# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Zhaomin Hou' _publ_contact_author_address ; Organometallic Chemistry Laboratory RIKEN Institute Hirosawa 2-1 Wako Saitama 351-0198 JAPAN ; _publ_contact_author_email HOUZ@RIKEN.JP _publ_section_title ; Synthesis and Styrene Polymerisation Catalysis of h5- and h1-Pyrrolyl-Ligated Cationic Rare Earth Metal Aminobenzyl Complexes ; loop_ _publ_author_name 'Zhaomin Hou' 'Tomohiro Mashiko' 'Masayoshi Nishiura' data_1 _database_code_depnum_ccdc_archive 'CCDC 659963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common PyrScBz2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H44 N3 Sc' _chemical_formula_weight 491.64 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' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2137(14) _cell_length_b 21.339(3) _cell_length_c 11.5163(14) _cell_angle_alpha 90.00 _cell_angle_beta 92.376(2) _cell_angle_gamma 90.00 _cell_volume 2753.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8016 _exptl_absorpt_correction_T_max 0.9182 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14647 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.56 _reflns_number_total 5662 _reflns_number_gt 4895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+1.1758P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5662 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_restrained_S_all 1.202 _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 Sc1 Sc 0.22747(3) 0.161669(18) 0.47491(3) 0.01970(11) Uani 1 1 d . . . N1 N 0.06342(15) 0.12105(8) 0.59141(15) 0.0215(4) Uani 1 1 d . . . N2 N 0.20753(16) 0.07671(8) 0.32730(16) 0.0252(4) Uani 1 1 d . . . N3 N 0.36962(16) 0.25024(9) 0.47883(16) 0.0279(4) Uani 1 1 d . . . C1 C 0.02789(18) 0.18125(9) 0.56246(17) 0.0204(4) Uani 1 1 d . . . C2 C 0.10456(19) 0.22495(10) 0.61621(18) 0.0233(4) Uani 1 1 d . . . H2 H 0.1012 0.2692 0.6080 0.028 Uiso 1 1 calc R . . C3 C 0.1882(2) 0.19025(10) 0.68543(18) 0.0248(5) Uani 1 1 d . . . H3 H 0.2524 0.2067 0.7325 0.030 Uiso 1 1 calc R . . C4 C 0.15813(19) 0.12687(10) 0.67117(17) 0.0225(4) Uani 1 1 d . . . C5 C -0.09511(18) 0.19240(10) 0.50527(18) 0.0227(4) Uani 1 1 d . . . C6 C -0.1864(2) 0.17086(12) 0.5935(2) 0.0335(5) Uani 1 1 d . . . H6A H -0.1762 0.1260 0.6087 0.050 Uiso 1 1 calc R . . H6B H -0.2674 0.1787 0.5617 0.050 Uiso 1 1 calc R . . H6C H -0.1736 0.1942 0.6662 0.050 Uiso 1 1 calc R . . C7 C -0.1149(2) 0.26190(11) 0.4792(2) 0.0342(5) Uani 1 1 d . . . H7A H -0.1062 0.2860 0.5515 0.051 Uiso 1 1 calc R . . H7B H -0.1954 0.2680 0.4445 0.051 Uiso 1 1 calc R . . H7C H -0.0558 0.2763 0.4247 0.051 Uiso 1 1 calc R . . C8 C -0.1164(2) 0.15406(12) 0.3941(2) 0.0328(5) Uani 1 1 d . . . H8A H -0.0645 0.1696 0.3340 0.049 Uiso 1 1 calc R . . H8B H -0.2001 0.1582 0.3670 0.049 Uiso 1 1 calc R . . H8C H -0.0984 0.1099 0.4101 0.049 Uiso 1 1 calc R . . C9 C 0.19487(19) 0.07286(10) 0.75149(19) 0.0253(5) Uani 1 1 d . . . C10 C 0.1109(3) 0.07705(13) 0.8542(2) 0.0420(6) Uani 1 1 d . . . H10A H 0.1243 0.1168 0.8953 0.063 Uiso 1 1 calc R . . H10B H 0.1273 0.0421 0.9078 0.063 Uiso 1 1 calc R . . H10C H 0.0277 0.0749 0.8247 0.063 Uiso 1 1 calc R . . C11 C 0.3243(2) 0.07917(11) 0.7983(2) 0.0351(6) Uani 1 1 d . . . H11A H 0.3782 0.0765 0.7337 0.053 Uiso 1 1 calc R . . H11B H 0.3425 0.0453 0.8537 0.053 Uiso 1 1 calc R . . H11C H 0.3348 0.1197 0.8374 0.053 Uiso 1 1 calc R . . C12 C 0.1758(2) 0.00921(10) 0.6934(2) 0.0307(5) Uani 1 1 d . . . H12A H 0.0957 0.0076 0.6561 0.046 Uiso 1 1 calc R . . H12B H 0.1839 -0.0240 0.7520 0.046 Uiso 1 1 calc R . . H12C H 0.2356 0.0031 0.6347 0.046 Uiso 1 1 calc R . . C13 C 0.3911(2) 0.09779(11) 0.4953(2) 0.0296(5) Uani 1 1 d . . . H13A H 0.4572 0.1185 0.5401 0.036 Uiso 1 1 calc R . . H13B H 0.3714 0.0577 0.5334 0.036 Uiso 1 1 calc R . . C14 C 0.4212(2) 0.08806(10) 0.3719(2) 0.0281(5) Uani 1 1 d . . . C15 C 0.32936(19) 0.08080(10) 0.2855(2) 0.0255(5) Uani 1 1 d . . . C16 C 0.3542(2) 0.07947(10) 0.1683(2) 0.0313(5) Uani 1 1 d . . . H16 H 0.2909 0.0746 0.1115 0.038 Uiso 1 1 calc R . . C17 C 0.4709(2) 0.08518(12) 0.1336(2) 0.0393(6) Uani 1 1 d . . . H17 H 0.4873 0.0849 0.0534 0.047 Uiso 1 1 calc R . . C18 C 0.5625(2) 0.09122(12) 0.2160(2) 0.0401(6) Uani 1 1 d . . . H18 H 0.6425 0.0947 0.1929 0.048 Uiso 1 1 calc R . . C19 C 0.5378(2) 0.09216(12) 0.3327(2) 0.0367(6) Uani 1 1 d . . . H19 H 0.6023 0.0957 0.3885 0.044 Uiso 1 1 calc R . . C20 C 0.1871(2) 0.01257(11) 0.3760(2) 0.0346(5) Uani 1 1 d . . . H20A H 0.1791 -0.0178 0.3123 0.052 Uiso 1 1 calc R . . H20B H 0.1139 0.0127 0.4197 0.052 Uiso 1 1 calc R . . H20C H 0.2549 0.0009 0.4279 0.052 Uiso 1 1 calc R . . C21 C 0.1150(2) 0.08628(11) 0.2340(2) 0.0319(5) Uani 1 1 d . . . H21A H 0.1267 0.1272 0.1975 0.048 Uiso 1 1 calc R . . H21B H 0.0359 0.0849 0.2670 0.048 Uiso 1 1 calc R . . H21C H 0.1211 0.0532 0.1756 0.048 Uiso 1 1 calc R . . C22 C 0.17923(19) 0.22749(9) 0.32368(18) 0.0233(4) Uani 1 1 d . . . H22A H 0.2284 0.2178 0.2566 0.028 Uiso 1 1 calc R . . H22B H 0.0941 0.2224 0.2992 0.028 Uiso 1 1 calc R . . C23 C 0.20240(18) 0.29289(10) 0.36428(17) 0.0224(4) Uani 1 1 d . . . C24 C 0.29696(19) 0.30478(10) 0.44439(19) 0.0252(5) Uani 1 1 d . . . C25 C 0.3210(2) 0.36499(11) 0.4858(2) 0.0335(5) Uani 1 1 d . . . H25 H 0.3864 0.3721 0.5393 0.040 Uiso 1 1 calc R . . C26 C 0.2489(2) 0.41465(11) 0.4484(2) 0.0386(6) Uani 1 1 d . . . H26 H 0.2648 0.4558 0.4767 0.046 Uiso 1 1 calc R . . C27 C 0.1548(2) 0.40447(11) 0.3709(2) 0.0342(5) Uani 1 1 d . . . H27 H 0.1056 0.4385 0.3456 0.041 Uiso 1 1 calc R . . C28 C 0.1316(2) 0.34450(10) 0.3294(2) 0.0278(5) Uani 1 1 d . . . H28 H 0.0660 0.3381 0.2759 0.033 Uiso 1 1 calc R . . C29 C 0.4336(2) 0.25876(13) 0.5925(2) 0.0444(7) Uani 1 1 d . . . H29A H 0.4979 0.2894 0.5848 0.067 Uiso 1 1 calc R . . H29B H 0.4676 0.2186 0.6187 0.067 Uiso 1 1 calc R . . H29C H 0.3778 0.2739 0.6495 0.067 Uiso 1 1 calc R . . C30 C 0.4619(2) 0.24091(12) 0.3910(2) 0.0352(6) Uani 1 1 d . . . H30A H 0.4229 0.2307 0.3157 0.053 Uiso 1 1 calc R . . H30B H 0.5150 0.2065 0.4157 0.053 Uiso 1 1 calc R . . H30C H 0.5086 0.2794 0.3838 0.053 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 Sc1 0.0218(2) 0.0179(2) 0.0194(2) 0.00034(15) 0.00034(14) -0.00157(15) N1 0.0237(9) 0.0177(9) 0.0233(9) 0.0005(7) 0.0031(7) -0.0001(7) N2 0.0257(9) 0.0202(9) 0.0299(10) -0.0033(7) 0.0039(8) -0.0012(7) N3 0.0298(10) 0.0269(10) 0.0265(10) 0.0023(8) -0.0059(8) -0.0072(8) C1 0.0263(10) 0.0160(10) 0.0191(10) 0.0008(7) 0.0046(8) 0.0014(8) C2 0.0318(11) 0.0152(10) 0.0233(11) -0.0011(8) 0.0048(9) 0.0002(8) C3 0.0293(11) 0.0242(11) 0.0209(10) -0.0011(8) -0.0010(9) -0.0026(9) C4 0.0252(10) 0.0224(11) 0.0199(10) 0.0017(8) 0.0006(8) 0.0007(8) C5 0.0232(10) 0.0199(11) 0.0252(11) 0.0013(8) 0.0035(8) 0.0017(8) C6 0.0278(12) 0.0360(14) 0.0374(13) 0.0036(10) 0.0091(10) 0.0025(10) C7 0.0321(12) 0.0264(12) 0.0437(14) 0.0071(10) -0.0019(11) 0.0049(10) C8 0.0276(11) 0.0398(14) 0.0307(12) -0.0050(10) -0.0011(9) -0.0005(10) C9 0.0292(11) 0.0223(11) 0.0243(11) 0.0044(8) -0.0005(9) 0.0016(9) C10 0.0528(16) 0.0399(15) 0.0342(14) 0.0139(11) 0.0112(12) 0.0129(12) C11 0.0395(13) 0.0301(13) 0.0346(13) 0.0045(10) -0.0122(11) 0.0006(10) C12 0.0334(12) 0.0217(11) 0.0366(13) 0.0059(9) -0.0050(10) -0.0015(9) C13 0.0274(11) 0.0300(12) 0.0312(12) 0.0013(9) -0.0017(9) 0.0011(9) C14 0.0277(11) 0.0212(11) 0.0357(13) 0.0028(9) 0.0057(9) 0.0061(9) C15 0.0267(11) 0.0155(10) 0.0346(12) -0.0004(8) 0.0057(9) 0.0033(8) C16 0.0369(13) 0.0250(12) 0.0322(12) -0.0020(9) 0.0062(10) 0.0032(10) C17 0.0481(15) 0.0325(14) 0.0386(14) 0.0037(11) 0.0188(12) 0.0093(11) C18 0.0309(13) 0.0362(14) 0.0545(17) 0.0058(12) 0.0170(12) 0.0069(11) C19 0.0293(12) 0.0317(13) 0.0491(15) 0.0019(11) 0.0040(11) 0.0067(10) C20 0.0429(14) 0.0239(12) 0.0374(14) -0.0021(10) 0.0061(11) -0.0080(10) C21 0.0311(12) 0.0314(13) 0.0330(13) -0.0077(10) -0.0021(10) -0.0017(10) C22 0.0278(11) 0.0212(11) 0.0207(10) 0.0002(8) -0.0021(9) -0.0038(8) C23 0.0261(10) 0.0222(11) 0.0194(10) 0.0020(8) 0.0059(8) -0.0043(8) C24 0.0289(11) 0.0228(11) 0.0243(11) 0.0017(8) 0.0055(9) -0.0058(9) C25 0.0398(13) 0.0288(13) 0.0323(13) -0.0061(10) 0.0045(11) -0.0146(10) C26 0.0490(15) 0.0227(12) 0.0450(15) -0.0075(10) 0.0148(12) -0.0089(11) C27 0.0376(13) 0.0233(12) 0.0427(14) 0.0035(10) 0.0124(11) 0.0020(10) C28 0.0303(11) 0.0256(12) 0.0281(11) 0.0035(9) 0.0055(9) -0.0021(9) C29 0.0531(16) 0.0403(15) 0.0379(14) 0.0087(11) -0.0216(13) -0.0209(13) C30 0.0272(12) 0.0309(13) 0.0475(15) 0.0055(11) 0.0030(11) -0.0031(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 C22 2.285(2) . ? Sc1 C13 2.290(2) . ? Sc1 N3 2.4717(18) . ? Sc1 N1 2.4780(18) . ? Sc1 N2 2.4889(18) . ? Sc1 C1 2.527(2) . ? Sc1 C4 2.532(2) . ? Sc1 C3 2.556(2) . ? Sc1 C2 2.561(2) . ? N1 C4 1.381(3) . ? N1 C1 1.382(3) . ? N2 C15 1.470(3) . ? N2 C21 1.476(3) . ? N2 C20 1.500(3) . ? N3 C24 1.466(3) . ? N3 C29 1.478(3) . ? N3 C30 1.490(3) . ? C1 C2 1.396(3) . ? C1 C5 1.522(3) . ? C2 C3 1.415(3) . ? C3 C4 1.402(3) . ? C4 C9 1.524(3) . ? C5 C7 1.528(3) . ? C5 C8 1.530(3) . ? C5 C6 1.542(3) . ? C9 C12 1.525(3) . ? C9 C11 1.533(3) . ? C9 C10 1.545(3) . ? C13 C14 1.489(3) . ? C14 C19 1.404(3) . ? C14 C15 1.411(3) . ? C15 C16 1.390(3) . ? C16 C17 1.389(3) . ? C17 C18 1.375(4) . ? C18 C19 1.383(4) . ? C22 C23 1.491(3) . ? C23 C24 1.400(3) . ? C23 C28 1.406(3) . ? C24 C25 1.393(3) . ? C25 C26 1.391(4) . ? C26 C27 1.371(4) . ? C27 C28 1.387(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 C22 Sc1 C13 127.40(8) . . ? C22 Sc1 N3 71.09(7) . . ? C13 Sc1 N3 86.55(8) . . ? C22 Sc1 N1 118.04(7) . . ? C13 Sc1 N1 110.25(7) . . ? N3 Sc1 N1 138.62(6) . . ? C22 Sc1 N2 85.15(7) . . ? C13 Sc1 N2 71.66(7) . . ? N3 Sc1 N2 127.52(6) . . ? N1 Sc1 N2 93.86(6) . . ? C22 Sc1 C1 90.97(7) . . ? C13 Sc1 C1 140.95(8) . . ? N3 Sc1 C1 116.58(7) . . ? N1 Sc1 C1 32.03(6) . . ? N2 