data_UO2(NO3)2(L4d)2_(R=tBu) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H30 N4 O10 U ' _chemical_formula_sum 'C16 H30 N4 O10 U' _chemical_formula_weight 676.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y, z+1/2' _cell_length_a 17.364(6) _cell_length_b 7.385(3) _cell_length_c 18.031(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2312(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23945 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 7.076 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.1641 _exptl_absorpt_correction_T_max 0.5380 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 20977 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5129 _reflns_number_gt 4586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+7.8225P] 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 SHELXL _refine_ls_extinction_coef 0.00057(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.528(12) _refine_ls_number_reflns 5129 _refine_ls_number_parameters 282 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.373713(10) 0.008187(19) 0.40716(6) 0.02197(8) Uani 1 1 d . . . O1 O 0.4333(2) -0.1822(5) 0.4217(3) 0.0335(12) Uani 1 1 d . . . O2 O 0.3146(2) 0.1999(5) 0.3932(3) 0.0312(11) Uani 1 1 d . . . O3 O 0.4699(3) 0.1315(6) 0.3276(3) 0.0336(11) Uani 1 1 d . . . O4 O 0.2769(3) -0.1155(6) 0.4849(3) 0.0323(11) Uani 1 1 d . . . O5 O 0.4702(3) 0.2093(8) 0.4704(3) 0.0438(13) Uani 1 1 d . . . O6 O 0.3837(3) 0.0953(7) 0.5405(3) 0.0377(11) Uani 1 1 d . . . O7 O 0.4644(4) 0.2880(9) 0.5871(4) 0.0646(18) Uani 1 1 d . . . O8 O 0.2771(3) -0.1906(7) 0.3429(3) 0.0411(13) Uani 1 1 d . . . O9 O 0.3609(3) -0.0707(7) 0.2708(3) 0.0371(11) Uani 1 1 d . . . O10 O 0.2732(3) -0.2482(8) 0.2242(3) 0.0541(15) Uani 1 1 d . . . N1 N 0.5630(3) 0.3120(7) 0.2787(3) 0.0280(11) Uani 1 1 d . . . N2 N 0.1882(3) -0.2986(7) 0.5394(3) 0.0287(11) Uani 1 1 d . . . N3 N 0.4401(3) 0.2017(8) 0.5352(3) 0.0384(13) Uani 1 1 d . . . N4 N 0.3022(3) -0.1730(8) 0.2763(4) 0.0359(13) Uani 1 1 d . . . C1 C 0.4930(3) 0.2816(9) 0.3069(3) 0.0277(12) Uani 1 1 d . . . C2 C 0.4477(4) 0.4537(10) 0.3107(4) 0.0382(15) Uani 1 1 d . . . H2A H 0.4397 0.4914 0.3628 0.046 Uiso 1 1 calc R . . H2B H 0.3969 0.4392 0.2865 0.046 Uiso 1 1 calc R . . C3 C 0.4969(5) 0.5919(10) 0.2692(4) 0.0448(17) Uani 1 1 d . . . H3A H 0.4733 0.6221 0.2208 0.054 Uiso 1 1 calc R . . H3B H 0.5022 0.7045 0.2986 0.054 Uiso 1 1 calc R . . C4 C 0.5741(5) 0.5038(8) 0.2583(6) 0.0424(19) Uani 1 1 d . . . H4A H 0.5909 0.5145 0.2060 0.051 Uiso 1 1 calc R . . H4B H 