# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1855 data_A910259K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H48 Cr N7 O7 S4' _chemical_formula_weight 955.12 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2051(5) _cell_length_b 9.5548(7) _cell_length_c 16.1340(11) _cell_angle_alpha 75.502(3) _cell_angle_beta 78.898(4) _cell_angle_gamma 74.485(4) _cell_volume 1169.23(14) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 499 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9103 _exptl_absorpt_correction_T_max 0.9103 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12540 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 26.03 _reflns_number_total 4554 _reflns_number_gt 3424 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+0.2763P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0088(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4554 _refine_ls_number_parameters 366 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.991 _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 Cr1 Cr 0.5000 -1.0000 -0.5000 0.02216(16) Uani 1 2 d S . . S1 S 1.00907(8) -0.94129(7) -0.68523(4) 0.03434(18) Uani 1 1 d . . . S2 S 0.50927(9) -0.82934(8) -0.24949(4) 0.0435(2) Uani 1 1 d . . . N2 N 0.7122(2) -0.9486(2) -0.56847(12) 0.0283(4) Uani 1 1 d . . . N3 N 0.5400(2) -0.9377(2) -0.39817(12) 0.0286(4) Uani 1 1 d . . . N1 N 0.3658(2) -0.7840(2) -0.54288(11) 0.0236(4) Uani 1 1 d . . . C1 C 0.2111(3) -0.7563(2) -0.56407(13) 0.0240(5) Uani 1 1 d . . . H1 H 0.1631 -0.8382 -0.5605 0.027(6) Uiso 1 1 calc R . . C2 C 0.1128(3) -0.6115(2) -0.59185(13) 0.0246(5) Uani 1 1 d . . . C3 C 0.1856(3) -0.4896(2) -0.59869(14) 0.0267(5) Uani 1 1 d . . . C4 C 0.3523(3) -0.5223(3) -0.57654(14) 0.0289(5) Uani 1 1 d . . . H4 H 0.4060 -0.4437 -0.5807 0.037(7) Uiso 1 1 calc R . . C5 C 0.4359(3) -0.6650(3) -0.54948(14) 0.0267(5) Uani 1 1 d . . . H5 H 0.5473 -0.6837 -0.5344 0.032(6) Uiso 1 1 calc R . . C6 C -0.0532(3) -0.5857(3) -0.61323(14) 0.0293(5) Uani 1 1 d . . . H6 H -0.1018 -0.6673 -0.6093 0.036(7) Uiso 1 1 calc R . . C7 C -0.1439(3) -0.4440(3) -0.63947(15) 0.0328(6) Uani 1 1 d . . . H7 H -0.2561 -0.4268 -0.6532 0.038(7) Uiso 1 1 calc R . . C8 C -0.0707(3) -0.3232(3) -0.64619(15) 0.0336(6) Uani 1 1 d . . . H8 H -0.1342 -0.2250 -0.6651 0.053(8) Uiso 1 1 calc R . . C9 C 0.0886(3) -0.3441(3) -0.62625(15) 0.0321(6) Uani 1 1 d . . . H9 H 0.1349 -0.2610 -0.6308 0.049(8) Uiso 1 1 calc R . . C10 C 0.8363(3) -0.9452(2) -0.61786(14) 0.0240(5) Uani 1 1 d . . . C11 C 0.5266(3) -0.8926(2) -0.33576(14) 0.0264(5) Uani 1 1 d . . . C12 C 0.2026(5) -0.6892(4) -1.03917(19) 0.0484(8) Uani 1 1 d . . . H12A H 0.103(4) -0.721(3) -1.0314(18) 0.059(9) Uiso 1 1 d . . . H12B H 0.297(4) -0.759(3) -1.0615(18) 0.047(8) Uiso 1 1 d . . . C13 C 0.2625(4) -0.7834(3) -0.89545(18) 0.0453(7) Uani 1 1 d . . . H13A H 0.3577 -0.8627 -0.9139 0.041(7) Uiso 1 1 calc R . . H13B H 0.1577 -0.8220 -0.8790 0.061(9) Uiso 1 1 calc R . . C14 C 0.3013(3) -0.7402(3) -0.82036(17) 0.0437(7) Uani 1 1 d . . . H14A H 0.2113 -0.6547 -0.8053 0.065(10) Uiso 1 1 calc R . . H14B H 0.3046 -0.8241 -0.7697 0.045(7) Uiso 1 1 calc R . . C15 C 0.5127(4) -0.6664(3) -0.77141(16) 0.0461(7) Uani 1 1 d . . . H15A H 0.5202 -0.7528 -0.7222 0.048(8) Uiso 1 1 calc R . . H15B H 0.4270 -0.5815 -0.7526 0.059(9) Uiso 1 1 calc R . . C16 C 0.6832(4) -0.6275(3) -0.79921(16) 0.0456(7) Uani 1 1 d . . . H16A H 0.7250 -0.6129 -0.7491 0.074(10) Uiso 1 1 calc R . . H16B H 0.7668 -0.7094 -0.8221 0.061(9) Uiso 1 1 calc R . . C17 C 0.8242(4) -0.4489(4) -0.89185(18) 0.0461(7) Uani 1 1 d . . . H17A H 0.920(4) -0.540(3) -0.9146(18) 0.055(8) Uiso 1 1 d . . . H17B H 0.859(4) -0.424(3) -0.8399(19) 0.056(8) Uiso 1 1 d . . . O1 O 0.2390(2) -0.65615(19) -0.96471(10) 0.0360(4) Uani 1 1 d . . . O2 O 0.4628(2) -0.70108(18) -0.84224(10) 0.0350(4) Uani 1 1 d . . . O3 O 0.6666(2) -0.49503(19) -0.86416(10) 0.0367(4) Uani 1 1 d . . . O4 O 0.4467(5) -0.4403(4) -0.9817(2) 0.0487(10) Uani 0.50 1 d PG . . H1O H 0.5486 -0.4702 -0.9682 0.073 Uiso 0.50 1 d PG . . H2O H 0.4103 -0.5168 -0.9756 0.073 Uiso 0.50 1 d PG . . N4 N -0.2160(9) 0.1644(8) -0.0451(6) 0.0514(18) Uani 0.50 1 d PD . . H19 H -0.3131 0.2310 -0.0503 0.062 Uiso 0.50 1 calc PR . . C19 C -0.0295(14) -0.0231(11) 0.0467(8) 0.039(3) Uani 0.50 1 d PD . . C18 C -0.1812(16) 0.0870(12) 0.0300(6) 0.041(3) Uani 0.50 1 d PD . . H18 H -0.2644 0.1053 0.0783 0.049 Uiso 0.50 1 calc PR . . C20 C 0.0900(15) -0.0423(14) -0.0279(6) 0.037(3) Uani 0.50 1 d PD . . C21 C 0.0498(13) 0.0397(10) -0.1108(7) 0.039(2) Uani 0.50 1 d PD . . H21 H 0.1270 0.0233 -0.1613 0.046 Uiso 0.50 1 calc PR . . C22 C -0.1004(15) 0.1416(13) -0.1165(8) 0.046(3) Uani 0.50 1 d PD . . H22 H -0.1261 0.1989 -0.1717 0.055 Uiso 0.50 1 calc PR . . C23 C 0.0051(14) -0.1067(12) 0.1273(7) 0.037(2) Uani 0.50 1 d PD . . H23 H -0.0782 -0.0942 0.1763 0.044 Uiso 0.50 1 calc PR . . C24 C 0.1563(14) -0.2064(11) 0.1375(7) 0.054(3) Uani 0.50 1 d PD . . H24 H 0.1807 -0.2608 0.1934 0.065 Uiso 0.50 1 calc PR . . C25 C 0.2730(11) -0.2276(11) 0.0663(6) 0.056(2) Uani 0.50 1 d PD . . H25 H 0.3776 -0.2988 0.0745 0.067 Uiso 0.50 1 calc PR . . C26 C 0.2482(14) -0.1525(12) -0.0160(10) 0.054(3) Uani 0.50 1 d PD . . H26 H 0.3321 -0.1720 -0.0638 0.064 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0194(3) 0.0225(3) 0.0218(3) -0.0040(2) -0.0026(2) -0.0010(2) S1 0.0291(3) 0.0328(4) 0.0386(4) -0.0080(3) 0.0074(3) -0.0111(3) S2 0.0453(4) 0.0520(5) 0.0339(4) -0.0198(3) -0.0110(3) 0.0013(3) N2 0.0242(10) 0.0259(11) 0.0301(10) -0.0033(8) -0.0033(9) -0.0006(8) N3 0.0264(10) 0.0281(11) 0.0285(10) -0.0058(9) -0.0058(8) -0.0003(8) N1 0.0243(10) 0.0251(10) 0.0207(9) -0.0067(8) -0.0020(7) -0.0032(8) C1 0.0227(12) 0.0235(12) 0.0242(11) -0.0059(9) -0.0034(9) -0.0019(10) C2 0.0263(12) 0.0231(12) 0.0211(11) -0.0045(9) -0.0032(9) -0.0004(10) C3 0.0299(13) 0.0254(13) 0.0227(11) -0.0064(9) -0.0019(9) -0.0028(10) C4 0.0303(13) 0.0284(13) 0.0309(12) -0.0102(10) -0.0051(10) -0.0068(11) C5 0.0245(12) 0.0290(13) 0.0267(12) -0.0067(10) -0.0029(9) -0.0058(10) C6 0.0308(13) 0.0244(13) 0.0316(12) -0.0042(10) -0.0084(10) -0.0031(10) C7 0.0277(13) 0.0339(14) 0.0327(13) -0.0066(11) -0.0095(10) 0.0032(11) C8 0.0389(14) 0.0232(13) 