Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Mike Ward' _publ_contact_author_address ; Department of Chemistry University of Sheffield Dainton Building Sheffield S3 7HF UNITED KINGDOM ; _publ_contact_author_fax '01142 229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_section_title ; Polynuclear lanthanide complexes of a series of bridging ligands containing two tridentate N,N',O-donor units: structures and luminescence properties ; _publ_contact_letter ; This CIF file contains details of the 11 crystal structure in the paper Polynuclear lanthanide(III) complexes of a series of bridging ...' by T. K. Ronson et al, submitted to Dalton Trans. for publication. ; loop_ _publ_author_name M.D.Ward H.Adams S.Faulkner L.P.Harding S.Pope T.K.Ronson ; D.Sykes ; #======================================================== data_imw373m _database_code_depnum_ccdc_archive 'CCDC 630959' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H38 N8 O2' _chemical_formula_weight 590.72 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' _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 5.3464(6) _cell_length_b 11.5521(13) _cell_length_c 13.1243(14) _cell_angle_alpha 71.846(8) _cell_angle_beta 81.774(8) _cell_angle_gamma 81.590(8) _cell_volume 757.84(15) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1867 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 24.25 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 314 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9809 _exptl_absorpt_correction_T_max 0.9983 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12699 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2668 _reflns_number_gt 1884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0542P)^2^+0.1094P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2668 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.0977 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 O1 O 0.2960(3) 0.66252(12) 0.85884(11) 0.0281(4) Uani 1 1 d . . . N1 N 0.5068(3) 0.96978(14) 0.24132(12) 0.0219(4) Uani 1 1 d . . . N2 N 0.6393(3) 0.95140(14) 0.32653(13) 0.0226(4) Uani 1 1 d . . . N3 N 0.4810(3) 0.73751(14) 0.58844(13) 0.0218(4) Uani 1 1 d . . . N4 N 0.3045(3) 0.52304(14) 0.77000(13) 0.0234(4) Uani 1 1 d . . . C1 C 1.1300(4) 1.09210(18) -0.07202(16) 0.0234(5) Uani 1 1 d . . . H1 H 1.2177 1.1561 -0.1215 0.028 Uiso 1 1 calc R . . C2 C 0.9259(4) 1.12016(18) -0.00227(15) 0.0233(5) Uani 1 1 d . . . H2 H 0.8767 1.2032 -0.0041 0.028 Uiso 1 1 calc R . . C3 C 0.7929(4) 1.02862(17) 0.07012(15) 0.0202(4) Uani 1 1 d . . . C4 C 0.5661(4) 1.06471(18) 0.14124(15) 0.0230(5) Uani 1 1 d . . . H4A H 0.5986 1.1382 0.1588 0.028 Uiso 1 1 calc R . . H4B H 0.4158 1.0876 0.1002 0.028 Uiso 1 1 calc R . . C5 C 0.3217(4) 0.89477(18) 0.26379(16) 0.0246(5) Uani 1 1 d . . . H5 H 0.2060 0.8925 0.2160 0.029 Uiso 1 1 calc R . . C6 C 0.3321(4) 0.82296(18) 0.36795(16) 0.0237(5) Uani 1 1 d . . . H6 H 0.2272 0.7607 0.4074 0.028 Uiso 1 1 calc R . . C7 C 0.5319(4) 0.86104(17) 0.40424(15) 0.0214(4) Uani 1 1 d . . . C8 C 0.6146(4) 0.82046(17) 0.51342(15) 0.0205(4) Uani 1 1 d . . . C9 C 0.8152(4) 0.86919(18) 0.53703(16) 0.0233(5) Uani 1 1 d . . . H9 H 0.9049 0.9280 0.4820 0.028 Uiso 1 1 calc R . . C10 C 0.8823(4) 0.83136(17) 0.64080(15) 0.0235(5) Uani 1 1 d . . . H10 H 1.0210 0.8620 0.6581 0.028 Uiso 1 1 calc R . . C11 C 0.7435(4) 0.74784(17) 0.71929(16) 0.0226(5) Uani 1 1 d . . . H11 H 0.7841 0.7206 0.7917 0.027 Uiso 1 1 calc R . . C12 C 0.5435(4) 0.70445(17) 0.69017(16) 0.0209(4) Uani 1 1 d . . . C13 C 0.3728(4) 0.62707(18) 0.77875(16) 0.0223(5) Uani 1 1 d . . . C14 C 0.4050(4) 0.46803(19) 0.68390(16) 0.0277(5) Uani 1 1 d . . . H14A H 0.4645 0.3806 0.7165 0.033 Uiso 1 1 calc R . . H14B H 0.5533 0.5094 0.6423 0.033 Uiso 1 1 calc R . . C15 C 0.2097(4) 0.4773(2) 0.60750(17) 0.0372(6) Uani 1 1 d . . . H15A H 0.0619 0.4368 0.6482 0.056 Uiso 1 1 calc R . . H15B H 0.2850 0.4373 0.5528 0.056 Uiso 1 1 calc R . . H15C H 0.1561 0.5638 0.5722 0.056 Uiso 1 1 calc R . . C16 C 0.1461(4) 0.44976(18) 0.86128(16) 0.0259(5) Uani 1 1 d . . . H16A H 0.0569 0.3962 0.8360 0.031 Uiso 1 1 calc R . . H16B H 0.0160 0.5051 0.8900 0.031 Uiso 1 1 calc R . . C17 C 0.3037(4) 0.37140(19) 0.95053(17) 0.0329(5) Uani 1 1 d . . . H17A H 0.4327 0.3165 0.9223 0.049 Uiso 1 1 calc R . . H17B H 0.1929 0.3227 1.0094 0.049 Uiso 1 1 calc R . . H17C H 0.3872 0.4243 0.9776 0.049 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 O1 0.0356(8) 0.0277(8) 0.0230(8) -0.0101(7) 0.0018(6) -0.0087(7) N1 0.0244(9) 0.0237(9) 0.0190(9) -0.0075(7) -0.0018(7) -0.0048(7) N2 0.0249(9) 0.0243(9) 0.0192(9) -0.0067(8) -0.0021(7) -0.0043(7) N3 0.0243(9) 0.0203(9) 0.0212(9) -0.0070(7) -0.0010(7) -0.0030(7) N4 0.0279(9) 0.0222(9) 0.0210(9) -0.0070(7) 0.0002(7) -0.0071(7) C1 0.0267(11) 0.0232(11) 0.0204(11) -0.0039(9) -0.0016(9) -0.0090(9) C2 0.0264(11) 0.0204(11) 0.0252(11) -0.0087(9) -0.0021(9) -0.0047(9) C3 0.0233(10) 0.0217(11) 0.0186(10) -0.0087(9) -0.0048(8) -0.0037(9) C4 0.0257(11) 0.0224(11) 0.0197(11) -0.0045(9) -0.0021(9) -0.0029(9) C5 0.0245(11) 0.0275(11) 0.0253(12) -0.0111(10) -0.0012(9) -0.0082(9) C6 0.0248(11) 0.0233(11) 0.0259(12) -0.0103(9) 0.0003(9) -0.0079(9) C7 0.0236(10) 0.0199(10) 0.0212(11) -0.0081(9) 0.0018(8) -0.0038(9) C8 0.0218(10) 0.0188(10) 0.0210(11) -0.0078(9) 0.0001(8) -0.0005(8) C9 0.0238(11) 0.0220(11) 0.0250(11) -0.0083(9) 0.0010(9) -0.0058(9) C10 0.0228(10) 0.0243(11) 0.0259(12) -0.0108(9) -0.0019(9) -0.0039(9) C11 0.0242(10) 0.0229(11) 0.0211(11) -0.0080(9) -0.0033(9) -0.0001(9) C12 0.0240(10) 0.0167(10) 0.0222(11) -0.0078(9) 0.0004(8) -0.0014(8) C13 0.0229(10) 0.0219(11) 0.0218(11) -0.0056(9) -0.0040(9) -0.0018(9) C14 0.0332(12) 0.0246(11) 0.0275(12) -0.0112(10) 0.0022(9) -0.0079(9) C15 0.0457(14) 0.0430(14) 0.0285(13) -0.0150(11) -0.0026(10) -0.0142(11) C16 0.0325(12) 0.0222(11) 0.0243(11) -0.0066(9) -0.0008(9) -0.0099(9) C17 0.0452(14) 0.0260(12) 0.0303(12) -0.0064(10) -0.0067(10) -0.0138(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C13 1.240(2) . ? N1 C5 1.351(2) . ? N1 N2 1.354(2) . ? N1 C4 1.454(2) . ? N2 C7 1.343(2) . ? N3 C8 1.345(2) . ? N3 C12 1.346(2) . ? N4 C13 1.348(2) . ? N4 C14 1.464(2) . ? N4 C16 1.468(2) . ? C1 C3 1.389(3) 2_775 ? C1 C2 1.389(3) . ? C1 H1 0.9500 . ? C2 C3 1.388(3) . ? C2 H2 0.9500 . ? C3 C1 1.389(3) 2_775 ? C3 C4 1.512(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.364(3) . ? C5 H5 0.9500 . ? C6 C7 1.405(3) . ? C6 H6 0.9500 . ? C7 C8 1.473(3) . ? C8 C9 1.394(3) . ? C9 C10 1.377(3) . ? C9 H9 0.9500 . ? C10 C11 1.383(3) . ? C10 H10 0.9500 . ? C11 C12 1.391(3) . ? C11 H11 0.9500 . ? C12 C13 1.507(3) . ? C14 C15 1.519(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.516(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 N1 N2 112.38(16) . . ? C5 N1 C4 127.51(16) . . ? N2 N1 C4 120.07(15) . . ? C7 N2 N1 104.18(14) . . ? C8 N3 C12 117.28(16) . . ? C13 N4 C14 125.03(17) . . ? C13 N4 C16 117.57(16) . . ? C14 N4 C16 116.78(15) . . ? C3 C1 C2 120.61(18) 2_775 . ? C3 C1 H1 119.7 2_775 . ? C2 C1 H1 119.7 . . ? C3 C2 C1 120.93(18) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C1 118.46(17) . 2_775 ? C2 C3 C4 118.72(17) . . ? C1 C3 C4 122.80(17) 2_775 . ? N1 C4 C3 114.46(16) . . ? N1 C4 H4A 108.6 . . ? C3 C4 H4A 108.6 . . ? N1 C4 H4B 108.6 . . ? C3 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? N1 C5 C6 107.14(17) . . ? N1 C5 H5 126.4 . . ? C6 C5 H5 126.4 . . ? C5 C6 C7 105.02(17) . . ? C5 C6 H6 127.5 . . ? C7 C6 H6 127.5 . . ? N2 C7 C6 111.28(17) . . ? N2 C7 C8 120.38(16) . . ? C6 C7 C8 128.17(18) . . ? N3 C8 C9 122.59(18) . . ? N3 C8 C7 116.22(16) . . ? C9 C8 C7 121.15(18) . . ? C10 C9 C8 119.41(18) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 118.67(17) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C10 C11 C12 118.75(18) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? N3 C12 C11 123.24(18) . . ? N3 C12 C13 118.48(16) . . ? C11 C12 C13 117.97(17) . . ? O1 C13 N4 121.33(18) . . ? O1 C13 C12 118.10(17) . . ? N4 C13 C12 120.57(17) . . ? N4 C14 C15 112.82(17) . . ? N4 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? N4 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C17 111.60(16) . . ? N4 C16 H16A 109.3 . . ? C17 C16 H16A 109.3 . . ? N4 C16 H16B 109.3 . . ? C17 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 N2 C7 0.3(2) . . . . ? C4 N1 N2 C7 178.47(15) . . . . ? C3 C1 C2 C3 -0.6(3) 2_775 . . . ? C1 C2 C3 C1 0.6(3) . . . 2_775 ? C1 C2 C3 C4 -177.71(17) . . . . ? C5 N1 C4 C3 -101.5(2) . . . . ? N2 N1 C4 C3 80.6(2) . . . . ? C2 C3 C4 N1 -155.05(16) . . . . ? C1 C3 C4 N1 26.7(2) 2_775 . . . ? N2 N1 C5 C6 -0.4(2) . . . . ? C4 N1 C5 C6 -178.38(17) . . . . ? N1 C5 C6 C7 0.3(2) . . . . ? N1 N2 C7 C6 -0.1(2) . . . . ? N1 N2 C7 C8 -175.83(16) . . . . ? C5 C6 C7 N2 -0.1(2) . . . . ? C5 C6 C7 C8 175.19(18) . . . . ? C12 N3 C8 C9 1.8(3) . . . . ? C12 N3 C8 C7 -176.19(16) . . . . ? N2 C7 C8 N3 174.12(16) . . . . ? C6 C7 C8 N3 -0.8(3) . . . . ? N2 C7 C8 C9 -3.9(3) . . . . ? C6 C7 C8 C9 -178.82(19) . . . . ? N3 C8 C9 C10 0.3(3) . . . . ? C7 C8 C9 C10 178.20(17) . . . . ? C8 C9 C10 C11 -1.5(3) . . . . ? C9 C10 C11 C12 0.6(3) . . . . ? C8 N3 C12 C11 -2.8(3) . . . . ? C8 N3 C12 C13 170.73(16) . . . . ? C10 C11 C12 N3 1.6(3) . . . . ? C10 C11 C12 C13 -171.94(17) . . . . ? C14 N4 C13 O1 -173.72(17) . . . . ? C16 N4 C13 O1 -3.0(3) . . . . ? C14 N4 C13 C12 7.0(3) . . . . ? C16 N4 C13 C12 177.64(16) . . . . ? N3 C12 C13 O1 -127.90(19) . . . . ? C11 C12 C13 O1 46.0(3) . . . . ? N3 C12 C13 N4 51.4(3) . . . . ? C11 C12 C13 N4 -134.71(19) . . . . ? C13 N4 C14 C15 -110.1(2) . . . . ? C16 N4 C14 C15 79.2(2) . . . . ? C13 N4 C16 C17 -80.3(2) . . . . ? C14 N4 C16 C17 91.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.172 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.045 #===END data_imw477 _database_code_depnum_ccdc_archive 'CCDC 630960' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H114 Cl6 N24 Nd2 O30' _chemical_formula_weight 2657.35 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 13.6489(7) _cell_length_b 13.6489(7) _cell_length_c 40.211(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6487.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9792 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour 'pale purple' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 0.991 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8417 _exptl_absorpt_correction_T_max 0.9614 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART 4000 CCDarea detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 187247 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5063 _reflns_number_gt 4730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1330P)^2^+41.1600P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5063 _refine_ls_number_parameters 261 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.2298 _refine_ls_wR_factor_gt 0.2238 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.0000 0.0000 0.397370(11) 0.01588(19) Uani 1 3 d S . . O1 O -0.0460(4) 0.1079(4) 0.43537(10) 0.0224(9) Uani 1 1 d . . . N1 N 0.2331(5) 0.0444(5) 0.33841(14) 0.0274(12) Uani 1 1 d . . . N2 N 0.1806(4) 0.0883(5) 0.35650(11) 0.0185(9) Uani 1 1 d . . . N3 N 0.1312(5) 0.2181(5) 0.39722(12) 0.0230(12) Uani 1 1 d . . . N4 N -0.0799(5) 0.2530(5) 0.43660(13) 0.0237(11) Uani 1 1 d . . . C1 C 0.1771(9) -0.1466(7) 0.26703(18) 0.046(2) Uani 1 1 d . . . H1 H 0.1770 -0.2060 0.2784 0.056 Uiso 1 1 calc R . . C2 C 0.1772(6) -0.0594(6) 0.28491(14) 0.0229(13) Uani 1 1 d . . . C3 C 0.1740(8) 0.0274(7) 0.26740(18) 0.0390(19) Uani 1 1 d . . . H3 H 0.1718 0.0853 0.2789 0.047 Uiso 1 1 calc R . . C4 C 0.1712(6) -0.0641(6) 0.32257(16) 0.0245(13) Uani 1 1 d . . . H4A H 0.0926 -0.0991 0.3293 0.029 Uiso 1 1 calc R . . H4B H 0.2004 -0.1118 0.3304 0.029 Uiso 1 1 calc R . . C5 C 0.3445(7) 0.1192(7) 0.33469(19) 0.0351(17) Uani 1 1 d . . . H5 H 0.3964 0.1067 0.3232 0.042 Uiso 1 1 calc R . . C6 C 0.3676(7) 0.2188(7) 0.35121(18) 0.0343(18) Uani 1 1 d . . . H6 H 0.4364 0.2859 0.3528 0.041 Uiso 1 1 calc R . . C7 C 0.2657(6) 0.1945(6) 0.36444(17) 0.0254(14) Uani 1 1 d . . . C8 C 0.2371(6) 0.2679(6) 0.38417(15) 0.0219(13) Uani 1 1 d . . . C9 C 0.3166(6) 0.3808(6) 0.38940(17) 0.0284(14) Uani 1 1 d . . . H9 H 0.3879 0.4128 0.3797 0.034 Uiso 1 1 calc R . . C10 C 0.2866(7) 0.4460(6) 0.40993(18) 0.0318(16) Uani 1 1 d . . . H10 H 0.3380 0.5217 0.4142 0.038 Uiso 1 1 calc R . . C11 C 0.1802(6) 0.3947(6) 0.42325(17) 0.0277(15) Uani 1 1 d . . . H11 H 0.1592 0.4353 0.4373 0.033 Uiso 1 1 calc R . . C12 C 0.1030(6) 0.2818(6) 0.41594(16) 0.0230(13) Uani 1 1 d . . . C13 C -0.0150(6) 0.2103(5) 0.43002(14) 0.0203(12) Uani 1 1 d . . . C14 C -0.0646(6) 0.3621(6) 0.42405(18) 0.0287(15) Uani 1 1 d . . . H14A H -0.1305 0.3482 0.4112 0.034 Uiso 1 1 calc R . . H14B H 0.0008 0.3972 0.4095 0.034 Uiso 1 1 calc R . . C15 C -0.0481(6) 0.4428(6) 0.4529(2) 0.0311(15) Uani 1 1 d . . . H15A H -0.1148 0.4102 0.4665 0.047 Uiso 1 1 calc R . . H15B H -0.0350 0.5138 0.4441 0.047 Uiso 1 1 calc R . . H15C H 0.0157 0.4549 0.4660 0.047 Uiso 1 1 calc R . . C16 C -0.1877(6) 0.1798(6) 0.45349(17) 0.0263(13) Uani 1 1 d . . . H16A H -0.2242 0.1060 0.4430 0.032 Uiso 1 1 calc R . . H16B H -0.2368 0.2117 0.4508 0.032 Uiso 1 1 calc R . . C17 C -0.1739(7) 0.1656(7) 0.49042(17) 0.0326(14) Uani 1 1 d . . . H17A H -0.1325 0.1263 0.4933 0.049 Uiso 1 1 calc R . . H17B H -0.2471 0.1228 0.5005 0.049 Uiso 1 1 calc R . . H17C H -0.1332 0.2387 0.5007 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.6667 0.3333 0.51434(6) 0.0179(4) Uani 1 3 d S . . O2 O 0.6667 0.3333 0.4781(2) 0.0342(18) Uani 1 3 d S . . O3 O 0.7813(4) 0.3914(5) 0.52603(12) 0.0296(10) Uani 1 1 d . . . Cl3 Cl 0.4114(6) 0.6297(6) 0.34044(15) 0.0479(17) Uani 0.33 1 d PD A -1 O7 O 0.467(2) 0.7270(18) 0.3207(6) 0.069(6) Uiso 0.33 1 d PD A -1 O8 O 0.337(2) 0.5290(19) 0.3242(7) 0.084(8) Uiso 0.33 1 d PD A -1 O9 O 0.506(2) 0.627(3) 0.3554(7) 0.080 Uiso 0.33 1 d PD A -1 O10 O 0.343(2) 0.646(2) 0.3632(3) 0.034(4) Uiso 0.33 1 d PD A -1 Cl2 Cl 0.6667 0.3333 0.3657(3) 0.067(2) Uiso 0.522(11) 3 d SPDU . 1 O4 O 0.624(2) 0.400(2) 0.3454(5) 0.101(6) Uiso 0.522(11) 1 d PDU . 1 O5 O 0.6667 0.3333 0.3999(5) 0.126(15) Uiso 0.522(11) 3 d SPD . 1 Cl2' Cl 0.6667 0.3333 0.3444(3) 0.070(2) Uiso 0.478(11) 3 d SPDU . 2 O4' O 0.623(2) 0.4024(19) 0.3601(5) 0.086(5) Uiso 0.478(11) 1 d PDU . 2 O5' O 0.6667 0.3333 0.3109(5) 0.078(9) Uiso 0.478(11) 3 d SPD . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0179(2) 0.0179(2) 0.0118(3) 0.000 0.000 0.00897(11) O1 0.028(2) 0.024(2) 0.0160(19) -0.0013(16) 0.0037(17) 0.0139(19) N1 0.030(3) 0.036(3) 0.020(3) -0.004(2) 0.000(2) 0.019(3) N2 0.025(2) 0.023(3) 0.0106(19) 0.001(2) 0.0032(17) 0.014(3) N3 0.029(3) 0.022(3) 0.013(2) 0.0011(18) 0.0016(19) 0.008(2) N4 0.024(3) 0.023(3) 0.025(3) 0.003(2) 0.005(2) 0.013(2) C1 0.101(8) 0.041(5) 0.027(4) -0.001(3) -0.009(4) 0.058(6) C2 0.030(3) 0.035(4) 0.010(3) 0.001(2) 0.003(2) 0.021(3) C3 0.068(6) 0.037(4) 0.023(4) -0.002(3) -0.001(3) 0.035(4) C4 0.032(4) 0.026(3) 0.018(3) -0.001(2) 0.000(3) 0.016(3) C5 0.029(4) 0.044(5) 0.033(4) -0.008(3) 0.003(3) 0.020(4) C6 0.019(3) 0.041(4) 0.034(4) -0.012(3) 0.005(3) 0.008(3) C7 0.019(3) 0.035(4) 0.023(3) -0.003(3) -0.001(2) 0.014(3) C8 0.022(3) 0.029(3) 0.017(3) 0.003(2) -0.002(2) 0.015(3) C9 0.018(3) 0.035(4) 0.026(3) 0.003(3) 0.003(3) 0.009(3) C10 0.034(4) 0.027(4) 0.028(3) 0.001(3) 0.000(3) 0.011(3) C11 0.034(4) 0.020(3) 0.025(3) -0.001(2) 0.001(3) 0.010(3) C12 0.020(3) 0.032(3) 0.018(3) -0.002(2) -0.003(2) 0.015(3) C13 0.019(3) 0.017(3) 0.019(3) -0.001(2) -0.001(2) 0.005(2) C14 0.025(3) 0.029(3) 0.036(4) 0.009(3) 0.004(3) 0.016(3) C15 0.030(4) 0.022(3) 0.041(4) 0.002(3) 0.009(3) 0.012(3) C16 0.021(3) 0.021(3) 0.036(3) -0.003(3) 0.008(3) 0.010(2) C17 0.031(4) 0.032(4) 0.030(3) -0.007(3) 0.009(3) 0.012(3) Cl1 0.0155(6) 0.0155(6) 0.0226(11) 0.000 0.000 0.0078(3) O2 0.039(3) 0.039(3) 0.025(4) 0.000 0.000 0.0195(14) O3 0.020(2) 0.027(3) 0.037(2) -0.003(2) -0.0066(18) 0.008(2) Cl3 0.058(4) 0.052(4) 0.028(3) -0.002(2) -0.001(3) 0.023(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 Nd1 O1 2.413(4) 3 ? Nd1 O1 2.413(4) 2 ? Nd1 O1 2.413(4) . ? Nd1 N3 2.596(6) 2 ? Nd1 N3 2.596(6) . ? Nd1 N3 2.596(6) 3 ? Nd1 N2 2.694(5) 3 ? Nd1 N2 2.694(5) . ? Nd1 N2 2.694(5) 2 ? O1 C13 1.259(8) . ? N1 C5 1.350(10) . ? N1 N2 1.353(8) . ? N1 C4 1.435(9) . ? N2 C7 1.368(9) . ? N3 C12 1.344(9) . ? N3 C8 1.358(8) . ? N4 C13 1.308(9) . ? N4 C16 1.468(9) . ? N4 C14 1.485(9) . ? C1 C1 1.369(14) 10_556 ? C1 C2 1.389(9) . ? C1 H1 0.9300 . ? C2 C3 1.398(10) . ? C2 C4 1.516(8) . ? C3 C3 1.399(14) 10_556 ? C3 H3 0.9300 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.400(11) . ? C5 H5 0.9300 . ? C6 C7 1.366(10) . ? C6 H6 0.9300 . ? C7 C8 1.476(9) . ? C8 C9 1.387(10) . ? C9 C10 1.416(11) . ? C9 H9 0.9300 . ? C10 C11 1.367(10) . ? C10 H10 0.9300 . ? C11 C12 1.396(10) . ? C11 H11 0.9300 . ? C12 C13 1.515(9) . ? C14 C15 1.536(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.521(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? Cl1 O3 1.434(4) 3_665 ? Cl1 O3 1.434(4) . ? Cl1 O3 1.434(4) 2_655 ? Cl1 O2 1.458(9) . ? Cl3 O8 1.398(17) . ? Cl3 O7 1.401(17) . ? Cl3 O10 1.405(13) . ? Cl3 O9 1.440(18) . ? Cl2 O5 1.375(19) . ? Cl2 O4 1.537(16) 2_655 ? Cl2 O4 1.537(16) 3_665 ? Cl2 O4 1.537(16) . ? Cl2' O5' 1.349(18) . ? Cl2' O4' 1.482(16) 3_665 ? Cl2' O4' 1.482(16) 2_655 ? Cl2' O4' 1.482(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nd1 O1 84.17(16) 3 2 ? O1 Nd1 O1 84.17(16) 3 . ? O1 Nd1 O1 84.17(16) 2 . ? O1 Nd1 N3 140.40(15) 3 2 ? O1 Nd1 N3 62.75(16) 2 2 ? O1 Nd1 N3 72.04(17) . 2 ? O1 Nd1 N3 72.04(17) 3 . ? O1 Nd1 N3 140.40(15) 2 . ? O1 Nd1 N3 62.75(16) . . ? N3 Nd1 N3 120.000(1) 2 . ? O1 Nd1 N3 62.75(16) 3 3 ? O1 Nd1 N3 72.04(17) 2 3 ? O1 Nd1 N3 140.40(15) . 3 ? N3 Nd1 N3 119.999(3) 2 3 ? N3 Nd1 N3 119.999(3) . 3 ? O1 Nd1 N2 124.91(17) 3 3 ? O1 Nd1 N2 77.72(15) 2 3 ? O1 Nd1 N2 143.08(18) . 3 ? N3 Nd1 N2 71.08(18) 2 3 ? N3 Nd1 N2 141.88(15) . 3 ? N3 Nd1 N2 62.19(18) 3 3 ? O1 Nd1 N2 77.72(15) 3 . ? O1 Nd1 N2 143.08(18) 2 . ? O1 Nd1 N2 124.91(17) . . ? N3 Nd1 N2 141.88(15) 2 . ? N3 Nd1 N2 62.19(18) . . ? N3 Nd1 N2 71.08(18) 3 . ? N2 Nd1 N2 86.66(15) 3 . ? O1 Nd1 N2 143.08(18) 3 2 ? O1 Nd1 N2 124.91(17) 2 2 ? O1 Nd1 N2 77.72(15) . 2 ? N3 Nd1 N2 62.19(18) 2 2 ? N3 Nd1 N2 71.08(18) . 2 ? N3 Nd1 N2 141.88(15) 3 2 ? N2 Nd1 N2 86.66(15) 3 2 ? N2 Nd1 N2 86.66(15) . 2 ? C13 O1 Nd1 121.6(4) . . ? C5 N1 N2 111.7(6) . . ? C5 N1 C4 126.1(6) . . ? N2 N1 C4 121.8(6) . . ? N1 N2 C7 103.7(5) . . ? N1 N2 Nd1 134.3(5) . . ? C7 N2 Nd1 115.7(4) . . ? C12 N3 C8 118.1(6) . . ? C12 N3 Nd1 118.9(4) . . ? C8 N3 Nd1 121.7(4) . . ? C13 N4 C16 117.5(5) . . ? C13 N4 C14 126.2(6) . . ? C16 N4 C14 115.5(5) . . ? C1 C1 C2 121.2(4) 10_556 . ? C1 C1 H1 119.4 10_556 . ? C2 C1 H1 119.4 . . ? C1 C2 C3 118.6(6) . . ? C1 C2 C4 120.3(6) . . ? C3 C2 C4 121.0(6) . . ? C2 C3 C3 120.2(4) . 10_556 ? C2 C3 H3 119.9 . . ? C3 C3 H3 119.9 10_556 . ? N1 C4 C2 114.1(6) . . ? N1 C4 H4A 108.7 . . ? C2 C4 H4A 108.7 . . ? N1 C4 H4B 108.7 . . ? C2 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? N1 C5 C6 107.7(6) . . ? N1 C5 H5 126.2 . . ? C6 C5 H5 126.2 . . ? C7 C6 C5 104.0(7) . . ? C7 C6 H6 128.0 . . ? C5 C6 H6 128.0 . . ? N2 C7 C6 112.9(6) . . ? N2 C7 C8 118.2(6) . . ? C6 C7 C8 128.9(7) . . ? N3 C8 C9 122.9(6) . . ? N3 C8 C7 116.4(6) . . ? C9 C8 C7 120.7(6) . . ? C8 C9 C10 118.4(6) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C11 C10 C9 118.3(7) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C10 C11 C12 120.3(7) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? N3 C12 C11 122.0(6) . . ? N3 C12 C13 110.4(6) . . ? C11 C12 C13 127.3(6) . . ? O1 C13 N4 122.2(6) . . ? O1 C13 C12 116.0(6) . . ? N4 C13 C12 121.8(6) . . ? N4 C14 C15 111.1(6) . . ? N4 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N4 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C17 113.1(6) . . ? N4 C16 H16A 109.0 . . ? C17 C16 H16A 109.0 . . ? N4 C16 H16B 109.0 . . ? C17 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O3 Cl1 O3 109.8(2) 3_665 . ? O3 Cl1 O3 109.8(2) 3_665 2_655 ? O3 Cl1 O3 109.8(2) . 2_655 ? O3 Cl1 O2 109.1(2) 3_665 . ? O3 Cl1 O2 109.1(2) . . ? O3 Cl1 O2 109.1(2) 2_655 . ? O8 Cl3 O7 116.7(16) . . ? O8 Cl3 O10 104.1(18) . . ? O7 Cl3 O10 107.9(15) . . ? O8 Cl3 O9 112.9(18) . . ? O7 Cl3 O9 101.4(17) . . ? O10 Cl3 O9 114.2(14) . . ? O5 Cl2 O4 122.0(10) . 2_655 ? O5 Cl2 O4 122.0(10) . 3_665 ? O4 Cl2 O4 94.6(13) 2_655 3_665 ? O5 Cl2 O4 122.0(10) . . ? O4 Cl2 O4 94.6(13) 2_655 . ? O4 Cl2 O4 94.6(13) 3_665 . ? O5' Cl2' O4' 115.2(10) . 3_665 ? O5' Cl2' O4' 115.2(10) . 2_655 ? O4' Cl2' O4' 103.1(12) 3_665 2_655 ? O5' Cl2' O4' 115.2(10) . . ? O4' Cl2' O4' 103.1(12) 3_665 . ? O4' Cl2' O4' 103.1(12) 2_655 . ? 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 Nd1 O1 C13 97.3(6) 3 . . . ? O1 Nd1 O1 C13 -178.0(5) 2 . . . ? N3 Nd1 O1 C13 -114.8(5) 2 . . . ? N3 Nd1 O1 C13 24.5(5) . . . . ? N3 Nd1 O1 C13 129.5(5) 3 . . . ? N2 Nd1 O1 C13 -117.5(5) 3 . . . ? N2 Nd1 O1 C13 26.7(5) . . . . ? N2 Nd1 O1 C13 -50.4(5) 2 . . . ? C5 N1 N2 C7 -1.0(7) . . . . ? C4 N1 N2 C7 -174.5(6) . . . . ? C5 N1 N2 Nd1 -150.7(5) . . . . ? C4 N1 N2 Nd1 35.8(8) . . . . ? O1 Nd1 N2 N1 91.6(5) 3 . . . ? O1 Nd1 N2 N1 29.1(6) 2 . . . ? O1 Nd1 N2 N1 165.4(5) . . . . ? N3 Nd1 N2 N1 -88.3(6) 2 . . . ? N3 Nd1 N2 N1 167.6(6) . . . . ? N3 Nd1 N2 N1 26.5(5) 3 . . . ? N2 Nd1 N2 N1 -35.3(6) 3 . . . ? N2 Nd1 N2 N1 -122.1(5) 2 . . . ? O1 Nd1 N2 C7 -55.5(5) 3 . . . ? O1 Nd1 N2 C7 -117.9(5) 2 . . . ? O1 Nd1 N2 C7 18.4(5) . . . . ? N3 Nd1 N2 C7 124.6(5) 2 . . . ? N3 Nd1 N2 C7 20.5(4) . . . . ? N3 Nd1 N2 C7 -120.6(5) 3 . . . ? N2 Nd1 N2 C7 177.7(5) 3 . . . ? N2 Nd1 N2 C7 90.9(6) 2 . . . ? O1 Nd1 N3 C12 -98.3(5) 3 . . . ? O1 Nd1 N3 C12 -42.3(6) 2 . . . ? O1 Nd1 N3 C12 -5.6(4) . . . . ? N3 Nd1 N3 C12 40.1(6) 2 . . . ? N3 Nd1 N3 C12 -140.3(4) 3 . . . ? N2 Nd1 N3 C12 137.5(4) 3 . . . ? N2 Nd1 N3 C12 176.4(5) . . . . ? N2 Nd1 N3 C12 80.0(5) 2 . . . ? O1 Nd1 N3 C8 68.7(4) 3 . . . ? O1 Nd1 N3 C8 124.7(4) 2 . . . ? O1 Nd1 N3 C8 161.4(5) . . . . ? N3 Nd1 N3 C8 -152.8(4) 2 . . . ? N3 Nd1 N3 C8 26.7(6) 3 . . . ? N2 Nd1 N3 C8 -55.4(6) 3 . . . ? N2 Nd1 N3 C8 -16.6(4) . . . . ? N2 Nd1 N3 C8 -113.0(5) 2 . . . ? C1 C1 C2 C3 1.9(10) 10_556 . . . ? C1 C1 C2 C4 176.9(4) 10_556 . . . ? C1 C2 C3 C3 -1.8(10) . . . 10_556 ? C4 C2 C3 C3 -176.8(4) . . . 10_556 ? C5 N1 C4 C2 -57.1(9) . . . . ? N2 N1 C4 C2 115.4(7) . . . . ? C1 C2 C4 N1 146.2(8) . . . . ? C3 C2 C4 N1 -38.9(10) . . . . ? N2 N1 C5 C6 -0.1(9) . . . . ? C4 N1 C5 C6 173.1(7) . . . . ? N1 C5 C6 C7 1.1(9) . . . . ? N1 N2 C7 C6 1.7(8) . . . . ? Nd1 N2 C7 C6 158.1(5) . . . . ? N1 N2 C7 C8 179.2(6) . . . . ? Nd1 N2 C7 C8 -24.4(8) . . . . ? C5 C6 C7 N2 -1.7(9) . . . . ? C5 C6 C7 C8 -178.9(7) . . . . ? C12 N3 C8 C9 0.1(9) . . . . ? Nd1 N3 C8 C9 -167.0(5) . . . . ? C12 N3 C8 C7 178.6(6) . . . . ? Nd1 N3 C8 C7 11.4(7) . . . . ? N2 C7 C8 N3 9.7(9) . . . . ? C6 C7 C8 N3 -173.3(7) . . . . ? N2 C7 C8 C9 -171.8(6) . . . . ? C6 C7 C8 C9 5.2(11) . . . . ? N3 C8 C9 C10 1.6(10) . . . . ? C7 C8 C9 C10 -176.8(6) . . . . ? C8 C9 C10 C11 -0.8(11) . . . . ? C9 C10 C11 C12 -1.6(11) . . . . ? C8 N3 C12 C11 -2.6(9) . . . . ? Nd1 N3 C12 C11 164.9(5) . . . . ? C8 N3 C12 C13 -176.4(5) . . . . ? Nd1 N3 C12 C13 -8.9(7) . . . . ? C10 C11 C12 N3 3.4(10) . . . . ? C10 C11 C12 C13 176.1(7) . . . . ? Nd1 O1 C13 N4 141.2(5) . . . . ? Nd1 O1 C13 C12 -39.7(7) . . . . ? C16 N4 C13 O1 5.5(9) . . . . ? C14 N4 C13 O1 -164.1(6) . . . . ? C16 N4 C13 C12 -173.6(6) . . . . ? C14 N4 C13 C12 16.8(10) . . . . ? N3 C12 C13 O1 30.1(8) . . . . ? C11 C12 C13 O1 -143.2(7) . . . . ? N3 C12 C13 N4 -150.7(6) . . . . ? C11 C12 C13 N4 35.9(10) . . . . ? C13 N4 C14 C15 -119.5(7) . . . . ? C16 N4 C14 C15 70.7(7) . . . . ? C13 N4 C16 C17 76.1(7) . . . . ? C14 N4 C16 C17 -113.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.822 _refine_diff_density_min -1.723 _refine_diff_density_rms 0.209 #===END data_imw334 _database_code_depnum_ccdc_archive 'CCDC 630961' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H114 Cl6 La2 N24 O30' _chemical_formula_weight 2646.69 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 13.8557(4) _cell_length_b 13.8557(4) _cell_length_c 40.129(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6671.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5280 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 21.04 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2700 _exptl_absorpt_coefficient_mu 0.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8655 _exptl_absorpt_correction_T_max 0.9677 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76518 _diffrn_reflns_av_R_equivalents 0.1334 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 26.43 _reflns_number_total 4661 _reflns_number_gt 3598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1535P)^2^+114.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4661 _refine_ls_number_parameters 239 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.1445 _refine_ls_R_factor_gt 0.1191 _refine_ls_wR_factor_ref 0.3344 _refine_ls_wR_factor_gt 0.3149 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.186 _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 La1 La 0.0000 0.0000 0.39899(2) 0.0221(3) Uani 1 3 d S . . O1 O -0.0476(7) 0.1115(7) 0.4361(2) 0.0227(19) Uani 1 1 d . . . N1 N 0.2333(9) 0.0528(10) 0.3386(3) 0.033(3) Uani 1 1 d . . . N2 N 0.1793(8) 0.0960(10) 0.3569(2) 0.0200(19) Uani 1 1 d . . . N3 N 0.1292(9) 0.2215(9) 0.3978(2) 0.024(2) Uani 1 1 d . . . N4 N -0.0821(10) 0.2546(9) 0.4365(3) 0.028(2) Uani 1 1 d . . . C1 C 0.1777(12) -0.1352(10) 0.2664(3) 0.031(2) Uani 1 1 d U . . H1 H 0.1779 -0.1938 0.2777 0.037 Uiso 1 1 calc R . . C2 C 0.1775(13) -0.0473(11) 0.2854(3) 0.031(2) Uani 1 1 d U . . C3 C 0.1771(13) 0.0411(13) 0.2673(4) 0.036(3) Uani 1 1 d . . . H3 H 0.1768 0.0992 0.2788 0.043 Uiso 1 1 calc R . . C4 C 0.1711(13) -0.0561(12) 0.3227(3) 0.036(3) Uani 1 1 d . . . H4A H 0.0937 -0.0914 0.3295 0.043 Uiso 1 1 calc R . . H4B H 0.2008 -0.1028 0.3300 0.043 Uiso 1 1 calc R . . C5 C 0.3442(14) 0.1313(15) 0.3340(5) 0.051(4) Uani 1 1 d U . . H5 H 0.3968 0.1220 0.3222 0.062 Uiso 1 1 calc R . . C6 C 0.3616(14) 0.2260(17) 0.3503(5) 0.049(4) Uani 1 1 d U . . H6 H 0.4274 0.2944 0.3510 0.059 Uiso 1 1 calc R . . C7 C 0.2635(12) 0.1994(13) 0.3650(3) 0.029(3) Uani 1 1 d . . . C8 C 0.2315(11) 0.2687(11) 0.3852(3) 0.023(3) Uani 1 1 d . . . C9 C 0.3099(10) 0.3804(12) 0.3912(3) 0.028(3) Uani 1 1 d . . . H9 H 0.3813 0.4125 0.3823 0.034 Uiso 1 1 calc R . . C10 C 0.2779(14) 0.4430(12) 0.4112(4) 0.038(4) Uani 1 1 d . . . H10 H 0.3278 0.5179 0.4153 0.045 Uiso 1 1 calc R . . C11 C 0.1755(10) 0.3945(11) 0.4243(4) 0.028(3) Uani 1 1 d . . . H11 H 0.1554 0.4348 0.4383 0.034 Uiso 1 1 calc R . . C12 C 0.0980(10) 0.2826(11) 0.4169(3) 0.023(3) Uani 1 1 d . . . C13 C -0.0201(9) 0.2132(10) 0.4304(3) 0.020(2) Uani 1 1 d . . . C14 C -0.0665(12) 0.3619(11) 0.4241(4) 0.031(3) Uani 1 1 d . . . H14A H -0.1319 0.3479 0.4115 0.037 Uiso 1 1 calc R . . H14B H -0.0032 0.3948 0.4091 0.037 Uiso 1 1 calc R . . C15 C -0.0477(13) 0.4445(11) 0.4515(4) 0.034(3) Uani 1 1 d . . . H15A H -0.1137 0.4166 0.4649 0.051 Uiso 1 1 calc R . . H15B H -0.0311 0.5145 0.4418 0.051 Uiso 1 1 calc R . . H15C H 0.0137 0.4548 0.4652 0.051 Uiso 1 1 calc R . . C16 C -0.1899(13) 0.1803(13) 0.4529(3) 0.032(3) Uani 1 1 d . . . H16A H -0.2233 0.1073 0.4426 0.039 Uiso 1 1 calc R . . H16B H -0.2396 0.2096 0.4494 0.039 Uiso 1 1 calc R . . C17 C -0.1796(16) 0.1676(14) 0.4894(3) 0.039(3) Uani 1 1 d . . . H17A H -0.1341 0.1344 0.4932 0.059 Uiso 1 1 calc R . . H17B H -0.2523 0.1208 0.4988 0.059 Uiso 1 1 calc R . . H17C H -0.1458 0.2396 0.4999 0.059 Uiso 1 1 calc R . . Cl1 Cl 0.6667 0.3333 0.51450(11) 0.0196(9) Uiso 1 3 d S . . O2 O 0.6667 0.3333 0.4776(2) 0.046(4) Uiso 1 3 d SD . . O3 O 0.7799(7) 0.3937(9) 0.52654(18) 0.0286(18) Uiso 1 1 d D . . Cl3 Cl 0.4271(13) 0.6275(14) 0.3389(4) 0.080 Uiso 0.33 1 d PD A -1 O7 O 0.481(3) 0.723(2) 0.3180(7) 0.074 Uiso 0.33 1 d PD A -1 O8 O 0.376(3) 0.526(2) 0.3202(8) 0.098 Uiso 0.33 1 d PD A -1 O9 O 0.516(2) 0.625(3) 0.3560(8) 0.080 Uiso 0.33 1 d PD A -1 O10 O 0.350(3) 0.634(3) 0.3610(7) 0.080 Uiso 0.33 1 d PD A -1 Cl2 Cl 0.6667 0.3333 0.3623(3) 0.065 Uiso 0.688(15) 3 d SPDU . 1 O4 O 0.632(2) 0.402(2) 0.3465(3) 0.089 Uiso 0.688(15) 1 d PDU . 1 O5 O 0.6667 0.3333 0.3971(3) 0.080 Uiso 0.688(15) 3 d SPD . 1 Cl2' Cl 0.6667 0.3333 0.3472(7) 0.068 Uiso 0.312(15) 3 d SPDU . 2 O4' O 0.634(5) 0.403(4) 0.3629(7) 0.081 Uiso 0.312(15) 1 d PDU . 2 O5' O 0.6667 0.3333 0.3123(7) 0.088 Uiso 0.312(15) 3 d SPD . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0227(4) 0.0227(4) 0.0210(5) 0.000 0.000 0.0114(2) O1 0.018(4) 0.022(4) 0.025(4) 0.000(3) 0.003(3) 0.008(4) N1 0.009(5) 0.020(6) 0.056(8) -0.009(6) 0.008(5) -0.005(5) N2 0.022(5) 0.012(5) 0.022(4) -0.006(4) 0.001(4) 0.006(5) N3 0.023(6) 0.025(5) 0.030(5) -0.001(4) 0.001(4) 0.017(5) N4 0.030(6) 0.023(6) 0.033(6) -0.006(5) 0.003(5) 0.015(5) C1 0.048(6) 0.017(5) 0.034(5) -0.001(4) -0.001(5) 0.021(5) C2 0.045(6) 0.018(5) 0.032(5) -0.001(4) 0.000(5) 0.019(5) C3 0.046(9) 0.035(8) 0.036(8) -0.005(6) 0.000(7) 0.027(7) C4 0.038(8) 0.029(8) 0.028(7) -0.013(6) 0.002(6) 0.008(7) C5 0.024(6) 0.054(7) 0.071(10) -0.024(6) 0.003(6) 0.015(6) C6 0.022(6) 0.052(7) 0.070(10) -0.024(6) 0.003(6) 0.016(6) C7 0.028(7) 0.040(8) 0.029(7) -0.010(6) -0.005(6) 0.025(7) C8 0.017(6) 0.027(7) 0.027(6) 0.002(5) -0.001(5) 0.014(5) C9 0.009(6) 0.030(7) 0.032(7) 0.005(6) 0.000(5) 0.000(5) C10 0.041(9) 0.019(7) 0.041(8) -0.008(6) 0.004(7) 0.005(7) C11 0.017(7) 0.027(7) 0.042(7) 0.001(6) 0.005(5) 0.013(5) C12 0.013(6) 0.027(7) 0.029(6) 0.002(5) 0.003(5) 0.010(6) C13 0.007(6) 0.012(5) 0.032(6) 0.000(5) 0.005(5) -0.003(4) C14 0.021(7) 0.021(7) 0.042(8) -0.001(6) 0.000(6) 0.005(6) C15 0.032(8) 0.018(6) 0.048(8) -0.005(6) 0.006(7) 0.009(6) C16 0.025(8) 0.023(7) 0.045(7) -0.012(7) -0.006(7) 0.010(5) C17 0.052(11) 0.022(8) 0.044(7) -0.013(8) 0.005(9) 0.019(6) _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 La1 O1 2.461(9) . ? La1 O1 2.461(9) 3 ? La1 O1 2.461(9) 2 ? La1 N3 2.671(11) 2 ? La1 N3 2.671(11) . ? La1 N3 2.671(11) 3 ? La1 N2 2.737(9) 2 ? La1 N2 2.737(9) 3 ? La1 N2 2.737(9) . ? O1 C13 1.283(15) . ? N1 N2 1.380(16) . ? N1 C5 1.38(2) . ? N1 C4 1.458(17) . ? N2 C7 1.361(18) . ? N3 C8 1.330(16) . ? N3 C12 1.360(16) . ? N4 C13 1.273(16) . ? N4 C14 1.478(18) . ? N4 C16 1.48(2) . ? C1 C1 1.32(3) 10_556 ? C1 C2 1.437(18) . ? C1 H1 0.9300 . ? C2 C3 1.426(19) . ? C2 C4 1.499(19) . ? C3 C3 1.39(3) 10_556 ? C3 H3 0.9300 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.38(2) . ? C5 H5 0.9300 . ? C6 C7 1.35(2) . ? C6 H6 0.9300 . ? C7 C8 1.482(17) . ? C8 C9 1.398(19) . ? C9 C10 1.41(2) . ? C9 H9 0.9300 . ? C10 C11 1.34(2) . ? C10 H10 0.9300 . ? C11 C12 1.407(18) . ? C11 H11 0.9300 . ? C12 C13 1.525(16) . ? C14 C15 1.512(19) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.491(19) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? Cl1 O3 1.443(8) . ? Cl1 O3 1.443(8) 3_665 ? Cl1 O3 1.443(8) 2_655 ? Cl1 O2 1.481(11) . ? Cl3 O9 1.422(5) . ? Cl3 O7 1.427(5) . ? Cl3 O10 1.428(5) . ? Cl3 O8 1.428(5) . ? Cl2 O5 1.396(5) . ? Cl2 O4 1.408(5) 2_655 ? Cl2 O4 1.408(5) 3_665 ? Cl2 O4 1.408(5) . ? Cl2' O5' 1.399(5) . ? Cl2' O4' 1.405(5) 3_665 ? Cl2' O4' 1.405(5) 2_655 ? Cl2' O4' 1.405(5) . ? 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 La1 O1 87.2(3) . 3 ? O1 La1 O1 87.2(3) . 2 ? O1 La1 O1 87.2(3) 3 2 ? O1 La1 N3 73.0(3) . 2 ? O1 La1 N3 143.1(3) 3 2 ? O1 La1 N3 61.7(3) 2 2 ? O1 La1 N3 61.7(3) . . ? O1 La1 N3 73.0(3) 3 . ? O1 La1 N3 143.1(3) 2 . ? N3 La1 N3 119.970(14) 2 . ? O1 La1 N3 143.1(3) . 3 ? O1 La1 N3 61.7(3) 3 3 ? O1 La1 N3 73.0(3) 2 3 ? N3 La1 N3 119.970(14) 2 3 ? N3 La1 N3 119.970(15) . 3 ? O1 La1 N2 76.7(3) . 2 ? O1 La1 N2 145.0(3) 3 2 ? O1 La1 N2 122.1(3) 2 2 ? N3 La1 N2 60.5(3) 2 2 ? N3 La1 N2 72.1(3) . 2 ? N3 La1 N2 140.2(3) 3 2 ? O1 La1 N2 145.0(3) . 3 ? O1 La1 N2 122.1(3) 3 3 ? O1 La1 N2 76.7(3) 2 3 ? N3 La1 N2 72.1(3) 2 3 ? N3 La1 N2 140.2(3) . 3 ? N3 La1 N2 60.5(3) 3 3 ? N2 La1 N2 85.9(3) 2 3 ? O1 La1 N2 122.1(3) . . ? O1 La1 N2 76.7(3) 3 . ? O1 La1 N2 145.0(3) 2 . ? N3 La1 N2 140.2(3) 2 . ? N3 La1 N2 60.5(3) . . ? N3 La1 N2 72.1(3) 3 . ? N2 La1 N2 85.9(3) 2 . ? N2 La1 N2 85.9(3) 3 . ? C13 O1 La1 123.8(7) . . ? N2 N1 C5 111.1(11) . . ? N2 N1 C4 120.9(11) . . ? C5 N1 C4 127.3(13) . . ? C7 N2 N1 102.6(10) . . ? C7 N2 La1 117.1(8) . . ? N1 N2 La1 132.4(8) . . ? C8 N3 C12 120.1(11) . . ? C8 N3 La1 120.6(8) . . ? C12 N3 La1 117.8(8) . . ? C13 N4 C14 126.7(12) . . ? C13 N4 C16 116.5(11) . . ? C14 N4 C16 116.0(11) . . ? C1 C1 C2 122.0(7) 10_556 . ? C1 C1 H1 119.0 10_556 . ? C2 C1 H1 119.0 . . ? C3 C2 C1 117.4(12) . . ? C3 C2 C4 123.5(13) . . ? C1 C2 C4 119.0(12) . . ? C3 C3 C2 120.6(8) 10_556 . ? C3 C3 H3 119.7 10_556 . ? C2 C3 H3 119.7 . . ? N1 C4 C2 111.8(12) . . ? N1 C4 H4A 109.3 . . ? C2 C4 H4A 109.3 . . ? N1 C4 H4B 109.3 . . ? C2 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C6 C5 N1 106.5(14) . . ? C6 C5 H5 126.8 . . ? N1 C5 H5 126.8 . . ? C7 C6 C5 105.9(16) . . ? C7 C6 H6 127.0 . . ? C5 C6 H6 127.0 . . ? N2 C7 C6 113.4(13) . . ? N2 C7 C8 115.9(12) . . ? C6 C7 C8 130.3(15) . . ? N3 C8 C9 121.7(12) . . ? N3 C8 C7 118.7(12) . . ? C9 C8 C7 119.6(12) . . ? C8 C9 C10 118.2(12) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? C11 C10 C9 119.8(13) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 120.3(13) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? N3 C12 C11 119.9(11) . . ? N3 C12 C13 112.5(11) . . ? C11 C12 C13 127.3(11) . . ? N4 C13 O1 124.4(11) . . ? N4 C13 C12 122.5(11) . . ? O1 C13 C12 113.1(10) . . ? N4 C14 C15 113.6(12) . . ? N4 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? N4 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C17 113.4(13) . . ? N4 C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? N4 C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O3 Cl1 O3 109.4(4) . 3_665 ? O3 Cl1 O3 109.4(4) . 2_655 ? O3 Cl1 O3 109.4(4) 3_665 2_655 ? O3 Cl1 O2 109.6(4) . . ? O3 Cl1 O2 109.6(4) 3_665 . ? O3 Cl1 O2 109.6(4) 2_655 . ? O9 Cl3 O7 104.1(9) . . ? O9 Cl3 O10 112.7(5) . . ? O7 Cl3 O10 111.7(5) . . ? O9 Cl3 O8 103.9(9) . . ? O7 Cl3 O8 112.4(4) . . ? O10 Cl3 O8 111.6(5) . . ? O5 Cl2 O4 116.8(6) . 2_655 ? O5 Cl2 O4 116.8(6) . 3_665 ? O4 Cl2 O4 101.3(7) 2_655 3_665 ? O5 Cl2 O4 116.8(6) . . ? O4 Cl2 O4 101.3(7) 2_655 . ? O4 Cl2 O4 101.3(7) 3_665 . ? O5' Cl2' O4' 116.8(6) . 3_665 ? O5' Cl2' O4' 116.8(6) . 2_655 ? O4' Cl2' O4' 101.3(8) 3_665 2_655 ? O5' Cl2' O4' 116.8(6) . . ? O4' Cl2' O4' 101.3(8) 3_665 . ? O4' Cl2' O4' 101.3(8) 2_655 . ? 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 La1 O1 C13 97.3(10) 3 . . . ? O1 La1 O1 C13 -175.4(9) 2 . . . ? N3 La1 O1 C13 -114.2(9) 2 . . . ? N3 La1 O1 C13 25.2(8) . . . . ? N3 La1 O1 C13 128.3(9) 3 . . . ? N2 La1 O1 C13 -51.4(9) 2 . . . ? N2 La1 O1 C13 -113.6(9) 3 . . . ? N2 La1 O1 C13 25.0(10) . . . . ? C5 N1 N2 C7 -4.4(17) . . . . ? C4 N1 N2 C7 -175.6(13) . . . . ? C5 N1 N2 La1 -151.3(11) . . . . ? C4 N1 N2 La1 37.5(18) . . . . ? O1 La1 N2 C7 23.6(11) . . . . ? O1 La1 N2 C7 -54.4(9) 3 . . . ? O1 La1 N2 C7 -119.1(10) 2 . . . ? N3 La1 N2 C7 125.9(9) 2 . . . ? N3 La1 N2 C7 23.4(9) . . . . ? N3 La1 N2 C7 -118.5(10) 3 . . . ? N2 La1 N2 C7 95.1(12) 2 . . . ? N2 La1 N2 C7 -178.7(11) 3 . . . ? O1 La1 N2 N1 166.9(10) . . . . ? O1 La1 N2 N1 88.9(11) 3 . . . ? O1 La1 N2 N1 24.2(13) 2 . . . ? N3 La1 N2 N1 -90.8(12) 2 . . . ? N3 La1 N2 N1 166.7(11) . . . . ? N3 La1 N2 N1 24.8(10) 3 . . . ? N2 La1 N2 N1 -121.6(9) 2 . . . ? N2 La1 N2 N1 -35.4(11) 3 . . . ? O1 La1 N3 C8 161.5(10) . . . . ? O1 La1 N3 C8 65.4(9) 3 . . . ? O1 La1 N3 C8 125.7(9) 2 . . . ? N3 La1 N3 C8 -152.6(7) 2 . . . ? N3 La1 N3 C8 24.0(12) 3 . . . ? N2 La1 N3 C8 -114.3(9) 2 . . . ? N2 La1 N3 C8 -54.7(11) 3 . . . ? N2 La1 N3 C8 -18.7(8) . . . . ? O1 La1 N3 C12 -4.1(8) . . . . ? O1 La1 N3 C12 -100.3(9) 3 . . . ? O1 La1 N3 C12 -39.9(11) 2 . . . ? N3 La1 N3 C12 41.8(11) 2 . . . ? N3 La1 N3 C12 -141.7(7) 3 . . . ? N2 La1 N3 C12 80.1(9) 2 . . . ? N2 La1 N3 C12 139.7(8) 3 . . . ? N2 La1 N3 C12 175.6(10) . . . . ? C1 C1 C2 C3 0.1(18) 10_556 . . . ? C1 C1 C2 C4 176.6(10) 10_556 . . . ? C1 C2 C3 C3 -0.1(18) . . . 10_556 ? C4 C2 C3 C3 -176.5(11) . . . 10_556 ? N2 N1 C4 C2 114.3(15) . . . . ? C5 N1 C4 C2 -55(2) . . . . ? C3 C2 C4 N1 -37(2) . . . . ? C1 C2 C4 N1 146.6(15) . . . . ? N2 N1 C5 C6 1(2) . . . . ? C4 N1 C5 C6 171.6(16) . . . . ? N1 C5 C6 C7 3(2) . . . . ? N1 N2 C7 C6 6.3(17) . . . . ? La1 N2 C7 C6 159.4(12) . . . . ? N1 N2 C7 C8 179.9(11) . . . . ? La1 N2 C7 C8 -27.0(15) . . . . ? C5 C6 C7 N2 -6(2) . . . . ? C5 C6 C7 C8 -178.2(15) . . . . ? C12 N3 C8 C9 0.9(18) . . . . ? La1 N3 C8 C9 -164.4(10) . . . . ? C12 N3 C8 C7 178.9(12) . . . . ? La1 N3 C8 C7 13.7(15) . . . . ? N2 C7 C8 N3 9.6(18) . . . . ? C6 C7 C8 N3 -178.2(16) . . . . ? N2 C7 C8 C9 -172.3(12) . . . . ? C6 C7 C8 C9 0(2) . . . . ? N3 C8 C9 C10 0(2) . . . . ? C7 C8 C9 C10 -178.2(13) . . . . ? C8 C9 C10 C11 1(2) . . . . ? C9 C10 C11 C12 -3(2) . . . . ? C8 N3 C12 C11 -2.6(18) . . . . ? La1 N3 C12 C11 163.1(10) . . . . ? C8 N3 C12 C13 -177.3(11) . . . . ? La1 N3 C12 C13 -11.6(13) . . . . ? C10 C11 C12 N3 4(2) . . . . ? C10 C11 C12 C13 177.6(14) . . . . ? C14 N4 C13 O1 -165.7(12) . . . . ? C16 N4 C13 O1 3.7(19) . . . . ? C14 N4 C13 C12 17(2) . . . . ? C16 N4 C13 C12 -173.7(11) . . . . ? La1 O1 C13 N4 141.6(11) . . . . ? La1 O1 C13 C12 -40.8(13) . . . . ? N3 C12 C13 N4 -150.4(12) . . . . ? C11 C12 C13 N4 35(2) . . . . ? N3 C12 C13 O1 31.9(15) . . . . ? C11 C12 C13 O1 -142.3(14) . . . . ? C13 N4 C14 C15 -117.6(15) . . . . ? C16 N4 C14 C15 73.0(15) . . . . ? C13 N4 C16 C17 78.2(15) . . . . ? C14 N4 C16 C17 -111.3(13) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.418 _refine_diff_density_min -2.643 _refine_diff_density_rms 0.285 #===END data_src0057 _database_code_depnum_ccdc_archive 'CCDC 630962' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C146 H196 Cl12 N37 Nd4 O69.50' _chemical_formula_weight 4583.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 21.7720(2) _cell_length_b 22.2268(3) _cell_length_c 24.6165(3) _cell_angle_alpha 69.8650(10) _cell_angle_beta 83.7540(10) _cell_angle_gamma 70.5190(10) _cell_volume 10543.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 46550 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4662 _exptl_absorpt_coefficient_mu 1.209 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6184 _exptl_absorpt_correction_T_max 0.9880 _exptl_absorpt_process_details 'sadabs v2.10 (G. M. Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 190146 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 37016 _reflns_number_gt 29177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (R. W. W. Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997; and COLLECT' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997; and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1511P)^2^+74.6899P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 37016 _refine_ls_number_parameters 2225 _refine_ls_number_restraints 401 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.2673 _refine_ls_wR_factor_gt 0.2427 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 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 Nd1 Nd 0.77834(3) 0.27187(3) 0.76404(2) 0.04883(15) Uani 1 1 d . . . Nd2 Nd 0.87056(2) -0.26995(2) 0.874112(17) 0.03134(12) Uani 1 1 d . . . Nd3 Nd 1.39165(2) -0.34465(2) 0.747901(19) 0.03682(13) Uani 1 1 d . . . Nd4 Nd 1.27097(2) 0.21701(2) 0.60886(2) 0.04081(14) Uani 1 1 d . . . O101 O 0.7199(4) 0.3765(3) 0.7840(3) 0.0629(19) Uani 1 1 d . . . O102 O 0.9543(3) -0.3741(3) 0.9305(2) 0.0408(13) Uani 1 1 d . . . O201 O 0.7885(3) -0.3133(3) 0.9304(3) 0.0459(14) Uani 1 1 d . . . O202 O 1.4866(3) -0.3117(3) 0.7547(3) 0.0455(14) Uani 1 1 d . . . O301 O 1.4678(3) -0.4561(3) 0.7777(3) 0.0551(17) Uani 1 1 d . A . O302 O 1.2098(3) 0.3161(4) 0.6338(3) 0.0591(18) Uani 1 1 d . A . O402 O 0.7270(4) 0.2125(4) 0.8470(3) 0.0609(18) Uani 1 1 d . A . O501 O 0.8695(5) 0.3182(5) 0.7458(4) 0.085(3) Uani 1 1 d . . . N502 N 0.7547(6) 0.3711(7) 0.6685(5) 0.088(3) Uiso 1 1 d D . . C501 C 0.7321(11) 0.4260(12) 0.6384(10) 0.128(6) Uiso 1 1 d D . . C502 C 0.6961(16) 0.5006(16) 0.6029(15) 0.214(13) Uiso 1 1 d D . . H50A H 0.6771 0.5021 0.5680 0.320 Uiso 1 1 calc R . . H50B H 0.7271 0.5261 0.5919 0.320 Uiso 1 1 calc R . . H50C H 0.6615 0.5206 0.6264 0.320 Uiso 1 1 calc R . . O503 O 0.6642(4) 0.2996(4) 0.7338(4) 0.085(3) Uani 1 1 d . . . O504 O 0.8018(3) -0.1639(3) 0.8905(2) 0.0419(13) Uani 1 1 d . . . O505 O 0.7706(3) -0.2213(3) 0.8109(3) 0.0468(14) Uani 1 1 d . . . O506 O 0.8627(3) -0.3553(3) 0.8332(3) 0.0499(15) Uani 1 1 d . . . O507 O 1.3158(3) -0.3972(4) 0.8128(3) 0.0561(17) Uani 1 1 d . . . O508 O 1.3523(4) -0.4113(4) 0.7007(3) 0.0608(18) Uani 1 1 d . . . O509 O 1.4566(3) -0.3535(4) 0.6597(3) 0.0592(18) Uani 1 1 d . . . O510 O 1.3528(4) 0.1053(4) 0.6539(4) 0.079(3) Uani 1 1 d . A . O511 O 1.3442(4) 0.1765(4) 0.5323(4) 0.091(3) Uani 1 1 d . A . O512 O 1.2485(3) 0.3062(3) 0.5103(3) 0.0516(16) Uani 1 1 d . A . N101 N 0.7416(4) 0.4604(4) 0.8039(4) 0.063(2) Uani 1 1 d D . . N102 N 0.8089(4) 0.2840(4) 0.8596(4) 0.052(2) Uani 1 1 d . . . N103 N 0.8789(4) 0.1724(4) 0.8321(4) 0.0465(18) Uani 1 1 d . . . N104 N 0.9247(4) 0.1140(4) 0.8316(4) 0.0501(19) Uani 1 1 d . . . N105 N 0.8542(4) -0.1345(3) 0.7274(3) 0.0417(16) Uani 1 1 d . . . N106 N 0.8920(3) -0.1923(3) 0.7670(3) 0.0342(14) Uani 1 1 d . . . N107 N 0.9781(3) -0.3143(3) 0.8212(3) 0.0342(14) Uani 1 1 d . . . N108 N 1.0633(3) -0.4217(4) 0.9495(3) 0.0436(17) Uani 1 1 d D . . N201 N 0.7098(3) -0.3028(4) 0.9961(3) 0.0500(19) Uani 1 1 d D . . N202 N 0.8673(3) -0.2857(3) 0.9847(3) 0.0347(14) Uani 1 1 d . . . N203 N 0.9517(3) -0.2266(3) 0.9158(3) 0.0361(15) Uani 1 1 d . . . N204 N 0.9945(3) -0.1909(4) 0.8952(3) 0.0404(16) Uani 1 1 d . . . N205 N 1.2329(3) -0.2726(4) 0.6657(3) 0.0458(18) Uani 1 1 d . . . N206 N 1.2860(3) -0.2626(4) 0.6804(3) 0.0420(16) Uani 1 1 d . . . N207 N 1.3931(3) -0.2258(4) 0.6798(3) 0.0402(16) Uani 1 1 d . . . N208 N 1.5189(4) -0.2274(4) 0.7613(4) 0.054(2) Uani 1 1 d . . . N301 N 1.5113(5) -0.5578(4) 0.8414(3) 0.061(2) Uani 1 1 d D A . N302 N 1.4405(3) -0.3928(3) 0.8530(3) 0.0375(15) Uani 1 1 d . . . N303 N 1.3449(3) -0.2696(3) 0.8178(3) 0.0368(15) Uani 1 1 d . A . N304 N 1.2964(3) -0.2127(4) 0.8185(3) 0.0409(16) Uani 1 1 d . A . N305 N 1.2359(5) 0.0946(4) 0.5501(3) 0.056(2) Uani 1 1 d . . . N306 N 1.2153(4) 0.1492(3) 0.5684(3) 0.0398(16) Uani 1 1 d . A . N307 N 1.1462(3) 0.2711(3) 0.5828(3) 0.0371(15) Uani 1 1 d . A . N308 N 1.1197(4) 0.3845(5) 0.6614(4) 0.072(3) Uani 1 1 d D . . N403 N 1.2311(5) 0.1571(4) 0.7145(4) 0.060(2) Uani 1 1 d . A . N404 N 1.1934(6) 0.1160(5) 0.7387(4) 0.073(3) Uani 1 1 d . . . N405 N 0.8557(5) 0.2484(5) 0.6245(4) 0.073(3) Uani 1 1 d . A . N406 N 0.8257(4) 0.2247(4) 0.6763(4) 0.057(2) Uani 1 1 d . A . N407 N 0.7541(4) 0.1652(4) 0.7607(3) 0.0460(18) Uani 1 1 d . . . N408 N 0.7132(6) 0.1168(5) 0.9085(4) 0.084(3) Uani 1 1 d D A . C101 C 0.9088(4) 0.0500(4) 0.7719(4) 0.045(2) Uani 1 1 d . . . C102 C 0.9163(5) 0.0346(5) 0.7211(4) 0.055(2) Uani 1 1 d . . . H102 H 0.9433 0.0530 0.6916 0.066 Uiso 1 1 calc R . . C103 C 0.8861(5) -0.0063(5) 0.7120(4) 0.052(2) Uani 1 1 d . . . H103 H 0.8912 -0.0147 0.6762 0.062 Uiso 1 1 calc R . . C104 C 0.8475(4) -0.0357(4) 0.7556(4) 0.045(2) Uani 1 1 d . . . C105 C 0.8411(5) -0.0220(4) 0.8067(4) 0.046(2) Uani 1 1 d . . . H105 H 0.8151 -0.0416 0.8366 0.055 Uiso 1 1 calc R . . C106 C 0.8711(5) 0.0192(4) 0.8157(4) 0.048(2) Uani 1 1 d . . . H106 H 0.8664 0.0270 0.8518 0.058 Uiso 1 1 calc R . . C107 C 0.9410(5) 0.0971(5) 0.7781(5) 0.053(2) Uani 1 1 d . . . H10A H 0.9888 0.0764 0.7767 0.064 Uiso 1 1 calc R . . H10B H 0.9283 0.1394 0.7447 0.064 Uiso 1 1 calc R . . C108 C 0.9521(5) 0.0770(6) 0.8837(5) 0.062(3) Uani 1 1 d . . . H108 H 0.9855 0.0345 0.8927 0.074 Uiso 1 1 calc R . . C109 C 0.9241(5) 0.1106(5) 0.9215(5) 0.060(3) Uani 1 1 d . . . H109 H 0.9329 0.0966 0.9617 0.072 Uiso 1 1 calc R . . C110 C 0.8797(5) 0.1700(5) 0.8880(5) 0.051(2) Uani 1 1 d . . . C111 C 0.8404(5) 0.2302(5) 0.9032(5) 0.053(2) Uani 1 1 d . . . C112 C 0.8370(5) 0.2307(6) 0.9604(5) 0.063(3) Uani 1 1 d . . . H112 H 0.8576 0.1912 0.9912 0.076 Uiso 1 1 calc R . . C113 C 0.8028(5) 0.2904(6) 0.9702(6) 0.067(3) Uani 1 1 d . . . H113 H 0.7994 0.2927 1.0083 0.080 Uiso 1 1 calc R . . C114 C 0.7732(6) 0.3476(6) 0.9237(5) 0.067(3) Uani 1 1 d . . . H114 H 0.7502 0.3895 0.9295 0.080 Uiso 1 1 calc R . . C115 C 0.7782(5) 0.3419(5) 0.8694(5) 0.054(2) Uani 1 1 d . . . C116 C 0.7448(5) 0.3959(6) 0.8159(6) 0.066(3) Uani 1 1 d . . . C117 C 0.7828(6) 0.4852(7) 0.8298(6) 0.082(4) Uani 1 1 d D . . H11A H 0.8117 0.4467 0.8598 0.099 Uiso 1 1 calc R . . H11B H 0.8105 0.5056 0.7995 0.099 Uiso 1 1 calc R . . C118 C 0.7423(10) 0.5360(7) 0.8562(7) 0.109(6) Uani 1 1 d . . . H11C H 0.7162 0.5758 0.8261 0.163 Uiso 1 1 calc R . . H11D H 0.7705 0.5492 0.8752 0.163 Uiso 1 1 calc R . . H11E H 0.7132 0.5165 0.8849 0.163 Uiso 1 1 calc R . . C119 C 0.7031(6) 0.5108(6) 0.7521(4) 0.072(3) Uiso 1 1 d D . . H11F H 0.7113 0.4913 0.7204 0.087 Uiso 1 1 calc R . . H11G H 0.7176 0.5513 0.7391 0.087 Uiso 1 1 calc R . . C120 C 0.6312(7) 0.5315(8) 0.7643(7) 0.096(4) Uiso 1 1 d . . . H12A H 0.6158 0.4925 0.7735 0.143 Uiso 1 1 calc R . . H12B H 0.6079 0.5673 0.7302 0.143 Uiso 1 1 calc R . . H12C H 0.6232 0.5483 0.7973 0.143 Uiso 1 1 calc R . . C121 C 0.8103(5) -0.0776(4) 0.7455(4) 0.043(2) Uani 1 1 d . . . H12Y H 0.7878 -0.0957 0.7816 0.052 Uiso 1 1 calc R . . H12Z H 0.7767 -0.0485 0.7152 0.052 Uiso 1 1 calc R . . C122 C 0.8691(5) -0.1327(5) 0.6731(4) 0.052(2) Uani 1 1 d . . . H122 H 0.8496 -0.0972 0.6391 0.062 Uiso 1 1 calc R . . C123 C 0.9193(5) -0.1933(5) 0.6755(4) 0.047(2) Uani 1 1 d . . . H123 H 0.9404 -0.2075 0.6441 0.057 Uiso 1 1 calc R . . C124 C 0.9310(4) -0.2280(4) 0.7350(4) 0.0392(18) Uani 1 1 d . . . C125 C 0.9778(4) -0.2935(4) 0.7626(4) 0.0364(18) Uani 1 1 d . . . C126 C 1.0200(5) -0.3327(5) 0.7322(4) 0.046(2) Uani 1 1 d . . . H126 H 1.0200 -0.3166 0.6911 0.055 Uiso 1 1 calc R . . C127 C 1.0611(4) -0.3938(5) 0.7617(4) 0.049(2) Uani 1 1 d . . . H127 H 1.0884 -0.4217 0.7410 0.058 Uiso 1 1 calc R . . C128 C 1.0640(4) -0.4166(5) 0.8220(4) 0.044(2) Uani 1 1 d . . . H128 H 1.0936 -0.4589 0.8431 0.053 Uiso 1 1 calc R . . C129 C 1.0212(4) -0.3741(4) 0.8496(4) 0.0358(17) Uani 1 1 d . . . C130 C 1.0129(4) -0.3912(4) 0.9137(4) 0.0372(18) Uani 1 1 d . . . C131 C 1.0527(5) -0.4416(6) 1.0130(3) 0.059(3) Uani 1 1 d D . . H13A H 1.0663 -0.4915 1.0296 0.071 Uiso 1 1 calc R . . H13B H 1.0057 -0.4239 1.0208 0.071 Uiso 1 1 calc R . . C132 C 1.0906(6) -0.4151(7) 1.0421(5) 0.076(3) Uani 1 1 d . . . H13C H 1.1373 -0.4339 1.0357 0.114 Uiso 1 1 calc R . . H13D H 1.0819 -0.4285 1.0837 0.114 Uiso 1 1 calc R . . H13E H 1.0773 -0.3657 1.0258 0.114 Uiso 1 1 calc R . . C133 C 1.1327(3) -0.4352(5) 0.9318(4) 0.048(2) Uani 1 1 d D . . H13F H 1.1540 -0.4139 0.9500 0.057 Uiso 1 1 calc R . . H13G H 1.1352 -0.4149 0.8893 0.057 Uiso 1 1 calc R . . C134 C 1.1682(6) -0.5102(5) 0.9495(6) 0.070(3) Uani 1 1 d . . . H13H H 1.1688 -0.5297 0.9918 0.105 Uiso 1 1 calc R . . H13I H 1.2130 -0.5179 0.9352 0.105 Uiso 1 1 calc R . . H13J H 1.1459 -0.5316 0.9330 0.105 Uiso 1 1 calc R . . C201 C 1.0548(4) -0.1969(4) 0.8033(4) 0.0374(18) Uani 1 1 d . . . C202 C 1.0548(4) -0.1733(5) 0.7432(4) 0.048(2) Uani 1 1 d . . . H202 H 1.0227 -0.1326 0.7228 0.057 Uiso 1 1 calc R . . C203 C 1.1009(4) -0.2087(5) 0.7130(4) 0.048(2) Uani 1 1 d . . . H203 H 1.1006 -0.1922 0.6719 0.057 Uiso 1 1 calc R . . C204 C 1.1484(4) -0.2691(5) 0.7427(4) 0.0414(19) Uani 1 1 d . . . C205 C 1.1489(4) -0.2910(5) 0.8016(4) 0.0418(19) Uani 1 1 d . . . H205 H 1.1816 -0.3313 0.8220 0.050 Uiso 1 1 calc R . . C206 C 1.1029(4) -0.2560(4) 0.8321(4) 0.042(2) Uani 1 1 d . . . H206 H 1.1041 -0.2724 0.8732 0.051 Uiso 1 1 calc R . . C207 C 1.0007(4) -0.1564(5) 0.8335(4) 0.0415(19) Uani 1 1 d . . . H20A H 1.0085 -0.1135 0.8287 0.050 Uiso 1 1 calc R . . H20B H 0.9588 -0.1449 0.8141 0.050 Uiso 1 1 calc R . . C208 C 1.0273(5) -0.1916(5) 0.9386(4) 0.050(2) Uani 1 1 d . . . H208 H 1.0595 -0.1703 0.9344 0.060 Uiso 1 1 calc R . . C209 C 1.0070(5) -0.2275(5) 0.9887(4) 0.051(2) Uani 1 1 d . . . H209 H 1.0219 -0.2370 1.0265 0.061 Uiso 1 1 calc R . . C210 C 0.9590(4) -0.2478(4) 0.9733(4) 0.0393(18) Uani 1 1 d . . . C211 C 0.9172(4) -0.2846(4) 1.0107(3) 0.0394(19) Uani 1 1 d . . . C212 C 0.9282(5) -0.3172(5) 1.0702(4) 0.055(2) Uani 1 1 d . . . H212 H 0.9646 -0.3171 1.0882 0.066 Uiso 1 1 calc R . . C213 C 0.8862(5) -0.3491(5) 1.1019(4) 0.053(2) Uani 1 1 d . . . H213 H 0.8941 -0.3731 1.1420 0.064 Uiso 1 1 calc R . . C214 C 0.8319(5) -0.3466(5) 1.0756(4) 0.049(2) Uani 1 1 d . . . H214 H 0.8013 -0.3673 1.0976 0.059 Uiso 1 1 calc R . . C215 C 0.8232(4) -0.3134(4) 1.0170(4) 0.0381(18) Uani 1 1 d . . . C216 C 0.7711(4) -0.3098(4) 0.9793(4) 0.0405(19) Uani 1 1 d . . . C217 C 0.6810(6) -0.2912(8) 1.0506(5) 0.083(4) Uani 1 1 d D . . H21A H 0.6430 -0.2496 1.0412 0.099 Uiso 1 1 calc R . . H21B H 0.7136 -0.2843 1.0710 0.099 Uiso 1 1 calc R . . C218 C 0.6597(8) -0.3501(10) 1.0906(7) 0.107(6) Uani 1 1 d . . . H21C H 0.6370 -0.3651 1.0679 0.161 Uiso 1 1 calc R . . H21D H 0.6302 -0.3357 1.1200 0.161 Uiso 1 1 calc R . . H21E H 0.6980 -0.3875 1.1095 0.161 Uiso 1 1 calc R . . C219 C 0.6630(4) -0.3007(6) 0.9553(4) 0.059(3) Uani 1 1 d D . . H21F H 0.6180 -0.2797 0.9665 0.070 Uiso 1 1 calc R . . H21G H 0.6704 -0.2724 0.9158 0.070 Uiso 1 1 calc R . . C220 C 0.6702(6) -0.3693(6) 0.9550(6) 0.077(4) Uani 1 1 d . . . H22A H 0.7090 -0.3847 0.9330 0.116 Uiso 1 1 calc R . . H22B H 0.6316 -0.3682 0.9371 0.116 Uiso 1 1 calc R . . H22C H 0.6748 -0.4006 0.9949 0.116 Uiso 1 1 calc R . . C221 C 1.1967(4) -0.3112(5) 0.7097(4) 0.047(2) Uani 1 1 d . . . H22D H 1.2280 -0.3500 0.7375 0.057 Uiso 1 1 calc R . . H22E H 1.1728 -0.3294 0.6906 0.057 Uiso 1 1 calc R . . C222 C 1.2154(5) -0.2346(7) 0.6104(4) 0.066(3) Uani 1 1 d . . . H222 H 1.1792 -0.2329 0.5908 0.079 Uiso 1 1 calc R . . C223 C 1.2574(5) -0.1994(6) 0.5873(4) 0.059(3) Uani 1 1 d . . . H223 H 1.2570 -0.1688 0.5492 0.071 Uiso 1 1 calc R . . C224 C 1.3004(4) -0.2177(5) 0.6309(4) 0.045(2) Uani 1 1 d . . . C225 C 1.3569(4) -0.1967(5) 0.6312(4) 0.046(2) Uani 1 1 d . . . C226 C 1.3725(5) -0.1477(5) 0.5839(5) 0.060(3) Uani 1 1 d . . . H226 H 1.3453 -0.1261 0.5504 0.072 Uiso 1 1 calc R . . C227 C 1.4260(6) -0.1311(5) 0.5857(5) 0.068(3) Uani 1 1 d . . . H227 H 1.4375 -0.0989 0.5529 0.082 Uiso 1 1 calc R . . C228 C 1.4648(5) -0.1607(5) 0.6354(5) 0.060(3) Uani 1 1 d . . . H228 H 1.5028 -0.1495 0.6372 0.071 Uiso 1 1 calc R . . C229 C 1.4456(4) -0.2078(5) 0.6826(4) 0.048(2) Uani 1 1 d . . . C230 C 1.4853(4) -0.2508(5) 0.7362(4) 0.049(2) Uani 1 1 d . . . C231 C 1.5677(5) -0.2765(5) 0.8068(5) 0.059(3) Uani 1 1 d . . . H23A H 1.5565 -0.2662 0.8434 0.071 Uiso 1 1 calc R . . H23B H 1.5667 -0.3228 0.8138 0.071 Uiso 1 1 calc R . . C232 C 1.6336(6) -0.2732(7) 0.7888(6) 0.079(4) Uani 1 1 d . . . H23C H 1.6475 -0.2903 0.7562 0.119 Uiso 1 1 calc R . . H23D H 1.6641 -0.3009 0.8213 0.119 Uiso 1 1 calc R . . H23E H 1.6333 -0.2262 0.7770 0.119 Uiso 1 1 calc R . . C233 C 1.5067(5) -0.1548(6) 0.7508(6) 0.071(3) Uani 1 1 d . . . H23F H 1.4724 -0.1278 0.7208 0.085 Uiso 1 1 calc R . . H23G H 1.5470 -0.1434 0.7359 0.085 Uiso 1 1 calc R . . C234 C 1.4858(7) -0.1358(8) 0.8046(8) 0.099(5) Uani 1 1 d . . . H23H H 1.4472 -0.1492 0.8207 0.148 Uiso 1 1 calc R . . H23I H 1.4752 -0.0869 0.7950 0.148 Uiso 1 1 calc R . . H23J H 1.5212 -0.1592 0.8332 0.148 Uiso 1 1 calc R . . C301 C 1.2573(4) -0.1197(4) 0.7257(4) 0.042(2) Uani 1 1 d . A . C302 C 1.2141(5) -0.0877(5) 0.6789(4) 0.050(2) Uani 1 1 d . . . H302 H 1.1770 -0.1014 0.6797 0.060 Uiso 1 1 calc R . . C303 C 1.2243(5) -0.0361(5) 0.6309(5) 0.054(2) Uani 1 1 d . A . H303 H 1.1945 -0.0153 0.5993 0.065 Uiso 1 1 calc R . . C304 C 1.2779(5) -0.0149(5) 0.6291(4) 0.051(2) Uani 1 1 d . . . C305 C 1.3195(5) -0.0449(4) 0.6767(4) 0.047(2) Uani 1 1 d . A . H305 H 1.3553 -0.0295 0.6768 0.057 Uiso 1 1 calc R . . C306 C 1.3097(4) -0.0968(4) 0.7242(4) 0.047(2) Uani 1 1 d . . . H306 H 1.3391 -0.1169 0.7561 0.056 Uiso 1 1 calc R A . C307 C 1.2446(4) -0.1773(4) 0.7745(4) 0.0405(19) Uani 1 1 d . . . H30A H 1.2032 -0.1596 0.7933 0.049 Uiso 1 1 calc R A . H30B H 1.2390 -0.2102 0.7582 0.049 Uiso 1 1 calc R . . C308 C 1.3010(5) -0.1937(5) 0.8643(4) 0.051(2) Uani 1 1 d . . . H308 H 1.2727 -0.1554 0.8731 0.061 Uiso 1 1 calc R A . C309 C 1.3558(5) -0.2418(5) 0.8958(4) 0.050(2) Uani 1 1 d . A . H309 H 1.3724 -0.2430 0.9304 0.060 Uiso 1 1 calc R . . C310 C 1.3808(4) -0.2871(5) 0.8660(4) 0.0414(19) Uani 1 1 d . . . C311 C 1.4343(4) -0.3508(5) 0.8830(4) 0.0408(19) Uani 1 1 d . A . C312 C 1.4776(4) -0.3685(5) 0.9291(4) 0.048(2) Uani 1 1 d . . . H312 H 1.4733 -0.3380 0.9496 0.057 Uiso 1 1 calc R A . C313 C 1.5258(4) -0.4296(5) 0.9437(4) 0.048(2) Uani 1 1 d . A . H313 H 1.5553 -0.4422 0.9744 0.058 Uiso 1 1 calc R . . C314 C 1.5307(4) -0.4732(5) 0.9127(4) 0.048(2) Uani 1 1 d . . . H314 H 1.5635 -0.5162 0.9221 0.057 Uiso 1 1 calc R A . C315 C 1.4869(4) -0.4527(4) 0.8679(4) 0.0400(19) Uani 1 1 d . A . C316 C 1.4883(5) -0.4907(5) 0.8273(4) 0.051(2) Uani 1 1 d . . . C317 C 1.5185(7) -0.5878(7) 0.7942(5) 0.081(4) Uiso 1 1 d D . . H31A H 1.5540 -0.6316 0.8040 0.097 Uiso 1 1 calc R A . H31B H 1.5294 -0.5571 0.7574 0.097 Uiso 1 1 calc R . . C318 C 1.4545(11) -0.5984(12) 0.7877(10) 0.148(8) Uiso 1 1 d . A . H31C H 1.4421 -0.6256 0.8252 0.223 Uiso 1 1 calc R . . H31D H 1.4597 -0.6219 0.7595 0.223 Uiso 1 1 calc R . . H31E H 1.4204 -0.5544 0.7743 0.223 Uiso 1 1 calc R . . C319 C 1.5271(6) -0.6078(5) 0.9011(4) 0.066(3) Uani 1 1 d D . . H31Y H 1.5053 -0.6423 0.9073 0.080 Uiso 1 1 calc R A . H31Z H 1.5096 -0.5842 0.9297 0.080 Uiso 1 1 calc R . . C320 C 1.6002(7) -0.6428(7) 0.9111(6) 0.088(4) Uani 1 1 d . A . H32A H 1.6192 -0.6590 0.8788 0.132 Uiso 1 1 calc R . . H32B H 1.6078 -0.6812 0.9472 0.132 Uiso 1 1 calc R . . H32C H 1.6206 -0.6108 0.9138 0.132 Uiso 1 1 calc R . . C321 C 1.2938(6) 0.0371(5) 0.5766(4) 0.058(3) Uani 1 1 d . A . H32D H 1.3253 0.0543 0.5878 0.069 Uiso 1 1 calc R . . H32E H 1.3150 0.0152 0.5475 0.069 Uiso 1 1 calc R . . C322 C 1.1947(7) 0.0985(6) 0.5115(5) 0.076(4) Uani 1 1 d . A . H322 H 1.1999 0.0659 0.4931 0.091 Uiso 1 1 calc R . . C323 C 1.1442(6) 0.1568(5) 0.5032(5) 0.065(3) Uani 1 1 d . . . H323 H 1.1073 0.1729 0.4787 0.078 Uiso 1 1 calc R A . C324 C 1.1587(5) 0.1879(4) 0.5389(4) 0.044(2) Uani 1 1 d . A . C325 C 1.1218(4) 0.2524(4) 0.5460(4) 0.0410(19) Uani 1 1 d . . . C326 C 1.0632(5) 0.2931(5) 0.5152(5) 0.053(2) Uani 1 1 d . A . H326 H 1.0463 0.2784 0.4899 0.064 Uiso 1 1 calc R . . C327 C 1.0320(5) 0.3528(6) 0.5222(6) 0.068(3) Uani 1 1 d . . . H327 H 0.9920 0.3802 0.5024 0.082 Uiso 1 1 calc R A . C328 C 1.0571(5) 0.3750(5) 0.5580(5) 0.057(3) Uani 1 1 d . A . H328 H 1.0364 0.4186 0.5611 0.069 Uiso 1 1 calc R . . C329 C 1.1139(4) 0.3316(5) 0.5897(4) 0.046(2) Uani 1 1 d . . . C330 C 1.1485(5) 0.3452(5) 0.6300(5) 0.054(2) Uani 1 1 d . A . C331 C 1.0480(5) 0.4185(6) 0.6648(6) 0.077(4) Uani 1 1 d D . . H33A H 1.0240 0.3975 0.6488 0.092 Uiso 1 1 calc R . . H33B H 1.0356 0.4113 0.7059 0.092 Uiso 1 1 calc R . . C332 C 1.0282(9) 0.4925(7) 0.6326(8) 0.116(6) Uani 1 1 d . . . H33C H 1.0497 0.5140 0.6498 0.174 Uiso 1 1 calc R . . H33D H 0.9808 0.5121 0.6348 0.174 Uiso 1 1 calc R . . H33E H 1.0411 0.5000 0.5920 0.174 Uiso 1 1 calc R . . C333 C 1.1602(8) 0.3917(9) 0.7028(6) 0.100(5) Uiso 1 1 d D . . H33F H 1.1424 0.4370 0.7070 0.121 Uiso 1 1 calc R . . H33G H 1.2058 0.3847 0.6893 0.121 Uiso 1 1 calc R . . C334 C 1.1565(11) 0.3344(11) 0.7624(9) 0.136(7) Uiso 1 1 d . . . H33H H 1.1118 0.3448 0.7770 0.203 Uiso 1 1 calc R . . H33I H 1.1861 0.3325 0.7907 0.203 Uiso 1 1 calc R . . H33J H 1.1693 0.2906 0.7562 0.203 Uiso 1 1 calc R . . C401 C 1.0939(6) 0.1430(6) 0.6847(5) 0.065(3) Uani 1 1 d . . . C402 C 1.0585(7) 0.1324(7) 0.6467(5) 0.073(4) Uani 1 1 d . A . H402 H 1.0769 0.0937 0.6349 0.087 Uiso 1 1 calc R . . C403 C 0.9976(7) 0.1762(7) 0.6259(5) 0.072(3) Uani 1 1 d . . . H403 H 0.9750 0.1674 0.6000 0.087 Uiso 1 1 calc R A . C404 C 0.9690(7) 0.2338(7) 0.6426(5) 0.075(4) Uani 1 1 d . A . C405 C 1.0041(7) 0.2439(7) 0.6805(6) 0.077(4) Uani 1 1 d . . . H405 H 0.9859 0.2825 0.6924 0.093 Uiso 1 1 calc R A . C406 C 1.0639(7) 0.2001(7) 0.7011(6) 0.075(4) Uani 1 1 d . A . H406 H 1.0858 0.2088 0.7275 0.090 Uiso 1 1 calc R . . C407 C 1.1602(6) 0.0942(6) 0.7049(5) 0.065(3) Uani 1 1 d . A . H40A H 1.1558 0.0497 0.7286 0.078 Uiso 1 1 calc R . . H40B H 1.1870 0.0883 0.6708 0.078 Uiso 1 1 calc R . . C408 C 1.1896(10) 0.1031(10) 0.7971(6) 0.115(6) Uani 1 1 d . A . H408 H 1.1666 0.0756 0.8234 0.138 Uiso 1 1 calc R . . C409 C 1.2243(11) 0.1361(10) 0.8112(7) 0.120(7) Uani 1 1 d . . . H409 H 1.2303 0.1366 0.8486 0.144 Uiso 1 1 calc R A . C410 C 1.2494(7) 0.1694(7) 0.7586(5) 0.075(3) Uani 1 1 d D A . C421 C 0.9014(7) 0.2836(7) 0.6204(6) 0.077(3) Uani 1 1 d . . . H42A H 0.8857 0.3144 0.6435 0.093 Uiso 1 1 calc R A . H42B H 0.9047 0.3112 0.5796 0.093 Uiso 1 1 calc R . . C422 C 0.8427(7) 0.2267(8) 0.5852(5) 0.087(4) Uani 1 1 d . . . H422 H 0.8582 0.2368 0.5466 0.104 Uiso 1 1 calc R A . C423 C 0.8036(8) 0.1876(8) 0.6080(5) 0.086(4) Uani 1 1 d . A . H423 H 0.7864 0.1654 0.5896 0.103 Uiso 1 1 calc R . . C424 C 0.7947(6) 0.1878(5) 0.6645(4) 0.058(3) Uani 1 1 d . . . C425 C 0.7550(5) 0.1551(5) 0.7101(5) 0.054(2) Uani 1 1 d . A . C426 C 0.7209(5) 0.1177(5) 0.6995(5) 0.060(3) Uani 1 1 d . . . H426 H 0.7237 0.1106 0.6633 0.072 Uiso 1 1 calc R A . C427 C 0.6829(6) 0.0912(6) 0.7429(6) 0.071(3) Uani 1 1 d . A . H427 H 0.6580 0.0663 0.7366 0.085 Uiso 1 1 calc R . . C428 C 0.6807(5) 0.1004(5) 0.7947(5) 0.061(3) Uani 1 1 d . . . H428 H 0.6538 0.0828 0.8248 0.073 Uiso 1 1 calc R A . C429 C 0.7188(5) 0.1362(5) 0.8033(5) 0.053(2) Uani 1 1 d . A . C430 C 0.7196(5) 0.1556(6) 0.8561(4) 0.058(3) Uani 1 1 d . . . C431 C 0.7041(10) 0.1459(10) 0.9566(7) 0.119(6) Uiso 1 1 d D . . H43A H 0.7016 0.1940 0.9403 0.143 Uiso 1 1 calc R A . H43B H 0.6626 0.1434 0.9766 0.143 Uiso 1 1 calc R . . C432 C 0.7542(13) 0.1118(14) 0.9954(12) 0.171(10) Uiso 1 1 d . A . H43C H 0.7409 0.0793 1.0288 0.256 Uiso 1 1 calc R . . H43D H 0.7656 0.1439 1.0082 0.256 Uiso 1 1 calc R . . H43E H 0.7921 0.0877 0.9771 0.256 Uiso 1 1 calc R . . C433 C 0.7096(8) 0.0471(6) 0.9213(7) 0.098(4) Uiso 1 1 d D . . H43F H 0.7421 0.0154 0.9518 0.118 Uiso 1 1 calc R A . H43G H 0.7223 0.0341 0.8860 0.118 Uiso 1 1 calc R . . C434 C 0.6406(10) 0.0379(10) 0.9416(9) 0.124(6) Uiso 1 1 d . A . H43H H 0.6292 0.0462 0.9786 0.186 Uiso 1 1 calc R . . H43I H 0.6424 -0.0083 0.9463 0.186 Uiso 1 1 calc R . . H43J H 0.6075 0.0701 0.9124 0.186 Uiso 1 1 calc R . . O1A O 1.3640(7) 0.2595(7) 0.5839(6) 0.053(4) Uiso 0.517(8) 1 d PD A 1 N1 N 1.4660(15) 0.258(2) 0.6029(14) 0.181(16) Uiso 0.517(8) 1 d PD A 1 C11 C 1.2963(7) 0.2103(8) 0.7444(6) 0.085(3) Uiso 0.517(8) 1 d PGDU A 1 C12 C 1.3080(9) 0.2383(10) 0.7832(6) 0.087(3) Uiso 0.517(8) 1 d PGDU A 1 H12 H 1.2860 0.2326 0.8192 0.104 Uiso 0.517(8) 1 calc PR A 1 C13 C 1.3519(9) 0.2746(10) 0.7693(7) 0.088(3) Uiso 0.517(8) 1 d PGDU A 1 H13 H 1.3599 0.2937 0.7958 0.105 Uiso 0.517(8) 1 calc PR A 1 C14 C 1.3840(8) 0.2828(9) 0.7166(7) 0.088(3) Uiso 0.517(8) 1 d PGDU A 1 H14 H 1.4140 0.3076 0.7071 0.105 Uiso 0.517(8) 1 calc PR A 1 C15 C 1.3724(7) 0.2548(8) 0.6778(5) 0.064(3) Uiso 0.517(8) 1 d PGDU A 1 N2 N 1.3285(6) 0.2185(6) 0.6917(5) 0.040(3) Uiso 0.517(8) 1 d PGD A 1 C16 C 1.3963(10) 0.2627(11) 0.6203(8) 0.065(3) Uiso 0.517(8) 1 d PDU A 1 C17 C 1.4792(19) 0.2781(19) 0.5391(15) 0.145(8) Uiso 0.517(8) 1 d PDU A 1 H17A H 1.5029 0.3116 0.5264 0.173 Uiso 0.517(8) 1 calc PR A 1 H17B H 1.4388 0.2954 0.5159 0.173 Uiso 0.517(8) 1 calc PR A 1 C18 C 1.522(2) 0.208(2) 0.5373(19) 0.145(8) Uiso 0.517(8) 1 d PDU A 1 H18A H 1.5370 0.2113 0.4976 0.218 Uiso 0.517(8) 1 calc PR A 1 H18B H 1.4972 0.1763 0.5505 0.218 Uiso 0.517(8) 1 calc PR A 1 H18C H 1.5602 0.1915 0.5628 0.218 Uiso 0.517(8) 1 calc PR A 1 C19 C 1.525(2) 0.212(3) 0.639(2) 0.23(2) Uiso 0.517(8) 1 d PDU A 1 H19A H 1.5565 0.1849 0.6171 0.277 Uiso 0.517(8) 1 calc PR A 1 H19B H 1.5130 0.1810 0.6751 0.277 Uiso 0.517(8) 1 calc PR A 1 C20 C 1.551(3) 0.265(3) 0.650(3) 0.23(2) Uiso 0.517(8) 1 d PDU A 1 H20C H 1.5910 0.2418 0.6727 0.348 Uiso 0.517(8) 1 calc PR A 1 H20D H 1.5178 0.2910 0.6711 0.348 Uiso 0.517(8) 1 calc PR A 1 H20E H 1.5592 0.2965 0.6128 0.348 Uiso 0.517(8) 1 calc PR A 1 O1A' O 1.3473(8) 0.2750(8) 0.6007(6) 0.054(4) Uiso 0.483(8) 1 d PD A 2 N1' N 1.3698(19) 0.3680(16) 0.6094(13) 0.165(15) Uiso 0.483(8) 1 d PD A 2 C11' C 1.2904(8) 0.2014(8) 0.7624(6) 0.086(3) Uiso 0.483(8) 1 d PGDU A 2 C12' C 1.3141(9) 0.2106(10) 0.8082(5) 0.087(3) Uiso 0.483(8) 1 d PGDU A 2 H12' H 1.3032 0.1892 0.8469 0.104 Uiso 0.483(8) 1 calc PR A 2 C13' C 1.3538(9) 0.2511(11) 0.7975(7) 0.088(3) Uiso 0.483(8) 1 d PGDU A 2 H13' H 1.3700 0.2573 0.8288 0.106 Uiso 0.483(8) 1 calc PR A 2 C14' C 1.3698(9) 0.2824(9) 0.7410(8) 0.088(3) Uiso 0.483(8) 1 d PGDU A 2 H14' H 1.3969 0.3101 0.7336 0.106 Uiso 0.483(8) 1 calc PR A 2 C15' C 1.3461(8) 0.2733(8) 0.6952(6) 0.064(3) Uiso 0.483(8) 1 d PGDU A 2 N2' N 1.3064(7) 0.2328(7) 0.7059(5) 0.049(4) Uiso 0.483(8) 1 d PGD A 2 C16' C 1.3581(12) 0.2998(11) 0.6346(8) 0.064(3) Uiso 0.483(8) 1 d PDU A 2 C17' C 1.369(2) 0.4040(19) 0.5461(13) 0.141(8) Uiso 0.483(8) 1 d PDU A 2 H17C H 1.3704 0.4507 0.5370 0.169 Uiso 0.483(8) 1 calc PR A 2 H17D H 1.3321 0.4046 0.5261 0.169 Uiso 0.483(8) 1 calc PR A 2 C18' C 1.434(2) 0.357(2) 0.5328(19) 0.144(8) Uiso 0.483(8) 1 d PDU A 2 H18D H 1.4421 0.3713 0.4910 0.216 Uiso 0.483(8) 1 calc PR A 2 H18E H 1.4324 0.3104 0.5458 0.216 Uiso 0.483(8) 1 calc PR A 2 H18F H 1.4698 0.3582 0.5531 0.216 Uiso 0.483(8) 1 calc PR A 2 C19' C 1.357(2) 0.415(2) 0.643(2) 0.170(15) Uiso 0.483(8) 1 d PDU A 2 H19C H 1.3324 0.3997 0.6791 0.204 Uiso 0.483(8) 1 calc PR A 2 H19D H 1.3321 0.4613 0.6204 0.204 Uiso 0.483(8) 1 calc