# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2008 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Mike Ward' 'W Clegg' 'M Hardie' 'Luca Russo' 'Brian F. Taylor' 'Ian S Tidmarsh' _publ_contact_author_name 'Mike Ward' _publ_contact_author_email M.D.WARD@SHEFFIELD.AC.UK _publ_section_title ; Further investigations into tetrahedral M4L6 cage complexes containing guest anions: new structures and NMR spectroscopic studies. ; # Attachment 'B816864D_crystaldata.cif' data_imw1045p-1 _database_code_depnum_ccdc_archive 'CCDC 708981' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 N6' _chemical_formula_weight 492.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.7446(9) _cell_length_b 11.5028(11) _cell_length_c 11.7836(11) _cell_angle_alpha 98.106(6) _cell_angle_beta 98.719(6) _cell_angle_gamma 100.454(6) _cell_volume 1264.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6284 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.43 _exptl_crystal_description Prismatic _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9766 _exptl_absorpt_correction_T_max 0.9921 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20069 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5148 _reflns_number_gt 4085 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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 processing was carried out to 0.8 angstroms as the data was only complete to this resolution. Hydrogen atoms were included in calculated positions. 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^)+(0.0442P)^2^+0.3739P] 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 5148 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 N11 N 0.45386(13) 0.22504(11) 0.98104(10) 0.0287(3) Uani 1 1 d . . . C12 C 0.39431(14) 0.31510(13) 0.94938(11) 0.0236(3) Uani 1 1 d . . . C13 C 0.27946(16) 0.34763(14) 0.99394(12) 0.0283(3) Uani 1 1 d . . . H13 H 0.2407 0.4123 0.9703 0.034 Uiso 1 1 calc R . . C14 C 0.22293(17) 0.28389(15) 1.07328(12) 0.0337(4) Uani 1 1 d . . . H14 H 0.1441 0.3037 1.1044 0.040 Uiso 1 1 calc R . . C15 C 0.28289(17) 0.19093(14) 1.10652(12) 0.0332(4) Uani 1 1 d . . . H15 H 0.2460 0.1454 1.1605 0.040 Uiso 1 1 calc R . . C16 C 0.39810(17) 0.16597(14) 1.05915(12) 0.0319(3) Uani 1 1 d . . . H16 H 0.4402 0.1032 1.0835 0.038 Uiso 1 1 calc R . . N21 N 0.48282(12) 0.50479(10) 0.74754(9) 0.0220(3) Uani 1 1 d . . . N22 N 0.39697(12) 0.46320(10) 0.81945(9) 0.0234(3) Uani 1 1 d . . . C23 C 0.45805(14) 0.37995(12) 0.86401(11) 0.0226(3) Uani 1 1 d . . . C24 C 0.58239(15) 0.36887(13) 0.82070(12) 0.0265(3) Uani 1 1 d . . . H24 H 0.6442 0.3163 0.8387 0.032 Uiso 1 1 calc R . . C25 C 0.59491(15) 0.45046(13) 0.74687(12) 0.0258(3) Uani 1 1 d . . . H25 H 0.6686 0.4661 0.7033 0.031 Uiso 1 1 calc R . . C26 C 0.45174(15) 0.60167(12) 0.68748(11) 0.0246(3) Uani 1 1 d . . . H26A H 0.5374 0.6369 0.6585 0.029 Uiso 1 1 calc R . . H26B H 0.4307 0.6652 0.7441 0.029 Uiso 1 1 calc R . . C31 C 0.28064(14) 0.44592(12) 0.53319(11) 0.0211(3) Uani 1 1 d . . . H31 H 0.3258 0.3866 0.5619 0.025 Uiso 1 1 calc R . . C32 C 0.32771(14) 0.56320(12) 0.58545(11) 0.0209(3) Uani 1 1 d . . . C33 C 0.25965(14) 0.65452(12) 0.54346(11) 0.0212(3) Uani 1 1 d . . . C34 C 0.14877(14) 0.62216(12) 0.45124(11) 0.0217(3) Uani 1 1 d . . . H34 H 0.1045 0.6828 0.4243 0.026 Uiso 1 1 calc R . . C35 C 0.09712(14) 0.50076(12) 0.39396(11) 0.0201(3) Uani 1 1 d . . . C36 C 0.16475(14) 0.40966(12) 0.43602(11) 0.0201(3) Uani 1 1 d . . . C41 C -0.17687(15) 0.31262(13) 0.14372(11) 0.0253(3) Uani 1 1 d . . . H41 H -0.2233 0.3713 0.1151 0.030 Uiso 1 1 calc R . . C42 C -0.21913(15) 0.19559(14) 0.09073(12) 0.0280(3) Uani 1 1 d . . . H42 H -0.2943 0.1736 0.0253 0.034 Uiso 1 1 calc R . . C43 C -0.15206(16) 0.10588(14) 0.13225(12) 0.0290(3) Uani 1 1 d . . . H43 H -0.1823 0.0247 0.0941 0.035 Uiso 1 1 calc R . . C44 C -0.04437(15) 0.13588(13) 0.22673(12) 0.0257(3) Uani 1 1 d . . . H44 H -0.0011 0.0749 0.2541 0.031 Uiso 1 1 calc R . . C45 C 0.00420(14) 0.25712(12) 0.28491(11) 0.0214(3) Uani 1 1 d . . . C46 C -0.06277(14) 0.34827(12) 0.24253(11) 0.0215(3) Uani 1 1 d . . . C51 C 0.11690(14) 0.29027(12) 0.38100(11) 0.0211(3) Uani 1 1 d . . . H51 H 0.1612 0.2302 0.4089 0.025 Uiso 1 1 calc R . . C52 C -0.01502(14) 0.46777(12) 0.29816(11) 0.0217(3) Uani 1 1 d . . . H52 H -0.0595 0.5279 0.2705 0.026 Uiso 1 1 calc R . . N61 N 0.88496(12) 1.04853(10) 0.58404(10) 0.0254(3) Uani 1 1 d . . . C62 C 0.78321(15) 1.03415(12) 0.64930(11) 0.0233(3) Uani 1 1 d . . . C63 C 0.80096(16) 1.09647(13) 0.76314(12) 0.0285(3) Uani 1 1 d . . . H63 H 0.7264 1.0858 0.8065 0.034 Uiso 1 1 calc R . . C64 C 0.92948(16) 1.17417(14) 0.81162(13) 0.0331(4) Uani 1 1 d . . . H64 H 0.9446 1.2169 0.8891 0.040 Uiso 1 1 calc R . . C65 C 1.03540(16) 1.18851(13) 0.74540(13) 0.0308(3) Uani 1 1 d . . . H65 H 1.1245 1.2409 0.7764 0.037 Uiso 1 1 calc R . . C66 C 1.00807(15) 1.12442(13) 0.63266(12) 0.0272(3) Uani 1 1 d . . . H66 H 1.0807 1.1349 0.5873 0.033 Uiso 1 1 calc R . . N71 N 0.44781(12) 0.83441(10) 0.57079(9) 0.0218(3) Uani 1 1 d . . . N72 N 0.54904(12) 0.91260(10) 0.65160(9) 0.0229(3) Uani 1 1 d . . . C73 C 0.65181(14) 0.94729(12) 0.59240(11) 0.0219(3) Uani 1 1 d . . . C74 C 0.61623(15) 0.89162(12) 0.47440(11) 0.0235(3) Uani 1 1 d . . . H74 H 0.6715 0.9012 0.4152 0.028 Uiso 1 1 calc R . . C75 C 0.48466(15) 0.82088(12) 0.46404(11) 0.0237(3) Uani 1 1 d . . . H75 H 0.4293 0.7714 0.3949 0.028 Uiso 1 1 calc R . . C76 C 0.30993(14) 0.78501(12) 0.59908(12) 0.0234(3) Uani 1 1 d . . . H76A H 0.2394 0.8313 0.5709 0.028 Uiso 1 1 calc R . . H76B H 0.3183 0.7927 0.6847 0.028 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 N11 0.0288(7) 0.0309(7) 0.0245(6) 0.0071(5) 0.0009(5) 0.0032(5) C12 0.0224(7) 0.0279(7) 0.0166(6) 0.0019(5) -0.0009(5) 0.0000(6) C13 0.0288(8) 0.0337(8) 0.0222(7) 0.0062(6) 0.0036(6) 0.0054(6) C14 0.0287(8) 0.0464(10) 0.0251(7) 0.0070(7) 0.0076(6) 0.0026(7) C15 0.0337(9) 0.0385(9) 0.0229(7) 0.0095(6) 0.0029(6) -0.0050(7) C16 0.0333(8) 0.0325(8) 0.0269(7) 0.0096(6) -0.0008(6) 0.0007(7) N21 0.0212(6) 0.0257(6) 0.0186(5) 0.0043(5) 0.0039(4) 0.0032(5) N22 0.0219(6) 0.0292(6) 0.0189(5) 0.0050(5) 0.0042(4) 0.0035(5) C23 0.0225(7) 0.0254(7) 0.0175(6) 0.0013(5) 0.0006(5) 0.0031(6) C24 0.0268(8) 0.0297(8) 0.0253(7) 0.0059(6) 0.0061(6) 0.0096(6) C25 0.0226(7) 0.0319(8) 0.0243(7) 0.0039(6) 0.0081(6) 0.0067(6) C26 0.0257(7) 0.0245(7) 0.0226(7) 0.0057(6) 0.0026(6) 0.0033(6) C31 0.0216(7) 0.0233(7) 0.0207(6) 0.0071(5) 0.0060(5) 0.0065(6) C32 0.0203(7) 0.0256(7) 0.0186(6) 0.0061(5) 0.0074(5) 0.0043(6) C33 0.0218(7) 0.0227(7) 0.0214(6) 0.0060(5) 0.0097(5) 0.0040(6) C34 0.0227(7) 0.0226(7) 0.0235(7) 0.0084(5) 0.0086(5) 0.0070(6) C35 0.0193(7) 0.0241(7) 0.0200(6) 0.0073(5) 0.0087(5) 0.0050(6) C36 0.0202(7) 0.0237(7) 0.0190(6) 0.0067(5) 0.0078(5) 0.0053(6) C41 0.0237(7) 0.0319(8) 0.0222(7) 0.0070(6) 0.0053(6) 0.0078(6) C42 0.0237(7) 0.0382(9) 0.0206(7) 0.0026(6) 0.0025(6) 0.0058(6) C43 0.0293(8) 0.0286(8) 0.0267(7) -0.0012(6) 0.0054(6) 0.0042(6) C44 0.0262(7) 0.0262(7) 0.0264(7) 0.0051(6) 0.0067(6) 0.0080(6) C45 0.0202(7) 0.0255(7) 0.0204(6) 0.0052(5) 0.0081(5) 0.0050(6) C46 0.0192(7) 0.0279(7) 0.0192(6) 0.0059(5) 0.0076(5) 0.0049(6) C51 0.0214(7) 0.0222(7) 0.0227(6) 0.0073(5) 0.0067(5) 0.0073(6) C52 0.0215(7) 0.0256(7) 0.0214(6) 0.0083(5) 0.0071(5) 0.0075(6) N61 0.0234(6) 0.0268(6) 0.0267(6) 0.0068(5) 0.0041(5) 0.0058(5) C62 0.0244(7) 0.0228(7) 0.0244(7) 0.0074(5) 0.0037(6) 0.0075(6) C63 0.0279(8) 0.0305(8) 0.0266(7) 0.0029(6) 0.0059(6) 0.0053(6) C64 0.0343(9) 0.0329(9) 0.0279(8) -0.0012(6) 0.0022(6) 0.0044(7) C65 0.0272(8) 0.0275(8) 0.0342(8) 0.0051(6) -0.0008(6) 0.0027(6) C66 0.0235(7) 0.0284(8) 0.0313(7) 0.0093(6) 0.0059(6) 0.0054(6) N71 0.0235(6) 0.0202(6) 0.0214(6) 0.0039(4) 0.0043(5) 0.0033(5) N72 0.0250(6) 0.0209(6) 0.0222(6) 0.0042(5) 0.0028(5) 0.0045(5) C73 0.0229(7) 0.0210(7) 0.0239(7) 0.0065(5) 0.0050(5) 0.0076(6) C74 0.0246(7) 0.0251(7) 0.0224(7) 0.0054(5) 0.0063(5) 0.0065(6) C75 0.0268(7) 0.0243(7) 0.0205(6) 0.0028(5) 0.0048(5) 0.0068(6) C76 0.0238(7) 0.0241(7) 0.0240(7) 0.0057(5) 0.0073(6) 0.0055(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N11 C16 1.3409(19) . ? N11 C12 1.3457(18) . ? C12 C13 1.394(2) . ? C12 C23 1.4788(19) . ? C13 C14 1.385(2) . ? C13 H13 0.9500 . ? C14 C15 1.383(2) . ? C14 H14 0.9500 . ? C15 C16 1.384(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 N22 1.3530(15) . ? N21 C25 1.3537(18) . ? N21 C26 1.4542(17) . ? N22 C23 1.3420(17) . ? C23 C24 1.4035(19) . ? C24 C25 1.369(2) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C32 1.5222(18) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C32 1.3657(19) . ? C31 C36 1.4362(18) . ? C31 H31 0.9500 . ? C32 C33 1.4450(18) . ? C33 C34 1.3678(19) . ? C33 C76 1.5102(19) . ? C34 C35 1.4266(19) . ? C34 H34 0.9500 . ? C35 C52 1.4026(18) . ? C35 C36 1.4409(18) . ? C36 C51 1.3959(19) . ? C41 C42 1.362(2) . ? C41 C46 1.4379(18) . ? C41 H41 0.9500 . ? C42 C43 1.422(2) . ? C42 H42 0.9500 . ? C43 C44 1.366(2) . ? C43 H43 0.9500 . ? C44 C45 1.425(2) . ? C44 H44 0.9500 . ? C45 C51 1.4082(18) . ? C45 C46 1.4393(18) . ? C46 C52 1.3989(19) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? N61 C66 1.3416(18) . ? N61 C62 1.3452(18) . ? C62 C63 1.399(2) . ? C62 C73 1.4745(19) . ? C63 C64 1.388(2) . ? C63 H63 0.9500 . ? C64 C65 1.386(2) . ? C64 H64 0.9500 . ? C65 C66 1.387(2) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? N71 C75 1.3555(17) . ? N71 N72 1.3567(16) . ? N71 C76 1.4667(17) . ? N72 C73 1.3394(18) . ? C73 C74 1.4091(19) . ? C74 C75 1.366(2) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 N11 C12 117.08(13) . . ? N11 C12 C13 122.82(13) . . ? N11 C12 C23 116.32(12) . . ? C13 C12 C23 120.86(13) . . ? C14 C13 C12 118.77(14) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C15 C14 C13 119.05(15) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 118.28(13) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? N11 C16 C15 123.98(14) . . ? N11 C16 H16 118.0 . . ? C15 C16 H16 118.0 . . ? N22 N21 C25 112.09(11) . . ? N22 N21 C26 119.48(11) . . ? C25 N21 C26 128.34(12) . . ? C23 N22 N21 104.39(11) . . ? N22 C23 C24 111.48(12) . . ? N22 C23 C12 120.10(12) . . ? C24 C23 C12 128.42(12) . . ? C25 C24 C23 104.77(12) . . ? C25 C24 H24 127.6 . . ? C23 C24 H24 127.6 . . ? N21 C25 C24 107.26(12) . . ? N21 C25 H25 126.4 . . ? C24 C25 H25 126.4 . . ? N21 C26 C32 114.10(11) . . ? N21 C26 H26A 108.7 . . ? C32 C26 H26A 108.7 . . ? N21 C26 H26B 108.7 . . ? C32 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C32 C31 C36 121.88(12) . . ? C32 C31 H31 119.1 . . ? C36 C31 H31 119.1 . . ? C31 C32 C33 119.85(12) . . ? C31 C32 C26 121.80(12) . . ? C33 C32 C26 118.35(12) . . ? C34 C33 C32 119.36(12) . . ? C34 C33 C76 119.60(12) . . ? C32 C33 C76 121.03(12) . . ? C33 C34 C35 122.43(12) . . ? C33 C34 H34 118.8 . . ? C35 C34 H34 118.8 . . ? C52 C35 C34 122.46(12) . . ? C52 C35 C36 119.32(12) . . ? C34 C35 C36 118.21(12) . . ? C51 C36 C31 122.37(12) . . ? C51 C36 C35 119.36(12) . . ? C31 C36 C35 118.27(12) . . ? C42 C41 C46 120.69(13) . . ? C42 C41 H41 119.7 . . ? C46 C41 H41 119.7 . . ? C41 C42 C43 120.79(13) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C44 C43 C42 120.31(14) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 121.07(13) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C51 C45 C44 121.95(12) . . ? C51 C45 C46 119.29(12) . . ? C44 C45 C46 118.75(12) . . ? C52 C46 C41 122.34(12) . . ? C52 C46 C45 119.27(12) . . ? C41 C46 C45 118.39(12) . . ? C36 C51 C45 121.32(12) . . ? C36 C51 H51 119.3 . . ? C45 C51 H51 119.3 . . ? C46 C52 C35 121.44(12) . . ? C46 C52 H52 119.3 . . ? C35 C52 H52 119.3 . . ? C66 N61 C62 117.57(12) . . ? N61 C62 C63 122.49(13) . . ? N61 C62 C73 115.13(12) . . ? C63 C62 C73 122.38(13) . . ? C64 C63 C62 118.83(14) . . ? C64 C63 H63 120.6 . . ? C62 C63 H63 120.6 . . ? C65 C64 C63 119.03(14) . . ? C65 C64 H64 120.5 . . ? C63 C64 H64 120.5 . . ? C64 C65 C66 118.33(14) . . ? C64 C65 H65 120.8 . . ? C66 C65 H65 120.8 . . ? N61 C66 C65 123.74(14) . . ? N61 C66 H66 118.1 . . ? C65 C66 H66 118.1 . . ? C75 N71 N72 112.29(11) . . ? C75 N71 C76 126.48(11) . . ? N72 N71 C76 120.83(11) . . ? C73 N72 N71 104.08(10) . . ? N72 C73 C74 111.72(12) . . ? N72 C73 C62 121.54(12) . . ? C74 C73 C62 126.74(12) . . ? C75 C74 C73 104.68(12) . . ? C75 C74 H74 127.7 . . ? C73 C74 H74 127.7 . . ? N71 C75 C74 107.22(12) . . ? N71 C75 H75 126.4 . . ? C74 C75 H75 126.4 . . ? N71 C76 C33 110.77(11) . . ? N71 C76 H76A 109.5 . . ? C33 C76 H76A 109.5 . . ? N71 C76 H76B 109.5 . . ? C33 C76 H76B 109.5 . . ? H76A C76 H76B 108.1 . . ? 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 C16 N11 C12 C13 -0.1(2) . . . . ? C16 N11 C12 C23 179.45(12) . . . . ? N11 C12 C13 C14 -0.7(2) . . . . ? C23 C12 C13 C14 179.70(13) . . . . ? C12 C13 C14 C15 0.6(2) . . . . ? C13 C14 C15 C16 0.4(2) . . . . ? C12 N11 C16 C15 1.2(2) . . . . ? C14 C15 C16 N11 -1.3(2) . . . . ? C25 N21 N22 C23 -0.34(14) . . . . ? C26 N21 N22 C23 -177.21(11) . . . . ? N21 N22 C23 C24 0.11(15) . . . . ? N21 N22 C23 C12 179.01(11) . . . . ? N11 C12 C23 N22 173.66(12) . . . . ? C13 C12 C23 N22 -6.7(2) . . . . ? N11 C12 C23 C24 -7.6(2) . . . . ? C13 C12 C23 C24 171.97(14) . . . . ? N22 C23 C24 C25 0.15(16) . . . . ? C12 C23 C24 C25 -178.64(13) . . . . ? N22 N21 C25 C24 0.45(16) . . . . ? C26 N21 C25 C24 176.97(13) . . . . ? C23 C24 C25 N21 -0.35(15) . . . . ? N22 N21 C26 C32 -75.12(15) . . . . ? C25 N21 C26 C32 108.58(15) . . . . ? C36 C31 C32 C33 0.42(19) . . . . ? C36 C31 C32 C26 -179.24(12) . . . . ? N21 C26 C32 C31 -19.47(18) . . . . ? N21 C26 C32 C33 160.87(11) . . . . ? C31 C32 C33 C34 -0.22(19) . . . . ? C26 C32 C33 C34 179.45(12) . . . . ? C31 C32 C33 C76 -179.65(12) . . . . ? C26 C32 C33 C76 0.02(18) . . . . ? C32 C33 C34 C35 -0.14(19) . . . . ? C76 C33 C34 C35 179.29(11) . . . . ? C33 C34 C35 C52 -178.91(12) . . . . ? C33 C34 C35 C36 0.30(19) . . . . ? C32 C31 C36 C51 179.18(12) . . . . ? C32 C31 C36 C35 -0.26(19) . . . . ? C52 C35 C36 C51 -0.32(18) . . . . ? C34 C35 C36 C51 -179.56(12) . . . . ? C52 C35 C36 C31 179.13(11) . . . . ? C34 C35 C36 C31 -0.11(17) . . . . ? C46 C41 C42 C43 0.4(2) . . . . ? C41 C42 C43 C44 0.4(2) . . . . ? C42 C43 C44 C45 -0.7(2) . . . . ? C43 C44 C45 C51 -178.72(13) . . . . ? C43 C44 C45 C46 0.2(2) . . . . ? C42 C41 C46 C52 179.04(13) . . . . ? C42 C41 C46 C45 -0.84(19) . . . . ? C51 C45 C46 C52 -0.38(18) . . . . ? C44 C45 C46 C52 -179.34(12) . . . . ? C51 C45 C46 C41 179.50(12) . . . . ? C44 C45 C46 C41 0.55(18) . . . . ? C31 C36 C51 C45 -179.18(12) . . . . ? C35 C36 C51 C45 0.25(19) . . . . ? C44 C45 C51 C36 179.02(12) . . . . ? C46 C45 C51 C36 0.10(19) . . . . ? C41 C46 C52 C35 -179.56(12) . . . . ? C45 C46 C52 C35 0.32(19) . . . . ? C34 C35 C52 C46 179.24(12) . . . . ? C36 C35 C52 C46 0.03(19) . . . . ? C66 N61 C62 C63 1.20(19) . . . . ? C66 N61 C62 C73 -178.43(11) . . . . ? N61 C62 C63 C64 -1.4(2) . . . . ? C73 C62 C63 C64 178.17(13) . . . . ? C62 C63 C64 C65 0.7(2) . . . . ? C63 C64 C65 C66 0.2(2) . . . . ? C62 N61 C66 C65 -0.3(2) . . . . ? C64 C65 C66 N61 -0.4(2) . . . . ? C75 N71 N72 C73 -0.51(14) . . . . ? C76 N71 N72 C73 -173.77(11) . . . . ? N71 N72 C73 C74 0.07(14) . . . . ? N71 N72 C73 C62 179.74(11) . . . . ? N61 C62 C73 N72 171.38(12) . . . . ? C63 C62 C73 N72 -8.3(2) . . . . ? N61 C62 C73 C74 -9.00(19) . . . . ? C63 C62 C73 C74 171.37(13) . . . . ? N72 C73 C74 C75 0.37(15) . . . . ? C62 C73 C74 C75 -179.28(12) . . . . ? N72 N71 C75 C74 0.76(15) . . . . ? C76 N71 C75 C74 173.56(12) . . . . ? C73 C74 C75 N71 -0.65(14) . . . . ? C75 N71 C76 C33 46.50(17) . . . . ? N72 N71 C76 C33 -141.26(11) . . . . ? C34 C33 C76 N71 -108.26(14) . . . . ? C32 C33 C76 N71 71.17(15) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.320 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.040 #===END data_mjh_shef2_0m _database_code_depnum_ccdc_archive 'CCDC 708982' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C192 H144 B8 F32 N36 Zn4' _chemical_formula_weight 3911.39 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 19.8865(6) _cell_length_b 19.8865(6) _cell_length_c 48.236(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 16520.2(13) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 888 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 21.01 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5988 _exptl_absorpt_coefficient_mu 0.511 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9319 _exptl_absorpt_correction_T_max 0.9749 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55589 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4820 _reflns_number_gt 3137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. Hydrogen atoms were included in calculated positions. The data was used to a resolution of 45 degrees 2-theta as the intensity of the data dropped rapidly after this point. The structure is of a [Zn4L6][BF4]8 host-guest cage. The structure manifests as a superimposition of both possible enantiomers and therefore suffers severe disorder. The pyridyl-pyrazole residues have been modelled to account for this and so appear as component 1: N11X > C16X N12X C1X C2X C2'X N1X, component 2: N11Y > C16Y N1Y C2Y C2'Y C1Y; and component 1: N21X > C26X N13X C3X C4X C4'X NX3, component 2: N21Y > C26Y N13Y N3Y C4Y C4'Y C3Y. The residues beginning N11X and N11Y were best resolved and were used as a model to which the residues beginning N21X and N21Y were restrained. All the five and six-membered rings in the structure have been constrained to be ideal. The model benefited from the application of displacement restraints to the thermal parameters of all the atoms involved in the disordered groups. Of the eight BF4 counter-ions required to quench the charge of the cationic cage only four could be found from the data. The four unfound counter-ions are assumed to be highly disordered and we were therefore unable to satisfactory model the associated electron density. The BF4 ions found from the data have been constrained to be ideal. Displacement restrains have been applied to all constituent BF4 atoms' isotropic and anisotropic thermal parameters. The BF4 anions display greater than average isotropic and anisotropic thermal parameters. Attempts to split these anions were unsuccessful leading to an unstable refinement. A 'SQUEEZE' function has been used to eliminate a number of voids containing several highly disordered counter-ions and solvent molecules. loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 89 46 ' ' 2 0.000 0.000 0.246 112 54 ' ' 3 0.000 0.000 0.754 112 62 ' ' 4 0.167 0.333 0.333 88 46 ' ' 5 0.167 0.833 0.333 88 46 ' ' 6 0.333 0.667 0.420 112 62 ' ' 7 0.333 0.667 0.913 111 54 ' ' 8 0.333 0.167 0.667 88 46 ' ' 9 0.500 1.000 0.000 89 46 ' ' 10 0.500 0.500 1.000 89 46 ' ' 11 0.667 0.333 0.087 111 61 ' ' 12 0.667 0.333 0.580 112 55 ' ' 13 0.667 0.833 0.333 88 46 ' ' 14 0.833 0.667 0.667 88 46 ' ' 15 0.833 0.167 0.667 88 46 ' ' _platon_squeeze_details ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4820 _refine_ls_number_parameters 268 _refine_ls_number_restraints 178 _refine_ls_R_factor_all 0.2118 _refine_ls_R_factor_gt 0.1872 _refine_ls_wR_factor_ref 0.5105 _refine_ls_wR_factor_gt 0.4858 _refine_ls_goodness_of_fit_ref 2.161 _refine_ls_restrained_S_all 2.524 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.56077(15) 0.57710(13) 0.12462(4) 0.0657(11) Uani 0.50 1 d P . 1 N11X N 0.6415(6) 0.6521(6) 0.0939(2) 0.082(5) Uiso 0.50 1 d PGD . 1 C12X C 0.6113(4) 0.6789(6) 0.0734(2) 0.066(5) Uiso 0.50 1 d PGDU . 1 C13X C 0.6602(6) 0.7311(7) 0.0536(2) 0.063(5) Uiso 0.50 1 d PGDU . 1 H13X H 0.6395 0.7494 0.0396 0.075 Uiso 0.50 1 calc PR . 1 C14X C 0.7392(6) 0.7567(7) 0.0541(2) 0.073(6) Uiso 0.50 1 d PGDU . 1 H14X H 0.7726 0.7924 0.0406 0.088 Uiso 0.50 1 calc PR . 1 C15X C 0.7694(4) 0.7299(8) 0.0746(3) 0.077(6) Uiso 0.50 1 d PGDU . 1 H15X H 0.8235 0.7474 0.0749 0.092 Uiso 0.50 1 calc PR . 1 C16X C 0.7206(7) 0.6777(8) 0.0944(3) 0.081(6) Uiso 0.50 1 d PGDU . 1 H16X H 0.7412 0.6594 0.1084 0.098 Uiso 0.50 1 calc PR . 1 N12X N 0.4062(7) 0.5804(12) 0.0918(4) 0.096(11) Uiso 0.50 1 d PGDU . 1 C1X C 0.4002(5) 0.6129(12) 0.0663(4) 0.086(10) Uiso 0.50 1 d PGDU . 1 H1X H 0.3537 0.6066 0.0584 0.104 Uiso 0.50 1 calc PR . 1 C2X C 0.4759(8) 0.6565(10) 0.0549(3) 0.048(6) Uiso 0.50 1 d PGDU . 1 H2X H 0.4889 0.6845 0.0379 0.057 Uiso 0.50 1 calc PR . 1 C2'X C 0.5287(5) 0.6509(11) 0.0733(3) 0.062(8) Uiso 0.50 1 d PGDU . 1 N1X N 0.4856(9) 0.6039(10) 0.0960(3) 0.064(6) Uiso 0.50 1 d PGDU . 1 N21X N 0.6451(7) 0.5650(7) 0.1502(2) 0.080(5) Uiso 0.50 1 d PGD . 1 C22X C 0.6837(7) 0.6226(6) 0.1700(3) 0.074(6) Uiso 0.50 1 d PGDU . 1 C23X C 0.7375(8) 0.6194(7) 0.1875(3) 0.108(8) Uiso 0.50 1 d PGDU . 1 H23X H 0.7639 0.6587 0.2010 0.129 Uiso 0.50 1 calc PR . 1 C24X C 0.7528(8) 0.5586(9) 0.1852(3) 0.086(6) Uiso 0.50 1 d PGDU . 1 H24X H 0.7896 0.5564 0.1972 0.103 Uiso 0.50 1 calc PR . 1 C25X C 0.7142(9) 0.5010(7) 0.1654(3) 0.108(8) Uiso 0.50 1 d PGDU . 1 H25X H 0.7246 0.4595 0.1639 0.130 Uiso 0.50 1 calc PR . 1 C26X C 0.6604(9) 0.5042(7) 0.1479(3) 0.101(8) Uiso 0.50 1 d PGDU . 1 H26X H 0.6340 0.4649 0.1344 0.121 Uiso 0.50 1 calc PR . 1 N13X N 0.6038(7) 0.7517(8) 0.1576(2) 0.045(6) Uiso 0.50 1 d PGDU . 1 C3X C 0.6585(9) 0.7944(7) 0.1787(3) 0.099(9) Uiso 0.50 1 d PGDU . 1 H3X H 0.6692 0.8431 0.1860 0.119 Uiso 0.50 1 calc PR . 1 C4X C 0.6945(6) 0.7513(8) 0.1870(2) 0.077(6) Uiso 0.50 1 d PGDU . 1 H4X H 0.7335 0.7662 0.2008 0.092 Uiso 0.50 1 calc PR . 1 C4'X C 0.6619(9) 0.6821(8) 0.1710(3) 0.073(6) Uiso 0.50 1 d PGDU . 1 N3X N 0.6059(7) 0.6824(7) 0.1529(2) 0.069(5) Uiso 0.50 1 d PGDU . 1 Zn2 Zn 0.3333(16) 0.667(4) 0.04433(8) 0.0576(13) Uani 0.50 3 d SPG . 2 N11Y N 0.4407(5) 0.7284(6) 0.0219(2) 0.059(4) Uiso 0.50 1 d PGD . 2 C12Y C 0.5025(7) 0.7230(5) 0.03277(18) 0.067(5) Uiso 0.50 1 d PGDU . 2 C13Y C 0.5764(6) 0.7673(7) 0.0216(2) 0.073(6) Uiso 0.50 1 d PGDU . 2 H13Y H 0.6186 0.7636 0.0291 0.088 Uiso 0.50 1 calc PR . 2 C14Y C 0.5885(6) 0.8171(7) -0.0004(3) 0.084(6) Uiso 0.50 1 d PGDU . 2 H14Y H 0.6390 0.8475 -0.0081 0.101 Uiso 0.50 1 calc PR . 2 C15Y C 0.5267(8) 0.8226(7) -0.0113(2) 0.097(7) Uiso 0.50 1 d PGDU . 2 H15Y H 0.5350 0.8566 -0.0264 0.117 Uiso 0.50 1 calc PR . 2 C16Y C 0.4528(7) 0.7783(8) -0.0002(2) 0.086(7) Uiso 0.50 1 d PGDU . 2 H16Y H 0.4106 0.7820 -0.0076 0.103 Uiso 0.50 1 calc PR . 2 N12Y N 0.4097(7) 0.5853(8) 0.0890(3) 0.038(6) Uiso 0.50 1 d PGDU . 2 N1Y N 0.4133(7) 0.6347(9) 0.0671(3) 0.055(5) Uiso 0.50 1 d PGDU . 2 C2Y C 0.4891(9) 0.6702(10) 0.0556(3) 0.072(9) Uiso 0.50 1 d PGDU . 2 C2'Y C 0.5324(6) 0.6428(11) 0.0703(4) 0.071(9) Uiso 0.50 1 d PGDU . 2 H2'Y H 0.5850 0.6570 0.0670 0.085 Uiso 0.50 1 calc PR . 2 C1Y C 0.4834(8) 0.5904(10) 0.0910(3) 0.087(10) Uiso 0.50 1 d PGDU . 2 H1Y H 0.4974 0.5634 0.1039 0.104 Uiso 0.50 1 calc PR . 2 N21Y N 0.7212(7) 0.8567(7) 0.2313(2) 0.072(5) Uiso 0.50 1 d PGD . 2 C22Y C 0.7254(6) 0.7969(7) 0.21798(18) 0.073(6) Uiso 0.50 1 d PGDU . 2 C23Y C 0.7671(9) 0.7654(8) 0.2298(3) 0.099(7) Uiso 0.50 1 d PGDU . 2 H23Y H 0.7700 0.7245 0.2207 0.119 Uiso 0.50 1 calc PR . 2 C24Y C 0.8046(9) 0.7935(10) 0.2550(3) 0.098(7) Uiso 0.50 1 d PGDU . 2 H24Y H 0.8332 0.7719 0.2632 0.118 Uiso 0.50 1 calc PR . 2 C25Y C 0.8005(9) 0.8532(9) 0.2684(2) 0.113(8) Uiso 0.50 1 d PGDU . 2 H25Y H 0.8261 0.8725 0.2856 0.136 Uiso 0.50 1 calc PR . 2 C26Y C 0.7587(9) 0.8848(8) 0.2565(3) 0.114(9) Uiso 0.50 1 d PGDU . 2 H26Y H 0.7559 0.9257 0.2657 0.137 Uiso 0.50 1 calc PR . 2 N13Y N 0.6050(10) 0.7597(11) 0.1560(3) 0.095(11) Uiso 0.50 1 d PGDU . 2 N3Y N 0.6379(9) 0.7976(8) 0.1815(3) 0.066(5) Uiso 0.50 1 d PGDU . 2 C4Y C 0.6834(8) 0.7667(9) 0.1922(2) 0.074(6) Uiso 0.50 1 d PGDU . 2 C4'Y C 0.6786(10) 0.7098(9) 0.1733(3) 0.072(6) Uiso 0.50 1 d PGDU . 2 H4'Y H 0.7035 0.6798 0.1753 0.087 Uiso 0.50 1 calc PR . 2 C3Y C 0.6302(10) 0.7054(10) 0.1510(3) 0.078(7) Uiso 0.50 1 d PGDU . 2 H3Y H 0.6169 0.6720 0.1354 0.093 Uiso 0.50 1 calc PR . 2 C126 C 0.3490(6) 0.5412(5) 0.1081(2) 0.073(3) Uani 1 1 d D . . H12A H 0.3156 0.5650 0.1082 0.087 Uiso 1 1 calc R . 1 H12B H 0.3693 0.5451 0.1271 0.087 Uiso 1 1 calc R . 1 C132 C 0.5555(6) 0.7705(6) 0.1420(2) 0.071(3) Uani 1 1 d D . . H13A H 0.5331 0.7934 0.1546 0.085 Uiso 1 1 calc R . 1 H13B H 0.5118 0.7216 0.1346 0.085 Uiso 1 1 calc R . 