Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'William Evans' _publ_contact_author_email WEVANS@UCI.EDU _publ_section_title ; Sigma Bond Metathesis with Pentamethylcyclopentadienyl Ligands in Sterically Crowded (C5Me5)3M Complexes ; loop_ _publ_author_name 'William Evans' 'Thomas Mueller' 'Joseph W Ziller' # Attachment 'TJM29 is 3.CIF' data_tjm29 _database_code_depnum_ccdc_archive 'CCDC 765768' #TrackingRef 'TJM29 is 3.CIF' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H70 Ce2 S2' _chemical_formula_weight 1039.44 _chemical_absolute_configuration ad 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnn2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 10.3287(7) _cell_length_b 11.7979(8) _cell_length_c 19.4736(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2373.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 9884 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.28 _exptl_crystal_description polyhedron _exptl_crystal_colour purple _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 2.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5649 _exptl_absorpt_correction_T_max 0.7008 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(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 APEX II CCD' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26891 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5782 _reflns_number_gt 5498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0359P)^2^+0.7357P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(14) _refine_ls_number_reflns 5782 _refine_ls_number_parameters 264 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0584 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.029 _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 Ce1 Ce 0.5000 0.5000 0.508349(6) 0.01302(6) Uani 1 2 d S . . Ce2 Ce 0.5000 0.5000 0.247361(7) 0.01324(6) Uani 1 2 d S . . S1 S 0.39024(4) 0.40728(3) 0.37740(5) 0.01783(8) Uani 1 1 d . . . C1 C 0.2469(3) 0.50284(14) 0.55845(14) 0.0196(5) Uani 1 1 d . . . C2 C 0.24852(19) 0.59129(16) 0.50923(11) 0.0170(4) Uani 1 1 d . . . C3 C 0.32871(18) 0.67933(16) 0.53436(10) 0.0163(4) Uani 1 1 d . . . C4 C 0.37579(19) 0.64619(17) 0.60032(11) 0.0182(4) Uani 1 1 d . . . C5 C 0.32277(19) 0.53819(19) 0.61569(11) 0.0193(4) Uani 1 1 d . . . C6 C 0.1695(2) 0.39468(18) 0.55369(12) 0.0260(4) Uani 1 1 d . . . H6A H 0.2092 0.3367 0.5829 0.039 Uiso 1 1 calc R . . H6B H 0.1684 0.3683 0.5060 0.039 Uiso 1 1 calc R . . H6C H 0.0806 0.4089 0.5691 0.039 Uiso 1 1 calc R . . C7 C 0.16550(19) 0.59837(18) 0.44595(11) 0.0224(4) Uani 1 1 d . . . H7A H 0.0901 0.6464 0.4553 0.034 Uiso 1 1 calc R . . H7B H 0.1364 0.5222 0.4331 0.034 Uiso 1 1 calc R . . H7C H 0.2159 0.6311 0.4082 0.034 Uiso 1 1 calc R . . C8 C 0.3446(2) 0.79402(17) 0.50165(11) 0.0204(4) Uani 1 1 d . . . H8A H 0.3625 0.7847 0.4526 0.031 Uiso 1 1 calc R . . H8B H 0.4168 0.8341 0.5235 0.031 Uiso 1 1 calc R . . H8C H 0.2649 0.8379 0.5076 0.031 Uiso 1 1 calc R . . C9 C 0.4494(2) 0.72303(18) 0.64845(12) 0.0242(4) Uani 1 1 d . . . H9A H 0.4715 0.6814 0.6904 0.036 Uiso 1 1 calc R . . H9B H 0.3955 0.7886 0.6602 0.036 Uiso 1 1 calc R . . H9C H 0.5289 0.7491 0.6260 0.036 Uiso 1 1 calc R . . C10 C 0.3204(3) 0.4805(2) 0.68499(13) 0.0255(5) Uani 1 1 d . . . H10A H 0.4017 0.4958 0.7092 0.038 Uiso 1 1 calc R . . H10B H 0.3103 0.3986 0.6787 0.038 Uiso 1 1 calc R . . H10C H 0.2477 0.5097 0.7120 0.038 Uiso 1 1 calc R . . C11 C 0.3168(2) 0.59136(17) 0.15659(11) 0.0181(4) Uani 1 1 d . . . C12 C 0.27700(18) 0.62833(17) 0.22292(11) 0.0168(4) Uani 1 1 d . . . C13 C 0.36781(19) 0.70826(17) 0.24678(10) 0.0171(4) Uani 1 1 d . . . C14 C 0.4663(2) 0.71897(16) 0.19648(11) 0.0168(4) Uani 1 1 d . . . C15 C 0.43369(19) 0.64859(16) 0.13976(10) 0.0163(4) Uani 1 1 d . . . C16 C 0.2368(3) 0.5179(2) 0.10956(14) 0.0266(5) Uani 1 1 d . . . H16A H 0.2667 0.5274 0.0622 0.040 Uiso 1 1 calc R . . H16B H 0.1456 0.5401 0.1128 0.040 Uiso 1 1 calc R . . H16C H 0.2462 0.4383 0.1231 0.040 Uiso 1 1 calc R . . C17 C 0.15099(19) 0.5956(2) 0.25695(12) 0.0253(5) Uani 1 1 d . . . H17A H 0.1648 0.5289 0.2860 0.038 Uiso 1 1 calc R . . H17B H 0.0864 0.5779 0.2217 0.038 Uiso 1 1 calc R . . H17C H 0.1200 0.6588 0.2852 0.038 Uiso 1 1 calc R . . C18 C 0.3545(2) 0.78007(19) 0.30994(11) 0.0238(4) Uani 1 1 d . . . H18A H 0.2638 0.8026 0.3156 0.036 Uiso 1 1 calc R . . H18B H 0.4085 0.8479 0.3053 0.036 Uiso 1 1 calc R . . H18C H 0.3825 0.7366 0.3502 0.036 Uiso 1 1 calc R . . C19 C 0.5769(2) 0.80222(18) 0.19952(12) 0.0249(4) Uani 1 1 d . . . H19A H 0.6470 0.7764 0.1694 0.037 Uiso 1 1 calc R . . H19B H 0.6090 0.8074 0.2468 0.037 Uiso 1 1 calc R . . H19C H 0.5468 0.8769 0.1844 0.037 Uiso 1 1 calc R . . C20 C 0.49795(18) 0.6513(2) 0.07019(13) 0.0239(5) Uani 1 1 d . . . H20A H 0.5561 0.7168 0.0675 0.036 Uiso 1 1 calc R . . H20B H 0.4317 0.6573 0.0344 0.036 Uiso 1 1 calc R . . H20C H 0.5478 0.5815 0.0635 0.036 Uiso 1 1 calc R . . C21 C 0.29782(16) 0.28014(13) 0.37831(13) 0.0163(3) Uani 1 1 d . . . C22 C 0.3470(2) 0.1821(2) 0.40844(12) 0.0260(4) Uani 1 1 d . . . H22A H 0.4295 0.1843 0.4300 0.031 Uiso 1 1 calc R . . C23 C 0.2777(2) 0.0814(2) 0.40749(13) 0.0313(5) Uani 1 1 d . . . H23A H 0.3131 0.0153 0.4281 0.038 Uiso 1 1 calc R . . C24 C 0.1571(2) 0.07700(17) 0.37663(17) 0.0317(4) Uani 1 1 d . . . H24A H 0.1101 0.0078 0.3750 0.038 Uiso 1 1 calc R . . C25 C 0.1061(2) 0.1738(2) 0.34837(14) 0.0338(5) Uani 1 1 d . . . H25A H 0.0224 0.1716 0.3282 0.041 Uiso 1 1 calc R . . C26 C 0.1752(2) 0.27537(18) 0.34874(13) 0.0251(4) Uani 1 1 d . . . H26A H 0.1386 0.3415 0.3288 0.030 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 Ce1 0.01274(11) 0.01202(10) 0.01429(11) 0.000 0.000 0.00163(4) Ce2 0.01402(11) 0.01153(10) 0.01417(11) 0.000 0.000 -0.00011(4) S1 0.01851(18) 0.01754(18) 0.01744(18) -0.0032(2) 0.0030(2) -0.00655(16) C1 0.0183(11) 0.0162(11) 0.0242(12) 0.0000(6) 0.0069(10) 0.0012(6) C2 0.0146(9) 0.0167(9) 0.0198(9) -0.0005(7) 0.0047(7) 0.0020(7) C3 0.0167(9) 0.0150(9) 0.0172(9) -0.0020(7) 0.0036(7) 0.0035(7) C4 0.0164(9) 0.0187(10) 0.0194(10) -0.0036(7) 0.0034(7) 0.0056(7) C5 0.0212(9) 0.0197(10) 0.0171(9) 0.0002(8) 0.0041(8) 0.0053(9) C6 0.0268(11) 0.0207(10) 0.0306(11) 0.0004(8) 0.0077(9) -0.0054(8) C7 0.0175(9) 0.0264(10) 0.0233(10) -0.0007(8) -0.0013(8) 0.0031(8) C8 0.0239(10) 0.0177(9) 0.0197(10) 0.0009(7) 0.0069(8) 0.0018(8) C9 0.0253(11) 0.0223(10) 0.0250(10) -0.0046(8) -0.0020(9) 0.0059(9) C10 0.0309(13) 0.0266(10) 0.0190(11) 0.0069(9) 0.0064(10) 0.0096(10) C11 0.0186(9) 0.0169(9) 0.0188(9) 0.0008(7) -0.0022(7) 0.0000(8) C12 0.0152(9) 0.0152(8) 0.0199(9) 0.0038(8) -0.0014(8) -0.0009(7) C13 0.0177(9) 0.0159(9) 0.0176(9) 0.0002(7) -0.0018(7) 0.0030(7) C14 0.0173(8) 0.0125(9) 0.0205(10) 0.0026(7) 0.0000(8) 0.0002(8) C15 0.0178(9) 0.0140(8) 0.0171(9) 0.0019(7) 0.0002(7) 0.0005(7) C16 0.0280(12) 0.0227(10) 0.0292(12) -0.0007(9) -0.0085(11) -0.0041(9) C17 0.0157(10) 0.0369(13) 0.0232(10) 0.0074(9) 0.0004(8) -0.0012(9) C18 0.0256(10) 0.0274(10) 0.0185(9) -0.0037(8) -0.0012(8) 0.0041(8) C19 0.0229(10) 0.0235(10) 0.0282(11) 0.0055(8) -0.0008(8) -0.0067(8) C20 0.0313(14) 0.0205(12) 0.0200(12) 0.0030(10) 0.0055(7) 0.0062(7) C21 0.0183(7) 0.0164(7) 0.0142(7) -0.0006(10) 0.0011(9) -0.0038(6) C22 0.0212(10) 0.0276(11) 0.0291(10) 0.0063(9) -0.0064(9) -0.0027(8) C23 0.0334(12) 0.0231(11) 0.0374(12) 0.0090(9) 0.0007(10) -0.0018(9) C24 0.0325(10) 0.0260(10) 0.0367(10) -0.0026(12) 0.0016(14) -0.0148(8) C25 0.0232(10) 0.0364(13) 0.0418(13) 0.0018(11) -0.0089(10) -0.0138(10) C26 0.0197(10) 0.0229(10) 0.0328(10) 0.0045(9) -0.0045(9) -0.0029(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 Cnt1 2.530 . ? Ce2 Cnt2 2.530 . ? Ce1 C1 2.790(3) 2_665 ? Ce1 C1 2.790(3) . ? Ce1 C4 2.7980(19) 2_665 ? Ce1 C4 2.7980(19) . ? Ce1 C3 2.8041(18) . ? Ce1 C3 2.8041(18) 2_665 ? Ce1 C2 2.8119(19) 2_665 ? Ce1 C2 2.8120(19) . ? Ce1 C5 2.815(2) . ? Ce1 C5 2.815(2) 2_665 ? Ce1 S1 2.9975(8) . ? Ce1 S1 2.9975(8) 2_665 ? Ce2 C14 2.7886(19) 2_665 ? Ce2 C14 2.7886(19) . ? Ce2 C12 2.7971(19) 2_665 ? Ce2 C12 2.7971(19) . ? Ce2 C11 2.805(2) . ? Ce2 C11 2.805(2) 2_665 ? Ce2 C13 2.8109(19) . ? Ce2 C13 2.8109(19) 2_665 ? Ce2 C15 2.8165(19) 2_665 ? Ce2 C15 2.8165(19) . ? Ce2 S1 2.9824(8) 2_665 ? Ce2 S1 2.9824(8) . ? S1 C21 1.7780(16) . ? C1 C2 1.417(3) . ? C1 C5 1.425(3) . ? C1 C6 1.509(3) . ? C2 C3 1.416(3) . ? C2 C7 1.504(3) . ? C3 C4 1.428(3) . ? C3 C8 1.504(3) . ? C4 C5 1.419(3) . ? C4 C9 1.509(3) . ? C5 C10 1.512(3) . ? C11 C15 1.421(3) . ? C11 C12 1.424(3) . ? C11 C16 1.508(3) . ? C12 C13 1.409(3) . ? C12 C17 1.511(3) . ? C13 C14 1.418(3) . ? C13 C18 1.500(3) . ? C14 C15 1.422(3) . ? C14 C19 1.508(3) . ? C15 C20 1.509(3) . ? C21 C26 1.392(3) . ? C21 C22 1.393(3) . ? C22 C23 1.387(3) . ? C23 C24 1.384(3) . ? C24 C25 1.373(3) . ? C25 C26 1.395(3) . ? 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 Cnt1 Ce1 S1 102.5 . . ? Cnt1 Ce1 S1 120.5 2_665 . ? Cnt1 Ce1 Cnt1 129.7 2_665 . ? Cnt2 Ce2 S1 115.6 . . ? Cnt2 Ce2 S1 106.5 2_665 . ? Cnt2 Ce2 Cnt2 130.1 2_665 . ? C1 Ce1 C1 139.07(12) 2_665 . ? C1 Ce1 C4 48.64(6) 2_665 2_665 ? C1 Ce1 C4 102.30(7) . 2_665 ? C1 Ce1 C4 102.30(7) 2_665 . ? C1 Ce1 C4 48.64(6) . . ? C4 Ce1 C4 100.40(9) 2_665 . ? C1 Ce1 C3 122.47(6) 2_665 . ? C1 Ce1 C3 48.45(5) . . ? C4 Ce1 C3 129.70(6) 2_665 . ? C4 Ce1 C3 29.54(6) . . ? C1 Ce1 C3 48.45(5) 2_665 2_665 ? C1 Ce1 C3 122.47(6) . 2_665 ? C4 Ce1 C3 29.53(6) 2_665 2_665 ? C4 Ce1 C3 129.70(6) . 2_665 ? C3 Ce1 C3 159.18(8) . 2_665 ? C1 Ce1 C2 29.30(6) 2_665 2_665 ? C1 Ce1 C2 150.20(6) . 