0.6133 0.5609 0.2905 0.051 Uiso 1 1 calc R . . C5 C 0.6224(3) 0.1693(9) 0.2709(4) 0.0323(14) Uani 1 1 d . . . C6 C 0.5942(5) 0.0296(11) 0.2159(5) 0.0451(19) Uani 1 1 d . . . H6A H 0.5832 0.0886 0.1684 0.054 Uiso 1 1 calc R . . H6B H 0.5471 -0.0272 0.2349 0.054 Uiso 1 1 calc R . . H6C H 0.6339 -0.0631 0.2088 0.054 Uiso 1 1 calc R . . C7 C 0.6398(4) 0.0834(12) 0.3461(5) 0.0461(18) Uani 1 1 d . . . H7A H 0.6583 0.1767 0.3804 0.055 Uiso 1 1 calc R . . H7B H 0.6794 -0.0099 0.3401 0.055 Uiso 1 1 calc R . . H7C H 0.5928 0.0283 0.3660 0.055 Uiso 1 1 calc R . . C8 C 0.6971(4) 0.2528(12) 0.2412(6) 0.049(2) Uani 1 1 d . . . H8A H 0.7165 0.3422 0.2767 0.059 Uiso 1 1 calc R . . H8B H 0.6869 0.3121 0.1936 0.059 Uiso 1 1 calc R . . H8C H 0.7357 0.1573 0.2343 0.059 Uiso 1 1 calc R . . C9 C 0.2559(4) -0.2672(8) 0.5089(4) 0.0293(13) Uani 1 1 d . . . C10 C 0.3036(4) -0.4352(9) 0.5057(5) 0.0431(17) Uani 1 1 d . . . H10A H 0.3547 -0.4151 0.5286 0.052 Uiso 1 1 calc R . . H10B H 0.3109 -0.4754 0.4538 0.052 Uiso 1 1 calc R . . C11 C 0.2575(5) -0.5742(10) 0.5496(5) 0.0479(19) Uani 1 1 d . . . H11A H 0.2827 -0.5996 0.5977 0.057 Uiso 1 1 calc R . . H11B H 0.2531 -0.6888 0.5215 0.057 Uiso 1 1 calc R . . C12 C 0.1781(6) -0.4901(8) 0.5617(6) 0.045(2) Uani 1 1 d . . . H12A H 0.1388 -0.5505 0.5304 0.054 Uiso 1 1 calc R . . H12B H 0.1624 -0.4993 0.6143 0.054 Uiso 1 1 calc R . . C13 C 0.1258(3) -0.1612(9) 0.5466(4) 0.0337(14) Uani 1 1 d . . . C14 C 0.1547(5) -0.0091(8) 0.5980(6) 0.0406(18) Uani 1 1 d . . . H14A H 0.1671 -0.0599 0.6468 0.049 Uiso 1 1 calc R . . H14B H 0.1144 0.0829 0.6035 0.049 Uiso 1 1 calc R . . H14C H 0.2008 0.0464 0.5766 0.049 Uiso 1 1 calc R . . C15 C 0.1047(4) -0.0895(12) 0.4703(5) 0.0462(18) Uani 1 1 d . . . H15A H 0.1500 -0.0335 0.4475 0.055 Uiso 1 1 calc R . . H15B H 0.0637 0.0009 0.4751 0.055 Uiso 1 1 calc R . . H15C H 0.0867 -0.1897 0.4392 0.055 Uiso 1 1 calc R . . C16 C 0.0543(4) -0.2477(11) 0.5812(6) 0.048(2) Uani 1 1 d . . . H16A H 0.0669 -0.2927 0.6309 0.057 Uiso 1 1 calc R . . H16B H 0.0370 -0.3486 0.5501 0.057 Uiso 1 1 calc R . . H16C H 0.0132 -0.1572 0.5848 0.057 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 0.02083(11) 0.02077(11) 0.02432(11) -0.00162(19) 0.00223(12) 0.00006(6) O1 0.030(2) 0.029(2) 0.041(4) 0.0040(19) 0.001(2) 0.0061(15) O2 0.0303(19) 0.0305(19) 0.033(3) -0.0013(18) 0.0035(19) 0.0047(15) O3 0.029(2) 0.033(3) 0.039(3) 0.001(2) 0.008(2) -0.001(2) O4 0.034(2) 0.029(2) 0.034(3) 0.003(2) 0.008(2) -0.0006(19) O5 0.041(3) 0.060(4) 0.031(3) -0.003(3) 0.001(2) -0.018(3) O6 