Sc1 C1 109.69(6) . . ? C22 Sc1 C4 142.09(7) . . ? C13 Sc1 C4 90.49(8) . . ? N3 Sc1 C4 115.45(7) . . ? N1 Sc1 C4 31.97(6) . . ? N2 Sc1 C4 111.95(7) . . ? C1 Sc1 C4 51.87(7) . . ? C22 Sc1 C3 122.12(7) . . ? C13 Sc1 C3 102.33(8) . . ? N3 Sc1 C3 86.36(7) . . ? N1 Sc1 C3 53.77(6) . . ? N2 Sc1 C3 143.86(7) . . ? C1 Sc1 C3 52.55(7) . . ? C4 Sc1 C3 31.98(7) . . ? C22 Sc1 C2 92.49(7) . . ? C13 Sc1 C2 134.34(8) . . ? N3 Sc1 C2 87.07(7) . . ? N1 Sc1 C2 53.79(6) . . ? N2 Sc1 C2 141.50(7) . . ? C1 Sc1 C2 31.83(7) . . ? C4 Sc1 C2 52.70(7) . . ? C3 Sc1 C2 32.11(7) . . ? C4 N1 C1 106.44(17) . . ? C4 N1 Sc1 76.16(11) . . ? C1 N1 Sc1 75.95(11) . . ? C15 N2 C21 112.82(18) . . ? C15 N2 C20 109.58(17) . . ? C21 N2 C20 106.54(17) . . ? C15 N2 Sc1 97.01(12) . . ? C21 N2 Sc1 115.90(13) . . ? C20 N2 Sc1 114.83(14) . . ? C24 N3 C29 112.70(19) . . ? C24 N3 C30 108.43(17) . . ? C29 N3 C30 107.01(19) . . ? C24 N3 Sc1 104.56(12) . . ? C29 N3 Sc1 113.53(14) . . ? C30 N3 Sc1 110.55(14) . . ? N1 C1 C2 110.37(18) . . ? N1 C1 C5 119.79(17) . . ? C2 C1 C5 128.16(18) . . ? N1 C1 Sc1 72.02(11) . . ? C2 C1 Sc1 75.40(12) . . ? C5 C1 Sc1 130.90(14) . . ? C1 C2 C3 106.37(18) . . ? C1 C2 Sc1 72.76(12) . . ? C3 C2 Sc1 73.75(12) . . ? C4 C3 C2 106.75(18) . . ? C4 C3 Sc1 73.07(12) . . ? C2 C3 Sc1 74.14(12) . . ? N1 C4 C3 109.86(18) . . ? N1 C4 C9 121.12(18) . . ? C3 C4 C9 126.93(19) . . ? N1 C4 Sc1 71.87(11) . . ? C3 C4 Sc1 74.95(12) . . ? C9 C4 Sc1 132.72(15) . . ? C1 C5 C7 111.01(17) . . ? C1 C5 C8 112.70(18) . . ? C7 C5 C8 109.77(19) . . ? C1 C5 C6 106.42(17) . . ? C7 C5 C6 108.90(18) . . ? C8 C5 C6 107.87(18) . . ? C4 C9 C12 112.18(18) . . ? C4 C9 C11 112.04(18) . . ? C12 C9 C11 110.24(18) . . ? C4 C9 C10 105.24(18) . . ? C12 C9 C10 107.98(19) . . ? C11 C9 C10 108.9(2) . . ? C14 C13 Sc1 101.39(14) . . ? C19 C14 C15 116.3(2) . . ? C19 C14 C13 123.3(2) . . ? C15 C14 C13 120.1(2) . . ? C16 C15 C14 121.2(2) . . ? C16 C15 N2 122.9(2) . . ? C14 C15 N2 115.91(19) . . ? C17 C16 C15 120.4(2) . . ? C18 C17 C16 119.7(2) . . ? C17 C18 C19 119.9(2) . . ? C18 C19 C14 122.5(2) . . ? C23 C22 Sc1 107.68(13) . . ? C24 C23 C28 116.70(19) . . ? C24 C23 C22 119.58(19) . . ? C28 C23 C22 123.68(19) . . ? C25 C24 C23 121.6(2) . . ? C25 C24 N3 122.8(2) . . ? C23 C24 N3 115.58(18) . . ? C26 C25 C24 119.7(2) . . ? C27 C26 C25 120.2(2) . . ? C26 C27 C28 119.9(2) . . ? C27 C28 C23 121.9(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.56 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.274 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.052 # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 659964' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common PyrLaBz2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H44 La N3' _chemical_formula_weight 585.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.643(4) _cell_length_b 28.397(10) _cell_length_c 17.549(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.699(4) _cell_angle_gamma 90.00 _cell_volume 5802(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 1.494 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5222 _exptl_absorpt_correction_T_max 0.6629 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29800 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.11 _reflns_number_total 10248 _reflns_number_gt 6281 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10248 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.42363(3) 0.371099(14) 0.63745(2) 0.04112(12) Uani 1 1 d . . . La2 La 0.08164(3) 0.634724(14) 0.89103(2) 0.04110(12) Uani 1 1 d . . . N1 N 0.2934(5) 0.4496(2) 0.6139(3) 0.0533(15) Uani 1 1 d . . . N2 N 0.3859(5) 0.2922(2) 0.5555(3) 0.0576(16) Uani 1 1 d . . . N3 N 0.5894(5) 0.4139(2) 0.7304(3) 0.0536(16) Uani 1 1 d . . . N4 N 0.2210(5) 0.5585(2) 0.8760(3) 0.0484(14) Uani 1 1 d . . . N5 N 0.1122(5) 0.7114(2) 0.8063(3) 0.0564(16) Uani 1 1 d . . . N6 N -0.0807(5) 0.5947(3) 0.9845(3) 0.072(2) Uani 1 1 d . . . C1 C 0.4521(6) 0.4108(3) 0.5104(4) 0.061(2) Uani 1 1 d . . . H1A H 0.4878 0.4423 0.5152 0.073 Uiso 1 1 d R . . H1B H 0.4957 0.3911 0.4742 0.073 Uiso 1 1 d R . . C2 C 0.3315(6) 0.4129(2) 0.4922(3) 0.0478(17) Uani 1 1 d . . . C3 C 0.2500(6) 0.4300(2) 0.5434(4) 0.0462(17) Uani 1 1 d . . . C4 C 0.1341(7) 0.4286(3) 0.5261(4) 0.071(2) Uani 1 1 d . . . H4 H 0.0811 0.4412 0.5614 0.085 Uiso 1 1 d R . . C5 C 0.0941(8) 0.4098(4) 0.4599(5) 0.087(3) Uani 1 1 d . . . H5 H 0.0140 0.4099 0.4488 0.104 Uiso 1 1 d R . . C6 C 0.1687(9) 0.3907(3) 0.4093(5) 0.089(3) Uani 1 1 d . . . H6 H 0.1412 0.3765 0.3635 0.106 Uiso 1 1 d R . . C7 C 0.2847(7) 0.3923(3) 0.4256(4) 0.067(2) Uani 1 1 d . . . H7 H 0.3359 0.3788 0.3900 0.080 Uiso 1 1 d R . . C8 C 0.3456(8) 0.4962(3) 0.6038(4) 0.090(3) Uani 1 1 d . . . H8A H 0.4024 0.4948 0.5631 0.135 Uiso 1 1 d R . . H8B H 0.3834 0.5059 0.6515 0.135 Uiso 1 1 d R . . H8C H 0.2858 0.5191 0.5902 0.135 Uiso 1 1 d R . . C9 C 0.2053(7) 0.4527(3) 0.6734(4) 0.086(3) Uani 1 1 d . . . H9A H 0.1443 0.4743 0.6568 0.129 Uiso 1 1 d R . . H9B H 0.2405 0.4644 0.7207 0.129 Uiso 1 1 d R . . H9C H 0.1726 0.4214 0.6823 0.129 Uiso 1 1 d R . . C10 C 0.2257(5) 0.3280(2) 0.6635(4) 0.0517(18) Uani 1 1 d . . . H10A H 0.1840 0.3401 0.7083 0.062 Uiso 1 1 d R . . H10B H 0.1745 0.3254 0.6183 0.062 Uiso 1 1 d R . . C11 C 0.2946(6) 0.2867(3) 0.6785(4) 0.0519(18) Uani 1 1 d . . . C12 C 0.3792(6) 0.2696(3) 0.6301(4) 0.0538(18) Uani 1 1 d . . . C13 C 0.4521(7) 0.2327(3) 0.6491(6) 0.080(3) Uani 1 1 d . . . H13 H 0.5078 0.2222 0.6139 0.096 Uiso 1 1 d R . . C14 C 0.4432(9) 0.2118(4) 0.7189(8) 0.113(4) Uani 1 1 d . . . H14 H 0.4915 0.1860 0.7324 0.135 Uiso 1 1 d R . . C15 C 0.3643(10) 0.2281(4) 0.7690(6) 0.105(3) Uani 1 1 d . . . H15 H 0.3598 0.2143 0.8182 0.125 Uiso 1 1 d R . . C16 C 0.2914(7) 0.2641(3) 0.7498(5) 0.072(2) Uani 1 1 d . . . H16 H 0.2366 0.2742 0.7859 0.086 Uiso 1 1 d R . . C17 C 0.4943(7) 0.2850(3) 0.5160(5) 0.083(3) Uani 1 1 d . . . H17A H 0.5585 0.2931 0.5503 0.125 Uiso 1 1 d R . . H17B H 0.4965 0.3052 0.4708 0.125 Uiso 1 1 d R . . H17C H 0.5008 0.2520 0.5006 0.125 Uiso 1 1 d R . . C18 C 0.2910(6) 0.2784(3) 0.5056(4) 0.074(2) Uani 1 1 d . . . H18A H 0.3060 0.2471 0.4846 0.111 Uiso 1 1 d R . . H18B H 0.2832 0.3012 0.4640 0.111 Uiso 1 1 d R . . H18C H 0.2198 0.2777 0.5348 0.111 Uiso 1 1 d R . . C19 C 0.6555(5) 0.3980(3) 0.6733(4) 0.0497(18) Uani 1 1 d . . . C20 C 0.6603(6) 0.3486(3) 0.6748(4) 0.061(2) Uani 1 1 d . . . H20 H 0.6990 0.3286 0.6399 0.073 Uiso 1 1 d R . . C21 C 0.5962(6) 0.3346(3) 0.7384(4) 0.060(2) Uani 1 1 d . . . H21 H 0.5843 0.3034 0.7562 0.071 Uiso 1 1 d R . . C22 C 0.5538(6) 0.3761(3) 0.7698(4) 0.0490(18) Uani 1 1 d . . . C23 C 0.7337(6) 0.4300(3) 0.6300(4) 0.057(2) Uani 1 1 d . . . C24 C 0.8467(6) 0.4332(4) 0.6761(5) 0.099(3) Uani 1 1 d . . . H24A H 0.8303 0.4432 0.7283 0.149 Uiso 1 1 d R . . H24B H 0.8979 0.4560 0.6521 0.149 Uiso 1 1 d R . . H24C H 0.8838 0.4022 0.6773 0.149 Uiso 1 1 d R . . C25 C 0.7597(7) 0.4113(3) 0.5507(4) 0.088(3) Uani 1 1 d . . . H25A H 0.7883 0.3789 0.5546 0.132 Uiso 1 1 d R . . H25B H 0.8182 0.4312 0.5270 0.132 Uiso 1 1 d R . . H25C H 0.6895 0.4118 0.5194 0.132 Uiso 1 1 d R . . C26 C 0.6855(7) 0.4795(3) 0.6247(5) 0.081(3) Uani 1 1 d . . . H26A H 0.6182 0.4796 0.5907 0.121 Uiso 1 1 d R . . H26B H 0.7442 0.5007 0.6045 0.121 Uiso 1 1 d R . . H26C H 0.6632 0.4901 0.6755 0.121 Uiso 1 1 d R . . C27 C 0.4897(6) 0.3809(3) 0.8431(4) 0.058(2) Uani 1 1 d . . . C28 C 0.5417(8) 0.4195(4) 0.8901(5) 0.129(5) Uani 1 1 d . . . H28A H 0.5337 0.4495 0.8629 0.193 Uiso 1 1 d R . . H28B H 0.6232 0.4128 0.8992 0.193 Uiso 1 1 d R . . H28C H 0.5020 0.4215 0.9389 0.193 Uiso 1 1 d R . . C29 C 0.4970(10) 0.3370(4) 0.8898(5) 0.149(5) Uani 1 1 d . . . H29A H 0.4540 0.3414 0.9370 0.224 Uiso 1 1 d R . . H29B H 0.5776 0.3303 0.9023 0.224 Uiso 1 1 d R . . H29C H 0.4641 0.3107 0.8609 0.224 Uiso 1 1 d R . . C30 C 0.3663(7) 0.3913(4) 0.8300(5) 0.111(4) Uani 1 1 d . . . H30A H 0.3298 0.3646 0.8037 0.167 Uiso 1 1 d R . . H30B H 0.3586 0.4196 0.7985 0.167 Uiso 1 1 d R . . H30C H 0.3289 0.3964 0.8790 0.167 Uiso 1 1 d R . . C31 C 0.0544(6) 0.5897(3) 0.7661(3) 0.057(2) Uani 1 1 d . . . H31A H 0.0232 0.5576 0.7735 0.069 Uiso 1 1 d R . . H31B H 0.0076 0.6071 0.7280 0.069 Uiso 1 1 d R . . C32 C 0.1744(6) 0.5899(2) 0.7495(3) 0.0490(18) Uani 1 1 d . . . C33 C 0.2614(6) 0.5767(2) 0.8026(3) 0.0493(18) Uani 1 1 d . . . C34 C 0.3750(6) 0.5810(3) 0.7866(4) 0.064(2) Uani 1 1 d . . . H34 H 0.4305 0.5709 0.8232 0.077 Uiso 1 1 d R . . C35 C 0.4113(7) 0.5994(3) 0.7192(5) 0.070(2) Uani 1 1 d . . . H35 H 0.4908 0.6015 0.7081 0.085 Uiso 1 1 d R . . C36 C 0.3296(8) 0.6149(3) 0.6678(5) 0.073(2) Uani 1 1 d . . . H36 H 0.3524 0.6295 0.6217 0.088 Uiso 1 1 d R . . C37 C 0.2168(7) 0.6093(3) 0.6828(4) 0.0562(19) Uani 1 1 d . . . H37 H 0.1629 0.6194 0.6452 0.067 Uiso 1 1 d R . . C38 C 0.1758(7) 0.5107(3) 0.8711(4) 0.072(2) Uani 1 1 d . . . H38A H 0.1276 0.5076 0.8252 0.108 Uiso 1 1 d R . . H38B H 0.1297 0.5040 0.9162 0.108 Uiso 1 1 d R . . H38C H 0.2396 0.4883 0.8687 0.108 Uiso 1 1 d R . . C39 C 0.3110(6) 0.5586(3) 0.9362(4) 0.068(2) Uani 1 1 d . . . H39A H 0.2773 0.5492 0.9848 0.102 Uiso 1 1 d R . . H39B H 0.3436 0.5903 0.9410 0.102 Uiso 1 1 d R . . H39C H 0.3718 0.5363 0.9226 0.102 Uiso 1 1 d R . . C40 C 0.2747(5) 0.6798(2) 0.9168(4) 0.0531(19) Uani 1 1 d . . . H40A H 0.3175 0.6688 0.9625 0.064 Uiso 1 1 d R . . H40B H 0.3254 0.6817 0.8720 0.064 Uiso 1 1 d R . . C41 C 0.2060(6) 0.7217(2) 0.9291(4) 0.0512(18) Uani 1 1 d . . . C42 C 0.1198(6) 0.7366(2) 0.8771(4) 0.0501(18) Uani 1 1 d . . . C43 C 0.0481(7) 0.7740(3) 0.8932(5) 0.075(2) Uani 1 1 d . . . H43 H -0.0076 0.7836 0.8564 0.090 Uiso 1 1 d R . . C44 C 0.0560(9) 0.7971(3) 0.9603(7) 0.099(3) Uani 1 1 d . . . H44 H 0.0053 0.8224 0.9712 0.119 Uiso 1 1 d R . . C45 C 0.1379(9) 0.7837(3) 1.0126(6) 0.091(3) Uani 1 1 d . . . H45 