814(3) 0.0184(14) Uani 1 1 d . . . N31 N 0.8042(4) -0.0024(4) 0.3783(4) 0.0195(14) Uani 1 1 d . . . N32 N 0.7201(4) 0.0269(4) 0.4201(4) 0.0189(14) Uani 1 1 d . . . N33 N 0.7423(4) 0.0828(4) 0.4560(4) 0.0185(14) Uani 1 1 d . . . N41 N 0.4497(5) 0.0592(4) 0.2699(4) 0.0209(14) Uani 1 1 d . . . N42 N 0.4494(5) 0.0085(4) 0.3480(4) 0.0201(14) Uani 1 1 d . . . N43 N 0.6218(4) 0.0573(4) 0.6205(4) 0.0184(14) Uani 1 1 d . . . N51 N 0.6963(5) -0.1644(4) 0.3794(4) 0.0218(15) Uani 1 1 d . . . N52 N 0.6067(4) -0.1359(4) 0.4172(4) 0.0185(14) Uani 1 1 d . . . N53 N 0.4545(4) 0.2090(4) 0.5426(3) 0.0167(14) Uani 1 1 d . . . C1 C 0.8217(7) 0.1474(7) 0.1643(5) 0.033(2) Uani 1 1 d . . . C2 C 0.9025(7) 0.2183(7) 0.1168(6) 0.040(2) Uani 1 1 d . . . C3 C 0.8803(8) 0.3105(7) 0.0630(6) 0.047(2) Uani 1 1 d . . . H3 H 0.8120 0.3309 0.0559 0.056 Uiso 1 1 calc R . . C4 C 0.9547(8) 0.3742(8) 0.0191(7) 0.058(3) Uani 1 1 d . . . H4 H 0.9384 0.4357 -0.0187 0.069 Uiso 1 1 calc R . . C5 C 1.0560(8) 0.3434(9) 0.0333(7) 0.064(3) Uani 1 1 d . . . H5 H 1.1077 0.3861 0.0058 0.077 Uiso 1 1 calc R . . C6 C 1.0796(8) 0.2546(8) 0.0853(7) 0.060(3) Uani 1 1 d . . . H6 H 1.1479 0.2358 0.0932 0.072 Uiso 1 1 calc R . . C7 C 1.0061(7) 0.1896(8) 0.1278(6) 0.051(3) Uani 1 1 d . . . H7 H 1.0244 0.1271 0.1636 0.061 Uiso 1 1 calc R . . C8 C 0.6750(7) -0.0539(7) 0.1619(5) 0.037(2) Uani 1 1 d . . . C9 C 0.6633(6) -0.1130(6) 0.1157(5) 0.032(2) Uani 1 1 d . . . C10 C 0.5865(8) -0.0923(7) 0.0722(6) 0.043(2) Uani 1 1 d . . . H10 H 0.5414 -0.0359 0.0677 0.052 Uiso 1 1 calc R . . C11 C 0.5736(8) -0.1518(7) 0.0350(5) 0.043(2) Uani 1 1 d . . . H11 H 0.5198 -0.1358 0.0061 0.052 Uiso 1 1 calc R . . C12 C 0.6380(9) -0.2336(7) 0.0399(5) 0.049(3) Uani 1 1 d . . . H12 H 0.6283 -0.2749 0.0154 0.058 Uiso 1 1 calc R . . C13 C 0.7172(9) -0.2548(8) 0.0809(6) 0.054(3) Uani 1 1 d . . . H13 H 0.7641 -0.3092 0.0816 0.065 Uiso 1 1 calc R . . C14 C 0.7306(8) -0.1985(7) 0.1218(6) 0.047(2) Uani 1 1 d . . . H14 H 0.7827 -0.2167 0.1525 0.057 Uiso 1 1 calc R . . C21 C 0.5899(7) 0.3137(6) 0.2494(5) 0.031(2) Uani 1 1 d . . . C22 C 0.6025(9) 0.3913(6) 0.1766(5) 0.049(3) Uani 1 1 d . . . H22 H 0.5949 0.3852 0.1300 0.059 Uiso 1 1 calc R . . C23 C 0.6269(10) 0.4781(7) 0.1764(6) 0.063(3) Uani 1 1 d . . . H23 H 0.6377 0.5315 0.1282 0.075 Uiso 1 1 calc R . . C24 C 0.6363(10) 0.4887(7) 0.2473(6) 0.062(3) Uani 1 1 d . . . H24 H 0.6516 0.5492 0.2444 0.074 Uiso 1 1 calc R . . C25 C 0.6234(7) 0.4122(6) 0.3203(5) 0.037(2) Uani 1 1 d . . . H25 H 0.6298 0.4196 0.3667 0.044 Uiso 1 1 calc R . . C26 C 0.6000(6) 0.3224(5) 0.3216(5) 0.0242(18) Uani 1 1 d . . . C31 C 0.8870(5) 0.0346(5) 0.3875(4) 0.0194(17) Uani 1 1 d . . . C32 C 0.9917(6) 0.0272(6) 0.3562(5) 0.0273(19) Uani 1 1 d . . . H32 H 1.0175 -0.0071 0.3224 0.033 Uiso 1 1 calc R . . C33 C 1.0549(6) 0.0728(6) 0.3776(5) 0.035(2) Uani 1 1 d . . . H33 H 1.1257 0.0684 0.3585 0.041 Uiso 1 1 calc R . . C34 C 1.0166(6) 0.1263(6) 0.4278(5) 0.034(2) Uani 1 1 d . . . H34 H 1.0625 0.1568 0.4403 0.040 Uiso 1 1 calc R . . C35 C 0.9124(6) 0.1347(5) 0.4588(5) 0.0239(18) Uani 1 1 d . . . H35 H 0.8867 0.1697 0.4921 0.029 Uiso 1 1 calc R . . C36 C 0.8476(5) 0.0873(5) 0.4371(4) 0.0206(17) Uani 1 1 d . . . C41 C 0.3734(6) 0.0284(6) 0.2496(5) 0.0247(18) Uani 1 1 d . . . C42 C 0.3401(6) 0.0576(6) 0.1758(5) 0.030(2) Uani 1 1 d . . . H42 H 0.3705 0.1065 0.1300 0.036 Uiso 1 1 calc R . . C43 C 0.2603(7) 0.0099(7) 0.1754(5) 0.041(2) Uani 1 1 d . . . H43 H 0.2358 0.0270 0.1279 0.049 Uiso 1 1 calc R . . C44 C 0.7857(6) 0.0641(7) 0.7557(5) 0.035(2) Uani 1 1 d . . . H44 H 0.8388 0.0954 0.7589 0.043 Uiso 1 1 calc R . . C45 C 0.7536(6) 0.0915(6) 0.6828(5) 0.030(2) Uani 1 1 d . . . H45 H 0.7856 0.1390 0.6369 0.036 Uiso 1 1 calc R . . C46 C 0.6728(6) 0.0456(6) 0.6811(4) 0.0211(17) Uani 1 1 d . . . C51 C 0.6945(6) -0.2641(6) 0.3997(5) 0.0251(18) Uani 1 1 d . . . C52 C 0.7681(6) -0.3338(6) 0.3799(6) 0.038(2) Uani 1 1 d . . . H52 H 0.8305 -0.3160 0.3459 0.045 Uiso 1 1 calc R . . C53 C 0.7431(7) -0.4290(7) 0.4132(7) 0.048(3) Uani 1 1 d . . . H53 H 0.7898 -0.4772 0.4010 0.057 Uiso 1 1 calc R . . C54 C 0.3496(7) 0.4574(6) 0.5351(6) 0.044(3) Uani 1 1 d . . . H54 H 0.3613 0.5239 0.5121 0.053 Uiso 1 1 calc R . . C55 C 0.4234(6) 0.3905(6) 0.5174(5) 0.030(2) Uani 1 1 d . . . H55 H 0.4861 0.4095 0.4843 0.036 Uiso 1 1 calc R . . C56 C 0.4010(6) 0.2926(6) 0.5507(5) 0.0240(18) Uani 1 1 d . . . C60X C 0.803(5) 0.459(3) 0.672(4) 0.090(2) Uani 0.185(16) 1 d PDU A 1 H60A H 0.8645 0.4780 0.6805 0.108 Uiso 0.185(16) 1 calc PR A 1 H60B H 0.7886 0.5063 0.6202 0.108 Uiso 0.185(16) 1 calc PR A 1 C61X C 0.833(4) 0.363(3) 0.662(2) 0.089(2) Uani 0.185(16) 1 d PDU A 1 H61A H 0.8344 0.3132 0.7156 0.107 Uiso 0.185(16) 1 calc PR A 1 H61B H 0.7764 0.3497 0.6433 0.107 Uiso 0.185(16) 1 calc PR A 1 C62X C 0.925(3) 0.344(3) 0.6139(11) 0.087(2) Uani 0.185(16) 1 d PDU A 1 H62A H 0.9434 0.2740 0.6400 0.105 Uiso 0.185(16) 1 calc PR A 1 H62B H 0.9755 0.3772 0.6226 0.105 Uiso 0.185(16) 1 calc PR A 1 C60Y C 0.8155(11) 0.4246(13) 0.7077(9) 0.091(2) Uani 0.815(16) 1 d PDU A 2 H60C H 0.8162 0.3549 0.7409 0.109 Uiso 0.815(16) 1 calc PR A 2 H60D H 0.8709 0.4506 0.7181 0.109 Uiso 0.815(16) 1 calc PR A 2 C61Y C 0.8383(11) 0.4348(11) 0.6225(8) 0.089(2) Uani 0.815(16) 1 d PDU A 2 H61C H 0.7809 0.4127 0.6111 0.106 Uiso 0.815(16) 1 calc PR A 2 H61D H 0.8423 0.5042 0.5892 0.106 Uiso 0.815(16) 1 calc PR A 2 C62Y C 0.9301(11) 0.3822(13) 0.6011(9) 0.087(2) Uani 0.815(16) 1 d PDU A 2 H62C H 0.9350 0.3194 0.6455 0.105 Uiso 0.815(16) 1 calc PR A 2 H62D H 0.9868 0.4178 0.5984 0.105 Uiso 0.815(16) 1 calc PR A 2 C63 C 0.9507(10) 0.3608(9) 0.5313(7) 0.084(2) Uani 1 1 d DU . . H63A H 1.0245 0.3523 0.5166 0.126 Uiso 1 1 calc R A 1 H63B H 0.9259 0.4269 0.5008 0.126 Uiso 1 1 calc R A 1 H63C H 0.9191 0.3146 0.5205 0.126 Uiso 1 1 calc R A 1 C64 C 0.6372(10) 0.4179(8) 