1 C141 C 0.3154(6) 0.4221(6) 0.0783(2) 0.070(3) Uani 1 1 d . . . H141 H 0.3591 0.4547 0.0671 0.084 Uiso 1 1 calc R . . C142 C 0.2979(5) 0.4535(5) 0.1005(2) 0.058(3) Uani 1 1 d . . . C143 C 0.2326(6) 0.4056(6) 0.11744(18) 0.058(3) Uani 1 1 d . . . C144 C 0.1904(6) 0.3304(5) 0.11206(19) 0.063(3) Uani 1 1 d . . . H144 H 0.1483 0.2994 0.1241 0.076 Uiso 1 1 calc R . . C145 C 0.2040(5) 0.2932(5) 0.08933(18) 0.055(2) Uani 1 1 d . . . C146 C 0.2704(5) 0.3430(5) 0.0718(2) 0.059(3) Uani 1 1 d . . . C151 C 0.1253(7) 0.1016(6) 0.0528(3) 0.081(3) Uani 1 1 d . . . H151 H 0.0821 0.0691 0.0642 0.098 Uiso 1 1 calc R . . C152 C 0.1414(7) 0.0716(7) 0.0300(2) 0.080(3) Uani 1 1 d . . . H152 H 0.1083 0.0183 0.0256 0.096 Uiso 1 1 calc R . . C153 C 0.2059(8) 0.1173(7) 0.0128(3) 0.088(4) Uani 1 1 d . . . H153 H 0.2170 0.0947 -0.0026 0.106 Uiso 1 1 calc R . . C154 C 0.2521(8) 0.1947(7) 0.0185(2) 0.095(4) Uani 1 1 d . . . H154 H 0.2943 0.2259 0.0065 0.114 Uiso 1 1 calc R . . C155 C 0.2380(6) 0.2305(6) 0.0428(2) 0.066(3) Uani 1 1 d . . . C156 C 0.1740(6) 0.1830(6) 0.0598(2) 0.063(3) Uani 1 1 d . . . C161 C 0.1604(6) 0.2173(6) 0.0831(2) 0.067(3) Uani 1 1 d . . . H161 H 0.1184 0.1853 0.0950 0.081 Uiso 1 1 calc R . . C162 C 0.2843(4) 0.3100(3) 0.04839(11) 0.073(3) Uani 1 1 d . . . H162 H 0.3255 0.3418 0.0361 0.088 Uiso 1 1 calc R . . F11 F 0.3501(4) 0.7384(3) 0.15519(11) 0.145(3) Uani 1 1 d RDU . . F12 F 0.3333(4) 0.6667(3) 0.13802(11) 0.130(5) Uani 1 3 d SRDU . . B13 B 0.3333(4) 0.6667(3) 0.16667(11) 0.087(5) Uani 2.00 6 d SPRDU . . F21 F 1.0000(4) 1.0000(3) 0.15227(11) 0.169(6) Uani 1 3 d SRDU . . F22 F 0.9375(4) 0.9333(3) 0.11318(11) 0.187(5) Uani 1 1 d RDU . . B23 B 1.0000(4) 1.0000(3) 0.12365(11) 0.160(11) Uani 1 3 d SRDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0824(19) 0.0625(16) 0.0541(17) 0.0058(11) 0.0004(11) 0.0377(13) Zn2 0.0571(16) 0.0571(16) 0.059(3) 0.000 0.000 0.0286(8) C126 0.065(7) 0.053(6) 0.084(7) -0.019(5) 0.011(6) 0.017(5) C132 0.072(7) 0.087(7) 0.059(6) 0.007(5) -0.002(5) 0.043(6) C141 0.073(7) 0.066(7) 0.068(7) -0.012(5) 0.009(5) 0.032(6) C142 0.056(6) 0.050(6) 0.064(6) 0.002(5) 0.002(5) 0.024(5) C143 0.077(7) 0.063(7) 0.042(5) -0.002(5) -0.009(5) 0.041(6) C144 0.072(7) 0.054(6) 0.052(6) 0.000(5) 0.000(5) 0.022(5) C145 0.054(6) 0.057(6) 0.052(6) 0.005(5) 0.004(5) 0.026(5) C146 0.060(6) 0.054(6) 0.063(6) 0.002(5) -0.004(5) 0.028(5) C151 0.083(8) 0.058(7) 0.103(9) -0.011(6) -0.012(7) 0.035(6) C152 0.096(9) 0.063(7) 0.083(8) -0.023(7) -0.020(7) 0.041(7) C153 0.112(10) 0.074(8) 0.088(9) -0.019(7) -0.008(8) 0.053(8) C154 0.110(10) 0.084(9) 0.078(8) -0.005(7) 0.017(7) 0.040(8) C155 0.081(7) 0.068(7) 0.058(6) -0.011(5) -0.007(6) 0.044(6) C156 0.060(6) 0.067(7) 0.070(7) -0.006(5) -0.010(5) 0.038(6) C161 0.070(7) 0.061(7) 0.071(7) 0.002(5) 0.000(5) 0.033(6) C162 0.089(8) 0.057(7) 0.073(7) -0.003(5) 0.018(6) 0.035(6) F11 0.139(7) 0.125(7) 0.172(9) 0.012(6) 0.003(7) 0.068(6) F12 0.133(7) 0.133(7) 0.123(11) 0.000 0.000 0.067(3) B13 0.086(7) 0.086(7) 0.087(12) 0.000 0.000 0.043(4) F21 0.197(10) 0.197(10) 0.112(11) 0.000 0.000 0.099(5) F22 0.165(9) 0.179(10) 0.191(10) -0.004(8) -0.060(8) 0.068(8) B23 0.168(14) 0.168(14) 0.14(2) 0.000 0.000 0.084(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N11X 2.147(9) . ? Zn1 N21X 2.190(10) . ? Zn1 N3X 2.273(10) . ? Zn1 N1X 2.283(12) . ? Zn1 C3X 2.53(4) 14_455 ? N11X C12X 1.3900 . ? N11X C16X 1.3900 . ? C12X C13X 1.3900 . ? C12X C2'X 1.448(2) . ? C13X C14X 1.3900 . ? C13X H13X 0.9500 . ? C14X C15X 1.3900 . ? C14X H14X 0.9500 . ? C15X C16X 1.3900 . ? C15X H15X 0.9500 . ? C16X H16X 0.9500 . ? N12X C126 1.279(11) . ? N12X C1X 1.4200 . ? N12X N1X 1.4200 . ? C1X C2X 1.4200 . ? C1X H1X 0.9500 . ? C2X C2'X 1.4200 . ? C2X H2X 0.9500 . ? C2'X N1X 1.4200 . ? N21X C22X 1.3900 . ? N21X C26X 1.3900 . ? C22X C23X 1.3900 . ? C22X C4'X 1.449(2) . ? C23X C24X 1.3900 . ? C23X H23X 0.9500 . ? C24X C25X 1.3900 . ? C24X H24X 0.9500 . ? C25X C26X 1.3900 . ? C25X H25X 0.9500 . ? C26X H26X 0.9500 . ? N13X C132 1.411(11) . ? N13X C3X 1.4200 . ? N13X N3X 1.4200 . ? C3X C4X 1.4200 . ? C3X Zn1 2.525(11) 15 ? C3X H3X 0.9500 . ? C4X C4'X 1.4200 . ? C4X H4X 0.9500 . ? C4'X N3X 1.4200 . ? Zn2 N11Y 2.15(3) . ? Zn2 N11Y 2.15(4) 2_665 ? Zn2 N11Y 2.15(6) 3_565 ? Zn2 N1Y 2.27(7) 2_665 ? Zn2 N1Y 2.27(3) . ? Zn2 N1Y 2.27(5) 3_565 ? N11Y C12Y 1.3900 . ? N11Y C16Y 1.3900 . ? C12Y C13Y 1.3900 . ? C12Y C2Y 1.450(2) . ? C13Y C14Y 1.3900 . ? C13Y H13Y 0.9500 . ? C14Y C15Y 1.3900 . ? C14Y H14Y 0.9500 . ? C15Y C16Y 1.3900 . ? C15Y H15Y 0.9500 . ? C16Y H16Y 0.9500 . ? N12Y N1Y 1.4200 . ? N12Y C1Y 1.4200 . ? N12Y C126 1.420(12) . ? N1Y C2Y 1.4200 . ? C2Y C2'Y 1.4200 . ? C2'Y C1Y 1.4200 . ? C2'Y H2'Y 0.9500 . ? C1Y H1Y 0.9500 . ? N21Y C22Y 1.3900 . ? N21Y C26Y 1.3900 . ? C22Y C23Y 1.3900 . ? C22Y C4Y 1.448(2) . ? C23Y C24Y 1.3900 . ? C23Y H23Y 0.9500 . ? C24Y C25Y 1.3900 . ? C24Y H24Y 0.9500 . ? C25Y C26Y 1.3900 . ? C25Y H25Y 0.9500 . ? C26Y H26Y 0.9500 . ? N13Y C132 1.300(12) . ? N13Y N3Y 1.4200 . ? N13Y C3Y 1.4200 . ? N3Y C4Y 1.4200 . ? C4Y C4'Y 1.4200 . ? C4'Y C3Y 1.4200 . ? C4'Y H4'Y 0.9500 . ? C3Y H3Y 0.9500 . ? C126 C142 1.560(13) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? C132 C143 1.547(13) 2_665 ? C132 H13A 0.9900 . ? C132 H13B 0.9900 . ? C141 C142 1.369(13) . ? C141 C146 1.402(13) . ? C141 H141 0.9500 . ? C142 C143 1.422(13) . ? C143 C144 1.324(12) . ? C143 C132 1.547(13) 3_565 ? C144 C145 1.423(13) . ? C144 H144 0.9500 . ? C145 C161 1.346(13) . ? C145 C146 1.460(13) . ? C146 C162 1.401(11) . ? C151 C152 1.362(15) . ? C151 C156 1.450(14) . ? C151 H151 0.9500 . ? C152 C153 1.415(16) . ? C152 H152 0.9500 . ? C153 C154 1.369(15) . ? C153 H153 0.9500 . ? C154 C155 1.471(15) . ? C154 H154 0.9500 . ? C155 C162 1.401(11) . ? C155 C156 1.406(14) . ? C156 C161 1.412(13) . ? C161 H161 0.9500 . ? C162 H162 0.9500 . ? F11 B13 1.4057 . ? F11 F12 1.5349 . ? F11 F11 1.701(8) 14_455 ? F11 F11 1.701(8) 15 ? F12 B13 1.3818 . ? F12 F11 1.535(9) 3_565 ? F12 F11 1.535(9) 2_665 ? B13 F12 1.382(11) 13_565 ? B13 F11 1.406(9) 3_565 ? B13 F11 1.406(10) 2_665 ? B13 F11 1.406(12) 13_565 ? B13 F11 1.406(7) 14_455 ? B13 F11 1.406(7) 15 ? F21 B23 1.3804 . ? F22 B23 1.3830 . ? B23 F22 1.383(10) 2_765 ? B23 F22 1.383(10) 3_675 ? 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 N11X Zn1 N21X 96.8(5) . . ? N11X Zn1 N3X 87.8(5) . . ? N21X Zn1 N3X 78.0(4) . . ? N11X Zn1 N1X 76.7(4) . . ? N21X Zn1 N1X 172.8(5) . . ? N3X Zn1 N1X 98.6(6) . . ? N11X Zn1 C3X 169.5(10) . 14_455 ? N21X Zn1 C3X 84.5(9) . 14_455 ? N3X Zn1 C3X 102.7(9) . 14_455 ? N1X Zn1 C3X 102.5(9) . 14_455 ? C12X N11X C16X 120.0 . . ? C12X N11X Zn1 116.1(6) . . ? C16X N11X Zn1 123.8(6) . . ? C13X C12X N11X 120.0 . . ? C13X C12X C2'X 121.2(9) . . ? N11X C12X C2'X 118.8(9) . . ? C14X C13X C12X 120.0 . . ? C14X C13X H13X 120.0 . . ? C12X C13X H13X 120.0 . . ? C13X C14X C15X 120.0 . . ? C13X C14X H14X 120.0 . . ? C15X C14X H14X 120.0 . . ? C16X C15X C14X 120.0 . . ? C16X C15X H15X 120.0 . . ? C14X C15X H15X 120.0 . . ? C15X C16X N11X 120.0 . . ? C15X C16X H16X 120.0 . . ? N11X C16X H16X 120.0 . . ? C126 N12X C1X 123.9(15) . . ? C126 N12X N1X 128.0(15) . . ? C1X N12X N1X 108.0 . . ? N12X C1X C2X 108.0 . . ? N12X C1X H1X 126.0 . . ? C2X C1X H1X 126.0 . . ? C1X C2X C2'X 108.0 . . ? C1X C2X H2X 126.0 . . ? C2'X C2X H2X 126.0 . . ? N1X C2'X C2X 108.0 . . ? N1X C2'X C12X 116.3(11) . . ? C2X C2'X C12X 135.7(11) . . ? C2'X N1X N12X 108.0 . . ? C2'X N1X Zn1 111.8(9) . . ? N12X N1X Zn1 139.5(9) . . ? C22X N21X C26X 120.0 . . ? C22X N21X Zn1 115.7(7) . . ? C26X N21X Zn1 124.3(7) . . ? N21X C22X C23X 120.0 . . ? N21X C22X C4'X 115.5(10) . . ? C23X C22X C4'X 124.5(10) . . ? C22X C23X C24X 120.0 . . ? C22X C23X H23X 120.0 . . ? C24X C23X H23X 120.0 . . ? C25X C24X C23X 120.0 . . ? C25X C24X H24X 120.0 . . ? C23X C24X H24X 120.0 . . ? C24X C25X C26X 120.0 . . ? C24X C25X H25X 120.0 . . ? C26X C25X H25X 120.0 . . ? C25X C26X N21X 120.0 . . ? C25X C26X H26X 120.0 . . ? N21X C26X H26X 120.0 . . ? C132 N13X C3X 130.3(10) . . ? C132 N13X N3X 121.6(10) . . ? C3X N13X N3X 108.0 . . ? C4X C3X N13X 108.0 . . ? C4X C3X Zn1 124.2(7) . 15 ? N13X C3X Zn1 123.2(6) . 15 ? C4X C3X H3X 126.0 . . ? N13X C3X H3X 126.0 . . ? Zn1 C3X H3X 19.2 15 . ? C3X C4X C4'X 108.0 . . ? C3X C4X H4X 126.0 . . ? C4'X C4X H4X 126.0 . . ? C4X C4'X N3X 108.0 . . ? C4X C4'X C22X 129.3(11) . . ? N3X C4'X C22X 122.4(10) . . ? N13X N3X C4'X 108.0 . . ? N13X N3X Zn1 143.3(7) . . ? C4'X N3X Zn1 108.4(7) . . ? N11Y Zn2 N11Y 96.8(19) . 2_665 ? N11Y Zn2 N11Y 96.8(12) . 3_565 ? N11Y Zn2 N11Y 96.8(9) 2_665 3_565 ? N11Y Zn2 N1Y 88(3) . 2_665 ? N11Y Zn2 N1Y 77(2) 2_665 2_665 ? N11Y Zn2 N1Y 172.1(15) 3_565 2_665 ? N11Y Zn2 N1Y 76.7(6) . . ? N11Y Zn2 N1Y 172(3) 2_665 . ? N11Y Zn2 N1Y 88(2) 3_565 . ? N1Y Zn2 N1Y 98.6(15) 2_665 . ? N11Y Zn2 N1Y 172(4) . 3_565 ? N11Y Zn2 N1Y 88.4(15) 2_665 3_565 ? N11Y Zn2 N1Y 77(2) 3_565 3_565 ? N1Y Zn2 N1Y 98.6(15) 2_665 3_565 ? N1Y Zn2 N1Y 99(2) . 3_565 ? C12Y N11Y C16Y 120.0 . . ? C12Y N11Y Zn2 115.4(11) . . ? C16Y N11Y Zn2 124.2(12) . . ? N11Y C12Y C13Y 120.0 . . ? N11Y C12Y C2Y 119.6(9) . . ? C13Y C12Y C2Y 120.4(9) . . ? C14Y C13Y C12Y 120.0 . . ? C14Y C13Y H13Y 120.0 . . ? C12Y C13Y H13Y 120.0 . . ? C15Y C14Y C13Y 120.0 . . ? C15Y C14Y H14Y 120.0 . . ? C13Y C14Y H14Y 120.0 . . ? C14Y C15Y C16Y 120.0 . . ? C14Y C15Y H15Y 120.0 . . ? C16Y C15Y H15Y 120.0 . . ? C15Y C16Y N11Y 120.0 . . ? C15Y C16Y H16Y 120.0 . . ? N11Y C16Y H16Y 120.0 . . ? N1Y N12Y C1Y 108.0 . . ? N1Y N12Y C126 130.0(11) . . ? C1Y N12Y C126 121.9(11) . . ? C2Y N1Y N12Y 108.0 . . ? C2Y N1Y Zn2 112.9(12) . . ? N12Y N1Y Zn2 139.0(13) . . ? C2'Y C2Y N1Y 108.0 . . ? C2'Y C2Y C12Y 137.0(11) . . ? N1Y C2Y C12Y 115.0(11) . . ? C2Y C2'Y C1Y 108.0 . . ? C2Y C2'Y H2'Y 126.0 . . ? C1Y C2'Y H2'Y 126.0 . . ? C2'Y C1Y N12Y 108.0 . . ? C2'Y C1Y H1Y 126.0 . . ? N12Y C1Y H1Y 126.0 . . ? C22Y N21Y C26Y 120.0 . . ? N21Y C22Y C23Y 120.0 . . ? N21Y C22Y C4Y 118.9(10) . . ? C23Y C22Y C4Y 121.0(10) . . ? C24Y C23Y C22Y 120.0 . . ? C24Y C23Y H23Y 120.0 . . ? C22Y C23Y H23Y 120.0 . . ? C23Y C24Y C25Y 120.0 . . ? C23Y C24Y H24Y 120.0 . . ? C25Y C24Y H24Y 120.0 . . ? C26Y C25Y C24Y 120.0 . . ? C26Y C25Y H25Y 120.0 . . ? C24Y C25Y H25Y 120.0 . . ? C25Y C26Y N21Y 120.0 . . ? C25Y C26Y H26Y 120.0 . . ? N21Y C26Y H26Y 120.0 . . ? C132 N13Y N3Y 123.5(13) . . ? C132 N13Y C3Y 128.3(13) . . ? N3Y N13Y C3Y 108.0 . . ? C4Y N3Y N13Y 108.0 . . ? N3Y C4Y C4'Y 108.0 . . ? N3Y C4Y C22Y 119.4(11) . . ? C4'Y C4Y C22Y 132.6(11) . . ? C4Y C4'Y C3Y 108.0 . . ? C4Y C4'Y H4'Y 126.0 . . ? C3Y C4'Y H4'Y 126.0 . . ? C4'Y C3Y N13Y 108.0 . . ? C4'Y C3Y H3Y 126.0 . . ? N13Y C3Y H3Y 126.0 . . ? N12X C126 N12Y 3.1(13) . . ? N12X C126 C142 114.9(13) . . ? N12Y C126 C142 114.6(9) . . ? N12X C126 H12A 108.5 . . ? N12Y C126 H12A 106.0 . . ? C142 C126 H12A 108.5 . . ? N12X C126 H12B 108.5 . . ? N12Y C126 H12B 111.3 . . ? C142 C126 H12B 108.5 . . ? H12A C126 H12B 107.5 . . ? N13Y C132 N13X 5.2(13) . . ? N13Y C132 C143 112.0(12) . 2_665 ? N13X C132 C143 116.3(9) . 2_665 ? N13Y C132 H13A 107.8 . . ? N13X C132 H13A 108.2 . . ? C143 C132 H13A 108.2 2_665 . ? N13Y C132 H13B 113.1 . . ? N13X C132 H13B 108.2 . . ? C143 C132 H13B 108.2 2_665 . ? H13A C132 H13B 107.4 . . ? C142 C141 C146 121.4(10) . . ? C142 C141 H141 119.3 . . ? C146 C141 H141 119.3 . . ? C141 C142 C143 120.0(9) . . ? C141 C142 C126 121.3(9) . . ? C143 C142 C126 118.7(8) . . ? C144 C143 C142 119.7(9) . . ? C144 C143 C132 122.7(9) . 3_565 ? C142 C143 C132 117.6(8) . 3_565 ? C143 C144 C145 124.0(9) . . ? C143 C144 H144 118.0 . . ? C145 C144 H144 118.0 . . ? C161 C145 C144 124.9(9) . . ? C161 C145 C146 119.2(9) . . ? C144 C145 C146 115.9(8) . . ? C162 C146 C141 122.8(8) . . ? C162 C146 C145 118.2(8) . . ? C141 C146 C145 119.0(9) . . ? C152 C151 C156 120.3(11) . . ? C152 C151 H151 119.9 . . ? C156 C151 H151 119.9 . . ? C151 C152 C153 122.0(10) . . ? C151 C152 H152 119.0 . . ? C153 C152 H152 119.0 . . ? C154 C153 C152 119.1(11) . . ? C154 C153 H153 120.5 . . ? C152 C153 H153 120.5 . . ? C153 C154 C155 121.5(12) . . ? C153 C154 H154 119.2 . . ? C155 C154 H154 119.2 . . ? C162 C155 C156 120.7(8) . . ? C162 C155 C154 121.5(10) . . ? C156 C155 C154 117.7(10) . . ? C155 C156 C161 117.7(9) . . ? C155 C156 C151 119.4(10) . . ? C161 C156 C151 122.9(10) . . ? C145 C161 C156 123.3(10) . . ? C145 C161 H161 118.3 . . ? C156 C161 H161 118.3 . . ? C146 C162 C155 120.7(7) . . ? C146 C162 H162 119.6 . . ? C155 C162 H162 119.6 . . ? B13 F11 F12 55.8 . . ? B13 F11 F11 52.8(2) . 14_455 ? F12 F11 F11 91.8(3) . 14_455 ? B13 F11 F11 52.8(2) . 15 ? F12 F11 F11 91.8(3) . 15 ? F11 F11 F11 82.2(5) 14_455 15 ? B13 F12 F11 57.3(2) . 3_565 ? B13 F12 F11 57.3 . . ? F11 F12 F11 93.6(3) 3_565 . ? B13 F12 F11 57.3(2) . 2_665 ? F11 F12 F11 93.6 3_565 2_665 ? F11 F12 F11 93.6(3) . 2_665 ? F12 B13 F12 180.0(6) . 13_565 ? F12 B13 F11 66.82(17) . 3_565 ? F12 B13 F11 113.2(7) 13_565 3_565 ? F12 B13 F11 66.8 . . ? F12 B13 F11 113.2(5) 13_565 . ? F11 B13 F11 105.5(4) 3_565 . ? F12 B13 F11 66.82(17) . 2_665 ? F12 B13 F11 113.2(7) 13_565 2_665 ? F11 B13 F11 105.52(18) 3_565 2_665 ? F11 B13 F11 105.5(4) . 2_665 ? F12 B13 F11 113.2(5) . 13_565 ? F12 B13 F11 66.8(5) 13_565 13_565 ? F11 B13 F11 74.5(5) 3_565 13_565 ? F11 B13 F11 180.0(6) . 13_565 ? F11 B13 F11 74.5(5) 2_665 13_565 ? F12 B13 F11 113.2(4) . 14_455 ? F12 B13 F11 66.8(6) 13_565 14_455 ? F11 B13 F11 74.5(4) 3_565 14_455 ? F11 B13 F11 74.5(3) . 14_455 ? F11 B13 F11 180.0(7) 2_665 14_455 ? F11 B13 F11 105.5(5) 13_565 14_455 ? F12 B13 F11 113.2(4) . 15 ? F12 B13 F11 66.8(6) 13_565 15 ? F11 B13 F11 180.0(5) 3_565 15 ? F11 B13 F11 74.5(3) . 15 ? F11 B13 F11 74.5(4) 2_665 15 ? F11 B13 F11 105.5(5) 13_565 15 ? F11 B13 F11 105.5(6) 14_455 15 ? F21 B23 F22 111.40(16) . 2_765 ? F21 B23 F22 111.40(16) . 3_675 ? F22 B23 F22 107.5(2) 2_765 3_675 ? F21 B23 F22 111.4 . . ? F22 B23 F22 107.5(4) 2_765 . ? F22 B23 F22 107.5(4) 3_675 . ? 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 N21X Zn1 N11X C12X -176.4(7) . . . . ? N3X Zn1 N11X C12X -98.8(7) . . . . ? N1X Zn1 N11X C12X 0.7(7) . . . . ? C3X Zn1 N11X C12X 87(5) 14_455 . . . ? N21X Zn1 N11X C16X -0.2(6) . . . . ? N3X Zn1 N11X C16X 77.5(6) . . . . ? N1X Zn1 N11X C16X 176.9(7) . . . . ? C3X Zn1 N11X C16X -96(5) 14_455 . . . ? C16X N11X C12X C13X 0.0 . . . . ? Zn1 N11X C12X C13X 176.4(8) . . . . ? C16X N11X C12X C2'X 179.6(12) . . . . ? Zn1 N11X C12X C2'X -3.9(12) . . . . ? N11X C12X C13X C14X 0.0 . . . . ? C2'X C12X C13X C14X -179.6(12) . . . . ? C12X C13X C14X C15X 0.0 . . . . ? C13X C14X C15X C16X 0.0 . . . . ? C14X C15X C16X N11X 0.0 . . . . ? C12X N11X C16X C15X 0.0 . . . . ? Zn1 N11X C16X C15X -176.1(8) . . . . ? C126 N12X C1X C2X 176(2) . . . . ? N1X N12X C1X C2X 0.0 . . . . ? N12X C1X C2X C2'X 0.0 . . . . ? C1X C2X C2'X N1X 0.0 . . . . ? C1X C2X C2'X C12X 178(2) . . . . ? C13X C12X C2'X N1X -174.0(10) . . . . ? N11X C12X C2'X N1X 6.4(17) . . . . ? C13X C12X C2'X C2X 9(2) . . . . ? N11X C12X C2'X C2X -171.1(14) . . . . ? C2X C2'X N1X N12X 0.0 . . . . ? C12X C2'X N1X N12X -178.2(19) . . . . ? C2X C2'X N1X Zn1 172.8(13) . . . . ? C12X C2'X N1X Zn1 -5.4(16) . . . . ? C126 N12X N1X C2'X -176(2) . . . . ? C1X N12X N1X C2'X 0.0 . . . . ? C126 N12X N1X Zn1 15(3) . . . . ? C1X N12X N1X Zn1 -169.6(18) . . . . ? N11X Zn1 N1X C2'X 2.6(10) . . . . ? N21X Zn1 N1X C2'X 27(5) . . . . ? N3X Zn1 N1X C2'X 88.2(10) . . . . ? C3X Zn1 N1X C2'X -166.6(13) 14_455 . . . ? N11X Zn1 N1X N12X 172.0(17) . . . . ? N21X Zn1 N1X N12X -164(4) . . . . ? N3X Zn1 N1X N12X -102.4(17) . . . . ? C3X Zn1 N1X N12X 3(2) 14_455 . . . ? N11X Zn1 N21X C22X 86.0(7) . . . . ? N3X Zn1 N21X C22X -0.2(7) . . . . ? N1X Zn1 N21X C22X 62(5) . . . . ? C3X Zn1 N21X C22X -104.5(11) 14_455 . . . ? N11X Zn1 N21X C26X -95.0(6) . . . . ? N3X Zn1 N21X C26X 178.8(6) . . . . ? N1X Zn1 N21X C26X -119(5) . . . . ? C3X Zn1 N21X C26X 74.5(11) 14_455 . . . ? C26X N21X C22X C23X 0.0 . . . . ? Zn1 N21X C22X C23X 179.0(8) . . . . ? C26X N21X C22X C4'X -178.4(10) . . . . ? Zn1 N21X C22X C4'X 0.6(11) . . . . ? N21X C22X C23X C24X 0.0 . . . . ? C4'X C22X C23X C24X 178.3(11) . . . . ? C22X C23X C24X C25X 0.0 . . . . ? C23X C24X C25X C26X 0.0 . . . . ? C24X C25X C26X N21X 0.0 . . . . ? C22X N21X C26X C25X 0.0 . . . . ? Zn1 N21X C26X C25X -178.9(9) . . . . ? C132 N13X C3X C4X -177.4(11) . . . . ? N3X N13X C3X C4X 0.0 . . . . ? C132 N13X C3X Zn1 25.8(9) . . . 15 ? N3X N13X C3X Zn1 -156.8(13) . . . 15 ? N13X C3X C4X C4'X 0.0 . . . . ? Zn1 C3X C4X C4'X 156.5(13) 15 . . . ? C3X C4X C4'X N3X 0.0 . . . . ? C3X C4X C4'X C22X 174.0(16) . . . . ? N21X C22X C4'X C4X -174.2(11) . . . . ? C23X C22X C4'X C4X 7.5(18) . . . . ? N21X C22X C4'X N3X -0.9(13) . . . . ? C23X C22X C4'X N3X -179.2(6) . . . . ? C132 N13X N3X C4'X 177.6(10) . . . . ? C3X N13X N3X C4'X 0.0 . . . . ? C132 N13X N3X Zn1 5(2) . . . . ? C3X N13X N3X Zn1 -172.4(15) . . . . ? C4X C4'X N3X N13X 0.0 . . . . ? C22X C4'X N3X N13X -174.5(15) . . . . ? C4X C4'X N3X Zn1 175.2(9) . . . . ? C22X C4'X N3X Zn1 0.7(8) . . . . ? N11X Zn1 N3X N13X 74.7(15) . . . . ? N21X Zn1 N3X N13X 172.1(16) . . . . ? N1X Zn1 N3X N13X -1.5(16) . . . . ? C3X Zn1 N3X N13X -106.4(7) 14_455 . . . ? N11X Zn1 N3X C4'X -97.6(4) . . . . ? N21X Zn1 N3X C4'X -0.2(4) . . . . ? N1X Zn1 N3X C4'X -173.8(5) . . . . ? C3X Zn1 N3X C4'X 81.2(8) 14_455 . . . ? N11Y Zn2 N11Y C12Y 171.5(11) 2_665 . . . ? N11Y Zn2 N11Y C12Y -90.8(9) 3_565 . . . ? N1Y Zn2 N11Y C12Y 95(2) 2_665 . . . ? N1Y Zn2 N11Y C12Y -4(2) . . . . ? N1Y Zn2 N11Y C12Y -57(10) 3_565 . . . ? N11Y Zn2 N11Y C16Y -1(3) 2_665 . . . ? N11Y Zn2 N11Y C16Y 96(2) 3_565 . . . ? N1Y Zn2 N11Y C16Y -77.7(13) 2_665 . . . ? N1Y Zn2 N11Y C16Y -176.9(7) . . . . ? N1Y Zn2 N11Y C16Y 130(10) 3_565 . . . ? C16Y N11Y C12Y C13Y 0.0 . . . . ? Zn2 N11Y C12Y C13Y -173.1(19) . . . . ? C16Y N11Y C12Y C2Y -179.3(11) . . . . ? Zn2 N11Y C12Y C2Y 8(2) . . . . ? N11Y C12Y C13Y C14Y 0.0 . . . . ? C2Y C12Y C13Y C14Y 179.2(12) . . . . ? C12Y C13Y C14Y C15Y 0.0 . . . . ? C13Y C14Y C15Y C16Y 0.0 . . . . ? C14Y C15Y C16Y N11Y 0.0 . . . . ? C12Y N11Y C16Y C15Y 0.0 . . . . ? Zn2 N11Y C16Y C15Y 172.5(19) . . . . ? C1Y N12Y N1Y C2Y 0.0 . . . . ? C126 N12Y N1Y C2Y 175.5(17) . . . . ? C1Y N12Y N1Y Zn2 175(3) . . . . ? C126 N12Y N1Y Zn2 -9(3) . . . . ? N11Y Zn2 N1Y C2Y 0(2) . . . . ? N11Y Zn2 N1Y C2Y -34(13) 2_665 . . . ? N11Y Zn2 N1Y C2Y 97.7(16) 3_565 . . . ? N1Y Zn2 N1Y C2Y -86.0(18) 2_665 . . . ? N1Y Zn2 N1Y C2Y 173.9(14) 3_565 . . . ? N11Y Zn2 N1Y N12Y -175.1(16) . . . . ? N11Y Zn2 N1Y N12Y 151(10) 2_665 . . . ? N11Y Zn2 N1Y N12Y -77.7(18) 3_565 . . . ? N1Y Zn2 N1Y N12Y 99(3) 2_665 . . . ? N1Y Zn2 N1Y N12Y -1(4) 3_565 . . . ? N12Y N1Y C2Y C2'Y 0.0 . . . . ? Zn2 N1Y C2Y C2'Y -177(2) . . . . ? N12Y N1Y C2Y C12Y -179.8(17) . . . . ? Zn2 N1Y C2Y C12Y 3(2) . . . . ? N11Y C12Y C2Y C2'Y 172.9(13) . . . . ? C13Y C12Y C2Y C2'Y -6(2) . . . . ? N11Y C12Y C2Y N1Y -7.4(16) . . . . ? C13Y C12Y C2Y N1Y 173.4(9) . . . . ? N1Y C2Y C2'Y C1Y 0.0 . . . . ? C12Y C2Y C2'Y C1Y 180(2) . . . . ? C2Y C2'Y C1Y N12Y 0.0 . . . . ? N1Y N12Y C1Y C2'Y 0.0 . . . . ? C126 N12Y C1Y C2'Y -175.9(16) . . . . ? C26Y N21Y C22Y C23Y 0.0 . . . . ? C26Y N21Y C22Y C4Y 177.8(10) . . . . ? N21Y C22Y C23Y C24Y 0.0 . . . . ? C4Y C22Y C23Y C24Y -177.7(11) . . . . ? C22Y C23Y C24Y C25Y 0.0 . . . . ? C23Y C24Y C25Y C26Y 0.0 . . . . ? C24Y C25Y C26Y N21Y 0.0 . . . . ? C22Y N21Y C26Y C25Y 0.0 . . . . ? C132 N13Y N3Y C4Y 174.6(19) . . . . ? C3Y N13Y N3Y C4Y 0.0 . . . . ? N13Y N3Y C4Y C4'Y 0.0 . . . . ? N13Y N3Y C4Y C22Y 178.5(15) . . . . ? N21Y C22Y C4Y N3Y -1.2(15) . . . . ? C23Y C22Y C4Y N3Y 176.5(9) . . . . ? N21Y C22Y C4Y C4'Y 176.8(11) . . . . ? C23Y C22Y C4Y C4'Y -5.4(17) . . . . ? N3Y C4Y C4'Y C3Y 0.0 . . . . ? C22Y C4Y C4'Y C3Y -178.2(17) . . . . ? C4Y C4'Y C3Y N13Y 0.0 . . . . ? C132 N13Y C3Y C4'Y -174(2) . . . . ? N3Y N13Y C3Y C4'Y 0.0 . . . . ? C1X N12X C126 N12Y -3(30) . . . . ? N1X N12X C126 N12Y 172(32) . . . . ? C1X N12X C126 C142 83.6(17) . . . . ? N1X N12X C126 C142 -101.2(19) . . . . ? N1Y N12Y C126 N12X -166(32) . . . . ? C1Y N12Y C126 N12X 9(30) . . . . ? N1Y N12Y C126 C142 99.0(15) . . . . ? C1Y N12Y C126 C142 -86.1(14) . . . . ? N3Y N13Y C132 N13X -114(12) . . . . ? C3Y N13Y C132 N13X 59(11) . . . . ? N3Y N13Y C132 C143 100.4(14) . . . 2_665 ? C3Y N13Y C132 C143 -86.1(16) . . . 2_665 ? C3X N13X C132 N13Y 43(12) . . . . ? N3X N13X C132 N13Y -134(13) . . . . ? C3X N13X C132 C143 79.2(9) . . . 2_665 ? N3X N13X C132 C143 -97.8(13) . . . 2_665 ? C146 C141 C142 C143 -0.2(15) . . . . ? C146 C141 C142 C126 178.8(9) . . . . ? N12X C126 C142 C141 1.4(17) . . . . ? N12Y C126 C142 C141 4.9(15) . . . . ? N12X C126 C142 C143 -179.6(13) . . . . ? N12Y C126 C142 C143 -176.1(10) . . . . ? C141 C142 C143 C144 1.8(14) . . . . ? C126 C142 C143 C144 -177.2(9) . . . . ? C141 C142 C143 C132 -179.1(9) . . . 3_565 ? C126 C142 C143 C132 1.9(13) . . . 3_565 ? C142 C143 C144 C145 -2.4(15) . . . . ? C132 C143 C144 C145 178.5(9) 3_565 . . . ? C143 C144 C145 C161 -178.1(10) . . . . ? C143 C144 C145 C146 1.4(14) . . . . ? C142 C141 C146 C162 176.4(9) . . . . ? C142 C141 C146 C145 -0.7(15) . . . . ? C161 C145 C146 C162 2.5(13) . . . . ? C144 C145 C146 C162 -177.1(8) . . . . ? C161 C145 C146 C141 179.8(9) . . . . ? C144 C145 C146 C141 0.2(13) . . . . ? C156 C151 C152 C153 1.1(17) . . . . ? C151 C152 C153 C154 -2.3(18) . . . . ? C152 C153 C154 C155 2.4(19) . . . . ? C153 C154 C155 C162 -178.6(10) . . . . ? C153 C154 C155 C156 -1.5(17) . . . . ? C162 C155 C156 C161 -2.9(13) . . . . ? C154 C155 C156 C161 180.0(9) . . . . ? C162 C155 C156 C151 177.5(8) . . . . ? C154 C155 C156 C151 0.3(14) . . . . ? C152 C151 C156 C155 -0.2(15) . . . . ? C152 C151 C156 C161 -179.8(10) . . . . ? C144 C145 C161 C156 177.6(9) . . . . ? C146 C145 C161 C156 -2.0(14) . . . . ? C155 C156 C161 C145 2.1(14) . . . . ? C151 C156 C161 C145 -178.2(9) . . . . ? C141 C146 C162 C155 179.6(9) . . . . ? C145 C146 C162 C155 -3.3(12) . . . . ? C156 C155 C162 C146 3.5(12) . . . . ? C154 C155 C162 C146 -179.4(9) . . . . ? F11 F11 F12 B13 41.1(3) 14_455 . . . ? F11 F11 F12 B13 -41.2(3) 15 . . . ? B13 F11 F12 F11 -46.9(3) . . . 3_565 ? F11 F11 F12 F11 -5.8(3) 14_455 . . 3_565 ? F11 F11 F12 F11 -88.1(3) 15 . . 3_565 ? B13 F11 F12 F11 46.9(3) . . . 2_665 ? F11 F11 F12 F11 88.1(3) 14_455 . . 2_665 ? F11 F11 F12 F11 5.8(3) 15 . . 2_665 ? F11 F12 B13 F12 165(100) 3_565 . . 13_565 ? F11 F12 B13 F12 45(100) . . . 13_565 ? F11 F12 B13 F12 -75(100) 2_665 . . 13_565 ? F11 F12 B13 F11 -120.0(5) . . . 3_565 ? F11 F12 B13 F11 120.0(5) 2_665 . . 3_565 ? F11 F12 B13 F11 120.0(5) 3_565 . . . ? F11 F12 B13 F11 -120.0(5) 2_665 . . . ? F11 F12 B13 F11 -120.0(5) 3_565 . . 2_665 ? F11 F12 B13 F11 120.0(5) . . . 2_665 ? F11 F12 B13 F11 -60.0(3) 3_565 . . 13_565 ? F11 F12 B13 F11 180.0(6) . . . 13_565 ? F11 F12 B13 F11 60.0(3) 2_665 . . 13_565 ? F11 F12 B13 F11 60.0(3) 3_565 . . 14_455 ? F11 F12 B13 F11 -60.0(3) . . . 14_455 ? F11 F12 B13 F11 180.0(5) 2_665 . . 14_455 ? F11 F12 B13 F11 180.0(5) 3_565 . . 15 ? F11 F12 B13 F11 60.0(3) . . . 15 ? F11 F12 B13 F11 -60.0(3) 2_665 . . 15 ? F11 F11 B13 F12 -124.3(4) 14_455 . . . ? F11 F11 B13 F12 124.3(4) 15 . . . ? F12 F11 B13 F12 180.0(6) . . . 13_565 ? F11 F11 B13 F12 55.7(7) 14_455 . . 13_565 ? F11 F11 B13 F12 -55.7(7) 15 . . 13_565 ? F12 F11 B13 F11 55.7(3) . . . 3_565 ? F11 F11 B13 F11 -68.6(5) 14_455 . . 3_565 ? F11 F11 B13 F11 180.0(5) 15 . . 3_565 ? F12 F11 B13 F11 -55.7(3) . . . 2_665 ? F11 F11 B13 F11 180.0(5) 14_455 . . 2_665 ? F11 F11 B13 F11 68.6(5) 15 . . 2_665 ? F12 F11 B13 F11 -157(100) . . . 13_565 ? F11 F11 B13 F11 78(100) 14_455 . . 13_565 ? F11 F11 B13 F11 -33(100) 15 . . 13_565 ? F12 F11 B13 F11 124.3(4) . . . 14_455 ? F11 F11 B13 F11 -111.4(8) 15 . . 14_455 ? F12 F11 B13 F11 -124.3(4) . . . 15 ? F11 F11 B13 F11 111.4(8) 14_455 . . 15 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.677 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.214 #===END data_imw1233p21c _database_code_depnum_ccdc_archive 'CCDC 708983' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H28 B2 Cd F8 N8 O4' _chemical_formula_weight 850.62 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.0291(3) _cell_length_b 13.6181(3) _cell_length_c 16.6842(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.2560(10) _cell_angle_gamma 90.00 _cell_volume 3237.56(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9195 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 30.43 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6542 _exptl_absorpt_correction_T_max 0.7474 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57974 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0115 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7425 _reflns_number_gt 7253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. 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^)+(0.0241P)^2^+8.8018P] 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 7425 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.253 _refine_ls_restrained_S_all 1.253 _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 Cd1 Cd 0.502746(14) 0.403878(16) 0.222332(13) 0.01715(7) Uani 1 1 d . . . N11 N 0.44794(16) 0.41520(18) 0.32369(16) 0.0165(5) Uani 1 1 d . . . C12 C 0.50590(19) 0.38483(19) 0.40805(18) 0.0148(5) Uani 1 1 d . . . C13 C 0.4783(2) 0.3851(2) 0.47571(19) 0.0188(6) Uani 1 1 d . . . H13 H 0.5202 0.3640 0.5349 0.023 Uiso 1 1 calc R . . C15 C 0.3292(2) 0.4479(2) 0.3689(2) 0.0241(6) Uani 1 1 d . . . H15 H 0.2675 0.4700 0.3538 0.029 Uiso 1 1 calc R . . C14 C 0.3888(2) 0.4168(2) 0.4554(2) 0.0233(6) Uani 1 1 d . . . H14 H 0.3684 0.4171 0.5006 0.028 Uiso 1 1 calc R . . C16 C 0.3615(2) 0.4462(2) 0.3048(2) 0.0211(6) Uani 1 1 d . . . H16 H 0.3210 0.4678 0.2454 0.025 Uiso 1 1 calc R . . N21 N 0.70926(16) 0.30703(17) 0.39268(17) 0.0173(5) Uani 1 1 d . . . N22 N 0.62120(16) 0.34361(17) 0.35672(16) 0.0158(4) Uani 1 1 d . . . C23 C 0.59977(19) 0.35026(19) 0.42544(18) 0.0155(5) Uani 1 1 d . . . C24 C 0.6749(2) 0.3179(2) 0.5057(2) 0.0205(6) Uani 1 1 d . . . H24 H 0.6782 0.3155 0.5640 0.025 Uiso 1 1 calc R . . C25 C 0.7428(2) 0.2902(2) 0.4816(2) 0.0220(6) Uani 1 1 d . . . H25 H 0.8028 0.2639 0.5207 0.026 Uiso 1 1 calc R . . C26 C 0.75531(19) 0.2830(2) 0.3363(2) 0.0193(6) Uani 1 1 d . . . H26A H 0.7107 0.2951 0.2723 0.023 Uiso 1 1 calc R . . H26B H 0.7716 0.2123 0.3430 0.023 Uiso 1 1 calc R . . N31 N 0.42446(16) 0.36473(17) 0.07392(15) 0.0147(4) Uani 1 1 d . . . C32 C 0.47400(19) 0.37070(19) 0.02637(18) 0.0148(5) Uani 1 1 d . . . C33 C 0.4347(2) 0.3470(2) -0.06441(19) 0.0182(5) Uani 1 1 d . . . H33 H 0.4707 0.3518 -0.0963 0.022 Uiso 1 1 calc R . . C34 C 0.3424(2) 0.3163(2) -0.10769(19) 0.0201(6) Uani 1 1 d . . . H34 H 0.3144 0.2988 -0.1697 0.024 Uiso 1 1 calc R . . C35 C 0.2907(2) 0.3110(2) -0.06002(19) 0.0200(6) Uani 1 1 d . . . H35 H 0.2269 0.2909 -0.0887 0.024 Uiso 1 1 calc R . . C36 C 0.3348(2) 0.3361(2) 0.03049(19) 0.0178(5) Uani 1 1 d . . . H36 H 0.2997 0.3327 0.0633 0.021 Uiso 1 1 calc R . . N41 N 0.69373(16) 0.45806(18) 0.19105(16) 0.0179(5) Uani 1 1 d . . . N42 N 0.60348(16) 0.43156(17) 0.16267(16) 0.0156(4) Uani 1 1 d . . . C43 C 0.5712(2) 0.4048(2) 0.07606(19) 0.0159(5) Uani 1 1 d . . . C44 C 0.6418(2) 0.4155(2) 0.0493(2) 0.0187(5) Uani 1 1 d . . . H44 H 0.6374 0.4025 -0.0085 0.022 Uiso 1 1 calc R . . C45 C 0.7185(2) 0.4487(2) 0.1244(2) 0.0202(6) Uani 1 1 d . . . H45 H 0.7785 0.4626 0.1287 0.024 Uiso 1 1 calc R . . C46 C 0.74855(19) 0.4964(2) 0.28236(19) 0.0186(5) Uani 1 1 d . . . H46A H 0.7110 0.4908 0.3156 0.022 Uiso 1 1 calc R . . H46B H 0.7615 0.5670 0.2788 0.022 Uiso 1 1 calc R . . C51 C 0.9294(2) 0.2999(2) 0.4120(2) 0.0215(6) Uani 1 1 d . . . H51 H 0.9316 0.2334 0.4298 0.026 Uiso 1 1 calc R . . C52 C 0.84379(19) 0.3430(2) 0.3612(2) 0.0188(5) Uani 1 1 d . . . C53 C 0.84044(19) 0.4429(2) 0.33404(19) 0.0173(5) Uani 1 1 d . . . C54 C 0.9221(2) 0.4941(2) 0.35768(19) 0.0185(5) Uani 1 1 d . . . H54 H 0.9190 0.5601 0.3381 0.022 Uiso 1 1 calc R . . C55 C 1.0111(2) 0.4504(2) 0.41075(19) 0.0188(5) Uani 1 1 d . . . C56 C 1.0152(2) 0.3521(2) 0.4388(2) 0.0200(6) Uani 1 1 d . . . C61 C 1.0958(2) 0.5041(2) 0.4381(2) 0.0204(6) Uani 1 1 d . . . H61 H 1.0936 0.5701 0.4188 0.025 Uiso 1 1 calc R . . C62 C 1.1802(2) 0.4613(2) 0.4920(2) 0.0225(6) Uani 1 1 d . . . H62 H 1.2364 0.4979 0.5100 0.027 Uiso 1 1 calc R . . C63 C 1.1846(2) 0.3637(2) 0.5211(2) 0.0241(6) Uani 1 1 d . . . H63 H 1.2437 0.3351 0.5595 0.029 Uiso 1 1 calc R . . C64 C 1.1041(2) 0.3092(2) 0.4945(2) 0.0245(6) Uani 1 1 d . . . H64 H 1.1079 0.2429 0.5133 0.029 Uiso 1 1 calc R . . B11 B 0.5159(2) 0.6397(2) 0.2776(2) 0.0199(6) Uani 1 1 d . . . F12 F 0.46752(14) 0.57922(14) 0.20005(13) 0.0291(4) Uani 1 1 d . . . F13 F 0.58739(12) 0.58170(13) 0.34258(12) 0.0242(4) Uani 1 1 d . . . F14 F 0.55731(14) 0.72065(13) 0.25754(13) 0.0270(4) Uani 1 1 d . . . F15 F 0.45582(13) 0.67421(14) 0.31016(12) 0.0258(4) Uani 1 1 d . . . B21 B 0.1740(3) 0.5083(3) 0.0460(2) 0.0236(7) Uani 1 1 d . . . F22 F 0.26122(16) 0.55592(18) 0.08355(16) 0.0438(5) Uani 1 1 d . . . F23 F 0.14696(15) 0.48544(18) -0.04357(14) 0.0385(5) Uani 1 1 d . . . F24 F 0.10772(17) 0.56875(17) 0.05242(15) 0.0417(5) Uani 1 1 d . . . F25 F 0.18367(15) 0.42284(15) 0.09461(14) 0.0341(5) Uani 1 1 d . . . O11S O 0.0965(2) 0.7260(3) 0.3066(2) 0.0610(9) Uani 1 1 d . . . O12S O 0.1829(2) 0.6317(3) 0.2722(2) 0.0509(8) Uani 1 1 d . . . N13S N 0.1068(2) 0.6583(2) 0.2632(2) 0.0363(7) Uani 1 1 d . . . C14S C 0.0222(3) 0.6066(4) 0.1980(3) 0.0485(10) Uani 