2_665 ? C4 Ce1 C2 48.43(6) 2_665 2_665 ? C4 Ce1 C2 130.97(6) . 2_665 ? C3 Ce1 C2 150.54(6) . 2_665 ? C3 Ce1 C2 29.20(6) 2_665 2_665 ? C1 Ce1 C2 150.20(6) 2_665 . ? C1 Ce1 C2 29.30(6) . . ? C4 Ce1 C2 130.98(6) 2_665 . ? C4 Ce1 C2 48.43(6) . . ? C3 Ce1 C2 29.20(6) . . ? C3 Ce1 C2 150.54(6) 2_665 . ? C2 Ce1 C2 179.30(9) 2_665 . ? C1 Ce1 C5 110.58(7) 2_665 . ? C1 Ce1 C5 29.45(7) . . ? C4 Ce1 C5 85.50(6) 2_665 . ? C4 Ce1 C5 29.28(6) . . ? C3 Ce1 C5 48.30(6) . . ? C3 Ce1 C5 113.38(6) 2_665 . ? C2 Ce1 C5 131.11(6) 2_665 . ? C2 Ce1 C5 48.20(6) . . ? C1 Ce1 C5 29.45(7) 2_665 2_665 ? C1 Ce1 C5 110.58(7) . 2_665 ? C4 Ce1 C5 29.28(6) 2_665 2_665 ? C4 Ce1 C5 85.49(6) . 2_665 ? C3 Ce1 C5 113.38(6) . 2_665 ? C3 Ce1 C5 48.30(6) 2_665 2_665 ? C2 Ce1 C5 48.20(6) 2_665 2_665 ? C2 Ce1 C5 131.10(6) . 2_665 ? C5 Ce1 C5 84.09(9) . 2_665 ? C1 Ce1 S1 130.35(5) 2_665 . ? C1 Ce1 S1 86.99(6) . . ? C4 Ce1 S1 119.54(4) 2_665 . ? C4 Ce1 S1 126.59(4) . . ? C3 Ce1 S1 100.98(4) . . ? C3 Ce1 S1 96.72(4) 2_665 . ? C2 Ce1 S1 102.40(4) 2_665 . ? C2 Ce1 S1 78.21(4) . . ? C5 Ce1 S1 116.37(4) . . ? C5 Ce1 S1 145.02(5) 2_665 . ? C1 Ce1 S1 86.99(6) 2_665 2_665 ? C1 Ce1 S1 130.35(5) . 2_665 ? C4 Ce1 S1 126.59(4) 2_665 2_665 ? C4 Ce1 S1 119.54(4) . 2_665 ? C3 Ce1 S1 96.72(4) . 2_665 ? C3 Ce1 S1 100.98(4) 2_665 2_665 ? C2 Ce1 S1 78.21(4) 2_665 2_665 ? C2 Ce1 S1 102.40(4) . 2_665 ? C5 Ce1 S1 145.02(5) . 2_665 ? C5 Ce1 S1 116.38(4) 2_665 2_665 ? S1 Ce1 S1 63.41(2) . 2_665 ? C14 Ce2 C14 138.38(9) 2_665 . ? C14 Ce2 C12 48.35(6) 2_665 2_665 ? C14 Ce2 C12 122.93(6) . 2_665 ? C14 Ce2 C12 122.94(6) 2_665 . ? C14 Ce2 C12 48.35(6) . . ? C12 Ce2 C12 160.41(9) 2_665 . ? C14 Ce2 C11 102.49(6) 2_665 . ? C14 Ce2 C11 48.39(6) . . ? C12 Ce2 C11 131.02(6) 2_665 . ? C12 Ce2 C11 29.45(6) . . ? C14 Ce2 C11 48.39(6) 2_665 2_665 ? C14 Ce2 C11 102.49(6) . 2_665 ? C12 Ce2 C11 29.46(6) 2_665 2_665 ? C12 Ce2 C11 131.02(6) . 2_665 ? C11 Ce2 C11 101.86(9) . 2_665 ? C14 Ce2 C13 150.33(6) 2_665 . ? C14 Ce2 C13 29.34(6) . . ? C12 Ce2 C13 150.74(6) 2_665 . ? C12 Ce2 C13 29.10(6) . . ? C11 Ce2 C13 48.23(6) . . ? C11 Ce2 C13 131.38(6) 2_665 . ? C14 Ce2 C13 29.34(6) 2_665 2_665 ? C14 Ce2 C13 150.33(6) . 2_665 ? C12 Ce2 C13 29.10(6) 2_665 2_665 ? C12 Ce2 C13 150.74(6) . 2_665 ? C11 Ce2 C13 131.38(6) . 2_665 ? C11 Ce2 C13 48.23(6) 2_665 2_665 ? C13 Ce2 C13 179.54(8) . 2_665 ? C14 Ce2 C15 29.40(6) 2_665 2_665 ? C14 Ce2 C15 110.03(6) . 2_665 ? C12 Ce2 C15 48.42(6) 2_665 2_665 ? C12 Ce2 C15 114.24(6) . 2_665 ? C11 Ce2 C15 86.24(6) . 2_665 ? C11 Ce2 C15 29.29(6) 2_665 2_665 ? C13 Ce2 C15 131.24(6) . 2_665 ? C13 Ce2 C15 48.31(6) 2_665 2_665 ? C14 Ce2 C15 110.04(6) 2_665 . ? C14 Ce2 C15 29.40(6) . . ? C12 Ce2 C15 114.24(6) 2_665 . ? C12 Ce2 C15 48.42(6) . . ? C11 Ce2 C15 29.29(6) . . ? C11 Ce2 C15 86.24(6) 2_665 . ? C13 Ce2 C15 48.31(6) . . ? C13 Ce2 C15 131.24(6) 2_665 . ? C15 Ce2 C15 83.86(8) 2_665 . ? C14 Ce2 S1 126.45(5) 2_665 2_665 ? C14 Ce2 S1 90.53(4) . 2_665 ? C12 Ce2 S1 91.72(4) 2_665 2_665 ? C12 Ce2 S1 105.01(4) . 2_665 ? C11 Ce2 S1 130.59(4) . 2_665 ? C11 Ce2 S1 114.81(4) 2_665 2_665 ? C13 Ce2 S1 82.38(4) . 2_665 ? C13 Ce2 S1 98.01(4) 2_665 2_665 ? C15 Ce2 S1 140.14(4) 2_665 2_665 ? C15 Ce2 S1 119.72(4) . 2_665 ? C14 Ce2 S1 90.53(4) 2_665 . ? C14 Ce2 S1 126.45(5) . . ? C12 Ce2 S1 105.01(4) 2_665 . ? C12 Ce2 S1 91.72(4) . . ? C11 Ce2 S1 114.81(4) . . ? C11 Ce2 S1 130.59(4) 2_665 . ? C13 Ce2 S1 98.01(4) . . ? C13 Ce2 S1 82.38(4) 2_665 . ? C15 Ce2 S1 119.72(4) 2_665 . ? C15 Ce2 S1 140.14(4) . . ? S1 Ce2 S1 63.77(2) 2_665 . ? C21 S1 Ce2 121.46(8) . . ? C21 S1 Ce1 120.16(8) . . ? Ce2 S1 Ce1 116.406(13) . . ? C2 C1 C5 107.89(18) . . ? C2 C1 C6 126.0(2) . . ? C5 C1 C6 125.9(2) . . ? C2 C1 Ce1 76.20(13) . . ? C5 C1 Ce1 76.23(13) . . ? C6 C1 Ce1 117.70(14) . . ? C3 C2 C1 108.26(19) . . ? C3 C2 C7 125.18(18) . . ? C1 C2 C7 126.1(2) . . ? C3 C2 Ce1 75.09(11) . . ? C1 C2 Ce1 74.50(13) . . ? C7 C2 Ce1 122.89(13) . . ? C2 C3 C4 108.01(18) . . ? C2 C3 C8 125.26(18) . . ? C4 C3 C8 126.15(18) . . ? C2 C3 Ce1 75.71(11) . . ? C4 C3 Ce1 74.99(10) . . ? C8 C3 Ce1 122.22(13) . . ? C5 C4 C3 107.71(18) . . ? C5 C4 C9 127.07(19) . . ? C3 C4 C9 124.44(19) . . ? C5 C4 Ce1 76.02(11) . . ? C3 C4 Ce1 75.47(11) . . ? C9 C4 Ce1 122.47(13) . . ? C4 C5 C1 108.06(18) . . ? C4 C5 C10 126.8(2) . . ? C1 C5 C10 123.9(2) . . ? C4 C5 Ce1 74.70(11) . . ? C1 C5 Ce1 74.32(13) . . ? C10 C5 Ce1 126.98(14) . . ? C15 C11 C12 107.99(18) . . ? C15 C11 C16 126.77(19) . . ? C12 C11 C16 124.7(2) . . ? C15 C11 Ce2 75.81(11) . . ? C12 C11 Ce2 74.98(11) . . ? C16 C11 Ce2 122.11(14) . . ? C13 C12 C11 108.17(18) . . ? C13 C12 C17 126.87(19) . . ? C11 C12 C17 124.64(18) . . ? C13 C12 Ce2 75.99(11) . . ? C11 C12 Ce2 75.57(11) . . ? C17 C12 Ce2 119.77(13) . . ? C12 C13 C14 108.04(18) . . ? C12 C13 C18 125.99(19) . . ? C14 C13 C18 125.57(19) . . ? C12 C13 Ce2 74.91(11) . . ? C14 C13 Ce2 74.46(11) . . ? C18 C13 Ce2 122.34(13) . . ? C13 C14 C15 108.32(18) . . ? C13 C14 C19 125.07(19) . . ? C15 C14 C19 126.18(19) . . ? C13 C14 Ce2 76.20(11) . . ? C15 C14 Ce2 76.39(11) . . ? C19 C14 Ce2 119.67(14) . . ? C11 C15 C14 107.43(18) . . ? C11 C15 C20 126.19(19) . . ? C14 C15 C20 125.50(19) . . ? C11 C15 Ce2 74.89(11) . . ? C14 C15 Ce2 74.22(11) . . ? C20 C15 Ce2 125.04(13) . . ? C26 C21 C22 118.21(16) . . ? C26 C21 S1 121.22(14) . . ? C22 C21 S1 120.57(15) . . ? C23 C22 C21 121.12(19) . . ? C24 C23 C22 120.2(2) . . ? C25 C24 C23 119.19(19) . . ? C24 C25 C26 121.1(2) . . ? C21 C26 C25 120.16(19) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.152 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.076 # Attachment 'TJM30 is 2b.CIF' data_tjm30 _database_code_depnum_ccdc_archive 'CCDC 765769' #TrackingRef 'TJM30 is 2b.CIF' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H109 La2 N2 Se2' _chemical_formula_weight 1570.46 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9927(9) _cell_length_b 15.3140(9) _cell_length_c 16.9117(10) _cell_angle_alpha 88.5675(7) _cell_angle_beta 88.8528(7) _cell_angle_gamma 79.9654(7) _cell_volume 3821.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9720 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 28.32 _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1606 _exptl_absorpt_coefficient_mu 2.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5357 _exptl_absorpt_correction_T_max 0.8337 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 APEX II CCD' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44479 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.50 _reflns_number_total 17502 _reflns_number_gt 15175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0291P)^2^+1.6113P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17502 _refine_ls_number_parameters 828 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.314378(7) 0.048090(7) 0.497811(6) 0.01470(3) Uani 1 1 d . . . Se1 Se 0.496960(13) -0.078959(14) 0.443058(12) 0.02033(5) Uani 1 1 d . . . N1 N 0.27818(11) -0.05940(12) 0.38924(10) 0.0217(4) Uani 1 1 d . . . C1 C 0.31252(14) 0.21813(14) 0.42403(13) 0.0250(4) Uani 1 1 d . . . C2 C 0.24310(14) 0.23386(14) 0.48263(13) 0.0250(4) Uani 1 1 d . . . C3 C 0.17056(14) 0.19349(14) 0.45837(13) 0.0234(4) Uani 1 1 d . . . C4 C 0.19592(14) 0.15008(14) 0.38680(12) 0.0226(4) Uani 1 1 d . . . C5 C 0.28372(14) 0.16567(14) 0.36477(13) 0.0244(4) Uani 1 1 d . . . C6 C 0.39614(16) 0.26069(16) 0.41939(17) 0.0377(6) Uani 1 1 d . . . H6A H 0.3815 0.3213 0.4389 0.056 Uiso 1 1 calc R . . H6B H 0.4175 0.2623 0.3643 0.056 Uiso 1 1 calc R . . H6C H 0.4437 0.2261 0.4519 0.056 Uiso 1 1 calc R . . C7 C 0.23973(18) 0.29386(17) 0.55203(16) 0.0398(6) Uani 1 1 d . . . H7A H 0.1823 0.3358 0.5521 0.060 Uiso 1 1 calc R . . H7B H 0.2903 0.3267 0.5480 0.060 Uiso 1 1 calc R . . H7C H 0.2444 0.2582 0.6012 0.060 Uiso 1 1 calc R . . C8 C 0.07379(15) 0.21559(18) 0.48784(14) 0.0352(6) Uani 1 1 d . . . H8A H 0.0399 0.2617 0.4535 0.053 Uiso 1 1 calc R . . H8B H 0.0727 0.2371 0.5420 0.053 Uiso 1 1 calc R . . H8C H 0.0459 0.1623 0.4872 0.053 Uiso 1 1 calc R . . C9 C 0.13319(16) 0.10787(16) 0.33753(14) 0.0319(5) Uani 1 1 d . . . H9A H 0.0877 0.1542 0.3136 0.048 Uiso 1 1 calc R . . H9B H 0.1029 0.0685 0.3712 0.048 Uiso 1 1 calc R . . H9C H 0.1681 0.0734 0.2957 0.048 Uiso 1 1 calc R . . C10 C 0.33110(17) 0.14094(17) 0.28750(14) 0.0361(6) Uani 1 1 d . . . H10A H 0.3130 0.1885 0.2481 0.054 Uiso 1 1 calc R . . H10B H 0.3144 0.0858 0.2693 0.054 Uiso 1 1 calc R . . H10C H 0.3968 0.1324 0.2946 0.054 Uiso 1 1 calc R . . C11 C 0.28253(13) -0.10857(13) 0.58016(12) 0.0205(4) Uani 1 1 d . . . C12 C 0.19554(13) -0.05617(13) 0.56894(12) 0.0198(4) Uani 1 1 d . . . C13 C 0.18817(13) 0.01883(14) 0.61735(12) 0.0206(4) Uani 1 1 d . . . C14 C 0.27081(14) 0.01367(14) 0.65790(11) 0.0207(4) Uani 1 1 d . . . C15 C 0.32851(13) -0.06527(14) 0.63563(12) 0.0208(4) Uani 1 1 d . . . C16 C 0.31822(16) -0.19764(14) 0.54543(14) 0.0301(5) Uani 1 1 d . . . H16A H 0.3312 -0.2422 0.5882 0.045 Uiso 1 1 calc R . . H16B H 0.3739 -0.1945 0.5150 0.045 Uiso 1 1 calc R . . H16C H 0.2728 -0.2142 0.5105 0.045 Uiso 1 1 calc R . . C17 C 0.11906(15) -0.08032(17) 0.52283(13) 0.0309(5) Uani 1 1 d . . . H17A H 0.0683 -0.0860 0.5589 0.046 Uiso 1 1 calc R . . H17B H 0.1396 -0.1369 0.4967 0.046 Uiso 1 1 calc R . . H17C H 0.0994 -0.0339 0.4829 0.046 Uiso 1 1 calc R . . C18 C 0.10190(15) 0.08012(16) 0.63824(14) 0.0317(5) Uani 1 1 d . . . H18A H 0.0790 0.0620 0.6897 0.048 Uiso 1 1 calc R . . H18B H 0.0567 0.0774 0.5977 0.048 Uiso 1 1 calc R . . H18C H 0.1137 0.1409 0.6410 