0.0315(13) -0.0035(10) -0.0078(11) 0.0049(11) C9 0.0377(14) 0.0236(13) 0.0326(13) -0.0037(10) -0.0066(11) -0.0038(11) C10 0.0273(13) 0.0159(11) 0.0274(12) -0.0028(9) -0.0078(10) -0.0017(9) C11 0.0210(12) 0.0259(13) 0.0271(12) -0.0007(10) -0.0057(9) 0.0006(10) C12 0.0517(19) 0.059(2) 0.0472(17) -0.0173(15) -0.0034(14) -0.0305(17) C13 0.0416(16) 0.0390(16) 0.0542(17) 0.0013(13) -0.0004(13) -0.0221(14) C14 0.0375(15) 0.0492(17) 0.0363(14) 0.0073(13) 0.0033(12) -0.0173(14) C15 0.0558(18) 0.0549(19) 0.0272(14) -0.0013(13) -0.0038(12) -0.0200(16) C16 0.0560(18) 0.0520(18) 0.0319(14) -0.0027(13) -0.0170(13) -0.0158(15) C17 0.0400(16) 0.070(2) 0.0373(15) -0.0126(15) -0.0082(12) -0.0246(16) O1 0.0377(10) 0.0373(10) 0.0342(9) -0.0031(8) -0.0024(7) -0.0165(8) O2 0.0358(10) 0.0381(10) 0.0282(9) -0.0012(7) 0.0008(7) -0.0129(8) O3 0.0350(10) 0.0399(10) 0.0342(9) -0.0039(8) -0.0050(7) -0.0103(8) O4 0.053(3) 0.049(3) 0.045(2) 0.0050(19) -0.0140(19) -0.021(2) N4 0.047(5) 0.040(4) 0.064(5) -0.015(4) -0.021(4) 0.010(3) C19 0.040(6) 0.040(6) 0.043(7) -0.016(5) -0.005(4) -0.011(4) C18 0.043(8) 0.038(7) 0.039(4) -0.019(5) 0.012(7) -0.008(6) C20 0.036(8) 0.051(9) 0.030(5) -0.022(6) 0.010(7) -0.018(7) C21 0.051(6) 0.037(5) 0.035(6) -0.021(4) 0.001(4) -0.014(4) C22 0.048(9) 0.054(8) 0.040(6) -0.020(5) -0.005(6) -0.012(8) C23 0.041(7) 0.036(6) 0.033(4) -0.010(4) 0.000(5) -0.008(6) C24 0.045(6) 0.066(7) 0.049(5) -0.020(5) -0.011(4) 0.000(5) C25 0.035(4) 0.059(6) 0.072(6) -0.029(5) -0.016(4) 0.015(4) C26 0.042(6) 0.060(7) 0.064(7) -0.039(7) 0.006(5) -0.005(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 Cr1 N2 1.9842(19) 2_634 ? Cr1 N2 1.9842(19) . ? Cr1 N3 1.9906(19) 2_634 ? Cr1 N3 1.9906(19) . ? Cr1 N1 2.0772(18) . ? Cr1 N1 2.0772(18) 2_634 ? S1 C10 1.614(2) . ? S2 C11 1.619(2) . ? N2 C10 1.169(3) . ? N3 C11 1.167(3) . ? N1 C1 1.320(3) . ? N1 C5 1.378(3) . ? C1 C2 1.413(3) . ? C1 H1 0.9500 . ? C2 C6 1.412(3) . ? C2 C3 1.417(3) . ? C3 C9 1.414(3) . ? C3 C4 1.414(3) . ? C4 C5 1.355(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.365(3) . ? C6 H6 0.9500 . ? C7 C8 1.410(3) . ? C7 H7 0.9500 . ? C8 C9 1.357(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C12 O1 1.418(3) . ? C12 C17 1.494(4) 2_643 ? C12 H12A 0.92(3) . ? C12 H12B 0.96(3) . ? C13 O1 1.429(3) . ? C13 C14 1.486(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O2 1.427(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O2 1.424(3) . ? C15 C16 1.499(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O3 1.420(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O3 1.432(3) . ? C17 C12 1.494(4) 2_643 ? C17 H17A 1.10(3) . ? C17 H17B 1.03(3) . ? O4 H1O 0.8596 . ? O4 H2O 0.8387 . ? N4 C18 1.292(13) . ? N4 C22 1.367(14) . ? N4 H19 0.8800 . ? C19 C23 1.382(14) . ? C19 C20 1.415(12) . ? C19 C18 1.419(12) . ? C18 H18 0.9500 . ? C20 C21 1.420(13) . ? C20 C26 1.447(13) . ? C21 C22 1.354(13) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.357(12) . ? C23 H23 0.9500 . ? C24 C25 1.366(14) . ? C24 H24 0.9500 . ? C25 C26 1.366(16) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cr1 N2 180.0 2_634 . ? N2 Cr1 N3 91.64(8) 2_634 2_634 ? N2 Cr1 N3 88.36(8) . 