PR A 2 C20' C 1.428(2) 0.409(3) 0.658(2) 0.170(15) Uiso 0.483(8) 1 d PDU A 2 H20F H 1.4247 0.4397 0.6800 0.255 Uiso 0.483(8) 1 calc PR A 2 H20G H 1.4514 0.4225 0.6222 0.255 Uiso 0.483(8) 1 calc PR A 2 H20H H 1.4508 0.3628 0.6814 0.255 Uiso 0.483(8) 1 calc PR A 2 Cl1 Cl 0.87655(12) 0.06126(13) 0.12388(13) 0.0607(6) Uani 1 1 d D . . O1 O 0.9150(5) 0.0613(4) 0.0722(4) 0.079(2) Uani 1 1 d . B . O2 O 0.9059(9) 0.0011(7) 0.1697(7) 0.095(5) Uiso 0.50 1 d PDU B 1 O3 O 0.8139(7) 0.0590(8) 0.1097(8) 0.080(4) Uiso 0.50 1 d PDU B 1 O4 O 0.8663(7) 0.1204(6) 0.1381(7) 0.065(4) Uiso 0.50 1 d PDU B 1 O2' O 0.9215(9) 0.0310(9) 0.1717(7) 0.097(5) Uiso 0.50 1 d PDU B 2 O3' O 0.8218(7) 0.0386(9) 0.1391(9) 0.093(5) Uiso 0.50 1 d PDU B 2 O4' O 0.8536(7) 0.1335(6) 0.1131(7) 0.061(3) Uiso 0.50 1 d PDU B 2 Cl2 Cl 0.36830(15) 0.08186(16) 0.16769(15) 0.0767(8) Uani 1 1 d D . . O7 O 0.3160(5) 0.0625(6) 0.1572(5) 0.097(3) Uani 1 1 d . C . O5 O 0.4155(13) 0.0694(14) 0.1231(11) 0.122(6) Uiso 0.46(2) 1 d PDU C 1 O6 O 0.4016(16) 0.0411(13) 0.2209(9) 0.139(8) Uiso 0.46(2) 1 d PDU C 1 O8 O 0.3565(12) 0.1504(8) 0.1629(11) 0.090(5) Uiso 0.46(2) 1 d PDU C 1 O5' O 0.4296(9) 0.0477(11) 0.1494(11) 0.119(6) Uiso 0.54(2) 1 d PDU C 2 O6' O 0.3641(14) 0.0673(13) 0.2291(6) 0.136(7) Uiso 0.54(2) 1 d PDU C 2 O8' O 0.3441(9) 0.1513(7) 0.1361(9) 0.093(5) Uiso 0.54(2) 1 d PDU C 2 Cl3 Cl 0.7479(3) 0.0413(2) 0.5641(2) 0.0493(11) Uiso 0.50 1 d PDU D 1 O9 O 0.7136(11) 0.0287(10) 0.5277(8) 0.095(5) Uiso 0.50 1 d PDU D 1 O10 O 0.7400(13) 0.0118(11) 0.6227(8) 0.109(5) Uiso 0.50 1 d PDU D 1 O11 O 0.8149(12) 0.0058(13) 0.5564(12) 0.135(6) Uiso 0.50 1 d PDU D 1 O12 O 0.7320(10) 0.1112(7) 0.5512(7) 0.076(4) Uiso 0.50 1 d PDU D 1 Cl3' Cl 0.7180(3) 0.0453(3) 0.5738(2) 0.0590(12) Uiso 0.50 1 d PDU E 2 O9' O 0.6867(10) 0.0244(10) 0.5408(8) 0.089(5) Uiso 0.50 1 d PDU E 2 O10' O 0.6991(12) 0.0227(11) 0.6309(8) 0.106(5) Uiso 0.50 1 d PDU E 2 O11' O 0.7876(13) 0.0217(14) 0.5764(12) 0.132(5) Uiso 0.50 1 d PDU E 2 O12' O 0.6967(9) 0.1161(7) 0.5566(7) 0.071(4) Uiso 0.50 1 d PDU E 2 Cl11 Cl 0.68835(11) 0.43267(11) 0.03473(9) 0.0445(5) Uani 1 1 d D . . O13 O 0.7215(4) 0.3752(4) 0.0812(3) 0.0630(19) Uani 1 1 d D . . O14 O 0.6499(4) 0.4127(4) 0.0043(3) 0.071(2) Uani 1 1 d D . . O15 O 0.7340(3) 0.4584(4) -0.0050(3) 0.0595(18) Uani 1 1 d D . . O16 O 0.6469(4) 0.4839(4) 0.0581(3) 0.071(2) Uani 1 1 d D . . Cl5 Cl 0.9280(3) 0.3038(5) 0.4264(3) 0.0662(16) Uiso 0.498(10) 1 d PDU F 1 O17 O 0.8850(9) 0.3473(12) 0.3802(7) 0.090(5) Uiso 0.498(10) 1 d PDU F 1 O18 O 0.9950(8) 0.2908(11) 0.4089(8) 0.085(4) Uiso 0.498(10) 1 d PDU F 1 O19 O 0.9189(8) 0.3276(9) 0.4719(6) 0.062(4) Uiso 0.498(10) 1 d PDU F 1 O20 O 0.9356(11) 0.2316(12) 0.4497(10) 0.095(4) Uiso 0.498(10) 1 d PDU F 1 Cl5' Cl 0.9366(3) 0.2696(5) 0.4366(3) 0.0602(15) Uiso 0.502(10) 1 d PDU F 2 O17' O 0.8980(9) 0.3082(11) 0.3857(7) 0.086(5) Uiso 0.502(10) 1 d PDU F 2 O18' O 1.0029(7) 0.2479(11) 0.4251(9) 0.088(4) Uiso 0.502(10) 1 d PDU F 2 O19' O 0.9274(8) 0.2928(10) 0.4822(6) 0.067(4) Uiso 0.502(10) 1 d PDU F 2 O20' O 0.9173(12) 0.2090(11) 0.4623(10) 0.113(6) Uiso 0.502(10) 1 d PDU F 2 Cl6 Cl 1.03457(13) -0.48551(14) 0.20772(12) 0.0609(6) Uani 1 1 d . . . O21 O 1.0746(5) -0.5254(6) 0.2566(4) 0.114(4) Uani 1 1 d . . . O22 O 1.0449(6) -0.4200(5) 0.1842(4) 0.096(3) Uani 1 1 d . . . O23 O 1.0511(4) -0.5184(4) 0.1646(4) 0.081(2) Uani 1 1 d . . . O24 O 0.9675(4) -0.4744(5) 0.2219(4) 0.078(2) Uani 1 1 d . . . Cl7 Cl 0.1408(2) 0.48974(18) 0.46075(19) 0.1024(12) Uani 1 1 d D . . O25 O 0.1502(8) 0.4672(8) 0.4131(6) 0.174(6) Uiso 1 1 d D . . O26 O 0.0748(6) 0.5053(8) 0.4761(7) 0.190(7) Uiso 1 1 d D . . O27 O 0.1558(8) 0.5505(7) 0.4426(7) 0.203(8) Uiso 1 1 d D . . O28 O 0.1799(6) 0.4424(6) 0.5064(5) 0.125(4) Uiso 1 1 d D . . Cl12 Cl 0.2394(2) 0.13833(17) 0.97190(14) 0.0892(11) Uani 1 1 d . . . O29 O 0.2150(6) 0.1961(5) 0.9233(4) 0.104(4) Uani 1 1 d . . . O30 O 0.1852(6) 0.1318(6) 1.0141(5) 0.108(4) Uani 1 1 d . . . O31 O 0.2891(6) 0.1452(8) 1.0000(5) 0.130(4) Uani 1 1 d . . . O32 O 0.2625(7) 0.0803(4) 0.9538(4) 0.116(4) Uani 1 1 d . . . Cl9 Cl 0.24259(19) 0.48355(19) 0.7728(2) 0.0526(9) Uiso 0.756(9) 1 d PDU G 1 O33 O 0.1989(7) 0.4507(7) 0.8036(6) 0.103(4) Uiso 0.756(9) 1 d PDU G 1 O34 O 0.2100(6) 0.5259(6) 0.7191(6) 0.082(3) Uiso 0.756(9) 1 d PDU G 1 O35 O 0.2386(8) 0.5254(8) 0.8096(7) 0.111(4) Uiso 0.756(9) 1 d PDU G 1 O36 O 0.3071(9) 0.4609(11) 0.7587(9) 0.149(7) Uiso 0.756(9) 1 d PDU G 1 Cl9' Cl 0.2531(6) 0.4739(6) 0.7942(7) 0.055(2) Uiso 0.244(9) 1 d PDU G 2 O33' O 0.1977(15) 0.493(2) 0.8259(16) 0.110(5) Uiso 0.244(9) 1 d PDU G 2 O34' O 0.234(2) 0.5288(15) 0.7378(12) 0.092(6) Uiso 0.244(9) 1 d PDU G 2 O35' O 0.2973(19) 0.491(2) 0.8214(18) 0.120(7) Uiso 0.244(9) 1 d PDU G 2 O36' O 0.286(2) 0.4208(19) 0.774(2) 0.138(9) Uiso 0.244(9) 1 d PDU G 2 Cl10 Cl 0.62096(19) 0.6920(2) 0.61062(16) 0.1070(14) Uani 1 1 d D . . O37 O 0.5849(9) 0.6444(9) 0.6214(8) 0.131(6) Uiso 0.628(11) 1 d PDU H 1 O38 O 0.5871(9) 0.7522(8) 0.5626(8) 0.154(6) Uiso 0.628(11) 1 d PDU H 1 O39 O 0.6135(10) 0.7139(10) 0.6599(7) 0.150(7) Uiso 0.628(11) 1 d PDU H 1 O40 O 0.6844(7) 0.6652(9) 0.5956(9) 0.140(6) Uiso 0.628(11) 1 d PDU H 1 O37' O 0.5613(10) 0.6845(16) 0.6304(12) 0.138(8) Uiso 0.372(11) 1 d PDU H 2 O38' O 0.6367(14) 0.6862(15) 0.5546(8) 0.139(6) Uiso 0.372(11) 1 d PDU H 2 O39' O 0.6227(15) 0.7574(11) 0.6090(14) 0.161(6) Uiso 0.372(11) 1 d PDU H 2 O40' O 0.6740(11) 0.6422(12) 0.6497(11) 0.137(7) Uiso 0.372(11) 1 d PDU H 2 Cl4 Cl 0.4711(3) 0.7788(3) 0.1587(4) 0.176(3) Uani 1 1 d D . . O41 O 0.5322(12) 0.7543(19) 0.1245(15) 0.261(15) Uiso 0.50 1 d PDU I 1 O42 O 0.4612(16) 0.8513(11) 0.1530(18) 0.241(11) Uiso 0.50 1 d PDU I 1 O43 O 0.4138(10) 0.7696(13) 0.1376(12) 0.128(6) Uiso 0.50 1 d PDU I 1 O44 O 0.4831(17) 0.7351(18) 0.2231(9) 0.246(12) Uiso 0.50 1 d PDU I 1 O41' O 0.5277(13) 0.7270(15) 0.1424(17) 0.262(15) Uiso 0.50 1 d PDU I 2 O42' O 0.4924(17) 0.802(2) 0.2032(14) 0.245(11) Uiso 0.50 1 d PDU I 2 O43' O 0.4143(10) 0.7531(12) 0.1811(11) 0.125(6) Uiso 0.50 1 d PDU I 2 O44' O 0.4485(16) 0.8430(14) 0.1045(13) 0.241(12) Uiso 0.50 1 d PDU I 2 Cl8 Cl 0.4749(8) 0.7815(9) 0.0013(7) 0.168(4) Uiso 0.50 1 d PDU J 1 O45 O 0.5100(15) 0.7233(13) -0.0080(15) 0.165(9) Uiso 0.50 1 d PDU J 1 O46 O 0.448(2) 0.767(2) 0.0609(13) 0.262(14) Uiso 0.50 1 d PDU J 1 O47 O 0.506(2) 0.834(2) -0.002(2) 0.264(13) Uiso 0.50 1 d PDU J 1 O48 O 0.4212(19) 0.817(2) -0.0411(19) 0.32(2) Uiso 0.50 1 d PDU J 1 Cl8' Cl 0.4868(9) 0.8053(9) -0.0241(8) 0.178(4) Uiso 0.50 1 d PDU K 2 O45' O 0.4939(16) 0.7605(16) -0.0505(14) 0.167(9) Uiso 0.50 1 d PDU K 2 O46' O 0.494(3) 0.771(2) 0.0402(11) 0.265(13) Uiso 0.50 1 d PDU K 2 O47' O 0.529(2) 0.849(2) -0.031(2) 0.262(14) Uiso 0.50 1 d PDU K 2 O48' O 0.4226(17) 0.858(2) -0.038(2) 0.32(2) Uiso 0.50 1 d PDU K 2 N1S N 0.2051(10) 0.3363(10) 0.2660(8) 0.149(6) Uiso 1 1 d D . . C1S C 0.1877(10) 0.3329(11) 0.3131(8) 0.123(6) Uiso 1 1 d D . . C2S C 0.1649(12) 0.3323(12) 0.3716(9) 0.149(8) Uiso 1 1 d D . . H2S1 H 0.1408 0.3785 0.3708 0.224 Uiso 1 1 calc R . . H2S2 H 0.2025 0.3137 0.3978 0.224 Uiso 1 1 calc R . . H2S3 H 0.1363 0.3041 0.3852 0.224 Uiso 1 1 calc R . . N2S N 0.6458(9) -0.0222(9) 0.2299(8) 0.135(6) Uiso 1 1 d D . . C3S C 0.6557(11) 0.0019(11) 0.1806(9) 0.132(7) Uiso 1 1 d D . . C4S C 0.6675(13) 0.0383(13) 0.1189(9) 0.161(9) Uiso 1 1 d D . . H4S1 H 0.6896 0.0053 0.0993 0.242 Uiso 1 1 calc R . . H4S2 H 0.6948 0.0660 0.1174 0.242 Uiso 1 1 calc R . . H4S3 H 0.6257 0.0673 0.0996 0.242 Uiso 1 1 calc R . . N3S N 1.2689(8) 0.1699(9) 0.3070(8) 0.129(5) Uiso 1 1 d D . . C5S C 1.2944(12) 0.1538(12) 0.3520(9) 0.145(8) Uiso 1 1 d D . . C6S C 1.3098(13) 0.1495(14) 0.4111(10) 0.173(10) Uiso 1 1 d D . . H6S1 H 1.3248 0.1874 0.4083 0.259 Uiso 1 1 calc R . . H6S2 H 1.3441 0.1068 0.4288 0.259 Uiso 1 1 calc R . . H6S3 H 1.2706 0.1515 0.4350 0.259 Uiso 1 1 calc R . . O1W O 1.1388(6) -0.4494(6) 0.2991(5) 0.114(4) Uiso 1 1 d . . . O2W O 0.5149(6) -0.0172(6) 0.4629(5) 0.047(3) Uiso 0.50 1 d P . . N4S N 0.9489(8) -0.1826(9) 1.1225(7) 0.130(5) Uiso 1 1 d D . . C7S C 0.9228(9) -0.1334(9) 1.0843(8) 0.114(5) Uiso 1 1 d D . . C8S C 0.9043(14) -0.0722(12) 1.0317(10) 0.179(10) Uiso 1 1 d D . . H8S1 H 0.8868 -0.0317 1.0433 0.269 Uiso 1 1 calc R . . H8S2 H 0.8711 -0.0751 1.0096 0.269 Uiso 1 1 calc R . . H8S3 H 0.9428 -0.0696 1.0075 0.269 Uiso 1 1 calc R . . O3W O 1.5521(12) 0.4692(13) 0.6231(11) 0.118(7) Uiso 0.50 1 d P L 1 O3W' O 1.5794(13) 0.4297(13) 0.5820(12) 0.125(8) Uiso 0.50 1 d P M 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0519(3) 0.0448(3) 0.0501(3) -0.0201(2) 0.0022(2) -0.0117(2) Nd2 0.0346(2) 0.0304(2) 0.0292(2) -0.01057(17) 0.00057(17) -0.00981(17) Nd3 0.0353(2) 0.0413(3) 0.0306(2) -0.00921(19) -0.00170(17) -0.01020(19) Nd4 0.0365(3) 0.0353(2) 0.0488(3) -0.0080(2) -0.0094(2) -0.01221(19) O101 0.063(4) 0.046(4) 0.073(5) -0.023(4) -0.013(4) -0.002(3) O102 0.041(3) 0.037(3) 0.036(3) -0.007(2) -0.001(2) -0.007(3) O201 0.048(4) 0.056(4) 0.042(3) -0.016(3) 0.005(3) -0.029(3) O202 0.033(3) 0.050(4) 0.047(4) -0.006(3) 0.000(3) -0.015(3) O301 0.065(4) 0.048(4) 0.047(4) -0.016(3) -0.016(3) -0.006(3) O302 0.054(4) 0.065(4) 0.071(5) -0.043(4) -0.008(3) -0.012(3) O402 0.065(5) 0.078(5) 0.051(4) -0.031(4) 0.015(3) -0.031(4) O501 0.104(7) 0.092(6) 0.086(6) -0.042(5) 0.023(5) -0.061(6) O503 0.068(5) 0.073(5) 0.111(7) -0.040(5) -0.029(5) 0.000(4) O504 0.050(3) 0.035(3) 0.036(3) -0.013(2) -0.001(3) -0.006(3) O505 0.044(3) 0.050(4) 0.046(4) -0.013(3) -0.011(3) -0.013(3) O506 0.054(4) 0.048(4) 0.058(4) -0.026(3) -0.007(3) -0.018(3) O507 0.059(4) 0.081(5) 0.040(3) -0.012(3) -0.002(3) -0.045(4) O508 0.061(4) 0.066(5) 0.063(4) -0.029(4) -0.007(3) -0.018(4) O509 0.060(4) 0.067(5) 0.045(4) -0.018(3) 0.010(3) -0.017(4) O510 0.067(5) 0.044(4) 0.108(7) 0.001(4) -0.034(5) -0.010(4) O511 0.080(6) 0.061(5) 0.110(7) -0.023(5) 0.048(5) -0.014(4) O512 0.051(4) 0.058(4) 0.045(4) -0.012(3) 0.006(3) -0.022(3) N101 0.064(6) 0.050(5) 0.072(6) -0.025(4) -0.007(5) -0.005(4) N102 0.046(4) 0.049(5) 0.069(5) -0.035(4) 0.002(4) -0.008(4) N103 0.044(4) 0.046(4) 0.057(5) -0.029(4) 0.003(3) -0.010(3) N104 0.050(4) 0.036(4) 0.062(5) -0.024(4) 0.005(4) -0.003(3) N105 0.053(4) 0.033(4) 0.034(4) -0.010(3) -0.004(3) -0.008(3) N106 0.038(4) 0.034(3) 0.028(3) -0.009(3) 0.000(3) -0.010(3) N107 0.037(4) 0.031(3) 0.037(4) -0.014(3) -0.001(3) -0.011(3) N108 0.045(4) 0.037(4) 0.043(4) -0.009(3) -0.007(3) -0.008(3) N201 0.039(4) 0.049(4) 0.061(5) -0.018(4) 0.003(4) -0.014(3) N202 0.039(4) 0.034(3) 0.032(3) -0.009(3) 0.000(3) -0.014(3) N203 0.034(3) 0.040(4) 0.036(4) -0.013(3) 0.000(3) -0.014(3) N204 0.039(4) 0.045(4) 0.039(4) -0.012(3) 0.002(3) -0.019(3) N205 0.032(4) 0.071(5) 0.040(4) -0.025(4) -0.002(3) -0.015(3) N206 0.035(4) 0.051(4) 0.036(4) -0.015(3) -0.003(3) -0.008(3) N207 0.033(4) 0.044(4) 0.036(4) -0.008(3) 0.002(3) -0.008(3) N208 0.037(4) 0.057(5) 0.070(6) -0.022(4) -0.004(4) -0.015(4) N301 0.078(6) 0.042(5) 0.064(6) -0.017(4) -0.017(5) -0.015(4) N302 0.037(4) 0.041(4) 0.035(4) -0.009(3) 0.003(3) -0.016(3) N303 0.031(3) 0.041(4) 0.039(4) -0.015(3) -0.001(3) -0.010(3) N304 0.038(4) 0.043(4) 0.039(4) -0.013(3) -0.001(3) -0.008(3) N305 0.084(6) 0.032(4) 0.042(4) -0.011(3) -0.015(4) -0.004(4) N306 0.054(4) 0.032(4) 0.036(4) -0.010(3) -0.002(3) -0.016(3) N307 0.035(4) 0.038(4) 0.038(4) -0.013(3) 0.000(3) -0.011(3) N308 0.085(7) 0.072(6) 0.068(6) -0.044(5) 0.000(5) -0.014(5) N403 0.088(7) 0.056(5) 0.043(5) -0.017(4) -0.004(4) -0.029(5) N404 0.109(8) 0.076(6) 0.048(5) -0.018(5) 0.015(5) -0.052(6) N405 0.092(7) 0.088(7) 0.038(5) -0.015(5) 0.017(5) -0.039(6) N406 0.068(5) 0.054(5) 0.047(5) -0.014(4) 0.007(4) -0.022(4) N407 0.052(4) 0.045(4) 0.036(4) -0.014(3) 0.004(3) -0.010(3) N408 0.116(9) 0.071(7) 0.051(6) -0.021(5) 0.032(6) -0.020(6) C101 0.048(5) 0.029(4) 0.052(5) -0.016(4) 0.008(4) -0.005(4) C102 0.071(7) 0.047(5) 0.048(5) -0.018(4) 0.019(5) -0.024(5) C103 0.064(6) 0.046(5) 0.043(5) -0.017(4) 0.012(4) -0.018(5) C104 0.043(5) 0.034(4) 0.044(5) -0.008(4) 0.000(4) 0.000(4) C105 0.056(5) 0.036(5) 0.042(5) -0.013(4) 0.008(4) -0.012(4) C106 0.063(6) 0.036(5) 0.046(5) -0.020(4) 0.010(4) -0.013(4) C107 0.049(5) 0.049(5) 0.064(6) -0.030(5) 0.023(5) -0.014(4) C108 0.053(6) 0.052(6) 0.075(8) -0.027(6) 0.010(5) -0.006(5) C109 0.061(6) 0.050(6) 0.059(6) -0.021(5) -0.001(5) -0.002(5) C110 0.042(5) 0.049(5) 0.063(6) -0.028(5) -0.002(4) -0.007(4) C111 0.040(5) 0.054(6) 0.070(7) -0.037(5) -0.009(5) -0.002(4) C112 0.055(6) 0.069(7) 0.071(7) -0.037(6) -0.013(5) -0.008(5) C113 0.059(6) 0.075(8) 0.075(8) -0.048(7) -0.002(6) -0.008(6) C114 0.071(7) 0.061(7) 0.079(8) -0.048(6) 0.000(6) -0.007(6) C115 0.044(5) 0.048(5) 0.073(7) -0.033(5) 0.000(5) -0.005(4) C116 0.050(6) 0.057(7) 0.096(9) -0.046(6) 0.006(6) -0.003(5) C117 0.099(10) 0.070(8) 0.085(9) -0.029(7) -0.005(7) -0.030(7) C118 0.179(18) 0.062(8) 0.089(11) -0.031(8) -0.007(11) -0.034(10) C121 0.052(5) 0.031(4) 0.040(5) -0.009(4) 0.001(4) -0.009(4) C122 0.076(7) 0.043(5) 0.033(5) -0.010(4) -0.007(4) -0.017(5) C123 0.066(6) 0.047(5) 0.031(4) -0.016(4) 0.000(4) -0.017(4) C124 0.044(5) 0.041(5) 0.031(4) -0.011(4) -0.001(3) -0.010(4) C125 0.036(4) 0.041(4) 0.035(4) -0.016(4) 0.003(3) -0.014(4) C126 0.051(5) 0.054(6) 0.041(5) -0.028(4) 0.007(4) -0.015(4) C127 0.044(5) 0.058(6) 0.056(6) -0.039(5) 0.009(4) -0.013(4) C128 0.035(4) 0.043(5) 0.057(6) -0.022(4) -0.003(4) -0.009(4) C129 0.036(4) 0.031(4) 0.044(5) -0.018(4) -0.003(3) -0.009(3) C130 0.037(4) 0.027(4) 0.047(5) -0.013(4) -0.001(4) -0.008(3) C131 0.053(6) 0.061(6) 0.041(5) -0.001(5) -0.009(4) -0.005(5) C132 0.069(7) 0.098(9) 0.055(7) -0.032(7) -0.013(6) -0.007(7) C133 0.042(5) 0.041(5) 0.054(6) -0.013(4) -0.006(4) -0.007(4) C134 0.055(6) 0.052(6) 0.093(9) -0.028(6) -0.012(6) 0.003(5) C201 0.033(4) 0.043(5) 0.042(5) -0.014(4) 0.001(3) -0.020(4) C202 0.042(5) 0.049(5) 0.044(5) -0.006(4) -0.009(4) -0.011(4) C203 0.047(5) 0.065(6) 0.033(5) -0.016(4) 0.000(4) -0.020(5) C204 0.031(4) 0.048(5) 0.052(5) -0.019(4) -0.003(4) -0.016(4) C205 0.033(4) 0.045(5) 0.046(5) -0.009(4) -0.005(4) -0.015(4) C206 0.047(5) 0.043(5) 0.036(4) -0.005(4) -0.005(4) -0.019(4) C207 0.038(4) 0.044(5) 0.041(5) -0.009(4) 0.003(4) -0.017(4) C208 0.048(5) 0.059(6) 0.056(6) -0.024(5) 0.002(4) -0.030(5) C209 0.060(6) 0.064(6) 0.040(5) -0.018(5) 0.002(4) -0.032(5) C210 0.041(5) 0.042(5) 0.040(5) -0.018(4) 0.002(4) -0.016(4) C211 0.049(5) 0.042(5) 0.028(4) -0.012(4) -0.001(4) -0.014(4) C212 0.066(6) 0.066(6) 0.041(5) -0.016(5) -0.006(5) -0.031(5) C213 0.064(6) 0.065(6) 0.031(5) -0.008(4) 0.002(4) -0.030(5) C214 0.056(6) 0.054(6) 0.041(5) -0.013(4) 0.007(4) -0.026(5) C215 0.039(4) 0.035(4) 0.040(5) -0.012(4) 0.007(4) -0.014(4) C216 0.046(5) 0.034(4) 0.043(5) -0.012(4) 0.004(4) -0.016(4) C217 0.060(7) 0.116(11) 0.085(9) -0.061(9) 0.027(6) -0.024(7) C218 0.094(11) 0.173(17) 0.077(9) -0.050(11) 0.043(8) -0.074(11) C219 0.042(5) 0.065(7) 0.066(7) -0.017(5) 0.005(5) -0.020(5) C220 0.069(8) 0.065(7) 0.100(10) -0.011(7) -0.023(7) -0.033(6) C221 0.040(5) 0.057(6) 0.052(5) -0.025(5) -0.002(4) -0.016(4) C222 0.053(6) 0.104(9) 0.038(5) -0.028(6) -0.011(5) -0.012(6) C223 0.055(6) 0.084(8) 0.029(5) -0.013(5) -0.007(4) -0.014(5) C224 0.043(5) 0.047(5) 0.034(4) -0.009(4) -0.001(4) -0.006(4) C225 0.044(5) 0.042(5) 0.040(5) -0.009(4) 0.002(4) -0.004(4) C226 0.060(6) 0.051(6) 0.050(6) -0.002(5) -0.006(5) -0.008(5) C227 0.077(8) 0.046(6) 0.060(7) 0.005(5) 0.004(6) -0.017(5) C228 0.053(6) 0.053(6) 0.065(7) -0.005(5) 0.002(5) -0.022(5) C229 0.041(5) 0.043(5) 0.051(5) -0.013(4) 0.003(4) -0.008(4) C230 0.032(4) 0.053(6) 0.054(6) -0.010(5) 0.000(4) -0.011(4) C231 0.046(6) 0.056(6) 0.069(7) -0.015(5) -0.014(5) -0.011(5) C232 0.051(6) 0.070(8) 0.092(9) 0.002(7) -0.012(6) -0.013(6) C233 0.047(6) 0.053(6) 0.110(10) -0.021(6) -0.013(6) -0.015(5) C234 0.078(9) 0.090(10) 0.148(15) -0.062(10) -0.013(9) -0.024(8) C301 0.041(5) 0.036(4) 0.052(5) -0.022(4) -0.005(4) -0.006(4) C302 0.047(5) 0.041(5) 0.061(6) -0.015(4) -0.014(4) -0.010(4) C303 0.056(6) 0.047(5) 0.055(6) -0.012(5) -0.015(5) -0.012(5) C304 0.060(6) 0.037(5) 0.050(5) -0.018(4) 0.000(5) -0.004(4) C305 0.044(5) 0.036(5) 0.057(6) -0.013(4) -0.002(4) -0.009(4) C306 0.038(5) 0.039(5) 0.058(6) -0.014(4) -0.004(4) -0.005(4) C307 0.032(4) 0.041(5) 0.045(5) -0.013(4) -0.004(4) -0.007(4) C308 0.051(5) 0.055(6) 0.050(5) -0.026(5) 0.000(4) -0.012(4) C309 0.046(5) 0.062(6) 0.043(5) -0.022(5) -0.004(4) -0.011(4) C310 0.042(5) 0.049(5) 0.033(4) -0.013(4) -0.002(4) -0.013(4) C311 0.038(4) 0.051(5) 0.032(4) -0.008(4) 0.001(3) -0.018(4) C312 0.042(5) 0.063(6) 0.040(5) -0.018(4) -0.003(4) -0.017(4) C313 0.040(5) 0.061(6) 0.041(5) -0.012(4) -0.007(4) -0.015(4) C314 0.039(5) 0.050(5) 0.042(5) -0.005(4) -0.007(4) -0.006(4) C315 0.035(4) 0.037(4) 0.044(5) -0.008(4) -0.003(4) -0.011(4) C316 0.054(6) 0.046(5) 0.046(5) -0.005(4) -0.014(4) -0.013(4) C319 0.089(8) 0.040(5) 0.058(7) -0.002(5) -0.015(6) -0.016(5) C320 0.102(10) 0.062(7) 0.077(9) -0.024(7) -0.027(7) 0.013(7) C321 0.081(7) 0.032(5) 0.048(6) -0.010(4) -0.003(5) -0.005(5) C322 0.137(12) 0.046(6) 0.049(6) -0.017(5) -0.024(7) -0.025(7) C323 0.095(9) 0.046(6) 0.056(6) -0.016(5) -0.028(6) -0.016(6) C324 0.058(6) 0.038(5) 0.040(5) -0.008(4) -0.006(4) -0.024(4) C325 0.037(4) 0.040(5) 0.041(5) -0.007(4) -0.002(4) -0.012(4) C326 0.042(5) 0.057(6) 0.058(6) -0.012(5) -0.018(4) -0.014(4) C327 0.043(6) 0.061(7) 0.086(8) -0.020(6) -0.012(5) 0.001(5) C328 0.045(5) 0.052(6) 0.066(7) -0.021(5) -0.005(5) -0.001(4) C329 0.041(5) 0.042(5) 0.047(5) -0.017(4) -0.001(4) -0.003(4) C330 0.058(6) 0.048(5) 0.059(6) -0.026(5) 0.005(5) -0.014(5) C331 0.069(7) 0.074(8) 0.084(9) -0.046(7) 0.016(6) -0.002(6) C332 0.132(14) 0.069(9) 0.122(14) -0.046(9) 0.016(11) 0.010(9) C401 0.094(9) 0.072(7) 0.052(6) -0.025(5) 0.036(6) -0.061(7) C402 0.102(10) 0.074(8) 0.068(7) -0.042(6) 0.035(7) -0.051(8) C403 0.099(10) 0.081(8) 0.052(6) -0.027(6) 0.024(6) -0.048(8) C404 0.109(10) 0.083(8) 0.056(7) -0.033(6) 0.044(7) -0.065(8) C405 0.101(10) 0.077(8) 0.074(8) -0.043(7) 0.042(8) -0.048(8) C406 0.091(9) 0.089(9) 0.074(8) -0.049(7) 0.035(7) -0.054(8) C407 0.089(8) 0.062(7) 0.062(7) -0.026(5) 0.023(6) -0.048(6) C408 0.172(18) 0.132(14) 0.041(7) -0.013(8) 0.030(9) -0.071(13) C409 0.19(2) 0.147(16) 0.058(9) -0.041(10) 0.002(10) -0.083(15) C410 0.096(9) 0.085(8) 0.050(6) -0.026(6) -0.021(6) -0.025(7) C421 0.090(9) 0.072(8) 0.065(8) -0.010(6) 0.016(7) -0.038(7) C422 0.104(10) 0.119(12) 0.045(7) -0.036(7) 0.022(7) -0.044(9) C423 0.122(12) 0.097(10) 0.053(7) -0.031(7) 0.003(7) -0.048(9) C424 0.074(7) 0.053(6) 0.047(6) -0.018(5) 0.013(5) -0.021(5) C425 0.056(6) 0.042(5) 0.059(6) -0.021(5) -0.003(5) -0.005(4) C426 0.068(7) 0.047(6) 0.067(7) -0.025(5) -0.001(5) -0.015(5) C427 0.077(8) 0.047(6) 0.091(9) -0.034(6) -0.006(7) -0.010(6) C428 0.052(6) 0.045(5) 0.077(8) -0.015(5) 0.014(5) -0.015(5) C429 0.049(5) 0.041(5) 0.060(6) -0.015(4) 0.006(5) -0.006(4) C430 0.060(6) 0.060(6) 0.045(6) -0.020(5) 0.014(5) -0.011(5) Cl1 0.0522(14) 0.0510(14) 0.0792(18) -0.0266(13) 0.0062(12) -0.0132(11) O1 0.094(6) 0.070(5) 0.070(5) -0.029(4) 0.012(5) -0.019(5) Cl2 0.0607(17) 0.0638(17) 0.092(2) -0.0196(16) -0.0142(15) -0.0045(13) O7 0.079(6) 0.113(8) 0.105(8) -0.035(6) 0.008(5) -0.041(6) Cl11 0.0457(11) 0.0527(12) 0.0364(11) -0.0126(9) -0.0013(9) -0.0187(10) O13 0.079(5) 0.052(4) 0.049(4) -0.002(3) -0.010(4) -0.021(4) O14 0.065(5) 0.096(6) 0.067(5) -0.031(4) -0.005(4) -0.039(4) O15 0.061(4) 0.069(5) 0.052(4) -0.020(3) 0.014(3) -0.027(4) O16 0.086(6) 0.064(5) 0.060(5) -0.026(4) 0.018(4) -0.018(4) Cl6 0.0553(14) 0.0642(16) 0.0626(16) -0.0278(13) -0.0007(12) -0.0106(12) O21 0.075(6) 0.151(10) 0.073(6) -0.005(6) -0.017(5) -0.008(6) O22 0.139(9) 0.088(6) 0.095(7) -0.048(6) 0.021(6) -0.068(6) O23 0.092(6) 0.060(5) 0.099(7) -0.048(5) 0.025(5) -0.022(4) O24 0.052(4) 0.088(6) 0.108(7) -0.057(5) 0.010(4) -0.016(4) Cl7 0.097(3) 0.065(2) 0.112(3) -0.014(2) 0.003(2) -0.0007(18) Cl12 0.128(3) 0.076(2) 0.0552(17) -0.0320(16) -0.0148(18) -0.0069(19) O29 0.166(10) 0.062(5) 0.068(6) -0.025(5) -0.022(6) -0.006(6) O30 0.151(10) 0.125(9) 0.084(7) -0.071(7) 0.019(7) -0.058(8) O31 0.122(9) 0.182(13) 0.094(8) -0.070(8) -0.020(7) -0.027(9) O32 0.204(12) 0.058(5) 0.058(5) -0.026(4) -0.009(6) 0.003(6) Cl10 0.084(2) 0.143(4) 0.065(2) -0.015(2) 0.0292(18) -0.028(2) Cl4 0.144(5) 0.136(5) 0.281(10) -0.113(6) -0.023(5) -0.033(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 Nd1 O402 2.408(7) . ? Nd1 O101 2.437(7) . ? Nd1 O501 2.461(8) . ? Nd1 O503 2.486(8) . ? Nd1 N502 2.568(13) . ? Nd1 N407 2.623(8) . ? Nd1 N102 2.635(8) . ? Nd1 N406 2.680(9) . ? Nd1 N103 2.741(8) . ? Nd2 O201 2.393(6) . ? Nd2 O504 2.475(6) . ? Nd2 O102 2.477(6) . ? Nd2 O506 2.492(6) . ? Nd2 O505 2.516(6) . ? Nd2 N107 2.614(7) . ? Nd2 N202 2.618(7) . ? Nd2 N106 2.700(6) . ? Nd2 N203 2.703(7) . ? Nd3 O301 2.387(6) . ? Nd3 O202 2.451(6) . ? Nd3 O507 2.465(6) . ? Nd3 O509 2.488(7) . ? Nd3 O508 2.555(7) . ? Nd3 N207 2.604(7) . ? Nd3 N302 2.627(7) . ? Nd3 N303 2.692(7) . ? Nd3 N206 2.706(7) . ? Nd4 O1A' 2.375(14) . ? Nd4 O302 2.407(7) . ? Nd4 O1A 2.444(13) . ? Nd4 O510 2.481(7) . ? Nd4 O512 2.522(6) . ? Nd4 N2 2.522(10) . ? Nd4 O511 2.542(8) . ? Nd4 N307 2.629(7) . ? Nd4 N403 2.680(9) . ? Nd4 N306 2.692(7) . ? Nd4 N2' 2.754(11) . ? O101 C116 1.258(13) . ? O102 C130 1.270(10) . ? O201 C216 1.244(10) . ? O202 C230 1.262(11) . ? O301 C316 1.233(11) . ? O302 C330 1.273(12) . ? O402 C430 1.268(13) . ? N502 C501 1.16(2) . ? C501 C502 1.55(3) . ? C502 H50A 0.9800 . ? C502 H50B 0.9800 . ? C502 H50C 0.9800 . ? N101 C116 1.340(14) . ? N101 C117 1.486(5) . ? N101 C119 1.486(5) . ? N102 C115 1.329(12) . ? N102 C111 1.334(13) . ? N103 N104 1.350(10) . ? N103 C110 1.359(13) . ? N104 C108 1.338(14) . ? N104 C107 1.467(12) . ? N105 C122 1.331(12) . ? N105 N106 1.373(9) . ? N105 C121 1.483(11) . ? N106 C124 1.344(11) . ? N107 C129 1.345(10) . ? N107 C125 1.355(10) . ? N108 C130 1.320(11) . ? N108 C133 1.486(5) . ? N108 C131 1.486(5) . ? N201 C216 1.328(11) . ? N201 C217 1.486(5) . ? N201 C219 1.486(5) . ? N202 C211 1.331(11) . ? N202 C215 1.352(10) . ? N203 C210 1.340(11) . ? N203 N204 1.367(9) . ? N204 C208 1.339(12) . ? N204 C207 1.461(11) . ? N205 C222 1.348(13) . ? N205 N206 1.355(10) . ? N205 C221 1.468(12) . ? N206 C224 1.365(12) . ? N207 C225 1.343(12) . ? N207 C229 1.346(12) . ? N208 C230 1.327(13) . ? N208 C233 1.478(14) . ? N208 C231 1.489(13) . ? N301 C316 1.334(12) . ? N301 C319 1.498(6) . ? N301 C317 1.498(6) . ? N302 C315 1.333(11) . ? N302 C311 1.342(11) . ? N303 N304 1.355(10) . ? N303 C310 1.359(11) . ? N304 C308 1.356(12) . ? N304 C307 1.466(11) . ? N305 C322 1.338(14) . ? N305 N306 1.359(10) . ? N305 C321 1.476(13) . ? N306 C324 1.358(12) . ? N307 C325 1.338(11) . ? N307 C329 1.353(11) . ? N308 C330 1.324(12) . ? N308 C333 1.498(6) . ? N308 C331 1.498(6) . ? N403 C410 1.337(13) . ? N403 N404 1.371(13) . ? N404 C408 1.366(16) . ? N404 C407 1.448(15) . ? N405 C422 1.310(16) . ? N405 N406 1.384(12) . ? N405 C421 1.435(16) . ? N406 C424 1.339(14) . ? N407 C425 1.337(12) . ? N407 C429 1.341(12) . ? N408 C430 1.305(14) . ? N408 C433 1.498(6) . ? N408 C431 1.498(6) . ? C101 C102 1.386(14) . ? C101 C106 1.407(13) . ? C101 C107 1.495(14) . ? C102 C103 1.371(14) . ? C102 H102 0.9500 . ? C103 C104 1.403(13) . ? C103 H103 0.9500 . ? C104 C105 1.375(13) . ? C104 C121 1.515(13) . ? C105 C106 1.373(13) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C107 H10A 0.9900 . ? C107 H10B 0.9900 . ? C108 C109 1.359(15) . ? C108 H108 0.9500 . ? C109 C110 1.390(14) . ? C109 H109 0.9500 . ? C110 C111 1.476(13) . ? C111 C112 1.405(15) . ? C112 C113 1.376(15) . ? C112 H112 0.9500 . ? C113 C114 1.397(17) . ? C113 H113 0.9500 . ? C114 C115 1.377(15) . ? C114 H114 0.9500 . ? C115 C116 1.497(17) . ? C117 C118 1.479(19) . ? C117 H11A 0.9900 . ? C117 H11B 0.9900 . ? C118 H11C 0.9800 . ? C118 H11D 0.9800 . ? C118 H11E 0.9800 . ? C119 C120 1.505(19) . ? C119 H11F 0.9900 . ? C119 H11G 0.9900 . ? C120 H12A 0.9800 . ? C120 H12B 0.9800 . ? C120 H12C 0.9800 . ? C121 H12Y 0.9900 . ? C121 H12Z 0.9900 . ? C122 C123 1.411(14) . ? C122 H122 0.9500 . ? C123 C124 1.406(12) . ? C123 H123 0.9500 . ? C124 C125 1.448(12) . ? C125 C126 1.388(12) . ? C126 C127 1.351(14) . ? C126 H126 0.9500 . ? C127 C128 1.394(14) . ? C127 H127 0.9500 . ? C128 C129 1.393(12) . ? C128 H128 0.9500 . ? C129 C130 1.496(12) . ? C131 C132 1.514(16) . ? C131 H13A 0.9900 . ? C131 H13B 0.9900 . ? C132 H13C 0.9800 . ? C132 H13D 0.9800 . ? C132 H13E 0.9800 . ? C133 C134 1.509(13) . ? C133 H13F 0.9900 . ? C133 H13G 0.9900 . ? C134 H13H 0.9800 . ? C134 H13I 0.9800 . ? C134 H13J 0.9800 . ? C201 C206 1.389(12) . ? C201 C202 1.391(12) . ? C201 C207 1.521(12) . ? C202 C203 1.375(13) . ? C202 H202 0.9500 . ? C203 C204 1.403(13) . ? C203 H203 0.9500 . ? C204 C205 1.361(13) . ? C204 C221 1.523(13) . ? C205 C206 1.376(13) . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? C207 H20A 0.9900 . ? C207 H20B 0.9900 . ? C208 C209 1.338(13) . ? C208 H208 0.9500 . ? C209 C210 1.399(12) . ? C209 H209 0.9500 . ? C210 C211 1.463(12) . ? C211 C212 1.398(13) . ? C212 C213 1.358(14) . ? C212 H212 0.9500 . ? C213 C214 1.384(14) . ? C213 H213 0.9500 . ? C214 C215 1.376(13) . ? C214 H214 0.9500 . ? C215 C216 1.508(13) . ? C217 C218 1.52(2) . ? C217 H21A 0.9900 . ? C217 H21B 0.9900 . ? C218 H21C 0.9800 . ? C218 H21D 0.9800 . ? C218 H21E 0.9800 . ? C219 C220 1.483(16) . ? C219 H21F 0.9900 . ? C219 H21G 0.9900 . ? C220 H22A 0.9800 . ? C220 H22B 0.9800 . ? C220 H22C 0.9800 . ? C221 H22D 0.9900 . ? C221 H22E 0.9900 . ? C222 C223 1.353(16) . ? C222 H222 0.9500 . ? C223 C224 1.364(13) . ? C223 H223 0.9500 . ? C224 C225 1.456(14) . ? C225 C226 1.395(14) . ? C226 C227 1.345(16) . ? C226 H226 0.9500 . ? C227 C228 1.393(16) . ? C227 H227 0.9500 . ? C228 C229 1.403(14) . ? C228 H228 0.9500 . ? C229 C230 1.493(13) . ? C231 C232 1.474(15) . ? C231 H23A 0.9900 . ? C231 H23B 0.9900 . ? C232 H23C 0.9800 . ? C232 H23D 0.9800 . ? C232 H23E 0.9800 . ? C233 C234 1.50(2) . ? C233 H23F 0.9900 . ? C233 H23G 0.9900 . ? C234 H23H 0.9800 . ? C234 H23I 0.9800 . ? C234 H23J 0.9800 . ? C301 C306 1.388(13) . ? C301 C302 1.395(13) . ? C301 C307 1.504(13) . ? C302 C303 1.393(14) . ? C302 H302 0.9500 . ? C303 C304 1.388(14) . ? C303 H303 0.9500 . ? C304 C305 1.389(14) . ? C304 C321 1.505(14) . ? C305 C306 1.388(13) . ? C305 H305 0.9500 . ? C306 H306 0.9500 . ? C307 H30A 0.9900 . ? C307 H30B 0.9900 . ? C308 C309 1.394(14) . ? C308 H308 0.9500 . ? C309 C310 1.380(13) . ? C309 H309 0.9500 . ? C310 C311 1.461(13) . ? C311 C312 1.418(12) . ? C312 C313 1.367(14) . ? C312 H312 0.9500 . ? C313 C314 1.399(14) . ? C313 H313 0.9500 . ? C314 C315 1.387(12) . ? C314 H314 0.9500 . ? C315 C316 1.508(13) . ? C317 C318 1.52(2) . ? C317 H31A 0.9900 . ? C317 H31B 0.9900 . ? C318 H31C 0.9800 . ? C318 H31D 0.9800 . ? C318 H31E 0.9800 . ? C319 C320 1.527(18) . ? C319 H31Y 0.9900 . ? C319 H31Z 0.9900 . ? C320 H32A 0.9800 . ? C320 H32B 0.9800 . ? C320 H32C 0.9800 . ? C321 H32D 0.9900 . ? C321 H32E 0.9900 . ? C322 C323 1.359(17) . ? C322 H322 0.9500 . ? C323 C324 1.406(13) . ? C323 H323 0.9500 . ? C324 C325 1.449(13) . ? C325 C326 1.410(12) . ? C326 C327 1.335(15) . ? C326 H326 0.9500 . ? C327 C328 1.379(16) . ? C327 H327 0.9500 . ? C328 C329 1.402(13) . ? C328 H328 0.9500 . ? C329 C330 1.469(14) . ? C331 C332 1.490(19) . ? C331 H33A 0.9900 . ? C331 H33B 0.9900 . ? C332 H33C 0.9800 . ? C332 H33D 0.9800 . ? C332 H33E 0.9800 . ? C333 C334 1.59(2) . ? C333 H33F 0.9900 . ? C333 H33G 0.9900 . ? C334 H33H 0.9800 . ? C334 H33I 0.9800 . ? C334 H33J 0.9800 . ? C401 C406 1.394(17) . ? C401 C402 1.397(17) . ? C401 C407 1.499(18) . ? C402 C403 1.383(19) . ? C402 H402 0.9500 . ? C403 C404 1.404(17) . ? C403 H403 0.9500 . ? C404 C405 1.384(19) . ? C404 C421 1.54(2) . ? C405 C406 1.36(2) . ? C405 H405 0.9500 . ? C406 H406 0.9500 . ? C407 H40A 0.9900 . ? C407 H40B 0.9900 . ? C408 C409 1.35(2) . ? C408 H408 0.9500 . ? C409 C410 1.41(2) . ? C409 H409 0.9500 . ? C410 C11' 1.342(17) . ? C410 C11 1.520(17) . ? C421 H42A 0.9900 . ? C421 H42B 0.9900 . ? C422 C423 1.361(19) . ? C422 H422 0.9500 . ? C423 C424 1.383(16) . ? C423 H423 0.9500 . ? C424 C425 1.477(15) . ? C425 C426 1.384(15) . ? C426 C427 1.366(17) . ? C426 H426 0.9500 . ? C427 C428 1.354(17) . ? C427 H427 0.9500 . ? C428 C429 1.399(15) . ? C428 H428 0.9500 . ? C429 C430 1.506(15) . ? C431 C432 1.36(3) . ? C431 H43A 0.9900 . ? C431 H43B 0.9900 . ? C432 H43C 0.9800 . ? C432 H43D 0.9800 . ? C432 H43E 0.9800 . ? C433 C434 1.59(2) . ? C433 H43F 0.9900 . ? C433 H43G 0.9900 . ? C434 H43H 0.9800 . ? C434 H43I 0.9800 . ? C434 H43J 0.9800 . ? O1A C16 1.23(2) . ? N1 C19 1.486(5) . ? N1 C17 1.501(19) . ? N1 C16 1.51(3) . ? C11 C12 1.3900 . ? C11 N2 1.3900 . ? C12 C13 1.3900 . ? C12 H12 0.9500 . ? C13 C14 1.3900 . ? C13 H13 0.9500 . ? C14 C15 1.3900 . ? C14 H14 0.9500 . ? C15 N2 1.3900 . ? C15 C16 1.43(2) . ? C17 C18 1.54(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.59(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20C 0.9800 . ? C20 H20D 0.9800 . ? C20 H20E 0.9800 . ? O1A' C16' 1.23(2) . ? N1' C19' 1.486(5) . ? N1' C17' 1.486(5) . ? N1' C16' 1.52(3) . ? C11' C12' 1.3900 . ? C11' N2' 1.3900 . ? C12' C13' 1.3900 . ? C12' H12' 0.9500 . ? C13' C14' 1.3900 . ? C13' H13' 0.9500 . ? C14' C15' 1.3900 . ? C14' H14' 0.9500 . ? C15' N2' 1.3900 . ? C15' C16' 1.43(2) . ? C17' C18' 1.53(4) . ? C17' H17C 0.9900 . ? C17' H17D 0.9900 . ? C18' H18D 0.9800 . ? C18' H18E 0.9800 . ? C18' H18F 0.9800 . ? C19' C20' 1.58(5) . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C20' H20F 0.9800 . ? C20' H20G 0.9800 . ? C20' H20H 0.9800 . ? Cl1 O3' 1.411(13) . ? Cl1 O4 1.417(11) . ? Cl1 O2 1.420(13) . ? Cl1 O2' 1.437(13) . ? Cl1 O1 1.445(9) . ? Cl1 O4' 1.449(11) . ? Cl1 O3 1.464(12) . ? Cl2 O8' 1.408(13) . ? Cl2 O5' 1.410(14) . ? Cl2 O6 1.420(15) . ? Cl2 O7 1.420(10) . ? Cl2 O8 1.422(14) . ? Cl2 O6' 1.431(15) . ? Cl2 O5 1.453(15) . ? Cl3 O9 1.378(15) . ? Cl3 O10 1.382(18) . ? Cl3 O12 1.399(13) . ? Cl3 O11 1.44(2) . ? Cl3' O10' 1.386(18) . ? Cl3' O9' 1.389(15) . ? Cl3' O12' 1.405(13) . ? Cl3' O11' 1.43(3) . ? Cl11 O13 1.422(7) . ? Cl11 O15 1.432(7) . ? Cl11 O14 1.439(7) . ? Cl11 O16 1.447(8) . ? Cl5 O19 1.366(13) . ? Cl5 O17 1.407(17) . ? Cl5 O18 1.437(15) . ? Cl5 O20 1.46(2) . ? Cl5' O19' 1.357(13) . ? Cl5' O18' 1.392(15) . ? Cl5' O17' 1.423(16) . ? Cl5' O20' 1.46(2) . ? Cl6 O21 1.404(10) . ? Cl6 O24 1.422(8) . ? Cl6 O23 1.439(8) . ? Cl6 O22 1.454(9) . ? Cl7 O28 1.375(11) . ? Cl7 O25 1.397(12) . ? Cl7 O26 1.402(13) . ? Cl7 O27 1.406(13) . ? Cl12 O29 1.411(10) . ? Cl12 O31 1.420(12) . ? Cl12 O32 1.424(9) . ? Cl12 O30 1.497(12) . ? Cl9 O36 1.375(19) . ? Cl9 O33 1.392(14) . ? Cl9 O34 1.427(13) . ? Cl9 O35 1.485(16) . ? Cl9' O33' 1.39(2) . ? Cl9' O36' 1.39(2) . ? Cl9' O35' 1.45(2) . ? Cl9' O34' 1.49(2) . ? Cl10 O40 1.375(14) . ? Cl10 O37' 1.380(16) . ? Cl10 O38' 1.423(16) . ? Cl10 O39 1.430(14) . ? Cl10 O39' 1.454(16) . ? Cl10 O37 1.456(13) . ? Cl10 O40' 1.462(16) . ? Cl10 O38 1.475(14) . ? Cl4 O43 1.501(16) . ? Cl4 O41' 1.506(18) . ? Cl4 O43' 1.506(16) . ? Cl4 O42 1.509(18) . ? Cl4 O42' 1.533(18) . ? Cl4 O41 1.536(18) . ? Cl4 O44 1.546(18) . ? Cl4 O44' 1.555(18) . ? Cl8 O45 1.348(17) . ? Cl8 O48 1.468(19) . ? Cl8 O46 1.491(19) . ? Cl8 O47 1.504(18) . ? Cl8' O45' 1.327(17) . ? Cl8' O48' 1.474(19) . ? Cl8' O47' 1.493(18) . ? Cl8' O46' 1.502(19) . ? N1S C1S 1.166(16) . ? C1S C2S 1.466(18) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? N2S C3S 1.173(16) . ? C3S C4S 1.494(19) . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? N3S C5S 1.180(17) . ? C5S C6S 1.492(19) . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? N4S C7S 1.182(16) . ? C7S C8S 1.492(19) . ? C8S H8S1 0.9800 . ? C8S H8S2 0.9800 . ? C8S H8S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O402 Nd1 O101 88.8(3) . . ? O402 Nd1 O501 137.0(3) . . ? O101 Nd1 O501 83.0(3) . . ? O402 Nd1 O503 74.3(3) . . ? O101 Nd1 O503 75.4(3) . . ? O501 Nd1 O503 141.8(3) . . ? O402 Nd1 N502 143.1(3) . . ? O101 Nd1 N502 70.6(3) . . ? O501 Nd1 N502 72.2(4) . . ? O503 Nd1 N502 71.1(4) . . ? O402 Nd1 N407 62.3(2) . . ? O101 Nd1 N407 138.2(3) . . ? O501 Nd1 N407 138.8(3) . . ? O503 Nd1 N407 68.2(3) . . ? N502 Nd1 N407 114.1(3) . . ? O402 Nd1 N102 68.8(3) . . ? O101 Nd1 N102 62.5(2) . . ? O501 Nd1 N102 70.0(3) . . ? O503 Nd1 N102 123.2(3) . . ? N502 Nd1 N102 121.9(3) . . ? N407 Nd1 N102 123.6(2) . . ? O402 Nd1 N406 122.9(3) . . ? O101 Nd1 N406 141.5(3) . . ? O501 Nd1 N406 85.8(3) . . ? O503 Nd1 N406 91.8(3) . . ? N502 Nd1 N406 71.0(3) . . ? N407 Nd1 N406 61.1(2) . . ? N102 Nd1 N406 144.6(3) . . ? O402 Nd1 N103 74.9(3) . . ? O101 Nd1 N103 122.8(2) . . ? O501 Nd1 N103 74.6(3) . . ? O503 Nd1 N103 143.5(3) . . ? N502 Nd1 N103 142.0(3) . . ? N407 Nd1 N103 80.5(2) . . ? N102 Nd1 N103 60.5(2) . . ? N406 Nd1 N103 88.9(2) . . ? O201 Nd2 O504 83.0(2) . . ? O201 Nd2 O102 88.8(2) . . ? O504 Nd2 O102 135.61(19) . . ? O201 Nd2 O506 75.2(2) . . ? O504 Nd2 O506 140.1(2) . . ? O102 Nd2 O506 77.5(2) . . ? O201 Nd2 O505 73.1(2) . . ? O504 Nd2 O505 71.5(2) . . ? O102 Nd2 O505 146.1(2) . . ? O506 Nd2 O505 70.3(2) . . ? O201 Nd2 N107 137.8(2) . . ? O504 Nd2 N107 139.2(2) . . ? O102 Nd2 N107 62.4(2) . . ? O506 Nd2 N107 69.2(2) . . ? O505 Nd2 N107 113.5(2) . . ? O201 Nd2 N202 62.9(2) . . ? O504 Nd2 N202 70.1(2) . . ? O102 Nd2 N202 67.4(2) . . ? O506 Nd2 N202 124.5(2) . . ? O505 Nd2 N202 123.8(2) . . ? N107 Nd2 N202 122.5(2) . . ? O201 Nd2 N106 141.4(2) . . ? O504 Nd2 N106 86.91(19) . . ? O102 Nd2 N106 122.98(19) . . ? O506 Nd2 N106 89.8(2) . . ? O505 Nd2 N106 68.4(2) . . ? N107 Nd2 N106 61.1(2) . . ? N202 Nd2 N106 145.4(2) . . ? O201 Nd2 N203 124.0(2) . . ? O504 Nd2 N203 74.2(2) . . ? O102 Nd2 N203 74.9(2) . . ? O506 Nd2 N203 145.5(2) . . ? O505 Nd2 N203 139.0(2) . . ? N107 Nd2 N203 79.8(2) . . ? N202 Nd2 N203 61.3(2) . . ? N106 Nd2 N203 88.2(2) . . ? O301 Nd3 O202 83.4(2) . . ? O301 Nd3 O507 84.7(3) . . ? O202 Nd3 O507 138.8(2) . . ? O301 Nd3 O509 75.6(2) . . ? O202 Nd3 O509 74.8(2) . . ? O507 Nd3 O509 138.8(2) . . ? O301 Nd3 O508 74.5(2) . . ? O202 Nd3 O508 142.0(2) . . ? O507 Nd3 O508 70.0(2) . . ? O509 Nd3 O508 70.0(2) . . ? O301 Nd3 N207 136.2(2) . . ? O202 Nd3 N207 63.0(2) . . ? O507 Nd3 N207 139.1(2) . . ? O509 Nd3 N207 69.4(2) . . ? O508 Nd3 N207 115.0(2) . . ? O301 Nd3 N302 62.3(2) . . ? O202 Nd3 N302 66.5(2) . . ? O507 Nd3 N302 73.0(2) . . ? O509 Nd3 N302 124.5(2) . . ? O508 Nd3 N302 124.7(2) . . ? N207 Nd3 N302 120.0(2) . . ? O301 Nd3 N303 124.2(2) . . ? O202 Nd3 N303 79.4(2) . . ? O507 Nd3 N303 75.2(2) . . ? O509 Nd3 N303 145.3(2) . . ? O508 Nd3 N303 138.5(2) . . ? N207 Nd3 N303 78.5(2) . . ? N302 Nd3 N303 62.1(2) . . ? O301 Nd3 N206 144.3(2) . . ? O202 Nd3 N206 124.2(2) . . ? O507 Nd3 N206 85.9(2) . . ? O509 Nd3 N206 89.6(2) . . ? O508 Nd3 N206 69.9(2) . . ? N207 Nd3 N206 61.4(2) . . ? N302 Nd3 N206 145.2(2) . . ? N303 Nd3 N206 86.1(2) . . ? O1A' Nd4 O302 75.8(5) . . ? O1A' Nd4 O1A 15.0(4) . . ? O302 Nd4 O1A 89.7(4) . . ? O1A' Nd4 O510 92.4(4) . . ? O302 Nd4 O510 138.5(3) . . ? O1A Nd4 O510 85.5(4) . . ? O1A' Nd4 O512 75.7(4) . . ? O302 Nd4 O512 78.7(2) . . ? O1A Nd4 O512 72.6(3) . . ? O510 Nd4 O512 137.4(3) . . ? O1A' Nd4 N2 54.1(4) . . ? O302 Nd4 N2 71.7(3) . . ? O1A Nd4 N2 63.5(4) . . ? O510 Nd4 N2 69.3(4) . . ? O512 Nd4 N2 126.1(3) . . ? O1A' Nd4 O511 81.4(5) . . ? O302 Nd4 O511 143.7(3) . . ? O1A Nd4 O511 66.4(4) . . ? O510 Nd4 O511 69.4(3) . . ? O512 Nd4 O511 68.4(3) . . ? N2 Nd4 O511 115.8(4) . . ? O1A' Nd4 N307 127.1(4) . . ? O302 Nd4 N307 61.5(2) . . ? O1A Nd4 N307 133.7(4) . . ? O510 Nd4 N307 140.3(2) . . ? O512 Nd4 N307 67.0(2) . . ? N2 Nd4 N307 127.7(3) . . ? O511 Nd4 N307 115.6(3) . . ? O1A' Nd4 N403 118.7(4) . . ? O302 Nd4 N403 80.8(3) . . ? O1A Nd4 N403 127.9(4) . . ? O510 Nd4 N403 70.3(3) . . ? O512 Nd4 N403 150.9(3) . . ? N2 Nd4 N403 65.0(3) . . ? O511 Nd4 N403 135.3(3) . . ? N307 Nd4 N403 85.0(3) . . ? O1A' Nd4 N306 151.2(4) . . ? O302 Nd4 N306 123.2(2) . . ? O1A Nd4 N306 136.9(4) . . ? O510 Nd4 N306 85.5(2) . . ? O512 Nd4 N306 86.4(2) . . ? N2 Nd4 N306 147.4(3) . . ? O511 Nd4 N306 71.0(3) . . ? N307 Nd4 N306 62.2(2) . . ? N403 Nd4 N306 87.6(2) . . ? O1A' Nd4 N2' 60.4(4) . . ? O302 Nd4 N2' 61.0(4) . . ? O1A Nd4 N2' 71.9(4) . . ? O510 Nd4 N2' 78.4(4) . . ? O512 Nd4 N2' 125.4(3) . . ? N2 Nd4 N2' 12.7(4) . . ? O511 Nd4 N2' 128.4(4) . . ? N307 Nd4 N2' 115.0(4) . . ? N403 Nd4 N2' 58.7(3) . . ? N306 Nd4 N2' 145.8(3) . . ? C116 O101 Nd1 120.5(6) . . ? C130 O102 Nd2 122.2(5) . . ? C216 O201 Nd2 124.7(5) . . ? C230 O202 Nd3 122.1(5) . . ? C316 O301 Nd3 126.9(6) . . ? C330 O302 Nd4 127.6(6) . . ? C430 O402 Nd1 126.0(6) . . ? C501 N502 Nd1 156.9(15) . . ? N502 C501 C502 174(3) . . ? C501 C502 H50A 109.5 . . ? C501 C502 H50B 109.5 . . ? H50A C502 H50B 109.5 . . ? C501 C502 H50C 109.5 . . ? H50A C502 H50C 109.5 . . ? H50B C502 H50C 109.5 . . ? C116 N101 C117 126.4(9) . . ? C116 N101 C119 117.0(9) . . ? C117 N101 C119 115.3(9) . . ? C115 N102 C111 119.0(9) . . ? C115 N102 Nd1 117.3(7) . . ? C111 N102 Nd1 121.6(6) . . ? N104 N103 C110 103.3(8) . . ? N104 N103 Nd1 138.9(6) . . ? C110 N103 Nd1 116.5(6) . . ? C108 N104 N103 112.2(8) . . ? C108 N104 C107 126.6(8) . . ? N103 N104 C107 121.1(8) . . ? C122 N105 N106 112.4(7) . . ? C122 N105 C121 125.7(7) . . ? N106 N105 C121 121.2(7) . . ? C124 N106 N105 104.8(6) . . ? C124 N106 Nd2 113.4(5) . . ? N105 N106 Nd2 133.9(5) . . ? C129 N107 C125 118.1(7) . . ? C129 N107 Nd2 118.0(5) . . ? C125 N107 Nd2 118.5(5) . . ? C130 N108 C133 125.2(7) . . ? C130 N108 C131 120.0(7) . . ? C133 N108 C131 114.7(7) . . ? C216 N201 C217 126.3(8) . . ? C216 N201 C219 118.2(7) . . ? C217 N201 C219 115.4(8) . . ? C211 N202 C215 119.3(7) . . ? C211 N202 Nd2 121.0(5) . . ? C215 N202 Nd2 117.1(5) . . ? C210 N203 N204 103.9(6) . . ? C210 N203 Nd2 117.1(5) . . ? N204 N203 Nd2 138.8(5) . . ? C208 N204 N203 111.1(7) . . ? C208 N204 C207 126.6(7) . . ? N203 N204 C207 122.2(7) . . ? C222 N205 N206 110.3(8) . . ? C222 N205 C221 128.0(8) . . ? N206 N205 C221 120.9(7) . . ? N205 N206 C224 103.8(7) . . ? N205 N206 Nd3 133.4(6) . . ? C224 N206 Nd3 113.3(5) . . ? C225 N207 C229 119.4(8) . . ? C225 N207 Nd3 118.7(6) . . ? C229 N207 Nd3 117.4(6) . . ? C230 N208 C233 123.8(9) . . ? C230 N208 C231 118.6(8) . . ? C233 N208 C231 117.3(9) . . ? C316 N301 C319 126.5(8) . . ? C316 N301 C317 118.0(9) . . ? C319 N301 C317 115.3(9) . . ? C315 N302 C311 119.4(7) . . ? C315 N302 Nd3 117.7(6) . . ? C311 N302 Nd3 119.8(5) . . ? N304 N303 C310 104.3(7) . . ? N304 N303 Nd3 139.0(5) . . ? C310 N303 Nd3 116.4(5) . . ? N303 N304 C308 112.4(7) . . ? N303 N304 C307 122.7(7) . . ? C308 N304 C307 124.9(7) . . ? C322 N305 N306 111.9(8) . . ? C322 N305 C321 127.4(9) . . ? N306 N305 C321 120.4(8) . . ? C324 N306 N305 104.1(7) . . ? C324 N306 Nd4 114.3(5) . . ? N305 N306 Nd4 136.7(6) . . ? C325 N307 C329 118.6(7) . . ? C325 N307 Nd4 119.0(5) . . ? C329 N307 Nd4 118.3(5) . . ? C330 N308 C333 118.7(10) . . ? C330 N308 C331 126.6(9) . . ? C333 N308 C331 114.5(10) . . ? C410 N403 N404 105.3(9) . . ? C410 N403 Nd4 116.7(8) . . ? N404 N403 Nd4 137.9(6) . . ? C408 N404 N403 110.3(12) . . ? C408 N404 C407 126.5(12) . . ? N403 N404 C407 123.1(9) . . ? C422 N405 N406 110.9(10) . . ? C422 N405 C421 127.5(11) . . ? N406 N405 C421 121.1(10) . . ? C424 N406 N405 103.1(9) . . ? C424 N406 Nd1 116.2(6) . . ? N405 N406 Nd1 134.6(7) . . ? C425 N407 C429 117.2(9) . . ? C425 N407 Nd1 119.8(6) . . ? C429 N407 Nd1 118.6(6) . . ? C430 N408 C433 122.4(11) . . ? C430 N408 C431 117.9(12) . . ? C433 N408 C431 119.5(12) . . ? C102 C101 C106 117.3(9) . . ? C102 C101 C107 119.5(9) . . ? C106 C101 C107 123.3(8) . . ? C103 C102 C101 122.2(9) . . ? C103 C102 H102 118.9 . . ? C101 C102 H102 118.9 . . ? C102 C103 C104 120.0(9) . . ? C102 C103 H103 120.0 . . ? C104 C103 H103 120.0 . . ? C105 C104 C103 118.2(9) . . ? C105 C104 C121 120.5(8) . . ? C103 C104 C121 121.2(8) . . ? C106 C105 C104 121.8(9) . . ? C106 C105 H105 119.1 . . ? C104 C105 H105 119.1 . . ? C105 C106 C101 120.5(9) . . ? C105 C106 H106 119.8 . . ? C101 C106 H106 119.8 . . ? N104 C107 C101 114.1(8) . . ? N104 C107 H10A 108.7 . . ? C101 C107 H10A 108.7 . . ? N104 C107 H10B 108.7 . . ? C101 C107 H10B 108.7 . . ? H10A C107 H10B 107.6 . . ? N104 C108 C109 108.4(9) . . ? N104 C108 H108 125.8 . . ? C109 C108 H108 125.8 . . ? C108 C109 C110 104.2(10) . . ? C108 C109 H109 127.9 . . ? C110 C109 H109 127.9 . . ? N103 C110 C109 111.9(8) . . ? N103 C110 C111 118.3(9) . . ? C109 C110 C111 129.5(10) . . ? N102 C111 C112 122.3(9) . . ? N102 C111 C110 116.2(9) . . ? C112 C111 C110 121.6(10) . . ? C113 C112 C111 117.8(11) . . ? C113 C112 H112 121.1 . . ? C111 C112 H112 121.1 . . ? C112 C113 C114 119.5(11) . . ? C112 C113 H113 120.2 . . ? C114 C113 H113 120.2 . . ? C115 C114 C113 118.4(9) . . ? C115 C114 H114 120.8 . . ? C113 C114 H114 120.8 . . ? N102 C115 C114 122.7(10) . . ? N102 C115 C116 111.4(9) . . ? C114 C115 C116 125.6(9) . . ? O101 C116 N101 123.2(11) . . ? O101 C116 C115 115.5(10) . . ? N101 C116 C115 121.4(10) . . ? C118 C117 N101 111.2(12) . . ? C118 C117 H11A 109.4 . . ? N101 C117 H11A 109.4 . . ? C118 C117 H11B 109.4 . . ? N101 C117 H11B 109.4 . . ? H11A C117 H11B 108.0 . . ? C117 C118 H11C 109.5 . . ? C117 C118 H11D 109.5 . . ? H11C C118 H11D 109.5 . . ? C117 C118 H11E 109.5 . . ? H11C C118 H11E 109.5 . . ? H11D C118 H11E 109.5 . . ? N101 C119 C120 111.9(10) . . ? N101 C119 H11F 109.2 . . ? C120 C119 H11F 109.2 . . ? N101 C119 H11G 109.2 . . ? C120 C119 H11G 109.2 . . ? H11F C119 H11G 107.9 . . ? C119 C120 H12A 109.5 . . ? C119 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? C119 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? N105 C121 C104 111.5(7) . . ? N105 C121 H12Y 109.3 . . ? C104 C121 H12Y 109.3 . . ? N105 C121 H12Z 109.3 . . ? C104 C121 H12Z 109.3 . . ? H12Y C121 H12Z 108.0 . . ? N105 C122 C123 107.1(8) . . ? N105 C122 H122 126.4 . . ? C123 C122 H122 126.4 . . ? C124 C123 C122 104.3(8) . . ? C124 C123 H123 127.8 . . ? C122 C123 H123 127.8 . . ? N106 C124 C123 111.3(8) . . ? N106 C124 C125 120.5(7) . . ? C123 C124 C125 128.2(8) . . ? N107 C125 C126 121.5(8) . . ? N107 C125 C124 115.0(7) . . ? C126 C125 C124 123.5(8) . . ? C127 C126 C125 119.4(9) . . ? C127 C126 H126 120.3 . . ? C125 C126 H126 120.3 . . ? C126 C127 C128 121.0(8) . . ? C126 C127 H127 119.5 . . ? C128 C127 H127 119.5 . . ? C129 C128 C127 116.5(8) . . ? C129 C128 H128 121.7 . . ? C127 C128 H128 121.7 . . ? N107 C129 C128 123.4(8) . . ? N107 C129 C130 111.4(7) . . ? C128 C129 C130 125.0(8) . . ? O102 C130 N108 123.3(8) . . ? O102 C130 C129 115.0(7) . . ? N108 C130 C129 121.8(7) . . ? N108 C131 C132 111.7(9) . . ? N108 C131 H13A 109.3 . . ? C132 C131 H13A 109.3 . . ? N108 C131 H13B 109.3 . . ? C132 C131 H13B 109.3 . . ? H13A C131 H13B 107.9 . . ? C131 C132 H13C 109.5 . . ? C131 C132 H13D 109.5 . . ? H13C C132 H13D 109.5 . . ? C131 C132 H13E 109.5 . . ? H13C C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? N108 C133 C134 110.9(8) . . ? N108 C133 H13F 109.5 . . ? C134 C133 H13F 109.5 . . ? N108 C133 H13G 109.5 . . ? C134 C133 H13G 109.5 . . ? H13F C133 H13G 108.0 . . ? C133 C134 H13H 109.5 . . ? C133 C134 H13I 109.5 . . ? H13H C134 H13I 109.5 . . ? C133 C134 H13J 109.5 . . ? H13H C134 H13J 109.5 . . ? H13I C134 H13J 109.5 . . ? C206 C201 C202 118.6(8) . . ? C206 C201 C207 124.0(8) . . ? C202 C201 C207 117.3(8) . . ? C203 C202 C201 120.5(9) . . ? C203 C202 H202 119.8 . . ? C201 C202 H202 119.8 . . ? C202 C203 C204 120.3(8) . . ? C202 C203 H203 119.9 . . ? C204 C203 H203 119.9 . . ? C205 C204 C203 118.9(8) . . ? C205 C204 C221 120.5(8) . . ? C203 C204 C221 120.6(8) . . ? C204 C205 C206 121.3(8) . . ? C204 C205 H205 119.4 . . ? C206 C205 H205 119.4 . . ? C205 C206 C201 120.5(8) . . ? C205 C206 H206 119.8 . . ? C201 C206 H206 119.8 . . ? N204 C207 C201 114.6(7) . . ? N204 C207 H20A 108.6 . . ? C201 C207 H20A 108.6 . . ? N204 C207 H20B 108.6 . . ? C201 C207 H20B 108.6 . . ? H20A C207 H20B 107.6 . . ? C209 C208 N204 108.6(8) . . ? C209 C208 H208 125.7 . . ? N204 C208 H208 125.7 . . ? C208 C209 C210 105.1(8) . . ? C208 C209 H209 127.4 . . ? C210 C209 H209 127.4 . . ? N203 C210 C209 111.2(8) . . ? N203 C210 C211 119.7(7) . . ? C209 C210 C211 129.1(8) . . ? N202 C211 C212 121.1(8) . . ? N202 C211 C210 115.8(7) . . ? C212 C211 C210 123.0(8) . . ? C213 C212 C211 119.2(9) . . ? C213 C212 H212 120.4 . . ? C211 C212 H212 120.4 . . ? C212 C213 C214 119.9(9) . . ? C212 C213 H213 120.1 . . ? C214 C213 H213 120.1 . . ? C215 C214 C213 118.5(9) . . ? C215 C214 H214 120.7 . . ? C213 C214 H214 120.7 . . ? N202 C215 C214 121.7(8) . . ? N202 C215 C216 110.9(7) . . ? C214 C215 C216 127.1(8) . . ? O201 C216 N201 120.8(8) . . ? O201 C216 C215 116.0(7) . . ? N201 C216 C215 123.2(8) . . ? N201 C217 C218 112.1(11) . . ? N201 C217 H21A 109.2 . . ? C218 C217 H21A 109.2 . . ? N201 C217 H21B 109.2 . . ? C218 C217 H21B 109.2 . . ? H21A C217 H21B 107.9 . . ? C217 C218 H21C 109.5 . . ? C217 C218 H21D 109.5 . . ? H21C C218 H21D 109.5 . . ? C217 C218 H21E 109.5 . . ? H21C C218 H21E 109.5 . . ? H21D C218 H21E 109.5 . . ? C220 C219 N201 111.5(9) . . ? C220 C219 H21F 109.3 . . ? N201 C219 H21F 109.3 . . ? C220 C219 H21G 109.3 . . ? N201 C219 H21G 109.3 . . ? H21F C219 H21G 108.0 . . ? C219 C220 H22A 109.5 . . ? C219 C220 H22B 109.5 . . ? H22A C220 H22B 109.5 . . ? C219 C220 H22C 109.5 . . ? H22A C220 H22C 109.5 . . ? H22B C220 H22C 109.5 . . ? N205 C221 C204 113.1(8) . . ? N205 C221 H22D 109.0 . . ? C204 C221 H22D 109.0 . . ? N205 C221 H22E 109.0 . . ? C204 C221 H22E 109.0 . . ? H22D C221 H22E 107.8 . . ? N205 C222 C223 109.2(9) . . ? N205 C222 H222 125.4 . . ? C223 C222 H222 125.4 . . ? C222 C223 C224 104.7(9) . . ? C222 C223 H223 127.7 . . ? C224 C223 H223 127.7 . . ? C223 C224 N206 112.0(9) . . ? C223 C224 C225 129.6(9) . . ? N206 C224 C225 118.3(8) . . ? N207 C225 C226 121.0(9) . . ? N207 C225 C224 116.9(8) . . ? C226 C225 C224 122.0(9) . . ? C227 C226 C225 119.9(10) . . ? C227 C226 H226 120.1 . . ? C225 C226 H226 120.1 . . ? C226 C227 C228 120.4(10) . . ? C226 C227 H227 119.8 . . ? C228 C227 H227 119.8 . . ? C227 C228 C229 117.6(10) . . ? C227 C228 H228 121.2 . . ? C229 C228 H228 121.2 . . ? N207 C229 C228 121.7(9) . . ? N207 C229 C230 112.8(8) . . ? C228 C229 C230 124.8(9) . . ? O202 C230 N208 122.3(9) . . ? O202 C230 C229 115.2(9) . . ? N208 C230 C229 122.4(9) . . ? C232 C231 N208 110.6(9) . . ? C232 C231 H23A 109.5 . . ? N208 C231 H23A 109.5 . . ? C232 C231 H23B 109.5 . . ? N208 C231 H23B 109.5 . . ? H23A C231 H23B 108.1 . . ? C231 C232 H23C 109.5 . . ? C231 C232 H23D 109.5 . . ? H23C C232 H23D 109.5 . . ? C231 C232 H23E 109.5 . . ? H23C C232 H23E 109.5 . . ? H23D C232 H23E 109.5 . . ? N208 C233 C234 112.4(11) . . ? N208 C233 H23F 109.1 . . ? C234 C233 H23F 109.1 . . ? N208 C233 H23G 109.1 . . ? C234 C233 H23G 109.1 . . ? H23F C233 H23G 107.8 . . ? C233 C234 H23H 109.5 . . ? C233 C234 H23I 109.5 . . ? H23H C234 H23I 109.5 . . ? C233 C234 H23J 109.5 . . ? H23H C234 H23J 109.5 . . ? H23I C234 H23J 109.5 . . ? C306 C301 C302 118.0(9) . . ? C306 C301 C307 124.0(8) . . ? C302 C301 C307 118.0(8) . . ? C303 C302 C301 121.3(9) . . ? C303 C302 H302 119.3 . . ? C301 C302 H302 119.3 . . ? C304 C303 C302 120.2(9) . . ? C304 C303 H303 119.9 . . ? C302 C303 H303 119.9 . . ? C303 C304 C305 118.4(9) . . ? C303 C304 C321 122.3(9) . . ? C305 C304 C321 119.2(10) . . ? C306 C305 C304 121.2(9) . . ? C306 C305 H305 119.4 . . ? C304 C305 H305 119.4 . . ? C305 C306 C301 120.7(9) . . ? C305 C306 H306 119.6 . . ? C301 C306 H306 119.6 . . ? N304 C307 C301 114.1(7) . . ? N304 C307 H30A 108.7 . . ? C301 C307 H30A 108.7 . . ? N304 C307 H30B 108.7 . . ? C301 C307 H30B 108.7 . . ? H30A C307 H30B 107.6 . . ? N304 C308 C309 106.3(8) . . ? N304 C308 H308 126.9 . . ? C309 C308 H308 126.9 . . ? C310 C309 C308 105.5(8) . . ? C310 C309 H309 127.3 . . ? C308 C309 H309 127.3 . . ? N303 C310 C309 111.5(8) . . ? N303 C310 C311 119.8(8) . . ? C309 C310 C311 128.3(8) . . ? N302 C311 C312 120.9(8) . . ? N302 C311 C310 116.8(7) . . ? C312 C311 C310 122.3(8) . . ? C313 C312 C311 119.4(9) . . ? C313 C312 H312 120.3 . . ? C311 C312 H312 120.3 . . ? C312 C313 C314 118.8(8) . . ? C312 C313 H313 120.6 . . ? C314 C313 H313 120.6 . . ? C315 C314 C313 118.8(9) . . ? C315 C314 H314 120.6 . . ? C313 C314 H314 120.6 . . ? N302 C315 C314 122.6(8) . . ? N302 C315 C316 111.3(7) . . ? C314 C315 C316 125.9(8) . . ? O301 C316 N301 119.5(9) . . ? O301 C316 C315 116.4(8) . . ? N301 C316 C315 124.1(8) . . ? N301 C317 C318 108.6(12) . . ? N301 C317 H31A 110.0 . . ? C318 C317 H31A 110.0 . . ? N301 C317 H31B 110.0 . . ? C318 C317 H31B 110.0 . . ? H31A C317 H31B 108.3 . . ? C317 C318 H31C 109.5 . . ? C317 C318 H31D 109.5 . . ? H31C C318 H31D 109.5 . . ? C317 C318 H31E 109.5 . . ? H31C C318 H31E 109.5 . . ? H31D C318 H31E 109.5 . . ? N301 C319 C320 112.4(10) . . ? N301 C319 H31Y 109.1 . . ? C320 C319 H31Y 109.1 . . ? N301 C319 H31Z 109.1 . . ? C320 C319 H31Z 109.1 . . ? H31Y C319 H31Z 107.9 . . ? C319 C320 H32A 109.5 . . ? C319 C320 H32B 109.5 . . ? H32A C320 H32B 109.5 . . ? C319 C320 H32C 109.5 . . ? H32A C320 H32C 109.5 . . ? H32B C320 H32C 109.5 . . ? N305 C321 C304 113.0(9) . . ? N305 C321 H32D 109.0 . . ? C304 C321 H32D 109.0 . . ? N305 C321 H32E 109.0 . . ? C304 C321 H32E 109.0 . . ? H32D C321 H32E 107.8 . . ? N305 C322 C323 108.5(9) . . ? N305 C322 H322 125.7 . . ? C323 C322 H322 125.7 . . ? C322 C323 C324 104.6(10) . . ? C322 C323 H323 127.7 . . ? C324 C323 H323 127.7 . . ? N306 C324 C323 110.9(8) . . ? N306 C324 C325 120.9(8) . . ? C323 C324 C325 128.2(9) . . ? N307 C325 C326 121.9(8) . . ? N307 C325 C324 116.8(7) . . ? C326 C325 C324 121.3(8) . . ? C327 C326 C325 118.9(10) . . ? C327 C326 H326 120.6 . . ? C325 C326 H326 120.6 . . ? C326 C327 C328 120.7(10) . . ? C326 C327 H327 119.6 . . ? C328 C327 H327 119.6 . . ? C327 C328 C329 118.5(9) . . ? C327 C328 H328 120.8 . . ? C329 C328 H328 120.8 . . ? N307 C329 C328 121.2(9) . . ? N307 C329 C330 111.5(8) . . ? C328 C329 C330 127.2(9) . . ? O302 C330 N308 120.1(9) . . ? O302 C330 C329 115.8(8) . . ? N308 C330 C329 124.1(9) . . ? C332 C331 N308 112.5(12) . . ? C332 C331 H33A 109.1 . . ? N308 C331 H33A 109.1 . . ? C332 C331 H33B 109.1 . . ? N308 C331 H33B 109.1 . . ? H33A C331 H33B 107.8 . . ? C331 C332 H33C 109.5 . . ? C331 C332 H33D 109.5 . . ? H33C C332 H33D 109.5 . . ? C331 C332 H33E 109.5 . . ? H33C C332 H33E 109.5 . . ? H33D C332 H33E 109.5 . . ? N308 C333 C334 104.7(12) . . ? N308 C333 H33F 110.8 . . ? C334 C333 H33F 110.8 . . ? N308 C333 H33G 110.8 . . ? C334 C333 H33G 110.8 . . ? H33F C333 H33G 108.9 . . ? C333 C334 H33H 109.5 . . ? C333 C334 H33I 109.5 . . ? H33H C334 H33I 109.5 . . ? C333 C334 H33J 109.5 . . ? H33H C334 H33J 109.5 . . ? H33I C334 H33J 109.5 . . ? C406 C401 C402 116.0(13) . . ? C406 C401 C407 124.3(12) . . ? C402 C401 C407 119.6(11) . . ? C403 C402 C401 122.3(12) . . ? C403 C402 H402 118.8 . . ? C401 C402 H402 118.8 . . ? C402 C403 C404 120.2(13) . . ? C402 C403 H403 119.9 . . ? C404 C403 H403 119.9 . . ? C405 C404 C403 117.2(14) . . ? C405 C404 C421 121.0(12) . . ? C403 C404 C421 121.8(13) . . ? C406 C405 C404 122.0(12) . . ? C406 C405 H405 119.0 . . ? C404 C405 H405 119.0 . . ? C405 C406 C401 122.1(13) . . ? C405 C406 H406 118.9 . . ? C401 C406 H406 118.9 . . ? N404 C407 C401 112.9(10) . . ? N404 C407 H40A 109.0 . . ? C401 C407 H40A 109.0 . . ? N404 C407 H40B 109.0 . . ? C401 C407 H40B 109.0 . . ? H40A C407 H40B 107.8 . . ? C409 C408 N404 108.1(14) . . ? C409 C408 H408 125.9 . . ? N404 C408 H408 125.9 . . ? C408 C409 C410 105.4(13) . . ? C408 C409 H409 127.3 . . ? C410 C409 H409 127.3 . . ? N403 C410 C11' 132.7(13) . . ? N403 C410 C409 110.9(13) . . ? C11' C410 C409 116.1(12) . . ? N403 C410 C11 116.5(11) . . ? C11' C410 C11 16.3(8) . . ? C409 C410 C11 132.4(12) . . ? N405 C421 C404 111.0(10) . . ? N405 C421 H42A 109.4 . . ? C404 C421 H42A 109.4 . . ? N405 C421 H42B 109.4 . . ? C404 C421 H42B 109.4 . . ? H42A C421 H42B 108.0 . . ? N405 C422 C423 109.8(11) . . ? N405 C422 H422 125.1 . . ? C423 C422 H422 125.1 . . ? C422 C423 C424 103.5(12) . . ? C422 C423 H423 128.2 . . ? C424 C423 H423 128.2 . . ? N406 C424 C423 112.7(10) . . ? N406 C424 C425 118.8(9) . . ? C423 C424 C425 128.5(11) . . ? N407 C425 C426 123.6(10) . . ? N407 C425 C424 115.5(9) . . ? C426 C425 C424 120.9(10) . . ? C427 C426 C425 117.9(11) . . ? C427 C426 H426 121.1 . . ? C425 C426 H426 121.1 . . ? C428 C427 C426 120.2(11) . . ? C428 C427 H427 119.9 . . ? C426 C427 H427 119.9 . . ? C427 C428 C429 118.9(11) . . ? C427 C428 H428 120.6 . . ? C429 C428 H428 120.6 . . ? N407 C429 C428 122.0(10) . . ? N407 C429 C430 110.8(9) . . ? C428 C429 C430 126.7(10) . . ? O402 C430 N408 120.9(10) . . ? O402 C430 C429 116.2(9) . . ? N408 C430 C429 122.9(10) . . ? C432 C431 N408 111.1(18) . . ? C432 C431 H43A 109.4 . . ? N408 C431 H43A 109.4 . . ? C432 C431 H43B 109.4 . . ? N408 C431 H43B 109.4 . . ? H43A C431 H43B 108.0 . . ? C431 C432 H43C 109.5 . . ? C431 C432 H43D 109.5 . . ? H43C C432 H43D 109.5 . . ? C431 C432 H43E 109.5 . . ? H43C C432 H43E 109.5 . . ? H43D C432 H43E 109.5 . . ? N408 C433 C434 115.6(13) . . ? N408 C433 H43F 108.4 . . ? C434 C433 H43F 108.4 . . ? N408 C433 H43G 108.4 . . ? C434 C433 H43G 108.4 . . ? H43F C433 H43G 107.4 . . ? C433 C434 H43H 109.5 . . ? C433 C434 H43I 109.5 . . ? H43H C434 H43I 109.5 . . ? C433 C434 H43J 109.5 . . ? H43H C434 H43J 109.5 . . ? H43I C434 H43J 109.5 . . ? C16 O1A Nd4 123.0(12) . . ? C19 N1 C17 113(3) . . ? C19 N1 C16 125(3) . . ? C17 N1 C16 116(3) . . ? C12 C11 N2 120.0 . . ? C12 C11 C410 121.4(10) . . ? N2 C11 C410 118.6(10) . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? N2 C15 C14 120.0 . . ? N2 C15 C16 112.0(11) . . ? C14 C15 C16 127.8(11) . . ? C15 N2 C11 120.0 . . ? C15 N2 Nd4 117.1(6) . . ? C11 N2 Nd4 116.9(7) . . ? O1A C16 C15 119.7(16) . . ? O1A C16 N1 114(2) . . ? C15 C16 N1 124.4(19) . . ? N1 C17 C18 98(3) . . ? N1 C17 H17A 112.2 . . ? C18 C17 H17A 112.2 . . ? N1 C17 H17B 112.2 . . ? C18 C17 H17B 112.2 . . ? H17A C17 H17B 109.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C20 100(3) . . ? N1 C19 H19A 111.9 . . ? C20 C19 H19A 111.8 . . ? N1 C19 H19B 111.8 . . ? C20 C19 H19B 111.8 . . ? H19A C19 H19B 109.6 . . ? C19 C20 H20C 109.5 . . ? C19 C20 H20D 109.5 . . ? H20C C20 H20D 109.5 . . ? C19 C20 H20E 109.5 . . ? H20C C20 H20E 109.5 . . ? H20D C20 H20E 109.5 . . ? C16' O1A' Nd4 128.7(15) . . ? C19' N1' C17' 112(3) . . ? C19' N1' C16' 121(3) . . ? C17' N1' C16' 123(3) . . ? C410 C11' C12' 133.9(11) . . ? C410 C11' N2' 106.0(11) . . ? C12' C11' N2' 120.0 . . ? C13' C12' C11' 120.0 . . ? C13' C12' H12' 120.0 . . ? C11' C12' H12' 120.0 . . ? C14' C13' C12' 120.0 . . ? C14' C13' H13' 120.0 . . ? C12' C13' H13' 120.0 . . ? C13' C14' C15' 120.0 . . ? C13' C14' H14' 120.0 . . ? C15' C14' H14' 120.0 . . ? N2' C15' C14' 120.0 . . ? N2' C15' C16' 111.7(11) . . ? C14' C15' C16' 128.3(12) . . ? C15' N2' C11' 120.0 . . ? C15' N2' Nd4 114.6(6) . . ? C11' N2' Nd4 125.3(6) . . ? O1A' C16' C15' 120.5(17) . . ? O1A' C16' N1' 117.7(19) . . ? C15' C16' N1' 120.4(18) . . ? N1' C17' C18' 97(3) . . ? N1' C17' H17C 112.4 . . ? C18' C17' H17C 112.4 . . ? N1' C17' H17D 112.4 . . ? C18' C17' H17D 112.4 . . ? H17C C17' H17D 109.9 . . ? C17' C18' H18D 109.5 . . ? C17' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C17' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? N1' C19' C20' 103(3) . . ? N1' C19' H19C 111.2 . . ? C20' C19' H19C 111.2 . . ? N1' C19' H19D 111.2 . . ? C20' C19' H19D 111.2 . . ? H19C C19' H19D 109.1 . . ? C19' C20' H20F 109.5 . . ? C19' C20' H20G 109.5 . . ? H20F C20' H20G 109.5 . . ? C19' C20' H20H 109.5 . . ? H20F C20' H20H 109.5 . . ? H20G C20' H20H 109.5 . . ? O3' Cl1 O4 110.4(11) . . ? O3' Cl1 O2 82.3(10) . . ? O4 Cl1 O2 112.8(9) . . ? O3' Cl1 O2' 109.9(9) . . ? O4 Cl1 O2' 82.9(10) . . ? O2 Cl1 O2' 35.0(9) . . ? O3' Cl1 O1 125.9(10) . . ? O4 Cl1 O1 112.4(8) . . ? O2 Cl1 O1 109.2(9) . . ? O2' Cl1 O1 106.8(9) . . ? O3' Cl1 O4' 107.1(8) . . ? O4 Cl1 O4' 25.5(8) . . ? O2 Cl1 O4' 138.2(10) . . ? O2' Cl1 O4' 107.4(9) . . ? O1 Cl1 O4' 98.0(7) . . ? O3' Cl1 O3 28.6(9) . . ? O4 Cl1 O3 109.3(8) . . ? O2 Cl1 O3 108.3(9) . . ? O2' Cl1 O3 138.5(10) . . ? O1 Cl1 O3 104.6(9) . . ? O4' Cl1 O3 94.3(9) . . ? O8' Cl2 O5' 114.6(10) . . ? O8' Cl2 O6 137.1(13) . . ? O5' Cl2 O6 77.6(13) . . ? O8' Cl2 O7 98.2(10) . . ? O5' Cl2 O7 114.4(12) . . ? O6 Cl2 O7 114.3(14) . . ? O8' Cl2 O8 29.9(10) . . ? O5' Cl2 O8 117.1(14) . . ? O6 Cl2 O8 107.2(12) . . ? O7 Cl2 O8 118.7(11) . . ? O8' Cl2 O6' 113.6(10) . . ? O5' Cl2 O6' 113.4(10) . . ? O6 Cl2 O6' 35.9(12) . . ? O7 Cl2 O6' 101.1(13) . . ? O8 Cl2 O6' 87.3(13) . . ? O8' Cl2 O5 92.0(13) . . ? O5' Cl2 O5 27.8(13) . . ? O6 Cl2 O5 105.3(12) . . ? O7 Cl2 O5 104.4(14) . . ? O8 Cl2 O5 105.7(11) . . ? O6' Cl2 O5 140.6(13) . . ? O9 Cl3 O10 116.0(14) . . ? O9 Cl3 O12 109.2(11) . . ? O10 Cl3 O12 109.2(12) . . ? O9 Cl3 O11 104.7(14) . . ? O10 Cl3 O11 101.6(15) . . ? O12 Cl3 O11 116.1(14) . . ? O10' Cl3' O9' 108.2(13) . . ? O10' Cl3' O12' 106.5(12) . . ? O9' Cl3' O12' 109.7(11) . . ? O10' Cl3' O11' 104.3(14) . . ? O9' Cl3' O11' 118.9(15) . . ? O12' Cl3' O11' 108.6(14) . . ? O13 Cl11 O15 110.5(5) . . ? O13 Cl11 O14 108.7(5) . . ? O15 Cl11 O14 108.4(5) . . ? O13 Cl11 O16 108.7(5) . . ? O15 Cl11 O16 110.2(5) . . ? O14 Cl11 O16 110.3(5) . . ? O19 Cl5 O17 112.3(12) . . ? O19 Cl5 O18 109.4(10) . . ? O17 Cl5 O18 112.2(12) . . ? O19 Cl5 O20 107.7(11) . . ? O17 Cl5 O20 121.2(13) . . ? O18 Cl5 O20 92.1(13) . . ? O19' Cl5' O18' 109.5(11) . . ? O19' Cl5' O17' 119.9(12) . . ? O18' Cl5' O17' 112.9(11) . . ? O19' Cl5' O20' 100.3(12) . . ? O18' Cl5' O20' 106.6(14) . . ? O17' Cl5' O20' 106.0(12) . . ? O21 Cl6 O24 111.5(6) . . ? O21 Cl6 O23 109.3(7) . . ? O24 Cl6 O23 109.6(5) . . ? O21 Cl6 O22 109.5(7) . . ? O24 Cl6 O22 107.9(6) . . ? O23 Cl6 O22 109.1(5) . . ? O28 Cl7 O25 110.8(7) . . ? O28 Cl7 O26 111.4(8) . . ? O25 Cl7 O26 109.7(8) . . ? O28 Cl7 O27 111.0(8) . . ? O25 Cl7 O27 106.8(8) . . ? O26 Cl7 O27 106.9(8) . . ? O29 Cl12 O31 110.7(8) . . ? O29 Cl12 O32 108.9(6) . . ? O31 Cl12 O32 111.7(8) . . ? O29 Cl12 O30 108.4(8) . . ? O31 Cl12 O30 107.6(7) . . ? O32 Cl12 O30 109.4(7) . . ? O36 Cl9 O33 133.1(12) . . ? O36 Cl9 O34 105.1(10) . . ? O33 Cl9 O34 104.2(8) . . ? O36 Cl9 O35 106.5(11) . . ? O33 Cl9 O35 97.4(9) . . ? O34 Cl9 O35 109.1(8) . . ? O33' Cl9' O36' 139(3) . . ? O33' Cl9' O35' 98(2) . . ? O36' Cl9' O35' 112(2) . . ? O33' Cl9' O34' 99.5(19) . . ? O36' Cl9' O34' 99(2) . . ? O35' Cl9' O34' 106(2) . . ? O40 Cl10 O37' 150.3(15) . . ? O40 Cl10 O38' 58.9(13) . . ? O37' Cl10 O38' 113.8(11) . . ? O40 Cl10 O39 114.9(9) . . ? O37' Cl10 O39 79.7(14) . . ? O38' Cl10 O39 162.6(14) . . ? O40 Cl10 O39' 99.3(15) . . ? O37' Cl10 O39' 110.0(11) . . ? O38' Cl10 O39' 108.2(11) . . ? O39 Cl10 O39' 55.2(14) . . ? O40 Cl10 O37 111.4(9) . . ? O37' Cl10 O37 39.4(13) . . ? O38' Cl10 O37 89.2(14) . . ? O39 Cl10 O37 108.0(9) . . ? O39' Cl10 O37 149.3(13) . . ? O40 Cl10 O40' 53.4(13) . . ? O37' Cl10 O40' 111.8(11) . . ? O38' Cl10 O40' 107.3(10) . . ? O39 Cl10 O40' 75.5(14) . . ? O39' Cl10 O40' 105.3(10) . . ? O37 Cl10 O40' 92.7(14) . . ? O40 Cl10 O38 109.9(9) . . ? O37' Cl10 O38 88.9(14) . . ? O38' Cl10 O38 65.3(13) . . ? O39 Cl10 O38 105.7(9) . . ? O39' Cl10 O38 61.8(14) . . ? O37 Cl10 O38 106.5(9) . . ? O40' Cl10 O38 159.0(14) . . ? O43 Cl4 O41' 102.2(18) . . ? O43 Cl4 O43' 39.1(11) . . ? O41' Cl4 O43' 112.3(11) . . ? O43 Cl4 O42 113.1(11) . . ? O41' Cl4 O42 131(2) . . ? O43' Cl4 O42 116.4(17) . . ? O43 Cl4 O42' 143.4(16) . . ? O41' Cl4 O42' 110.5(11) . . ? O43' Cl4 O42' 110.3(10) . . ? O42 Cl4 O42' 54.5(16) . . ? O43 Cl4 O41 109.7(10) . . ? O41' Cl4 O41 25(2) . . ? O43' Cl4 O41 132.8(17) . . ? O42 Cl4 O41 108.5(10) . . ? O42' Cl4 O41 106.9(19) . . ? O43 Cl4 O44 108.4(10) . . ? O41' Cl4 O44 90(2) . . ? O43' Cl4 O44 70.8(14) . . ? O42 Cl4 O44 108.6(10) . . ? O42' Cl4 O44 57.2(15) . . ? O41 Cl4 O44 108.3(11) . . ? O43 Cl4 O44' 77.6(14) . . ? O41' Cl4 O44' 109.1(11) . . ? O43' Cl4 O44' 108.8(10) . . ? O42 Cl4 O44' 51.8(16) . . ? O42' Cl4 O44' 105.6(10) . . ? O41 Cl4 O44' 88(2) . . ? O44 Cl4 O44' 158.9(19) . . ? O45 Cl8 O48 108(2) . . ? O45 Cl8 O46 110(2) . . ? O48 Cl8 O46 109(2) . . ? O45 Cl8 O47 121(2) . . ? O48 Cl8 O47 105(2) . . ? O46 Cl8 O47 103(2) . . ? O45' Cl8' O48' 110(2) . . ? O45' Cl8' O47' 127(2) . . ? O48' Cl8' O47' 100(2) . . ? O45' Cl8' O46' 110(2) . . ? O48' Cl8' O46' 111(2) . . ? O47' Cl8' O46' 98.2(19) . . ? N1S C1S C2S 177(2) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N2S C3S C4S 175(2) . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? N3S C5S C6S 163(3) . . ? C5S C6S H6S1 109.5 . . ? C5S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? N4S C7S C8S 168(2) . . ? C7S C8S H8S1 109.5 . . ? C7S C8S H8S2 109.5 . . ? H8S1 C8S H8S2 109.5 . . ? C7S C8S H8S3 109.5 . . ? H8S1 C8S H8S3 109.5 . . ? H8S2 C8S H8S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O402 Nd1 O101 C116 90.8(9) . . . . ? O501 Nd1 O101 C116 -46.9(9) . . . . ? O503 Nd1 O101 C116 164.8(10) . . . . ? N502 Nd1 O101 C116 -120.5(10) . . . . ? N407 Nd1 O101 C116 134.8(9) . . . . ? N102 Nd1 O101 C116 24.1(9) . . . . ? N406 Nd1 O101 C116 -121.1(9) . . . . ? N103 Nd1 O101 C116 19.6(10) . . . . ? O201 Nd2 O102 C130 164.2(6) . . . . ? O504 Nd2 O102 C130 -117.1(6) . . . . ? O506 Nd2 O102 C130 89.1(6) . . . . ? O505 Nd2 O102 C130 107.9(6) . . . . ? N107 Nd2 O102 C130 16.3(6) . . . . ? N202 Nd2 O102 C130 -134.7(6) . . . . ? N106 Nd2 O102 C130 7.7(7) . . . . ? N203 Nd2 O102 C130 -69.9(6) . . . . ? O504 Nd2 O201 C216 -54.5(7) . . . . ? O102 Nd2 O201 C216 81.8(7) . . . . ? O506 Nd2 O201 C216 159.2(7) . . . . ? O505 Nd2 O201 C216 -127.2(7) . . . . ? N107 Nd2 O201 C216 126.3(7) . . . . ? N202 Nd2 O201 C216 16.7(7) . . . . ? N106 Nd2 O201 C216 -130.5(7) . . . . ? N203 Nd2 O201 C216 11.0(8) . . . . ? O301 Nd3 O202 C230 170.3(7) . . . . ? O507 Nd3 O202 C230 -115.6(7) . . . . ? O509 Nd3 O202 C230 93.6(7) . . . . ? O508 Nd3 O202 C230 116.0(7) . . . . ? N207 Nd3 O202 C230 19.3(7) . . . . ? N302 Nd3 O202 C230 -127.1(7) . . . . ? N303 Nd3 O202 C230 -63.1(7) . . . . ? N206 Nd3 O202 C230 14.8(8) . . . . ? O202 Nd3 O301 C316 78.4(8) . . . . ? O507 Nd3 O301 C316 -62.1(8) . . . . ? O509 Nd3 O301 C316 154.4(9) . . . . ? O508 Nd3 O301 C316 -132.8(9) . . . . ? N207 Nd3 O301 C316 117.0(8) . . . . ? N302 Nd3 O301 C316 11.6(8) . . . . ? N303 Nd3 O301 C316 6.0(9) . . . . ? N206 Nd3 O301 C316 -137.5(8) . . . . ? O1A' Nd4 O302 C330 155.2(10) . . . . ? O1A Nd4 O302 C330 149.6(9) . . . . ? O510 Nd4 O302 C330 -127.5(8) . . . . ? O512 Nd4 O302 C330 77.3(9) . . . . ? N2 Nd4 O302 C330 -148.4(9) . . . . ? O511 Nd4 O302 C330 102.6(10) . . . . ? N307 Nd4 O302 C330 7.4(8) . . . . ? N403 Nd4 O302 C330 -81.9(9) . . . . ? N306 Nd4 O302 C330 -0.9(10) . . . . ? N2' Nd4 O302 C330 -141.0(10) . . . . ? O101 Nd1 O402 C430 158.4(9) . . . . ? O501 Nd1 O402 C430 -123.1(9) . . . . ? O503 Nd1 O402 C430 83.2(9) . . . . ? N502 Nd1 O402 C430 103.9(10) . . . . ? N407 Nd1 O402 C430 10.0(8) . . . . ? N102 Nd1 O402 C430 -140.8(9) . . . . ? N406 Nd1 O402 C430 1.4(10) . . . . ? N103 Nd1 O402 C430 -77.1(9) . . . . ? O402 Nd1 N502 C501 51(4) . . . . ? O101 Nd1 N502 C501 -8(4) . . . . ? O501 Nd1 N502 C501 -97(4) . . . . ? O503 Nd1 N502 C501 72(4) . . . . ? N407 Nd1 N502 C501 127(4) . . . . ? N102 Nd1 N502 C501 -46(4) . . . . ? N406 Nd1 N502 C501 171(4) . . . . ? N103 Nd1 N502 C501 -127(4) . . . . ? Nd1 N502 C501 C502 -24(27) . . . . ? O402 Nd1 N102 C115 -102.1(8) . . . . ? O101 Nd1 N102 C115 -1.9(7) . . . . ? O501 Nd1 N102 C115 90.6(8) . . . . ? O503 Nd1 N102 C115 -49.1(8) . . . . ? N502 Nd1 N102 C115 38.1(9) . . . . ? N407 Nd1 N102 C115 -133.4(7) . . . . ? N406 Nd1 N102 C115 140.4(7) . . . . ? N103 Nd1 N102 C115 173.7(8) . . . . ? O402 Nd1 N102 C111 61.1(8) . . . . ? O101 Nd1 N102 C111 161.3(8) . . . . ? O501 Nd1 N102 C111 -106.2(8) . . . . ? O503 Nd1 N102 C111 114.2(8) . . . . ? N502 Nd1 N102 C111 -158.7(8) . . . . ? N407 Nd1 N102 C111 29.8(8) . . . . ? N406 Nd1 N102 C111 -56.4(10) . . . . ? N103 Nd1 N102 C111 -23.1(7) . . . . ? O402 Nd1 N103 N104 109.9(9) . . . . ? O101 Nd1 N103 N104 -171.5(8) . . . . ? O501 Nd1 N103 N104 -100.7(9) . . . . ? O503 Nd1 N103 N104 76.8(10) . . . . ? N502 Nd1 N103 N104 -71.0(11) . . . . ? N407 Nd1 N103 N104 46.2(9) . . . . ? N102 Nd1 N103 N104 -176.1(10) . . . . ? N406 Nd1 N103 N104 -14.7(9) . . . . ? O402 Nd1 N103 C110 -53.9(7) . . . . ? O101 Nd1 N103 C110 24.6(8) . . . . ? O501 Nd1 N103 C110 95.4(7) . . . . ? O503 Nd1 N103 C110 -87.1(8) . . . . ? N502 Nd1 N103 C110 125.1(8) . . . . ? N407 Nd1 N103 C110 -117.7(7) . . . . ? N102 Nd1 N103 C110 20.0(6) . . . . ? N406 Nd1 N103 C110 -178.6(7) . . . . ? C110 N103 N104 C108 0.5(11) . . . . ? Nd1 N103 N104 C108 -164.7(8) . . . . ? C110 N103 N104 C107 -178.2(8) . . . . ? Nd1 N103 N104 C107 16.6(14) . . . . ? C122 N105 N106 C124 -1.2(10) . . . . ? C121 N105 N106 C124 -172.0(8) . . . . ? C122 N105 N106 Nd2 -146.7(7) . . . . ? C121 N105 N106 Nd2 42.6(11) . . . . ? O201 Nd2 N106 C124 -105.2(6) . . . . ? O504 Nd2 N106 C124 -179.9(6) . . . . ? O102 Nd2 N106 C124 35.2(6) . . . . ? O506 Nd2 N106 C124 -39.7(6) . . . . ? O505 Nd2 N106 C124 -108.5(6) . . . . ? N107 Nd2 N106 C124 26.5(5) . . . . ? N202 Nd2 N106 C124 132.9(6) . . . . ? N203 Nd2 N106 C124 105.9(6) . . . . ? O201 Nd2 N106 N105 38.1(8) . . . . ? O504 Nd2 N106 N105 -36.6(7) . . . . ? O102 Nd2 N106 N105 178.5(6) . . . . ? O506 Nd2 N106 N105 103.6(7) . . . . ? O505 Nd2 N106 N105 34.7(7) . . . . ? N107 Nd2 N106 N105 169.8(7) . . . . ? N202 Nd2 N106 N105 -83.8(8) . . . . ? N203 Nd2 N106 N105 -110.8(7) . . . . ? O201 Nd2 N107 C129 -46.0(7) . . . . ? O504 Nd2 N107 C129 135.2(5) . . . . ? O102 Nd2 N107 C129 6.2(5) . . . . ? O506 Nd2 N107 C129 -80.2(6) . . . . ? O505 Nd2 N107 C129 -136.3(5) . . . . ? N202 Nd2 N107 C129 38.2(6) . . . . ? N106 Nd2 N107 C129 178.0(6) . . . . ? N203 Nd2 N107 C129 84.4(6) . . . . ? O201 Nd2 N107 C125 107.7(6) . . . . ? O504 Nd2 N107 C125 -71.1(6) . . . . ? O102 Nd2 N107 C125 160.0(6) . . . . ? O506 Nd2 N107 C125 73.5(6) . . . . ? O505 Nd2 N107 C125 17.4(6) . . . . ? N202 Nd2 N107 C125 -168.1(5) . . . . ? N106 Nd2 N107 C125 -28.3(5) . . . . ? N203 Nd2 N107 C125 -121.9(6) . . . . ? O201 Nd2 N202 C211 165.2(7) . . . . ? O504 Nd2 N202 C211 -102.6(6) . . . . ? O102 Nd2 N202 C211 64.4(6) . . . . ? O506 Nd2 N202 C211 119.6(6) . . . . ? O505 Nd2 N202 C211 -152.2(6) . . . . ? N107 Nd2 N202 C211 33.8(7) . . . . ? N106 Nd2 N202 C211 -51.4(8) . . . . ? N203 Nd2 N202 C211 -20.2(6) . . . . ? O201 Nd2 N202 C215 3.3(5) . . . . ? O504 Nd2 N202 C215 95.6(6) . . . . ? O102 Nd2 N202 C215 -97.4(6) . . . . ? O506 Nd2 N202 C215 -42.2(6) . . . . ? O505 Nd2 N202 C215 46.0(6) . . . . ? N107 Nd2 N202 C215 -128.0(5) . . . . ? N106 Nd2 N202 C215 146.8(5) . . . . ? N203 Nd2 N202 C215 178.0(6) . . . . ? O201 Nd2 N203 C210 19.6(7) . . . . ? O504 Nd2 N203 C210 89.4(6) . . . . ? O102 Nd2 N203 C210 -58.3(6) . . . . ? O506 Nd2 N203 C210 -96.3(7) . . . . ? O505 Nd2 N203 C210 123.5(6) . . . . ? N107 Nd2 N203 C210 -122.3(6) . . . . ? N202 Nd2 N203 C210 13.8(6) . . . . ? N106 Nd2 N203 C210 176.8(6) . . . . ? O201 Nd2 N203 N204 -166.9(7) . . . . ? O504 Nd2 N203 N204 -97.1(8) . . . . ? O102 Nd2 N203 N204 115.1(8) . . . . ? O506 Nd2 N203 N204 77.1(9) . . . . ? O505 Nd2 N203 N204 -63.0(9) . . . . ? N107 Nd2 N203 N204 51.2(8) . . . . ? N202 Nd2 N203 N204 -172.7(8) . . . . ? N106 Nd2 N203 N204 -9.8(8) . . . . ? C210 N203 N204 C208 1.1(9) . . . . ? Nd2 N203 N204 C208 -172.9(6) . . . . ? C210 N203 N204 C207 -177.8(8) . . . . ? Nd2 N203 N204 C207 8.2(12) . . . . ? C222 N205 N206 C224 -1.1(10) . . . . ? C221 N205 N206 C224 -171.8(8) . . . . ? C222 N205 N206 Nd3 -143.7(7) . . . . ? C221 N205 N206 Nd3 45.7(11) . . . . ? O301 Nd3 N206 N205 36.4(9) . . . . ? O202 Nd3 N206 N205 171.6(6) . . . . ? O507 Nd3 N206 N205 -38.6(7) . . . . ? O509 Nd3 N206 N205 100.5(7) . . . . ? O508 Nd3 N206 N205 31.7(7) . . . . ? N207 Nd3 N206 N205 167.1(8) . . . . ? N302 Nd3 N206 N205 -90.7(8) . . . . ? N303 Nd3 N206 N205 -114.0(7) . . . . ? O301 Nd3 N206 C224 -103.6(7) . . . . ? O202 Nd3 N206 C224 31.6(7) . . . . ? O507 Nd3 N206 C224 -178.6(6) . . . . ? O509 Nd3 N206 C224 -39.6(6) . . . . ? O508 Nd3 N206 C224 -108.4(6) . . . . ? N207 Nd3 N206 C224 27.0(6) . . . . ? N302 Nd3 N206 C224 129.3(6) . . . . ? N303 Nd3 N206 C224 106.0(6) . . . . ? O301 Nd3 N207 C225 113.1(6) . . . . ? O202 Nd3 N207 C225 157.2(7) . . . . ? O507 Nd3 N207 C225 -68.3(7) . . . . ? O509 Nd3 N207 C225 74.2(6) . . . . ? O508 Nd3 N207 C225 19.6(7) . . . . ? N302 Nd3 N207 C225 -167.0(6) . . . . ? N303 Nd3 N207 C225 -118.9(6) . . . . ? N206 Nd3 N207 C225 -27.1(6) . . . . ? O301 Nd3 N207 C229 -43.1(8) . . . . ? O202 Nd3 N207 C229 1.0(6) . . . . ? O507 Nd3 N207 C229 135.5(6) . . . . ? O509 Nd3 N207 C229 -81.9(6) . . . . ? O508 Nd3 N207 C229 -136.6(6) . . . . ? N302 Nd3 N207 C229 36.9(7) . . . . ? N303 Nd3 N207 C229 84.9(6) . . . . ? N206 Nd3 N207 C229 176.7(7) . . . . ? O301 Nd3 N302 C315 5.3(6) . . . . ? O202 Nd3 N302 C315 -89.7(6) . . . . ? O507 Nd3 N302 C315 98.2(6) . . . . ? O509 Nd3 N302 C315 -40.0(7) . . . . ? O508 Nd3 N302 C315 48.4(7) . . . . ? N207 Nd3 N302 C315 -124.4(6) . . . . ? N303 Nd3 N302 C315 -179.9(6) . . . . ? N206 Nd3 N302 C315 153.6(5) . . . . ? O301 Nd3 N302 C311 165.3(7) . . . . ? O202 Nd3 N302 C311 70.2(6) . . . . ? O507 Nd3 N302 C311 -101.9(6) . . . . ? O509 Nd3 N302 C311 120.0(6) . . . . ? O508 Nd3 N302 C311 -151.7(6) . . . . ? N207 Nd3 N302 C311 35.6(7) . . . . ? N303 Nd3 N302 C311 -20.0(6) . . . . ? N206 Nd3 N302 C311 -46.4(8) . . . . ? O301 Nd3 N303 N304 -166.3(7) . . . . ? O202 Nd3 N303 N304 119.2(8) . . . . ? O507 Nd3 N303 N304 -93.6(8) . . . . ? O509 Nd3 N303 N304 76.8(9) . . . . ? O508 Nd3 N303 N304 -60.0(9) . . . . ? N207 Nd3 N303 N304 54.9(8) . . . . ? N302 Nd3 N303 N304 -171.9(8) . . . . ? N206 Nd3 N303 N304 -6.7(8) . . . . ? O301 Nd3 N303 C310 20.8(7) . . . . ? O202 Nd3 N303 C310 -53.7(6) . . . . ? O507 Nd3 N303 C310 93.6(6) . . . . ? O509 Nd3 N303 C310 -96.1(7) . . . . ? O508 Nd3 N303 C310 127.1(6) . . . . ? N207 Nd3 N303 C310 -118.0(6) . . . . ? N302 Nd3 N303 C310 15.2(6) . . . . ? N206 Nd3 N303 C310 -179.6(6) . . . . ? C310 N303 N304 C308 0.9(10) . . . . ? Nd3 N303 N304 C308 -172.5(6) . . . . ? C310 N303 N304 C307 -178.2(7) . . . . ? Nd3 N303 N304 C307 8.3(12) . . . . ? C322 N305 N306 C324 -0.1(11) . . . . ? C321 N305 N306 C324 -174.4(9) . . . . ? C322 N305 N306 Nd4 -152.1(8) . . . . ? C321 N305 N306 Nd4 33.6(13) . . . . ? O1A' Nd4 N306 C324 -97.0(10) . . . . ? O302 Nd4 N306 C324 28.4(7) . . . . ? O1A Nd4 N306 C324 -105.4(7) . . . . ? O510 Nd4 N306 C324 176.2(6) . . . . ? O512 Nd4 N306 C324 -45.7(6) . . . . ? N2 Nd4 N306 C324 137.4(8) . . . . ? O511 Nd4 N306 C324 -114.1(6) . . . . ? N307 Nd4 N306 C324 20.1(6) . . . . ? N403 Nd4 N306 C324 105.8(6) . . . . ? N2' Nd4 N306 C324 114.5(8) . . . . ? O1A' Nd4 N306 N305 53.1(12) . . . . ? O302 Nd4 N306 N305 178.5(7) . . . . ? O1A Nd4 N306 N305 44.7(10) . . . . ? O510 Nd4 N306 N305 -33.7(8) . . . . ? O512 Nd4 N306 N305 104.4(8) . . . . ? N2 Nd4 N306 N305 -72.5(10) . . . . ? O511 Nd4 N306 N305 36.0(8) . . . . ? N307 Nd4 N306 N305 170.2(8) . . . . ? N403 Nd4 N306 N305 -104.1(8) . . . . ? N2' Nd4 N306 N305 -95.4(10) . . . . ? O1A' Nd4 N307 C325 125.6(7) . . . . ? O302 Nd4 N307 C325 165.9(7) . . . . ? O1A Nd4 N307 C325 107.8(8) . . . . ? O510 Nd4 N307 C325 -61.3(8) . . . . ? O512 Nd4 N307 C325 76.5(6) . . . . ? N2 Nd4 N307 C325 -164.7(6) . . . . ? O511 Nd4 N307 C325 26.7(7) . . . . ? N403 Nd4 N307 C325 -111.8(6) . . . . ? N306 Nd4 N307 C325 -21.9(6) . . . . ? N2' Nd4 N307 C325 -163.7(6) . . . . ? O1A' Nd4 N307 C329 -31.6(8) . . . . ? O302 Nd4 N307 C329 8.8(6) . . . . ? O1A Nd4 N307 C329 -49.4(9) . . . . ? O510 Nd4 N307 C329 141.6(7) . . . . ? O512 Nd4 N307 C329 -80.6(6) . . . . ? N2 Nd4 N307 C329 38.2(8) . . . . ? O511 Nd4 N307 C329 -130.4(6) . . . . ? N403 Nd4 N307 C329 91.0(6) . . . . ? N306 Nd4 N307 C329 -179.1(7) . . . . ? N2' Nd4 N307 C329 39.1(7) . . . . ? O1A' Nd4 N403 C410 8.4(11) . . . . ? O302 Nd4 N403 C410 -59.7(9) . . . . ? O1A Nd4 N403 C410 22.7(11) . . . . ? O510 Nd4 N403 C410 90.1(9) . . . . ? O512 Nd4 N403 C410 -105.6(10) . . . . ? N2 Nd4 N403 C410 14.3(9) . . . . ? O511 Nd4 N403 C410 116.5(9) . . . . ? N307 Nd4 N403 C410 -121.6(9) . . . . ? N306 Nd4 N403 C410 176.1(9) . . . . ? N2' Nd4 N403 C410 1.8(9) . . . . ? O1A' Nd4 N403 N404 -174.1(11) . . . . ? O302 Nd4 N403 N404 117.8(11) . . . . ? O1A Nd4 N403 N404 -159.8(11) . . . . ? O510 Nd4 N403 N404 -92.4(11) . . . . ? O512 Nd4 N403 N404 71.9(13) . . . . ? N2 Nd4 N403 N404 -168.2(12) . . . . ? O511 Nd4 N403 N404 -65.9(13) . . . . ? N307 Nd4 N403 N404 56.0(11) . . . . ? N306 Nd4 N403 N404 -6.4(11) . . . . ? N2' Nd4 N403 N404 179.4(13) . . . . ? C410 N403 N404 C408 -0.7(16) . . . . ? Nd4 N403 N404 C408 -178.4(11) . . . . ? C410 N403 N404 C407 175.9(12) . . . . ? Nd4 N403 N404 C407 -1.8(19) . . . . ? C422 N405 N406 C424 0.3(14) . . . . ? C421 N405 N406 C424 -171.9(11) . . . . ? C422 N405 N406 Nd1 -149.7(10) . . . . ? C421 N405 N406 Nd1 38.1(16) . . . . ? O402 Nd1 N406 C424 31.6(9) . . . . ? O101 Nd1 N406 C424 -109.4(8) . . . . ? O501 Nd1 N406 C424 177.4(8) . . . . ? O503 Nd1 N406 C424 -40.8(8) . . . . ? N502 Nd1 N406 C424 -110.0(8) . . . . ? N407 Nd1 N406 C424 23.0(7) . . . . ? N102 Nd1 N406 C424 131.3(8) . . . . ? N103 Nd1 N406 C424 102.8(8) . . . . ? O402 Nd1 N406 N405 178.7(9) . . . . ? O101 Nd1 N406 N405 37.8(12) . . . . ? O501 Nd1 N406 N405 -35.5(10) . . . . ? O503 Nd1 N406 N405 106.3(10) . . . . ? N502 Nd1 N406 N405 37.1(10) . . . . ? N407 Nd1 N406 N405 170.1(11) . . . . ? N102 Nd1 N406 N405 -81.5(11) . . . . ? N103 Nd1 N406 N405 -110.1(10) . . . . ? O402 Nd1 N407 C425 163.6(8) . . . . ? O101 Nd1 N407 C425 111.9(7) . . . . ? O501 Nd1 N407 C425 -65.5(9) . . . . ? O503 Nd1 N407 C425 80.4(7) . . . . ? N502 Nd1 N407 C425 24.6(8) . . . . ? N102 Nd1 N407 C425 -163.3(7) . . . . ? N406 Nd1 N407 C425 -24.6(7) . . . . ? N103 Nd1 N407 C425 -118.6(7) . . . . ? O402 Nd1 N407 C429 7.7(7) . . . . ? O101 Nd1 N407 C429 -44.0(8) . . . . ? O501 Nd1 N407 C429 138.6(7) . . . . ? O503 Nd1 N407 C429 -75.4(7) . . . . ? N502 Nd1 N407 C429 -131.3(7) . . . . ? N102 Nd1 N407 C429 40.8(8) . . . . ? N406 Nd1 N407 C429 179.5(8) . . . . ? N103 Nd1 N407 C429 85.5(7) . . . . ? C106 C101 C102 C103 3.0(15) . . . . ? C107 C101 C102 C103 -177.6(10) . . . . ? C101 C102 C103 C104 -1.9(16) . . . . ? C102 C103 C104 C105 0.3(14) . . . . ? C102 C103 C104 C121 176.3(9) . . . . ? C103 C104 C105 C106 0.0(14) . . . . ? C121 C104 C105 C106 -176.0(8) . . . . ? C104 C105 C106 C101 1.2(14) . . . . ? C102 C101 C106 C105 -2.7(14) . . . . ? C107 C101 C106 C105 178.0(9) . . . . ? C108 N104 C107 C101 82.5(13) . . . . ? N103 N104 C107 C101 -99.0(10) . . . . ? C102 C101 C107 N104 174.9(9) . . . . ? C106 C101 C107 N104 -5.8(14) . . . . ? N103 N104 C108 C109 0.4(13) . . . . ? C107 N104 C108 C109 179.0(9) . . . . ? N104 C108 C109 C110 -1.2(13) . . . . ? N104 N103 C110 C109 -1.3(11) . . . . ? Nd1 N103 C110 C109 167.9(7) . . . . ? N104 N103 C110 C111 173.0(8) . . . . ? Nd1 N103 C110 C111 -17.8(11) . . . . ? C108 C109 C110 N103 1.6(13) . . . . ? C108 C109 C110 C111 -171.9(11) . . . . ? C115 N102 C111 C112 6.4(15) . . . . ? Nd1 N102 C111 C112 -156.6(8) . . . . ? C115 N102 C111 C110 -173.1(9) . . . . ? Nd1 N102 C111 C110 24.0(12) . . . . ? N103 C110 C111 N102 -2.8(14) . . . . ? C109 C110 C111 N102 170.4(11) . . . . ? N103 C110 C111 C112 177.8(10) . . . . ? C109 C110 C111 C112 -9.1(18) . . . . ? N102 C111 C112 C113 -3.8(17) . . . . ? C110 C111 C112 C113 175.6(10) . . . . ? C111 C112 C113 C114 -0.1(17) . . . . ? C112 C113 C114 C115 1.3(18) . . . . ? C111 N102 C115 C114 -5.1(16) . . . . ? Nd1 N102 C115 C114 158.6(9) . . . . ? C111 N102 C115 C116 -178.9(9) . . . . ? Nd1 N102 C115 C116 -15.3(11) . . . . ? C113 C114 C115 N102 1.3(18) . . . . ? C113 C114 C115 C116 174.2(11) . . . . ? Nd1 O101 C116 N101 138.1(9) . . . . ? Nd1 O101 C116 C115 -42.7(13) . . . . ? C117 N101 C116 O101 -163.3(11) . . . . ? C119 N101 C116 O101 3.6(16) . . . . ? C117 N101 C116 C115 17.6(17) . . . . ? C119 N101 C116 C115 -175.5(10) . . . . ? N102 C115 C116 O101 37.0(13) . . . . ? C114 C115 C116 O101 -136.6(12) . . . . ? N102 C115 C116 N101 -143.8(10) . . . . ? C114 C115 C116 N101 42.6(17) . . . . ? C116 N101 C117 C118 -124.7(13) . . . . ? C119 N101 C117 C118 68.3(15) . . . . ? C116 N101 C119 C120 80.7(14) . . . . ? C117 N101 C119 C120 -111.0(13) . . . . ? C122 N105 C121 C104 -90.9(11) . . . . ? N106 N105 C121 C104 78.7(10) . . . . ? C105 C104 C121 N105 -127.7(8) . . . . ? C103 C104 C121 N105 56.3(11) . . . . ? N106 N105 C122 C123 1.1(11) . . . . ? C121 N105 C122 C123 171.4(8) . . . . ? N105 C122 C123 C124 -0.4(11) . . . . ? N105 N106 C124 C123 0.9(10) . . . . ? Nd2 N106 C124 C123 154.5(6) . . . . ? N105 N106 C124 C125 -179.3(7) . . . . ? Nd2 N106 C124 C125 -25.8(10) . . . . ? C122 C123 C124 N106 -0.3(11) . . . . ? C122 C123 C124 C125 180.0(9) . . . . ? C129 N107 C125 C126 0.8(12) . . . . ? Nd2 N107 C125 C126 -152.9(7) . . . . ? C129 N107 C125 C124 -178.9(7) . . . . ? Nd2 N107 C125 C124 27.4(9) . . . . ? N106 C124 C125 N107 0.4(12) . . . . ? C123 C124 C125 N107 -179.9(9) . . . . ? N106 C124 C125 C126 -179.3(8) . . . . ? C123 C124 C125 C126 0.4(15) . . . . ? N107 C125 C126 C127 1.9(13) . . . . ? C124 C125 C126 C127 -178.5(9) . . . . ? C125 C126 C127 C128 -3.2(14) . . . . ? C126 C127 C128 C129 2.0(13) . . . . ? C125 N107 C129 C128 -2.1(12) . . . . ? Nd2 N107 C129 C128 151.7(7) . . . . ? C125 N107 C129 C130 -177.2(7) . . . . ? Nd2 N107 C129 C130 -23.3(8) . . . . ? C127 C128 C129 N107 0.8(13) . . . . ? C127 C128 C129 C130 175.2(8) . . . . ? Nd2 O102 C130 N108 144.9(6) . . . . ? Nd2 O102 C130 C129 -35.0(9) . . . . ? C133 N108 C130 O102 -172.2(8) . . . . ? C131 N108 C130 O102 3.9(13) . . . . ? C133 N108 C130 C129 7.7(12) . . . . ? C131 N108 C130 C129 -176.1(8) . . . . ? N107 C129 C130 O102 37.5(10) . . . . ? C128 C129 C130 O102 -137.5(8) . . . . ? N107 C129 C130 N108 -142.5(8) . . . . ? C128 C129 C130 N108 42.6(12) . . . . ? C130 N108 C131 C132 -127.3(9) . . . . ? C133 N108 C131 C132 49.2(11) . . . . ? C130 N108 C133 C134 -116.9(10) . . . . ? C131 N108 C133 C134 66.9(11) . . . . ? C206 C201 C202 C203 1.1(13) . . . . ? C207 C201 C202 C203 -177.6(8) . . . . ? C201 C202 C203 C204 0.2(14) . . . . ? C202 C203 C204 C205 -1.5(13) . . . . ? C202 C203 C204 C221 175.7(8) . . . . ? C203 C204 C205 C206 1.6(13) . . . . ? C221 C204 C205 C206 -175.6(8) . . . . ? C204 C205 C206 C201 -0.3(13) . . . . ? C202 C201 C206 C205 -1.1(12) . . . . ? C207 C201 C206 C205 177.6(8) . . . . ? C208 N204 C207 C201 86.1(11) . . . . ? N203 N204 C207 C201 -95.2(9) . . . . ? C206 C201 C207 N204 -11.7(12) . . . . ? C202 C201 C207 N204 167.0(8) . . . . ? N203 N204 C208 C209 -0.1(11) . . . . ? C207 N204 C208 C209 178.6(9) . . . . ? N204 C208 C209 C210 -0.8(11) . . . . ? N204 N203 C210 C209 -1.6(10) . . . . ? Nd2 N203 C210 C209 174.0(6) . . . . ? N204 N203 C210 C211 175.9(7) . . . . ? Nd2 N203 C210 C211 -8.5(10) . . . . ? C208 C209 C210 N203 1.5(11) . . . . ? C208 C209 C210 C211 -175.7(9) . . . . ? C215 N202 C211 C212 6.2(13) . . . . ? Nd2 N202 C211 C212 -155.2(7) . . . . ? C215 N202 C211 C210 -174.2(7) . . . . ? Nd2 N202 C211 C210 24.4(10) . . . . ? N203 C210 C211 N202 -9.7(12) . . . . ? C209 C210 C211 N202 167.3(9) . . . . ? N203 C210 C211 C212 169.9(9) . . . . ? C209 C210 C211 C212 -13.1(15) . . . . ? N202 C211 C212 C213 -1.6(15) . . . . ? C210 C211 C212 C213 178.8(9) . . . . ? C211 C212 C213 C214 -2.7(16) . . . . ? C212 C213 C214 C215 2.3(15) . . . . ? C211 N202 C215 C214 -6.6(12) . . . . ? Nd2 N202 C215 C214 155.5(7) . . . . ? C211 N202 C215 C216 -179.9(7) . . . . ? Nd2 N202 C215 C216 -17.7(8) . . . . ? C213 C214 C215 N202 2.4(14) . . . . ? C213 C214 C215 C216 174.4(9) . . . . ? Nd2 O201 C216 N201 146.6(7) . . . . ? Nd2 O201 C216 C215 -33.0(10) . . . . ? C217 N201 C216 O201 -173.5(10) . . . . ? C219 N201 C216 O201 1.2(13) . . . . ? C217 N201 C216 C215 6.0(15) . . . . ? C219 N201 C216 C215 -179.2(8) . . . . ? N202 C215 C216 O201 31.9(10) . . . . ? C214 C215 C216 O201 -140.9(9) . . . . ? N202 C215 C216 N201 -147.7(8) . . . . ? C214 C215 C216 N201 39.5(14) . . . . ? C216 N201 C217 C218 -114.9(13) . . . . ? C219 N201 C217 C218 70.3(14) . . . . ? C216 N201 C219 C220 78.9(12) . . . . ? C217 N201 C219 C220 -105.8(12) . . . . ? C222 N205 C221 C204 -86.7(12) . . . . ? N206 N205 C221 C204 82.1(10) . . . . ? C205 C204 C221 N205 -127.9(9) . . . . ? C203 C204 C221 N205 54.9(11) . . . . ? N206 N205 C222 C223 0.8(12) . . . . ? C221 N205 C222 C223 170.6(9) . . . . ? N205 C222 C223 C224 -0.2(13) . . . . ? C222 C223 C224 N206 -0.5(12) . . . . ? C222 C223 C224 C225 179.1(10) . . . . ? N205 N206 C224 C223 1.0(10) . . . . ? Nd3 N206 C224 C223 152.3(7) . . . . ? N205 N206 C224 C225 -178.7(8) . . . . ? Nd3 N206 C224 C225 -27.4(10) . . . . ? C229 N207 C225 C226 -0.5(13) . . . . ? Nd3 N207 C225 C226 -156.2(7) . . . . ? C229 N207 C225 C224 -179.3(8) . . . . ? Nd3 N207 C225 C224 25.0(10) . . . . ? C223 C224 C225 N207 -176.5(10) . . . . ? N206 C224 C225 N207 3.2(12) . . . . ? C223 C224 C225 C226 4.8(16) . . . . ? N206 C224 C225 C226 -175.6(9) . . . . ? N207 C225 C226 C227 2.8(16) . . . . ? C224 C225 C226 C227 -178.5(10) . . . . ? C225 C226 C227 C228 -2.4(18) . . . . ? C226 C227 C228 C229 -0.1(17) . . . . ? C225 N207 C229 C228 -2.1(14) . . . . ? Nd3 N207 C229 C228 153.9(8) . . . . ? C225 N207 C229 C230 -172.6(8) . . . . ? Nd3 N207 C229 C230 -16.6(10) . . . . ? C227 C228 C229 N207 2.4(15) . . . . ? C227 C228 C229 C230 171.7(10) . . . . ? Nd3 O202 C230 N208 146.8(7) . . . . ? Nd3 O202 C230 C229 -35.7(10) . . . . ? C233 N208 C230 O202 -164.1(10) . . . . ? C231 N208 C230 O202 9.9(14) . . . . ? C233 N208 C230 C229 18.5(15) . . . . ? C231 N208 C230 C229 -167.4(9) . . . . ? N207 C229 C230 O202 33.4(12) . . . . ? C228 C229 C230 O202 -136.8(10) . . . . ? N207 C229 C230 N208 -149.1(9) . . . . ? C228 C229 C230 N208 40.8(15) . . . . ? C230 N208 C231 C232 117.9(11) . . . . ? C233 N208 C231 C232 -67.7(13) . . . . ? C230 N208 C233 C234 117.4(12) . . . . ? C231 N208 C233 C234 -56.8(13) . . . . ? C306 C301 C302 C303 2.5(14) . . . . ? C307 C301 C302 C303 -177.0(9) . . . . ? C301 C302 C303 C304 -0.7(15) . . . . ? C302 C303 C304 C305 -1.9(14) . . . . ? C302 C303 C304 C321 175.5(9) . . . . ? C303 C304 C305 C306 2.7(14) . . . . ? C321 C304 C305 C306 -174.8(9) . . . . ? C304 C305 C306 C301 -0.8(14) . . . . ? C302 C301 C306 C305 -1.8(13) . . . . ? C307 C301 C306 C305 177.7(8) . . . . ? N303 N304 C307 C301 -95.3(9) . . . . ? C308 N304 C307 C301 85.6(11) . . . . ? C306 C301 C307 N304 -6.1(12) . . . . ? C302 C301 C307 N304 173.4(8) . . . . ? N303 N304 C308 C309 -0.7(11) . . . . ? C307 N304 C308 C309 178.4(8) . . . . ? N304 C308 C309 C310 0.1(11) . . . . ? N304 N303 C310 C309 -0.8(10) . . . . ? Nd3 N303 C310 C309 174.4(6) . . . . ? N304 N303 C310 C311 173.6(7) . . . . ? Nd3 N303 C310 C311 -11.2(10) . . . . ? C308 C309 C310 N303 0.4(11) . . . . ? C308 C309 C310 C311 -173.4(9) . . . . ? C315 N302 C311 C312 2.2(12) . . . . ? Nd3 N302 C311 C312 -157.4(6) . . . . ? C315 N302 C311 C310 -177.5(7) . . . . ? Nd3 N302 C311 C310 22.9(10) . . . . ? N303 C310 C311 N302 -7.2(12) . . . . ? C309 C310 C311 N302 166.2(9) . . . . ? N303 C310 C311 C312 173.1(8) . . . . ? C309 C310 C311 C312 -13.5(15) . . . . ? N302 C311 C312 C313 -1.2(13) . . . . ? C310 C311 C312 C313 178.5(8) . . . . ? C311 C312 C313 C314 -0.1(14) . . . . ? C312 C313 C314 C315 0.4(14) . . . . ? C311 N302 C315 C314 -1.9(13) . . . . ? Nd3 N302 C315 C314 158.1(7) . . . . ? C311 N302 C315 C316 -177.1(7) . . . . ? Nd3 N302 C315 C316 -17.0(9) . . . . ? C313 C314 C315 N302 0.6(14) . . . . ? C313 C314 C315 C316 175.0(9) . . . . ? Nd3 O301 C316 N301 156.4(8) . . . . ? Nd3 O301 C316 C315 -25.1(13) . . . . ? C319 N301 C316 O301 -168.5(10) . . . . ? C317 N301 C316 O301 7.0(16) . . . . ? C319 N301 C316 C315 13.1(17) . . . . ? C317 N301 C316 C315 -171.3(10) . . . . ? N302 C315 C316 O301 26.5(12) . . . . ? C314 C315 C316 O301 -148.5(10) . . . . ? N302 C315 C316 N301 -155.2(10) . . . . ? C314 C315 C316 N301 29.9(15) . . . . ? C316 N301 C317 C318 -87.9(15) . . . . ? C319 N301 C317 C318 88.2(15) . . . . ? C316 N301 C319 C320 -110.0(13) . . . . ? C317 N301 C319 C320 74.4(13) . . . . ? C322 N305 C321 C304 -85.2(14) . . . . ? N306 N305 C321 C304 88.2(11) . . . . ? C303 C304 C321 N305 42.6(13) . . . . ? C305 C304 C321 N305 -140.0(9) . . . . ? N306 N305 C322 C323 -0.5(14) . . . . ? C321 N305 C322 C323 173.3(11) . . . . ? N305 C322 C323 C324 0.8(14) . . . . ? N305 N306 C324 C323 0.6(11) . . . . ? Nd4 N306 C324 C323 160.0(7) . . . . ? N305 N306 C324 C325 -178.9(8) . . . . ? Nd4 N306 C324 C325 -19.5(10) . . . . ? C322 C323 C324 N306 -0.9(13) . . . . ? C322 C323 C324 C325 178.5(10) . . . . ? C329 N307 C325 C326 -1.3(13) . . . . ? Nd4 N307 C325 C326 -158.3(7) . . . . ? C329 N307 C325 C324 178.7(8) . . . . ? Nd4 N307 C325 C324 21.6(10) . . . . ? N306 C324 C325 N307 -0.5(12) . . . . ? C323 C324 C325 N307 -179.8(10) . . . . ? N306 C324 C325 C326 179.5(9) . . . . ? C323 C324 C325 C326 0.1(15) . . . . ? N307 C325 C326 C327 1.5(15) . . . . ? C324 C325 C326 C327 -178.4(10) . . . . ? C325 C326 C327 C328 1.3(18) . . . . ? C326 C327 C328 C329 -4.1(18) . . . . ? C325 N307 C329 C328 -1.7(13) . . . . ? Nd4 N307 C329 C328 155.6(8) . . . . ? C325 N307 C329 C330 -177.9(8) . . . . ? Nd4 N307 C329 C330 -20.6(10) . . . . ? C327 C328 C329 N307 4.4(16) . . . . ? C327 C328 C329 C330 179.9(11) . . . . ? Nd4 O302 C330 N308 158.3(8) . . . . ? Nd4 O302 C330 C329 -21.2(13) . . . . ? C333 N308 C330 O302 -2.2(17) . . . . ? C331 N308 C330 O302 -175.6(11) . . . . ? C333 N308 C330 C329 177.3(11) . . . . ? C331 N308 C330 C329 3.9(19) . . . . ? N307 C329 C330 O302 26.3(13) . . . . ? C328 C329 C330 O302 -149.6(11) . . . . ? N307 C329 C330 N308 -153.3(10) . . . . ? C328 C329 C330 N308 30.8(17) . . . . ? C330 N308 C331 C332 -105.5(15) . . . . ? C333 N308 C331 C332 80.9(15) . . . . ? C330 N308 C333 C334 -91.8(15) . . . . ? C331 N308 C333 C334 82.4(15) . . . . ? C406 C401 C402 C403 0.9(16) . . . . ? C407 C401 C402 C403 -179.0(10) . . . . ? C401 C402 C403 C404 -0.1(17) . . . . ? C402 C403 C404 C405 -0.2(16) . . . . ? C402 C403 C404 C421 -179.9(10) . . . . ? C403 C404 C405 C406 -0.2(17) . . . . ? C421 C404 C405 C406 179.5(11) . . . . ? C404 C405 C406 C401 1.1(19) . . . . ? C402 C401 C406 C405 -1.3(16) . . . . ? C407 C401 C406 C405 178.5(11) . . . . ? C408 N404 C407 C401 88.5(17) . . . . ? N403 N404 C407 C401 -87.5(13) . . . . ? C406 C401 C407 N404 -6.3(14) . . . . ? C402 C401 C407 N404 173.6(9) . . . . ? N403 N404 C408 C409 1(2) . . . . ? C407 N404 C408 C409 -175.9(15) . . . . ? N404 C408 C409 C410 0(2) . . . . ? N404 N403 C410 C11' 173.8(17) . . . . ? Nd4 N403 C410 C11' -8(2) . . . . ? N404 N403 C410 C409 0.5(16) . . . . ? Nd4 N403 C410 C409 178.8(12) . . . . ? N404 N403 C410 C11 175.8(12) . . . . ? Nd4 N403 C410 C11 -5.9(15) . . . . ? C408 C409 C410 N403 0(2) . . . . ? C408 C409 C410 C11' -174.7(17) . . . . ? C408 C409 C410 C11 -174.4(17) . . . . ? C422 N405 C421 C404 -90.0(16) . . . . ? N406 N405 C421 C404 80.7(14) . . . . ? C405 C404 C421 N405 -133.3(11) . . . . ? C403 C404 C421 N405 46.5(14) . . . . ? N406 N405 C422 C423 -0.1(17) . . . . ? C421 N405 C422 C423 171.4(13) . . . . ? N405 C422 C423 C424 -0.2(18) . . . . ? N405 N406 C424 C423 -0.4(14) . . . . ? Nd1 N406 C424 C423 156.2(9) . . . . ? N405 N406 C424 C425 -178.5(9) . . . . ? Nd1 N406 C424 C425 -21.9(12) . . . . ? C422 C423 C424 N406 0.3(16) . . . . ? C422 C423 C424 C425 178.2(12) . . . . ? C429 N407 C425 C426 1.2(14) . . . . ? Nd1 N407 C425 C426 -155.0(8) . . . . ? C429 N407 C425 C424 -179.8(9) . . . . ? Nd1 N407 C425 C424 24.1(11) . . . . ? N406 C424 C425 N407 -0.6(14) . . . . ? C423 C424 C425 N407 -178.4(12) . . . . ? N406 C424 C425 C426 178.5(10) . . . . ? C423 C424 C425 C426 0.7(18) . . . . ? N407 C425 C426 C427 1.7(16) . . . . ? C424 C425 C426 C427 -177.3(10) . . . . ? C425 C426 C427 C428 -1.7(16) . . . . ? C426 C427 C428 C429 -1.1(16) . . . . ? C425 N407 C429 C428 -4.2(14) . . . . ? Nd1 N407 C429 C428 152.3(7) . . . . ? C425 N407 C429 C430 -176.7(8) . . . . ? Nd1 N407 C429 C430 -20.3(10) . . . . ? C427 C428 C429 N407 4.3(15) . . . . ? C427 C428 C429 C430 175.6(10) . . . . ? Nd1 O402 C430 N408 155.4(9) . . . . ? Nd1 O402 C430 C429 -24.6(13) . . . . ? C433 N408 C430 O402 -175.1(12) . . . . ? C431 N408 C430 O402 9.5(19) . . . . ? C433 N408 C430 C429 4.9(19) . . . . ? C431 N408 C430 C429 -170.5(12) . . . . ? N407 C429 C430 O402 28.3(13) . . . . ? C428 C429 C430 O402 -143.8(11) . . . . ? N407 C429 C430 N408 -151.7(11) . . . . ? C428 C429 C430 N408 36.2(17) . . . . ? C430 N408 C431 C432 -117(2) . . . . ? C433 N408 C431 C432 67(2) . . . . ? C430 N408 C433 C434 -109.8(16) . . . . ? C431 N408 C433 C434 65(2) . . . . ? O1A' Nd4 O1A C16 48(2) . . . . ? O302 Nd4 O1A C16 69.8(17) . . . . ? O510 Nd4 O1A C16 -69.0(17) . . . . ? O512 Nd4 O1A C16 148.1(17) . . . . ? N2 Nd4 O1A C16 0.2(16) . . . . ? O511 Nd4 O1A C16 -138.4(17) . . . . ? N307 Nd4 O1A C16 118.0(16) . . . . ? N403 Nd4 O1A C16 -8.3(19) . . . . ? N306 Nd4 O1A C16 -147.4(15) . . . . ? N2' Nd4 O1A C16 10.3(16) . . . . ? N403 C410 C11 C12 166.2(10) . . . . ? C11' C410 C11 C12 -19(4) . . . . ? C409 C410 C11 C12 -20(2) . . . . ? N403 C410 C11 N2 -14.7(18) . . . . ? C11' C410 C11 N2 160(5) . . . . ? C409 C410 C11 N2 159.3(17) . . . . ? N2 C11 C12 C13 0.0 . . . . ? C410 C11 C12 C13 179.1(16) . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 N2 0.0 . . . . ? C13 C14 C15 C16 174.3(19) . . . . ? C14 C15 N2 C11 0.0 . . . . ? C16 C15 N2 C11 -175.1(16) . . . . ? C14 C15 N2 Nd4 152.0(9) . . . . ? C16 C15 N2 Nd4 -23.1(15) . . . . ? C12 C11 N2 C15 0.0 . . . . ? C410 C11 N2 C15 -179.1(15) . . . . ? C12 C11 N2 Nd4 -152.1(9) . . . . ? C410 C11 N2 Nd4 28.8(14) . . . . ? O1A' Nd4 N2 C15 -1.0(8) . . . . ? O302 Nd4 N2 C15 -86.3(8) . . . . ? O1A Nd4 N2 C15 12.8(8) . . . . ? O510 Nd4 N2 C15 108.3(8) . . . . ? O512 Nd4 N2 C15 -26.1(9) . . . . ? O511 Nd4 N2 C15 55.2(8) . . . . ? N307 Nd4 N2 C15 -113.4(8) . . . . ? N403 Nd4 N2 C15 -174.6(8) . . . . ? N306 Nd4 N2 C15 150.1(7) . . . . ? N2' Nd4 N2 C15 -117(2) . . . . ? O1A' Nd4 N2 C11 151.9(10) . . . . ? O302 Nd4 N2 C11 66.5(8) . . . . ? O1A Nd4 N2 C11 165.7(9) . . . . ? O510 Nd4 N2 C11 -98.9(8) . . . . ? O512 Nd4 N2 C11 126.8(7) . . . . ? O511 Nd4 N2 C11 -151.9(7) . . . . ? N307 Nd4 N2 C11 39.5(9) . . . . ? N403 Nd4 N2 C11 -21.7(7) . . . . ? N306 Nd4 N2 C11 -57.0(10) . . . . ? N2' Nd4 N2 C11 35.6(17) . . . . ? Nd4 O1A C16 C15 -13(3) . . . . ? Nd4 O1A C16 N1 153.0(19) . . . . ? N2 C15 C16 O1A 24(3) . . . . ? C14 C15 C16 O1A -150.7(16) . . . . ? N2 C15 C16 N1 -141(2) . . . . ? C14 C15 C16 N1 45(3) . . . . ? C19 N1 C16 O1A -129(4) . . . . ? C17 N1 C16 O1A 23(4) . . . . ? C19 N1 C16 C15 37(5) . . . . ? C17 N1 C16 C15 -171(3) . . . . ? C19 N1 C17 C18 42(5) . . . . ? C16 N1 C17 C18 -113(3) . . . . ? C17 N1 C19 C20 92(5) . . . . ? C16 N1 C19 C20 -115(5) . . . . ? O302 Nd4 O1A' C16' 46.7(18) . . . . ? O1A Nd4 O1A' C16' -156(3) . . . . ? O510 Nd4 O1A' C16' -93.0(18) . . . . ? O512 Nd4 O1A' C16' 128.4(19) . . . . ? N2 Nd4 O1A' C16' -30.9(17) . . . . ? O511 Nd4 O1A' C16' -161.7(18) . . . . ? N307 Nd4 O1A' C16' 82.6(18) . . . . ? N403 Nd4 O1A' C16' -24(2) . . . . ? N306 Nd4 O1A' C16' -178.1(15) . . . . ? N2' Nd4 O1A' C16' -17.8(17) . . . . ? N403 C410 C11' C12' -174.2(13) . . . . ? C409 C410 C11' C12' -1(2) . . . . ? C11 C410 C11' C12' 179(5) . . . . ? N403 C410 C11' N2' 10(2) . . . . ? C409 C410 C11' N2' -177.3(14) . . . . ? C11 C410 C11' N2' 3(4) . . . . ? C410 C11' C12' C13' -176(2) . . . . ? N2' C11' C12' C13' 0.0 . . . . ? C11' C12' C13' C14' 0.0 . . . . ? C12' C13' C14' C15' 0.0 . . . . ? C13' C14' C15' N2' 0.0 . . . . ? C13' C14' C15' C16' -179(2) . . . . ? C14' C15' N2' C11' 0.0 . . . . ? C16' C15' N2' C11' 178.8(18) . . . . ? C14' C15' N2' Nd4 -176.9(10) . . . . ? C16' C15' N2' Nd4 1.8(16) . . . . ? C410 C11' N2' C15' 176.8(16) . . . . ? C12' C11' N2' C15' 0.0 . . . . ? C410 C11' N2' Nd4 -6.6(15) . . . . ? C12' C11' N2' Nd4 176.6(11) . . . . ? O1A' Nd4 N2' C15' 6.3(9) . . . . ? O302 Nd4 N2' C15' -83.2(9) . . . . ? O1A Nd4 N2' C15' 16.8(9) . . . . ? O510 Nd4 N2' C15' 105.8(9) . . . . ? O512 Nd4 N2' C15' -35.1(10) . . . . ? N2 Nd4 N2' C15' 62.8(17) . . . . ? O511 Nd4 N2' C15' 54.2(10) . . . . ? N307 Nd4 N2' C15' -113.7(8) . . . . ? N403 Nd4 N2' C15' 179.6(10) . . . . ? N306 Nd4 N2' C15' 169.4(8) . . . . ? O1A' Nd4 N2' C11' -170.5(11) . . . . ? O302 Nd4 N2' C11' 100.0(10) . . . . ? O1A Nd4 N2' C11' -159.9(11) . . . . ? O510 Nd4 N2' C11' -70.9(10) . . . . ? O512 Nd4 N2' C11' 148.2(9) . . . . ? N2 Nd4 N2' C11' -114(2) . . . . ? O511 Nd4 N2' C11' -122.5(10) . . . . ? N307 Nd4 N2' C11' 69.5(10) . . . . ? N403 Nd4 N2' C11' 2.9(9) . . . . ? N306 Nd4 N2' C11' -7.3(13) . . . . ? Nd4 O1A' C16' C15' 27(3) . . . . ? Nd4 O1A' C16' N1' -139(2) . . . . ? N2' C15' C16' O1A' -16(3) . . . . ? C14' C15' C16' O1A' 162.2(17) . . . . ? N2' C15' C16' N1' 150(2) . . . . ? C14' C15' C16' N1' -31(3) . . . . ? C19' N1' C16' O1A' 155(3) . . . . ? C17' N1' C16' O1A' -1(5) . . . . ? C19' N1' C16' C15' -12(5) . . . . ? C17' N1' C16' C15' -168(3) . . . . ? C19' N1' C17' C18' 130(4) . . . . ? C16' N1' C17' C18' -72(4) . . . . ? C17' N1' C19' C20' -94(4) . . . . ? C16' N1' C19' C20' 108(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.765 _refine_diff_density_min -1.743 _refine_diff_density_rms 0.253 #===END data_imw702 _database_code_depnum_ccdc_archive 'CCDC 630963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70.50 H89.50 Cl6 La2 N18.50 O36' _chemical_formula_weight 2262.63 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' La La -0.2871 2.4523 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 25.4319(14) _cell_length_b 16.2490(8) _cell_length_c 28.1488(14) _cell_angle_alpha 90.00 _cell_angle_beta 98.599(3) _cell_angle_gamma 90.00 _cell_volume 11501.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7781 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 22.47 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4584 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8257 _exptl_absorpt_correction_T_max 0.9029 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 218051 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 20238 _reflns_number_gt 12825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20238 _refine_ls_number_parameters 1124 _refine_ls_number_restraints 176 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.2002 _refine_ls_wR_factor_gt 0.1847 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.081 _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 La1 La 0.373365(18) 0.02947(2) 0.627459(14) 0.05502(15) Uani 1 1 d . . . La2 La 0.201374(16) 0.48776(2) 0.456770(12) 0.05089(14) Uani 1 1 d . . . O1 O 0.1323(2) 0.5914(3) 0.45240(16) 0.0602(12) Uani 1 1 d . . . O2 O 0.4477(2) 0.0485(3) 0.69232(17) 0.0770(15) Uani 1 1 d . B . O3 O 0.2469(2) 0.5651(3) 0.40017(15) 0.0660(13) Uani 1 1 d . B . O4 O 0.39743(18) -0.1178(2) 0.63506(14) 0.0545(11) Uani 1 1 d . B . O5 O 0.2250(2) 0.3486(3) 0.49595(16) 0.0691(13) Uani 1 1 d . . . O6 O 0.30548(19) 0.1295(3) 0.58329(16) 0.0645(13) Uani 1 1 d . B . N1 N 0.0450(2) 0.6218(4) 0.44033(19) 0.0617(15) Uani 1 1 d . . . N2 N 0.1293(2) 0.4994(3) 0.37693(17) 0.0573(15) Uani 1 1 d . . . N3 N 0.2163(2) 0.4022(3) 0.37834(18) 0.0572(14) Uani 1 1 d . . . N4 N 0.2581(3) 0.3581(3) 0.36623(19) 0.0676(17) Uani 1 1 d . . . N5 N 0.3564(2) -0.0254(3) 0.4945(2) 0.0574(15) Uani 1 1 d . . . N6 N 0.3874(2) -0.0144(3) 0.53691(18) 0.0504(13) Uani 1 1 d . B . N7 N 0.4714(3) -0.0049(3) 0.6101(2) 0.0578(15) Uani 1 1 d . B . N8 N 0.5309(3) 0.0876(4) 0.7186(2) 0.0747(18) Uani 1 1 d . . . N9 N 0.3186(2) 0.6391(4) 0.39135(19) 0.0650(16) Uani 1 1 d . B . N10 N 0.2381(2) 0.6388(3) 0.48199(17) 0.0494(13) Uani 1 1 d . . . N11 N 0.1931(2) 0.5441(3) 0.54643(17) 0.0514(13) Uani 1 1 d . B . N12 N 0.1717(2) 0.5156(3) 0.58471(17) 0.0496(13) Uani 1 1 d . B . N13 N 0.3416(2) 0.1896(3) 0.71833(19) 0.0585(15) Uani 1 1 d . . . N14 N 0.3398(2) 0.1120(3) 0.70222(18) 0.0557(14) Uani 1 1 d . B . N15 N 0.3427(2) -0.0576(3) 0.69823(17) 0.0519(13) Uani 1 1 d . B . N16 N 0.36224(19) -0.2428(3) 0.63436(15) 0.0429(11) Uani 1 1 d . . . C1 C 0.3455(3) 0.2244(4) 0.4505(3) 0.069(2) Uani 1 1 d . . . H1 H 0.3753 0.2581 0.4564 0.082 Uiso 1 1 calc R . . C2 C 0.3471(3) 0.1468(4) 0.4717(3) 0.069(2) Uani 1 1 d . B . H2 H 0.3773 0.1294 0.4920 0.082 Uiso 1 1 calc R . . C4 C 0.2584(3) 0.1253(4) 0.4332(2) 0.070(2) Uani 1 1 d . B . H4 H 0.2283 0.0922 0.4275 0.084 Uiso 1 1 calc R . . C5 C 0.2580(4) 0.2018(5) 0.4133(3) 0.079(2) Uani 1 1 d . . . H5 H 0.2276 0.2204 0.3938 0.095 Uiso 1 1 calc R . . C6 C 0.3021(3) 0.2519(4) 0.4217(2) 0.0599(19) Uani 1 1 d . . . C7 C 0.3028(3) 0.3381(4) 0.4002(2) 0.066(2) Uani 1 1 d . . . H7A H 0.3057 0.3779 0.4261 0.080 Uiso 1 1 calc R . . H7B H 0.3344 0.3433 0.3849 0.080 Uiso 1 1 calc R . . C8 C 0.2483(4) 0.3366(5) 0.3191(2) 0.089(2) Uani 1 1 d U . . H8 H 0.2704 0.3044 0.3032 0.107 Uiso 1 1 calc R . . C9 C 0.2005(4) 0.3699(5) 0.2986(2) 0.089(2) Uani 1 1 d U . . H9 H 0.1842 0.3670 0.2667 0.106 Uiso 1 1 calc R . . C10 C 0.1821(3) 0.4095(4) 0.3375(2) 0.067(2) Uani 1 1 d . . . C11 C 0.1351(3) 0.4642(4) 0.3355(2) 0.0635(19) Uani 1 1 d . . . C12 C 0.1016(3) 0.4784(6) 0.2934(3) 0.0819(18) Uani 1 1 d U . . H12 H 0.1075 0.4521 0.2653 0.098 Uiso 1 1 calc R . . C13 C 0.0605(3) 0.5300(6) 0.2927(3) 0.0830(16) Uani 1 1 d U . . H13 H 0.0373 0.5388 0.2644 0.100 Uiso 1 1 calc R . . C14 C 0.0526(3) 0.5715(6) 0.3356(2) 0.0794(18) Uani 1 1 d U . . H14 H 0.0253 0.6096 0.3356 0.095 Uiso 1 1 calc R . . C15 C 0.0868(3) 0.5532(4) 0.3772(2) 0.0631(19) Uani 1 1 d . . . C16 C 0.0872(3) 0.5897(4) 0.4253(2) 0.0594(18) Uani 1 1 d . . . C17 C -0.0103(3) 0.6183(5) 0.4166(3) 0.072(2) Uani 1 1 d . . . H17A H -0.0330 0.6023 0.4399 0.087 Uiso 1 1 calc R . . H17B H -0.0136 0.5767 0.3916 0.087 Uiso 1 1 calc R . . C18 C -0.0288(3) 0.7001(5) 0.3948(3) 0.082(2) Uani 1 1 d . . . H18A H -0.0264 0.7412 0.4196 0.123 Uiso 1 1 calc R . . H18B H -0.0651 0.6955 0.3796 0.123 Uiso 1 1 calc R . . H18C H -0.0068 0.7157 0.3714 0.123 Uiso 1 1 calc R . . C19 C 0.0525(3) 0.6596(5) 0.4899(3) 0.075(2) Uani 1 1 d . . . H19A H 0.0872 0.6858 0.4962 0.090 Uiso 1 1 calc R . . H19B H 0.0257 0.7014 0.4915 0.090 Uiso 1 1 calc R . . C20 C 0.0485(3) 0.5957(6) 0.5269(3) 0.082(2) Uani 1 1 d . . . H20A H 0.0131 0.5736 0.5225 0.123 Uiso 1 1 calc R . . H20B H 0.0564 0.6198 0.5583 0.123 Uiso 1 1 calc R . . H20C H 0.0734 0.5524 0.5238 0.123 Uiso 1 1 calc R . . C21 C 0.3020(3) 0.0118(4) 0.4834(3) 0.066(2) Uani 1 1 d . B . H21A H 0.2862 0.0149 0.5127 0.079 Uiso 1 1 calc R . . H21B H 0.2797 -0.0233 0.4610 0.079 Uiso 1 1 calc R . . C22 C 0.3812(3) -0.0670(4) 0.4628(2) 0.0633(16) Uani 1 1 d U B . H22 H 0.3669 -0.0820 0.4317 0.076 Uiso 1 1 calc R . . C23 C 0.4317(3) -0.0828(4) 0.4856(2) 0.0623(15) Uani 1 1 d U . . H23 H 0.4588 -0.1097 0.4731 0.075 Uiso 1 1 calc R B . C24 C 0.4336(3) -0.0499(3) 0.5315(2) 0.0519(17) Uani 1 1 d . B . C25 C 0.4770(3) -0.0488(4) 0.5711(2) 0.0589(19) Uani 1 1 d . . . C26 C 0.5236(3) -0.0942(4) 0.5686(3) 0.073(2) Uani 1 1 d . B . H26 H 0.5277 -0.1243 0.5413 0.087 Uiso 1 1 calc R . . C27 C 0.5631(4) -0.0927(5) 0.6083(3) 0.080(2) Uani 1 1 d . . . H27 H 0.5940 -0.1232 0.6079 0.096 Uiso 1 1 calc R B . C28 C 0.5572(4) -0.0464(5) 0.6482(3) 0.081(2) Uani 1 1 d . B . H28 H 0.5837 -0.0451 0.6748 0.097 Uiso 1 1 calc R . . C29 C 0.5104(3) -0.0018(4) 0.6478(3) 0.0589(19) Uani 1 1 d . . . C30 C 0.4961(4) 0.0480(4) 0.6882(2) 0.064(2) Uani 1 1 d . B . C31 C 0.5114(4) 0.1320(6) 0.7596(3) 0.105(3) Uiso 1 1 d . . . H31A H 0.4823 0.1014 0.7699 0.125 Uiso 1 1 calc R . . H31B H 0.5399 0.1358 0.7865 0.125 Uiso 1 1 calc R . . C32 C 0.4931(5) 0.2149(7) 0.7444(4) 0.132(4) Uiso 1 1 d . . . H32A H 0.5232 0.2508 0.7455 0.198 Uiso 1 1 calc R . . H32B H 0.4698 0.2352 0.7656 0.198 Uiso 1 1 calc R . . H32C H 0.4743 0.2127 0.7122 0.198 Uiso 1 1 calc R . . C33 C 0.5856(3) 0.1046(5) 0.7150(3) 0.081(2) Uiso 1 1 d . . . H33A H 0.5914 0.1634 0.7187 0.097 Uiso 1 1 calc R . . H33B H 0.5920 0.0897 0.6830 0.097 Uiso 1 1 calc R . . C34 C 0.6267(4) 0.0600(7) 0.7519(4) 0.117(3) Uiso 1 1 d . . . H34A H 0.6225 0.0772 0.7837 0.176 Uiso 1 1 calc R . . H34B H 0.6619 0.0733 0.7459 0.176 Uiso 1 1 calc R . . H34C H 0.6213 0.0016 0.7490 0.176 Uiso 1 1 calc R . . C35 C 0.2119(3) 0.3043(4) 0.6300(2) 0.0521(17) Uani 1 1 d . . . H35 H 0.1797 0.2766 0.6224 0.063 Uiso 1 1 calc R . . C36 C 0.2543(3) 0.2630(4) 0.6528(2) 0.0594(18) Uani 1 1 d . B . H36 H 0.2511 0.2078 0.6606 0.071 Uiso 1 1 calc R . . C37 C 0.3030(3) 0.3029(4) 0.6649(2) 0.0556(18) Uani 1 1 d . . . C38 C 0.3062(3) 0.3857(4) 0.6534(2) 0.0553(17) Uani 1 1 d . B . H38 H 0.3378 0.4143 0.6621 0.066 Uiso 1 1 calc R . . C39 C 0.2622(3) 0.4256(4) 0.6288(2) 0.0563(17) Uani 1 1 d . . . H39 H 0.2652 0.4802 0.6198 0.068 Uiso 1 1 calc R B . C40 C 0.2145(3) 0.3861(4) 0.6176(2) 0.0533(17) Uani 1 1 d . B . C41 C 0.1653(3) 0.4281(4) 0.5924(2) 0.0560(17) Uani 1 1 d . . . H41A H 0.1548 0.4017 0.5616 0.067 Uiso 1 1 calc R B . H41B H 0.1368 0.4202 0.6113 0.067 Uiso 1 1 calc R . . C42 C 0.1648(3) 0.5785(4) 0.6151(2) 0.0519(16) Uani 1 1 d . . . H42 H 0.1515 0.5736 0.6441 0.062 Uiso 1 1 calc R B . C43 C 0.1803(3) 0.6484(4) 0.5965(2) 0.0553(17) Uani 1 1 d . B . H43 H 0.1793 0.7010 0.6092 0.066 Uiso 1 1 calc R . . C44 C 0.1986(2) 0.6259(4) 0.5535(2) 0.0492(15) Uani 1 1 d . . . C45 C 0.2187(2) 0.6770(4) 0.5178(2) 0.0496(15) Uani 1 1 d . B . C46 C 0.2162(3) 0.7623(4) 0.5190(2) 0.0627(19) Uani 1 1 d . . . H46 H 0.2025 0.7890 0.5437 0.075 Uiso 1 1 calc R B . C47 C 0.2342(3) 0.8066(4) 0.4833(3) 0.071(2) Uani 1 1 d . B . H47 H 0.2311 0.8636 0.4825 0.085 Uiso 1 1 calc R . . C48 C 0.2571(3) 0.7658(4) 0.4481(3) 0.0659(19) Uani 1 1 d . . . H48 H 0.2711 0.7954 0.4246 0.079 Uiso 1 1 calc R B . C49 C 0.2588(3) 0.6817(4) 0.4485(2) 0.0544(16) Uani 1 1 d . B . C50 C 0.2761(3) 0.6262(4) 0.4115(2) 0.0542(17) Uani 1 1 d . . . C51 C 0.3605(3) 0.7003(5) 0.4078(3) 0.0669(19) Uiso 1 1 d . . . H51A H 0.3941 0.6722 0.4173 0.080 Uiso 1 1 calc R B . H51B H 0.3515 0.7292 0.4357 0.080 Uiso 1 1 calc R . . C52 C 0.3663(3) 0.7611(5) 0.3690(3) 0.085(2) Uiso 1 1 d . B . H52A H 0.3720 0.7323 0.3404 0.128 Uiso 1 1 calc R . . H52B H 0.3961 0.7965 0.3793 0.128 Uiso 1 1 calc R . . H52C H 0.3345 0.7936 0.3623 0.128 Uiso 1 1 calc R . . C53 C 0.3343(4) 0.5712(6) 0.3578(3) 0.097(3) Uiso 1 1 d . . . H53A H 0.3715 0.5777 0.3545 0.116 Uiso 1 1 calc R B . H53B H 0.3302 0.5179 0.3723 0.116 Uiso 1 1 calc R . . C54 C 0.3028(4) 0.5726(8) 0.3102(4) 0.129(4) Uiso 1 1 d . B . H54A H 0.2661 0.5817 0.3131 0.194 Uiso 1 1 calc R . . H54B H 0.3063 0.5209 0.2945 0.194 Uiso 1 1 calc R . . H54C H 0.3151 0.6161 0.2916 0.194 Uiso 1 1 calc R . . C55 C 0.3525(3) 0.2602(4) 0.6871(2) 0.0600(19) Uani 1 1 d . B . H55A H 0.3754 0.2994 0.7062 0.072 Uiso 1 1 calc R . . H55B H 0.3712 0.2401 0.6619 0.072 Uiso 1 1 calc R . . C56 C 0.3312(3) 0.1957(4) 0.7630(2) 0.067(2) Uani 1 1 d . B . H56 H 0.3302 0.2441 0.7804 0.081 Uiso 1 1 calc R . . C57 C 0.3223(3) 0.1186(4) 0.7788(3) 0.071(2) Uani 1 1 d . . . H57 H 0.3136 0.1034 0.8085 0.085 Uiso 1 1 calc R B . C58 C 0.3291(3) 0.0674(4) 0.7403(2) 0.0604(19) Uani 1 1 d . B . C59 C 0.3282(3) -0.0222(4) 0.7380(2) 0.0573(18) Uani 1 1 d . . . C60 C 0.3156(3) -0.0696(4) 0.7757(2) 0.072(2) Uani 1 1 d . B . H60 H 0.3048 -0.0444 0.8023 0.086 Uiso 1 1 calc R . . C61 C 0.3190(3) -0.1540(4) 0.7736(2) 0.069(2) Uani 1 1 d . . . H61 H 0.3107 -0.1860 0.7988 0.083 Uiso 1 1 calc R B . C62 C 0.3346(3) -0.1905(3) 0.7342(2) 0.0555(17) Uani 1 1 d . B . H62 H 0.3380 -0.2474 0.7326 0.067 Uiso 1 1 calc R . . C63 C 0.3455(3) -0.1397(3) 0.6960(2) 0.0493(15) Uani 1 1 d . . . C64 C 0.3684(2) -0.1683(3) 0.6532(2) 0.0459(14) Uani 1 1 d . B . C65 C 0.3214(3) -0.3025(4) 0.6432(2) 0.0522(16) Uani 1 1 d . . . H65A H 0.3019 -0.3201 0.6126 0.063 Uiso 1 1 calc R . . H65B H 0.2965 -0.2759 0.6611 0.063 Uiso 1 1 calc R . . C66 C 0.3448(3) -0.3773(3) 0.6707(2) 0.0615(19) Uani 1 1 d . . . H66A H 0.3739 -0.3981 0.6562 0.092 Uiso 1 1 calc R . . H66B H 0.3179 -0.4190 0.6700 0.092 Uiso 1 1 calc R . . H66C H 0.3572 -0.3621 0.7034 0.092 Uiso 1 1 calc R . . C67 C 0.3932(3) -0.2648(4) 0.5957(2) 0.0538(17) Uani 1 1 d . . . H67A H 0.4273 -0.2371 0.6014 0.065 Uiso 1 1 calc R . . H67B H 0.3998 -0.3237 0.5966 0.065 Uiso 1 1 calc R . . C68 C 0.3656(3) -0.2422(4) 0.5474(2) 0.0662(19) Uani 1 1 d . . . H68A H 0.3314 -0.2686 0.5419 0.099 Uiso 1 1 calc R . . H68B H 0.3864 -0.2598 0.5235 0.099 Uiso 1 1 calc R . . H68C H 0.3609 -0.1836 0.5456 0.099 Uiso 1 1 calc R . . C69 C 0.3040(3) 0.0969(4) 0.4622(2) 0.0563(18) Uani 1 1 d . . . Cl1 Cl 0.09523(9) 0.33411(14) 0.45688(8) 0.0835(6) Uani 1 1 d D . . Cl2 Cl 0.34717(8) 0.50540(10) 0.52005(6) 0.0594(4) Uani 1 1 d . . . Cl3 Cl 0.45560(8) 0.21023(9) 0.58774(7) 0.0735(6) Uani 1 1 d D . . Cl5 Cl 0.90104(7) 0.56169(10) 0.28219(5) 0.0595(4) Uani 1 1 d D . . O10 O 0.1144(2) 0.4143(3) 0.47195(18) 0.0774(14) Uani 1 1 d . A . O11 O 0.0504(3) 0.3416(6) 0.4202(3) 0.140(3) Uani 1 1 d . A . O12 O 0.0947(7) 0.2880(7) 0.5037(4) 0.075(3) Uiso 0.478(19) 1 d PDU A 1 O13 O 0.1381(5) 0.3085(12) 0.4319(5) 0.094(4) Uiso 0.478(19) 1 d PDU A 1 O12' O 0.0695(6) 0.2957(7) 0.4926(4) 0.075(3) Uiso 0.522(19) 1 d PDU A 2 O13' O 0.1357(4) 0.2742(8) 0.4450(5) 0.077(3) Uiso 0.522(19) 1 d PDU A 2 O14 O 0.2987(2) 0.4727(3) 0.49235(18) 0.0708(14) Uani 1 1 d . . . O15 O 0.3322(3) 0.5448(4) 0.5613(2) 0.106(2) Uani 1 1 d . . . O16 O 0.3694(2) 0.5624(4) 0.4920(2) 0.0887(17) Uani 1 1 d . . . O17 O 0.3825(2) 0.4395(4) 0.5326(3) 0.107(2) Uani 1 1 d . . . O18 O 0.4198(3) 0.1622(5) 0.6118(3) 0.0453(19) Uiso 0.514(11) 1 d PDU B 1 O19 O 0.4341(4) 0.2880(5) 0.5726(4) 0.076(3) Uiso 0.514(11) 1 d PDU B 1 O20 O 0.5021(4) 0.2135(9) 0.6226(4) 0.100(4) Uiso 0.514(11) 1 d PDU B 1 O21 O 0.4662(4) 0.1658(7) 0.5460(3) 0.082(3) Uiso 0.514(11) 1 d PD B 1 O18' O 0.4051(3) 0.1646(5) 0.5939(3) 0.0419(19) Uiso 0.486(11) 1 d PDU B 2 O19' O 0.4477(4) 0.2947(5) 0.6034(4) 0.080(3) Uiso 0.486(11) 1 d PDU B 2 O20' O 0.5028(4) 0.1779(8) 0.6125(4) 0.092(3) Uiso 0.486(11) 1 d PDU B 2 O21' O 0.4558(4) 0.2085(9) 0.5364(3) 0.093(4) Uiso 0.486(11) 1 d PD B 2 Cl4 Cl 0.23935(7) -0.05319(9) 0.60124(6) 0.0576(4) Uani 1 1 d . . . O22 O 0.29332(19) -0.0624(3) 0.58980(15) 0.0619(12) Uani 1 1 d . B . O23 O 0.2385(2) 0.0171(3) 0.63167(17) 0.0712(14) Uani 1 1 d . B . O24 O 0.2052(2) -0.0419(3) 0.55733(18) 0.0740(14) Uani 1 1 d . B . O25 O 0.22611(19) -0.1264(3) 0.62515(16) 0.0667(13) Uani 1 1 d . B . O28 O 0.9226(2) 0.5220(4) 0.32565(19) 0.0852(17) Uani 1 1 d D C . O26 O 0.9248(9) 0.5837(13) 0.2419(7) 0.087(4) Uiso 0.221(8) 1 d PDU C 1 O27 O 0.8747(9) 0.4797(10) 0.2716(10) 0.094(5) Uiso 0.221(8) 1 d PDU C 1 O29 O 0.8686(9) 0.6159(11) 0.3020(9) 0.066(5) Uiso 0.221(8) 1 d PDU C 1 O26' O 0.9416(3) 0.6201(4) 0.2717(3) 0.084(2) Uiso 0.779(8) 1 d PDU C 2 O27' O 0.8914(3) 0.5059(5) 0.2440(3) 0.089(2) Uiso 0.779(8) 1 d PDU C 2 O29' O 0.8514(3) 0.6055(4) 0.2855(3) 0.072(2) Uiso 0.779(8) 1 d PDU C 2 O1W O 0.3167(2) 0.2924(3) 0.55232(17) 0.0703(14) Uani 1 1 d . . . O2S O 0.5262(4) 0.4439(7) 0.5995(4) 0.173(3) Uiso 1 1 d D . . O1S O 0.5432(4) 0.4008(7) 0.6759(4) 0.186(4) Uiso 1 1 d D . . N1S N 0.5144(5) 0.4372(8) 0.6425(5) 0.167(4) Uiso 1 1 d D . . C1S C 0.4651(5) 0.4600(8) 0.6494(5) 0.135(4) Uiso 1 1 d . . . H1S1 H 0.4565 0.4339 0.6778 0.203 Uiso 1 1 calc R . . H1S2 H 0.4399 0.4436 0.6222 0.203 Uiso 1 1 calc R . . H1S3 H 0.4639 0.5187 0.6531 0.203 Uiso 1 1 calc R . . N2S N 0.7500 0.3906(5) 0.2500 0.063(2) Uani 1 2 d S . . O3S O 0.7752(3) 0.3538(4) 0.28368(19) 0.0934(18) Uani 1 1 d . . . C2S C 0.7500 0.4791(6) 0.2500 0.076(3) Uani 1 2 d S . . H2S1 H 0.7716 0.4988 0.2272 0.114 Uiso 0.50 1 calc PR . . H2S2 H 0.7641 0.4988 0.2815 0.114 Uiso 0.50 1 calc PR . . H2S3 H 0.7143 0.4988 0.2413 0.114 Uiso 0.50 1 calc PR . . O5S O 0.1968(3) 0.1584(5) 0.5391(2) 0.116(2) Uiso 1 1 d . . . N3S N 0.1525(4) 0.1317(6) 0.5411(4) 0.125(3) Uiso 1 1 d . . . O4S O 0.1377(4) 0.1343(6) 0.5816(4) 0.161(3) Uiso 1 1 d . . . C3S C 0.1175(5) 0.0979(9) 0.5060(5) 0.165(5) Uiso 1 1 d . . . H3S1 H 0.1353 0.0843 0.4792 0.248 Uiso 1 1 calc R . . H3S2 H 0.0894 0.1364 0.4959 0.248 Uiso 1 1 calc R . . H3S3 H 0.1029 0.0489 0.5178 0.248 Uiso 1 1 calc R . . Cl6 Cl 0.2601(2) 0.9597(3) 0.34041(15) 0.1859(19) Uani 1 1 d DU . . O30 O 0.2528(6) 0.8907(8) 0.3028(5) 0.315(9) Uani 1 1 d DU . . O33 O 0.2345(7) 0.9392(9) 0.3821(4) 0.361(13) Uani 1 1 d DU . . O32 O 0.3196(3) 0.9744(6) 0.3535(3) 0.183(5) Uani 1 1 d DU . . O31 O 0.2390(6) 1.0371(7) 0.3147(4) 0.290(9) Uani 1 1 d DU . . 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 La1 0.0945(3) 0.02726(19) 0.0557(2) -0.00335(15) 0.0517(2) -0.00655(17) La2 0.0771(3) 0.0423(2) 0.0406(2) -0.00778(15) 0.03265(19) -0.01271(18) O1 0.073(3) 0.057(3) 0.054(3) -0.020(2) 0.020(2) -0.008(2) O2 0.107(4) 0.068(3) 0.067(3) -0.023(3) 0.050(3) -0.023(3) O3 0.103(4) 0.051(3) 0.054(3) -0.010(2) 0.045(3) -0.029(3) O4 0.090(3) 0.029(2) 0.055(2) 0.0000(18) 0.042(2) -0.001(2) O5 0.105(4) 0.047(3) 0.066(3) -0.008(2) 0.048(3) -0.016(3) O6 0.097(4) 0.038(2) 0.071(3) 0.001(2) 0.053(3) 0.000(2) N1 0.069(4) 0.064(4) 0.057(3) -0.020(3) 0.026(3) -0.008(3) N2 0.085(4) 0.052(3) 0.042(3) -0.012(2) 0.029(3) -0.017(3) N3 0.100(4) 0.038(3) 0.041(3) 0.000(2) 0.033(3) -0.005(3) N4 0.109(5) 0.054(3) 0.048(3) 0.008(3) 0.041(3) 0.017(3) N5 0.091(4) 0.038(3) 0.053(3) 0.008(2) 0.041(3) 0.001(3) N6 0.081(4) 0.035(3) 0.042(3) 0.003(2) 0.032(3) -0.001(3) N7 0.096(5) 0.031(3) 0.057(3) -0.001(2) 0.047(3) -0.008(3) N8 0.090(5) 0.075(4) 0.069(4) -0.013(3) 0.044(4) -0.012(4) N9 0.081(4) 0.069(4) 0.054(3) 0.001(3) 0.041(3) -0.010(3) N10 0.069(4) 0.040(3) 0.044(3) -0.002(2) 0.023(3) -0.015(2) N11 0.066(4) 0.055(3) 0.039(3) -0.007(2) 0.025(2) -0.025(3) N12 0.069(4) 0.049(3) 0.039(3) -0.008(2) 0.034(3) -0.014(3) N13 0.089(4) 0.028(2) 0.071(3) -0.002(2) 0.053(3) -0.003(3) N14 0.091(4) 0.031(3) 0.057(3) -0.004(2) 0.048(3) -0.006(3) N15 0.078(4) 0.032(3) 0.056(3) -0.005(2) 0.042(3) -0.006(2) N16 0.064(3) 0.033(2) 0.037(3) 0.0026(19) 0.023(2) -0.002(2) C1 0.084(5) 0.042(4) 0.096(5) 0.017(4) 0.064(5) 0.012(4) C2 0.083(5) 0.046(4) 0.091(5) 0.020(4) 0.056(4) 0.009(4) C4 0.102(6) 0.053(4) 0.054(4) 0.012(3) 0.010(4) -0.008(4) C5 0.126(7) 0.060(5) 0.052(4) 0.015(4) 0.010(4) 0.008(5) C6 0.101(6) 0.041(4) 0.047(4) -0.002(3) 0.042(4) 0.008(4) C7 0.113(6) 0.039(4) 0.054(4) 0.003(3) 0.034(4) 0.013(4) C8 0.159(7) 0.079(4) 0.037(3) 0.004(3) 0.042(4) 0.039(4) C9 0.158(7) 0.079(4) 0.037(3) 0.002(3) 0.042(4) 0.036(4) C10 0.114(6) 0.051(4) 0.046(4) -0.009(3) 0.042(4) -0.006(4) C11 0.095(6) 0.058(4) 0.043(4) -0.011(3) 0.029(4) -0.011(4) C12 0.085(4) 0.113(5) 0.052(3) -0.027(3) 0.023(3) -0.011(3) C13 0.084(4) 0.117(4) 0.051(3) -0.027(3) 0.019(3) -0.006(3) C14 0.080(4) 0.112(5) 0.050(3) -0.026(3) 0.021(3) -0.009(3) C15 0.078(5) 0.063(4) 0.056(4) -0.018(3) 0.033(4) -0.025(4) C16 0.080(5) 0.046(4) 0.057(4) -0.007(3) 0.027(4) -0.007(4) C17 0.070(5) 0.091(6) 0.059(4) -0.015(4) 0.016(4) -0.022(4) C18 0.077(5) 0.098(7) 0.073(5) -0.006(5) 0.020(4) -0.009(5) C19 0.075(5) 0.089(6) 0.065(5) -0.045(4) 0.023(4) -0.006(4) C20 0.080(5) 0.114(7) 0.056(4) -0.029(5) 0.023(4) -0.001(5) C21 0.094(6) 0.047(4) 0.061(4) 0.007(3) 0.030(4) 0.004(4) C22 0.108(4) 0.037(3) 0.053(3) 0.000(2) 0.039(3) 0.006(3) C23 0.106(4) 0.038(3) 0.052(3) -0.002(2) 0.042(3) 0.007(3) C24 0.087(5) 0.031(3) 0.045(4) 0.005(3) 0.035(4) 0.003(3) C25 0.098(5) 0.032(3) 0.060(4) 0.013(3) 0.053(4) 0.005(3) C26 0.119(7) 0.049(4) 0.059(5) 0.010(3) 0.041(5) 0.029(4) C27 0.117(7) 0.075(5) 0.057(5) 0.011(4) 0.035(5) 0.038(5) C28 0.140(8) 0.064(5) 0.043(4) 0.011(3) 0.028(4) 0.021(5) C29 0.092(6) 0.031(3) 0.062(4) 0.004(3) 0.040(4) 0.001(3) C30 0.096(6) 0.050(4) 0.054(4) -0.007(3) 0.038(4) -0.018(4) C35 0.071(5) 0.041(3) 0.054(4) -0.012(3) 0.041(3) -0.021(3) C36 0.091(5) 0.036(3) 0.062(4) -0.005(3) 0.045(4) -0.015(4) C37 0.079(5) 0.038(3) 0.063(4) -0.006(3) 0.054(4) -0.003(3) C38 0.074(5) 0.040(3) 0.061(4) -0.007(3) 0.038(4) -0.010(3) C39 0.077(5) 0.039(3) 0.061(4) -0.007(3) 0.036(4) -0.008(4) C40 0.078(5) 0.050(4) 0.042(3) -0.016(3) 0.041(3) -0.020(4) C41 0.078(5) 0.055(4) 0.043(3) -0.007(3) 0.037(3) -0.015(4) C42 0.070(4) 0.056(4) 0.036(3) -0.006(3) 0.030(3) -0.011(3) C43 0.070(5) 0.055(4) 0.047(4) -0.018(3) 0.025(3) -0.009(3) C44 0.053(4) 0.051(4) 0.049(3) -0.018(3) 0.024(3) -0.011(3) C45 0.064(4) 0.042(3) 0.050(3) -0.011(3) 0.029(3) -0.020(3) C46 0.069(5) 0.054(4) 0.074(5) -0.019(3) 0.040(4) -0.016(3) C47 0.094(6) 0.041(4) 0.087(5) -0.003(4) 0.044(4) -0.014(4) C48 0.087(5) 0.047(4) 0.071(5) 0.001(3) 0.037(4) -0.023(4) C49 0.069(4) 0.046(4) 0.053(4) -0.006(3) 0.026(3) -0.014(3) C50 0.073(5) 0.062(4) 0.032(3) 0.011(3) 0.022(3) -0.005(4) C55 0.099(5) 0.031(3) 0.064(4) -0.001(3) 0.058(4) 0.001(3) C56 0.119(6) 0.035(3) 0.059(4) -0.010(3) 0.053(4) -0.002(4) C57 0.114(6) 0.042(4) 0.074(5) -0.010(3) 0.071(4) -0.004(4) C58 0.095(5) 0.033(3) 0.066(4) -0.006(3) 0.053(4) -0.012(3) C59 0.085(5) 0.036(3) 0.062(4) -0.005(3) 0.052(4) -0.008(3) C60 0.132(7) 0.040(4) 0.060(4) -0.001(3) 0.069(4) 0.002(4) C61 0.120(6) 0.043(4) 0.058(4) -0.002(3) 0.061(4) -0.010(4) C62 0.091(5) 0.025(3) 0.059(4) 0.001(3) 0.043(4) -0.008(3) C63 0.070(4) 0.034(3) 0.051(4) 0.004(3) 0.033(3) -0.007(3) C64 0.068(4) 0.026(3) 0.050(3) 0.001(2) 0.030(3) -0.002(3) C65 0.064(4) 0.039(3) 0.057(4) -0.009(3) 0.024(3) -0.014(3) C66 0.113(6) 0.027(3) 0.053(4) 0.002(3) 0.040(4) -0.003(3) C67 0.088(5) 0.027(3) 0.055(4) -0.001(3) 0.037(3) 0.001(3) C68 0.095(5) 0.052(4) 0.059(4) 0.000(3) 0.033(4) -0.006(4) C69 0.084(5) 0.046(4) 0.050(4) 0.000(3) 0.045(4) -0.003(4) Cl1 0.0966(16) 0.0875(14) 0.0769(13) -0.0153(11) 0.0473(12) -0.0130(12) Cl2 0.0797(12) 0.0473(9) 0.0562(10) 0.0009(7) 0.0264(9) -0.0137(8) Cl3 0.0932(14) 0.0335(8) 0.1127(15) 0.0082(8) 0.0765(12) 0.0029(8) Cl5 0.0844(12) 0.0516(9) 0.0490(9) 0.0005(7) 0.0317(8) -0.0028(9) O10 0.099(4) 0.065(3) 0.076(3) 0.004(3) 0.038(3) -0.021(3) O11 0.105(5) 0.176(8) 0.134(6) -0.027(6) -0.003(5) -0.028(5) O14 0.083(4) 0.056(3) 0.075(3) -0.017(2) 0.019(3) -0.004(3) O15 0.154(6) 0.110(5) 0.068(3) -0.035(3) 0.056(4) -0.043(4) O16 0.095(4) 0.087(4) 0.093(4) 0.032(3) 0.043(3) -0.009(3) O17 0.101(4) 0.068(4) 0.147(6) 0.011(4) -0.005(4) -0.002(3) Cl4 0.0889(12) 0.0397(8) 0.0536(9) -0.0015(7) 0.0419(9) -0.0061(8) O22 0.088(3) 0.051(3) 0.056(3) 0.008(2) 0.041(2) -0.002(2) O23 0.117(4) 0.044(3) 0.064(3) -0.008(2) 0.049(3) -0.015(3) O24 0.106(4) 0.057(3) 0.065(3) 0.001(2) 0.030(3) 0.013(3) O25 0.097(4) 0.045(2) 0.070(3) -0.004(2) 0.052(3) -0.014(2) O28 0.089(4) 0.104(4) 0.066(3) 0.020(3) 0.026(3) -0.014(3) O1W 0.107(4) 0.039(2) 0.079(3) 0.008(2) 0.059(3) 0.010(2) N2S 0.085(6) 0.056(5) 0.054(5) 0.000 0.036(5) 0.000 O3S 0.133(5) 0.082(4) 0.064(3) 0.005(3) 0.009(3) 0.020(4) C2S 0.118(10) 0.043(6) 0.076(7) 0.000 0.046(7) 0.000 Cl6 0.202(4) 0.224(5) 0.122(3) -0.033(3) -0.008(3) 0.075(4) O30 0.338(18) 0.35(2) 0.251(14) -0.174(15) 0.040(13) 0.009(16) O33 0.75(4) 0.230(15) 0.110(9) 0.019(9) 0.074(15) 0.03(2) O32 0.118(7) 0.272(13) 0.140(8) -0.064(7) -0.043(6) 0.060(7) O31 0.41(2) 0.236(14) 0.187(11) 0.020(10) -0.068(12) 0.169(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 La1 O2 2.443(6) . ? La1 O4 2.471(4) . ? La1 O18 2.529(7) . ? La1 O6 2.555(5) . ? La1 O18' 2.568(7) . ? La1 O22 2.617(5) . ? La1 N15 2.654(5) . ? La1 N7 2.670(6) . ? La1 N6 2.721(5) . ? La1 N14 2.737(4) . ? La2 O1 2.422(5) . ? La2 O3 2.451(4) . ? La2 O14 2.538(5) . ? La2 O5 2.548(5) . ? La2 O10 2.605(5) . ? La2 N3 2.683(5) . ? La2 N10 2.683(5) . ? La2 N2 2.687(6) . ? La2 N11 2.722(5) . ? O1 C16 1.279(8) . ? O2 C30 1.253(9) . ? O3 C50 1.252(8) . ? O4 C64 1.262(6) . ? N1 C16 1.320(8) . ? N1 C17 1.464(9) . ? N1 C19 1.510(8) . ? N2 C11 1.328(8) . ? N2 C15 1.391(9) . ? N3 C10 1.338(9) . ? N3 N4 1.367(7) . ? N4 C8 1.358(8) . ? N4 C7 1.410(9) . ? N5 C22 1.350(8) . ? N5 N6 1.341(8) . ? N5 C21 1.498(9) . ? N6 C24 1.339(8) . ? N7 C25 1.335(8) . ? N7 C29 1.341(9) . ? N8 C30 1.305(9) . ? N8 C33 1.435(10) . ? N8 C31 1.506(11) . ? N9 C50 1.311(8) . ? N9 C51 1.480(9) . ? N9 C53 1.544(10) . ? N10 C45 1.339(7) . ? N10 C49 1.342(7) . ? N11 N12 1.359(6) . ? N11 C44 1.348(8) . ? N12 C42 1.361(7) . ? N12 C41 1.452(8) . ? N13 C56 1.327(7) . ? N13 N14 1.338(6) . ? N13 C55 1.496(7) . ? N14 C58 1.354(7) . ? N15 C63 1.337(7) . ? N15 C59 1.358(7) . ? N16 C64 1.322(7) . ? N16 C65 1.468(7) . ? N16 C67 1.480(7) . ? C1 C6 1.344(10) . ? C1 C2 1.392(9) . ? C1 H1 0.9300 . ? C2 C69 1.359(10) . ? C2 H2 0.9300 . ? C4 C5 1.362(10) . ? C4 C69 1.394(10) . ? C4 H4 0.9300 . ? C5 C6 1.378(11) . ? C5 H5 0.9300 . ? C6 C7 1.527(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.377(11) . ? C8 H8 0.9300 . ? C9 C10 1.410(9) . ? C9 H9 0.9300 . ? C10 C11 1.483(10) . ? C11 C12 1.372(11) . ? C12 C13 1.338(11) . ? C12 H12 0.9300 . ? C13 C14 1.422(10) . ? C13 H13 0.9300 . ? C14 C15 1.384(10) . ? C14 H14 0.9300 . ? C15 C16 1.476(9) . ? C17 C18 1.510(11) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.485(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C69 1.510(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.370(10) . ? C22 H22 0.9300 . ? C23 C24 1.391(8) . ? C23 H23 0.9300 . ? C24 C25 1.447(10) . ? C25 C26 1.407(9) . ? C26 C27 1.386(11) . ? C26 H26 0.9300 . ? C27 C28 1.380(10) . ? C27 H27 0.9300 . ? C28 C29 1.391(11) . ? C28 H28 0.9300 . ? C29 C30 1.487(9) . ? C31 C32 1.467(14) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.540(12) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.350(9) . ? C35 C40 1.378(9) . ? C35 H35 0.9300 . ? C36 C37 1.393(9) . ? C36 H36 0.9300 . ? C37 C38 1.389(8) . ? C37 C55 1.491(10) . ? C38 C39 1.385(9) . ? C38 H38 0.9300 . ? C39 C40 1.367(9) . ? C39 H39 0.9300 . ? C40 C41 1.504(10) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.336(9) . ? C42 H42 0.9300 . ? C43 C44 1.408(8) . ? C43 H43 0.9300 . ? C44 C45 1.455(8) . ? C45 C46 1.387(9) . ? C46 C47 1.371(9) . ? C46 H46 0.9300 . ? C47 C48 1.390(9) . ? C47 H47 0.9300 . ? C48 C49 1.368(9) . ? C48 H48 0.9300 . ? C49 C50 1.493(8) . ? C51 C52 1.498(10) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.453(12) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.359(9) . ? C56 H56 0.9300 . ? C57 C58 1.398(8) . ? C57 H57 0.9300 . ? C58 C59 1.457(8) . ? C59 C60 1.388(8) . ? C60 C61 1.375(9) . ? C60 H60 0.9300 . ? C61 C62 1.367(8) . ? C61 H61 0.9300 . ? C62 C63 1.415(7) . ? C62 H62 0.9300 . ? C63 C64 1.490(8) . ? C65 C66 1.515(8) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 C68 1.478(9) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? Cl1 O11 1.424(7) . ? Cl1 O12' 1.423(9) . ? Cl1 O10 1.432(5) . ? Cl1 O13 1.443(11) . ? Cl1 O13' 1.491(9) . ? Cl1 O12 1.519(10) . ? Cl2 O16 1.391(5) . ? Cl2 O17 1.409(6) . ? Cl2 O15 1.426(5) . ? Cl2 O14 1.457(5) . ? Cl3 O20' 1.397(9) . ? Cl3 O19 1.417(8) . ? Cl3 O20 1.420(9) . ? Cl3 O21 1.439(8) . ? Cl3 O21' 1.447(9) . ? Cl3 O18 1.443(7) . ? Cl3 O19' 1.464(9) . ? Cl3 O18' 1.515(7) . ? Cl5 O29 1.380(13) . ? Cl5 O26 1.409(13) . ? Cl5 O27' 1.398(7) . ? Cl5 O28 1.419(5) . ? Cl5 O26' 1.463(7) . ? Cl5 O29' 1.465(6) . ? Cl5 O27 1.502(14) . ? Cl4 O24 1.412(5) . ? Cl4 O23 1.429(5) . ? Cl4 O25 1.432(4) . ? Cl4 O22 1.464(5) . ? O2S N1S 1.295(11) . ? O1S N1S 1.251(11) . ? N1S C1S 1.349(15) . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? N2S O3S 1.219(6) . ? N2S O3S 1.219(6) 2_655 ? N2S C2S 1.437(12) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? O5S N3S 1.215(10) . ? N3S O4S 1.252(11) . ? N3S C3S 1.346(14) . ? C3S H3S1 0.9600 . ? C3S H3S2 0.9600 . ? C3S H3S3 0.9600 . ? Cl6 O33 1.461(10) . ? Cl6 O32 1.522(8) . ? Cl6 O31 1.509(9) . ? Cl6 O30 1.533(10) . ? 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 La1 O4 84.49(16) . . ? O2 La1 O18 72.1(3) . . ? O4 La1 O18 136.5(2) . . ? O2 La1 O6 132.38(16) . . ? O4 La1 O6 143.02(15) . . ? O18 La1 O6 70.8(2) . . ? O2 La1 O18' 85.2(3) . . ? O4 La1 O18' 140.6(2) . . ? O18 La1 O18' 13.1(2) . . ? O6 La1 O18' 60.2(2) . . ? O2 La1 O22 147.44(15) . . ? O4 La1 O22 69.53(15) . . ? O18 La1 O22 140.4(2) . . ? O6 La1 O22 74.80(14) . . ? O18' La1 O22 127.4(2) . . ? O2 La1 N15 77.74(17) . . ? O4 La1 N15 61.00(13) . . ? O18 La1 N15 141.5(2) . . ? O6 La1 N15 116.87(15) . . ? O18' La1 N15 151.2(2) . . ? O22 La1 N15 72.67(14) . . ? O2 La1 N7 61.56(18) . . ? O4 La1 N7 65.65(14) . . ? O18 La1 N7 70.9(2) . . ? O6 La1 N7 128.71(15) . . ? O18' La1 N7 76.0(2) . . ? O22 La1 N7 119.85(15) . . ? N15 La1 N7 114.37(16) . . ? O2 La1 N6 122.54(17) . . ? O4 La1 N6 76.24(13) . . ? O18 La1 N6 86.0(2) . . ? O6 La1 N6 83.36(15) . . ? O18' La1 N6 77.7(2) . . ? O22 La1 N6 70.99(14) . . ? N15 La1 N6 131.15(14) . . ? N7 La1 N6 61.13(18) . . ? O2 La1 N14 70.06(17) . . ? O4 La1 N14 120.63(13) . . ? O18 La1 N14 85.6(2) . . ? O6 La1 N14 78.27(15) . . ? O18' La1 N14 90.9(2) . . ? O22 La1 N14 106.12(14) . . ? N15 La1 N14 61.56(14) . . ? N7 La1 N14 130.54(18) . . ? N6 La1 N14 161.45(16) . . ? O1 La2 O3 91.11(16) . . ? O1 La2 O14 138.02(15) . . ? O3 La2 O14 77.23(17) . . ? O1 La2 O5 139.55(15) . . ? O3 La2 O5 129.27(15) . . ? O14 La2 O5 65.85(16) . . ? O1 La2 O10 72.54(16) . . ? O3 La2 O10 146.78(17) . . ? O14 La2 O10 133.85(16) . . ? O5 La2 O10 70.93(16) . . ? O1 La2 N3 120.57(17) . . ? O3 La2 N3 65.96(14) . . ? O14 La2 N3 91.47(17) . . ? O5 La2 N3 80.98(14) . . ? O10 La2 N3 97.19(16) . . ? O1 La2 N10 66.34(16) . . ? O3 La2 N10 61.54(14) . . ? O14 La2 N10 72.77(15) . . ? O5 La2 N10 130.31(16) . . ? O10 La2 N10 130.26(16) . . ? N3 La2 N10 127.25(14) . . ? O1 La2 N2 60.64(16) . . ? O3 La2 N2 75.51(16) . . ? O14 La2 N2 147.15(16) . . ? O5 La2 N2 120.77(16) . . ? O10 La2 N2 71.27(16) . . ? N3 La2 N2 60.71(18) . . ? N10 La2 N2 108.92(16) . . ? O1 La2 N11 69.98(16) . . ? O3 La2 N11 122.66(14) . . ? O14 La2 N11 82.67(16) . . ? O5 La2 N11 86.72(15) . . ? O10 La2 N11 79.44(15) . . ? N3 La2 N11 167.67(16) . . ? N10 La2 N11 61.27(14) . . ? N2 La2 N11 127.90(17) . . ? C16 O1 La2 126.5(4) . . ? C30 O2 La1 126.3(4) . . ? C50 O3 La2 124.1(4) . . ? C64 O4 La1 120.8(4) . . ? C16 N1 C17 127.7(6) . . ? C16 N1 C19 117.3(6) . . ? C17 N1 C19 114.7(5) . . ? C11 N2 C15 117.8(6) . . ? C11 N2 La2 123.6(5) . . ? C15 N2 La2 118.2(4) . . ? C10 N3 N4 105.2(5) . . ? C10 N3 La2 120.5(4) . . ? N4 N3 La2 133.4(4) . . ? C8 N4 N3 110.0(6) . . ? C8 N4 C7 127.9(6) . . ? N3 N4 C7 122.1(5) . . ? C22 N5 N6 112.6(6) . . ? C22 N5 C21 125.0(6) . . ? N6 N5 C21 122.2(5) . . ? C24 N6 N5 104.5(5) . . ? C24 N6 La1 117.4(4) . . ? N5 N6 La1 136.6(4) . . ? C25 N7 C29 120.9(6) . . ? C25 N7 La1 118.6(5) . . ? C29 N7 La1 116.6(4) . . ? C30 N8 C33 128.2(6) . . ? C30 N8 C31 117.9(7) . . ? C33 N8 C31 113.3(7) . . ? C50 N9 C51 125.0(6) . . ? C50 N9 C53 117.1(6) . . ? C51 N9 C53 115.7(6) . . ? C45 N10 C49 121.0(5) . . ? C45 N10 La2 118.1(3) . . ? C49 N10 La2 116.6(4) . . ? N12 N11 C44 105.3(5) . . ? N12 N11 La2 135.8(4) . . ? C44 N11 La2 116.6(4) . . ? N11 N12 C42 110.4(5) . . ? N11 N12 C41 121.3(5) . . ? C42 N12 C41 127.8(5) . . ? C56 N13 N14 112.9(5) . . ? C56 N13 C55 125.5(5) . . ? N14 N13 C55 121.6(5) . . ? N13 N14 C58 103.7(4) . . ? N13 N14 La1 136.3(3) . . ? C58 N14 La1 118.0(4) . . ? C63 N15 C59 118.9(5) . . ? C63 N15 La1 118.3(3) . . ? C59 N15 La1 122.6(4) . . ? C64 N16 C65 125.5(5) . . ? C64 N16 C67 118.3(5) . . ? C65 N16 C67 115.5(4) . . ? C6 C1 C2 121.9(7) . . ? C6 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C69 C2 C1 119.1(8) . . ? C69 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C5 C4 C69 119.8(8) . . ? C5 C4 H4 120.1 . . ? C69 C4 H4 120.1 . . ? C4 C5 C6 120.9(8) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 118.7(6) . . ? C1 C6 C7 119.1(7) . . ? C5 C6 C7 122.1(7) . . ? N4 C7 C6 115.1(7) . . ? N4 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? N4 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? N4 C8 C9 109.3(7) . . ? N4 C8 H8 125.3 . . ? C9 C8 H8 125.3 . . ? C8 C9 C10 103.1(7) . . ? C8 C9 H9 128.4 . . ? C10 C9 H9 128.4 . . ? N3 C10 C9 112.3(7) . . ? N3 C10 C11 120.2(5) . . ? C9 C10 C11 127.0(7) . . ? N2 C11 C12 123.4(7) . . ? N2 C11 C10 114.8(6) . . ? C12 C11 C10 121.8(6) . . ? C13 C12 C11 120.0(7) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.7(8) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 117.8(8) . . ? C15 C14 H14 121.1 . . ? C13 C14 H14 121.1 . . ? N2 C15 C14 121.3(6) . . ? N2 C15 C16 111.0(6) . . ? C14 C15 C16 127.5(7) . . ? O1 C16 N1 120.1(6) . . ? O1 C16 C15 116.0(6) . . ? N1 C16 C15 123.9(7) . . ? N1 C17 C18 111.7(6) . . ? N1 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N1 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N1 110.5(6) . . ? C20 C19 H19A 109.5 . . ? N1 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? N1 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 C69 111.5(6) . . ? N5 C21 H21A 109.3 . . ? C69 C21 H21A 109.3 . . ? N5 C21 H21B 109.3 . . ? C69 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? N5 C22 C23 106.4(6) . . ? N5 C22 H22 126.8 . . ? C23 C22 H22 126.8 . . ? C22 C23 C24 105.3(6) . . ? C22 C23 H23 127.4 . . ? C24 C23 H23 127.4 . . ? N6 C24 C23 111.2(6) . . ? N6 C24 C25 119.2(5) . . ? C23 C24 C25 129.6(6) . . ? N7 C25 C26 121.0(7) . . ? N7 C25 C24 118.6(6) . . ? C26 C25 C24 120.4(6) . . ? C27 C26 C25 117.8(7) . . ? C27 C26 H26 121.1 . . ? C25 C26 H26 121.1 . . ? C28 C27 C26 120.7(8) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 118.4(8) . . ? C27 C28 H28 120.8 . . ? C29 C28 H28 120.8 . . ? N7 C29 C28 121.2(6) . . ? N7 C29 C30 112.9(7) . . ? C28 C29 C30 125.8(8) . . ? O2 C30 N8 121.2(6) . . ? O2 C30 C29 115.5(7) . . ? N8 C30 C29 123.4(7) . . ? C32 C31 N8 110.1(8) . . ? C32 C31 H31A 109.6 . . ? N8 C31 H31A 109.6 . . ? C32 C31 H31B 109.6 . . ? N8 C31 H31B 109.6 . . ? H31A C31 H31B 108.2 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N8 C33 C34 115.4(8) . . ? N8 C33 H33A 108.4 . . ? C34 C33 H33A 108.4 . . ? N8 C33 H33B 108.4 . . ? C34 C33 H33B 108.4 . . ? H33A C33 H33B 107.