# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Hardwick, Hardwick' ' Royal, Drew' 'Helliwell, Madeleine' 'Pope, Simon' 'Ashton, Lorna' 'Goodacre, Royston' 'Sharrad, Clint' _publ_contact_author_name 'Sharrad, Clint' _publ_contact_author_email clint.a.sharrad@manchester.ac.uk _publ_section_title ; Structural, Spectroscopic and Redox Properties of Uranyl Complexes with a Maleonitrile Containing Ligand ; # Attachment '- salmntall.cif' data_bcas021p21n _database_code_depnum_ccdc_archive 'CCDC 802704' #TrackingRef '- salmntall.cif' _audit_creation_date 2009-03-02T17:23:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; 'salmnt(Et2N)2).DCM' ; _chemical_formula_sum 'C27 H32 Cl2 N6 O2' _chemical_formula_weight 543.49 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.622(5) _cell_length_b 8.457(5) _cell_length_c 22.219(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 96.106(5) _cell_angle_gamma 90.000(5) _cell_volume 2732(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1060 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 22.26 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour 'dark red' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.35 _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.274 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.19 _diffrn_reflns_av_unetI/netI 0.2022 _diffrn_reflns_number 19354 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 5001 _reflns_number_gt 2125 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1104P)^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_number_reflns 5001 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.184 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.242 _refine_ls_wR_factor_gt 0.191 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.35 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.1 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 C27A C 0.9629(8) 0.1398(14) 1.1398(5) 0.045(4) Uiso 0.806(4) 1 d P A 1 H27A H 1.0032 0.1597 1.1766 0.054 Uiso 0.806(4) 1 calc PR A 1 H27B H 0.9239 0.0508 1.1473 0.054 Uiso 0.806(4) 1 calc PR A 1 Cl1A Cl 0.89385(14) 0.3071(2) 1.12265(10) 0.0401(7) Uiso 0.806(4) 1 d P A 1 Cl2A Cl 1.02908(18) 0.0912(3) 1.08215(12) 0.0664(9) Uiso 0.806(4) 1 d P A 1 C27B C 0.964(3) 0.150(5) 1.157(2) 0.029(12) Uiso 0.194(4) 1 d P A 2 H27C H 0.9614 0.2168 1.1923 0.035 Uiso 0.194(4) 1 calc PR A 2 H27D H 0.9248 0.0593 1.1602 0.035 Uiso 0.194(4) 1 calc PR A 2 Cl1B Cl 1.0760(9) 0.0915(16) 1.1511(6) 0.090(5) Uiso 0.194(4) 1 d P A 2 Cl2B Cl 0.9317(10) 0.2553(16) 1.0911(7) 0.092(5) Uiso 0.194(4) 1 d P A 2 O2 O 0.6425(2) 0.0330(5) 1.10030(16) 0.0277(10) Uani 1 1 d . . . H2 H 0.6297 0.0498 1.064 0.042 Uiso 1 1 calc R . . O1 O 0.4755(2) 0.2628(4) 1.07465(16) 0.0250(9) Uani 1 1 d . . . H1 H 0.5037 0.2315 1.047 0.038 Uiso 1 1 calc R . . N5 N 0.6596(3) 0.0151(5) 0.98619(19) 0.0195(11) Uani 1 1 d . . . N2 N 0.5125(3) 0.2252(5) 0.96050(19) 0.0192(10) Uani 1 1 d . . . C7 C 0.4106(3) 0.3677(6) 1.0527(2) 0.0190(12) Uani 1 1 d . . . C9 C 0.3313(3) 0.5197(6) 0.9721(2) 0.0206(13) Uani 1 1 d . . . H9 H 0.323 0.5498 0.9316 0.025 Uiso 1 1 calc R . . N1 N 0.2344(3) 0.6160(5) 1.1125(2) 0.0268(12) Uani 1 1 d . . . N6 N 0.8526(3) -0.2508(6) 1.2384(2) 0.0310(13) Uani 1 1 d . . . C16 C 0.7289(3) -0.0810(6) 0.9988(2) 0.0200(13) Uani 1 1 d . . . H16 H 0.7592 -0.1221 0.9675 0.024 Uiso 1 1 calc R . . C17 C 0.7589(3) -0.1238(6) 1.0595(2) 0.0173(12) Uani 1 1 d . . . C22 C 0.8333(4) -0.2275(6) 1.0731(2) 0.0230(13) Uani 1 1 d . . . H22 H 0.8626 -0.2685 1.0414 0.028 Uiso 1 1 calc R . . C6 C 0.3555(3) 0.4350(6) 1.0924(2) 0.0215(13) Uani 1 1 d . . . H6 H 0.3636 0.4057 1.133 0.026 Uiso 1 1 calc R . . C14 C 0.6301(4) 0.0580(6) 0.9271(2) 0.0196(13) Uani 1 1 d . . . C12 C 0.5580(4) 0.1609(6) 0.9156(2) 0.0178(12) Uani 1 1 d . . . C18 C 0.7158(4) -0.0654(6) 1.1085(2) 0.0227(13) Uani 1 1 d . . . C11 C 0.4496(4) 0.3331(6) 0.9468(2) 0.0209(13) Uani 1 1 d . . . H11 H 0.4381 0.364 0.9065 0.025 Uiso 1 1 calc R . . C20 C 0.8209(4) -0.2100(7) 1.1800(2) 0.0233(13) Uani 1 1 d . . . C8 C 0.3982(3) 0.4054(6) 0.9898(2) 0.0177(12) Uani 1 1 d . . . C10 C 0.2782(4) 0.5886(6) 1.0111(2) 0.0203(13) Uani 1 1 d . . . H10 H 0.235 0.6643 0.997 0.024 Uiso 1 1 calc R . . C13 C 0.5326(4) 0.2029(7) 0.8519(3) 0.0242(13) Uani 1 1 d . . . C4 C 0.1549(4) 0.7135(7) 1.0899(3) 0.0337(15) Uani 1 1 d . . . H4A H 0.1747 0.7923 1.0623 0.04 Uiso 1 1 calc R . . H4B H 0.1328 0.769 1.1237 0.04 Uiso 1 1 calc R . . C21 C 0.8644(4) -0.2705(6) 1.1306(2) 0.0234(13) Uani 1 1 d . . . H21 H 0.914 -0.3392 1.1375 0.028 Uiso 1 1 calc R . . C15 C 0.6763(4) -0.0023(7) 0.8780(3) 0.0263(14) Uani 1 1 d . . . C23 C 0.9374(4) -0.3401(8) 1.2535(3) 0.0392(17) Uani 1 1 d . . . H23A H 0.9378 -0.4296 1.2262 0.047 Uiso 1 1 calc R . . H23B H 0.9378 -0.3814 1.2942 0.047 Uiso 1 1 calc R . . C19 C 0.7465(4) -0.1083(7) 1.1673(2) 0.0283(14) Uani 1 1 d . . . H19 H 0.7168 -0.0684 1.199 0.034 Uiso 1 1 calc R . . C5 C 0.2880(4) 0.5460(6) 1.0733(2) 0.0213(13) Uani 1 1 d . . . C2 C 0.2424(4) 0.5723(8) 1.1771(3) 0.0376(16) Uani 1 1 d . . . H2A H 0.2232 0.6615 1.2001 0.045 Uiso 1 1 calc R . . H2B H 0.3065 0.5514 1.1906 0.045 Uiso 1 1 calc R . . C3 C 0.0760(4) 0.6189(8) 1.0575(3) 0.0446(18) Uani 1 1 d . . . H3A H 0.0262 0.689 1.0442 0.067 Uiso 1 1 calc R . . H3B H 0.0553 0.5417 1.0846 0.067 Uiso 1 1 calc R . . H3C H 0.0967 0.5664 1.0231 0.067 Uiso 1 1 calc R . . C24 C 1.0248(4) -0.2431(8) 1.2496(3) 0.0446(19) Uani 1 1 d . . . H24A H 1.0777 -0.3091 1.2595 0.067 Uiso 1 1 calc R . . H24B H 1.0262 -0.1565 1.2776 0.067 Uiso 1 1 calc R . . H24C H 1.0254 -0.2028 1.2092 0.067 Uiso 1 1 calc R . . C25 C 0.8089(5) -0.1816(8) 1.2884(3) 0.0475(19) Uani 1 1 d . . . H25A H 0.7426 -0.1839 1.2789 0.057 Uiso 1 1 calc R . . H25B H 0.8245 -0.2435 1.3248 0.057 Uiso 1 1 calc R . . C26 C 0.8388(4) -0.0215(9) 1.2988(3) 0.052(2) Uani 1 1 d . . . H26C H 0.81 0.0219 1.332 0.078 Uiso 1 1 calc R . . H26A H 0.8221 0.0402 1.263 0.078 Uiso 1 1 calc R . . H26B H 0.9044 -0.0194 1.3083 0.078 Uiso 1 1 calc R . . C1 C 0.1861(5) 0.4295(8) 1.1908(3) 0.052(2) Uani 1 1 d . . . H1A H 0.194 0.409 1.2335 0.077 Uiso 1 1 calc R . . H1B H 0.2063 0.3394 1.1695 0.077 Uiso 1 1 calc R . . H1C H 0.1224 0.4494 1.178 0.077 Uiso 1 1 calc R . . N4 N 0.7173(4) -0.0524(6) 0.8412(2) 0.0391(14) Uani 1 1 d . . . N3 N 0.5107(3) 0.2362(6) 0.8025(2) 0.0377(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2 0.020(2) 0.044(3) 0.019(2) -0.0060(18) -0.0003(17) 0.0104(19) O1 0.026(2) 0.033(2) 0.016(2) 0.0018(17) 0.0055(17) 0.0077(19) N5 0.020(2) 0.020(3) 0.019(3) -0.001(2) 0.003(2) -0.003(2) N2 0.016(2) 0.024(3) 0.018(2) 0.001(2) 0.0012(19) -0.001(2) C7 0.016(3) 0.017(3) 0.023(3) 0.001(2) -0.005(2) 0.000(2) C9 0.019(3) 0.025(3) 0.018(3) -0.002(2) -0.001(2) 0.000(3) N1 0.028(3) 0.027(3) 0.027(3) -0.002(2) 0.009(2) 0.006(2) N6 0.021(3) 0.052(3) 0.020(3) 0.009(2) 0.006(2) 0.011(2) C16 0.017(3) 0.023(3) 0.021(3) -0.006(3) 0.005(2) -0.005(3) C17 0.013(3) 0.024(3) 0.015(3) -0.002(2) -0.001(2) 0.000(2) C22 0.018(3) 0.028(3) 0.024(3) -0.008(3) 0.010(2) 0.001(3) C6 0.021(3) 0.027(3) 0.016(3) -0.003(2) 0.001(2) -0.002(3) C14 0.024(3) 0.019(3) 0.015(3) -0.003(2) 0.000(2) -0.002(3) C12 0.021(3) 0.020(3) 0.013(3) -0.005(2) 0.004(2) -0.001(2) C18 0.019(3) 0.023(3) 0.026(3) -0.001(3) 0.001(3) 0.000(3) C11 0.021(3) 0.026(3) 0.016(3) -0.002(2) 0.001(2) -0.008(3) C20 0.018(3) 0.028(3) 0.023(3) 0.004(3) 0.001(2) 0.001(3) C8 0.013(3) 0.022(3) 0.018(3) 0.000(2) 0.001(2) -0.002(2) C10 0.017(3) 0.021(3) 0.023(3) 0.000(2) 0.001(2) 0.001(2) C13 0.022(3) 0.027(3) 0.024(3) -0.004(3) 0.004(3) 0.006(3) C4 0.031(3) 0.037(4) 0.035(4) -0.004(3) 0.012(3) 0.011(3) C21 0.020(3) 0.024(3) 0.027(3) -0.001(3) 0.002(3) 0.005(2) C15 0.028(3) 0.029(4) 0.022(3) -0.005(3) 0.001(3) 0.005(3) C23 0.032(4) 0.056(5) 0.029(4) 0.015(3) 0.000(3) 0.019(3) C19 0.029(3) 0.045(4) 0.011(3) -0.004(3) 0.005(3) 0.006(3) C5 0.019(3) 0.020(3) 0.025(3) -0.005(2) 0.000(2) 0.002(3) C2 0.043(4) 0.046(4) 0.026(3) -0.004(3) 0.011(3) 0.016(3) C3 0.018(3) 0.059(5) 0.058(5) 0.009(4) 0.008(3) 0.004(3) C24 0.022(3) 0.077(5) 0.035(4) -0.002(4) 0.003(3) 0.012(3) C25 0.055(5) 0.056(5) 0.030(4) 0.010(4) -0.003(3) 0.014(4) C26 0.041(4) 0.082(6) 0.033(4) -0.004(4) 0.008(3) 0.011(4) C1 0.078(5) 0.043(5) 0.038(4) 0.010(3) 0.027(4) 0.013(4) N4 0.044(3) 0.050(4) 0.023(3) -0.005(3) 0.004(3) 0.021(3) N3 0.039(3) 0.050(4) 0.023(3) -0.004(3) 0.000(2) 0.012(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C27A Cl2A 1.735(12) . ? C27A Cl1A 1.756(12) . ? C27A H27A 0.97 . ? C27A H27B 0.97 . ? C27B Cl1B 1.72(4) . ? C27B Cl2B 1.74(4) . ? C27B H27C 0.97 . ? C27B H27D 0.97 . ? O2 C18 1.353(6) . ? O2 H2 0.82 . ? O1 C7 1.351(6) . ? O1 H1 0.82 . ? N5 C16 1.306(6) . ? N5 C14 1.386(6) . ? N2 C11 1.308(7) . ? N2 C12 1.370(6) . ? C7 C6 1.378(7) . ? C7 C8 1.428(7) . ? C9 C10 1.356(7) . ? C9 C8 1.401(7) . ? C9 H9 0.93 . ? N1 C5 1.367(7) . ? N1 C4 1.469(7) . ? N1 C2 1.474(7) . ? N6 C20 1.374(7) . ? N6 C23 1.460(7) . ? N6 C25 1.461(8) . ? C16 C17 1.421(7) . ? C16 H16 0.93 . ? C17 C18 1.404(7) . ? C17 C22 1.405(7) . ? C22 C21 1.358(7) . ? C22 H22 0.93 . ? C6 C5 1.396(7) . ? C6 H6 0.93 . ? C14 C12 1.370(7) . ? C14 C15 1.436(8) . ? C12 C13 1.468(8) . ? C18 C19 1.385(7) . ? C11 C8 1.416(7) . ? C11 H11 0.93 . ? C20 C19 1.392(7) . ? C20 C21 1.422(7) . ? C10 C5 1.421(7) . ? C10 H10 0.93 . ? C13 N3 1.146(7) . ? C4 C3 1.521(8) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C21 H21 0.93 . ? C15 N4 1.147(7) . ? C23 C24 1.529(8) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C19 H19 0.93 . ? C2 C1 1.510(9) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 C26 1.434(9) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26 H26C 0.96 . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? 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 Cl2A C27A Cl1A 112.5(7) . . ? Cl2A C27A H27A 109.1 . . ? Cl1A C27A H27A 109.1 . . ? Cl2A C27A H27B 109.1 . . ? Cl1A C27A H27B 109.1 . . ? H27A C27A H27B 107.8 . . ? Cl1B C27B Cl2B 105(2) . . ? Cl1B C27B H27C 110.7 . . ? Cl2B C27B H27C 110.7 . . ? Cl1B C27B H27D 110.7 . . ? Cl2B C27B H27D 110.7 . . ? H27C C27B H27D 108.8 . . ? C18 O2 H2 109.5 . . ? C7 O1 H1 109.5 . . ? C16 N5 C14 121.5(5) . . ? C11 N2 C12 119.4(5) . . ? O1 C7 C6 118.4(5) . . ? O1 C7 C8 120.7(5) . . ? C6 C7 C8 120.8(5) . . ? C10 C9 C8 123.2(5) . . ? C10 C9 H9 118.4 . . ? C8 C9 H9 118.4 . . ? C5 N1 C4 120.7(5) . . ? C5 N1 C2 121.4(5) . . ? C4 N1 C2 116.8(5) . . ? C20 N6 C23 122.6(5) . . ? C20 N6 C25 119.1(5) . . ? C23 N6 C25 117.5(5) . . ? N5 C16 C17 121.1(5) . . ? N5 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C18 C17 C22 117.1(5) . . ? C18 C17 C16 121.8(5) . . ? C22 C17 C16 121.1(5) . . ? C21 C22 C17 122.9(5) . . ? C21 C22 H22 118.6 . . ? C17 C22 H22 118.6 . . ? C7 C6 C5 121.7(5) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C12 C14 N5 119.9(5) . . ? C12 C14 C15 119.9(5) . . ? N5 C14 C15 120.1(5) . . ? N2 C12 C14 122.7(5) . . ? N2 C12 C13 120.9(5) . . ? C14 C12 C13 116.4(5) . . ? O2 C18 C19 117.5(5) . . ? O2 C18 C17 121.8(5) . . ? C19 C18 C17 120.7(5) . . ? N2 C11 C8 123.6(5) . . ? N2 C11 H11 118.2 . . ? C8 C11 H11 118.2 . . ? N6 C20 C19 121.6(5) . . ? N6 C20 C21 120.4(5) . . ? C19 C20 C21 118.0(5) . . ? C9 C8 C11 120.9(5) . . ? C9 C8 C7 116.2(5) . . ? C11 C8 C7 122.9(5) . . ? C9 C10 C5 120.6(5) . . ? C9 C10 H10 119.7 . . ? C5 C10 H10 119.7 . . ? N3 C13 C12 178.4(6) . . ? N1 C4 C3 113.6(5) . . ? N1 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? N1 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C22 C21 C20 119.8(5) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? N4 C15 C14 176.2(6) . . ? N6 C23 C24 113.8(5) . . ? N6 C23 H23A 108.8 . . ? C24 C23 H23A 108.8 . . ? N6 C23 H23B 108.8 . . ? C24 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C18 C19 C20 121.4(5) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? N1 C5 C6 122.2(5) . . ? N1 C5 C10 120.4(5) . . ? C6 C5 C10 117.4(5) . . ? N1 C2 C1 114.1(5) . . ? N1 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? N1 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N6 110.5(6) . . ? C26 C25 H25A 109.6 . . ? N6 C25 H25A 109.6 . . ? C26 C25 H25B 109.6 . . ? N6 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C25 C26 H26C 109.5 . . ? C25 C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26C C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 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 C14 N5 C16 C17 179.7(5) . . . . ? N5 C16 C17 C18 0.1(8) . . . . ? N5 C16 C17 C22 179.8(5) . . . . ? C18 C17 C22 C21 -0.7(8) . . . . ? C16 C17 C22 C21 179.6(5) . . . . ? O1 C7 C6 C5 179.0(5) . . . . ? C8 C7 C6 C5 -2.2(8) . . . . ? C16 N5 C14 C12 -179.0(5) . . . . ? C16 N5 C14 C15 -0.5(8) . . . . ? C11 N2 C12 C14 174.1(5) . . . . ? C11 N2 C12 C13 -4.5(7) . . . . ? N5 C14 C12 N2 0.0(8) . . . . ? C15 C14 C12 N2 -178.5(5) . . . . ? N5 C14 C12 C13 178.6(5) . . . . ? C15 C14 C12 C13 0.1(8) . . . . ? C22 C17 C18 O2 -178.8(5) . . . . ? C16 C17 C18 O2 1.0(8) . . . . ? C22 C17 C18 C19 0.5(8) . . . . ? C16 C17 C18 C19 -179.8(5) . . . . ? C12 N2 C11 C8 179.3(5) . . . . ? C23 N6 C20 C19 -171.8(6) . . . . ? C25 N6 C20 C19 -1.9(8) . . . . ? C23 N6 C20 C21 7.6(9) . . . . ? C25 N6 C20 C21 177.5(6) . . . . ? C10 C9 C8 C11 177.8(5) . . . . ? C10 C9 C8 C7 -2.2(8) . . . . ? N2 C11 C8 C9 -179.6(5) . . . . ? N2 C11 C8 C7 0.4(8) . . . . ? O1 C7 C8 C9 -177.8(5) . . . . ? C6 C7 C8 C9 3.5(7) . . . . ? O1 C7 C8 C11 2.2(8) . . . . ? C6 C7 C8 C11 -176.5(5) . . . . ? C8 C9 C10 C5 -0.3(8) . . . . ? N2 C12 C13 N3 -3E1(2) . . . . ? C14 C12 C13 N3 15E1(2) . . . . ? C5 N1 C4 C3 69.4(7) . . . . ? C2 N1 C4 C3 -98.9(6) . . . . ? C17 C22 C21 C20 0.2(8) . . . . ? N6 C20 C21 C22 -179.0(5) . . . . ? C19 C20 C21 C22 0.4(8) . . . . ? C12 C14 C15 N4 160(10) . . . . ? N5 C14 C15 N4 -19(10) . . . . ? C20 N6 C23 C24 74.6(8) . . . . ? C25 N6 C23 C24 -95.5(7) . . . . ? O2 C18 C19 C20 179.4(5) . . . . ? C17 C18 C19 C20 0.1(9) . . . . ? N6 C20 C19 C18 178.8(5) . . . . ? C21 C20 C19 C18 -0.6(8) . . . . ? C4 N1 C5 C6 -170.6(5) . . . . ? C2 N1 C5 C6 -2.8(8) . . . . ? C4 N1 C5 C10 11.4(8) . . . . ? C2 N1 C5 C10 179.1(5) . . . . ? C7 C6 C5 N1 -178.5(5) . . . . ? C7 C6 C5 C10 -0.4(8) . . . . ? C9 C10 C5 N1 179.9(5) . . . . ? C9 C10 C5 C6 1.7(8) . . . . ? C5 N1 C2 C1 -84.9(7) . . . . ? C4 N1 C2 C1 83.3(6) . . . . ? C20 N6 C25 C26 -76.7(7) . . . . ? C23 N6 C25 C26 93.7(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N2 0.82 1.94 2.668(6) 147 . O2 H2 N5 0.82 1.85 2.579(6) 147 . #===END #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary _ccdc_compound_id 1.(CH3CH2)2O # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _ccdc_temp_data_collection 100(2) _ccdc_ls_R_squared 0.0362 _ccdc_disorder ; The diethyl amino arm containing atoms C3 and C4 are disordered between 2 sites, site "a" with 72.6 % and site "b" with 27.4 % occupancies. The diethyl ether solvent of crystallisation is disordered over three sites, site "S" with 50 % occupancy and sites "T" and "U" each with 25 % occupancies. ; #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ data_bcas072a _database_code_depnum_ccdc_archive 'CCDC 802705' #TrackingRef '- salmntall.cif' _audit_creation_date 2009-08-11T13:48:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; '[UO2(salmnt(Et2N)2)(H2O)].(CH3CH2)2O' ; _chemical_formula_sum 'C30 H40 N6 O6 U' _chemical_formula_weight 818.71 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.599(5) _cell_length_b 11.889(5) _cell_length_c 20.758(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 107.496(5) _cell_angle_gamma 90.000(5) _cell_volume 3200.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 920 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 23.36 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4657 _exptl_absorpt_correction_T_max 0.6640 _exptl_absorpt_process_details SADABS #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_unetI/netI 0.0504 _diffrn_reflns_number 25120 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.6 _diffrn_reflns_theta_max 26.41 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 6544 _reflns_number_gt 5173 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0349P)^2^+5.7998P] 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_number_reflns 6544 _refine_ls_number_parameters 494 _refine_ls_number_restraints 255 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.237 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.143 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.307102(15) 0.552351(16) 0.526959(11) 0.01751(7) Uani 1 1 d . . . O1 O 0.3641(3) 0.4272(3) 0.56897(19) 0.0210(9) Uani 1 1 d . . . O2 O 0.2557(3) 0.6799(3) 0.48552(19) 0.0231(9) Uani 1 1 d . . . O3 O 0.1694(3) 0.4616(3) 0.46098(19) 0.0222(9) Uani 1 1 d . . . O4 O 0.4697(3) 0.6244(3) 0.5587(2) 0.0209(9) Uani 1 1 d . . . O5 O 0.3690(3) 0.5058(3) 0.4321(2) 0.0234(9) Uani 1 1 d . . . N1 N -0.0518(4) 0.1630(4) 0.3533(2) 0.0295(12) Uani 1 1 d . . . N2 N 0.1779(3) 0.5144(4) 0.5946(2) 0.0187(10) Uani 1 1 d . . . N3 N 0.1040(4) 0.5180(4) 0.7433(2) 0.0270(12) Uani 1 1 d . . . N4 N 0.3102(4) 0.7574(4) 0.7878(3) 0.0328(13) Uani 1 1 d . . . N5 N 0.3352(3) 0.6746(4) 0.6324(2) 0.0176(10) Uani 1 1 d . . . N6 N 0.6755(3) 0.9215(4) 0.5159(2) 0.0212(11) Uani 1 1 d . . . C1 C -0.0908(5) -0.0274(5) 0.3890(3) 0.0306(15) Uani 1 1 d . . . H1A H -0.1469 -0.0782 0.386 0.046 Uiso 1 1 calc R A . H1B H -0.057 -0.0098 0.4356 0.046 Uiso 1 1 calc R . . H1C H -0.0424 -0.0619 0.3697 0.046 Uiso 1 1 calc R . . C2 C -0.1317(4) 0.0789(5) 0.3511(3) 0.0269(14) Uani 1 1 d . A . H2A H -0.1666 0.0601 0.3044 0.032 Uiso 1 1 calc R . . H2B H -0.1822 0.1118 0.37 0.032 Uiso 1 1 calc R . . C3 C -0.0318(11) 0.1995(11) 0.2447(6) 0.076(3) Uani 0.726(13) 1 d PDU A 1 H3A H 0.0128 0.182 0.218 0.114 Uiso 0.726(13) 1 calc PR A 1 H3B H -0.0336 0.2794 0.2507 0.114 Uiso 0.726(13) 1 calc PR A 1 H3C H -0.1001 0.1726 0.2222 0.114 Uiso 0.726(13) 1 calc PR A 1 C3B C 0.054(3) 0.100(3) 0.2706(17) 0.073(5) Uani 0.274(13) 1 d PDU A 2 H3B1 H 0.0187 0.0315 0.2524 0.109 Uiso 0.274(13) 1 calc PR A 2 H3B2 H 0.1211 0.0822 0.3002 0.109 Uiso 0.274(13) 1 calc PR A 2 H3B3 H 0.0601 0.1467 0.2344 0.109 Uiso 0.274(13) 1 calc PR A 2 C4 C 0.0028(8) 0.1512(8) 0.3034(4) 0.068(2) Uani 0.726(13) 1 d PDU A 1 H4A H 0.0725 0.1783 0.324 0.081 Uiso 0.726(13) 1 calc PR A 1 H4B H 0.0079 0.0713 0.2954 0.081 Uiso 0.726(13) 1 calc PR A 1 C4B C 0.0028(8) 0.1512(8) 0.3034(4) 0.068(2) Uani 0.274(13) 1 d PD A 2 H4C H -0.051 0.1803 0.265 0.081 Uiso 0.274(13) 1 calc PR A 2 H4D H 0.0491 0.2146 0.3178 0.081 Uiso 0.274(13) 1 calc PR A 2 C5 C -0.0144(4) 0.2328(5) 0.4067(3) 0.0208(12) Uani 1 1 d . A . C6 C -0.0515(4) 0.2268(5) 0.4641(3) 0.0217(12) Uani 1 1 d . . . H6 H -0.1034 0.176 0.4643 0.026 Uiso 1 1 calc R A . C7 C -0.0115(4) 0.2949(5) 0.5184(3) 0.0220(12) Uani 1 1 d . A . H7 H -0.0374 0.2893 0.555 0.026 Uiso 1 1 calc R . . C8 C 0.0676(4) 0.3735(4) 0.5216(3) 0.0174(11) Uani 1 1 d . . . C9 C 0.1014(4) 0.3852(5) 0.4632(3) 0.0184(12) Uani 1 1 d . A . C10 C 0.0609(4) 0.3145(4) 0.4077(3) 0.0190(12) Uani 1 1 d . . . H10 H 0.0845 0.3217 0.3703 0.023 Uiso 1 1 calc R A . C11 C 0.1039(4) 0.4386(5) 0.5806(3) 0.0187(11) Uani 1 1 d . A . H11 H 0.0718 0.4267 0.6137 0.022 Uiso 1 1 calc R . . C12 C 0.2001(4) 0.5696(4) 0.6570(3) 0.0182(12) Uani 1 1 d . . . C13 C 0.1453(4) 0.5422(5) 0.7050(3) 0.0210(12) Uani 1 1 d . . . C14 C 0.2750(4) 0.6495(5) 0.6742(3) 0.0199(12) Uani 1 1 d . . . C15 C 0.2937(4) 0.7081(5) 0.7378(3) 0.0228(13) Uani 1 1 d . . . C16 C 0.3917(4) 0.7685(4) 0.6445(3) 0.0179(11) Uani 1 1 d . . . H16 H 0.3847 0.8152 0.6787 0.022 Uiso 1 1 calc R . . C17 C 0.4611(4) 0.8030(5) 0.6098(3) 0.0203(12) Uani 1 1 d . . . C18 C 0.4996(4) 0.9138(4) 0.6191(3) 0.0195(12) Uani 1 1 d . . . H18 H 0.4776 0.9612 0.6477 0.023 Uiso 1 1 calc R . . C19 C 0.5674(4) 0.9549(5) 0.5885(3) 0.0222(12) Uani 1 1 d . . . H19 H 0.5892 1.0293 0.5955 0.027 Uiso 1 1 calc R . . C20 C 0.6052(4) 0.8843(5) 0.5456(3) 0.0194(12) Uani 1 1 d . . . C21 C 0.5682(4) 0.7730(5) 0.5365(3) 0.0208(12) Uani 1 1 d . . . H21 H 0.5921 0.7253 0.5089 0.025 Uiso 1 1 calc R . . C22 C 0.4985(4) 0.7321(5) 0.5665(3) 0.0188(12) Uani 1 1 d . . . C23 C 0.7259(4) 0.8444(5) 0.4806(3) 0.0244(13) Uani 1 1 d . . . H23A H 0.7302 0.7704 0.5009 0.029 Uiso 1 1 calc R . . H23B H 0.7956 0.8704 0.4864 0.029 Uiso 1 1 calc R . . C24 C 0.6690(5) 0.8353(5) 0.4055(3) 0.0304(14) Uani 1 1 d . . . H24A H 0.7047 0.7838 0.3849 0.046 Uiso 1 1 calc R . . H24B H 0.666 0.908 0.3849 0.046 Uiso 1 1 calc R . . H24C H 0.6002 0.8084 0.3995 0.046 Uiso 1 1 calc R . . C35 C 0.7092(4) 1.0386(5) 0.5201(3) 0.0262(13) Uani 1 1 d . . . H35A H 0.6531 1.0868 0.5228 0.031 Uiso 1 1 calc R . . H35B H 0.7261 1.058 0.4793 0.031 Uiso 1 1 calc R . . C36 C 0.8031(5) 1.0604(5) 0.5812(3) 0.0353(15) Uani 1 1 d . . . H36A H 0.8221 1.1383 0.5822 0.053 Uiso 1 1 calc R . . H36B H 0.8596 1.0145 0.5781 0.053 Uiso 1 1 calc R . . H36C H 0.7866 1.042 0.6218 0.053 Uiso 1 1 calc R . . C1S C 0.3879(12) 0.4294(15) 0.2809(9) 0.058(5) Uani 0.5 1 d PD B 1 H1S1 H 0.4362 0.4723 0.3154 0.087 Uiso 0.5 1 calc PR B 1 H1S2 H 0.4164 0.4149 0.2446 0.087 Uiso 0.5 1 calc PR B 1 H1S3 H 0.3741 0.3593 0.2995 0.087 Uiso 0.5 1 calc PR B 1 O1S O 0.2559(9) 0.5368(10) 0.3045(7) 0.062(2) Uani 0.5 1 d PDU B 1 C2S C 0.2895(13) 0.4944(17) 0.2546(7) 0.069(3) Uani 0.5 1 d PDU B 1 H2S1 H 0.3003 0.5557 0.2266 0.083 Uiso 0.5 1 calc PR B 1 H2S2 H 0.2368 0.4456 0.2264 0.083 Uiso 0.5 1 calc PR B 1 C3S C 0.1989(13) 0.6332(15) 0.2848(9) 0.070(2) Uani 0.5 1 d PDU B 1 H3S1 H 0.1678 0.6323 0.2362 0.084 Uiso 0.5 1 calc PR B 1 H3S2 H 0.2442 0.698 0.2961 0.084 Uiso 0.5 1 calc PR B 1 C4S C 0.1164(11) 0.6442(16) 0.3181(8) 0.059(3) Uani 0.5 1 d PDU B 1 H4S1 H 0.0627 0.5908 0.2987 0.088 Uiso 0.5 1 calc PR B 1 H4S2 H 0.0886 0.719 0.3113 0.088 Uiso 0.5 1 calc PR B 1 H4S3 H 0.1449 0.6299 0.3656 0.088 Uiso 0.5 1 calc PR B 1 O1T O 0.2375(15) 0.4213(19) 0.3171(9) 0.060(3) Uani 0.25 1 d PDU C 2 C1T C 0.369(2) 0.375(3) 0.2691(19) 0.061(5) Uani 0.25 1 d PDU C 2 H1S4 H 0.4185 0.4053 0.3084 0.092 Uiso 0.25 1 calc PR C 2 H1S5 H 0.3493 0.4319 0.2347 0.092 Uiso 0.25 1 calc PR C 2 H1S6 H 0.3982 0.3121 0.2525 0.092 Uiso 0.25 1 calc PR C 2 C2T C 0.2742(19) 0.337(2) 0.2875(13) 0.058(3) Uani 0.25 1 d PDU C 2 H2T1 H 0.2213 0.3127 0.2471 0.07 Uiso 0.25 1 calc PR C 2 H2T2 H 0.2921 0.2733 0.3181 0.07 Uiso 0.25 1 calc PR C 2 C3T C 0.165(2) 0.485(3) 0.2724(13) 0.060(3) Uani 0.25 1 d PDU C 2 H3T1 H 0.1041 0.4407 0.2525 0.072 Uiso 0.25 1 calc PR C 2 H3T2 H 0.192 0.5102 0.2364 0.072 Uiso 0.25 1 calc PR C 2 C4T C 0.137(3) 0.587(2) 0.3074(17) 0.060(3) Uani 0.25 1 d PDU C 2 H4T1 H 0.0909 0.5642 0.3319 0.089 Uiso 0.25 1 calc PR C 2 H4T2 H 0.1046 0.6422 0.2743 0.089 Uiso 0.25 1 calc PR C 2 H4T3 H 0.1987 0.6179 0.3381 0.089 Uiso 0.25 1 calc PR C 2 C2U C 0.1729(18) 0.536(2) 0.2825(18) 0.063(2) Uani 0.25 1 d PDU D 3 H2U1 H 0.1331 0.5757 0.2424 0.076 Uiso 0.25 1 calc PR D 3 H2U2 H 0.1377 0.5412 0.3167 0.076 Uiso 0.25 1 calc PR D 3 O1U O 0.2742(17) 0.5802(19) 0.3069(15) 0.066(2) Uani 0.25 1 d PDU D 3 C1U C 0.187(2) 0.414(2) 0.2662(14) 0.055(3) Uani 0.25 1 d PDU D 3 H1U1 H 0.1896 0.408 0.2205 0.083 Uiso 0.25 1 calc PR D 3 H1U2 H 0.1311 0.3699 0.2714 0.083 Uiso 0.25 1 calc PR D 3 H1U3 H 0.251 0.3862 0.2965 0.083 Uiso 0.25 1 calc PR D 3 C3U C 0.269(2) 0.694(2) 0.3167(18) 0.076(3) Uani 0.25 1 d PDU D 3 H3U1 H 0.2199 0.7086 0.3415 0.091 Uiso 0.25 1 calc PR D 3 H3U2 H 0.2442 0.7313 0.2733 0.091 Uiso 0.25 1 calc PR D 3 C4U C 0.373(3) 0.740(3) 0.356(2) 0.117(5) Uani 0.25 1 d PDU D 3 H4U1 H 0.4259 0.6971 0.3447 0.176 Uiso 0.25 1 calc PR D 3 H4U2 H 0.382 0.7343 0.4031 0.176 Uiso 0.25 1 calc PR D 3 H4U3 H 0.3777 0.8171 0.3435 0.176 Uiso 0.25 1 calc PRU D 3 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 0.01526(11) 0.01508(10) 0.02474(12) 0.00115(10) 0.00985(8) -0.00065(9) O1 0.024(2) 0.016(2) 0.026(2) -0.0004(16) 