# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Polly Louise Arnold' _publ_contact_author_address ; Department of Chemistry University of Nottingham University Park Nottingham NOTTS NG7 2RD UNITED KINGDOM ; _publ_contact_author_email POLLY.ARNOLD@NOTTINGHAM.AC.UK _publ_section_title ; Bent metal carbene geometries in amido N-heterocyclic carbene complexes ; loop_ _publ_author_name 'Polly Louise Arnold' 'Stephen T. Liddle' 'Shaheed A. Mungur' 'Mark J. Sarsfield' 'Claire Wilson' data_litpcb _database_code_depnum_ccdc_archive 'CCDC 244355' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H48 Li2 N6' _chemical_formula_sum 'C26 H48 Li2 N6' _chemical_formula_weight 458.58 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' Li Li -0.0003 0.0001 '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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6274(13) _cell_length_b 19.835(3) _cell_length_c 28.003(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5902.9(13) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5125 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 26.7 _exptl_crystal_description colourless _exptl_crystal_colour block _exptl_crystal_size_max .36 _exptl_crystal_size_mid .29 _exptl_crystal_size_min .27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.032 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.061 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 41265 _diffrn_reflns_av_R_equivalents 0.1060 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 24.71 _reflns_number_total 5024 _reflns_number_gt 2946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.625' _computing_cell_refinement 'Bruker SAINT v6.36a' _computing_data_reduction 'Bruker SAINT v6.36a; Bruker SHELXTL v6.12' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL v6.12' _computing_publication_material 'enCIFer(Allen et al.,2004); PLATON(Spek,2003)' _refine_special_details ; Disorder in one tBu group modelled as two half occcupied sites with isotropic adps and suitable geometry restraints. ; _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^)+(0.0789P)^2^] 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 5024 _refine_ls_number_parameters 304 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1378 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.004 _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 Li1 Li 0.5174(4) -0.03746(18) 0.13867(13) 0.0317(9) Uani 1 1 d . . . Li2 Li 0.5304(4) 0.07526(18) 0.10690(14) 0.0337(9) Uani 1 1 d . . . N1 N 0.39212(16) 0.00647(9) 0.09370(6) 0.0278(4) Uani 1 1 d . . . N2 N 0.45141(17) -0.14332(8) 0.07822(7) 0.0286(4) Uani 1 1 d . . . N3 N 0.41733(16) -0.19727(8) 0.14280(7) 0.0304(5) Uani 1 1 d . . . N21 N 0.66373(16) 0.02563(8) 0.14441(6) 0.0289(4) Uani 1 1 d . . . N22 N 0.75391(18) 0.12022(9) 0.06584(6) 0.0314(5) Uani 1 1 d . . . N23 N 0.68328(17) 0.21951(9) 0.07680(7) 0.0335(5) Uani 1 1 d . A . C1 C 0.4746(2) -0.14049(10) 0.12589(8) 0.0289(5) Uani 1 1 d . . . C2 C 0.3802(2) -0.19875(11) 0.06571(9) 0.0368(6) Uani 1 1 d . . . H2A H 0.3512 -0.2101 0.0347 0.044 Uiso 1 1 calc R . . C3 C 0.3603(2) -0.23318(11) 0.10599(9) 0.0381(6) Uani 1 1 d . . . H3A H 0.3156 -0.2744 0.1090 0.046 Uiso 1 1 calc R . . C10 C 0.2669(2) 0.03087(12) 0.10716(9) 0.0367(6) Uani 1 1 d . . . C11 C 0.4838(2) -0.08772(11) 0.04610(8) 0.0324(6) Uani 1 1 d . . . H11A H 0.4874 -0.1047 0.0129 0.039 Uiso 1 1 calc R . . H11B H 0.5682 -0.0703 0.0545 0.039 Uiso 1 1 calc R . . C12 C 0.3886(2) -0.03060(11) 0.04899(8) 0.0326(5) Uani 1 1 d . . . H12A H 0.4044 0.0012 0.0224 0.039 Uiso 1 1 calc R . . H12B H 0.3031 -0.0495 0.0446 0.039 Uiso 1 1 calc R . . C17 C 0.1783(3) -0.02683(15) 0.12204(11) 0.0627(8) Uani 1 1 d . . . H17A H 0.2180 -0.0535 0.1474 0.094 Uiso 1 1 calc R . . H17B H 0.1615 -0.0558 0.0944 0.094 Uiso 1 1 calc R . . H17C H 0.0989 -0.0079 0.1338 0.094 Uiso 1 1 calc R . . C18 C 0.2039(3) 0.07266(15) 0.06736(10) 0.0603(9) Uani 1 1 d . . . H18A H 0.2598 0.1096 0.0580 0.090 Uiso 1 1 calc R . . H18B H 0.1242 0.0912 0.0791 0.090 Uiso 1 1 calc R . . H18C H 0.1876 0.0437 0.0397 0.090 Uiso 1 1 calc R . . C19 C 0.2833(2) 0.07706(13) 0.15009(9) 0.0469(7) Uani 1 1 d . . . H19A H 0.3234 0.0520 0.1762 0.070 Uiso 1 1 calc R . . H19B H 0.2007 0.0934 0.1606 0.070 Uiso 1 1 calc R . . H19C H 0.3363 0.1155 0.1412 0.070 Uiso 1 1 calc R . . C20 C 0.4136(2) -0.21858(11) 0.19373(9) 0.0351(6) Uani 1 1 d . . . C21 C 0.6454(2) 0.15364(11) 0.07566(8) 0.0307(5) Uani 1 1 d . . . C22 C 0.8558(2) 0.16284(13) 0.06214(9) 0.0437(7) Uani 1 1 d . . . H22A H 0.9405 0.1503 0.0561 0.052 Uiso 1 1 calc R . . C23 C 0.8119(2) 0.22564(13) 0.06882(10) 0.0457(7) Uani 1 1 d . . . H23A H 0.8593 0.2662 0.0682 0.055 Uiso 1 1 calc R . . C27 C 0.2769(2) -0.22878(14) 0.20846(10) 0.0546(8) Uani 1 1 d . . . H27A H 0.2311 -0.1861 0.2052 0.082 Uiso 1 1 calc R . . H27B H 0.2735 -0.2438 0.2418 0.082 Uiso 1 1 calc R . . H27C H 0.2382 -0.2629 0.1879 0.082 Uiso 1 1 calc R . . C28 C 0.4887(3) -0.28376(12) 0.19845(10) 0.0519(7) Uani 1 1 d . . . H28A H 0.5759 -0.2758 0.1886 0.078 Uiso 1 1 calc R . . H28B H 0.4513 -0.3185 0.1780 0.078 Uiso 1 1 calc R . . H28C H 0.4871 -0.2989 0.2318 0.078 Uiso 1 1 calc R . . C29 C 0.4732(3) -0.16406(12) 0.22459(9) 0.0455(7) Uani 1 1 d . . . H29A H 0.4251 -0.1222 0.2214 0.068 Uiso 1 1 calc R . . H29B H 0.5601 -0.1564 0.2142 0.068 Uiso 1 1 calc R . . H29C H 0.4727 -0.1785 0.2581 0.068 Uiso 1 1 calc R . . C30 C 0.6950(2) 0.03485(10) 0.19507(8) 0.0297(5) Uani 1 1 d . . . C31 C 0.7627(2) 0.04649(11) 0.06571(8) 0.0352(6) Uani 1 1 d . . . H31A H 0.8362 0.0328 0.0463 0.042 Uiso 1 1 calc R . . H31B H 0.6864 0.0277 0.0504 0.042 Uiso 1 1 calc R . . C32 C 0.7758(2) 0.01659(11) 0.11533(8) 0.0353(6) Uani 1 1 d . . . H32A H 0.7939 -0.0322 0.1125 0.042 Uiso 1 1 calc R . . H32B H 0.8482 0.0380 0.1316 0.042 Uiso 1 1 calc R . . C37 C 0.7662(2) 0.10124(11) 0.20455(9) 0.0441(7) Uani 1 1 d . . . H37A H 0.7175 0.1391 0.1918 0.066 Uiso 1 1 calc R . . H37B H 0.8486 0.0996 0.1889 0.066 Uiso 1 1 calc R . . H37C H 0.7777 0.1072 0.2390 0.066 Uiso 1 1 calc R . . C38 C 0.7723(2) -0.02406(11) 0.21528(9) 0.0401(6) Uani 1 1 d . . . H38A H 0.7277 -0.0665 0.2094 0.060 Uiso 1 1 calc R . . H38B H 0.7839 -0.0178 0.2497 0.060 Uiso 1 1 calc R . . H38C H 0.8547 -0.0254 0.1996 0.060 Uiso 1 1 calc R . . C39 C 0.5719(2) 0.03830(13) 0.22279(9) 0.0444(7) Uani 1 1 d . . . H39A H 0.5205 0.0755 0.2105 0.067 Uiso 1 1 calc R . . H39B H 0.5899 0.0459 0.2567 0.067 Uiso 1 1 calc R . . H39C H 0.5261 -0.0043 0.2190 0.067 Uiso 1 1 calc R . . C40 C 0.6020(2) 0.27855(11) 0.08813(9) 0.0414(6) Uani 1 1 d D . . C47 C 0.4645(5) 0.2573(3) 0.0763(2) 0.0521(16) Uiso 0.50 1 d PD A 1 H47A H 0.4611 0.2389 0.0438 0.078 Uiso 0.50 1 calc PR A 1 H47B H 0.4092 0.2967 0.0785 0.078 Uiso 0.50 1 calc PR A 1 H47C H 0.4366 0.2229 0.0990 0.078 Uiso 0.50 1 calc PR A 1 C48 C 0.6178(8) 0.3008(4) 0.1382(2) 0.085(3) Uiso 0.50 1 d PD A 1 H48A H 0.5439 0.2873 0.1568 0.128 Uiso 0.50 1 calc PR A 1 H48B H 0.6266 0.3499 0.1391 0.128 Uiso 0.50 1 calc PR A 1 H48C H 0.6933 0.2798 0.1517 0.128 Uiso 0.50 1 calc PR A 1 C49 C 0.6343(8) 0.3339(3) 0.0518(2) 0.045(2) Uiso 0.50 1 d PD A 1 H49A H 0.6028 0.3209 0.0202 0.067 Uiso 0.50 1 calc PR A 1 H49B H 0.7258 0.3397 0.0504 0.067 Uiso 0.50 1 calc PR A 1 H49C H 0.5950 0.3764 0.0617 0.067 Uiso 0.50 1 calc PR A 1 C47' C 0.4699(4) 