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 122.3(6) . . ? C36 C35 H35 118.8 . . ? C40 C35 H35 118.8 . . ? C35 C36 C37 120.2(6) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C38 118.3(7) . . ? C36 C37 C55 123.3(6) . . ? C38 C37 C55 118.3(6) . . ? C39 C38 C37 119.9(7) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C40 C39 C38 121.3(6) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C35 117.9(7) . . ? C39 C40 C41 122.9(6) . . ? C35 C40 C41 119.2(6) . . ? N12 C41 C40 114.3(5) . . ? N12 C41 H41A 108.7 . . ? C40 C41 H41A 108.7 . . ? N12 C41 H41B 108.7 . . ? C40 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C43 C42 N12 108.4(5) . . ? C43 C42 H42 125.8 . . ? N12 C42 H42 125.8 . . ? C42 C43 C44 105.8(6) . . ? C42 C43 H43 127.1 . . ? C44 C43 H43 127.1 . . ? N11 C44 C43 110.0(5) . . ? N11 C44 C45 120.1(5) . . ? C43 C44 C45 129.8(6) . . ? N10 C45 C46 120.4(5) . . ? N10 C45 C44 117.5(5) . . ? C46 C45 C44 122.1(5) . . ? C47 C46 C45 119.0(6) . . ? C47 C46 H46 120.5 . . ? C45 C46 H46 120.5 . . ? C46 C47 C48 119.6(6) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C49 C48 C47 119.1(6) . . ? C49 C48 H48 120.5 . . ? C47 C48 H48 120.5 . . ? N10 C49 C48 120.7(6) . . ? N10 C49 C50 111.3(5) . . ? C48 C49 C50 127.5(6) . . ? O3 C50 N9 120.9(6) . . ? O3 C50 C49 115.6(5) . . ? N9 C50 C49 123.5(6) . . ? N9 C51 C52 111.0(6) . . ? N9 C51 H51A 109.4 . . ? C52 C51 H51A 109.4 . . ? N9 C51 H51B 109.4 . . ? C52 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 N9 113.3(8) . . ? C54 C53 H53A 108.9 . . ? N9 C53 H53A 108.9 . . ? C54 C53 H53B 108.9 . . ? N9 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C37 C55 N13 112.7(5) . . ? C37 C55 H55A 109.1 . . ? N13 C55 H55A 109.1 . . ? C37 C55 H55B 109.1 . . ? N13 C55 H55B 109.1 . . ? H55A C55 H55B 107.8 . . ? N13 C56 C57 108.0(5) . . ? N13 C56 H56 126.0 . . ? C57 C56 H56 126.0 . . ? C56 C57 C58 104.4(5) . . ? C56 C57 H57 127.8 . . ? C58 C57 H57 127.8 . . ? N14 C58 C57 111.0(5) . . ? N14 C58 C59 120.2(5) . . ? C57 C58 C59 128.8(6) . . ? N15 C59 C60 121.1(5) . . ? N15 C59 C58 117.1(5) . . ? C60 C59 C58 121.7(5) . . ? C61 C60 C59 119.8(5) . . ? C61 C60 H60 120.1 . . ? C59 C60 H60 120.1 . . ? C62 C61 C60 119.7(6) . . ? C62 C61 H61 120.1 . . ? C60 C61 H61 120.1 . . ? C61 C62 C63 118.3(5) . . ? C61 C62 H62 120.8 . . ? C63 C62 H62 120.8 . . ? N15 C63 C62 122.0(5) . . ? N15 C63 C64 112.2(5) . . ? C62 C63 C64 125.2(5) . . ? O4 C64 N16 118.3(5) . . ? O4 C64 C63 116.6(5) . . ? N16 C64 C63 125.0(5) . . ? N16 C65 C66 112.6(5) . . ? N16 C65 H65A 109.1 . . ? C66 C65 H65A 109.1 . . ? N16 C65 H65B 109.1 . . ? C66 C65 H65B 109.1 . . ? H65A C65 H65B 107.8 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C68 C67 N16 112.6(5) . . ? C68 C67 H67A 109.1 . . ? N16 C67 H67A 109.1 . . ? C68 C67 H67B 109.1 . . ? N16 C67 H67B 109.1 . . ? H67A C67 H67B 107.8 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C2 C69 C4 119.6(6) . . ? C2 C69 C21 122.9(7) . . ? C4 C69 C21 117.5(6) . . ? O11 Cl1 O12' 98.5(8) . . ? O11 Cl1 O10 109.7(5) . . ? O12' Cl1 O10 111.2(5) . . ? O11 Cl1 O13 104.6(7) . . ? O12' Cl1 O13 132.6(8) . . ? O10 Cl1 O13 99.1(7) . . ? O11 Cl1 O13' 113.5(6) . . ? O12' Cl1 O13' 106.1(6) . . ? O10 Cl1 O13' 116.4(6) . . ? O13 Cl1 O13' 26.5(7) . . ? O11 Cl1 O12 124.2(8) . . ? O12' Cl1 O12 26.5(5) . . ? O10 Cl1 O12 103.8(5) . . ? O13 Cl1 O12 112.7(8) . . ? O13' Cl1 O12 88.2(6) . . ? O16 Cl2 O17 110.5(4) . . ? O16 Cl2 O15 110.1(4) . . ? O17 Cl2 O15 112.0(4) . . ? O16 Cl2 O14 108.8(3) . . ? O17 Cl2 O14 108.3(3) . . ? O15 Cl2 O14 106.9(3) . . ? O20' Cl3 O19 138.6(7) . . ? O20' Cl3 O20 26.5(7) . . ? O19 Cl3 O20 114.7(6) . . ? O20' Cl3 O21 88.0(7) . . ? O19 Cl3 O21 108.3(6) . . ? O20 Cl3 O21 110.2(6) . . ? O20' Cl3 O21' 111.1(6) . . ? O19 Cl3 O21' 77.1(6) . . ? O20 Cl3 O21' 124.4(7) . . ? O21 Cl3 O21' 31.2(5) . . ? O20' Cl3 O18 96.7(6) . . ? O19 Cl3 O18 112.4(5) . . ? O20 Cl3 O18 102.3(6) . . ? O21 Cl3 O18 108.8(5) . . ? O21' Cl3 O18 123.8(6) . . ? O20' Cl3 O19' 110.5(6) . . ? O19 Cl3 O19' 35.9(5) . . ? O20 Cl3 O19' 84.0(6) . . ? O21 Cl3 O19' 140.1(6) . . ? O21' Cl3 O19' 109.8(6) . . ? O18 Cl3 O19' 103.9(5) . . ? O20' Cl3 O18' 116.0(6) . . ? O19 Cl3 O18' 100.1(5) . . ? O20 Cl3 O18' 124.8(6) . . ? O21 Cl3 O18' 96.5(5) . . ? O21' Cl3 O18' 103.6(5) . . ? O18 Cl3 O18' 22.6(4) . . ? O19' Cl3 O18' 105.5(5) . . ? O29 Cl5 O26 121.2(11) . . ? O29 Cl5 O27' 132.6(12) . . ? O26 Cl5 O27' 66.0(9) . . ? O29 Cl5 O28 96.8(11) . . ? O26 Cl5 O28 130.8(10) . . ? O27' Cl5 O28 111.6(4) . . ? O29 Cl5 O26' 98.6(9) . . ? O26 Cl5 O26' 43.3(9) . . ? O27' Cl5 O26' 108.2(4) . . ? O28 Cl5 O26' 106.0(4) . . ? O29 Cl5 O29' 24.6(11) . . ? O26 Cl5 O29' 113.9(10) . . ? O27' Cl5 O29' 108.1(4) . . ? O28 Cl5 O29' 113.1(4) . . ? O26' Cl5 O29' 109.7(4) . . ? O29 Cl5 O27 111.7(10) . . ? O26 Cl5 O27 107.4(10) . . ? O27' Cl5 O27 41.5(9) . . ? O28 Cl5 O27 82.6(11) . . ? O26' Cl5 O27 147.4(9) . . ? O29' Cl5 O27 94.6(10) . . ? Cl1 O10 La2 128.9(3) . . ? Cl2 O14 La2 150.8(3) . . ? Cl3 O18 La1 152.4(5) . . ? Cl3 O18' La1 141.2(5) . . ? O24 Cl4 O23 111.0(3) . . ? O24 Cl4 O25 111.3(3) . . ? O23 Cl4 O25 110.9(3) . . ? O24 Cl4 O22 107.1(3) . . ? O23 Cl4 O22 108.2(3) . . ? O25 Cl4 O22 108.2(3) . . ? Cl4 O22 La1 123.4(2) . . ? O1S N1S O2S 123.4(14) . . ? O1S N1S C1S 118.3(13) . . ? O2S N1S C1S 117.6(13) . . ? N1S C1S H1S1 109.5 . . ? N1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? N1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O3S N2S O3S 121.2(9) . 2_655 ? O3S N2S C2S 119.4(4) . . ? O3S N2S C2S 119.4(4) 2_655 . ? N2S C2S H2S1 109.5 . . ? N2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? N2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? O5S N3S O4S 116.0(11) . . ? O5S N3S C3S 128.8(12) . . ? O4S N3S C3S 115.2(12) . . ? N3S C3S H3S1 109.5 . . ? N3S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? N3S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? O33 Cl6 O32 112.7(6) . . ? O33 Cl6 O31 114.0(8) . . ? O32 Cl6 O31 104.7(7) . . ? O33 Cl6 O30 111.4(8) . . ? O32 Cl6 O30 107.2(6) . . ? O31 Cl6 O30 106.3(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 La2 O1 C16 95.7(5) . . . . ? O14 La2 O1 C16 167.8(5) . . . . ? O5 La2 O1 C16 -81.1(5) . . . . ? O10 La2 O1 C16 -54.8(5) . . . . ? N3 La2 O1 C16 33.2(5) . . . . ? N10 La2 O1 C16 153.8(5) . . . . ? N2 La2 O1 C16 23.1(5) . . . . ? N11 La2 O1 C16 -139.7(5) . . . . ? O4 La1 O2 C30 77.4(6) . . . . ? O18 La1 O2 C30 -65.4(6) . . . . ? O6 La1 O2 C30 -105.8(6) . . . . ? O18' La1 O2 C30 -64.5(6) . . . . ? O22 La1 O2 C30 113.9(6) . . . . ? N15 La1 O2 C30 138.9(6) . . . . ? N7 La1 O2 C30 12.2(5) . . . . ? N6 La1 O2 C30 7.6(6) . . . . ? N14 La1 O2 C30 -157.2(6) . . . . ? O1 La2 O3 C50 79.5(5) . . . . ? O14 La2 O3 C50 -59.8(5) . . . . ? O5 La2 O3 C50 -103.2(5) . . . . ? O10 La2 O3 C50 138.3(5) . . . . ? N3 La2 O3 C50 -157.3(6) . . . . ? N10 La2 O3 C50 17.3(5) . . . . ? N2 La2 O3 C50 138.7(6) . . . . ? N11 La2 O3 C50 12.7(6) . . . . ? O2 La1 O4 C64 108.0(5) . . . . ? O18 La1 O4 C64 164.6(5) . . . . ? O6 La1 O4 C64 -68.1(5) . . . . ? O18' La1 O4 C64 -176.5(5) . . . . ? O22 La1 O4 C64 -52.0(4) . . . . ? N15 La1 O4 C64 28.9(4) . . . . ? N7 La1 O4 C64 169.2(5) . . . . ? N6 La1 O4 C64 -126.6(5) . . . . ? N14 La1 O4 C64 45.0(5) . . . . ? O1 La2 N2 C11 164.9(5) . . . . ? O3 La2 N2 C11 65.2(5) . . . . ? O14 La2 N2 C11 30.4(6) . . . . ? O5 La2 N2 C11 -62.2(5) . . . . ? O10 La2 N2 C11 -115.1(5) . . . . ? N3 La2 N2 C11 -5.1(5) . . . . ? N10 La2 N2 C11 117.7(5) . . . . ? N11 La2 N2 C11 -174.4(4) . . . . ? O1 La2 N2 C15 -6.8(4) . . . . ? O3 La2 N2 C15 -106.5(5) . . . . ? O14 La2 N2 C15 -141.3(4) . . . . ? O5 La2 N2 C15 126.2(4) . . . . ? O10 La2 N2 C15 73.3(4) . . . . ? N3 La2 N2 C15 -176.7(5) . . . . ? N10 La2 N2 C15 -54.0(5) . . . . ? N11 La2 N2 C15 13.9(5) . . . . ? O1 La2 N3 C10 -7.4(5) . . . . ? O3 La2 N3 C10 -83.6(5) . . . . ? O14 La2 N3 C10 -158.9(5) . . . . ? O5 La2 N3 C10 135.8(5) . . . . ? O10 La2 N3 C10 66.5(5) . . . . ? N10 La2 N3 C10 -89.6(5) . . . . ? N2 La2 N3 C10 2.7(4) . . . . ? N11 La2 N3 C10 139.8(7) . . . . ? O1 La2 N3 N4 159.8(5) . . . . ? O3 La2 N3 N4 83.6(5) . . . . ? O14 La2 N3 N4 8.3(5) . . . . ? O5 La2 N3 N4 -57.0(5) . . . . ? O10 La2 N3 N4 -126.3(5) . . . . ? N10 La2 N3 N4 77.6(5) . . . . ? N2 La2 N3 N4 170.0(6) . . . . ? N11 La2 N3 N4 -53.0(10) . . . . ? C10 N3 N4 C8 -2.2(7) . . . . ? La2 N3 N4 C8 -170.8(5) . . . . ? C10 N3 N4 C7 179.6(6) . . . . ? La2 N3 N4 C7 11.0(9) . . . . ? C22 N5 N6 C24 0.5(6) . . . . ? C21 N5 N6 C24 -174.5(5) . . . . ? C22 N5 N6 La1 -164.6(4) . . . . ? C21 N5 N6 La1 20.4(8) . . . . ? O2 La1 N6 C24 20.3(5) . . . . ? O4 La1 N6 C24 -53.9(4) . . . . ? O18 La1 N6 C24 86.1(4) . . . . ? O6 La1 N6 C24 157.2(4) . . . . ? O18' La1 N6 C24 96.3(5) . . . . ? O22 La1 N6 C24 -126.6(4) . . . . ? N15 La1 N6 C24 -82.6(5) . . . . ? N7 La1 N6 C24 15.7(4) . . . . ? N14 La1 N6 C24 149.3(5) . . . . ? O2 La1 N6 N5 -176.1(5) . . . . ? O4 La1 N6 N5 109.8(5) . . . . ? O18 La1 N6 N5 -110.3(5) . . . . ? O6 La1 N6 N5 -39.1(5) . . . . ? O18' La1 N6 N5 -100.1(5) . . . . ? O22 La1 N6 N5 37.0(5) . . . . ? N15 La1 N6 N5 81.0(5) . . . . ? N7 La1 N6 N5 179.3(5) . . . . ? N14 La1 N6 N5 -47.0(8) . . . . ? O2 La1 N7 C25 164.8(5) . . . . ? O4 La1 N7 C25 67.6(4) . . . . ? O18 La1 N7 C25 -115.7(5) . . . . ? O6 La1 N7 C25 -71.9(4) . . . . ? O18' La1 N7 C25 -103.0(5) . . . . ? O22 La1 N7 C25 22.3(5) . . . . ? N15 La1 N7 C25 105.5(4) . . . . ? N6 La1 N7 C25 -19.6(4) . . . . ? N14 La1 N7 C25 178.1(4) . . . . ? O2 La1 N7 C29 6.7(4) . . . . ? O4 La1 N7 C29 -90.5(4) . . . . ? O18 La1 N7 C29 86.2(5) . . . . ? O6 La1 N7 C29 129.9(4) . . . . ? O18' La1 N7 C29 98.8(5) . . . . ? O22 La1 N7 C29 -135.9(4) . . . . ? N15 La1 N7 C29 -52.6(4) . . . . ? N6 La1 N7 C29 -177.7(5) . . . . ? N14 La1 N7 C29 19.9(5) . . . . ? O1 La2 N10 C45 56.9(5) . . . . ? O3 La2 N10 C45 162.1(5) . . . . ? O14 La2 N10 C45 -113.4(5) . . . . ? O5 La2 N10 C45 -78.9(5) . . . . ? O10 La2 N10 C45 20.1(5) . . . . ? N3 La2 N10 C45 168.3(4) . . . . ? N2 La2 N10 C45 101.2(5) . . . . ? N11 La2 N10 C45 -22.3(4) . . . . ? O1 La2 N10 C49 -99.9(5) . . . . ? O3 La2 N10 C49 5.2(4) . . . . ? O14 La2 N10 C49 89.8(5) . . . . ? O5 La2 N10 C49 124.2(4) . . . . ? O10 La2 N10 C49 -136.8(4) . . . . ? N3 La2 N10 C49 11.4(5) . . . . ? N2 La2 N10 C49 -55.7(5) . . . . ? N11 La2 N10 C49 -179.2(5) . . . . ? O1 La2 N11 N12 103.1(6) . . . . ? O3 La2 N11 N12 -178.9(5) . . . . ? O14 La2 N11 N12 -109.3(6) . . . . ? O5 La2 N11 N12 -43.2(6) . . . . ? O10 La2 N11 N12 28.0(6) . . . . ? N3 La2 N11 N12 -47.1(11) . . . . ? N10 La2 N11 N12 176.4(6) . . . . ? N2 La2 N11 N12 84.0(6) . . . . ? O1 La2 N11 C44 -56.3(5) . . . . ? O3 La2 N11 C44 21.6(5) . . . . ? O14 La2 N11 C44 91.3(5) . . . . ? O5 La2 N11 C44 157.4(5) . . . . ? O10 La2 N11 C44 -131.4(5) . . . . ? N3 La2 N11 C44 153.5(7) . . . . ? N10 La2 N11 C44 17.0(4) . . . . ? N2 La2 N11 C44 -75.4(5) . . . . ? C44 N11 N12 C42 -0.8(7) . . . . ? La2 N11 N12 C42 -161.8(5) . . . . ? C44 N11 N12 C41 -173.1(6) . . . . ? La2 N11 N12 C41 25.9(9) . . . . ? C56 N13 N14 C58 -2.0(8) . . . . ? C55 N13 N14 C58 -179.8(6) . . . . ? C56 N13 N14 La1 -164.4(5) . . . . ? C55 N13 N14 La1 17.8(10) . . . . ? O2 La1 N14 N13 80.2(7) . . . . ? O4 La1 N14 N13 150.8(6) . . . . ? O18 La1 N14 N13 7.7(7) . . . . ? O6 La1 N14 N13 -63.6(6) . . . . ? O18' La1 N14 N13 -4.3(7) . . . . ? O22 La1 N14 N13 -133.8(6) . . . . ? N15 La1 N14 N13 166.8(7) . . . . ? N7 La1 N14 N13 67.9(7) . . . . ? N6 La1 N14 N13 -55.6(9) . . . . ? O2 La1 N14 C58 -80.3(5) . . . . ? O4 La1 N14 C58 -9.8(6) . . . . ? O18 La1 N14 C58 -152.9(6) . . . . ? O6 La1 N14 C58 135.8(5) . . . . ? O18' La1 N14 C58 -164.9(6) . . . . ? O22 La1 N14 C58 65.6(5) . . . . ? N15 La1 N14 C58 6.2(5) . . . . ? N7 La1 N14 C58 -92.7(5) . . . . ? N6 La1 N14 C58 143.8(5) . . . . ? O2 La1 N15 C63 -105.0(5) . . . . ? O4 La1 N15 C63 -14.5(5) . . . . ? O18 La1 N15 C63 -143.9(5) . . . . ? O6 La1 N15 C63 123.5(5) . . . . ? O18' La1 N15 C63 -160.0(6) . . . . ? O22 La1 N15 C63 61.3(5) . . . . ? N7 La1 N15 C63 -54.3(5) . . . . ? N6 La1 N15 C63 17.8(6) . . . . ? N14 La1 N15 C63 -178.7(6) . . . . ? O2 La1 N15 C59 70.1(5) . . . . ? O4 La1 N15 C59 160.6(6) . . . . ? O18 La1 N15 C59 31.2(7) . . . . ? O6 La1 N15 C59 -61.4(6) . . . . ? O18' La1 N15 C59 15.1(8) . . . . ? O22 La1 N15 C59 -123.6(6) . . . . ? N7 La1 N15 C59 120.8(5) . . . . ? N6 La1 N15 C59 -167.1(5) . . . . ? N14 La1 N15 C59 -3.6(5) . . . . ? C6 C1 C2 C69 1.3(10) . . . . ? C69 C4 C5 C6 -0.5(11) . . . . ? C2 C1 C6 C5 0.4(10) . . . . ? C2 C1 C6 C7 179.3(6) . . . . ? C4 C5 C6 C1 -0.8(11) . . . . ? C4 C5 C6 C7 -179.7(6) . . . . ? C8 N4 C7 C6 -80.4(9) . . . . ? N3 N4 C7 C6 97.5(7) . . . . ? C1 C6 C7 N4 173.0(6) . . . . ? C5 C6 C7 N4 -8.1(9) . . . . ? N3 N4 C8 C9 2.9(9) . . . . ? C7 N4 C8 C9 -179.0(7) . . . . ? N4 C8 C9 C10 -2.3(9) . . . . ? N4 N3 C10 C9 0.7(8) . . . . ? La2 N3 C10 C9 171.1(5) . . . . ? N4 N3 C10 C11 -171.3(6) . . . . ? La2 N3 C10 C11 -0.8(8) . . . . ? C8 C9 C10 N3 1.0(9) . . . . ? C8 C9 C10 C11 172.3(7) . . . . ? C15 N2 C11 C12 0.0(10) . . . . ? La2 N2 C11 C12 -171.7(6) . . . . ? C15 N2 C11 C10 178.3(6) . . . . ? La2 N2 C11 C10 6.6(8) . . . . ? N3 C10 C11 N2 -3.7(9) . . . . ? C9 C10 C11 N2 -174.3(7) . . . . ? N3 C10 C11 C12 174.6(7) . . . . ? C9 C10 C11 C12 4.0(12) . . . . ? N2 C11 C12 C13 0.1(13) . . . . ? C10 C11 C12 C13 -178.1(8) . . . . ? C11 C12 C13 C14 1.5(13) . . . . ? C12 C13 C14 C15 -3.1(13) . . . . ? C11 N2 C15 C14 -1.8(10) . . . . ? La2 N2 C15 C14 170.4(5) . . . . ? C11 N2 C15 C16 -177.5(6) . . . . ? La2 N2 C15 C16 -5.3(7) . . . . ? C13 C14 C15 N2 3.3(11) . . . . ? C13 C14 C15 C16 178.3(7) . . . . ? La2 O1 C16 N1 146.4(5) . . . . ? La2 O1 C16 C15 -35.8(8) . . . . ? C17 N1 C16 O1 -173.3(6) . . . . ? C19 N1 C16 O1 0.0(10) . . . . ? C17 N1 C16 C15 9.0(11) . . . . ? C19 N1 C16 C15 -177.7(6) . . . . ? N2 C15 C16 O1 23.7(8) . . . . ? C14 C15 C16 O1 -151.6(7) . . . . ? N2 C15 C16 N1 -158.5(6) . . . . ? C14 C15 C16 N1 26.1(11) . . . . ? C16 N1 C17 C18 -106.7(8) . . . . ? C19 N1 C17 C18 79.9(8) . . . . ? C16 N1 C19 C20 -85.3(8) . . . . ? C17 N1 C19 C20 88.9(8) . . . . ? C22 N5 C21 C69 -85.5(8) . . . . ? N6 N5 C21 C69 88.9(7) . . . . ? N6 N5 C22 C23 -1.1(7) . . . . ? C21 N5 C22 C23 173.8(5) . . . . ? N5 C22 C23 C24 1.2(7) . . . . ? N5 N6 C24 C23 0.3(6) . . . . ? La1 N6 C24 C23 168.8(4) . . . . ? N5 N6 C24 C25 179.6(5) . . . . ? La1 N6 C24 C25 -11.9(7) . . . . ? C22 C23 C24 N6 -1.0(7) . . . . ? C22 C23 C24 C25 179.8(6) . . . . ? C29 N7 C25 C26 1.1(9) . . . . ? La1 N7 C25 C26 -156.2(5) . . . . ? C29 N7 C25 C24 180.0(5) . . . . ? La1 N7 C25 C24 22.8(7) . . . . ? N6 C24 C25 N7 -6.9(8) . . . . ? C23 C24 C25 N7 172.2(6) . . . . ? N6 C24 C25 C26 172.0(6) . . . . ? C23 C24 C25 C26 -8.8(10) . . . . ? N7 C25 C26 C27 0.8(10) . . . . ? C24 C25 C26 C27 -178.2(6) . . . . ? C25 C26 C27 C28 -1.4(11) . . . . ? C26 C27 C28 C29 0.3(12) . . . . ? C25 N7 C29 C28 -2.2(9) . . . . ? La1 N7 C29 C28 155.4(5) . . . . ? C25 N7 C29 C30 -178.3(5) . . . . ? La1 N7 C29 C30 -20.6(6) . . . . ? C27 C28 C29 N7 1.5(11) . . . . ? C27 C28 C29 C30 177.0(7) . . . . ? La1 O2 C30 N8 153.9(5) . . . . ? La1 O2 C30 C29 -27.7(9) . . . . ? C33 N8 C30 O2 -168.9(7) . . . . ? C31 N8 C30 O2 1.6(11) . . . . ? C33 N8 C30 C29 12.8(12) . . . . ? C31 N8 C30 C29 -176.7(7) . . . . ? N7 C29 C30 O2 30.7(8) . . . . ? C28 C29 C30 O2 -145.1(8) . . . . ? N7 C29 C30 N8 -150.9(7) . . . . ? C28 C29 C30 N8 33.3(11) . . . . ? C30 N8 C31 C32 -86.3(10) . . . . ? C33 N8 C31 C32 85.6(10) . . . . ? C30 N8 C33 C34 -112.4(10) . . . . ? C31 N8 C33 C34 76.8(10) . . . . ? C40 C35 C36 C37 0.2(9) . . . . ? C35 C36 C37 C38 0.8(9) . . . . ? C35 C36 C37 C55 -175.7(5) . . . . ? C36 C37 C38 C39 -2.5(9) . . . . ? C55 C37 C38 C39 174.2(5) . . . . ? C37 C38 C39 C40 3.2(9) . . . . ? C38 C39 C40 C35 -2.1(8) . . . . ? C38 C39 C40 C41 177.8(5) . . . . ? C36 C35 C40 C39 0.4(8) . . . . ? C36 C35 C40 C41 -179.6(5) . . . . ? N11 N12 C41 C40 83.4(7) . . . . ? C42 N12 C41 C40 -87.5(8) . . . . ? C39 C40 C41 N12 -4.8(8) . . . . ? C35 C40 C41 N12 175.2(5) . . . . ? N11 N12 C42 C43 1.5(8) . . . . ? C41 N12 C42 C43 173.2(6) . . . . ? N12 C42 C43 C44 -1.5(8) . . . . ? N12 N11 C44 C43 -0.2(7) . . . . ? La2 N11 C44 C43 165.1(4) . . . . ? N12 N11 C44 C45 -177.5(6) . . . . ? La2 N11 C44 C45 -12.2(8) . . . . ? C42 C43 C44 N11 1.1(8) . . . . ? C42 C43 C44 C45 178.0(7) . . . . ? C49 N10 C45 C46 4.7(10) . . . . ? La2 N10 C45 C46 -151.1(5) . . . . ? C49 N10 C45 C44 -177.9(6) . . . . ? La2 N10 C45 C44 26.3(7) . . . . ? N11 C44 C45 N10 -9.1(9) . . . . ? C43 C44 C45 N10 174.2(6) . . . . ? N11 C44 C45 C46 168.2(6) . . . . ? C43 C44 C45 C46 -8.5(11) . . . . ? N10 C45 C46 C47 -0.5(11) . . . . ? C44 C45 C46 C47 -177.8(6) . . . . ? C45 C46 C47 C48 -3.4(11) . . . . ? C46 C47 C48 C49 3.2(12) . . . . ? C45 N10 C49 C48 -5.0(10) . . . . ? La2 N10 C49 C48 151.2(6) . . . . ? C45 N10 C49 C50 -178.0(6) . . . . ? La2 N10 C49 C50 -21.8(7) . . . . ? C47 C48 C49 N10 0.9(11) . . . . ? C47 C48 C49 C50 172.8(7) . . . . ? La2 O3 C50 N9 144.0(5) . . . . ? La2 O3 C50 C49 -36.2(8) . . . . ? C51 N9 C50 O3 -168.8(6) . . . . ? C53 N9 C50 O3 -6.6(10) . . . . ? C51 N9 C50 C49 11.4(10) . . . . ? C53 N9 C50 C49 173.6(6) . . . . ? N10 C49 C50 O3 36.9(8) . . . . ? C48 C49 C50 O3 -135.5(8) . . . . ? N10 C49 C50 N9 -143.2(6) . . . . ? C48 C49 C50 N9 44.3(11) . . . . ? C50 N9 C51 C52 -120.9(7) . . . . ? C53 N9 C51 C52 76.7(8) . . . . ? C50 N9 C53 C54 78.9(10) . . . . ? C51 N9 C53 C54 -117.2(9) . . . . ? C36 C37 C55 N13 -31.1(8) . . . . ? C38 C37 C55 N13 152.4(5) . . . . ? C56 N13 C55 C37 -79.5(9) . . . . ? N14 N13 C55 C37 98.1(7) . . . . ? N14 N13 C56 C57 0.7(9) . . . . ? C55 N13 C56 C57 178.4(7) . . . . ? N13 C56 C57 C58 0.9(9) . . . . ? N13 N14 C58 C57 2.5(8) . . . . ? La1 N14 C58 C57 168.8(5) . . . . ? N13 N14 C58 C59 -175.0(6) . . . . ? La1 N14 C58 C59 -8.7(9) . . . . ? C56 C57 C58 N14 -2.2(9) . . . . ? C56 C57 C58 C59 175.1(8) . . . . ? C63 N15 C59 C60 -0.9(11) . . . . ? La1 N15 C59 C60 -176.0(6) . . . . ? C63 N15 C59 C58 176.1(6) . . . . ? La1 N15 C59 C58 1.0(9) . . . . ? N14 C58 C59 N15 5.3(10) . . . . ? C57 C58 C59 N15 -171.7(8) . . . . ? N14 C58 C59 C60 -177.7(7) . . . . ? C57 C58 C59 C60 5.3(13) . . . . ? N15 C59 C60 C61 1.7(12) . . . . ? C58 C59 C60 C61 -175.2(8) . . . . ? C59 C60 C61 C62 -0.3(13) . . . . ? C60 C61 C62 C63 -1.7(11) . . . . ? C59 N15 C63 C62 -1.2(10) . . . . ? La1 N15 C63 C62 174.1(5) . . . . ? C59 N15 C63 C64 -172.8(6) . . . . ? La1 N15 C63 C64 2.5(7) . . . . ? C61 C62 C63 N15 2.5(10) . . . . ? C61 C62 C63 C64 173.0(7) . . . . ? La1 O4 C64 N16 142.1(4) . . . . ? La1 O4 C64 C63 -40.6(7) . . . . ? C65 N16 C64 O4 -165.4(6) . . . . ? C67 N16 C64 O4 4.8(9) . . . . ? C65 N16 C64 C63 17.5(10) . . . . ? C67 N16 C64 C63 -172.3(6) . . . . ? N15 C63 C64 O4 23.1(9) . . . . ? C62 C63 C64 O4 -148.2(6) . . . . ? N15 C63 C64 N16 -159.8(6) . . . . ? C62 C63 C64 N16 28.9(11) . . . . ? C64 N16 C65 C66 -112.9(6) . . . . ? C67 N16 C65 C66 76.6(6) . . . . ? C64 N16 C67 C68 -87.9(7) . . . . ? C65 N16 C67 C68 83.3(6) . . . . ? C1 C2 C69 C4 -2.5(10) . . . . ? C1 C2 C69 C21 180.0(6) . . . . ? C5 C4 C69 C2 2.1(10) . . . . ? C5 C4 C69 C21 179.8(7) . . . . ? N5 C21 C69 C2 -27.5(9) . . . . ? N5 C21 C69 C4 154.9(6) . . . . ? O11 Cl1 O10 La2 -108.9(5) . . . . ? O12' Cl1 O10 La2 143.2(8) . . . . ? O13 Cl1 O10 La2 0.3(8) . . . . ? O13' Cl1 O10 La2 21.6(8) . . . . ? O12 Cl1 O10 La2 116.5(7) . . . . ? O1 La2 O10 Cl1 143.1(4) . . . . ? O3 La2 O10 Cl1 79.4(5) . . . . ? O14 La2 O10 Cl1 -75.8(4) . . . . ? O5 La2 O10 Cl1 -54.6(4) . . . . ? N3 La2 O10 Cl1 23.2(4) . . . . ? N10 La2 O10 Cl1 178.2(3) . . . . ? N2 La2 O10 Cl1 78.9(4) . . . . ? N11 La2 O10 Cl1 -144.8(4) . . . . ? O16 Cl2 O14 La2 -75.7(7) . . . . ? O17 Cl2 O14 La2 164.2(6) . . . . ? O15 Cl2 O14 La2 43.3(7) . . . . ? O1 La2 O14 Cl2 1.9(8) . . . . ? O3 La2 O14 Cl2 79.1(6) . . . . ? O5 La2 O14 Cl2 -136.6(7) . . . . ? O10 La2 O14 Cl2 -114.6(6) . . . . ? N3 La2 O14 Cl2 144.0(7) . . . . ? N10 La2 O14 Cl2 15.2(6) . . . . ? N2 La2 O14 Cl2 113.6(6) . . . . ? N11 La2 O14 Cl2 -46.9(6) . . . . ? O20' Cl3 O18 La1 -74.4(15) . . . . ? O19 Cl3 O18 La1 135.7(13) . . . . ? O20 Cl3 O18 La1 -100.7(15) . . . . ? O21 Cl3 O18 La1 15.8(16) . . . . ? O21' Cl3 O18 La1 46.6(17) . . . . ? O19' Cl3 O18 La1 172.5(14) . . . . ? O18' Cl3 O18 La1 75.6(17) . . . . ? O2 La1 O18 Cl3 100.8(13) . . . . ? O4 La1 O18 Cl3 39.9(15) . . . . ? O6 La1 O18 Cl3 -109.6(13) . . . . ? O18' La1 O18 Cl3 -75.2(16) . . . . ? O22 La1 O18 Cl3 -78.6(13) . . . . ? N15 La1 O18 Cl3 141.0(11) . . . . ? N7 La1 O18 Cl3 35.5(12) . . . . ? N6 La1 O18 Cl3 -25.3(13) . . . . ? N14 La1 O18 Cl3 171.3(13) . . . . ? O20' Cl3 O18' La1 -11.1(12) . . . . ? O19 Cl3 O18' La1 -170.2(9) . . . . ? O20 Cl3 O18' La1 -40.3(12) . . . . ? O21 Cl3 O18' La1 79.9(10) . . . . ? O21' Cl3 O18' La1 110.8(10) . . . . ? O18 Cl3 O18' La1 -44.7(11) . . . . ? O19' Cl3 O18' La1 -133.7(9) . . . . ? O2 La1 O18' Cl3 39.0(8) . . . . ? O4 La1 O18' Cl3 -36.3(10) . . . . ? O18 La1 O18' Cl3 42.8(11) . . . . ? O6 La1 O18' Cl3 -175.2(9) . . . . ? O22 La1 O18' Cl3 -139.9(7) . . . . ? N15 La1 O18' Cl3 92.5(8) . . . . ? N7 La1 O18' Cl3 -22.9(8) . . . . ? N6 La1 O18' Cl3 -85.8(8) . . . . ? N14 La1 O18' Cl3 108.9(8) . . . . ? O24 Cl4 O22 La1 124.9(3) . . . . ? O23 Cl4 O22 La1 5.2(4) . . . . ? O25 Cl4 O22 La1 -115.0(3) . . . . ? O2 La1 O22 Cl4 90.6(4) . . . . ? O4 La1 O22 Cl4 129.8(3) . . . . ? O18 La1 O22 Cl4 -90.4(4) . . . . ? O6 La1 O22 Cl4 -60.1(3) . . . . ? O18' La1 O22 Cl4 -91.4(3) . . . . ? N15 La1 O22 Cl4 65.0(3) . . . . ? N7 La1 O22 Cl4 173.6(3) . . . . ? N6 La1 O22 Cl4 -148.2(3) . . . . ? N14 La1 O22 Cl4 12.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.753 _refine_diff_density_min -1.074 _refine_diff_density_rms 0.107 #===END data_src0399 _database_code_depnum_ccdc_archive 'CCDC 630964' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H47 Cl3 La N9 O17' _chemical_formula_weight 1123.09 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' La La -0.2871 2.4523 '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 12.822(5) _cell_length_b 13.698(5) _cell_length_c 13.940(6) _cell_angle_alpha 87.044(15) _cell_angle_beta 74.85(2) _cell_angle_gamma 83.25(2) _cell_volume 2346.3(15) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1336 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 1.160 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8362 _exptl_absorpt_correction_T_max 0.9885 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21600 _diffrn_reflns_av_R_equivalents 0.1306 _diffrn_reflns_av_sigmaI/netI 0.1460 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 23.00 _reflns_number_total 6271 _reflns_number_gt 4242 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6271 _refine_ls_number_parameters 579 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2090 _refine_ls_R_factor_gt 0.1560 _refine_ls_wR_factor_ref 0.3951 _refine_ls_wR_factor_gt 0.3606 _refine_ls_goodness_of_fit_ref 1.376 _refine_ls_restrained_S_all 1.376 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.19650(9) 0.76915(9) 0.72048(9) 0.0536(6) Uani 1 1 d . . . Cl1 Cl -0.0974(4) 0.7074(4) 0.8483(4) 0.0600(15) Uani 1 1 d . . . Cl2 Cl 0.1352(4) 0.1720(4) 0.6643(5) 0.0677(16) Uani 1 1 d . . . Cl3 Cl 0.4618(5) 0.0292(5) 0.2237(5) 0.0851(19) Uani 1 1 d D . . O1 O 0.1474(10) 0.8794(10) 0.8611(11) 0.057(4) Uani 1 1 d . . . O2 O 0.3679(11) 0.7517(10) 0.7717(10) 0.059(4) Uani 1 1 d . . . O3 O 0.0057(11) 0.7139(10) 0.7761(10) 0.068(4) Uani 1 1 d . . . O4 O -0.0807(11) 0.6919(11) 0.9449(12) 0.071(4) Uani 1 1 d . . . O5 O -0.1636(15) 0.7965(14) 0.8419(13) 0.093(5) Uani 1 1 d . . . O6 O -0.1384(14) 0.6260(12) 0.8208(12) 0.085(5) Uani 1 1 d . . . O7 O 0.2087(14) 0.1294(14) 0.7168(13) 0.102(6) Uani 1 1 d . . . O8 O 0.1851(12) 0.2326(13) 0.5855(11) 0.081(5) Uani 1 1 d . . . O9 O 0.0965(18) 0.0979(14) 0.6178(17) 0.112(7) Uani 1 1 d . . . O10 O 0.0497(11) 0.2288(11) 0.7302(12) 0.078(5) Uani 1 1 d . . . O11 O 0.553(4) 0.002(4) 0.265(5) 0.103(9) Uiso 0.44(6) 1 d PDU A 1 O11' O 0.511(4) 0.033(3) 0.304(3) 0.102(9) Uiso 0.56(6) 1 d PDU A 2 O12 O 0.527(2) 0.0550(18) 0.1294(18) 0.145(9) Uani 1 1 d . A . O13 O 0.4193(15) -0.0597(12) 0.2229(14) 0.093(6) Uani 1 1 d . A . O14 O 0.374(2) 0.1090(16) 0.252(2) 0.156(10) Uani 1 1 d . A . O20 O 0.0583(14) 0.9020(12) 0.6654(13) 0.092(5) Uani 1 1 d . . . H2A H -0.0054 0.9024 0.6579 0.110 Uiso 1 1 d R . . H2B H 0.0531 0.9631 0.6507 0.110 Uiso 1 1 d R . . O21 O 0.2890(12) 0.9237(10) 0.6579(11) 0.072(4) Uani 1 1 d . . . H2D H 0.2415 0.9671 0.6899 0.087 Uiso 1 1 d R . . H2C H 0.3378 0.9451 0.6797 0.087 Uiso 1 1 d R . . N1 N 0.2283(11) 0.4917(13) 0.6863(12) 0.057(5) Uani 1 1 d . . . N2 N 0.2187(13) 0.5690(11) 0.7413(13) 0.055(4) Uani 1 1 d . . . N3 N 0.1690(13) 0.6949(14) 0.9029(11) 0.059(5) Uani 1 1 d . . . N4 N 0.2085(12) 0.9183(14) 0.9859(14) 0.066(6) Uani 1 1 d . . . N5 N 0.1168(14) 0.7356(12) 0.4846(12) 0.056(4) Uani 1 1 d . . . N6 N 0.1918(14) 0.7340(13) 0.5348(14) 0.065(5) Uani 1 1 d . . . N7 N 0.3822(11) 0.7359(12) 0.5805(12) 0.046(4) Uani 1 1 d . . . N8 N 0.5368(13) 0.6823(15) 0.7595(16) 0.070(5) Uani 1 1 d . . . C1 C 0.5659(19) 0.4694(16) 0.5569(18) 0.066(6) Uani 1 1 d . . . H1 H 0.6135 0.4486 0.5978 0.079 Uiso 1 1 calc R . . C2 C 0.4601(14) 0.4686(13) 0.5956(13) 0.046(5) Uani 1 1 d . . . H2 H 0.4334 0.4457 0.6620 0.055 Uiso 1 1 calc R . . C3 C 0.3895(13) 0.5009(13) 0.5398(15) 0.045(5) Uani 1 1 d . . . C4 C 0.2673(16) 0.5000(16) 0.5822(19) 0.070(7) Uani 1 1 d . . . H4A H 0.2309 0.5614 0.5598 0.084 Uiso 1 1 calc R . . H4B H 0.2445 0.4446 0.5526 0.084 Uiso 1 1 calc R . . C5 C 0.2044(18) 0.4094(16) 0.743(2) 0.073(7) Uani 1 1 d . . . H5 H 0.2072 0.3453 0.7188 0.088 Uiso 1 1 calc R . . C6 C 0.1763(17) 0.4348(16) 0.8385(17) 0.068(6) Uani 1 1 d . . . H6 H 0.1557 0.3922 0.8945 0.081 Uiso 1 1 calc R . . C7 C 0.1826(16) 0.5330(16) 0.8403(18) 0.070(7) Uani 1 1 d . . . C8 C 0.1608(17) 0.5970(15) 0.9177(16) 0.059(6) Uani 1 1 d . . . C9 C 0.1258(18) 0.5621(17) 1.0195(18) 0.070(7) Uani 1 1 d . . . H9 H 0.1147 0.4948 1.0324 0.085 Uiso 1 1 calc R . . C10 C 0.1088(15) 0.6220(17) 1.0956(17) 0.062(6) Uani 1 1 d . . . H10 H 0.0900 0.5968 1.1619 0.075 Uiso 1 1 calc R . . C11 C 0.1184(16) 0.7187(16) 1.0781(14) 0.058(6) Uani 1 1 d . . . H11 H 0.1023 0.7630 1.1316 0.070 Uiso 1 1 calc R . . C12 C 0.1529(16) 0.7527(15) 0.9789(17) 0.057(5) Uani 1 1 d . . . C13 C 0.1733(18) 0.8555(16) 0.9370(15) 0.060(6) Uani 1 1 d . . . C14 C 0.2155(18) 1.0202(17) 0.9425(17) 0.068(6) Uani 1 1 d . . . H14A H 0.2618 1.0541 0.9738 0.082 Uiso 1 1 calc R . . H14B H 0.2518 1.0158 0.8706 0.082 Uiso 1 1 calc R . . C15 C 0.109(2) 1.0807(19) 0.9551(18) 0.078(7) Uani 1 1 d . . . H15A H 0.0618 1.0471 0.9259 0.116 Uiso 1 1 calc R . . H15B H 0.1202 1.1448 0.9217 0.116 Uiso 1 1 calc R . . H15C H 0.0750 1.0902 1.0261 0.116 Uiso 1 1 calc R . . C16 C 0.2512(19) 0.8970(19) 1.0742(19) 0.075(7) Uani 1 1 d . . . H16A H 0.3252 0.9177 1.0602 0.090 Uiso 1 1 calc R . . H16B H 0.2567 0.8252 1.0879 0.090 Uiso 1 1 calc R . . C17 C 0.179(2) 0.9495(17) 1.166(2) 0.097(9) Uani 1 1 d . . . H17A H 0.1639 1.0192 1.1495 0.145 Uiso 1 1 calc R . . H17B H 0.2170 0.9433 1.2192 0.145 Uiso 1 1 calc R . . H17C H 0.1110 0.9197 1.1883 0.145 Uiso 1 1 calc R . . C18 C -0.0079(16) 0.4326(15) 0.5748(16) 0.056(5) Uani 1 1 d . . . H18 H -0.0147 0.3863 0.6286 0.067 Uiso 1 1 calc R . . C19 C -0.0049(16) 0.5294(17) 0.5920(15) 0.059(6) Uani 1 1 d . . . H19 H -0.0072 0.5490 0.6569 0.071 Uiso 1 1 calc R . . C20 C 0.0014(13) 0.5983(14) 0.5167(15) 0.044(5) Uani 1 1 d . . . C21 C 0.0066(16) 0.7056(14) 0.5347(15) 0.057(5) Uani 1 1 d . . . H21A H -0.0491 0.7470 0.5088 0.068 Uiso 1 1 calc R . . H21B H -0.0094 0.7162 0.6071 0.068 Uiso 1 1 calc R . . C22 C 0.1502(16) 0.7655(15) 0.3872(18) 0.064(6) Uani 1 1 d . . . H22 H 0.1078 0.7764 0.3403 0.077 Uiso 1 1 calc R . . C23 C 0.2602(17) 0.7766(19) 0.372(2) 0.079(7) Uani 1 1 d . . . H23 H 0.3101 0.7936 0.3117 0.094 Uiso 1 1 calc R . . C24 C 0.2793(16) 0.7578(14) 0.461(2) 0.064(6) Uani 1 1 d . . . C25 C 0.3837(14) 0.7601(16) 0.491(2) 0.063(6) Uani 1 1 d . . . C26 C 0.4709(16) 0.7986(15) 0.4175(17) 0.066(6) Uani 1 1 d . . . H26 H 0.4661 0.8196 0.3526 0.080 Uiso 1 1 calc R . . C27 C 0.5602(17) 0.8020(19) 0.4501(17) 0.073(7) Uani 1 1 d . . . H27 H 0.6210 0.8276 0.4059 0.088 Uiso 1 1 calc R . . C28 C 0.5698(16) 0.7693(19) 0.5473(15) 0.068(6) Uani 1 1 d . . . H28 H 0.6358 0.7672 0.5667 0.082 Uiso 1 1 calc R . . C29 C 0.4728(17) 0.7407(14) 0.6117(16) 0.058(6) Uani 1 1 d . . . C30 C 0.4617(19) 0.7243(14) 0.7183(14) 0.053(6) Uani 1 1 d . . . C31 C 0.6423(17) 0.6405(16) 0.7009(18) 0.068(6) Uani 1 1 d . . . H31A H 0.6971 0.6863 0.6990 0.081 Uiso 1 1 calc R . . H31B H 0.6388 0.6317 0.6318 0.081 Uiso 1 1 calc R . . C32 C 0.678(2) 0.5373(18) 0.747(2) 0.082(7) Uani 1 1 d . . . H32A H 0.6650 0.5426 0.8192 0.122 Uiso 1 1 calc R . . H32B H 0.7556 0.5183 0.7177 0.122 Uiso 1 1 calc R . . H32C H 0.6358 0.4873 0.7328 0.122 Uiso 1 1 calc R . . C33 C 0.514(2) 0.6832(16) 0.8715(17) 0.070(6) Uani 1 1 d . . . H33A H 0.5836 0.6801 0.8895 0.084 Uiso 1 1 calc R . . H33B H 0.4715 0.7467 0.8947 0.084 Uiso 1 1 calc R . . C34 C 0.456(2) 0.606(2) 0.923(2) 0.100(10) Uani 1 1 d . . . H34A H 0.3867 0.6075 0.9053 0.150 Uiso 1 1 calc R . . H34B H 0.4414 0.6155 0.9951 0.150 Uiso 1 1 calc R . . H34C H 0.4991 0.5431 0.9056 0.150 Uiso 1 1 calc R . . O1W O -0.146(2) 0.903(2) 0.640(2) 0.168(10) Uiso 1 1 d . . . H1B H -0.1340 0.9030 0.5773 0.201 Uiso 1 1 d R . . H1A H -0.2117 0.8991 0.6716 0.201 Uiso 1 1 d R . . N1S N 0.509(2) 0.337(2) 0.813(2) 0.119(8) Uiso 1 1 d . . . C1S C 0.465(3) 0.273(3) 0.864(3) 0.115(10) Uiso 1 1 d . . . C2S C 0.381(3) 0.208(3) 0.921(3) 0.134(12) Uiso 1 1 d . . . H2S1 H 0.4171 0.1531 0.9520 0.201 Uiso 1 1 calc R . . H2S2 H 0.3445 0.1835 0.8755 0.201 Uiso 1 1 calc R . . H2S3 H 0.3279 0.2469 0.9726 0.201 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 La1 0.0478(8) 0.0550(9) 0.0516(9) -0.0073(5) 0.0062(5) -0.0210(5) Cl1 0.052(3) 0.062(4) 0.061(4) -0.005(3) 0.002(2) -0.019(3) Cl2 0.051(3) 0.061(4) 0.084(4) -0.005(3) 0.000(3) -0.014(3) Cl3 0.081(4) 0.086(5) 0.090(5) 0.005(4) -0.019(4) -0.023(4) O1 0.056(8) 0.062(9) 0.045(9) -0.006(7) 0.010(7) -0.022(6) O2 0.063(9) 0.062(9) 0.045(8) -0.004(6) 0.008(7) -0.025(7) O3 0.060(8) 0.070(10) 0.066(10) -0.011(7) 0.012(7) -0.029(7) O4 0.051(8) 0.092(11) 0.073(11) -0.016(8) -0.003(7) -0.039(7) O5 0.089(12) 0.091(13) 0.088(13) 0.022(10) -0.014(10) -0.001(10) O6 0.104(12) 0.083(11) 0.077(11) -0.006(8) -0.011(9) -0.067(10) O7 0.085(12) 0.113(15) 0.078(12) 0.059(11) 0.009(9) 0.013(10) O8 0.067(9) 0.102(12) 0.062(10) 0.018(9) 0.005(8) -0.021(8) O9 0.138(17) 0.075(13) 0.137(17) 0.007(11) -0.048(14) -0.039(12) O10 0.051(8) 0.065(10) 0.100(12) -0.011(8) 0.002(8) 0.019(7) O12 0.18(2) 0.123(19) 0.115(19) 0.017(14) 0.000(17) -0.029(16) O13 0.111(13) 0.069(11) 0.113(14) 0.026(10) -0.041(11) -0.044(10) O14 0.15(2) 0.072(14) 0.22(3) -0.012(15) 0.002(19) -0.005(14) O20 0.081(11) 0.062(10) 0.117(15) -0.006(9) 0.006(10) -0.014(8) O21 0.070(9) 0.055(9) 0.086(11) -0.004(7) -0.001(8) -0.024(7) N1 0.036(8) 0.074(13) 0.050(11) -0.001(9) 0.017(7) -0.022(8) N2 0.061(10) 0.042(10) 0.062(12) -0.010(8) -0.012(9) -0.014(8) N3 0.054(10) 0.089(14) 0.023(9) -0.004(9) 0.009(7) -0.008(9) N4 0.035(8) 0.087(14) 0.068(13) -0.032(11) 0.015(8) -0.026(8) N5 0.061(10) 0.058(11) 0.045(11) -0.007(8) 0.003(9) -0.025(8) N6 0.059(11) 0.061(12) 0.074(13) -0.018(9) -0.009(10) -0.017(8) N7 0.031(8) 0.066(11) 0.046(11) -0.005(8) -0.007(7) -0.029(7) N8 0.034(9) 0.086(14) 0.092(16) -0.004(11) -0.015(10) -0.016(9) C1 0.071(15) 0.063(15) 0.068(16) 0.004(11) -0.031(13) 0.001(11) C2 0.045(11) 0.053(12) 0.034(11) -0.007(8) 0.006(9) -0.015(9) C3 0.030(9) 0.050(12) 0.066(14) -0.017(10) -0.027(10) -0.013(8) C4 0.050(12) 0.047(13) 0.11(2) -0.039(12) -0.015(12) -0.002(9) C5 0.072(14) 0.046(14) 0.088(19) -0.013(12) 0.008(13) -0.017(11) C6 0.072(14) 0.060(15) 0.066(16) 0.001(11) 0.004(12) -0.041(11) C7 0.052(12) 0.062(15) 0.078(17) -0.006(12) 0.022(11) -0.022(10) C8 0.067(13) 0.046(13) 0.062(15) -0.003(11) -0.005(11) -0.023(10) C9 0.080(15) 0.053(14) 0.066(16) 0.013(12) 0.010(12) -0.026(11) C10 0.044(11) 0.074(17) 0.065(15) 0.011(13) 0.000(10) -0.025(10) C11 0.069(13) 0.072(16) 0.026(11) 0.010(9) 0.003(9) -0.017(11) C12 0.059(12) 0.044(12) 0.073(17) 0.005(11) -0.026(11) -0.005(9) C13 0.083(15) 0.074(15) 0.010(11) 0.007(10) 0.016(10) -0.026(12) C14 0.062(14) 0.074(16) 0.065(15) -0.005(12) -0.001(11) -0.035(12) C15 0.088(18) 0.092(18) 0.063(16) -0.020(13) -0.022(13) -0.040(15) C16 0.066(14) 0.090(18) 0.084(18) -0.002(14) -0.035(14) -0.035(13) C17 0.12(2) 0.045(15) 0.11(2) 0.000(14) 0.000(17) -0.020(14) C18 0.059(12) 0.055(14) 0.051(14) -0.001(10) -0.004(10) -0.020(10) C19 0.061(13) 0.080(17) 0.042(13) -0.001(12) -0.015(10) -0.027(11) C20 0.030(9) 0.061(13) 0.053(13) -0.006(10) -0.025(8) -0.019(8) C21 0.060(12) 0.050(13) 0.052(13) 0.005(9) 0.001(10) -0.009(9) C22 0.053(12) 0.054(14) 0.087(18) -0.003(11) -0.025(12) 0.006(10) C23 0.047(13) 0.100(19) 0.10(2) 0.005(16) -0.017(13) -0.036(12) C24 0.042(11) 0.040(12) 0.098(19) 0.021(11) 0.000(12) -0.009(9) C25 0.029(10) 0.072(15) 0.086(19) -0.001(12) -0.011(10) -0.013(9) C26 0.050(12) 0.066(15) 0.065(15) 0.011(11) 0.019(11) -0.017(10) C27 0.044(12) 0.12(2) 0.056(15) 0.004(13) -0.007(10) -0.033(12) C28 0.036(10) 0.12(2) 0.042(13) 0.007(12) -0.001(9) -0.017(11) C29 0.066(13) 0.042(12) 0.060(14) -0.014(9) -0.002(11) -0.010(9) C30 0.083(16) 0.047(12) 0.032(12) 0.014(9) -0.005(11) -0.043(11) C31 0.064(13) 0.061(15) 0.082(17) 0.020(12) -0.025(12) -0.015(11) C32 0.069(15) 0.083(18) 0.090(19) -0.002(14) -0.016(13) -0.006(13) C33 0.098(17) 0.056(14) 0.061(16) 0.008(11) -0.031(13) -0.003(12) C34 0.079(17) 0.14(3) 0.09(2) 0.060(18) -0.031(15) -0.047(17) _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 La1 O1 2.440(14) . ? La1 O2 2.465(15) . ? La1 O21 2.550(13) . ? La1 O3 2.558(12) . ? La1 O20 2.617(19) . ? La1 N3 2.641(16) . ? La1 N7 2.663(14) . ? La1 N6 2.674(19) . ? La1 N2 2.732(16) . ? Cl1 O6 1.398(14) . ? Cl1 O5 1.414(18) . ? Cl1 O4 1.420(17) . ? Cl1 O3 1.446(13) . ? Cl2 O7 1.397(19) . ? Cl2 O8 1.403(15) . ? Cl2 O10 1.414(14) . ? Cl2 O9 1.431(19) . ? Cl3 O13 1.394(16) . ? Cl3 O12 1.41(2) . ? Cl3 O11' 1.42(3) . ? Cl3 O11 1.43(3) . ? Cl3 O14 1.46(2) . ? O1 C13 1.21(2) . ? O2 C30 1.26(3) . ? O20 H2A 0.8500 . ? O20 H2B 0.8501 . ? O21 H2D 0.8500 . ? O21 H2C 0.8501 . ? N1 N2 1.31(2) . ? N1 C5 1.36(3) . ? N1 C4 1.41(3) . ? N2 C7 1.42(3) . ? N3 C12 1.31(3) . ? N3 C8 1.36(3) . ? N4 C13 1.31(3) . ? N4 C16 1.48(3) . ? N4 C14 1.50(3) . ? N5 N6 1.33(2) . ? N5 C22 1.37(3) . ? N5 C21 1.50(2) . ? N6 C24 1.37(3) . ? N7 C25 1.28(3) . ? N7 C29 1.35(3) . ? N8 C30 1.31(3) . ? N8 C31 1.45(3) . ? N8 C33 1.51(3) . ? C1 C2 1.32(3) . ? C1 C3 1.38(3) 2_666 ? C1 H1 0.9500 . ? C2 C3 1.36(3) . ? C2 H2 0.9500 . ? C3 C1 1.38(3) 2_666 ? C3 C4 1.52(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.34(3) . ? C5 H5 0.9500 . ? C6 C7 1.36(3) . ? C6 H6 0.9500 . ? C7 C8 1.38(3) . ? C8 C9 1.45(3) . ? C9 C10 1.33(3) . ? C9 H9 0.9500 . ? C10 C11 1.35(3) . ? C10 H10 0.9500 . ? C11 C12 1.41(3) . ? C11 H11 0.9500 . ? C12 C13 1.52(3) . ? C14 C15 1.48(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.52(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.34(3) 2_566 ? C18 C19 1.37(3) . ? C18 H18 0.9500 . ? C19 C20 1.37(3) . ? C19 H19 0.9500 . ? C20 C18 1.34(3) 2_566 ? C20 C21 1.52(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.40(3) . ? C22 H22 0.9500 . ? C23 C24 1.34(3) . ? C23 H23 0.9500 . ? C24 C25 1.50(3) . ? C25 C26 1.43(3) . ? C26 C27 1.34(3) . ? C26 H26 0.9500 . ? C27 C28 1.44(3) . ? C27 H27 0.9500 . ? C28 C29 1.42(3) . ? C28 H28 0.9500 . ? C29 C30 1.46(3) . ? C31 C32 1.59(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.42(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O1W H1B 0.8494 . ? O1W H1A 0.8500 . ? N1S C1S 1.20(4) . ? C1S C2S 1.50(5) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 La1 O2 79.4(5) . . ? O1 La1 O21 74.2(4) . . ? O2 La1 O21 73.4(5) . . ? O1 La1 O3 88.7(4) . . ? O2 La1 O3 139.8(5) . . ? O21 La1 O3 139.7(5) . . ? O1 La1 O20 78.7(6) . . ? O2 La1 O20 141.6(5) . . ? O21 La1 O20 70.5(5) . . ? O3 La1 O20 70.5(5) . . ? O1 La1 N3 60.4(5) . . ? O2 La1 N3 68.8(5) . . ? O21 La1 N3 124.6(5) . . ? O3 La1 N3 72.0(5) . . ? O20 La1 N3 124.1(5) . . ? O1 La1 N7 130.4(4) . . ? O2 La1 N7 61.9(5) . . ? O21 La1 N7 66.1(5) . . ? O3 La1 N7 140.9(4) . . ? O20 La1 N7 112.6(5) . . ? N3 La1 N7 122.7(5) . . ? O1 La1 N6 149.0(6) . . ? O2 La1 N6 121.8(5) . . ? O21 La1 N6 89.7(5) . . ? O3 La1 N6 86.9(5) . . ? O20 La1 N6 70.9(6) . . ? N3 La1 N6 144.8(6) . . ? N7 La1 N6 60.4(5) . . ? O1 La1 N2 123.3(5) . . ? O2 La1 N2 82.4(5) . . ? O21 La1 N2 147.1(5) . . ? O3 La1 N2 72.3(5) . . ? O20 La1 N2 136.0(5) . . ? N3 La1 N2 62.9(5) . . ? N7 La1 N2 83.0(5) . . ? N6 La1 N2 84.3(5) . . ? O6 Cl1 O5 112.8(12) . . ? O6 Cl1 O4 110.2(9) . . ? O5 Cl1 O4 111.3(10) . . ? O6 Cl1 O3 105.1(9) . . ? O5 Cl1 O3 107.5(10) . . ? O4 Cl1 O3 109.7(9) . . ? O7 Cl2 O8 111.6(10) . . ? O7 Cl2 O10 108.8(11) . . ? O8 Cl2 O10 109.1(10) . . ? O7 Cl2 O9 110.5(13) . . ? O8 Cl2 O9 104.7(12) . . ? O10 Cl2 O9 112.1(12) . . ? O13 Cl3 O12 112.3(14) . . ? O13 Cl3 O11' 112.1(18) . . ? O12 Cl3 O11' 115(2) . . ? O13 Cl3 O11 103(2) . . ? O12 Cl3 O11 94(3) . . ? O11' Cl3 O11 30(2) . . ? O13 Cl3 O14 110.5(13) . . ? O12 Cl3 O14 107.2(16) . . ? O11' Cl3 O14 99(3) . . ? O11 Cl3 O14 128(3) . . ? C13 O1 La1 120.6(14) . . ? C30 O2 La1 126.7(13) . . ? Cl1 O3 La1 152.2(9) . . ? La1 O20 H2A 134.7 . . ? La1 O20 H2B 138.5 . . ? H2A O20 H2B 86.7 . . ? La1 O21 H2D 100.1 . . ? La1 O21 H2C 125.8 . . ? H2D O21 H2C 90.6 . . ? N2 N1 C5 111.8(18) . . ? N2 N1 C4 119.8(16) . . ? C5 N1 C4 128.3(19) . . ? N1 N2 C7 104.3(15) . . ? N1 N2 La1 138.4(13) . . ? C7 N2 La1 114.7(12) . . ? C12 N3 C8 120.4(17) . . ? C12 N3 La1 120.7(14) . . ? C8 N3 La1 118.6(13) . . ? C13 N4 C16 127(2) . . ? C13 N4 C14 117(2) . . ? C16 N4 C14 116.2(17) . . ? N6 N5 C22 114.4(16) . . ? N6 N5 C21 120.2(16) . . ? C22 N5 C21 125.4(19) . . ? N5 N6 C24 101.1(19) . . ? N5 N6 La1 136.9(12) . . ? C24 N6 La1 116.0(16) . . ? C25 N7 C29 118.8(15) . . ? C25 N7 La1 118.8(12) . . ? C29 N7 La1 114.7(12) . . ? C30 N8 C31 122(2) . . ? C30 N8 C33 117.9(18) . . ? C31 N8 C33 119.9(19) . . ? C2 C1 C3 123(2) . 2_666 ? C2 C1 H1 118.4 . . ? C3 C1 H1 118.4 2_666 . ? C1 C2 C3 119.7(18) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C1 117.0(16) . 2_666 ? C2 C3 C4 120.8(19) . . ? C1 C3 C4 122.2(19) 2_666 . ? N1 C4 C3 117.4(19) . . ? N1 C4 H4A 107.9 . . ? C3 C4 H4A 107.9 . . ? N1 C4 H4B 107.9 . . ? C3 C4 H4B 107.9 . . ? H4A C4 H4B 107.2 . . ? C6 C5 N1 107.9(19) . . ? C6 C5 H5 126.1 . . ? N1 C5 H5 126.1 . . ? C5 C6 C7 107(2) . . ? C5 C6 H6 126.4 . . ? C7 C6 H6 126.4 . . ? C6 C7 C8 132(2) . . ? C6 C7 N2 108.8(19) . . ? C8 C7 N2 119.5(18) . . ? N3 C8 C7 122.3(19) . . ? N3 C8 C9 117.0(18) . . ? C7 C8 C9 121(2) . . ? C10 C9 C8 122(2) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 120(2) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 119(2) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? N3 C12 C11 122.4(19) . . ? N3 C12 C13 107.1(19) . . ? C11 C12 C13 130(2) . . ? O1 C13 N4 121(2) . . ? O1 C13 C12 117(2) . . ? N4 C13 C12 121(2) . . ? C15 C14 N4 114.4(17) . . ? C15 C14 H14A 108.7 . . ? N4 C14 H14A 108.7 . . ? C15 C14 H14B 108.7 . . ? N4 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C17 112(2) . . ? N4 C16 H16A 109.2 . . ? C17 C16 H16A 109.1 . . ? N4 C16 H16B 109.1 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C19 121.3(19) 2_566 . ? C20 C18 H18 119.4 2_566 . ? C19 C18 H18 119.4 . . ? C18 C19 C20 120.7(19) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C18 C20 C19 118.0(18) 2_566 . ? C18 C20 C21 120.9(18) 2_566 . ? C19 C20 C21 121.0(18) . . ? N5 C21 C20 110.7(15) . . ? N5 C21 H21A 109.5 . . ? C20 C21 H21A 109.5 . . ? N5 C21 H21B 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? N5 C22 C23 105(2) . . ? N5 C22 H22 127.5 . . ? C23 C22 H22 127.5 . . ? C24 C23 C22 104(2) . . ? C24 C23 H23 127.9 . . ? C22 C23 H23 127.9 . . ? C23 C24 N6 115(2) . . ? C23 C24 C25 128.4(18) . . ? N6 C24 C25 116(2) . . ? N7 C25 C26 127(2) . . ? N7 C25 C24 116.5(17) . . ? C26 C25 C24 116(2) . . ? C27 C26 C25 113(2) . . ? C27 C26 H26 123.5 . . ? C25 C26 H26 123.5 . . ? C26 C27 C28 124.4(18) . . ? C26 C27 H27 117.8 . . ? C28 C27 H27 117.8 . . ? C29 C28 C27 114.3(19) . . ? C29 C28 H28 122.8 . . ? C27 C28 H28 122.8 . . ? N7 C29 C28 122(2) . . ? N7 C29 C30 116.1(18) . . ? C28 C29 C30 121(2) . . ? O2 C30 N8 120.0(17) . . ? O2 C30 C29 114(2) . . ? N8 C30 C29 126(2) . . ? N8 C31 C32 110.7(18) . . ? N8 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? N8 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N8 116(2) . . ? C34 C33 H33A 108.3 . . ? N8 C33 H33A 108.3 . . ? C34 C33 H33B 108.3 . . ? N8 C33 H33B 108.3 . . ? H33A C33 H33B 107.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? H1B O1W H1A 114.5 . . ? N1S C1S C2S 163(4) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 La1 O1 C13 -43.3(13) . . . . ? O21 La1 O1 C13 -118.8(14) . . . . ? O3 La1 O1 C13 98.1(14) . . . . ? O20 La1 O1 C13 168.5(14) . . . . ? N3 La1 O1 C13 28.2(13) . . . . ? N7 La1 O1 C13 -81.2(15) . . . . ? N6 La1 O1 C13 179.9(13) . . . . ? N2 La1 O1 C13 30.3(15) . . . . ? O1 La1 O2 C30 -157.1(15) . . . . ? O21 La1 O2 C30 -80.5(14) . . . . ? O3 La1 O2 C30 127.8(14) . . . . ? O20 La1 O2 C30 -100.8(15) . . . . ? N3 La1 O2 C30 140.7(15) . . . . ? N7 La1 O2 C30 -9.2(13) . . . . ? N6 La1 O2 C30 -1.6(16) . . . . ? N2 La1 O2 C30 76.9(14) . . . . ? O6 Cl1 O3 La1 -157(2) . . . . ? O5 Cl1 O3 La1 82(2) . . . . ? O4 Cl1 O3 La1 -39(2) . . . . ? O1 La1 O3 Cl1 -14(2) . . . . ? O2 La1 O3 Cl1 58(2) . . . . ? O21 La1 O3 Cl1 -77(2) . . . . ? O20 La1 O3 Cl1 -92(2) . . . . ? N3 La1 O3 Cl1 45(2) . . . . ? N7 La1 O3 Cl1 165.2(18) . . . . ? N6 La1 O3 Cl1 -163(2) . . . . ? N2 La1 O3 Cl1 112(2) . . . . ? C5 N1 N2 C7 -2(2) . . . . ? C4 N1 N2 C7 -177.5(18) . . . . ? C5 N1 N2 La1 -161.5(16) . . . . ? C4 N1 N2 La1 23(3) . . . . ? O1 La1 N2 N1 167.9(15) . . . . ? O2 La1 N2 N1 -120.1(17) . . . . ? O21 La1 N2 N1 -78(2) . . . . ? O3 La1 N2 N1 91.6(17) . . . . ? O20 La1 N2 N1 57.9(19) . . . . ? N3 La1 N2 N1 170.0(18) . . . . ? N7 La1 N2 N1 -57.6(17) . . . . ? N6 La1 N2 N1 3.1(17) . . . . ? O1 La1 N2 C7 9.7(15) . . . . ? O2 La1 N2 C7 81.7(14) . . . . ? O21 La1 N2 C7 124.2(14) . . . . ? O3 La1 N2 C7 -66.6(14) . . . . ? O20 La1 N2 C7 -100.3(15) . . . . ? N3 La1 N2 C7 11.8(13) . . . . ? N7 La1 N2 C7 144.2(14) . . . . ? N6 La1 N2 C7 -155.1(14) . . . . ? O1 La1 N3 C12 -6.5(13) . . . . ? O2 La1 N3 C12 83.1(15) . . . . ? O21 La1 N3 C12 33.0(16) . . . . ? O3 La1 N3 C12 -105.6(15) . . . . ? O20 La1 N3 C12 -55.6(16) . . . . ? N7 La1 N3 C12 114.9(14) . . . . ? N6 La1 N3 C12 -161.4(14) . . . . ? N2 La1 N3 C12 175.4(16) . . . . ? O1 La1 N3 C8 166.8(16) . . . . ? O2 La1 N3 C8 -103.5(15) . . . . ? O21 La1 N3 C8 -153.7(13) . . . . ? O3 La1 N3 C8 67.7(14) . . . . ? O20 La1 N3 C8 117.7(14) . . . . ? N7 La1 N3 C8 -71.8(15) . . . . ? N6 La1 N3 C8 11.9(19) . . . . ? N2 La1 N3 C8 -11.2(14) . . . . ? C22 N5 N6 C24 -4(2) . . . . ? C21 N5 N6 C24 175.3(17) . . . . ? C22 N5 N6 La1 145.1(15) . . . . ? C21 N5 N6 La1 -35(3) . . . . ? O1 La1 N6 N5 -53(2) . . . . ? O2 La1 N6 N5 179.5(17) . . . . ? O21 La1 N6 N5 -110.4(18) . . . . ? O3 La1 N6 N5 29.5(18) . . . . ? O20 La1 N6 N5 -41.0(18) . . . . ? N3 La1 N6 N5 81(2) . . . . ? N7 La1 N6 N5 -173(2) . . . . ? N2 La1 N6 N5 102.0(19) . . . . ? O1 La1 N6 C24 93.6(16) . . . . ? O2 La1 N6 C24 -34.1(16) . . . . ? O21 La1 N6 C24 36.0(15) . . . . ? O3 La1 N6 C24 175.9(15) . . . . ? O20 La1 N6 C24 105.4(15) . . . . ? N3 La1 N6 C24 -132.1(14) . . . . ? N7 La1 N6 C24 -26.4(13) . . . . ? N2 La1 N6 C24 -111.6(15) . . . . ? O1 La1 N7 C25 -114.6(14) . . . . ? O2 La1 N7 C25 -157.8(16) . . . . ? O21 La1 N7 C25 -74.7(15) . . . . ? O3 La1 N7 C25 66.4(17) . . . . ? O20 La1 N7 C25 -20.2(16) . . . . ? N3 La1 N7 C25 168.4(14) . . . . ? N6 La1 N7 C25 29.6(14) . . . . ? N2 La1 N7 C25 117.0(15) . . . . ? O1 La1 N7 C29 34.6(16) . . . . ? O2 La1 N7 C29 -8.7(12) . . . . ? O21 La1 N7 C29 74.5(13) . . . . ? O3 La1 N7 C29 -144.4(12) . . . . ? O20 La1 N7 C29 129.0(13) . . . . ? N3 La1 N7 C29 -42.5(15) . . . . ? N6 La1 N7 C29 178.7(15) . . . . ? N2 La1 N7 C29 -93.8(14) . . . . ? C3 C1 C2 C3 -2(3) 2_666 . . . ? C1 C2 C3 C1 2(3) . . . 2_666 ? C1 C2 C3 C4 179.5(18) . . . . ? N2 N1 C4 C3 78(2) . . . . ? C5 N1 C4 C3 -97(2) . . . . ? C2 C3 C4 N1 17(3) . . . . ? C1 C3 C4 N1 -165.1(19) 2_666 . . . ? N2 N1 C5 C6 1(3) . . . . ? C4 N1 C5 C6 176(2) . . . . ? N1 C5 C6 C7 0(3) . . . . ? C5 C6 C7 C8 178(2) . . . . ? C5 C6 C7 N2 -1(3) . . . . ? N1 N2 C7 C6 2(2) . . . . ? La1 N2 C7 C6 167.3(14) . . . . ? N1 N2 C7 C8 -178(2) . . . . ? La1 N2 C7 C8 -13(3) . . . . ? C12 N3 C8 C7 -176(2) . . . . ? La1 N3 C8 C7 10(3) . . . . ? C12 N3 C8 C9 5(3) . . . . ? La1 N3 C8 C9 -168.8(15) . . . . ? C6 C7 C8 N3 -178(2) . . . . ? N2 C7 C8 N3 2(3) . . . . ? C6 C7 C8 C9 1(4) . . . . ? N2 C7 C8 C9 -179(2) . . . . ? N3 C8 C9 C10 -4(3) . . . . ? C7 C8 C9 C10 177(2) . . . . ? C8 C9 C10 C11 4(3) . . . . ? C9 C10 C11 C12 -4(3) . . . . ? C8 N3 C12 C11 -5(3) . . . . ? La1 N3 C12 C11 168.2(15) . . . . ? C8 N3 C12 C13 177.4(18) . . . . ? La1 N3 C12 C13 -9(2) . . . . ? C10 C11 C12 N3 5(3) . . . . ? C10 C11 C12 C13 -179(2) . . . . ? La1 O1 C13 N4 139.1(16) . . . . ? La1 O1 C13 C12 -47(2) . . . . ? C16 N4 C13 O1 -174.5(19) . . . . ? C14 N4 C13 O1 0(3) . . . . ? C16 N4 C13 C12 12(3) . . . . ? C14 N4 C13 C12 -174.3(18) . . . . ? N3 C12 C13 O1 35(3) . . . . ? C11 C12 C13 O1 -142(2) . . . . ? N3 C12 C13 N4 -150.9(19) . . . . ? C11 C12 C13 N4 32(3) . . . . ? C13 N4 C14 C15 75(2) . . . . ? C16 N4 C14 C15 -111(2) . . . . ? C13 N4 C16 C17 -115(2) . . . . ? C14 N4 C16 C17 71(2) . . . . ? C20 C18 C19 C20 2(3) 2_566 . . . ? C18 C19 C20 C18 -2(3) . . . 2_566 ? C18 C19 C20 C21 -179.0(18) . . . . ? N6 N5 C21 C20 -95(2) . . . . ? C22 N5 C21 C20 85(2) . . . . ? C18 C20 C21 N5 -67(2) 2_566 . . . ? C19 C20 C21 N5 110(2) . . . . ? N6 N5 C22 C23 5(2) . . . . ? C21 N5 C22 C23 -174.6(19) . . . . ? N5 C22 C23 C24 -3(2) . . . . ? C22 C23 C24 N6 1(3) . . . . ? C22 C23 C24 C25 -179(2) . . . . ? N5 N6 C24 C23 2(3) . . . . ? La1 N6 C24 C23 -155.2(18) . . . . ? N5 N6 C24 C25 -178.1(17) . . . . ? La1 N6 C24 C25 25(2) . . . . ? C29 N7 C25 C26 -4(3) . . . . ? La1 N7 C25 C26 143.9(18) . . . . ? C29 N7 C25 C24 -177.3(17) . . . . ? La1 N7 C25 C24 -29(2) . . . . ? C23 C24 C25 N7 -178(2) . . . . ? N6 C24 C25 N7 3(3) . . . . ? C23 C24 C25 C26 8(4) . . . . ? N6 C24 C25 C26 -171.4(19) . . . . ? N7 C25 C26 C27 4(3) . . . . ? C24 C25 C26 C27 178(2) . . . . ? C25 C26 C27 C28 1(4) . . . . ? C26 C27 C28 C29 -6(4) . . . . ? C25 N7 C29 C28 -2(3) . . . . ? La1 N7 C29 C28 -150.7(17) . . . . ? C25 N7 C29 C30 172.4(18) . . . . ? La1 N7 C29 C30 23(2) . . . . ? C27 C28 C29 N7 6(3) . . . . ? C27 C28 C29 C30 -168(2) . . . . ? La1 O2 C30 N8 -153.5(14) . . . . ? La1 O2 C30 C29 24(2) . . . . ? C31 N8 C30 O2 173.7(17) . . . . ? C33 N8 C30 O2 -10(3) . . . . ? C31 N8 C30 C29 -4(3) . . . . ? C33 N8 C30 C29 172.9(17) . . . . ? N7 C29 C30 O2 -31(2) . . . . ? C28 C29 C30 O2 143(2) . . . . ? N7 C29 C30 N8 146.8(19) . . . . ? C28 C29 C30 N8 -39(3) . . . . ? C30 N8 C31 C32 -137(2) . . . . ? C33 N8 C31 C32 46(3) . . . . ? C30 N8 C33 C34 85(3) . . . . ? C31 N8 C33 C34 -98(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O20 H2A O1W 0.85 1.88 2.73(4) 179.4 . O20 H2B O9 0.85 1.99 2.80(2) 159.3 1_565 O21 H2D O7 0.85 2.25 2.96(2) 142.3 1_565 O21 H2C O11 0.85 1.98 2.83(4) 177.8 2_666 O21 H2C O11' 0.85 2.06 2.88(4) 161.0 2_666 O1W H1B O9 0.85 2.64 3.49(4) 179.3 2_566 O1W H1A O14 0.85 2.09 2.94(4) 179.6 2_566 _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 2.462 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.237 #===END data_imw534 _database_code_depnum_ccdc_archive 'CCDC 630965' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H104 Cl5 N19 O30 Yb2' _chemical_formula_weight 2335.15 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' Yb Yb -0.3850 5.5486 '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 14.5305(9) _cell_length_b 14.6421(9) _cell_length_c 24.2903(15) _cell_angle_alpha 91.300(3) _cell_angle_beta 105.283(2) _cell_angle_gamma 103.157(2) _cell_volume 4835.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8800 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.07 _exptl_crystal_description plate _exptl_crystal_colour clear _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2364 _exptl_absorpt_coefficient_mu 2.148 _exptl_absorpt_correction_type mullti-scan _exptl_absorpt_correction_T_min 0.7250 _exptl_absorpt_correction_T_max 0.9788 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69390 _diffrn_reflns_av_R_equivalents 0.0717 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.87 _diffrn_reflns_theta_max 26.00 _reflns_number_total 18874 _reflns_number_gt 14039 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0465P)^2^+16.3072P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18874 _refine_ls_number_parameters 1284 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.0977 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.998 _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 Yb1 Yb 0.200626(16) 0.946641(17) 0.722247(9) 0.01541(7) Uani 1 1 d . . . Yb2 Yb -0.196830(17) 0.701158(17) 0.763976(9) 0.01712(7) Uani 1 1 d . . . O1 O 0.2391(3) 0.9619(3) 0.63878(15) 0.0199(8) Uani 1 1 d . . . O2 O -0.3391(3) 0.6185(3) 0.70472(16) 0.0255(9) Uani 1 1 d . . . O3 O 0.2097(3) 1.0983(3) 0.74874(15) 0.0205(8) Uani 1 1 d . . . O4 O -0.2418(3) 0.8186(3) 0.80026(16) 0.0234(9) Uani 1 1 d . . . O200 O 0.0910(3) 0.8863(3) 0.76682(15) 0.0217(9) Uani 1 1 d . . . O201 O -0.0482(3) 0.7952(3) 0.77343(16) 0.0258(9) Uani 1 1 d . . . O202 O 0.2738(3) 0.8234(3) 0.73704(17) 0.0253(9) Uani 1 1 d . . . H2A H 0.2969 0.8083 0.7705 0.030 Uiso 1 1 d R . . H2B H 0.2984 0.8082 0.7111 0.030 Uiso 1 1 d R . . O203 O -0.1372(3) 0.5714(3) 0.78032(16) 0.0255(9) Uani 1 1 d . . . H2C H -0.1010 0.5780 0.8146 0.031 Uiso 1 1 d R . . H2D H -0.1774 0.5183 0.7689 0.031 Uiso 1 1 d R . . N1 N 0.3706(3) 1.0343(3) 0.73300(18) 0.0182(10) Uani 1 1 d . . . N2 N 0.3099(3) 0.9823(3) 0.82541(18) 0.0199(10) Uani 1 1 d . . . N3 N 0.3068(3) 0.9589(4) 0.87867(18) 0.0222(11) Uani 1 1 d . . . N4 N -0.0480(3) 0.7391(4) 0.91584(19) 0.0252(11) Uani 1 1 d . . . N5 N -0.1340(3) 0.7095(3) 0.87403(19) 0.0215(11) Uani 1 1 d . . . N6 N -0.3198(3) 0.6235(3) 0.81249(19) 0.0202(10) Uani 1 1 d . . . N7 N 0.3470(3) 0.9812(3) 0.58603(19) 0.0200(10) Uani 1 1 d . . . N8 N -0.4848(4) 0.5148(4) 0.6795(2) 0.0328(13) Uani 1 1 d . . . N9 N 0.0722(3) 1.0144(3) 0.66131(18) 0.0168(10) Uani 1 1 d . . . N10 N 0.0682(3) 0.8307(3) 0.64501(19) 0.0197(10) Uani 1 1 d . . . N11 N 0.0522(3) 0.7405(3) 0.62401(19) 0.0207(10) Uani 1 1 d . . . N12 N -0.1622(4) 0.5950(4) 0.6335(2) 0.0239(11) Uani 1 1 d . . . N13 N -0.1711(3) 0.6701(3) 0.66322(19) 0.0214(11) Uani 1 1 d . . . N14 N -0.2440(3) 0.8149(3) 0.69551(19) 0.0216(11) Uani 1 1 d . . . N15 N 0.1429(4) 1.2190(3) 0.7597(2) 0.0248(11) Uani 1 1 d . . . N16 N -0.2837(4) 0.9548(4) 0.8077(2) 0.0311(12) Uani 1 1 d . . . C1 C 0.1476(4) 0.9474(4) 0.9007(2) 0.0225(13) Uani 1 1 d . . . C2 C 0.0598(4) 0.8924(4) 0.9086(2) 0.0245(13) Uani 1 1 d . . . C3 C -0.0079(5) 0.9373(5) 0.9209(3) 0.0321(15) Uani 1 1 d . . . H3 H -0.0672 0.9009 0.9266 0.039 Uiso 1 1 calc R . . C4 C 0.0101(6) 1.0349(5) 0.9251(3) 0.0390(17) Uani 1 1 d . . . H4 H -0.0367 1.0648 0.9335 0.047 Uiso 1 1 calc R . . C5 C 0.0962(5) 1.0885(5) 0.9169(3) 0.0376(16) Uani 1 1 d . . . H5 H 0.1082 1.1552 0.9192 0.045 Uiso 1 1 calc R . . C6 C 0.1654(5) 1.0441(5) 0.9054(3) 0.0293(14) Uani 1 1 d . . . H6 H 0.2253 1.0810 0.9007 0.035 Uiso 1 1 calc R . . C7 C 0.2210(4) 0.8964(4) 0.8886(2) 0.0251(13) Uani 1 1 d . . . H7A H 0.2425 0.8602 0.9215 0.030 Uiso 1 1 calc R . . H7B H 0.1879 0.8509 0.8545 0.030 Uiso 1 1 calc R . . C8 C 0.3890(4) 1.0045(5) 0.9188(2) 0.0282(14) Uani 1 1 d . . . H8 H 0.4032 0.9987 0.9589 0.034 Uiso 1 1 calc R . . C9 C 0.4483(4) 1.0606(4) 0.8914(2) 0.0254(13) Uani 1 1 d . . . H9 H 0.5108 1.1020 0.9083 0.030 Uiso 1 1 calc R . . C10 C 0.3974(4) 1.0443(4) 0.8336(2) 0.0192(12) Uani 1 1 d . . . C11 C 0.4256(4) 1.0798(4) 0.7831(2) 0.0180(12) Uani 1 1 d . . . C12 C 0.5052(4) 1.1570(4) 0.7869(2) 0.0253(13) Uani 1 1 d . . . H12 H 0.5442 1.1883 0.8230 0.030 Uiso 1 1 calc R . . C13 C 0.5253(4) 1.1864(4) 0.7368(3) 0.0270(14) Uani 1 1 d . . . H13 H 0.5768 1.2404 0.7380 0.032 Uiso 1 1 calc R . . C14 C 0.4705(4) 1.1372(4) 0.6847(2) 0.0244(13) Uani 1 1 d . . . H14 H 0.4844 1.1558 0.6499 0.029 Uiso 1 1 calc R . . C15 C 0.3943(4) 1.0595(4) 0.6847(2) 0.0196(12) Uani 1 1 d . . . C16 C 0.3248(4) 0.9995(4) 0.6338(2) 0.0193(12) Uani 1 1 d . . . C17 C 0.2685(4) 0.9224(4) 0.5388(2) 0.0271(14) Uani 1 1 d . . . H17A H 0.2851 0.9344 0.5023 0.032 Uiso 1 1 calc R . . H17B H 0.2061 0.9408 0.5364 0.032 Uiso 1 1 calc R . . C18 C 0.2538(5) 0.8177(5) 0.5468(3) 0.0351(16) Uani 1 1 d . . . H18A H 0.2288 0.8041 0.5803 0.053 Uiso 1 1 calc R . . H18B H 0.3167 0.8003 0.5527 0.053 Uiso 1 1 calc R . . H18C H 0.2063 0.7814 0.5126 0.053 Uiso 1 1 calc R . . C19 C 0.4474(4) 1.0029(4) 0.5791(2) 0.0230(13) Uani 1 1 d . . . H19A H 0.4593 0.9456 0.5628 0.028 Uiso 1 1 calc R . . H19B H 0.4955 1.0215 0.6172 0.028 Uiso 1 1 calc R . . C20 C 0.4632(5) 1.0813(5) 0.5405(3) 0.0303(15) Uani 1 1 d . . . H20A H 0.4488 1.1374 0.5557 0.045 Uiso 1 1 calc R . . H20B H 0.4194 1.0611 0.5018 0.045 Uiso 1 1 calc R . . H20C H 0.5317 1.0961 0.5390 0.045 Uiso 1 1 calc R . . C21 C 0.0435(4) 0.7873(4) 0.9038(2) 0.0224(13) Uani 1 1 d . . . H21A H 0.0421 0.7657 0.8646 0.027 Uiso 1 1 calc R . . H21B H 0.0994 0.7698 0.9310 0.027 Uiso 1 1 calc R . . C22 C -0.0610(5) 0.7274(5) 0.9684(3) 0.0342(16) Uani 1 1 d . . . H22 H -0.0112 0.7430 1.0038 0.041 Uiso 1 1 calc R . . C23 C -0.1584(5) 0.6892(5) 0.9615(3) 0.0345(16) Uani 1 1 d . . . H23 H -0.1903 0.6728 0.9906 0.041 Uiso 1 1 calc R . . C24 C -0.2012(4) 0.6792(4) 0.9022(2) 0.0234(13) Uani 1 1 d . . . C25 C -0.3034(4) 0.6398(4) 0.8696(2) 0.0199(12) Uani 1 1 d . . . C26 C -0.3801(5) 0.6193(5) 0.8956(3) 0.0300(15) Uani 1 1 d . . . H26 H -0.3670 0.6279 0.9361 0.036 Uiso 1 1 calc R . . C27 C -0.4748(5) 0.5862(5) 0.8614(3) 0.0338(16) Uani 1 1 d . . . H27 H -0.5283 0.5742 0.8779 0.041 Uiso 1 1 calc R . . C28 C -0.4920(5) 0.5704(5) 0.8028(3) 0.0300(15) Uani 1 1 d . . . H28 H -0.5571 0.5494 0.7786 0.036 Uiso 1 1 calc R . . C29 C -0.4116(4) 0.5861(4) 0.7800(2) 0.0214(12) Uani 1 1 d . . . C30 C -0.4134(4) 0.5719(4) 0.7184(2) 0.0257(14) Uani 1 1 d . . . C31 C -0.4783(5) 0.5127(7) 0.6199(3) 0.058(3) Uani 1 1 d . . . H31A H -0.5452 0.4918 0.5935 0.069 Uiso 1 1 calc R . . H31B H -0.4490 0.5771 0.6117 0.069 Uiso 1 1 calc R . . C32 C -0.4192(7) 0.4501(8) 0.6100(4) 0.080(3) Uani 1 1 d . . . H32A H -0.4503 0.3856 0.6157 0.121 Uiso 1 1 calc R . . H32B H -0.3534 0.4696 0.6369 0.121 Uiso 1 1 calc R . . H32C H -0.4139 0.4527 0.5707 0.121 Uiso 1 1 calc R . . C33 C -0.5669(4) 0.4418(5) 0.6893(3) 0.0349(16) Uani 1 1 d . . . H33A H -0.5525 0.4320 0.7306 0.042 Uiso 1 1 calc R . . H33B H -0.5719 0.3816 0.6681 0.042 Uiso 1 1 calc R . . C34 C -0.6644(5) 0.4689(6) 0.6703(3) 0.0446(19) Uani 1 1 d . . . H34A H -0.6770 0.4827 0.6301 0.067 Uiso 1 1 calc R . . H34B H -0.6622 0.5248 0.6941 0.067 Uiso 1 1 calc R . . H34C H -0.7172 0.4167 0.6745 0.067 Uiso 1 1 calc R . . C35 C 0.0548(4) 0.5736(4) 0.6312(2) 0.0230(13) Uani 1 1 d . . . C36 C -0.0346(5) 0.5096(4) 0.6287(2) 0.0241(13) Uani 1 1 d . . . C37 C -0.0564(5) 0.4244(4) 0.5974(2) 0.0259(14) Uani 1 1 d . . . H37 H -0.1166 0.3804 0.5954 0.031 Uiso 1 1 calc R . . C38 C 0.0064(5) 0.4005(4) 0.5686(2) 0.0269(14) Uani 1 1 d . . . H38 H -0.0112 0.3411 0.5471 0.032 Uiso 1 1 calc R . . C39 C 0.0941(5) 0.4623(5) 0.5711(3) 0.0311(15) Uani 1 1 d . . . H39 H 0.1379 0.4458 0.5519 0.037 Uiso 1 1 calc R . . C40 C 0.1180(4) 0.5489(4) 0.6020(3) 0.0254(13) Uani 1 1 d . . . H40 H 0.1783 0.5924 0.6034 0.031 Uiso 1 1 calc R . . C41 C 0.0848(5) 0.6705(4) 0.6629(3) 0.0293(14) Uani 1 1 d . . . H41A H 0.0550 0.6690 0.6952 0.035 Uiso 1 1 calc R . . H41B H 0.1572 0.6892 0.6787 0.035 Uiso 1 1 calc R . . C42 C -0.0040(4) 0.7256(4) 0.5696(2) 0.0221(13) Uani 1 1 d . . . H42 H -0.0245 0.6675 0.5465 0.026 Uiso 1 1 calc R . . C43 C -0.0266(4) 0.8077(4) 0.5530(2) 0.0212(12) Uani 1 1 d . . . H43 H -0.0646 0.8191 0.5167 0.025 Uiso 1 1 calc R . . C44 C 0.0188(4) 0.8718(4) 0.6016(2) 0.0193(12) Uani 1 1 d . . . C45 C 0.0172(4) 0.9698(4) 0.6100(2) 0.0181(12) Uani 1 1 d . . . C46 C -0.0379(4) 1.0156(4) 0.5687(2) 0.0259(14) Uani 1 1 d . . . H46 H -0.0779 0.9827 0.5332 0.031 Uiso 1 1 calc R . . C47 C -0.0334(5) 1.1092(5) 0.5802(3) 0.0294(14) Uani 1 1 d . . . H47 H -0.0690 1.1420 0.5522 0.035 Uiso 1 1 calc R . . C48 C 0.0232(5) 1.1555(4) 0.6328(3) 0.0286(14) Uani 1 1 d . . . H48 H 0.0272 1.2202 0.6414 0.034 Uiso 1 1 calc R . . C49 C 0.0739(4) 1.1049(4) 0.6725(2) 0.0190(12) Uani 1 1 d . . . C50 C 0.1451(4) 1.1425(4) 0.7300(2) 0.0200(12) Uani 1 1 d . . . C51 C 0.2268(5) 1.2538(4) 0.8112(2) 0.0295(14) Uani 1 1 d . . . H51A H 0.2413 1.2000 0.8330 0.035 Uiso 1 1 calc R . . H51B H 0.2088 1.2970 0.8363 0.035 Uiso 1 1 calc R . . C52 C 0.3189(5) 1.3058(5) 0.7950(3) 0.0378(17) Uani 1 1 d . . . H52A H 0.3086 1.3650 0.7794 0.057 Uiso 1 1 calc R . . H52B H 0.3316 1.2663 0.7660 0.057 Uiso 1 1 calc R . . H52C H 0.3755 1.3193 0.8291 0.057 Uiso 1 1 calc R . . C53 C 0.0583(5) 1.2617(5) 0.7524(3) 0.0358(16) Uani 1 1 d . . . H53A H 0.0381 1.2597 0.7883 0.043 Uiso 1 1 calc R . . H53B H 0.0023 1.2239 0.7217 0.043 Uiso 1 1 calc R . . C54 C 0.0803(6) 1.3620(5) 0.7374(4) 0.049(2) Uani 1 1 d . . . H54A H 0.1013 1.3647 0.7022 0.074 Uiso 1 1 calc R . . H54B H 0.1330 1.4006 0.7688 0.074 Uiso 1 1 calc R . . H54C H 0.0211 1.3860 0.7316 0.074 Uiso 1 1 calc R . . C55 C -0.1051(5) 0.5289(5) 0.6609(3) 0.0321(15) Uani 1 1 d . . . H55A H -0.1510 0.4688 0.6633 0.038 Uiso 1 1 calc R . . H55B H -0.0675 0.5552 0.7004 0.038 Uiso 1 1 calc R . . C56 C -0.2081(5) 0.5923(5) 0.5775(3) 0.0297(14) Uani 1 1 d . . . H56 H -0.2123 0.5453 0.5487 0.036 Uiso 1 1 calc R . . C57 C -0.2475(4) 0.6686(4) 0.5689(2) 0.0258(14) Uani 1 1 d . . . H57 H -0.2838 0.6859 0.5338 0.031 Uiso 1 1 calc R . . C58 C -0.2227(4) 0.7155(4) 0.6232(2) 0.0218(13) Uani 1 1 d . . . C59 C -0.2455(4) 0.8020(4) 0.6407(2) 0.0225(13) Uani 1 1 d . . . C60 C -0.2634(5) 0.8698(5) 0.6018(3) 0.0315(15) Uani 1 1 d . . . H60 H -0.2651 0.8592 0.5627 0.038 Uiso 1 1 calc R . . C61 C -0.2784(6) 0.9518(5) 0.6222(3) 0.0454(19) Uani 1 1 d . . . H61 H -0.2870 1.0005 0.5976 0.054 Uiso 1 1 calc R . . C62 C -0.2809(6) 0.9638(5) 0.6784(3) 0.047(2) Uani 1 1 d . . . H62 H -0.2943 1.0192 0.6921 0.056 Uiso 1 1 calc R . . C63 C -0.2635(5) 0.8928(4) 0.7146(3) 0.0273(14) Uani 1 1 d . . . C64 C -0.2641(5) 0.8902(4) 0.7769(3) 0.0271(14) Uani 1 1 d . . . C65 C -0.2801(5) 0.9386(5) 0.8683(3) 0.0368(16) Uani 1 1 d . . . H65A H -0.2576 0.9998 0.8918 0.044 Uiso 1 1 calc R . . H65B H -0.2323 0.9004 0.8831 0.044 Uiso 1 1 calc R . . C66 C -0.3811(6) 0.8878(6) 0.8734(4) 0.054(2) Uani 1 1 d . . . H66A H -0.4037 0.8276 0.8498 0.082 Uiso 1 1 calc R . . H66B H -0.4278 0.9268 0.8602 0.082 Uiso 1 1 calc R . . H66C H -0.3766 0.8764 0.9135 0.082 Uiso 1 1 calc R . . C67 C -0.3127(6) 1.0417(5) 0.7892(3) 0.046(2) Uani 1 1 d . . . H67A H -0.3545 1.0580 0.8123 0.055 Uiso 1 1 calc R . . H67B H -0.3519 1.0309 0.7486 0.055 Uiso 1 1 calc R . . C68 C -0.2236(7) 1.1227(5) 0.7960(3) 0.052(2) Uani 1 1 d . . . H68A H -0.1815 1.1061 0.7738 0.077 Uiso 1 1 calc R . . H68B H -0.1866 1.1357 0.8365 0.077 Uiso 1 1 calc R . . H68C H -0.2449 1.1789 0.7821 0.077 Uiso 1 1 calc R . . C200 C 0.0037(4) 0.8728(5) 0.7675(2) 0.0265(14) Uani 1 1 d . . . C201 C -0.0303(7) 0.9652(7) 0.7719(4) 0.069(3) Uani 1 1 d . . . H20D H -0.0636 0.9791 0.7336 0.103 Uiso 1 1 calc R . . H20E H 0.0271 1.0172 0.7891 0.103 Uiso 1 1 calc R . . H20F H -0.0757 0.9577 0.7959 0.103 Uiso 1 1 calc R . . Cl1 Cl 0.25624(11) 0.81601(12) 0.04484(6) 0.0304(3) Uani 1 1 d . . . O10 O 0.3163(4) 0.8963(5) 0.0277(2) 0.0660(18) Uani 1 1 d . . . O11 O 0.1663(3) 0.8377(4) 0.04701(19) 