0.7262(9) 0.088(2) Uani 1 1 d DU A . H64A H 0.6366 0.4346 0.6700 0.106 Uiso 1 1 calc R B 1 H64B H 0.5700 0.4411 0.7490 0.106 Uiso 1 1 calc R B 1 C65X C 0.6496(13) 0.3060(9) 0.7662(11) 0.080(2) Uani 0.710(12) 1 d PDU A 1 H65A H 0.7053 0.2799 0.7342 0.096 Uiso 0.710(12) 1 calc PR A 1 H65B H 0.6687 0.2881 0.8181 0.096 Uiso 0.710(12) 1 calc PR A 1 C66X C 0.5544(13) 0.2609(11) 0.7762(10) 0.080(2) Uani 0.710(12) 1 d PDU A 1 H66A H 0.5680 0.1899 0.8007 0.096 Uiso 0.710(12) 1 calc PR A 1 H66B H 0.5019 0.2816 0.8135 0.096 Uiso 0.710(12) 1 calc PR A 1 C67X C 0.5110(14) 0.2830(13) 0.7042(10) 0.077(3) Uani 0.710(12) 1 d PDU A 1 H67A H 0.5047 0.3531 0.6754 0.115 Uiso 0.710(12) 1 calc PR A 1 H67B H 0.4439 0.2585 0.7190 0.115 Uiso 0.710(12) 1 calc PR A 1 H67C H 0.5560 0.2518 0.6709 0.115 Uiso 0.710(12) 1 calc PR A 1 C65Y C 0.597(3) 0.347(2) 0.726(3) 0.084(2) Uani 0.290(12) 1 d PDU A 2 H65C H 0.6297 0.2921 0.7656 0.100 Uiso 0.290(12) 1 calc PR A 2 H65D H 0.6345 0.3433 0.6752 0.100 Uiso 0.290(12) 1 calc PR A 2 C66Y C 0.505(2) 0.306(3) 0.732(3) 0.082(3) Uani 0.290(12) 1 d PDU A 2 H66C H 0.4643 0.3560 0.6947 0.099 Uiso 0.290(12) 1 calc PR A 2 H66D H 0.4662 0.2945 0.7849 0.099 Uiso 0.290(12) 1 calc PR A 2 C67Y C 0.508(4) 0.213(2) 0.717(3) 0.079(4) Uani 0.290(12) 1 d PDU A 2 H67D H 0.5486 0.2200 0.6660 0.118 Uiso 0.290(12) 1 calc PR A 2 H67E H 0.4387 0.2005 0.7189 0.118 Uiso 0.290(12) 1 calc PR A 2 H67F H 0.5383 0.1591 0.7582 0.118 Uiso 0.290(12) 1 calc PR A 2 C68 C 0.7179(12) 0.4647(13) 0.8193(8) 0.115(3) Uani 1 1 d DU A . H68A H 0.7365 0.3958 0.8495 0.138 Uiso 1 1 calc R . . H68B H 0.7738 0.5013 0.8164 0.138 Uiso 1 1 calc R . . C69 C 0.6267(11) 0.4960(13) 0.8663(8) 0.116(3) Uani 1 1 d DU . . H69A H 0.5716 0.4549 0.8758 0.139 Uiso 1 1 calc R A . H69B H 0.6033 0.5636 0.8360 0.139 Uiso 1 1 calc R . . C70 C 0.6461(12) 0.4900(12) 0.9449(8) 0.113(3) Uani 1 1 d DU A . H70A H 0.5800 0.5044 0.9748 0.136 Uiso 1 1 calc R . . H70B H 0.6694 0.4220 0.9739 0.136 Uiso 1 1 calc R . . C71 C 0.7169(11) 0.5501(11) 0.9468(9) 0.104(3) Uani 1 1 d DU . . H71A H 0.7543 0.5813 0.8939 0.156 Uiso 1 1 calc R A . H71B H 0.7647 0.5102 0.9816 0.156 Uiso 1 1 calc R . . H71C H 0.6799 0.5998 0.9661 0.156 Uiso 1 1 calc R . . C72X C 0.6907(12) 0.5882(8) 0.6967(12) 0.072(3) Uani 0.701(10) 1 d PDU A 1 H72A H 0.6802 0.6065 0.6423 0.086 Uiso 0.701(10) 1 calc PR A 1 H72B H 0.6253 0.6037 0.7269 0.086 Uiso 0.701(10) 1 calc PR A 1 C73X C 0.7626(12) 0.6482(8) 0.6956(10) 0.072(3) Uani 0.701(10) 1 d PDU A 1 H73A H 0.8258 0.6399 0.6600 0.087 Uiso 0.701(10) 1 calc PR A 1 H73B H 0.7792 0.6264 0.7487 0.087 Uiso 0.701(10) 1 calc PR A 1 C74X C 0.7234(13) 0.7604(9) 0.6679(9) 0.073(3) Uani 0.701(10) 1 d PDU A 1 H74A H 0.6590 0.7686 0.7023 0.087 Uiso 0.701(10) 1 calc PR A 1 H74B H 0.7738 0.7964 0.6738 0.087 Uiso 0.701(10) 1 calc PR A 1 C72Y C 0.717(3) 0.566(2) 0.6514(18) 0.073(3) Uani 0.299(10) 1 d PDU A 2 H72C H 0.7137 0.5405 0.6109 0.087 Uiso 0.299(10) 1 calc PR A 2 H72D H 0.6524 0.6056 0.6574 0.087 Uiso 0.299(10) 1 calc PR A 2 C73Y C 0.7965(19) 0.6310(13) 0.6189(19) 0.074(3) Uani 0.299(10) 1 d PDU A 2 H73C H 0.8533 0.6010 0.5906 0.089 Uiso 0.299(10) 1 calc PR A 2 H73D H 0.8215 0.6340 0.6633 0.089 Uiso 0.299(10) 1 calc PR A 2 C74Y C 0.774(2) 0.7337(14) 0.5643(17) 0.075(3) Uani 0.299(10) 1 d PDU A 2 H74C H 0.8404 0.7622 0.5426 0.090 Uiso 0.299(10) 1 calc PR A 2 H74D H 0.7499 0.7297 0.5201 0.090 Uiso 0.299(10) 1 calc PR A 2 C75 C 0.7074(9) 0.8009(9) 0.5881(7) 0.079(3) Uani 1 1 d DU . . O1S O 0.9668(9) 0.4771(9) 0.2968(7) 0.0405(19) Uani 0.50 1 d PU . . C1S C 0.9382(15) 0.5285(13) 0.2168(11) 0.041(2) Uani 0.50 1 d PU . . H1S1 H 0.8751 0.5713 0.2200 0.049 Uiso 0.50 1 calc PR . . H1S2 H 0.9927 0.5690 0.1810 0.049 Uiso 0.50 1 calc PR . . C2S C 0.9233(15) 0.4602(13) 0.1876(11) 0.042(2) Uani 0.50 1 d PU . . H2S1 H 0.9795 0.4578 0.1447 0.051 Uiso 0.50 1 calc PR . . H2S2 H 0.8587 0.4776 0.1670 0.051 Uiso 0.50 1 calc PR . . C3S C 0.9204(15) 0.3617(13) 0.2563(10) 0.040(2) Uani 0.50 1 d PU . . H3S1 H 0.8565 0.3329 0.2640 0.048 Uiso 0.50 1 calc PR . . H3S2 H 0.9781 0.3166 0.2457 0.048 Uiso 0.50 1 calc PR . . C4S C 0.9269(14) 0.3797(13) 0.3265(11) 0.039(2) Uani 0.50 1 d PU . . H4S1 H 0.9735 0.3292 0.3580 0.046 Uiso 0.50 1 calc PR . . H4S2 H 0.8592 0.3795 0.3595 0.046 Uiso 0.50 1 calc PR . . C7S C 0.8465(11) 0.0816(11) 0.9852(9) 0.024(2) Uani 0.50 1 d PU . . H7S1 H 0.8489 0.0734 1.0395 0.029 Uiso 0.50 1 calc PR . . H7S2 H 0.8318 0.0194 0.9856 0.029 Uiso 0.50 1 calc PR . . C6S C 0.9474(12) 0.1119(12) 0.9326(10) 0.038(2) Uani 0.50 1 d PU . . H5S1 H 1.0008 0.1011 0.9642 0.045 Uiso 0.50 1 calc PR . . H5S2 H 0.9691 0.0750 0.8978 0.045 Uiso 0.50 1 calc PR . . C5S C 0.9282(10) 0.2135(12) 0.8877(10) 0.035(2) Uani 0.50 1 d PDU . . H6S1 H 0.9672 0.2306 0.8339 0.042 Uiso 0.50 1 calc PR . . H6S2 H 0.9482 0.2531 0.9125 0.042 Uiso 0.50 1 calc PR . . O2S O 0.8173(8) 0.2309(8) 0.8861(7) 0.045(2) Uani 0.50 1 d PDU . . C8S C 0.7635(11) 0.1619(11) 0.9525(8) 0.028(2) Uani 0.50 1 d PDU . . H8S1 H 0.7121 0.1363 0.9374 0.034 Uiso 0.50 1 calc PR . . H8S2 H 0.7293 0.1906 0.9915 0.034 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N60 0.100(4) 0.060(4) 0.116(5) -0.025(4) -0.043(4) -0.006(3) V1 0.0125(7) 0.0181(7) 0.0167(7) -0.0088(5) -0.0022(5) -0.0006(5) V2 0.0212(7) 0.0235(7) 0.0167(7) -0.0076(6) -0.0033(6) -0.0027(6) V3 0.0160(7) 0.0288(8) 0.0234(8) -0.0157(6) 0.0008(6) -0.0016(6) V4 0.0134(7) 0.0181(7) 0.0205(7) -0.0103(6) -0.0030(5) -0.0009(5) Cl1 0.0339(12) 0.0350(12) 0.0268(11) -0.0065(9) -0.0134(9) -0.0015(9) Cl2 0.0203(11) 0.0497(14) 0.0540(15) -0.0344(12) 0.0012(10) 0.0032(10) Cl3 0.0203(10) 0.0236(10) 0.0340(11) -0.0164(9) -0.0049(8) -0.0041(8) O1 0.019(3) 0.020(3) 0.015(3) -0.009(2) -0.004(2) -0.002(2) O2 0.019(3) 0.023(3) 0.015(3) -0.009(2) 0.000(2) -0.004(2) O3 0.028(3) 0.035(3) 0.024(3) -0.011(3) -0.007(3) 