0.048 Uiso 1 1 calc R . . C19 C 0.28666(16) 0.07534(17) 0.72208(13) 0.0329(5) Uani 1 1 d . . . H19A H 0.2550 0.0611 0.7707 0.049 Uiso 1 1 calc R . . H19B H 0.2636 0.1367 0.7054 0.049 Uiso 1 1 calc R . . H19C H 0.3517 0.0684 0.7320 0.049 Uiso 1 1 calc R . . C20 C 0.41938(15) -0.10180(16) 0.67011(14) 0.0310(5) Uani 1 1 d . . . H20A H 0.4213 -0.1640 0.6862 0.047 Uiso 1 1 calc R . . H20B H 0.4291 -0.0675 0.7163 0.047 Uiso 1 1 calc R . . H20C H 0.4670 -0.0977 0.6303 0.047 Uiso 1 1 calc R . . C21 C 0.26035(13) -0.10969(14) 0.34640(12) 0.0227(4) Uani 1 1 d . . . C22 C 0.23242(15) -0.17298(16) 0.29121(14) 0.0290(5) Uani 1 1 d . . . C23 C 0.29932(18) -0.26094(16) 0.29680(16) 0.0386(6) Uani 1 1 d . . . H23A H 0.3007 -0.2839 0.3515 0.058 Uiso 1 1 calc R . . H23B H 0.3600 -0.2511 0.2806 0.058 Uiso 1 1 calc R . . H23C H 0.2801 -0.3040 0.2619 0.058 Uiso 1 1 calc R . . C24 C 0.13740(17) -0.1880(2) 0.31684(18) 0.0487(8) Uani 1 1 d . . . H24A H 0.0956 -0.1312 0.3160 0.073 Uiso 1 1 calc R . . H24B H 0.1395 -0.2138 0.3705 0.073 Uiso 1 1 calc R . . H24C H 0.1165 -0.2286 0.2804 0.073 Uiso 1 1 calc R . . C25 C 0.23213(19) -0.13334(18) 0.20756(14) 0.0417(6) Uani 1 1 d . . . H25A H 0.1912 -0.0760 0.2058 0.063 Uiso 1 1 calc R . . H25B H 0.2114 -0.1737 0.1707 0.063 Uiso 1 1 calc R . . H25C H 0.2936 -0.1249 0.1925 0.063 Uiso 1 1 calc R . . C26 C 0.50449(13) -0.14090(14) 0.34521(12) 0.0215(4) Uani 1 1 d . . . C27 C 0.47333(15) -0.09851(15) 0.27486(13) 0.0272(5) Uani 1 1 d . . . H27A H 0.4439 -0.0383 0.2752 0.033 Uiso 1 1 calc R . . C28 C 0.48501(16) -0.14388(18) 0.20374(14) 0.0343(6) Uani 1 1 d . . . H28A H 0.4638 -0.1142 0.1559 0.041 Uiso 1 1 calc R . . C29 C 0.52700(16) -0.23107(19) 0.20247(15) 0.0388(6) Uani 1 1 d . . . H29A H 0.5350 -0.2617 0.1540 0.047 Uiso 1 1 calc R . . C30 C 0.55748(17) -0.27387(18) 0.27205(16) 0.0421(6) Uani 1 1 d . . . H30A H 0.5867 -0.3341 0.2713 0.051 Uiso 1 1 calc R . . C31 C 0.54584(15) -0.22959(15) 0.34311(14) 0.0312(5) Uani 1 1 d . . . H31A H 0.5663 -0.2601 0.3908 0.037 Uiso 1 1 calc R . . La2 La 0.974795(7) 0.679769(7) 0.012498(6) 0.01574(3) Uani 1 1 d . . . Se2 Se 0.951641(15) 0.492983(13) 0.084645(12) 0.02156(5) Uani 1 1 d . . . N2 N 1.06612(13) 0.72408(12) -0.11091(10) 0.0248(4) Uani 1 1 d . . . C32 C 1.09609(14) 0.67146(13) 0.14272(12) 0.0214(4) Uani 1 1 d . . . C33 C 1.02016(14) 0.73738(14) 0.16063(12) 0.0220(4) Uani 1 1 d . . . C34 C 1.02416(15) 0.81250(13) 0.11075(12) 0.0237(4) Uani 1 1 d . . . C35 C 1.09981(15) 0.79134(14) 0.05927(12) 0.0235(4) Uani 1 1 d . . . C36 C 1.14490(14) 0.70434(14) 0.07894(12) 0.0224(4) Uani 1 1 d . . . C37 C 1.12671(16) 0.58915(14) 0.19211(13) 0.0271(5) Uani 1 1 d . . . H37A H 1.1143 0.6022 0.2481 0.041 Uiso 1 1 calc R . . H37B H 1.1919 0.5692 0.1838 0.041 Uiso 1 1 calc R . . H37C H 1.0939 0.5424 0.1766 0.041 Uiso 1 1 calc R . . C38 C 0.95078(15) 0.72928(15) 0.22495(13) 0.0281(5) Uani 1 1 d . . . H38A H 0.9802 0.7240 0.2765 0.042 Uiso 1 1 calc R . . H38B H 0.9238 0.6765 0.2164 0.042 Uiso 1 1 calc R . . H38C H 0.9033 0.7821 0.2237 0.042 Uiso 1 1 calc R . . C39 C 0.97484(17) 0.90576(14) 0.12199(15) 0.0341(5) Uani 1 1 d . . . H39A H 1.0134 0.9394 0.1505 0.051 Uiso 1 1 calc R . . H39B H 0.9188 0.9044 0.1525 0.051 Uiso 1 1 calc R . . H39C H 0.9601 0.9342 0.0702 0.051 Uiso 1 1 calc R . . C40 C 1.13537(17) 0.85729(15) 0.00484(14) 0.0322(5) Uani 1 1 d . . . H40A H 1.1599 0.9002 0.0363 0.048 Uiso 1 1 calc R . . H40B H 1.0860 0.8885 -0.0278 0.048 Uiso 1 1 calc R . . H40C H 1.1834 0.8260 -0.0294 0.048 Uiso 1 1 calc R . . C41 C 1.23302(15) 0.65924(16) 0.04308(14) 0.0305(5) Uani 1 1 d . . . H41A H 1.2811 0.6925 0.0553 0.046 Uiso 1 1 calc R . . H41B H 1.2271 0.6571 -0.0144 0.046 Uiso 1 1 calc R . . H41C H 1.2483 0.5987 0.0650 0.046 Uiso 1 1 calc R . . C42 C 0.80169(14) 0.67027(14) -0.04727(13) 0.0244(4) Uani 1 1 d . . . C43 C 0.84220(14) 0.71997(14) -0.10524(13) 0.0247(4) Uani 1 1 d . . . C44 C 0.84827(14) 0.80347(14) -0.07278(12) 0.0237(4) Uani 1 1 d . . . C45 C 0.81109(14) 0.80485(14) 0.00445(13) 0.0250(5) Uani 1 1 d . . . C46 C 0.78395(14) 0.72279(14) 0.02110(13) 0.0250(4) Uani 1 1 d . . . C47 C 0.77309(16) 0.58212(15) -0.05957(15) 0.0342(5) Uani 1 1 d . . . H47A H 0.7362 0.5857 -0.1071 0.051 Uiso 1 1 calc R . . H47B H 0.7375 0.5671 -0.0136 0.051 Uiso 1 1 calc R . . H47C H 0.8270 0.5362 -0.0660 0.051 Uiso 1 1 calc R . . C48 C 0.86753(16) 0.69057(16) -0.18844(13) 0.0312(5) Uani 1 1 d . . . H48A H 0.8126 0.6951 -0.2198 0.047 Uiso 1 1 calc R . . H48B H 0.8992 0.6289 -0.1871 0.047 Uiso 1 1 calc R . . H48C H 0.9073 0.7286 -0.2125 0.047 Uiso 1 1 calc R . . C49 C 0.87803(18) 0.88119(15) -0.11548(14) 0.0346(5) Uani 1 1 d . . . H49A H 0.8246 0.9232 -0.1327 0.052 Uiso 1 1 calc R . . H49B H 0.9154 0.8603 -0.1617 0.052 Uiso 1 1 calc R . . H49C H 0.9134 0.9107 -0.0798 0.052 Uiso 1 1 calc R . . C50 C 0.77963(17) 0.88683(16) 0.05207(15) 0.0369(6) Uani 1 1 d . . . H50A H 0.7151 0.9083 0.0429 0.055 Uiso 1 1 calc R . . H50B H 0.8144 0.9330 0.0358 0.055 Uiso 1 1 calc R . . H50C H 0.7889 0.8725 0.1084 0.055 Uiso 1 1 calc R . . C51 C 0.73567(17) 0.69994(17) 0.09581(15) 0.0372(6) Uani 1 1 d . . . H51A H 0.6974 0.7535 0.1159 0.056 Uiso 1 1 calc R . . H51B H 0.7804 0.6756 0.1356 0.056 Uiso 1 1 calc R . . H51C H 0.6978 0.6558 0.0844 0.056 Uiso 1 1 calc R . . C52 C 1.10705(15) 0.74876(14) -0.16176(13) 0.0240(4) Uani 1 1 d . . . C53 C 1.15709(15) 0.78493(15) -0.22761(13) 0.0276(5) Uani 1 1 d . . . C54 C 1.13365(17) 0.74421(17) -0.30462(13) 0.0347(5) Uani 1 1 d . . . H54A H 1.1526 0.6797 -0.3015 0.052 Uiso 1 1 calc R . . H54B H 1.1652 0.7685 -0.3491 0.052 Uiso 1 1 calc R . . H54C H 1.0681 0.7584 -0.3126 0.052 Uiso 1 1 calc R . . C55 C 1.25896(17) 0.76140(18) -0.21187(16) 0.0382(6) Uani 1 1 d . . . H55A H 1.2768 0.6968 -0.2076 0.057 Uiso 1 1 calc R . . H55B H 1.2724 0.7881 -0.1624 0.057 Uiso 1 1 calc R . . H55C H 1.2928 0.7843 -0.2556 0.057 Uiso 1 1 calc R . . C56 C 1.12678(19) 0.88586(16) -0.22997(16) 0.0404(6) Uani 1 1 d . . . H56A H 1.1400 0.9102 -0.1793 0.061 Uiso 1 1 calc R . . H56B H 1.0615 0.9000 -0.2394 0.061 Uiso 1 1 calc R . . H56C H 1.1595 0.9119 -0.2727 0.061 Uiso 1 1 calc R . . C57 C 0.87324(14) 0.49030(13) 0.17596(12) 0.0217(4) Uani 1 1 d . . . C58 C 0.78291(15) 0.48136(14) 0.16900(13) 0.0274(5) Uani 1 1 d . . . H58A H 0.7600 0.4715 0.1186 0.033 Uiso 1 1 calc R . . C59 C 0.72570(16) 0.48673(15) 0.23547(15) 0.0332(5) Uani 1 1 d . . . H59A H 0.6640 0.4814 0.2299 0.040 Uiso 1 1 calc R . . C60 C 0.75819(17) 0.49975(16) 0.30919(14) 0.0351(6) Uani 1 1 d . . . H60A H 0.7189 0.5041 0.3542 0.042 Uiso 1 1 calc R . . C61 C 0.84821(18) 0.50647(16) 0.31719(14) 0.0346(5) Uani 1 1 d . . . H61A H 0.8711 0.5147 0.3679 0.042 Uiso 1 1 calc R . . C62 C 0.90550(16) 0.50117(15) 0.25091(13) 0.0269(5) Uani 1 1 d . . . H62A H 0.9675 0.5051 0.2571 0.032 Uiso 1 1 calc R . . C63 C 0.5434(2) -0.0890(2) -0.10056(19) 0.0577(8) Uani 1 1 d . . . H63A H 0.5785 -0.0537 -0.1306 0.069 Uiso 1 1 calc R . . C64 C 0.5834(2) -0.1701(2) -0.07154(16) 0.0475(7) Uani 1 1 d . . . H64A H 0.6458 -0.1917 -0.0820 0.057 Uiso 1 1 calc R . . C65 C 0.5328(2) -0.2197(2) -0.02746(19) 0.0582(8) Uani 1 1 d . . . H65A H 0.5603 -0.2761 -0.0069 0.070 Uiso 1 1 calc R . . C66 C 0.4422(2) -0.1890(2) -0.0123(2) 0.0599(9) Uani 1 1 d . . . H66A H 0.4075 -0.2239 0.0187 0.072 Uiso 1 1 calc R . . C67 C 0.4025(2) -0.1078(2) -0.0422(2) 0.0612(9) Uani 1 1 d . . . H67A H 0.3401 -0.0863 -0.0321 0.073 Uiso 1 1 calc R . . C68 C 0.4531(2) -0.0578(2) -0.0868(2) 0.0685(10) Uani 1 1 d . . . H68A H 0.4257 -0.0018 -0.1082 0.082 Uiso 1 1 calc R . . C69 C 0.8928(2) 0.5209(2) 0.6026(2) 0.0655(10) Uani 1 1 d . . . H69A H 0.9332 0.5547 0.6245 0.079 Uiso 1 1 calc R . . C70 C 0.7997(2) 0.5485(2) 0.6100(2) 0.0643(9) Uani 1 1 d . . . H70A H 0.7760 0.6011 0.6374 0.077 Uiso 1 1 calc R . . C71 C 0.7426(2) 0.4990(2) 0.5774(2) 0.0594(9) Uani 1 1 d . . . H71A H 0.6789 0.5168 0.5829 0.071 Uiso 1 1 calc R . . C72 C 0.7768(2) 0.4242(2) 0.5371(2) 0.0572(8) Uani 1 1 d . . . H72A H 0.7368 0.3915 0.5130 0.069 Uiso 1 1 calc R . . C73 C 0.8682(2) 0.3959(2) 0.5310(2) 0.0633(9) Uani 1 1 d . . . H73A H 0.8915 0.3427 0.5043 0.076 Uiso 1 1 calc R . . C74 C 0.9259(2) 0.4442(3) 0.5634(2) 0.0666(10) Uani 1 1 d . . . H74A H 0.9895 0.4248 0.5588 0.080 Uiso 1 1 calc R . . C75 C 0.5127(3) -0.4864(4) 0.1094(3) 0.0920(14) Uani 1 1 d . . . H75A H 0.5368 -0.4507 0.0706 0.110 Uiso 1 1 calc R . . C76 C 0.5411(3) -0.5793(4) 0.1123(3) 0.0943(16) Uani 1 1 d . . . H76 H 0.5844 -0.6083 0.0755 0.113 Uiso 1 1 calc R . . C77 C 0.5032(3) -0.6262(3) 0.1707(3) 0.0888(14) Uani 1 1 d . . . H77A H 0.5212 -0.6887 0.1749 0.107 Uiso 1 1 calc R . . C78 C 0.4401(4) -0.5842(3) 0.2227(3) 0.0995(15) Uani 1 1 d . . . H78A H 0.4145 -0.6180 0.2622 0.119 Uiso 1 1 calc R . . C79 C 0.4140(3) -0.4963(3) 0.2188(3) 0.0906(14) Uani 1 1 d . . . H79A H 0.3699 -0.4683 0.2553 0.109 Uiso 1 1 calc R . . C80 C 0.4487(3) -0.4483(3) 0.1649(3) 0.0801(13) Uani 1 1 d . . . H80A H 0.4296 -0.3858 0.1637 0.096 Uiso 1 1 calc R . . C81 C 0.5078(2) 0.5330(2) 0.4243(2) 0.0531(8) Uani 1 1 d . . . H81 H 0.5131 0.5559 0.3720 0.064 Uiso 1 1 calc R . . C82 C 0.53450(19) 0.4439(2) 0.4402(2) 0.0538(8) Uani 1 1 d . . . H82 H 0.5584 0.4053 0.3990 0.065 Uiso 1 1 calc R . . C83 C 0.52660(19) 0.41073(19) 0.5155(2) 0.0517(8) Uani 1 1 d . . . H83 H 0.5448 0.3491 0.5263 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01194(5) 0.01701(6) 0.01541(6) -0.00160(4) 0.00095(4) -0.00321(4) Se1 0.01374(9) 0.02597(11) 0.02185(10) -0.00715(8) 0.00118(7) -0.00425(8) N1 