0.2570(3) 0.1011(2) 0.0444(14) Uiso 0.50 1 d PD A 2 H47D H 0.4294 0.2366 0.0732 0.067 Uiso 0.50 1 calc PR A 2 H47E H 0.4215 0.2965 0.1114 0.067 Uiso 0.50 1 calc PR A 2 H47F H 0.4733 0.2241 0.1272 0.067 Uiso 0.50 1 calc PR A 2 C48' C 0.6603(6) 0.3112(3) 0.13475(16) 0.0347(14) Uiso 0.50 1 d PD A 2 H48D H 0.7506 0.3187 0.1300 0.052 Uiso 0.50 1 calc PR A 2 H48E H 0.6476 0.2808 0.1619 0.052 Uiso 0.50 1 calc PR A 2 H48F H 0.6188 0.3544 0.1412 0.052 Uiso 0.50 1 calc PR A 2 C49' C 0.6029(7) 0.3303(4) 0.0488(2) 0.054(3) Uiso 0.50 1 d PD A 2 H49D H 0.5661 0.3108 0.0199 0.081 Uiso 0.50 1 calc PR A 2 H49E H 0.6898 0.3442 0.0423 0.081 Uiso 0.50 1 calc PR A 2 H49F H 0.5536 0.3697 0.0587 0.081 Uiso 0.50 1 calc PR A 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 Li1 0.034(2) 0.028(2) 0.033(2) -0.0006(17) -0.0043(17) 0.0003(17) Li2 0.030(2) 0.031(2) 0.040(2) 0.0018(18) 0.0006(18) -0.0005(17) N1 0.0253(10) 0.0271(10) 0.0309(11) 0.0003(8) -0.0021(8) 0.0022(8) N2 0.0279(10) 0.0230(10) 0.0349(12) -0.0022(8) -0.0005(8) 0.0001(8) N3 0.0262(10) 0.0225(10) 0.0423(12) -0.0013(9) -0.0023(9) 0.0002(8) N21 0.0276(10) 0.0271(10) 0.0320(11) -0.0004(8) -0.0020(9) 0.0013(8) N22 0.0294(11) 0.0301(10) 0.0348(11) 0.0010(9) 0.0009(9) -0.0004(9) N23 0.0257(11) 0.0276(10) 0.0472(13) 0.0030(9) 0.0013(9) -0.0031(9) C1 0.0248(12) 0.0236(12) 0.0382(14) 0.0017(10) 0.0004(10) 0.0017(10) C2 0.0333(14) 0.0327(13) 0.0445(16) -0.0093(12) -0.0044(12) 0.0009(11) C3 0.0332(14) 0.0264(12) 0.0549(17) -0.0064(12) -0.0015(12) -0.0051(10) C10 0.0282(13) 0.0374(13) 0.0445(15) -0.0014(12) 0.0005(11) 0.0064(11) C11 0.0341(14) 0.0330(13) 0.0300(13) -0.0001(11) 0.0020(11) -0.0012(11) C12 0.0314(13) 0.0320(13) 0.0345(13) 0.0027(11) -0.0030(11) -0.0005(11) C17 0.0359(16) 0.073(2) 0.079(2) -0.0066(17) 0.0153(15) -0.0072(15) C18 0.0534(18) 0.069(2) 0.0589(19) -0.0057(16) -0.0167(15) 0.0314(15) C19 0.0428(16) 0.0507(16) 0.0471(16) -0.0065(14) 0.0038(13) 0.0170(13) C20 0.0326(14) 0.0292(12) 0.0435(15) 0.0083(11) -0.0006(11) -0.0005(11) C21 0.0307(13) 0.0292(12) 0.0323(14) 0.0031(10) -0.0026(10) -0.0004(11) C22 0.0267(14) 0.0427(15) 0.0616(19) 0.0058(13) 0.0064(12) -0.0023(12) C23 0.0301(14) 0.0395(15) 0.0674(19) 0.0059(13) 0.0052(13) -0.0091(12) C27 0.0421(17) 0.0643(19) 0.0575(19) 0.0120(15) 0.0074(13) -0.0005(14) C28 0.0543(18) 0.0334(14) 0.068(2) 0.0096(13) -0.0083(15) 0.0033(13) C29 0.0582(18) 0.0371(14) 0.0413(16) 0.0046(12) -0.0013(13) -0.0046(13) C30 0.0298(13) 0.0255(12) 0.0339(14) -0.0006(10) -0.0052(11) -0.0063(10) C31 0.0372(14) 0.0308(13) 0.0376(14) -0.0035(11) 0.0013(11) 0.0031(11) C32 0.0339(14) 0.0312(13) 0.0409(15) -0.0018(11) -0.0011(11) 0.0039(11) C37 0.0495(17) 0.0324(13) 0.0504(17) -0.0054(12) -0.0085(13) -0.0085(12) C38 0.0443(15) 0.0369(14) 0.0389(15) 0.0022(11) -0.0106(12) -0.0012(12) C39 0.0432(16) 0.0529(16) 0.0371(15) -0.0045(13) 0.0004(12) -0.0045(13) C40 0.0399(15) 0.0296(13) 0.0548(17) 0.0026(12) 0.0055(13) 0.0005(11) _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 Li1 N21 2.002(4) . ? Li1 N1 2.029(4) . ? Li1 C1 2.124(4) . ? Li1 Li2 2.410(5) . ? Li2 N21 2.020(4) . ? Li2 N1 2.039(4) . ? Li2 C21 2.162(4) . ? Li2 C31 2.784(5) . ? N1 C12 1.452(3) . ? N1 C10 1.465(3) . ? N2 C1 1.359(3) . ? N2 C2 1.380(3) . ? N2 C11 1.464(3) . ? N3 C1 1.365(3) . ? N3 C3 1.392(3) . ? N3 C20 1.488(3) . ? N21 C32 1.454(3) . ? N21 C30 1.469(3) . ? N22 C21 1.358(3) . ? N22 C22 1.377(3) . ? N22 C31 1.465(3) . ? N23 C21 1.367(3) . ? N23 C23 1.390(3) . ? N23 C40 1.489(3) . ? C2 C3 1.336(3) . ? C10 C19 1.522(3) . ? C10 C17 1.540(3) . ? C10 C18 1.542(3) . ? C11 C12 1.521(3) . ? C20 C29 1.522(3) . ? C20 C27 1.524(3) . ? C20 C28 1.525(3) . ? C22 C23 1.343(3) . ? C30 C39 1.522(3) . ? C30 C38 1.536(3) . ? C30 C37 1.541(3) . ? C31 C32 1.517(3) . ? C40 C48 1.479(6) . ? C40 C49' 1.505(5) . ? C40 C47' 1.511(5) . ? C40 C49 1.535(5) . ? C40 C47 1.557(5) . ? C40 C48' 1.584(5) . ? 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 N21 Li1 N1 106.92(18) . . ? N21 Li1 C1 141.4(2) . . ? N1 Li1 C1 99.67(17) . . ? N21 Li1 Li2 53.52(14) . . ? N1 Li1 Li2 53.86(13) . . ? C1 Li1 Li2 147.4(2) . . ? N21 Li2 N1 105.88(17) . . ? N21 Li2 C21 99.46(18) . . ? N1 Li2 C21 144.6(2) . . ? N21 Li2 Li1 52.85(13) . . ? N1 Li2 Li1 53.48(13) . . ? C21 Li2 Li1 148.1(2) . . ? N21 Li2 C31 59.57(12) . . ? N1 Li2 C31 115.26(17) . . ? C21 Li2 C31 58.57(12) . . ? Li1 Li2 C31 90.77(15) . . ? C12 N1 C10 111.45(17) . . ? C12 N1 Li1 109.54(16) . . ? C10 N1 Li1 125.31(18) . . ? C12 N1 Li2 120.90(17) . . ? C10 N1 Li2 112.76(17) . . ? Li1 N1 Li2 72.66(16) . . ? C1 N2 C2 112.46(18) . . ? C1 N2 C11 122.00(17) . . ? C2 N2 C11 125.0(2) . . ? C1 N3 C3 111.1(2) . . ? C1 N3 C20 125.35(19) . . ? C3 N3 C20 123.56(19) . . ? C32 N21 C30 111.78(17) . . ? C32 N21 Li1 120.94(17) . . ? C30 N21 Li1 109.34(16) . . ? C32 N21 Li2 110.09(18) . . ? C30 N21 Li2 126.90(17) . . ? Li1 N21 Li2 73.63(16) . . ? C21 N22 C22 112.51(18) . . ? C21 N22 C31 122.79(19) . . ? C22 N22 C31 124.2(2) . . ? C21 N23 C23 111.7(2) . . ? C21 N23 C40 125.84(18) . . ? C23 N23 C40 122.39(19) . . ? N2 C1 N3 103.04(18) . . ? N2 C1 Li1 104.13(17) . . ? N3 C1 Li1 146.2(2) . . ? C3 C2 N2 106.3(2) . . ? C2 C3 N3 107.1(2) . . ? N1 C10 C19 107.36(19) . . ? N1 C10 C17 112.31(19) . . ? C19 C10 C17 107.7(2) . . ? N1 C10 C18 112.7(2) . . ? C19 C10 C18 107.3(2) . . ? C17 C10 C18 109.2(2) . . ? N2 C11 C12 111.85(18) . . ? N1 C12 C11 113.95(18) . . ? N3 C20 C29 109.34(18) . . ? N3 C20 C27 108.81(19) . . ? C29 C20 C27 109.7(2) . . ? N3 C20 C28 108.0(2) . . ? C29 C20 C28 109.6(2) . . ? C27 C20 C28 111.3(2) . . ? N22 C21 N23 102.78(18) . . ? N22 C21 Li2 102.18(17) . . ? N23 C21 Li2 147.5(2) . . ? C23 C22 N22 106.6(2) . . ? C22 C23 N23 106.4(2) . . ? N21 C30 C39 107.67(18) . . ? N21 C30 C38 112.46(18) . . ? C39 C30 C38 107.81(19) . . ? N21 C30 C37 112.57(18) . . ? C39 C30 C37 107.17(19) . . ? C38 C30 C37 108.90(19) . . ? N22 C31 C32 113.19(19) . . ? N22 C31 Li2 74.81(14) . . ? C32 C31 Li2 77.42(15) . . ? N21 C32 C31 112.92(18) . . ? C48 C40 N23 111.8(4) . . ? C48 C40 C49' 119.3(5) . . ? N23 C40 C49' 112.1(4) . . ? C48 C40 C47' 87.8(4) . . ? N23 C40 C47' 111.6(3) . . ? C49' C40 C47' 112.0(4) . . ? C48 C40 C49 112.9(4) . . ? N23 C40 C49 106.9(3) . . ? C49' C40 C49 13.2(5) . . ? C47' C40 C49 124.7(4) . . ? C48 C40 C47 112.9(4) . . ? N23 C40 C47 106.6(3) . . ? C49' C40 C47 92.0(4) . . ? C47' C40 C47 26.3(3) . . ? C49 C40 C47 105.2(4) . . ? C48 C40 C48' 18.6(4) . . ? N23 C40 C48' 105.7(3) . . ? C49' C40 C48' 108.7(4) . . ? C47' C40 C48' 106.3(3) . . ? C49 C40 C48' 99.5(4) . . ? C47 C40 C48' 130.8(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.303 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.040 #======end data_MGCBTB _database_code_depnum_ccdc_archive 'CCDC 244356' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H48 Mg N6' _chemical_formula_sum 'C26 H48 Mg N6' _chemical_formula_weight 469.01 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' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.4773(8) _cell_length_b 17.5050(13) _cell_length_c 28.222(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.341(2) _cell_angle_gamma 90.00 _cell_volume 5645.4(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6054 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.26 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.104 