1 1 d . . . H14A H 0.0305 0.5868 0.1457 0.073 Uiso 1 1 calc R . . H14B H -0.0322 0.6503 0.1785 0.073 Uiso 1 1 calc R . . H14C H 0.0119 0.5481 0.2266 0.073 Uiso 1 1 calc R . . O21S O 0.1276(2) 0.2320(2) 0.2251(2) 0.0560(8) Uani 1 1 d . . . O22S O 0.1056(3) 0.3609(3) 0.2842(2) 0.0663(10) Uani 1 1 d . . . N23S N 0.0871(2) 0.3095(2) 0.2170(2) 0.0393(7) Uani 1 1 d . . . C24S C 0.0186(3) 0.3444(4) 0.1304(3) 0.0475(10) Uani 1 1 d . . . H24A H 0.0492 0.3876 0.1048 0.071 Uiso 1 1 calc R . . H24B H -0.0303 0.3810 0.1374 0.071 Uiso 1 1 calc R . . H24C H -0.0097 0.2884 0.0901 0.071 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 Cd1 0.01551(10) 0.02419(12) 0.01367(10) 0.00220(8) 0.00833(8) 0.00083(8) N11 0.0164(11) 0.0162(11) 0.0178(11) -0.0018(9) 0.0086(9) -0.0003(9) C12 0.0191(13) 0.0083(12) 0.0184(13) -0.0014(9) 0.0097(11) -0.0034(9) C13 0.0274(15) 0.0131(13) 0.0185(13) -0.0034(10) 0.0129(12) -0.0068(11) C15 0.0205(14) 0.0229(15) 0.0334(16) -0.0075(13) 0.0161(13) -0.0025(12) C14 0.0307(16) 0.0207(15) 0.0277(15) -0.0089(12) 0.0212(13) -0.0094(12) C16 0.0192(13) 0.0202(14) 0.0233(14) -0.0041(11) 0.0094(11) 0.0001(11) N21 0.0148(11) 0.0116(11) 0.0240(12) 0.0033(9) 0.0076(9) 0.0002(8) N22 0.0155(11) 0.0128(11) 0.0198(11) 0.0015(9) 0.0085(9) 0.0003(8) C23 0.0188(13) 0.0101(12) 0.0174(12) -0.0010(10) 0.0081(10) -0.0044(10) C24 0.0232(14) 0.0172(14) 0.0189(13) 0.0057(11) 0.0076(11) -0.0029(11) C25 0.0201(13) 0.0161(14) 0.0241(14) 0.0064(11) 0.0052(11) -0.0019(11) C26 0.0165(13) 0.0128(13) 0.0298(15) 0.0010(11) 0.0115(12) 0.0012(10) N31 0.0189(11) 0.0118(10) 0.0153(11) 0.0020(8) 0.0093(9) 0.0012(9) C32 0.0194(13) 0.0095(12) 0.0180(13) 0.0027(10) 0.0106(11) 0.0032(10) C33 0.0260(14) 0.0144(13) 0.0176(13) 0.0036(10) 0.0129(11) 0.0048(11) C34 0.0276(15) 0.0143(13) 0.0161(13) 0.0018(10) 0.0081(11) 0.0047(11) C35 0.0197(13) 0.0172(14) 0.0203(14) 0.0024(11) 0.0066(11) 0.0008(11) C36 0.0201(13) 0.0161(13) 0.0190(13) 0.0030(10) 0.0104(11) 0.0005(10) N41 0.0158(11) 0.0179(12) 0.0225(12) 0.0025(9) 0.0109(9) 0.0015(9) N42 0.0156(11) 0.0138(11) 0.0187(11) 0.0019(9) 0.0089(9) 0.0000(8) C43 0.0220(13) 0.0097(12) 0.0195(13) 0.0026(10) 0.0125(11) 0.0040(10) C44 0.0256(14) 0.0124(13) 0.0243(14) 0.0022(11) 0.0168(12) 0.0033(11) C45 0.0216(13) 0.0160(13) 0.0295(15) 0.0040(11) 0.0173(12) 0.0037(11) C46 0.0184(13) 0.0143(13) 0.0225(14) 0.0015(11) 0.0089(11) 0.0010(10) C51 0.0198(14) 0.0124(13) 0.0332(16) 0.0013(11) 0.0129(12) 0.0004(11) C52 0.0170(13) 0.0143(13) 0.0268(14) -0.0013(11) 0.0114(11) -0.0005(10) C53 0.0162(12) 0.0158(13) 0.0209(13) -0.0004(11) 0.0094(11) 0.0011(10) C54 0.0202(13) 0.0146(13) 0.0227(13) 0.0006(11) 0.0116(11) -0.0005(10) C55 0.0178(13) 0.0200(14) 0.0213(13) -0.0023(11) 0.0114(11) -0.0017(11) C56 0.0167(13) 0.0169(14) 0.0274(15) -0.0014(11) 0.0110(12) 0.0007(11) C61 0.0212(14) 0.0195(14) 0.0246(14) -0.0021(11) 0.0139(12) -0.0043(11) C62 0.0177(13) 0.0254(15) 0.0273(15) -0.0067(12) 0.0127(12) -0.0031(11) C63 0.0167(13) 0.0233(15) 0.0308(16) -0.0025(12) 0.0097(12) 0.0042(11) C64 0.0213(14) 0.0162(14) 0.0357(17) 0.0001(12) 0.0127(13) 0.0038(11) B11 0.0256(16) 0.0161(15) 0.0195(15) 0.0023(12) 0.0117(13) 0.0035(12) F12 0.0403(11) 0.0238(10) 0.0259(9) -0.0003(8) 0.0175(8) 0.0029(8) F13 0.0230(9) 0.0209(9) 0.0257(9) 0.0066(7) 0.0086(7) 0.0028(7) F14 0.0378(10) 0.0160(9) 0.0298(10) 0.0022(7) 0.0179(8) -0.0045(8) F15 0.0287(9) 0.0287(10) 0.0226(9) -0.0030(7) 0.0139(8) 0.0051(8) B21 0.0264(17) 0.0214(17) 0.0271(17) 0.0017(13) 0.0158(14) 0.0051(13) F22 0.0426(12) 0.0475(14) 0.0497(13) -0.0069(11) 0.0284(11) -0.0149(11) F23 0.0377(11) 0.0549(14) 0.0271(10) 0.0008(10) 0.0185(9) 0.0102(10) F24 0.0505(13) 0.0405(13) 0.0427(12) 0.0044(10) 0.0287(11) 0.0231(11) F25 0.0400(11) 0.0258(10) 0.0406(11) 0.0078(9) 0.0220(10) 0.0043(8) O11S 0.062(2) 0.060(2) 0.0500(19) -0.0170(16) 0.0160(16) 0.0121(17) O12S 0.0436(16) 0.066(2) 0.0440(16) 0.0118(15) 0.0207(14) 0.0163(15) N13S 0.0418(17) 0.0383(18) 0.0306(15) 0.0042(13) 0.0181(14) 0.0063(14) C14S 0.049(2) 0.055(3) 0.046(2) -0.009(2) 0.026(2) -0.011(2) O21S 0.0471(17) 0.0418(18) 0.062(2) 0.0013(15) 0.0097(15) 0.0117(14) O22S 0.071(2) 0.075(3) 0.0482(19) -0.0230(18) 0.0231(18) -0.010(2) N23S 0.0471(19) 0.0349(18) 0.0439(18) 0.0019(14) 0.0277(16) 0.0027(14) C24S 0.040(2) 0.053(3) 0.048(2) 0.008(2) 0.0185(19) 0.0024(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N11 2.240(2) . ? Cd1 N31 2.268(2) . ? Cd1 N42 2.283(2) . ? Cd1 N22 2.325(2) . ? Cd1 F12 2.4426(19) . ? N11 C16 1.340(4) . ? N11 C12 1.348(4) . ? C12 C13 1.388(4) . ? C12 C23 1.473(4) . ? C13 C14 1.383(4) . ? C13 H13 0.9500 . ? C15 C14 1.383(5) . ? C15 C16 1.386(4) . ? C15 H15 0.9500 . ? C14 H14 0.9500 . ? C16 H16 0.9500 . ? N21 C25 1.346(4) . ? N21 N22 1.351(3) . ? N21 C26 1.474(4) . ? N22 C23 1.342(3) . ? C23 C24 1.401(4) . ? C24 C25 1.376(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C52 1.521(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? N31 C36 1.337(4) . ? N31 C32 1.358(3) . ? C32 C33 1.386(4) . ? C32 C43 1.466(4) . ? C33 C34 1.381(4) . ? C33 H33 0.9500 . ? C34 C35 1.388(4) . ? C34 H34 0.9500 . ? C35 C36 1.385(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? N41 C45 1.348(4) . ? N41 N42 1.349(3) . ? N41 C46 1.463(4) . ? N42 C43 1.343(4) . ? C43 C44 1.401(4) . ? C44 C45 1.370(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C53 1.510(4) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C51 C52 1.371(4) . ? C51 C56 1.425(4) . ? C51 H51 0.9500 . ? C52 C53 1.427(4) . ? C53 C54 1.372(4) . ? C54 C55 1.421(4) . ? C54 H54 0.9500 . ? C55 C56 1.410(4) . ? C55 C61 1.420(4) . ? C56 C64 1.422(4) . ? C61 C62 1.366(4) . ? C61 H61 0.9500 . ? C62 C63 1.407(5) . ? C62 H62 0.9500 . ? C63 C64 1.373(4) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? B11 F15 1.387(4) . ? B11 F13 1.404(4) . ? B11 F14 1.404(4) . ? B11 F12 1.427(4) . ? B21 F25 1.386(4) . ? B21 F24 1.387(4) . ? B21 F23 1.387(4) . ? B21 F22 1.402(4) . ? O11S N13S 1.229(4) . ? O12S N13S 1.213(4) . ? N13S C14S 1.472(5) . ? C14S H14A 0.9800 . ? C14S H14B 0.9800 . ? C14S H14C 0.9800 . ? O21S N23S 1.214(4) . ? O22S N23S 1.237(5) . ? N23S C24S 1.437(5) . ? C24S H24A 0.9800 . ? C24S H24B 0.9800 . ? C24S H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Cd1 N31 128.93(8) . . ? N11 Cd1 N42 156.66(9) . . ? N31 Cd1 N42 73.20(8) . . ? N11 Cd1 N22 74.08(8) . . ? N31 Cd1 N22 140.26(8) . . ? N42 Cd1 N22 92.89(8) . . ? N11 Cd1 F12 84.51(8) . . ? N31 Cd1 F12 95.16(7) . . ? N42 Cd1 F12 86.13(7) . . ? N22 Cd1 F12 121.44(7) . . ? C16 N11 C12 119.1(2) . . ? C16 N11 Cd1 124.4(2) . . ? C12 N11 Cd1 116.50(18) . . ? N11 C12 C13 121.6(3) . . ? N11 C12 C23 117.2(2) . . ? C13 C12 C23 121.2(3) . . ? C14 C13 C12 118.8(3) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C14 C15 C16 118.4(3) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C15 C14 C13 119.7(3) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? N11 C16 C15 122.4(3) . . ? N11 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C25 N21 N22 111.2(2) . . ? C25 N21 C26 126.9(2) . . ? N22 N21 C26 121.7(2) . . ? C23 N22 N21 105.6(2) . . ? C23 N22 Cd1 112.61(18) . . ? N21 N22 Cd1 141.64(18) . . ? N22 C23 C24 110.6(2) . . ? N22 C23 C12 119.4(2) . . ? C24 C23 C12 130.0(3) . . ? C25 C24 C23 104.8(3) . . ? C25 C24 H24 127.6 . . ? C23 C24 H24 127.6 . . ? N21 C25 C24 107.8(3) . . ? N21 C25 H25 126.1 . . ? C24 C25 H25 126.1 . . ? N21 C26 C52 112.6(2) . . ? N21 C26 H26A 109.1 . . ? C52 C26 H26A 109.1 . . ? N21 C26 H26B 109.1 . . ? C52 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C36 N31 C32 118.1(2) . . ? C36 N31 Cd1 125.46(18) . . ? C32 N31 Cd1 116.40(18) . . ? N31 C32 C33 122.0(3) . . ? N31 C32 C43 116.3(2) . . ? C33 C32 C43 121.7(2) . . ? C34 C33 C32 118.9(3) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 119.6(3) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 118.1(3) . . ? C36 C35 H35 121.0 . . ? C34 C35 H35 121.0 . . ? N31 C36 C35 123.3(3) . . ? N31 C36 H36 118.4 . . ? C35 C36 H36 118.4 . . ? C45 N41 N42 111.0(2) . . ? C45 N41 C46 129.0(2) . . ? N42 N41 C46 119.8(2) . . ? C43 N42 N41 105.8(2) . . ? C43 N42 Cd1 115.07(18) . . ? N41 N42 Cd1 138.59(18) . . ? N42 C43 C44 110.2(3) . . ? N42 C43 C32 118.7(2) . . ? C44 C43 C32 131.1(3) . . ? C45 C44 C43 105.1(3) . . ? C45 C44 H44 127.5 . . ? C43 C44 H44 127.5 . . ? N41 C45 C44 107.8(2) . . ? N41 C45 H45 126.1 . . ? C44 C45 H45 126.1 . . ? N41 C46 C53 112.7(2) . . ? N41 C46 H46A 109.1 . . ? C53 C46 H46A 109.1 . . ? N41 C46 H46B 109.1 . . ? C53 C46 H46B 109.1 . . ? H46A C46 H46B 107.8 . . ? C52 C51 C56 122.0(3) . . ? C52 C51 H51 119.0 . . ? C56 C51 H51 119.0 . . ? C51 C52 C53 119.1(3) . . ? C51 C52 C26 118.9(3) . . ? C53 C52 C26 122.1(2) . . ? C54 C53 C52 120.1(3) . . ? C54 C53 C46 118.1(3) . . ? C52 C53 C46 121.8(2) . . ? C53 C54 C55 121.3(3) . . ? C53 C54 H54 119.3 . . ? C55 C54 H54 119.3 . . ? C56 C55 C61 119.4(3) . . ? C56 C55 C54 119.0(3) . . ? C61 C55 C54 121.6(3) . . ? C55 C56 C64 119.1(3) . . ? C55 C56 C51 118.5(3) . . ? C64 C56 C51 122.4(3) . . ? C62 C61 C55 120.3(3) . . ? C62 C61 H61 119.9 . . ? C55 C61 H61 119.9 . . ? C61 C62 C63 120.6(3) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 119.7 . . ? C64 C63 C62 120.5(3) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C56 120.1(3) . . ? C63 C64 H64 119.9 . . ? C56 C64 H64 119.9 . . ? F15 B11 F13 110.9(2) . . ? F15 B11 F14 108.4(3) . . ? F13 B11 F14 108.6(3) . . ? F15 B11 F12 111.3(3) . . ? F13 B11 F12 106.8(2) . . ? F14 B11 F12 110.9(2) . . ? B11 F12 Cd1 115.73(17) . . ? F25 B21 F24 109.7(3) . . ? F25 B21 F23 109.8(3) . . ? F24 B21 F23 110.1(3) . . ? F25 B21 F22 107.8(3) . . ? F24 B21 F22 109.4(3) . . ? F23 B21 F22 109.9(3) . . ? O12S N13S O11S 123.2(4) . . ? O12S N13S C14S 118.9(4) . . ? O11S N13S C14S 117.9(3) . . ? N13S C14S H14A 109.5 . . ? N13S C14S H14B 109.5 . . ? H14A C14S H14B 109.5 . . ? N13S C14S H14C 109.5 . . ? H14A C14S H14C 109.5 . . ? H14B C14S H14C 109.5 . . ? O21S N23S O22S 119.8(4) . . ? O21S N23S C24S 121.5(4) . . ? O22S N23S C24S 118.7(4) . . ? N23S C24S H24A 109.5 . . ? N23S C24S H24B 109.5 . . ? H24A C24S H24B 109.5 . . ? N23S C24S H24C 109.5 . . ? H24A C24S H24C 109.5 . . ? H24B C24S H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N31 Cd1 N11 C16 -33.9(3) . . . . ? N42 Cd1 N11 C16 125.1(3) . . . . ? N22 Cd1 N11 C16 -176.8(2) . . . . ? F12 Cd1 N11 C16 58.3(2) . . . . ? N31 Cd1 N11 C12 143.49(18) . . . . ? N42 Cd1 N11 C12 -57.5(3) . . . . ? N22 Cd1 N11 C12 0.60(19) . . . . ? F12 Cd1 N11 C12 -124.3(2) . . . . ? C16 N11 C12 C13 -0.1(4) . . . . ? Cd1 N11 C12 C13 -177.7(2) . . . . ? C16 N11 C12 C23 179.3(2) . . . . ? Cd1 N11 C12 C23 1.7(3) . . . . ? N11 C12 C13 C14 0.5(4) . . . . ? C23 C12 C13 C14 -178.9(2) . . . . ? C16 C15 C14 C13 0.1(4) . . . . ? C12 C13 C14 C15 -0.5(4) . . . . ? C12 N11 C16 C15 -0.2(4) . . . . ? Cd1 N11 C16 C15 177.1(2) . . . . ? C14 C15 C16 N11 0.3(5) . . . . ? C25 N21 N22 C23 0.4(3) . . . . ? C26 N21 N22 C23 175.9(2) . . . . ? C25 N21 N22 Cd1 176.1(2) . . . . ? C26 N21 N22 Cd1 -8.4(4) . . . . ? N11 Cd1 N22 C23 -2.99(18) . . . . ? N31 Cd1 N22 C23 -135.75(18) . . . . ? N42 Cd1 N22 C23 157.33(19) . . . . ? F12 Cd1 N22 C23 70.1(2) . . . . ? N11 Cd1 N22 N21 -178.5(3) . . . . ? N31 Cd1 N22 N21 48.7(3) . . . . ? N42 Cd1 N22 N21 -18.2(3) . . . . ? F12 Cd1 N22 N21 -105.4(3) . . . . ? N21 N22 C23 C24 0.1(3) . . . . ? Cd1 N22 C23 C24 -176.96(18) . . . . ? N21 N22 C23 C12 -177.9(2) . . . . ? Cd1 N22 C23 C12 5.0(3) . . . . ? N11 C12 C23 N22 -4.8(4) . . . . ? C13 C12 C23 N22 174.7(2) . . . . ? N11 C12 C23 C24 177.7(3) . . . . ? C13 C12 C23 C24 -2.9(4) . . . . ? N22 C23 C24 C25 -0.6(3) . . . . ? C12 C23 C24 C25 177.1(3) . . . . ? N22 N21 C25 C24 -0.8(3) . . . . ? C26 N21 C25 C24 -176.0(3) . . . . ? C23 C24 C25 N21 0.8(3) . . . . ? C25 N21 C26 C52 -66.7(4) . . . . ? N22 N21 C26 C52 118.6(3) . . . . ? N11 Cd1 N31 C36 -5.3(3) . . . . ? N42 Cd1 N31 C36 -176.8(2) . . . . ? N22 Cd1 N31 C36 109.5(2) . . . . ? F12 Cd1 N31 C36 -92.4(2) . . . . ? N11 Cd1 N31 C32 175.10(17) . . . . ? N42 Cd1 N31 C32 3.62(18) . . . . ? N22 Cd1 N31 C32 -70.1(2) . . . . ? F12 Cd1 N31 C32 88.00(19) . . . . ? C36 N31 C32 C33 -0.8(4) . . . . ? Cd1 N31 C32 C33 178.8(2) . . . . ? C36 N31 C32 C43 178.5(2) . . . . ? Cd1 N31 C32 C43 -1.9(3) . . . . ? N31 C32 C33 C34 -0.1(4) . . . . ? C43 C32 C33 C34 -179.4(2) . . . . ? C32 C33 C34 C35 0.9(4) . . . . ? C33 C34 C35 C36 -0.8(4) . . . . ? C32 N31 C36 C35 0.9(4) . . . . ? Cd1 N31 C36 C35 -178.7(2) . . . . ? C34 C35 C36 N31 -0.1(4) . . . . ? C45 N41 N42 C43 0.1(3) . . . . ? C46 N41 N42 C43 176.8(2) . . . . ? C45 N41 N42 Cd1 170.9(2) . . . . ? C46 N41 N42 Cd1 -12.4(4) . . . . ? N11 Cd1 N42 C43 -168.1(2) . . . . ? N31 Cd1 N42 C43 -5.06(18) . . . . ? N22 Cd1 N42 C43 137.04(19) . . . . ? F12 Cd1 N42 C43 -101.63(19) . . . . ? N11 Cd1 N42 N41 21.6(4) . . . . ? N31 Cd1 N42 N41 -175.3(3) . . . . ? N22 Cd1 N42 N41 -33.2(3) . . . . ? F12 Cd1 N42 N41 88.1(3) . . . . ? N41 N42 C43 C44 -0.6(3) . . . . ? Cd1 N42 C43 C44 -173.91(18) . . . . ? N41 N42 C43 C32 179.3(2) . . . . ? Cd1 N42 C43 C32 6.0(3) . . . . ? N31 C32 C43 N42 -2.8(4) . . . . ? C33 C32 C43 N42 176.5(3) . . . . ? N31 C32 C43 C44 177.1(3) . . . . ? C33 C32 C43 C44 -3.6(5) . . . . ? N42 C43 C44 C45 0.8(3) . . . . ? C32 C43 C44 C45 -179.1(3) . . . . ? N42 N41 C45 C44 0.4(3) . . . . ? C46 N41 C45 C44 -175.9(3) . . . . ? C43 C44 C45 N41 -0.7(3) . . . . ? C45 N41 C46 C53 -56.4(4) . . . . ? N42 N41 C46 C53 127.6(3) . . . . ? C56 C51 C52 C53 0.3(5) . . . . ? C56 C51 C52 C26 -179.1(3) . . . . ? N21 C26 C52 C51 101.9(3) . . . . ? N21 C26 C52 C53 -77.5(3) . . . . ? C51 C52 C53 C54 0.9(4) . . . . ? C26 C52 C53 C54 -179.7(3) . . . . ? C51 C52 C53 C46 -176.6(3) . . . . ? C26 C52 C53 C46 2.8(4) . . . . ? N41 C46 C53 C54 114.6(3) . . . . ? N41 C46 C53 C52 -67.9(3) . . . . ? C52 C53 C54 C55 -1.3(4) . . . . ? C46 C53 C54 C55 176.3(3) . . . . ? C53 C54 C55 C56 0.5(4) . . . . ? C53 C54 C55 C61 -177.7(3) . . . . ? C61 C55 C56 C64 0.4(4) . . . . ? C54 C55 C56 C64 -177.9(3) . . . . ? C61 C55 C56 C51 178.9(3) . . . . ? C54 C55 C56 C51 0.6(4) . . . . ? C52 C51 C56 C55 -1.0(5) . . . . ? C52 C51 C56 C64 177.4(3) . . . . ? C56 C55 C61 C62 -0.8(4) . . . . ? C54 C55 C61 C62 177.5(3) . . . . ? C55 C61 C62 C63 0.0(4) . . . . ? C61 C62 C63 C64 1.1(5) . . . . ? C62 C63 C64 C56 -1.5(5) . . . . ? C55 C56 C64 C63 0.7(5) . . . . ? C51 C56 C64 C63 -177.7(3) . . . . ? F15 B11 F12 Cd1 -108.6(2) . . . . ? F13 B11 F12 Cd1 12.5(3) . . . . ? F14 B11 F12 Cd1 130.6(2) . . . . ? N11 Cd1 F12 B11 60.27(19) . . . . ? N31 Cd1 F12 B11 -171.04(19) . . . . ? N42 Cd1 F12 B11 -98.32(19) . . . . ? N22 Cd1 F12 B11 -7.3(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.341 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.088 #===END data_imw1247p21c _database_code_depnum_ccdc_archive 'CCDC 708984' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C173 H158 B8 Cd4 F32 N36 O8' _chemical_formula_weight 4013.43 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.0402(7) _cell_length_b 19.5943(6) _cell_length_c 43.0372(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.863(2) _cell_angle_gamma 90.00 _cell_volume 18562.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9687 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 24.97 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8128 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6679 _exptl_absorpt_correction_T_max 0.8981 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 286472 _diffrn_reflns_av_R_equivalents 0.0899 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 24.71 _reflns_number_total 31653 _reflns_number_gt 23404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure is a [Cd4(L)6][BF4]8.5MeOH.3H2O host-guest cage. The data was solved by direct methods. Data processing was conducted to a resolution to 0.85 angstrom as the data was only complete to this resolution, higher resolution data being of very weak intensity even after long exposure to the X-ray beam. Of the expected eight BF4 anions only six have been included in the refinement. The remaining two anions could be found from the data but they were highly disordered. Attempts to split the electron density over two sites was of moderate success (after the application of harsh displacement and geometric restraints. Subsequent refinements suggested that additional splitting was required and further attempts to model the disorder resulted in a refinement with large shift that failed to stabilise. As a result the associated electron density was removed using a 'SQUEEZE' function, and thus the anions have been omitted from the refinement. The 'SQUEEZE' function was also used to remove a number of highly fluxional solvent molecules that could not be satisfactorily modelled (see SQUEEZE details below). Of the found BF4 anions the residues B21 F22 > F25 and B41 F42 > F45 display rotational disorder along the B21-F22 B41-F42 axes. The disordered fluorine atoms have been split over two sites (60:40 and 55:45 respectively). The disordered groups have been left isotropic. Global displacement restraints were applied to B and F atoms and geometric restraints have been used to improve the appearance of both ordered and disordered BF4 anions. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.369 0.002 0.357 192 121 ' ' 2 1.000 0.000 0.500 335 147 ' ' 3 0.631 -0.002 0.643 192 118 ' ' 4 0.574 0.083 0.329 7 1 ' ' 5 1.000 0.500 0.000 336 147 ' ' 6 0.369 0.498 0.857 192 119 ' ' 7 0.631 0.502 0.143 192 119 ' ' 8 0.574 0.417 0.829 7 1 ' ' 9 0.426 0.583 0.171 7 2 ' ' 10 0.426 0.917 0.671 7 2 ' ' _platon_squeeze_details ; The lattice contains five MeOH solvent molecules. All solvent MeOH molecules except for O41S C42S have had their occupancies set to 10.5 to bring their thermal parameters in line with those of the main residue. Geometric and displacement restrains were employed to improve the appearance of solvent molecules. The water molecule O1 is disordered over two sites (60:40) and has been modelled as such. The water molecules O3S and O4S have had their occupancies set to 10.5 for the same reasons as outlined above. All solvent molecules have been left isotropic due to their inherently fluxional nature. Alcohol and water protons could not be found from the data and were therefore omitted from the refinement. This results in a discrepancy of 44 protons from the UNIT instruction (when Z = 4, 20 protons from the solvent alcohol molecules and 24 from the water molecules). The final R1 value is higher than would normally be acceptable at ca 0.11. Attempts to obtain a better data were hampered by the weakly diffracting nature of the crystals at higher resolutions, presumably due to the large number of voids present in the structure and lattice and the high disorder arising from a combination of fluxional solvent molecules and counter-ions. The high concentration of solvent molecules resulted in a rapid loss of crystallinity when the crystals were removed from the mother liquor adding further complication. Given these factors we feel that the R1 value obtained for this structure is reasonable. A lower R1 value could be obtained by allowing a 'SQUEEZE' function to remove all electron density associated with the found solvent molecules (0.09). This did not form the final refinement as doing such was felt to portray a misleading view of the overall packing within the lattice. 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^)+(0.0902P)^2^+307.1890P] 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 31653 _refine_ls_number_parameters 2217 _refine_ls_number_restraints 228 _refine_ls_R_factor_all 0.1426 _refine_ls_R_factor_gt 0.1148 _refine_ls_wR_factor_ref 0.2849 _refine_ls_wR_factor_gt 0.2724 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.135 _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 Cd1 Cd 0.65222(3) 0.56716(4) 0.288653(19) 0.0311(2) Uani 1 1 d . . . Cd2 Cd 1.05584(3) 0.65881(4) 0.386150(17) 0.02738(19) Uani 1 1 d . . . Cd3 Cd 0.68561(4) 0.77733(4) 0.47829(2) 0.0391(2) Uani 1 1 d . . . Cd4 Cd 0.81944(3) 0.98839(4) 0.302583(18) 0.0296(2) Uani 1 1 d . . . N111 N 0.6360(4) 0.6006(5) 0.2375(2) 0.036(2) Uani 1 1 d . . . C112 C 0.6849(5) 0.6191(5) 0.2215(3) 0.036(3) Uani 1 1 d . . . C113 C 0.6792(6) 0.6385(6) 0.1905(3) 0.046(3) Uani 1 1 d . . . H113 H 0.7140 0.6499 0.1795 0.055 Uiso 1 1 calc R . . C114 C 0.6217(7) 0.6409(7) 0.1761(3) 0.056(4) Uani 1 1 d . . . H114 H 0.6165 0.6531 0.1547 0.067 Uiso 1 1 calc R . . C115 C 0.5716(6) 0.6253(7) 0.1932(4) 0.061(4) Uani 1 1 d . . . H115 H 0.5317 0.6287 0.1839 0.073 Uiso 1 1 calc R . . C116 C 0.5806(6) 0.6046(6) 0.2240(3) 0.049(3) Uani 1 1 d . . . H116 H 0.5465 0.5931 0.2356 0.059 Uiso 1 1 calc R . . N121 N 0.8078(4) 0.6058(4) 0.2772(2) 0.030(2) Uani 1 1 d . . . N122 N 0.7479(4) 0.6032(4) 0.2689(2) 0.0261(19) Uani 1 1 d . . . C123 C 0.7444(5) 0.6169(5) 0.2386(2) 0.030(2) Uani 1 1 d . . . C124 C 0.8011(5) 0.6314(6) 0.2282(3) 0.039(3) Uani 1 1 d . . . H124 H 0.8105 0.6440 0.2077 0.047 Uiso 1 1 calc R . . C125 C 0.8414(5) 0.6240(5) 0.2532(3) 0.035(3) Uani 1 1 d . . . H125 H 0.8842 0.6304 0.2536 0.041 Uiso 1 1 calc R . . C126 C 0.8302(5) 0.5932(6) 0.3095(2) 0.034(3) Uani 1 1 d . . . H12A H 0.7953 0.5929 0.3231 0.041 Uiso 1 1 calc R . . H12B H 0.8573 0.6312 0.3163 0.041 Uiso 1 1 calc R . . N131 N 1.0903(4) 0.6150(5) 0.4340(2) 0.033(2) Uani 1 1 d . . . C132 C 1.0563(6) 0.5703(6) 0.4479(3) 0.042(3) Uani 1 1 d . . . C133 C 1.0743(6) 0.5410(8) 0.4760(3) 0.055(4) Uani 1 1 d . . . H133 H 1.0482 0.5102 0.4859 0.066 Uiso 1 1 calc R . . C134 C 1.1298(7) 0.5564(9) 0.4894(3) 0.068(4) Uani 1 1 d . . . H134 H 1.1438 0.5351 0.5082 0.082 Uiso 1 1 calc R . . C135 C 1.1652(6) 0.6033(8) 0.4752(3) 0.057(4) Uani 1 1 d . . . H135 H 1.2033 0.6166 0.4845 0.068 Uiso 1 1 calc R . . C136 C 1.1453(5) 0.6301(7) 0.4480(3) 0.045(3) Uani 1 1 d . . . H136 H 1.1709 0.6613 0.4379 0.054 Uiso 1 1 calc R . . N141 N 0.9264(4) 0.5566(4) 0.3968(2) 0.031(2) Uani 1 1 d . . . N142 N 0.9802(4) 0.5848(4) 0.4056(2) 0.028(2) Uani 1 1 d . . . C143 C 0.9968(5) 0.5534(5) 0.4323(2) 0.034(3) Uani 1 1 d . . . C144 C 0.9541(6) 0.5053(6) 0.4400(3) 0.048(3) Uani 1 1 d . . . H144 H 0.9553 0.4765 0.4578 0.058 Uiso 1 1 calc R . . C145 C 0.9108(5) 0.5077(6) 0.4171(3) 0.037(3) Uani 1 1 d . . . H145 H 0.8754 0.4800 0.4154 0.045 Uiso 1 1 calc R . . C146 C 0.8959(5) 0.5739(6) 0.3668(2) 0.035(3) Uani 1 1 d . . . H14A H 0.9150 0.6155 0.3586 0.042 Uiso 1 1 calc R . . H14B H 0.8529 0.5848 0.3702 0.042 Uiso 1 1 calc R . . C151 C 0.8617(5) 0.4754(5) 0.2925(2) 0.029(2) Uani 1 1 d . . . H151 H 0.8385 0.4810 0.2735 0.035 Uiso 1 1 calc R . . C152 C 0.8639(4) 0.5277(5) 0.3135(3) 0.029(2) Uani 1 1 d . . . C153 C 0.8981(5) 0.5179(6) 0.3425(2) 0.033(2) Uani 1 1 d . . . C154 C 0.9296(5) 0.4586(5) 0.3482(3) 0.031(2) Uani 1 1 d . . . H154 H 0.9529 0.4536 0.3672 0.038 Uiso 1 1 calc R . . C155 C 0.9282(5) 0.4043(5) 0.3264(2) 0.031(2) Uani 1 1 d . . . C156 C 0.8929(4) 0.4128(5) 0.2981(3) 0.030(2) Uani 1 1 d . . . C161 C 0.9580(5) 0.3419(6) 0.3322(3) 0.040(3) Uani 1 1 d . . . H161 H 0.9824 0.3363 0.3509 0.048 Uiso 1 1 calc R . . C162 C 0.9525(6) 0.2891(6) 0.3115(3) 0.045(3) Uani 1 1 d . . . H162 H 0.9725 0.2469 0.3158 0.054 Uiso 1 1 calc R . . C163 C 0.9169(6) 0.2980(6) 0.2836(3) 0.046(3) Uani 1 1 d . . . H163 H 0.9132 0.2613 0.2693 0.055 Uiso 1 1 calc R . . C164 C 0.8882(4) 0.3568(6) 0.2769(3) 0.034(3) Uani 1 1 d . . . H164 H 0.8646 0.3613 0.2579 0.041 Uiso 1 1 calc R . . N211 N 0.6783(4) 0.4532(5) 0.2761(2) 0.034(2) Uani 1 1 d . . . C212 C 0.7099(5) 0.4186(5) 0.2988(2) 0.028(2) Uani 1 1 d . . . C213 C 0.7343(6) 0.3549(6) 0.2929(3) 0.046(3) Uani 1 1 d . . . H213 H 0.7583 0.3317 0.3086 0.055 Uiso 1 1 calc R . . C214 C 0.7232(7) 0.3257(6) 0.2641(3) 0.051(3) Uani 1 1 d . . . H214 H 0.7384 0.2815 0.2598 0.062 Uiso 1 1 calc R . . C215 C 0.6901(7) 0.3609(7) 0.2417(3) 0.053(3) Uani 1 1 d . . . H215 H 0.6831 0.3422 0.2214 0.063 Uiso 1 1 calc R . . C216 C 0.6673(6) 0.4234(6) 0.2489(3) 0.043(3) Uani 1 1 d . . . H216 H 0.6423 0.4465 0.2336 0.051 Uiso 1 1 calc R . . N221 N 0.7099(4) 0.5314(4) 0.3634(2) 0.0274(19) Uani 1 1 d . . . N222 N 0.6977(4) 0.5169(4) 0.3329(2) 0.0289(19) Uani 1 1 d . . . C223 C 0.7180(5) 0.4520(5) 0.3288(3) 0.031(2) Uani 1 1 d . . . C224 C 0.7420(5) 0.4261(6) 0.3573(3) 0.037(3) Uani 1 1 d . . . H224 H 0.7588 0.3822 0.3612 0.044 Uiso 1 1 calc R . . C225 C 0.7358(5) 0.4781(6) 0.3782(3) 0.035(3) Uani 1 1 d . . . H225 H 0.7478 0.4765 0.3997 0.042 Uiso 1 1 calc R . . C226 C 0.6903(5) 0.5957(5) 0.3759(3) 0.031(2) Uani 1 1 d . . . H22A H 0.6902 0.6303 0.3591 0.037 Uiso 1 1 calc R . . H22B H 0.7207 0.6104 0.3923 0.037 Uiso 1 1 calc R . . N231 N 0.6341(5) 0.8783(6) 0.4871(2) 0.047(3) Uani 1 1 d . . . C232 C 0.6020(6) 0.9057(6) 0.4630(3) 0.043(3) Uani 1 1 d . . . C233 C 0.5753(6) 0.9713(7) 0.4641(4) 0.062(4) Uani 1 1 d . . . H233 H 0.5526 0.9903 0.4468 0.075 Uiso 1 1 calc R . . C234 C 0.5850(8) 1.0075(8) 0.4934(5) 0.087(6) Uani 1 1 d . . . H234 H 0.5689 1.0521 0.4956 0.104 Uiso 1 1 calc R . . C235 C 0.6172(9) 0.9778(11) 0.5178(4) 0.086(6) Uani 1 1 d . . . H235 H 0.6230 1.0010 0.5371 0.103 Uiso 1 1 calc R . . C236 C 0.6412(7) 0.9127(7) 0.5138(3) 0.060(4) Uani 1 1 d . . . H236 H 0.6635 0.8920 0.5308 0.071 Uiso 1 1 calc R . . N241 N 0.6128(4) 0.7859(4) 0.4027(2) 0.032(2) Uani 1 1 d . . . N242 N 0.6304(4) 0.8111(5) 0.4313(2) 0.035(2) Uani 1 1 d . . . C243 C 0.5955(5) 0.8676(6) 0.4339(3) 0.040(3) Uani 1 1 d . . . C244 C 0.5581(6) 0.8759(6) 0.4080(3) 0.044(3) Uani 1 1 d . . . H244 H 0.5296 0.9117 0.4042 0.052 Uiso 1 1 calc R . . C245 C 0.5694(6) 0.8234(6) 0.3888(3) 0.045(3) Uani 1 1 d . . . H245 H 0.5499 0.8150 0.3690 0.054 Uiso 1 1 calc R . . C246 C 0.6384(5) 0.7221(5) 0.3918(3) 0.032(2) Uani 1 1 d . . . H24A H 0.6795 0.7167 0.4018 0.039 Uiso 1 1 calc R . . H24B H 0.6432 0.7262 0.3691 0.039 Uiso 1 1 calc R . . C251 C 0.5971(5) 0.5365(5) 0.3942(3) 0.033(2) Uani 1 1 d . . . H251 H 0.6138 0.4941 0.3881 0.040 Uiso 1 1 calc R . . C252 C 0.6294(5) 0.5954(5) 0.3893(2) 0.028(2) Uani 1 1 d . . . C253 C 0.6036(5) 0.6589(6) 0.3974(2) 0.031(2) Uani 1 1 d . . . C254 C 0.5480(5) 0.6613(6) 0.4108(2) 0.032(2) Uani 1 1 d . . . H254 H 0.5320 0.7040 0.4169 0.039 Uiso 1 1 calc R . . C255 C 0.5141(5) 0.6003(6) 0.4155(2) 0.033(3) Uani 1 1 d . . . C256 C 0.5403(4) 0.5366(5) 0.4080(3) 0.032(2) Uani 1 1 d . . . C261 C 0.4569(5) 0.6006(7) 0.4284(3) 0.048(3) Uani 1 1 d . . . H261 H 0.4395 0.6429 0.4341 0.057 Uiso 1 1 calc R . . C262 C 0.4255(5) 0.5410(7) 0.4331(3) 0.046(3) Uani 1 1 d . . . H262 H 0.3868 0.5422 0.4418 0.056 Uiso 1 1 calc R . . C263 C 0.4512(6) 0.4779(7) 0.4246(3) 0.055(4) Uani 1 1 d . . . H263 H 0.4293 0.4367 0.4271 0.066 Uiso 1 1 calc R . . C264 C 0.5062(5) 0.4767(6) 0.4133(3) 0.043(3) Uani 1 1 d . . . H264 H 0.5234 0.4337 0.4085 0.052 Uiso 1 1 calc R . . N311 N 0.5587(4) 0.5451(4) 0.3074(2) 0.035(2) Uani 1 1 d . . . C312 C 0.5254(4) 0.5978(6) 0.3181(3) 0.031(2) Uani 1 1 d . . . C313 C 0.4744(5) 0.5881(6) 0.3351(3) 0.036(3) Uani 1 1 d . . . H313 H 0.4525 0.6259 0.3426 0.044 Uiso 1 1 calc R . . C314 C 0.4560(6) 0.5216(6) 0.3409(3) 0.048(3) Uani 1 1 d . . . H314 H 0.4213 0.5136 0.3526 0.058 Uiso 1 1 calc R . . C315 C 0.4878(5) 0.4680(7) 0.3298(3) 0.051(3) Uani 1 1 d . . . H315 H 0.4753 0.4224 0.3332 0.061 Uiso 1 1 calc R . . C316 C 0.5391(6) 0.4820(6) 0.3132(3) 0.049(3) Uani 1 1 d . . . H316 H 0.5615 0.4446 0.3057 0.059 Uiso 1 1 calc R . . N321 N 0.6080(4) 0.6728(4) 0.3043(2) 0.0283(19) Uani 1 1 d . . . N322 N 0.6149(4) 0.7411(4) 0.2995(2) 0.032(2) Uani 1 1 d . . . C323 C 0.5644(6) 0.7745(6) 0.3051(3) 0.051(3) Uani 1 1 d . . . H323 H 0.5592 0.8226 0.3041 0.062 Uiso 1 1 calc R . . C324 C 0.5218(5) 0.7289(6) 0.3126(3) 0.044(3) Uani 1 1 d . . . H324 H 0.4809 0.7378 0.3171 0.053 Uiso 1 1 calc R . . C325 C 0.5505(4) 0.6668(5) 0.3121(3) 0.030(2) Uani 1 1 d . . . C326 C 0.6737(4) 0.7684(6) 0.2911(3) 0.033(2) Uani 1 1 d . . . H32A H 0.7055 0.7346 0.2973 0.039 Uiso 1 1 calc R . . H32B H 0.6821 0.8102 0.3035 0.039 Uiso 1 1 calc R . . N331 N 0.9178(4) 1.0178(4) 0.2892(2) 0.031(2) Uani 1 1 d . . . C332 C 0.9515(4) 0.9695(5) 0.2753(2) 0.024(2) Uani 1 1 d . . . C333 C 1.0121(5) 0.9773(6) 0.2713(2) 0.033(3) Uani 1 1 d . . . H333 H 1.0343 0.9436 0.2608 0.040 Uiso 1 1 calc R . . C334 C 1.0406(5) 1.0358(6) 0.2830(3) 0.041(3) Uani 1 1 d . . . H334 H 1.0830 1.0418 0.2812 0.049 Uiso 1 1 calc R . . C335 C 1.0070(5) 1.0854(6) 0.2974(3) 0.041(3) Uani 1 1 d . . . H335 H 1.0255 1.1260 0.3054 0.049 Uiso 1 1 calc R . . C336 C 0.9464(6) 1.0735(6) 0.2995(3) 0.039(3) Uani 1 1 d . . . H336 H 0.9229 1.1077 0.3089 0.046 Uiso 1 1 calc R . . N341 N 0.8472(4) 0.8334(4) 0.26458(19) 0.0257(18) Uani 1 1 d . . . N342 N 0.8656(4) 0.8933(4) 0.27846(19) 0.0233(18) Uani 1 1 d . . . C343 C 0.9184(4) 0.9061(5) 0.2662(2) 0.024(2) Uani 1 1 d . . . C344 C 0.9346(4) 0.8559(5) 0.2454(2) 0.027(2) Uani 1 1 d . . . H344 H 0.9704 0.8534 0.2340 0.032 Uiso 1 1 calc R . . C345 C 0.8871(4) 0.8107(5) 0.2449(2) 0.028(2) Uani 1 1 d . . . H345 H 0.8833 0.7703 0.2328 0.034 Uiso 1 1 calc R . . C346 C 0.7886(5) 0.8022(5) 0.2733(2) 0.029(2) Uani 1 1 d . . . H34A H 0.7961 0.7540 0.2792 0.035 Uiso 1 1 calc R . . H34B H 0.7744 0.8262 0.2918 0.035 Uiso 1 1 calc R . . C351 C 0.6321(5) 0.7868(6) 0.2362(3) 0.038(3) Uani 1 1 d . . . H351 H 0.5926 0.7761 0.2426 0.045 Uiso 1 1 calc R . . C352 C 0.6796(5) 0.7853(5) 0.2576(3) 0.029(2) Uani 1 1 d . . . C353 C 0.7393(4) 0.8044(5) 0.2482(2) 0.025(2) Uani 1 1 d . . . C354 C 0.7479(4) 0.8227(6) 0.2183(2) 0.030(2) Uani 1 1 d . . . H354 H 0.7873 0.8362 0.2127 0.036 Uiso 1 1 calc R . . C355 C 0.6995(5) 0.8223(6) 0.1951(3) 0.041(3) Uani 1 1 d . . . C356 C 0.6398(5) 0.8040(6) 0.2046(3) 0.036(3) Uani 1 1 d . . . C361 C 0.7078(6) 0.8407(7) 0.1642(3) 0.050(3) Uani 1 1 d . . . H361 H 0.7470 0.8531 0.1579 0.061 Uiso 1 1 calc R . . C362 C 0.6598(6) 0.8407(8) 0.1433(3) 0.064(4) Uani 1 1 d . . . H362 H 0.6661 0.8534 0.1224 0.077 Uiso 1 1 calc R . . C363 C 0.6008(6) 0.8224(8) 0.1515(3) 0.061(4) Uani 1 1 d . . . H363 H 0.5679 0.8223 0.1364 0.073 Uiso 1 1 calc R . . C364 C 0.5920(5) 0.8049(6) 0.1818(3) 0.042(3) Uani 1 1 d . . . H364 H 0.5523 0.7930 0.1876 0.051 Uiso 1 1 calc R . . N411 N 1.1322(4) 0.7361(4) 0.37960(19) 0.0279(19) Uani 1 1 d . . . C412 C 1.1285(5) 0.7971(5) 0.3946(2) 0.028(2) Uani 1 1 d . . . C413 C 1.1744(5) 0.8459(6) 0.3932(3) 0.039(3) Uani 1 1 d . . . H413 H 1.1719 0.8884 0.4037 0.046 Uiso 1 1 calc R . . C414 C 1.2236(5) 0.8302(7) 0.3760(3) 0.047(3) Uani 1 1 d . . . H414 H 1.2559 0.8621 0.3753 0.056 Uiso 1 1 calc R . . C415 C 1.2275(5) 0.7693(7) 0.3599(3) 0.048(3) Uani 1 1 d . . . H415 H 1.2609 0.7594 0.3475 0.058 Uiso 1 1 calc R . . C416 C 1.1808(5) 0.7244(7) 0.3628(3) 0.043(3) Uani 1 1 d . . . H416 H 1.1828 0.6820 0.3522 0.051 Uiso 1 1 calc R . . N421 N 0.9863(4) 0.7856(4) 0.42910(19) 0.0280(19) Uani 1 1 d . . . N422 N 1.0282(4) 0.7618(4) 0.41000(18) 0.0231(18) Uani 1 1 d . . . C423 C 1.0743(5) 0.8079(5) 0.4116(2) 0.027(2) Uani 1 1 d . . . C424 C 1.0597(5) 0.8604(5) 0.4322(3) 0.034(3) Uani 1 1 d . . . H424 H 1.0837 0.8992 0.4377 0.041 Uiso 1 1 calc R . . C425 C 1.0048(5) 0.8446(5) 0.4424(3) 0.034(2) Uani 1 1 d . . . H425 H 0.9828 0.8707 0.4567 0.040 Uiso 1 1 calc R . . C426 C 0.9294(5) 0.7481(6) 0.4329(2) 0.031(2) Uani 1 1 d . . . H42A H 0.9245 0.7130 0.4164 0.037 Uiso 1 1 calc R . . H42B H 0.8947 0.7801 0.4305 0.037 Uiso 1 1 calc R . . N431 N 0.6133(4) 0.6978(5) 0.4910(2) 0.040(2) Uani 1 1 d . . . C432 C 0.6233(5) 0.6335(6) 0.4835(3) 0.034(3) Uani 1 1 d . . . C433 C 0.5819(5) 0.5815(6) 0.4897(3) 0.036(3) Uani 1 1 d . . . H433 H 0.5907 0.5352 0.4851 0.043 Uiso 1 1 calc R . . C434 C 0.5275(5) 0.5998(6) 0.5028(3) 0.041(3) Uani 1 1 d . . . H434 H 0.4978 0.5660 0.5064 0.050 Uiso 1 1 calc R . . C435 C 0.5172(6) 0.6655(7) 0.5102(3) 0.053(3) Uani 1 1 d . . . H435 H 0.4810 0.6783 0.5198 0.063 Uiso 1 1 calc R . . C436 C 0.5614(7) 0.7150(7) 0.5035(3) 0.060(4) Uani 1 1 d . . . H436 H 0.5539 0.7616 0.5081 0.072 Uiso 1 1 calc R . . N441 N 0.7698(4) 0.6372(4) 0.4541(2) 0.029(2) Uani 1 1 d . . . N442 N 0.7196(4) 0.6675(4) 0.4638(2) 0.030(2) Uani 1 1 d . . . C443 C 0.6819(5) 0.6166(5) 0.4702(2) 0.033(3) Uani 1 1 d . . . C444 C 0.7074(5) 0.5554(6) 0.4647(2) 0.035(3) Uani 1 1 d . . . H444 H 0.6897 0.5118 0.4674 0.043 Uiso 1 1 calc R . . C445 C 0.7640(5) 0.5689(6) 0.4543(3) 0.039(3) Uani 1 1 d . . . H445 H 0.7934 0.5365 0.4485 0.046 Uiso 1 1 calc R . . C446 C 0.8233(4) 0.6773(6) 0.4462(2) 0.030(2) Uani 1 1 d . . . H44A H 0.8101 0.7246 0.4414 0.035 Uiso 1 1 calc R . . H44B H 0.8398 0.6580 0.4272 0.035 Uiso 1 1 calc R . . C451 C 0.9751(5) 0.7148(6) 0.4863(2) 0.037(3) Uani 1 1 d . . . H451 H 1.0120 0.7362 0.4813 0.044 Uiso 1 1 calc R . . C452 C 0.9283(5) 0.7135(5) 0.4648(2) 0.028(2) Uani 1 1 d . . . C453 C 0.8738(4) 0.6796(5) 0.4716(2) 0.027(2) Uani 1 1 d . . . C454 C 0.8684(5) 0.6476(6) 0.5002(3) 0.033(3) Uani 1 1 d . . . H454 H 0.8327 0.6228 0.5044 0.040 Uiso 1 1 calc R . . C455 C 0.9167(5) 0.6523(6) 0.5232(3) 0.033(2) Uani 1 1 d . . . C456 C 0.9706(5) 0.6853(6) 0.5161(3) 0.035(3) Uani 1 1 d . . . C461 C 0.9114(6) 0.6250(7) 0.5536(3) 0.051(3) Uani 1 1 d . . . H461 H 0.8758 0.6010 0.5587 0.061 Uiso 1 1 calc R . . C462 C 0.9579(6) 0.6336(7) 0.5752(3) 0.053(4) Uani 1 1 d . . . H462 H 0.9530 0.6182 0.5959 0.064 Uiso 1 1 calc R . . C463 C 1.0114(6) 0.6635(8) 0.5683(3) 0.059(4) Uani 1 1 d . . . H463 H 1.0431 0.6671 0.5840 0.071 Uiso 1 1 calc R . . C464 C 1.0203(6) 0.6887(7) 0.5389(3) 0.051(3) Uani 1 1 d . . . H464 H 1.0582 0.7077 0.5339 0.061 Uiso 1 1 calc R . . N511 N 1.0911(4) 0.5624(4) 0.35962(19) 0.0257(19) Uani 1 1 d . . . C512 C 1.0688(5) 0.5551(5) 0.3304(2) 0.028(2) Uani 1 1 d . . . C513 C 1.0730(5) 0.4949(5) 0.3146(3) 0.033(2) Uani 1 1 d . . . H513 H 1.0556 0.4905 0.2940 0.040 Uiso 1 1 calc R . . C514 C 1.1041(6) 0.4389(6) 0.3294(3) 0.041(3) Uani 1 1 d . . . H514 H 1.1080 0.3963 0.3191 0.049 Uiso 1 1 calc R . . C515 C 1.1281(5) 0.4487(5) 0.3589(3) 0.034(3) Uani 1 1 d . . . H515 H 1.1499 0.4131 0.3694 0.041 Uiso 1 1 calc R . . C516 C 1.1204(5) 0.5098(5) 0.3730(2) 0.035(3) Uani 1 1 d . . . H516 H 1.1369 0.5153 0.3936 0.042 Uiso 1 1 calc R . . N521 N 0.9954(4) 0.7132(4) 0.31389(19) 0.0275(19) Uani 1 1 d . . . N522 N 1.0186(4) 0.6657(4) 0.33369(18) 0.0233(18) Uani 1 1 d . . . C523 C 1.0377(5) 0.6142(5) 0.3154(2) 0.025(2) Uani 1 1 d . . . C524 C 1.0261(5) 0.6303(5) 0.2847(2) 0.034(3) Uani 1 1 d . . . H524 H 1.0350 0.6032 0.2672 0.041 Uiso 1 1 calc R . . C525 C 0.9994(5) 0.6919(5) 0.2842(2) 0.031(2) Uani 1 1 d . . . H525 H 0.9857 0.7162 0.2661 0.038 Uiso 1 1 calc R . . C526 C 0.9697(4) 0.7752(5) 0.3257(3) 0.028(2) Uani 1 1 d . . . H52A H 0.9525 0.7651 0.3460 0.033 Uiso 1 1 calc R . . H52B H 0.9359 0.7899 0.3113 0.033 Uiso 1 1 calc R . . N531 N 0.7930(4) 1.0878(4) 0.3271(2) 0.032(2) Uani 1 1 d . . . C532 C 0.8121(4) 1.0946(5) 0.3578(2) 0.027(2) Uani 1 1 d . . . C533 C 0.7930(5) 1.1496(6) 0.3752(3) 0.040(3) Uani 1 1 d . . . H533 H 0.8076 1.1557 0.3962 0.048 Uiso 1 1 calc R . . C534 C 0.7508(6) 1.1969(6) 0.3609(3) 0.046(3) Uani 1 1 d . . . H534 H 0.7358 1.2343 0.3723 0.055 Uiso 1 1 calc R . . C535 C 0.7331(5) 1.1871(5) 0.3313(3) 0.038(3) Uani 1 1 d . . . H535 H 0.7045 1.2174 0.3216 0.045 Uiso 1 1 calc R . . C536 C 0.7558(5) 1.1331(6) 0.3144(3) 0.039(3) Uani 1 1 d . . . H536 H 0.7440 1.1291 0.2929 0.047 Uiso 1 1 calc R . . N541 N 0.9063(4) 0.9516(4) 0.3713(2) 0.0282(19) Uani 1 1 d . . . N542 N 0.8661(4) 0.9873(4) 0.3538(2) 0.0276(19) Uani 1 1 d . . . C543 C 0.8542(5) 1.0432(5) 0.3709(2) 0.029(2) Uani 1 1 d . . . C544 C 0.8879(5) 1.0428(6) 0.3990(3) 0.037(3) Uani 1 1 d . . . H544 H 0.8882 1.0761 0.4151 0.045 Uiso 1 1 calc R . . C545 C 0.9197(5) 0.9853(6) 0.3982(3) 0.039(3) Uani 1 1 d . . . H545 H 0.9478 0.9700 0.4143 0.047 Uiso 1 1 calc R . . C546 C 0.9312(5) 0.8885(5) 0.3605(2) 0.031(2) Uani 1 1 d . . . H54A H 0.9029 0.8697 0.3441 0.037 Uiso 1 1 calc R . . H54B H 0.9329 0.8556 0.3780 0.037 Uiso 1 1 calc R . . C551 C 1.0695(5) 0.8338(5) 0.3181(2) 0.028(2) Uani 1 1 d . . . H551 H 1.0820 0.7954 0.3066 0.033 Uiso 1 1 calc R . . C552 C 1.0135(5) 0.8331(5) 0.3300(2) 0.026(2) Uani 1 1 d . . . C553 C 0.9943(5) 0.8925(5) 0.3475(2) 0.028(2) Uani 1 1 d . . . C554 C 1.0324(5) 0.9451(5) 0.3528(3) 0.032(2) Uani 1 1 d . . . H554 H 1.0196 0.9823 0.3650 0.039 Uiso 1 1 calc R . . C555 C 1.0914(5) 0.9471(5) 0.3406(2) 0.032(2) Uani 1 1 d . . . C556 C 1.1104(5) 0.8904(5) 0.3223(2) 0.033(2) Uani 1 1 d . . . C561 C 1.1312(6) 1.0018(6) 0.3462(3) 0.041(3) Uani 1 1 d . . . H561 H 1.1199 1.0386 0.3590 0.050 Uiso 1 1 calc R . . C562 C 1.1864(5) 1.0021(6) 0.3331(3) 0.043(3) Uani 1 1 d . . . H562 H 1.2131 1.0395 0.3371 0.051 Uiso 1 1 calc R . . C563 C 1.2046(6) 0.9489(6) 0.3142(3) 0.046(3) Uani 1 1 d . . . H563 H 1.2424 0.9512 0.3046 0.055 Uiso 1 1 calc R . . C564 C 1.1671(5) 0.8930(6) 0.3095(3) 0.036(3) Uani 1 1 d . . . H564 H 1.1803 0.8558 0.2973 0.044 Uiso 1 1 calc R . . N611 N 0.7421(5) 0.7698(5) 0.5256(2) 0.047(3) Uani 1 1 d . . . C612 C 0.7971(6) 0.8015(6) 0.5271(3) 0.046(3) Uani 1 1 d . . . C613 C 0.8363(7) 0.7958(7) 0.5533(3) 0.059(4) Uani 1 1 d . . . H613 H 0.8734 0.8205 0.5546 0.071 Uiso 1 1 calc R . . C614 C 0.8210(8) 0.7548(9) 0.5770(3) 0.078(5) Uani 1 1 d . . . H614 H 0.8478 0.7495 0.5948 0.093 Uiso 1 1 calc R . . C615 C 0.7655(9) 0.7205(9) 0.5751(4) 0.081(5) Uani 1 1 d . . . H615 H 0.7538 0.6918 0.5916 0.097 Uiso 1 1 calc R . . C616 C 0.7277(8) 0.7290(9) 0.5488(3) 0.079(5) Uani 1 1 d . . . H616 H 0.6903 0.7049 0.5473 0.095 Uiso 1 1 calc R . . N621 N 0.8013(4) 0.8862(4) 0.4546(2) 0.031(2) Uani 1 1 d . . . N622 N 0.7751(4) 0.8419(5) 0.4744(2) 0.037(2) Uani 1 1 d . . . C623 C 0.8122(5) 0.8426(6) 0.5002(3) 0.037(3) Uani 1 1 d . . . C624 C 0.8590(6) 0.8894(6) 0.4968(3) 0.042(3) Uani 1 1 d . . . H624 H 0.8902 0.9014 0.5119 0.050 Uiso 1 1 calc R . . C625 C 0.8509(6) 0.9137(6) 0.4682(3) 0.046(3) Uani 1 1 d . . . H625 H 0.8766 0.9459 0.4588 0.055 Uiso 1 1 calc R . . C626 C 0.7735(5) 0.8985(5) 0.4245(3) 0.037(3) Uani 1 1 d . . . H62A H 0.7468 0.8593 0.4189 0.044 Uiso 1 1 calc R . . H62B H 0.8058 0.8999 0.4093 0.044 Uiso 1 1 calc R . . N631 N 0.7622(4) 0.9940(4) 0.2566(2) 0.0284(19) Uani 1 1 d . . . C632 C 0.7019(5) 0.9800(5) 0.2575(2) 0.033(2) Uani 1 1 d . . . C633 C 0.6647(6) 0.9796(7) 0.2308(3) 0.047(3) Uani 1 1 d . . . H633 H 0.6225 0.9709 0.2318 0.057 Uiso 1 1 calc R . . C634 C 0.6896(5) 0.9919(7) 0.2023(3) 0.044(3) Uani 1 1 d . . . H634 H 0.6646 0.9916 0.1837 0.053 Uiso 1 1 calc R . . C635 C 0.7517(6) 1.0047(6) 0.2013(3) 0.045(3) Uani 1 1 d . . . H635 H 0.7703 1.0126 0.1821 0.054 Uiso 1 1 calc R . . C636 C 0.7846(5) 1.0054(6) 0.2291(3) 0.037(3) Uani 1 1 d . . . H636 H 0.8268 1.0149 0.2286 0.045 Uiso 1 1 calc R . . N641 N 0.6842(4) 0.9406(5) 0.3365(2) 0.038(2) Uani 1 1 d . . . N642 N 0.7176(4) 0.9517(4) 0.31220(19) 0.0282(19) Uani 1 1 d . . . C643 C 0.6790(4) 0.9649(5) 0.2883(3) 0.029(2) Uani 1 1 d . . . C644 C 0.6194(6) 0.9587(6) 0.2971(3) 0.042(3) Uani 1 1 d . . . H644 H 0.5835 0.9633 0.2841 0.051 Uiso 1 1 calc R . . C645 C 0.6233(5) 0.9446(6) 0.3280(3) 0.043(3) Uani 1 1 d . . . H645 H 0.5904 0.9387 0.3412 0.052 Uiso 1 1 calc R . . C646 C 0.7108(6) 0.9226(6) 0.3668(2) 0.036(3) Uani 1 1 d . . . H64A H 0.7541 0.9115 0.3646 0.044 Uiso 1 1 calc R . . H64B H 0.6905 0.8809 0.3741 0.044 Uiso 1 1 calc R . . C651 C 0.7330(5) 1.0092(5) 0.4447(3) 0.038(3) Uani 1 1 d . . . H651 H 0.7536 1.0001 0.4642 0.046 Uiso 1 1 calc R . . C652 C 0.7364(5) 0.9633(5) 0.4210(3) 0.033(3) Uani 1 1 d . . . C653 C 0.7064(5) 0.9776(5) 0.3915(3) 0.034(3) Uani 1 1 d . . . C654 C 0.6753(5) 1.0358(6) 0.3872(3) 0.040(3) Uani 1 1 d . . . H654 H 0.6567 1.0451 0.3673 0.048 Uiso 1 1 calc R . . C655 C 0.6692(6) 1.0841(6) 0.4114(3) 0.042(3) Uani 1 1 d . . . C656 C 0.6990(5) 1.0705(6) 0.4406(3) 0.043(3) Uani 1 1 d . . . C661 C 0.6355(6) 1.1458(6) 0.4070(4) 0.053(3) Uani 1 1 d . . . H661 H 0.6151 1.1556 0.3876 0.063 Uiso 1 1 calc R . . C662 C 0.6332(8) 1.1900(7) 0.4309(4) 0.072(5) Uani 1 1 d . . . H662 H 0.6114 1.2314 0.4278 0.086 Uiso 1 1 calc R . . C663 C 0.6615(7) 1.1773(7) 0.4602(4) 0.063(4) Uani 1 1 d . . . H663 H 0.6579 1.2093 0.4766 0.075 Uiso 1 1 calc R . . C664 C 0.6934(8) 1.1204(6) 0.4650(4) 0.069(5) Uani 1 1 d . . . H664 H 0.7129 1.1124 0.4849 0.083 Uiso 1 1 calc R . . B11 B 0.1961(7) 0.2475(7) 0.6390(4) 0.0456(9) Uani 1 1 d U . . F12 F 0.2220(3) 0.2372(3) 0.61085(16) 0.0458(11) Uani 1 1 d U . . F13 F 0.2327(3) 0.2908(3) 0.65762(16) 0.0460(11) Uani 1 1 d U . . F14 F 0.1384(3) 0.2746(3) 0.63440(16) 0.0468(11) Uani 1 1 d U . . F15 F 0.1915(3) 0.1843(3) 0.65426(16) 0.0455(11) Uani 1 1 d U . . B21 B 0.1206(2) 0.2761(3) 0.83703(16) 0.0647(15) Uiso 1 1 d DU . . F22 F 0.0953(3) 0.2897(3) 0.80742(17) 0.0609(15) Uiso 1 1 d DU A . F23X F 0.0742(4) 0.2704(7) 0.85764(17) 0.0675(18) Uiso 0.591(14) 1 d PDU A 1 F24X F 0.1596(5) 0.3290(5) 0.8461(2) 0.0646(18) Uiso 0.591(14) 1 d PDU A 1 F25X F 0.1528(6) 0.2150(5) 0.8362(2) 0.0655(18) Uiso 0.591(14) 1 d PDU A 1 F23Y F 0.0838(6) 0.3044(9) 0.85899(17) 0.0669(18) Uiso 0.409(14) 1 d PDU A 2 F24Y F 0.1783(5) 0.3051(9) 0.8399(2) 0.0645(18) Uiso 0.409(14) 1 d PDU A 2 F25Y F 0.1246(8) 0.2058(4) 0.8412(2) 0.0659(18) Uiso 0.409(14) 1 d PDU A 2 B31 B 0.1939(9) 0.6506(10) 0.5692(5) 0.0697(12) Uani 1 1 d U . . F32 F 0.2064(4) 0.5853(4) 0.5577(2) 0.0699(13) Uani 1 1 d U . . F33 F 0.1562(4) 0.6417(4) 0.5939(2) 0.0708(13) Uani 1 1 d U . . F34 F 0.2478(4) 0.6784(4) 0.5811(2) 0.0684(13) Uani 1 1 d U . . F35 F 0.1683(4) 0.6900(4) 0.5461(2) 0.0708(13) Uani 1 1 d U . . B41 B 0.2642(3) 0.4567(4) 0.44030(13) 0.0822(18) Uiso 1 1 d DU . . F42 F 0.2778(4) 0.5250(5) 0.44590(19) 0.0839(19) Uiso 1 1 d DU B . F43X F 0.3166(4) 0.4171(5) 0.4405(6) 0.082(2) Uiso 0.46(3) 1 d PDU B 1 F44X F 0.2276(10) 0.4303(6) 0.4627(4) 0.082(2) Uiso 0.46(3) 1 d PDU B 1 F45X F 0.2338(10) 0.4477(5) 0.4115(3) 0.083(2) Uiso 0.46(3) 1 d PDU B 1 F43Y F 0.3123(5) 0.4228(5) 0.4274(5) 0.081(2) Uiso 0.54(3) 1 d PDU B 2 F44Y F 0.2139(7) 0.4496(5) 0.4197(4) 0.083(2) Uiso 0.54(3) 1 d PDU B 2 F45Y F 0.2513(10) 0.4227(5) 0.4675(2) 0.082(2) Uiso 0.54(3) 1 d PDU B 2 B51 B 0.1812(8) 0.6728(8) 0.2718(4) 0.0522(10) Uani 1 1 d U . . F52 F 0.2433(3) 0.6698(4) 0.26499(17) 0.0520(11) Uani 1 1 d U . . F53 F 0.1726(3) 0.6380(4) 0.29921(16) 0.0519(11) Uani 1 1 d U . . F54 F 0.1484(3) 0.6423(4) 0.24694(17) 0.0526(11) Uani 1 1 d U . . F55 F 0.1650(3) 0.7400(4) 0.27450(17) 0.0533(11) Uani 1 1 d U . . B61 B 0.4209(11) 0.7900(12) 0.1568(5) 0.0863(15) Uani 1 1 d U . . F62 F 0.4418(5) 0.7232(5) 0.1594(2) 0.0875(16) Uani 1 1 d U . . F63 F 0.4527(5) 0.8228(5) 0.1343(2) 0.0862(16) Uani 1 1 d U . . F64 F 0.3596(5) 0.7918(5) 0.1482(2) 0.0859(16) Uani 1 1 d U . . F65 F 0.4314(5) 0.8210(5) 0.1853(2) 0.0865(16) Uani 1 1 d U . . O11S O 0.6063(8) 0.1467(10) 0.5415(4) 0.061(5) Uiso 0.50 1 d PD . . C12S C 0.5562(11) 0.1863(14) 0.5292(7) 0.064(8) Uiso 0.50 1 d PD . . H12C H 0.5319 0.2020 0.5462 0.095 Uiso 0.50 1 calc PR . . H12D H 0.5309 0.1581 0.5149 0.095 Uiso 0.50 1 calc PR . . H12E H 0.5715 0.2258 0.5180 0.095 Uiso 0.50 1 calc PR . . O21S O 0.4758(7) 0.0529(9) 0.4140(3) 0.048(4) Uiso 0.50 1 d PD . . C22S C 0.4931(10) 0.0596(12) 0.3825(4) 0.038(5) Uiso 0.50 1 d PD . . H22C H 0.4790 0.1036 0.3742 0.058 Uiso 0.50 1 calc PR . . H22D H 0.4746 0.0226 0.3700 0.058 Uiso 0.50 1 calc PR . . H22E H 0.5374 0.0570 0.3819 0.058 Uiso 0.50 1 calc PR . . O31S O 0.0679(8) 0.0488(9) 0.4318(4) 0.055(5) Uiso 0.50 1 d PD . . C32S C 0.0509(16) 0.1015(14) 0.4101(7) 0.082(10) Uiso 0.50 1 d PD . . H32C H 0.0369 0.1415 0.4214 0.123 Uiso 0.50 1 calc PR . . H32D H 0.0181 0.0851 0.3958 0.123 Uiso 0.50 1 calc PR . . H32E H 0.0861 0.1141 0.3983 0.123 Uiso 0.50 1 calc PR . . O41S O 0.3881(4) 0.5826(4) 0.52773(19) 0.046(2) Uiso 1 1 d D . . C42S C 0.3472(5) 0.6234(6) 0.5087(3) 0.053(3) Uiso 1 1 d D . . H42C H 0.3468 0.6700 0.5169 0.080 Uiso 1 1 calc R . . H42D H 0.3062 0.6040 0.5089 0.080 Uiso 1 1 calc R . . H42E H 0.3606 0.6240 0.4873 0.080 Uiso 1 1 calc R . . O51S O 0.2961(10) 0.5833(9) 0.3749(5) 0.076(6) Uiso 0.50 1 d PD . . C52S C 0.3085(11) 0.5126(9) 0.3698(6) 0.047(6) Uiso 0.50 1 d PD . . H52C H 0.3517 0.5065 0.3664 0.071 Uiso 0.50 1 calc PR . . H52D H 0.2843 0.4965 0.3516 0.071 Uiso 0.50 1 calc PR . . H52E H 0.2978 0.4862 0.3881 0.071 Uiso 0.50 1 calc PR . . O61S O 0.3002(11) 0.7665(11) 0.4601(5) 0.085(7) Uiso 0.50 1 d PD . . C62S C 0.2994(15) 0.7142(14) 0.4370(7) 0.073(9) Uiso 0.50 1 d PD . . H62C H 0.3258 0.7273 0.4203 0.110 Uiso 0.50 1 calc PR . . H62D H 0.2578 0.7080 0.4283 0.110 Uiso 0.50 1 calc PR . . H62E H 0.3139 0.6713 0.4464 0.110 Uiso 0.50 1 calc PR . . O71S O 0.1810(8) 0.9984(9) 0.4305(4) 0.056(5) Uiso 0.50 1 d PD . . C72S C 0.2146(14) 0.9788(17) 0.4583(5) 0.075(9) Uiso 0.50 1 d PD . . H72A H 0.2289 1.0198 0.4695 0.113 Uiso 0.50 1 calc PR . . H72B H 0.2496 0.9511 0.4530 0.113 Uiso 0.50 1 calc PR . . H72C H 0.1885 0.9522 0.4715 0.113 Uiso 0.50 1 calc PR . . O81S O 0.3891(12) 0.7175(12) 0.3641(6) 0.101(8) Uiso 0.50 1 d PD . . C82S C 0.3990(16) 0.7871(13) 0.3728(8) 0.078(9) Uiso 0.50 1 d PD . . H82A H 0.3724 0.7992 0.3895 0.117 Uiso 0.50 1 calc PR . . H82B H 0.3900 0.8166 0.3548 0.117 Uiso 0.50 1 calc PR . . H82C H 0.4415 0.7933 0.3801 0.117 Uiso 0.50 1 calc PR . . O91S O 0.4361(9) 0.6526(11) 0.2586(4) 0.066(5) Uiso 0.50 1 d PD . . C92S C 0.4022(11) 0.6468(14) 0.2295(5) 0.054(7) Uiso 0.50 1 d PD . . H92A H 0.3617 0.6666 0.2314 0.081 Uiso 0.50 1 calc PR . . H92B H 0.3983 0.5986 0.2238 0.081 Uiso 0.50 1 calc PR . . H92C H 0.4234 0.6713 0.2134 0.081 Uiso 0.50 1 calc PR . . O1X O 0.4464(10) 0.1761(11) 0.4406(5) 0.090(8) Uiso 0.59(3) 1 d PU C 1 O1Y O 0.4490(12) 0.2247(14) 0.4168(6) 0.073(9) Uiso 0.41(3) 1 d PU C 2 O2S O 0.3669(4) 0.6323(5) 0.5865(2) 0.060(2) Uiso 1 1 d . . . O3S O 0.3518(7) 0.6796(8) 0.3028(4) 0.041(4) Uiso 0.50 1 d P . . O4S O 0.5269(7) 0.2913(8) 0.2569(4) 0.045(4) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0291(4) 0.0257(4) 0.0380(5) 0.0004(3) -0.0010(3) 0.0009(3) Cd2 0.0369(4) 0.0206(4) 0.0244(4) -0.0024(3) -0.0007(3) -0.0005(3) Cd3 0.0467(5) 0.0324(5) 0.0382(5) -0.0012(4) 0.0015(4) -0.0165(4) Cd4 0.0315(4) 0.0257(4) 0.0312(4) -0.0066(3) -0.0016(3) 0.0005(3) N111 0.041(5) 0.030(5) 0.035(5) -0.007(4) -0.012(4) 0.004(4) C112 0.053(7) 0.024(6) 0.030(6) -0.003(5) 0.000(5) 0.014(5) C113 0.058(8) 0.039(7) 0.039(7) -0.007(6) -0.006(6) 0.008(6) C114 0.071(10) 0.057(9) 0.039(8) -0.002(6) -0.002(7) 0.006(7) C115 0.050(8) 0.057(9) 0.072(10) 0.003(8) -0.040(8) 0.006(7) C116 0.050(8) 0.040(7) 0.057(9) -0.001(6) -0.010(6) 0.008(6) N121 0.024(4) 0.034(5) 0.032(5) -0.004(4) 0.002(4) 0.000(4) N122 0.023(4) 0.022(4) 0.033(5) -0.004(4) 0.002(4) 0.001(3) C123 0.041(6) 0.012(5) 0.035(6) -0.005(4) 0.001(5) 0.006(4) C124 0.045(7) 0.035(6) 0.039(7) -0.005(5) 0.014(6) 0.004(5) C125 0.036(6) 0.022(5) 0.046(7) -0.004(5) -0.001(5) 0.003(5) C126 0.033(6) 0.035(6) 0.033(6) -0.009(5) -0.007(5) -0.011(5) N131 0.043(5) 0.033(5) 0.024(5) 0.002(4) -0.004(4) 0.003(4) C132 0.056(8) 0.042(7) 0.026(6) 0.008(5) -0.003(5) 0.000(6) C133 0.060(9) 0.069(9) 0.034(7) 0.013(7) -0.009(6) -0.016(7) C134 0.059(9) 0.099(13) 0.045(8) 0.026(8) -0.012(7) 0.005(9) C135 0.056(8) 0.073(10) 0.039(8) 0.012(7) -0.011(6) -0.005(7) C136 0.033(6) 0.057(8) 0.044(8) -0.011(6) -0.006(5) -0.011(6) N141 0.028(5) 0.031(5) 0.035(5) -0.002(4) 0.000(4) -0.006(4) N142 0.034(5) 0.021(4) 0.031(5) -0.008(4) -0.005(4) -0.011(4) C143 0.051(7) 0.030(6) 0.021(6) -0.003(5) 0.000(5) -0.014(5) C144 0.075(9) 0.043(7) 0.027(6) 0.003(5) 0.004(6) -0.011(7) C145 0.041(6) 0.030(6) 0.042(7) -0.011(5) 0.011(5) -0.018(5) C146 0.040(6) 0.036(6) 0.028(6) -0.006(5) -0.003(5) 0.002(5) C151 0.039(6) 0.025(6) 0.024(6) -0.001(4) 0.001(4) -0.005(5) C152 0.026(5) 0.018(5) 0.044(7) -0.005(5) 0.009(5) -0.007(4) C153 0.036(6) 0.037(6) 0.024(6) -0.008(5) 0.002(5) -0.017(5) C154 0.036(6) 0.019(5) 0.040(6) 0.000(5) 0.001(5) 0.004(4) C155 0.032(6) 0.032(6) 0.028(6) -0.003(5) -0.001(5) -0.008(5) C156 0.021(5) 0.031(6) 0.039(6) -0.009(5) 0.004(4) -0.002(4) C161 0.047(7) 0.026(6) 0.047(7) -0.005(5) 0.001(6) 0.008(5) C162 0.051(7) 0.028(6) 0.057(8) -0.005(6) 0.013(6) -0.003(5) C163 0.052(7) 0.032(7) 0.054(8) -0.022(6) 0.007(6) -0.005(6) C164 0.019(5) 0.040(7) 0.043(7) -0.011(5) 0.002(5) 0.001(5) N211 0.029(5) 0.036(5) 0.037(5) -0.008(4) 0.010(4) 0.004(4) C212 0.034(6) 0.018(5) 0.033(6) -0.003(4) 0.004(5) -0.001(4) C213 0.055(8) 0.025(6) 0.060(9) 0.004(6) 0.017(6) 0.006(5) C214 0.079(10) 0.034(7) 0.043(8) -0.016(6) 0.011(7) -0.004(7) C215 0.073(9) 0.045(8) 0.040(8) -0.017(6) 0.007(7) -0.006(7) C216 0.068(8) 0.024(6) 0.034(7) -0.009(5) -0.010(6) 0.004(6) N221 0.022(4) 0.024(5) 0.036(5) -0.002(4) -0.006(4) 0.001(4) N222 0.023(4) 0.026(5) 0.038(5) 0.003(4) 0.004(4) -0.002(4) C223 0.025(5) 0.032(6) 0.036(6) 0.006(5) 0.000(4) -0.001(4) C224 0.043(6) 0.032(6) 0.035(6) 0.011(5) -0.009(5) 0.004(5) C225 0.030(6) 0.042(7) 0.033(6) 0.014(5) -0.003(5) -0.006(5) C226 0.028(5) 0.031(6) 0.034(6) -0.003(5) -0.003(5) -0.008(5) N231 0.048(6) 0.052(7) 0.042(6) -0.011(5) 0.012(5) -0.017(5) C232 0.053(7) 0.027(6) 0.050(8) -0.016(6) 0.015(6) -0.021(6) C233 0.049(8) 0.043(8) 0.097(12) -0.020(8) 0.024(8) -0.015(6) C234 0.073(11) 0.048(9) 0.143(18) -0.057(11) 0.036(12) -0.026(8) C235 0.100(14) 0.103(16) 0.055(11) -0.019(10) 0.020(10) -0.001(12) C236 0.087(11) 0.048(8) 0.045(8) -0.013(7) 0.013(7) -0.007(8) N241 0.038(5) 0.028(5) 0.030(5) -0.002(4) -0.001(4) -0.009(4) N242 0.045(6) 0.027(5) 0.033(5) 0.000(4) -0.002(4) -0.012(4) C243 0.044(7) 0.035(7) 0.042(7) -0.004(5) 0.011(6) -0.012(5) C244 0.043(7) 0.034(7) 0.054(8) -0.009(6) -0.002(6) -0.007(5) C245 0.049(7) 0.047(8) 0.037(7) 0.004(6) -0.006(6) -0.001(6) C246 0.028(5) 0.036(6) 0.034(6) -0.010(5) 0.005(5) 0.004(5) C251 0.032(6) 0.025(6) 0.044(7) 0.004(5) 0.007(5) 0.001(5) C252 0.034(6) 0.034(6) 0.016(5) -0.002(4) -0.001(4) -0.006(5) C253 0.033(6) 0.032(6) 0.026(6) 0.000(5) -0.006(4) -0.007(5) C254 0.035(6) 0.034(6) 0.028(6) -0.003(5) -0.004(5) -0.006(5) C255 0.030(6) 0.049(7) 0.019(5) 0.005(5) -0.004(4) -0.002(5) C256 0.021(5) 0.030(6) 0.043(7) 0.004(5) -0.005(5) -0.008(4) C261 0.038(7) 0.042(7) 0.064(9) 0.002(6) 0.010(6) 0.005(6) C262 0.029(6) 0.075(10) 0.034(7) 0.004(6) -0.002(5) -0.015(6) C263 0.052(8) 0.048(8) 0.065(9) 0.009(7) 0.007(7) -0.027(7) C264 0.030(6) 0.038(7) 0.062(8) 0.007(6) 0.001(6) -0.011(5) N311 0.037(5) 0.022(5) 0.045(6) 0.006(4) -0.007(4) -0.013(4) C312 0.017(5) 0.035(6) 0.039(6) -0.008(5) -0.002(4) 0.003(4) C313 0.026(6) 0.041(7) 0.041(7) 0.011(5) -0.008(5) -0.004(5) C314 0.043(7) 0.043(7) 0.058(8) 0.007(6) -0.001(6) 0.009(6) C315 0.037(7) 0.040(7) 0.076(10) 0.020(7) 0.002(6) -0.017(6) C316 0.042(7) 0.035(7) 0.070(9) 0.003(6) 0.010(6) -0.003(6) N321 0.024(4) 0.022(4) 0.039(5) 0.007(4) -0.005(4) 0.001(3) N322 0.022(4) 0.024(5) 0.049(6) -0.002(4) -0.003(4) -0.009(4) C323 0.062(9) 0.032(7) 0.061(9) -0.010(6) 0.020(7) 0.014(6) C324 0.032(6) 0.022(6) 0.078(9) -0.003(6) 0.007(6) 0.006(5) C325 0.017(5) 0.029(6) 0.043(7) -0.001(5) 0.004(4) -0.004(4) C326 0.019(5) 0.038(6) 0.041(7) -0.002(5) 0.001(4) -0.003(5) N331 0.032(5) 0.020(4) 0.043(6) 0.003(4) 0.008(4) -0.008(4) C332 0.019(5) 0.024(5) 0.027(5) 0.008(4) -0.003(4) -0.002(4) C333 0.029(6) 0.039(6) 0.032(6) 0.015(5) -0.004(5) -0.004(5) C334 0.028(6) 0.049(7) 0.045(7) 0.015(6) -0.004(5) -0.020(5) C335 0.046(7) 0.040(7) 0.034(7) 0.009(5) -0.014(5) -0.014(6) C336 0.058(8) 0.026(6) 0.032(6) 0.000(5) 0.001(5) -0.005(5) N341 0.032(5) 0.019(4) 0.025(5) 0.002(4) -0.004(4) -0.002(4) N342 0.029(4) 0.015(4) 0.026(5) -0.002(3) -0.001(4) -0.002(3) C343 0.016(5) 0.027(5) 0.029(6) 0.008(4) -0.002(4) 0.012(4) C344 0.025(5) 0.022(5) 0.032(6) 0.000(4) -0.004(4) 0.001(4) C345 0.030(5) 0.023(5) 0.031(6) -0.002(4) 0.002(5) 0.003(4) C346 0.033(6) 0.016(5) 0.036(6) -0.002(4) -0.005(5) -0.004(4) C351 0.037(6) 0.028(6) 0.048(7) -0.005(5) -0.002(5) 0.001(5) C352 0.028(5) 0.018(5) 0.041(6) -0.005(5) 0.000(5) -0.005(4) C353 0.022(5) 0.021(5) 0.033(6) -0.007(4) -0.005(4) -0.008(4) C354 0.017(5) 0.043(6) 0.030(6) -0.009(5) -0.006(4) -0.010(4) C355 0.038(6) 0.045(7) 0.042(7) -0.004(6) 0.002(5) 0.018(5) C356 0.043(6) 0.027(6) 0.038(7) -0.017(5) -0.002(5) 0.000(5) C361 0.043(7) 0.077(10) 0.030(7) -0.003(6) -0.006(5) 0.007(7) C362 0.061(9) 0.098(12) 0.031(7) -0.010(7) -0.002(6) 0.041(9) C363 0.043(8) 0.079(10) 0.060(9) -0.033(8) -0.003(6) 0.028(7) C364 0.038(6) 0.049(7) 0.040(7) -0.013(6) 0.000(5) 0.012(6) N411 0.030(5) 0.028(5) 0.025(5) 0.002(4) 0.002(4) -0.002(4) C412 0.033(6) 0.033(6) 0.016(5) 0.010(4) -0.005(4) -0.004(5) C413 0.046(7) 0.026(6) 0.043(7) 0.001(5) -0.002(5) -0.013(5) C414 0.025(6) 0.061(9) 0.053(8) 0.010(7) -0.007(5) -0.013(6) C415 0.030(6) 0.066(9) 0.051(8) 0.013(7) 0.013(5) -0.010(6) C416 0.044(7) 0.045(7) 0.038(7) -0.005(6) -0.005(5) 0.012(6) N421 0.028(4) 0.029(5) 0.027(5) -0.003(4) 0.004(4) 0.001(4) N422 0.029(4) 0.017(4) 0.024(4) -0.003(3) 0.003(3) 0.002(3) C423 0.037(6) 0.027(5) 0.018(5) 0.001(4) 0.003(4) 0.001(5) C424 0.036(6) 0.018(5) 0.048(7) -0.008(5) -0.003(5) -0.008(4) C425 0.041(6) 0.028(6) 0.031(6) -0.004(5) 0.001(5) 0.000(5) C426 0.033(6) 0.034(6) 0.026(6) 0.008(5) 0.008(4) 0.013(5) N431 0.043(6) 0.037(6) 0.041(6) -0.001(5) 0.016(5) -0.013(5) C432 0.039(6) 0.034(6) 0.029(6) 0.005(5) -0.008(5) -0.008(5) C433 0.026(5) 0.042(7) 0.038(7) 0.009(5) -0.010(5) -0.006(5) C434 0.033(6) 0.048(8) 0.042(7) 0.005(6) -0.010(5) -0.024(6) C435 0.050(8) 0.055(9) 0.054(8) -0.005(7) 0.013(6) -0.010(7) C436 0.067(9) 0.047(8) 0.067(10) -0.002(7) 0.019(8) -0.014(7) N441 0.028(5) 0.032(5) 0.027(5) 0.002(4) 0.000(4) -0.009(4) N442 0.022(4) 0.031(5) 0.036(5) 0.003(4) -0.001(4) -0.012(4) C443 0.040(6) 0.029(6) 0.027(6) 0.008(5) -0.012(5) -0.016(5) C444 0.040(6) 0.037(7) 0.029(6) 0.006(5) -0.003(5) -0.020(5) C445 0.045(7) 0.033(6) 0.038(7) 0.001(5) -0.003(5) 0.002(5) C446 