0.0178(8) 0.0250(9) 0.0227(9) -0.0036(7) -0.0020(7) -0.0041(7) C1 0.0208(10) 0.0180(10) 0.0351(12) 0.0068(9) -0.0022(9) -0.0012(8) C2 0.0227(11) 0.0189(10) 0.0316(12) -0.0007(9) -0.0038(9) 0.0016(8) C3 0.0193(10) 0.0232(11) 0.0262(11) 0.0033(8) -0.0001(8) 0.0002(8) C4 0.0192(10) 0.0215(10) 0.0260(11) 0.0041(8) -0.0042(8) -0.0010(8) C5 0.0216(11) 0.0234(11) 0.0258(11) 0.0073(8) 0.0005(8) 0.0015(8) C6 0.0256(12) 0.0282(12) 0.0600(17) 0.0117(11) -0.0024(11) -0.0086(10) C7 0.0401(15) 0.0310(13) 0.0472(15) -0.0127(11) -0.0090(12) -0.0003(11) C8 0.0211(11) 0.0462(15) 0.0335(13) 0.0063(11) 0.0003(10) 0.0065(10) C9 0.0284(12) 0.0342(13) 0.0321(12) 0.0014(10) -0.0110(10) -0.0022(10) C10 0.0325(13) 0.0411(14) 0.0286(12) 0.0101(10) 0.0059(10) 0.0082(11) C11 0.0189(10) 0.0209(10) 0.0219(10) 0.0021(8) 0.0056(8) -0.0051(8) C12 0.0162(10) 0.0244(10) 0.0201(10) 0.0019(8) 0.0027(8) -0.0075(8) C13 0.0180(10) 0.0236(10) 0.0195(10) 0.0018(8) 0.0066(8) -0.0031(8) C14 0.0216(10) 0.0247(11) 0.0169(10) 0.0006(8) 0.0037(8) -0.0077(8) C15 0.0151(9) 0.0278(11) 0.0191(10) 0.0042(8) 0.0035(8) -0.0035(8) C16 0.0329(12) 0.0213(11) 0.0358(13) -0.0016(9) 0.0106(10) -0.0048(9) C17 0.0225(11) 0.0447(14) 0.0286(12) -0.0013(10) 0.0004(9) -0.0148(10) C18 0.0264(12) 0.0324(13) 0.0327(12) 0.0033(10) 0.0106(10) 0.0033(10) C19 0.0335(13) 0.0431(14) 0.0255(12) -0.0098(10) 0.0074(10) -0.0161(11) C20 0.0205(11) 0.0406(14) 0.0311(12) 0.0102(10) -0.0011(9) -0.0043(10) C21 0.0163(10) 0.0266(11) 0.0241(11) -0.0015(9) -0.0001(8) -0.0009(8) C22 0.0230(11) 0.0342(13) 0.0320(12) -0.0137(10) -0.0006(9) -0.0092(9) C23 0.0406(14) 0.0297(13) 0.0465(15) -0.0123(11) 0.0032(12) -0.0081(11) C24 0.0287(13) 0.0643(19) 0.0590(18) -0.0348(15) 0.0078(12) -0.0209(13) C25 0.0462(16) 0.0495(16) 0.0304(13) -0.0117(12) -0.0122(11) -0.0077(13) C26 0.0145(9) 0.0277(11) 0.0238(10) -0.0075(8) 0.0033(8) -0.0070(8) C27 0.0249(11) 0.0300(12) 0.0285(12) -0.0027(9) 0.0001(9) -0.0092(9) C28 0.0327(13) 0.0515(16) 0.0229(11) -0.0046(10) 0.0035(10) -0.0188(11) C29 0.0270(12) 0.0572(17) 0.0349(14) -0.0246(12) 0.0104(10) -0.0126(12) C30 0.0340(14) 0.0391(15) 0.0514(16) -0.0233(12) 0.0018(12) 0.0015(11) C31 0.0272(12) 0.0306(12) 0.0345(13) -0.0072(10) -0.0016(10) -0.0005(9) La2 0.01861(6) 0.01307(6) 0.01569(6) -0.00035(4) 0.00158(4) -0.00334(4) Se2 0.02917(11) 0.01557(10) 0.02003(10) -0.00079(7) 0.00738(8) -0.00497(8) N2 0.0315(10) 0.0210(9) 0.0231(9) -0.0001(7) 0.0029(8) -0.0080(8) C32 0.0255(11) 0.0206(10) 0.0196(10) -0.0027(8) -0.0025(8) -0.0075(8) C33 0.0281(11) 0.0207(10) 0.0188(10) -0.0048(8) -0.0007(8) -0.0081(8) C34 0.0303(11) 0.0169(10) 0.0249(11) -0.0040(8) -0.0037(9) -0.0062(8) C35 0.0315(12) 0.0202(10) 0.0215(10) -0.0001(8) -0.0039(9) -0.0116(9) C36 0.0244(11) 0.0212(10) 0.0233(10) -0.0036(8) -0.0022(8) -0.0079(8) C37 0.0331(12) 0.0228(11) 0.0262(11) 0.0016(9) -0.0042(9) -0.0068(9) C38 0.0326(12) 0.0268(12) 0.0257(11) -0.0054(9) 0.0041(9) -0.0068(9) C39 0.0419(14) 0.0191(11) 0.0412(14) -0.0069(10) -0.0051(11) -0.0032(10) C40 0.0446(14) 0.0259(12) 0.0306(12) 0.0017(9) -0.0018(10) -0.0192(10) C41 0.0277(12) 0.0309(12) 0.0343(13) -0.0015(10) 0.0032(10) -0.0093(10) C42 0.0172(10) 0.0225(11) 0.0316(12) -0.0030(9) -0.0025(8) 0.0025(8) C43 0.0226(11) 0.0243(11) 0.0250(11) -0.0015(9) -0.0054(8) 0.0026(8) C44 0.0253(11) 0.0202(10) 0.0240(11) 0.0017(8) -0.0042(8) 0.0008(8) C45 0.0238(11) 0.0218(11) 0.0268(11) -0.0035(8) -0.0010(9) 0.0034(8) C46 0.0183(10) 0.0256(11) 0.0294(11) 0.0001(9) 0.0016(8) 0.0005(8) C47 0.0284(12) 0.0291(12) 0.0460(15) -0.0037(11) -0.0070(10) -0.0067(10) C48 0.0364(13) 0.0317(12) 0.0233(11) -0.0034(9) -0.0054(10) 0.0008(10) C49 0.0441(15) 0.0235(12) 0.0340(13) 0.0069(10) -0.0032(11) -0.0007(10) C50 0.0350(13) 0.0325(13) 0.0400(14) -0.0126(11) 0.0000(11) 0.0047(10) C51 0.0281(13) 0.0424(15) 0.0388(14) 0.0018(11) 0.0101(10) -0.0008(11) C52 0.0277(11) 0.0182(10) 0.0259(11) 0.0001(8) 0.0017(9) -0.0041(8) C53 0.0311(12) 0.0255(11) 0.0262(11) 0.0048(9) 0.0098(9) -0.0064(9) C54 0.0397(14) 0.0384(14) 0.0253(12) 0.0035(10) 0.0073(10) -0.0062(11) C55 0.0343(14) 0.0407(14) 0.0413(14) 0.0039(11) 0.0081(11) -0.0133(11) C56 0.0555(17) 0.0236(12) 0.0409(14) 0.0079(10) 0.0177(12) -0.0070(11) C57 0.0279(11) 0.0160(10) 0.0207(10) 0.0011(8) 0.0060(8) -0.0032(8) C58 0.0280(12) 0.0263(11) 0.0284(12) 0.0014(9) 0.0004(9) -0.0061(9) C59 0.0238(12) 0.0301(12) 0.0454(14) 0.0017(10) 0.0084(10) -0.0057(9) C60 0.0387(14) 0.0322(13) 0.0333(13) -0.0040(10) 0.0181(11) -0.0050(11) C61 0.0460(15) 0.0373(13) 0.0225(11) -0.0054(10) 0.0062(10) -0.0127(11) C62 0.0291(12) 0.0283(12) 0.0249(11) -0.0014(9) 0.0027(9) -0.0100(9) C63 0.0515(19) 0.061(2) 0.0539(19) 0.0091(15) 0.0161(15) 0.0052(15) C64 0.0402(15) 0.0563(18) 0.0403(15) -0.0046(13) -0.0066(12) 0.0086(13) C65 0.066(2) 0.0464(18) 0.059(2) 0.0052(15) -0.0141(17) -0.0020(16) C66 0.070(2) 0.059(2) 0.057(2) -0.0024(16) 0.0032(17) -0.0296(18) C67 0.0405(17) 0.068(2) 0.074(2) -0.0112(18) 0.0082(16) -0.0041(16) C68 0.055(2) 0.060(2) 0.079(2) 0.0171(18) 0.0163(18) 0.0176(17) C69 0.063(2) 0.069(2) 0.067(2) 0.0328(19) -0.0294(18) -0.0207(18) C70 0.070(2) 0.0441(18) 0.073(2) 0.0097(16) -0.0105(18) 0.0060(16) C71 0.0399(17) 0.0446(18) 0.090(3) 0.0144(17) 0.0034(16) 0.0008(14) C72 0.0450(17) 0.0476(18) 0.077(2) 0.0152(16) 0.0022(16) -0.0061(14) C73 0.0490(19) 0.068(2) 0.069(2) 0.0022(18) 0.0140(17) -0.0010(17) C74 0.0383(17) 0.084(3) 0.073(2) 0.017(2) 0.0056(16) -0.0004(17) C75 0.093(3) 0.106(4) 0.087(3) 0.005(3) -0.033(3) -0.044(3) C76 0.062(3) 0.129(4) 0.088(3) -0.049(3) -0.018(2) 0.001(3) C77 0.097(3) 0.059(2) 0.105(4) -0.018(2) -0.047(3) 0.011(2) C78 0.126(4) 0.097(4) 0.071(3) 0.012(3) -0.026(3) -0.008(3) C79 0.107(4) 0.086(3) 0.074(3) -0.016(3) -0.024(3) 0.002(3) C80 0.083(3) 0.058(2) 0.096(3) -0.015(2) -0.042(3) 0.002(2) C81 0.0448(17) 0.0511(18) 0.065(2) -0.0030(15) -0.0024(15) -0.0131(14) C82 0.0384(16) 0.0486(18) 0.076(2) -0.0204(16) 0.0042(15) -0.0097(13) C83 0.0336(15) 0.0354(15) 0.087(2) -0.0086(15) -0.0046(15) -0.0053(12) _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 Cnt1 2.596 . ? La1 Cnt2 2.569 . ? La2 Cnt3 2.597 . ? La2 Cnt4 2.560 . ? La1 N1 2.6226(17) . ? La1 C13 2.8222(19) . ? La1 C12 2.8250(19) . ? La1 C14 2.8306(19) . ? La1 C5 2.840(2) . ? La1 C11 2.851(2) . ? La1 C4 2.853(2) . ? La1 C1 2.855(2) . ? La1 C15 2.860(2) . ? La1 C2 2.866(2) . ? La1 C3 2.892(2) . ? La1 Se1 3.1347(3) 2_656 ? La1 Se1 3.2045(3) . ? Se1 C26 1.920(2) . ? Se1 La1 3.1348(3) 2_656 ? N1 C21 1.139(3) . ? C1 C2 1.417(3) . ? C1 C5 1.420(3) . ? C1 C6 1.510(3) . ? C2 C3 1.414(3) . ? C2 C7 1.503(3) . ? C3 C4 1.409(3) . ? C3 C8 1.509(3) . ? C4 C5 1.419(3) . ? C4 C9 1.506(3) . ? C5 C10 1.500(3) . ? C11 C15 1.418(3) . ? C11 C12 1.421(3) . ? C11 C16 1.505(3) . ? C12 C13 1.414(3) . ? C12 C17 1.503(3) . ? C13 C14 1.417(3) . ? C13 C18 1.501(3) . ? C14 C15 1.413(3) . ? C14 C19 1.505(3) . ? C15 C20 1.503(3) . ? C21 C22 1.479(3) . ? C22 C25 1.525(3) . ? C22 C24 1.534(3) . ? C22 C23 1.535(3) . ? C26 C27 1.390(3) . ? C26 C31 1.392(3) . ? C27 C28 1.397(3) . ? C28 C29 1.374(4) . ? C29 C30 1.379(4) . ? C30 C31 1.388(3) . ? La2 N2 2.6133(18) . ? La2 C33 2.8115(19) . ? La2 C43 2.823(2) . ? La2 C46 2.824(2) . ? La2 C44 2.826(2) . ? La2 C42 2.832(2) . ? La2 C45 2.841(2) . ? La2 C34 2.861(2) . ? La2 C32 2.870(2) . ? La2 C35 2.881(2) . ? La2 C36 2.895(2) . ? La2 Se2 3.1537(3) . ? La2 Se2 3.1689(3) 2_765 ? Se2 C57 1.926(2) . ? Se2 La2 3.1689(3) 2_765 ? N2 C52 1.141(3) . ? C32 C33 1.417(3) . ? C32 C36 1.422(3) . ? C32 C37 1.503(3) . ? C33 C34 1.418(3) . ? C33 C38 1.508(3) . ? C34 C35 1.413(3) . ? C34 C39 1.504(3) . ? C35 C36 1.420(3) . ? C35 C40 1.508(3) . ? C36 C41 1.504(3) . ? C42 C43 1.417(3) . ? C42 C46 1.419(3) . ? C42 C47 1.506(3) . ? C43 C44 1.422(3) . ? C43 C48 1.509(3) . ? C44 C45 1.409(3) . ? C44 C49 1.505(3) . ? C45 C46 1.407(3) . ? C45 C50 1.509(3) . ? C46 C51 1.507(3) . ? C52 C53 1.480(3) . ? C53 C54 1.531(3) . ? C53 C56 1.533(3) . ? C53 C55 1.534(3) . ? C57 C62 1.390(3) . ? C57 C58 1.392(3) . ? C58 C59 1.396(3) . ? C59 C60 1.379(4) . ? C60 C61 1.381(4) . ? C61 C62 1.394(3) . ? C63 C64 1.366(4) . ? C63 C68 1.373(4) . ? C64 C65 1.363(4) . ? C65 C66 1.380(5) . ? C66 C67 1.370(5) . ? C67 C68 1.372(5) . ? C69 C74 1.374(5) . ? C69 C70 1.390(5) . ? C70 C71 1.371(5) . ? C71 C72 1.364(4) . ? C72 C73 1.365(4) . ? C73 C74 1.363(5) . ? C75 C80 1.391(6) . ? C75 C76 1.413(6) . ? C76 C77 1.378(7) . ? C77 C78 1.364(6) . ? C78 C79 1.335(6) . ? C79 C80 1.313(6) . ? C81 C82 1.375(4) . ? C81 C83 1.384(4) 2_666 ? C82 C83 1.369(5) . ? C83 C81 1.384(4) 2_666 ? 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 Cnt1 La1 Se1 124.8 . . ? Cnt1 La1 Se1 107.0 . 2_656 ? Cnt1 La1 N1 95.2 . . ? Cnt2 La1 Se1 103.8 . . ? Cnt2 La1 Se1 104.1 . 2_656 ? Cnt2 La1 N1 93.9 . . ? Cnt1 La1 Cnt2 130.7 . . ? Cnt3 La2 Se2 105.5 . . ? Cnt3 La2 Se2 121.4 . 2_765 ? Cnt3 La2 N2 92.7 . . ? Cnt4 La2 Se1 103.8 . . ? Cnt4 La2 Se1 107.2 . 