# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/190 data_anka4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H48 Ho N13 O15' _chemical_formula_weight 887.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ho' 'Ho' -0.2175 4.6783 '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 9.535(2) _cell_length_b 12.520(3) _cell_length_c 17.012(3) _cell_angle_alpha 71.89(3) _cell_angle_beta 81.55(3) _cell_angle_gamma 68.90(3) _cell_volume 1799.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 13.5 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 1.65 _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'flotation in CH3Cl/CH3Br' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 2.280 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM4' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5333 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2. _diffrn_reflns_theta_max 23. _reflns_number_total 5332 _reflns_number_gt 4960 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4 software (1996)' _computing_cell_refinement 'Kuma KM4 software (1996)' _computing_data_reduction 'Kuma KM4 software (1996)' _computing_structure_solution 'SHELXS (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4975 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 5.609 _refine_ls_restrained_S_all 5.609 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho Ho 0.21269(4) 0.30125(3) 0.25427(2) 0.02301(13) Uani 1 d . . . O1 O 0.1433(6) 0.5079(4) 0.2284(3) 0.0322(13) Uani 1 d . . . O2 O 0.1042(9) 0.6918(5) 0.1470(4) 0.074(3) Uani 1 d . . . O3 O 0.0743(6) 0.3485(5) 0.1330(3) 0.0338(13) Uani 1 d . . . O4 O 0.1010(7) 0.3113(5) 0.0109(3) 0.0468(16) Uani 1 d . . . O5 O 0.2134(6) 0.3266(5) 0.3839(3) 0.0330(13) Uani 1 d . . . O6 O 0.2760(8) 0.4110(6) 0.4638(4) 0.064(2) Uani 1 d . . . O7 O 0.3308(7) 0.1549(5) 0.1880(3) 0.0393(15) Uani 1 d . . . O8 O 0.4668(8) -0.0208(6) 0.1713(4) 0.064(2) Uani 1 d . . . O9 O -0.0411(6) 0.3731(4) 0.2911(3) 0.0316(13) Uani 1 d . . . O10 O -0.2240(7) 0.3749(5) 0.3868(4) 0.0489(17) Uani 1 d . . . O11 O -0.0854(7) -0.0196(5) 0.3822(4) 0.0468(16) Uani 1 d . . . O12 O -0.1198(8) 0.0176(6) 0.2482(4) 0.0568(19) Uani 1 d . . . OW1 O 0.3088(9) 0.0661(7) 0.0289(5) 0.079(2) Uani 1 d . . . OW2 O 0.5039(16) 0.2717(9) 0.5887(9) 0.205(7) Uani 1 d . . . OW3 O -0.2806(14) 0.3507(10) 0.5521(8) 0.159(5) Uani 1 d . . . N1 N 0.3215(7) 0.4052(6) 0.1121(4) 0.0305(16) Uani 1 d . . . N2 N 0.4527(7) 0.3435(6) 0.2741(4) 0.0323(16) Uani 1 d . . . N3 N 0.4164(7) 0.1039(6) 0.3435(4) 0.0304(16) Uani 1 d . . . N4 N 0.0947(7) 0.1386(5) 0.3415(4) 0.0256(15) Uani 1 d . . . N21 N -0.2255(10) 0.0258(8) 0.0986(5) 0.072(3) Uani 1 d . . . H21A H -0.2716 -0.0096 0.0810 0.086 Uiso 1 calc R . . H21B H -0.2134 0.0087 0.1507 0.086 