0.022(5) 0.039(6) 0.027(6) 0.005(5) -0.001(4) -0.009(5) C451 0.024(5) 0.057(8) 0.030(6) 0.006(5) 0.001(5) 0.001(5) C452 0.029(5) 0.022(5) 0.034(6) -0.001(4) 0.011(5) 0.009(4) C453 0.026(5) 0.022(5) 0.034(6) 0.005(4) 0.002(4) 0.004(4) C454 0.025(5) 0.037(6) 0.037(6) 0.017(5) -0.006(5) 0.007(5) C455 0.027(5) 0.035(6) 0.037(6) 0.004(5) -0.004(5) -0.004(5) C456 0.030(6) 0.039(6) 0.035(6) 0.004(5) 0.002(5) -0.007(5) C461 0.052(8) 0.069(9) 0.031(7) 0.019(6) 0.000(6) -0.019(7) C462 0.047(8) 0.067(9) 0.046(8) 0.025(7) 0.000(6) -0.001(7) C463 0.048(8) 0.090(11) 0.037(8) 0.017(7) -0.016(6) -0.015(8) C464 0.052(8) 0.064(9) 0.035(7) 0.011(6) -0.007(6) -0.005(7) N511 0.039(5) 0.014(4) 0.024(5) -0.003(3) 0.001(4) 0.012(4) C512 0.038(6) 0.019(5) 0.027(6) 0.000(4) 0.005(5) -0.005(4) C513 0.045(6) 0.030(6) 0.026(6) 0.003(5) 0.009(5) 0.004(5) C514 0.063(8) 0.022(6) 0.036(7) -0.007(5) 0.002(6) 0.010(5) C515 0.042(6) 0.028(6) 0.034(6) 0.002(5) 0.002(5) 0.016(5) C516 0.053(7) 0.027(6) 0.024(6) 0.003(5) -0.002(5) 0.012(5) N521 0.037(5) 0.018(4) 0.027(5) 0.005(4) 0.004(4) -0.003(4) N522 0.029(4) 0.018(4) 0.022(4) -0.002(3) -0.001(3) -0.002(3) C523 0.032(5) 0.019(5) 0.025(6) -0.003(4) -0.003(4) -0.003(4) C524 0.050(7) 0.027(6) 0.026(6) -0.008(5) 0.000(5) -0.009(5) C525 0.047(6) 0.030(6) 0.017(5) 0.003(4) -0.004(5) -0.004(5) C526 0.029(5) 0.015(5) 0.040(6) 0.001(4) 0.003(5) 0.006(4) N531 0.031(5) 0.026(5) 0.039(6) -0.004(4) 0.000(4) 0.000(4) C532 0.025(5) 0.017(5) 0.039(6) -0.006(4) 0.001(4) -0.002(4) C533 0.042(7) 0.036(7) 0.043(7) -0.013(5) 0.006(5) 0.003(5) C534 0.049(7) 0.028(6) 0.062(9) -0.014(6) 0.002(6) 0.012(5) C535 0.034(6) 0.022(6) 0.057(8) -0.001(5) 0.004(5) 0.008(5) C536 0.052(7) 0.028(6) 0.037(7) -0.002(5) 0.005(5) -0.001(5) N541 0.027(4) 0.026(5) 0.031(5) 0.006(4) -0.003(4) 0.003(4) N542 0.030(5) 0.023(4) 0.030(5) 0.001(4) 0.004(4) 0.000(4) C543 0.029(5) 0.022(5) 0.036(6) -0.004(5) 0.009(5) -0.001(4) C544 0.051(7) 0.034(6) 0.027(6) -0.009(5) 0.007(5) -0.007(5) C545 0.042(7) 0.041(7) 0.033(7) 0.001(5) -0.001(5) 0.004(6) C546 0.038(6) 0.023(5) 0.030(6) 0.003(4) -0.001(5) 0.007(5) C551 0.037(6) 0.022(5) 0.023(5) 0.004(4) -0.009(4) -0.001(4) C552 0.042(6) 0.013(5) 0.023(5) 0.007(4) -0.003(4) 0.008(4) C553 0.029(5) 0.023(5) 0.031(6) 0.004(4) -0.001(4) 0.000(4) C554 0.038(6) 0.022(5) 0.037(6) -0.002(5) 0.002(5) -0.003(5) C555 0.036(6) 0.028(6) 0.032(6) 0.001(5) 0.005(5) -0.002(5) C556 0.038(6) 0.030(6) 0.029(6) 0.005(5) -0.013(5) -0.003(5) C561 0.054(7) 0.031(6) 0.039(7) 0.006(5) -0.001(6) -0.006(5) C562 0.042(7) 0.036(7) 0.050(8) 0.006(6) 0.002(6) -0.015(5) C563 0.042(7) 0.046(7) 0.051(8) 0.011(6) 0.013(6) -0.006(6) C564 0.028(6) 0.042(7) 0.039(7) 0.001(5) 0.000(5) -0.003(5) N611 0.052(6) 0.043(6) 0.045(6) 0.015(5) -0.008(5) -0.016(5) C612 0.061(8) 0.035(7) 0.041(7) -0.002(6) -0.009(6) -0.017(6) C613 0.067(9) 0.043(8) 0.064(9) 0.007(7) -0.025(7) -0.021(7) C614 0.097(13) 0.096(13) 0.037(8) 0.020(8) -0.026(8) -0.009(11) C615 0.111(14) 0.069(11) 0.058(10) 0.027(8) -0.022(10) -0.027(10) C616 0.106(13) 0.092(12) 0.038(8) 0.023(8) -0.022(8) -0.048(11) N621 0.026(5) 0.028(5) 0.038(5) 0.004(4) 0.003(4) -0.008(4) N622 0.043(5) 0.030(5) 0.037(5) -0.001(4) -0.002(4) -0.017(4) C623 0.042(6) 0.034(6) 0.035(7) -0.007(5) -0.002(5) 0.000(5) C624 0.053(7) 0.033(6) 0.038(7) -0.006(5) -0.009(6) -0.012(6) C625 0.049(7) 0.035(7) 0.054(8) -0.008(6) 0.010(6) -0.021(6) C626 0.055(7) 0.024(6) 0.032(6) -0.006(5) 0.009(5) -0.006(5) N631 0.027(4) 0.024(5) 0.034(5) -0.005(4) 0.007(4) -0.001(4) C632 0.043(6) 0.031(6) 0.023(6) 0.000(5) -0.003(5) 0.012(5) C633 0.036(6) 0.049(8) 0.056(8) -0.005(6) 0.001(6) 0.002(6) C634 0.041(7) 0.058(8) 0.033(7) -0.014(6) -0.006(5) 0.021(6) C635 0.059(8) 0.043(7) 0.033(7) 0.002(6) 0.000(6) 0.015(6) C636 0.045(7) 0.035(6) 0.034(7) 0.005(5) 0.012(5) -0.003(5) N641 0.035(5) 0.042(6) 0.038(6) -0.007(5) 0.008(4) 0.001(4) N642 0.036(5) 0.022(4) 0.027(5) 0.000(4) 0.004(4) -0.005(4) C643 0.025(5) 0.020(5) 0.042(7) -0.005(5) 0.002(5) -0.003(4) C644 0.043(7) 0.036(7) 0.047(8) -0.002(6) -0.005(6) 0.004(5) C645 0.038(7) 0.040(7) 0.053(8) -0.014(6) 0.008(6) -0.001(5) C646 0.053(7) 0.028(6) 0.029(6) 0.000(5) 0.009(5) 0.005(5) C651 0.049(7) 0.025(6) 0.040(7) -0.003(5) 0.001(5) -0.001(5) C652 0.039(6) 0.026(6) 0.035(6) -0.009(5) 0.010(5) -0.014(5) C653 0.043(6) 0.022(5) 0.038(7) -0.003(5) 0.018(5) -0.013(5) C654 0.049(7) 0.028(6) 0.043(7) 0.007(5) 0.011(6) 0.003(5) C655 0.052(7) 0.027(6) 0.049(8) 0.001(5) 0.024(6) -0.005(5) C656 0.041(7) 0.031(6) 0.058(8) -0.009(6) 0.016(6) -0.001(5) C661 0.065(9) 0.023(6) 0.070(9) -0.006(6) 0.003(7) 0.005(6) C662 0.095(12) 0.030(7) 0.092(13) 0.005(8) 0.034(10) 0.017(8) C663 0.077(10) 0.038(8) 0.073(11) -0.021(7) 0.004(8) 0.002(7) C664 0.117(14) 0.022(7) 0.071(10) -0.012(7) 0.024(9) -0.012(8) B11 0.049(2) 0.0376(19) 0.050(2) -0.0031(17) 0.0019(17) -0.0042(17) F12 0.050(2) 0.038(2) 0.049(2) -0.0035(19) 0.004(2) -0.0036(19) F13 0.050(2) 0.038(2) 0.050(2) -0.0046(19) 0.000(2) -0.0057(19) F14 0.050(2) 0.039(2) 0.052(2) -0.002(2) 0.002(2) -0.0027(19) F15 0.050(2) 0.037(2) 0.049(2) -0.0015(19) 0.001(2) -0.0046(19) B31 0.068(3) 0.065(3) 0.075(3) 0.007(2) -0.014(2) 0.003(2) F32 0.069(3) 0.064(3) 0.074(3) 0.006(3) -0.015(2) 0.002(2) F33 0.068(3) 0.067(3) 0.076(3) 0.007(3) -0.012(2) 0.003(2) F34 0.065(3) 0.064(3) 0.074(3) 0.006(3) -0.014(2) 0.002(2) F35 0.069(3) 0.066(3) 0.075(3) 0.008(3) -0.015(2) 0.004(2) B51 0.059(2) 0.049(2) 0.049(2) -0.0007(18) 0.0057(18) -0.0017(19) F52 0.057(2) 0.050(2) 0.049(2) 0.001(2) 0.007(2) -0.003(2) F53 0.059(2) 0.049(2) 0.047(2) -0.001(2) 0.006(2) -0.001(2) F54 0.059(2) 0.050(2) 0.048(2) -0.002(2) 0.005(2) -0.002(2) F55 0.060(2) 0.049(2) 0.051(2) -0.001(2) 0.004(2) 0.000(2) B61 0.096(3) 0.080(3) 0.082(3) 0.017(3) -0.010(3) -0.017(3) F62 0.098(4) 0.080(3) 0.083(3) 0.015(3) -0.011(3) -0.015(3) F63 0.094(4) 0.081(3) 0.082(3) 0.018(3) -0.009(3) -0.018(3) F64 0.094(4) 0.080(3) 0.082(3) 0.017(3) -0.010(3) -0.018(3) F65 0.097(4) 0.080(3) 0.081(3) 0.016(3) -0.011(3) -0.017(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 Cd1 N311 2.293(9) . ? Cd1 N111 2.308(9) . ? Cd1 N222 2.326(9) . ? Cd1 N211 2.374(9) . ? Cd1 N321 2.399(8) . ? Cd1 N122 2.418(8) . ? Cd2 N411 2.292(8) . ? Cd2 N131 2.325(9) . ? Cd2 N422 2.358(8) . ? Cd2 N511 2.358(7) . ? Cd2 N522 2.367(8) . ? Cd2 N142 2.393(8) . ? Cd3 N431 2.314(9) . ? Cd3 N231 2.321(11) . ? Cd3 N611 2.338(10) . ? Cd3 N622 2.356(9) . ? Cd3 N442 2.372(9) . ? Cd3 N242 2.399(9) . ? Cd4 N631 2.296(9) . ? Cd4 N531 2.304(9) . ? Cd4 N331 2.343(8) . ? Cd4 N342 2.385(8) . ? Cd4 N542 2.386(9) . ? Cd4 N642 2.413(8) . ? N111 C116 1.327(15) . ? N111 C112 1.356(15) . ? C112 C113 1.385(16) . ? C112 C123 1.473(16) . ? C113 C114 1.385(18) . ? C113 H113 0.9500 . ? C114 C115 1.39(2) . ? C114 H114 0.9500 . ? C115 C116 1.393(19) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 C125 1.350(14) . ? N121 N122 1.352(11) . ? N121 C126 1.470(14) . ? N122 C123 1.328(13) . ? C123 C124 1.379(15) . ? C124 C125 1.368(16) . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? C126 C152 1.488(15) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? N131 C132 1.317(15) . ? N131 C136 1.358(14) . ? C132 C133 1.379(16) . ? C132 C143 1.480(16) . ? C133 C134 1.360(19) . ? C133 H133 0.9500 . ? C134 C135 1.37(2) . ? C134 H134 0.9500 . ? C135 C136 1.337(18) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? N141 N142 1.345(11) . ? N141 C145 1.351(14) . ? N141 C146 1.466(14) . ? N142 C143 1.336(14) . ? C143 C144 1.385(16) . ? C144 C145 1.338(17) . ? C144 H144 0.9500 . ? C145 H145 0.9500 . ? C146 C153 1.518(14) . ? C146 H14A 0.9900 . ? C146 H14B 0.9900 . ? C151 C152 1.365(14) . ? C151 C156 1.420(15) . ? C151 H151 0.9500 . ? C152 C153 1.441(15) . ? C153 C154 1.369(15) . ? C154 C155 1.416(15) . ? C154 H154 0.9500 . ? C155 C161 1.404(15) . ? C155 C156 1.422(15) . ? C156 C164 1.429(15) . ? C161 C162 1.368(16) . ? C161 H161 0.9500 . ? C162 C163 1.412(18) . ? C162 H162 0.9500 . ? C163 C164 1.339(16) . ? C163 H163 0.9500 . ? C164 H164 0.9500 . ? N211 C216 1.322(14) . ? N211 C212 1.354(14) . ? C212 C213 1.387(15) . ? C212 C223 1.451(15) . ? C213 C214 1.379(18) . ? C213 H213 0.9500 . ? C214 C215 1.367(19) . ? C214 H214 0.9500 . ? C215 C216 1.365(17) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? N221 C225 1.337(13) . ? N221 N222 1.357(12) . ? N221 C226 1.443(13) . ? N222 C223 1.363(13) . ? C223 C224 1.403(15) . ? C224 C225 1.373(16) . ? C224 H224 0.9500 . ? C225 H225 0.9500 . ? C226 C252 1.489(14) . ? C226 H22A 0.9900 . ? C226 H22B 0.9900 . ? N231 C232 1.337(17) . ? N231 C236 1.338(16) . ? C232 C233 1.415(18) . ? C232 C243 1.460(16) . ? C233 C234 1.46(2) . ? C233 H233 0.9500 . ? C234 C235 1.37(3) . ? C234 H234 0.9500 . ? C235 C236 1.40(2) . ? C235 H235 0.9500 . ? C236 H236 0.9500 . ? N241 C245 1.325(15) . ? N241 N242 1.364(12) . ? N241 C246 1.460(13) . ? N242 C243 1.355(15) . ? C243 C244 1.361(17) . ? C244 C245 1.350(17) . ? C244 H244 0.9500 . ? C245 H245 0.9500 . ? C246 C253 1.483(15) . ? C246 H24A 0.9900 . ? C246 H24B 0.9900 . ? C251 C252 1.378(15) . ? C251 C256 1.412(14) . ? C251 H251 0.9500 . ? C252 C253 1.418(15) . ? C253 C254 1.380(15) . ? C254 C255 1.430(15) . ? C254 H254 0.9500 . ? C255 C261 1.401(16) . ? C255 C256 1.421(16) . ? C256 C264 1.418(15) . ? C261 C262 1.378(18) . ? C261 H261 0.9500 . ? C262 C263 1.414(19) . ? C262 H262 0.9500 . ? C263 C264 1.331(17) . ? C263 H263 0.9500 . ? C264 H264 0.9500 . ? N311 C316 1.338(15) . ? N311 C312 1.360(14) . ? C312 C313 1.384(15) . ? C312 C325 1.489(15) . ? C313 C314 1.391(17) . ? C313 H313 0.9500 . ? C314 C315 1.363(18) . ? C314 H314 0.9500 . ? C315 C316 1.393(17) . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? N321 C325 1.334(12) . ? N321 N322 1.363(12) . ? N322 C323 1.323(15) . ? N322 C326 1.465(12) . ? C323 C324 1.347(17) . ? C323 H323 0.9500 . ? C324 C325 1.372(15) . ? C324 H324 0.9500 . ? C326 C352 1.492(15) . ? C326 H32A 0.9900 . ? C326 H32B 0.9900 . ? N331 C336 1.324(14) . ? N331 C332 1.361(13) . ? C332 C333 1.364(14) . ? C332 C343 1.483(14) . ? C333 C334 1.389(16) . ? C333 H333 0.9500 . ? C334 C335 1.385(18) . ? C334 H334 0.9500 . ? C335 C336 1.365(16) . ? C335 H335 0.9500 . ? C336 H336 0.9500 . ? N341 C345 1.325(13) . ? N341 N342 1.370(11) . ? N341 C346 1.494(13) . ? N342 C343 1.326(12) . ? C343 C344 1.390(14) . ? C344 C345 1.371(14) . ? C344 H344 0.9500 . ? C345 H345 0.9500 . ? C346 C353 1.493(14) . ? C346 H34A 0.9900 . ? C346 H34B 0.9900 . ? C351 C352 1.359(15) . ? C351 C356 1.420(16) . ? C351 H351 0.9500 . ? C352 C353 1.445(14) . ? C353 C354 1.357(15) . ? C354 C355 1.425(15) . ? C354 H354 0.9500 . ? C355 C361 1.401(17) . ? C355 C356 1.441(16) . ? C356 C364 1.403(16) . ? C361 C362 1.355(18) . ? C361 H361 0.9500 . ? C362 C363 1.41(2) . ? C362 H362 0.9500 . ? C363 C364 1.372(19) . ? C363 H363 0.9500 . ? C364 H364 0.9500 . ? N411 C416 1.343(14) . ? N411 C412 1.363(13) . ? C412 C413 1.396(15) . ? C412 C423 1.447(14) . ? C413 C414 1.377(17) . ? C413 H413 0.9500 . ? C414 C415 1.384(19) . ? C414 H414 0.9500 . ? C415 C416 1.365(17) . ? C415 H415 0.9500 . ? C416 H416 0.9500 . ? N421 C425 1.345(13) . ? N421 N422 1.349(11) . ? N421 C426 1.472(13) . ? N422 C423 1.358(13) . ? C423 C424 1.406(14) . ? C424 C425 1.343(15) . ? C424 H424 0.9500 . ? C425 H425 0.9500 . ? C426 C452 1.532(14) . ? C426 H42A 0.9900 . ? C426 H42B 0.9900 . ? N431 C432 1.322(15) . ? N431 C436 1.332(16) . ? C432 C433 1.401(15) . ? C432 C443 1.478(16) . ? C433 C434 1.396(16) . ? C433 H433 0.9500 . ? C434 C435 1.349(18) . ? C434 H434 0.9500 . ? C435 C436 1.413(18) . ? C435 H435 0.9500 . ? C436 H436 0.9500 . ? N441 N442 1.341(12) . ? N441 C445 1.344(14) . ? N441 C446 1.469(12) . ? N442 C443 1.336(13) . ? C443 C444 1.350(16) . ? C444 C445 1.371(16) . ? C444 H444 0.9500 . ? C445 H445 0.9500 . ? C446 C453 1.519(14) . ? C446 H44A 0.9900 . ? C446 H44B 0.9900 . ? C451 C452 1.351(15) . ? C451 C456 1.414(15) . ? C451 H451 0.9500 . ? C452 C453 1.416(14) . ? C453 C454 1.395(14) . ? C454 C455 1.418(15) . ? C454 H454 0.9500 . ? C455 C456 1.401(15) . ? C455 C461 1.425(16) . ? C456 C464 1.435(16) . ? C461 C462 1.361(18) . ? C461 H461 0.9500 . ? C462 C463 1.361(18) . ? C462 H462 0.9500 . ? C463 C464 1.382(17) . ? C463 H463 0.9500 . ? C464 H464 0.9500 . ? N511 C516 1.332(13) . ? N511 C512 1.333(13) . ? C512 C513 1.369(14) . ? C512 C523 1.477(14) . ? C513 C514 1.428(15) . ? C513 H513 0.9500 . ? C514 C515 1.363(16) . ? C514 H514 0.9500 . ? C515 C516 1.357(15) . ? C515 H515 0.9500 . ? C516 H516 0.9500 . ? N521 N522 1.347(11) . ? N521 C525 1.351(13) . ? N521 C526 1.444(12) . ? N522 C523 1.360(12) . ? C523 C524 1.369(15) . ? C524 C525 1.342(15) . ? C524 H524 0.9500 . ? C525 H525 0.9500 . ? C526 C552 1.495(14) . ? C526 H52A 0.9900 . ? C526 H52B 0.9900 . ? N531 C536 1.308(14) . ? N531 C532 1.375(14) . ? C532 C533 1.390(14) . ? C532 C543 1.463(14) . ? C533 C534 1.430(17) . ? C533 H533 0.9500 . ? C534 C535 1.326(17) . ? C534 H534 0.9500 . ? C535 C536 1.392(15) . ? C535 H535 0.9500 . ? C536 H536 0.9500 . ? N541 N542 1.333(11) . ? N541 C545 1.352(14) . ? N541 C546 1.440(13) . ? N542 C543 1.351(13) . ? C543 C544 1.389(16) . ? C544 C545 1.329(16) . ? C544 H544 0.9500 . ? C545 H545 0.9500 . ? C546 C553 1.525(14) . ? C546 H54A 0.9900 . ? C546 H54B 0.9900 . ? C551 C552 1.358(14) . ? C551 C556 1.435(14) . ? C551 H551 0.9500 . ? C552 C553 1.462(14) . ? C553 C554 1.341(14) . ? C554 C555 1.427(15) . ? C554 H554 0.9500 . ? C555 C561 1.397(15) . ? C555 C556 1.437(15) . ? C556 C564 1.392(15) . ? C561 C562 1.364(17) . ? C561 H561 0.9500 . ? C562 C563 1.394(17) . ? C562 H562 0.9500 . ? C563 C564 1.381(16) . ? C563 H563 0.9500 . ? C564 H564 0.9500 . ? N611 C616 1.330(17) . ? N611 C612 1.361(15) . ? C612 C613 1.391(18) . ? C612 C623 1.463(17) . ? C613 C614 1.36(2) . ? C613 H613 0.9500 . ? C614 C615 1.40(2) . ? C614 H614 0.9500 . ? C615 C616 1.38(2) . ? C615 H615 0.9500 . ? C616 H616 0.9500 . ? N621 C625 1.328(14) . ? N621 N622 1.366(12) . ? N621 C626 1.424(14) . ? N622 C623 1.344(14) . ? C623 C624 1.393(16) . ? C624 C625 1.325(17) . ? C624 H624 0.9500 . ? C625 H625 0.9500 . ? C626 C652 1.514(16) . ? C626 H62A 0.9900 . ? C626 H62B 0.9900 . ? N631 C636 1.324(13) . ? N631 C632 1.359(14) . ? C632 C633 1.381(16) . ? C632 C643 1.469(15) . ? C633 C634 1.389(17) . ? C633 H633 0.9500 . ? C634 C635 1.394(17) . ? C634 H634 0.9500 . ? C635 C636 1.368(16) . ? C635 H635 0.9500 . ? C636 H636 0.9500 . ? N641 N642 1.326(12) . ? N641 C645 1.376(15) . ? N641 C646 1.445(14) . ? N642 C643 1.328(13) . ? C643 C644 1.390(15) . ? C644 C645 1.359(17) . ? C644 H644 0.9500 . ? C645 H645 0.9500 . ? C646 C653 1.521(14) . ? C646 H64A 0.9900 . ? C646 H64B 0.9900 . ? C651 C652 1.367(15) . ? C651 C656 1.422(16) . ? C651 H651 0.9500 . ? C652 C653 1.428(16) . ? C653 C654 1.338(16) . ? C654 C655 1.418(16) . ? C654 H654 0.9500 . ? C655 C656 1.414(18) . ? C655 C661 1.426(17) . ? C656 C664 1.444(18) . ? C661 C662 1.35(2) . ? C661 H661 0.9500 . ? C662 C663 1.40(2) . ? C662 H662 0.9500 . ? C663 C664 1.33(2) . ? C663 H663 0.9500 . ? C664 H664 0.9500 . ? B11 F12 1.380(16) . ? B11 F14 1.382(16) . ? B11 F13 1.396(16) . ? B11 F15 1.408(16) . ? B21 F25Y 1.390(5) . ? B21 F24X 1.390(5) . ? B21 F23X 1.391(5) . ? B21 F22 1.392(5) . ? B21 F24Y 1.392(5) . ? B21 F23Y 1.392(5) . ? B21 F25X 1.393(5) . ? B31 F35 1.36(2) . ? B31 F34 1.38(2) . ? B31 F33 1.39(2) . ? B31 F32 1.40(2) . ? B41 F43Y 1.389(5) . ? B41 F45X 1.389(5) . ? B41 F45Y 1.390(5) . ? B41 F44X 1.390(5) . ? B41 F42 1.390(5) . ? B41 F44Y 1.391(5) . ? B41 F43X 1.391(5) . ? B51 F55 1.370(18) . ? B51 F53 1.383(17) . ? B51 F54 1.395(18) . ? B51 F52 1.417(17) . ? B61 F65 1.38(2) . ? B61 F64 1.38(2) . ? B61 F63 1.38(2) . ? B61 F62 1.39(3) . ? O11S C12S 1.429(2) . ? C12S H12C 0.9800 . ? C12S H12D 0.9800 . ? C12S H12E 0.9800 . ? O21S C22S 1.430(2) . ? C22S H22C 0.9800 . ? C22S H22D 0.9800 . ? C22S H22E 0.9800 . ? O31S C32S 1.430(2) . ? C32S H32C 0.9800 . ? C32S H32D 0.9800 . ? C32S H32E 0.9800 . ? O41S C42S 1.430(2) . ? C42S H42C 0.9800 . ? C42S H42D 0.9800 . ? C42S H42E 0.9800 . ? O51S C52S 1.430(2) . ? C52S H52C 0.9800 . ? C52S H52D 0.9800 . ? C52S H52E 0.9800 . ? O61S C62S 1.430(2) . ? C62S H62C 0.9800 . ? C62S H62D 0.9800 . ? C62S H62E 0.9800 . ? O71S C72S 1.430(2) . ? C72S H72A 0.9800 . ? C72S H72B 0.9800 . ? C72S H72C 0.9800 . ? O81S C82S 1.429(2) . ? C82S H82A 0.9800 . ? C82S H82B 0.9800 . ? C82S H82C 0.9800 . ? O91S C92S 1.429(2) . ? C92S H92A 0.9800 . ? C92S H92B 0.9800 . ? C92S H92C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N311 Cd1 N111 106.9(3) . . ? N311 Cd1 N222 89.5(3) . . ? N111 Cd1 N222 160.2(3) . . ? N311 Cd1 N211 97.7(3) . . ? N111 Cd1 N211 94.4(3) . . ? N222 Cd1 N211 71.9(3) . . ? N311 Cd1 N321 71.3(3) . . ? N111 Cd1 N321 88.6(3) . . ? N222 Cd1 N321 107.5(3) . . ? N211 Cd1 N321 169.0(3) . . ? N311 Cd1 N122 173.9(3) . . ? N111 Cd1 N122 71.2(3) . . ? N222 Cd1 N122 93.7(3) . . ? N211 Cd1 N122 88.3(3) . . ? N321 Cd1 N122 102.7(3) . . ? N411 Cd2 N131 98.2(3) . . ? N411 Cd2 N422 72.2(3) . . ? N131 Cd2 N422 90.6(3) . . ? N411 Cd2 N511 102.0(3) . . ? N131 Cd2 N511 91.9(3) . . ? N422 Cd2 N511 174.1(3) . . ? N411 Cd2 N522 93.8(3) . . ? N131 Cd2 N522 161.6(3) . . ? N422 Cd2 N522 106.4(3) . . ? N511 Cd2 N522 72.0(3) . . ? N411 Cd2 N142 166.5(3) . . ? N131 Cd2 N142 70.6(3) . . ? N422 Cd2 N142 99.6(3) . . ? N511 Cd2 N142 86.3(3) . . ? N522 Cd2 N142 98.9(3) . . ? N431 Cd3 N231 100.8(3) . . ? N431 Cd3 N611 95.4(3) . . ? N231 Cd3 N611 99.0(4) . . ? N431 Cd3 N622 165.3(4) . . ? N231 Cd3 N622 88.4(3) . . ? N611 Cd3 N622 71.6(3) . . ? N431 Cd3 N442 71.4(3) . . ? N231 Cd3 N442 168.4(3) . . ? N611 Cd3 N442 90.5(3) . . ? N622 Cd3 N442 101.1(3) . . ? N431 Cd3 N242 93.4(3) . . ? N231 Cd3 N242 70.7(4) . . ? N611 Cd3 N242 167.6(3) . . ? N622 Cd3 N242 100.6(3) . . ? N442 Cd3 N242 100.6(3) . . ? N631 Cd4 N531 102.3(3) . . ? N631 Cd4 N331 104.6(3) . . ? N531 Cd4 N331 99.4(3) . . ? N631 Cd4 N342 83.7(3) . . ? N531 Cd4 N342 169.4(3) . . ? N331 Cd4 N342 70.4(3) . . ? N631 Cd4 N542 171.9(3) . . ? N531 Cd4 N542 72.1(3) . . ? N331 Cd4 N542 82.4(3) . . ? N342 Cd4 N542 102.8(3) . . ? N631 Cd4 N642 71.7(3) . . ? N531 Cd4 N642 85.1(3) . . ? N331 Cd4 N642 174.8(3) . . ? N342 Cd4 N642 105.2(3) . . ? N542 Cd4 N642 101.6(3) . . ? C116 N111 C112 120.0(11) . . ? C116 N111 Cd1 121.9(9) . . ? C112 N111 Cd1 118.1(7) . . ? N111 C112 C113 121.7(11) . . ? N111 C112 C123 116.7(10) . . ? C113 C112 C123 121.6(11) . . ? C114 C113 C112 118.6(13) . . ? C114 C113 H113 120.7 . . ? C112 C113 H113 120.7 . . ? C113 C114 C115 119.1(13) . . ? C113 C114 H114 120.4 . . ? C115 C114 H114 120.4 . . ? C114 C115 C116 119.3(12) . . ? C114 C115 H115 120.3 . . ? C116 C115 H115 120.3 . . ? N111 C116 C115 121.2(13) . . ? N111 C116 H116 119.4 . . ? C115 C116 H116 119.4 . . ? C125 N121 N122 111.9(9) . . ? C125 N121 C126 126.5(9) . . ? N122 N121 C126 121.5(8) . . ? C123 N122 N121 105.2(8) . . ? C123 N122 Cd1 113.3(7) . . ? N121 N122 Cd1 140.7(7) . . ? N122 C123 C124 110.5(10) . . ? N122 C123 C112 120.2(10) . . ? C124 C123 C112 129.2(11) . . ? C125 C124 C123 106.7(10) . . ? C125 C124 H124 126.6 . . ? C123 C124 H124 126.6 . . ? N121 C125 C124 105.7(10) . . ? N121 C125 H125 127.2 . . ? C124 C125 H125 127.2 . . ? N121 C126 C152 113.3(9) . . ? N121 C126 H12A 108.9 . . ? C152 C126 H12A 108.9 . . ? N121 C126 H12B 108.9 . . ? C152 C126 H12B 108.9 . . ? H12A C126 H12B 107.7 . . ? C132 N131 C136 117.5(10) . . ? C132 N131 Cd2 118.6(7) . . ? C136 N131 Cd2 123.8(8) . . ? N131 C132 C133 121.9(12) . . ? N131 C132 C143 117.0(10) . . ? C133 C132 C143 121.0(11) . . ? C134 C133 C132 119.5(13) . . ? C134 C133 H133 120.3 . . ? C132 C133 H133 120.3 . . ? C133 C134 C135 118.7(13) . . ? C133 C134 H134 120.6 . . ? C135 C134 H134 120.6 . . ? C136 C135 C134 119.1(13) . . ? C136 C135 H135 120.4 . . ? C134 C135 H135 120.4 . . ? C135 C136 N131 123.1(12) . . ? C135 C136 H136 118.4 . . ? N131 C136 H136 118.4 . . ? N142 N141 C145 111.0(9) . . ? N142 N141 C146 120.8(9) . . ? C145 N141 C146 127.7(9) . . ? C143 N142 N141 104.6(8) . . ? C143 N142 Cd2 114.5(7) . . ? N141 N142 Cd2 140.4(7) . . ? N142 C143 C144 111.1(10) . . ? N142 C143 C132 119.1(9) . . ? C144 C143 C132 129.8(11) . . ? C145 C144 C143 105.5(11) . . ? C145 C144 H144 127.3 . . ? C143 C144 H144 127.3 . . ? C144 C145 N141 107.8(10) . . ? C144 C145 H145 126.1 . . ? N141 C145 H145 126.1 . . ? N141 C146 C153 114.3(9) . . ? N141 C146 H14A 108.7 . . ? C153 C146 H14A 108.7 . . ? N141 C146 H14B 108.7 . . ? C153 C146 H14B 108.7 . . ? H14A C146 H14B 107.6 . . ? C152 C151 C156 122.4(10) . . ? C152 C151 H151 118.8 . . ? C156 C151 H151 118.8 . . ? C151 C152 C153 118.2(10) . . ? C151 C152 C126 124.8(10) . . ? C153 C152 C126 116.9(9) . . ? C154 C153 C152 120.4(10) . . ? C154 C153 C146 121.7(10) . . ? C152 C153 C146 117.9(10) . . ? C153 C154 C155 121.8(10) . . ? C153 C154 H154 119.1 . . ? C155 C154 H154 119.1 . . ? C161 C155 C154 122.8(10) . . ? C161 C155 C156 119.1(10) . . ? C154 C155 C156 118.1(10) . . ? C151 C156 C155 119.1(9) . . ? C151 C156 C164 122.4(10) . . ? C155 C156 C164 118.5(10) . . ? C162 C161 C155 121.1(11) . . ? C162 C161 H161 119.4 . . ? C155 C161 H161 119.4 . . ? C161 C162 C163 119.2(11) . . ? C161 C162 H162 120.4 . . ? C163 C162 H162 120.4 . . ? C164 C163 C162 121.9(11) . . ? C164 C163 H163 119.1 . . ? C162 C163 H163 119.1 . . ? C163 C164 C156 120.2(11) . . ? C163 C164 H164 119.9 . . ? C156 C164 H164 119.9 . . ? C216 N211 C212 118.9(9) . . ? C216 N211 Cd1 125.6(8) . . ? C212 N211 Cd1 115.4(7) . . ? N211 C212 C213 120.7(10) . . ? N211 C212 C223 116.9(9) . . ? C213 C212 C223 122.4(11) . . ? C214 C213 C212 118.9(12) . . ? C214 C213 H213 120.5 . . ? C212 C213 H213 120.5 . . ? C215 C214 C213 119.4(12) . . ? C215 C214 H214 120.3 . . ? C213 C214 H214 120.3 . . ? C216 C215 C214 118.8(12) . . ? C216 C215 H215 120.6 . . ? C214 C215 H215 120.6 . . ? N211 C216 C215 123.0(12) . . ? N211 C216 H216 118.5 . . ? C215 C216 H216 118.5 . . ? C225 N221 N222 110.9(9) . . ? C225 N221 C226 129.2(9) . . ? N222 N221 C226 119.7(8) . . ? N221 N222 C223 105.7(8) . . ? N221 N222 Cd1 139.4(6) . . ? C223 N222 Cd1 114.9(7) . . ? N222 C223 C224 109.6(10) . . ? N222 C223 C212 120.6(9) . . ? C224 C223 C212 129.7(10) . . ? C225 C224 C223 105.1(10) . . ? C225 C224 H224 127.4 . . ? C223 C224 H224 127.4 . . ? N221 C225 C224 108.7(10) . . ? N221 C225 H225 125.7 . . ? C224 C225 H225 125.7 . . ? N221 C226 C252 115.6(8) . . ? N221 C226 H22A 108.4 . . ? C252 C226 H22A 108.4 . . ? N221 C226 H22B 108.4 . . ? C252 C226 H22B 108.4 . . ? H22A C226 H22B 107.4 . . ? C232 N231 C236 120.0(12) . . ? C232 N231 Cd3 117.4(8) . . ? C236 N231 Cd3 122.2(10) . . ? N231 C232 C233 123.0(12) . . ? N231 C232 C243 119.0(11) . . ? C233 C232 C243 117.9(13) . . ? C232 C233 C234 115.3(16) . . ? C232 C233 H233 122.3 . . ? C234 C233 H233 122.3 . . ? C235 C234 C233 120.5(16) . . ? C235 C234 H234 119.8 . . ? C233 C234 H234 119.8 . . ? C234 C235 C236 118.7(16) . . ? C234 C235 H235 120.7 . . ? C236 C235 H235 120.7 . . ? N231 C236 C235 122.6(16) . . ? N231 C236 H236 118.7 . . ? C235 C236 H236 118.7 . . ? C245 N241 N242 112.0(9) . . ? C245 N241 C246 127.7(10) . . ? N242 N241 C246 120.2(9) . . ? C243 N242 N241 103.3(9) . . ? C243 N242 Cd3 115.0(7) . . ? N241 N242 Cd3 140.4(7) . . ? N242 C243 C244 110.8(10) . . ? N242 C243 C232 117.0(11) . . ? C244 C243 C232 132.1(12) . . ? C245 C244 C243 106.7(12) . . ? C245 C244 H244 126.7 . . ? C243 C244 H244 126.7 . . ? N241 C245 C244 107.2(11) . . ? N241 C245 H245 126.4 . . ? C244 C245 H245 126.4 . . ? N241 C246 C253 116.9(9) . . ? N241 C246 H24A 108.1 . . ? C253 C246 H24A 108.1 . . ? N241 C246 H24B 108.1 . . ? C253 C246 H24B 108.1 . . ? H24A C246 H24B 107.3 . . ? C252 C251 C256 122.6(10) . . ? C252 C251 H251 118.7 . . ? C256 C251 H251 118.7 . . ? C251 C252 C253 118.7(9) . . ? C251 C252 C226 123.0(10) . . ? C253 C252 C226 118.2(9) . . ? C254 C253 C252 120.5(10) . . ? C254 C253 C246 121.1(10) . . ? C252 C253 C246 118.4(9) . . ? C253 C254 C255 120.8(10) . . ? C253 C254 H254 119.6 . . ? C255 C254 H254 119.6 . . ? C261 C255 C256 118.6(10) . . ? C261 C255 C254 122.7(11) . . ? C256 C255 C254 118.7(9) . . ? C251 C256 C264 123.7(11) . . ? C251 C256 C255 118.5(9) . . ? C264 C256 C255 117.7(10) . . ? C262 C261 C255 121.5(12) . . ? C262 C261 H261 119.3 . . ? C255 C261 H261 119.3 . . ? C261 C262 C263 119.5(11) . . ? C261 C262 H262 120.3 . . ? C263 C262 H262 120.3 . . ? C264 C263 C262 119.7(11) . . ? C264 C263 H263 120.2 . . ? C262 C263 H263 120.2 . . ? C263 C264 C256 122.9(12) . . ? C263 C264 H264 118.5 . . ? C256 C264 H264 118.5 . . ? C316 N311 C312 117.0(10) . . ? C316 N311 Cd1 123.0(8) . . ? C312 N311 Cd1 119.1(7) . . ? N311 C312 C313 122.8(10) . . ? N311 C312 C325 114.8(9) . . ? C313 C312 C325 122.3(10) . . ? C312 C313 C314 118.4(11) . . ? C312 C313 H313 120.8 . . ? C314 C313 H313 120.8 . . ? C315 C314 C313 119.8(12) . . ? C315 C314 H314 120.1 . . ? C313 C314 H314 120.1 . . ? C314 C315 C316 118.3(12) . . ? C314 C315 H315 120.8 . . ? C316 C315 H315 120.8 . . ? N311 C316 C315 123.7(12) . . ? N311 C316 H316 118.2 . . ? C315 C316 H316 118.2 . . ? C325 N321 N322 103.9(8) . . ? C325 N321 Cd1 113.5(6) . . ? N322 N321 Cd1 139.1(7) . . ? C323 N322 N321 110.9(9) . . ? C323 N322 C326 128.9(10) . . ? N321 N322 C326 120.1(8) . . ? N322 C323 C324 108.5(11) . . ? N322 C323 H323 125.7 . . ? C324 C323 H323 125.7 . . ? C323 C324 C325 105.0(10) . . ? C323 C324 H324 127.5 . . ? C325 C324 H324 127.5 . . ? N321 C325 C324 111.6(9) . . ? N321 C325 C312 119.4(9) . . ? C324 C325 C312 128.9(9) . . ? N322 C326 C352 116.1(9) . . ? N322 C326 H32A 108.3 . . ? C352 C326 H32A 108.3 . . ? N322 C326 H32B 108.3 . . ? C352 C326 H32B 108.3 . . ? H32A C326 H32B 107.4 . . ? C336 N331 C332 117.3(9) . . ? C336 N331 Cd4 123.5(8) . . ? C332 N331 Cd4 117.9(6) . . ? N331 C332 C333 122.4(10) . . ? N331 C332 C343 115.3(8) . . ? C333 C332 C343 122.2(9) . . ? C332 C333 C334 118.3(11) . . ? C332 C333 H333 120.8 . . ? C334 C333 H333 120.8 . . ? C335 C334 C333 120.0(10) . . ? C335 C334 H334 120.0 . . ? C333 C334 H334 120.0 . . ? C336 C335 C334 117.1(11) . . ? C336 C335 H335 121.4 . . ? C334 C335 H335 121.4 . . ? N331 C336 C335 124.8(11) . . ? N331 C336 H336 117.6 . . ? C335 C336 H336 117.6 . . ? C345 N341 N342 112.0(8) . . ? C345 N341 C346 129.1(9) . . ? N342 N341 C346 118.9(8) . . ? C343 N342 N341 103.6(8) . . ? C343 N342 Cd4 115.4(6) . . ? N341 N342 Cd4 137.4(6) . . ? N342 C343 C344 112.5(9) . . ? N342 C343 C332 118.8(9) . . ? C344 C343 C332 128.7(9) . . ? C345 C344 C343 104.2(9) . . ? C345 C344 H344 127.9 . . ? C343 C344 H344 127.9 . . ? N341 C345 C344 107.7(9) . . ? N341 C345 H345 126.1 . . ? C344 C345 H345 126.1 . . ? C353 C346 N341 114.5(8) . . ? C353 C346 H34A 108.6 . . ? N341 C346 H34A 108.6 . . ? C353 C346 H34B 108.6 . . ? N341 C346 H34B 108.6 . . ? H34A C346 H34B 107.6 . . ? C352 C351 C356 121.9(11) . . ? C352 C351 H351 119.0 . . ? C356 C351 H351 119.0 . . ? C351 C352 C353 