# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Lappert, M.' _publ_contact_author_email m.f.lappert@sussex.ac.uk _publ_section_title ; Crystalline di- or trianionic metal (Al, Sm) \^I^2^-diketiminates ; _publ_requested_category FM loop_ _publ_author_name M.Lappert A.Protchenko P.Hitchcock M.Coles A.Khvostov # Attachment 'MFL-Dalton-feb2010[1].cif' data_(3)-may505 _database_code_depnum_ccdc_archive 'CCDC 768769' #TrackingRef 'MFL-Dalton-feb2010[1].cif' _audit_creation_date 2005-05-10T15:23:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C27 H45 Al K2 N2 O Si2' _chemical_formula_sum 'C27 H45 Al K2 N2 O Si2' _chemical_formula_weight 575.01 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.8525(7) _cell_length_b 14.1721(8) _cell_length_c 16.9078(7) _cell_angle_alpha 90 _cell_angle_beta 101.807(3) _cell_angle_gamma 90 _cell_volume 3249.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28710 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.414 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8677 _exptl_absorpt_correction_T_max 0.9984 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.37081E-1 _diffrn_orient_matrix_ub_12 0.14061E-1 _diffrn_orient_matrix_ub_13 -0.559635E-1 _diffrn_orient_matrix_ub_21 -0.627394E-1 _diffrn_orient_matrix_ub_22 0.41235E-2 _diffrn_orient_matrix_ub_23 0.203782E-1 _diffrn_orient_matrix_ub_31 0.113021E-1 _diffrn_orient_matrix_ub_32 0.690229E-1 _diffrn_orient_matrix_ub_33 0.101832E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_unetI/netI 0.0548 _diffrn_reflns_number 20825 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 6334 _reflns_number_gt 4600 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; For the two methyl groups, C22 and C23, showing short contacts to K the H atoms were refined; other H atopms were in riding mode. 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^)+(0.0331P)^2^+3.2269P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6334 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.081 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.1003 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.558 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.056 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Al Al -0.14137(6) -0.09041(6) 0.22639(5) 0.0290(2) Uani 1 1 d . . . K1 K 0.01589(5) -0.14594(5) 0.07749(3) 0.03411(17) Uani 1 1 d . . . K2 K -0.09037(5) 0.17520(5) 0.25638(4) 0.04385(19) Uani 1 1 d . . . Si1 Si 0.01873(6) -0.26222(6) 0.26059(5) 0.0344(2) Uani 1 1 d . A 1 Si2 Si -0.22618(5) -0.04549(6) 0.04305(4) 0.02953(19) Uani 1 1 d . A 1 O O 0.05267(19) 0.2752(2) 0.34563(15) 0.0716(8) Uani 1 1 d . B 1 N1 N -0.01498(16) -0.14608(16) 0.24406(12) 0.0275(5) Uani 1 1 d . A 1 N2 N -0.13938(15) -0.02318(16) 0.12939(12) 0.0276(5) Uani 1 1 d . A 1 C1 C 0.05253(18) -0.06889(19) 0.24975(14) 0.0251(6) Uani 1 1 d . A 1 C2 C 0.03334(18) 0.00791(19) 0.19917(14) 0.0240(6) Uani 1 1 d . A 1 H2 H 0.0856 0.0525 0.2063 0.029 Uiso 1 1 calc R A 1 C3 C -0.05026(18) 0.03397(19) 0.13758(14) 0.0241(6) Uani 1 1 d . A 1 C4 C 0.13469(19) -0.06127(18) 0.32081(15) 0.0269(6) Uani 1 1 d . A 1 C5 C 0.2248(2) -0.0188(2) 0.31726(17) 0.0344(7) Uani 1 1 d . A 1 H5 H 0.2363 0.0015 0.2664 0.041 Uiso 1 1 calc R A 1 C6 C 0.2977(2) -0.0056(2) 0.38570(18) 0.0423(8) Uani 1 1 d . A 1 H6 H 0.3578 0.0244 0.3814 0.051 Uiso 1 1 calc R A 1 C7 C 0.2837(2) -0.0357(2) 0.46036(18) 0.0431(8) Uani 1 1 d . A 1 H7 H 0.3337 -0.0269 0.5074 0.052 Uiso 1 1 calc R A 1 C8 C 0.1962(2) -0.0788(2) 0.46515(17) 0.0421(8) Uani 1 1 d . A 1 H8 H 0.1859 -0.0995 0.5162 0.051 Uiso 1 1 calc R A 1 C9 C 0.1226(2) -0.0925(2) 0.39701(15) 0.0331(6) Uani 1 1 d . A 1 H9 H 0.0633 -0.1235 0.4019 0.04 Uiso 1 1 calc R A 1 C10 C -0.05068(19) 0.12596(19) 0.10344(14) 0.0257(6) Uani 1 1 d . . 1 C11 C 0.0386(2) 0.18059(19) 0.10605(15) 0.0292(6) Uani 1 1 d . . 1 H11 H 0.1003 0.1525 0.1289 0.035 Uiso 1 1 calc R . 1 C12 C 0.0378(2) 0.2710(2) 0.07688(16) 0.0362(7) Uani 1 1 d . . 1 H12 H 0.0987 0.3033 0.0806 0.043 Uiso 1 1 calc R . 1 C13 C -0.0490(3) 0.3169(2) 0.04211(18) 0.0448(8) Uani 1 1 d . . 1 H13 H -0.0484 0.3784 0.0199 0.054 Uiso 1 1 calc R . 1 C14 C -0.1371(2) 0.2689(2) 0.04104(17) 0.0415(8) Uani 1 1 d . . 1 H14 H -0.1977 0.2998 0.0198 0.05 Uiso 1 1 calc R . 1 C15 C -0.1390(2) 0.1779(2) 0.06980(16) 0.0335(7) Uani 1 1 d . . 1 H15 H -0.2011 0.1483 0.0673 0.04 Uiso 1 1 calc R . 1 C16 C 0.1534(2) -0.2809(2) 0.2640(2) 0.0531(9) Uani 1 1 d . A 1 H16C H 0.192 -0.2495 0.3119 0.08 Uiso 1 1 calc R A 1 H16B H 0.1708 -0.2543 0.2153 0.08 Uiso 1 1 calc R A 1 H16A H 0.1679 -0.3486 0.2667 0.08 Uiso 1 1 calc R A 1 C17 C -0.0136(3) -0.3130(3) 0.3539(2) 0.0593(10) Uani 1 1 d . A 1 H17C H 0.001 -0.3807 0.3566 0.089 Uiso 1 1 calc R A 1 H17B H -0.0839 -0.3033 0.3524 0.089 Uiso 1 1 calc R A 1 H17A H 0.0253 -0.2816 0.4016 0.089 Uiso 1 1 calc R A 1 C18 C -0.0483(3) -0.3373(2) 0.1741(2) 0.0536(9) Uani 1 1 d . A 1 H18C H -0.0302 -0.3169 0.1237 0.08 Uiso 1 1 calc R A 1 H18B H -0.1197 -0.3304 0.1694 0.08 Uiso 1 1 calc R A 1 H18A H -0.0299 -0.4036 0.1844 0.08 Uiso 1 1 calc R A 1 C19 C -0.2447(2) -0.1749(2) 0.02161(18) 0.0421(8) Uani 1 1 d . A 1 H19C H -0.2698 -0.205 0.0656 0.063 Uiso 1 1 calc R A 1 H19B H -0.1816 -0.2038 0.0174 0.063 Uiso 1 1 calc R A 1 H19A H -0.2922 -0.1836 -0.0294 0.063 Uiso 1 1 calc R A 1 C20 C -0.3514(2) -0.0007(3) 0.04943(19) 0.0469(8) Uani 1 1 d . A 1 H20C H -0.3504 0.0684 0.0511 0.07 Uiso 1 1 calc R A 1 H20B H -0.3697 -0.0251 0.0985 0.07 Uiso 1 1 calc R A 1 H20A H -0.3996 -0.0219 0.002 0.07 Uiso 1 1 calc R A 1 C21 C -0.1925(2) 0.0023(2) -0.05142(15) 0.0344(7) Uani 1 1 d . . 