# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1849 data_compound_val(CodpkNCO) _publ_contact_author ; Prof. Roberto 'Cort\'es Dpto. Qu\'imica Inorg\'anica Universidad del Pa\'is Vasco Apartado 450 01080 Vitoria Spain ; _publ_contact_author_phone '34 45 013008' _publ_contact_author_fax '34 45 134762' _publ_contact_author_email qipcomor@lg.ehu.es data_val(CodpkNCO) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_sum 'C25 H20 Co2 N6 O6' _chemical_formula_weight 618.33 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 13.0395(13) _cell_length_b 12.3033(13) _cell_length_c 19.3648(15) _cell_angle_alpha 90.00 _cell_angle_beta 122.575(9) _cell_angle_gamma 90.00 _cell_volume 2618.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 1.319 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 14672 _diffrn_reflns_av_R_equivalents 0.1483 _diffrn_reflns_av_sigmaI/netI 0.2575 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 30.53 _reflns_number_total 6653 _reflns_number_gt 2375 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6653 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2125 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.799 _refine_ls_shift/su_max 0.728 _refine_ls_shift/su_mean 0.129 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.61625(7) 0.57434(5) 0.04604(4) 0.0278(2) Uani 1 1 d . . . Co2 Co 0.65502(7) 0.31378(6) 0.05153(5) 0.0344(2) Uani 1 1 d . . . O1 O 0.5495(3) 0.4414(3) 0.07052(19) 0.0264(8) Uani 1 1 d . . . O2 O 0.4779(3) 0.4894(3) 0.1513(2) 0.0369(10) Uani 1 1 d . . . H1O2 H 0.4896 0.4832 0.1972 0.080(5) Uiso 1 1 calc R . . O3 O 0.6873(3) 0.4475(3) 0.0032(2) 0.0306(9) Uani 1 1 d . . . O4 O 0.8519(3) 0.4090(3) -0.0109(3) 0.0481(11) Uani 1 1 d . . . O5 O 0.8435(5) 0.0932(4) -0.0107(3) 0.103(2) Uani 1 1 d . . . O6 O 0.4008(6) 0.1663(5) -0.1630(4) 0.141(3) Uani 1 1 d . . . N1 N 0.6143(4) 0.2462(4) 0.1356(3) 0.0394(12) Uani 1 1 d . . . N2 N 0.7318(4) 0.5599(3) 0.1779(3) 0.0324(11) Uani 1 1 d . . . N3 N 0.8421(4) 0.3655(4) 0.1469(3) 0.0399(12) Uani 1 1 d . . . N4 N 0.7374(4) 0.6559(4) 0.0243(3) 0.0348(12) Uani 1 1 d . . . N5 N 0.7270(5) 0.1813(4) 0.0309(3) 0.0619(16) Uani 1 1 d . . . N6 N 0.4747(4) 0.2912(3) -0.0540(3) 0.0393(13) Uani 1 1 d . . . C1 C 0.6118(6) 0.1380(5) 0.1475(4) 0.0584(19) Uani 1 1 d . . . H1 H 0.6472 0.0912 0.1284 0.080(5) Uiso 1 1 calc R . . C2 C 0.5596(7) 0.0949(6) 0.1861(5) 0.076(2) Uani 1 1 d . . . H2 H 0.5559 0.0200 0.1907 0.080(5) Uiso 