# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Cationic scandium aminobenzyl complexes. synthesis, structure, and unprecedented catalysis of copolymerization of 1-hexene and dicyclopentadiene ; _publ_contact_author_name 'Zhaomin Hou' _publ_contact_author_email HOUZ@RIKEN.JP loop_ _publ_author_name 'Xiaofang Li' M.Nishiura K.Mori T.Mashiko 'Zhaomin Hou' # Attachment '1a.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 637040' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cp'ScBz2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H45 N2 Sc Si' _chemical_formula_weight 506.73 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' Si Si 0.0817 0.0704 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.299(2) _cell_length_b 10.594(2) _cell_length_c 13.624(3) _cell_angle_alpha 91.641(3) _cell_angle_beta 95.407(2) _cell_angle_gamma 106.911(2) _cell_volume 1413.3(5) _cell_formula_units_Z 2 _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 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 0.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8954 _exptl_absorpt_correction_T_max 0.9382 _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 7426 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4888 _reflns_number_gt 3684 _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^)+(0.0400P)^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 4888 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 0.75449(4) 0.34759(4) 0.21700(3) 0.02149(12) Uani 1 1 d . . . Si1 Si 0.76350(8) 0.72125(7) 0.29398(5) 0.03605(19) Uani 1 1 d . . . N1 N 0.91644(18) 0.26051(18) 0.13035(13) 0.0264(4) Uani 1 1 d . . . N2 N 0.50934(18) 0.29960(18) 0.17059(14) 0.0264(4) Uani 1 1 d . . . C1 C 0.7794(2) 0.4389(2) 0.06709(16) 0.0280(5) Uani 1 1 d . . . H1A H 0.7043 0.4768 0.0472 0.034 Uiso 1 1 calc R . . H1B H 0.8678 0.5088 0.0684 0.034 Uiso 1 1 calc R . . C2 C 0.7743(2) 0.3253(2) 0.00007(16) 0.0264(5) Uani 1 1 d . . . C3 C 0.8400(2) 0.2315(2) 0.03206(17) 0.0263(5) Uani 1 1 d . . . C4 C 0.8317(2) 0.1210(2) -0.02721(18) 0.0343(6) Uani 1 1 d . . . H4 H 0.8786 0.0604 -0.0047 0.041 Uiso 1 1 calc R . . C5 C 0.7562(3) 0.0972(2) -0.11876(19) 0.0395(6) Uani 1 1 d . . . H5 H 0.7512 0.0209 -0.1591 0.047 Uiso 1 1 calc R . . C6 C 0.6885(2) 0.1854(3) -0.15092(18) 0.0370(6) Uani 1 1 d . . . H6 H 0.6350 0.1693 -0.2132 0.044 Uiso 1 1 calc R . . C7 C 0.6986(2) 0.2966(2) -0.09266(17) 0.0317(6) Uani 1 1 d . . . H7 H 0.6518 0.3566 -0.1165 0.038 Uiso 1 1 calc R . . C8 C 1.0526(2) 0.3542(2) 0.11965(18) 0.0336(6) Uani 1 1 d . . . H8A H 1.1027 0.3114 0.0786 0.050 Uiso 1 1 calc R . . H8B H 1.1040 0.3801 0.1850 0.050 Uiso 1 1 calc R . . H8C H 1.0408 0.4329 0.0883 0.050 Uiso 1 1 calc R . . C9 C 0.9396(2) 0.1420(2) 0.17485(18) 0.0339(6) Uani 1 1 d . . . H9A H 0.8530 0.0712 0.1707 0.051 Uiso 1 1 calc R . . H9B H 0.9764 0.1638 0.2443 0.051 Uiso 1 1 calc R . . H9C H 1.0048 0.1125 0.1391 0.051 Uiso 1 1 calc R . . C10 C 0.6501(2) 0.1317(2) 0.24514(17) 0.0264(5) Uani 1 1 d . . . H10A H 0.6307 0.0757 0.1829 0.032 Uiso 1 1 calc R . . H10B H 0.7085 0.0980 0.2931 0.032 Uiso 1 1 calc R . . C11 C 0.5216(2) 0.1317(2) 0.28557(16) 0.0240(5) Uani 1 1 d . . . C12 C 0.4496(2) 0.2177(2) 0.24890(16) 0.0242(5) Uani 1 1 d . . . C13 C 0.3303(2) 0.2231(2) 0.28506(17) 0.0305(6) Uani 1 1 d . . . H13 H 0.2827 0.2807 0.2578 0.037 Uiso 1 1 calc R . . C14 C 0.2798(2) 0.1453(2) 0.36068(18) 0.0360(6) Uani 1 1 d . . . H14 H 0.1975 0.1488 0.3853 0.043 Uiso 1 1 calc R . . C15 C 0.3498(2) 0.0627(2) 0.39999(18) 0.0353(6) Uani 1 1 d . . . H15 H 0.3166 0.0099 0.4526 0.042 Uiso 1 1 calc R . . C16 C 0.4682(2) 0.0565(2) 0.36299(17) 0.0288(5) Uani 1 1 d . . . H16 H 0.5151 -0.0010 0.3912 0.035 Uiso 1 1 calc R . . C17 C 0.4690(2) 0.4219(2) 0.16266(19) 0.0363(6) Uani 1 1 d . . . H17A H 0.3722 0.3997 0.1377 0.054 Uiso 1 1 calc R . . H17B H 0.5240 0.4790 0.1171 0.054 Uiso 1 1 calc R . . H17C H 0.4841 0.4683 0.2279 0.054 Uiso 1 1 calc R . . C18 C 0.4628(2) 0.2233(2) 0.07392(17) 0.0341(6) Uani 1 1 d . . . H18A H 0.4909 0.1425 0.0750 0.051 Uiso 1 1 calc R . . H18B H 0.5036 0.2772 0.0212 0.051 Uiso 1 1 calc R . . H18C H 0.3631 0.1998 0.0618 0.051 Uiso 1 1 calc R . . C19 C 0.8010(2) 0.5620(2) 0.31952(16) 0.0248(5) Uani 1 1 d . . . C20 C 0.7346(2) 0.4589(2) 0.37940(16) 0.0238(5) Uani 1 1 d . . . C21 C 0.8214(2) 0.3804(2) 0.40207(16) 0.0251(5) Uani 1 1 d . . . C22 C 0.9435(2) 0.4347(2) 0.35945(16) 0.0264(5) Uani 1 1 d . . . C23 C 0.9320(2) 0.5447(2) 0.30812(16) 0.0250(5) Uani 1 1 d . . . C24 C 0.6070(2) 0.4457(3) 0.42779(18) 0.0352(6) Uani 1 1 d . . . H24A H 0.5656 0.3529 0.4408 0.053 Uiso 1 1 calc R . . H24B H 0.5425 0.4760 0.3840 0.053 Uiso 1 1 calc R . . H24C H 0.6294 0.4996 0.4902 0.053 Uiso 1 1 calc R . . C25 C 0.7986(3) 0.2702(2) 0.47156(18) 0.0409(7) Uani 1 1 d . . . H25A H 0.8460 0.3044 0.5369 0.061 Uiso 1 1 calc R . . H25B H 0.8342 0.2007 0.4464 0.061 Uiso 1 1 calc R . . H25C H 0.7006 0.2335 0.4766 0.061 Uiso 1 1 calc R . . C26 C 1.0709(2) 0.3941(3) 0.38392(19) 0.0414(7) Uani 1 1 d . . . H26A H 1.1435 0.4453 0.3467 0.062 Uiso 1 1 calc R . . H26B H 1.0519 0.2997 0.3661 0.062 Uiso 1 1 calc R . . H26C H 1.1002 0.4109 0.4548 0.062 Uiso 1 1 calc R . . C27 C 1.0443(2) 0.6370(2) 0.25893(18) 0.0380(6) Uani 1 1 d . . . H27A H 1.0827 0.7192 0.3001 0.057 Uiso 1 1 calc R . . H27B H 1.0073 0.6565 0.1941 0.057 Uiso 1 1 calc R . . H27C H 1.1161 0.5951 0.2505 0.057 Uiso 1 1 calc R . . C28 C 0.8959(3) 0.8585(3) 0.3689(2) 0.0489(7) Uani 1 1 d . . . H28A H 0.8681 0.9394 0.3666 0.073 Uiso 1 1 calc R . . H28B H 0.9836 0.8735 0.3418 0.073 Uiso 1 1 calc R . . H28C H 0.9052 0.8343 0.4375 0.073 Uiso 1 1 calc R . . C29 C 0.7639(4) 0.7597(3) 0.1608(2) 0.0637(9) Uani 1 1 d . . . H29A H 0.7032 0.6840 0.1200 0.096 Uiso 1 1 calc R . . H29B H 0.8568 0.7779 0.1419 0.096 Uiso 1 1 calc R . . H29C H 0.7320 0.8374 0.1506 0.096 Uiso 1 1 calc R . . C30 C 0.5978(3) 0.7318(3) 0.3338(2) 0.0601(9) Uani 1 1 d . . . H30A H 0.5861 0.8179 0.3186 0.090 Uiso 1 1 calc R . . H30B H 0.5980 0.7215 0.4051 0.090 Uiso 1 1 calc R . . H30C H 0.5225 0.6614 0.2986 0.090 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 0.0239(2) 0.0215(2) 0.0192(2) 0.00136(18) 0.00143(17) 0.00714(19) Si1 0.0525(5) 0.0238(4) 0.0325(4) -0.0016(3) -0.0059(3) 0.0159(3) N1 0.0288(11) 0.0252(11) 0.0253(11) 0.0019(9) 0.0040(8) 0.0076(9) N2 0.0272(11) 0.0242(11) 0.0272(11) 0.0065(9) 0.0015(8) 0.0067(9) C1 0.0312(13) 0.0285(13) 0.0248(13) 0.0043(10) 0.0046(10) 0.0088(11) C2 0.0283(13) 0.0257(13) 0.0233(13) 0.0039(10) 0.0074(10) 0.0030(11) C3 0.0257(13) 0.0255(13) 0.0250(13) 0.0008(10) 0.0048(10) 0.0026(10) C4 0.0385(15) 0.0285(14) 0.0360(15) -0.0004(12) 0.0075(12) 