1 H21C H -0.2411 -0.019 -0.0986 0.052 Uiso 1 1 calc R . 1 H21B H -0.127 -0.0207 -0.0554 0.052 Uiso 1 1 calc R . 1 H21A H -0.1919 0.0714 -0.0495 0.052 Uiso 1 1 calc R . 1 C22 C -0.1532(3) -0.0092(3) 0.3199(2) 0.0459(8) Uani 1 1 d . B 1 H22C H -0.172(3) -0.047(3) 0.359(2) 0.062(11) Uiso 1 1 d . C 1 H22B H -0.202(3) 0.040(3) 0.307(2) 0.067(12) Uiso 1 1 d . D 1 H22A H -0.094(3) 0.028(3) 0.350(2) 0.070(12) Uiso 1 1 d . E 1 C23 C -0.2483(3) -0.1855(3) 0.2216(2) 0.0440(8) Uani 1 1 d . . 1 H23C H -0.311(3) -0.165(3) 0.198(2) 0.077(13) Uiso 1 1 d . F 1 H23A H -0.244(2) -0.207(3) 0.276(2) 0.063(11) Uiso 1 1 d . G 1 H23B H -0.243(3) -0.241(3) 0.194(2) 0.069(13) Uiso 1 1 d . H 1 C24 C 0.1115(5) 0.2368(6) 0.4140(4) 0.170(4) Uani 1 1 d . B 1 H24B H 0.1305 0.2878 0.4541 0.204 Uiso 1 1 calc R B 1 H24A H 0.1727 0.213 0.3993 0.204 Uiso 1 1 calc R B 1 C25 C 0.0694(4) 0.1635(3) 0.4508(3) 0.0944(16) Uani 1 1 d . B 1 H25C H 0.0099 0.1864 0.4674 0.142 Uiso 1 1 calc R B 1 H25B H 0.1169 0.1413 0.4984 0.142 Uiso 1 1 calc R B 1 H25A H 0.0521 0.1114 0.4124 0.142 Uiso 1 1 calc R B 1 C26 C 0.0939(4) 0.3576(5) 0.3173(4) 0.134(2) Uani 1 1 d . B 1 H26B H 0.1204 0.3987 0.3641 0.161 Uiso 1 1 calc R B 1 H26A H 0.1497 0.3388 0.2924 0.161 Uiso 1 1 calc R B 1 C27 C 0.0265(4) 0.4093(4) 0.2611(4) 0.1048(18) Uani 1 1 d . B 1 H27C H -0.0003 0.3692 0.2146 0.157 Uiso 1 1 calc R B 1 H27B H 0.0599 0.4638 0.2431 0.157 Uiso 1 1 calc R B 1 H27A H -0.0272 0.4312 0.2862 0.157 Uiso 1 1 calc R B 1 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 Al 0.0299(4) 0.0299(5) 0.0283(4) 0.0011(4) 0.0085(3) -0.0037(4) K1 0.0436(4) 0.0310(4) 0.0285(3) -0.0021(3) 0.0092(3) 0.0019(3) K2 0.0499(4) 0.0435(4) 0.0394(4) -0.0090(3) 0.0120(3) 0.0120(3) Si1 0.0440(5) 0.0237(4) 0.0343(4) 0.0045(3) 0.0051(4) -0.0007(4) Si2 0.0247(4) 0.0340(5) 0.0291(4) -0.0023(3) 0.0037(3) 0.0004(3) O 0.0593(16) 0.080(2) 0.0655(16) 0.0203(15) -0.0093(13) -0.0143(15) N1 0.0314(12) 0.0231(13) 0.0281(11) 0.0023(10) 0.0062(10) -0.0040(10) N2 0.0242(11) 0.0312(14) 0.0268(11) 0.0028(10) 0.0036(9) -0.0032(10) C1 0.0276(13) 0.0231(15) 0.0246(13) 0.0000(11) 0.0053(11) -0.0003(11) C2 0.0249(13) 0.0241(15) 0.0239(13) -0.0017(11) 0.0070(11) -0.0033(11) C3 0.0252(13) 0.0247(15) 0.0225(12) -0.0027(11) 0.0052(10) 0.0034(11) C4 0.0330(14) 0.0194(15) 0.0271(13) -0.0010(11) 0.0038(11) 0.0030(12) C5 0.0350(15) 0.0342(18) 0.0324(15) 0.0041(13) 0.0035(12) -0.0001(13) C6 0.0342(16) 0.042(2) 0.0446(18) 0.0037(15) -0.0064(14) -0.0029(14) C7 0.0471(19) 0.0360(19) 0.0384(17) -0.0028(14) -0.0095(14) 0.0039(15) C8 0.062(2) 0.0360(19) 0.0251(14) 0.0011(13) 0.0024(14) 0.0029(16) C9 0.0433(16) 0.0278(16) 0.0275(14) 0.0012(12) 0.0060(12) -0.0022(14) C10 0.0319(14) 0.0240(15) 0.0205(12) -0.0026(11) 0.0040(11) 0.0055(12) C11 0.0358(15) 0.0255(16) 0.0261(13) 0.0015(12) 0.0059(12) 0.0028(12) C12 0.0517(18) 0.0246(16) 0.0311(15) -0.0017(13) 0.0055(14) -0.0012(14) C13 0.070(2) 0.0190(16) 0.0405(17) 0.0034(14) 0.0003(16) 0.0029(16) C14 0.0526(19) 0.0282(18) 0.0369(16) -0.0009(14) -0.0066(14) 0.0163(15) C15 0.0366(16) 0.0319(17) 0.0289(14) -0.0025(13) -0.0008(12) 0.0081(13) C16 0.052(2) 0.037(2) 0.069(2) -0.0019(18) 0.0107(18) 0.0110(17) C17 0.084(3) 0.041(2) 0.053(2) 0.0170(17) 0.0153(19) -0.006(2) C18 0.069(2) 0.0302(19) 0.056(2) -0.0024(16) 0.0002(18) -0.0021(17) C19 0.0431(17) 0.042(2) 0.0391(16) -0.0061(15) 0.0037(14) -0.0088(15) C20 0.0305(15) 0.061(2) 0.0489(18) -0.0076(17) 0.0071(14) 0.0032(16) C21 0.0361(15) 0.0370(18) 0.0284(14) -0.0031(13) 0.0025(12) 0.0040(14) C22 0.057(2) 0.044(2) 0.0412(19) -0.0048(17) 0.0201(17) -0.0011(19) C23 0.0390(19) 0.050(2) 0.0435(19) 0.0056(18) 0.0094(16) -0.0146(17) C24 0.115(5) 0.220(8) 0.136(5) 0.092(6) -0.067(4) -0.047(5) C25 0.097(4) 0.074(3) 0.099(4) 0.032(3) -0.009(3) 0.001(3) C26 0.097(4) 0.137(6) 0.155(6) 0.041(5) -0.007(4) -0.064(4) C27 0.136(5) 0.064(3) 0.136(5) 0.019(3) 0.080(4) 0.002(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Al N1 1.888(2) . ? Al N2 1.902(2) . ? Al C22 1.990(3) . ? Al C23 1.992(3) . ? K1 N1 2.934(2) . ? K1 C3 2.959(3) . ? K1 C2 2.973(3) . ? K1 N2 3.033(2) . ? K1 C1 3.054(2) . ? K1 C11 3.079(3) 3 ? K1 C12 3.117(3) 3 ? K1 C10 3.205(2) 3 ? K1 C13 3.248(3) 3 ? K1 C21 3.282(3) 3 ? K1 C15 3.325(3) 3 ? K2 O 2.644(3) . ? K2 C10 2.839(2) . ? K2 C3 2.968(3) . ? K2 C22 3.021(4) . ? K2 C23 3.061(3) 2_455 ? K2 C15 3.088(3) . ? K2 C2 3.189(3) . ? K2 H22B 2.72(4) . ? K2 H22A 2.62(4) . ? Si1 N1 1.718(2) . ? Si1 C17 1.870(3) . ? Si1 C16 1.874(3) . ? Si1 C18 1.892(3) . ? Si2 N2 1.720(2) . ? Si2 C20 1.870(3) . ? Si2 C19 1.877(3) . ? Si2 C21 1.879(3) . ? O C24 1.382(5) . ? O C26 1.425(6) . ? N1 C1 1.430(3) . ? N2 C3 1.459(3) . ? C1 C2 1.376(4) . ? C1 C4 1.480(3) . ? C2 C3 1.438(3) . ? C2 H2 0.95 . ? C3 C10 1.425(4) . ? C4 C5 1.398(4) . ? C4 C9 1.404(4) . ? C5 C6 1.384(4) . ? C5 H5 0.95 . ? C6 C7 1.383(4) . ? C6 H6 0.95 . ? C7 C8 1.374(4) . ? C7 H7 0.95 . ? C8 C9 1.387(4) . ? C8 H8 0.95 . ? C9 H9 0.95 . ? C10 C15 1.442(4) . ? C10 C11 1.452(4) . ? C10 K1 3.205(2) 3 ? C11 C12 1.372(4) . ? C11 K1 3.079(3) 3 ? C11 H11 0.95 . ? C12 C13 1.387(4) . ? C12 K1 3.117(3) 3 ? C12 H12 0.95 . ? C13 C14 1.394(4) . ? C13 K1 3.248(3) 3 ? C13 H13 0.95 . ? C14 C15 1.381(4) . ? C14 K1 3.353(3) 3 ? C14 H14 0.95 . ? C15 K1 3.325(3) 3 ? C15 H15 0.95 . ? C16 H16C 0.98 . ? C16 H16B 0.98 . ? C16 H16A 0.98 . ? C17 H17C 0.98 . ? C17 H17B 0.98 . ? C17 H17A 0.98 . ? C18 H18C 0.98 . ? C18 H18B 0.98 . ? C18 H18A 0.98 . ? C19 H19C 0.98 . ? C19 H19B 0.98 . ? C19 H19A 0.98 . ? C20 H20C 0.98 . ? C20 H20B 0.98 . ? C20 H20A 0.98 . ? C21 K1 3.282(3) 3 ? C21 H21C 0.98 . ? C21 H21B 0.98 . ? C21 H21A 0.98 . ? C22 H22C 0.93(4) . ? C22 H22B 0.96(4) . ? C22 H22A 1.01(4) . ? C23 K2 3.061(3) 2_445 ? C23 H23C 0.93(4) . ? C23 H23A 0.96(4) . ? C23 H23B 0.93(4) . ? C24 C25 1.398(7) . ? C24 H24B 0.99 . ? C24 H24A 0.99 . ? C25 H25C 0.98 . ? C25 H25B 0.98 . ? C25 H25A 0.98 . ? C26 C27 1.395(7) . ? C26 H26B 0.99 . ? C26 H26A 0.99 . ? C27 H27C 0.98 . ? C27 H27B 0.98 . ? C27 H27A 0.98 . ? 