2_765 ? Cnt4 La2 N2 96.4 . . ? Cnt3 La2 Cnt4 130.8 . . ? N1 La1 C13 100.72(6) . . ? N1 La1 C12 73.34(6) . . ? C13 La1 C12 29.01(6) . . ? N1 La1 C14 119.05(6) . . ? C13 La1 C14 29.04(6) . . ? C12 La1 C14 47.80(6) . . ? N1 La1 C5 78.93(6) . . ? C13 La1 C5 127.33(6) . . ? C12 La1 C5 128.37(6) . . ? C14 La1 C5 147.07(6) . . ? N1 La1 C11 73.93(6) . . ? C13 La1 C11 47.72(6) . . ? C12 La1 C11 28.98(6) . . ? C14 La1 C11 47.63(6) . . ? C5 La1 C11 149.61(6) . . ? N1 La1 C4 72.15(6) . . ? C13 La1 C4 100.10(6) . . ? C12 La1 C4 100.24(6) . . ? C14 La1 C4 125.61(6) . . ? C5 La1 C4 28.87(6) . . ? C11 La1 C4 125.87(6) . . ? N1 La1 C1 107.67(6) . . ? C13 La1 C1 122.26(6) . . ? C12 La1 C1 140.66(6) . . ? C14 La1 C1 126.60(6) . . ? C5 La1 C1 28.86(6) . . ? C11 La1 C1 169.34(6) . . ? C4 La1 C1 47.34(6) . . ? N1 La1 C15 101.40(6) . . ? C13 La1 C15 47.52(6) . . ? C12 La1 C15 47.54(6) . . ? C14 La1 C15 28.75(6) . . ? C5 La1 C15 174.85(6) . . ? C11 La1 C15 28.76(6) . . ? C4 La1 C15 146.28(6) . . ? C1 La1 C15 150.83(6) . . ? N1 La1 C2 119.24(6) . . ? C13 La1 C2 93.63(6) . . ? C12 La1 C2 115.25(6) . . ? C14 La1 C2 101.23(6) . . ? C5 La1 C2 47.43(6) . . ? C11 La1 C2 141.27(6) . . ? C4 La1 C2 47.18(6) . . ? C1 La1 C2 28.67(6) . . ? C15 La1 C2 129.45(6) . . ? N1 La1 C3 96.44(6) . . ? C13 La1 C3 81.36(6) . . ? C12 La1 C3 93.80(6) . . ? C14 La1 C3 101.10(6) . . ? C5 La1 C3 47.07(6) . . ? C11 La1 C3 122.76(6) . . ? C4 La1 C3 28.39(6) . . ? C1 La1 C3 46.89(6) . . ? C15 La1 C3 127.96(6) . . ? C2 La1 C3 28.42(6) . . ? N1 La1 Se1 129.08(4) . 2_656 ? C13 La1 Se1 115.65(4) . 2_656 ? C12 La1 Se1 128.54(4) . 2_656 ? C14 La1 Se1 87.05(4) . 2_656 ? C5 La1 Se1 102.77(4) . 2_656 ? C11 La1 Se1 104.83(4) . 2_656 ? C4 La1 Se1 129.30(4) . 2_656 ? C1 La1 Se1 82.52(4) . 2_656 ? C15 La1 Se1 81.07(4) . 2_656 ? C2 La1 Se1 93.76(4) . 2_656 ? C3 La1 Se1 122.17(4) . 2_656 ? N1 La1 Se1 70.16(4) . . ? C13 La1 Se1 129.02(4) . . ? C12 La1 Se1 109.12(4) . . ? C14 La1 Se1 111.05(4) . . ? C5 La1 Se1 100.83(4) . . ? C11 La1 Se1 82.70(4) . . ? C4 La1 Se1 121.89(4) . . ? C1 La1 Se1 107.84(4) . . ? C15 La1 Se1 84.05(4) . . ? C2 La1 Se1 135.50(4) . . ? C3 La1 Se1 147.78(4) . . ? Se1 La1 Se1 59.447(7) 2_656 . ? C26 Se1 La1 113.27(6) . 2_656 ? C26 Se1 La1 121.41(6) . . ? La1 Se1 La1 120.552(7) 2_656 . ? C21 N1 La1 175.05(17) . . ? C2 C1 C5 108.06(19) . . ? C2 C1 C6 125.7(2) . . ? C5 C1 C6 125.7(2) . . ? C2 C1 La1 76.11(12) . . ? C5 C1 La1 74.98(12) . . ? C6 C1 La1 121.76(14) . . ? C3 C2 C1 107.79(19) . . ? C3 C2 C7 124.9(2) . . ? C1 C2 C7 126.7(2) . . ? C3 C2 La1 76.79(12) . . ? C1 C2 La1 75.22(12) . . ? C7 C2 La1 121.06(15) . . ? C4 C3 C2 108.38(18) . . ? C4 C3 C8 123.4(2) . . ? C2 C3 C8 125.8(2) . . ? C4 C3 La1 74.27(11) . . ? C2 C3 La1 74.80(12) . . ? C8 C3 La1 131.30(15) . . ? C3 C4 C5 108.07(18) . . ? C3 C4 C9 124.34(19) . . ? C5 C4 C9 126.9(2) . . ? C3 C4 La1 77.34(12) . . ? C5 C4 La1 75.07(12) . . ? C9 C4 La1 121.31(14) . . ? C4 C5 C1 107.65(19) . . ? C4 C5 C10 125.3(2) . . ? C1 C5 C10 126.6(2) . . ? C4 C5 La1 76.06(12) . . ? C1 C5 La1 76.16(12) . . ? C10 C5 La1 119.97(14) . . ? C15 C11 C12 107.65(18) . . ? C15 C11 C16 125.13(19) . . ? C12 C11 C16 127.05(19) . . ? C15 C11 La1 75.98(11) . . ? C12 C11 La1 74.49(11) . . ? C16 C11 La1 119.26(13) . . ? C13 C12 C11 108.09(17) . . ? C13 C12 C17 124.56(19) . . ? C11 C12 C17 126.88(19) . . ? C13 C12 La1 75.39(11) . . ? C11 C12 La1 76.53(11) . . ? C17 C12 La1 120.42(13) . . ? C12 C13 C14 108.01(17) . . ? C12 C13 C18 125.75(19) . . ? C14 C13 C18 124.57(19) . . ? C12 C13 La1 75.60(11) . . ? C14 C13 La1 75.81(11) . . ? C18 C13 La1 126.34(14) . . ? C15 C14 C13 107.99(18) . . ? C15 C14 C19 126.9(2) . . ? C13 C14 C19 124.52(19) . . ? C15 C14 La1 76.79(11) . . ? C13 C14 La1 75.15(11) . . ? C19 C14 La1 121.15(14) . . ? C14 C15 C11 108.24(17) . . ? C14 C15 C20 126.1(2) . . ? C11 C15 C20 125.4(2) . . ? C14 C15 La1 74.46(11) . . ? C11 C15 La1 75.27(11) . . ? C20 C15 La1 120.69(13) . . ? N1 C21 C22 177.2(2) . . ? C21 C22 C25 108.7(2) . . ? C21 C22 C24 107.70(18) . . ? C25 C22 C24 111.1(2) . . ? C21 C22 C23 108.91(19) . . ? C25 C22 C23 110.7(2) . . ? C24 C22 C23 109.7(2) . . ? C27 C26 C31 118.5(2) . . ? C27 C26 Se1 121.75(16) . . ? C31 C26 Se1 119.71(17) . . ? C26 C27 C28 120.4(2) . . ? C29 C28 C27 120.4(2) . . ? C28 C29 C30 119.6(2) . . ? C29 C30 C31 120.5(2) . . ? C30 C31 C26 120.6(2) . . ? N2 La2 C33 117.31(6) . . ? N2 La2 C43 76.47(6) . . ? C33 La2 C43 140.94(6) . . ? N2 La2 C46 121.57(6) . . ? C33 La2 C46 100.59(6) . . ? C43 La2 C46 47.87(6) . . ? N2 La2 C44 75.56(6) . . ? C33 La2 C44 114.75(6) . . ? C43 La2 C44 29.16(6) . . ? C46 La2 C44 47.77(6) . . ? N2 La2 C42 104.18(6) . . ? C33 La2 C42 129.05(6) . . ? C43 La2 C42 29.03(6) . . ? C46 La2 C42 29.06(6) . . ? C44 La2 C42 47.89(6) . . ? N2 La2 C45 102.55(6) . . ? C33 La2 C45 93.44(6) . . ? C43 La2 C45 47.59(6) . . ? C46 La2 C45 28.76(6) . . ? C44 La2 C45 28.79(6) . . ? C42 La2 C45 47.53(6) . . ? N2 La2 C34 94.34(6) . . ? C33 La2 C34 28.95(6) . . ? C43 La2 C34 122.39(6) . . ? C46 La2 C34 100.87(6) . . ? C44 La2 C34 93.24(6) . . ? C42 La2 C34 128.04(6) . . ? C45 La2 C34 81.39(6) . . ? N2 La2 C32 105.30(6) . . ? C33 La2 C32 28.86(6) . . ? C43 La2 C32 169.25(6) . . ? C46 La2 C32 126.14(6) . . ? C44 La2 C32 140.42(6) . . ? C42 La2 C32 150.44(6) . . ? C45 La2 C32 122.26(6) . . ? C34 La2 C32 47.24(6) . . ? N2 La2 C35 70.03(6) . . ? C33 La2 C35 47.39(6) . . ? C43 La2 C35 126.34(6) . . ? C46 La2 C35 125.98(6) . . ? C44 La2 C35 100.72(6) . . ? C42 La2 C35 147.18(6) . . ? C45 La2 C35 100.93(6) . . ? C34 La2 C35 28.49(6) . . ? C32 La2 C35 47.04(6) . . ? N2 La2 C36 76.88(6) . . ? C33 La2 C36 47.39(6) . . ? C43 La2 C36 150.07(6) . . ? C46 La2 C36 146.53(6) . . ? C44 La2 C36 128.61(6) . . ? C42 La2 C36 175.03(6) . . ? C45 La2 C36 127.54(6) . . ? C34 La2 C36 47.02(6) . . ? C32 La2 C36 28.56(6) . . ? C35 La2 C36 28.46(6) . . ? N2 La2 Se2 131.57(4) . . ? C33 La2 Se2 91.61(4) . . ? C43 La2 Se2 105.78(5) . . ? C46 La2 Se2 86.07(4) . . ? C44 La2 Se2 128.63(4) . . ? C42 La2 Se2 81.00(4) . . ? C45 La2 Se2 114.22(5) . . ? C34 La2 Se2 120.55(4) . . ? C32 La2 Se2 81.17(4) . . ? C35 La2 Se2 127.84(4) . . ? C36 La2 Se2 102.01(4) . . ? N2 La2 Se2 71.25(4) . 2_765 ? C33 La2 Se2 132.44(4) . 2_765 ? C43 La2 Se2 86.07(4) . 2_765 ? C46 La2 Se2 113.94(4) . 2_765 ? C44 La2 Se2 112.64(4) . 2_765 ? C42 La2 Se2 86.89(4) . 2_765 ? C45 La2 Se2 132.15(4) . 2_765 ? C34 La2 Se2 144.97(4) . 2_765 ? C32 La2 Se2 104.58(4) . 2_765 ? C35 La2 Se2 119.20(4) . 2_765 ? C36 La2 Se2 98.03(4) . 2_765 ? Se2 La2 Se2 60.866(8) . 2_765 ? C57 Se2 La2 117.95(6) . . ? C57 Se2 La2 121.83(6) . 2_765 ? La2 Se2 La2 119.135(7) . 2_765 ? C52 N2 La2 174.92(16) . . ? C33 C32 C36 107.83(18) . . ? C33 C32 C37 124.82(19) . . ? C36 C32 C37 126.58(19) . . ? C33 C32 La2 73.26(11) . . ? C36 C32 La2 76.67(11) . . ? C37 C32 La2 123.87(13) . . ? C32 C33 C34 108.17(18) . . ? C32 C33 C38 125.00(19) . . ? C34 C33 C38 126.75(19) . . ? C32 C33 La2 77.87(11) . . ? C34 C33 La2 77.45(11) . . ? C38 C33 La2 113.83(13) . . ? C35 C34 C33 107.88(18) . . ? C35 C34 C39 123.0(2) . . ? C33 C34 C39 127.3(2) . . ? C35 C34 La2 76.57(11) . . ? C33 C34 La2 73.61(11) . . ? C39 C34 La2 127.86(15) . . ? C34 C35 C36 108.29(18) . . ? C34 C35 C40 124.4(2) . . ? C36 C35 C40 126.3(2) . . ? C34 C35 La2 74.95(12) . . ? C36 C35 La2 76.30(11) . . ? C40 C35 La2 124.17(14) . . ? C35 C36 C32 107.74(18) . . ? C35 C36 C41 125.47(19) . . ? C32 C36 C41 126.59(19) . . ? C35 C36 La2 75.24(12) . . ? C32 C36 La2 74.77(11) . . ? C41 C36 La2 120.08(13) . . ? C43 C42 C46 107.70(19) . . ? C43 C42 C47 125.8(2) . . ? C46 C42 C47 126.2(2) . . ? C43 C42 La2 75.10(12) . . ? C46 C42 La2 75.13(12) . . ? C47 C42 La2 120.97(14) . . ? C42 C43 C44 107.96(18) . . ? C42 C43 C48 125.1(2) . . ? C44 C43 C48 126.8(2) . . ? C42 C43 La2 75.87(12) . . ? C44 C43 La2 75.56(12) . . ? C48 C43 La2 118.13(14) . . ? C45 C44 C43 107.66(19) . . ? C45 C44 C49 125.2(2) . . ? C43 C44 C49 126.8(2) . . ? C45 C44 La2 76.21(12) . . ? C43 C44 La2 75.27(12) . . ? C49 C44 La2 120.21(15) . . ? C46 C45 C44 108.64(19) . . ? C46 C45 C50 123.5(2) . . ? C44 C45 C50 125.6(2) . . ? C46 C45 La2 74.92(12) . . ? C44 C45 La2 75.01(12) . . ? C50 C45 La2 129.98(15) . . ? C45 C46 C42 108.01(19) . . ? C45 C46 C51 125.0(2) . . ? C42 C46 C51 126.7(2) . . ? C45 C46 La2 76.32(12) . . ? C42 C46 La2 75.81(12) . . ? C51 C46 La2 118.95(15) . . ? N2 C52 C53 177.2(2) . . ? C52 C53 C54 108.36(19) . . ? C52 C53 C56 107.54(18) . . ? C54 C53 C56 110.8(2) . . ? C52 C53 C55 108.86(19) . . ? C54 C53 C55 110.87(19) . . ? C56 C53 C55 110.3(2) . . ? C62 C57 C58 118.32(19) . . ? C62 C57 Se2 119.92(16) . . ? C58 C57 Se2 121.71(16) . . ? C57 C58 C59 120.5(2) . . ? C60 C59 C58 120.4(2) . . ? C59 C60 C61 119.6(2) . . ? C60 C61 C62 120.1(2) . . ? C57 C62 C61 121.0(2) . . ? C64 C63 C68 120.9(3) . . ? C65 C64 C63 119.2(3) . . ? C64 C65 C66 120.8(3) . . ? C67 C66 C65 119.6(3) . . ? C66 C67 C68 119.9(3) . . ? C67 C68 C63 119.7(3) . . ? C74 C69 C70 119.6(3) . . ? C71 C70 C69 119.3(3) . . ? C72 C71 C70 120.3(3) . . ? C71 C72 C73 120.6(3) . . ? C74 C73 C72 119.8(4) . . ? C73 C74 C69 120.5(3) . . ? C80 C75 C76 118.5(5) . . ? C77 C76 C75 117.1(4) . . ? C78 C77 C76 121.1(4) . . ? C79 C78 C77 120.8(5) . . ? C80 C79 C78 120.7(5) . . ? C79 C80 C75 121.8(4) . . ? C82 C81 C83 119.9(3) . 2_666 ? C83 C82 C81 120.1(3) . . ? C82 C83 C81 120.0(3) . 2_666 ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 0.853 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.071 # Attachment '2b.cif' data_tjm4 _database_code_depnum_ccdc_archive 'CCDC 765770' #TrackingRef '2b.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H70 La2 Se2' _chemical_formula_weight 1130.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 Orthorhombic _symmetry_space_group_name_H-M Pnn2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 10.3729(10) _cell_length_b 12.0187(12) _cell_length_c 19.4835(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2429.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 1016 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.26 _exptl_crystal_description Irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 3.