Uiso 1 calc R . . N22 N -0.1041(10) 0.1615(7) 0.0741(5) 0.065(3) Uani 1 d . . . H22A H -0.0710 0.2149 0.0401 0.078 Uiso 1 calc R . . H22B H -0.0925 0.1438 0.1264 0.078 Uiso 1 calc R . . N23 N -0.1929(12) 0.1307(7) -0.0332(5) 0.081(3) Uani 1 d . . . H23A H -0.2392 0.0947 -0.0499 0.097 Uiso 1 calc R . . H23B H -0.1594 0.1830 -0.0684 0.097 Uiso 1 calc R . . N31 N 0.6500(10) 0.6167(7) 0.2663(5) 0.062(2) Uani 1 d . . . H31A H 0.6899 0.5450 0.2966 0.074 Uiso 1 calc R . . H31B H 0.5781 0.6671 0.2864 0.074 Uiso 1 calc R . . N32 N 0.8068(8) 0.5749(6) 0.1578(4) 0.048(2) Uani 1 d . . . H32A H 0.8481 0.5029 0.1871 0.058 Uiso 1 calc R . . H32B H 0.8373 0.5979 0.1073 0.058 Uiso 1 calc R . . N33 N 0.6309(11) 0.7605(7) 0.1437(5) 0.084(3) Uani 1 d . . . H33A H 0.6592 0.7831 0.0927 0.101 Uiso 1 calc R . . H33B H 0.5591 0.8094 0.1651 0.101 Uiso 1 calc R . . N41 N -0.1417(9) 0.7598(7) 0.4190(5) 0.057(2) Uani 1 d . . . H41A H -0.1531 0.8342 0.4083 0.069 Uiso 1 calc R . . H41B H -0.1697 0.7225 0.4668 0.069 Uiso 1 calc R . . N42 N -0.0685(10) 0.5883(7) 0.3796(6) 0.067(3) Uani 1 d . . . H42A H -0.0996 0.5526 0.4271 0.080 Uiso 1 calc R . . H42B H -0.0292 0.5501 0.3432 0.080 Uiso 1 calc R . . N43 N -0.0387(11) 0.7607(7) 0.2897(5) 0.072(3) Uani 1 d . . . H43A H -0.0505 0.8351 0.2792 0.086 Uiso 1 calc R . . H43B H 0.0009 0.7240 0.2524 0.086 Uiso 1 calc R . . C1 C 0.1572(10) 0.5816(8) 0.1605(5) 0.040(2) Uani 1 d . . . C2 C 0.2407(10) 0.5347(7) 0.0894(5) 0.037(2) Uani 1 d . . . H2A H 0.1695 0.5539 0.0477 0.044 Uiso 1 calc R . . H2B H 0.3125 0.5755 0.0648 0.044 Uiso 1 calc R . . C3 C 0.1445(10) 0.3380(7) 0.0658(5) 0.033(2) Uani 1 d . . . C4 C 0.2942(9) 0.3548(7) 0.0498(5) 0.036(2) Uani 1 d . . . H4A H 0.3724 0.2787 0.0518 0.043 Uiso 1 calc R . . H4B H 0.2983 0.4082 -0.0051 0.043 Uiso 1 calc R . . C5 C 0.4831(9) 0.3788(8) 0.1215(5) 0.038(2) Uani 1 d . . . H5A H 0.5243 0.4219 0.0714 0.046 Uiso 1 calc R . . H5B H 0.5359 0.2942 0.1292 0.046 Uiso 1 calc R . . C6 C 0.5086(10) 0.4136(8) 0.1946(5) 0.041(2) Uani 1 d . . . H6A H 0.6151 0.3986 0.1975 0.049 Uiso 1 calc R . . H6B H 0.4560 0.4981 0.1871 0.049 Uiso 1 calc R . . C7 C 0.2912(10) 0.3813(7) 0.3996(5) 0.038(2) Uani 1 d . . . C8 C 0.4098(10) 0.4117(7) 0.3370(5) 0.038(2) Uani 1 d . . . H8A H 0.3733 0.4963 0.3088 0.046 Uiso 1 calc R . . H8B H 0.4989 0.3960 0.3658 0.046 Uiso 1 calc R . . C9 C 0.5765(9) 0.2301(7) 0.3043(5) 0.041(2) Uani 1 d . . . H9A H 0.6553 0.2467 0.3234 0.050 Uiso 1 calc R . . H9B H 0.6186 0.1958 0.2586 0.050 Uiso 1 calc R . . C10 C 0.5274(9) 0.1414(7) 0.3727(5) 0.039(2) Uani 1 d . . . H10A H 0.4818 0.1761 0.4178 0.046 Uiso 1 calc R . . H10B H 0.6143 0.0721 0.3933 0.046 Uiso 1 calc R . . C11 C 0.4268(10) 0.0509(7) 0.2124(5) 0.037(2) Uani 1 d . . . C12 C 0.4981(10) 0.0182(7) 0.2947(5) 