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.960 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24105 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.033 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6476 _reflns_number_gt 4722 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0652P)^2^+2.7138P] 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 6476 _refine_ls_number_parameters 325 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.040 _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 Mg1 Mg 0.71956(4) 0.06977(3) 0.621936(17) 0.02059(13) Uani 1 1 d . . . C1 C 0.78040(13) 0.11969(8) 0.55449(5) 0.0227(3) Uani 1 1 d . A . N1 N 0.88119(11) 0.14109(7) 0.53624(5) 0.0250(3) Uani 1 1 d . . . N2 N 0.69830(11) 0.12743(7) 0.51699(4) 0.0242(3) Uani 1 1 d . . . C2 C 0.74617(15) 0.15203(10) 0.47677(6) 0.0326(4) Uani 1 1 d . A . H2A H 0.7056 0.1611 0.4464 0.039 Uiso 1 1 calc R . . C3 C 0.86112(15) 0.16071(10) 0.48871(6) 0.0335(4) Uani 1 1 d . A . H3A H 0.9178 0.1771 0.4685 0.040 Uiso 1 1 calc R . . C4 C 1.00015(14) 0.13701(10) 0.56278(7) 0.0328(4) Uani 0.80 1 d P A 1 C5 C 1.0275(2) 0.05509(15) 0.57654(11) 0.0501(7) Uani 0.80 1 d P A 1 H5A H 0.9638 0.0342 0.5934 0.075 Uiso 0.80 1 calc PR A 1 H5B H 1.1007 0.0531 0.5973 0.075 Uiso 0.80 1 calc PR A 1 H5C H 1.0357 0.0249 0.5478 0.075 Uiso 0.80 1 calc PR A 1 C6 C 1.0913(2) 0.17322(19) 0.53583(9) 0.0413(6) Uani 0.80 1 d P A 1 H6A H 1.0983 0.1447 0.5064 0.062 Uiso 0.80 1 calc PR A 1 H6B H 1.1665 0.1727 0.5553 0.062 Uiso 0.80 1 calc PR A 1 H6C H 1.0688 0.2261 0.5281 0.062 Uiso 0.80 1 calc PR A 1 C7 C 0.99594(19) 0.18341(15) 0.61041(8) 0.0384(5) Uani 0.80 1 d P A 1 H7A H 0.9768 0.2369 0.6029 0.058 Uiso 0.80 1 calc PR A 1 H7B H 1.0724 0.1807 0.6290 0.058 Uiso 0.80 1 calc PR A 1 H7C H 0.9360 0.1616 0.6290 0.058 Uiso 0.80 1 calc PR A 1 C4A C 1.00015(14) 0.13701(10) 0.56278(7) 0.0328(4) Uani 0.20 1 d PD A 2 C5A C 1.0539(8) 0.0683(4) 0.5361(3) 0.042(2) Uiso 0.20 1 d PD A 2 H5A1 H 1.0066 0.0223 0.5396 0.063 Uiso 0.20 1 calc PR A 2 H5A2 H 1.1342 0.0590 0.5498 0.063 Uiso 0.20 1 calc PR A 2 H5A3 H 1.0541 0.0807 0.5022 0.063 Uiso 0.20 1 calc PR A 2 C6A C 1.0627(11) 0.2063(7) 0.5456(4) 0.045(3) Uiso 0.20 1 d P A 2 H6A1 H 1.0542 0.2074 0.5107 0.068 Uiso 0.20 1 calc PR A 2 H6A2 H 1.1459 0.2036 0.5569 0.068 Uiso 0.20 1 calc PR A 2 H6A3 H 1.0285 0.2527 0.5579 0.068 Uiso 0.20 1 calc PR A 2 C7A C 1.0000(9) 0.1183(6) 0.61418(19) 0.045(2) Uiso 0.20 1 d PD A 2 H7A1 H 0.9537 0.1564 0.6296 0.068 Uiso 0.20 1 calc PR A 2 H7A2 H 1.0805 0.1186 0.6292 0.068 Uiso 0.20 1 calc PR A 2 H7A3 H 0.9657 0.0676 0.6176 0.068 Uiso 0.20 1 calc PR A 2 C8 C 0.57416(14) 0.10558(10) 0.51617(6) 0.0292(4) Uani 1 1 d . A . H8A H 0.5685 0.0493 0.5133 0.035 Uiso 1 1 calc R . . H8B H 0.5314 0.1279 0.4874 0.035 Uiso 1 1 calc R . . C9 C 0.51350(14) 0.13007(10) 0.55912(6) 0.0300(4) Uani 1 1 d . . . H9A H 0.5289 0.1851 0.5649 0.036 Uiso 1 1 calc R A . H9B H 0.4280 0.1237 0.5517 0.036 Uiso 1 1 calc R . . N3 N 0.54939(11) 0.08835(7) 0.60229(5) 0.0249(3) Uani 1 1 d . A . C10 C 0.45180(13) 0.06901(10) 0.63017(6) 0.0286(3) Uani 1 1 d . . . C11 C 0.37766(16) 0.13917(11) 0.64078(8) 0.0421(5) Uani 1 1 d . A . H11A H 0.4278 0.1778 0.6575 0.063 Uiso 1 1 calc R . . H11B H 0.3163 0.1238 0.6608 0.063 Uiso 1 1 calc R . . H11C H 0.3417 0.1606 0.6108 0.063 Uiso 1 1 calc R . . C12 C 0.37141(16) 0.00790(11) 0.60502(7) 0.0413(4) Uani 1 1 d . A . H12A H 0.4155 -0.0396 0.6022 0.062 Uiso 1 1 calc R . . H12B H 0.3427 0.0260 0.5732 0.062 Uiso 1 1 calc R . . H12C H 0.3049 -0.0016 0.6236 0.062 Uiso 1 1 calc R . . C13 C 0.50289(16) 0.03588(11) 0.67756(6) 0.0382(4) Uani 1 1 d . A . H13A H 0.5520 -0.0083 0.6717 0.057 Uiso 1 1 calc R . . H13B H 0.4392 0.0198 0.6961 0.057 Uiso 1 1 calc R . . H13C H 0.5503 0.0748 0.6953 0.057 Uiso 1 1 calc R . . C14 C 0.78442(13) 0.12599(8) 0.69194(5) 0.0227(3) Uani 1 1 d . . . N4 N 0.79070(11) 0.19672(7) 0.71246(5) 0.0249(3) Uani 1 1 d . . . N5 N 0.82962(11) 0.07950(7) 0.72768(4) 0.0236(3) Uani 1 1 d . . . C15 C 0.86213(15) 0.11948(10) 0.76879(6) 0.0314(4) Uani 1 1 d . . . H15A H 0.8952 0.0989 0.7982 0.038 Uiso 1 1 calc R . . C16 C 0.83801(15) 0.19298(10) 0.75924(6) 0.0328(4) Uani 1 1 d . . . H16A H 0.8510 0.2347 0.7806 0.039 Uiso 1 1 calc R . . C17 C 0.74356(16) 0.26940(9) 0.69095(6) 0.0316(4) Uani 1 1 d . . . C18 C 0.63956(19) 0.29321(12) 0.71786(7) 0.0466(5) Uani 1 1 d . . . H18A H 0.5788 0.2538 0.7140 0.070 Uiso 1 1 calc R . . H18B H 0.6078 0.3417 0.7050 0.070 Uiso 1 1 calc R . . H18C H 0.6655 0.2994 0.7517 0.070 Uiso 1 1 calc R . . C19 C 0.70202(17) 0.25794(10) 0.63893(6) 0.0346(4) Uani 1 1 d . . . H19A H 0.7677 0.2408 0.6217 0.052 Uiso 1 1 calc R . . H19B H 0.6715 0.3063 0.6254 0.052 Uiso 1 1 calc R . . H19C H 0.6400 0.2193 0.6360 0.052 Uiso 1 1 calc R . . C20 C 0.8404(2) 0.32949(12) 0.69661(9) 0.0558(6) Uani 1 1 d . . . H20A H 0.9080 0.3118 0.6808 0.084 Uiso 1 1 calc R . . H20B H 0.8640 0.3376 0.7305 0.084 Uiso 1 1 calc R . . H20C H 0.8115 0.3776 0.6822 0.084 Uiso 1 1 calc R . . C21 C 0.83248(15) -0.00462(9) 0.72579(6) 0.0275(3) Uani 1 1 d . . . H21A H 0.7522 -0.0241 0.7281 0.033 Uiso 1 1 calc R . . H21B H 0.8821 -0.0235 0.7539 0.033 Uiso 1 1 calc R . . C22 C 0.87789(14) -0.03784(9) 0.68156(6) 0.0269(3) Uani 1 1 d . . . H22A H 0.9528 -0.0125 0.6765 0.032 Uiso 1 1 calc R . . H22B H 0.8945 -0.0928 0.6872 0.032 Uiso 1 1 calc R . . N6 N 0.79964(11) -0.03030(7) 0.63860(5) 0.0238(3) Uani 1 1 d . . . C23 C 0.78273(14) -0.10160(9) 0.61185(6) 0.0267(3) Uani 1 1 d . . . C24 C 0.71248(18) -0.16017(10) 0.63824(7) 0.0423(5) Uani 1 1 d . . . H24A H 0.6348 -0.1394 0.6424 0.063 Uiso 1 1 calc R . . H24B H 0.7537 -0.1710 0.6695 0.063 Uiso 1 1 calc R . . H24C H 0.7041 -0.2075 0.6197 0.063 Uiso 1 1 calc R . . C25 C 0.71339(16) -0.08308(10) 0.56439(6) 0.0362(4) Uani 1 1 d . . . H25A H 0.6384 -0.0599 0.5703 0.054 Uiso 1 1 calc R . . H25B H 0.6993 -0.1302 0.5460 0.054 Uiso 1 1 calc R . . H25C H 0.7581 -0.0473 0.5465 0.054 Uiso 1 1 calc R . . C26 C 0.89846(16) -0.13961(10) 0.60089(7) 0.0358(4) Uani 1 1 d . . . H26A H 0.9452 -0.1031 0.5844 0.054 Uiso 1 1 calc R . . H26B H 0.8814 -0.1844 0.5806 0.054 Uiso 1 1 calc R . . H26C H 0.9423 -0.1555 0.6307 0.054 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 Mg1 0.0193(2) 0.0196(2) 0.0226(3) 0.00137(19) 0.00008(19) 0.00114(19) C1 0.0222(7) 0.0204(7) 0.0255(8) -0.0019(6) 0.0016(6) -0.0012(6) N1 0.0221(6) 0.0262(7) 0.0270(7) 0.0020(5) 0.0029(5) -0.0023(5) N2 0.0232(6) 0.0257(7) 0.0232(7) 0.0016(5) -0.0001(5) -0.0019(5) C2 0.0345(9) 0.0392(10) 0.0241(8) 0.0061(7) 0.0023(7) -0.0022(7) C3 0.0334(9) 0.0387(10) 0.0294(9) 0.0066(7) 0.0082(7) -0.0025(7) C4 0.0190(8) 0.0337(9) 0.0453(10) 0.0074(8) 0.0006(7) -0.0032(7) C5 0.0268(12) 0.0419(14) 0.080(2) 0.0115(13) -0.0030(12) 0.0043(10) C6 0.0243(12) 0.0660(19) 0.0340(13) 0.0012(12) 0.0047(10) -0.0129(12) C7 0.0260(11) 0.0574(15) 0.0312(12) 0.0014(10) -0.0004(9) -0.0099(10) C4A 0.0190(8) 0.0337(9) 0.0453(10) 0.0074(8) 0.0006(7) -0.0032(7) C8 0.0219(8) 0.0357(9) 0.0290(8) 0.0037(7) -0.0035(6) -0.0050(7) C9 0.0200(8) 0.0351(9) 0.0344(9) 0.0077(7) -0.0006(6) 0.0039(6) N3 0.0190(6) 0.0288(7) 0.0271(7) 0.0060(5) 0.0023(5) 0.0030(5) C10 0.0208(7) 0.0313(9) 0.0341(9) 0.0023(7) 0.0045(6) 0.0007(6) C11 0.0321(10) 0.0434(11) 0.0528(12) 0.0009(9) 0.0144(8) 0.0096(8) C12 0.0304(9) 0.0417(11) 0.0518(12) 