# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_platon _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18 Al2 N2 O12' _chemical_formula_weight 412.22 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 11.1089(10) _cell_length_b 9.4830(8) _cell_length_c 7.6116(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.026(3) _cell_angle_gamma 90.00 _cell_volume 743.33(11) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 3384 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 24.96 _exptl_crystal_description blocky _exptl_crystal_colour colorless _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 428 _exptl_absorpt_coefficient_mu 0.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7023 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(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 KappaCCD _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6460 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1317 _reflns_number_gt 1260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'APEX2 (Bruker AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalMaker v2.5.0' _computing_publication_material 'enCIFer 1.4' _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^)+(0.0391P)^2^+0.4853P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(19) _refine_ls_number_reflns 1317 _refine_ls_number_parameters 118 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0692 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.000 _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 Al1 Al -0.11684(6) 0.31910(7) 0.33517(8) 0.01717(16) Uani 1 1 d . . . O1 O 0.06046(13) 0.32720(18) 0.40327(18) 0.0182(3) Uani 1 1 d . . . H6 H 0.0927 0.3663 0.3163 0.027 Uiso 1 1 d R . . O2 O -0.16810(16) 0.46352(19) -0.1727(2) 0.0246(4) Uani 1 1 d . . . O3 O -0.29185(14) 0.31098(18) 0.2963(2) 0.0222(3) Uani 1 1 d . . . O4 O -0.12092(15) 0.12070(18) 0.3233(2) 0.0210(4) Uani 1 1 d . . . H5A H -0.1978 0.0658 0.2840 0.031 Uiso 1 1 d R . . H5B H -0.0535 0.0673 0.3062 0.031 Uiso 1 1 d R . . O5 O -0.14861(15) 0.3277(2) 0.0743(2) 0.0229(3) Uani 1 1 d . . . O6 O -0.47218(16) 0.4292(2) 0.2552(3) 0.0360(5) Uani 1 1 d . . . N1 N -0.1471(2) 0.5387(2) 0.3012(3) 0.0194(4) Uani 1 1 d . . . C1 C -0.1217(2) 0.5752(3) 0.1278(3) 0.0239(5) Uani 1 1 d . . . H1A H -0.0319 0.6039 0.1629 0.029 Uiso 1 1 calc R . . H1B H -0.1768 0.6533 0.0627 0.029 Uiso 1 1 calc R . . C2 C -0.3584(2) 0.4236(3) 0.2725(3) 0.0231(5) Uani 1 1 d . . . C3 C -0.0740(2) 0.6357(2) 0.4630(3) 0.0238(5) Uani 1 1 d . . . H3A H -0.0996 0.6128 0.5683 0.029 Uiso 1 1 calc R . . H3B H -0.1032 0.7311 0.4240 0.029 Uiso 1 1 calc R . . C4 C -0.2894(2) 0.5593(3) 0.2618(3) 0.0256(5) Uani 1 1 d . . . H4A H -0.3310 0.5999 0.1365 0.031 Uiso 1 1 calc R . . H4B H -0.2985 0.6260 0.3527 0.031 Uiso 1 1 calc R . . C5 C -0.1494(2) 0.4479(3) -0.0031(3) 0.0220(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0194(3) 0.0181(3) 0.0151(3) -0.0001(3) 0.0077(2) 0.0012(3) O1 0.0204(7) 0.0212(7) 0.0157(7) 0.0003(7) 0.0098(6) -0.0017(8) O2 0.0266(8) 0.0333(10) 0.0162(8) 0.0033(6) 0.0105(6) 0.0079(7) O3 0.0193(7) 0.0223(8) 0.0263(7) 0.0014(8) 0.0100(6) 0.0035(8) O4 0.0181(8) 0.0208(9) 0.0250(8) -0.0023(6) 0.0090(7) 0.0011(6) O5 0.0275(8) 0.0233(8) 0.0175(7) 0.0004(8) 0.0079(6) 0.0016(8) O6 0.0218(9) 0.0287(10) 0.0604(13) -0.0061(9) 0.0187(8) 0.0028(8) N1 0.0235(11) 0.0196(11) 0.0179(9) 0.0014(8) 0.0111(8) 0.0023(8) C1 0.0296(13) 0.0257(12) 0.0183(11) 0.0048(10) 0.0112(10) 0.0018(11) C2 0.0243(13) 0.0252(13) 0.0211(12) -0.0010(9) 0.0097(10) 0.0018(11) C3 0.0325(14) 0.0211(12) 0.0181(11) -0.0013(9) 0.0099(10) 0.0021(10) C4 0.0259(13) 0.0227(13) 0.0315(13) 0.0026(10) 0.0144(10) 0.0059(10) C5 0.0176(11) 0.0287(13) 0.0214(12) 0.0014(10) 0.0095(9) 0.0046(10) _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 Al1 O1 1.8408(15) . ? Al1 O1 1.8511(14) 2_556 ? Al1 O3 1.8551(15) . ? Al1 O4 1.8833(18) . ? Al1 O5 1.8839(15) . ? Al1 N1 2.110(2) . ? Al1 Al1 2.8548(12) 2_556 ? O1 Al1 1.8511(14) 2_556 ? O1 H6 0.9385 . ? O2 C5 1.237(3) . ? O3 C2 1.273(3) . ? O4 H5A 0.9475 . ? O4 H5B 0.9521 . ? O5 C5 1.281(3) . ? O6 C2 1.222(3) . ? N1 C1 1.490(3) . ? N1 C4 1.507(3) . ? N1 C3 1.507(3) . ? C1 C5 1.522(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.516(4) . ? C3 C3 1.525(5) 2_556 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 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 O1 Al1 O1 78.51(7) . 2_556 ? O1 Al1 O3 173.38(7) . . ? O1 Al1 O3 94.88(7) 2_556 . ? O1 Al1 O4 93.39(8) . . ? O1 Al1 O4 94.89(8) 2_556 . ? O3 Al1 O4 86.90(8) . . ? O1 Al1 O5 93.02(6) . . ? O1 Al1 O5 170.40(8) 2_556 . ? O3 Al1 O5 93.59(7) . . ? O4 Al1 O5 90.07(8) . . ? O1 Al1 N1 95.61(8) . . ? O1 Al1 N1 93.72(8) 2_556 . ? O3 Al1 N1 84.96(8) . . ? O4 Al1 N1 168.62(7) . . ? O5 Al1 N1 82.52(8) . . ? O1 Al1 Al1 39.49(4) . 2_556 ? O1 Al1 Al1 39.22(4) 2_556 2_556 ? O3 Al1 Al1 133.90(5) . 2_556 ? O4 Al1 Al1 92.27(5) . 2_556 ? O5 Al1 Al1 132.50(6) . 2_556 ? N1 Al1 Al1 99.10(6) . 2_556 ? Al1 O1 Al1 101.29(7) . 2_556 ? Al1 O1 H6 117.9 . . ? Al1 O1 H6 135.2 2_556 . ? C2 O3 Al1 120.41(16) . . ? Al1 O4 H5A 124.5 . . ? Al1 O4 H5B 122.1 . . ? H5A O4 H5B 109.0 . . ? C5 O5 Al1 119.30(16) . . ? C1 N1 C4 109.03(18) . . ? C1 N1 C3 111.03(18) . . ? C4 N1 C3 106.68(17) . . ? C1 N1 Al1 105.28(14) . . ? C4 N1 Al1 105.05(14) . . ? C3 N1 Al1 119.34(14) . . ? N1 C1 C5 109.67(19) . . ? N1 C1 H1A 109.7 . . ? C5 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C5 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? O6 C2 O3 125.1(2) . . ? O6 C2 C4 118.7(2) . . ? O3 C2 C4 116.2(2) . . ? N1 C3 C3 118.56(19) . 2_556 ? N1 C3 H3A 107.7 . . ? C3 C3 H3A 107.7 2_556 . ? N1 C3 H3B 107.7 . . ? C3 C3 H3B 107.7 2_556 . ? H3A C3 H3B 107.1 . . ? N1 C4 C2 113.14(19) . . ? N1 C4 H4A 109.0 . . ? C2 C4 H4A 108.9 . . ? N1 C4 H4B 108.9 . . ? C2 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? O2 C5 O5 123.8(2) . . ? O2 C5 C1 120.1(2) . . ? O5 C5 C1 116.11(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Al1 O1 Al1 4.85(12) 2_556 . . 2_556 ? O3 Al1 O1 Al1 2.9(8) . . . 2_556 ? O4 Al1 O1 Al1 -89.46(9) . . . 2_556 ? O5 Al1 O1 Al1 -179.71(8) . . . 2_556 ? N1 Al1 O1 Al1 97.51(8) . . . 2_556 ? O1 Al1 O3 C2 93.2(8) . . . . ? O1 Al1 O3 C2 91.29(16) 2_556 . . . ? O4 Al1 O3 C2 -174.06(16) . . . . ? O5 Al1 O3 C2 -84.19(16) . . . . ? N1 Al1 O3 C2 -2.02(15) . . . . ? Al1 Al1 O3 C2 95.76(15) 2_556 . . . ? O1 Al1 O5 C5 -82.66(16) . . . . ? O1 Al1 O5 C5 -54.8(6) 2_556 . . . ? O3 Al1 O5 C5 97.04(16) . . . . ? O4 Al1 O5 C5 -176.06(15) . . . . ? N1 Al1 O5 C5 12.61(15) . . . . ? Al1 Al1 O5 C5 -82.91(16) 2_556 . . . ? O1 Al1 N1 C1 70.29(15) . . . . ? O1 Al1 N1 C1 149.09(15) 2_556 . . . ? O3 Al1 N1 C1 -116.34(15) . . . . ? O4 Al1 N1 C1 -71.8(4) . . . . ? O5 Al1 N1 C1 -22.03(14) . . . . ? Al1 Al1 N1 C1 109.97(14) 2_556 . . . ? O1 Al1 N1 C4 -174.66(13) . . . . ? O1 Al1 N1 C4 -95.87(13) 2_556 . . . ? O3 Al1 N1 C4 -1.29(13) . . . . ? O4 Al1 N1 C4 43.2(4) . . . . ? O5 Al1 N1 C4 93.02(14) . . . . ? Al1 Al1 N1 C4 -134.99(12) 2_556 . . . ? O1 Al1 N1 C3 -55.18(16) . . . . ? O1 Al1 N1 C3 23.62(17) 2_556 . . . ? O3 Al1 N1 C3 118.19(17) . . . . ? O4 Al1 N1 C3 162.7(3) . . . . ? O5 Al1 N1 C3 -147.50(17) . . . . ? Al1 Al1 N1 C3 -15.50(16) 2_556 . . . ? C4 N1 C1 C5 -85.1(2) . . . . ? C3 N1 C1 C5 157.67(18) . . . . ? Al1 N1 C1 C5 27.2(2) . . . . ? Al1 O3 C2 O6 -176.25(18) . . . . ? Al1 O3 C2 C4 4.9(2) . . . . ? C1 N1 C3 C3 -62.4(2) . . . 