0.044(3) 0.041(3) 0.029(2) 0.001(2) 0.000(2) -0.008(2) O7 0.080(4) 0.074(4) 0.040(4) -0.014(3) -0.008(3) -0.032(4) O8 0.039(3) 0.046(3) 0.038(3) -0.007(3) 0.002(2) -0.014(2) O9 0.038(2) 0.043(3) 0.031(2) -0.005(2) 0.004(2) -0.006(2) O10 0.068(4) 0.060(3) 0.035(3) -0.016(3) -0.009(3) -0.017(3) N1 0.028(3) 0.027(3) 0.029(3) 0.000(2) 0.003(2) -0.0029(19) N2 0.026(2) 0.029(3) 0.032(3) -0.002(2) 0.003(2) -0.002(2) N3 0.044(3) 0.041(3) 0.031(3) -0.003(3) -0.004(3) -0.007(3) N4 0.038(3) 0.035(3) 0.035(3) -0.007(2) -0.001(3) -0.004(2) C1 0.029(3) 0.033(3) 0.021(3) 0.001(3) 0.000(3) -0.003(2) C2 0.036(4) 0.036(3) 0.042(4) 0.005(3) 0.010(3) 0.004(3) C3 0.066(5) 0.030(3) 0.038(4) 0.005(3) 0.009(4) 0.003(3) C4 0.043(4) 0.034(4) 0.051(5) 0.011(3) 0.012(4) -0.004(3) C5 0.030(3) 0.037(3) 0.030(3) -0.001(3) 0.000(3) -0.001(2) C6 0.045(4) 0.046(4) 0.044(5) -0.018(3) -0.002(4) 0.010(3) C7 0.040(4) 0.050(4) 0.048(5) 0.008(4) -0.002(3) 0.010(3) C8 0.026(3) 0.055(5) 0.067(6) 0.008(4) 0.014(4) 0.003(3) C9 0.035(3) 0.028(3) 0.025(3) -0.001(2) 0.002(3) 0.000(3) C10 0.044(4) 0.030(3) 0.055(5) 0.005(3) 0.014(4) 0.004(3) C11 0.064(5) 0.031(4) 0.049(5) 0.008(3) 0.019(4) 0.008(3) C12 0.053(5) 0.027(4) 0.056(6) 0.011(3) 0.013(4) -0.003(3) C13 0.029(3) 0.034(3) 0.038(4) -0.002(3) 0.002(3) 0.001(2) C14 0.039(4) 0.033(4) 0.050(5) -0.013(3) 0.006(4) 0.003(3) C15 0.031(4) 0.058(5) 0.050(4) 0.005(4) -0.001(3) 0.007(3) C16 0.029(3) 0.050(4) 0.064(6) 0.008(4) 0.016(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 1.766(4) . ? U1 O2 1.767(4) . ? U1 O4 2.371(5) . ? U1 O3 2.383(5) . ? U1 O6 2.496(5) . ? U1 O8 2.513(5) . ? U1 O5 2.513(5) . ? U1 O9 2.536(5) . ? U1 N3 2.950(6) . ? U1 N4 2.984(6) . ? O3 C1 1.236(8) . ? O4 C9 1.256(8) . ? O5 N3 1.280(8) . ? O6 N3 1.259(7) . ? O7 N3 1.209(8) . ? O8 N4 1.285(8) . ? O9 N4 1.274(7) . ? O10 N4 1.201(8) . ? N1 C1 1.338(8) . ? N1 C4 1.476(8) . ? N1 C5 1.481(8) . ? N2 C9 1.318(8) . ? N2 C12 1.481(7) . ? N2 C13 1.490(8) . ? C1 C2 1.496(9) . ? C2 C3 1.526(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.503(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.513(10) . ? C5 C7 1.527(10) . ? C5 C8 1.533(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.493(9) . ? C10 C11 1.523(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.528(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C15 1.518(11) . ? C13 C16 1.529(9) . ? C13 C14 1.541(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 179.5(3) . . ? O1 U1 O4 91.23(19) . . ? O2 U1 O4 88.90(18) . . ? O1 U1 O3 88.99(19) . . ? O2 