0.0045(9) 0.0032(8) -0.0068(8) C13 0.0302(9) 0.0488(11) 0.0366(10) 0.0109(8) 0.0091(7) -0.0010(8) C14 0.0224(7) 0.0212(7) 0.0248(8) 0.0007(6) 0.0031(6) -0.0001(6) N4 0.0273(7) 0.0221(7) 0.0252(7) -0.0018(5) 0.0024(5) 0.0017(5) N5 0.0251(7) 0.0243(7) 0.0212(6) 0.0005(5) 0.0014(5) 0.0021(5) C15 0.0353(9) 0.0361(9) 0.0219(8) -0.0041(7) -0.0018(7) 0.0074(7) C16 0.0376(9) 0.0324(9) 0.0276(9) -0.0093(7) -0.0011(7) 0.0064(7) C17 0.0402(9) 0.0206(8) 0.0332(9) -0.0015(6) -0.0003(7) 0.0036(7) C18 0.0550(12) 0.0444(11) 0.0393(11) -0.0102(9) -0.0018(9) 0.0227(10) C19 0.0470(10) 0.0243(8) 0.0322(9) 0.0039(7) 0.0017(8) 0.0077(7) C20 0.0690(15) 0.0307(11) 0.0646(14) 0.0013(10) -0.0095(12) -0.0140(10) C21 0.0318(8) 0.0243(8) 0.0257(8) 0.0057(6) -0.0011(6) 0.0007(6) C22 0.0275(8) 0.0203(8) 0.0316(9) 0.0005(6) -0.0038(6) 0.0034(6) N6 0.0248(7) 0.0183(6) 0.0271(7) -0.0010(5) -0.0035(5) 0.0018(5) C23 0.0282(8) 0.0206(8) 0.0306(8) -0.0023(6) -0.0011(7) 0.0021(6) C24 0.0454(11) 0.0278(9) 0.0534(12) -0.0018(8) 0.0032(9) -0.0098(8) C25 0.0392(10) 0.0311(9) 0.0360(10) -0.0097(7) -0.0092(8) 0.0067(8) C26 0.0370(10) 0.0307(9) 0.0388(10) -0.0053(7) -0.0005(8) 0.0101(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 Mg1 N3 2.0065(13) . ? Mg1 N6 2.0136(13) . ? Mg1 C1 2.2632(16) . ? Mg1 C14 2.2697(16) . ? C1 N2 1.3566(19) . ? C1 N1 1.362(2) . ? N1 C3 1.383(2) . ? N1 C4 1.497(2) . ? N2 C2 1.375(2) . ? N2 C8 1.473(2) . ? C2 C3 1.340(2) . ? C4 C6 1.491(3) . ? C4 C5 1.511(3) . ? C4 C7 1.575(3) . ? C8 C9 1.515(2) . ? C9 N3 1.447(2) . ? N3 C10 1.467(2) . ? C10 C13 1.524(2) . ? C10 C11 1.539(2) . ? C10 C12 1.542(2) . ? C14 N5 1.3607(19) . ? C14 N4 1.3660(19) . ? N4 C16 1.382(2) . ? N4 C17 1.489(2) . ? N5 C15 1.376(2) . ? N5 C21 1.474(2) . ? C15 C16 1.338(2) . ? C17 C19 1.514(2) . ? C17 C20 1.528(3) . ? C17 C18 1.531(3) . ? C21 C22 1.513(2) . ? C22 N6 1.4459(19) . ? N6 C23 1.4622(19) . ? C23 C25 1.528(2) . ? C23 C24 1.539(2) . ? C23 C26 1.542(2) . ? 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 N3 Mg1 N6 128.09(6) . . ? N3 Mg1 C1 94.22(6) . . ? N6 Mg1 C1 111.26(6) . . ? N3 Mg1 C14 113.71(6) . . ? N6 Mg1 C14 93.92(5) . . ? C1 Mg1 C14 117.57(6) . . ? N2 C1 N1 103.32(13) . . ? N2 C1 Mg1 116.64(10) . . ? N1 C1 Mg1 139.79(11) . . ? C1 N1 C3 111.37(13) . . ? C1 N1 C4 124.41(13) . . ? C3 N1 C4 123.99(14) . . ? C1 N2 C2 111.91(13) . . ? C1 N2 C8 125.92(13) . . ? C2 N2 C8 121.90(13) . . ? C3 C2 N2 106.72(15) . . ? C2 C3 N1 106.68(15) . . ? C6 C4 N1 112.03(16) . . ? C6 C4 C5 113.3(2) . . ? N1 C4 C5 109.37(15) . . ? C6 C4 C7 107.15(17) . . ? N1 C4 C7 107.67(14) . . ? C5 C4 C7 107.00(19) . . ? N2 C8 C9 115.46(13) . . ? N3 C9 C8 114.50(13) . . ? C9 N3 C10 113.35(12) . . ? C9 N3 Mg1 120.53(10) . . ? C10 N3 Mg1 125.91(10) . . ? N3 C10 C13 107.93(13) . . ? N3 C10 C11 112.57(14) . . ? C13 C10 C11 107.90(15) . . ? N3 C10 C12 111.54(14) . . ? C13 C10 C12 107.75(14) . . ? C11 C10 C12 108.97(14) . . ? N5 C14 N4 103.09(13) . . ? N5 C14 Mg1 117.22(10) . . ? N4 C14 Mg1 139.66(11) . . ? C14 N4 C16 111.27(13) . . ? C14 N4 C17 126.76(13) . . ? C16 N4 C17 121.70(13) . . ? C14 N5 C15 112.05(13) . . ? C14 N5 C21 125.38(13) . . ? C15 N5 C21 122.22(13) . . ? C16 C15 N5 106.52(14) . . ? C15 C16 N4 107.07(14) . . ? N4 C17 C19 110.59(13) . . ? N4 C17 C20 108.18(15) . . ? C19 C17 C20 110.66(16) . . ? N4 C17 C18 107.51(14) . . ? C19 C17 C18 109.11(15) . . ? C20 C17 C18 110.74(16) . . ? N5 C21 C22 115.10(13) . . ? N6 C22 C21 114.96(13) . . ? C22 N6 C23 113.41(12) . . ? C22 N6 Mg1 120.64(10) . . ? C23 N6 Mg1 125.88(10) . . ? N6 C23 C25 107.75(13) . . ? N6 C23 C24 111.66(14) . . ? C25 C23 C24 108.18(14) . . ? N6 C23 C26 113.35(13) . . ? C25 C23 C26 107.69(14) . . ? C24 C23 C26 108.02(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.615 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.045 #======end data_im3abs _database_code_depnum_ccdc_archive 'CCDC 244357' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains the 2 half molecules, with the U atoms lying on inversion centres; also there is half a molecule of toluene, disordered over 2 sites related by a centre of symmetry. The C atoms, C24, C25 and C26 are disordered over two sites each whose occupancies were constrained to sum to unity. Non-H atoms were refined anisotropically with restraints, except those of the partially occupied atoms. H atoms were included in calculated positions except those bonded to the disordered toluene molecule. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29.50 H51.50 N6 O2 U' _chemical_formula_weight 760.30 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' U U -9.6767 9.6646 '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 11.473(5) _cell_length_b 11.700(5) _cell_length_c 13.665(5) _cell_angle_alpha 66.755(5) _cell_angle_beta 80.951(5) _cell_angle_gamma 78.183(5) _cell_volume 1643.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4122 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.58 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 757 _exptl_absorpt_coefficient_mu 4.971 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5226 _exptl_absorpt_correction_T_max 0.8259 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus 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 13270 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.39 _reflns_number_total 6649 _reflns_number_gt 4149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-97 (Altomare,et al 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0388P)^2^+0.4634P] 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 6649 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0684 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _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 U1 U 0.0000 1.0000 0.0000 0.01558(9) Uani 1 2 d S . . O1 O 0.0779(3) 1.0892(4) -0.1232(3) 0.0209(8) Uani 1 1 d . . . N1 N 0.1404(4) 0.8230(4) 0.0217(3) 0.0173(10) Uani 1 1 d . . . N2 N 0.2087(4) 0.9064(4) 0.1791(4) 0.0206(10) Uani 1 1 d . . . N3 N 0.2468(4) 1.0936(4) 0.0936(4) 0.0225(11) Uani 1 1 d . . . C1 C 0.2278(6) 0.7939(6) -0.0608(5) 0.0260(13) Uani 1 1 d . . . C2 C 0.1753(6) 0.8548(6) -0.1695(4) 0.0297(14) Uani 1 1 d . . . H2A H 0.0998 0.8282 -0.1635 0.045 Uiso 1 1 calc R . . H2B H 0.2292 0.8294 -0.2212 0.045 Uiso 1 1 calc R . . H2C H 0.1641 0.9448 -0.1920 0.045 Uiso 1 1 calc R . . C3 C 0.2520(6) 0.6516(6) -0.0382(5) 0.0344(16) Uani 1 1 d . . . H3A H 0.2957 0.6080 0.0241 0.052 Uiso 1 1 calc R . . H3B H 0.2981 0.6372 -0.0984 0.052 Uiso 1 1 calc R . . H3C H 0.1775 0.6210 -0.0260 0.052 Uiso 1 1 calc R . . C4 C 0.3433(6) 0.8436(7) -0.0692(6) 0.0381(17) Uani 1 1 d . . . H4A H 0.3266 0.9333 -0.0887 0.057 Uiso 1 1 calc R . . H4B H 0.3990 0.8239 -0.1227 0.057 Uiso 1 1 calc R . . H4C H 0.3771 0.8050 -0.0015 0.057 Uiso 1 1 calc R . . C5 C 0.1709(5) 0.7373(5) 0.1293(4) 0.0256(13) Uani 1 1 d . . . H5A H 0.2540 0.6995 0.1245 0.031 Uiso 1 1 calc R . . H5B H 0.1234 0.6700 0.1531 0.031 Uiso 1 1 calc R . . C6 C 0.1532(5) 0.7936(5) 0.2149(4) 0.0226(12) Uani 1 1 d . . . H6A H 0.0684 0.8145 0.2326 0.027 Uiso 1 1 calc R . . H6B H 0.1878 0.7316 0.2790 0.027 Uiso 1 1 calc R . . C7 C 0.1644(5) 1.0186(5) 0.1059(4) 0.0179(11) Uani 1 1 d . . . C8 C 0.3156(6) 0.9103(6) 0.2093(5) 0.0357(16) Uani 1 1 d . . . H8 H 0.3623 0.8441 0.2580 0.043 Uiso 1 1 calc R . . C9 C 0.3405(5) 1.0263(6) 0.1562(5) 