0.000(3) O4 0.031(3) 0.046(4) 0.035(4) -0.020(3) 0.004(3) -0.005(3) O5 0.035(3) 0.030(3) 0.025(3) -0.011(3) 0.001(3) -0.003(3) O6 0.032(3) 0.049(4) 0.037(4) -0.026(3) -0.002(3) -0.007(3) N21 0.027(4) 0.018(3) 0.019(4) -0.006(3) -0.007(3) 0.001(3) N22 0.018(3) 0.023(3) 0.020(4) -0.010(3) -0.007(3) 0.000(3) N23 0.016(3) 0.018(3) 0.020(3) -0.008(3) -0.003(3) 0.000(3) N31 0.016(3) 0.024(3) 0.021(3) -0.012(3) -0.001(3) 0.001(3) N32 0.014(3) 0.021(3) 0.022(3) -0.009(3) -0.005(3) 0.003(3) N33 0.017(4) 0.020(3) 0.022(3) -0.012(3) -0.005(3) -0.001(3) N41 0.018(3) 0.028(4) 0.017(4) -0.006(3) -0.008(3) 0.002(3) N42 0.015(3) 0.022(3) 0.023(4) -0.008(3) -0.003(3) 0.000(3) N43 0.015(3) 0.022(3) 0.023(4) -0.014(3) -0.001(3) -0.004(3) N51 0.017(3) 0.023(4) 0.029(4) -0.014(3) -0.006(3) 0.003(3) N52 0.013(3) 0.022(3) 0.021(3) -0.011(3) -0.002(3) 0.002(3) N53 0.014(3) 0.019(3) 0.022(3) -0.011(3) -0.006(3) -0.001(3) C1 0.034(6) 0.042(6) 0.026(5) -0.017(5) -0.011(4) 0.007(4) C2 0.031(5) 0.055(6) 0.040(6) -0.029(5) 0.010(4) -0.016(5) C3 0.046(6) 0.047(6) 0.050(6) -0.019(5) -0.019(5) 0.005(5) C4 0.043(6) 0.044(6) 0.071(8) -0.011(6) 0.004(6) -0.011(5) C5 0.041(7) 0.064(8) 0.076(8) -0.025(7) 0.010(6) -0.010(6) C6 0.028(6) 0.063(8) 0.071(8) -0.014(7) 0.010(5) -0.009(5) C7 0.035(6) 0.067(7) 0.047(6) -0.022(6) -0.002(5) -0.001(5) C8 0.031(5) 0.045(6) 0.026(5) -0.008(4) 0.011(4) -0.013(5) C9 0.030(5) 0.042(5) 0.030(5) -0.020(4) 0.004(4) -0.011(4) C10 0.049(6) 0.039(6) 0.041(6) -0.006(5) -0.016(5) -0.009(5) C11 0.061(7) 0.043(6) 0.038(6) -0.024(5) -0.013(5) -0.009(5) C12 0.080(8) 0.042(6) 0.026(5) -0.009(5) -0.018(5) -0.008(5) C13 0.065(7) 0.057(7) 0.052(7) -0.041(6) 0.001(6) 0.002(6) C14 0.048(6) 0.050(6) 0.046(6) -0.022(5) -0.007(5) -0.003(5) C21 0.040(5) 0.023(5) 0.028(5) -0.009(4) -0.008(4) 0.001(4) C22 0.092(8) 0.027(5) 0.027(5) -0.006(4) -0.016(5) -0.004(5) C23 0.128(11) 0.022(5) 0.035(6) -0.002(5) -0.019(6) -0.010(6) C24 0.127(10) 0.018(5) 0.038(6) -0.007(5) -0.010(6) -0.015(6) C25 0.062(6) 0.022(5) 0.027(5) -0.012(4) -0.007(4) 0.000(4) C26 0.031(5) 0.018(4) 0.025(4) -0.011(4) -0.003(4) -0.003(3) C31 0.014(4) 0.023(4) 0.025(4) -0.012(4) -0.007(3) 0.002(3) C32 0.016(4) 0.032(5) 0.032(5) -0.015(4) 0.003(4) -0.002(3) C33 0.010(4) 0.041(5) 0.052(6) -0.022(5) 0.004(4) -0.002(4) C34 0.027(5) 0.030(5) 0.052(6) -0.019(5) -0.014(4) -0.005(4) C35 0.021(4) 0.024(4) 0.030(5) -0.013(4) -0.005(4) -0.003(3) C36 0.016(4) 0.020(4) 0.024(4) -0.006(4) -0.005(3) 0.001(3) C41 0.019(4) 0.036(5) 0.024(5) -0.014(4) -0.008(4) -0.001(4) C42 0.026(5) 0.043(5) 0.021(4) -0.006(4) -0.009(4) -0.006(4) C43 0.028(5) 0.073(7) 0.034(5) -0.028(5) -0.015(4) -0.003(5) C44 0.022(5) 0.059(6) 0.030(5) -0.017(5) -0.006(4) -0.015(4) C45 0.017(4) 0.048(5) 0.029(5) -0.018(4) 0.001(4) -0.010(4) C46 0.018(4) 0.029(4) 0.019(4) -0.012(4) -0.005(3) 0.000(3) C51 0.022(4) 0.026(5) 0.033(5) -0.018(4) -0.006(4) 0.001(3) C52 0.018(4) 0.039(5) 0.068(7) -0.038(5) -0.002(4) 0.003(4) C53 0.030(5) 0.037(6) 0.093(8) -0.048(6) -0.005(5) 0.006(4) C54 0.033(5) 0.027(5) 0.085(8) -0.030(5) -0.020(5) 0.001(4) C55 0.025(5) 0.022(5) 0.048(5) -0.017(4) -0.010(4) 0.001(4) C56 0.023(4) 0.027(5) 0.032(5) -0.020(4) -0.009(4) 0.001(3) C60X 0.102(4) 0.059(4) 0.116(5) -0.027(4) -0.043(4) -0.006(3) C61X 0.100(4) 0.059(4) 0.116(5) -0.027(4) -0.044(4) -0.008(4) C62X 0.098(4) 0.058(4) 0.115(5) -0.028(4) -0.045(4) -0.009(4) C60Y 0.101(4) 0.060(4) 0.116(5) -0.027(4) -0.042(4) -0.006(3) C61Y 0.100(4) 0.057(4) 0.117(5) -0.027(4) -0.043(4) -0.008(3) C62Y 0.099(4) 0.058(4) 0.116(5) -0.030(4) -0.044(4) -0.009(3) C63 0.093(5) 0.057(5) 0.115(5) -0.029(4) -0.047(4) -0.009(4) C64 0.102(4) 0.059(4) 0.110(5) -0.024(4) -0.045(4) -0.005(3) C65X 0.100(5) 0.057(4) 0.099(5) -0.032(4) -0.049(4) -0.003(4) C66X 0.098(5) 0.059(4) 0.098(5) -0.031(4) -0.046(4) -0.003(4) C67X 0.099(6) 0.055(6) 0.095(6) -0.034(6) -0.041(5) -0.009(5) C65Y 0.100(5) 0.060(4) 0.101(5) -0.028(4) -0.045(4) -0.001(4) C66Y 0.100(5) 0.059(5) 0.099(6) -0.030(5) -0.043(5) -0.001(4) C67Y 0.096(8) 0.060(7) 0.090(8) -0.029(6) -0.042(7) 0.001(6) C68 0.100(7) 0.137(8) 0.118(7) -0.057(6) -0.041(6) 0.020(6) C69 0.100(7) 0.135(8) 0.119(7) -0.054(6) -0.041(6) 0.022(6) C70 0.095(7) 0.131(8) 0.115(7) -0.051(6) -0.041(6) 0.030(5) C71 0.094(8) 0.119(9) 0.102(8) -0.053(7) -0.034(7) 0.036(6) C72X 0.053(5) 0.079(6) 0.081(6) -0.017(5) -0.030(5) -0.001(4) C73X 0.054(5) 0.079(5) 0.082(6) -0.020(5) -0.030(5) -0.001(4) C74X 0.050(5) 0.080(5) 0.086(6) -0.024(5) -0.026(5) 0.000(4) C72Y 0.053(6) 0.080(6) 0.082(7) -0.019(6) -0.031(6) -0.001(5) C73Y 0.055(5) 0.083(6) 0.082(6) -0.020(5) -0.030(5) -0.003(4) C74Y 0.053(6) 0.084(6) 0.083(6) -0.018(5) -0.031(5) -0.005(4) C75 0.054(5) 0.084(5) 0.087(6) -0.014(5) -0.028(5) -0.001(4) O1S 0.040(5) 0.044(5) 0.039(4) -0.014(4) -0.011(4) -0.007(4) C1S 0.039(5) 0.044(5) 0.038(4) -0.012(4) -0.009(4) -0.006(4) C2S 0.043(5) 0.048(5) 0.035(4) -0.013(4) -0.008(4) -0.008(4) C3S 0.043(5) 0.045(5) 0.034(5) -0.015(4) -0.006(4) -0.006(4) C4S 0.041(5) 0.042(5) 0.035(4) -0.014(4) -0.009(4) -0.005(4) C7S 0.018(4) 0.030(4) 0.017(4) -0.005(3) 0.004(3) 0.000(3) C6S 0.021(4) 0.036(4) 0.028(5) 0.007(4) 0.011(4) 0.006(3) C5S 0.023(4) 0.032(4) 0.028(5) 0.001(4) 0.010(4) 0.003(3) O2S 0.023(4) 0.039(4) 0.038(4) 0.008(3) 0.010(3) 0.009(3) C8S 0.020(4) 0.032(5) 0.022(4) -0.005(4) 0.005(3) 0.003(3) _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 N60 C60Y 1.461(12) . ? N60 C60X 1.472(15) . ? N60 C64 1.495(11) . ? N60 C72X 1.564(12) . ? N60 C68 1.564(13) . ? N60 C72Y 1.572(14) . ? V1 O1 2.016(4) . ? V1 O1 2.025(5) 2_656 ? V1 O2 2.051(5) . ? V1 N42 2.135(6) . ? V1 N32 2.146(6) . ? V1 N52 2.148(6) . ? V1 N22 2.167(6) . ? V2 O2 1.886(5) . ? V2 O5 2.012(5) . ? V2 O3 2.034(6) . ? V2 N21 2.121(6) . ? V2 N41 2.145(6) . ? V2 Cl1 2.355(2) . ? V3 O2 1.905(5) . ? V3 O4 