0.0118(17) 0.0005(16) O2 0.020(2) 0.024(2) 0.029(2) 0.0006(18) 0.0124(17) 0.0014(17) O3 0.023(2) 0.021(2) 0.026(2) 0.0010(17) 0.0131(17) -0.0058(16) O4 0.0176(19) 0.016(2) 0.033(2) 0.0004(17) 0.0136(17) 0.0003(16) O5 0.021(2) 0.027(2) 0.026(2) 0.0016(17) 0.0125(17) 0.0016(17) N1 0.038(3) 0.025(3) 0.032(3) -0.007(2) 0.019(2) -0.010(2) N2 0.017(2) 0.019(2) 0.021(3) 0.0035(19) 0.008(2) 0.0006(19) N3 0.029(3) 0.032(3) 0.022(3) -0.002(2) 0.011(2) -0.006(2) N4 0.042(3) 0.031(3) 0.029(3) -0.001(3) 0.016(3) -0.014(3) N5 0.015(2) 0.018(2) 0.022(2) 0.003(2) 0.0092(19) 0.0026(18) N6 0.019(2) 0.018(3) 0.028(3) 0.005(2) 0.008(2) -0.0007(19) C1 0.027(3) 0.024(3) 0.038(4) -0.003(3) 0.006(3) -0.010(3) C2 0.019(3) 0.028(3) 0.034(3) -0.006(3) 0.007(3) -0.006(2) C3 0.089(7) 0.066(7) 0.069(6) -0.010(5) 0.017(6) -0.003(6) C3B 0.098(9) 0.067(8) 0.059(8) -0.014(8) 0.033(8) -0.013(8) C4 0.100(6) 0.067(5) 0.048(4) -0.026(4) 0.040(5) -0.044(5) C4B 0.100(6) 0.067(5) 0.048(4) -0.026(4) 0.040(5) -0.044(5) C5 0.021(3) 0.017(3) 0.025(3) 0.001(2) 0.008(2) 0.003(2) C6 0.021(3) 0.018(3) 0.027(3) 0.004(2) 0.007(2) 0.000(2) C7 0.019(3) 0.022(3) 0.028(3) 0.006(2) 0.012(2) 0.001(2) C8 0.014(3) 0.016(3) 0.022(3) 0.004(2) 0.006(2) 0.002(2) C9 0.011(3) 0.019(3) 0.025(3) 0.006(2) 0.006(2) 0.004(2) C10 0.017(3) 0.022(3) 0.021(3) 0.002(2) 0.011(2) 0.004(2) C11 0.016(3) 0.020(3) 0.022(3) 0.007(2) 0.009(2) 0.002(2) C12 0.018(3) 0.015(3) 0.023(3) 0.003(2) 0.010(2) 0.004(2) C13 0.023(3) 0.018(3) 0.022(3) -0.003(2) 0.006(2) 0.001(2) C14 0.021(3) 0.016(3) 0.022(3) 0.000(2) 0.006(2) 0.001(2) C15 0.021(3) 0.021(3) 0.028(3) 0.004(3) 0.010(3) -0.003(2) C16 0.016(3) 0.018(3) 0.020(3) 0.001(2) 0.004(2) 0.004(2) C17 0.022(3) 0.021(3) 0.017(3) 0.001(2) 0.004(2) 0.000(2) C18 0.016(3) 0.016(3) 0.023(3) -0.003(2) 0.001(2) 0.002(2) C19 0.021(3) 0.020(3) 0.026(3) 0.000(3) 0.007(2) 0.000(2) C20 0.016(3) 0.021(3) 0.020(3) 0.006(2) 0.003(2) 0.001(2) C21 0.021(3) 0.020(3) 0.024(3) 0.002(2) 0.010(2) 0.000(2) C22 0.016(3) 0.017(3) 0.023(3) 0.000(2) 0.004(2) 0.001(2) C23 0.016(3) 0.022(3) 0.038(4) 0.008(3) 0.012(3) 0.001(2) C24 0.029(3) 0.028(3) 0.038(4) 0.007(3) 0.017(3) 0.005(3) C35 0.025(3) 0.021(3) 0.033(3) 0.011(3) 0.010(3) -0.001(3) C36 0.026(3) 0.026(3) 0.049(4) 0.002(3) 0.003(3) -0.008(3) C1S 0.067(12) 0.065(13) 0.044(11) 0.003(10) 0.018(9) 0.009(10) O1S 0.056(4) 0.098(6) 0.037(3) 0.023(4) 0.020(3) 0.022(4) C2S 0.064(5) 0.103(7) 0.042(4) 0.020(5) 0.019(4) 0.021(5) C3S 0.064(4) 0.100(6) 0.047(4) 0.021(4) 0.017(3) 0.022(4) C4S 0.043(6) 0.081(8) 0.050(6) 0.007(7) 0.013(5) 0.006(6) O1T 0.054(5) 0.096(6) 0.033(4) 0.023(5) 0.020(4) 0.019(5) C1T 0.057(9) 0.097(12) 0.033(10) 0.015(10) 0.018(8) 0.021(9) C2T 0.055(6) 0.094(7) 0.027(6) 0.021(6) 0.016(5) 0.019(5) C3T 0.054(5) 0.097(6) 0.035(4) 0.025(5) 0.019(4) 0.018(5) C4T 0.047(6) 0.090(7) 0.044(6) 0.023(6) 0.017(5) 0.011(6) C2U 0.057(4) 0.098(6) 0.038(4) 0.023(5) 0.020(4) 0.019(4) O1U 0.061(4) 0.099(6) 0.042(4) 0.021(5) 0.019(4) 0.022(4) C1U 0.051(6) 0.098(7) 0.026(6) 0.023(6) 0.025(5) 0.019(6) C3U 0.071(5) 0.101(6) 0.054(5) 0.019(5) 0.018(4) 0.020(5) C4U 0.104(7) 0.125(7) 0.118(8) 0.003(7) 0.025(7) -0.008(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O2 1.780(4) . ? U1 O1 1.780(4) . ? U1 O3 2.237(4) . ? U1 O4 2.276(4) . ? U1 O5 2.427(4) . ? U1 N5 2.559(4) . ? U1 N2 2.597(4) . ? O3 C9 1.307(6) . ? O4 C22 1.335(6) . ? N1 C5 1.356(7) . ? N1 C4 1.451(9) . ? N1 C2 1.467(7) . ? N2 C11 1.316(7) . ? N2 C12 1.401(7) . ? N3 C13 1.138(7) . ? N4 C15 1.155(7) . ? N5 C16 1.336(7) . ? N5 C14 1.392(7) . ? N6 C20 1.357(7) . ? N6 C35 1.460(7) . ? N6 C23 1.466(7) . ? C1 C2 1.504(8) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.300(13) . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C3B H3B1 0.96 . ? C3B H3B2 0.96 . ? C3B H3B3 0.96 . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C10 1.407(7) . ? C5 C6 1.427(8) . ? C6 C7 1.362(8) . ? C6 H6 0.93 . ? C7 C8 1.411(7) . ? C7 H7 0.93 . ? C8 C11 1.406(7) . ? C8 C9 1.427(7) . ? C9 C10 1.398(7) . ? C10 H10 0.93 . ? C11 H11 0.93 . ? C12 C14 1.360(7) . ? C12 C13 1.451(8) . ? C14 C15 1.445(8) . ? C16 C17 1.408(7) . ? C16 H16 0.93 . ? C17 C18 1.410(7) . ? C17 C22 1.432(7) . ? C18 C19 1.358(8) . ? C18 H18 0.93 . ? C19 C20 1.428(8) . ? C19 H19 0.93 . ? C20 C21 1.407(8) . ? C21 C22 1.372(7) . ? C21 H21 0.93 . ? C23 C24 1.521(8) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C35 C36 1.527(8) . ? C35 H35A 0.97 . ? C35 H35B 0.97 . ? C36 H36A 0.96 . ? C36 H36B 0.96 . ? C36 H36C 0.96 . ? C1S C2S 1.499(17) . ? C1S H1S1 0.96 . ? C1S H1S2 0.96 . ? C1S H1S3 0.96 . ? O1S C2S 1.350(14) . ? O1S C3S 1.376(14) . ? C2S H2S1 0.97 . ? C2S H2S2 0.97 . ? C3S C4S 1.489(17) . ? C3S H3S1 0.97 . ? C3S H3S2 0.97 . ? C4S H4S1 0.96 . ? C4S H4S2 0.96 . ? C4S H4S3 0.96 . ? O1T C2T 1.349(17) . ? O1T C3T 1.364(17) . ? C1T C2T 1.52(2) . ? C1T H1S4 0.96 . ? C1T H1S5 0.96 . ? C1T H1S6 0.96 . ? C2T H2T1 0.97 . ? C2T H2T2 0.97 . ? C3T C4T 1.51(2) . ? C3T H3T1 0.97 . ? C3T H3T2 0.97 . ? C4T H4T1 0.96 . ? C4T H4T2 0.96 . ? C4T H4T3 0.96 . ? C2U O1U 1.419(17) . ? C2U C1U 1.51(2) . ? C2U H2U1 0.97 . ? C2U H2U2 0.97 . ? O1U C3U 1.371(17) . ? C1U H1U1 0.96 . ? C1U H1U2 0.96 . ? C1U H1U3 0.96 . ? C3U C4U 1.51(2) . ? C3U H3U1 0.97 . ? C3U H3U2 0.97 . ? C4U H4U1 0.96 . ? C4U H4U2 0.96 . ? C4U H4U3 0.96 . ? 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 O2 U1 O1 177.46(17) . . ? O2 U1 O3 88.85(16) . . ? O1 U1 O3 93.34(16) . . ? O2 U1 O4 91.47(15) . . ? O1 U1 O4 86.01(15) . . ? O3 U1 O4 156.97(13) . . ? O2 U1 O5 89.09(15) . . ? O1 U1 O5 90.03(15) . . ? O3 U1 O5 79.85(13) . . ? O4 U1 O5 77.12(13) . . ? O2 U1 N5 82.26(16) . . ? O1 U1 N5 97.15(16) . . ? O3 U1 N5 132.82(13) . . ? O4 U1 N5 69.92(13) . . ? O5 U1 N5 145.59(13) . . ? O2 U1 N2 100.24(15) . . ? O1 U1 N2 81.72(16) . . ? O3 U1 N2 70.68(14) . . ? O4 U1 N2 131.69(14) . . ? O5 U1 N2 148.76(14) . . ? N5 U1 N2 65.63(14) . . ? C9 O3 U1 141.7(3) . . ? C22 O4 U1 128.3(3) . . ? C5 N1 C4 119.8(5) . . ? C5 N1 C2 122.2(5) . . ? C4 N1 C2 116.5(5) . . ? C11 N2 C12 117.6(5) . . ? C11 N2 U1 126.6(4) . . ? C12 N2 U1 115.1(3) . . ? C16 N5 C14 118.4(5) . . ? C16 N5 U1 124.3(3) . . ? C14 N5 U1 116.6(3) . . ? C20 N6 C35 122.4(5) . . ? C20 N6 C23 121.4(5) . . ? C35 N6 C23 116.1(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 113.8(5) . . ? N1 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? N1 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C3 C4 N1 120.5(11) . . ? C3 C4 H4A 107.2 . . ? N1 C4 H4A 107.2 . . ? C3 C4 H4B 107.2 . . ? N1 C4 H4B 107.2 . . ? H4A C4 H4B 106.8 . . ? N1 C5 C10 121.8(5) . . ? N1 C5 C6 120.8(5) . . ? C10 C5 C6 117.4(5) . . ? C7 C6 C5 120.5(5) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 122.8(5) . . ? C6 C7 H7 118.6 . . ? C8 C7 H7 118.6 . . ? C11 C8 C7 118.0(5) . . ? C11 C8 C9 124.6(5) . . ? C7 C8 C9 117.4(5) . . ? O3 C9 C10 119.8(5) . . ? O3 C9 C8 120.6(5) . . ? C10 C9 C8 119.6(5) . . ? C9 C10 C5 122.2(5) . . ? C9 C10 H10 118.9 . . ? C5 C10 H10 118.9 . . ? N2 C11 C8 127.9(5) . . ? N2 C11 H11 116 . . ? C8 C11 H11 116 . . ? C14 C12 N2 120.5(5) . . ? C14 C12 C13 118.3(5) . . ? N2 C12 C13 121.2(5) . . ? N3 C13 C12 178.0(6) . . ? C12 C14 N5 121.3(5) . . ? C12 C14 C15 119.3(5) . . ? N5 C14 C15 119.4(5) . . ? N4 C15 C14 177.9(6) . . ? N5 C16 C17 125.7(5) . . ? N5 C16 H16 117.1 . . ? C17 C16 H16 117.1 . . ? C16 C17 C18 118.7(5) . . ? C16 C17 C22 124.6(5) . . ? C18 C17 C22 116.6(5) . . ? C19 C18 C17 123.2(5) . . ? C19 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? C18 C19 C20 120.2(5) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? N6 C20 C21 121.1(5) . . ? N6 C20 C19 121.7(5) . . ? C21 C20 C19 117.1(5) . . ? C22 C21 C20 122.6(5) . . ? C22 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? O4 C22 C21 120.2(5) . . ? O4 C22 C17 119.6(5) . . ? C21 C22 C17 120.1(5) . . ? N6 C23 C24 112.7(5) . . ? N6 C23 H23A 109 . . ? C24 C23 H23A 109 . . ? N6 C23 H23B 109 . . ? C24 C23 H23B 109 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N6 C35 C36 112.4(5) . . ? N6 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? N6 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C2S O1S C3S 111.9(13) . . ? O1S C2S C1S 112.5(12) . . ? O1S C2S H2S1 109.1 . . ? C1S C2S H2S1 109.1 . . ? O1S C2S H2S2 109.1 . . ? C1S C2S H2S2 109.1 . . ? H2S1 C2S H2S2 107.8 . . ? O1S C3S C4S 111.8(13) . . ? O1S C3S H3S1 109.3 . . ? C4S C3S H3S1 109.3 . . ? O1S C3S H3S2 109.3 . . ? C4S C3S H3S2 109.3 . . ? H3S1 C3S H3S2 107.9 . . ? C2T O1T C3T 113.3(17) . . ? C2T C1T H1S4 109.5 . . ? C2T C1T H1S5 109.5 . . ? H1S4 C1T H1S5 109.5 . . ? C2T C1T H1S6 109.5 . . ? H1S4 C1T H1S6 109.5 . . ? H1S5 C1T H1S6 109.5 . . ? O1T C2T C1T 110.5(17) . . ? O1T C2T H2T1 109.6 . . ? C1T C2T H2T1 109.6 . . ? O1T C2T H2T2 109.6 . . ? C1T C2T H2T2 109.6 . . ? H2T1 C2T H2T2 108.1 . . ? O1T C3T C4T 110.6(17) . . ? O1T C3T H3T1 109.5 . . ? C4T C3T H3T1 109.5 . . ? O1T C3T H3T2 109.5 . . ? C4T C3T H3T2 109.5 . . ? H3T1 C3T H3T2 108.1 . . ? C3T C4T H4T1 109.5 . . ? C3T C4T H4T2 109.5 . . ? H4T1 C4T H4T2 109.5 . . ? C3T C4T H4T3 109.5 . . ? H4T1 C4T H4T3 109.5 . . ? H4T2 C4T H4T3 109.5 . . ? O1U C2U C1U 105.0(15) . . ? O1U C2U H2U1 110.8 . . ? C1U C2U H2U1 110.8 . . ? O1U C2U H2U2 110.8 . . ? C1U C2U H2U2 110.8 . . ? H2U1 C2U H2U2 108.8 . . ? C3U O1U C2U 109.3(17) . . ? O1U C3U C4U 110.6(17) . . ? O1U C3U H3U1 109.5 . . ? C4U C3U H3U1 109.5 . . ? O1U C3U H3U2 109.5 . . ? C4U C3U H3U2 109.5 . . ? H3U1 C3U H3U2 108.1 . . ? 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 O2 U1 O3 C9 -136.0(6) . . . . ? O1 U1 O3 C9 45.3(6) . . . . ? O4 U1 O3 C9 132.9(5) . . . . ? O5 U1 O3 C9 134.7(6) . . . . ? N5 U1 O3 C9 -57.7(6) . . . . ? N2 U1 O3 C9 -34.7(5) . . . . ? O2 U1 O4 C22 24.0(4) . . . . ? O1 U1 O4 C22 -156.3(4) . . . . ? O3 U1 O4 C22 114.5(5) . . . . ? O5 U1 O4 C22 112.7(4) . . . . ? N5 U1 O4 C22 -57.2(4) . . . . ? N2 U1 O4 C22 -81.1(5) . . . . ? O2 U1 N2 C11 105.2(4) . . . . ? O1 U1 N2 C11 -76.4(4) . . . . ? O3 U1 N2 C11 20.1(4) . . . . ? O4 U1 N2 C11 -153.5(4) . . . . ? O5 U1 N2 C11 -0.2(6) . . . . ? N5 U1 N2 C11 -178.2(5) . . . . ? O2 U1 N2 C12 -84.6(4) . . . . ? O1 U1 N2 C12 93.7(4) . . . . ? O3 U1 N2 C12 -169.7(4) . . . . ? O4 U1 N2 C12 16.7(4) . . . . ? O5 U1 N2 C12 169.9(3) . . . . ? N5 U1 N2 C12 -8.0(3) . . . . ? O2 U1 N5 C16 -58.7(4) . . . . ? O1 U1 N5 C16 118.8(4) . . . . ? O3 U1 N5 C16 -139.9(4) . . . . ? O4 U1 N5 C16 35.8(4) . . . . ? O5 U1 N5 C16 18.2(5) . . . . ? N2 U1 N5 C16 -163.7(4) . . . . ? O2 U1 N5 C14 111.5(4) . . . . ? O1 U1 N5 C14 -71.0(4) . . . . ? O3 U1 N5 C14 30.3(4) . . . . ? O4 U1 N5 C14 -154.1(4) . . . . ? O5 U1 N5 C14 -171.6(3) . . . . ? N2 U1 N5 C14 6.5(3) . . . . ? C5 N1 C2 C1 -81.3(7) . . . . ? C4 N1 C2 C1 84.7(8) . . . . ? C5 N1 C4 C3 -104.4(10) . . . . ? C2 N1 C4 C3 89.3(11) . . . . ? C4 N1 C5 C10 15.6(9) . . . . ? C2 N1 C5 C10 -178.9(5) . . . . ? C4 N1 C5 C6 -165.2(7) . . . . ? C2 N1 C5 C6 0.3(8) . . . . ? N1 C5 C6 C7 178.0(5) . . . . ? C10 C5 C6 C7 -2.7(8) . . . . ? C5 C6 C7 C8 -0.3(8) . . . . ? C6 C7 C8 C11 -179.3(5) . . . . ? C6 C7 C8 C9 3.8(8) . . . . ? U1 O3 C9 C10 -147.6(4) . . . . ? U1 O3 C9 C8 32.8(8) . . . . ? C11 C8 C9 O3 -1.3(8) . . . . ? C7 C8 C9 O3 175.3(5) . . . . ? C11 C8 C9 C10 179.1(5) . . . . ? C7 C8 C9 C10 -4.2(7) . . . . ? O3 C9 C10 C5 -178.3(5) . . . . ? C8 C9 C10 C5 1.3(8) . . . . ? N1 C5 C10 C9 -178.6(5) . . . . ? C6 C5 C10 C9 2.2(8) . . . . ? C12 N2 C11 C8 179.5(5) . . . . ? U1 N2 C11 C8 -10.5(8) . . . . ? C7 C8 C11 N2 178.5(5) . . . . ? C9 C8 C11 N2 -4.8(9) . . . . ? C11 N2 C12 C14 -179.4(5) . . . . ? U1 N2 C12 C14 9.5(6) . . . . ? C11 N2 C12 C13 1.4(7) . . . . ? U1 N2 C12 C13 -169.7(4) . . . . ? C14 C12 C13 N3 -100(18) . . . . ? N2 C12 C13 N3 79(18) . . . . ? N2 C12 C14 N5 -3.4(8) . . . . ? C13 C12 C14 N5 175.8(5) . . . . ? N2 C12 C14 C15 177.7(5) . . . . ? C13 C12 C14 C15 -3.1(8) . . . . ? C16 N5 C14 C12 166.1(5) . . . . ? U1 N5 C14 C12 -4.7(6) . . . . ? C16 N5 C14 C15 -15.0(7) . . . . ? U1 N5 C14 C15 174.2(4) . . . . ? C12 C14 C15 N4 -161(19) . . . . ? N5 C14 C15 N4 20(19) . . . . ? C14 N5 C16 C17 176.1(5) . . . . ? U1 N5 C16 C17 -13.9(7) . . . . ? N5 C16 C17 C18 167.7(5) . . . . ? N5 C16 C17 C22 -14.2(9) . . . . ? C16 C17 C18 C19 179.5(5) . . . . ? C22 C17 C18 C19 1.3(8) . . . . ? C17 C18 C19 C20 -1.6(8) . . . . ? C35 N6 C20 C21 175.1(5) . . . . ? C23 N6 C20 C21 -8.0(8) . . . . ? C35 N6 C20 C19 -6.4(8) . . . . ? C23 N6 C20 C19 170.4(5) . . . . ? C18 C19 C20 N6 -177.8(5) . . . . ? C18 C19 C20 C21 0.7(8) . . . . ? N6 C20 C21 C22 178.9(5) . . . . ? C19 C20 C21 C22 0.4(8) . . . . ? U1 O4 C22 C21 -129.8(5) . . . . ? U1 O4 C22 C17 53.9(7) . . . . ? C20 C21 C22 O4 -176.9(5) . . . . ? C20 C21 C22 C17 -0.7(8) . . . . ? C16 C17 C22 O4 -2.0(8) . . . . ? C18 C17 C22 O4 176.1(5) . . . . ? C16 C17 C22 C21 -178.2(5) . . . . ? C18 C17 C22 C21 -0.1(8) . . . . ? C20 N6 C23 C24 92.1(6) . . . . ? C35 N6 C23 C24 -90.9(6) . . . . ? C20 N6 C35 C36 90.1(6) . . . . ? C23 N6 C35 C36 -86.9(6) . . . . ? C3S O1S C2S C1S 152.0(17) . . . . ? C2S O1S C3S C4S 147.5(16) . . . . ? C3T O1T C2T C1T 91(3) . . . . ? C2T O1T C3T C4T -173(3) . . . . ? C1U C2U O1U C3U 174(3) . . . . ? C2U O1U C3U C4U 169(3) . . . . ? #===END #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary _ccdc_compound_id 2a # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _ccdc_temp_data_collection 100(2) _ccdc_ls_R_squared 0.0476 #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ data_bcas119p21na _database_code_depnum_ccdc_archive 'CCDC 802706' #TrackingRef '- salmntall.cif' _audit_creation_date 2010-08-24T12:42:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; [UO2(salmnt(Et2N)2)(py)] ; _chemical_formula_sum 'C62 H66 N14 O8 U2' _chemical_formula_weight 1611.35 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.524(5) _cell_length_b 27.818(5) _cell_length_c 19.211(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 91.028(5) _cell_angle_gamma 90.000(5) _cell_volume 6158(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5893 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.35 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.32 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.377650 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_unetI/netI 0.0755 _diffrn_reflns_number 43986 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.37 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 11235 _reflns_number_gt 8510 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0371P)^2^+8.3099P] 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_number_reflns 11235 _refine_ls_number_parameters 775 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.54 _refine_diff_density_min -1.727 _refine_diff_density_rms 0.166 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.80271(2) 0.189389(10) 0.763163(14) 0.01572(8) Uani 1 1 d . . . U2 U 0.29031(2) 0.053028(10) 0.748975(14) 0.01527(8) Uani 1 1 d . . . O4 O 0.6315(4) 0.20220(19) 0.8117(3) 0.0264(13) Uani 1 1 d . . . O6 O 0.3488(4) 0.04408(18) 0.8349(2) 0.0199(12) Uani 1 1 d . . . O7 O 0.4682(4) 0.04266(18) 0.7066(3) 0.0216(12) Uani 1 1 d . . . N2 N 0.9006(5) 0.1159(2) 0.7072(3) 0.0175(14) Uani 1 1 d . . . O2 O 0.7331(5) 0.19786(19) 0.6798(3) 0.0245(13) Uani 1 1 d . . . O5 O 0.2324(4) 0.05818(17) 0.6625(3) 0.0192(11) Uani 1 1 d . . . N1 N 1.2531(5) 0.2686(2) 0.5582(3) 0.0204(15) Uani 1 1 d . . . N14 N 0.2936(6) -0.0398(2) 0.7389(3) 0.0216(15) Uani 1 1 d . . . N13 N -0.1586(5) -0.0381(2) 0.9356(3) 0.0208(15) Uani 1 1 d . . . N12 N 0.1852(5) 0.1248(2) 0.8062(3) 0.0177(14) Uani 1 1 d . . . N8 N 0.7278(5) 0.0166(2) 0.5196(3) 0.0194(14) Uani 1 1 d . . . O8 O 0.1150(4) 0.03014(17) 0.7814(3) 0.0181(12) Uani 1 1 d . . . O3 O 0.9728(4) 0.21276(18) 0.7196(3) 0.0190(12) Uani 1 1 d . . . C14 C 0.7560(6) 0.0675(3) 0.7630(4) 0.0185(17) Uani 1 1 d . . . N4 N 0.6747(6) -0.0176(2) 0.7878(4) 0.0269(16) Uani 1 1 d . . . C47 C 0.0987(6) 0.1221(3) 0.8506(4) 0.0154(16) Uani 1 1 d . . . H47 H 0.0778 0.1505 0.8724 0.018 Uiso 1 1 calc R . . N7 N 0.7863(5) 0.2806(2) 0.7882(3) 0.0235(16) Uani 1 1 d . . . N5 N 0.7046(5) 0.1080(2) 0.7922(3) 0.0194(14) Uani 1 1 d . . . N9 N 0.3793(5) 0.1369(2) 0.7240(3) 0.0173(9) Uani 1 1 d U . . C48 C 0.0348(6) 0.0807(2) 0.8683(4) 0.0146(16) Uani 1 1 d . . . C35 C 0.7401(6) -0.0338(3) 0.5368(4) 0.0215(18) Uani 1 1 d . . . H35A H 0.7391 -0.0373 0.587 0.026 Uiso 1 1 calc R . . H35B H 0.815 -0.0449 0.5211 0.026 Uiso 1 1 calc R . . C43 C 0.3273(6) 0.1761(3) 0.7538(4) 0.0150(16) Uani 1 1 d . . . C46 C 0.1824(6) 0.2122(3) 0.8274(4) 0.0174(17) Uani 1 1 d . . . C4 C 1.2642(7) 0.3158(3) 0.5906(4) 0.0276(19) Uani 1 1 d . . . H4A H 1.3422 0.3277 0.5837 0.033 Uiso 1 1 calc R . . H4B H 1.2532 0.3125 0.6403 0.033 Uiso 1 1 calc R . . C39 C 0.5261(6) 0.1104(3) 0.6402(4) 0.0171(10) Uani 1 1 d U . . C61 C 0.1993(7) -0.1148(3) 0.7158(4) 0.027(2) Uani 1 1 d . . . H61 H 0.1329 -0.1312 0.7014 0.033 Uiso 1 1 calc R . . C5 C 1.1882(6) 0.2328(3) 0.5848(4) 0.0197(17) Uani 1 1 d . . . O1 O 0.8705(4) 0.18318(17) 0.8465(2) 0.0188(11) Uani 1 1 d . . . C51 C -0.0962(6) 0.0003(3) 0.9140(4) 0.0199(17) Uani 1 1 d . . . C7 C 1.1314(6) 0.1488(3) 0.5858(4) 0.0197(17) Uani 1 1 d . . . H7 H 1.1408 0.118 0.5682 0.024 Uiso 1 1 calc R . . C45 C 0.2333(6) 0.1705(3) 0.7954(4) 0.0156(16) Uani 1 1 d . . . C24 C 0.3323(7) 0.3127(3) 0.9375(4) 0.030(2) Uani 1 1 d . . . H24A H 0.3525 0.3462 0.9397 0.045 Uiso 1 1 calc R . . H24B H 0.2502 0.3092 0.9431 0.045 Uiso 1 1 calc R . . H24C H 0.3539 0.2999 0.8932 0.045 Uiso 1 1 calc R . . C18 C 0.4724(7) 0.1213(3) 0.9217(4) 0.0223(18) Uani 1 1 d . . . H18 H 0.4605 0.0885 0.9276 0.027 Uiso 1 1 calc R . . C34 C 0.6460(7) -0.0654(3) 0.5048(4) 0.0249(19) Uani 1 1 d . . . H34A H 0.6591 -0.0982 0.5184 0.037 Uiso 1 1 calc R . . H34B H 0.6479 -0.0629 0.455 0.037 Uiso 1 1 calc R . . H34C H 0.5716 -0.0551 0.5208 0.037 Uiso 1 1 calc R . . C37 C 0.6593(6) 0.0975(3) 0.5455(4) 0.0226(18) Uani 1 1 d . . . H37 H 0.702 0.1101 0.5092 0.027 Uiso 1 1 calc R . . C38 C 0.5958(6) 0.1271(3) 0.5849(4) 0.0210(18) Uani 1 1 d . . . H38 H 0.5975 0.1599 0.5756 0.025 Uiso 1 1 calc R . . C54 C -0.1648(6) -0.0826(3) 0.8953(4) 0.0245(18) Uani 1 1 d . . . H54A H -0.1607 -0.0749 0.8462 0.029 Uiso 1 1 calc R . . H54B H -0.2393 -0.0978 0.9031 0.029 Uiso 1 1 calc R . . C41 C 0.5944(6) 0.0293(3) 0.6141(4) 0.0191(17) Uani 1 1 d . . . H41 H 0.5951 -0.0034 0.6241 0.023 Uiso 1 1 calc R . . C59 C 0.3958(8) -0.1139(3) 0.7561(5) 0.035(2) Uani 1 1 d . . . H59 H 0.4634 -0.1298 0.7698 0.043 Uiso 1 1 calc R . . C56 C -0.2313(6) -0.0353(3) 0.9983(4) 0.0236(18) Uani 1 1 d . . . H56A H -0.1934 -0.0146 1.0324 0.028 Uiso 1 1 calc R . . H56B H -0.2377 -0.0671 1.0185 0.028 Uiso 1 1 calc R . . N11 N 0.1415(6) 0.2450(2) 0.8525(4) 0.0256(16) Uani 1 1 d . . . C57 C -0.3535(7) -0.0158(3) 0.9824(5) 0.035(2) Uani 1 1 d . . . H57A H -0.3967 -0.0145 1.0246 0.053 Uiso 1 1 calc R . . H57B H -0.3924 -0.0366 0.9496 0.053 Uiso 1 1 calc R . . H57C H -0.3479 0.0159 0.9629 0.053 Uiso 1 1 calc R . . N3 N 0.9271(6) -0.0077(3) 0.6651(4) 0.0274(16) Uani 1 1 d . . . C49 C -0.0465(7) 0.0844(3) 0.9221(4) 0.0229(18) Uani 1 1 d . . . H49 H -0.0576 0.1143 0.9426 0.027 Uiso 1 1 calc R . . C60 C 0.2992(8) -0.1395(3) 0.7344(4) 0.034(2) Uani 1 1 d . . . H60 H 0.3012 -0.1729 0.7323 0.041 Uiso 1 1 calc R . . C13 C 0.8929(6) 0.0273(3) 0.6909(4) 0.0216(18) Uani 1 1 d . . . C23 C 0.3971(7) 0.2854(3) 0.9959(4) 0.0265(19) Uani 1 1 d . . . H23A H 0.4799 0.2897 0.9906 0.032 Uiso 1 1 calc R . . H23B H 0.3761 0.2989 1.0405 0.032 Uiso 1 1 calc R . . C30 C 0.6679(8) 0.3510(3) 0.7853(5) 0.039(2) Uani 1 1 d . . . H30 H 0.5966 0.3652 0.7748 0.046 Uiso 1 1 calc R . . C11 C 0.9873(6) 0.1167(3) 0.6629(4) 0.0180(17) Uani 1 1 d . . . H11 H 1.0089 0.0871 0.6449 0.022 Uiso 1 1 calc R . . C32 C 0.9121(6) 0.0569(3) 0.4879(4) 0.0254(18) Uani 1 1 d . . . H32A H 0.9544 0.0688 0.4488 0.038 Uiso 1 1 calc R . . H32B H 0.9571 0.0327 0.5115 0.038 Uiso 1 1 calc R . . H32C H 0.8971 0.0829 0.5193 0.038 Uiso 1 1 calc R . . C44 C 0.3701(6) 0.2246(3) 0.7422(4) 0.0204(18) Uani 1 1 d . . . C19 C 0.4094(7) 0.1519(3) 0.9601(4) 0.0208(18) Uani 1 1 d . . . H19 H 0.3544 0.1401 0.9906 0.025 Uiso 1 1 calc R . . C26 C 0.3295(7) 0.1988(3) 1.1105(4) 0.029(2) Uani 1 1 d . . . H26A H 0.267 0.1885 1.1394 0.043 Uiso 1 1 calc R . . H26B H 0.3728 0.2237 1.1338 0.043 Uiso 1 1 calc R . . H26C H 0.3796 0.172 1.1015 0.043 Uiso 1 1 calc R . . C2 C 1.3177(7) 0.2627(3) 0.4929(4) 0.029(2) Uani 1 1 d . . . H2A H 1.3204 0.2933 0.4687 0.035 Uiso 1 1 calc R . . H2B H 1.277 0.24 0.4629 0.035 Uiso 1 1 calc R . . C27 C 0.8720(7) 0.3066(3) 0.8157(4) 0.030(2) Uani 1 1 d . . . H27 H 0.9429 0.2919 0.8253 0.035 Uiso 1 1 calc R . . C29 C 0.7564(9) 0.3782(3) 0.8127(5) 0.045(3) Uani 1 1 d . . . H29 H 0.7476 0.4111 0.819 0.054 Uiso 1 1 calc R . . C17 C 0.5566(6) 0.1364(3) 0.8723(4) 0.0184(17) Uani 1 1 d . . . C62 C 0.1998(7) -0.0654(3) 0.7190(4) 0.0237(18) Uani 1 1 d . . . H62 H 0.1322 -0.0489 0.7069 0.028 Uiso 1 1 calc R . . C31 C 0.6844(7) 0.3030(3) 0.7732(4) 0.0235(19) Uani 1 1 d . . . H31 H 0.6236 0.2851 0.7541 0.028 Uiso 1 1 calc R . . C28 C 0.8593(9) 0.3555(3) 0.8308(5) 0.043(3) Uani 1 1 d . . . H28 H 0.9192 0.3724 0.8526 0.052 Uiso 1 1 calc R . . C55 C -0.0682(7) -0.1184(3) 0.9139(5) 0.029(2) Uani 1 1 d . . . H55A H -0.0769 -0.1467 0.8857 0.043 Uiso 1 1 calc R . . H55B H -0.073 -0.127 0.9621 0.043 Uiso 1 1 calc R . . H55C H 0.0058 -0.1039 0.9055 0.043 Uiso 1 1 calc R . . N6 N 0.3707(5) 0.2344(2) 0.9955(3) 0.0233(15) Uani 1 1 d . . . C3 C 1.1777(8) 0.3522(3) 0.5617(5) 0.036(2) Uani 1 1 d . . . H3A H 1.1888 0.3825 0.5849 0.054 Uiso 1 1 calc R . . H3B H 1.1002 0.3409 0.5692 0.054 Uiso 1 1 calc R . . H3C H 1.1894 0.3562 0.5127 0.054 Uiso 1 1 calc R . . C25 C 0.2813(7) 0.2177(3) 1.0432(4) 0.027(2) Uani 1 1 d . . . H25A H 0.2363 0.1925 1.0205 0.033 Uiso 1 1 calc R . . H25B H 0.2291 0.2441 1.0529 0.033 Uiso 1 1 calc R . . C1 C 1.4424(7) 0.2448(4) 0.5067(5) 0.041(2) Uani 1 1 d . . . H1A H 1.4813 0.2411 0.4633 0.062 Uiso 1 1 calc R . . H1B H 1.44 0.2143 0.5303 0.062 Uiso 1 1 calc R . . H1C H 1.4835 0.2676 0.5353 0.062 Uiso 1 1 calc R . . N10 N 0.4025(5) 0.2628(2) 0.7326(3) 0.0225(15) Uani 1 1 d . . . C10 C 1.1127(6) 0.2408(3) 0.6410(4) 0.0193(17) Uani 1 1 d . . . H10 H 1.1087 0.2713 0.6606 0.023 Uiso 1 1 calc R . . C42 C 0.4616(6) 0.1449(3) 0.6771(4) 0.0169(9) Uani 1 1 d U . . H42 H 0.4783 0.177 0.6678 0.02 Uiso 1 1 calc R . . C50 C -0.1099(7) 0.0463(3) 0.9456(4) 0.0212(18) Uani 1 1 d . . . H50 H -0.1616 0.0504 0.9817 0.025 Uiso 1 1 calc R . . C21 C 0.5079(6) 0.2186(3) 0.9045(4) 0.0193(17) Uani 1 1 d . . . H21 H 0.5206 0.2514 0.8993 0.023 Uiso 1 1 calc R . . C40 C 0.5271(6) 0.0600(3) 0.6539(4) 0.0185(17) Uani 1 1 d . . . C12 C 0.8493(6) 0.0710(3) 0.7211(4) 0.0167(16) Uani 1 1 d . . . C8 C 1.0504(6) 0.1561(3) 0.6398(4) 0.0159(16) Uani 1 1 d . . . C33 C 0.7972(7) 0.0353(3) 0.4624(4) 0.0234(18) Uani 1 1 d . . . H33A H 0.7528 0.0598 0.4376 0.028 Uiso 1 1 calc R . . H33B H 0.8128 0.0095 0.43 0.028 Uiso 1 1 calc R . . C15 C 0.7104(6) 0.0202(3) 0.7765(4) 0.0205(18) Uani 1 1 d . . . C53 C 0.0456(6) 0.0347(3) 0.8358(4) 0.0157(16) Uani 1 1 d . . . C52 C -0.0179(6) -0.0044(3) 0.8583(4) 0.0191(17) Uani 1 1 d . . . H52 H -0.0093 -0.034 0.8366 0.023 Uiso 1 1 calc R . . C36 C 0.6623(6) 0.0468(3) 0.5584(4) 0.0202(17) Uani 1 1 d . . . C22 C 0.5689(6) 0.1866(3) 0.8630(4) 0.0195(17) Uani 1 1 d . . . C16 C 0.6173(6) 0.1008(3) 0.8358(4) 0.0184(17) Uani 1 1 d . . . H16 H 0.5944 0.0691 0.8427 0.022 Uiso 1 1 calc R . . C9 C 1.0435(6) 0.2038(3) 0.6679(4) 0.0173(17) Uani 1 1 d . . . C20 C 0.4274(6) 0.2028(3) 0.9539(4) 0.0191(17) Uani 1 1 d . . . C58 C 0.3906(7) -0.0641(3) 0.7573(4) 0.0272(19) Uani 1 1 d . . . H58 H 0.4562 -0.0469 0.7712 0.033 Uiso 1 1 calc R . . C6 C 1.1954(6) 0.1849(3) 0.5588(4) 0.0256(19) Uani 1 1 d . . . H6 H 1.2452 0.1783 0.5224 0.031 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 0.01132(15) 