Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Olivier Tardif' _publ_contact_author_email OLIVIER@RIKEN.JP _publ_section_title ; Generation of cationic indenyl silylamide gadolinium and scandium complexes [(Ind)Ln{N(SiMe3)2}]+[B(C6F5)4]- and their reactivity for 1,3-butadiene polymerization ; loop_ _publ_author_name 'Olivier Tardif' 'Shojiro Kaita' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 670476' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (IndMe)2GdN _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 Gd N Si2' _chemical_formula_sum 'C26 H36 Gd N Si2' _chemical_formula_weight 575.99 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' Gd Gd -0.1653 3.9035 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 11.0223(11) _cell_length_b 15.5294(15) _cell_length_c 15.0108(14) _cell_angle_alpha 90.00 _cell_angle_beta 91.161(2) _cell_angle_gamma 90.00 _cell_volume 2568.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 11619 _cell_measurement_theta_min 3.2532 _cell_measurement_theta_max 30.9807 _exptl_crystal_description Platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 2.688 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.1968 _exptl_absorpt_correction_T_max 0.4602 _exptl_absorpt_process_details NUMABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku AFC-8 with Saturn70 CCD detector' _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 39568 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7435 _reflns_number_gt 6459 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear SM (Rigaku/MSC, 2005)' _computing_cell_refinement 'CrystalClear SM' _computing_data_reduction 'CrystalClear SM' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL97 _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^)+(0.0168P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7435 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0531 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.007 _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 Gd1 Gd 0.110563(8) 0.211978(5) 0.676582(6) 0.01119(4) Uani 1 1 d . . . N1 N -0.07221(15) 0.27618(9) 0.68047(11) 0.0148(3) Uani 1 1 d . . . Si1 Si -0.11167(5) 0.38041(3) 0.70313(4) 0.01767(11) Uani 1 1 d . . . Si2 Si -0.17084(5) 0.19292(3) 0.66488(4) 0.01606(11) Uani 1 1 d . . . C1 C 0.3743(2) 0.33742(13) 0.76878(15) 0.0302(5) Uani 1 1 d . . . H1A H 0.4441 0.3349 0.8102 0.045 Uiso 1 1 calc R . . H1B H 0.3373 0.3947 0.7714 0.045 Uiso 1 1 calc R . . H1C H 0.4014 0.3262 0.7081 0.045 Uiso 1 1 calc R . . C2 C 0.2826(2) 0.27063(12) 0.79430(14) 0.0201(4) Uani 1 1 d . . . C3 C 0.1688(2) 0.28705(11) 0.83129(14) 0.0192(4) Uani 1 1 d . . . H3 H 0.1332 0.3423 0.8385 0.023 Uiso 1 1 calc R . . C4 C 0.1154(2) 0.20735(11) 0.85610(13) 0.0163(4) Uani 1 1 d . . . C5 C 0.00516(19) 0.18416(13) 0.89711(13) 0.0208(4) Uani 1 1 d . . . H5 H -0.0516 0.2273 0.9130 0.025 Uiso 1 1 calc R . . C6 C -0.01872(19) 0.09957(13) 0.91348(12) 0.0214(4) Uani 1 1 d . . . H6 H -0.0917 0.0843 0.9421 0.026 Uiso 1 1 calc R . . C7 C 0.06324(19) 0.03409(13) 0.88866(13) 0.0220(4) Uani 1 1 d . . . H7 H 0.0443 -0.0243 0.9012 0.026 Uiso 1 1 calc R . . C8 C 0.16892(19) 0.05309(12) 0.84711(12) 0.0198(4) Uani 1 1 d . . . H8 H 0.2222 0.0083 0.8298 0.024 Uiso 1 1 calc R . . C9 C 0.19861(17) 0.14047(12) 0.83003(12) 0.0151(4) Uani 1 1 d . . . C10 C 0.29954(18) 0.18069(12) 0.78999(13) 0.0185(4) Uani 1 1 d . . . H10 H 0.3668 0.1520 0.7647 0.022 Uiso 1 1 calc R . . C11 C 0.0362(2) 0.33896(15) 0.46881(14) 0.0310(5) Uani 1 1 d . . . H11A H 0.0295 0.3349 0.4037 0.047 Uiso 1 1 calc R . . H11B H 0.0685 0.3956 0.4856 0.047 Uiso 1 1 calc R . . H11C H -0.0441 0.3314 0.4945 0.047 Uiso 1 1 calc R . . C12 C 0.12072(19) 0.26952(14) 0.50368(13) 0.0203(4) Uani 1 1 d . . . C13 C 0.23579(19) 0.28311(11) 0.54265(14) 0.0188(4) Uani 1 1 d . . . H13 H 0.2702 0.3374 0.5576 0.023 Uiso 1 1 calc R . . C14 C 0.29279(19) 0.20070(12) 0.55618(13) 0.0167(4) Uani 1 1 d . . . C15 C 0.41047(18) 0.17506(13) 0.58399(13) 0.0217(4) Uani 1 1 d . . . H15 H 0.4700 0.2171 0.5993 0.026 Uiso 1 1 calc R . . C16 C 0.43822(19) 0.08932(13) 0.58879(13) 0.0250(5) Uani 1 1 d . . . H16 H 0.5178 0.0720 0.6063 0.030 Uiso 1 1 calc R . . C17 C 0.3496(2) 0.02618(13) 0.56794(13) 0.0273(5) Uani 1 1 d . . . H17 H 0.3703 -0.0330 0.5735 0.033 Uiso 1 1 calc R . . C18 C 0.2348(2) 0.04828(12) 0.53993(13) 0.0227(4) Uani 1 1 d . . . H18 H 0.1761 0.0050 0.5269 0.027 Uiso 1 1 calc R . . C19 C 0.20448(18) 0.13654(12) 0.53059(12) 0.0168(4) Uani 1 1 d . . . C20 C 0.09881(19) 0.18013(13) 0.49973(12) 0.0198(4) Uani 1 1 d . . . H20 H 0.0255 0.1536 0.4797 0.024 Uiso 1 1 calc R . . C21 C 0.0207(2) 0.45354(12) 0.68516(14) 0.0267(5) Uani 1 1 d . . . H21A H 0.0873 0.4377 0.7262 0.040 Uiso 1 1 calc R . . H21B H -0.0035 0.5132 0.6962 0.040 Uiso 1 1 calc R . . H21C H 0.0476 0.4479 0.6236 0.040 Uiso 1 1 calc R . . C22 C -0.1588(2) 0.39615(13) 0.82139(13) 0.0276(5) Uani 1 1 d . . . H22A H -0.2278 0.3585 0.8338 0.041 Uiso 1 1 calc R . . H22B H -0.1823 0.4563 0.8303 0.041 Uiso 1 1 calc R . . H22C H -0.0908 0.3818 0.8618 0.041 Uiso 1 1 calc R . . C23 C -0.2412(2) 0.41989(15) 0.63141(16) 0.0367(6) Uani 1 1 d . . . H23A H -0.2192 0.4163 0.5686 0.055 Uiso 1 1 calc R . . H23B H -0.2593 0.4799 0.6466 0.055 Uiso 1 1 calc R . . H23C H -0.3129 0.3842 0.6416 0.055 Uiso 1 1 calc R . . C24 C -0.28924(19) 0.18205(14) 0.75185(14) 0.0254(5) Uani 1 1 d . . . H24A H -0.2499 0.1781 0.8108 0.038 Uiso 1 1 calc R . . H24B H -0.3371 0.1299 0.7405 0.038 Uiso 1 1 calc R . . H24C H -0.3427 0.2324 0.7498 0.038 Uiso 1 1 calc R . . C25 C -0.2485(2) 0.19211(14) 0.55303(14) 0.0263(5) Uani 1 1 d . . . H25A H -0.2998 0.2434 0.5468 0.039 Uiso 1 1 calc R . . H25B H -0.2989 0.1403 0.5473 0.039 Uiso 1 1 calc R . . H25C H -0.1875 0.1922 0.5064 0.039 Uiso 1 1 calc R . . C26 C -0.07634(17) 0.08967(11) 0.67151(13) 0.0189(4) Uani 1 1 d . . . H26A H -0.0137 0.0913 0.6261 0.028 Uiso 1 1 calc R . . H26B H -0.1292 0.0398 0.6610 0.028 Uiso 1 1 calc R . . H26C H -0.0378 0.0851 0.7307 0.028 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 Gd1 0.01053(5) 0.01466(5) 0.00836(6) 0.00033(3) -0.00033(4) 0.00008(3) N1 0.0135(8) 0.0175(7) 0.0132(8) 0.0015(6) -0.0013(6) 0.0015(6) Si1 0.0161(3) 0.0174(3) 0.0194(3) 0.0007(2) 0.0001(2) 0.0041(2) Si2 0.0120(3) 0.0224(3) 0.0137(3) -0.0001(2) -0.0006(2) -0.0023(2) C1 0.0289(13) 0.0287(11) 0.0325(13) 0.0064(10) -0.0106(10) -0.0111(9) C2 0.0220(11) 0.0215(9) 0.0164(11) 0.0025(8) -0.0093(8) -0.0044(8) C3 0.0277(12) 0.0157(9) 0.0139(11) -0.0033(7) -0.0074(9) 0.0010(7) C4 0.0221(11) 0.0184(9) 0.0081(10) -0.0012(7) -0.0042(8) 0.0037(7) C5 0.0266(12) 0.0259(10) 0.0100(10) -0.0015(8) 0.0011(8) 0.0072(9) C6 0.0219(11) 0.0314(11) 0.0109(10) 0.0042(8) 0.0034(8) 0.0001(8) C7 0.0285(12) 0.0211(10) 0.0164(10) 0.0066(8) -0.0013(8) -0.0006(8) C8 0.0258(11) 0.0173(9) 0.0161(10) 0.0020(8) -0.0016(8) 0.0058(8) C9 0.0165(9) 0.0189(9) 0.0099(9) 0.0018(7) -0.0033(7) 0.0031(7) C10 0.0165(10) 0.0222(10) 0.0167(10) 0.0045(8) -0.0052(8) 0.0017(8) C11 0.0303(13) 0.0423(13) 0.0207(12) 0.0100(10) 0.0022(9) 0.0147(10) C12 0.0191(11) 0.0331(11) 0.0090(10) 0.0050(8) 0.0031(8) 0.0064(8) C13 0.0202(11) 0.0183(9) 0.0181(11) 0.0053(7) 0.0060(8) 0.0008(7) C14 0.0153(10) 0.0223(9) 0.0128(10) 0.0030(7) 0.0047(8) 0.0010(7) C15 0.0149(10) 0.0297(11) 0.0204(11) 0.0031(9) 0.0020(8) -0.0018(8) C16 0.0202(11) 0.0347(12) 0.0204(11) 0.0074(9) 0.0042(8) 0.0122(9) C17 0.0383(14) 0.0223(10) 0.0216(11) 0.0050(9) 0.0095(9) 0.0100(9) C18 0.0305(12) 0.0203(10) 0.0176(10) -0.0029(8) 0.0064(8) -0.0029(8) C19 0.0176(10) 0.0244(9) 0.0085(9) -0.0003(8) 0.0043(7) 0.0003(8) C20 0.0192(11) 0.0316(11) 0.0086(9) -0.0002(8) -0.0002(7) -0.0005(8) C21 0.0320(13) 0.0196(10) 0.0286(12) 0.0036(9) 0.0014(9) -0.0020(9) C22 0.0285(12) 0.0256(11) 0.0291(12) -0.0064(9) 0.0064(9) 0.0034(9) C23 0.0300(14) 0.0366(13) 0.0432(14) -0.0009(11) -0.0092(11) 0.0158(10) C24 0.0185(11) 0.0352(11) 0.0227(11) -0.0015(10) 0.0037(8) -0.0048(9) C25 0.0165(11) 0.0394(12) 0.0227(12) -0.0013(10) -0.0032(9) -0.0044(9) C26 0.0186(10) 0.0182(9) 0.0199(10) -0.0011(8) -0.0008(8) -0.0058(7) _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 Gd1 N1 2.2496(16) . ? Gd1 C3 2.665(2) . ? Gd1 C4 2.695(2) . ? Gd1 C13 2.6982(19) . ? Gd1 C20 2.7009(19) . ? Gd1 C10 2.7072(19) . ? Gd1 C19 2.7090(18) . ? Gd1 C9 2.7185(17) . ? Gd1 C2 2.723(2) . ? Gd1 C14 2.7347(19) . ? Gd1 C12 2.749(2) . ? Gd1 Si2 3.1172(6) . ? N1 Si2 1.7023(16) . ? N1 Si1 1.7121(15) . ? Si1 C21 1.873(2) . ? Si1 C23 1.874(2) . ? Si1 C22 1.876(2) . ? Si2 C25 1.869(2) . ? Si2 C24 1.872(2) . ? Si2 C26 1.9135(19) . ? C1 C2 1.503(3) . ? C2 C3 1.406(3) . ? C2 C10 1.411(3) . ? C3 C4 1.423(3) . ? C4 C5 1.420(3) . ? C4 C9 1.445(3) . ? C5 C6 1.363(3) . ? C6 C7 1.415(3) . ? C7 C8 1.365(3) . ? C8 C9 1.420(3) . ? C9 C10 1.420(3) . ? C11 C12 1.511(3) . ? C12 C13 1.402(3) . ? C12 C20 1.410(3) . ? C13 C14 1.438(2) . ? C14 C15 1.412(3) . ? C14 C19 1.440(3) . ? C15 C16 1.368(3) . ? C16 C17 1.414(3) . ? C17 C18 1.370(3) . ? C18 C19 1.417(3) . ? C19 C20 1.417(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 N1 Gd1 C3 89.05(6) . . ? N1 Gd1 C4 89.17(6) . . ? C3 Gd1 C4 30.78(6) . . ? N1 Gd1 C13 108.05(6) . . ? C3 Gd1 C13 110.64(7) . . ? C4 Gd1 C13 139.10(7) . . ? N1 Gd1 C20 94.68(6) . . ? C3 Gd1 C20 160.46(6) . . ? C4 Gd1 C20 167.81(6) . . ? C13 Gd1 C20 50.03(6) . . ? N1 Gd1 C10 137.84(6) . . ? C3 Gd1 C10 50.36(6) . . ? C4 Gd1 C10 50.73(6) . . ? C13 Gd1 C10 98.24(6) . . ? C20 Gd1 C10 127.31(6) . . ? N1 Gd1 C19 124.73(6) . . ? C3 Gd1 C19 143.60(6) . . ? C4 Gd1 C19 142.86(6) . . ? C13 Gd1 C19 50.55(6) . . ? C20 Gd1 C19 30.37(6) . . ? C10 Gd1 C19 97.43(6) . . ? N1 Gd1 C9 117.62(6) . . ? C3 Gd1 C9 50.57(6) . . ? C4 Gd1 C9 30.95(5) . . ? C13 Gd1 C9 128.27(6) . . ? C20 Gd1 C9 140.10(6) . . ? C10 Gd1 C9 30.34(5) . . ? C19 Gd1 C9 111.91(6) . . ? N1 Gd1 C2 116.57(6) . . ? C3 Gd1 C2 30.23(6) . . ? C4 Gd1 C2 50.25(6) . . ? C13 Gd1 C2 89.23(7) . . ? C20 Gd1 C2 135.89(6) . . ? C10 Gd1 C2 30.12(6) . . ? C19 Gd1 C2 113.40(6) . . ? C9 Gd1 C2 49.81(6) . . ? N1 Gd1 C14 135.70(6) . . ? C3 Gd1 C14 115.91(7) . . ? C4 Gd1 C14 131.23(6) . . ? C13 Gd1 C14 30.69(5) . . ? C20 Gd1 C14 50.20(6) . . ? C10 Gd1 C14 80.68(6) . . ? C19 Gd1 C14 30.66(6) . . ? C9 Gd1 C14 106.23(6) . . ? C2 Gd1 C14 86.51(7) . . ? N1 Gd1 C12 86.22(6) . . ? C3 Gd1 C12 131.81(6) . . ? C4 Gd1 C12 162.21(6) . . ? C13 Gd1 C12 29.81(6) . . ? C20 Gd1 C12 29.97(6) . . ? C10 Gd1 C12 127.33(6) . . ? C19 Gd1 C12 49.71(6) . . ? C9 Gd1 C12 155.78(6) . . ? C2 Gd1 C12 117.57(6) . . ? C14 Gd1 C12 49.64(6) . . ? N1 Gd1 Si2 32.11(4) . . ? C3 Gd1 Si2 108.19(5) . . ? C4 Gd1 Si2 93.06(5) . . ? C13 Gd1 Si2 121.36(5) . . ? C20 Gd1 Si2 84.23(5) . . ? C10 Gd1 Si2 140.39(4) . . ? C19 Gd1 Si2 108.03(4) . . ? C9 Gd1 Si2 110.29(4) . . ? C2 Gd1 Si2 138.38(5) . . ? C14 Gd1 Si2 134.43(5) . . ? C12 Gd1 Si2 92.13(5) . . ? Si2 N1 Si1 125.54(10) . . ? Si2 N1 Gd1 103.27(7) . . ? Si1 N1 Gd1 130.95(9) . . ? N1 Si1 C21 110.05(9) . . ? N1 Si1 C23 112.88(10) . . ? C21 Si1 C23 107.80(11) . . ? N1 Si1 C22 112.80(9) . . ? C21 Si1 C22 106.78(10) . . ? C23 Si1 C22 106.19(11) . . ? N1 Si2 C25 114.09(9) . . ? N1 Si2 C24 115.15(9) . . ? C25 Si2 C24 108.22(10) . . ? N1 Si2 C26 106.49(8) . . ? C25 Si2 C26 106.25(9) . . ? C24 Si2 C26 105.94(9) . . ? C25 Si2 Gd1 119.23(7) . . ? C24 Si2 Gd1 132.55(7) . . ? C26 Si2 Gd1 62.40(6) . . ? C3 C2 C10 108.52(17) . . ? C3 C2 C1 125.84(19) . . ? C10 C2 C1 125.5(2) . . ? C3 C2 Gd1 72.62(12) . . ? C10 C2 Gd1 74.34(11) . . ? C1 C2 Gd1 121.91(13) . . ? C2 C3 C4 108.80(17) . . ? C2 C3 Gd1 77.14(12) . . ? C4 C3 Gd1 75.77(11) . . ? C5 C4 C3 134.10(19) . . ? C5 C4 C9 119.25(17) . . ? C3 C4 C9 106.65(19) . . ? C5 C4 Gd1 116.13(14) . . ? C3 C4 Gd1 73.44(11) . . ? C9 C4 Gd1 75.41(11) . . ? C6 C5 C4 119.52(18) . . ? C5 C6 C7 121.23(19) . . ? C8 C7 C6 121.35(18) . . ? C7 C8 C9 119.41(18) . . ? C10 C9 C8 133.00(18) . . ? C10 C9 C4 107.78(16) . . ? C8 C9 C4 119.21(17) . . ? C10 C9 Gd1 74.39(10) . . ? C8 C9 Gd1 117.62(12) . . ? C4 C9 Gd1 73.63(10) . . ? C2 C10 C9 108.10(17) . . ? C2 C10 Gd1 75.55(11) . . ? C9 C10 Gd1 75.27(11) . . ? C13 C12 C20 108.58(17) . . ? C13 C12 C11 125.7(2) . . ? C20 C12 C11 125.7(2) . . ? C13 C12 Gd1 73.08(11) . . ? C20 C12 Gd1 73.12(10) . . ? C11 C12 Gd1 121.48(13) . . ? C12 C13 C14 108.29(17) . . ? C12 C13 Gd1 77.12(12) . . ? C14 C13 Gd1 76.06(11) . . ? C15 C14 C13 133.53(19) . . ? C15 C14 C19 119.73(17) . . ? C13 C14 C19 106.69(18) . . ? C15 C14 Gd1 120.35(13) . . ? C13 C14 Gd1 73.25(11) . . ? C19 C14 Gd1 73.68(11) . . ? C16 C15 C14 119.55(19) . . ? C15 C16 C17 120.70(19) . . ? C18 C17 C16 121.60(19) . . ? C17 C18 C19 119.15(19) . . ? C18 C19 C20 133.23(19) . . ? C18 C19 C14 119.11(18) . . ? C20 C19 C14 107.67(17) . . ? C18 C19 Gd1 115.55(12) . . ? C20 C19 Gd1 