# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'M. Ephritikhine' 'Pierre Thuery' 'Claude Villiers' _publ_contact_author_name 'M. Ephritikhine' _publ_contact_author_address ; Laboratoire de Chimie de coordination Service de Chimie Moleculaire CEA Saclay, Batiment 125 Gif sur Yvette 91191 Gif sur Yvette F91191 FRANCE ; _publ_contact_author_email EPHRI@DRECAM.CEA.FR _publ_requested_journal 'Chemical Communications' _publ_section_title ; The first urea azine molecule and its coordination to uranium in the first actinide guanidinate complexes ; data_1 _database_code_depnum_ccdc_archive 'CCDC 643701' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H48 N6' _chemical_formula_weight 444.70 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.1574(16) _cell_length_b 17.4268(19) _cell_length_c 12.5035(9) _cell_angle_alpha 90.00 _cell_angle_beta 126.373(6) _cell_angle_gamma 90.00 _cell_volume 2659.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 62798 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type none _exptl_special_details 'crystal-to-detector distance 30 mm' _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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and eight \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 62798 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.68 _reflns_number_total 2524 _reflns_number_gt 2140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms bound to N atoms were found on a Fourier-difference map and all the other ones were introduced at calculated positions. All were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0570P)^2^+0.7723P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2524 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.150 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.037 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 N1 N 0.54444(8) -0.00261(5) 0.06897(9) 0.0290(2) Uani 1 1 d . . . N2 N 0.46713(8) 0.11367(5) 0.07896(9) 0.0283(2) Uani 1 1 d . . . H2 H 0.4143 0.1014 -0.0176 0.034 Uiso 1 1 d R . . N3 N 0.63286(8) 0.06639(6) 0.26692(9) 0.0296(2) Uani 1 1 d . . . H3 H 0.6112 0.0918 0.3162 0.036 Uiso 1 1 d R . . C1 C 0.54783(9) 0.05659(6) 0.13421(11) 0.0273(3) Uani 1 1 d . . . C2 C 0.50045(9) 0.19555(7) 0.10439(11) 0.0281(3) Uani 1 1 d . . . H2A H 0.5448 0.2045 0.2004 0.034 Uiso 1 1 calc R . . C3 C 0.39751(10) 0.24534(7) 0.03778(11) 0.0311(3) Uani 1 1 d . . . H3A H 0.4188 0.2977 0.0694 0.037 Uiso 1 1 calc R . . H3B H 0.3522 0.2269 0.0636 0.037 Uiso 1 1 calc R . . C4 C 0.32996(10) 0.24497(7) -0.11387(12) 0.0326(3) Uani 1 1 d . . . H4A H 0.2696 0.2809 -0.1504 0.039 Uiso 1 1 calc R . . H4B H 0.2994 0.1942 -0.1470 0.039 Uiso 1 1 calc R . . C5 C 0.40005(10) 0.26712(7) -0.16018(12) 0.0335(3) Uani 1 1 d . . . H5A H 0.3567 0.2623 -0.2560 0.040 Uiso 1 1 calc R . . H5B H 0.4226 0.3203 -0.1374 0.040 Uiso 1 1 calc R . . C6 C 0.50152(10) 0.21614(7) -0.09595(12) 0.0326(3) Uani 1 1 d . . . H6A H 0.5465 0.2335 -0.1228 0.039 Uiso 1 1 calc R . . H6B H 0.4791 0.1638 -0.1267 0.039 Uiso 1 1 calc R . . C7 C 0.56883(10) 0.21809(7) 0.05547(11) 0.0311(3) Uani 1 1 d . . . H7A H 0.5979 0.2694 0.0867 0.037 Uiso 1 1 calc R . . H7B H 0.6303 0.1831 0.0929 0.037 Uiso 1 1 calc R . . C8 C 0.71246(9) 0.00443(6) 0.34129(11) 0.0290(3) Uani 1 1 d . . . H8 H 0.7290 -0.0189 0.2837 0.035 Uiso 1 1 calc R . . C9 C 0.81822(10) 0.03867(7) 0.46202(12) 0.0351(3) Uani 1 1 d . . . H9A H 0.8023 0.0656 0.5166 0.042 Uiso 1 1 calc R . . H9B H 0.8475 0.0755 0.4324 0.042 Uiso 1 1 calc R . . C10 C 0.90402(10) -0.02345(8) 0.54513(13) 0.0393(3) Uani 1 1 d . . . H10A H 0.9267 -0.0460 0.4941 0.047 Uiso 1 1 calc R . . H10B H 0.9679 -0.0003 0.6240 0.047 Uiso 1 1 calc R . . C11 C 0.85946(10) -0.08631(8) 0.58625(12) 0.0364(3) Uani 1 1 d . . . H11A H 0.9141 -0.1263 0.6337 0.044 Uiso 1 1 calc R . . H11B H 0.8444 -0.0650 0.6455 0.044 Uiso 1 1 calc R . . C12 C 0.75486(10) -0.12054(7) 0.46479(12) 0.0334(3) Uani 1 1 d . . . H12A H 0.7259 -0.1587 0.4930 0.040 Uiso 1 1 calc R . . H12B H 0.7713 -0.1459 0.4095 0.040 Uiso 1 1 calc R . . C13 C 0.66890(9) -0.05826(7) 0.38427(11) 0.0307(3) Uani 1 1 d . . . H13A H 0.6483 -0.0357 0.4375 0.037 Uiso 1 1 calc R . . H13B H 0.6039 -0.0811 0.3062 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 N1 0.0292(5) 0.0302(5) 0.0228(5) 0.0016(4) 0.0128(4) 0.0014(4) N2 0.0291(5) 0.0265(5) 0.0261(5) 0.0018(4) 0.0145(4) 0.0009(4) N3 0.0304(5) 0.0294(5) 0.0243(5) 0.0008(4) 0.0136(4) 0.0033(4) C1 0.0276(6) 0.0274(6) 0.0264(6) 0.0029(4) 0.0158(5) 0.0007(5) C2 0.0305(6) 0.0272(6) 0.0247(6) -0.0003(4) 0.0154(5) 0.0004(5) C3 0.0339(6) 0.0311(6) 0.0304(6) 0.0023(5) 0.0203(5) 0.0033(5) C4 0.0319(6) 0.0329(6) 0.0299(6) 0.0038(5) 0.0166(5) 0.0042(5) C5 0.0380(7) 0.0343(7) 0.0278(6) 0.0034(5) 0.0193(5) 0.0019(5) C6 0.0363(6) 0.0343(7) 0.0311(6) 0.0024(5) 0.0222(5) 0.0015(5) C7 0.0310(6) 0.0300(6) 0.0315(6) 0.0010(5) 0.0180(5) 0.0001(5) C8 0.0297(6) 0.0287(6) 0.0255(6) 0.0016(5) 0.0148(5) 0.0024(5) C9 0.0327(6) 0.0323(6) 0.0310(6) 0.0028(5) 0.0137(5) -0.0033(5) C10 0.0294(6) 0.0410(7) 0.0340(7) 0.0064(5) 0.0116(5) -0.0015(5) C11 0.0330(6) 0.0373(7) 0.0319(6) 0.0077(5) 0.0154(5) 0.0031(5) C12 0.0333(6) 0.0305(6) 0.0346(7) 0.0042(5) 0.0192(5) 0.0013(5) C13 0.0290(6) 0.0307(6) 0.0293(6) 0.0003(5) 0.0157(5) -0.0006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.2971(15) . ? N1 N1 1.4290(18) 5_655 ? N2 C1 1.4004(14) . ? N2 C2 1.4837(15) . ? N2 H2 0.9990 . ? N3 C1 1.3809(14) . ? N3 C8 1.4681(14) . ? N3 H3 0.9603 . ? C2 C3 1.5296(16) . ? C2 C7 1.5344(16) . ? C2 H2A 0.9800 . ? C3 C4 1.5300(16) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.5305(17) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.5280(17) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.5282(16) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.5278(16) . ? C8 C13 1.5295(16) . ? C8 H8 0.9800 . ? C9 C10 1.5298(17) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.5273(18) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.5232(17) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.5275(16) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? 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 C1 N1 N1 111.46(11) . 5_655 ? C1 N2 C2 119.38(9) . . ? C1 N2 H2 106.5 . . ? C2 N2 H2 113.0 . . ? C1 N3 C8 120.06(9) . . ? C1 N3 H3 113.4 . . ? C8 N3 H3 113.4 . . ? N1 C1 N3 120.98(10) . . ? N1 C1 N2 123.88(10) . . ? N3 C1 N2 115.13(10) . . ? N2 C2 C3 108.73(9) . . ? N2 C2 C7 112.67(9) . . ? C3 C2 C7 110.47(9) . . ? N2 C2 H2A 108.3 . . ? C3 C2 H2A 108.3 . . ? C7 C2 H2A 108.3 . . ? C2 C3 C4 112.91(10) . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 C5 111.30(10) . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 111.27(10) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 111.26(10) . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C6 C7 C2 112.06(10) . . ? C6 C7 H7A 109.2 . . ? C2 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C2 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N3 C8 C9 108.98(9) . . ? N3 C8 C13 112.58(9) . . ? C9 C8 C13 110.51(9) . . ? N3 C8 H8 108.2 . . ? C9 C8 H8 108.2 . . ? C13 C8 H8 108.2 . . ? C8 C9 C10 111.47(10) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 111.63(10) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 110.61(10) . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 C13 110.82(10) . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C12 C13 C8 111.22(9) . . ? C12 C13 H13A 109.4 . . ? C8 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? C8 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? 