U1 O3 90.89(19) . . ? O4 U1 O3 179.2(2) . . ? O1 U1 O6 91.2(2) . . ? O2 U1 O6 88.4(2) . . ? O4 U1 O6 65.12(17) . . ? O3 U1 O6 115.63(16) . . ? O1 U1 O8 89.7(2) . . ? O2 U1 O8 90.8(2) . . ? O4 U1 O8 64.79(18) . . ? O3 U1 O8 114.5(2) . . ? O6 U1 O8 129.90(17) . . ? O1 U1 O5 90.7(2) . . ? O2 U1 O5 88.77(19) . . ? O4 U1 O5 115.59(19) . . ? O3 U1 O5 65.16(18) . . ? O6 U1 O5 50.47(16) . . ? O8 U1 O5 179.4(2) . . ? O1 U1 O9 90.7(2) . . ? O2 U1 O9 89.7(2) . . ? O4 U1 O9 114.98(17) . . ? O3 U1 O9 64.27(17) . . ? O6 U1 O9 178.06(17) . . ? O8 U1 O9 50.24(17) . . ? O5 U1 O9 129.37(17) . . ? O1 U1 N3 92.3(2) . . ? O2 U1 N3 87.16(19) . . ? O4 U1 N3 90.07(17) . . ? O3 U1 N3 90.67(17) . . ? O6 U1 N3 25.00(15) . . ? O8 U1 N3 154.82(18) . . ? O5 U1 N3 25.53(16) . . ? O9 U1 N3 154.70(17) . . ? O1 U1 N4 90.3(2) . . ? O2 U1 N4 90.3(2) . . ? O4 U1 N4 89.97(17) . . ? O3 U1 N4 89.28(18) . . ? O6 U1 N4 155.07(15) . . ? O8 U1 N4 25.21(17) . . ? O5 U1 N4 154.40(18) . . ? O9 U1 N4 25.03(15) . . ? N3 U1 N4 177.42(17) . . ? C1 O3 U1 138.7(4) . . ? C9 O4 U1 138.9(4) . . ? N3 O5 U1 96.7(4) . . ? N3 O6 U1 98.1(4) . . ? N4 O8 U1 98.4(4) . . ? N4 O9 U1 97.6(4) . . ? C1 N1 C4 112.0(6) . . ? C1 N1 C5 123.3(5) . . ? C4 N1 C5 124.7(5) . . ? C9 N2 C12 112.7(6) . . ? C9 N2 C13 124.4(5) . . ? C12 N2 C13 122.7(6) . . ? O7 N3 O6 122.8(6) . . ? O7 N3 O5 122.8(6) . . ? O6 N3 O5 114.5(5) . . ? O7 N3 U1 176.6(5) . . ? O6 N3 U1 56.9(3) . . ? O5 N3 U1 57.8(3) . . ? O10 N4 O9 123.4(6) . . ? O10 N4 O8 122.8(6) . . ? O9 N4 O8 113.8(6) . . ? O10 N4 U1 179.0(5) . . ? O9 N4 U1 57.4(3) . . ? O8 N4 U1 56.4(3) . . ? O3 C1 N1 124.0(6) . . ? O3 C1 C2 125.3(6) . . ? N1 C1 C2 110.6(6) . . ? C1 C2 C3 104.6(6) . . ? C1 C2 H2A 110.8 . . ? C3 C2 H2A 110.8 . . ? C1 C2 H2B 110.8 . . ? C3 C2 H2B 110.8 . . ? H2A C2 H2B 108.9 . . ? C4 C3 C2 105.9(6) . . ? C4 C3 H3A 110.6 . . ? C2 C3 H3A 110.6 . . ? C4 C3 H3B 110.6 . . ? C2 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? N1 C4 C3 105.5(6) . . ? N1 C4 H4A 110.6 . . ? C3 C4 H4A 110.6 . . ? N1 C4 H4B 110.6 . . ? C3 C4 H4B 110.6 . . ? H4A C4 H4B 108.8 . . ? N1 C5 C6 108.8(5) . . ? N1 C5 C7 110.4(6) . . ? C6 C5 C7 111.3(7) . . ? N1 C5 C8 109.6(6) . . ? C6 C5 C8 108.6(7) . . ? C7 C5 C8 108.1(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 N2 124.1(6) . . ? O4 C9 C10 124.5(6) . . ? N2 C9 C10 111.4(6) . . ? C9 C10 C11 104.4(6) . . ? C9 C10 H10A 110.9 . . ? C11 C10 H10A 110.9 . . ? C9 C10 H10B 110.9 . . ? C11 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? C10 C11 C12 106.0(6) . . ? C10 C11 