74.50(11) . . ? C14 C19 Gd1 75.65(11) . . ? C12 C20 C19 108.52(18) . . ? C12 C20 Gd1 76.91(11) . . ? C19 C20 Gd1 75.13(10) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.112 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.095 #===END #Attachment 'compound 7.cif' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 670547' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (IndMe)(THF)3GdNTMS _chemical_melting_point ? _chemical_formula_moiety 'C28 H51 Gd N O3 Si2, C24 H20 B' _chemical_formula_sum 'C52 H71 B Gd N O3 Si2' _chemical_formula_weight 982.34 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' Gd Gd -0.1653 3.9035 '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' Si Si 0.0817 0.0704 '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+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 15.4220(14) _cell_length_b 23.773(2) _cell_length_c 27.047(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9916.5(15) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 11516 _cell_measurement_theta_min 3.0409 _cell_measurement_theta_max 27.4920 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4088 _exptl_absorpt_coefficient_mu 1.427 _exptl_absorpt_correction_type NUMERICAL _exptl_absorpt_correction_T_min 0.4956 _exptl_absorpt_correction_T_max 0.7399 _exptl_absorpt_process_details NUMABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku AFC-8 with Saturn70 CCD detector' _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 43594 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.52 _reflns_number_total 11297 _reflns_number_gt 8891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear SM (Rigaku/MSC, 2005)' _computing_cell_refinement 'CrystalClear SM' _computing_data_reduction 'CrystalClear SM' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL97 _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^)+(0.0402P)^2^+4.6031P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11297 _refine_ls_number_parameters 549 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.019 _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 Gd1 Gd 0.797854(8) 0.218257(5) 0.097443(5) 0.01935(5) Uani 1 1 d . . . B1 B 0.7723(2) 0.00029(14) 0.37650(13) 0.0292(7) Uani 1 1 d . . . N1 N 0.82975(16) 0.28899(9) 0.15118(9) 0.0265(5) Uani 1 1 d . . . O1 O 0.81171(14) 0.14457(9) 0.15805(8) 0.0350(5) Uani 1 1 d . . . O2 O 0.87656(13) 0.13983(8) 0.05302(8) 0.0304(5) Uani 1 1 d . . . O3 O 0.86443(13) 0.26916(8) 0.03120(8) 0.0283(4) Uani 1 1 d . . . Si1 Si 0.93899(6) 0.28950(4) 0.16422(4) 0.0357(2) Uani 1 1 d . . . Si2 Si 0.76660(6) 0.33780(3) 0.18208(3) 0.02934(18) Uani 1 1 d . . . C1 C 0.5994(2) 0.16666(14) 0.16464(13) 0.0438(8) Uani 1 1 d . . . H1A H 0.5370 0.1589 0.1638 0.066 Uiso 1 1 calc R . . H1B H 0.6120 0.1935 0.1912 0.066 Uiso 1 1 calc R . . H1C H 0.6310 0.1316 0.1707 0.066 Uiso 1 1 calc R . . C2 C 0.62732(19) 0.19117(13) 0.11587(12) 0.0302(7) Uani 1 1 d . . . C3 C 0.65003(19) 0.16037(12) 0.07326(12) 0.0322(7) Uani 1 1 d . . . H3 H 0.6574 0.1207 0.0715 0.039 Uiso 1 1 calc R . . C4 C 0.66011(18) 0.19877(12) 0.03328(11) 0.0281(6) Uani 1 1 d . . . C5 C 0.6738(2) 0.19142(14) -0.01801(12) 0.0345(7) Uani 1 1 d . . . H5 H 0.6825 0.1548 -0.0312 0.041 Uiso 1 1 calc R . . C6 C 0.6743(2) 0.23723(15) -0.04840(12) 0.0394(8) Uani 1 1 d . . . H6 H 0.6834 0.2322 -0.0829 0.047 Uiso 1 1 calc R . . C7 C 0.6616(2) 0.29199(15) -0.02950(13) 0.0393(8) Uani 1 1 d . . . H7 H 0.6622 0.3231 -0.0516 0.047 Uiso 1 1 calc R . . C8 C 0.64832(19) 0.30133(13) 0.01999(12) 0.0325(7) Uani 1 1 d . . . H8 H 0.6402 0.3384 0.0322 0.039 Uiso 1 1 calc R . . C9 C 0.64705(17) 0.25446(12) 0.05248(11) 0.0271(6) Uani 1 1 d . . . C10 C 0.62923(18) 0.24920(13) 0.10413(11) 0.0290(6) Uani 1 1 d . . . H10 H 0.6203 0.2793 0.1266 0.035 Uiso 1 1 calc R . . C11 C 0.9650(3) 0.28020(17) 0.23162(15) 0.0568(11) Uani 1 1 d . . . H11A H 0.9896 0.3152 0.2447 0.085 Uiso 1 1 calc R . . H11B H 1.0072 0.2497 0.2355 0.085 Uiso 1 1 calc R . . H11C H 0.9119 0.2709 0.2498 0.085 Uiso 1 1 calc R . . C12 C 1.0023(2) 0.35120(16) 0.14004(15) 0.0575(11) Uani 1 1 d . . . H12A H 1.0178 0.3445 0.1054 0.086 Uiso 1 1 calc R . . H12B H 1.0552 0.3559 0.1597 0.086 Uiso 1 1 calc R . . H12C H 0.9668 0.3853 0.1425 0.086 Uiso 1 1 calc R . . C13 C 0.9869(2) 0.22790(14) 0.13053(13) 0.0404(8) Uani 1 1 d . . . H13A H 0.9580 0.1933 0.1412 0.061 Uiso 1 1 calc R . . H13B H 1.0490 0.2254 0.1379 0.061 Uiso 1 1 calc R . . H13C H 0.9787 0.2329 0.0949 0.061 Uiso 1 1 calc R . . C14 C 0.6932(2) 0.30343(15) 0.22761(14) 0.0427(8) Uani 1 1 d . . . H14A H 0.6545 0.2773 0.2103 0.064 Uiso 1 1 calc R . . H14B H 0.6587 0.3322 0.2446 0.064 Uiso 1 1 calc R . . H14C H 0.7278 0.2827 0.2519 0.064 Uiso 1 1 calc R . . C15 C 0.7030(2) 0.38300(14) 0.13854(15) 0.0496(10) Uani 1 1 d . . . H15A H 0.7423 0.4089 0.1214 0.074 Uiso 1 1 calc R . . H15B H 0.6599 0.4046 0.1572 0.074 Uiso 1 1 calc R . . H15C H 0.6735 0.3592 0.1142 0.074 Uiso 1 1 calc R . . C16 C 0.8297(3) 0.39028(15) 0.21908(16) 0.0552(11) Uani 1 1 d . . . H16A H 0.8571 0.3714 0.2472 0.083 Uiso 1 1 calc R . . H16B H 0.7905 0.4197 0.2312 0.083 Uiso 1 1 calc R . . H16C H 0.8745 0.4073 0.1982 0.083 Uiso 1 1 calc R . . C17 C 0.8312(3) 0.15214(15) 0.21074(13) 0.0471(9) Uani 1 1 d . . . H17A H 0.7810 0.1689 0.2282 0.056 Uiso 1 1 calc R . . H17B H 0.8820 0.1771 0.2151 0.056 Uiso 1 1 calc R . . C18 C 0.8500(3) 0.09448(15) 0.23019(15) 0.0567(10) Uani 1 1 d . . . H18A H 0.9128 0.0861 0.2284 0.068 Uiso 1 1 calc R . . H18B H 0.8305 0.0907 0.2649 0.068 Uiso 1 1 calc R . . C19 C 0.7998(4) 0.05664(18) 0.19705(17) 0.0874(19) Uani 1 1 d . . . H19A H 0.8282 0.0194 0.1945 0.105 Uiso 1 1 calc R . . H19B H 0.7401 0.0513 0.2098 0.105 Uiso 1 1 calc R . . C20 C 0.7981(3) 0.08446(14) 0.14898(15) 0.0532(11) Uani 1 1 d . . . H20A H 0.7416 0.0782 0.1325 0.064 Uiso 1 1 calc R . . H20B H 0.8446 0.0694 0.1275 0.064 Uiso 1 1 calc R . . C21 C 0.9671(2) 0.12245(17) 0.05969(18) 0.0641(13) Uani 1 1 d . . . H21A H 0.9770 0.1089 0.0938 0.077 Uiso 1 1 calc R . . H21B H 1.0070 0.1542 0.0530 0.077 Uiso 1 1 calc R . . C22 C 0.9808(3) 0.0757(2) 0.0229(3) 0.119(3) Uani 1 1 d . . . H22A H 1.0091 0.0903 -0.0073 0.143 Uiso 1 1 calc R . . H22B H 1.0181 0.0460 0.0373 0.143 Uiso 1 1 calc R . . C23 C 0.9013(3) 0.0545(2) 0.0119(2) 0.0875(18) Uani 1 1 d . . . H23A H 0.8859 0.0241 0.0353 0.105 Uiso 1 1 calc R . . H23B H 0.9009 0.0390 -0.0220 0.105 Uiso 1 1 calc R . . C24 C 0.8380(2) 0.10225(13) 0.01611(13) 0.0382(8) Uani 1 1 d . . . H24A H 0.8312 0.1217 -0.0160 0.046 Uiso 1 1 calc R . . H24B H 0.7806 0.0886 0.0272 0.046 Uiso 1 1 calc R . . C25 C 0.9070(2) 0.24778(13) -0.01317(12) 0.0364(7) Uani 1 1 d . . . H25A H 0.8710 0.2185 -0.0292 0.044 Uiso 1 1 calc R . . H25B H 0.9642 0.2314 -0.0049 0.044 Uiso 1 1 calc R . . C26 C 0.9173(2) 0.29811(14) -0.04676(13) 0.0407(8) Uani 1 1 d . . . H26A H 0.8653 0.3036 -0.0677 0.049 Uiso 1 1 calc R . . H26B H 0.9689 0.2941 -0.0683 0.049 Uiso 1 1 calc R . . C27 C 0.9284(2) 0.34624(13) -0.01046(13) 0.0410(8) Uani 1 1 d . . . H27A H 0.9883 0.3477 0.0026 0.049 Uiso 1 1 calc R . . H27B H 0.9140 0.3828 -0.0260 0.049 Uiso 1 1 calc R . . C28 C 0.8644(2) 0.33147(11) 0.02952(13) 0.0349(7) Uani 1 1 d . . . H28A H 0.8827 0.3474 0.0617 0.042 Uiso 1 1 calc R . . H28B H 0.8060 0.3460 0.0213 0.042 Uiso 1 1 calc R . . C29 C 0.7495(2) 0.03800(12) 0.46851(13) 0.0381(8) Uani 1 1 d . . . H29 H 0.7021 0.0593 0.4561 0.046 Uiso 1 1 calc R . . C30 C 0.7667(3) 0.03979(13) 0.51858(14) 0.0511(10) Uani 1 1 d . . . H30 H 0.7305 0.0614 0.5397 0.061 Uiso 1 1 calc R . . C31 C 0.8356(3) 0.01064(14) 0.53821(14) 0.0531(10) Uani 1 1 d . . . H31 H 0.8479 0.0124 0.5726 0.064 Uiso 1 1 calc R . . C32 C 0.8864(2) -0.02125(14) 0.50678(13) 0.0466(9) Uani 1 1 d . . . H32 H 0.9346 -0.0415 0.5195 0.056 Uiso 1 1 calc R . . C33 C 0.8673(2) -0.02376(12) 0.45641(12) 0.0357(7) Uani 1 1 d . . . H33 H 0.9022 -0.0468 0.4357 0.043 Uiso 1 1 calc R . . C34 C 0.79861(19) 0.00627(12) 0.43515(12) 0.0285(6) Uani 1 1 d . . . C35 C 0.7039(2) -0.05242(13) 0.37423(12) 0.0329(7) Uani 1 1 d . . . C36 C 0.6143(2) -0.04540(17) 0.37918(16) 0.0554(10) Uani 1 1 d . . . H36 H 0.5918 -0.0084 0.3829 0.066 Uiso 1 1 calc R . . C37 C 0.5569(3) -0.0904(2) 0.3789(2) 0.0766(15) Uani 1 1 d . . . H37 H 0.4965 -0.0835 0.3823 0.092 Uiso 1 1 calc R . . C38 C 0.5860(3) -0.14434(19) 0.37381(18) 0.0726(15) Uani 1 1 d . . . H38 H 0.5464 -0.1749 0.3728 0.087 Uiso 1 1 calc R . . C39 C 0.6732(3) -0.15341(16) 0.37025(16) 0.0600(12) Uani 1 1 d . . . H39 H 0.6946 -0.1907 0.3674 0.072 Uiso 1 1 calc R . . C40 C 0.7309(3) -0.10851(13) 0.37076(13) 0.0408(8) Uani 1 1 d . . . H40 H 0.7912 -0.1162 0.3687 0.049 Uiso 1 1 calc R . . C41 C 0.8575(2) -0.00940(11) 0.34141(12) 0.0304(7) Uani 1 1 d . . . C42 C 0.8534(2) -0.03988(13) 0.29722(12) 0.0384(8) Uani 1 1 d . . . H42 H 0.8010 -0.0590 0.2895 0.046 Uiso 1 1 calc R . . C43 C 0.9216(3) -0.04368(15) 0.26414(14) 0.0516(10) Uani 1 1 d . . . H43 H 0.9154 -0.0652 0.2347 0.062 Uiso 1 1 calc R . . C44 C 1.0057(2) 0.01379(15) 0.31678(18) 0.0550(11) Uani 1 1 d . . . H44 H 1.0586 0.0326 0.3239 0.066 Uiso 1 1 calc R . . C45 C 0.9977(3) -0.01665(15) 0.27371(16) 0.0562(11) Uani 1 1 d . . . H45 H 1.0446 -0.0188 0.2510 0.067 Uiso 1 1 calc R . . C46 C 0.9364(2) 0.01728(13) 0.35028(14) 0.0412(8) Uani 1 1 d . . . H46 H 0.9435 0.0384 0.3798 0.049 Uiso 1 1 calc R . . C47 C 0.7304(2) 0.05904(13) 0.35454(12) 0.0313(7) Uani 1 1 d . . . C48 C 0.6675(2) 0.06019(16) 0.31741(13) 0.0447(8) Uani 1 1 d . . . H48 H 0.6440 0.0255 0.3064 0.054 Uiso 1 1 calc R . . C49 C 0.6375(3) 0.10959(18) 0.29570(15) 0.0568(11) Uani 1 1 d . . . H49 H 0.5933 0.1081 0.2713 0.068 Uiso 1 1 calc R . . C50 C 0.6718(3) 0.16034(17) 0.30964(15) 0.0564(11) Uani 1 1 d . . . H50 H 0.6519 0.1943 0.2950 0.068 Uiso 1 1 calc R . . C51 C 0.7359(3) 0.16111(14) 0.34539(14) 0.0528(10) Uani 1 1 d . . . H51 H 0.7610 0.1959 0.3550 0.063 Uiso 1 1 calc R . . C52 C 0.7639(3) 0.11148(12) 0.36745(13) 0.0411(8) Uani 1 1 d . . . H52 H 0.8075 0.1134 0.3922 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01650(8) 0.01939(8) 0.02216(8) 0.00071(5) -0.00132(5) -0.00040(5) B1 0.0295(18) 0.0270(16) 0.0309(19) -0.0017(13) -0.0031(15) -0.0026(14) N1 0.0191(12) 0.0312(12) 0.0293(13) -0.0069(10) 0.0039(10) -0.0063(10) O1 0.0449(14) 0.0315(11) 0.0286(12) 0.0066(9) -0.0044(10) 0.0041(10) O2 0.0287(11) 0.0266(10) 0.0358(12) -0.0056(8) -0.0040(9) 0.0045(9) O3 0.0272(11) 0.0255(9) 0.0321(12) 0.0044(8) 0.0078(9) 0.0015(8) Si1 0.0198(4) 0.0504(5) 0.0368(5) -0.0166(4) 0.0006(4) -0.0067(4) Si2 0.0267(4) 0.0297(4) 0.0316(5) -0.0059(3) 0.0082(4) -0.0040(4) C1 0.040(2) 0.052(2) 0.040(2) 0.0080(16) 0.0049(16) -0.0082(17) C2 0.0207(15) 0.0376(16) 0.0324(17) 0.0043(13) -0.0019(13) -0.0065(13) C3 0.0252(16) 0.0298(14) 0.0415(19) 0.0016(13) -0.0054(14) -0.0040(13) C4 0.0181(14) 0.0324(14) 0.0337(17) -0.0026(12) -0.0053(13) -0.0023(12) C5 0.0248(16) 0.0443(17) 0.0345(18) -0.0052(14) -0.0087(14) -0.0015(14) C6 0.0284(17) 0.065(2) 0.0249(16) 0.0030(15) -0.0046(14) 0.0030(16) C7 0.0287(17) 0.0521(19) 0.0371(19) 0.0131(15) -0.0046(15) 0.0006(16) C8 0.0223(15) 0.0347(15) 0.0405(19) 0.0064(13) -0.0027(14) 0.0021(13) C9 0.0146(13) 0.0343(15) 0.0323(16) 0.0045(12) -0.0045(12) -0.0008(12) C10 0.0175(14) 0.0377(16) 0.0317(16) -0.0026(12) -0.0014(12) 0.0010(13) C11 0.038(2) 0.087(3) 0.046(2) -0.021(2) -0.0151(18) 0.001(2) C12 0.040(2) 0.070(2) 0.062(3) -0.030(2) 0.0171(19) -0.029(2) C13 0.0219(16) 0.061(2) 0.0388(19) -0.0116(16) -0.0054(14) 0.0072(15) C14 0.042(2) 0.0415(18) 0.044(2) -0.0062(16) 0.0137(16) -0.0042(15) C15 0.067(3) 0.0343(17) 0.047(2) -0.0003(16) 0.0077(19) 0.0135(17) C16 0.045(2) 0.052(2) 0.069(3) -0.030(2) 0.015(2) -0.0109(18) C17 0.063(2) 0.051(2) 0.0274(18) 0.0070(15) -0.0046(17) 0.0020(19) C18 0.070(3) 0.057(2) 0.043(2) 0.0136(18) -0.013(2) 0.010(2) C19 0.167(6) 0.047(2) 0.048(3) 0.018(2) -0.028(3) -0.009(3) C20 0.082(3) 0.0296(16) 0.048(2) 0.0092(15) -0.008(2) -0.0038(18) C21 0.039(2) 0.059(2) 0.094(4) -0.038(2) -0.022(2) 0.0213(19) C22 0.069(3) 0.107(4) 0.180(6) -0.112(4) -0.056(4) 0.052(3) C23 0.060(3) 0.078(3) 0.125(5) -0.070(3) -0.028(3) 0.026(2) C24 0.0348(18) 0.0398(17) 0.0399(19) -0.0117(14) -0.0056(15) 0.0043(15) C25 0.0380(19) 0.0357(16) 0.0355(18) 0.0027(14) 0.0135(15) 0.0085(15) C26 0.0380(19) 0.0452(17) 0.039(2) 0.0099(15) 0.0109(16) 0.0054(16) C27 0.0316(18) 0.0386(17) 0.053(2) 0.0101(16) 0.0077(16) -0.0033(15) C28 0.0342(18) 0.0235(14) 0.047(2) 0.0052(13) 0.0072(15) -0.0017(13) C29 0.048(2) 0.0290(15) 0.0370(19) 0.0032(13) 0.0038(15) -0.0014(15) C30 0.085(3) 0.0319(16) 0.037(2) -0.0038(15) 0.016(2) -0.0099(19) C31 0.087(3) 0.0373(18) 0.034(2) 0.0062(15) -0.007(2) -0.020(2) C32 0.054(2) 0.0417(18) 0.044(2) 0.0127(16) -0.0157(18) -0.0161(17) C33 0.0380(18) 0.0334(15) 0.0357(18) 