0.0403(12) Uani 1 1 d . . . O12 O 0.3087(4) 0.7968(4) 0.10038(18) 0.0458(13) Uani 1 1 d . . . O13 O 0.2357(4) 0.7375(4) 0.0035(2) 0.0538(15) Uani 1 1 d . . . Cl2 Cl 0.52635(13) 0.20662(13) 0.31475(7) 0.0382(4) Uani 1 1 d . . . O14 O 0.4664(5) 0.2410(4) 0.2681(2) 0.0649(17) Uani 1 1 d . . . O15 O 0.6283(4) 0.2566(6) 0.3251(3) 0.085(2) Uani 1 1 d . . . O16 O 0.4944(5) 0.2144(6) 0.3641(3) 0.083(2) Uani 1 1 d . . . O17 O 0.5221(6) 0.1114(5) 0.3011(3) 0.087(2) Uani 1 1 d . . . Cl3 Cl 0.7030(4) 0.5741(5) 1.0662(3) 0.0526(17) Uani 0.50 1 d PDU A 1 O18 O 0.8055(8) 0.6253(10) 1.0862(5) 0.069(4) Uani 0.50 1 d PD A 1 Cl3' Cl 0.6632(4) 0.5533(5) 1.0561(3) 0.0515(16) Uani 0.50 1 d PDU A 2 O18' O 0.5626(7) 0.5124(9) 1.0271(5) 0.062(3) Uani 0.50 1 d PD A 2 O19 O 0.6633(6) 0.6491(5) 1.0505(3) 0.091(2) Uani 1 1 d D . . O20 O 0.7102(6) 0.5148(5) 1.0228(3) 0.090(2) Uani 1 1 d D . . O21 O 0.6823(5) 0.5294(4) 1.1137(2) 0.0666(18) Uani 1 1 d D . . Cl4 Cl 0.74275(10) 0.77822(10) 0.42055(6) 0.0242(3) Uani 1 1 d . . . O22 O 0.7291(3) 0.7982(3) 0.36156(18) 0.0384(11) Uani 1 1 d . . . O23 O 0.8089(3) 0.7174(3) 0.43485(18) 0.0336(11) Uani 1 1 d . . . O24 O 0.6485(3) 0.7334(3) 0.42892(19) 0.0375(11) Uani 1 1 d . . . O25 O 0.7827(3) 0.8646(3) 0.4577(2) 0.0411(12) Uani 1 1 d . . . Cl5 Cl -0.25491(11) 0.22281(11) 0.63831(6) 0.0287(3) Uani 1 1 d D . . O29 O -0.3318(3) 0.1612(3) 0.6552(2) 0.0376(11) Uani 1 1 d . B . O26 O -0.1886(8) 0.1751(8) 0.6231(5) 0.063(2) Uani 0.50 1 d PDU B 1 O27 O -0.1921(8) 0.2866(8) 0.6874(4) 0.061(2) Uani 0.50 1 d PDU B 1 O28 O -0.2859(8) 0.2806(8) 0.5941(5) 0.059(2) Uani 0.50 1 d PDU B 1 O26' O -0.2639(8) 0.1922(8) 0.5802(4) 0.049(2) Uani 0.50 1 d PDU B 2 O27' O -0.1633(7) 0.2203(9) 0.6733(5) 0.061(2) Uani 0.50 1 d PDU B 2 O28' O -0.2798(8) 0.3129(6) 0.6363(5) 0.050(2) Uani 0.50 1 d PDU B 2 O1W O -0.2609(5) 0.4094(4) 0.7457(3) 0.076(2) Uani 1 1 d . . . H2W H -0.2396 0.3720 0.7278 0.091 Uiso 1 1 d R . . H1W H -0.2974 0.3934 0.7678 0.091 Uiso 1 1 d R . . N1S N 1.3761(5) 0.6129(5) 1.1790(3) 0.0566(18) Uani 1 1 d . . . C1S C 1.3968(6) 0.6208(6) 1.1361(4) 0.049(2) Uani 1 1 d . . . C2S C 1.4226(6) 0.6352(6) 1.0822(3) 0.052(2) Uani 1 1 d . . . H2S1 H 1.3637 0.6126 1.0501 0.078 Uiso 1 1 calc R . . H2S2 H 1.4717 0.6003 1.0800 0.078 Uiso 1 1 calc R . . H2S3 H 1.4497 0.7025 1.0805 0.078 Uiso 1 1 calc R . . N2S N 0.3053(5) 0.5798(5) 0.5272(3) 0.0534(18) Uani 1 1 d . . . C3S C 0.3692(7) 0.6325(6) 0.5205(3) 0.052(2) Uani 1 1 d . . . C4S C 0.4527(7) 0.7010(6) 0.5104(4) 0.071(3) Uani 1 1 d . . . H4S1 H 0.4300 0.7316 0.4756 0.107 Uiso 1 1 calc R . . H4S2 H 0.5025 0.6686 0.5057 0.107 Uiso 1 1 calc R . . H4S3 H 0.4813 0.7486 0.5432 0.107 Uiso 1 1 calc R . . N3S N 0.6439(6) 0.2327(5) 1.1538(3) 0.061(2) Uani 1 1 d . . . C5S C 0.6093(6) 0.2506(6) 1.1075(4) 0.055(2) Uani 1 1 d . . . C6S C 0.5707(8) 0.2740(8) 1.0491(4) 0.073(3) Uani 1 1 d . . . H6S1 H 0.5893 0.3424 1.0476 0.110 Uiso 1 1 calc R . . H6S2 H 0.4989 0.2520 1.0374 0.110 Uiso 1 1 calc R . . H6S3 H 0.5980 0.2433 1.0230 0.110 Uiso 1 1 calc R . . O1S O 0.9883(5) 0.4552(5) 1.1335(3) 0.0727(19) Uani 1 1 d . . . C11S C 0.8760(7) 0.3884(7) 1.1904(3) 0.065(3) Uani 1 1 d . . . H11A H 0.9050 0.3338 1.1957 0.097 Uiso 1 1 calc R . . H11B H 0.8063 0.3688 1.1892 0.097 Uiso 1 1 calc R . . H11C H 0.9105 0.4366 1.2223 0.097 Uiso 1 1 calc R . . C12S C 0.8856(7) 0.4287(8) 1.1340(4) 0.076(3) Uani 1 1 d . . . H12A H 0.8477 0.3812 1.1016 0.091 Uiso 1 1 calc R . . H12B H 0.8577 0.4847 1.1291 0.091 Uiso 1 1 calc R . . C13S C 0.9998(10) 0.4990(10) 1.0826(5) 0.103(4) Uani 1 1 d . . . H13A H 0.9565 0.5432 1.0733 0.123 Uiso 1 1 calc R . . H13B H 0.9809 0.4505 1.0499 0.123 Uiso 1 1 calc R . . C14S C 1.1075(12) 0.5525(13) 1.0928(6) 0.158(8) Uani 1 1 d . . . H14A H 1.1183 0.6144 1.1129 0.238 Uiso 1 1 calc R . . H14B H 1.1224 0.5605 1.0558 0.238 Uiso 1 1 calc R . . H14C H 1.1504 0.5167 1.1160 0.238 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 Yb1 0.01176(12) 0.01683(14) 0.01658(12) 0.00200(9) 0.00351(9) 0.00172(10) Yb2 0.01431(13) 0.01785(14) 0.01895(12) 0.00331(9) 0.00555(10) 0.00212(10) O1 0.016(2) 0.022(2) 0.0184(19) 0.0012(16) 0.0040(16) -0.0007(17) O2 0.016(2) 0.032(2) 0.024(2) 0.0041(18) 0.0059(17) -0.0036(18) O3 0.017(2) 0.017(2) 0.023(2) -0.0010(16) 0.0015(16) 0.0020(17) O4 0.027(2) 0.024(2) 0.025(2) 0.0068(17) 0.0099(17) 0.0128(19) O200 0.015(2) 0.025(2) 0.022(2) 0.0044(16) 0.0039(16) -0.0009(17) O201 0.023(2) 0.030(2) 0.020(2) 0.0045(17) 0.0059(17) -0.0027(19) O202 0.021(2) 0.024(2) 0.029(2) 0.0020(17) 0.0030(17) 0.0068(18) O203 0.028(2) 0.027(2) 0.023(2) 0.0025(17) 0.0078(17) 0.0087(19) N1 0.013(2) 0.021(3) 0.020(2) 0.0024(19) 0.0045(19) 0.006(2) N2 0.017(2) 0.024(3) 0.017(2) 0.0025(19) 0.0040(19) 0.004(2) N3 0.017(2) 0.030(3) 0.016(2) 0.005(2) 0.0024(19) 0.001(2) N4 0.018(3) 0.035(3) 0.016(2) 0.005(2) 0.001(2) 0.000(2) N5 0.020(3) 0.025(3) 0.019(2) 0.004(2) 0.005(2) 0.004(2) N6 0.018(2) 0.019(3) 0.023(2) 0.0049(19) 0.006(2) 0.001(2) N7 0.020(3) 0.021(3) 0.020(2) 0.0014(19) 0.0072(19) 0.003(2) N8 0.022(3) 0.041(3) 0.026(3) 0.004(2) 0.007(2) -0.011(3) N9 0.013(2) 0.017(3) 0.019(2) 0.0025(18) 0.0050(18) 0.0004(19) N10 0.020(3) 0.016(3) 0.022(2) 0.0011(19) 0.006(2) 0.000(2) N11 0.020(3) 0.019(3) 0.022(2) 0.0007(19) 0.004(2) 0.004(2) N12 0.023(3) 0.027(3) 0.025(3) 0.002(2) 0.012(2) 0.007(2) N13 0.019(3) 0.024(3) 0.021(2) 0.002(2) 0.008(2) 0.001(2) N14 0.017(2) 0.023(3) 0.023(2) 0.006(2) 0.003(2) 0.003(2) N15 0.022(3) 0.020(3) 0.031(3) 0.000(2) 0.004(2) 0.006(2) N16 0.040(3) 0.030(3) 0.029(3) 0.003(2) 0.011(2) 0.018(3) C1 0.023(3) 0.030(4) 0.012(3) 0.002(2) 0.003(2) 0.004(3) C2 0.030(3) 0.026(3) 0.015(3) 0.003(2) 0.005(2) 0.003(3) C3 0.032(4) 0.039(4) 0.030(3) 0.004(3) 0.014(3) 0.012(3) C4 0.047(4) 0.040(4) 0.038(4) 0.002(3) 0.019(3) 0.018(4) C5 0.047(4) 0.027(4) 0.041(4) 0.003(3) 0.016(3) 0.010(3) C6 0.029(3) 0.028(4) 0.033(3) 0.006(3) 0.014(3) 0.003(3) C7 0.024(3) 0.029(4) 0.019(3) 0.005(2) 0.004(2) 0.000(3) C8 0.024(3) 0.040(4) 0.016(3) -0.001(3) 0.002(2) 0.003(3) C9 0.013(3) 0.031(4) 0.025(3) 0.000(3) 0.002(2) -0.003(3) C10 0.011(3) 0.021(3) 0.023(3) 0.000(2) 0.002(2) 0.003(2) C11 0.012(3) 0.025(3) 0.019(3) 0.003(2) 0.005(2) 0.007(2) C12 0.016(3) 0.030(4) 0.027(3) -0.001(3) 0.005(2) 0.001(3) C13 0.015(3) 0.026(3) 0.034(3) 0.000(3) 0.007(3) -0.006(3) C14 0.015(3) 0.031(4) 0.027(3) 0.003(3) 0.007(2) 0.002(3) C15 0.019(3) 0.018(3) 0.025(3) 0.004(2) 0.008(2) 0.007(2) C16 0.016(3) 0.022(3) 0.021(3) 0.007(2) 0.005(2) 0.006(2) C17 0.025(3) 0.034(4) 0.019(3) -0.001(3) 0.003(2) 0.006(3) C18 0.032(4) 0.028(4) 0.042(4) -0.001(3) 0.007(3) 0.006(3) C19 0.018(3) 0.031(4) 0.025(3) 0.003(2) 0.013(2) 0.006(3) C20 0.035(4) 0.034(4) 0.028(3) 0.005(3) 0.016(3) 0.011(3) C21 0.019(3) 0.029(3) 0.018(3) 0.003(2) 0.004(2) 0.004(3) C22 0.035(4) 0.045(4) 0.017(3) 0.005(3) 0.005(3) 0.002(3) C23 0.029(4) 0.047(4) 0.024(3) 0.002(3) 0.012(3) -0.003(3) C24 0.027(3) 0.024(3) 0.021(3) 0.004(2) 0.011(2) 0.003(3) C25 0.019(3) 0.015(3) 0.024(3) 0.004(2) 0.006(2) 0.001(2) C26 0.027(3) 0.030(4) 0.032(3) 0.001(3) 0.017(3) -0.003(3) C27 0.027(4) 0.039(4) 0.039(4) 0.006(3) 0.019(3) 0.002(3) C28 0.021(3) 0.033(4) 0.033(3) 0.002(3) 0.010(3) -0.001(3) C29 0.018(3) 0.019(3) 0.029(3) 0.006(2) 0.010(2) 0.004(2) C30 0.015(3) 0.030(4) 0.030(3) 0.005(3) 0.003(2) 0.004(3) C31 0.031(4) 0.086(7) 0.037(4) -0.008(4) 0.011(3) -0.026(4) C32 0.063(6) 0.096(8) 0.068(6) -0.035(6) 0.037(5) -0.028(6) C33 0.023(3) 0.040(4) 0.033(3) 0.003(3) 0.008(3) -0.011(3) C34 0.026(4) 0.057(5) 0.041(4) 0.007(4) 0.006(3) -0.007(4) C35 0.028(3) 0.016(3) 0.024(3) -0.001(2) 0.003(2) 0.007(3) C36 0.031(3) 0.022(3) 0.021(3) 0.002(2) 0.009(3) 0.008(3) C37 0.032(4) 0.016(3) 0.030(3) 0.003(2) 0.013(3) 0.000(3) C38 0.038(4) 0.021(3) 0.026(3) 0.003(2) 0.012(3) 0.011(3) C39 0.033(4) 0.033(4) 0.036(3) 0.008(3) 0.018(3) 0.014(3) C40 0.016(3) 0.023(3) 0.033(3) 0.004(3) 0.002(2) 0.002(3) C41 0.041(4) 0.014(3) 0.027(3) 0.002(2) 0.001(3) 0.003(3) C42 0.021(3) 0.025(3) 0.015(3) -0.001(2) 0.000(2) 0.002(3) C43 0.020(3) 0.022(3) 0.015(3) 0.002(2) -0.001(2) 0.000(2) C44 0.014(3) 0.021(3) 0.021(3) 0.002(2) 0.003(2) 0.005(2) C45 0.013(3) 0.019(3) 0.022(3) 0.004(2) 0.008(2) -0.001(2) C46 0.022(3) 0.027(3) 0.022(3) 0.004(2) 0.000(2) -0.001(3) C47 0.025(3) 0.031(4) 0.027(3) 0.008(3) -0.005(3) 0.008(3) C48 0.029(4) 0.019(3) 0.035(3) 0.006(3) 0.003(3) 0.008(3) C49 0.014(3) 0.021(3) 0.023(3) 0.003(2) 0.008(2) 0.004(2) C50 0.018(3) 0.015(3) 0.028(3) 0.005(2) 0.009(2) 0.003(2) C51 0.037(4) 0.025(3) 0.023(3) 0.000(3) 0.004(3) 0.005(3) C52 0.031(4) 0.033(4) 0.037(4) -0.005(3) 0.001(3) -0.007(3) C53 0.033(4) 0.035(4) 0.041(4) -0.002(3) 0.007(3) 0.014(3) C54 0.050(5) 0.021(4) 0.068(5) -0.010(3) -0.004(4) 0.016(3) C55 0.038(4) 0.033(4) 0.036(3) 0.007(3) 0.019(3) 0.019(3) C56 0.028(3) 0.036(4) 0.027(3) -0.003(3) 0.013(3) 0.007(3) C57 0.020(3) 0.033(4) 0.022(3) 0.005(3) 0.006(2) 0.003(3) C58 0.020(3) 0.023(3) 0.024(3) 0.008(2) 0.012(2) 0.001(3) C59 0.018(3) 0.023(3) 0.025(3) 0.005(2) 0.006(2) 0.002(3) C60 0.035(4) 0.036(4) 0.021(3) 0.005(3) 0.006(3) 0.006(3) C61 0.075(6) 0.036(4) 0.029(4) 0.009(3) 0.009(4) 0.026(4) C62 0.086(6) 0.027(4) 0.029(4) 0.007(3) 0.005(4) 0.031(4) C63 0.033(4) 0.026(4) 0.027(3) 0.006(3) 0.009(3) 0.015(3) C64 0.027(3) 0.028(4) 0.029(3) 0.005(3) 0.009(3) 0.011(3) C65 0.048(4) 0.036(4) 0.031(3) -0.001(3) 0.012(3) 0.019(3) C66 0.058(5) 0.056(5) 0.065(5) 0.011(4) 0.038(4) 0.020(4) C67 0.071(6) 0.040(5) 0.041(4) 0.004(3) 0.018(4) 0.035(4) C68 0.086(7) 0.035(4) 0.039(4) 0.009(3) 0.019(4) 0.023(4) C200 0.022(3) 0.030(4) 0.028(3) 0.011(3) 0.009(3) 0.005(3) C201 0.054(6) 0.074(7) 0.073(6) 0.012(5) 0.017(5) 0.007(5) Cl1 0.0224(8) 0.0459(10) 0.0199(7) -0.0025(6) -0.0005(6) 0.0104(7) O10 0.041(3) 0.093(5) 0.041(3) 0.011(3) 0.003(3) -0.020(3) O11 0.027(3) 0.052(3) 0.041(3) -0.007(2) 0.003(2) 0.016(2) O12 0.045(3) 0.067(4) 0.023(2) 0.002(2) -0.004(2) 0.023(3) O13 0.056(3) 0.070(4) 0.033(3) -0.021(3) -0.007(2) 0.035(3) Cl2 0.0340(9) 0.0465(11) 0.0399(9) 0.0096(8) 0.0099(7) 0.0214(8) O14 0.077(4) 0.056(4) 0.058(4) 0.018(3) -0.002(3) 0.031(3) O15 0.042(4) 0.121(6) 0.074(4) -0.007(4) 0.004(3) -0.002(4) O16 0.079(5) 0.128(6) 0.057(4) -0.010(4) 0.027(3) 0.048(5) O17 0.155(7) 0.066(5) 0.086(5) 0.032(4) 0.061(5) 0.081(5) Cl3 0.060(5) 0.064(3) 0.043(3) 0.009(2) 0.025(3) 0.020(3) O18 0.044(7) 0.096(10) 0.053(7) -0.013(7) 0.011(6) -0.008(7) Cl3' 0.058(5) 0.062(3) 0.042(3) 0.011(2) 0.024(3) 0.017(3) O18' 0.036(6) 0.091(9) 0.052(7) -0.015(6) 0.012(5) 0.004(6) O19 0.167(8) 0.062(5) 0.056(4) 0.015(3) 0.034(4) 0.048(5) O20 0.148(7) 0.080(5) 0.058(4) -0.003(3) 0.054(4) 0.028(5) O21 0.078(4) 0.069(4) 0.046(3) 0.011(3) 0.026(3) -0.008(3) Cl4 0.0219(7) 0.0226(8) 0.0246(7) 0.0020(6) -0.0002(6) 0.0063(6) O22 0.033(3) 0.053(3) 0.028(2) 0.013(2) 0.003(2) 0.012(2) O23 0.035(3) 0.029(3) 0.035(2) -0.0007(19) -0.003(2) 0.019(2) O24 0.030(3) 0.044(3) 0.038(3) 0.006(2) 0.012(2) 0.003(2) O25 0.038(3) 0.023(3) 0.052(3) -0.008(2) -0.008(2) 0.013(2) Cl5 0.0277(8) 0.0259(8) 0.0350(8) 0.0059(6) 0.0144(7) 0.0045(7) O29 0.026(2) 0.035(3) 0.056(3) 0.014(2) 0.019(2) 0.005(2) O26 0.047(4) 0.066(5) 0.078(5) -0.003(4) 0.023(4) 0.012(4) O27 0.050(4) 0.060(5) 0.062(5) 0.004(4) 0.016(4) -0.005(4) O28 0.058(4) 0.057(5) 0.059(4) 0.020(4) 0.018(4) 0.004(4) O26' 0.051(4) 0.058(5) 0.047(4) 0.001(4) 0.030(3) 0.012(4) O27' 0.040(4) 0.071(5) 0.067(5) 0.010(4) 0.013(4) 0.005(4) O28' 0.057(4) 0.040(4) 0.056(4) 0.006(4) 0.021(4) 0.007(4) O1W 0.095(5) 0.050(4) 0.073(4) -0.014(3) 0.046(4) -0.028(4) N1S 0.071(5) 0.037(4) 0.068(5) 0.002(3) 0.034(4) 0.007(4) C1S 0.054(5) 0.037(5) 0.055(5) -0.003(4) 0.011(4) 0.015(4) C2S 0.064(6) 0.048(5) 0.044(4) 0.003(4) 0.009(4) 0.020(4) N2S 0.061(5) 0.045(4) 0.051(4) -0.006(3) 0.024(4) -0.004(4) C3S 0.076(6) 0.034(5) 0.049(5) -0.002(4) 0.032(4) 0.003(4) C4S 0.086(7) 0.054(6) 0.070(6) -0.003(5) 0.043(5) -0.015(5) N3S 0.093(6) 0.060(5) 0.053(4) 0.034(4) 0.037(4) 0.042(4) C5S 0.052(5) 0.057(6) 0.068(6) 0.011(5) 0.029(5) 0.023(4) C6S 0.085(7) 0.094(8) 0.052(5) 0.009(5) 0.024(5) 0.039(6) O1S 0.059(4) 0.084(5) 0.068(4) 0.025(4) -0.002(3) 0.024(4) C11S 0.083(7) 0.061(6) 0.048(5) -0.007(4) 0.003(5) 0.029(5) C12S 0.059(6) 0.081(8) 0.084(7) 0.003(6) -0.001(5) 0.035(6) C13S 0.123(11) 0.125(11) 0.075(7) 0.047(7) 0.034(7) 0.050(9) C14S 0.137(14) 0.198(18) 0.108(11) 0.078(12) 0.022(10) -0.016(13) _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 Yb1 O200 2.192(4) . ? Yb1 O1 2.244(4) . ? Yb1 O3 2.263(4) . ? Yb1 O202 2.284(4) . ? Yb1 N1 2.453(4) . ? Yb1 N9 2.473(4) . ? Yb1 N2 2.557(4) . ? Yb1 N10 2.563(5) . ? Yb2 O4 2.216(4) . ? Yb2 O201 2.232(4) . ? Yb2 O2 2.241(4) . ? Yb2 O203 2.263(4) . ? Yb2 N14 2.460(5) . ? Yb2 N6 2.474(4) . ? Yb2 N5 2.577(4) . ? Yb2 N13 2.616(4) . ? Yb2 H2C 2.6543 . ? Yb2 H2D 2.7579 . ? O1 C16 1.281(6) . ? O2 C30 1.267(7) . ? O3 C50 1.253(7) . ? O4 C64 1.269(7) . ? O200 C200 1.242(7) . ? O201 C200 1.248(7) . ? O202 H2A 0.8501 . ? O202 H2B 0.8501 . ? O203 H2C 0.8500 . ? O203 H2D 0.8497 . ? N1 C11 1.332(7) . ? N1 C15 1.344(7) . ? N2 C10 1.346(7) . ? N2 N3 1.356(6) . ? N3 C8 1.348(7) . ? N3 C7 1.449(7) . ? N4 C22 1.348(7) . ? N4 N5 1.359(6) . ? N4 C21 1.462(7) . ? N5 C24 1.337(7) . ? N6 C29 1.340(7) . ? N6 C25 1.350(7) . ? N7 C16 1.320(7) . ? N7 C17 1.475(7) . ? N7 C19 1.475(7) . ? N8 C30 1.311(8) . ? N8 C31 1.475(8) . ? N8 C33 1.484(7) . ? N9 C49 1.340(7) . ? N9 C45 1.349(7) . ? N10 C44 1.347(7) . ? N10 N11 1.352(6) . ? N11 C42 1.341(7) . ? N11 C41 1.481(7) . ? N12 C56 1.345(8) . ? N12 N13 1.351(7) . ? N12 C55 1.473(8) . ? N13 C58 1.349(7) . ? N14 C59 1.335(7) . ? N14 C63 1.337(8) . ? N15 C50 1.330(7) . ? N15 C53 1.475(8) . ? N15 C51 1.481(8) . ? N16 C64 1.320(8) . ? N16 C67 1.473(8) . ? N16 C65 1.483(8) . ? C1 C6 1.377(9) . ? C1 C2 1.407(8) . ? C1 C7 1.516(9) . ? C2 C3 1.391(9) . ? C2 C21 1.500(8) . ? C3 C4 1.389(10) . ? C3 H3 0.9500 . ? C4 C5 1.382(10) . ? C4 H4 0.9500 . ? C5 C6 1.397(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.365(8) . ? C8 H8 0.9500 . ? C9 C10 1.391(8) . ? C9 H9 0.9500 . ? C10 C11 1.461(7) . ? C11 C12 1.403(8) . ? C12 C13 1.381(8) . ? C12 H12 0.9500 . ? C13 C14 1.387(8) . ? C13 H13 0.9500 . ? C14 C15 1.395(8) . ? C14 H14 0.9500 . ? C15 C16 1.486(8) . ? C17 C18 1.523(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.514(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.362(9) . ? C22 H22 0.9500 . ? C23 C24 1.399(8) . ? C23 H23 0.9500 . ? C24 C25 1.461(8) . ? C25 C26 1.400(8) . ? C26 C27 1.377(9) . ? C26 H26 0.9500 . ? C27 C28 1.382(9) . ? C27 H27 0.9500 . ? C28 C29 1.396(8) . ? C28 H28 0.9500 . ? C29 C30 1.499(8) . ? C31 C32 1.447(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.517(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C40 1.401(8) . ? C35 C36 1.404(8) . ? C35 C41 1.512(8) . ? C36 C37 1.373(8) . ? C36 C55 1.511(8) . ? C37 C38 1.384(8) . ? C37 H37 0.9500 . ? C38 C39 1.370(9) . ? C38 H38 0.9500 . ? C39 C40 1.382(9) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.359(8) . ? C42 H42 0.9500 . ? C43 C44 1.403(8) . ? C43 H43 0.9500 . ? C44 C45 1.451(8) . ? C45 C46 1.396(8) . ? C46 C47 1.376(9) . ? C46 H46 0.9500 . ? C47 C48 1.384(8) . ? C47 H47 0.9500 . ? C48 C49 1.390(8) . ? C48 H48 0.9500 . ? C49 C50 1.506(8) . ? C51 C52 1.535(9) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.504(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.363(9) . ? C56 H56 0.9500 . ? C57 C58 1.391(8) . ? C57 H57 0.9500 . ? C58 C59 1.461(9) . ? C59 C60 1.405(8) . ? C60 C61 1.373(10) . ? C60 H60 0.9500 . ? C61 C62 1.382(9) . ? C61 H61 0.9500 . ? C62 C63 1.401(9) . ? C62 H62 0.9500 . ? C63 C64 1.517(8) . ? C65 C66 1.525(10) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.514(11) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C200 C201 1.553(11) . ? C201 H20D 0.9800 . ? C201 H20E 0.9800 . ? C201 H20F 0.9800 . ? Cl1 O11 1.426(5) . ? Cl1 O13 1.432(5) . ? Cl1 O12 1.433(4) . ? Cl1 O10 1.436(6) . ? Cl2 O16 1.406(6) . ? Cl2 O17 1.409(6) . ? Cl2 O14 1.415(5) . ? Cl2 O15 1.448(6) . ? Cl3 O19 1.371(9) . ? Cl3 O21 1.406(8) . ? Cl3 O20 1.389(9) . ? Cl3 O18 1.452(12) . ? Cl3' O20 1.371(9) . ? Cl3' O18' 1.424(11) . ? Cl3' O19 1.412(9) . ? Cl3' O21 1.421(8) . ? Cl4 O23 1.438(4) . ? Cl4 O22 1.440(4) . ? Cl4 O25 1.445(5) . ? Cl4 O24 1.446(5) . ? Cl5 O27' 1.386(9) . ? Cl5 O29 1.425(4) . ? Cl5 O26 1.427(10) . ? Cl5 O28 1.425(9) . ? Cl5 O26' 1.436(8) . ? Cl5 O28' 1.443(9) . ? Cl5 O27 1.454(9) . ? O1W H2W 0.8503 . ? O1W H1W 0.8502 . ? N1S C1S 1.160(10) . ? C1S C2S 1.460(11) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? N2S C3S 1.114(10) . ? C3S C4S 1.467(12) . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? N3S C5S 1.167(10) . ? C5S C6S 1.461(12) . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? O1S C13S 1.437(11) . ? O1S C12S 1.458(11) . ? C11S C12S 1.530(13) . ? C11S H11A 0.9800 . ? C11S H11B 0.9800 . ? C11S H11C 0.9800 . ? C12S H12A 0.9900 . ? C12S H12B 0.9900 . ? C13S C14S 1.534(18) . ? C13S H13A 0.9900 . ? C13S H13B 0.9900 . ? C14S H14A 0.9800 . ? C14S H14B 0.9800 . ? C14S H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O200 Yb1 O1 147.49(14) . . ? O200 Yb1 O3 95.23(14) . . ? O1 Yb1 O3 100.78(14) . . ? O200 Yb1 O202 92.90(15) . . ? O1 Yb1 O202 89.23(14) . . ? O3 Yb1 O202 146.37(14) . . ? O200 Yb1 N1 145.79(14) . . ? O1 Yb1 N1 66.57(14) . . ? O3 Yb1 N1 73.27(15) . . ? O202 Yb1 N1 81.79(15) . . ? O200 Yb1 N9 86.43(14) . . ? O1 Yb1 N9 75.16(14) . . ? O3 Yb1 N9 65.20(14) . . ? O202 Yb1 N9 148.04(14) . . ? N1 Yb1 N9 115.44(15) . . ? O200 Yb1 N2 81.11(14) . . ? O1 Yb1 N2 130.57(14) . . ? O3 Yb1 N2 73.21(14) . . ? O202 Yb1 N2 75.93(15) . . ? N1 Yb1 N2 64.78(14) . . ? N9 Yb1 N2 135.11(15) . . ? O200 Yb1 N10 76.65(14) . . ? O1 Yb1 N10 71.31(14) . . ? O3 Yb1 N10 129.58(14) . . ? O202 Yb1 N10 84.04(15) . . ? N1 Yb1 N10 135.53(14) . . ? N9 Yb1 N10 64.68(15) . . ? N2 Yb1 N10 149.14(15) . . ? O4 Yb2 O201 89.79(15) . . ? O4 Yb2 O2 102.30(15) . . ? O201 Yb2 O2 147.57(13) . . ? O4 Yb2 O203 147.25(14) . . ? O201 Yb2 O203 93.07(15) . . ? O2 Yb2 O203 92.53(15) . . ? O4 Yb2 N14 65.43(15) . . ? O201 Yb2 N14 81.02(15) . . ? O2 Yb2 N14 77.09(15) . . ? O203 Yb2 N14 147.16(15) . . ? O4 Yb2 N6 75.44(15) . . ? O201 Yb2 N6 146.94(14) . . ? O2 Yb2 N6 65.43(14) . . ? O203 Yb2 N6 84.79(15) . . ? N14 Yb2 N6 117.23(16) . . ? O4 Yb2 N5 71.91(15) . . ? O201 Yb2 N5 82.55(14) . . ? O2 Yb2 N5 129.75(14) . . ? O203 Yb2 N5 76.14(15) . . ? N14 Yb2 N5 134.04(16) . . ? N6 Yb2 N5 64.87(15) . . ? O4 Yb2 N13 130.98(15) . . ? O201 Yb2 N13 78.38(14) . . ? O2 Yb2 N13 70.93(14) . . ? O203 Yb2 N13 81.39(14) . . ? N14 Yb2 N13 65.77(16) . . ? N6 Yb2 N13 133.36(15) . . ? N5 Yb2 N13 149.55(15) . . ? O4 Yb2 H2C 131.1 . . ? O201 Yb2 H2C 85.7 . . ? O2 Yb2 H2C 107.2 . . ? O203 Yb2 H2C 17.7 . . ? N14 Yb2 H2C 158.9 . . ? N6 Yb2 H2C 82.4 . . ? N5 Yb2 H2C 59.2 . . ? N13 Yb2 H2C 95.6 . . ? O4 Yb2 H2D 148.1 . . ? O201 Yb2 H2D 107.9 . . ? O2 Yb2 H2D 77.0 . . ? O203 Yb2 H2D 15.9 . . ? N14 Yb2 H2D 141.8 . . ? N6 Yb2 H2D 75.5 . . ? N5 Yb2 H2D 84.1 . . ? N13 Yb2 H2D 79.5 . . ? H2C Yb2 H2D 31.0 . . ? C16 O1 Yb1 124.8(3) . . ? C30 O2 Yb2 127.3(4) . . ? C50 O3 Yb1 125.9(4) . . ? C64 O4 Yb2 129.1(4) . . ? C200 O200 Yb1 146.1(4) . . ? C200 O201 Yb2 149.5(4) . . ? Yb1 O202 H2A 121.6 . . ? Yb1 O202 H2B 116.8 . . ? H2A O202 H2B 117.0 . . ? Yb2 O203 H2C 108.2 . . ? Yb2 O203 H2D 117.3 . . ? H2C O203 H2D 116.9 . . ? C11 N1 C15 119.6(5) . . ? C11 N1 Yb1 120.4(3) . . ? C15 N1 Yb1 116.7(4) . . ? C10 N2 N3 104.6(4) . . ? C10 N2 Yb1 116.4(3) . . ? N3 N2 Yb1 138.9(3) . . ? C8 N3 N2 111.5(5) . . ? C8 N3 C7 126.7(5) . . ? N2 N3 C7 121.7(4) . . ? C22 N4 N5 111.7(5) . . ? C22 N4 C21 125.5(5) . . ? N5 N4 C21 122.4(4) . . ? C24 N5 N4 104.5(4) . . ? C24 N5 Yb2 116.8(4) . . ? N4 N5 Yb2 138.7(3) . . ? C29 N6 C25 119.2(5) . . ? C29 N6 Yb2 117.8(3) . . ? C25 N6 Yb2 120.7(4) . . ? C16 N7 C17 117.7(5) . . ? C16 N7 C19 124.9(5) . . ? C17 N7 C19 116.8(4) . . ? C30 N8 C31 117.9(5) . . ? C30 N8 C33 127.2(5) . . ? C31 N8 C33 114.5(5) . . ? C49 N9 C45 118.9(5) . . ? C49 N9 Yb1 119.0(3) . . ? C45 N9 Yb1 120.1(4) . . ? C44 N10 N11 104.6(4) . . ? C44 N10 Yb1 114.3(4) . . ? N11 N10 Yb1 136.9(3) . . ? C42 N11 N10 111.4(5) . . ? C42 N11 C41 128.5(5) . . ? N10 N11 C41 119.6(4) . . ? C56 N12 N13 111.2(5) . . ? C56 N12 C55 126.4(5) . . ? N13 N12 C55 122.4(5) . . ? C58 N13 N12 104.5(4) . . ? C58 N13 Yb2 111.6(4) . . ? N12 N13 Yb2 135.2(3) . . ? C59 N14 C63 120.0(5) . . ? C59 N14 Yb2 120.9(4) . . ? C63 N14 Yb2 119.0(4) . . ? C50 N15 C53 126.1(5) . . ? C50 N15 C51 116.1(5) . . ? C53 N15 C51 116.8(5) . . ? C64 N16 C67 128.0(5) . . ? C64 N16 C65 117.7(5) . . ? C67 N16 C65 114.3(5) . . ? C6 C1 C2 120.0(6) . . ? C6 C1 C7 122.3(5) . . ? C2 C1 C7 117.7(5) . . ? C3 C2 C1 119.0(6) . . ? C3 C2 C21 122.5(6) . . ? C1 C2 C21 118.5(5) . . ? C2 C3 C4 120.7(6) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 120.0(7) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 119.7(6) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C1 C6 C5 120.6(6) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? N3 C7 C1 113.4(5) . . ? N3 C7 H7A 108.9 . . ? C1 C7 H7A 108.9 . . ? N3 C7 H7B 108.9 . . ? C1 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N3 C8 C9 107.6(5) . . ? N3 C8 H8 126.2 . . ? C9 C8 H8 126.2 . . ? C8 C9 C10 105.2(5) . . ? C8 C9 H9 127.4 . . ? C10 C9 H9 127.4 . . ? N2 C10 C9 111.1(5) . . ? N2 C10 C11 118.1(5) . . ? C9 C10 C11 130.7(5) . . ? N1 C11 C12 121.8(5) . . ? N1 C11 C10 115.7(5) . . ? C12 C11 C10 122.5(5) . . ? C13 C12 C11 118.3(5) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C12 C13 C14 120.0(6) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 118.1(5) . . ? C13 C14 H14 120.9 . . ? C15 C14 H14 120.9 . . ? N1 C15 C14 121.9(5) . . ? N1 C15 C16 111.1(5) . . ? C14 C15 C16 126.7(5) . . ? O1 C16 N7 119.6(5) . . ? O1 C16 C15 115.8(5) . . ? N7 C16 C15 124.5(5) . . ? N7 C17 C18 112.5(5) . . ? N7 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? N7 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N7 C19 C20 112.1(5) . . ? N7 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N7 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N4 C21 C2 112.8(5) . . ? N4 C21 H21A 109.0 . . ? C2 C21 H21A 109.0 . . ? N4 C21 H21B 109.0 . . ? C2 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? N4 C22 C23 107.5(5) . . ? N4 C22 H22 126.3 . . ? C23 C22 H22 126.3 . . ? C22 C23 C24 105.1(5) . . ? C22 C23 H23 127.4 . . ? C24 C23 H23 127.4 . . ? N5 C24 C23 111.2(5) . . ? N5 C24 C25 119.1(5) . . ? C23 C24 C25 129.6(5) . . ? N6 C25 C26 121.6(5) . . ? N6 C25 C24 116.0(5) . . ? C26 C25 C24 122.4(5) . . ? C27 C26 C25 118.6(6) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C26 C27 C28 119.9(6) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C29 118.7(6) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? N6 C29 C28 121.8(5) . . ? N6 C29 C30 110.7(5) . . ? C28 C29 C30 127.4(5) . . ? O2 C30 N8 119.8(5) . . ? O2 C30 C29 115.8(5) . . ? N8 C30 C29 124.4(5) . . ? C32 C31 N8 111.6(8) . . ? C32 C31 H31A 109.3 . . ? N8 C31 H31A 109.3 . . ? C32 C31 H31B 109.3 . . ? N8 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N8 C33 C34 112.2(6) . . ? N8 C33 H33A 109.2 . . ? C34 C33 H33A 109.2 . . ? N8 C33 H33B 109.2 . . ? C34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 119.4(5) . . ? C40 C35 C41 118.1(5) . . ? C36 C35 C41 122.5(5) . . ? C37 C36 C35 118.1(5) . . ? C37 C36 C55 119.0(6) . . ? C35 C36 C55 122.9(5) . . ? C36 C37 C38 122.2(6) . . ? C36 C37 H37 118.9 . . ? C38 C37 H37 118.9 . . ? C39 C38 C37 120.1(6) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 119.1(6) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? C39 C40 C35 121.0(6) . . ? C39 C40 H40 119.5 . . ? C35 C40 H40 119.5 . . ? N11 C41 C35 110.6(5) . . ? N11 C41 H41A 109.5 . . ? C35 C41 H41A 109.5 . . ? N11 C41 H41B 109.5 . . ? C35 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? N11 C42 C43 108.6(5) . . ? N11 C42 H42 125.7 . . ? C43 C42 H42 125.7 . . ? C42 C43 C44 104.4(5) . . ? C42 C43 H43 127.8 . . ? C44 C43 H43 127.8 . . ? N10 C44 C43 111.0(5) . . ? N10 C44 C45 119.7(5) . . ? C43 C44 C45 129.3(5) . . ? N9 C45 C46 121.5(5) . . ? N9 C45 C44 115.3(5) . . ? C46 C45 C44 123.2(5) . . ? C47 C46 C45 118.9(5) . . ? C47 C46 H46 120.6 . . ? C45 C46 H46 120.6 . . ? C46 C47 C48 119.9(6) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C47 C48 C49 118.2(6) . . ? C47 C48 H48 120.9 . . ? C49 C48 H48 120.9 . . ? N9 C49 C48 122.6(5) . . ? N9 C49 C50 110.0(5) . . ? C48 C49 C50 127.1(5) . . ? O3 C50 N15 120.5(5) . . ? O3 C50 C49 116.1(5) . . ? N15 C50 C49 123.3(5) . . ? N15 C51 C52 111.4(5) . . ? N15 C51 H51A 109.4 . . ? C52 C51 H51A 109.4 . . ? N15 C51 H51B 109.4 . . ? C52 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N15 C53 C54 112.9(6) . . ? N15 C53 H53A 109.0 . . ? C54 C53 H53A 109.0 . . ? N15 C53 H53B 109.0 . . ? C54 C53 H53B 109.0 . . ? H53A C53 H53B 107.8 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N12 C55 C36 112.8(5) . . ? N12 C55 H55A 109.0 . . ? C36 C55 H55A 109.0 . . ? N12 C55 H55B 109.0 . . ? C36 C55 H55B 109.0 . . ? H55A C55 H55B 107.8 . . ? N12 C56 C57 108.4(5) . . ? N12 C56 H56 125.8 . . ? C57 C56 H56 125.8 . . ? C56 C57 C58 104.4(5) . . ? C56 C57 H57 127.8 . . ? C58 C57 H57 127.8 . . ? N13 C58 C57 111.4(5) . . ? N13 C58 C59 119.3(5) . . ? C57 C58 C59 129.3(5) . . ? N14 C59 C60 122.3(6) . . ? N14 C59 C58 116.8(5) . . ? C60 C59 C58 120.9(5) . . ? C61 C60 C59 117.6(6) . . ? C61 C60 H60 121.2 . . ? C59 C60 H60 121.2 . . ? C60 C61 C62 120.4(6) . . ? C60 C61 H61 119.8 . . ? C62 C61 H61 119.8 . . ? C61 C62 C63 118.8(6) . . ? C61 C62 H62 120.6 . . ? C63 C62 H62 120.6 . . ? N14 C63 C62 120.8(6) . . ? N14 C63 C64 111.2(5) . . ? C62 C63 C64 127.9(6) . . ? O4 C64 N16 118.9(5) . . ? O4 C64 C63 114.8(5) . . ? N16 C64 C63 126.3(6) . . ? N16 C65 C66 110.9(6) . . ? N16 C65 H65A 109.5 . . ? C66 C65 H65A 109.5 . . ? N16 C65 H65B 109.5 . . ? C66 C65 H65B 109.5 . . ? H65A C65 H65B 108.1 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N16 C67 C68 111.2(6) . . ? N16 C67 H67A 109.4 . . ? C68 C67 H67A 109.4 . . ? N16 C67 H67B 109.4 . . ? C68 C67 H67B 109.4 . . ? H67A C67 H67B 108.0 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O200 C200 O201 124.3(6) . . ? O200 C200 C201 113.4(6) . . ? O201 C200 C201 121.3(6) . . ? C200 C201 H20D 109.5 . . ? C200 C201 H20E 109.5 . . ? H20D C201 H20E 109.5 . . ? C200 C201 H20F 109.5 . . ? H20D C201 H20F 109.5 . . ? H20E C201 H20F 109.5 . . ? O11 Cl1 O13 109.5(3) . . ? O11 Cl1 O12 110.3(3) . . ? O13 Cl1 O12 111.2(3) . . ? O11 Cl1 O10 108.7(4) . . ? O13 Cl1 O10 109.0(4) . . ? O12 Cl1 O10 108.1(3) . . ? O16 Cl2 O17 109.3(4) . . ? O16 Cl2 O14 110.5(4) . . ? O17 Cl2 O14 109.6(4) . . ? O16 Cl2 O15 110.8(4) . . ? O17 Cl2 O15 106.2(5) . . ? O14 Cl2 O15 110.5(4) . . ? O19 Cl3 O21 117.3(6) . . ? O19 Cl3 O20 117.6(6) . . ? O21 Cl3 O20 115.2(6) . . ? O19 Cl3 O18 98.0(8) . . ? O21 Cl3 O18 105.1(7) . . ? O20 Cl3 O18 98.7(7) . . ? O20 Cl3' O18' 101.6(7) . . ? O20 Cl3' O19 116.0(6) . . ? O18' Cl3' O19 98.9(8) . . ? O20 Cl3' O21 115.4(6) . . ? O18' Cl3' O21 108.8(7) . . ? O19 Cl3' O21 113.6(6) . . ? Cl3 O19 Cl3' 23.7(4) . . ? Cl3' O20 Cl3 24.0(4) . . ? Cl3 O21 Cl3' 23.4(4) . . ? O23 Cl4 O22 109.9(3) . . ? O23 Cl4 O25 109.3(3) . . ? O22 Cl4 O25 110.2(3) . . ? O23 Cl4 O24 110.0(3) . . ? O22 Cl4 O24 109.0(3) . . ? O25 Cl4 O24 108.4(3) . . ? O27' Cl5 O29 111.3(5) . . ? O27' Cl5 O26 54.8(7) . . ? O29 Cl5 O26 113.0(5) . . ? O27' Cl5 O28 132.8(7) . . ? O29 Cl5 O28 115.5(5) . . ? O26 Cl5 O28 109.1(7) . . ? O27' Cl5 O26' 110.3(7) . . ? O29 Cl5 O26' 107.0(5) . . ? O26 Cl5 O26' 57.3(6) . . ? O28 Cl5 O26' 61.2(7) . . ? O27' Cl5 O28' 116.7(7) . . ? O29 Cl5 O28' 105.1(5) . . ? O26 Cl5 O28' 141.4(7) . . ? O28 Cl5 O28' 44.7(6) . . ? O26' Cl5 O28' 105.9(6) . . ? O27' Cl5 O27 50.6(7) . . ? O29 Cl5 O27 109.2(5) . . ? O26 Cl5 O27 102.8(7) . . ? O28 Cl5 O27 106.3(7) . . ? O26' Cl5 O27 143.5(6) . . ? O28' Cl5 O27 69.4(7) . . ? H2W O1W H1W 125.4 . . ? N1S C1S C2S 177.4(9) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N2S C3S C4S 178.8(9) . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? N3S C5S C6S 177.2(9) . . ? C5S C6S H6S1 109.5 . . ? C5S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? C13S O1S C12S 111.9(8) . . ? C12S C11S H11A 109.5 . . ? C12S C11S H11B 109.5 . . ? H11A C11S H11B 109.5 . . ? C12S C11S H11C 109.5 . . ? H11A C11S H11C 109.5 . . ? H11B C11S H11C 109.5 . . ? O1S C12S C11S 110.8(7) . . ? O1S C12S H12A 109.5 . . ? C11S C12S H12A 109.5 . . ? O1S C12S H12B 109.5 . . ? C11S C12S H12B 109.5 . . ? H12A C12S H12B 108.1 . . ? O1S C13S C14S 109.0(10) . . ? O1S C13S H13A 109.9 . . ? C14S C13S H13A 109.9 . . ? O1S C13S H13B 109.9 . . ? C14S C13S H13B 109.9 . . ? H13A C13S H13B 108.3 . . ? C13S C14S H14A 109.5 . . ? C13S C14S H14B 109.5 . . ? H14A C14S H14B 109.5 . . ? C13S C14S H14C 109.5 . . ? H14A C14S H14C 109.5 . . ? H14B C14S H14C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O200 Yb1 O1 C16 -171.0(4) . . . . ? O3 Yb1 O1 C16 70.9(4) . . . . ? O202 Yb1 O1 C16 -76.8(4) . . . . ? N1 Yb1 O1 C16 4.6(4) . . . . ? N9 Yb1 O1 C16 131.4(4) . . . . ? N2 Yb1 O1 C16 -6.2(5) . . . . ? N10 Yb1 O1 C16 -160.8(5) . . . . ? O4 Yb2 O2 C30 -68.0(5) . . . . ? O201 Yb2 O2 C30 -177.6(4) . . . . ? O203 Yb2 O2 C30 82.6(5) . . . . ? N14 Yb2 O2 C30 -128.8(5) . . . . ? N6 Yb2 O2 C30 -0.5(5) . . . . ? N5 Yb2 O2 C30 8.6(6) . . . . ? N13 Yb2 O2 C30 162.6(5) . . . . ? O200 Yb1 O3 C50 -72.2(4) . . . . ? O1 Yb1 O3 C50 79.4(4) . . . . ? O202 Yb1 O3 C50 -175.4(4) . . . . ? N1 Yb1 O3 C50 140.7(4) . . . . ? N9 Yb1 O3 C50 11.4(4) . . . . ? N2 Yb1 O3 C50 -151.2(4) . . . . ? N10 Yb1 O3 C50 4.8(5) . . . . ? O201 Yb2 O4 C64 75.5(5) . . . . ? O2 Yb2 O4 C64 -74.1(5) . . . . ? O203 Yb2 O4 C64 170.9(4) . . . . ? N14 Yb2 O4 C64 -4.7(5) . . . . ? N6 Yb2 O4 C64 -134.4(5) . . . . ? N5 Yb2 O4 C64 157.8(5) . . . . ? N13 Yb2 O4 C64 1.2(6) . . . . ? O1 Yb1 O200 C200 -47.5(8) . . . . ? O3 Yb1 O200 C200 72.1(7) . . . . ? O202 Yb1 O200 C200 -140.6(7) . . . . ? N1 Yb1 O200 C200 139.8(7) . . . . ? N9 Yb1 O200 C200 7.4(7) . . . . ? N2 Yb1 O200 C200 144.1(7) . . . . ? N10 Yb1 O200 C200 -57.4(7) . . . . ? O4 Yb2 O201 C200 -45.5(8) . . . . ? O2 Yb2 O201 C200 67.6(9) . . . . ? O203 Yb2 O201 C200 167.2(8) . . . . ? N14 Yb2 O201 C200 19.7(8) . . . . ? N6 Yb2 O201 C200 -107.7(8) . . . . ? N5 Yb2 O201 C200 -117.2(8) . . . . ? N13 Yb2 O201 C200 86.6(8) . . . . ? O200 Yb1 N1 C11 -14.5(6) . . . . ? O1 Yb1 N1 C11 169.7(5) . . . . ? O3 Yb1 N1 C11 59.7(4) . . . . ? O202 Yb1 N1 C11 -97.5(4) . . . . ? N9 Yb1 N1 C11 110.8(4) . . . . ? N2 Yb1 N1 C11 -19.3(4) . . . . ? N10 Yb1 N1 C11 -170.3(4) . . . . ? O200 Yb1 N1 C15 -173.8(4) . . . . ? O1 Yb1 N1 C15 10.5(4) . . . . ? O3 Yb1 N1 C15 -99.6(4) . . . . ? O202 Yb1 N1 C15 103.2(4) . . . . ? N9 Yb1 N1 C15 -48.5(4) . . . . ? N2 Yb1 N1 C15 -178.5(4) . . . . ? N10 Yb1 N1 C15 30.4(5) . . . . ? O200 Yb1 N2 C10 -165.6(4) . . . . ? O1 Yb1 N2 C10 22.6(5) . . . . ? O3 Yb1 N2 C10 -67.4(4) . . . . ? O202 Yb1 N2 C10 99.1(4) . . . . ? N1 Yb1 N2 C10 11.7(4) . . . . ? N9 Yb1 N2 C10 -89.9(4) . . . . ? N10 Yb1 N2 C10 150.2(4) . . . . ? O200 Yb1 N2 N3 11.9(5) . . . . ? O1 Yb1 N2 N3 -159.9(5) . . . . ? O3 Yb1 N2 N3 110.1(6) . . . . ? O202 Yb1 N2 N3 -83.4(6) . . . . ? N1 Yb1 N2 N3 -170.8(6) . . . . ? N9 Yb1 N2 N3 87.6(6) . . . . ? N10 Yb1 N2 N3 -32.3(7) . . . . ? C10 N2 N3 C8 0.0(7) . . . . ? Yb1 N2 N3 C8 -177.7(4) . . . . ? C10 N2 N3 C7 176.8(5) . . . . ? Yb1 N2 N3 C7 -0.9(9) . . . . ? C22 N4 N5 C24 0.1(7) . . . . ? C21 N4 N5 C24 -173.3(5) . . . . ? C22 N4 N5 Yb2 178.3(5) . . . . ? C21 N4 N5 Yb2 5.0(9) . . . . ? O4 Yb2 N5 C24 73.7(4) . . . . ? O201 Yb2 N5 C24 165.9(4) . . . . ? O2 Yb2 N5 C24 -17.4(5) . . . . ? O203 Yb2 N5 C24 -99.0(4) . . . . ? N14 Yb2 N5 C24 96.1(4) . . . . ? N6 Yb2 N5 C24 -8.3(4) . . . . ? N13 Yb2 N5 C24 -142.6(4) . . . . ? O4 Yb2 N5 N4 -104.4(6) . . . . ? O201 Yb2 N5 N4 -12.2(6) . . . . ? O2 Yb2 N5 N4 164.5(5) . . . . ? O203 Yb2 N5 N4 82.9(6) . . . . ? N14 Yb2 N5 N4 -82.0(6) . . . . ? N6 Yb2 N5 N4 173.6(6) . . . . ? N13 Yb2 N5 N4 39.3(7) . . . . ? O4 Yb2 N6 C29 100.4(4) . . . . ? O201 Yb2 N6 C29 166.4(4) . . . . ? O2 Yb2 N6 C29 -10.8(4) . . . . ? O203 Yb2 N6 C29 -106.0(4) . . . . ? N14 Yb2 N6 C29 48.4(5) . . . . ? N5 Yb2 N6 C29 176.9(5) . . . . ? N13 Yb2 N6 C29 -33.0(5) . . . . ? O4 Yb2 N6 C25 -62.2(4) . . . . ? O201 Yb2 N6 C25 3.8(6) . . . . ? O2 Yb2 N6 C25 -173.4(5) . . . . ? O203 Yb2 N6 C25 91.5(4) . . . . ? N14 Yb2 N6 C25 -114.1(4) . . . . ? N5 Yb2 N6 C25 14.3(4) . . . . ? N13 Yb2 N6 C25 164.4(4) . . . . ? O200 Yb1 N9 C49 99.8(4) . . . . ? O1 Yb1 N9 C49 -107.2(4) . . . . ? O3 Yb1 N9 C49 2.4(4) . . . . ? O202 Yb1 N9 C49 -170.4(3) . . . . ? N1 Yb1 N9 C49 -52.8(4) . . . . ? N2 Yb1 N9 C49 26.2(5) . . . . ? N10 Yb1 N9 C49 176.7(4) . . . . ? O200 Yb1 N9 C45 -96.6(4) . . . . ? O1 Yb1 N9 C45 56.3(4) . . . . ? O3 Yb1 N9 C45 165.9(4) . . . . ? O202 Yb1 N9 C45 -6.9(5) . . . . ? N1 Yb1 N9 C45 110.8(4) . . . . ? N2 Yb1 N9 C45 -170.2(3) . . . . ? N10 Yb1 N9 C45 -19.7(4) . . . . ? O200 Yb1 N10 C44 112.7(4) . . . . ? O1 Yb1 N10 C44 -61.7(4) . . . . ? O3 Yb1 N10 C44 26.9(4) . . . . ? O202 Yb1 N10 C44 -152.9(4) . . . . ? N1 Yb1 N10 C44 -81.0(4) . . . . ? N9 Yb1 N10 C44 20.3(4) . . . . ? N2 Yb1 N10 C44 157.7(3) . . . . ? O200 Yb1 N10 N11 -94.8(5) . . . . ? O1 Yb1 N10 N11 90.8(5) . . . . ? O3 Yb1 N10 N11 179.5(4) . . . . ? O202 Yb1 N10 N11 -0.4(5) . . . . ? N1 Yb1 N10 N11 71.5(5) . . . . ? N9 Yb1 N10 N11 172.8(5) . . . . ? N2 Yb1 N10 N11 -49.8(6) . . . . ? C44 N10 N11 C42 0.6(6) . . . . ? Yb1 N10 N11 C42 -153.6(4) . . . . ? C44 N10 N11 C41 -171.8(5) . . . . ? Yb1 N10 N11 C41 34.0(7) . . . . ? C56 N12 N13 C58 -1.3(6) . . . . ? C55 N12 N13 C58 176.4(5) . . . . ? C56 N12 N13 Yb2 141.9(4) . . . . ? C55 N12 N13 Yb2 -40.4(8) . . . . ? O4 Yb2 N13 C58 -23.6(4) . . . . ? O201 Yb2 N13 C58 -103.0(4) . . . . ? O2 Yb2 N13 C58 66.3(4) . . . . ? O203 Yb2 N13 C58 162.0(4) . . . . ? N14 Yb2 N13 C58 -17.7(4) . . . . ? N6 Yb2 N13 C58 87.7(4) . . . . ? N5 Yb2 N13 C58 -155.3(4) . . . . ? O4 Yb2 N13 N12 -165.0(4) . . . . ? O201 Yb2 N13 N12 115.6(5) . . . . ? O2 Yb2 N13 N12 -75.1(5) . . . . ? O203 Yb2 N13 N12 20.6(5) . . . . ? N14 Yb2 N13 N12 -159.1(5) . . . . ? N6 Yb2 N13 N12 -53.8(6) . . . . ? N5 Yb2 N13 N12 63.2(6) . . . . ? O4 Yb2 N14 C59 -177.3(5) . . . . ? O201 Yb2 N14 C59 88.8(4) . . . . ? O2 Yb2 N14 C59 -67.1(4) . . . . ? O203 Yb2 N14 C59 7.2(6) . . . . ? N6 Yb2 N14 C59 -120.4(4) . . . . ? N5 Yb2 N14 C59 159.2(4) . . . . ? N13 Yb2 N14 C59 7.6(4) . . . . ? O4 Yb2 N14 C63 6.1(4) . . . . ? O201 Yb2 N14 C63 -87.8(4) . . . . ? O2 Yb2 N14 C63 116.3(5) . . . . ? O203 Yb2 N14 C63 -169.4(4) . . . . ? N6 Yb2 N14 C63 63.0(5) . . . . ? N5 Yb2 N14 C63 -17.4(5) . . . . ? N13 Yb2 N14 C63 -169.0(5) . . . . ? C6 C1 C2 C3 0.2(8) . . . . ? C7 C1 C2 C3 178.6(5) . . . . ? C6 C1 C2 C21 -179.3(5) . . . . ? C7 C1 C2 C21 -0.9(7) . . . . ? C1 C2 C3 C4 0.4(9) . . . . ? C21 C2 C3 C4 179.9(6) . . . . ? C2 C3 C4 C5 0.0(10) . . . . ? C3 C4 C5 C6 -1.0(10) . . . . ? C2 C1 C6 C5 -1.2(9) . . . . ? C7 C1 C6 C5 -179.6(5) . . . . ? C4 C5 C6 C1 1.6(10) . . . . ? C8 N3 C7 C1 85.6(7) . . . . ? N2 N3 C7 C1 -90.6(6) . . . . ? C6 C1 C7 N3 -4.1(8) . . . . ? C2 C1 C7 N3 177.5(5) . . . . ? N2 N3 C8 C9 0.6(7) . . . . ? C7 N3 C8 C9 -176.0(6) . . . . ? N3 C8 C9 C10 -1.0(7) . . . . ? N3 N2 C10 C9 -0.7(7) . . . . ? Yb1 N2 C10 C9 177.6(4) . . . . ? N3 N2 C10 C11 176.9(5) . . . . ? Yb1 N2 C10 C11 -4.7(7) . . . . ? C8 C9 C10 N2 1.0(7) . . . . ? C8 C9 C10 C11 -176.2(6) . . . . ? C15 N1 C11 C12 3.4(8) . . . . ? Yb1 N1 C11 C12 -155.3(4) . . . . ? C15 N1 C11 C10 -176.8(5) . . . . ? Yb1 N1 C11 C10 24.5(6) . . . . ? N2 C10 C11 N1 -12.2(8) . . . . ? C9 C10 C11 N1 164.8(6) . . . . ? N2 C10 C11 C12 167.5(6) . . . . ? C9 C10 C11 C12 -15.4(10) . . . . ? N1 C11 C12 C13 0.7(9) . . . . ? C10 C11 C12 C13 -179.1(6) . . . . ? C11 C12 C13 C14 -3.0(9) . . . . ? C12 C13 C14 C15 1.3(9) . . . . ? C11 N1 C15 C14 -5.3(8) . . . . ? Yb1 N1 C15 C14 154.1(5) . . . . ? C11 N1 C15 C16 179.3(5) . . . . ? Yb1 N1 C15 C16 -21.3(6) . . . . ? C13 C14 C15 N1 3.0(9) . . . . ? C13 C14 C15 C16 177.6(6) . . . . ? Yb1 O1 C16 N7 160.3(4) . . . . ? Yb1 O1 C16 C15 -17.6(7) . . . . ? C17 N7 C16 O1 4.0(8) . . . . ? C19 N7 C16 O1 -166.4(5) . . . . ? C17 N7 C16 C15 -178.3(5) . . . . ? C19 N7 C16 C15 11.3(9) . . . . ? N1 C15 C16 O1 25.0(7) . . . . ? C14 C15 C16 O1 -150.1(6) . . . . ? N1 C15 C16 N7 -152.8(5) . . . . ? C14 C15 C16 N7 32.1(9) . . . . ? C16 N7 C17 C18 -80.8(7) . . . . ? C19 N7 C17 C18 90.3(6) . . . . ? C16 N7 C19 C20 -110.4(6) . . . . ? C17 N7 C19 C20 79.2(6) . . . . ? C22 N4 C21 C2 -80.4(7) . . . . ? N5 N4 C21 C2 92.0(6) . . . . ? C3 C2 C21 N4 -2.4(8) . . . . ? C1 C2 C21 N4 177.1(5) . . . . ? N5 N4 C22 C23 -0.1(8) . . . . ? C21 N4 C22 C23 173.0(6) . . . . ? N4 C22 C23 C24 0.0(8) . . . . ? N4 N5 C24 C23 -0.1(7) . . . . ? Yb2 N5 C24 C23 -178.8(4) . . . . ? N4 N5 C24 C25 -178.6(5) . . . . ? Yb2 N5 C24 C25 2.7(7) . . . . ? C22 C23 C24 N5 0.0(8) . . . . ? C22 C23 C24 C25 178.3(6) . . . . ? C29 N6 C25 C26 -0.5(8) . . . . ? Yb2 N6 C25 C26 161.8(5) . . . . ? C29 N6 C25 C24 179.0(5) . . . . ? Yb2 N6 C25 C24 -18.7(7) . . . . ? N5 C24 C25 N6 10.0(8) . . . . ? C23 C24 C25 N6 -168.2(6) . . . . ? N5 C24 C25 C26 -170.5(6) . . . . ? C23 C24 C25 C26 11.3(10) . . . . ? N6 C25 C26 C27 -3.4(9) . . . . ? C24 C25 C26 C27 177.2(6) . . . . ? C25 C26 C27 C28 2.6(10) . . . . ? C26 C27 C28 C29 1.8(10) . . . . ? C25 N6 C29 C28 5.2(9) . . . . ? Yb2 N6 C29 C28 -157.6(5) . . . . ? C25 N6 C29 C30 -178.8(5) . . . . ? Yb2 N6 C29 C30 18.3(6) . . . . ? C27 C28 C29 N6 -5.9(9) . . . . ? C27 C28 C29 C30 178.8(6) . . . . ? Yb2 O2 C30 N8 -168.7(4) . . . . ? Yb2 O2 C30 C29 10.3(8) . . . . ? C31 N8 C30 O2 -4.5(10) . . . . ? C33 N8 C30 O2 167.2(6) . . . . ? C31 N8 C30 C29 176.6(7) . . . . ? C33 N8 C30 C29 -11.7(11) . . . . ? N6 C29 C30 O2 -18.5(8) . . . . ? C28 C29 C30 O2 157.2(6) . . . . ? N6 C29 C30 N8 160.5(6) . . . . ? C28 C29 C30 N8 -23.8(10) . . . . ? C30 N8 C31 C32 84.5(9) . . . . ? C33 N8 C31 C32 -88.3(8) . . . . ? C30 N8 C33 C34 108.4(8) . . . . ? C31 N8 C33 C34 -79.7(8) . . . . ? C40 C35 C36 C37 0.1(8) . . . . ? C41 C35 C36 C37 178.1(5) . . . . ? C40 C35 C36 C55 177.4(5) . . . . ? C41 C35 C36 C55 -4.6(9) . . . . ? C35 C36 C37 C38 -0.1(9) . . . . ? C55 C36 C37 C38 -177.5(6) . . . . ? C36 C37 C38 C39 0.5(9) . . . . ? C37 C38 C39 C40 -0.9(9) . . . . ? C38 C39 C40 C35 0.9(9) . . . . ? C36 C35 C40 C39 -0.5(9) . . . . ? C41 C35 C40 C39 -178.6(5) . . . . ? C42 N11 C41 C35 6.1(9) . . . . ? N10 N11 C41 C35 177.0(5) . . . . ? C40 C35 C41 N11 86.5(7) . . . . ? C36 C35 C41 N11 -91.5(7) . . . . ? N10 N11 C42 C43 0.2(7) . . . . ? C41 N11 C42 C43 171.7(6) . . . . ? N11 C42 C43 C44 -0.9(6) . . . . ? N11 N10 C44 C43 -1.2(6) . . . . ? Yb1 N10 C44 C43 159.8(4) . . . . ? N11 N10 C44 C45 177.9(5) . . . . ? Yb1 N10 C44 C45 -21.1(6) . . . . ? C42 C43 C44 N10 1.3(7) . . . . ? C42 C43 C44 C45 -177.7(6) . . . . ? C49 N9 C45 C46 -0.3(8) . . . . ? Yb1 N9 C45 C46 -163.8(4) . . . . ? C49 N9 C45 C44 -179.4(5) . . . . ? Yb1 N9 C45 C44 17.0(6) . . . . ? N10 C44 C45 N9 3.9(7) . . . . ? C43 C44 C45 N9 -177.2(5) . . . . ? N10 C44 C45 C46 -175.3(5) . . . . ? C43 C44 C45 C46 3.6(9) . . . . ? N9 C45 C46 C47 2.0(8) . . . . ? C44 C45 C46 C47 -178.9(6) . . . . ? C45 C46 C47 C48 -1.7(9) . . . . ? C46 C47 C48 C49 -0.2(9) . . . . ? C45 N9 C49 C48 -1.7(8) . . . . ? Yb1 N9 C49 C48 162.0(4) . . . . ? C45 N9 C49 C50 -175.9(4) . . . . ? Yb1 N9 C49 C50 -12.1(5) . . . . ? C47 C48 C49 N9 2.0(9) . . . . ? C47 C48 C49 C50 175.0(6) . . . . ? Yb1 O3 C50 N15 159.1(4) . . . . ? Yb1 O3 C50 C49 -22.3(6) . . . . ? C53 N15 C50 O3 -161.4(5) . . . . ? C51 N15 C50 O3 7.1(8) . . . . ? C53 N15 C50 C49 20.1(9) . . . . ? C51 N15 C50 C49 -171.4(5) . . . . ? N9 C49 C50 O3 21.1(7) . . . . ? C48 C49 C50 O3 -152.7(6) . . . . ? N9 C49 C50 N15 -160.4(5) . . . . ? C48 C49 C50 N15 25.8(9) . . . . ? C50 N15 C51 C52 76.5(7) . . . . ? C53 N15 C51 C52 -113.9(6) . . . . ? C50 N15 C53 C54 -120.9(7) . . . . ? C51 N15 C53 C54 70.7(7) . . . . ? C56 N12 C55 C36 46.1(8) . . . . ? N13 N12 C55 C36 -131.1(6) . . . . ? C37 C36 C55 N12 -106.0(7) . . . . ? C35 C36 C55 N12 76.7(7) . . . . ? N13 N12 C56 C57 1.1(7) . . . . ? C55 N12 C56 C57 -176.4(5) . . . . ? N12 C56 C57 C58 -0.4(7) . . . . ? N12 N13 C58 C57 1.0(6) . . . . ? Yb2 N13 C58 C57 -152.0(4) . . . . ? N12 N13 C58 C59 -179.6(5) . . . . ? Yb2 N13 C58 C59 27.4(6) . . . . ? C56 C57 C58 N13 -0.4(7) . . . . ? C56 C57 C58 C59 -179.7(6) . . . . ? C63 N14 C59 C60 2.4(9) . . . . ? Yb2 N14 C59 C60 -174.1(4) . . . . ? C63 N14 C59 C58 179.5(5) . . . . ? Yb2 N14 C59 C58 3.0(7) . . . . ? N13 C58 C59 N14 -22.0(8) . . . . ? C57 C58 C59 N14 157.4(6) . . . . ? N13 C58 C59 C60 155.2(5) . . . . ? C57 C58 C59 C60 -25.5(9) . . . . ? N14 C59 C60 C61 0.9(10) . . . . ? C58 C59 C60 C61 -176.1(6) . . . . ? C59 C60 C61 C62 -3.5(11) . . . . ? C60 C61 C62 C63 2.9(12) . . . . ? C59 N14 C63 C62 -3.1(9) . . . . ? Yb2 N14 C63 C62 173.5(5) . . . . ? C59 N14 C63 C64 176.5(5) . . . . ? Yb2 N14 C63 C64 -6.9(7) . . . . ? C61 C62 C63 N14 0.4(11) . . . . ? C61 C62 C63 C64 -179.0(7) . . . . ? Yb2 O4 C64 N16 -176.3(4) . . . . ? Yb2 O4 C64 C63 2.8(8) . . . . ? C67 N16 C64 O4 -178.7(6) . . . . ? C65 N16 C64 O4 -1.0(9) . . . . ? C67 N16 C64 C63 2.4(11) . . . . ? C65 N16 C64 C63 -179.9(6) . . . . ? N14 C63 C64 O4 3.2(8) . . . . ? C62 C63 C64 O4 -177.3(7) . . . . ? N14 C63 C64 N16 -177.9(6) . . . . ? C62 C63 C64 N16 1.7(11) . . . . ? C64 N16 C65 C66 -91.8(7) . . . . ? C67 N16 C65 C66 86.2(7) . . . . ? C64 N16 C67 C68 -88.5(8) . . . . ? C65 N16 C67 C68 93.7(7) . . . . ? Yb1 O200 C200 O201 130.9(6) . . . . ? Yb1 O200 C200 C201 -60.2(9) . . . . ? Yb2 O201 C200 O200 -160.8(5) . . . . ? Yb2 O201 C200 C201 31.2(11) . . . . ? O21 Cl3 O19 Cl3' -74.2(12) . . . . ? O20 Cl3 O19 Cl3' 70.0(13) . . . . ? O18 Cl3 O19 Cl3' 174.2(16) . . . . ? O20 Cl3' O19 Cl3 -69.8(12) . . . . ? O18' Cl3' O19 Cl3 -177.4(16) . . . . ? O21 Cl3' O19 Cl3 67.4(12) . . . . ? O18' Cl3' O20 Cl3 172.5(18) . . . . ? O19 Cl3' O20 Cl3 66.5(13) . . . . ? O21 Cl3' O20 Cl3 -70.0(13) . . . . ? O19 Cl3 O20 Cl3' -73.4(13) . . . . ? O21 Cl3 O20 Cl3' 71.5(13) . . . . ? O18 Cl3 O20 Cl3' -177.2(18) . . . . ? O19 Cl3 O21 Cl3' 75.6(13) . . . . ? O20 Cl3 O21 Cl3' -69.4(13) . . . . ? O18 Cl3 O21 Cl3' -176.9(18) . . . . ? O20 Cl3' O21 Cl3 71.7(13) . . . . ? O18' Cl3' O21 Cl3 -174.9(18) . . . . ? O19 Cl3' O21 Cl3 -65.8(13) . . . . ? C13S O1S C12S C11S -176.2(9) . . . . ? C12S O1S C13S C14S 162.1(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O202 H2A N3S 0.85 1.98 2.830(8) 175.8 2_667 O202 H2B O15 0.85 1.93 2.735(8) 157.8 2_666 O202 H2B Cl2 0.85 2.83 3.563(4) 145.3 2_666 O203 H2C O1S 0.85 1.95 2.692(7) 145.0 2_667 O203 H2C N5 0.85 2.58 2.995(6) 110.9 . O203 H2D O1W 0.85 1.75 2.595(7) 179.5 . O1W H2W O27 0.85 1.92 2.773(14) 179.6 . O1W H2W O28' 0.85 2.24 2.898(12) 134.0 . O1W H2W Cl5 0.85 2.98 3.766(6) 155.5 . O1W H1W N1S 0.85 1.93 2.765(9) 167.2 2_667 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.565 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.137 #===END data_imw643 _database_code_depnum_ccdc_archive 'CCDC 630966' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71.50 H90.50 Cl5 N18.50 O34 Yb2' _chemical_formula_weight 2276.45 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' Yb Yb -0.3850 5.5486 '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' _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 14.2898(4) _cell_length_b 14.6413(4) _cell_length_c 22.2647(6) _cell_angle_alpha 93.0760(10) _cell_angle_beta 96.0590(10) _cell_angle_gamma 103.8040(10) _cell_volume 4483.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7235 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 36.83 _exptl_crystal_description needle _exptl_crystal_colour clear _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2292 _exptl_absorpt_coefficient_mu 2.317 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6419 _exptl_absorpt_correction_T_max 0.8735 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45717 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 20180 _reflns_number_gt 17659 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0422P)^2^+21.5675P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20180 _refine_ls_number_parameters 1165 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.037 _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 Yb1 Yb 0.766912(12) 0.313512(12) 0.720441(8) 0.01286(5) Uani 1 1 d . . . Yb2 Yb 0.352623(12) 0.054012(12) 0.760257(8) 0.01145(5) Uani 1 1 d . . . O1 O 0.8901(2) 0.4036(2) 0.78267(14) 0.0186(6) Uani 1 1 d . . . O2 O 0.2900(2) 0.0373(2) 0.84819(13) 0.0156(6) Uani 1 1 d . . . O3 O 0.8166(2) 0.1891(2) 0.68421(14) 0.0187(6) Uani 1 1 d . . . O4 O 0.3533(2) -0.0981(2) 0.73182(14) 0.0166(6) Uani 1 1 d . . . O5 O 0.2816(2) 0.1751(2) 0.74474(15) 0.0225(7) Uani 1 1 d . . . H5A H 0.2253 0.1707 0.7553 0.027 Uiso 1 1 d R . . H5B H 0.3038 0.2175 0.7218 0.027 Uiso 1 1 d R . . O6 O 0.7054(3) 0.4391(2) 0.69886(15) 0.0271(8) Uani 1 1 d . . . H6A H 0.6459 0.4334 0.6863 0.032 Uiso 1 1 d R . . H6B H 0.7319 0.4977 0.6994 0.032 Uiso 1 1 d R . . O200 O 0.6150(2) 0.2240(2) 0.70814(14) 0.0202(7) Uani 1 1 d . . . O201 O 0.4750(2) 0.1223(2) 0.71290(14) 0.0204(7) Uani 1 1 d . . . C200 C 0.5646(3) 0.1501(4) 0.7237(2) 0.0242(10) Uani 1 1 d . . . H200 H 0.5899 0.0980 0.7301 0.029 Uiso 1 1 d R . . N1 N 1.0294(3) 0.5138(3) 0.80768(17) 0.0181(7) Uani 1 1 d . . . N2 N 0.9077(3) 0.3872(3) 0.66970(17) 0.0168(7) Uani 1 1 d . . . N3 N 0.7360(3) 0.3012(3) 0.60378(17) 0.0172(7) Uani 1 1 d . . . N4 N 0.6606(3) 0.2719(3) 0.55898(17) 0.0216(8) Uani 1 1 d . . . N5 N 0.2890(3) 0.0361(3) 0.59362(16) 0.0171(7) Uani 1 1 d . . . N6 N 0.2710(3) 0.0153(3) 0.65062(16) 0.0154(7) Uani 1 1 d . . . N7 N 0.1834(2) -0.0380(2) 0.74941(16) 0.0137(7) Uani 1 1 d . . . N8 N 0.1673(3) 0.0145(3) 0.90502(16) 0.0168(7) Uani 1 1 d . . . N9 N 0.7910(3) 0.2011(3) 0.79554(16) 0.0154(7) Uani 1 1 d . . . N10 N 0.8730(3) 0.0590(3) 0.68481(18) 0.0207(8) Uani 1 1 d . . . N11 N 0.7065(3) 0.3449(3) 0.82537(17) 0.0163(7) Uani 1 1 d . . . N12 N 0.6894(3) 0.4221(3) 0.85509(17) 0.0169(7) Uani 1 1 d . . . N13 N 0.4727(3) 0.2641(3) 0.86456(16) 0.0158(7) Uani 1 1 d . . . N14 N 0.4639(3) 0.1744(2) 0.84241(16) 0.0143(7) Uani 1 1 d . . . N15 N 0.4692(2) -0.0092(3) 0.82513(16) 0.0143(7) Uani 1 1 d . . . N16 N 0.4304(3) -0.2143(3) 0.72286(17) 0.0179(7) Uani 1 1 d . . . C1 C 0.4635(3) 0.0581(3) 0.58128(19) 0.0169(8) Uani 1 1 d . . . C2 C 0.4547(3) -0.0370(3) 0.5865(2) 0.0215(9) Uani 1 1 d . . . H2 H 0.3939 -0.0763 0.5890 0.026 Uiso 1 1 calc R . . C3 C 0.5351(4) -0.0751(3) 0.5881(2) 0.0249(10) Uani 1 1 d . . . H3 H 0.5283 -0.1392 0.5923 0.030 Uiso 1 1 calc R . . C4 C 0.6259(4) -0.0167(4) 0.5833(2) 0.0242(10) Uani 1 1 d . . . H4 H 0.6803 -0.0414 0.5846 0.029 Uiso 1 1 calc R . . C5 C 0.6350(3) 0.0782(4) 0.5768(2) 0.0233(10) Uani 1 1 d . . . H5 H 0.6956 0.1167 0.5727 0.028 Uiso 1 1 calc R . . C6 C 0.5553(3) 0.1174(3) 0.57611(19) 0.0170(8) Uani 1 1 d . . . C7 C 0.5641(3) 0.2221(3) 0.5709(2) 0.0207(9) Uani 1 1 d . . . H7A H 0.5166 0.2300 0.5384 0.025 Uiso 1 1 calc R . . H7B H 0.5495 0.2498 0.6082 0.025 Uiso 1 1 calc R . . C8 C 0.6912(4) 0.2799(4) 0.5033(2) 0.0321(12) Uani 1 1 d . . . H8 H 0.6524 0.2635 0.4662 0.039 Uiso 1 1 calc R . . C9 C 0.7898(4) 0.3165(4) 0.5117(2) 0.0322(12) Uani 1 1 d . . . H9 H 0.8311 0.3301 0.4820 0.039 Uiso 1 1 calc R . . C10 C 0.8149(3) 0.3288(3) 0.5747(2) 0.0210(9) Uani 1 1 d . . . C11 C 0.9096(3) 0.3685(3) 0.6101(2) 0.0212(9) Uani 1 1 d . . . C12 C 0.9966(4) 0.3865(4) 0.5845(2) 0.0272(11) Uani 1 1 d . . . H12 H 0.9963 0.3766 0.5428 0.033 Uiso 1 1 calc R . . C13 C 1.0829(4) 0.4191(4) 0.6219(2) 0.0281(11) Uani 1 1 d . . . H13 H 1.1418 0.4275 0.6060 0.034 Uiso 1 1 calc R . . C14 C 1.0812(3) 0.4394(3) 0.6837(2) 0.0220(9) Uani 1 1 d . . . H14 H 1.1386 0.4612 0.7098 0.026 Uiso 1 1 calc R . . C15 C 0.9913(3) 0.4260(3) 0.7052(2) 0.0170(8) Uani 1 1 d . . . C16 C 0.9715(3) 0.4490(3) 0.7684(2) 0.0160(8) Uani 1 1 d . . . C17 C 0.9965(4) 0.5303(4) 0.8669(2) 0.0273(11) Uani 1 1 d . . . H17A H 1.0521 0.5577 0.8967 0.033 Uiso 1 1 calc R . . H17B H 0.9624 0.4708 0.8803 0.033 Uiso 1 1 calc R . . C18 C 0.9290(5) 0.5972(4) 0.8614(3) 0.0393(13) Uiso 1 1 d . . . H18A H 0.9650 0.6581 0.8525 0.059 Uiso 1 1 calc R . . H18B H 0.9025 0.6029 0.8989 0.059 Uiso 1 1 calc R . . H18C H 0.8772 0.5724 0.8293 0.059 Uiso 1 1 calc R . . C19 C 1.1193(3) 0.5813(3) 0.7958(2) 0.0205(9) Uani 1 1 d . . . H19A H 1.1200 0.6437 0.8133 0.025 Uiso 1 1 calc R . . H19B H 1.1194 0.5843 0.7524 0.025 Uiso 1 1 calc R . . C20 C 1.2104(4) 0.5536(4) 0.8221(2) 0.0282(11) Uani 1 1 d . . . H20A H 1.2094 0.5483 0.8649 0.042 Uiso 1 1 calc R . . H20B H 1.2667 0.6011 0.8155 0.042 Uiso 1 1 calc R . . H20C H 1.2125 0.4942 0.8027 0.042 Uiso 1 1 calc R . . C21 C 0.3773(3) 0.1021(3) 0.5820(2) 0.0174(8) Uani 1 1 d . . . H21A H 0.3932 0.1545 0.6129 0.021 Uiso 1 1 calc R . . H21B H 0.3656 0.1271 0.5432 0.021 Uiso 1 1 calc R . . C22 C 0.2196(3) -0.0183(4) 0.5514(2) 0.0212(9) Uani 1 1 d . . . H22 H 0.2177 -0.0166 0.5096 0.025 Uiso 1 1 calc R . . C23 C 0.1532(3) -0.0758(3) 0.5813(2) 0.0210(9) Uani 1 1 d . . . H23 H 0.0975 -0.1206 0.5646 0.025 Uiso 1 1 calc R . . C24 C 0.1875(3) -0.0526(3) 0.64282(19) 0.0156(8) Uani 1 1 d . . . C25 C 0.1437(3) -0.0878(3) 0.69644(19) 0.0145(8) Uani 1 1 d . . . C26 C 0.0673(3) -0.1679(3) 0.6933(2) 0.0189(9) Uani 1 1 d . . . H26 H 0.0405 -0.2011 0.6562 0.023 Uiso 1 1 calc R . . C27 C 0.0319(3) -0.1972(3) 0.7467(2) 0.0190(9) Uani 1 1 d . . . H27 H -0.0174 -0.2518 0.7460 0.023 Uiso 1 1 calc R . . C28 C 0.0709(3) -0.1441(3) 0.8010(2) 0.0174(8) Uani 1 1 d . . . H28 H 0.0474 -0.1619 0.8372 0.021 Uiso 1 1 calc R . . C29 C 0.1454(3) -0.0641(3) 0.80037(19) 0.0148(8) Uani 1 1 d . . . C30 C 0.2030(3) -0.0012(3) 0.85427(19) 0.0146(8) Uani 1 1 d . . . C31 C 0.0641(3) -0.0102(3) 0.9137(2) 0.0193(9) Uani 1 1 d . . . H31A H 0.0253 -0.0299 0.8746 0.023 Uiso 1 1 calc R . . H31B H 0.0469 0.0454 0.9303 0.023 Uiso 1 1 calc R . . C32 C 0.0397(4) -0.0888(4) 0.9558(2) 0.0253(10) Uani 1 1 d . . . H32A H 0.0562 -0.1441 0.9395 0.038 Uiso 1 1 calc R . . H32B H -0.0285 -0.1030 0.9596 0.038 Uiso 1 1 calc R . . H32C H 0.0761 -0.0687 0.9950 0.038 Uiso 1 1 calc R . . C33 C 0.2350(3) 0.0732(3) 0.9553(2) 0.0208(9) Uani 1 1 d . . . H33A H 0.2971 0.0569 0.9571 0.025 Uiso 1 1 calc R . . H33B H 0.2094 0.0597 0.9934 0.025 Uiso 1 1 calc R . . C34 C 0.2502(4) 0.1787(4) 0.9474(2) 0.0292(11) Uani 1 1 d . . . H34A H 0.2809 0.1934 0.9116 0.044 Uiso 1 1 calc R . . H34B H 0.2906 0.2143 0.9821 0.044 Uiso 1 1 calc R . . H34C H 0.1885 0.1945 0.9435 0.044 Uiso 1 1 calc R . . C35 C 0.4631(3) 0.4291(3) 0.8607(2) 0.0173(8) Uani 1 1 d . . . C36 C 0.3921(3) 0.4509(3) 0.8939(2) 0.0213(9) Uani 1 1 d . . . H36 H 0.3330 0.4070 0.8933 0.026 Uiso 1 1 calc R . . C37 C 0.4087(3) 0.5363(3) 0.9275(2) 0.0224(9) Uani 1 1 d . . . H37 H 0.3609 0.5497 0.9493 0.027 Uiso 1 1 calc R . . C38 C 0.4964(4) 0.6020(3) 0.9286(2) 0.0222(9) Uani 1 1 d . . . H38 H 0.5078 0.6597 0.9512 0.027 Uiso 1 1 calc R . . C39 C 0.5675(3) 0.5813(3) 0.8961(2) 0.0202(9) Uani 1 1 d . . . H39 H 0.6267 0.6254 0.8975 0.024 Uiso 1 1 calc R . . C40 C 0.5520(3) 0.4958(3) 0.8611(2) 0.0170(8) Uani 1 1 d . . . C41 C 0.6304(3) 0.4797(3) 0.8245(2) 0.0206(9) Uani 1 1 d . . . H41A H 0.6008 0.4482 0.7852 0.025 Uiso 1 1 calc R . . H41B H 0.6722 0.5401 0.8179 0.025 Uiso 1 1 calc R . . C42 C 0.7242(3) 0.4308(3) 0.9147(2) 0.0200(9) Uani 1 1 d . . . H42 H 0.7217 0.4790 0.9430 0.024 Uiso 1 1 calc R . . C43 C 0.7637(3) 0.3559(3) 0.9256(2) 0.0201(9) Uani 1 1 d . . . H43 H 0.7925 0.3421 0.9623 0.024 Uiso 1 1 calc R . . C44 C 0.7510(3) 0.3047(3) 0.86930(19) 0.0156(8) Uani 1 1 d . . . C45 C 0.7758(3) 0.2159(3) 0.8533(2) 0.0176(8) Uani 1 1 d . . . C46 C 0.7784(4) 0.1489(4) 0.8956(2) 0.0238(10) Uani 1 1 d . . . H46 H 0.7724 0.1621 0.9362 0.029 Uiso 1 1 calc R . . C47 C 0.7902(4) 0.0626(4) 0.8748(2) 0.0320(12) Uani 1 1 d . . . H47 H 0.7882 0.0149 0.9010 0.038 Uiso 1 1 calc R . . C48 C 0.8049(4) 0.0461(4) 0.8149(2) 0.0287(11) Uani 1 1 d . . . H48 H 0.8111 -0.0127 0.8005 0.034 Uiso 1 1 calc R . . C49 C 0.8103(3) 0.1187(3) 0.7770(2) 0.0203(9) Uani 1 1 d . . . C50 C 0.8338(3) 0.1215(3) 0.7123(2) 0.0189(9) Uani 1 1 d . . . C51 C 0.8960(4) 0.0735(4) 0.6222(2) 0.0251(10) Uani 1 1 d . . . H51A H 0.8529 0.1079 0.6025 0.030 Uiso 1 1 calc R . . H51B H 0.8850 0.0127 0.5996 0.030 Uiso 1 1 calc R . . C52 C 1.0005(4) 0.1278(4) 0.6212(3) 0.0373(13) Uani 1 1 d . . . H52A H 1.0116 0.1882 0.6434 0.056 Uiso 1 1 calc R . . H52B H 1.0126 0.1365 0.5801 0.056 Uiso 1 1 calc R . . H52C H 1.0434 0.0930 0.6396 0.056 Uiso 1 1 calc R . . C53 C 0.9002(4) -0.0233(3) 0.7106(2) 0.0261(10) Uani 1 1 d . . . H53A H 0.9162 -0.0106 0.7541 0.031 Uiso 1 1 calc R . . H53B H 0.9575 -0.0330 0.6940 0.031 Uiso 1 1 calc R . . C54 C 0.8184(4) -0.1126(4) 0.6967(3) 0.0321(12) Uani 1 1 d . . . H54A H 0.7626 -0.1042 0.7148 0.048 Uiso 1 1 calc R . . H54B H 0.8392 -0.1649 0.7129 0.048 Uiso 1 1 calc R . . H54C H 0.8018 -0.1248 0.6536 0.048 Uiso 1 1 calc R . . C55 C 0.4398(4) 0.3331(3) 0.8262(2) 0.0210(9) Uani 1 1 d . . . H55A H 0.3704 0.3119 0.8142 0.025 Uiso 1 1 calc R . . H55B H 0.4719 0.3373 0.7898 0.025 Uiso 1 1 calc R . . C56 C 0.5172(3) 0.2803(3) 0.9220(2) 0.0187(9) Uani 1 1 d . . . H56 H 0.5308 0.3370 0.9459 0.022 Uiso 1 1 calc R . . C57 C 0.5388(3) 0.1982(3) 0.93872(19) 0.0178(8) Uani 1 1 d . . . H57 H 0.5693 0.1876 0.9758 0.021 Uiso 1 1 calc R . . C58 C 0.5049(3) 0.1340(3) 0.88779(19) 0.0142(8) Uani 1 1 d . . . C59 C 0.5084(3) 0.0358(3) 0.87947(19) 0.0143(8) Uani 1 1 d . . . C60 C 0.5486(3) -0.0103(3) 0.9252(2) 0.0180(8) Uani 1 1 d . . . H60 H 0.5778 0.0223 0.9620 0.022 Uiso 1 1 calc R . . C61 C 0.5444(3) -0.1047(3) 0.9147(2) 0.0209(9) Uani 1 1 d . . . H61 H 0.5687 -0.1370 0.9451 0.025 Uiso 1 1 calc R . . C62 C 0.5038(3) -0.1518(3) 0.8585(2) 0.0183(9) Uani 1 1 d . . . H62 H 0.5003 -0.2157 0.8508 0.022 Uiso 1 1 calc R . . C63 C 0.4687(3) -0.1012(3) 0.8145(2) 0.0156(8) Uani 1 1 d . . . C64 C 0.4151(3) -0.1402(3) 0.75315(19) 0.0154(8) Uani 1 1 d . . . C65 C 0.5168(4) -0.2534(4) 0.7343(2) 0.0259(10) Uani 1 1 d . . . H65A H 0.5609 -0.2154 0.7675 0.031 Uiso 1 1 calc R . . H65B H 0.5504 -0.2494 0.6986 0.031 Uiso 1 1 calc R . . C66 C 0.4903(4) -0.3553(4) 0.7499(3) 0.0372(13) Uani 1 1 d . . . H66A H 0.4564 -0.3597 0.7851 0.056 Uiso 1 1 calc R . . H66B H 0.5483 -0.3769 0.7581 0.056 Uiso 1 1 calc R . . H66C H 0.4492 -0.3937 0.7164 0.056 Uiso 1 1 calc R . . C67 C 0.3631(4) -0.2542(3) 0.6674(2) 0.0213(9) Uani 1 1 d . . . H67A H 0.3935 -0.2923 0.6425 0.026 Uiso 1 1 calc R . . H67B H 0.3510 -0.2030 0.6442 0.026 Uiso 1 1 calc R . . C68 C 0.2670(4) -0.3143(4) 0.6817(2) 0.0303(11) Uani 1 1 d . . . H68A H 0.2779 -0.3688 0.7008 0.045 Uiso 1 1 calc R . . H68B H 0.2237 -0.3342 0.6449 0.045 Uiso 1 1 calc R . . H68C H 0.2387 -0.2781 0.7085 0.045 Uiso 1 1 calc R . . Cl1 Cl 0.78060(8) 0.78510(8) 0.85573(6) 0.0261(2) Uani 1 1 d . . . O10 O 0.8005(4) 0.7402(5) 0.9091(3) 0.0734(19) Uani 1 1 d . . . O11 O 0.7363(4) 0.7147(3) 0.8075(2) 0.0535(13) Uani 1 1 d . . . O12 O 0.8676(3) 0.8455(3) 0.83934(17) 0.0305(8) Uani 1 1 d . . . O13 O 0.7130(4) 0.8380(4) 0.8663(4) 0.086(2) Uani 1 1 d . . . Cl2 Cl 1.26354(7) 0.78412(7) 0.92044(5) 0.0180(2) Uani 1 1 d . . . O14 O 1.2945(3) 0.8702(2) 0.95978(16) 0.0278(8) Uani 1 1 d . . . O15 O 1.1678(3) 0.7343(3) 0.93153(18) 0.0313(8) Uani 1 1 d . . . O16 O 1.3307(3) 0.7261(2) 0.93312(16) 0.0259(7) Uani 1 1 d . . . O17 O 1.2611(3) 0.8061(3) 0.85800(15) 0.0281(8) Uani 1 1 d . . . Cl3 Cl 0.07626(9) 0.22127(9) 0.80770(6) 0.0270(2) Uani 1 1 d . . . O18 O 0.1027(3) 0.1396(3) 0.7819(2) 0.0476(12) Uani 1 1 d . . . O19 O 0.0254(4) 0.1930(4) 0.8587(2) 0.0585(14) Uani 1 1 d . . . O20 O 0.0143(3) 0.2523(3) 0.7632(2) 0.0381(9) Uani 1 1 d . . . O21 O 0.1629(3) 0.2934(3) 0.8258(2) 0.0528(13) Uani 1 1 d . . . Cl5 Cl 0.93234(10) 0.63206(9) 0.58792(6) 0.0340(3) Uani 1 1 d . . . O26 O 0.9753(3) 0.5998(3) 0.6412(2) 0.0429(10) Uani 1 1 d . . . O27 O 0.8821(3) 0.5546(3) 0.5451(2) 0.0460(11) Uani 1 1 d . . . O28 O 1.0070(3) 0.6942(3) 0.5599(2) 0.0480(12) Uani 1 1 d . . . O29 O 0.8626(3) 0.6848(3) 0.6057(2) 0.0442(10) Uani 1 1 d . . . C1S C 0.8181(5) 0.7406(4) 0.4706(3) 0.0405(14) Uani 1 1 d D . . H1S1 H 0.7924 0.7591 0.4328 0.061 Uiso 1 1 calc R . . H1S2 H 0.7740 0.6852 0.4814 0.061 Uiso 1 1 calc R . . H1S3 H 0.8798 0.7273 0.4666 0.061 Uiso 1 1 calc R . . N1S N 0.8303(4) 0.8173(4) 0.5179(2) 0.0396(12) Uani 1 1 d D . . O1S O 0.7541(4) 0.8296(4) 0.5362(2) 0.0514(13) Uani 1 1 d D . . O2S O 0.9056(4) 0.8753(3) 0.5285(2) 0.0523(12) Uani 1 1 d D . . C2S C 0.6203(7) 0.5508(6) 0.5499(4) 0.068(2) Uiso 1 1 d D . . H2S1 H 0.5874 0.4935 0.5655 0.102 Uiso 1 1 calc R . . H2S2 H 0.6888 0.5626 0.5623 0.102 Uiso 1 1 calc R . . H2S3 H 0.6083 0.5447 0.5065 0.102 Uiso 1 1 calc R . . N2S N 0.5841(8) 0.6298(7) 0.5736(5) 0.103(3) Uiso 1 1 d D . . O3S O 0.5189(6) 0.6642(6) 0.5568(4) 0.104(2) Uiso 1 1 d D . . O4S O 0.6334(9) 0.6710(9) 0.6243(6) 0.181(5) Uiso 1 1 d D . . C3S C 1.0597(10) 0.4719(9) 0.9954(7) 0.050(3) Uiso 0.50 1 d PD . . H3SA H 1.1058 0.5313 0.9949 0.075 Uiso 0.50 1 calc PR . . H3SB H 1.0419 0.4645 1.0356 0.075 Uiso 0.50 1 calc PR . . H3SC H 1.0029 0.4700 0.9677 0.075 Uiso 0.50 1 calc PR . . N3S N 1.1029(6) 0.3953(6) 0.9773(5) 0.036(2) Uiso 0.50 1 d PD . . O5S O 1.1754(6) 0.4250(6) 0.9667(4) 0.044(2) Uiso 0.50 1 d PD . . O6S O 1.0326(6) 0.3196(6) 0.9802(4) 0.044(2) Uiso 0.50 1 d PD . . O1W O 0.7990(5) 0.6176(3) 0.7169(2) 0.0628(15) Uani 1 1 d . . . H1B H 0.7428 0.6146 0.6988 0.075 Uiso 1 1 d R . . H1A H 0.8455 0.6129 0.6970 0.075 Uiso 1 1 d R . . Cl4 Cl 0.4040(3) -0.6088(3) 0.6471(2) 0.0396(8) Uani 0.641(7) 1 d PDU A 1 O22 O 0.3419(7) -0.5456(7) 0.6488(5) 0.085(3) Uiso 0.641(7) 1 d PDU A 1 O23 O 0.4252(7) -0.6232(7) 0.5863(4) 0.075(3) Uiso 0.641(7) 1 d PDU A 1 O25 O 0.4864(5) -0.5821(6) 0.6898(4) 0.052(2) Uiso 0.641(7) 1 d PDU A 1 Cl4' Cl 0.3805(7) -0.6064(6) 0.6610(4) 0.0531(16) Uani 0.359(7) 1 d PDU A 2 O22' O 0.3555(12) -0.5596(11) 0.6085(7) 0.076(4) Uiso 0.359(7) 1 d PDU A 2 O23' O 0.4914(10) -0.5834(13) 0.6655(10) 0.086(5) Uiso 0.359(7) 1 d PDU A 2 O25' O 0.3441(14) -0.5726(14) 0.7125(7) 0.086(4) Uiso 0.359(7) 1 d PDU A 2 O24 O 0.3449(5) -0.7038(4) 0.6570(3) 0.0844(19) 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 Yb1 0.01196(9) 0.01304(9) 0.01260(9) -0.00108(6) 0.00044(6) 0.00207(6) Yb2 0.01016(8) 0.01254(9) 0.01084(9) -0.00122(6) -0.00055(6) 0.00247(6) O1 0.0155(15) 0.0223(16) 0.0146(15) -0.0027(12) 0.0003(11) -0.0004(12) O2 0.0130(14) 0.0195(15) 0.0128(14) -0.0026(12) 0.0006(11) 0.0020(11) O3 0.0231(16) 0.0190(16) 0.0151(15) -0.0006(12) 0.0010(12) 0.0085(13) O4 0.0162(14) 0.0168(15) 0.0163(15) -0.0017(12) -0.0027(11) 0.0058(12) O5 0.0210(16) 0.0196(16) 0.0268(17) -0.0012(13) -0.0029(13) 0.0081(13) O6 0.042(2) 0.0213(17) 0.0225(17) 0.0034(14) 0.0074(15) 0.0144(15) O200 0.0150(15) 0.0237(17) 0.0182(15) -0.0004(13) 0.0007(12) -0.0013(12) O201 0.0146(15) 0.0281(17) 0.0142(15) -0.0004(13) -0.0001(11) -0.0015(13) C200 0.019(2) 0.027(2) 0.025(2) 0.006(2) 0.0015(18) 0.0021(18) N1 0.0177(18) 0.0167(18) 0.0162(18) -0.0010(14) -0.0009(14) -0.0012(14) N2 0.0153(17) 0.0175(18) 0.0152(17) -0.0008(14) 0.0006(13) 0.0004(14) N3 0.0163(17) 0.0182(18) 0.0141(17) -0.0025(14) -0.0019(14) 0.0012(14) N4 0.0187(19) 0.027(2) 0.0153(18) -0.0008(15) -0.0013(14) -0.0006(16) N5 0.0141(17) 0.0246(19) 0.0115(17) 0.0013(14) -0.0017(13) 0.0036(15) N6 0.0139(17) 0.0185(18) 0.0134(17) -0.0004(14) -0.0001(13) 0.0042(14) N7 0.0115(16) 0.0152(17) 0.0140(17) -0.0002(13) 0.0003(13) 0.0033(13) N8 0.0157(17) 0.0223(19) 0.0124(17) -0.0020(14) 0.0006(13) 0.0056(14) N9 0.0152(17) 0.0171(18) 0.0144(17) 0.0003(14) 0.0014(13) 0.0055(14) N10 0.0231(19) 0.0192(19) 0.0204(19) -0.0032(15) -0.0001(15) 0.0085(15) N11 0.0155(17) 0.0165(18) 0.0166(18) -0.0007(14) 0.0029(13) 0.0034(14) N12 0.0185(18) 0.0166(18) 0.0155(18) -0.0015(14) 0.0034(14) 0.0043(14) N13 0.0167(17) 0.0147(17) 0.0148(17) -0.0016(14) -0.0014(13) 0.0035(14) N14 0.0151(17) 0.0132(17) 0.0140(17) -0.0012(13) -0.0002(13) 0.0036(13) N15 0.0114(16) 0.0159(17) 0.0148(17) -0.0015(14) -0.0006(13) 0.0030(13) N16 0.0211(19) 0.0166(18) 0.0156(18) -0.0011(14) -0.0006(14) 0.0054(15) C1 0.016(2) 0.024(2) 0.0095(18) -0.0004(16) -0.0008(15) 0.0030(17) C2 0.020(2) 0.024(2) 0.019(2) -0.0002(18) 0.0005(17) 0.0017(18) C3 0.029(3) 0.020(2) 0.026(2) -0.0015(19) -0.0001(19) 0.0080(19) C4 0.022(2) 0.030(3) 0.022(2) -0.0053(19) 0.0001(18) 0.012(2) C5 0.018(2) 0.031(3) 0.020(2) -0.0027(19) 0.0022(17) 0.0042(19) C6 0.017(2) 0.022(2) 0.0093(18) -0.0019(16) -0.0012(15) 0.0017(17) C7 0.017(2) 0.025(2) 0.017(2) 0.0005(18) -0.0014(16) 0.0010(17) C8 0.029(3) 0.044(3) 0.013(2) -0.002(2) -0.0010(19) -0.008(2) C9 0.024(3) 0.049(3) 0.014(2) -0.003(2) 0.0015(18) -0.009(2) C10 0.019(2) 0.025(2) 0.015(2) -0.0033(17) 0.0011(17) -0.0010(18) C11 0.019(2) 0.023(2) 0.019(2) -0.0016(18) 0.0000(17) 0.0026(18) C12 0.024(2) 0.036(3) 0.018(2) -0.006(2) 0.0069(19) 0.001(2) C13 0.020(2) 0.034(3) 0.028(3) -0.007(2) 0.0066(19) 0.003(2) C14 0.014(2) 0.026(2) 0.024(2) -0.0045(19) -0.0002(17) 0.0033(17) C15 0.017(2) 0.015(2) 0.017(2) -0.0011(16) 0.0006(16) 0.0026(16) C16 0.0148(19) 0.0127(19) 0.018(2) 0.0000(16) -0.0006(15) 0.0004(15) C17 0.027(2) 0.030(3) 0.016(2) -0.0053(19) 0.0017(18) -0.009(2) C19 0.018(2) 0.018(2) 0.021(2) -0.0011(17) 0.0001(17) -0.0032(17) C20 0.022(2) 0.034(3) 0.024(2) -0.001(2) -0.0049(19) 0.001(2) C21 0.015(2) 0.021(2) 0.015(2) 0.0020(17) 0.0003(15) 0.0022(16) C22 0.019(2) 0.030(2) 0.012(2) -0.0021(18) -0.0034(16) 0.0033(18) C23 0.018(2) 0.027(2) 0.014(2) -0.0048(18) -0.0019(16) 0.0007(18) C24 0.0135(19) 0.017(2) 0.016(2) -0.0020(16) 0.0002(15) 0.0035(15) C25 0.0114(18) 0.018(2) 0.0146(19) -0.0017(16) -0.0004(15) 0.0057(15) C26 0.015(2) 0.021(2) 0.018(2) -0.0063(17) -0.0015(16) 0.0024(17) C27 0.0133(19) 0.018(2) 0.023(2) -0.0019(17) 0.0010(16) 0.0010(16) C28 0.015(2) 0.020(2) 0.018(2) 0.0019(17) 0.0048(16) 0.0044(16) C29 0.0129(19) 0.019(2) 0.0129(19) -0.0020(16) -0.0008(15) 0.0058(16) C30 0.0144(19) 0.016(2) 0.0141(19) 0.0013(16) 0.0010(15) 0.0055(15) C31 0.016(2) 0.027(2) 0.016(2) -0.0024(17) 0.0043(16) 0.0068(17) C32 0.025(2) 0.029(3) 0.021(2) 0.0014(19) 0.0095(19) 0.0027(19) C33 0.021(2) 0.026(2) 0.014(2) -0.0040(17) -0.0012(16) 0.0068(18) C34 0.032(3) 0.024(3) 0.028(3) -0.011(2) -0.002(2) 0.004(2) C35 0.020(2) 0.014(2) 0.017(2) -0.0022(16) -0.0043(16) 0.0070(16) C36 0.017(2) 0.023(2) 0.024(2) 0.0023(18) -0.0002(17) 0.0053(17) C37 0.022(2) 0.026(2) 0.023(2) 0.0011(19) 0.0052(18) 0.0121(19) C38 0.033(3) 0.015(2) 0.019(2) -0.0020(17) 0.0030(19) 0.0080(18) C39 0.024(2) 0.015(2) 0.020(2) -0.0006(17) 0.0030(17) 0.0031(17) C40 0.020(2) 0.017(2) 0.016(2) 0.0018(16) 0.0019(16) 0.0070(16) C41 0.023(2) 0.023(2) 0.019(2) 0.0045(18) 0.0067(17) 0.0108(18) C42 0.021(2) 0.023(2) 0.016(2) -0.0039(17) 0.0040(17) 0.0044(17) C43 0.020(2) 0.026(2) 0.014(2) 0.0000(17) 0.0020(16) 0.0049(18) C44 0.016(2) 0.018(2) 0.0125(19) 0.0013(16) 0.0020(15) 0.0033(16) C45 0.017(2) 0.020(2) 0.015(2) -0.0005(17) -0.0006(16) 0.0037(16) C46 0.028(2) 0.026(2) 0.018(2) 0.0033(19) 0.0031(18) 0.0085(19) C47 0.048(3) 0.028(3) 0.026(3) 0.010(2) 0.007(2) 0.016(2) C48 0.046(3) 0.021(2) 0.023(2) 0.0015(19) 0.004(2) 0.015(2) C49 0.022(2) 0.019(2) 0.019(2) -0.0006(17) 0.0008(17) 0.0052(17) C50 0.018(2) 0.020(2) 0.019(2) -0.0039(17) -0.0010(16) 0.0078(17) C51 0.030(3) 0.026(2) 0.022(2) -0.0035(19) 0.0053(19) 0.012(2) C52 0.034(3) 0.042(3) 0.038(3) 0.003(3) 0.015(2) 0.010(3) C53 0.031(3) 0.023(2) 0.030(3) 0.000(2) 0.000(2) 0.018(2) C54 0.044(3) 0.023(3) 0.028(3) -0.002(2) -0.001(2) 0.009(2) C55 0.027(2) 0.017(2) 0.018(2) -0.0007(17) -0.0056(17) 0.0074(18) C56 0.020(2) 0.018(2) 0.015(2) -0.0050(16) -0.0004(16) 0.0014(17) C57 0.019(2) 0.020(2) 0.0124(19) -0.0017(16) -0.0033(15) 0.0028(17) C58 0.0113(18) 0.016(2) 0.0133(19) -0.0009(16) -0.0006(14) 0.0017(15) C59 0.0112(18) 0.016(2) 0.0139(19) -0.0001(16) -0.0002(14) 0.0018(15) C60 0.017(2) 0.020(2) 0.015(2) 0.0001(17) -0.0021(16) 0.0034(16) C61 0.022(2) 0.023(2) 0.017(2) 0.0040(18) -0.0036(17) 0.0064(18) C62 0.018(2) 0.014(2) 0.023(2) 0.0003(17) 0.0000(17) 0.0054(16) C63 0.0116(18) 0.017(2) 0.018(2) 0.0006(16) 0.0007(15) 0.0029(15) C64 0.0142(19) 0.0146(19) 0.016(2) -0.0002(16) 0.0017(15) 0.0014(15) C65 0.023(2) 0.028(3) 0.030(3) -0.005(2) 0.0018(19) 0.013(2) C66 0.041(3) 0.026(3) 0.046(3) -0.005(2) -0.009(3) 0.018(2) C67 0.032(2) 0.016(2) 0.015(2) -0.0037(16) -0.0009(18) 0.0050(18) C68 0.030(3) 0.027(3) 0.026(3) -0.002(2) -0.004(2) -0.004(2) Cl1 0.0195(5) 0.0235(6) 0.0339(6) -0.0006(5) 0.0077(4) 0.0015(4) O10 0.054(3) 0.096(5) 0.059(3) 0.041(3) 0.002(3) -0.010(3) O11 0.056(3) 0.046(3) 0.045(3) -0.012(2) 0.014(2) -0.014(2) O12 0.0198(17) 0.034(2) 0.035(2) 0.0078(16) 0.0059(15) 0.0005(15) O13 0.040(3) 0.046(3) 0.174(7) -0.021(4) 0.037(4) 0.012(2) Cl2 0.0180(5) 0.0184(5) 0.0161(5) -0.0013(4) -0.0033(4) 0.0046(4) O14 0.0312(19) 0.0215(17) 0.0280(19) -0.0081(14) -0.0074(15) 0.0079(14) O15 0.0217(18) 0.034(2) 0.034(2) -0.0012(16) 0.0043(15) -0.0002(15) O16 0.0286(18) 0.0253(18) 0.0245(17) -0.0037(14) -0.0074(14) 0.0142(14) O17 0.0309(19) 0.034(2) 0.0185(17) 0.0052(15) -0.0030(14) 0.0092(15) Cl3 0.0238(6) 0.0258(6) 0.0309(6) -0.0014(5) -0.0046(5) 0.0092(5) O18 0.034(2) 0.034(2) 0.077(3) -0.009(2) -0.002(2) 0.0175(18) O19 0.062(3) 0.079(4) 0.037(3) 0.011(3) 0.007(2) 0.021(3) O20 0.034(2) 0.038(2) 0.045(2) 0.0078(19) -0.0051(18) 0.0169(18) O21 0.039(3) 0.038(3) 0.070(3) -0.005(2) -0.016(2) -0.001(2) Cl5 0.0382(7) 0.0273(6) 0.0318(7) -0.0008(5) 0.0015(5) 0.0009(5) O26 0.055(3) 0.029(2) 0.043(2) 0.0050(18) -0.004(2) 0.0114(19) O27 0.051(3) 0.028(2) 0.049(3) -0.0078(19) -0.010(2) -0.0009(19) O28 0.050(3) 0.049(3) 0.033(2) -0.013(2) 0.015(2) -0.011(2) O29 0.045(3) 0.050(3) 0.042(2) 0.007(2) 0.011(2) 0.016(2) C1S 0.057(4) 0.036(3) 0.029(3) -0.006(2) 0.008(3) 0.012(3) N1S 0.051(3) 0.033(3) 0.032(3) -0.016(2) 0.020(2) 0.003(2) O1S 0.054(3) 0.083(4) 0.032(2) 0.007(2) 0.004(2) 0.047(3) O2S 0.063(3) 0.040(3) 0.052(3) -0.008(2) 0.002(2) 0.015(2) O1W 0.093(4) 0.042(3) 0.050(3) 0.002(2) 0.032(3) -0.001(3) Cl4 0.0442(19) 0.0371(12) 0.0403(19) 0.0016(12) -0.0005(12) 0.0186(12) Cl4' 0.072(3) 0.0355(19) 0.050(3) 0.000(2) -0.015(3) 0.022(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1 2.223(3) . ? Yb1 O200 2.232(3) . ? Yb1 O3 2.247(3) . ? Yb1 O6 2.271(3) . ? Yb1 N2 2.463(4) . ? Yb1 N9 2.463(4) . ? Yb1 N3 2.578(4) . ? Yb1 N11 2.629(4) . ? Yb1 C16 3.157(4) . ? Yb1 C50 3.180(5) . ? Yb2 O201 2.199(3) . ? Yb2 O2 2.238(3) . ? Yb2 O5 2.268(3) . ? Yb2 O4 2.285(3) . ? Yb2 N7 2.452(3) . ? Yb2 N15 2.468(4) . ? Yb2 N6 2.565(4) . ? Yb2 N14 2.586(4) . ? Yb2 C30 3.147(4) . ? Yb2 C64 3.178(4) . ? O1 C16 1.275(5) . ? O2 C30 1.261(5) . ? O3 C50 1.258(6) . ? O4 C64 1.260(5) . ? O5 H5A 0.8501 . ? O5 H5B 0.8498 . ? O6 H6A 0.8500 . ? O6 H6B 0.8501 . ? O200 C200 1.237(6) . ? O201 C200 1.241(6) . ? C200 H200 0.9300 . ? N1 C16 1.317(6) . ? N1 C17 1.473(6) . ? N1 C19 1.479(5) . ? N2 C15 1.342(5) . ? N2 C11 1.344(6) . ? N3 C10 1.348(6) . ? N3 N4 1.359(5) . ? N4 C8 1.359(6) . ? N4 C7 1.456(6) . ? N5 N6 1.357(5) . ? N5 C22 1.359(6) . ? N5 C21 1.451(5) . ? N6 C24 1.346(5) . ? N7 C29 1.344(5) . ? N7 C25 1.346(5) . ? N8 C30 1.319(5) . ? N8 C31 1.468(5) . ? N8 C33 1.484(6) . ? N9 C45 1.341(6) . ? N9 C49 1.353(6) . ? N10 C50 1.335(6) . ? N10 C53 1.478(6) . ? N10 C51 1.480(6) . ? N11 C44 1.347(6) . ? N11 N12 1.364(5) . ? N12 C42 1.355(6) . ? N12 C41 1.471(6) . ? N13 C56 1.348(6) . ? N13 N14 1.349(5) . ? N13 C55 1.485(5) . ? N14 C58 1.349(5) . ? N15 C59 1.344(5) . ? N15 C63 1.353(6) . ? N16 C64 1.320(6) . ? N16 C67 1.482(6) . ? N16 C65 1.485(6) . ? C1 C2 1.380(7) . ? C1 C6 1.409(6) . ? C1 C21 1.522(6) . ? C2 C3 1.390(7) . ? C2 H2 0.9300 . ? C3 C4 1.392(7) . ? C3 H3 0.9300 . ? C4 C5 1.381(7) . ? C4 H4 0.9300 . ? C5 C6 1.391(7) . ? C5 H5 0.9300 . ? C6 C7 1.519(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.372(7) . ? C8 H8 0.9300 . ? C9 C10 1.403(6) . ? C9 H9 0.9300 . ? C10 C11 1.464(6) . ? C11 C12 1.396(6) . ? C12 C13 1.380(7) . ? C12 H12 0.9300 . ? C13 C14 1.397(7) . ? C13 H13 0.9300 . ? C14 C15 1.392(6) . ? C14 H14 0.9300 . ? C15 C16 1.502(6) . ? C17 C18 1.531(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.523(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.367(6) . ? C22 H22 0.9300 . ? C23 C24 1.399(6) . ? C23 H23 0.9300 . ? C24 C25 1.467(6) . ? C25 C26 1.392(6) . ? C26 C27 1.390(6) . ? C26 H26 0.9300 . ? C27 C28 1.389(6) . ? C27 H27 0.9300 . ? C28 C29 1.383(6) . ? C28 H28 0.9300 . ? C29 C30 1.510(6) . ? C31 C32 1.523(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.529(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.402(6) . ? C35 C40 1.404(6) . ? C35 C55 1.512(6) . ? C36 C37 1.378(7) . ? C36 H36 0.9300 . ? C37 C38 1.383(7) . ? C37 H37 0.9300 . ? C38 C39 1.389(7) . ? C38 H38 0.9300 . ? C39 C40 1.395(6) . ? C39 H39 0.9300 . ? C40 C41 1.508(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.369(7) . ? C42 H42 0.9300 . ? C43 C44 1.397(6) . ? C43 H43 0.9300 . ? C44 C45 1.463(6) . ? C45 C46 1.402(6) . ? C46 C47 1.377(7) . ? C46 H46 0.9300 . ? C47 C48 1.389(7) . ? C47 H47 0.9300 . ? C48 C49 1.384(7) . ? C48 H48 0.9300 . ? C49 C50 1.514(6) . ? C51 C52 1.518(7) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.523(7) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.372(6) . ? C56 H56 0.9300 . ? C57 C58 1.398(6) . ? C57 H57 0.9300 . ? C58 C59 1.453(6) . ? C59 C60 1.399(6) . ? C60 C61 1.375(6) . ? C60 H60 0.9300 . ? C61 C62 1.394(6) . ? C61 H61 0.9300 . ? C62 C63 1.383(6) . ? C62 H62 0.9300 . ? C63 C64 1.505(6) . ? C65 C66 1.518(7) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 C68 1.519(7) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? Cl1 O13 1.405(5) . ? Cl1 O10 1.424(5) . ? Cl1 O11 1.429(5) . ? Cl1 O12 1.437(4) . ? Cl2 O15 1.442(4) . ? Cl2 O17 1.443(3) . ? Cl2 O16 1.443(3) . ? Cl2 O14 1.444(4) . ? Cl3 O20 1.424(4) . ? Cl3 O21 1.426(4) . ? Cl3 O19 1.439(5) . ? Cl3 O18 1.446(4) . ? Cl5 O26 1.433(4) . ? Cl5 O27 1.436(4) . ? Cl5 O28 1.447(4) . ? Cl5 O29 1.471(5) . ? C1S N1S 1.463(7) . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? N1S O2S 1.194(6) . ? N1S O1S 1.251(6) . ? C2S N2S 1.470(11) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? N2S O3S 1.197(9) . ? N2S O4S 1.299(11) . ? C3S N3S 1.462(12) . ? C3S H3SA 0.9600 . ? C3S H3SB 0.9600 . ? C3S H3SC 0.9600 . ? N3S O5S 1.080(10) . ? N3S O6S 1.316(10) . ? O1W H1B 0.8499 . ? O1W H1A 0.8505 . ? Cl4 O25 1.394(8) . ? Cl4 O22 1.428(9) . ? Cl4 O23 1.434(9) . ? Cl4 O24 1.486(8) . ? Cl4' O24 1.390(10) . ? Cl4' O25' 1.421(13) . ? Cl4' O22' 1.442(12) . ? Cl4' O23' 1.530(13) . ? 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 Yb1 O200 148.08(11) . . ? O1 Yb1 O3 107.35(12) . . ? O200 Yb1 O3 88.88(12) . . ? O1 Yb1 O6 91.92(13) . . ? O200 Yb1 O6 88.14(13) . . ? O3 Yb1 O6 147.04(12) . . ? O1 Yb1 N2 65.96(12) . . ? O200 Yb1 N2 145.84(12) . . ? O3 Yb1 N2 76.85(12) . . ? O6 Yb1 N2 87.56(13) . . ? O1 Yb1 N9 79.71(12) . . ? O200 Yb1 N9 82.74(12) . . ? O3 Yb1 N9 65.26(12) . . ? O6 Yb1 N9 146.43(12) . . ? N2 Yb1 N9 117.30(12) . . ? O1 Yb1 N3 129.64(11) . . ? O200 Yb1 N3 81.18(12) . . ? O3 Yb1 N3 71.45(12) . . ? O6 Yb1 N3 75.66(12) . . ? N2 Yb1 N3 64.93(12) . . ? N9 Yb1 N3 133.86(12) . . ? O1 Yb1 N11 71.09(11) . . ? O200 Yb1 N11 77.40(11) . . ? O3 Yb1 N11 129.85(11) . . ? O6 Yb1 N11 81.25(12) . . ? N2 Yb1 N11 135.09(12) . . ? N9 Yb1 N11 65.26(12) . . ? N3 Yb1 N11 148.83(12) . . ? O1 Yb1 C16 18.84(11) . . ? O200 Yb1 C16 166.85(12) . . ? O3 Yb1 C16 98.96(12) . . ? O6 Yb1 C16 90.88(13) . . ? N2 Yb1 C16 47.12(12) . . ? N9 Yb1 C16 90.92(12) . . ? N3 Yb1 C16 111.27(11) . . ? N11 Yb1 C16 89.49(11) . . ? O1 Yb1 C50 100.43(12) . . ? O200 Yb1 C50 86.48(12) . . ? O3 Yb1 C50 18.18(11) . . ? O6 Yb1 C50 164.27(12) . . ? N2 Yb1 C50 88.61(12) . . ? N9 Yb1 C50 47.09(12) . . ? N3 Yb1 C50 88.90(12) . . ? N11 Yb1 C50 111.88(12) . . ? C16 Yb1 C50 97.65(11) . . ? O201 Yb2 O2 147.20(11) . . ? O201 Yb2 O5 90.75(13) . . ? O2 Yb2 O5 88.83(12) . . ? O201 Yb2 O4 96.74(12) . . ? O2 Yb2 O4 101.44(11) . . ? O5 Yb2 O4 146.71(11) . . ? O201 Yb2 N7 146.00(12) . . ? O2 Yb2 N7 66.28(11) . . ? O5 Yb2 N7 82.43(12) . . ? O4 Yb2 N7 73.30(11) . . ? O201 Yb2 N15 87.45(12) . . ? O2 Yb2 N15 75.63(11) . . ? O5 Yb2 N15 147.11(12) . . ? O4 Yb2 N15 65.90(11) . . ? N7 Yb2 N15 115.74(12) . . ? O201 Yb2 N6 80.81(11) . . ? O2 Yb2 N6 130.75(11) . . ? O5 Yb2 N6 77.12(12) . . ? O4 Yb2 N6 72.20(11) . . ? N7 Yb2 N6 65.20(12) . . ? N15 Yb2 N6 134.64(12) . . ? O201 Yb2 N14 76.35(11) . . ? O2 Yb2 N14 71.07(11) . . ? O5 Yb2 N14 82.70(11) . . ? O4 Yb2 N14 130.60(11) . . ? N7 Yb2 N14 134.88(11) . . ? N15 Yb2 N14 64.97(12) . . ? N6 Yb2 N14 149.16(11) . . ? O201 Yb2 C30 165.06(12) . . ? O2 Yb2 C30 18.95(11) . . ? O5 Yb2 C30 84.72(12) . . ? O4 Yb2 C30 94.82(11) . . ? N7 Yb2 C30 47.42(11) . . ? N15 Yb2 C30 88.66(11) . . ? N6 Yb2 C30 111.86(11) . . ? N14 Yb2 C30 88.93(11) . . ? O201 Yb2 C64 91.38(12) . . ? O2 Yb2 C64 97.02(11) . . ? O5 Yb2 C64 165.59(11) . . ? O4 Yb2 C64 18.97(11) . . ? N7 Yb2 C64 87.86(11) . . ? N15 Yb2 C64 47.26(11) . . ? N6 Yb2 C64 89.16(11) . . ? N14 Yb2 C64 111.65(11) . . ? C30 Yb2 C64 96.54(11) . . ? C16 O1 Yb1 126.9(3) . . ? C30 O2 Yb2 125.8(3) . . ? C50 O3 Yb1 128.0(3) . . ? C64 O4 Yb2 124.9(3) . . ? Yb2 O5 H5A 118.4 . . ? Yb2 O5 H5B 120.8 . . ? H5A O5 H5B 119.2 . . ? Yb1 O6 H6A 122.7 . . ? Yb1 O6 H6B 132.1 . . ? H6A O6 H6B 105.2 . . ? C200 O200 Yb1 141.7(3) . . ? C200 O201 Yb2 137.9(3) . . ? O200 C200 O201 125.9(5) . . ? O200 C200 H200 121.3 . . ? O201 C200 H200 108.3 . . ? C16 N1 C17 117.7(4) . . ? C16 N1 C19 126.4(4) . . ? C17 N1 C19 115.4(4) . . ? C15 N2 C11 119.1(4) . . ? C15 N2 Yb1 117.1(3) . . ? C11 N2 Yb1 121.5(3) . . ? C10 N3 N4 104.9(4) . . ? C10 N3 Yb1 116.1(3) . . ? N4 N3 Yb1 138.9(3) . . ? N3 N4 C8 111.3(4) . . ? N3 N4 C7 122.3(4) . . ? C8 N4 C7 125.4(4) . . ? N6 N5 C22 111.3(4) . . ? N6 N5 C21 122.0(4) . . ? C22 N5 C21 126.4(4) . . ? C24 N6 N5 104.6(3) . . ? C24 N6 Yb2 115.3(3) . . ? N5 N6 Yb2 139.7(3) . . ? C29 N7 C25 119.0(4) . . ? C29 N7 Yb2 117.3(3) . . ? C25 N7 Yb2 119.5(3) . . ? C30 N8 C31 125.7(4) . . ? C30 N8 C33 117.3(4) . . ? C31 N8 C33 116.4(4) . . ? C45 N9 C49 119.3(4) . . ? C45 N9 Yb1 121.0(3) . . ? C49 N9 Yb1 119.4(3) . . ? C50 N10 C53 127.3(4) . . ? C50 N10 C51 118.1(4) . . ? C53 N10 C51 114.6(4) . . ? C44 N11 N12 103.7(3) . . ? C44 N11 Yb1 110.8(3) . . ? N12 N11 Yb1 134.1(3) . . ? C42 N12 N11 111.9(4) . . ? C42 N12 C41 126.7(4) . . ? N11 N12 C41 121.1(4) . . ? C56 N13 N14 111.6(4) . . ? C56 N13 C55 127.3(4) . . ? N14 N13 C55 121.0(3) . . ? C58 N14 N13 105.0(3) . . ? C58 N14 Yb2 113.6(3) . . ? N13 N14 Yb2 137.7(3) . . ? C59 N15 C63 119.2(4) . . ? C59 N15 Yb2 119.6(3) . . ? C63 N15 Yb2 117.9(3) . . ? C64 N16 C67 117.6(4) . . ? C64 N16 C65 125.7(4) . . ? C67 N16 C65 116.2(4) . . ? C2 C1 C6 119.5(4) . . ? C2 C1 C21 122.1(4) . . ? C6 C1 C21 118.3(4) . . ? C1 C2 C3 121.2(4) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C2 C3 C4 119.5(5) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.7(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.4(4) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 118.8(4) . . ? C5 C6 C7 122.2(4) . . ? C1 C6 C7 119.0(4) . . ? N4 C7 C6 112.4(4) . . ? N4 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N4 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? N4 C8 C9 107.6(4) . . ? N4 C8 H8 126.2 . . ? C9 C8 H8 126.2 . . ? C8 C9 C10 105.0(4) . . ? C8 C9 H9 127.5 . . ? C10 C9 H9 127.5 . . ? N3 C10 C9 111.1(4) . . ? N3 C10 C11 119.3(4) . . ? C9 C10 C11 129.5(4) . . ? N2 C11 C12 121.7(4) . . ? N2 C11 C10 115.4(4) . . ? C12 C11 C10 123.0(4) . . ? C13 C12 C11 118.9(4) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 119.5(4) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 118.1(4) . . ? C15 C14 H14 121.0 . . ? C13 C14 H14 121.0 . . ? N2 C15 C14 122.3(4) . . ? N2 C15 C16 110.2(4) . . ? C14 C15 C16 127.5(4) . . ? O1 C16 N1 119.5(4) . . ? O1 C16 C15 115.6(4) . . ? N1 C16 C15 124.8(4) . . ? O1 C16 Yb1 34.3(2) . . ? N1 C16 Yb1 152.1(3) . . ? C15 C16 Yb1 81.9(2) . . ? N1 C17 C18 109.5(4) . . ? N1 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? N1 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C20 112.3(4) . . ? N1 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N1 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 C1 113.3(4) . . ? N5 C21 H21A 108.9 . . ? C1 C21 H21A 108.9 . . ? N5 C21 H21B 108.9 . . ? C1 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? N5 C22 C23 107.7(4) . . ? N5 C22 H22 126.1 . . ? C23 C22 H22 126.1 . . ? C22 C23 C24 104.9(4) . . ? C22 C23 H23 127.6 . . ? C24 C23 H23 127.6 . . ? N6 C24 C23 111.5(4) . . ? N6 C24 C25 118.9(4) . . ? C23 C24 C25 129.6(4) . . ? N7 C25 C26 121.9(4) . . ? N7 C25 C24 115.5(4) . . ? C26 C25 C24 122.6(4) . . ? C27 C26 C25 118.5(4) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C28 C27 C26 119.4(4) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 118.6(4) . . ? C29 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? N7 C29 C28 122.3(4) . . ? N7 C29 C30 110.0(4) . . ? C28 C29 C30 127.3(4) . . ? O2 C30 N8 120.6(4) . . ? O2 C30 C29 115.6(4) . . ? N8 C30 C29 123.8(4) . . ? O2 C30 Yb2 35.20(19) . . ? N8 C30 Yb2 152.5(3) . . ? C29 C30 Yb2 81.9(2) . . ? N8 C31 C32 112.5(4) . . ? N8 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? N8 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N8 C33 C34 111.9(4) . . ? N8 C33 H33A 109.2 . . ? C34 C33 H33A 109.2 . . ? N8 C33 H33B 109.2 . . ? C34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 119.4(4) . . ? C36 C35 C55 117.6(4) . . ? C40 C35 C55 123.0(4) . . ? C37 C36 C35 121.0(4) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C36 C37 C38 119.9(4) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C37 C38 C39 119.8(4) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C38 C39 C40 121.4(4) . . ? C38 C39 H39 119.3 . . ? C40 C39 H39 119.3 . . ? C39 C40 C35 118.5(4) . . ? C39 C40 C41 118.8(4) . . ? C35 C40 C41 122.8(4) . . ? N12 C41 C40 111.8(4) . . ? N12 C41 H41A 109.3 . . ? C40 C41 H41A 109.3 . . ? N12 C41 H41B 109.3 . . ? C40 C41 H41B 109.3 . . ? H41A C41 H41B 107.9 . . ? N12 C42 C43 107.6(4) . . ? N12 C42 H42 126.2 . . ? C43 C42 H42 126.2 . . ? C42 C43 C44 104.6(4) . . ? C42 C43 H43 127.7 . . ? C44 C43 H43 127.7 . . ? N11 C44 C43 112.2(4) . . ? N11 C44 C45 118.2(4) . . ? C43 C44 C45 129.6(4) . . ? N9 C45 C46 122.6(4) . . ? N9 C45 C44 116.2(4) . . ? C46 C45 C44 121.1(4) . . ? C47 C46 C45 117.2(4) . . ? C47 C46 H46 121.4 . . ? C45 C46 H46 121.4 . . ? C46 C47 C48 120.5(5) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C49 C48 C47 118.9(5) . . ? C49 C48 H48 120.5 . . ? C47 C48 H48 120.5 . . ? N9 C49 C48 121.0(4) . . ? N9 C49 C50 109.8(4) . . ? C48 C49 C50 129.2(4) . . ? O3 C50 N10 119.3(4) . . ? O3 C50 C49 116.4(4) . . ? N10 C50 C49 124.3(4) . . ? O3 C50 Yb1 33.9(2) . . ? N10 C50 Yb1 152.7(3) . . ? C49 C50 Yb1 82.7(3) . . ? N10 C51 C52 111.8(4) . . ? N10 C51 H51A 109.3 . . ? C52 C51 H51A 109.3 . . ? N10 C51 H51B 109.3 . . ? C52 C51 H51B 109.3 . . ? H51A C51 H51B 107.9 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N10 C53 C54 111.7(4) . . ? N10 C53 H53A 109.3 . . ? C54 C53 H53A 109.3 . . ? N10 C53 H53B 109.3 . . ? C54 C53 H53B 109.3 . . ? H53A C53 H53B 107.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N13 C55 C35 110.2(4) . . ? N13 C55 H55A 109.6 . . ? C35 C55 H55A 109.6 . . ? N13 C55 H55B 109.6 . . ? C35 C55 H55B 109.6 . . ? H55A C55 H55B 108.1 . . ? N13 C56 C57 107.7(4) . . ? N13 C56 H56 126.1 . . ? C57 C56 H56 126.1 . . ? C56 C57 C58 104.8(4) . . ? C56 C57 H57 127.6 . . ? C58 C57 H57 127.6 . . ? N14 C58 C57 110.9(4) . . ? N14 C58 C59 119.9(4) . . ? C57 C58 C59 129.1(4) . . ? N15 C59 C60 121.5(4) . . ? N15 C59 C58 116.0(4) . . ? C60 C59 C58 122.5(4) . . ? C61 C60 C59 118.9(4) . . ? C61 C60 H60 120.5 . . ? C59 C60 H60 120.5 . . ? C60 C61 C62 119.8(4) . . ? C60 C61 H61 120.1 . . ? C62 C61 H61 120.1 . . ? C63 C62 C61 118.3(4) . . ? C63 C62 H62 120.8 . . ? C61 C62 H62 120.8 . . ? N15 C63 C62 122.2(4) . . ? N15 C63 C64 110.9(4) . . ? C62 C63 C64 126.5(4) . . ? O4 C64 N16 121.1(4) . . ? O4 C64 C63 115.9(4) . . ? N16 C64 C63 123.0(4) . . ? O4 C64 Yb2 36.1(2) . . ? N16 C64 Yb2 152.4(3) . . ? C63 C64 Yb2 82.0(2) . . ? N16 C65 C66 112.4(4) . . ? N16 C65 H65A 109.1 . . ? C66 C65 H65A 109.1 . . ? N16 C65 H65B 109.1 . . ? C66 C65 H65B 109.1 . . ? H65A C65 H65B 107.9 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N16 C67 C68 112.2(4) . . ? N16 C67 H67A 109.2 . . ? C68 C67 H67A 109.2 . . ? N16 C67 H67B 109.2 . . ? C68 C67 H67B 109.2 . . ? H67A C67 H67B 107.9 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O13 Cl1 O10 108.5(5) . . ? O13 Cl1 O11 107.3(4) . . ? O10 Cl1 O11 109.2(4) . . ? O13 Cl1 O12 110.0(3) . . ? O10 Cl1 O12 111.2(3) . . ? O11 Cl1 O12 110.5(3) . . ? O15 Cl2 O17 109.4(2) . . ? O15 Cl2 O16 109.6(2) . . ? O17 Cl2 O16 109.9(2) . . ? O15 Cl2 O14 109.3(2) . . ? O17 Cl2 O14 109.7(2) . . ? O16 Cl2 O14 109.0(2) . . ? O20 Cl3 O21 110.5(3) . . ? O20 Cl3 O19 109.9(3) . . ? O21 Cl3 O19 111.4(3) . . ? O20 Cl3 O18 108.9(3) . . ? O21 Cl3 O18 108.4(3) . . ? O19 Cl3 O18 107.7(3) . . ? O26 Cl5 O27 111.4(3) . . ? O26 Cl5 O28 109.6(3) . . ? O27 Cl5 O28 109.4(3) . . ? O26 Cl5 O29 108.6(3) . . ? O27 Cl5 O29 108.8(3) . . ? O28 Cl5 O29 109.0(3) . . ? N1S C1S H1S1 109.5 . . ? N1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? N1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O2S N1S O1S 121.9(5) . . ? O2S N1S C1S 120.2(5) . . ? O1S N1S C1S 116.1(5) . . ? N2S C2S H2S1 109.5 . . ? N2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? N2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? O3S N2S O4S 112.9(11) . . ? O3S N2S C2S 134.2(10) . . ? O4S N2S C2S 112.9(10) . . ? N3S C3S H3SA 109.5 . . ? N3S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? N3S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? O5S N3S O6S 148.2(11) . . ? O5S N3S C3S 109.1(10) . . ? O6S N3S C3S 102.7(9) . . ? H1B O1W H1A 120.7 . . ? O25 Cl4 O22 113.3(6) . . ? O25 Cl4 O23 113.7(6) . . ? O22 Cl4 O23 109.6(6) . . ? O25 Cl4 O24 110.8(5) . . ? O22 Cl4 O24 107.0(5) . . ? O23 Cl4 O24 101.6(5) . . ? O24 Cl4' O25' 105.0(11) . . ? O24 Cl4' O22' 116.1(9) . . ? O25' Cl4' O22' 110.6(10) . . ? O24 Cl4' O23' 108.8(9) . . ? O25' Cl4' O23' 114.4(14) . . ? O22' Cl4' O23' 102.2(9) . . ? Cl4' O24 Cl4 19.1(4) . . ? 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 O200 Yb1 O1 C16 -176.7(3) . . . . ? O3 Yb1 O1 C16 65.8(4) . . . . ? O6 Yb1 O1 C16 -87.1(4) . . . . ? N2 Yb1 O1 C16 -0.6(3) . . . . ? N9 Yb1 O1 C16 125.6(4) . . . . ? N3 Yb1 O1 C16 -14.2(4) . . . . ? N11 Yb1 O1 C16 -167.2(4) . . . . ? C50 Yb1 O1 C16 83.1(4) . . . . ? O201 Yb2 O2 C30 166.6(3) . . . . ? O5 Yb2 O2 C30 77.1(3) . . . . ? O4 Yb2 O2 C30 -71.0(3) . . . . ? N7 Yb2 O2 C30 -5.2(3) . . . . ? N15 Yb2 O2 C30 -132.2(4) . . . . ? N6 Yb2 O2 C30 5.3(4) . . . . ? N14 Yb2 O2 C30 159.8(4) . . . . ? C64 Yb2 O2 C30 -89.7(3) . . . . ? O1 Yb1 O3 C50 69.9(4) . . . . ? O200 Yb1 O3 C50 -82.1(4) . . . . ? O6 Yb1 O3 C50 -167.0(3) . . . . ? N2 Yb1 O3 C50 129.2(4) . . . . ? N9 Yb1 O3 C50 0.4(4) . . . . ? N3 Yb1 O3 C50 -163.2(4) . . . . ? N11 Yb1 O3 C50 -9.6(4) . . . . ? C16 Yb1 O3 C50 87.3(4) . . . . ? O201 Yb2 O4 C64 74.4(3) . . . . ? O2 Yb2 O4 C64 -78.2(3) . . . . ? O5 Yb2 O4 C64 176.2(3) . . . . ? N7 Yb2 O4 C64 -138.9(3) . . . . ? N15 Yb2 O4 C64 -9.8(3) . . . . ? N6 Yb2 O4 C64 152.5(4) . . . . ? N14 Yb2 O4 C64 -3.4(4) . . . . ? C30 Yb2 O4 C64 -96.1(3) . . . . ? O1 Yb1 O200 C200 -64.0(6) . . . . ? O3 Yb1 O200 C200 58.2(5) . . . . ? O6 Yb1 O200 C200 -154.6(5) . . . . ? N2 Yb1 O200 C200 122.5(5) . . . . ? N9 Yb1 O200 C200 -7.0(5) . . . . ? N3 Yb1 O200 C200 129.6(6) . . . . ? N11 Yb1 O200 C200 -73.2(5) . . . . ? C16 Yb1 O200 C200 -68.7(8) . . . . ? C50 Yb1 O200 C200 40.2(5) . . . . ? O2 Yb2 O201 C200 33.8(6) . . . . ? O5 Yb2 O201 C200 122.8(5) . . . . ? O4 Yb2 O201 C200 -89.7(5) . . . . ? N7 Yb2 O201 C200 -159.6(5) . . . . ? N15 Yb2 O201 C200 -24.3(5) . . . . ? N6 Yb2 O201 C200 -160.3(5) . . . . ? N14 Yb2 O201 C200 40.5(5) . . . . ? C30 Yb2 O201 C200 50.7(8) . . . . ? C64 Yb2 O201 C200 -71.4(5) . . . . ? Yb1 O200 C200 O201 172.3(3) . . . . ? Yb2 O201 C200 O200 -139.5(4) . . . . ? O1 Yb1 N2 C15 13.5(3) . . . . ? O200 Yb1 N2 C15 -170.3(3) . . . . ? O3 Yb1 N2 C15 -102.6(3) . . . . ? O6 Yb1 N2 C15 106.7(3) . . . . ? N9 Yb1 N2 C15 -49.8(3) . . . . ? N3 Yb1 N2 C15 -178.0(4) . . . . ? N11 Yb1 N2 C15 31.6(4) . . . . ? C16 Yb1 N2 C15 13.2(3) . . . . ? C50 Yb1 N2 C15 -88.6(3) . . . . ? O1 Yb1 N2 C11 176.3(4) . . . . ? O200 Yb1 N2 C11 -7.5(5) . . . . ? O3 Yb1 N2 C11 60.2(4) . . . . ? O6 Yb1 N2 C11 -90.5(4) . . . . ? N9 Yb1 N2 C11 113.0(4) . . . . ? N3 Yb1 N2 C11 -15.3(3) . . . . ? N11 Yb1 N2 C11 -165.6(3) . . . . ? C16 Yb1 N2 C11 176.0(4) . . . . ? C50 Yb1 N2 C11 74.2(4) . . . . ? O1 Yb1 N3 C10 22.8(4) . . . . ? O200 Yb1 N3 C10 -166.4(3) . . . . ? O3 Yb1 N3 C10 -74.7(3) . . . . ? O6 Yb1 N3 C10 103.2(3) . . . . ? N2 Yb1 N3 C10 9.1(3) . . . . ? N9 Yb1 N3 C10 -95.5(3) . . . . ? N11 Yb1 N3 C10 146.6(3) . . . . ? C16 Yb1 N3 C10 18.0(4) . . . . ? C50 Yb1 N3 C10 -79.8(3) . . . . ? O1 Yb1 N3 N4 -159.2(4) . . . . ? O200 Yb1 N3 N4 11.6(4) . . . . ? O3 Yb1 N3 N4 103.3(5) . . . . ? O6 Yb1 N3 N4 -78.8(5) . . . . ? N2 Yb1 N3 N4 -172.9(5) . . . . ? N9 Yb1 N3 N4 82.5(5) . . . . ? N11 Yb1 N3 N4 -35.4(6) . . . . ? C16 Yb1 N3 N4 -164.0(4) . . . . ? C50 Yb1 N3 N4 98.2(4) . . . . ? C10 N3 N4 C8 0.6(6) . . . . ? Yb1 N3 N4 C8 -177.6(4) . . . . ? C10 N3 N4 C7 169.8(4) . . . . ? Yb1 N3 N4 C7 -8.4(7) . . . . ? C22 N5 N6 C24 -0.9(5) . . . . ? C21 N5 N6 C24 -175.5(4) . . . . ? C22 N5 N6 Yb2 171.7(3) . . . . ? C21 N5 N6 Yb2 -2.8(7) . . . . ? O201 Yb2 N6 C24 164.6(3) . . . . ? O2 Yb2 N6 C24 -25.5(4) . . . . ? O5 Yb2 N6 C24 -102.5(3) . . . . ? O4 Yb2 N6 C24 64.4(3) . . . . ? N7 Yb2 N6 C24 -15.0(3) . . . . ? N15 Yb2 N6 C24 87.5(3) . . . . ? N14 Yb2 N6 C24 -152.9(3) . . . . ? C30 Yb2 N6 C24 -23.6(3) . . . . ? C64 Yb2 N6 C24 73.1(3) . . . . ? O201 Yb2 N6 N5 -7.5(4) . . . . ? O2 Yb2 N6 N5 162.4(4) . . . . ? O5 Yb2 N6 N5 85.4(4) . . . . ? O4 Yb2 N6 N5 -107.7(4) . . . . ? N7 Yb2 N6 N5 172.9(5) . . . . ? N15 Yb2 N6 N5 -84.6(5) . . . . ? N14 Yb2 N6 N5 35.0(5) . . . . ? C30 Yb2 N6 N5 164.2(4) . . . . ? C64 Yb2 N6 N5 -99.1(4) . . . . ? O201 Yb2 N7 C29 177.5(3) . . . . ? O2 Yb2 N7 C29 -10.4(3) . . . . ? O5 Yb2 N7 C29 -102.5(3) . . . . ? O4 Yb2 N7 C29 100.6(3) . . . . ? N15 Yb2 N7 C29 48.7(3) . . . . ? N6 Yb2 N7 C29 178.3(3) . . . . ? N14 Yb2 N7 C29 -30.7(4) . . . . ? C30 Yb2 N7 C29 -12.7(3) . . . . ? C64 Yb2 N7 C29 88.2(3) . . . . ? O201 Yb2 N7 C25 20.8(4) . . . . ? O2 Yb2 N7 C25 -167.2(3) . . . . ? O5 Yb2 N7 C25 100.8(3) . . . . ? O4 Yb2 N7 C25 -56.2(3) . . . . ? N15 Yb2 N7 C25 -108.0(3) . . . . ? N6 Yb2 N7 C25 21.5(3) . . . . ? N14 Yb2 N7 C25 172.5(3) . . . . ? C30 Yb2 N7 C25 -169.4(4) . . . . ? C64 Yb2 N7 C25 -68.5(3) . . . . ? O1 Yb1 N9 C45 64.7(3) . . . . ? O200 Yb1 N9 C45 -88.5(3) . . . . ? O3 Yb1 N9 C45 179.4(4) . . . . ? O6 Yb1 N9 C45 -13.0(5) . . . . ? N2 Yb1 N9 C45 120.7(3) . . . . ? N3 Yb1 N9 C45 -158.8(3) . . . . ? N11 Yb1 N9 C45 -9.1(3) . . . . ? C16 Yb1 N9 C45 79.9(3) . . . . ? C50 Yb1 N9 C45 179.5(4) . . . . ? O1 Yb1 N9 C49 -122.0(3) . . . . ? O200 Yb1 N9 C49 84.8(3) . . . . ? O3 Yb1 N9 C49 -7.3(3) . . . . ? O6 Yb1 N9 C49 160.3(3) . . . . ? N2 Yb1 N9 C49 -66.0(3) . . . . ? N3 Yb1 N9 C49 14.5(4) . . . . ? N11 Yb1 N9 C49 164.2(4) . . . . ? C16 Yb1 N9 C49 -106.7(3) . . . . ? C50 Yb1 N9 C49 -7.1(3) . . . . ? O1 Yb1 N11 C44 -65.4(3) . . . . ? O200 Yb1 N11 C44 109.4(3) . . . . ? O3 Yb1 N11 C44 31.7(3) . . . . ? O6 Yb1 N11 C44 -160.5(3) . . . . ? N2 Yb1 N11 C44 -83.0(3) . . . . ? N9 Yb1 N11 C44 21.7(3) . . . . ? N3 Yb1 N11 C44 157.1(3) . . . . ? C16 Yb1 N11 C44 -69.5(3) . . . . ? C50 Yb1 N11 C44 28.5(3) . . . . ? O1 Yb1 N11 N12 70.8(4) . . . . ? O200 Yb1 N11 N12 -114.3(4) . . . . ? O3 Yb1 N11 N12 168.0(3) . . . . ? O6 Yb1 N11 N12 -24.3(4) . . . . ? N2 Yb1 N11 N12 53.3(4) . . . . ? N9 Yb1 N11 N12 157.9(4) . . . . ? N3 Yb1 N11 N12 -66.6(5) . . . . ? C16 Yb1 N11 N12 66.7(4) . . . . ? C50 Yb1 N11 N12 164.7(4) . . . . ? C44 N11 N12 C42 1.6(5) . . . . ? Yb1 N11 N12 C42 -136.7(3) . . . . ? C44 N11 N12 C41 -172.3(4) . . . . ? Yb1 N11 N12 C41 49.4(5) . . . . ? C56 N13 N14 C58 -0.3(5) . . . . ? C55 N13 N14 C58 176.9(4) . . . . ? C56 N13 N14 Yb2 155.2(3) . . . . ? C55 N13 N14 Yb2 -27.6(6) . . . . ? O201 Yb2 N14 C58 -112.6(3) . . . . ? O2 Yb2 N14 C58 63.6(3) . . . . ? O5 Yb2 N14 C58 154.8(3) . . . . ? O4 Yb2 N14 C58 -25.4(3) . . . . ? N7 Yb2 N14 C58 83.2(3) . . . . ? N15 Yb2 N14 C58 -19.0(3) . . . . ? N6 Yb2 N14 C58 -155.9(3) . . . . ? C30 Yb2 N14 C58 70.0(3) . . . . ? C64 Yb2 N14 C58 -26.6(3) . . . . ? O201 Yb2 N14 N13 93.3(4) . . . . ? O2 Yb2 N14 N13 -90.5(4) . . . . ? O5 Yb2 N14 N13 0.8(4) . . . . ? O4 Yb2 N14 N13 -179.5(4) . . . . ? N7 Yb2 N14 N13 -70.9(4) . . . . ? N15 Yb2 N14 N13 -173.1(4) . . . . ? N6 Yb2 N14 N13 50.0(5) . . . . ? C30 Yb2 N14 N13 -84.0(4) . . . . ? C64 Yb2 N14 N13 179.4(4) . . . . ? O201 Yb2 N15 C59 96.7(3) . . . . ? O2 Yb2 N15 C59 -54.9(3) . . . . ? O5 Yb2 N15 C59 9.3(4) . . . . ? O4 Yb2 N15 C59 -164.7(3) . . . . ? N7 Yb2 N15 C59 -109.1(3) . . . . ? N6 Yb2 N15 C59 171.1(3) . . . . ? N14 Yb2 N15 C59 20.6(3) . . . . ? C30 Yb2 N15 C59 -68.8(3) . . . . ? C64 Yb2 N15 C59 -169.0(4) . . . . ? O201 Yb2 N15 C63 -103.9(3) . . . . ? O2 Yb2 N15 C63 104.5(3) . . . . ? O5 Yb2 N15 C63 168.7(3) . . . . ? O4 Yb2 N15 C63 -5.3(3) . . . . ? N7 Yb2 N15 C63 50.2(3) . . . . ? N6 Yb2 N15 C63 -29.5(4) . . . . ? N14 Yb2 N15 C63 180.0(3) . . . . ? C30 Yb2 N15 C63 90.5(3) . . . . ? C64 Yb2 N15 C63 -9.6(3) . . . . ? C6 C1 C2 C3 1.4(7) . . . . ? C21 C1 C2 C3 -177.5(4) . . . . ? C1 C2 C3 C4 -1.0(7) . . . . ? C2 C3 C4 C5 -0.4(7) . . . . ? C3 C4 C5 C6 1.4(7) . . . . ? C4 C5 C6 C1 -1.1(7) . . . . ? C4 C5 C6 C7 178.1(4) . . . . ? C2 C1 C6 C5 -0.3(6) . . . . ? C21 C1 C6 C5 178.6(4) . . . . ? C2 C1 C6 C7 -179.5(4) . . . . ? C21 C1 C6 C7 -0.6(6) . . . . ? N3 N4 C7 C6 -81.9(5) . . . . ? C8 N4 C7 C6 85.8(6) . . . . ? C5 C6 C7 N4 7.4(6) . . . . ? C1 C6 C7 N4 -173.4(4) . . . . ? N3 N4 C8 C9 -0.5(7) . . . . ? C7 N4 C8 C9 -169.3(5) . . . . ? N4 C8 C9 C10 0.3(7) . . . . ? N4 N3 C10 C9 -0.4(6) . . . . ? Yb1 N3 C10 C9 178.2(4) . . . . ? N4 N3 C10 C11 177.6(4) . . . . ? Yb1 N3 C10 C11 -3.7(6) . . . . ? C8 C9 C10 N3 0.1(7) . . . . ? C8 C9 C10 C11 -177.7(5) . . . . ? C15 N2 C11 C12 1.5(7) . . . . ? Yb1 N2 C11 C12 -161.0(4) . . . . ? C15 N2 C11 C10 -178.3(4) . . . . ? Yb1 N2 C11 C10 19.3(6) . . . . ? N3 C10 C11 N2 -9.5(7) . . . . ? C9 C10 C11 N2 168.1(5) . . . . ? N3 C10 C11 C12 170.7(5) . . . . ? C9 C10 C11 C12 -11.6(9) . . . . ? N2 C11 C12 C13 3.8(8) . . . . ? C10 C11 C12 C13 -176.5(5) . . . . ? C11 C12 C13 C14 -4.3(8) . . . . ? C12 C13 C14 C15 -0.3(8) . . . . ? C11 N2 C15 C14 -6.4(7) . . . . ? Yb1 N2 C15 C14 156.8(4) . . . . ? C11 N2 C15 C16 174.8(4) . . . . ? Yb1 N2 C15 C16 -22.0(5) . . . . ? C13 C14 C15 N2 5.7(7) . . . . ? C13 C14 C15 C16 -175.6(5) . . . . ? Yb1 O1 C16 N1 166.4(3) . . . . ? Yb1 O1 C16 C15 -10.7(5) . . . . ? C17 N1 C16 O1 0.2(6) . . . . ? C19 N1 C16 O1 -171.1(4) . . . . ? C17 N1 C16 C15 177.1(4) . . . . ? C19 N1 C16 C15 5.8(7) . . . . ? C17 N1 C16 Yb1 16.6(9) . . . . ? C19 N1 C16 Yb1 -154.8(5) . . . . ? N2 C15 C16 O1 21.3(5) . . . . ? C14 C15 C16 O1 -157.5(5) . . . . ? N2 C15 C16 N1 -155.7(4) . . . . ? C14 C15 C16 N1 25.5(7) . . . . ? N2 C15 C16 Yb1 15.2(3) . . . . ? C14 C15 C16 Yb1 -163.5(5) . . . . ? O200 Yb1 C16 O1 7.8(7) . . . . ? O3 Yb1 C16 O1 -118.2(4) . . . . ? O6 Yb1 C16 O1 93.4(4) . . . . ? N2 Yb1 C16 O1 179.2(4) . . . . ? N9 Yb1 C16 O1 -53.1(4) . . . . ? N3 Yb1 C16 O1 168.3(3) . . . . ? N11 Yb1 C16 O1 12.1(4) . . . . ? C50 Yb1 C16 O1 -99.9(4) . . . . ? O1 Yb1 C16 N1 -25.8(6) . . . . ? O200 Yb1 C16 N1 -18.1(10) . . . . ? O3 Yb1 C16 N1 -144.0(6) . . . . ? O6 Yb1 C16 N1 67.5(7) . . . . ? N2 Yb1 C16 N1 153.4(7) . . . . ? N9 Yb1 C16 N1 -78.9(7) . . . . ? N3 Yb1 C16 N1 142.5(6) . . . . ? N11 Yb1 C16 N1 -13.7(7) . . . . ? C50 Yb1 C16 N1 -125.7(7) . . . . ? O1 Yb1 C16 C15 170.2(5) . . . . ? O200 Yb1 C16 C15 178.0(5) . . . . ? O3 Yb1 C16 C15 52.0(2) . . . . ? O6 Yb1 C16 C15 -96.4(2) . . . . ? N2 Yb1 C16 C15 -10.6(2) . . . . ? N9 Yb1 C16 C15 117.1(2) . . . . ? N3 Yb1 C16 C15 -21.5(3) . . . . ? N11 Yb1 C16 C15 -177.7(2) . . . . ? C50 Yb1 C16 C15 70.3(2) . . . . ? C16 N1 C17 C18 -83.0(5) . . . . ? C19 N1 C17 C18 89.3(5) . . . . ? C16 N1 C19 C20 -103.9(5) . . . . ? C17 N1 C19 C20 84.6(5) . . . . ? N6 N5 C21 C1 82.2(5) . . . . ? C22 N5 C21 C1 -91.5(5) . . . . ? C2 C1 C21 N5 4.8(6) . . . . ? C6 C1 C21 N5 -174.1(4) . . . . ? N6 N5 C22 C23 0.7(5) . . . . ? C21 N5 C22 C23 175.0(4) . . . . ? N5 C22 C23 C24 -0.2(5) . . . . ? N5 N6 C24 C23 0.8(5) . . . . ? Yb2 N6 C24 C23 -174.0(3) . . . . ? N5 N6 C24 C25 -176.4(4) . . . . ? Yb2 N6 C24 C25 8.8(5) . . . . ? C22 C23 C24 N6 -0.4(5) . . . . ? C22 C23 C24 C25 176.5(4) . . . . ? C29 N7 C25 C26 -2.9(6) . . . . ? Yb2 N7 C25 C26 153.5(3) . . . . ? C29 N7 C25 C24 178.0(4) . . . . ? Yb2 N7 C25 C24 -25.6(5) . . . . ? N6 C24 C25 N7 10.2(6) . . . . ? C23 C24 C25 N7 -166.5(5) . . . . ? N6 C24 C25 C26 -168.9(4) . . . . ? C23 C24 C25 C26 14.4(7) . . . . ? N7 C25 C26 C27 -0.5(7) . . . . ? C24 C25 C26 C27 178.6(4) . . . . ? C25 C26 C27 C28 2.4(7) . . . . ? C26 C27 C28 C29 -1.1(7) . . . . ? C25 N7 C29 C28 4.3(6) . . . . ? Yb2 N7 C29 C28 -152.6(3) . . . . ? C25 N7 C29 C30 177.9(4) . . . . ? Yb2 N7 C29 C30 21.0(4) . . . . ? C27 C28 C29 N7 -2.3(7) . . . . ? C27 C28 C29 C30 -174.8(4) . . . . ? Yb2 O2 C30 N8 -161.6(3) . . . . ? Yb2 O2 C30 C29 18.2(5) . . . . ? C31 N8 C30 O2 167.2(4) . . . . ? C33 N8 C30 O2 -4.0(6) . . . . ? C31 N8 C30 C29 -12.6(7) . . . . ? C33 N8 C30 C29 176.2(4) . . . . ? C31 N8 C30 Yb2 144.1(5) . . . . ? C33 N8 C30 Yb2 -27.2(8) . . . . ? N7 C29 C30 O2 -25.0(5) . . . . ? C28 C29 C30 O2 148.2(4) . . . . ? N7 C29 C30 N8 154.8(4) . . . . ? C28 C29 C30 N8 -32.0(7) . . . . ? N7 C29 C30 Yb2 -14.5(3) . . . . ? C28 C29 C30 Yb2 158.7(4) . . . . ? O201 Yb2 C30 O2 -29.0(6) . . . . ? O5 Yb2 C30 O2 -101.9(3) . . . . ? O4 Yb2 C30 O2 111.5(3) . . . . ? N7 Yb2 C30 O2 173.6(4) . . . . ? N15 Yb2 C30 O2 45.9(3) . . . . ? N6 Yb2 C30 O2 -175.7(3) . . . . ? N14 Yb2 C30 O2 -19.1(3) . . . . ? C64 Yb2 C30 O2 92.6(3) . . . . ? O201 Yb2 C30 N8 6.9(9) . . . . ? O2 Yb2 C30 N8 35.9(6) . . . . ? O5 Yb2 C30 N8 -65.9(6) . . . . ? O4 Yb2 C30 N8 147.5(6) . . . . ? N7 Yb2 C30 N8 -150.5(7) . . . . ? N15 Yb2 C30 N8 81.8(6) . . . . ? N6 Yb2 C30 N8 -139.8(6) . . . . ? N14 Yb2 C30 N8 16.8(6) . . . . ? C64 Yb2 C30 N8 128.5(6) . . . . ? O201 Yb2 C30 C29 167.5(4) . . . . ? O2 Yb2 C30 C29 -163.5(5) . . . . ? O5 Yb2 C30 C29 94.7(2) . . . . ? O4 Yb2 C30 C29 -51.9(2) . . . . ? N7 Yb2 C30 C29 10.1(2) . . . . ? N15 Yb2 C30 C29 -117.6(2) . . . . ? N6 Yb2 C30 C29 20.8(3) . . . . ? N14 Yb2 C30 C29 177.4(2) . . . . ? C64 Yb2 C30 C29 -70.9(2) . . . . ? C30 N8 C31 C32 111.6(5) . . . . ? C33 N8 C31 C32 -77.1(5) . . . . ? C30 N8 C33 C34 81.2(5) . . . . ? C31 N8 C33 C34 -90.8(5) . . . . ? C40 C35 C36 C37 -0.7(7) . . . . ? C55 C35 C36 C37 178.7(4) . . . . ? C35 C36 C37 C38 0.0(7) . . . . ? C36 C37 C38 C39 -0.2(7) . . . . ? C37 C38 C39 C40 1.0(7) . . . . ? C38 C39 C40 C35 -1.6(7) . . . . ? C38 C39 C40 C41 177.1(4) . . . . ? C36 C35 C40 C39 1.4(6) . . . . ? C55 C35 C40 C39 -177.9(4) . . . . ? C36 C35 C40 C41 -177.3(4) . . . . ? C55 C35 C40 C41 3.4(7) . . . . ? C42 N12 C41 C40 -43.3(6) . . . . ? N11 N12 C41 C40 129.6(4) . . . . ? C39 C40 C41 N12 99.5(5) . . . . ? C35 C40 C41 N12 -81.8(5) . . . . ? N11 N12 C42 C43 -1.6(5) . . . . ? C41 N12 C42 C43 172.0(4) . . . . ? N12 C42 C43 C44 0.8(5) . . . . ? N12 N11 C44 C43 -1.1(5) . . . . ? Yb1 N11 C44 C43 148.2(3) . . . . ? N12 N11 C44 C45 177.1(4) . . . . ? Yb1 N11 C44 C45 -33.7(4) . . . . ? C42 C43 C44 N11 0.2(5) . . . . ? C42 C43 C44 C45 -177.7(4) . . . . ? C49 N9 C45 C46 -0.5(7) . . . . ? Yb1 N9 C45 C46 172.8(3) . . . . ? C49 N9 C45 C44 -177.3(4) . . . . ? Yb1 N9 C45 C44 -4.0(5) . . . . ? N11 C44 C45 N9 27.2(6) . . . . ? C43 C44 C45 N9 -155.1(4) . . . . ? N11 C44 C45 C46 -149.7(4) . . . . ? C43 C44 C45 C46 28.0(7) . . . . ? N9 C45 C46 C47 -4.7(7) . . . . ? C44 C45 C46 C47 171.9(5) . . . . ? C45 C46 C47 C48 4.0(8) . . . . ? C46 C47 C48 C49 1.8(9) . . . . ? C45 N9 C49 C48 6.6(7) . . . . ? Yb1 N9 C49 C48 -166.8(4) . . . . ? C45 N9 C49 C50 -174.9(4) . . . . ? Yb1 N9 C49 C50 11.7(5) . . . . ? C47 C48 C49 N9 -7.3(8) . . . . ? C47 C48 C49 C50 174.5(5) . . . . ? Yb1 O3 C50 N10 -172.7(3) . . . . ? Yb1 O3 C50 C49 5.6(6) . . . . ? C53 N10 C50 O3 178.6(4) . . . . ? C51 N10 C50 O3 1.0(6) . . . . ? C53 N10 C50 C49 0.4(7) . . . . ? C51 N10 C50 C49 -177.2(4) . . . . ? C53 N10 C50 Yb1 169.8(5) . . . . ? C51 N10 C50 Yb1 -7.8(9) . . . . ? N9 C49 C50 O3 -11.1(6) . . . . ? C48 C49 C50 O3 167.3(5) . . . . ? N9 C49 C50 N10 167.2(4) . . . . ? C48 C49 C50 N10 -14.4(8) . . . . ? N9 C49 C50 Yb1 -7.9(3) . . . . ? C48 C49 C50 Yb1 170.5(5) . . . . ? O1 Yb1 C50 O3 -114.3(4) . . . . ? O200 Yb1 C50 O3 97.1(4) . . . . ? O6 Yb1 C50 O3 26.9(7) . . . . ? N2 Yb1 C50 O3 -49.0(4) . . . . ? N9 Yb1 C50 O3 -179.5(4) . . . . ? N3 Yb1 C50 O3 15.9(4) . . . . ? N11 Yb1 C50 O3 172.1(4) . . . . ? C16 Yb1 C50 O3 -95.4(4) . . . . ? O1 Yb1 C50 N10 -100.4(7) . . . . ? O200 Yb1 C50 N10 111.0(7) . . . . ? O3 Yb1 C50 N10 13.9(6) . . . . ? O6 Yb1 C50 N10 40.8(10) . . . . ? N2 Yb1 C50 N10 -35.1(7) . . . . ? N9 Yb1 C50 N10 -165.6(8) . . . . ? N3 Yb1 C50 N10 29.8(7) . . . . ? N11 Yb1 C50 N10 -174.0(7) . . . . ? C16 Yb1 C50 N10 -81.5(7) . . . . ? O1 Yb1 C50 C49 70.8(3) . . . . ? O200 Yb1 C50 C49 -77.8(3) . . . . ? O3 Yb1 C50 C49 -174.9(5) . . . . ? O6 Yb1 C50 C49 -148.0(4) . . . . ? N2 Yb1 C50 C49 136.1(3) . . . . ? N9 Yb1 C50 C49 5.6(2) . . . . ? N3 Yb1 C50 C49 -159.0(3) . . . . ? N11 Yb1 C50 C49 -2.9(3) . . . . ? C16 Yb1 C50 C49 89.7(3) . . . . ? C50 N10 C51 C52 93.8(5) . . . . ? C53 N10 C51 C52 -84.0(5) . . . . ? C50 N10 C53 C54 93.0(6) . . . . ? C51 N10 C53 C54 -89.3(5) . . . . ? C56 N13 C55 C35 0.0(6) . . . . ? N14 N13 C55 C35 -176.8(4) . . . . ? C36 C35 C55 N13 -91.1(5) . . . . ? C40 C35 C55 N13 88.3(5) . . . . ? N14 N13 C56 C57 -0.1(5) . . . . ? C55 N13 C56 C57 -177.0(4) . . . . ? N13 C56 C57 C58 0.3(5) . . . . ? N13 N14 C58 C57 0.5(5) . . . . ? Yb2 N14 C58 C57 -161.8(3) . . . . ? N13 N14 C58 C59 -180.0(4) . . . . ? Yb2 N14 C58 C59 17.8(5) . . . . ? C56 C57 C58 N14 -0.5(5) . . . . ? C56 C57 C58 C59 180.0(4) . . . . ? C63 N15 C59 C60 0.1(6) . . . . ? Yb2 N15 C59 C60 159.2(3) . . . . ? C63 N15 C59 C58 -179.1(4) . . . . ? Yb2 N15 C59 C58 -20.0(5) . . . . ? N14 C58 C59 N15 0.2(6) . . . . ? C57 C58 C59 N15 179.7(4) . . . . ? N14 C58 C59 C60 -179.0(4) . . . . ? C57 C58 C59 C60 0.4(7) . . . . ? N15 C59 C60 C61 -2.6(6) . . . . ? C58 C59 C60 C61 176.6(4) . . . . ? C59 C60 C61 C62 2.4(7) . . . . ? C60 C61 C62 C63 0.1(7) . . . . ? C59 N15 C63 C62 2.5(6) . . . . ? Yb2 N15 C63 C62 -157.0(3) . . . . ? C59 N15 C63 C64 175.6(4) . . . . ? Yb2 N15 C63 C64 16.1(4) . . . . ? C61 C62 C63 N15 -2.6(7) . . . . ? C61 C62 C63 C64 -174.6(4) . . . . ? Yb2 O4 C64 N16 -158.3(3) . . . . ? Yb2 O4 C64 C63 22.0(5) . . . . ? C67 N16 C64 O4 -8.5(6) . . . . ? C65 N16 C64 O4 162.4(4) . . . . ? C67 N16 C64 C63 171.2(4) . . . . ? C65 N16 C64 C63 -17.9(7) . . . . ? C67 N16 C64 Yb2 -36.6(8) . . . . ? C65 N16 C64 Yb2 134.3(5) . . . . ? N15 C63 C64 O4 -24.0(5) . . . . ? C62 C63 C64 O4 148.7(4) . . . . ? N15 C63 C64 N16 156.3(4) . . . . ? C62 C63 C64 N16 -31.0(7) . . . . ? N15 C63 C64 Yb2 -11.1(3) . . . . ? C62 C63 C64 Yb2 161.6(4) . . . . ? O201 Yb2 C64 O4 -106.9(3) . . . . ? O2 Yb2 C64 O4 104.9(3) . . . . ? O5 Yb2 C64 O4 -8.5(7) . . . . ? N7 Yb2 C64 O4 39.1(3) . . . . ? N15 Yb2 C64 O4 167.8(4) . . . . ? N6 Yb2 C64 O4 -26.1(3) . . . . ? N14 Yb2 C64 O4 177.2(3) . . . . ? C30 Yb2 C64 O4 85.8(3) . . . . ? O201 Yb2 C64 N16 -63.8(6) . . . . ? O2 Yb2 C64 N16 148.0(6) . . . . ? O5 Yb2 C64 N16 34.7(9) . . . . ? O4 Yb2 C64 N16 43.1(6) . . . . ? N7 Yb2 C64 N16 82.2(6) . . . . ? N15 Yb2 C64 N16 -149.0(7) . . . . ? N6 Yb2 C64 N16 17.0(6) . . . . ? N14 Yb2 C64 N16 -139.6(6) . . . . ? C30 Yb2 C64 N16 128.9(6) . . . . ? O201 Yb2 C64 C63 93.0(2) . . . . ? O2 Yb2 C64 C63 -55.3(2) . . . . ? O5 Yb2 C64 C63 -168.6(4) . . . . ? O4 Yb2 C64 C63 -160.1(5) . . . . ? N7 Yb2 C64 C63 -121.0(2) . . . . ? N15 Yb2 C64 C63 7.7(2) . . . . ? N6 Yb2 C64 C63 173.7(2) . . . . ? N14 Yb2 C64 C63 17.1(3) . . . . ? C30 Yb2 C64 C63 -74.3(2) . . . . ? C64 N16 C65 C66 120.6(5) . . . . ? C67 N16 C65 C66 -68.4(6) . . . . ? C64 N16 C67 C68 -78.1(5) . . . . ? C65 N16 C67 C68 110.1(5) . . . . ? O25' Cl4' O24 Cl4 -165(2) . . . . ? O22' Cl4' O24 Cl4 72.6(17) . . . . ? O23' Cl4' O24 Cl4 -42.0(16) . . . . ? O25 Cl4 O24 Cl4' 89.5(18) . . . . ? O22 Cl4 O24 Cl4' -34.5(16) . . . . ? O23 Cl4 O24 Cl4' -149.4(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O18 0.85 1.87 2.710(6) 169.9 . O5 H5B O24 0.85 1.95 2.786(7) 169.2 1_565 O6 H6A O25 0.85 2.25 3.055(8) 159.1 1_565 O6 H6A O23' 0.85 2.16 3.004(14) 173.2 1_565 O1W H1B O4S 0.85 2.47 3.239(14) 151.2 . O1W H1A O29 0.85 2.35 2.869(6) 120.0 . O1W H1A O26 0.85 2.38 3.227(7) 179.9 . _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.826 _refine_diff_density_min -1.456 _refine_diff_density_rms 0.145 #===END data_imw809m _database_code_depnum_ccdc_archive 'CCDC 630967' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H42 Cl3 La N8 O16' _chemical_formula_weight 1064.02 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' La La -0.2871 2.4523 '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 10.3119(11) _cell_length_b 14.1937(11) _cell_length_c 16.5841(15) _cell_angle_alpha 85.976(4) _cell_angle_beta 74.542(4) _cell_angle_gamma 73.206(3) _cell_volume 2239.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8708 _cell_measurement_theta_min 5.092 _cell_measurement_theta_max 54.988 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 1.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7362 _exptl_absorpt_correction_T_max 0.8991 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 4000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 53702 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.57 _reflns_number_total 10302 _reflns_number_gt 9478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0812P)^2^+13.8222P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10302 _refine_ls_number_parameters 520 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1719 _refine_ls_wR_factor_gt 0.1693 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.088 _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 La1 La 0.10871(3) 0.27609(2) 0.261361(17) 0.02578(10) Uani 1 1 d . . . O2 O -0.0957(4) 0.4011(3) 0.2262(2) 0.0370(9) Uani 1 1 d . A . O3 O -0.0776(5) 0.1895(3) 0.2532(3) 0.0444(10) Uani 1 1 d . A . O4 O 0.2358(5) 0.4024(3) 0.1929(3) 0.0404(10) Uani 1 1 d . A . N1 N 0.1536(4) 0.0654(3) 0.4229(3) 0.0259(8) Uani 1 1 d . . . N2 N 0.1678(5) 0.0955(3) 0.3426(3) 0.0301(9) Uani 1 1 d . A . N5 N 0.3341(4) 0.2825(3) 0.4171(3) 0.0256(8) Uani 1 1 d . . . N6 N 0.2226(4) 0.3249(3) 0.3860(3) 0.0237(8) Uani 1 1 d . A . N7 N 0.0024(4) 0.4585(3) 0.3398(3) 0.0267(9) Uani 1 1 d . A . N8 N -0.3056(6) 0.5161(4) 0.2669(3) 0.0427(12) Uani 1 1 d . . . C1 C 0.2166(6) 0.0666(4) 0.6151(4) 0.0317(11) Uani 1 1 d . . . H1 H 0.1304 0.0515 0.6386 0.038 Uiso 1 1 calc R . . C2 C 0.3177(6) 0.0457(4) 0.6596(4) 0.0364(12) Uani 1 1 d . . . H2 H 0.3016 0.0149 0.7126 0.044 Uiso 1 1 calc R . . C3 C 0.4428(6) 0.0700(4) 0.6264(4) 0.0349(12) Uani 1 1 d . . . H3 H 0.5111 0.0579 0.6574 0.042 Uiso 1 1 calc R . . C4 C 0.4668(5) 0.1117(4) 0.5479(4) 0.0317(11) Uani 1 1 d . A . H4 H 0.5529 0.1272 0.5251 0.038 Uiso 1 1 calc R . . C5 C 0.3672(5) 0.1314(4) 0.5015(3) 0.0271(10) Uani 1 1 d . . . C6 C 0.2394(5) 0.1093(3) 0.5366(3) 0.0257(10) Uani 1 1 d . A . C7 C 0.1251(5) 0.1343(4) 0.4909(3) 0.0254(9) Uani 1 1 d . A . H7A H 0.0350 0.1340 0.5311 0.030 Uiso 1 1 calc R . . H7B H 0.1154 0.2015 0.4679 0.030 Uiso 1 1 calc R . . C8 C 0.1741(5) -0.0324(4) 0.4300(4) 0.0283(10) Uani 1 1 d . A . H8 H 0.1695 -0.0689 0.4804 0.034 Uiso 1 1 calc R . . C9 C 0.2028(6) -0.0700(4) 0.3510(4) 0.0344(12) Uani 1 1 d . . . H9 H 0.2217 -0.1367 0.3354 0.041 Uiso 1 1 calc R A . C10 C 0.1978(6) 0.0126(4) 0.2985(4) 0.0343(12) Uani 1 1 d D A . C21 C 0.3987(5) 0.1754(4) 0.4152(3) 0.0281(10) Uani 1 1 d . A . H21A H 0.5015 0.1614 0.3926 0.034 Uiso 1 1 calc R . . H21B H 0.3630 0.1443 0.3774 0.034 Uiso 1 1 calc R . . C22 C 0.3712(5) 0.3477(4) 0.4543(4) 0.0314(11) Uani 1 1 d . A . H22 H 0.4463 0.3337 0.4804 0.038 Uiso 1 1 calc R . . C23 C 0.2804(6) 0.4389(4) 0.4477(3) 0.0303(11) Uani 1 1 d . . . H23 H 0.2796 0.5002 0.4678 0.036 Uiso 1 1 calc R A . C24 C 0.1900(5) 0.4212(4) 0.4051(3) 0.0261(10) Uani 1 1 d . A . C25 C 0.0748(5) 0.4931(4) 0.3811(3) 0.0267(10) Uani 1 1 d . . . C26 C 0.0451(6) 0.5934(4) 0.3979(4) 0.0346(12) Uani 1 1 d . A . H26 H 0.0973 0.6159 0.4278 0.042 Uiso 1 1 calc R . . C27 C -0.0609(7) 0.6590(4) 0.3703(4) 0.0400(13) Uani 1 1 d . . . H27 H -0.0807 0.7276 0.3791 0.048 Uiso 1 1 calc R A . C28 C -0.1370(6) 0.6244(4) 0.3304(4) 0.0399(14) Uani 1 1 d . A . H28 H -0.2112 0.6688 0.3116 0.048 Uiso 1 1 calc R . . C29 C -0.1057(6) 0.5231(4) 0.3172(3) 0.0318(11) Uani 1 1 d . . . C30 C -0.1723(6) 0.4764(4) 0.2688(3) 0.0356(12) Uani 1 1 d . A . C31 C -0.4144(7) 0.5828(7) 0.3312(5) 0.059(2) Uani 1 1 d . . . H31A H -0.3740 0.5901 0.3775 0.071 Uiso 1 1 calc R . . H31B H -0.4922 0.5530 0.3544 0.071 Uiso 1 1 calc R . . C32 C -0.4732(11) 0.6857(7) 0.2965(7) 0.086(4) Uani 1 1 d . . . H32A H -0.4017 0.7213 0.2846 0.129 Uiso 1 1 calc R . . H32B H -0.5565 0.7226 0.3379 0.129 Uiso 1 1 calc R . . H32C H -0.4985 0.6785 0.2448 0.129 Uiso 1 1 calc R . . C33 C -0.3578(8) 0.4728(5) 0.2089(4) 0.0455(14) Uani 1 1 d . . . H33A H -0.2804 0.4483 0.1586 0.055 Uiso 1 1 calc R . . H33B H -0.4321 0.5244 0.1909 0.055 Uiso 1 1 calc R . . C34 C -0.4151(9) 0.3902(5) 0.2468(5) 0.0535(17) Uani 1 1 d . . . H34A H -0.3414 0.3383 0.2636 0.080 Uiso 1 1 calc R . . H34B H -0.4485 0.3638 0.2057 0.080 Uiso 1 1 calc R . . H34C H -0.4932 0.4143 0.2960 0.080 Uiso 1 1 calc R . . Cl1 Cl 0.51196(17) 0.15344(14) 0.17416(13) 0.0585(5) Uani 1 1 d . . . O10 O 0.3800(4) 0.2022(4) 0.2295(3) 0.0467(11) Uani 1 1 d . A . O11 O 0.6222(5) 0.1582(4) 0.2089(5) 0.0703(18) Uani 1 1 d . A . O12 O 0.5221(8) 0.0544(6) 0.1657(8) 0.140(5) Uani 1 1 d . A . O13 O 0.5202(10) 0.2040(11) 0.0994(5) 0.156(5) Uani 1 1 d . A . Cl2 Cl -0.22501(12) 0.28689(9) 0.44897(7) 0.0279(2) Uani 1 1 d . . . O14 O -0.0819(4) 0.2815(3) 0.4023(2) 0.0323(8) Uani 1 1 d . A . O15 O -0.2692(4) 0.2135(3) 0.4165(3) 0.0388(9) Uani 1 1 d . A . O16 O -0.3135(4) 0.3827(3) 0.4399(3) 0.0420(10) Uani 1 1 d . A . O17 O -0.2270(5) 0.2674(4) 0.5350(3) 0.0512(12) Uani 1 1 d . A . O1 O 0.1200(9) 0.2862(5) 0.1068(4) 0.0285(14) Uiso 0.543(5) 1 d PDU A 1 N4 N 0.2673(10) 0.2469(7) -0.0190(6) 0.043(2) Uiso 0.543(5) 1 d PD A 1 C11 C 0.2439(8) 0.0066(5) 0.2131(3) 0.0323(15) Uiso 0.543(5) 1 d PGDU A 1 C12 C 0.3077(8) -0.0777(4) 0.1637(4) 0.0336(14) Uiso 0.543(5) 1 d PGU A 1 H12 H 0.3325 -0.1401 0.1890 0.040 Uiso 0.543(5) 1 calc PR A 1 C13 C 0.3351(8) -0.0706(4) 0.0771(4) 0.0372(14) Uiso 0.543(5) 1 d PGU A 1 H13 H 0.3787 -0.1282 0.0433 0.045 Uiso 0.543(5) 1 calc PR A 1 C14 C 0.2988(8) 0.0208(5) 0.0399(3) 0.0353(13) Uiso 0.543(5) 1 d PGU A 1 H14 H 0.3176 0.0257 -0.0192 0.042 Uiso 0.543(5) 1 calc PR A 1 C15 C 0.2351(8) 0.1051(4) 0.0894(4) 0.0328(13) Uiso 0.543(5) 1 d PGDU A 1 N3 N 0.2076(8) 0.0980(4) 0.1760(4) 0.0284(16) Uiso 0.543(5) 1 d PGDU A 1 C17 C 0.3956(18) 0.1828(15) -0.0762(11) 0.083(5) Uiso 0.543(5) 1 d PDU A 1 H17A H 0.4300 0.1202 -0.0480 0.100 Uiso 0.543(5) 1 calc PR A 1 H17B H 0.4707 0.2162 -0.0912 0.100 Uiso 0.543(5) 1 calc PR A 1 C18 C 0.358(2) 0.1624(17) -0.1536(12) 0.093(5) Uiso 0.543(5) 1 d PDU A 1 H18A H 0.2669 0.1489 -0.1379 0.139 Uiso 0.543(5) 1 calc PR A 1 H18B H 0.4298 0.1051 -0.1831 0.139 Uiso 0.543(5) 1 calc PR A 1 H18C H 0.3543 0.2198 -0.1903 0.139 Uiso 0.543(5) 1 calc PR A 1 C19 C 0.2338(14) 0.3529(9) -0.0429(9) 0.048(2) Uiso 0.543(5) 1 d PDU A 1 H19A H 0.3100 0.3629 -0.0906 0.057 Uiso 0.543(5) 1 calc PR A 1 H19B H 0.2291 0.3932 0.0047 0.057 Uiso 0.543(5) 1 calc PR A 1 C20 C 0.0972(15) 0.3872(11) -0.0670(9) 0.052(3) Uiso 0.543(5) 1 d PDU A 1 H20A H 0.0980 0.3437 -0.1105 0.078 Uiso 0.543(5) 1 calc PR A 1 H20B H 0.0845 0.4546 -0.0883 0.078 Uiso 0.543(5) 1 calc PR A 1 H20C H 0.0199 0.3858 -0.0178 0.078 Uiso 0.543(5) 1 calc PR A 1 C16 C 0.2073(11) 0.2212(8) 0.0556(6) 0.0329(16) Uiso 0.543(5) 1 d PDU A 1 O1' O 0.1746(10) 0.2713(6) 0.1095(5) 0.0274(16) Uiso 0.457(5) 1 d PDU A 2 C11' C 0.2059(9) 0.0205(6) 0.2048(3) 0.0288(16) Uiso 0.457(5) 1 d PGDU A 2 C12' C 0.2319(9) -0.0628(5) 0.1572(4) 0.0326(14) Uiso 0.457(5) 1 d PGU A 2 H12' H 0.2378 -0.1251 0.1834 0.039 Uiso 0.457(5) 1 calc PR A 2 C13' C 0.2491(10) -0.0551(5) 0.0712(4) 0.0361(15) Uiso 0.457(5) 1 d PGU A 2 H13' H 0.2668 -0.1121 0.0386 0.043 Uiso 0.457(5) 1 calc PR A 2 C14' C 0.2403(10) 0.0360(6) 0.0328(3) 0.0358(15) Uiso 0.457(5) 1 d PGU A 2 H14' H 0.2521 0.0413 -0.0260 0.043 Uiso 0.457(5) 1 calc PR A 2 C15' C 0.2144(10) 0.1194(5) 0.0805(5) 0.0348(14) Uiso 0.457(5) 1 d PGDU A 2 N3' N 0.1971(10) 0.1116(5) 0.1665(5) 0.0277(18) Uiso 0.457(5) 1 d PGDU A 2 N4' N 0.1062(12) 0.2221(7) 0.0043(7) 0.038(2) Uiso 0.457(5) 1 d PD A 2 C18' C 0.1392(17) 0.1432(13) -0.1313(9) 0.054(3) Uiso 0.457(5) 1 d PDU A 2 H18D H 0.0921 0.2003 -0.1600 0.081 Uiso 0.457(5) 1 calc PR A 2 H18E H 0.1354 0.0827 -0.1545 0.081 Uiso 0.457(5) 1 calc PR A 2 H18F H 0.2373 0.1421 -0.1394 0.081 Uiso 0.457(5) 1 calc PR A 2 C17' C 0.0667(16) 0.1500(11) -0.0389(8) 0.047(3) Uiso 0.457(5) 1 d PDU A 2 H17C H -0.0361 0.1705 -0.0314 0.056 Uiso 0.457(5) 1 calc PR A 2 H17D H 0.0925 0.0844 -0.0133 0.056 Uiso 0.457(5) 1 calc PR A 2 C19' C 0.0477(15) 0.3282(10) -0.0142(10) 0.049(3) Uiso 0.457(5) 1 d PDU A 2 H19C H -0.0005 0.3653 0.0389 0.059 Uiso 0.457(5) 1 calc PR A 2 H19D H -0.0222 0.3346 -0.0468 0.059 Uiso 0.457(5) 1 calc PR A 2 C20' C 0.1641(19) 0.3717(13) -0.0639(11) 0.053(3) Uiso 0.457(5) 1 d PDU A 2 H20D H 0.2387 0.3584 -0.0349 0.079 Uiso 0.457(5) 1 calc PR A 2 H20E H 0.1259 0.4430 -0.0689 0.079 Uiso 0.457(5) 1 calc PR A 2 H20F H 0.2024 0.3417 -0.1198 0.079 Uiso 0.457(5) 1 calc PR A 2 C16' C 0.1688(14) 0.2038(9) 0.0642(8) 0.0323(16) Uiso 0.457(5) 1 d PDU A 2 Cl3 Cl 0.24070(19) -0.34029(13) 0.18961(16) 0.0633(5) Uani 1 1 d . . . O21 O 0.1818(8) -0.2647(4) 0.2484(4) 0.0781(19) Uani 1 1 d . . . O20 O 0.3540(8) -0.3202(5) 0.1306(4) 0.0772(18) Uani 1 1 d . . . O18 O 0.2969(8) -0.4306(6) 0.2343(5) 0.085(2) Uiso 1 1 d . . . O19 O 0.1414(9) -0.3685(6) 0.1619(5) 0.098(2) Uiso 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 La1 0.02973(16) 0.02261(15) 0.02244(15) -0.00167(10) 0.00119(11) -0.01026(11) O2 0.041(2) 0.037(2) 0.0293(19) 0.0024(16) -0.0097(17) -0.0058(17) O3 0.036(2) 0.045(2) 0.051(3) -0.004(2) -0.0038(19) -0.0169(19) O4 0.047(2) 0.031(2) 0.037(2) -0.0033(16) 0.0083(18) -0.0185(18) N1 0.0201(19) 0.022(2) 0.034(2) -0.0007(16) -0.0026(16) -0.0067(15) N2 0.031(2) 0.028(2) 0.028(2) -0.0050(17) 0.0034(17) -0.0125(18) N5 0.0186(18) 0.022(2) 0.034(2) -0.0019(16) -0.0026(16) -0.0058(15) N6 0.0204(18) 0.0188(19) 0.027(2) -0.0012(15) 0.0003(15) -0.0042(15) N7 0.025(2) 0.024(2) 0.023(2) 0.0038(15) 0.0014(16) -0.0015(16) N8 0.041(3) 0.053(3) 0.030(2) -0.001(2) -0.012(2) -0.004(2) C1 0.030(3) 0.023(2) 0.040(3) 0.001(2) -0.008(2) -0.006(2) C2 0.035(3) 0.026(3) 0.045(3) 0.003(2) -0.012(2) -0.004(2) C3 0.031(3) 0.025(3) 0.049(3) -0.002(2) -0.017(2) -0.001(2) C4 0.021(2) 0.024(2) 0.048(3) -0.003(2) -0.010(2) -0.0028(19) C5 0.021(2) 0.019(2) 0.039(3) -0.0021(19) -0.007(2) -0.0022(17) C6 0.022(2) 0.016(2) 0.037(3) -0.0030(18) -0.0069(19) -0.0011(17) C7 0.019(2) 0.022(2) 0.031(2) -0.0020(19) -0.0022(18) -0.0036(17) C8 0.021(2) 0.023(2) 0.041(3) 0.000(2) -0.006(2) -0.0080(18) C9 0.028(3) 0.026(3) 0.045(3) -0.004(2) 0.002(2) -0.011(2) C10 0.036(3) 0.028(3) 0.035(3) -0.007(2) 0.007(2) -0.017(2) C21 0.021(2) 0.019(2) 0.038(3) -0.0028(19) 0.0000(19) -0.0020(17) C22 0.025(2) 0.029(3) 0.042(3) -0.002(2) -0.005(2) -0.011(2) C23 0.029(3) 0.024(2) 0.036(3) -0.003(2) -0.002(2) -0.010(2) C24 0.024(2) 0.020(2) 0.028(2) -0.0035(18) 0.0046(18) -0.0079(18) C25 0.026(2) 0.022(2) 0.024(2) 0.0002(18) 0.0034(18) -0.0044(18) C26 0.039(3) 0.024(2) 0.033(3) -0.003(2) 0.001(2) -0.004(2) C27 0.044(3) 0.024(3) 0.040(3) -0.003(2) 0.003(3) -0.002(2) C28 0.039(3) 0.028(3) 0.037(3) 0.009(2) -0.002(2) 0.006(2) C29 0.030(3) 0.030(3) 0.027(2) 0.006(2) -0.004(2) 0.000(2) C30 0.037(3) 0.039(3) 0.023(2) 0.007(2) -0.005(2) -0.004(2) C31 0.034(3) 0.081(6) 0.051(4) -0.019(4) -0.012(3) 0.006(3) C32 0.079(6) 0.068(6) 0.108(8) -0.041(5) -0.061(6) 0.029(5) C33 0.051(4) 0.045(4) 0.041(3) 0.002(3) -0.017(3) -0.010(3) C34 0.068(5) 0.046(4) 0.047(4) 0.004(3) -0.024(3) -0.010(3) Cl1 0.0375(8) 0.0544(10) 0.0694(11) -0.0347(9) 0.0233(8) -0.0170(7) O10 0.024(2) 0.057(3) 0.050(3) -0.026(2) 0.0065(18) -0.0060(18) O11 0.024(2) 0.057(3) 0.122(5) -0.011(3) -0.001(3) -0.013(2) O12 0.062(4) 0.070(5) 0.285(14) -0.093(7) -0.026(6) -0.009(4) O13 0.098(6) 0.298(16) 0.053(4) 0.026(7) 0.016(4) -0.064(8) Cl2 0.0225(5) 0.0347(6) 0.0262(6) 0.0037(5) -0.0028(4) -0.0113(5) O14 0.0203(17) 0.042(2) 0.0310(19) 0.0052(16) -0.0011(14) -0.0101(15) O15 0.037(2) 0.038(2) 0.043(2) -0.0016(18) -0.0038(18) -0.0196(18) O16 0.032(2) 0.035(2) 0.058(3) -0.0080(19) -0.0149(19) -0.0035(17) O17 0.055(3) 0.080(4) 0.029(2) 0.016(2) -0.0081(19) -0.040(3) Cl3 0.0439(9) 0.0352(8) 0.1057(16) -0.0078(9) -0.0005(9) -0.0185(7) O21 0.096(5) 0.048(3) 0.089(5) -0.004(3) 0.000(4) -0.040(3) O20 0.093(5) 0.083(4) 0.053(3) 0.001(3) 0.001(3) -0.040(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 La1 O1' 2.428(8) . ? La1 O2 2.506(4) . ? La1 O1 2.530(7) . ? La1 O4 2.549(4) . ? La1 O3 2.597(4) . ? La1 O10 2.607(4) . ? La1 O14 2.612(4) . ? La1 N3' 2.697(5) . ? La1 N7 2.770(4) . ? La1 N3 2.771(5) . ? La1 N2 2.794(5) . ? La1 N6 2.845(4) . ? O2 C30 1.258(7) . ? N1 C8 1.344(6) . ? N1 N2 1.353(6) . ? N1 C7 1.458(6) . ? N2 C10 1.343(7) . ? N5 C22 1.341(7) . ? N5 N6 1.350(6) . ? N5 C21 1.471(6) . ? N6 C24 1.350(6) . ? N7 C25 1.341(7) . ? N7 C29 1.344(7) . ? N8 C30 1.335(8) . ? N8 C33 1.463(8) . ? N8 C31 1.477(9) . ? C1 C2 1.386(8) . ? C1 C6 1.387(8) . ? C1 H1 0.9500 . ? C2 C3 1.392(8) . ? C2 H2 0.9500 . ? C3 C4 1.382(8) . ? C3 H3 0.9500 . ? C4 C5 1.397(7) . ? C4 H4 0.9500 . ? C5 C6 1.406(7) . ? C5 C21 1.513(7) . ? C6 C7 1.513(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.373(8) . ? C8 H8 0.9500 . ? C9 C10 1.408(8) . ? C9 H9 0.9500 . ? C10 C11 1.368(7) . ? C10 C11' 1.531(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.377(8) . ? C22 H22 0.9500 . ? C23 C24 1.394(7) . ? C23 H23 0.9500 . ? C24 C25 1.451(7) . ? C25 C26 1.398(7) . ? C26 C27 1.374(9) . ? C26 H26 0.9500 . ? C27 C28 1.355(10) . ? C27 H27 0.9500 . ? C28 C29 1.400(8) . ? C28 H28 0.9500 . ? C29 C30 1.479(9) . ? C31 C32 1.545(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.488(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? Cl1 O13 1.383(10) . ? Cl1 O12 1.393(7) . ? Cl1 O11 1.425(6) . ? Cl1 O10 1.432(4) . ? Cl2 O16 1.425(4) . ? Cl2 O17 1.429(4) . ? Cl2 O15 1.438(4) . ? Cl2 O14 1.455(4) . ? O1 C16 1.268(11) . ? N4 C16 1.306(12) . ? N4 C19 1.493(13) . ? N4 C17 1.495(14) . ? C11 C12 1.3900 . ? C11 N3 1.3900 . ? C12 C13 1.3900 . ? C12 H12 0.9500 . ? C13 C14 1.3900 . ? C13 H13 0.9500 . ? C14 C15 1.3900 . ? C14 H14 0.9500 . ? C15 N3 1.3900 . ? C15 C16 1.672(12) . ? C17 C18 1.502(17) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.502(14) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O1' C16' 1.280(12) . ? C11' C12' 1.3900 . ? C11' N3' 1.3900 . ? C12' C13' 1.3900 . ? C12' H12' 0.9500 . ? C13' C14' 1.3900 . ? C13' H13' 0.9500 . ? C14' C15' 1.3900 . ? C14' H14' 0.9500 . ? C15' C16' 1.195(14) . ? C15' N3' 1.3900 . ? N4' C16' 1.297(13) . ? N4' C17' 1.492(13) . ? N4' C19' 1.495(13) . ? C18' C17' 1.511(15) . ? C18' H18D 0.9800 . ? C18' H18E 0.9800 . ? C18' H18F 0.9800 . ? C17' H17C 0.9900 . ? C17' H17D 0.9900 . ? C19' C20' 1.527(15) . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C20' H20D 0.9800 . ? C20' H20E 0.9800 . ? C20' H20F 0.9800 . ? Cl3 O21 1.388(7) . ? Cl3 O19 1.390(9) . ? Cl3 O20 1.396(6) . ? Cl3 O18 1.481(8) . ? 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' La1 O2 77.6(2) . . ? O1' La1 O1 12.6(2) . . ? O2 La1 O1 66.1(2) . . ? O1' La1 O4 65.6(2) . . ? O2 La1 O4 82.08(15) . . ? O1 La1 O4 70.35(19) . . ? O1' La1 O3 86.4(2) . . ? O2 La1 O3 71.02(15) . . ? O1 La1 O3 78.1(2) . . ? O4 La1 O3 144.85(16) . . ? O1' La1 O10 78.5(3) . . ? O2 La1 O10 147.92(15) . . ? O1 La1 O10 91.1(2) . . ? O4 La1 O10 68.61(16) . . ? O3 La1 O10 128.31(15) . . ? O1' La1 O14 149.4(2) . . ? O2 La1 O14 79.95(13) . . ? O1 La1 O14 137.4(2) . . ? O4 La1 O14 131.13(13) . . ? O3 La1 O14 66.63(13) . . ? O10 La1 O14 129.29(14) . . ? O1' La1 N3' 54.7(3) . . ? O2 La1 N3' 112.8(2) . . ? O1 La1 N3' 59.2(2) . . ? O4 La1 N3' 110.9(2) . . ? O3 La1 N3' 62.5(2) . . ? O10 La1 N3' 68.6(2) . . ? O14 La1 N3' 118.0(2) . . ? O1' La1 N7 118.0(2) . . ? O2 La1 N7 59.67(13) . . ? O1 La1 N7 112.77(18) . . ? O4 La1 N7 65.88(12) . . ? O3 La1 N7 115.21(14) . . ? O10 La1 N7 115.54(14) . . ? O14 La1 N7 65.78(12) . . ? N3' La1 N7 171.66(19) . . ? O1' La1 N3 59.4(2) . . ? O2 La1 N3 117.31(18) . . ? O1 La1 N3 64.3(2) . . ? O4 La1 N3 113.33(19) . . ? O3 La1 N3 63.5(2) . . ? O10 La1 N3 66.33(19) . . ? O14 La1 N3 115.33(19) . . ? N3' La1 N3 5.2(3) . . ? N7 La1 N3 176.81(17) . . ? O1' La1 N2 116.6(2) . . ? O2 La1 N2 139.50(14) . . ? O1 La1 N2 121.65(18) . . ? O4 La1 N2 138.33(14) . . ? O3 La1 N2 72.34(15) . . ? O10 La1 N2 71.27(15) . . ? O14 La1 N2 70.11(12) . . ? N3' La1 N2 62.60(19) . . ? N7 La1 N2 125.17(12) . . ? N3 La1 N2 57.61(17) . . ? O1' La1 N6 135.0(2) . . ? O2 La1 N6 118.33(12) . . ? O1 La1 N6 144.09(19) . . ? O4 La1 N6 75.00(13) . . ? O3 La1 N6 137.79(13) . . ? O10 La1 N6 67.28(13) . . ? O14 La1 N6 74.51(12) . . ? N3' La1 N6 128.8(2) . . ? N7 La1 N6 58.68(12) . . ? N3 La1 N6 124.36(17) . . ? N2 La1 N6 79.66(12) . . ? C30 O2 La1 126.2(4) . . ? C8 N1 N2 112.2(4) . . ? C8 N1 C7 126.2(5) . . ? N2 N1 C7 121.5(4) . . ? C10 N2 N1 104.5(4) . . ? C10 N2 La1 118.6(4) . . ? N1 N2 La1 135.9(3) . . ? C22 N5 N6 112.5(4) . . ? C22 N5 C21 124.7(4) . . ? N6 N5 C21 122.7(4) . . ? N5 N6 C24 104.2(4) . . ? N5 N6 La1 135.9(3) . . ? C24 N6 La1 116.8(3) . . ? C25 N7 C29 118.0(5) . . ? C25 N7 La1 122.1(3) . . ? C29 N7 La1 117.5(4) . . ? C30 N8 C33 117.4(5) . . ? C30 N8 C31 125.4(5) . . ? C33 N8 C31 115.4(6) . . ? C2 C1 C6 121.0(5) . . ? C2 C1 H1 119.5 . . ? C6 C1 H1 119.5 . . ? C1 C2 C3 119.8(6) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 119.5(5) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 121.4(5) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 118.7(5) . . ? C4 C5 C21 119.7(5) . . ? C6 C5 C21 121.6(5) . . ? C1 C6 C5 119.6(5) . . ? C1 C6 C7 119.6(5) . . ? C5 C6 C7 120.7(5) . . ? N1 C7 C6 112.5(4) . . ? N1 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N1 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N1 C8 C9 107.6(5) . . ? N1 C8 H8 126.2 . . ? C9 C8 H8 126.2 . . ? C8 C9 C10 104.4(5) . . ? C8 C9 H9 127.8 . . ? C10 C9 H9 127.8 . . ? N2 C10 C11 123.9(5) . . ? N2 C10 C9 111.3(5) . . ? C11 C10 C9 123.7(5) . . ? N2 C10 C11' 118.7(5) . . ? C11 C10 C11' 16.2(5) . . ? C9 C10 C11' 129.7(5) . . ? N5 C21 C5 111.5(4) . . ? N5 C21 H21A 109.3 . . ? C5 C21 H21A 109.3 . . ? N5 C21 H21B 109.3 . . ? C5 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? N5 C22 C23 107.3(5) . . ? N5 C22 H22 126.4 . . ? C23 C22 H22 126.4 . . ? C22 C23 C24 104.7(5) . . ? C22 C23 H23 127.7 . . ? C24 C23 H23 127.7 . . ? N6 C24 C23 111.4(5) . . ? N6 C24 C25 121.4(5) . . ? C23 C24 C25 127.2(5) . . ? N7 C25 C26 122.3(5) . . ? N7 C25 C24 116.5(4) . . ? C26 C25 C24 121.2(5) . . ? C27 C26 C25 118.9(6) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C28 C27 C26 119.2(5) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C29 119.7(5) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? N7 C29 C28 121.7(6) . . ? N7 C29 C30 112.6(5) . . ? C28 C29 C30 125.2(5) . . ? O2 C30 N8 121.8(6) . . ? O2 C30 C29 117.0(5) . . ? N8 C30 C29 121.0(5) . . ? N8 C31 C32 112.6(7) . . ? N8 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? N8 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N8 C33 C34 112.6(6) . . ? N8 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? N8 C33 H33B 109.1 . . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O13 Cl1 O12 113.2(8) . . ? O13 Cl1 O11 109.9(6) . . ? O12 Cl1 O11 107.6(5) . . ? O13 Cl1 O10 106.6(5) . . ? O12 Cl1 O10 110.2(4) . . ? O11 Cl1 O10 109.2(3) . . ? Cl1 O10 La1 150.9(3) . . ? O16 Cl2 O17 110.5(3) . . ? O16 Cl2 O15 110.5(3) . . ? O17 Cl2 O15 109.7(3) . . ? O16 Cl2 O14 109.1(3) . . ? O17 Cl2 O14 108.4(3) . . ? O15 Cl2 O14 108.6(2) . . ? Cl2 O14 La1 151.2(2) . . ? C16 O1 La1 121.4(7) . . ? C16 N4 C19 119.7(10) . . ? C16 N4 C17 124.2(11) . . ? C19 N4 C17 114.1(12) . . ? C10 C11 C12 127.8(5) . . ? C10 C11 N3 111.9(5) . . ? C12 C11 N3 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 N3 120.0 . . ? C14 C15 C16 126.1(5) . . ? N3 C15 C16 113.2(5) . . ? C15 N3 C11 120.0 . . ? C15 N3 La1 115.2(3) . . ? C11 N3 La1 124.5(3) . . ? N4 C17 C18 108.4(15) . . ? N4 C17 H17A 110.0 . . ? C18 C17 H17A 110.0 . . ? N4 C17 H17B 110.0 . . ? C18 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? N4 C19 C20 112.2(10) . . ? N4 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N4 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? O1 C16 N4 119.8(10) . . ? O1 C16 C15 116.0(8) . . ? N4 C16 C15 124.2(8) . . ? C16' O1' La1 125.5(8) . . ? C12' C11' N3' 120.0 . . ? C12' C11' C10 120.8(5) . . ? N3' C11' C10 119.0(5) . . ? C11' C12' C13' 120.0 . . ? C11' C12' H12' 120.0 . . ? C13' C12' H12' 120.0 . . ? C14' C13' C12' 120.0 . . ? C14' C13' H13' 120.0 . . ? C12' C13' H13' 120.0 . . ? C13' C14' C15' 120.0 . . ? C13' C14' H14' 120.0 . . ? C15' C14' H14' 120.0 . . ? C16' C15' C14' 128.9(8) . . ? C16' C15' N3' 108.3(8) . . ? C14' C15' N3' 120.0 . . ? C15' N3' C11' 120.0 . . ? C15' N3' La1 119.7(4) . . ? C11' N3' La1 119.6(4) . . ? C16' N4' C17' 126.9(11) . . ? C16' N4' C19' 116.4(11) . . ? C17' N4' C19' 116.0(11) . . ? C17' C18' H18D 109.5 . . ? C17' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C17' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? N4' C17' C18' 111.4(12) . . ? N4' C17' H17C 109.3 . . ? C18' C17' H17C 109.3 . . ? N4' C17' H17D 109.3 . . ? C18' C17' H17D 109.3 . . ? H17C C17' H17D 108.0 . . ? N4' C19' C20' 110.7(12) . . ? N4' C19' H19C 109.5 . . ? C20' C19' H19C 109.5 . . ? N4' C19' H19D 109.5 . . ? C20' C19' H19D 109.5 . . ? H19C C19' H19D 108.1 . . ? C19' C20' H20D 109.5 . . ? C19' C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? C19' C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? C15' C16' O1' 119.6(10) . . ? C15' C16' N4' 117.1(10) . . ? O1' C16' N4' 123.1(11) . . ? O21 Cl3 O19 113.1(5) . . ? O21 Cl3 O20 109.3(4) . . ? O19 Cl3 O20 118.9(5) . . ? O21 Cl3 O18 107.0(5) . . ? O19 Cl3 O18 100.1(5) . . ? O20 Cl3 O18 107.4(4) . . ? 