H 0.1437 0.7998 1.0599 0.109 Uiso 1 1 d R . . C46 C 0.2119(7) 0.7472(3) 0.9977(4) 0.068(2) Uani 1 1 d . . . H46 H 0.2686 0.7391 1.0347 0.082 Uiso 1 1 d R . . C47 C 0.0038(7) 0.7163(3) 0.7642(5) 0.085(3) Uani 1 1 d . . . H47A H -0.0601 0.7080 0.7974 0.128 Uiso 1 1 d R . . H47B H 0.0039 0.6953 0.7199 0.128 Uiso 1 1 d R . . H47C H -0.0050 0.7490 0.7470 0.128 Uiso 1 1 d R . . C48 C 0.2069(7) 0.7251(3) 0.7540(4) 0.073(2) Uani 1 1 d . . . H48A H 0.1883 0.7553 0.7298 0.109 Uiso 1 1 d R . . H48B H 0.2157 0.7009 0.7147 0.109 Uiso 1 1 d R . . H48C H 0.2788 0.7281 0.7832 0.109 Uiso 1 1 d R . . C49 C -0.1468(6) 0.6065(3) 0.9279(4) 0.058(2) Uani 1 1 d . . . C50 C -0.1536(7) 0.6575(4) 0.9259(5) 0.088(3) Uani 1 1 d . . . H50 H -0.1938 0.6765 0.8898 0.105 Uiso 1 1 d R . . C51 C -0.0877(7) 0.6730(4) 0.9891(5) 0.088(3) Uani 1 1 d . . . H51 H -0.0762 0.7046 1.0052 0.106 Uiso 1 1 d R . . C52 C -0.0410(6) 0.6308(3) 1.0246(4) 0.058(2) Uani 1 1 d . . . C53 C -0.2281(6) 0.5775(3) 0.8835(4) 0.062(2) Uani 1 1 d . . . C54 C -0.3392(6) 0.5758(4) 0.9298(5) 0.116(4) Uani 1 1 d . . . H54A H -0.3213 0.5657 0.9820 0.174 Uiso 1 1 d R . . H54B H -0.3929 0.5534 0.9062 0.174 Uiso 1 1 d R . . H54C H -0.3742 0.6072 0.9309 0.174 Uiso 1 1 d R . . C55 C -0.1769(8) 0.5275(3) 0.8797(5) 0.108(3) Uani 1 1 d . . . H55A H -0.1302 0.5246 0.8338 0.161 Uiso 1 1 d R . . H55B H -0.2393 0.5043 0.8778 0.161 Uiso 1 1 d R . . H55C H -0.1288 0.5219 0.9249 0.161 Uiso 1 1 d R . . C56 C -0.2551(8) 0.5950(5) 0.8061(5) 0.142(5) Uani 1 1 d . . . H56A H -0.2457 0.6293 0.8049 0.213 Uiso 1 1 d R . . H56B H -0.3346 0.5869 0.7926 0.213 Uiso 1 1 d R . . H56C H -0.2030 0.5805 0.7696 0.213 Uiso 1 1 d R . . C57 C 0.0202(6) 0.6311(3) 1.0970(4) 0.0558(19) Uani 1 1 d . . . C58 C -0.0448(7) 0.6038(4) 1.1541(4) 0.130(5) Uani 1 1 d . . . H58A H -0.0575 0.5718 1.1352 0.195 Uiso 1 1 d R . . H58B H -0.1191 0.6191 1.1628 0.195 Uiso 1 1 d R . . H58C H -0.0009 0.6027 1.2021 0.195 Uiso 1 1 d R . . C59 C 0.0295(15) 0.6784(4) 1.1316(7) 0.206(8) Uani 1 1 d . . . H59A H 0.0023 0.6772 1.1842 0.309 Uiso 1 1 d R . . H59B H -0.0175 0.7007 1.1023 0.309 Uiso 1 1 d R . . H59C H 0.1099 0.6887 1.1314 0.309 Uiso 1 1 d R . . C60 C 0.1364(8) 0.6134(6) 1.0897(5) 0.195(8) Uani 1 1 d . . . H60A H 0.1341 0.5793 1.0809 0.292 Uiso 1 1 d R . . H60B H 0.1799 0.6200 1.1366 0.292 Uiso 1 1 d R . . H60C H 0.1736 0.6288 1.0466 0.292 Uiso 1 1 d 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 0.0359(2) 0.0483(3) 0.0392(2) -0.0019(2) -0.00020(15) -0.00005(19) La2 0.0339(2) 0.0472(3) 0.0423(2) 0.0041(2) 0.00142(15) 0.00016(19) N1 0.065(4) 0.052(4) 0.042(3) -0.002(3) -0.003(3) 0.008(3) N2 0.055(4) 0.059(4) 0.060(4) -0.020(3) 0.015(3) -0.010(3) N3 0.048(4) 0.074(5) 0.039(3) -0.003(3) -0.006(3) -0.003(3) N4 0.053(4) 0.048(4) 0.044(3) -0.004(3) -0.002(3) 0.010(3) N5 0.049(4) 0.057(4) 0.063(4) 0.021(3) -0.006(3) -0.011(3) N6 0.057(4) 0.114(6) 0.044(4) 0.011(4) 0.010(3) -0.039(4) C1 0.060(5) 0.072(6) 0.049(4) 0.007(4) 0.004(4) 0.001(4) C2 0.052(4) 0.058(5) 0.033(4) 0.008(3) 0.004(3) -0.004(4) C3 0.046(4) 0.047(4) 0.045(4) 0.009(3) -0.001(3) -0.003(3) C4 0.064(5) 0.088(7) 0.062(5) 0.014(5) -0.002(4) 0.019(5) C5 0.062(6) 0.130(9) 0.067(6) 0.019(6) -0.026(5) -0.012(6) C6 0.114(9) 0.095(7) 0.055(5) 0.007(5) -0.044(6) -0.024(6) C7 0.078(6) 0.089(6) 0.034(4) -0.001(4) 0.000(4) 0.005(5) C8 0.134(9) 0.058(6) 0.078(6) -0.012(5) -0.024(6) 0.001(6) C9 0.113(7) 0.099(7) 0.045(5) 0.001(5) 0.012(5) 0.050(6) C10 0.045(4) 0.064(5) 0.046(4) -0.017(4) 0.005(3) -0.008(4) C11 0.047(4) 0.050(5) 0.059(5) 0.000(4) 0.006(3) -0.008(4) C12 0.050(4) 0.046(5) 0.066(5) -0.005(4) 0.001(4) -0.005(4) C13 0.063(6) 0.052(6) 0.126(8) -0.001(6) 0.000(5) 0.004(4) C14 0.090(9) 0.068(7) 0.179(13) 0.037(8) -0.014(8) 0.000(6) C15 0.114(9) 0.088(8) 0.112(9) 0.050(7) -0.006(7) -0.012(7) C16 0.063(6) 0.079(6) 0.074(6) 0.013(5) 0.008(4) -0.021(5) C17 0.075(6) 0.080(7) 0.095(6) -0.032(5) 0.029(5) 0.000(5) C18 0.073(6) 0.080(6) 0.068(5) -0.025(5) 0.001(4) -0.004(5) C19 0.038(4) 0.073(6) 0.038(4) -0.003(4) -0.003(3) -0.001(4) C20 0.054(5) 0.073(6) 0.056(5) 0.001(4) 0.008(4) 0.006(4) C21 0.061(5) 0.060(5) 0.058(5) 0.012(4) -0.002(4) 0.014(4) C22 0.045(4) 0.059(5) 0.042(4) 0.002(4) -0.014(3) -0.004(4) C23 0.041(4) 0.079(6) 0.051(5) 0.007(4) -0.001(3) -0.004(4) C24 0.046(5) 0.163(10) 0.088(6) 0.014(6) -0.020(4) -0.024(6) C25 0.061(6) 0.137(9) 0.067(6) 0.002(6) 0.012(4) 0.003(5) C26 0.087(6) 0.067(6) 0.088(6) 0.015(5) -0.015(5) -0.024(5) C27 0.041(4) 0.091(6) 0.043(4) 0.000(4) 0.007(3) 0.006(4) C28 0.096(8) 0.225(14) 0.067(6) -0.058(7) 0.026(5) -0.057(8) C29 0.174(12) 0.181(13) 0.094(8) 0.076(9) 0.060(8) 0.058(10) C30 0.053(6) 0.208(12) 0.073(6) -0.041(7) -0.002(4) 0.029(6) C31 0.052(5) 0.076(6) 0.044(4) 0.007(4) -0.016(3) -0.006(4) C32 0.057(5) 0.058(5) 0.032(4) -0.007(3) 0.002(3) 0.000(4) C33 0.052(5) 0.060(5) 0.035(4) -0.008(3) 0.002(3) -0.004(4) C34 0.040(5) 0.090(6) 0.064(5) -0.023(5) 0.004(4) 0.005(4) C35 0.050(5) 0.084(7) 0.077(6) -0.028(5) 0.022(4) -0.010(5) C36 0.102(8) 0.055(6) 0.062(5) -0.001(4) 0.030(5) -0.003(5) C37 0.067(5) 0.065(5) 0.037(4) -0.001(4) 0.005(3) -0.001(4) C38 0.091(6) 0.061(6) 0.064(5) 0.008(5) 0.009(4) 0.006(5) C39 0.072(6) 0.079(6) 0.052(5) -0.002(4) -0.012(4) 0.031(4) C40 0.036(4) 0.060(5) 0.063(5) 0.013(4) -0.002(3) 0.000(4) C41 0.045(4) 0.046(5) 0.063(5) 0.005(4) 0.002(3) -0.016(4) C42 0.038(4) 0.041(4) 0.071(5) 0.008(4) 0.004(3) 0.000(3) C43 0.061(6) 0.047(5) 0.117(8) 0.005(5) 0.008(5) 0.001(4) C44 0.083(8) 0.051(6) 0.165(11) -0.015(7) 0.030(7) 0.001(5) C45 0.101(8) 0.066(7) 0.105(8) -0.033(6) 0.036(6) -0.020(6) C46 0.068(6) 0.064(6) 0.072(6) -0.009(5) 0.004(4) -0.020(5) C47 0.068(6) 0.095(7) 0.092(6) 0.037(5) -0.038(5) -0.012(5) C48 0.082(6) 0.068(6) 0.068(5) 0.019(4) 0.000(4) -0.010(5) C49 0.039(4) 0.085(6) 0.049(5) 0.008(4) 0.008(3) -0.006(4) C50 0.069(6) 0.109(9) 0.085(7) -0.001(6) -0.005(5) 0.002(6) C51 0.079(7) 0.110(8) 0.076(6) -0.007(6) 0.010(5) 0.006(6) C52 0.049(4) 0.077(6) 0.049(4) 0.001(5) 0.011(3) -0.026(4) C53 0.041(4) 0.097(7) 0.050(5) -0.006(4) 0.001(3) -0.017(4) C54 0.043(5) 0.226(13) 0.080(6) -0.016(7) 0.014(4) -0.041(6) C55 0.110(8) 0.093(8) 0.120(8) -0.028(7) 0.033(6) -0.035(7) C56 0.065(7) 0.294(17) 0.067(6) 0.025(8) 0.002(5) 0.030(8) C57 0.044(4) 0.082(6) 0.041(4) -0.012(4) 0.000(3) -0.007(4) C58 0.070(6) 0.261(14) 0.058(6) 0.058(7) -0.013(4) -0.051(8) C59 0.35(2) 0.134(12) 0.128(11) -0.039(10) -0.001(12) -0.096(14) C60 0.054(6) 0.45(2) 0.075(7) 0.072(11) -0.006(5) 0.067(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 C1 2.524(6) . ? La1 C10 2.654(6) . ? La1 N2 2.695(6) . ? La1 N1 2.724(6) . ? La1 C22 2.761(6) . ? La1 N3 2.790(5) . ? La1 C21 2.856(7) . ? La1 C19 2.869(6) . ? La1 C20 2.896(7) . ? La1 C11 2.922(7) . ? La1 C12 2.932(7) . ? La1 C2 2.997(6) . ? La2 C31 2.554(6) . ? La2 C40 2.621(6) . ? La2 N5 2.662(5) . ? La2 N4 2.720(5) . ? La2 N6 2.762(5) . ? La2 C52 2.762(6) . ? La2 C51 2.849(8) . ? La2 C49 2.860(7) . ? La2 C50 2.888(9) . ? La2 C41 2.936(7) . ? La2 C42 2.937(7) . ? La2 C32 3.004(6) . ? N1 C3 1.443(8) . ? N1 C8 1.470(9) . ? N1 C9 1.476(8) . ? N2 C18 1.455(8) . ? N2 C17 1.461(8) . ? N2 C12 1.463(9) . ? N3 C22 1.347(8) . ? N3 C19 1.348(8) . ? N4 C38 1.459(9) . ? N4 C33 1.470(8) . ? N4 C39 1.479(8) . ? N5 C42 1.436(8) . ? N5 C47 1.462(8) . ? N5 C48 1.495(8) . ? N6 C49 1.294(8) . ? N6 C52 1.322(9) . ? C1 C2 1.438(9) . ? C2 C3 1.401(8) . ? C2 C7 1.412(9) . ? C3 C4 1.380(9) . ? C4 C5 1.356(11) . ? C5 C6 1.362(12) . ? C6 C7 1.377(11) . ? C10 C11 1.443(9) . ? C11 C12 1.396(9) . ? C11 C16 1.408(9) . ? C12 C13 1.384(10) . ? C13 C14 1.368(12) . ? C14 C15 1.360(13) . ? C15 C16 1.366(12) . ? C19 C20 1.405(10) . ? C19 C23 1.499(9) . ? C20 C21 1.408(9) . ? C21 C22 1.393(9) . ? C22 C27 1.502(9) . ? C23 C26 1.514(10) . ? C23 C25 1.524(9) . ? C23 C24 1.539(9) . ? C27 C30 1.483(10) . ? C27 C29 1.492(11) . ? C27 C28 1.495(11) . ? C31 C32 1.431(9) . ? C32 C37 1.390(9) . ? C32 C33 1.418(9) . ? C33 C34 1.361(9) . ? C34 C35 1.365(10) . ? C35 C36 1.374(11) . ? C36 C37 1.351(10) . ? C40 C41 1.452(9) . ? C41 C46 1.406(9) . ? C41 C42 1.414(9) . ? C42 C43 1.382(10) . ? C43 C44 1.351(12) . ? C44 C45 1.370(12) . ? C45 C46 1.373(11) . ? C49 C50 1.451(11) . ? C49 C53 1.471(10) . ? C50 C51 1.411(11) . ? C51 C52 1.453(11) . ? C52 C57 1.448(9) . ? C53 C56 1.476(10) . ? C53 C54 1.537(9) . ? C53 C55 1.541(11) . ? C57 C60 1.451(11) . ? C57 C59 1.477(12) . ? C57 C58 1.483(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 La1 C10 118.8(2) . . ? C1 La1 N2 85.5(2) . . ? C10 La1 N2 64.70(18) . . ? C1 La1 N1 65.2(2) . . ? C10 La1 N1 85.4(2) . . ? N2 La1 N1 120.80(18) . . ? C1 La1 C22 130.1(2) . . ? C10 La1 C22 110.3(2) . . ? N2 La1 C22 125.1(2) . . ? N1 La1 C22 112.64(19) . . ? C1 La1 N3 103.0(2) . . ? C10 La1 N3 134.13(18) . . ? N2 La1 N3 141.35(18) . . ? N1 La1 N3 96.44(18) . . ? C22 La1 N3 28.07(16) . . ? C1 La1 C21 127.6(2) . . ? C10 La1 C21 109.4(2) . . ? N2 La1 C21 97.9(2) . . ? N1 La1 C21 141.0(2) . . ? C22 La1 C21 28.64(19) . . ? N3 La1 C21 47.1(2) . . ? C1 La1 C19 86.6(2) . . ? C10 La1 C19 154.4(2) . . ? N2 La1 C19 119.0(2) . . ? N1 La1 C19 109.6(2) . . ? C22 La1 C19 45.29(19) . . ? N3 La1 C19 27.52(16) . . ? C21 La1 C19 46.2(2) . . ? C1 La1 C20 99.4(2) . . ? C10 La1 C20 133.2(2) . . ? N2 La1 C20 94.9(2) . . ? N1 La1 C20 137.9(2) . . ? C22 La1 C20 46.4(2) . . ? N3 La1 C20 46.7(2) . . ? C21 La1 C20 28.32(18) . . ? C19 La1 C20 28.2(2) . . ? C1 La1 C11 131.1(2) . . ? C10 La1 C11 29.49(19) . . ? N2 La1 C11 50.90(19) . . ? N1 La1 C11 114.9(2) . . ? C22 La1 C11 96.5(2) . . ? N3 La1 C11 124.56(19) . . ? C21 La1 C11 84.8(2) . . ? C19 La1 C11 130.5(2) . . ? C20 La1 C11 104.7(2) . . ? C1 La1 C12 115.2(2) . . ? C10 La1 C12 53.2(2) . . ? N2 La1 C12 29.75(17) . . ? N1 La1 C12 134.44(19) . . ? C22 La1 C12 