2_556 ? C4 N1 C3 C3 178.92(18) . . . 2_556 ? Al1 N1 C3 C3 60.3(2) . . . 2_556 ? C1 N1 C4 C2 116.2(2) . . . . ? C3 N1 C4 C2 -123.8(2) . . . . ? Al1 N1 C4 C2 3.8(2) . . . . ? O6 C2 C4 N1 175.28(19) . . . . ? O3 C2 C4 N1 -5.8(3) . . . . ? Al1 O5 C5 O2 179.26(16) . . . . ? Al1 O5 C5 C1 1.0(2) . . . . ? N1 C1 C5 O2 160.9(2) . . . . ? N1 C1 C5 O5 -20.7(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.203 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.048 _database_code_depnum_ccdc_archive 'CCDC 939971' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p21c _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetraaquahexakisethylenediaminethorium(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H20 N2 O12 Th' _chemical_formula_weight 592.32 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' Th Th -7.2400 8.8979 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5283(5) _cell_length_b 12.0641(7) _cell_length_c 15.8846(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.335(2) _cell_angle_gamma 90.00 _cell_volume 1576.12(16) _cell_formula_units_Z 4 _cell_measurement_temperature 181(2) _cell_measurement_reflns_used 9994 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.43 _exptl_crystal_description blocky _exptl_crystal_colour colorless _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.180 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 9.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.254 _exptl_absorpt_correction_T_max 0.534 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 181(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 KappaCCD _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23554 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0152 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3586 _reflns_number_gt 3434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'APEX2 (Bruker AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalMaker v2.5.0' _computing_publication_material 'enCIFer 1.4' _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^)+(0.0179P)^2^+1.4763P] 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 SHELXL _refine_ls_extinction_coef 0.00093(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3586 _refine_ls_number_parameters 251 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0134 _refine_ls_R_factor_gt 0.0123 _refine_ls_wR_factor_ref 0.0340 _refine_ls_wR_factor_gt 0.0335 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.005 _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 Th1 Th 0.592673(9) 0.621451(5) 0.242576(4) 0.01144(4) Uani 1 1 d . . . O1 O 0.3577(2) 0.49481(13) 0.23237(10) 0.0183(3) Uani 1 1 d D . . O2 O 0.70678(19) 0.74414(13) 0.36213(10) 0.0182(3) Uani 1 1 d . . . O3 O 0.72629(19) 0.44475(12) 0.28990(10) 0.0191(3) Uani 1 1 d . . . O4 O 0.3653(2) 0.68270(14) 0.11432(10) 0.0214(3) Uani 1 1 d D . . O5 O 0.5418(2) 0.49499(13) 0.12065(10) 0.0193(3) Uani 1 1 d . . . O6 O 0.5425(2) 0.56383(14) 0.38898(10) 0.0234(4) Uani 1 1 d D . . O7 O 0.6694(2) 0.79852(12) 0.18810(10) 0.0187(3) Uani 1 1 d . . . O8 O 0.3825(2) 0.74644(13) 0.28230(11) 0.0190(3) Uani 1 1 d D . . O9 O 0.8677(2) 0.89077(13) 0.40076(12) 0.0251(4) Uani 1 1 d . . . O10 O 0.6236(2) 0.35569(14) 0.05151(11) 0.0230(4) Uani 1 1 d . . . O11 O 0.8621(2) 0.34909(14) 0.40650(11) 0.0253(4) Uani 1 1 d . . . O12 O 0.6539(2) 0.89911(14) 0.06908(11) 0.0255(4) Uani 1 1 d . . . N1 N 0.8002(2) 0.62157(13) 0.13084(13) 0.0157(4) Uani 1 1 d . . . N2 N 0.9261(2) 0.61768(14) 0.32201(13) 0.0156(4) Uani 1 1 d . . . C1 C 0.8380(3) 0.43395(18) 0.36204(14) 0.0174(4) Uani 1 1 d . . . C2 C 0.8440(3) 0.79363(18) 0.37665(14) 0.0160(4) Uani 1 1 d . . . C3 C 0.9430(3) 0.53562(18) 0.39254(14) 0.0185(4) Uani 1 1 d . . . H3A H 0.9112 0.5701 0.4421 0.022 Uiso 1 1 calc R . . H3B H 1.0583 0.5127 0.4134 0.022 Uiso 1 1 calc R . . C4 C 1.0234(3) 0.58203(19) 0.26221(15) 0.0193(4) Uani 1 1 d . . . H4A H 1.0079 0.5016 0.2506 0.023 Uiso 1 1 calc R . . H4B H 1.1402 0.5953 0.2901 0.023 Uiso 1 1 calc R . . C5 C 0.9728(3) 0.6450(2) 0.17715(15) 0.0190(4) Uani 1 1 d . . . H5A H 0.9866 0.7255 0.1889 0.023 Uiso 1 1 calc R . . H5B H 1.0436 0.6236 0.1395 0.023 Uiso 1 1 calc R . . C6 C 0.6849(3) 0.81134(18) 0.11058(14) 0.0164(4) Uani 1 1 d . . . C7 C 0.9836(3) 0.72691(18) 0.36053(16) 0.0196(5) Uani 1 1 d . . . H7A H 1.0337 0.7682 0.3204 0.023 Uiso 1 1 calc R . . H7B H 1.0676 0.7160 0.4163 0.023 Uiso 1 1 calc R . . C8 C 0.7390(3) 0.71181(18) 0.06779(14) 0.0174(4) Uani 1 1 d . . . H8A H 0.6463 0.6840 0.0209 0.021 Uiso 1 1 calc R . . H8B H 0.8259 0.7346 0.0406 0.021 Uiso 1 1 calc R . . C9 C 0.7920(3) 0.51446(18) 0.08373(16) 0.0202(5) Uani 1 1 d . . . H9A H 0.8890 0.4695 0.1115 0.024 Uiso 1 1 calc R . . H9B H 0.7935 0.5289 0.0226 0.024 Uiso 1 1 calc R . . C10 C 0.6416(3) 0.45040(18) 0.08432(13) 0.0158(4) Uani 1 1 d . . . H1A H 0.361(3) 0.4277(13) 0.2643(13) 0.019 Uiso 1 1 d D . . H1B H 0.300(3) 0.4759(19) 0.1745(8) 0.019 Uiso 1 1 d D . . H4C H 0.299(3) 0.7450(14) 0.1108(15) 0.019 Uiso 1 1 d D . . H4D H 0.351(3) 0.661(2) 0.0560(8) 0.019 Uiso 1 1 d D . . H6A H 0.475(3) 0.5044(15) 0.3930(15) 0.019 Uiso 1 1 d D . . H6B H 0.582(3) 0.590(2) 0.4462(9) 0.019 Uiso 1 1 d D . . H8C H 0.420(3) 0.7652(19) 0.3424(7) 0.019 Uiso 1 1 d D . . H8D H 0.346(3) 0.8148(13) 0.2534(13) 0.019 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Th1 0.01366(5) 0.00983(5) 0.01117(5) -0.00018(2) 0.00385(3) -0.00015(2) O1 0.0226(8) 0.0155(7) 0.0173(8) -0.0004(6) 0.0061(7) -0.0036(6) O2 0.0186(8) 0.0194(8) 0.0172(7) -0.0056(6) 0.0059(6) -0.0037(6) O3 0.0209(8) 0.0138(7) 0.0190(8) 0.0003(6) -0.0008(6) -0.0006(6) O4 0.0249(9) 0.0232(8) 0.0144(7) -0.0017(6) 0.0025(6) 0.0080(7) O5 0.0201(8) 0.0216(8) 0.0178(8) -0.0064(6) 0.0078(6) -0.0006(6) O6 0.0332(10) 0.0234(8) 0.0143(8) -0.0009(6) 0.0077(7) -0.0107(7) O7 0.0290(9) 0.0145(7) 0.0152(7) 0.0001(6) 0.0106(6) 0.0007(6) O8 0.0234(8) 0.0155(7) 0.0179(8) -0.0017(6) 0.0052(7) 0.0046(6) O9 0.0270(10) 0.0181(8) 0.0308(10) -0.0071(7) 0.0086(8) -0.0047(7) O10 0.0312(10) 0.0177(7) 0.0212(8) -0.0056(7) 0.0089(7) -0.0011(7) O11 0.0301(10) 0.0163(8) 0.0256(9) 0.0068(7) 0.0009(7) -0.0013(7) O12 0.0405(11) 0.0171(8) 0.0207(9) 0.0069(7) 0.0113(8) 0.0080(7) N1 0.0184(10) 0.0118(9) 0.0174(9) 0.0010(6) 0.0060(8) 0.0010(7) N2 0.0150(9) 0.0127(9) 0.0187(10) 0.0008(6) 0.0038(7) -0.0005(6) C1 0.0199(11) 0.0147(10) 0.0174(10) 0.0003(8) 0.0047(9) 0.0030(8) C2 0.0188(11) 0.0177(10) 0.0114(10) 0.0002(8) 0.0036(8) -0.0026(8) C3 0.0208(11) 0.0165(10) 0.0153(10) 0.0017(8) -0.0001(9) -0.0005(9) C4 0.0172(11) 0.0182(11) 0.0233(11) 0.0022(9) 0.0066(9) 0.0026(9) C5 0.0174(11) 0.0200(10) 0.0217(11) 0.0012(9) 0.0089(9) -0.0004(9) C6 0.0176(11) 0.0158(10) 0.0158(10) 0.0006(8) 0.0045(8) -0.0001(8) C7 0.0170(11) 0.0145(10) 0.0261(12) -0.0020(9) 0.0038(9) -0.0040(8) C8 0.0230(11) 0.0162(10) 0.0149(10) 0.0014(8) 0.0083(9) 0.0030(9) C9 0.0248(12) 0.0146(10) 0.0246(12) -0.0021(9) 0.0124(9) 0.0016(9) C10 0.0196(11) 0.0164(10) 0.0102(9) 0.0010(7) 0.0019(8) 0.0034(8) _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 Th1 O2 2.4014(15) . ? Th1 O5 2.4130(15) . ? Th1 O3 2.4403(15) . ? Th1 O7 2.4576(15) . ? Th1 O1 2.4911(16) . ? Th1 O4 2.5233(16) . ? Th1 O8 2.5461(16) . ? Th1 O6 2.5693(16) . ? Th1 N2 2.790(2) . ? Th1 N1 2.819(2) . ? O1 H1A 0.952(10) . ? O1 H1B 0.948(9) . ? O2 C2 1.279(3) . ? O3 C1 1.289(3) . ? O4 H4C 0.935(10) . ? O4 H4D 0.939(10) . ? O5 C10 