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 Al N2 99.75(10) . . ? N1 Al C22 109.92(14) . . ? N2 Al C22 114.44(14) . . ? N1 Al C23 112.42(15) . . ? N2 Al C23 116.46(13) . . ? C22 Al C23 104.03(17) . . ? N1 K1 C3 63.56(7) . . ? N1 K1 C2 48.97(6) . . ? C3 K1 C2 28.06(7) . . ? N1 K1 N2 58.08(6) . . ? C3 K1 N2 28.16(6) . . ? C2 K1 N2 48.79(6) . . ? N1 K1 C1 27.53(6) . . ? C3 K1 C1 50.74(7) . . ? C2 K1 C1 26.35(7) . . ? N2 K1 C1 60.54(6) . . ? N1 K1 C11 155.98(7) . 3 ? C3 K1 C11 117.01(7) . 3 ? C2 K1 C11 141.50(7) . 3 ? N2 K1 C11 109.93(7) . 3 ? C1 K1 C11 167.60(7) . 3 ? N1 K1 C12 138.31(7) . 3 ? C3 K1 C12 137.73(7) . 3 ? C2 K1 C12 165.50(7) . 3 ? N2 K1 C12 120.44(7) . 3 ? C1 K1 C12 165.15(8) . 3 ? C11 K1 C12 25.58(7) 3 3 ? N1 K1 C10 174.96(7) . 3 ? C3 K1 C10 111.67(7) . 3 ? C2 K1 C10 126.07(7) . 3 ? N2 K1 C10 118.66(6) . 3 ? C1 K1 C10 148.26(7) . 3 ? C11 K1 C10 26.63(7) 3 3 ? C12 K1 C10 46.19(7) 3 3 ? N1 K1 C13 131.61(7) . 3 ? C3 K1 C13 161.76(7) . 3 ? C2 K1 C13 167.41(8) . 3 ? N2 K1 C13 143.80(7) . 3 ? C1 K1 C13 147.50(7) . 3 ? C11 K1 C13 44.79(7) 3 3 ? C12 K1 C13 25.07(7) 3 3 ? C10 K1 C13 53.40(7) 3 3 ? N1 K1 C21 112.86(6) . 3 ? C3 K1 C21 78.65(7) . 3 ? C2 K1 C21 71.38(7) . 3 ? N2 K1 C21 105.99(7) . 3 ? C1 K1 C21 85.60(7) . 3 ? C11 K1 C21 89.97(7) 3 3 ? C12 K1 C21 107.29(7) 3 3 ? C10 K1 C21 63.59(7) 3 3 ? C13 K1 C21 100.09(8) 3 3 ? N1 K1 C15 156.46(7) . 3 ? C3 K1 C15 128.10(7) . 3 ? C2 K1 C15 129.54(7) . 3 ? N2 K1 C15 142.93(6) . 3 ? C1 K1 C15 138.79(7) . 3 ? C11 K1 C15 44.04(7) 3 3 ? C12 K1 C15 50.69(8) 3 3 ? C10 K1 C15 25.42(6) 3 3 ? C13 K1 C15 43.34(8) 3 3 ? C21 K1 C15 58.20(7) 3 3 ? O K2 C10 112.93(9) . . ? O K2 C3 121.72(8) . . ? C10 K2 C3 28.31(7) . . ? O K2 C22 119.86(9) . . ? C10 K2 C22 103.59(9) . . ? C3 K2 C22 76.40(8) . . ? O K2 C23 93.75(10) . 2_455 ? C10 K2 C23 123.49(9) . 2_455 ? C3 K2 C23 139.44(9) . 2_455 ? C22 K2 C23 104.10(11) . 2_455 ? O K2 C15 123.91(9) . . ? C10 K2 C15 27.75(7) . . ? C3 K2 C15 49.37(7) . . ? C22 K2 C15 110.82(9) . . ? C23 K2 C15 95.98(9) 2_455 . ? O K2 C2 100.68(8) . . ? C10 K2 C2 47.52(7) . . ? C3 K2 C2 26.71(6) . . ? C22 K2 C2 71.14(8) . . ? C23 K2 C2 165.29(9) 2_455 . ? C15 K2 C2 73.61(7) . . ? O K2 H22B 127.4(7) . . ? C10 K2 H22B 110.2(8) . . ? C3 K2 H22B 86.3(8) . . ? C22 K2 H22B 18.4(8) . . ? C23 K2 H22B 86.5(9) 2_455 . ? C15 K2 H22B 108.3(7) . . ? C2 K2 H22B 87.0(8) . . ? O K2 H22A 100.9(9) . . ? C10 K2 H22A 112.6(8) . . ? C3 K2 H22A 84.3(8) . . ? C22 K2 H22A 19.1(8) . . ? C23 K2 H22A 109.5(8) 2_455 . ? C15 K2 H22A 126.7(8) . . ? C2 K2 H22A 70.7(8) . . ? H22B K2 H22A 33.2(10) . . ? N1 Si1 C17 113.70(15) . . ? N1 Si1 C16 112.09(14) . . ? C17 Si1 C16 109.15(17) . . ? N1 Si1 C18 109.83(13) . . ? C17 Si1 C18 105.75(17) . . ? C16 Si1 C18 105.84(16) . . ? N2 Si2 C20 112.58(13) . . ? N2 Si2 C19 112.80(13) . . ? C20 Si2 C19 104.56(15) . . ? N2 Si2 C21 113.78(12) . . ? C20 Si2 C21 108.73(14) . . ? C19 Si2 C21 103.62(14) . . ? C24 O C26 113.3(4) . . ? C24 O K2 120.7(3) . . ? C26 O K2 123.6(3) . . ? C1 N1 Si1 124.75(18) . . ? C1 N1 Al 105.28(16) . . ? Si1 N1 Al 129.69(13) . . ? C1 N1 K1 80.92(13) . . ? Si1 N1 K1 93.94(9) . . ? Al N1 K1 99.23(8) . . ? C3 N2 Si2 127.83(17) . . ? C3 N2 Al 110.95(15) . . ? Si2 N2 Al 120.59(12) . . ? C3 N2 K1 73.11(13) . . ? Si2 N2 K1 93.61(9) . . ? Al N2 K1 95.65(9) . . ? C2 C1 N1 121.5(2) . . ? C2 C1 C4 117.7(2) . . ? N1 C1 C4 119.6(2) . . ? C2 C1 K1 73.55(14) . . ? N1 C1 K1 71.55(13) . . ? C4 C1 K1 138.62(17) . . ? C1 C2 C3 132.7(2) . . ? C1 C2 K1 80.10(15) . . ? C3 C2 K1 75.40(14) . . ? C1 C2 K2 116.55(16) . . ? C3 C2 K2 68.02(14) . . ? K1 C2 K2 141.47(9) . . ? C1 C2 H2 113.7 . . ? C3 C2 H2 113.7 . . ? K1 C2 H2 121.9 . . ? K2 C2 H2 84.8 . . ? C10 C3 C2 117.6(2) . . ? C10 C3 N2 122.4(2) . . ? C2 C3 N2 117.8(2) . . ? C10 C3 K1 128.69(16) . . ? C2 C3 K1 76.54(14) . . ? N2 C3 K1 78.73(14) . . ? C10 C3 K2 70.82(14) . . ? C2 C3 K2 85.27(14) . . ? N2 C3 K2 99.59(14) . . ? K1 C3 K2 158.08(10) . . ? C5 C4 C9 116.8(2) . . ? C5 C4 C1 122.8(2) . . ? C9 C4 C1 120.4(2) . . ? C6 C5 C4 121.8(3) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C7 C6 C5 120.4(3) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 C6 118.7(3) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 C8 C9 121.4(3) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 120.8(3) . . ? C8 C9 H9 119.6 . . ? C4 C9 H9 119.6 . . ? C3 C10 C15 124.0(2) . . ? C3 C10 C11 122.9(2) . . ? C15 C10 C11 112.9(2) . . ? C3 C10 K2 80.88(14) . . ? C15 C10 K2 85.80(15) . . ? C11 C10 K2 99.43(15) . . ? C3 C10 K1 118.58(16) . 3 ? C15 C10 K1 81.93(15) . 3 ? C11 C10 K1 71.85(14) . 3 ? K2 C10 K1 160.50(10) . 3 ? C12 C11 C10 122.9(3) . . ? C12 C11 K1 78.73(15) . 3 ? C10 C11 K1 81.53(14) . 3 ? C12 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? K1 C11 H11 111 3 . ? C11 C12 C13 122.2(3) . . ? C11 C12 K1 75.69(16) . 3 ? C13 C12 K1 82.75(17) . 3 ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? K1 C12 H12 112.7 3 . ? C12 C13 C14 117.2(3) . . ? C12 C13 K1 72.17(17) . 3 ? C14 C13 K1 82.10(18) . 