# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Martin Schroder' _publ_contact_author_address ; School of Chemistry The University of Nottingham University Park Nottingham UNITED KINGDOM ; _publ_contact_author_email M.SCHRODER@NOTTINGHAM.AC.UK _publ_section_title ; Unprecedented Bilayer Topologies in 5- and 6-Connected Frameworks Polymers ; loop_ _publ_author_name 'Martin Schroder' 'Alexander J. Blake' 'Neil Champness' 'Robert J. Hill' 'Peter Hubberstey' ; D.-L.Long ; 'Mark S. Turvey' 'Claire Wilson' data_YBNOPY _database_code_depnum_ccdc_archive 'CCDC 239605' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 N6 O8 Yb, 3(C F3 O3 S)' _chemical_formula_sum 'C33 H24 F9 N6 O17 S3 Yb' _chemical_formula_weight 1216.8 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 orthorhombic _symmetry_space_group_name_H-M Pcca _symmetry_Int_Tables_number 54 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 16.794(3) _cell_length_b 13.764(3) _cell_length_c 20.044(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4633.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5448 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.1 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2396 _exptl_absorpt_coefficient_mu 2.264 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.684 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19315 _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_av_sigmaI/netI 0.075 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.58 _reflns_number_total 5345 _reflns_number_gt 3592 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL; OLEX (Dolomanov, 2003)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _refine_special_details ; ? ; _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^)+(0.0691P)^2^+137.3763P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5345 _refine_ls_number_parameters 268 _refine_ls_number_restraints 119 _refine_ls_R_factor_all 0.1400 _refine_ls_R_factor_gt 0.0965 _refine_ls_wR_factor_ref 0.2489 _refine_ls_wR_factor_gt 0.2217 _refine_ls_goodness_of_fit_ref 1.223 _refine_ls_restrained_S_all 1.215 _refine_ls_shift/su_max 0.017 _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 Yb1 Yb 0.5000 -0.34358(5) 0.7500 0.0155(2) Uani 1 2 d SU . . N1 N 0.3275(6) -0.3100(8) 0.8217(5) 0.020(2) Uani 1 1 d U . . O1 O 0.3732(5) -0.2932(6) 0.7684(4) 0.0180(16) Uani 1 1 d U . . C1 C 0.2552(9) -0.3489(14) 0.8129(7) 0.044(4) Uani 1 1 d U . . H8A H 0.2376 -0.3657 0.7694 0.053 Uiso 1 1 calc R . . N2 N 0.4201(6) -0.3901(7) 0.5982(5) 0.0171(19) Uani 1 1 d U . . O2 O 0.4691(5) -0.4117(6) 0.6483(4) 0.0229(17) Uani 1 1 d U . . C2 C 0.2065(8) -0.3644(14) 0.8668(7) 0.045(5) Uani 1 1 d U . . H9A H 0.1558 -0.3937 0.8603 0.054 Uiso 1 1 calc R . . N3 N 0.4188(6) -0.1492(7) 0.6742(5) 0.0194(19) Uani 1 1 d U . . O3 O 0.4799(4) -0.2124(6) 0.6765(4) 0.0202(17) Uani 1 1 d U . . C3 C 0.2305(7) -0.3375(10) 0.9318(6) 0.026(3) Uani 1 1 d U . . O4 O 0.4202(5) -0.4836(6) 0.7782(4) 0.0181(16) Uani 1 1 d U . . C4 C 0.3054(7) -0.3016(11) 0.9384(6) 0.027(3) Uani 1 1 d U . . H5A H 0.3255 -0.2874 0.9816 0.033 Uiso 1 1 calc R . . C5 C 0.3535(7) -0.2850(10) 0.8825(6) 0.023(3) Uani 1 1 d U . . H4A H 0.4044 -0.2560 0.8877 0.028 Uiso 1 1 calc R . . C6 C 0.4528(7) -0.3795(11) 0.5374(6) 0.028(3) Uani 1 1 d U . . H13A H 0.5090 -0.3830 0.5320 0.034 Uiso 1 1 calc R . . C7 C 0.4043(7) -0.3636(11) 0.4825(6) 0.031(3) Uani 1 1 d U . . H17A H 0.4276 -0.3565 0.4396 0.037 Uiso 1 1 calc R . . C8 C 0.3221(7) -0.3580(10) 0.4892(6) 0.023(3) Uani 1 1 d U . . C9 C 0.2915(7) -0.3691(9) 0.5539(6) 0.021(2) Uani 1 1 d U . . H18A H 0.2356 -0.3658 0.5608 0.025 Uiso 1 1 calc R . . C10 C 0.3409(7) -0.3847(10) 0.6075(6) 0.024(3) Uani 1 1 d U . . H3A H 0.3191 -0.3916 0.6510 0.029 Uiso 1 1 calc R . . C11 C 0.3799(7) -0.1351(7) 0.6149(6) 0.016(2) Uani 1 1 d U . . H16A H 0.3983 -0.1671 0.5758 0.019 Uiso 1 1 calc R . . C12 C 0.3155(7) -0.0758(8) 0.6114(6) 0.019(2) Uani 1 1 d U . . H1A H 0.2897 -0.0656 0.5699 0.023 Uiso 1 1 calc R . . C13 C 0.2868(7) -0.0295(8) 0.6691(6) 0.017(2) Uani 1 1 d U . . C14 C 0.3300(7) -0.0416(8) 0.7271(6) 0.019(2) Uani 1 1 d U . . H7A H 0.3141 -0.0082 0.7665 0.023 Uiso 1 1 calc R . . C15 C 0.3956(7) -0.1014(9) 0.7287(6) 0.022(2) Uani 1 1 d U . . H2A H 0.4247 -0.1087 0.7690 0.027 Uiso 1 1 calc R . . S1A S 0.08271(19) -0.3497(2) 0.64096(15) 0.0258(7) Uiso 1 1 d DU . . F1A F 0.1777(9) -0.2040(13) 0.6444(8) 0.126(6) Uiso 1 1 d DU . . C1A C 0.1060(9) -0.2169(19) 0.6653(7) 0.091(8) Uiso 1 1 d DU . . O1A O 0.0921(6) -0.3538(9) 0.5697(4) 0.053(3) Uiso 1 1 d DU . . S1B S 0.2855(10) -0.0309(14) 0.4123(9) 0.133(7) Uiso 0.50 1 d PDU . . F1B F 0.379(3) 0.053(2) 0.4766(17) 0.19(2) Uiso 0.50 1 d PDU . . C1B C 0.3962(19) -0.0130(17) 0.4344(13) 0.23(5) Uiso 0.50 1 d PDU . . O1B O 0.259(2) 0.0541(19) 0.3760(14) 0.098(11) Uiso 0.50 1 d PDU . . F2A F 0.0553(10) -0.1643(13) 0.6341(8) 0.130(6) Uiso 1 1 d DU . . O2A O 0.1428(5) -0.4022(6) 0.6780(4) 0.028(2) Uiso 1 1 d DU . . F2B F 0.4318(16) 0.0142(19) 0.3819(12) 0.093(8) Uiso 0.50 1 d PDU . . O2B O 0.315(3) -0.108(2) 0.3704(19) 0.23(3) Uiso 0.50 1 d PDU . . F3A F 0.0995(9) -0.2123(12) 0.7286(7) 0.112(5) Uiso 1 1 d DU . . O3A O 0.0022(5) -0.3622(6) 0.6644(4) 0.0296(19) Uiso 1 1 d DU . . F3B F 0.4095(17) -0.0984(17) 0.4553(12) 0.090(8) Uiso 0.50 1 d PDU . . O3B O 0.2344(15) -0.0598(18) 0.4662(11) 0.069(8) Uiso 0.50 1 d PDU . . 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 0.0090(3) 0.0246(4) 0.0127(3) 0.000 0.0000(3) 0.000 N1 0.009(4) 0.030(6) 0.022(4) 0.001(4) 0.004(3) 0.000(4) O1 0.011(4) 0.024(4) 0.019(4) 0.003(3) 0.004(3) 0.002(3) C1 0.021(6) 0.089(13) 0.022(6) -0.009(8) 0.005(5) -0.024(7) N2 0.016(4) 0.020(5) 0.015(4) 0.000(4) -0.005(3) 0.001(4) O2 0.026(4) 0.025(4) 0.018(4) 0.000(3) -0.007(3) 0.002(4) C2 0.015(6) 0.094(14) 0.026(6) -0.019(8) 0.009(5) -0.024(7) N3 0.013(4) 0.020(5) 0.026(5) 0.002(4) 0.001(4) 0.003(4) O3 0.011(4) 0.024(4) 0.026(4) 0.001(3) 0.005(3) 0.009(3) C3 0.018(6) 0.041(8) 0.018(5) 0.004(6) 0.002(4) -0.003(6) O4 0.011(4) 0.024(4) 0.019(4) 0.001(3) 0.002(3) 0.001(3) C4 0.014(6) 0.051(9) 0.017(5) -0.006(6) -0.002(4) 0.001(6) C5 0.016(6) 0.030(7) 0.024(5) 0.005(5) -0.001(4) -0.009(5) C6 0.009(5) 0.054(9) 0.020(5) 0.003(6) -0.002(4) 0.001(6) C7 0.015(5) 0.060(10) 0.016(5) 0.001(6) -0.003(4) 0.003(6) C8 0.013(5) 0.035(7) 0.019(5) -0.001(5) -0.005(4) 0.003(5) C9 0.011(5) 0.024(7) 0.028(6) 0.005(5) 0.000(4) -0.002(5) C10 0.017(5) 0.037(7) 0.019(5) -0.002(5) 0.003(4) 0.000(5) C11 0.021(6) 0.007(5) 0.019(5) -0.002(4) 0.002(4) 0.001(4) C12 0.019(6) 0.017(6) 0.023(5) 0.001(4) -0.002(4) 0.002(4) C13 0.013(5) 0.014(5) 0.025(5) 0.003(4) 0.004(4) 0.001(4) C14 0.022(6) 0.014(5) 0.022(5) -0.003(4) 0.005(4) 0.002(4) C15 0.021(6) 0.024(6) 0.023(5) -0.001(4) -0.002(4) 0.004(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 Yb1 O1 2.270(8) . ? Yb1 O2 2.303(8) . ? Yb1 O3 2.355(8) . ? Yb1 O4 2.414(8) . ? N1 O1 1.335(12) . ? N1 C1 1.338(17) . ? N1 C5 1.340(15) . ? C1 C2 1.372(18) . ? C1 H8A 0.9500 . ? N2 O2 1.331(12) . ? N2 C6 1.345(15) . ? N2 C10 1.346(15) . ? C2 C3 1.415(18) . ? C2 H9A 0.9500 . ? N3 C15 1.333(16) . ? N3 O3 1.346(12) . ? N3 C11 1.370(15) . ? C3 C4 1.358(18) . ? C3 C8 1.476(16) 8_656 ? C4 C5 1.400(17) . ? C4 H5A 0.9500 . ? C5 H4A 0.9500 . ? C6 C7 1.386(17) . ? C6 H13A 0.9500 . ? C7 C8 1.389(17) . ? C7 H17A 0.9500 . ? C8 C9 1.404(17) . ? C9 C10 1.375(17) . ? C9 H18A 0.9500 . ? C10 H3A 0.9500 . ? C11 C12 1.356(16) . ? C11 H16A 0.9500 . ? C12 C13 1.405(16) . ? C12 H1A 0.9500 . ? C13 C14 1.381(17) . ? C13 C13 1.48(2) 2 ? C14 C15 1.376(17) . ? C14 H7A 0.9500 . ? C15 H2A 0.9500 . ? S1A O1A 1.438(8) . ? S1A O3A 1.442(7) . ? S1A O2A 1.445(7) . ? S1A C1A 1.93(3) . ? F1A C1A 1.286(12) . ? C1A F3A 1.275(12) . ? C1A F2A 1.28(3) . ? S1B O3B 1.437(9) . ? S1B O2B 1.443(10) . ? S1B O1B 1.449(9) . ? F1B C1B 1.269(12) . ? C1B F2B 1.267(12) . ? C1B F3B 1.268(12) . ? 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 O1 144.4(4) . 3_656 ? O1 Yb1 O2 93.3(3) . . ? O1 Yb1 O2 101.1(3) 3_656 . ? O2 Yb1 O2 132.0(4) . 3_656 ? O1 Yb1 O3 78.4(3) . 3_656 ? O2 Yb1 O3 153.9(3) . 3_656 ? O1 Yb1 O3 74.5(3) . . ? O2 Yb1 O3 74.1(3) . . ? O3 Yb1 O3 79.9(4) 3_656 . ? O1 Yb1 O4 71.6(3) . . ? O1 Yb1 O4 143.4(3) 3_656 . ? O2 Yb1 O4 75.9(3) . . ? O2 Yb1 O4 66.0(3) 3_656 . ? O3 Yb1 O4 123.0(3) 3_656 . ? O3 Yb1 O4 132.7(3) . . ? O4 Yb1 O4 74.1(4) . 3_656 ? O1 N1 C1 119.0(10) . . ? O1 N1 C5 119.7(9) . . ? C1 N1 C5 121.2(11) . . ? N1 O1 Yb1 128.0(6) . . ? N1 C1 C2 120.0(13) . . ? N1 C1 H8A 120.0 . . ? C2 C1 H8A 120.0 . . ? O2 N2 C6 117.1(9) . . ? O2 N2 C10 121.3(10) . . ? C6 N2 C10 121.5(10) . . ? N2 O2 Yb1 135.7(7) . . ? C1 C2 C3 121.0(12) . . ? C1 C2 H9A 119.5 . . ? C3 C2 H9A 119.5 . . ? C15 N3 O3 120.9(10) . . ? C15 N3 C11 120.1(10) . . ? O3 N3 C11 118.9(9) . . ? N3 O3 Yb1 128.8(6) . . ? C4 C3 C2 116.7(11) . . ? C4 C3 C8 123.3(11) . 8_656 ? C2 C3 C8 119.8(11) . 8_656 ? C3 C4 C5 121.1(12) . . ? C3 C4 H5A 119.5 . . ? C5 C4 H5A 119.5 . . ? N1 C5 C4 119.9(11) . . ? N1 C5 H4A 120.0 . . ? C4 C5 H4A 120.0 . . ? N2 C6 C7 119.7(11) . . ? N2 C6 H13A 120.1 . . ? C7 C6 H13A 120.1 . . ? C6 C7 C8 121.2(12) . . ? C6 C7 H17A 119.4 . . ? C8 C7 H17A 119.4 . . ? C7 C8 C9 116.5(11) . . ? C7 C8 C3 122.0(11) . 8_655 ? C9 C8 C3 121.4(11) . 8_655 ? C10 C9 C8 121.2(11) . . ? C10 C9 H18A 119.4 . . ? C8 C9 H18A 119.4 . . ? N2 C10 C9 119.9(11) . . ? N2 C10 H3A 120.1 . . ? C9 C10 H3A 120.1 . . ? C12 C11 N3 120.6(11) . . ? C12 C11 H16A 119.7 . . ? N3 C11 H16A 119.7 . . ? C11 C12 C13 120.3(11) . . ? C11 C12 H1A 119.8 . . ? C13 C12 H1A 119.8 . . ? C14 C13 C12 117.3(10) . . ? C14 C13 C13 120.3(7) . 2 ? C12 C13 C13 122.4(7) . 2 ? C15 C14 C13 120.8(11) . . ? C15 C14 H7A 119.6 . . ? C13 C14 H7A 119.6 . . ? N3 C15 C14 120.7(11) . . ? N3 C15 H2A 119.6 . . ? C14 C15 H2A 119.6 . . ? O1A S1A O3A 114.9(6) . . ? O1A S1A O2A 114.5(6) . . ? O3A S1A O2A 115.3(5) . . ? O1A S1A C1A 105.4(7) . . ? O3A S1A C1A 102.8(6) . . ? O2A S1A C1A 101.6(6) . . ? F3A C1A F2A 113.7(14) . . ? F3A C1A F1A 113.4(14) . . ? F2A C1A F1A 112.7(14) . . ? F3A C1A S1A 106.3(16) . . ? F2A C1A S1A 106.0(16) . . ? F1A C1A S1A 103.8(16) . . ? O3B S1B O2B 115.8(12) . . ? O3B S1B O1B 114.6(12) . . ? O2B S1B O1B 114.2(12) . . ? O3B S1B C1B 116.0(16) . . ? O1B S1B C1B 108.1(19) . . ? F2B C1B F3B 117.8(14) . . ? F2B C1B F1B 116.8(15) . . ? F3B C1B F1B 118.6(15) . . ? F2B C1B S1B 108(2) . . ? F3B C1B S1B 97(2) . . ? F1B C1B S1B 92(3) . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.37 _refine_diff_density_min -1.57 _refine_diff_density_rms 0.25 data_lapyon _database_code_depnum_ccdc_archive 'CCDC 239606' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 La N7 O13' _chemical_formula_weight 701.31 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.008(8) _cell_length_b 13.389(4) _cell_length_c 13.982(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.29(2) _cell_angle_gamma 90.00 _cell_volume 4853(2) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 30 _cell_measurement_theta_max 32 _exptl_crystal_description column _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.920 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 1.846 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.561 # VALUE FROM DATA SUMMARY SHEET _exptl_absorpt_correction_T_max 0.680 # VALUE FROM DATA SUMMARY SHEET _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 1997b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Stoe Stadi-4 four-circle' _diffrn_measurement_method omega/theta _diffrn_detector_area_resol_mean MoK\a _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'random variation +/-4.4' _diffrn_reflns_number 8938 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4771 _reflns_number_gt 4122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe STADI4 v1.07 (Stoe & Cie, 1997a)' _computing_cell_refinement 'Stoe STADI4' _computing_data_reduction 'X-RED v1.09 (Stoe & Cie, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC v5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXTL/PC v5.03 (Sheldrick, 1994)' _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^)+(0.0197P)^2^+17.8401P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 4771 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0634 _refine_ls_wR_factor_gt 0.0592 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 La La 0.126119(7) 0.724253(13) 0.163378(13) 0.02387(6) Uani 1 1 d . . . O1 O 0.14947(9) 0.87233(16) 0.28499(18) 0.0356(6) Uani 1 1 d . . . O2 O 0.04228(8) 0.78295(18) 0.18573(17) 0.0316(5) Uani 1 1 d . . . O3 O 0.07545(10) 0.58036(16) 0.2090(2) 0.0390(6) Uani 1 1 d . . . O4 O 0.18129(8) 0.66652(18) 0.32851(17) 0.0334(5) Uani 1 1 d . . . O11 O 0.19247(15) 0.5852(3) 0.1505(3) 0.0697(10) Uani 1 1 d . . . O12 O 0.12064(16) 0.5713(2) 0.0366(3) 0.0691(10) Uani 1 1 d . . . O13 O 0.18785(18) 0.4902(2) 0.0230(3) 0.0911(14) Uani 1 1 d . . . O21 O 0.21260(11) 0.8137(3) 0.1605(2) 0.0589(8) Uani 1 1 d . . . O22 O 0.16918(10) 0.7594(2) 0.01761(19) 0.0423(6) Uani 1 1 d . . . O23 O 0.23536(12) 0.8560(2) 0.0297(2) 0.0542(8) Uani 1 1 d . . . O31 O 0.05678(10) 0.74857(19) -0.01206(19) 0.0414(6) Uani 1 1 d . . . O32 O 0.09343(10) 0.88593(19) 0.05270(18) 0.0392(6) Uani 1 1 d . . . O33 O 0.03478(11) 0.8894(2) -0.0894(2) 0.0586(8) Uani 1 1 d . . . N1 N 0.1677(2) 0.5478(2) 0.0694(3) 0.0618(12) Uani 1 1 d . . . N2 N 0.20650(12) 0.8107(2) 0.0673(2) 0.0390(7) Uani 1 1 d . . . N3 N 0.06126(11) 0.8413(2) -0.0177(2) 0.0366(7) Uani 1 1 d . . . N10 N 0.14022(11) 0.9696(2) 0.2755(2) 0.0292(6) Uani 1 1 d . . . N20 N -0.00605(10) 0.7869(2) 0.1286(2) 0.0275(6) Uani 1 1 d . . . N30 N 0.08655(11) 0.4833(2) 0.2197(2) 0.0330(6) Uani 1 1 d . . . N40 N 0.23171(10) 0.6731(2) 0.37038(19) 0.0268(6) Uani 1 1 d . . . C11 C 0.17962(13) 1.0356(3) 0.2989(3) 0.0363(8) Uani 1 1 d . . . H11A H 0.2134 1.0128 0.3209 0.044 Uiso 1 1 calc R . . C12 C 0.16995(14) 1.1362(3) 0.2904(3) 0.0374(8) Uani 1 1 d . . . H12A H 0.1974 1.1809 0.3078 0.045 Uiso 1 1 calc R . . C13 C 0.11997(13) 1.1729(2) 0.2564(2) 0.0287(7) Uani 1 1 d . . . C14 C 0.08073(13) 1.1024(2) 0.2341(3) 0.0342(8) Uani 1 1 d . . . H14A H 0.0466 1.1235 0.2114 0.041 Uiso 1 1 calc R . . C15 C 0.09134(13) 1.0024(3) 0.2451(3) 0.0348(8) Uani 1 1 d . . . H15A H 0.0644 0.9567 0.2313 0.042 Uiso 1 1 calc R . . C21 C -0.02494(13) 0.8741(3) 0.0863(3) 0.0335(8) Uani 1 1 d . . . H21A H -0.0033 0.9293 0.0936 0.040 Uiso 1 1 calc R . . C22 C -0.07578(13) 0.8827(3) 0.0323(3) 0.0347(8) Uani 1 1 d . . . H22A H -0.0882 0.9435 0.0032 0.042 Uiso 1 1 calc R . . C23 C -0.10872(12) 0.8015(2) 0.0210(2) 0.0279(7) Uani 1 1 d . . . C24 C -0.08774(12) 0.7114(3) 0.0636(2) 0.0316(7) Uani 1 1 d . . . H24A H -0.1084 0.6548 0.0559 0.038 Uiso 1 1 calc R . . C25 C -0.03646(12) 0.7056(2) 0.1173(3) 0.0317(7) Uani 1 1 d . . . H25A H -0.0229 0.6453 0.1458 0.038 Uiso 1 1 calc R . . C31 C 0.05360(15) 0.4163(3) 0.1643(3) 0.0439(10) Uani 1 1 d . . . H31A H 0.0238 0.4383 0.1176 0.053 Uiso 1 1 calc R . . C32 C 0.06357(14) 0.3163(3) 0.1761(3) 0.0422(9) Uani 1 1 d . . . H32A H 0.0400 0.2711 0.1380 0.051 Uiso 1 1 calc R . . C33 