1.267(3) . ? O6 H6A 0.930(10) . ? O6 H6B 0.937(10) . ? O7 C6 1.282(3) . ? O8 H8C 0.951(10) . ? O8 H8D 0.954(10) . ? O9 C2 1.233(3) . ? O10 C10 1.248(3) . ? O11 C1 1.230(3) . ? O12 C6 1.238(3) . ? N1 C8 1.478(3) . ? N1 C9 1.486(3) . ? N1 C5 1.488(3) . ? N2 C3 1.473(3) . ? N2 C4 1.481(3) . ? N2 C7 1.481(3) . ? C1 C3 1.520(3) . ? C2 C7 1.514(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.510(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C8 1.511(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.500(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Th1 O5 166.83(6) . . ? O2 Th1 O3 103.66(5) . . ? O5 Th1 O3 70.44(5) . . ? O2 Th1 O7 69.68(5) . . ? O5 Th1 O7 105.97(5) . . ? O3 Th1 O7 136.19(5) . . ? O2 Th1 O1 125.47(5) . . ? O5 Th1 O1 65.74(5) . . ? O3 Th1 O1 77.67(5) . . ? O7 Th1 O1 142.64(5) . . ? O2 Th1 O4 121.48(5) . . ? O5 Th1 O4 66.45(5) . . ? O3 Th1 O4 134.51(5) . . ? O7 Th1 O4 71.37(6) . . ? O1 Th1 O4 72.17(6) . . ? O2 Th1 O8 66.65(5) . . ? O5 Th1 O8 125.76(5) . . ? O3 Th1 O8 137.99(5) . . ? O7 Th1 O8 80.97(5) . . ? O1 Th1 O8 76.84(5) . . ? O4 Th1 O8 65.52(5) . . ? O2 Th1 O6 65.20(5) . . ? O5 Th1 O6 121.18(5) . . ? O3 Th1 O6 70.17(6) . . ? O7 Th1 O6 132.65(5) . . ? O1 Th1 O6 64.48(5) . . ? O4 Th1 O6 122.25(6) . . ? O8 Th1 O6 68.85(6) . . ? O2 Th1 N2 60.07(5) . . ? O5 Th1 N2 107.35(5) . . ? O3 Th1 N2 60.62(5) . . ? O7 Th1 N2 80.73(5) . . ? O1 Th1 N2 136.53(5) . . ? O4 Th1 N2 147.53(6) . . ? O8 Th1 N2 126.71(5) . . ? O6 Th1 N2 88.86(6) . . ? O2 Th1 N1 107.88(5) . . ? O5 Th1 N1 60.30(5) . . ? O3 Th1 N1 82.80(5) . . ? O7 Th1 N1 60.51(5) . . ? O1 Th1 N1 126.00(5) . . ? O4 Th1 N1 88.16(6) . . ? O8 Th1 N1 139.13(5) . . ? O6 Th1 N1 148.51(6) . . ? N2 Th1 N1 63.26(6) . . ? Th1 O1 H1A 125.4(16) . . ? Th1 O1 H1B 114.2(15) . . ? H1A O1 H1B 104.3(16) . . ? C2 O2 Th1 126.18(14) . . ? C1 O3 Th1 122.52(13) . . ? Th1 O4 H4C 127.5(15) . . ? Th1 O4 H4D 126.0(15) . . ? H4C O4 H4D 104.3(16) . . ? C10 O5 Th1 129.33(14) . . ? Th1 O6 H6A 121.6(14) . . ? Th1 O6 H6B 133.1(15) . . ? H6A O6 H6B 105.3(17) . . ? C6 O7 Th1 123.21(13) . . ? Th1 O8 H8C 108.4(15) . . ? Th1 O8 H8D 123.4(16) . . ? H8C O8 H8D 104.9(16) . . ? C8 N1 C9 109.77(18) . . ? C8 N1 C5 108.71(17) . . ? C9 N1 C5 108.86(18) . . ? C8 N1 Th1 105.01(13) . . ? C9 N1 Th1 111.28(13) . . ? C5 N1 Th1 113.10(13) . . ? C3 N2 C4 109.52(17) . . ? C3 N2 C7 109.19(18) . . ? C4 N2 C7 110.08(18) . . ? C3 N2 Th1 103.75(13) . . ? C4 N2 Th1 113.06(13) . . ? C7 N2 Th1 111.03(13) . . ? O11 C1 O3 124.5(2) . . ? O11 C1 C3 119.6(2) . . ? O3 C1 C3 115.88(19) . . ? O9 C2 O2 124.5(2) . . ? O9 C2 C7 119.1(2) . . ? O2 C2 C7 116.37(18) . . ? N2 C3 C1 111.65(18) . . ? N2 C3 H3A 109.3 . . ? C1 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? C1 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? N2 C4 C5 110.58(18) . . ? N2 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N1 C5 C4 110.97(19) . . ? N1 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? N1 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? O12 C6 O7 123.6(2) . . ? O12 C6 C8 119.2(2) . . ? O7 C6 C8 117.22(19) . . ? N2 C7 C2 110.72(18) . . ? N2 C7 H7A 109.5 . . ? C2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N1 C8 C6 112.08(17) . . ? N1 C8 H8A 109.2 . . ? C6 C8 H8A 109.2 . . ? N1 C8 H8B 109.2 . . ? C6 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N1 C9 C10 111.80(18) . . ? N1 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N1 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? O10 C10 O5 123.7(2) . . ? O10 C10 C9 118.7(2) . . ? O5 C10 C9 117.56(19) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.603 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.081 _database_code_depnum_ccdc_archive 'CCDC 939972' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_th2al6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 Al6 N8 O67 Th2' _chemical_formula_weight 2074.43 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 '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 10.9899(12) _cell_length_b 11.6107(12) _cell_length_c 14.3350(17) _cell_angle_alpha 73.012(4) _cell_angle_beta 87.411(4) _cell_angle_gamma 75.717(4) _cell_volume 1694.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5979 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 23.80 _exptl_crystal_description blocky _exptl_crystal_colour clear _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.033 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 994 _exptl_absorpt_coefficient_mu 4.600 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7698 _exptl_absorpt_correction_T_max 0.9774 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 KappaCCD _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32516 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.09 _reflns_number_total 5989 _reflns_number_gt 5034 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'APEX2 (Bruker AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalMaker v2.5.0' _computing_publication_material 'enCIFer 1.4' _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^)+(0.0505P)^2^+3.4849P] 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 5989 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _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 Th1 Th 0.29193(2) 0.30672(2) 0.323060(19) 0.01682(9) Uani 1 1 d . . . Al1 Al 0.01512(17) 0.48456(17) 0.39829(14) 0.0155(4) Uani 1 1 d . . . Al2 Al 0.23050(17) 0.39111(18) 0.54638(15) 0.0162(4) Uani 1 1 d . . . Al3 Al 0.14940(19) 0.27852(19) 0.78821(15) 0.0195(4) Uani 1 1 d . . . O1 O 0.1891(4) 0.4830(4) 0.4088(3) 0.0155(10) Uani 1 1 d . . . O2 O 0.2467(4) 0.2876(4) 0.6778(3) 0.0217(10) Uani 1 1 d . . . O3 O 0.2980(4) 0.2629(4) 0.4955(3) 0.0184(10) Uani 1 1 d . . . O4 O 0.1497(4) 0.5290(4) 0.5857(3) 0.0169(10) Uani 1 1 d . . . O5 O -0.0114(4) 0.6063(4) 0.2791(3) 0.0193(10) Uani 1 1 d . . . O6 O 0.0727(4) 0.3517(4) 0.3497(3) 0.0185(10) Uani 1 1 d . . . O7 O 0.0947(5) 0.1401(4) 0.7732(4) 0.0295(12) Uani 1 1 d . . . O8 O 0.2177(4) 0.4011(4) 0.8217(4) 0.0252(11) Uani 1 1 d . . . O9 O 0.1855(4) 0.2785(4) 0.1870(4) 0.0263(11) Uani 1 1 d . . . O10 O 0.4962(4) 0.1682(4) 0.3856(4) 0.0255(11) Uani 1 1 d . . . O11 O -0.0547(4) 0.6118(4) 0.4638(3) 0.0161(10) Uani 1 1 d . . . O12 O 0.4351(4) 0.4334(4) 0.3295(4) 0.0239(11) Uani 1 1 d . . . O13 O 0.6093(5) 0.5004(5) 0.2953(4) 0.0322(13) Uani 1 1 d . . . O14 O 0.3873(4) 0.4311(4) 0.5489(3) 0.0219(11) Uani 1 1 d . . . O15 O 0.2279(5) 0.0998(4) 0.3953(4) 0.0272(11) Uani 1 1 d . . . O16 O 0.2057(4) 0.5084(4) 0.2036(3) 0.0230(11) Uani 1 1 d . . . O17 O 0.1702(5) 0.6325(6) 0.0520(4) 0.0444(16) Uani 1 1 d . . . O18 O 0.0563(4) 0.2654(4) 0.9071(4) 0.0270(11) Uani 1 1 d . . . O19 O 0.2820(5) 0.1527(5) 0.8692(4) 0.0316(13) Uani 1 1 d . . . O20 O 0.1291(6) 0.1778(5) 0.0937(4) 0.0416(15) Uani 1 1 d . . . O21 O 0.6361(5) -0.0140(5) 0.4353(4) 0.0385(14) Uani 1 1 d . . . O22 O 0.5169(6) 0.2208(6) 0.7590(5) 0.0457(15) Uani 1 1 d . . . O23 O 0.6631(6) 0.2358(6) 0.8466(5) 0.0578(18) Uani 1 1 d . . . O24 O -0.0234(8) 0.1472(9) 0.3269(6) 0.082(3) Uani 1 1 d . . . O25 O -0.1880(9) 0.2505(8) 0.3792(9) 0.103(3) Uani 1 1 d . . . O26 O -0.1148(12) 0.0570(10) 0.4504(9) 0.133(4) Uani 1 1 d . . . O27 O 0.4986(6) 0.1858(8) 0.9140(5) 0.065(2) Uani 1 1 d . . . O28 O 0.6032(6) 0.2578(6) 0.5124(5) 0.0492(16) Uani 1 1 d . . . O29 O 0.0537(6) 0.5578(6) 0.8980(5) 0.0541(18) Uani 1 1 d . . . O30 O -0.0116(5) 0.1674(5) 