3 ? C12 C13 H13 121.4 . . ? C14 C13 H13 121.4 . . ? K1 C13 H13 115.2 3 . ? C15 C14 C13 122.1(3) . . ? C15 C14 K1 76.91(17) . 3 ? C13 C14 K1 73.59(18) . 3 ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? K1 C14 H14 121.7 3 . ? C14 C15 C10 122.6(3) . . ? C14 C15 K2 110.82(18) . . ? C10 C15 K2 66.45(13) . . ? C14 C15 K1 79.23(18) . 3 ? C10 C15 K1 72.64(15) . 3 ? K2 C15 K1 136.48(9) . 3 ? C14 C15 H15 118.7 . . ? C10 C15 H15 118.7 . . ? K2 C15 H15 92.6 . . ? K1 C15 H15 120.4 3 . ? Si1 C16 H16C 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? Si1 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? Si1 C17 H17C 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? Si1 C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? Si1 C18 H18C 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18C C18 H18B 109.5 . . ? Si1 C18 H18A 109.5 . . ? H18C C18 H18A 109.5 . . ? H18B C18 H18A 109.5 . . ? Si2 C19 H19C 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? Si2 C19 H19A 109.5 . . ? H19C C19 H19A 109.5 . . ? H19B C19 H19A 109.5 . . ? Si2 C20 H20C 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20C C20 H20B 109.5 . . ? Si2 C20 H20A 109.5 . . ? H20C C20 H20A 109.5 . . ? H20B C20 H20A 109.5 . . ? Si2 C21 K1 131.23(12) . 3 ? Si2 C21 H21C 109.5 . . ? K1 C21 H21C 119.2 3 . ? Si2 C21 H21B 109.5 . . ? K1 C21 H21B 58 3 . ? H21C C21 H21B 109.5 . . ? Si2 C21 H21A 109.5 . . ? K1 C21 H21A 51.9 3 . ? H21C C21 H21A 109.5 . . ? H21B C21 H21A 109.5 . . ? Al C22 K2 98.11(14) . . ? Al C22 H22C 108(2) . . ? K2 C22 H22C 154(2) . . ? Al C22 H22B 114(2) . . ? K2 C22 H22B 63(2) . . ? H22C C22 H22B 107(3) . . ? Al C22 H22A 120(2) . . ? K2 C22 H22A 58(2) . . ? H22C C22 H22A 105(3) . . ? H22B C22 H22A 101(3) . . ? Al C23 K2 170.61(19) . 2_445 ? Al C23 H23C 115(2) . . ? K2 C23 H23C 67(2) 2_445 . ? Al C23 H23A 106(2) . . ? K2 C23 H23A 66(2) 2_445 . ? H23C C23 H23A 113(3) . . ? Al C23 H23B 118(2) . . ? K2 C23 H23B 69(2) 2_445 . ? H23C C23 H23B 102(3) . . ? H23A C23 H23B 102(3) . . ? O C24 C25 115.9(5) . . ? O C24 H24B 108.3 . . ? C25 C24 H24B 108.3 . . ? O C24 H24A 108.3 . . ? C25 C24 H24A 108.3 . . ? H24B C24 H24A 107.4 . . ? C24 C25 H25C 109.5 . . ? C24 C25 H25B 109.5 . . ? H25C C25 H25B 109.5 . . ? C24 C25 H25A 109.5 . . ? H25C C25 H25A 109.5 . . ? H25B C25 H25A 109.5 . . ? C27 C26 O 113.6(4) . . ? C27 C26 H26B 108.8 . . ? O C26 H26B 108.8 . . ? C27 C26 H26A 108.8 . . ? O C26 H26A 108.8 . . ? H26B C26 H26A 107.7 . . ? C26 C27 H27C 109.5 . . ? C26 C27 H27B 109.5 . . ? H27C C27 H27B 109.5 . . ? C26 C27 H27A 109.5 . . ? H27C C27 H27A 109.5 . . ? H27B C27 H27A 109.5 . . ? #===END data_(4)-nov1500 _database_code_depnum_ccdc_archive 'CCDC 768770' #TrackingRef 'MFL-Dalton-feb2010[1].cif' _audit_creation_date 2000-11-16T09:59:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ((KSm(Me3SiCPhCHCPhNSiMe3)2)2) _chemical_formula_moiety 'C42 H58 K N4 Si4 Sm' _chemical_formula_structural 'C42 H58 K N4 Si4 Sm' _chemical_formula_sum 'C42 H58 K N4 Si4 Sm' _chemical_formula_weight 920.74 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.0232(5) _cell_length_b 20.0158(5) _cell_length_c 17.9052(7) _cell_angle_alpha 90 _cell_angle_beta 94.925(2) _cell_angle_gamma 90 _cell_volume 4650.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19687 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.487 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_T_max 0.754 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 27295 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_unetI/netI 0.063 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 8199 _reflns_number_gt 6183 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The Si2 Me3Si group refined poorly and distance(SADI) and DELU constraints were applied to it. 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^)+(0.0354P)^2^+2.4694P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8199 _refine_ls_number_parameters 477 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.089 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.709 _refine_diff_density_min -0.867 _refine_diff_density_rms 0.086 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Sm Sm -0.005560(17) 0.237942(10) 0.087192(12) 0.02925(8) Uani 1 1 d . . . K K 0.03235(8) 0.03655(4) 0.12713(5) 0.0397(2) Uani 1 1 d . . . Si1 Si -0.20767(11) 0.36260(7) 0.13769(9) 0.0511(4) Uani 1 1 d . . . Si2 Si 0.05521(14) 0.34322(8) -0.07762(8) 0.0618(4) Uani 1 1 d DU . . Si3 Si 0.11360(10) 0.15223(6) 0.26300(7) 0.0379(3) Uani 1 1 d . . . Si4 Si -0.20118(9) 0.10646(6) 0.04483(7) 0.0375(3) Uani 1 1 d . . . N1 N -0.0802(3) 0.33665(16) 0.13781(19) 0.0348(8) Uani 1 1 d . . . N2 N 0.0688(3) 0.32489(16) 0.01778(19) 0.0353(8) Uani 1 1 d . . . N3 N 0.0879(3) 0.16776(15) 0.16974(18) 0.0303(8) Uani 1 1 d . . . N4 N -0.0819(3) 0.13941(16) 0.04475(18) 0.0331(8) Uani 1 1 d . . . C1 C 0.0052(3) 0.36146(18) 0.1742(2) 0.0324(10) Uani 1 1 d . . . C2 C 0.1047(4) 0.35698(19) 0.1475(2) 0.0322(10) Uani 1 1 d . . . H2 H 0.160(3) 0.3673(17) 0.180(2) 0.025(10) Uiso 1 1 d . . . C3 C 0.1312(3) 0.35092(19) 0.0724(2) 0.0322(10) Uani 1 1 d . . . C4 C 0.0006(3) 0.3955(2) 0.2485(2) 0.0396(11) Uani 1 1 d . . . C5 C 0.0509(4) 0.4552(2) 0.2643(3) 0.0544(13) Uani 1 1 d . . . H5 H 0.0917 0.4742 0.2282 0.065 Uiso 1 1 calc R . . C6 C 0.0431(5) 0.4880(3) 0.3320(4) 0.083(2) Uani 1 1 d . . . H6 H 0.0775 0.5293 0.342 0.099 Uiso 1 1 calc R . . C7 C -0.0153(6) 0.4598(4) 0.3842(4) 0.092(2) Uani 1 1 d . . . H7 H -0.0219 0.4821 0.4304 0.111 Uiso 1 1 calc R . . C8 C -0.0644(5) 0.3996(4) 0.3702(3) 0.0789(19) Uani 