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' La1 O2 C30 -149.9(5) . . . . ? O1 La1 O2 C30 -155.2(5) . . . . ? O4 La1 O2 C30 -83.3(5) . . . . ? O3 La1 O2 C30 119.7(5) . . . . ? O10 La1 O2 C30 -107.0(5) . . . . ? O14 La1 O2 C30 51.1(5) . . . . ? N3' La1 O2 C30 167.3(5) . . . . ? N7 La1 O2 C30 -16.6(4) . . . . ? N3 La1 O2 C30 164.5(5) . . . . ? N2 La1 O2 C30 93.4(5) . . . . ? N6 La1 O2 C30 -15.1(5) . . . . ? C8 N1 N2 C10 0.2(6) . . . . ? C7 N1 N2 C10 177.8(4) . . . . ? C8 N1 N2 La1 168.2(4) . . . . ? C7 N1 N2 La1 -14.2(7) . . . . ? O1' La1 N2 C10 -15.7(5) . . . . ? O2 La1 N2 C10 86.9(4) . . . . ? O1 La1 N2 C10 -2.5(5) . . . . ? O4 La1 N2 C10 -98.1(4) . . . . ? O3 La1 N2 C10 60.8(4) . . . . ? O10 La1 N2 C10 -81.9(4) . . . . ? O14 La1 N2 C10 131.7(4) . . . . ? N3' La1 N2 C10 -6.9(4) . . . . ? N7 La1 N2 C10 169.6(4) . . . . ? N3 La1 N2 C10 -8.5(4) . . . . ? N6 La1 N2 C10 -151.2(4) . . . . ? O1' La1 N2 N1 177.6(5) . . . . ? O2 La1 N2 N1 -79.8(5) . . . . ? O1 La1 N2 N1 -169.2(5) . . . . ? O4 La1 N2 N1 95.2(5) . . . . ? O3 La1 N2 N1 -105.9(5) . . . . ? O10 La1 N2 N1 111.5(5) . . . . ? O14 La1 N2 N1 -35.0(4) . . . . ? N3' La1 N2 N1 -173.5(5) . . . . ? N7 La1 N2 N1 2.9(5) . . . . ? N3 La1 N2 N1 -175.2(5) . . . . ? N6 La1 N2 N1 42.1(4) . . . . ? C22 N5 N6 C24 0.1(5) . . . . ? C21 N5 N6 C24 175.7(4) . . . . ? C22 N5 N6 La1 158.3(4) . . . . ? C21 N5 N6 La1 -26.1(7) . . . . ? O1' La1 N6 N5 -72.9(5) . . . . ? O2 La1 N6 N5 -174.2(4) . . . . ? O1 La1 N6 N5 -86.5(5) . . . . ? O4 La1 N6 N5 -102.1(4) . . . . ? O3 La1 N6 N5 93.3(4) . . . . ? O10 La1 N6 N5 -29.3(4) . . . . ? O14 La1 N6 N5 116.6(4) . . . . ? N3' La1 N6 N5 2.9(5) . . . . ? N7 La1 N6 N5 -172.7(5) . . . . ? N3 La1 N6 N5 6.2(5) . . . . ? N2 La1 N6 N5 44.6(4) . . . . ? O1' La1 N6 C24 83.3(4) . . . . ? O2 La1 N6 C24 -18.0(4) . . . . ? O1 La1 N6 C24 69.7(5) . . . . ? O4 La1 N6 C24 54.2(3) . . . . ? O3 La1 N6 C24 -110.5(3) . . . . ? O10 La1 N6 C24 126.9(4) . . . . ? O14 La1 N6 C24 -87.2(3) . . . . ? N3' La1 N6 C24 159.1(4) . . . . ? N7 La1 N6 C24 -16.4(3) . . . . ? N3 La1 N6 C24 162.4(3) . . . . ? N2 La1 N6 C24 -159.2(3) . . . . ? O1' La1 N7 C25 -109.8(4) . . . . ? O2 La1 N7 C25 -163.4(4) . . . . ? O1 La1 N7 C25 -122.5(4) . . . . ? O4 La1 N7 C25 -68.4(4) . . . . ? O3 La1 N7 C25 150.4(3) . . . . ? O10 La1 N7 C25 -19.5(4) . . . . ? O14 La1 N7 C25 104.2(4) . . . . ? N3' La1 N7 C25 -137.3(15) . . . . ? N3 La1 N7 C25 -145(3) . . . . ? N2 La1 N7 C25 64.9(4) . . . . ? N6 La1 N7 C25 18.2(3) . . . . ? O1' La1 N7 C29 52.5(5) . . . . ? O2 La1 N7 C29 -1.2(3) . . . . ? O1 La1 N7 C29 39.8(4) . . . . ? O4 La1 N7 C29 93.8(4) . . . . ? O3 La1 N7 C29 -47.4(4) . . . . ? O10 La1 N7 C29 142.8(4) . . . . ? O14 La1 N7 C29 -93.6(4) . . . . ? N3' La1 N7 C29 24.9(16) . . . . ? N3 La1 N7 C29 18(4) . . . . ? N2 La1 N7 C29 -132.9(4) . . . . ? N6 La1 N7 C29 -179.6(4) . . . . ? C6 C1 C2 C3 1.6(8) . . . . ? C1 C2 C3 C4 -2.2(8) . . . . ? C2 C3 C4 C5 0.9(8) . . . . ? C3 C4 C5 C6 0.9(8) . . . . ? C3 C4 C5 C21 -178.9(5) . . . . ? C2 C1 C6 C5 0.3(8) . . . . ? C2 C1 C6 C7 -178.0(5) . . . . ? C4 C5 C6 C1 -1.5(7) . . . . ? C21 C5 C6 C1 178.3(5) . . . . ? C4 C5 C6 C7 176.7(4) . . . . ? C21 C5 C6 C7 -3.4(7) . . . . ? C8 N1 C7 C6 58.3(6) . . . . ? N2 N1 C7 C6 -119.0(5) . . . . ? C1 C6 C7 N1 -104.8(5) . . . . ? C5 C6 C7 N1 77.0(6) . . . . ? N2 N1 C8 C9 -0.3(6) . . . . ? C7 N1 C8 C9 -177.7(4) . . . . ? N1 C8 C9 C10 0.2(6) . . . . ? N1 N2 C10 C11 -168.4(6) . . . . ? La1 N2 C10 C11 21.2(8) . . . . ? N1 N2 C10 C9 -0.1(6) . . . . ? La1 N2 C10 C9 -170.6(4) . . . . ? N1 N2 C10 C11' 173.7(5) . . . . ? La1 N2 C10 C11' 3.2(7) . . . . ? C8 C9 C10 N2 0.0(6) . . . . ? C8 C9 C10 C11 168.2(6) . . . . ? C8 C9 C10 C11' -173.0(6) . . . . ? C22 N5 C21 C5 67.0(6) . . . . ? N6 N5 C21 C5 -108.1(5) . . . . ? C4 C5 C21 N5 -98.8(5) . . . . ? C6 C5 C21 N5 81.3(6) . . . . ? N6 N5 C22 C23 -0.2(6) . . . . ? C21 N5 C22 C23 -175.7(5) . . . . ? N5 C22 C23 C24 0.2(6) . . . . ? N5 N6 C24 C23 0.0(5) . . . . ? La1 N6 C24 C23 -163.1(3) . . . . ? N5 N6 C24 C25 179.3(4) . . . . ? La1 N6 C24 C25 16.1(6) . . . . ? C22 C23 C24 N6 -0.1(6) . . . . ? C22 C23 C24 C25 -179.3(5) . . . . ? C29 N7 C25 C26 -2.7(7) . . . . ? La1 N7 C25 C26 159.4(4) . . . . ? C29 N7 C25 C24 179.5(4) . . . . ? La1 N7 C25 C24 -18.3(6) . . . . ? N6 C24 C25 N7 0.5(7) . . . . ? C23 C24 C25 N7 179.7(5) . . . . ? N6 C24 C25 C26 -177.2(5) . . . . ? C23 C24 C25 C26 1.9(8) . . . . ? N7 C25 C26 C27 -0.7(8) . . . . ? C24 C25 C26 C27 176.9(5) . . . . ? C25 C26 C27 C28 2.4(9) . . . . ? C26 C27 C28 C29 -0.7(9) . . . . ? C25 N7 C29 C28 4.6(7) . . . . ? La1 N7 C29 C28 -158.4(4) . . . . ? C25 N7 C29 C30 177.3(4) . . . . ? La1 N7 C29 C30 14.3(6) . . . . ? C27 C28 C29 N7 -2.9(9) . . . . ? C27 C28 C29 C30 -174.8(5) . . . . ? La1 O2 C30 N8 -152.3(4) . . . . ? La1 O2 C30 C29 31.5(7) . . . . ? C33 N8 C30 O2 -3.9(9) . . . . ? C31 N8 C30 O2 160.1(7) . . . . ? C33 N8 C30 C29 172.1(5) . . . . ? C31 N8 C30 C29 -23.9(10) . . . . ? N7 C29 C30 O2 -28.5(7) . . . . ? C28 C29 C30 O2 144.0(6) . . . . ? N7 C29 C30 N8 155.3(5) . . . . ? C28 C29 C30 N8 -32.2(9) . . . . ? C30 N8 C31 C32 117.9(8) . . . . ? C33 N8 C31 C32 -77.7(9) . . . . ? C30 N8 C33 C34 88.3(8) . . . . ? C31 N8 C33 C34 -77.3(8) . . . . ? O13 Cl1 O10 La1 50.2(9) . . . . ? O12 Cl1 O10 La1 -73.1(9) . . . . ? O11 Cl1 O10 La1 168.9(6) . . . . ? O1' La1 O10 Cl1 -19.4(7) . . . . ? O2 La1 O10 Cl1 -62.1(8) . . . . ? O1 La1 O10 Cl1 -19.2(7) . . . . ? O4 La1 O10 Cl1 -87.5(7) . . . . ? O3 La1 O10 Cl1 56.5(7) . . . . ? O14 La1 O10 Cl1 146.2(6) . . . . ? N3' La1 O10 Cl1 36.9(7) . . . . ? N7 La1 O10 Cl1 -135.2(6) . . . . ? N3 La1 O10 Cl1 42.0(6) . . . . ? N2 La1 O10 Cl1 104.0(7) . . . . ? N6 La1 O10 Cl1 -169.6(7) . . . . ? O16 Cl2 O14 La1 -70.0(6) . . . . ? O17 Cl2 O14 La1 169.6(5) . . . . ? O15 Cl2 O14 La1 50.5(6) . . . . ? O1' La1 O14 Cl2 -3.3(8) . . . . ? O2 La1 O14 Cl2 40.1(5) . . . . ? O1 La1 O14 Cl2 3.4(6) . . . . ? O4 La1 O14 Cl2 110.2(5) . . . . ? O3 La1 O14 Cl2 -33.4(5) . . . . ? O10 La1 O14 Cl2 -154.7(5) . . . . ? N3' La1 O14 Cl2 -70.4(6) . . . . ? N7 La1 O14 Cl2 101.3(5) . . . . ? N3 La1 O14 Cl2 -75.4(5) . . . . ? N2 La1 O14 Cl2 -112.2(5) . . . . ? N6 La1 O14 Cl2 163.5(5) . . . . ? O1' La1 O1 C16 36.9(12) . . . . ? O2 La1 O1 C16 -167.6(9) . . . . ? O4 La1 O1 C16 102.5(9) . . . . ? O3 La1 O1 C16 -93.3(8) . . . . ? O10 La1 O1 C16 35.7(8) . . . . ? O14 La1 O1 C16 -127.4(8) . . . . ? N3' La1 O1 C16 -28.3(8) . . . . ? N7 La1 O1 C16 154.2(8) . . . . ? N3 La1 O1 C16 -27.2(8) . . . . ? N2 La1 O1 C16 -32.9(9) . . . . ? N6 La1 O1 C16 86.6(9) . . . . ? N2 C10 C11 C12 163.7(5) . . . . ? C9 C10 C11 C12 -3.1(10) . . . . ? C11' C10 C11 C12 -120(2) . . . . ? N2 C10 C11 N3 -22.4(8) . . . . ? C9 C10 C11 N3 170.8(5) . . . . ? C11' C10 C11 N3 53.9(17) . . . . ? C10 C11 C12 C13 173.5(7) . . . . ? N3 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 N3 0.0 . . . . ? C13 C14 C15 C16 169.9(8) . . . . ? C14 C15 N3 C11 0.0 . . . . ? C16 C15 N3 C11 -171.1(7) . . . . ? C14 C15 N3 La1 173.2(5) . . . . ? C16 C15 N3 La1 2.1(6) . . . . ? C10 C11 N3 C15 -174.4(6) . . . . ? C12 C11 N3 C15 0.0 . . . . ? C10 C11 N3 La1 13.0(6) . . . . ? C12 C11 N3 La1 -172.6(5) . . . . ? O1' La1 N3 C15 -3.1(4) . . . . ? O2 La1 N3 C15 51.0(4) . . . . ? O1 La1 N3 C15 10.1(3) . . . . ? O4 La1 N3 C15 -42.1(4) . . . . ? O3 La1 N3 C15 99.2(3) . . . . ? O10 La1 N3 C15 -93.5(3) . . . . ? O14 La1 N3 C15 142.6(3) . . . . ? N3' La1 N3 C15 21(4) . . . . ? N7 La1 N3 C15 33(4) . . . . ? N2 La1 N3 C15 -175.7(4) . . . . ? N6 La1 N3 C15 -129.4(3) . . . . ? O1' La1 N3 C11 169.8(5) . . . . ? O2 La1 N3 C11 -136.1(4) . . . . ? O1 La1 N3 C11 -177.1(5) . . . . ? O4 La1 N3 C11 130.8(4) . . . . ? O3 La1 N3 C11 -87.9(4) . . . . ? O10 La1 N3 C11 79.3(4) . . . . ? O14 La1 N3 C11 -44.5(4) . . . . ? N3' La1 N3 C11 -166(4) . . . . ? N7 La1 N3 C11 -154(3) . . . . ? N2 La1 N3 C11 -2.8(3) . . . . ? N6 La1 N3 C11 43.5(5) . . . . ? C16 N4 C17 C18 117.5(17) . . . . ? C19 N4 C17 C18 -78.4(18) . . . . ? C16 N4 C19 C20 -79.6(15) . . . . ? C17 N4 C19 C20 115.5(13) . . . . ? La1 O1 C16 N4 -142.4(9) . . . . ? La1 O1 C16 C15 38.8(12) . . . . ? C19 N4 C16 O1 0.7(17) . . . . ? C17 N4 C16 O1 164.0(13) . . . . ? C19 N4 C16 C15 179.4(9) . . . . ? C17 N4 C16 C15 -17.3(19) . . . . ? C14 C15 C16 O1 164.1(8) . . . . ? N3 C15 C16 O1 -25.4(11) . . . . ? C14 C15 C16 N4 -14.6(14) . . . . ? N3 C15 C16 N4 155.8(9) . . . . ? O2 La1 O1' C16' -103.7(10) . . . . ? O1 La1 O1' C16' -81.0(16) . . . . ? O4 La1 O1' C16' 169.4(11) . . . . ? O3 La1 O1' C16' -32.4(10) . . . . ? O10 La1 O1' C16' 97.9(10) . . . . ? O14 La1 O1' C16' -59.9(12) . . . . ? N3' La1 O1' C16' 26.2(9) . . . . ? N7 La1 O1' C16' -149.1(9) . . . . ? N3 La1 O1' C16' 28.8(9) . . . . ? N2 La1 O1' C16' 35.8(11) . . . . ? N6 La1 O1' C16' 138.3(9) . . . . ? N2 C10 C11' C12' -177.8(5) . . . . ? C11 C10 C11' C12' 69.1(17) . . . . ? C9 C10 C11' C12' -5.3(10) . . . . ? N2 C10 C11' N3' 6.9(8) . . . . ? C11 C10 C11' N3' -106.2(18) . . . . ? C9 C10 C11' N3' 179.4(6) . . . . ? N3' C11' C12' C13' 0.0 . . . . ? C10 C11' C12' C13' -175.3(7) . . . . ? C11' C12' C13' C14' 0.0 . . . . ? C12' C13' C14' C15' 0.0 . . . . ? C13' C14' C15' C16' -158.9(13) . . . . ? C13' C14' C15' N3' 0.0 . . . . ? C16' C15' N3' C11' 162.8(10) . . . . ? C14' C15' N3' C11' 0.0 . . . . ? C16' C15' N3' La1 -8.0(9) . . . . ? C14' C15' N3' La1 -170.8(6) . . . . ? C12' C11' N3' C15' 0.0 . . . . ? C10 C11' N3' C15' 175.4(7) . . . . ? C12' C11' N3' La1 170.8(6) . . . . ? C10 C11' N3' La1 -13.8(6) . . . . ? O1' La1 N3' C15' -8.3(4) . . . . ? O2 La1 N3' C15' 46.0(4) . . . . ? O1 La1 N3' C15' 5.7(4) . . . . ? O4 La1 N3' C15' -44.0(4) . . . . ? O3 La1 N3' C15' 98.0(4) . . . . ? O10 La1 N3' C15' -99.3(4) . . . . ? O14 La1 N3' C15' 136.5(4) . . . . ? N7 La1 N3' C15' 21.7(18) . . . . ? N3 La1 N3' C15' -163(4) . . . . ? N2 La1 N3' C15' -178.6(5) . . . . ? N6 La1 N3' C15' -131.2(4) . . . . ? O1' La1 N3' C11' -179.2(6) . . . . ? O2 La1 N3' C11' -124.8(4) . . . . ? O1 La1 N3' C11' -165.1(6) . . . . ? O4 La1 N3' C11' 145.2(4) . . . . ? O3 La1 N3' C11' -72.9(4) . . . . ? O10 La1 N3' C11' 89.8(4) . . . . ? O14 La1 N3' C11' -34.3(5) . . . . ? N7 La1 N3' C11' -149.2(13) . . . . ? N3 La1 N3' C11' 26(4) . . . . ? N2 La1 N3' C11' 10.5(4) . . . . ? N6 La1 N3' C11' 57.9(5) . . . . ? C16' N4' C17' C18' -118.8(16) . . . . ? C19' N4' C17' C18' 71.4(16) . . . . ? C16' N4' C19' C20' 77.2(17) . . . . ? C17' N4' C19' C20' -112.0(14) . . . . ? C14' C15' C16' O1' -168.0(9) . . . . ? N3' C15' C16' O1' 31.2(15) . . . . ? C14' C15' C16' N4' 16.9(19) . . . . ? N3' C15' C16' N4' -143.9(11) . . . . ? La1 O1' C16' C15' -46.7(18) . . . . ? La1 O1' C16' N4' 128.1(12) . . . . ? C17' N4' C16' C15' 9(2) . . . . ? C19' N4' C16' C15' 179.0(12) . . . . ? C17' N4' C16' O1' -165.6(13) . . . . ? C19' N4' C16' O1' 4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.646 _refine_diff_density_min -2.230 _refine_diff_density_rms 0.162 #===END data_imw699 _database_code_depnum_ccdc_archive 'CCDC 630968' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70.50 H83.50 Cl5 N17.50 O30 Yb2' _chemical_formula_weight 2179.38 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' Yb Yb -0.3850 5.5486 '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 21.4427(11) _cell_length_b 15.7294(7) _cell_length_c 28.4809(14) _cell_angle_alpha 90.00 _cell_angle_beta 104.093(2) _cell_angle_gamma 90.00 _cell_volume 9316.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9710 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 24.09 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4376 _exptl_absorpt_coefficient_mu 2.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6406 _exptl_absorpt_correction_T_max 0.8083 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 210751 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16413 _reflns_number_gt 12509 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0687P)^2^+120.3725P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16413 _refine_ls_number_parameters 1083 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1732 _refine_ls_wR_factor_gt 0.1626 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.004 _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 Yb1 Yb 0.231427(17) 0.38863(2) 0.099704(13) 0.02602(12) Uani 1 1 d . A . Yb2 Yb 0.188763(19) 0.60662(2) 0.284407(14) 0.02796(12) Uani 1 1 d . A . N1 N 0.3587(4) 0.7495(6) 0.2748(3) 0.053(3) Uani 1 1 d . A . N2 N 0.2995(4) 0.5493(5) 0.3035(3) 0.0344(18) Uani 1 1 d . . . N3 N 0.1986(4) 0.4425(5) 0.2992(3) 0.0319(18) Uani 1 1 d . . . N4 N 0.1595(4) 0.3740(5) 0.2995(3) 0.039(2) Uani 1 1 d . . . N5 N 0.0580(3) 0.4160(5) 0.0600(3) 0.0313(17) Uani 1 1 d . . . N6 N 0.1150(3) 0.3828(5) 0.0548(3) 0.0292(17) Uani 1 1 d . . . N7 N 0.2115(3) 0.3197(5) 0.0203(3) 0.0325(18) Uani 1 1 d . . . N8 N 0.3816(4) 0.3005(7) 0.0328(4) 0.057(3) Uani 1 1 d . A . N9 N 0.2208(6) 0.6093(7) 0.4406(3) 0.077(4) Uani 1 1 d D . . N10 N 0.1556(4) 0.7216(5) 0.3307(3) 0.0285(17) Uani 1 1 d . A . N11 N 0.1359(3) 0.7303(5) 0.2328(3) 0.0283(16) Uani 1 1 d . . . N12 N 0.1177(4) 0.7534(5) 0.1859(3) 0.0303(17) Uani 1 1 d . . . N13 N 0.3615(4) 0.5507(5) 0.1433(3) 0.0333(18) Uani 1 1 d . . . N14 N 0.3286(3) 0.4790(5) 0.1468(3) 0.0295(17) Uani 1 1 d . . . N15 N 0.2908(4) 0.3235(5) 0.1750(3) 0.0326(17) Uani 1 1 d . A . N16 N 0.1893(6) 0.1419(9) 0.1520(5) 0.088(4) Uiso 1 1 d D . . O1 O 0.2642(3) 0.7041(4) 0.2854(2) 0.0407(17) Uani 1 1 d . A . O2 O 0.3192(3) 0.3428(5) 0.0797(2) 0.0420(17) Uani 1 1 d . A . O3 O 0.2141(5) 0.5873(5) 0.3633(3) 0.074(3) Uani 1 1 d . . . O4 O 0.1961(3) 0.2604(4) 0.1141(2) 0.0370(15) Uani 1 1 d . . . O5 O 0.0806(3) 0.5833(4) 0.2716(2) 0.0331(15) Uani 1 1 d . . . O6 O 0.1853(3) 0.5505(4) 0.2119(2) 0.0297(14) Uani 1 1 d . . . O7 O 0.1930(3) 0.4653(4) 0.1518(2) 0.0286(13) Uani 1 1 d . . . C1 C 0.0675(4) 0.4073(6) 0.1916(4) 0.034(2) Uani 1 1 d . . . H1 H 0.0750 0.4644 0.1996 0.040 Uiso 1 1 calc R . . C2 C 0.0532(4) 0.3833(5) 0.1432(4) 0.031(2) Uani 1 1 d . . . C3 C 0.0385(6) 0.2989(6) 0.1320(4) 0.047(3) Uani 1 1 d . . . H3 H 0.0274 0.2820 0.0997 0.057 Uiso 1 1 calc R . . C4 C 0.0401(6) 0.2402(7) 0.1672(5) 0.058(3) Uani 1 1 d . . . H4 H 0.0300 0.1838 0.1591 0.069 Uiso 1 1 calc R . . C5 C 0.0567(5) 0.2648(6) 0.2155(4) 0.045(3) Uani 1 1 d . . . H5 H 0.0583 0.2243 0.2395 0.053 Uiso 1 1 calc R . . C6 C 0.0709(4) 0.3482(6) 0.2282(4) 0.034(2) Uani 1 1 d . . . C7 C 0.0902(4) 0.3739(6) 0.2799(4) 0.037(2) Uani 1 1 d . . . H7A H 0.0737 0.4305 0.2832 0.045 Uiso 1 1 calc R . . H7B H 0.0708 0.3353 0.2988 0.045 Uiso 1 1 calc R . . C8 C 0.1949(6) 0.3059(6) 0.3169(5) 0.053(3) Uani 1 1 d . . . H8 H 0.1790 0.2517 0.3198 0.063 Uiso 1 1 calc R . . C9 C 0.2578(6) 0.3290(8) 0.3294(5) 0.063(3) Uani 1 1 d . . . H9 H 0.2930 0.2950 0.3430 0.075 Uiso 1 1 calc R . . C10 C 0.2581(5) 0.4145(6) 0.3174(4) 0.037(2) Uani 1 1 d . . . C11 C 0.3126(5) 0.4713(7) 0.3214(4) 0.045(3) Uani 1 1 d . . . C12 C 0.3734(5) 0.4452(7) 0.3434(5) 0.059(3) Uani 1 1 d . . . H12 H 0.3814 0.3899 0.3549 0.070 Uiso 1 1 calc R . . C13 C 0.4230(6) 0.5040(8) 0.3480(6) 0.070(4) Uani 1 1 d . . . H13 H 0.4650 0.4889 0.3632 0.084 Uiso 1 1 calc R . . C14 C 0.4090(5) 0.5854(8) 0.3296(5) 0.057(3) Uani 1 1 d . . . H14 H 0.4415 0.6257 0.3328 0.068 Uiso 1 1 calc R . . C15 C 0.3479(5) 0.6057(7) 0.3072(4) 0.041(2) Uani 1 1 d . A . C16 C 0.3218(5) 0.6904(7) 0.2881(3) 0.041(2) Uani 1 1 d . . . C17 C 0.3271(6) 0.8357(9) 0.2661(6) 0.079(5) Uani 1 1 d . . . H17A H 0.2851 0.8292 0.2440 0.094 Uiso 1 1 calc R A . H17B H 0.3527 0.8717 0.2503 0.094 Uiso 1 1 calc R . . C18 C 0.3189(9) 0.8805(10) 0.3118(7) 0.094(5) Uani 1 1 d . A . H18A H 0.2866 0.8518 0.3239 0.140 Uiso 1 1 calc R . . H18B H 0.3060 0.9384 0.3042 0.140 Uiso 1 1 calc R . . H18C H 0.3589 0.8796 0.3359 0.140 Uiso 1 1 calc R . . C19 C 0.4225(7) 0.7397(10) 0.2662(5) 0.074(4) Uani 1 1 d . . . H19A H 0.4227 0.7629 0.2347 0.088 Uiso 1 1 calc R A . H19B H 0.4330 0.6797 0.2661 0.088 Uiso 1 1 calc R . . C20 C 0.4730(6) 0.7848(9) 0.3050(5) 0.074(4) Uani 1 1 d . A . H20A H 0.4612 0.8434 0.3065 0.111 Uiso 1 1 calc R . . H20B H 0.5140 0.7812 0.2971 0.111 Uiso 1 1 calc R . . H20C H 0.4757 0.7583 0.3357 0.111 Uiso 1 1 calc R . . C21 C 0.0506(5) 0.4511(6) 0.1048(3) 0.034(2) Uani 1 1 d . . . H21A H 0.0097 0.4806 0.0991 0.041 Uiso 1 1 calc R . . H21B H 0.0844 0.4924 0.1165 0.041 Uiso 1 1 calc R . . C22 C 0.0109(5) 0.3995(6) 0.0204(4) 0.040(2) Uani 1 1 d . . . H22 H -0.0318 0.4164 0.0155 0.048 Uiso 1 1 calc R . . C23 C 0.0358(5) 0.3542(7) -0.0113(4) 0.041(2) Uani 1 1 d . . . H23 H 0.0143 0.3331 -0.0414 0.049 Uiso 1 1 calc R . . C24 C 0.0998(5) 0.3466(6) 0.0111(3) 0.035(2) Uani 1 1 d . . . C25 C 0.1517(5) 0.3036(6) -0.0055(3) 0.036(2) Uani 1 1 d . . . C26 C 0.1387(5) 0.2488(8) -0.0450(4) 0.053(3) Uani 1 1 d . . . H26 H 0.0970 0.2407 -0.0635 0.064 Uiso 1 1 calc R . . C27 C 0.1907(6) 0.2064(9) -0.0558(5) 0.068(4) Uani 1 1 d . . . H27 H 0.1838 0.1670 -0.0809 0.082 Uiso 1 1 calc R . . C28 C 0.2509(6) 0.2227(9) -0.0297(5) 0.069(4) Uani 1 1 d . . . H28 H 0.2855 0.1950 -0.0372 0.082 Uiso 1 1 calc R . . C29 C 0.2615(5) 0.2805(7) 0.0083(4) 0.040(2) Uani 1 1 d . A . C30 C 0.3238(5) 0.3076(7) 0.0422(4) 0.042(3) Uani 1 1 d . . . C31 C 0.4355(6) 0.3266(13) 0.0701(6) 0.097(6) Uani 1 1 d . . . H31A H 0.4732 0.2956 0.0667 0.116 Uiso 1 1 calc R A . H31B H 0.4277 0.3119 0.1012 0.116 Uiso 1 1 calc R . . C32 C 0.4486(8) 0.4193(15) 0.0691(10) 0.156(12) Uani 1 1 d . A . H32A H 0.4582 0.4338 0.0389 0.234 Uiso 1 1 calc R . . H32B H 0.4846 0.4334 0.0953 0.234 Uiso 1 1 calc R . . H32C H 0.4114 0.4504 0.0725 0.234 Uiso 1 1 calc R . . C33 C 0.3955(7) 0.2741(10) -0.0130(5) 0.071(4) Uani 1 1 d . . . H33A H 0.4281 0.3108 -0.0204 0.086 Uiso 1 1 calc R A . H33B H 0.3569 0.2790 -0.0390 0.086 Uiso 1 1 calc R . . C34 C 0.4197(7) 0.1797(11) -0.0089(6) 0.097(6) Uani 1 1 d . A . H34A H 0.4561 0.1742 0.0182 0.145 Uiso 1 1 calc R . . H34B H 0.4318 0.1641 -0.0380 0.145 Uiso 1 1 calc R . . H34C H 0.3858 0.1429 -0.0045 0.145 Uiso 1 1 calc R . . C35 C 0.2414(4) 0.6664(6) 0.1310(3) 0.031(2) Uani 1 1 d . . . H35 H 0.2278 0.6101 0.1298 0.037 Uiso 1 1 calc R . . C36 C 0.3003(4) 0.6843(6) 0.1210(3) 0.032(2) Uani 1 1 d . . . C37 C 0.3217(5) 0.7669(6) 0.1239(4) 0.047(3) Uani 1 1 d . . . H37 H 0.3610 0.7803 0.1173 0.056 Uiso 1 1 calc R . . C38 C 0.2827(5) 0.8318(7) 0.1371(5) 0.063(4) Uani 1 1 d . . . H38 H 0.2975 0.8876 0.1408 0.076 Uiso 1 1 calc R . . C39 C 0.2243(5) 0.8122(6) 0.1442(4) 0.046(3) Uani 1 1 d . . . H39 H 0.1980 0.8556 0.1506 0.056 Uiso 1 1 calc R . . C40 C 0.2025(5) 0.7279(6) 0.1423(3) 0.031(2) Uani 1 1 d . . . C41 C 0.1363(4) 0.7063(6) 0.1476(3) 0.031(2) Uani 1 1 d . . . H41A H 0.1055 0.7177 0.1172 0.038 Uiso 1 1 calc R . . H41B H 0.1346 0.6459 0.1542 0.038 Uiso 1 1 calc R . . C42 C 0.0850(5) 0.8284(6) 0.1804(4) 0.040(2) Uani 1 1 d . . . H42 H 0.0674 0.8557 0.1512 0.048 Uiso 1 1 calc R . . C43 C 0.0825(4) 0.8559(6) 0.2247(4) 0.036(2) Uani 1 1 d . . . H43 H 0.0633 0.9053 0.2325 0.043 Uiso 1 1 calc R . . C44 C 0.1150(4) 0.7938(5) 0.2565(3) 0.029(2) Uani 1 1 d . . . C45 C 0.1257(4) 0.7905(6) 0.3091(3) 0.033(2) Uani 1 1 d . . . C46 C 0.1079(5) 0.8552(7) 0.3359(4) 0.041(2) Uani 1 1 d . . . H46 H 0.0872 0.9032 0.3205 0.050 Uiso 1 1 calc R . . C47 C 0.1205(6) 0.8485(7) 0.3842(4) 0.051(3) Uani 1 1 d . . . H47 H 0.1092 0.8925 0.4023 0.061 Uiso 1 1 calc R . . C48 C 0.1500(5) 0.7771(7) 0.4070(4) 0.043(3) Uani 1 1 d . A . H48 H 0.1574 0.7709 0.4404 0.052 Uiso 1 1 calc R . . C49 C 0.1683(4) 0.7156(6) 0.3794(4) 0.035(2) Uani 1 1 d . . . C50 C 0.2018(6) 0.6336(6) 0.3957(4) 0.045(3) Uani 1 1 d . A . C51 C 0.2519(9) 0.5215(13) 0.4496(7) 0.110(6) Uiso 1 1 d . A . H51A H 0.2450 0.4973 0.4793 0.132 Uiso 1 1 calc R . . H51B H 0.2333 0.4835 0.4231 0.132 Uiso 1 1 calc R . . C52 C 0.3185(10) 0.5322(14) 0.4533(8) 0.122(7) Uiso 1 1 d . . . H52A H 0.3247 0.5527 0.4230 0.183 Uiso 1 1 calc R A . H52B H 0.3401 0.4787 0.4609 0.183 Uiso 1 1 calc R . . H52C H 0.3357 0.5726 0.4784 0.183 Uiso 1 1 calc R . . C54 C 0.1734(9) 0.6567(13) 0.5085(7) 0.060(4) Uiso 0.632(15) 1 d PDU A 1 H54A H 0.1348 0.6772 0.4868 0.090 Uiso 0.632(15) 1 calc PR A 1 H54B H 0.1809 0.6877 0.5384 0.090 Uiso 0.632(15) 1 calc PR A 1 H54C H 0.1687 0.5973 0.5147 0.090 Uiso 0.632(15) 1 calc PR A 1 C53 C 0.2289(9) 0.6690(13) 0.4861(7) 0.058(4) Uiso 0.632(15) 1 d PDU A 1 H53A H 0.2688 0.6556 0.5095 0.069 Uiso 0.632(15) 1 calc PR A 1 H53B H 0.2308 0.7279 0.4763 0.069 Uiso 0.632(15) 1 calc PR A 1 C54' C 0.2240(16) 0.657(2) 0.5212(11) 0.058(4) Uiso 0.368(15) 1 d PDU A 2 H54D H 0.2508 0.6114 0.5373 0.087 Uiso 0.368(15) 1 calc PR A 2 H54E H 0.2007 0.6809 0.5428 0.087 Uiso 0.368(15) 1 calc PR A 2 H54F H 0.2504 0.6999 0.5119 0.087 Uiso 0.368(15) 1 calc PR A 2 C53' C 0.1778(13) 0.623(2) 0.4774(10) 0.058(4) Uiso 0.368(15) 1 d PDU A 2 H53C H 0.1438 0.6640 0.4649 0.069 Uiso 0.368(15) 1 calc PR A 2 H53D H 0.1588 0.5703 0.4843 0.069 Uiso 0.368(15) 1 calc PR A 2 C55 C 0.3390(5) 0.6141(6) 0.1050(4) 0.037(2) Uani 1 1 d . . . H55A H 0.3127 0.5861 0.0767 0.045 Uiso 1 1 calc R . . H55B H 0.3758 0.6388 0.0959 0.045 Uiso 1 1 calc R . . C56 C 0.4146(5) 0.5570(7) 0.1789(4) 0.044(3) Uani 1 1 d . . . H56 H 0.4440 0.6015 0.1835 0.053 Uiso 1 1 calc R . . C57 C 0.4184(5) 0.4880(7) 0.2070(4) 0.045(3) Uani 1 1 d . . . H57 H 0.4506 0.4745 0.2343 0.053 Uiso 1 1 calc R . . C58 C 0.3640(4) 0.4412(6) 0.1866(3) 0.033(2) Uani 1 1 d . . . C59 C 0.3437(4) 0.3592(6) 0.2030(3) 0.033(2) Uani 1 1 d . . . C60 C 0.3785(6) 0.3208(7) 0.2441(4) 0.050(3) Uani 1 1 d . . . H60 H 0.4161 0.3453 0.2624 0.060 Uiso 1 1 calc R . . C61 C 0.3567(8) 0.2454(10) 0.2575(6) 0.088(5) Uani 1 1 d . . . H61 H 0.3779 0.2194 0.2863 0.106 Uiso 1 1 calc R . . C62 C 0.3034(7) 0.2081(8) 0.2285(5) 0.066(4) Uani 1 1 d . B . H62 H 0.2895 0.1554 0.2368 0.079 Uiso 1 1 calc R . . C63 C 0.2707(5) 0.2480(6) 0.1876(4) 0.034(2) Uani 1 1 d . . . C64 C 0.2162(5) 0.2146(6) 0.1501(4) 0.043(3) Uani 1 1 d . A . C65 C 0.2205(12) 0.0591(15) 0.1772(8) 0.068(4) Uiso 0.552(17) 1 d PDU B 1 H65A H 0.2664 0.0654 0.1910 0.082 Uiso 0.552(17) 1 calc PR B 1 H65B H 0.2126 0.0104 0.1557 0.082 Uiso 0.552(17) 1 calc PR B 1 C66 C 0.1802(13) 0.055(2) 0.2182(9) 0.072(5) Uiso 0.552(17) 1 d PDU B 1 H66A H 0.1825 0.1089 0.2342 0.108 Uiso 0.552(17) 1 calc PR B 1 H66B H 0.1980 0.0117 0.2414 0.108 Uiso 0.552(17) 1 calc PR B 1 H66C H 0.1361 0.0415 0.2033 0.108 Uiso 0.552(17) 1 calc PR B 1 C65' C 0.1786(15) 0.1199(18) 0.2050(9) 0.069(4) Uiso 0.448(17) 1 d PDU B 2 H65C H 0.2039 0.1578 0.2292 0.083 Uiso 0.448(17) 1 calc PR B 2 H65D H 0.1337 0.1260 0.2052 0.083 Uiso 0.448(17) 1 calc PR B 2 C66' C 0.2017(17) 0.0225(18) 0.2163(12) 0.068(5) Uiso 0.448(17) 1 d PDU B 2 H66D H 0.1785 -0.0136 0.1908 0.102 Uiso 0.448(17) 1 calc PR B 2 H66E H 0.1933 0.0051 0.2465 0.102 Uiso 0.448(17) 1 calc PR B 2 H66F H 0.2469 0.0183 0.2183 0.102 Uiso 0.448(17) 1 calc PR B 2 C67 C 0.1393(8) 0.1128(11) 0.1088(6) 0.087(5) Uiso 1 1 d . B . H67A H 0.1128 0.0693 0.1184 0.105 Uiso 1 1 calc R . . H67B H 0.1117 0.1602 0.0953 0.105 Uiso 1 1 calc R . . C68 C 0.1702(11) 0.0781(15) 0.0717(8) 0.134(8) Uiso 1 1 d . . . H68A H 0.2038 0.1158 0.0679 0.201 Uiso 1 1 calc R B . H68B H 0.1387 0.0729 0.0415 0.201 Uiso 1 1 calc R . . H68C H 0.1880 0.0232 0.0818 0.201 Uiso 1 1 calc R . . C100 C 0.2075(4) 0.4863(6) 0.1945(4) 0.031(2) Uani 1 1 d . A . H100 H 0.2371 0.4525 0.2158 0.037 Uiso 1 1 calc R . . Cl1 Cl 0.17801(14) 0.56179(17) 0.01853(10) 0.0522(7) Uani 1 1 d . A . O10 O 0.2220(3) 0.5052(4) 0.0511(2) 0.0366(15) Uani 1 1 d . . . O11 O 0.1320(4) 0.5932(6) 0.0450(4) 0.082(3) Uani 1 1 d . . . O12 O 0.2159(5) 0.6281(6) 0.0064(4) 0.091(4) Uani 1 1 d . . . O13 O 0.1447(4) 0.5156(5) -0.0227(3) 0.062(2) Uani 1 1 d . . . Cl2 Cl 0.49034(14) 0.2517(2) 0.38059(14) 0.0652(9) Uani 1 1 d D . . O14 O 0.5163(10) 0.3233(15) 0.4120(11) 0.086(5) Uiso 0.52(4) 1 d PDU C 1 O14' O 0.5100(12) 0.3401(11) 0.3880(13) 0.082(6) Uiso 0.48(4) 1 d PDU C 2 O15 O 0.4221(4) 0.2475(6) 0.3764(3) 0.067(2) Uani 1 1 d . C . O16 O 0.5204(5) 0.1893(10) 0.4150(4) 0.111(4) Uani 1 1 d . C . O17 O 0.5046(5) 0.2353(8) 0.3357(4) 0.087(3) Uani 1 1 d . C . Cl3 Cl 0.94587(12) 0.60803(17) 0.16790(10) 0.0466(6) Uani 1 1 d . . . O22 O 0.9080(6) 0.6804(7) 0.1584(4) 0.114(5) Uani 1 1 d . . . O23 O 0.9299(5) 0.5665(7) 0.2088(4) 0.094(4) Uani 1 1 d . . . O24 O 1.0120(4) 0.6246(7) 0.1803(4) 0.082(3) Uani 1 1 d . . . O25 O 0.9299(4) 0.5550(6) 0.1277(3) 0.068(3) Uani 1 1 d . . . Cl4 Cl 0.04241(16) 0.50529(19) 0.38229(10) 0.0548(7) Uani 1 1 d D . . O18 O 0.0083(4) 0.5239(5) 0.3343(3) 0.062(2) Uani 1 1 d . D . O19 O 0.0887(8) 0.4420(10) 0.3857(7) 0.081(4) Uiso 0.50 1 d PDU D 1 O20 O -0.0110(7) 0.4749(10) 0.4017(6) 0.071(4) Uiso 0.50 1 d PDU D 1 O21 O 0.0651(8) 0.5831(9) 0.4048(7) 0.077(5) Uiso 0.50 1 d PDU D 1 O19' O 0.0393(10) 0.4197(9) 0.3971(7) 0.084(4) Uiso 0.50 1 d PDU D 2 O20' O 0.0403(10) 0.5603(12) 0.4201(7) 0.095(5) Uiso 0.50 1 d PDU D 2 O21' O 0.1086(8) 0.5113(13) 0.3765(8) 0.101(5) Uiso 0.50 1 d PDU D 2 Cl5 Cl 0.6308(3) 0.5861(4) 0.3867(2) 0.0717(17) Uiso 0.616(6) 1 d PD E 1 O26 O 0.6392(12) 0.5423(15) 0.3443(7) 0.136(7) Uiso 0.616(6) 1 d PDU E 1 O27 O 0.6612(12) 0.5453(16) 0.4299(7) 0.144(9) Uiso 0.616(6) 1 d PD E 1 O28 O 0.6662(8) 0.6622(10) 0.3888(7) 0.097(6) Uiso 0.616(6) 1 d PD E 1 O29 O 0.5666(7) 0.6085(11) 0.3869(6) 0.088(5) Uiso 0.616(6) 1 d PD E 1 Cl5' Cl 0.5806(4) 0.5236(5) 0.2792(3) 0.058(2) Uiso 0.384(6) 1 d PD E 2 O26' O 0.6447(11) 0.532(2) 0.3094(12) 0.122(8) Uiso 0.384(6) 1 d PDU E 2 O27' O 0.5908(11) 0.5326(15) 0.2304(6) 0.070(7) Uiso 0.384(6) 1 d PD E 2 O28' O 0.5411(10) 0.5952(12) 0.2844(8) 0.062(6) Uiso 0.384(6) 1 d PD E 2 O29' O 0.5520(7) 0.4390(9) 0.2916(5) 0.030(4) Uiso 0.384(6) 1 d PD E 2 C1S C 0.3808(14) 0.807(2) 0.4824(11) 0.194(12) Uiso 1 1 d . . . H1S1 H 0.3405 0.8183 0.4902 0.291 Uiso 1 1 calc R . . H1S2 H 0.4052 0.8591 0.4850 0.291 Uiso 1 1 calc R . . H1S3 H 0.4045 0.7659 0.5044 0.291 Uiso 1 1 calc R . . N1S N 0.3696(11) 0.7762(13) 0.4347(8) 0.137(7) Uiso 1 1 d . . . O1S O 0.4117(10) 0.7590(13) 0.4153(7) 0.178(7) Uiso 1 1 d . . . O2S O 0.3210(9) 0.7406(11) 0.4142(6) 0.145(5) Uiso 1 1 d . . . N2S N 0.9606(9) 0.3742(13) 0.4586(7) 0.053(5) Uiso 0.50 1 d PD . . O4S O 0.9635(9) 0.3101(13) 0.4418(7) 0.079(5) Uiso 0.50 1 d PD . . O3S O 0.9230(11) 0.4225(18) 0.4418(9) 0.117(8) Uiso 0.50 1 d PD . . C2S C 1.0073(16) 0.3934(18) 0.4999(12) 0.092(10) Uiso 0.50 1 d PD . . H2S1 H 0.9996 0.3617 0.5268 0.138 Uiso 0.50 1 calc PR . . H2S2 H 1.0061 0.4532 0.5066 0.138 Uiso 0.50 1 calc PR . . H2S3 H 1.0488 0.3788 0.4952 0.138 Uiso 0.50 1 calc PR . . 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 Yb1 0.0259(2) 0.0226(2) 0.0312(2) -0.00422(16) 0.01000(16) 0.00198(16) Yb2 0.0356(2) 0.0210(2) 0.0318(2) -0.00342(16) 0.01689(17) -0.00044(17) N1 0.038(5) 0.058(6) 0.057(6) 0.012(5) -0.003(4) -0.022(5) N2 0.034(4) 0.033(4) 0.042(5) -0.006(4) 0.019(4) -0.007(4) N3 0.033(4) 0.020(4) 0.049(5) -0.002(3) 0.024(4) -0.007(3) N4 0.048(5) 0.027(4) 0.049(5) 0.005(4) 0.024(4) -0.002(4) N5 0.023(4) 0.029(4) 0.044(5) 0.002(3) 0.013(3) 0.000(3) N6 0.020(4) 0.024(4) 0.044(5) -0.004(3) 0.010(3) 0.004(3) N7 0.024(4) 0.037(5) 0.038(4) -0.008(4) 0.010(3) 0.003(3) N8 0.034(5) 0.081(7) 0.059(6) -0.014(5) 0.019(4) 0.018(5) N9 0.138(11) 0.067(7) 0.035(5) 0.010(5) 0.043(6) 0.049(7) N10 0.037(4) 0.024(4) 0.030(4) -0.006(3) 0.017(3) 0.001(3) N11 0.032(4) 0.024(4) 0.030(4) -0.005(3) 0.008(3) -0.004(3) N12 0.033(4) 0.024(4) 0.038(4) -0.001(3) 0.018(4) -0.006(3) N13 0.028(4) 0.027(4) 0.045(5) -0.001(4) 0.010(4) -0.007(3) N14 0.029(4) 0.023(4) 0.039(4) -0.002(3) 0.015(3) 0.002(3) N15 0.035(4) 0.023(4) 0.041(4) 0.001(3) 0.012(4) 0.006(3) O1 0.035(4) 0.035(4) 0.049(4) 0.002(3) 0.003(3) -0.013(3) O2 0.031(4) 0.058(5) 0.038(4) -0.019(3) 0.011(3) 0.010(3) O3 0.162(10) 0.026(4) 0.035(4) 0.003(3) 0.027(5) 0.029(5) O4 0.042(4) 0.027(4) 0.045(4) -0.004(3) 0.015(3) -0.005(3) O5 0.031(3) 0.028(3) 0.044(4) 0.000(3) 0.018(3) -0.001(3) O6 0.037(4) 0.022(3) 0.034(3) -0.004(3) 0.016(3) -0.004(3) O7 0.036(3) 0.022(3) 0.031(3) -0.004(3) 0.014(3) -0.002(3) C1 0.031(5) 0.022(5) 0.053(6) -0.002(4) 0.020(4) -0.002(4) C2 0.030(5) 0.019(4) 0.052(6) -0.002(4) 0.024(4) 0.000(4) C3 0.064(7) 0.025(5) 0.057(7) -0.004(5) 0.020(6) 0.002(5) C4 0.076(9) 0.023(6) 0.074(9) -0.001(5) 0.018(7) -0.007(5) C5 0.058(7) 0.025(5) 0.054(7) 0.008(5) 0.020(5) -0.005(5) C6 0.029(5) 0.029(5) 0.050(6) 0.003(4) 0.021(4) -0.003(4) C7 0.032(5) 0.023(5) 0.063(7) 0.006(4) 0.021(5) -0.004(4) C8 0.060(7) 0.020(5) 0.079(8) 0.011(5) 0.018(6) 0.003(5) C9 0.049(7) 0.039(7) 0.098(10) 0.002(7) 0.015(7) 0.001(6) C10 0.035(5) 0.018(5) 0.064(7) 0.001(4) 0.021(5) 0.001(4) C11 0.043(6) 0.032(6) 0.060(7) -0.013(5) 0.012(5) 0.005(5) C12 0.039(6) 0.039(6) 0.101(10) -0.001(6) 0.022(6) 0.021(5) C13 0.032(6) 0.048(8) 0.125(12) -0.018(8) 0.008(7) 0.009(6) C14 0.035(6) 0.049(7) 0.094(10) -0.018(6) 0.029(6) -0.009(5) C15 0.031(5) 0.045(6) 0.050(6) -0.016(5) 0.013(5) 0.003(5) C16 0.051(7) 0.042(6) 0.030(5) -0.003(4) 0.008(5) -0.013(5) C17 0.043(7) 0.073(10) 0.104(11) 0.058(9) -0.013(7) -0.020(7) C18 0.102(13) 0.057(9) 0.110(14) -0.009(9) 0.003(11) 0.014(9) C19 0.079(10) 0.094(11) 0.057(8) -0.014(7) 0.036(7) -0.027(8) C20 0.050(8) 0.075(10) 0.101(11) -0.002(8) 0.025(7) -0.028(7) C21 0.033(5) 0.026(5) 0.048(6) -0.003(4) 0.020(4) 0.004(4) C22 0.022(5) 0.042(6) 0.055(6) 0.007(5) 0.004(4) -0.005(4) C23 0.028(5) 0.048(6) 0.041(6) -0.005(5) -0.004(4) -0.001(5) C24 0.035(5) 0.035(5) 0.037(5) 0.001(4) 0.013(4) 0.001(4) C25 0.033(5) 0.040(6) 0.035(5) -0.006(4) 0.005(4) 0.008(4) C26 0.044(6) 0.073(8) 0.038(6) -0.021(6) 0.001(5) 0.004(6) C27 0.058(8) 0.083(10) 0.062(8) -0.043(7) 0.014(6) 0.006(7) C28 0.054(8) 0.084(10) 0.072(9) -0.046(8) 0.023(7) -0.001(7) C29 0.040(6) 0.044(6) 0.040(6) -0.010(5) 0.014(5) 0.007(5) C30 0.029(5) 0.045(6) 0.055(7) -0.008(5) 0.013(5) 0.015(5) C31 0.027(6) 0.175(19) 0.085(10) -0.050(12) 0.008(7) 0.029(9) C32 0.046(9) 0.17(2) 0.25(3) -0.14(2) 0.031(13) -0.031(12) C33 0.066(8) 0.095(11) 0.069(9) -0.006(8) 0.048(7) 0.015(8) C34 0.073(10) 0.123(14) 0.109(13) -0.044(11) 0.052(9) 0.021(10) C35 0.035(5) 0.026(5) 0.033(5) -0.007(4) 0.011(4) -0.011(4) C36 0.034(5) 0.025(5) 0.038(5) 0.002(4) 0.013(4) -0.005(4) C37 0.041(6) 0.029(6) 0.075(8) 0.001(5) 0.024(6) -0.007(5) C38 0.047(7) 0.024(6) 0.123(11) -0.015(6) 0.029(7) -0.023(5) C39 0.043(6) 0.026(5) 0.079(8) -0.002(5) 0.032(6) -0.001(4) C40 0.041(5) 0.022(5) 0.031(5) -0.001(4) 0.012(4) -0.004(4) C41 0.036(5) 0.025(5) 0.035(5) 0.000(4) 0.014(4) -0.002(4) C42 0.035(5) 0.036(6) 0.050(6) 0.004(5) 0.013(5) 0.012(5) C43 0.033(5) 0.027(5) 0.051(6) 0.000(4) 0.015(5) 0.006(4) C44 0.034(5) 0.017(4) 0.041(5) -0.004(4) 0.019(4) 0.000(4) C45 0.032(5) 0.030(5) 0.042(5) -0.009(4) 0.017(4) -0.007(4) C46 0.039(6) 0.039(6) 0.049(6) -0.009(5) 0.017(5) 0.007(5) C47 0.061(7) 0.048(7) 0.051(7) -0.019(5) 0.027(6) 0.004(6) C48 0.058(7) 0.046(6) 0.030(5) -0.014(5) 0.018(5) -0.010(5) C49 0.031(5) 0.039(6) 0.040(6) -0.005(4) 0.018(4) -0.008(4) C50 0.075(8) 0.031(5) 0.037(6) 0.005(4) 0.027(5) 0.005(5) C55 0.035(5) 0.036(5) 0.046(6) -0.004(5) 0.019(4) -0.009(4) C56 0.030(5) 0.045(6) 0.056(7) 0.000(5) 0.009(5) -0.013(5) C57 0.030(5) 0.046(6) 0.049(6) 0.007(5) -0.006(5) 0.000(5) C58 0.031(5) 0.028(5) 0.042(5) -0.006(4) 0.011(4) 0.009(4) C59 0.029(5) 0.030(5) 0.042(5) -0.004(4) 0.011(4) 0.008(4) C60 0.051(7) 0.044(7) 0.051(7) 0.008(5) 0.004(5) 0.006(5) C61 0.103(12) 0.069(10) 0.077(10) 0.033(8) -0.010(9) -0.010(9) C62 0.093(10) 0.043(7) 0.057(8) 0.015(6) 0.010(7) -0.016(7) C63 0.035(5) 0.028(5) 0.044(6) 0.007(4) 0.021(4) 0.003(4) C64 0.041(6) 0.012(4) 0.078(8) 0.009(5) 0.019(5) -0.001(4) C100 0.024(5) 0.027(5) 0.045(6) -0.002(4) 0.016(4) 0.003(4) Cl1 0.0558(17) 0.0371(14) 0.0520(16) 0.0100(12) -0.0094(13) -0.0056(13) O10 0.036(4) 0.035(4) 0.038(4) 0.010(3) 0.009(3) 0.002(3) O11 0.056(6) 0.073(6) 0.103(8) -0.029(6) -0.008(5) 0.029(5) O12 0.098(8) 0.069(6) 0.081(7) 0.043(5) -0.024(6) -0.039(6) O13 0.081(6) 0.058(5) 0.037(4) 0.003(4) -0.002(4) -0.017(5) Cl2 0.0358(15) 0.061(2) 0.097(3) -0.0120(18) 0.0115(16) 0.0116(14) O15 0.038(4) 0.069(6) 0.095(7) -0.003(5) 0.019(4) 0.012(4) O16 0.051(6) 0.175(13) 0.104(9) 0.029(8) 0.013(6) 0.033(7) O17 0.062(6) 0.119(9) 0.086(7) 0.006(6) 0.030(5) 0.019(6) Cl3 0.0377(13) 0.0434(15) 0.0569(16) -0.0170(13) 0.0078(12) 0.0089(12) O22 0.132(10) 0.092(8) 0.097(8) -0.033(6) -0.013(7) 0.082(8) O23 0.109(8) 0.106(8) 0.085(7) -0.026(6) 0.058(7) -0.043(7) O24 0.061(6) 0.090(7) 0.084(7) 0.028(6) -0.003(5) -0.027(5) O25 0.043(5) 0.095(7) 0.070(6) -0.037(5) 0.022(4) -0.006(5) Cl4 0.073(2) 0.0483(16) 0.0478(16) -0.0012(13) 0.0240(14) -0.0105(14) O18 0.071(6) 0.061(5) 0.062(5) 0.003(4) 0.029(5) 0.007(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 Yb1 O2 2.216(6) . ? Yb1 O7 2.221(6) . ? Yb1 O4 2.228(6) . ? Yb1 O10 2.276(6) . ? Yb1 N15 2.437(8) . ? Yb1 N7 2.451(7) . ? Yb1 N6 2.513(7) . ? Yb1 N14 2.608(7) . ? Yb1 C30 3.133(9) . ? Yb1 C64 3.144(9) . ? Yb2 O3 2.200(7) . ? Yb2 O1 2.224(6) . ? Yb2 O6 2.229(6) . ? Yb2 O5 2.287(6) . ? Yb2 N10 2.444(7) . ? Yb2 N2 2.474(8) . ? Yb2 N11 2.533(7) . ? Yb2 N3 2.617(7) . ? Yb2 C16 3.121(11) . ? Yb2 C50 3.143(10) . ? N1 C16 1.333(13) . ? N1 C19 1.457(16) . ? N1 C17 1.509(17) . ? N2 C11 1.331(13) . ? N2 C15 1.349(13) . ? N3 C10 1.328(12) . ? N3 N4 1.366(10) . ? N4 C8 1.336(13) . ? N4 C7 1.455(12) . ? N5 C22 1.345(12) . ? N5 N6 1.370(10) . ? N5 C21 1.433(12) . ? N6 C24 1.335(12) . ? N7 C25 1.339(12) . ? N7 C29 1.351(12) . ? N8 C30 1.335(13) . ? N8 C31 1.425(16) . ? N8 C33 1.465(14) . ? N9 C50 1.301(14) . ? N9 C51 1.53(2) . ? N9 C53' 1.57(2) . ? N9 C53 1.574(19) . ? N10 C45 1.332(12) . ? N10 C49 1.350(12) . ? N11 C44 1.343(11) . ? N11 N12 1.346(10) . ? N12 C42 1.363(12) . ? N12 C41 1.452(11) . ? N13 C56 1.332(12) . ? N13 N14 1.346(10) . ? N13 C55 1.468(12) . ? N14 C58 1.340(12) . ? N15 C59 1.340(12) . ? N15 C63 1.342(12) . ? N16 C64 1.288(16) . ? N16 C67 1.495(19) . ? N16 C65 1.56(2) . ? N16 C65' 1.62(2) . ? O1 C16 1.239(12) . ? O2 C30 1.229(12) . ? O3 C50 1.254(12) . ? O4 C64 1.240(12) . ? O6 C100 1.268(10) . ? O7 C100 1.225(11) . ? C1 C6 1.384(13) . ? C1 C2 1.390(14) . ? C1 H1 0.9300 . ? C2 C3 1.383(13) . ? C2 C21 1.519(13) . ? C3 C4 1.358(15) . ? C3 H3 0.9300 . ? C4 C5 1.388(16) . ? C4 H4 0.9300 . ? C5 C6 1.376(14) . ? C5 H5 0.9300 . ? C6 C7 1.487(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.358(16) . ? C8 H8 0.9300 . ? C9 C10 1.388(15) . ? C9 H9 0.9300 . ? C10 C11 1.454(14) . ? C11 C12 1.366(15) . ? C12 C13 1.391(17) . ? C12 H12 0.9300 . ? C13 C14 1.388(18) . ? C13 H13 0.9300 . ? C14 C15 1.349(15) . ? C14 H14 0.9300 . ? C15 C16 1.496(15) . ? C17 C18 1.53(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.521(18) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.358(15) . ? C22 H22 0.9300 . ? C23 C24 1.371(13) . ? C23 H23 0.9300 . ? C24 C25 1.475(13) . ? C25 C26 1.389(14) . ? C26 C27 1.397(16) . ? C26 H26 0.9300 . ? C27 C28 1.347(17) . ? C27 H27 0.9300 . ? C28 C29 1.389(15) . ? C28 H28 0.9300 . ? C29 C30 1.506(14) . ? C31 C32 1.49(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.57(2) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C40 1.366(13) . ? C35 C36 1.389(12) . ? C35 H35 0.9300 . ? C36 C37 1.374(13) . ? C36 C55 1.517(13) . ? C37 C38 1.428(16) . ? C37 H37 0.9300 . ? C38 C39 1.352(14) . ? C38 H38 0.9300 . ? C39 C40 1.403(13) . ? C39 H39 0.9300 . ? C40 C41 1.502(13) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.349(14) . ? C42 H42 0.9300 . ? C43 C44 1.398(13) . ? C43 H43 0.9300 . ? C44 C45 1.460(13) . ? C45 C46 1.380(13) . ? C46 C47 1.340(15) . ? C46 H46 0.9300 . ? C47 C48 1.373(16) . ? C47 H47 0.9300 . ? C48 C49 1.363(14) . ? C48 H48 0.9300 . ? C49 C50 1.496(14) . ? C51 C52 1.42(2) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C54 C53 1.49(2) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54' C53' 1.49(2) . ? C54' H54D 0.9600 . ? C54' H54E 0.9600 . ? C54' H54F 0.9600 . ? C53' H53C 0.9700 . ? C53' H53D 0.9700 . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.339(15) . ? C56 H56 0.9300 . ? C57 C58 1.382(14) . ? C57 H57 0.9300 . ? C58 C59 1.473(14) . ? C59 C60 1.366(14) . ? C60 C61 1.363(18) . ? C60 H60 0.9300 . ? C61 C62 1.369(19) . ? C61 H61 0.9300 . ? C62 C63 1.358(15) . ? C62 H62 0.9300 . ? C63 C64 1.475(15) . ? C65 C66 1.61(3) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C65' C66' 1.62(3) . ? C65' H65C 0.9700 . ? C65' H65D 0.9700 . ? C66' H66D 0.9600 . ? C66' H66E 0.9600 . ? C66' H66F 0.9600 . ? C67 C68 1.48(2) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C100 H100 0.9300 . ? Cl1 O12 1.415(9) . ? Cl1 O13 1.418(8) . ? Cl1 O10 1.456(7) . ? Cl1 O11 1.466(10) . ? Cl2 O17 1.408(10) . ? Cl2 O16 1.425(12) . ? Cl2 O15 1.441(8) . ? Cl2 O14' 1.455(16) . ? Cl2 O14 1.462(16) . ? Cl3 O22 1.386(9) . ? Cl3 O25 1.389(8) . ? Cl3 O24 1.399(9) . ? Cl3 O23 1.448(10) . ? Cl4 O20' 1.392(14) . ? Cl4 O19 1.392(13) . ? Cl4 O21 1.412(13) . ? Cl4 O18 1.414(9) . ? Cl4 O19' 1.417(13) . ? Cl4 O20 1.469(13) . ? Cl4 O21' 1.471(14) . ? Cl5 O27 1.401(15) . ? Cl5 O28 1.410(13) . ? Cl5 O29 1.421(13) . ? Cl5 O26 1.439(15) . ? Cl5' O28' 1.439(14) . ? Cl5' O26' 1.440(16) . ? Cl5' O27' 1.465(14) . ? Cl5' O29' 1.542(12) . ? C1S N1S 1.41(3) . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? N1S O1S 1.20(2) . ? N1S O2S 1.20(2) . ? N2S O4S 1.13(2) . ? N2S O3S 1.13(3) . ? N2S C2S 1.38(4) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? 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 Yb1 O7 145.6(2) . . ? O2 Yb1 O4 95.8(3) . . ? O7 Yb1 O4 99.8(2) . . ? O2 Yb1 O10 93.5(3) . . ? O7 Yb1 O10 88.7(2) . . ? O4 Yb1 O10 149.1(2) . . ? O2 Yb1 N15 78.2(3) . . ? O7 Yb1 N15 80.8(2) . . ? O4 Yb1 N15 65.5(3) . . ? O10 Yb1 N15 145.4(2) . . ? O2 Yb1 N7 65.6(2) . . ? O7 Yb1 N7 148.0(2) . . ? O4 Yb1 N7 77.2(3) . . ? O10 Yb1 N7 79.9(3) . . ? N15 Yb1 N7 124.2(3) . . ? O2 Yb1 N6 131.1(2) . . ? O7 Yb1 N6 82.9(2) . . ? O4 Yb1 N6 73.8(2) . . ? O10 Yb1 N6 77.9(2) . . ? N15 Yb1 N6 132.3(3) . . ? N7 Yb1 N6 65.6(2) . . ? O2 Yb1 N14 71.8(2) . . ? O7 Yb1 N14 75.0(2) . . ? O4 Yb1 N14 131.6(2) . . ? O10 Yb1 N14 79.3(2) . . ? N15 Yb1 N14 66.2(2) . . ? N7 Yb1 N14 130.8(2) . . ? N6 Yb1 N14 148.4(2) . . ? O2 Yb1 C30 17.9(3) . . ? O7 Yb1 C30 162.8(2) . . ? O4 Yb1 C30 90.9(3) . . ? O10 Yb1 C30 89.0(3) . . ? N15 Yb1 C30 91.6(3) . . ? N7 Yb1 C30 47.7(3) . . ? N6 Yb1 C30 113.3(3) . . ? N14 Yb1 C30 87.9(2) . . ? O2 Yb1 C64 91.3(3) . . ? O7 Yb1 C64 94.1(3) . . ? O4 Yb1 C64 18.2(3) . . ? O10 Yb1 C64 167.2(3) . . ? N15 Yb1 C64 47.4(3) . . ? N7 Yb1 C64 91.3(3) . . ? N6 Yb1 C64 90.0(3) . . ? N14 Yb1 C64 113.5(3) . . ? C30 Yb1 C64 91.9(3) . . ? O3 Yb2 O1 94.9(3) . . ? O3 Yb2 O6 146.6(2) . . ? O1 Yb2 O6 98.3(2) . . ? O3 Yb2 O5 97.4(3) . . ? O1 Yb2 O5 144.9(2) . . ? O6 Yb2 O5 89.2(2) . . ? O3 Yb2 N10 65.4(3) . . ? O1 Yb2 N10 77.8(3) . . ? O6 Yb2 N10 147.6(2) . . ? O5 Yb2 N10 77.7(2) . . ? O3 Yb2 N2 74.9(3) . . ? O1 Yb2 N2 66.0(3) . . ? O6 Yb2 N2 82.7(2) . . ? O5 Yb2 N2 149.1(2) . . ? N10 Yb2 N2 122.7(3) . . ? O3 Yb2 N11 131.5(2) . . ? O1 Yb2 N11 72.5(2) . . ? O6 Yb2 N11 81.8(2) . . ? O5 Yb2 N11 74.8(2) . . ? N10 Yb2 N11 66.3(2) . . ? N2 Yb2 N11 132.6(2) . . ? O3 Yb2 N3 73.1(3) . . ? O1 Yb2 N3 130.4(2) . . ? O6 Yb2 N3 75.0(2) . . ? O5 Yb2 N3 84.6(2) . . ? N10 Yb2 N3 131.8(2) . . ? N2 Yb2 N3 64.5(2) . . ? N11 Yb2 N3 149.1(2) . . ? O3 Yb2 C16 91.6(3) . . ? O1 Yb2 C16 18.7(3) . . ? O6 Yb2 C16 91.3(2) . . ? O5 Yb2 C16 162.9(3) . . ? N10 Yb2 C16 93.1(3) . . ? N2 Yb2 C16 47.6(3) . . ? N11 Yb2 C16 88.3(3) . . ? N3 Yb2 C16 112.0(3) . . ? O3 Yb2 C50 18.1(3) . . ? O1 Yb2 C50 90.5(3) . . ? O6 Yb2 C50 164.2(2) . . ? O5 Yb2 C50 91.1(3) . . ? N10 Yb2 C50 47.3(3) . . ? N2 Yb2 C50 89.0(3) . . ? N11 Yb2 C50 113.6(2) . . ? N3 Yb2 C50 89.2(3) . . ? C16 Yb2 C50 93.0(3) . . ? C16 N1 C19 128.3(11) . . ? C16 N1 C17 113.6(10) . . ? C19 N1 C17 118.0(10) . . ? C11 N2 C15 119.3(9) . . ? C11 N2 Yb2 121.4(7) . . ? C15 N2 Yb2 117.2(6) . . ? C10 N3 N4 105.6(7) . . ? C10 N3 Yb2 114.9(6) . . ? N4 N3 Yb2 138.9(6) . . ? C8 N4 N3 109.9(8) . . ? C8 N4 C7 125.1(8) . . ? N3 N4 C7 124.7(8) . . ? C22 N5 N6 110.1(8) . . ? C22 N5 C21 126.7(8) . . ? N6 N5 C21 122.6(7) . . ? C24 N6 N5 103.9(7) . . ? C24 N6 Yb1 118.5(6) . . ? N5 N6 Yb1 137.1(6) . . ? C25 N7 C29 119.3(8) . . ? C25 N7 Yb1 121.2(6) . . ? C29 N7 Yb1 117.7(6) . . ? C30 N8 C31 116.8(10) . . ? C30 N8 C33 126.9(10) . . ? C31 N8 C33 116.2(10) . . ? C50 N9 C51 116.6(11) . . ? C50 N9 C53' 121.4(15) . . ? C51 N9 C53' 108.6(16) . . ? C50 N9 C53 125.4(12) . . ? C51 N9 C53 116.4(13) . . ? C53' N9 C53 48.2(14) . . ? C45 N10 C49 119.0(8) . . ? C45 N10 Yb2 121.6(6) . . ? C49 N10 Yb2 119.4(6) . . ? C44 N11 N12 104.3(7) . . ? C44 N11 Yb2 115.8(6) . . ? N12 N11 Yb2 139.8(5) . . ? N11 N12 C42 111.4(8) . . ? N11 N12 C41 122.7(7) . . ? C42 N12 C41 125.7(8) . . ? C56 N13 N14 111.8(8) . . ? C56 N13 C55 125.5(8) . . ? N14 N13 C55 122.7(7) . . ? C58 N14 N13 103.7(7) . . ? C58 N14 Yb1 114.2(6) . . ? N13 N14 Yb1 141.8(6) . . ? C59 N15 C63 119.5(8) . . ? C59 N15 Yb1 122.1(6) . . ? C63 N15 Yb1 118.3(6) . . ? C64 N16 C67 118.4(13) . . ? C64 N16 C65 128.0(15) . . ? C67 N16 C65 105.4(15) . . ? C64 N16 C65' 113.4(16) . . ? C67 N16 C65' 117.8(16) . . ? C65 N16 C65' 62.2(15) . . ? C16 O1 Yb2 126.3(7) . . ? C30 O2 Yb1 128.5(6) . . ? C50 O3 Yb2 129.0(7) . . ? C64 O4 Yb1 127.8(6) . . ? C100 O6 Yb2 138.3(6) . . ? C100 O7 Yb1 139.8(6) . . ? C6 C1 C2 121.5(9) . . ? C6 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 118.2(9) . . ? C3 C2 C21 122.8(9) . . ? C1 C2 C21 119.0(8) . . ? C4 C3 C2 121.2(11) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.8(10) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 120.8(10) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 118.4(10) . . ? C5 C6 C7 120.7(9) . . ? C1 C6 C7 120.9(8) . . ? N4 C7 C6 113.0(8) . . ? N4 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? N4 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N4 C8 C9 108.7(10) . . ? N4 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? C8 C9 C10 105.0(10) . . ? C8 C9 H9 127.5 . . ? C10 C9 H9 127.5 . . ? N3 C10 C9 110.8(9) . . ? N3 C10 C11 120.3(8) . . ? C9 C10 C11 128.9(10) . . ? N2 C11 C12 122.8(10) . . ? N2 C11 C10 116.5(9) . . ? C12 C11 C10 120.7(10) . . ? C11 C12 C13 117.7(11) . . ? C11 C12 H12 121.1 . . ? C13 C12 H12 121.1 . . ? C14 C13 C12 119.3(11) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C15 C14 C13 119.4(11) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 N2 121.4(11) . . ? C14 C15 C16 128.1(10) . . ? N2 C15 C16 110.2(8) . . ? O1 C16 N1 120.8(10) . . ? O1 C16 C15 117.2(9) . . ? N1 C16 C15 122.0(10) . . ? O1 C16 Yb2 35.1(5) . . ? N1 C16 Yb2 152.3(8) . . ? C15 C16 Yb2 83.9(6) . . ? N1 C17 C18 114.4(11) . . ? N1 C17 H17A 108.7 . . ? C18 C17 H17A 108.7 . . ? N1 C17 H17B 108.7 . . ? C18 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C20 111.1(11) . . ? N1 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? N1 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 C2 112.2(7) . . ? N5 C21 H21A 109.2 . . ? C2 C21 H21A 109.2 . . ? N5 C21 H21B 109.2 . . ? C2 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? N5 C22 C23 108.8(8) . . ? N5 C22 H22 125.6 . . ? C23 C22 H22 125.6 . . ? C22 C23 C24 104.3(9) . . ? C22 C23 H23 127.9 . . ? C24 C23 H23 127.9 . . ? N6 C24 C23 112.8(9) . . ? N6 C24 C25 117.6(8) . . ? C23 C24 C25 129.6(9) . . ? N7 C25 C26 122.5(9) . . ? N7 C25 C24 115.7(8) . . ? C26 C25 C24 121.8(9) . . ? C25 C26 C27 117.6(10) . . ? C25 C26 H26 121.2 . . ? C27 C26 H26 121.2 . . ? C28 C27 C26 119.7(11) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 120.5(11) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? N7 C29 C28 120.4(10) . . ? N7 C29 C30 110.1(8) . . ? C28 C29 C30 129.5(10) . . ? O2 C30 N8 119.1(10) . . ? O2 C30 C29 116.0(8) . . ? N8 C30 C29 124.7(9) . . ? O2 C30 Yb1 33.6(4) . . ? N8 C30 Yb1 151.0(8) . . ? C29 C30 Yb1 82.9(5) . . ? N8 C31 C32 113.0(16) . . ? N8 C31 H31A 109.0 . . ? C32 C31 H31A 109.0 . . ? N8 C31 H31B 109.0 . . ? C32 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N8 C33 C34 109.8(12) . . ? N8 C33 H33A 109.7 . . ? C34 C33 H33A 109.7 . . ? N8 C33 H33B 109.7 . . ? C34 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 122.9(9) . . ? C40 C35 H35 118.5 . . ? C36 C35 H35 118.5 . . ? C37 C36 C35 119.1(9) . . ? C37 C36 C55 120.4(8) . . ? C35 C36 C55 120.4(8) . . ? C36 C37 C38 118.9(9) . . ? C36 C37 H37 120.6 . . ? C38 C37 H37 120.6 . . ? C39 C38 C37 120.1(9) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 121.4(10) . . ? C38 C39 H39 119.3 . . ? C40 C39 H39 119.3 . . ? C35 C40 C39 117.5(9) . . ? C35 C40 C41 120.7(8) . . ? C39 C40 C41 121.6(8) . . ? N12 C41 C40 113.5(7) . . ? N12 C41 H41A 108.9 . . ? C40 C41 H41A 108.9 . . ? N12 C41 H41B 108.9 . . ? C40 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? C43 C42 N12 107.8(9) . . ? C43 C42 H42 126.1 . . ? N12 C42 H42 126.1 . . ? C42 C43 C44 104.7(8) . . ? C42 C43 H43 127.6 . . ? C44 C43 H43 127.6 . . ? N11 C44 C43 111.7(8) . . ? N11 C44 C45 120.2(8) . . ? C43 C44 C45 128.1(8) . . ? N10 C45 C46 120.7(9) . . ? N10 C45 C44 116.1(8) . . ? C46 C45 C44 123.1(9) . . ? C47 C46 C45 119.8(10) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C46 C47 C48 120.3(10) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C49 C48 C47 118.1(10) . . ? C49 C48 H48 121.0 . . ? C47 C48 H48 121.0 . . ? N10 C49 C48 122.0(10) . . ? N10 C49 C50 110.0(8) . . ? C48 C49 C50 128.0(9) . . ? O3 C50 N9 118.9(10) . . ? O3 C50 C49 116.2(9) . . ? N9 C50 C49 124.8(9) . . ? O3 C50 Yb2 33.0(5) . . ? N9 C50 Yb2 151.9(8) . . ? C49 C50 Yb2 83.3(6) . . ? C52 C51 N9 107.2(17) . . ? C52 C51 H51A 110.3 . . ? N9 C51 H51A 110.3 . . ? C52 C51 H51B 110.3 . . ? N9 C51 H51B 110.3 . . ? H51A C51 H51B 108.5 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 N9 109.5(14) . . ? C54 C53 H53A 109.8 . . ? N9 C53 H53A 109.8 . . ? C54 C53 H53B 109.8 . . ? N9 C53 H53B 109.8 . . ? H53A C53 H53B 108.2 . . ? C53' C54' H54D 109.5 . . ? C53' C54' H54E 109.5 . . ? H54D C54' H54E 109.5 . . ? C53' C54' H54F 109.5 . . ? H54D C54' H54F 109.5 . . ? H54E C54' H54F 109.5 . . ? C54' C53' N9 103(2) . . ? C54' C53' H53C 111.1 . . ? N9 C53' H53C 111.1 . . ? C54' C53' H53D 111.1 . . ? N9 C53' H53D 111.1 . . ? H53C C53' H53D 109.1 . . ? N13 C55 C36 112.1(8) . . ? N13 C55 H55A 109.2 . . ? C36 C55 H55A 109.2 . . ? N13 C55 H55B 109.2 . . ? C36 C55 H55B 109.2 . . ? H55A C55 H55B 107.9 . . ? N13 C56 C57 108.2(9) . . ? N13 C56 H56 125.9 . . ? C57 C56 H56 125.9 . . ? C56 C57 C58 105.0(9) . . ? C56 C57 H57 127.5 . . ? C58 C57 H57 127.5 . . ? N14 C58 C57 111.4(9) . . ? N14 C58 C59 120.5(8) . . ? C57 C58 C59 128.1(9) . . ? N15 C59 C60 122.0(10) . . ? N15 C59 C58 116.8(8) . . ? C60 C59 C58 121.1(9) . . ? C61 C60 C59 118.2(12) . . ? C61 C60 H60 120.9 . . ? C59 C60 H60 120.9 . . ? C60 C61 C62 119.8(13) . . ? C60 C61 H61 120.1 . . ? C62 C61 H61 120.1 . . ? C63 C62 C61 120.0(11) . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? N15 C63 C62 120.4(10) . . ? N15 C63 C64 111.7(8) . . ? C62 C63 C64 127.5(10) . . ? O4 C64 N16 118.8(11) . . ? O4 C64 C63 116.5(8) . . ? N16 C64 C63 124.6(11) . . ? O4 C64 Yb1 34.1(4) . . ? N16 C64 Yb1 152.9(10) . . ? C63 C64 Yb1 82.5(5) . . ? N16 C65 C66 97.0(16) . . ? N16 C65 H65A 112.4 . . ? C66 C65 H65A 112.4 . . ? N16 C65 H65B 112.4 . . ? C66 C65 H65B 112.4 . . ? H65A C65 H65B 109.9 . . ? C66' C65' N16 106.4(19) . . ? C66' C65' H65C 110.4 . . ? N16 C65' H65C 110.4 . . ? C66' C65' H65D 110.4 . . ? N16 C65' H65D 110.4 . . ? H65C C65' H65D 108.6 . . ? C65' C66' H66D 109.5 . . ? C65' C66' H66E 109.5 . . ? H66D C66' H66E 109.5 . . ? C65' C66' H66F 109.5 . . ? H66D C66' H66F 109.5 . . ? H66E C66' H66F 109.5 . . ? C68 C67 N16 110.1(15) . . ? C68 C67 H67A 109.6 . . ? N16 C67 H67A 109.6 . . ? C68 C67 H67B 109.6 . . ? N16 C67 H67B 109.6 . . ? H67A C67 H67B 108.1 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O7 C100 O6 125.1(9) . . ? O7 C100 H100 117.5 . . ? O6 C100 H100 117.5 . . ? O12 Cl1 O13 112.3(6) . . ? O12 Cl1 O10 106.5(5) . . ? O13 Cl1 O10 109.4(5) . . ? O12 Cl1 O11 112.1(7) . . ? O13 Cl1 O11 109.4(6) . . ? O10 Cl1 O11 107.0(5) . . ? Cl1 O10 Yb1 145.9(4) . . ? O17 Cl2 O16 109.7(7) . . ? O17 Cl2 O15 110.9(6) . . ? O16 Cl2 O15 107.8(6) . . ? O17 Cl2 O14' 100.8(15) . . ? O16 Cl2 O14' 119.5(15) . . ? O15 Cl2 O14' 108.0(10) . . ? O17 Cl2 O14 124.3(13) . . ? O16 Cl2 O14 93.9(14) . . ? O15 Cl2 O14 108.2(10) . . ? O14' Cl2 O14 28.4(11) . . ? O22 Cl3 O25 108.4(6) . . ? O22 Cl3 O24 114.0(8) . . ? O25 Cl3 O24 110.5(6) . . ? O22 Cl3 O23 106.6(8) . . ? O25 Cl3 O23 109.4(6) . . ? O24 Cl3 O23 107.7(6) . . ? O20' Cl4 O19 123.1(13) . . ? O20' Cl4 O21 35.1(9) . . ? O19 Cl4 O21 115.3(9) . . ? O20' Cl4 O18 120.9(10) . . ? O19 Cl4 O18 114.1(9) . . ? O21 Cl4 O18 107.4(9) . . ? O20' Cl4 O19' 110.4(10) . . ? O19 Cl4 O19' 52.0(9) . . ? O21 Cl4 O19' 136.4(12) . . ? O18 Cl4 O19' 115.7(9) . . ? O20' Cl4 O20 74.6(10) . . ? O19 Cl4 O20 110.4(9) . . ? O21 Cl4 O20 109.0(8) . . ? O18 Cl4 O20 99.5(8) . . ? O19' Cl4 O20 58.8(9) . . ? O20' Cl4 O21' 105.2(10) . . ? O19 Cl4 O21' 50.5(10) . . ? O21 Cl4 O21' 76.1(10) . . ? O18 Cl4 O21' 99.4(10) . . ? O19' Cl4 O21' 102.2(9) . . ? O20 Cl4 O21' 157.8(11) . . ? O27 Cl5 O28 102.8(14) . . ? O27 Cl5 O29 110.7(13) . . ? O28 Cl5 O29 107.5(11) . . ? O27 Cl5 O26 113.1(16) . . ? O28 Cl5 O26 105.5(13) . . ? O29 Cl5 O26 116.1(13) . . ? O28' Cl5' O26' 111.5(19) . . ? O28' Cl5' O27' 104.5(14) . . ? O26' Cl5' O27' 102.5(19) . . ? O28' Cl5' O29' 112.0(12) . . ? O26' Cl5' O29' 108.6(17) . . ? O27' Cl5' O29' 117.4(12) . . ? N1S C1S H1S1 109.5 . . ? N1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? N1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O1S N1S O2S 109(2) . . ? O1S N1S C1S 124(3) . . ? O2S N1S C1S 124(3) . . ? O4S N2S O3S 122(3) . . ? O4S N2S C2S 117(2) . . ? O3S N2S C2S 121(2) . . ? N2S C2S H2S1 109.5 . . ? N2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? N2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Yb2 N2 C11 64.3(8) . . . . ? O1 Yb2 N2 C11 166.8(8) . . . . ? O6 Yb2 N2 C11 -90.7(8) . . . . ? O5 Yb2 N2 C11 -14.7(10) . . . . ? N10 Yb2 N2 C11 110.9(8) . . . . ? N11 Yb2 N2 C11 -162.5(7) . . . . ? N3 Yb2 N2 C11 -13.9(7) . . . . ? C16 Yb2 N2 C11 170.9(9) . . . . ? C50 Yb2 N2 C11 75.8(8) . . . . ? O3 Yb2 N2 C15 -99.2(7) . . . . ? O1 Yb2 N2 C15 3.3(7) . . . . ? O6 Yb2 N2 C15 105.8(7) . . . . ? O5 Yb2 N2 C15 -178.2(6) . . . . ? N10 Yb2 N2 C15 -52.5(8) . . . . ? N11 Yb2 N2 C15 34.1(8) . . . . ? N3 Yb2 N2 C15 -177.3(8) . . . . ? C16 Yb2 N2 C15 7.4(6) . . . . ? C50 Yb2 N2 C15 -87.7(7) . . . . ? O3 Yb2 N3 C10 -70.1(7) . . . . ? O1 Yb2 N3 C10 11.7(8) . . . . ? O6 Yb2 N3 C10 99.9(7) . . . . ? O5 Yb2 N3 C10 -169.5(7) . . . . ? N10 Yb2 N3 C10 -101.2(7) . . . . ? N2 Yb2 N3 C10 10.9(7) . . . . ? N11 Yb2 N3 C10 142.6(7) . . . . ? C16 Yb2 N3 C10 14.7(7) . . . . ? C50 Yb2 N3 C10 -78.3(7) . . . . ? O3 Yb2 N3 N4 99.4(9) . . . . ? O1 Yb2 N3 N4 -178.8(8) . . . . ? O6 Yb2 N3 N4 -90.6(9) . . . . ? O5 Yb2 N3 N4 0.0(9) . . . . ? N10 Yb2 N3 N4 68.3(10) . . . . ? N2 Yb2 N3 N4 -179.6(10) . . . . ? N11 Yb2 N3 N4 -47.9(11) . . . . ? C16 Yb2 N3 N4 -175.8(8) . . . . ? C50 Yb2 N3 N4 91.2(9) . . . . ? C10 N3 N4 C8 -0.9(11) . . . . ? Yb2 N3 N4 C8 -171.1(8) . . . . ? C10 N3 N4 C7 -176.0(9) . . . . ? Yb2 N3 N4 C7 13.8(14) . . . . ? C22 N5 N6 C24 0.0(10) . . . . ? C21 N5 N6 C24 171.5(8) . . . . ? C22 N5 N6 Yb1 171.8(7) . . . . ? C21 N5 N6 Yb1 -16.7(13) . . . . ? O2 Yb1 N6 C24 0.0(8) . . . . ? O7 Yb1 N6 C24 174.2(7) . . . . ? O4 Yb1 N6 C24 -83.4(7) . . . . ? O10 Yb1 N6 C24 84.0(7) . . . . ? N15 Yb1 N6 C24 -115.3(7) . . . . ? N7 Yb1 N6 C24 -0.3(6) . . . . ? N14 Yb1 N6 C24 128.8(7) . . . . ? C30 Yb1 N6 C24 0.4(7) . . . . ? C64 Yb1 N6 C24 -91.7(7) . . . . ? O2 Yb1 N6 N5 -170.8(7) . . . . ? O7 Yb1 N6 N5 3.3(8) . . . . ? O4 Yb1 N6 N5 105.7(8) . . . . ? O10 Yb1 N6 N5 -86.8(8) . . . . ? N15 Yb1 N6 N5 73.9(9) . . . . ? N7 Yb1 N6 N5 -171.2(9) . . . . ? N14 Yb1 N6 N5 -42.0(10) . . . . ? C30 Yb1 N6 N5 -170.5(8) . . . . ? C64 Yb1 N6 N5 97.4(8) . . . . ? O2 Yb1 N7 C25 173.0(8) . . . . ? O7 Yb1 N7 C25 -17.6(10) . . . . ? O4 Yb1 N7 C25 70.4(7) . . . . ? O10 Yb1 N7 C25 -88.5(8) . . . . ? N15 Yb1 N7 C25 118.5(7) . . . . ? N6 Yb1 N7 C25 -7.3(7) . . . . ? N14 Yb1 N7 C25 -154.8(7) . . . . ? C30 Yb1 N7 C25 173.6(9) . . . . ? C64 Yb1 N7 C25 82.1(8) . . . . ? O2 Yb1 N7 C29 8.3(7) . . . . ? O7 Yb1 N7 C29 177.7(6) . . . . ? O4 Yb1 N7 C29 -94.2(7) . . . . ? O10 Yb1 N7 C29 106.9(7) . . . . ? N15 Yb1 N7 C29 -46.1(8) . . . . ? N6 Yb1 N7 C29 -172.0(8) . . . . ? N14 Yb1 N7 C29 40.5(8) . . . . ? C30 Yb1 N7 C29 8.9(7) . . . . ? C64 Yb1 N7 C29 -82.6(7) . . . . ? O3 Yb2 N10 C45 178.7(8) . . . . ? O1 Yb2 N10 C45 77.5(7) . . . . ? O6 Yb2 N10 C45 -8.9(9) . . . . ? O5 Yb2 N10 C45 -77.1(7) . . . . ? N2 Yb2 N10 C45 128.2(7) . . . . ? N11 Yb2 N10 C45 1.5(6) . . . . ? N3 Yb2 N10 C45 -148.3(6) . . . . ? C16 Yb2 N10 C45 88.4(7) . . . . ? C50 Yb2 N10 C45 179.7(8) . . . . ? O3 Yb2 N10 C49 -0.6(7) . . . . ? O1 Yb2 N10 C49 -101.8(7) . . . . ? O6 Yb2 N10 C49 171.8(6) . . . . ? O5 Yb2 N10 C49 103.6(7) . . . . ? N2 Yb2 N10 C49 -51.2(7) . . . . ? N11 Yb2 N10 C49 -177.8(7) . . . . ? N3 Yb2 N10 C49 32.4(8) . . . . ? C16 Yb2 N10 C49 -91.0(7) . . . . ? C50 Yb2 N10 C49 0.3(6) . . . . ? O3 Yb2 N11 C44 -5.5(8) . . . . ? O1 Yb2 N11 C44 -86.2(6) . . . . ? O6 Yb2 N11 C44 172.3(6) . . . . ? O5 Yb2 N11 C44 81.0(6) . . . . ? N10 Yb2 N11 C44 -2.0(6) . . . . ? N2 Yb2 N11 C44 -115.5(6) . . . . ? N3 Yb2 N11 C44 131.0(6) . . . . ? C16 Yb2 N11 C44 -96.1(6) . . . . ? C50 Yb2 N11 C44 -3.5(7) . . . . ? O3 Yb2 N11 N12 179.2(8) . . . . ? O1 Yb2 N11 N12 98.5(9) . . . . ? O6 Yb2 N11 N12 -3.0(8) . . . . ? O5 Yb2 N11 N12 -94.4(8) . . . . ? N10 Yb2 N11 N12 -177.4(9) . . . . ? N2 Yb2 N11 N12 69.1(9) . . . . ? N3 Yb2 N11 N12 -44.4(11) . . . . ? C16 Yb2 N11 N12 88.5(8) . . . . ? C50 Yb2 N11 N12 -178.9(8) . . . . ? C44 N11 N12 C42 -1.4(10) . . . . ? Yb2 N11 N12 C42 174.3(7) . . . . ? C44 N11 N12 C41 173.8(8) . . . . ? Yb2 N11 N12 C41 -10.5(13) . . . . ? C56 N13 N14 C58 0.3(10) . . . . ? C55 N13 N14 C58 -178.1(8) . . . . ? C56 N13 N14 Yb1 -171.7(7) . . . . ? C55 N13 N14 Yb1 9.9(14) . . . . ? O2 Yb1 N14 C58 -80.8(6) . . . . ? O7 Yb1 N14 C58 90.4(6) . . . . ? O4 Yb1 N14 C58 0.6(7) . . . . ? O10 Yb1 N14 C58 -178.1(6) . . . . ? N15 Yb1 N14 C58 4.0(6) . . . . ? N7 Yb1 N14 C58 -111.5(6) . . . . ? N6 Yb1 N14 C58 137.4(6) . . . . ? C30 Yb1 N14 C58 -88.7(6) . . . . ? C64 Yb1 N14 C58 2.5(7) . . . . ? O2 Yb1 N14 N13 90.6(9) . . . . ? O7 Yb1 N14 N13 -98.2(9) . . . . ? O4 Yb1 N14 N13 172.0(8) . . . . ? O10 Yb1 N14 N13 -6.7(9) . . . . ? N15 Yb1 N14 N13 175.5(9) . . . . ? N7 Yb1 N14 N13 59.9(10) . . . . ? N6 Yb1 N14 N13 -51.2(11) . . . . ? C30 Yb1 N14 N13 82.8(9) . . . . ? C64 Yb1 N14 N13 173.9(8) . . . . ? O2 Yb1 N15 C59 72.5(7) . . . . ? O7 Yb1 N15 C59 -80.2(7) . . . . ? O4 Yb1 N15 C59 174.5(7) . . . . ? O10 Yb1 N15 C59 -6.3(9) . . . . ? N7 Yb1 N15 C59 121.6(7) . . . . ? N6 Yb1 N15 C59 -151.6(6) . . . . ? N14 Yb1 N15 C59 -2.7(6) . . . . ? C30 Yb1 N15 C59 84.3(7) . . . . ? C64 Yb1 N15 C59 175.5(8) . . . . ? O2 Yb1 N15 C63 -105.3(7) . . . . ? O7 Yb1 N15 C63 102.0(7) . . . . ? O4 Yb1 N15 C63 -3.2(6) . . . . ? O10 Yb1 N15 C63 175.9(6) . . . . ? N7 Yb1 N15 C63 -56.1(7) . . . . ? N6 Yb1 N15 C63 30.6(8) . . . . ? N14 Yb1 N15 C63 179.6(7) . . . . ? C30 Yb1 N15 C63 -93.5(7) . . . . ? C64 Yb1 N15 C63 -2.3(6) . . . . ? O3 Yb2 O1 C16 80.5(8) . . . . ? O6 Yb2 O1 C16 -68.7(8) . . . . ? O5 Yb2 O1 C16 -169.2(7) . . . . ? N10 Yb2 O1 C16 144.0(8) . . . . ? N2 Yb2 O1 C16 9.4(7) . . . . ? N11 Yb2 O1 C16 -147.3(8) . . . . ? N3 Yb2 O1 C16 8.7(9) . . . . ? C50 Yb2 O1 C16 98.1(8) . . . . ? O7 Yb1 O2 C30 -168.6(8) . . . . ? O4 Yb1 O2 C30 74.6(9) . . . . ? O10 Yb1 O2 C30 -75.9(9) . . . . ? N15 Yb1 O2 C30 138.0(10) . . . . ? N7 Yb1 O2 C30 1.5(9) . . . . ? N6 Yb1 O2 C30 1.1(11) . . . . ? N14 Yb1 O2 C30 -153.4(10) . . . . ? C64 Yb1 O2 C30 92.2(9) . . . . ? O1 Yb2 O3 C50 76.5(12) . . . . ? O6 Yb2 O3 C50 -170.4(9) . . . . ? O5 Yb2 O3 C50 -70.5(12) . . . . ? N10 Yb2 O3 C50 2.3(11) . . . . ? N2 Yb2 O3 C50 140.0(12) . . . . ? N11 Yb2 O3 C50 5.7(14) . . . . ? N3 Yb2 O3 C50 -152.6(12) . . . . ? C16 Yb2 O3 C50 94.9(12) . . . . ? O2 Yb1 O4 C64 76.4(8) . . . . ? O7 Yb1 O4 C64 -72.9(8) . . . . ? O10 Yb1 O4 C64 -176.9(7) . . . . ? N15 Yb1 O4 C64 2.2(8) . . . . ? N7 Yb1 O4 C64 139.7(9) . . . . ? N6 Yb1 O4 C64 -152.4(9) . . . . ? N14 Yb1 O4 C64 5.6(9) . . . . ? C30 Yb1 O4 C64 93.6(8) . . . . ? O3 Yb2 O6 C100 -13.0(11) . . . . ? O1 Yb2 O6 C100 99.2(8) . . . . ? O5 Yb2 O6 C100 -115.2(8) . . . . ? N10 Yb2 O6 C100 179.6(7) . . . . ? N2 Yb2 O6 C100 34.9(8) . . . . ? N11 Yb2 O6 C100 170.0(8) . . . . ? N3 Yb2 O6 C100 -30.6(8) . . . . ? C16 Yb2 O6 C100 81.9(8) . . . . ? C50 Yb2 O6 C100 -23.9(15) . . . . ? O2 Yb1 O7 C100 -30.5(11) . . . . ? O4 Yb1 O7 C100 85.2(9) . . . . ? O10 Yb1 O7 C100 -124.7(9) . . . . ? N15 Yb1 O7 C100 22.2(9) . . . . ? N7 Yb1 O7 C100 166.7(8) . . . . ? N6 Yb1 O7 C100 157.3(9) . . . . ? N14 Yb1 O7 C100 -45.4(9) . . . . ? C30 Yb1 O7 C100 -42.3(14) . . . . ? C64 Yb1 O7 C100 67.8(9) . . . . ? C6 C1 C2 C3 3.7(14) . . . . ? C6 C1 C2 C21 -179.6(8) . . . . ? C1 C2 C3 C4 -2.1(16) . . . . ? C21 C2 C3 C4 -178.7(10) . . . . ? C2 C3 C4 C5 -0.1(19) . . . . ? C3 C4 C5 C6 0.8(18) . . . . ? C4 C5 C6 C1 0.7(16) . . . . ? C4 C5 C6 C7 -178.6(10) . . . . ? C2 C1 C6 C5 -3.0(14) . . . . ? C2 C1 C6 C7 176.3(8) . . . . ? C8 N4 C7 C6 -83.8(12) . . . . ? N3 N4 C7 C6 90.6(11) . . . . ? C5 C6 C7 N4 93.1(11) . . . . ? C1 C6 C7 N4 -86.2(11) . . . . ? N3 N4 C8 C9 1.5(14) . . . . ? C7 N4 C8 C9 176.6(10) . . . . ? N4 C8 C9 C10 -1.4(15) . . . . ? N4 N3 C10 C9 0.0(12) . . . . ? Yb2 N3 C10 C9 172.9(8) . . . . ? N4 N3 C10 C11 178.7(9) . . . . ? Yb2 N3 C10 C11 -8.5(12) . . . . ? C8 C9 C10 N3 0.8(14) . . . . ? C8 C9 C10 C11 -177.6(11) . . . . ? C15 N2 C11 C12 -0.2(16) . . . . ? Yb2 N2 C11 C12 -163.3(9) . . . . ? C15 N2 C11 C10 178.4(9) . . . . ? Yb2 N2 C11 C10 15.3(12) . . . . ? N3 C10 C11 N2 -3.6(15) . . . . ? C9 C10 C11 N2 174.7(12) . . . . ? N3 C10 C11 C12 175.0(11) . . . . ? C9 C10 C11 C12 -6.7(19) . . . . ? N2 C11 C12 C13 1.5(19) . . . . ? C10 C11 C12 C13 -177.0(12) . . . . ? C11 C12 C13 C14 -1(2) . . . . ? C12 C13 C14 C15 -1(2) . . . . ? C13 C14 C15 N2 2.2(18) . . . . ? C13 C14 C15 C16 175.4(11) . . . . ? C11 N2 C15 C14 -1.7(15) . . . . ? Yb2 N2 C15 C14 162.1(8) . . . . ? C11 N2 C15 C16 -176.0(9) . . . . ? Yb2 N2 C15 C16 -12.2(10) . . . . ? Yb2 O1 C16 N1 160.8(7) . . . . ? Yb2 O1 C16 C15 -19.8(12) . . . . ? C19 N1 C16 O1 -166.4(10) . . . . ? C17 N1 C16 O1 10.8(15) . . . . ? C19 N1 C16 C15 14.3(17) . . . . ? C17 N1 C16 C15 -168.5(10) . . . . ? C19 N1 C16 Yb2 -142.5(13) . . . . ? C17 N1 C16 Yb2 35(2) . . . . ? C14 C15 C16 O1 -153.9(11) . . . . ? N2 C15 C16 O1 19.9(13) . . . . ? C14 C15 C16 N1 25.5(17) . . . . ? N2 C15 C16 N1 -160.7(9) . . . . ? C14 C15 C16 Yb2 -165.2(11) . . . . ? N2 C15 C16 Yb2 8.6(7) . . . . ? O3 Yb2 C16 O1 -100.5(8) . . . . ? O6 Yb2 C16 O1 112.7(8) . . . . ? O5 Yb2 C16 O1 21.4(13) . . . . ? N10 Yb2 C16 O1 -35.1(8) . . . . ? N2 Yb2 C16 O1 -168.3(9) . . . . ? N11 Yb2 C16 O1 31.0(8) . . . . ? N3 Yb2 C16 O1 -172.9(7) . . . . ? C50 Yb2 C16 O1 -82.5(8) . . . . ? O3 Yb2 C16 N1 -137.8(16) . . . . ? O1 Yb2 C16 N1 -37.3(15) . . . . ? O6 Yb2 C16 N1 75.4(17) . . . . ? O5 Yb2 C16 N1 -16(2) . . . . ? N10 Yb2 C16 N1 -72.4(17) . . . . ? N2 Yb2 C16 N1 154.4(18) . . . . ? N11 Yb2 C16 N1 -6.3(16) . . . . ? N3 Yb2 C16 N1 149.8(16) . . . . ? C50 Yb2 C16 N1 -119.8(16) . . . . ? O3 Yb2 C16 C15 61.8(6) . . . . ? O1 Yb2 C16 C15 162.3(11) . . . . ? O6 Yb2 C16 C15 -84.9(6) . . . . ? O5 Yb2 C16 C15 -176.2(7) . . . . ? N10 Yb2 C16 C15 127.2(6) . . . . ? N2 Yb2 C16 C15 -6.0(5) . . . . ? N11 Yb2 C16 C15 -166.7(6) . . . . ? N3 Yb2 C16 C15 -10.6(6) . . . . ? C50 Yb2 C16 C15 79.8(6) . . . . ? C16 N1 C17 C18 70.0(14) . . . . ? C19 N1 C17 C18 -112.4(13) . . . . ? C16 N1 C19 C20 -111.1(14) . . . . ? C17 N1 C19 C20 71.8(15) . . . . ? C22 N5 C21 C2 100.3(11) . . . . ? N6 N5 C21 C2 -69.8(10) . . . . ? C3 C2 C21 N5 -24.1(13) . . . . ? C1 C2 C21 N5 159.4(8) . . . . ? N6 N5 C22 C23 0.8(11) . . . . ? C21 N5 C22 C23 -170.2(9) . . . . ? N5 C22 C23 C24 -1.3(12) . . . . ? N5 N6 C24 C23 -0.9(11) . . . . ? Yb1 N6 C24 C23 -174.5(7) . . . . ? N5 N6 C24 C25 -179.4(8) . . . . ? Yb1 N6 C24 C25 7.0(11) . . . . ? C22 C23 C24 N6 1.4(12) . . . . ? C22 C23 C24 C25 179.7(10) . . . . ? C29 N7 C25 C26 -1.1(16) . . . . ? Yb1 N7 C25 C26 -165.5(9) . . . . ? C29 N7 C25 C24 177.9(9) . . . . ? Yb1 N7 C25 C24 13.5(12) . . . . ? N6 C24 C25 N7 -13.3(13) . . . . ? C23 C24 C25 N7 168.5(10) . . . . ? N6 C24 C25 C26 165.7(10) . . . . ? C23 C24 C25 C26 -12.5(18) . . . . ? N7 C25 C26 C27 3.4(18) . . . . ? C24 C25 C26 C27 -175.5(11) . . . . ? C25 C26 C27 C28 -3(2) . . . . ? C26 C27 C28 C29 1(2) . . . . ? C25 N7 C29 C28 -1.5(16) . . . . ? Yb1 N7 C29 C28 163.5(10) . . . . ? C25 N7 C29 C30 -179.7(9) . . . . ? Yb1 N7 C29 C30 -14.7(11) . . . . ? C27 C28 C29 N7 2(2) . . . . ? C27 C28 C29 C30 179.4(13) . . . . ? Yb1 O2 C30 N8 166.3(8) . . . . ? Yb1 O2 C30 C29 -9.9(14) . . . . ? C31 N8 C30 O2 6.6(18) . . . . ? C33 N8 C30 O2 -169.0(12) . . . . ? C31 N8 C30 C29 -177.6(13) . . . . ? C33 N8 C30 C29 7(2) . . . . ? C31 N8 C30 Yb1 22(2) . . . . ? C33 N8 C30 Yb1 -153.3(13) . . . . ? N7 C29 C30 O2 15.7(14) . . . . ? C28 C29 C30 O2 -162.3(13) . . . . ? N7 C29 C30 N8 -160.2(11) . . . . ? C28 C29 C30 N8 22(2) . . . . ? N7 C29 C30 Yb1 10.2(8) . . . . ? C28 C29 C30 Yb1 -167.8(13) . . . . ? O7 Yb1 C30 O2 22.2(15) . . . . ? O4 Yb1 C30 O2 -106.4(9) . . . . ? O10 Yb1 C30 O2 104.5(9) . . . . ? N15 Yb1 C30 O2 -40.9(9) . . . . ? N7 Yb1 C30 O2 -178.2(11) . . . . ? N6 Yb1 C30 O2 -179.1(9) . . . . ? N14 Yb1 C30 O2 25.2(9) . . . . ? C64 Yb1 C30 O2 -88.3(9) . . . . ? O2 Yb1 C30 N8 -25.3(14) . . . . ? O7 Yb1 C30 N8 -3(2) . . . . ? O4 Yb1 C30 N8 -131.7(17) . . . . ? O10 Yb1 C30 N8 79.3(17) . . . . ? N15 Yb1 C30 N8 -66.2(17) . . . . ? N7 Yb1 C30 N8 156.5(18) . . . . ? N6 Yb1 C30 N8 155.6(16) . . . . ? N14 Yb1 C30 N8 -0.1(17) . . . . ? C64 Yb1 C30 N8 -113.6(17) . . . . ? O2 Yb1 C30 C29 171.1(13) . . . . ? O7 Yb1 C30 C29 -166.8(7) . . . . ? O4 Yb1 C30 C29 64.7(6) . . . . ? O10 Yb1 C30 C29 -84.4(6) . . . . ? N15 Yb1 C30 C29 130.2(6) . . . . ? N7 Yb1 C30 C29 -7.1(5) . . . . ? N6 Yb1 C30 C29 -8.0(7) . . . . ? N14 Yb1 C30 C29 -163.8(6) . . . . ? C64 Yb1 C30 C29 82.8(6) . . . . ? C30 N8 C31 C32 -85.4(17) . . . . ? C33 N8 C31 C32 90.7(16) . . . . ? C30 N8 C33 C34 -102.9(15) . . . . ? C31 N8 C33 C34 81.5(17) . . . . ? C40 C35 C36 C37 1.8(15) . . . . ? C40 C35 C36 C55 -175.4(9) . . . . ? C35 C36 C37 C38 0.2(17) . . . . ? C55 C36 C37 C38 177.4(11) . . . . ? C36 C37 C38 C39 -3(2) . . . . ? C37 C38 C39 C40 5(2) . . . . ? C36 C35 C40 C39 -0.6(14) . . . . ? C36 C35 C40 C41 173.6(9) . . . . ? C38 C39 C40 C35 -2.6(17) . . . . ? C38 C39 C40 C41 -176.8(11) . . . . ? N11 N12 C41 C40 -82.0(10) . . . . ? C42 N12 C41 C40 92.5(11) . . . . ? C35 C40 C41 N12 143.0(9) . . . . ? C39 C40 C41 N12 -43.0(13) . . . . ? N11 N12 C42 C43 1.0(11) . . . . ? C41 N12 C42 C43 -174.0(8) . . . . ? N12 C42 C43 C44 -0.2(11) . . . . ? N12 N11 C44 C43 1.3(10) . . . . ? Yb2 N11 C44 C43 -175.6(6) . . . . ? N12 N11 C44 C45 179.5(8) . . . . ? Yb2 N11 C44 C45 2.5(10) . . . . ? C42 C43 C44 N11 -0.7(11) . . . . ? C42 C43 C44 C45 -178.7(9) . . . . ? C49 N10 C45 C46 0.0(13) . . . . ? Yb2 N10 C45 C46 -179.4(7) . . . . ? C49 N10 C45 C44 178.4(8) . . . . ? Yb2 N10 C45 C44 -0.9(11) . . . . ? N11 C44 C45 N10 -1.2(13) . . . . ? C43 C44 C45 N10 176.6(9) . . . . ? N11 C44 C45 C46 177.2(9) . . . . ? C43 C44 C45 C46 -5.0(15) . . . . ? N10 C45 C46 C47 -0.2(15) . . . . ? C44 C45 C46 C47 -178.6(10) . . . . ? C45 C46 C47 C48 -1.2(17) . . . . ? C46 C47 C48 C49 2.7(17) . . . . ? C45 N10 C49 C48 1.7(14) . . . . ? Yb2 N10 C49 C48 -179.0(7) . . . . ? C45 N10 C49 C50 -179.9(8) . . . . ? Yb2 N10 C49 C50 -0.6(10) . . . . ? C47 C48 C49 N10 -3.0(15) . . . . ? C47 C48 C49 C50 178.9(10) . . . . ? Yb2 O3 C50 N9 179.0(10) . . . . ? Yb2 O3 C50 C49 -3.4(17) . . . . ? C51 N9 C50 O3 -5(2) . . . . ? C53' N9 C50 O3 -141.4(17) . . . . ? C53 N9 C50 O3 160.2(13) . . . . ? C51 N9 C50 C49 177.6(12) . . . . ? C53' N9 C50 C49 41(2) . . . . ? C53 N9 C50 C49 -17(2) . . . . ? C51 N9 C50 Yb2 -4(3) . . . . ? C53' N9 C50 Yb2 -140.3(19) . . . . ? C53 N9 C50 Yb2 161.3(14) . . . . ? N10 C49 C50 O3 2.2(14) . . . . ? C48 C49 C50 O3 -179.5(11) . . . . ? N10 C49 C50 N9 179.7(12) . . . . ? C48 C49 C50 N9 -2.0(19) . . . . ? N10 C49 C50 Yb2 0.4(7) . . . . ? C48 C49 C50 Yb2 178.7(10) . . . . ? O1 Yb2 C50 O3 -104.3(12) . . . . ? O6 Yb2 C50 O3 19.7(18) . . . . ? O5 Yb2 C50 O3 110.7(12) . . . . ? N10 Yb2 C50 O3 -177.2(13) . . . . ? N2 Yb2 C50 O3 -38.4(12) . . . . ? N11 Yb2 C50 O3 -175.3(11) . . . . ? N3 Yb2 C50 O3 26.1(12) . . . . ? C16 Yb2 C50 O3 -85.8(12) . . . . ? O3 Yb2 C50 N9 -1.8(18) . . . . ? O1 Yb2 C50 N9 -106(2) . . . . ? O6 Yb2 C50 N9 18(3) . . . . ? O5 Yb2 C50 N9 109(2) . . . . ? N10 Yb2 C50 N9 -179(2) . . . . ? N2 Yb2 C50 N9 -40(2) . . . . ? N11 Yb2 C50 N9 -177(2) . . . . ? N3 Yb2 C50 N9 24(2) . . . . ? C16 Yb2 C50 N9 -88(2) . . . . ? O3 Yb2 C50 C49 176.9(15) . . . . ? O1 Yb2 C50 C49 72.6(6) . . . . ? O6 Yb2 C50 C49 -163.3(8) . . . . ? O5 Yb2 C50 C49 -72.3(6) . . . . ? N10 Yb2 C50 C49 -0.3(5) . . . . ? N2 Yb2 C50 C49 138.6(6) . . . . ? N11 Yb2 C50 C49 1.6(7) . . . . ? N3 Yb2 C50 C49 -156.9(6) . . . . ? C16 Yb2 C50 C49 91.1(6) . . . . ? C50 N9 C51 C52 88.1(19) . . . . ? C53' N9 C51 C52 -130.3(18) . . . . ? C53 N9 C51 C52 -78.4(19) . . . . ? C50 N9 C53 C54 103.1(19) . . . . ? C51 N9 C53 C54 -91.6(19) . . . . ? C53' N9 C53 C54 0(2) . . . . ? C50 N9 C53' C54' -135(2) . . . . ? C51 N9 C53' C54' 86(3) . . . . ? C53 N9 C53' C54' -23.4(19) . . . . ? C56 N13 C55 C36 -84.5(11) . . . . ? N14 N13 C55 C36 93.7(10) . . . . ? C37 C36 C55 N13 117.1(10) . . . . ? C35 C36 C55 N13 -65.8(11) . . . . ? N14 N13 C56 C57 0.5(12) . . . . ? C55 N13 C56 C57 178.9(9) . . . . ? N13 C56 C57 C58 -1.1(12) . . . . ? N13 N14 C58 C57 -1.0(10) . . . . ? Yb1 N14 C58 C57 173.5(7) . . . . ? N13 N14 C58 C59 -179.9(8) . . . . ? Yb1 N14 C58 C59 -5.3(10) . . . . ? C56 C57 C58 N14 1.4(12) . . . . ? C56 C57 C58 C59 -179.9(9) . . . . ? C63 N15 C59 C60 0.7(14) . . . . ? Yb1 N15 C59 C60 -177.0(8) . . . . ? C63 N15 C59 C58 178.8(8) . . . . ? Yb1 N15 C59 C58 1.1(11) . . . . ? N14 C58 C59 N15 3.1(12) . . . . ? C57 C58 C59 N15 -175.5(10) . . . . ? N14 C58 C59 C60 -178.7(9) . . . . ? C57 C58 C59 C60 2.7(16) . . . . ? N15 C59 C60 C61 -2.7(17) . . . . ? C58 C59 C60 C61 179.2(12) . . . . ? C59 C60 C61 C62 4(2) . . . . ? C60 C61 C62 C63 -3(2) . . . . ? C59 N15 C63 C62 0.2(14) . . . . ? Yb1 N15 C63 C62 178.0(9) . . . . ? C59 N15 C63 C64 -173.9(8) . . . . ? Yb1 N15 C63 C64 3.9(10) . . . . ? C61 C62 C63 N15 1(2) . . . . ? C61 C62 C63 C64 174.1(13) . . . . ? Yb1 O4 C64 N16 179.9(9) . . . . ? Yb1 O4 C64 C63 -1.0(13) . . . . ? C67 N16 C64 O4 5.6(18) . . . . ? C65 N16 C64 O4 149.2(15) . . . . ? C65' N16 C64 O4 -138.6(15) . . . . ? C67 N16 C64 C63 -173.5(11) . . . . ? C65 N16 C64 C63 -30(2) . . . . ? C65' N16 C64 C63 42.3(19) . . . . ? C67 N16 C64 Yb1 6(3) . . . . ? C65 N16 C64 Yb1 149.4(16) . . . . ? C65' N16 C64 Yb1 -138.4(19) . . . . ? N15 C63 C64 O4 -2.1(13) . . . . ? C62 C63 C64 O4 -175.7(11) . . . . ? N15 C63 C64 N16 177.0(11) . . . . ? C62 C63 C64 N16 3.4(19) . . . . ? N15 C63 C64 Yb1 -2.7(7) . . . . ? C62 C63 C64 Yb1 -176.3(11) . . . . ? O2 Yb1 C64 O4 -104.8(8) . . . . ? O7 Yb1 C64 O4 109.2(8) . . . . ? O10 Yb1 C64 O4 7.3(17) . . . . ? N15 Yb1 C64 O4 -177.3(10) . . . . ? N7 Yb1 C64 O4 -39.2(8) . . . . ? N6 Yb1 C64 O4 26.4(8) . . . . ? N14 Yb1 C64 O4 -175.4(8) . . . . ? C30 Yb1 C64 O4 -86.9(8) . . . . ? O2 Yb1 C64 N16 -105(2) . . . . ? O7 Yb1 C64 N16 109(2) . . . . ? O4 Yb1 C64 N16 -0.3(16) . . . . ? O10 Yb1 C64 N16 7(3) . . . . ? N15 Yb1 C64 N16 -178(2) . . . . ? N7 Yb1 C64 N16 -39(2) . . . . ? N6 Yb1 C64 N16 26(2) . . . . ? N14 Yb1 C64 N16 -175.7(19) . . . . ? C30 Yb1 C64 N16 -87(2) . . . . ? O2 Yb1 C64 C63 74.4(6) . . . . ? O7 Yb1 C64 C63 -71.6(6) . . . . ? O4 Yb1 C64 C63 179.1(12) . . . . ? O10 Yb1 C64 C63 -173.6(10) . . . . ? N15 Yb1 C64 C63 1.8(5) . . . . ? N7 Yb1 C64 C63 140.0(6) . . . . ? N6 Yb1 C64 C63 -154.5(6) . . . . ? N14 Yb1 C64 C63 3.7(6) . . . . ? C30 Yb1 C64 C63 92.2(6) . . . . ? C64 N16 C65 C66 113.9(19) . . . . ? C67 N16 C65 C66 -98.8(18) . . . . ? C65' N16 C65 C66 14.9(19) . . . . ? C64 N16 C65' C66' -135(2) . . . . ? C67 N16 C65' C66' 81(2) . . . . ? C65 N16 C65' C66' -13(2) . . . . ? C64 N16 C67 C68 79.6(19) . . . . ? C65 N16 C67 C68 -71.4(18) . . . . ? C65' N16 C67 C68 -137.8(18) . . . . ? Yb1 O7 C100 O6 158.3(6) . . . . ? Yb2 O6 C100 O7 172.7(6) . . . . ? O12 Cl1 O10 Yb1 174.4(8) . . . . ? O13 Cl1 O10 Yb1 -64.0(9) . . . . ? O11 Cl1 O10 Yb1 54.4(9) . . . . ? O2 Yb1 O10 Cl1 142.6(8) . . . . ? O7 Yb1 O10 Cl1 -71.7(8) . . . . ? O4 Yb1 O10 Cl1 35.2(10) . . . . ? N15 Yb1 O10 Cl1 -143.3(7) . . . . ? N7 Yb1 O10 Cl1 78.2(8) . . . . ? N6 Yb1 O10 Cl1 11.2(7) . . . . ? N14 Yb1 O10 Cl1 -146.7(8) . . . . ? C30 Yb1 O10 Cl1 125.3(8) . . . . ? C64 Yb1 O10 Cl1 30.8(17) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.403 _refine_diff_density_min -2.175 _refine_diff_density_rms 0.159 #===END data_imw739 _database_code_depnum_ccdc_archive 'CCDC 630969' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H98 Cl5 La2 N21 O39' _chemical_formula_weight 2360.80 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' La La -0.2871 2.4523 '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 15.3123(12) _cell_length_b 18.8994(16) _cell_length_c 34.341(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.066(5) _cell_angle_gamma 90.00 _cell_volume 9862.