data_14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Tb(IA)3(H2O)2(Hg2Cl4)]n.n(HgCl2).nH2O' ; _chemical_name_common '[Tb(IA)3(H2O)2(Hg2Cl4)]n.n(HgCl2).nH2O' _chemical_melting_point 'not measured' _chemical_formula_moiety '[Tb(IA)3(H2O)2(Hg2Cl4)]n.n(HgCl2).nH2O' _chemical_formula_sum 'C18 H18 Cl6 Hg3 N3 O9 Tb' _chemical_formula_weight 1393.74 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9193(4) _cell_length_b 9.5228(3) _cell_length_c 32.7149(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.100(2) _cell_angle_gamma 90.00 _cell_volume 3703.81(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8985 _cell_measurement_theta_min 3.7450 _cell_measurement_theta_max 28.5010 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 14.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.301 _exptl_absorpt_correction_T_max 0.554 _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'micro-focus sealed X-ray tube' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova (Mo) X-ray Source' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.0894 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19656 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6285 _reflns_number_gt 5261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0766P)^2^+213.6083P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6285 _refine_ls_number_parameters 360 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0880 _refine_ls_wR_factor_ref 0.2133 _refine_ls_wR_factor_gt 0.2046 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.003 _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 Hg1 Hg -0.26624(2) 0.96908(3) 0.748787(7) 0.03943(8) Uani 1 1 d . . . Hg2 Hg -0.59024(2) 0.93139(3) 0.735923(7) 0.03294(7) Uani 1 1 d . . . Hg3 Hg -0.59738(3) 0.45959(4) 0.737979(9) 0.04538(9) Uani 1 1 d . . . Cl1 Cl -0.42803(15) 1.1753(2) 0.72958(5) 0.0476(5) Uani 1 1 d . . . Cl2 Cl -0.25906(16) 0.96822(17) 0.81939(5) 0.0365(5) Uani 1 1 d . . . Cl3 Cl -0.42014(12) 0.74119(17) 0.73136(5) 0.0323(4) Uani 1 1 d . . . Cl4 Cl -0.74400(12) 0.71060(17) 0.74992(4) 0.0264(4) Uani 1 1 d . . . Cl5 Cl -0.62947(19) 0.46108(18) 0.66738(5) 0.0478(6) Uani 1 1 d . . . Cl6 Cl -0.55357(14) 0.45892(17) 0.80742(5) 0.0352(4) Uani 1 1 d . . . Tb1 Tb 0.00029(3) 1.23100(3) 0.500339(8) 0.03059(9) Uani 1 1 d . . . O1W O 0.1779(5) 1.3657(5) 0.49520(17) 0.0483(16) Uani 1 1 d . . . O2W O -0.1930(5) 1.3318(6) 0.50116(18) 0.0560(18) Uani 1 1 d . . . O1 O -0.1148(4) 0.8877(5) 0.54440(14) 0.0410(10) Uani 1 1 d U . . O2 O -0.0910(5) 1.1129(5) 0.55261(13) 0.0433(15) Uani 1 1 d . . . O3 O -0.8817(4) 0.9156(5) 0.53912(15) 0.0407(10) Uani 1 1 d U . . O4 O -0.8576(5) 1.1442(5) 0.54728(16) 0.0501(16) Uani 1 1 d . . . O5 O -0.5039(4) 0.9070(5) 0.95252(15) 0.0454(10) Uani 1 1 d U . . O6 O -0.5329(5) 1.1291(6) 0.94215(16) 0.0502(11) Uani 1 1 d U . . N1 N -0.2251(4) 0.9739(5) 0.68676(14) 0.0215(9) Uani 1 1 d U . . N2 N -0.6578(4) 0.9570(5) 0.67414(14) 0.0240(10) Uani 1 1 d U . . N3 N -0.5654(4) 0.9553(5) 0.80058(13) 0.0178(9) Uani 1 1 d U . . C1 C -0.2094(6) 1.0987(7) 0.66862(19) 0.0346(19) Uani 1 1 d . . . H1A H -0.2205 1.1809 0.6831 0.042 Uiso 1 1 calc R . . C2 C -0.1775(5) 1.1070(6) 0.62955(18) 0.0252(10) Uani 1 1 d U . . H2A H -0.1668 1.1947 0.6179 0.030 Uiso 1 1 calc R . . C3 C -0.1609(5) 0.9889(6) 0.60710(16) 0.0216(15) Uani 1 1 d . . . C4 C -0.1809(5) 0.8600(6) 0.62482(19) 0.0269(11) Uani 1 1 d U . . H4A H -0.1751 0.7775 0.6099 0.032 Uiso 1 1 calc R . . C5 C -0.2096(5) 0.8556(6) 0.66493(17) 0.0218(10) Uani 1 1 d U . . H5A H -0.2186 0.7689 0.6773 0.026 Uiso 1 1 calc R . . C6 C -0.1192(6) 0.9997(7) 0.56394(18) 0.0316(18) Uani 1 1 d . . . C7 C -0.6698(6) 1.0867(6) 0.65819(18) 0.0307(18) Uani 1 1 d . . . H7A H -0.6381 1.1632 0.6724 0.037 Uiso 1 1 calc R . . C8 C -0.7289(5) 1.1067(7) 0.62078(19) 0.0300(11) Uani 1 1 d U . . H8A H -0.7392 1.1975 0.6107 0.036 Uiso 1 1 calc R . . C9 C -0.7730(5) 0.9953(6) 0.59797(16) 0.0226(15) Uani 1 1 d . . . C10 C -0.7562(5) 0.8615(6) 0.61395(18) 0.0246(10) Uani 1 1 d U . . H10A H -0.7842 0.7839 0.5993 0.030 Uiso 1 1 calc R . . C11 C -0.6984(5) 0.8435(6) 0.65146(16) 0.0251(16) Uani 1 1 d . . . H11A H -0.6865 0.7533 0.6617 0.030 Uiso 1 1 calc R . . C12 C -0.8440(6) 1.0185(6) 0.55744(18) 0.0341(19) Uani 1 1 d . . . C13 C -0.5557(5) 1.0804(6) 0.81692(16) 0.0194(10) Uani 1 1 d U . . H13A H -0.5578 1.1579 0.7996 0.023 Uiso 1 1 calc R . . C14 C -0.5424(5) 1.1030(6) 0.85860(17) 0.0227(15) Uani 1 1 d . . . H14A H -0.5361 1.1940 0.8688 0.027 Uiso 1 1 calc R . . C15 C -0.5385(5) 0.9902(6) 0.88511(16) 0.0176(10) Uani 1 1 d U . . C16 C -0.5462(5) 0.8542(6) 0.86802(16) 0.0185(10) Uani 1 1 d U . . H16A H -0.5422 0.7744 0.8844 0.022 Uiso 1 1 calc R . . C17 C -0.5602(5) 0.8446(6) 0.82527(16) 0.0210(10) Uani 1 1 d U . . H17A H -0.5662 0.7558 0.8135 0.025 Uiso 1 1 calc R . . C18 C -0.5235(5) 1.0093(6) 0.93058(18) 0.0234(10) Uani 1 1 d U . . O3WA O 0.347(3) 1.354(4) 0.4331(11) 0.138(12) Uiso 0.30 1 d P . . O3WB O 0.4451(13) 1.3312(17) 0.3770(5) 0.138(5) Uiso 0.70 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.05439(15) 0.04624(15) 0.01905(11) 0.00109(11) 0.01235(10) -0.00330(13) Hg2 0.04249(13) 0.04788(14) 0.00747(9) 0.00037(10) -0.00508(9) 0.00164(12) Hg3 0.04876(15) 0.05606(17) 0.03041(13) 0.00131(13) -0.00358(12) -0.00104(14) Cl1 0.0490(9) 0.0575(10) 0.0392(8) 0.0220(8) 0.0245(7) 0.0179(8) Cl2 0.0591(10) 0.0299(7) 0.0210(7) 0.0015(6) 0.0066(7) -0.0030(8) Cl3 0.0230(7) 0.0320(8) 0.0430(8) -0.0081(7) 0.0102(6) -0.0021(6) Cl4 0.0282(7) 0.0312(7) 0.0189(6) 0.0017(6) -0.0045(6) -0.0023(6) Cl5 0.0839(13) 0.0302(8) 0.0290(8) 0.0026(7) 0.0031(9) 0.0012(9) Cl6 0.0395(8) 0.0294(7) 0.0352(8) 0.0018(7) -0.0078(7) -0.0032(7) Tb1 0.0577(2) 0.02139(13) 0.01203(12) 0.00177(12) -0.00226(13) 0.00107(14) O1W 0.061(3) 0.029(2) 0.056(3) -0.011(2) 0.011(3) -0.009(2) O2W 0.048(3) 0.066(3) 0.052(3) 0.002(3) -0.005(3) 0.016(3) O1 0.0471(17) 0.0431(17) 0.0340(16) -0.0048(14) 0.0107(14) 0.0006(15) O2 0.088(3) 0.027(2) 0.0163(19) 0.0025(19) 0.011(2) -0.013(2) O3 0.0448(17) 0.0396(17) 0.0365(17) -0.0008(14) -0.0061(14) -0.0102(14) O4 0.060(3) 0.049(3) 0.040(3) 0.013(2) -0.007(2) 0.029(2) O5 0.0555(18) 0.0404(17) 0.0398(17) 0.0023(15) 0.0005(15) -0.0003(15) O6 0.0583(18) 0.0461(18) 0.0454(18) -0.0046(15) -0.0023(15) 0.0034(15) N1 0.0269(16) 0.0202(16) 0.0181(15) -0.0007(13) 0.0072(13) 0.0000(14) N2 0.0274(17) 0.0237(16) 0.0210(16) 0.0001(14) 0.0031(13) 0.0020(14) N3 0.0235(15) 0.0168(15) 0.0148(15) 0.0020(13) 0.0127(12) 0.0006(13) C1 0.047(4) 0.034(3) 0.023(3) 0.007(3) 0.005(3) 0.005(3) C2 0.0285(18) 0.0249(18) 0.0225(17) -0.0017(15) 0.0053(15) 0.0028(15) C3 0.025(3) 0.024(3) 0.016(2) -0.009(2) 0.004(2) -0.003(2) C4 0.0313(18) 0.0231(18) 0.0267(18) -0.0017(15) 0.0041(15) 0.0001(15) C5 0.0242(17) 0.0231(17) 0.0186(17) 0.0025(15) 0.0063(14) 0.0020(15) C6 0.048(4) 0.030(3) 0.017(3) -0.004(3) 0.008(3) 0.005(3) C7 0.050(4) 0.019(3) 0.021(3) 0.002(3) -0.012(3) -0.006(3) C8 0.0357(19) 0.0274(18) 0.0264(18) 0.0046(15) -0.0001(15) 0.0005(15) C9 0.029(3) 0.027(3) 0.012(2) 0.002(2) 0.000(2) -0.014(2) C10 0.0271(18) 0.0245(18) 0.0222(17) 0.0021(15) 0.0012(15) 0.0008(15) C11 0.045(3) 0.021(3) 0.009(2) -0.001(2) 0.002(2) -0.004(3) C12 0.062(4) 0.022(3) 0.019(3) 0.007(3) 0.011(3) 0.003(3) C13 0.0229(17) 0.0189(17) 0.0159(16) 0.0044(14) -0.0019(14) 0.0021(15) C14 