0.039(2) Uani 1 d . . . H12A H 0.4989 -0.0611 0.3266 0.047 Uiso 1 calc R . . H12B H 0.6016 0.0164 0.2844 0.047 Uiso 1 calc R . . C13 C 0.3332(9) 0.0477(7) 0.4141(5) 0.035(2) Uani 1 d . . . H13A H 0.2933 0.0991 0.4504 0.042 Uiso 1 calc R . . H13B H 0.4016 -0.0273 0.4453 0.042 Uiso 1 calc R . . C14 C 0.2053(9) 0.0252(7) 0.3866(5) 0.037(2) Uani 1 d . . . H14A H 0.2448 -0.0270 0.3509 0.044 Uiso 1 calc R . . H14B H 0.1556 -0.0144 0.4347 0.044 Uiso 1 calc R . . C15 C -0.1004(9) 0.3242(7) 0.3556(5) 0.0281(18) Uani 1 d . . . C16 C -0.0199(9) 0.1971(7) 0.3975(5) 0.0306(19) Uani 1 d . . . H16A H 0.0286 0.1922 0.4454 0.037 Uiso 1 calc R . . H16B H -0.0919 0.1552 0.4167 0.037 Uiso 1 calc R . . C17 C -0.0680(10) 0.0298(7) 0.3095(6) 0.039(2) Uani 1 d . . . C18 C 0.0180(9) 0.1197(7) 0.2795(5) 0.033(2) Uani 1 d . . . H18A H 0.0934 0.0944 0.2380 0.040 Uiso 1 calc R . . H18B H -0.0526 0.1963 0.2519 0.040 Uiso 1 calc R . . C20 C -0.1734(12) 0.1059(8) 0.0458(6) 0.053(3) Uani 1 d . . . C30 C 0.6987(11) 0.6489(8) 0.1898(6) 0.046(2) Uani 1 d . . . C40 C -0.0812(11) 0.7030(8) 0.3625(6) 0.047(2) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho 0.0274(2) 0.0205(2) 0.0208(2) -0.00400(16) -0.00110(16) -0.00902(17) O1 0.048(4) 0.022(3) 0.027(3) -0.004(3) 0.006(3) -0.017(3) O2 0.132(7) 0.020(4) 0.048(4) -0.005(3) 0.025(4) -0.016(4) O3 0.037(3) 0.034(3) 0.026(3) -0.003(3) -0.006(3) -0.010(3) O4 0.064(4) 0.054(4) 0.033(4) -0.013(3) -0.007(3) -0.029(4) O5 0.044(4) 0.033(3) 0.024(3) -0.005(3) -0.001(3) -0.017(3) O6 0.100(6) 0.089(6) 0.036(4) -0.035(4) 0.013(4) -0.061(5) O7 0.050(4) 0.027(3) 0.030(3) -0.010(3) -0.010(3) 0.005(3) O8 0.082(5) 0.041(4) 0.067(5) -0.040(4) -0.017(4) 0.009(4) O9 0.033(3) 0.026(3) 0.030(3) -0.002(3) 0.003(3) -0.010(3) O10 0.043(4) 0.040(4) 0.053(4) -0.012(3) 0.012(3) -0.008(3) O11 0.066(5) 0.041(4) 0.042(4) -0.006(3) 0.000(3) -0.032(3) O12 0.073(5) 0.056(4) 0.061(5) -0.019(4) -0.016(4) -0.037(4) OW1 0.102(7) 0.074(5) 0.072(5) -0.034(4) -0.023(5) -0.025(5) OW2 0.228(16) 0.080(8) 0.300(18) -0.054(10) -0.133(14) 0.005(9) OW3 0.186(13) 0.153(11) 0.167(12) -0.075(9) 0.040(10) -0.084(10) N1 0.037(4) 0.030(4) 0.026(4) -0.011(3) 0.003(3) -0.012(3) N2 0.036(4) 0.033(4) 0.030(4) -0.006(3) -0.001(3) -0.017(3) N3 0.029(4) 0.031(4) 0.027(4) -0.007(3) -0.011(3) -0.002(3) N4 0.033(4) 0.024(4) 0.022(3) -0.004(3) -0.003(3) -0.014(3) N21 0.101(8) 0.090(7) 0.048(5) -0.003(5) -0.003(5) -0.074(7) N22 0.085(7) 0.055(6) 0.066(6) -0.009(5) -0.012(5) -0.040(5) N23 0.147(10) 0.063(6) 0.043(6) 0.003(5) -0.015(6) -0.058(7) N31 0.082(7) 0.042(5) 0.048(5) -0.013(4) 0.011(5) -0.010(5) N32 0.051(5) 0.039(5) 0.036(4) -0.005(4) -0.001(4) 0.002(4) N33 0.130(9) 0.031(5) 0.054(6) -0.007(4) 0.004(6) 0.008(5) N41 0.098(7) 0.039(5) 0.044(5) -0.017(4) 