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8157 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 25.68 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4800 _exptl_absorpt_coefficient_mu 1.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7294 _exptl_absorpt_correction_T_max 0.9578 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'BRUKER SMART 4000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93382 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0726 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17276 _reflns_number_gt 11904 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0730P)^2^+158.2698P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17276 _refine_ls_number_parameters 1190 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.1284 _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.2343 _refine_ls_wR_factor_gt 0.1987 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.16152(4) 0.07691(3) 0.395049(17) 0.02123(16) Uani 1 1 d . . . La2 La 0.19730(4) 0.44233(3) 0.409242(19) 0.02917(18) Uani 1 1 d . . . O1 O 0.2773(4) -0.0002(3) 0.4250(2) 0.0258(16) Uani 1 1 d . . . O2 O 0.2628(6) 0.5193(4) 0.3624(3) 0.046(2) Uani 1 1 d . B . O3 O 0.0505(4) 0.0981(4) 0.3356(2) 0.0279(16) Uani 1 1 d . . . O4 O 0.0742(5) 0.4246(4) 0.3544(2) 0.0352(18) Uani 1 1 d . B . O5 O 0.2235(5) 0.3968(4) 0.4795(2) 0.0336(18) Uani 1 1 d . B . O6 O 0.1822(4) 0.1134(4) 0.4670(2) 0.0263(16) Uani 1 1 d . . . O7 O 0.1538(5) 0.3188(4) 0.4110(2) 0.0304(17) Uani 1 1 d . B . O8 O 0.1410(5) 0.2041(4) 0.3973(2) 0.0290(17) Uani 1 1 d . B . N1 N 0.3336(5) -0.1087(4) 0.4359(3) 0.030(2) Uani 1 1 d . . . N2 N 0.1186(5) -0.0367(4) 0.4357(2) 0.0256(19) Uani 1 1 d . . . N3 N -0.0079(5) 0.0657(4) 0.4121(2) 0.0246(19) Uani 1 1 d . . . N4 N -0.0858(5) 0.0953(4) 0.3973(3) 0.0256(19) Uani 1 1 d . . . N5 N -0.0155(6) 0.4418(4) 0.4558(3) 0.030(2) Uani 1 1 d . . . N6 N 0.0416(6) 0.4739(5) 0.4346(2) 0.028(2) Uani 1 1 d . B . N7 N 0.1286(6) 0.5715(5) 0.3920(3) 0.033(2) Uani 1 1 d . B . N9 N 0.0174(6) 0.0499(5) 0.2755(3) 0.030(2) Uani 1 1 d . . . N8 N 0.3186(7) 0.6222(5) 0.3469(3) 0.050(3) Uani 1 1 d . . . N10 N 0.2185(5) 0.1155(4) 0.3254(2) 0.0253(19) Uani 1 1 d . . . N11 N 0.3306(5) 0.1296(4) 0.3941(2) 0.0241(19) Uani 1 1 d . . . N12 N 0.4043(5) 0.1284(4) 0.4202(3) 0.027(2) Uani 1 1 d . . . N13 N 0.4382(6) 0.3882(5) 0.4326(3) 0.034(2) Uani 1 1 d . . . N14 N 0.3648(6) 0.3873(5) 0.4070(3) 0.034(2) Uani 1 1 d . B . N15 N 0.2367(6) 0.3764(5) 0.3450(3) 0.035(2) Uani 1 1 d . B . N16 N 0.0147(7) 0.3345(5) 0.3175(3) 0.042(3) Uani 1 1 d . . . C1 C -0.0505(7) 0.2680(5) 0.4276(3) 0.026(2) Uani 1 1 d . B . H1 H 0.0075 0.2654 0.4205 0.031 Uiso 1 1 calc R . . C2 C -0.0698(7) 0.3186(5) 0.4546(3) 0.029(2) Uani 1 1 d . . . C3 C -0.1542(9) 0.3205(6) 0.4659(4) 0.044(3) Uani 1 1 d . B . H3 H -0.1681 0.3537 0.4850 0.052 Uiso 1 1 calc R . . C4 C -0.2176(8) 0.2733(6) 0.4492(4) 0.046(3) Uani 1 1 d . . . H4 H -0.2749 0.2742 0.4570 0.056 Uiso 1 1 calc R B . C5 C -0.1987(7) 0.2259(5) 0.4218(4) 0.034(3) Uani 1 1 d . B . H5 H -0.2438 0.1956 0.4099 0.041 Uiso 1 1 calc R . . C6 C -0.1148(6) 0.2208(5) 0.4107(3) 0.025(2) Uani 1 1 d . . . C7 C -0.0922(7) 0.1673(5) 0.3817(3) 0.030(2) Uani 1 1 d . B . H7A H -0.1377 0.1684 0.3586 0.036 Uiso 1 1 calc R . . H7B H -0.0353 0.1804 0.3728 0.036 Uiso 1 1 calc R . . C8 C -0.1545(6) 0.0535(5) 0.4033(3) 0.028(2) Uani 1 1 d . . . H8 H -0.2149 0.0631 0.3952 0.033 Uiso 1 1 calc R . . C9 C -0.1213(7) -0.0047(5) 0.4231(3) 0.029(2) Uani 1 1 d . . . H9 H -0.1534 -0.0435 0.4317 0.034 Uiso 1 1 calc R . . C10 C -0.0306(6) 0.0042(5) 0.4282(3) 0.024(2) Uani 1 1 d . . . C11 C 0.0362(7) -0.0434(5) 0.4464(3) 0.026(2) Uani 1 1 d . . . C12 C 0.0185(7) -0.0943(6) 0.4733(3) 0.035(3) Uani 1 1 d . . . H12 H -0.0396 -0.0996 0.4799 0.042 Uiso 1 1 calc R . . C13 C 0.0850(7) -0.1373(6) 0.4906(3) 0.035(3) Uani 1 1 d . . . H13 H 0.0740 -0.1710 0.5099 0.042 Uiso 1 1 calc R . . C14 C 0.1682(7) -0.1301(6) 0.4792(3) 0.029(2) Uani 1 1 d . . . H14 H 0.2153 -0.1590 0.4906 0.035 Uiso 1 1 calc R . . C15 C 0.1819(6) -0.0804(5) 0.4511(3) 0.025(2) Uani 1 1 d . . . C16 C 0.2689(7) -0.0631(5) 0.4365(3) 0.027(2) Uani 1 1 d . . . C17 C 0.3292(7) -0.1856(6) 0.4423(4) 0.037(3) Uani 1 1 d . . . H17A H 0.3552 -0.2104 0.4211 0.044 Uiso 1 1 calc R . . H17B H 0.2669 -0.2002 0.4410 0.044 Uiso 1 1 calc R . . C18 C 0.3779(7) -0.2073(6) 0.4817(4) 0.038(3) Uani 1 1 d . . . H18A H 0.4410 -0.1987 0.4818 0.057 Uiso 1 1 calc R . . H18B H 0.3679 -0.2577 0.4861 0.057 Uiso 1 1 calc R . . H18C H 0.3561 -0.1795 0.5026 0.057 Uiso 1 1 calc R . . C19 C 0.4171(7) -0.0827(6) 0.4234(4) 0.039(3) Uani 1 1 d . . . H19A H 0.4655 -0.1150 0.4336 0.047 Uiso 1 1 calc R . . H19B H 0.4305 -0.0353 0.4349 0.047 Uiso 1 1 calc R . . C20 C 0.4133(9) -0.0779(8) 0.3797(4) 0.058(4) Uani 1 1 d . . . H20A H 0.4043 -0.1253 0.3683 0.087 Uiso 1 1 calc R . . H20B H 0.4686 -0.0582 0.3729 0.087 Uiso 1 1 calc R . . H20C H 0.3643 -0.0472 0.3694 0.087 Uiso 1 1 calc R . . C21 C 0.0001(7) 0.3697(6) 0.4716(3) 0.032(3) Uani 1 1 d . B . H21A H 0.0015 0.3709 0.5005 0.039 Uiso 1 1 calc R . . H21B H 0.0583 0.3529 0.4656 0.039 Uiso 1 1 calc R . . C22 C -0.0837(8) 0.4846(6) 0.4601(4) 0.040(3) Uani 1 1 d . B . H22 H -0.1319 0.4733 0.4739 0.049 Uiso 1 1 calc R . . C23 C -0.0723(7) 0.5466(6) 0.4414(3) 0.035(3) Uani 1 1 d . . . H23 H -0.1105 0.5864 0.4392 0.042 Uiso 1 1 calc R B . C24 C 0.0070(7) 0.5393(5) 0.4261(3) 0.027(2) Uani 1 1 d . B . C25 C 0.0498(7) 0.5899(5) 0.4035(3) 0.030(2) Uani 1 1 d . . . C26 C 0.0131(9) 0.6556(6) 0.3937(4) 0.043(3) Uani 1 1 d . B . H26 H -0.0404 0.6691 0.4029 0.052 Uiso 1 1 calc R . . C27 C 0.0534(9) 0.7005(7) 0.3708(4) 0.049(3) Uani 1 1 d . . . H27 H 0.0273 0.7448 0.3631 0.059 Uiso 1 1 calc R B . C28 C 0.1335(9) 0.6810(6) 0.3589(4) 0.046(3) Uani 1 1 d . B . H28 H 0.1628 0.7119 0.3430 0.056 Uiso 1 1 calc R . . C29 C 0.1706(8) 0.6158(5) 0.3704(3) 0.033(3) Uani 1 1 d . . . C30 C 0.2543(9) 0.5849(6) 0.3593(3) 0.041(3) Uani 1 1 d . B . C31 C 0.3278(10) 0.7014(8) 0.3493(5) 0.066(4) Uani 1 1 d . . . H31A H 0.2846 0.7206 0.3657 0.079 Uiso 1 1 calc R . . H31B H 0.3874 0.7136 0.3620 0.079 Uiso 1 1 calc R . . C32 C 0.3132(11) 0.7354(8) 0.3094(5) 0.070(5) Uani 1 1 d . . . H32A H 0.3600 0.7208 0.2940 0.104 Uiso 1 1 calc R . . H32B H 0.3140 0.7870 0.3123 0.104 Uiso 1 1 calc R . . H32C H 0.2560 0.7206 0.2959 0.104 Uiso 1 1 calc R . . C33 C 0.3955(10) 0.5848(8) 0.3344(4) 0.061(4) Uiso 1 1 d . . . H33A H 0.3750 0.5399 0.3214 0.073 Uiso 1 1 calc R . . H33B H 0.4207 0.6142 0.3147 0.073 Uiso 1 1 calc R . . C34 C 0.4635(16) 0.5690(14) 0.3657(7) 0.132(9) Uiso 1 1 d . . . H34A H 0.4838 0.6130 0.3790 0.197 Uiso 1 1 calc R . . H34B H 0.5129 0.5461 0.3551 0.197 Uiso 1 1 calc R . . H34C H 0.4403 0.5372 0.3845 0.197 Uiso 1 1 calc R . . C35 C 0.4126(7) 0.2544(6) 0.4670(3) 0.033(3) Uani 1 1 d . B . H35 H 0.4192 0.2577 0.4399 0.039 Uiso 1 1 calc R . . C36 C 0.4183(7) 0.3157(6) 0.4912(4) 0.035(3) Uani 1 1 d . . . C37 C 0.4085(7) 0.3110(6) 0.5299(3) 0.033(3) Uani 1 1 d . B . H37 H 0.4134 0.3526 0.5456 0.040 Uiso 1 1 calc R . . C38 C 0.3914(7) 0.2473(6) 0.5468(4) 0.033(3) Uani 1 1 d . . . H38 H 0.3836 0.2449 0.5738 0.040 Uiso 1 1 calc R B . C39 C 0.3859(6) 0.1869(6) 0.5240(3) 0.031(3) Uani 1 1 d . B . H39 H 0.3743 0.1428 0.5356 0.037 Uiso 1 1 calc R . . C40 C 0.3971(6) 0.1896(6) 0.4840(3) 0.028(2) Uani 1 1 d . . . C41 C 0.4004(7) 0.1205(5) 0.4622(3) 0.028(2) Uani 1 1 d . B . H41A H 0.4526 0.0935 0.4738 0.034 Uiso 1 1 calc R . . H41B H 0.3475 0.0923 0.4660 0.034 Uiso 1 1 calc R . . C42 C 0.4788(7) 0.1379(6) 0.4032(4) 0.035(3) Uani 1 1 d . . . H42 H 0.5373 0.1383 0.4161 0.043 Uiso 1 1 calc R . . C43 C 0.4534(8) 0.1470(6) 0.3641(4) 0.038(3) Uani 1 1 d . . . H43 H 0.4902 0.1554 0.3442 0.045 Uiso 1 1 calc R . . C44 C 0.3616(7) 0.1412(6) 0.3596(3) 0.029(2) Uani 1 1 d . . . C45 C 0.2978(7) 0.1429(5) 0.3234(3) 0.030(2) Uani 1 1 d . . . C46 C 0.3222(8) 0.1689(6) 0.2884(3) 0.036(3) Uani 1 1 d . . . H46 H 0.3804 0.1852 0.2870 0.044 Uiso 1 1 calc R . . C47 C 0.2600(9) 0.1703(6) 0.2559(4) 0.042(3) Uani 1 1 d . . . H47 H 0.2740 0.1900 0.2320 0.051 Uiso 1 1 calc R . . C48 C 0.1767(8) 0.1431(6) 0.2582(3) 0.034(3) Uani 1 1 d . . . H48 H 0.1330 0.1441 0.2360 0.041 Uiso 1 1 calc R . . C49 C 0.1585(7) 0.1142(6) 0.2933(3) 0.029(2) Uani 1 1 d . . . C50 C 0.0712(7) 0.0864(5) 0.3016(3) 0.028(2) Uani 1 1 d . . . C51 C 0.0395(9) 0.0228(6) 0.2388(3) 0.042(3) Uani 1 1 d . . . H51A H 0.0293 -0.0289 0.2381 0.050 Uiso 1 1 calc R . . H51B H 0.1030 0.0308 0.2376 0.050 Uiso 1 1 calc R . . C52 C -0.0119(9) 0.0556(7) 0.2034(3) 0.048(3) Uani 1 1 d . . . H52A H -0.0745 0.0444 0.2032 0.073 Uiso 1 1 calc R . . H52B H 0.0090 0.0367 0.1796 0.073 Uiso 1 1 calc R . . H52C H -0.0038 0.1070 0.2043 0.073 Uiso 1 1 calc R . . C53 C -0.0684(8) 0.0284(7) 0.2869(4) 0.043(3) Uani 1 1 d . . . H53A H -0.0605 0.0146 0.3149 0.052 Uiso 1 1 calc R . . H53B H -0.0896 -0.0137 0.2714 0.052 Uiso 1 1 calc R . . C54 C -0.1371(8) 0.0857(8) 0.2807(4) 0.055(4) Uani 1 1 d . . . H54A H -0.1175 0.1270 0.2967 0.082 Uiso 1 1 calc R . . H54B H -0.1927 0.0682 0.2885 0.082 Uiso 1 1 calc R . . H54C H -0.1459 0.0993 0.2530 0.082 Uiso 1 1 calc R . . C55 C 0.4370(8) 0.3884(6) 0.4739(3) 0.038(3) Uani 1 1 d . B . H55A H 0.3915 0.4222 0.4804 0.046 Uiso 1 1 calc R . . H55B H 0.4946 0.4056 0.4866 0.046 Uiso 1 1 calc R . . C56 C 0.5098(9) 0.3788(7) 0.4132(4) 0.051(3) Uani 1 1 d . B . H56 H 0.5695 0.3779 0.4247 0.061 Uiso 1 1 calc R . . C57 C 0.4807(8) 0.3709(8) 0.3747(4) 0.050(3) Uani 1 1 d . . . H57 H 0.5150 0.3625 0.3539 0.061 Uiso 1 1 calc R B . C58 C 0.3879(8) 0.3778(6) 0.3720(3) 0.037(3) Uani 1 1 d . B . C59 C 0.3206(8) 0.3735(5) 0.3374(3) 0.036(3) Uani 1 1 d . . . C60 C 0.3433(9) 0.3636(6) 0.2992(3) 0.044(3) Uani 1 1 d . B . H60 H 0.4029 0.3603 0.2943 0.052 Uiso 1 1 calc R . . C61 C 0.2750(9) 0.3592(7) 0.2696(4) 0.046(3) Uani 1 1 d . . . H61 H 0.2881 0.3558 0.2433 0.056 Uiso 1 1 calc R B . C62 C 0.1857(10) 0.3595(7) 0.2765(4) 0.049(3) Uani 1 1 d . B . H62 H 0.1390 0.3537 0.2558 0.059 Uiso 1 1 calc R . . C63 C 0.1704(9) 0.3689(6) 0.3159(3) 0.036(3) Uani 1 1 d . . . C64 C 0.0819(8) 0.3763(6) 0.3296(3) 0.036(3) Uani 1 1 d . B . C65 C 0.0236(9) 0.2694(6) 0.2943(4) 0.044(3) Uani 1 1 d . . . H65A H 0.0101 0.2277 0.3100 0.052 Uiso 1 1 calc R . . H65B H 0.0853 0.2650 0.2887 0.052 Uiso 1 1 calc R . . C66 C -0.0376(10) 0.2697(7) 0.2556(4) 0.051(4) Uani 1 1 d . . . H66A H -0.0983 0.2778 0.2609 0.077 Uiso 1 1 calc R . . H66B H -0.0339 0.2240 0.2425 0.077 Uiso 1 1 calc R . . H66C H -0.0199 0.3075 0.2387 0.077 Uiso 1 1 calc R . . C67 C -0.0675(9) 0.3419(7) 0.3355(4) 0.046(3) Uani 1 1 d . . . H67A H -0.0523 0.3546 0.3634 0.055 Uiso 1 1 calc R . . H67B H -0.0974 0.2954 0.3345 0.055 Uiso 1 1 calc R . . C68 C -0.1317(9) 0.3965(8) 0.3163(4) 0.054(4) Uani 1 1 d . . . H68A H -0.1058 0.4438 0.3201 0.081 Uiso 1 1 calc R . . H68B H -0.1865 0.3945 0.3283 0.081 Uiso 1 1 calc R . . H68C H -0.1442 0.3865 0.2882 0.081 Uiso 1 1 calc R . . C100 C 0.1831(7) 0.2590(5) 0.4062(3) 0.029(2) Uani 1 1 d . . . H100 H 0.2453 0.2545 0.4097 0.035 Uiso 1 1 calc R B . Cl1 Cl 0.13720(19) -0.09916(14) 0.33591(9) 0.0391(7) Uani 1 1 d . . . O10 O 0.1655(6) -0.0288(4) 0.3486(2) 0.042(2) Uani 1 1 d . . . O11 O 0.0467(7) -0.1062(7) 0.3388(4) 0.096(4) Uani 1 1 d . . . O12 O 0.1551(9) -0.1062(6) 0.2970(3) 0.086(4) Uani 1 1 d . . . O13 O 0.1861(6) -0.1486(4) 0.3615(3) 0.060(3) Uani 1 1 d . . . O18 O 0.6777(5) 0.0873(4) 0.4461(2) 0.0373(19) Uani 1 1 d . . . O19 O 0.5802(5) 0.0141(4) 0.4754(3) 0.046(2) Uani 1 1 d . . . O20 O 0.7296(5) -0.0118(4) 0.4824(2) 0.0349(18) Uani 1 1 d . . . O21 O 0.6461(6) -0.0258(5) 0.4216(2) 0.056(2) Uani 1 1 d . . . Cl4 Cl 0.65699(16) 0.01558(13) 0.45621(8) 0.0284(6) Uani 1 1 d . . . Cl3 Cl 0.4321(2) 0.22371(19) 0.69355(11) 0.0543(9) Uani 1 1 d D . . O23 O 0.3403(6) 0.2087(6) 0.6860(3) 0.074(3) Uani 1 1 d . A . O22 O 0.466(2) 0.1746(15) 0.7244(9) 0.085(6) Uiso 0.37(3) 1 d PDU A 1 O24 O 0.450(2) 0.2956(10) 0.7089(9) 0.068(6) Uiso 0.37(3) 1 d PDU A 1 O25 O 0.478(2) 0.215(2) 0.6599(7) 0.075(6) Uiso 0.37(3) 1 d PDU A 1 O22' O 0.4864(13) 0.1638(8) 0.7078(7) 0.083(5) Uiso 0.63(3) 1 d PDU A 2 O24' O 0.4439(14) 0.2812(9) 0.7207(5) 0.071(4) Uiso 0.63(3) 1 d PDU A 2 O25' O 0.4571(14) 0.2450(12) 0.6552(4) 0.071(5) Uiso 0.63(3) 1 d PDU A 2 Cl5 Cl 0.15175(16) 0.25238(12) 0.03555(7) 0.0256(6) Uani 1 1 d . . . O26 O 0.1822(5) 0.3206(4) 0.0497(2) 0.0335(18) Uani 1 1 d . . . O27 O 0.0585(5) 0.2464(4) 0.0357(2) 0.0358(19) Uani 1 1 d . . . O28 O 0.1732(5) 0.2439(4) -0.0041(2) 0.0319(18) Uani 1 1 d . . . O29 O 0.1944(5) 0.1971(4) 0.0596(2) 0.0370(19) Uani 1 1 d . . . O1S O 0.1807(14) 0.0950(11) 0.1625(6) 0.153(7) Uiso 1 1 d . . . O2S O 0.2445(11) 0.0275(10) 0.1218(5) 0.133(6) Uiso 1 1 d . . . N1S N 0.2431(15) 0.0840(12) 0.1463(6) 0.129(7) Uiso 1 1 d . . . C1S C 0.3085(13) 0.1319(11) 0.1418(6) 0.093(6) Uiso 1 1 d . . . H1S1 H 0.3086 0.1425 0.1139 0.139 Uiso 1 1 calc R . . H1S2 H 0.3655 0.1118 0.1524 0.139 Uiso 1 1 calc R . . H1S3 H 0.2980 0.1754 0.1560 0.139 Uiso 1 1 calc R . . O3S O 0.1226(7) 0.2838(6) 0.1915(3) 0.071(3) Uani 1 1 d . . . O4S O 0.1676(6) 0.3927(6) 0.1865(3) 0.059(3) Uani 1 1 d . . . N2S N 0.1487(7) 0.3334(6) 0.1723(3) 0.049(3) Uani 1 1 d . . . C2S C 0.1540(11) 0.3243(9) 0.1315(4) 0.066(4) Uani 1 1 d . . . H2S1 H 0.1012 0.3441 0.1163 0.099 Uiso 1 1 calc R . . H2S2 H 0.1583 0.2738 0.1256 0.099 Uiso 1 1 calc R . . H2S3 H 0.2062 0.3489 0.1244 0.099 Uiso 1 1 calc R . . C3S C 0.6614(11) 0.4037(9) 0.8333(5) 0.072(5) Uiso 1 1 d . . . H3S1 H 0.6775 0.4140 0.8612 0.109 Uiso 1 1 calc R . . H3S2 H 0.7150 0.3977 0.8206 0.109 Uiso 1 1 calc R . . H3S3 H 0.6265 0.3602 0.8304 0.109 Uiso 1 1 calc R . . O5S O 0.5447(12) 0.4449(10) 0.7914(5) 0.141(6) Uiso 1 1 d . . . O6S O 0.6378(12) 0.5277(11) 0.8261(5) 0.147(6) Uiso 1 1 d . . . N3S N 0.6167(14) 0.4546(11) 0.8172(6) 0.118(6) Uiso 1 1 d . . . N4S N 0.3762(16) 0.9677(15) 0.2291(7) 0.143(8) Uiso 1 1 d . . . O8S O 0.4030(14) 0.9247(12) 0.2086(6) 0.159(7) Uiso 1 1 d . . . C4S C 0.3557(14) 0.9493(11) 0.2676(6) 0.097(6) Uiso 1 1 d . . . H4S1 H 0.2946 0.9329 0.2658 0.146 Uiso 1 1 calc R . . H4S2 H 0.3631 0.9910 0.2847 0.146 Uiso 1 1 calc R . . H4S3 H 0.3953 0.9117 0.2786 0.146 Uiso 1 1 calc R . . O7S O 0.327(2) 1.0192(17) 0.2150(9) 0.236(12) Uiso 1 1 d . . . O1W O 0.2958(7) 0.4682(5) 0.5465(3) 0.071(3) Uani 1 1 d . . . O9S O 0.7482(11) 0.2654(8) 0.8016(4) 0.112(5) Uiso 1 1 d D . . C5S C 0.5950(11) 0.2575(9) 0.7885(5) 0.076(5) Uiso 1 1 d D . . H5S1 H 0.5820 0.3047 0.7776 0.114 Uiso 1 1 calc R . . H5S2 H 0.5498 0.2440 0.8050 0.114 Uiso 1 1 calc R . . H5S3 H 0.5956 0.2232 0.7671 0.114 Uiso 1 1 calc R . . N5S N 0.6751(14) 0.2581(9) 0.8106(6) 0.117(6) Uiso 1 1 d D . . O10S O 0.6739(18) 0.2255(14) 0.8435(8) 0.222(11) Uiso 1 1 d D . . Cl2 Cl 0.3093(3) 0.5846(2) 0.46602(11) 0.0760(13) Uani 1 1 d D . . O17 O 0.3436(6) 0.5969(5) 0.5049(3) 0.052(2) Uani 1 1 d . B . O16 O 0.2858(7) 0.6475(5) 0.4457(3) 0.068(3) Uani 1 1 d . B . O14 O 0.3365(10) 0.5257(7) 0.4430(4) 0.051(3) Uiso 0.549(11) 1 d PDU B 1 O15 O 0.2139(9) 0.5520(8) 0.4717(5) 0.049(3) Uiso 0.549(11) 1 d PDU B 1 O14' O 0.3990(11) 0.5718(11) 0.4502(6) 0.062(5) Uiso 0.451(11) 1 d PDU B 2 O15' O 0.2709(11) 0.5178(8) 0.4567(5) 0.050(3) Uiso 0.451(11) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0219(3) 0.0140(3) 0.0283(3) 0.0004(2) 0.0049(2) 0.0005(2) La2 0.0381(4) 0.0146(3) 0.0353(4) 0.0023(3) 0.0069(3) 0.0056(3) O1 0.019(4) 0.016(4) 0.043(4) 0.007(3) 0.006(3) 0.001(3) O2 0.055(6) 0.020(5) 0.068(6) 0.007(4) 0.024(5) 0.009(4) O3 0.028(4) 0.024(4) 0.033(4) 0.000(3) 0.009(3) 0.005(3) O4 0.044(5) 0.025(4) 0.035(4) -0.001(3) 0.000(4) 0.003(3) O5 0.039(4) 0.023(4) 0.039(4) 0.003(3) 0.009(4) 0.004(3) O6 0.027(4) 0.020(4) 0.032(4) -0.001(3) 0.004(3) 0.001(3) O7 0.034(4) 0.016(4) 0.042(4) 0.002(3) 0.010(3) 0.003(3) O8 0.030(4) 0.018(4) 0.040(4) -0.005(3) 0.008(3) -0.001(3) N1 0.023(5) 0.018(5) 0.050(6) -0.003(4) 0.009(4) 0.001(4) N2 0.027(5) 0.022(5) 0.026(5) 0.002(4) -0.002(4) -0.001(4) N3 0.024(4) 0.024(5) 0.026(5) 0.004(4) 0.002(4) 0.000(4) N4 0.024(5) 0.016(4) 0.038(5) 0.001(4) 0.007(4) 0.003(3) N5 0.030(5) 0.014(4) 0.047(6) -0.002(4) 0.009(4) 0.004(4) N6 0.036(5) 0.023(5) 0.026(5) 0.000(4) 0.003(4) 0.004(4) N7 0.044(6) 0.021(5) 0.032(5) -0.005(4) 0.001(4) -0.003(4) N9 0.037(5) 0.024(5) 0.029(5) -0.003(4) 0.000(4) -0.003(4) N8 0.048(7) 0.025(6) 0.082(8) 0.010(5) 0.028(6) 0.002(5) N10 0.021(5) 0.021(5) 0.034(5) -0.002(4) 0.005(4) 0.000(4) N11 0.022(5) 0.019(5) 0.030(5) 0.000(4) 0.001(4) 0.001(3) N12 0.024(5) 0.021(5) 0.037(5) 0.003(4) 0.006(4) 0.001(4) N13 0.034(6) 0.023(5) 0.046(6) 0.002(4) 0.008(5) 0.000(4) N14 0.046(6) 0.017(5) 0.043(6) 0.004(4) 0.014(5) 0.003(4) N15 0.041(6) 0.019(5) 0.046(6) 0.001(4) 0.013(5) 0.003(4) N16 0.057(7) 0.036(6) 0.033(6) 0.004(4) -0.001(5) 0.009(5) C1 0.023(6) 0.020(5) 0.036(6) 0.015(4) 0.005(5) 0.005(4) C2 0.039(7) 0.012(5) 0.039(6) 0.009(4) 0.012(5) 0.007(4) C3 0.059(8) 0.017(6) 0.058(8) -0.001(5) 0.022(7) -0.004(5) C4 0.034(7) 0.027(7) 0.083(10) 0.003(6) 0.024(7) 0.010(5) C5 0.020(6) 0.016(6) 0.067(8) 0.006(5) 0.006(5) 0.003(4) C6 0.020(5) 0.018(5) 0.039(6) 0.008(4) 0.008(4) 0.002(4) C7 0.029(6) 0.022(6) 0.039(7) 0.008(5) 0.004(5) 0.008(4) C8 0.014(5) 0.020(5) 0.050(7) 0.001(5) 0.007(5) 0.000(4) C9 0.025(6) 0.020(6) 0.044(7) 0.001(5) 0.015(5) -0.004(4) C10 0.023(5) 0.020(5) 0.030(6) 0.000(4) 0.005(4) -0.003(4) C11 0.023(5) 0.014(5) 0.041(6) -0.003(4) 0.003(5) -0.003(4) C12 0.030(6) 0.021(6) 0.054(7) 0.005(5) 0.008(5) -0.011(5) C13 0.026(6) 0.029(6) 0.049(7) 0.013(5) 0.000(5) -0.007(5) C14 0.024(6) 0.027(6) 0.034(6) 0.010(5) -0.009(5) -0.006(4) C15 0.023(5) 0.013(5) 0.037(6) -0.002(4) 0.000(4) -0.007(4) C16 0.027(6) 0.024(6) 0.030(6) 0.000(4) -0.001(4) 0.000(4) C17 0.029(6) 0.017(6) 0.064(8) -0.006(5) 0.010(6) 0.001(5) C18 0.026(6) 0.025(6) 0.061(8) 0.006(5) 0.000(5) 0.004(5) C19 0.022(6) 0.026(6) 0.071(9) -0.002(6) 0.009(6) 0.001(5) C20 0.049(8) 0.052(9) 0.078(11) -0.006(7) 0.035(8) -0.008(7) C21 0.038(7) 0.023(6) 0.034(6) 0.001(5) -0.003(5) 0.003(5) C22 0.036(7) 0.023(6) 0.064(8) -0.002(6) 0.011(6) 0.001(5) C23 0.033(6) 0.017(6) 0.054(8) -0.002(5) -0.003(5) -0.001(5) C24 0.031(6) 0.014(5) 0.036(6) -0.003(4) -0.004(5) 0.000(4) C25 0.038(6) 0.020(6) 0.031(6) -0.003(4) 0.005(5) 0.005(5) C26 0.051(8) 0.024(7) 0.059(8) 0.001(6) 0.023(6) 0.001(5) C27 0.060(9) 0.028(7) 0.064(9) 0.007(6) 0.027(7) 0.011(6) C28 0.055(8) 0.026(7) 0.061(9) 0.008(6) 0.018(7) 0.004(6) C29 0.050(7) 0.012(5) 0.038(7) 0.000(4) 0.009(5) 0.003(5) C30 0.057(8) 0.032(7) 0.033(7) -0.001(5) 0.005(6) 0.000(6) C31 0.054(9) 0.043(9) 0.100(13) 0.006(8) 0.013(8) -0.018(7) C32 0.076(11) 0.035(8) 0.102(13) 0.022(8) 0.030(10) 0.003(7) C35 0.025(6) 0.036(7) 0.036(7) 0.002(5) -0.005(5) 0.004(5) C36 0.021(6) 0.030(6) 0.053(8) 0.000(5) 0.001(5) 0.006(5) C37 0.029(6) 0.026(6) 0.045(7) -0.008(5) 0.002(5) 0.009(5) C38 0.028(6) 0.028(6) 0.045(7) -0.001(5) 0.008(5) 0.006(5) C39 0.014(5) 0.023(6) 0.056(8) 0.005(5) 0.007(5) 0.007(4) C40 0.014(5) 0.026(6) 0.043(7) 0.001(5) -0.001(5) -0.002(4) C41 0.018(5) 0.023(6) 0.042(7) 0.007(5) -0.004(5) -0.002(4) C42 0.013(5) 0.036(7) 0.059(8) 0.005(6) 0.009(5) 0.002(5) C43 0.034(7) 0.031(7) 0.050(8) 0.014(5) 0.011(6) -0.002(5) C44 0.027(6) 0.023(6) 0.038(6) 0.002(5) 0.006(5) 0.001(4) C45 0.031(6) 0.016(5) 0.041(7) 0.002(5) 0.005(5) 0.002(4) C46 0.036(7) 0.032(7) 0.044(7) 0.004(5) 0.015(6) 0.005(5) C47 0.060(9) 0.034(7) 0.036(7) 0.004(5) 0.018(6) -0.006(6) C48 0.054(8) 0.025(6) 0.025(6) -0.005(5) 0.005(5) -0.005(5) C49 0.034(6) 0.025(6) 0.028(6) -0.001(4) 0.005(5) 0.007(5) C50 0.033(6) 0.014(5) 0.038(6) 0.001(4) 0.007(5) 0.006(4) C51 0.059(8) 0.026(6) 0.040(7) -0.011(5) 0.003(6) -0.009(6) C52 0.064(9) 0.045(8) 0.034(7) -0.008(6) -0.004(6) -0.004(7) C53 0.033(7) 0.048(8) 0.049(8) -0.010(6) 0.003(6) -0.010(6) C54 0.040(8) 0.058(9) 0.065(9) -0.004(7) 0.005(7) -0.005(7) C55 0.043(7) 0.025(6) 0.047(8) -0.002(5) 0.002(6) -0.005(5) C56 0.041(8) 0.045(8) 0.066(10) 0.003(7) 0.008(7) -0.002(6) C57 0.038(7) 0.064(10) 0.052(9) -0.003(7) 0.014(6) 0.010(6) C58 0.048(8) 0.024(6) 0.040(7) 0.000(5) 0.013(6) 0.001(5) C59 0.056(8) 0.013(6) 0.040(7) 0.005(5) 0.013(6) 0.003(5) C60 0.060(9) 0.035(7) 0.036(7) -0.001(5) 0.005(6) 0.012(6) C61 0.068(9) 0.041(8) 0.035(7) -0.001(6) 0.027(7) 0.008(7) C62 0.067(9) 0.038(8) 0.043(8) 0.001(6) 0.007(7) 0.010(7) C63 0.062(8) 0.020(6) 0.029(6) -0.001(5) 0.017(6) 0.005(5) C64 0.051(8) 0.028(7) 0.029(6) 0.011(5) 0.003(5) 0.002(5) C65 0.070(9) 0.017(6) 0.044(7) 0.000(5) 0.007(6) 0.008(6) C66 0.078(10) 0.028(7) 0.047(8) -0.005(6) 0.005(7) 0.007(6) C67 0.057(8) 0.034(7) 0.045(8) 0.004(6) 0.001(6) -0.011(6) C68 0.049(8) 0.053(9) 0.060(9) 0.012(7) 0.010(7) 0.003(7) C100 0.027(6) 0.022(6) 0.039(7) 0.000(5) 0.007(5) 0.006(5) Cl1 0.0447(17) 0.0188(14) 0.0509(18) -0.0066(12) -0.0064(14) 0.0029(12) O10 0.062(6) 0.018(4) 0.045(5) -0.006(3) 0.003(4) 0.002(4) O11 0.038(6) 0.082(9) 0.162(12) 0.021(8) -0.012(7) -0.015(6) O12 0.146(11) 0.066(8) 0.045(6) -0.019(5) 0.000(7) 0.012(7) O13 0.066(6) 0.023(5) 0.086(7) 0.008(4) -0.006(5) 0.009(4) O18 0.028(4) 0.027(4) 0.058(5) 0.005(4) 0.009(4) 0.005(3) O19 0.025(4) 0.040(5) 0.075(6) 0.018(4) 0.021(4) 0.007(4) O20 0.025(4) 0.034(5) 0.046(5) 0.009(4) 0.005(3) 0.002(3) O21 0.075(7) 0.050(6) 0.038(5) 0.003(4) -0.007(5) -0.005(5) Cl4 0.0217(13) 0.0229(13) 0.0408(15) 0.0032(11) 0.0047(11) -0.0008(10) Cl3 0.0434(19) 0.051(2) 0.070(2) -0.0064(17) 0.0145(17) -0.0031(15) O23 0.035(5) 0.101(9) 0.088(8) 0.024(7) 0.016(5) -0.015(5) Cl5 0.0272(14) 0.0182(13) 0.0323(14) -0.0003(10) 0.0074(11) -0.0040(10) O26 0.043(5) 0.020(4) 0.039(4) -0.008(3) 0.011(4) -0.006(3) O27 0.022(4) 0.035(5) 0.051(5) 0.000(4) 0.007(4) -0.004(3) O28 0.045(5) 0.020(4) 0.032(4) -0.001(3) 0.008(3) -0.001(3) O29 0.039(5) 0.028(4) 0.044(5) 0.003(3) 0.002(4) -0.002(3) O3S 0.082(8) 0.065(7) 0.066(7) 0.018(6) 0.012(6) -0.005(6) O4S 0.060(6) 0.060(7) 0.058(6) -0.009(5) 0.007(5) 0.004(5) N2S 0.052(7) 0.050(8) 0.043(7) -0.003(6) 0.003(5) 0.000(6) C2S 0.079(11) 0.069(11) 0.052(9) -0.014(8) 0.013(8) -0.001(9) O1W 0.078(8) 0.050(6) 0.080(7) 0.001(5) -0.013(6) -0.003(5) Cl2 0.129(4) 0.045(2) 0.051(2) -0.0089(17) -0.001(2) 0.031(2) O17 0.044(5) 0.059(6) 0.053(6) -0.006(4) 0.003(4) -0.007(4) O16 0.082(7) 0.033(5) 0.082(7) 0.008(5) -0.020(6) -0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O1 2.423(6) . ? La1 O8 2.427(7) . ? La1 O3 2.524(7) . ? La1 O6 2.548(7) . ? La1 O10 2.563(7) . ? La1 N2 2.687(8) . ? La1 N3 2.736(8) . ? La1 N10 2.744(8) . ? La1 N11 2.778(8) . ? La2 O15' 2.346(16) . ? La2 O7 2.430(7) . ? La2 O2 2.471(8) . ? La2 O4 2.518(7) . ? La2 O5 2.548(7) . ? La2 N15 2.666(9) . ? La2 N7 2.695(9) . ? La2 N6 2.704(9) . ? La2 N14 2.778(9) . ? La2 O14 2.785(15) . ? La2 O15 2.971(16) . ? O1 C16 1.266(12) . ? O2 C30 1.249(14) . ? O3 C50 1.265(12) . ? O4 C64 1.265(13) . ? O7 C100 1.235(12) . ? O8 C100 1.240(12) . ? N1 C16 1.315(13) . ? N1 C17 1.472(13) . ? N1 C19 1.482(13) . ? N2 C15 1.332(13) . ? N2 C11 1.362(13) . ? N3 C10 1.350(13) . ? N3 N4 1.358(11) . ? N4 C8 1.352(13) . ? N4 C7 1.463(13) . ? N5 C22 1.343(14) . ? N5 N6 1.347(12) . ? N5 C21 1.476(13) . ? N6 C24 1.362(13) . ? N7 C29 1.335(14) . ? N7 C25 1.361(14) . ? N9 C50 1.333(14) . ? N9 C51 1.437(14) . ? N9 C53 1.473(14) . ? N8 C30 1.324(16) . ? N8 C33 1.482(17) . ? N8 C31 1.505(17) . ? N10 C45 1.330(13) . ? N10 C49 1.346(13) . ? N11 C44 1.348(13) . ? N11 N12 1.352(11) . ? N12 C42 1.355(13) . ? N12 C41 1.456(13) . ? N13 N14 1.338(13) . ? N13 C56 1.364(16) . ? N13 C55 1.421(15) . ? N14 C58 1.307(14) . ? N15 C59 1.343(15) . ? N15 C63 1.344(15) . ? N16 C64 1.323(15) . ? N16 C67 1.474(16) . ? N16 C65 1.481(14) . ? C1 C2 1.388(15) . ? C1 C6 1.402(14) . ? C1 H1 0.9500 . ? C2 C3 1.394(16) . ? C2 C21 1.505(15) . ? C3 C4 1.390(17) . ? C3 H3 0.9500 . ? C4 C5 1.356(17) . ? C4 H4 0.9500 . ? C5 C6 1.386(14) . ? C5 H5 0.9500 . ? C6 C7 1.490(15) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.359(14) . ? C8 H8 0.9500 . ? C9 C10 1.388(14) . ? C9 H9 0.9500 . ? C10 C11 1.445(14) . ? C11 C12 1.384(15) . ? C12 C13 1.379(15) . ? C12 H12 0.9500 . ? C13 C14 1.384(15) . ? C13 H13 0.9500 . ? C14 C15 1.380(14) . ? C14 H14 0.9500 . ? C15 C16 1.517(14) . ? C17 C18 1.519(16) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.496(18) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.358(16) . ? C22 H22 0.9500 . ? C23 C24 1.387(16) . ? C23 H23 0.9500 . ? C24 C25 1.439(15) . ? C25 C26 1.387(15) . ? C26 C27 1.355(17) . ? C26 H26 0.9500 . ? C27 C28 1.390(17) . ? C27 H27 0.9500 . ? C28 C29 1.393(16) . ? C28 H28 0.9500 . ? C29 C30 1.499(17) . ? C31 C32 1.50(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.43(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C40 1.389(15) . ? C35 C36 1.421(16) . ? C35 H35 0.9500 . ? C36 C37 1.360(16) . ? C36 C55 1.538(16) . ? C37 C38 1.376(16) . ? C37 H37 0.9500 . ? C38 C39 1.380(15) . ? C38 H38 0.9500 . ? C39 C40 1.407(15) . ? C39 H39 0.9500 . ? C40 C41 1.511(15) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.361(16) . ? C42 H42 0.9500 . ? C43 C44 1.400(15) . ? C43 H43 0.9500 . ? C44 C45 1.485(15) . ? C45 C46 1.390(15) . ? C46 C47 1.375(17) . ? C46 H46 0.9500 . ? C47 C48 1.387(17) . ? C47 H47 0.9500 . ? C48 C49 1.382(15) . ? C48 H48 0.9500 . ? C49 C50 1.496(15) . ? C51 C52 1.498(17) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.508(18) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.351(18) . ? C56 H56 0.9500 . ? C57 C58 1.420(17) . ? C57 H57 0.9500 . ? C58 C59 1.475(17) . ? C59 C60 1.412(16) . ? C60 C61 1.368(18) . ? C60 H60 0.9500 . ? C61 C62 1.416(19) . ? C61 H61 0.9500 . ? C62 C63 1.413(16) . ? C62 H62 0.9500 . ? C63 C64 1.494(17) . ? C65 C66 1.529(18) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.518(18) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C100 H100 0.9500 . ? Cl1 O12 1.402(11) . ? Cl1 O11 1.408(11) . ? Cl1 O13 1.429(9) . ? Cl1 O10 1.448(8) . ? O18 Cl4 1.444(8) . ? O19 Cl4 1.418(8) . ? O20 Cl4 1.438(8) . ? O21 Cl4 1.414(9) . ? Cl3 O23 1.426(10) . ? Cl3 O24' 1.429(12) . ? Cl3 O25 1.435(15) . ? Cl3 O22' 1.454(13) . ? Cl3 O22 1.456(15) . ? Cl3 O25' 1.472(12) . ? Cl3 O24 1.472(15) . ? Cl5 O27 1.433(8) . ? Cl5 O26 1.435(7) . ? Cl5 O29 1.439(8) . ? Cl5 O28 1.448(7) . ? O1S N1S 1.18(2) . ? O2S N1S 1.36(2) . ? N1S C1S 1.37(3) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? O3S N2S 1.240(14) . ? O4S N2S 1.241(14) . ? N2S C2S 1.427(17) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C3S N3S 1.27(2) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? O5S N3S 1.34(2) . ? O6S N3S 1.44(2) . ? N4S O8S 1.18(3) . ? N4S O7S 1.29(3) . ? N4S C4S 1.44(3) . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? O9S N5S 1.21(2) . ? C5S N5S 1.36(2) . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 0.9800 . ? N5S O10S 1.29(3) . ? Cl2 O17 1.392(9) . ? Cl2 O16 1.403(10) . ? Cl2 O15' 1.413(14) . ? Cl2 O14 1.455(13) . ? Cl2 O14' 1.557(15) . ? Cl2 O15 1.619(13) . ? 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 La1 O8 132.3(2) . . ? O1 La1 O3 145.4(2) . . ? O8 La1 O3 77.9(2) . . ? O1 La1 O6 75.8(2) . . ? O8 La1 O6 72.7(2) . . ? O3 La1 O6 137.1(2) . . ? O1 La1 O10 73.9(2) . . ? O8 La1 O10 143.6(2) . . ? O3 La1 O10 71.6(2) . . ? O6 La1 O10 143.7(2) . . ? O1 La1 N2 60.8(2) . . ? O8 La1 N2 137.2(2) . . ? O3 La1 N2 111.3(2) . . ? O6 La1 N2 73.8(2) . . ? O10 La1 N2 74.1(3) . . ? O1 La1 N3 121.8(2) . . ? O8 La1 N3 86.6(2) . . ? O3 La1 N3 67.9(2) . . ? O6 La1 N3 79.7(2) . . ? O10 La1 N3 99.7(3) . . ? N2 La1 N3 61.9(2) . . ? O1 La1 N10 103.6(2) . . ? O8 La1 N10 79.7(2) . . ? O3 La1 N10 60.5(2) . . ? O6 La1 N10 139.4(2) . . ? O10 La1 N10 68.3(3) . . ? N2 La1 N10 142.2(2) . . ? N3 La1 N10 128.2(2) . . ? O1 La1 N11 65.5(2) . . ? O8 La1 N11 76.7(2) . . ? O3 La1 N11 118.0(2) . . ? O6 La1 N11 84.8(2) . . ? O10 La1 N11 100.3(3) . . ? N2 La1 N11 125.5(2) . . ? N3 La1 N11 160.0(2) . . ? N10 La1 N11 59.9(2) . . ? O15' La2 O7 132.5(5) . . ? O15' La2 O2 84.0(5) . . ? O7 La2 O2 135.8(3) . . ? O15' La2 O4 148.4(5) . . ? O7 La2 O4 73.1(2) . . ? O2 La2 O4 85.3(3) . . ? O15' La2 O5 62.7(5) . . ? O7 La2 O5 70.3(2) . . ? O2 La2 O5 141.8(3) . . ? O4 La2 O5 132.8(2) . . ? O15' La2 N15 136.1(5) . . ? O7 La2 N15 70.3(3) . . ? O2 La2 N15 65.5(3) . . ? O4 La2 N15 62.9(3) . . ? O5 La2 N15 126.9(3) . . ? O15' La2 N7 75.1(5) . . ? O7 La2 N7 140.8(3) . . ? O2 La2 N7 60.2(3) . . ? O4 La2 N7 73.7(3) . . ? O5 La2 N7 121.7(2) . . ? N15 La2 N7 111.3(3) . . ? O15' La2 N6 90.5(5) . . ? O7 La2 N6 87.1(2) . . ? O2 La2 N6 121.6(3) . . ? O4 La2 N6 70.2(3) . . ? O5 La2 N6 79.1(2) . . ? N15 La2 N6 131.9(3) . . ? N7 La2 N6 62.3(3) . . ? O15' La2 N14 83.1(5) . . ? O7 La2 N14 84.1(2) . . ? O2 La2 N14 75.7(3) . . ? O4 La2 N14 122.6(3) . . ? O5 La2 N14 82.0(3) . . ? N15 La2 N14 59.9(3) . . ? N7 La2 N14 132.1(3) . . ? N6 La2 N14 161.0(3) . . ? O15' La2 O14 24.5(5) . . ? O7 La2 O14 137.0(4) . . ? O2 La2 O14 65.6(4) . . ? O4 La2 O14 148.3(4) . . ? O5 La2 O14 76.9(4) . . ? N15 La2 O14 111.6(4) . . ? N7 La2 O14 80.6(4) . . ? N6 La2 O14 113.6(3) . . ? N14 La2 O14 64.0(3) . . ? O15' La2 O15 23.6(5) . . ? O7 La2 O15 130.6(3) . . ? O2 La2 O15 93.1(3) . . ? O4 La2 O15 128.5(3) . . ? O5 La2 O15 64.0(3) . . ? N15 La2 O15 156.3(3) . . ? N7 La2 O15 61.5(4) . . ? N6 La2 O15 67.3(3) . . ? N14 La2 O15 106.5(3) . . ? O14 La2 O15 46.5(4) . . ? C16 O1 La1 126.9(6) . . ? C30 O2 La2 126.4(8) . . ? C50 O3 La1 119.8(6) . . ? C64 O4 La2 118.4(7) . . ? C100 O7 La2 140.4(7) . . ? C100 O8 La1 140.5(7) . . ? C16 N1 C17 126.6(9) . . ? C16 N1 C19 117.8(9) . . ? C17 N1 C19 115.3(8) . . ? C15 N2 C11 119.2(9) . . ? C15 N2 La1 119.3(6) . . ? C11 N2 La1 120.5(6) . . ? C10 N3 N4 104.3(8) . . ? C10 N3 La1 116.9(6) . . ? N4 N3 La1 134.5(6) . . ? C8 N4 N3 111.6(8) . . ? C8 N4 C7 125.5(9) . . ? N3 N4 C7 122.5(8) . . ? C22 N5 N6 110.7(9) . . ? C22 N5 C21 127.5(10) . . ? N6 N5 C21 121.9(8) . . ? N5 N6 C24 105.2(8) . . ? N5 N6 La2 136.9(6) . . ? C24 N6 La2 117.8(7) . . ? C29 N7 C25 120.4(9) . . ? C29 N7 La2 119.3(7) . . ? C25 N7 La2 120.2(7) . . ? C50 N9 C51 125.6(10) . . ? C50 N9 C53 117.4(9) . . ? C51 N9 C53 116.6(9) . . ? C30 N8 C33 119.2(11) . . ? C30 N8 C31 125.5(11) . . ? C33 N8 C31 114.7(11) . . ? C45 N10 C49 120.0(9) . . ? C45 N10 La1 122.6(7) . . ? C49 N10 La1 116.8(6) . . ? C44 N11 N12 103.4(8) . . ? C44 N11 La1 119.8(6) . . ? N12 N11 La1 133.6(6) . . ? N11 N12 C42 112.9(9) . . ? N11 N12 C41 121.6(8) . . ? C42 N12 C41 125.4(9) . . ? N14 N13 C56 109.8(10) . . ? N14 N13 C55 122.9(9) . . ? C56 N13 C55 126.7(11) . . ? C58 N14 N13 107.8(10) . . ? C58 N14 La2 115.5(8) . . ? N13 N14 La2 132.9(7) . . ? C59 N15 C63 120.3(10) . . ? C59 N15 La2 119.9(7) . . ? C63 N15 La2 116.0(7) . . ? C64 N16 C67 118.9(10) . . ? C64 N16 C65 123.0(11) . . ? C67 N16 C65 116.4(10) . . ? C2 C1 C6 121.2(10) . . ? C2 C1 H1 119.4 . . ? C6 C1 H1 119.4 . . ? C1 C2 C3 119.0(10) . . ? C1 C2 C21 120.0(10) . . ? C3 C2 C21 121.0(10) . . ? C4 C3 C2 119.5(11) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 120.9(11) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 121.3(11) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 118.0(10) . . ? C5 C6 C7 122.0(10) . . ? C1 C6 C7 120.0(9) . . ? N4 C7 C6 113.4(9) . . ? N4 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? N4 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N4 C8 C9 107.3(9) . . ? N4 C8 H8 126.3 . . ? C9 C8 H8 126.3 . . ? C8 C9 C10 105.8(9) . . ? C8 C9 H9 127.1 . . ? C10 C9 H9 127.1 . . ? N3 C10 C9 110.9(9) . . ? N3 C10 C11 120.5(9) . . ? C9 C10 C11 128.5(9) . . ? N2 C11 C12 120.5(9) . . ? N2 C11 C10 117.2(9) . . ? C12 C11 C10 122.4(9) . . ? C13 C12 C11 120.2(10) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 118.4(10) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 119.2(10) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N2 C15 C14 122.2(9) . . ? N2 C15 C16 111.1(9) . . ? C14 C15 C16 126.4(9) . . ? O1 C16 N1 120.4(9) . . ? O1 C16 C15 115.7(9) . . ? N1 C16 C15 123.9(9) . . ? N1 C17 C18 111.9(9) . . ? N1 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? N1 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C20 112.5(10) . . ? N1 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? N1 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 C2 112.0(8) . . ? N5 C21 H21A 109.2 . . ? C2 C21 H21A 109.2 . . ? N5 C21 H21B 109.2 . . ? C2 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? N5 C22 C23 108.7(11) . . ? N5 C22 H22 125.6 . . ? C23 C22 H22 125.6 . . ? C22 C23 C24 105.2(10) . . ? C22 C23 H23 127.4 . . ? C24 C23 H23 127.4 . . ? N6 C24 C23 110.2(9) . . ? N6 C24 C25 121.8(10) . . ? C23 C24 C25 128.0(10) . . ? N7 C25 C26 120.3(10) . . ? N7 C25 C24 117.8(9) . . ? C26 C25 C24 121.9(10) . . ? C27 C26 C25 120.2(12) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 119.0(12) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C27 C28 C29 119.6(12) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? N7 C29 C28 120.3(11) . . ? N7 C29 C30 112.4(9) . . ? C28 C29 C30 127.1(11) . . ? O2 C30 N8 118.8(12) . . ? O2 C30 C29 116.7(11) . . ? N8 C30 C29 124.5(11) . . ? C32 C31 N8 112.0(13) . . ? C32 C31 H31A 109.2 . . ? N8 C31 H31A 109.2 . . ? C32 C31 H31B 109.2 . . ? N8 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N8 114.2(15) . . ? C34 C33 H33A 108.7 . . ? N8 C33 H33A 108.7 . . ? C34 C33 H33B 108.7 . . ? N8 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 118.3(11) . . ? C40 C35 H35 120.8 . . ? C36 C35 H35 120.8 . . ? C37 C36 C35 120.8(11) . . ? C37 C36 C55 118.9(10) . . ? C35 C36 C55 120.3(11) . . ? C36 C37 C38 121.2(11) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C37 C38 C39 119.1(11) . . ? C37 C38 H38 120.5 . . ? C39 C38 H38 120.5 . . ? C38 C39 C40 121.2(10) . . ? C38 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C35 C40 C39 119.3(10) . . ? C35 C40 C41 122.4(10) . . ? C39 C40 C41 118.0(9) . . ? N12 C41 C40 114.2(8) . . ? N12 C41 H41A 108.7 . . ? C40 C41 H41A 108.7 . . ? N12 C41 H41B 108.7 . . ? C40 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? N12 C42 C43 106.8(10) . . ? N12 C42 H42 126.6 . . ? C43 C42 H42 126.6 . . ? C42 C43 C44 105.1(10) . . ? C42 C43 H43 127.5 . . ? C44 C43 H43 127.5 . . ? N11 C44 C43 111.8(10) . . ? N11 C44 C45 118.3(9) . . ? C43 C44 C45 129.8(10) . . ? N10 C45 C46 121.8(10) . . ? N10 C45 C44 117.3(9) . . ? C46 C45 C44 120.8(10) . . ? C47 C46 C45 118.2(11) . . ? C47 C46 H46 120.9 . . ? C45 C46 H46 120.9 . . ? C46 C47 C48 119.9(11) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C49 C48 C47 118.7(11) . . ? C49 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? N10 C49 C48 121.1(10) . . ? N10 C49 C50 112.7(9) . . ? C48 C49 C50 125.9(10) . . ? O3 C50 N9 120.5(10) . . ? O3 C50 C49 116.5(9) . . ? N9 C50 C49 123.0(9) . . ? N9 C51 C52 114.0(11) . . ? N9 C51 H51A 108.8 . . ? C52 C51 H51A 108.8 . . ? N9 C51 H51B 108.8 . . ? C52 C51 H51B 108.8 . . ? H51A C51 H51B 107.7 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N9 C53 C54 113.3(11) . . ? N9 C53 H53A 108.9 . . ? C54 C53 H53A 108.9 . . ? N9 C53 H53B 108.9 . . ? C54 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N13 C55 C36 114.1(9) . . ? N13 C55 H55A 108.7 . . ? C36 C55 H55A 108.7 . . ? N13 C55 H55B 108.7 . . ? C36 C55 H55B 108.7 . . ? H55A C55 H55B 107.6 . . ? C57 C56 N13 107.7(12) . . ? C57 C56 H56 126.1 . . ? N13 C56 H56 126.1 . . ? C56 C57 C58 105.1(11) . . ? C56 C57 H57 127.4 . . ? C58 C57 H57 127.4 . . ? N14 C58 C57 109.5(11) . . ? N14 C58 C59 120.5(11) . . ? C57 C58 C59 130.0(11) . . ? N15 C59 C60 122.5(11) . . ? N15 C59 C58 115.5(10) . . ? C60 C59 C58 121.9(11) . . ? C61 C60 C59 116.4(12) . . ? C61 C60 H60 121.8 . . ? C59 C60 H60 121.8 . . ? C60 C61 C62 122.8(11) . . ? C60 C61 H61 118.6 . . ? C62 C61 H61 118.6 . . ? C63 C62 C61 116.0(12) . . ? C63 C62 H62 122.0 . . ? C61 C62 H62 122.0 . . ? N15 C63 C62 121.8(12) . . ? N15 C63 C64 112.7(9) . . ? C62 C63 C64 125.3(12) . . ? O4 C64 N16 120.6(11) . . ? O4 C64 C63 116.4(11) . . ? N16 C64 C63 123.1(11) . . ? N16 C65 C66 112.2(10) . . ? N16 C65 H65A 109.2 . . ? C66 C65 H65A 109.2 . . ? N16 C65 H65B 109.2 . . ? C66 C65 H65B 109.2 . . ? H65A C65 H65B 107.9 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N16 C67 C68 115.1(10) . . ? N16 C67 H67A 108.5 . . ? C68 C67 H67A 108.5 . . ? N16 C67 H67B 108.5 . . ? C68 C67 H67B 108.5 . . ? H67A C67 H67B 107.5 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O7 C100 O8 127.8(10) . . ? O7 C100 H100 116.1 . . ? O8 C100 H100 116.1 . . ? O12 Cl1 O11 111.6(8) . . ? O12 Cl1 O13 111.9(7) . . ? O11 Cl1 O13 110.0(7) . . ? O12 Cl1 O10 106.7(6) . . ? O11 Cl1 O10 109.0(7) . . ? O13 Cl1 O10 107.5(5) . . ? Cl1 O10 La1 150.9(5) . . ? O21 Cl4 O19 111.2(6) . . ? O21 Cl4 O20 109.2(5) . . ? O19 Cl4 O20 108.9(5) . . ? O21 Cl4 O18 108.9(5) . . ? O19 Cl4 O18 110.4(5) . . ? O20 Cl4 O18 108.2(5) . . ? O23 Cl3 O24' 108.2(10) . . ? O23 Cl3 O25 113.9(15) . . ? O24' Cl3 O25 125.1(15) . . ? O23 Cl3 O22' 114.6(10) . . ? O24' Cl3 O22' 110.6(9) . . ? O25 Cl3 O22' 82.3(13) . . ? O23 Cl3 O22 105.1(16) . . ? O24' Cl3 O22 90.3(14) . . ? O25 Cl3 O22 110.3(12) . . ? O22' Cl3 O22 28.3(13) . . ? O23 Cl3 O25' 104.5(9) . . ? O24' Cl3 O25' 110.5(9) . . ? O25 Cl3 O25' 26.2(13) . . ? O22' Cl3 O25' 108.3(8) . . ? O22 Cl3 O25' 135.8(14) . . ? O23 Cl3 O24 112.5(15) . . ? O24' Cl3 O24 19.9(13) . . ? O25 Cl3 O24 107.8(12) . . ? O22' Cl3 O24 121.7(16) . . ? O22 Cl3 O24 107.1(12) . . ? O25' Cl3 O24 90.7(13) . . ? O27 Cl5 O26 110.6(5) . . ? O27 Cl5 O29 108.8(5) . . ? O26 Cl5 O29 110.7(5) . . ? O27 Cl5 O28 109.6(5) . . ? O26 Cl5 O28 108.4(4) . . ? O29 Cl5 O28 108.7(5) . . ? O1S N1S O2S 120(2) . . ? O1S N1S C1S 125(3) . . ? O2S N1S C1S 112(2) . . ? N1S C1S H1S1 109.5 . . ? N1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? N1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O4S N2S O3S 123.4(12) . . ? O4S N2S C2S 117.0(12) . . ? O3S N2S C2S 119.5(12) . . ? N2S C2S H2S1 109.5 . . ? N2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? N2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N3S C3S H3S1 109.5 . . ? N3S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? N3S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? C3S N3S O5S 123(2) . . ? C3S N3S O6S 123(2) . . ? O5S N3S O6S 114.5(19) . . ? O8S N4S O7S 122(3) . . ? O8S N4S C4S 121(3) . . ? O7S N4S C4S 110(3) . . ? N4S C4S H4S1 109.5 . . ? N4S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? N4S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? N5S C5S H5S1 109.5 . . ? N5S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? N5S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? O9S N5S O10S 113(2) . . ? O9S N5S C5S 131(2) . . ? O10S N5S C5S 112(2) . . ? O17 Cl2 O16 112.2(6) . . ? O17 Cl2 O15' 117.7(9) . . ? O16 Cl2 O15' 124.8(9) . . ? O17 Cl2 O14 123.4(8) . . ? O16 Cl2 O14 116.7(8) . . ? O15' Cl2 O14 48.1(9) . . ? O17 Cl2 O14' 96.7(9) . . ? O16 Cl2 O14' 98.1(10) . . ? O15' Cl2 O14' 98.2(9) . . ? O14 Cl2 O14' 50.8(8) . . ? O17 Cl2 O15 100.8(7) . . ? O16 Cl2 O15 101.7(8) . . ? O15' Cl2 O15 48.0(8) . . ? O14 Cl2 O15 95.6(8) . . ? O14' Cl2 O15 146.2(10) . . ? Cl2 O14 La2 113.8(8) . . ? Cl2 O15 La2 100.1(7) . . ? Cl2 O15' La2 148.4(12) . . ? 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 O8 La1 O1 C16 147.5(8) . . . . ? O3 La1 O1 C16 -67.1(9) . . . . ? O6 La1 O1 C16 97.7(8) . . . . ? O10 La1 O1 C16 -62.0(8) . . . . ? N2 La1 O1 C16 18.5(8) . . . . ? N3 La1 O1 C16 29.6(9) . . . . ? N10 La1 O1 C16 -124.2(8) . . . . ? N11 La1 O1 C16 -171.6(9) . . . . ? O15' La2 O2 C30 -56.2(11) . . . . ? O7 La2 O2 C30 153.8(9) . . . . ? O4 La2 O2 C30 94.0(10) . . . . ? O5 La2 O2 C30 -84.5(11) . . . . ? N15 La2 O2 C30 156.3(11) . . . . ? N7 La2 O2 C30 20.1(9) . . . . ? N6 La2 O2 C30 30.7(11) . . . . ? N14 La2 O2 C30 -140.6(11) . . . . ? O14 La2 O2 C30 -73.0(10) . . . . ? O15 La2 O2 C30 -34.4(10) . . . . ? O1 La1 O3 C50 -39.8(9) . . . . ? O8 La1 O3 C50 114.7(7) . . . . ? O6 La1 O3 C50 162.1(7) . . . . ? O10 La1 O3 C50 -45.1(7) . . . . ? N2 La1 O3 C50 -109.0(7) . . . . ? N3 La1 O3 C50 -154.1(8) . . . . ? N10 La1 O3 C50 29.9(7) . . . . ? N11 La1 O3 C50 47.1(8) . . . . ? O15' La2 O4 C64 157.0(10) . . . . ? O7 La2 O4 C64 -54.4(8) . . . . ? O2 La2 O4 C64 86.5(8) . . . . ? O5 La2 O4 C64 -94.8(8) . . . . ? N15 La2 O4 C64 21.6(7) . . . . ? N7 La2 O4 C64 146.7(8) . . . . ? N6 La2 O4 C64 -147.5(8) . . . . ? N14 La2 O4 C64 16.8(9) . . . . ? O14 La2 O4 C64 109.3(9) . . . . ? O15 La2 O4 C64 176.7(8) . . . . ? O15' La2 O7 C100 -87.3(13) . . . . ? O2 La2 O7 C100 50.2(12) . . . . ? O4 La2 O7 C100 114.4(11) . . . . ? O5 La2 O7 C100 -95.9(11) . . . . ? N15 La2 O7 C100 47.8(11) . . . . ? N7 La2 O7 C100 147.7(10) . . . . ? N6 La2 O7 C100 -175.4(11) . . . . ? N14 La2 O7 C100 -12.3(11) . . . . ? O14 La2 O7 C100 -53.1(13) . . . . ? O15 La2 O7 C100 -119.0(11) . . . . ? O1 La1 O8 C100 16.5(12) . . . . ? O3 La1 O8 C100 -144.3(11) . . . . ? O6 La1 O8 C100 67.3(11) . . . . ? O10 La1 O8 C100 -110.7(11) . . . . ? N2 La1 O8 C100 107.2(11) . . . . ? N3 La1 O8 C100 147.6(11) . . . . ? N10 La1 O8 C100 -82.6(11) . . . . ? N11 La1 O8 C100 -21.3(11) . . . . ? O1 La1 N2 C15 -2.1(7) . . . . ? O8 La1 N2 C15 -124.2(7) . . . . ? O3 La1 N2 C15 140.5(7) . . . . ? O6 La1 N2 C15 -84.6(7) . . . . ? O10 La1 N2 C15 78.0(7) . . . . ? N3 La1 N2 C15 -171.5(8) . . . . ? N10 La1 N2 C15 71.5(8) . . . . ? N11 La1 N2 C15 -13.5(8) . . . . ? O1 La1 N2 C11 166.6(8) . . . . ? O8 La1 N2 C11 44.5(9) . . . . ? O3 La1 N2 C11 -50.8(8) . . . . ? O6 La1 N2 C11 84.1(7) . . . . ? O10 La1 N2 C11 -113.3(8) . . . . ? N3 La1 N2 C11 -2.8(7) . . . . ? N10 La1 N2 C11 -119.8(7) . . . . ? N11 La1 N2 C11 155.2(7) . . . . ? O1 La1 N3 C10 -18.9(8) . . . . ? O8 La1 N3 C10 -158.0(7) . . . . ? O3 La1 N3 C10 123.6(7) . . . . ? O6 La1 N3 C10 -85.0(7) . . . . ? O10 La1 N3 C10 58.1(7) . . . . ? N2 La1 N3 C10 -8.0(6) . . . . ? N10 La1 N3 C10 128.0(7) . . . . ? N11 La1 N3 C10 -125.0(8) . . . . ? O1 La1 N3 N4 -171.8(8) . . . . ? O8 La1 N3 N4 49.2(9) . . . . ? O3 La1 N3 N4 -29.2(8) . . . . ? O6 La1 N3 N4 122.2(9) . . . . ? O10 La1 N3 N4 -94.7(9) . . . . ? N2 La1 N3 N4 -160.8(9) . . . . ? N10 La1 N3 N4 -24.8(10) . . . . ? N11 La1 N3 N4 82.2(11) . . . . ? C10 N3 N4 C8 -1.1(11) . . . . ? La1 N3 N4 C8 154.0(7) . . . . ? C10 N3 N4 C7 171.8(9) . . . . ? La1 N3 N4 C7 -33.1(13) . . . . ? C22 N5 N6 C24 0.7(12) . . . . ? C21 N5 N6 C24 -178.4(9) . . . . ? C22 N5 N6 La2 178.8(8) . . . . ? C21 N5 N6 La2 -0.4(15) . . . . ? O15' La2 N6 N5 -105.3(10) . . . . ? O7 La2 N6 N5 27.2(9) . . . . ? O2 La2 N6 N5 171.4(9) . . . . ? O4 La2 N6 N5 100.3(10) . . . . ? O5 La2 N6 N5 -43.3(9) . . . . ? N15 La2 N6 N5 87.2(10) . . . . ? N7 La2 N6 N5 -178.2(10) . . . . ? N14 La2 N6 N5 -35.2(15) . . . . ? O14 La2 N6 N5 -113.7(10) . . . . ? O15 La2 N6 N5 -109.5(10) . . . . ? O15' La2 N6 C24 72.5(8) . . . . ? O7 La2 N6 C24 -155.0(7) . . . . ? O2 La2 N6 C24 -10.8(8) . . . . ? O4 La2 N6 C24 -81.9(7) . . . . ? O5 La2 N6 C24 134.5(7) . . . . ? N15 La2 N6 C24 -95.0(8) . . . . ? N7 La2 N6 C24 -0.4(7) . . . . ? N14 La2 N6 C24 142.6(8) . . . . ? O14 La2 N6 C24 64.1(8) . . . . ? O15 La2 N6 C24 68.3(8) . . . . ? O15' La2 N7 C29 83.6(9) . . . . ? O7 La2 N7 C29 -135.1(7) . . . . ? O2 La2 N7 C29 -8.0(7) . . . . ? O4 La2 N7 C29 -101.9(8) . . . . ? O5 La2 N7 C29 127.4(8) . . . . ? N15 La2 N7 C29 -50.5(8) . . . . ? N6 La2 N7 C29 -177.7(9) . . . . ? N14 La2 N7 C29 17.6(9) . . . . ? O14 La2 N7 C29 59.2(8) . . . . ? O15 La2 N7 C29 104.5(8) . . . . ? O15' La2 N7 C25 -99.7(9) . . . . ? O7 La2 N7 C25 41.6(9) . . . . ? O2 La2 N7 C25 168.7(9) . . . . ? O4 La2 N7 C25 74.8(8) . . . . ? O5 La2 N7 C25 -55.9(8) . . . . ? N15 La2 N7 C25 126.2(7) . . . . ? N6 La2 N7 C25 -1.0(7) . . . . ? N14 La2 N7 C25 -165.7(7) . . . . ? O14 La2 N7 C25 -124.1(8) . . . . ? O15 La2 N7 C25 -78.8(8) . . . . ? O1 La1 N10 C45 -52.8(8) . . . . ? O8 La1 N10 C45 78.5(8) . . . . ? O3 La1 N10 C45 160.4(8) . . . . ? O6 La1 N10 C45 31.1(9) . . . . ? O10 La1 N10 C45 -119.0(8) . . . . ? N2 La1 N10 C45 -112.3(8) . . . . ? N3 La1 N10 C45 155.7(7) . . . . ? N11 La1 N10 C45 -2.0(7) . . . . ? O1 La1 N10 C49 135.7(7) . . . . ? O8 La1 N10 C49 -93.0(7) . . . . ? O3 La1 N10 C49 -11.1(6) . . . . ? O6 La1 N10 C49 -140.4(6) . . . . ? O10 La1 N10 C49 69.5(7) . . . . ? N2 La1 N10 C49 76.2(8) . . . . ? N3 La1 N10 C49 -15.8(8) . . . . ? N11 La1 N10 C49 -173.5(8) . . . . ? O1 La1 N11 C44 117.0(8) . . . . ? O8 La1 N11 C44 -92.9(7) . . . . ? O3 La1 N11 C44 -24.6(8) . . . . ? O6 La1 N11 C44 -166.3(7) . . . . ? O10 La1 N11 C44 50.0(7) . . . . ? N2 La1 N11 C44 127.8(7) . . . . ? N3 La1 N11 C44 -126.9(8) . . . . ? N10 La1 N11 C44 -7.2(7) . . . . ? O1 La1 N11 N12 -38.8(8) . . . . ? O8 La1 N11 N12 111.3(8) . . . . ? O3 La1 N11 N12 179.6(7) . . . . ? O6 La1 N11 N12 37.9(8) . . . . ? O10 La1 N11 N12 -105.8(8) . . . . ? N2 La1 N11 N12 -28.0(9) . . . . ? N3 La1 N11 N12 77.3(11) . . . . ? N10 La1 N11 N12 -163.0(9) . . . . ? C44 N11 N12 C42 -0.6(11) . . . . ? La1 N11 N12 C42 158.0(7) . . . . ? C44 N11 N12 C41 177.0(9) . . . . ? La1 N11 N12 C41 -24.5(13) . . . . ? C56 N13 N14 C58 -0.2(12) . . . . ? C55 N13 N14 C58 -171.7(10) . . . . ? C56 N13 N14 La2 -156.7(8) . . . . ? C55 N13 N14 La2 31.9(14) . . . . ? O15' La2 N14 C58 -133.2(9) . . . . ? O7 La2 N14 C58 92.7(8) . . . . ? O2 La2 N14 C58 -47.7(8) . . . . ? O4 La2 N14 C58 27.1(9) . . . . ? O5 La2 N14 C58 163.5(8) . . . . ? N15 La2 N14 C58 22.1(7) . . . . ? N7 La2 N14 C58 -70.4(9) . . . . ? N6 La2 N14 C58 155.5(8) . . . . ? O14 La2 N14 C58 -117.1(9) . . . . ? O15 La2 N14 C58 -136.7(8) . . . . ? O15' La2 N14 N13 21.9(9) . . . . ? O7 La2 N14 N13 -112.3(9) . . . . ? O2 La2 N14 N13 107.4(9) . . . . ? O4 La2 N14 N13 -177.8(8) . . . . ? O5 La2 N14 N13 -41.4(9) . . . . ? N15 La2 N14 N13 177.2(10) . . . . ? N7 La2 N14 N13 84.7(9) . . . . ? N6 La2 N14 N13 -49.4(14) . . . . ? O14 La2 N14 N13 38.0(9) . . . . ? O15 La2 N14 N13 18.4(9) . . . . ? O15' La2 N15 C59 11.6(11) . . . . ? O7 La2 N15 C59 -119.8(8) . . . . ? O2 La2 N15 C59 62.0(8) . . . . ? O4 La2 N15 C59 159.6(8) . . . . ? O5 La2 N15 C59 -75.6(8) . . . . ? N7 La2 N15 C59 102.1(8) . . . . ? N6 La2 N15 C59 173.4(7) . . . . ? N14 La2 N15 C59 -25.1(7) . . . . ? O14 La2 N15 C59 14.0(9) . . . . ? O15 La2 N15 C59 34.6(13) . . . . ? O15' La2 N15 C63 -146.6(9) . . . . ? O7 La2 N15 C63 82.0(8) . . . . ? O2 La2 N15 C63 -96.2(8) . . . . ? O4 La2 N15 C63 1.4(7) . . . . ? O5 La2 N15 C63 126.2(7) . . . . ? N7 La2 N15 C63 -56.1(8) . . . . ? N6 La2 N15 C63 15.2(9) . . . . ? N14 La2 N15 C63 176.7(8) . . . . ? O14 La2 N15 C63 -144.2(8) . . . . ? O15 La2 N15 C63 -123.6(10) . . . . ? C6 C1 C2 C3 2.3(15) . . . . ? C6 C1 C2 C21 -178.6(9) . . . . ? C1 C2 C3 C4 -2.0(17) . . . . ? C21 C2 C3 C4 178.9(11) . . . . ? C2 C3 C4 C5 -0.5(19) . . . . ? C3 C4 C5 C6 2.7(19) . . . . ? C4 C5 C6 C1 -2.4(16) . . . . ? C4 C5 C6 C7 177.8(11) . . . . ? C2 C1 C6 C5 -0.1(15) . . . . ? C2 C1 C6 C7 179.7(9) . . . . ? C8 N4 C7 C6 75.7(13) . . . . ? N3 N4 C7 C6 -96.1(11) . . . . ? C5 C6 C7 N4 -73.4(13) . . . . ? C1 C6 C7 N4 106.8(11) . . . . ? N3 N4 C8 C9 1.0(12) . . . . ? C7 N4 C8 C9 -171.5(9) . . . . ? N4 C8 C9 C10 -0.6(12) . . . . ? N4 N3 C10 C9 0.7(11) . . . . ? La1 N3 C10 C9 -159.6(7) . . . . ? N4 N3 C10 C11 178.7(9) . . . . ? La1 N3 C10 C11 18.4(12) . . . . ? C8 C9 C10 N3 -0.1(12) . . . . ? C8 C9 C10 C11 -177.9(10) . . . . ? C15 N2 C11 C12 0.9(15) . . . . ? La1 N2 C11 C12 -167.8(8) . . . . ? C15 N2 C11 C10 -178.6(9) . . . . ? La1 N2 C11 C10 12.7(12) . . . . ? N3 C10 C11 N2 -21.1(14) . . . . ? C9 C10 C11 N2 156.6(10) . . . . ? N3 C10 C11 C12 159.4(10) . . . . ? C9 C10 C11 C12 -23.0(17) . . . . ? N2 C11 C12 C13 2.2(17) . . . . ? C10 C11 C12 C13 -178.3(10) . . . . ? C11 C12 C13 C14 -2.6(17) . . . . ? C12 C13 C14 C15 0.1(17) . . . . ? C11 N2 C15 C14 -3.5(15) . . . . ? La1 N2 C15 C14 165.3(8) . . . . ? C11 N2 C15 C16 -178.4(9) . . . . ? La1 N2 C15 C16 -9.5(11) . . . . ? C13 C14 C15 N2 3.1(16) . . . . ? C13 C14 C15 C16 177.1(10) . . . . ? La1 O1 C16 N1 150.0(8) . . . . ? La1 O1 C16 C15 -31.1(12) . . . . ? C17 N1 C16 O1 -169.6(10) . . . . ? C19 N1 C16 O1 3.1(15) . . . . ? C17 N1 C16 C15 11.5(17) . . . . ? C19 N1 C16 C15 -175.8(10) . . . . ? N2 C15 C16 O1 24.2(13) . . . . ? C14 C15 C16 O1 -150.4(10) . . . . ? N2 C15 C16 N1 -156.9(10) . . . . ? C14 C15 C16 N1 28.5(16) . . . . ? C16 N1 C17 C18 -107.9(12) . . . . ? C19 N1 C17 C18 79.2(12) . . . . ? C16 N1 C19 C20 -80.2(13) . . . . ? C17 N1 C19 C20 93.3(12) . . . . ? C22 N5 C21 C2 63.7(15) . . . . ? N6 N5 C21 C2 -117.2(11) . . . . ? C1 C2 C21 N5 107.5(11) . . . . ? C3 C2 C21 N5 -73.4(13) . . . . ? N6 N5 C22 C23 0.1(13) . . . . ? C21 N5 C22 C23 179.2(10) . . . . ? N5 C22 C23 C24 -0.9(13) . . . . ? N5 N6 C24 C23 -1.3(11) . . . . ? La2 N6 C24 C23 -179.8(7) . . . . ? N5 N6 C24 C25 -179.8(9) . . . . ? La2 N6 C24 C25 1.7(12) . . . . ? C22 C23 C24 N6 1.4(13) . . . . ? C22 C23 C24 C25 179.8(11) . . . . ? C29 N7 C25 C26 -1.5(16) . . . . ? La2 N7 C25 C26 -178.1(8) . . . . ? C29 N7 C25 C24 179.0(10) . . . . ? La2 N7 C25 C24 2.3(12) . . . . ? N6 C24 C25 N7 -2.7(15) . . . . ? C23 C24 C25 N7 179.1(10) . . . . ? N6 C24 C25 C26 177.7(10) . . . . ? C23 C24 C25 C26 -0.5(18) . . . . ? N7 C25 C26 C27 3.3(19) . . . . ? C24 C25 C26 C27 -177.1(12) . . . . ? C25 C26 C27 C28 -3(2) . . . . ? C26 C27 C28 C29 0(2) . . . . ? C25 N7 C29 C28 -1.0(16) . . . . ? La2 N7 C29 C28 175.7(9) . . . . ? C25 N7 C29 C30 -177.6(9) . . . . ? La2 N7 C29 C30 -0.9(12) . . . . ? C27 C28 C29 N7 1.7(19) . . . . ? C27 C28 C29 C30 177.7(12) . . . . ? La2 O2 C30 N8 150.6(9) . . . . ? La2 O2 C30 C29 -28.9(15) . . . . ? C33 N8 C30 O2 4.5(18) . . . . ? C31 N8 C30 O2 -166.8(12) . . . . ? C33 N8 C30 C29 -176.0(11) . . . . ? C31 N8 C30 C29 13(2) . . . . ? N7 C29 C30 O2 17.3(15) . . . . ? C28 C29 C30 O2 -158.9(12) . . . . ? N7 C29 C30 N8 -162.2(12) . . . . ? C28 C29 C30 N8 22(2) . . . . ? C30 N8 C31 C32 -110.9(16) . . . . ? C33 N8 C31 C32 77.5(16) . . . . ? C30 N8 C33 C34 -86.3(19) . . . . ? C31 N8 C33 C34 85.9(19) . . . . ? C40 C35 C36 C37 -0.3(16) . . . . ? C40 C35 C36 C55 178.9(10) . . . . ? C35 C36 C37 C38 -1.0(16) . . . . ? C55 C36 C37 C38 179.8(10) . . . . ? C36 C37 C38 C39 1.2(16) . . . . ? C37 C38 C39 C40 -0.2(16) . . . . ? C36 C35 C40 C39 1.2(15) . . . . ? C36 C35 C40 C41 -172.7(9) . . . . ? C38 C39 C40 C35 -1.0(15) . . . . ? C38 C39 C40 C41 173.2(9) . . . . ? N11 N12 C41 C40 -91.7(11) . . . . ? C42 N12 C41 C40 85.5(12) . . . . ? C35 C40 C41 N12 -11.1(14) . . . . ? C39 C40 C41 N12 174.9(8) . . . . ? N11 N12 C42 C43 0.9(12) . . . . ? C41 N12 C42 C43 -176.6(9) . . . . ? N12 C42 C43 C44 -0.7(12) . . . . ? N12 N11 C44 C43 0.1(11) . . . . ? La1 N11 C44 C43 -162.1(7) . . . . ? N12 N11 C44 C45 177.6(8) . . . . ? La1 N11 C44 C45 15.3(12) . . . . ? C42 C43 C44 N11 0.4(13) . . . . ? C42 C43 C44 C45 -176.7(11) . . . . ? C49 N10 C45 C46 -2.0(15) . . . . ? La1 N10 C45 C46 -173.2(8) . . . . ? C49 N10 C45 C44 -178.7(9) . . . . ? La1 N10 C45 C44 10.1(12) . . . . ? N11 C44 C45 N10 -16.9(14) . . . . ? C43 C44 C45 N10 160.1(11) . . . . ? N11 C44 C45 C46 166.5(10) . . . . ? C43 C44 C45 C46 -16.6(17) . . . . ? N10 C45 C46 C47 4.6(16) . . . . ? C44 C45 C46 C47 -178.9(10) . . . . ? C45 C46 C47 C48 -3.1(17) . . . . ? C46 C47 C48 C49 -0.6(17) . . . . ? C45 N10 C49 C48 -1.9(15) . . . . ? La1 N10 C49 C48 169.8(8) . . . . ? C45 N10 C49 C50 -175.8(9) . . . . ? La1 N10 C49 C50 -4.1(10) . . . . ? C47 C48 C49 N10 3.2(16) . . . . ? C47 C48 C49 C50 176.3(10) . . . . ? La1 O3 C50 N9 133.0(8) . . . . ? La1 O3 C50 C49 -45.9(11) . . . . ? C51 N9 C50 O3 -168.6(10) . . . . ? C53 N9 C50 O3 3.9(15) . . . . ? C51 N9 C50 C49 10.2(16) . . . . ? C53 N9 C50 C49 -177.2(10) . . . . ? N10 C49 C50 O3 31.2(13) . . . . ? C48 C49 C50 O3 -142.3(11) . . . . ? N10 C49 C50 N9 -147.6(10) . . . . ? C48 C49 C50 N9 38.8(16) . . . . ? C50 N9 C51 C52 -115.1(13) . . . . ? C53 N9 C51 C52 72.3(13) . . . . ? C50 N9 C53 C54 83.2(13) . . . . ? C51 N9 C53 C54 -103.6(12) . . . . ? N14 N13 C55 C36 77.9(13) . . . . ? C56 N13 C55 C36 -92.1(14) . . . . ? C37 C36 C55 N13 -174.6(10) . . . . ? C35 C36 C55 N13 6.1(15) . . . . ? N14 N13 C56 C57 -0.7(14) . . . . ? C55 N13 C56 C57 170.3(11) . . . . ? N13 C56 C57 C58 1.3(15) . . . . ? N13 N14 C58 C57 1.1(13) . . . . ? La2 N14 C58 C57 162.1(8) . . . . ? N13 N14 C58 C59 179.2(9) . . . . ? La2 N14 C58 C59 -19.7(13) . . . . ? C56 C57 C58 N14 -1.5(15) . . . . ? C56 C57 C58 C59 -179.4(12) . . . . ? C63 N15 C59 C60 0.9(16) . . . . ? La2 N15 C59 C60 -156.4(8) . . . . ? C63 N15 C59 C58 -176.3(9) . . . . ? La2 N15 C59 C58 26.5(12) . . . . ? N14 C58 C59 N15 -3.2(15) . . . . ? C57 C58 C59 N15 174.5(12) . . . . ? N14 C58 C59 C60 179.6(11) . . . . ? C57 C58 C59 C60 -2.6(19) . . . . ? N15 C59 C60 C61 1.9(17) . . . . ? C58 C59 C60 C61 178.9(11) . . . . ? C59 C60 C61 C62 -4.2(18) . . . . ? C60 C61 C62 C63 3.7(18) . . . . ? C59 N15 C63 C62 -1.5(16) . . . . ? La2 N15 C63 C62 156.6(9) . . . . ? C59 N15 C63 C64 -177.9(9) . . . . ? La2 N15 C63 C64 -19.7(11) . . . . ? C61 C62 C63 N15 -0.7(17) . . . . ? C61 C62 C63 C64 175.2(11) . . . . ? La2 O4 C64 N16 137.0(9) . . . . ? La2 O4 C64 C63 -41.8(12) . . . . ? C67 N16 C64 O4 -4.2(16) . . . . ? C65 N16 C64 O4 -168.6(10) . . . . ? C67 N16 C64 C63 174.5(10) . . . . ? C65 N16 C64 C63 10.1(16) . . . . ? N15 C63 C64 O4 40.9(13) . . . . ? C62 C63 C64 O4 -135.3(12) . . . . ? N15 C63 C64 N16 -137.9(11) . . . . ? C62 C63 C64 N16 45.8(17) . . . . ? C64 N16 C65 C66 -124.1(12) . . . . ? C67 N16 C65 C66 71.1(14) . . . . ? C64 N16 C67 C68 87.3(14) . . . . ? C65 N16 C67 C68 -107.3(12) . . . . ? La2 O7 C100 O8 -156.3(8) . . . . ? La1 O8 C100 O7 -166.4(7) . . . . ? O12 Cl1 O10 La1 160.3(10) . . . . ? O11 Cl1 O10 La1 39.7(13) . . . . ? O13 Cl1 O10 La1 -79.5(11) . . . . ? O1 La1 O10 Cl1 89.2(10) . . . . ? O8 La1 O10 Cl1 -128.6(9) . . . . ? O3 La1 O10 Cl1 -93.9(11) . . . . ? O6 La1 O10 Cl1 54.6(12) . . . . ? N2 La1 O10 Cl1 25.7(10) . . . . ? N3 La1 O10 Cl1 -31.2(11) . . . . ? N10 La1 O10 Cl1 -158.6(11) . . . . ? N11 La1 O10 Cl1 149.8(10) . . . . ? O17 Cl2 O14 La2 126.1(8) . . . . ? O16 Cl2 O14 La2 -86.9(9) . . . . ? O15' Cl2 O14 La2 27.1(11) . . . . ? O14' Cl2 O14 La2 -164.9(16) . . . . ? O15 Cl2 O14 La2 19.3(9) . . . . ? O15' La2 O14 Cl2 -29.5(11) . . . . ? O7 La2 O14 Cl2 -121.7(8) . . . . ? O2 La2 O14 Cl2 106.6(9) . . . . ? O4 La2 O14 Cl2 81.4(11) . . . . ? O5 La2 O14 Cl2 -80.7(9) . . . . ? N15 La2 O14 Cl2 154.5(8) . . . . ? N7 La2 O14 Cl2 45.2(8) . . . . ? N6 La2 O14 Cl2 -8.9(10) . . . . ? N14 La2 O14 Cl2 -168.1(10) . . . . ? O15 La2 O14 Cl2 -14.3(7) . . . . ? O17 Cl2 O15 La2 -142.3(5) . . . . ? O16 Cl2 O15 La2 102.1(6) . . . . ? O15' Cl2 O15 La2 -24.6(11) . . . . ? O14 Cl2 O15 La2 -16.7(8) . . . . ? O14' Cl2 O15 La2 -23(2) . . . . ? O15' La2 O15 Cl2 27.7(11) . . . . ? O7 La2 O15 Cl2 132.8(5) . . . . ? O2 La2 O15 Cl2 -39.7(7) . . . . ? O4 La2 O15 Cl2 -126.1(6) . . . . ? O5 La2 O15 Cl2 108.5(7) . . . . ? N15 La2 O15 Cl2 -14.9(14) . . . . ? N7 La2 O15 Cl2 -93.1(7) . . . . ? N6 La2 O15 Cl2 -162.8(8) . . . . ? N14 La2 O15 Cl2 36.3(7) . . . . ? O14 La2 O15 Cl2 11.9(6) . . . . ? O17 Cl2 O15' La2 177.9(17) . . . . ? O16 Cl2 O15' La2 26(3) . . . . ? O14 Cl2 O15' La2 -71(2) . . . . ? O14' Cl2 O15' La2 -80(2) . . . . ? O15 Cl2 O15' La2 99(2) . . . . ? O7 La2 O15' Cl2 174.7(17) . . . . ? O2 La2 O15' Cl2 23(2) . . . . ? O4 La2 O15' Cl2 -48(3) . . . . ? O5 La2 O15' Cl2 -176(2) . . . . ? N15 La2 O15' Cl2 68(2) . . . . ? N7 La2 O15' Cl2 -38(2) . . . . ? N6 La2 O15' Cl2 -99(2) . . . . ? N14 La2 O15' Cl2 99(2) . . . . ? O14 La2 O15' Cl2 62(2) . . . . ? O15 La2 O15' Cl2 -89(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.898 _refine_diff_density_min -1.738 _refine_diff_density_rms 0.212 #===END