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 N2 H2 N1 1.00 2.06 2.6103(13) 112.4 5_655 N3 H3 N2 0.96 2.26 3.1864(14) 160.9 2_655 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 643702' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H124 Cl6 Li2 N12 O4 U2' _chemical_formula_weight 1876.43 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.2729(6) _cell_length_b 21.7473(6) _cell_length_c 22.4638(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7949.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 157305 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light green' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3760 _exptl_absorpt_coefficient_mu 4.322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.370 _exptl_absorpt_correction_T_max 0.649 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 mm' _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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and three \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 157305 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7519 _reflns_number_gt 5555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms bound to N atoms were found on a Fourier-difference map and all the others were introduced at calculated positions. All were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0235P)^2^+2.5276P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7519 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.524 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.107 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 U U 0.587132(8) 0.007858(6) 0.066408(6) 0.02521(6) Uani 1 1 d . . . Li Li 0.7675(4) 0.0034(3) 0.1673(3) 0.0385(16) Uani 1 1 d . . . Cl1 Cl 0.68149(6) -0.07525(4) 0.13390(4) 0.0365(2) Uani 1 1 d . . . Cl2 Cl 0.72631(6) 0.07614(4) 0.09872(4) 0.0310(2) Uani 1 1 d . . . Cl3 Cl 0.51160(6) 0.03165(4) 0.17012(4) 0.0338(2) Uani 1 1 d . . . N1 N 0.55259(18) 0.02220(13) -0.03828(13) 0.0246(7) Uani 1 1 d . . . N2 N 0.50794(18) 0.07619(13) -0.05791(12) 0.0266(7) Uani 1 1 d . . . N3 N 0.67296(18) -0.02102(13) -0.02107(13) 0.0261(7) Uani 1 1 d . . . N4 N 0.65816(18) 0.04208(13) -0.10973(13) 0.0278(7) Uani 1 1 d . . . H4 H 0.6021 0.0519 -0.1229 0.033 Uiso 1 1 d R . . N5 N 0.54391(19) 0.10937(13) 0.03874(13) 0.0252(7) Uani 1 1 d . . . N6 N 0.47104(19) 0.17402(13) -0.02755(13) 0.0302(8) Uani 1 1 d . . . H6 H 0.4651 0.2006 0.0020 0.036 Uiso 1 1 d R . . O1 O 0.88210(17) -0.01692(13) 0.16800(13) 0.0450(7) Uani 1 1 d . . . O2 O 0.75668(17) 0.03537(12) 0.24725(11) 0.0390(7) Uani 1 1 d . . . C1 C 0.6319(2) 0.01410(16) -0.05805(16) 0.0271(9) Uani 1 1 d . . . C2 C 0.7495(2) -0.05229(16) -0.03811(16) 0.0287(9) Uani 1 1 d . . . H2 H 0.7582 -0.0464 -0.0809 0.034 Uiso 1 1 calc R . . C3 C 0.7392(2) -0.12094(15) -0.02608(17) 0.0313(9) Uani 1 1 d . . . H3A H 0.6940 -0.1365 -0.0498 0.038 Uiso 1 1 calc R . . H3B H 0.7254 -0.1270 0.0155 0.038 Uiso 1 1 calc R . . C4 C 0.8168(2) -0.15744(17) -0.04068(19) 0.0368(10) Uani 1 1 d . . . H4A H 0.8090 -0.2000 -0.0291 0.044 Uiso 1 1 calc R . . H4B H 0.8263 -0.1563 -0.0833 0.044 Uiso 1 1 calc R . . C5 C 0.8912(2) -0.13150(17) -0.00863(18) 0.0379(11) Uani 1 1 d . . . H5A H 0.8848 -0.1371 0.0340 0.045 Uiso 1 1 calc R . . H5B H 0.9401 -0.1536 -0.0210 0.045 Uiso 1 1 calc R . . C6 C 0.9014(2) -0.06370(17) -0.02238(18) 0.0350(10) Uani 1 1 d . . . H6A H 0.9121 -0.0584 -0.0646 0.042 Uiso 1 1 calc R . . H6B H 0.9481 -0.0476 -0.0006 0.042 Uiso 1 1 calc R . . C7 C 0.8243(2) -0.02778(17) -0.00527(18) 0.0321(10) Uani 1 1 d . . . H7A H 0.8154 -0.0311 0.0373 0.039 Uiso 1 1 calc R . . H7B H 0.8319 0.0153 -0.0149 0.039 Uiso 1 1 calc R . . C8 C 0.7314(2) 0.08139(17) -0.11289(16) 0.0321(9) Uani 1 1 d . . . H8 H 0.7804 0.0555 -0.1092 0.038 Uiso 1 1 calc R . . C9 C 0.7314(3) 0.11175(18) -0.17433(16) 0.0365(10) Uani 1 1 d . . . H9A H 0.7403 0.0805 -0.2044 0.044 Uiso 1 1 calc R . . H9B H 0.6779 0.1301 -0.1815 0.044 Uiso 1 1 calc R . . C10 C 0.7967(3) 0.16070(19) -0.18048(18) 0.0449(11) Uani 1 1 d . . . H10A H 0.7905 0.1811 -0.2186 0.054 Uiso 1 1 calc R . . H10B H 0.8505 0.1415 -0.1796 0.054 Uiso 1 1 calc R . . C11 C 0.7914(3) 0.20804(19) -0.13123(18) 0.0460(12) Uani 1 1 d . . . H11A H 0.7391 0.2294 -0.1335 0.055 Uiso 1 1 calc R . . H11B H 0.8349 0.2381 -0.1360 0.055 Uiso 1 1 calc R . . C12 C 0.7995(3) 0.17650(19) -0.07042(18) 0.0463(12) Uani 1 1 d . . . H12A H 0.8527 0.1566 -0.0675 0.056 Uiso 1 1 calc R . . H12B H 0.7957 0.2070 -0.0390 0.056 Uiso 1 1 calc R . . C13 C 0.7319(3) 0.12914(17) -0.06289(17) 0.0355(10) Uani 1 1 d . . . H13A H 0.6792 0.1499 -0.0620 0.043 Uiso 1 1 calc R . . H13B H 0.7392 0.1083 -0.0251 0.043 Uiso 1 1 calc R . . C14 C 0.5084(2) 0.12017(16) -0.01429(16) 0.0269(9) Uani 1 1 d . . . C15 C 0.5544(2) 0.15826(16) 0.08367(16) 0.0279(9) Uani 1 1 d . . . H15 H 0.5831 0.1375 0.1163 0.033 Uiso 1 1 calc R . . C16 C 0.4767(2) 0.18298(17) 0.11295(16) 0.0344(10) Uani 1 1 d . . . H16A H 0.4468 0.2086 0.0851 0.041 Uiso 1 1 calc R . . H16B H 0.4414 0.1492 0.1247 0.041 Uiso 1 1 calc R . . C17 C 0.5010(3) 0.22033(19) 0.16724(17) 0.0427(11) Uani 1 1 d . . . H17A H 0.5264 0.1933 0.1963 0.051 Uiso 1 1 calc R . . H17B H 0.4520 0.2377 0.1852 0.051 Uiso 1 1 calc R . . C18 C 0.5603(3) 0.27205(19) 0.15208(19) 0.0471(12) Uani 1 1 d . . . H18A H 0.5770 0.2927 0.1884 0.057 Uiso 1 1 calc R . . H18B H 0.5327 0.3019 0.1270 0.057 Uiso 1 1 calc R . . C19 C 0.6360(3) 0.24759(18) 0.11999(19) 0.0427(11) Uani 1 1 d . . . H19A H 0.6702 0.2819 0.1078 0.051 Uiso 1 1 calc R . . H19B H 0.6677 0.2224 0.1472 0.051 Uiso 1 1 calc R . . C20 C 0.6135(3) 0.20964(17) 0.06550(17) 0.0345(10) Uani 1 1 d . . . H20A H 0.6627 0.1920 0.0482 0.041 Uiso 1 1 calc R . . H20B H 0.5877 0.2357 0.0359 0.041 Uiso 1 1 calc R . . C21 C 0.4513(2) 0.19574(17) -0.08812(17) 0.0318(10) Uani 1 1 d . . . H21 H 0.4281 0.1617 -0.1112 0.038 Uiso 1 1 calc R . . C22 C 0.5290(2) 0.21937(19) -0.11909(18) 0.0416(11) Uani 1 1 d . . . H22A H 0.5549 0.2505 -0.0944 0.050 Uiso 1 1 calc R . . H22B H 0.5676 0.1857 -0.1240 0.050 Uiso 1 1 calc R . . C23 C 0.5092(3) 0.2464(2) -0.17909(18) 0.0490(12) Uani 1 1 d . . . H23A H 0.4868 0.2147 -0.2048 0.059 Uiso 1 1 calc R . . H23B H 0.5591 0.2619 -0.1973 0.059 Uiso 1 1 calc R . . C24 C 0.4469(3) 0.2987(2) -0.1728(2) 0.0535(13) Uani 1 1 d . . . H24A H 0.4705 0.3316 -0.1491 0.064 Uiso 1 1 calc R . . H24B H 0.4337 0.3151 -0.2118 0.064 Uiso 1 1 calc R . . C25 C 0.3684(3) 0.2754(2) -0.14279(19) 0.0490(12) Uani 1 1 d . . . H25A H 0.3303 0.3093 -0.1377 0.059 Uiso 1 1 calc R . . H25B H 0.3425 0.2449 -0.1680 0.059 Uiso 1 1 calc R . . C26 C 0.3873(3) 0.24735(18) -0.08291(17) 0.0377(10) Uani 1 1 d . . . H26A H 0.3371 0.2309 -0.0658 0.045 Uiso 1 1 calc R . . H26B H 0.4078 0.2790 -0.0564 0.045 Uiso 1 1 calc R . . C27 C 0.9088(3) -0.06238(18) 0.21092(19) 0.0442(11) Uani 1 1 d . . . H27A H 0.8778 -0.1002 0.2060 0.053 Uiso 1 1 calc R . . H27B H 0.9004 -0.0473 0.2511 0.053 Uiso 1 1 calc R . . C28 C 0.9987(3) -0.0736(2) 0.19962(19) 0.0454(11) Uani 1 1 d . . . H28A H 1.0324 -0.0527 0.2289 0.054 Uiso 1 1 calc R . . H28B H 1.0112 -0.1172 0.2004 0.054 Uiso 1 1 calc R . . C29 C 1.0118(3) -0.0473(2) 0.1386(2) 0.0519(12) Uani 1 1 d . . . H29A H 0.9981 -0.0770 0.1079 0.062 Uiso 1 1 calc R . . H29B H 1.0682 -0.0339 0.1331 0.062 Uiso 1 1 calc R . . C30 C 0.9534(3) 0.00613(19) 0.1381(2) 0.0480(12) Uani 1 1 d . . . H30A H 0.9765 0.0410 0.1592 0.058 Uiso 1 1 calc R . . H30B H 0.9404 0.0185 0.0977 0.058 Uiso 1 1 calc R . . C31 C 0.6806(3) 0.0477(2) 0.27510(19) 0.0469(12) Uani 1 1 d . . . H31A H 0.6805 0.0327 0.3158 0.056 Uiso 1 1 calc R . . H31B H 0.6359 0.0283 0.2536 0.056 Uiso 1 1 calc R . . C32 C 0.6724(3) 0.1160(2) 0.2737(2) 0.0612(14) Uani 1 1 d . . . H32A H 0.6364 0.1306 0.3050 0.073 Uiso 1 1 calc R . . H32B H 0.6518 0.1301 0.2355 0.073 Uiso 1 1 calc R . . C33 C 0.7609(3) 0.1369(2) 0.2839(2) 0.0596(14) Uani 1 1 d . . . H33A H 0.7734 0.1730 0.2602 0.072 Uiso 1 1 calc R . . H33B H 0.7704 0.1463 0.3255 0.072 Uiso 1 1 calc R . . C34 C 0.8112(3) 0.0834(2) 0.2646(2) 0.0599(14) Uani 1 1 d . . . H34A H 0.8461 0.0950 0.2315 0.072 Uiso 1 1 calc R . . H34B H 0.8459 0.0697 0.2971 0.072 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 U 0.02606(9) 0.02604(8) 0.02352(8) 0.00202(6) 0.00000(7) 0.00078(6) Li 0.037(4) 0.041(4) 0.038(4) -0.002(3) -0.006(3) -0.001(3) Cl1 0.0366(6) 0.0327(5) 0.0402(6) 0.0076(5) -0.0088(5) 0.0000(5) Cl2 0.0294(5) 0.0320(5) 0.0318(5) 0.0012(4) -0.0031(5) -0.0021(4) Cl3 0.0352(6) 0.0404(6) 0.0257(5) -0.0012(4) 0.0044(5) -0.0026(5) N1 0.0248(17) 0.0241(16) 0.0250(16) 0.0052(14) 0.0026(15) 0.0031(14) N2 0.0259(18) 0.0249(16) 0.0289(18) 0.0004(15) 0.0033(15) 0.0055(14) N3 0.0254(18) 0.0269(17) 0.0261(17) 0.0025(14) -0.0019(15) 0.0013(14) N4 0.0198(17) 0.0358(18) 0.0279(18) 0.0057(15) 0.0054(15) 0.0012(14) N5 0.0258(18) 0.0266(17) 0.0234(17) 0.0027(14) 0.0026(16) -0.0025(14) N6 0.040(2) 0.0257(17) 0.0253(18) -0.0025(14) -0.0054(16) 0.0039(16) O1 0.0365(17) 0.0511(18) 0.0474(18) 0.0126(15) 0.0009(15) 0.0047(14) O2 0.0379(17) 0.0416(16) 0.0374(16) -0.0013(14) 0.0012(15) -0.0043(14) C1 0.026(2) 0.0249(19) 0.030(2) -0.0049(18) 0.0023(19) -0.0040(17) C2 0.031(2) 0.029(2) 0.025(2) 0.0002(17) 0.004(2) 0.0044(18) C3 0.028(2) 0.030(2) 0.036(2) -0.0008(18) -0.004(2) 0.0006(18) C4 0.040(3) 0.029(2) 0.041(2) 0.0015(19) -0.002(2) 0.003(2) C5 0.035(3) 0.038(2) 0.041(3) 0.001(2) 0.002(2) 0.006(2) C6 0.028(2) 0.040(2) 0.036(2) 0.0009(19) 0.0034(19) -0.0009(19) C7 0.028(2) 0.029(2) 0.040(2) 0.0018(19) 0.008(2) -0.0002(18) C8 0.027(2) 0.036(2) 0.033(2) -0.0005(19) 0.0019(19) -0.0031(19) C9 0.040(3) 0.044(2) 0.025(2) 0.0031(19) 0.005(2) -0.001(2) C10 0.044(3) 0.049(3) 0.041(3) 0.011(2) 0.008(2) -0.005(2) C11 0.048(3) 0.039(3) 0.051(3) 0.003(2) 0.003(2) -0.007(2) C12 0.049(3) 0.043(3) 0.047(3) 0.002(2) -0.005(2) -0.008(2) C13 0.037(3) 0.039(2) 0.031(2) 0.0013(19) -0.001(2) -0.0026(19) C14 0.019(2) 0.028(2) 0.033(2) 0.0074(18) 0.006(2) 0.0006(17) C15 0.031(2) 0.029(2) 0.023(2) 0.0019(17) -0.0008(18) 0.0060(18) C16 0.038(3) 0.035(2) 0.031(2) 0.0010(19) -0.002(2) 0.0066(19) C17 0.044(3) 0.049(3) 0.035(2) -0.011(2) -0.002(2) 0.017(2) C18 0.061(3) 0.037(2) 0.043(3) -0.009(2) -0.013(3) 0.008(2) C19 0.045(3) 0.029(2) 0.054(3) -0.003(2) -0.018(2) -0.005(2) C20 0.039(3) 0.027(2) 0.038(2) 0.0032(19) -0.004(2) -0.0023(18) C21 0.032(2) 0.026(2) 0.038(2) 0.0034(18) -0.002(2) 0.0064(18) C22 0.035(3) 0.046(3) 0.044(3) 0.007(2) 0.004(2) 0.006(2) C23 0.049(3) 0.053(3) 0.044(3) 0.013(2) 0.007(2) 0.011(2) C24 0.061(3) 0.050(3) 0.050(3) 0.017(2) 0.008(3) 0.018(3) C25 0.049(3) 0.052(3) 0.046(3) 0.016(2) -0.002(2) 0.016(2) C26 0.033(2) 0.042(2) 0.038(2) 0.008(2) 0.006(2) 0.006(2) C27 0.047(3) 0.037(2) 0.049(3) -0.001(2) 0.002(2) 0.003(2) C28 0.038(3) 0.048(3) 0.050(3) 0.001(2) 0.000(2) 0.005(2) C29 0.037(3) 0.057(3) 0.061(3) 0.004(3) 0.009(2) 0.001(2) C30 0.043(3) 0.046(3) 0.054(3) 0.003(2) 0.008(2) 0.002(2) C31 0.035(3) 0.069(3) 0.036(2) -0.002(2) 0.000(2) -0.004(2) C32 0.058(4) 0.077(4) 0.049(3) 0.000(3) -0.003(3) 0.026(3) C33 0.076(4) 0.046(3) 0.057(3) -0.008(2) 0.024(3) -0.008(3) C34 0.047(3) 0.047(3) 0.086(4) -0.019(3) -0.006(3) -0.002(2) _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 U N5 2.399(3) . ? U N2 2.402(3) 5_655 ? U N1 2.438(3) . ? U N1 2.449(3) 5_655 ? U N3 2.491(3) . ? U Cl3 2.6845(9) . ? U Cl2 2.8038(9) . ? U Cl1 2.8148(9) . ? U Li 3.711(7) . ? Li O1 1.916(8) . ? Li O2 1.933(7) . ? Li Cl2 2.309(7) . ? Li Cl1 2.334(6) . ? N1 C1 1.376(5) . ? N1 N2 1.449(4) . ? N1 U 2.449(3) 5_655 ? N2 C14 1.369(4) . ? N2 U 2.402(3) 5_655 ? N3 C1 1.312(4) . ? N3 C2 1.471(4) . ? N4 C1 1.379(4) . ? N4 C8 1.468(4) . ? N4 H4 0.9820 . ? N5 C14 1.344(4) . ? N5 C15 1.476(4) . ? N6 C14 1.353(4) . ? N6 C21 1.476(5) . ? N6 H6 0.8853 . ? O1 C30 1.432(5) . ? O1 C27 1.447(5) . ? O2 C31 1.413(5) . ? O2 C34 1.426(5) . ? C2 C7 1.519(5) . ? C2 C3 1.527(5) . ? C2 H2 0.9800 . ? C3 C4 1.527(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.518(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.516(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.527(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.530(5) . ? C8 C9 1.530(5) . ? C8 H8 0.9800 . ? C9 C10 1.510(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.514(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.534(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.516(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C15 C16 1.522(5) . ? C15 C20 1.530(5) . ? C15 H15 0.9800 . ? C16 C17 1.518(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.521(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.523(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.521(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.533(5) . ? C21 C26 1.536(5) . ? C21 H21 0.9800 . ? C22 C23 1.505(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.531(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.530(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.509(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.505(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.501(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.502(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.492(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.526(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.486(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? 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 N5 U N2 119.39(10) . 5_655 ? N5 U N1 64.20(10) . . ? N2 U N1 82.66(10) 5_655 . ? N5 U N1 84.64(10) . 5_655 ? N2 U N1 34.75(9) 5_655 5_655 ? N1 U N1 64.61(12) . 5_655 ? N5 U N3 101.07(10) . . ? N2 U N3 96.12(9) 5_655 . ? N1 U N3 53.17(10) . . ? N1 U N3 104.46(10) 5_655 . ? N5 U Cl3 85.02(7) . . ? N2 U Cl3 85.45(7) 5_655 . ? N1 U Cl3 134.98(7) . . ? N1 U Cl3 81.39(7) 5_655 . ? N3 U Cl3 171.83(7) . . ? N5 U Cl2 79.43(7) . . ? N2 U Cl2 160.69(7) 5_655 . ? N1 U Cl2 111.60(7) . . ? N1 U Cl2 163.38(7) 5_655 . ? N3 U Cl2 83.39(7) . . ? Cl3 U Cl2 92.47(3) . . ? N5 U Cl1 152.92(7) . . ? N2 U Cl1 84.58(7) 5_655 . ? N1 U Cl1 136.68(7) . . ? N1 U Cl1 118.30(7) 5_655 . ? N3 U Cl1 87.55(7) . . ? Cl3 U Cl1 84.61(3) . . ? Cl2 U Cl1 76.11(3) . . ? O1 Li O2 99.5(3) . . ? O1 Li Cl2 116.5(3) . . ? O2 Li Cl2 110.3(3) . . ? O1 Li Cl1 114.7(3) . . ? O2 Li Cl1 120.5(3) . . ? Cl2 Li Cl1 96.5(2) . . ? Li Cl1 U 91.73(16) . . ? Li Cl2 U 92.56(17) . . ? C1 N1 N2 118.4(3) . . ? C1 N1 U 94.5(2) . . ? N2 N1 U 120.8(2) . . ? C1 N1 U 138.9(2) . 5_655 ? N2 N1 U 70.87(17) . 5_655 ? U N1 U 115.39(11) . 5_655 ? C14 N2 N1 110.2(3) . . ? C14 N2 U 126.3(2) . 5_655 ? N1 N2 U 74.37(17) . 5_655 ? C1 N3 C2 122.4(3) . . ? C1 N3 U 93.9(2) . . ? C2 N3 U 142.8(2) . . ? C1 N4 C8 123.3(3) . . ? C1 N4 H4 93.6 . . ? C8 N4 H4 127.8 . . ? C14 N5 C15 122.0(3) . . ? C14 N5 U 121.1(2) . . ? C15 N5 U 116.9(2) . . ? C14 N6 C21 125.3(3) . . ? C14 N6 H6 116.7 . . ? C21 N6 H6 117.3 . . ? C30 O1 C27 108.0(3) . . ? C30 O1 Li 134.8(3) . . ? C27 O1 Li 117.0(3) . . ? C31 O2 C34 106.6(3) . . ? C31 O2 Li 124.0(3) . . ? C34 O2 Li 117.5(3) . . ? N3 C1 N1 110.4(3) . . ? N3 C1 N4 129.2(3) . . ? N1 C1 N4 120.4(3) . . ? N3 C2 C7 112.9(3) . . ? N3 C2 C3 108.2(3) . . ? C7 C2 C3 110.2(3) . . ? N3 C2 H2 108.5 . . ? C7 C2 H2 108.5 . . ? C3 C2 H2 108.5 . . ? C2 C3 C4 112.3(3) . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 111.4(3) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 110.6(3) . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C5 C6 C7 110.9(3) . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.0 . . ? C2 C7 C6 110.9(3) . . ? C2 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N4 C8 C13 111.4(3) . . ? N4 C8 C9 107.2(3) . . ? C13 C8 C9 111.7(3) . . ? N4 C8 H8 108.8 . . ? C13 C8 H8 108.8 . . ? C9 C8 H8 108.8 . . ? C10 C9 C8 112.8(3) . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? C8 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 C11 111.9(3) . . ? C9 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 110.0(3) . . ? C10 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? C10 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C13 C12 C11 109.9(3) . . ? C13 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? C13 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C12 C13 C8 112.6(3) . . ? C12 C13 H13A 109.1 . . ? C8 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? C8 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? N5 C14 N6 122.6(3) . . ? N5 C14 N2 121.0(3) . . ? N6 C14 N2 116.4(3) . . ? N5 C15 C16 117.0(3) . . ? N5 C15 C20 114.6(3) . . ? C16 C15 C20 112.3(3) . . ? N5 C15 H15 103.6 . . ? C16 C15 H15 103.6 . . ? C20 C15 H15 103.6 . . ? C17 C16 C15 108.7(3) . . ? C17 C16 H16A 110.0 . . ? C15 C16 H16A 110.0 . . ? C17 C16 H16B 110.0 . . ? C15 C16 H16B 110.0 . . ? H16A C16 H16B 108.3 . . ? C16 C17 C18 112.4(3) . . ? C16 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? C16 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? C17 C18 C19 111.1(3) . . ? C17 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C20 C19 C18 112.1(3) . . ? C20 C19 H19A 109.2 . . ? C18 C19 H19A 109.2 . . ? C20 C19 H19B 109.2 . . ? C18 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C19 C20 C15 109.5(3) . . ? C19 C20 H20A 109.8 . . ? C15 C20 H20A 109.8 . . ? C19 C20 H20B 109.8 . . ? C15 C20 H20B 109.8 . . ? H20A C20 H20B 108.2 . . ? N6 C21 C22 110.3(3) . . ? N6 C21 C26 108.1(3) . . ? C22 C21 C26 110.5(3) . . ? N6 C21 H21 109.3 . . ? C22 C21 H21 109.3 . . ? C26 C21 H21 109.3 . . ? C23 C22 C21 111.1(3) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 110.4(3) . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C25 C24 C23 110.3(4) . . ? C25 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? C25 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C26 C25 C24 110.9(4) . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C21 111.4(3) . . ? C25 C26 H26A 109.3 . . ? C21 C26 H26A 109.3 . . ? C25 C26 H26B 109.3 . . ? C21 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? O1 C27 C28 106.9(3) . . ? O1 C27 H27A 110.3 . . ? C28 C27 H27A 110.3 . . ? O1 C27 H27B 110.3 . . ? C28 C27 H27B 110.3 . . ? H27A C27 H27B 108.6 . . ? C29 C28 C27 103.3(4) . . ? C29 C28 H28A 111.1 . . ? C27 C28 H28A 111.1 . . ? C29 C28 H28B 111.1 . . ? C27 C28 H28B 111.1 . . ? H28A C28 H28B 109.1 . . ? C28 C29 C30 102.2(4) . . ? C28 C29 H29A 111.3 . . ? C30 C29 H29A 111.3 . . ? C28 C29 H29B 111.3 . . ? C30 C29 H29B 111.3 . . ? H29A C29 H29B 109.2 . . ? O1 C30 C29 103.8(3) . . ? O1 C30 H30A 111.0 . . ? C29 C30 H30A 111.0 . . ? O1 C30 H30B 111.0 . . ? C29 C30 H30B 111.0 . . ? H30A C30 H30B 109.0 . . ? O2 C31 C32 104.9(4) . . ? O2 C31 H31A 110.8 . . ? C32 C31 H31A 110.8 . . ? O2 C31 H31B 110.8 . . ? C32 C31 H31B 110.8 . . ? H31A C31 H31B 108.8 . . ? C31 C32 C33 102.1(4) . . ? C31 C32 H32A 111.3 . . ? C33 C32 H32A 111.3 . . ? C31 C32 H32B 111.3 . . ? C33 C32 H32B 111.3 . . ? H32A C32 H32B 109.2 . . ? C34 C33 C32 104.1(4) . . ? C34 C33 H33A 110.9 . . ? C32 C33 H33A 110.9 . . ? C34 C33 H33B 110.9 . . ? C32 C33 H33B 110.9 . . ? H33A C33 H33B 109.0 . . ? O2 C34 C33 108.1(4) . . ? O2 C34 H34A 110.1 . . ? C33 C34 H34A 110.1 . . ? O2 C34 H34B 110.1 . . ? C33 C34 H34B 110.1 . . ? H34A C34 H34B 108.4 . . ? 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 N4 H4 N2 0.98 2.18 2.807(4) 120.2 . N4 H4 Cl3 0.98 2.80 3.470(3) 125.9 5_655 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 643703' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C156 H276 Cl12 N36 U6' _chemical_formula_weight 4509.71 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' Cl Cl 0.1484 0.1585 '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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6490(18) _cell_length_b 15.660(2) _cell_length_c 25.593(4) _cell_angle_alpha 78.538(7) _cell_angle_beta 83.988(8) _cell_angle_gamma 65.304(8) _cell_volume 4869.4(12) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 120010 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light green' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2220 _exptl_absorpt_coefficient_mu 5.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.513 _exptl_absorpt_correction_T_max 0.813 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 mm' _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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and six \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 120010 _diffrn_reflns_av_R_equivalents 0.0947 _diffrn_reflns_av_sigmaI/netI 0.1806 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.68 _reflns_number_total 18129 _reflns_number_gt 8046 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints on bond lengths and/or displacement parameters for many atoms, particularly in the cyclohexane rings. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Large voids in the lattice likely indicate the presence of unresolved solvent molecules. 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^)+(0.0834P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18129 _refine_ls_number_parameters 946 _refine_ls_number_restraints 145 _refine_ls_R_factor_all 0.1619 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.1774 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 0.873 _refine_ls_restrained_S_all 0.876 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.715 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.154 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 0.52459(4) 0.18289(4) 0.35106(2) 0.07202(19) Uani 1 1 d . . . U2 U 0.64946(4) 0.25878(4) 0.21374(2) 0.06537(18) Uani 1 1 d . . . U3 U 0.50803(4) 0.49816(3) 0.079011(19) 0.05444(16) Uani 1 1 d . . . Cl1 Cl 0.4312(4) 0.1931(3) 0.44690(15) 0.1005(13) Uani 1 1 d . . . Cl2 Cl 0.8296(3) 0.2259(3) 0.25845(15) 0.0866(11) Uani 1 1 d . . . Cl3 Cl 0.7602(3) 0.1653(2) 0.13723(13) 0.0699(9) Uani 1 1 d . . . Cl4 Cl 0.6787(3) 0.4153(2) 0.15285(13) 0.0682(9) Uani 1 1 d . . . Cl5 Cl 0.4847(2) 0.3370(2) 0.14095(13) 0.0661(9) Uani 1 1 d . . . Cl6 Cl 0.4181(3) 0.5950(2) 0.15872(14) 0.0730(9) Uani 1 1 d . . . N1A N 0.6584(9) 0.1275(7) 0.2821(5) 0.073(3) Uani 1 1 d . . . N2A N 0.6020(8) 0.1217(7) 0.2395(4) 0.062(3) Uani 1 1 d . . . N3A N 0.7074(10) 0.0567(8) 0.3656(5) 0.090(4) Uani 1 1 d . . . N4A N 0.7822(10) -0.0345(9) 0.2974(5) 0.094(4) Uani 1 1 d . . . H4A H 0.7483 -0.0735 0.3089 0.113 Uiso 1 1 d R . . N5A N 0.5071(9) 0.0666(8) 0.3100(5) 0.081(3) Uani 1 1 d . . . N6A N 0.4775(13) 0.0641(9) 0.2216(5) 0.065(4) Uani 1 1 d D . . H6A H 0.4105 0.0781 0.2358 0.079 Uiso 1 1 d R . . C1A C 0.7207(13) 0.0476(12) 0.3128(7) 0.093(5) Uani 1 1 d . . . C2A C 0.7702(13) -0.0279(14) 0.4058(7) 0.116(6) Uani 1 1 d . . . H2A H 0.7704 -0.0865 0.3976 0.139 Uiso 1 1 calc R . . C3A C 0.7212(15) -0.0108(13) 0.4594(7) 0.126(6) Uani 1 1 d . . . H3A1 H 0.6474 -0.0050 0.4608 0.151 Uiso 1 1 calc R . . H3A2 H 0.7202 0.0482 0.4664 0.151 Uiso 1 1 calc R . . C4A C 