0.6024(4) 0.0387(14) Uani 1 1 d . . . O31 O 0.2452(5) 0.7186(5) 0.3457(4) 0.0425(15) Uani 1 1 d . . . O32 O 0.2421(7) -0.0694(6) 0.9620(6) 0.070(2) Uani 1 1 d . . . O33 O -0.1793(10) 0.2053(10) 1.1453(8) 0.037(3) Uiso 0.50 1 d P . . O34A O -0.0293(16) 0.0093(15) 0.9101(12) 0.063(4) Uiso 0.50 1 d P . . O34B O -0.0807(15) 0.0554(14) 0.8804(11) 0.057(4) Uiso 0.50 1 d P . . N1 N 0.4094(6) 0.1152(5) 0.2372(4) 0.0271(14) Uani 1 1 d . . . N2 N 0.4360(5) 0.3777(5) 0.1577(4) 0.0227(13) Uani 1 1 d . . . N3 N 0.5578(6) 0.2162(6) 0.8384(6) 0.0374(17) Uani 1 1 d . . . N4 N -0.1115(10) 0.1548(9) 0.3811(9) 0.075(3) Uani 1 1 d . . . C1 C 0.5450(7) 0.0563(7) 0.3836(5) 0.0260(17) Uani 1 1 d . . . C2 C 0.5293(6) 0.4479(6) 0.2792(5) 0.0217(15) Uani 1 1 d . . . C3 C 0.2013(7) 0.1861(7) 0.1540(5) 0.0262(17) Uani 1 1 d . . . C4 C 0.4829(7) 0.0102(7) 0.3149(6) 0.0318(18) Uani 1 1 d . . . H4A H 0.5465 -0.0418 0.2857 0.038 Uiso 1 1 calc R . . H4B H 0.4278 -0.0398 0.3510 0.038 Uiso 1 1 calc R . . C5 C 0.2374(7) 0.5487(7) 0.1170(6) 0.0275(17) Uani 1 1 d . . . C6 C 0.3128(7) 0.0789(7) 0.1934(6) 0.0325(19) Uani 1 1 d . . . H6A H 0.2849 0.0137 0.2421 0.039 Uiso 1 1 calc R . . H6B H 0.3488 0.0458 0.1408 0.039 Uiso 1 1 calc R . . C7 C 0.4602(8) 0.2855(8) 0.1031(6) 0.039(2) Uani 1 1 d . . . H7A H 0.5248 0.3025 0.0563 0.047 Uiso 1 1 calc R . . H7B H 0.3843 0.2947 0.0667 0.047 Uiso 1 1 calc R . . C8 C 0.5007(9) 0.1555(7) 0.1654(7) 0.042(2) Uani 1 1 d . . . H8A H 0.5183 0.1012 0.1237 0.050 Uiso 1 1 calc R . . H8B H 0.5784 0.1457 0.1996 0.050 Uiso 1 1 calc R . . C9 C 0.5523(8) 0.3914(9) 0.1944(6) 0.039(2) Uani 1 1 d . . . H9A H 0.5902 0.4439 0.1419 0.047 Uiso 1 1 calc R . . H9B H 0.6109 0.3106 0.2157 0.047 Uiso 1 1 calc R . . C10 C 0.3704(8) 0.4987(8) 0.0924(6) 0.042(2) Uani 1 1 d . . . H10A H 0.3704 0.4917 0.0266 0.051 Uiso 1 1 calc R . . H10B H 0.4180 0.5588 0.0923 0.051 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 Th1 0.01254(13) 0.01965(14) 0.01688(14) -0.00615(10) -0.00053(9) -0.00022(9) Al1 0.0125(10) 0.0170(10) 0.0149(10) -0.0040(8) -0.0008(8) -0.0006(8) Al2 0.0115(10) 0.0187(10) 0.0169(11) -0.0054(8) -0.0009(8) -0.0006(8) Al3 0.0154(10) 0.0212(11) 0.0179(11) -0.0025(9) -0.0028(8) -0.0004(8) O1 0.013(2) 0.017(2) 0.014(2) -0.0027(19) -0.0008(18) -0.0002(18) O2 0.020(3) 0.025(3) 0.019(3) -0.006(2) -0.001(2) -0.003(2) O3 0.019(2) 0.017(2) 0.017(3) -0.0059(19) -0.0029(19) 0.0031(19) O4 0.010(2) 0.020(2) 0.020(3) -0.008(2) -0.0016(18) 0.0001(18) O5 0.015(2) 0.025(3) 0.013(2) -0.004(2) -0.0019(19) 0.0021(19) O6 0.011(2) 0.021(2) 0.022(3) -0.007(2) 0.0007(19) 0.0007(19) O7 0.031(3) 0.024(3) 0.031(3) -0.005(2) -0.003(2) -0.005(2) O8 0.025(3) 0.032(3) 0.023(3) -0.012(2) -0.001(2) -0.009(2) O9 0.025(3) 0.026(3) 0.027(3) -0.012(2) -0.003(2) 0.000(2) O10 0.019(3) 0.024(3) 0.030(3) -0.011(2) -0.006(2) 0.008(2) O11 0.012(2) 0.020(2) 0.016(2) -0.007(2) -0.0021(18) -0.0008(19) O12 0.019(3) 0.030(3) 0.027(3) -0.013(2) 0.001(2) -0.008(2) O13 0.024(3) 0.047(3) 0.036(3) -0.020(3) 0.005(2) -0.017(2) O14 0.011(2) 0.028(3) 0.025(3) -0.005(2) 0.001(2) -0.005(2) O15 0.028(3) 0.022(3) 0.030(3) -0.005(2) 0.001(2) -0.005(2) O16 0.021(3) 0.025(3) 0.018(3) -0.003(2) 0.006(2) -0.002(2) O17 0.028(3) 0.054(4) 0.027(3) 0.009(3) 0.002(3) 0.008(3) O18 0.024(3) 0.030(3) 0.023(3) -0.003(2) 0.002(2) -0.004(2) O19 0.020(3) 0.034(3) 0.029(3) 0.002(2) -0.008(2) 0.004(2) O20 0.049(4) 0.042(3) 0.035(3) -0.013(3) -0.019(3) -0.005(3) O21 0.035(3) 0.031(3) 0.043(4) -0.010(3) -0.014(3) 0.007(3) O22 0.041(4) 0.056(4) 0.042(4) -0.016(3) -0.008(3) -0.012(3) O23 0.045(4) 0.073(5) 0.061(5) -0.013(4) -0.010(3) -0.029(3) O24 0.055(5) 0.113(7) 0.081(6) -0.018(5) 0.020(4) -0.038(5) O25 0.085(7) 0.055(5) 0.173(11) -0.047(6) -0.021(6) -0.004(5) O26 0.154(11) 0.092(8) 0.132(10) -0.002(7) 0.050(8) -0.036(7) O27 0.040(4) 0.127(7) 0.038(4) -0.034(4) 0.003(3) -0.026(4) O28 0.044(4) 0.061(4) 0.045(4) -0.024(3) -0.013(3) -0.005(3) O29 0.051(4) 0.053(4) 0.060(4) -0.033(3) -0.009(3) 0.008(3) O30 0.045(4) 0.034(3) 0.038(3) -0.005(3) -0.006(3) -0.016(3) O31 0.034(3) 0.045(4) 0.050(4) -0.010(3) -0.001(3) -0.015(3) O32 0.078(5) 0.052(4) 0.068(5) 0.008(4) -0.013(4) -0.019(4) N1 0.028(3) 0.025(3) 0.025(4) -0.007(3) -0.003(3) -0.002(3) N2 0.020(3) 0.026(3) 0.022(3) -0.010(3) 0.004(2) -0.004(3) N3 0.027(4) 0.039(4) 0.048(5) -0.015(4) -0.006(4) -0.007(3) N4 0.064(7) 0.054(6) 0.115(9) -0.019(6) 0.014(6) -0.036(5) C1 0.023(4) 0.027(4) 0.024(4) -0.005(3) 0.002(3) -0.002(3) C2 0.015(4) 0.021(4) 0.028(4) -0.006(3) -0.005(3) -0.003(3) C3 0.036(4) 0.026(4) 0.017(4) -0.006(3) -0.001(3) -0.008(3) C4 0.029(4) 0.026(4) 0.034(5) -0.010(4) 0.001(3) 0.004(3) C5 0.023(4) 0.032(4) 0.026(4) -0.006(4) 0.002(3) -0.007(3) C6 0.035(5) 0.028(4) 0.034(5) -0.014(4) -0.008(4) 0.001(3) C7 0.040(5) 0.045(5) 0.032(5) -0.015(4) 0.013(4) -0.009(4) C8 0.051(6) 0.029(5) 0.045(5) -0.013(4) 0.020(4) -0.010(4) C9 0.031(5) 0.061(6) 0.037(5) -0.025(4) 0.013(4) -0.020(4) C10 0.032(5) 0.044(5) 0.036(5) -0.003(4) 0.014(4) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 O6 2.374(4) . ? Th1 O3 2.374(4) . ? Th1 O12 2.426(5) . ? Th1 O10 2.447(4) . ? Th1 O16 2.454(5) . ? Th1 O9 2.460(5) . ? Th1 O15 2.579(5) . ? Th1 O1 2.680(4) . ? Th1 N2 2.822(6) . ? Th1 N1 2.857(6) . ? Th1 Al1 3.5478(19) . ? Al1 O6 1.837(5) . ? Al1 O5 1.853(5) . ? Al1 O4 1.855(5) 2_566 ? Al1 O1 1.920(5) . ? Al1 O11 1.959(5) . ? Al1 O11 1.973(5) 2_566 ? Al1 Al2 2.924(3) 2_566 ? Al2 O3 1.828(5) . ? Al2 O4 1.857(5) . ? Al2 O14 1.896(5) . ? Al2 O2 1.905(5) . ? Al2 O11 1.954(5) 2_566 ? Al2 O1 1.961(5) . ? Al2 Al1 2.924(3) 2_566 ? Al3 O5 1.843(5) 2_566 ? Al3 O2 1.861(5) . ? Al3 O7 1.918(5) . ? Al3 O19 1.928(5) . ? Al3 O18 1.934(5) . ? Al3 O8 1.945(5) . ? O4 Al1 1.855(5) 2_566 ? O5 Al3 1.843(5) 2_566 ? O9 C3 1.265(8) . ? O10 C1 1.286(8) . ? O11 Al2 1.954(5) 2_566 ? O11 Al1 1.973(5) 2_566 ? O12 C2 1.253(8) . ? O13 C2 1.250(8) . ? O16 C5 1.258(9) . ? O17 C5 1.240(9) . ? O20 C3 1.239(9) . ? O21 C1 1.236(9) . ? O22 N3 1.224(9) . ? O23 N3 1.250(9) . ? O24 N4 1.216(12) . ? O25 N4 1.211(12) . ? O26 N4 1.278(13) . ? O27 N3 1.245(9) . ? O34A O34B 0.725(18) . ? N1 C6 1.461(9) . ? N1 C8 1.464(10) . ? N1 C4 1.476(9) . ? N2 C9 1.465(10) . ? N2 C7 1.470(10) . ? N2 C10 1.471(10) . ? C1 C4 1.509(11) . ? C2 C9 1.525(10) . ? C3 C6 1.506(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C10 1.500(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.480(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 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 O6 Th1 O3 81.01(15) . . ? O6 Th1 O12 126.99(15) . . ? O3 Th1 O12 83.66(16) . . ? O6 Th1 O10 145.04(17) . . ? O3 Th1 O10 71.58(15) . . ? O12 Th1 O10 71.80(16) . . ? O6 Th1 O16 75.01(15) . . ? O3 Th1 O16 126.88(15) . . ? O12 Th1 O16 74.79(16) . . ? O10 Th1 O16 139.27(16) . . ? O6 Th1 O9 71.99(16) . . ? O3 Th1 O9 143.17(16) . . ? O12 Th1 O9 132.71(17) . . ? O10 Th1 O9 119.68(15) . . ? O16 Th1 O9 69.78(16) . . ? O6 Th1 O15 71.53(15) . . ? O3 Th1 O15 72.70(15) . . ? O12 Th1 O15 147.60(16) . . ? O10 Th1 O15 79.76(16) . . ? O16 Th1 O15 137.35(16) . . ? O9 Th1 O15 75.22(16) . . ? O6 Th1 O1 60.21(14) . . ? O3 Th1 O1 59.07(13) . . ? O12 Th1 O1 68.35(14) . . ? O10 Th1 O1 118.28(14) . . ? O16 Th1 O1 67.86(14) . . ? O9 Th1 O1 122.03(14) . . ? O15 Th1 O1 114.52(14) . . ? O6 Th1 N2 132.88(16) . . ? O3 Th1 N2 141.46(16) . . ? O12 Th1 N2 61.95(16) . . ? O10 Th1 N2 80.98(17) . . ? O16 Th1 N2 62.90(16) . . ? O9 Th1 N2 74.30(17) . . ? O15 Th1 N2 128.86(16) . . ? O1 Th1 N2 116.37(15) . . ? O6 Th1 N1 121.39(16) . . ? O3 Th1 N1 119.15(16) . . ? O12 Th1 N1 110.42(17) . . ? O10 Th1 N1 59.48(16) . . ? O16 Th1 N1 113.84(16) . . ? O9 Th1 N1 60.22(16) . . ? O15 Th1 N1 65.39(17) . . ? O1 Th1 N1 177.75(15) . . ? N2 Th1 N1 63.96(17) . . ? O6 Th1 Al1 28.17(11) . . ? O3 Th1 Al1 70.42(11) . . ? O12 Th1 Al1 99.15(11) . . ? O10 Th1 Al1 141.68(12) . . ? O16 Th1 Al1 66.12(11) . . ? O9 Th1 Al1 94.21(11) . . ? O15 Th1 Al1 93.54(11) . . ? O1 Th1 Al1 32.25(10) . . ? N2 Th1 Al1 128.62(12) . . ? N1 Th1 Al1 149.47(13) . . ? O6 Al1 O5 96.8(2) . . ? O6 Al1 O4 96.9(2) . 