100.5(2) . . ? N3 La1 C12 125.06(19) . . ? C21 La1 C12 78.0(2) . . ? C19 La1 C12 115.9(2) . . ? C20 La1 C12 87.7(2) . . ? C11 La1 C12 27.59(18) . . ? C1 La1 C2 28.57(19) . . ? C10 La1 C2 91.5(2) . . ? N2 La1 C2 79.67(19) . . ? N1 La1 C2 49.80(17) . . ? C22 La1 C2 151.9(2) . . ? N3 La1 C2 124.21(18) . . ? C21 La1 C2 155.8(2) . . ? C19 La1 C2 114.03(19) . . ? C20 La1 C2 127.53(19) . . ? C11 La1 C2 110.73(19) . . ? C12 La1 C2 106.90(19) . . ? C31 La2 C40 119.3(2) . . ? C31 La2 N5 86.9(2) . . ? C40 La2 N5 64.97(19) . . ? C31 La2 N4 65.56(19) . . ? C40 La2 N4 83.89(19) . . ? N5 La2 N4 120.82(18) . . ? C31 La2 N6 103.0(2) . . ? C40 La2 N6 133.6(2) . . ? N5 La2 N6 139.9(2) . . ? N4 La2 N6 98.3(2) . . ? C31 La2 C52 130.4(2) . . ? C40 La2 C52 109.0(2) . . ? N5 La2 C52 125.5(2) . . ? N4 La2 C52 111.4(2) . . ? N6 La2 C52 27.68(18) . . ? C31 La2 C51 129.0(2) . . ? C40 La2 C51 108.0(2) . . ? N5 La2 C51 97.1(2) . . ? N4 La2 C51 141.3(2) . . ? N6 La2 C51 46.7(3) . . ? C52 La2 C51 30.0(2) . . ? C31 La2 C49 87.0(2) . . ? C40 La2 C49 153.6(2) . . ? N5 La2 C49 119.1(2) . . ? N4 La2 C49 110.9(2) . . ? N6 La2 C49 26.54(17) . . ? C52 La2 C49 45.9(2) . . ? C51 La2 C49 47.0(3) . . ? C31 La2 C50 100.7(2) . . ? C40 La2 C50 131.9(3) . . ? N5 La2 C50 93.9(2) . . ? N4 La2 C50 140.2(2) . . ? N6 La2 C50 46.2(2) . . ? C52 La2 C50 47.7(2) . . ? C51 La2 C50 28.5(2) . . ? C49 La2 C50 29.2(2) . . ? C31 La2 C41 132.2(2) . . ? C40 La2 C41 29.60(19) . . ? N5 La2 C41 50.98(19) . . ? N4 La2 C41 113.46(19) . . ? N6 La2 C41 123.3(2) . . ? C52 La2 C41 95.7(2) . . ? C51 La2 C41 83.4(2) . . ? C49 La2 C41 129.9(2) . . ? C50 La2 C41 103.3(3) . . ? C31 La2 C42 116.0(2) . . ? C40 La2 C42 53.38(19) . . ? N5 La2 C42 29.19(17) . . ? N4 La2 C42 133.20(18) . . ? N6 La2 C42 124.0(2) . . ? C52 La2 C42 101.0(2) . . ? C51 La2 C42 77.4(2) . . ? C49 La2 C42 115.9(2) . . ? C50 La2 C42 86.6(2) . . ? C41 La2 C42 27.86(18) . . ? C31 La2 C32 28.38(18) . . ? C40 La2 C32 91.9(2) . . ? N5 La2 C32 80.37(19) . . ? N4 La2 C32 50.32(17) . . ? N6 La2 C32 124.9(2) . . ? C52 La2 C32 151.6(2) . . ? C51 La2 C32 156.9(2) . . ? C49 La2 C32 114.4(2) . . ? C50 La2 C32 128.5(2) . . ? C41 La2 C32 111.30(19) . . ? C42 La2 C32 107.00(19) . . ? C3 N1 C8 112.7(5) . . ? C3 N1 C9 113.1(6) . . ? C8 N1 C9 108.9(6) . . ? C3 N1 La1 90.2(4) . . ? C8 N1 La1 121.7(5) . . ? C9 N1 La1 109.4(4) . . ? C18 N2 C17 109.4(6) . . ? C18 N2 C12 111.8(6) . . ? C17 N2 C12 114.8(6) . . ? C18 N2 La1 131.5(5) . . ? C17 N2 La1 103.4(4) . . ? C12 N2 La1 84.1(4) . . ? C22 N3 C19 107.2(6) . . ? C22 N3 La1 74.7(3) . . ? C19 N3 La1 79.5(4) . . ? C38 N4 C33 113.3(5) . . ? C38 N4 C39 107.2(6) . . ? C33 N4 C39 113.2(6) . . ? C38 N4 La2 122.1(4) . . ? C33 N4 La2 90.2(4) . . ? C39 N4 La2 110.4(4) . . ? C42 N5 C47 115.7(6) . . ? C42 N5 C48 111.3(5) . . ? C47 N5 C48 107.7(6) . . ? C42 N5 La2 86.1(4) . . ? C47 N5 La2 103.9(4) . . ? C48 N5 La2 131.4(5) . . ? C49 N6 C52 114.2(8) . . ? C49 N6 La2 80.9(4) . . ? C52 N6 La2 76.2(4) . . ? C2 C1 La1 94.3(4) . . ? C3 C2 C7 114.6(6) . . ? C3 C2 C1 122.7(6) . . ? C7 C2 C1 122.2(7) . . ? C3 C2 La1 80.3(4) . . ? C7 C2 La1 132.2(5) . . ? C1 C2 La1 57.1(3) . . ? C4 C3 C2 121.2(7) . . ? C4 C3 N1 122.0(6) . . ? C2 C3 N1 116.8(6) . . ? C4 C3 La1 137.3(5) . . ? C2 C3 La1 73.2(4) . . ? N1 C3 La1 62.0(3) . . ? C5 C4 C3 121.6(8) . . ? C4 C5 C6 120.0(8) . . ? C5 C6 C7 118.9(8) . . ? C6 C7 C2 123.6(8) . . ? C11 C10 La1 85.6(4) . . ? C12 C11 C16 114.0(7) . . ? C12 C11 C10 124.7(7) . . ? C16 C11 C10 120.8(7) . . ? C12 C11 La1 76.6(4) . . ? C16 C11 La1 127.8(5) . . ? C10 C11 La1 64.9(4) . . ? C13 C12 C11 123.6(8) . . ? C13 C12 N2 120.6(7) . . ? C11 C12 N2 115.9(6) . . ? C13 C12 La1 128.7(5) . . ? C11 C12 La1 75.8(4) . . ? N2 C12 La1 66.1(3) . . ? C14 C13 C12 119.5(9) . . ? C15 C14 C13 119.2(10) . . ? C14 C15 C16 121.2(10) . . ? C15 C16 C11 122.5(8) . . ? N3 C19 C20 110.1(6) . . ? N3 C19 C23 121.9(7) . . ? C20 C19 C23 126.2(7) . . ? N3 C19 La1 73.0(4) . . ? C20 C19 La1 77.0(4) . . ? C23 C19 La1 128.7(4) . . ? C19 C20 C21 105.9(7) . . ? C19 C20 La1 74.8(4) . . ? C21 C20 La1 74.3(4) . . ? C22 C21 C20 105.6(7) . . ? C22 C21 La1 71.9(4) . . ? C20 C21 La1 77.4(4) . . ? N3 C22 C21 111.0(6) . . ? N3 C22 C27 121.8(7) . . ? C21 C22 C27 126.7(7) . . ? N3 C22 La1 77.2(3) . . ? C21 C22 La1 79.5(4) . . ? C27 C22 La1 116.9(4) . . ? C19 C23 C26 111.5(6) . . ? C19 C23 C25 112.3(7) . . ? C26 C23 C25 110.2(7) . . ? C19 C23 C24 106.8(6) . . ? C26 C23 C24 107.0(7) . . ? C25 C23 C24 108.8(6) . . ? C30 C27 C29 107.4(8) . . ? C30 C27 C28 108.9(7) . . ? C29 C27 C28 106.8(8) . . ? C30 C27 C22 112.1(6) . . ? C29 C27 C22 111.7(7) . . ? C28 C27 C22 109.7(6) . . ? C32 C31 La2 93.5(4) . . ? C37 C32 C33 113.5(6) . . ? C37 C32 C31 122.1(6) . . ? C33 C32 C31 123.8(6) . . ? C37 C32 La2 131.5(5) . . ? C33 C32 La2 80.2(4) . . ? C31 C32 La2 58.1(3) . . ? C34 C33 C32 122.0(7) . . ? C34 C33 N4 122.3(6) . . ? C32 C33 N4 115.8(6) . . ? C34 C33 La2 136.1(5) . . ? C32 C33 La2 72.9(4) . . ? N4 C33 La2 61.5(3) . . ? C33 C34 C35 121.6(7) . . ? C34 C35 C36 118.2(7) . . ? C37 C36 C35 120.1(8) . . ? C36 C37 C32 124.5(7) . . ? C41 C40 La2 87.3(4) . . ? C46 C41 C42 115.1(7) . . ? C46 C41 C40 122.0(7) . . ? C42 C41 C40 122.5(7) . . ? C46 C41 La2 130.4(5) . . ? C42 C41 La2 76.1(4) . . ? C40 C41 La2 63.1(4) . . ? C43 C42 C41 121.6(7) . . ? C43 C42 N5 122.0(7) . . ? C41 C42 N5 116.4(6) . . ? C43 C42 La2 130.4(5) . . ? C41 C42 La2 76.0(4) . . ? N5 C42 La2 64.7(3) . . ? C44 C43 C42 121.1(9) . . ? C43 C44 C45 119.2(9) . . ? C44 C45 C46 121.0(9) . . ? C45 C46 C41 121.9(8) . . ? N6 C49 C50 107.9(8) . . ? N6 C49 C53 129.4(8) . . ? C50 C49 C53 120.8(8) . . ? N6 C49 La2 72.5(4) . . ? C50 C49 La2 76.4(4) . . ? C53 C49 La2 129.1(5) . . ? C51 C50 C49 105.2(8) . . ? C51 C50 La2 74.2(5) . . ? C49 C50 La2 74.3(4) . . ? C50 C51 C52 106.1(9) . . ? C50 C51 La2 77.3(5) . . ? C52 C51 La2 71.7(4) . . ? N6 C52 C57 129.6(8) . . ? N6 C52 C51 106.5(7) . . ? C57 C52 C51 123.2(8) . . ? N6 C52 La2 76.2(4) . . ? C57 C52 La2 119.3(5) . . ? C51 C52 La2 78.3(4) . . ? C49 C53 C56 115.2(8) . . ? C49 C53 C54 106.1(6) . . ? C56 C53 C54 109.1(7) . . ? C49 C53 C55 107.0(7) . . ? C56 C53 C55 110.4(8) . . ? C54 C53 C55 108.8(7) . . ? C52 C57 C60 111.7(7) . . ? C52 C57 C59 113.6(9) . . ? C60 C57 C59 106.8(9) . . ? C52 C57 C58 109.8(6) . . ? C60 C57 C58 111.2(8) . . ? C59 C57 C58 103.4(8) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.081 _refine_diff_density_min -1.192 _refine_diff_density_rms 0.086 # Attachment '4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 659965' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Me4PyrScBz2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 N3 Sc' _chemical_formula_weight 435.54 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' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.575(4) _cell_length_b 19.292(8) _cell_length_c 14.179(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.858(6) _cell_angle_gamma 90.00 _cell_volume 2340.4(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.332 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8258 _exptl_absorpt_correction_T_max 0.9071 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11701 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4109 _reflns_number_gt 2892 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+1.6910P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4109 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0994 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1676 _refine_ls_wR_factor_gt 0.1539 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 Sc1 Sc 0.74013(8) 0.85678(3) 0.10830(5) 0.0205(2) Uani 1 1 d . . . N1 N 0.7265(3) 0.88957(15) 0.2642(2) 0.0263(7) Uani 1 1 d . . . N2 N 0.7457(3) 0.87817(14) -0.0515(2) 0.0235(7) Uani 1 1 d . . . N3 N 0.7478(3) 0.74701(13) 0.1099(2) 0.0235(6) Uani 1 1 d . . . C1 C 0.9506(4) 0.92176(18) 0.1420(3) 0.0283(8) Uani 1 1 d . . . H1A H 1.0335 0.9115 0.0988 0.034 Uiso 1 1 calc R . . H1B H 0.9247 0.9717 0.1380 0.034 Uiso 1 1 calc R . . C2 C 0.9991(4) 0.90164(17) 0.2393(3) 0.0256(8) Uani 1 1 d . . . C3 C 0.8878(4) 0.88355(18) 0.3016(3) 0.0243(8) Uani 1 1 d . . . C4 C 0.9283(4) 0.8612(2) 0.3913(3) 0.0325(9) Uani 1 1 d . . . H4 H 0.8491 0.8509 0.4329 0.039 Uiso 1 1 calc R . . C5 C 1.0820(5) 0.8535(2) 0.4217(3) 0.0429(10) Uani 1 1 d . . . H5 H 1.1099 0.8370 0.4836 0.052 Uiso 1 1 calc R . . C6 C 1.1956(5) 0.8699(2) 0.3618(3) 0.0407(10) Uani 1 1 d . . . H6 H 1.3027 0.8645 0.3821 0.049 Uiso 1 1 calc R . . C7 C 1.1546(5) 0.8939(2) 0.2727(3) 0.0336(9) Uani 1 1 d . . . H7 H 1.2347 0.9056 0.2324 0.040 Uiso 1 1 calc R . . C8 C 0.6210(4) 0.8400(2) 0.3062(3) 0.0384(10) Uani 1 1 d . . . H8A H 0.6627 0.7930 0.3009 0.058 Uiso 1 1 calc R . . H8B H 0.5174 0.8426 0.2726 0.058 Uiso 1 1 calc R . . H8C H 0.6124 0.8515 0.3730 0.058 Uiso 1 1 calc R . . C9 C 0.6699(5) 0.9604(2) 0.2796(3) 0.0397(10) Uani 1 1 d . . . H9A H 0.6762 0.9705 0.3475 0.059 Uiso 1 1 calc R . . H9B H 0.5611 0.9644 0.2542 0.059 Uiso 1 1 calc R . . H9C H 0.7347 0.9935 0.2473 0.059 Uiso 1 1 calc R . . C10 C 0.5203(4) 0.91395(18) 0.0697(3) 0.0273(8) Uani 1 1 d . . . H10A H 0.4397 0.9030 0.1142 0.033 Uiso 1 1 calc R . . H10B H 0.5388 0.9646 0.0704 0.033 Uiso 1 1 calc R . . C11 C 0.4712(4) 0.89006(17) -0.0262(2) 0.0243(8) Uani 1 1 d . . . C12 C 0.5836(4) 0.87166(17) -0.0882(3) 0.0250(8) Uani 1 1 d . . . C13 C 0.5443(5) 0.8489(2) -0.1777(3) 0.0351(9) Uani 1 1 d . . . H13 H 0.6237 0.8388 -0.2192 0.042 Uiso 1 1 calc R . . C14 C 0.3902(5) 0.8407(2) -0.2078(3) 0.0453(11) Uani 1 1 d . . . H14 H 0.3625 0.8244 -0.2699 0.054 Uiso 1 1 calc R . . C15 C 0.2761(5) 0.8562(2) -0.1477(3) 0.0448(11) Uani 1 1 d . . . H15 H 0.1691 0.8498 -0.1676 0.054 Uiso 1 1 calc R . . C16 C 0.3169(4) 0.8808(2) -0.0588(3) 0.0325(9) Uani 1 1 d . . . H16 H 0.2367 0.8919 -0.0183 0.039 Uiso 