0.0043(13) -0.0042(14) -0.0051(14) C34 0.0313(17) 0.0236(13) 0.0306(17) 0.0012(12) 0.0008(13) -0.0062(12) C35 0.0313(17) 0.0384(16) 0.0289(17) 0.0022(13) -0.0043(13) -0.0073(14) C36 0.041(2) 0.055(2) 0.070(3) 0.008(2) 0.003(2) -0.0106(19) C37 0.039(2) 0.094(4) 0.097(4) 0.028(3) -0.009(2) -0.028(2) C38 0.070(3) 0.070(3) 0.077(3) 0.028(2) -0.030(3) -0.045(3) C39 0.087(3) 0.0375(19) 0.055(3) 0.0110(17) -0.025(2) -0.022(2) C40 0.048(2) 0.0336(16) 0.041(2) 0.0044(14) -0.0126(16) -0.0075(16) C41 0.0306(17) 0.0249(13) 0.0357(17) 0.0060(12) 0.0018(13) 0.0035(13) C42 0.046(2) 0.0382(16) 0.0308(18) 0.0037(14) -0.0018(15) 0.0083(16) C43 0.073(3) 0.047(2) 0.034(2) 0.0108(16) 0.0121(19) 0.026(2) C44 0.038(2) 0.0406(19) 0.087(3) 0.022(2) 0.017(2) -0.0015(17) C45 0.061(3) 0.0439(19) 0.064(3) 0.0265(19) 0.031(2) 0.026(2) C46 0.0380(19) 0.0295(15) 0.056(2) 0.0026(15) 0.0069(16) -0.0035(15) C47 0.0270(15) 0.0367(15) 0.0303(17) 0.0008(13) 0.0040(13) 0.0035(14) C48 0.0377(19) 0.055(2) 0.041(2) 0.0075(17) -0.0019(16) 0.0027(17) C49 0.044(2) 0.080(3) 0.046(2) 0.020(2) 0.0024(18) 0.022(2) C50 0.070(3) 0.055(2) 0.045(2) 0.0203(18) 0.024(2) 0.038(2) C51 0.087(3) 0.0307(16) 0.041(2) 0.0021(15) 0.019(2) 0.0136(19) C52 0.058(2) 0.0308(15) 0.0343(18) -0.0006(13) 0.0057(17) 0.0043(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 Gd1 N1 2.276(2) . ? Gd1 O3 2.3935(19) . ? Gd1 O1 2.409(2) . ? Gd1 O2 2.5285(19) . ? Gd1 C10 2.709(3) . ? Gd1 C3 2.742(3) . ? Gd1 C2 2.753(3) . ? Gd1 C9 2.762(3) . ? Gd1 C4 2.782(3) . ? Gd1 Si1 3.2967(9) . ? B1 C41 1.637(5) . ? B1 C35 1.639(5) . ? B1 C34 1.643(5) . ? B1 C47 1.649(5) . ? N1 Si1 1.721(3) . ? N1 Si2 1.730(2) . ? O1 C20 1.465(4) . ? O1 C17 1.467(4) . ? O2 C24 1.466(4) . ? O2 C21 1.467(4) . ? O3 C25 1.459(3) . ? O3 C28 1.482(3) . ? Si1 C13 1.876(3) . ? Si1 C12 1.879(4) . ? Si1 C11 1.880(4) . ? Si2 C14 1.861(3) . ? Si2 C15 1.872(4) . ? Si2 C16 1.872(4) . ? C1 C2 1.505(4) . ? C2 C3 1.410(4) . ? C2 C10 1.416(4) . ? C3 C4 1.424(4) . ? C4 C5 1.414(4) . ? C4 C9 1.436(4) . ? C5 C6 1.365(5) . ? C6 C7 1.412(5) . ? C7 C8 1.372(5) . ? C8 C9 1.419(4) . ? C9 C10 1.429(4) . ? C17 C18 1.497(5) . ? C18 C19 1.488(6) . ? C19 C20 1.459(5) . ? C21 C22 1.507(5) . ? C22 C23 1.357(6) . ? C23 C24 1.502(5) . ? C25 C26 1.511(4) . ? C26 C27 1.517(5) . ? C27 C28 1.505(4) . ? C29 C30 1.381(5) . ? C29 C34 1.399(4) . ? C30 C31 1.375(6) . ? C31 C32 1.383(5) . ? C32 C33 1.395(4) . ? C33 C34 1.401(4) . ? C35 C36 1.399(5) . ? C35 C40 1.400(4) . ? C36 C37 1.388(5) . ? C37 C38 1.366(6) . ? C38 C39 1.366(6) . ? C39 C40 1.390(5) . ? C41 C46 1.394(4) . ? C41 C42 1.399(4) . ? C42 C43 1.384(5) . ? C43 C45 1.362(6) . ? C44 C45 1.377(6) . ? C44 C46 1.403(5) . ? C47 C52 1.394(4) . ? C47 C48 1.397(5) . ? C48 C49 1.392(5) . ? C49 C50 1.370(6) . ? C50 C51 1.383(6) . ? C51 C52 1.391(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 N1 Gd1 O3 90.67(8) . . ? N1 Gd1 O1 94.79(9) . . ? O3 Gd1 O1 147.05(7) . . ? N1 Gd1 O2 138.10(8) . . ? O3 Gd1 O2 79.12(6) . . ? O1 Gd1 O2 75.20(7) . . ? N1 Gd1 C10 87.95(9) . . ? O3 Gd1 C10 108.94(8) . . ? O1 Gd1 C10 103.72(8) . . ? O2 Gd1 C10 133.86(8) . . ? N1 Gd1 C3 134.64(9) . . ? O3 Gd1 C3 115.59(9) . . ? O1 Gd1 C3 82.59(8) . . ? O2 Gd1 C3 85.17(8) . . ? C10 Gd1 C3 49.76(9) . . ? N1 Gd1 C2 105.28(9) . . ? O3 Gd1 C2 131.57(8) . . ? O1 Gd1 C2 77.96(8) . . ? O2 Gd1 C2 111.85(8) . . ? C10 Gd1 C2 30.03(9) . . ? C3 Gd1 C2 29.73(9) . . ? N1 Gd1 C9 103.47(9) . . ? O3 Gd1 C9 82.77(8) . . ? O1 Gd1 C9 126.94(8) . . ? O2 Gd1 C9 115.14(8) . . ? C10 Gd1 C9 30.27(8) . . ? C3 Gd1 C9 49.55(8) . . ? C2 Gd1 C9 49.33(9) . . ? N1 Gd1 C4 133.34(9) . . ? O3 Gd1 C4 86.83(8) . . ? O1 Gd1 C4 111.79(8) . . ? O2 Gd1 C4 86.98(8) . . ? C10 Gd1 C4 49.74(9) . . ? C3 Gd1 C4 29.86(9) . . ? C2 Gd1 C4 49.05(9) . . ? C9 Gd1 C4 30.03(8) . . ? N1 Gd1 Si1 29.31(6) . . ? O3 Gd1 Si1 82.36(5) . . ? O1 Gd1 Si1 86.69(6) . . ? O2 Gd1 Si1 108.80(5) . . ? C10 Gd1 Si1 117.24(7) . . ? C3 Gd1 Si1 159.63(7) . . ? C2 Gd1 Si1 130.67(7) . . ? C9 Gd1 Si1 129.57(6) . . ? C4 Gd1 Si1 158.67(6) . . ? C41 B1 C35 112.8(3) . . ? C41 B1 C34 112.0(3) . . ? C35 B1 C34 105.1(2) . . ? C41 B1 C47 103.0(2) . . ? C35 B1 C47 112.5(3) . . ? C34 B1 C47 111.8(2) . . ? Si1 N1 Si2 116.57(14) . . ? Si1 N1 Gd1 110.33(12) . . ? Si2 N1 Gd1 133.02(13) . . ? C20 O1 C17 108.1(2) . . ? C20 O1 Gd1 125.7(2) . . ? C17 O1 Gd1 126.15(18) . . ? C24 O2 C21 107.3(2) . . ? C24 O2 Gd1 125.34(17) . . ? C21 O2 Gd1 127.31(18) . . ? C25 O3 C28 108.8(2) . . ? C25 O3 Gd1 129.23(16) . . ? C28 O3 Gd1 121.89(17) . . ? N1 Si1 C13 106.27(13) . . ? N1 Si1 C12 116.25(16) . . ? C13 Si1 C12 103.65(17) . . ? N1 Si1 C11 114.01(16) . . ? C13 Si1 C11 107.16(17) . . ? C12 Si1 C11 108.57(18) . . ? N1 Si1 Gd1 40.35(8) . . ? C13 Si1 Gd1 65.97(10) . . ? C12 Si1 Gd1 123.59(13) . . ? C11 Si1 Gd1 127.73(13) . . ? N1 Si2 C14 111.55(14) . . ? N1 Si2 C15 112.09(15) . . ? C14 Si2 C15 110.47(17) . . ? N1 Si2 C16 114.36(15) . . ? C14 Si2 C16 104.77(18) . . ? C15 Si2 C16 103.07(18) . . ? C3 C2 C10 108.5(3) . . ? C3 C2 C1 125.9(3) . . ? C10 C2 C1 125.4(3) . . ? C3 C2 Gd1 74.70(16) . . ? C10 C2 Gd1 73.24(16) . . ? C1 C2 Gd1 121.5(2) . . ? C2 C3 C4 108.4(3) . . ? C2 C3 Gd1 75.57(17) . . ? C4 C3 Gd1 76.62(16) . . ? C5 C4 C3 133.0(3) . . ? C5 C4 C9 119.3(3) . . ? C3 C4 C9 107.5(3) . . ? C5 C4 Gd1 121.3(2) . . ? C3 C4 Gd1 73.52(16) . . ? C9 C4 Gd1 74.22(16) . . ? C6 C5 C4 119.5(3) . . ? C5 C6 C7 121.1(3) . . ? C8 C7 C6 121.5(3) . . ? C7 C8 C9 118.6(3) . . ? C8 C9 C10 132.6(3) . . ? C8 C9 C4 119.9(3) . . ? C10 C9 C4 107.4(3) . . ? C8 C9 Gd1 120.37(19) . . ? C10 C9 Gd1 72.79(16) . . ? C4 C9 Gd1 75.75(16) . . ? C2 C10 C9 108.0(3) . . ? C2 C10 Gd1 76.72(17) . . ? C9 C10 Gd1 76.93(16) . . ? O1 C17 C18 105.6(3) . . ? C19 C18 C17 103.9(3) . . ? C20 C19 C18 105.8(4) . . ? C19 C20 O1 106.9(3) . . ? O2 C21 C22 105.1(3) . . ? C23 C22 C21 107.0(4) . . ? C22 C23 C24 106.9(3) . . ? O2 C24 C23 104.4(3) . . ? O3 C25 C26 105.4(2) . . ? C25 C26 C27 102.7(3) . . ? C28 C27 C26 102.4(3) . . ? O3 C28 C27 104.8(2) . . ? C30 C29 C34 123.0(3) . . ? C31 C30 C29 120.8(4) . . ? C30 C31 C32 118.5(4) . . ? C31 C32 C33 120.2(4) . . ? C32 C33 C34 122.6(3) . . ? C29 C34 C33 114.8(3) . . ? C29 C34 B1 122.4(3) . . ? C33 C34 B1 122.6(3) . . ? C36 C35 C40 114.4(3) . . ? C36 C35 B1 122.7(3) . . ? C40 C35 B1 122.7(3) . . ? C37 C36 C35 122.5(4) . . ? C38 C37 C36 121.0(4) . . ? C39 C38 C37 118.6(4) . . ? C38 C39 C40 120.6(4) . . ? C39 C40 C35 122.8(4) . . ? C46 C41 C42 114.9(3) . . ? C46 C41 B1 122.5(3) . . ? C42 C41 B1 122.2(3) . . ? C43 C42 C41 123.5(4) . . ? C45 C43 C42 120.1(4) . . ? C45 C44 C46 120.6(4) . . ? C43 C45 C44 119.0(3) . . ? C41 C46 C44 121.8(4) . . ? C52 C47 C48 114.8(3) . . ? C52 C47 B1 121.5(3) . . ? C48 C47 B1 123.2(3) . . ? C49 C48 C47 123.4(4) . . ? C50 C49 C48 119.9(4) . . ? C49 C50 C51 118.7(3) . . ? C50 C51 C52 120.7(4) . . ? C51 C52 C47 122.4(4) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.805 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.088 #===END #===END #Attachment 'compound5.cif' data_compound5 _database_code_depnum_ccdc_archive 'CCDC 670548' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common (IndMe)(PhNMe2)ScNTMS _chemical_melting_point ? _chemical_formula_moiety 'C24 H38 N2 Sc Si2, C24 B F20' _chemical_formula_sum 'C48 H38 B F20 N2 Sc Si2' _chemical_formula_weight 1134.75 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' F F 0.0171 0.0103 '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' Si Si 0.0817 0.0704 '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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.125(3) _cell_length_b 13.378(5) _cell_length_c 14.834(4) _cell_angle_alpha 96.813(7) _cell_angle_beta 92.136(4) _cell_angle_gamma 97.660(11) _cell_volume 2364.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 2077 _cell_measurement_theta_min 3.1698 _cell_measurement_theta_max 30.9952 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 0.324 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.8698 _exptl_absorpt_correction_T_max 0.9382 _exptl_absorpt_process_details NUMABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku AFC-8 with Saturn70 CCD detector' _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 26223 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 31.00 _reflns_number_total 14514 _reflns_number_gt 10210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear SM (Rigaku/MSC, 2005)' _computing_cell_refinement 'CrystalClear SM' _computing_data_reduction 'CrystalClear SM' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL97 _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^)+(0.0735P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14514 _refine_ls_number_parameters 677 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1214 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _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 0.25072(3) 0.43389(2) 0.25448(2) 0.01718(8) Uani 1 1 d . . . N1 N 0.34582(12) 0.56963(11) 0.26305(10) 0.0200(3) Uani 1 1 d . . . N2 N 0.34529(14) 0.31558(12) 0.31500(11) 0.0255(3) Uani 1 1 d . . . Si1 Si 0.35636(4) 0.68369(4) 0.33541(3) 0.02262(11) Uani 1 1 d . . . Si2 Si 0.41954(4) 0.55507(4) 0.16591(3) 0.02319(11) Uani 1 1 d . . . B1 B 0.77571(15) 0.02116(14) 0.24910(12) 0.0158(3) Uani 1 1 d . . . F1 F 0.55931(9) 0.09028(8) 0.27097(7) 0.0237(2) Uani 1 1 d . . . F2 F 0.37448(9) 0.03384(9) 0.16395(8) 0.0311(3) Uani 1 1 d . . . F3 F 0.37043(9) -0.10699(9) 0.01581(8) 0.0308(3) Uani 1 1 d . . . F4 F 0.55842(10) -0.19154(8) -0.02353(8) 0.0299(2) Uani 1 1 d . . . F5 F 0.74036(9) -0.14130(8) 0.08150(7) 0.0274(2) Uani 1 1 d . . . F6 F 0.75032(8) -0.19093(7) 0.26944(7) 0.0212(2) Uani 1 1 d . . . F7 F 0.89940(9) -0.32074(8) 0.24417(8) 0.0269(2) Uani 1 1 d . . . F8 F 1.10567(9) -0.25775(8) 0.19068(8) 0.0271(2) Uani 1 1 d . . . F9 F 1.16252(8) -0.05791(9) 0.16621(8) 0.0269(2) Uani 1 1 d . . . F10 F 1.01951(8) 0.07366(7) 0.19534(7) 0.0229(2) Uani 1 1 d . . . F11 F 0.84294(9) 0.06364(8) 0.07047(7) 0.0221(2) Uani 1 1 d . . . F12 F 0.85085(9) 0.23966(9) 0.00059(7) 0.0267(2) Uani 1 1 d . . . F13 F 0.80887(10) 0.41064(8) 0.10598(8) 0.0329(3) Uani 1 1 d . . . F14 F 0.75889(10) 0.40061(8) 0.28189(8) 0.0307(3) Uani 1 1 d . . . F15 F 0.75288(9) 0.22910(8) 0.35406(7) 0.0246(2) Uani 1 1 d . . . F16 F 0.94916(8) 0.11700(8) 0.38003(7) 0.0247(2) Uani 1 1 d . . . F17 F 0.96053(9) 0.11172(9) 0.55897(7) 0.0302(3) Uani 1 1 d . . . F18 F 0.78538(10) 0.01697(9) 0.64187(7) 0.0317(3) Uani 1 1 d . . . F19 F 0.59870(9) -0.07027(9) 0.54054(7) 0.0287(2) Uani 1 1 d . . . F20 F 0.58781(8) -0.07237(8) 0.36164(7) 0.0238(2) Uani 1 1 d . . . C1 C 0.01896(17) 0.43542(16) 0.39647(13) 0.0303(4) Uani 1 1 d . . . H1A H -0.0619 0.4167 0.3978 0.045 Uiso 1 1 calc R . . H1B H 0.0390 0.5078 0.4186 0.045 Uiso 1 1 calc R . . H1C H 0.0569 0.3950 0.4355 0.045 Uiso 1 1 calc R . . C2 C 0.05405(15) 0.41515(14) 0.30065(12) 0.0225(3) Uani 1 1 d . . . C3 C 0.06860(15) 0.48750(13) 0.23843(12) 0.0216(3) Uani 1 1 d . . . H3 H 0.0657 0.5583 0.2515 0.026 Uiso 1 1 calc R . . C4 C 0.08845(14) 0.43491(13) 0.15237(12) 0.0193(3) Uani 1 1 d . . . C5 C 0.10467(16) 0.46800(14) 0.06589(12) 0.0245(4) Uani 1 1 d . . . H5 H 0.1061 0.5376 0.0580 0.029 Uiso 1 1 calc R . . C6 C 0.11822(16) 0.39708(15) -0.00621(13) 0.0261(4) Uani 1 1 d . . . H6 H 0.1269 0.4178 -0.0649 0.031 Uiso 1 1 calc R . . C7 C 0.11946(16) 0.29371(14) 0.00533(12) 0.0254(4) Uani 1 1 d . . . H7 H 0.1285 0.2467 -0.0462 0.030 Uiso 1 1 calc R . . C8 C 0.10819(15) 0.25932(13) 0.08778(12) 0.0215(3) Uani 1 1 d . . . H8 H 0.1122 0.1901 0.0944 0.026 Uiso 1 1 calc R . . C9 C 0.09028(14) 0.32964(12) 0.16373(11) 0.0183(3) Uani 1 1 d . . . C10 C 0.07194(14) 0.31965(13) 0.25708(12) 0.0209(3) Uani 1 1 d . . . H10 H 0.0718 0.2592 0.2849 0.025 Uiso 1 1 calc R . . C11 C 0.22915(19) 0.68806(15) 0.40211(14) 0.0311(4) Uani 1 1 d . . . H11A H 0.1661 0.6968 0.3619 0.047 Uiso 1 1 calc R . . H11B H 0.2424 0.7452 0.4508 0.047 Uiso 1 1 calc R . . H11C H 0.2122 0.6244 0.4286 0.047 Uiso 1 1 calc R . . C12 C 0.37536(17) 0.79613(14) 0.27176(14) 0.0284(4) Uani 1 1 d . . . H12A H 0.4462 0.7985 0.2418 0.043 Uiso 1 1 calc R . . H12B H 0.3760 0.8583 0.3141 0.043 Uiso 1 1 calc R . . H12C H 0.3139 0.7908 0.2258 0.043 Uiso 1 1 calc R . . C13 C 0.47998(19) 0.69418(15) 0.41734(14) 0.0348(5) Uani 1 1 d . . . H13A H 0.4702 0.6380 0.4544 0.052 Uiso 1 1 calc R . . H13B H 0.4868 0.7590 0.4569 0.052 Uiso 1 1 calc R . . H13C H 0.5476 0.6910 0.3835 0.052 Uiso 1 1 calc R . . C14 C 0.38134(19) 0.63152(16) 0.07541(14) 0.0347(5) Uani 1 1 d . . . H14A H 0.3006 0.6324 0.0728 0.052 Uiso 1 1 calc R . . H14B H 0.4035 0.6012 0.0166 0.052 Uiso 1 1 calc R . . H14C H 0.4198 0.7012 0.0892 0.052 Uiso 1 1 calc R . . C15 C 0.57388(17) 0.57477(18) 0.18719(16) 0.0378(5) Uani 1 1 d . . . H15A H 0.5992 