0.01632(16) 0.01959(15) 0.00123(12) 0.00246(11) -0.00041(12) U2 0.01104(14) 0.01556(15) 0.01923(15) -0.00035(12) 0.00108(11) -0.00105(12) O4 0.018(3) 0.020(3) 0.042(4) 0.011(3) 0.013(3) 0.000(2) O6 0.021(3) 0.022(3) 0.016(3) 0.004(2) -0.003(2) -0.007(2) O7 0.016(3) 0.016(3) 0.033(3) 0.004(2) 0.002(2) 0.004(2) N2 0.021(4) 0.014(3) 0.018(3) 0.002(3) -0.001(3) -0.001(3) O2 0.026(3) 0.025(3) 0.022(3) 0.000(2) -0.004(2) -0.003(2) O5 0.017(3) 0.018(3) 0.023(3) -0.003(2) 0.004(2) 0.004(2) N1 0.018(3) 0.019(4) 0.024(4) 0.002(3) 0.003(3) -0.003(3) N14 0.021(4) 0.020(4) 0.024(4) 0.001(3) 0.001(3) -0.003(3) N13 0.014(3) 0.022(4) 0.026(4) 0.004(3) 0.003(3) -0.002(3) N12 0.012(3) 0.019(4) 0.022(3) -0.002(3) 0.005(3) -0.002(3) N8 0.013(3) 0.018(4) 0.027(4) -0.007(3) 0.005(3) -0.003(3) O8 0.021(3) 0.012(3) 0.022(3) -0.008(2) 0.007(2) -0.005(2) O3 0.016(3) 0.020(3) 0.021(3) -0.006(2) 0.008(2) -0.003(2) C14 0.014(4) 0.020(4) 0.021(4) 0.007(3) -0.003(3) -0.001(3) N4 0.017(4) 0.025(4) 0.038(4) 0.009(3) -0.007(3) -0.004(3) C47 0.007(4) 0.020(4) 0.019(4) -0.002(3) 0.002(3) 0.004(3) N7 0.017(4) 0.030(4) 0.024(4) 0.003(3) 0.010(3) 0.000(3) N5 0.016(3) 0.020(4) 0.023(4) 0.001(3) 0.004(3) 0.004(3) N9 0.016(2) 0.016(2) 0.020(2) 0.0037(18) 0.0004(17) -0.0014(18) C48 0.017(4) 0.011(4) 0.016(4) 0.000(3) 0.003(3) 0.001(3) C35 0.015(4) 0.020(4) 0.030(5) -0.008(3) -0.001(3) 0.001(3) C43 0.008(4) 0.015(4) 0.022(4) -0.001(3) -0.002(3) 0.001(3) C46 0.009(4) 0.020(4) 0.023(4) 0.001(3) -0.003(3) -0.002(3) C4 0.024(4) 0.023(5) 0.035(5) 0.003(4) 0.005(4) -0.010(4) C39 0.016(2) 0.016(2) 0.020(2) 0.0034(19) 0.0002(18) -0.0020(18) C61 0.029(5) 0.016(4) 0.038(5) -0.008(4) 0.010(4) -0.011(4) C5 0.010(4) 0.026(5) 0.024(4) 0.001(3) -0.004(3) 0.001(3) O1 0.023(3) 0.017(3) 0.017(3) 0.000(2) 0.005(2) 0.002(2) C51 0.014(4) 0.021(4) 0.024(4) 0.004(3) -0.004(3) 0.002(3) C7 0.017(4) 0.016(4) 0.026(4) 0.004(3) -0.001(3) 0.006(3) C45 0.015(4) 0.016(4) 0.016(4) -0.001(3) 0.001(3) -0.001(3) C24 0.030(5) 0.023(5) 0.036(5) -0.005(4) 0.002(4) 0.002(4) C18 0.026(5) 0.022(4) 0.019(4) 0.005(3) -0.001(3) -0.012(4) C34 0.029(5) 0.021(5) 0.025(4) -0.002(3) 0.000(4) -0.003(4) C37 0.016(4) 0.025(5) 0.027(5) 0.004(4) 0.001(3) -0.007(3) C38 0.009(4) 0.017(4) 0.037(5) -0.002(4) 0.004(3) -0.003(3) C54 0.015(4) 0.021(4) 0.038(5) 0.006(4) 0.002(4) -0.005(3) C41 0.017(4) 0.015(4) 0.025(4) 0.000(3) -0.007(3) 0.001(3) C59 0.035(5) 0.033(5) 0.039(6) 0.011(4) 0.004(4) 0.008(4) C56 0.017(4) 0.027(5) 0.028(5) 0.006(4) 0.007(3) -0.007(3) N11 0.017(4) 0.021(4) 0.039(4) -0.006(3) 0.002(3) -0.004(3) C57 0.025(5) 0.035(5) 0.046(6) 0.015(4) 0.007(4) 0.001(4) N3 0.021(4) 0.029(4) 0.032(4) -0.002(3) -0.005(3) -0.001(3) C49 0.023(4) 0.023(5) 0.022(4) -0.004(3) 0.003(3) 0.002(4) C60 0.053(6) 0.008(4) 0.041(5) 0.000(4) 0.021(5) -0.006(4) C13 0.013(4) 0.027(5) 0.025(5) 0.000(4) -0.003(3) -0.004(4) C23 0.027(5) 0.021(5) 0.032(5) -0.012(4) -0.001(4) -0.006(4) C30 0.035(6) 0.028(5) 0.053(6) 0.006(5) 0.018(5) 0.011(4) C11 0.021(4) 0.014(4) 0.019(4) -0.004(3) -0.001(3) 0.006(3) C32 0.023(4) 0.021(5) 0.032(5) -0.005(4) 0.008(4) 0.001(4) C44 0.008(4) 0.027(5) 0.026(5) -0.001(4) -0.001(3) 0.002(3) C19 0.020(4) 0.024(5) 0.018(4) 0.002(3) 0.005(3) -0.006(3) C26 0.033(5) 0.031(5) 0.022(4) -0.011(4) 0.011(4) -0.017(4) C2 0.026(5) 0.037(5) 0.026(5) 0.011(4) 0.007(4) -0.002(4) C27 0.028(5) 0.030(5) 0.031(5) -0.005(4) 0.009(4) -0.003(4) C29 0.069(8) 0.008(4) 0.059(7) -0.008(4) 0.031(6) -0.007(5) C17 0.014(4) 0.026(5) 0.016(4) -0.004(3) -0.002(3) -0.002(3) C62 0.018(4) 0.031(5) 0.022(4) -0.005(4) 0.006(3) 0.000(4) C31 0.023(4) 0.024(5) 0.024(4) 0.006(4) 0.009(3) 0.006(4) C28 0.045(6) 0.036(6) 0.049(6) -0.015(5) 0.013(5) -0.016(5) C55 0.018(4) 0.022(5) 0.045(6) 0.003(4) -0.006(4) -0.004(4) N6 0.010(3) 0.027(4) 0.033(4) -0.001(3) 0.009(3) -0.004(3) C3 0.037(5) 0.031(5) 0.040(6) 0.008(4) -0.004(4) 0.002(4) C25 0.024(5) 0.024(5) 0.036(5) -0.011(4) 0.012(4) -0.008(4) C1 0.025(5) 0.062(7) 0.038(6) -0.003(5) 0.011(4) 0.000(5) N10 0.017(4) 0.017(4) 0.033(4) -0.002(3) 0.005(3) -0.001(3) C10 0.009(4) 0.023(4) 0.026(4) -0.001(3) -0.001(3) 0.004(3) C42 0.016(2) 0.015(2) 0.020(2) 0.0037(18) 0.0003(17) -0.0019(17) C50 0.022(4) 0.020(4) 0.022(4) 0.006(3) 0.006(3) 0.003(3) C21 0.012(4) 0.017(4) 0.029(5) 0.003(3) 0.001(3) -0.004(3) C40 0.005(4) 0.027(5) 0.023(4) 0.001(3) 0.002(3) -0.003(3) C12 0.010(4) 0.016(4) 0.024(4) -0.003(3) 0.001(3) 0.003(3) C8 0.013(4) 0.022(4) 0.013(4) -0.001(3) 0.000(3) 0.004(3) C33 0.021(4) 0.023(4) 0.027(5) 0.003(3) 0.005(4) 0.008(3) C15 0.013(4) 0.030(5) 0.019(4) 0.000(4) 0.000(3) 0.001(4) C53 0.008(4) 0.020(4) 0.019(4) 0.007(3) 0.001(3) 0.003(3) C52 0.020(4) 0.014(4) 0.024(4) 0.003(3) 0.002(3) 0.005(3) C36 0.010(4) 0.030(5) 0.021(4) 0.001(4) -0.002(3) -0.005(3) C22 0.011(4) 0.021(4) 0.026(4) 0.010(3) -0.004(3) -0.004(3) C16 0.016(4) 0.019(4) 0.019(4) 0.001(3) 0.002(3) -0.007(3) C9 0.009(4) 0.026(4) 0.017(4) 0.002(3) -0.004(3) -0.005(3) C20 0.013(4) 0.023(4) 0.021(4) 0.000(3) -0.004(3) -0.003(3) C58 0.023(5) 0.023(5) 0.036(5) 0.006(4) 0.002(4) 0.000(4) C6 0.015(4) 0.031(5) 0.031(5) 0.002(4) 0.004(3) 0.010(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.776(5) . ? U1 O2 1.794(5) . ? U1 O4 2.226(5) . ? U1 O3 2.242(5) . ? U1 N2 2.580(6) . ? U1 N7 2.591(7) . ? U1 N5 2.595(6) . ? U2 O5 1.785(5) . ? U2 O6 1.789(5) . ? U2 O8 2.219(5) . ? U2 O7 2.239(5) . ? U2 N14 2.589(6) . ? U2 N12 2.590(6) . ? U2 N9 2.596(6) . ? O4 C22 1.305(9) . ? O7 C40 1.320(9) . ? N2 C11 1.324(9) . ? N2 C12 1.409(9) . ? N1 C5 1.351(9) . ? N1 C4 1.456(10) . ? N1 C2 1.480(10) . ? N14 C62 1.343(9) . ? N14 C58 1.349(10) . ? N13 C51 1.357(9) . ? N13 C54 1.463(10) . ? N13 C56 1.481(9) . ? N12 C47 1.325(9) . ? N12 C45 1.405(9) . ? N8 C36 1.360(9) . ? N8 C35 1.445(9) . ? N8 C33 1.467(9) . ? O8 C53 1.332(8) . ? O3 C9 1.320(8) . ? C14 C12 1.359(10) . ? C14 N5 1.395(9) . ? C14 C15 1.441(11) . ? N4 C15 1.153(10) . ? C47 C48 1.412(10) . ? C47 H47 0.93 . ? N7 C27 1.326(10) . ? N7 C31 1.355(9) . ? N5 C16 1.336(9) . ? N9 C42 1.338(9) . ? N9 C43 1.375(9) . ? C48 C49 1.411(10) . ? C48 C53 1.429(10) . ? C35 C34 1.518(10) . ? C35 H35A 0.97 . ? C35 H35B 0.97 . ? C43 C45 1.365(10) . ? C43 C44 1.455(11) . ? C46 N11 1.138(9) . ? C46 C45 1.441(10) . ? C4 C3 1.520(11) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C39 C42 1.412(10) . ? C39 C38 1.421(10) . ? C39 C40 1.428(10) . ? C61 C60 1.382(12) . ? C61 C62 1.375(11) . ? C61 H61 0.93 . ? C5 C10 1.417(10) . ? C5 C6 1.426(11) . ? C51 C52 1.418(10) . ? C51 C50 1.425(10) . ? C7 C6 1.355(11) . ? C7 C8 1.424(10) . ? C7 H7 0.93 . ? C24 C23 1.538(11) . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C18 C19 1.348(10) . ? C18 C17 1.433(10) . ? C18 H18 0.93 . ? C34 H34A 0.96 . ? C34 H34B 0.96 . ? C34 H34C 0.96 . ? C37 C38 1.344(10) . ? C37 C36 1.432(11) . ? C37 H37 0.93 . ? C38 H38 0.93 . ? C54 C55 1.530(10) . ? C54 H54A 0.97 . ? C54 H54B 0.97 . ? C41 C40 1.392(10) . ? C41 C36 1.422(10) . ? C41 H41 0.93 . ? C59 C60 1.380(12) . ? C59 C58 1.386(11) . ? C59 H59 0.93 . ? C56 C57 1.534(11) . ? C56 H56A 0.97 . ? C56 H56B 0.97 . ? C57 H57A 0.96 . ? C57 H57B 0.96 . ? C57 H57C 0.96 . ? N3 C13 1.164(10) . ? C49 C50 1.369(10) . ? C49 H49 0.93 . ? C60 H60 0.93 . ? C13 C12 1.440(11) . ? C23 N6 1.451(10) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C30 C29 1.366(13) . ? C30 C31 1.370(11) . ? C30 H30 0.93 . ? C11 C8 1.393(10) . ? C11 H11 0.93 . ? C32 C33 1.528(10) . ? C32 H32A 0.96 . ? C32 H32B 0.96 . ? C32 H32C 0.96 . ? C44 N10 1.142(9) . ? C19 C20 1.437(10) . ? C19 H19 0.93 . ? C26 C25 1.493(11) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C2 C1 1.540(11) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C27 C28 1.397(12) . ? C27 H27 0.93 . ? C29 C28 1.383(14) . ? C29 H29 0.93 . ? C17 C16 1.406(10) . ? C17 C22 1.416(10) . ? C62 H62 0.93 . ? C31 H31 0.93 . ? C28 H28 0.93 . ? C55 H55A 0.96 . ? C55 H55B 0.96 . ? C55 H55C 0.96 . ? N6 C20 1.362(9) . ? N6 C25 1.467(9) . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C10 C9 1.407(10) . ? C10 H10 0.93 . ? C42 H42 0.93 . ? C50 H50 0.93 . ? C21 C22 1.394(10) . ? C21 C20 1.410(10) . ? C21 H21 0.93 . ? C8 C9 1.433(10) . ? C33 H33A 0.97 . ? C33 H33B 0.97 . ? C53 C52 1.384(10) . ? C52 H52 0.93 . ? C16 H16 0.93 . ? C58 H58 0.93 . ? C6 H6 0.93 . ? 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 O2 177.9(2) . . ? O1 U1 O4 90.9(2) . . ? O2 U1 O4 88.1(2) . . ? O1 U1 O3 89.5(2) . . ? O2 U1 O3 90.5(2) . . ? O4 U1 O3 153.84(18) . . ? O1 U1 N2 96.3(2) . . ? O2 U1 N2 85.6(2) . . ? O4 U1 N2 134.34(19) . . ? O3 U1 N2 71.49(18) . . ? O1 U1 N7 87.7(2) . . ? O2 U1 N7 90.2(2) . . ? O4 U1 N7 72.37(19) . . ? O3 U1 N7 81.51(18) . . ? N2 U1 N7 152.62(19) . . ? O1 U1 N5 84.7(2) . . ? O2 U1 N5 96.7(2) . . ? O4 U1 N5 69.93(19) . . ? O3 U1 N5 136.09(18) . . ? N2 U1 N5 66.00(19) . . ? N7 U1 N5 141.36(19) . . ? O5 U2 O6 176.6(2) . . ? O5 U2 O8 87.6(2) . . ? O6 U2 O8 91.8(2) . . ? O5 U2 O7 90.1(2) . . ? O6 U2 O7 89.2(2) . . ? O8 U2 O7 155.52(18) . . ? O5 U2 N14 90.9(2) . . ? O6 U2 N14 85.7(2) . . ? O8 U2 N14 75.48(19) . . ? O7 U2 N14 80.20(19) . . ? O5 U2 N12 99.4(2) . . ? O6 U2 N12 83.5(2) . . ? O8 U2 N12 70.53(18) . . ? O7 U2 N12 133.80(18) . . ? N14 U2 N12 143.87(19) . . ? O5 U2 N9 84.2(2) . . ? O6 U2 N9 98.7(2) . . ? O8 U2 N9 132.41(18) . . ? O7 U2 N9 71.41(18) . . ? N14 U2 N9 151.14(19) . . ? N12 U2 N9 64.86(19) . . ? C22 O4 U1 140.3(5) . . ? C40 O7 U2 136.0(4) . . ? C11 N2 C12 117.5(6) . . ? C11 N2 U1 126.5(5) . . ? C12 N2 U1 115.8(4) . . ? C5 N1 C4 123.2(6) . . ? C5 N1 C2 122.0(7) . . ? C4 N1 C2 114.9(6) . . ? C62 N14 C58 117.8(7) . . ? C62 N14 U2 122.5(5) . . ? C58 N14 U2 119.6(5) . . ? C51 N13 C54 121.8(6) . . ? C51 N13 C56 121.2(6) . . ? C54 N13 C56 116.8(6) . . ? C47 N12 C45 116.8(6) . . ? C47 N12 U2 126.3(5) . . ? C45 N12 U2 116.5(4) . . ? C36 N8 C35 121.8(6) . . ? C36 N8 C33 120.4(6) . . ? C35 N8 C33 117.6(6) . . ? C53 O8 U2 139.0(4) . . ? C9 O3 U1 141.4(4) . . ? C12 C14 N5 121.7(7) . . ? C12 C14 C15 117.8(7) . . ? N5 C14 C15 120.5(6) . . ? N12 C47 C48 127.1(7) . . ? N12 C47 H47 116.4 . . ? C48 C47 H47 116.4 . . ? C27 N7 C31 118.0(7) . . ? C27 N7 U1 123.5(5) . . ? C31 N7 U1 118.5(5) . . ? C16 N5 C14 117.3(6) . . ? C16 N5 U1 127.0(5) . . ? C14 N5 U1 115.4(4) . . ? C42 N9 C43 117.8(6) . . ? C42 N9 U2 124.2(5) . . ? C43 N9 U2 117.4(4) . . ? C47 C48 C49 118.2(7) . . ? C47 C48 C53 125.0(6) . . ? C49 C48 C53 116.8(6) . . ? N8 C35 C34 113.7(6) . . ? N8 C35 H35A 108.8 . . ? C34 C35 H35A 108.8 . . ? N8 C35 H35B 108.8 . . ? C34 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C45 C43 N9 120.6(7) . . ? C45 C43 C44 118.0(7) . . ? N9 C43 C44 121.3(6) . . ? N11 C46 C45 179.6(9) . . ? N1 C4 C3 113.1(7) . . ? N1 C4 H4A 109 . . ? C3 C4 H4A 109 . . ? N1 C4 H4B 109 . . ? C3 C4 H4B 109 . . ? H4A C4 H4B 107.8 . . ? C42 C39 C38 117.6(7) . . ? C42 C39 C40 125.3(7) . . ? C38 C39 C40 117.0(7) . . ? C60 C61 C62 118.9(8) . . ? C60 C61 H61 120.6 . . ? C62 C61 H61 120.6 . . ? N1 C5 C10 121.6(7) . . ? N1 C5 C6 121.4(7) . . ? C10 C5 C6 117.0(7) . . ? N13 C51 C52 120.4(7) . . ? N13 C51 C50 120.9(7) . . ? C52 C51 C50 118.7(7) . . ? C6 C7 C8 122.8(7) . . ? C6 C7 H7 118.6 . . ? C8 C7 H7 118.6 . . ? C43 C45 N12 120.6(6) . . ? C43 C45 C46 119.4(7) . . ? N12 C45 C46 119.9(6) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C18 C17 123.8(7) . . ? C19 C18 H18 118.1 . . ? C17 C18 H18 118.1 . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C38 C37 C36 121.2(7) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 122.8(7) . . ? C37 C38 H38 118.6 . . ? C39 C38 H38 118.6 . . ? N13 C54 C55 113.5(6) . . ? N13 C54 H54A 108.9 . . ? C55 C54 H54A 108.9 . . ? N13 C54 H54B 108.9 . . ? C55 C54 H54B 108.9 . . ? H54A C54 H54B 107.7 . . ? C40 C41 C36 121.6(7) . . ? C40 C41 H41 119.2 . . ? C36 C41 H41 119.2 . . ? C60 C59 C58 119.0(8) . . ? C60 C59 H59 120.5 . . ? C58 C59 H59 120.5 . . ? N13 C56 C57 112.8(7) . . ? N13 C56 H56A 109 . . ? C57 C56 H56A 109 . . ? N13 C56 H56B 109 . . ? C57 C56 H56B 109 . . ? H56A C56 H56B 107.8 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C50 C49 C48 123.3(7) . . ? C50 C49 H49 118.3 . . ? C48 C49 H49 118.3 . . ? C61 C60 C59 119.0(8) . . ? C61 C60 H60 120.5 . . ? C59 C60 H60 120.5 . . ? N3 C13 C12 178.5(8) . . ? N6 C23 C24 112.4(6) . . ? N6 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N6 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C29 C30 C31 119.9(9) . . ? C29 C30 H30 120 . . ? C31 C30 H30 120 . . ? N2 C11 C8 128.5(7) . . ? N2 C11 H11 115.7 . . ? C8 C11 H11 115.7 . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N10 C44 C43 179.2(9) . . ? C18 C19 C20 119.9(7) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N1 C2 C1 111.8(7) . . ? N1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? N7 C27 C28 122.2(9) . . ? N7 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? C30 C29 C28 118.4(8) . . ? C30 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? C16 C17 C22 125.5(7) . . ? C16 C17 C18 118.2(7) . . ? C22 C17 C18 116.3(7) . . ? N14 C62 C61 123.0(8) . . ? N14 C62 H62 118.5 . . ? C61 C62 H62 118.5 . . ? N7 C31 C30 122.3(8) . . ? N7 C31 H31 118.8 . . ? C30 C31 H31 118.8 . . ? C29 C28 C27 119.0(9) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C20 N6 C23 122.0(6) . . ? C20 N6 C25 120.8(6) . . ? C23 N6 C25 117.2(6) . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N6 C25 C26 113.4(7) . . ? N6 C25 H25A 108.9 . . ? C26 C25 H25A 108.9 . . ? N6 C25 H25B 108.9 . . ? C26 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C9 C10 C5 121.7(7) . . ? C9 C10 H10 119.2 . . ? C5 C10 H10 119.2 . . ? N9 C42 C39 127.6(7) . . ? N9 C42 H42 116.2 . . ? C39 C42 H42 116.2 . . ? C49 C50 C51 119.4(7) . . ? C49 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C22 C21 C20 122.1(7) . . ? C22 C21 H21 119 . . ? C20 C21 H21 119 . . ? O7 C40 C41 119.8(7) . . ? O7 C40 C39 119.8(7) . . ? C41 C40 C39 120.3(7) . . ? C14 C12 N2 121.0(7) . . ? C14 C12 C13 117.7(7) . . ? N2 C12 C13 121.4(6) . . ? C11 C8 C7 118.2(7) . . ? C11 C8 C9 125.2(7) . . ? C7 C8 C9 116.6(7) . . ? N8 C33 C32 112.4(6) . . ? N8 C33 H33A 109.1 . . ? C32 C33 H33A 109.1 . . ? N8 C33 H33B 109.1 . . ? C32 C33 H33B 109.1 . . ? H33A C33 H33B 107.9 . . ? N4 C15 C14 179.3(9) . . ? O8 C53 C52 119.8(7) . . ? O8 C53 C48 119.1(6) . . ? C52 C53 C48 121.0(6) . . ? C53 C52 C51 120.7(7) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? N8 C36 C41 121.2(7) . . ? N8 C36 C37 121.8(7) . . ? C41 C36 C37 117.0(7) . . ? O4 C22 C21 120.7(7) . . ? O4 C22 C17 118.7(7) . . ? C21 C22 C17 120.4(7) . . ? N5 C16 C17 126.3(7) . . ? N5 C16 H16 116.8 . . ? C17 C16 H16 116.8 . . ? O3 C9 C10 119.9(7) . . ? O3 C9 C8 119.8(6) . . ? C10 C9 C8 120.2(7) . . ? N6 C20 C21 121.5(7) . . ? N6 C20 C19 121.0(7) . . ? C21 C20 C19 117.4(7) . . ? N14 C58 C59 122.2(8) . . ? N14 C58 H58 118.9 . . ? C59 C58 H58 118.9 . . ? C7 C6 C5 121.6(7) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? 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 O4 C22 -40.7(8) . . . . ? O2 U1 O4 C22 141.1(8) . . . . ? O3 U1 O4 C22 -131.5(7) . . . . ? N2 U1 O4 C22 59.1(9) . . . . ? N7 U1 O4 C22 -128.1(8) . . . . ? N5 U1 O4 C22 43.3(8) . . . . ? O5 U2 O7 C40 37.0(7) . . . . ? O6 U2 O7 C40 -146.3(7) . . . . ? O8 U2 O7 C40 121.3(7) . . . . ? N14 U2 O7 C40 127.9(7) . . . . ? N12 U2 O7 C40 -66.1(7) . . . . ? N9 U2 O7 C40 -46.8(7) . . . . ? O1 U1 N2 C11 -103.8(6) . . . . ? O2 U1 N2 C11 75.6(6) . . . . ? O4 U1 N2 C11 158.7(5) . . . . ? O3 U1 N2 C11 -16.4(5) . . . . ? N7 U1 N2 C11 -6.5(8) . . . . ? N5 U1 N2 C11 174.9(6) . . . . ? O1 U1 N2 C12 82.0(5) . . . . ? O2 U1 N2 C12 -98.7(5) . . . . ? O4 U1 N2 C12 -15.6(6) . . . . ? O3 U1 N2 C12 169.3(5) . . . . ? N7 U1 N2 C12 179.3(5) . . . . ? N5 U1 N2 C12 0.6(5) . . . . ? O5 U2 N14 C62 -52.3(6) . . . . ? O6 U2 N14 C62 127.9(6) . . . . ? O8 U2 N14 C62 35.0(6) . . . . ? O7 U2 N14 C62 -142.2(6) . . . . ? N12 U2 N14 C62 55.1(7) . . . . ? N9 U2 N14 C62 -131.8(6) . . . . ? O5 U2 N14 C58 131.0(6) . . . . ? O6 U2 N14 C58 -48.8(6) . . . . ? O8 U2 N14 C58 -141.8(6) . . . . ? O7 U2 N14 C58 41.1(6) . . . . ? N12 U2 N14 C58 -121.6(6) . . . . ? N9 U2 N14 C58 51.5(8) . . . . ? O5 U2 N12 C47 107.1(6) . . . . ? O6 U2 N12 C47 -71.1(6) . . . . ? O8 U2 N12 C47 23.0(5) . . . . ? O7 U2 N12 C47 -153.7(5) . . . . ? N14 U2 N12 C47 2.3(7) . . . . ? N9 U2 N12 C47 -174.0(6) . . . . ? O5 U2 N12 C45 -80.8(5) . . . . ? O6 U2 N12 C45 101.0(5) . . . . ? O8 U2 N12 C45 -164.8(5) . . . . ? O7 U2 N12 C45 18.4(6) . . . . ? N14 U2 N12 C45 174.5(4) . . . . ? N9 U2 N12 C45 -1.8(5) . . . . ? O5 U2 O8 C53 -144.6(7) . . . . ? O6 U2 O8 C53 38.7(7) . . . . ? O7 U2 O8 C53 130.6(7) . . . . ? N14 U2 O8 C53 123.8(7) . . . . ? N12 U2 O8 C53 -43.7(7) . . . . ? N9 U2 O8 C53 -64.8(7) . . . . ? O1 U1 O3 C9 129.8(8) . . . . ? O2 U1 O3 C9 -52.2(8) . . . . ? O4 U1 O3 C9 -139.0(7) . . . . ? N2 U1 O3 C9 33.0(7) . . . . ? N7 U1 O3 C9 -142.4(8) . . . . ? N5 U1 O3 C9 48.0(8) . . . . ? C45 N12 C47 C48 178.1(7) . . . . ? U2 N12 C47 C48 -9.8(10) . . . . ? O1 U1 N7 C27 44.3(6) . . . . ? O2 U1 N7 C27 -136.0(6) . . . . ? O4 U1 N7 C27 136.0(6) . . . . ? O3 U1 N7 C27 -45.5(6) . . . . ? N2 U1 N7 C27 -55.1(8) . . . . ? N5 U1 N7 C27 123.0(6) . . . . ? O1 U1 N7 C31 -134.9(5) . . . . ? O2 U1 N7 C31 44.8(5) . . . . ? O4 U1 N7 C31 -43.2(5) . . . . ? O3 U1 N7 C31 135.3(5) . . . . ? N2 U1 N7 C31 125.7(5) . . . . ? N5 U1 N7 C31 -56.2(7) . . . . ? C12 C14 N5 C16 -176.5(7) . . . . ? C15 C14 N5 C16 4.0(10) . . . . ? C12 C14 N5 U1 -1.6(9) . . . . ? C15 C14 N5 U1 178.9(5) . . . . ? O1 U1 N5 C16 75.4(6) . . . . ? O2 U1 N5 C16 -103.1(6) . . . . ? O4 U1 N5 C16 -17.5(6) . . . . ? O3 U1 N5 C16 159.2(5) . . . . ? N2 U1 N5 C16 174.7(6) . . . . ? N7 U1 N5 C16 -4.3(8) . . . . ? O1 U1 N5 C14 -98.9(5) . . . . ? O2 U1 N5 C14 82.6(5) . . . . ? O4 U1 N5 C14 168.2(5) . . . . ? O3 U1 N5 C14 -15.1(6) . . . . ? N2 U1 N5 C14 0.4(5) . . . . ? N7 U1 N5 C14 -178.6(4) . . . . ? O5 U2 N9 C42 -66.8(6) . . . . ? O6 U2 N9 C42 111.4(6) . . . . ? O8 U2 N9 C42 -148.1(5) . . . . ? O7 U2 N9 C42 25.3(5) . . . . ? N14 U2 N9 C42 14.5(8) . . . . ? N12 U2 N9 C42 -170.1(6) . . . . ? O5 U2 N9 C43 103.9(5) . . . . ? O6 U2 N9 C43 -77.9(5) . . . . ? O8 U2 N9 C43 22.7(6) . . . . ? O7 U2 N9 C43 -164.0(5) . . . . ? N14 U2 N9 C43 -174.8(4) . . . . ? N12 U2 N9 C43 0.7(5) . . . . ? N12 C47 C48 C49 173.8(7) . . . . ? N12 C47 C48 C53 -6.5(12) . . . . ? C36 N8 C35 C34 87.7(9) . . . . ? C33 N8 C35 C34 -97.9(8) . . . . ? C42 N9 C43 C45 171.9(7) . . . . ? U2 N9 C43 C45 0.6(9) . . . . ? C42 N9 C43 C44 -7.9(10) . . . . ? U2 N9 C43 C44 -179.2(5) . . . . ? C5 N1 C4 C3 -93.8(9) . . . . ? C2 N1 C4 C3 85.6(8) . . . . ? C4 N1 C5 C10 9.2(11) . . . . ? C2 N1 C5 C10 -170.1(7) . . . . ? C4 N1 C5 C6 -168.9(7) . . . . ? C2 N1 C5 C6 11.9(11) . . . . ? C54 N13 C51 C52 -11.5(11) . . . . ? C56 N13 C51 C52 173.6(7) . . . . ? C54 N13 C51 C50 166.8(7) . . . . ? C56 N13 C51 C50 -8.1(11) . . . . ? N9 C43 C45 N12 -2.5(11) . . . . ? C44 C43 C45 N12 177.3(6) . . . . ? N9 C43 C45 C46 178.5(6) . . . . ? C44 C43 C45 C46 -1.7(10) . . . . ? C47 N12 C45 C43 176.0(7) . . . . ? U2 N12 C45 C43 3.1(9) . . . . ? C47 N12 C45 C46 -5.0(10) . . . . ? U2 N12 C45 C46 -177.9(5) . . . . ? N11 C46 C45 C43 13E1(10) . . . . ? N11 C46 C45 N12 -5E1(10) . . . . ? C36 C37 C38 C39 -1.5(12) . . . . ? C42 C39 C38 C37 -178.9(7) . . . . ? C40 C39 C38 C37 1.1(11) . . . . ? C51 N13 C54 C55 88.9(9) . . . . ? C56 N13 C54 C55 -96.0(8) . . . . ? C51 N13 C56 C57 86.4(9) . . . . ? C54 N13 C56 C57 -88.8(8) . . . . ? C47 C48 C49 C50 -177.3(7) . . . . ? C53 C48 C49 C50 2.9(11) . . . . ? C62 C61 C60 C59 0.6(12) . . . . ? C58 C59 C60 C61 -1.3(13) . . . . ? C12 N2 C11 C8 178.7(7) . . . . ? U1 N2 C11 C8 4.6(11) . . . . ? C45 C43 C44 N10 -6E1(7) . . . . ? N9 C43 C44 N10 12E1(7) . . . . ? C17 C18 C19 C20 -1.7(12) . . . . ? C5 N1 C2 C1 -91.5(9) . . . . ? C4 N1 C2 C1 89.2(8) . . . . ? C31 N7 C27 C28 1.4(12) . . . . ? U1 N7 C27 C28 -177.8(6) . . . . ? C31 C30 C29 C28 -3.1(14) . . . . ? C19 C18 C17 C16 179.5(7) . . . . ? C19 C18 C17 C22 -2.3(11) . . . . ? C58 N14 C62 C61 -0.9(11) . . . . ? U2 N14 C62 C61 -177.7(6) . . . . ? C60 C61 C62 N14 0.6(12) . . . . ? C27 N7 C31 C30 0.3(12) . . . . ? U1 N7 C31 C30 179.5(6) . . . . ? C29 C30 C31 N7 0.7(13) . . . . ? C30 C29 C28 C27 4.7(14) . . . . ? N7 C27 C28 C29 -3.9(14) . . . . ? C24 C23 N6 C20 84.2(9) . . . . ? C24 C23 N6 C25 -97.1(8) . . . . ? C20 N6 C25 C26 82.9(9) . . . . ? C23 N6 C25 C26 -95.9(8) . . . . ? N1 C5 C10 C9 178.8(7) . . . . ? C6 C5 C10 C9 -3.0(11) . . . . ? C43 N9 C42 C39 180.0(7) . . . . ? U2 N9 C42 C39 -9.3(10) . . . . ? C38 C39 C42 N9 170.1(7) . . . . ? C40 C39 C42 N9 -9.9(12) . . . . ? C48 C49 C50 C51 -1.2(12) . . . . ? N13 C51 C50 C49 -179.3(7) . . . . ? C52 C51 C50 C49 -1.0(11) . . . . ? U2 O7 C40 C41 -137.6(6) . . . . ? U2 O7 C40 C39 45.6(10) . . . . ? C36 C41 C40 O7 -177.8(6) . . . . ? C36 C41 C40 C39 -1.0(11) . . . . ? C42 C39 C40 O7 -3.1(11) . . . . ? C38 C39 C40 O7 177.0(6) . . . . ? C42 C39 C40 C41 -179.9(7) . . . . ? C38 C39 C40 C41 0.2(11) . . . . ? N5 C14 C12 N2 2.3(11) . . . . ? C15 C14 C12 N2 -178.2(6) . . . . ? N5 C14 C12 C13 -177.2(7) . . . . ? C15 C14 C12 C13 2.3(10) . . . . ? C11 N2 C12 C14 -176.6(7) . . . . ? U1 N2 C12 C14 -1.8(9) . . . . ? C11 N2 C12 C13 2.9(10) . . . . ? U1 N2 C12 C13 177.7(5) . . . . ? N3 C13 C12 C14 10E1(3) . . . . ? N3 C13 C12 N2 -8E1(3) . . . . ? N2 C11 C8 C7 -172.9(7) . . . . ? N2 C11 C8 C9 9.4(12) . . . . ? C6 C7 C8 C11 178.8(7) . . . . ? C6 C7 C8 C9 -3.3(11) . . . . ? C36 N8 C33 C32 81.0(8) . . . . ? C35 N8 C33 C32 -93.5(8) . . . . ? C12 C14 C15 N4 9E1(9) . . . . ? N5 C14 C15 N4 -9E1(8) . . . . ? U2 O8 C53 C52 -138.7(6) . . . . ? U2 O8 C53 C48 43.7(10) . . . . ? C47 C48 C53 O8 -4.6(11) . . . . ? C49 C48 C53 O8 175.2(6) . . . . ? C47 C48 C53 C52 177.8(7) . . . . ? C49 C48 C53 C52 -2.5(10) . . . . ? O8 C53 C52 C51 -177.2(6) . . . . ? C48 C53 C52 C51 0.4(11) . . . . ? N13 C51 C52 C53 179.7(7) . . . . ? C50 C51 C52 C53 1.3(11) . . . . ? C35 N8 C36 C41 -5.7(11) . . . . ? C33 N8 C36 C41 180.0(6) . . . . ? C35 N8 C36 C37 173.7(7) . . . . ? C33 N8 C36 C37 -0.6(11) . . . . ? C40 C41 C36 N8 -179.9(7) . . . . ? C40 C41 C36 C37 0.7(10) . . . . ? C38 C37 C36 N8 -178.8(7) . . . . ? C38 C37 C36 C41 0.6(11) . . . . ? U1 O4 C22 C21 138.2(7) . . . . ? U1 O4 C22 C17 -46.8(11) . . . . ? C20 C21 C22 O4 171.3(7) . . . . ? C20 C21 C22 C17 -3.7(11) . . . . ? C16 C17 C22 O4 7.8(11) . . . . ? C18 C17 C22 O4 -170.2(6) . . . . ? C16 C17 C22 C21 -177.1(7) . . . . ? C18 C17 C22 C21 4.9(10) . . . . ? C14 N5 C16 C17 177.7(7) . . . . ? U1 N5 C16 C17 3.5(11) . . . . ? C22 C17 C16 N5 7.7(12) . . . . ? C18 C17 C16 N5 -174.4(7) . . . . ? U1 O3 C9 C10 149.3(6) . . . . ? U1 O3 C9 C8 -31.5(11) . . . . ? C5 C10 C9 O3 -179.0(6) . . . . ? C5 C10 C9 C8 1.7(11) . . . . ? C11 C8 C9 O3 -0.1(11) . . . . ? C7 C8 C9 O3 -177.9(6) . . . . ? C11 C8 C9 C10 179.1(7) . . . . ? C7 C8 C9 C10 1.4(10) . . . . ? C23 N6 C20 C21 -5.7(11) . . . . ? C25 N6 C20 C21 175.6(7) . . . . ? C23 N6 C20 C19 172.8(7) . . . . ? C25 N6 C20 C19 -5.9(11) . . . . ? C22 C21 C20 N6 178.2(7) . . . . ? C22 C21 C20 C19 -0.4(11) . . . . ? C18 C19 C20 N6 -175.5(7) . . . . ? C18 C19 C20 C21 3.1(11) . . . . ? C62 N14 C58 C59 0.1(12) . . . . ? U2 N14 C58 C59 176.9(6) . . . . ? C60 C59 C58 N14 1.0(13) . . . . ? C8 C7 C6 C5 2.1(12) . . . . ? N1 C5 C6 C7 179.3(7) . . . . ? C10 C5 C6 C7 1.1(11) . . . . ? #===END #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary _ccdc_compound_id 2b # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _ccdc_temp_data_collection 100(2) _ccdc_ls_R_squared 0.0586 #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ data_bcas030p_1 _database_code_depnum_ccdc_archive 'CCDC 802707' #TrackingRef '- salmntall.cif' _audit_creation_date 2009-01-09T17:35:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; '[UO2(salmnt(Et2N)2)(py)]' ; _chemical_formula_sum 'C31 H33 N7 O4 U' _chemical_formula_weight 805.67 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.002(5) _cell_length_b 13.122(5) _cell_length_c 13.456(5) _cell_angle_alpha 111.483(5) _cell_angle_beta 91.195(5) _cell_angle_gamma 105.695(5) _cell_volume 1567.