0.0348(16) Uani 1 1 d . . . H9 H 0.4078 1.0565 0.1603 0.042 Uiso 1 1 calc R . . C10 C 0.2452(5) 1.2266(5) 0.0155(5) 0.0242(13) Uani 1 1 d . . . C11 C 0.3095(6) 1.2236(6) -0.0895(5) 0.0379(16) Uani 1 1 d . . . H11A H 0.3904 1.1821 -0.0784 0.057 Uiso 1 1 calc R . . H11B H 0.3095 1.3082 -0.1406 0.057 Uiso 1 1 calc R . . H11C H 0.2693 1.1787 -0.1159 0.057 Uiso 1 1 calc R . . C12 C 0.1154(6) 1.2918(5) 0.0018(5) 0.0352(16) Uani 1 1 d . . . H12A H 0.0764 1.2529 -0.0313 0.053 Uiso 1 1 calc R . . H12B H 0.1138 1.3793 -0.0425 0.053 Uiso 1 1 calc R . . H12C H 0.0746 1.2840 0.0705 0.053 Uiso 1 1 calc R . . C13 C 0.3085(6) 1.2957(6) 0.0593(6) 0.0380(17) Uani 1 1 d . . . H13A H 0.2689 1.2940 0.1271 0.057 Uiso 1 1 calc R . . H13B H 0.3067 1.3815 0.0103 0.057 Uiso 1 1 calc R . . H13C H 0.3899 1.2554 0.0684 0.057 Uiso 1 1 calc R . . U2 U 0.5000 0.5000 0.5000 0.01707(9) Uani 1 2 d S . . O2 O 0.4141(3) 0.6286(4) 0.4015(3) 0.0277(9) Uani 1 1 d . . . N4 N 0.4605(4) 0.3590(4) 0.4364(4) 0.0229(11) Uani 1 1 d . . . N5 N 0.2990(5) 0.3021(5) 0.6356(4) 0.0301(12) Uani 1 1 d . . . N6 N 0.1850(5) 0.4712(6) 0.6331(4) 0.0340(13) Uani 1 1 d . A . C14 C 0.4270(5) 0.3837(6) 0.3279(5) 0.0300(14) Uani 1 1 d . . . C15 C 0.4758(6) 0.5014(8) 0.2453(5) 0.050(2) Uani 1 1 d . . . H15A H 0.4395 0.5737 0.2621 0.076 Uiso 1 1 calc R . . H15B H 0.4576 0.5141 0.1752 0.076 Uiso 1 1 calc R . . H15C H 0.5609 0.4897 0.2471 0.076 Uiso 1 1 calc R . . C16 C 0.2903(5) 0.4075(7) 0.3265(5) 0.0370(16) Uani 1 1 d . . . H16A H 0.2587 0.3331 0.3741 0.056 Uiso 1 1 calc R . . H16B H 0.2701 0.4281 0.2553 0.056 Uiso 1 1 calc R . . H16C H 0.2569 0.4762 0.3491 0.056 Uiso 1 1 calc R . . C17 C 0.4801(6) 0.2735(8) 0.2910(6) 0.056(2) Uani 1 1 d . . . H17A H 0.5642 0.2517 0.2997 0.084 Uiso 1 1 calc R . . H17B H 0.4677 0.2982 0.2171 0.084 Uiso 1 1 calc R . . H17C H 0.4414 0.2019 0.3332 0.084 Uiso 1 1 calc R . . C18 C 0.4477(6) 0.2314(6) 0.5085(6) 0.0359(16) Uani 1 1 d . . . H18A H 0.5244 0.1782 0.5074 0.043 Uiso 1 1 calc R . . H18B H 0.3920 0.2020 0.4805 0.043 Uiso 1 1 calc R . . C19 C 0.4051(6) 0.2121(6) 0.6238(5) 0.0390(17) Uani 1 1 d . . . H19A H 0.3868 0.1272 0.6605 0.047 Uiso 1 1 calc R . . H19B H 0.4695 0.2198 0.6580 0.047 Uiso 1 1 calc R . . C20 C 0.3014(5) 0.4256(6) 0.6099(4) 0.0256(13) Uani 1 1 d . . . C21 C 0.1879(6) 0.2710(7) 0.6714(5) 0.0411(18) Uani 1 1 d . . . H21 H 0.1667 0.1915 0.6927 0.049 Uiso 1 1 calc R . . C22 C 0.1160(6) 0.3753(8) 0.6701(5) 0.046(2) Uani 1 1 d . . . H22 H 0.0344 0.3832 0.6901 0.055 Uiso 1 1 calc R . . C23 C 0.1323(5) 0.6026(7) 0.6188(6) 0.0358(16) Uani 1 1 d . . . C24A C 0.2253(12) 0.6538(13) 0.6479(12) 0.033(4) Uiso 0.487(13) 1 d P A 1 H24A H 0.2435 0.6035 0.7202 0.050 Uiso 0.487(13) 1 calc PR A 1 H24B H 0.1958 0.7392 0.6414 0.050 Uiso 0.487(13) 1 calc PR A 1 H24C H 0.2964 0.6516 0.6006 0.050 Uiso 0.487(13) 1 calc PR A 1 C25A C 0.0243(15) 0.5860(16) 0.7027(13) 0.048(4) Uiso 0.487(13) 1 d P A 1 H25A H -0.0172 0.6672 0.6999 0.072 Uiso 0.487(13) 1 calc PR A 1 H25B H 0.0513 0.5382 0.7726 0.072 Uiso 0.487(13) 1 calc PR A 1 H25C H -0.0288 0.5421 0.6880 0.072 Uiso 0.487(13) 1 calc PR A 1 C26A C 0.1054(16) 0.6531(15) 0.5106(12) 0.047(4) Uiso 0.487(13) 1 d P A 1 H26A H 0.0712 0.7404 0.4910 0.070 Uiso 0.487(13) 1 calc PR A 1 H26B H 0.0493 0.6078 0.5019 0.070 Uiso 0.487(13) 1 calc PR A 1 H26C H 0.1773 0.6453 0.4655 0.070 Uiso 0.487(13) 1 calc PR A 1 C24B C 0.2218(14) 0.7006(14) 0.5677(13) 0.046(5) Uiso 0.513(13) 1 d P A 2 H24D H 0.2903 0.6726 0.6084 0.069 Uiso 0.513(13) 1 calc PR A 2 H24E H 0.1828 0.7812 0.5682 0.069 Uiso 0.513(13) 1 calc PR A 2 H24F H 0.2468 0.7076 0.4954 0.069 Uiso 0.513(13) 1 calc PR A 2 C25B C 0.0660(13) 0.6204(14) 0.7182(11) 0.041(4) Uiso 0.513(13) 1 d P A 2 H25D H 0.0315 0.7073 0.7009 0.061 Uiso 0.513(13) 1 calc PR A 2 H25E H 0.1206 0.5959 0.7720 0.061 Uiso 0.513(13) 1 calc PR A 2 H25F H 0.0037 0.5692 0.7446 0.061 Uiso 0.513(13) 1 calc PR A 2 C26B C 0.0340(12) 0.6598(12) 0.5311(10) 0.032(3) Uiso 0.513(13) 1 d P A 2 H26D H 0.0101 0.7483 0.5159 0.049 Uiso 0.513(13) 1 calc PR A 2 H26E H -0.0344 0.6177 0.5590 0.049 Uiso 0.513(13) 1 calc PR A 2 H26F H 0.0684 0.6474 0.4667 0.049 Uiso 0.513(13) 1 calc PR A 2 C1S C 1.1393(14) 1.0378(15) 0.5459(12) 0.051(4) Uiso 0.50 1 d P . . C2S C 1.0261(9) 0.9945(9) 0.5843(8) 0.070(3) Uiso 1 1 d . . . C3S C 0.9067(13) 0.9537(14) 0.6213(12) 0.042(3) Uiso 0.50 1 d P . . C4S C 0.8246(9) 0.9514(10) 0.5733(8) 0.082(3) Uiso 1 1 d . . . C5S C 0.9475(14) 0.9955(15) 0.5384(13) 0.050(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 U1 0.01762(19) 0.0157(2) 0.01342(18) -0.00528(15) 0.00002(14) -0.00391(15) O1 0.0169(19) 0.022(2) 0.024(2) -0.0108(17) 0.0019(16) -0.0007(16) N1 0.021(2) 0.016(2) 0.014(2) -0.0085(19) 0.0066(18) -0.0028(19) N2 0.022(2) 0.023(3) 0.019(2) -0.008(2) -0.0044(19) -0.004(2) N3 0.022(2) 0.021(3) 0.022(3) -0.003(2) -0.009(2) -0.003(2) C1 0.031(4) 0.023(3) 0.026(3) -0.015(3) 0.002(3) -0.003(3) C2 0.039(4) 0.029(3) 0.021(3) -0.013(3) 0.002(3) 0.001(3) C3 0.044(4) 0.027(3) 0.034(4) -0.020(3) -0.007(3) 0.009(3) C4 0.030(4) 0.046(4) 0.049(5) -0.031(4) 0.009(3) -0.009(3) C5 0.033(3) 0.019(3) 0.022(3) -0.007(3) 0.001(3) -0.003(3) C6 0.031(3) 0.017(3) 0.015(3) 0.000(2) -0.005(2) -0.004(2) C7 0.020(3) 0.018(3) 0.015(3) -0.006(2) 0.001(2) -0.006(2) C8 0.031(3) 0.035(4) 0.034(4) -0.001(3) -0.021(3) 0.000(3) C9 0.025(3) 0.031(4) 0.041(4) 0.000(3) -0.017(3) -0.004(3) C10 0.023(3) 0.020(3) 0.030(3) -0.005(3) -0.013(2) -0.004(2) C11 0.050(4) 0.031(4) 0.029(4) -0.005(3) -0.002(3) -0.014(3) C12 0.036(4) 0.014(3) 0.049(4) 0.002(3) -0.020(3) -0.002(3) C13 0.041(4) 0.029(4) 0.051(4) -0.016(3) -0.021(3) -0.004(3) U2 0.01586(19) 0.0179(2) 0.01761(19) -0.00601(16) -0.00209(14) -0.00386(15) O2 0.024(2) 0.020(2) 0.034(2) -0.0010(19) -0.0158(18) -0.0019(17) N4 0.023(3) 0.023(3) 0.025(3) -0.012(2) -0.004(2) -0.001(2) N5 0.033(3) 0.034(3) 0.021(3) -0.001(2) -0.006(2) -0.018(2) N6 0.028(3) 0.060(4) 0.029(3) -0.029(3) 0.006(2) -0.021(3) C14 0.024(3) 0.049(4) 0.027(3) -0.024(3) -0.003(3) -0.009(3) C15 0.053(5) 0.094(7) 0.018(3) -0.024(4) 0.005(3) -0.038(5) C16 0.028(3) 0.051(4) 0.041(4) -0.026(4) -0.006(3) -0.005(3) C17 0.028(4) 0.104(7) 0.066(5) -0.068(5) 0.002(4) -0.006(4) C18 0.029(4) 0.029(4) 0.058(5) -0.025(3) -0.011(3) 0.000(3) C19 0.047(4) 0.020(3) 0.040(4) 0.012(3) -0.022(3) -0.018(3) C20 0.022(3) 0.040(4) 0.015(3) -0.009(3) 0.000(2) -0.011(3) C21 0.048(4) 0.058(5) 0.021(3) -0.008(3) 0.003(3) -0.036(4) C22 0.036(4) 0.078(6) 0.036(4) -0.026(4) 0.015(3) -0.040(4) C23 0.018(3) 0.062(5) 0.039(4) -0.032(4) 0.006(3) -0.010(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 U1 O1 1.801(4) . ? U1 O1 1.801(4) 2_575 ? U1 N1 2.296(4) 2_575 ? U1 N1 2.296(4) . ? U1 C7 2.640(5) . ? U1 C7 2.640(5) 2_575 ? N1 C5 1.464(7) . ? N1 C1 1.484(7) . ? N2 C7 1.354(7) . ? N2 C8 1.369(7) . ? N2 C6 1.457(7) . ? N3 C7 1.366(7) . ? N3 C9 1.385(7) . ? N3 C10 1.499(7) . ? C1 C4 1.525(8) . ? C1 C2 1.531(8) . ? C1 C3 1.540(8) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.523(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 C9 1.329(9) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.516(8) . ? C10 C13 1.516(8) . ? C10 C12 1.531(8) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? U2 O2 1.805(4) 2_666 ? U2 O2 1.805(4) . ? U2 N4 2.291(5) 2_666 ? U2 N4 2.291(5) . ? U2 C20 2.629(6) 2_666 ? U2 C20 2.629(6) . ? N4 C18 1.451(8) . ? N4 C14 1.491(7) . ? N5 C20 1.350(8) . ? N5 C21 1.360(8) . ? N5 C19 1.472(8) . ? N6 C20 1.370(7) . ? N6 C22 1.390(8) . ? N6 C23 1.479(9) . ? C14 C16 1.538(8) . ? C14 C15 1.540(9) . ? C14 C17 1.544(9) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.514(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C21 C22 1.322(10) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C26A 1.419(16) . ? C23 C24A 1.496(14) . ? C23 C25B 1.517(14) . ? C23 C25A 1.538(16) . ? C23 C24B 1.574(16) . ? C23 C26B 1.624(13) . ? C24A H24A 0.9600 . ? C24A H24B 0.9600 . ? C24A H24C 0.9600 . ? C25A H25A 0.9600 . ? C25A H25B 0.9600 . ? C25A H25C 0.9600 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C24B H24D 0.9600 . ? C24B H24E 0.9600 . ? C24B H24F 0.9600 . ? C25B H25D 0.9600 . ? C25B H25E 0.9600 . ? C25B H25F 0.9600 . ? C26B H26D 0.9600 . ? C26B H26E 0.9600 . ? C26B H26F 0.9600 . ? C1S C2S 1.437(17) . ? C1S C4S 1.578(17) 2_776 ? C1S C5S 1.83(2) 2_776 ? C2S C5S 1.171(16) . ? C2S C3S 1.489(17) . ? C2S C5S 1.618(17) 2_776 ? C3S C5S 1.109(19) . ? C3S C4S 1.240(16) . ? C4S C5S 1.541(18) . ? C4S C1S 1.578(17) 2_776 ? C5S C5S 1.46(3) 2_776 ? C5S C2S 1.618(17) 2_776 ? C5S C1S 1.83(2) 2_776 ? 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 U1 O1 180.0 . 2_575 ? O1 U1 N1 88.04(16) . 2_575 ? O1 U1 N1 91.97(16) 2_575 2_575 ? O1 U1 N1 91.96(16) . . ? O1 U1 N1 88.03(16) 2_575 . ? N1 U1 N1 180.0 2_575 . ? O1 U1 C7 89.09(16) . . ? O1 U1 C7 90.91(16) 2_575 . ? N1 U1 C7 105.17(16) 2_575 . ? N1 U1 C7 74.83(16) . . ? O1 U1 C7 90.91(16) . 2_575 ? O1 U1 C7 89.09(16) 2_575 2_575 ? N1 U1 C7 74.83(16) 2_575 2_575 ? N1 U1 C7 105.17(16) . 2_575 ? C7 U1 C7 180.0 . 2_575 ? C5 N1 C1 111.0(4) . . ? C5 N1 U1 119.7(3) . . ? C1 N1 U1 127.9(3) . . ? C7 N2 C8 111.6(5) . . ? C7 N2 C6 123.8(5) . . ? C8 N2 C6 124.5(5) . . ? C7 N3 C9 110.8(5) . . ? C7 N3 C10 125.7(4) . . ? C9 N3 C10 123.3(5) . . ? N1 C1 C4 110.4(5) . . ? N1 C1 C2 109.9(5) . . ? C4 C1 C2 109.1(5) . . ? N1 C1 C3 111.4(5) . . ? C4 C1 C3 111.2(5) . . ? C2 C1 C3 104.7(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 117.1(5) . . ? N1 C5 H5A 108.0 . . ? C6 C5 H5A 108.0 . . ? N1 C5 H5B 108.0 . . ? C6 C5 H5B 108.0 . . ? H5A C5 H5B 107.3 . . ? N2 C6 C5 111.5(5) . . ? N2 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N2 C7 N3 103.5(4) . . ? N2 C7 U1 112.8(3) . . ? N3 C7 U1 140.0(4) . . ? C9 C8 N2 107.3(5) . . ? C9 C8 H8 126.3 . . ? N2 C8 H8 126.3 . . ? C8 C9 N3 106.8(6) . . ? C8 C9 H9 126.6 . . ? N3 C9 H9 126.6 . . ? N3 C10 C11 108.3(5) . . ? N3 C10 C13 108.9(5) . . ? C11 C10 C13 110.3(5) . . ? N3 C10 C12 109.1(5) . . ? C11 C10 C12 111.4(5) . . ? C13 C10 C12 108.9(5) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 U2 O2 180.0(2) 2_666 . ? O2 U2 N4 91.12(18) 2_666 2_666 ? O2 U2 N4 88.88(18) . 2_666 ? O2 U2 N4 88.88(18) 2_666 . ? O2 U2 N4 91.12(18) . . ? N4 U2 N4 180.0 2_666 . ? O2 U2 C20 90.08(18) 2_666 2_666 ? O2 U2 C20 89.92(18) . 2_666 ? N4 U2 C20 75.18(18) 2_666 2_666 ? N4 U2 C20 104.82(18) . 2_666 ? O2 U2 C20 89.92(18) 2_666 . ? O2 U2 C20 90.08(18) . . ? N4 U2 C20 104.82(18) 2_666 . ? N4 U2 C20 75.18(18) . . ? C20 U2 C20 180.000(1) 2_666 . ? C18 N4 C14 110.8(5) . . ? C18 N4 U2 120.4(4) . . ? C14 N4 U2 128.2(4) . . ? C20 N5 C21 112.7(6) . . ? C20 N5 C19 123.3(5) . . ? C21 N5 C19 123.9(6) . . ? C20 N6 C22 110.2(6) . . ? C20 N6 C23 127.8(5) . . ? C22 N6 C23 121.9(6) . . ? N4 C14 C16 110.4(5) . . ? N4 C14 C15 110.0(5) . . ? C16 C14 C15 108.2(6) . . ? N4 C14 C17 112.0(5) . . ? C16 C14 C17 109.1(5) . . ? C15 C14 C17 107.0(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 C19 116.7(5) . . ? N4 C18 H18A 108.1 . . ? C19 C18 H18A 108.1 . . ? N4 C18 H18B 108.1 . . ? C19 C18 H18B 108.1 . . ? H18A C18 H18B 107.3 . . ? N5 C19 C18 113.5(5) . . ? N5 C19 H19A 108.9 . . ? C18 C19 H19A 108.9 . . ? N5 C19 H19B 108.9 . . ? C18 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? N5 C20 N6 103.0(5) . . ? N5 C20 U2 113.5(4) . . ? N6 C20 U2 141.6(5) . . ? C22 C21 N5 106.8(6) . . ? C22 C21 H21 126.6 . . ? N5 C21 H21 126.6 . . ? C21 C22 N6 107.3(6) . . ? C21 C22 H22 126.3 . . ? N6 C22 H22 126.3 . . ? C26A C23 N6 101.6(8) . . ? C26A C23 C24A 118.0(10) . . ? N6 C23 C24A 105.3(7) . . ? C26A C23 C25B 132.4(10) . . ? N6 C23 C25B 115.1(8) . . ? C24A C23 C25B 81.5(8) . . ? C26A C23 C25A 115.8(10) . . ? N6 C23 C25A 102.7(8) . . ? C24A C23 C25A 111.0(9) . . ? C25B C23 C25A 29.7(7) . . ? C26A C23 C24B 79.5(9) . . ? N6 C23 C24B 114.9(7) . . ? C24A C23 C24B 38.5(7) . . ? C25B C23 C24B 108.7(9) . . ? C25A C23 C24B 135.8(10) . . ? C26A C23 C26B 30.3(7) . . ? N6 C23 C26B 111.4(7) . . ? C24A C23 C26B 135.1(9) . . ? C25B C23 C26B 104.5(8) . . ? C25A C23 C26B 85.5(8) . . ? C24B C23 C26B 100.7(9) . . ? C23 C24A H24A 109.5 . . ? C23 C24A H24B 109.5 . . ? C23 C24A H24C 109.5 . . ? C23 C25A H25A 109.5 . . ? C23 C25A H25B 109.5 . . ? C23 C25A H25C 109.5 . . ? C23 C26A H26A 109.5 . . ? C23 C26A H26B 109.5 . . ? C23 C26A H26C 109.5 . . ? C23 C24B H24D 109.5 . . ? C23 C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C23 C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C23 C25B H25D 109.5 . . ? C23 C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C23 C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C23 C26B H26D 109.5 . . ? C23 C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C23 C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C2S C1S C4S 111.0(12) . 2_776 ? C2S C1S C5S 57.9(8) . 2_776 ? C4S C1S C5S 53.2(8) 2_776 2_776 ? C5S C2S C1S 131.2(14) . . ? C5S C2S C3S 47.4(9) . . ? C1S C2S C3S 178.0(12) . . ? C5S C2S C5S 60.6(13) . 2_776 ? C1S C2S C5S 73.3(9) . 2_776 ? C3S C2S C5S 105.8(11) . 2_776 ? C5S C3S C4S 81.8(14) . . ? C5S C3S C2S 51.1(11) . . ? C4S C3S C2S 132.9(14) . . ? C3S C4S C5S 45.4(9) . . ? C3S C4S C1S 115.1(12) . 2_776 ? C5S C4S C1S 71.8(10) . 2_776 ? C3S C5S C2S 81.5(14) . . ? C3S C5S C5S 149(2) . 2_776 ? C2S C5S C5S 75.0(14) . 2_776 ? C3S C5S C4S 52.8(10) . . ? C2S C5S C4S 134.2(15) . . ? C5S C5S C4S 145.5(19) 2_776 . ? C3S C5S C2S 152.1(17) . 2_776 ? C2S C5S C2S 119.4(13) . 2_776 ? C5S C5S C2S 44.4(9) 2_776 2_776 ? C4S C5S C2S 103.8(12) . 2_776 ? C3S C5S C1S 105.9(15) . 2_776 ? C2S C5S C1S 161.9(14) . 2_776 ? C5S C5S C1S 91.9(15) 2_776 2_776 ? C4S C5S C1S 55.0(8) . 2_776 ? C2S C5S C1S 48.8(8) 2_776 2_776 ? 