1.974(6) . ? V3 O6 1.998(6) . ? V3 N51 2.117(6) . ? V3 N31 2.118(6) . ? V3 Cl2 2.356(2) . ? V4 O1 1.793(5) . ? V4 N33 2.122(6) . ? V4 N43 2.131(6) . ? V4 N23 2.132(6) . ? V4 N53 2.145(6) . ? V4 Cl3 2.354(2) . ? O1 V1 2.025(5) 2_656 ? O3 C1 1.237(10) . ? O4 C1 1.215(10) . ? O5 C8 1.242(10) . ? O6 C8 1.229(11) . ? N21 N22 1.323(8) . ? N21 C21 1.377(10) . ? N22 N23 1.332(8) . ? N23 C26 1.362(10) . ? N31 N32 1.327(8) . ? N31 C31 1.375(9) . ? N32 N33 1.347(8) . ? N33 C36 1.371(9) . ? N41 N42 1.338(8) . ? N41 C41 1.352(9) . ? N42 N43 1.340(8) 2_656 ? N43 N42 1.340(8) 2_656 ? N43 C46 1.375(9) . ? N51 N52 1.336(8) . ? N51 C51 1.374(9) . ? N52 N53 1.331(8) 2_656 ? N53 N52 1.331(8) 2_656 ? N53 C56 1.368(9) . ? C1 C2 1.501(12) . ? C2 C3 1.364(13) . ? C2 C7 1.407(13) . ? C3 C4 1.369(14) . ? C3 H3 0.9300 . ? C4 C5 1.395(15) . ? C4 H4 0.9300 . ? C5 C6 1.322(15) . ? C5 H5 0.9300 . ? C6 C7 1.369(14) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.489(12) . ? C9 C10 1.358(12) . ? C9 C14 1.404(13) . ? C10 C11 1.364(12) . ? C10 H10 0.9300 . ? C11 C12 1.346(13) . ? C11 H11 0.9300 . ? C12 C13 1.356(14) . ? C12 H12 0.9300 . ? C13 C14 1.379(13) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C21 C22 1.379(12) . ? C21 C26 1.429(11) . ? C22 C23 1.375(13) . ? C22 H22 0.9300 . ? C23 C24 1.414(14) . ? C23 H23 0.9300 . ? C24 C25 1.374(13) . ? C24 H24 0.9300 . ? C25 C26 1.404(11) . ? C25 H25 0.9300 . ? C31 C32 1.389(10) . ? C31 C36 1.395(10) . ? C32 C33 1.365(11) . ? C32 H32 0.9300 . ? C33 C34 1.411(11) . ? C33 H33 0.9300 . ? C34 C35 1.383(11) . ? C34 H34 0.9300 . ? C35 C36 1.403(10) . ? C35 H35 0.9300 . ? C41 C42 1.407(11) . ? C41 C46 1.409(11) 2_656 ? C42 C43 1.371(12) . ? C42 H42 0.9300 . ? C43 C44 1.404(12) 2_656 ? C43 H43 0.9300 . ? C44 C45 1.388(12) . ? C44 C43 1.404(12) 2_656 ? C44 H44 0.9300 . ? C45 C46 1.373(11) . ? C45 H45 0.9300 . ? C46 C41 1.409(11) 2_656 ? C51 C52 1.401(11) . ? C51 C56 1.410(11) 2_656 ? C52 C53 1.361(12) . ? C52 H52 0.9300 . ? C53 C54 1.394(13) 2_656 ? C53 H53 0.9300 . ? C54 C55 1.358(11) . ? C54 C53 1.394(13) 2_656 ? C54 H54 0.9300 . ? C55 C56 1.386(11) . ? C55 H55 0.9300 . ? C56 C51 1.410(11) 2_656 ? C60X C61X 1.479(13) . ? C60X H60A 0.9700 . ? C60X H60B 0.9700 . ? C61X C62X 1.406(13) . ? C61X H61A 0.9700 . ? C61X H61B 0.9700 . ? C62X C63 1.418(13) . ? C62X H62A 0.9700 . ? C62X H62B 0.9700 . ? C60Y C61Y 1.487(12) . ? C60Y H60C 0.9700 . ? C60Y H60D 0.9700 . ? C61Y C62Y 1.404(12) . ? C61Y H61C 0.9700 . ? C61Y H61D 0.9700 . ? C62Y C63 1.408(11) . ? C62Y H62C 0.9700 . ? C62Y H62D 0.9700 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 C65Y 1.263(14) . ? C64 C65X 1.520(14) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65X C66X 1.468(15) . ? C65X H65A 0.9700 . ? C65X H65B 0.9700 . ? C66X C67X 1.465(16) . ? C66X H66A 0.9700 . ? C66X H66B 0.9700 . ? C67X H67A 0.9600 . ? C67X H67B 0.9600 . ? C67X H67C 0.9600 . ? C65Y C66Y 1.419(18) . ? C65Y H65C 0.9700 . ? C65Y H65D 0.9700 . ? C66Y C67Y 1.484(19) . ? C66Y H66C 0.9700 . ? C66Y H66D 0.9700 . ? C67Y H67D 0.9600 . ? C67Y H67E 0.9600 . ? C67Y H67F 0.9600 . ? C68 C69 1.453(14) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.498(13) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.411(14) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72X C73X 1.398(14) . ? C72X H72A 0.9700 . ? C72X H72B 0.9700 . ? C73X C74X 1.565(14) . ? C73X H73A 0.9700 . ? C73X H73B 0.9700 . ? C74X C75 1.407(15) . ? C74X H74A 0.9700 . ? C74X H74B 0.9700 . ? C72Y C73Y 1.418(19) . ? C72Y H72C 0.9700 . ? C72Y H72D 0.9700 . ? C73Y C74Y 1.479(17) . ? C73Y H73C 0.9700 . ? C73Y H73D 0.9700 . ? C74Y C75 1.362(19) . ? C74Y H74C 0.9700 . ? C74Y H74D 0.9700 . ? O1S C4S 1.47(2) . ? O1S C1S 1.47(2) . ? C1S C2S 1.38(2) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S C3S 1.51(2) . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C3S C4S 1.45(2) . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C4S H4S1 0.9700 . ? C4S H4S2 0.9700 . ? C7S C6S 1.49(2) . ? C7S C8S 1.51(2) . ? C7S H7S1 0.9700 . ? C7S H7S2 0.9700 . ? C6S C5S 1.41(2) . ? C6S H5S1 0.9700 . ? C6S H5S2 0.9700 . ? C5S O2S 1.458(14) . ? C5S H6S1 0.9700 . ? C5S H6S2 0.9700 . ? O2S C8S 1.387(14) . ? C8S H8S1 0.9700 . ? C8S H8S2 0.9700 . ? 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 C60Y N60 C60X 27(3) . . ? C60Y N60 C64 104.0(10) . . ? C60X N60 C64 101(3) . . ? C60Y N60 C72X 123.3(12) . . ? C60X N60 C72X 102.0(19) . . ? C64 N60 C72X 112.8(9) . . ? C60Y N60 C68 105.9(10) . . ? C60X N60 C68 130(4) . . ? C64 N60 C68 114.0(11) . . ? C72X N60 C68 96.8(11) . . ? C60Y N60 C72Y 96.5(18) . . ? C60X N60 C72Y 70(3) . . ? C64 N60 C72Y 100.2(13) . . ? C72X N60 C72Y 37.0(16) . . ? C68 N60 C72Y 132.1(18) . . ? O1 V1 O1 68.0(2) . 2_656 ? O1 V1 O2 146.11(19) . . ? O1 V1 O2 145.88(19) 2_656 . ? O1 V1 N42 125.0(2) . . ? O1 V1 N42 77.5(2) 2_656 . ? O2 V1 N42 77.6(2) . . ? O1 V1 N32 77.2(2) . . ? O1 V1 N32 124.5(2) 2_656 . ? O2 V1 N32 77.9(2) . . ? N42 V1 N32 155.5(2) . . ? O1 V1 N52 125.5(2) . . ? O1 V1 N52 76.8(2) 2_656 . ? O2 V1 N52 77.4(2) . . ? N42 V1 N52 83.4(2) . . ? N32 V1 N52 91.2(2) . . ? O1 V1 N22 77.3(2) . . ? O1 V1 N22 126.7(2) 2_656 . ? O2 V1 N22 77.1(2) . . ? N42 V1 N22 92.0(2) . . ? N32 V1 N22 82.6(2) . . ? N52 V1 N22 154.5(2) . . ? O2 V2 O5 92.5(2) . . ? O2 V2 O3 92.4(2) . . ? O5 V2 O3 92.9(2) . . ? O2 V2 N21 83.9(2) . . ? O5 V2 N21 176.4(2) . . ? O3 V2 N21 87.9(2) . . ? O2 V2 N41 84.6(2) . . ? O5 V2 N41 88.1(2) . . ? O3 V2 N41 176.9(2) . . ? N21 V2 N41 90.9(2) . . ? O2 V2 Cl1 174.97(16) . . ? O5 V2 Cl1 91.60(17) . . ? O3 V2 Cl1 90.19(16) . . ? N21 V2 Cl1 91.94(17) . . ? N41 V2 Cl1 92.73(17) . . ? O2 V3 O4 94.0(2) . . ? O2 V3 O6 92.0(2) . . ? O4 V3 O6 93.0(2) . . ? O2 V3 N51 85.0(2) . . ? O4 V3 N51 177.3(2) . . ? O6 V3 N51 89.6(2) . . ? O2 V3 N31 84.1(2) . . ? O4 V3 N31 87.9(2) . . ? O6 V3 N31 176.1(2) . . ? N51 V3 N31 89.5(2) . . ? O2 V3 Cl2 175.80(16) . . ? O4 V3 Cl2 88.78(19) . . ? O6 V3 Cl2 91.03(18) . . ? N51 V3 Cl2 92.08(17) . . ? N31 V3 Cl2 92.82(17) . . ? O1 V4 N33 84.8(2) . . ? O1 V4 N43 84.5(2) . . ? N33 V4 N43 90.4(2) . . ? O1 V4 N23 85.3(2) . . ? N33 V4 N23 87.1(2) . . ? N43 V4 N23 169.7(2) . . ? O1 V4 N53 83.0(2) . . ? N33 V4 N53 167.6(2) . . ? N43 V4 N53 90.7(2) . . ? N23 V4 N53 89.6(2) . . ? O1 V4 Cl3 178.61(17) . . ? N33 V4 Cl3 96.43(17) . . ? N43 V4 Cl3 94.78(16) . . ? N23 V4 Cl3 95.40(17) . . ? N53 V4 Cl3 95.81(16) . . ? V4 O1 V1 124.1(2) . . ? V4 O1 V1 123.9(2) . 