0.029(3) 0.017(2) 0.022(3) -0.003(2) 0.007(2) 0.014(2) C15 0.0194(17) 0.0174(17) 0.0165(16) -0.0008(14) 0.0041(14) -0.0030(14) C16 0.0245(17) 0.0161(17) 0.0151(17) -0.0016(14) 0.0025(14) -0.0005(15) C17 0.0276(18) 0.0198(17) 0.0155(17) -0.0052(14) 0.0013(14) 0.0032(15) C18 0.0272(18) 0.0183(17) 0.0245(17) 0.0050(15) 0.0000(15) -0.0022(15) _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 Hg1 N1 2.122(5) . ? Hg1 Cl2 2.3051(15) . ? Hg1 Cl1 2.7920(19) . ? Hg1 Cl3 2.8723(16) . ? Hg2 N3 2.127(4) . ? Hg2 N2 2.136(5) . ? Hg2 Cl3 2.7307(16) . ? Hg2 Cl4 2.8477(16) . ? Hg3 Cl6 2.2943(17) . ? Hg3 Cl5 2.3140(18) . ? Tb1 O5 2.276(5) 2_456 ? Tb1 O3 2.313(5) 3_476 ? Tb1 O6 2.334(5) 4_685 ? Tb1 O4 2.354(5) 1_655 ? Tb1 O1 2.360(5) 3_576 ? Tb1 O2 2.375(5) . ? Tb1 O1W 2.491(5) . ? Tb1 O2W 2.498(6) . ? O1 C6 1.247(8) . ? O1 Tb1 2.360(5) 3_576 ? O2 C6 1.196(8) . ? O3 C12 1.218(8) . ? O3 Tb1 2.313(5) 3_476 ? O4 C12 1.250(8) . ? O4 Tb1 2.354(5) 1_455 ? O5 C18 1.222(8) . ? O5 Tb1 2.276(5) 2_446 ? O6 C18 1.210(8) . ? O6 Tb1 2.334(5) 4_586 ? N1 C1 1.347(8) . ? N1 C5 1.353(7) . ? N2 C7 1.345(8) . ? N2 C11 1.378(8) . ? N3 C13 1.307(7) . ? N3 C17 1.327(7) . ? C1 C2 1.361(9) . ? C1 H1A 0.9300 . ? C2 C3 1.365(8) . ? C2 H2A 0.9300 . ? C3 C4 1.385(8) . ? C3 C6 1.534(8) . ? C4 C5 1.380(8) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C7 C8 1.381(8) . ? C7 H7A 0.9300 . ? C8 C9 1.379(8) . ? C8 H8A 0.9300 . ? C9 C10 1.386(8) . ? C9 C12 1.537(8) . ? C10 C11 1.375(8) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.379(8) . ? C13 H13A 0.9300 . ? C14 C15 1.379(8) . ? C14 H14A 0.9300 . ? C15 C16 1.411(8) . ? C15 C18 1.497(8) . ? C16 C17 1.400(7) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? 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 N1 Hg1 Cl2 164.51(14) . . ? N1 Hg1 Cl1 88.44(13) . . ? Cl2 Hg1 Cl1 101.75(6) . . ? N1 Hg1 Cl3 90.83(13) . . ? Cl2 Hg1 Cl3 100.00(6) . . ? Cl1 Hg1 Cl3 93.76(5) . . ? N3 Hg2 N2 160.96(18) . . ? N3 Hg2 Cl3 94.26(12) . . ? N2 Hg2 Cl3 104.78(14) . . ? N3 Hg2 Cl4 87.98(12) . . ? N2 Hg2 Cl4 91.88(14) . . ? Cl3 Hg2 Cl4 90.46(5) . . ? Cl6 Hg3 Cl5 176.36(7) . . ? Hg2 Cl3 Hg1 87.37(5) . . ? O5 Tb1 O3 143.49(19) 2_456 3_476 ? O5 Tb1 O6 97.26(18) 2_456 4_685 ? O3 Tb1 O6 80.11(18) 3_476 4_685 ? O5 Tb1 O4 80.71(18) 2_456 1_655 ? O3 Tb1 O4 122.32(17) 3_476 1_655 ? O6 Tb1 O4 143.57(19) 4_685 1_655 ? O5 Tb1 O1 142.11(18) 2_456 3_576 ? O3 Tb1 O1 73.87(17) 3_476 3_576 ? O6 Tb1 O1 80.75(18) 4_685 