2_566 ? O5 Al1 O4 96.6(2) . 2_566 ? O6 Al1 O1 85.4(2) . . ? O5 Al1 O1 94.0(2) . . ? O4 Al1 O1 168.7(2) 2_566 . ? O6 Al1 O11 172.7(2) . . ? O5 Al1 O11 89.5(2) . . ? O4 Al1 O11 78.69(19) 2_566 . ? O1 Al1 O11 97.86(19) . . ? O6 Al1 O11 95.3(2) . 2_566 ? O5 Al1 O11 165.4(2) . 2_566 ? O4 Al1 O11 90.0(2) 2_566 2_566 ? O1 Al1 O11 78.83(19) . 2_566 ? O11 Al1 O11 79.0(2) . 2_566 ? O6 Al1 Al2 134.72(17) . 2_566 ? O5 Al1 Al2 87.54(15) . 2_566 ? O4 Al1 Al2 38.05(14) 2_566 2_566 ? O1 Al1 Al2 139.42(16) . 2_566 ? O11 Al1 Al2 41.57(13) . 2_566 ? O11 Al1 Al2 89.71(14) 2_566 2_566 ? O6 Al1 Th1 37.60(14) . . ? O5 Al1 Th1 93.40(15) . . ? O4 Al1 Th1 134.31(15) 2_566 . ? O1 Al1 Th1 48.15(13) . . ? O11 Al1 Th1 145.99(15) . . ? O11 Al1 Th1 91.24(13) 2_566 . ? Al2 Al1 Th1 172.32(8) 2_566 . ? O3 Al2 O4 173.5(2) . . ? O3 Al2 O14 92.6(2) . . ? O4 Al2 O14 90.8(2) . . ? O3 Al2 O2 94.0(2) . . ? O4 Al2 O2 91.2(2) . . ? O14 Al2 O2 94.5(2) . . ? O3 Al2 O11 97.1(2) . 2_566 ? O4 Al2 O11 78.77(19) . 2_566 ? O14 Al2 O11 167.8(2) . 2_566 ? O2 Al2 O11 92.2(2) . 2_566 ? O3 Al2 O1 82.7(2) . . ? O4 Al2 O1 91.5(2) . . ? O14 Al2 O1 95.7(2) . . ? O2 Al2 O1 169.4(2) . . ? O11 Al2 O1 78.31(19) 2_566 . ? O3 Al2 Al1 138.63(17) . 2_566 ? O4 Al2 Al1 38.00(14) . 2_566 ? O14 Al2 Al1 128.69(17) . 2_566 ? O2 Al2 Al1 85.52(15) . 2_566 ? O11 Al2 Al1 41.71(13) 2_566 2_566 ? O1 Al2 Al1 90.28(14) . 2_566 ? O5 Al3 O2 93.8(2) 2_566 . ? O5 Al3 O7 93.5(2) 2_566 . ? O2 Al3 O7 92.3(2) . . ? O5 Al3 O19 174.0(2) 2_566 . ? O2 Al3 O19 91.9(2) . . ? O7 Al3 O19 84.4(2) . . ? O5 Al3 O18 89.1(2) 2_566 . ? O2 Al3 O18 177.0(2) . . ? O7 Al3 O18 88.5(2) . . ? O19 Al3 O18 85.3(2) . . ? O5 Al3 O8 94.2(2) 2_566 . ? O2 Al3 O8 91.4(2) . . ? O7 Al3 O8 171.2(2) . . ? O19 Al3 O8 87.5(2) . . ? O18 Al3 O8 87.4(2) . . ? Al1 O1 Al2 102.2(2) . . ? Al1 O1 Th1 99.60(18) . . ? Al2 O1 Th1 100.67(17) . . ? Al3 O2 Al2 135.7(3) . . ? Al2 O3 Th1 117.4(2) . . ? Al1 O4 Al2 103.9(2) 2_566 . ? Al3 O5 Al1 135.1(3) 2_566 . ? Al1 O6 Th1 114.2(2) . . ? C3 O9 Th1 130.7(4) . . ? C1 O10 Th1 130.2(4) . . ? Al2 O11 Al1 96.7(2) 2_566 . ? Al2 O11 Al1 100.6(2) 2_566 2_566 ? Al1 O11 Al1 101.0(2) . 2_566 ? C2 O12 Th1 128.7(4) . . ? C5 O16 Th1 128.6(4) . . ? C6 N1 C8 111.4(7) . . ? C6 N1 C4 111.7(6) . . ? C8 N1 C4 105.7(6) . . ? C6 N1 Th1 109.1(4) . . ? C8 N1 Th1 111.1(4) . . ? C4 N1 Th1 107.8(4) . . ? C9 N2 C7 112.0(6) . . ? C9 N2 C10 108.2(6) . . ? C7 N2 C10 108.7(6) . . ? C9 N2 Th1 106.1(4) . . ? C7 N2 Th1 111.2(4) . . ? C10 N2 Th1 110.5(4) . . ? O22 N3 O27 120.9(7) . . ? O22 N3 O23 120.9(8) . . ? O27 N3 O23 118.0(7) . . ? O25 N4 O24 124.3(11) . . ? O25 N4 O26 118.5(12) . . ? O24 N4 O26 116.8(11) . . ? O21 C1 O10 124.1(7) . . ? O21 C1 C4 119.6(6) . . ? O10 C1 C4 116.3(6) . . ? O13 C2 O12 125.2(7) . . ? O13 C2 C9 117.1(6) . . ? O12 C2 C9 117.6(6) . . ? O20 C3 O9 123.9(7) . . ? O20 C3 C6 118.7(6) . . ? O9 C3 C6 117.4(6) . . ? N1 C4 C1 110.8(6) . . ? N1 C4 H4A 109.5 . . ? C1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? O17 C5 O16 125.2(7) . . ? O17 C5 C10 117.2(7) . . ? O16 C5 C10 117.4(7) . . ? N1 C6 C3 112.3(6) . . ? N1 C6 H6A 109.1 . . ? C3 C6 H6A 109.1 . . ? N1 C6 H6B 109.1 . . ? C3 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 113.8(7) . . ? N2 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N2 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C7 114.7(7) . . ? N1 C8 H8A 108.6 . . ? C7 C8 H8A 108.6 . . ? N1 C8 H8B 108.6 . . ? C7 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? N2 C9 C2 112.0(6) . . ? N2 C9 H9A 109.2 . . ? C2 C9 H9A 109.2 . . ? N2 C9 H9B 109.2 . . ? C2 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? N2 C10 C5 115.9(7) . . ? N2 C10 H10A 108.3 . . ? C5 C10 H10A 108.3 . . ? N2 C10 H10B 108.3 . . ? C5 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.967 _refine_diff_density_min -1.296 _refine_diff_density_rms 0.177 _database_code_depnum_ccdc_archive 'CCDC 939973' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety '[Th4(H2O)4Al10(H2O)8(OH)28(C10H12N2O8)4]?(H2O)32 ' _chemical_formula_sum 'C40 H48 Al10 N8 O103.50 Th4' _chemical_melting_point ? _exptl_crystal_description blocky _exptl_crystal_colour clear _diffrn_ambient_temperature 483(2) _chemical_formula_weight 3494.82 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 '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' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3172(8) _cell_length_b 16.6099(14) _cell_length_c 19.5080(14) _cell_angle_alpha 102.314(3) _cell_angle_beta 95.615(3) _cell_angle_gamma 92.473(3) _cell_volume 2929.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 483(2) _cell_measurement_reflns_used 9844 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 26.20 _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1662 _exptl_absorpt_coefficient_mu 5.268 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6469 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 70550 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 26.37 _reflns_number_total 11946 _reflns_number_gt 9744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'APEX2 (Bruker AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalMaker v2.5.0' _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^)+(0.0473P)^2^+22.2448P] 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 11946 _refine_ls_number_parameters 693 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Th1 Th 0.47918(3) 0.367984(15) 0.144704(11) 0.01987(7) Uani 1 1 d . . . Th2 Th 0.48039(3) 0.801045(14) 0.307633(12) 0.01974(7) Uani 1 1 d . . . Al1 Al 0.4562(2) 0.57642(12) 0.24692(10) 0.0181(4) Uani 1 1 d . . . Al2 Al 0.7247(2) 0.52567(12) 0.47163(10) 0.0172(4) Uani 1 1 d . . . Al3 Al 0.6050(2) 0.45851(12) 0.32387(9) 0.0174(4) Uani 1 1 d . . . Al4 Al 0.5968(2) 0.64189(12) 0.39490(10) 0.0180(4) Uani 1 1 d . . . Al5 Al 0.5102(2) 0.34283(12) 0.44038(10) 0.0188(4) Uani 1 1 d . . . O1 O 0.5366(5) 0.3652(3) 0.3519(2) 0.0191(9) Uani 1 1 d . . . O2 O 0.6340(5) 0.5820(3) 0.5482(2) 0.0212(10) Uani 1 1 d . . . O3 O 0.7809(5) 0.4668(3) 0.3821(2) 0.0190(9) Uani 1 1 d . . . O4 O 0.5499(5) 0.5307(3) 0.4087(2) 0.0179(9) Uani 1 1 d . . . O5 O 0.7685(5) 0.6225(3) 0.4411(2) 0.0211(10) Uani 1 1 d . . . O6 O 0.5024(5) 0.5140(3) 0.1625(2) 0.0199(10) Uani 1 1 d . . . O7 O 0.6571(5) 0.4227(3) 0.4854(2) 0.0199(9) Uani 1 1 d . . . O8 O 0.7080(5) 0.3992(3) 0.0935(3) 0.0302(11) Uani 1 1 d . . . O9 O 0.6654(5) 0.4029(3) 0.2413(2) 0.0214(10) Uani 1 1 d . . . O10 O 0.4034(6) 0.3906(3) 0.0277(2) 0.0321(12) Uani 1 1 d . . . O11 O 0.6566(5) 0.2585(3) 0.4218(2) 0.0250(10) Uani 1 1 d . . . O12 O 0.8976(5) 0.5293(3) 0.5265(2) 0.0245(10) Uani 1 1 d . . . O13 O 0.6398(5) 0.5690(3) 0.3031(2) 0.0181(9) Uani 1 1 d . . . O14 O 0.4253(5) 0.6444(3) 0.3356(2) 0.0193(9) Uani 1 1 d . . . O15 O 0.6604(5) 