1 1 calc R . . C17 C 0.8494(4) 0.8258(2) -0.0898(3) 0.0333(9) Uani 1 1 d . . . H17A H 0.8047 0.7796 -0.0823 0.050 Uiso 1 1 calc R . . H17B H 0.9525 0.8281 -0.0556 0.050 Uiso 1 1 calc R . . H17C H 0.8601 0.8350 -0.1570 0.050 Uiso 1 1 calc R . . C18 C 0.8040(5) 0.9475(2) -0.0747(3) 0.0346(9) Uani 1 1 d . . . H18A H 0.8002 0.9530 -0.1436 0.052 Uiso 1 1 calc R . . H18B H 0.9120 0.9526 -0.0485 0.052 Uiso 1 1 calc R . . H18C H 0.7384 0.9829 -0.0476 0.052 Uiso 1 1 calc R . . C19 C 0.8774(4) 0.70691(17) 0.1335(3) 0.0262(8) Uani 1 1 d . . . C20 C 0.8409(5) 0.63833(18) 0.1261(3) 0.0296(9) Uani 1 1 d . . . C21 C 0.6803(5) 0.63506(18) 0.0954(3) 0.0316(9) Uani 1 1 d . . . C22 C 0.6273(4) 0.70233(18) 0.0860(3) 0.0270(8) Uani 1 1 d . . . C23 C 1.0310(4) 0.73862(19) 0.1616(3) 0.0352(10) Uani 1 1 d . . . H23A H 1.0291 0.7576 0.2256 0.053 Uiso 1 1 calc R . . H23B H 1.0525 0.7759 0.1174 0.053 Uiso 1 1 calc R . . H23C H 1.1129 0.7033 0.1603 0.053 Uiso 1 1 calc R . . C24 C 0.9479(6) 0.5781(2) 0.1440(3) 0.0468(12) Uani 1 1 d . . . H24A H 1.0547 0.5949 0.1583 0.070 Uiso 1 1 calc R . . H24B H 0.9450 0.5486 0.0877 0.070 Uiso 1 1 calc R . . H24C H 0.9143 0.5513 0.1977 0.070 Uiso 1 1 calc R . . C25 C 0.5887(6) 0.5701(2) 0.0778(3) 0.0509(13) Uani 1 1 d . . . H25A H 0.4815 0.5818 0.0552 0.076 Uiso 1 1 calc R . . H25B H 0.5872 0.5436 0.1367 0.076 Uiso 1 1 calc R . . H25C H 0.6373 0.5422 0.0300 0.076 Uiso 1 1 calc R . . C26 C 0.4687(5) 0.7266(2) 0.0554(3) 0.0361(10) Uani 1 1 d . . . H26A H 0.4376 0.7635 0.0977 0.054 Uiso 1 1 calc R . . H26B H 0.3950 0.6878 0.0574 0.054 Uiso 1 1 calc R . . H26C H 0.4682 0.7444 -0.0094 0.054 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 Sc1 0.0238(4) 0.0180(3) 0.0196(4) 0.0007(3) 0.0013(3) -0.0001(3) N1 0.0260(17) 0.0292(15) 0.0235(18) -0.0020(12) 0.0010(13) 0.0022(13) N2 0.0227(16) 0.0242(14) 0.0239(17) 0.0008(12) 0.0042(13) -0.0006(12) N3 0.0298(17) 0.0199(14) 0.0207(16) 0.0007(12) 0.0010(12) -0.0009(13) C1 0.031(2) 0.0282(19) 0.026(2) 0.0008(15) 0.0031(16) -0.0054(16) C2 0.032(2) 0.0213(17) 0.024(2) -0.0053(14) -0.0005(16) -0.0021(15) C3 0.0253(19) 0.0277(17) 0.020(2) -0.0048(14) 0.0026(15) -0.0002(15) C4 0.028(2) 0.045(2) 0.024(2) 0.0011(17) 0.0030(17) 0.0001(18) C5 0.042(3) 0.063(3) 0.023(2) 0.006(2) -0.0032(19) 0.006(2) C6 0.026(2) 0.063(3) 0.033(3) -0.001(2) -0.0038(18) 0.0011(19) C7 0.027(2) 0.045(2) 0.029(2) -0.0018(17) 0.0029(17) -0.0034(18) C8 0.028(2) 0.059(3) 0.028(2) 0.0070(19) 0.0048(18) -0.0071(19) C9 0.047(3) 0.040(2) 0.032(2) -0.0138(18) -0.0024(19) 0.0164(19) C10 0.028(2) 0.0308(19) 0.023(2) 0.0013(15) 0.0055(16) 0.0044(16) C11 0.027(2) 0.0234(17) 0.022(2) 0.0027(14) 0.0029(16) 0.0017(15) C12 0.027(2) 0.0270(18) 0.021(2) 0.0036(14) 0.0005(15) -0.0018(15) C13 0.032(2) 0.048(2) 0.025(2) -0.0046(17) 0.0044(17) 0.0041(18) C14 0.038(2) 0.071(3) 0.027(2) -0.014(2) -0.0055(19) -0.001(2) C15 0.028(2) 0.069(3) 0.037(3) -0.009(2) -0.0008(18) -0.005(2) C16 0.027(2) 0.042(2) 0.029(2) -0.0016(17) 0.0038(17) 0.0038(17) C17 0.028(2) 0.046(2) 0.026(2) -0.0050(17) 0.0047(17) 0.0050(18) C18 0.037(2) 0.037(2) 0.030(2) 0.0097(17) 0.0042(18) -0.0090(17) C19 0.036(2) 0.0245(18) 0.019(2) 0.0002(14) 0.0023(16) 0.0050(16) C20 0.042(2) 0.0236(18) 0.024(2) 0.0023(15) 0.0054(17) 0.0042(17) C21 0.051(2) 0.0219(19) 0.023(2) -0.0027(14) 0.0080(18) -0.0089(17) C22 0.037(2) 0.0254(18) 0.019(2) 0.0005(14) 0.0050(16) -0.0039(16) C23 0.034(2) 0.029(2) 0.042(3) 0.0017(17) -0.0059(19) 0.0063(17) C24 0.068(3) 0.027(2) 0.046(3) 0.0029(18) 0.009(2) 0.014(2) C25 0.074(3) 0.029(2) 0.050(3) -0.0018(19) 0.010(2) -0.019(2) C26 0.036(2) 0.035(2) 0.038(3) 0.0020(17) 0.0004(19) -0.0106(18) _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 Sc1 N3 2.119(3) . ? Sc1 C10 2.221(4) . ? Sc1 C1 2.223(4) . ? Sc1 N2 2.306(3) . ? Sc1 N1 2.309(3) . ? N1 C3 1.453(5) . ? N1 C8 1.469(5) . ? N1 C9 1.471(5) . ? N2 C12 1.457(5) . ? N2 C18 1.472(4) . ? N2 C17 1.473(4) . ? N3 C22 1.371(5) . ? N3 C19 1.377(5) . ? C1 C2 1.466(5) . ? C2 C3 1.388(5) . ? C2 C7 1.393(5) . ? C3 C4 1.366(5) . ? C4 C5 1.367(6) . ? C5 C6 1.371(6) . ? C6 C7 1.369(6) . ? C10 C11 1.470(5) . ? C11 C16 1.383(5) . ? C11 C12 1.393(5) . ? C12 C13 1.363(5) . ? C13 C14 1.370(6) . ? C14 C15 1.373(6) . ? C15 C16 1.370(6) . ? C19 C20 1.362(5) . ? C19 C23 1.482(5) . ? C20 C21 1.417(6) . ? C20 C24 1.492(5) . ? C21 C22 1.379(5) . ? C21 C25 1.491(5) . ? C22 C26 1.475(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Sc1 C10 121.62(13) . . ? N3 Sc1 C1 122.48(13) . . ? C10 Sc1 C1 115.89(14) . . ? N3 Sc1 N2 100.75(11) . . ? C10 Sc1 N2 75.06(12) . . ? C1 Sc1 N2 92.32(12) . . ? N3 Sc1 N1 105.50(11) . . ? C10 Sc1 N1 90.18(12) . . ? C1 Sc1 N1 74.47(12) . . ? N2 Sc1 N1 153.74(10) . . ? C3 N1 C8 113.4(3) . . ? C3 N1 C9 109.6(3) . . ? C8 N1 C9 109.0(3) . . ? C3 N1 Sc1 102.7(2) . . ? C8 N1 Sc1 106.4(2) . . ? C9 N1 Sc1 115.8(2) . . ? C12 N2 C18 109.2(3) . . ? C12 N2 C17 113.2(3) . . ? C18 N2 C17 108.5(3) . . ? C12 N2 Sc1 104.7(2) . . ? C18 N2 Sc1 114.3(2) . . ? C17 N2 Sc1 107.0(2) . . ? C22 N3 C19 106.8(3) . . ? C22 N3 Sc1 127.1(2) . . ? C19 N3 Sc1 126.0(2) . . ? C2 C1 Sc1 103.2(2) . . ? C3 C2 C7 116.1(3) . . ? C3 C2 C1 120.1(3) . . ? C7 C2 C1 123.5(3) . . ? C4 C3 C2 122.0(3) . . ? C4 C3 N1 122.8(3) . . ? C2 C3 N1 115.2(3) . . ? C3 C4 C5 120.4(4) . . ? C4 C5 C6 119.4(4) . . ? C7 C6 C5 120.0(4) . . ? C6 C7 C2 122.0(4) . . ? C11 C10 Sc1 105.0(2) . . ? C16 C11 C12 116.3(3) . . ? C16 C11 C10 123.9(3) . . ? C12 C11 C10 119.7(3) . . ? C13 C12 C11 122.1(3) . . ? C13 C12 N2 122.0(3) . . ? C11 C12 N2 115.9(3) . . ? C12 C13 C14 120.0(4) . . ? C13 C14 C15 119.6(4) . . ? C16 C15 C14 119.8(4) . . ? C15 C16 C11 122.1(4) . . ? C20 C19 N3 110.4(3) . . ? C20 C19 C23 128.1(3) . . ? N3 C19 C23 121.4(3) . . ? C19 C20 C21 106.3(3) . . ? C19 C20 C24 127.4(4) . . ? C21 C20 C24 126.3(4) . . ? C22 C21 C20 107.1(3) . . ? C22 C21 C25 127.5(4) . . ? C20 C21 C25 125.4(4) . . ? N3 C22 C21 109.3(3) . . ? N3 C22 C26 122.6(3) . . ? C21 C22 C26 128.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sc1 N3 C19 C20 -179.5(2) . . . . ? Sc1 N3 C22 C21 179.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.361 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.090 # Attachment '6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 659966' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common PyrScBzB _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H42 B F20 N2 O2 Sc' _chemical_formula_weight 1126.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.6894(12) _cell_length_b 20.7503(14) _cell_length_c 26.9268(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9883.8(12) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4576 _exptl_absorpt_coefficient_mu 0.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8565 _exptl_absorpt_correction_T_max 0.8783 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49807 _diffrn_reflns_av_R_equivalents 0.1223 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.09 _reflns_number_total 8768 _reflns_number_gt 6217 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8768 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.18906(2) 0.10012(2) 0.558635(15) 0.02921(12) Uani 1 1 d . . . F1 F 0.40102(9) 0.21583(8) 0.39475(5) 0.0552(4) Uani 1 1 d . . . F2 F 0.49551(10) 0.14410(10) 0.44644(6) 0.0774(5) Uani 1 1 d . . . F3 F 0.52775(10) 0.02088(10) 0.41781(7) 0.0856(6) Uani 1 1 d . . . F4 F 0.46434(9) -0.02708(8) 0.33404(7) 0.0694(5) Uani 1 1 d . . . F5 F 0.37265(8) 0.04501(7) 0.27953(5) 0.0477(4) Uani 1 1 d . . . F6 F 0.46089(7) 0.26002(7) 0.30073(5) 0.0466(4) Uani 1 1 d . . . F7 F 0.57431(8) 0.27309(8) 0.23694(6) 0.0585(4) Uani 1 1 d . . . F8 F 0.57416(8) 0.20532(8) 0.14987(6) 0.0629(4) Uani 1 1 d . . . F9 F 0.45689(9) 0.12515(7) 0.12913(5) 0.0556(4) Uani 1 1 d . . . F10 F 0.34260(7) 0.11285(6) 0.19067(5) 0.0441(3) Uani 1 1 d . . . F11 F 0.24434(8) 0.19230(7) 0.38518(5) 0.0465(4) Uani 1 1 d . . . F12 F 0.17093(8) 0.29576(8) 0.41734(5) 0.0571(4) Uani 1 1 d . . . F13 F 0.17590(9) 0.40779(7) 0.36471(6) 0.0613(4) Uani 1 1 d . . . F14 F 0.26196(9) 0.41442(7) 0.28135(5) 0.0577(4) Uani 1 1 d . . . F15 F 0.33546(8) 0.31311(6) 0.24833(5) 0.0449(3) Uani 1 1 d . . . F16 F 0.23809(7) 0.20908(6) 0.20764(5) 0.0433(3) Uani 1 1 d . . . F17 F 0.10780(8) 0.15535(8) 0.18016(6) 0.0614(4) Uani 1 1 d . . . F18 F 0.04414(9) 0.06090(9) 0.23654(7) 0.0770(5) Uani 1 1 d . . . F19 F 0.11571(8) 0.02009(8) 0.31961(7) 0.0699(5) Uani 1 1 d . . . F20 F 0.24646(7) 0.06772(7) 0.34618(5) 0.0485(4) Uani 1 1 d . . . O1 O 0.16015(9) 0.19451(7) 0.59447(6) 0.0419(4) Uani 1 1 d . . . O2 O 0.19303(9) 0.09063(8) 0.64055(6) 0.0426(4) Uani 1 1 d . . . N1 N 0.08920(10) 0.11504(9) 0.50120(7) 0.0408(5) Uani 1 1 d . . . N2 N 0.31731(10) 0.06538(9) 0.55510(7) 0.0364(5) Uani 1 1 d . . . B1 B 0.33046(14) 0.17763(12) 0.29423(9) 0.0327(6) Uani 1 1 d . . . C1 C 0.11688(12) 0.01260(11) 0.56568(9) 0.0368(5) Uani 1 1 d . . . H1A H 0.1138 -0.0133 0.5349 0.044 Uiso 1 1 d R . . H1B H 0.1298 -0.0148 0.5946 0.044 Uiso 1 1 d R . . C2 C 0.05090(13) 0.05440(11) 0.57393(9) 0.0387(6) Uani 1 1 d . . . C3 C 0.03583(13) 0.10618(12) 0.54178(9) 0.0406(6) Uani 1 1 d . . . C4 C -0.02498(14) 0.14771(13) 0.55009(12) 0.0565(7) Uani 1 1 d . . . H4 H -0.0349 0.1817 0.5273 0.068 Uiso 1 1 d R . . C5 C -0.07034(15) 0.13979(14) 0.59085(13) 0.0669(9) Uani 1 1 d . . . H5 H -0.1123 0.1676 0.5960 0.080 Uiso 1 1 d R . . C6 C -0.05475(17) 0.09107(13) 0.62450(13) 0.0658(9) Uani 1 1 d . . . H6 H -0.0850 0.0864 0.6534 0.079 Uiso 1 1 d R . . C7 C 0.00459(15) 0.04945(12) 0.61603(11) 0.0518(7) Uani 1 1 d . . . H7 H 0.0144 0.0163 0.6395 0.062 Uiso 1 1 d R . . C8 C 0.07420(15) 0.06801(14) 0.46046(10) 0.0542(7) Uani 1 1 d . . . H8A H 0.0745 0.0242 0.4740 0.081 Uiso 1 1 d R . . H8B H 0.1135 0.0720 0.4350 0.081 Uiso 1 1 d R . . H8C H 0.0247 0.0770 