H11A 110.5 . . ? C12 C11 H11A 110.5 . . ? C10 C11 H11B 110.5 . . ? C12 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? N2 C12 C11 104.0(6) . . ? N2 C12 H12A 111.0 . . ? C11 C12 H12A 111.0 . . ? N2 C12 H12B 111.0 . . ? C11 C12 H12B 111.0 . . ? H12A C12 H12B 109.0 . . ? N2 C13 C15 109.5(6) . . ? N2 C13 C16 110.0(6) . . ? C15 C13 C16 108.6(6) . . ? N2 C13 C14 108.2(5) . . ? C15 C13 C14 111.7(6) . . ? C16 C13 C14 108.9(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 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 O3 C1 -152.0(7) . . . . ? O2 U1 O3 C1 27.5(7) . . . . ? O4 U1 O3 C1 102(12) . . . . ? O6 U1 O3 C1 -61.1(7) . . . . ? O8 U1 O3 C1 118.8(7) . . . . ? O5 U1 O3 C1 -60.8(7) . . . . ? O9 U1 O3 C1 116.7(7) . . . . ? N3 U1 O3 C1 -59.7(7) . . . . ? N4 U1 O3 C1 117.7(7) . . . . ? O1 U1 O4 C9 -22.4(7) . . . . ? O2 U1 O4 C9 158.1(7) . . . . ? O3 U1 O4 C9 83(12) . . . . ? O6 U1 O4 C9 -113.2(7) . . . . ? O8 U1 O4 C9 66.7(7) . . . . ? O5 U1 O4 C9 -113.8(7) . . . . ? O9 U1 O4 C9 68.9(7) . . . . ? N3 U1 O4 C9 -114.8(7) . . . . ? N4 U1 O4 C9 67.8(7) . . . . ? O1 U1 O5 N3 -93.9(4) . . . . ? O2 U1 O5 N3 86.0(4) . . . . ? O4 U1 O5 N3 -2.2(5) . . . . ? O3 U1 O5 N3 177.5(5) . . . . ? O6 U1 O5 N3 -2.9(4) . . . . ? O8 U1 O5 N3 129(22) . . . . ? O9 U1 O5 N3 174.6(4) . . . . ? N4 U1 O5 N3 174.0(4) . . . . ? O1 U1 O6 N3 92.9(4) . . . . ? O2 U1 O6 N3 -86.8(4) . . . . ? O4 U1 O6 N3 -176.4(4) . . . . ? O3 U1 O6 N3 3.4(4) . . . . ? O8 U1 O6 N3 -176.5(4) . . . . ? O5 U1 O6 N3 3.0(4) . . . . ? O9 U1 O6 N3 -83(5) . . . . ? N4 U1 O6 N3 -173.9(4) . . . . ? O1 U1 O8 N4 -91.2(4) . . . . ? O2 U1 O8 N4 88.9(4) . . . . ? O4 U1 O8 N4 177.3(5) . . . . ? O3 U1 O8 N4 -2.5(4) . . . . ? O6 U1 O8 N4 177.4(4) . . . . ? O5 U1 O8 N4 46(23) . . . . ? O9 U1 O8 N4 -0.1(4) . . . . ? N3 U1 O8 N4 173.9(4) . . . . ? O1 U1 O9 N4 89.1(4) . . . . ? O2 U1 O9 N4 -91.2(4) . . . . ? O4 U1 O9 N4 -2.6(4) . . . . ? O3 U1 O9 N4 177.6(4) . . . . ? O6 U1 O9 N4 -95(5) . . . . ? O8 U1 O9 N4 0.1(4) . . . . ? O5 U1 O9 N4 -179.4(3) . . . . ? N3 U1 O9 N4 -174.0(4) . . . . ? U1 O6 N3 O7 176.0(6) . . . . ? U1 O6 N3 O5 -4.9(6) . . . . ? U1 O5 N3 O7 -176.0(6) . . . . ? U1 O5 N3 O6 4.9(6) . . . . ? O1 U1 N3 O7 -173(9) . . . . ? O2 U1 N3 O7 7(9) . . . . ? O4 U1 N3 O7 -82(9) . . . . ? O3 U1 N3 O7 98(9) . . . . ? O6 U1 N3 O7 -85(9) . . . . ? O8 U1 N3 O7 -79(9) . . . . ? O5 U1 N3 O7 100(9) . . . . ? O9 U1 N3 O7 90(9) . . . . ? N4 U1 N3 O7 9(11) . . . . ? O1 U1 N3 O6 -87.9(4) . . . . ? O2 U1 N3 O6 92.2(4) . . . . ? O4 U1 N3 O6 3.3(4) . . . . ? O3 