0.0092(12) C5 0.0489(17) 0.0299(15) 0.0340(15) -0.0091(12) 0.0088(13) 0.0022(13) C6 0.0364(15) 0.0412(16) 0.0249(14) -0.0022(12) 0.0017(11) -0.0010(13) C7 0.0353(14) 0.0341(14) 0.0248(13) 0.0049(11) 0.0042(11) 0.0082(12) C8 0.0277(14) 0.0387(15) 0.0314(14) -0.0014(12) 0.0035(11) 0.0053(12) C9 0.0361(14) 0.0323(14) 0.0377(15) 0.0038(12) 0.0072(11) 0.0158(12) C10 0.0258(13) 0.0282(13) 0.0266(13) 0.0001(10) 0.0005(10) 0.0109(10) C11 0.0266(13) 0.0175(12) 0.0258(13) -0.0008(10) -0.0006(10) 0.0045(10) C12 0.0256(12) 0.0207(12) 0.0233(12) -0.0005(10) -0.0009(10) 0.0033(10) C13 0.0256(13) 0.0321(14) 0.0345(14) 0.0039(11) 0.0018(11) 0.0097(11) C14 0.0317(14) 0.0396(15) 0.0395(15) 0.0040(13) 0.0125(11) 0.0123(12) C15 0.0379(15) 0.0347(15) 0.0314(14) 0.0086(12) 0.0094(11) 0.0052(12) C16 0.0345(14) 0.0245(13) 0.0272(13) 0.0045(11) 0.0023(11) 0.0087(11) C17 0.0333(14) 0.0308(14) 0.0468(16) 0.0134(12) 0.0024(12) 0.0123(12) C18 0.0331(14) 0.0404(15) 0.0244(13) 0.0038(11) -0.0023(11) 0.0054(12) C19 0.0282(13) 0.0235(13) 0.0218(12) -0.0043(10) -0.0020(10) 0.0082(10) C20 0.0260(12) 0.0247(13) 0.0188(12) -0.0023(10) 0.0004(9) 0.0055(10) C21 0.0319(13) 0.0227(12) 0.0182(12) -0.0016(10) -0.0031(10) 0.0063(10) C22 0.0273(13) 0.0297(13) 0.0215(12) -0.0074(10) -0.0046(10) 0.0107(11) C23 0.0274(13) 0.0240(12) 0.0207(12) -0.0046(10) 0.0003(10) 0.0043(10) C24 0.0334(14) 0.0443(16) 0.0275(14) -0.0030(12) 0.0053(11) 0.0105(12) C25 0.0564(18) 0.0343(15) 0.0281(14) 0.0040(12) -0.0073(12) 0.0106(13) C26 0.0385(15) 0.0502(17) 0.0385(16) -0.0127(13) -0.0106(12) 0.0237(14) C27 0.0373(15) 0.0349(15) 0.0343(15) -0.0033(12) 0.0069(12) -0.0016(12) C28 0.065(2) 0.0300(15) 0.0496(18) -0.0054(13) -0.0063(15) 0.0157(14) C29 0.116(3) 0.0323(16) 0.0406(18) 0.0043(14) -0.0114(18) 0.0248(18) C30 0.062(2) 0.0423(18) 0.082(2) -0.0156(16) -0.0113(17) 0.0323(16) _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 C10 2.287(2) . ? Sc1 C1 2.289(2) . ? Sc1 N2 2.4427(19) . ? Sc1 N1 2.4960(19) . ? Sc1 C19 2.529(2) . ? Sc1 C20 2.531(2) . ? Sc1 C21 2.537(2) . ? Sc1 C23 2.539(2) . ? Sc1 C22 2.559(2) . ? Si1 C30 1.871(3) . ? Si1 C29 1.872(3) . ? Si1 C19 1.872(2) . ? Si1 C28 1.875(3) . ? N1 C3 1.465(3) . ? N1 C9 1.480(3) . ? N1 C8 1.486(3) . ? N2 C12 1.461(3) . ? N2 C17 1.475(3) . ? N2 C18 1.487(3) . ? C1 C2 1.475(3) . ? C2 C7 1.397(3) . ? C2 C3 1.412(3) . ? C3 C4 1.380(3) . ? C4 C5 1.382(3) . ? C5 C6 1.376(3) . ? C6 C7 1.374(3) . ? C10 C11 1.480(3) . ? C11 C16 1.397(3) . ? C11 C12 1.407(3) . ? C12 C13 1.381(3) . ? C13 C14 1.383(3) . ? C14 C15 1.376(3) . ? C15 C16 1.380(3) . ? C19 C20 1.431(3) . ? C19 C23 1.435(3) . ? C20 C21 1.407(3) . ? C20 C24 1.498(3) . ? C21 C22 1.409(3) . ? C21 C25 1.504(3) . ? C22 C23 1.404(3) . ? C22 C26 1.508(3) . ? C23 C27 1.506(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 Sc1 C1 127.11(9) . . ? C10 Sc1 N2 71.33(7) . . ? C1 Sc1 N2 85.73(7) . . ? C10 Sc1 N1 85.60(7) . . ? C1 Sc1 N1 70.85(7) . . ? N2 Sc1 N1 126.68(7) . . ? C10 Sc1 C19 133.11(8) . . ? C1 Sc1 C19 96.79(8) . . ? N2 Sc1 C19 100.11(7) . . ? N1 Sc1 C19 128.99(7) . . ? C10 Sc1 C20 100.27(8) . . ? C1 Sc1 C20 127.75(8) . . ? N2 Sc1 C20 90.72(7) . . ? N1 Sc1 C20 141.45(7) . . ? C19 Sc1 C20 32.85(7) . . ? C10 Sc1 C21 86.15(8) . . ? C1 Sc1 C21 146.34(8) . . ? N2 Sc1 C21 113.48(7) . . ? N1 Sc1 C21 112.01(7) . . ? C19 Sc1 C21 54.18(7) . . ? C20 Sc1 C21 32.24(7) . . ? C10 Sc1 C23 137.46(8) . . ? C1 Sc1 C23 93.03(8) . . ? N2 Sc1 C23 132.59(7) . . ? N1 Sc1 C23 96.84(7) . . ? C19 Sc1 C23 32.89(7) . . ? C20 Sc1 C23 53.73(7) . . ? C21 Sc1 C23 53.47(7) . . ? C10 Sc1 C22 106.21(8) . . ? C1 Sc1 C22 119.22(8) . . ? N2 Sc1 C22 143.46(7) . . ? N1 Sc1 C22 88.46(7) . . ? C19 Sc1 C22 53.85(7) . . ? C20 Sc1 C22 53.19(7) . . ? C21 Sc1 C22 32.10(7) . . ? C23 Sc1 C22 31.98(7) . . ? C30 Si1 C29 107.21(15) . . ? C30 Si1 C19 114.40(12) . . ? C29 Si1 C19 113.33(12) . . ? C30 Si1 C28 104.28(13) . . ? C29 Si1 C28 108.64(14) . . ? C19 Si1 C28 108.49(11) . . ? C3 N1 C9 113.04(18) . . ? C3 N1 C8 107.59(17) . . ? C9 N1 C8 107.37(17) . . ? C3 N1 Sc1 98.89(12) . . ? C9 N1 Sc1 112.58(13) . . ? C8 N1 Sc1 117.23(14) . . ? C12 N2 C17 113.61(18) . . ? C12 N2 C18 109.08(17) . . ? C17 N2 C18 106.76(17) . . ? C12 N2 Sc1 103.11(12) . . ? C17 N2 Sc1 111.48(13) . . ? C18 N2 Sc1 112.91(14) . . ? C2 C1 Sc1 102.99(14) . . ? C7 C2 C3 115.9(2) . . ? C7 C2 C1 124.2(2) . . ? C3 C2 C1 119.7(2) . . ? C4 C3 C2 121.1(2) . . ? C4 C3 N1 123.3(2) . . ? C2 C3 N1 115.6(2) . . ? C3 C4 C5 121.0(2) . . ? C6 C5 C4 119.3(2) . . ? C7 C6 C5 119.8(2) . . ? C6 C7 C2 123.0(2) . . ? C11 C10 Sc1 105.30(14) . . ? C16 C11 C12 116.0(2) . . ? C16 C11 C10 124.6(2) . . ? C12 C11 C10 119.29(19) . . ? C13 C12 C11 121.6(2) . . ? C13 C12 N2 122.85(19) . . ? C11 C12 N2 115.50(18) . . ? C12 C13 C14 120.4(2) . . ? C15 C14 C13 119.4(2) . . ? C14 C15 C16 120.1(2) . . ? C15 C16 C11 122.5(2) . . ? C20 C19 C23 106.15(18) . . ? C20 C19 Si1 129.22(17) . . ? C23 C19 Si1 121.74(16) . . ? C20 C19 Sc1 73.62(12) . . ? C23 C19 Sc1 73.92(13) . . ? Si1 C19 Sc1 132.57(11) . . ? C21 C20 C19 108.78(19) . . ? C21 C20 C24 122.6(2) . . ? C19 C20 C24 127.7(2) . . ? C21 C20 Sc1 74.13(13) . . ? C19 C20 Sc1 73.53(12) . . ? C24 C20 Sc1 126.96(16) . . ? C20 C21 C22 108.03(19) . . ? C20 C21 C25 126.5(2) . . ? C22 C21 C25 124.9(2) . . ? C20 C21 Sc1 73.63(12) . . ? C22 C21 Sc1 74.80(13) . . ? C25 C21 Sc1 124.23(15) . . ? C23 C22 C21 108.52(19) . . ? C23 C22 C26 127.2(2) . . ? C21 C22 C26 123.3(2) . . ? C23 C22 Sc1 73.23(12) . . ? C21 C22 Sc1 73.10(13) . . ? C26 C22 Sc1 128.64(16) . . ? C22 C23 C19 108.49(19) . . ? C22 C23 C27 125.3(2) . . ? C19 C23 C27 125.9(2) . . ? C22 C23 Sc1 74.79(13) . . ? C19 C23 Sc1 73.19(13) . . ? C27 C23 Sc1 123.06(15) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.299 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.050 # Attachment '1b.