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4839 _exptl_absorpt_correction_T_max 0.5336 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 SMART1K CCD' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25662 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.30 _reflns_number_total 6015 _reflns_number_gt 5560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0224P)^2^+0.8962P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.768(9) _refine_ls_number_reflns 6015 _refine_ls_number_parameters 265 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0461 _refine_ls_wR_factor_gt 0.0445 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.173 _refine_ls_shift/su_mean 0.004 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 0.5000 0.5000 0.515662(7) 0.01681(6) Uani 1 2 d S . . La2 La 0.5000 0.5000 0.242455(7) 0.01722(6) Uani 1 2 d S . . Se1 Se 0.385737(18) 0.406532(15) 0.37860(3) 0.02140(5) Uani 1 1 d . . . C1 C 0.2450(3) 0.5086(2) 0.56479(13) 0.0245(5) Uani 1 1 d . . . C2 C 0.2496(2) 0.5942(2) 0.51530(14) 0.0208(5) Uani 1 1 d . . . C3 C 0.3310(3) 0.6790(2) 0.53979(13) 0.0224(5) Uani 1 1 d . . . C4 C 0.3767(3) 0.6472(2) 0.60630(14) 0.0240(6) Uani 1 1 d . . . C5 C 0.3212(3) 0.5422(2) 0.62152(14) 0.0247(5) Uani 1 1 d . . . C6 C 0.1675(3) 0.4032(2) 0.55915(15) 0.0352(6) Uani 1 1 d . . . H6A H 0.1993 0.3488 0.5926 0.053 Uiso 1 1 calc R . . H6B H 0.1762 0.3727 0.5127 0.053 Uiso 1 1 calc R . . H6C H 0.0766 0.4194 0.5684 0.053 Uiso 1 1 calc R . . C7 C 0.1662(3) 0.6023(2) 0.45149(13) 0.0284(5) Uani 1 1 d . . . H7A H 0.0967 0.6561 0.4594 0.043 Uiso 1 1 calc R . . H7B H 0.1290 0.5292 0.4413 0.043 Uiso 1 1 calc R . . H7C H 0.2190 0.6269 0.4126 0.043 Uiso 1 1 calc R . . C8 C 0.3541(3) 0.7888(2) 0.50450(14) 0.0302(6) Uani 1 1 d . . . H8A H 0.3734 0.7758 0.4559 0.045 Uiso 1 1 calc R . . H8B H 0.4271 0.8268 0.5262 0.045 Uiso 1 1 calc R . . H8C H 0.2768 0.8352 0.5084 0.045 Uiso 1 1 calc R . . C9 C 0.4506(3) 0.7223(2) 0.65349(15) 0.0347(6) Uani 1 1 d . . . H9A H 0.4654 0.6842 0.6973 0.052 Uiso 1 1 calc R . . H9B H 0.4011 0.7905 0.6615 0.052 Uiso 1 1 calc R . . H9C H 0.5336 0.7412 0.6325 0.052 Uiso 1 1 calc R . . C10 C 0.3196(3) 0.4857(2) 0.69069(14) 0.0347(7) Uani 1 1 d . . . H10A H 0.4006 0.5013 0.7148 0.052 Uiso 1 1 calc R . . H10B H 0.3102 0.4052 0.6844 0.052 Uiso 1 1 calc R . . H10C H 0.2471 0.5140 0.7178 0.052 Uiso 1 1 calc R . . C11 C 0.3153(3) 0.5909(2) 0.15280(14) 0.0243(5) Uani 1 1 d . . . C12 C 0.2743(3) 0.6251(2) 0.21954(14) 0.0219(5) Uani 1 1 d . . . C13 C 0.3630(2) 0.7038(2) 0.24372(13) 0.0210(5) Uani 1 1 d . . . C14 C 0.4608(2) 0.7181(2) 0.19381(12) 0.0215(5) Uani 1 1 d . . . C15 C 0.4303(3) 0.6492(2) 0.13673(14) 0.0220(5) Uani 1 1 d . . . C16 C 0.2376(3) 0.5178(2) 0.10555(16) 0.0383(7) Uani 1 1 d . . . H16A H 0.2734 0.5219 0.0591 0.057 Uiso 1 1 calc R . . H16B H 0.1478 0.5433 0.1049 0.057 Uiso 1 1 calc R . . H16C H 0.2409 0.4408 0.1219 0.057 Uiso 1 1 calc R . . C17 C 0.1518(3) 0.5882(3) 0.25393(16) 0.0363(7) Uani 1 1 d . . . H17A H 0.1718 0.5321 0.2889 0.054 Uiso 1 1 calc R . . H17B H 0.0936 0.5560 0.2196 0.054 Uiso 1 1 calc R . . H17C H 0.1101 0.6522 0.2757 0.054 Uiso 1 1 calc R . . C18 C 0.3477(3) 0.7726(2) 0.30787(13) 0.0298(6) Uani 1 1 d . . . H18A H 0.2651 0.8121 0.3064 0.045 Uiso 1 1 calc R . . H18B H 0.4182 0.8266 0.3108 0.045 Uiso 1 1 calc R . . H18C H 0.3498 0.7238 0.3481 0.045 Uiso 1 1 calc R . . C19 C 0.5705(3) 0.7988(2) 0.19812(15) 0.0315(6) Uani 1 1 d . . . H19A H 0.6360 0.7792 0.1639 0.047 Uiso 1 1 calc R . . H19B H 0.6086 0.7958 0.2441 0.047 Uiso 1 1 calc R . . H19C H 0.5388 0.8742 0.1891 0.047 Uiso 1 1 calc R . . C20 C 0.4948(3) 0.6533(2) 0.06761(14) 0.0333(7) Uani 1 1 d . . . H20A H 0.5671 0.7057 0.0692 0.050 Uiso 1 1 calc R . . H20B H 0.4325 0.6777 0.0329 0.050 Uiso 1 1 calc R . . H20C H 0.5269 0.5791 0.0557 0.050 Uiso 1 1 calc R . . C21 C 0.29174(17) 0.26866(15) 0.3790(2) 0.0205(4) Uani 1 1 d . . . C22 C 0.3487(3) 0.1711(2) 0.40094(14) 0.0337(6) Uani 1 1 d . . . H22A H 0.4356 0.1720 0.4163 0.040 Uiso 1 1 calc R . . C23 C 0.2805(3) 0.0718(2) 0.40085(16) 0.0412(8) Uani 1 1 d . . . H23A H 0.3211 0.0052 0.4158 0.049 Uiso 1 1 calc R . . C24 C 0.1553(3) 0.0693(2) 0.3794(3) 0.0447(6) Uani 1 1 d . . . H24A H 0.1086 0.0012 0.3791 0.054 Uiso 1 1 calc R . . C25 C 0.0974(3) 0.1662(3) 0.35805(17) 0.0502(10) Uani 1 1 d . . . H25A H 0.0102 0.1649 0.3431 0.060 Uiso 1 1 calc R . . C26 C 0.1648(3) 0.2659(2) 0.35807(14) 0.0349(7) Uani 1 1 d . . . H26A H 0.1235 0.3324 0.3436 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01850(14) 0.01568(14) 0.01626(14) 0.000 0.000 0.00239(9) La2 0.02093(15) 0.01476(14) 0.01597(14) 0.000 0.000 -0.00125(9) Se1 0.02509(9) 0.01973(9) 0.01938(8) -0.00225(18) 0.00263(17) -0.00763(7) C1 0.0237(13) 0.0234(12) 0.0264(12) 0.0007(10) 0.0083(10) 0.0023(9) C2 0.0209(13) 0.0185(12) 0.0230(13) -0.0002(10) 0.0063(10) 0.0036(10) C3 0.0281(14) 0.0177(13) 0.0213(13) 0.0001(10) 0.0073(10) 0.0055(11) C4 0.0256(15) 0.0241(14) 0.0224(13) -0.0048(11) 0.0052(11) 0.0051(12) C5 0.0291(13) 0.0266(14) 0.0183(12) 0.0010(11) 0.0073(10) 0.0061(12) C6 0.0351(15) 0.0309(15) 0.0397(15) 0.0018(12) 0.0107(12) -0.0054(12) C7 0.0244(12) 0.0353(15) 0.0256(13) 0.0005(10) 0.0007(10) 0.0070(11) C8 0.0434(16) 0.0197(13) 0.0276(13) 0.0003(10) 0.0119(11) 0.0024(11) C9 0.0396(16) 0.0299(15) 0.0345(15) -0.0075(12) -0.0022(12) 0.0051(13) C10 0.0448(17) 0.0342(16) 0.0251(13) 0.0088(11) 0.0109(12) 0.0126(13) C11 0.0285(14) 0.0212(14) 0.0232(13) 0.0009(10) -0.0056(10) 0.0002(12) C12 0.0208(13) 0.0205(13) 0.0245(13) 0.0090(10) -0.0034(11) -0.0034(11) C13 0.0231(13) 0.0220(13) 0.0179(12) 0.0006(10) -0.0019(10) 0.0038(10) C14 0.0250(11) 0.0175(11) 0.0219(11) 0.0018(9) 0.0010(9) 0.0021(9) C15 0.0267(15) 0.0185(12) 0.0208(12) 0.0026(10) 0.0000(11) 0.0016(11) C16 0.0473(19) 0.0326(15) 0.0349(16) -0.0036(12) -0.0129(14) -0.0057(13) C17 0.0230(14) 0.0480(18) 0.0378(16) 0.0131(14) -0.0009(11) -0.0015(12) C18 0.0352(15) 0.0315(14) 0.0227(12) -0.0045(10) -0.0010(10) 0.0078(11) C19 0.0322(14) 0.0270(13) 0.0353(14) 0.0077(11) -0.0003(11) -0.0083(11) C20 0.0487(18) 0.0269(14) 0.0244(13) 0.0080(11) 0.0095(11) 0.0082(11) C21 0.0215(9) 0.0203(8) 0.0196(8) -0.0041(18) 0.0038(18) -0.0072(7) C22 0.0260(13) 0.0281(13) 0.0469(17) 0.0058(11) -0.0065(11) -0.0054(10) C23 0.0473(17) 0.0216(12) 0.055(2) 0.0086(11) 0.0029(13) -0.0069(12) C24 0.0487(14) 0.0326(12) 0.0529(14) -0.001(3) -0.008(3) -0.0235(11) C25 0.0338(16) 0.0499(18) 0.067(3) 0.0096(15) -0.0146(14) -0.0183(14) C26 0.0262(12) 0.0319(13) 0.0465(18) 0.0064(11) -0.0081(11) -0.0074(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 La1 Cnt1 2.547 . ? La2 Cnt2 2.551 . ? La1 C4 2.808(3) 2_665 ? La1 C4 2.808(3) . ? La1 C1 2.815(3) . ? La1 C1 2.815(3) 2_665 ? La1 C3 2.815(2) 2_665 ? La1 C3 2.815(2) . ? La1 C5 2.820(3) . ? La1 C5 2.820(3) 2_665 ? La1 C2 2.833(2) 2_665 ? La1 C2 2.833(2) . ? La1 Se1 3.1302(6) 2_665 ? La1 Se1 3.1303(6) . ? La2 C11 2.813(3) . ? La2 C11 2.813(3) 2_665 ? La2 C14 2.817(2) . ? La2 C14 2.817(2) 2_665 ? La2 C12 2.818(3) 2_665 ? La2 C12 2.818(3) . ? La2 C15 2.825(3) 2_665 ? La2 C15 2.825(3) . ? La2 C13 2.832(2) . ? La2 C13 2.832(2) 2_665 ? La2 Se1 3.1149(6) . ? La2 Se1 3.1149(6) 2_665 ? Se1 C21 1.9226(17) . ? C1 C2 1.411(3) . ? C1 C5 1.418(4) . ? C1 C6 1.504(4) . ? C2 C3 1.407(4) . ? C2 C7 1.518(4) . ? C3 C4 1.432(4) . ? C3 C8 1.507(4) . ? C4 C5 1.418(4) . ? C4 C9 1.499(4) . ? C5 C10 1.509(4) . ? C11 C15 1.419(4) . ? C11 C12 1.429(4) . ? C11 C16 1.506(4) . ? C12 C13 1.400(4) . ? C12 C17 1.504(4) . ? C13 C14 1.416(3) . ? C13 C18 1.507(3) . ? C14 C15 1.422(4) . ? C14 C19 1.498(4) . ? C15 C20 1.505(4) . ? C21 C26 1.379(3) . ? C21 C22 1.381(3) . ? C22 C23 1.387(4) . ? C23 C24 1.365(4) . ? C24 C25 1.375(5) . ? C25 C26 1.388(4) . ? 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 Cnt1 La1 Se1 102.1 . . ? Cnt1 La1 Se1 119.5 . 2_665 ? Cnt1 La1 Cnt1 131.3 . 2_665 ? Cnt2 La2 Se1 114.2 . . ? Cnt2 La2 Se1 106.3 . 2_665 ? Cnt2 La2 Cnt2 132.1 . 2_665 ? C4 La1 C4 102.05(12) 2_665 . ? C4 La1 C1 103.72(8) 2_665 . ? C4 La1 C1 48.32(8) . . ? C4 La1 C1 48.32(8) 2_665 2_665 ? C4 La1 C1 103.72(8) . 2_665 ? C1 La1 C1 140.24(11) . 2_665 ? C4 La1 C3 29.51(8) 2_665 2_665 ? C4 La1 C3 131.31(8) . 2_665 ? C1 La1 C3 123.81(8) . 2_665 ? C1 La1 C3 47.93(8) 2_665 2_665 ? C4 La1 C3 131.32(8) 2_665 . ? C4 La1 C3 29.51(8) . . ? C1 La1 C3 47.93(8) . . ? C1 La1 C3 123.81(8) 2_665 . ? C3 La1 C3 160.77(11) 2_665 . ? C4 La1 C5 87.30(8) 2_665 . ? C4 La1 C5 29.19(8) . . ? C1 La1 C5 29.14(8) . . ? C1 La1 C5 112.08(8) 2_665 . ? C3 La1 C5 115.15(8) 2_665 . ? C3 La1 C5 47.99(8) . . ? C4 La1 C5 29.19(8) 2_665 2_665 ? C4 La1 C5 87.30(8) . 2_665 ? C1 La1 C5 112.08(8) . 2_665 ? C1 La1 C5 29.14(8) 2_665 2_665 ? C3 La1 C5 47.99(8) 2_665 2_665 ? C3 La1 C5 115.15(8) . 2_665 ? C5 La1 C5 85.98(12) . 2_665 ? C4 La1 C2 48.11(8) 2_665 2_665 ? C4 La1 C2 132.13(8) . 2_665 ? C1 La1 C2 151.27(8) . 2_665 ? C1 La1 C2 28.93(7) 2_665 2_665 ? C3 La1 C2 28.84(8) 2_665 2_665 ? C3 La1 C2 151.25(8) . 2_665 ? C5 La1 C2 132.58(8) . 2_665 ? C5 La1 C2 47.70(8) 2_665 2_665 ? C4 La1 C2 132.13(8) 2_665 . ? C4 La1 C2 48.11(8) . . ? C1 La1 C2 28.93(7) . . ? C1 La1 C2 151.27(8) 2_665 . ? C3 La1 C2 151.25(8) 2_665 . ? C3 La1 C2 28.84(8) . . ? C5 La1 C2 47.70(8) . . ? C5 La1 C2 132.58(8) 2_665 . ? C2 La1 C2 179.72(11) 2_665 . ? C4 La1 Se1 126.17(6) 2_665 2_665 ? C4 La1 Se1 118.88(6) . 2_665 ? C1 La1 Se1 129.25(5) . 