0.017(5) -0.036(5) N42 0.090(7) 0.036(5) 0.080(7) -0.023(5) 0.002(6) -0.024(5) N43 0.126(9) 0.046(5) 0.049(5) -0.029(4) 0.025(6) -0.033(6) C1 0.052(6) 0.034(5) 0.033(5) -0.010(4) 0.006(4) -0.016(5) C2 0.047(6) 0.032(5) 0.028(5) -0.003(4) 0.000(4) -0.016(4) C3 0.044(5) 0.026(5) 0.023(5) 0.002(4) -0.008(4) -0.008(4) C4 0.048(6) 0.039(5) 0.023(4) -0.010(4) 0.006(4) -0.018(4) C5 0.041(5) 0.045(5) 0.033(5) -0.013(4) 0.010(4) -0.021(4) C6 0.040(5) 0.051(6) 0.038(5) -0.009(4) 0.007(4) -0.030(5) C7 0.050(6) 0.034(5) 0.034(5) -0.005(4) -0.007(4) -0.020(5) C8 0.047(6) 0.041(5) 0.036(5) -0.013(4) -0.001(4) -0.024(5) C9 0.035(5) 0.042(5) 0.046(6) -0.010(4) -0.008(4) -0.012(4) C10 0.030(5) 0.039(5) 0.044(5) -0.008(4) -0.010(4) -0.008(4) C11 0.035(5) 0.033(5) 0.039(5) -0.010(4) 0.003(4) -0.007(4) C12 0.037(5) 0.032(5) 0.041(5) -0.008(4) -0.009(4) -0.003(4) C13 0.038(5) 0.032(5) 0.029(5) 0.003(4) -0.009(4) -0.012(4) C14 0.044(5) 0.028(5) 0.034(5) -0.003(4) -0.005(4) -0.011(4) C15 0.030(5) 0.029(5) 0.032(5) -0.013(4) -0.001(4) -0.014(4) C16 0.038(5) 0.034(5) 0.025(4) -0.008(4) -0.002(4) -0.019(4) C17 0.038(5) 0.031(5) 0.056(6) -0.018(5) -0.007(5) -0.013(4) C18 0.041(5) 0.036(5) 0.030(5) -0.013(4) -0.001(4) -0.019(4) C20 0.066(7) 0.041(6) 0.047(6) -0.004(5) 0.000(5) -0.022(5) C30 0.067(7) 0.037(6) 0.034(5) -0.006(4) -0.006(5) -0.018(5) C40 0.058(7) 0.034(6) 0.056(7) -0.019(5) -0.004(5) -0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho O7 2.307(5) . yes Ho O9 2.323(5) . yes Ho O5 2.326(5) . yes Ho O1 2.340(5) . yes Ho O3 2.415(5) . yes Ho N2 2.615(6) . yes Ho N1 2.626(6) . yes Ho N4 2.627(6) . yes Ho N3 2.695(6) . yes O1 C1 1.257(9) . no O2 C1 1.244(10) . no O3 C3 1.256(9) . no O4 C3 1.251(9) . no O5 C7 1.275(9) . no O6 C7 1.233(10) . no O7 C11 1.274(9) . no O8 C11 1.226(9) . no O9 C15 1.244(9) . no O10 C15 1.249(9) . no O11 C17 1.216(10) . no O12 C17 1.287(10) . no N1 C2 1.473(9) . no N1 C5 1.477(10) . no N1 C4 1.485(9) . no N2 C9 1.480(10) . no N2 C8 1.495(9) . no N2 C6 1.506(10) . no N3 C13 1.471(10) . no N3 C12 1.486(10) . no N3 C10 1.499(10) . no N4 C16 1.479(9) . no N4 C14 1.483(9) . no N4 C18 1.487(9) . no N21 C20 1.314(11) . no N22 C20 1.337(12) . no N23 C20 1.308(12) . no N31 C30 1.305(11) . no N32 C30 1.295(11) . no N33 C30 1.343(11) . no N41 C40 1.315(11) . no N42 C40 1.337(11) . no N43 C40 1.315(11) . no C1 C2 1.505(11) . no C3 C4 1.490(11) . no C5 C6 1.515(11) . no C7 C8 1.504(11) . no C9 C10 1.489(11) . no C11 C12 1.521(11) . no C13 C14 1.511(11) . no C15 C16 1.485(10) . no C17 C18 1.544(11) . no 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 O7 Ho O9 127.8(2) . . yes O7 Ho O5 137.28(19) . . yes O9 Ho O5 76.41(19) . . yes O7 Ho O1 139.81(18) . . yes O9 Ho O1 72.22(18) . . yes O5 Ho O1 76.25(18) . . yes