0.6463 0.2099 0.057 Uiso 1 1 calc R . . H15B H 0.6093 0.5565 0.1304 0.057 Uiso 1 1 calc R . . H15C H 0.5943 0.5318 0.2325 0.057 Uiso 1 1 calc R . . C16 C 0.37805(16) 0.41525(14) 0.11678(12) 0.0244(4) Uani 1 1 d . . . H16A H 0.4183 0.3722 0.1515 0.037 Uiso 1 1 calc R . . H16B H 0.3971 0.4058 0.0530 0.037 Uiso 1 1 calc R . . H16C H 0.2976 0.3963 0.1208 0.037 Uiso 1 1 calc R . . C17 C 0.47015(18) 0.33740(19) 0.32278(15) 0.0369(5) Uani 1 1 d . . . H17A H 0.4931 0.4099 0.3427 0.055 Uiso 1 1 calc R . . H17B H 0.4999 0.3191 0.2634 0.055 Uiso 1 1 calc R . . H17C H 0.4990 0.2974 0.3672 0.055 Uiso 1 1 calc R . . C18 C 0.3135(2) 0.20967(15) 0.26992(14) 0.0356(5) Uani 1 1 d . . . H18A H 0.3486 0.1629 0.3041 0.053 Uiso 1 1 calc R . . H18B H 0.3386 0.2044 0.2077 0.053 Uiso 1 1 calc R . . H18C H 0.2323 0.1920 0.2683 0.053 Uiso 1 1 calc R . . C19 C 0.30036(15) 0.33518(14) 0.40365(12) 0.0224(3) Uani 1 1 d . . . C20 C 0.32031(16) 0.43508(14) 0.44663(12) 0.0238(4) Uani 1 1 d . . . H20 H 0.3618 0.4863 0.4175 0.029 Uiso 1 1 calc R . . C21 C 0.28000(17) 0.46016(15) 0.53145(13) 0.0268(4) Uani 1 1 d . . . H21 H 0.2937 0.5284 0.5599 0.032 Uiso 1 1 calc R . . C22 C 0.22025(18) 0.38678(16) 0.57457(14) 0.0308(4) Uani 1 1 d . . . H22 H 0.1944 0.4038 0.6333 0.037 Uiso 1 1 calc R . . C23 C 0.19796(18) 0.28736(16) 0.53152(14) 0.0320(4) Uani 1 1 d . . . H23 H 0.1556 0.2369 0.5608 0.038 Uiso 1 1 calc R . . C24 C 0.23696(17) 0.26119(14) 0.44630(13) 0.0287(4) Uani 1 1 d . . . H24 H 0.2206 0.1933 0.4171 0.034 Uiso 1 1 calc R . . C25 C 0.66007(13) -0.02551(12) 0.18646(11) 0.0165(3) Uani 1 1 d . . . C26 C 0.56229(14) 0.01725(12) 0.20040(11) 0.0184(3) Uani 1 1 d . . . C27 C 0.46555(14) -0.00909(13) 0.14502(13) 0.0213(3) Uani 1 1 d . . . C28 C 0.46285(14) -0.08036(13) 0.06999(12) 0.0223(4) Uani 1 1 d . . . C29 C 0.55789(15) -0.12345(13) 0.05099(12) 0.0211(3) Uani 1 1 d . . . C30 C 0.65240(14) -0.09552(13) 0.10860(12) 0.0195(3) Uani 1 1 d . . . C31 C 0.87440(14) -0.05188(12) 0.23047(11) 0.0167(3) Uani 1 1 d . . . C32 C 0.85290(13) -0.15377(13) 0.24452(11) 0.0170(3) Uani 1 1 d . . . C33 C 0.92803(14) -0.22211(12) 0.23204(11) 0.0186(3) Uani 1 1 d . . . C34 C 1.03278(14) -0.19096(13) 0.20451(11) 0.0193(3) Uani 1 1 d . . . C35 C 1.06023(14) -0.09067(13) 0.19155(11) 0.0193(3) Uani 1 1 d . . . C36 C 0.98250(14) -0.02429(12) 0.20594(11) 0.0177(3) Uani 1 1 d . . . C37 C 0.80077(13) 0.13580(12) 0.21624(11) 0.0164(3) Uani 1 1 d . . . C38 C 0.82479(14) 0.14636(13) 0.12672(11) 0.0179(3) Uani 1 1 d . . . C39 C 0.82847(14) 0.23606(14) 0.08818(11) 0.0204(3) Uani 1 1 d . . . C40 C 0.80700(15) 0.32235(13) 0.14087(12) 0.0230(4) Uani 1 1 d . . . C41 C 0.78168(15) 0.31703(13) 0.23005(12) 0.0219(3) Uani 1 1 d . . . C42 C 0.77963(14) 0.22568(13) 0.26585(11) 0.0190(3) Uani 1 1 d . . . C43 C 0.76694(14) 0.02449(12) 0.36017(11) 0.0171(3) Uani 1 1 d . . . C44 C 0.85926(14) 0.06904(12) 0.41650(11) 0.0183(3) Uani 1 1 d . . . C45 C 0.86781(15) 0.06773(13) 0.50965(12) 0.0223(3) Uani 1 1 d . . . C46 C 0.77923(16) 0.02061(13) 0.55145(11) 0.0225(3) Uani 1 1 d . . . C47 C 0.68511(15) -0.02394(13) 0.49972(12) 0.0206(3) Uani 1 1 d . . . C48 C 0.68143(14) -0.02237(13) 0.40649(11) 0.0191(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.01782(16) 0.01472(15) 0.01896(16) 0.00316(11) -0.00023(12) 0.00150(11) N1 0.0230(7) 0.0167(7) 0.0196(7) 0.0030(5) -0.0014(6) 0.0003(5) N2 0.0312(9) 0.0256(8) 0.0215(8) 0.0031(6) 0.0017(6) 0.0106(6) Si1 0.0273(3) 0.0156(2) 0.0237(3) 0.00251(17) -0.00569(19) 0.00040(18) Si2 0.0220(3) 0.0238(3) 0.0225(3) 0.00488(18) 0.00082(19) -0.00313(19) B1 0.0147(8) 0.0153(8) 0.0162(8) 0.0012(6) -0.0008(6) -0.0010(6) F1 0.0211(5) 0.0227(5) 0.0268(6) -0.0018(4) 0.0022(4) 0.0054(4) F2 0.0162(5) 0.0318(6) 0.0450(7) 0.0011(5) -0.0001(5) 0.0062(4) F3 0.0212(6) 0.0333(6) 0.0345(6) 0.0036(5) -0.0137(5) -0.0040(4) F4 0.0357(6) 0.0272(6) 0.0231(6) -0.0059(4) -0.0062(5) 0.0008(5) F5 0.0255(6) 0.0309(6) 0.0245(6) -0.0078(4) -0.0039(4) 0.0112(4) F6 0.0166(5) 0.0186(5) 0.0281(6) 0.0065(4) 0.0038(4) -0.0023(4) F7 0.0330(6) 0.0168(5) 0.0332(6) 0.0090(4) 0.0062(5) 0.0059(4) F8 0.0243(6) 0.0296(6) 0.0307(6) 0.0064(4) 0.0047(5) 0.0132(4) F9 0.0156(5) 0.0351(6) 0.0306(6) 0.0075(5) 0.0052(4) 0.0014(4) F10 0.0195(5) 0.0174(5) 0.0312(6) 0.0069(4) 0.0021(4) -0.0033(4) F11 0.0261(5) 0.0232(5) 0.0171(5) 0.0007(4) 0.0019(4) 0.0055(4) F12 0.0301(6) 0.0333(6) 0.0180(5) 0.0107(4) 0.0023(4) 0.0023(5) F13 0.0455(7) 0.0212(6) 0.0340(6) 0.0144(5) -0.0032(5) 0.0039(5) F14 0.0454(7) 0.0169(5) 0.0300(6) 0.0004(4) -0.0014(5) 0.0083(5) F15 0.0369(6) 0.0206(5) 0.0164(5) 0.0011(4) 0.0036(4) 0.0050(4) F16 0.0194(5) 0.0299(6) 0.0225(5) 0.0050(4) -0.0010(4) -0.0060(4) F17 0.0287(6) 0.0363(6) 0.0217(6) 0.0012(4) -0.0098(4) -0.0048(5) F18 0.0428(7) 0.0367(7) 0.0136(5) 0.0044(4) -0.0021(5) -0.0020(5) F19 0.0306(6) 0.0314(6) 0.0228(6) 0.0064(4) 0.0077(5) -0.0046(5) F20 0.0194(5) 0.0282(6) 0.0212(5) 0.0036(4) -0.0016(4) -0.0065(4) C1 0.0266(10) 0.0402(11) 0.0227(9) -0.0023(8) 0.0055(8) 0.0040(8) C2 0.0179(8) 0.0284(9) 0.0198(8) -0.0007(6) 0.0004(6) 0.0018(7) C3 0.0195(8) 0.0192(8) 0.0261(9) 0.0003(6) -0.0010(7) 0.0057(6) C4 0.0180(8) 0.0174(8) 0.0224(8) 0.0023(6) -0.0007(6) 0.0026(6) C5 0.0267(9) 0.0240(9) 0.0237(9) 0.0069(7) -0.0029(7) 0.0047(7) C6 0.0285(10) 0.0301(10) 0.0206(9) 0.0062(7) -0.0008(7) 0.0057(7) C7 0.0262(9) 0.0282(9) 0.0205(9) -0.0020(7) -0.0005(7) 0.0047(7) C8 0.0232(9) 0.0174(8) 0.0225(9) -0.0010(6) -0.0022(7) 0.0026(6) C9 0.0173(8) 0.0169(8) 0.0197(8) 0.0016(6) -0.0012(6) 0.0003(6) C10 0.0213(8) 0.0201(8) 0.0204(8) 0.0032(6) 0.0006(6) -0.0013(6) C11 0.0436(12) 0.0217(9) 0.0275(10) -0.0001(7) 0.0041(9) 0.0052(8) C12 0.0269(10) 0.0205(9) 0.0367(11) 0.0077(7) -0.0054(8) -0.0020(7) C13 0.0437(12) 0.0230(10) 0.0343(11) 0.0019(8) -0.0163(9) -0.0011(8) C14 0.0441(12) 0.0318(11) 0.0269(10) 0.0095(8) 0.0025(9) -0.0054(9) C15 0.0248(10) 0.0447(13) 0.0400(13) 0.0023(9) 0.0039(9) -0.0071(9) C16 0.0240(9) 0.0287(9) 0.0202(9) 0.0004(7) 0.0024(7) 0.0040(7) C17 0.0299(11) 0.0545(14) 0.0310(11) 0.0102(9) 0.0016(9) 0.0186(10) C18 0.0564(14) 0.0239(10) 0.0299(11) 0.0041(8) 0.0012(10) 0.0174(9) C19 0.0256(9) 0.0238(9) 0.0197(8) 0.0057(6) -0.0012(7) 0.0081(7) C20 0.0271(9) 0.0225(9) 0.0222(9) 0.0063(7) -0.0007(7) 0.0021(7) C21 0.0327(10) 0.0257(9) 0.0218(9) 0.0020(7) 0.0005(7) 0.0042(7) C22 0.0341(11) 0.0369(11) 0.0219(9) 0.0065(8) 0.0033(8) 0.0035(8) C23 0.0379(11) 0.0298(10) 0.0294(10) 0.0147(8) 0.0015(8) -0.0010(8) C24 0.0389(11) 0.0196(9) 0.0282(10) 0.0084(7) -0.0024(8) 0.0022(8) C25 0.0153(7) 0.0158(7) 0.0185(8) 0.0038(6) -0.0005(6) 0.0008(6) C26 0.0178(8) 0.0170(8) 0.0198(8) 0.0011(6) 0.0012(6) 0.0009(6) C27 0.0146(8) 0.0202(8) 0.0300(9) 0.0059(7) 0.0013(7) 0.0032(6) C28 0.0186(8) 0.0215(8) 0.0248(9) 0.0052(6) -0.0071(7) -0.0044(6) C29 0.0254(9) 0.0175(8) 0.0186(8) -0.0001(6) -0.0043(7) -0.0005(6) C30 0.0195(8) 0.0183(8) 0.0204(8) 0.0011(6) -0.0012(6) 0.0036(6) C31 0.0176(8) 0.0168(8) 0.0148(7) 0.0016(5) -0.0020(6) 0.0005(6) C32 0.0145(7) 0.0205(8) 0.0153(7) 0.0029(6) -0.0008(6) -0.0003(6) C33 0.0236(8) 0.0142(7) 0.0182(8) 0.0049(6) -0.0015(6) 0.0014(6) C34 0.0202(8) 0.0218(8) 0.0174(8) 0.0035(6) -0.0007(6) 0.0076(6) C35 0.0131(7) 0.0271(9) 0.0173(8) 0.0037(6) -0.0006(6) 0.0007(6) C36 0.0185(8) 0.0158(8) 0.0181(8) 0.0040(6) -0.0008(6) -0.0009(6) C37 0.0152(7) 0.0171(8) 0.0163(7) 0.0025(5) -0.0021(6) 0.0008(6) C38 0.0166(8) 0.0188(8) 0.0177(8) 0.0021(6) -0.0010(6) 0.0007(6) C39 0.0190(8) 0.0252(9) 0.0176(8) 0.0080(6) -0.0010(6) 0.0009(6) C40 0.0250(9) 0.0184(8) 0.0259(9) 0.0093(6) -0.0049(7) -0.0001(7) C41 0.0259(9) 0.0154(8) 0.0235(9) 0.0006(6) -0.0031(7) 0.0028(6) C42 0.0205(8) 0.0186(8) 0.0173(8) 0.0020(6) -0.0010(6) 0.0011(6) C43 0.0190(8) 0.0155(7) 0.0164(8) 0.0016(5) -0.0013(6) 0.0014(6) C44 0.0182(8) 0.0169(8) 0.0192(8) 0.0029(6) -0.0004(6) -0.0006(6) C45 0.0239(9) 0.0208(8) 0.0207(8) 0.0001(6) -0.0058(7) 0.0014(7) C46 0.0319(10) 0.0214(8) 0.0141(8) 0.0022(6) -0.0013(7) 0.0041(7) C47 0.0242(9) 0.0186(8) 0.0190(8) 0.0037(6) 0.0039(6) 0.0012(6) C48 0.0185(8) 0.0173(8) 0.0204(8) 0.0020(6) -0.0016(6) -0.0005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 N1 2.0049(15) . ? Sc1 N2 2.3173(16) . ? Sc1 C3 2.4229(19) . ? Sc1 C4 2.4404(18) . ? Sc1 C10 2.4845(18) . ? Sc1 C9 2.4855(18) . ? Sc1 C2 2.4942(19) . ? Sc1 C19 2.7944(17) . ? Sc1 Si2 2.8923(8) . ? Sc1 C16 2.614(2) . ? N1 Si2 1.7289(16) . ? N1 Si1 1.7453(16) . ? N2 C19 1.451(2) . ? N2 C18 1.488(3) . ? N2 C17 1.501(3) . ? Si1 C12 1.8623(19) . ? Si1 C11 1.867(2) . ? Si1 C13 1.874(2) . ? Si2 C14 1.862(2) . ? Si2 C15 1.864(2) . ? Si2 C16 1.919(2) . ? B1 C43 1.651(2) . ? B1 C31 1.654(3) . ? B1 C37 1.657(2) . ? B1 C25 1.659(2) . ? F1 C26 1.350(2) . ? F2 C27 1.335(2) . ? F3 C28 1.3367(19) . ? F4 C29 1.347(2) . ? F5 C30 1.350(2) . ? F6 C32 1.3578(18) . ? F7 C33 1.3537(19) . ? F8 C34 1.3424(19) . ? F9 C35 1.3419(18) . ? F10 C36 1.3566(19) . ? F11 C38 1.352(2) . ? F12 C39 1.3423(19) . ? F13 C40 1.3424(19) . ? F14 C41 1.346(2) . ? F15 C42 1.357(2) . ? F16 C44 1.3536(18) . ? F17 C45 1.344(2) . ? F18 C46 1.3475(19) . ? F19 C47 1.3460(19) . ? F20 C48 1.3469(19) . ? C1 C2 1.503(3) . ? C2 C10 1.409(3) . ? C2 C3 1.414(2) . ? C3 C4 1.428(2) . ? C4 C5 1.418(2) . ? C4 C9 1.441(2) . ? C5 C6 1.373(3) . ? C6 C7 1.416(3) . ? C7 C8 1.362(2) . ? C8 C9 1.422(2) . ? C9 C10 1.430(2) . ? C19 C20 1.397(3) . ? C19 C24 1.398(3) . ? C20 C21 1.387(3) . ? C21 C22 1.375(3) . ? C22 C23 1.393(3) . ? C23 C24 1.388(3) . ? C25 C30 1.390(2) . ? C25 C26 1.395(2) . ? C26 C27 1.387(2) . ? C27 C28 1.373(3) . ? C28 C29 1.379(3) . ? C29 C30 1.386(2) . ? C31 C36 1.387(2) . ? C31 C32 1.395(2) . ? C32 C33 1.376(2) . ? C33 C34 1.375(2) . ? C34 C35 1.377(2) . ? C35 C36 1.384(2) . ? C37 C38 1.389(2) . ? C37 C42 1.393(2) . ? C38 C39 1.385(2) . ? C39 C40 1.376(3) . ? C40 C41 1.377(3) . ? C41 C42 1.387(2) . ? C43 C48 1.386(2) . ? C43 C44 1.393(2) . ? C44 C45 1.384(2) . ? C45 C46 1.377(2) . ? C46 C47 1.375(3) . ? C47 C48 1.385(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sc1 N2 111.28(6) . . ? N1 Sc1 C3 99.34(6) . . ? N2 Sc1 C3 143.16(6) . . ? N1 Sc1 C4 108.62(6) . . ? N2 Sc1 C4 138.11(6) . . ? C3 Sc1 C4 34.14(6) . . ? N1 Sc1 C10 154.26(6) . . ? N2 Sc1 C10 90.14(6) . . ? C3 Sc1 C10 55.89(6) . . ? C4 Sc1 C10 55.96(6) . . ? N1 Sc1 C9 141.20(6) . . ? N2 Sc1 C9 104.17(6) . . ? C3 Sc1 C9 56.33(6) . . ? C4 Sc1 C9 34.00(5) . . ? C10 Sc1 C9 33.43(5) . . ? N1 Sc1 C2 122.19(6) . . ? N2 Sc1 C2 110.05(6) . . ? C3 Sc1 C2 33.37(6) . . ? C4 Sc1 C2 55.37(6) . . ? C10 Sc1 C2 32.88(6) . . ? C9 Sc1 C2 54.94(6) . . ? N1 Sc1 C19 110.05(6) . . ? N2 Sc1 C19 31.23(5) . . ? C3 Sc1 C19 119.05(6) . . ? C4 Sc1 C19 136.49(6) . . ? C10 Sc1 C19 80.67(6) . . ? C9 Sc1 C19 108.40(6) . . ? C2 Sc1 C19 86.99(6) . . ? N1 Sc1 Si2 35.89(4) . . ? N2 Sc1 Si2 104.22(5) . . ? C3 Sc1 Si2 112.62(5) . . ? C4 Sc1 Si2 100.45(5) . . ? C10 Sc1 Si2 153.56(4) . . ? C9 Sc1 Si2 120.27(4) . . ? C2 Sc1 Si2 145.47(5) . . ? C19 Sc1 Si2 122.62(4) . . ? Si2 N1 Si1 123.18(8) . . ? Si2 N1 Sc1 101.29(7) . . ? Si1 N1 Sc1 135.33(9) . . ? C19 N2 C18 114.15(15) . . ? C19 N2 C17 110.13(15) . . ? C18 N2 C17 108.05(16) . . ? C19 N2 Sc1 92.85(10) . . ? C18 N2 Sc1 113.99(12) . . ? C17 N2 Sc1 117.16(12) . . ? N1 Si1 C12 111.93(9) . . ? N1 Si1 C11 110.43(8) . . ? C12 Si1 C11 108.91(10) . . ? N1 Si1 C13 109.64(9) . . ? C12 Si1 C13 107.60(9) . . ? C11 Si1 C13 108.23(11) . . ? N1 Si2 C14 114.81(9) . . ? N1 Si2 C15 114.29(9) . . ? C14 Si2 C15 109.47(10) . . ? N1 Si2 C16 104.59(8) . . ? C14 Si2 C16 106.18(9) . . ? C15 Si2 C16 106.74(10) . . ? N1 Si2 Sc1 42.83(5) . . ? C14 Si2 Sc1 121.22(7) . . ? C15 Si2 Sc1 129.29(8) . . ? C16 Si2 Sc1 61.99(6) . . ? C43 B1 C31 101.18(12) . . ? C43 B1 C37 112.91(13) . . ? C31 B1 C37 115.66(13) . . ? C43 B1 C25 116.02(13) . . ? C31 B1 C25 111.26(13) . . ? C37 B1 C25 100.50(12) . . ? C10 C2 C3 109.16(16) . . ? C10 C2 C1 125.28(17) . . ? C3 C2 C1 125.49(18) . . ? C10 C2 Sc1 73.18(10) . . ? C3 C2 Sc1 70.54(10) . . ? C1 C2 Sc1 124.98(13) . . ? C2 C3 C4 107.64(15) . . ? C2 C3 Sc1 76.08(10) . . ? C4 C3 Sc1 73.60(10) . . ? C5 C4 C3 132.16(16) . . ? C5 C4 C9 120.05(16) . . ? C3 C4 C9 107.79(14) . . ? C5 C4 Sc1 118.98(12) . . ? C3 C4 Sc1 72.26(10) . . ? C9 C4 Sc1 74.71(9) . . ? C6 C5 C4 118.44(17) . . ? C5 C6 C7 121.21(16) . . ? C8 C7 C6 122.27(17) . . ? C7 C8 C9 118.32(16) . . ? C8 C9 C10 133.15(16) . . ? C8 C9 C4 119.64(15) . . ? C10 C9 C4 107.22(15) . . ? C8 C9 Sc1 120.53(12) . . ? C10 C9 Sc1 73.25(10) . . ? C4 C9 Sc1 71.28(9) . . ? C2 C10 C9 108.02(15) . . ? C2 C10 Sc1 73.94(10) . . ? C9 C10 Sc1 73.32(9) . . ? C20 C19 C24 119.10(17) . . ? C20 C19 N2 116.95(16) . . ? C24 C19 N2 123.93(17) . . ? C20 C19 Sc1 81.77(10) . . ? C24 C19 Sc1 131.68(13) . . ? N2 C19 Sc1 55.92(8) . . ? C21 C20 C19 120.52(16) . . ? C22 C21 C20 120.38(18) . . ? C21 