3_576 ? O4 Tb1 O1 79.35(17) 1_655 3_576 ? O5 Tb1 O2 81.27(17) 2_456 . ? O3 Tb1 O2 79.81(17) 3_476 . ? O6 Tb1 O2 142.95(19) 4_685 . ? O4 Tb1 O2 73.10(18) 1_655 . ? O1 Tb1 O2 122.34(17) 3_576 . ? O5 Tb1 O1W 72.04(18) 2_456 . ? O3 Tb1 O1W 139.57(18) 3_476 . ? O6 Tb1 O1W 75.29(18) 4_685 . ? O4 Tb1 O1W 69.47(18) 1_655 . ? O1 Tb1 O1W 70.90(17) 3_576 . ? O2 Tb1 O1W 136.70(17) . . ? O5 Tb1 O2W 71.49(19) 2_456 . ? O3 Tb1 O2W 73.19(18) 3_476 . ? O6 Tb1 O2W 71.75(19) 4_685 . ? O4 Tb1 O2W 138.54(19) 1_655 . ? O1 Tb1 O2W 139.97(17) 3_576 . ? O2 Tb1 O2W 72.77(19) . . ? O1W Tb1 O2W 126.28(18) . . ? C6 O1 Tb1 140.8(5) . 3_576 ? C6 O2 Tb1 143.5(4) . . ? C12 O3 Tb1 161.7(5) . 3_476 ? C12 O4 Tb1 125.7(5) . 1_455 ? C18 O5 Tb1 168.0(5) . 2_446 ? C18 O6 Tb1 141.2(5) . 4_586 ? C1 N1 C5 118.2(5) . . ? C1 N1 Hg1 119.3(4) . . ? C5 N1 Hg1 122.4(4) . . ? C7 N2 C11 119.2(5) . . ? C7 N2 Hg2 119.6(4) . . ? C11 N2 Hg2 120.9(4) . . ? C13 N3 C17 118.4(5) . . ? C13 N3 Hg2 120.4(4) . . ? C17 N3 Hg2 121.2(4) . . ? N1 C1 C2 121.4(6) . . ? N1 C1 H1A 119.3 . . ? C2 C1 H1A 119.3 . . ? C1 C2 C3 121.2(6) . . ? C1 C2 H2A 119.4 . . ? C3 C2 H2A 119.4 . . ? C2 C3 C4 118.0(5) . . ? C2 C3 C6 120.6(5) . . ? C4 C3 C6 121.5(5) . . ? C5 C4 C3 119.1(6) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? N1 C5 C4 121.9(5) . . ? N1 C5 H5A 119.0 . . ? C4 C5 H5A 119.0 . . ? O2 C6 O1 126.1(6) . . ? O2 C6 C3 117.6(5) . . ? O1 C6 C3 116.3(6) . . ? N2 C7 C8 120.2(6) . . ? N2 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C9 C8 C7 121.6(6) . . ? C9 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? C8 C9 C10 117.6(5) . . ? C8 C9 C12 121.4(5) . . ? C10 C9 C12 120.8(5) . . ? C11 C10 C9 120.0(5) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 N2 121.1(5) . . ? C10 C11 H11A 119.4 . . ? N2 C11 H11A 119.4 . . ? O3 C12 O4 127.1(6) . . ? O3 C12 C9 118.1(5) . . ? O4 C12 C9 114.8(5) . . ? N3 C13 C14 123.2(5) . . ? N3 C13 H13A 118.4 . . ? C14 C13 H13A 118.4 . . ? C13 C14 C15 119.8(5) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C14 C15 C16 117.9(5) . . ? C14 C15 C18 121.8(5) . . ? C16 C15 C18 120.3(5) . . ? C17 C16 C15 117.1(5) . . ? C17 C16 H16A 121.5 . . ? C15 C16 H16A 121.5 . . ? N3 C17 C16 123.6(5) . . ? N3 C17 H17A 118.2 . . ? C16 C17 H17A 118.2 . . ? O6 C18 O5 125.9(6) . . ? O6 C18 C15 114.7(5) . . ? O5 C18 C15 119.4(5) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 3.376 _refine_diff_density_min -3.576 _refine_diff_density_rms 0.381