1 1 calc R . . C3 C 0.5125(7) 0.1636(6) 0.2181(4) 0.072(2) Uani 1 1 d . . . H3 H 0.4786 0.1355 0.2460 0.080(5) Uiso 1 1 calc R . . C4 C 0.5158(6) 0.2749(5) 0.2086(4) 0.0487(17) Uani 1 1 d . . . H4 H 0.4838 0.3223 0.2297 0.080(5) Uiso 1 1 calc R . . C5 C 0.5677(5) 0.3143(5) 0.1671(3) 0.0355(14) Uani 1 1 d . . . C6 C 0.5705(5) 0.4337(4) 0.1483(3) 0.0325(13) Uani 1 1 d . . . C7 C 0.6906(5) 0.4889(4) 0.2104(3) 0.0295(13) Uani 1 1 d . . . C8 C 0.7512(5) 0.4719(5) 0.2945(3) 0.0411(16) Uani 1 1 d . . . H8 H 0.7207 0.4238 0.3162 0.080(5) Uiso 1 1 calc R . . C9 C 0.8583(6) 0.5283(5) 0.3452(4) 0.0501(18) Uani 1 1 d . . . H9 H 0.9021 0.5169 0.4015 0.080(5) Uiso 1 1 calc R . . C10 C 0.8995(6) 0.6016(5) 0.3114(4) 0.0559(19) Uani 1 1 d . . . H10 H 0.9706 0.6410 0.3444 0.080(5) Uiso 1 1 calc R . . C11 C 0.8334(6) 0.6149(5) 0.2282(4) 0.0446(16) Uani 1 1 d . . . H11 H 0.8609 0.6648 0.2056 0.080(5) Uiso 1 1 calc R . . C12 C 0.9108(7) 0.3294(5) 0.2235(4) 0.0562(19) Uani 1 1 d . . . H12 H 0.8773 0.2801 0.2425 0.080(5) Uiso 1 1 calc R . . C13 C 1.0290(8) 0.3619(6) 0.2758(5) 0.074(2) Uani 1 1 d . . . H13 H 1.0731 0.3375 0.3297 0.080(5) Uiso 1 1 calc R . . C14 C 1.0817(7) 0.4306(6) 0.2478(5) 0.081(3) Uani 1 1 d . . . H14 H 1.1626 0.4515 0.2818 0.080(5) Uiso 1 1 calc R . . C15 C 1.0117(6) 0.4683(5) 0.1675(4) 0.0591(19) Uani 1 1 d . . . H15 H 1.0449 0.5153 0.1470 0.080(5) Uiso 1 1 calc R . . C16 C 0.8929(5) 0.4352(5) 0.1191(4) 0.0402(15) Uani 1 1 d . . . C17 C 0.8061(5) 0.4710(4) 0.0297(3) 0.0352(14) Uani 1 1 d . . . C18 C 0.8161(5) 0.5927(5) 0.0176(3) 0.0368(14) Uani 1 1 d . . . C19 C 0.8961(6) 0.6370(6) -0.0004(4) 0.0532(18) Uani 1 1 d . . . H19 H 0.9493 0.5918 -0.0049 0.080(5) Uiso 1 1 calc R . . C20 C 0.8984(6) 0.7468(6) -0.0116(4) 0.062(2) Uani 1 1 d . . . H20 H 0.9534 0.7768 -0.0228 0.080(5) Uiso 1 1 calc R . . C21 C 0.8173(6) 0.8114(6) -0.0059(4) 0.0582(19) Uani 1 1 d . . . H21 H 0.8156 0.8861 -0.0140 0.080(5) Uiso 1 1 calc R . . C22 C 0.7380(5) 0.7636(5) 0.0121(3) 0.0431(16) Uani 1 1 d . . . H22 H 0.6832 0.8076 0.0159 0.080(5) Uiso 1 1 calc R . . C23 C 0.7720(6) 0.3914(6) -0.0938(5) 0.075(2) Uani 1 1 d . . . H23A H 0.8118 0.3497 -0.1147 0.080(5) Uiso 1 1 calc R . . H23B H 0.7464 0.4599 -0.1218 0.080(5) Uiso 1 1 calc R . . H23C H 0.7023 0.3522 -0.1025 0.080(5) Uiso 1 1 calc R . . C24 C 0.7823(7) 0.1398(6) 0.0097(4) 0.060(2) Uani 1 1 d . . . C25 C 0.4390(6) 0.2283(6) -0.1071(4) 0.059(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0342(5) 