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3850 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 25.06 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prismatic _exptl_crystal_colour 'dark purple' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.293980 _exptl_absorpt_correction_T_max 0.769950 _exptl_absorpt_process_details SADABS #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_unetI/netI 0.0826 _diffrn_reflns_number 11282 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 5632 _reflns_number_gt 4890 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0986P)^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_number_reflns 5632 _refine_ls_number_parameters 388 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1443 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.08 _refine_diff_density_min -3.792 _refine_diff_density_rms 0.268 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.99293(4) 0.71953(3) 0.69334(3) 0.01386(14) Uani 1 1 d . . . N2 N 0.9178(9) 0.6014(7) 0.4880(6) 0.0188(14) Uani 1 1 d U . . N7 N 0.9573(8) 0.7447(8) 0.8914(7) 0.0209(19) Uani 1 1 d . . . C21 C 1.3379(10) 1.0315(8) 0.9025(8) 0.018(2) Uani 1 1 d . . . H21 H 1.2879 1.0442 0.9611 0.022 Uiso 1 1 calc R . . O3 O 0.8432(7) 0.5462(5) 0.6699(5) 0.0185(15) Uani 1 1 d . . . C14 C 1.1078(10) 0.7332(9) 0.4580(8) 0.018(2) Uani 1 1 d . . . C12 C 0.9914(11) 0.6435(8) 0.4207(8) 0.0195(14) Uani 1 1 d U . . C27 C 0.9230(11) 0.6520(8) 0.9176(8) 0.021(2) Uani 1 1 d . . . H27 H 0.9024 0.5795 0.8628 0.025 Uiso 1 1 calc R . . O4 O 1.1324(7) 0.9017(5) 0.7892(5) 0.0170(12) Uani 1 1 d U . . C4 C 0.4311(11) 0.2699(10) 0.7396(8) 0.025(2) Uani 1 1 d . . . H4A H 0.5281 0.2713 0.7487 0.03 Uiso 1 1 calc R . . H4B H 0.373 0.1982 0.7408 0.03 Uiso 1 1 calc R . . C11 C 0.7889(10) 0.5201(9) 0.4477(8) 0.0188(19) Uani 1 1 d U . . H11 H 0.7592 0.4999 0.3753 0.023 Uiso 1 1 calc R . . C17 C 1.3423(10) 0.9304(9) 0.7087(8) 0.019(2) Uani 1 1 d . . . C16 C 1.2793(11) 0.8583(8) 0.6025(8) 0.019(2) Uani 1 1 d . . . H16 H 1.3361 0.8595 0.5488 0.023 Uiso 1 1 calc R . . C25 C 1.6936(11) 1.2426(9) 1.0310(8) 0.025(2) Uani 1 1 d . . . H25A H 1.7515 1.1954 0.9949 0.03 Uiso 1 1 calc R . . H25B H 1.7293 1.2777 1.1072 0.03 Uiso 1 1 calc R . . O1 O 0.8532(7) 0.7746(6) 0.6800(5) 0.0220(16) Uani 1 1 d . . . C8 C 0.6972(10) 0.4640(8) 0.5005(8) 0.016(2) Uani 1 1 d . . . O2 O 1.1335(7) 0.6685(6) 0.7114(5) 0.0183(15) Uani 1 1 d . . . C3 C 0.4078(12) 0.3697(10) 0.8348(9) 0.029(3) Uani 1 1 d . . . H3A H 0.432 0.363 0.901 0.044 Uiso 1 1 calc R . . H3B H 0.3111 0.3673 0.828 0.044 Uiso 1 1 calc R . . H3C H 0.4657 0.4412 0.8347 0.044 Uiso 1 1 calc R . . C9 C 0.5665(10) 0.3846(9) 0.4404(8) 0.020(2) Uani 1 1 d . . . H9 H 0.5472 0.3745 0.3689 0.024 Uiso 1 1 calc R . . C26 C 1.7087(11) 1.3374(10) 0.9881(9) 0.029(3) Uani 1 1 d . . . H26A H 1.8055 1.3817 0.9999 0.043 Uiso 1 1 calc R . . H26B H 1.6545 1.3865 1.0251 0.043 Uiso 1 1 calc R . . H26C H 1.6756 1.3037 0.9123 0.043 Uiso 1 1 calc R . . C20 C 1.4809(11) 1.0932(8) 0.9192(8) 0.019(2) Uani 1 1 d . . . C28 C 0.9172(12) 0.6608(10) 1.0237(8) 0.028(2) Uani 1 1 d . . . H28 H 0.8973 0.5955 1.0397 0.034 Uiso 1 1 calc R . . C1 C 0.2327(13) 0.0861(10) 0.5125(10) 0.036(3) Uani 1 1 d . . . H1A H 0.137 0.0507 0.479 0.055 Uiso 1 1 calc R . . H1B H 0.2533 0.0486 0.5576 0.055 Uiso 1 1 calc R . . H1C H 0.2938 0.0793 0.4579 0.055 Uiso 1 1 calc R . . C31 C 0.9809(11) 0.8481(9) 0.9706(7) 0.022(2) Uani 1 1 d . . . H31 H 1.0027 0.9123 0.9529 0.026 Uiso 1 1 calc R . . C2 C 0.2545(10) 0.2111(9) 0.5799(9) 0.022(2) Uani 1 1 d . . . H2A H 0.2303 0.2476 0.5341 0.026 Uiso 1 1 calc R . . H2B H 0.1913 0.2171 0.634 0.026 Uiso 1 1 calc R . . C24 C 1.4105(11) 1.2830(10) 1.1369(9) 0.029(3) Uani 1 1 d . . . H24A H 1.366 1.2922 1.2009 0.044 Uiso 1 1 calc R . . H24B H 1.3416 1.2631 1.0768 0.044 Uiso 1 1 calc R . . H24C H 1.4805 1.3536 1.1467 0.044 Uiso 1 1 calc R . . C23 C 1.4790(12) 1.1882(9) 1.1155(9) 0.026(2) Uani 1 1 d . . . H23A H 1.5473 1.2082 1.177 0.031 Uiso 1 1 calc R . . H23B H 1.4082 1.1177 1.1077 0.031 Uiso 1 1 calc R . . N5 N 1.1508(8) 0.7900(6) 0.5698(6) 0.0156(17) Uani 1 1 d . . . C22 C 1.2680(10) 0.9524(8) 0.8023(7) 0.0167(12) Uani 1 1 d U . . N1 N 0.3987(9) 0.2731(7) 0.6338(7) 0.0215(19) Uani 1 1 d . . . N6 N 1.5498(9) 1.1681(8) 1.0170(7) 0.0222(19) Uani 1 1 d . . . C19 C 1.5549(11) 1.0701(9) 0.8252(8) 0.022(2) Uani 1 1 d . . . H19 H 1.6498 1.1085 0.8327 0.027 Uiso 1 1 calc R . . C15 C 1.1837(11) 0.7765(8) 0.3844(8) 0.020(2) Uani 1 1 d . . . N4 N 1.2388(10) 0.8130(8) 0.3235(7) 0.032(2) Uani 1 1 d . . . C18 C 1.4876(10) 0.9938(9) 0.7271(8) 0.021(2) Uani 1 1 d . . . H18 H 1.5382 0.982 0.6689 0.025 Uiso 1 1 calc R . . C29 C 0.9415(12) 0.7690(9) 1.1056(8) 0.025(2) Uani 1 1 d . . . H29 H 0.9358 0.7766 1.1768 0.031 Uiso 1 1 calc R . . C10 C 0.4689(11) 0.3229(8) 0.4826(8) 0.020(2) Uani 1 1 d . . . H10 H 0.385 0.2735 0.4403 0.024 Uiso 1 1 calc R . . N3 N 0.9081(10) 0.5532(8) 0.2123(7) 0.026(2) Uani 1 1 d . . . C7 C 0.7235(10) 0.4749(8) 0.6099(8) 0.017(2) Uani 1 1 d . . . C5 C 0.4948(10) 0.3335(9) 0.5910(8) 0.020(2) Uani 1 1 d . . . C6 C 0.6248(11) 0.4103(9) 0.6520(8) 0.023(2) Uani 1 1 d . . . H6 H 0.6445 0.4177 0.7226 0.028 Uiso 1 1 calc R . . C13 C 0.9447(11) 0.5917(9) 0.3042(9) 0.022(2) Uani 1 1 d . . . C30 C 0.9742(12) 0.8644(10) 1.0799(9) 0.031(3) Uani 1 1 d . . . H30 H 0.9913 0.9376 1.133 0.037 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 0.0172(2) 0.0137(2) 0.0094(2) 0.00326(15) 0.00011(13) 0.00429(15) N2 0.032(3) 0.011(3) 0.012(3) 0.003(2) -0.007(2) 0.006(2) N7 0.011(4) 0.031(5) 0.020(5) 0.007(4) 0.007(3) 0.009(4) C21 0.022(5) 0.016(5) 0.020(5) 0.008(4) 0.007(4) 0.010(4) O3 0.019(4) 0.013(3) 0.016(4) 0.004(3) -0.001(3) -0.004(3) C14 0.019(5) 0.027(6) 0.015(5) 0.012(4) 0.003(4) 0.011(4) C12 0.031(3) 0.012(3) 0.012(3) 0.002(2) -0.006(2) 0.006(2) C27 0.026(6) 0.011(5) 0.018(5) -0.001(4) 0.001(4) 0.003(4) O4 0.025(3) 0.009(3) 0.011(3) -0.002(2) 0.001(2) 0.004(2) C4 0.019(5) 0.033(6) 0.024(6) 0.017(5) 0.002(4) 0.004(5) C11 0.021(4) 0.023(5) 0.011(5) 0.002(3) -0.002(3) 0.011(3) C17 0.021(5) 0.018(5) 0.020(5) 0.007(4) 0.003(4) 0.011(4) C16 0.034(6) 0.017(5) 0.014(5) 0.010(4) 0.012(4) 0.013(5) C25 0.026(6) 0.026(6) 0.017(5) 0.000(5) -0.008(4) 0.009(5) O1 0.016(3) 0.031(4) 0.008(3) 0.002(3) -0.005(3) -0.002(3) C8 0.018(5) 0.014(5) 0.016(5) 0.003(4) 0.004(4) 0.008(4) O2 0.014(3) 0.023(4) 0.004(3) -0.002(3) 0.000(3) -0.004(3) C3 0.026(6) 0.042(7) 0.029(6) 0.019(6) 0.005(5) 0.016(5) C9 0.024(5) 0.022(5) 0.016(5) 0.010(4) -0.004(4) 0.007(4) C26 0.020(5) 0.032(6) 0.027(6) 0.005(5) -0.004(5) 0.006(5) C20 0.027(6) 0.012(5) 0.014(5) 0.002(4) -0.001(4) 0.008(4) C28 0.036(6) 0.028(6) 0.019(6) 0.006(5) 0.002(5) 0.010(5) C1 0.035(7) 0.021(6) 0.041(7) 0.004(5) -0.003(6) 0.002(5) C31 0.036(6) 0.025(6) 0.006(5) 0.008(4) 0.009(4) 0.009(5) C2 0.016(5) 0.019(5) 0.034(6) 0.013(5) 0.004(4) 0.006(4) C24 0.025(6) 0.031(6) 0.030(6) 0.007(5) 0.001(5) 0.012(5) C23 0.033(6) 0.027(6) 0.018(5) 0.009(5) 0.002(5) 0.010(5) N5 0.023(4) 0.005(4) 0.015(4) 0.003(3) -0.001(3) -0.001(3) C22 0.025(3) 0.009(3) 0.011(3) -0.001(2) 0.001(2) 0.004(2) N1 0.019(4) 0.021(5) 0.027(5) 0.012(4) 0.004(4) 0.006(4) N6 0.022(5) 0.031(5) 0.016(4) 0.010(4) 0.001(4) 0.010(4) C19 0.016(5) 0.024(6) 0.024(6) 0.008(5) 0.003(4) 0.005(4) C15 0.022(5) 0.014(5) 0.018(5) 0.000(4) -0.002(4) 0.004(4) N4 0.040(6) 0.036(6) 0.019(5) 0.011(4) 0.004(4) 0.011(5) C18 0.019(5) 0.020(5) 0.026(6) 0.010(5) 0.012(4) 0.007(4) C29 0.038(7) 0.026(6) 0.016(5) 0.009(5) 0.010(5) 0.013(5) C10 0.025(5) 0.016(5) 0.013(5) -0.001(4) -0.001(4) 0.006(4) N3 0.040(6) 0.025(5) 0.010(5) 0.003(4) -0.004(4) 0.010(4) C7 0.018(5) 0.011(5) 0.020(5) 0.006(4) -0.005(4) 0.003(4) C5 0.018(5) 0.018(5) 0.025(6) 0.010(5) 0.002(4) 0.005(4) C6 0.023(5) 0.026(6) 0.014(5) 0.003(4) -0.007(4) 0.007(5) C13 0.027(6) 0.017(5) 0.024(6) 0.009(5) 0.005(5) 0.007(5) C30 0.040(7) 0.021(6) 0.028(6) 0.003(5) 0.015(5) 0.010(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O2 1.760(7) . ? U1 O1 1.772(7) . ? U1 O3 2.264(6) . ? U1 O4 2.277(6) . ? U1 N5 2.560(8) . ? U1 N2 2.598(8) . ? U1 N7 2.607(8) . ? N2 C12 1.357(13) . ? N2 C11 1.377(13) . ? N7 C31 1.338(13) . ? N7 C27 1.346(13) . ? C21 C22 1.388(14) . ? C21 C20 1.407(14) . ? C21 H21 0.93 . ? O3 C7 1.328(12) . ? C14 C12 1.340(15) . ? C14 N5 1.408(13) . ? C14 C15 1.446(13) . ? C12 C13 1.467(14) . ? C27 C28 1.394(14) . ? C27 H27 0.93 . ? O4 C22 1.315(12) . ? C4 N1 1.471(13) . ? C4 C3 1.535(15) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C11 C8 1.391(13) . ? C11 H11 0.93 . ? C17 C16 1.408(14) . ? C17 C18 1.430(14) . ? C17 C22 1.453(13) . ? C16 N5 1.310(13) . ? C16 H16 0.93 . ? C25 N6 1.467(14) . ? C25 C26 1.529(15) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C8 C9 1.432(14) . ? C8 C7 1.437(13) . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C9 C10 1.365(14) . ? C9 H9 0.93 . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C20 N6 1.349(13) . ? C20 C19 1.456(14) . ? C28 C29 1.395(15) . ? C28 H28 0.93 . ? C1 C2 1.506(15) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C31 C30 1.412(14) . ? C31 H31 0.93 . ? C2 N1 1.469(13) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C24 C23 1.519(14) . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C23 N6 1.487(13) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? N1 C5 1.353(12) . ? C19 C18 1.352(15) . ? C19 H19 0.93 . ? C15 N4 1.170(13) . ? C18 H18 0.93 . ? C29 C30 1.377(15) . ? C29 H29 0.93 . ? C10 C5 1.424(14) . ? C10 H10 0.93 . ? N3 C13 1.159(13) . ? C7 C6 1.391(14) . ? C5 C6 1.421(14) . ? C6 H6 0.93 . ? C30 H30 0.93 . ? 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 O2 U1 O1 177.9(3) . . ? O2 U1 O3 88.9(3) . . ? O1 U1 O3 92.0(3) . . ? O2 U1 O4 88.9(3) . . ? O1 U1 O4 89.5(3) . . ? O3 U1 O4 155.9(2) . . ? O2 U1 N5 81.3(3) . . ? O1 U1 N5 99.4(3) . . ? O3 U1 N5 132.5(2) . . ? O4 U1 N5 70.8(2) . . ? O2 U1 N2 98.7(3) . . ? O1 U1 N2 83.4(3) . . ? O3 U1 N2 71.6(2) . . ? O4 U1 N2 132.5(2) . . ? N5 U1 N2 64.3(3) . . ? O2 U1 N7 86.4(3) . . ? O1 U1 N7 91.9(3) . . ? O3 U1 N7 78.3(3) . . ? O4 U1 N7 77.6(3) . . ? N5 U1 N7 146.1(3) . . ? N2 U1 N7 149.3(3) . . ? C12 N2 C11 118.9(8) . . ? C12 N2 U1 116.8(6) . . ? C11 N2 U1 121.9(6) . . ? C31 N7 C27 118.0(9) . . ? C31 N7 U1 122.1(7) . . ? C27 N7 U1 119.7(7) . . ? C22 C21 C20 122.8(9) . . ? C22 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? C7 O3 U1 138.4(6) . . ? C12 C14 N5 119.7(9) . . ? C12 C14 C15 120.2(9) . . ? N5 C14 C15 120.0(9) . . ? C14 C12 N2 121.4(9) . . ? C14 C12 C13 118.1(9) . . ? N2 C12 C13 120.5(9) . . ? N7 C27 C28 122.4(10) . . ? N7 C27 H27 118.8 . . ? C28 C27 H27 118.8 . . ? C22 O4 U1 133.8(6) . . ? N1 C4 C3 113.8(9) . . ? N1 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? N1 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N2 C11 C8 128.9(9) . . ? N2 C11 H11 115.5 . . ? C8 C11 H11 115.5 . . ? C16 C17 C18 119.0(9) . . ? C16 C17 C22 124.7(9) . . ? C18 C17 C22 116.2(9) . . ? N5 C16 C17 128.1(9) . . ? N5 C16 H16 115.9 . . ? C17 C16 H16 115.9 . . ? N6 C25 C26 114.7(8) . . ? N6 C25 H25A 108.6 . . ? C26 C25 H25A 108.6 . . ? N6 C25 H25B 108.6 . . ? C26 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? C11 C8 C9 117.8(9) . . ? C11 C8 C7 125.9(9) . . ? C9 C8 C7 116.3(8) . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C10 C9 C8 123.3(9) . . ? C10 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N6 C20 C21 122.9(9) . . ? N6 C20 C19 120.4(9) . . ? C21 C20 C19 116.6(9) . . ? C29 C28 C27 119.0(10) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N7 C31 C30 123.1(10) . . ? N7 C31 H31 118.4 . . ? C30 C31 H31 118.4 . . ? N1 C2 C1 113.5(9) . . ? N1 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? N1 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N6 C23 C24 112.8(9) . . ? N6 C23 H23A 109 . . ? C24 C23 H23A 109 . . ? N6 C23 H23B 109 . . ? C24 C23 H23B 109 . . ? H23A C23 H23B 107.8 . . ? C16 N5 C14 117.8(8) . . ? C16 N5 U1 123.5(6) . . ? C14 N5 U1 117.2(6) . . ? O4 C22 C21 120.7(8) . . ? O4 C22 C17 119.0(8) . . ? C21 C22 C17 120.2(9) . . ? C5 N1 C2 122.2(9) . . ? C5 N1 C4 121.7(9) . . ? C2 N1 C4 116.1(8) . . ? C20 N6 C25 122.2(8) . . ? C20 N6 C23 121.6(9) . . ? C25 N6 C23 115.9(9) . . ? C18 C19 C20 120.9(9) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? N4 C15 C14 176.3(11) . . ? C19 C18 C17 123.2(9) . . ? C19 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? C30 C29 C28 119.2(10) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C9 C10 C5 120.5(9) . . ? C9 C10 H10 119.8 . . ? C5 C10 H10 119.8 . . ? O3 C7 C6 120.4(9) . . ? O3 C7 C8 119.4(8) . . ? C6 C7 C8 120.2(9) . . ? N1 C5 C6 121.6(9) . . ? N1 C5 C10 121.0(9) . . ? C6 C5 C10 117.4(9) . . ? C7 C6 C5 122.3(9) . . ? C7 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? N3 C13 C12 178.4(11) . . ? C29 C30 C31 118.1(10) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? 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 O2 U1 N2 C12 -82.3(7) . . . . ? O1 U1 N2 C12 97.4(7) . . . . ? O3 U1 N2 C12 -168.2(8) . . . . ? O4 U1 N2 C12 14.2(8) . . . . ? N5 U1 N2 C12 -6.4(7) . . . . ? N7 U1 N2 C12 180.0(6) . . . . ? O2 U1 N2 C11 115.6(7) . . . . ? O1 U1 N2 C11 -64.7(7) . . . . ? O3 U1 N2 C11 29.7(7) . . . . ? O4 U1 N2 C11 -147.9(6) . . . . ? N5 U1 N2 C11 -168.5(8) . . . . ? N7 U1 N2 C11 17.8(10) . . . . ? O2 U1 N7 C31 112.5(8) . . . . ? O1 U1 N7 C31 -66.2(8) . . . . ? O3 U1 N7 C31 -157.9(8) . . . . ? O4 U1 N7 C31 22.9(8) . . . . ? N5 U1 N7 C31 43.9(10) . . . . ? N2 U1 N7 C31 -146.4(7) . . . . ? O2 U1 N7 C27 -63.1(7) . . . . ? O1 U1 N7 C27 118.2(7) . . . . ? O3 U1 N7 C27 26.5(7) . . . . ? O4 U1 N7 C27 -152.7(8) . . . . ? N5 U1 N7 C27 -131.7(7) . . . . ? N2 U1 N7 C27 38.0(10) . . . . ? O2 U1 O3 C7 -142.6(9) . . . . ? O1 U1 O3 C7 39.3(9) . . . . ? O4 U1 O3 C7 132.6(9) . . . . ? N5 U1 O3 C7 -65.4(10) . . . . ? N2 U1 O3 C7 -43.0(9) . . . . ? N7 U1 O3 C7 130.8(9) . . . . ? N5 C14 C12 N2 -3.9(15) . . . . ? C15 C14 C12 N2 -179.8(9) . . . . ? N5 C14 C12 C13 175.8(9) . . . . ? C15 C14 C12 C13 0.0(15) . . . . ? C11 N2 C12 C14 170.9(9) . . . . ? U1 N2 C12 C14 8.2(13) . . . . ? C11 N2 C12 C13 -8.9(14) . . . . ? U1 N2 C12 C13 -171.5(7) . . . . ? C31 N7 C27 C28 -2.8(15) . . . . ? U1 N7 C27 C28 173.0(8) . . . . ? O2 U1 O4 C22 30.7(8) . . . . ? O1 U1 O4 C22 -150.6(8) . . . . ? O3 U1 O4 C22 115.5(9) . . . . ? N5 U1 O4 C22 -50.5(8) . . . . ? N2 U1 O4 C22 -70.1(9) . . . . ? N7 U1 O4 C22 117.3(8) . . . . ? C12 N2 C11 C8 178.7(10) . . . . ? U1 N2 C11 C8 -19.5(14) . . . . ? C18 C17 C16 N5 176.6(9) . . . . ? C22 C17 C16 N5 -8.2(16) . . . . ? N2 C11 C8 C9 178.3(9) . . . . ? N2 C11 C8 C7 -4.3(16) . . . . ? C11 C8 C9 C10 178.9(9) . . . . ? C7 C8 C9 C10 1.2(14) . . . . ? C22 C21 C20 N6 -178.4(9) . . . . ? C22 C21 C20 C19 -0.2(14) . . . . ? N7 C27 C28 C29 3.0(17) . . . . ? C27 N7 C31 C30 1.3(16) . . . . ? U1 N7 C31 C30 -174.3(8) . . . . ? C17 C16 N5 C14 174.7(9) . . . . ? C17 C16 N5 U1 -19.3(14) . . . . ? C12 C14 N5 C16 164.3(9) . . . . ? C15 C14 N5 C16 -19.8(13) . . . . ? C12 C14 N5 U1 -2.5(12) . . . . ? C15 C14 N5 U1 173.3(7) . . . . ? O2 U1 N5 C16 -57.5(7) . . . . ? O1 U1 N5 C16 120.6(8) . . . . ? O3 U1 N5 C16 -137.9(7) . . . . ? O4 U1 N5 C16 34.4(7) . . . . ? N2 U1 N5 C16 -161.6(8) . . . . ? N7 U1 N5 C16 12.6(10) . . . . ? O2 U1 N5 C14 108.6(7) . . . . ? O1 U1 N5 C14 -73.4(7) . . . . ? O3 U1 N5 C14 28.2(8) . . . . ? O4 U1 N5 C14 -159.5(7) . . . . ? N2 U1 N5 C14 4.5(6) . . . . ? N7 U1 N5 C14 178.7(6) . . . . ? U1 O4 C22 C21 -140.1(8) . . . . ? U1 O4 C22 C17 44.0(13) . . . . ? C20 C21 C22 O4 -176.0(9) . . . . ? C20 C21 C22 C17 -0.2(15) . . . . ? C16 C17 C22 O4 0.7(15) . . . . ? C18 C17 C22 O4 176.1(9) . . . . ? C16 C17 C22 C21 -175.2(9) . . . . ? C18 C17 C22 C21 0.1(14) . . . . ? C1 C2 N1 C5 95.4(12) . . . . ? C1 C2 N1 C4 -87.2(12) . . . . ? C3 C4 N1 C5 86.4(12) . . . . ? C3 C4 N1 C2 -91.1(11) . . . . ? C21 C20 N6 C25 -171.9(9) . . . . ? C19 C20 N6 C25 10.0(14) . . . . ? C21 C20 N6 C23 1.8(15) . . . . ? C19 C20 N6 C23 -176.4(9) . . . . ? C26 C25 N6 C20 69.6(13) . . . . ? C26 C25 N6 C23 -104.4(10) . . . . ? C24 C23 N6 C20 -89.2(12) . . . . ? C24 C23 N6 C25 84.9(11) . . . . ? N6 C20 C19 C18 178.9(10) . . . . ? C21 C20 C19 C18 0.6(15) . . . . ? C12 C14 C15 N4 63(17) . . . . ? N5 C14 C15 N4 -113(17) . . . . ? C20 C19 C18 C17 -0.7(16) . . . . ? C16 C17 C18 C19 175.9(10) . . . . ? C22 C17 C18 C19 0.3(15) . . . . ? C27 C28 C29 C30 -1.6(17) . . . . ? C8 C9 C10 C5 -1.3(15) . . . . ? U1 O3 C7 C6 -144.5(8) . . . . ? U1 O3 C7 C8 36.1(14) . . . . ? C11 C8 C7 O3 1.9(15) . . . . ? C9 C8 C7 O3 179.4(8) . . . . ? C11 C8 C7 C6 -177.5(9) . . . . ? C9 C8 C7 C6 0.0(14) . . . . ? C2 N1 C5 C6 167.9(9) . . . . ? C4 N1 C5 C6 -9.4(15) . . . . ? C2 N1 C5 C10 -11.7(15) . . . . ? C4 N1 C5 C10 171.0(9) . . . . ? C9 C10 C5 N1 179.8(9) . . . . ? C9 C10 C5 C6 0.1(15) . . . . ? O3 C7 C6 C5 179.5(9) . . . . ? C8 C7 C6 C5 -1.1(15) . . . . ? N1 C5 C6 C7 -178.6(9) . . . . ? C10 C5 C6 C7 1.0(15) . . . . ? C14 C12 C13 N3 -5E1(4) . . . . ? N2 C12 C13 N3 13E1(4) . . . . ? C28 C29 C30 C31 0.3(17) . . . . ? N7 C31 C30 C29 -0.1(17) . . . . ? #===END #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary _ccdc_compound_id 3 # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _ccdc_temp_data_collection 100(2) _ccdc_ls_R_squared 0.0456 #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ data_bcas061abs _database_code_depnum_ccdc_archive 'CCDC 802708' #TrackingRef '- salmntall.cif' _audit_creation_date 2009-06-01T04:43:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; '[UO2(salmnt(Et2N)2)(DMSO)]' ; _chemical_formula_sum 'C28 H34 N6 O5 S U' _chemical_formula_weight 804.7 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.491(5) _cell_length_b 11.801(5) _cell_length_c 12.408(5) _cell_angle_alpha 63.464(5) _cell_angle_beta 75.586(5) _cell_angle_gamma 85.808(5) _cell_volume 1456.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2628 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 23.84 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prismatic _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.433986 _exptl_absorpt_correction_T_max 0.89000 _exptl_absorpt_process_details SADABS #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_unetI/netI 0.0697 _diffrn_reflns_number 10565 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.33 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 5242 _reflns_number_gt 4599 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0484P)^2^+8.4080P] 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_number_reflns 5242 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.732 _refine_diff_density_min -3.156 _refine_diff_density_rms 0.18 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.20981(3) 0.06586(3) 1.16073(3) 0.01507(10) Uani 1 1 d . . . S1 S 0.18168(18) 0.03227(19) 1.47690(18) 0.0217(4) Uani 1 1 d . . . O4 O 0.0790(5) -0.0988(5) 1.2821(5) 0.0270(14) Uani 1 1 d . . . O3 O 0.3264(5) 0.2346(5) 1.1102(5) 0.0205(12) Uani 1 1 d . . . O5 O 0.1531(5) 0.0918(5) 1.3494(5) 0.0217(12) Uani 1 1 d . . . O1 O 0.3235(5) -0.0377(5) 1.2156(5) 0.0239(13) Uani 1 1 d . . . O2 O 0.0989(5) 0.1711(5) 1.0994(5) 0.0236(13) Uani 1 1 d . . . N5 N 0.1631(6) -0.0456(6) 1.0327(6) 0.0185(14) Uani 1 1 d . . . C18 C -0.0931(7) -0.2814(8) 1.2002(7) 0.0252(19) Uani 1 1 d . . . H18 H -0.0979 -0.292 1.1315 0.03 Uiso 1 1 calc R . . N1 N 0.6646(6) 0.4435(6) 1.1096(6) 0.0230(15) Uani 1 1 d . . . C10 C 0.4961(7) 0.3331(8) 1.1116(7) 0.0205(17) Uani 1 1 d . . . H10 H 0.4487 0.3536 1.1724 0.025 Uiso 1 1 calc R . . C24 C -0.2563(9) -0.6316(9) 1.5600(9) 0.037(2) Uani 1 1 d . . . H24A H -0.3151 -0.6931 1.5729 0.055 Uiso 1 1 calc R . . H24B H -0.2173 -0.6651 1.6274 0.055 Uiso 1 1 calc R . . H24C H -0.1976 -0.6126 1.4833 0.055 Uiso 1 1 calc R . . N2 N 0.3567(6) 0.1248(6) 0.9496(6) 0.0181(14) Uani 1 1 d . . . N6 N -0.2326(6) -0.4146(7) 1.5343(6) 0.0273(16) Uani 1 1 d . . . C23 C -0.3172(8) -0.5129(9) 1.5541(9) 0.033(2) Uani 1 1 d . . . H23A H -0.3579 -0.4805 1.487 0.04 Uiso 1 1 calc R . . H23B H -0.3775 -0.533 1.631 0.04 Uiso 1 1 calc R . . C12 C 0.3282(7) 0.0813(8) 0.8713(7) 0.0194(17) Uani 1 1 d . . . C20 C -0.1595(8) -0.3433(8) 1.4206(8) 0.0260(19) Uani 1 1 d . . . C16 C 0.0726(7) -0.1279(7) 1.0659(7) 0.0171(16) Uani 1 1 d . . . H16 H 0.0598 -0.1454 1.0036 0.021 Uiso 1 1 calc R . . C22 C -0.0002(7) -0.1794(7) 1.2902(7) 0.0184(17) Uani 1 1 d . . . C27 C 0.3406(8) 0.0303(10) 1.4485(9) 0.039(2) Uani 1 1 d . . . H27A H 0.3734 0.1153 1.4137 0.059 Uiso 1 1 calc R . . H27B H 0.3713 -0.0052 1.3914 0.059 Uiso 1 1 calc R . . H27C H 0.3632 -0.0203 1.5252 0.059 Uiso 1 1 calc R . . C9 C 0.4436(7) 0.2651(7) 1.0694(7) 0.0201(17) Uani 1 1 d . . . C14 C 0.2327(7) -0.0014(7) 0.9120(7) 0.0204(17) Uani 1 1 d . . . C3 C 0.8731(8) 0.4199(9) 1.1380(8) 0.032(2) Uani 1 1 d . . . H3A H 0.9522 0.4599 1.1003 0.048 Uiso 1 1 calc R . . H3B H 0.8754 0.336 1.1434 0.048 Uiso 1 1 calc R . . H3C H 0.846 0.4148 1.2198 0.048 Uiso 1 1 calc R . . C7 C 0.6374(7) 0.2738(8) 0.9302(7) 0.0223(18) Uani 1 1 d . . . H7 H 0.6853 0.2548 0.8685 0.027 Uiso 1 1 calc R . . C1 C 0.5766(8) 0.3525(9) 1.3374(8) 0.029(2) Uani 1 1 d . . . H1A H 0.5291 0.3749 1.4 0.044 Uiso 1 1 calc R . . H1B H 0.6536 0.3261 1.355 0.044 Uiso 1 1 calc R . . H1C H 0.5361 0.2844 1.337 0.044 Uiso 1 1 calc R . . C2 C 0.5941(7) 0.4667(8) 1.2112(7) 0.0233(18) Uani 1 1 d . . . H2A H 0.5158 0.494 1.1955 0.028 Uiso 1 1 calc R . . H2B H 0.6332 0.5355 1.2134 0.028 Uiso 1 1 calc R . . C21 C -0.0730(7) -0.2549(8) 1.4051(8) 0.0247(19) Uani 1 1 d . . . H21 H -0.0647 -0.2474 1.4743 0.03 Uiso 1 1 calc R . . C11 C 0.4664(7) 0.1752(8) 0.9165(7) 0.0214(18) Uani 1 1 d . . . H11 H 0.5179 0.1713 0.8475 0.026 Uiso 1 1 calc R . . C8 C 0.5144(7) 0.2342(7) 0.9737(7) 0.0181(17) Uani 1 1 d . . . C5 C 0.6184(7) 0.3733(7) 1.0669(7) 0.0197(17) Uani 1 1 d . . . C17 C -0.0062(7) -0.1917(7) 1.1840(7) 0.0172(16) Uani 1 1 d . . . C25 C -0.2145(8) -0.4103(8) 1.6457(8) 0.027(2) Uani 1 1 d . . . H25A H -0.284 -0.4508 1.714 0.033 Uiso 1 1 calc R . . H25B H -0.2091 -0.3224 1.6302 0.033 Uiso 1 1 calc R . . C15 C 0.2119(7) -0.0465(8) 0.8282(8) 0.0223(18) Uani 1 1 d . . . C19 C -0.1694(8) -0.3525(8) 1.3114(8) 0.028(2) Uani 1 1 d . . . H19 H -0.2276 -0.4067 1.3169 0.033 Uiso 1 1 calc R . . C4 C 0.7882(7) 0.4964(8) 1.0603(8) 0.0248(19) Uani 1 1 d . . . H4A H 0.7882 0.5815 1.0536 0.03 Uiso 1 1 calc R . . H4B H 0.8175 0.5028 0.9773 0.03 Uiso 1 1 calc R . . C6 C 0.6884(7) 0.3386(8) 0.9751(7) 0.0238(19) Uani 1 1 d . . . H6 H 0.7703 0.3606 0.9454 0.029 Uiso 1 1 calc R . . C28 C 0.1487(8) -0.1325(8) 1.5387(8) 0.029(2) Uani 1 1 d . . . H28A H 0.0632 -0.1478 1.5597 0.043 Uiso 1 1 calc R . . H28B H 0.1786 -0.1772 1.6118 0.043 Uiso 1 1 calc R . . H28C H 0.1863 -0.1618 1.478 0.043 Uiso 1 1 calc R . . C13 C 0.3969(7) 0.1270(8) 0.7428(8) 0.0257(19) Uani 1 1 d . . . N4 N 0.1990(7) -0.0822(7) 0.7604(7) 0.0315(18) Uani 1 1 d . . . N3 N 0.4495(7) 0.1658(8) 0.6428(7) 0.0350(19) Uani 1 1 d . . . C26 C -0.1028(8) -0.4745(9) 1.6836(8) 0.036(2) Uani 1 1 d . . . H26A H -0.0957 -0.4684 1.7563 0.054 Uiso 1 1 calc R . . H26B H -0.0333 -0.4338 1.6172 0.054 Uiso 1 1 calc R . . H26C H -0.1083 -0.5622 1.7013 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 U1 0.01505(15) 0.01446(16) 0.01401(15) -0.00552(11) -0.00085(10) -0.00414(10) S1 0.0254(11) 0.0198(11) 0.0210(10) -0.0112(9) -0.0030(8) -0.0007(8) O4 0.036(3) 0.021(3) 0.021(3) -0.007(3) -0.002(3) -0.014(3) O3 0.015(3) 0.021(3) 0.025(3) -0.013(2) 0.003(2) -0.003(2) O5 0.026(3) 0.024(3) 0.016(3) -0.010(2) -0.004(2) -0.001(2) O1 0.031(3) 0.022(3) 0.013(3) -0.004(2) -0.004(2) -0.002(3) O2 0.026(3) 0.022(3) 0.020(3) -0.007(3) -0.003(2) -0.002(2) N5 0.021(3) 0.016(3) 0.014(3) -0.003(3) -0.002(3) -0.006(3) C18 0.031(5) 0.028(5) 0.016(4) -0.003(4) -0.013(4) -0.012(4) N1 0.016(3) 0.026(4) 0.023(4) -0.009(3) 0.000(3) -0.010(3) C10 0.011(4) 0.025(4) 0.023(4) -0.011(4) 0.003(3) -0.007(3) C24 0.038(5) 0.032(6) 0.029(5) -0.007(4) -0.001(4) -0.005(4) N2 0.020(3) 0.022(4) 0.016(3) -0.011(3) -0.004(3) -0.004(3) N6 0.027(4) 0.024(4) 0.026(4) -0.010(3) 0.001(3) -0.008(3) C23 0.027(5) 0.040(6) 0.032(5) -0.016(4) -0.004(4) -0.002(4) C12 0.016(4) 0.027(5) 0.018(4) -0.014(4) -0.002(3) 0.001(3) C20 0.028(5) 0.019(4) 0.023(4) -0.003(4) -0.002(4) -0.008(4) C16 0.023(4) 0.011(4) 0.019(4) -0.006(3) -0.010(3) 0.003(3) C22 0.024(4) 0.013(4) 0.018(4) -0.005(3) -0.009(3) 0.003(3) C27 0.027(5) 0.058(7) 0.038(6) -0.024(5) -0.011(4) -0.004(5) C9 0.022(4) 0.014(4) 0.018(4) 0.001(3) -0.010(3) -0.001(3) C14 0.028(4) 0.017(4) 0.017(4) -0.009(3) -0.004(3) -0.001(3) C3 0.024(5) 0.038(6) 0.028(5) -0.011(4) -0.002(4) -0.004(4) C7 0.020(4) 0.026(5) 0.014(4) -0.006(4) 0.002(3) -0.005(3) C1 0.023(4) 0.037(5) 0.025(5) -0.014(4) -0.001(4) 0.004(4) C2 0.020(4) 0.023(5) 0.029(5) -0.015(4) 0.000(4) -0.006(3) C21 0.028(5) 0.025(5) 0.019(4) -0.008(4) -0.002(4) -0.007(4) C11 0.021(4) 0.022(4) 0.015(4) -0.005(3) -0.001(3) 0.004(3) C8 0.018(4) 0.018(4) 0.012(4) -0.002(3) -0.001(3) -0.006(3) C5 0.015(4) 0.020(4) 0.022(4) -0.008(3) -0.002(3) -0.004(3) C17 0.020(4) 0.014(4) 0.017(4) -0.007(3) -0.002(3) -0.002(3) C25 0.028(5) 0.026(5) 0.023(4) -0.011(4) 0.004(4) -0.008(4) C15 0.021(4) 0.025(5) 0.024(4) -0.013(4) -0.005(3) -0.003(3) C19 0.030(5) 0.025(5) 0.026(5) -0.008(4) -0.007(4) -0.008(4) C4 0.022(4) 0.027(5) 0.021(4) -0.007(4) -0.002(3) -0.009(4) C6 0.012(4) 0.026(5) 0.017(4) 0.000(4) 0.006(3) -0.004(3) C28 0.033(5) 0.027(5) 0.025(5) -0.007(4) -0.010(4) -0.006(4) C13 0.020(4) 0.032(5) 0.023(5) -0.009(4) -0.005(4) -0.004(4) N4 0.031(4) 0.039(5) 0.024(4) -0.016(4) 0.000(3) -0.008(3) N3 0.028(4) 0.052(5) 0.020(4) -0.013(4) 0.003(3) -0.011(4) C26 0.027(5) 0.043(6) 0.027(5) -0.008(4) 0.004(4) -0.016(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.769(6) . ? U1 O2 1.776(6) . ? U1 O4 2.233(5) . ? U1 O3 2.238(5) . ? U1 O5 2.419(5) . ? U1 N2 2.557(6) . ? U1 N5 2.634(6) . ? S1 O5 1.528(6) . ? S1 C27 1.772(9) . ? S1 C28 1.773(9) . ? O4 C22 1.318(9) . ? O3 C9 1.330(9) . ? N5 C16 1.331(10) . ? N5 C14 1.386(10) . ? C18 C19 1.359(11) . ? C18 C17 1.421(10) . ? C18 H18 0.93 . ? N1 C5 1.359(10) . ? N1 C2 1.444(10) . ? N1 C4 1.462(10) . ? C10 C9 1.373(11) . ? C10 C5 1.408(10) . ? C10 H10 0.93 . ? C24 C23 1.499(13) . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? N2 C11 1.321(10) . ? N2 C12 1.394(10) . ? N6 C20 1.362(10) . ? N6 C23 1.464(11) . ? N6 C25 1.471(11) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C12 C14 1.360(11) . ? C12 C13 1.458(11) . ? C20 C21 1.411(11) . ? C20 C19 1.438(12) . ? C16 C17 1.410(11) . ? C16 H16 0.93 . ? C22 C21 1.381(11) . ? C22 C17 1.408(10) . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? C9 C8 1.438(11) . ? C14 C15 1.435(11) . ? C3 C4 1.503(12) . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C7 C6 1.359(12) . ? C7 C8 1.415(11) . ? C7 H7 0.93 . ? C1 C2 1.518(11) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C21 H21 0.93 . ? C11 C8 1.408(11) . ? C11 H11 0.93 . ? C5 C6 1.423(11) . ? C25 C26 1.511(12) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C15 N4 1.138(10) . ? C19 H19 0.93 . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C6 H6 0.93 . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C13 N3 1.128(11) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? 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 O2 177.7(3) . . ? O1 U1 O4 87.0(2) . . ? O2 U1 O4 94.3(2) . . ? O1 U1 O3 91.0(2) . . ? O2 U1 O3 88.6(2) . . ? O4 U1 O3 157.4(2) . . ? O1 U1 O5 91.0(2) . . ? O2 U1 O5 91.1(2) . . ? O4 U1 O5 79.10(19) . . ? O3 U1 O5 78.46(18) . . ? O1 U1 N2 82.9(2) . . ? O2 U1 N2 94.8(2) . . ? O4 U1 N2 131.7(2) . . ? O3 U1 N2 70.17(19) . . ? O5 U1 N2 147.86(19) . . ? O1 U1 N5 94.8(2) . . ? O2 U1 N5 83.8(2) . . ? O4 U1 N5 69.3(2) . . ? O3 U1 N5 133.26(19) . . ? O5 U1 N5 147.45(19) . . ? N2 U1 N5 64.69(19) . . ? O5 S1 C27 106.1(4) . . ? O5 S1 C28 105.5(4) . . ? C27 S1 C28 99.1(5) . . ? C22 O4 U1 147.9(5) . . ? C9 O3 U1 136.0(5) . . ? S1 O5 U1 137.6(3) . . ? C16 N5 C14 117.0(7) . . ? C16 N5 U1 127.3(5) . . ? C14 N5 U1 115.3(5) . . ? C19 C18 C17 123.1(8) . . ? C19 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? C5 N1 C2 121.2(6) . . ? C5 N1 C4 123.1(7) . . ? C2 N1 C4 115.6(6) . . ? C9 C10 C5 123.0(8) . . ? C9 C10 H10 118.5 . . ? C5 C10 H10 118.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C11 N2 C12 116.3(7) . . ? C11 N2 U1 125.0(5) . . ? C12 N2 U1 117.8(5) . . ? C20 N6 C23 121.8(7) . . ? C20 N6 C25 120.4(7) . . ? C23 N6 C25 116.9(7) . . ? N6 C23 C24 112.4(7) . . ? N6 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N6 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C14 C12 N2 120.6(7) . . ? C14 C12 C13 118.5(7) . . ? N2 C12 C13 120.8(7) . . ? N6 C20 C21 121.0(8) . . ? N6 C20 C19 121.7(7) . . ? C21 C20 C19 117.4(7) . . ? N5 C16 C17 127.9(7) . . ? N5 C16 H16 116.1 . . ? C17 C16 H16 116.1 . . ? O4 C22 C21 118.9(7) . . ? O4 C22 C17 120.2(7) . . ? C21 C22 C17 120.8(7) . . ? S1 C27 H27A 109.5 . . ? S1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O3 C9 C10 120.8(7) . . ? O3 C9 C8 119.5(7) . . ? C10 C9 C8 119.6(7) . . ? C12 C14 N5 120.7(7) . . ? C12 C14 C15 117.5(7) . . ? N5 C14 C15 121.7(7) . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C7 C8 122.5(8) . . ? C6 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 114.2(7) . . ? N1 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? N1 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C22 C21 C20 122.0(8) . . ? C22 C21 H21 119 . . ? C20 C21 H21 119 . . ? N2 C11 C8 127.5(7) . . ? N2 C11 H11 116.2 . . ? C8 C11 H11 116.2 . . ? C11 C8 C7 119.1(7) . . ? C11 C8 C9 123.8(7) . . ? C7 C8 C9 117.0(7) . . ? N1 C5 C10 120.4(7) . . ? N1 C5 C6 122.8(7) . . ? C10 C5 C6 116.8(7) . . ? C22 C17 C16 124.5(7) . . ? C22 C17 C18 117.0(7) . . ? C16 C17 C18 118.3(7) . . ? N6 C25 C26 113.3(7) . . ? N6 C25 H25A 108.9 . . ? C26 C25 H25A 108.9 . . ? N6 C25 H25B 108.9 . . ? C26 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? N4 C15 C14 178.0(9) . . ? C18 C19 C20 119.7(8) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? N1 C4 C3 113.9(7) . . ? N1 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? N1 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C7 C6 C5 121.0(7) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? S1 C28 H28A 109.5 . . ? S1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C13 C12 178.1(10) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 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 O4 C22 -115.7(10) . . . . ? O2 U1 O4 C22 62.3(10) . . . . ? O3 U1 O4 C22 158.9(9) . . . . ? O5 U1 O4 C22 152.7(10) . . . . ? N2 U1 O4 C22 -38.0(11) . . . . ? N5 U1 O4 C22 -19.4(10) . . . . ? O1 U1 O3 C9 33.2(7) . . . . ? O2 U1 O3 C9 -144.5(7) . . . . ? O4 U1 O3 C9 117.8(8) . . . . ? O5 U1 O3 C9 124.1(7) . . . . ? N2 U1 O3 C9 -48.8(7) . . . . ? N5 U1 O3 C9 -64.4(8) . . . . ? C27 S1 O5 U1 49.4(6) . . . . ? C28 S1 O5 U1 -55.1(6) . . . . ? O1 U1 O5 S1 -9.3(5) . . . . ? O2 U1 O5 S1 171.5(5) . . . . ? O4 U1 O5 S1 77.4(5) . . . . ? O3 U1 O5 S1 -100.2(5) . . . . ? N2 U1 O5 S1 -87.5(6) . . . . ? N5 U1 O5 S1 91.3(6) . . . . ? O1 U1 N5 C16 100.3(6) . . . . ? O2 U1 N5 C16 -81.6(6) . . . . ? O4 U1 N5 C16 15.4(6) . . . . ? O3 U1 N5 C16 -163.7(6) . . . . ? O5 U1 N5 C16 0.8(8) . . . . ? N2 U1 N5 C16 -179.9(7) . . . . ? O1 U1 N5 C14 -88.0(6) . . . . ? O2 U1 N5 C14 90.1(5) . . . . ? O4 U1 N5 C14 -172.9(6) . . . . ? O3 U1 N5 C14 7.9(7) . . . . ? O5 U1 N5 C14 172.5(5) . . . . ? N2 U1 N5 C14 -8.2(5) . . . . ? O1 U1 N2 C11 -61.6(6) . . . . ? O2 U1 N2 C11 118.8(6) . . . . ? O4 U1 N2 C11 -141.1(6) . . . . ? O3 U1 N2 C11 32.0(6) . . . . ? O5 U1 N2 C11 18.9(8) . . . . ? N5 U1 N2 C11 -160.4(7) . . . . ? O1 U1 N2 C12 106.6(6) . . . . ? O2 U1 N2 C12 -73.0(6) . . . . ? O4 U1 N2 C12 27.1(7) . . . . ? O3 U1 N2 C12 -159.7(6) . . . . ? O5 U1 N2 C12 -172.9(5) . . . . ? N5 U1 N2 C12 7.8(5) . . . . ? C20 N6 C23 C24 77.2(11) . . . . ? C25 N6 C23 C24 -92.6(9) . . . . ? C11 N2 C12 C14 162.0(8) . . . . ? U1 N2 C12 C14 -7.2(10) . . . . ? C11 N2 C12 C13 -20.4(11) . . . . ? U1 N2 C12 C13 170.3(6) . . . . ? C23 N6 C20 C21 -175.7(8) . . . . ? C25 N6 C20 C21 -6.3(13) . . . . ? C23 N6 C20 C19 5.9(13) . . . . ? C25 N6 C20 C19 175.4(8) . . . . ? C14 N5 C16 C17 176.1(7) . . . . ? U1 N5 C16 C17 -12.4(11) . . . . ? U1 O4 C22 C21 -168.7(7) . . . . ? U1 O4 C22 C17 14.2(15) . . . . ? U1 O3 C9 C10 -141.5(6) . . . . ? U1 O3 C9 C8 42.9(10) . . . . ? C5 C10 C9 O3 -176.8(7) . . . . ? C5 C10 C9 C8 -1.1(12) . . . . ? N2 C12 C14 N5 -1.2(12) . . . . ? C13 C12 C14 N5 -178.7(7) . . . . ? N2 C12 C14 C15 -177.3(7) . . . . ? C13 C12 C14 C15 5.1(12) . . . . ? C16 N5 C14 C12 -178.9(7) . . . . ? U1 N5 C14 C12 8.5(10) . . . . ? C16 N5 C14 C15 -2.9(11) . . . . ? U1 N5 C14 C15 -175.5(6) . . . . ? C5 N1 C2 C1 73.6(10) . . . . ? C4 N1 C2 C1 -104.3(8) . . . . ? O4 C22 C21 C20 -179.9(8) . . . . ? C17 C22 C21 C20 -2.8(13) . . . . ? N6 C20 C21 C22 -178.3(8) . . . . ? C19 C20 C21 C22 0.2(13) . . . . ? C12 N2 C11 C8 174.9(8) . . . . ? U1 N2 C11 C8 -16.7(12) . . . . ? N2 C11 C8 C7 175.1(8) . . . . ? N2 C11 C8 C9 -9.4(13) . . . . ? C6 C7 C8 C11 175.6(8) . . . . ? C6 C7 C8 C9 -0.2(12) . . . . ? O3 C9 C8 C11 1.8(12) . . . . ? C10 C9 C8 C11 -173.9(8) . . . . ? O3 C9 C8 C7 177.3(7) . . . . ? C10 C9 C8 C7 1.6(11) . . . . ? C2 N1 C5 C10 7.1(12) . . . . ? C4 N1 C5 C10 -175.1(7) . . . . ? C2 N1 C5 C6 -174.0(7) . . . . ? C4 N1 C5 C6 3.8(12) . . . . ? C9 C10 C5 N1 178.1(8) . . . . ? C9 C10 C5 C6 -0.9(12) . . . . ? O4 C22 C17 C16 3.8(12) . . . . ? C21 C22 C17 C16 -173.3(8) . . . . ? O4 C22 C17 C18 179.4(7) . . . . ? C21 C22 C17 C18 2.3(12) . . . . ? N5 C16 C17 C22 -1.0(13) . . . . ? N5 C16 C17 C18 -176.6(8) . . . . ? C19 C18 C17 C22 0.8(13) . . . . ? C19 C18 C17 C16 176.7(8) . . . . ? C20 N6 C25 C26 -71.3(10) . . . . ? C23 N6 C25 C26 98.7(9) . . . . ? C12 C14 C15 N4 4E1(3) . . . . ? N5 C14 C15 N4 -14E1(3) . . . . ? C17 C18 C19 C20 -3.4(14) . . . . ? N6 C20 C19 C18 -178.7(8) . . . . ? C21 C20 C19 C18 2.9(13) . . . . ? C5 N1 C4 C3 -99.2(9) . . . . ? C2 N1 C4 C3 78.7(9) . . . . ? C8 C7 C6 C5 -1.9(13) . . . . ? N1 C5 C6 C7 -176.6(8) . . . . ? C10 C5 C6 C7 2.4(12) . . . . ? C14 C12 C13 N3 12E1(3) . . . . ? N2 C12 C13 N3 -6E1(3) . . . . ? #===END #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary _ccdc_compound_id 4 # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _ccdc_temp_data_collection 100(2) _ccdc_ls_R_squared 0.0722 _ccdc_disorder ; Ethyl arm containing atoms C3 and C4 is disordered over two sites with 65.7 % occupancy on site A and 34.3 % occupancy on site B. Atoms C27, C28 and C29 of the coordinated DMF molecule are disordered over two sites with 62.3 % occupancy on site A and 37.7 % occupancy on site B. ; #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ data_bcas071p21ca _database_code_depnum_ccdc_archive 'CCDC 802709' #TrackingRef '- salmntall.cif' _audit_creation_date 2009-07-21T13:56:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; '[UO2(salmnt(Et2N)2)(DMF)]' ; _chemical_formula_sum 'C29 H35 N7 O5 U' _chemical_formula_weight 799.67 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.364(5) _cell_length_b 22.050(5) _cell_length_c 11.064(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 99.161(5) _cell_angle_gamma 90.000(5) _cell_volume 2977.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1009 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 15.60 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour 'dark purple' _exptl_crystal_size_min 0.01 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.333420 _exptl_absorpt_correction_T_max 0.946000 _exptl_absorpt_process_details SADABS #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.13 _diffrn_reflns_av_unetI/netI 0.1242 _diffrn_reflns_number 21018 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.21 _diffrn_reflns_theta_full 25.21 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 5309 _reflns_number_gt 3577 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0434P)^2^+19.3158P] 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_number_reflns 5309 _refine_ls_number_parameters 376 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1207 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.1368 _refine_ls_wR_factor_gt 0.1218 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.189 _refine_diff_density_min -2.637 _refine_diff_density_rms 0.208 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.68777(4) 0.08061(2) 0.27693(4) 0.01990(15) Uani 1 1 d . B . O1 O 0.7597(7) 0.0430(4) 0.1711(7) 0.027(2) Uani 1 1 d . . . O5 O 0.5466(7) 0.0047(4) 0.2531(9) 0.034(2) Uani 1 1 d . . . N6 N 0.3677(8) 0.1649(5) -0.2782(9) 0.025(3) Uani 1 1 d . . . C11 C 0.9271(11) 0.0968(5) 0.5001(11) 0.022(3) Uani 1 1 d . B . H11 H 0.9879 0.1189 0.5359 0.026 Uiso 1 1 calc R . . C16 C 0.7227(10) 0.2098(6) 0.0951(12) 0.025(3) Uani 1 1 d . B . H16 H 0.7631 0.2436 0.0785 0.03 Uiso 1 1 calc R . . N1 N 0.8798(9) -0.1119(5) 0.7692(10) 0.030(3) Uani 1 1 d U . . C20 C 0.4527(11) 0.1722(6) -0.1843(12) 0.027(3) Uani 1 1 d . B . C1 C 0.6813(13) -0.1298(6) 0.7809(14) 0.041(4) Uani 1 1 d . . . H1A H 0.6247 -0.1597 0.7628 0.061 Uiso 1 1 calc R A . H1B H 0.6596 -0.0934 0.7359 0.061 Uiso 1 1 calc R . . H1C H 0.6929 -0.1211 0.867 0.061 Uiso 1 1 calc R . . O3 O 0.7530(7) 0.0126(4) 0.4229(8) 0.024(2) Uani 1 1 d . . . C18 C 0.6190(10) 0.2279(6) -0.1066(12) 0.026(3) Uani 1 1 d . B . H18 H 0.6697 0.2579 -0.1167 0.031 Uiso 1 1 calc R . . C19 C 0.5362(10) 0.2179(6) -0.1970(12) 0.027(3) Uani 1 1 d . . . H19 H 0.5312 0.2402 -0.269 0.033 Uiso 1 1 calc R . . O2 O 0.6208(7) 0.1216(4) 0.3829(7) 0.026(2) Uani 1 1 d . . . C8 C 0.9129(10) 0.0424(5) 0.5577(10) 0.018(3) Uani 1 1 d . . . C10 C 0.8155(11) -0.0503(6) 0.5926(12) 0.025(3) Uani 1 1 d . . . H10 H 0.7591 -0.0777 0.5682 0.03 Uiso 1 1 calc R A . C6 C 0.9800(12) -0.0213(6) 0.7332(12) 0.030(3) Uani 1 1 d . . . H6 H 1.0323 -0.0291 0.8016 0.037 Uiso 1 1 calc R A . N2 N 0.8694(8) 0.1229(5) 0.4033(9) 0.022(2) Uani 1 1 d . . . C25 C 0.3528(11) 0.2030(6) -0.3859(12) 0.033(3) Uani 1 1 d . . . H25A H 0.3717 0.2445 -0.3619 0.039 Uiso 1 1 calc R . . H25B H 0.2762 0.2024 -0.423 0.039 Uiso 1 1 calc R . . O4 O 0.5643(7) 0.1162(4) 0.1200(8) 0.027(2) Uani 1 1 d . . . C23 C 0.2747(11) 0.1272(6) -0.2601(12) 0.028(3) Uani 1 1 d . . . H23A H 0.3011 0.0924 -0.2105 0.033 Uiso 1 1 calc R . . H23B H 0.2387 0.1124 -0.3389 0.033 Uiso 1 1 calc R . . C26 C 0.4224(12) 0.1827(7) -0.4799(13) 0.039(4) Uani 1 1 d . . . H26A H 0.4095 0.2091 -0.5498 0.058 Uiso 1 1 calc R . . H26B H 0.4032 0.1419 -0.505 0.058 Uiso 1 1 calc R . . H26C H 0.4984 0.1843 -0.4444 0.058 Uiso 1 1 calc R . . C14 C 0.8446(11) 0.2097(6) 0.2713(12) 0.025(3) Uani 1 1 d . . . C12 C 0.9026(11) 0.1800(6) 0.3707(12) 0.024(3) Uani 1 1 d U B . C24 C 0.1929(11) 0.1610(6) -0.1987(11) 0.031(3) Uani 1 1 d . . . H24A H 0.1333 0.1345 -0.1889 0.047 Uiso 1 1 calc R . . H24B H 0.1654 0.1951 -0.2482 0.047 Uiso 1 1 calc R . . H24C H 0.2277 0.175 -0.1199 0.047 Uiso 1 1 calc R . . N5 N 0.7563(8) 0.1820(5) 0.2001(9) 0.020(2) Uani 1 1 d . B . C5 C 0.8898(11) -0.0618(5) 0.6993(12) 0.023(3) Uani 1 1 d . A . N7 N 0.3822(9) -0.0410(5) 0.2299(11) 0.033(3) Uani 1 1 d . . . C9 C 0.8239(11) 0.0015(6) 0.5220(11) 0.026(3) Uani 1 1 d . A . C7 C 0.9874(10) 0.0271(6) 0.6661(11) 0.024(3) Uani 1 1 d . A . H7 H 1.0455 0.0534 0.6907 0.028 Uiso 1 1 calc R . . C21 C 0.4658(10) 0.1400(6) -0.0749(11) 0.024(3) Uani 1 1 d . . . H21 H 0.4128 0.1114 -0.0642 0.029 Uiso 1 1 calc R B . C15 C 0.8809(11) 0.2701(6) 0.2476(11) 0.024(3) Uani 1 1 d . B . C2 C 0.7877(11) -0.1539(6) 0.7441(12) 0.029(3) Uani 1 1 d . A . H2A H 0.8073 -0.1915 0.7878 0.035 Uiso 1 1 calc R . . H2B H 0.7748 -0.1631 0.6573 0.035 Uiso 1 1 calc R . . C22 C 0.5538(11) 0.1480(6) 0.0197(12) 0.025(3) Uani 1 1 d . B . C3A C 0.9438(19) -0.0845(11) 0.982(2) 0.044(6) Uiso 0.66(2) 1 d P A 1 H3A1 H 1.0003 -0.0913 1.0509 0.066 Uiso 0.66(2) 1 calc PR A 1 H3A2 H 0.874 -0.0949 1.0039 0.066 Uiso 0.66(2) 1 calc PR A 1 H3A3 H 0.9436 -0.0425 0.9589 0.066 Uiso 0.66(2) 1 calc PR A 1 C4A C 0.965(2) -0.1244(11) 0.873(2) 0.037(7) Uiso 0.66(2) 1 d P A 1 H4A1 H 1.0368 -0.1151 0.8522 0.044 Uiso 0.66(2) 1 calc PR A 1 H4A2 H 0.9644 -0.1669 0.8955 0.044 Uiso 0.66(2) 1 calc PR A 1 C4B C 0.922(4) -0.110(2) 0.911(4) 0.029(3) Uiso 0.34(2) 1 d PU A 2 H4B1 H 0.9247 -0.0685 0.94 0.035 Uiso 0.34(2) 1 calc PR A 2 H4B2 H 0.8724 -0.1327 0.9541 0.035 Uiso 0.34(2) 1 calc PR A 2 C3B C 1.034(3) -0.1379(18) 0.933(4) 0.030(3) Uiso 0.34(2) 1 d PU A 2 H3B1 H 1.0614 -0.1377 1.0195 0.044 Uiso 0.34(2) 1 calc PR A 2 H3B2 H 1.0823 -0.1148 0.8912 0.044 Uiso 0.34(2) 1 calc PR A 2 H3B3 H 1.0302 -0.1788 0.9036 0.044 Uiso 0.34(2) 1 calc PR A 2 C17 C 0.6331(10) 0.1944(6) 0.0055(11) 0.023(3) Uani 1 1 d . . . C27A C 0.4576(16) -0.0051(9) 0.1881(19) 0.022(6) Uiso 0.62(2) 1 d P B 3 H27A H 0.4421 0.0121 0.1105 0.026 Uiso 0.62(2) 1 calc PR B 3 C28A C 0.3924(17) -0.0664(9) 0.3446(18) 0.023(6) Uiso 0.62(2) 1 d P B 3 H28A H 0.328 -0.0897 0.3511 0.035 Uiso 0.62(2) 1 calc PR B 3 H28B H 0.4008 -0.0349 0.4052 0.035 Uiso 0.62(2) 1 calc PR B 3 H28C H 0.4554 -0.0924 0.3574 0.035 Uiso 0.62(2) 1 calc PR B 3 C29A C 0.278(2) -0.0507(12) 0.144(2) 0.042(7) Uiso 0.62(2) 1 d P B 3 H29A H 0.2306 -0.0765 0.1823 0.063 Uiso 0.62(2) 1 calc PR B 3 H29B H 0.2934 -0.0696 0.0707 0.063 Uiso 0.62(2) 1 calc PR B 3 H29C H 0.2427 -0.0124 0.1247 0.063 Uiso 0.62(2) 1 calc PR B 3 C27B C 0.482(3) -0.0250(18) 0.295(4) 0.041(12) Uiso 0.38(2) 1 d P B 4 H27B H 0.4992 -0.038 0.3758 0.049 Uiso 0.38(2) 1 calc PR B 4 C28B C 0.320(4) -0.087(2) 0.298(4) 0.051(13) Uiso 0.38(2) 1 d P B 4 H28D H 0.2516 -0.097 0.2482 0.077 Uiso 0.38(2) 1 calc PR B 4 H28E H 0.3078 -0.0704 0.374 0.077 Uiso 0.38(2) 1 calc PR B 4 H28F H 0.3636 -0.1235 0.3129 0.077 Uiso 0.38(2) 1 calc PR B 4 C29B C 0.339(4) -0.027(2) 0.112(4) 0.049(13) Uiso 0.38(2) 1 d P B 4 H29D H 0.2673 -0.0444 0.0923 0.073 Uiso 0.38(2) 1 calc PR B 4 H29E H 0.3854 -0.0423 0.0577 0.073 Uiso 0.38(2) 1 calc PR B 4 H29F H 0.3335 0.0165 0.1036 0.073 Uiso 0.38(2) 1 calc PR B 4 N4 N 0.9063(10) 0.3172(6) 0.2281(11) 0.038(3) Uani 1 1 d . . . N3 N 1.0751(9) 0.2305(4) 0.4923(10) 0.026(2) Uani 1 1 d U B . C13 C 0.9990(11) 0.2084(6) 0.4376(13) 0.026(2) Uani 1 1 d U . . 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 0.0174(2) 0.0188(2) 0.0229(2) 0.0017(3) 0.00158(16) -0.0018(3) O1 0.021(5) 0.045(6) 0.017(5) -0.012(4) 0.012(4) -0.002(4) O5 0.028(6) 0.026(6) 0.046(6) 0.007(5) 0.001(5) -0.004(4) N6 0.017(6) 0.040(7) 0.018(6) -0.004(5) -0.001(5) -0.005(5) C11 0.031(8) 0.007(7) 0.028(7) -0.008(5) 0.006(6) -0.004(5) C16 0.020(7) 0.028(8) 0.029(8) 0.012(6) 0.013(6) 0.004(6) N1 0.030(3) 0.029(3) 0.029(3) 0.0003(10) 0.0040(11) -0.0005(10) C20 0.021(8) 0.031(8) 0.028(8) -0.009(6) 0.002(6) -0.002(6) C1 0.053(10) 0.024(8) 0.045(9) 0.000(8) 0.011(7) -0.008(8) O3 0.022(5) 0.023(5) 0.026(5) 0.001(4) -0.001(4) -0.007(4) C18 0.008(6) 0.035(8) 0.034(8) 0.010(6) -0.001(6) -0.004(6) C19 0.023(8) 0.029(8) 0.028(8) -0.005(6) -0.001(6) 0.000(6) O2 0.030(5) 0.026(5) 0.023(5) -0.017(4) 0.013(4) 0.002(4) C8 0.029(8) 0.017(7) 0.007(6) -0.003(5) 0.005(5) -0.003(6) C10 0.023(7) 0.015(7) 0.035(8) -0.003(6) 0.001(6) -0.004(6) C6 0.041(9) 0.023(8) 0.026(8) 0.001(6) 0.001(7) 0.003(7) N2 0.016(6) 0.022(6) 0.027(6) 0.006(5) 0.004(5) -0.001(5) C25 0.026(8) 0.039(9) 0.032(8) -0.003(7) 0.000(6) -0.002(7) O4 0.020(5) 0.031(5) 0.029(5) 0.004(4) 0.002(4) -0.010(4) C23 0.037(8) 0.020(7) 0.026(8) 0.006(6) 0.002(6) -0.004(6) C26 0.036(9) 0.044(10) 0.038(9) -0.002(7) 0.010(7) -0.009(8) C14 0.026(8) 0.017(7) 0.031(8) 0.006(6) 0.003(6) -0.003(6) C12 0.027(7) 0.020(7) 0.026(7) 0.001(6) 0.009(5) -0.002(5) C24 0.024(7) 0.041(9) 0.027(8) -0.001(6) -0.001(6) -0.017(7) N5 0.016(6) 0.022(6) 0.022(6) -0.005(5) 0.006(5) -0.007(5) C5 0.026(7) 0.017(8) 0.028(7) 0.005(5) 0.011(6) 0.003(5) N7 0.025(7) 0.030(7) 0.045(8) -0.012(6) 0.009(6) -0.006(5) C9 0.032(8) 0.026(8) 0.020(7) -0.002(6) 0.007(6) 0.006(6) C7 0.018(7) 0.029(8) 0.024(7) -0.010(6) 0.005(6) 0.001(6) C21 0.017(7) 0.028(8) 0.026(7) 0.003(6) 0.004(6) -0.009(6) C15 0.024(8) 0.025(8) 0.019(7) 0.010(6) -0.005(6) 0.006(6) C2 0.037(9) 0.024(8) 0.023(8) 0.002(6) -0.003(6) 0.003(7) C22 0.030(8) 0.022(7) 0.022(7) -0.004(6) -0.002(6) -0.005(6) C17 0.016(7) 0.030(8) 0.023(7) -0.010(6) 0.006(6) 0.003(6) N4 0.035(8) 0.030(8) 0.044(8) 0.008(6) -0.010(6) -0.015(6) N3 0.029(5) 0.011(5) 0.037(5) 0.004(4) 0.002(4) 0.001(4) C13 0.029(5) 0.011(5) 0.037(6) 0.004(4) 0.002(4) 0.001(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.784(8) . ? U1 O2 1.785(8) . ? U1 O3 2.257(8) . ? U1 O4 2.262(9) . ? U1 O5 2.403(9) . ? U1 N5 2.582(10) . ? U1 N2 2.621(10) . ? O5 C27B 1.19(4) . ? O5 C27A 1.23(2) . ? N6 C20 1.365(15) . ? N6 C25 1.446(16) . ? N6 C23 1.459(15) . ? C11 N2 1.320(15) . ? C11 C8 1.383(16) . ? C11 H11 0.93 . ? C16 N5 1.322(15) . ? C16 C17 1.406(17) . ? C16 H16 0.93 . ? N1 C5 1.365(15) . ? N1 C2 1.459(17) . ? N1 C4A 1.46(3) . ? N1 C4B 1.57(4) . ? C20 C21 1.391(18) . ? C20 C19 1.464(18) . ? C1 C2 1.533(19) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? O3 C9 1.313(14) . ? C18 C19 1.331(16) . ? C18 C17 1.430(17) . ? C18 H18 0.93 . ? C19 H19 0.93 . ? C8 C9 1.429(17) . ? C8 C7 1.431(16) . ? C10 C9 1.397(17) . ? C10 C5 1.399(17) . ? C10 H10 0.93 . ? C6 C7 1.312(17) . ? C6 C5 1.431(18) . ? C6 H6 0.93 . ? N2 C12 1.390(15) . ? C25 C26 1.519(18) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? O4 C22 1.301(15) . ? C23 C24 1.502(17) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C14 C12 1.378(17) . ? C14 N5 1.383(16) . ? C14 C15 1.444(18) . ? C12 C13 1.442(18) . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? N7 C27A 1.36(2) . ? N7 C29B 1.36(4) . ? N7 C27B 1.37(4) . ? N7 C28A 1.37(2) . ? N7 C29A 1.49(3) . ? N7 C28B 1.54(4) . ? C7 H7 0.93 . ? C21 C22 1.397(16) . ? C21 H21 0.93 . ? C15 N4 1.115(16) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C22 C17 1.443(17) . ? C3A C4A 1.55(3) . ? C3A H3A1 0.96 . ? C3A H3A2 0.96 . ? C3A H3A3 0.96 . ? C4A H4A1 0.97 . ? C4A H4A2 0.97 . ? C4B C3B 1.50(6) . ? C4B H4B1 0.97 . ? C4B H4B2 0.97 . ? C3B H3B1 0.96 . ? C3B H3B2 0.96 . ? C3B H3B3 0.96 . ? C27A H27A 0.93 . ? C28A H28A 0.96 . ? C28A H28B 0.96 . ? C28A H28C 0.96 . ? C29A H29A 0.96 . ? C29A H29B 0.96 . ? C29A H29C 0.96 . ? C27B H27B 0.93 . ? C28B H28D 0.96 . ? C28B H28E 0.96 . ? C28B H28F 0.96 . ? C29B H29D 0.96 . ? C29B H29E 0.96 . ? C29B H29F 0.96 . ? N3 C13 1.144(16) . ? 