O7 Ho O3 72.09(19) . . yes O9 Ho O3 72.97(19) . . yes O5 Ho O3 147.79(19) . . yes O1 Ho O3 85.07(19) . . yes O7 Ho N2 97.3(2) . . yes O9 Ho N2 134.9(2) . . yes O5 Ho N2 67.49(19) . . yes O1 Ho N2 73.6(2) . . yes O3 Ho N2 131.74(19) . . yes O7 Ho N1 73.6(2) . . yes O9 Ho N1 120.76(19) . . yes O5 Ho N1 128.53(19) . . yes O1 Ho N1 66.53(18) . . yes O3 Ho N1 63.11(19) . . yes N2 Ho N1 68.7(2) . . yes O7 Ho N4 80.4(2) . . yes O9 Ho N4 64.58(18) . . yes O5 Ho N4 81.79(18) . . yes O1 Ho N4 134.96(19) . . yes O3 Ho N4 93.81(18) . . yes N2 Ho N4 131.71(19) . . yes N1 Ho N4 149.42(19) . . yes O7 Ho N3 64.76(18) . . yes O9 Ho N3 125.21(19) . . yes O5 Ho N3 72.55(19) . . yes O1 Ho N3 137.71(19) . . yes O3 Ho N3 134.84(18) . . yes N2 Ho N3 68.5(2) . . yes N1 Ho N3 113.9(2) . . yes N4 Ho N3 67.2(2) . . yes C1 O1 Ho 126.7(5) . . no C3 O3 Ho 119.5(5) . . no C7 O5 Ho 123.4(5) . . no C11 O7 Ho 131.6(5) . . no C15 O9 Ho 123.7(5) . . no C2 N1 C5 111.0(6) . . no C2 N1 C4 109.0(6) . . no C5 N1 C4 112.8(6) . . no C2 N1 Ho 110.1(4) . . no C5 N1 Ho 107.5(5) . . no C4 N1 Ho 106.3(4) . . no C9 N2 C8 109.9(6) . . no C9 N2 C6 107.5(6) . . no C8 N2 C6 110.3(6) . . no C9 N2 Ho 110.3(5) . . no C8 N2 Ho 106.5(5) . . no C6 N2 Ho 112.3(5) . . no C13 N3 C12 109.7(6) . . no C13 N3 C10 110.7(6) . . no C12 N3 C10 109.1(6) . . no C13 N3 Ho 106.8(4) . . no C12 N3 Ho 112.4(4) . . no C10 N3 Ho 108.1(5) . . no C16 N4 C14 112.7(6) . . no C16 N4 C18 109.2(6) . . no C14 N4 C18 111.2(6) . . no C16 N4 Ho 104.8(4) . . no C14 N4 Ho 114.4(5) . . no C18 N4 Ho 104.0(4) . . no O2 C1 O1 124.7(8) . . no O2 C1 C2 116.8(7) . . no O1 C1 C2 118.5(7) . . no N1 C2 C1 114.5(7) . . no O4 C3 O3 125.2(8) . . no O4 C3 C4 116.2(7) . . no O3 C3 C4 118.5(7) . . no N1 C4 C3 110.8(7) . . no N1 C5 C6 111.6(7) . . no N2 C6 C5 110.6(7) . . no O6 C7 O5 124.0(8) . . no O6 C7 C8 117.0(8) . . no O5 C7 C8 119.0(7) . . no N2 C8 C7 113.6(7) . . no N2 C9 C10 113.1(7) . . no C9 C10 N3 110.9(7) . . no O8 C11 O7 122.9(8) . . no O8 C11 C12 119.5(8) . . no O7 C11 C12 117.5(7) . . no N3 C12 C11 112.2(6) . . no N3 C13 C14 111.9(6) . . no N4 C14 C13 110.9(6) . . no O9 C15 O10 124.2(8) . . no O9 C15 C16 117.8(7) . . no O10 C15 C16 118.0(7) . . no N4 C16 C15 111.8(6) . . no O11 C17 O12 125.9(8) . . no O11 C17 C18 122.9(8) . . no O12 C17 C18 111.2(8) . . no N4 C18 C17 118.5(7) . . no N23 C20 N21 119.1(10) . . no N23 C20 N22 121.6(9) . . no N21 C20 N22 119.3(9) . . no N32 C30 N31 121.4(9) . . no N32 C30 N33 120.3(9) . . no N31 C30 N33 118.3(9) . . no N41 C40 N43 119.6(8) . . no N41 C40 N42 119.1(9) . . no N43 C40 N42 121.3(9) . . no _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.05 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.289 _refine_diff_density_min -1.556 _refine_diff_density_rms 0.121