1 1 d . . . H8 H -0.1036 0.3802 0.407 0.095 Uiso 1 1 calc R . . C9 C -0.0566(4) 0.3674(3) 0.3027(3) 0.0570(14) Uani 1 1 d . . . H9 H -0.0904 0.3258 0.2932 0.068 Uiso 1 1 calc R . . C10 C 0.2355(3) 0.3761(2) 0.0586(2) 0.0345(10) Uani 1 1 d . . . C11 C 0.2662(4) 0.4407(2) 0.0770(3) 0.0427(11) Uani 1 1 d . . . H11 H 0.2201 0.4699 0.0993 0.051 Uiso 1 1 calc R . . C12 C 0.3642(4) 0.4634(3) 0.0632(3) 0.0547(14) Uani 1 1 d . . . H12 H 0.3842 0.508 0.0751 0.066 Uiso 1 1 calc R . . C13 C 0.4315(4) 0.4209(3) 0.0324(3) 0.0571(14) Uani 1 1 d . . . H13 H 0.4981 0.4363 0.0228 0.068 Uiso 1 1 calc R . . C14 C 0.4035(4) 0.3567(3) 0.0155(3) 0.0602(15) Uani 1 1 d . . . H14 H 0.4512 0.3273 -0.0046 0.072 Uiso 1 1 calc R . . C15 C 0.3055(4) 0.3340(2) 0.0277(3) 0.0475(12) Uani 1 1 d . . . H15 H 0.2862 0.2895 0.0148 0.057 Uiso 1 1 calc R . . C16 C -0.2252(4) 0.4484(2) 0.1739(4) 0.0694(17) Uani 1 1 d . . . H16C H -0.2984 0.4603 0.1678 0.104 Uiso 1 1 calc R . . H16B H -0.1858 0.4801 0.1459 0.104 Uiso 1 1 calc R . . H16A H -0.2006 0.4502 0.2272 0.104 Uiso 1 1 calc R . . C17 C -0.2829(4) 0.3016(3) 0.1889(4) 0.080(2) Uani 1 1 d . . . H17C H -0.2593 0.3026 0.2423 0.12 Uiso 1 1 calc R . . H17B H -0.273 0.2566 0.169 0.12 Uiso 1 1 calc R . . H17A H -0.3562 0.3133 0.1823 0.12 Uiso 1 1 calc R . . C18 C -0.2567(5) 0.3629(4) 0.0366(4) 0.096(2) Uani 1 1 d . . . H18C H -0.249 0.3183 0.0155 0.144 Uiso 1 1 calc R . . H18B H -0.2172 0.3952 0.0095 0.144 Uiso 1 1 calc R . . H18A H -0.3297 0.3756 0.0319 0.144 Uiso 1 1 calc R . . C19 C 0.0386(8) 0.4347(3) -0.0861(4) 0.173(4) Uani 1 1 d DU . . H19A H -0.0174 0.4491 -0.0566 0.26 Uiso 1 1 calc R . . H19B H 0.0219 0.4466 -0.1388 0.26 Uiso 1 1 calc R . . H19C H 0.1027 0.457 -0.0673 0.26 Uiso 1 1 calc R . . C20 C -0.0654(4) 0.3017(3) -0.1128(3) 0.0712(16) Uani 1 1 d DU . . H20A H -0.1217 0.3171 -0.0842 0.107 Uiso 1 1 calc R . . H20B H -0.0576 0.2532 -0.1071 0.107 Uiso 1 1 calc R . . H20C H -0.0812 0.3126 -0.1659 0.107 Uiso 1 1 calc R . . C21 C 0.1587(6) 0.3128(6) -0.1324(4) 0.204(5) Uani 1 1 d DU . . H21A H 0.165 0.2642 -0.1267 0.305 Uiso 1 1 calc R . . H21B H 0.2239 0.334 -0.1142 0.305 Uiso 1 1 calc R . . H21C H 0.1423 0.3239 -0.1854 0.305 Uiso 1 1 calc R . . C22 C 0.1501(3) 0.15992(18) 0.1088(2) 0.0289(9) Uani 1 1 d . . . C23 C 0.1077(3) 0.14381(18) 0.0355(2) 0.0274(9) Uani 1 1 d . . . H23 H 0.152(3) 0.1492(16) 0.002(2) 0.018(10) Uiso 1 1 d . . . C24 C 0.0042(3) 0.13409(18) 0.0008(2) 0.0294(9) Uani 1 1 d . . . C25 C 0.2624(3) 0.17383(18) 0.1177(2) 0.0298(9) Uani 1 1 d . . . C26 C 0.3320(3) 0.1410(2) 0.0757(3) 0.0406(11) Uani 1 1 d . . . H26 H 0.3067 0.1088 0.0397 0.049 Uiso 1 1 calc R . . C27 C 0.4361(4) 0.1537(2) 0.0844(3) 0.0517(13) Uani 1 1 d . . . H27 H 0.4811 0.1309 0.054 0.062 Uiso 1 1 calc R . . C28 C 0.4757(4) 0.1992(2) 0.1369(3) 0.0501(13) Uani 1 1 d . . . H28 H 0.5477 0.2077 0.1431 0.06 Uiso 1 1 calc R . . C29 C 0.4100(4) 0.2320(2) 0.1797(3) 0.0439(12) Uani 1 1 d . . . H29 H 0.4367 0.2634 0.2162 0.053 Uiso 1 1 calc R . . C30 C 0.3051(3) 0.2200(2) 0.1706(2) 0.0374(10) Uani 1 1 d . . . H30 H 0.2609 0.2435 0.201 0.045 Uiso 1 1 calc R . . C31 C -0.0078(3) 0.12129(18) -0.0799(2) 0.0301(10) Uani 1 1 d . . . C32 C 0.0742(4) 0.1046(2) -0.1235(2) 0.0405(11) Uani 1 1 d . . . H32 H 0.1422 0.103 -0.0998 0.049 Uiso 1 1 calc R . . C33 C 0.0591(4) 0.0904(2) -0.1998(3) 0.0498(13) Uani 1 1 d . . . H33 H 0.1166 0.0796 -0.2267 0.06 Uiso 1 1 calc R . . C34 C -0.0383(5) 0.0919(2) -0.2368(3) 0.0531(14) Uani 1 1 d . . . H34 H -0.0487 0.0816 -0.2887 0.064 Uiso 1 1 calc R . . C35 C -0.1198(4) 0.1086(2) -0.1966(3) 0.0511(13) Uani 1 1 d . . . H35 H -0.1873 0.1104 -0.2213 0.061 Uiso 1 1 calc R . . C36 C -0.1056(4) 0.1229(2) -0.1208(2) 0.0407(11) Uani 1 1 d . . . H36 H -0.1641 0.1343 -0.0951 0.049 Uiso 1 1 calc R . . C37 C 0.2156(4) 0.0866(2) 0.2812(3) 0.0535(13) Uani 1 1 d . . . H37C H 0.2822 0.1046 0.2691 0.08 Uiso 1 1 calc R . . H37B H 0.198 0.0475 0.2497 0.08 Uiso 1 1 calc R . . H37A H 0.2197 0.0736 0.3341 0.08 Uiso 1 1 calc R . . C38 C -0.0083(4) 0.1198(3) 0.2994(3) 0.0688(16) Uani 1 1 d . . . H38C H 0.0054 0.1074 0.3523 0.103 Uiso 1 1 calc R . . H38B H -0.0323 0.0804 0.2703 0.103 Uiso 1 1 calc R . . H38A H -0.0614 0.1546 0.2945 0.103 Uiso 1 1 calc R . . C39 C 0.1497(5) 0.2263(2) 0.3236(3) 0.0581(14) Uani 1 1 d . . . H39C H 0.0939 0.2594 0.3185 0.087 Uiso 1 1 calc R . . H39B H 0.2131 0.2463 0.3079 0.087 Uiso 1 1 calc R . . H39A H 0.1609 0.2121 0.376 0.087 Uiso 1 1 calc R . . C40 C -0.2302(4) 0.0954(3) 0.1445(3) 0.0564(14) Uani 1 1 d . . . H40C H -0.3009 0.0789 0.146 0.085 Uiso 1 1 calc R . . H40B H -0.2229 0.1383 0.1707 0.085 Uiso 1 1 calc R . . H40A H -0.182 0.063 0.1691 0.085 Uiso 1 1 calc R . . C41 C -0.3069(4) 0.1619(3) 0.0017(3) 0.0613(15) Uani 1 1 d . . . H41C H -0.3737 0.1402 0.0056 0.092 Uiso 1 1 calc R . . H41B H -0.2967 0.1695 -0.0512 0.092 Uiso 1 1 calc R . . H41A H -0.3054 0.2047 0.0282 0.092 Uiso 1 1 calc R . . C42 C -0.2171(4) 0.0220(2) -0.0010(3) 0.0558(14) Uani 1 1 d . . . H42C H -0.169 -0.0097 0.0249 0.084 Uiso 1 1 calc R . . H42B H -0.2027 0.0255 -0.0537 0.084 Uiso 1 1 calc R . . H42A H -0.2879 0.0063 0.0019 0.084 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 Sm 0.02806(13) 0.03075(13) 0.02851(13) -0.00158(9) -0.00004(9) -0.00113(9) K 0.0470(6) 0.0333(5) 0.0385(6) 0.0030(4) 0.0023(5) -0.0062(4) Si1 0.0307(8) 0.0529(8) 0.0703(10) -0.0163(7) 0.0069(7) 0.0026(6) Si2 0.0796(12) 0.0763(10) 0.0289(8) 0.0042(7) 0.0007(8) -0.0248(9) Si3 0.0416(8) 0.0464(7) 0.0253(7) 0.0008(5) 0.0004(6) 0.0006(6) Si4 0.0273(7) 