C22 C23 119.56(19) . . ? C24 C23 C22 120.76(17) . . ? C23 C24 C19 119.64(18) . . ? C30 C25 C26 112.89(15) . . ? C30 C25 B1 125.95(15) . . ? C26 C25 B1 120.35(15) . . ? F1 C26 C27 116.22(15) . . ? F1 C26 C25 119.49(15) . . ? C27 C26 C25 124.28(16) . . ? F2 C27 C28 119.39(16) . . ? F2 C27 C26 120.73(17) . . ? C28 C27 C26 119.88(16) . . ? F3 C28 C27 120.86(17) . . ? F3 C28 C29 120.46(17) . . ? C27 C28 C29 118.68(16) . . ? F4 C29 C28 119.89(15) . . ? F4 C29 C30 120.61(16) . . ? C28 C29 C30 119.49(16) . . ? F5 C30 C29 113.75(15) . . ? F5 C30 C25 121.49(15) . . ? C29 C30 C25 124.74(16) . . ? C36 C31 C32 112.84(15) . . ? C36 C31 B1 128.22(14) . . ? C32 C31 B1 118.86(14) . . ? F6 C32 C33 116.37(14) . . ? F6 C32 C31 119.08(15) . . ? C33 C32 C31 124.51(15) . . ? F7 C33 C34 119.20(15) . . ? F7 C33 C32 120.90(15) . . ? C34 C33 C32 119.88(15) . . ? F8 C34 C33 120.10(15) . . ? F8 C34 C35 121.39(15) . . ? C33 C34 C35 118.50(16) . . ? F9 C35 C34 119.70(16) . . ? F9 C35 C36 120.63(15) . . ? C34 C35 C36 119.67(15) . . ? F10 C36 C35 114.98(14) . . ? F10 C36 C31 120.50(15) . . ? C35 C36 C31 124.51(15) . . ? C38 C37 C42 113.37(14) . . ? C38 C37 B1 120.18(15) . . ? C42 C37 B1 125.31(14) . . ? F11 C38 C39 115.96(15) . . ? F11 C38 C37 119.11(14) . . ? C39 C38 C37 124.90(16) . . ? F12 C39 C40 119.80(15) . . ? F12 C39 C38 121.27(16) . . ? C40 C39 C38 118.93(16) . . ? F13 C40 C39 120.83(16) . . ? F13 C40 C41 119.99(17) . . ? C39 C40 C41 119.18(15) . . ? F14 C41 C40 119.72(15) . . ? F14 C41 C42 120.42(16) . . ? C40 C41 C42 119.86(17) . . ? F15 C42 C41 114.79(15) . . ? F15 C42 C37 121.44(14) . . ? C41 C42 C37 123.76(16) . . ? C48 C43 C44 113.40(15) . . ? C48 C43 B1 127.62(14) . . ? C44 C43 B1 118.57(14) . . ? F16 C44 C45 115.70(15) . . ? F16 C44 C43 119.60(14) . . ? C45 C44 C43 124.70(15) . . ? F17 C45 C46 120.22(16) . . ? F17 C45 C44 120.93(16) . . ? C46 C45 C44 118.86(16) . . ? F18 C46 C47 120.38(16) . . ? F18 C46 C45 120.33(16) . . ? C47 C46 C45 119.28(16) . . ? F19 C47 C46 119.27(15) . . ? F19 C47 C48 121.02(16) . . ? C46 C47 C48 119.70(16) . . ? F20 C48 C47 114.99(14) . . ? F20 C48 C43 120.95(15) . . ? C47 C48 C43 124.05(16) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.513 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.074 #===END #Attachement 'compound6.cif' data_compound6 _database_code_depnum_ccdc_archive 'CCDC 670549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (IndMe)(THF)2ScNTMS _chemical_melting_point ? _chemical_formula_moiety 'C24 H43 N O2 Sc Si2, C24 B F20' _chemical_formula_sum 'C48 H43 B F20 N O2 Sc Si2' _chemical_formula_weight 1157.78 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' F F 0.0171 0.0103 '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' Sc Sc 0.2519 0.3716 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.206(3) _cell_length_b 19.410(3) _cell_length_c 16.909(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.299(2) _cell_angle_gamma 90.00 _cell_volume 4989.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 15687 _cell_measurement_theta_min 3.0966 _cell_measurement_theta_max 27.5229 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 0.311 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.8889 _exptl_absorpt_correction_T_max 0.9235 _exptl_absorpt_process_details NUMABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku AFC-8 with Saturn70 CCD detector' _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 25331 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.52 _reflns_number_total 11383 _reflns_number_gt 8284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear SM (Rigaku/MSC, 2005)' _computing_cell_refinement 'CrystalClear SM' _computing_data_reduction 'CrystalClear SM' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL97 _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^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11383 _refine_ls_number_parameters 684 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.010 _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 0.21638(2) 0.074369(17) 0.23885(2) 0.01493(9) Uani 1 1 d . . . N1 N 0.26585(10) 0.09435(8) 0.13131(10) 0.0178(3) Uani 1 1 d . . . Si1 Si 0.22283(4) 0.07035(3) 0.03944(4) 0.02349(14) Uani 1 1 d . . . Si2 Si 0.35730(3) 0.14869(3) 0.13650(3) 0.01803(12) Uani 1 1 d . . . O1 O 0.14421(8) -0.02138(6) 0.22644(9) 0.0212(3) Uani 1 1 d . . . O2 O 0.31401(8) 0.00852(6) 0.29632(9) 0.0205(3) Uani 1 1 d . . . B1 B 0.73698(13) 0.12088(10) 0.29287(13) 0.0140(4) Uani 1 1 d . . . F1 F 0.71119(7) 0.26659(5) 0.31171(7) 0.0211(3) Uani 1 1 d . . . F2 F 0.58013(8) 0.33200(6) 0.38117(8) 0.0339(3) Uani 1 1 d . . . F3 F 0.44734(8) 0.25887(7) 0.44834(9) 0.0392(3) Uani 1 1 d . . . F4 F 0.58279(7) 0.05237(6) 0.38048(8) 0.0256(3) Uani 1 1 d . . . F5 F 0.45447(8) 0.11909(7) 0.44957(8) 0.0347(3) Uani 1 1 d . . . F6 F 0.87902(7) 0.08771(5) 0.19074(7) 0.0210(3) Uani 1 1 d . . . F7 F 0.90379(7) 0.12802(6) 0.04249(7) 0.0283(3) Uani 1 1 d . . . F8 F 0.78410(8) 0.21217(6) -0.03224(7) 0.0303(3) Uani 1 1 d . . . F9 F 0.61181(7) 0.21482(6) 0.19129(7) 0.0225(3) Uani 1 1 d . . . F10 F 0.64095(8) 0.25601(6) 0.04732(8) 0.0302(3) Uani 1 1 d . . . F11 F 0.75656(7) 0.06978(6) 0.45164(7) 0.0238(3) Uani 1 1 d . . . F12 F 0.87420(8) 0.10761(6) 0.56348(8) 0.0322(3) Uani 1 1 d . . . F13 F 1.00369(8) 0.19908(6) 0.52972(8) 0.0310(3) Uani 1 1 d . . . F14 F 1.01370(7) 0.25133(5) 0.38099(8) 0.0243(3) Uani 1 1 d . . . F15 F 0.89809(7) 0.21548(5) 0.26899(7) 0.0195(2) Uani 1 1 d . . . F16 F 0.56001(8) -0.06806(6) 0.16889(8) 0.0293(3) Uani 1 1 d . . . F17 F 0.58824(7) 0.06260(5) 0.21064(7) 0.0220(3) Uani 1 1 d . . . F18 F 0.67755(8) -0.16787(5) 0.21174(9) 0.0328(3) Uani 1 1 d . . . F19 F 0.82885(8) -0.13202(6) 0.29238(8) 0.0334(3) Uani 1 1 d . . . F20 F 0.86072(7) -0.00207(5) 0.33097(7) 0.0232(3) Uani 1 1 d . . . C1 C 0.08480(14) 0.21015(10) 0.16329(13) 0.0258(5) Uani 1 1 d . . . H1A H 0.0551 0.2534 0.1763 0.039 Uiso 1 1 calc R . . H1B H 0.0438 0.1800 0.1341 0.039 Uiso 1 1 calc R . . H1C H 0.1357 0.2200 0.1306 0.039 Uiso 1 1 calc R . . C2 C 0.11516(12) 0.17493(9) 0.23826(12) 0.0186(4) Uani 1 1 d . . . C3 C 0.18987(12) 0.19200(9) 0.28475(13) 0.0190(4) Uani 1 1 d . . . H3 H 0.2339 0.2244 0.2712 0.023 Uiso 1 1 calc R . . C4 C 0.18822(12) 0.15232(9) 0.35594(13) 0.0186(4) Uani 1 1 d . . . C5 C 0.24028(14) 0.15363(10) 0.42644(13) 0.0253(5) Uani 1 1 d . . . H5 H 0.2913 0.1817 0.4303 0.030 Uiso 1 1 calc R . . C6 C 0.21592(15) 0.11391(11) 0.48863(14) 0.0303(5) Uani 1 1 d . . . H6 H 0.2496 0.1156 0.5366 0.036 Uiso 1 1 calc R . . C7 C 0.14178(15) 0.07022(11) 0.48355(14) 0.0286(5) Uani 1 1 d . . . H7 H 0.1262 0.0436 0.5282 0.034 Uiso 1 1 calc R . . C8 C 0.09195(13) 0.06563(10) 0.41527(13) 0.0231(4) Uani 1 1 d . . . H8 H 0.0434 0.0349 0.4120 0.028 Uiso 1 1 calc R . . C9 C 0.11339(12) 0.10702(9) 0.34995(12) 0.0177(4) Uani 1 1 d . . . C10 C 0.07144(12) 0.11978(9) 0.27499(12) 0.0178(4) Uani 1 1 d . . . H10 H 0.0224 0.0953 0.2535 0.021 Uiso 1 1 calc R . . C11 C 0.10558(14) 0.04185(11) 0.04687(14) 0.0309(5) Uani 1 1 d . . . H11A H 0.1034 -0.0021 0.0752 0.046 Uiso 1 1 calc R . . H11B H 0.0798 0.0361 -0.0064 0.046 Uiso 1 1 calc R . . H11C H 0.0723 0.0766 0.0756 0.046 Uiso 1 1 calc R . . C12 C 0.28718(16) -0.00169(12) -0.00494(15) 0.0376(6) Uani 1 1 d . . . H12A H 0.3479 0.0134 -0.0128 0.056 Uiso 1 1 calc R . . H12B H 0.2602 -0.0147 -0.0560 0.056 Uiso 1 1 calc R . . H12C H 0.2871 -0.0415 0.0308 0.056 Uiso 1 1 calc R . . C13 C 0.22168(17) 0.14153(13) -0.03519(14) 0.0387(6) Uani 1 1 d . . . H13A H 0.1884 0.1807 -0.0148 0.058 Uiso 1 1 calc R . . H13B H 0.1938 0.1252 -0.0846 0.058 Uiso 1 1 calc R . . H13C H 0.2822 0.1559 -0.0452 0.058 Uiso 1 1 calc R . . C14 C 0.44887(13) 0.11505(11) 0.07560(14) 0.0261(5) Uani 1 1 d . . . H14A H 0.4645 0.0684 0.0933 0.039 Uiso 1 1 calc R . . H14B H 0.5002 0.1453 0.0818 0.039 Uiso 1 1 calc R . . H14C H 0.4300 0.1138 0.0198 0.039 Uiso 1 1 calc R . . C15 C 0.33282(14) 0.23980(10) 0.10685(14) 0.0261(5) Uani 1 1 d . . . H15A H 0.3097 0.2407 0.0523 0.039 Uiso 1 1 calc R . . H15B H 0.3869 0.2672 0.1105 0.039 Uiso 1 1 calc R . . H15C H 0.2891 0.2592 0.1422 0.039 Uiso 1 1 calc R . . C16 C 0.39999(13) 0.15577(10) 0.24217(13) 0.0221(4) Uani 1 1 d . . . H16A H 0.3631 0.1279 0.2766 0.033 Uiso 1 1 calc R . . H16B H 0.3982 0.2040 0.2591 0.033 Uiso 1 1 calc R . . H16C H 0.4607 0.1390 0.2455 0.033 Uiso 1 1 calc R . . C17 C 0.05272(13) -0.04156(10) 0.24373(15) 0.0275(5) Uani 1 1 d . . . H17A H 0.0105 -0.0181 0.2074 0.033 Uiso 1 1 calc R . . H17B H 0.0382 -0.0297 0.2989 0.033 Uiso 1 1 calc R . . C18 C 0.04978(15) -0.11889(10) 0.23141(15) 0.0301(5) Uani 1 1 d . . . H18A H -0.0098 -0.1343 0.2144 0.036 Uiso 1 1 calc R . . H18B H 0.0680 -0.1439 0.2801 0.036 Uiso 1 1 calc R . . C19 C 0.11570(14) -0.12913(10) 0.16617(14) 0.0260(5) Uani 1 1 d . . . H19A H 0.1365 -0.1774 0.1641 0.031 Uiso 1 1 calc R . . H19B H 0.0904 -0.1160 0.1139 0.031 Uiso 1 1 calc R . . C20 C 0.18877(14) -0.08081(9) 0.19176(15) 0.0261(5) Uani 1 1 d . . . H20A H 0.2284 -0.1032 0.2313 0.031 Uiso 1 1 calc R . . H20B H 0.2237 -0.0665 0.1459 0.031 Uiso 1 1 calc R . . C21 C 0.39380(13) -0.02140(11) 0.26195(15) 0.0287(5) Uani 1 1 d . . . H21A H 0.4423 0.0126 0.2624 0.034 Uiso 1 1 calc R . . H21B H 0.3820 -0.0365 0.2068 0.034 Uiso 1 1 calc R . . C22 C 0.41691(17) -0.08210(12) 0.31394(16) 0.0396(6) Uani 1 1 d . . . H22A H 0.3902 -0.1249 0.2926 0.048 Uiso 1 1 calc R . . H22B H 0.4815 -0.0883 0.3183 0.048 Uiso 1 1 calc R . . C23 C 0.3801(2) -0.06478(17) 0.39172(19) 0.0630(9) Uani 1 1 d . . . H23A H 0.3626 -0.1072 0.4199 0.076 Uiso 1 1 calc R . . H23B H 0.4242 -0.0399 0.4249 0.076 Uiso 1 1 calc R . . C24 C 0.30317(15) -0.02088(12) 0.37539(14) 0.0315(5) Uani 1 1 d . . . H24A H 0.2485 -0.0485 0.3770 0.038 Uiso 1 1 calc R . . H24B H 0.2998 0.0163 0.4153 0.038 Uiso 1 1 calc R . . C25 C 0.65304(11) 0.15594(9) 0.33893(12) 0.0162(4) Uani 1 1 d . . . C26 C 0.64772(12) 0.22716(10) 0.34474(12) 0.0179(4) Uani 1 1 d . . . C27 C 0.58067(13) 0.26263(10) 0.37944(13) 0.0219(4) Uani 1 1 d . . . C28 C 0.51426(13) 0.22603(11) 0.41405(13) 0.0252(5) Uani 1 1 d . . . C29 C 0.51801(12) 0.15547(11) 0.41436(13) 0.0240(5) Uani 1 1 d . . . C30 C 0.58627(12) 0.12206(10) 0.37760(12) 0.0189(4) Uani 1 1 d . . . C31 C 0.74726(12) 0.15158(9) 0.20249(12) 0.0150(4) Uani 1 1 d . . . C32 C 0.81835(12) 0.13092(9) 0.15775(12) 0.0165(4) Uani 1 1 d . . . C33 C 0.83296(12) 0.15053(10) 0.08128(12) 0.0189(4) Uani 1 1 d . . . C34 C 0.77326(13) 0.19308(10) 0.04337(12) 0.0207(4) Uani 1 1 d . . . C35 C 0.70045(13) 0.21449(10) 0.08335(13) 0.0205(4) Uani 1 1 d . . . C36 C 0.68806(12) 0.19280(9) 0.16003(12) 0.0177(4) Uani 1 1 d . . . C37 C 0.82081(12) 0.13952(9) 0.35382(12) 0.0157(4) Uani 1 1 d . . . C38 C 0.82010(12) 0.11482(9) 0.43060(12) 0.0183(4) Uani 1 1 d . . . C39 C 0.87969(13) 0.13335(10) 0.48968(12) 0.0213(4) Uani 1 1 d . . . C40 C 0.94551(13) 0.17977(10) 0.47275(13) 0.0209(4) Uani 1 1 d . . . C41 C 0.94977(12) 0.20571(9) 0.39816(13) 0.0186(4) Uani 1 1 d . . . C42 C 0.88864(12) 0.18584(9) 0.34059(12) 0.0162(4) Uani 1 1 d . . . C43 C 0.72409(12) 0.03769(9) 0.27630(12) 0.0161(4) Uani 1 1 d . . . C44 C 0.65005(12) 0.01569(9) 0.23330(12) 0.0183(4) Uani 1 1 d . . . C45 C 0.63333(13) -0.05151(10) 0.21085(13) 0.0220(4) Uani 1 1 d . . . C46 C 0.69332(13) -0.10190(9) 0.23208(13) 0.0232(5) Uani 1 1 d . . . C47 C 0.76853(14) -0.08345(10) 0.27270(13) 0.0238(5) Uani 1 1 d . . . C48 C 0.78281(12) -0.01548(9) 0.29337(12) 0.0190(4) 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 0.01478(17) 0.01523(16) 0.0148(2) 0.00021(14) 0.00040(14) 0.00073(13) N1 0.0188(8) 0.0186(7) 0.0159(9) 0.0003(7) -0.0003(7) -0.0021(6) Si1 0.0263(3) 0.0284(3) 0.0158(3) -0.0028(2) -0.0009(2) -0.0069(2) Si2 0.0180(3) 0.0200(3) 0.0161(3) 0.0014(2) 0.0003(2) -0.0029(2) O1 0.0173(7) 0.0169(6) 0.0296(9) -0.0044(6) 0.0049(6) -0.0004(5) O2 0.0171(6) 0.0237(7) 0.0209(8) 0.0059(6) 0.0030(6) 0.0030(5) B1 0.0121(9) 0.0169(9) 0.0130(11) 0.0013(8) -0.0011(8) 0.0028(8) F1 0.0231(6) 0.0188(5) 0.0213(7) -0.0001(5) 0.0013(5) 0.0000(4) F2 0.0380(7) 0.0252(6) 0.0384(9) -0.0082(6) 0.0025(6) 0.0103(5) F3 0.0277(7) 0.0527(8) 0.0375(9) -0.0162(7) 0.0103(6) 0.0135(6) F4 0.0248(6) 0.0246(6) 0.0277(7) 0.0026(5) 0.0062(5) -0.0040(5) F5 0.0216(6) 0.0503(8) 0.0328(8) -0.0034(7) 0.0111(6) -0.0072(6) F6 0.0164(5) 0.0267(6) 0.0198(7) 0.0000(5) -0.0011(5) 0.0064(4) F7 0.0225(6) 0.0443(7) 0.0184(7) -0.0032(6) 0.0063(5) 0.0031(5) F8 0.0364(7) 0.0410(7) 0.0135(7) 0.0069(6) 0.0037(5) -0.0008(6) F9 0.0185(6) 0.0317(6) 0.0173(6) 0.0010(5) -0.0011(5) 0.0086(5) F10 0.0352(7) 0.0354(7) 0.0196(7) 0.0081(6) -0.0062(6) 0.0125(5) F11 0.0233(6) 0.0300(6) 0.0179(7) 0.0070(5) -0.0011(5) -0.0037(5) F12 0.0416(7) 0.0407(7) 0.0140(7) 0.0058(6) -0.0063(6) -0.0041(6) F13 0.0331(7) 