0.7909(13) -0.0992(14) 0.5044(7) 0.133(7) Uani 1 1 d DU . . H4A1 H 0.7574 -0.0906 0.5394 0.160 Uiso 1 1 calc R . . H4A2 H 0.7949 -0.1589 0.4969 0.160 Uiso 1 1 calc R . . C5A C 0.9021(14) -0.1001(16) 0.5025(8) 0.112(7) Uani 1 1 d DU . . H5A1 H 0.9453 -0.1499 0.5302 0.134 Uiso 1 1 calc R . . H5A2 H 0.8968 -0.0394 0.5092 0.134 Uiso 1 1 calc R . . C6A C 0.9584(17) -0.1181(15) 0.4468(8) 0.116(7) Uani 1 1 d . . . H6A1 H 0.9635 -0.1784 0.4397 0.139 Uiso 1 1 calc R . . H6A2 H 1.0308 -0.1207 0.4463 0.139 Uiso 1 1 calc R . . C7A C 0.8871(14) -0.0317(13) 0.4023(7) 0.119(6) Uani 1 1 d . . . H7A1 H 0.8850 0.0282 0.4084 0.142 Uiso 1 1 calc R . . H7A2 H 0.9186 -0.0419 0.3671 0.142 Uiso 1 1 calc R . . C8A C 0.8179(13) -0.0478(12) 0.2419(6) 0.092(5) Uani 1 1 d . . . H8A H 0.7710 0.0071 0.2171 0.110 Uiso 1 1 calc R . . C9A C 0.9326(16) -0.0555(14) 0.2345(8) 0.127(6) Uani 1 1 d . . . H9A1 H 0.9769 -0.1050 0.2620 0.152 Uiso 1 1 calc R . . H9A2 H 0.9338 0.0043 0.2385 0.152 Uiso 1 1 calc R . . C10A C 0.9822(14) -0.0802(12) 0.1767(7) 0.120(6) Uani 1 1 d D . . H10A H 0.9455 -0.0261 0.1493 0.144 Uiso 1 1 calc R . . H10B H 1.0580 -0.0922 0.1747 0.144 Uiso 1 1 calc R . . C11A C 0.9695(14) -0.1664(11) 0.1667(7) 0.103(5) Uani 1 1 d DU . . H11A H 0.9937 -0.1758 0.1305 0.124 Uiso 1 1 calc R . . H11B H 1.0161 -0.2219 0.1906 0.124 Uiso 1 1 calc R . . C12A C 0.8599(14) -0.1604(13) 0.1742(7) 0.117(6) Uani 1 1 d . . . H12A H 0.8591 -0.2203 0.1701 0.141 Uiso 1 1 calc R . . H12B H 0.8143 -0.1105 0.1473 0.141 Uiso 1 1 calc R . . C13A C 0.8146(14) -0.1379(12) 0.2313(7) 0.106(5) Uani 1 1 d . . . H13A H 0.7406 -0.1319 0.2350 0.128 Uiso 1 1 calc R . . H13B H 0.8564 -0.1910 0.2579 0.128 Uiso 1 1 calc R . . C14A C 0.5291(15) 0.0831(12) 0.2562(6) 0.105(6) Uani 1 1 d . . . C15A C 0.4609(14) -0.0052(12) 0.3320(7) 0.106(5) Uani 1 1 d . . . H15A H 0.3954 0.0111 0.3127 0.127 Uiso 1 1 calc R . . C16A C 0.5412(17) -0.1079(13) 0.3259(8) 0.104(6) Uani 1 1 d . . . H16A H 0.5409 -0.1134 0.2888 0.124 Uiso 1 1 calc R . . H16B H 0.6126 -0.1137 0.3324 0.124 Uiso 1 1 calc R . . C17A C 0.529(3) -0.186(2) 0.3565(12) 0.130(11) Uani 1 1 d . . . H17A H 0.5943 -0.2432 0.3541 0.156 Uiso 1 1 calc R . . H17B H 0.4701 -0.1947 0.3430 0.156 Uiso 1 1 calc R . . C18A C 0.506(2) -0.173(2) 0.4119(12) 0.126(10) Uani 1 1 d U . . H18A H 0.4947 -0.2275 0.4326 0.151 Uiso 1 1 calc R . . H18B H 0.5679 -0.1708 0.4260 0.151 Uiso 1 1 calc R . . C19A C 0.413(2) -0.088(2) 0.4176(13) 0.127(11) Uani 1 1 d U . . H19A H 0.3970 -0.0849 0.4552 0.152 Uiso 1 1 calc R . . H19B H 0.3517 -0.0886 0.4022 0.152 Uiso 1 1 calc R . . C20A C 0.4318(16) -0.0055(13) 0.3915(8) 0.095(6) Uani 1 1 d U . . H20A H 0.4899 -0.0028 0.4091 0.114 Uiso 1 1 calc R . . H20B H 0.3674 0.0515 0.3956 0.114 Uiso 1 1 calc R . . C21A C 0.4635(16) 0.1043(14) 0.1639(6) 0.109(8) Uani 1 1 d DU . . H21A H 0.4575 0.1693 0.1623 0.131 Uiso 1 1 calc R . . C22A C 0.570(2) 0.0578(16) 0.1373(9) 0.121(12) Uani 1 1 d DU . . H22A H 0.6304 0.0507 0.1574 0.145 Uiso 1 1 calc R . . H22B H 0.5745 0.0884 0.1008 0.145 Uiso 1 1 calc R . . C23A C 0.5563(15) -0.0340(13) 0.1414(8) 0.137(7) Uani 1 1 d DU . . H23A H 0.6235 -0.0787 0.1280 0.164 Uiso 1 1 calc R . . H23B H 0.5524 -0.0576 0.1793 0.164 Uiso 1 1 calc R . . C24A C 0.4679(16) -0.045(2) 0.1167(14) 0.131(13) Uani 1 1 d DU . . H24A H 0.4781 -0.0374 0.0782 0.157 Uiso 1 1 calc R . . H24B H 0.4705 -0.1088 0.1296 0.157 Uiso 1 1 calc R . . C25A C 0.3610(17) 0.0275(15) 0.1310(10) 0.102(7) Uani 1 1 d DU . . H25A H 0.3347 0.0006 0.1639 0.122 Uiso 1 1 calc R . . H25B H 0.3108 0.0399 0.1034 0.122 Uiso 1 1 calc R . . C26A C 0.3594(17) 0.1209(15) 0.1378(9) 0.115(7) Uani 1 1 d . . . H26A H 0.2977 0.1526 0.1600 0.137 Uiso 1 1 calc R . . H26B H 0.3528 0.1618 0.1034 0.137 Uiso 1 1 calc R . . N1B N 0.4989(10) 0.3144(7) 0.2770(4) 0.069(3) Uani 1 1 d . . . N2B N 0.5628(9) 0.3693(7) 0.2737(5) 0.072(3) Uani 1 1 d . . . N3B N 0.3541(8) 0.2939(8) 0.3084(4) 0.067(3) Uani 1 1 d . . . N4B N 0.3439(9) 0.4529(8) 0.2679(4) 0.078(3) Uani 1 1 d . . . H4B H 0.3105 0.4620 0.2375 0.094 Uiso 1 1 d R . . N5B N 0.5893(9) 0.2942(9) 0.3621(5) 0.083(4) Uani 1 1 d . . . N6B N 0.6486(10) 0.4199(9) 0.3248(5) 0.091(4) Uani 1 1 d . . . H6B H 0.6117 0.4509 0.3514 0.109 Uiso 1 1 d R . . C1B C 0.3909(10) 0.3560(11) 0.2845(5) 0.061(4) Uani 1 1 d . . . C2B C 0.2353(11) 0.3159(10) 0.3070(6) 0.074(4) Uani 1 1 d . . . H2B H 0.1996 0.3771 0.2835 0.089 Uiso 1 1 calc R . . C3B C 0.2233(11) 0.2389(10) 0.2847(6) 0.085(4) Uani 1 1 d . . . H3B1 H 0.2609 0.1777 0.3069 0.102 Uiso 1 1 calc R . . H3B2 H 0.2561 0.2363 0.2492 0.102 Uiso 1 1 calc R . . C4B C 0.1045(12) 0.2575(11) 0.2819(7) 0.096(5) Uani 1 1 d . . . H4B1 H 0.0671 0.3176 0.2586 0.116 Uiso 1 1 calc R . . H4B2 H 0.0987 0.2071 0.2675 0.116 Uiso 1 1 calc R . . C5B C 0.0537(14) 0.2611(13) 0.3372(7) 0.115(6) Uani 1 1 d D . . H5B1 H -0.0226 0.2768 0.3353 0.138 Uiso 1 1 calc R . . H5B2 H 0.0866 0.1989 0.3594 0.138 Uiso 1 1 calc R . . C6B C 0.0682(13) 0.3342(12) 0.3619(7) 0.115(6) Uani 1 1 d D . . H6B1 H 0.0264 0.3971 0.3423 0.138 Uiso 1 1 calc R . . H6B2 H 0.0391 0.3315 0.3982 0.138 Uiso 1 1 calc R . . C7B C 0.1818(11) 0.3225(11) 0.3632(6) 0.089(5) Uani 1 1 d . . . H7B1 H 0.2218 0.2651 0.3878 0.107 Uiso 1 1 calc R . . H7B2 H 0.1835 0.3764 0.3757 0.107 Uiso 1 1 calc R . . C8B C 0.2645(12) 0.5135(10) 0.3025(6) 0.080(4) Uani 1 1 d . . . H8B H 0.2004 0.4992 0.3069 0.096 Uiso 1 1 calc R . . C9B C 0.3114(12) 0.4972(11) 0.3571(6) 0.095(5) Uani 1 1 d . . . H9B1 H 0.3305 0.4317 0.3746 0.114 Uiso 1 1 calc R . . H9B2 H 0.3759 0.5098 0.3531 0.114 Uiso 1 1 calc R . . C10B C 0.2262(15) 0.5646(13) 0.3895(7) 0.126(6) Uani 1 1 d U . . H10C H 0.1638 0.5489 0.3944 0.151 Uiso 1 1 calc R . . H10D H 0.2540 0.5557 0.4245 0.151 Uiso 1 1 calc R . . C11B C 0.1915(16) 0.6676(13) 0.3638(7) 0.094(6) Uani 1 1 d U . . H11C H 0.1357 0.7073 0.3860 0.113 Uiso 1 1 calc R . . H11D H 0.2524 0.6850 0.3617 0.113 Uiso 1 1 calc R . . C12B C 0.1501(14) 0.6864(12) 0.3100(7) 0.118(6) Uani 1 1 d U . . H12C H 0.1354 0.7518 0.2936 0.142 Uiso 1 1 calc R . . H12D H 0.0830 0.6783 0.3125 0.142 Uiso 1 1 calc R . . C13B C 0.2336(12) 0.6173(11) 0.2747(6) 0.097(5) Uani 1 1 d . . . H13C H 0.2028 0.6270 0.2404 0.116 Uiso 1 1 calc R . . H13D H 0.2975 0.6306 0.2686 0.116 Uiso 1 1 calc R . . C14B C 0.6017(12) 0.3605(11) 0.3210(6) 0.078(4) Uani 1 1 d . . . C15B C 0.6393(13) 0.2825(13) 0.4142(7) 0.109(6) Uani 1 1 d . . . H15B H 0.6248 0.2304 0.4366 0.130 Uiso 1 1 calc R . . C16B C 0.7631(15) 0.2414(13) 0.4102(7) 0.126(6) Uani 1 1 d . . . H16C H 0.7859 0.2875 0.3874 0.152 Uiso 1 1 calc R . . H16D H 0.7898 0.1842 0.3943 0.152 Uiso 1 1 calc R . . C17B C 0.8125(18) 0.2162(15) 0.4682(9) 0.129(8) Uani 1 1 d DU . . H17C H 0.8143 0.1550 0.4864 0.155 Uiso 1 1 calc R . . H17D H 0.8857 0.2123 0.4650 0.155 Uiso 1 1 calc R . . C18B C 0.7428(15) 0.2934(16) 0.4993(9) 0.107(8) Uani 1 1 d DU . . H18C H 0.7617 0.2661 0.5362 0.128 Uiso 1 1 calc R . . H18D H 0.7702 0.3426 0.4895 0.128 Uiso 1 1 calc R . . C19B C 0.6219(15) 0.3465(17) 0.5005(8) 0.116(8) Uani 1 1 d DU . . H19C H 0.6020 0.4064 0.5129 0.139 Uiso 1 1 calc R . . H19D H 0.5896 0.3088 0.5247 0.139 Uiso 1 1 calc R . . C20B C 0.5814(16) 0.3654(14) 0.4444(7) 0.132(7) Uani 1 1 d DU . . H20C H 0.5902 0.4213 0.4243 0.158 Uiso 1 1 calc R . . H20D H 0.5050 0.3796 0.4466 0.158 Uiso 1 1 calc R . . C21B C 0.6614(13) 0.4945(11) 0.2818(6) 0.083(4) Uani 1 1 d . . . H21B H 0.6501 0.4822 0.2473 0.099 Uiso 1 1 calc R . . C22B C 0.7763(13) 0.4872(12) 0.2825(7) 0.109(6) Uani 1 1 d . . . H22C H 0.7909 0.4918 0.3179 0.130 Uiso 1 1 calc R . . H22D H 0.8267 0.4255 0.2747 0.130 Uiso 1 1 calc R . . C23B C 0.7930(13) 0.5621(13) 0.2438(7) 0.113(6) Uani 1 1 d . . . H23C H 0.7877 0.5530 0.2079 0.136 Uiso 1 1 calc R . . H23D H 0.8646 0.5588 0.2474 0.136 Uiso 1 1 calc R . . C24B C 0.7111(16) 0.6568(12) 0.2525(7) 0.076(5) Uani 1 1 d . . . H24C H 0.7212 0.7059 0.2257 0.091 Uiso 1 1 calc R . . H24D H 0.7208 0.6678 0.2872 0.091 Uiso 1 1 calc R . . C25B C 0.5963(14) 0.6640(12) 0.2496(7) 0.108(5) Uani 1 1 d . . . H25C H 0.5445 0.7262 0.2560 0.129 Uiso 1 1 calc R . . H25D H 0.5847 0.6565 0.2143 0.129 Uiso 1 1 calc R . . C26B C 0.5813(12) 0.5907(11) 0.2890(7) 0.096(5) Uani 1 1 d . . . H26C H 0.5092 0.5943 0.2864 0.115 Uiso 1 1 calc R . . H26D H 0.5879 0.6013 0.3243 0.115 Uiso 1 1 calc R . . N1C N 0.4518(7) 0.5973(7) -0.0075(4) 0.057(3) Uani 1 1 d . . . N2C N 0.3520(7) 0.6076(6) -0.0290(4) 0.049(2) Uani 1 1 d . . . N3C N 0.5372(7) 0.6417(6) 0.0401(4) 0.053(3) Uani 1 1 d . . . N4C N 0.3941(8) 0.7622(7) -0.0154(4) 0.062(3) Uani 1 1 d . . . H4C H 0.3337 0.7580 -0.0234 0.074 Uiso 1 1 d R . . N5C N 0.3233(7) 0.5424(6) 0.0592(4) 0.056(3) Uani 1 1 d . . . N6C N 0.1905(7) 0.5917(7) -0.0068(4) 0.060(3) Uani 1 1 d . . . H6C H 0.1994 0.5349 -0.0141 0.072 Uiso 1 1 d R . . C1C C 0.4617(10) 0.6713(9) 0.0069(5) 0.055(3) Uani 1 1 d . . . C2C C 0.5921(10) 0.6985(8) 0.0510(5) 0.056(3) Uani 1 1 d . . . H2C H 0.5393 0.7522 0.0669 0.067 Uiso 1 1 calc R . . C3C C 0.6792(15) 0.6429(12) 0.0887(7) 0.085(5) Uani 1 1 d . . . H3C1 H 0.7308 0.5888 0.0735 0.102 Uiso 1 1 calc R . . H3C2 H 0.6490 0.6181 0.1211 0.102 Uiso 1 1 calc R . . C4C C 0.7404(14) 0.6981(12) 0.1039(7) 0.072(5) Uani 1 1 d . . . H4C1 H 0.6914 0.7497 0.1218 0.086 Uiso 1 1 calc R . . H4C2 H 0.7979 0.6557 0.1280 0.086 Uiso 1 1 calc R . . C5C C 0.7842(12) 0.7356(13) 0.0565(8) 0.113(6) Uani 1 1 d . . . H5C1 H 0.8397 0.6833 0.0414 0.135 Uiso 1 1 calc R . . H5C2 H 0.8175 0.7747 0.0653 0.135 Uiso 1 1 calc R . . C6C C 0.6991(17) 0.7943(15) 0.0161(8) 0.106(7) Uani 1 1 d . . . H6C1 H 0.6465 0.8493 0.0302 0.128 Uiso 1 1 calc R . . H6C2 H 0.7320 0.8173 -0.0159 0.128 Uiso 1 1 calc R . . C7C C 0.6442(15) 0.7384(13) 0.0024(6) 0.082(6) Uani 1 1 d . . . H7C1 H 0.6962 0.6861 -0.0140 0.099 Uiso 1 1 calc R . . H7C2 H 0.5892 0.7787 -0.0234 0.099 Uiso 1 1 calc R . . C8C C 0.3597(14) 0.8446(10) 0.0126(6) 0.098(5) Uani 1 1 d . . . H8C H 0.4223 0.8604 0.0117 0.117 Uiso 1 1 calc R . . C9C C 0.2730(11) 0.9302(10) -0.0200(6) 0.099(5) Uani 1 1 d D . . H9C1 H 0.2673 0.9881 -0.0093 0.119 Uiso 1 1 calc R . . H9C2 H 0.2948 0.9331 -0.0574 0.119 Uiso 1 1 calc R . . C10C C 0.1637(12) 0.9259(14) -0.0134(8) 0.124(7) Uani 1 1 d D . . H10E H 0.1652 0.8753 -0.0305 0.149 Uiso 1 1 calc R . . H10F H 0.1099 0.9857 -0.0307 0.149 Uiso 1 1 calc R . . C11C C 0.1326(13) 0.9077(12) 0.0454(7) 0.108(5) Uani 1 1 d U . . H11E H 0.0653 0.8997 0.0491 0.129 Uiso 1 1 calc R . . H11F H 0.1231 0.9613 0.0620 0.129 Uiso 1 1 calc R . . C12C C 0.2263(15) 0.8138(14) 0.0732(8) 0.129(6) Uani 1 1 d U . . H12E H 0.2054 0.7970 0.1099 0.155 Uiso 1 1 calc R . . H12F H 0.2387 0.7614 0.0549 0.155 Uiso 1 1 calc R . . C13C C 0.3247(14) 0.8289(13) 0.0719(8) 0.116(6) Uani 1 1 d . . . H13E H 0.3806 0.7737 0.0917 0.139 Uiso 1 1 calc R . . H13F H 0.3117 0.8843 0.0876 0.139 Uiso 1 1 calc R . . C14C C 0.2902(10) 0.5769(8) 0.0092(6) 0.057(3) Uani 1 1 d . . . C15C C 0.2542(10) 0.5171(9) 0.1013(5) 0.065(4) Uani 1 1 d . . . H15C H 0.2974 0.4943 0.1335 0.079 Uiso 1 1 calc R . . C16C C 0.1518(10) 0.5990(9) 0.1155(5) 0.065(4) Uani 1 1 d . . . H16E H 0.1696 0.6502 0.1212 0.079 Uiso 1 1 calc R . . H16F H 0.1031 0.6234 0.0859 0.079 Uiso 1 1 calc R . . C17C C 0.0958(11) 0.5680(10) 0.1651(6) 0.083(4) Uani 1 1 d . . . H17E H 0.0278 0.6203 0.1713 0.099 Uiso 1 1 calc R . . H17F H 0.1405 0.5512 0.1958 0.099 Uiso 1 1 calc R . . C18C C 0.0745(11) 0.4799(11) 0.1582(6) 0.094(5) Uani 1 1 d . . . H18E H 0.0423 0.4582 0.1908 0.113 Uiso 1 1 calc R . . H18F H 0.0242 0.4986 0.1297 0.113 Uiso 1 1 calc R . . C19C C 0.1760(10) 0.4015(9) 0.1456(6) 0.072(4) Uani 1 1 d . . . H19E H 0.1612 0.3476 0.1417 0.086 Uiso 1 1 calc R . . H19F H 0.2251 0.3811 0.1748 0.086 Uiso 1 1 calc R . . C20C C 0.2280(9) 0.4319(8) 0.0953(5) 0.058(3) Uani 1 1 d . . . H20E H 0.1799 0.4508 0.0658 0.070 Uiso 1 1 calc R . . H20F H 0.2940 0.3790 0.0875 0.070 Uiso 1 1 calc R . . C21C C 0.1309(9) 0.6624(9) -0.0522(5) 0.065(4) Uani 1 1 d . . . H21C H 0.1804 0.6856 -0.0746 0.078 Uiso 1 1 calc R . . C22C C 0.0399(11) 0.7490(10) -0.0276(7) 0.102(5) Uani 1 1 d . . . H22E H -0.0089 0.7270 -0.0044 0.122 Uiso 1 1 calc R . . H22F H 0.0725 0.7752 -0.0068 0.122 Uiso 1 1 calc R . . C23C C -0.0206(14) 0.8236(12) -0.0730(7) 0.110(5) Uani 1 1 d U . . H23E H -0.0774 0.8763 -0.0587 0.132 Uiso 1 1 calc R . . H23F H 0.0283 0.8480 -0.0942 0.132 Uiso 1 1 calc R . . C24C C -0.0671(16) 0.7887(14) -0.1064(8) 0.126(6) Uani 1 1 d U . . H24E H -0.1051 0.8397 -0.1349 0.151 Uiso 1 1 calc R . . H24F H -0.1188 0.7670 -0.0859 0.151 Uiso 1 1 calc R . . C25C C 0.0205(12) 0.7063(12) -0.1301(6) 0.097(5) Uani 1 1 d . . . H25E H 0.0700 0.7288 -0.1522 0.117 Uiso 1 1 calc R . . H25F H -0.0122 0.6827 -0.1525 0.117 Uiso 1 1 calc R . . C26C C 0.0847(12) 0.6226(12) -0.0844(6) 0.095(5) Uani 1 1 d . . . H26E H 0.0365 0.5978 -0.0628 0.114 Uiso 1 1 calc R . . H26F H 0.1412 0.5710 -0.0997 0.114 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 0.0768(4) 0.0718(4) 0.0586(4) -0.0095(3) 0.0001(3) -0.0229(3) U2 0.0609(3) 0.0673(4) 0.0619(4) -0.0103(3) -0.0029(3) -0.0203(3) U3 0.0481(3) 0.0583(3) 0.0581(3) -0.0148(2) 0.0012(2) -0.0213(2) Cl1 0.123(3) 0.118(3) 0.058(2) -0.023(2) 0.015(2) -0.046(3) Cl2 0.070(2) 0.096(3) 0.087(3) -0.017(2) -0.015(2) -0.024(2) Cl3 0.063(2) 0.072(2) 0.068(2) -0.0143(18) 0.0072(17) -0.0217(18) Cl4 0.060(2) 0.077(2) 0.069(2) -0.0082(18) -0.0078(17) -0.0296(18) Cl5 0.060(2) 0.065(2) 0.071(2) -0.0053(17) -0.0077(17) -0.0240(18) Cl6 0.069(2) 0.080(2) 0.074(2) -0.0288(19) 0.0063(18) -0.0292(19) N1A 0.081(8) 0.043(7) 0.070(8) 0.000(6) -0.009(7) -0.005(6) N2A 0.059(7) 0.073(7) 0.054(7) -0.007(6) 0.002(6) -0.028(6) N3A 0.096(9) 0.077(9) 0.075(9) 0.002(7) -0.015(8) -0.016(7) N4A 0.110(10) 0.086(10) 0.078(10) -0.012(8) 0.013(8) -0.036(9) N5A 0.083(8) 0.070(8) 0.091(10) -0.031(7) 0.012(7) -0.027(7) N6A 0.110(13) 0.070(10) 0.034(9) 0.000(7) -0.024(9) -0.053(10) C1A 0.093(12) 0.076(12) 0.089(14) -0.038(11) 0.010(10) -0.007(10) C2A 0.089(12) 0.148(17) 0.080(13) -0.021(12) -0.013(10) -0.014(12) C3A 0.119(10) 0.124(10) 0.110(10) -0.022(8) 0.001(8) -0.026(8) C4A 0.127(10) 0.142(10) 0.106(10) 0.008(8) -0.008(8) -0.043(8) C5A 0.102(10) 0.125(10) 0.082(10) -0.013(8) -0.005(8) -0.021(8) C6A 0.103(10) 0.125(11) 0.103(10) -0.011(8) -0.006(8) -0.034(8) C7A 0.116(9) 0.121(9) 0.107(9) -0.015(7) -0.012(8) -0.037(8) C8A 0.092(12) 0.092(12) 0.071(12) -0.001(9) 0.002(9) -0.025(10) C9A 0.133(10) 0.125(10) 0.127(10) -0.031(8) 0.003(8) -0.054(8) C10A 0.112(14) 0.128(16) 0.108(15) -0.047(12) 0.037(11) -0.036(12) C11A 0.104(9) 0.091(8) 0.104(9) -0.027(7) 0.017(7) -0.030(7) C12A 0.120(15) 0.148(16) 0.108(15) -0.072(12) 0.023(12) -0.063(13) C13A 0.110(13) 0.110(14) 0.101(14) -0.032(11) 0.015(11) -0.045(11) C14A 0.119(15) 0.105(13) 0.045(11) 0.014(9) 0.018(10) -0.017(11) C15A 0.122(14) 0.101(13) 0.089(13) -0.008(10) 0.018(10) -0.048(12) C16A 0.124(10) 0.082(9) 0.103(10) -0.031(8) 0.035(8) -0.041(8) C17A 0.142(14) 0.123(13) 0.121(14) -0.021(9) 0.017(9) -0.054(10) C18A 0.133(13) 0.121(13) 0.107(13) -0.012(9) 0.007(9) -0.041(9) C19A 0.130(13) 0.128(13) 0.121(14) -0.017(9) 0.018(9) -0.058(10) C20A 0.111(10) 0.089(9) 0.095(10) -0.029(8) 0.020(8) -0.048(8) C21A 0.126(11) 0.110(11) 0.141(12) -0.036(8) -0.005(8) -0.088(9) C22A 