U1 N3 O6 -176.9(4) . . . . ? O8 U1 N3 O6 6.3(6) . . . . ? O5 U1 N3 O6 -174.7(7) . . . . ? O9 U1 N3 O6 175.5(4) . . . . ? N4 U1 N3 O6 94(4) . . . . ? O1 U1 N3 O5 86.8(4) . . . . ? O2 U1 N3 O5 -93.1(4) . . . . ? O4 U1 N3 O5 178.0(4) . . . . ? O3 U1 N3 O5 -2.2(4) . . . . ? O6 U1 N3 O5 174.7(7) . . . . ? O8 U1 N3 O5 -179.0(5) . . . . ? O9 U1 N3 O5 -9.8(7) . . . . ? N4 U1 N3 O5 -91(4) . . . . ? U1 O9 N4 O10 -179.3(6) . . . . ? U1 O9 N4 O8 -0.1(6) . . . . ? U1 O8 N4 O10 179.3(6) . . . . ? U1 O8 N4 O9 0.1(6) . . . . ? O1 U1 N4 O10 51(30) . . . . ? O2 U1 N4 O10 -129(30) . . . . ? O4 U1 N4 O10 -40(30) . . . . ? O3 U1 N4 O10 140(30) . . . . ? O6 U1 N4 O10 -43(30) . . . . ? O8 U1 N4 O10 -38(30) . . . . ? O5 U1 N4 O10 143(30) . . . . ? O9 U1 N4 O10 142(30) . . . . ? N3 U1 N4 O10 -131(29) . . . . ? O1 U1 N4 O9 -91.1(4) . . . . ? O2 U1 N4 O9 88.7(4) . . . . ? O4 U1 N4 O9 177.7(4) . . . . ? O3 U1 N4 O9 -2.1(4) . . . . ? O6 U1 N4 O9 175.4(4) . . . . ? O8 U1 N4 O9 -179.9(6) . . . . ? O5 U1 N4 O9 1.0(6) . . . . ? N3 U1 N4 O9 87(4) . . . . ? O1 U1 N4 O8 88.8(4) . . . . ? O2 U1 N4 O8 -91.3(4) . . . . ? O4 U1 N4 O8 -2.4(4) . . . . ? O3 U1 N4 O8 177.8(4) . . . . ? O6 U1 N4 O8 -4.7(6) . . . . ? O5 U1 N4 O8 -179.0(5) . . . . ? O9 U1 N4 O8 179.9(6) . . . . ? N3 U1 N4 O8 -93(4) . . . . ? U1 O3 C1 N1 159.0(5) . . . . ? U1 O3 C1 C2 -20.1(11) . . . . ? C4 N1 C1 O3 179.6(7) . . . . ? C5 N1 C1 O3 -1.8(10) . . . . ? C4 N1 C1 C2 -1.3(9) . . . . ? C5 N1 C1 C2 177.3(6) . . . . ? O3 C1 C2 C3 -172.5(7) . . . . ? N1 C1 C2 C3 8.3(8) . . . . ? C1 C2 C3 C4 -11.8(9) . . . . ? C1 N1 C4 C3 -6.4(9) . . . . ? C5 N1 C4 C3 175.0(6) . . . . ? C2 C3 C4 N1 11.2(9) . . . . ? C1 N1 C5 C6 64.8(9) . . . . ? C4 N1 C5 C6 -116.7(8) . . . . ? C1 N1 C5 C7 -57.6(8) . . . . ? C4 N1 C5 C7 120.9(8) . . . . ? C1 N1 C5 C8 -176.5(7) . . . . ? C4 N1 C5 C8 1.9(10) . . . . ? U1 O4 C9 N2 -164.3(5) . . . . ? U1 O4 C9 C10 14.8(11) . . . . ? C12 N2 C9 O4 179.0(7) . . . . ? C13 N2 C9 O4 3.0(11) . . . . ? C12 N2 C9 C10 -0.2(9) . . . . ? C13 N2 C9 C10 -176.3(6) . . . . ? O4 C9 C10 C11 173.3(7) . . . . ? N2 C9 C10 C11 -7.4(9) . . . . ? C9 C10 C11 C12 11.7(9) . . . . ? C9 N2 C12 C11 7.7(9) . . . . ? C13 N2 C12 C11 -176.1(6) . . . . ? C10 C11 C12 N2 -11.8(9) . . . . ? C9 N2 C13 C15 57.9(8) . . . . ? C12 N2 C13 C15 -117.7(8) . . . . ? C9 N2 C13 C16 177.2(7) . . . . ? C12 N2 C13 C16 1.5(10) . . . . ? C9 N2 C13 C14 -64.0(9) . . . . ? C12 N2 C13 C14 120.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 4.348 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.114