0.0281(4) 0.0324(4) -0.0010(4) 0.0254(4) -0.0006(4) Co2 0.0420(5) 0.0321(4) 0.0421(5) 0.0012(4) 0.0312(4) 0.0061(4) O1 0.041(2) 0.0290(19) 0.023(2) 0.0026(17) 0.0263(18) 0.0038(17) O2 0.048(3) 0.043(2) 0.039(2) 0.0007(18) 0.036(2) 0.009(2) O3 0.023(2) 0.038(2) 0.037(2) 0.0045(18) 0.0206(18) 0.0023(17) O4 0.042(3) 0.068(3) 0.052(3) -0.012(2) 0.037(2) 0.003(2) O5 0.125(5) 0.107(5) 0.116(5) -0.009(4) 0.091(4) 0.035(4) O6 0.152(6) 0.118(5) 0.125(5) -0.084(5) 0.056(5) -0.006(5) N1 0.053(3) 0.027(3) 0.048(3) 0.011(2) 0.033(3) 0.007(2) N2 0.034(3) 0.029(3) 0.036(3) -0.008(2) 0.021(3) -0.004(2) N3 0.045(3) 0.040(3) 0.039(3) 0.003(2) 0.025(3) 0.013(3) N4 0.035(3) 0.040(3) 0.037(3) -0.001(2) 0.024(2) -0.005(2) N5 0.059(4) 0.052(4) 0.079(4) -0.010(3) 0.040(3) 0.015(3) N6 0.055(3) 0.024(3) 0.050(4) -0.011(2) 0.035(3) -0.003(2) C1 0.078(5) 0.036(4) 0.075(5) 0.010(4) 0.051(4) 0.013(4) C2 0.126(7) 0.034(4) 0.099(6) 0.018(4) 0.079(6) 0.007(4) C3 0.101(6) 0.058(5) 0.076(5) 0.017(4) 0.060(5) -0.005(4) C4 0.065(5) 0.045(4) 0.050(4) 0.005(3) 0.040(4) -0.007(3) C5 0.042(4) 0.035(3) 0.034(4) 0.009(3) 0.024(3) 0.002(3) C6 0.038(4) 0.033(3) 0.033(3) 0.005(3) 0.024(3) 0.009(3) C7 0.034(4) 0.029(3) 0.031(4) 0.001(3) 0.021(3) 0.007(3) C8 0.050(4) 0.047(4) 0.027(4) 0.004(3) 0.021(3) 0.006(3) C9 0.049(5) 0.060(4) 0.033(4) -0.016(3) 0.017(4) -0.003(4) C10 0.058(5) 0.062(5) 0.044(5) -0.008(3) 0.025(4) -0.014(4) C11 0.054(4) 0.048(4) 0.032(4) 0.000(3) 0.024(4) 0.004(3) C12 0.073(6) 0.052(4) 0.050(5) 0.008(4) 0.037(4) 0.025(4) C13 0.072(6) 0.071(6) 0.046(5) 0.005(4) 0.011(5) 0.030(5) C14 0.043(5) 0.074(6) 0.081(6) -0.002(5) 0.003(5) 0.009(5) C15 0.029(4) 0.068(5) 0.069(5) 0.003(4) 0.019(4) -0.003(4) C16 0.034(4) 0.043(4) 0.050(4) -0.002(3) 0.026(3) 0.006(3) C17 0.030(4) 0.045(4) 0.039(4) -0.001(3) 0.025(3) 0.007(3) C18 0.034(4) 0.047(4) 0.040(4) 0.003(3) 0.026(3) -0.002(3) C19 0.052(4) 0.063(5) 0.073(5) 0.006(4) 0.052(4) 0.000(4) C20 0.062(5) 0.066(5) 0.089(6) 0.013(4) 0.061(5) -0.002(4) C21 0.067(5) 0.055(4) 0.065(5) 0.004(4) 0.044(4) -0.018(4) C22 0.048(4) 0.037(4) 0.052(4) -0.006(3) 0.033(4) -0.016(3) C23 0.073(5) 0.097(6) 0.082(6) -0.003(5) 0.059(5) 0.010(5) C24 0.067(6) 0.059(5) 0.055(5) 0.000(4) 0.033(4) 0.020(4) C25 0.052(5) 0.048(4) 0.066(6) -0.013(4) 0.025(4) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.025(3) . ? Co1 N6 2.088(4) 3_665 ? Co1 N4 2.096(4) . ? Co1 O1 2.133(3) 3_665 ? Co1 