0.0355(7) 0.0236(7) -0.0072(6) -0.0148(6) -0.0023(5) F14 0.0202(6) 0.0236(6) 0.0288(7) -0.0034(5) -0.0026(5) -0.0047(5) F15 0.0200(5) 0.0218(5) 0.0167(6) 0.0017(5) 0.0007(5) -0.0025(4) F16 0.0246(6) 0.0288(6) 0.0344(8) -0.0089(6) -0.0042(6) -0.0070(5) F17 0.0155(5) 0.0225(5) 0.0276(7) -0.0020(5) -0.0056(5) 0.0029(4) F18 0.0452(8) 0.0158(5) 0.0375(8) -0.0037(6) 0.0038(6) -0.0017(5) F19 0.0371(7) 0.0231(6) 0.0399(9) 0.0042(6) -0.0002(6) 0.0147(5) F20 0.0195(6) 0.0262(6) 0.0237(7) 0.0020(5) -0.0059(5) 0.0069(5) C1 0.0294(11) 0.0251(10) 0.0227(12) 0.0043(9) -0.0030(9) 0.0068(9) C2 0.0210(10) 0.0168(8) 0.0178(11) -0.0006(8) -0.0001(8) 0.0065(7) C3 0.0189(9) 0.0168(9) 0.0213(11) -0.0011(8) 0.0008(8) -0.0017(7) C4 0.0185(9) 0.0177(9) 0.0197(11) -0.0040(8) -0.0011(8) 0.0041(7) C5 0.0257(11) 0.0278(10) 0.0223(12) -0.0065(9) -0.0045(9) 0.0031(9) C6 0.0355(12) 0.0377(12) 0.0173(12) -0.0029(10) -0.0055(10) 0.0101(10) C7 0.0373(12) 0.0305(11) 0.0182(12) 0.0046(9) 0.0070(10) 0.0109(10) C8 0.0258(10) 0.0204(9) 0.0236(12) -0.0001(9) 0.0078(9) 0.0047(8) C9 0.0169(9) 0.0163(8) 0.0199(11) -0.0017(8) 0.0025(8) 0.0028(7) C10 0.0155(9) 0.0182(9) 0.0195(11) -0.0034(8) -0.0002(8) 0.0027(7) C11 0.0291(12) 0.0360(12) 0.0273(13) -0.0004(10) -0.0066(10) -0.0057(10) C12 0.0406(13) 0.0427(13) 0.0297(14) -0.0159(11) 0.0084(11) -0.0104(11) C13 0.0483(15) 0.0492(14) 0.0183(13) 0.0062(11) -0.0074(11) -0.0154(12) C14 0.0222(10) 0.0326(11) 0.0237(12) 0.0010(9) 0.0008(9) -0.0026(9) C15 0.0338(12) 0.0226(10) 0.0221(12) 0.0032(9) 0.0008(10) -0.0052(9) C16 0.0207(10) 0.0246(10) 0.0207(11) -0.0001(9) -0.0026(9) -0.0028(8) C17 0.0187(10) 0.0256(10) 0.0386(14) -0.0096(10) 0.0109(9) -0.0068(8) C18 0.0328(12) 0.0239(10) 0.0340(14) -0.0052(10) 0.0113(10) -0.0099(9) C19 0.0310(11) 0.0190(9) 0.0282(13) -0.0046(9) 0.0063(10) -0.0024(8) C20 0.0257(11) 0.0177(9) 0.0353(14) -0.0057(9) 0.0077(10) 0.0008(8) C21 0.0207(10) 0.0337(11) 0.0321(14) 0.0069(10) 0.0081(9) 0.0088(9) C22 0.0386(13) 0.0408(13) 0.0399(16) 0.0134(12) 0.0104(12) 0.0184(11) C23 0.072(2) 0.074(2) 0.0434(19) 0.0280(16) 0.0184(16) 0.0423(17) C24 0.0364(12) 0.0348(12) 0.0236(13) 0.0110(10) 0.0072(10) 0.0089(10) C25 0.0125(8) 0.0226(9) 0.0134(10) -0.0007(8) -0.0040(7) 0.0009(7) C26 0.0157(9) 0.0259(10) 0.0119(10) -0.0008(8) -0.0027(8) 0.0004(8) C27 0.0219(10) 0.0249(10) 0.0186(11) -0.0065(9) -0.0047(9) 0.0072(8) C28 0.0187(10) 0.0395(12) 0.0173(11) -0.0105(9) 0.0016(8) 0.0086(9) C29 0.0169(9) 0.0397(12) 0.0156(11) -0.0035(9) 0.0008(8) -0.0021(9) C30 0.0180(9) 0.0238(9) 0.0147(10) -0.0006(8) -0.0031(8) 0.0001(8) C31 0.0146(9) 0.0169(8) 0.0134(10) -0.0019(8) -0.0021(7) -0.0021(7) C32 0.0154(9) 0.0181(8) 0.0158(10) -0.0011(8) -0.0053(8) 0.0006(7) C33 0.0172(9) 0.0236(9) 0.0161(10) -0.0031(8) 0.0031(8) -0.0027(8) C34 0.0264(10) 0.0255(10) 0.0103(10) 0.0026(8) -0.0005(8) -0.0054(8) C35 0.0237(10) 0.0217(9) 0.0157(11) 0.0020(8) -0.0065(8) 0.0025(8) C36 0.0163(9) 0.0202(9) 0.0165(10) -0.0022(8) -0.0010(8) 0.0008(7) C37 0.0143(9) 0.0169(8) 0.0157(10) -0.0020(8) -0.0011(8) 0.0055(7) C38 0.0158(9) 0.0207(9) 0.0185(11) 0.0008(8) -0.0001(8) 0.0020(7) C39 0.0277(10) 0.0261(10) 0.0099(10) 0.0008(8) -0.0029(8) 0.0050(8) C40 0.0212(10) 0.0244(9) 0.0168(11) -0.0069(8) -0.0080(8) 0.0038(8) C41 0.0158(9) 0.0162(8) 0.0238(11) -0.0041(8) 0.0010(8) 0.0012(7) C42 0.0197(9) 0.0160(8) 0.0128(10) -0.0004(7) 0.0012(8) 0.0057(7) C43 0.0173(9) 0.0184(9) 0.0128(10) 0.0008(8) 0.0033(8) 0.0009(7) C44 0.0177(9) 0.0185(9) 0.0187(11) 0.0014(8) 0.0013(8) 0.0034(7) C45 0.0202(10) 0.0246(10) 0.0214(11) -0.0022(9) 0.0019(9) -0.0048(8) C46 0.0304(11) 0.0147(9) 0.0249(12) -0.0023(8) 0.0067(9) -0.0017(8) C47 0.0288(11) 0.0201(9) 0.0226(12) 0.0051(9) 0.0048(9) 0.0087(8) C48 0.0185(9) 0.0233(9) 0.0150(10) 0.0032(8) 0.0000(8) 0.0011(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 N1 2.0211(18) . ? Sc1 O1 2.1661(13) . ? Sc1 O2 2.1718(13) . ? Sc1 C3 2.4480(19) . ? Sc1 C10 2.4634(19) . ? Sc1 C2 2.4855(18) . ? Sc1 C4 2.536(2) . ? Sc1 C9 2.553(2) . ? Sc1 Si2 3.1362(7) . ? N1 Si1 1.7354(17) . ? N1 Si2 1.7460(16) . ? Si1 C12 1.873(2) . ? Si1 C11 1.874(2) . ? Si1 C13 1.871(2) . ? Si2 C14 1.868(2) . ? Si2 C15 1.873(2) . ? Si2 C16 1.892(2) . ? O1 C20 1.467(2) . ? O1 C17 1.481(2) . ? O2 C24 1.466(3) . ? O2 C21 1.476(2) . ? B1 C43 1.650(3) . ? B1 C31 1.651(3) . ? B1 C25 1.656(3) . ? B1 C37 1.661(3) . ? F1 C26 1.362(2) . ? F2 C27 1.347(2) . ? F3 C28 1.343(2) . ? F4 C30 1.355(2) . ? F5 C29 1.346(2) . ? F6 C32 1.357(2) . ? F7 C33 1.347(2) . ? F8 C34 1.345(2) . ? F9 C36 1.354(2) . ? F10 C35 1.347(2) . ? F11 C38 1.356(2) . ? F12 C39 1.349(2) . ? F13 C40 1.346(2) . ? F14 C41 1.351(2) . ? F15 C42 1.351(2) . ? F16 C45 1.347(2) . ? F17 C44 1.358(2) . ? F18 C46 1.346(2) . ? F19 C47 1.352(2) . ? F20 C48 1.357(2) . ? C1 C2 1.504(3) . ? C2 C3 1.406(3) . ? C2 C10 1.411(3) . ? C3 C4 1.430(3) . ? C4 C5 1.416(3) . ? C4 C9 1.440(3) . ? C5 C6 1.362(3) . ? C6 C7 1.412(3) . ? C7 C8 1.369(3) . ? C8 C9 1.410(3) . ? C9 C10 1.428(3) . ? C17 C18 1.516(3) . ? C18 C19 1.520(3) . ? C19 C20 1.510(3) . ? C21 C22 1.507(3) . ? C22 C23 1.479(4) . ? C23 C24 1.469(3) . ? C25 C30 1.386(3) . ? C25 C26 1.388(3) . ? C26 C27 1.373(3) . ? C27 C28 1.376(3) . ? C28 C29 1.371(3) . ? C29 C30 1.383(3) . ? C31 C36 1.392(3) . ? C31 C32 1.392(3) . ? C32 C33 1.371(3) . ? C33 C34 1.375(3) . ? C34 C35 1.375(3) . ? C35 C36 1.380(3) . ? C37 C38 1.384(3) . ? C37 C42 1.390(3) . ? C38 C39 1.381(3) . ? C39 C40 1.381(3) . ? C40 C41 1.361(3) . ? C41 C42 1.385(3) . ? C43 C48 1.391(3) . ? C43 C44 1.393(3) . ? C44 C45 1.380(3) . ? C45 C46 1.379(3) . ? C46 C47 1.368(3) . ? C47 C48 1.381(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 N1 Sc1 O1 105.99(6) . . ? N1 Sc1 O2 104.54(6) . . ? O1 Sc1 O2 83.00(5) . . ? N1 Sc1 C3 100.00(7) . . ? O1 Sc1 C3 138.10(6) . . ? O2 Sc1 C3 121.52(6) . . ? N1 Sc1 C10 120.52(7) . . ? O1 Sc1 C10 82.93(6) . . ? O2 Sc1 C10 134.90(6) . . ? C3 Sc1 C10 55.46(6) . . ? N1 Sc1 C2 95.10(7) . . ? O1 Sc1 C2 111.17(6) . . ? O2 Sc1 C2 151.75(6) . . ? C3 Sc1 C2 33.11(6) . . ? C10 Sc1 C2 33.14(6) . . ? N1 Sc1 C4 131.36(6) . . ? O1 Sc1 C4 119.56(6) . . ? O2 Sc1 C4 97.33(6) . . ? C3 Sc1 C4 33.28(6) . . ? C10 Sc1 C4 54.90(6) . . ? C2 Sc1 C4 54.49(6) . . ? N1 Sc1 C9 149.49(6) . . ? O1 Sc1 C9 88.08(6) . . ? O2 Sc1 C9 103.96(6) . . ? C3 Sc1 C9 55.03(6) . . ? C10 Sc1 C9 33.01(6) . . ? C2 Sc1 C9 54.40(6) . . ? C4 Sc1 C9 32.87(6) . . ? N1 Sc1 Si2 30.95(4) . . ? O1 Sc1 Si2 133.80(4) . . ? O2 Sc1 Si2 92.81(4) . . ? C3 Sc1 Si2 82.27(5) . . ? C10 Sc1 Si2 126.77(5) . . ? C2 Sc1 Si2 93.87(5) . . ? C4 Sc1 Si2 106.62(5) . . ? C9 Sc1 Si2 136.90(4) . . ? Si1 N1 Si2 119.39(10) . . ? Si1 N1 Sc1 127.84(9) . . ? Si2 N1 Sc1 112.51(9) . . ? N1 Si1 C12 111.67(10) . . ? N1 Si1 C11 111.05(10) . . ? C12 Si1 C11 108.24(10) . . ? N1 Si1 C13 113.78(9) . . ? C12 Si1 C13 106.14(12) . . ? C11 Si1 C13 105.60(11) . . ? N1 Si2 C14 111.34(9) . . ? N1 Si2 C15 113.80(9) . . ? C14 Si2 C15 109.18(10) . . ? N1 Si2 C16 110.32(9) . . ? C14 Si2 C16 107.57(9) . . ? C15 Si2 C16 104.24(9) . . ? N1 Si2 Sc1 36.54(6) . . ? C14 Si2 Sc1 132.10(7) . . ? C15 Si2 Sc1 116.60(7) . . ? C16 Si2 Sc1 74.72(6) . . ? C20 O1 C17 108.39(14) . . ? C20 O1 Sc1 118.41(11) . . ? C17 O1 Sc1 133.16(11) . . ? C24 O2 C21 108.43(15) . . ? C24 O2 Sc1 123.17(12) . . ? C21 O2 Sc1 127.95(12) . . ? C43 B1 C31 102.08(15) . . ? C43 B1 C25 113.08(15) . . ? C31 B1 C25 112.16(15) . . ? C43 B1 C37 113.90(14) . . ? C31 B1 C37 114.10(15) . . ? C25 B1 C37 101.97(15) . . ? C3 C2 C10 108.39(17) . . ? C3 C2 C1 126.35(18) . . ? C10 C2 C1 125.24(17) . . ? C3 C2 Sc1 71.97(10) . . ? C10 C2 Sc1 72.57(10) . . ? C1 C2 Sc1 122.59(14) . . ? C2 C3 C4 108.31(17) . . ? C2 C3 Sc1 74.91(11) . . ? C4 C3 Sc1 76.74(10) . . ? C5 C4 C3 132.76(18) . . ? C5 C4 C9 119.74(19) . . ? C3 C4 C9 107.38(17) . . ? C5 C4 Sc1 124.54(13) . . ? C3 C4 Sc1 69.98(11) . . ? C9 C4 Sc1 74.21(11) . . ? C6 C5 C4 118.9(2) . . ? C5 C6 C7 121.6(2) . . ? C8 C7 C6 121.1(2) . . ? C7 C8 C9 119.35(19) . . ? C8 C9 C10 133.45(18) . . ? C8 C9 C4 119.29(19) . . ? C10 C9 C4 107.05(17) . . ? C8 C9 Sc1 126.27(13) . . ? C10 C9 Sc1 70.06(11) . . ? C4 C9 Sc1 72.93(11) . . ? C2 C10 C9 108.46(16) . . ? C2 C10 Sc1 74.29(11) . . ? C9 C10 Sc1 76.93(11) . . ? O1 C17 C18 105.05(15) . . ? C17 C18 C19 102.20(16) . . ? C20 C19 C18 101.76(17) . . ? O1 C20 C19 105.04(16) . . ? O2 C21 C22 105.12(18) . . ? C23 C22 C21 104.67(19) . . ? C24 C23 C22 106.3(2) . . ? O2 C24 C23 107.0(2) . . ? C30 C25 C26 113.24(17) . . ? C30 C25 B1 127.40(16) . . ? C26 C25 B1 119.28(16) . . ? F1 C26 C27 115.70(17) . . ? F1 C26 C25 119.19(17) . . ? C27 C26 C25 125.08(19) . . ? F2 C27 C26 121.04(19) . . ? F2 C27 C28 120.12(18) . . ? C26 C27 C28 118.83(18) . . ? F3 C28 C29 120.3(2) . . ? F3 C28 C27 120.60(19) . . ? C29 C28 C27 119.10(18) . . ? F5 C29 C28 119.70(18) . . ? F5 C29 C30 120.41(19) . . ? C28 C29 C30 119.89(19) . . ? F4 C30 C25 121.37(17) . . ? F4 C30 C29 114.93(18) . . ? C25 C30 C29 123.68(18) . . ? C36 C31 C32 112.72(18) . . ? C36 C31 B1 127.68(17) . . ? C32 C31 B1 119.35(16) . . ? F6 C32 C33 115.85(17) . . ? F6 C32 C31 118.90(18) . . ? C33 C32 C31 125.24(18) . . ? F7 C33 C32 121.19(17) . . ? F7 C33 C34 119.65(19) . . ? C32 C33 C34 119.15(18) . . ? F8 C34 C33 120.99(19) . . ? F8 C34 C35 120.11(18) . . ? C33 C34 C35 118.87(19) . . ? F10 C35 C34 119.91(19) . . ? F10 C35 C36 120.19(19) . . ? C34 C35 C36 119.90(18) . . ? F9 C36 C35 113.99(16) . . ? F9 C36 C31 121.98(18) . . ? C35 C36 C31 124.03(19) . . ? C38 C37 C42 113.36(17) . . ? C38 C37 B1 118.97(16) . . ? C42 C37 B1 127.07(17) . . ? F11 C38 C39 115.95(18) . . ? F11 C38 C37 119.34(16) . . ? C39 C38 C37 124.70(18) . . ? F12 C39 C38 121.30(18) . . ? F12 C39 C40 119.58(17) . . ? C38 C39 C40 119.12(19) . . ? F13 C40 C41 121.05(18) . . ? F13 C40 C39 120.06(19) . . ? C41 C40 C39 118.90(18) . . ? F14 C41 C40 119.41(17) . . ? F14 C41 C42 120.39(18) . . ? C40 C41 C42 120.19(17) . . ? F15 C42 C41 115.33(16) . . ? F15 C42 C37 120.93(17) . . ? C41 C42 C37 123.74(19) . . ? C48 C43 C44 112.84(16) . . ? C48 C43 B1 128.15(16) . . ? C44 C43 B1 118.70(15) . . ? F17 C44 C45 115.73(16) . . ? F17 C44 C43 119.19(16) . . ? C45 C44 C43 125.08(17) . . ? F16 C45 C46 120.18(17) . . ? F16 C45 C44 121.02(17) . . ? C46 C45 C44 118.80(18) . . ? F18 C46 C47 121.29(17) . . ? F18 C46 C45 119.68(18) . . ? C47 C46 C45 119.03(17) . . ? F19 C47 C46 119.72(17) . . ? F19 C47 C48 120.14(18) . . ? C46 C47 C48 120.14(17) . . ? F20 C48 C47 115.63(16) . . ? F20 C48 C43 120.30(16) . . ? C47 C48 C43 124.05(18) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.782 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.061 #===END # Attachement 'compound4.cif' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 670550' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (IndMe)2ScNTMS _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 N Sc Si2' _chemical_formula_sum 'C26 H36 N Sc Si2' _chemical_formula_weight 463.70 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 10.9022(17) _cell_length_b 15.712(2) _cell_length_c 14.570(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.884(3) _cell_angle_gamma 90.00 _cell_volume 2495.