C 0.10842(13) 0.2804(2) 0.2444(2) 0.0292(7) Uani 1 1 d . . . C34 C 0.14104(15) 0.3520(3) 0.2997(3) 0.0414(9) Uani 1 1 d . . . H34A H 0.1713 0.3322 0.3463 0.050 Uiso 1 1 calc R . . C35 C 0.12944(15) 0.4525(3) 0.2869(3) 0.0439(10) Uani 1 1 d . . . H35A H 0.1518 0.4992 0.3256 0.053 Uiso 1 1 calc R . . C41 C 0.25888(13) 0.5901(2) 0.4059(3) 0.0325(7) Uani 1 1 d . . . H41A H 0.2426 0.5282 0.3973 0.039 Uiso 1 1 calc R . . C42 C 0.31060(13) 0.5966(3) 0.4549(3) 0.0338(8) Uani 1 1 d . . . H42A H 0.3288 0.5391 0.4805 0.041 Uiso 1 1 calc R . . C43 C 0.33600(12) 0.6880(3) 0.4667(2) 0.0294(7) Uani 1 1 d . . . C44 C 0.30668(13) 0.7712(2) 0.4262(3) 0.0337(8) Uani 1 1 d . . . H44A H 0.3224 0.8335 0.4310 0.040 Uiso 1 1 calc R . . C45 C 0.25501(13) 0.7627(2) 0.3794(3) 0.0337(8) Uani 1 1 d . . . H45A H 0.2359 0.8193 0.3536 0.040 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 La 0.02001(9) 0.01856(9) 0.02959(10) 0.00109(7) 0.00131(7) 0.00168(7) O1 0.0385(13) 0.0176(11) 0.0434(14) -0.0017(10) -0.0004(11) 0.0054(10) O2 0.0183(10) 0.0340(13) 0.0371(12) 0.0030(10) -0.0010(9) 0.0031(10) O3 0.0366(13) 0.0154(11) 0.0627(17) 0.0050(11) 0.0101(12) 0.0025(10) O4 0.0190(11) 0.0330(13) 0.0408(13) 0.0047(11) -0.0038(9) 0.0006(10) O11 0.085(3) 0.067(2) 0.060(2) 0.0084(18) 0.0271(19) 0.043(2) O12 0.093(3) 0.0424(17) 0.079(2) -0.0201(17) 0.037(2) -0.0105(19) O13 0.160(4) 0.0324(16) 0.121(3) -0.0025(19) 0.105(3) 0.016(2) O21 0.0484(17) 0.090(2) 0.0375(15) -0.0094(16) 0.0102(13) -0.0305(17) O22 0.0352(14) 0.0491(16) 0.0409(14) -0.0064(12) 0.0082(11) -0.0079(12) O23 0.0543(18) 0.0527(18) 0.0627(19) 0.0022(14) 0.0279(15) -0.0154(15) O31 0.0380(14) 0.0383(15) 0.0409(14) -0.0009(11) -0.0005(11) -0.0032(11) O32 0.0424(14) 0.0291(12) 0.0384(13) 0.0045(11) -0.0012(11) 0.0004(11) O33 0.0505(17) 0.066(2) 0.0473(16) 0.0260(15) -0.0064(14) 0.0095(16) N1 0.105(4) 0.0234(17) 0.078(3) 0.0108(18) 0.060(3) 0.014(2) N2 0.0359(16) 0.0363(17) 0.0465(18) -0.0025(14) 0.0144(14) -0.0012(14) N3 0.0326(16) 0.0414(18) 0.0343(15) 0.0098(14) 0.0068(13) 0.0079(14) N10 0.0304(15) 0.0224(13) 0.0305(14) 0.0012(11) 0.0016(11) 0.0030(11) N20 0.0205(12) 0.0289(14) 0.0315(14) 0.0046(11) 0.0044(11) 0.0045(11) N30 0.0346(16) 0.0188(13) 0.0444(16) 0.0006(12) 0.0092(13) -0.0017(12) N40 0.0230(13) 0.0270(13) 0.0260(13) 0.0017(11) -0.0003(10) -0.0001(11) C11 0.0278(17) 0.0269(17) 0.048(2) 0.0004(15) 0.0001(15) 0.0018(14) C12 0.0293(18) 0.0273(18) 0.051(2) 0.0018(16) 0.0033(16) -0.0033(14) C13 0.0326(17) 0.0210(15) 0.0313(16) 0.0003(13) 0.0071(13) 0.0022(13) C14 0.0277(17) 0.0251(16) 0.045(2) 0.0005(15) 0.0020(15) 0.0010(14) C15 0.0306(18) 0.0228(16) 0.046(2) -0.0026(15) 0.0030(15) -0.0008(14) C21 0.0249(16) 0.0261(16) 0.045(2) 0.0057(15) 0.0028(14) 0.0008(14) C22 0.0271(17) 0.0280(17) 0.044(2) 0.0082(15) 0.0019(15) 0.0047(14) C23 0.0206(15) 0.0309(17) 0.0300(16) 0.0011(13) 0.0037(12) 0.0006(13) C24 0.0251(16) 0.0291(17) 0.0366(17) 0.0023(14) 0.0021(14) -0.0010(14) C25 0.0276(16) 0.0253(17) 0.0392(18) 0.0034(14) 0.0042(14) 0.0030(13) C31 0.038(2) 0.0298(19) 0.051(2) 0.0006(17) -0.0075(17) 0.0028(16) C32 0.042(2) 0.0249(17) 0.048(2) -0.0063(16) -0.0071(17) -0.0022(16) C33 0.0331(17) 0.0209(15) 0.0321(16) 0.0014(13) 0.0066(14) -0.0001(14) C34 0.038(2) 0.0234(17) 0.053(2) 0.0024(16) -0.0047(17) -0.0014(15) C35 0.040(2) 0.0254(18) 0.054(2) -0.0019(16) -0.0078(18) -0.0035(16) C41 0.0286(17) 0.0218(16) 0.0423(19) 0.0049(14) 0.0022(15) -0.0014(13) C42 0.0240(16) 0.0265(17) 0.045(2) 0.0065(15) 0.0000(14) 0.0011(13) C43 0.0242(15) 0.0298(17) 0.0308(16) -0.0008(14) 0.0019(13) 0.0002(14) C44 0.0304(17) 0.0205(15) 0.0445(19) -0.0009(15) 0.0012(15) -0.0013(14) C45 0.0306(17) 0.0230(16) 0.0401(19) 0.0023(14) -0.0021(15) 0.0017(14) _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 La O1 2.573(2) . ? La O2 2.498(2) . ? La O3 2.546(2) . ? La O4 2.494(2) . ? La O11 2.626(3) . ? La O12 2.686(3) . ? La O21 2.635(3) . ? La O22 2.657(3) . ? La O31 2.656(3) . ? La O32 2.663(2) . ? O1 N10 1.326(3) . ? O2 N20 1.326(3) . ? O3 N30 1.332(3) . ? O4 N40 1.326(3) . ? O11 N1 1.248(5) . ? O12 N1 1.265(5) . ? O13 N1 1.228(4) . ? O21 N2 1.267(4) . ? O22 N2 1.256(4) . ? O23 N2 1.218(4) . ? O31 N3 1.252(4) . ? O32 N3 1.265(4) . ? O33 N3 1.236(4) . ? N10 C15 1.342(4) . ? N10 C11 1.351(4) . ? N20 C21 1.343(4) . ? N20 C25 1.345(4) . ? N30 C35 1.336(4) . ? N30 C31 1.345(4) . ? N40 C45 1.345(4) . ? N40 C41 1.347(4) . ? C11 C12 1.371(5) . ? C12 C13 1.389(5) . ? C13 C14 1.387(5) . ? C13 C33 1.473(4) 1_565 ? C14 C15 1.369(5) . ? C21 C22 1.374(4) . ? C22 C23 1.386(5) . ? C23 C24 1.393(4) . ? C23 C43 1.480(4) 8_465 ? C24 C25 1.380(4) . ? C31 C32 1.367(5) . ? C32 C33 1.400(5) . ? C33 C34 1.382(5) . ? C33 C13 1.473(4) 1_545 ? C34 C35 1.381(5) . ? C41 C42 1.375(5) . ? C42 C43 1.390(5) . ? C43 C44 1.391(5) . ? C43 C23 1.480(4) 8_566 ? C44 C45 1.370(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 O2 La O1 74.79(8) . . ? O3 La O1 117.83(9) . . ? O4 La O1 69.81(8) . . ? O4 La O2 107.99(8) . . ? O2 La O3 68.71(8) . . ? O4 La O3 75.94(8) . . ? O4 La O11 66.53(10) . . ? O2 La O11 153.11(10) . . ? O3 La O11 84.59(11) . . ? O1 La O11 123.13(11) . . ? O4 La O21 81.55(9) . . ? O2 La O21 134.21(10) . . ? O3 La O21 152.73(10) . . ? O1 La O21 66.78(9) . . ? O11 La O21 72.33(12) . . ? O4 La O31 167.58(8) . . ? O2 La O31 69.38(8) . . ? O3 La O31 92.00(8) . . ? O1 La O31 119.65(8) . . ? O11 La O31 109.97(10) . . ? O21 La O31 109.18(9) . . ? O4 La O22 119.26(8) . . ? O2 La O22 130.35(8) . . ? O3 La O22 135.09(8) . . ? O1 La O22 106.95(8) . . ? O11 La O22 67.60(10) . . ? O21 La O22 47.71(8) . . ? O31 La O22 67.46(9) . . ? O4 La O32 143.56(8) . . ? O2 La O32 69.67(8) . . ? O3 La O32 130.30(8) . . ? O1 La O32 74.78(8) . . ? O11 La O32 131.14(10) . . ? O21 La O32 76.85(10) . . ? O31 La O32 47.99(8) . . ? O22 La O32 63.59(8) . . ? O4 La O12 106.43(11) . . ? O2 La O12 116.01(10) . . ? O3 La O12 69.78(10) . . ? O1 La O12 169.10(10) . . ? O11 La O12 47.62(12) . . ? O21 La O12 102.80(11) . . ? O31 La O12 65.78(11) . . ? O22 La O12 65.39(10) . . ? O32 La O12 106.75(10) . . ? N10 O1 La 133.35(18) . . ? N20 O2 La 135.29(19) . . ? N30 O3 La 130.3(2) . . ? N40 O4 La 131.41(19) . . ? N1 O11 La 98.3(3) . . ? N1 O12 La 95.0(3) . . ? N2 O21 La 98.1(2) . . ? N2 O22 La 97.4(2) . . ? N3 O31 La 97.14(19) . . ? N3 O32 La 96.42(19) . . ? O13 N1 O11 121.8(5) . . ? O13 N1 O12 120.9(5) . . ? O11 N1 O12 117.2(4) . . ? O13 N1 La 168.5(3) . . ? O11 N1 La 57.9(2) . . ? O12 N1 La 60.8(2) . . ? O23 N2 O22 123.0(3) . . ? O23 N2 O21 120.9(3) . . ? O22 N2 O21 116.1(3) . . ? O33 N3 O31 121.5(3) . . ? O33 N3 O32 120.0(3) . . ? O31 N3 O32 118.5(3) . . ? O1 N10 C15 119.6(3) . . ? O1 N10 C11 120.3(3) . . ? C15 N10 C11 120.0(3) . . ? O2 N20 C21 119.2(3) . . ? O2 N20 C25 120.3(3) . . ? C21 N20 C25 120.5(3) . . ? O3 N30 C35 120.3(3) . . ? O3 N30 C31 119.6(3) . . ? C35 N30 C31 120.1(3) . . ? O4 N40 C45 119.7(3) . . ? O4 N40 C41 119.6(3) . . ? C45 N40 C41 120.6(3) . . ? N10 C11 C12 120.3(3) . . ? C11 C12 C13 121.3(3) . . ? C14 C13 C12 116.4(3) . . ? C14 C13 C33 121.0(3) . 1_565 ? C12 C13 C33 122.6(3) . 1_565 ? C15 C14 C13 121.1(3) . . ? N10 C15 C14 120.8(3) . . ? N20 C21 C22 120.8(3) . . ? C21 C22 C23 120.5(3) . . ? C22 C23 C24 117.3(3) . . ? C22 C23 C43 120.5(3) . 8_465 ? C24 C23 C43 122.2(3) . 8_465 ? C25 C24 C23 120.5(3) . . ? N20 C25 C24 120.3(3) . . ? N30 C31 C32 120.5(3) . . ? C31 C32 C33 121.5(3) . . ? C34 C33 C32 115.9(3) . . ? C34 C33 C13 122.2(3) . 1_545 ? C32 C33 C13 121.9(3) . 1_545 ? C35 C34 C33 121.1(3) . . ? N30 C35 C34 120.8(3) . . ? N40 C41 C42 120.2(3) . . ? C41 C42 C43 120.9(3) . . ? C42 C43 C44 116.8(3) . . ? C42 C43 C23 122.6(3) . 8_566 ? C44 C43 C23 120.6(3) . 8_566 ? C45 C44 C43 121.1(3) . . ? N40 C45 C44 120.4(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.353 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.085 #=== END of CIF data_ERNOI1 _database_code_depnum_ccdc_archive 'CCDC 239607' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H43 Er I9 N11 O13' _chemical_formula_weight 2387.37 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 43.203(8) _cell_length_b 19.245(4) _cell_length_c 17.168(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14274(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13082 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 27.4 _exptl_crystal_description 'trigonal prism' _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8840 _exptl_absorpt_coefficient_mu 5.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.575 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 106550 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_sigmaI/netI 0.033 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 27.45 _reflns_number_total 15426 _reflns_number_gt 14261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.625' _computing_cell_refinement 'Bruker SMART v5.625' _computing_data_reduction 'Bruker SAINT v6.36a, SHELXTL v6.12' _computing_structure_solution SIR-92 _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^)+(0.022P)^2^+470.0P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15426 _refine_ls_number_parameters 812 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.169 _refine_ls_wR_factor_gt 0.166 _refine_ls_goodness_of_fit_ref 1.305 _refine_ls_restrained_S_all 1.305 _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 Er1 Er -0.143550(11) -0.25042(2) -0.49196(2) 0.01145(11) Uani 1 1 d . . . O1 O -0.10185(19) -0.2423(4) -0.4025(5) 0.0237(18) Uani 1 1 d . . . N2 N -0.0717(2) -0.2478(5) -0.4140(6) 0.022(2) Uani 1 1 d . . . C3 C -0.0593(3) -0.3087(6) -0.4397(7) 0.021(2) Uani 1 1 d . . . H3A H -0.0723 -0.3477 -0.4486 0.026 Uiso 1 1 calc R . . C4 C -0.0276(3) -0.3136(6) -0.4527(7) 0.021(2) Uani 1 1 d . . . H4A H -0.0190 -0.3565 -0.4695 0.025 Uiso 1 1 calc R . . C5 C -0.0080(3) -0.2557(6) -0.4415(7) 0.020(2) Uani 1 1 d . . . C6 C -0.0220(3) -0.1965(6) -0.4124(7) 0.024(2) Uani 1 1 d . . . H6A H -0.0094 -0.1576 -0.4006 0.028 Uiso 1 1 calc R . . C7 C -0.0532(3) -0.1915(6) -0.3999(6) 0.019(2) Uani 1 1 d . . . H7A H -0.0619 -0.1492 -0.3816 0.022 Uiso 1 1 calc R . . C8 C 0.0254(3) -0.2601(6) -0.4584(7) 0.020(2) Uani 1 1 d . . . C9 C 0.0403(3) -0.3232(7) -0.4663(7) 0.026(3) Uani 1 1 d . . . H9A H 0.0290 -0.3646 -0.4564 0.032 Uiso 1 1 calc R . . C10 C 0.0711(3) -0.3282(7) -0.4881(8) 0.030(3) Uani 1 1 d . . . H10A H 0.0806 -0.3724 -0.4938 0.037 Uiso 1 1 calc R . . N11 N 0.0876(3) -0.2697(6) -0.5012(7) 0.036(3) Uani 1 1 d . . . C12 C 0.0738(3) -0.2054(7) -0.4917(9) 0.037(3) Uani 1 1 d . . . H12A H 0.0857 -0.1644 -0.4986 0.044 Uiso 1 1 calc R . . C13 C 0.0431(3) -0.2002(7) -0.4723(8) 0.028(3) Uani 1 1 d . . . H13A H 0.0337 -0.1557 -0.4683 0.033 Uiso 1 1 calc R . . O14 O 0.1160(2) -0.2750(6) -0.5274(7) 0.050(3) Uani 1 1 d . . . O15 O -0.10458(19) -0.2583(4) -0.5851(5) 0.0230(17) Uani 1 1 d . . . N16 N -0.0758(2) -0.2425(5) -0.6020(5) 0.020(2) Uani 1 1 d . . . C17 C -0.0585(3) -0.2920(6) -0.6374(8) 0.025(3) Uani 1 1 d . . . H17A H -0.0672 -0.3361 -0.6494 0.030 Uiso 1 1 calc R . . C18 C -0.0281(3) -0.2770(6) -0.6557(7) 0.021(2) Uani 1 1 d . . . H18A H -0.0158 -0.3122 -0.6791 0.026 Uiso 1 1 calc R . . C19 C -0.0147(3) -0.2122(6) -0.6413(6) 0.022(2) Uani 1 1 d . . . C20 C -0.0343(3) -0.1624(6) -0.6080(7) 0.026(3) Uani 1 1 d . . . H20A H -0.0269 -0.1166 -0.5991 0.032 Uiso 1 1 calc R . . C21 C -0.0641(3) -0.1798(6) -0.5883(7) 0.026(3) Uani 1 1 d . . . H21A H -0.0768 -0.1459 -0.5640 0.031 Uiso 1 1 calc R . . C22 C 0.0177(3) -0.1983(6) -0.6603(7) 0.022(2) Uani 1 1 d . . . C23 C 0.0398(3) -0.2515(7) -0.6608(8) 0.030(3) Uani 1 1 d . . . H23A H 0.0336 -0.2971 -0.6467 0.036 Uiso 1 1 calc R . . C24 C 0.0701(3) -0.2400(6) -0.6811(8) 0.027(3) Uani 1 1 d . . . H24A H 0.0844 -0.2775 -0.6827 0.032 Uiso 1 1 calc R . . N25 N 0.0793(2) -0.1748(5) -0.6986(6) 0.025(2) Uani 1 1 d . . . C26 C 0.0589(3) -0.1206(7) -0.6985(8) 0.030(3) Uani 1 1 d . . . H26A H 0.0656 -0.0754 -0.7125 0.036 Uiso 1 1 calc R . . C27 C 0.0287(3) -0.1317(6) -0.6783(7) 0.024(3) Uani 1 1 d . . . H27A H 0.0148 -0.0933 -0.6764 0.028 Uiso 1 1 calc R . . O28 O 0.1083(2) -0.1637(5) -0.7199(6) 0.036(2) Uani 1 1 d . . . O29 O -0.12694(18) -0.1352(4) -0.4959(5) 0.0186(16) Uani 1 1 d . . . N30 N -0.1351(2) -0.0860(5) -0.5466(5) 0.0156(18) Uani 1 1 d . . . C31 C -0.1420(3) -0.0228(5) -0.5203(7) 0.020(2) Uani 1 1 d . . . H31A H -0.1421 -0.0145 -0.4658 0.025 Uiso 1 1 calc R . . C32 C -0.1490(3) 0.0308(6) -0.5704(7) 0.019(2) Uani 1 1 d . . . H32A H -0.1550 0.0747 -0.5501 0.023 Uiso 1 1 calc R . . C33 C -0.1474(3) 0.0211(6) -0.6503(6) 0.018(2) Uani 1 1 d . . . C34 C -0.1405(3) -0.0461(6) -0.6762(7) 0.022(2) Uani 1 1 d . . . H34A H -0.1400 -0.0552 -0.7306 0.026 Uiso 1 1 calc R . . C35 C -0.1343(3) -0.0995(6) -0.6249(7) 0.020(2) Uani 1 1 d . . . H35A H -0.1296 -0.1447 -0.6435 0.024 Uiso 1 1 calc R . . C36 C -0.1517(3) 0.0783(6) -0.7074(6) 0.020(2) Uani 1 1 d . . . C37 C -0.1458(3) -0.1467(6) -0.1884(8) 0.031(3) Uani 1 1 d . . . H37A H -0.1397 -0.1584 -0.1369 0.047 Uiso 1 1 calc R . . C38 C -0.1486(3) -0.1983(6) -0.2445(8) 0.030(3) Uani 1 1 d . . . H38A H -0.1438 -0.2450 -0.2313 0.036 Uiso 1 1 calc R . . N39 N -0.1577(2) -0.1834(5) -0.3162(5) 0.0156(19) Uani 1 1 d . . . C40 C -0.1658(3) -0.1177(6) -0.3358(7) 0.025(3) Uani 1 1 d . . . H40A H -0.1739 -0.1081 -0.3862 0.030 Uiso 1 1 calc R . . C41 C -0.1623(4) -0.0644(7) -0.2819(8) 0.033(3) Uani 1 1 d . . . O42 O -0.16104(18) -0.2349(4) -0.3675(4) 0.0165(15) Uani 1 1 d . . . O43 O -0.16357(18) -0.2681(4) -0.6149(4) 0.0167(16) Uani 1 1 d . . . N44 N -0.1586(2) -0.3181(5) -0.6660(5) 0.0171(19) Uani 1 1 d . . . C45 C -0.1484(3) -0.3022(6) -0.7384(7) 0.021(2) Uani 1 1 d . . . H45A H -0.1444 -0.2551 -0.7514 0.025 Uiso 1 1 calc R . . C46 C -0.1439(3) -0.3533(6) -0.7936(6) 0.020(2) Uani 1 1 d . . . H46A H -0.1369 -0.3412 -0.8443 0.031 Uiso 1 1 calc R . . C47 C -0.1497(2) -0.5769(5) -0.2749(6) 0.015(2) Uani 1 1 d . . . C48 C -0.1601(3) -0.5630(5) -0.1994(6) 0.020(2) Uani 1 1 d . . . H48A H -0.1641 -0.5164 -0.1843 0.030 Uiso 1 1 calc R . . C49 C -0.1647(3) -0.3846(6) -0.6470(6) 0.021(2) Uani 1 1 d . . . H49A H -0.1722 -0.3953 -0.5964 0.032 Uiso 1 1 calc R . . C50 C -0.1447(3) -0.5212(5) -0.3322(7) 0.017(2) Uani 1 1 d . . . C51 C -0.1384(3) -0.4533(6) -0.3080(7) 0.020(2) Uani 1 1 d . . . H51A H -0.1383 -0.4427 -0.2539 0.024 Uiso 1 1 calc R . . C52 C -0.1323(3) -0.4012(5) -0.3616(7) 0.019(2) Uani 1 1 d . . . H52A H -0.1284 -0.3552 -0.3442 0.022 Uiso 1 1 calc R . . N53 N -0.1320(2) -0.4154(5) -0.4376(5) 0.0165(19) Uani 1 1 d . . . C54 C -0.1386(3) -0.4797(5) -0.4647(6) 0.016(2) Uani 1 1 d . . . H54A H -0.1392 -0.4885 -0.5191 0.019 Uiso 1 1 calc R . . C55 C -0.1445(3) -0.5326(6) -0.4117(6) 0.017(2) Uani 1 1 d . . . H55A H -0.1485 -0.5780 -0.4307 0.020 Uiso 1 1 calc R . . O56 O -0.12543(19) -0.3656(4) -0.4892(5) 0.0192(17) Uani 1 1 d . . . O57 O -0.18764(18) -0.1740(4) -0.5078(4) 0.0145(15) Uani 1 1 d . . . N58 N -0.2071(2) -0.1708(5) -0.5675(5) 0.0174(19) Uani 1 1 d . . . C59 C -0.2229(3) -0.2279(5) -0.5904(7) 0.018(2) Uani 1 1 d . . . H59A H -0.2218 -0.2695 -0.5607 0.026 Uiso 1 1 calc R . . C60 C -0.2713(3) -0.3948(6) -0.1689(7) 0.022(2) Uani 1 1 d . . . H60A H -0.2692 -0.4383 -0.1947 0.033 Uiso 1 1 calc R . . C61 C -0.2564(3) -0.3367(5) -0.1992(7) 0.017(2) Uani 1 1 d . . . C62 C -0.2594(3) -0.2747(5) -0.1563(7) 0.016(2) Uani 1 1 d . . . H62A H -0.2489 -0.2341 -0.1734 0.025 Uiso 1 1 calc R . . C63 C -0.2113(3) -0.1093(6) -0.6035(7) 0.020(2) Uani 1 1 d . . . H63A H -0.2020 -0.0685 -0.5828 0.030 Uiso 1 1 calc R . . C64 C -0.2395(3) -0.3362(6) -0.2742(7) 0.019(2) Uani 1 1 d . . . C65 C -0.2251(3) -0.3954(6) -0.3050(7) 0.021(2) Uani 1 1 d . . . H65A H -0.2273 -0.4385 -0.2785 0.026 Uiso 1 1 calc R . . C66 C -0.2081(3) -0.3932(6) -0.3716(7) 0.018(2) Uani 1 1 d . . . H66A H -0.1983 -0.4340 -0.3909 0.022 Uiso 1 1 calc R . . N67 N -0.2051(2) -0.3319(5) -0.4102(6) 0.0172(19) Uani 1 1 d . . . C68 C -0.2205(3) -0.2744(5) -0.3868(6) 0.015(2) Uani 1 1 d . . . H68A H -0.2194 -0.2332 -0.4172 0.019 Uiso 1 1 calc R . . C69 C -0.2377(3) -0.2751(6) -0.3192(7) 0.022(2) Uani 1 1 d . . . H69A H -0.2484 -0.2344 -0.3029 0.027 Uiso 1 1 calc R . . O70 O -0.18653(17) -0.3284(4) -0.4707(4) 0.0138(15) Uani 1 1 d . . . O71 O -0.1097(2) -0.3266(5) -0.1911(6) 0.030(2) Uani 1 1 d . . . N72 N -0.0802(2) -0.3256(5) -0.2108(6) 0.025(2) Uani 1 1 d . . . C73 C -0.0647(3) -0.3847(7) -0.2239(9) 0.032(3) Uani 1 1 d . . . H73A H -0.0754 -0.4277 -0.2226 0.038 Uiso 1 1 calc R . . C74 C -0.0337(3) -0.3843(6) -0.2392(7) 0.024(3) Uani 1 1 d . . . H74A H -0.0234 -0.4270 -0.2486 0.029 Uiso 1 1 calc R . . C75 C -0.0171(3) -0.3230(6) -0.2412(7) 0.023(2) Uani 1 1 d . . . C76 C -0.0336(3) -0.2617(6) -0.2301(7) 0.026(3) Uani 1 1 d . . . H76A H -0.0233 -0.2182 -0.2334 0.032 Uiso 1 1 calc R . . C77 C -0.0651(3) -0.2639(6) -0.2142(7) 0.027(3) Uani 1 1 d . . . H77A H -0.0761 -0.2219 -0.2056 0.032 Uiso 1 1 calc R . . I78 I -0.06342(2) -0.52050(4) -0.06408(5) 0.03016(19) Uani 1 1 d . . . I79 I 0.00007(2) -0.53684(4) -0.11772(5) 0.02589(17) Uani 1 1 d . . . I80 I 0.06297(2) -0.55924(4) -0.17591(6) 0.0314(2) Uani 1 1 d . . . I81 I -0.06429(2) -0.06266(5) -0.19952(7) 0.0432(2) Uani 1 1 d . . . I82 I 0.0000 -0.05982(6) -0.2500 0.0304(3) Uani 1 2 d S . . I83 I -0.06560(2) -0.00337(5) -0.46214(6) 0.0373(2) Uani 1 1 d . . . I84 I 0.0000 0.0000 -0.5000 0.0317(3) Uani 1 2 d S . . I85 I -0.26401(3) -0.09089(6) -0.41817(6) 0.0479(3) Uani 1 1 d . . . I86 I -0.25423(2) -0.08641(4) -0.24991(6) 0.0328(2) Uani 1 1 d . . . I87 I -0.24620(3) -0.07773(6) -0.08181(7) 0.0597(4) Uani 1 1 d . . . O88 O -0.1463(3) -0.4140(6) -0.1062(6) 0.051(3) Uani 1 1 d . . . C89 C -0.1739(5) -0.3750(12) -0.1066(13) 0.067(6) Uani 1 1 d . . . O90 O -0.3395(4) -0.3165(9) -0.4733(10) 0.025(4) Uiso 0.50 1 d P . . O91 O -0.1680(5) -0.0768(12) -0.8736(14) 0.049(6) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0169(2) 0.0076(2) 0.0098(2) 0.00022(16) 0.00019(17) 0.00010(17) O1 0.025(4) 0.017(4) 0.029(5) -0.003(3) -0.008(4) 0.002(3) N2 0.023(5) 0.022(5) 0.021(5) -0.001(4) -0.007(4) 0.000(4) C3 0.017(6) 0.023(6) 0.024(6) 0.000(5) -0.004(5) 0.000(4) C4 0.021(6) 0.018(6) 0.023(6) -0.002(5) -0.004(5) 0.000(4) C5 0.024(6) 0.011(5) 0.026(6) 0.007(4) -0.003(5) 0.000(4) C6 0.032(7) 0.021(6) 0.018(6) -0.002(5) -0.006(5) -0.004(5) C7 0.025(6) 0.016(5) 0.015(5) -0.003(4) -0.003(4) -0.007(4) C8 0.019(6) 0.023(6) 0.018(5) -0.002(4) -0.005(4) 0.001(5) C9 0.027(6) 0.025(6) 0.027(6) 0.010(5) 0.010(5) -0.001(5) C10 0.029(7) 0.026(7) 0.036(7) -0.003(6) 0.006(6) 0.009(5) N11 0.027(6) 0.038(7) 0.043(7) 0.001(5) -0.001(5) 0.003(5) C12 0.033(7) 0.026(7) 0.052(9) 0.001(6) -0.005(7) -0.007(6) C13 0.036(7) 0.020(6) 0.027(7) 0.003(5) -0.007(5) -0.005(5) O14 0.027(5) 0.055(7) 0.068(8) 0.019(6) 0.013(5) -0.004(5) O15 0.021(4) 0.024(4) 0.024(4) 0.004(3) 0.006(3) -0.001(3) N16 0.019(5) 0.026(5) 0.014(4) 0.003(4) 0.005(4) 0.003(4) C17 0.028(6) 0.015(5) 0.032(7) 0.006(5) 0.001(5) 0.001(5) C18 0.027(6) 0.015(5) 0.021(6) 0.003(4) 0.005(5) -0.001(5) C19 0.035(7) 0.019(6) 0.011(5) 0.006(4) -0.002(5) -0.006(5) C20 0.032(7) 0.020(6) 0.027(7) 0.001(5) -0.003(5) 0.002(5) C21 0.035(7) 0.019(6) 0.023(6) -0.002(5) -0.002(5) -0.001(5) C22 0.026(6) 0.025(6) 0.015(5) 0.003(5) -0.003(5) 0.005(5) C23 0.038(7) 0.020(6) 0.032(7) 0.009(5) 0.008(6) -0.001(5) C24 0.031(7) 0.013(6) 0.037(7) 0.003(5) 0.006(5) 0.000(5) N25 0.027(5) 0.021(5) 0.027(5) 0.000(4) 0.008(4) 0.002(4) C26 0.034(7) 0.023(6) 0.033(7) 0.010(5) 0.001(6) 0.004(5) C27 0.028(6) 0.023(6) 0.020(6) -0.001(5) 0.003(5) 0.007(5) O28 0.034(5) 0.033(5) 0.042(6) 0.001(4) 0.017(4) -0.005(4) O29 0.022(4) 0.009(3) 0.026(4) 0.008(3) -0.004(3) 0.000(3) N30 0.017(4) 0.013(4) 0.017(5) 0.003(3) 0.005(4) -0.002(3) C31 0.037(7) 0.007(5) 0.017(5) 0.006(4) -0.006(5) 0.001(4) C32 0.023(6) 0.010(5) 0.024(6) 0.007(4) -0.002(5) 0.002(4) C33 0.027(6) 0.011(5) 0.016(5) 0.007(4) -0.003(5) -0.002(4) C34 0.031(6) 0.015(5) 0.019(6) -0.001(4) 0.008(5) -0.004(5) C35 0.025(6) 0.014(5) 0.020(6) -0.006(4) -0.002(5) 0.005(4) C36 0.027(6) 0.019(6) 0.013(5) 0.006(4) -0.005(4) 0.003(5) C37 0.051(9) 0.018(6) 0.025(7) 0.003(5) -0.007(6) 0.004(6) C38 0.043(8) 0.013(5) 0.034(7) -0.004(5) -0.015(6) 0.002(5) N39 0.019(5) 0.012(4) 0.016(5) -0.007(3) 0.007(4) 0.001(3) C40 0.036(7) 0.023(6) 0.015(6) 0.001(5) 0.000(5) 0.000(5) C41 0.048(8) 0.018(6) 0.031(7) -0.001(5) 0.001(6) 0.003(6) O42 0.024(4) 0.013(4) 0.013(4) -0.003(3) 0.002(3) -0.004(3) O43 0.028(4) 0.011(4) 0.011(4) -0.002(3) 0.001(3) 0.003(3) N44 0.024(5) 0.011(4) 0.017(5) -0.004(4) 0.004(4) -0.003(4) C45 0.030(6) 0.016(5) 0.017(6) -0.001(4) 0.004(5) -0.005(5) C46 0.028(6) 0.019(6) 0.014(5) -0.002(4) 0.006(5) -0.008(5) C47 0.018(5) 0.009(5) 0.017(5) 0.007(4) 0.000(4) 0.002(4) C48 0.040(7) 0.006(5) 0.014(5) 0.001(4) 0.004(5) 0.004(4) C49 0.031(6) 0.022(6) 0.012(5) -0.001(4) 0.006(5) -0.007(5) C50 0.019(5) 0.012(5) 0.019(5) -0.002(4) -0.005(4) 0.000(4) C51 0.031(6) 0.016(5) 0.013(5) -0.005(4) 0.006(5) 0.001(5) C52 0.029(6) 0.005(5) 0.022(6) 0.002(4) -0.002(5) 0.002(4) N53 0.020(5) 0.011(4) 0.019(5) 0.006(4) 0.002(4) -0.001(3) C54 0.021(5) 0.014(5) 0.012(5) -0.002(4) -0.001(4) 0.002(4) C55 0.021(5) 0.013(5) 0.018(5) 0.006(4) -0.001(4) 0.003(4) O56 0.026(4) 0.008(4) 0.023(4) 0.007(3) 0.004(3) 0.003(3) O57 0.024(4) 0.012(3) 0.008(3) 0.000(3) -0.002(3) 0.001(3) N58 0.020(5) 0.014(4) 0.018(5) -0.004(4) -0.004(4) 0.002(4) C59 0.019(5) 0.010(5) 0.023(6) 0.003(4) -0.003(4) 0.002(4) C60 0.031(7) 0.010(5) 0.025(6) -0.001(4) 0.004(5) -0.001(5) C61 0.018(5) 0.009(5) 0.025(6) 0.006(4) 0.007(4) 0.003(4) C62 0.021(6) 0.005(4) 0.023(6) 0.003(4) -0.004(4) -0.007(4) C63 0.020(6) 0.010(5) 0.029(6) 0.002(4) -0.002(5) 0.002(4) C64 0.027(6) 0.014(5) 0.017(5) 0.003(4) 0.011(5) -0.001(4) C65 0.021(6) 0.016(5) 0.027(6) 0.002(5) 0.001(5) -0.005(4) C66 0.020(6) 0.012(5) 0.022(6) 0.000(4) 0.009(4) 0.003(4) N67 0.014(4) 0.010(4) 0.027(5) -0.004(4) 0.008(4) 0.000(3) C68 0.027(6) 0.008(5) 0.011(5) -0.002(4) 0.004(4) 0.004(4) C69 0.028(6) 0.015(5) 0.024(6) -0.003(4) 0.009(5) 0.000(5) O70 0.018(4) 0.019(4) 0.004(3) 0.000(3) 0.007(3) -0.002(3) O71 0.028(5) 0.028(5) 0.035(5) 0.007(4) 0.001(4) 0.003(4) N72 0.030(6) 0.022(5) 0.024(5) 0.001(4) -0.003(4) 0.002(4) C73 0.029(7) 0.020(6) 0.046(8) -0.001(6) -0.015(6) -0.003(5) C74 0.030(6) 0.014(5) 0.029(7) -0.003(5) -0.002(5) 0.002(5) C75 0.035(7) 0.020(6) 0.014(5) 0.006(4) -0.004(5) 0.002(5) C76 0.046(8) 0.015(6) 0.017(6) 0.000(4) -0.003(5) -0.002(5) C77 0.036(7) 0.019(6) 0.025(6) -0.001(5) 0.002(5) 0.007(5) I78 0.0305(4) 0.0224(4) 0.0375(5) 0.0006(3) 0.0082(4) -0.0021(3) I79 0.0280(4) 0.0203(4) 0.0293(4) 0.0029(3) 0.0018(3) -0.0024(3) I80 0.0264(4) 0.0255(4) 0.0421(5) 0.0073(4) 0.0048(4) 0.0002(3) I81 0.0450(6) 0.0282(5) 0.0563(6) 0.0085(4) 0.0091(5) 0.0050(4) I82 0.0442(7) 0.0151(5) 0.0319(6) 0.000 -0.0023(5) 0.000 I83 0.0367(5) 0.0262(4) 0.0489(6) 0.0005(4) -0.0053(4) -0.0078(4) I84 0.0400(7) 0.0192(5) 0.0360(6) 0.0012(5) -0.0093(5) -0.0076(5) I85 0.0625(7) 0.0393(5) 0.0419(6) 0.0021(4) 0.0047(5) 0.0192(5) I86 0.0411(5) 0.0139(4) 0.0435(5) 0.0004(3) 0.0090(4) 0.0002(3) I87 0.0969(10) 0.0404(6) 0.0418(6) 0.0002(5) 0.0027(6) -0.0371(6) O88 0.082(9) 0.032(6) 0.039(6) 0.010(5) -0.003(6) -0.014(6) C89 0.062(12) 0.075(14) 0.065(13) 0.016(11) 0.009(10) 0.023(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 Er1 O1 2.373(8) . ? Er1 O15 2.327(8) . ? Er1 O29 2.332(7) . ? Er1 O42 2.286(7) . ? Er1 O43 2.306(7) . ? Er1 O56 2.351(7) . ? Er1 O57 2.422(7) . ? Er1 O70 2.415(7) . ? O1 N2 1.323(13) . ? N2 C3 1.360(15) . ? N2 C7 1.369(14) . ? C3 C4 1.391(16) . ? C3 H3A 0.9500 . ? C4 C5 1.412(16) . ? C4 H4A 0.9500 . ? C5 C6 1.382(16) . ? C5 C8 1.476(16) . ? C6 C7 1.367(17) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.381(17) . ? C8 C13 1.402(17) . ? C9 C10 1.388(17) . ? C9 H9A 0.9500 . ? C10 N11 1.351(18) . ? C10 H10A 0.9500 . ? N11 O14 1.312(15) . ? N11 C12 1.383(18) . ? C12 C13 1.37(2) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? O15 N16 1.314(12) . ? N16 C21 1.329(15) . ? N16 C17 1.353(15) . ? C17 C18 1.383(17) . ? C17 H17A 0.9500 . ? C18 C19 1.397(16) . ? C18 H18A 0.9500 . ? C19 C20 1.398(17) . ? C19 C22 1.464(17) . ? C20 C21 1.374(18) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.399(17) . ? C22 C27 1.401(17) . ? C23 C24 1.372(18) . ? C23 H23A 0.9500 . ? C24 N25 1.352(15) . ? C24 H24A 0.9500 . ? N25 O28 1.319(13) . ? N25 C26 1.367(16) . ? C26 C27 1.366(18) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? O29 N30 1.333(11) . ? N30 C31 1.332(14) . ? N30 C35 1.368(14) . ? C31 C32 1.377(14) . ? C31 H31A 0.9500 . ? C32 C33 1.385(16) . ? C32 H32A 0.9500 . ? C33 C34 1.399(16) . ? C33 C36 1.487(14) . ? C34 C35 1.380(16) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.379(17) 8 ? C36 C41 1.384(18) 8 ? C37 C36 1.379(17) 8_556 ? C37 C38 1.390(17) . ? C37 H37A 0.9500 . ? C38 N39 1.323(16) . ? C38 H38A 0.9500 . ? N39 O42 1.335(11) . ? N39 C40 1.354(15) . ? C40 C41 1.390(17) . ? C40 H40A 0.9500 . ? O43 N44 1.320(11) . ? N44 C49 1.348(14) . ? N44 C45 1.353(14) . ? C45 C46 1.380(15) . ? C45 H45A 0.9500 . ? C46 C47 1.403(15) 8_545 ? C46 H46A 0.9500 . ? C47 C48 1.398(15) . ? C47 C50 1.470(14) . ? C48 C49 1.365(15) 8_546 ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C50 C55 1.382(15) . ? C50 C51 1.398(15) . ? C51 C52 1.387(15) . ? C51 H51A 0.9500 . ? C52 N53 1.333(15) . ? C52 H52A 0.9500 . ? N53 O56 1.336(11) . ? N53 C54 1.351(14) . ? C54 C55 1.389(14) . ? C54 H54A 0.9500 . ? C55 H55A 0.9500 . ? O57 N58 1.326(11) . ? N58 C63 1.348(14) . ? N58 C59 1.353(14) . ? C59 C62 1.367(16) 2_444 ? C59 H59A 0.9500 . ? C60 C63 1.354(17) 2_445 ? C60 C61 1.391(15) . ? C60 H60A 0.9500 . ? C61 C62 1.408(15) . ? C61 C64 1.482(15) . ? C62 H62A 0.9500 . ? C63 H63A 0.9500 . ? C64 C65 1.402(16) . ? C64 C69 1.409(15) . ? C65 C66 1.359(16) . ? C65 H65A 0.9500 . ? C66 N67 1.359(14) . ? C66 H66A 0.9500 . ? N67 O70 1.315(11) . ? N67 C68 1.352(13) . ? C68 C69 1.380(15) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? O71 N72 1.318(14) . ? N72 C73 1.339(16) . ? N72 C77 1.355(16) . ? C73 C74 1.361(18) . ? C73 H73A 0.9500 . ? C74 C75 1.381(16) . ? C74 H74A 0.9500 . ? C75 C76 1.392(17) . ? C75 C75 1.51(3) 4_554 ? C76 C77 1.386(19) . ? C76 H76A 0.9500 . ? C77 H77A 0.9500 . ? I78 I79 2.9103(13) . ? I79 I80 2.9275(13) . ? I81 I82 2.9103(12) . ? I83 I84 2.9084(11) . ? I85 I86 2.9207(16) . ? I86 I87 2.9114(16) . ? O88 C89 1.41(2) . ? 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 O42 Er1 O43 138.7(3) . . ? O42 Er1 O15 152.9(3) . . ? O43 Er1 O15 68.4(3) . . ? O42 Er1 O29 90.3(3) . . ? O43 Er1 O29 103.3(3) . . ? O15 Er1 O29 79.6(3) . . ? O42 Er1 O56 102.4(3) . . ? O43 Er1 O56 90.3(3) . . ? O15 Er1 O56 73.2(3) . . ? O29 Er1 O56 142.6(3) . . ? O42 Er1 O1 68.7(3) . . ? O43 Er1 O1 152.5(3) . . ? O15 Er1 O1 84.3(3) . . ? O29 Er1 O1 73.9(3) . . ? O56 Er1 O1 78.2(3) . . ? O42 Er1 O70 71.7(2) . . ? O43 Er1 O70 76.0(3) . . ? O15 Er1 O70 128.3(3) . . ? O29 Er1 O70 146.3(3) . . ? O56 Er1 O70 70.6(3) . . ? O1 Er1 O70 121.8(3) . . ? O42 Er1 O57 76.5(3) . . ? O43 Er1 O57 72.0(2) . . ? O15 Er1 O57 122.1(3) . . ? O29 Er1 O57 70.2(3) . . ? O56 Er1 O57 146.8(3) . . ? O1 Er1 O57 129.1(3) . . ? O70 Er1 O57 77.8(3) . . ? N2 O1 Er1 130.3(7) . . ? O1 N2 C3 120.3(10) . . ? O1 N2 C7 119.0(10) . . ? C3 N2 C7 120.7(10) . . ? N2 C3 C4 119.9(11) . . ? N2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C5 120.9(11) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C6 C5 C4 116.0(11) . . ? C6 C5 C8 123.1(11) . . ? C4 C5 C8 120.9(10) . . ? C7 C6 C5 123.1(11) . . ? C7 C6 H6A 118.4 . . ? C5 C6 H6A 118.4 . . ? C6 C7 N2 119.3(11) . . ? C6 C7 H7A 120.3 . . ? N2 C7 H7A 120.3 . . ? C9 C8 C13 116.9(11) . . ? C9 C8 C5 121.7(11) . . ? C13 C8 C5 121.3(11) . . ? C8 C9 C10 122.3(12) . . ? C8 C9 H9A 118.8 . . ? C10 C9 H9A 118.8 . . ? N11 C10 C9 119.5(12) . . ? N11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? O14 N11 C10 119.0(12) . . ? O14 N11 C12 121.0(12) . . ? C10 N11 C12 119.9(12) . . ? C13 C12 N11 120.8(13) . . ? C13 C12 H12A 119.6 . . ? N11 C12 H12A 119.6 . . ? C12 C13 C8 120.6(12) . . ? C12 C13 H13A 119.7 . . ? C8 C13 H13A 119.7 . . ? N16 O15 Er1 145.3(7) . . ? O15 N16 C21 122.0(10) . . ? O15 N16 C17 117.2(10) . . ? C21 N16 C17 120.7(11) . . ? N16 C17 C18 118.6(11) . . ? N16 C17 H17A 120.7 . . ? C18 C17 H17A 120.7 . . ? C17 C18 C19 122.6(11) . . ? C17 C18 H18A 118.7 . . ? C19 C18 H18A 118.7 . . ? C18 C19 C20 115.7(11) . . ? C18 C19 C22 121.3(11) . . ? C20 C19 C22 123.0(11) . . ? C21 C20 C19 120.1(12) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? N16 C21 C20 122.2(12) . . ? N16 C21 H21A 118.9 . . ? C20 C21 H21A 118.9 . . ? C23 C22 C27 116.0(11) . . ? C23 C22 C19 121.3(11) . . ? C27 C22 C19 122.7(11) . . ? C24 C23 C22 122.2(12) . . ? C24 C23 H23A 118.9 . . ? C22 C23 H23A 118.9 . . ? N25 C24 C23 119.3(12) . . ? N25 C24 H24A 120.4 . . ? C23 C24 H24A 120.4 . . ? O28 N25 C24 119.6(10) . . ? O28 N25 C26 119.3(10) . . ? C24 N25 C26 121.0(11) . . ? C27 C26 N25 120.0(12) . . ? C27 C26 H26A 120.0 . . ? N25 C26 H26A 120.0 . . ? C26 C27 C22 121.4(11) . . ? C26 C27 H27A 119.3 . . ? C22 C27 H27A 119.3 . . ? N30 O29 Er1 127.8(6) . . ? C31 N30 O29 119.1(9) . . ? C31 N30 C35 120.7(9) . . ? O29 N30 C35 120.1(9) . . ? N30 C31 C32 121.5(11) . . ? N30 C31 H31A 119.3 . . ? C32 C31 H31A 119.3 . . ? C31 C32 C33 120.4(11) . . ? C31 C32 H32A 119.8 . . ? C33 C32 H32A 119.8 . . ? C32 C33 C34 116.7(10) . . ? C32 C33 C36 123.2(10) . . ? C34 C33 C36 120.1(10) . . ? C35 C34 C33 121.8(11) . . ? C35 C34 H34A 119.1 . . ? C33 C34 H34A 119.1 . . ? N30 C35 C34 118.8(10) . . ? N30 C35 H35A 120.6 . . ? C34 C35 H35A 120.6 . . ? C37 C36 C41 117.7(11) 8 8 ? C37 C36 C33 121.8(11) 8 . ? C41 C36 C33 120.5(11) 8 . ? C36 C37 C38 120.1(12) 8_556 . ? C36 C37 H37A 119.9 8_556 . ? C38 C37 H37A 119.9 . . ? N39 C38 C37 121.0(11) . . ? N39 C38 H38A 119.5 . . ? C37 C38 H38A 119.5 . . ? C38 N39 O42 119.0(9) . . ? C38 N39 C40 120.8(10) . . ? O42 N39 C40 120.1(9) . . ? N39 C40 C41 119.7(11) . . ? N39 C40 H40A 120.2 . . ? C41 C40 H40A 120.2 . . ? C36 C41 C40 120.5(12) 8_556 . ? N39 O42 Er1 132.7(6) . . ? N44 O43 Er1 130.9(6) . . ? O43 N44 C49 120.0(9) . . ? O43 N44 C45 119.9(9) . . ? C49 N44 C45 120.1(9) . . ? N44 C45 C46 121.0(10) . . ? N44 C45 H45A 119.5 . . ? C46 C45 H45A 119.5 . . ? C45 C46 C47 120.0(10) . 