0.4456 0.081 Uiso 1 1 d R . . C9 C 0.08844(15) 0.18006(13) 0.47869(11) 0.0573(8) Uani 1 1 d . . . H9A H 0.0411 0.1862 0.4603 0.086 Uiso 1 1 d R . . H9B H 0.1313 0.1844 0.4559 0.086 Uiso 1 1 d R . . H9C H 0.0924 0.2126 0.5049 0.086 Uiso 1 1 d R . . C10 C 0.32341(12) 0.13094(12) 0.54677(9) 0.0374(6) Uani 1 1 d . . . C11 C 0.28987(13) 0.14645(11) 0.50170(9) 0.0391(6) Uani 1 1 d . . . H11 H 0.2843 0.1884 0.4880 0.047 Uiso 1 1 d R . . C12 C 0.26574(12) 0.08841(11) 0.48016(8) 0.0367(5) Uani 1 1 d . . . H12 H 0.2408 0.0837 0.4491 0.044 Uiso 1 1 d R . . C13 C 0.28515(12) 0.03902(11) 0.51281(8) 0.0337(5) Uani 1 1 d . . . C14 C 0.37543(14) 0.17263(13) 0.57866(10) 0.0514(7) Uani 1 1 d . . . C15 C 0.3582(2) 0.1680(3) 0.63254(12) 0.137(2) Uani 1 1 d . . . H15A H 0.3663 0.1237 0.6439 0.205 Uiso 1 1 d R . . H15B H 0.3054 0.1803 0.6383 0.205 Uiso 1 1 d R . . H15C H 0.3915 0.1972 0.6510 0.205 Uiso 1 1 d R . . C16 C 0.45509(15) 0.1499(2) 0.56971(13) 0.0875(12) Uani 1 1 d . . . H16A H 0.4900 0.1750 0.5903 0.131 Uiso 1 1 d R . . H16B H 0.4680 0.1558 0.5346 0.131 Uiso 1 1 d R . . H16C H 0.4591 0.1042 0.5784 0.131 Uiso 1 1 d R . . C17 C 0.3720(3) 0.24211(17) 0.56199(19) 0.1269(19) Uani 1 1 d . . . H17A H 0.3229 0.2606 0.5712 0.190 Uiso 1 1 d R . . H17B H 0.3782 0.2442 0.5259 0.190 Uiso 1 1 d R . . H17C H 0.4125 0.2666 0.5781 0.190 Uiso 1 1 d R . . C18 C 0.29144(14) -0.03258(11) 0.50236(9) 0.0418(6) Uani 1 1 d . . . C19 C 0.37018(14) -0.04132(14) 0.47794(10) 0.0548(7) Uani 1 1 d . . . H19A H 0.3710 -0.0192 0.4458 0.082 Uiso 1 1 d R . . H19B H 0.3801 -0.0873 0.4730 0.082 Uiso 1 1 d R . . H19C H 0.4091 -0.0230 0.4996 0.082 Uiso 1 1 d R . . C20 C 0.23167(15) -0.05543(13) 0.46509(11) 0.0568(7) Uani 1 1 d . . . H20A H 0.1813 -0.0507 0.4797 0.085 Uiso 1 1 d R . . H20B H 0.2406 -0.1008 0.4569 0.085 Uiso 1 1 d R . . H20C H 0.2349 -0.0294 0.4348 0.085 Uiso 1 1 d R . . C21 C 0.28797(17) -0.07302(13) 0.54966(11) 0.0604(8) Uani 1 1 d . . . H21A H 0.3249 -0.0566 0.5737 0.091 Uiso 1 1 d R . . H21B H 0.2997 -0.1180 0.5417 0.091 Uiso 1 1 d R . . H21C H 0.2371 -0.0704 0.5639 0.091 Uiso 1 1 d R . . C22 C 0.16614(16) 0.14083(13) 0.67275(9) 0.0507(7) Uani 1 1 d . . . H22A H 0.2092 0.1640 0.6880 0.061 Uiso 1 1 d R . . H22B H 0.1346 0.1224 0.6996 0.061 Uiso 1 1 d R . . C23 C 0.12047(15) 0.18557(13) 0.64151(10) 0.0491(7) Uani 1 1 d . . . H23A H 0.0697 0.1672 0.6355 0.059 Uiso 1 1 d R . . H23B H 0.1144 0.2275 0.6586 0.059 Uiso 1 1 d R . . C24 C 0.22682(19) 0.03738(14) 0.66721(10) 0.0622(8) Uani 1 1 d . . . H24A H 0.2645 0.0539 0.6906 0.093 Uiso 1 1 d R . . H24B H 0.2513 0.0081 0.6436 0.093 Uiso 1 1 d R . . H24C H 0.1875 0.0140 0.6855 0.093 Uiso 1 1 d R . . C25 C 0.16519(17) 0.26054(12) 0.57920(12) 0.0585(7) Uani 1 1 d . . . H25A H 0.1142 0.2781 0.5748 0.088 Uiso 1 1 d R . . H25B H 0.1929 0.2632 0.5477 0.088 Uiso 1 1 d R . . H25C H 0.1919 0.2854 0.6046 0.088 Uiso 1 1 d R . . C26 C 0.38045(12) 0.13454(12) 0.33402(8) 0.0359(5) Uani 1 1 d . . . C27 C 0.41402(13) 0.15565(13) 0.37720(9) 0.0431(6) Uani 1 1 d . . . C28 C 0.46307(14) 0.11883(15) 0.40543(10) 0.0535(7) Uani 1 1 d . . . C29 C 0.47972(14) 0.05690(15) 0.39102(11) 0.0556(8) Uani 1 1 d . . . C30 C 0.44752(14) 0.03301(13) 0.34921(10) 0.0495(7) Uani 1 1 d . . . C31 C 0.40008(13) 0.07157(12) 0.32156(9) 0.0399(6) Uani 1 1 d . . . C32 C 0.39345(12) 0.18733(10) 0.24931(8) 0.0313(5) Uani 1 1 d . . . C33 C 0.45638(13) 0.22635(11) 0.25781(8) 0.0360(5) Uani 1 1 d . . . C34 C 0.51581(13) 0.23372(12) 0.22568(9) 0.0411(6) Uani 1 1 d . . . C35 C 0.51629(13) 0.19964(12) 0.18174(9) 0.0414(6) Uani 1 1 d . . . C36 C 0.45726(13) 0.15965(12) 0.17184(8) 0.0393(6) Uani 1 1 d . . . C37 C 0.39782(12) 0.15394(11) 0.20474(8) 0.0340(5) Uani 1 1 d . . . C38 C 0.29614(12) 0.24602(11) 0.31558(8) 0.0321(5) Uani 1 1 d . . . C39 C 0.25181(13) 0.24693(11) 0.35821(8) 0.0364(5) Uani 1 1 d . . . C40 C 0.21274(13) 0.29966(13) 0.37538(8) 0.0405(6) Uani 1 1 d . . . C41 C 0.21524(14) 0.35659(12) 0.34960(9) 0.0426(6) Uani 1 1 d . . . C42 C 0.25856(14) 0.35900(11) 0.30733(8) 0.0400(6) Uani 1 1 d . . . C43 C 0.29687(13) 0.30511(11) 0.29125(8) 0.0347(5) Uani 1 1 d . . . C44 C 0.25245(12) 0.14003(10) 0.27704(8) 0.0316(5) Uani 1 1 d . . . C45 C 0.21144(12) 0.15995(11) 0.23594(8) 0.0353(5) Uani 1 1 d . . . C46 C 0.14378(14) 0.13392(12) 0.22110(9) 0.0433(6) Uani 1 1 d . . . C47 C 0.11146(14) 0.08560(13) 0.24913(10) 0.0491(7) Uani 1 1 d . . . C48 C 0.14767(13) 0.06531(12) 0.29055(10) 0.0462(6) Uani 1 1 d . . . C49 C 0.21644(13) 0.09184(11) 0.30394(9) 0.0371(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.0296(2) 0.0291(2) 0.0289(2) 0.00002(17) 0.00123(17) -0.00292(18) F1 0.0627(10) 0.0606(10) 0.0424(8) -0.0031(7) -0.0132(7) -0.0077(8) F2 0.0689(11) 0.1104(15) 0.0530(10) 0.0106(10) -0.0310(8) -0.0121(11) F3 0.0589(11) 0.1018(14) 0.0962(14) 0.0366(12) -0.0316(10) 0.0148(10) F4 0.0532(10) 0.0546(10) 0.1004(13) 0.0157(9) -0.0053(9) 0.0142(8) F5 0.0451(8) 0.0435(8) 0.0546(9) -0.0011(7) -0.0053(7) 0.0044(7) F6 0.0412(8) 0.0593(9) 0.0393(8) -0.0106(7) -0.0012(6) -0.0139(7) F7 0.0364(8) 0.0737(11) 0.0654(10) -0.0022(8) 0.0025(7) -0.0232(8) F8 0.0440(9) 0.0873(12) 0.0573(10) 0.0003(9) 0.0235(7) -0.0046(8) F9 0.0614(10) 0.0594(9) 0.0460(9) -0.0155(7) 0.0153(7) 0.0005(8) F10 0.0423(8) 0.0451(8) 0.0449(8) -0.0100(6) 0.0029(6) -0.0108(6) F11 0.0531(9) 0.0473(8) 0.0390(8) 0.0066(7) 0.0134(6) -0.0035(7) F12 0.0582(9) 0.0657(10) 0.0473(9) -0.0079(8) 0.0213(7) -0.0030(8) F13 0.0708(11) 0.0597(10) 0.0534(9) -0.0119(8) 0.0006(8) 0.0239(8) F14 0.0860(12) 0.0415(8) 0.0457(9) 0.0057(7) 0.0003(8) 0.0107(8) F15 0.0572(9) 0.0447(8) 0.0329(7) 0.0061(6) 0.0092(6) 0.0004(7) F16 0.0430(8) 0.0448(8) 0.0422(8) 0.0136(6) -0.0080(6) -0.0077(6) F17 0.0513(9) 0.0670(10) 0.0658(10) 0.0155(8) -0.0280(8) -0.0108(8) F18 0.0422(9) 0.0818(12) 0.1070(14) 0.0194(11) -0.0249(9) -0.0285(9) F19 0.0481(9) 0.0728(11) 0.0889(12) 0.0325(10) 0.0031(9) -0.0254(8) F20 0.0432(8) 0.0569(9) 0.0456(8) 0.0204(7) -0.0020(6) -0.0071(7) O1 0.0467(10) 0.0309(9) 0.0479(10) -0.0034(7) 0.0120(8) -0.0030(7) O2 0.0564(11) 0.0430(10) 0.0283(8) -0.0026(7) 0.0036(7) -0.0007(8) N1 0.0331(10) 0.0458(12) 0.0436(12) 0.0059(10) -0.0050(9) -0.0055(9) N2 0.0297(10) 0.0448(12) 0.0347(11) -0.0035(9) -0.0015(8) 0.0007(9) B1 0.0321(14) 0.0349(14) 0.0311(14) 0.0036(11) 0.0004(11) -0.0059(11) C1 0.0386(13) 0.0318(12) 0.0401(13) -0.0012(10) 0.0033(10) -0.0035(10) C2 0.0339(12) 0.0309(12) 0.0514(15) -0.0067(11) 0.0055(11) -0.0115(10) C3 0.0290(12) 0.0403(14) 0.0526(15) -0.0014(12) 0.0002(11) -0.0072(11) C4 0.0348(14) 0.0472(16) 0.087(2) 0.0060(15) 0.0002(14) 0.0001(12) C5 0.0388(16) 0.0460(17) 0.116(3) -0.0072(18) 0.0227(17) -0.0014(13) C6 0.0568(18) 0.0430(16) 0.098(2) -0.0090(16) 0.0415(17) -0.0097(14) C7 0.0531(16) 0.0356(14) 0.0666(18) -0.0018(13) 0.0227(14) -0.0115(13) C8 0.0456(15) 0.0735(19) 0.0436(15) -0.0029(14) -0.0132(12) -0.0064(14) C9 0.0491(16) 0.0609(18) 0.0620(18) 0.0258(15) -0.0106(13) -0.0030(14) C10 0.0283(12) 0.0433(14) 0.0405(14) -0.0076(11) 0.0054(10) -0.0052(10) C11 0.0384(13) 0.0380(13) 0.0407(14) 0.0052(11) 0.0070(11) -0.0061(11) C12 0.0324(12) 0.0483(14) 0.0293(12) 0.0000(11) 0.0001(10) -0.0011(11) C13 0.0292(11) 0.0410(13) 0.0310(12) -0.0047(10) 0.0014(9) -0.0011(10) C14 0.0368(14) 0.0610(18) 0.0563(17) -0.0171(14) 0.0016(12) -0.0140(13) C15 0.115(3) 0.246(6) 0.049(2) -0.056(3) 0.018(2) -0.118(4) C16 0.0344(15) 0.130(3) 0.098(3) -0.052(2) -0.0070(16) -0.0086(18) C17 0.117(4) 0.063(2) 0.201(5) -0.015(3) -0.065(3) -0.033(2) C18 0.0401(13) 0.0381(13) 0.0471(14) -0.0065(12) 0.0017(11) 0.0026(11) C19 0.0433(15) 0.0605(17) 0.0607(17) -0.0188(14) 0.0010(13) 0.0095(13) C20 0.0443(15) 0.0538(17) 0.0722(19) -0.0296(15) 0.0033(14) 0.0003(13) C21 0.0671(19) 0.0420(15) 0.072(2) 0.0026(14) 0.0081(15) 0.0127(14) C22 0.0638(17) 0.0503(16) 0.0380(14) -0.0106(12) 0.0135(12) -0.0113(14) C23 0.0494(16) 0.0434(15) 0.0544(16) -0.0158(13) 0.0206(13) -0.0081(12) C24 0.094(2) 0.0539(17) 0.0392(15) 0.0086(13) -0.0051(15) 0.0043(16) C25 0.0702(19) 0.0302(14) 0.075(2) 0.0025(14) 0.0062(16) -0.0014(13) C26 0.0281(12) 0.0445(14) 0.0352(13) 0.0065(11) 0.0011(10) -0.0050(10) C27 0.0395(14) 0.0491(16) 0.0408(14) 0.0062(12) -0.0028(11) -0.0071(12) C28 0.0381(14) 0.080(2) 0.0427(15) 0.0170(14) -0.0139(12) -0.0129(14) C29 0.0348(14) 0.073(2) 0.0594(18) 0.0274(16) -0.0109(13) 0.0019(14) C30 0.0331(13) 0.0513(16) 0.0642(19) 0.0144(14) 0.0031(13) 0.0029(12) C31 0.0302(12) 0.0477(15) 0.0418(14) 0.0067(12) -0.0003(11) -0.0023(11) C32 0.0287(11) 0.0331(12) 0.0321(12) 0.0015(10) -0.0030(9) -0.0019(10) C33 0.0331(12) 0.0412(14) 0.0337(13) -0.0021(10) -0.0018(10) -0.0026(10) C34 0.0287(12) 0.0474(14) 0.0473(14) 0.0033(12) 0.0008(11) -0.0076(11) C35 0.0301(12) 0.0521(15) 0.0420(14) 0.0049(12) 0.0118(11) 0.0011(11) C36 0.0409(13) 0.0438(14) 0.0333(13) -0.0034(11) 0.0045(10) 0.0044(11) C37 0.0314(12) 0.0342(12) 0.0366(13) 0.0004(10) 0.0000(10) -0.0026(10) C38 0.0283(11) 0.0398(13) 0.0282(11) -0.0003(10) -0.0017(9) -0.0062(10) C39 0.0365(13) 0.0401(14) 0.0328(12) 0.0030(11) -0.0008(10) -0.0054(11) C40 0.0354(13) 0.0558(16) 0.0304(13) -0.0072(12) 0.0034(10) -0.0048(12) C41 0.0433(14) 0.0459(15) 0.0385(14) -0.0110(12) -0.0053(11) 0.0075(12) C42 0.0469(14) 0.0391(14) 0.0340(13) 0.0029(11) -0.0098(11) -0.0012(11) C43 0.0370(13) 0.0410(13) 0.0260(12) -0.0005(10) 0.0001(10) -0.0042(11) C44 0.0285(11) 0.0343(12) 0.0321(12) 0.0001(10) 0.0012(9) 0.0007(10) C45 0.0312(12) 0.0354(13) 0.0394(13) 0.0032(10) 0.0004(10) -0.0018(10) C46 0.0367(13) 0.0462(15) 0.0471(15) 0.0048(12) -0.0110(11) -0.0003(11) C47 0.0298(13) 0.0488(16) 0.0688(18) 0.0033(14) -0.0082(12) -0.0104(12) C48 0.0324(13) 0.0452(15) 0.0611(17) 0.0139(13) 0.0071(12) -0.0077(11) C49 0.0310(12) 0.0399(13) 0.0405(14) 0.0059(11) -0.0015(10) -0.0008(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 