0.0417(7) 0.0435(8) -0.0010(5) 0.0031(6) -0.0065(5) N1 0.028(2) 0.0359(19) 0.041(2) -0.0049(15) 0.0048(17) -0.0020(15) N2 0.039(2) 0.0383(19) 0.028(2) -0.0026(15) 0.0035(17) -0.0062(16) N3 0.028(2) 0.0341(18) 0.0287(19) -0.0026(14) 0.0023(16) -0.0012(15) N4 0.028(2) 0.0394(19) 0.032(2) -0.0019(15) 0.0044(17) -0.0039(15) C1 0.033(3) 0.032(2) 0.033(2) 0.0012(17) 0.003(2) 0.0039(18) C2 0.032(3) 0.037(2) 0.027(2) -0.0056(17) -0.004(2) -0.0039(19) C3 0.036(3) 0.031(2) 0.030(2) 0.0039(17) 0.005(2) 0.0029(18) C4 0.033(3) 0.050(3) 0.036(3) -0.003(2) 0.001(2) 0.011(2) C5 0.052(3) 0.065(3) 0.046(3) -0.018(2) 0.000(3) 0.001(3) C6 0.084(5) 0.094(5) 0.068(5) -0.043(4) -0.009(4) 0.013(4) C7 0.081(5) 0.146(7) 0.048(4) -0.043(4) -0.004(4) 0.040(5) C8 0.065(4) 0.136(6) 0.037(3) -0.002(4) 0.014(3) 0.033(4) C9 0.055(4) 0.076(4) 0.041(3) 0.004(3) 0.010(3) 0.011(3) C10 0.036(3) 0.041(2) 0.027(2) 0.0059(18) 0.004(2) 0.002(2) C11 0.040(3) 0.046(3) 0.042(3) -0.003(2) 0.006(2) -0.007(2) C12 0.054(4) 0.058(3) 0.052(3) 0.006(2) 0.008(3) -0.025(3) C13 0.034(3) 0.075(4) 0.064(4) 0.018(3) 0.013(3) -0.008(3) C14 0.047(3) 0.067(4) 0.071(4) 0.016(3) 0.030(3) 0.012(3) C15 0.050(3) 0.041(3) 0.056(3) 0.007(2) 0.025(3) -0.003(2) C16 0.052(4) 0.049(3) 0.110(5) 0.001(3) 0.021(3) 0.008(3) C17 0.049(4) 0.054(3) 0.142(6) -0.028(3) 0.036(4) -0.016(3) C18 0.051(4) 0.147(6) 0.086(5) -0.017(4) -0.022(4) 0.026(4) C19 0.318(13) 0.084(4) 0.100(6) 0.062(4) -0.090(7) -0.095(5) C20 0.097(4) 0.068(4) 0.044(3) 0.002(3) -0.024(3) -0.006(3) C21 0.107(6) 0.464(16) 0.044(5) -0.047(8) 0.031(5) -0.008(9) C22 0.027(2) 0.029(2) 0.031(2) -0.0003(17) 0.0033(19) 0.0006(17) C23 0.024(2) 0.033(2) 0.027(2) -0.0011(17) 0.007(2) -0.0025(17) C24 0.031(3) 0.031(2) 0.025(2) 0.0012(16) 0.0007(19) -0.0048(17) C25 0.027(2) 0.031(2) 0.031(2) 0.0015(17) -0.0009(19) -0.0036(17) C26 0.030(3) 0.043(3) 0.049(3) -0.013(2) 0.004(2) -0.006(2) C27 0.032(3) 0.059(3) 0.064(4) -0.016(3) 0.010(3) -0.004(2) C28 0.030(3) 0.058(3) 0.062(3) -0.007(3) 0.001(3) -0.011(2) C29 0.038(3) 0.047(3) 0.045(3) -0.007(2) -0.004(2) -0.012(2) C30 0.036(3) 0.040(2) 0.037(3) -0.0034(19) 0.002(2) 0.0005(19) C31 0.033(3) 0.028(2) 0.029(2) 0.0013(16) 0.001(2) -0.0042(17) C32 0.045(3) 0.043(3) 0.033(3) -0.0012(19) 0.003(2) -0.010(2) C33 0.069(4) 0.051(3) 0.031(3) -0.003(2) 0.015(3) -0.016(3) C34 0.082(4) 0.050(3) 0.026(3) 0.003(2) -0.003(3) -0.012(3) C35 0.061(4) 0.050(3) 0.039(3) 0.002(2) -0.018(3) -0.002(2) C36 0.042(3) 0.046(3) 0.032(3) 0.0006(19) -0.003(2) -0.003(2) C37 0.065(4) 0.050(3) 0.044(3) 0.013(2) -0.005(3) 0.002(2) C38 0.067(4) 0.107(5) 0.034(3) 0.001(3) 0.011(3) -0.010(3) C39 0.076(4) 0.062(3) 0.034(3) -0.006(2) -0.006(3) 0.013(3) C40 0.041(3) 0.077(4) 0.053(3) 0.000(3) 0.012(3) -0.015(3) C41 0.038(3) 0.075(4) 0.071(4) 0.001(3) 0.003(3) 0.008(3) C42 0.054(3) 0.045(3) 0.067(4) -0.007(2) 0.003(3) -0.020(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sm N4 2.308(3) . ? Sm N3 2.309(3) . ? Sm N2 2.391(3) . ? Sm N1 2.412(3) . ? Sm C22 2.562(4) . ? Sm C24 2.601(4) . ? Sm C23 2.611(4) . ? Sm C3 2.905(4) . ? Sm C1 2.919(4) . ? Sm C2 2.940(4) . ? K N3 2.812(3) . ? K N4 2.873(3) . ? K C23 2.923(4) . ? K C22 2.940(4) . ? K C24 2.987(4) . ? K C33 3.136(4) 3 ? K C32 3.145(4) 3 ? K C34 3.232(5) 3 ? K C31 3.279(4) 3 ? K C35 3.323(5) 3 ? K C36 3.336(4) 3 ? K Si3 3.4581(15) . ? Si1 N1 1.740(4) . ? Si1 C17 1.856(6) . ? Si1 C16 1.857(5) . ? Si1 C18 1.866(6) . ? Si2 N2 1.741(4) . ? Si2 C21 1.837(7) . ? Si2 C20 1.840(5) . ? Si2 C19 1.849(6) . ? Si3 N3 1.703(3) . ? Si3 C39 1.873(5) . ? Si3 C37 1.876(5) . ? Si3 C38 1.882(5) . ? Si4 N4 1.688(4) . ? Si4 C40 1.869(5) . ? Si4 C41 1.881(5) . ? Si4 C42 1.882(4) . ? N1 C1 1.335(5) . ? N2 C3 1.324(5) . ? N3 C22 1.422(5) . ? N4 C24 1.428(5) . ? C1 C2 1.423(6) . ? C1 C4 1.501(6) . ? C2 C3 1.422(6) . ? C3 C10 1.489(6) . ? C4 C5 1.381(6) . ? C4 C9 1.391(7) . ? C5 C6 1.390(7) . ? C6 C7 1.377(9) . ? C7 C8 1.376(9) . ? C8 C9 1.382(7) . ? C10 C11 1.386(6) . ? C10 C15 1.389(6) . ? C11 C12 1.397(6) . ? C12 C13 1.370(7) . ? C13 C14 1.363(7) . ? C14 C15 1.389(7) . ? C22 C23 1.418(6) . ? C22 C25 1.484(6) . ? C23 C24 1.448(6) . ? C24 C31 1.463(5) . ? C25 C26 1.391(6) . ? C25 C30 1.404(5) . ? C26 C27 1.376(6) . ? C27 C28 1.376(6) . ? C28 C29 1.365(6) . ? C29 C30 1.383(6) . ? C31 C36 1.414(6) . ? C31 C32 1.415(6) . ? C31 K 3.279(4) 3 ? C32 C33 1.392(6) . ? C32 K 3.145(4) 3 ? C33 C34 1.380(7) . ? C33 K 3.136(4) 3 ? C34 C35 1.375(7) . ? C34 K 3.232(5) 3 ? C35 C36 1.385(6) . ? C35 K 3.323(5) 3 ? C36 K 3.336(4) 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 N4 Sm N3 83.07(11) . . ? N4 Sm N2 129.28(11) . . ? N3 Sm N2 124.10(12) . . ? N4 Sm N1 130.36(12) . . ? N3 Sm N1 117.71(11) . . ? N2 Sm N1 78.08(12) . . ? N4 Sm C22 80.90(12) . . ? N3 Sm C22 33.43(12) . . ? N2 Sm C22 99.88(12) . . ? N1 Sm C22 141.38(12) . . ? N4 Sm C24 33.15(12) . . ? N3 Sm C24 81.05(12) . . ? N2 Sm C24 103.29(12) . . ? N1 Sm C24 156.90(12) . . ? C22 Sm C24 61.60(12) . . ? N4 Sm C23 60.47(12) . . ? N3 Sm C23 60.34(12) . . ? N2 Sm C23 94.27(12) . . ? N1 Sm C23 169.17(12) . . ? C22 Sm C23 31.80(12) . . ? C24 Sm C23 32.26(12) . . ? N4 Sm C3 152.32(12) . . ? N3 Sm C3 103.78(11) . . ? N2 Sm C3 26.77(11) . . ? N1 Sm C3 70.51(11) . . ? C22 Sm C3 90.28(12) . . ? C24 Sm C3 120.43(12) . . ? C23 Sm C3 99.21(12) . . ? N4 Sm C1 154.03(12) . . ? N3 Sm C1 100.09(11) . . ? N2 Sm C1 70.00(11) . . ? N1 Sm C1 26.91(11) . . ? C22 Sm C1 115.76(12) . . ? C24 Sm C1 172.66(12) . . ? C23 Sm C1 142.92(12) . . ? C3 Sm C1 52.23(12) . . ? N4 Sm C2 175.43(12) . . ? N3 Sm C2 92.51(11) . . ? N2 Sm C2 52.71(11) . . ? N1 Sm C2 52.98(12) . . ? C22 Sm C2 94.77(12) . . ? C24 Sm C2 145.00(12) . . ? C23 Sm C2 116.24(12) . . ? C3 Sm C2 28.15(11) . . ? C1 Sm C2 28.10(12) . . ? N4 Sm K 42.45(8) . . ? N3 Sm K 40.91(8) . . ? N2 Sm K 139.03(8) . . ? N1 Sm K 141.53(8) . . ? C22 Sm K 45.19(9) . . ? C24 Sm K 46.32(8) . . ? C23 Sm K 44.93(9) . . ? C3 Sm K 135.47(8) . . ? C1 Sm K 137.49(8) . . ? C2 Sm K 133.03(9) . . ? N3 K N4 65.16(9) . . ? N3 K C23 51.34(10) . . ? N4 K C23 50.89(11) . . ? N3 K C22 28.51(10) . . ? N4 K C22 65.98(10) . . ? C23 K C22 27.99(11) . . ? N3 K C24 66.86(10) . . ? N4 K C24 28.13(10) . . ? C23 K C24 28.34(11) . . ? C22 K C24 52.98(11) . . ? N3 K C33 137.92(11) . 