0.7362(3) 0.3701(2) 0.0223(10) Uani 1 1 d . . . O16 O 0.4292(5) 0.4694(3) 0.2691(2) 0.0191(9) Uani 1 1 d . . . O17 O 0.4850(5) 0.3105(3) 0.5244(2) 0.0202(10) Uani 1 1 d . . . O18 O 0.2521(5) 0.5720(3) 0.2188(3) 0.0295(11) Uani 1 1 d . . . O19 O 0.4980(5) 0.6757(3) 0.2226(2) 0.0219(10) Uani 1 1 d . . . O20 O 0.3662(6) 0.2533(3) 0.3935(2) 0.0283(11) Uani 1 1 d . . . O21 O 0.6307(6) 0.9014(3) 0.4027(3) 0.0301(11) Uani 1 1 d . . . O22 O 0.3746(5) 0.2933(3) 0.2238(2) 0.0276(11) Uani 1 1 d . . . O23 O 0.7202(6) 0.8116(3) 0.2561(3) 0.0325(12) Uani 1 1 d . . . O24 O 0.4027(6) 0.8406(3) 0.2001(3) 0.0357(13) Uani 1 1 d . . . O25 O 0.6198(6) 0.2484(3) 0.1574(3) 0.0333(12) Uani 1 1 d . . . O26 O 0.2318(5) 0.4152(3) 0.1488(3) 0.0313(12) Uani 1 1 d . . . O27 O 0.3812(6) 0.8057(3) 0.4182(2) 0.0278(11) Uani 1 1 d . . . O28 O 0.2273(6) 0.7499(3) 0.2790(3) 0.0322(12) Uani 1 1 d . . . O29 O 0.3144(8) 0.8706(3) 0.5201(3) 0.0452(16) Uani 1 1 d . . . O30 O 0.3817(6) 0.3727(4) -0.0890(3) 0.0403(14) Uani 1 1 d . . . O31 O 0.8512(6) 0.9624(4) 0.4258(3) 0.0453(15) Uani 1 1 d . . . O32 O -0.0072(7) 0.7521(4) 0.2932(4) 0.0580(19) Uani 1 1 d . . . O33 O 0.8186(7) 0.1832(4) 0.1332(3) 0.0473(15) Uani 1 1 d . . . O34 O 0.2335(8) 0.2047(4) 0.2605(3) 0.058(2) Uani 1 1 d . . . O35 O 0.3664(9) 0.9155(4) 0.1200(3) 0.061(2) Uani 1 1 d . . . O36 O -0.0060(7) 0.4096(5) 0.1391(4) 0.071(2) Uani 1 1 d . . . O37 O 0.8838(7) 0.9168(4) 0.1678(3) 0.014(2) Uiso 0.634(16) 1 d P A 1 O38 O 0.8416(16) 0.8577(9) 0.1528(8) 0.033(5) Uiso 0.366(16) 1 d P A 2 O39 O -0.020(3) 0.4097(16) -0.0877(14) 0.051(6) Uiso 0.25 1 d P . . O40 O 0.919(2) 0.0352(12) 0.0636(11) 0.029(4) Uiso 0.25 1 d P . . O41 O 0.8152(6) 0.3649(4) 0.5923(3) 0.0432(14) Uiso 1 1 d . . . O42 O 0.1965(6) 0.4106(3) 0.3209(3) 0.0373(13) Uiso 1 1 d . . . O43 O 0.6827(7) 0.1852(4) 0.2840(3) 0.0439(14) Uiso 1 1 d . . . O44 O 1.0577(7) 0.6743(4) 0.6020(3) 0.0487(15) Uiso 1 1 d . . . O45 O 0.2913(7) 0.1435(4) 0.4665(4) 0.0527(16) Uiso 1 1 d . . . O46 O 1.0014(7) 0.5204(4) 0.3232(3) 0.0515(16) Uiso 1 1 d . . . O47 O 0.9294(7) 0.3114(4) 0.2491(3) 0.0506(16) Uiso 1 1 d . . . O48 O -0.0286(9) 0.1198(5) 0.2783(4) 0.068(2) Uiso 1 1 d . . . O49 O 1.0035(8) 1.1085(5) 0.4238(4) 0.067(2) Uiso 1 1 d . . . O50 O 0.7363(9) 0.4625(5) -0.0190(4) 0.071(2) Uiso 1 1 d . . . O51 O -0.1277(8) 0.6029(5) 0.2328(4) 0.067(2) Uiso 1 1 d . . . O52 O 1.0083(9) 0.2418(5) 0.5485(5) 0.078(2) Uiso 1 1 d . . . O53 O 0.1536(14) 0.6536(8) 0.1166(7) 0.047(3) Uiso 0.50 1 d P . . O54 O 0.1070(17) 0.8063(11) 0.0983(8) 0.066(4) Uiso 0.50 1 d P . . O55 O 0.1065(17) 0.4209(10) -0.0934(8) 0.068(4) Uiso 0.50 1 d P . . O56 O 0.795(4) -0.008(2) -0.0482(17) 0.072(9) Uiso 0.25 1 d P . . O57 O 0.901(3) 1.0136(16) 0.1526(14) 0.052(6) Uiso 0.25 1 d P . . O58 O -0.096(3) 0.237(2) -0.1109(17) 0.065(8) Uiso 0.25 1 d P . . N1 N 0.5538(7) 0.9663(4) 0.2948(3) 0.0294(14) Uani 1 1 d . . . N2 N 0.2754(7) 0.9163(4) 0.3453(3) 0.0276(13) Uani 1 1 d . . . N3 N 0.2382(7) 0.2517(4) 0.0874(3) 0.0329(15) Uani 1 1 d . . . N4 N 0.5242(8) 0.2446(4) 0.0247(3) 0.0365(16) Uani 1 1 d . . . C1 C 0.1088(8) 0.3785(5) 0.1250(4) 0.0354(18) Uani 1 1 d . . . C2 C 0.7322(9) 0.9495(4) 0.3913(4) 0.0302(16) Uani 1 1 d . . . C3 C 0.1144(9) 0.7868(5) 0.2952(4) 0.0356(18) Uani 1 1 d . . . C4 C 0.3272(8) 0.8663(4) 0.4566(4) 0.0282(16) Uani 1 1 d . . . C5 C 0.4261(9) 0.3518(5) -0.0339(4) 0.0325(17) Uani 1 1 d . . . C6 C 0.7063(9) 0.2131(5) 0.1148(4) 0.0325(17) Uani 1 1 d . . . C7 C 0.2782(9) 0.2346(5) 0.2129(4) 0.0343(18) Uani 1 1 d . . . C8 C 0.4275(10) 0.9054(5) 0.1767(4) 0.0363(19) Uani 1 1 d . . . C9 C 0.6999(9) 0.9892(5) 0.3284(4) 0.0322(17) Uani 1 1 d . . . H9A H 0.7126 1.0487 0.3441 0.039 Uiso 1 1 calc R . . H9B H 0.7678 0.9719 0.2943 0.039 Uiso 1 1 calc R . . C10 C 0.2846(10) 0.9373(5) 0.4244(4) 0.0373(19) Uani 1 1 d . . . H10A H 0.3548 0.9837 0.4425 0.045 Uiso 1 1 calc R . . H10B H 0.1915 0.9541 0.4385 0.045 Uiso 1 1 calc R . . C11 C 0.6685(9) 0.2138(5) 0.0381(4) 0.0379(19) Uani 1 1 d . . . H11A H 0.7405 0.2486 0.0234 0.046 Uiso 1 1 calc R . . H11B H 0.6705 0.1583 0.0099 0.046 Uiso 1 1 calc R . . C12 C 0.5374(10) 0.9688(5) 0.2188(4) 0.040(2) Uani 1 1 d . . . H12A H 0.5095 1.0231 0.2139 0.048 Uiso 1 1 calc R . . H12B H 0.6297 0.9601 0.2003 0.048 Uiso 1 1 calc R . . C13 C 0.2181(11) 0.1980(6) 0.1377(4) 0.049(2) Uani 1 1 d . . . H13A H 0.2636 0.1469 0.1218 0.059 Uiso 1 1 calc R . . H13B H 0.1155 0.1843 0.1365 0.059 Uiso 1 1 calc R . . C14 C 0.5149(10) 0.2785(6) -0.0395(4) 0.043(2) Uani 1 1 d . . . H14A H 0.4732 0.2358 -0.0794 0.051 Uiso 1 1 calc R . . H14B H 0.6117 0.2941 -0.0485 0.051 Uiso 1 1 calc R . . C15 C 0.1287(9) 0.8795(5) 0.3152(5) 0.044(2) Uani 1 1 d . . . H15A H 0.0999 0.9006 0.2736 0.053 Uiso 1 1 calc R . . H15B H 0.0616 0.8979 0.3494 0.053 Uiso 1 1 calc R . . C16 C 0.1061(9) 0.2966(6) 0.0781(5) 0.045(2) Uani 1 1 d . . . H16A H 0.0919 0.3028 0.0296 0.055 Uiso 1 1 calc R . . H16B H 0.0237 0.2633 0.0860 0.055 Uiso 1 1 calc R . . C17 C 0.3004(8) 0.9930(5) 0.3198(4) 0.0301(16) Uani 1 1 d . . . H17A H 0.2426 1.0353 0.3436 0.036 Uiso 1 1 calc R . . H17B H 0.2695 0.9827 0.2696 0.036 Uiso 1 1 calc R . . C18 C 0.4570(9) 1.0237(5) 0.3332(4) 0.0335(18) Uani 1 1 d . . . H18A H 0.4670 1.0763 0.3194 0.040 Uiso 1 1 calc R . . H18B H 0.4875 1.0331 0.3834 0.040 Uiso 1 1 calc R . . C19 C 0.2643(10) 0.2003(6) 0.0173(4) 0.040(2) Uani 1 1 d . . . H19A H 0.1977 0.1516 0.0057 0.048 Uiso 1 1 calc R . . H19B H 0.2457 0.2318 -0.0188 0.048 Uiso 1 1 calc R . . C20 C 0.4162(10) 0.1742(6) 0.0176(5) 0.048(2) Uani 1 1 d . . . H20A H 0.4371 0.1471 0.0565 0.058 Uiso 1 1 calc R . . H20B H 0.4247 0.1345 -0.0259 0.058 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 Th1 0.02601(14) 0.02177(13) 0.01071(12) 0.00086(9) 0.00322(9) -0.00004(10) Th2 0.02630(14) 0.01897(13) 0.01421(12) 0.00317(9) 0.00394(9) 0.00271(10) Al1 0.0240(10) 0.0194(10) 0.0109(9) 0.0026(7) 0.0032(7) 0.0019(8) Al2 0.0211(10) 0.0182(10) 0.0122(9) 0.0032(7) 0.0021(7) 0.0008(8) Al3 0.0244(10) 0.0171(9) 0.0106(9) 0.0020(7) 0.0033(7) 0.0009(8) Al4 0.0247(10) 0.0178(10) 0.0117(9) 0.0032(7) 0.0029(7) 0.0019(8) Al5 0.0278(11) 0.0173(9) 0.0111(9) 0.0018(7) 0.0042(8) 0.0012(8) O1 0.029(3) 0.018(2) 0.011(2) 0.0038(17) 0.0028(18) 0.0002(19) O2 0.026(2) 0.023(2) 0.014(2) 0.0035(18) 0.0013(18) 0.0040(19) O3 0.022(2) 0.021(2) 0.013(2) 0.0009(18) 0.0021(17) 0.0001(18) O4 0.024(2) 0.017(2) 0.011(2) 0.0008(17) -0.0004(17) -0.0003(18) O5 0.025(2) 0.021(2) 0.018(2) 0.0058(18) 0.0024(18) 0.0017(19) O6 0.025(2) 0.026(2) 0.009(2) 0.0025(18) 0.0038(17) 0.0035(19) O7 0.027(2) 0.019(2) 0.014(2) 0.0049(18) 0.0006(18) 0.0002(19) O8 0.025(3) 0.045(3) 0.022(3) 0.008(2) 0.007(2) 0.001(2) O9 0.026(2) 0.026(2) 0.011(2) 0.0003(18) 0.0033(18) 0.002(2) O10 0.039(3) 0.044(3) 0.012(2) 0.004(2) 0.003(2) 0.003(2) O11 0.033(3) 0.022(2) 0.023(2) 0.007(2) 0.009(2) 0.006(2) O12 0.023(2) 0.033(3) 0.017(2) 0.005(2) -0.0008(19) 0.002(2) O13 0.023(2) 0.018(2) 0.012(2) 0.0023(17) 0.0011(17) -0.0009(18) O14 0.026(2) 0.019(2) 0.012(2) 0.0017(17) 0.0012(18) 0.0045(19) O15 0.031(3) 0.023(2) 0.015(2) 0.0084(19) 0.0041(19) 0.002(2) O16 0.025(2) 0.020(2) 0.011(2) 0.0008(17) 0.0020(17) -0.0010(18) O17 0.031(3) 0.018(2) 0.013(2) 0.0035(17) 0.0064(18) 0.0030(19) O18 0.024(3) 0.036(3) 0.027(3) 0.003(2) 0.001(2) 0.003(2) O19 0.034(3) 0.016(2) 0.016(2) 0.0033(18) 0.0039(19) 0.0025(19) O20 0.040(3) 0.022(3) 0.021(2) 0.003(2) 0.000(2) -0.011(2) O21 