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 637041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cp*ScBz2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H39 N2 Sc' _chemical_formula_weight 448.57 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 13.670(3) _cell_length_b 11.343(2) _cell_length_c 16.507(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.449(3) _cell_angle_gamma 90.00 _cell_volume 2524.9(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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.308 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8488 _exptl_absorpt_correction_T_max 0.8866 _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 13168 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.09 _reflns_number_total 4966 _reflns_number_gt 3803 _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^)+(0.0600P)^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 4966 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.73583(2) 0.61603(3) 0.83294(2) 0.02665(11) Uani 1 1 d . . . N1 N 0.82465(11) 0.42602(13) 0.86256(10) 0.0366(4) Uani 1 1 d . . . N2 N 0.67350(11) 0.74218(13) 0.93173(9) 0.0322(4) Uani 1 1 d . . . C1 C 0.62579(13) 0.47565(16) 0.86463(12) 0.0376(4) Uani 1 1 d . . . H1A H 0.5653 0.5124 0.8791 0.045 Uiso 1 1 calc R . . H1B H 0.6068 0.4198 0.8186 0.045 Uiso 1 1 calc R . . C2 C 0.68465(14) 0.41710(15) 0.93607(12) 0.0360(4) Uani 1 1 d . . . C3 C 0.64733(17) 0.38984(17) 1.00810(14) 0.0466(5) Uani 1 1 d . . . H3 H 0.5785 0.3999 1.0087 0.056 Uiso 1 1 calc R . . C4 C 0.7068(2) 0.34898(19) 1.07820(14) 0.0555(6) Uani 1 1 d . . . H4 H 0.6789 0.3320 1.1259 0.067 Uiso 1 1 calc R . . C5 C 0.80686(19) 0.33295(19) 1.07864(14) 0.0558(6) Uani 1 1 d . . . H5 H 0.8484 0.3062 1.1270 0.067 Uiso 1 1 calc R . . C6 C 0.84659(16) 0.35603(17) 1.00816(13) 0.0438(5) Uani 1 1 d . . . H6 H 0.9152 0.3431 1.0080 0.053 Uiso 1 1 calc R . . C7 C 0.78715(14) 0.39770(15) 0.93828(12) 0.0333(4) Uani 1 1 d . . . C8 C 0.79867(18) 0.32759(18) 0.80275(13) 0.0519(6) Uani 1 1 d . . . H8A H 0.7274 0.3115 0.7965 0.078 Uiso 1 1 calc R . . H8B H 0.8358 0.2567 0.8231 0.078 Uiso 1 1 calc R . . H8C H 0.8158 0.3500 0.7495 0.078 Uiso 1 1 calc R . . C9 C 0.93380(15) 0.4393(2) 0.87489(15) 0.0514(6) Uani 1 1 d . . . H9A H 0.9651 0.3627 0.8893 0.077 Uiso 1 1 calc R . . H9B H 0.9547 0.4956 0.9194 0.077 Uiso 1 1 calc R . . H9C H 0.9538 0.4684 0.8242 0.077 Uiso 1 1 calc R . . C10 C 0.86926(14) 0.70107(16) 0.91471(12) 0.0380(5) Uani 1 1 d . . . H10A H 0.8851 0.6592 0.9679 0.046 Uiso 1 1 calc R . . H10B H 0.9284 0.7002 0.8873 0.046 Uiso 1 1 calc R . . C11 C 0.83664(14) 0.82347(17) 0.92676(11) 0.0369(5) Uani 1 1 d . . . C12 C 0.89793(17) 0.92284(19) 0.92577(13) 0.0485(6) Uani 1 1 d . . . H12 H 0.9652 0.9119 0.9196 0.058 Uiso 1 1 calc R . . C13 C 0.8632(2) 1.03588(19) 0.93350(14) 0.0572(6) Uani 1 1 d . . . H13 H 0.9065 1.1011 0.9324 0.069 Uiso 1 1 calc R . . C14 C 0.7662(2) 1.05484(19) 0.94285(14) 0.0563(6) Uani 1 1 d . . . H14 H 0.7426 1.1327 0.9486 0.068 Uiso 1 1 calc R . . C15 C 0.70371(17) 0.95958(17) 0.94374(12) 0.0458(5) Uani 1 1 d . . . H15 H 0.6368 0.9718 0.9506 0.055 Uiso 1 1 calc R . . C16 C 0.73807(15) 0.84584(16) 0.93471(11) 0.0347(4) Uani 1 1 d . . . C17 C 0.56734(14) 0.76906(19) 0.90713(14) 0.0462(5) Uani 1 1 d . . . H17A H 0.5580 0.8167 0.8569 0.069 Uiso 1 1 calc R . . H17B H 0.5435 0.8130 0.9512 0.069 Uiso 1 1 calc R . . H17C H 0.5299 0.6954 0.8969 0.069 Uiso 1 1 calc R . . C18 C 0.68571(17) 0.68867(18) 1.01551(12) 0.0456(5) Uani 1 1 d . . . H18A H 0.6703 0.7477 1.0549 0.068 Uiso 1 1 calc R . . H18B H 0.7543 0.6617 1.0316 0.068 Uiso 1 1 calc R . . H18C H 0.6405 0.6215 1.0150 0.068 Uiso 1 1 calc R . . C19 C 0.78414(14) 0.73522(17) 0.71652(11) 0.0363(4) Uani 1 1 d . . . C20 C 0.78034(15) 0.61658(17) 0.68925(12) 0.0375(5) Uani 1 1 d . . . C21 C 0.68131(14) 0.57812(16) 0.68069(11) 0.0354(4) Uani 1 1 d . . . C22 C 0.62299(14) 0.67306(16) 0.70249(11) 0.0336(4) Uani 1 1 d . . . C23 C 0.68648(14) 0.77046(16) 0.72353(11) 0.0325(4) Uani 1 1 d . . . C24 C 0.87244(16) 0.8149(2) 0.72172(14) 0.0573(6) Uani 1 1 d . . . H24A H 0.8661 0.8797 0.7598 0.086 Uiso 1 1 calc R . . H24B H 0.8760 0.8472 0.6672 0.086 Uiso 1 1 calc R . . H24C H 0.9329 0.7701 0.7415 0.086 Uiso 1 1 calc R . . C25 C 0.86569(16) 0.5537(2) 0.65990(14) 0.0565(6) Uani 1 1 d . . . H25A H 0.8775 0.5890 0.6082 0.085 Uiso 1 1 calc R . . H25B H 0.8493 0.4701 0.6512 0.085 Uiso 1 1 calc R . . H25C H 0.9255 0.5614 0.7013 0.085 Uiso 1 1 calc R . . C26 C 0.63881(17) 0.46424(18) 0.64273(13) 0.0515(6) Uani 1 1 d . . . H26A H 0.6919 0.4171 0.6256 0.077 Uiso 1 1 calc R . . H26B H 0.5885 0.4817 0.5948 0.077 Uiso 1 1 calc R . . H26C H 0.6084 0.4200 0.6831 0.077 Uiso 1 1 calc R . . C27 C 0.51145(15) 0.6720(2) 0.69358(14) 0.0500(6) Uani 1 1 d . . . H27A H 0.4891 0.7430 0.7191 0.075 Uiso 1 1 calc R . . H27B H 0.4902 0.6019 0.7207 0.075 Uiso 1 1 calc R . . H27C H 0.4826 0.6705 0.6352 0.075 Uiso 1 1 calc R . . C28 C 0.65546(18) 0.89655(17) 0.73258(13) 0.0482(5) Uani 1 1 d . . . H28A H 0.5895 0.8984 0.7485 0.072 Uiso 1 1 calc R . . H28B H 0.6535 0.9378 0.6802 0.072 Uiso 1 1 calc R . . H28C H 0.7032 0.9355 0.7750 0.072 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 0.02551(19) 0.02737(19) 0.02692(19) 0.00098(14) 0.00390(13) -0.00087(14) N1 0.0375(9) 0.0325(8) 0.0412(10) 0.0013(7) 0.0104(7) 0.0038(7) N2 0.0347(9) 0.0312(8) 0.0311(8) 0.0004(6) 0.0066(7) 0.0001(7) C1 0.0320(10) 0.0326(10) 0.0480(12) 0.0018(9) 0.0058(8) -0.0024(8) C2 0.0402(11) 0.0235(9) 0.0458(12) 0.0007(8) 0.0111(9) -0.0049(8) C3 0.0533(13) 0.0336(11) 0.0568(14) 0.0069(10) 0.0210(11) -0.0044(9) C4 0.0858(19) 0.0396(12) 0.0463(13) 0.0081(10) 0.0264(13) -0.0044(12) C5 0.0778(18) 0.0442(13) 0.0426(13) 0.0095(10) 0.0012(12) -0.0026(12) C6 0.0474(13) 0.0347(11) 0.0474(13) 0.0044(9) 0.0021(10) 0.0015(9) C7 0.0392(11) 0.0230(9) 0.0377(11) 0.0000(8) 0.0066(8) -0.0012(8) C8 0.0746(16) 0.0384(12) 0.0443(13) -0.0040(10) 0.0145(11) 0.0113(11) C9 0.0370(12) 0.0552(14) 0.0652(15) 0.0145(11) 0.0179(11) 0.0157(10) C10 0.0304(10) 0.0410(11) 0.0405(11) 0.0028(9) -0.0005(8) -0.0012(8) C11 0.0423(12) 0.0369(11) 0.0282(10) 0.0016(8) -0.0042(8) -0.0067(9) C12 0.0502(13) 0.0479(12) 0.0436(13) 0.0014(10) -0.0033(10) -0.0152(10) C13 0.0815(18) 0.0372(12) 0.0480(14) 0.0032(10) -0.0033(12) -0.0213(12) C14 0.090(2) 0.0312(12) 0.0444(13) -0.0006(9) 0.0023(12) -0.0027(12) C15 0.0647(14) 0.0345(11) 0.0380(11) -0.0025(9) 0.0081(10) 0.0031(10) C16 0.0457(12) 0.0311(10) 0.0258(9) 0.0007(8) 0.0015(8) -0.0019(8) C17 0.0382(12) 0.0489(12) 0.0542(14) 0.0008(10) 0.0160(10) 0.0062(10) C18 0.0686(15) 0.0404(11) 0.0302(10) 0.0022(9) 0.0148(10) -0.0030(10) C19 0.0376(11) 0.0444(11) 0.0270(10) 0.0034(8) 0.0060(8) -0.0107(9) C20 0.0425(12) 0.0445(11) 0.0267(9) 0.0024(8) 0.0090(8) 0.0013(9) C21 0.0416(11) 0.0357(10) 0.0281(10) 0.0008(8) 0.0030(8) -0.0047(8) C22 0.0365(10) 0.0362(10) 0.0265(9) 0.0049(8) 0.0005(8) -0.0037(8) C23 0.0404(11) 0.0324(10) 0.0238(9) 0.0043(7) 0.0027(8) -0.0033(8) C24 0.0545(14) 0.0742(16) 0.0443(13) 0.0052(12) 0.0115(10) -0.0288(12) C25 0.0571(15) 0.0731(16) 0.0442(13) 0.0031(12) 0.0232(11) 0.0124(12) C26 0.0696(15) 0.0430(12) 0.0387(12) -0.0060(10) -0.0007(10) -0.0108(11) C27 0.0380(12) 0.0564(13) 0.0515(13) 0.0052(11) -0.0049(10) -0.0024(10) C28 0.0679(15) 0.0366(11) 0.0393(12) 0.0064(9) 0.0065(10) 0.0021(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 C10 2.2959(19) . ? Sc1 C1 2.3088(19) . ? Sc1 N2 