2_656 ? V1 O1 V1 112.0(2) . 2_656 ? V2 O2 V3 123.0(2) . . ? V2 O2 V1 118.8(2) . . ? V3 O2 V1 118.1(2) . . ? C1 O3 V2 132.7(6) . . ? C1 O4 V3 133.1(6) . . ? C8 O5 V2 133.4(6) . . ? C8 O6 V3 135.5(6) . . ? N22 N21 C21 107.4(6) . . ? N22 N21 V2 115.1(4) . . ? C21 N21 V2 133.2(5) . . ? N21 N22 N23 112.4(6) . . ? N21 N22 V1 122.3(4) . . ? N23 N22 V1 124.0(4) . . ? N22 N23 C26 107.2(6) . . ? N22 N23 V4 112.6(4) . . ? C26 N23 V4 138.7(5) . . ? N32 N31 C31 107.3(5) . . ? N32 N31 V3 115.1(4) . . ? C31 N31 V3 133.6(5) . . ? N31 N32 N33 111.8(5) . . ? N31 N32 V1 122.7(4) . . ? N33 N32 V1 124.1(4) . . ? N32 N33 C36 106.2(5) . . ? N32 N33 V4 112.5(4) . . ? C36 N33 V4 139.9(5) . . ? N42 N41 C41 107.4(6) . . ? N42 N41 V2 113.5(4) . . ? C41 N41 V2 134.6(5) . . ? N41 N42 N43 111.8(6) . 2_656 ? N41 N42 V1 123.3(5) . . ? N43 N42 V1 124.1(5) 2_656 . ? N42 N43 C46 106.3(6) 2_656 . ? N42 N43 V4 112.9(4) 2_656 . ? C46 N43 V4 140.1(5) . . ? N52 N51 C51 105.5(6) . . ? N52 N51 V3 114.3(4) . . ? C51 N51 V3 137.9(5) . . ? N53 N52 N51 113.0(5) 2_656 . ? N53 N52 V1 124.6(4) 2_656 . ? N51 N52 V1 122.4(4) . . ? N52 N53 C56 106.9(6) 2_656 . ? N52 N53 V4 111.9(4) 2_656 . ? C56 N53 V4 140.4(5) . . ? O4 C1 O3 126.8(9) . . ? O4 C1 C2 117.5(8) . . ? O3 C1 C2 115.7(8) . . ? C3 C2 C7 117.7(9) . . ? C3 C2 C1 123.1(9) . . ? C7 C2 C1 119.2(9) . . ? C2 C3 C4 122.6(10) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C3 C4 C5 117.6(10) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? C6 C5 C4 121.0(10) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 121.7(11) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C6 C7 C2 119.3(10) . . ? C6 C7 H7 120.4 . . ? C2 C7 H7 120.4 . . ? O6 C8 O5 124.0(9) . . ? O6 C8 C9 118.5(8) . . ? O5 C8 C9 117.5(8) . . ? C10 C9 C14 118.2(8) . . ? C10 C9 C8 123.3(8) . . ? C14 C9 C8 118.3(8) . . ? C9 C10 C11 121.8(9) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C12 C11 C10 120.6(9) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 119.0(9) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C12 C13 C14 122.2(10) . . ? C12 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C13 C14 C9 118.1(9) . . ? C13 C14 H14 120.9 . . ? C9 C14 H14 120.9 . . ? N21 C21 C22 131.7(8) . . ? N21 C21 C26 106.0(7) . . ? C22 C21 C26 122.2(8) . . ? C23 C22 C21 116.6(9) . . ? C23 C22 H22 121.7 . . ? C21 C22 H22 121.7 . . ? C22 C23 C24 122.0(9) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C25 C24 C23 122.0(9) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C24 C25 C26 116.8(8) . . ? C24 C25 H25 121.6 . . ? C26 C25 H25 121.6 . . ? N23 C26 C25 132.8(7) . . ? N23 C26 C21 107.0(6) . . ? C25 C26 C21 120.3(7) . . ? N31 C31 C32 131.2(7) . . ? N31 C31 C36 106.7(6) . . ? C32 C31 C36 122.1(7) . . ? C33 C32 C31 116.5(7) . . ? C33 C32 H32 121.7 . . ? C31 C32 H32 121.7 . . ? C32 C33 C34 122.2(7) . . ? C32 C33 H33 118.9 . . ? C34 C33 H33 118.9 . . ? C35 C34 C33 121.7(7) . . ? C35 C34 H34 119.2 . . ? C33 C34 H34 119.2 . . ? C34 C35 C36 116.1(7) . . ? C34 C35 H35 122.0 . . ? C36 C35 H35 122.0 . . ? N33 C36 C31 108.0(6) . . ? N33 C36 C35 130.6(7) . . ? C31 C36 C35 121.4(7) . . ? N41 C41 C42 130.9(7) . . ? N41 C41 C46 107.3(6) . 2_656 ? C42 C41 C46 121.8(7) . 2_656 ? C43 C42 C41 116.1(8) . . ? C43 C42 H42 121.9 . . ? C41 C42 H42 121.9 . . ? C42 C43 C44 122.2(8) . 2_656 ? C42 C43 H43 118.9 . . ? C44 C43 H43 118.9 2_656 . ? C45 C44 C43 121.4(8) . 2_656 ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 2_656 . ? C46 C45 C44 117.5(8) . . ? C46 C45 H45 121.3 . . ? C44 C45 H45 121.3 . . ? C45 C46 N43 131.9(7) . . ? C45 C46 C41 121.0(7) . 2_656 ? N43 C46 C41 107.2(6) . 2_656 ? N51 C51 C52 131.4(7) . . ? N51 C51 C56 108.0(6) . 2_656 ? C52 C51 C56 120.6(7) . 2_656 ? C53 C52 C51 116.3(8) . . ? C53 C52 H52 121.9 . . ? C51 C52 H52 121.9 . . ? C52 C53 C54 122.8(8) . 2_656 ? C52 C53 H53 118.6 . . ? C54 C53 H53 118.6 2_656 . ? C55 C54 C53 121.8(8) . 2_656 ? C55 C54 H54 119.1 . . ? C53 C54 H54 119.1 2_656 . ? C54 C55 C56 117.0(8) . . ? C54 C55 H55 121.5 . . ? C56 C55 H55 121.5 . . ? N53 C56 C55 132.0(7) . . ? N53 C56 C51 106.5(6) . 2_656 ? C55 C56 C51 121.4(7) . 2_656 ? N60 C60X C61X 123(2) . . ? N60 C60X H60A 106.6 . . ? C61X C60X H60A 106.6 . . ? N60 C60X H60B 106.6 . . ? C61X C60X H60B 106.6 . . ? H60A C60X H60B 106.6 . . ? C62X C61X C60X 123(2) . . ? C62X C61X H61A 106.7 . . ? C60X C61X H61A 106.7 . . ? C62X C61X H61B 106.7 . . ? C60X C61X H61B 106.7 . . ? H61A C61X H61B 106.6 . . ? C61X C62X C63 133(2) . . ? C61X C62X H62A 104.0 . . ? C63 C62X H62A 104.0 . . ? C61X C62X H62B 104.0 . . ? C63 C62X H62B 104.0 . . ? H62A C62X H62B 105.5 . . ? N60 C60Y C61Y 115.7(11) . . ? N60 C60Y H60C 108.4 . . ? C61Y C60Y H60C 108.4 . . ? N60 C60Y H60D 108.4 . . ? C61Y C60Y H60D 108.4 . . ? H60C C60Y H60D 107.4 . . ? C62Y C61Y C60Y 115.0(12) . . ? C62Y C61Y H61C 108.5 . . ? C60Y C61Y H61C 108.5 . . ? C62Y C61Y H61D 108.5 . . ? C60Y C61Y H61D 108.5 . . ? H61C C61Y H61D 107.5 . . ? C61Y C62Y C63 122.8(12) . . ? C61Y C62Y H62C 106.6 . . ? C63 C62Y H62C 106.6 . . ? C61Y C62Y H62D 106.6 . . ? C63 C62Y H62D 106.6 . . ? H62C C62Y H62D 106.6 . . ? C62Y C63 C62X 22(2) . . ? C62Y C63 H63A 107.5 . . ? C62X C63 H63A 109.5 . . ? C62Y C63 H63B 90.9 . . ? C62X C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62Y