2_665 ? C1 La1 Se1 86.99(6) 2_665 2_665 ? C3 La1 Se1 100.43(6) 2_665 2_665 ? C3 La1 Se1 95.97(6) . 2_665 ? C5 La1 Se1 143.95(6) . 2_665 ? C5 La1 Se1 116.08(6) 2_665 2_665 ? C2 La1 Se1 78.13(6) 2_665 2_665 ? C2 La1 Se1 101.63(5) . 2_665 ? C4 La1 Se1 118.88(6) 2_665 . ? C4 La1 Se1 126.18(6) . . ? C1 La1 Se1 86.99(6) . . ? C1 La1 Se1 129.25(5) 2_665 . ? C3 La1 Se1 95.97(6) 2_665 . ? C3 La1 Se1 100.43(6) . . ? C5 La1 Se1 116.08(6) . . ? C5 La1 Se1 143.95(6) 2_665 . ? C2 La1 Se1 101.63(5) 2_665 . ? C2 La1 Se1 78.13(6) . . ? Se1 La1 Se1 62.892(14) 2_665 . ? C11 La2 C11 103.25(11) . 2_665 ? C11 La2 C14 48.04(8) . . ? C11 La2 C14 104.53(8) 2_665 . ? C11 La2 C14 104.53(8) . 2_665 ? C11 La2 C14 48.04(8) 2_665 2_665 ? C14 La2 C14 140.68(10) . 2_665 ? C11 La2 C12 132.42(8) . 2_665 ? C11 La2 C12 29.39(8) 2_665 2_665 ? C14 La2 C12 124.29(8) . 2_665 ? C14 La2 C12 47.94(8) 2_665 2_665 ? C11 La2 C12 29.39(8) . . ? C11 La2 C12 132.42(8) 2_665 . ? C14 La2 C12 47.94(8) . . ? C14 La2 C12 124.29(8) 2_665 . ? C12 La2 C12 161.77(11) 2_665 . ? C11 La2 C15 88.16(8) . 2_665 ? C11 La2 C15 29.15(8) 2_665 2_665 ? C14 La2 C15 112.47(7) . 2_665 ? C14 La2 C15 29.20(7) 2_665 2_665 ? C12 La2 C15 48.18(8) 2_665 2_665 ? C12 La2 C15 115.83(8) . 2_665 ? C11 La2 C15 29.15(8) . . ? C11 La2 C15 88.16(8) 2_665 . ? C14 La2 C15 29.20(7) . . ? C14 La2 C15 112.47(7) 2_665 . ? C12 La2 C15 115.83(8) 2_665 . ? C12 La2 C15 48.18(8) . . ? C15 La2 C15 86.37(11) 2_665 . ? C11 La2 C13 47.76(8) . . ? C11 La2 C13 133.08(8) 2_665 . ? C14 La2 C13 29.02(7) . . ? C14 La2 C13 151.67(7) 2_665 . ? C12 La2 C13 151.63(7) 2_665 . ? C12 La2 C13 28.70(8) . . ? C15 La2 C13 133.13(8) 2_665 . ? C15 La2 C13 47.85(8) . . ? C11 La2 C13 133.08(8) . 2_665 ? C11 La2 C13 47.76(8) 2_665 2_665 ? C14 La2 C13 151.67(7) . 2_665 ? C14 La2 C13 29.03(7) 2_665 2_665 ? C12 La2 C13 28.70(8) 2_665 2_665 ? C12 La2 C13 151.63(7) . 2_665 ? C15 La2 C13 47.85(8) 2_665 2_665 ? C15 La2 C13 133.13(8) . 2_665 ? C13 La2 C13 179.00(10) . 2_665 ? C11 La2 Se1 114.18(6) . . ? C11 La2 Se1 130.37(6) 2_665 . ? C14 La2 Se1 124.55(5) . . ? C14 La2 Se1 90.34(5) 2_665 . ? C12 La2 Se1 104.98(6) 2_665 . ? C12 La2 Se1 90.65(6) . . ? C15 La2 Se1 119.30(6) 2_665 . ? C15 La2 Se1 138.81(6) . . ? C13 La2 Se1 96.52(5) . . ? C13 La2 Se1 82.63(5) 2_665 . ? C11 La2 Se1 130.38(6) . 2_665 ? C11 La2 Se1 114.18(6) 2_665 2_665 ? C14 La2 Se1 90.34(5) . 2_665 ? C14 La2 Se1 124.55(5) 2_665 2_665 ? C12 La2 Se1 90.65(6) 2_665 2_665 ? C12 La2 Se1 104.98(6) . 2_665 ? C15 La2 Se1 138.81(6) 2_665 2_665 ? C15 La2 Se1 119.30(6) . 2_665 ? C13 La2 Se1 82.63(5) . 2_665 ? C13 La2 Se1 96.52(5) 2_665 2_665 ? Se1 La2 Se1 63.237(15) . 2_665 ? C21 Se1 La2 120.50(13) . . ? C21 Se1 La1 119.83(13) . . ? La2 Se1 La1 116.936(8) . . ? C2 C1 C5 107.8(2) . . ? C2 C1 C6 125.6(3) . . ? C5 C1 C6 126.5(2) . . ? C2 C1 La1 76.26(14) . . ? C5 C1 La1 75.61(15) . . ? C6 C1 La1 116.50(16) . . ? C3 C2 C1 108.5(2) . . ? C3 C2 C7 125.0(2) . . ? C1 C2 C7 126.0(2) . . ? C3 C2 La1 74.86(14) . . ? C1 C2 La1 74.81(14) . . ? C7 C2 La1 123.39(16) . . ? C2 C3 C4 108.2(2) . . ? C2 C3 C8 125.1(2) . . ? C4 C3 C8 126.5(3) . . ? C2 C3 La1 76.29(14) . . ? C4 C3 La1 74.95(15) . . ? C8 C3 La1 119.61(18) . . ? C5 C4 C3 107.0(3) . . ? C5 C4 C9 127.9(3) . . ? C3 C4 C9 124.3(3) . . ? C5 C4 La1 75.88(15) . . ? C3 C4 La1 75.54(14) . . ? C9 C4 La1 122.16(19) . . ? C4 C5 C1 108.5(2) . . ? C4 C5 C10 126.3(3) . . ? C1 C5 C10 124.2(3) . . ? C4 C5 La1 74.93(15) . . ? C1 C5 La1 75.24(15) . . ? C10 C5 La1 125.40(18) . . ? C15 C11 C12 108.0(2) . . ? C15 C11 C16 127.1(3) . . ? C12 C11 C16 124.4(3) . . ? C15 C11 La2 75.87(15) . . ? C12 C11 La2 75.50(15) . . ? C16 C11 La2 121.18(19) . . ? C13 C12 C11 107.8(2) . . ? C13 C12 C17 127.2(3) . . ? C11 C12 C17 124.9(3) . . ? C13 C12 La2 76.18(15) . . ? C11 C12 La2 75.12(15) . . ? C17 C12 La2 118.27(18) . . ? C12 C13 C14 108.8(2) . . ? C12 C13 C18 125.5(2) . . ? C14 C13 C18 125.4(2) . . ? C12 C13 La2 75.12(15) . . ? C14 C13 La2 74.89(14) . . ? C18 C13 La2 122.31(16) . . ? C13 C14 C15 107.9(2) . . ? C13 C14 C19 125.8(2) . . ? C15 C14 C19 126.1(2) . . ? C13 C14 La2 76.08(14) . . ? C15 C14 La2 75.73(14) . . ? C19 C14 La2 118.29(17) . . ? C11 C15 C14 107.6(2) . . ? C11 C15 C20 126.0(3) . . ? C14 C15 C20 125.6(3) . . ? C11 C15 La2 74.98(15) . . ? C14 C15 La2 75.08(14) . . ? C20 C15 La2 124.04(18) . . ? C26 C21 C22 118.7(2) . . ? C26 C21 Se1 120.23(18) . . ? C22 C21 Se1 121.10(18) . . ? C21 C22 C23 120.8(2) . . ? C24 C23 C22 120.3(3) . . ? C23 C24 C25 119.3(2) . . ? C24 C25 C26 120.8(3) . . ? C21 C26 C25 120.1(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.499 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.063 # Attachment 'tjm35 is 5.cif' data_tjm35 _database_code_depnum_ccdc_archive 'CCDC 765771' #TrackingRef 'tjm35 is 5.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H70 Pr2 S2' _chemical_formula_weight 1041.02 _chemical_absolute_configuration ad 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnn2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 10.3504(6) _cell_length_b 11.7647(7) _cell_length_c 19.4542(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2368.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 148(2) _cell_measurement_reflns_used 9960 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.27 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 2.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6979 _exptl_absorpt_correction_T_max 0.7671 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 148(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25686 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5403 _reflns_number_gt 4399 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 Version 2.2-0' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT Version 7.46a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0538P)^2^+0.6425P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 5403 _refine_ls_number_parameters 264 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.5000 0.5000 0.508226(12) 0.01697(12) Uani 1 2 d S . . Pr2 Pr 0.5000 0.5000 0.247474(12) 0.01714(12) Uani 1 2 d S . . S1 S 0.39132(9) 0.40818(7) 0.37740(10) 0.02366(19) Uani 1 1 d . . . C1 C 0.2510(5) 0.5029(3) 0.5589(3) 0.0234(10) Uani 1 1 d . . . C2 C 0.2504(4) 0.5904(4) 0.5089(2) 0.0213(9) Uani 1 1 d . . . C3 C 0.3304(4) 0.6791(4) 0.5339(2) 0.0214(9) Uani 1 1 d . . . C4 C 0.3792(4) 0.6457(4) 0.6001(2) 0.0248(10) Uani 1 1 d . . . C5 C 0.3263(5) 0.5392(4) 0.6157(2) 0.0257(10) Uani 1 1 d . . . C6 C 0.1728(5) 0.3949(4) 0.5550(3) 0.0353(11) Uani 1 1 d . . . H6A H 0.2188 0.3338 0.5790 0.053 Uiso 1 1 calc R . . H6B H 0.1605 0.3736 0.5067 0.053 Uiso 1 1 calc R . . H6C H 0.0885 0.4070 0.5767 0.053 Uiso 1 1 calc R . . C7 C 0.1668(4) 0.5971(4) 0.4465(2) 0.0278(10) Uani 1 1 d . . . H7A H 0.0916 0.6452 0.4563 0.042 Uiso 1 1 calc R . . H7B H 0.1376 0.5206 0.4340 0.042 Uiso 1 1 calc R . . H7C H 0.2162 0.6299 0.4084 0.042 Uiso 1 1 calc R . . C8 C 0.3466(5) 0.7936(4) 0.5005(2) 0.0283(10) Uani 1 1 d . . . H8A H 0.3655 0.7835 0.4515 0.042 Uiso 1 1 calc R . . H8B H 0.4180 0.8343 0.5225 0.042 Uiso 1 1 calc R . . H8C H 0.2667 0.8375 0.5057 0.042 Uiso 1 1 calc R . . C9 C 0.4514(5) 0.7246(4) 0.6470(3) 0.0330(11) Uani 1 1 d . . . H9A H 0.4727 0.6848 0.6898 0.049 Uiso 1 1 calc R . . H9B H 0.3975 0.7909 0.6574 0.049 Uiso 1 1 calc R . . H9C H 0.5312 0.7496 0.6245 0.049 Uiso 1 1 calc R . . C10 C 0.3230(6) 0.4818(4) 0.6850(3) 0.0354(12) Uani 1 1 d . . . H10A H 0.4069 0.4909 0.7076 0.053 Uiso 1 1 calc R . . H10B H 0.3045 0.4007 0.6789 0.053 Uiso 1 1 calc R . . H10C H 0.2554 0.5164 0.7133 0.053 Uiso 1 1 calc R . . C11 C 0.3187(4) 0.5901(4) 0.1569(2) 0.0239(9) Uani 1 1 d . . . C12 C 0.2784(4) 0.6273(4) 0.2231(2) 0.0212(9) Uani 1 1 d . . . C13 C 0.3696(4) 0.7074(4) 0.2468(2) 0.0220(9) Uani 1 1 d . . . C14 C 0.4673(4) 0.7176(4) 0.1971(2) 0.0223(9) Uani 1 1 d . . . C15 C 0.4358(4) 0.6487(4) 0.1406(2) 0.0219(9) Uani 1 1 d . . . C16 C 0.2378(6) 0.5185(4) 0.1093(3) 0.0340(12) Uani 1 1 d . . . H16A H 0.2716 0.5246 0.0624 0.051 Uiso 1 1 calc R . . H16B H 0.1482 0.5454 0.1103 0.051 Uiso 1 1 calc R . . H16C H 0.2409 0.4390 0.1242 0.051 Uiso 1 1 calc R . . C17 C 0.1524(4) 0.5951(4) 0.2567(3) 0.0329(11) Uani 1 1 d . . . H17A H 0.1673 0.5337 0.2898 0.049 Uiso 1 1 calc R . . H17B H 0.0913 0.5695 0.2215 0.049 Uiso 1 1 calc R . . H17C H 0.1167 0.6613 0.2807 0.049 Uiso 1 1 calc R . . C18 C 0.3562(5) 0.7792(4) 0.3102(2) 0.0318(10) Uani 1 1 d . . . H18A H 0.2734 0.8195 0.3090 0.048 Uiso 1 1 calc R . . H18B H 0.4270 0.8345 0.3120 0.048 Uiso 1 1 calc R . . H18C H 0.3596 0.7305 0.3510 0.048 Uiso 1 1 calc R . . C19 C 0.5792(4) 0.8004(4) 0.2002(3) 0.0309(10) Uani 1 1 d . . . H19A H 0.6496 0.7728 0.1709 0.046 Uiso 1 1 calc R . . H19B H 0.6098 0.8067 0.2477 0.046 Uiso 1 1 calc R . . H19C H 0.5506 0.8751 0.1840 0.046 Uiso 1 1 calc R . . C20 C 0.4988(4) 0.6517(5) 0.0711(3) 0.0332(12) Uani 1 1 d . . . H20A H 0.5613 0.7142 0.0695 0.050 Uiso 1 1 calc R . . H20B H 0.4328 0.6633 0.0356 0.050 Uiso 1 1 calc R . . H20C H 0.5435 0.5796 0.0627 0.050 Uiso 1 1 calc R . . C21 C 0.2981(3) 0.2811(3) 0.3784(3) 0.0205(7) Uani 1 1 d . . . C22 C 0.3458(5) 0.1826(4) 0.4091(3) 0.0356(11) Uani 1 1 d . . . H22A H 0.4277 0.1840 0.4312 0.043 Uiso 1 1 calc R . . C23 C 0.2755(5) 0.0836(4) 0.4078(3) 0.0410(12) Uani 1 1 d . . . H23A H 0.3104 0.0167 0.4279 0.049 Uiso 1 1 calc R . . C24 C 0.1554(4) 0.0798(4) 0.3775(4) 0.0417(11) Uani 1 1 d . . . H24A H 0.1075 0.0109 0.3764 0.050 Uiso 1 1 calc R . . C25 C 0.1066(5) 0.1761(5) 