Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Rita Delgado' _publ_contact_author_address ; ITQB - Instituto de Tecnologia Quimica e Biologica, UNL Apartado 127 Oeiras 2781-901 PORTUGAL ; _publ_contact_author_email DELGADO@ITQB.UNL.PT _publ_section_title ; New dioxadiaza- and trioxadiaza- macrocycles containing one dibenzofuran unit with two amino pendant arms: synthesis, protonation and complexation studies ; loop_ _publ_author_name R.Delgado M.Drew V.Felix 'Feng Li.' 'Li Li.' data_compound_cu_complex _database_code_depnum_ccdc_archive 'CCDC 629721' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 Cl Cu N5 O6' _chemical_formula_weight 587.55 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.301(3) _cell_length_b 11.589(3) _cell_length_c 12.641(3) _cell_angle_alpha 76.76(2) _cell_angle_beta 85.04(2) _cell_angle_gamma 77.46(2) _cell_volume 1293.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 614 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_type Empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 1.00 _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 'Oxford Diffaction X-Calibur System' _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 8864 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.2345 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 30.19 _reflns_number_total 7079 _reflns_number_gt 2861 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,1999) _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^)+(0.0785P)^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 7079 _refine_ls_number_parameters 327 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1575 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1769 _refine_ls_wR_factor_gt 0.1595 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.882 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C12 C 0.9119(5) 0.8026(4) 0.7979(4) 0.0247(12) Uani 1 d . . . H12A H 0.9283 0.8301 0.7186 0.030 Uiso 1 calc R . . H12B H 1.0086 0.7867 0.8314 0.030 Uiso 1 calc R . . C13 C 0.8129(5) 0.9061(4) 0.8392(4) 0.0223(11) Uani 1 d . . . C14 C 0.8709(6) 0.9743(4) 0.8979(4) 0.0282(12) Uani 1 d . . . H14 H 0.9705 0.9485 0.9186 0.034 Uiso 1 calc R . . C15 C 0.7850(6) 1.0801(4) 0.9270(4) 0.0308(13) Uani 1 d . . . H15 H 0.8286 1.1245 0.9654 0.037 Uiso 1 calc R . . C16 C 0.6382(6) 1.1201(4) 0.9003(4) 0.0263(12) Uani 1 d . . . H16 H 0.5817 1.1919 0.9187 0.032 Uiso 1 calc R . . C17 C 0.5751(5) 1.0520(4) 0.8454(4) 0.0242(12) Uani 1 d . . . C18 C 0.6637(5) 0.9485(4) 0.8178(4) 0.0240(12) Uani 1 d . . . C20 C 0.4368(6) 0.9563(4) 