8_545 ? C45 C46 H46A 120.0 . . ? C47 C46 H46A 120.0 8_545 . ? C48 C47 C46 116.9(9) . 8_546 ? C48 C47 C50 121.9(10) . . ? C46 C47 C50 121.2(10) 8_546 . ? C49 C48 C47 121.1(10) 8_546 . ? C49 C48 H48A 119.5 8_546 . ? C47 C48 H48A 119.5 . . ? N44 C49 C48 120.9(10) . 8_545 ? N44 C49 H49A 119.5 . . ? C48 C49 H49A 119.5 8_545 . ? C55 C50 C51 116.0(10) . . ? C55 C50 C47 123.2(10) . . ? C51 C50 C47 120.7(10) . . ? C52 C51 C50 121.0(10) . . ? C52 C51 H51A 119.5 . . ? C50 C51 H51A 119.5 . . ? N53 C52 C51 120.2(10) . . ? N53 C52 H52A 119.9 . . ? C51 C52 H52A 119.9 . . ? C52 N53 O56 120.2(9) . . ? C52 N53 C54 121.5(9) . . ? O56 N53 C54 118.3(9) . . ? N53 C54 C55 118.9(10) . . ? N53 C54 H54A 120.5 . . ? C55 C54 H54A 120.5 . . ? C50 C55 C54 122.2(10) . . ? C50 C55 H55A 118.9 . . ? C54 C55 H55A 118.9 . . ? N53 O56 Er1 128.3(6) . . ? N58 O57 Er1 127.9(6) . . ? O57 N58 C63 118.7(9) . . ? O57 N58 C59 120.4(9) . . ? C63 N58 C59 120.8(10) . . ? N58 C59 C62 119.6(10) . 2_444 ? N58 C59 H59A 120.2 . . ? C62 C59 H59A 120.2 2_444 . ? C63 C60 C61 121.3(11) 2_445 . ? C63 C60 H60A 119.3 2_445 . ? C61 C60 H60A 119.3 . . ? C60 C61 C62 116.4(10) . . ? C60 C61 C64 124.0(10) . . ? C62 C61 C64 119.6(9) . . ? C59 C62 C61 121.0(10) 2_445 . ? C59 C62 H62A 119.5 2_445 . ? C61 C62 H62A 119.5 . . ? N58 C63 C60 120.4(10) . 2_444 ? N58 C63 H63A 119.8 . . ? C60 C63 H63A 119.8 2_444 . ? C65 C64 C69 116.7(10) . . ? C65 C64 C61 122.8(10) . . ? C69 C64 C61 120.5(10) . . ? C66 C65 C64 122.1(11) . . ? C66 C65 H65A 119.0 . . ? C64 C65 H65A 119.0 . . ? N67 C66 C65 119.2(10) . . ? N67 C66 H66A 120.4 . . ? C65 C66 H66A 120.4 . . ? O70 N67 C68 119.5(9) . . ? O70 N67 C66 119.1(9) . . ? C68 N67 C66 121.3(9) . . ? N67 C68 C69 120.5(10) . . ? N67 C68 H68A 119.8 . . ? C69 C68 H68A 119.8 . . ? C68 C69 C64 119.9(10) . . ? C68 C69 H69A 120.1 . . ? C64 C69 H69A 120.1 . . ? N67 O70 Er1 128.4(6) . . ? O71 N72 C73 121.0(11) . . ? O71 N72 C77 119.3(10) . . ? C73 N72 C77 119.7(11) . . ? N72 C73 C74 121.3(12) . . ? N72 C73 H73A 119.4 . . ? C74 C73 H73A 119.4 . . ? C73 C74 C75 121.4(11) . . ? C73 C74 H74A 119.3 . . ? C75 C74 H74A 119.3 . . ? C74 C75 C76 116.9(12) . . ? C74 C75 C75 121.0(7) . 4_554 ? C76 C75 C75 122.0(8) . 4_554 ? C77 C76 C75 120.3(12) . . ? C77 C76 H76A 119.9 . . ? C75 C76 H76A 119.9 . . ? N72 C77 C76 120.5(11) . . ? N72 C77 H77A 119.8 . . ? C76 C77 H77A 119.8 . . ? I78 I79 I80 177.22(4) . . ? I81 I82 I81 177.85(6) 4_554 . ? I83 I84 I83 180.000(8) . 5_554 ? I87 I86 I85 177.83(5) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 3.28 _refine_diff_density_min -2.05 _refine_diff_density_rms 0.28 #===END of CIF data_LANBBP _database_code_depnum_ccdc_archive 'CCDC 239608' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point '(C36 H41 La N5 O9), 2(C24 H20 B), 2.7(C H4 O)' _chemical_formula_sum 'C86.70 H91.80 B2 La N5 O11.70' _chemical_formula_weight 1551.58 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' B B 0.0013 0.0007 '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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 49.269(7) _cell_length_b 17.698(3) _cell_length_c 18.718(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.946(3) _cell_angle_gamma 90.00 _cell_volume 15693(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5614 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 25.95 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6461 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 0.901 _exptl_absorpt_process_details 'SADABS (Bruker, 1999b)' _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 CCD Area Detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 70902 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.051 _diffrn_reflns_limit_h_min -62 _diffrn_reflns_limit_h_max 57 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 27.03 _reflns_number_total 15221 _reflns_number_gt 9822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999a)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 1999)' _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^)+(0.0982P)^2^+89.1026P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'refined in riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 15221 _refine_ls_number_parameters 1002 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.105 _refine_ls_R_factor_gt 0.068 _refine_ls_wR_factor_ref 0.208 _refine_ls_wR_factor_gt 0.181 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 La La 0.126446(7) 0.745574(19) 0.094890(19) 0.03878(13) Uani 1 1 d . . . O1 O 0.1610(2) 0.6738(5) 0.2110(4) 0.069(3) Uani 0.80(2) 1 d P A 1 C1 C 0.1692(3) 0.5998(7) 0.2338(7) 0.093(5) Uani 0.80(2) 1 d P A 1 O5 O 0.1919(2) 0.7951(5) 0.2937(5) 0.056(2) Uiso 0.50 1 d PD B 1 C5 C 0.2205(5) 0.8095(13) 0.3161(12) 0.102(6) Uiso 0.50 1 d PD B 1 O1' O 0.1492(7) 0.6425(17) 0.2033(15) 0.047(8) Uiso 0.20(2) 1 d P A 2 C1' C 0.1466(7) 0.5632(18) 0.2138(18) 0.044(10) Uiso 0.20(2) 1 d P A 2 O5' O 0.2027(6) 0.6676(16) 0.2701(16) 0.076(8) Uiso 0.20 1 d PD C 2 C5' C 0.1979(13) 0.739(3) 0.300(3) 0.109(18) Uiso 0.20 1 d PD C 2 O2 O 0.07096(10) 0.7192(3) 0.0836(3) 0.0652(13) Uani 1 1 d . A . C2 C 0.0508(2) 0.6542(5) 0.0688(6) 0.089(3) Uani 1 1 d . . . H2A H 0.0376 0.6596 0.0991 0.133 Uiso 1 1 calc R A . H2B H 0.0613 0.6068 0.0815 0.133 Uiso 1 1 calc R . . H2C H 0.0403 0.6537 0.0161 0.133 Uiso 1 1 calc R . . O20 O 0.10286(11) 0.7465(3) -0.0413(3) 0.0591(12) Uani 1 1 d . A . O30 O 0.10254(12) 0.8707(3) 0.0901(2) 0.0609(13) Uani 1 1 d . A . O40 O 0.11332(10) 0.6139(2) 0.0753(3) 0.0542(12) Uani 1 1 d . A . O50 O 0.16352(10) 0.6749(3) 0.0543(3) 0.0677(15) Uani 1 1 d . A . O60 O 0.11755(13) 0.7757(3) 0.2192(3) 0.0700(15) Uani 1 1 d . A . O11 O 0.15242(11) 0.8392(3) 0.0309(3) 0.0619(13) Uani 1 1 d . A . O12 O 0.16895(11) 0.8297(3) 0.1535(3) 0.0700(14) Uani 1 1 d . A . C11 C 0.17008(15) 0.8578(4) 0.0917(5) 0.064(2) Uani 1 1 d . A . C12 C 0.19260(16) 0.9161(5) 0.0944(5) 0.073(2) Uani 1 1 d D A 1 C13 C 0.1892(2) 0.9543(6) 0.0151(8) 0.067(4) Uani 0.675(12) 1 d PD A 1 C14 C 0.2155(3) 1.0054(7) 0.0199(12) 0.095(6) Uani 0.675(12) 1 d PD A 1 C15 C 0.2021(4) 1.0829(10) -0.0017(13) 0.097(9) Uani 0.675(12) 1 d PD A 1 C16 C 0.1782(3) 1.0830(7) 0.0366(9) 0.086(5) Uani 0.675(12) 1 d PD A 1 C17 C 0.1646(2) 1.0089(6) -0.0005(7) 0.066(3) Uani 0.675(12) 1 d PD A 1 C18 C 0.1604(3) 1.0331(9) -0.0850(8) 0.079(4) Uani 0.675(12) 1 d PD A 1 C19 C 0.1851(4) 1.0820(10) -0.0850(10) 0.106(6) Uani 0.675(12) 1 d PD A 1 C13' C 0.1813(4) 0.9932(10) 0.0534(11) 0.053(6) Uiso 0.325(12) 1 d PDU A 2 C14' C 0.2028(5) 1.0604(12) 0.0761(13) 0.060(6) Uiso 0.325(12) 1 d PDU A 2 C15' C 0.2062(8) 1.093(2) 0.0021(18) 0.063(9) Uiso 0.325(12) 1 d PDU A 2 C16' C 0.2070(5) 1.0145(15) -0.0367(16) 0.068(7) Uiso 0.325(12) 1 d PDU A 2 C17' C 0.1781(5) 0.9852(15) -0.0299(13) 0.069(7) Uiso 0.325(12) 1 d PDU A 2 C18' C 0.1567(7) 1.0559(17) -0.061(2) 0.102(11) Uiso 0.325(12) 1 d PDU A 2 C19' C 0.1767(5) 1.1230(16) -0.0439(16) 0.075(7) Uiso 0.325(12) 1 d PDU A 2 N20 N 0.10423(12) 0.7984(3) -0.0906(3) 0.0480(13) Uani 1 1 d . . . C21 C 0.09562(16) 0.8694(4) -0.0827(4) 0.0565(18) Uani 1 1 d . A . H21A H 0.0886 0.8819 -0.0417 0.068 Uiso 1 1 calc R . . C22 C 0.09704(14) 0.9232(4) -0.1337(4) 0.0522(16) Uani 1 1 d . . . H22A H 0.0914 0.9734 -0.1267 0.063 Uiso 1 1 calc R A . C23 C 0.10644(13) 0.9072(4) -0.1954(3) 0.0448(14) Uani 1 1 d . . . C24 C 0.11519(14) 0.8337(4) -0.2008(4) 0.0478(15) Uani 1 1 d . . . H24A H 0.1221 0.8195 -0.2415 0.057 Uiso 1 1 calc R A . C25 C 0.11396(13) 0.7813(4) -0.1480(4) 0.0476(15) Uani 1 1 d . A . H25A H 0.1202 0.7312 -0.1527 0.057 Uiso 1 1 calc R . . N30 N 0.10385(13) 0.9224(3) 0.1434(3) 0.0495(13) Uani 1 1 d . . . C31 C 0.12328(19) 0.9759(5) 0.1542(5) 0.075(2) Uani 1 1 d . A . H31A H 0.1362 0.9759 0.1247 0.090 Uiso 1 1 calc R . . C32 C 0.12547(17) 1.0322(4) 0.2075(5) 0.068(2) Uani 1 1 d . . . H32A H 0.1400 1.0692 0.2150 0.081 Uiso 1 1 calc R A . C33 C 0.10649(13) 1.0337(3) 0.2488(3) 0.0425(14) Uani 1 1 d . . . C34 C 0.08629(14) 0.9758(4) 0.2354(4) 0.0525(17) Uani 1 1 d . . . H34A H 0.0729 0.9743 0.2635 0.063 Uiso 1 1 calc R A . C35 C 0.08547(15) 0.9216(4) 0.1829(4) 0.0556(17) Uani 1 1 d . A . H35A H 0.0715 0.8831 0.1748 0.067 Uiso 1 1 calc R . . N40 N 0.11449(11) 0.5622(3) 0.0254(3) 0.0462(13) Uani 1 1 d . . . C41 C 0.09230(15) 0.5531(4) -0.0349(4) 0.0602(19) Uani 1 1 d . A . H41A H 0.0766 0.5863 -0.0429 0.072 Uiso 1 1 calc R . . C42 C 0.09229(15) 0.4969(4) -0.0844(4) 0.0616(19) Uani 1 1 d . . . H42A H 0.0764 0.4912 -0.1264 0.074 Uiso 1 1 calc R A . C43 C 0.11496(13) 0.4475(3) -0.0748(4) 0.0435(14) Uani 1 1 d . . . C44 C 0.13808(14) 0.4606(4) -0.0132(4) 0.0485(15) Uani 1 1 d . . . H44A H 0.1544 0.4298 -0.0050 0.058 Uiso 1 1 calc R A . C45 C 0.13706(14) 0.5177(4) 0.0352(4) 0.0505(16) Uani 1 1 d . A . H45A H 0.1528 0.5259 0.0770 0.061 Uiso 1 1 calc R . . N50 N 0.18705(12) 0.6977(3) 0.0405(4) 0.0555(15) Uani 1 1 d . . . C51 C 0.18683(17) 0.7240(7) -0.0267(5) 0.090(3) Uani 1 1 d . A . H51A H 0.1694 0.7282 -0.0639 0.109 Uiso 1 1 calc R . . C52 C 0.21090(16) 0.7449(6) -0.0428(4) 0.089(3) Uani 1 1 d . . . H52A H 0.2099 0.7634 -0.0911 0.107 Uiso 1 1 calc R A . C53 C 0.23684(13) 0.7400(4) 0.0094(4) 0.0480(15) Uani 1 1 d . . . C54 C 0.23642(14) 0.7154(5) 0.0787(4) 0.064(2) Uani 1 1 d . . . H54A H 0.2535 0.7129 0.1174 0.076 Uiso 1 1 calc R A . C55 C 0.21145(16) 0.6943(5) 0.0928(5) 0.066(2) Uani 1 1 d . A . H55A H 0.2117 0.6770 0.1410 0.079 Uiso 1 1 calc R . . N60 N 0.11658(13) 0.7244(3) 0.2689(4) 0.0580(15) Uani 1 1 d . . . C61 C 0.10012(17) 0.6643(6) 0.2500(5) 0.077(2) Uani 1 1 d . A . H61A H 0.0886 0.6601 0.2004 0.092 Uiso 1 1 calc R . . C62 C 0.09917(18) 0.6076(5) 0.3001(5) 0.079(3) Uani 1 1 d . . . H62A H 0.0874 0.5648 0.2845 0.095 Uiso 1 1 calc R A . C63 C 0.11536(13) 0.6137(4) 0.3727(4) 0.0471(15) Uani 1 1 d . . . C64 C 0.13127(16) 0.6774(4) 0.3911(4) 0.0575(18) Uani 1 1 d . . . H64A H 0.1432 0.6819 0.4403 0.069 Uiso 1 1 calc R A . C65 C 0.13097(16) 0.7331(4) 0.3439(5) 0.066(2) Uani 1 1 d . A . H65A H 0.1405 0.7791 0.3610 0.080 Uiso 1 1 calc R . . B1 B 0.18462(15) 0.7024(4) 0.6958(5) 0.0479(18) Uani 1 1 d . . . C111 C 0.20098(14) 0.7803(4) 0.7289(4) 0.0518(16) Uani 1 1 d . . . C112 C 0.22445(18) 0.8094(5) 0.7131(5) 0.075(2) Uani 1 1 d . . . H11A H 0.2330 0.7816 0.6816 0.090 Uiso 1 1 calc R . . C113 C 0.2364(2) 0.8799(6) 0.7422(7) 0.103(3) Uani 1 1 d . . . H11B H 0.2527 0.8978 0.7295 0.123 Uiso 1 1 calc R . . C114 C 0.2255(3) 0.9215(6) 0.7868(7) 0.105(4) Uani 1 1 d . . . H11C H 0.2339 0.9678 0.8070 0.126 Uiso 1 1 calc R . . C115 C 0.2024(3) 0.8961(7) 0.8021(6) 0.115(5) Uani 1 1 d . . . H11D H 0.1935 0.9260 0.8313 0.138 Uiso 1 1 calc R . . C116 C 0.19090(17) 0.8260(5) 0.7760(4) 0.073(2) Uani 1 1 d . . . H11E H 0.1752 0.8086 0.7914 0.087 Uiso 1 1 calc R . . C121 C 0.15238(13) 0.7215(4) 0.6470(3) 0.0451(14) Uani 1 1 d . . . C122 C 0.14246(14) 0.7931(4) 0.6254(4) 0.0540(17) Uani 1 1 d . . . H12C H 0.1545 0.8354 0.6412 0.065 Uiso 1 1 calc R . . C123 C 0.11468(17) 0.8045(4) 0.5802(4) 0.069(2) Uani 1 1 d . . . H12D H 0.1082 0.8546 0.5673 0.083 Uiso 1 1 calc R . . C124 C 0.09713(15) 0.7466(4) 0.5549(4) 0.0595(18) Uani 1 1 d . . . H12E H 0.0786 0.7554 0.5240 0.071 Uiso 1 1 calc R . . C125 C 0.10641(14) 0.6743(4) 0.5744(4) 0.0520(16) Uani 1 1 d . . . H12F H 0.0943 0.6326 0.5572 0.062 Uiso 1 1 calc R . . C126 C 0.13339(13) 0.6627(4) 0.6188(4) 0.0524(17) Uani 1 1 d . . . H12G H 0.1395 0.6122 0.6311 0.063 Uiso 1 1 calc R . . C131 C 0.18499(14) 0.6496(4) 0.7676(4) 0.0559(18) Uani 1 1 d . . . C132 C 0.16106(16) 0.6315(4) 0.7906(4) 0.063(2) Uani 1 1 d . . . H13B H 0.1435 0.6528 0.7637 0.076 Uiso 1 1 calc R . . C133 C 0.1613(2) 0.5849(6) 0.8494(6) 0.091(3) Uani 1 1 d . . . H13C H 0.1443 0.5732 0.8618 0.109 Uiso 1 1 calc R . . C134 C 0.1866(2) 0.5558(7) 0.8898(7) 0.131(5) Uani 1 1 d . . . H13D H 0.1871 0.5223 0.9298 0.157 Uiso 1 1 calc R . . C135 C 0.2113(2) 0.5744(7) 0.8736(6) 0.117(4) Uani 1 1 d . . . H13E H 0.2289 0.5573 0.9046 0.141 Uiso 1 1 calc R . . C136 C 0.21035(19) 0.6186(6) 0.8112(5) 0.091(3) Uani 1 1 d . . . H13F H 0.2273 0.6279 0.7979 0.109 Uiso 1 1 calc R . . C141 C 0.19870(13) 0.6594(4) 0.6368(4) 0.0549(18) Uani 1 1 d . . . C142 C 0.20687(15) 0.5849(5) 0.6391(6) 0.077(3) Uani 1 1 d . . . H14C H 0.2056 0.5541 0.6796 0.093 Uiso 1 1 calc R . . C143 C 0.21742(16) 0.5525(5) 0.5810(7) 0.085(3) Uani 1 1 d . . . H14D H 0.2233 0.5012 0.5836 0.102 Uiso 1 1 calc R . . C144 C 0.21879(18) 0.5970(6) 0.5219(7) 0.089(3) Uani 1 1 d . . . H14E H 0.2257 0.5758 0.4836 0.107 Uiso 1 1 calc R . . C145 C 0.21050(19) 0.6709(6) 0.5168(6) 0.087(3) Uani 1 1 d . . . H14F H 0.2117 0.7013 0.4760 0.104 Uiso 1 1 calc R . . C146 C 0.20035(17) 0.6998(5) 0.5725(5) 0.068(2) Uani 1 1 d . . . H14G H 0.1940 0.7507 0.5677 0.082 Uiso 1 1 calc R . . B2 B 0.0000 0.5028(6) 0.7500 0.048(2) Uani 1 2 d S . . C211 C 0.02718(13) 0.5528(4) 0.7421(4) 0.0516(16) Uani 1 1 d . . . C212 C 0.04510(14) 0.5286(4) 0.7015(4) 0.0591(18) Uani 1 1 d . . . H21B H 0.0414 0.4817 0.6761 0.071 Uiso 1 1 calc R . . C213 C 0.06851(15) 0.5707(5) 0.6964(4) 0.066(2) Uani 1 1 d . . . H21C H 0.0802 0.5525 0.6674 0.079 Uiso 1 1 calc R . . C214 C 0.07458(17) 0.6376(5) 0.7328(5) 0.072(2) Uani 1 1 d . . . H21D H 0.0904 0.6665 0.7292 0.086 Uiso 1 1 calc R . . C215 C 0.05742(16) 0.6635(5) 0.7753(5) 0.072(2) Uani 1 1 d . . . H21E H 0.0617 0.7098 0.8017 0.087 Uiso 1 1 calc R . . C216 C 0.03425(15) 0.6220(5) 0.7792(4) 0.063(2) Uani 1 1 d . . . H21F H 0.0226 0.6409 0.8080 0.075 Uiso 1 1 calc R . . C221 C 0.01311(13) 0.4536(4) 0.8267(4) 0.0551(17) Uani 1 1 d . . . C222 C 0.02562(15) 0.3839(4) 0.8293(4) 0.0621(19) Uani 1 1 d . . . H22B H 0.0261 0.3603 0.7841 0.075 Uiso 1 1 calc R . . C223 C 0.03763(18) 0.3470(5) 0.8961(5) 0.076(2) Uani 1 1 d . . . H22C H 0.0460 0.2987 0.8958 0.091 Uiso 1 1 calc R . . C224 C 0.03742(16) 0.3805(5) 0.9635(5) 0.070(2) Uani 1 1 d . . . H22D H 0.0448 0.3544 1.0091 0.084 Uiso 1 1 calc R . . C225 C 0.02652(15) 0.4511(5) 0.9626(4) 0.064(2) Uani 1 1 d . . . H22E H 0.0270 0.4760 1.0078 0.076 Uiso 1 1 calc R . . C226 C 0.01483(14) 0.4861(4) 0.8960(4) 0.0578(18) Uani 1 1 d . . . H22F H 0.0074 0.5355 0.8969 0.069 Uiso 1 1 calc R . . B3 B 0.0000 0.0161(7) 0.7500 0.052(3) Uani 1 2 d S . . C311 C 0.02575(14) 0.0694(4) 0.8000(4) 0.0522(17) Uani 1 1 d . . . C312 C 0.03363(18) 0.1371(5) 0.7712(4) 0.067(2) Uani 1 1 d . . . H31B H 0.0227 0.1547 0.7241 0.080 Uiso 1 1 calc R . . C313 C 0.05711(19) 0.1791(5) 0.8104(5) 0.073(2) Uani 1 1 d . . . H31C H 0.0621 0.2239 0.7891 0.087 Uiso 1 1 calc R . . C314 C 0.07280(17) 0.1567(5) 0.8782(5) 0.073(2) Uani 1 1 d . . . H31D H 0.0887 0.1856 0.9045 0.088 Uiso 1 1 calc R . . C315 C 0.06566(15) 0.0924(5) 0.9085(4) 0.063(2) Uani 1 1 d . . . H31E H 0.0764 0.0771 0.9566 0.075 Uiso 1 1 calc R . . C316 C 0.04277(15) 0.0484(4) 0.8701(4) 0.0564(18) Uani 1 1 d . . . H31F H 0.0386 0.0030 0.8921 0.068 Uiso 1 1 