0.3495(3) 0.0468(14) Uani 1 1 d . . . H25A H 0.0230 0.1745 0.3294 0.056 Uiso 1 1 calc R . . C26 C 0.1764(4) 0.2775(4) 0.3495(3) 0.0336(11) Uani 1 1 d . . . H26A H 0.1403 0.3441 0.3297 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 Pr1 0.0169(2) 0.0154(2) 0.0185(3) 0.000 0.000 0.00132(12) Pr2 0.0184(2) 0.0149(2) 0.0181(3) 0.000 0.000 0.00030(12) S1 0.0252(4) 0.0235(4) 0.0223(4) -0.0035(7) 0.0033(6) -0.0085(4) C1 0.023(2) 0.021(2) 0.026(2) 0.0007(16) 0.0060(19) -0.0008(16) C2 0.021(2) 0.019(2) 0.024(2) -0.0005(18) 0.0034(17) 0.0016(18) C3 0.023(2) 0.017(2) 0.024(2) -0.0022(18) 0.0044(18) 0.0031(18) C4 0.025(2) 0.027(2) 0.022(2) -0.0066(18) 0.0059(19) 0.008(2) C5 0.029(2) 0.025(2) 0.023(2) -0.0012(19) 0.008(2) 0.011(2) C6 0.035(3) 0.027(3) 0.043(3) -0.001(2) 0.008(2) -0.006(2) C7 0.022(2) 0.033(3) 0.028(2) -0.0016(19) -0.0019(18) 0.0038(19) C8 0.032(2) 0.024(2) 0.029(2) -0.0020(18) 0.0109(19) -0.0017(19) C9 0.033(3) 0.035(3) 0.031(3) -0.005(2) 0.001(2) 0.006(2) C10 0.042(3) 0.037(3) 0.027(3) 0.005(2) 0.012(2) 0.015(2) C11 0.024(2) 0.021(2) 0.026(2) 0.0021(19) -0.0012(18) 0.0050(19) C12 0.018(2) 0.019(2) 0.026(2) 0.0044(18) -0.0040(18) -0.0009(17) C13 0.025(2) 0.020(2) 0.022(2) -0.0012(17) -0.0020(16) 0.0042(17) C14 0.025(2) 0.016(2) 0.026(2) 0.0036(17) 0.0011(18) 0.0009(17) C15 0.023(2) 0.017(2) 0.026(2) 0.0044(17) -0.0028(19) 0.0034(18) C16 0.034(3) 0.031(3) 0.037(3) -0.003(2) -0.012(2) -0.002(2) C17 0.019(2) 0.046(3) 0.033(3) 0.008(2) 0.0017(19) -0.001(2) C18 0.035(3) 0.036(3) 0.024(2) -0.002(2) -0.0019(19) 0.005(2) C19 0.030(2) 0.028(2) 0.035(3) 0.007(2) -0.002(2) -0.008(2) C20 0.044(3) 0.028(3) 0.027(3) 0.008(2) 0.010(2) 0.0078(19) C21 0.0235(17) 0.0197(16) 0.0184(16) 0.000(3) 0.006(2) -0.0063(13) C22 0.030(2) 0.037(3) 0.040(3) 0.007(2) -0.009(2) -0.005(2) C23 0.047(3) 0.027(3) 0.049(3) 0.016(2) 0.000(3) -0.002(2) C24 0.047(3) 0.031(2) 0.047(2) -0.002(3) 0.004(4) -0.020(2) C25 0.033(3) 0.051(3) 0.056(3) 0.005(3) -0.006(3) -0.019(3) C26 0.029(2) 0.027(2) 0.045(3) 0.002(2) -0.009(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 Cnt1 2.507 . ? Pr2 Cnt2 2.509 . ? Pr1 C1 2.760(5) 2_665 ? Pr1 C1 2.760(5) . ? Pr1 C4 2.774(4) . ? Pr1 C4 2.774(4) 2_665 ? Pr1 C3 2.788(4) . ? Pr1 C3 2.788(4) 2_665 ? Pr1 C2 2.794(4) . ? Pr1 C2 2.794(4) 2_665 ? Pr1 C5 2.797(4) 2_665 ? Pr1 C5 2.797(4) . ? Pr1 S1 2.9849(17) . ? Pr1 S1 2.9849(17) 2_665 ? Pr2 C14 2.762(4) 2_665 ? Pr2 C14 2.762(4) . ? Pr2 C12 2.780(4) . ? Pr2 C12 2.780(4) 2_665 ? Pr2 C11 2.784(4) . ? Pr2 C11 2.784(4) 2_665 ? Pr2 C13 2.789(4) 2_665 ? Pr2 C13 2.789(4) . ? Pr2 C15 2.797(4) 2_665 ? Pr2 C15 2.797(4) . ? Pr2 S1 2.9700(18) 2_665 ? Pr2 S1 2.9700(18) . ? S1 C21 1.780(3) . ? C1 C2 1.417(6) . ? C1 C5 1.418(7) . ? C1 C6 1.509(6) . ? C2 C3 1.418(6) . ? C2 C7 1.492(6) . ? C3 C4 1.438(7) . ? C3 C8 1.504(6) . ? C4 C5 1.401(7) . ? C4 C9 1.502(7) . ? C5 C10 1.507(7) . ? C11 C12 1.424(6) . ? C11 C15 1.429(6) . ? C11 C16 1.506(7) . ? C12 C13 1.411(6) . ? C12 C17 1.507(6) . ? C13 C14 1.404(6) . ? C13 C18 1.501(6) . ? C14 C15 1.405(6) . ? C14 C19 1.515(6) . ? C15 C20 1.502(6) . ? C21 C26 1.380(6) . ? C21 C22 1.394(6) . ? C22 C23 1.374(7) . ? C23 C24 1.377(7) . ? C24 C25 1.354(7) . ? C25 C26 1.396(6) . ? 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 Cnt1 Pr1 S1 102.8 . . ? Cnt1 Pr1 S1 120.7 . 2_665 ? Cnt1 Pr1 Cnt1 129.2 . 2_665 ? Cnt2 Pr2 S1 115.7 . . ? Cnt2 Pr2 S1 106.7 . 2_665 ? Cnt2 Pr2 Cnt2 129.9 . 2_665 ? C1 Pr1 C1 138.1(2) 2_665 . ? C1 Pr1 C4 101.44(14) 2_665 . ? C1 Pr1 C4 48.79(13) . . ? C1 Pr1 C4 48.79(13) 2_665 2_665 ? C1 Pr1 C4 101.44(14) . 2_665 ? C4 Pr1 C4 99.8(2) . 2_665 ? C1 Pr1 C3 122.25(12) 2_665 . ? C1 Pr1 C3 48.58(12) . . ? C4 Pr1 C3 29.97(13) . . ? C4 Pr1 C3 129.46(14) 2_665 . ? C1 Pr1 C3 48.58(12) 2_665 2_665 ? C1 Pr1 C3 122.25(12) . 2_665 ? C4 Pr1 C3 129.46(14) . 2_665 ? C4 Pr1 C3 29.97(13) 2_665 2_665 ? C3 Pr1 C3 159.37(19) . 2_665 ? C1 Pr1 C2 150.06(13) 2_665 . ? C1 Pr1 C2 29.54(12) . . ? C4 Pr1 C2 49.07(14) . . ? C4 Pr1 C2 130.46(13) 2_665 . ? C3 Pr1 C2 29.43(12) . . ? C3 Pr1 C2 150.37(12) 2_665 . ? C1 Pr1 C2 29.54(12) 2_665 2_665 ? C1 Pr1 C2 150.06(13) . 2_665 ? C4 Pr1 C2 130.46(13) . 2_665 ? C4 Pr1 C2 49.07(14) 2_665 2_665 ? C3 Pr1 C2 150.37(12) . 2_665 ? C3 Pr1 C2 29.43(12) 2_665 2_665 ? C2 Pr1 C2 179.45(18) . 2_665 ? C1 Pr1 C5 29.56(14) 2_665 2_665 ? C1 Pr1 C5 109.59(15) . 2_665 ? C4 Pr1 C5 84.83(14) . 2_665 ? C4 Pr1 C5 29.13(14) 2_665 2_665 ? C3 Pr1 C5 113.31(14) . 2_665 ? C3 Pr1 C5 48.43(14) 2_665 2_665 ? C2 Pr1 C5 130.83(14) . 2_665 ? C2 Pr1 C5 48.62(14) 2_665 2_665 ? C1 Pr1 C5 109.59(15) 2_665 . ? C1 Pr1 C5 29.56(14) . . ? C4 Pr1 C5 29.13(14) . . ? C4 Pr1 C5 84.83(14) 2_665 . ? C3 Pr1 C5 48.43(14) . . ? C3 Pr1 C5 113.31(14) 2_665 . ? C2 Pr1 C5 48.62(14) . . ? C2 Pr1 C5 130.83(14) 2_665 . ? C5 Pr1 C5 83.2(2) 2_665 . ? C1 Pr1 S1 130.70(10) 2_665 . ? C1 Pr1 S1 87.55(10) . . ? C4 Pr1 S1 127.09(10) . . ? C4 Pr1 S1 119.70(10) 2_665 . ? C3 Pr1 S1 100.89(9) . . ? C3 Pr1 S1 96.69(10) 2_665 . ? C2 Pr1 S1 78.08(9) . . ? C2 Pr1 S1 102.40(9) 2_665 . ? C5 Pr1 S1 145.11(10) 2_665 . ? C5 Pr1 S1 117.07(11) . . ? C1 Pr1 S1 87.55(10) 2_665 2_665 ? C1 Pr1 S1 130.70(10) . 2_665 ? C4 Pr1 S1 119.70(10) . 2_665 ? C4 Pr1 S1 127.09(10) 2_665 2_665 ? C3 Pr1 S1 96.69(10) . 2_665 ? C3 Pr1 S1 100.89(9) 2_665 2_665 ? C2 Pr1 S1 102.40(9) . 2_665 ? C2 Pr1 S1 78.08(9) 2_665 2_665 ? C5 Pr1 S1 117.07(11) 2_665 2_665 ? C5 Pr1 S1 145.11(10) . 2_665 ? S1 Pr1 S1 63.00(5) . 2_665 ? C14 Pr2 C14 138.45(19) 2_665 . ? C14 Pr2 C12 122.70(13) 2_665 . ? C14 Pr2 C12 48.62(13) . . ? C14 Pr2 C12 48.62(13) 2_665 2_665 ? C14 Pr2 C12 122.70(13) . 2_665 ? C12 Pr2 C12 160.39(19) . 2_665 ? C14 Pr2 C11 102.18(14) 2_665 . ? C14 Pr2 C11 48.69(14) . . ? C12 Pr2 C11 29.66(13) . . ? C12 Pr2 C11 130.79(14) 2_665 . ? C14 Pr2 C11 48.69(14) 2_665 2_665 ? C14 Pr2 C11 102.18(14) . 2_665 ? C12 Pr2 C11 130.79(14) . 2_665 ? C12 Pr2 C11 29.66(13) 2_665 2_665 ? C11 Pr2 C11 101.44(19) . 2_665 ? C14 Pr2 C13 29.30(13) 2_665 2_665 ? C14 Pr2 C13 150.33(13) . 2_665 ? C12 Pr2 C13 150.47(12) . 2_665 ? C12 Pr2 C13 29.35(12) 2_665 2_665 ? C11 Pr2 C13 131.04(13) . 2_665 ? C11 Pr2 C13 48.53(13) 2_665 2_665 ? C14 Pr2 C13 150.33(13) 2_665 . ? C14 Pr2 C13 29.30(13) . . ? C12 Pr2 C13 29.35(12) . . ? C12 Pr2 C13 150.47(12) 2_665 . ? C11 Pr2 C13 48.53(13) . . ? C11 Pr2 C13 131.04(13) 2_665 . ? C13 Pr2 C13 179.49(18) 2_665 . ? C14 Pr2 C15 29.27(13) 2_665 2_665 ? C14 Pr2 C15 110.19(14) . 2_665 ? C12 Pr2 C15 113.98(13) . 2_665 ? C12 Pr2 C15 48.73(13) 2_665 2_665 ? C11 Pr2 C15 85.85(13) . 2_665 ? C11 Pr2 C15 29.67(13) 2_665 2_665 ? C13 Pr2 C15 48.28(13) 2_665 2_665 ? C13 Pr2 C15 131.21(13) . 2_665 ? C14 Pr2 C15 110.19(14) 2_665 . ? C14 Pr2 C15 29.27(13) . . ? C12 Pr2 C15 48.73(13) . . ? C12 Pr2 C15 113.98(13) 2_665 . ? C11 Pr2 C15 29.67(13) . . ? C11 Pr2 C15 85.85(13) 2_665 . ? C13 Pr2 C15 131.21(13) 2_665 . ? C13 Pr2 C15 48.28(13) . . ? C15 Pr2 C15 83.96(18) 2_665 . ? C14 Pr2 S1 126.33(10) 2_665 2_665 ? C14 Pr2 S1 90.64(10) . 2_665 ? C12 Pr2 S1 105.16(9) . 2_665 ? C12 Pr2 S1 91.63(10) 2_665 2_665 ? C11 Pr2 S1 130.97(10) . 2_665 ? C11 Pr2 S1 114.96(9) 2_665 2_665 ? C13 Pr2 S1 97.97(9) 2_665 2_665 ? C13 Pr2 S1 82.47(9) . 2_665 ? C15 Pr2 S1 140.35(10) 2_665 2_665 ? C15 Pr2 S1 119.69(9) . 2_665 ? C14 Pr2 S1 90.64(10) 2_665 . ? C14 Pr2 S1 126.33(10) . . ? C12 Pr2 S1 91.63(10) . . ? C12 Pr2 S1 105.16(9) 2_665 . ? C11 Pr2 S1 114.96(9) . . ? C11 Pr2 S1 130.97(10) 2_665 . ? C13 Pr2 S1 82.47(9) 2_665 . ? C13 Pr2 S1 97.97(9) . . ? C15 Pr2 S1 119.69(9) 2_665 . ? C15 Pr2 S1 140.35(10) . . ? S1 Pr2 S1 63.35(5) 2_665 . ? C21 S1 Pr2 121.36(18) . . ? C21 S1 Pr1 119.92(18) . . ? Pr2 S1 Pr1 116.83(3) . . ? C2 C1 C5 108.6(4) . . ? C2 C1 C6 125.1(5) . . ? C5 C1 C6 126.0(4) . . ? C2 C1 Pr1 76.6(3) . . ? C5 C1 Pr1 76.6(3) . . ? C6 C1 Pr1 118.2(3) . . ? C1 C2 C3 107.3(4) . . ? C1 C2 C7 126.8(4) . . ? C3 C2 C7 125.3(4) . . ? C1 C2 Pr1 73.9(3) . . ? C3 C2 Pr1 75.0(2) . . ? C7 C2 Pr1 123.5(3) . . ? C2 C3 C4 108.1(4) . . ? C2 C3 C8 125.2(4) . . ? C4 C3 C8 126.3(4) . . ? C2 C3 Pr1 75.5(2) . . ? C4 C3 Pr1 74.5(2) . . ? C8 C3 Pr1 121.9(3) . . ? C5 C4 C3 107.6(4) . . ? C5 C4 C9 128.0(4) . . ? C3 C4 C9 123.4(4) . . ? C5 C4 Pr1 76.3(2) . . ? C3 C4 Pr1 75.6(2) . . ? C9 C4 Pr1 123.4(3) . . ? C4 C5 C1 108.4(4) . . ? C4 C5 C10 127.2(5) . . ? C1 C5 C10 123.3(5) . . ? C4 C5 Pr1 74.5(2) . . ? C1 C5 Pr1 73.8(3) . . ? C10 C5 Pr1 127.5(3) . . ? C12 C11 C15 107.5(4) . . ? C12 C11 C16 124.4(4) . . ? C15 C11 C16 127.2(4) . . ? C12 C11 Pr2 75.0(2) . . ? C15 C11 Pr2 75.7(2) . . ? C16 C11 Pr2 123.5(3) . . ? C13 C12 C11 107.8(4) . . ? C13 C12 C17 127.2(4) . . ? C11 C12 C17 124.7(4) . . ? C13 C12 Pr2 75.7(2) . . ? C11 C12 Pr2 75.3(2) . . ? C17 C12 Pr2 120.3(3) . . ? C14 C13 C12 108.3(4) . . ? C14 C13 C18 125.7(4) . . ? C12 C13 C18 125.7(4) . . ? C14 C13 Pr2 74.3(2) . . ? C12 C13 Pr2 75.0(2) . . ? C18 C13 Pr2 122.2(3) . . ? C13 C14 C15 108.8(4) . . ? C13 C14 C19 125.3(4) . . ? C15 C14 C19 125.4(4) . . ? C13 C14 Pr2 76.4(2) . . ? C15 C14 Pr2 76.8(2) . . ? C19 C14 Pr2 119.2(3) . . ? C14 C15 C11 107.5(4) . . ? C14 C15 C20 126.2(4) . . ? C11 C15 C20 125.4(4) . . ? C14 C15 Pr2 74.0(2) . . ? C11 C15 Pr2 74.6(2) . . ? C20 C15 Pr2 125.5(3) . . ? C26 C21 C22 118.2(4) . . ? C26 C21 S1 121.0(3) . . ? C22 C21 S1 120.7(3) . . ? C23 C22 C21 120.6(4) . . ? C22 C23 C24 120.9(5) . . ? C25 C24 C23 118.8(4) . . ? C24 C25 C26 121.5(5) . . ? C21 C26 C25 119.9(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.663 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.128