N2 2.162(4) . ? Co1 O3 2.193(3) . ? Co2 N5 2.025(5) . ? Co2 O3 2.046(3) . ? Co2 N1 2.135(4) . ? Co2 N6 2.146(5) . ? Co2 N3 2.217(5) . ? Co2 O1 2.244(3) . ? O1 C6 1.382(6) . ? O1 Co1 2.133(3) 3_665 ? O2 C6 1.416(6) . ? O2 H1O2 0.8200 . ? O3 C17 1.375(6) . ? O4 C23 1.381(7) . ? O4 C17 1.437(6) . ? O5 C24 1.208(8) . ? O6 C25 1.193(8) . ? N1 C1 1.354(7) . ? N1 C5 1.357(6) . ? N2 C11 1.331(7) . ? N2 C7 1.347(6) . ? N3 C12 1.330(7) . ? N3 C16 1.360(7) . ? N4 C18 1.348(6) . ? N4 C22 1.347(7) . ? N5 C24 1.127(8) . ? N6 C25 1.165(7) . ? N6 Co1 2.088(4) 3_665 ? C1 C2 1.360(9) . ? C1 H1 0.9300 . ? C2 C3 1.374(9) . ? C2 H2 0.9300 . ? C3 C4 1.385(8) . ? C3 H3 0.9300 . ? C4 C5 1.388(7) . ? C4 H4 0.9300 . ? C5 C6 1.519(7) . ? C6 C7 1.527(7) . ? C7 C8 1.391(7) . ? C8 C9 1.385(8) . ? C8 H8 0.9300 . ? C9 C10 1.382(8) . ? C9 H9 0.9300 . ? C10 C11 1.367(8) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.372(9) . ? C12 H12 0.9300 . ? C13 C14 1.371(10) . ? C13 H13 0.9300 . ? C14 C15 1.393(9) . ? C14 H14 0.9300 . ? C15 C16 1.371(7) . ? C15 H15 0.9300 . ? C16 C17 1.537(8) . ? C17 C18 1.532(7) . ? C18 C19 1.378(7) . ? C19 C20 1.371(8) . ? C19 H19 0.9300 . ? C20 C21 1.375(8) . ? C20 H20 0.9300 . ? C21 C22 1.388(7) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N6 106.87(15) . 3_665 ? O1 Co1 N4 153.96(16) . . ? N6 Co1 N4 98.91(18) 3_665 . ? O1 Co1 O1 81.73(13) . 3_665 ? N6 Co1 O1 81.81(16) 3_665 3_665 ? N4 Co1 O1 105.95(14) . 3_665 ? O1 Co1 N2 76.79(15) . . ? N6 Co1 N2 92.31(17) 3_665 . ? N4 Co1 N2 98.91(17) . . ? O1 Co1 N2 155.04(15) 3_665 . ? O1 Co1 O3 80.55(13) . . ? N6 Co1 O3 164.48(16) 3_665 . ? N4 Co1 O3 75.35(15) . . ? O1 Co1 O3 85.92(12) 3_665 . ? N2 Co1 O3 102.76(14) . . ? N5 Co2 O3 109.04(19) . . ? N5 Co2 N1 99.7(2) . . ? O3 Co2 N1 149.25(16) . . ? N5 Co2 N6 95.44(19) . . ? O3 Co2 N6 93.33(15) . . ? N1 Co2 N6 94.63(18) . . ? N5 Co2 N3 88.66(19) . . ? O3 Co2 N3 75.27(16) . . ? N1 Co2 N3 95.17(18) . . ? N6 Co2 N3 168.59(18) . . ? N5 Co2 O1 170.18(18) . . ? O3 Co2 O1 78.90(12) . . ? N1 Co2 O1 73.82(15) . . ? N6 Co2 O1 78.01(14) . . ? N3 Co2 O1 99.16(14) . . ? C6 O1 Co1 116.9(3) . . ? C6 O1 Co1 129.8(3) . 3_665 ? Co1 O1 Co1 98.27(13) . 