0.043(3) 0.024(3) 0.023(3) 0.006(2) 0.000(2) -0.005(2) O22 0.032(3) 0.031(3) 0.018(2) 0.002(2) 0.002(2) -0.009(2) O23 0.032(3) 0.039(3) 0.030(3) 0.012(2) 0.010(2) 0.002(2) O24 0.056(4) 0.035(3) 0.017(2) 0.007(2) 0.002(2) 0.007(3) O25 0.047(3) 0.031(3) 0.023(3) 0.003(2) 0.013(2) 0.011(2) O26 0.026(3) 0.037(3) 0.027(3) 0.001(2) 0.000(2) -0.001(2) O27 0.045(3) 0.025(3) 0.017(2) 0.006(2) 0.011(2) 0.010(2) O28 0.030(3) 0.034(3) 0.032(3) 0.004(2) 0.005(2) 0.007(2) O29 0.085(5) 0.032(3) 0.026(3) 0.011(2) 0.023(3) 0.023(3) O30 0.050(4) 0.054(4) 0.016(3) 0.010(2) 0.003(2) -0.003(3) O31 0.038(3) 0.049(4) 0.044(4) 0.006(3) -0.005(3) -0.003(3) O32 0.032(3) 0.045(4) 0.099(6) 0.018(4) 0.013(3) 0.006(3) O33 0.050(4) 0.051(4) 0.038(3) 0.001(3) 0.005(3) 0.020(3) O34 0.067(5) 0.076(5) 0.027(3) 0.014(3) -0.001(3) -0.044(4) O35 0.101(6) 0.055(4) 0.026(3) 0.014(3) -0.011(3) 0.019(4) O36 0.031(4) 0.074(5) 0.093(6) -0.013(4) 0.000(4) 0.002(3) N1 0.042(4) 0.024(3) 0.022(3) 0.002(2) 0.010(3) 0.001(3) N2 0.036(3) 0.025(3) 0.025(3) 0.007(2) 0.009(3) 0.011(3) N3 0.046(4) 0.032(4) 0.016(3) -0.001(3) 0.001(3) -0.008(3) N4 0.045(4) 0.047(4) 0.015(3) 0.000(3) 0.006(3) 0.004(3) C1 0.024(4) 0.051(5) 0.031(4) 0.007(4) 0.003(3) -0.003(4) C2 0.041(5) 0.020(4) 0.028(4) -0.001(3) 0.005(3) -0.001(3) C3 0.031(4) 0.041(5) 0.037(4) 0.014(4) 0.003(3) 0.003(4) C4 0.038(4) 0.024(4) 0.024(4) 0.006(3) 0.009(3) 0.005(3) C5 0.038(4) 0.043(5) 0.013(3) 0.002(3) 0.001(3) -0.005(4) C6 0.039(4) 0.027(4) 0.028(4) -0.002(3) 0.003(3) 0.005(3) C7 0.047(5) 0.035(4) 0.018(4) 0.003(3) 0.001(3) -0.012(4) C8 0.052(5) 0.037(4) 0.022(4) 0.006(3) 0.007(3) 0.020(4) C9 0.044(5) 0.025(4) 0.029(4) 0.007(3) 0.012(3) -0.003(3) C10 0.062(6) 0.030(4) 0.026(4) 0.012(3) 0.017(4) 0.018(4) C11 0.041(5) 0.038(5) 0.031(4) -0.005(3) 0.010(3) 0.009(4) C12 0.063(6) 0.039(5) 0.024(4) 0.017(3) 0.005(4) 0.007(4) C13 0.069(6) 0.044(5) 0.029(4) 0.008(4) 0.000(4) -0.031(5) C14 0.050(5) 0.061(6) 0.016(4) 0.002(4) 0.006(3) 0.013(4) C15 0.037(5) 0.042(5) 0.056(6) 0.010(4) 0.009(4) 0.013(4) C16 0.030(4) 0.054(6) 0.043(5) -0.005(4) -0.006(4) -0.007(4) C17 0.040(4) 0.027(4) 0.027(4) 0.009(3) 0.009(3) 0.014(3) C18 0.053(5) 0.021(4) 0.029(4) 0.009(3) 0.009(4) 0.007(3) C19 0.049(5) 0.047(5) 0.016(4) -0.002(3) -0.005(3) -0.006(4) C20 0.058(6) 0.045(5) 0.032(5) -0.010(4) 0.003(4) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 O6 2.373(5) . ? Th1 O9 2.389(4) . ? Th1 O22 2.424(5) . ? Th1 O10 2.435(5) . ? Th1 O25 2.469(5) . ? Th1 O26 2.470(5) . ? Th1 O8 2.522(5) . ? Th1 O16 2.737(4) . ? Th1 N4 2.843(6) . ? Th1 N3 2.870(6) . ? Th1 Al3 3.5575(19) . ? Th2 O24 2.384(5) . ? Th2 O19 2.391(4) . ? Th2 O15 2.402(5) . ? Th2 O27 2.416(5) . ? Th2 O28 2.441(5) . ? Th2 O21 2.480(5) . ? Th2 O23 2.553(5) . ? Th2 N2 2.800(6) . ? Th2 O14 2.806(4) . ? Th2 N1 2.869(6) . ? Th2 Al4 3.5873(19) . ? Al1 O19 1.847(5) . ? Al1 O6 1.850(5) . ? Al1 O14 1.908(5) . ? Al1 O18 1.921(5) . ? Al1 O16 1.930(5) . ? Al1 O13 1.963(5) . ? Al2 O12 1.837(5) . ? Al2 O5 1.873(5) . ? Al2 O7 1.878(5) . ? Al2 O2 1.881(5) . ? Al2 O3 1.943(5) . ? Al2 O4 1.958(5) . ? Al2 Al4 2.910(3) . ? Al2 Al3 2.948(3) . ? Al3 O9 1.831(5) . ? Al3 O1 1.857(5) . ? Al3 O3 1.883(5) . ? Al3 O16 1.902(5) . ? Al3 O4 1.952(5) . ? Al3 O13 1.983(5) . ? Al4 O15 1.828(5) . ? Al4 O5 1.834(5) . ? Al4 O17 1.855(5) 2_666 ? Al4 O14 1.887(5) . ? Al4 O4 1.959(5) . ? Al4 O13 2.022(5) . ? Al5 O17 1.863(5) . ? Al5 O2 1.871(5) 2_666 ? Al5 O7 1.876(5) . ? Al5 O1 1.878(5) . ? Al5 O20 1.963(5) . ? Al5 O11 2.000(5) . ? O2 Al5 1.871(5) 2_666 ? O10 C5 1.278(8) . ? O17 Al4 1.855(5) 2_666 ? O21 C2 1.278(9) . ? O22 C7 1.265(9) . ? O24 C8 1.276(10) . ? O25 C6 1.283(9) . ? O26 C1 1.272(9) . ? O27 C4 1.273(8) . ? O28 C3 1.273(9) . ? O29 C4 1.243(9) . ? O30 C5 1.237(9) . ? O31 C2 1.225(10) . ? O32 C3 1.242(10) . ? O33 C6 1.232(10) . ? O34 C7 1.240(9) . ? O35 C8 1.240(10) . ? O36 C1 1.237(10) . ? O37 O57 1.70(3) . ? O39 O55 1.20(3) . ? O39 O53 1.57(3) 2_565 ? O53 O39 1.57(3) 2_565 ? O54 O58 0.82(3) 2_565 ? O58 O54 0.82(3) 2_565 ? N1 C9 1.449(10) . ? N1 C18 1.478(10) . ? N1 C12 1.485(9) . ? N2 C17 1.480(9) . ? N2 C15 1.485(11) . ? N2 C10 1.502(9) . ? N3 C13 1.480(10) . ? N3 C16 1.483(11) . ? N3 C19 1.497(9) . ? N4 C14 1.476(10) . ? N4 C11 1.477(11) . ? N4 C20 1.483(11) . ? C1 C16 1.466(12) . ? C2 C9 1.524(11) . ? C3 C15 1.501(12) . ? C4 C10 1.500(10) . ? C5 C14 1.493(12) . ? C6 C11 1.506(11) . ? C7 C13 1.506(11) . ? C8 C12 1.485(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.504(11) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.497(13) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 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 O6 Th1 O9 78.46(15) . . ? O6 Th1 O22 124.73(15) . . ? O9 Th1 O22 81.67(16) . . ? O6 Th1 O10 77.36(16) . . ? O9 Th1 O10 143.42(17) . . ? O22 Th1 O10 134.87(17) . . ? O6 Th1 O25 141.71(17) . . ? O9 Th1 O25 68.25(17) . . ? O22 Th1 O25 69.47(17) . . ? O10 Th1 O25 119.88(17) . . ? O6 Th1 O26 73.72(16) . . ? O9 Th1 O26 124.10(16) . . ? O22 Th1 O26 76.24(18) . . ? O10 Th1 O26 73.91(17) . . ? O25 Th1 O26 141.37(18) . . ? O6 Th1 O8 74.74(16) . . ? O9 Th1 O8 73.44(15) . . ? O22 Th1 O8 144.59(17) . . ? O10 Th1 O8 73.97(17) . . ? O25 Th1 O8 78.00(17) . . ? O26 Th1 O8 138.86(17) . . ? O6 Th1 O16 58.00(13) . . ? O9 Th1 O16 59.41(14) . . ? O22 Th1 O16 67.42(15) . . ? O10 Th1 O16 125.13(16) . . ? O25 Th1 O16 114.96(15) . . ? O26 Th1 O16 64.71(15) . . ? O8 Th1 O16 117.17(15) . . ? O6 Th1 N4 129.82(17) . . ? O9 Th1 N4 119.06(18) . . ? O22 Th1 N4 104.92(18) . . ? O10 Th1 N4 61.22(19) . . ? O25 Th1 N4 59.12(18) . . ? O26 Th1 N4 116.07(18) . . ? O8 Th1 N4 67.86(19) . . ? O16 Th1 N4 172.16(17) . . ? O6 Th1 N3 131.19(18) . . ? O9 Th1 N3 142.06(17) . . ? O22 Th1 N3 62.35(16) . . ? O10 Th1 N3 73.71(18) . . ? O25 Th1 N3 87.07(19) . . ? O26 Th1 N3 60.98(18) . . ? O8 Th1 N3 130.69(17) . . ? O16 Th1 N3 111.78(16) . . ? N4 Th1 N3 64.19(19) . . ? O6 Th1 Al3 69.60(11) . . ? O9 Th1 Al3 27.97(11) . . ? O22 Th1 Al3 68.94(11) . . ? O10 Th1 Al3 146.96(13) . . ? O25 Th1 Al3 87.70(12) . . ? O26 Th1 Al3 96.30(12) . . ? O8 Th1 Al3 96.79(12) . . ? O16 Th1 Al3 31.93(10) . . ? N4 Th1 Al3 145.11(14) . . ? N3 Th1 Al3 129.60(12) . . ? O24 Th2 O19 78.49(17) . . ? O24 Th2 O15 146.54(17) . . ? O19 Th2 O15 79.30(16) . . ? O24 Th2 O27 135.07(18) . . ? O19 Th2 O27 123.32(16) . . ? O15 Th2 O27 78.32(16) . . ? O24 Th2 O28 74.70(19) . . ? O19 Th2 O28 78.35(17) . . ? O15 Th2 O28 124.31(17) . . ? O27 Th2 O28 72.97(18) . . ? O24 Th2 O21 119.25(18) . . ? O19 Th2 O21 140.70(17) . . ? O15 Th2 O21 67.50(16) . . ? O27 Th2 O21 70.80(17) . . ? O28 Th2 O21 137.94(17) . . ? O24 Th2 O23 79.04(19) . . ? O19 Th2 O23 72.24(17) . . ? O15 Th2 O23 70.50(16) . . ? O27 Th2 O23 141.82(17) . . ? O28 Th2 O23 143.76(17) . . ? O21 Th2 O23 77.15(17) . . ? O24 Th2 N2 75.87(18) . . ? O19 Th2 N2 138.54(18) . . ? O15 Th2 N2 135.76(16) . . ? O27 Th2 N2 62.19(17) . . ? O28 Th2 N2 63.79(18) . . ? O21 Th2 N2 80.68(18) . . ? O23 Th2 N2 132.23(18) . . ? O24 Th2 O14 125.18(16) . . ? O19 Th2 O14 57.27(14) . . ? O15 Th2 O14 58.33(14) . . ? O27 Th2 O14 66.62(14) . . ? O28 Th2 O14 66.62(16) . . ? O21 Th2 O14 115.52(14) . . ? O23 Th2 O14 111.69(15) . . ? N2 Th2 O14 116.03(16) . . ? O24 Th2 N1 61.28(18) . . ? O19 Th2 N1 127.41(16) . . ? O15 Th2 N1 116.64(18) . . ? O27 Th2 N1 109.18(16) . . ? O28 Th2 N1 117.53(18) . . ? O21 Th2 N1 58.03(17) . . ? O23 Th2 N1 68.25(17) . . ? N2 Th2 N1 