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 O2 176.9(4) . . ? O1 U1 O3 90.1(4) . . ? O2 U1 O3 91.0(4) . . ? O1 U1 O4 90.2(4) . . ? O2 U1 O4 90.1(4) . . ? O3 U1 O4 154.2(3) . . ? O1 U1 O5 91.9(4) . . ? O2 U1 O5 91.1(4) . . ? O3 U1 O5 77.6(3) . . ? O4 U1 O5 76.6(3) . . ? O1 U1 N5 87.8(4) . . ? O2 U1 N5 89.3(4) . . ? O3 U1 N5 135.4(3) . . ? O4 U1 N5 70.3(3) . . ? O5 U1 N5 146.9(3) . . ? O1 U1 N2 92.4(3) . . ? O2 U1 N2 85.3(4) . . ? O3 U1 N2 71.1(3) . . ? O4 U1 N2 134.6(3) . . ? O5 U1 N2 148.5(3) . . ? N5 U1 N2 64.5(3) . . ? C27B O5 C27A 62(2) . . ? C27B O5 U1 150(2) . . ? C27A O5 U1 138.6(11) . . ? C20 N6 C25 122.7(11) . . ? C20 N6 C23 119.4(11) . . ? C25 N6 C23 116.4(10) . . ? N2 C11 C8 131.3(12) . . ? N2 C11 H11 114.4 . . ? C8 C11 H11 114.4 . . ? N5 C16 C17 127.5(12) . . ? N5 C16 H16 116.2 . . ? C17 C16 H16 116.2 . . ? C5 N1 C2 123.0(11) . . ? C5 N1 C4A 118.6(14) . . ? C2 N1 C4A 118.4(13) . . ? C5 N1 C4B 119.9(19) . . ? C2 N1 C4B 109.2(18) . . ? C4A N1 C4B 30.2(15) . . ? N6 C20 C21 124.8(12) . . ? N6 C20 C19 118.5(12) . . ? C21 C20 C19 116.7(12) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C9 O3 U1 146.7(8) . . ? C19 C18 C17 122.6(12) . . ? C19 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C18 C19 C20 120.8(13) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C11 C8 C9 124.7(11) . . ? C11 C8 C7 118.6(11) . . ? C9 C8 C7 116.5(11) . . ? C9 C10 C5 121.5(12) . . ? C9 C10 H10 119.2 . . ? C5 C10 H10 119.2 . . ? C7 C6 C5 118.7(13) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C11 N2 C12 117.5(11) . . ? C11 N2 U1 125.8(8) . . ? C12 N2 U1 116.5(8) . . ? N6 C25 C26 112.4(12) . . ? N6 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? N6 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.9 . . ? C22 O4 U1 143.6(8) . . ? N6 C23 C24 112.4(11) . . ? N6 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N6 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C12 C14 N5 120.5(12) . . ? C12 C14 C15 116.5(12) . . ? N5 C14 C15 122.9(11) . . ? C14 C12 N2 120.0(12) . . ? C14 C12 C13 119.1(12) . . ? N2 C12 C13 120.9(11) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C16 N5 C14 113.9(11) . . ? C16 N5 U1 128.2(9) . . ? C14 N5 U1 117.7(8) . . ? N1 C5 C10 121.2(12) . . ? N1 C5 C6 119.6(12) . . ? C10 C5 C6 119.2(11) . . ? C27A N7 C29B 74(2) . . ? C27A N7 C27B 55(2) . . ? C29B N7 C27B 129(3) . . ? C27A N7 C28A 125.8(15) . . ? C29B N7 C28A 160(2) . . ? C27B N7 C28A 71(2) . . ? C27A N7 C29A 116.0(16) . . ? C29B N7 C29A 42.0(19) . . ? C27B N7 C29A 171(2) . . ? C28A N7 C29A 118.1(16) . . ? C27A N7 C28B 167(2) . . ? C29B N7 C28B 118(3) . . ? C27B N7 C28B 113(3) . . ? C28A N7 C28B 42.2(17) . . ? C29A N7 C28B 76.6(19) . . ? O3 C9 C10 121.3(12) . . ? O3 C9 C8 119.7(11) . . ? C10 C9 C8 119.0(12) . . ? C6 C7 C8 125.0(13) . . ? C6 C7 H7 117.5 . . ? C8 C7 H7 117.5 . . ? C20 C21 C22 123.8(12) . . ? C20 C21 H21 118.1 . . ? C22 C21 H21 118.1 . . ? N4 C15 C14 178.3(15) . . ? N1 C2 C1 113.9(11) . . ? N1 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? N1 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? O4 C22 C21 122.1(12) . . ? O4 C22 C17 119.9(11) . . ? C21 C22 C17 118.0(12) . . ? C4A C3A H3A1 109.5 . . ? C4A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C4A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? N1 C4A C3A 108.2(19) . . ? N1 C4A H4A1 110.1 . . ? C3A C4A H4A1 110.1 . . ? N1 C4A H4A2 110.1 . . ? C3A C4A H4A2 110.1 . . ? H4A1 C4A H4A2 108.4 . . ? C3B C4B N1 108(3) . . ? C3B C4B H4B1 110.2 . . ? N1 C4B H4B1 110.2 . . ? C3B C4B H4B2 110.2 . . ? N1 C4B H4B2 110.2 . . ? H4B1 C4B H4B2 108.5 . . ? C4B C3B H3B1 109.5 . . ? C4B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C4B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C16 C17 C18 117.4(12) . . ? C16 C17 C22 124.6(12) . . ? C18 C17 C22 118.0(11) . . ? O5 C27A N7 119.9(18) . . ? O5 C27A H27A 120 . . ? N7 C27A H27A 120 . . ? N7 C28A H28A 109.5 . . ? N7 C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? N7 C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? N7 C29A H29A 109.5 . . ? N7 C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? N7 C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? O5 C27B N7 123(4) . . ? O5 C27B H27B 118.6 . . ? N7 C27B H27B 118.6 . . ? N7 C28B H28D 109.5 . . ? N7 C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? N7 C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? N7 C29B H29D 109.5 . . ? N7 C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? N7 C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? N3 C13 C12 178.9(15) . . ? 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 O5 C27B 145(4) . . . . ? O2 U1 O5 C27B -35(4) . . . . ? O3 U1 O5 C27B 56(4) . . . . ? O4 U1 O5 C27B -125(4) . . . . ? N5 U1 O5 C27B -126(4) . . . . ? N2 U1 O5 C27B 48(4) . . . . ? O1 U1 O5 C27A -90.2(17) . . . . ? O2 U1 O5 C27A 89.4(17) . . . . ? O3 U1 O5 C27A -179.9(17) . . . . ? O4 U1 O5 C27A -0.5(17) . . . . ? N5 U1 O5 C27A -1(2) . . . . ? N2 U1 O5 C27A 172.1(16) . . . . ? C25 N6 C20 C21 174.7(12) . . . . ? C23 N6 C20 C21 8.9(19) . . . . ? C25 N6 C20 C19 -4.1(18) . . . . ? C23 N6 C20 C19 -170.0(11) . . . . ? O1 U1 O3 C9 103.0(14) . . . . ? O2 U1 O3 C9 -74.1(14) . . . . ? O4 U1 O3 C9 -166.3(13) . . . . ? O5 U1 O3 C9 -165.1(15) . . . . ? N5 U1 O3 C9 15.9(16) . . . . ? N2 U1 O3 C9 10.5(14) . . . . ? C17 C18 C19 C20 2(2) . . . . ? N6 C20 C19 C18 178.1(12) . . . . ? C21 C20 C19 C18 -0.8(19) . . . . ? N2 C11 C8 C9 -2(2) . . . . ? N2 C11 C8 C7 -177.3(12) . . . . ? C8 C11 N2 C12 177.1(13) . . . . ? C8 C11 N2 U1 2.5(19) . . . . ? O1 U1 N2 C11 -93.2(10) . . . . ? O2 U1 N2 C11 88.8(10) . . . . ? O3 U1 N2 C11 -3.9(9) . . . . ? O4 U1 N2 C11 174.2(9) . . . . ? O5 U1 N2 C11 4.4(13) . . . . ? N5 U1 N2 C11 -179.6(11) . . . . ? O1 U1 N2 C12 92.2(9) . . . . ? O2 U1 N2 C12 -85.9(9) . . . . ? O3 U1 N2 C12 -178.5(9) . . . . ? O4 U1 N2 C12 -0.4(10) . . . . ? O5 U1 N2 C12 -170.3(8) . . . . ? N5 U1 N2 C12 5.7(8) . . . . ? C20 N6 C25 C26 82.5(16) . . . . ? C23 N6 C25 C26 -111.3(13) . . . . ? O1 U1 O4 C22 -57.4(14) . . . . ? O2 U1 O4 C22 119.5(14) . . . . ? O3 U1 O4 C22 -148.1(12) . . . . ? O5 U1 O4 C22 -149.4(14) . . . . ? N5 U1 O4 C22 30.2(13) . . . . ? N2 U1 O4 C22 36.1(15) . . . . ? C20 N6 C23 C24 83.1(14) . . . . ? C25 N6 C23 C24 -83.7(14) . . . . ? N5 C14 C12 N2 -2.9(19) . . . . ? C15 C14 C12 N2 176.7(11) . . . . ? N5 C14 C12 C13 175.5(12) . . . . ? C15 C14 C12 C13 -4.9(19) . . . . ? C11 N2 C12 C14 -179.2(12) . . . . ? U1 N2 C12 C14 -4.1(15) . . . . ? C11 N2 C12 C13 2.4(18) . . . . ? U1 N2 C12 C13 177.5(9) . . . . ? C17 C16 N5 C14 -177.4(12) . . . . ? C17 C16 N5 U1 7.8(19) . . . . ? C12 C14 N5 C16 -166.9(12) . . . . ? C15 C14 N5 C16 13.6(18) . . . . ? C12 C14 N5 U1 8.5(16) . . . . ? C15 C14 N5 U1 -171.1(10) . . . . ? O1 U1 N5 C16 73.8(10) . . . . ? O2 U1 N5 C16 -107.5(10) . . . . ? O3 U1 N5 C16 161.8(9) . . . . ? O4 U1 N5 C16 -17.1(10) . . . . ? O5 U1 N5 C16 -16.4(13) . . . . ? N2 U1 N5 C16 167.5(11) . . . . ? O1 U1 N5 C14 -100.8(9) . . . . ? O2 U1 N5 C14 77.9(9) . . . . ? O3 U1 N5 C14 -12.8(11) . . . . ? O4 U1 N5 C14 168.2(9) . . . . ? O5 U1 N5 C14 169.0(8) . . . . ? N2 U1 N5 C14 -7.1(8) . . . . ? C2 N1 C5 C10 -4.9(19) . . . . ? C4A N1 C5 C10 174.6(15) . . . . ? C4B N1 C5 C10 -151(2) . . . . ? C2 N1 C5 C6 177.1(12) . . . . ? C4A N1 C5 C6 -3(2) . . . . ? C4B N1 C5 C6 31(3) . . . . ? C9 C10 C5 N1 178.7(12) . . . . ? C9 C10 C5 C6 -3.4(19) . . . . ? C7 C6 C5 N1 -179.0(12) . . . . ? C7 C6 C5 C10 3.0(19) . . . . ? U1 O3 C9 C10 168.3(10) . . . . ? U1 O3 C9 C8 -13(2) . . . . ? C5 C10 C9 O3 -179.0(11) . . . . ? C5 C10 C9 C8 2.1(19) . . . . ? C11 C8 C9 O3 5.1(19) . . . . ? C7 C8 C9 O3 -179.5(11) . . . . ? C11 C8 C9 C10 -176.0(12) . . . . ? C7 C8 C9 C10 -0.6(17) . . . . ? C5 C6 C7 C8 -2(2) . . . . ? C11 C8 C7 C6 176.1(13) . . . . ? C9 C8 C7 C6 0.4(19) . . . . ? N6 C20 C21 C22 179.7(12) . . . . ? C19 C20 C21 C22 -1.5(19) . . . . ? C12 C14 C15 N4 -15E1(5) . . . . ? N5 C14 C15 N4 3E1(5) . . . . ? C5 N1 C2 C1 -75.5(16) . . . . ? C4A N1 C2 C1 105.0(17) . . . . ? C4B N1 C2 C1 73(2) . . . . ? U1 O4 C22 C21 154.7(10) . . . . ? U1 O4 C22 C17 -27(2) . . . . ? C20 C21 C22 O4 -178.8(13) . . . . ? C20 C21 C22 C17 3.0(19) . . . . ? C5 N1 C4A C3A 81(2) . . . . ? C2 N1 C4A C3A -99.2(18) . . . . ? C4B N1 C4A C3A -20(4) . . . . ? C5 N1 C4B C3B -97(3) . . . . ? C2 N1 C4B C3B 113(3) . . . . ? C4A N1 C4B C3B -1(3) . . . . ? N5 C16 C17 C18 -174.1(12) . . . . ? N5 C16 C17 C22 7(2) . . . . ? C19 C18 C17 C16 -178.9(12) . . . . ? C19 C18 C17 C22 0.1(19) . . . . ? O4 C22 C17 C16 -2(2) . . . . ? C21 C22 C17 C16 176.6(12) . . . . ? O4 C22 C17 C18 179.5(11) . . . . ? C21 C22 C17 C18 -2.2(18) . . . . ? C27B O5 C27A N7 -3(2) . . . . ? U1 O5 C27A N7 -155.1(11) . . . . ? C29B N7 C27A O5 -176(3) . . . . ? C27B N7 C27A O5 3(2) . . . . ? C28A N7 C27A O5 4(3) . . . . ? C29A N7 C27A O5 -179.2(17) . . . . ? C28B N7 C27A O5 -21(10) . . . . ? C27A O5 C27B N7 3(3) . . . . ? U1 O5 C27B N7 145(2) . . . . ? C27A N7 C27B O5 -3(3) . . . . ? C29B N7 C27B O5 -1(5) . . . . ? C28A N7 C27B O5 178(4) . . . . ? C29A N7 C27B O5 -13(16) . . . . ? C28B N7 C27B O5 171(3) . . . . ? C14 C12 C13 N3 15E1(9) . . . . ? N2 C12 C13 N3 -3E1(9) . . . . ? #===END #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary _ccdc_compound_id 5.H2O # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _ccdc_temp_data_collection 100(2) _ccdc_ls_R_squared 0.0263 #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ data_bcas059abs _database_code_depnum_ccdc_archive 'CCDC 802710' #TrackingRef '- salmntall.cif' _audit_creation_date 2009-07-20T11:50:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; '[UO2(salmnt(Et2N)2)(TPPO)].H2O' ; _chemical_formula_sum 'C44 H45 N6 O6 P U' _chemical_formula_weight 1022.86 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.164(5) _cell_length_b 14.139(5) _cell_length_c 14.165(5) _cell_angle_alpha 107.335(5) _cell_angle_beta 105.515(5) _cell_angle_gamma 90.276(5) _cell_volume 2047.9(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9215 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.41 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prismatic _exptl_crystal_colour 'dark purple' _exptl_crystal_size_min 0.35 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.162010 _exptl_absorpt_correction_T_max 0.242000 _exptl_absorpt_process_details SADABS #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_unetI/netI 0.0291 _diffrn_reflns_number 14955 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.41 _diffrn_reflns_theta_full 25.41 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 7425 _reflns_number_gt 6821 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0359P)^2^+2.8226P] 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_number_reflns 7425 _refine_ls_number_parameters 522 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.065 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.263 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.098 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 1.616347(13) -0.099955(9) 1.198042(10) 0.02247(6) Uani 1 1 d . . . P1 P 1.77253(9) -0.34332(7) 1.17629(7) 0.02096(19) Uani 1 1 d . . . O5 O 1.7003(2) -0.25385(18) 1.1943(2) 0.0257(6) Uani 1 1 d . . . O4 O 1.5538(3) -0.14349(19) 1.3189(2) 0.0307(6) Uani 1 1 d . . . O3 O 1.7016(4) -0.1308(2) 1.0674(3) 0.0566(11) Uani 1 1 d . . . O1 O 1.4719(3) -0.15732(19) 1.1079(2) 0.0337(7) Uani 1 1 d . . . C37 C 2.1028(4) -0.1918(3) 1.2205(3) 0.0344(10) Uani 1 1 d . . . H37 H 2.1397 -0.127 1.2533 0.041 Uiso 1 1 calc R . . C23 C 1.2347(4) -0.2554(3) 1.5635(3) 0.0365(10) Uani 1 1 d . . . H23A H 1.2416 -0.1873 1.6079 0.044 Uiso 1 1 calc R . . H23B H 1.2499 -0.298 1.6071 0.044 Uiso 1 1 calc R . . N5 N 1.4851(3) 0.0358(2) 1.2769(2) 0.0220(6) Uani 1 1 d . . . O2 O 1.7560(3) -0.0344(2) 1.2889(2) 0.0364(7) Uani 1 1 d . . . N6 N 1.3311(3) -0.2653(2) 1.5094(2) 0.0303(7) Uani 1 1 d . . . C21 C 1.4420(4) -0.2049(3) 1.4107(3) 0.0260(8) Uani 1 1 d . . . H21 H 1.4831 -0.2626 1.4002 0.031 Uiso 1 1 calc R . . C20 C 1.3565(4) -0.1939(3) 1.4683(3) 0.0267(8) Uani 1 1 d . . . C29 C 1.6043(4) -0.6020(3) 0.9552(3) 0.0309(9) Uani 1 1 d . . . H29 H 1.581 -0.6668 0.9507 0.037 Uiso 1 1 calc R . . C11 C 1.6611(4) 0.0681(3) 1.0646(3) 0.0253(8) Uani 1 1 d . . . H11 H 1.6515 0.1293 1.0528 0.03 Uiso 1 1 calc R . . N4 N 1.3666(4) 0.2687(3) 1.3257(3) 0.0358(8) Uani 1 1 d . . . C28 C 1.6641(4) -0.5341(3) 1.0507(3) 0.0273(8) Uani 1 1 d . . . H28 H 1.6801 -0.5532 1.11 0.033 Uiso 1 1 calc R . . C7 C 1.7857(4) 0.0401(3) 0.9446(3) 0.0385(10) Uani 1 1 d . . . H7 H 1.7709 0.1034 0.9398 0.046 Uiso 1 1 calc R . . C13 C 1.5592(4) 0.2277(3) 1.1658(3) 0.0319(9) Uani 1 1 d . . . C27 C 1.6997(3) -0.4376(3) 1.0569(3) 0.0208(7) Uani 1 1 d . . . C8 C 1.7305(4) 0.0040(3) 1.0084(3) 0.0259(8) Uani 1 1 d . . . C22 C 1.4684(4) -0.1323(3) 1.3681(3) 0.0242(8) Uani 1 1 d . . . C19 C 1.2967(4) -0.1037(3) 1.4857(3) 0.0268(8) Uani 1 1 d . . . H19 H 1.2409 -0.0933 1.5254 0.032 Uiso 1 1 calc R . . C34 C 1.9931(4) -0.3840(3) 1.1222(3) 0.0339(9) Uani 1 1 d . . . H34 H 1.9563 -0.4487 1.0886 0.041 Uiso 1 1 calc R . . N2 N 1.6076(3) 0.0531(2) 1.1320(2) 0.0247(7) Uani 1 1 d . . . C33 C 1.9266(3) -0.3116(3) 1.1713(3) 0.0234(8) Uani 1 1 d . . . C36 C 2.1685(4) -0.2639(3) 1.1725(3) 0.0364(10) Uani 1 1 d . . . H36 H 2.2497 -0.2479 1.1733 0.044 Uiso 1 1 calc R . . C38 C 1.9822(4) -0.2156(3) 1.2201(3) 0.0304(9) Uani 1 1 d . . . H38 H 1.9385 -0.1667 1.2528 0.037 Uiso 1 1 calc R . . C16 C 1.4178(3) 0.0319(3) 1.3392(3) 0.0245(8) Uani 1 1 d . . . H16 H 1.3741 0.0869 1.3583 0.029 Uiso 1 1 calc R . . C31 C 1.6141(4) -0.4766(3) 0.8733(3) 0.0321(9) Uani 1 1 d . . . H31 H 1.5976 -0.4578 0.8138 0.039 Uiso 1 1 calc R . . C15 C 1.4200(4) 0.2047(3) 1.2912(3) 0.0291(9) Uani 1 1 d . . . C18 C 1.3212(3) -0.0331(3) 1.4443(3) 0.0243(8) Uani 1 1 d . . . H18 H 1.2826 0.0256 1.458 0.029 Uiso 1 1 calc R . . C6 C 1.8586(4) -0.0138(4) 0.8907(4) 0.0426(11) Uani 1 1 d . . . H6 H 1.8944 0.0133 0.8513 0.051 Uiso 1 1 calc R . . C17 C 1.4033(3) -0.0451(3) 1.3810(3) 0.0224(8) Uani 1 1 d . . . C35 C 2.1133(4) -0.3600(3) 1.1232(4) 0.0441(11) Uani 1 1 d . . . H35 H 2.1575 -0.4086 1.0907 0.053 Uiso 1 1 calc R . . C32 C 1.6734(4) -0.4084(3) 0.9686(3) 0.0265(8) Uani 1 1 d . . . H32 H 1.6955 -0.3433 0.9733 0.032 Uiso 1 1 calc R . . C24 C 1.1035(5) -0.2818(4) 1.4926(4) 0.0539(13) Uani 1 1 d . . . H24A H 1.0453 -0.2737 1.5329 0.081 Uiso 1 1 calc R . . H24B H 1.095 -0.3497 1.4496 0.081 Uiso 1 1 calc R . . H24C H 1.0867 -0.2389 1.4503 0.081 Uiso 1 1 calc R . . C12 C 1.5477(4) 0.1307(3) 1.1805(3) 0.0245(8) Uani 1 1 d . . . C14 C 1.4858(4) 0.1217(3) 1.2481(3) 0.0244(8) Uani 1 1 d . . . C39 C 1.7900(4) -0.3927(3) 1.2822(3) 0.0252(8) Uani 1 1 d . . . C30 C 1.5794(3) -0.5741(3) 0.8675(3) 0.0318(9) Uani 1 1 d . . . H30 H 1.5394 -0.62 0.8039 0.038 Uiso 1 1 calc R . . C41 C 1.8707(4) -0.5065(3) 1.3757(4) 0.0406(11) Uani 1 1 d . . . H41 H 1.9146 -0.5614 1.3808 0.049 Uiso 1 1 calc R . . C40 C 1.8585(4) -0.4731(3) 1.2915(3) 0.0327(9) Uani 1 1 d . . . H40 H 1.8964 -0.5045 1.2408 0.039 Uiso 1 1 calc R . . C9 C 1.7527(4) -0.0938(3) 1.0119(3) 0.0326(9) Uani 1 1 d . A . N3 N 1.5768(4) 0.3038(3) 1.1585(3) 0.0440(10) Uani 1 1 d . . . C44 C 1.7359(4) -0.3440(3) 1.3600(3) 0.0311(9) Uani 1 1 d . . . H44 H 1.6906 -0.2899 1.3547 0.037 Uiso 1 1 calc R . . C25 C 1.3804(5) -0.3621(3) 1.4825(3) 0.0372(10) Uani 1 1 d . . . H25A H 1.3748 -0.3947 1.5327 0.045 Uiso 1 1 calc R . . H25B H 1.4681 -0.3516 1.4875 0.045 Uiso 1 1 calc R . . C42 C 1.8169(4) -0.4577(4) 1.4527(4) 0.0421(11) Uani 1 1 d . . . H42 H 1.8259 -0.4796 1.5097 0.051 Uiso 1 1 calc R . . N1 N 1.9534(4) -0.1675(3) 0.8386(4) 0.0551(12) Uani 1 1 d D . . C5 C 1.8812(4) -0.1122(3) 0.8940(3) 0.0385(10) Uani 1 1 d . A . C43 C 1.7504(4) -0.3772(4) 1.4453(3) 0.0397(11) Uani 1 1 d . . . H43 H 1.7151 -0.3449 1.4974 0.048 Uiso 1 1 calc R . . C10 C 1.8277(4) -0.1489(3) 0.9561(3) 0.0382(10) Uani 1 1 d . . . H10 H 1.8428 -0.2124 0.9602 0.046 Uiso 1 1 calc R A . C2 C 2.0189(5) -0.1244(4) 0.7784(4) 0.0545(13) Uani 1 1 d . A . H2A H 2.0511 -0.0561 0.8179 0.065 Uiso 1 1 calc R . . H2B H 2.089 -0.162 0.7671 0.065 Uiso 1 1 calc R . . C26 C 1.3143(6) -0.4316(3) 1.3752(4) 0.0536(14) Uani 1 1 d . . . H26A H 1.3524 -0.4932 1.3636 0.08 Uiso 1 1 calc R . . H26B H 1.3211 -0.4011 1.3245 0.08 Uiso 1 1 calc R . . H26C H 1.2279 -0.4444 1.3699 0.08 Uiso 1 1 calc R . . C1 C 1.9318(6) -0.1272(6) 0.6773(5) 0.087(2) Uani 1 1 d . . . H1A H 1.9754 -0.0998 0.64 0.131 Uiso 1 1 calc R A . H1B H 1.8634 -0.0888 0.6885 0.131 Uiso 1 1 calc R . . H1C H 1.9005 -0.1949 0.638 0.131 Uiso 1 1 calc R . . O6 O 1.9354(12) -0.0886(11) 0.4658(8) 0.355(11) Uani 1 1 d . . . C4A C 1.9992(10) -0.2596(7) 0.8588(9) 0.042(3) Uiso 0.497(13) 1 d PD A 1 H4A1 H 2.0171 -0.25 0.9321 0.051 Uiso 0.497(13) 1 calc PR A 1 H4A2 H 2.0769 -0.2705 0.8406 0.051 Uiso 0.497(13) 1 calc PR A 1 C3A C 1.9094(9) -0.3523(8) 0.8008(8) 0.050(3) Uiso 0.497(13) 1 d PD A 1 H3A1 H 1.946 -0.4084 0.8181 0.075 Uiso 0.497(13) 1 calc PR A 1 H3A2 H 1.8926 -0.3638 0.728 0.075 Uiso 0.497(13) 1 calc PR A 1 H3A3 H 1.8328 -0.3433 0.8197 0.075 Uiso 0.497(13) 1 calc PR A 1 C3B C 2.0431(11) -0.2934(10) 0.8956(9) 0.062(4) Uiso 0.503(13) 1 d P A 2 H3B1 H 2.0432 -0.3637 0.885 0.093 Uiso 0.503(13) 1 calc PR A 2 H3B2 H 2.0293 -0.261 0.9612 0.093 Uiso 0.503(13) 1 calc PR A 2 H3B3 H 2.1222 -0.2677 0.8943 0.093 Uiso 0.503(13) 1 calc PR A 2 C4B C 1.9428(11) -0.2747(8) 0.8132(9) 0.047(3) Uiso 0.503(13) 1 d P A 2 H4B1 H 1.9553 -0.3061 0.746 0.056 Uiso 0.503(13) 1 calc PR A 2 H4B2 H 1.8617 -0.2993 0.8134 0.056 Uiso 0.503(13) 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 U1 0.03523(9) 0.01335(8) 0.02273(8) 0.00566(5) 0.01450(6) 0.00229(5) P1 0.0253(5) 0.0163(4) 0.0243(5) 0.0079(4) 0.0102(4) 0.0014(4) O5 0.0335(15) 0.0184(13) 0.0286(14) 0.0062(11) 0.0154(12) 0.0034(11) O4 0.0430(17) 0.0260(14) 0.0352(15) 0.0160(12) 0.0237(13) 0.0124(12) O3 0.111(3) 0.0219(15) 0.069(2) 0.0190(16) 0.072(2) 0.0159(17) O1 0.0492(18) 0.0168(13) 0.0326(15) 0.0087(12) 0.0065(13) 0.0041(12) C37 0.036(2) 0.030(2) 0.034(2) 0.0138(18) 0.0005(18) -0.0118(18) C23 0.038(2) 0.040(2) 0.037(2) 0.018(2) 0.014(2) -0.0028(19) N5 0.0263(16) 0.0172(15) 0.0224(16) 0.0055(12) 0.0074(13) -0.0002(12) O2 0.0361(16) 0.0201(14) 0.0520(19) 0.0069(13) 0.0158(14) 0.0025(12) N6 0.041(2) 0.0267(17) 0.0260(17) 0.0079(14) 0.0138(15) -0.0046(15) C21 0.039(2) 0.0201(18) 0.0212(19) 0.0063(15) 0.0113(17) 0.0013(16) C20 0.032(2) 0.0253(19) 0.0183(18) 0.0047(15) 0.0016(16) -0.0073(16) C29 0.023(2) 0.0226(19) 0.045(2) 0.0038(18) 0.0134(18) -0.0008(16) C11 0.030(2) 0.0217(18) 0.0247(19) 0.0126(16) 0.0032(16) -0.0006(15) N4 0.047(2) 0.0249(18) 0.037(2) 0.0085(15) 0.0143(17) 0.0095(16) C28 0.028(2) 0.0217(19) 0.036(2) 0.0103(17) 0.0138(17) 0.0028(16) C7 0.045(3) 0.042(3) 0.045(3) 0.030(2) 0.022(2) 0.014(2) C13 0.050(3) 0.022(2) 0.028(2) 0.0118(17) 0.0136(19) 0.0042(18) C27 0.0167(17) 0.0190(17) 0.0276(19) 0.0054(15) 0.0096(15) 0.0019(14) C8 0.030(2) 0.029(2) 0.0219(19) 0.0127(16) 0.0073(16) -0.0015(16) C22 0.032(2) 0.0215(18) 0.0194(18) 0.0047(15) 0.0093(16) -0.0006(15) C19 0.026(2) 0.031(2) 0.0223(19) 0.0057(16) 0.0089(16) -0.0028(16) C34 0.026(2) 0.025(2) 0.049(3) 0.0084(19) 0.0114(19) 0.0002(17) N2 0.0349(18) 0.0163(15) 0.0223(16) 0.0054(13) 0.0079(14) -0.0018(13) C33 0.0245(19) 0.0239(19) 0.0243(19) 0.0127(15) 0.0051(15) 0.0001(15) C36 0.021(2) 0.045(3) 0.044(3) 0.019(2) 0.0031(18) -0.0059(18) C38 0.034(2) 0.026(2) 0.031(2) 0.0081(17) 0.0082(18) -0.0025(17) C16 0.0248(19) 0.0190(18) 0.0257(19) 0.0033(15) 0.0047(16) 0.0008(15) C31 0.029(2) 0.041(2) 0.027(2) 0.0087(18) 0.0121(17) 0.0049(18) C15 0.040(2) 0.021(2) 0.025(2) 0.0082(16) 0.0064(18) -0.0002(18) C18 0.025(2) 0.0219(18) 0.0238(19) 0.0045(15) 0.0063(16) 0.0025(15) C6 0.051(3) 0.049(3) 0.053(3) 0.036(2) 0.033(2) 0.018(2) C17 0.0243(19) 0.0200(18) 0.0205(18) 0.0037(15) 0.0057(15) -0.0018(15) C35 0.030(2) 0.036(2) 0.064(3) 0.008(2) 0.016(2) 0.0038(19) C32 0.028(2) 0.027(2) 0.028(2) 0.0089(16) 0.0132(17) 0.0037(16) C24 0.046(3) 0.054(3) 0.062(3) 0.020(3) 0.014(3) -0.013(2) C12 0.034(2) 0.0163(17) 0.0213(18) 0.0061(15) 0.0041(16) -0.0011(15) C14 0.033(2) 0.0146(17) 0.0239(19) 0.0044(15) 0.0061(16) 0.0021(15) C39 0.026(2) 0.0224(19) 0.027(2) 0.0107(16) 0.0051(16) -0.0033(15) C30 0.0183(19) 0.036(2) 0.032(2) -0.0030(18) 0.0080(16) -0.0007(16) C41 0.041(3) 0.037(2) 0.046(3) 0.027(2) 0.001(2) -0.003(2) C40 0.038(2) 0.030(2) 0.034(2) 0.0157(18) 0.0086(18) 0.0008(18) C9 0.045(3) 0.024(2) 0.031(2) 0.0047(17) 0.0198(19) -0.0025(18) N3 0.072(3) 0.0246(19) 0.044(2) 0.0155(17) 0.024(2) 0.0072(18) C44 0.030(2) 0.036(2) 0.030(2) 0.0115(18) 0.0106(17) -0.0012(17) C25 0.063(3) 0.026(2) 0.031(2) 0.0130(18) 0.023(2) -0.003(2) C42 0.042(3) 0.054(3) 0.036(2) 0.027(2) 0.005(2) -0.012(2) N1 0.073(3) 0.046(2) 0.070(3) 0.024(2) 0.053(3) 0.018(2) C5 0.042(3) 0.042(3) 0.037(2) 0.013(2) 0.019(2) 0.002(2) C43 0.036(2) 0.054(3) 0.031(2) 0.014(2) 0.0122(19) -0.006(2) C10 0.060(3) 0.022(2) 0.041(2) 0.0081(18) 0.030(2) 0.0017(19) C2 0.052(3) 0.062(3) 0.053(3) 0.019(3) 0.019(3) 0.011(3) C26 0.098(4) 0.032(2) 0.035(3) 0.006(2) 0.031(3) -0.011(3) C1 0.053(4) 0.129(6) 0.060(4) 0.000(4) 0.017(3) 0.012(4) O6 0.315(15) 0.45(2) 0.184(10) -0.006(11) -0.007(9) 0.322(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O2 1.775(3) . ? U1 O1 1.777(3) . ? U1 O3 2.233(3) . ? U1 O4 2.250(3) . ? U1 O5 2.365(3) . ? U1 N5 2.589(3) . ? U1 N2 2.593(3) . ? P1 O5 1.498(3) . ? P1 C27 1.792(4) . ? P1 C33 1.800(4) . ? P1 C39 1.801(4) . ? O4 C22 1.308(4) . ? O3 C9 1.303(5) . ? C37 C36 1.378(6) . ? C37 C38 1.384(6) . ? C37 H37 0.93 . ? C23 N6 1.464(5) . ? C23 C24 1.509(6) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? N5 C16 1.316(5) . ? N5 C14 1.392(5) . ? N6 C20 1.371(5) . ? N6 C25 1.459(5) . ? C21 C20 1.394(5) . ? C21 C22 1.403(5) . ? C21 H21 0.93 . ? C20 C19 1.429(6) . ? C29 C30 1.374(6) . ? C29 C28 1.390(6) . ? C29 H29 0.93 . ? C11 N2 1.318(5) . ? C11 C8 1.401(6) . ? C11 H11 0.93 . ? N4 C15 1.144(5) . ? C28 C27 1.391(5) . ? C28 H28 0.93 . ? C7 C6 1.347(6) . ? C7 C8 1.425(5) . ? C7 H7 0.93 . ? C13 N3 1.132(5) . ? C13 C12 1.457(5) . ? C27 C32 1.390(5) . ? C8 C9 1.419(6) . ? C22 C17 1.424(5) . ? C19 C18 1.357(5) . ? C19 H19 0.93 . ? C34 C35 1.378(6) . ? C34 C33 1.394(6) . ? C34 H34 0.93 . ? N2 C12 1.388(5) . ? C33 C38 1.382(5) . ? C36 C35 1.382(6) . ? C36 H36 0.93 . ? C38 H38 0.93 . ? C16 C17 1.413(5) . ? C16 H16 0.93 . ? C31 C32 1.389(6) . ? C31 C30 1.402(6) . ? C31 H31 0.93 . ? C15 C14 1.453(5) . ? C18 C17 1.423(5) . ? C18 H18 0.93 . ? C6 C5 1.428(6) . ? C6 H6 0.93 . ? C35 H35 0.93 . ? C32 H32 0.93 . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C12 C14 1.356(5) . ? C39 C40 1.393(6) . ? C39 C44 1.400(6) . ? C30 H30 0.93 . ? C41 C40 1.384(6) . ? C41 C42 1.390(7) . ? C41 H41 0.93 . ? C40 H40 0.93 . ? C9 C10 1.388(6) . ? C44 C43 1.393(6) . ? C44 H44 0.93 . ? C25 C26 1.524(6) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C42 C43 1.376(7) . ? C42 H42 0.93 . ? N1 C5 1.362(6) . ? N1 C4B 1.447(11) . ? N1 C4A 1.480(10) . ? N1 C2 1.507(6) . ? C5 C10 1.397(6) . ? C43 H43 0.93 . ? C10 H10 0.93 . ? C2 C1 1.490(8) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C4A C3A 1.517(12) . ? C4A H4A1 0.97 . ? C4A H4A2 0.97 . ? C3A H3A1 0.96 . ? C3A H3A2 0.96 . ? C3A H3A3 0.96 . ? C3B C4B 1.475(17) . ? C3B H3B1 0.96 . ? C3B H3B2 0.96 . ? C3B H3B3 0.96 . ? C4B H4B1 0.97 . ? C4B H4B2 0.97 . ? 