C63 H63C 127.9 . . ? C62X C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65Y C64 N60 159(2) . . ? C65Y C64 C65X 44(2) . . ? N60 C64 C65X 117.1(10) . . ? C65Y C64 H64A 76.3 . . ? N60 C64 H64A 108.0 . . ? C65X C64 H64A 108.0 . . ? C65Y C64 H64B 89.6 . . ? N60 C64 H64B 108.0 . . ? C65X C64 H64B 108.0 . . ? H64A C64 H64B 107.3 . . ? C66X C65X C64 112.2(12) . . ? C66X C65X H65A 109.2 . . ? C64 C65X H65A 109.2 . . ? C66X C65X H65B 109.2 . . ? C64 C65X H65B 109.2 . . ? H65A C65X H65B 107.9 . . ? C67X C66X C65X 117.1(14) . . ? C67X C66X H66A 108.0 . . ? C65X C66X H66A 108.0 . . ? C67X C66X H66B 108.0 . . ? C65X C66X H66B 108.0 . . ? H66A C66X H66B 107.3 . . ? C64 C65Y C66Y 147(3) . . ? C64 C65Y H65C 100.0 . . ? C66Y C65Y H65C 100.0 . . ? C64 C65Y H65D 100.0 . . ? C66Y C65Y H65D 100.0 . . ? H65C C65Y H65D 104.2 . . ? C65Y C66Y C67Y 121(2) . . ? C65Y C66Y H66C 107.0 . . ? C67Y C66Y H66C 107.0 . . ? C65Y C66Y H66D 107.0 . . ? C67Y C66Y H66D 107.0 . . ? H66C C66Y H66D 106.7 . . ? C66Y C67Y H67D 109.5 . . ? C66Y C67Y H67E 109.5 . . ? H67D C67Y H67E 109.5 . . ? C66Y C67Y H67F 109.5 . . ? H67D C67Y H67F 109.5 . . ? H67E C67Y H67F 109.5 . . ? C69 C68 N60 121.1(11) . . ? C69 C68 H68A 107.0 . . ? N60 C68 H68A 107.0 . . ? C69 C68 H68B 107.0 . . ? N60 C68 H68B 107.0 . . ? H68A C68 H68B 106.8 . . ? C68 C69 C70 112.9(11) . . ? C68 C69 H69A 109.0 . . ? C70 C69 H69A 109.0 . . ? C68 C69 H69B 109.0 . . ? C70 C69 H69B 109.0 . . ? H69A C69 H69B 107.8 . . ? C71 C70 C69 119.8(14) . . ? C71 C70 H70A 107.4 . . ? C69 C70 H70A 107.4 . . ? C71 C70 H70B 107.4 . . ? C69 C70 H70B 107.4 . . ? H70A C70 H70B 106.9 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C73X C72X N60 117.7(11) . . ? C73X C72X H72A 107.9 . . ? N60 C72X H72A 107.9 . . ? C73X C72X H72B 107.9 . . ? N60 C72X H72B 107.9 . . ? H72A C72X H72B 107.2 . . ? C72X C73X C74X 113.5(11) . . ? C72X C73X H73A 108.9 . . ? C74X C73X H73A 108.9 . . ? C72X C73X H73B 108.9 . . ? C74X C73X H73B 108.9 . . ? H73A C73X H73B 107.7 . . ? C75 C74X C73X 112.8(12) . . ? C75 C74X H74A 109.0 . . ? C73X C74X H74A 109.0 . . ? C75 C74X H74B 109.0 . . ? C73X C74X H74B 109.0 . . ? H74A C74X H74B 107.8 . . ? C73Y C72Y N60 122.7(19) . . ? C73Y C72Y H72C 106.6 . . ? N60 C72Y H72C 106.6 . . ? C73Y C72Y H72D 106.6 . . ? N60 C72Y H72D 106.6 . . ? H72C C72Y H72D 106.6 . . ? C72Y C73Y C74Y 119.8(19) . . ? C72Y C73Y H73C 107.4 . . ? C74Y C73Y H73C 107.4 . . ? C72Y C73Y H73D 107.4 . . ? C74Y C73Y H73D 107.4 . . ? H73C C73Y H73D 106.9 . . ? C75 C74Y C73Y 123(2) . . ? C75 C74Y H74C 106.6 . . ? C73Y C74Y H74C 106.6 . . ? C75 C74Y H74D 106.6 . . ? C73Y C74Y H74D 106.6 . . ? H74C C74Y H74D 106.6 . . ? C74Y C75 C74X 95.8(16) . . ? C4S O1S C1S 104.6(12) . . ? C2S C1S O1S 109.7(15) . . ? C2S C1S H1S1 109.7 . . ? O1S C1S H1S1 109.7 . . ? C2S C1S H1S2 109.7 . . ? O1S C1S H1S2 109.7 . . ? H1S1 C1S H1S2 108.2 . . ? C1S C2S C3S 106.8(15) . . ? C1S C2S H2S1 110.4 . . ? C3S C2S H2S1 110.4 . . ? C1S C2S H2S2 110.4 . . ? C3S C2S H2S2 110.4 . . ? H2S1 C2S H2S2 108.6 . . ? C4S C3S C2S 106.9(15) . . ? C4S C3S H3S1 110.3 . . ? C2S C3S H3S1 110.3 . . ? C4S C3S H3S2 110.3 . . ? C2S C3S H3S2 110.3 . . ? H3S1 C3S H3S2 108.6 . . ? C3S C4S O1S 106.0(14) . . ? C3S C4S H4S1 110.5 . . ? O1S C4S H4S1 110.5 . . ? C3S C4S H4S2 110.5 . . ? O1S C4S H4S2 110.5 . . ? H4S1 C4S H4S2 108.7 . . ? C6S C7S C8S 107.6(12) . . ? C6S C7S H7S1 110.2 . . ? C8S C7S H7S1 110.2 . . ? C6S C7S H7S2 110.2 . . ? C8S C7S H7S2 110.2 . . ? H7S1 C7S H7S2 108.5 . . ? C5S C6S C7S 104.8(13) . . ? C5S C6S H5S1 110.8 . . ? C7S C6S H5S1 110.8 . . ? C5S C6S H5S2 110.8 . . ? C7S C6S H5S2 110.8 . . ? H5S1 C6S H5S2 108.9 . . ? C6S C5S O2S 106.4(13) . . ? C6S C5S H6S1 110.5 . . ? O2S C5S H6S1 110.5 . . ? C6S C5S H6S2 110.5 . . ? O2S C5S H6S2 110.5 . . ? H6S1 C5S H6S2 108.6 . . ? C8S O2S C5S 110.8(11) . . ? O2S C8S C7S 103.9(11) . . ? O2S C8S H8S1 111.0 . . ? C7S C8S H8S1 111.0 . . ? O2S C8S H8S2 111.0 . . ? C7S C8S H8S2 111.0 . . ? H8S1 C8S H8S2 109.0 . . ? 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 N33 V4 O1 V1 -44.2(3) . . . . ? N43 V4 O1 V1 -135.2(3) . . . . ? N23 V4 O1 V1 43.3(3) . . . . ? N53 V4 O1 V1 133.4(3) . . . . ? Cl3 V4 O1 V1 164(7) . . . . ? N33 V4 O1 V1 134.5(3) . . . 2_656 ? N43 V4 O1 V1 43.6(3) . . . 2_656 ? N23 V4 O1 V1 -138.0(3) . . . 2_656 ? N53 V4 O1 V1 -47.8(3) . . . 2_656 ? Cl3 V4 O1 V1 -17(7) . . . 2_656 ? O1 V1 O1 V4 178.9(5) 2_656 . . . ? O2 V1 O1 V4 -0.6(5) . . . . ? N42 V1 O1 V4 -125.7(3) . . . . ? N32 V1 O1 V4 42.9(3) . . . . ? N52 V1 O1 V4 125.1(3) . . . . ? N22 V1 O1 V4 -42.3(3) . . . . ? O1 V1 O1 V1 0.000(2) 2_656 . . 2_656 ? O2 V1 O1 V1 -179.5(3) . . . 2_656 ? N42 V1 O1 V1 55.4(3) . . . 2_656 ? N32 V1 O1 V1 -136.0(3) . . . 2_656 ? N52 V1 O1 V1 -53.8(3) . . . 2_656 ? N22 V1 O1 V1 138.8(3) . . . 2_656 ? O5 V2 O2 V3 48.1(3) . . . . ? O3 V2 O2 V3 -45.0(3) . . . . ? N21 V2 O2 V3 -132.6(3) . . . . ? N41 V2 O2 V3 135.9(3) . . . . ? Cl1 V2 O2 V3 -166.4(17) . . . . ? O5 V2 O2 V1 -132.5(3) . . . . ? O3 V2 O2 V1 134.5(3) . . . . ? N21 V2 O2 V1 46.8(3) . . . . ? N41 V2 O2 V1 -44.7(3) . . . . ? Cl1 V2 O2 V1 13(2) . . . . ? O4 V3 O2 V2 46.2(3) . . . . ? O6 V3 O2 V2 -47.0(3) . . . . ? N51 V3 O2 V2 -136.4(3) . . . . ? N31 V3 O2 V2 133.6(3) . . . . ? Cl2 V3 O2 V2 177(2) . . . . ? O4 V3 O2 V1 -133.2(3) . . . . ? O6 V3 O2 V1 133.6(3) . . . . ? N51 V3 O2 V1 44.2(3) . . . . ? N31 V3 O2 V1 -45.8(3) . . . . ? Cl2 V3 O2 V1 -2(2) . . . . ? O1 V1 O2 V2 -89.4(4) . . . . ? O1 V1 O2 V2 91.4(4) 2_656 . . . ? N42 V1 O2 V2 47.3(3) . . . . ? N32 V1 O2 V2 -132.8(3) . . . . ? N52 V1 O2 V2 133.2(3) . . . . ? N22 V1 O2 V2 -47.7(3) . . . . ? O1 V1 O2 V3 90.0(4) . . . . ? O1 V1 O2 V3 -89.2(4) 2_656 . . . ? N42 V1 O2 V3 -133.2(3) . . . . ? N32 V1 O2 V3 46.7(3) . . . . ? N52 V1 O2 V3 -47.3(3) . . . . ? N22 V1 O2 V3 131.7(3) . . . . ? O2 V2 O3 C1 16.2(7) . . . . ? O5 V2 