calc R . . C321 C -0.01462(13) -0.0329(4) 0.8030(4) 0.0515(16) Uani 1 1 d . . . C322 C -0.01750(15) -0.0051(5) 0.8708(4) 0.0573(18) Uani 1 1 d . . . H32B H -0.0093 0.0425 0.8878 0.069 Uiso 1 1 calc R . . C323 C -0.03156(16) -0.0428(5) 0.9140(4) 0.069(2) Uani 1 1 d . . . H32C H -0.0328 -0.0213 0.9595 0.083 Uiso 1 1 calc R . . C324 C -0.04375(17) -0.1116(5) 0.8915(5) 0.072(2) Uani 1 1 d . . . H32D H -0.0532 -0.1382 0.9216 0.087 Uiso 1 1 calc R . . C325 C -0.04213(15) -0.1420(5) 0.8248(5) 0.070(2) Uani 1 1 d . . . H32E H -0.0505 -0.1896 0.8085 0.084 Uiso 1 1 calc R . . C326 C -0.02794(14) -0.1015(5) 0.7811(4) 0.0619(19) Uani 1 1 d . . . H32F H -0.0275 -0.1221 0.7346 0.074 Uiso 1 1 calc R . . O3 O 0.03153(12) 0.8254(4) 0.0688(4) 0.0899(19) Uani 1 1 d . . . C3 C 0.0036(2) 0.7954(7) 0.0675(7) 0.105(4) Uani 1 1 d . . . O4 O 0.02706(14) 0.8541(4) 0.9249(4) 0.100(2) Uani 1 1 d . . . C4 C 0.0255(3) 0.7776(6) 0.8934(7) 0.105(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La 0.0409(2) 0.0379(2) 0.0390(2) -0.00486(16) 0.01344(14) 0.00036(16) O1 0.062(5) 0.068(5) 0.071(5) 0.010(4) 0.007(4) 0.015(4) C1 0.105(11) 0.078(8) 0.091(9) 0.022(7) 0.015(7) 0.026(7) O2 0.052(3) 0.067(3) 0.073(3) -0.006(3) 0.011(3) 0.001(2) C2 0.081(6) 0.076(6) 0.103(7) 0.005(5) 0.015(5) -0.015(5) O20 0.083(3) 0.049(3) 0.040(2) 0.004(2) 0.008(2) -0.009(2) O30 0.099(4) 0.048(3) 0.037(2) -0.004(2) 0.021(3) 0.024(3) O40 0.061(3) 0.037(2) 0.075(3) -0.009(2) 0.038(3) -0.008(2) O50 0.055(3) 0.050(3) 0.116(5) -0.012(3) 0.053(3) -0.010(2) O60 0.109(4) 0.039(2) 0.077(4) 0.015(3) 0.050(3) 0.019(3) O11 0.061(3) 0.059(3) 0.063(3) 0.006(2) 0.013(3) -0.013(2) O12 0.063(3) 0.071(3) 0.067(4) 0.008(3) 0.003(3) -0.018(3) C11 0.046(4) 0.063(5) 0.077(6) 0.004(4) 0.008(4) -0.002(3) C12 0.047(4) 0.069(5) 0.095(6) 0.021(5) 0.007(4) -0.012(4) C13 0.049(6) 0.053(6) 0.107(11) -0.002(7) 0.036(7) -0.008(5) C14 0.053(8) 0.063(8) 0.177(19) 0.012(9) 0.042(10) -0.011(6) C15 0.099(14) 0.049(8) 0.16(2) -0.034(9) 0.074(13) -0.045(8) C16 0.072(9) 0.058(7) 0.144(14) -0.021(8) 0.054(9) -0.004(6) C17 0.056(7) 0.057(7) 0.079(9) -0.003(6) 0.011(6) 0.004(5) C18 0.080(9) 0.085(10) 0.082(10) 0.009(8) 0.038(8) 0.003(7) C19 0.100(12) 0.112(13) 0.113(14) 0.005(11) 0.040(11) -0.036(10) N20 0.056(3) 0.046(3) 0.038(3) -0.001(2) 0.006(3) -0.007(2) C21 0.067(5) 0.053(4) 0.051(4) 0.000(3) 0.020(4) 0.006(3) C22 0.057(4) 0.053(4) 0.045(4) 0.006(3) 0.010(3) 0.012(3) C23 0.044(3) 0.047(3) 0.041(3) -0.001(3) 0.007(3) 0.000(3) C24 0.050(4) 0.053(4) 0.041(4) 0.000(3) 0.013(3) -0.001(3) C25 0.047(4) 0.041(3) 0.053(4) 0.002(3) 0.011(3) 0.004(3) N30 0.068(4) 0.038(3) 0.045(3) 0.002(2) 0.019(3) 0.005(3) C31 0.097(6) 0.072(5) 0.077(6) -0.003(4) 0.061(5) 0.016(5) C32 0.076(5) 0.059(4) 0.080(6) -0.010(4) 0.041(5) -0.012(4) C33 0.050(4) 0.042(3) 0.038(3) 0.005(3) 0.016(3) 0.006(3) C34 0.048(4) 0.057(4) 0.053(4) -0.015(3) 0.014(3) -0.005(3) C35 0.056(4) 0.058(4) 0.053(4) -0.009(3) 0.015(3) 0.000(3) N40 0.052(3) 0.039(3) 0.054(3) -0.004(2) 0.026(3) -0.007(2) C41 0.053(4) 0.057(4) 0.074(5) 0.000(4) 0.021(4) 0.013(3) C42 0.050(4) 0.068(5) 0.062(5) -0.018(4) 0.007(3) -0.001(3) C43 0.038(3) 0.043(3) 0.053(4) -0.002(3) 0.017(3) -0.006(3) C44 0.044(4) 0.045(3) 0.059(4) -0.005(3) 0.017(3) -0.002(3) C45 0.051(4) 0.045(4) 0.057(4) -0.001(3) 0.017(3) -0.003(3) N50 0.044(3) 0.054(3) 0.075(4) -0.009(3) 0.029(3) -0.006(3) C51 0.044(4) 0.171(10) 0.055(5) -0.020(6) 0.011(4) -0.029(5) C52 0.045(4) 0.184(11) 0.036(4) 0.006(5) 0.008(3) -0.023(5) C53 0.036(3) 0.065(4) 0.045(3) -0.004(3) 0.014(3) -0.002(3) C54 0.035(4) 0.104(6) 0.052(4) 0.015(4) 0.012(3) 0.009(4) C55 0.060(5) 0.083(6) 0.065(5) 0.021(4) 0.035(4) 0.012(4) N60 0.061(4) 0.043(3) 0.077(4) 0.012(3) 0.030(3) 0.013(3) C61 0.060(5) 0.112(7) 0.053(5) 0.020(5) 0.008(4) -0.002(5) C62 0.071(5) 0.086(6) 0.073(6) 0.034(5) 0.009(4) -0.021(5) C63 0.044(4) 0.051(4) 0.050(4) 0.004(3) 0.019(3) 0.007(3) C64 0.073(5) 0.046(4) 0.056(4) 0.005(3) 0.022(4) 0.001(3) C65 0.062(5) 0.044(4) 0.073(5) 0.018(4) -0.016(4) -0.012(3) B1 0.035(4) 0.050(4) 0.057(5) 0.004(4) 0.011(3) 0.004(3) C111 0.047(4) 0.056(4) 0.048(4) -0.002(3) 0.005(3) 0.008(3) C112 0.066(5) 0.068(5) 0.089(6) -0.011(5) 0.018(5) -0.010(4) C113 0.088(7) 0.074(6) 0.126(9) 0.002(6) -0.003(7) -0.024(5) C114 0.099(8) 0.066(6) 0.124(9) -0.041(6) -0.014(7) 0.002(6) C115 0.104(9) 0.101(8) 0.110(9) -0.064(7) -0.022(7) 0.026(7) C116 0.059(5) 0.091(6) 0.058(5) -0.020(4) -0.001(4) 0.011(4) C121 0.043(3) 0.058(4) 0.034(3) -0.001(3) 0.010(3) 0.006(3) C122 0.046(4) 0.051(4) 0.057(4) -0.001(3) 0.001(3) 0.003(3) C123 0.065(5) 0.057(4) 0.068(5) 0.007(4) -0.010(4) 0.018(4) C124 0.043(4) 0.073(5) 0.055(4) -0.007(4) -0.001(3) 0.005(4) C125 0.044(4) 0.060(4) 0.051(4) -0.007(3) 0.011(3) 0.002(3) C126 0.042(4) 0.052(4) 0.063(4) -0.006(3) 0.014(3) 0.008(3) C131 0.038(4) 0.066(4) 0.056(4) 0.012(4) -0.001(3) 0.009(3) C132 0.052(4) 0.071(5) 0.063(5) 0.018(4) 0.011(4) 0.006(4) C133 0.079(6) 0.100(7) 0.097(7) 0.042(6) 0.031(5) 0.003(5) C134 0.095(8) 0.150(11) 0.148(11) 0.101(9) 0.036(8) 0.025(8) C135 0.069(6) 0.173(12) 0.103(8) 0.081(8) 0.011(6) 0.041(7) C136 0.058(5) 0.123(8) 0.089(7) 0.046(6) 0.015(5) 0.024(5) C141 0.028(3) 0.057(4) 0.073(5) -0.012(4) 0.003(3) 0.003(3) C142 0.042(4) 0.063(5) 0.108(7) -0.022(5) -0.012(4) 0.014(3) C143 0.041(4) 0.071(6) 0.127(9) -0.030(6) -0.004(5) 0.017(4) C144 0.054(5) 0.094(7) 0.119(9) -0.035(7) 0.023(5) 0.001(5) C145 0.083(6) 0.099(7) 0.093(7) -0.021(6) 0.047(6) -0.010(5) C146 0.066(5) 0.068(5) 0.075(6) -0.011(4) 0.027(4) 0.001(4) B2 0.044(6) 0.059(6) 0.038(6) 0.000 0.006(5) 0.000 C211 0.040(4) 0.068(4) 0.044(4) 0.000(3) 0.008(3) -0.001(3) C212 0.049(4) 0.061(4) 0.067(5) -0.009(4) 0.015(4) 0.001(3) C213 0.049(4) 0.085(6) 0.068(5) -0.005(4) 0.023(4) 0.002(4) C214 0.054(5) 0.086(6) 0.077(6) -0.005(5) 0.022(4) -0.011(4) C215 0.054(5) 0.090(6) 0.075(6) -0.019(5) 0.020(4) -0.012(4) C216 0.049(4) 0.080(5) 0.063(5) -0.017(4) 0.022(4) -0.011(4) C221 0.035(3) 0.068(5) 0.063(5) 0.003(4) 0.015(3) 0.004(3) C222 0.058(4) 0.064(5) 0.061(5) 0.005(4) 0.010(4) 0.005(4) C223 0.071(5) 0.067(5) 0.082(6) -0.003(5) 0.009(5) 0.025(4) C224 0.052(4) 0.090(6) 0.062(5) 0.014(5) 0.003(4) 0.010(4) C225 0.050(4) 0.084(6) 0.057(5) 0.002(4) 0.016(4) 0.011(4) C226 0.049(4) 0.070(5) 0.055(4) 0.000(4) 0.014(3) 0.008(3) B3 0.049(6) 0.071(7) 0.038(6) 0.000 0.015(5) 0.000 C311 0.044(4) 0.077(5) 0.038(4) -0.003(3) 0.017(3) -0.001(3) C312 0.077(5) 0.076(5) 0.057(5) 0.000(4) 0.034(4) -0.004(4) C313 0.084(6) 0.068(5) 0.080(6) -0.015(5) 0.045(5) -0.023(4) C314 0.057(5) 0.092(6) 0.075(6) -0.027(5) 0.026(4) -0.021(4) C315 0.051(4) 0.086(6) 0.050(4) -0.021(4) 0.012(3) -0.007(4) C316 0.055(4) 0.071(5) 0.050(4) -0.010(4) 0.025(3) -0.004(3) C321 0.034(3) 0.068(4) 0.048(4) 0.006(3) 0.005(3) -0.001(3) C322 0.059(4) 0.079(5) 0.035(4) -0.002(3) 0.013(3) -0.012(4) C323 0.065(5) 0.089(6) 0.056(5) 0.008(4) 0.024(4) -0.012(4) C324 0.065(5) 0.087(6) 0.068(5) 0.020(5) 0.024(4) -0.010(4) C325 0.043(4) 0.073(5) 0.090(6) 0.017(5) 0.010(4) -0.008(4) C326 0.044(4) 0.078(5) 0.060(5) 0.001(4) 0.006(3) 0.003(4) O3 0.066(4) 0.097(5) 0.107(5) -0.028(4) 0.024(3) -0.004(3) C3 0.070(6) 0.131(9) 0.126(9) -0.026(7) 0.045(6) -0.019(6) O4 0.085(4) 0.103(5) 0.110(5) 0.015(4) 0.025(4) 0.007(4) C4 0.120(9) 0.084(7) 0.110(8) -0.010(6) 0.031(7) 0.024(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 La O11 2.580(5) . yes La O12 2.558(5) . yes La O20 2.495(5) . yes La O30 2.498(4) . yes La O40 2.420(4) . yes La O50 2.498(4) . yes La O60 2.540(5) . yes La O1 2.684(7) . yes La O2 2.724(5) . yes La O1' 2.73(3) . ? O1 C1 1.402(13) . ? O5 C5 1.38(2) . ? O1' C1' 1.43(4) . ? O5' C5' 1.43(3) . ? O2 C2 1.494(10) . ? O20 N20 1.316(7) . yes O30 N30 1.343(7) . yes O40 N40 1.319(6) . yes O50 N50 1.318(7) . yes O60 N60 1.310(7) . yes O11 C11 1.272(9) . ? O12 C11 1.273(9) . ? C11 C12 1.506(10) . ? C12 C13 1.597(15) . ? C13 C17 1.512(14) . ? C13 C14 1.564(14) . ? C14 C15 1.53(2) . ? C15 C16 1.54(3) . ? C15 C19 1.55(2) . ? C16 C17 1.546(16) . ? C17 C18 1.596(16) . ? C18 C19 1.495(17) . ? C13' C17' 1.53(2) . ? C13' C14' 1.57(2) . ? C14' C15' 1.55(3) . ? C15' C16' 1.57(4) . ? C15' C19' 1.57(3) . ? C16' C17' 1.55(3) . ? C17' C18' 1.63(3) . ? C18' C19' 1.52(3) . ? N20 C25 1.327(8) . ? N20 C21 1.347(8) . ? C21 C22 1.364(9) . ? C22 C23 1.387(9) . ? C23 C24 1.382(9) . ? C23 C33 1.480(9) 6_575 ? C24 C25 1.369(9) . ? N30 C35 1.318(9) . ? N30 C31 1.322(10) . ? C31 C32 1.394(11) . ? C32 C33 1.367(9) . ? C33 C34 1.402(9) . ? C33 C23 1.480(9) 6_576 ? C34 C35 1.366(9) . ? N40 C45 1.334(8) . ? N40 C41 1.348(9) . ? C41 C42 1.359(10) . ? C42 C43 1.390(9) . ? C43 C44 1.399(9) . ? C43 C63 1.466(9) 6_565 ? C44 C45 1.369(9) . ? N50 C55 1.326(9) . ? N50 C51 1.338(10) . ? C51 C52 1.353(11) . ? C52 C53 1.382(10) . ? C53 C54 1.375(9) . ? C53 C53 1.477(12) 7_565 ? C54 C55 1.378(10) . ? N60 C61 1.325(10) . ? N60 C65 1.396(10) . ? C61 C62 1.382(11) . ? C62 C63 1.379(10) . ? C63 C64 1.362(9) . ? C63 C43 1.466(9) 6_566 ? C64 C65 1.321(10) . ? B1 C111 1.632(11) . ? B1 C131 1.632(10) . ? B1 C121 1.636(9) . ? B1 C141 1.643(10) . ? C111 C112 1.370(11) . ? C111 C116 1.385(10) . ? C112 C113 1.423(12) . ? C113 C114 1.334(15) . ? C114 C115 1.326(16) . ? C115 C116 1.394(13) . ? C121 C122 1.378(9) . ? C121 C126 1.402(9) . ? C122 C123 1.412(10) . ? C123 C124 1.340(10) . ? C124 C125 1.373(10) . ? C125 C126 1.377(9) . ? C131 C132 1.399(10) . ? C131 C136 1.403(10) . ? C132 C133 1.374(11) . ? C133 C134 1.370(13) . ? C134 C135 1.371(14) . ? C135 C136 1.396(13) . ? C141 C142 1.376(10) . ? C141 C146 1.421(11) . ? C142 C143 1.447(13) . ? C143 C144 1.374(14) . ? C144 C145 1.366(13) . ? C145 C146 1.373(11) . ? B2 C211 1.645(9) 2_556 ? B2 C211 1.645(9) . ? B2 C221 1.651(9) 2_556 ? B2 C221 1.651(9) . ? C211 C212 1.382(9) . ? C211 C216 1.403(10) . ? C212 C213 1.398(10) . ? C213 C214 1.357(11) . ? C214 C215 1.388(11) . ? C215 C216 1.376(10) . ? C221 C222 1.373(10) . ? C221 C226 1.401(10) . ? C222 C223 1.391(11) . ? C223 C224 1.397(12) . ? C224 C225 1.359(11) . ? C225 C226 1.369(10) . ? B3 C321 1.627(9) 2_556 ? B3 C321 1.627(10) . ? B3 C311 1.649(10) . ? B3 C311 1.649(10) 2_556 ? C311 C316 1.400(10) . ? C311 C312 1.412(10) . ? C312 C313 1.401(11) . ? C313 C314 1.352(12) . ? C314 C315 1.360(12) . ? C315 C316 1.396(10) . ? C321 C326 1.388(10) . ? C321 C322 1.405(10) . ? C322 C323 1.374(10) . ? C323 C324 1.372(12) . ? C324 C325 1.382(12) . ? C325 C326 1.408(11) . ? O3 C3 1.467(11) . ? O4 C4 1.470(12) . ? 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 O40 La O20 79.70(16) . . yes O20 La O30 82.80(15) . . yes O40 La O30 138.13(17) . . ? O50 La O30 144.05(17) . . ? O20 La O50 82.33(19) . . yes O40 La O50 70.07(15) . . yes O20 La O60 141.79(19) . . ? O30 La O60 69.44(15) . . yes O40 La O60 103.58(16) . . ? O50 La O60 135.11(19) . . ? O20 La O11 70.88(16) . . yes O30 La O11 72.74(17) . . yes O40 La O11 133.93(16) . . ? O50 La O11 71.49(17) . . yes O60 La O11 121.55(17) . . ? O12 La O11 51.20(17) . . yes O20 La O12 122.06(17) . . ? O30 La O12 79.73(18) . . yes O40 La O12 141.17(17) . . ? O50 La O12 80.85(18) . . yes O60 La O12 79.18(19) . . yes O20 La O1 147.6(2) . . ? O30 La O1 129.6(2) . . ? O40 La O1 75.6(3) . . yes O50 La O1 69.8(2) . . yes O60 La O1 65.71(19) . . yes O11 La O1 113.2(3) . . ? O12 La O1 70.5(3) . . yes O20 La O2 75.28(17) . . yes O30 La O2 72.31(17) . . yes O40 La O2 66.56(16) . . yes O50 La O2 133.84(16) . . ? O60 La O2 71.64(18) . . yes O11 La O2 133.57(16) . . ? O12 La O2 145.00(17) . . ? O1 La O2 112.5(3) . . ? O20 La O1' 138.1(6) . . ? O30 La O1' 135.4(6) . . ? O40 La O1' 60.5(7) . . ? O50 La O1' 72.9(6) . . ? O60 La O1' 66.3(5) . . ? O11 La O1' 128.3(7) . . ? O12 La O1' 87.1(8) . . ? O1 La O1' 16.7(6) . . ? O2 La O1' 98.1(7) . . ? C1 O1 La 139.0(8) . . ? C1' O1' La 136(2) . . ? C2 O2 La 138.4(5) . . ? N20 O20 La 128.4(4) . . ? N30 O30 La 130.7(4) . . ? N40 O40 La 135.5(3) . . ? N50 O50 La 131.5(4) . . ? N60 O60 La 123.7(4) . . ? C11 O11 La 93.2(4) . . ? C11 O12 La 94.2(4) . . ? O11 C11 O12 121.4(7) . . ? O11 C11 C12 121.6(8) . . ? O12 C11 C12 116.9(7) . . ? C11 C12 C13 111.7(7) . . ? C17 C13 C14 104.3(9) . . ? C17 C13 C12 109.0(9) . . ? C14 C13 C12 108.5(11) . . ? C15 C14 C13 102.4(11) . . ? C14 C15 C16 102.0(12) . . ? C14 C15 C19 109.3(17) . . ? C16 C15 C19 101.3(14) . . ? C15 C16 C17 94.6(11) . . ? C13 C17 C16 103.5(9) . . ? C13 C17 C18 104.1(11) . . ? C16 C17 C18 98.1(11) . . ? C19 C18 C17 105.7(12) . . ? C18 C19 C15 102.7(13) . . ? C17' C13' C14' 102.7(17) . . ? C15' C14' C13' 106(2) . . ? C14' C15' C16' 96(2) . . ? C14' C15' C19' 108(3) . . ? C16' C15' C19' 101(2) . . ? C17' C16' C15' 97(2) . . ? C13' C17' C16' 102.1(19) . . ? C13' C17' C18' 99(2) . . ? C16' C17' C18' 103(2) . . ? C19' C18' C17' 102(2) . . ? C18' C19' C15' 107(2) . . ? O20 N20 C25 120.5(5) . . ? O20 N20 C21 119.7(6) . . ? C25 N20 C21 119.8(6) . . ? N20 C21 C22 119.8(7) . . ? C21 C22 C23 122.2(6) . . ? C24 C23 C22 115.8(6) . . ? C24 C23 C33 123.6(6) . 6_575 ? C22 C23 C33 120.6(6) . 6_575 ? C25 C24 C23 120.6(6) . . ? N20 C25 C24 121.8(6) . . ? C35 N30 C31 120.2(6) . . ? C35 N30 O30 120.7(6) . . ? C31 N30 O30 119.1(6) . . ? N30 C31 C32 122.2(7) . . ? C33 C32 C31 119.2(7) . . ? C32 C33 C34 116.6(6) . . ? C32 C33 C23 123.2(6) . 6_576 ? C34 C33 C23 120.2(6) . 6_576 ? C35 C34 C33 121.3(6) . . ? N30 C35 C34 120.5(7) . . ? O40 N40 C45 120.5(6) . . ? O40 N40 C41 119.5(5) . . ? C45 N40 C41 119.9(6) . . ? N40 C41 C42 120.4(6) . . ? C41 C42 C43 121.5(7) . . ? C42 C43 C44 116.4(6) . . ? C42 C43 C63 122.4(6) . 6_565 ? C44 C43 C63 121.1(6) . 6_565 ? C45 C44 C43 119.9(6) . . ? N40 C45 C44 121.7(7) . . ? O50 N50 C55 120.6(6) . . ? O50 N50 C51 120.6(6) . . ? C55 N50 C51 118.7(6) . . ? N50 C51 C52 121.6(8) . . ? C51 C52 C53 121.5(8) . . ? C54 C53 C52 115.9(6) . . ? C54 C53 C53 122.8(7) . 7_565 ? C52 C53 C53 121.3(8) . 7_565 ? C53 C54 C55 120.8(7) . . ? N50 C55 C54 121.5(7) . . ? O60 N60 C61 120.3(7) . . ? O60 N60 C65 122.0(6) . . ? C61 N60 C65 117.5(6) . . ? N60 C61 C62 122.3(8) . . ? C63 C62 C61 119.6(8) . . ? C64 C63 C62 116.7(7) . . ? C64 C63 C43 123.7(6) . 6_566 ? C62 C63 C43 119.5(6) . 6_566 ? C65 C64 C63 123.3(7) . . ? C64 C65 N60 119.9(7) . . ? C111 B1 C131 106.2(6) . . ? C111 B1 C121 109.8(5) . . ? C131 B1 C121 111.6(5) . . ? C111 B1 C141 113.0(5) . . ? C131 B1 C141 112.2(6) . . ? C121 B1 C141 104.2(5) . . ? C112 C111 C116 112.9(8) . . ? C112 C111 B1 126.4(7) . . ? C116 C111 B1 120.6(7) . . ? C111 C112 C113 122.1(9) . . ? C114 C113 C112 121.9(11) . . ? C115 C114 C113 117.8(10) . . ? C114 C115 C116 121.0(10) . . ? C111 C116 C115 124.1(10) . . ? C122 C121 C126 115.3(6) . . ? C122 C121 B1 124.5(6) . . ? C126 C121 B1 120.1(6) . . ? C121 C122 C123 120.9(7) . . ? C124 C123 C122 121.9(7) . . ? C123 C124 C125 118.9(7) . . ? C124 C125 C126 119.7(7) . . ? C125 C126 C121 123.3(6) . . ? C132 C131 C136 115.0(7) . . ? C132 C131 B1 124.4(6) . . ? C136 C131 B1 120.6(7) . . ? C133 C132 C131 124.3(7) . . ? C134 C133 C132 118.2(9) . . ? C133 C134 C135 121.1(9) . . ? C134 C135 C136 119.5(9) . . ? C135 C136 C131 121.7(8) . . ? C142 C141 C146 115.1(8) . . ? C142 C141 B1 126.6(8) . . ? C146 C141 B1 118.0(6) . . ? C141 C142 C143 121.2(10) . . ? C144 C143 C142 119.0(8) . . ? C145 C144 C143 121.7(10) . . ? C144 C145 C146 118.0(10) . . ? C145 C146 C141 124.9(8) . . ? C211 B2 C211 115.0(8) 2_556 . ? C211 B2 C221 103.2(3) 2_556 2_556 ? C211 B2 C221 109.8(3) . 