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 O2 U1 O1 175.93(12) . . ? O2 U1 O3 92.61(15) . . ? O1 U1 O3 88.64(15) . . ? O2 U1 O4 92.28(13) . . ? O1 U1 O4 88.37(12) . . ? O3 U1 O4 152.63(10) . . ? O2 U1 O5 90.84(11) . . ? O1 U1 O5 93.22(11) . . ? O3 U1 O5 76.61(10) . . ? O4 U1 O5 76.41(9) . . ? O2 U1 N5 91.04(12) . . ? O1 U1 N5 85.36(12) . . ? O3 U1 N5 135.42(11) . . ? O4 U1 N5 71.35(9) . . ? O5 U1 N5 147.75(9) . . ? O2 U1 N2 83.95(12) . . ? O1 U1 N2 92.84(11) . . ? O3 U1 N2 70.38(10) . . ? O4 U1 N2 136.95(10) . . ? O5 U1 N2 146.25(9) . . ? N5 U1 N2 65.88(10) . . ? O5 P1 C27 112.65(16) . . ? O5 P1 C33 111.46(16) . . ? C27 P1 C33 106.24(17) . . ? O5 P1 C39 108.66(17) . . ? C27 P1 C39 110.09(17) . . ? C33 P1 C39 107.61(17) . . ? P1 O5 U1 165.29(16) . . ? C22 O4 U1 143.8(2) . . ? C9 O3 U1 146.8(3) . . ? C36 C37 C38 120.2(4) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? N6 C23 C24 113.8(4) . . ? N6 C23 H23A 108.8 . . ? C24 C23 H23A 108.8 . . ? N6 C23 H23B 108.8 . . ? C24 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C16 N5 C14 117.2(3) . . ? C16 N5 U1 127.5(2) . . ? C14 N5 U1 115.3(2) . . ? C20 N6 C25 120.4(3) . . ? C20 N6 C23 121.1(3) . . ? C25 N6 C23 117.3(3) . . ? C20 C21 C22 122.4(4) . . ? C20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? N6 C20 C21 122.0(4) . . ? N6 C20 C19 120.1(4) . . ? C21 C20 C19 117.9(3) . . ? C30 C29 C28 120.5(4) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? N2 C11 C8 128.5(3) . . ? N2 C11 H11 115.8 . . ? C8 C11 H11 115.8 . . ? C29 C28 C27 119.5(4) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C6 C7 C8 122.7(4) . . ? C6 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? N3 C13 C12 175.1(5) . . ? C32 C27 C28 120.3(3) . . ? C32 C27 P1 116.5(3) . . ? C28 C27 P1 123.1(3) . . ? C11 C8 C9 125.0(3) . . ? C11 C8 C7 117.8(4) . . ? C9 C8 C7 117.2(4) . . ? O4 C22 C21 120.4(3) . . ? O4 C22 C17 120.3(3) . . ? C21 C22 C17 119.3(3) . . ? C18 C19 C20 120.1(4) . . ? C18 C19 H19 120 . . ? C20 C19 H19 120 . . ? C35 C34 C33 120.2(4) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C11 N2 C12 117.2(3) . . ? C11 N2 U1 127.6(2) . . ? C12 N2 U1 115.0(2) . . ? C38 C33 C34 119.2(4) . . ? C38 C33 P1 120.1(3) . . ? C34 C33 P1 120.7(3) . . ? C37 C36 C35 119.8(4) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C33 C38 C37 120.3(4) . . ? C33 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? N5 C16 C17 128.4(3) . . ? N5 C16 H16 115.8 . . ? C17 C16 H16 115.8 . . ? C32 C31 C30 119.5(4) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? N4 C15 C14 178.5(4) . . ? C19 C18 C17 122.9(4) . . ? C19 C18 H18 118.6 . . ? C17 C18 H18 118.6 . . ? C7 C6 C5 120.4(4) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C16 C17 C18 117.7(3) . . ? C16 C17 C22 125.0(3) . . ? C18 C17 C22 117.2(3) . . ? C34 C35 C36 120.3(4) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C31 C32 C27 119.9(4) . . ? C31 C32 H32 120 . . ? C27 C32 H32 120 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C14 C12 N2 121.9(3) . . ? C14 C12 C13 118.0(3) . . ? N2 C12 C13 119.9(3) . . ? C12 C14 N5 121.5(3) . . ? C12 C14 C15 118.4(3) . . ? N5 C14 C15 120.1(3) . . ? C40 C39 C44 119.6(4) . . ? C40 C39 P1 123.0(3) . . ? C44 C39 P1 117.4(3) . . ? C29 C30 C31 120.3(4) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C40 C41 C42 119.6(4) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C41 C40 C39 120.3(4) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? O3 C9 C10 120.9(4) . . ? O3 C9 C8 119.3(4) . . ? C10 C9 C8 119.8(4) . . ? C43 C44 C39 119.6(4) . . ? C43 C44 H44 120.2 . . ? C39 C44 H44 120.2 . . ? N6 C25 C26 114.8(4) . . ? N6 C25 H25A 108.6 . . ? C26 C25 H25A 108.6 . . ? N6 C25 H25B 108.6 . . ? C26 C25 H25B 108.6 . . ? H25A C25 H25B 107.5 . . ? C43 C42 C41 120.6(4) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C5 N1 C4B 120.2(5) . . ? C5 N1 C4A 120.4(5) . . ? C4B N1 C4A 29.5(5) . . ? C5 N1 C2 121.2(4) . . ? C4B N1 C2 116.6(5) . . ? C4A N1 C2 116.2(5) . . ? N1 C5 C10 121.7(4) . . ? N1 C5 C6 120.6(4) . . ? C10 C5 C6 117.7(4) . . ? C42 C43 C44 120.2(4) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C9 C10 C5 122.2(4) . . ? C9 C10 H10 118.9 . . ? C5 C10 H10 118.9 . . ? C1 C2 N1 110.8(5) . . ? C1 C2 H2A 109.5 . . ? N1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C4A C3A 114.7(9) . . ? N1 C4A H4A1 108.6 . . ? C3A C4A H4A1 108.6 . . ? N1 C4A H4A2 108.6 . . ? C3A C4A H4A2 108.6 . . ? H4A1 C4A H4A2 107.6 . . ? C4A C3A H3A1 109.5 . . ? C4A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C4A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C4B C3B H3B1 109.5 . . ? C4B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C4B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? N1 C4B C3B 103.5(9) . . ? N1 C4B H4B1 111.1 . . ? C3B C4B H4B1 111.1 . . ? N1 C4B H4B2 111.1 . . ? C3B C4B H4B2 111.1 . . ? H4B1 C4B H4B2 109 . . ? 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 C27 P1 O5 U1 -86.6(7) . . . . ? C33 P1 O5 U1 32.7(7) . . . . ? C39 P1 O5 U1 151.1(6) . . . . ? O2 U1 O5 P1 -74.1(7) . . . . ? O1 U1 O5 P1 106.2(7) . . . . ? O3 U1 O5 P1 18.4(7) . . . . ? O4 U1 O5 P1 -166.3(7) . . . . ? N5 U1 O5 P1 -167.4(6) . . . . ? N2 U1 O5 P1 6.2(8) . . . . ? O2 U1 O4 C22 115.1(4) . . . . ? O1 U1 O4 C22 -60.9(4) . . . . ? O3 U1 O4 C22 -144.8(4) . . . . ? O5 U1 O4 C22 -154.6(4) . . . . ? N5 U1 O4 C22 24.7(4) . . . . ? N2 U1 O4 C22 31.5(5) . . . . ? O2 U1 O3 C9 -62.0(6) . . . . ? O1 U1 O3 C9 114.1(6) . . . . ? O4 U1 O3 C9 -162.1(5) . . . . ? O5 U1 O3 C9 -152.3(7) . . . . ? N5 U1 O3 C9 32.1(7) . . . . ? N2 U1 O3 C9 20.6(6) . . . . ? O2 U1 N5 C16 -102.1(3) . . . . ? O1 U1 N5 C16 79.8(3) . . . . ? O3 U1 N5 C16 163.1(3) . . . . ? O4 U1 N5 C16 -10.1(3) . . . . ? O5 U1 N5 C16 -8.9(4) . . . . ? N2 U1 N5 C16 175.0(3) . . . . ? O2 U1 N5 C14 78.7(3) . . . . ? O1 U1 N5 C14 -99.4(3) . . . . ? O3 U1 N5 C14 -16.1(3) . . . . ? O4 U1 N5 C14 170.8(3) . . . . ? O5 U1 N5 C14 171.9(2) . . . . ? N2 U1 N5 C14 -4.2(2) . . . . ? C24 C23 N6 C20 78.7(5) . . . . ? C24 C23 N6 C25 -88.9(5) . . . . ? C25 N6 C20 C21 -8.4(6) . . . . ? C23 N6 C20 C21 -175.7(4) . . . . ? C25 N6 C20 C19 172.9(4) . . . . ? C23 N6 C20 C19 5.6(5) . . . . ? C22 C21 C20 N6 179.8(4) . . . . ? C22 C21 C20 C19 -1.5(6) . . . . ? C30 C29 C28 C27 -0.6(6) . . . . ? C29 C28 C27 C32 1.4(5) . . . . ? C29 C28 C27 P1 177.9(3) . . . . ? O5 P1 C27 C32 54.9(3) . . . . ? C33 P1 C27 C32 -67.5(3) . . . . ? C39 P1 C27 C32 176.3(3) . . . . ? O5 P1 C27 C28 -121.8(3) . . . . ? C33 P1 C27 C28 115.9(3) . . . . ? C39 P1 C27 C28 -0.3(4) . . . . ? N2 C11 C8 C9 2.3(7) . . . . ? N2 C11 C8 C7 -176.2(4) . . . . ? C6 C7 C8 C11 177.1(4) . . . . ? C6 C7 C8 C9 -1.5(7) . . . . ? U1 O4 C22 C21 155.3(3) . . . . ? U1 O4 C22 C17 -26.1(6) . . . . ? C20 C21 C22 O4 176.6(3) . . . . ? C20 C21 C22 C17 -1.9(6) . . . . ? N6 C20 C19 C18 -179.5(4) . . . . ? C21 C20 C19 C18 1.8(5) . . . . ? C8 C11 N2 C12 177.5(4) . . . . ? C8 C11 N2 U1 3.3(6) . . . . ? O2 U1 N2 C11 86.3(3) . . . . ? O1 U1 N2 C11 -96.2(3) . . . . ? O3 U1 N2 C11 -8.7(3) . . . . ? O4 U1 N2 C11 173.1(3) . . . . ? O5 U1 N2 C11 3.9(4) . . . . ? N5 U1 N2 C11 -179.8(3) . . . . ? O2 U1 N2 C12 -88.0(3) . . . . ? O1 U1 N2 C12 89.5(3) . . . . ? O3 U1 N2 C12 177.0(3) . . . . ? O4 U1 N2 C12 -1.2(3) . . . . ? O5 U1 N2 C12 -170.4(2) . . . . ? N5 U1 N2 C12 5.8(2) . . . . ? C35 C34 C33 C38 0.6(6) . . . . ? C35 C34 C33 P1 -176.8(4) . . . . ? O5 P1 C33 C38 24.6(4) . . . . ? C27 P1 C33 C38 147.6(3) . . . . ? C39 P1 C33 C38 -94.5(3) . . . . ? O5 P1 C33 C34 -158.2(3) . . . . ? C27 P1 C33 C34 -35.1(4) . . . . ? C39 P1 C33 C34 82.8(4) . . . . ? C38 C37 C36 C35 0.4(7) . . . . ? C34 C33 C38 C37 -0.3(6) . . . . ? P1 C33 C38 C37 177.0(3) . . . . ? C36 C37 C38 C33 -0.2(6) . . . . ? C14 N5 C16 C17 -178.7(4) . . . . ? U1 N5 C16 C17 2.1(6) . . . . ? C20 C19 C18 C17 1.4(6) . . . . ? C8 C7 C6 C5 1.5(8) . . . . ? N5 C16 C17 C18 -177.9(4) . . . . ? N5 C16 C17 C22 4.8(6) . . . . ? C19 C18 C17 C16 177.7(4) . . . . ? C19 C18 C17 C22 -4.8(6) . . . . ? O4 C22 C17 C16 3.7(6) . . . . ? C21 C22 C17 C16 -177.8(4) . . . . ? O4 C22 C17 C18 -173.7(3) . . . . ? C21 C22 C17 C18 4.9(5) . . . . ? C33 C34 C35 C36 -0.3(7) . . . . ? C37 C36 C35 C34 -0.2(7) . . . . ? C30 C31 C32 C27 1.1(6) . . . . ? C28 C27 C32 C31 -1.6(5) . . . . ? P1 C27 C32 C31 -178.4(3) . . . . ? C11 N2 C12 C14 177.5(4) . . . . ? U1 N2 C12 C14 -7.6(5) . . . . ? C11 N2 C12 C13 -7.7(5) . . . . ? U1 N2 C12 C13 167.3(3) . . . . ? N3 C13 C12 C14 105(5) . . . . ? N3 C13 C12 N2 -70(5) . . . . ? N2 C12 C14 N5 3.7(6) . . . . ? C13 C12 C14 N5 -171.3(4) . . . . ? N2 C12 C14 C15 -176.7(3) . . . . ? C13 C12 C14 C15 8.3(5) . . . . ? C16 N5 C14 C12 -177.0(4) . . . . ? U1 N5 C14 C12 2.3(5) . . . . ? C16 N5 C14 C15 3.5(5) . . . . ? U1 N5 C14 C15 -177.2(3) . . . . ? N4 C15 C14 C12 159(18) . . . . ? N4 C15 C14 N5 -21(18) . . . . ? O5 P1 C39 C40 -176.5(3) . . . . ? C27 P1 C39 C40 59.7(4) . . . . ? C33 P1 C39 C40 -55.7(4) . . . . ? O5 P1 C39 C44 0.6(3) . . . . ? C27 P1 C39 C44 -123.2(3) . . . . ? C33 P1 C39 C44 121.5(3) . . . . ? C28 C29 C30 C31 0.0(6) . . . . ? C32 C31 C30 C29 -0.3(6) . . . . ? C42 C41 C40 C39 -1.7(6) . . . . ? C44 C39 C40 C41 1.6(6) . . . . ? P1 C39 C40 C41 178.7(3) . . . . ? U1 O3 C9 C10 158.9(5) . . . . ? U1 O3 C9 C8 -21.5(9) . . . . ? C11 C8 C9 O3 3.1(7) . . . . ? C7 C8 C9 O3 -178.4(4) . . . . ? C11 C8 C9 C10 -177.2(4) . . . . ? C7 C8 C9 C10 1.3(6) . . . . ? C40 C39 C44 C43 -0.6(6) . . . . ? P1 C39 C44 C43 -177.8(3) . . . . ? C20 N6 C25 C26 -75.1(5) . . . . ? C23 N6 C25 C26 92.6(4) . . . . ? C40 C41 C42 C43 0.8(7) . . . . ? C4B N1 C5 C10 21.6(9) . . . . ? C4A N1 C5 C10 -12.7(9) . . . . ? C2 N1 C5 C10 -175.1(5) . . . . ? C4B N1 C5 C6 -158.9(7) . . . . ? C4A N1 C5 C6 166.7(6) . . . . ? C2 N1 C5 C6 4.4(8) . . . . ? C7 C6 C5 N1 179.1(5) . . . . ? C7 C6 C5 C10 -1.4(7) . . . . ? C41 C42 C43 C44 0.3(7) . . . . ? C39 C44 C43 C42 -0.4(6) . . . . ? O3 C9 C10 C5 178.4(5) . . . . ? C8 C9 C10 C5 -1.3(7) . . . . ? N1 C5 C10 C9 -179.2(5) . . . . ? C6 C5 C10 C9 1.3(7) . . . . ? C5 N1 C2 C1 -81.4(7) . . . . ? C4B N1 C2 C1 82.4(8) . . . . ? C4A N1 C2 C1 115.5(7) . . . . ? C5 N1 C4A C3A 86.2(9) . . . . ? C4B N1 C4A C3A -12.3(10) . . . . ? C2 N1 C4A C3A -110.6(8) . . . . ? C5 N1 C4B C3B -95.3(9) . . . . ? C4A N1 C4B C3B 3.9(11) . . . . ? C2 N1 C4B C3B 100.7(8) . . . . ? #===END #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary _ccdc_compound_id '[UO2(salophen)(py)]' # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _ccdc_temp_data_collection 100(2) _ccdc_ls_R_squared 0.0287 #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ data_bcas006p _database_code_depnum_ccdc_archive 'CCDC 802711' #TrackingRef '- salmntall.cif' _audit_creation_date 2008-10-30T23:59:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; '[UO2(salophen)(py)]' ; _chemical_formula_sum 'C25 H19 N3 O4 U' _chemical_formula_weight 663.46 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.3821(14) _cell_length_b 9.6222(8) _cell_length_c 14.6513(12) _cell_angle_alpha 90 _cell_angle_beta 113.8580(10) _cell_angle_gamma 90 _cell_volume 2241.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4618 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 25.32 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prismatic _exptl_crystal_colour Orange _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.28 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.548 _exptl_absorpt_correction_T_max 0.695 _exptl_absorpt_process_details SADABS #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_unetI/netI 0.0351 _diffrn_reflns_number 11185 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.33 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 4078 _reflns_number_gt 3655 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0265P)^2^+3.9686P] 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_number_reflns 4078 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0629 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.983 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.142 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.251052(11) 0.090049(18) 0.766577(13) 0.01242(7) Uani 1 1 d . . . O1 O 0.2730(2) 0.2014(3) 0.8722(2) 0.0177(8) Uani 1 1 d . . . O3 O 0.1352(2) 0.0095(3) 0.7798(2) 0.0164(7) Uani 1 1 d . . . O4 O 0.3885(2) 0.0953(3) 0.7955(2) 0.0159(7) Uani 1 1 d . . . C5 C -0.0670(3) 0.0253(5) 0.5648(4) 0.0173(11) Uani 1 1 d . . . H5 H -0.097 0.0846 0.5123 0.021 Uiso 1 1 calc R . . N3 N 0.3067(3) -0.1208(4) 0.8845(3) 0.0180(9) Uani 1 1 d . . . N1 N 0.1248(2) 0.2370(4) 0.6597(3) 0.0132(8) Uani 1 1 d . . . C9 C 0.0890(3) 0.4870(5) 0.6263(4) 0.0184(11) Uani 1 1 d . . . H9 H 0.0367 0.4732 0.6281 0.022 Uiso 1 1 calc R . . O2 O 0.2301(2) -0.0197(3) 0.6603(2) 0.0148(7) Uani 1 1 d . . . C18 C 0.5370(3) -0.0008(5) 0.6907(4) 0.0205(11) Uani 1 1 d . . . H18 H 0.5826 -0.0603 0.705 0.025 Uiso 1 1 calc R . . C11 C 0.1909(3) 0.6398(5) 0.6073(4) 0.0209(12) Uani 1 1 d . . . H11 H 0.2065 0.7283 0.5959 0.025 Uiso 1 1 calc R . . C6 C 0.0146(3) 0.0632(5) 0.6317(4) 0.0136(10) Uani 1 1 d . . . C14 C 0.3306(3) 0.2728(5) 0.6202(3) 0.0148(10) Uani 1 1 d . . . H14 H 0.3244 0.3362 0.5698 0.018 Uiso 1 1 calc R . . C15 C 0.3982(3) 0.1749(5) 0.6453(4) 0.0137(10) Uani 1 1 d . . . C19 C 0.4946(3) 0.0005(5) 0.7516(4) 0.0175(11) Uani 1 1 d . . . H19 H 0.5119 -0.0583 0.8067 0.021 Uiso 1 1 calc R . . C10 C 0.1128(3) 0.6190(5) 0.6097(4) 0.0189(11) Uani 1 1 d . . . H10 H 0.0763 0.6936 0.6002 0.023 Uiso 1 1 calc R . . C8 C 0.1432(3) 0.3752(5) 0.6402(3) 0.0151(11) Uani 1 1 d . . . C2 C 0.0204(3) -0.1487(5) 0.7233(4) 0.0180(11) Uani 1 1 d . . . H2 H 0.0484 -0.2078 0.7768 0.022 Uiso 1 1 calc R . . C24 C 0.2779(4) -0.3417(6) 0.9377(5) 0.0280(13) Uani 1 1 d . . . H24 H 0.244 -0.4203 0.9247 0.034 Uiso 1 1 calc R . . C16 C 0.4448(3) 0.1717(5) 0.5854(4) 0.0174(11) Uani 1 1 d . . . H16 H 0.4288 0.2293 0.5298 0.021 Uiso 1 1 calc R . . C1 C 0.0597(3) -0.0246(5) 0.7133(4) 0.0155(11) Uani 1 1 d . . . C23 C 0.3488(4) -0.3299(6) 1.0254(4) 0.0273(14) Uani 1 1 d . . . H23 H 0.3617 -0.3981 1.0742 0.033 Uiso 1 1 calc R . . C7 C 0.0476(3) 0.1947(5) 0.6165(4) 0.0161(11) Uani 1 1 d . . . H7 H 0.0096 0.2553 0.5709 0.019 Uiso 1 1 calc R . . C25 C 0.2586(3) -0.2347(5) 0.8700(4) 0.0235(12) Uani 1 1 d . . . H25 H 0.2101 -0.2415 0.8116 0.028 Uiso 1 1 calc R . . C3 C -0.0594(3) -0.1837(5) 0.6546(4) 0.0205(12) Uani 1 1 d . . . H3 H -0.0836 -0.2668 0.662 0.025 Uiso 1 1 calc R . . N2 N 0.2772(2) 0.2808(4) 0.6614(3) 0.0130(8) Uani 1 1 d . . . C4 C -0.1037(3) -0.0975(5) 0.5751(4) 0.0203(11) Uani 1 1 d . . . H4 H -0.1572 -0.1219 0.5294 0.024 Uiso 1 1 calc R . . C12 C 0.2457(3) 0.5299(5) 0.6219(4) 0.0170(11) Uani 1 1 d . . . H12 H 0.298 0.5443 0.6203 0.02 Uiso 1 1 calc R . . C20 C 0.4254(3) 0.0889(5) 0.7324(3) 0.0136(10) Uani 1 1 d . . . C13 C 0.2222(3) 0.3976(5) 0.6388(3) 0.0146(10) Uani 1 1 d . . . C17 C 0.5128(3) 0.0862(5) 0.6072(4) 0.0209(11) Uani 1 1 d . . . H17 H 0.5426 0.0859 0.5669 0.025 Uiso 1 1 calc R . . C21 C 0.3769(3) -0.1146(5) 0.9679(4) 0.0209(12) Uani 1 1 d . . . H21 H 0.4117 -0.0376 0.978 0.025 Uiso 1 1 calc R . . C22 C 0.4002(4) -0.2164(6) 1.0397(4) 0.0280(13) Uani 1 1 d . . . H22 H 0.4497 -0.2086 1.0969 0.034 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 0.01342(11) 0.01030(10) 0.01314(10) 0.00065(7) 0.00494(7) -0.00038(8) O1 0.022(2) 0.0158(19) 0.0166(18) -0.0043(14) 0.0086(16) -0.0039(15) O3 0.0150(19) 0.0167(19) 0.0177(18) 0.0031(14) 0.0068(15) 0.0008(15) O4 0.0155(19) 0.0163(18) 0.0146(17) -0.0006(14) 0.0046(14) -0.0001(15) C5 0.016(3) 0.018(3) 0.019(3) 0.001(2) 0.009(2) 0.004(2) N3 0.019(2) 0.017(2) 0.018(2) 0.0034(17) 0.0073(19) 0.0011(18) N1 0.013(2) 0.012(2) 0.017(2) -0.0004(17) 0.0080(17) 0.0001(17) C9 0.016(3) 0.025(3) 0.015(3) 0.002(2) 0.008(2) 0.001(2) O2 0.018(2) 0.0095(17) 0.0164(17) -0.0014(14) 0.0058(15) -0.0014(14) C18 0.012(3) 0.019(3) 0.024(3) -0.004(2) 0.002(2) 0.003(2) C11 0.031(3) 0.011(3) 0.018(3) 0.002(2) 0.007(2) -0.004(2) C6 0.015(3) 0.013(3) 0.017(2) -0.0002(19) 0.010(2) 0.000(2) C14 0.016(3) 0.009(2) 0.015(2) -0.0014(19) 0.001(2) -0.005(2) C15 0.014(3) 0.007(2) 0.018(3) -0.0034(19) 0.004(2) -0.0031(19) C19 0.017(3) 0.016(3) 0.016(2) 0.001(2) 0.004(2) 0.001(2) C10 0.023(3) 0.016(3) 0.019(3) 0.002(2) 0.010(2) 0.007(2) C8 0.020(3) 0.015(3) 0.009(2) -0.0006(19) 0.004(2) 0.000(2) C2 0.022(3) 0.017(3) 0.021(3) 0.002(2) 0.015(2) 0.003(2) C24 0.020(3) 0.019(3) 0.049(4) 0.009(3) 0.019(3) 0.001(2) C16 0.016(3) 0.015(3) 0.022(3) -0.002(2) 0.008(2) -0.003(2) C1 0.018(3) 0.015(3) 0.017(3) -0.004(2) 0.012(2) 0.002(2) C23 0.041(4) 0.019(3) 0.028(3) 0.016(2) 0.020(3) 0.017(3) C7 0.021(3) 0.014(3) 0.015(2) 0.003(2) 0.009(2) 0.007(2) C25 0.016(3) 0.019(3) 0.030(3) 0.003(2) 0.003(2) 0.002(2) C3 0.023(3) 0.017(3) 0.029(3) -0.005(2) 0.018(3) -0.007(2) N2 0.011(2) 0.012(2) 0.013(2) 0.0013(16) 0.0018(17) 0.0007(17) C4 0.019(3) 0.022(3) 0.021(3) -0.003(2) 0.009(2) -0.001(2) C12 0.020(3) 0.017(3) 0.016(3) 0.001(2) 0.010(2) 0.003(2) C20 0.014(3) 0.010(2) 0.014(2) -0.003(2) 0.003(2) -0.006(2) C13 0.019(3) 0.009(2) 0.015(2) 0.0013(19) 0.005(2) 0.003(2) C17 0.020(3) 0.023(3) 0.024(3) -0.008(2) 0.013(2) -0.003(2) C21 0.024(3) 0.011(3) 0.023(3) 0.000(2) 0.005(2) 0.005(2) C22 0.033(3) 0.025(3) 0.018(3) 0.000(2) 0.002(2) 0.016(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.792(3) . ? U1 O2 1.793(3) . ? U1 O3 2.238(3) . ? U1 O4 2.253(3) . ? U1 N1 2.547(4) . ? U1 N2 2.553(4) . ? U1 N3 2.585(4) . ? O3 C1 1.320(6) . ? O4 C20 1.321(6) . ? C5 C4 1.379(7) . ? C5 C6 1.407(7) . ? C5 H5 0.93 . ? N3 C21 1.334(7) . ? N3 C25 1.342(7) . ? N1 C7 1.295(6) . ? N1 C8 1.424(6) . ? C9 C10 1.387(7) . ? C9 C8 1.389(7) . ? C9 H9 0.93 . ? C18 C19 1.369(7) . ? C18 C17 1.399(7) . ? C18 H18 0.93 . ? C11 C12 1.380(7) . ? C11 C10 1.387(7) . ? C11 H11 0.93 . ? C6 C1 1.415(7) . ? C6 C7 1.444(7) . ? C14 N2 1.298(6) . ? C14 C15 1.434(7) . ? C14 H14 0.93 . ? C15 C16 1.416(7) . ? C15 C20 1.431(7) . ? C19 C20 1.406(7) . ? C19 H19 0.93 . ? C10 H10 0.93 . ? C8 C13 1.398(7) . ? C2 C3 1.386(7) . ? C2 C1 1.413(7) . ? C2 H2 0.93 . ? C24 C25 1.374(7) . ? C24 C23 1.379(8) . ? C24 H24 0.93 . ? C16 C17 1.367(7) . ? C16 H16 0.93 . ? C23 C22 1.371(8) . ? C23 H23 0.93 . ? C7 H7 0.93 . ? C25 H25 0.93 . ? C3 C4 1.383(7) . ? C3 H3 0.93 . ? N2 C13 1.425(6) . ? C4 H4 0.93 . ? C12 C13 1.390(7) . ? C12 H12 0.93 . ? C17 H17 0.93 . ? C21 C22 1.373(7) . ? C21 H21 0.93 . ? C22 H22 0.93 . ? 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 O2 179.10(15) . . ? O1 U1 O3 90.98(14) . . ? O2 U1 O3 89.87(13) . . ? O1 U1 O4 89.16(14) . . ? O2 U1 O4 90.19(13) . . ? O3 U1 O4 156.19(12) . . ? O1 U1 N1 91.62(14) . . ? O2 U1 N1 88.38(14) . . ? O3 U1 N1 70.33(12) . . ? O4 U1 N1 133.47(12) . . ? O1 U1 N2 93.67(14) . . ? O2 U1 N2 85.54(13) . . ? O3 U1 N2 133.42(12) . . ? O4 U1 N2 70.29(12) . . ? N1 U1 N2 63.23(12) . . ? O1 U1 N3 90.05(14) . . ? O2 U1 N3 90.43(14) . . ? O3 U1 N3 77.13(13) . . ? O4 U1 N3 79.06(12) . . ? N1 U1 N3 147.44(13) . . ? N2 U1 N3 149.05(13) . . ? C1 O3 U1 133.0(3) . . ? C20 O4 U1 130.2(3) . . ? C4 C5 C6 121.8(5) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C21 N3 C25 117.5(4) . . ? C21 N3 U1 122.2(3) . . ? C25 N3 U1 119.6(3) . . ? C7 N1 C8 117.9(4) . . ? C7 N1 U1 126.2(3) . . ? C8 N1 U1 115.7(3) . . ? C10 C9 C8 120.1(5) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C19 C18 C17 120.9(5) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C12 C11 C10 120.4(5) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C5 C6 C1 119.5(4) . . ? C5 C6 C7 118.2(4) . . ? C1 C6 C7 122.3(5) . . ? N2 C14 C15 125.9(4) . . ? N2 C14 H14 117.1 . . ? C15 C14 H14 117.1 . . ? C16 C15 C20 118.4(4) . . ? C16 C15 C14 118.0(4) . . ? C20 C15 C14 123.3(4) . . ? C18 C19 C20 121.2(5) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C11 C10 C9 120.0(5) . . ? C11 C10 H10 120 . . ? C9 C10 H10 120 . . ? C9 C8 C13 119.4(5) . . ? C9 C8 N1 123.9(4) . . ? C13 C8 N1 116.7(4) . . ? C3 C2 C1 120.9(5) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C25 C24 C23 118.4(5) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? C17 C16 C15 121.7(5) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? O3 C1 C2 120.8(4) . . ? O3 C1 C6 121.4(4) . . ? C2 C1 C6 117.8(5) . . ? C22 C23 C24 119.3(5) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? N1 C7 C6 126.7(5) . . ? N1 C7 H7 116.7 . . ? C6 C7 H7 116.7 . . ? N3 C25 C24 122.9(5) . . ? N3 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C4 C3 C2 121.2(5) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C14 N2 C13 118.5(4) . . ? C14 N2 U1 125.0(3) . . ? C13 N2 U1 116.1(3) . . ? C5 C4 C3 118.8(5) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C11 C12 C13 119.7(5) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? O4 C20 C19 120.4(4) . . ? O4 C20 C15 121.2(4) . . ? C19 C20 C15 118.4(4) . . ? C12 C13 C8 120.3(4) . . ? C12 C13 N2 123.1(4) . . ? C8 C13 N2 116.5(4) . . ? C16 C17 C18 119.4(5) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? N3 C21 C22 123.1(5) . . ? N3 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C23 C22 C21 118.6(5) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? 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 O3 C1 141.9(4) . . . . ? O2 U1 O3 C1 -37.8(4) . . . . ? O4 U1 O3 C1 -128.0(4) . . . . ? N1 U1 O3 C1 50.5(4) . . . . ? N2 U1 O3 C1 45.9(5) . . . . ? N3 U1 O3 C1 -128.3(4) . . . . ? O1 U1 O4 C20 -147.9(4) . . . . ? O2 U1 O4 C20 31.5(4) . . . . ? O3 U1 O4 C20 121.6(4) . . . . ? N1 U1 O4 C20 -56.4(4) . . . . ? N2 U1 O4 C20 -53.7(4) . . . . ? N3 U1 O4 C20 121.9(4) . . . . ? O1 U1 N3 C21 -43.3(4) . . . . ? O2 U1 N3 C21 135.9(4) . . . . ? O3 U1 N3 C21 -134.3(4) . . . . ? O4 U1 N3 C21 45.8(4) . . . . ? N1 U1 N3 C21 -136.4(4) . . . . ? N2 U1 N3 C21 53.9(5) . . . . ? O1 U1 N3 C25 127.2(4) . . . . ? O2 U1 N3 C25 -53.6(4) . . . . ? O3 U1 N3 C25 36.2(4) . . . . ? O4 U1 N3 C25 -143.7(4) . . . . ? N1 U1 N3 C25 34.1(5) . . . . ? N2 U1 N3 C25 -135.6(4) . . . . ? O1 U1 N1 C7 -120.6(4) . . . . ? O2 U1 N1 C7 60.3(4) . . . . ? O3 U1 N1 C7 -30.1(4) . . . . ? O4 U1 N1 C7 149.0(3) . . . . ? N2 U1 N1 C7 146.1(4) . . . . ? N3 U1 N1 C7 -28.0(5) . . . . ? O1 U1 N1 C8 64.8(3) . . . . ? O2 U1 N1 C8 -114.3(3) . . . . ? O3 U1 N1 C8 155.3(3) . . . . ? O4 U1 N1 C8 -25.6(4) . . . . ? N2 U1 N1 C8 -28.5(3) . . . . ? N3 U1 N1 C8 157.4(3) . . . . ? C4 C5 C6 C1 -1.7(7) . . . . ? C4 C5 C6 C7 -179.0(4) . . . . ? N2 C14 C15 C16 173.4(5) . . . . ? N2 C14 C15 C20 -12.1(8) . . . . ? C17 C18 C19 C20 0.0(8) . . . . ? C12 C11 C10 C9 -0.3(8) . . . . ? C8 C9 C10 C11 -0.2(7) . . . . ? C10 C9 C8 C13 1.0(7) . . . . ? C10 C9 C8 N1 178.6(4) . . . . ? C7 N1 C8 C9 35.7(7) . . . . ? U1 N1 C8 C9 -149.2(4) . . . . ? C7 N1 C8 C13 -146.7(4) . . . . ? U1 N1 C8 C13 28.4(5) . . . . ? C20 C15 C16 C17 2.0(7) . . . . ? C14 C15 C16 C17 176.8(5) . . . . ? U1 O3 C1 C2 134.8(4) . . . . ? U1 O3 C1 C6 -47.1(6) . . . . ? C3 C2 C1 O3 178.9(4) . . . . ? C3 C2 C1 C6 0.8(7) . . . . ? C5 C6 C1 O3 -177.6(4) . . . . ? C7 C6 C1 O3 -0.4(7) . . . . ? C5 C6 C1 C2 0.6(7) . . . . ? C7 C6 C1 C2 177.7(4) . . . . ? C25 C24 C23 C22 -3.7(8) . . . . ? C8 N1 C7 C6 -175.1(4) . . . . ? U1 N1 C7 C6 10.4(7) . . . . ? C5 C6 C7 N1 -168.4(4) . . . . ? C1 C6 C7 N1 14.4(7) . . . . ? C21 N3 C25 C24 1.2(8) . . . . ? U1 N3 C25 C24 -169.7(4) . . . . ? C23 C24 C25 N3 1.6(8) . . . . ? C1 C2 C3 C4 -1.1(7) . . . . ? C15 C14 N2 C13 170.2(4) . . . . ? C15 C14 N2 U1 -16.8(7) . . . . ? O1 U1 N2 C14 124.1(4) . . . . ? O2 U1 N2 C14 -55.5(4) . . . . ? O3 U1 N2 C14 -141.1(4) . . . . ? O4 U1 N2 C14 36.3(4) . . . . ? N1 U1 N2 C14 -145.9(4) . . . . ? N3 U1 N2 C14 27.9(5) . . . . ? O1 U1 N2 C13 -62.7(3) . . . . ? O2 U1 N2 C13 117.7(3) . . . . ? O3 U1 N2 C13 32.1(4) . . . . ? O4 U1 N2 C13 -150.5(3) . . . . ? N1 U1 N2 C13 27.3(3) . . . . ? N3 U1 N2 C13 -158.9(3) . . . . ? C6 C5 C4 C3 1.4(7) . . . . ? C2 C3 C4 C5 0.1(7) . . . . ? C10 C11 C12 C13 0.1(7) . . . . ? U1 O4 C20 C19 -133.6(4) . . . . ? U1 O4 C20 C15 48.7(6) . . . . ? C18 C19 C20 O4 -175.6(5) . . . . ? C18 C19 C20 C15 2.1(7) . . . . ? C16 C15 C20 O4 174.7(4) . . . . ? C14 C15 C20 O4 0.2(7) . . . . ? C16 C15 C20 C19 -3.1(7) . . . . ? C14 C15 C20 C19 -177.6(5) . . . . ? C11 C12 C13 C8 0.7(7) . . . . ? C11 C12 C13 N2 -175.5(4) . . . . ? C9 C8 C13 C12 -1.2(7) . . . . ? N1 C8 C13 C12 -179.0(4) . . . . ? C9 C8 C13 N2 175.2(4) . . . . ? N1 C8 C13 N2 -2.5(6) . . . . ? C14 N2 C13 C12 -34.5(7) . . . . ? U1 N2 C13 C12 151.8(4) . . . . ? C14 N2 C13 C8 149.2(4) . . . . ? U1 N2 C13 C8 -24.5(5) . . . . ? C15 C16 C17 C18 0.1(8) . . . . ? C19 C18 C17 C16 -1.2(8) . . . . ? C25 N3 C21 C22 -1.9(8) . . . . ? U1 N3 C21 C22 168.8(4) . . . . ? C24 C23 C22 C21 3.1(8) . . . . ? N3 C21 C22 C23 -0.3(8) . . . . ? #===END #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary _ccdc_compound_id '[UO2(salen)(TPPO)].TPPO' # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _ccdc_temp_data_collection 100(2) _ccdc_ls_R_squared 0.0392 #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ data_bcas090p_1a _database_code_depnum_ccdc_archive 'CCDC 802712' #TrackingRef '- salmntall.cif' _audit_creation_date 2009-10-16T11:30:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; [UO2(salen)(TPPO)].TPPO ; _chemical_formula_sum 'C52 H44 N2 O6 P2 U' _chemical_formula_weight 1092.86 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.554(5) _cell_length_b 15.309(5) _cell_length_c 17.738(5) _cell_angle_alpha 97.947(5) _cell_angle_beta 92.478(5) _cell_angle_gamma 