O3 C1 -76.5(7) . . . . ? N21 V2 O3 C1 100.0(7) . . . . ? N41 V2 O3 C1 32(4) . . . . ? Cl1 V2 O3 C1 -168.1(7) . . . . ? O2 V3 O4 C1 -17.6(8) . . . . ? O6 V3 O4 C1 74.6(8) . . . . ? N51 V3 O4 C1 -86(5) . . . . ? N31 V3 O4 C1 -101.6(7) . . . . ? Cl2 V3 O4 C1 165.5(7) . . . . ? O2 V2 O5 C8 -19.0(7) . . . . ? O3 V2 O5 C8 73.6(7) . . . . ? N21 V2 O5 C8 -29(4) . . . . ? N41 V2 O5 C8 -103.5(7) . . . . ? Cl1 V2 O5 C8 163.9(7) . . . . ? O2 V3 O6 C8 15.8(8) . . . . ? O4 V3 O6 C8 -78.3(8) . . . . ? N51 V3 O6 C8 100.8(8) . . . . ? N31 V3 O6 C8 25(4) . . . . ? Cl2 V3 O6 C8 -167.2(8) . . . . ? O2 V2 N21 N22 -21.1(5) . . . . ? O5 V2 N21 N22 -11(4) . . . . ? O3 V2 N21 N22 -113.8(5) . . . . ? N41 V2 N21 N22 63.3(5) . . . . ? Cl1 V2 N21 N22 156.1(5) . . . . ? O2 V2 N21 C21 131.9(7) . . . . ? O5 V2 N21 C21 142(4) . . . . ? O3 V2 N21 C21 39.2(7) . . . . ? N41 V2 N21 C21 -143.6(7) . . . . ? Cl1 V2 N21 C21 -50.9(7) . . . . ? C21 N21 N22 N23 0.1(8) . . . . ? V2 N21 N22 N23 159.8(4) . . . . ? C21 N21 N22 V1 -167.2(5) . . . . ? V2 N21 N22 V1 -7.5(7) . . . . ? O1 V1 N22 N21 -172.5(6) . . . . ? O1 V1 N22 N21 -122.9(5) 2_656 . . . ? O2 V1 N22 N21 29.8(5) . . . . ? N42 V1 N22 N21 -47.0(5) . . . . ? N32 V1 N22 N21 109.0(5) . . . . ? N52 V1 N22 N21 31.9(9) . . . . ? O1 V1 N22 N23 21.7(5) . . . . ? O1 V1 N22 N23 71.3(6) 2_656 . . . ? O2 V1 N22 N23 -136.0(5) . . . . ? N42 V1 N22 N23 147.2(5) . . . . ? N32 V1 N22 N23 -56.8(5) . . . . ? N52 V1 N22 N23 -133.9(6) . . . . ? N21 N22 N23 C26 -0.4(8) . . . . ? V1 N22 N23 C26 166.6(5) . . . . ? N21 N22 N23 V4 -169.1(4) . . . . ? V1 N22 N23 V4 -2.0(6) . . . . ? O1 V4 N23 N22 -20.9(4) . . . . ? N33 V4 N23 N22 64.1(5) . . . . ? N43 V4 N23 N22 -12.2(15) . . . . ? N53 V4 N23 N22 -103.9(5) . . . . ? Cl3 V4 N23 N22 160.3(4) . . . . ? O1 V4 N23 C26 175.6(7) . . . . ? N33 V4 N23 C26 -99.4(7) . . . . ? N43 V4 N23 C26 -175.7(11) . . . . ? N53 V4 N23 C26 92.6(7) . . . . ? Cl3 V4 N23 C26 -3.2(7) . . . . ? O2 V3 N31 N32 21.2(5) . . . . ? O4 V3 N31 N32 115.4(5) . . . . ? O6 V3 N31 N32 12(4) . . . . ? N51 V3 N31 N32 -63.9(5) . . . . ? Cl2 V3 N31 N32 -155.9(5) . . . . ? O2 V3 N31 C31 -132.9(7) . . . . ? O4 V3 N31 C31 -38.6(7) . . . . ? O6 V3 N31 C31 -142(3) . . . . ? N51 V3 N31 C31 142.1(7) . . . . ? Cl2 V3 N31 C31 50.0(7) . . . . ? C31 N31 N32 N33 0.8(8) . . . . ? V3 N31 N32 N33 -159.8(4) . . . . ? C31 N31 N32 V1 167.7(5) . . . . ? V3 N31 N32 V1 7.1(7) . . . . ? O1 V1 N32 N31 173.6(6) . . . . ? O1 V1 N32 N31 122.2(5) 2_656 . . . ? O2 V1 N32 N31 -29.5(5) . . . . ? N42 V1 N32 N31 -29.3(9) . . . . ? N52 V1 N32 N31 47.4(5) . . . . ? N22 V1 N32 N31 -107.8(5) . . . . ? O1 V1 N32 N33 -21.1(5) . . . . ? O1 V1 N32 N33 -72.5(6) 2_656 . . . ? O2 V1 N32 N33 135.8(5) . . . . ? N42 V1 N32 N33 136.0(6) . . . . ? N52 V1 N32 N33 -147.3(5) . . . . ? N22 V1 N32 N33 57.5(5) . . . . ? N31 N32 N33 C36 -1.4(7) . . . . ? V1 N32 N33 C36 -168.1(5) . . . . ? N31 N32 N33 V4 167.5(4) . . . . ? V1 N32 N33 V4 0.8(6) . . . . ? O1 V4 N33 N32 22.1(5) . . . . ? N43 V4 N33 N32 106.6(5) . . . . ? N23 V4 N33 N32 -63.5(5) . . . . ? N53 V4 N33 N32 11.1(14) . . . . ? Cl3 V4 N33 N32 -158.6(4) . . . . ? O1 V4 N33 C36 -174.5(8) . . . . ? N43 V4 N33 C36 -90.1(8) . . . . ? N23 V4 N33 C36 99.9(8) . . . . ? N53 V4 N33 C36 174.5(9) . . . . ? Cl3 V4 N33 C36 4.8(8) . . . . ? O2 V2 N41 N42 17.7(5) . . . . ? O5 V2 N41 N42 110.4(5) . . . . ? O3 V2 N41 N42 2(4) . . . . ? N21 V2 N41 N42 -66.1(5) . . . . ? Cl1 V2 N41 N42 -158.1(5) . . . . ? O2 V2 N41 C41 -134.9(7) . . . . ? O5 V2 N41 C41 -42.1(7) . . . . ? O3 V2 N41 C41 -151(4) . . . . ? N21 V2 N41 C41 141.4(7) . . . . ? Cl1 V2 N41 C41 49.4(7) . . . . ? C41 N41 N42 N43 2.3(8) . . . 2_656 ? V2 N41 N42 N43 -157.6(4) . . . 2_656 ? C41 N41 N42 V1 171.9(5) . . . . ? V2 N41 N42 V1 12.0(7) . . . . ? O1 V1 N42 N41 119.5(5) . . . . ? O1 V1 N42 N41 170.9(6) 2_656 . . . ? O2 V1 N42 N41 -32.7(5) . . . . ? N32 V1 N42 N41 -32.9(9) . . . . ? N52 V1 N42 N41 -111.2(5) . . . . ? N22 V1 N42 N41 43.6(5) . . . . ? O1 V1 N42 N43 -72.2(6) . . . 2_656 ? O1 V1 N42 N43 -20.8(5) 2_656 . . 2_656 ? O2 V1 N42 N43 135.6(5) . . . 2_656 ? N32 V1 N42 N43 135.4(6) . . . 2_656 ? N52 V1 N42 N43 57.1(5) . . . 2_656 ? N22 V1 N42 N43 -148.1(5) . . . 2_656 ? O1 V4 N43 N42 -22.1(4) . . . 2_656 ? N33 V4 N43 N42 -106.8(5) . . . 2_656 ? N23 V4 N43 N42 -30.8(15) . . . 2_656 ? N53 V4 N43 N42 60.8(5) . . . 2_656 ? Cl3 V4 N43 N42 156.7(4) . . . 2_656 ? O1 V4 N43 C46 169.0(7) . . . . ? N33 V4 N43 C46 84.3(7) . . . . ? N23 V4 N43 C46 160.3(11) . . . . ? N53 V4 N43 C46 -108.1(7) . . . . ? Cl3 V4 N43 C46 -12.2(7) . . . . ? O2 V3 N51 N52 -15.9(5) . . . . ? O4 V3 N51 N52 53(5) . . . . ? O6 V3 N51 N52 -108.0(5) . . . . ? N31 V3 N51 N52 68.2(5) . . . . ? Cl2 V3 N51 N52 161.0(4) . . . . ? O2 V3 N51 C51 143.6(7) . . . . ? O4 V3 N51 C51 -148(5) . . . . ? O6 V3 N51 C51 51.5(7) . . . . ? N31 V3 N51 C51 -132.3(7) . . . . ? Cl2 V3 N51 C51 -39.5(7) . . . . ? C51 N51 N52 N53 -2.8(8) . . . 2_656 ? V3 N51 N52 N53 163.1(4) . . . 2_656 ? C51 N51 N52 V1 179.5(5) . . . . ? V3 N51 N52 V1 -14.6(6) . . . . ? O1 V1 N52 N53 65.0(6) . . . 2_656 ? O1 V1 N52 N53 14.8(5) 2_656 . . 2_656 ? O2 V1 N52 N53 -142.6(6) . . . 2_656 ? N42 V1 N52 N53 -63.9(5) . . . 2_656 ? N32 V1 N52 N53 140.1(5) . . . 2_656 ? N22 V1 N52 N53 -144.7(5) . . . 2_656 ? O1 V1 N52 N51 -117.5(5) . . . . ? O1 V1 N52 N51 -167.8(5) 2_656 . . . ? O2 V1 N52 N51 34.8(5) . . . . ? N42 V1 N52 N51 113.6(5) . . . . ? N32 V1 N52 N51 -42.5(5) . . . . ? N22 V1 N52 N51 32.7(9) . . . . ? O1 V4 N53 N52 29.3(4) . . . 2_656 ? N33 V4 N53 N52 40.4(13) . . . 2_656 ? N43 V4 N53 N52 -55.1(5) . . . 2_656 ? N23 V4 N53 N52 114.7(5) . . . 2_656 ? Cl3 V4 N53 N52 -149.9(4) . . . 