2_556 ? C211 B2 C221 109.8(3) 2_556 . ? C211 B2 C221 103.2(3) . . ? C221 B2 C221 116.3(9) 2_556 . ? C212 C211 C216 115.6(6) . . ? C212 C211 B2 122.8(6) . . ? C216 C211 B2 121.5(6) . . ? C211 C212 C213 122.4(7) . . ? C214 C213 C212 120.2(7) . . ? C213 C214 C215 119.3(8) . . ? C216 C215 C214 119.9(8) . . ? C215 C216 C211 122.5(7) . . ? C222 C221 C226 115.1(7) . . ? C222 C221 B2 124.7(7) . . ? C226 C221 B2 119.9(6) . . ? C221 C222 C223 122.0(8) . . ? C222 C223 C224 120.3(7) . . ? C225 C224 C223 118.7(8) . . ? C224 C225 C226 119.6(8) . . ? C225 C226 C221 124.1(7) . . ? C321 B3 C321 115.6(9) 2_556 . ? C321 B3 C311 104.5(3) 2_556 . ? C321 B3 C311 111.1(3) . . ? C321 B3 C311 111.1(3) 2_556 2_556 ? C321 B3 C311 104.5(3) . 2_556 ? C311 B3 C311 110.3(9) . 2_556 ? C316 C311 C312 115.2(7) . . ? C316 C311 B3 123.3(7) . . ? C312 C311 B3 121.2(6) . . ? C313 C312 C311 121.6(8) . . ? C314 C313 C312 120.9(8) . . ? C313 C314 C315 119.3(8) . . ? C314 C315 C316 121.1(8) . . ? C315 C316 C311 121.7(7) . . ? C326 C321 C322 114.6(7) . . ? C326 C321 B3 122.7(7) . . ? C322 C321 B3 122.4(7) . . ? C323 C322 C321 123.6(7) . . ? C324 C323 C322 120.0(8) . . ? C323 C324 C325 119.6(8) . . ? C324 C325 C326 119.1(8) . . ? C321 C326 C325 123.0(8) . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 1.68 # Highest peak 1.68 at 0.1426 0.7478 0.1184 [0.80 A from LA] _refine_diff_density_min -0.65 _refine_diff_density_rms 0.10 #===END of CIF data_LACLBZ _database_code_depnum_ccdc_archive 'CCDC 239609' _refine_special_details ; Some Percholorate anions were treated disorder models on two positions with partial occupancy and geometry restrained tetrahedron by using instructions SADI on distances of Cl-O and O...O separation. Due to partial occupancy, some sites or close region were reassigned to solvent molecules. Solvated solvent molecules were treated being chlorobenzene and methanol molecules, which in some regions share the space with partial occupancies. The benzene ring of chlorobenzene molecules were restrained to be approximate hexagons with instructions FLAT and SAME. The number of solvent molecules were determined by elemental analysis. Two pyridine rings involving C242 and C272 of the pyridine N-oxide ligands were treated as being rotation disorder models along the N-O bond axis. No hydrogen atoms were added for these disordered solvent and ligands regions. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C40 H32 La N8 O8 3+), 3(Cl O4 -), (C6 H5 Cl), (C H4 O)' _chemical_formula_sum 'C47 H41 Cl4 La N8 O21' _chemical_formula_weight 1334.59 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.6846(8) _cell_length_b 19.8749(9) _cell_length_c 32.669(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.664(2) _cell_angle_gamma 90.00 _cell_volume 10646(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19023 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 26.9 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5376 _exptl_absorpt_coefficient_mu 1.091 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details '(XABS2; Parkin et al., 1995)' _exptl_absorpt_correction_T_min 0.471 _exptl_absorpt_correction_T_max 1.310 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 94959 _diffrn_reflns_av_R_equivalents 0.118 _diffrn_reflns_av_sigmaI/netI 0.065 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 26.00 _reflns_number_total 20663 _reflns_number_gt 13084 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'SAINT version 6.02a (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 6.12 (Bruker, 2001)' _computing_publication_material 'enCIFer (Allen et al., 2004; PLATON (Spek, 2003)' _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^)+(0.111P)^2^+6.01] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 20663 _refine_ls_number_parameters 1496 _refine_ls_number_restraints 264 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.194 _refine_ls_wR_factor_gt 0.175 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.08 _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 La1 La 0.81039(2) 0.850462(16) 0.397305(11) 0.01978(11) Uani 1 1 d . . . La2 La 0.31081(2) 0.347431(16) 0.415392(12) 0.02235(12) Uani 1 1 d . . . O110 O 0.8887(3) 0.8093(2) 0.34567(14) 0.0340(11) Uani 1 1 d . . . O120 O 0.8712(3) 0.9483(2) 0.36377(14) 0.0322(11) Uani 1 1 d . . . O130 O 0.6974(3) 0.8991(2) 0.34630(15) 0.0334(11) Uani 1 1 d . . . O140 O 0.7236(3) 0.7580(2) 0.35890(14) 0.0326(11) Uani 1 1 d . . . O150 O 0.8518(3) 0.7473(2) 0.43518(15) 0.0333(11) Uani 1 1 d . . . O160 O 0.9558(3) 0.8626(2) 0.44029(15) 0.0312(11) Uani 1 1 d . . . O170 O 0.7995(3) 0.9525(2) 0.43723(14) 0.0292(10) Uani 1 1 d . . . O180 O 0.6953(3) 0.8335(2) 0.43709(15) 0.0295(10) Uani 1 1 d . . . O210 O 0.3442(3) 0.4525(2) 0.45806(14) 0.0280(10) Uani 1 1 d . . . O220 O 1.2118(3) 0.3617(2) 0.46599(16) 0.0333(11) Uani 1 1 d . . . O230 O 1.3208(3) 1.2412(2) 0.45526(15) 0.0310(11) Uani 1 1 d . . . O240 O 0.4583(3) 1.3387(2) 0.44992(17) 0.0387(13) Uani 1 1 d . . . O250 O 1.1932(3) 0.3987(2) 0.37099(16) 0.0399(12) Uani 1 1 d . . . O260 O 0.2874(3) 0.7594(2) 0.11900(14) 0.0323(11) Uani 1 1 d . . . O270 O 0.3755(3) 1.2961(2) 0.35948(16) 0.0426(13) Uani 1 1 d . . . O280 O 1.1327(3) 0.9375(2) 0.12442(14) 0.0319(11) Uani 1 1 d . . . N110 N 0.9325(3) 0.7537(3) 0.34472(17) 0.0294(13) Uani 1 1 d . . . C111 C 1.0117(5) 0.7569(4) 0.3500(4) 0.073(3) Uani 1 1 d . . . H111 H 1.0375 0.7997 0.3531 0.087 Uiso 1 1 calc R . . C112 C 1.0587(5) 0.7000(4) 0.3513(3) 0.064(3) Uani 1 1 d . . . H112 H 1.1165 0.7042 0.3568 0.077 Uiso 1 1 calc R . . C113 C 1.0254(4) 0.6389(3) 0.3451(2) 0.0369(17) Uani 1 1 d . . . C114 C 0.9421(6) 0.6389(4) 0.3365(5) 0.124(7) Uani 1 1 d . . . H114 H 0.9143 0.5974 0.3303 0.149 Uiso 1 1 calc R . . C115 C 0.8972(6) 0.6967(4) 0.3364(4) 0.095(5) Uani 1 1 d . . . H115 H 0.8394 0.6945 0.3302 0.114 Uiso 1 1 calc R . . N120 N 0.9071(3) 0.9429(3) 0.33074(18) 0.0311(13) Uani 1 1 d . . . C121 C 0.9893(5) 0.9448(4) 0.3361(2) 0.045(2) Uani 1 1 d . . . H121 H 1.0205 0.9502 0.3633 0.054 Uiso 1 1 calc R . . C122 C 1.0280(4) 0.9390(4) 0.3032(2) 0.046(2) Uani 1 1 d . . . H122 H 1.0859 0.9399 0.3075 0.056 Uiso 1 1 calc R . . C123 C 0.9819(4) 0.9317(3) 0.2622(2) 0.0291(15) Uani 1 1 d . . . C124 C 0.8980(4) 0.9296(3) 0.2591(2) 0.0311(15) Uani 1 1 d . . . H124 H 0.8647 0.9240 0.2324 0.037 Uiso 1 1 calc R . . C125 C 0.8617(4) 0.9353(3) 0.2927(2) 0.0313(15) Uani 1 1 d . . . H125 H 0.8039 0.9338 0.2893 0.038 Uiso 1 1 calc R . . N130 N 0.6512(3) 0.9534(3) 0.34509(18) 0.0324(13) Uani 1 1 d . . . C131 C 0.6842(5) 1.0145(3) 0.3425(3) 0.052(2) Uani 1 1 d . . . H131 H 0.7403 1.0190 0.3411 0.062 Uiso 1 1 calc R . . C132 C 0.6361(6) 1.0701(4) 0.3417(4) 0.078(4) Uani 1 1 d . . . H132 H 0.6594 1.1134 0.3400 0.094 Uiso 1 1 calc R . . C133 C 0.5529(6) 1.0648(4) 0.3435(3) 0.059(3) Uani 1 1 d . . . C134 C 0.5224(5) 1.0012(4) 0.3458(2) 0.0407(18) Uani 1 1 d . . . H134 H 0.4664 0.9952 0.3470 0.049 Uiso 1 1 calc R . . C135 C 0.5725(4) 0.9462(3) 0.3463(2) 0.0342(16) Uani 1 1 d . . . H135 H 0.5505 0.9024 0.3476 0.041 Uiso 1 1 calc R . . N140 N 0.6641(3) 0.7616(3) 0.32537(17) 0.0289(12) Uani 1 1 d . . . C141 C 0.5876(4) 0.7424(4) 0.3290(2) 0.0413(18) Uani 1 1 d . . . H141 H 0.5776 0.7268 0.3551 0.050 Uiso 1 1 calc R . . C142 C 0.5260(5) 0.7453(4) 0.2960(2) 0.050(2) Uani 1 1 d . . . H142 H 0.4729 0.7319 0.2993 0.060 Uiso 1 1 calc R . . C143 C 0.5384(4) 0.7678(3) 0.2566(2) 0.0290(15) Uani 1 1 d . . . C144 C 0.6176(4) 0.7852(3) 0.2545(2) 0.0316(15) Uani 1 1 d . . . H144 H 0.6298 0.7997 0.2286 0.038 Uiso 1 1 calc R . . C145 C 0.6789(4) 0.7824(3) 0.2884(2) 0.0338(16) Uani 1 1 d . . . H145 H 0.7326 0.7952 0.2859 0.041 Uiso 1 1 calc R . . N150 N 0.9012(3) 0.6943(2) 0.44150(18) 0.0305(13) Uani 1 1 d . . . C151 C 0.8689(5) 0.6336(3) 0.4302(3) 0.054(2) Uani 1 1 d . . . H151 H 0.8125 0.6293 0.4186 0.065 Uiso 1 1 calc R . . C152 C 0.9188(5) 0.5772(4) 0.4356(3) 0.061(3) Uani 1 1 d . . . H152 H 0.8964 0.5344 0.4272 0.074 Uiso 1 1 calc R . . C153 C 1.0009(4) 0.5824(3) 0.4531(2) 0.0349(17) Uani 1 1 d . . . C154 C 1.0297(5) 0.6460(3) 0.4644(3) 0.046(2) Uani 1 1 d . . . H154 H 1.0854 0.6520 0.4768 0.056 Uiso 1 1 calc R . . C155 C 0.9792(4) 0.7006(4) 0.4578(3) 0.045(2) Uani 1 1 d . . . H155 H 1.0008 0.7441 0.4651 0.053 Uiso 1 1 calc R . . N160 N 1.0091(3) 0.9131(2) 0.44706(17) 0.0265(12) Uani 1 1 d . . . C161 C 1.0882(4) 0.9009(3) 0.4535(3) 0.0390(18) Uani 1 1 d . . . H161 H 1.1073 0.8558 0.4544 0.047 Uiso 1 1 calc R . . C162 C 1.1434(4) 0.9535(3) 0.4589(3) 0.0424(19) Uani 1 1 d . . . H162 H 1.2000 0.9436 0.4634 0.051 Uiso 1 1 calc R . . C163 C 1.1189(4) 1.0196(3) 0.4579(2) 0.0263(14) Uani 1 1 d . . . C164 C 1.0359(4) 1.0295(3) 0.4530(2) 0.0362(17) Uani 1 1 d . . . H164 H 1.0154 1.0740 0.4536 0.043 Uiso 1 1 calc R . . C165 C 0.9826(4) 0.9766(3) 0.4474(2) 0.0362(17) Uani 1 1 d . . . H165 H 0.9257 0.9851 0.4437 0.043 Uiso 1 1 calc R . . N170 N 0.7546(3) 1.0064(2) 0.43967(18) 0.0300(13) Uani 1 1 d . . . C171 C 0.7865(5) 1.0681(3) 0.4364(3) 0.058(3) Uani 1 1 d . . . H171 H 0.8411 1.0722 0.4323 0.069 Uiso 1 1 calc R . . C172 C 0.7415(5) 1.1245(4) 0.4389(4) 0.075(4) Uani 1 1 d . . . H172 H 0.7639 1.1676 0.4351 0.090 Uiso 1 1 calc R . . C173 C 0.6635(5) 1.1191(3) 0.4468(3) 0.053(2) Uani 1 1 d . . . C174 C 0.6316(4) 1.0557(3) 0.4500(2) 0.0373(17) Uani 1 1 d . . . H174 H 0.5772 1.0508 0.4544 0.045 Uiso 1 1 calc R . . C175 C 0.6782(4) 0.9998(3) 0.4468(2) 0.0270(15) Uani 1 1 d . . . H175 H 0.6564 0.9563 0.4496 0.032 Uiso 1 1 calc R . . N180 N 0.6468(3) 0.7808(2) 0.43935(16) 0.0248(12) Uani 1 1 d . . . C181 C 0.5650(4) 0.7888(3) 0.4295(2) 0.0279(15) Uani 1 1 d . . . H181 H 0.5428 0.8318 0.4211 0.034 Uiso 1 1 calc R . . C182 C 0.5136(4) 0.7355(3) 0.4315(2) 0.0291(15) Uani 1 1 d . . . H182 H 0.4563 0.7413 0.4238 0.035 Uiso 1 1 calc R . . C183 C 0.5458(4) 0.6727(3) 0.4449(2) 0.0262(14) Uani 1 1 d . . . C184 C 0.6300(4) 0.6676(3) 0.4549(2) 0.0294(15) Uani 1 1 d . . . H184 H 0.6541 0.6257 0.4642 0.035 Uiso 1 1 calc R . . C185 C 0.6789(4) 0.7216(3) 0.4518(2) 0.0279(15) Uani 1 1 d . . . H185 H 0.7364 0.7167 0.4585 0.034 Uiso 1 1 calc R . . N210 N 0.3932(3) 0.5045(2) 0.45553(16) 0.0257(12) Uani 1 1 d . . . C211 C 0.3639(4) 0.5675(3) 0.4581(2) 0.0319(16) Uani 1 1 d . . . H211 H 0.3094 0.5741 0.4621 0.038 Uiso 1 1 calc R . . C212 C 0.4136(4) 0.6224(3) 0.4550(2) 0.0336(16) Uani 1 1 d . . . H212 H 0.3929 0.6665 0.4571 0.040 Uiso 1 1 calc R . . C213 C 0.4919(4) 0.6143(3) 0.4489(2) 0.0262(14) Uani 1 1 d . . . C214 C 0.5205(4) 0.5478(3) 0.4474(2) 0.0269(14) Uani 1 1 d . . . H214 H 0.5750 0.5401 0.4438 0.032 Uiso 1 1 calc R . . C215 C 0.4716(4) 0.4948(3) 0.4510(2) 0.0267(14) Uani 1 1 d . . . H215 H 0.4923 0.4504 0.4505 0.032 Uiso 1 1 calc R . . N220 N 1.1601(3) 0.4140(3) 0.46374(19) 0.0326(14) Uani 1 1 d . . . C221 C 1.1837(4) 0.4705(3) 0.4845(2) 0.0312(16) Uani 1 1 d . . . H221 H 1.2363 0.4732 0.5015 0.037 Uiso 1 1 calc R . . C222 C 1.1324(4) 0.5248(3) 0.4815(2) 0.0358(17) Uani 1 1 d . . . H222 H 1.1510 0.5649 0.4961 0.043 Uiso 1 1 calc R . . C223 C 1.0544(4) 0.5232(3) 0.4580(2) 0.0348(17) Uani 1 1 d . . . C224 C 1.0310(5) 0.4619(4) 0.4389(3) 0.050(2) Uani 1 1 d . . . H224 H 0.9772 0.4566 0.4235 0.060 Uiso 1 1 calc R . . C225 C 1.0849(5) 0.4087(3) 0.4418(3) 0.046(2) Uani 1 1 d . . . H225 H 1.0680 0.3676 0.4279 0.055 Uiso 1 1 calc R . . N230 N 1.2733(3) 1.1882(2) 0.45798(16) 0.0261(12) Uani 1 1 d . . . C231 C 1.3031(4) 1.1262(3) 0.4532(2) 0.0301(15) Uani 1 1 d . . . H231 H 1.3577 1.1211 0.4491 0.036 Uiso 1 1 calc R . . C232 C 1.2549(4) 1.0704(3) 0.4544(2) 0.0308(15) Uani 1 1 d . . . H232 H 1.2763 1.0269 0.4511 0.037 Uiso 1 1 calc R . . C233 C 1.1741(4) 1.0774(3) 0.4604(2) 0.0267(14) Uani 1 1 d . . . C234 C 1.1485(4) 1.1424(3) 0.4675(2) 0.0297(15) Uani 1 1 d . . . H234 H 1.0958 1.1489 0.4738 0.036 Uiso 1 1 calc R . . C235 C 1.1974(4) 1.1968(3) 0.4655(2) 0.0278(14) Uani 1 1 d . . . H235 H 1.1779 1.2407 0.4695 0.033 Uiso 1 1 calc R . . N240 N 0.5100(3) 1.2874(3) 0.4506(2) 0.0449(17) Uani 1 1 d . . . C241 C 0.4979(4) 1.2311(3) 0.4703(2) 0.0272(14) Uani 1 1 d . . . H241 H 0.4543 1.2290 0.4853 0.033 Uiso 1 1 calc R . . C242 C 0.5471(4) 1.1756(3) 0.4696(2) 0.0309(15) Uani 1 1 d . . . H242 H 0.5358 1.1351 0.4829 0.037 Uiso 1 1 calc R A . C243 C 0.6126(5) 1.1790(4) 0.4497(3) 0.060(3) Uani 1 1 d . A . C244 C 0.6417(9) 1.2432(7) 0.4474(6) 0.041(4) Uani 0.50 1 d P A 1 C245 C 0.5891(10) 1.2984(6) 0.4461(6) 0.037(4) Uani 0.50 1 d P A 1 C246 C 0.6117(8) 1.2346(6) 0.4172(5) 0.028(3) Uani 0.50 1 d P A 2 C247 C 0.5595(9) 1.2913(7) 0.4185(5) 0.034(3) Uani 0.50 1 d P A 2 N250 N 1.1572(3) 0.4571(3) 0.36177(19) 0.0352(14) Uani 1 1 d . . . C251 C 1.0825(5) 0.4583(4) 0.3404(4) 0.086(4) Uani 1 1 d . . . H251 H 1.0585 0.4177 0.3285 0.103 Uiso 1 1 calc R . . C252 C 1.0380(6) 0.5172(4) 0.3348(4) 0.089(4) Uani 1 1 d . . . H252 H 0.9827 0.5161 0.3209 0.107 Uiso 1 1 calc R . . C253 C 1.0731(5) 0.5772(3) 0.3490(3) 0.0417(19) Uani 1 1 d . . . C254 C 1.1534(4) 0.5748(3) 0.3696(2) 0.0347(17) Uani 1 1 d . . . H254 H 1.1805 0.6152 0.3796 0.042 Uiso 1 1 calc R . . C255 C 1.1944(4) 0.5148(3) 0.3757(2) 0.0337(16) Uani 1 1 d . . . H255 H 1.2496 0.5140 0.3898 0.040 Uiso 1 1 calc R . . N260 N 0.3466(3) 0.7645(3) 0.15157(17) 0.0290(12) Uani 1 1 d . . . C261 C 0.4240(4) 0.7603(3) 0.1463(2) 0.0314(15) Uani 1 1 d . . . H261 H 0.4357 0.7553 0.1190 0.038 Uiso 1 1 calc R . . C262 C 0.4879(4) 0.7634(3) 0.1806(2) 0.0307(15) Uani 1 1 d . . . H262 H 0.5428 0.7615 0.1765 0.037 Uiso 1 1 calc R . . C263 C 0.4717(4) 0.7690(3) 0.2204(2) 0.0307(15) Uani 1 1 d . . . C264 C 0.3903(4) 0.7734(4) 0.2244(2) 0.0398(18) Uani 1 1 d . . . H264 H 0.3765 0.7775 0.2512 0.048 Uiso 1 1 calc R . . C265 C 0.3300(4) 0.7719(4) 0.1899(2) 0.0371(17) Uani 1 1 d . . . H265 H 0.2748 0.7763 0.1932 0.045 Uiso 1 1 calc R . . N270 N 0.4143(4) 1.2411(3) 0.3541(2) 0.0487(18) Uani 1 1 d . . . C271 C 0.3860(4) 1.1809(3) 0.3617(2) 0.0350(16) Uani 1 1 d . . . H271 H 0.3345 1.1774 0.3700 0.042 Uiso 1 1 calc R . . C272 C 0.4298(4) 1.1236(3) 0.3579(2) 0.0338(16) Uani 1 1 d . . . H272 H 0.4079 1.0814 0.3639 0.041 Uiso 1 1 calc R B . C273 C 0.5026(6) 1.1249(4) 0.3459(3) 0.072(3) Uani 1 1 d . B . C274 C 0.5104(9) 1.1828(6) 0.3210(5) 0.032(3) Uani 0.50 1 d P B 1 C275 C 0.4666(9) 1.2406(6) 0.3263(5) 0.027(3) Uani 0.50 1 d P B 1 C276 C 0.5504(10) 1.1952(7) 0.3540(5) 0.040(4) Uani 0.50 1 d P B 2 C277 C 0.5003(10) 1.2508(7) 0.3543(6) 0.041(4) Uani 0.50 1 d P B 2 N280 N 1.0982(3) 0.9333(3) 0.15711(17) 0.0282(12) Uani 1 1 d . . . C281 C 1.0168(4) 0.9416(3) 0.1525(2) 0.0342(16) Uani 1 1 d . . . H281 H 0.9855 0.9491 0.1255 0.041 Uiso 1 1 calc R . . C282 C 0.9782(4) 0.9394(3) 0.1862(2) 0.0311(15) Uani 1 1 d . . . H282 H 0.9207 0.9450 0.1822 0.037 