O2 2.2156(16) . ? Sc1 C1 2.228(2) . ? Sc1 O1 2.2424(16) . ? Sc1 N1 2.3681(19) . ? Sc1 N2 2.3823(18) . ? Sc1 C13 2.453(2) . ? Sc1 C10 2.482(2) . ? Sc1 C12 2.523(2) . ? Sc1 C11 2.541(2) . ? Sc1 C2 2.654(2) . ? Sc1 C3 2.751(2) . ? F1 C27 1.355(3) . ? F2 C28 1.350(3) . ? F3 C29 1.342(3) . ? F4 C30 1.345(3) . ? F5 C31 1.349(3) . ? F6 C33 1.353(2) . ? F7 C34 1.353(3) . ? F8 C35 1.341(3) . ? F9 C36 1.355(3) . ? F10 C37 1.351(2) . ? F11 C39 1.353(3) . ? F12 C40 1.353(3) . ? F13 C41 1.334(3) . ? F14 C42 1.347(3) . ? F15 C43 1.352(2) . ? F16 C45 1.357(2) . ? F17 C46 1.349(3) . ? F18 C47 1.340(3) . ? F19 C48 1.346(3) . ? F20 C49 1.351(3) . ? O1 C25 1.433(3) . ? O1 C23 1.460(3) . ? O2 C22 1.436(3) . ? O2 C24 1.447(3) . ? N1 C3 1.456(3) . ? N1 C9 1.479(3) . ? N1 C8 1.492(3) . ? N2 C10 1.383(3) . ? N2 C13 1.386(3) . ? B1 C38 1.647(3) . ? B1 C44 1.651(3) . ? B1 C26 1.652(3) . ? B1 C32 1.657(3) . ? C1 C2 1.471(3) . ? C2 C7 1.402(3) . ? C2 C3 1.405(3) . ? C3 C4 1.396(3) . ? C4 C5 1.369(4) . ? C5 C6 1.385(4) . ? C6 C7 1.378(4) . ? C10 C11 1.389(3) . ? C10 C14 1.527(3) . ? C11 C12 1.403(3) . ? C12 C13 1.393(3) . ? C13 C18 1.516(3) . ? C14 C15 1.486(4) . ? C14 C16 1.505(4) . ? C14 C17 1.511(5) . ? C18 C21 1.526(4) . ? C18 C20 1.533(4) . ? C18 C19 1.551(3) . ? C22 C23 1.491(4) . ? C26 C27 1.377(3) . ? C26 C31 1.393(3) . ? C27 C28 1.384(3) . ? C28 C29 1.374(4) . ? C29 C30 1.356(4) . ? C30 C31 1.378(3) . ? C32 C37 1.388(3) . ? C32 C33 1.395(3) . ? C33 C34 1.370(3) . ? C34 C35 1.378(3) . ? C35 C36 1.360(3) . ? C36 C37 1.380(3) . ? C38 C43 1.390(3) . ? C38 C39 1.390(3) . ? C39 C40 1.374(3) . ? C40 C41 1.371(3) . ? C41 C42 1.373(3) . ? C42 C43 1.377(3) . ? C44 C45 1.386(3) . ? C44 C49 1.389(3) . ? C45 C46 1.373(3) . ? C46 C47 1.379(3) . ? C47 C48 1.353(4) . ? C48 C49 1.383(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 O2 Sc1 C1 82.00(8) . . ? O2 Sc1 O1 69.91(6) . . ? C1 Sc1 O1 122.99(7) . . ? O2 Sc1 N1 133.26(7) . . ? C1 Sc1 N1 74.61(8) . . ? O1 Sc1 N1 89.81(7) . . ? O2 Sc1 N2 89.01(6) . . ? C1 Sc1 N2 107.61(8) . . ? O1 Sc1 N2 119.91(6) . . ? N1 Sc1 N2 136.37(7) . . ? O2 Sc1 C13 115.65(7) . . ? C1 Sc1 C13 91.07(8) . . ? O1 Sc1 C13 145.67(7) . . ? N1 Sc1 C13 104.83(7) . . ? N2 Sc1 C13 33.26(6) . . ? O2 Sc1 C10 96.94(7) . . ? C1 Sc1 C10 140.33(8) . . ? O1 Sc1 C10 92.80(7) . . ? N1 Sc1 C10 126.63(7) . . ? N2 Sc1 C10 32.96(7) . . ? C13 Sc1 C10 53.48(8) . . ? O2 Sc1 C12 143.93(7) . . ? C1 Sc1 C12 107.52(8) . . ? O1 Sc1 C12 124.55(7) . . ? N1 Sc1 C12 82.34(7) . . ? N2 Sc1 C12 54.93(7) . . ? C13 Sc1 C12 32.48(7) . . ? C10 Sc1 C12 53.28(7) . . ? O2 Sc1 C11 127.75(7) . . ? C1 Sc1 C11 139.64(8) . . ? O1 Sc1 C11 95.12(7) . . ? N1 Sc1 C11 94.59(7) . . ? N2 Sc1 C11 54.69(7) . . ? C13 Sc1 C11 53.54(8) . . ? C10 Sc1 C11 32.08(7) . . ? C12 Sc1 C11 32.17(7) . . ? O2 Sc1 C2 80.96(7) . . ? C1 Sc1 C2 33.66(7) . . ? O1 Sc1 C2 92.03(7) . . ? N1 Sc1 C2 57.39(7) . . ? N2 Sc1 C2 140.81(7) . . ? C13 Sc1 C2 122.10(7) . . ? C10 Sc1 C2 173.72(8) . . ? C12 Sc1 C2 126.21(7) . . ? C11 Sc1 C2 151.08(8) . . ? O2 Sc1 C3 101.51(7) . . ? C1 Sc1 C3 59.11(8) . . ? O1 Sc1 C3 78.83(7) . . ? N1 Sc1 C3 31.94(7) . . ? N2 Sc1 C3 160.99(7) . . ? C13 Sc1 C3 128.55(7) . . ? C10 Sc1 C3 155.57(8) . . ? C12 Sc1 C3 113.33(8) . . ? C11 Sc1 C3 125.08(8) . . ? C2 Sc1 C3 30.07(7) . . ? C25 O1 C23 113.59(19) . . ? C25 O1 Sc1 134.21(16) . . ? C23 O1 Sc1 111.84(13) . . ? C22 O2 C24 113.02(19) . . ? C22 O2 Sc1 121.73(15) . . ? C24 O2 Sc1 125.10(15) . . ? C3 N1 C9 114.6(2) . . ? C3 N1 C8 110.74(19) . . ? C9 N1 C8 107.1(2) . . ? C3 N1 Sc1 88.69(13) . . ? C9 N1 Sc1 113.18(15) . . ? C8 N1 Sc1 121.83(15) . . ? C10 N2 C13 106.67(19) . . ? C10 N2 Sc1 77.47(12) . . ? C13 N2 Sc1 76.19(12) . . ? C38 B1 C44 101.35(17) . . ? C38 B1 C26 115.92(19) . . ? C44 B1 C26 111.93(18) . . ? C38 B1 C32 113.45(18) . . ? C44 B1 C32 114.51(18) . . ? C26 B1 C32 100.32(17) . . ? C2 C1 Sc1 89.25(13) . . ? C7 C2 C3 116.3(2) . . ? C7 C2 C1 122.8(2) . . ? C3 C2 C1 120.5(2) . . ? C7 C2 Sc1 133.59(18) . . ? C3 C2 Sc1 78.80(13) . . ? C1 C2 Sc1 57.09(11) . . ? C4 C3 C2 121.3(2) . . ? C4 C3 N1 122.8(2) . . ? C2 C3 N1 115.8(2) . . ? C4 C3 Sc1 139.53(18) . . ? C2 C3 Sc1 71.13(13) . . ? N1 C3 Sc1 59.38(11) . . ? C5 C4 C3 120.4(3) . . ? C4 C5 C6 119.7(3) . . ? C7 C6 C5 120.0(3) . . ? C6 C7 C2 122.2(3) . . ? N2 C10 C11 109.7(2) . . ? N2 C10 C14 120.9(2) . . ? C11 C10 C14 128.1(2) . . ? N2 C10 Sc1 69.57(12) . . ? C11 C10 Sc1 76.30(13) . . ? C14 C10 Sc1 130.59(16) . . ? C10 C11 C12 107.0(2) . . ? C10 C11 Sc1 71.63(13) . . ? C12 C11 Sc1 73.22(13) . . ? C13 C12 C11 107.2(2) . . ? C13 C12 Sc1 71.02(12) . . ? C11 C12 Sc1 74.61(13) . . ? N2 C13 C12 109.24(19) . . ? N2 C13 C18 120.6(2) . . ? C12 C13 C18 128.4(2) . . ? N2 C13 Sc1 70.55(11) . . ? C12 C13 Sc1 76.50(13) . . ? C18 C13 Sc1 130.58(15) . . ? C15 C14 C16 109.2(3) . . ? C15 C14 C17 110.1(3) . . ? C16 C14 C17 106.8(3) . . ? C15 C14 C10 112.9(2) . . ? C16 C14 C10 107.3(2) . . ? C17 C14 C10 110.4(3) . . ? C13 C18 C21 112.4(2) . . ? C13 C18 C20 112.0(2) . . ? C21 C18 C20 110.4(2) . . ? C13 C18 C19 105.0(2) . . ? C21 C18 C19 109.0(2) . . ? C20 C18 C19 107.8(2) . . ? O2 C22 C23 106.9(2) . . ? O1 C23 C22 108.0(2) . . ? C27 C26 C31 113.2(2) . . ? C27 C26 B1 127.3(2) . . ? C31 C26 B1 119.0(2) . . ? F1 C27 C26 121.0(2) . . ? F1 C27 C28 115.1(2) . . ? C26 C27 C28 124.0(3) . . ? F2 C28 C29 120.2(2) . . ? F2 C28 C27 120.1(3) . . ? C29 C28 C27 119.7(2) . . ? F3 C29 C30 120.6(3) . . ? F3 C29 C28 120.3(3) . . ? C30 C29 C28 119.1(2) . . ? F4 C30 C29 119.9(2) . . ? F4 C30 C31 120.6(3) . . ? C29 C30 C31 119.5(3) . . ? F5 C31 C30 115.8(2) . . ? F5 C31 C26 119.7(2) . . ? C30 C31 C26 124.5(2) . . ? C37 C32 C33 112.8(2) . . ? C37 C32 B1 127.45(19) . . ? C33 C32 B1 119.16(19) . . ? F6 C33 C34 115.9(2) . . ? F6 C33 C32 119.14(19) . . ? C34 C33 C32 125.0(2) . . ? F7 C34 C33 120.8(2) . . ? F7 C34 C35 119.8(2) . . ? C33 C34 C35 119.3(2) . . ? F8 C35 C36 120.9(2) . . ? F8 C35 C34 120.6(2) . . ? C36 C35 C34 118.5(2) . . ? F9 C36 C35 119.5(2) . . ? F9 C36 C37 119.7(2) . . ? C35 C36 C37 120.8(2) . . ? F10 C37 C36 115.1(2) . . ? F10 C37 C32 121.15(19) . . ? C36 C37 C32 123.7(2) . . ? C43 C38 C39 112.5(2) . . ? C43 C38 B1 126.30(19) . . ? C39 C38 B1 120.5(2) . . ? F11 C39 C40 115.9(2) . . ? F11 C39 C38 119.1(2) . . ? C40 C39 C38 124.9(2) . . ? F12 C40 C41 119.5(2) . . ? F12 C40 C39 120.5(2) . . ? C41 C40 C39 120.0(2) . . ? F13 C41 C40 121.0(2) . . ? F13 C41 C42 121.0(2) . . ? C40 C41 C42 118.0(2) . . ? F14 C42 C41 119.1(2) . . ? F14 C42 C43 120.5(2) . . ? C41 C42 C43 120.4(2) . . ? F15 C43 C42 114.7(2) . . ? F15 C43 C38 121.0(2) . . ? C42 C43 C38 124.3(2) . . ? C45 C44 C49 113.0(2) . . ? C45 C44 B1 121.34(19) . . ? C49 C44 B1 125.2(2) . . ? F16 C45 C46 115.8(2) . . ? F16 C45 C44 119.37(19) . . ? C46 C45 C44 124.8(2) . . ? F17 C46 C45 121.3(2) . . ? F17 C46 C47 119.4(2) . . ? C45 C46 C47 119.2(2) . . ? F18 C47 C48 120.7(2) . . ? F18 C47 C46 120.5(2) . . ? C48 C47 C46 118.7(2) . . ? F19 C48 C47 119.8(2) . . ? F19 C48 C49 119.7(2) . . ? C47 C48 C49 120.5(2) . . ? F20 C49 C48 114.7(2) . . ? F20 C49 C44 121.7(2) . . ? C48 C49 C44 123.6(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.418 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.065 # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 668429' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common PyrYBz2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H44 N3 Y' _chemical_formula_weight 535.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.140(2) _cell_length_b 21.396(4) _cell_length_c 11.757(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.477(2) _cell_angle_gamma 90.00 _cell_volume 2797.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 2.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3646 _exptl_absorpt_correction_T_max 0.4189 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15602 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.07 _reflns_number_total 5515 _reflns_number_gt 3747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5515 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0623 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.23725(2) 0.157557(11) 0.45785(2) 0.02104(7) Uani 1 1 d . . . N1 N 0.21461(19) 0.06703(9) 0.31470(18) 0.0259(5) Uani 1 1 d . . . N2 N 0.38844(19) 0.24819(9) 0.45556(17) 0.0252(5) Uani 1 1 d . . . N3 N 0.06392(18) 0.12272(9) 0.58461(16) 0.0211(5) Uani 1 1 d . . . C1 C 0.4105(2) 0.08661(12) 0.4805(2) 0.0311(7) Uani 1 1 d . . . H1A H 0.4793 0.1055 0.5253 0.037 Uiso 1 1 calc R . . H1B H 0.3894 0.0459 0.5140 0.037 Uiso 1 1 calc R . . C2 C 0.4317(2) 0.08181(11) 0.3580(2) 0.0270(6) Uani 1 1 d . . . C3 C 0.3362(2) 0.07505(11) 0.2747(2) 0.0246(6) Uani 1 1 d . . . C4 C 0.3558(2) 0.07745(11) 0.1582(2) 0.0308(7) Uani 1 1 d . . . H4 H 0.2900 0.0729 0.1036 0.037 Uiso 1 1 calc R . . C5 C 0.4705(3) 0.08645(12) 0.1225(2) 0.0368(8) Uani 1 1 d . . . H5 H 0.4837 0.0882 0.0435 0.044 Uiso 1 1 calc R . . C6 C 0.5657(3) 0.09293(12) 0.2026(3) 0.0381(8) Uani 1 1 d . . . H6 H 0.6446 0.0994 0.1785 0.046 Uiso 1 1 calc R . . C7 C 0.5470(2) 0.09013(12) 0.3173(2) 0.0335(7) Uani 1 1 d . . . H7 H 0.6140 0.0939 0.3707 0.040 Uiso 1 1 calc R . . C8 C 0.1170(2) 0.07704(12) 0.2253(2) 0.0332(7) Uani 1 1 d . . . H8A H 0.1259 0.1184 0.1911 0.050 Uiso 1 1 calc R . . H8B H 0.0390 0.0744 0.2594 0.050 Uiso 1 1 calc R . . H8C H 0.1214 0.0449 0.1664 0.050 Uiso 1 1 calc R . . C9 C 0.1997(3) 0.00236(11) 0.3596(2) 0.0344(7) Uani 1 1 d . . . H9A H 0.1942 -0.0273 0.2960 0.052 Uiso 1 1 calc R . . H9B H 0.1261 0.0002 0.4010 0.052 Uiso 1 1 calc R . . H9C H 0.2691 -0.0082 0.4113 0.052 Uiso 1 1 calc R . . C10 C 0.1925(2) 0.22884(10) 0.2985(2) 0.0246(6) Uani 1 1 d . . . H10A H 0.2456 0.2204 0.2357 0.029 Uiso 1 1 calc R . . H10B H 0.1077 0.2246 0.2692 0.029 Uiso 1 1 calc