2.4268(15) . ? Sc1 N1 2.4827(16) . ? Sc1 C22 2.5188(18) . ? Sc1 C19 2.5246(19) . ? Sc1 C23 2.5269(18) . ? Sc1 C21 2.5380(19) . ? Sc1 C20 2.544(2) . ? N1 C7 1.462(2) . ? N1 C9 1.480(2) . ? N1 C8 1.494(3) . ? N2 C16 1.466(2) . ? N2 C17 1.473(2) . ? N2 C18 1.494(2) . ? C1 C2 1.472(3) . ? C2 C3 1.403(3) . ? C2 C7 1.413(3) . ? C3 C4 1.381(3) . ? C4 C5 1.378(3) . ? C5 C6 1.387(3) . ? C6 C7 1.381(3) . ? C10 C11 1.482(3) . ? C11 C16 1.398(3) . ? C11 C12 1.406(3) . ? C12 C13 1.381(3) . ? C13 C14 1.377(3) . ? C14 C15 1.379(3) . ? C15 C16 1.389(3) . ? C19 C23 1.416(3) . ? C19 C20 1.417(3) . ? C19 C24 1.499(3) . ? C20 C21 1.407(3) . ? C20 C25 1.513(3) . ? C21 C22 1.421(3) . ? C21 C26 1.510(3) . ? C22 C23 1.413(2) . ? C22 C27 1.508(3) . ? C23 C28 1.506(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 Sc1 C1 129.85(7) . . ? C10 Sc1 N2 71.93(6) . . ? C1 Sc1 N2 86.60(6) . . ? C10 Sc1 N1 86.17(6) . . ? C1 Sc1 N1 70.88(6) . . ? N2 Sc1 N1 126.43(5) . . ? C10 Sc1 C22 135.29(7) . . ? C1 Sc1 C22 92.32(6) . . ? N2 Sc1 C22 100.94(6) . . ? N1 Sc1 C22 127.04(6) . . ? C10 Sc1 C19 86.60(7) . . ? C1 Sc1 C19 143.46(7) . . ? N2 Sc1 C19 111.12(6) . . ? N1 Sc1 C19 115.74(6) . . ? C22 Sc1 C19 53.96(6) . . ? C10 Sc1 C23 102.83(6) . . ? C1 Sc1 C23 122.19(7) . . ? N2 Sc1 C23 89.40(6) . . ? N1 Sc1 C23 143.82(6) . . ? C22 Sc1 C23 32.52(6) . . ? C19 Sc1 C23 32.57(6) . . ? C10 Sc1 C21 136.81(7) . . ? C1 Sc1 C21 90.64(7) . . ? N2 Sc1 C21 133.39(6) . . ? N1 Sc1 C21 95.89(6) . . ? C22 Sc1 C21 32.64(6) . . ? C19 Sc1 C21 53.70(6) . . ? C23 Sc1 C21 53.78(6) . . ? C10 Sc1 C20 104.99(7) . . ? C1 Sc1 C20 118.52(7) . . ? N2 Sc1 C20 142.12(6) . . ? N1 Sc1 C20 90.10(6) . . ? C22 Sc1 C20 53.76(6) . . ? C19 Sc1 C20 32.48(6) . . ? C23 Sc1 C20 53.74(6) . . ? C21 Sc1 C20 32.15(6) . . ? C7 N1 C9 113.06(16) . . ? C7 N1 C8 108.78(15) . . ? C9 N1 C8 106.96(16) . . ? C7 N1 Sc1 97.49(10) . . ? C9 N1 Sc1 112.84(12) . . ? C8 N1 Sc1 117.58(12) . . ? C16 N2 C17 113.80(15) . . ? C16 N2 C18 108.64(14) . . ? C17 N2 C18 107.13(15) . . ? C16 N2 Sc1 102.68(11) . . ? C17 N2 Sc1 112.05(11) . . ? C18 N2 Sc1 112.60(11) . . ? C2 C1 Sc1 101.65(11) . . ? C3 C2 C7 116.15(19) . . ? C3 C2 C1 123.45(18) . . ? C7 C2 C1 120.01(17) . . ? C4 C3 C2 122.5(2) . . ? C5 C4 C3 119.7(2) . . ? C4 C5 C6 119.7(2) . . ? C7 C6 C5 120.5(2) . . ? C6 C7 C2 121.33(19) . . ? C6 C7 N1 123.26(18) . . ? C2 C7 N1 115.41(16) . . ? C11 C10 Sc1 104.19(12) . . ? C16 C11 C12 116.16(19) . . ? C16 C11 C10 119.90(17) . . ? C12 C11 C10 123.82(19) . . ? C13 C12 C11 121.9(2) . . ? C14 C13 C12 120.5(2) . . ? C13 C14 C15 119.2(2) . . ? C14 C15 C16 120.4(2) . . ? C15 C16 C11 121.77(19) . . ? C15 C16 N2 122.41(18) . . ? C11 C16 N2 115.82(16) . . ? C23 C19 C20 107.94(16) . . ? C23 C19 C24 125.87(19) . . ? C20 C19 C24 125.31(19) . . ? C23 C19 Sc1 73.81(10) . . ? C20 C19 Sc1 74.50(11) . . ? C24 C19 Sc1 126.03(13) . . ? C21 C20 C19 108.10(17) . . ? C21 C20 C25 126.98(19) . . ? C19 C20 C25 123.99(19) . . ? C21 C20 Sc1 73.70(11) . . ? C19 C20 Sc1 73.02(11) . . ? C25 C20 Sc1 127.77(14) . . ? C20 C21 C22 108.07(16) . . ? C20 C21 C26 127.25(19) . . ? C22 C21 C26 124.04(18) . . ? C20 C21 Sc1 74.15(11) . . ? C22 C21 Sc1 72.94(10) . . ? C26 C21 Sc1 125.90(13) . . ? C23 C22 C21 107.90(16) . . ? C23 C22 C27 126.94(18) . . ? C21 C22 C27 124.74(17) . . ? C23 C22 Sc1 74.06(10) . . ? C21 C22 Sc1 74.42(10) . . ? C27 C22 Sc1 123.30(13) . . ? C22 C23 C19 107.97(16) . . ? C22 C23 C28 126.54(18) . . ? C19 C23 C28 124.10(18) . . ? C22 C23 Sc1 73.43(10) . . ? C19 C23 Sc1 73.63(10) . . ? C28 C23 Sc1 129.34(13) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.232 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.048 # Attachment '1c.cif' data_1c _database_code_depnum_ccdc_archive 'CCDC 637042' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common C5Me4HScBz2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H37 N2 Sc' _chemical_formula_weight 434.55 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 9.493(11) _cell_length_b 17.612(19) _cell_length_c 14.571(17) _cell_angle_alpha 90.00 _cell_angle_beta 91.82(2) _cell_angle_gamma 90.00 _cell_volume 2435(5) _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 ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8835 _exptl_absorpt_correction_T_max 0.9843 _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 10038 _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_av_sigmaI/netI 0.2179 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4285 _reflns_number_gt 1537 _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^)+(0.0088P)^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 4285 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1526 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 0.694 _refine_ls_restrained_S_all 0.694 _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 0.25327(8) 0.47191(4) 0.76506(5) 0.0406(2) Uani 1 1 d . . . N1 N 0.2194(4) 0.33958(17) 0.7153(2) 0.0542(10) Uani 1 1 d . . . N2 N 0.4053(4) 0.57455(17) 0.7136(2) 0.0487(10) Uani 1 1 d . . . C1 C 0.4545(4) 0.40474(19) 0.8019(2) 0.0495(12) Uani 1 1 d . . . H1A H 0.5356 0.4386 0.8156 0.059 Uiso 1 1 calc R . . H1B H 0.4411 0.3699 0.8542 0.059 Uiso 1 1 calc R . . C2 C 0.4705(5) 0.3631(2) 0.7148(3) 0.0504(12) Uani 1 1 d . . . C3 C 0.3516(6) 0.3319(2) 0.6698(3) 0.0556(13) Uani 1 1 d . . . C4 C 0.3604(6) 0.2953(2) 0.5859(3) 0.0781(17) Uani 1 1 d . . . H4 H 0.2785 0.2737 0.5574 0.094 Uiso 1 1 calc R . . C5 C 0.4869(8) 0.2903(3) 0.5443(4) 0.110(3) Uani 1 1 d . . . H5 H 0.4929 0.2649 0.4870 0.132 Uiso 1 1 calc R . . C6 C 0.6059(7) 0.3220(3) 0.5848(4) 0.091(2) Uani 1 1 d . . . H6 H 0.6935 0.3195 0.5552 0.109 Uiso 1 1 calc R . . C7 C 0.5969(5) 0.3574(2) 0.6690(4) 0.0707(15) Uani 1 1 d . . . H7 H 0.6798 0.3786 0.6967 0.085 Uiso 1 1 calc R . . C8 C 0.0924(5) 0.3331(2) 0.6536(3) 0.0867(17) Uani 1 1 d . . . H8A H 0.1040 0.3652 0.5994 0.130 Uiso 1 1 calc R . . H8B H 0.0092 0.3496 0.6864 0.130 Uiso 1 1 calc R . . H8C H 0.0802 0.2801 0.6343 0.130 Uiso 1 1 calc R . . C9 C 0.2108(5) 0.2786(2) 0.7855(3) 0.0755(16) Uani 1 1 d . . . H9A H 0.2121 0.2289 0.7553 0.113 Uiso 1 1 calc R . . H9B H 0.1231 0.2841 0.8186 0.113 Uiso 1 1 calc R . . H9C H 0.2914 0.2825 0.8290 0.113 Uiso 1 1 calc R . . C10 C 0.1815(4) 0.50572(19) 0.6210(2) 0.0508(12) Uani 1 1 d . . . H10A H 0.2426 0.4824 0.5749 0.061 Uiso 1 1 calc R . . H10B H 0.0830 0.4896 0.6081 0.061 Uiso 1 1 calc R . . C11 C 0.1934(5) 0.5897(3) 0.6192(3) 0.0496(12) Uani 1 1 d . . . C12 C 0.3046(5) 0.6250(3) 0.6668(3) 0.0512(12) Uani 1 1 d . . . C13 C 0.3205(5) 0.7038(3) 0.6697(3) 0.0677(15) Uani 1 1 d . . . H13 H 0.4001 0.7261 0.7003 0.081 Uiso 1 1 calc R . . C14 C 0.2184(7) 