Uiso 1 1 calc R . . C283 C 1.0228(4) 0.9290(3) 0.2260(2) 0.0285(15) Uani 1 1 d . . . C284 C 1.1061(4) 0.9204(4) 0.2292(2) 0.046(2) Uani 1 1 d . . . H284 H 1.1387 0.9128 0.2559 0.055 Uiso 1 1 calc R . . C285 C 1.1434(4) 0.9225(4) 0.1948(2) 0.0381(17) Uani 1 1 d . . . H285 H 1.2007 0.9163 0.1980 0.046 Uiso 1 1 calc R . . Cl1 Cl 0.06723(10) 0.44633(8) 0.06267(6) 0.0362(4) Uani 1 1 d . . . O11 O 0.0715(3) 0.4067(3) 0.09962(17) 0.0512(14) Uani 1 1 d . . . O12 O 0.1345(3) 0.4298(2) 0.04265(17) 0.0446(13) Uani 1 1 d . . . O13 O -0.0083(3) 0.4320(2) 0.03498(17) 0.0412(12) Uani 1 1 d . . . O14 O 0.0711(3) 0.5171(2) 0.07294(18) 0.0486(14) Uani 1 1 d . . . Cl2 Cl 0.56326(12) 0.72520(10) 0.06258(8) 0.0536(6) Uani 1 1 d . . . O21 O 0.4891(4) 0.7619(3) 0.05639(19) 0.0579(15) Uiso 1 1 d . . . O22 O 0.5581(4) 0.6730(3) 0.0328(2) 0.0608(16) Uiso 1 1 d . . . O23 O 0.5733(5) 0.6929(4) 0.1010(3) 0.103(3) Uiso 1 1 d . . . O24 O 0.6282(5) 0.7675(4) 0.0557(3) 0.103(3) Uiso 1 1 d . . . Cl3 Cl 0.1297(5) 0.4452(3) 0.23548(18) 0.077(2) Uani 0.50 1 d PDU C -1 O31 O 0.0523(8) 0.4248(8) 0.2368(6) 0.118(6) Uiso 0.50 1 d PDU C -1 O32 O 0.1683(11) 0.4682(9) 0.2793(4) 0.129(7) Uiso 0.50 1 d PDU C -1 O33 O 0.1383(10) 0.5052(7) 0.2129(5) 0.100(5) Uiso 0.50 1 d PDU C -1 O34 O 0.1892(12) 0.3956(9) 0.2297(7) 0.139(10) Uiso 0.50 1 d PDU C -1 Cl3' Cl 0.1572(5) 0.4160(5) 0.2200(3) 0.122(4) Uani 0.50 1 d PD D -2 O31' O 0.1706(9) 0.4309(8) 0.2651(4) 0.089(5) Uiso 0.50 1 d PD D -2 O32' O 0.2249(11) 0.3641(9) 0.2216(7) 0.179(10) Uiso 0.50 1 d PD D -2 O33' O 0.1765(10) 0.4699(7) 0.1962(5) 0.103(5) Uiso 0.50 1 d PD D -2 O34' O 0.0869(8) 0.3853(7) 0.2043(5) 0.097(5) Uiso 0.50 1 d PD D -2 Cl4 Cl 0.7935(3) 0.9569(2) 0.08393(15) 0.0567(11) Uani 0.50 1 d PD E -1 O41 O 0.8243(6) 0.9439(5) 0.0487(3) 0.040(2) Uiso 0.50 1 d PD E -1 O42 O 0.7083(6) 0.9413(5) 0.0776(4) 0.060(3) Uiso 0.50 1 d PD E -1 O43 O 0.8382(8) 0.9122(6) 0.1146(4) 0.086(4) Uiso 0.50 1 d PD E -1 O44 O 0.8053(12) 1.0237(7) 0.0988(6) 0.131(8) Uiso 0.50 1 d PD E -1 Cl4' Cl 0.8114(3) 1.0603(2) 0.14644(19) 0.0720(16) Uani 0.50 1 d PD F -2 O41' O 0.7959(7) 0.9944(5) 0.1590(4) 0.066(3) Uiso 0.50 1 d PD F -2 O42' O 0.7559(9) 1.1067(7) 0.1550(5) 0.117(6) Uiso 0.50 1 d PD F -2 O43' O 0.8937(8) 1.0751(8) 0.1544(6) 0.131(7) Uiso 0.50 1 d PD F -2 O44' O 0.7894(14) 1.0543(12) 0.0983(4) 0.173(11) Uiso 0.50 1 d PD F -2 Cl5 Cl 0.2680(8) 0.2277(6) 0.0485(5) 0.105(6) Uani 0.50 1 d PD G -1 O51 O 0.2752(7) 0.1634(5) 0.0329(4) 0.063(3) Uiso 0.50 1 d PD G -1 O52 O 0.2377(8) 0.2208(7) 0.0880(4) 0.077(4) Uiso 0.50 1 d PD G -1 O53 O 0.3481(7) 0.2573(6) 0.0593(4) 0.079(4) Uiso 0.50 1 d PD G -1 O54 O 0.2126(11) 0.2665(9) 0.0208(6) 0.150(8) Uiso 0.50 1 d PD G -1 Cl5' Cl 0.2646(8) 0.2483(6) 0.0569(4) 0.074(3) Uani 0.50 1 d PD H -2 O51' O 0.2759(10) 0.1808(6) 0.0625(6) 0.103(5) Uiso 0.50 1 d PD H -2 O52' O 0.1810(7) 0.2664(6) 0.0612(4) 0.079(4) Uiso 0.50 1 d PD H -2 O53' O 0.3127(10) 0.2867(8) 0.0936(5) 0.144(7) Uiso 0.50 1 d PD H -2 O54' O 0.2831(11) 0.2831(8) 0.0230(5) 0.124(6) Uiso 0.50 1 d PD H -2 Cl6 Cl 0.6800(2) 1.27920(18) 0.30276(13) 0.0452(9) Uani 0.50 1 d PD I -1 O61 O 0.6199(6) 1.2588(5) 0.2625(3) 0.051(3) Uiso 0.50 1 d PD I -1 O62 O 0.6325(7) 1.3179(6) 0.3254(4) 0.069(4) Uiso 0.50 1 d PD I -1 O63 O 0.7411(6) 1.3197(6) 0.2905(4) 0.068(3) Uiso 0.50 1 d PD I -1 O64 O 0.7094(8) 1.2239(6) 0.3267(4) 0.085(4) Uiso 0.50 1 d PD I -1 Cl6' Cl 0.6494(3) 0.9473(2) 0.19728(17) 0.0684(14) Uani 0.50 1 d PD J -2 O61' O 0.6384(6) 0.9714(5) 0.2369(3) 0.043(2) Uiso 0.50 1 d PD J -2 O62' O 0.5876(7) 0.8997(6) 0.1806(4) 0.080(4) Uiso 0.50 1 d PD J -2 O63' O 0.6525(9) 0.9994(6) 0.1682(4) 0.086(4) Uiso 0.50 1 d PD J -2 O64' O 0.7249(7) 0.9104(7) 0.2074(5) 0.106(5) Uiso 0.50 1 d PD J -2 Cl10 Cl 0.8753(4) 1.1154(3) 0.3115(2) 0.0938(19) Uani 0.50 1 d P K -1 C11 C 0.9729(8) 1.1022(8) 0.3106(4) 0.054(4) Uiso 0.50 1 d PD K -1 C12 C 0.9937(10) 1.0938(10) 0.2709(5) 0.072(6) Uiso 0.50 1 d PD K -1 C13 C 1.0789(11) 1.0829(13) 0.2716(6) 0.087(8) Uiso 0.50 1 d PD K -1 C14 C 1.1373(11) 1.0794(13) 0.3054(6) 0.107(8) Uiso 0.50 1 d PD K -1 C15 C 1.1153(10) 1.0894(13) 0.3420(6) 0.097(8) Uiso 0.50 1 d PD K -1 C16 C 1.0327(10) 1.0987(10) 0.3469(5) 0.071(5) Uiso 0.50 1 d PD K -1 Cl20 Cl 1.0435(3) 1.1016(2) 0.2468(2) 0.0811(17) Uani 0.50 1 d P L -2 C21 C 0.9424(8) 1.1005(5) 0.2483(4) 0.041(4) Uiso 0.50 1 d PD L -2 C22 C 0.9209(8) 1.1120(6) 0.2873(4) 0.050(4) Uiso 0.50 1 d PD L -2 C23 C 0.8350(9) 1.1148(7) 0.2871(5) 0.066(6) Uiso 0.50 1 d PD L -2 C24 C 0.7774(10) 1.1075(7) 0.2538(5) 0.070(5) Uiso 0.50 1 d PD L -2 C25 C 0.8000(9) 1.0966(7) 0.2173(5) 0.081(6) Uiso 0.50 1 d PD L -2 C26 C 0.8828(9) 1.0922(6) 0.2118(4) 0.059(5) Uiso 0.50 1 d PD L -2 Cl30 Cl 0.1136(3) 0.1143(2) 0.15428(13) 0.0613(12) Uani 0.50 1 d P M -1 C31 C 0.1920(10) 0.1487(6) 0.1846(5) 0.058(5) Uiso 0.50 1 d PD M -1 C32 C 0.2117(9) 0.2169(6) 0.1808(5) 0.044(4) Uiso 0.50 1 d PD M -1 C33 C 0.2782(13) 0.2431(9) 0.2100(7) 0.112(9) Uiso 0.50 1 d PD M -1 C34 C 0.3239(15) 0.2058(10) 0.2387(8) 0.139(11) Uiso 0.50 1 d PD M -1 C35 C 0.3050(12) 0.1416(9) 0.2409(6) 0.087(7) Uiso 0.50 1 d PD M -1 C36 C 0.2397(10) 0.1071(7) 0.2148(5) 0.065(5) Uiso 0.50 1 d PD M -1 C41 C 0.6204(12) 1.0425(9) 0.2447(10) 0.124(10) Uiso 0.50 1 d PD I 1 C42 C 0.6877(11) 1.0858(10) 0.2458(8) 0.094(7) Uiso 0.50 1 d PD I 1 C43 C 0.6751(13) 1.1558(10) 0.2520(10) 0.124(10) Uiso 0.50 1 d PD I 1 C44 C 0.6044(12) 1.1850(9) 0.2553(9) 0.105(8) Uiso 0.50 1 d PD I 1 C45 C 0.5425(10) 1.1426(8) 0.2548(7) 0.074(6) Uiso 0.50 1 d PD I 1 C46 C 0.5465(11) 1.0712(9) 0.2514(8) 0.096(7) Uiso 0.50 1 d PD I 1 O1 O 0.7503(7) 1.2180(6) 0.3627(4) 0.062(3) Uiso 0.50 1 d PD N 2 C1 C 0.7529(12) 1.2820(8) 0.3471(6) 0.071(5) Uiso 0.50 1 d PD N 2 O2 O 0.6307(8) 0.9567(6) 0.1294(4) 0.067(3) Uiso 0.50 1 d PD O 1 C2 C 0.6182(14) 0.8908(9) 0.1390(8) 0.089(7) Uiso 0.50 1 d PD O 1 O3 O 0.3451(10) 0.2588(8) 0.2509(5) 0.022(4) Uiso 0.25 1 d P P 2 C4 C 0.2849(11) 0.4280(8) 0.1335(5) 0.053(4) Uiso 0.50 1 d PD Q 1 O4 O 0.2729(14) 0.4284(11) 0.1684(6) 0.057(6) Uiso 0.25 1 d PD Q 1 O4' O 0.2807(13) 0.3716(9) 0.1273(7) 0.051(6) Uiso 0.25 1 d PD Q 1 O5 O 1.1756(15) 1.0898(12) 0.3513(8) 0.066(7) Uiso 0.25 1 d PD R 2 C5 C 1.2483(16) 1.0757(15) 0.3519(10) 0.044(7) Uiso 0.25 1 d PD R 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 0.02034(19) 0.02068(18) 0.0178(2) 0.00031(14) 0.00209(14) 0.00245(14) La2 0.0226(2) 0.02136(18) 0.0239(2) 0.00313(15) 0.00642(16) 0.00340(14) O110 0.043(3) 0.031(2) 0.032(3) 0.002(2) 0.017(2) 0.013(2) O120 0.040(3) 0.034(2) 0.027(3) 0.000(2) 0.018(2) -0.003(2) O130 0.035(3) 0.028(2) 0.033(3) 0.001(2) -0.005(2) 0.009(2) O140 0.033(3) 0.031(2) 0.028(3) -0.003(2) -0.008(2) 0.006(2) O150 0.026(2) 0.024(2) 0.049(3) 0.008(2) 0.006(2) 0.0056(19) O160 0.029(3) 0.026(2) 0.037(3) 0.002(2) 0.002(2) -0.0065(19) O170 0.030(2) 0.024(2) 0.036(3) -0.004(2) 0.012(2) 0.0034(19) O180 0.031(3) 0.026(2) 0.034(3) -0.0036(19) 0.011(2) -0.0068(19) O210 0.030(2) 0.025(2) 0.031(3) -0.0009(19) 0.011(2) -0.0052(19) O220 0.032(3) 0.023(2) 0.050(3) 0.009(2) 0.021(2) 0.0104(19) O230 0.027(2) 0.028(2) 0.037(3) 0.004(2) 0.003(2) -0.0050(19) O240 0.027(3) 0.023(2) 0.065(4) -0.002(2) 0.007(2) 0.0052(19) O250 0.033(3) 0.027(2) 0.055(4) 0.007(2) -0.005(2) 0.010(2) O260 0.036(3) 0.032(2) 0.024(3) 0.000(2) -0.007(2) -0.001(2) O270 0.055(3) 0.038(3) 0.042(3) 0.006(2) 0.026(3) 0.019(2) O280 0.042(3) 0.030(2) 0.029(3) -0.008(2) 0.021(2) -0.006(2) N110 0.035(3) 0.029(3) 0.027(3) 0.003(2) 0.011(3) 0.006(2) C111 0.043(5) 0.028(4) 0.141(10) -0.013(5) 0.004(6) 0.008(4) C112 0.035(5) 0.036(4) 0.118(9) -0.020(5) 0.004(5) -0.001(4) C113 0.035(4) 0.030(3) 0.041(5) 0.001(3) -0.007(3) 0.007(3) C114 0.046(6) 0.027(4) 0.272(19) -0.035(7) -0.042(8) 0.007(4) C115 0.036(5) 0.039(5) 0.191(14) -0.018(6) -0.026(7) 0.005(4) N120 0.032(3) 0.033(3) 0.031(4) 0.000(3) 0.015(3) -0.001(2) C121 0.037(4) 0.080(6) 0.018(4) -0.006(4) 0.007(3) -0.010(4) C122 0.027(4) 0.091(6) 0.021(4) 0.000(4) 0.006(3) -0.008(4) C123 0.030(4) 0.040(4) 0.018(4) -0.003(3) 0.006(3) -0.006(3) C124 0.031(4) 0.043(4) 0.018(4) -0.001(3) 0.000(3) 0.000(3) C125 0.027(4) 0.039(4) 0.027(4) 0.001(3) 0.003(3) 0.000(3) N130 0.037(3) 0.027(3) 0.033(4) 0.004(2) 0.005(3) 0.012(3) C131 0.053(5) 0.029(4) 0.086(7) 0.011(4) 0.046(5) 0.006(4) C132 0.083(7) 0.027(4) 0.148(11) 0.027(5) 0.084(7) 0.018(4) C133 0.072(6) 0.034(4) 0.086(7) 0.020(4) 0.055(6) 0.019(4) C134 0.043(4) 0.040(4) 0.043(5) 0.011(3) 0.016(4) 0.014(3) C135 0.038(4) 0.033(3) 0.030(4) 0.004(3) 0.002(3) 0.001(3) N140 0.029(3) 0.028(3) 0.027(3) -0.005(2) -0.004(3) 0.002(2) C141 0.040(4) 0.067(5) 0.016(4) 0.000(4) 0.002(3) -0.014(4) C142 0.037(4) 0.081(6) 0.029(5) 0.002(4) 0.000(4) -0.022(4) C143 0.038(4) 0.028(3) 0.019(4) -0.005(3) 0.000(3) -0.004(3) C144 0.033(4) 0.038(4) 0.022(4) 0.000(3) 0.002(3) -0.002(3) C145 0.027(4) 0.045(4) 0.030(4) 0.003(3) 0.005(3) 0.000(3) N150 0.030(3) 0.024(3) 0.040(4) 0.012(2) 0.014(3) 0.007(2) C151 0.031(4) 0.030(4) 0.099(8) 0.007(4) 0.006(4) 0.006(3) C152 0.038(5) 0.024(4) 0.123(9) 0.005(4) 0.016(5) 0.009(3) C153 0.033(4) 0.033(4) 0.042(5) 0.013(3) 0.014(3) 0.005(3) C154 0.037(4) 0.031(4) 0.065(6) -0.004(4) -0.007(4) 0.008(3) C155 0.034(4) 0.035(4) 0.061(6) -0.005(4) -0.003(4) 0.009(3) N160 0.025(3) 0.025(3) 0.029(3) -0.001(2) 0.004(2) -0.004(2) C161 0.027(4) 0.028(3) 0.063(6) -0.003(3) 0.009(4) 0.002(3) C162 0.030(4) 0.033(4) 0.066(6) 0.000(4) 0.012(4) 0.002(3) C163 0.027(3) 0.031(3) 0.021(4) -0.002(3) 0.005(3) -0.004(3) C164 0.032(4) 0.026(3) 0.049(5) -0.003(3) 0.004(3) -0.001(3) C165 0.032(4) 0.030(3) 0.044(5) -0.003(3) 0.002(3) 0.002(3) N170 0.025(3) 0.024(3) 0.043(4) -0.001(2) 0.012(3) 0.002(2) C171 0.037(4) 0.025(4) 0.121(9) 0.002(4) 0.040(5) 0.000(3) C172 0.045(5) 0.028(4) 0.168(11) 0.006(5) 0.059(6) 0.001(4) C173 0.035(4) 0.026(4) 0.105(8) 0.004(4) 0.032(5) 0.006(3) C174 0.030(4) 0.031(3) 0.054(5) -0.001(3) 0.015(3) -0.003(3) C175 0.026(3) 0.021(3) 0.035(4) 0.000(3) 0.008(3) -0.004(3) N180 0.028(3) 0.027(3) 0.021(3) -0.003(2) 0.007(2) -0.006(2) C181 0.025(3) 0.025(3) 0.034(4) 0.003(3) 0.006(3) 0.001(3) C182 0.024(3) 0.033(3) 0.029(4) -0.002(3) 0.001(3) 0.002(3) C183 0.028(4) 0.027(3) 0.024(4) -0.002(3) 0.005(3) -0.002(3) C184 0.026(4) 0.031(3) 0.031(4) -0.003(3) 0.005(3) -0.002(3) C185 0.024(3) 0.028(3) 0.032(4) -0.004(3) 0.006(3) 0.002(3) N210 0.026(3) 0.026(3) 0.026(3) -0.002(2) 0.006(2) -0.006(2) C211 0.029(4) 0.030(3) 0.039(4) -0.007(3) 0.011(3) -0.002(3) C212 0.032(4) 0.025(3) 0.045(5) -0.006(3) 0.010(3) -0.003(3) C213 0.026(3) 0.027(3) 0.024(4) -0.002(3) 0.001(3) -0.003(3) C214 0.024(3) 0.033(3) 0.023(4) -0.002(3) 0.003(3) -0.003(3) C215 0.025(3) 0.027(3) 0.029(4) 0.002(3) 0.007(3) 0.001(3) N220 0.031(3) 0.028(3) 0.045(4) 0.014(3) 0.023(3) 0.008(2) C221 0.035(4) 0.025(3) 0.037(4) 0.004(3) 0.016(3) 0.005(3) C222 0.042(4) 0.032(4) 0.036(4) 0.006(3) 0.014(4) 0.007(3) C223 0.034(4) 0.030(3) 0.046(5) 0.011(3) 0.021(3) 0.008(3) C224 0.032(4) 0.036(4) 0.083(7) 0.006(4) 0.011(4) 0.000(3) C225 0.036(4) 0.023(3) 0.081(7) 0.003(4) 0.017(4) 0.004(3) N230 0.029(3) 0.023(3) 0.025(3) 0.007(2) 0.001(2) -0.003(2) C231 0.029(4) 0.032(3) 0.031(4) 0.004(3) 0.009(3) 0.002(3) C232 0.035(4) 0.026(3) 0.032(4) -0.001(3) 0.008(3) -0.001(3) C233 0.029(4) 0.029(3) 0.021(4) 0.003(3) 0.003(3) -0.002(3) C234 0.027(4) 0.036(4) 0.026(4) 0.007(3) 0.006(3) 0.004(3) C235 0.030(4) 0.028(3) 0.025(4) 0.003(3) 0.004(3) 0.003(3) N240 0.028(3) 0.022(3) 0.087(6) 0.003(3) 0.018(3) 0.006(2) C241 0.024(3) 0.031(3) 0.024(4) 0.001(3) -0.001(3) 0.005(3) C242 0.026(4) 0.029(3) 0.034(4) -0.005(3) -0.001(3) 0.004(3) C243 0.042(5) 0.025(4) 0.121(9) 0.000(4) 0.037(5) 0.003(3) C244 0.029(8) 0.040(8) 0.059(12) -0.003(8) 0.023(8) -0.008(7) C245 0.037(9) 0.020(7) 0.059(12) 0.012(7) 0.023(9) 0.004(6) C246 0.026(7) 0.029(7) 0.026(8) -0.001(6) -0.002(6) -0.001(6) C247 0.031(8) 0.041(8) 0.027(9) -0.002(7) -0.002(7) 0.002(6) N250 0.035(3) 0.026(3) 0.040(4) 0.002(3) -0.004(3) 0.002(2) C251 0.052(6) 0.029(4) 0.148(11) -0.021(5) -0.058(6) 0.009(4) C252 0.054(6) 0.041(5) 0.143(11) -0.024(6) -0.055(6) 0.014(4) C253 0.042(4) 0.029(4) 0.050(5) -0.006(3) -0.002(4) 0.007(3) C254 0.032(4) 0.026(3) 0.043(5) -0.005(3) 0.000(3) 0.001(3) C255 0.032(4) 0.034(4) 0.032(4) 0.002(3) -0.001(3) 0.001(3) N260 0.034(3) 0.027(3) 0.022(3) -0.004(2) -0.003(3) 0.001(2) C261 0.035(4) 0.033(3) 0.026(4) -0.003(3) 0.004(3) 0.006(3) C262 0.028(4) 0.039(4) 0.023(4) 0.003(3) -0.001(3) 0.007(3) C263 0.042(4) 0.027(3) 0.021(4) -0.002(3) 0.001(3) 0.000(3) C264 0.036(4) 0.059(5) 0.023(4) 0.001(3) 0.001(3) -0.008(4) C265 0.029(4) 0.054(4) 0.026(4) -0.004(3) 0.001(3) -0.006(3) N270 0.056(4) 0.038(3) 0.063(5) 0.015(3) 0.039(4) 0.022(3) C271 0.033(4) 0.041(4) 0.032(4) 0.003(3) 0.011(3) 0.008(3) C272 0.039(4) 0.033(3) 0.029(4) 0.004(3) 0.007(3) 0.005(3) C273 0.077(7) 0.043(5) 0.117(9) 0.047(5) 0.071(7) 0.032(5) C274 0.039(8) 0.023(6) 0.037(9) 0.008(6) 0.020(7) 0.011(6) C275 0.037(8) 0.029(7) 0.016(8) -0.005(6) 0.007(6) 0.000(6) C276 0.053(10) 0.029(7) 0.039(10) -0.003(7) 0.007(8) 0.003(7) C277 0.046(10) 0.034(8) 0.050(11) 0.002(8) 0.023(9) 0.005(7) N280 0.031(3) 0.033(3) 0.023(3) -0.007(2) 0.009(3) -0.004(2) C281 0.040(4) 0.037(4) 0.025(4) 0.003(3) 0.005(3) -0.004(3) C282 0.030(4) 0.039(4) 0.025(4) -0.001(3) 0.006(3) 0.002(3) C283 0.029(4) 0.036(3) 0.020(4) -0.006(3) 0.005(3) 0.000(3) C284 0.030(4) 0.086(6) 0.021(4) -0.012(4) 0.003(3) -0.001(4) C285 0.028(4) 0.055(4) 0.032(5) -0.008(4) 0.009(3) -0.003(3) Cl1 0.0350(9) 0.0367(9) 0.0391(11) -0.0003(8) 0.0127(8) -0.0024(7) O11 0.054(3) 0.058(3) 0.043(4) 0.016(3) 0.013(3) 0.001(3) O12 0.040(3) 0.048(3) 0.051(4) -0.002(3) 0.021(3) 0.000(2) O13 0.032(3) 0.042(3) 0.047(3) -0.006(2) 0.004(2) -0.002(2) O14 0.054(3) 0.038(3) 0.056(4) -0.010(3) 0.016(3) -0.008(2) Cl2 0.0367(11) 0.0479(11) 0.0795(17) -0.0125(11) 0.0197(11) -0.0008(9) Cl3 0.118(6) 0.068(3) 0.037(3) 0.007(2) -0.004(3) 0.036(3) Cl3' 0.079(5) 0.162(9) 0.121(8) 0.090(7) 0.007(5) 0.003(6) Cl4 0.047(2) 0.056(2) 0.066(3) 0.020(2) 0.007(2) -0.002(2) Cl4' 0.038(2) 0.039(2) 0.135(5) 0.020(3) 0.005(3) 0.0087(18) Cl5 0.036(4) 0.103(8) 0.169(13) 0.083(8) -0.001(6) 0.004(5) Cl5' 0.046(5) 0.093(7) 0.079(5) 0.047(4) 0.005(3) -0.022(4) Cl6 0.048(2) 0.0414(19) 0.053(3) 0.0061(18) 0.027(2) 0.0002(17) Cl6' 0.051(3) 0.051(2) 0.094(4) 0.008(3) -0.008(3) 0.000(2) Cl10 0.118(5) 0.056(3) 0.099(5) -0.010(3) -0.001(4) 0.003(3) Cl20 0.059(3) 0.051(3) 0.138(6) -0.010(3) 0.032(4) 0.000(2) Cl30 0.085(3) 0.058(2) 0.031(2) -0.0134(19) -0.015(2) 0.013(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 La1 O150 2.429(4) . ? La1 O170 2.436(4) . ? La1 O110 2.457(4) . ? La1 O130 2.470(4) . ? La1 O140 2.525(4) . ? La1 O180 2.533(4) . ? La1 O120 2.534(4) . ? La1 O160 2.580(5) . ? La2 O250 2.437(4) 1_455 ? La2 O230 2.470(4) 1_445 ? La2 O280 2.498(4) 2_645 ? La2 O270 2.504(5) 1_545 ? La2 O260 2.515(4) 2_545 ? La2 O210 2.515(4) . ? La2 O240 2.516(5) 1_545 ? La2 O220 2.560(4) 1_455 ? O110 N110 1.329(6) . ? O120 N120 1.332(7) . ? O130 N130 1.322(6) . ? O140 N140 1.338(7) . ? O150 N150 