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 O1 U1 N1 C5 145.5(4) . . . . ? O1 U1 N1 C5 -34.5(4) 2_575 . . . ? N1 U1 N1 C5 55(5) 2_575 . . . ? C7 U1 N1 C5 57.0(4) . . . . ? C7 U1 N1 C5 -123.0(4) 2_575 . . . ? O1 U1 N1 C1 -19.6(5) . . . . ? O1 U1 N1 C1 160.4(5) 2_575 . . . ? N1 U1 N1 C1 -110(5) 2_575 . . . ? C7 U1 N1 C1 -108.2(5) . . . . ? C7 U1 N1 C1 71.8(5) 2_575 . . . ? C5 N1 C1 C4 -76.9(6) . . . . ? U1 N1 C1 C4 89.4(6) . . . . ? C5 N1 C1 C2 162.8(5) . . . . ? U1 N1 C1 C2 -31.0(7) . . . . ? C5 N1 C1 C3 47.2(6) . . . . ? U1 N1 C1 C3 -146.6(4) . . . . ? C1 N1 C5 C6 140.9(5) . . . . ? U1 N1 C5 C6 -26.6(7) . . . . ? C7 N2 C6 C5 73.1(7) . . . . ? C8 N2 C6 C5 -102.1(6) . . . . ? N1 C5 C6 N2 -50.2(7) . . . . ? C8 N2 C7 N3 -1.4(6) . . . . ? C6 N2 C7 N3 -177.2(5) . . . . ? C8 N2 C7 U1 161.6(4) . . . . ? C6 N2 C7 U1 -14.2(6) . . . . ? C9 N3 C7 N2 1.6(6) . . . . ? C10 N3 C7 N2 175.7(5) . . . . ? C9 N3 C7 U1 -153.6(5) . . . . ? C10 N3 C7 U1 20.5(9) . . . . ? O1 U1 C7 N2 -130.4(4) . . . . ? O1 U1 C7 N2 49.6(4) 2_575 . . . ? N1 U1 C7 N2 141.9(4) 2_575 . . . ? N1 U1 C7 N2 -38.1(4) . . . . ? C7 U1 C7 N2 -178(8) 2_575 . . . ? O1 U1 C7 N3 23.4(6) . . . . ? O1 U1 C7 N3 -156.6(6) 2_575 . . . ? N1 U1 C7 N3 -64.3(6) 2_575 . . . ? N1 U1 C7 N3 115.7(6) . . . . ? C7 U1 C7 N3 -24(8) 2_575 . . . ? C7 N2 C8 C9 0.7(7) . . . . ? C6 N2 C8 C9 176.4(6) . . . . ? N2 C8 C9 N3 0.4(8) . . . . ? C7 N3 C9 C8 -1.3(8) . . . . ? C10 N3 C9 C8 -175.5(6) . . . . ? C7 N3 C10 C11 -87.4(7) . . . . ? C9 N3 C10 C11 86.0(7) . . . . ? C7 N3 C10 C13 152.7(5) . . . . ? C9 N3 C10 C13 -34.0(8) . . . . ? C7 N3 C10 C12 33.9(8) . . . . ? C9 N3 C10 C12 -152.7(6) . . . . ? O2 U2 N4 C18 33.2(4) 2_666 . . . ? O2 U2 N4 C18 -146.8(4) . . . . ? N4 U2 N4 C18 -54(35) 2_666 . . . ? C20 U2 N4 C18 123.0(4) 2_666 . . . ? C20 U2 N4 C18 -57.0(4) . . . . ? O2 U2 N4 C14 -156.7(5) 2_666 . . . ? O2 U2 N4 C14 23.3(5) . . . . ? N4 U2 N4 C14 116(35) 2_666 . . . ? C20 U2 N4 C14 -66.9(5) 2_666 . . . ? C20 U2 N4 C14 113.1(5) . . . . ? C18 N4 C14 C16 77.6(6) . . . . ? U2 N4 C14 C16 -93.3(6) . . . . ? C18 N4 C14 C15 -163.0(5) . . . . ? U2 N4 C14 C15 26.1(7) . . . . ? C18 N4 C14 C17 -44.2(7) . . . . ? U2 N4 C14 C17 144.9(4) . . . . ? C14 N4 C18 C19 -144.4(5) . . . . ? U2 N4 C18 C19 27.2(7) . . . . ? C20 N5 C19 C18 -70.4(8) . . . . ? C21 N5 C19 C18 108.1(7) . . . . ? N4 C18 C19 N5 48.7(8) . . . . ? C21 N5 C20 N6 1.0(7) . . . . ? C19 N5 C20 N6 179.7(5) . . . . ? C21 N5 C20 U2 -166.6(4) . . . . ? C19 N5 C20 U2 12.1(7) . . . . ? C22 N6 C20 N5 -1.1(6) . . . . ? C23 N6 C20 N5 -178.5(5) . . . . ? C22 N6 C20 U2 160.5(5) . . . . ? C23 N6 C20 U2 -17.0(10) . . . . ? O2 U2 C20 N5 -50.9(4) 2_666 . . . ? O2 U2 C20 N5 129.1(4) . . . . ? N4 U2 C20 N5 -142.1(4) 2_666 . . . ? N4 U2 C20 N5 37.9(4) . . . . ? C20 U2 C20 N5 -26(77) 2_666 . . . ? O2 U2 C20 N6 148.7(6) 2_666 . . . ? O2 U2 C20 N6 -31.3(6) . . . . ? N4 U2 C20 N6 57.6(7) 2_666 . . . ? N4 U2 C20 N6 -122.4(7) . . . . ? C20 U2 C20 N6 174(77) 2_666 . . . ? C20 N5 C21 C22 -0.5(8) . . . . ? C19 N5 C21 C22 -179.2(6) . . . . ? N5 C21 C22 N6 -0.2(7) . . . . ? C20 N6 C22 C21 0.8(7) . . . . ? C23 N6 C22 C21 178.4(6) . . . . ? C20 N6 C23 C26A 85.5(10) . . . . ? C22 N6 C23 C26A -91.7(10) . . . . ? C20 N6 C23 C24A -38.1(10) . . . . ? C22 N6 C23 C24A 144.7(8) . . . . ? C20 N6 C23 C25B -125.7(9) . . . . ? C22 N6 C23 C25B 57.1(10) . . . . ? C20 N6 C23 C25A -154.3(9) . . . . ? C22 N6 C23 C25A 28.5(10) . . . . ? C20 N6 C23 C24B 1.8(11) . . . . ? C22 N6 C23 C24B -175.4(8) . . . . ? C20 N6 C23 C26B 115.5(8) . . . . ? C22 N6 C23 C26B -61.7(9) . . . . ? C4S C1S C2S C5S -21(2) 2_776 . . . ? C5S C1S C2S C5S -20(2) 2_776 . . . ? C4S C1S C2S C3S -66(36) 2_776 . . . ? C5S C1S C2S C3S -65(36) 2_776 . . . ? C4S C1S C2S C5S -1.1(11) 2_776 . . 2_776 ? C1S C2S C3S C5S 46(36) . . . . ? C5S C2S C3S C5S -17.8(18) 2_776 . . . ? C5S C2S C3S C4S 2.3(17) . . . . ? C1S C2S C3S C4S 49(36) . . . . ? C5S C2S C3S C4S -16(2) 2_776 . . . ? C2S C3S C4S C5S -1.8(13) . . . . ? C5S C3S C4S C1S 18.9(16) . . . 2_776 ? C2S C3S C4S C1S 17(2) . . . 2_776 ? C4S C3S C5S C2S -178.3(12) . . . . ? C4S C3S C5S C5S -138(4) . . . 2_776 ? C2S C3S C5S C5S 40(4) . . . 2_776 ? C2S C3S C5S C4S 178.3(12) . . . . ? C4S C3S C5S C2S -37(4) . . . 2_776 ? C2S C3S C5S C2S 141(4) . . . 2_776 ? C4S C3S C5S C1S -15.2(13) . . . 2_776 ? C2S C3S C5S C1S 163.1(16) . . . 2_776 ? C1S C2S C5S C3S -178.1(15) . . . . ? C5S C2S C5S C3S 160(2) 2_776 . . . ? C1S C2S C5S C5S 22(2) . . . 2_776 ? C3S C2S C5S C5S -160(2) . . . 2_776 ? C1S C2S C5S C4S -180.0(14) . . . . ? C3S C2S C5S C4S -1.9(14) . . . . ? C5S C2S C5S C4S 158(3) 2_776 . . . ? C1S C2S C5S C2S 22(2) . . . 2_776 ? C3S C2S C5S C2S -160(2) . . . 2_776 ? C5S C2S C5S C2S 0.002(1) 2_776 . . 2_776 ? C1S C2S C5S C1S 66(5) . . . 2_776 ? C3S C2S C5S C1S -116(5) . . . 2_776 ? C5S C2S C5S C1S 45(4) 2_776 . . 2_776 ? C1S C4S C5S C3S -162.0(15) 2_776 . . . ? C3S C4S C5S C2S 2.3(17) . . . . ? C1S C4S C5S C2S -160(2) 2_776 . . . ? C3S C4S C5S C5S 143(4) . . . 2_776 ? C1S C4S C5S C5S -19(3) 2_776 . . 2_776 ? C3S C4S C5S C2S 163.0(17) . . . 2_776 ? C1S C4S C5S C2S 1.0(10) 2_776 . . 2_776 ? C3S C4S C5S C1S 162.0(15) . . . 2_776 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.897 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.131 #======end data_h:\im13\work\im13abs _database_code_depnum_ccdc_archive 'CCDC 244358' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H52 N6 O2 U' _chemical_formula_weight 838.87 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.899(5) _cell_length_b 10.128(5) _cell_length_c 15.221(5) _cell_angle_alpha 90.000 _cell_angle_beta 97.608(5) _cell_angle_gamma 90.000 _cell_volume 3499(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1379 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 19.01 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 4.679 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7059 _exptl_absorpt_correction_T_max 0.9122 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus 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 12229 _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _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 1.79 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3085 _reflns_number_gt 1924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-97 (Altomare,et al 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0340P)^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 3085 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 U1 U 0.7500 0.2500 0.5000 0.01800(12) Uani 1 2 d S . . O1 O 0.7744(2) 0.1136(5) 0.5716(3) 0.0278(13) Uani 1 1 d . . . N1 N 0.6893(3) 0.1128(7) 0.4115(4) 0.0291(16) Uani 1 1 d . . . N2 N 0.7876(3) 0.1149(7) 0.2987(4) 0.0342(17) Uani 1 1 d . . . N3 N 0.8698(3) 0.1257(6) 0.3813(4) 0.0266(15) Uani 1 1 d . . . C1 C 0.6714(4) -0.0259(8) 0.4242(5) 0.033(2) Uani 1 1 d . . . C2 C 0.6579(5) -0.0400(10) 0.5182(6) 0.077(4) Uani 1 1 d . . . H2A H 0.6919 -0.0156 0.5587 0.116 Uiso 1 1 calc R . . H2B H 0.6476 -0.1300 0.5287 0.116 Uiso 1 1 calc R . . H2C H 0.6255 0.0165 0.5269 0.116 Uiso 1 1 calc R . . C3 C 0.6134(4) -0.0581(9) 0.3667(7) 0.061(3) Uani 1 1 d . . . H3A H 0.5851 0.0096 0.3737 0.092 Uiso 1 1 calc R . . H3B H 0.5989 -0.1415 0.3846 0.092 Uiso 1 1 calc R . . H3C H 0.6198 -0.0627 0.3057 0.092 Uiso 1 1 calc R . . C4 C 0.7168(4) -0.1257(8) 0.4076(7) 0.053(3) Uani 1 1 d . . . H4A H 0.7212 -0.1260 0.3457 0.079 Uiso 1 1 calc R . . H4B H 0.7045 -0.2116 0.4246 0.079 Uiso 1 1 calc R . . H4C H 0.7537 -0.1036 0.4418 0.079 Uiso 1 1 calc R . . C5 C 0.6821(3) 0.1538(9) 0.3191(5) 0.036(2) Uani 1 1 d . . . H5A H 0.6799 0.2495 0.3185 0.043 Uiso 1 1 calc R . . H5B H 0.6440 0.1217 0.2921 0.043 Uiso 1 1 calc R . . C6 C 0.7250(4) 0.1160(13) 0.2604(6) 0.068(4) Uani 1 1 d . . . H6A H 0.7206 0.1759 0.2102 0.081 Uiso 1 1 calc R . . H6B H 0.7148 0.0283 0.2376 0.081 Uiso 1 1 calc R . . C7 C 0.8120(3) 0.1621(8) 0.3784(5) 0.0263(18) Uani 1 1 d . . . C8 C 0.8282(4) 0.0526(8) 0.2530(6) 0.038(2) Uani 1 1 d . . . H8 H 0.8210 0.0141 0.1972 0.046 Uiso 1 1 calc R . . C9 C 0.8797(4) 0.0589(8) 0.3050(5) 0.033(2) Uani 1 1 d . . . H9 H 0.9154 0.0250 0.2926 0.039 Uiso 1 1 calc R . . C10 C 0.9155(3) 0.1547(7) 0.4524(5) 0.0244(18) Uani 1 1 d . . . C11 C 0.9516(3) 0.2671(10) 0.4438(5) 0.033(2) Uani 1 1 d . . . C12 C 0.9939(4) 0.2962(7) 0.5146(6) 0.033(2) Uani 1 1 d . . . H12 