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9982 _cell_measurement_theta_min 3.5006 _cell_measurement_theta_max 31.0092 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.6973 _exptl_absorpt_correction_T_max 0.8549 _exptl_absorpt_process_details NUMABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku AFC-8 with Saturn70 CCD detector' _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 13713 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0854 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 29.12 _reflns_number_total 6624 _reflns_number_gt 4428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear SM (Rigaku/MSC, 2005)' _computing_cell_refinement 'CrystalClear SM' _computing_data_reduction 'CrystalClear SM' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL97 _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^)+(0.0468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6624 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1071 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.013 _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 0.89262(3) 0.21543(2) 0.82586(2) 0.01224(9) Uani 1 1 d . . . N1 N 1.06331(13) 0.27318(9) 0.82355(9) 0.0149(3) Uani 1 1 d . . . Si1 Si 1.10590(5) 0.37644(3) 0.80054(3) 0.01923(12) Uani 1 1 d . . . Si2 Si 1.16587(5) 0.19231(3) 0.84016(3) 0.01734(12) Uani 1 1 d . . . C1 C 0.63324(18) 0.33205(12) 0.73907(14) 0.0278(5) Uani 1 1 d . . . H1A H 0.6697 0.3890 0.7372 0.042 Uiso 1 1 calc R . . H1B H 0.6028 0.3208 0.8008 0.042 Uiso 1 1 calc R . . H1C H 0.5650 0.3288 0.6946 0.042 Uiso 1 1 calc R . . C2 C 0.72855(17) 0.26689(11) 0.71543(12) 0.0183(4) Uani 1 1 d . . . C3 C 0.71303(16) 0.17734(11) 0.72062(11) 0.0166(4) Uani 1 1 d . . . H3 H 0.6457 0.1484 0.7470 0.020 Uiso 1 1 calc R . . C4 C 0.81606(16) 0.13875(11) 0.67930(11) 0.0147(3) Uani 1 1 d . . . C5 C 0.84482(17) 0.05246(11) 0.65931(11) 0.0194(4) Uani 1 1 d . . . H5 H 0.7913 0.0080 0.6774 0.023 Uiso 1 1 calc R . . C6 C 0.95005(18) 0.03433(12) 0.61390(12) 0.0220(4) Uani 1 1 d . . . H6 H 0.9685 -0.0231 0.5990 0.026 Uiso 1 1 calc R . . C7 C 1.03257(18) 0.09976(12) 0.58845(12) 0.0214(4) Uani 1 1 d . . . H7 H 1.1059 0.0850 0.5579 0.026 Uiso 1 1 calc R . . C8 C 1.00904(17) 0.18376(11) 0.60691(11) 0.0186(4) Uani 1 1 d . . . H8 H 1.0656 0.2267 0.5899 0.022 Uiso 1 1 calc R . . C9 C 0.89876(17) 0.20532(11) 0.65181(11) 0.0154(4) Uani 1 1 d . . . C10 C 0.84396(17) 0.28385(11) 0.67717(11) 0.0172(4) Uani 1 1 d . . . H10 H 0.8793 0.3386 0.6696 0.021 Uiso 1 1 calc R . . C11 C 0.97295(18) 0.32685(13) 1.03430(12) 0.0265(4) Uani 1 1 d . . . H11A H 0.9840 0.3166 1.1003 0.040 Uiso 1 1 calc R . . H11B H 0.9376 0.3835 1.0245 0.040 Uiso 1 1 calc R . . H11C H 1.0526 0.3235 1.0042 0.040 Uiso 1 1 calc R . . C12 C 0.88807(17) 0.26080(12) 0.99426(11) 0.0191(4) Uani 1 1 d . . . C13 C 0.90952(17) 0.17284(12) 0.99136(11) 0.0187(4) Uani 1 1 d . . . H13 H 0.9841 0.1452 1.0083 0.022 Uiso 1 1 calc R . . C14 C 0.80055(16) 0.13177(11) 0.95878(11) 0.0161(4) Uani 1 1 d . . . C15 C 0.76771(18) 0.04485(11) 0.94695(12) 0.0210(4) Uani 1 1 d . . . H15 H 0.8274 0.0013 0.9546 0.025 Uiso 1 1 calc R . . C16 C 0.64877(19) 0.02486(12) 0.92440(12) 0.0246(4) Uani 1 1 d . . . H16 H 0.6261 -0.0332 0.9175 0.029 Uiso 1 1 calc R . . C17 C 0.55926(18) 0.08863(13) 0.91117(12) 0.0239(4) Uani 1 1 d . . . H17 H 0.4768 0.0727 0.8979 0.029 Uiso 1 1 calc R . . C18 C 0.58893(17) 0.17334(12) 0.91717(12) 0.0201(4) Uani 1 1 d . . . H18 H 0.5282 0.2157 0.9066 0.024 Uiso 1 1 calc R . . C19 C 0.71114(17) 0.19668(11) 0.93934(11) 0.0167(4) Uani 1 1 d . . . C20 C 0.77081(17) 0.27665(11) 0.95544(12) 0.0183(4) Uani 1 1 d . . . H20 H 0.7372 0.3311 0.9422 0.022 Uiso 1 1 calc R . . C21 C 0.97525(19) 0.45167(12) 0.82087(14) 0.0284(5) Uani 1 1 d . . . H21A H 0.9040 0.4342 0.7836 0.043 Uiso 1 1 calc R . . H21B H 0.9996 0.5095 0.8036 0.043 Uiso 1 1 calc R . . H21C H 0.9540 0.4506 0.8860 0.043 Uiso 1 1 calc R . . C22 C 1.2391(2) 0.41250(15) 0.87421(15) 0.0366(5) Uani 1 1 d . . . H22A H 1.2177 0.4075 0.9391 0.055 Uiso 1 1 calc R . . H22B H 1.2583 0.4720 0.8601 0.055 Uiso 1 1 calc R . . H22C H 1.3107 0.3768 0.8618 0.055 Uiso 1 1 calc R . . C23 C 1.15539(19) 0.39331(13) 0.67930(13) 0.0268(4) Uani 1 1 d . . . H23A H 1.2247 0.3558 0.6662 0.040 Uiso 1 1 calc R . . H23B H 1.1803 0.4527 0.6712 0.040 Uiso 1 1 calc R . . H23C H 1.0870 0.3803 0.6372 0.040 Uiso 1 1 calc R . . C24 C 1.07825(17) 0.08767(12) 0.82884(12) 0.0215(4) Uani 1 1 d . . . H24A H 0.9904 0.0983 0.8361 0.032 Uiso 1 1 calc R . . H24B H 1.1069 0.0480 0.8764 0.032 Uiso 1 1 calc R . . H24C H 1.0924 0.0630 0.7681 0.032 Uiso 1 1 calc R . . C25 C 1.24404(17) 0.19231(13) 0.95524(12) 0.0255(4) Uani 1 1 d . . . H25A H 1.2961 0.2429 0.9611 0.038 Uiso 1 1 calc R . . H25B H 1.2948 0.1411 0.9616 0.038 Uiso 1 1 calc R . . H25C H 1.1823 0.1929 1.0034 0.038 Uiso 1 1 calc R . . C26 C 1.29074(17) 0.18698(14) 0.75302(13) 0.0274(4) Uani 1 1 d . . . H26A H 1.2541 0.1835 0.6913 0.041 Uiso 1 1 calc R . . H26B H 1.3415 0.1365 0.7646 0.041 Uiso 1 1 calc R . . H26C H 1.3418 0.2382 0.7577 0.041 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 0.01196(17) 0.01552(16) 0.00923(15) -0.00073(12) -0.00070(11) 0.00005(13) N1 0.0125(7) 0.0207(8) 0.0116(7) -0.0006(6) -0.0002(5) -0.0017(6) Si1 0.0168(3) 0.0216(3) 0.0192(2) -0.0008(2) -0.0008(2) -0.0051(2) Si2 0.0125(3) 0.0267(3) 0.0128(2) 0.00068(19) -0.00076(18) 0.0027(2) C1 0.0253(11) 0.0253(10) 0.0326(11) -0.0043(8) -0.0068(9) 0.0074(9) C2 0.0197(10) 0.0196(9) 0.0153(8) -0.0024(7) -0.0069(7) 0.0037(7) C3 0.0147(9) 0.0204(9) 0.0147(8) -0.0008(7) -0.0034(6) -0.0029(7) C4 0.0164(9) 0.0171(8) 0.0105(7) -0.0003(6) -0.0028(6) -0.0028(7) C5 0.0234(10) 0.0173(9) 0.0176(8) -0.0012(7) -0.0023(7) -0.0043(7) C6 0.0282(11) 0.0184(9) 0.0193(9) -0.0043(7) -0.0004(8) 0.0026(8) C7 0.0205(10) 0.0289(10) 0.0149(8) -0.0031(7) 0.0027(7) 0.0009(8) C8 0.0214(10) 0.0237(9) 0.0109(8) 0.0027(7) 0.0001(7) -0.0045(8) C9 0.0199(9) 0.0188(9) 0.0075(7) 0.0015(6) -0.0029(6) -0.0005(7) C10 0.0227(10) 0.0142(8) 0.0145(8) 0.0024(6) -0.0068(7) -0.0017(7) C11 0.0250(11) 0.0375(11) 0.0171(9) -0.0102(8) 0.0018(8) -0.0105(9) C12 0.0177(10) 0.0293(10) 0.0102(8) -0.0050(7) 0.0035(7) -0.0050(8) C13 0.0166(9) 0.0292(10) 0.0103(8) 0.0019(7) -0.0003(7) 0.0005(8) C14 0.0161(9) 0.0219(9) 0.0103(7) -0.0001(7) 0.0029(6) -0.0013(7) C15 0.0244(10) 0.0206(9) 0.0182(9) 0.0012(7) 0.0040(7) -0.0001(8) C16 0.0308(12) 0.0223(10) 0.0207(9) -0.0022(8) 0.0024(8) -0.0088(8) C17 0.0184(10) 0.0342(11) 0.0193(9) -0.0040(8) 0.0023(7) -0.0082(8) C18 0.0138(9) 0.0274(10) 0.0192(9) -0.0038(7) 0.0018(7) 0.0004(8) C19 0.0164(9) 0.0220(9) 0.0119(8) -0.0029(6) 0.0030(6) -0.0008(7) C20 0.0175(9) 0.0204(9) 0.0170(8) -0.0040(7) 0.0034(7) -0.0011(7) C21 0.0335(12) 0.0213(10) 0.0305(11) -0.0041(8) 0.0000(9) -0.0018(9) C22 0.0309(13) 0.0410(13) 0.0376(12) -0.0001(10) -0.0065(10) -0.0152(10) C23 0.0269(11) 0.0264(10) 0.0271(10) 0.0040(8) 0.0041(8) -0.0045(9) C24 0.0226(10) 0.0242(10) 0.0177(9) 0.0013(7) -0.0005(7) 0.0076(8) C25 0.0162(10) 0.0413(12) 0.0189(9) 0.0020(8) -0.0037(7) 0.0027(8) C26 0.0163(10) 0.0450(12) 0.0210(9) 0.0020(9) 0.0029(7) 0.0069(9) _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 N1 2.0711(15) . ? Sc1 C10 2.4689(17) . ? Sc1 C13 2.5066(17) . ? Sc1 C20 2.5161(18) . ? Sc1 C2 2.5206(17) . ? Sc1 C3 2.5397(17) . ? Sc1 C9 2.5429(16) . ? Sc1 C12 2.5562(17) . ? Sc1 C14 2.5585(17) . ? Sc1 C4 2.5794(16) . ? Sc1 C19 2.6146(18) . ? Sc1 Si2 3.0052(7) . ? Sc1 C24 2.850(2) . ? N1 Si2 1.7072(15) . ? N1 Si1 1.7220(15) . ? Si1 C23 1.8738(19) . ? Si1 C21 1.878(2) . ? Si1 C22 1.880(2) . ? Si2 C25 1.8691(18) . ? Si2 C26 1.8777(19) . ? Si2 C24 1.907(2) . ? C1 C2 1.502(2) . ? C2 C10 1.409(3) . ? C2 C3 1.419(2) . ? C3 C4 1.419(2) . ? C4 C5 1.423(2) . ? C4 C9 1.442(2) . ? C5 C6 1.363(3) . ? C6 C7 1.419(3) . ? C7 C8 1.372(2) . ? C8 C9 1.419(3) . ? C9 C10 1.422(2) . ? C11 C12 1.502(2) . ? C12 C13 1.402(3) . ? C12 C20 1.412(2) . ? C13 C14 1.427(2) . ? C14 C15 1.422(2) . ? C14 C19 1.436(2) . ? C15 C16 1.369(3) . ? C16 C17 1.410(3) . ? C17 C18 1.372(3) . ? C18 C19 1.414(2) . ? C19 C20 1.433(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sc1 C10 88.62(6) . . ? N1 Sc1 C13 94.58(6) . . ? C10 Sc1 C13 166.43(6) . . ? N1 Sc1 C20 109.24(6) . . ? C10 Sc1 C20 112.54(6) . . ? C13 Sc1 C20 53.99(6) . . ? N1 Sc1 C2 118.56(6) . . ? C10 Sc1 C2 32.80(6) . . ? C13 Sc1 C2 137.79(6) . . ? C20 Sc1 C2 88.79(6) . . ? N1 Sc1 C3 141.07(6) . . ? C10 Sc1 C3 54.52(6) . . ? C13 Sc1 C3 124.23(6) . . ? C20 Sc1 C3 97.60(6) . . ? C2 Sc1 C3 32.57(5) . . ? N1 Sc1 C9 88.49(6) . . ? C10 Sc1 C9 32.93(5) . . ? C13 Sc1 C9 160.06(6) . . ? C20 Sc1 C9 142.61(6) . . ? C2 Sc1 C9 54.04(6) . . ? C3 Sc1 C9 54.20(6) . . ? N1 Sc1 C12 85.65(6) . . ? C10 Sc1 C12 135.54(6) . . ? C13 Sc1 C12 32.15(6) . . ? C20 Sc1 C12 32.31(6) . . ? C2 Sc1 C12 119.95(6) . . ? C3 Sc1 C12 128.24(6) . . ? C9 Sc1 C12 167.38(6) . . ? N1 Sc1 C14 126.91(6) . . ? C10 Sc1 C14 143.75(6) . . ? C13 Sc1 C14 32.70(5) . . ? C20 Sc1 C14 53.89(6) . . ? C2 Sc1 C14 111.42(6) . . ? C3 Sc1 C14 91.61(6) . . ? C9 Sc1 C14 137.69(6) . . ? C12 Sc1 C14 53.35(6) . . ? N1 Sc1 C4 118.07(5) . . ? C10 Sc1 C4 54.16(6) . . ? C13 Sc1 C4 133.61(6) . . ? C20 Sc1 C4 129.20(6) . . ? C2 Sc1 C4 53.42(5) . . ? C3 Sc1 C4 32.17(5) . . ? C9 Sc1 C4 32.69(5) . . ? C12 Sc1 C4 156.07(6) . . ? C14 Sc1 C4 105.13(6) . . ? N1 Sc1 C19 138.47(6) . . ? C10 Sc1 C19 116.72(6) . . ? C13 Sc1 C19 53.61(6) . . ? C20 Sc1 C19 32.36(5) . . ? C2 Sc1 C19 84.45(6) . . ? C3 Sc1 C19 76.79(6) . . ? C9 Sc1 C19 130.96(6) . . ? C12 Sc1 C19 53.01(6) . . ? C14 Sc1 C19 32.21(5) . . ? C4 Sc1 C19 103.45(6) . . ? N1 Sc1 Si2 33.29(4) . . ? C10 Sc1 Si2 108.23(5) . . ? C13 Sc1 Si2 80.96(4) . . ? C20 Sc1 Si2 121.89(4) . . ? C2 Sc1 Si2 140.89(5) . . ? C3 Sc1 Si2 140.13(4) . . ? C9 Sc1 Si2 91.16(4) . . ? C12 Sc1 Si2 90.06(4) . . ? C14 Sc1 Si2 106.59(4) . . ? C4 Sc1 Si2 107.98(4) . . ? C19 Sc1 Si2 134.55(4) . . ? Si2 N1 Si1 123.43(9) . . ? Si2 N1 Sc1 104.97(7) . . ? Si1 N1 Sc1 131.37(8) . . ? N1 Si1 C23 113.53(8) . . ? N1 Si1 C21 110.79(8) . . ? C23 Si1 C21 106.85(9) . . ? N1 Si1 C22 112.40(9) . . ? C23 Si1 C22 105.34(10) . . ? C21 Si1 C22 107.54(10) . . ? N1 Si2 C25 114.57(8) . . ? N1 Si2 C26 114.67(8) . . ? C25 Si2 C26 106.34(9) . . ? N1 Si2 C24 107.65(8) . . ? C25 Si2 C24 107.36(9) . . ? C26 Si2 C24 105.69(9) . . ? N1 Si2 Sc1 41.74(5) . . ? C25 Si2 Sc1 120.00(6) . . ? C26 Si2 Sc1 133.38(6) . . ? C24 Si2 Sc1 66.64(6) . . ? C10 C2 C3 108.45(15) . . ? C10 C2 C1 125.91(17) . . ? C3 C2 C1 125.44(17) . . ? C10 C2 Sc1 71.59(10) . . ? C3 C2 Sc1 74.45(10) . . ? C1 C2 Sc1 123.97(12) . . ? C4 C3 C2 107.78(15) . . ? C4 C3 Sc1 75.46(10) . . ? C2 C3 Sc1 72.97(10) . . ? C3 C4 C5 132.27(16) . . ? C3 C4 C9 108.09(15) . . ? C5 C4 C9 119.59(16) . . ? C3 C4 Sc1 72.38(9) . . ? C5 C4 Sc1 123.03(11) . . ? C9 C4 Sc1 72.27(9) . . ? C6 C5 C4 119.22(17) . . ? C5 C6 C7 121.14(17) . . ? C8 C7 C6 121.63(18) . . ? C7 C8 C9 118.85(17) . . ? C8 C9 C10 133.58(17) . . ? C8 C9 C4 119.54(16) . . ? C10 C9 C4 106.87(16) . . ? C8 C9 Sc1 120.69(11) . . ? C10 C9 Sc1 70.67(9) . . ? C4 C9 Sc1 75.05(9) . . ? C2 C10 C9 108.65(16) . . ? C2 C10 Sc1 75.62(10) . . ? C9 C10 Sc1 76.40(9) . . ? C13 C12 C20 108.19(16) . . ? C13 C12 C11 126.18(18) . . ? C20 C12 C11 125.60(18) . . ? C13 C12 Sc1 71.98(9) . . ? C20 C12 Sc1 72.28(10) . . ? C11 C12 Sc1 122.98(12) . . ? C12 C13 C14 108.50(16) . . ? C12 C13 Sc1 75.88(10) . . ? C14 C13 Sc1 75.65(10) . . ? C15 C14 C13 132.97(17) . . ? C15 C14 C19 119.31(17) . . ? C13 C14 C19 107.68(16) . . ? C15 C14 Sc1 120.19(11) . . ? C13 C14 Sc1 71.65(9) . . ? C19 C14 Sc1 76.05(10) . . ? C16 C15 C14 119.02(18) . . ? C15 C16 C17 121.38(18) . . ? C18 C17 C16 121.24(18) . . ? C17 C18 C19 119.10(17) . . ? C18 C19 C20 133.51(17) . . ? C18 C19 C14 119.67(16) . . ? C20 C19 C14 106.59(16) . . ? C18 C19 Sc1 127.17(12) . . ? C20 C19 Sc1 70.04(10) . . ? C14 C19 Sc1 71.75(10) . . ? C12 C20 C19 108.48(16) . . ? C12 C20 Sc1 75.41(10) . . ? C19 C20 Sc1 77.61(10) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 29.12 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.593 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.070 #===END #Attachment 'compound3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 670551' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (PhInd)2GdNTMS _chemical_melting_point ? _chemical_formula_moiety 'C36 H40 Gd N Si2' _chemical_formula_sum 'C36 H40 Gd N Si2' _chemical_formula_weight 700.12 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' Gd Gd -0.1653 3.9035 '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' _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 9.772(3) _cell_length_b 9.914(2) _cell_length_c 17.750(6) _cell_angle_alpha 77.26(3) _cell_angle_beta 75.60(3) _cell_angle_gamma 77.78(3) _cell_volume 1602.