106.066(5) _cell_volume 2202.6(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3601 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 24.18 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.594060 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_unetI/netI 0.1167 _diffrn_reflns_number 16089 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.53 _diffrn_reflns_theta_full 25.53 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _reflns_number_total 8060 _reflns_number_gt 6271 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0444P)^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_number_reflns 8060 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.922 _refine_diff_density_min -1.347 _refine_diff_density_rms 0.211 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 1.24591(4) 1.48492(2) 0.628535(17) 0.01683(10) Uani 1 1 d . . . P1 P 1.1454(2) 1.48888(14) 0.83400(12) 0.0202(4) Uani 1 1 d . . . P2 P 0.7390(3) 1.03578(15) 0.83046(13) 0.0257(5) Uani 1 1 d . . . O4 O 1.3295(6) 1.3577(4) 0.6329(3) 0.0239(12) Uani 1 1 d . . . O3 O 1.1660(6) 1.6098(3) 0.6732(3) 0.0222(12) Uani 1 1 d . . . O2 O 1.0356(6) 1.4206(3) 0.6108(3) 0.0202(12) Uani 1 1 d . . . O1 O 1.4565(6) 1.5502(3) 0.6442(3) 0.0193(12) Uani 1 1 d . . . O5 O 1.2274(6) 1.4751(3) 0.7617(3) 0.0216(12) Uani 1 1 d . . . O6 O 0.8433(7) 1.0779(4) 0.9035(3) 0.0324(14) Uani 1 1 d . . . N1 N 1.2574(7) 1.5897(4) 0.5250(3) 0.0194(14) Uani 1 1 d . . . C28 C 0.8324(9) 1.3915(5) 0.8644(5) 0.0240(18) Uani 1 1 d . . . H28 H 0.8833 1.3691 0.9017 0.029 Uiso 1 1 calc R . . N2 N 1.2462(7) 1.4002(4) 0.4919(3) 0.0174(14) Uani 1 1 d . . . C6 C 1.2096(9) 1.7285(5) 0.5944(5) 0.0241(18) Uani 1 1 d . . . C41 C 0.5319(10) 1.0426(5) 0.8368(5) 0.0272(19) Uani 1 1 d . . . C26 C 0.5870(10) 1.3988(6) 0.7978(5) 0.0264(19) Uani 1 1 d . . . H26 H 0.4737 1.3817 0.79 0.032 Uiso 1 1 calc R . . C31 C 1.3235(10) 1.4154(6) 1.0252(5) 0.029(2) Uani 1 1 d . . . H31 H 1.3707 1.4433 1.0739 0.034 Uiso 1 1 calc R . . C16 C 1.3479(9) 1.2819(5) 0.5940(5) 0.0212(18) Uani 1 1 d . . . C2 C 1.1322(9) 1.7548(5) 0.7234(5) 0.0262(19) Uani 1 1 d . . . H2 H 1.104 1.7341 0.7693 0.031 Uiso 1 1 calc R . . C8 C 1.2965(9) 1.5490(5) 0.4498(4) 0.0218(18) Uani 1 1 d . . . H8A H 1.4121 1.5539 0.4511 0.026 Uiso 1 1 calc R . . H8B H 1.2705 1.5819 0.4103 0.026 Uiso 1 1 calc R . . C4 C 1.1747(11) 1.8757(6) 0.6472(5) 0.034(2) Uani 1 1 d . . . H4 H 1.1774 1.9357 0.6421 0.041 Uiso 1 1 calc R . . C48 C 0.8195(10) 0.8773(6) 0.8493(5) 0.030(2) Uani 1 1 d . . . H48 H 0.8908 0.914 0.8898 0.036 Uiso 1 1 calc R . . C15 C 1.4074(10) 1.2202(5) 0.6313(5) 0.032(2) Uani 1 1 d . . . H15 H 1.4371 1.234 0.6836 0.038 Uiso 1 1 calc R . . C17 C 1.1982(9) 1.6072(5) 0.8775(4) 0.0196(17) Uani 1 1 d . . . C5 C 1.2092(10) 1.8182(5) 0.5877(5) 0.028(2) Uani 1 1 d . . . H5 H 1.233 1.8397 0.5418 0.034 Uiso 1 1 calc R . . C1 C 1.1701(9) 1.6949(5) 0.6644(4) 0.0230(18) Uani 1 1 d . . . C27 C 0.6615(10) 1.3647(6) 0.8529(5) 0.0267(19) Uani 1 1 d . . . H27 H 0.599 1.3244 0.882 0.032 Uiso 1 1 calc R . . C10 C 1.2607(9) 1.3204(6) 0.4678(5) 0.0250(19) Uani 1 1 d . . . H10 H 1.2377 1.2994 0.4157 0.03 Uiso 1 1 calc R . . C45 C 0.2973(10) 1.0154(6) 0.9104(5) 0.034(2) Uani 1 1 d . . . H45 H 0.2463 0.9936 0.9521 0.041 Uiso 1 1 calc R . . C29 C 1.2076(8) 1.4265(5) 0.9023(4) 0.0190(17) Uani 1 1 d . . . C18 C 1.3438(10) 1.6677(6) 0.8641(5) 0.029(2) Uani 1 1 d . . . H18 H 1.4106 1.648 0.8297 0.034 Uiso 1 1 calc R . . C37 C 0.9343(11) 1.0888(7) 0.6292(5) 0.038(2) Uani 1 1 d . . . H37 H 0.9704 1.0572 0.5881 0.046 Uiso 1 1 calc R . . C21 C 1.1469(10) 1.7282(5) 0.9670(5) 0.028(2) Uani 1 1 d . . . H21 H 1.0812 1.7485 1.0017 0.033 Uiso 1 1 calc R . . C32 C 1.3028(10) 1.3236(6) 1.0034(5) 0.032(2) Uani 1 1 d . . . H32 H 1.3335 1.2892 1.0375 0.038 Uiso 1 1 calc R . . C35 C 0.8155(9) 1.0883(5) 0.7491(5) 0.0245(19) Uani 1 1 d . . . C14 C 1.4218(12) 1.1392(6) 0.5904(5) 0.038(2) Uani 1 1 d . . . H14 H 1.4591 1.099 0.6162 0.046 Uiso 1 1 calc R . . C23 C 0.9252(9) 1.4507(5) 0.8208(4) 0.0208(17) Uani 1 1 d . . . C49 C 0.8104(10) 0.7848(6) 0.8314(5) 0.029(2) Uani 1 1 d . . . H49 H 0.8748 0.7594 0.8602 0.035 Uiso 1 1 calc R . . C11 C 1.3094(9) 1.2591(5) 0.5137(5) 0.0232(18) Uani 1 1 d . . . C7 C 1.2483(9) 1.6726(5) 0.5296(4) 0.0206(17) Uani 1 1 d . . . H7 H 1.2691 1.6998 0.4859 0.025 Uiso 1 1 calc R . . C43 C 0.2906(11) 1.0844(6) 0.7991(6) 0.039(2) Uani 1 1 d . . . H43 H 0.2361 1.1091 0.7649 0.047 Uiso 1 1 calc R . . C34 C 1.1888(10) 1.3323(6) 0.8801(5) 0.030(2) Uani 1 1 d . . . H34 H 1.1441 1.3038 0.8311 0.036 Uiso 1 1 calc R . . C24 C 0.8482(9) 1.4847(5) 0.7660(4) 0.0231(18) Uani 1 1 d . . . H24 H 0.9101 1.5256 0.7371 0.028 Uiso 1 1 calc R . . C25 C 0.6805(9) 1.4582(5) 0.7543(4) 0.0243(18) Uani 1 1 d . . . H25 H 0.6298 1.4804 0.7168 0.029 Uiso 1 1 calc R . . C44 C 0.2159(11) 1.0527(6) 0.8605(6) 0.039(2) Uani 1 1 d . . . H44 H 0.111 1.0562 0.8686 0.047 Uiso 1 1 calc R . . C36 C 0.8712(10) 1.0434(6) 0.6880(5) 0.030(2) Uani 1 1 d . . . H36 H 0.8661 0.9817 0.6864 0.036 Uiso 1 1 calc R . . C40 C 0.8289(10) 1.1813(6) 0.7509(5) 0.031(2) Uani 1 1 d . . . H40 H 0.7963 1.2134 0.7928 0.037 Uiso 1 1 calc R . . C47 C 0.7222(10) 0.9147(5) 0.8068(5) 0.0247(18) Uani 1 1 d . . . C33 C 1.2364(11) 1.2819(6) 0.9307(5) 0.034(2) Uani 1 1 d . . . H33 H 1.2237 1.2195 0.9158 0.04 Uiso 1 1 calc R . . C38 C 0.9443(10) 1.1799(6) 0.6310(5) 0.036(2) Uani 1 1 d . . . H38 H 0.9881 1.2101 0.5914 0.043 Uiso 1 1 calc R . . C39 C 0.8894(11) 1.2270(6) 0.6916(5) 0.035(2) Uani 1 1 d . . . H39 H 0.8931 1.2884 0.6925 0.042 Uiso 1 1 calc R . . C52 C 0.6129(10) 0.8584(6) 0.7464(5) 0.028(2) Uani 1 1 d . . . H52 H 0.546 0.8832 0.7184 0.034 Uiso 1 1 calc R . . C20 C 1.2938(10) 1.7877(6) 0.9534(5) 0.030(2) Uani 1 1 d . . . H20 H 1.3269 1.8478 0.9792 0.037 Uiso 1 1 calc R . . C50 C 0.7059(10) 0.7306(6) 0.7708(5) 0.032(2) Uani 1 1 d . . . H50 H 0.7032 0.6691 0.7582 0.038 Uiso 1 1 calc R . . C19 C 1.3905(10) 1.7580(6) 0.9018(5) 0.031(2) Uani 1 1 d . . . H19 H 1.4879 1.7985 0.892 0.037 Uiso 1 1 calc R . . C22 C 1.0983(10) 1.6391(5) 0.9293(5) 0.0255(19) Uani 1 1 d . . . H22 H 0.9989 1.5996 0.9381 0.031 Uiso 1 1 calc R . . C42 C 0.4489(10) 1.0798(6) 0.7876(5) 0.032(2) Uani 1 1 d . . . H42 H 0.4991 1.1022 0.7459 0.039 Uiso 1 1 calc R . . C3 C 1.1357(10) 1.8427(6) 0.7152(5) 0.033(2) Uani 1 1 d . . . H3 H 1.1116 1.8811 0.7556 0.04 Uiso 1 1 calc R . . C9 C 1.1974(9) 1.4487(5) 0.4324(4) 0.0209(17) Uani 1 1 d . . . H9A H 1.0818 1.4435 0.4324 0.025 Uiso 1 1 calc R . . H9B H 1.2179 1.4215 0.3824 0.025 Uiso 1 1 calc R . . C46 C 0.4528(10) 1.0099(6) 0.8994(5) 0.030(2) Uani 1 1 d . . . H46 H 0.5058 0.9844 0.9336 0.036 Uiso 1 1 calc R . . C30 C 1.2757(9) 1.4676(6) 0.9762(4) 0.0243(19) Uani 1 1 d . . . H30 H 1.2886 1.5298 0.9922 0.029 Uiso 1 1 calc R . . C51 C 0.6044(10) 0.7663(6) 0.7283(5) 0.030(2) Uani 1 1 d . . . H51 H 0.5321 0.7288 0.6885 0.036 Uiso 1 1 calc R . . C13 C 1.3825(12) 1.1165(6) 0.5127(5) 0.041(2) Uani 1 1 d . . . H13 H 1.3938 1.062 0.4863 0.049 Uiso 1 1 calc R . . C12 C 1.3254(11) 1.1769(6) 0.4745(5) 0.035(2) Uani 1 1 d . . . H12 H 1.2975 1.1622 0.4221 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 0.01436(15) 0.02377(17) 0.01529(16) 0.00628(11) 0.00297(10) 0.00844(11) P1 0.0171(10) 0.0289(12) 0.0169(11) 0.0062(9) 0.0028(8) 0.0088(9) P2 0.0283(12) 0.0258(12) 0.0236(12) 0.0052(10) 0.0030(10) 0.0082(10) O4 0.029(3) 0.029(3) 0.017(3) 0.006(2) 0.002(2) 0.013(3) O3 0.023(3) 0.026(3) 0.023(3) 0.007(2) 0.003(2) 0.014(2) O2 0.016(3) 0.029(3) 0.017(3) 0.008(2) 0.004(2) 0.007(2) O1 0.017(3) 0.021(3) 0.020(3) 0.004(2) 0.002(2) 0.006(2) O5 0.020(3) 0.031(3) 0.018(3) 0.007(2) 0.007(2) 0.011(2) O6 0.032(3) 0.036(3) 0.026(3) 0.002(3) -0.002(3) 0.006(3) N1 0.018(3) 0.026(4) 0.015(3) 0.005(3) 0.003(3) 0.007(3) C28 0.021(4) 0.031(5) 0.021(4) 0.004(4) 0.002(3) 0.008(4) N2 0.015(3) 0.025(4) 0.015(3) 0.007(3) 0.004(3) 0.007(3) C6 0.021(4) 0.027(5) 0.028(5) 0.004(4) 0.005(4) 0.012(4) C41 0.035(5) 0.023(4) 0.024(5) 0.004(4) 0.006(4) 0.009(4) C26 0.016(4) 0.036(5) 0.028(5) 0.004(4) 0.003(4) 0.011(4) C31 0.025(5) 0.043(6) 0.021(5) 0.012(4) 0.002(4) 0.011(4) C16 0.018(4) 0.021(4) 0.025(5) 0.003(4) 0.008(3) 0.005(3) C2 0.026(4) 0.031(5) 0.025(5) 0.007(4) 0.007(4) 0.012(4) C8 0.021(4) 0.026(4) 0.023(4) 0.010(4) 0.004(3) 0.011(3) C4 0.046(6) 0.020(5) 0.046(6) 0.010(4) 0.021(5) 0.019(4) C48 0.025(5) 0.037(5) 0.033(5) 0.013(4) 0.011(4) 0.011(4) C15 0.039(5) 0.028(5) 0.029(5) 0.003(4) 0.002(4) 0.014(4) C17 0.016(4) 0.024(4) 0.021(4) 0.008(3) 0.004(3) 0.007(3) C5 0.029(5) 0.028(5) 0.028(5) 0.012(4) 0.005(4) 0.006(4) C1 0.019(4) 0.030(5) 0.020(4) 0.003(4) -0.003(3) 0.007(4) C27 0.026(5) 0.031(5) 0.026(5) 0.004(4) 0.009(4) 0.012(4) C10 0.023(4) 0.037(5) 0.017(4) 0.006(4) 0.007(3) 0.011(4) C45 0.025(5) 0.038(5) 0.040(6) 0.007(4) 0.017(4) 0.009(4) C29 0.010(4) 0.031(5) 0.018(4) 0.007(4) 0.005(3) 0.006(3) C18 0.022(4) 0.034(5) 0.032(5) 0.006(4) 0.004(4) 0.010(4) C37 0.037(5) 0.051(6) 0.031(5) 0.007(5) 0.013(4) 0.017(5) C21 0.033(5) 0.028(5) 0.027(5) 0.005(4) 0.007(4) 0.015(4) C32 0.029(5) 0.050(6) 0.027(5) 0.021(5) 0.007(4) 0.020(4) C35 0.021(4) 0.025(5) 0.025(5) 0.003(4) 0.004(4) 0.003(4) C14 0.057(6) 0.036(5) 0.031(5) 0.009(4) 0.001(5) 0.027(5) C23 0.021(4) 0.024(4) 0.016(4) -0.002(3) -0.002(3) 0.008(3) C49 0.027(5) 0.032(5) 0.035(5) 0.014(4) 0.011(4) 0.012(4) C11 0.025(4) 0.025(4) 0.024(5) 0.007(4) 0.006(4) 0.014(4) C7 0.022(4) 0.022(4) 0.021(4) 0.009(3) 0.003(3) 0.008(3) C43 0.035(5) 0.039(6) 0.045(6) 0.006(5) -0.003(5) 0.013(4) C34 0.032(5) 0.037(5) 0.021(5) 0.003(4) -0.002(4) 0.013(4) C24 0.025(4) 0.025(4) 0.022(4) 0.005(4) 0.002(4) 0.011(4) C25 0.028(5) 0.030(5) 0.017(4) 0.002(4) 0.001(4) 0.013(4) C44 0.035(5) 0.030(5) 0.051(6) 0.004(5) 0.012(5) 0.008(4) C36 0.040(5) 0.026(5) 0.028(5) 0.008(4) 0.003(4) 0.012(4) C40 0.032(5) 0.027(5) 0.032(5) 0.004(4) 0.008(4) 0.006(4) C47 0.027(4) 0.027(5) 0.021(4) 0.006(4) 0.009(4) 0.008(4) C33 0.042(5) 0.031(5) 0.034(5) 0.009(4) 0.006(4) 0.019(4) C38 0.026(5) 0.044(6) 0.035(6) 0.021(5) 0.005(4) -0.001(4) C39 0.041(5) 0.024(5) 0.039(6) 0.013(4) 0.003(4) 0.003(4) C52 0.030(5) 0.033(5) 0.025(5) 0.010(4) 0.004(4) 0.011(4) C20 0.035(5) 0.034(5) 0.024(5) 0.002(4) 0.001(4) 0.014(4) C50 0.037(5) 0.019(4) 0.045(6) 0.013(4) 0.023(5) 0.010(4) C19 0.023(4) 0.028(5) 0.037(5) 0.007(4) 0.003(4) 0.001(4) C22 0.021(4) 0.029(5) 0.030(5) 0.008(4) 0.008(4) 0.012(4) C42 0.036(5) 0.040(5) 0.026(5) 0.007(4) 0.001(4) 0.019(4) C3 0.037(5) 0.034(5) 0.032(5) 0.000(4) 0.013(4) 0.016(4) C9 0.019(4) 0.029(4) 0.016(4) 0.002(4) -0.002(3) 0.011(3) C46 0.033(5) 0.034(5) 0.028(5) 0.007(4) 0.004(4) 0.015(4) C30 0.020(4) 0.034(5) 0.017(4) 0.004(4) 0.004(3) 0.005(4) C51 0.023(5) 0.033(5) 0.032(5) 0.003(4) 0.010(4) 0.004(4) C13 0.062(7) 0.029(5) 0.039(6) 0.004(5) 0.007(5) 0.027(5) C12 0.057(6) 0.026(5) 0.021(5) 0.001(4) 0.000(4) 0.013(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O2 1.786(5) . ? U1 O1 1.790(5) . ? U1 O3 2.259(5) . ? U1 O4 2.263(5) . ? U1 O5 2.396(5) . ? U1 N2 2.586(6) . ? U1 N1 2.589(6) . ? P1 O5 1.506(5) . ? P1 C17 1.792(8) . ? P1 C29 1.792(8) . ? P1 C23 1.805(8) . ? P2 O6 1.496(6) . ? P2 C47 1.806(8) . ? P2 C35 1.808(8) . ? P2 C41 1.811(9) . ? O4 C16 1.318(9) . ? O3 C1 1.325(9) . ? N1 C7 1.284(9) . ? N1 C8 1.483(9) . ? C28 C23 1.379(10) . ? C28 C27 1.402(11) . ? C28 H28 0.93 . ? N2 C10 1.279(9) . ? N2 C9 1.480(9) . ? C6 C5 1.395(11) . ? C6 C1 1.426(11) . ? C6 C7 1.444(10) . ? C41 C42 1.378(11) . ? C41 C46 1.405(11) . ? C26 C27 1.379(11) . ? C26 C25 1.382(10) . ? C26 H26 0.93 . ? C31 C32 1.364(12) . ? C31 C30 1.379(11) . ? C31 H31 0.93 . ? C16 C15 1.414(11) . ? C16 C11 1.420(11) . ? C2 C3 1.367(11) . ? C2 C1 1.404(11) . ? C2 H2 0.93 . ? C8 C9 1.516(10) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C4 C5 1.375(11) . ? C4 C3 1.388(12) . ? C4 H4 0.93 . ? C48 C47 1.386(11) . ? C48 C49 1.386(11) . ? C48 H48 0.93 . ? C15 C14 1.386(11) . ? C15 H15 0.93 . ? C17 C18 1.383(10) . ? C17 C22 1.411(10) . ? C5 H5 0.93 . ? C27 H27 0.93 . ? C10 C11 1.455(11) . ? C10 H10 0.93 . ? C45 C46 1.377(11) . ? C45 C44 1.378(13) . ? C45 H45 0.93 . ? C29 C30 1.399(10) . ? C29 C34 1.403(11) . ? C18 C19 1.389(11) . ? C18 H18 0.93 . ? C37 C38 1.369(12) . ? C37 C36 1.380(11) . ? C37 H37 0.93 . ? C21 C22 1.375(11) . ? C21 C20 1.386(11) . ? C21 H21 0.93 . ? C32 C33 1.378(12) . ? C32 H32 0.93 . ? C35 C36 1.375(11) . ? C35 C40 1.392(11) . ? C14 C13 1.376(12) . ? C14 H14 0.93 . ? C23 C24 1.386(10) . ? C49 C50 1.379(12) . ? C49 H49 0.93 . ? C11 C12 1.395(11) . ? C7 H7 0.93 . ? C43 C44 1.367(12) . ? C43 C42 1.397(12) . ? C43 H43 0.93 . ? C34 C33 1.379(11) . ? C34 H34 0.93 . ? C24 C25 1.376(11) . ? C24 H24 0.93 . ? C25 H25 0.93 . ? C44 H44 0.93 . ? C36 H36 0.93 . ? C40 C39 1.383(11) . ? C40 H40 0.93 . ? C47 C52 1.406(11) . ? C33 H33 0.93 . ? C38 C39 1.384(12) . ? C38 H38 0.93 . ? C39 H39 0.93 . ? C52 C51 1.383(11) . ? C52 H52 0.93 . ? C20 C19 1.374(11) . ? C20 H20 0.93 . ? C50 C51 1.393(12) . ? C50 H50 0.93 . ? C19 H19 0.93 . ? C22 H22 0.93 . ? C42 H42 0.93 . ? C3 H3 0.93 . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C46 H46 0.93 . ? C30 H30 0.93 . ? C51 H51 0.93 . ? C13 C12 1.396(12) . ? C13 H13 0.93 . ? C12 H12 0.93 . ? 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 O2 U1 O1 178.7(2) . . ? O2 U1 O3 88.5(2) . . ? O1 U1 O3 91.4(2) . . ? O2 U1 O4 93.2(2) . . ? O1 U1 O4 87.4(2) . . ? O3 U1 O4 157.66(18) . . ? O2 U1 O5 89.1(2) . . ? O1 U1 O5 92.2(2) . . ? O3 U1 O5 77.02(18) . . ? O4 U1 O5 80.74(17) . . ? O2 U1 N2 79.9(2) . . ? O1 U1 N2 99.2(2) . . ? O3 U1 N2 132.38(19) . . ? O4 U1 N2 69.67(18) . . ? O5 U1 N2 147.56(18) . . ? O2 U1 N1 98.4(2) . . ? O1 U1 N1 80.3(2) . . ? O3 U1 N1 69.50(19) . . ? O4 U1 N1 131.98(19) . . ? O5 U1 N1 145.38(18) . . ? N2 U1 N1 66.92(19) . . ? O5 P1 C17 112.5(3) . . ? O5 P1 C29 109.6(3) . . ? C17 P1 C29 107.1(4) . . ? O5 P1 C23 113.9(3) . . ? C17 P1 C23 105.9(3) . . ? C29 P1 C23 107.4(4) . . ? O6 P2 C47 111.5(4) . . ? O6 P2 C35 113.5(4) . . ? C47 P2 C35 106.6(4) . . ? O6 P2 C41 111.9(4) . . ? C47 P2 C41 105.7(4) . . ? C35 P2 C41 107.2(4) . . ? C16 O4 U1 146.3(5) . . ? C1 O3 U1 145.4(5) . . ? P1 O5 U1 150.1(3) . . ? C7 N1 C8 115.5(6) . . ? C7 N1 U1 130.9(5) . . ? C8 N1 U1 113.3(4) . . ? C23 C28 C27 120.3(8) . . ? C23 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C10 N2 C9 115.3(6) . . ? C10 N2 U1 131.6(5) . . ? C9 N2 U1 112.4(4) . . ? C5 C6 C1 119.2(7) . . ? C5 C6 C7 118.5(7) . . ? C1 C6 C7 122.3(7) . . ? C42 C41 C46 117.9(8) . . ? C42 C41 P2 125.8(7) . . ? C46 C41 P2 116.3(6) . . ? C27 C26 C25 120.1(7) . . ? C27 C26 H26 120 . . ? C25 C26 H26 120 . . ? C32 C31 C30 121.1(8) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? O4 C16 C15 120.7(7) . . ? O4 C16 C11 121.7(7) . . ? C15 C16 C11 117.6(7) . . ? C3 C2 C1 121.5(8) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? N1 C8 C9 108.9(6) . . ? N1 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? N1 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C5 C4 C3 119.0(8) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C47 C48 C49 119.9(8) . . ? C47 C48 H48 120 . . ? C49 C48 H48 120 . . ? C14 C15 C16 120.4(8) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C18 C17 C22 118.8(7) . . ? C18 C17 P1 120.1(6) . . ? C22 C17 P1 121.0(6) . . ? C4 C5 C6 121.7(8) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? O3 C1 C2 120.8(7) . . ? O3 C1 C6 121.6(7) . . ? C2 C1 C6 117.6(7) . . ? C26 C27 C28 119.4(8) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? N2 C10 C11 126.6(7) . . ? N2 C10 H10 116.7 . . ? C11 C10 H10 116.7 . . ? C46 C45 C44 121.1(9) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C30 C29 C34 118.7(7) . . ? C30 C29 P1 123.0(6) . . ? C34 C29 P1 118.3(6) . . ? C17 C18 C19 120.3(8) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C38 C37 C36 120.4(8) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C22 C21 C20 120.1(8) . . ? C22 C21 H21 120 . . ? C20 C21 H21 120 . . ? C31 C32 C33 120.0(8) . . ? C31 C32 H32 120 . . ? C33 C32 H32 120 . . ? C36 C35 C40 118.1(8) . . ? C36 C35 P2 123.8(6) . . ? C40 C35 P2 117.9(6) . . ? C13 C14 C15 122.1(8) . . ? C13 C14 H14 119 . . ? C15 C14 H14 119 . . ? C28 C23 C24 119.4(7) . . ? C28 C23 P1 122.3(6) . . ? C24 C23 P1 118.2(6) . . ? C50 C49 C48 120.0(8) . . ? C50 C49 H49 120 . . ? C48 C49 H49 120 . . ? C12 C11 C16 120.3(7) . . ? C12 C11 C10 116.7(7) . . ? C16 C11 C10 122.9(7) . . ? N1 C7 C6 127.7(7) . . ? N1 C7 H7 116.1 . . ? C6 C7 H7 116.1 . . ? C44 C43 C42 120.0(9) . . ? C44 C43 H43 120 . . ? C42 C43 H43 120 . . ? C33 C34 C29 120.1(8) . . ? C33 C34 H34 119.9 . . ? C29 C34 H34 119.9 . . ? C25 C24 C23 120.4(8) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.4(8) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C43 C44 C45 119.5(9) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C35 C36 C37 120.9(8) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C39 C40 C35 121.4(8) . . ? C39 C40 H40 119.3 . . ? C35 C40 H40 119.3 . . ? C48 C47 C52 119.8(8) . . ? C48 C47 P2 118.9(7) . . ? C52 C47 P2 121.3(6) . . ? C32 C33 C34 120.3(8) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C37 C38 C39 120.1(8) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 119.0(8) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C51 C52 C47 120.3(8) . . ? C51 C52 H52 119.9 . . ? C47 C52 H52 119.9 . . ? C19 C20 C21 120.1(8) . . ? C19 C20 H20 120 . . ? C21 C20 H20 120 . . ? C49 C50 C51 121.1(8) . . ? C49 C50 H50 119.4 . . ? C51 C50 H50 119.4 . . ? C20 C19 C18 120.4(8) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C22 C17 120.4(7) . . ? C21 C22 H22 119.8 . . ? C17 C22 H22 119.8 . . ? C41 C42 C43 121.2(9) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C2 C3 C4 121.0(8) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? N2 C9 C8 108.1(6) . . ? N2 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? N2 C9 H9B 110.1 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? C45 C46 C41 120.3(8) . . ? C45 C46 H46 119.9 . . ? C41 C46 H46 119.9 . . ? C31 C30 C29 119.7(8) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C52 C51 C50 118.9(8) . . ? C52 C51 H51 120.5 . . ? C50 C51 H51 120.5 . . ? C14 C13 C12 118.6(8) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C11 C12 C13 121.1(8) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? 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 O2 U1 O4 C16 69.6(9) . . . . ? O1 U1 O4 C16 -109.2(9) . . . . ? O3 U1 O4 C16 163.4(7) . . . . ? O5 U1 O4 C16 158.1(9) . . . . ? N2 U1 O4 C16 -8.4(8) . . . . ? N1 U1 O4 C16 -34.7(9) . . . . ? O2 U1 O3 C1 -119.7(9) . . . . ? O1 U1 O3 C1 59.0(9) . . . . ? O4 U1 O3 C1 145.5(8) . . . . ? O5 U1 O3 C1 150.9(9) . . . . ? N2 U1 O3 C1 -45.0(9) . . . . ? N1 U1 O3 C1 -20.2(8) . . . . ? C17 P1 O5 U1 -76.4(7) . . . . ? C29 P1 O5 U1 164.5(6) . . . . ? C23 P1 O5 U1 44.2(7) . . . . ? O2 U1 O5 P1 -53.3(6) . . . . ? O1 U1 O5 P1 126.3(6) . . . . ? O3 U1 O5 P1 35.4(6) . . . . ? O4 U1 O5 P1 -146.7(7) . . . . ? N2 U1 O5 P1 -122.6(6) . . . . ? N1 U1 O5 P1 50.2(8) . . . . ? O2 U1 N1 C7 97.8(7) . . . . ? O1 U1 N1 C7 -82.6(7) . . . . ? O3 U1 N1 C7 12.6(6) . . . . ? O4 U1 N1 C7 -160.1(6) . . . . ? O5 U1 N1 C7 -2.9(8) . . . . ? N2 U1 N1 C7 173.0(7) . . . . ? O2 U1 N1 C8 -88.7(5) . . . . ? O1 U1 N1 C8 90.9(5) . . . . ? O3 U1 N1 C8 -173.8(5) . . . . ? O4 U1 N1 C8 13.4(6) . . . . ? O5 U1 N1 C8 170.7(4) . . . . ? N2 U1 N1 C8 -13.5(4) . . . . ? O2 U1 N2 C10 -85.5(7) . . . . ? O1 U1 N2 C10 95.5(7) . . . . ? O3 U1 N2 C10 -164.0(6) . . . . ? O4 U1 N2 C10 11.8(6) . . . . ? O5 U1 N2 C10 -13.7(8) . . . . ? N1 U1 N2 C10 170.7(7) . . . . ? O2 U1 N2 C9 84.5(5) . . . . ? O1 U1 N2 C9 -94.6(5) . . . . ? O3 U1 N2 C9 6.0(6) . . . . ? O4 U1 N2 C9 -178.2(5) . . . . ? O5 U1 N2 C9 156.3(4) . . . . ? N1 U1 N2 C9 -19.3(4) . . . . ? O6 P2 C41 C42 126.0(7) . . . . ? C47 P2 C41 C42 -112.4(8) . . . . ? C35 P2 C41 C42 1.0(9) . . . . ? O6 P2 C41 C46 -51.5(7) . . . . ? C47 P2 C41 C46 70.1(7) . . . . ? C35 P2 C41 C46 -176.5(6) . . . . ? U1 O4 C16 C15 -177.5(6) . . . . ? U1 O4 C16 C11 2.6(13) . . . . ? C7 N1 C8 C9 -141.4(7) . . . . ? U1 N1 C8 C9 44.1(7) . . . . ? O4 C16 C15 C14 178.0(8) . . . . ? C11 C16 C15 C14 -2.0(12) . . . . ? O5 P1 C17 C18 -25.0(8) . . . . ? C29 P1 C17 C18 95.6(7) . . . . ? C23 P1 C17 C18 -150.0(7) . . . . ? O5 P1 C17 C22 159.0(6) . . . . ? C29 P1 C17 C22 -80.4(7) . . . . ? C23 P1 C17 C22 34.0(7) . . . . ? C3 C4 C5 C6 -1.4(13) . . . . ? C1 C6 C5 C4 1.2(13) . . . . ? C7 C6 C5 C4 -179.5(8) . . . . ? U1 O3 C1 C2 -162.7(6) . . . . ? U1 O3 C1 C6 18.6(13) . . . . ? C3 C2 C1 O3 -179.9(7) . . . . ? C3 C2 C1 C6 -1.2(12) . . . . ? C5 C6 C1 O3 178.9(7) . . . . ? C7 C6 C1 O3 -0.4(12) . . . . ? C5 C6 C1 C2 0.1(11) . . . . ? C7 C6 C1 C2 -179.1(7) . . . . ? C25 C26 C27 C28 0.4(12) . . . . ? C23 C28 C27 C26 -0.5(12) . . . . ? C9 N2 C10 C11 178.9(7) . . . . ? U1 N2 C10 C11 -11.3(12) . . . . ? O5 P1 C29 C30 125.5(6) . . . . ? C17 P1 C29 C30 3.1(7) . . . . ? C23 P1 C29 C30 -110.3(6) . . . . ? O5 P1 C29 C34 -53.6(7) . . . . ? C17 P1 C29 C34 -176.0(6) . . . . ? C23 P1 C29 C34 70.6(7) . . . . ? C22 C17 C18 C19 0.6(12) . . . . ? P1 C17 C18 C19 -175.5(6) . . . . ? C30 C31 C32 C33 1.5(13) . . . . ? O6 P2 C35 C36 114.3(7) . . . . ? C47 P2 C35 C36 -8.8(8) . . . . ? C41 P2 C35 C36 -121.6(7) . . . . ? O6 P2 C35 C40 -61.3(8) . . . . ? C47 P2 C35 C40 175.6(6) . . . . ? C41 P2 C35 C40 62.8(7) . . . . ? C16 C15 C14 C13 1.3(14) . . . . ? C27 C28 C23 C24 0.9(11) . . . . ? C27 C28 C23 P1 179.1(6) . . . . ? O5 P1 C23 C28 127.9(6) . . . . ? C17 P1 C23 C28 -107.9(7) . . . . ? C29 P1 C23 C28 6.3(7) . . . . ? O5 P1 C23 C24 -53.9(7) . . . . ? C17 P1 C23 C24 70.3(7) . . . . ? C29 P1 C23 C24 -175.5(6) . . . . ? C47 C48 C49 C50 0.7(12) . . . . ? O4 C16 C11 C12 -178.0(7) . . . . ? C15 C16 C11 C12 2.1(12) . . . . ? O4 C16 C11 C10 5.3(12) . . . . ? C15 C16 C11 C10 -174.6(7) . . . . ? N2 C10 C11 C12 -176.7(8) . . . . ? N2 C10 C11 C16 0.1(13) . . . . ? C8 N1 C7 C6 178.7(7) . . . . ? U1 N1 C7 C6 -7.8(12) . . . . ? C5 C6 C7 N1 178.8(8) . . . . ? C1 C6 C7 N1 -1.9(13) . . . . ? C30 C29 C34 C33 0.2(12) . . . . ? P1 C29 C34 C33 179.4(7) . . . . ? C28 C23 C24 C25 -1.2(11) . . . . ? P1 C23 C24 C25 -179.5(6) . . . . ? C23 C24 C25 C26 1.2(12) . . . . ? C27 C26 C25 C24 -0.8(12) . . . . ? C42 C43 C44 C45 -0.6(14) . . . . ? C46 C45 C44 C43 0.2(14) . . . . ? C40 C35 C36 C37 -1.7(13) . . . . ? P2 C35 C36 C37 -177.3(7) . . . . ? C38 C37 C36 C35 0.7(14) . . . . ? C36 C35 C40 C39 2.8(13) . . . . ? P2 C35 C40 C39 178.7(7) . . . . ? C49 C48 C47 C52 1.0(12) . . . . ? C49 C48 C47 P2 -179.0(6) . . . . ? O6 P2 C47 C48 -8.7(8) . . . . ? C35 P2 C47 C48 115.6(7) . . . . ? C41 P2 C47 C48 -130.5(7) . . . . ? O6 P2 C47 C52 171.3(6) . . . . ? C35 P2 C47 C52 -64.4(7) . . . . ? C41 P2 C47 C52 49.5(7) . . . . ? C31 C32 C33 C34 -0.8(13) . . . . ? C29 C34 C33 C32 0.0(13) . . . . ? C36 C37 C38 C39 -0.7(14) . . . . ? C35 C40 C39 C38 -2.9(13) . . . . ? C37 C38 C39 C40 1.7(13) . . . . ? C48 C47 C52 C51 -1.2(12) . . . . ? P2 C47 C52 C51 178.7(6) . . . . ? C22 C21 C20 C19 0.5(13) . . . . ? C48 C49 C50 C51 -2.1(12) . . . . ? C21 C20 C19 C18 -1.3(13) . . . . ? C17 C18 C19 C20 0.8(13) . . . . ? C20 C21 C22 C17 0.9(12) . . . . ? C18 C17 C22 C21 -1.4(12) . . . . ? P1 C17 C22 C21 174.6(6) . . . . ? C46 C41 C42 C43 -0.4(13) . . . . ? P2 C41 C42 C43 -177.9(7) . . . . ? C44 C43 C42 C41 0.7(14) . . . . ? C1 C2 C3 C4 1.0(13) . . . . ? C5 C4 C3 C2 0.3(14) . . . . ? C10 N2 C9 C8 -138.9(7) . . . . ? U1 N2 C9 C8 49.4(7) . . . . ? N1 C8 C9 N2 -62.1(7) . . . . ? C44 C45 C46 C41 0.2(13) . . . . ? C42 C41 C46 C45 -0.1(12) . . . . ? P2 C41 C46 C45 177.7(7) . . . . ? C32 C31 C30 C29 -1.3(12) . . . . ? C34 C29 C30 C31 0.4(11) . . . . ? P1 C29 C30 C31 -178.8(6) . . . . ? C47 C52 C51 C50 -0.1(12) . . . . ? C49 C50 C51 C52 1.8(12) . . . . ? C15 C14 C13 C12 -0.5(15) . . . . ? C16 C11 C12 C13 -1.4(13) . . . . ? C10 C11 C12 C13 175.5(8) . . . . ? C14 C13 C12 C11 0.5(15) . . . . ?