0.126(15) 0.111(14) 0.131(15) -0.028(9) -0.006(9) -0.051(10) C23A 0.135(10) 0.137(10) 0.145(11) -0.016(8) -0.009(8) -0.064(8) C24A 0.129(16) 0.129(15) 0.149(16) -0.042(10) -0.010(9) -0.057(10) C25A 0.098(10) 0.106(11) 0.109(11) -0.018(8) -0.028(8) -0.044(8) C26A 0.109(10) 0.103(10) 0.115(11) -0.017(8) -0.006(8) -0.027(8) N1B 0.090(9) 0.054(7) 0.064(8) -0.006(5) -0.022(6) -0.027(7) N2B 0.068(7) 0.070(8) 0.081(9) -0.019(6) -0.003(6) -0.028(7) N3B 0.063(8) 0.083(8) 0.053(7) -0.014(6) 0.013(6) -0.029(7) N4B 0.069(8) 0.077(9) 0.061(8) -0.036(7) -0.006(6) 0.008(7) N5B 0.091(9) 0.090(9) 0.046(7) -0.003(7) -0.025(7) -0.014(7) N6B 0.104(10) 0.081(9) 0.085(10) -0.023(8) -0.021(8) -0.026(8) C1B 0.037(8) 0.082(11) 0.052(9) -0.017(8) 0.003(6) -0.011(8) C2B 0.084(11) 0.079(10) 0.069(10) -0.010(8) 0.004(8) -0.045(9) C3B 0.085(11) 0.090(11) 0.065(10) 0.011(8) -0.001(8) -0.032(9) C4B 0.088(8) 0.108(9) 0.107(9) -0.002(7) -0.017(7) -0.056(7) C5B 0.095(13) 0.144(16) 0.111(15) 0.006(12) -0.005(11) -0.065(12) C6B 0.090(9) 0.128(10) 0.109(9) -0.006(8) 0.010(7) -0.036(7) C7B 0.072(10) 0.105(12) 0.075(11) 0.002(9) 0.019(8) -0.034(9) C8B 0.081(10) 0.077(11) 0.078(11) -0.014(9) -0.007(9) -0.028(9) C9B 0.089(11) 0.087(11) 0.083(12) -0.027(9) -0.005(9) -0.004(9) C10B 0.126(10) 0.142(10) 0.099(9) -0.035(8) -0.018(8) -0.033(8) C11B 0.109(10) 0.085(9) 0.084(9) -0.042(7) -0.008(8) -0.022(7) C12B 0.115(9) 0.107(9) 0.113(9) -0.029(7) -0.008(8) -0.020(7) C13B 0.090(11) 0.094(12) 0.098(13) -0.047(10) 0.017(9) -0.020(10) C14B 0.087(11) 0.073(11) 0.068(12) -0.028(9) -0.022(9) -0.015(9) C15B 0.096(13) 0.124(15) 0.088(13) 0.001(11) 0.011(10) -0.038(12) C16B 0.129(10) 0.130(10) 0.123(10) -0.006(8) -0.031(8) -0.056(8) C17B 0.131(11) 0.132(11) 0.129(12) -0.003(8) -0.030(8) -0.062(9) C18B 0.125(11) 0.108(11) 0.081(10) -0.017(8) -0.022(8) -0.037(8) C19B 0.133(12) 0.117(11) 0.105(12) -0.021(8) -0.003(9) -0.058(9) C20B 0.142(10) 0.140(10) 0.113(10) -0.036(8) 0.003(8) -0.051(8) C21B 0.092(12) 0.085(12) 0.075(11) -0.012(9) -0.009(9) -0.040(10) C22B 0.088(13) 0.087(12) 0.128(16) -0.027(11) 0.016(11) -0.014(10) C23B 0.089(12) 0.125(16) 0.115(15) -0.020(13) 0.036(11) -0.042(12) C24B 0.112(16) 0.060(12) 0.080(13) -0.026(9) 0.017(11) -0.056(12) C25B 0.107(14) 0.101(14) 0.106(14) -0.048(11) 0.020(11) -0.025(11) C26B 0.070(11) 0.078(12) 0.126(15) -0.007(11) -0.011(10) -0.019(10) N1C 0.053(6) 0.049(6) 0.072(7) -0.004(5) -0.017(5) -0.023(5) N2C 0.043(6) 0.048(6) 0.053(6) -0.012(5) 0.001(5) -0.013(5) N3C 0.046(6) 0.041(6) 0.066(7) -0.017(5) -0.014(5) -0.006(5) N4C 0.050(6) 0.053(7) 0.086(8) -0.024(6) 0.014(6) -0.022(6) N5C 0.046(6) 0.048(6) 0.067(8) -0.016(5) 0.008(6) -0.013(5) N6C 0.041(6) 0.066(7) 0.068(7) -0.025(6) 0.000(5) -0.013(5) C1C 0.046(8) 0.053(9) 0.065(9) -0.017(7) 0.006(7) -0.018(7) C2C 0.059(6) 0.045(6) 0.060(7) -0.013(5) 0.010(6) -0.019(5) C3C 0.116(15) 0.083(13) 0.070(13) -0.022(10) -0.010(11) -0.050(12) C4C 0.084(8) 0.076(8) 0.080(9) -0.019(7) -0.006(7) -0.053(7) C5C 0.057(10) 0.135(15) 0.155(18) -0.033(13) 0.000(11) -0.045(11) C6C 0.110(10) 0.108(10) 0.104(10) -0.011(8) 0.014(8) -0.053(8) C7C 0.107(14) 0.126(16) 0.066(12) -0.018(11) 0.000(10) -0.097(14) C8C 0.126(14) 0.058(10) 0.076(12) -0.021(9) 0.011(10) -0.004(10) C9C 0.118(14) 0.057(10) 0.099(13) -0.013(9) -0.003(10) -0.014(10) C10C 0.075(12) 0.149(17) 0.154(19) -0.009(13) -0.010(11) -0.056(12) C11C 0.092(8) 0.119(9) 0.095(9) -0.016(7) 0.013(7) -0.032(7) C12C 0.120(10) 0.136(10) 0.133(10) -0.019(8) -0.009(8) -0.054(8) C13C 0.108(14) 0.123(15) 0.134(18) -0.041(12) 0.012(12) -0.059(12) C14C 0.048(8) 0.051(8) 0.066(10) -0.013(7) 0.002(7) -0.014(7) C15C 0.062(9) 0.081(10) 0.047(8) -0.015(7) 0.016(7) -0.024(8) C16C 0.059(8) 0.073(9) 0.081(10) -0.029(8) 0.014(7) -0.040(8) C17C 0.064(9) 0.081(10) 0.090(12) -0.035(9) 0.014(8) -0.011(8) C18C 0.075(11) 0.126(14) 0.102(13) -0.014(10) 0.021(9) -0.068(11) C19C 0.042(8) 0.064(9) 0.110(12) -0.039(8) 0.003(8) -0.013(7) C20C 0.041(7) 0.057(8) 0.068(9) -0.015(7) 0.004(6) -0.011(6) C21C 0.035(7) 0.077(9) 0.068(9) 0.004(8) -0.004(7) -0.015(7) C22C 0.052(9) 0.081(11) 0.153(17) -0.005(11) 0.000(10) -0.016(9) C23C 0.101(9) 0.103(9) 0.116(9) -0.022(7) 0.006(7) -0.032(7) C24C 0.112(9) 0.126(10) 0.127(10) 0.005(8) -0.014(8) -0.045(8) C25C 0.092(12) 0.143(15) 0.077(11) -0.001(11) -0.002(9) -0.075(12) C26C 0.093(11) 0.144(14) 0.073(11) 0.019(10) -0.027(9) -0.084(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N5B 2.331(13) . ? U1 N5A 2.379(11) . ? U1 N1A 2.411(11) . ? U1 N1B 2.437(10) . ? U1 N3B 2.455(10) . ? U1 N3A 2.460(12) . ? U1 Cl1 2.645(4) . ? U1 C1A 2.855(16) . ? U1 C1B 2.874(14) . ? U1 U2 3.9304(9) . ? U2 N1A 2.389(10) . ? U2 N2B 2.391(11) . ? U2 N1B 2.444(12) . ? U2 N2A 2.444(11) . ? U2 Cl2 2.631(4) . ? U2 Cl3 2.633(3) . ? U2 Cl5 2.774(3) . ? U2 Cl4 2.786(3) . ? U2 U3 4.4585(9) . ? U3 N2C 2.392(9) 2_665 ? U3 N5C 2.401(9) . ? U3 N1C 2.428(9) . ? U3 N3C 2.446(9) . ? U3 N1C 2.465(10) 2_665 ? U3 Cl6 2.668(3) . ? U3 Cl5 2.821(3) . ? U3 C1C 2.825(13) . ? U3 Cl4 2.846(3) . ? U3 U3 4.0609(11) 2_665 ? N1A C1A 1.329(18) . ? N1A N2A 1.435(14) . ? N2A C14A 1.36(2) . ? N3A C1A 1.374(18) . ? N3A C2A 1.496(19) . ? N4A C1A 1.319(17) . ? N4A C8A 1.479(18) . ? N5A C14A 1.374(17) . ? N5A C15A 1.499(18) . ? N6A C14A 1.33(2) . ? N6A C21A 1.486(10) . ? C2A C3A 1.49(2) . ? C2A C7A 1.56(2) . ? C3A C4A 1.63(2) . ? C4A C5A 1.51(3) . ? C5A C6A 1.57(3) . ? C6A C7A 1.61(2) . ? C8A C13A 1.51(2) . ? C8A C9A 1.51(2) . ? C9A C10A 1.61(2) . ? C10A C11A 1.50(3) . ? C11A C12A 1.454(19) . ? C12A C13A 1.57(2) . ? C15A C20A 1.53(2) . ? C15A C16A 1.55(2) . ? C16A C17A 1.38(3) . ? C17A C18A 1.46(3) . ? C18A C19A 1.43(3) . ? C19A C20A 1.44(3) . ? C21A C22A 1.49(3) . ? C21A C26A 1.53(2) . ? C22A C23A 1.51(3) . ? C23A C24A 1.50(4) . ? C24A C25A 1.49(4) . ? C25A C26A 1.50(3) . ? N1B C1B 1.349(15) . ? N1B N2B 1.446(14) . ? N2B C14B 1.332(16) . ? N3B C1B 1.295(15) . ? N3B C2B 1.514(16) . ? N4B C1B 1.372(16) . ? N4B C8B 1.461(16) . ? N5B C14B 1.374(18) . ? N5B C15B 1.505(19) . ? N6B C14B 1.354(17) . ? N6B C21B 1.490(17) . ? C2B C3B 1.505(18) . ? C2B C7B 1.545(18) . ? C3B C4B 1.529(18) . ? C4B C5B 1.51(2) . ? C5B C6B 1.50(3) . ? C6B C7B 1.486(19) . ? C8B C9B 1.528(18) . ? C8B C13B 1.535(18) . ? C9B C10B 1.51(2) . ? C10B C11B 1.50(2) . ? C11B C12B 1.47(2) . ? C12B C13B 1.56(2) . ? C15B C20B 1.52(2) . ? C15B C16B 1.54(2) . ? C16B C17B 1.60(2) . ? C17B C18B 1.50(3) . ? C18B C19B 1.51(3) . ? C19B C20B 1.52(3) . ? C21B C26B 1.480(18) . ? C21B C22B 1.527(19) . ? C22B C23B 1.458(19) . ? C23B C24B 1.48(2) . ? C24B C25B 1.53(2) . ? C25B C26B 1.439(19) . ? N1C C1C 1.346(14) . ? N1C N2C 1.456(12) . ? N1C U3 2.465(10) 2_665 ? N2C C14C 1.369(14) . ? N2C U3 2.392(9) 2_665 ? N3C C1C 1.274(14) . ? N3C C2C 1.460(14) . ? N4C C1C 1.377(14) . ? N4C C8C 1.480(16) . ? N5C C14C 1.332(14) . ? N5C C15C 1.463(14) . ? N6C C14C 1.375(14) . ? N6C C21C 1.473(14) . ? C2C C3C 1.465(19) . ? C2C C7C 1.522(18) . ? C3C C4C 1.55(2) . ? C4C C5C 1.43(2) . ? C5C C6C 1.50(2) . ? C6C C7C 1.47(2) . ? C8C C9C 1.527(19) . ? C8C C13C 1.55(2) . ? C9C C10C 1.51(3) . ? C10C C11C 1.53(2) . ? C11C C12C 1.58(2) . ? C12C C13C 1.45(2) . ? C15C C16C 1.519(16) . ? C15C C20C 1.557(16) . ? C16C C17C 1.515(17) . ? C17C C18C 1.570(18) . ? C18C C19C 1.473(17) . ? C19C C20C 1.497(16) . ? C21C C26C 1.452(17) . ? C21C C22C 1.596(18) . ? C22C C23C 1.50(2) . ? C23C C24C 1.42(2) . ? C24C C25C 1.53(2) . ? C25C C26C 1.580(18) . ? 