0.7653(4) 0.0271(12) Uani 1 d . . . C21 C 0.4284(6) 1.0582(4) 0.8085(4) 0.0249(12) Uani 1 d . . . C22 C 0.2898(6) 1.1374(4) 0.8123(4) 0.0309(13) Uani 1 d . . . H22 H 0.2781 1.2075 0.8416 0.037 Uiso 1 calc R . . C23 C 0.1728(6) 1.1087(5) 0.7718(4) 0.0316(13) Uani 1 d . . . H23 H 0.0792 1.1615 0.7727 0.038 Uiso 1 calc R . . C24 C 0.1852(6) 1.0056(4) 0.7293(4) 0.0298(13) Uani 1 d . . . H24 H 0.1010 0.9913 0.7007 0.036 Uiso 1 calc R . . C25 C 0.3199(5) 0.9226(4) 0.7281(4) 0.0239(12) Uani 1 d . . . C26 C 0.3226(5) 0.8018(4) 0.6976(4) 0.0278(12) Uani 1 d . . . H26A H 0.3020 0.7437 0.7650 0.033 Uiso 1 calc R . . H26B H 0.2398 0.8142 0.6492 0.033 Uiso 1 calc R . . C28 C 0.4206(6) 0.6385(4) 0.6052(5) 0.0356(14) Uani 1 d . . . H28A H 0.3264 0.6688 0.5674 0.043 Uiso 1 calc R . . H28B H 0.4973 0.6122 0.5515 0.043 Uiso 1 calc R . . C29 C 0.4048(6) 0.5296(4) 0.6940(4) 0.0311(13) Uani 1 d . . . H29A H 0.3318 0.5560 0.7499 0.037 Uiso 1 calc R . . H29B H 0.3659 0.4722 0.6627 0.037 Uiso 1 calc R . . C31 C 0.6405(6) 0.3981(5) 0.6803(5) 0.0360(14) Uani 1 d . . . H31A H 0.6437 0.4434 0.6038 0.043 Uiso 1 calc R . . H31B H 0.6099 0.3210 0.6819 0.043 Uiso 1 calc R . . C32 C 0.7904(6) 0.3735(4) 0.7286(5) 0.0402(15) Uani 1 d . . . H32A H 0.7863 0.3301 0.8056 0.048 Uiso 1 calc R . . H32B H 0.8641 0.3227 0.6882 0.048 Uiso 1 calc R . . C34 C 0.9628(5) 0.4741(4) 0.7806(4) 0.0270(12) Uani 1 d . . . H34A H 1.0479 0.4255 0.7472 0.032 Uiso 1 calc R . . H34B H 0.9486 0.4316 0.8569 0.032 Uiso 1 calc R . . C35 C 0.9917(5) 0.5982(4) 0.7771(4) 0.0262(12) Uani 1 d . . . H35A H 1.0187 0.6348 0.7012 0.031 Uiso 1 calc R . . H35B H 1.0772 0.5892 0.8220 0.031 Uiso 1 calc R . . C112 C 0.6645(5) 0.6643(4) 0.9612(4) 0.0243(11) Uani 1 d . . . H11A H 0.6426 0.6205 1.0357 0.029 Uiso 1 calc R . . H11B H 0.6264 0.7520 0.9562 0.029 Uiso 1 calc R . . N113 N 0.5933(4) 0.6216(3) 0.8800(3) 0.0210(9) Uani 1 d . . . H11C H 0.4926 0.6470 0.8854 0.025 Uiso 1 calc R . . H11D H 0.6145 0.5384 0.8937 0.025 Uiso 1 calc R . . C271 C 0.4977(6) 0.8308(5) 0.5426(4) 0.0321(13) Uani 1 d . . . H27A H 0.4947 0.9097 0.5613 0.039 Uiso 1 calc R . . H27B H 0.4234 0.8432 0.4874 0.039 Uiso 1 calc R . . C272 C 0.6507(6) 0.7852(5) 0.4952(4) 0.0335(13) Uani 1 d . . . H27C H 0.6500 0.7148 0.4634 0.040 Uiso 1 calc R . . H27D H 0.6809 0.8498 0.4373 0.040 Uiso 1 calc R . . N11 N 0.8615(4) 0.6843(3) 0.8173(3) 0.0224(9) Uani 1 d . . . N27 N 0.4604(4) 0.7421(3) 0.6426(3) 0.0250(10) Uani 1 d . . . C111 C 0.8288(5) 0.6401(4) 0.9363(4) 0.0244(12) Uani 1 d . . . H11E H 0.8769 0.6817 0.9792 0.029 Uiso 1 calc R . . H11F H 0.8695 0.5521 0.9576 0.029 Uiso 1 calc R . . N273 N 0.7544(5) 0.7498(4) 0.5854(3) 0.0316(11) Uani 1 d . . . H27E H 0.7922 0.8159 0.5885 0.038 Uiso 1 calc R . . H27F H 0.8317 0.6910 0.5695 0.038 Uiso 1 calc R . . O19 O 0.5831(4) 0.8889(3) 0.7665(3) 0.0252(8) Uani 1 d . . . O30 O 0.5387(4) 0.4684(3) 0.7447(3) 0.0331(9) Uani 1 d . . . O33 O 0.8309(4) 0.4880(3) 0.7210(3) 0.0309(9) Uani 1 d . . . Cu Cu 0.66704(7) 0.68762(5) 0.73153(5) 0.0242(2) Uani 1 d . . . Cl Cl 0.75133(14) 0.34731(10) 1.03272(10) 0.0276(3) Uani 1 d . . . N81 N 0.9304(8) 1.0799(5) 0.5202(8) 0.073(4) Uiso 0.50 d PD . 1 O83 O 0.8804(8) 1.1834(5) 0.5370(7) 0.058(2) Uiso 0.50 d PD A 1 O82 O 0.8588(7) 0.9982(5) 0.5528(6) 0.042(2) Uiso 0.50 d PD . 1 O84 O 1.0498(7) 1.0589(7) 0.4681(8) 0.078(3) Uiso 0.50 d PD . 1 N91 N 1.0000 0.5000 0.5000 0.085(3) Uiso 1 d SD . 1 O92 O 1.0681(11) 0.3960(4) 0.5419(12) 0.196(8) Uiso 0.50 d PD . 1 O93 O 0.8738(4) 0.5127(8) 0.4660(7) 0.062(3) Uiso 0.50 d PD . 1 O94 O 1.0416(10) 0.5901(5) 0.5155(9) 0.107(4) Uiso 0.50 d PD . 1 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 C12 0.020(3) 0.022(3) 0.035(3) -0.009(2) -0.005(2) -0.005(2) C13 0.024(3) 0.016(2) 0.025(3) -0.002(2) 0.004(2) -0.005(2) C14 0.028(3) 0.023(3) 0.036(3) -0.007(2) -0.002(2) -0.010(2) C15 0.040(3) 0.021(3) 0.036(3) -0.008(2) -0.004(3) -0.012(2) C16 0.028(3) 0.022(3) 0.030(3) -0.011(2) 0.004(2) -0.004(2) C17 0.026(3) 0.019(3) 0.027(3) -0.006(2) -0.002(2) -0.004(2) C18 0.027(3) 0.021(3) 0.029(3) -0.010(2) 0.000(2) -0.011(2) C20 0.024(3) 0.021(3) 0.033(3) -0.002(2) 0.001(2) -0.003(2) C21 0.033(3) 0.017(2) 0.022(3) 0.000(2) 0.004(2) -0.005(2) C22 0.029(3) 0.023(3) 0.040(4) -0.009(2) 0.001(3) -0.002(2) C23 0.023(3) 0.029(3) 0.038(3) -0.002(2) 0.004(2) -0.002(2) C24 0.030(3) 0.027(3) 0.031(3) -0.005(2) 0.003(2) -0.004(2) C25 0.024(3) 0.016(2) 0.029(3) 0.002(2) 0.000(2) -0.006(2) C26 0.024(3) 0.023(3) 0.034(3) -0.001(2) -0.002(2) -0.004(2) C28 0.035(3) 0.028(3) 0.044(4) -0.010(3) -0.010(3) -0.002(2) C29 0.023(3) 0.028(3) 0.046(4) -0.016(3) 0.004(3) -0.009(2) C31 0.037(3) 0.029(3) 0.050(4) -0.024(3) -0.004(3) -0.005(2) C32 0.041(4) 0.017(3) 0.063(4) -0.015(3) 0.001(3) -0.001(2) C34 0.021(3) 0.023(3) 0.036(3) -0.009(2) 0.001(2) -0.002(2) C35 0.021(3) 0.019(3) 0.038(3) -0.008(2) 0.004(2) -0.003(2) C112 0.022(3) 0.027(3) 0.026(3) -0.010(2) 0.001(2) -0.007(2) N113 0.019(2) 0.018(2) 0.025(2) -0.0033(17) -0.0006(18) -0.0037(16) C271 0.033(3) 0.031(3) 0.026(3) -0.001(2) -0.005(2) 0.000(2) C272 0.036(3) 0.035(3) 0.031(3) -0.011(2) 0.003(3) -0.009(2) N11 0.021(2) 0.019(2) 