64.09(18) . . ? O14 Th2 N1 173.54(15) . . ? O24 Th2 Al4 148.39(13) . . ? O19 Th2 Al4 69.95(11) . . ? O15 Th2 Al4 27.43(11) . . ? O27 Th2 Al4 66.41(12) . . ? O28 Th2 Al4 96.88(13) . . ? O21 Th2 Al4 87.67(12) . . ? O23 Th2 Al4 92.53(12) . . ? N2 Th2 Al4 128.33(12) . . ? O14 Th2 Al4 31.41(10) . . ? N1 Th2 Al4 142.98(14) . . ? O19 Al1 O6 93.6(2) . . ? O19 Al1 O14 84.2(2) . . ? O6 Al1 O14 175.1(2) . . ? O19 Al1 O18 95.6(2) . . ? O6 Al1 O18 95.7(2) . . ? O14 Al1 O18 88.8(2) . . ? O19 Al1 O16 174.7(2) . . ? O6 Al1 O16 82.7(2) . . ? O14 Al1 O16 99.2(2) . . ? O18 Al1 O16 88.6(2) . . ? O19 Al1 O13 98.5(2) . . ? O6 Al1 O13 96.9(2) . . ? O14 Al1 O13 79.19(19) . . ? O18 Al1 O13 160.4(2) . . ? O16 Al1 O13 78.2(2) . . ? O12 Al2 O5 95.0(2) . . ? O12 Al2 O7 95.0(2) . . ? O5 Al2 O7 168.8(2) . . ? O12 Al2 O2 92.4(2) . . ? O5 Al2 O2 93.1(2) . . ? O7 Al2 O2 91.6(2) . . ? O12 Al2 O3 98.9(2) . . ? O5 Al2 O3 86.3(2) . . ? O7 Al2 O3 87.1(2) . . ? O2 Al2 O3 168.7(2) . . ? O12 Al2 O4 173.9(2) . . ? O5 Al2 O4 79.0(2) . . ? O7 Al2 O4 90.8(2) . . ? O2 Al2 O4 89.3(2) . . ? O3 Al2 O4 79.41(19) . . ? O12 Al2 Al4 132.30(18) . . ? O5 Al2 Al4 37.80(15) . . ? O7 Al2 Al4 132.69(17) . . ? O2 Al2 Al4 85.53(15) . . ? O3 Al2 Al4 87.07(15) . . ? O4 Al2 Al4 42.02(14) . . ? O12 Al2 Al3 137.76(17) . . ? O5 Al2 Al3 85.23(15) . . ? O7 Al2 Al3 83.92(15) . . ? O2 Al2 Al3 129.78(17) . . ? O3 Al2 Al3 38.87(14) . . ? O4 Al2 Al3 41.00(13) . . ? Al4 Al2 Al3 63.28(6) . . ? O9 Al3 O1 96.0(2) . . ? O9 Al3 O3 98.4(2) . . ? O1 Al3 O3 92.9(2) . . ? O9 Al3 O16 86.5(2) . . ? O1 Al3 O16 94.5(2) . . ? O3 Al3 O16 170.6(2) . . ? O9 Al3 O4 172.6(2) . . ? O1 Al3 O4 91.4(2) . . ? O3 Al3 O4 81.01(19) . . ? O16 Al3 O4 93.1(2) . . ? O9 Al3 O13 94.2(2) . . ? O1 Al3 O13 167.2(2) . . ? O3 Al3 O13 93.2(2) . . ? O16 Al3 O13 78.4(2) . . ? O4 Al3 O13 78.48(19) . . ? O9 Al3 Al2 138.78(18) . . ? O1 Al3 Al2 88.05(15) . . ? O3 Al3 Al2 40.35(14) . . ? O16 Al3 Al2 134.23(16) . . ? O4 Al3 Al2 41.14(14) . . ? O13 Al3 Al2 89.40(14) . . ? O9 Al3 Th1 37.73(15) . . ? O1 Al3 Th1 90.79(14) . . ? O3 Al3 Th1 136.12(15) . . ? O16 Al3 Th1 49.53(13) . . ? O4 Al3 Th1 142.61(15) . . ? O13 Al3 Th1 92.52(14) . . ? Al2 Al3 Th1 176.15(8) . . ? O15 Al4 O5 96.9(2) . . ? O15 Al4 O17 98.8(2) . 2_666 ? O5 Al4 O17 95.8(2) . 2_666 ? O15 Al4 O14 87.2(2) . . ? O5 Al4 O14 169.8(2) . . ? O17 Al4 O14 92.8(2) 2_666 . ? O15 Al4 O4 169.7(2) . . ? O5 Al4 O4 79.9(2) . . ? O17 Al4 O4 91.4(2) 2_666 . ? O14 Al4 O4 94.4(2) . . ? O15 Al4 O13 93.0(2) . . ? O5 Al4 O13 92.2(2) . . ? O17 Al4 O13 164.9(2) 2_666 . ? O14 Al4 O13 78.22(19) . . ? O4 Al4 O13 77.40(18) . . ? O15 Al4 Al2 135.67(18) . . ? O5 Al4 Al2 38.76(15) . . ? O17 Al4 Al2 88.49(16) 2_666 . ? O14 Al4 Al2 136.36(17) . . ? O4 Al4 Al2 41.99(14) . . ? O13 Al4 Al2 89.72(14) . . ? O15 Al4 Th2 37.26(15) . . ? O5 Al4 Th2 134.14(17) . . ? O17 Al4 Th2 91.72(15) 2_666 . ? O14 Al4 Th2 50.80(14) . . ? O4 Al4 Th2 145.15(15) . . ? O13 Al4 Th2 91.91(14) . . ? Al2 Al4 Th2 172.82(8) . . ? O17 Al5 O2 93.3(2) . 2_666 ? O17 Al5 O7 91.8(2) . . ? O2 Al5 O7 93.2(2) 2_666 . ? O17 Al5 O1 174.8(2) . . ? O2 Al5 O1 90.5(2) 2_666 . ? O7 Al5 O1 91.5(2) . . ? O17 Al5 O20 87.2(2) . . ? O2 Al5 O20 90.8(2) 2_666 . ? O7 Al5 O20 176.0(2) . . ? O1 Al5 O20 89.2(2) . . ? O17 Al5 O11 88.8(2) . . ? O2 Al5 O11 176.0(2) 2_666 . ? O7 Al5 O11 90.1(2) . . ? O1 Al5 O11 87.2(2) . . ? O20 Al5 O11 86.0(2) . . ? Al3 O1 Al5 133.2(3) . . ? Al5 O2 Al2 135.4(3) 2_666 . ? Al3 O3 Al2 100.8(2) . . ? Al3 O4 Al2 97.9(2) . . ? Al3 O4 Al4 103.6(2) . . ? Al2 O4 Al4 96.0(2) . . ? Al4 O5 Al2 103.4(2) . . ? Al1 O6 Th1 118.2(2) . . ? Al5 O7 Al2 135.1(3) . . ? Al3 O9 Th1 114.3(2) . . ? C5 O10 Th1 131.8(5) . . ? Al1 O13 Al3 99.7(2) . . ? Al1 O13 Al4 97.9(2) . . ? Al3 O13 Al4 100.2(2) . . ? Al4 O14 Al1 104.7(2) . . ? Al4 O14 Th2 97.79(19) . . ? Al1 O14 Th2 99.94(18) . . ? Al4 O15 Th2 115.3(2) . . ? Al3 O16 Al1 103.8(2) . . ? Al3 O16 Th1 98.55(18) . . ? Al1 O16 Th1 100.90(17) . . ? Al4 O17 Al5 133.7(3) 2_666 . ? Al1 O19 Th2 118.6(2) . . ? C2 O21 Th2 123.5(4) . . ? C7 O22 Th1 131.9(4) . . ? C8 O24 Th2 133.3(5) . . ? C6 O25 Th1 126.4(5) . . ? C1 O26 Th1 131.9(5) . . ? C4 O27 Th2 128.1(4) . . ? C3 O28 Th2 129.0(5) . . ? O55 O39 O53 142(2) . 2_565 ? C9 N1 C18 107.7(6) . . ? C9 N1 C12 113.0(6) . . ? C18 N1 C12 110.0(6) . . ? C9 N1 Th2 107.7(4) . . ? C18 N1 Th2 109.7(4) . . ? C12 N1 Th2 108.7(4) . . ? C17 N2 C15 108.1(6) . . ? C17 N2 C10 109.0(6) . . ? C15 N2 C10 109.8(7) . . ? C17 N2 Th2 112.9(4) . . ? C15 N2 Th2 109.6(4) . . ? C10 N2 Th2 107.4(4) . . ? C13 N3 C16 109.4(7) . . ? C13 N3 C19 109.9(7) . . ? C16 N3 C19 108.9(6) . . ? C13 N3 Th1 108.3(5) . . ? C16 N3 Th1 109.6(5) . . ? C19 N3 Th1 110.9(5) . . ? C14 N4 C11 110.6(6) . . ? C14 N4 C20 111.4(7) . . ? C11 N4 C20 107.3(7) . . ? C14 N4 Th1 110.8(5) . . ? C11 N4 Th1 107.8(4) . . ? C20 N4 Th1 108.8(5) . . ? O36 C1 O26 122.7(8) . . ? O36 C1 C16 119.9(7) . . ? O26 C1 C16 117.4(7) . . ? O31 C2 O21 124.2(7) . . ? O31 C2 C9 120.0(7) . . ? O21 C2 C9 115.7(7) . . ? O32 C3 O28 125.0(8) . . ? O32 C3 C15 117.8(7) . . ? O28 C3 C15 117.2(7) . . ? O29 C4 O27 122.9(7) . . ? O29 C4 C10 118.8(6) . . ? O27 C4 C10 118.2(6) . . ? O30 C5 O10 123.8(8) . . ? O30 C5 C14 118.1(7) . . ? O10 C5 C14 118.1(7) . . ? O33 C6 O25 124.3(7) . . ? O33 C6 C11 119.5(7) . . ? O25 C6 C11 116.0(7) . . ? O34 C7 O22 123.6(7) . . ? O34 C7 C13 118.6(7) . . ? O22 C7 C13 117.8(6) . . ? O35 C8 O24 122.4(8) . . ? O35 C8 C12 120.0(8) . . ? O24 C8 C12 117.6(7) . . ? N1 C9 C2 111.4(6) . . ? N1 C9 H9A 109.3 . . ? C2 C9 H9A 109.3 . . ? N1 C9 H9B 109.3 . . ? C2 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C4 C10 N2 112.6(6) . . ? C4 C10 H10A 109.1 . . ? N2 C10 H10A 109.1 . . ? C4 C10 H10B 109.1 . . ? N2 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? N4 C11 C6 112.1(6) . . ? N4 C11 H11A 109.2 . . ? C6 C11 H11A 109.2 . . ? N4 C11 H11B 109.2 . . ? C6 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C8 C12 N1 112.4(7) . . ? C8 C12 H12A 109.1 . . ? N1 C12 H12A 109.1 . . ? C8 C12 H12B 109.1 . . ? N1 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? N3 C13 C7 115.0(7) . . ? N3 C13 H13A 108.5 . . ? C7 C13 H13A 108.5 . . ? N3 C13 H13B 108.5 . . ? C7 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? N4 C14 C5 112.9(6) . . ? N4 C14 H14A 109.0 . . ? C5 C14 H14A 109.0 . . ? N4 C14 H14B 109.0 . . ? C5 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N2 C15 C3 115.4(7) . . ? N2 C15 H15A 108.4 . . ? C3 C15 H15A 108.4 . . ? N2 C15 H15B 108.4 . . ? C3 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C1 C16 N3 114.7(7) . . ? C1 C16 H16A 108.6 . . ? N3 C16 H16A 108.6 . . ? C1 C16 H16B 108.6 . . ? N3 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? N2 C17 C18 111.7(6) . . ? N2 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N2 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? N1 C18 C17 113.7(6) . . ? N1 C18 H18A 108.8 . . ? C17 C18 H18A 108.8 . . ? N1 C18 H18B 108.8 . . ? C17 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C20 C19 N3 111.6(6) . . ? C20 C19 H19A 109.3 . . ? N3 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? N3 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? N4 C20 C19 112.7(8) . . ? N4 C20 H20A 109.0 . . ? C19 C20 H20A 109.0 . . ? N4 C20 H20B 109.0 . . ? C19 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.162 _refine_diff_density_min -1.171 _refine_diff_density_rms 0.185 _database_code_depnum_ccdc_archive 'CCDC 939974'