3 ? N4 K C33 126.54(13) . 3 ? C23 K C33 170.39(12) . 3 ? C22 K C33 161.29(12) . 3 ? C24 K C33 144.85(13) . 3 ? N3 K C32 161.28(11) . 3 ? N4 K C32 115.16(11) . 3 ? C23 K C32 144.78(12) . 3 ? C22 K C32 170.21(12) . 3 ? C24 K C32 123.11(11) . 3 ? C33 K C32 25.61(11) 3 3 ? N3 K C34 125.85(11) . 3 ? N4 K C34 150.04(13) . 3 ? C23 K C34 159.05(14) . 3 ? C22 K C34 138.61(13) . 3 ? C24 K C34 167.21(12) . 3 ? C33 K C34 24.97(13) 3 3 ? C32 K C34 44.41(12) 3 3 ? N3 K C31 170.71(11) . 3 ? N4 K C31 121.56(10) . 3 ? C23 K C31 126.37(11) . 3 ? C22 K C31 145.17(11) . 3 ? C24 K C31 115.58(10) . 3 ? C33 K C31 45.10(11) 3 3 ? C32 K C31 25.34(11) 3 3 ? C34 K C31 52.20(11) 3 3 ? N3 K C35 130.02(11) . 3 ? N4 K C35 164.72(11) . 3 ? C23 K C35 137.03(13) . 3 ? C22 K C35 127.65(12) . 3 ? C24 K C35 150.56(12) . 3 ? C33 K C35 42.81(14) 3 3 ? C32 K C35 50.12(12) 3 3 ? C34 K C35 24.16(13) 3 3 ? C31 K C35 43.68(11) 3 3 ? N3 K C36 146.62(11) . 3 ? N4 K C36 143.64(10) . 3 ? C23 K C36 124.94(12) . 3 ? C22 K C36 130.26(12) . 3 ? C24 K C36 128.05(11) . 3 ? C33 K C36 50.13(13) 3 3 ? C32 K C36 42.86(12) 3 3 ? C34 K C36 42.94(12) 3 3 ? C31 K C36 24.67(10) 3 3 ? C35 K C36 24.00(11) 3 3 ? N3 K Si3 29.27(7) . . ? N4 K Si3 89.72(7) . . ? C23 K Si3 78.81(8) . . ? C22 K Si3 52.04(8) . . ? C24 K Si3 96.05(8) . . ? C33 K Si3 110.78(9) 3 . ? C32 K Si3 136.35(9) 3 . ? C34 K Si3 96.60(9) 3 . ? C31 K Si3 147.53(8) 3 . ? C35 K Si3 104.35(9) 3 . ? C36 K Si3 126.41(8) 3 . ? N1 Si1 C17 110.3(2) . . ? N1 Si1 C16 114.9(2) . . ? C17 Si1 C16 110.5(3) . . ? N1 Si1 C18 104.4(2) . . ? C17 Si1 C18 109.3(3) . . ? C16 Si1 C18 107.1(3) . . ? N2 Si2 C21 115.8(3) . . ? N2 Si2 C20 104.6(2) . . ? C21 Si2 C20 108.1(3) . . ? N2 Si2 C19 106.9(3) . . ? C21 Si2 C19 111.8(4) . . ? C20 Si2 C19 109.2(3) . . ? N3 Si3 C39 116.2(2) . . ? N3 Si3 C37 112.0(2) . . ? C39 Si3 C37 108.4(2) . . ? N3 Si3 C38 107.6(2) . . ? C39 Si3 C38 104.5(3) . . ? C37 Si3 C38 107.7(3) . . ? N3 Si3 K 53.84(11) . . ? C39 Si3 K 169.67(16) . . ? C37 Si3 K 79.79(16) . . ? C38 Si3 K 78.23(17) . . ? N4 Si4 C40 108.0(2) . . ? N4 Si4 C41 114.2(2) . . ? C40 Si4 C41 105.2(2) . . ? N4 Si4 C42 114.7(2) . . ? C40 Si4 C42 106.6(2) . . ? C41 Si4 C42 107.5(2) . . ? N4 Si4 K 53.04(12) . . ? C40 Si4 K 78.06(17) . . ? C41 Si4 K 166.71(17) . . ? C42 Si4 K 83.42(17) . . ? C1 N1 Si1 130.1(3) . . ? C1 N1 Sm 98.2(2) . . ? Si1 N1 Sm 131.24(17) . . ? C3 N2 Si2 130.3(3) . . ? C3 N2 Sm 98.8(2) . . ? Si2 N2 Sm 130.66(18) . . ? C22 N3 Si3 130.9(3) . . ? C22 N3 Sm 83.1(2) . . ? Si3 N3 Sm 141.90(18) . . ? C22 N3 K 80.7(2) . . ? Si3 N3 K 96.89(13) . . ? Sm N3 K 106.57(12) . . ? C24 N4 Si4 137.5(3) . . ? C24 N4 Sm 84.8(2) . . ? Si4 N4 Sm 134.77(18) . . ? C24 N4 K 80.4(2) . . ? Si4 N4 K 98.96(14) . . ? Sm N4 K 104.71(12) . . ? N1 C1 C2 123.9(4) . . ? N1 C1 C4 120.5(4) . . ? C2 C1 C4 115.7(4) . . ? N1 C1 Sm 54.9(2) . . ? C2 C1 Sm 76.7(2) . . ? C4 C1 Sm 148.6(3) . . ? C3 C2 C1 128.7(4) . . ? C3 C2 Sm 74.6(2) . . ? C1 C2 Sm 75.1(2) . . ? N2 C3 C2 123.3(4) . . ? N2 C3 C10 121.4(4) . . ? C2 C3 C10 115.3(4) . . ? N2 C3 Sm 54.5(2) . . ? C2 C3 Sm 77.3(2) . . ? C10 C3 Sm 148.6(3) . . ? C5 C4 C9 118.7(4) . . ? C5 C4 C1 121.3(4) . . ? C9 C4 C1 120.0(4) . . ? C4 C5 C6 121.2(6) . . ? C7 C6 C5 119.0(6) . . ? C8 C7 C6 120.7(6) . . ? C7 C8 C9 120.0(6) . . ? C8 C9 C4 120.4(6) . . ? C11 C10 C15 118.3(4) . . ? C11 C10 C3 121.6(4) . . ? C15 C10 C3 120.0(4) . . ? C10 C11 C12 120.7(5) . . ? C13 C12 C11 119.7(5) . . ? C14 C13 C12 120.4(5) . . ? C13 C14 C15 120.3(5) . . ? C14 C15 C10 120.5(4) . . ? C23 C22 N3 122.2(4) . . ? C23 C22 C25 116.4(4) . . ? N3 C22 C25 121.2(3) . . ? C23 C22 Sm 76.0(2) . . ? N3 C22 Sm 63.47(19) . . ? C25 C22 Sm 131.4(2) . . ? C23 C22 K 75.3(2) . . ? N3 C22 K 70.75(19) . . ? C25 C22 K 131.6(2) . . ? Sm C22 K 96.62(13) . . ? C22 C23 C24 134.6(4) . . ? C22 C23 Sm 72.2(2) . . ? C24 C23 Sm 73.5(2) . . ? C22 C23 K 76.7(2) . . ? C24 C23 K 78.3(2) . . ? Sm C23 K 95.96(14) . . ? N4 C24 C23 120.0(3) . . ? N4 C24 C31 122.4(4) . . ? C23 C24 C31 117.6(4) . . ? N4 C24 Sm 62.09(18) . . ? C23 C24 Sm 74.3(2) . . ? C31 C24 Sm 136.2(3) . . ? N4 C24 K 71.5(2) . . ? C23 C24 K 73.4(2) . . ? C31 C24 K 129.0(2) . . ? Sm C24 K 94.65(12) . . ? C26 C25 C30 115.9(4) . . ? C26 C25 C22 122.4(4) . . ? C30 C25 C22 121.7(4) . . ? C27 C26 C25 122.2(4) . . ? C28 C27 C26 120.5(5) . . ? C29 C28 C27 119.1(4) . . ? C28 C29 C30 120.7(4) . . ? C29 C30 C25 121.6(4) . . ? C36 C31 C32 114.1(4) . . ? C36 C31 C24 121.4(4) . . ? C32 C31 C24 124.4(4) . . ? C36 C31 K 79.9(2) . 3 ? C32 C31 K 72.1(2) . 3 ? C24 C31 K 115.0(2) . 3 ? C33 C32 C31 122.7(5) . . ? C33 C32 K 76.8(2) . 3 ? C31 C32 K 82.6(2) . 3 ? C34 C33 C32 120.9(5) . . ? C34 C33 K 81.4(3) . 3 ? C32 C33 K 77.6(2) . 3 ? C35 C34 C33 118.2(5) . . ? C35 C34 K 81.6(3) . 3 ? C33 C34 K 73.6(3) . 3 ? C34 C35 C36 121.4(5) . . ? C34 C35 K 74.2(3) . 3 ? C36 C35 K 78.5(3) . 