0.027(3) -0.0075(18) -0.0010(19) -0.0017(17) N27 0.025(2) 0.020(2) 0.029(3) -0.0039(18) 0.0037(19) -0.0064(18) C111 0.023(3) 0.022(3) 0.029(3) -0.010(2) -0.008(2) 0.000(2) N273 0.035(3) 0.033(3) 0.028(3) -0.005(2) -0.001(2) -0.013(2) O19 0.0203(19) 0.0181(17) 0.038(2) -0.0100(15) -0.0049(16) 0.0006(14) O30 0.036(2) 0.030(2) 0.032(2) -0.0088(16) 0.0018(17) -0.0024(16) O33 0.033(2) 0.0202(18) 0.040(2) -0.0111(16) -0.0026(18) -0.0016(15) Cu 0.0242(4) 0.0221(3) 0.0263(4) -0.0065(3) 0.0007(3) -0.0044(2) Cl 0.0271(7) 0.0221(6) 0.0332(8) -0.0059(5) 0.0019(6) -0.0055(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 C12 N11 1.505(6) . ? C12 C13 1.511(6) . ? C13 C18 1.395(6) . ? C13 C14 1.411(7) . ? C14 C15 1.417(7) . ? C15 C16 1.387(7) . ? C16 C17 1.405(7) . ? C17 C18 1.396(6) . ? C17 C21 1.461(7) . ? C18 O19 1.406(6) . ? C20 C25 1.383(7) . ? C20 C21 1.395(7) . ? C20 O19 1.413(6) . ? C21 C22 1.415(7) . ? C22 C23 1.373(7) . ? C23 C24 1.399(7) . ? C24 C25 1.405(7) . ? C25 C26 1.530(7) . ? C26 N27 1.512(6) . ? C28 C29 1.509(7) . ? C28 N27 1.512(6) . ? C29 O30 1.418(6) . ? C31 O30 1.435(6) . ? C31 C32 1.515(7) . ? C32 O33 1.437(6) . ? C34 O33 1.454(6) . ? C34 C35 1.510(6) . ? C35 N11 1.524(6) . ? C112 N113 1.494(6) . ? C112 C111 1.512(6) . ? N113 Cu 1.981(4) . ? C271 N27 1.503(6) . ? C271 C272 1.528(7) . ? C272 N273 1.484(6) . ? N11 C111 1.501(6) . ? N11 Cu 2.177(4) . ? N27 Cu 2.208(4) . ? N273 Cu 1.994(4) . ? O19 Cu 2.422(3) . ? N81 O82 1.2479(10) . ? N81 O84 1.2479(10) . ? N81 O83 1.2481(9) . ? N81 O84 1.552(11) 2_776 ? O82 O84 1.013(9) 2_776 ? O84 O82 1.013(9) 2_776 ? O84 N81 1.552(11) 2_776 ? O84 O84 1.814(14) 2_776 ? N91 O94 1.2497(10) 2_766 ? N91 O94 1.2497(10) . ? N91 O93 1.2517(10) 2_766 ? N91 O93 1.2517(10) . ? N91 O92 1.2523(10) . ? N91 O92 1.2523(10) 2_766 ? O92 O94 1.263(3) 2_766 ? O92 O93 1.270(3) 2_766 ? O93 O94 1.261(3) 2_766 ? O93 O92 1.270(3) 2_766 ? O94 O93 1.261(3) 2_766 ? O94 O92 1.263(3) 2_766 ? 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 C12 C13 118.1(4) . . ? C18 C13 C14 114.2(4) . . ? C18 C13 C12 125.0(4) . . ? C14 C13 C12 120.6(4) . . ? C13 C14 C15 122.0(5) . . ? C16 C15 C14 121.1(5) . . ? C15 C16 C17 118.6(4) . . ? C18 C17 C16 118.6(4) . . ? C18 C17 C21 105.7(4) . . ? C16 C17 C21 135.8(4) . . ? C13 C18 C17 125.5(5) . . ? C13 C18 O19 123.0(4) . . ? C17 C18 O19 111.4(4) . . ? C25 C20 C21 125.8(5) . . ? C25 C20 O19 123.8(4) . . ? C21 C20 O19 110.4(4) . . ? C20 C21 C22 118.1(5) . . ? C20 C21 C17 106.9(4) . . ? C22 C21 C17 134.9(5) . . ? C23 C22 C21 117.3(5) . . ? C22 C23 C24 123.0(5) . . ? C23 