0.7486(3) 0.6275(4) 0.084(2) Uani 1 1 d . . . H14 H 0.2267 0.8023 0.6299 0.101 Uiso 1 1 calc R . . C15 C 0.1064(6) 0.7163(3) 0.5825(4) 0.087(2) Uani 1 1 d . . . H15 H 0.0368 0.7477 0.5536 0.104 Uiso 1 1 calc R . . C16 C 0.0924(5) 0.6378(3) 0.5784(3) 0.0704(15) Uani 1 1 d . . . H16 H 0.0124 0.6164 0.5473 0.084 Uiso 1 1 calc R . . C17 C 0.4837(4) 0.6094(2) 0.7923(3) 0.0750(15) Uani 1 1 d . . . H17A H 0.5466 0.6489 0.7699 0.112 Uiso 1 1 calc R . . H17B H 0.5394 0.5704 0.8247 0.112 Uiso 1 1 calc R . . H17C H 0.4169 0.6320 0.8343 0.112 Uiso 1 1 calc R . . C18 C 0.5113(4) 0.5476(2) 0.6475(3) 0.0673(14) Uani 1 1 d . . . H18A H 0.4627 0.5241 0.5944 0.101 Uiso 1 1 calc R . . H18B H 0.5735 0.5102 0.6777 0.101 Uiso 1 1 calc R . . H18C H 0.5673 0.5908 0.6270 0.101 Uiso 1 1 calc R . . C19 C 0.0171(4) 0.5129(3) 0.8188(3) 0.0535(12) Uani 1 1 d . . . C20 C 0.1127(5) 0.5655(2) 0.8580(3) 0.0464(12) Uani 1 1 d . . . C21 C 0.2008(4) 0.5265(3) 0.9217(2) 0.0461(11) Uani 1 1 d . . . C22 C 0.1614(5) 0.4495(2) 0.9224(3) 0.0496(12) Uani 1 1 d . . . C23 C 0.0473(4) 0.4422(2) 0.8585(3) 0.0551(13) Uani 1 1 d . . . H23 H -0.0014 0.3963 0.8446 0.066 Uiso 1 1 calc R . . C24 C -0.1031(4) 0.5304(2) 0.7543(3) 0.0773(14) Uani 1 1 d . . . H24A H -0.1282 0.4849 0.7188 0.116 Uiso 1 1 calc R . . H24B H -0.0760 0.5711 0.7125 0.116 Uiso 1 1 calc R . . H24C H -0.1842 0.5468 0.7892 0.116 Uiso 1 1 calc R . . C25 C 0.1035(4) 0.6506(2) 0.8474(3) 0.0698(15) Uani 1 1 d . . . H25A H 0.0450 0.6716 0.8954 0.105 Uiso 1 1 calc R . . H25B H 0.0613 0.6629 0.7869 0.105 Uiso 1 1 calc R . . H25C H 0.1983 0.6726 0.8528 0.105 Uiso 1 1 calc R . . C26 C 0.3038(4) 0.5615(2) 0.9898(3) 0.0731(15) Uani 1 1 d . . . H26A H 0.2689 0.5555 1.0519 0.110 Uiso 1 1 calc R . . H26B H 0.3144 0.6157 0.9761 0.110 Uiso 1 1 calc R . . H26C H 0.3954 0.5362 0.9857 0.110 Uiso 1 1 calc R . . C27 C 0.2128(5) 0.3910(2) 0.9898(3) 0.0798(16) Uani 1 1 d . . . H27A H 0.3160 0.3896 0.9910 0.120 Uiso 1 1 calc R . . H27B H 0.1757 0.3411 0.9716 0.120 Uiso 1 1 calc R . . H27C H 0.1803 0.4039 1.0511 0.120 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 0.0381(5) 0.0412(5) 0.0424(5) -0.0029(4) -0.0012(4) -0.0003(5) N1 0.059(3) 0.042(2) 0.062(3) -0.002(2) 0.001(2) -0.007(2) N2 0.049(3) 0.043(2) 0.055(3) -0.0031(19) 0.004(2) -0.0021(19) C1 0.050(3) 0.046(3) 0.052(3) -0.002(2) -0.005(2) 0.001(2) C2 0.057(4) 0.037(3) 0.058(3) 0.011(2) 0.011(3) 0.008(3) C3 0.077(4) 0.039(3) 0.052(4) 0.006(2) 0.013(3) 0.002(3) C4 0.117(6) 0.052(4) 0.066(4) -0.015(3) 0.014(4) -0.007(3) C5 0.193(9) 0.054(4) 0.087(5) -0.009(3) 0.063(6) 0.007(5) C6 0.111(6) 0.067(5) 0.098(5) 0.010(4) 0.060(5) 0.019(4) C7 0.065(4) 0.051(3) 0.097(5) 0.010(3) 0.023(3) 0.011(3) C8 0.083(4) 0.068(3) 0.107(4) -0.013(3) -0.028(3) -0.020(3) C9 0.091(4) 0.047(3) 0.091(4) 0.011(3) 0.031(3) -0.009(3) C10 0.062(3) 0.043(3) 0.047(3) 0.000(2) -0.003(2) -0.008(2) C11 0.047(3) 0.068(4) 0.034(3) 0.008(2) 0.004(2) 0.006(3) C12 0.061(4) 0.042(3) 0.051(3) 0.012(3) 0.014(3) 0.013(3) C13 0.081(4) 0.050(4) 0.074(4) 0.001(3) 0.028(3) 0.003(3) C14 0.119(6) 0.054(4) 0.082(5) 0.017(3) 0.046(4) 0.030(4) C15 0.111(6) 0.084(5) 0.067(4) 0.033(4) 0.031(4) 0.052(4) C16 0.070(4) 0.087(4) 0.054(3) 0.017(3) 0.000(3) 0.024(3) C17 0.071(4) 0.064(3) 0.089(4) -0.004(3) -0.007(3) -0.015(3) C18 0.058(4) 0.061(3) 0.084(4) 0.004(3) 0.022(3) 0.001(3) C19 0.034(3) 0.070(4) 0.057(3) 0.006(3) 0.004(2) 0.008(3) C20 0.040(3) 0.051(3) 0.049(3) -0.001(2) 0.001(2) 0.003(2) C21 0.046(3) 0.055(3) 0.037(3) -0.007(3) 0.003(2) 0.005(3) C22 0.046(3) 0.055(3) 0.048(3) 0.005(2) 0.005(2) 0.011(2) C23 0.045(3) 0.059(3) 0.062(3) -0.003(3) 0.011(3) -0.008(3) C24 0.041(3) 0.102(4) 0.089(4) 0.005(3) -0.001(3) 0.009(3) C25 0.079(4) 0.057(3) 0.075(4) -0.004(3) 0.016(3) 0.019(3) C26 0.073(4) 0.093(4) 0.053(3) -0.022(3) -0.009(3) 0.017(3) C27 0.108(5) 0.080(4) 0.053(3) 0.018(3) 0.015(3) 0.018(3) _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 C10 2.266(4) . ? Sc1 C1 2.296(4) . ? Sc1 N2 2.446(4) . ? Sc1 N1 2.459(4) . ? Sc1 C23 2.474(4) . ? Sc1 C19 2.505(5) . ? Sc1 C22 2.510(5) . ? Sc1 C20 2.539(4) . ? Sc1 C21 2.541(4) . ? N1 C3 1.443(5) . ? N1 C8 1.486(5) . ? N1 C9 1.488(4) . ? N2 C12 1.458(5) . ? N2 C17 1.480(4) . ? N2 C18 1.493(4) . ? C1 C2 1.478(5) . ? C2 C7 1.395(5) . ? C2 C3 1.399(6) . ? C3 C4 1.388(5) . ? C4 C5 1.365(7) . ? C5 C6 1.376(7) . ? C6 C7 1.380(6) . ? C10 C11 1.483(5) . ? C11 C12 1.392(6) . ? C11 C16 1.398(5) . ? C12 C13 1.395(5) . ? C13 C14 1.379(6) . ? C14 C15 1.356(7) . ? C15 C16 1.390(6) . ? C19 C23 1.400(5) . ? C19 C20 1.406(5) . ? C19 C24 1.487(5) . ? C20 C21 1.408(5) . ? C20 C25 1.509(5) . ? C21 C22 1.407(5) . ? C21 C26 1.503(5) . ? C22 C23 1.412(5) . ? C22 C27 1.495(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 C10 Sc1 C1 125.11(14) . . ? C10 Sc1 N2 71.61(13) . . ? C1 Sc1 N2 87.59(15) . . ? C10 Sc1 N1 86.75(13) . . ? C1 Sc1 N1 71.36(13) . . ? N2 Sc1 N1 133.08(13) . . ? C10 Sc1 C23 110.25(17) . . ? C1 Sc1 C23 115.36(16) . . ? N2 Sc1 C23 144.06(13) . . ? N1 Sc1 C23 82.15(13) . . ? C10 Sc1 C19 88.18(15) . . ? C1 Sc1 C19 145.28(15) . . ? N2 Sc1 C19 115.17(15) . . ? N1 Sc1 C19 104.82(15) . . ? C23 Sc1 C19 32.66(12) . . ? C10 Sc1 C22 141.70(16) . . ? C1 Sc1 C22 90.92(14) . . ? N2 Sc1 C22 128.44(14) . . ? N1 Sc1 C22 94.27(14) . . ? C23 Sc1 C22 32.90(12) . . ? C19 Sc1 C22 54.50(13) . . ? C10 Sc1 C20 100.14(15) . . ? C1 Sc1 C20 131.09(15) . . ? N2 Sc1 C20 90.50(14) . . ? N1 Sc1 C20 134.98(14) . . ? C23 Sc1 C20 53.57(14) . . ? C19 Sc1 C20 32.35(12) . . ? C22 Sc1 C20 53.92(13) . . ? C10 Sc1 C21 132.16(15) . . ? C1 Sc1 C21 99.82(14) . . ? N2 Sc1 C21 97.47(14) . . ? N1 Sc1 C21 126.60(14) . . ? C23 Sc1 C21 53.47(14) . . ? C19 Sc1 C21 53.62(13) . . ? C22 Sc1 C21 32.34(12) . . ? C20 Sc1 C21 32.19(12) . . ? C3 N1 C8 114.5(4) . . ? C3 N1 C9 108.4(3) . . ? C8 N1 C9 107.4(3) . . ? C3 N1 Sc1 96.7(2) . . ? C8 N1 Sc1 110.3(2) . . ? C9 N1 Sc1 119.4(3) . . ? C12 N2 C17 114.5(3) . . ? C12 N2 C18 109.7(3) . . ? C17 N2 C18 107.4(3) . . ? C12 N2 Sc1 102.1(3) . . ? C17 N2 Sc1 110.9(2) . . ? C18 N2 Sc1 112.3(2) . . ? C2 C1 Sc1 99.4(3) . . ? C7 C2 C3 116.2(5) . . ? C7 C2 C1 124.0(5) . . ? C3 C2 C1 119.6(4) . . ? C4 C3 C2 121.6(5) . . ? C4 C3 N1 121.7(5) . . ? C2 C3 N1 116.6(4) . . ? C5 C4 C3 120.0(6) . . ? C4 C5 C6 120.4(6) . . ? C5 C6 C7 119.4(6) . . ? C6 C7 C2 122.4(5) . . ? C11 C10 Sc1 104.9(2) . . ? C12 C11 C16 116.1(4) . . ? C12 C11 C10 119.6(4) . . ? C16 C11 C10 124.0(5) . . ? C11 C12 C13 122.6(5) . . ? C11 C12 N2 115.8(4) . . ? C13 C12 N2 121.6(5) . . ? C14 C13 C12 118.8(5) . . ? C15 C14 C13 120.3(6) . . ? C14 C15 C16 120.7(6) . . ? C15 C16 C11 121.4(5) . . ? C23 C19 C20 107.3(4) . . ? C23 