119.1(10) . . ? C351 C352 C326 124.0(10) . . ? C353 C352 C326 116.9(9) . . ? C354 C353 C352 120.4(9) . . ? C354 C353 C346 124.1(9) . . ? C352 C353 C346 115.5(9) . . ? C353 C354 C355 121.7(10) . . ? C353 C354 H354 119.1 . . ? C355 C354 H354 119.1 . . ? C361 C355 C354 122.3(11) . . ? C361 C355 C356 119.8(11) . . ? C354 C355 C356 117.9(10) . . ? C364 C356 C351 123.4(11) . . ? C364 C356 C355 117.7(11) . . ? C351 C356 C355 118.9(10) . . ? C362 C361 C355 119.8(13) . . ? C362 C361 H361 120.1 . . ? C355 C361 H361 120.1 . . ? C361 C362 C363 122.1(13) . . ? C361 C362 H362 118.9 . . ? C363 C362 H362 118.9 . . ? C364 C363 C362 118.6(12) . . ? C364 C363 H363 120.7 . . ? C362 C363 H363 120.7 . . ? C363 C364 C356 122.0(12) . . ? C363 C364 H364 119.0 . . ? C356 C364 H364 119.0 . . ? C416 N411 C412 118.3(9) . . ? C416 N411 Cd2 124.3(8) . . ? C412 N411 Cd2 117.3(6) . . ? N411 C412 C413 121.3(10) . . ? N411 C412 C423 116.0(9) . . ? C413 C412 C423 122.7(10) . . ? C414 C413 C412 117.5(11) . . ? C414 C413 H413 121.3 . . ? C412 C413 H413 121.3 . . ? C413 C414 C415 122.2(11) . . ? C413 C414 H414 118.9 . . ? C415 C414 H414 118.9 . . ? C416 C415 C414 116.4(11) . . ? C416 C415 H415 121.8 . . ? C414 C415 H415 121.8 . . ? N411 C416 C415 124.3(12) . . ? N411 C416 H416 117.8 . . ? C415 C416 H416 117.8 . . ? C425 N421 N422 110.8(8) . . ? C425 N421 C426 128.6(9) . . ? N422 N421 C426 120.6(8) . . ? N421 N422 C423 105.8(8) . . ? N421 N422 Cd2 139.5(6) . . ? C423 N422 Cd2 112.5(6) . . ? N422 C423 C424 108.9(9) . . ? N422 C423 C412 120.7(9) . . ? C424 C423 C412 130.3(10) . . ? C425 C424 C423 106.1(9) . . ? C425 C424 H424 127.0 . . ? C423 C424 H424 127.0 . . ? C424 C425 N421 108.5(10) . . ? C424 C425 H425 125.8 . . ? N421 C425 H425 125.8 . . ? N421 C426 C452 111.8(9) . . ? N421 C426 H42A 109.2 . . ? C452 C426 H42A 109.2 . . ? N421 C426 H42B 109.2 . . ? C452 C426 H42B 109.2 . . ? H42A C426 H42B 107.9 . . ? C432 N431 C436 119.8(10) . . ? C432 N431 Cd3 117.3(7) . . ? C436 N431 Cd3 122.8(8) . . ? N431 C432 C433 121.9(11) . . ? N431 C432 C443 117.9(10) . . ? C433 C432 C443 120.0(10) . . ? C434 C433 C432 118.0(11) . . ? C434 C433 H433 121.0 . . ? C432 C433 H433 121.0 . . ? C435 C434 C433 119.9(11) . . ? C435 C434 H434 120.0 . . ? C433 C434 H434 120.0 . . ? C434 C435 C436 118.7(13) . . ? C434 C435 H435 120.7 . . ? C436 C435 H435 120.7 . . ? N431 C436 C435 121.5(13) . . ? N431 C436 H436 119.2 . . ? C435 C436 H436 119.2 . . ? N442 N441 C445 111.0(9) . . ? N442 N441 C446 121.2(8) . . ? C445 N441 C446 127.7(10) . . ? C443 N442 N441 105.3(9) . . ? C443 N442 Cd3 114.6(7) . . ? N441 N442 Cd3 139.5(6) . . ? N442 C443 C444 111.0(10) . . ? N442 C443 C432 118.5(10) . . ? C444 C443 C432 130.4(10) . . ? C443 C444 C445 106.2(10) . . ? C443 C444 H444 126.9 . . ? C445 C444 H444 126.9 . . ? N441 C445 C444 106.5(10) . . ? N441 C445 H445 126.8 . . ? C444 C445 H445 126.8 . . ? N441 C446 C453 114.7(8) . . ? N441 C446 H44A 108.6 . . ? C453 C446 H44A 108.6 . . ? N441 C446 H44B 108.6 . . ? C453 C446 H44B 108.6 . . ? H44A C446 H44B 107.6 . . ? C452 C451 C456 121.9(10) . . ? C452 C451 H451 119.1 . . ? C456 C451 H451 119.1 . . ? C451 C452 C453 119.7(10) . . ? C451 C452 C426 124.1(10) . . ? C453 C452 C426 116.2(9) . . ? C454 C453 C452 120.2(10) . . ? C454 C453 C446 122.0(9) . . ? C452 C453 C446 117.8(9) . . ? C453 C454 C455 119.5(10) . . ? C453 C454 H454 120.2 . . ? C455 C454 H454 120.2 . . ? C456 C455 C454 119.6(10) . . ? C456 C455 C461 118.9(10) . . ? C454 C455 C461 121.5(10) . . ? C455 C456 C451 119.0(10) . . ? C455 C456 C464 119.9(10) . . ? C451 C456 C464 121.1(10) . . ? C462 C461 C455 119.2(11) . . ? C462 C461 H461 120.4 . . ? C455 C461 H461 120.4 . . ? C461 C462 C463 122.5(12) . . ? C461 C462 H462 118.8 . . ? C463 C462 H462 118.8 . . ? C462 C463 C464 121.0(12) . . ? C462 C463 H463 119.5 . . ? C464 C463 H463 119.5 . . ? C463 C464 C456 118.2(12) . . ? C463 C464 H464 120.9 . . ? C456 C464 H464 120.9 . . ? C516 N511 C512 118.1(8) . . ? C516 N511 Cd2 125.2(7) . . ? C512 N511 Cd2 115.3(6) . . ? N511 C512 C513 122.1(10) . . ? N511 C512 C523 118.1(9) . . ? C513 C512 C523 119.8(9) . . ? C512 C513 C514 119.0(10) . . ? C512 C513 H513 120.5 . . ? C514 C513 H513 120.5 . . ? C515 C514 C513 117.5(10) . . ? C515 C514 H514 121.3 . . ? C513 C514 H514 121.3 . . ? C516 C515 C514 119.3(10) . . ? C516 C515 H515 120.3 . . ? C514 C515 H515 120.3 . . ? N511 C516 C515 124.0(10) . . ? N511 C516 H516 118.0 . . ? C515 C516 H516 118.0 . . ? N522 N521 C525 110.0(8) . . ? N522 N521 C526 120.2(8) . . ? C525 N521 C526 129.8(9) . . ? N521 N522 C523 105.4(8) . . ? N521 N522 Cd2 138.2(6) . . ? C523 N522 Cd2 114.1(6) . . ? N522 C523 C524 109.8(9) . . ? N522 C523 C512 118.4(9) . . ? C524 C523 C512 131.7(9) . . ? C525 C524 C523 106.5(9) . . ? C525 C524 H524 126.8 . . ? C523 C524 H524 126.8 . . ? C524 C525 N521 108.3(9) . . ? C524 C525 H525 125.9 . . ? N521 C525 H525 125.9 . . ? N521 C526 C552 114.8(8) . . ? N521 C526 H52A 108.6 . . ? C552 C526 H52A 108.6 . . ? N521 C526 H52B 108.6 . . ? C552 C526 H52B 108.6 . . ? H52A C526 H52B 107.5 . . ? C536 N531 C532 119.4(9) . . ? C536 N531 Cd4 123.4(8) . . ? C532 N531 Cd4 116.7(6) . . ? N531 C532 C533 120.5(10) . . ? N531 C532 C543 117.4(9) . . ? C533 C532 C543 122.1(10) . . ? C532 C533 C534 118.5(11) . . ? C532 C533 H533 120.8 . . ? C534 C533 H533 120.8 . . ? C535 C534 C533 118.3(11) . . ? C535 C534 H534 120.8 . . ? C533 C534 H534 120.8 . . ? C534 C535 C536 121.1(11) . . ? C534 C535 H535 119.5 . . ? C536 C535 H535 119.5 . . ? N531 C536 C535 122.1(11) . . ? N531 C536 H536 119.0 . . ? C535 C536 H536 119.0 . . ? N542 N541 C545 109.9(9) . . ? N542 N541 C546 121.3(8) . . ? C545 N541 C546 128.7(9) . . ? N541 N542 C543 105.0(8) . . ? N541 N542 Cd4 140.5(7) . . ? C543 N542 Cd4 114.0(7) . . ? N542 C543 C544 111.0(9) . . ? N542 C543 C532 119.2(9) . . ? C544 C543 C532 129.7(10) . . ? C545 C544 C543 104.1(10) . . ? C545 C544 H544 128.0 . . ? C543 C544 H544 128.0 . . ? C544 C545 N541 110.0(10) . . ? C544 C545 H545 125.0 . . ? N541 C545 H545 125.0 . . ? N541 C546 C553 116.3(9) . . ? N541 C546 H54A 108.2 . . ? C553 C546 H54A 108.2 . . ? N541 C546 H54B 108.2 . . ? C553 C546 H54B 108.2 . . ? H54A C546 H54B 107.4 . . ? C552 C551 C556 122.6(10) . . ? C552 C551 H551 118.7 . . ? C556 C551 H551 118.7 . . ? C551 C552 C553 118.6(9) . . ? C551 C552 C526 123.7(9) . . ? C553 C552 C526 117.7(9) . . ? C554 C553 C552 120.2(10) . . ? C554 C553 C546 123.5(10) . . ? C552 C553 C546 116.2(9) . . ? C553 C554 C555 122.3(10) . . ? C553 C554 H554 118.8 . . ? C555 C554 H554 118.8 . . ? C561 C555 C554 122.3(10) . . ? C561 C555 C556 119.3(10) . . ? C554 C555 C556 118.4(10) . . ? C564 C556 C551 123.4(10) . . ? C564 C556 C555 118.8(10) . . ? C551 C556 C555 117.8(10) . . ? C562 C561 C555 119.8(11) . . ? C562 C561 H561 120.1 . . ? C555 C561 H561 120.1 . . ? C561 C562 C563 121.7(11) . . ? C561 C562 H562 119.1 . . ? C563 C562 H562 119.1 . . ? C564 C563 C562 119.5(11) . . ? C564 C563 H563 120.3 . . ? C562 C563 H563 120.3 . . ? C563 C564 C556 120.8(11) . . ? C563 C564 H564 119.6 . . ? C556 C564 H564 119.6 . . ? C616 N611 C612 119.0(11) . . ? C616 N611 Cd3 123.8(9) . . ? C612 N611 Cd3 116.4(8) . . ? N611 C612 C613 121.1(12) . . ? N611 C612 C623 117.0(11) . . ? C613 C612 C623 121.9(11) . . ? C614 C613 C612 119.4(13) . . ? C614 C613 H613 120.3 . . ? C612 C613 H613 120.3 . . ? C613 C614 C615 119.4(13) . . ? C613 C614 H614 120.3 . . ? C615 C614 H614 120.3 . . ? C616 C615 C614 118.8(14) . . ? C616 C615 H615 120.6 . . ? C614 C615 H615 120.6 . . ? N611 C616 C615 122.2(15) . . ? N611 C616 H616 118.9 . . ? C615 C616 H616 118.9 . . ? C625 N621 N622 110.3(9) . . ? C625 N621 C626 129.7(10) . . ? N622 N621 C626 120.0(8) . . ? C623 N622 N621 104.4(9) . . ? C623 N622 Cd3 115.2(7) . . ? N621 N622 Cd3 140.1(7) . . ? N622 C623 C624 110.2(10) . . ? N622 C623 C612 119.5(10) . . ? C624 C623 C612 130.1(11) . . ? C625 C624 C623 105.5(10) . . ? C625 C624 H624 127.3 . . ? C623 C624 H624 127.3 . . ? C624 C625 N621 109.5(10) . . ? C624 C625 H625 125.3 . . ? N621 C625 H625 125.3 . . ? N621 C626 C652 116.1(9) . . ? N621 C626 H62A 108.3 . . ? C652 C626 H62A 108.3 . . ? N621 C626 H62B 108.3 . . ? C652 C626 H62B 108.3 . . ? H62A C626 H62B 107.4 . . ? C636 N631 C632 118.0(9) . . ? C636 N631 Cd4 124.5(7) . . ? C632 N631 Cd4 117.4(7) . . ? N631 C632 C633 121.1(10) . . ? N631 C632 C643 116.6(9) . . ? C633 C632 C643 122.2(11) . . ? C632 C633 C634 119.4(11) . . ? C632 C633 H633 120.3 . . ? C634 C633 H633 120.3 . . ? C633 C634 C635 119.4(11) . . ? C633 C634 H634 120.3 . . ? C635 C634 H634 120.3 . . ? C636 C635 C634 116.9(11) . . ? C636 C635 H635 121.6 . . ? C634 C635 H635 121.6 . . ? N631 C636 C635 125.2(11) . . ? N631 C636 H636 117.4 . . ? C635 C636 H636 117.4 . . ? N642 N641 C645 110.8(10) . . ? N642 N641 C646 122.3(9) . . ? C645 N641 C646 126.8(10) . . ? N641 N642 C643 106.6(9) . . ? N641 N642 Cd4 137.8(7) . . ? C643 N642 Cd4 111.9(6) . . ? N642 C643 C644 110.4(10) . . ? N642 C643 C632 120.1(9) . . ? C644 C643 C632 129.4(10) . . ? C645 C644 C643 105.8(11) . . ? C645 C644 H644 127.1 . . ? C643 C644 H644 127.1 . . ? C644 C645 N641 106.4(11) . . ? C644 C645 H645 126.8 . . ? N641 C645 H645 126.8 . . ? N641 C646 C653 115.0(9) . . ? N641 C646 H64A 108.5 . . ? C653 C646 H64A 108.5 . . ? N641 C646 H64B 108.5 . . ? C653 C646 H64B 108.5 . . ? H64A C646 H64B 107.5 . . ? C652 C651 C656 120.7(11) . . ? C652 C651 H651 119.7 . . ? C656 C651 H651 119.7 . . ? C651 C652 C653 119.6(11) . . ? C651 C652 C626 121.7(10) . . ? C653 C652 C626 118.6(9) . . ? C654 C653 C652 120.0(10) . . ? C654 C653 C646 123.8(11) . . ? C652 C653 C646 116.1(10) . . ? C653 C654 C655 122.3(12) . . ? C653 C654 H654 118.8 . . ? C655 C654 H654 118.8 . . ? C656 C655 C654 118.0(11) . . ? C656 C655 C661 119.6(11) . . ? C654 C655 C661 122.4(12) . . ? C655 C656 C651 119.3(11) . . ? C655 C656 C664 117.8(12) . . ? C651 C656 C664 123.0(13) . . ? C662 C661 C655 118.9(14) . . ? C662 C661 H661 120.6 . . ? C655 C661 H661 120.6 . . ? C661 C662 C663 122.7(14) . . ? C661 C662 H662 118.6 . . ? C663 C662 H662 118.6 . . ? C664 C663 C662 119.9(14) . . ? C664 C663 H663 120.0 . . ? C662 C663 H663 120.0 . . ? C663 C664 C656 121.2(16) . . ? C663 C664 H664 119.4 . . ? C656 C664 H664 119.4 . . ? F12 B11 F14 110.4(11) . . ? F12 B11 F13 109.8(11) . . ? F14 B11 F13 110.4(11) . . ? F12 B11 F15 108.9(11) . . ? F14 B11 F15 108.6(11) . . ? F13 B11 F15 108.7(11) . . ? F25Y B21 F24X 132.0(7) . . ? F25Y B21 F23X 83.2(6) . . ? F24X B21 F23X 110.1(4) . . ? F25Y B21 F22 109.2(4) . . ? F24X B21 F22 109.2(4) . . ? F23X B21 F22 109.0(4) . . ? F25Y B21 F24Y 110.0(4) . . ? F24X B21 F24Y 28.6(6) . . ? F23X B21 F24Y 132.3(7) . . ? F22 B21 F24Y 108.9(4) . . ? F25Y B21 F23Y 110.0(4) . . ? F24X B21 F23Y 83.3(6) . . ? F23X B21 F23Y 29.2(6) . . ? F22 B21 F23Y 108.9(4) . . ? F24Y B21 F23Y 109.8(4) . . ? F25Y B21 F25X 28.8(6) . . ? F24X B21 F25X 109.9(4) . . ? F23X B21 F25X 109.8(4) . . ? F22 B21 F25X 108.8(4) . . ? F24Y B21 F25X 83.7(6) . . ? F23Y B21 F25X 132.5(7) . . ? F35 B31 F34 111.5(15) . . ? F35 B31 F33 112.8(15) . . ? F34 B31 F33 107.4(15) . . ? F35 B31 F32 110.0(15) . . ? F34 B31 F32 108.1(14) . . ? F33 B31 F32 106.7(14) . . ? F43Y B41 F45X 85.9(7) . . ? F43Y B41 F45Y 107.4(5) . . ? F45X B41 F45Y 125.4(8) . . ? F43Y B41 F44X 125.5(8) . . ? F45X B41 F44X 107.5(5) . . ? F45Y B41 F44X 23.7(7) . . ? F43Y B41 F42 111.5(4) . . ? F45X B41 F42 111.6(4) . . ? F45Y B41 F42 111.5(4) . . ? F44X B41 F42 111.5(4) . . ? F43Y B41 F44Y 107.4(5) . . ? F45X B41 F44Y 24.0(7) . . ? F45Y B41 F44Y 107.3(5) . . ? F44X B41 F44Y 86.1(7) . . ? F42 B41 F44Y 111.4(4) . . ? F43Y B41 F43X 24.0(7) . . ? F45X B41 F43X 107.3(5) . . ? F45Y B41 F43X 86.1(7) . . ? F44X B41 F43X 107.3(5) . . ? F42 B41 F43X 111.4(4) . . ? F44Y B41 F43X 125.7(8) . . ? F55 B51 F53 110.8(12) . . ? F55 B51 F54 110.4(12) . . ? F53 B51 F54 110.9(12) . . ? F55 B51 F52 108.4(12) . . ? F53 B51 F52 109.3(12) . . ? F54 B51 F52 106.9(11) . . ? F65 B61 F64 110.2(19) . . ? F65 B61 F63 110.6(17) . . ? F64 B61 F63 108.8(16) . . ? F65 B61 F62 107.7(16) . . ? F64 B61 F62 111.1(17) . . ? F63 B61 F62 108.4(19) . . ? O11S C12S H12C 109.5 . . ? O11S C12S H12D 109.5 . . ? H12C C12S H12D 109.5 . . ? O11S C12S H12E 109.5 . . ? H12C C12S H12E 109.5 . . ? H12D C12S H12E 109.5 . . ? O21S C22S H22C 109.5 . . ? O21S C22S H22D 109.5 . . ? H22C C22S H22D 109.5 . . ? O21S C22S H22E 109.5 . . ? H22C C22S H22E 109.5 . . ? H22D C22S H22E 109.5 . . ? O31S C32S H32C 109.5 . . ? O31S C32S H32D 109.5 . . ? H32C C32S H32D 109.5 . . ? O31S C32S H32E 109.5 . . ? H32C C32S H32E 109.5 . . ? H32D C32S H32E 109.5 . . ? O41S C42S H42C 109.5 . . ? O41S C42S H42D 109.5 . . ? H42C C42S H42D 109.5 . . ? O41S C42S H42E 109.5 . . ? H42C C42S H42E 109.5 . . ? H42D C42S H42E 109.5 . . ? O51S C52S H52C 109.5 . . ? O51S C52S H52D 109.5 . . ? H52C C52S H52D 109.5 . . ? O51S C52S H52E 109.5 . . ? H52C C52S H52E 109.5 . . ? H52D C52S H52E 109.5 . . ? O61S C62S H62C 109.5 . . ? O61S C62S H62D 109.5 . . ? H62C C62S H62D 109.5 . . ? O61S C62S H62E 109.5 . . ? H62C C62S H62E 109.5 . . ? H62D C62S H62E 109.5 . . ? O71S C72S H72A 109.5 . . ? O71S C72S H72B 109.5 . . ? H72A C72S H72B 109.5 . . ? O71S C72S H72C 109.5 . . ? H72A C72S H72C 109.5 . . ? H72B C72S H72C 109.5 . . ? O81S C82S H82A 109.5 . . ? O81S C82S H82B 109.5 . . ? H82A C82S H82B 109.5 . . ? O81S C82S H82C 109.5 . . ? H82A C82S H82C 109.5 . . ? H82B C82S H82C 109.5 . . ? O91S C92S H92A 109.5 . . ? O91S C92S H92B 109.5 . . ? H92A C92S H92B 109.5 . . ? O91S C92S H92C 109.5 . . ? H92A C92S H92C 109.5 . . ? H92B C92S H92C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N311 Cd1 N111 C116 0.2(9) . . . . ? N222 Cd1 N111 C116 144.7(10) . . . . ? N211 Cd1 N111 C116 99.7(9) . . . . ? N321 Cd1 N111 C116 -69.8(9) . . . . ? N122 Cd1 N111 C116 -173.7(9) . . . . ? N311 Cd1 N111 C112 177.6(7) . . . . ? N222 Cd1 N111 C112 -37.9(14) . . . . ? N211 Cd1 N111 C112 -83.0(8) . . . . ? N321 Cd1 N111 C112 107.6(8) . . . . ? N122 Cd1 N111 C112 3.7(7) . . . . ? C116 N111 C112 C113 -3.9(16) . . . . ? Cd1 N111 C112 C113 178.7(8) . . . . ? C116 N111 C112 C123 176.7(10) . . . . ? Cd1 N111 C112 C123 -0.7(12) . . . . ? N111 C112 C113 C114 2.1(17) . . . . ? C123 C112 C113 C114 -178.6(11) . . . . ? C112 C113 C114 C115 1.3(19) . . . . ? C113 C114 C115 C116 -3(2) . . . . ? C112 N111 C116 C115 2.2(18) . . . . ? Cd1 N111 C116 C115 179.6(10) . . . . ? C114 C115 C116 N111 1(2) . . . . ? C125 N121 N122 C123 3.0(11) . . . . ? C126 N121 N122 C123 -180.0(9) . . . . ? C125 N121 N122 Cd1 171.1(8) . . . . ? C126 N121 N122 Cd1 -11.9(15) . . . . ? N311 Cd1 N122 C123 -79(3) . . . . ? N111 Cd1 N122 C123 -6.5(6) . . . . ? N222 Cd1 N122 C123 160.5(7) . . . . ? N211 Cd1 N122 C123 88.8(7) . . . . ? N321 Cd1 N122 C123 -90.6(7) . . . . ? N311 Cd1 N122 N121 114(3) . . . . ? N111 Cd1 N122 N121 -173.9(10) . . . . ? N222 Cd1 N122 N121 -6.9(10) . . . . ? N211 Cd1 N122 N121 -78.6(10) . . . . ? N321 Cd1 N122 N121 101.9(10) . . . . ? N121 N122 C123 C124 -3.0(11) . . . . ? Cd1 N122 C123 C124 -174.8(7) . . . . ? N121 N122 C123 C112 -179.4(8) . . . . ? Cd1 N122 C123 C112 8.8(11) . . . . ? N111 C112 C123 N122 -5.8(14) . . . . ? C113 C112 C123 N122 174.8(10) . . . . ? N111 C112 C123 C124 178.6(10) . . . . ? C113 C112 C123 C124 -0.8(17) . . . . ? N122 C123 C124 C125 2.0(12) . . . . ? C112 C123 C124 C125 177.9(10) . . . . ? N122 N121 C125 C124 -1.8(12) . . . . ? C126 N121 C125 C124 -178.7(10) . . . . ? C123 C124 C125 N121 -0.1(12) . . . . ? C125 N121 C126 C152 -73.6(13) . . . . ? N122 N121 C126 C152 109.9(10) . . . . ? N411 Cd2 N131 C132 175.5(9) . . . . ? N422 Cd2 N131 C132 103.4(9) . . . . ? N511 Cd2 N131 C132 -82.0(9) . . . . ? N522 Cd2 N131 C132 -54.0(14) . . . . ? N142 Cd2 N131 C132 3.4(8) . . . . ? N411 Cd2 N131 C136 -8.2(9) . . . . ? N422 Cd2 N131 C136 -80.3(9) . . . . ? N511 Cd2 N131 C136 94.3(9) . . . . ? N522 Cd2 N131 C136 122.3(11) . . . . ? N142 Cd2 N131 C136 179.7(10) . . . . ? C136 N131 C132 C133 2.0(18) . . . . ? Cd2 N131 C132 C133 178.6(10) . . . . ? C136 N131 C132 C143 -179.1(10) . . . . ? Cd2 N131 C132 C143 -2.5(14) . . . . ? N131 C132 C133 C134 -3(2) . . . . ? C143 C132 C133 C134 178.5(14) . . . . ? C132 C133 C134 C135 3(2) . . . . ? C133 C134 C135 C136 -3(2) . . . . ? C134 C135 C136 N131 2(2) . . . . ? C132 N131 C136 C135 -2.0(19) . . . . ? Cd2 N131 C136 C135 -178.3(11) . . . . ? C145 N141 N142 C143 -1.6(11) . . . . ? C146 N141 N142 C143 -174.6(9) . . . . ? C145 N141 N142 Cd2 168.6(8) . . . . ? C146 N141 N142 Cd2 -4.4(15) . . . . ? N411 Cd2 N142 C143 -39.5(17) . . . . ? N131 Cd2 N142 C143 -3.9(7) . . . . ? N422 Cd2 N142 C143 -91.1(7) . . . . ? N511 Cd2 N142 C143 89.4(7) . . . . ? N522 Cd2 N142 C143 160.5(7) . . . . ? N411 Cd2 N142 N141 151.0(12) . . . . ? N131 Cd2 N142 N141 -173.5(11) . . . . ? N422 Cd2 N142 N141 99.3(10) . . . . ? N511 Cd2 N142 N141 -80.2(10) . . . . ? N522 Cd2 N142 N141 -9.1(11) . . . . ? N141 N142 C143 C144 0.7(12) . . . . ? Cd2 N142 C143 C144 -172.5(8) . . . . ? N141 N142 C143 C132 177.4(10) . . . . ? Cd2 N142 C143 C132 4.2(13) . . . . ? N131 C132 C143 N142 -1.3(16) . . . . ? C133 C132 C143 N142 177.6(12) . . . . ? N131 C132 C143 C144 174.7(12) . . . . ? C133 C132 C143 C144 -6(2) . . . . ? N142 C143 C144 C145 0.4(14) . . . . ? C132 C143 C144 C145 -175.8(12) . . . . ? C143 C144 C145 N141 -1.4(14) . . . . ? N142 N141 C145 C144 1.9(13) . . . . ? C146 N141 C145 C144 174.3(10) . . . . ? N142 N141 C146 C153 106.5(11) . . . . ? C145 N141 C146 C153 -65.2(14) . . . . ? C156 C151 C152 C153 -1.4(15) . . . . ? C156 C151 C152 C126 -177.4(10) . . . . ? N121 C126 C152 C151 -16.6(14) . . . . ? N121 C126 C152 C153 167.4(9) . . . . ? C151 C152 C153 C154 2.7(15) . . . . ? C126 C152 C153 C154 179.0(10) . . . . ? C151 C152 C153 C146 -174.9(9) . . . . ? C126 C152 C153 C146 1.4(14) . . . . ? N141 C146 C153 C154 -4.0(15) . . . . ? N141 C146 C153 C152 173.6(9) . . . . ? C152 C153 C154 C155 -2.0(16) . . . . ? C146 C153 C154 C155 175.5(10) . . . . ? C153 C154 C155 C161 -177.3(10) . . . . ? C153 C154 C155 C156 -0.1(16) . . . . ? C152 C151 C156 C155 -0.7(15) . . . . ? C152 C151 C156 C164 176.8(10) . . . . ? C161 C155 C156 C151 178.7(10) . . . . ? C154 C155 C156 C151 1.4(15) . . . . ? C161 C155 C156 C164 1.1(15) . . . . ? C154 C155 C156 C164 -176.1(9) . . . . ? C154 C155 C161 C162 175.7(11) . . . . ? C156 C155 C161 C162 -1.4(17) . . . . ? C155 C161 C162 C163 0.8(18) . . . . ? C161 C162 C163 C164 -0.1(19) . . . . ? C162 C163 C164 C156 -0.2(18) . . . . ? C151 C156 C164 C163 -177.8(10) . . . . ? C155 C156 C164 C163 -0.4(16) . . . . ? N311 Cd1 N211 C216 91.5(10) . . . . ? N111 Cd1 N211 C216 -16.2(10) . . . . ? N222 Cd1 N211 C216 178.4(10) . . . . ? N321 Cd1 N211 C216 89.8(19) . . . . ? N122 Cd1 N211 C216 -87.1(10) . . . . ? N311 Cd1 N211 C212 -92.2(7) . . . . ? N111 Cd1 N211 C212 160.1(7) . . . . ? N222 Cd1 N211 C212 -5.3(7) . . . . ? N321 Cd1 N211 C212 -93.9(17) . . . . ? N122 Cd1 N211 C212 89.2(7) . . . . ? C216 N211 C212 C213 4.7(16) . . . . ? Cd1 N211 C212 C213 -171.8(8) . . . . ? C216 N211 C212 C223 -176.7(10) . . . . ? Cd1 N211 C212 C223 6.7(11) . . . . ? N211 C212 C213 C214 -3.3(17) . . . . ? C223 C212 C213 C214 178.2(11) . . . . ? C212 C213 C214 C215 2.0(19) . . . . ? C213 C214 C215 C216 -2(2) . . . . ? C212 N211 C216 C215 -4.9(18) . . . . ? Cd1 N211 C216 C215 171.2(10) . . . . ? C214 C215 C216 N211 4(2) . . . . ? C225 N221 N222 C223 -0.9(11) . . . . ? C226 N221 N222 C223 -176.2(8) . . . . ? C225 N221 N222 Cd1 176.7(7) . . . . ? C226 N221 N222 Cd1 1.5(14) . . . . ? N311 Cd1 N222 N221 -76.1(9) . . . . ? N111 Cd1 N222 N221 137.6(10) . . . . ? N211 Cd1 N222 N221 -174.4(10) . . . . ? N321 Cd1 N222 N221 -5.9(10) . . . . ? N122 Cd1 N222 N221 98.6(9) . . . . ? N311 Cd1 N222 C223 101.4(7) . . . . ? N111 Cd1 N222 C223 -44.8(13) . . . . ? N211 Cd1 N222 C223 3.1(6) . . . . ? N321 Cd1 N222 C223 171.6(6) . . . . ? N122 Cd1 N222 C223 -83.8(7) . . . . ? N221 N222 C223 C224 0.9(11) . . . . ? Cd1 N222 C223 C224 -177.4(7) . . . . ? N221 N222 C223 C212 177.4(9) . . . . ? Cd1 N222 C223 C212 -0.9(12) . . . . ? N211 C212 C223 N222 -4.0(14) . . . . ? C213 C212 C223 N222 174.5(10) . . . . ? N211 C212 C223 C224 171.7(11) . . . . ? C213 C212 C223 C224 -9.8(18) . . . . ? N222 C223 C224 C225 -0.6(12) . . . . ? C212 C223 C224 C225 -176.7(10) . . . . ? N222 N221 C225 C224 0.6(12) . . . . ? C226 N221 C225 C224 175.2(9) . . . . ? C223 C224 C225 N221 0.0(12) . . . . ? C225 N221 C226 C252 -82.6(13) . . . . ? N222 N221 C226 C252 91.6(11) . . . . ? N431 Cd3 N231 C232 -91.6(8) . . . . ? N611 Cd3 N231 C232 171.1(8) . . . . ? N622 Cd3 N231 C232 100.0(8) . . . . ? N442 Cd3 N231 C232 -45(2) . . . . ? N242 Cd3 N231 C232 -1.8(8) . . . . ? N431 Cd3 N231 C236 96.1(10) . . . . ? N611 Cd3 N231 C236 -1.1(10) . . . . ? N622 Cd3 N231 C236 -72.2(10) . . . . ? N442 Cd3 N231 C236 143.1(15) . . . . ? N242 Cd3 N231 C236 -174.0(11) . . . . ? C236 N231 C232 C233 1.1(18) . . . . ? Cd3 N231 C232 C233 -171.3(9) . . . . ? C236 N231 C232 C243 179.2(11) . . . . ? Cd3 N231 C232 C243 6.8(13) . . . . ? N231 C232 C233 C234 0.0(18) . . . . ? C243 C232 C233 C234 -178.2(11) . . . . ? C232 C233 C234 C235 -1(2) . . . . ? C233 C234 C235 C236 1(3) . . . . ? C232 N231 C236 C235 -1(2) . . . . ? Cd3 N231 C236 C235 170.9(12) . . . . ? C234 C235 C236 N231 0(3) . . . . ? C245 N241 N242 C243 -1.0(12) . . . . ? C246 N241 N242 C243 -177.0(9) . . . . ? C245 N241 N242 Cd3 164.4(9) . . . . ? C246 N241 N242 Cd3 -11.6(15) . . . . ? N431 Cd3 N242 C243 96.7(8) . . . . ? N231 Cd3 N242 C243 -3.5(7) . . . . ? N611 Cd3 N242 C243 -38(2) . . . . ? N622 Cd3 N242 C243 -88.1(8) . . . . ? N442 Cd3 N242 C243 168.5(7) . . . . ? N431 Cd3 N242 N241 -67.6(11) . . . . ? N231 Cd3 N242 N241 -167.9(11) . . . . ? N611 Cd3 N242 N241 157.4(14) . . . . ? N622 Cd3 N242 N241 107.6(10) . . . . ? N442 Cd3 N242 N241 4.1(11) . . . . ? N241 N242 C243 C244 0.5(12) . . . . ? Cd3 N242 C243 C244 -169.3(8) . . . . ? N241 N242 C243 C232 177.9(9) . . . . ? Cd3 N242 C243 C232 8.1(12) . . . . ? N231 C232 C243 N242 -10.2(16) . . . . ? C233 C232 C243 N242 168.0(10) . . . . ? N231 C232 C243 C244 166.6(12) . . . . ? C233 C232 C243 C244 -15.2(19) . . . . ? N242 C243 C244 C245 0.3(14) . . . . ? C232 C243 C244 C245 -176.7(12) . . . . ? N242 N241 C245 C244 1.2(13) . . . . ? C246 N241 C245 C244 176.8(10) . . . . ? C243 C244 C245 N241 -0.9(14) . . . . ? C245 N241 C246 C253 -81.3(14) . . . . ? N242 N241 C246 C253 93.9(11) . . . . ? C256 C251 C252 C253 -2.1(16) . . . . ? C256 C251 C252 C226 177.6(10) . . . . ? N221 C226 C252 C251 9.9(15) . . . . ? N221 C226 C252 C253 -170.3(9) . . . . ? C251 C252 C253 C254 1.7(15) . . . . ? C226 C252 C253 C254 -178.1(9) . . . . ? C251 C252 C253 C246 -179.5(10) . . . . ? C226 C252 C253 C246 0.7(14) . . . . ? N241 C246 C253 C254 3.6(15) . . . . ? N241 C246 C253 C252 -175.2(9) . . . . ? C252 C253 C254 C255 -2.5(15) . . . . ? C246 C253 C254 C255 178.7(10) . . . . ? C253 C254 C255 C261 -178.7(11) . . . . ? C253 C254 C255 C256 3.7(15) . . . . ? C252 C251 C256 C264 179.9(11) . . . . ? C252 C251 C256 C255 3.4(17) . . . . ? C261 C255 C256 C251 178.3(11) . . . . ? C254 C255 C256 C251 -4.0(15) . . . . ? C261 C255 C256 C264 1.5(16) . . . . ? C254 C255 C256 C264 179.2(10) . . . . ? C256 C255 C261 C262 -1.7(18) . . . . ? C254 C255 C261 C262 -179.3(11) . . . . ? C255 C261 C262 C263 -0.1(19) . . . . ? C261 C262 C263 C264 2(2) . . . . ? C262 C263 C264 C256 -2(2) . . . . ? C251 C256 C264 C263 -176.0(12) . . . . ? C255 C256 C264 C263 0.5(18) . . . . ? N111 Cd1 N311 C316 108.0(10) . . . . ? N222 Cd1 N311 C316 -60.7(10) . . . . ? N211 Cd1 N311 C316 10.9(10) . . . . ? N321 Cd1 N311 C316 -169.4(10) . . . . ? N122 Cd1 N311 C316 179(100) . . . . ? N111 Cd1 N311 C312 -83.6(8) . . . . ? N222 Cd1 N311 C312 107.7(8) . . . . ? N211 Cd1 N311 C312 179.3(8) . . . . ? N321 Cd1 N311 C312 -1.1(8) . . . . ? N122 Cd1 N311 C312 -13(3) . . . . ? C316 N311 C312 C313 1.7(16) . . . . ? Cd1 N311 C312 C313 -167.3(8) . . . . ? C316 N311 C312 C325 177.6(10) . . . . ? Cd1 N311 C312 C325 8.6(12) . . . . ? N311 C312 C313 C314 -1.2(17) . . . . ? C325 C312 C313 C314 -176.8(11) . . . . ? C312 C313 C314 C315 -0.4(18) . . . . ? C313 C314 C315 C316 1(2) . . . . ? C312 N311 C316 C315 -0.8(19) . . . . ? Cd1 N311 C316 C315 167.8(10) . . . . ? C314 C315 C316 N311 -1(2) . . . . ? N311 Cd1 N321 C325 -7.4(7) . . . . ? N111 Cd1 N321 C325 100.9(8) . . . . ? N222 Cd1 N321 C325 -90.7(7) . . . . ? N211 Cd1 N321 C325 -6(2) . . . . ? N122 Cd1 N321 C325 171.3(7) . . . . ? N311 Cd1 N321 N322 -161.6(11) . . . . ? N111 Cd1 N321 N322 -53.3(10) . . . . ? N222 Cd1 N321 N322 115.1(10) . . . . ? N211 Cd1 N321 N322 -159.8(14) . . . . ? N122 Cd1 N321 N322 17.1(10) . . . . ? C325 N321 N322 C323 1.8(13) . . . . ? Cd1 N321 N322 C323 157.5(9) . . . . ? C325 N321 N322 C326 178.4(9) . . . . ? Cd1 N321 N322 C326 -26.0(15) . . . . ? N321 N322 C323 C324 -2.6(15) . . . . ? C326 N322 C323 C324 -178.7(11) . . . . ? N322 C323 C324 C325 2.2(15) . . . . ? N322 N321 C325 C324 -0.4(13) . . . . ? Cd1 N321 C325 C324 -163.3(8) . . . . ? N322 N321 C325 C312 177.8(9) . . . . ? Cd1 N321 C325 C312 14.9(12) . . . . ? C323 C324 C325 N321 -1.1(15) . . . . ? C323 C324 C325 C312 -179.1(12) . . . . ? N311 C312 C325 N321 -16.1(15) . . . . ? C313 C312 C325 N321 159.8(10) . . . . ? N311 C312 C325 C324 161.8(12) . . . . ? C313 C312 C325 C324 -22.3(19) . . . . ? C323 N322 C326 C352 -82.3(15) . . . . ? N321 N322 C326 C352 101.9(11) . . . . ? N631 Cd4 N331 C336 115.0(9) . . . . ? N531 Cd4 N331 C336 9.5(9) . . . . ? N342 Cd4 N331 C336 -167.3(9) . . . . ? N542 Cd4 N331 C336 -60.8(9) . . . . ? N642 Cd4 N331 C336 159(3) . . . . ? N631 Cd4 N331 C332 -78.2(8) . . . . ? N531 Cd4 N331 C332 176.4(7) . . . . ? N342 Cd4 N331 C332 -0.5(7) . . . . ? N542 Cd4 N331 C332 106.0(8) . . . . ? N642 Cd4 N331 C332 -34(4) . . . . ? C336 N331 C332 C333 -1.2(15) . . . . ? Cd4 N331 C332 C333 -168.8(7) . . . . ? C336 N331 C332 C343 176.0(9) . . . . ? Cd4 N331 C332 C343 8.3(11) . . . . ? N331 C332 C333 C334 2.6(15) . . . . ? C343 C332 C333 C334 -174.4(9) . . . . ? C332 C333 C334 C335 -2.2(16) . . . . ? C333 C334 C335 C336 0.4(16) . . . . ? C332 N331 C336 C335 -0.8(16) . . . . ? Cd4 N331 C336 C335 166.2(9) . . . . ? C334 C335 C336 N331 1.1(17) . . . . ? C345 N341 N342 C343 0.3(10) . . . . ? C346 N341 N342 C343 179.2(8) . . . . ? C345 N341 N342 Cd4 156.2(7) . . . . ? C346 N341 N342 Cd4 -24.9(13) . . . . ? N631 Cd4 N342 C343 99.6(7) . . . . ? N531 Cd4 N342 C343 -25(2) . . . . ? N331 Cd4 N342 C343 -8.3(7) . . . . ? N542 Cd4 N342 C343 -85.4(7) . . . . ? N642 Cd4 N342 C343 168.7(7) . . . . ? N631 Cd4 N342 N341 -54.4(9) . . . . ? N531 Cd4 N342 N341 -179(100) . . . . ? N331 Cd4 N342 N341 -162.3(9) . . . . ? N542 Cd4 N342 N341 120.6(9) . . . . ? N642 Cd4 N342 N341 14.7(9) . . . . ? N341 N342 C343 C344 -0.9(10) . . . . ? Cd4 N342 C343 C344 -163.1(6) . . . . ? N341 N342 C343 C332 178.2(8) . . . . ? Cd4 N342 C343 C332 16.0(11) . . . . ? N331 C332 C343 N342 -16.6(13) . . . . ? C333 C332 C343 N342 160.6(9) . . . . ? N331 C332 C343 C344 162.4(10) . . . . ? C333 C332 C343 C344 -20.4(16) . . . . ? N342 C343 C344 C345 1.1(11) . . . . ? C332 C343 C344 C345 -177.9(9) . . . . ? N342 N341 C345 C344 0.4(11) . . . . ? C346 N341 C345 C344 -178.3(9) . . . . ? C343 C344 C345 N341 -0.9(11) . . . . ? C345 N341 C346 C353 -70.9(13) . . . . ? N342 N341 C346 C353 110.5(10) . . . . ? C356 C351 C352 C353 2.6(16) . . . . ? C356 C351 C352 C326 179.3(10) . . . . ? N322 C326 C352 C351 10.5(15) . . . . ? N322 C326 C352 C353 -172.7(9) . . . . ? C351 C352 C353 C354 -0.8(15) . . . . ? C326 C352 C353 C354 -177.8(10) . . . . ? C351 C352 C353 C346 179.2(9) . . . . ? C326 C352 C353 C346 2.2(13) . . . . ? N341 C346 C353 C354 10.1(14) . . . . ? N341 C346 C353 C352 -169.9(8) . . . . ? C352 C353 C354 C355 -1.6(16) . . . . ? C346 C353 C354 C355 178.4(10) . . . . ? C353 C354 C355 C361 -179.6(12) . . . . ? C353 C354 C355 C356 2.2(17) . . . . ? C352 C351 C356 C364 178.9(11) . . . . ? C352 C351 C356 C355 -1.9(16) . . . . ? C361 C355 C356 C364 0.5(17) . . . . ? C354 C355 C356 C364 178.8(10) . . . . ? C361 C355 C356 C351 -178.7(11) . . . . ? C354 C355 C356 C351 -0.5(16) . . . . ? C354 C355 C361 C362 -178.6(13) . . . . ? C356 C355 C361 C362 0(2) . . . . ? C355 C361 C362 C363 0(2) . . . . ? C361 C362 C363 C364 1(2) . . . . ? C362 C363 C364 C356 -1(2) . . . . ? C351 C356 C364 C363 179.2(12) . . . . ? C355 C356 C364 C363 0.1(17) . . . . ? N131 Cd2 N411 C416 97.0(9) . . . . ? N422 Cd2 N411 C416 -175.1(9) . . . . ? N511 Cd2 N411 C416 3.3(9) . . . . ? N522 Cd2 N411 C416 -69.1(9) . . . . ? N142 Cd2 N411 C416 130.7(13) . . . . ? N131 Cd2 N411 C412 -81.0(7) . . . . ? N422 Cd2 N411 C412 7.0(7) . . . . ? N511 Cd2 N411 C412 -174.7(7) . . . . ? N522 Cd2 N411 C412 112.9(7) . . . . ? N142 Cd2 N411 C412 -47.3(16) . . . . ? C416 N411 C412 C413 -1.4(15) . . . . ? Cd2 N411 C412 C413 176.7(8) . . . . ? C416 N411 C412 C423 178.2(9) . . . . ? Cd2 N411 C412 C423 -3.7(11) . . . . ? N411 C412 C413 C414 0.2(16) . . . . ? C423 C412 C413 C414 -179.4(10) . . . . ? C412 C413 C414 C415 1.7(18) . . . . ? C413 C414 C415 C416 -2.2(19) . . . . ? C412 N411 C416 C415 0.8(17) . . . . ? Cd2 N411 C416 C415 -177.2(9) . . . . ? C414 C415 C416 N411 1.0(19) . . . . ? C425 N421 N422 C423 0.0(11) . . . . ? C426 N421 N422 C423 179.6(8) . . . . ? C425 N421 N422 Cd2 160.5(8) . . . . ? C426 N421 N422 Cd2 -20.0(14) . . . . ? N411 Cd2 N422 N421 -169.0(10) . . . . ? N131 Cd2 N422 N421 -70.5(10) . . . . ? N511 Cd2 N422 N421 175(2) . . . . ? N522 Cd2 N422 N421 102.3(10) . . . . ? N142 Cd2 N422 N421 0.0(10) . . . . ? N411 Cd2 N422 C423 -9.3(6) . . . . ? N131 Cd2 N422 C423 89.1(7) . . . . ? N511 Cd2 N422 C423 -25(3) . . . . ? N522 Cd2 N422 C423 -98.1(7) . . . . ? N142 Cd2 N422 C423 159.6(6) . . . . ? N421 N422 C423 C424 0.1(11) . . . . ? Cd2 N422 C423 C424 -166.3(7) . . . . ? N421 N422 C423 C412 177.8(9) . . . . ? Cd2 N422 C423 C412 11.4(11) . . . . ? N411 C412 C423 N422 -5.6(14) . . . . ? C413 C412 C423 N422 173.9(10) . . . . ? N411 C412 C423 C424 171.6(10) . . . . ? C413 C412 C423 C424 -8.9(17) . . . . ? N422 C423 C424 C425 -0.2(12) . . . . ? C412 C423 C424 C425 -177.6(10) . . . . ? C423 C424 C425 N421 0.2(13) . . . . ? N422 N421 C425 C424 -0.1(12) . . . . ? C426 N421 C425 C424 -179.6(10) . . . . ? C425 N421 C426 C452 -72.7(13) . . . . ? N422 N421 C426 C452 107.9(10) . . . . ? N231 Cd3 N431 C432 168.4(8) . . . . ? N611 Cd3 N431 C432 -91.4(9) . . . . ? N622 Cd3 N431 C432 -63.9(17) . . . . ? N442 Cd3 N431 C432 -2.6(8) . . . . ? N242 Cd3 N431 C432 97.4(9) . . . . ? N231 Cd3 N431 C436 -7.2(11) . . . . ? N611 Cd3 N431 C436 93.0(11) . . . . ? N622 Cd3 N431 C436 120.4(15) . . . . ? N442 Cd3 N431 C436 -178.3(11) . . . . ? N242 Cd3 N431 C436 -78.3(11) . . . . ? C436 N431 C432 C433 -3.1(18) . . . . ? Cd3 N431 C432 C433 -178.9(8) . . . . ? C436 N431 C432 C443 -179.0(11) . . . . ? Cd3 N431 C432 C443 5.2(13) . . . . ? N431 C432 C433 C434 3.2(16) . . . . ? C443 C432 C433 C434 179.0(10) . . . . ? C432 C433 C434 C435 -2.7(17) . . . . ? C433 C434 C435 C436 2(2) . . . . ? C432 N431 C436 C435 3(2) . . . . ? Cd3 N431 C436 C435 178.1(10) . . . . ? C434 C435 C436 N431 -2(2) . . . . ? C445 N441 N442 C443 -0.2(11) . . . . ? C446 N441 N442 C443 -177.2(9) . . . . ? C445 N441 N442 Cd3 170.0(8) . . . . ? C446 N441 N442 Cd3 -7.1(15) . . . . ? N431 Cd3 N442 C443 -0.4(7) . . . . ? N231 Cd3 N442 C443 -50(2) . . . . ? N611 Cd3 N442 C443 95.1(7) . . . . ? N622 Cd3 N442 C443 166.5(7) . . . . ? N242 Cd3 N442 C443 -90.4(7) . . . . ? N431 Cd3 N442 N441 -170.0(11) . . . . ? N231 Cd3 N442 N441 140.8(15) . . . . ? N611 Cd3 N442 N441 -74.5(10) . . . . ? N622 Cd3 N442 N441 -3.1(11) . . . . ? N242 Cd3 N442 N441 100.0(10) . . . . ? N441 N442 C443 C444 0.2(12) . . . . ? Cd3 N442 C443 C444 -172.8(7) . . . . ? N441 N442 C443 C432 176.1(9) . . . . ? Cd3 N442 C443 C432 3.1(12) . . . . ? N431 C432 C443 N442 -5.6(15) . . . . ? C433 C432 C443 N442 178.4(10) . . . . ? N431 C432 C443 C444 169.4(11) . . . . ? C433 C432 C443 C444 -6.6(18) . . . . ? N442 C443 C444 C445 -0.1(13) . . . . ? C432 C443 C444 C445 -175.4(11) . . . . ? N442 N441 C445 C444 0.1(12) . . . . ? C446 N441 C445 C444 176.9(9) . . . . ? C443 C444 C445 N441 0.0(12) . . . . ? N442 N441 C446 C453 99.8(11) . . . . ? C445 N441 C446 C453 -76.7(14) . . . . ? C456 C451 C452 C453 -2.3(17) . . . . ? C456 C451 C452 C426 176.4(10) . . . . ? N421 C426 C452 C451 -2.6(14) . . . . ? N421 C426 C452 C453 176.1(8) . . . . ? C451 C452 C453 C454 -0.2(15) . . . . ? C426 C452 C453 C454 -179.0(9) . . . . ? C451 C452 C453 C446 -178.0(10) . . . . ? C426 C452 C453 C446 3.2(13) . . . . ? N441 C446 C453 C454 -1.9(15) . . . . ? N441 C446 C453 C452 175.9(9) . . . . ? C452 C453 C454 C455 3.3(16) . . . . ? C446 C453 C454 C455 -179.0(10) . . . . ? C453 C454 C455 C456 -4.0(17) . . . . ? C453 C454 C455 C461 175.1(11) . . . . ? C454 C455 C456 C451 1.6(17) . . . . ? C461 C455 C456 C451 -177.5(12) . . . . ? C454 C455 C456 C464 -178.3(11) . . . . ? C461 C455 C456 C464 2.6(18) . . . . ? C452 C451 C456 C455 1.6(18) . . . . ? C452 C451 C456 C464 -178.5(12) . . . . ? C456 C455 C461 C462 2(2) . . . . ? C454 C455 C461 C462 -177.0(13) . . . . ? C455 C461 C462 C463 -5(2) . . . . ? C461 C462 C463 C464 2(3) . . . . ? C462 C463 C464 C456 3(2) . . . . ? C455 C456 C464 C463 -5(2) . . . . ? C451 C456 C464 C463 175.1(13) . . . . ? N411 Cd2 N511 C516 97.3(9) . . . . ? N131 Cd2 N511 C516 -1.5(9) . . . . ? N422 Cd2 N511 C516 113(3) . . . . ? N522 Cd2 N511 C516 -172.5(9) . . . . ? N142 Cd2 N511 C516 -72.0(9) . . . . ? N411 Cd2 N511 C512 -96.8(7) . . . . ? N131 Cd2 N511 C512 164.4(7) . . . . ? N422 Cd2 N511 C512 -81(3) . . . . ? N522 Cd2 N511 C512 -6.6(7) . . . . ? N142 Cd2 N511 C512 93.9(7) . . . . ? C516 N511 C512 C513 2.7(15) . . . . ? Cd2 N511 C512 C513 -164.3(8) . . . . ? C516 N511 C512 C523 -178.4(9) . . . . ? Cd2 N511 C512 C523 14.7(11) . . . . ? N511 C512 C513 C514 -2.1(16) . . . . ? C523 C512 C513 C514 178.9(10) . . . . ? C512 C513 C514 C515 0.0(17) . . . . ? C513 C514 C515 C516 1.4(17) . . . . ? C512 N511 C516 C515 -1.1(17) . . . . ? Cd2 N511 C516 C515 164.4(9) . . . . ? C514 C515 C516 N511 -0.9(19) . . . . ? C525 N521 N522 C523 0.6(11) . . . . ? C526 N521 N522 C523 178.9(8) . . . . ? C525 N521 N522 Cd2 161.2(8) . . . . ? C526 N521 N522 Cd2 -20.4(14) . . . . ? N411 Cd2 N522 N521 -60.6(9) . . . . ? N131 Cd2 N522 N521 168.4(9) . . . . ? N422 Cd2 N522 N521 12.1(10) . . . . ? N511 Cd2 N522 N521 -162.0(10) . . . . ? N142 Cd2 N522 N521 114.9(9) . . . . ? N411 Cd2 N522 C523 98.9(7) . . . . ? N131 Cd2 N522 C523 -32.1(13) . . . . ? N422 Cd2 N522 C523 171.5(6) . . . . ? N511 Cd2 N522 C523 -2.5(6) . . . . ? N142 Cd2 N522 C523 -85.6(7) . . . . ? N521 N522 C523 C524 -0.2(11) . . . . ? Cd2 N522 C523 C524 -166.1(7) . . . . ? N521 N522 C523 C512 176.8(8) . . . . ? Cd2 N522 C523 C512 10.8(11) . . . . ? N511 C512 C523 N522 -17.6(14) . . . . ? C513 C512 C523 N522 161.4(9) . . . . ? N511 C512 C523 C524 158.5(11) . . . . ? C513 C512 C523 C524 -22.5(17) . . . . ? N522 C523 C524 C525 -0.3(12) . . . . ? C512 C523 C524 C525 -176.7(11) . . . . ? C523 C524 C525 N521 0.6(12) . . . . ? N522 N521 C525 C524 -0.7(12) . . . . ? C526 N521 C525 C524 -178.9(10) . . . . ? N522 N521 C526 C552 91.1(11) . . . . ? C525 N521 C526 C552 -90.9(13) . . . . ? N631 Cd4 N531 C536 -2.7(9) . . . . ? N331 Cd4 N531 C536 104.6(9) . . . . ? N342 Cd4 N531 C536 120.8(16) . . . . ? N542 Cd4 N531 C536 -176.6(9) . . . . ? N642 Cd4 N531 C536 -72.7(9) . . . . ? N631 Cd4 N531 C532 169.5(7) . . . . ? N331 Cd4 N531 C532 -83.2(7) . . . . ? N342 Cd4 N531 C532 -67.0(19) . . . . ? N542 Cd4 N531 C532 -4.4(7) . . . . ? N642 Cd4 N531 C532 99.4(7) . . . . ? C536 N531 C532 C533 -0.9(15) . . . . ? Cd4 N531 C532 C533 -173.4(8) . . . . ? C536 N531 C532 C543 -179.2(9) . . . . ? Cd4 N531 C532 C543 8.3(11) . . . . ? N531 C532 C533 C534 3.0(16) . . . . ? C543 C532 C533 C534 -178.8(10) . . . . ? C532 C533 C534 C535 -1.8(18) . . . . ? C533 C534 C535 C536 -1.3(18) . . . . ? C532 N531 C536 C535 -2.4(16) . . . . ? Cd4 N531 C536 C535 169.6(8) . . . . ? C534 C535 C536 N531 3.6(18) . . . . ? C545 N541 N542 C543 -1.1(11) . . . . ? C546 N541 N542 C543 -178.6(9) . . . . ? C545 N541 N542 Cd4 170.6(8) . . . . ? C546 N541 N542 Cd4 -6.9(15) . . . . ? N631 Cd4 N542 N541 141.4(18) . . . . ? N531 Cd4 N542 N541 -171.2(10) . . . . ? N331 Cd4 N542 N541 -68.8(10) . . . . ? N342 Cd4 N542 N541 -0.9(10) . . . . ? N642 Cd4 N542 N541 107.8(10) . . . . ? N631 Cd4 N542 C543 -47(2) . . . . ? N531 Cd4 N542 C543 0.0(7) . . . . ? N331 Cd4 N542 C543 102.4(7) . . . . ? N342 Cd4 N542 C543 170.3(7) . . . . ? N642 Cd4 N542 C543 -81.0(7) . . . . ? N541 N542 C543 C544 0.9(11) . . . . ? Cd4 N542 C543 C544 -173.4(7) . . . . ? N541 N542 C543 C532 178.5(9) . . . . ? Cd4 N542 C543 C532 4.3(11) . . . . ? N531 C532 C543 N542 -8.5(14) . . . . ? C533 C532 C543 N542 173.1(10) . . . . ? N531 C532 C543 C544 168.6(10) . . . . ? C533 C532 C543 C544 -9.7(17) . . . . ? N542 C543 C544 C545 -0.3(12) . . . . ? C532 C543 C544 C545 -177.7(11) . . . . ? C543 C544 C545 N541 -0.4(13) . . . . ? N542 N541 C545 C544 0.9(13) . . . . ? C546 N541 C545 C544 178.2(10) . . . . ? N542 N541 C546 C553 99.6(11) . . . . ? C545 N541 C546 C553 -77.4(14) . . . . ? C556 C551 C552 C553 0.3(14) . . . . ? C556 C551 C552 C526 179.4(9) . . . . ? N521 C526 C552 C551 12.9(14) . . . . ? N521 C526 C552 C553 -168.0(9) . . . . ? C551 C552 C553 C554 -2.6(15) . . . . ? C526 C552 C553 C554 178.2(10) . . . . ? C551 C552 C553 C546 -179.5(9) . . . . ? C526 C552 C553 C546 1.3(13) . . . . ? N541 C546 C553 C554 17.3(15) . . . . ? N541 C546 C553 C552 -166.0(9) . . . . ? C552 C553 C554 C555 2.7(16) . . . . ? C546 C553 C554 C555 179.3(10) . . . . ? C553 C554 C555 C561 -179.7(11) . . . . ? C553 C554 C555 C556 -0.4(16) . . . . ? C552 C551 C556 C564 -177.8(10) . . . . ? C552 C551 C556 C555 2.0(15) . . . . ? C561 C555 C556 C564 -2.8(15) . . . . ? C554 C555 C556 C564 177.9(10) . . . . ? C561 C555 C556 C551 177.4(10) . . . . ? C554 C555 C556 C551 -1.9(15) . . . . ? C554 C555 C561 C562 -177.9(11) . . . . ? C556 C555 C561 C562 2.8(17) . . . . ? C555 C561 C562 C563 0.0(18) . . . . ? C561 C562 C563 C564 -2.8(19) . . . . ? C562 C563 C564 C556 2.8(18) . . . . ? C551 C556 C564 C563 179.8(10) . . . . ? C555 C556 C564 C563 0.0(16) . . . . ? N431 Cd3 N611 C616 -0.1(14) . . . . ? N231 Cd3 N611 C616 101.7(13) . . . . ? N622 Cd3 N611 C616 -173.0(14) . . . . ? N442 Cd3 N611 C616 -71.5(13) . . . . ? N242 Cd3 N611 C616 134.7(17) . . . . ? N431 Cd3 N611 C612 169.7(9) . . . . ? N231 Cd3 N611 C612 -88.5(10) . . . . ? N622 Cd3 N611 C612 -3.2(9) . . . . ? N442 Cd3 N611 C612 98.3(9) . . . . ? N242 Cd3 N611 C612 -56(2) . . . . ? C616 N611 C612 C613 -5(2) . . . . ? Cd3 N611 C612 C613 -175.2(11) . . . . ? C616 N611 C612 C623 176.6(14) . . . . ? Cd3 N611 C612 C623 6.2(15) . . . . ? N611 C612 C613 C614 4(2) . . . . ? C623 C612 C613 C614 -177.4(14) . . . . ? C612 C613 C614 C615 -2(3) . . . . ? C613 C614 C615 C616 0(3) . . . . ? C612 N611 C616 C615 3(3) . . . . ? Cd3 N611 C616 C615 173.0(14) . . . . ? C614 C615 C616 N611 -1(3) . . . . ? C625 N621 N622 C623 -1.9(12) . . . . ? C626 N621 N622 C623 -179.7(9) . . . . ? C625 N621 N622 Cd3 170.9(9) . . . . ? C626 N621 N622 Cd3 -6.9(16) . . . . ? N431 Cd3 N622 C623 -29.3(18) . . . . ? N231 Cd3 N622 C623 99.6(8) . . . . ? N611 Cd3 N622 C623 -0.4(8) . . . . ? N442 Cd3 N622 C623 -87.2(8) . . . . ? N242 Cd3 N622 C623 169.7(8) . . . . ? N431 Cd3 N622 N621 158.5(12) . . . . ? N231 Cd3 N622 N621 -72.6(11) . . . . ? N611 Cd3 N622 N621 -172.6(12) . . . . ? N442 Cd3 N622 N621 100.6(11) . . . . ? N242 Cd3 N622 N621 -2.5(11) . . . . ? N621 N622 C623 C624 3.1(12) . . . . ? Cd3 N622 C623 C624 -171.8(8) . . . . ? N621 N622 C623 C612 178.6(10) . . . . ? Cd3 N622 C623 C612 3.7(14) . . . . ? N611 C612 C623 N622 -6.8(17) . . . . ? C613 C612 C623 N622 174.6(12) . . . . ? N611 C612 C623 C624 167.7(12) . . . . ? C613 C612 C623 C624 -11(2) . . . . ? N622 C623 C624 C625 -3.2(14) . . . . ? C612 C623 C624 C625 -178.1(13) . . . . ? C623 C624 C625 N621 1.9(14) . . . . ? N622 N621 C625 C624 -0.1(14) . . . . ? C626 N621 C625 C624 177.4(11) . . . . ? C625 N621 C626 C652 -77.5(15) . . . . ? N622 N621 C626 C652 99.8(11) . . . . ? N531 Cd4 N631 C636 108.8(8) . . . . ? N331 Cd4 N631 C636 5.5(9) . . . . ? N342 Cd4 N631 C636 -62.3(8) . . . . ? N542 Cd4 N631 C636 154.5(18) . . . . ? N642 Cd4 N631 C636 -170.7(9) . . . . ? N531 Cd4 N631 C632 -75.8(8) . . . . ? N331 Cd4 N631 C632 -179.1(7) . . . . ? N342 Cd4 N631 C632 113.1(7) . . . . ? N542 Cd4 N631 C632 -30(2) . . . . ? N642 Cd4 N631 C632 4.7(7) . . . . ? C636 N631 C632 C633 -1.7(15) . . . . ? Cd4 N631 C632 C633 -177.4(9) . . . . ? C636 N631 C632 C643 177.7(9) . . . . ? Cd4 N631 C632 C643 2.0(12) . . . . ? N631 C632 C633 C634 1.7(18) . . . . ? C643 C632 C633 C634 -177.7(11) . . . . ? C632 C633 C634 C635 -0.2(19) . . . . ? C633 C634 C635 C636 -1.1(18) . . . . ? C632 N631 C636 C635 0.4(17) . . . . ? Cd4 N631 C636 C635 175.7(9) . . . . ? C634 C635 C636 N631 1.0(18) . . . . ? C645 N641 N642 C643 1.9(12) . . . . ? C646 N641 N642 C643 178.3(9) . . . . ? C645 N641 N642 Cd4 157.3(8) . . . . ? C646 N641 N642 Cd4 -26.4(16) . . . . ? N631 Cd4 N642 N641 -165.8(11) . . . . ? N531 Cd4 N642 N641 -61.1(10) . . . . ? N331 Cd4 N642 N641 149(3) . . . . ? N342 Cd4 N642 N641 116.3(10) . . . . ? N542 Cd4 N642 N641 9.4(10) . . . . ? N631 Cd4 N642 C643 -11.3(7) . . . . ? N531 Cd4 N642 C643 93.4(7) . . . . ? N331 Cd4 N642 C643 -56(4) . . . . ? N342 Cd4 N642 C643 -89.2(7) . . . . ? N542 Cd4 N642 C643 163.9(7) . . . . ? N641 N642 C643 C644 -3.2(12) . . . . ? Cd4 N642 C643 C644 -165.7(7) . . . . ? N641 N642 C643 C632 179.6(9) . . . . ? Cd4 N642 C643 C632 17.1(11) . . . . ? N631 C632 C643 N642 -13.7(14) . . . . ? C633 C632 C643 N642 165.7(10) . . . . ? N631 C632 C643 C644 169.7(11) . . . . ? C633 C632 C643 C644 -10.9(18) . . . . ? N642 C643 C644 C645 3.2(13) . . . . ? C632 C643 C644 C645 -179.9(11) . . . . ? C643 C644 C645 N641 -1.9(13) . . . . ? N642 N641 C645 C644 0.1(13) . . . . ? C646 N641 C645 C644 -176.1(10) . . . . ? N642 N641 C646 C653 110.4(11) . . . . ? C645 N641 C646 C653 -73.9(14) . . . . ? C656 C651 C652 C653 1.3(16) . . . . ? C656 C651 C652 C626 178.6(10) . . . . ? N621 C626 C652 C651 3.9(15) . . . . ? N621 C626 C652 C653 -178.7(9) . . . . ? C651 C652 C653 C654 0.1(16) . . . . ? C626 C652 C653 C654 -177.3(10) . . . . ? C651 C652 C653 C646 -177.9(10) . . . . ? C626 C652 C653 C646 4.7(14) . . . . ? N641 C646 C653 C654 6.7(16) . . . . ? N641 C646 C653 C652 -175.3(9) . . . . ? C652 C653 C654 C655 -1.8(17) . . . . ? C646 C653 C654 C655 176.0(10) . . . . ? C653 C654 C655 C656 2.1(17) . . . . ? C653 C654 C655 C661 -179.3(11) . . . . ? C654 C655 C656 C651 -0.7(16) . . . . ? C661 C655 C656 C651 -179.3(11) . . . . ? C654 C655 C656 C664 179.0(11) . . . . ? C661 C655 C656 C664 0.4(17) . . . . ? C652 C651 C656 C655 -1.0(17) . . . . ? C652 C651 C656 C664 179.4(12) . . . . ? C656 C655 C661 C662 0.3(19) . . . . ? C654 C655 C661 C662 -178.3(13) . . . . ? C655 C661 C662 C663 -1(2) . . . . ? C661 C662 C663 C664 1(3) . . . . ? C662 C663 C664 C656 -1(2) . . . . ? C655 C656 C664 C663 0(2) . . . . ? C651 C656 C664 C663 179.5(13) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.599 _refine_diff_density_min -1.409 _refine_diff_density_rms 0.179 #===END data_ssh0399 _database_code_depnum_ccdc_archive 'CCDC 708985' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C168 H132 F24 N36 Si4 Zn4' _chemical_formula_weight 3484.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 32.973(10) _cell_length_b 32.973(10) _cell_length_c 32.973(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 35849(19) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9687 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 24.97 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14272 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8882 _exptl_absorpt_correction_T_max 0.9447 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6926 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD diffractometer' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 191194 _diffrn_reflns_av_R_equivalents 0.1191 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 22.49 _reflns_number_total 8337 _reflns_number_gt 4002 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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 processing was conducted to a resolution of 45 degrees 2Theta as the data was only complete to this resolution. The structure is of a [Zn4L6][SiF6]4 host-guest cage. All five and six membered rings have benefited from the application of geometric restraints. Given this it was felt inappropriate to make all carbon and nitrogen atoms anisotropic and so they have been left isotropic, with only the heaviest atoms anisotropic (Zn and Si) The encapsulated counter-ion Si11 F12 F13 is disordered with respect to the positioning of the fluorine atoms. Where possible geometric and displacement restraints have been applied to improve the appearance of this residue (that resides on a special position). The counter-ion Si21 F22 > F27 is also highly disordered and has been and has been treated in a similar manner. The lattice contained at least two highly disordered MeOH and two highly disordered H2O solvent molecules. These could to be modelled satisfactorily given their highly fluxional nature and their positioning on special positions. As a result the corresponding electron density was removed using a 'SQUEEZE' function has been used to eliminate a volume of ca. 8000 angstroms loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.023 -0.019 -0.022 7868 1057 ' ' _platon_squeeze_details The final R1 value is higher than would normally be acceptable at ca 0.16 Attempts to obtain a better data set were hampered by the weakly diffracting nature of the crystals, presumably due to the large number of voids present in the structure and lattice and the high disorder arising from a combination of fluxional solvent molecules and counter-ions. The high concentration of solvent molecules resulted in a rapid loss of crystallinity when the crystallinity were removed from the mother liquor adding further complication. Given these factors we feel that the R1 value obtained for this structure is reasonable. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8337 _refine_ls_number_parameters 247 _refine_ls_number_restraints 117 _refine_ls_R_factor_all 0.2315 _refine_ls_R_factor_gt 0.1578 _refine_ls_wR_factor_ref 0.4761 _refine_ls_wR_factor_gt 0.4413 _refine_ls_goodness_of_fit_ref 1.518 _refine_ls_restrained_S_all 1.510 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.54158(5) 0.04031(4) 0.24975(5) 0.1201(7) Uani 1 1 d . . . Zn2 Zn 0.74875(4) 0.24875(4) 0.25125(4) 0.1036(9) Uani 1 3 d S . . N111 N 0.5307(3) 0.3148(2) 0.4526(3) 0.142(4) Uiso 1 1 d G . . C112 C 0.5309(3) 0.3285(3) 0.4127(3) 0.134(4) Uiso 1 1 d G . . C113 C 0.5316(3) 0.3699(3) 0.4047(3) 0.152(5) Uiso 1 1 d G . . H113 H 0.5317 0.3792 0.3774 0.182 Uiso 1 1 calc R . . C114 C 0.5321(3) 0.3976(2) 0.4364(4) 0.195(7) Uiso 1 1 d G . . H114 H 0.5325 0.4258 0.4309 0.233 Uiso 1 1 calc R . . C115 C 0.5319(4) 0.3839(3) 0.4763(3) 0.174(6) Uiso 1 1 d G . . H115 H 0.5323 0.4028 0.4980 0.209 Uiso 1 1 calc R . . C116 C 0.5313(3) 0.3425(4) 0.4844(2) 0.192(7) Uiso 1 1 d G . . H116 H 0.5312 0.3331 0.5116 0.231 Uiso 1 1 calc R . . N121 N 0.5277(2) 0.23566(18) 0.3578(2) 0.114(3) Uiso 1 1 d G . . N122 N 0.5328(2) 0.2592(2) 0.39355(18) 0.115(3) Uiso 1 1 d G . . C123 C 0.5294(3) 0.3007(2) 0.3827(3) 0.125(4) Uiso 1 1 d G . . C124 C 0.5222(3) 0.3029(2) 0.3403(3) 0.145(5) Uiso 1 1 d G . . H124 H 0.5187 0.3270 0.3250 0.174 Uiso 1 1 calc R . . C125 C 0.5212(3) 0.2627(3) 0.32494(18) 0.139(5) Uiso 1 1 d G . . H125 H 0.5168 0.2552 0.2975 0.167 Uiso 1 1 calc R . . C126 C 0.5301(3) 0.1927(3) 0.3568(3) 0.103(3) Uiso 1 1 d . . . H12A H 0.5447 0.1835 0.3814 0.123 Uiso 1 1 calc R . . H12B H 0.5466 0.1847 0.3330 0.123 Uiso 1 1 calc R . . N131 N 0.5403(3) -0.0220(2) 0.2657(3) 0.140(4) Uiso 1 1 d G . . C132 C 0.5367(3) -0.0306(3) 0.3068(3) 0.119(4) Uiso 1 1 d G . . C133 C 0.5351(3) -0.0707(3) 0.3199(2) 0.163(6) Uiso 1 1 d G . . H133 H 0.5326 -0.0766 0.3480 0.195 Uiso 1 1 calc R . . C134 C 0.5373(3) -0.1021(2) 0.2918(4) 0.176(6) Uiso 1 1 d G . . H134 H 0.5362 -0.1295 0.3008 0.211 Uiso 1 1 calc R . . C135 C 0.5409(3) -0.0935(3) 0.2507(3) 0.170(6) Uiso 1 1 d G . . H135 H 0.5424 -0.1149 0.2316 0.204 Uiso 1 1 calc R . . C136 C 0.5425(3) -0.0534(3) 0.2377(2) 0.179(7) Uiso 1 1 d G . . H136 H 0.5450 -0.0475 0.2096 0.215 Uiso 1 1 calc R . . N141 N 0.5339(3) 0.06885(19) 0.3471(3) 0.128(3) Uiso 1 1 d G . . N142 N 0.5371(2) 0.0406(2) 0.31478(19) 0.106(3) Uiso 1 1 d G . . C143 C 0.5327(3) 0.00101(19) 0.3312(3) 0.129(4) Uiso 1 1 d G . . C144 C 0.5269(3) 0.0048(3) 0.3737(3) 0.152(5) Uiso 1 1 d G . . H144 H 0.5231 -0.0168 0.3923 0.182 Uiso 1 1 calc R . . C145 C 0.5276(3) 0.0468(3) 0.38353(19) 0.153(5) Uiso 1 1 d G . . H145 H 0.5244 0.0581 0.4098 0.184 Uiso 1 1 calc R . . C146 C 0.5341(3) 0.1116(3) 0.3416(4) 0.105(3) Uiso 1 1 d . . . H14A H 0.5443 0.1180 0.3140 0.126 Uiso 1 1 calc R . . H14B H 0.5529 0.1241 0.3614 0.126 Uiso 1 1 calc R . . C151 C 0.4535(2) 0.19003(17) 0.3601(2) 0.114(4) Uiso 1 1 d G . . H151 H 0.4523 0.2183 0.3655 0.137 Uiso 1 1 calc R . . C152 C 0.49085(17) 0.1712(2) 0.3547(2) 0.094(3) Uiso 1 1 d G . . C153 C 0.49264(16) 0.1298(2) 0.3467(2) 0.098(3) Uiso 1 1 d G . . C154 C 0.4571(2) 0.10734(17) 0.3440(2) 0.114(4) Uiso 1 1 d G . . H154 H 0.4583 0.0791 0.3386 0.137 Uiso 1 1 calc R . . C155 C 0.41976(17) 0.1262(2) 0.3494(2) 0.113(4) Uiso 1 1 d GD . . C156 C 0.41797(16) 0.1675(2) 0.3574(2) 0.118(4) Uiso 1 1 d GD . . C161 C 0.38413(19) 0.1041(2) 0.3447(4) 0.150(5) Uiso 1 1 d D . . H161 H 0.3852 0.0768 0.3356 0.180 Uiso 1 1 calc R . . C162 C 0.34697(17) 0.1221(4) 0.3533(5) 0.156(5) Uiso 1 1 d D . . H162 H 0.3228 0.1065 0.3523 0.187 Uiso 1 1 calc R . . C163 C 0.34534(18) 0.1630(4) 0.3635(4) 0.152(5) Uiso 1 1 d D . . H163 H 0.3199 0.1756 0.3681 0.182 Uiso 1 1 calc R . . C164 C 0.38090(19) 0.1854(2) 0.3668(4) 0.150(5) Uiso 1 1 d D . . H164 H 0.3799 0.2129 0.3754 0.180 Uiso 1 1 calc R . . N211 N 0.81189(18) 0.2379(2) 0.2479(2) 0.105(3) Uiso 1 1 d G . . C212 C 0.8229(2) 0.1978(2) 0.2410(2) 0.117(4) Uiso 1 1 d G . . C213 C 0.8636(3) 0.1869(2) 0.2400(3) 0.131(4) Uiso 1 1 d G . . H213 H 0.8711 0.1595 0.2353 0.158 Uiso 1 1 calc R . . C214 C 0.89334(18) 0.2162(3) 0.2458(3) 0.144(5) Uiso 1 1 d G . . H214 H 0.9212 0.2088 0.2452 0.173 Uiso 1 1 calc R . . C215 C 0.8824(2) 0.2563(3) 0.2527(3) 0.148(5) Uiso 1 1 d G . . H215 H 0.9027 0.2763 0.2567 0.178 Uiso 1 1 calc R . . C216 C 0.8416(3) 0.26717(19) 0.2537(3) 0.138(5) Uiso 1 1 d G . . H216 H 0.8342 0.2946 0.2584 0.166 Uiso 1 1 calc R . . N221 N 0.72618(17) 0.1496(2) 0.2381(2) 0.115(3) Uiso 1 1 d G . . N222 N 0.7521(2) 0.18371(17) 0.2428(2) 0.105(3) Uiso 1 1 d G . . C223 C 0.79279(18) 0.1701(2) 0.2389(3) 0.105(3) Uiso 1 1 d G . . C224 C 0.7920(2) 0.1276(2) 0.2317(3) 0.123(4) Uiso 1 1 d G . . H224 H 0.8150 0.1107 0.2279 0.147 Uiso 1 1 calc R . . C225 C 0.7508(3) 0.11500(17) 0.2313(3) 0.133(4) Uiso 1 1 d G . . H225 H 0.7414 0.0881 0.2271 0.159 Uiso 1 1 calc R . . C226 C 0.6849(3) 0.1533(3) 0.2394(3) 0.102(3) Uiso 1 1 d . . . H22A H 0.6778 0.1802 0.2508 0.122 Uiso 1 1 calc R . . H22B H 0.6738 0.1324 0.2579 0.122 Uiso 1 1 calc R . . N231 N 0.4778(2) 0.0491(3) 0.2457(2) 0.129(3) Uiso 1 1 d G . . C232 C 0.4657(2) 0.0883(2) 0.2361(2) 0.108(3) Uiso 1 1 d G . . C233 C 0.4247(3) 0.0971(2) 0.2314(3) 0.128(4) Uiso 1 1 d G . . H233 H 0.4164 0.1239 0.2248 0.154 Uiso 1 1 calc R . . C234 C 0.39591(19) 0.0667(3) 0.2362(3) 0.159(5) Uiso 1 1 d G . . H234 H 0.3679 0.0727 0.2330 0.190 Uiso 1 1 calc R . . C235 C 0.4081(3) 0.0275(3) 0.2458(3) 0.152(5) Uiso 1 1 d G . . H235 H 0.3884 0.0067 0.2491 0.183 Uiso 1 1 calc R . . C236 C 0.4490(3) 0.0187(2) 0.2506(3) 0.154(5) Uiso 1 1 d G . . H236 H 0.4573 -0.0081 0.2571 0.185 Uiso 1 1 calc R . . N241 N 0.56088(17) 0.1386(2) 0.2351(2) 0.118(3) Uiso 1 1 d G . . N242 N 0.5356(2) 0.10399(17) 0.2395(2) 0.105(3) Uiso 1 1 d G . . C243 C 0.49473(18) 0.1167(2) 0.2351(3) 0.116(4) Uiso 1 1 d G . . C244 C 0.4947(2) 0.1592(2) 0.2281(3) 0.123(4) Uiso 1 1 d G . . H244 H 0.4714 0.1757 0.2241 0.147 Uiso 1 1 calc R . . C245 C 0.5356(2) 0.17274(17) 0.2281(3) 0.113(4) Uiso 1 1 d G . . H245 H 0.5444 0.1999 0.2241 0.135 Uiso 1 1 calc R . . C246 C 0.6032(3) 0.1379(4) 0.2374(3) 0.111(4) Uiso 1 1 d . . . H24A H 0.6116 0.1127 0.2514 0.134 Uiso 1 1 calc R . . H24B H 0.6123 0.1611 0.2542 0.134 Uiso 1 1 calc R . . C251 C 0.68640(17) 0.1517(2) 0.1618(2) 0.113(4) Uiso 1 1 d G . . H251 H 0.7146 0.1577 0.1620 0.135 Uiso 1 1 calc R . . C252 C 0.6651(2) 0.1488(2) 0.19802(17) 0.105(3) Uiso 1 1 d G . . C253 C 0.6239(2) 0.1399(2) 0.19761(17) 0.099(3) Uiso 1 1 d G . . C254 C 0.60398(17) 0.1339(2) 0.1609(2) 0.111(4) Uiso 1 1 d G . . H254 H 0.5758 0.1279 0.1607 0.134 Uiso 1 1 calc R . . C255 C 0.6253(2) 0.1368(2) 0.12467(17) 0.115(4) Uiso 1 1 d GD . . C256 C 0.6665(2) 0.1457(2) 0.12508(17) 0.122(4) Uiso 1 1 d GD . . C261 C 0.6065(2) 0.1298(4) 0.08752(19) 0.141(5) Uiso 1 1 d D . . H261 H 0.5782 0.1243 0.0864 0.169 Uiso 1 1 calc R . . C262 C 0.6292(3) 0.1310(4) 0.05200(18) 0.143(5) Uiso 1 1 d D . . H262 H 0.6163 0.1252 0.0269 0.172 Uiso 1 1 calc R . . C263 C 0.6703(3) 0.1403(4) 0.05234(18) 0.147(5) Uiso 1 1 d D . . H263 H 0.6856 0.1404 0.0279 0.176 Uiso 1 1 calc R . . C264 C 0.6885(2) 0.1494(4) 0.0893(2) 0.142(5) Uiso 1 1 d D . . H264 H 0.7159 0.1582 0.0900 0.170 Uiso 1 1 calc R . . Si11 Si 0.64682(8) 0.14682(8) 0.35318(8) 0.0799(13) Uani 1 3 d SD . . F12X F 0.6145(3) 0.1730(4) 0.3795(3) 0.120(6) Uiso 0.536(18) 1 d PDU A 1 F13X F 0.6465(8) 0.1785(7) 0.3156(4) 0.299(15) Uiso 0.536(18) 1 d PDU A 1 F12Y F 0.6101(5) 0.1381(6) 0.3847(5) 0.186(11) Uiso 0.464(18) 1 d PDU A 2 F13Y F 0.6182(4) 0.1717(4) 0.3220(3) 0.118(6) Uiso 0.464(18) 1 d PDU A 2 Si21 Si 0.99577(9) 0.28378(9) 0.28978(9) 0.1036(11) Uani 1 1 d D . . F22 F 0.97712(18) 0.24912(18) 0.25907(18) 0.151(3) Uiso 1 1 d D B . F23 F 1.01445(18) 0.31842(19) 0.32046(19) 0.168(3) Uiso 1 1 d D B . F24X F 0.9665(3) 0.2663(3) 0.3257(2) 0.152(7) Uiso 0.484(13) 1 d PDU B 1 F25X F 0.9597(3) 0.3145(2) 0.2754(3) 0.131(6) Uiso 0.484(13) 1 d PDU B 1 F26X F 1.0243(3) 0.2999(3) 0.2527(2) 0.198(9) Uiso 0.484(13) 1 d PDU B 1 F27X F 1.0311(3) 0.2517(2) 0.3030(3) 0.154(7) Uiso 0.484(13) 1 d PDU B 1 F24Y F 0.94976(19) 0.2935(3) 0.3052(3) 0.146(6) Uiso 0.516(13) 1 d PDU B 2 F25Y F 0.9907(4) 0.3172(2) 0.2536(2) 0.180(8) Uiso 0.516(13) 1 d PDU B 2 F26Y F 1.0411(2) 0.2727(3) 0.2731(3) 0.175(7) Uiso 0.516(13) 1 d PDU B 2 F27Y F 1.0002(4) 0.2490(2) 0.3247(2) 0.194(8) Uiso 0.516(13) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.1136(12) 0.0992(11) 0.1474(14) -0.0226(9) -0.0229(9) 0.0134(8) Zn2 0.1036(9) 0.1036(9) 0.1036(9) -0.0028(7) -0.0028(7) 0.0028(7) Si11 0.0799(13) 0.0799(13) 0.0799(13) -0.0026(14) -0.0026(14) 0.0026(14) Si21 0.095(2) 0.097(2) 0.119(3) -0.0108(18) 0.0003(18) 0.0043(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N131 2.121(7) . ? Zn1 N231 2.127(7) . ? Zn1 N242 2.136(6) . ? Zn1 N142 2.149(6) . ? Zn1 N111 2.161(8) 8_645 ? Zn1 N122 2.17(5) 8_645 ? Zn2 N211 2.115(6) 8_645 ? Zn2 N211 2.115(6) . ? Zn2 N211 2.115(6) 11_556 ? Zn2 N222 2.166(13) 11_556 ? Zn2 N222 2.166(13) 8_645 ? Zn2 N222 2.166(6) . ? N111 C112 1.3900 . ? N111 C116 1.3900 . ? N111 Zn1 2.161(8) 11_556 ? C112 C123 1.349(9) . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C113 H113 0.9500 . ? C114 C115 1.3900 . ? C114 H114 0.9500 . ? C115 C116 1.3900 . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 C126 1.419(12) . ? N121 N122 1.4200 . ? N121 C125 1.4200 . ? N122 C123 1.4200 . ? N122 Zn1 2.173(6) 11_556 ? C123 C124 1.4200 . ? C124 C125 1.4200 . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? C126 C152 1.478(11) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? N131 C132 1.3900 . ? N131 C136 1.3900 . ? C132 C143 1.324(9) . ? C132 C133 1.3900 . ? C133 C134 1.3900 . ? C133 H133 0.9500 . ? C134 C135 1.3900 . ? C134 H134 0.9500 . ? C135 C136 1.3900 . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? N141 C145 1.4200 . ? N141 N142 1.4200 . ? N141 C146 1.423(12) . ? N142 C143 1.4200 . ? C143 C144 1.4200 . ? C144 C145 1.4200 . ? C144 H144 0.9500 . ? C145 H145 0.9500 . ? C146 C153 1.504(11) . ? C146 H14A 0.9900 . ? C146 H14B 0.9900 . ? C151 C152 1.3900 . ? C151 C156 1.3900 . ? C151 H151 0.9500 . ? C152 C153 1.3900 . ? C153 C154 1.3900 . ? C154 C155 1.3900 . ? C154 H154 0.9500 . ? C155 C156 1.3900 . ? C155 C161 1.3909(19) . ? C156 C164 1.3914(19) . ? C161 C162 1.3905(19) . ? C161 H161 0.9500 . ? C162 C163 1.390(2) . ? C162 H162 0.9500 . ? C163 C164 1.3906(19) . ? C163 H163 0.9500 . ? C164 H164 0.9500 . ? N211 C212 1.3900 . ? N211 C216 1.3900 . ? C212 C223 1.349(8) . ? C212 C213 1.3900 . ? C213 C214 1.3900 . ? C213 H213 0.9500 . ? C214 C215 1.3900 . ? C214 H214 0.9500 . ? C215 C216 1.3900 . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? N221 C226 1.368(11) . ? N221 N222 1.4200 . ? N221 C225 1.4200 . ? N222 C223 1.4200 . ? C223 C224 1.4200 . ? C224 C225 1.4200 . ? C224 H224 0.9500 . ? C225 H225 0.9500 . ? C226 C252 1.521(11) . ? C226 H22A 0.9900 . ? C226 H22B 0.9900 . ? N231 C232 1.3900 . ? N231 C236 1.3900 . ? C232 C243 1.341(8) . ? C232 C233 1.3900 . ? C233 C234 1.3900 . ? C233 H233 0.9500 . ? C234 C235 1.3900 . ? C234 H234 0.9500 . ? C235 C236 1.3900 . ? C235 H235 0.9500 . ? C236 H236 0.9500 . ? N241 C246 1.397(12) . ? N241 N242 1.4200 . ? N241 C245 1.4200 . ? N242 C243 1.4200 . ? C243 C244 1.4200 . ? C244 C245 1.4200 . ? C244 H244 0.9500 . ? C245 H245 0.9500 . ? C246 C253 1.481(12) . ? C246 H24A 0.9900 . ? C246 H24B 0.9900 . ? C251 C252 1.3900 . ? C251 C256 1.3900 . ? C251 H251 0.9500 . ? C252 C253 1.3900 . ? C253 C254 1.3900 . ? C254 C255 1.3900 . ? C254 H254 0.9500 . ? C255 C256 1.3900 . ? C255 C261 1.3917(19) . ? C256 C264 1.3908(19) . ? C261 C262 1.3905(19) . ? C261 H261 0.9500 . ? C262 C263 1.389(2) . ? C262 H262 0.9500 . ? C263 C264 1.3903(19) . ? C263 H263 0.9500 . ? C264 H264 0.9500 . ? Si11 F12Y 1.621(6) 11_556 ? Si11 F12Y 1.621(6) 8_645 ? Si11 F12Y 1.621(6) . ? Si11 F13Y 1.621(6) 11_556 ? Si11 F13Y 1.621(6) . ? Si11 F13Y 1.621(6) 8_645 ? Si11 F13X 1.621(7) 11_556 ? Si11 F13X 1.621(7) . ? Si11 F13X 1.621(7) 8_645 ? Si11 F12X 1.621(6) 8_645 ? Si11 F12X 1.621(6) 11_556 ? Si11 F12X 1.621(6) . ? F13X F13X 1.65(4) 11_556 ? F13X F13X 1.65(4) 8_645 ? F12Y F12Y 1.20(3) 8_645 ? F12Y F12Y 1.20(3) 11_556 ? Si21 F25X 1.632(6) . ? Si21 F24Y 1.632(6) . ? Si21 F24X 1.632(6) . ? Si21 F27Y 1.632(6) . ? Si21 F26X 1.632(6) . ? Si21 F27X 1.632(6) . ? Si21 F26Y 1.633(6) . ? Si21 F25Y 1.633(6) . ? Si21 F23 1.645(6) . ? Si21 F22 1.646(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N131 Zn1 N231 97.4(3) . . ? N131 Zn1 N242 171.8(3) . . ? N231 Zn1 N242 76.4(3) . . ? N131 Zn1 N142 75.8(3) . . ? N231 Zn1 N142 89.6(3) . . ? N242 Zn1 N142 98.5(3) . . ? N131 Zn1 N111 96.0(4) . 8_645 ? N231 Zn1 N111 92.6(4) . 8_645 ? N242 Zn1 N111 89.7(3) . 8_645 ? N142 Zn1 N111 171.8(3) . 8_645 ? N131 Zn1 N122 86.7(14) . 8_645 ? N231 Zn1 N122 168.6(8) . 8_645 ? N242 Zn1 N122 100.4(14) . 8_645 ? N142 Zn1 N122 101.7(7) . 8_645 ? N111 Zn1 N122 76.3(6) 8_645 8_645 ? N211 Zn2 N211 97.1(3) 8_645 . ? N211 Zn2 N211 97.1(3) 8_645 11_556 ? N211 Zn2 N211 97.1(3) . 11_556 ? N211 Zn2 N222 86.2(6) 8_645 11_556 ? N211 Zn2 N222 173.6(5) . 11_556 ? N211 Zn2 N222 77.0(5) 11_556 11_556 ? N211 Zn2 N222 77.0(6) 8_645 8_645 ? N211 Zn2 N222 86.2(6) . 8_645 ? N211 Zn2 N222 173.6(6) 11_556 8_645 ? N222 Zn2 N222 99.9(6) 11_556 8_645 ? N211 Zn2 N222 173.6(3) 8_645 . ? N211 Zn2 N222 77.0(3) . . ? N211 Zn2 N222 86.2(3) 11_556 . ? N222 Zn2 N222 99.9(6) 11_556 . ? N222 Zn2 N222 99.9(6) 8_645 . ? C112 N111 C116 120.0 . . ? C112 N111 Zn1 113.8(6) . 11_556 ? C116 N111 Zn1 125.3(6) . 11_556 ? C123 C112 N111 118.2(8) . . ? C123 C112 C113 121.8(8) . . ? N111 C112 C113 120.0 . . ? C114 C113 C112 120.0 . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C113 C114 C115 120.0 . . ? C113 C114 H114 120.0 . . ? C115 C114 H114 120.0 . . ? C114 C115 C116 120.0 . . ? C114 C115 H115 120.0 . . ? C116 C115 H115 120.0 . . ? C115 C116 N111 120.0 . . ? C115 C116 H116 120.0 . . ? N111 C116 H116 120.0 . . ? C126 N121 N122 123.9(7) . . ? C126 N121 C125 128.1(7) . . ? N122 N121 C125 108.0 . . ? C123 N122 N121 108.0 . . ? C123 N122 Zn1 112.8(5) . 11_556 ? N121 N122 Zn1 139.1(5) . 11_556 ? C112 C123 N122 117.9(8) . . ? C112 C123 C124 133.9(8) . . ? N122 C123 C124 108.0 . . ? C123 C124 C125 108.0 . . ? C123 C124 H124 126.0 . . ? C125 C124 H124 126.0 . . ? C124 C125 N121 108.0 . . ? C124 C125 H125 126.0 . . ? N121 C125 H125 126.0 . . ? N121 C126 C152 115.6(8) . . ? N121 C126 H12A 108.4 . . ? C152 C126 H12A 108.4 . . ? N121 C126 H12B 108.4 . . ? C152 C126 H12B 108.4 . . ? H12A C126 H12B 107.4 . . ? C132 N131 C136 120.0 . . ? C132 N131 Zn1 116.2(6) . . ? C136 N131 Zn1 123.8(6) . . ? C143 C132 N131 116.1(8) . . ? C143 C132 C133 123.8(8) . . ? N131 C132 C133 120.0 . . ? C134 C133 C132 120.0 . . ? C134 C133 H133 120.0 . . ? C132 C133 H133 120.0 . . ? C135 C134 C133 120.0 . . ? C135 C134 H134 120.0 . . ? C133 C134 H134 120.0 . . ? C134 C135 C136 120.0 . . ? C134 C135 H135 120.0 . . ? C136 C135 H135 120.0 . . ? C135 C136 N131 120.0 . . ? C135 C136 H136 120.0 . . ? N131 C136 H136 120.0 . . ? C145 N141 N142 108.0 . . ? C145 N141 C146 128.2(8) . . ? N142 N141 C146 123.7(8) . . ? C143 N142 N141 108.0 . . ? C143 N142 Zn1 112.6(5) . . ? N141 N142 Zn1 139.2(5) . . ? C132 C143 N142 118.8(8) . . ? C132 C143 C144 133.1(8) . . ? N142 C143 C144 108.0 . . ? C145 C144 C143 108.0 . . ? C145 C144 H144 126.0 . . ? C143 C144 H144 126.0 . . ? C144 C145 N141 108.0 . . ? C144 C145 H145 126.0 . . ? N141 C145 H145 126.0 . . ? N141 C146 C153 112.1(8) . . ? N141 C146 H14A 109.2 . . ? C153 C146 H14A 109.2 . . ? N141 C146 H14B 109.2 . . ? C153 C146 H14B 109.2 . . ? H14A C146 H14B 107.9 . . ? C152 C151 C156 120.0 . . ? C152 C151 H151 120.0 . . ? C156 C151 H151 120.0 . . ? C151 C152 C153 120.0 . . ? C151 C152 C126 123.7(6) . . ? C153 C152 C126 116.3(6) . . ? C152 C153 C154 120.0 . . ? C152 C153 C146 116.8(6) . . ? C154 C153 C146 123.2(6) . . ? C155 C154 C153 120.0 . . ? C155 C154 H154 120.0 . . ? C153 C154 H154 120.0 . . ? C154 C155 C156 120.0 . . ? C154 C155 C161 120.0(5) . . ? C156 C155 C161 119.9(5) . . ? C155 C156 C151 120.0 . . ? C155 C156 C164 119.6(5) . . ? C151 C156 C164 120.0(5) . . ? C162 C161 C155 119.9(2) . . ? C162 C161 H161 120.1 . . ? C155 C161 H161 120.1 . . ? C163 C162 C161 119.8(5) . . ? C163 C162 H162 120.1 . . ? C161 C162 H162 120.1 . . ? C162 C163 C164 120.1(5) . . ? C162 C163 H163 119.9 . . ? C164 C163 H163 119.9 . . ? C163 C164 C156 119.9(2) . . ? C163 C164 H164 120.1 . . ? C156 C164 H164 120.1 . . ? C212 N211 C216 120.0 . . ? C212 N211 Zn2 115.2(4) . . ? C216 N211 Zn2 124.7(4) . . ? C223 C212 N211 117.5(7) . . ? C223 C212 C213 122.3(7) . . ? N211 C212 C213 120.0 . . ? C212 C213 C214 120.0 . . ? C212 C213 H213 120.0 . . ? C214 C213 H213 120.0 . . ? C215 C214 C213 120.0 . . ? C215 C214 H214 120.0 . . ? C213 C214 H214 120.0 . . ? C214 C215 C216 120.0 . . ? C214 C215 H215 120.0 . . ? C216 C215 H215 120.0 . . ? C215 C216 N211 120.0 . . ? C215 C216 H216 120.0 . . ? N211 C216 H216 120.0 . . ? C226 N221 N222 121.8(7) . . ? C226 N221 C225 130.2(7) . . ? N222 N221 C225 108.0 . . ? N221 N222 C223 108.0 . . ? N221 N222 Zn2 140.0(4) . . ? C223 N222 Zn2 111.9(4) . . ? C212 C223 C224 133.6(7) . . ? C212 C223 N222 118.4(7) . . ? C224 C223 N222 108.0 . . ? C223 C224 C225 108.0 . . ? C223 C224 H224 126.0 . . ? C225 C224 H224 126.0 . . ? C224 C225 N221 108.0 . . ? C224 C225 H225 126.0 . . ? N221 C225 H225 126.0 . . ? N221 C226 C252 112.9(8) . . ? N221 C226 H22A 109.0 . . ? C252 C226 H22A 109.0 . . ? N221 C226 H22B 109.0 . . ? C252 C226 H22B 109.0 . . ? H22A C226 H22B 107.8 . . ? C232 N231 C236 120.0 . . ? C232 N231 Zn1 115.2(5) . . ? C236 N231 Zn1 124.8(5) . . ? C243 C232 N231 116.7(7) . . ? C243 C232 C233 123.1(7) . . ? N231 C232 C233 120.0 . . ? C232 C233 C234 120.0 . . ? C232 C233 H233 120.0 . . ? C234 C233 H233 120.0 . . ? C235 C234 C233 120.0 . . ? C235 C234 H234 120.0 . . ? C233 C234 H234 120.0 . . ? C234 C235 C236 120.0 . . ? C234 C235 H235 120.0 . . ? C236 C235 H235 120.0 . . ? C235 C236 N231 120.0 . . ? C235 C236 H236 120.0 . . ? N231 C236 H236 120.0 . . ? C246 N241 N242 124.5(7) . . ? C246 N241 C245 127.5(7) . . ? N242 N241 C245 108.0 . . ? N241 N242 C243 108.0 . . ? N241 N242 Zn1 138.8(4) . . ? C243 N242 Zn1 113.2(4) . . ? C232 C243 C244 133.9(7) . . ? C232 C243 N242 118.0(7) . . ? C244 C243 N242 108.0 . . ? C243 C244 C245 108.0 . . ? C243 C244 H244 126.0 . . ? C245 C244 H244 126.0 . . ? N241 C245 C244 108.0 . . ? N241 C245 H245 126.0 . . ? C244 C245 H245 126.0 . . ? N241 C246 C253 114.3(9) . . ? N241 C246 H24A 108.7 . . ? C253 C246 H24A 108.7 . . ? N241 C246 H24B 108.7 . . ? C253 C246 H24B 108.7 . . ? H24A C246 H24B 107.6 . . ? C252 C251 C256 120.0 . . ? C252 C251 H251 120.0 . . ? C256 C251 H251 120.0 . . ? C251 C252 C253 120.0 . . ? C251 C252 C226 123.3(6) . . ? C253 C252 C226 116.6(6) . . ? C254 C253 C252 120.0 . . ? C254 C253 C246 123.2(7) . . ? C252 C253 C246 116.8(7) . . ? C253 C254 C255 120.0 . . ? C253 C254 H254 120.0 . . ? C255 C254 H254 120.0 . . ? C254 C255 C256 120.0 . . ? C254 C255 C261 121.4(5) . . ? C256 C255 C261 118.6(5) . . ? C255 C256 C251 120.0 . . ? C255 C256 C264 121.3(5) . . ? C251 C256 C264 118.7(5) . . ? C262 C261 C255 119.8(2) . . ? C262 C261 H261 120.1 . . ? C255 C261 H261 120.1 . . ? C263 C262 C261 121.6(5) . . ? C263 C262 H262 119.2 . . ? C261 C262 H262 119.2 . . ? C262 C263 C264 118.4(5) . . ? C262 C263 H263 120.8 . . ? C264 C263 H263 120.8 . . ? C263 C264 C256 120.0(2) . . ? C263 C264 H264 120.0 . . ? C256 C264 H264 120.0 . . ? F12Y Si11 F12Y 43.6(12) 11_556 8_645 ? F12Y Si11 F12Y 43.6(12) 11_556 . ? F12Y Si11 F12Y 43.6(12) 8_645 . ? F12Y Si11 F13Y 93.5(5) 11_556 11_556 ? F12Y Si11 F13Y 134.1(10) 8_645 11_556 ? F12Y Si11 F13Y 96.7(10) . 11_556 ? F12Y Si11 F13Y 134.1(10) 11_556 . ? F12Y Si11 F13Y 96.7(10) 8_645 . ? F12Y Si11 F13Y 93.5(5) . . ? F13Y Si11 F13Y 110.1(5) 11_556 . ? F12Y Si11 F13Y 96.7(10) 11_556 8_645 ? F12Y Si11 F13Y 93.5(5) 8_645 8_645 ? F12Y Si11 F13Y 134.1(10) . 8_645 ? F13Y Si11 F13Y 110.1(5) 11_556 8_645 ? F13Y Si11 F13Y 110.1(5) . 8_645 ? F12Y Si11 F13X 126.8(9) 11_556 11_556 ? F12Y Si11 F13X 169.4(14) 8_645 11_556 ? F12Y Si11 F13X 127.8(13) . 11_556 ? F13Y Si11 F13X 35.3(9) 11_556 11_556 ? F13Y Si11 F13X 89.6(10) . 11_556 ? F13Y Si11 F13X 92.3(13) 8_645 11_556 ? F12Y Si11 F13X 169.4(14) 11_556 . ? F12Y Si11 F13X 127.8(13) 8_645 . ? F12Y Si11 F13X 126.8(9) . . ? F13Y Si11 F13X 92.3(13) 11_556 . ? F13Y Si11 F13X 35.3(9) . . ? F13Y Si11 F13X 89.6(10) 8_645 . ? F13X Si11 F13X 61.1(16) 11_556 . ? F12Y Si11 F13X 127.8(13) 11_556 8_645 ? F12Y Si11 F13X 126.8(9) 8_645 8_645 ? F12Y Si11 F13X 169.4(14) . 8_645 ? F13Y Si11 F13X 89.6(10) 11_556 8_645 ? F13Y Si11 F13X 92.3(13) . 8_645 ? F13Y Si11 F13X 35.3(9) 8_645 8_645 ? F13X Si11 F13X 61.1(16) 11_556 8_645 ? F13X Si11 F13X 61.1(16) . 8_645 ? F12Y Si11 F12X 83.2(9) 11_556 8_645 ? F12Y Si11 F12X 42.4(6) 8_645 8_645 ? F12Y Si11 F12X 80.0(11) . 8_645 ? F13Y Si11 F12X 176.5(8) 11_556 8_645 ? F13Y Si11 F12X 71.5(6) . 8_645 ? F13Y Si11 F12X 71.7(7) 8_645 8_645 ? F13X Si11 F12X 148.2(12) 11_556 8_645 ? F13X Si11 F12X 90.7(12) . 8_645 ? F13X Si11 F12X 93.5(5) 8_645 8_645 ? F12Y Si11 F12X 42.4(6) 11_556 11_556 ? F12Y Si11 F12X 80.0(11) 8_645 11_556 ? F12Y Si11 F12X 83.2(9) . 11_556 ? F13Y Si11 F12X 71.7(7) 11_556 11_556 ? F13Y Si11 F12X 176.5(8) . 11_556 ? F13Y Si11 F12X 71.5(6) 8_645 11_556 ? F13X Si11 F12X 93.5(5) 11_556 11_556 ? F13X Si11 F12X 148.2(12) . 11_556 ? F13X Si11 F12X 90.7(12) 8_645 11_556 ? F12X Si11 F12X 106.5(5) 8_645 11_556 ? F12Y Si11 F12X 80.0(11) 11_556 . ? F12Y Si11 F12X 83.2(9) 8_645 . ? F12Y Si11 F12X 42.4(6) . . ? F13Y Si11 F12X 71.5(6) 11_556 . ? F13Y Si11 F12X 71.7(7) . . ? F13Y Si11 F12X 176.5(8) 8_645 . ? F13X Si11 F12X 90.7(12) 11_556 . ? F13X Si11 F12X 93.5(5) . . ? F13X Si11 F12X 148.2(12) 8_645 . ? F12X Si11 F12X 106.5(5) 8_645 . ? F12X Si11 F12X 106.5(5) 11_556 . ? Si11 F13X F13X 59.4(8) . 11_556 ? Si11 F13X F13X 59.4(8) . 8_645 ? F13X F13X F13X 60.000(3) 11_556 8_645 ? F12Y F12Y F12Y 60.000(3) 8_645 11_556 ? F12Y F12Y Si11 68.2(6) 8_645 . ? F12Y F12Y Si11 68.2(6) 11_556 . ? F25X Si21 F24Y 44.9(3) . . ? F25X Si21 F24X 89.98(8) . . ? F24Y Si21 F24X 45.1(3) . . ? F25X Si21 F27Y 134.9(3) . . ? F24Y Si21 F27Y 90.02(8) . . ? F24X Si21 F27Y 44.9(3) . . ? F25X Si21 F26X 90.00(8) . . ? F24Y Si21 F26X 134.9(3) . . ? F24X Si21 F26X 177.8(4) . . ? F27Y Si21 F26X 135.0(3) . . ? F25X Si21 F27X 177.7(4) . . ? F24Y Si21 F27X 135.0(3) . . ? F24X Si21 F27X 89.96(8) . . ? F27Y Si21 F27X 45.0(3) . . ? F26X Si21 F27X 89.97(8) . . ? F25X Si21 F26Y 135.0(3) . . ? F24Y Si21 F26Y 177.7(4) . . ? F24X Si21 F26Y 134.9(3) . . ? F27Y Si21 F26Y 89.97(8) . . ? F26X Si21 F26Y 45.0(3) . . ? F27X Si21 F26Y 45.0(3) . . ? F25X Si21 F25Y 45.0(3) . . ? F24Y Si21 F25Y 89.95(8) . . ? F24X Si21 F25Y 135.0(3) . . ? F27Y Si21 F25Y 177.7(4) . . ? F26X Si21 F25Y 45.0(3) . . ? F27X Si21 F25Y 134.9(3) . . ? F26Y Si21 F25Y 89.97(8) . . ? F25X Si21 F23 91.2(2) . . ? F24Y Si21 F23 91.1(2) . . ? F24X Si21 F23 91.1(2) . . ? F27Y Si21 F23 91.2(2) . . ? F26X Si21 F23 91.1(2) . . ? F27X Si21 F23 91.1(2) . . ? F26Y Si21 F23 91.1(2) . . ? F25Y Si21 F23 91.1(2) . . ? F25X Si21 F22 88.9(2) . . ? F24Y Si21 F22 88.9(2) . . ? F24X Si21 F22 88.9(2) . . ? F27Y Si21 F22 88.9(2) . . ? F26X Si21 F22 88.9(2) . . ? F27X Si21 F22 88.9(2) . . ? F26Y Si21 F22 88.8(2) . . ? F25Y Si21 F22 88.9(2) . . ? F23 Si21 F22 179.96(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C116 N111 C112 C123 -178.4(9) . . . . ? Zn1 N111 C112 C123 11.8(8) 11_556 . . . ? C116 N111 C112 C113 0.0 . . . . ? Zn1 N111 C112 C113 -169.8(6) 11_556 . . . ? C123 C112 C113 C114 178.4(9) . . . . ? N111 C112 C113 C114 0.0 . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C116 0.0 . . . . ? C114 C115 C116 N111 0.0 . . . . ? C112 N111 C116 C115 0.0 . . . . ? Zn1 N111 C116 C115 168.5(6) 11_556 . . . ? C126 N121 N122 C123 178.6(9) . . . . ? C125 N121 N122 C123 0.0 . . . . ? C126 N121 N122 Zn1 -6.4(11) . . . 11_556 ? C125 N121 N122 Zn1 175.0(8) . . . 11_556 ? N111 C112 C123 N122 -7.7(10) . . . . ? C113 C112 C123 N122 173.9(5) . . . . ? N111 C112 C123 C124 167.2(7) . . . . ? C113 C112 C123 C124 -11.2(12) . . . . ? N121 N122 C123 C112 176.1(9) . . . . ? Zn1 N122 C123 C112 -0.3(8) 11_556 . . . ? N121 N122 C123 C124 0.0 . . . . ? Zn1 N122 C123 C124 -176.5(6) 11_556 . . . ? C112 C123 C124 C125 -175.3(11) . . . . ? N122 C123 C124 C125 0.0 . . . . ? C123 C124 C125 N121 0.0 . . . . ? C126 N121 C125 C124 -178.5(9) . . . . ? N122 N121 C125 C124 0.0 . . . . ? N122 N121 C126 C152 102.7(9) . . . . ? C125 N121 C126 C152 -79.0(11) . . . . ? N231 Zn1 N131 C132 -86.5(5) . . . . ? N242 Zn1 N131 C132 -46(2) . . . . ? N142 Zn1 N131 C132 1.2(4) . . . . ? N111 Zn1 N131 C132 -180.0(5) 8_645 . . . ? N122 Zn1 N131 C132 104.2(6) 8_645 . . . ? N231 Zn1 N131 C136 92.7(5) . . . . ? N242 Zn1 N131 C136 133(2) . . . . ? N142 Zn1 N131 C136 -179.5(5) . . . . ? N111 Zn1 N131 C136 -0.7(5) 8_645 . . . ? N122 Zn1 N131 C136 -76.6(6) 8_645 . . . ? C136 N131 C132 C143 -176.7(8) . . . . ? Zn1 N131 C132 C143 2.6(8) . . . . ? C136 N131 C132 C133 0.0 . . . . ? Zn1 N131 C132 C133 179.3(6) . . . . ? C143 C132 C133 C134 176.4(9) . . . . ? N131 C132 C133 C134 0.0 . . . . ? C132 C133 C134 C135 0.0 . . . . ? C133 C134 C135 C136 0.0 . . . . ? C134 C135 C136 N131 0.0 . . . . ? C132 N131 C136 C135 0.0 . . . . ? Zn1 N131 C136 C135 -179.2(6) . . . . ? C145 N141 N142 C143 0.0 . . . . ? C146 N141 N142 C143 -175.7(9) . . . . ? C145 N141 N142 Zn1 173.6(8) . . . . ? C146 N141 N142 Zn1 -2.1(12) . . . . ? N131 Zn1 N142 C143 -4.5(5) . . . . ? N231 Zn1 N142 C143 93.2(5) . . . . ? N242 Zn1 N142 C143 169.4(4) . . . . ? N111 Zn1 N142 C143 -13(3) 8_645 . . . ? N122 Zn1 N142 C143 -88.0(14) 8_645 . . . ? N131 Zn1 N142 N141 -177.9(8) . . . . ? N231 Zn1 N142 N141 -80.2(7) . . . . ? N242 Zn1 N142 N141 -4.0(7) . . . . ? N111 Zn1 N142 N141 174(2) 8_645 . . . ? N122 Zn1 N142 N141 98.6(15) 8_645 . . . ? N131 C132 C143 N142 -6.9(10) . . . . ? C133 C132 C143 N142 176.5(5) . . . . ? N131 C132 C143 C144 177.3(7) . . . . ? C133 C132 C143 C144 0.7(12) . . . . ? N141 N142 C143 C132 -176.7(9) . . . . ? Zn1 N142 C143 C132 7.8(8) . . . . ? N141 N142 C143 C144 0.0 . . . . ? Zn1 N142 C143 C144 -175.5(6) . . . . ? C132 C143 C144 C145 176.1(11) . . . . ? N142 C143 C144 C145 0.0 . . . . ? C143 C144 C145 N141 0.0 . . . . ? N142 N141 C145 C144 0.0 . . . . ? C146 N141 C145 C144 175.4(10) . . . . ? C145 N141 C146 C153 -69.3(11) . . . . ? N142 N141 C146 C153 105.5(9) . . . . ? C156 C151 C152 C153 0.0 . . . . ? C156 C151 C152 C126 179.7(8) . . . . ? N121 C126 C152 C151 -10.4(12) . . . . ? N121 C126 C152 C153 169.3(7) . . . . ? C151 C152 C153 C154 0.0 . . . . ? C126 C152 C153 C154 -179.7(7) . . . . ? C151 C152 C153 C146 -179.6(7) . . . . ? C126 C152 C153 C146 0.6(9) . . . . ? N141 C146 C153 C152 160.3(7) . . . . ? N141 C146 C153 C154 -19.4(11) . . . . ? C152 C153 C154 C155 0.0 . . . . ? C146 C153 C154 C155 179.6(8) . . . . ? C153 C154 C155 C156 0.0 . . . . ? C153 C154 C155 C161 176.7(9) . . . . ? C154 C155 C156 C151 0.0 . . . . ? C161 C155 C156 C151 -176.7(9) . . . . ? C154 C155 C156 C164 -173.5(10) . . . . ? C161 C155 C156 C164 9.7(11) . . . . ? C152 C151 C156 C155 0.0 . . . . ? C152 C151 C156 C164 173.5(10) . . . . ? C154 C155 C161 C162 174.7(10) . . . . ? C156 C155 C161 C162 -8.6(16) . . . . ? C155 C161 C162 C163 5(2) . . . . ? C161 C162 C163 C164 -3(2) . . . . ? C162 C163 C164 C156 4(2) . . . . ? C155 C156 C164 C163 -7.4(17) . . . . ? C151 C156 C164 C163 179.0(10) . . . . ? N211 Zn2 N211 C212 179.4(4) 8_645 . . . ? N211 Zn2 N211 C212 -82.4(5) 11_556 . . . ? N222 Zn2 N211 C212 -59(6) 11_556 . . . ? N222 Zn2 N211 C212 103.1(7) 8_645 . . . ? N222 Zn2 N211 C212 2.0(4) . . . . ? N211 Zn2 N211 C216 2.4(5) 8_645 . . . ? N211 Zn2 N211 C216 100.5(3) 11_556 . . . ? N222 Zn2 N211 C216 123(6) 11_556 . . . ? N222 Zn2 N211 C216 -74.0(7) 8_645 . . . ? N222 Zn2 N211 C216 -175.0(5) . . . . ? C216 N211 C212 C223 174.7(8) . . . . ? Zn2 N211 C212 C223 -2.5(7) . . . . ? C216 N211 C212 C213 0.0 . . . . ? Zn2 N211 C212 C213 -177.2(4) . . . . ? C223 C212 C213 C214 -174.5(8) . . . . ? N211 C212 C213 C214 0.0 . . . . ? C212 C213 C214 C215 0.0 . . . . ? C213 C214 C215 C216 0.0 . . . . ? C214 C215 C216 N211 0.0 . . . . ? C212 N211 C216 C215 0.0 . . . . ? Zn2 N211 C216 C215 176.9(5) . . . . ? C226 N221 N222 C223 -178.5(9) . . . . ? C225 N221 N222 C223 0.0 . . . . ? C226 N221 N222 Zn2 -2.1(11) . . . . ? C225 N221 N222 Zn2 176.4(8) . . . . ? N211 Zn2 N222 N221 159(2) 8_645 . . . ? N211 Zn2 N222 N221 -177.6(7) . . . . ? N211 Zn2 N222 N221 -79.4(7) 11_556 . . . ? N222 Zn2 N222 N221 -3.3(9) 11_556 . . . ? N222 Zn2 N222 N221 98.6(3) 8_645 . . . ? N211 Zn2 N222 C223 -25(3) 8_645 . . . ? N211 Zn2 N222 C223 -1.3(4) . . . . ? N211 Zn2 N222 C223 96.9(4) 11_556 . . . ? N222 Zn2 N222 C223 173.0(5) 11_556 . . . ? N222 Zn2 N222 C223 -85.1(8) 8_645 . . . ? N211 C212 C223 C224 178.7(6) . . . . ? C213 C212 C223 C224 -6.8(11) . . . . ? N211 C212 C223 N222 1.3(9) . . . . ? C213 C212 C223 N222 175.9(5) . . . . ? N221 N222 C223 C212 178.0(8) . . . . ? Zn2 N222 C223 C212 0.4(7) . . . . ? N221 N222 C223 C224 0.0 . . . . ? Zn2 N222 C223 C224 -177.5(5) . . . . ? C212 C223 C224 C225 -177.5(10) . . . . ? N222 C223 C224 C225 0.0 . . . . ? C223 C224 C225 N221 0.0 . . . . ? C226 N221 C225 C224 178.3(10) . . . . ? N222 N221 C225 C224 0.0 . . . . ? N222 N221 C226 C252 107.0(9) . . . . ? C225 N221 C226 C252 -71.1(11) . . . . ? N131 Zn1 N231 C232 178.8(5) . . . . ? N242 Zn1 N231 C232 4.3(4) . . . . ? N142 Zn1 N231 C232 103.2(4) . . . . ? N111 Zn1 N231 C232 -84.8(5) 8_645 . . . ? N122 Zn1 N231 C232 -71(7) 8_645 . . . ? N131 Zn1 N231 C236 -3.5(5) . . . . ? N242 Zn1 N231 C236 -178.0(5) . . . . ? N142 Zn1 N231 C236 -79.1(5) . . . . ? N111 Zn1 N231 C236 92.9(5) 8_645 . . . ? N122 Zn1 N231 C236 107(7) 8_645 . . . ? C236 N231 C232 C243 174.9(8) . . . . ? Zn1 N231 C232 C243 -7.3(7) . . . . ? C236 N231 C232 C233 0.0 . . . . ? Zn1 N231 C232 C233 177.8(5) . . . . ? C243 C232 C233 C234 -174.5(8) . . . . ? N231 C232 C233 C234 0.0 . . . . ? C232 C233 C234 C235 0.0 . . . . ? C233 C234 C235 C236 0.0 . . . . ? C234 C235 C236 N231 0.0 . . . . ? C232 N231 C236 C235 0.0 . . . . ? Zn1 N231 C236 C235 -177.6(6) . . . . ? C246 N241 N242 C243 -179.7(9) . . . . ? C245 N241 N242 C243 0.0 . . . . ? C246 N241 N242 Zn1 -0.5(11) . . . . ? C245 N241 N242 Zn1 179.3(7) . . . . ? N131 Zn1 N242 N241 138(2) . . . . ? N231 Zn1 N242 N241 179.8(7) . . . . ? N142 Zn1 N242 N241 92.3(7) . . . . ? N111 Zn1 N242 N241 -87.4(7) 8_645 . . . ? N122 Zn1 N242 N241 -11.4(8) 8_645 . . . ? N131 Zn1 N242 C243 -43(2) . . . . ? N231 Zn1 N242 C243 -0.9(4) . . . . ? N142 Zn1 N242 C243 -88.5(4) . . . . ? N111 Zn1 N242 C243 91.8(5) 8_645 . . . ? N122 Zn1 N242 C243 167.8(6) 8_645 . . . ? N231 C232 C243 C244 -177.6(6) . . . . ? C233 C232 C243 C244 -2.9(11) . . . . ? N231 C232 C243 N242 6.6(9) . . . . ? C233 C232 C243 N242 -178.7(5) . . . . ? N241 N242 C243 C232 176.8(8) . . . . ? Zn1 N242 C243 C232 -2.7(7) . . . . ? N241 N242 C243 C244 0.0 . . . . ? Zn1 N242 C243 C244 -179.5(5) . . . . ? C232 C243 C244 C245 -176.0(10) . . . . ? N242 C243 C244 C245 0.0 . . . . ? C246 N241 C245 C244 179.7(10) . . . . ? N242 N241 C245 C244 0.0 . . . . ? C243 C244 C245 N241 0.0 . . . . ? N242 N241 C246 C253 102.5(9) . . . . ? C245 N241 C246 C253 -77.2(11) . . . . ? C256 C251 C252 C253 0.0 . . . . ? C256 C251 C252 C226 177.5(8) . . . . ? N221 C226 C252 C251 -16.3(11) . . . . ? N221 C226 C252 C253 161.3(7) . . . . ? C251 C252 C253 C254 0.0 . . . . ? C226 C252 C253 C254 -177.7(7) . . . . ? C251 C252 C253 C246 -179.3(8) . . . . ? C226 C252 C253 C246 3.0(9) . . . . ? N241 C246 C253 C254 -13.8(12) . . . . ? N241 C246 C253 C252 165.5(7) . . . . ? C252 C253 C254 C255 0.0 . . . . ? C246 C253 C254 C255 179.2(8) . . . . ? C253 C254 C255 C256 0.0 . . . . ? C253 C254 C255 C261 178.1(10) . . . . ? C254 C255 C256 C251 0.0 . . . . ? C261 C255 C256 C251 -178.2(9) . . . . ? C254 C255 C256 C264 -178.9(9) . . . . ? C261 C255 C256 C264 2.9(11) . . . . ? C252 C251 C256 C255 0.0 . . . . ? C252 C251 C256 C264 178.9(9) . . . . ? C254 C255 C261 C262 -176.8(10) . . . . ? C256 C255 C261 C262 1.3(16) . . . . ? C255 C261 C262 C263 -2(2) . . . . ? C261 C262 C263 C264 -1(2) . . . . ? C262 C263 C264 C256 6(2) . . . . ? C255 C256 C264 C263 -6.5(16) . . . . ? C251 C256 C264 C263 174.6(10) . . . . ? F12Y Si11 F13X F13X 140(6) 11_556 . . 11_556 ? F12Y Si11 F13X F13X 173.0(16) 8_645 . . 11_556 ? F12Y Si11 F13X F13X 117.4(13) . . . 11_556 ? F13Y Si11 F13X F13X 17.3(15) 11_556 . . 11_556 ? F13Y Si11 F13X F13X 140(3) . . . 11_556 ? F13Y Si11 F13X F13X -92.8(15) 8_645 . . 11_556 ? F13X Si11 F13X F13X -71.0(7) 8_645 . . 11_556 ? F12X Si11 F13X F13X -164.5(13) 8_645 . . 11_556 ? F12X Si11 F13X F13X -41(3) 11_556 . . 11_556 ? F12X Si11 F13X F13X 88.9(13) . . . 11_556 ? F12Y Si11 F13X F13X -149(6) 11_556 . . 8_645 ? F12Y Si11 F13X F13X -116.0(11) 8_645 . . 8_645 ? F12Y Si11 F13X F13X -171.6(15) . . . 8_645 ? F13Y Si11 F13X F13X 88.3(13) 11_556 . . 8_645 ? F13Y Si11 F13X F13X -149(3) . . . 8_645 ? F13Y Si11 F13X F13X -21.8(12) 8_645 . . 8_645 ? F13X Si11 F13X F13X 71.0(7) 11_556 . . 8_645 ? F12X Si11 F13X F13X -93.5(9) 8_645 . . 8_645 ? F12X Si11 F13X F13X 30(2) 11_556 . . 8_645 ? F12X Si11 F13X F13X 159.9(11) . . . 8_645 ? F12Y Si11 F12Y F12Y -65.2(3) 11_556 . . 8_645 ? F13Y Si11 F12Y F12Y -153.2(16) 11_556 . . 8_645 ? F13Y Si11 F12Y F12Y 96.0(17) . . . 8_645 ? F13Y Si11 F12Y F12Y -27(2) 8_645 . . 8_645 ? F13X Si11 F12Y F12Y -171.7(19) 11_556 . . 8_645 ? F13X Si11 F12Y F12Y 109(2) . . . 8_645 ? F13X Si11 F12Y F12Y -27(9) 8_645 . . 8_645 ? F12X Si11 F12Y F12Y 25.5(17) 8_645 . . 8_645 ? F12X Si11 F12Y F12Y -82.6(17) 11_556 . . 8_645 ? F12X Si11 F12Y F12Y 154(3) . . . 8_645 ? F12Y Si11 F12Y F12Y 65.2(3) 8_645 . . 11_556 ? F13Y Si11 F12Y F12Y -88.1(14) 11_556 . . 11_556 ? F13Y Si11 F12Y F12Y 161.2(16) . . . 11_556 ? F13Y Si11 F12Y F12Y 39(2) 8_645 . . 11_556 ? F13X Si11 F12Y F12Y -106.6(18) 11_556 . . 11_556 ? F13X Si11 F12Y F12Y 174(2) . . . 11_556 ? F13X Si11 F12Y F12Y 38(9) 8_645 . . 11_556 ? F12X Si11 F12Y F12Y 90.6(16) 8_645 . . 11_556 ? F12X Si11 F12Y F12Y -17.5(16) 11_556 . . 11_556 ? F12X Si11 F12Y F12Y -141(3) . . . 11_556 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.243 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.102 #===END