2_634 ? N2 Cr1 N3 88.36(8) 2_634 . ? N2 Cr1 N3 91.64(8) . . ? N3 Cr1 N3 180.0 2_634 . ? N2 Cr1 N1 90.33(7) 2_634 . ? N2 Cr1 N1 89.67(7) . . ? N3 Cr1 N1 91.25(7) 2_634 . ? N3 Cr1 N1 88.75(7) . . ? N2 Cr1 N1 89.67(7) 2_634 2_634 ? N2 Cr1 N1 90.33(7) . 2_634 ? N3 Cr1 N1 88.75(7) 2_634 2_634 ? N3 Cr1 N1 91.25(7) . 2_634 ? N1 Cr1 N1 180.00(9) . 2_634 ? C10 N2 Cr1 163.92(18) . . ? C11 N3 Cr1 165.78(18) . . ? C1 N1 C5 118.05(19) . . ? C1 N1 Cr1 121.20(14) . . ? C5 N1 Cr1 120.75(15) . . ? N1 C1 C2 123.5(2) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C6 C2 C1 122.1(2) . . ? C6 C2 C3 119.7(2) . . ? C1 C2 C3 118.2(2) . . ? C9 C3 C4 124.1(2) . . ? C9 C3 C2 118.8(2) . . ? C4 C3 C2 117.2(2) . . ? C5 C4 C3 120.4(2) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 N1 122.7(2) . . ? C4 C5 H5 118.7 . . ? N1 C5 H5 118.7 . . ? C7 C6 C2 120.2(2) . . ? C7 C6 H6 119.9 . . ? C2 C6 H6 119.9 . . ? C6 C7 C8 119.8(2) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 121.5(2) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C3 120.0(2) . . ? C8 C9 H9 120.0 . . ? C3 C9 H9 120.0 . . ? N2 C10 S1 179.4(2) . . ? N3 C11 S2 179.6(2) . . ? O1 C12 C17 109.5(2) . 2_643 ? O1 C12 H12A 114.7(18) . . ? C17 C12 H12A 104.2(19) 2_643 . ? O1 C12 H12B 110.3(17) . . ? C17 C12 H12B 107.3(17) 2_643 . ? H12A C12 H12B 110(2) . . ? O1 C13 C14 109.0(2) . . ? O1 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? O1 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? O2 C14 C13 109.0(2) . . ? O2 C14 H14A 109.9 . . ? C13 C14 H14A 109.9 . . ? O2 C14 H14B 109.9 . . ? C13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? O2 C15 C16 108.9(2) . . ? O2 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? O2 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? O3 C16 C15 109.2(2) . . ? O3 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? O3 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? O3 C17 C12 109.0(2) . 2_643 ? O3 C17 H17A 108.0(15) . . ? C12 C17 H17A 112.2(15) 2_643 . ? O3 C17 H17B 108.4(15) . . ? C12 C17 H17B 108.3(16) 2_643 . ? H17A C17 H17B 111(2) . . ? C12 O1 C13 112.3(2) . . ? C15 O2 C14 112.06(18) . . ? C16 O3 C17 112.1(2) . . ? H1O O4 H2O 106.4 . . ? C18 N4 C22 119.3(8) . . ? C18 N4 H19 120.4 . . ? C22 N4 H19 120.4 . . ? C23 C19 C20 120.8(12) . . ? C23 C19 C18 125.1(11) . . ? C20 C19 C18 114.1(13) . . ? N4 C18 C19 125.7(11) . . ? N4 C18 H18 117.2 . . ? C19 C18 H18 117.2 . . ? C19 C20 C21 120.2(14) . . ? C19 C20 C26 117.3(11) . . ? C21 C20 C26 122.4(11) . . ? C22 C21 C20 118.9(10) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 N4 121.8(9) . . ? C21 C22 H22 119.1 . . ? N4 C22 H22 119.1 . . ? C24 C23 C19 121.0(9) . . ? C24 C23 H23 119.5 . . ? C19 C23 H23 119.5 . . ? C23 C24 C25 119.1(9) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C24 C25 C26 123.9(9) . . ? C24 C25 H25 118.1 . . ? C26 C25 H25 118.1 . . ? C25 C26 C20 117.8(11) . . ? C25 C26 H26 121.1 . . ? C20 C26 H26 121.1 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.340 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.055