C19 C24 126.1(5) . . ? C20 C19 C24 126.4(5) . . ? C23 C19 Sc1 72.4(2) . . ? C20 C19 Sc1 75.2(3) . . ? C24 C19 Sc1 122.6(3) . . ? C19 C20 C21 108.0(4) . . ? C19 C20 C25 125.3(4) . . ? C21 C20 C25 125.7(4) . . ? C19 C20 Sc1 72.5(3) . . ? C21 C20 Sc1 74.0(2) . . ? C25 C20 Sc1 128.3(3) . . ? C22 C21 C20 108.8(4) . . ? C22 C21 C26 123.9(4) . . ? C20 C21 C26 126.5(4) . . ? C22 C21 Sc1 72.6(2) . . ? C20 C21 Sc1 73.8(2) . . ? C26 C21 Sc1 127.3(3) . . ? C21 C22 C23 106.4(4) . . ? C21 C22 C27 126.0(4) . . ? C23 C22 C27 126.7(4) . . ? C21 C22 Sc1 75.0(2) . . ? C23 C22 Sc1 72.1(2) . . ? C27 C22 Sc1 126.4(3) . . ? C19 C23 C22 109.5(4) . . ? C19 C23 Sc1 74.9(2) . . ? C22 C23 Sc1 75.0(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.207 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.043 # Attachment '2a.cif' data_2a _database_code_depnum_ccdc_archive 'CCDC 637043' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cp'ScBz)(B(C6F5)4) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H33 B F20 N Sc Si' _chemical_formula_weight 1051.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 17.823(4) _cell_length_b 10.479(3) _cell_length_c 23.866(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4457.2(19) _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 block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 0.311 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8476 _exptl_absorpt_correction_T_max 0.9125 _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 22032 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.06 _reflns_number_total 7718 _reflns_number_gt 5002 _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^)+(0.0000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 7718 _refine_ls_number_parameters 631 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0402 _refine_ls_wR_factor_gt 0.0366 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.008 _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 0.45683(3) 0.36737(5) 0.24366(3) 0.03803(15) Uani 1 1 d . . . Si1 Si 0.63380(5) 0.57280(9) 0.24153(7) 0.0701(3) Uani 1 1 d . . . N1 N 0.45269(18) 0.2620(3) 0.32815(11) 0.0506(8) Uani 1 1 d . . . F1 F 0.47121(9) 0.29000(14) 0.14800(7) 0.0418(5) Uani 1 1 d . . . F2 F 0.56453(8) 0.25112(13) 0.22690(7) 0.0447(5) Uani 1 1 d . . . F3 F 0.65896(10) 0.04433(16) 0.22698(8) 0.0634(6) Uani 1 1 d . . . F4 F 0.65425(11) -0.11975(17) 0.13782(8) 0.0705(6) Uani 1 1 d . . . F5 F 0.56478(10) -0.07492(16) 0.05260(8) 0.0560(5) Uani 1 1 d . . . F6 F 0.41187(11) -0.09231(15) 0.08876(8) 0.0596(6) Uani 1 1 d . . . F7 F 0.31182(13) -0.2458(2) 0.04594(10) 0.0889(8) Uani 1 1 d . . . F8 F 0.26240(13) -0.21719(18) -0.06136(10) 0.0994(9) Uani 1 1 d . . . F9 F 0.31923(12) -0.02602(17) -0.12426(9) 0.0822(7) Uani 1 1 d . . . F10 F 0.41682(10) 0.13727(17) -0.08098(7) 0.0583(6) Uani 1 1 d . . . F11 F 0.54744(10) -0.00770(17) -0.06336(7) 0.0604(6) Uani 1 1 d . . . F12 F 0.67398(11) 0.04946(19) -0.11347(9) 0.0823(7) Uani 1 1 d . . . F13 F 0.75279(11) 0.25929(18) -0.08444(8) 0.0819(7) Uani 1 1 d . . . F14 F 0.69951(12) 0.41543(19) -0.00279(10) 0.0855(7) Uani 1 1 d . . . F15 F 0.57164(10) 0.36007(15) 0.04902(8) 0.0617(6) Uani 1 1 d . . . F16 F 0.46816(11) 0.39875(17) -0.03497(7) 0.0658(6) Uani 1 1 d . . . F17 F 0.35432(13) 0.55468(18) -0.03865(9) 0.0809(7) Uani 1 1 d . . . F18 F 0.23233(11) 0.51743(17) 0.02890(9) 0.0763(7) Uani 1 1 d . . . F19 F 0.23033(11) 0.31515(17) 0.09957(9) 0.0707(6) Uani 1 1 d . . . F20 F 0.34356(9) 0.15214(16) 0.10126(8) 0.0556(5) Uani 1 1 d . . . B1 B 0.4746(2) 0.1463(3) 0.03138(15) 0.0382(10) Uani 1 1 d . . . C1 C 0.34517(15) 0.2793(2) 0.24143(16) 0.0533(9) Uani 1 1 d . . . H1A H 0.3110 0.3082 0.2716 0.064 Uiso 1 1 calc R . . H1B H 0.3204 0.2828 0.2043 0.064 Uiso 1 1 calc R . . C2 C 0.38361(18) 0.1572(3) 0.25328(15) 0.0469(10) Uani 1 1 d . . . C3 C 0.43844(19) 0.1468(3) 0.29563(14) 0.0451(9) Uani 1 1 d . . . C4 C 0.4790(2) 0.0347(3) 0.30284(15) 0.0551(11) Uani 1 1 d . . . H4 H 0.5162 0.0297 0.3313 0.066 Uiso 1 1 calc R . . C5 C 0.4657(2) -0.0678(3) 0.26944(18) 0.0681(13) Uani 1 1 d . . . H5 H 0.4929 -0.1446 0.2753 0.082 Uiso 1 1 calc R . . C6 C 0.4139(2) -0.0614(3) 0.22759(17) 0.0715(13) Uani 1 1 d . . . H6 H 0.4055 -0.1336 0.2044 0.086 Uiso 1 1 calc R . . C7 C 0.3736(2) 0.0486(3) 0.21871(14) 0.0598(11) Uani 1 1 d . . . H7 H 0.3384 0.0518 0.1888 0.072 Uiso 1 1 calc R . . C8 C 0.5240(2) 0.2590(3) 0.35905(15) 0.0672(11) Uani 1 1 d . . . H8A H 0.5210 0.1951 0.3890 0.101 Uiso 1 1 calc R . . H8B H 0.5337 0.3431 0.3755 0.101 Uiso 1 1 calc R . . H8C H 0.5648 0.2367 0.3334 0.101 Uiso 1 1 calc R . . C9 C 0.3915(2) 0.2852(3) 0.37047(14) 0.0706(12) Uani 1 1 d . . . H9A H 0.3426 0.2811 0.3519 0.106 Uiso 1 1 calc R . . H9B H 0.3982 0.3698 0.3873 0.106 Uiso 1 1 calc R . . H9C H 0.3940 0.2199 0.3998 0.106 Uiso 1 1 calc R . . C10 C 0.52903(15) 0.5618(2) 0.23902(17) 0.0394(8) Uani 1 1 d . . . C11 C 0.4816(2) 0.5716(3) 0.28651(14) 0.0421(9) Uani 1 1 d . . . C12 C 0.4074(2) 0.5776(3) 0.26931(16) 0.0438(10) Uani 1 1 d . . . C13 C 0.4056(2) 0.5717(3) 0.21074(15) 0.0394(9) Uani 1 1 d . . . C14 C 0.4796(2) 0.5642(3) 0.19160(14) 0.0403(9) Uani 1 1 d . . . C15 C 0.5060(2) 0.5953(3) 0.34605(13) 0.0674(12) Uani 1 1 d . . . H15A H 0.5078 0.6874 0.3531 0.101 Uiso 1 1 calc R . . H15B H 0.5559 0.5584 0.3520 0.101 Uiso 1 1 calc R . . H15C H 0.4701 0.5556 0.3718 0.101 Uiso 1 1 calc R . . C16 C 0.3400(2) 0.5983(3) 0.30583(16) 0.0750(13) Uani 1 1 d . . . H16A H 0.3245 0.6879 0.3036 0.113 Uiso 1 1 calc R . . H16B H 0.3527 0.5771 0.3447 0.113 Uiso 1 1 calc R . . H16C H 0.2989 0.5436 0.2931 0.113 Uiso 1 1 calc R . . C17 C 0.33650(19) 0.5839(3) 0.17470(15) 0.0620(12) Uani 1 1 d . . . H17A H 0.2922 0.5591 0.1964 0.093 Uiso 1 1 calc R . . H17B H 0.3413 0.5280 0.1420 0.093 Uiso 1 1 calc R . . H17C H 0.3311 0.6726 0.1623 0.093 Uiso 1 1 calc R . . C18 C 0.5004(2) 0.5706(3) 0.13088(14) 0.0633(11) Uani 1 1 d . . . H18A H 0.4586 0.5387 0.1081 0.095 Uiso 1 1 calc R . . H18B H 0.5449 0.5180 0.1242 0.095 Uiso 1 1 calc R . . H18C H 0.5112 0.6593 0.1206 0.095 Uiso 1 1 calc R . . C19 C 0.6769(2) 0.5557(4) 0.17075(17) 0.1104(17) Uani 1 1 d . . . H19A H 0.6541 0.6175 0.1450 0.166 Uiso 1 1 calc R . . H19B H 0.6682 0.4691 0.1567 0.166 Uiso 1 1 calc R . . H19C H 0.7310 0.5715 0.1733 0.166 Uiso 1 1 calc R . . C20 C 0.6592(2) 0.7324(3) 0.26893(19) 0.1195(19) Uani 1 1 d . . . H20A H 0.7130 0.7471 0.2634 0.179 Uiso 1 1 calc R . . H20B H 0.6475 0.7366 0.3090 0.179 Uiso 1 1 calc R . . H20C H 0.6305 0.7979 0.2489 0.179 Uiso 1 1 calc R . . C21 C 0.6769(2) 0.4521(3) 0.28960(17) 0.0926(15) Uani 1 1 d . . . H21A H 0.7304 0.4711 0.2944 0.139 Uiso 1 1 calc R . . H21B H 0.6711 0.3667 0.2735 0.139 Uiso 1 1 calc R . . H21C H 0.6518 0.4555 0.3261 0.139 Uiso 1 1 calc R . . C22 C 0.51295(16) 0.1104(3) 0.09226(13) 0.0355(8) Uani 1 1 d . . . C23 C 0.51686(17) 0.1846(3) 0.13983(14) 0.0333(8) Uani 1 1 d . . . C24 C 0.56406(18) 0.1635(3) 0.18362(13) 0.0358(8) Uani 1 1 d . . . C25 C 0.61190(18) 0.0614(3) 0.18422(14) 0.0434(9) Uani 1 1 d . . . C26 C 0.60848(19) -0.0198(3) 0.13935(15) 0.0450(9) Uani 1 1 d . . . C27 C 0.56164(18) 0.0064(3) 0.09575(14) 0.0390(8) Uani 1 1 d . . . C28 C 0.42121(17) 0.0299(3) 0.00556(14) 0.0388(8) Uani 1 1 d . . . C29 C 0.3920(2) -0.0717(3) 0.03566(15) 0.0473(10) Uani 1 1 d . . . C30 C 0.3390(2) -0.1527(3) 0.01404(17) 0.0563(11) Uani 1 1 d . . . C31 C 0.3147(2) -0.1388(3) -0.03972(18) 0.0591(11) Uani 1 1 d . . . C32 C 0.3425(2) -0.0421(3) -0.07129(16) 0.0528(11) Uani 1 1 d . . . C33 C 0.39321(19) 0.0395(3) -0.04777(14) 0.0453(10) Uani 1 1 d . . . C34 C 0.54972(17) 0.1765(3) -0.00586(13) 0.0375(8) Uani 1 1 d . . . C35 C 0.58154(19) 0.1017(3) -0.04741(14) 0.0445(10) Uani 1 1 d . . . C36 C 0.6472(2) 0.1276(4) -0.07359(15) 0.0546(10) Uani 1 1 d . . . C37 C 0.6871(2) 0.2350(4) -0.05930(16) 0.0552(11) Uani 1 1 d . . . C38 C 0.6597(2) 0.3114(4) -0.01844(16) 0.0546(10) Uani 1 1 d . . . C39 C 0.5939(2) 0.2813(3) 0.00696(14) 0.0451(9) Uani 1 1 d . . . C40 C 0.41347(18) 0.2646(3) 0.03389(12) 0.0357(8) Uani 1 1 d . . . C41 C 0.4107(2) 0.3720(3) -0.00019(13) 0.0456(9) Uani 1 1 d . . . C42 C 0.3513(2) 0.4565(3) -0.00234(16) 0.0531(10) Uani 1 1 d . . . C43 C 0.2908(2) 0.4389(3) 0.03004(15) 0.0495(10) Uani 1 1 d . . . C44 C 0.2906(2) 0.3352(3) 0.06630(15) 0.0488(10) Uani 1 1 d . . . C45 C 0.3495(2) 0.2525(3) 0.06631(14) 0.0413(9) 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 0.0419(4) 0.0377(3) 0.0344(4) -0.0004(4) 0.0005(4) 0.0010(3) Si1 0.0453(6) 0.0653(7) 0.0999(9) 0.0091(8) -0.0096(8) -0.0102(6) N1 0.064(2) 0.052(2) 0.0357(19) 0.0074(15) -0.0016(17) 0.0051(17) F1 0.0495(13) 0.0394(10) 0.0363(12) -0.0037(9) -0.0046(10) 0.0072(10) F2 0.0454(12) 0.0487(10) 0.0400(12) -0.0081(9) -0.0063(10) 0.0010(9) F3 0.0592(13) 0.0711(13) 0.0599(16) -0.0035(11) -0.0202(12) 0.0197(11) F4 0.0731(15) 0.0631(13) 0.0753(15) -0.0073(12) -0.0114(12) 0.0327(12) F5 0.0699(14) 0.0494(11) 0.0488(13) -0.0158(11) -0.0062(12) 0.0199(11) F6 0.0792(15) 0.0526(12) 0.0471(14) 0.0063(10) -0.0083(12) -0.0130(11) F7 0.104(2) 0.0634(14) 0.099(2) 0.0099(14) -0.0141(16) -0.0323(14) F8 0.099(2) 0.0685(15) 0.130(2) -0.0107(14) -0.0585(17) -0.0186(14) F9 0.0960(18) 0.0862(16) 0.0645(17) -0.0149(13) -0.0399(14) 0.0053(14) F10 0.0635(15) 0.0706(13) 0.0408(13) 0.0020(11) -0.0057(11) -0.0003(12) F11 0.0571(14) 0.0683(14) 0.0557(14) -0.0257(11) 0.0061(11) 0.0019(12) F12 0.0735(16) 0.1085(17) 0.0649(16) -0.0221(14) 0.0231(13) 0.0149(14) F13 0.0562(15) 0.1102(17) 0.0794(18) 0.0170(15) 0.0211(13) -0.0023(14) F14 0.0733(16) 0.0836(15) 0.0997(19) -0.0020(15) 0.0155(14) -0.0316(14) F15 0.0713(14) 0.0545(12) 0.0593(14) -0.0153(11) 0.0091(11) -0.0155(11) F16 0.0819(16) 0.0668(13) 0.0486(13) 0.0166(10) 0.0200(13) 0.0199(13) F17 0.1059(19) 0.0605(14) 0.0762(17) 0.0210(13) -0.0037(14) 0.0270(14) F18 0.0614(15) 0.0628(13) 0.1049(19) -0.0077(13) -0.0175(14) 0.0222(12) F19 0.0446(13) 0.0807(14) 0.0869(17) -0.0083(13) 0.0131(13) 0.0063(12) F20 0.0523(12) 0.0583(12) 0.0562(13) 0.0075(11) 0.0107(11) -0.0008(11) B1 0.040(2) 0.038(2) 0.037(2) -0.0005(19) -0.002(2) 0.000(2) C1 0.049(2) 0.053(2) 0.058(2) 0.009(2) 0.005(2) 0.0000(17) C2 0.041(2) 0.048(2) 0.052(3) 0.011(2) 0.011(2) -0.0117(18) C3 0.052(3) 0.045(2) 0.038(2) 0.0092(19) 0.009(2) -0.009(2) C4 0.069(3) 0.046(2) 0.050(3) 0.013(2) 0.002(2) 0.004(2) C5 0.091(4) 0.039(2) 0.074(3) 0.014(2) 0.014(3) 0.005(2) C6 0.104(4) 0.044(2) 0.067(4) 0.004(2) 0.012(3) -0.016(3) C7 0.069(3) 0.055(2) 0.055(3) 0.010(2) 0.000(2) -0.030(2) C8 0.074(3) 0.072(3) 0.056(3) 0.008(2) -0.017(2) 0.002(2) C9 0.093(3) 0.065(3) 0.053(3) 0.005(2) 0.024(2) 0.009(2) C10 0.045(2) 0.0282(16) 0.045(2) 0.0028(19) -0.003(2) -0.0017(15) C11 0.059(3) 0.0317(19) 0.035(2) -0.0035(17) -0.012(2) -0.001(2) C12 0.051(3) 0.036(2) 0.044(3) -0.0079(19) 0.004(2) 0.009(2) C13 0.047(3) 0.0273(19) 0.044(3) -0.0031(17) -0.012(2) 0.0025(19) C14 0.056(3) 0.030(2) 0.035(2) 0.0015(16) 0.003(2) -0.002(2) C15 0.103(4) 0.052(2) 0.047(3) -0.008(2) -0.016(2) -0.004(2) C16 0.079(3) 0.072(3) 0.074(3) -0.009(2) 0.012(3) 0.023(2) C17 0.060(3) 0.057(3) 0.068(3) 0.002(2) -0.024(2) 0.010(2) C18 0.094(3) 0.049(2) 0.047(3) 0.0074(19) 0.015(2) -0.009(2) C19 0.053(3) 0.155(4) 0.124(4) 0.010(4) 0.034(3) 0.010(3) C20 0.099(4) 0.084(3) 0.175(6) 0.010(3) -0.035(3) -0.049(3) C21 0.048(3) 0.092(3) 0.138(4) 0.019(3) -0.023(3) -0.007(2) C22 0.035(2) 0.0382(19) 0.034(2) 0.0012(17) 0.0019(16) -0.0020(17) C23 0.036(2) 0.0256(17) 0.038(2) 0.0018(17) 0.0065(18) 0.0050(16) C24 0.039(2) 0.042(2) 0.027(2) -0.0060(17) 0.0003(17) -0.0054(18) C25 0.034(2) 0.052(2) 0.045(2) 0.005(2) -0.0059(19) 0.003(2) C26 0.051(2) 0.035(2) 0.049(3) -0.0044(19) -0.004(2) 0.0129(19) C27 0.041(2) 0.036(2) 0.040(2) -0.0062(18) 0.0040(19) 0.0031(18) C28 0.036(2) 0.039(2) 0.041(2) -0.0099(18) -0.0023(19) 0.0053(18) C29 0.052(3) 0.040(2) 0.050(3) -0.006(2) -0.008(2) -0.002(2) C30 0.058(3) 0.039(2) 0.072(3) 0.003(2) -0.007(2) -0.011(2) C31 0.051(3) 0.046(2) 0.081(3) -0.017(2) -0.025(2) -0.004(2) C32 0.058(3) 0.049(2) 0.051(3) -0.013(2) -0.019(2) 0.003(2) C33 0.050(3) 0.045(2) 0.041(3) -0.0005(19) 0.000(2) 0.005(2) C34 0.040(2) 0.042(2) 0.031(2) -0.0008(16) -0.0019(18) 0.0049(18) C35 0.041(2) 0.054(2) 0.038(2) -0.0078(19) -0.0020(19) -0.002(2) C36 0.047(3) 0.074(3) 0.043(3) -0.007(2) 0.006(2) 0.016(2) C37 0.038(3) 0.079(3) 0.049(3) 0.014(2) 0.005(2) -0.004(2) C38 0.052(3) 0.057(3) 0.055(3) 0.000(2) -0.001(2) -0.009(2) C39 0.046(2) 0.050(2) 0.039(2) -0.0013(19) 0.006(2) 0.001(2) C40 0.040(2) 0.0388(19) 0.028(2) -0.0047(16) 0.0003(18) 0.0007(17) C41 0.052(2) 0.058(3) 0.027(2) -0.0020(19) 0.0063(19) 0.000(2) C42 0.064(3) 0.045(2) 0.050(3) 0.000(2) -0.010(2) 0.014(2) C43 0.038(2) 0.053(3) 0.058(3) -0.015(2) -0.010(2) 0.013(2) C44 0.039(2) 0.056(3) 0.051(3) -0.014(2) 0.004(2) 0.002(2) C45 0.041(2) 0.040(2) 0.043(2) -0.0024(18) -0.0043(19) 0.0022(19) _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 C1 2.195(3) . ? Sc1 N1 2.300(3) . ? Sc1 F2 2.3084(16) . ? Sc1 C10 2.412(3) . ? Sc1 C11 2.413(3) . ? Sc1 F1 2.4363(18) . ? Sc1 C14 2.442(3) . ? Sc1 C12 2.450(3) . ? Sc1 C13 2.457(3) . ? Sc1 C2 2.570(3) . ? Sc1 C3 2.643(3) . ? Si1 C20 1.852(3) . ? Si1 C19 1.864(4) . ? Si1 C10 1.872(3) . ? Si1 C21 1.872(3) . ? N1 C3 1.457(4) . ? N1 C8 1.470(4) . ? N1 C9 1.506(4) . ? F1 C23 1.385(3) . ? F2 