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 1215 _cell_measurement_theta_min 2.1818 _cell_measurement_theta_max 34.9792 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 710 _exptl_absorpt_coefficient_mu 2.170 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.1387 _exptl_absorpt_correction_T_max 0.2960 _exptl_absorpt_process_details NUMABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku AFC-8 with Saturn70 CCD detector' _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 19841 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.1012 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 34.99 _reflns_number_total 13533 _reflns_number_gt 10586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear SM (Rigaku/MSC, 2005)' _computing_cell_refinement 'CrystalClear SM' _computing_data_reduction 'CrystalClear SM' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL97 _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^)+(0.0107P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13533 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.024 _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 Gd1 Gd 0.719220(12) 0.883146(13) 0.745147(7) 0.01688(3) Uani 1 1 d . . . N1 N 0.7997(2) 0.7191(2) 0.84166(11) 0.0198(4) Uani 1 1 d . . . Si1 Si 0.88570(8) 0.54968(8) 0.83984(4) 0.02423(15) Uani 1 1 d . . . Si2 Si 0.75807(7) 0.79868(8) 0.92237(4) 0.02204(15) Uani 1 1 d . . . C1 C 0.7264(3) 0.6170(3) 0.57773(16) 0.0251(5) Uani 1 1 d . . . H1 H 0.7069 0.5490 0.6242 0.030 Uiso 1 1 calc R . . C2 C 0.8156(3) 0.5756(4) 0.50967(19) 0.0361(7) Uani 1 1 d . . . H2 H 0.8570 0.4797 0.5106 0.043 Uiso 1 1 calc R . . C3 C 0.8453(3) 0.6714(4) 0.44066(17) 0.0368(7) Uani 1 1 d . . . H3 H 0.9097 0.6430 0.3951 0.044 Uiso 1 1 calc R . . C4 C 0.7790(3) 0.8099(4) 0.43959(16) 0.0335(7) Uani 1 1 d . . . H4 H 0.7948 0.8762 0.3920 0.040 Uiso 1 1 calc R . . C5 C 0.6903(3) 0.8527(3) 0.50669(15) 0.0258(5) Uani 1 1 d . . . H5 H 0.6452 0.9478 0.5046 0.031 Uiso 1 1 calc R . . C6 C 0.6656(2) 0.7567(3) 0.57840(14) 0.0201(5) Uani 1 1 d . . . C7 C 0.5789(2) 0.8031(3) 0.65224(14) 0.0177(4) Uani 1 1 d . . . C8 C 0.5111(2) 0.9428(3) 0.65994(14) 0.0177(4) Uani 1 1 d . . . H8 H 0.5156 1.0226 0.6189 0.021 Uiso 1 1 calc R . . C9 C 0.4359(2) 0.9425(3) 0.73917(14) 0.0187(5) Uani 1 1 d . . . C10 C 0.3465(3) 1.0493(3) 0.77826(16) 0.0246(5) Uani 1 1 d . . . H10 H 0.3318 1.1433 0.7510 0.030 Uiso 1 1 calc R . . C11 C 0.2807(3) 1.0148(3) 0.85696(17) 0.0303(6) Uani 1 1 d . . . H11 H 0.2199 1.0861 0.8834 0.036 Uiso 1 1 calc R . . C12 C 0.3019(3) 0.8768(3) 0.89862(16) 0.0307(6) Uani 1 1 d . . . H12 H 0.2541 0.8564 0.9524 0.037 Uiso 1 1 calc R . . C13 C 0.3896(3) 0.7718(3) 0.86343(15) 0.0255(5) Uani 1 1 d . . . H13 H 0.4049 0.6796 0.8930 0.031 Uiso 1 1 calc R . . C14 C 0.4590(2) 0.8006(3) 0.78157(14) 0.0194(5) Uani 1 1 d . . . C15 C 0.5502(2) 0.7165(3) 0.72757(14) 0.0188(5) Uani 1 1 d . . . H15 H 0.5859 0.6192 0.7398 0.023 Uiso 1 1 calc R . . C16 C 0.5944(3) 1.2952(3) 0.74173(17) 0.0285(6) Uani 1 1 d . . . H16 H 0.6416 1.2674 0.7848 0.034 Uiso 1 1 calc R . . C17 C 0.4652(3) 1.3870(3) 0.7493(2) 0.0344(7) Uani 1 1 d . . . H17 H 0.4235 1.4199 0.7976 0.041 Uiso 1 1 calc R . . C18 C 0.3977(3) 1.4304(3) 0.6866(2) 0.0421(8) Uani 1 1 d . . . H18 H 0.3083 1.4919 0.6920 0.051 Uiso 1 1 calc R . . C19 C 0.4596(3) 1.3846(3) 0.6158(2) 0.0392(8) Uani 1 1 d . . . H19 H 0.4144 1.4170 0.5720 0.047 Uiso 1 1 calc R . . C20 C 0.5878(3) 1.2912(3) 0.60867(18) 0.0297(6) Uani 1 1 d . . . H20 H 0.6297 1.2597 0.5599 0.036 Uiso 1 1 calc R . . C21 C 0.6558(3) 1.2431(3) 0.67226(16) 0.0249(5) Uani 1 1 d . . . C22 C 0.7866(2) 1.1323(3) 0.66559(15) 0.0216(5) Uani 1 1 d . . . C23 C 0.8255(2) 1.0436(3) 0.60964(14) 0.0222(5) Uani 1 1 d . . . H23 H 0.7782 1.0490 0.5681 0.027 Uiso 1 1 calc R . . C24 C 0.9479(2) 0.9440(3) 0.62543(14) 0.0204(5) Uani 1 1 d . . . C25 C 1.0332(3) 0.8348(3) 0.58612(15) 0.0250(5) Uani 1 1 d . . . H25 H 1.0073 0.8123 0.5428 0.030 Uiso 1 1 calc R . . C26 C 1.1537(3) 0.7625(3) 0.61203(16) 0.0278(6) Uani 1 1 d . . . H26 H 1.2139 0.6919 0.5848 0.033 Uiso 1 1 calc R . . C27 C 1.1901(3) 0.7912(3) 0.67867(16) 0.0263(6) Uani 1 1 d . . . H27 H 1.2746 0.7399 0.6951 0.032 Uiso 1 1 calc R . . C28 C 1.1056(2) 0.8917(3) 0.72008(15) 0.0241(5) Uani 1 1 d . . . H28 H 1.1295 0.9074 0.7658 0.029 Uiso 1 1 calc R . . C29 C 0.9826(2) 0.9716(3) 0.69375(14) 0.0200(5) Uani 1 1 d . . . C30 C 0.8799(3) 1.0874(3) 0.71923(15) 0.0223(5) Uani 1 1 d . . . H30 H 0.8750 1.1271 0.7641 0.027 Uiso 1 1 calc R . . C31 C 0.9264(3) 0.5078(3) 0.73802(16) 0.0349(7) Uani 1 1 d . . . H31A H 0.8373 0.5015 0.7241 0.052 Uiso 1 1 calc R . . H31B H 0.9915 0.4179 0.7365 0.052 Uiso 1 1 calc R . . H31C H 0.9719 0.5819 0.7002 0.052 Uiso 1 1 calc R . . C32 C 0.7746(4) 0.4176(3) 0.90388(19) 0.0486(9) Uani 1 1 d . . . H32A H 0.7672 0.4205 0.9596 0.073 Uiso 1 1 calc R . . H32B H 0.8200 0.3237 0.8933 0.073 Uiso 1 1 calc R . . H32C H 0.6786 0.4396 0.8922 0.073 Uiso 1 1 calc R . . C33 C 1.0609(3) 0.5137(4) 0.87252(19) 0.0419(8) Uani 1 1 d . . . H33A H 1.1192 0.5849 0.8425 0.063 Uiso 1 1 calc R . . H33B H 1.1123 0.4207 0.8630 0.063 Uiso 1 1 calc R . . H33C H 1.0426 0.5166 0.9290 0.063 Uiso 1 1 calc R . . C34 C 0.6498(3) 0.7050(3) 1.01393(15) 0.0310(6) Uani 1 1 d . . . H34A H 0.5612 0.6909 1.0025 0.047 Uiso 1 1 calc R . . H34B H 0.6262 0.7612 1.0558 0.047 Uiso 1 1 calc R . . H34C H 0.7054 0.6137 1.0313 0.047 Uiso 1 1 calc R . . C35 C 0.9172(3) 0.8416(3) 0.94797(17) 0.0340(7) Uani 1 1 d . . . H35A H 0.9714 0.7556 0.9728 0.051 Uiso 1 1 calc R . . H35B H 0.8845 0.9081 0.9848 0.051 Uiso 1 1 calc R . . H35C H 0.9788 0.8835 0.8997 0.051 Uiso 1 1 calc R . . C36 C 0.6413(3) 0.9734(3) 0.89591(15) 0.0254(5) Uani 1 1 d . . . H36A H 0.6932 1.0289 0.8489 0.038 Uiso 1 1 calc R . . H36B H 0.6171 1.0244 0.9402 0.038 Uiso 1 1 calc R . . H36C H 0.5531 0.9574 0.8849 0.038 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 Gd1 0.01392(6) 0.01956(6) 0.01533(6) 0.00332(4) -0.00082(4) -0.00824(4) N1 0.0156(9) 0.0240(11) 0.0166(9) 0.0041(8) -0.0019(8) -0.0063(8) Si1 0.0244(4) 0.0230(4) 0.0193(3) 0.0038(3) -0.0008(3) -0.0033(3) Si2 0.0169(3) 0.0289(4) 0.0172(3) 0.0005(3) -0.0005(3) -0.0054(3) C1 0.0234(13) 0.0265(14) 0.0265(13) -0.0058(11) -0.0047(11) -0.0062(10) C2 0.0267(15) 0.0419(19) 0.0407(18) -0.0183(15) -0.0049(13) 0.0008(13) C3 0.0247(14) 0.059(2) 0.0279(15) -0.0191(15) 0.0059(12) -0.0119(14) C4 0.0316(15) 0.048(2) 0.0221(13) -0.0039(13) 0.0037(11) -0.0231(14) C5 0.0246(13) 0.0323(15) 0.0222(12) -0.0018(11) -0.0021(10) -0.0151(11) C6 0.0147(10) 0.0263(13) 0.0202(11) -0.0017(10) -0.0029(9) -0.0087(9) C7 0.0155(10) 0.0177(11) 0.0200(11) 0.0015(9) -0.0030(9) -0.0088(8) C8 0.0145(10) 0.0165(11) 0.0210(11) 0.0007(9) -0.0023(9) -0.0060(8) C9 0.0121(10) 0.0203(11) 0.0234(12) -0.0011(9) -0.0020(9) -0.0071(9) C10 0.0177(12) 0.0229(13) 0.0330(14) -0.0055(11) -0.0027(10) -0.0054(10) C11 0.0185(12) 0.0388(17) 0.0347(15) -0.0151(13) 0.0028(11) -0.0080(12) C12 0.0212(13) 0.0464(19) 0.0241(13) -0.0074(13) 0.0060(10) -0.0164(12) C13 0.0221(12) 0.0327(15) 0.0198(12) 0.0016(11) 0.0019(10) -0.0146(11) C14 0.0125(10) 0.0229(12) 0.0212(11) 0.0012(9) 0.0008(9) -0.0103(9) C15 0.0165(11) 0.0187(11) 0.0201(11) 0.0011(9) -0.0008(9) -0.0085(9) C16 0.0282(14) 0.0180(12) 0.0376(16) 0.0026(11) -0.0049(12) -0.0105(11) C17 0.0311(15) 0.0161(12) 0.0504(19) -0.0005(13) -0.0002(14) -0.0076(11) C18 0.0257(15) 0.0176(13) 0.078(3) 0.0013(16) -0.0101(16) -0.0035(11) C19 0.0338(17) 0.0234(14) 0.060(2) 0.0080(15) -0.0195(16) -0.0091(13) C20 0.0288(14) 0.0183(12) 0.0407(16) 0.0043(12) -0.0108(13) -0.0071(11) C21 0.0210(12) 0.0165(11) 0.0353(15) 0.0054(11) -0.0057(11) -0.0092(10) C22 0.0193(11) 0.0177(11) 0.0253(12) 0.0045(10) -0.0018(10) -0.0101(9) C23 0.0181(11) 0.0283(13) 0.0189(11) 0.0039(10) -0.0019(9) -0.0121(10) C24 0.0168(11) 0.0241(12) 0.0185(11) 0.0014(9) 0.0023(9) -0.0122(9) C25 0.0222(12) 0.0328(15) 0.0163(11) -0.0006(10) 0.0036(9) -0.0098(11) C26 0.0217(13) 0.0313(15) 0.0251(13) -0.0028(11) 0.0042(10) -0.0060(11) C27 0.0140(11) 0.0308(15) 0.0298(14) 0.0039(11) -0.0024(10) -0.0068(10) C28 0.0168(11) 0.0317(14) 0.0247(12) -0.0002(11) -0.0028(10) -0.0128(10) C29 0.0136(10) 0.0213(12) 0.0224(12) 0.0026(10) -0.0001(9) -0.0086(9) C30 0.0194(11) 0.0233(12) 0.0252(12) -0.0010(10) -0.0021(10) -0.0118(10) C31 0.0334(16) 0.0383(18) 0.0289(15) -0.0074(13) -0.0007(12) -0.0023(13) C32 0.064(2) 0.0298(17) 0.0381(18) 0.0003(14) 0.0142(17) -0.0144(16) C33 0.0371(17) 0.044(2) 0.0376(18) -0.0052(15) -0.0139(15) 0.0139(15) C34 0.0256(14) 0.0391(17) 0.0203(12) 0.0051(12) 0.0011(10) -0.0057(12) C35 0.0263(14) 0.051(2) 0.0263(14) -0.0121(14) -0.0006(11) -0.0108(13) C36 0.0236(13) 0.0277(14) 0.0222(12) -0.0028(11) 0.0000(10) -0.0059(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 N1 2.258(2) . ? Gd1 C23 2.676(3) . ? Gd1 C15 2.682(2) . ? Gd1 C22 2.686(3) . ? Gd1 C30 2.712(3) . ? Gd1 C14 2.718(2) . ? Gd1 C7 2.719(2) . ? Gd1 C8 2.720(2) . ? Gd1 C9 2.730(2) . ? Gd1 C24 2.742(3) . ? Gd1 C29 2.768(2) . ? Gd1 Si2 3.1683(13) . ? N1 Si2 1.707(2) . ? N1 Si1 1.715(2) . ? Si1 C31 1.871(3) . ? Si1 C32 1.875(3) . ? Si1 C33 1.881(3) . ? Si2 C34 1.876(3) . ? Si2 C35 1.877(3) . ? Si2 C36 1.896(3) . ? C1 C6 1.388(4) . ? C1 C2 1.390(4) . ? C2 C3 1.383(4) . ? C3 C4 1.387(4) . ? C4 C5 1.380(4) . ? C5 C6 1.412(3) . ? C6 C7 1.482(3) . ? C7 C15 1.419(3) . ? C7 C8 1.423(3) . ? C8 C9 1.415(3) . ? C9 C10 1.413(4) . ? C9 C14 1.442(3) . ? C10 C11 1.385(4) . ? C11 C12 1.404(4) . ? C12 C13 1.361(4) . ? C13 C14 1.436(3) . ? C14 C15 1.422(3) . ? C16 C17 1.387(4) . ? C16 C21 1.389(4) . ? C17 C18 1.375(4) . ? C18 C19 1.382(5) . ? C19 C20 1.387(4) . ? C20 C21 1.394(3) . ? C21 C22 1.498(3) . ? C22 C23 1.400(4) . ? C22 C30 1.417(3) . ? C23 C24 1.425(3) . ? C24 C25 1.420(4) . ? C24 C29 1.432(3) . ? C25 C26 1.370(3) . ? C26 C27 1.417(4) . ? C27 C28 1.374(4) . ? C28 C29 1.415(3) . ? C29 C30 1.430(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 N1 Gd1 C23 138.81(7) . . ? N1 Gd1 C15 91.23(8) . . ? C23 Gd1 C15 113.29(8) . . ? N1 Gd1 C22 135.02(7) . . ? C23 Gd1 C22 30.26(8) . . ? C15 Gd1 C22 133.37(7) . . ? N1 Gd1 C30 104.58(8) . . ? C23 Gd1 C30 50.27(8) . . ? C15 Gd1 C30 163.04(7) . . ? C22 Gd1 C30 30.44(7) . . ? N1 Gd1 C14 92.99(8) . . ? C23 Gd1 C14 125.13(7) . . ? C15 Gd1 C14 30.52(7) . . ? C22 Gd1 C14 127.52(7) . . ? C30 Gd1 C14 150.19(8) . . ? N1 Gd1 C7 118.06(8) . . ? C23 Gd1 C7 83.05(8) . . ? C15 Gd1 C7 30.45(7) . . ? C22 Gd1 C7 104.28(8) . . ? C30 Gd1 C7 132.65(7) . . ? C14 Gd1 C7 50.07(7) . . ? N1 Gd1 C8 140.66(7) . . ? C23 Gd1 C8 74.93(8) . . ? C15 Gd1 C8 50.42(7) . . ? C22 Gd1 C8 84.23(8) . . ? C30 Gd1 C8 114.58(8) . . ? C14 Gd1 C8 50.21(7) . . ? C7 Gd1 C8 30.33(7) . . ? N1 Gd1 C9 121.32(8) . . ? C23 Gd1 C9 99.52(8) . . ? C15 Gd1 C9 50.53(8) . . ? C22 Gd1 C9 96.83(8) . . ? C30 Gd1 C9 122.07(8) . . ? C14 Gd1 C9 30.69(7) . . ? C7 Gd1 C9 49.94(8) . . ? C8 Gd1 C9 30.10(7) . . ? N1 Gd1 C24 108.91(8) . . ? C23 Gd1 C24 30.46(7) . . ? C15 Gd1 C24 119.18(8) . . ? C22 Gd1 C24 49.98(8) . . ? C30 Gd1 C24 50.09(8) . . ? C14 Gd1 C24 144.82(7) . . ? C7 Gd1 C24 94.84(8) . . ? C8 Gd1 C24 99.24(7) . . ? C9 Gd1 C24 127.61(7) . . ? N1 Gd1 C29 91.18(7) . . ? C23 Gd1 C29 50.00(7) . . ? C15 Gd1 C29 146.29(8) . . ? C22 Gd1 C29 49.85(7) . . ? C30 Gd1 C29 30.24(8) . . ? C14 Gd1 C29 174.78(7) . . ? C7 Gd1 C29 124.96(7) . . ? C8 Gd1 C29 124.92(7) . . ? C9 Gd1 C29 146.30(7) . . ? C24 Gd1 C29 30.13(7) . . ? N1 Gd1 Si2 31.32(6) . . ? C23 Gd1 Si2 139.28(6) . . ? C15 Gd1 Si2 106.93(6) . . ? C22 Gd1 Si2 116.69(6) . . ? C30 Gd1 Si2 89.92(6) . . ? C14 Gd1 Si2 93.17(6) . . ? C7 Gd1 Si2 137.38(5) . . ? C8 Gd1 Si2 140.61(6) . . ? C9 Gd1 Si2 110.91(6) . . ? C24 Gd1 Si2 119.90(6) . . ? C29 Gd1 Si2 92.02(6) . . ? Si2 N1 Si1 124.60(12) . . ? Si2 N1 Gd1 105.24(10) . . ? Si1 N1 Gd1 130.15(11) . . ? N1 Si1 C31 111.33(12) . . ? N1 Si1 C32 112.63(13) . . ? C31 Si1 C32 105.53(16) . . ? N1 Si1 C33 112.65(13) . . ? C31 Si1 C33 106.88(14) . . ? C32 Si1 C33 107.38(16) . . ? N1 Si2 C34 115.47(13) . . ? N1 Si2 C35 113.91(12) . . ? C34 Si2 C35 108.81(13) . . ? N1 Si2 C36 106.61(11) . . ? C34 Si2 C36 105.47(12) . . ? C35 Si2 C36 105.73(13) . . ? N1 Si2 Gd1 43.44(7) . . ? C34 Si2 Gd1 132.07(9) . . ? C35 Si2 Gd1 119.11(10) . . ? C36 Si2 Gd1 63.63(9) . . ? C6 C1 C2 120.6(3) . . ? C3 C2 C1 121.3(3) . . ? C2 C3 C4 118.4(3) . . ? C5 C4 C3 120.9(3) . . ? C4 C5 C6 120.8(3) . . ? C1 C6 C5 117.8(2) . . ? C1 C6 C7 120.9(2) . . ? C5 C6 C7 121.4(2) . . ? C15 C7 C8 108.2(2) . . ? C15 C7 C6 126.0(2) . . ? C8 C7 C6 125.8(2) . . ? C15 C7 Gd1 73.33(13) . . ? C8 C7 Gd1 74.87(13) . . ? C6 C7 Gd1 117.34(14) . . ? C9 C8 C7 108.3(2) . . ? C9 C8 Gd1 75.34(13) . . ? C7 C8 Gd1 74.80(13) . . ? C10 C9 C8 132.3(2) . . ? C10 C9 C14 120.0(2) . . ? C8 C9 C14 107.7(2) . . ? C10 C9 Gd1 118.63(16) . . ? C8 C9 Gd1 74.56(13) . . ? C14 C9 Gd1 74.20(12) . . ? C11 C10 C9 119.0(3) . . ? C10 C11 C12 121.5(3) . . ? C13 C12 C11 121.2(3) . . ? C12 C13 C14 119.9(3) . . ? C15 C14 C13 133.9(2) . . ? C15 C14 C9 107.6(2) . . ? C13 C14 C9 118.5(2) . . ? C15 C14 Gd1 73.34(13) . . ? C13 C14 Gd1 118.09(16) . . ? C9 C14 Gd1 75.11(13) . . ? C7 C15 C14 108.2(2) . . ? C7 C15 Gd1 76.23(13) . . ? C14 C15 Gd1 76.14(14) . . ? C17 C16 C21 121.1(3) . . ? C18 C17 C16 119.9(3) . . ? C17 C18 C19 120.1(3) . . ? C18 C19 C20 119.9(3) . . ? C19 C20 C21 120.7(3) . . ? C16 C21 C20 118.2(2) . . ? C16 C21 C22 122.0(2) . . ? C20 C21 C22 119.7(3) . . ? C23 C22 C30 108.7(2) . . ? C23 C22 C21 124.3(2) . . ? C30 C22 C21 126.6(2) . . ? C23 C22 Gd1 74.48(14) . . ? C30 C22 Gd1 75.76(14) . . ? C21 C22 Gd1 110.07(15) . . ? C22 C23 C24 108.6(2) . . ? C22 C23 Gd1 75.26(14) . . ? C24 C23 Gd1 77.30(14) . . ? C25 C24 C23 132.2(2) . . ? C25 C24 C29 120.4(2) . . ? C23 C24 C29 107.4(2) . . ? C25 C24 Gd1 118.78(17) . . ? C23 C24 Gd1 72.24(14) . . ? C29 C24 Gd1 75.95(13) . . ? C26 C25 C24 118.6(2) . . ? C25 C26 C27 121.1(3) . . ? C28 C27 C26 121.4(2) . . ? C27 C28 C29 119.2(2) . . ? C28 C29 C30 133.2(2) . . ? C28 C29 C24 119.2(2) . . ? C30 C29 C24 107.5(2) . . ? C28 C29 Gd1 121.39(17) . . ? C30 C29 Gd1 72.70(13) . . ? C24 C29 Gd1 73.92(13) . . ? C22 C30 C29 107.8(2) . . ? C22 C30 Gd1 73.80(14) . . ? C29 C30 Gd1 77.06(14) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 34.99 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 3.427 _refine_diff_density_min -3.172 _refine_diff_density_rms 0.135