H 1.0175 0.3702 0.5109 0.039 Uiso 1 1 calc R . . C13 C 1.0025(3) 0.2214(8) 0.5896(5) 0.033(2) Uani 1 1 d . . . C14 C 0.9673(3) 0.1103(8) 0.5944(5) 0.0302(19) Uani 1 1 d . . . H14 H 0.9729 0.0585 0.6453 0.036 Uiso 1 1 calc R . . C15 C 0.9243(3) 0.0741(8) 0.5262(5) 0.0254(18) Uani 1 1 d . . . C16 C 0.9438(4) 0.3438(8) 0.3596(6) 0.038(2) Uani 1 1 d . . . H16A H 0.9704 0.4175 0.3647 0.057 Uiso 1 1 calc R . . H16B H 0.9040 0.3753 0.3482 0.057 Uiso 1 1 calc R . . H16C H 0.9520 0.2880 0.3117 0.057 Uiso 1 1 calc R . . C17 C 1.0493(3) 0.2617(11) 0.6658(5) 0.043(2) Uani 1 1 d . . . H17A H 1.0855 0.2810 0.6431 0.064 Uiso 1 1 calc R . . H17B H 1.0555 0.1907 0.7078 0.064 Uiso 1 1 calc R . . H17C H 1.0363 0.3387 0.6945 0.064 Uiso 1 1 calc R . . C18 C 0.8907(3) -0.0512(7) 0.5335(5) 0.0282(19) Uani 1 1 d . . . H18A H 0.8505 -0.0307 0.5393 0.042 Uiso 1 1 calc R . . H18B H 0.9080 -0.0997 0.5845 0.042 Uiso 1 1 calc R . . H18C H 0.8921 -0.1034 0.4812 0.042 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 U1 0.01705(18) 0.01814(18) 0.01953(19) -0.0002(4) 0.00512(12) -0.0017(4) O1 0.027(3) 0.031(3) 0.026(3) 0.000(2) 0.008(3) 0.002(3) N1 0.025(4) 0.038(4) 0.023(4) -0.002(3) 0.002(3) -0.005(3) N2 0.035(4) 0.057(5) 0.011(3) -0.003(3) 0.006(3) -0.006(4) N3 0.028(4) 0.028(4) 0.027(4) 0.000(3) 0.011(3) -0.005(3) C1 0.042(5) 0.032(5) 0.027(5) -0.002(4) 0.013(4) -0.008(4) C2 0.128(11) 0.057(7) 0.052(7) -0.007(6) 0.033(7) -0.057(7) C3 0.039(6) 0.038(6) 0.105(9) -0.005(6) 0.001(6) -0.018(5) C4 0.041(6) 0.029(5) 0.090(8) 0.019(5) 0.016(5) -0.002(4) C5 0.030(5) 0.049(6) 0.027(5) 0.005(4) -0.005(4) -0.010(4) C6 0.039(6) 0.138(11) 0.026(5) 0.018(6) 0.000(5) -0.002(7) C7 0.021(4) 0.032(5) 0.027(5) 0.007(4) 0.009(4) 0.001(4) C8 0.049(6) 0.037(5) 0.033(5) -0.003(4) 0.022(5) -0.013(4) C9 0.031(5) 0.037(5) 0.031(5) -0.002(4) 0.010(4) 0.004(4) C10 0.022(4) 0.027(4) 0.027(5) -0.006(4) 0.013(4) 0.000(4) C11 0.031(4) 0.032(6) 0.037(4) -0.007(5) 0.013(3) 0.001(5) C12 0.032(5) 0.026(5) 0.042(5) -0.005(4) 0.012(4) -0.005(3) C13 0.027(4) 0.035(7) 0.037(5) -0.001(4) 0.008(3) 0.003(4) C14 0.030(5) 0.038(5) 0.026(5) 0.007(4) 0.016(4) -0.001(4) C15 0.021(4) 0.031(5) 0.025(4) -0.008(4) 0.006(3) 0.000(4) C16 0.031(5) 0.035(5) 0.048(6) 0.005(4) 0.009(4) -0.011(4) C17 0.042(4) 0.040(5) 0.045(5) -0.005(6) 0.001(4) -0.005(6) C18 0.022(4) 0.030(5) 0.031(5) -0.005(4) 0.000(4) 0.003(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 U1 O1 1.802(5) . ? U1 O1 1.802(5) 7_656 ? U1 N1 2.277(6) 7_656 ? U1 N1 2.277(6) . ? U1 C7 2.633(7) 7_656 ? U1 C7 2.633(7) . ? N1 C5 1.455(9) . ? N1 C1 1.483(10) . ? N2 C7 1.353(9) . ? N2 C8 1.385(10) . ? N2 C6 1.476(10) . ? N3 C7 1.369(9) . ? N3 C9 1.388(9) . ? N3 C10 1.433(9) . ? C1 C4 1.495(11) . ? C1 C2 1.510(11) . ? C1 C3 1.525(11) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.463(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 C9 1.331(11) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C15 1.381(10) . ? C10 C11 1.424(11) . ? C11 C12 1.381(11) . ? C11 C16 1.488(11) . ? C12 C13 1.363(11) . ? C12 H12 0.9300 . ? C13 C14 1.392(10) . ? C13 C17 1.527(11) . ? C14 C15 1.382(10) . ? C14 H14 0.9300 . ? C15 C18 1.495(10) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 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 U1 O1 179.999(2) . 7_656 ? O1 U1 N1 89.6(2) . 7_656 ? O1 U1 N1 90.4(2) 7_656 7_656 ? O1 U1 N1 90.4(2) . . ? O1 U1 N1 89.6(2) 7_656 . ? N1 U1 N1 179.998(1) 7_656 . ? O1 U1 C7 89.2(2) . 7_656 ? O1 U1 C7 90.8(2) 7_656 7_656 ? N1 U1 C7 73.8(2) 7_656 7_656 ? N1 U1 C7 106.2(2) . 7_656 ? O1 U1 C7 90.8(2) . . ? O1 U1 C7 89.2(2) 7_656 . ? N1 U1 C7 106.2(2) 7_656 . ? N1 U1 C7 73.8(2) . . ? C7 U1 C7 180.0(2) 7_656 . ? C5 N1 C1 113.5(6) . . ? C5 N1 U1 112.3(5) . . ? C1 N1 U1 131.2(5) . . ? C7 N2 C8 112.7(7) . . ? C7 N2 C6 128.0(7) . . ? C8 N2 C6 119.1(7) . . ? C7 N3 C9 111.6(6) . . ? C7 N3 C10 125.2(6) . . ? C9 N3 C10 123.2(6) . . ? N1 C1 C4 114.1(7) . . ? N1 C1 C2 107.9(7) . . ? C4 C1 C2 109.3(8) . . ? N1 C1 C3 111.3(7) . . ? C4 C1 C3 109.3(7) . . ? C2 C1 C3 104.6(8) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 121.1(7) . . ? N1 C5 H5A 107.1 . . ? C6 C5 H5A 107.1 . . ? N1 C5 H5B 107.1 . . ? C6 C5 H5B 107.1 . . ? H5A C5 H5B 106.8 . . ? C5 C6 N2 117.1(7) . . ? C5 C6 H6A 108.0 . . ? N2 C6 H6A 108.0 . . ? C5 C6 H6B 108.0 . . ? N2 C6 H6B 108.0 . . ? H6A C6 H6B 107.3 . . ? N2 C7 N3 102.5(6) . . ? N2 C7 U1 123.5(5) . . ? N3 C7 U1 132.6(5) . . ? C9 C8 N2 106.2(7) . . ? C9 C8 H8 126.9 . . ? N2 C8 H8 126.9 . . ? C8 C9 N3 107.0(7) . . ? C8 C9 H9 126.5 . . ? N3 C9 H9 126.5 . . ? C15 C10 C11 121.6(7) . . ? C15 C10 N3 120.4(7) . . ? C11 C10 N3 118.0(7) . . ? C12 C11 C10 117.0(8) . . ? C12 C11 C16 123.5(9) . . ? C10 C11 C16 119.4(7) . . ? C13 C12 C11 122.9(8) . . ? C13 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? C12 C13 C14 118.2(8) . . ? C12 C13 C17 119.8(8) . . ? C14 C13 C17 122.0(8) . . ? C15 C14 C13 122.3(8) . . ? C15 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C10 C15 C14 117.8(7) . . ? C10 C15 C18 122.7(7) . . ? C14 C15 C18 119.4(7) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 O1 U1 N1 C5 -148.4(5) . . . . ? O1 U1 N1 C5 31.6(5) 7_656 . . . ? N1 U1 N1 C5 89(13) 7_656 . . . ? C7 U1 N1 C5 122.3(5) 7_656 . . . ? C7 U1 N1 C5 -57.7(5) . . . . ? O1 U1 N1 C1 10.4(7) . . . . ? O1 U1 N1 C1 -169.6(7) 7_656 . . . ? N1 U1 N1 C1 -112(13) 7_656 . . . ? C7 U1 N1 C1 -78.9(7) 7_656 . . . ? C7 U1 N1 C1 101.1(7) . . . . ? C5 N1 C1 C4 80.4(9) . . . . ? U1 N1 C1 C4 -78.2(9) . . . . ? C5 N1 C1 C2 -158.0(8) . . . . ? U1 N1 C1 C2 43.4(10) . . . . ? C5 N1 C1 C3 -43.8(9) . . . . ? U1 N1 C1 C3 157.6(6) . . . . ? C1 N1 C5 C6 -78.6(10) . . . . ? U1 N1 C5 C6 84.1(9) . . . . ? N1 C5 C6 N2 -38.1(14) . . . . ? C7 N2 C6 C5 -10.1(15) . . . . ? C8 N2 C6 C5 165.7(9) . . . . ? C8 N2 C7 N3 -0.5(9) . . . . ? C6 N2 C7 N3 175.5(9) . . . . ? C8 N2 C7 U1 -168.9(5) . . . . ? C6 N2 C7 U1 7.2(12) . . . . ? C9 N3 C7 N2 0.2(8) . . . . ? C10 N3 C7 N2 178.8(7) . . . . ? C9 N3 C7 U1 167.0(6) . . . . ? C10 N3 C7 U1 -14.4(11) . . . . ? O1 U1 C7 N2 112.8(6) . . . . ? O1 U1 C7 N2 -67.2(6) 7_656 . . . ? N1 U1 C7 N2 -157.4(6) 7_656 . . . ? N1 U1 C7 N2 22.6(6) . . . . ? C7 U1 C7 N2 -124(28) 7_656 . . . ? O1 U1 C7 N3 -51.7(7) . . . . ? O1 U1 C7 N3 128.3(7) 7_656 . . . ? N1 U1 C7 N3 38.1(7) 7_656 . . . ? N1 U1 C7 N3 -141.9(7) . . . . ? C7 U1 C7 N3 71(28) 7_656 . . . ? C7 N2 C8 C9 0.6(10) . . . . ? C6 N2 C8 C9 -175.8(8) . . . . ? N2 C8 C9 N3 -0.4(9) . . . . ? C7 N3 C9 C8 0.1(9) . . . . ? C10 N3 C9 C8 -178.4(7) . . . . ? C7 N3 C10 C15 84.2(10) . . . . ? C9 N3 C10 C15 -97.4(9) . . . . ? C7 N3 C10 C11 -96.6(9) . . . . ? C9 N3 C10 C11 81.8(10) . . . . ? C15 C10 C11 C12 -3.3(12) . . . . ? N3 C10 C11 C12 177.5(7) . . . . ? C15 C10 C11 C16 174.6(7) . . . . ? N3 C10 C11 C16 -4.6(11) . . . . ? C10 C11 C12 C13 1.1(12) . . . . ? C16 C11 C12 C13 -176.7(8) . . . . ? C11 C12 C13 C14 0.5(12) . . . . ? C11 C12 C13 C17 -178.8(8) . . . . ? C12 C13 C14 C15 -0.2(12) . . . . ? C17 C13 C14 C15 179.1(7) . . . . ? C11 C10 C15 C14 3.7(11) . . . . ? N3 C10 C15 C14 -177.1(6) . . . . ? C11 C10 C15 C18 -174.3(7) . . . . ? N3 C10 C15 C18 4.9(11) . . . . ? C13 C14 C15 C10 -1.9(11) . . . . ? C13 C14 C15 C18 176.1(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.985 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.136 #======end