1.329(6) . ? O160 N160 1.332(6) . ? O170 N170 1.320(6) . ? O180 N180 1.334(6) . ? O210 N210 1.330(6) . ? O220 N220 1.344(6) . ? O220 La2 2.560(4) 1_655 ? O230 N230 1.331(6) . ? O230 La2 2.470(4) 1_665 ? O240 N240 1.332(7) . ? O240 La2 2.516(5) 1_565 ? O250 N250 1.316(6) . ? O250 La2 2.437(4) 1_655 ? O260 N260 1.316(7) . ? O260 La2 2.515(4) 2 ? O270 N270 1.300(7) . ? O270 La2 2.504(5) 1_565 ? O280 N280 1.306(6) . ? O280 La2 2.498(4) 2_655 ? N110 C115 1.282(10) . ? N110 C111 1.302(10) . ? C111 C112 1.374(10) . ? C112 C113 1.336(10) . ? C113 C114 1.365(12) . ? C113 C253 1.455(9) . ? C114 C115 1.371(12) . ? N120 C125 1.338(9) . ? N120 C121 1.352(9) . ? C121 C122 1.357(10) . ? C122 C123 1.423(10) . ? C123 C124 1.385(9) . ? C123 C283 1.471(9) . ? C124 C125 1.354(9) . ? N130 C135 1.328(9) . ? N130 C131 1.344(8) . ? C131 C132 1.362(10) . ? C132 C133 1.403(12) . ? C133 C134 1.369(10) . ? C133 C273 1.470(10) . ? C134 C135 1.375(9) . ? N140 C145 1.342(9) . ? N140 C141 1.357(9) . ? C141 C142 1.346(10) . ? C142 C143 1.413(10) . ? C143 C144 1.380(9) . ? C143 C263 1.466(9) . ? C144 C145 1.361(9) . ? N150 C155 1.318(9) . ? N150 C151 1.345(9) . ? C151 C152 1.388(10) . ? C152 C153 1.386(11) . ? C153 C154 1.379(9) . ? C153 C223 1.469(9) . ? C154 C155 1.366(9) . ? N160 C161 1.319(8) . ? N160 C165 1.339(8) . ? C161 C162 1.381(9) . ? C162 C163 1.375(9) . ? C163 C164 1.378(9) . ? C163 C233 1.465(8) . ? C164 C165 1.368(9) . ? N170 C175 1.343(8) . ? N170 C171 1.348(8) . ? C171 C172 1.360(10) . ? C172 C173 1.378(10) . ? C173 C174 1.379(9) . ? C173 C243 1.474(10) . ? C174 C175 1.371(9) . ? N180 C185 1.326(8) . ? N180 C181 1.352(8) . ? C181 C182 1.373(9) . ? C182 C183 1.397(9) . ? C183 C184 1.386(9) . ? C183 C213 1.488(8) . ? C184 C185 1.363(9) . ? N210 C211 1.352(8) . ? N210 C215 1.357(8) . ? C211 C212 1.386(9) . ? C212 C213 1.368(9) . ? C213 C214 1.408(8) . ? C214 C215 1.351(8) . ? N220 C225 1.330(9) . ? N220 C221 1.334(8) . ? C221 C222 1.368(9) . ? C222 C223 1.384(10) . ? C223 C224 1.392(10) . ? C224 C225 1.380(9) . ? N230 C235 1.344(8) . ? N230 C231 1.349(8) . ? C231 C232 1.376(9) . ? C232 C233 1.404(9) . ? C233 C234 1.394(8) . ? C234 C235 1.363(9) . ? N240 C241 1.324(8) . ? N240 C245 1.373(15) . ? N240 C247 1.452(17) . ? C241 C242 1.379(8) . ? C242 C243 1.374(10) . ? C243 C244 1.373(15) . ? C243 C246 1.531(16) . ? C244 C245 1.40(2) . ? C246 C247 1.429(19) . ? N250 C251 1.312(9) . ? N250 C255 1.342(8) . ? C251 C252 1.380(11) . ? C252 C253 1.371(10) . ? C253 C254 1.385(10) . ? C254 C255 1.371(9) . ? N260 C261 1.337(8) . ? N260 C265 1.341(9) . ? C261 C262 1.398(9) . ? C262 C263 1.382(9) . ? C263 C264 1.392(10) . ? C264 C265 1.363(10) . ? N270 C271 1.326(9) . ? N270 C275 1.371(14) . ? N270 C277 1.448(17) . ? C271 C272 1.371(9) . ? C272 C273 1.344(10) . ? C273 C274 1.430(14) . ? C273 C276 1.607(17) . ? C274 C275 1.390(17) . ? C276 C277 1.39(2) . ? N280 C285 1.338(9) . ? N280 C281 1.349(8) . ? C281 C282 1.375(9) . ? C282 C283 1.391(9) . ? C283 C284 1.385(9) . ? C284 C285 1.381(10) . ? Cl1 O11 1.432(5) . ? Cl1 O13 1.437(5) . ? Cl1 O12 1.438(5) . ? Cl1 O14 1.444(5) . ? Cl2 O23 1.390(9) . ? Cl2 O22 1.414(6) . ? Cl2 O21 1.419(6) . ? Cl2 O24 1.422(8) . ? Cl3 O31 1.363(12) . ? Cl3 O33 1.424(12) . ? Cl3 O34 1.436(13) . ? Cl3 O32 1.527(13) . ? Cl3' O34' 1.337(12) . ? Cl3' O33' 1.395(12) . ? Cl3' O31' 1.479(13) . ? Cl3' O32' 1.523(14) . ? Cl4 O41 1.370(9) . ? Cl4 O44 1.417(12) . ? Cl4 O42 1.432(9) . ? Cl4 O43 1.441(10) . ? Cl4' O42' 1.371(11) . ? Cl4' O43' 1.382(12) . ? Cl4' O41' 1.411(10) . ? Cl4' O44' 1.551(13) . ? Cl5 O51 1.389(14) . ? Cl5 O54 1.399(14) . ? Cl5 O53 1.443(14) . ? Cl5 O52 1.477(14) . ? Cl5' O51' 1.363(14) . ? Cl5' O54' 1.387(14) . ? Cl5' O52' 1.472(14) . ? Cl5' O53' 1.518(15) . ? Cl6 O64 1.386(10) . ? Cl6 O62 1.409(9) . ? Cl6 O63 1.414(9) . ? Cl6 O61 1.552(9) . ? O61 C44 1.50(2) . ? Cl6' O63' 1.413(10) . ? Cl6' O61' 1.423(9) . ? Cl6' O62' 1.432(10) . ? Cl6' O64' 1.442(11) . ? Cl10 C11 1.655(15) . ? C11 C16 1.404(10) . ? C11 C12 1.410(10) . ? C12 C13 1.434(12) . ? C13 C14 1.330(12) . ? C14 C15 1.331(12) . ? C15 C16 1.429(12) . ? Cl20 C21 1.696(13) . ? C21 C22 1.404(10) . ? C21 C26 1.413(10) . ? C22 C23 1.434(12) . ? C23 C24 1.320(12) . ? C24 C25 1.332(12) . ? C25 C26 1.428(12) . ? Cl30 C31 1.637(15) . ? C31 C32 1.405(10) . ? C31 C36 1.414(10) . ? C32 C33 1.422(12) . ? C33 C34 1.322(12) . ? C34 C35 1.319(12) . ? C35 C36 1.428(12) . ? C41 C42 1.411(11) . ? C41 C46 1.413(11) . ? C42 C43 1.427(12) . ? C43 C44 1.336(12) . ? C44 C45 1.331(12) . ? C45 C46 1.426(12) . ? O1 C1 1.376(15) . ? O2 C2 1.371(16) . ? C4 O4' 1.139(16) . ? C4 O4 1.195(17) . ? O5 C5 1.242(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O150 La1 O170 118.19(16) . . ? O150 La1 O110 86.08(15) . . ? O170 La1 O110 138.28(15) . . ? O150 La1 O130 141.60(15) . . ? O170 La1 O130 84.97(15) . . ? O110 La1 O130 95.94(15) . . ? O150 La1 O140 73.82(15) . . ? O170 La1 O140 141.20(14) . . ? O110 La1 O140 75.25(16) . . ? O130 La1 O140 69.75(14) . . ? O150 La1 O180 78.30(14) . . ? O170 La1 O180 72.39(14) . . ? O110 La1 O180 149.09(14) . . ? O130 La1 O180 80.89(15) . . ? O140 La1 O180 74.84(15) . . ? O150 La1 O120 140.32(15) . . ? O170 La1 O120 70.61(14) . . ? O110 La1 O120 69.66(14) . . ? O130 La1 O120 74.01(15) . . ? O140 La1 O120 125.61(15) . . ? O180 La1 O120 136.56(13) . . ? O150 La1 O160 69.63(14) . . ? O170 La1 O160 77.65(14) . . ? O110 La1 O160 80.73(16) . . ? O130 La1 O160 148.63(14) . . ? O140 La1 O160 137.20(13) . . ? O180 La1 O160 117.34(15) . . ? O120 La1 O160 75.64(14) . . ? O250 La2 O230 129.78(15) 1_455 1_445 ? O250 La2 O280 74.35(16) 1_455 2_645 ? O230 La2 O280 153.12(14) 1_445 2_645 ? O250 La2 O270 98.30(17) 1_455 1_545 ? O230 La2 O270 92.31(15) 1_445 1_545 ? O280 La2 O270 69.95(14) 2_645 1_545 ? O250 La2 O260 68.84(14) 1_455 2_545 ? O230 La2 O260 67.42(14) 1_445 2_545 ? O280 La2 O260 122.91(15) 2_645 2_545 ? O270 La2 O260 73.95(16) 1_545 2_545 ? O250 La2 O210 93.08(15) 1_455 . ? O230 La2 O210 115.52(15) 1_445 . ? O280 La2 O210 68.12(14) 2_645 . ? O270 La2 O210 131.42(15) 1_545 . ? O260 La2 O210 152.15(14) 2_545 . ? O250 La2 O240 155.30(15) 1_455 1_545 ? O230 La2 O240 74.91(14) 1_445 1_545 ? O280 La2 O240 81.41(15) 2_645 1_545 ? O270 La2 O240 77.37(17) 1_545 1_545 ? O260 La2 O240 130.88(14) 2_545 1_545 ? O210 La2 O240 73.20(14) . 1_545 ? O250 La2 O220 78.08(16) 1_455 1_455 ? O230 La2 O220 75.09(14) 1_445 1_455 ? O280 La2 O220 127.43(13) 2_645 1_455 ? O270 La2 O220 158.88(16) 1_545 1_455 ? O260 La2 O220 85.46(15) 2_545 1_455 ? O210 La2 O220 69.70(14) . 1_455 ? O240 La2 O220 114.36(17) 1_545 1_455 ? N110 O110 La1 131.1(4) . . ? N120 O120 La1 124.4(3) . . ? N130 O130 La1 135.0(4) . . ? N140 O140 La1 129.7(3) . . ? N150 O150 La1 149.0(4) . . ? N160 O160 La1 133.9(4) . . ? N170 O170 La1 143.9(4) . . ? N180 O180 La1 131.2(3) . . ? N210 O210 La2 133.3(3) . . ? N220 O220 La2 122.3(3) . 1_655 ? N230 O230 La2 136.8(4) . 1_665 ? N240 O240 La2 129.5(4) . 1_565 ? N250 O250 La2 142.0(4) . 1_655 ? N260 O260 La2 129.6(3) . 2 ? N270 O270 La2 137.3(4) . 1_565 ? N280 O280 La2 130.2(3) . 2_655 ? C115 N110 C111 119.1(7) . . ? C115 N110 O110 120.5(6) . . ? C111 N110 O110 120.3(6) . . ? N110 C111 C112 121.6(8) . . ? C113 C112 C111 121.7(8) . . ? C112 C113 C114 114.2(7) . . ? C112 C113 C253 123.2(7) . . ? C114 C113 C253 122.5(7) . . ? C113 C114 C115 122.4(8) . . ? N110 C115 C114 120.7(8) . . ? O120 N120 C125 119.9(6) . . ? O120 N120 C121 119.5(6) . . ? C125 N120 C121 120.6(6) . . ? N120 C121 C122 121.1(7) . . ? C121 C122 C123 120.0(7) . . ? C124 C123 C122 115.8(6) . . ? C124 C123 C283 123.6(6) . . ? C122 C123 C283 120.5(6) . . ? C125 C124 C123 122.4(6) . . ? N120 C125 C124 120.1(6) . . ? O130 N130 C135 119.1(5) . . ? O130 N130 C131 119.8(6) . . ? C135 N130 C131 121.1(6) . . ? N130 C131 C132 119.2(7) . . ? C131 C132 C133 121.4(7) . . ? C134 C133 C132 116.9(7) . . ? C134 C133 C273 121.6(8) . . ? C132 C133 C273 121.3(7) . . ? C133 C134 C135 120.2(7) . . ? N130 C135 C134 121.1(6) . . ? O140 N140 C145 121.4(6) . . ? O140 N140 C141 118.7(6) . . ? C145 N140 C141 119.9(6) . . ? C142 C141 N140 120.5(7) . . ? C141 C142 C143 121.7(7) . . ? C144 C143 C142 115.3(6) . . ? C144 C143 C263 123.1(6) . . ? C142 C143 C263 121.5(6) . . ? C145 C144 C143 122.1(7) . . ? N140 C145 C144 120.6(6) . . ? C155 N150 O150 121.6(5) . . ? C155 N150 C151 120.8(6) . . ? O150 N150 C151 117.6(6) . . ? N150 C151 C152 119.2(7) . . ? C153 C152 C151 121.1(7) . . ? C154 C153 C152 116.6(6) . . ? C154 C153 C223 122.1(7) . . ? C152 C153 C223 121.3(6) . . ? C155 C154 C153 120.8(7) . . ? N150 C155 C154 121.5(7) . . ? C161 N160 O160 120.4(5) . . ? C161 N160 C165 119.6(6) . . ? O160 N160 C165 120.0(5) . . ? N160 C161 C162 120.3(6) . . ? C163 C162 C161 122.1(7) . . ? C162 C163 C164 115.3(6) . . ? C162 C163 C233 124.6(6) . . ? C164 C163 C233 120.1(6) . . ? C165 C164 C163 121.4(6) . . ? N160 C165 C164 121.2(6) . . ? O170 N170 C175 119.9(5) . . ? O170 N170 C171 119.8(5) . . ? C175 N170 C171 120.2(5) . . ? N170 C171 C172 121.0(7) . . ? C171 C172 C173 119.9(7) . . ? C172 C173 C174 118.4(6) . . ? C172 C173 C243 121.6(7) . . ? C174 C173 C243 119.9(7) . . ? C175 C174 C173 120.2(6) . . ? N170 C175 C174 120.2(6) . . ? C185 N180 O180 119.9(5) . . ? C185 N180 C181 120.7(5) . . ? O180 N180 C181 119.4(5) . . ? N180 C181 C182 120.6(6) . . ? C181 C182 C183 119.9(6) . . ? C184 C183 C182 116.9(6) . . ? C184 C183 C213 121.7(6) . . ? C182 C183 C213 121.4(6) . . ? C185 C184 C183 121.3(6) . . ? N180 C185 C184 120.6(6) . . ? O210 N210 C211 118.8(5) . . ? O210 N210 C215 120.9(5) . . ? C211 N210 C215 120.3(5) . . ? N210 C211 C212 119.8(6) . . ? C213 C212 C211 121.2(6) . . ? C212 C213 C214 117.0(6) . . ? C212 C213 C183 122.0(6) . . ? C214 C213 C183 121.0(6) . . ? C215 C214 C213 121.0(6) . . ? C214 C215 N210 120.6(6) . . ? C225 N220 C221 120.1(6) . . ? C225 N220 O220 120.0(6) . . ? C221 N220 O220 119.9(6) . . ? N220 C221 C222 120.4(7) . . ? C221 C222 C223 122.2(7) . . ? C222 C223 C224 115.2(6) . . ? C222 C223 C153 122.2(7) . . ? C224 C223 C153 122.6(7) . . ? C225 C224 C223 121.0(8) . . ? N220 C225 C224 120.9(7) . . ? O230 N230 C235 120.3(5) . . ? O230 N230 C231 118.6(5) . . ? C235 N230 C231 121.1(5) . . ? N230 C231 C232 120.3(6) . . ? C231 C232 C233 120.4(6) . . ? C234 C233 C232 116.5(6) . . ? C234 C233 C163 121.8(6) . . ? C232 C233 C163 121.7(6) . . ? C235 C234 C233 121.5(6) . . ? N230 C235 C234 120.0(6) . . ? C241 N240 O240 119.9(6) . . ? C241 N240 C245 115.0(8) . . ? O240 N240 C245 120.6(7) . . ? C241 N240 C247 123.6(8) . . ? O240 N240 C247 113.6(8) . . ? N240 C241 C242 121.6(6) . . ? C243 C242 C241 119.8(7) . . ? C244 C243 C242 113.0(8) . . ? C244 C243 C173 122.3(9) . . ? C242 C243 C173 120.5(7) . . ? C242 C243 C246 117.2(8) . . ? C173 C243 C246 118.1(8) . . ? C243 C244 C245 120.4(12) . . ? N240 C245 C244 118.8(11) . . ? C247 C246 C243 118.4(12) . . ? C246 C247 N240 114.4(12) . . ? C251 N250 O250 119.0(6) . . ? C251 N250 C255 120.0(6) . . ? O250 N250 C255 120.9(6) . . ? N250 C251 C252 121.3(7) . . ? C253 C252 C251 120.5(8) . . ? C252 C253 C254 116.7(7) . . ? C252 C253 C113 120.8(7) . . ? C254 C253 C113 122.4(6) . . ? C255 C254 C253 120.9(6) . . ? N250 C255 C254 120.4(6) . . ? O260 N260 C261 119.3(6) . . ? O260 N260 C265 120.6(6) . . ? C261 N260 C265 120.0(6) . . ? N260 C261 C262 120.3(6) . . ? C263 C262 C261 120.4(6) . . ? C262 C263 C264 117.2(6) . . ? C262 C263 C143 120.5(6) . . ? C264 C263 C143 122.3(6) . . ? C265 C264 C263 120.4(7) . . ? N260 C265 C264 121.7(7) . . ? O270 N270 C271 122.0(6) . . ? O270 N270 C275 119.3(7) . . ? C271 N270 C275 114.3(8) . . ? O270 N270 C277 113.9(8) . . ? C271 N270 C277 120.5(8) . . ? N270 C271 C272 121.2(7) . . ? C273 C272 C271 122.5(7) . . ? C272 C273 C274 111.4(8) . . ? C272 C273 C133 123.8(7) . . ? C274 C273 C133 120.7(8) . . ? C272 C273 C276 114.6(9) . . ? C274 C273 C276 45.4(8) . . ? C133 C273 C276 116.4(9) . . ? C275 C274 C273 119.2(11) . . ? N270 C275 C274 120.2(11) . . ? C277 C276 C273 114.4(13) . . ? C276 C277 N270 119.4(13) . . ? O280 N280 C285 120.3(6) . . ? O280 N280 C281 119.2(6) . . ? C285 N280 C281 120.5(6) . . ? N280 C281 C282 121.2(7) . . ? C281 C282 C283 120.3(6) . . ? C284 C283 C282 116.4(6) . . ? C284 C283 C123 123.6(6) . . ? C282 C283 C123 119.9(6) . . ? C285 C284 C283 122.2(7) . . ? N280 C285 C284 119.4(7) . . ? O11 Cl1 O13 108.8(3) . . ? O11 Cl1 O12 109.7(3) . . ? O13 Cl1 O12 109.6(3) . . ? O11 Cl1 O14 110.3(3) . . ? O13 Cl1 O14 109.6(3) . . ? O12 Cl1 O14 108.9(3) . . ? O23 Cl2 O22 105.3(4) . . ? O23 Cl2 O21 108.8(4) . . ? O22 Cl2 O21 109.8(4) . . ? O23 Cl2 O24 116.5(5) . . ? O22 Cl2 O24 106.0(4) . . ? O21 Cl2 O24 110.1(4) . . ? O31 Cl3 O33 117.0(10) . . ? O31 Cl3 O34 118.9(11) . . ? O33 Cl3 O34 111.6(11) . . ? O31 Cl3 O32 107.3(10) . . ? O33 Cl3 O32 99.8(9) . . ? O34 Cl3 O32 98.4(10) . . ? O34' Cl3' O33' 114.3(10) . . ? O34' Cl3' O31' 115.8(10) . . ? O33' Cl3' O31' 113.2(11) . . ? O34' Cl3' O32' 107.2(11) . . ? O33' Cl3' O32' 107.0(11) . . ? O31' Cl3' O32' 97.4(10) . . ? O41 Cl4 O44 114.6(9) . . ? O41 Cl4 O42 110.8(7) . . ? O44 Cl4 O42 108.9(9) . . ? O41 Cl4 O43 104.1(7) . . ? O44 Cl4 O43 108.6(9) . . ? O42 Cl4 O43 109.8(7) . . ? O42' Cl4' O43' 120.2(10) . . ? O42' Cl4' O41' 113.5(9) . . ? O43' Cl4' O41' 111.8(8) . . ? O42' Cl4' O44' 102.6(10) . . ? O43' Cl4' O44' 104.3(10) . . ? O41' Cl4' O44' 101.6(9) . . ? O51 Cl5 O54 111.2(12) . . ? O51 Cl5 O53 109.0(11) . . ? O54 Cl5 O53 113.8(12) . . ? O51 Cl5 O52 107.7(10) . . ? O54 Cl5 O52 108.8(12) . . ? O53 Cl5 O52 106.0(11) . . ? O51' Cl5' O54' 123.6(13) . . ? O51' Cl5' O52' 109.7(10) . . ? O54' Cl5' O52' 108.1(11) . . ? O51' Cl5' O53' 110.3(11) . . ? O54' Cl5' O53' 102.5(11) . . ? O52' Cl5' O53' 100.0(11) . . ? O64 Cl6 O62 108.2(7) . . ? O64 Cl6 O63 114.4(8) . . ? O62 Cl6 O63 110.1(7) . . ? O64 Cl6 O61 112.1(7) . . ? O62 Cl6 O61 104.5(6) . . ? O63 Cl6 O61 107.1(7) . . ? C44 O61 Cl6 117.0(12) . . ? O63' Cl6' O61' 113.1(7) . . ? O63' Cl6' O62' 110.0(8) . . ? O61' Cl6' O62' 111.3(7) . . ? O63' Cl6' O64' 112.8(9) . . ? O61' Cl6' O64' 102.6(8) . . ? O62' Cl6' O64' 106.7(8) . . ? C16 C11 C12 120.9(12) . . ? C16 C11 Cl10 122.7(11) . . ? C12 C11 Cl10 116.4(11) . . ? C11 C12 C13 114.5(11) . . ? C14 C13 C12 126.4(13) . . ? C13 C14 C15 117.1(16) . . ? C14 C15 C16 123.6(13) . . ? C11 C16 C15 117.4(11) . . ? C22 C21 C26 121.7(11) . . ? C22 C21 Cl20 116.5(10) . . ? C26 C21 Cl20 121.7(9) . . ? C21 C22 C23 115.2(10) . . ? C24 C23 C22 125.0(12) . . ? C23 C24 C25 118.2(15) . . ? C24 C25 C26 124.2(12) . . ? C21 C26 C25 115.7(10) . . ? C32 C31 C36 121.0(11) . . ? C32 C31 Cl30 121.5(10) . . ? C36 C31 Cl30 117.5(10) . . ? C31 C32 C33 117.4(10) . . ? C34 C33 C32 123.1(13) . . ? C35 C34 C33 118.1(16) . . ? C34 C35 C36 126.4(13) . . ? C31 C36 C35 113.9(10) . . ? C42 C41 C46 117.5(12) . . ? C41 C42 C43 117.5(11) . . ? C44 C43 C42 126.2(13) . . ? C45 C44 C43 114.7(15) . . ? C45 C44 O61 137.0(16) . . ? C43 C44 O61 108.0(15) . . ? C44 C45 C46 125.7(13) . . ? C41 C46 C45 118.0(11) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.47 _refine_diff_density_min -1.00 _refine_diff_density_rms 0.14