C24 1.382(3) . ? F3 C25 1.333(3) . ? F4 C26 1.328(3) . ? F5 C27 1.338(3) . ? F6 C29 1.333(3) . ? F7 C30 1.329(4) . ? F8 C31 1.345(3) . ? F9 C32 1.341(4) . ? F10 C33 1.362(3) . ? F11 C35 1.352(3) . ? F12 C36 1.343(3) . ? F13 C37 1.340(4) . ? F14 C38 1.354(3) . ? F15 C39 1.359(3) . ? F16 C41 1.348(3) . ? F17 C42 1.346(4) . ? F18 C43 1.329(3) . ? F19 C44 1.352(4) . ? F20 C45 1.347(3) . ? B1 C34 1.638(4) . ? B1 C22 1.649(4) . ? B1 C40 1.652(4) . ? B1 C28 1.665(4) . ? C1 C2 1.478(4) . ? C2 C3 1.410(4) . ? C2 C7 1.417(4) . ? C3 C4 1.390(4) . ? C4 C5 1.358(4) . ? C5 C6 1.362(4) . ? C6 C7 1.374(4) . ? C10 C11 1.418(4) . ? C10 C14 1.434(4) . ? C11 C12 1.386(4) . ? C11 C15 1.507(4) . ? C12 C13 1.399(4) . ? C12 C16 1.499(4) . ? C13 C14 1.398(4) . ? C13 C17 1.508(4) . ? C14 C18 1.497(4) . ? C22 C23 1.378(4) . ? C22 C27 1.396(4) . ? C23 C24 1.360(4) . ? C24 C25 1.368(4) . ? C25 C26 1.369(4) . ? C26 C27 1.362(4) . ? C28 C33 1.371(4) . ? C28 C29 1.386(4) . ? C29 C30 1.372(4) . ? C30 C31 1.362(4) . ? C31 C32 1.357(5) . ? C32 C33 1.365(4) . ? C34 C39 1.385(4) . ? C34 C35 1.386(4) . ? C35 C36 1.354(4) . ? C36 C37 1.374(5) . ? C37 C38 1.353(5) . ? C38 C39 1.356(4) . ? C40 C45 1.384(4) . ? C40 C41 1.390(4) . ? C41 C42 1.382(4) . ? C42 C43 1.338(4) . ? C43 C44 1.389(4) . ? C44 C45 1.361(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sc1 N1 77.89(13) . . ? C1 Sc1 F2 121.86(8) . . ? N1 Sc1 F2 85.71(8) . . ? C1 Sc1 C10 146.93(10) . . ? N1 Sc1 C10 117.58(12) . . ? F2 Sc1 C10 89.66(8) . . ? C1 Sc1 C11 123.32(13) . . ? N1 Sc1 C11 93.46(11) . . ? F2 Sc1 C11 112.93(10) . . ? C10 Sc1 C11 34.18(11) . . ? C1 Sc1 F1 86.14(11) . . ? N1 Sc1 F1 131.68(8) . . ? F2 Sc1 F1 64.82(6) . . ? C10 Sc1 F1 100.48(11) . . ? C11 Sc1 F1 132.31(10) . . ? C1 Sc1 C14 119.59(12) . . ? N1 Sc1 C14 148.98(11) . . ? F2 Sc1 C14 102.67(10) . . ? C10 Sc1 C14 34.37(10) . . ? C11 Sc1 C14 55.67(9) . . ? F1 Sc1 C14 77.69(9) . . ? C1 Sc1 C12 93.33(12) . . ? N1 Sc1 C12 101.61(12) . . ? F2 Sc1 C12 144.77(10) . . ? C10 Sc1 C12 56.23(11) . . ? C11 Sc1 C12 33.11(10) . . ? F1 Sc1 C12 124.83(10) . . ? C14 Sc1 C12 55.08(11) . . ? C1 Sc1 C13 91.26(11) . . ? N1 Sc1 C13 133.39(12) . . ? F2 Sc1 C13 135.53(10) . . ? C10 Sc1 C13 56.46(10) . . ? C11 Sc1 C13 55.27(11) . . ? F1 Sc1 C13 91.69(9) . . ? C14 Sc1 C13 33.17(10) . . ? C12 Sc1 C13 33.14(8) . . ? C1 Sc1 C2 35.03(9) . . ? N1 Sc1 C2 59.60(11) . . ? F2 Sc1 C2 89.17(8) . . ? C10 Sc1 C2 177.02(13) . . ? C11 Sc1 C2 144.59(12) . . ? F1 Sc1 C2 81.49(9) . . ? C14 Sc1 C2 148.61(12) . . ? C12 Sc1 C2 124.43(12) . . ? C13 Sc1 C2 125.92(11) . . ? C1 Sc1 C3 62.04(10) . . ? N1 Sc1 C3 33.37(9) . . ? F2 Sc1 C3 73.92(8) . . ? C10 Sc1 C3 145.70(12) . . ? C11 Sc1 C3 126.83(12) . . ? F1 Sc1 C3 99.31(9) . . ? C14 Sc1 C3 176.27(11) . . ? C12 Sc1 C3 128.62(11) . . ? C13 Sc1 C3 150.00(12) . . ? C2 Sc1 C3 31.34(9) . . ? C20 Si1 C19 107.82(18) . . ? C20 Si1 C10 108.11(15) . . ? C19 Si1 C10 112.07(19) . . ? C20 Si1 C21 107.05(18) . . ? C19 Si1 C21 108.74(18) . . ? C10 Si1 C21 112.80(16) . . ? C3 N1 C8 113.6(3) . . ? C3 N1 C9 111.4(3) . . ? C8 N1 C9 107.0(3) . . ? C3 N1 Sc1 86.35(17) . . ? C8 N1 Sc1 115.0(2) . . ? C9 N1 Sc1 122.2(2) . . ? C23 F1 Sc1 117.32(17) . . ? C24 F2 Sc1 118.36(17) . . ? C34 B1 C22 100.6(2) . . ? C34 B1 C40 114.5(3) . . ? C22 B1 C40 114.4(3) . . ? C34 B1 C28 114.1(3) . . ? C22 B1 C28 113.3(3) . . ? C40 B1 C28 100.7(2) . . ? C2 C1 Sc1 86.50(18) . . ? C3 C2 C7 116.2(3) . . ? C3 C2 C1 121.7(3) . . ? C7 C2 C1 121.7(3) . . ? C3 C2 Sc1 77.2(2) . . ? C7 C2 Sc1 134.4(2) . . ? C1 C2 Sc1 58.47(15) . . ? C4 C3 C2 121.0(3) . . ? C4 C3 N1 122.9(3) . . ? C2 C3 N1 116.0(3) . . ? C4 C3 Sc1 137.1(2) . . ? C2 C3 Sc1 71.46(19) . . ? N1 C3 Sc1 60.28(15) . . ? C5 C4 C3 120.3(4) . . ? C4 C5 C6 120.6(4) . . ? C5 C6 C7 120.6(4) . . ? C6 C7 C2 121.2(4) . . ? C11 C10 C14 105.3(2) . . ? C11 C10 Si1 124.4(3) . . ? C14 C10 Si1 129.6(3) . . ? C11 C10 Sc1 72.93(17) . . ? C14 C10 Sc1 73.95(17) . . ? Si1 C10 Sc1 125.65(13) . . ? C12 C11 C10 109.6(3) . . ? C12 C11 C15 123.2(4) . . ? C10 C11 C15 126.4(4) . . ? C12 C11 Sc1 74.92(19) . . ? C10 C11 Sc1 72.89(17) . . ? C15 C11 Sc1 126.8(2) . . ? C11 C12 C13 108.4(3) . . ? C11 C12 C16 126.7(4) . . ? C13 C12 C16 124.7(4) . . ? C11 C12 Sc1 71.97(19) . . ? C13 C12 Sc1 73.7(2) . . ? C16 C12 Sc1 124.3(2) . . ? C14 C13 C12 107.9(3) . . ? C14 C13 C17 126.1(4) . . ? C12 C13 C17 125.8(4) . . ? C14 C13 Sc1 72.83(19) . . ? C12 C13 Sc1 73.2(2) . . ? C17 C13 Sc1 124.1(2) . . ? C13 C14 C10 108.8(3) . . ? C13 C14 C18 123.2(3) . . ? C10 C14 C18 127.8(4) . . ? C13 C14 Sc1 74.01(19) . . ? C10 C14 Sc1 71.69(17) . . ? C18 C14 Sc1 124.9(2) . . ? C23 C22 C27 111.1(3) . . ? C23 C22 B1 128.2(3) . . ? C27 C22 B1 119.2(3) . . ? C24 C23 C22 125.0(3) . . ? C24 C23 F1 112.6(3) . . ? C22 C23 F1 122.4(3) . . ? C23 C24 C25 121.4(3) . . ? C23 C24 F2 118.1(3) . . ? C25 C24 F2 120.5(3) . . ? F3 C25 C24 120.3(3) . . ? F3 C25 C26 122.9(3) . . ? C24 C25 C26 116.7(3) . . ? F4 C26 C27 121.0(3) . . ? F4 C26 C25 119.0(3) . . ? C27 C26 C25 120.0(3) . . ? F5 C27 C26 115.7(3) . . ? F5 C27 C22 118.5(3) . . ? C26 C27 C22 125.7(3) . . ? C33 C28 C29 113.6(3) . . ? C33 C28 B1 119.9(3) . . ? C29 C28 B1 125.8(3) . . ? F6 C29 C30 116.1(3) . . ? F6 C29 C28 121.2(3) . . ? C30 C29 C28 122.6(4) . . ? F7 C30 C31 120.2(4) . . ? F7 C30 C29 119.3(4) . . ? C31 C30 C29 120.5(4) . . ? F8 C31 C32 119.7(4) . . ? F8 C31 C30 121.1(4) . . ? C32 C31 C30 119.1(4) . . ? F9 C32 C31 120.3(3) . . ? F9 C32 C33 120.9(4) . . ? C31 C32 C33 118.8(4) . . ? F10 C33 C32 115.9(3) . . ? F10 C33 C28 118.9(3) . . ? C32 C33 C28 125.2(3) . . ? C39 C34 C35 111.9(3) . . ? C39 C34 B1 119.9(3) . . ? C35 C34 B1 127.8(3) . . ? F11 C35 C36 115.4(3) . . ? F11 C35 C34 119.8(3) . . ? C36 C35 C34 124.8(3) . . ? F12 C36 C35 120.8(4) . . ? F12 C36 C37 119.4(4) . . ? C35 C36 C37 119.8(4) . . ? F13 C37 C38 121.8(4) . . ? F13 C37 C36 119.8(4) . . ? C38 C37 C36 118.4(4) . . ? C37 C38 F14 119.1(4) . . ? C37 C38 C39 119.8(4) . . ? F14 C38 C39 121.1(4) . . ? C38 C39 F15 116.2(3) . . ? C38 C39 C34 125.2(3) . . ? F15 C39 C34 118.6(3) . . ? C45 C40 C41 111.9(3) . . ? C45 C40 B1 119.7(3) . . ? C41 C40 B1 127.6(3) . . ? F16 C41 C42 115.3(3) . . ? F16 C41 C40 120.1(3) . . ? C42 C41 C40 124.6(3) . . ? C43 C42 F17 120.6(4) . . ? C43 C42 C41 120.5(3) . . ? F17 C42 C41 118.8(4) . . ? F18 C43 C42 122.3(4) . . ? F18 C43 C44 119.7(4) . . ? C42 C43 C44 118.0(4) . . ? F19 C44 C45 120.9(3) . . ? F19 C44 C43 119.3(3) . . ? C45 C44 C43 119.7(3) . . ? F20 C45 C44 115.9(3) . . ? F20 C45 C40 118.8(3) . . ? C44 C45 C40 125.2(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.340 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.035