3_665 ? C6 O1 Co2 110.6(3) . . ? Co1 O1 Co2 98.53(13) . . ? Co1 O1 Co2 97.15(12) 3_665 . ? C6 O2 H1O2 109.4 . . ? C17 O3 Co2 117.7(3) . . ? C17 O3 Co1 109.2(3) . . ? Co2 O3 Co1 99.58(14) . . ? C23 O4 C17 116.4(4) . . ? C1 N1 C5 118.2(5) . . ? C1 N1 Co2 123.4(4) . . ? C5 N1 Co2 117.2(3) . . ? C11 N2 C7 118.5(5) . . ? C11 N2 Co1 127.5(4) . . ? C7 N2 Co1 113.9(4) . . ? C12 N3 C16 118.2(5) . . ? C12 N3 Co2 127.7(5) . . ? C16 N3 Co2 113.8(4) . . ? C18 N4 C22 118.3(5) . . ? C18 N4 Co1 116.0(4) . . ? C22 N4 Co1 125.6(4) . . ? C24 N5 Co2 153.1(6) . . ? C25 N6 Co1 128.2(5) . 3_665 ? C25 N6 Co2 129.6(5) . . ? Co1 N6 Co2 101.66(19) 3_665 . ? N1 C1 C2 122.8(6) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 119.0(6) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 119.7(7) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 118.8(6) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.4(5) . . ? N1 C5 C6 114.5(5) . . ? C4 C5 C6 124.0(5) . . ? O1 C6 O2 109.8(4) . . ? O1 C6 C5 108.1(4) . . ? O2 C6 C5 109.1(4) . . ? O1 C6 C7 110.2(4) . . ? O2 C6 C7 106.8(4) . . ? C5 C6 C7 112.8(4) . . ? N2 C7 C8 121.8(5) . . ? N2 C7 C6 114.7(5) . . ? C8 C7 C6 123.4(5) . . ? C9 C8 C7 118.3(6) . . ? C9 C8 H8 120.8 . . ? C7 C8 H8 120.9 . . ? C10 C9 C8 119.5(6) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 118.5(6) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.7 . . ? N2 C11 C10 123.3(6) . . ? N2 C11 H11 118.4 . . ? C10 C11 H11 118.3 . . ? N3 C12 C13 122.6(7) . . ? N3 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C14 C13 C12 119.5(7) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 118.7(7) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 119.0(7) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? N3 C16 C15 121.9(6) . . ? N3 C16 C17 114.0(5) . . ? C15 C16 C17 124.1(6) . . ? O3 C17 O4 113.7(4) . . ? O3 C17 C18 108.6(4) . . ? O4 C17 C18 109.9(5) . . ? O3 C17 C16 111.1(5) . . ? O4 C17 C16 101.2(4) . . ? C18 C17 C16 112.3(5) . . ? N4 C18 C19 121.0(5) . . ? N4 C18 C17 114.7(5) . . ? C19 C18 C17 124.3(6) . . ? C20 C19 C18 121.0(6) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 C19 118.2(6) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.9 . . ? C20 C21 C22 119.0(6) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? N4 C22 C21 122.5(6) . . ? N4 C22 H22 118.7 . . ? C21 C22 H22 118.8 . . ? O4 C23 H23A 109.4 . . ? O4 C23 H23B 109.4 . . ? H23A C23 H23B 109.5 . . ? O4 C23 H23C 109.6 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 O5 177.8(8) . . ? N6 C25 O6 178.1(8) . . ? _diffrn_measured_fraction_theta_max 0.830 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.830 _refine_diff_density_max 0.531 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.093