2_656 ? O1 V4 N53 C56 -162.9(8) . . . . ? N33 V4 N53 C56 -151.9(10) . . . . ? N43 V4 N53 C56 112.7(8) . . . . ? N23 V4 N53 C56 -77.5(8) . . . . ? Cl3 V4 N53 C56 17.8(8) . . . . ? V3 O4 C1 O3 -7.8(13) . . . . ? V3 O4 C1 C2 173.7(5) . . . . ? V2 O3 C1 O4 8.8(13) . . . . ? V2 O3 C1 C2 -172.6(5) . . . . ? O4 C1 C2 C3 177.9(8) . . . . ? O3 C1 C2 C3 -0.8(13) . . . . ? O4 C1 C2 C7 -2.5(12) . . . . ? O3 C1 C2 C7 178.8(8) . . . . ? C7 C2 C3 C4 1.3(15) . . . . ? C1 C2 C3 C4 -179.1(9) . . . . ? C2 C3 C4 C5 -2.6(16) . . . . ? C3 C4 C5 C6 2.3(18) . . . . ? C4 C5 C6 C7 -0.6(19) . . . . ? C5 C6 C7 C2 -0.8(17) . . . . ? C3 C2 C7 C6 0.5(15) . . . . ? C1 C2 C7 C6 -179.1(9) . . . . ? V3 O6 C8 O5 9.5(13) . . . . ? V3 O6 C8 C9 -171.0(5) . . . . ? V2 O5 C8 O6 -7.5(13) . . . . ? V2 O5 C8 C9 173.0(5) . . . . ? O6 C8 C9 C10 172.3(8) . . . . ? O5 C8 C9 C10 -8.2(12) . . . . ? O6 C8 C9 C14 -3.1(12) . . . . ? O5 C8 C9 C14 176.5(8) . . . . ? C14 C9 C10 C11 0.0(14) . . . . ? C8 C9 C10 C11 -175.4(9) . . . . ? C9 C10 C11 C12 -0.5(15) . . . . ? C10 C11 C12 C13 -1.3(15) . . . . ? C11 C12 C13 C14 3.8(16) . . . . ? C12 C13 C14 C9 -4.2(15) . . . . ? C10 C9 C14 C13 2.3(13) . . . . ? C8 C9 C14 C13 177.9(8) . . . . ? N22 N21 C21 C22 179.2(10) . . . . ? V2 N21 C21 C22 24.7(14) . . . . ? N22 N21 C21 C26 0.3(8) . . . . ? V2 N21 C21 C26 -154.2(6) . . . . ? N21 C21 C22 C23 -177.9(10) . . . . ? C26 C21 C22 C23 0.8(15) . . . . ? C21 C22 C23 C24 -1.5(18) . . . . ? C22 C23 C24 C25 1(2) . . . . ? C23 C24 C25 C26 -0.2(17) . . . . ? N22 N23 C26 C25 -179.1(8) . . . . ? V4 N23 C26 C25 -15.0(14) . . . . ? N22 N23 C26 C21 0.6(8) . . . . ? V4 N23 C26 C21 164.6(6) . . . . ? C24 C25 C26 N23 179.1(9) . . . . ? C24 C25 C26 C21 -0.5(13) . . . . ? N21 C21 C26 N23 -0.5(9) . . . . ? C22 C21 C26 N23 -179.5(8) . . . . ? N21 C21 C26 C25 179.2(7) . . . . ? C22 C21 C26 C25 0.2(13) . . . . ? N32 N31 C31 C32 -179.2(8) . . . . ? V3 N31 C31 C32 -23.7(12) . . . . ? N32 N31 C31 C36 0.1(8) . . . . ? V3 N31 C31 C36 155.6(5) . . . . ? N31 C31 C32 C33 -179.7(8) . . . . ? C36 C31 C32 C33 1.1(12) . . . . ? C31 C32 C33 C34 -1.1(13) . . . . ? C32 C33 C34 C35 0.7(14) . . . . ? C33 C34 C35 C36 -0.3(12) . . . . ? N32 N33 C36 C31 1.4(8) . . . . ? V4 N33 C36 C31 -162.6(6) . . . . ? N32 N33 C36 C35 -179.5(7) . . . . ? V4 N33 C36 C35 16.5(13) . . . . ? N31 C31 C36 N33 -1.0(8) . . . . ? C32 C31 C36 N33 178.4(7) . . . . ? N31 C31 C36 C35 179.8(7) . . . . ? C32 C31 C36 C35 -0.8(12) . . . . ? C34 C35 C36 N33 -178.7(8) . . . . ? C34 C35 C36 C31 0.3(11) . . . . ? N42 N41 C41 C42 179.6(8) . . . . ? V2 N41 C41 C42 -26.8(13) . . . . ? N42 N41 C41 C46 -1.3(8) . . . 2_656 ? V2 N41 C41 C46 152.4(5) . . . 2_656 ? N41 C41 C42 C43 179.0(8) . . . . ? C46 C41 C42 C43 0.0(12) 2_656 . . . ? C41 C42 C43 C44 -0.1(13) . . . 2_656 ? C43 C44 C45 C46 2.0(13) 2_656 . . . ? C44 C45 C46 N43 178.1(8) . . . . ? C44 C45 C46 C41 -1.8(12) . . . 2_656 ? N42 N43 C46 C45 178.6(8) 2_656 . . . ? V4 N43 C46 C45 -12.1(13) . . . . ? N42 N43 C46 C41 -1.5(8) 2_656 . . 2_656 ? V4 N43 C46 C41 167.8(6) . . . 2_656 ? N52 N51 C51 C52 -177.9(8) . . . . ? V3 N51 C51 C52 21.4(14) . . . . ? N52 N51 C51 C56 1.5(8) . . . 2_656 ? V3 N51 C51 C56 -159.2(6) . . . 2_656 ? N51 C51 C52 C53 177.3(9) . . . . ? C56 C51 C52 C53 -2.1(13) 2_656 . . . ? C51 C52 C53 C54 -0.7(15) . . . 2_656 ? C53 C54 C55 C56 2.3(13) 2_656 . . . ? N52 N53 C56 C55 -174.7(8) 2_656 . . . ? V4 N53 C56 C55 17.1(14) . . . . ? N52 N53 C56 C51 1.8(8) 2_656 . . 2_656 ? V4 N53 C56 C51 -166.3(6) . . . 2_656 ? C54 C55 C56 N53 176.6(8) . . . . ? C54 C55 C56 C51 0.5(12) . . . 2_656 ? C60Y N60 C60X C61X 57(4) . . . . ? C64 N60 C60X C61X -42(7) . . . . ? C72X N60 C60X C61X -159(6) . . . . ? C68 N60 C60X C61X 92(7) . . . . ? C72Y N60 C60X C61X -139(8) . . . . ? N60 C60X C61X C62X -169(5) . . . . ? C60X C61X C62X C63 -86(7) . . . . ? C60X N60 C60Y C61Y -20(5) . . . . ? C64 N60 C60Y C61Y 66.9(17) . . . . ? C72X N60 C60Y C61Y -63.0(19) . . . . ? C68 N60 C60Y C61Y -172.6(14) . . . . ? C72Y N60 C60Y C61Y -35(2) . . . . ? N60 C60Y C61Y C62Y -176.3(14) . . . . ? C60Y C61Y C62Y C63 162.4(16) . . . . ? C61Y C62Y C63 C62X -106(5) . . . . ? C61X C62X C63 C62Y 79(4) . . . . ? C60Y N60 C64 C65Y 26(8) . . . . ? C60X N60 C64 C65Y 54(8) . . . . ? C72X N60 C64 C65Y 162(7) . . . . ? C68 N60 C64 C65Y -88(8) . . . . ? C72Y N60 C64 C65Y 126(8) . . . . ? C60Y N60 C64 C65X 49.9(17) . . . . ? C60X N60 C64 C65X 78(3) . . . . ? C72X N60 C64 C65X -174.1(15) . . . . ? C68 N60 C64 C65X -65.0(17) . . . . ? C72Y N60 C64 C65X 149(2) . . . . ? C65Y C64 C65X C66X -28(3) . . . . ? N60 C64 C65X C66X 164.0(14) . . . . ? C64 C65X C66X C67X 56(2) . . . . ? N60 C64 C65Y C66Y 162(5) . . . . ? C65X C64 C65Y C66Y 132(11) . . . . ? C64 C65Y C66Y C67Y 174(7) . . . . ? C60Y N60 C68 C69 -173.1(16) . . . . ? C60X N60 C68 C69 171(2) . . . . ? C64 N60 C68 C69 -59.3(19) . . . . ? C72X N60 C68 C69 59.4(18) . . . . ? C72Y N60 C68 C69 72(3) . . . . ? N60 C68 C69 C70 -174.6(13) . . . . ? C68 C69 C70 C71 64(2) . . . . ? C60Y N60 C72X C73X -51(2) . . . . ? C60X N60 C72X C73X -70(4) . . . . ? C64 N60 C72X C73X -176.9(16) . . . . ? C68 N60 C72X C73X 63.4(19) . . . . ? C72Y N60 C72X C73X -101(3) . . . . ? N60 C72X C73X C74X -173.6(14) . . . . ? C72X C73X C74X C75 -65(2) . . . . ? C60Y N60 C72Y C73Y -59(4) . . . . ? C60X N60 C72Y C73Y -67(5) . . . . ? C64 N60 C72Y C73Y -165(4) . . . . ? C72X N60 C72Y C73Y 81(4) . . . . ? C68 N60 C72Y C73Y 59(5) . . . . ? N60 C72Y C73Y C74Y -155(3) . . . . ? C72Y C73Y C74Y C75 66(5) . . . . ? C73Y C74Y C75 C74X 30(3) . . . . ? C73X C74X C75 C74Y -24.4(19) . . . . ? C4S O1S C1S C2S -22.8(19) . . . . ? O1S C1S C2S C3S 12(2) . . . . ? C1S C2S C3S C4S 4(2) . . . . ? C2S C3S C4S O1S -17.8(19) . . . . ? C1S O1S C4S C3S 24.4(18) . . . . ? C8S C7S C6S C5S 15(2) . . . . ? C7S C6S C5S O2S -24.4(19) . . . . ? C6S C5S O2S C8S 26.3(19) . . . . ? C5S O2S C8S C7S -15.5(18) . . . . ? C6S C7S C8S O2S 0.0(18) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.612 _refine_diff_density_min -1.223 _refine_diff_density_rms 0.154