C24 C25 121.1(5) . . ? C20 C25 C24 114.5(5) . . ? C20 C25 C26 126.2(4) . . ? C24 C25 C26 119.1(5) . . ? N27 C26 C25 118.8(4) . . ? C29 C28 N27 115.4(4) . . ? O30 C29 C28 113.6(4) . . ? O30 C31 C32 107.1(4) . . ? O33 C32 C31 107.8(4) . . ? O33 C34 C35 108.6(4) . . ? C34 C35 N11 114.1(4) . . ? N113 C112 C111 107.8(4) . . ? C112 N113 Cu 109.5(3) . . ? N27 C271 C272 111.0(4) . . ? N273 C272 C271 107.4(4) . . ? C111 N11 C12 110.4(4) . . ? C111 N11 C35 110.6(3) . . ? C12 N11 C35 104.3(4) . . ? C111 N11 Cu 107.2(3) . . ? C12 N11 Cu 115.5(3) . . ? C35 N11 Cu 108.7(3) . . ? C271 N27 C26 108.5(3) . . ? C271 N27 C28 107.3(4) . . ? C26 N27 C28 106.3(4) . . ? C271 N27 Cu 103.1(3) . . ? C26 N27 Cu 118.3(3) . . ? C28 N27 Cu 112.7(3) . . ? N11 C111 C112 110.6(4) . . ? C272 N273 Cu 115.0(3) . . ? C18 O19 C20 105.5(3) . . ? C18 O19 Cu 125.5(3) . . ? C20 O19 Cu 127.3(3) . . ? C29 O30 C31 114.5(4) . . ? C32 O33 C34 111.4(3) . . ? N113 Cu N273 176.34(17) . . ? N113 Cu N11 82.66(16) . . ? N273 Cu N11 94.00(17) . . ? N113 Cu N27 100.88(16) . . ? N273 Cu N27 82.73(16) . . ? N11 Cu N27 165.03(13) . . ? N113 Cu O19 88.38(14) . . ? N273 Cu O19 92.84(15) . . ? N11 Cu O19 84.88(12) . . ? N27 Cu O19 80.72(13) . . ? O82 N81 O84 119.93(11) . . ? O82 N81 O83 119.97(11) . . ? O84 N81 O83 120.06(11) . . ? O82 N81 O84 40.6(4) . 2_776 ? O84 N81 O84 79.9(5) . 2_776 ? O83 N81 O84 159.4(5) . 2_776 ? O84 O82 N81 86.0(8) 2_776 . ? O82 O84 N81 151.9(9) 2_776 . ? O82 O84 N81 53.3(5) 2_776 2_776 ? N81 O84 N81 100.1(5) . 2_776 ? O82 O84 O84 95.5(8) 2_776 2_776 ? N81 O84 O84 57.4(3) . 2_776 ? N81 O84 O84 42.6(4) 2_776 2_776 ? O94 N91 O94 180.000(2) 2_766 . ? O94 N91 O93 119.45(13) 2_766 2_766 ? O94 N91 O93 60.55(13) . 2_766 ? O94 N91 O93 60.55(13) 2_766 . ? O94 N91 O93 119.45(13) . . ? O93 N91 O93 180.0 2_766 . ? O94 N91 O92 60.66(13) 2_766 . ? O94 N91 O92 119.34(13) . . ? O93 N91 O92 60.93(13) 2_766 . ? O93 N91 O92 119.07(13) . . ? O94 N91 O92 119.34(13) 2_766 2_766 ? O94 N91 O92 60.66(13) . 2_766 ? O93 N91 O92 119.07(13) 2_766 2_766 ? O93 N91 O92 60.93(13) . 2_766 ? O92 N91 O92 180.000(3) . 2_766 ? N91 O92 O94 59.57(9) . 2_766 ? N91 O92 O93 59.51(9) . 2_766 ? O94 O92 O93 117.0(3) 2_766 2_766 ? N91 O93 O94 59.65(9) . 2_766 ? N91 O93 O92 59.55(9) . 2_766 ? O94 O93 O92 117.2(3) 2_766 2_766 ? N91 O94 O93 59.81(9) . 2_766 ? N91 O94 O92 59.77(9) . 2_766 ? O93 O94 O92 117.5(3) 2_766 2_766 ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 30.19 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 1.716 _refine_diff_density_min -0.828 _refine_diff_density_rms 0.114