R . . C11 C 0.2154(2) 0.29193(11) 0.3470(2) 0.0231(6) Uani 1 1 d . . . C12 C 0.3121(2) 0.30250(12) 0.4278(2) 0.0238(6) Uani 1 1 d . . . C13 C 0.3320(2) 0.36072(12) 0.4776(2) 0.0321(7) Uani 1 1 d . . . H13 H 0.3984 0.3667 0.5311 0.039 Uiso 1 1 calc R . . C14 C 0.2556(3) 0.41018(13) 0.4496(2) 0.0387(8) Uani 1 1 d . . . H14 H 0.2692 0.4499 0.4840 0.046 Uiso 1 1 calc R . . C15 C 0.1592(3) 0.40131(13) 0.3712(2) 0.0352(7) Uani 1 1 d . . . H15 H 0.1062 0.4349 0.3520 0.042 Uiso 1 1 calc R . . C16 C 0.1404(2) 0.34351(12) 0.3210(2) 0.0275(6) Uani 1 1 d . . . H16 H 0.0744 0.3384 0.2668 0.033 Uiso 1 1 calc R . . C17 C 0.4778(2) 0.24123(12) 0.3667(2) 0.0332(7) Uani 1 1 d . . . H17A H 0.4353 0.2340 0.2924 0.050 Uiso 1 1 calc R . . H17B H 0.5306 0.2057 0.3859 0.050 Uiso 1 1 calc R . . H17C H 0.5260 0.2794 0.3636 0.050 Uiso 1 1 calc R . . C18 C 0.4591(3) 0.25356(13) 0.5663(2) 0.0410(8) Uani 1 1 d . . . H18A H 0.5184 0.2872 0.5618 0.061 Uiso 1 1 calc R . . H18B H 0.5007 0.2140 0.5835 0.061 Uiso 1 1 calc R . . H18C H 0.4049 0.2630 0.6266 0.061 Uiso 1 1 calc R . . C19 C 0.0302(2) 0.18265(11) 0.5524(2) 0.0204(6) Uani 1 1 d . . . C20 C 0.1102(2) 0.22610(11) 0.6039(2) 0.0226(6) Uani 1 1 d . . . H20 H 0.1083 0.2702 0.5941 0.027 Uiso 1 1 calc R . . C21 C 0.1943(2) 0.19162(11) 0.6733(2) 0.0234(6) Uani 1 1 d . . . H21 H 0.2603 0.2081 0.7188 0.028 Uiso 1 1 calc R . . C22 C 0.1617(2) 0.12854(11) 0.6624(2) 0.0210(6) Uani 1 1 d . . . C23 C -0.0913(2) 0.19380(11) 0.4896(2) 0.0226(6) Uani 1 1 d . . . C24 C -0.1114(2) 0.26363(11) 0.4680(2) 0.0343(7) Uani 1 1 d . . . H24A H -0.1055 0.2861 0.5407 0.052 Uiso 1 1 calc R . . H24B H -0.1915 0.2701 0.4305 0.052 Uiso 1 1 calc R . . H24C H -0.0502 0.2794 0.4188 0.052 Uiso 1 1 calc R . . C25 C -0.1039(2) 0.15801(13) 0.3772(2) 0.0340(6) Uani 1 1 d . . . H25A H -0.0459 0.1743 0.3251 0.051 Uiso 1 1 calc R . . H25B H -0.1857 0.1633 0.3429 0.051 Uiso 1 1 calc R . . H25C H -0.0882 0.1135 0.3914 0.051 Uiso 1 1 calc R . . C26 C -0.1888(2) 0.16979(11) 0.5663(2) 0.0305(7) Uani 1 1 d . . . H26A H -0.1784 0.1248 0.5787 0.046 Uiso 1 1 calc R . . H26B H -0.2685 0.1778 0.5292 0.046 Uiso 1 1 calc R . . H26C H -0.1815 0.1916 0.6397 0.046 Uiso 1 1 calc R . . C27 C 0.2007(2) 0.07434(11) 0.7399(2) 0.0233(6) Uani 1 1 d . . . C28 C 0.1218(3) 0.07752(13) 0.8430(2) 0.0405(8) Uani 1 1 d . . . H28A H 0.1395 0.1161 0.8857 0.061 Uiso 1 1 calc R . . H28B H 0.1389 0.0414 0.8926 0.061 Uiso 1 1 calc R . . H28C H 0.0367 0.0771 0.8162 0.061 Uiso 1 1 calc R . . C29 C 0.3334(2) 0.07967(12) 0.7821(2) 0.0325(7) Uani 1 1 d . . . H29A H 0.3839 0.0794 0.7166 0.049 Uiso 1 1 calc R . . H29B H 0.3551 0.0442 0.8320 0.049 Uiso 1 1 calc R . . H29C H 0.3460 0.1188 0.8246 0.049 Uiso 1 1 calc R . . C30 C 0.1791(2) 0.01127(11) 0.6800(2) 0.0297(7) Uani 1 1 d . . . H30A H 0.0954 0.0089 0.6493 0.045 Uiso 1 1 calc R . . H30B H 0.1949 -0.0227 0.7348 0.045 Uiso 1 1 calc R . . H30C H 0.2331 0.0073 0.6177 0.045 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 Y1 0.02073(13) 0.02262(13) 0.01960(13) -0.00015(14) -0.00010(9) -0.00027(14) N1 0.0238(14) 0.0264(13) 0.0278(13) -0.0034(10) 0.0030(10) -0.0010(10) N2 0.0227(13) 0.0302(13) 0.0219(13) 0.0019(10) -0.0053(10) -0.0056(10) N3 0.0201(13) 0.0232(12) 0.0198(12) -0.0001(10) 0.0008(10) 0.0006(10) C1 0.0297(17) 0.0339(17) 0.0291(17) -0.0002(13) -0.0033(13) 0.0025(13) C2 0.0272(17) 0.0188(14) 0.0352(17) -0.0013(12) 0.0041(13) 0.0067(12) C3 0.0271(17) 0.0171(14) 0.0301(17) -0.0018(12) 0.0066(13) 0.0016(12) C4 0.0348(19) 0.0249(16) 0.0330(17) -0.0010(13) 0.0042(14) 0.0018(13) C5 0.044(2) 0.0332(17) 0.0353(18) 0.0067(14) 0.0155(16) 0.0060(15) C6 0.0304(19) 0.0324(17) 0.053(2) 0.0049(15) 0.0168(16) 0.0063(14) C7 0.0235(17) 0.0330(16) 0.0439(19) -0.0014(14) 0.0008(14) 0.0061(13) C8 0.0305(18) 0.0334(17) 0.0357(18) -0.0097(14) 0.0011(14) -0.0023(14) C9 0.0401(19) 0.0292(16) 0.0345(18) -0.0051(13) 0.0074(14) -0.0056(14) C10 0.0223(16) 0.0269(15) 0.0242(15) 0.0005(12) -0.0010(12) -0.0070(12) C11 0.0230(16) 0.0287(16) 0.0180(15) 0.0050(12) 0.0036(12) -0.0051(12) C12 0.0254(16) 0.0262(16) 0.0203(15) 0.0018(12) 0.0049(12) -0.0045(12) C13 0.0337(18) 0.0332(18) 0.0296(16) -0.0030(13) 0.0024(13) -0.0126(13) C14 0.047(2) 0.0266(16) 0.0440(19) -0.0071(15) 0.0132(16) -0.0076(15) C15 0.0337(19) 0.0298(17) 0.0433(19) 0.0052(14) 0.0134(15) 0.0021(14) C16 0.0260(15) 0.0294(15) 0.0275(15) 0.0052(14) 0.0036(11) -0.0001(14) C17 0.0236(16) 0.0347(17) 0.0413(18) 0.0050(14) 0.0024(14) -0.0006(13) C18 0.041(2) 0.0452(18) 0.0343(18) 0.0095(15) -0.0149(15) -0.0138(15) C19 0.0239(16) 0.0212(14) 0.0163(14) 0.0003(11) 0.0037(12) 0.0018(12) C20 0.0274(16) 0.0183(14) 0.0226(15) -0.0011(12) 0.0054(12) 0.0004(12) C21 0.0216(16) 0.0279(16) 0.0207(15) -0.0027(12) 0.0015(12) -0.0028(12) C22 0.0192(15) 0.0245(15) 0.0195(15) -0.0010(12) 0.0032(12) 0.0017(12) C23 0.0200(15) 0.0234(14) 0.0245(15) 0.0017(12) 0.0009(12) 0.0006(12) C24 0.0285(17) 0.0312(16) 0.0426(18) 0.0070(14) -0.0038(14) 0.0027(13) C25 0.0225(15) 0.0477(17) 0.0312(15) -0.0072(16) -0.0029(12) 0.0013(15) C26 0.0246(15) 0.0335(17) 0.0336(16) 0.0029(13) 0.0029(12) -0.0004(12) C27 0.0253(16) 0.0233(15) 0.0207(15) 0.0021(12) -0.0026(12) 0.0003(12) C28 0.048(2) 0.0408(18) 0.0330(18) 0.0161(14) 0.0072(15) 0.0086(15) C29 0.0342(18) 0.0273(16) 0.0350(18) 0.0033(13) -0.0066(14) 0.0019(13) C30 0.0250(17) 0.0272(16) 0.0362(17) 0.0096(13) -0.0051(13) 0.0008(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 Y1 C10 2.443(2) . ? Y1 C1 2.457(3) . ? Y1 N1 2.568(2) . ? Y1 N2 2.570(2) . ? Y1 N3 2.6180(19) . ? Y1 C22 2.669(2) . ? Y1 C19 2.675(2) . ? Y1 C21 2.706(2) . ? Y1 C20 2.720(2) . ? Y1 C2 3.001(2) . ? Y1 C3 3.043(2) . ? N1 C3 1.471(3) . ? N1 C8 1.481(3) . ? N1 C9 1.494(3) . ? N2 C12 1.465(3) . ? N2 C18 1.484(3) . ? N2 C17 1.493(3) . ? N3 C19 1.382(3) . ? N3 C22 1.385(3) . ? C1 C2 1.477(3) . ? C2 C7 1.408(3) . ? C2 C3 1.410(3) . ? C3 C4 1.400(3) . ? C4 C5 1.382(3) . ? C5 C6 1.383(4) . ? C6 C7 1.378(3) . ? C10 C11 1.481(3) . ? C11 C16 1.406(3) . ? C11 C12 1.411(3) . ? C12 C13 1.388(3) . ? C13 C14 1.385(4) . ? C14 C15 1.384(4) . ? C15 C16 1.381(3) . ? C19 C20 1.400(3) . ? C19 C23 1.521(3) . ? C20 C21 1.412(3) . ? C21 C22 1.401(3) . ? C22 C27 1.522(3) . ? C23 C25 1.527(3) . ? C23 C24 1.530(3) . ? C23 C26 1.541(3) . ? C27 C30 1.534(3) . ? C27 C29 1.535(3) . ? C27 C28 1.541(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 C10 Y1 C1 126.23(8) . . ? C10 Y1 N1 87.77(8) . . ? C1 Y1 N1 69.53(8) . . ? C10 Y1 N2 67.93(7) . . ? C1 Y1 N2 87.50(8) . . ? N1 Y1 N2 126.91(6) . . ? C10 Y1 N3 119.41(7) . . ? C1 Y1 N3 111.35(7) . . ? N1 Y1 N3 96.42(6) . . ? N2 Y1 N3 136.66(6) . . ? C10 Y1 C22 140.84(8) . . ? C1 Y1 C22 92.70(8) . . ? N1 Y1 C22 113.03(7) . . ? N2 Y1 C22 115.32(7) . . ? N3 Y1 C22 30.36(6) . . ? C10 Y1 C19 93.01(8) . . ? C1 Y1 C19 140.38(8) . . ? N1 Y1 C19 111.77(7) . . ? N2 Y1 C19 115.79(7) . . ? N3 Y1 C19 30.26(6) . . ? C22 Y1 C19 49.10(7) . . ? C10 Y1 C21 120.67(8) . . ? C1 Y1 C21 104.33(8) . . ? N1 Y1 C21 143.18(7) . . ? N2 Y1 C21 87.70(7) . . ? N3 Y1 C21 50.61(7) . . ? C22 Y1 C21 30.21(7) . . ? C19 Y1 C21 49.52(7) . . ? C10 Y1 C20 93.31(8) . . ? C1 Y1 C20 134.44(8) . . ? N1 Y1 C20 141.83(7) . . ? N2 Y1 C20 88.07(7) . . ? N3 Y1 C20 50.51(7) . . ? C22 Y1 C20 49.61(7) . . ? C19 Y1 C20 30.06(7) . . ? C21 Y1 C20 30.17(7) . . ? C10 Y1 C2 98.96(8) . . ? C1 Y1 C2 29.29(7) . . ? N1 Y1 C2 51.75(7) . . ? N2 Y1 C2 85.08(7) . . ? N3 Y1 C2 130.07(7) . . ? C22 Y1 C2 120.09(7) . . ? C19 Y1 C2 158.76(7) . . ? C21 Y1 C2 133.20(8) . . ? C20 Y1 C2 162.52(8) . . ? C10 Y1 C3 83.41(8) . . ? C1 Y1 C3 53.29(8) . . ? N1 Y1 C3 28.84(6) . . ? N2 Y1 C3 99.47(7) . . ? N3 Y1 C3 123.31(6) . . ? C22 Y1 C3 130.57(7) . . ? C19 Y1 C3 140.28(7) . . ? C21 Y1 C3 155.65(7) . . ? C20 Y1 C3 169.89(8) . . ? C2 Y1 C3 26.96(7) . . ? C3 N1 C8 114.0(2) . . ? C3 N1 C9 110.2(2) . . ? C8 N1 C9 107.0(2) . . ? C3 N1 Y1 93.78(14) . . ? C8 N1 Y1 113.22(14) . . ? C9 N1 Y1 118.40(15) . . ? C12 N2 C18 113.8(2) . . ? C12 N2 C17 109.01(19) . . ? C18 N2 C17 106.3(2) . . ? C12 N2 Y1 103.24(14) . . ? C18 N2 Y1 111.25(15) . . ? C17 N2 Y1 113.40(15) . . ? C19 N3 C22 106.7(2) . . ? C19 N3 Y1 77.14(13) . . ? C22 N3 Y1 76.85(13) . . ? C2 C1 Y1 96.24(16) . . ? C7 C2 C3 116.2(2) . . ? C7 C2 C1 121.7(3) . . ? C3 C2 C1 121.7(2) . . ? C7 C2 Y1 139.39(18) . . ? C3 C2 Y1 78.17(15) . . ? C1 C2 Y1 54.47(13) . . ? C4 C3 C2 121.3(2) . . ? C4 C3 N1 121.2(2) . . ? C2 C3 N1 117.4(2) . . ? C4 C3 Y1 139.06(17) . . ? C2 C3 Y1 74.87(14) . . ? N1 C3 Y1 57.38(11) . . ? C5 C4 C3 120.2(3) . . ? C4 C5 C6 119.5(3) . . ? C7 C6 C5 120.4(3) . . ? C6 C7 C2 122.2(3) . . ? C11 C10 Y1 104.59(16) . . ? C16 C11 C12 116.1(2) . . ? C16 C11 C10 123.1(2) . . ? C12 C11 C10 120.8(2) . . ? C13 C12 C11 121.6(3) . . ? C13 C12 N2 122.8(2) . . ? C11 C12 N2 115.6(2) . . ? C14 C13 C12 120.3(3) . . ? C15 C14 C13 119.6(3) . . ? C16 C15 C14 119.9(3) . . ? C15 C16 C11 122.5(3) . . ? N3 C19 C20 110.0(2) . . ? N3 C19 C23 119.8(2) . . ? C20 C19 C23 129.1(2) . . ? N3 C19 Y1 72.60(13) . . ? C20 C19 Y1 76.76(14) . . ? C23 C19 Y1 126.46(15) . . ? C19 C20 C21 106.6(2) . . ? C19 C20 Y1 73.18(13) . . ? C21 C20 Y1 74.38(13) . . ? C22 C21 C20 107.0(2) . . ? C22 C21 Y1 73.41(14) . . ? C20 C21 Y1 75.45(14) . . ? N3 C22 C21 109.6(2) . . ? N3 C22 C27 120.7(2) . . ? C21 C22 C27 128.1(2) . . ? N3 C22 Y1 72.79(13) . . ? C21 C22 Y1 76.38(14) . . ? C27 C22 Y1 128.53(16) . . ? C19 C23 C25 112.0(2) . . ? C19 C23 C24 110.6(2) . . ? C25 C23 C24 109.9(2) . . ? C19 C23 C26 107.6(2) . . ? C25 C23 C26 107.9(2) . . ? C24 C23 C26 108.7(2) . . ? C22 C27 C30 111.4(2) . . ? C22 C27 C29 111.8(2) . . ? C30 C27 C29 109.6(2) . . ? C22 C27 C28 106.4(2) . . ? C30 C27 C28 108.6(2) . . ? C29 C27 C28 109.1(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.692 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.058