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 N5B U1 N5A 156.9(4) . . ? N5B U1 N1A 91.6(4) . . ? N5A U1 N1A 65.7(4) . . ? N5B U1 N1B 63.6(4) . . ? N5A U1 N1B 102.7(4) . . ? N1A U1 N1B 70.9(4) . . ? N5B U1 N3B 98.4(4) . . ? N5A U1 N3B 85.6(4) . . ? N1A U1 N3B 108.3(4) . . ? N1B U1 N3B 52.9(4) . . ? N5B U1 N3A 89.2(4) . . ? N5A U1 N3A 81.1(4) . . ? N1A U1 N3A 54.6(4) . . ? N1B U1 N3A 118.1(4) . . ? N3B U1 N3A 161.7(4) . . ? N5B U1 Cl1 89.8(3) . . ? N5A U1 Cl1 113.0(3) . . ? N1A U1 Cl1 159.8(3) . . ? N1B U1 Cl1 127.0(3) . . ? N3B U1 Cl1 91.4(3) . . ? N3A U1 Cl1 105.4(3) . . ? N5B U1 C1A 97.9(4) . . ? N5A U1 C1A 64.2(4) . . ? N1A U1 C1A 27.6(4) . . ? N1B U1 C1A 97.7(5) . . ? N3B U1 C1A 133.1(4) . . ? N3A U1 C1A 28.7(4) . . ? Cl1 U1 C1A 132.4(4) . . ? N5B U1 C1B 75.7(4) . . ? N5A U1 C1B 100.9(4) . . ? N1A U1 C1B 94.9(4) . . ? N1B U1 C1B 27.9(3) . . ? N3B U1 C1B 26.7(3) . . ? N3A U1 C1B 146.0(4) . . ? Cl1 U1 C1B 104.9(3) . . ? C1A U1 C1B 122.5(5) . . ? N1A U2 N2B 91.4(4) . . ? N1A U2 N1B 71.2(3) . . ? N2B U2 N1B 34.8(3) . . ? N1A U2 N2A 34.5(3) . . ? N2B U2 N2A 109.6(4) . . ? N1B U2 N2A 77.3(3) . . ? N1A U2 Cl2 80.5(3) . . ? N2B U2 Cl2 85.6(3) . . ? N1B U2 Cl2 109.1(3) . . ? N2A U2 Cl2 110.6(3) . . ? N1A U2 Cl3 99.7(3) . . ? N2B U2 Cl3 167.5(3) . . ? N1B U2 Cl3 156.0(3) . . ? N2A U2 Cl3 82.9(3) . . ? Cl2 U2 Cl3 90.45(11) . . ? N1A U2 Cl5 119.9(3) . . ? N2B U2 Cl5 96.1(3) . . ? N1B U2 Cl5 82.4(2) . . ? N2A U2 Cl5 88.2(3) . . ? Cl2 U2 Cl5 159.40(11) . . ? Cl3 U2 Cl5 83.43(10) . . ? N1A U2 Cl4 163.8(3) . . ? N2B U2 Cl4 82.0(3) . . ? N1B U2 Cl4 109.2(2) . . ? N2A U2 Cl4 161.3(3) . . ? Cl2 U2 Cl4 84.29(11) . . ? Cl3 U2 Cl4 85.77(10) . . ? Cl5 U2 Cl4 75.67(9) . . ? U1 U2 U3 131.700(18) . . ? N2C U3 N5C 119.1(3) 2_665 . ? N2C U3 N1C 84.4(3) 2_665 . ? N5C U3 N1C 65.2(3) . . ? N2C U3 N3C 96.5(3) 2_665 . ? N5C U3 N3C 102.9(3) . . ? N1C U3 N3C 52.5(3) . . ? N2C U3 N1C 34.9(3) 2_665 2_665 ? N5C U3 N1C 84.2(3) . 2_665 ? N1C U3 N1C 67.8(4) . 2_665 ? N3C U3 N1C 106.4(3) . 2_665 ? N2C U3 Cl6 157.5(2) 2_665 . ? N5C U3 Cl6 82.7(2) . . ? N1C U3 Cl6 111.9(2) . . ? N3C U3 Cl6 82.9(2) . . ? N1C U3 Cl6 165.4(2) 2_665 . ? N2C U3 Cl5 88.1(2) 2_665 . ? N5C U3 Cl5 82.5(2) . . ? N1C U3 Cl5 137.3(2) . . ? N3C U3 Cl5 169.9(2) . . ? N1C U3 Cl5 82.4(2) 2_665 . ? Cl6 U3 Cl5 89.43(10) . . ? N2C U3 C1C 99.4(3) 2_665 . ? N5C U3 C1C 78.4(3) . . ? N1C U3 C1C 28.4(3) . . ? N3C U3 C1C 26.8(3) . . ? N1C U3 C1C 93.5(3) 2_665 . ? Cl6 U3 C1C 90.2(3) . . ? Cl5 U3 C1C 160.8(3) . . ? N2C U3 Cl4 79.0(2) 2_665 . ? N5C U3 Cl4 150.1(3) . . ? N1C U3 Cl4 144.1(2) . . ? N3C U3 Cl4 98.0(2) . . ? N1C U3 Cl4 110.2(2) 2_665 . ? Cl6 U3 Cl4 78.86(10) . . ? Cl5 U3 Cl4 74.00(9) . . ? C1C U3 Cl4 124.7(3) . . ? U3 U3 U2 131.68(2) 2_665 . ? U2 Cl4 U3 104.66(10) . . ? U2 Cl5 U3 105.65(10) . . ? C1A N1A N2A 119.2(11) . . ? C1A N1A U2 147.1(11) . . ? N2A N1A U2 74.8(6) . . ? C1A N1A U1 95.1(9) . . ? N2A N1A U1 106.1(7) . . ? U2 N1A U1 109.9(4) . . ? C14A N2A N1A 113.9(12) . . ? C14A N2A U2 151.5(9) . . ? N1A N2A U2 70.7(6) . . ? C1A N3A C2A 118.2(13) . . ? C1A N3A U1 91.8(9) . . ? C2A N3A U1 140.7(10) . . ? C1A N4A C8A 125.6(14) . . ? C14A N5A C15A 119.7(14) . . ? C14A N5A U1 109.6(11) . . ? C15A N5A U1 129.8(10) . . ? C14A N6A C21A 127.2(14) . . ? N4A C1A N1A 126.8(16) . . ? N4A C1A N3A 121.6(16) . . ? N1A C1A N3A 111.4(13) . . ? N4A C1A U1 154.3(12) . . ? N1A C1A U1 57.3(8) . . ? N3A C1A U1 59.5(8) . . ? C3A C2A N3A 108.2(14) . . ? C3A C2A C7A 110.0(15) . . ? N3A C2A C7A 105.5(15) . . ? C2A C3A C4A 109.5(15) . . ? C5A C4A C3A 106.9(15) . . ? C4A C5A C6A 110.6(16) . . ? C5A C6A C7A 108.0(16) . . ? C2A C7A C6A 108.5(15) . . ? N4A C8A C13A 110.4(13) . . ? N4A C8A C9A 108.0(14) . . ? C13A C8A C9A 109.3(14) . . ? C8A C9A C10A 111.5(15) . . ? C11A C10A C9A 110.6(14) . . ? C12A C11A C10A 114.3(14) . . ? C11A C12A C13A 110.3(14) . . ? C8A C13A C12A 112.9(14) . . ? N6A C14A N2A 121.5(14) . . ? N6A C14A N5A 120.3(17) . . ? N2A C14A N5A 118.2(17) . . ? N5A C15A C20A 111.4(14) . . ? N5A C15A C16A 111.9(14) . . ? C20A C15A C16A 107.3(14) . . ? C17A C16A C15A 121(2) . . ? C16A C17A C18A 110(3) . . ? C19A C18A C17A 112(3) . . ? C18A C19A C20A 110(2) . . ? C19A C20A C15A 113.4(19) . . ? N6A C21A C22A 106.5(9) . . ? N6A C21A C26A 118.9(15) . . ? C22A C21A C26A 120.4(19) . . ? C21A C22A C23A 92.3(16) . . ? C24A C23A C22A 126(2) . . ? C25A C24A C23A 109.6(19) . . ? C24A C25A C26A 116(2) . . ? C25A C26A C21A 110.0(17) . . ? C1B N1B N2B 120.3(11) . . ? C1B N1B U1 94.3(9) . . ? N2B N1B U1 119.3(7) . . ? C1B N1B U2 146.9(8) . . ? N2B N1B U2 70.6(7) . . ? U1 N1B U2 107.2(4) . . ? C14B N2B N1B 111.2(12) . . ? C14B N2B U2 123.4(9) . . ? N1B N2B U2 74.6(7) . . ? C1B N3B C2B 120.4(11) . . ? C1B N3B U1 95.0(8) . . ? C2B N3B U1 144.0(8) . . ? C1B N4B C8B 119.7(11) . . ? C14B N5B C15B 116.8(13) . . ? C14B N5B U1 123.5(9) . . ? C15B N5B U1 118.7(10) . . ? C14B N6B C21B 127.2(13) . . ? N3B C1B N1B 110.9(13) . . ? N3B C1B N4B 133.5(12) . . ? N1B C1B N4B 115.5(13) . . ? N3B C1B U1 58.3(7) . . ? N1B C1B U1 57.8(7) . . ? N4B C1B U1 155.2(9) . . ? C3B C2B N3B 108.7(11) . . ? C3B C2B C7B 110.3(11) . . ? N3B C2B C7B 111.3(11) . . ? C2B C3B C4B 111.2(13) . . ? C5B C4B C3B 109.4(13) . . ? C6B C5B C4B 110.9(14) . . ? C7B C6B C5B 114.7(14) . . ? C6B C7B C2B 110.4(13) . . ? N4B C8B C9B 110.7(11) . . ? N4B C8B C13B 107.2(12) . . ? C9B C8B C13B 110.5(13) . . ? C10B C9B C8B 107.3(12) . . ? C11B C10B C9B 112.9(16) . . ? C12B C11B C10B 112.2(15) . . ? C11B C12B C13B 110.7(14) . . ? C8B C13B C12B 110.0(13) . . ? N2B C14B N6B 116.5(15) . . ? N2B C14B N5B 118.2(15) . . ? N6B C14B N5B 125.3(14) . . ? N5B C15B C20B 114.4(13) . . ? N5B C15B C16B 112.5(14) . . ? C20B C15B C16B 118.1(17) . . ? C15B C16B C17B 110.3(16) . . ? C18B C17B C16B 108.4(17) . . ? C19B C18B C17B 129(2) . . ? C18B C19B C20B 108.5(17) . . ? C19B C20B C15B 113.9(17) . . ? C26B C21B N6B 110.9(13) . . ? C26B C21B C22B 111.1(12) . . ? N6B C21B C22B 108.6(13) . . ? C23B C22B C21B 111.9(14) . . ? C22B C23B C24B 109.9(13) . . ? C23B C24B C25B 111.6(13) . . ? C26B C25B C24B 109.4(14) . . ? C25B C26B C21B 111.6(14) . . ? C1C N1C N2C 121.6(9) . . ? C1C N1C U3 92.4(7) . . ? N2C N1C U3 118.7(6) . . ? C1C N1C U3 144.1(8) . 2_665 ? N2C N1C U3 69.8(5) . 2_665 ? U3 N1C U3 112.2(4) . 2_665 ? C14C N2C N1C 111.9(9) . . ? C14C N2C U3 122.5(7) . 2_665 ? N1C N2C U3 75.3(5) . 2_665 ? C1C N3C C2C 124.6(10) . . ? C1C N3C U3 93.5(8) . . ? C2C N3C U3 140.5(7) . . ? C1C N4C C8C 122.6(11) . . ? C14C N5C C15C 121.4(10) . . ? C14C N5C U3 119.9(8) . . ? C15C N5C U3 118.1(8) . . ? C14C N6C C21C 125.9(10) . . ? N3C C1C N1C 110.5(11) . . ? N3C C1C N4C 131.2(12) . . ? N1C C1C N4C 118.2(11) . . ? N3C C1C U3 59.8(7) . . ? N1C C1C U3 59.1(6) . . ? N4C C1C U3 152.9(8) . . ? N3C C2C C3C 111.6(10) . . ? N3C C2C C7C 115.0(11) . . ? C3C C2C C7C 105.5(13) . . ? C2C C3C C4C 115.4(14) . . ? C5C C4C C3C 108.7(14) . . ? C4C C5C C6C 111.6(14) . . ? C7C C6C C5C 111.3(16) . . ? C6C C7C C2C 112.4(14) . . ? N4C C8C C9C 108.4(13) . . ? N4C C8C C13C 116.7(13) . . ? C9C C8C C13C 111.8(13) . . ? C10C C9C C8C 112.9(14) . . ? C9C C10C C11C 111.0(15) . . ? C10C C11C C12C 108.0(14) . . ? C13C C12C C11C 109.9(16) . . ? C12C C13C C8C 106.8(16) . . ? N5C C14C N2C 120.8(11) . . ? N5C C14C N6C 123.5(12) . . ? N2C C14C N6C 115.5(11) . . ? N5C C15C C16C 116.2(10) . . ? N5C C15C C20C 115.6(10) . . ? C16C C15C C20C 109.9(10) . . ? C17C C16C C15C 111.8(11) . . ? C16C C17C C18C 109.9(11) . . ? C19C C18C C17C 110.7(10) . . ? C18C C19C C20C 111.2(11) . . ? C19C C20C C15C 109.9(10) . . ? C26C C21C N6C 112.3(11) . . ? C26C C21C C22C 111.5(11) . . ? N6C C21C C22C 106.5(11) . . ? C23C C22C C21C 107.9(14) . . ? C24C C23C C22C 113.1(15) . . ? C23C C24C C25C 110.3(15) . . ? C24C C25C C26C 110.7(14) . . ? C21C C26C C25C 106.9(12) . . ?