3 ? C35 C36 C31 122.7(5) . . ? C35 C36 K 77.5(3) . 3 ? C31 C36 K 75.4(2) . 3 ? #===END data_(5)-jul1201 _database_code_depnum_ccdc_archive 'CCDC 768771' #TrackingRef 'MFL-Dalton-feb2010[1].cif' _audit_creation_date 2001-07-20T15:38:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common (Sm2(Me3SiNC(C6H4Ph)CHC(C6H4Ph)NSiMe3)3).hexane _chemical_formula_moiety '(C99 H111 N6 Si6 Sm2)(C6 H14)' _chemical_formula_sum 'C105 H125 N6 Si6 Sm2' _chemical_formula_weight 1940.35 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3495(6) _cell_length_b 16.7924(9) _cell_length_c 24.5587(14) _cell_angle_alpha 97.177(3) _cell_angle_beta 95.469(3) _cell_angle_gamma 111.259(3) _cell_volume 5408.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 46114 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2010 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.186 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.897 _exptl_absorpt_correction_T_max 0.941 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 26442 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_unetI/netI 0.0985 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 21.95 _diffrn_reflns_theta_full 21.95 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _reflns_number_total 12909 _reflns_number_gt 9200 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The hexane solvate molecule was pooorly defined and only 5 carbon atoms were included with isotropic displacement parameters. 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+22.3030P] 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_number_reflns 12909 _refine_ls_number_parameters 1038 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.094 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1412 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.879 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.113 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 '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' 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 Sm1 Sm 0.44232(3) 0.70955(3) 0.73217(2) 0.03342(16) Uani 1 1 d . . . Sm2 Sm 0.69841(3) 0.71673(3) 0.69260(2) 0.03203(16) Uani 1 1 d . . . Si1 Si 0.1519(2) 0.58340(19) 0.67422(13) 0.0477(8) Uani 1 1 d . . . Si2 Si 0.3486(2) 0.7900(2) 0.86592(13) 0.0525(8) Uani 1 1 d . . . Si3 Si 0.5637(2) 0.79304(17) 0.61356(11) 0.0363(6) Uani 1 1 d . . . Si4 Si 0.4804(2) 0.52447(17) 0.73139(11) 0.0392(7) Uani 1 1 d . . . Si5 Si 0.7993(2) 0.6512(2) 0.55856(12) 0.0492(8) Uani 1 1 d . . . Si6 Si 0.9637(2) 0.87789(18) 0.74425(12) 0.0432(7) Uani 1 1 d . . . N1 N 0.2698(5) 0.6705(5) 0.6895(3) 0.0370(19) Uani 1 1 d . . . N2 N 0.3837(6) 0.7876(5) 0.7992(3) 0.041(2) Uani 1 1 d . . . N3 N 0.5674(5) 0.7807(4) 0.6824(3) 0.0299(17) Uani 1 1 d . . . N4 N 0.5590(5) 0.6323(4) 0.7349(3) 0.0298(17) Uani 1 1 d . . . N5 N 0.7601(5) 0.6524(5) 0.6231(3) 0.0377(19) Uani 1 1 d . . . N6 N 0.8642(5) 0.7794(5) 0.7353(3) 0.0369(19) Uani 1 1 d . . . C1 C 0.2897(7) 0.7476(6) 0.6746(4) 0.039(2) Uani 1 1 d . . . C2 C 0.3576(7) 0.8277(6) 0.7077(4) 0.039(2) Uani 1 1 d . . . H2 H 0.3884 0.8735 0.6882 0.046 Uiso 1 1 calc R . . C3 C 0.3847(6) 0.8470(6) 0.7666(4) 0.037(2) Uani 1 1 d . . . C4 C 0.0512(8) 0.6260(9) 0.6651(6) 0.073(4) Uani 1 1 d . . . H4A H 0.0586 0.6692 0.6977 0.109 Uiso 1 1 calc R . . H4B H -0.0149 0.5784 0.6609 0.109 Uiso 1 1 calc R . . H4C H 0.0562 0.6532 0.6318 0.109 Uiso 1 1 calc R . . C5 C 0.1380(10) 0.5003(9) 0.6135(6) 0.091(5) Uani 1 1 d . . . H5A H 0.1919 0.478 0.6188 0.136 Uiso 1 1 calc R . . H5B H 0.1425 0.5264 0.5798 0.136 Uiso 1 1 calc R . . H5C H 0.0721 0.4526 0.6098 0.136 Uiso 1 1 calc R . . C6 C 0.1379(9) 0.5276(8) 0.7365(6) 0.077(4) Uani 1 1 d . . . H6A H 0.1446 0.5695 0.7697 0.116 Uiso 1 1 calc R . . H6B H 0.1905 0.5038 0.7414 0.116 Uiso 1 1 calc R . . H6C H 0.0711 0.4805 0.7309 0.116 Uiso 1 1 calc R . . C7 C 0.2433(10) 0.8278(9) 0.8645(6) 0.087(4) Uani 1 1 d . . . H7A H 0.2672 0.888 0.8583 0.13 Uiso 1 1 calc R . . H7B H 0.2176 0.8244 0.9001 0.13 Uiso 1 1 calc R . . H7C H 0.1891 0.7912 0.8345 0.13 Uiso 1 1 calc R . . C8 C 0.4505(11) 0.8593(8) 0.9243(5) 0.082(4) Uani 1 1 d . . . H8A H 0.5071 0.8397 0.9252 0.123 Uiso 1 1 calc R . . H8B H 0.4238 0.8547 0.9595 0.123 Uiso 1 1 calc R . . H8C H 0.4742 0.9199 0.9188 0.123 Uiso 1 1 calc R . . C9 C 0.3086(10) 0.6760(7) 0.8778(5) 0.069(3) Uani 1 1 d . . . H9A H 0.3666 0.6583 0.8787 0.103 Uiso 1 1 calc R . . H9B H 0.2552 0.638 0.8477 0.103 Uiso 1 1 calc R . . H9C H 0.2827 0.6715 0.9133 0.103 Uiso 1 1 calc R . . C10 C 0.2475(7) 0.7576(7) 0.6178(4) 0.043(3) Uani 1 1 d . . . C11 C 0.2194(7) 0.8263(6) 0.6108(5) 0.045(3) Uani 1 1 d . . . H11 H 0.2222 0.8672 0.642 0.055 Uiso 1 1 calc R . . C12 C 0.1867(7) 0.8353(7) 0.5574(4) 0.045(3) Uani 1 1 d . . . H12 H 0.1655 0.8819 0.5532 0.054 Uiso 1 1 calc R . . C13 C 0.1839(7) 0.7795(6) 0.5106(4) 0.042(3) Uani 1 1 d . . . C14 C 0.2127(7) 0.7102(6) 0.5193(4) 0.043(3) Uani 1 1 d . . . H14 H 0.2113 0.6698 0.4882 0.052 Uiso 1 1 calc R . . C15 C 0.2428(7) 0.6993(7) 0.5714(4) 0.045(3) Uani 1 1 d . . . H15 H 0.2607 0.6511 0.5758 0.053 Uiso 1 1 calc R . . C16 C 0.1554(7) 0.7945(7) 0.4542(4) 0.046(3) Uani 1 1 d . . . C17 C 0.1761(8) 0.8755(7) 0.4425(5) 0.058(3) Uani 1 1 d . . . H17 H 0.2072 0.924 0.4716 0.069 Uiso 1 1 calc R . . C18 C 0.1529(10) 0.8896(8) 0.3892(5) 0.068(3) Uani 1 1 d . . . H18 H 0.1664 0.9467 0.382 0.081 Uiso 1 1 calc R . . C19 C 0.1113(10) 0.8213(10) 0.3480(5) 0.076(4) Uani 1 1 d . . . H19 H 0.0973 0.8308 0.3113 0.091 Uiso 1 1 calc R . . C20 C 0.0886(10) 0.7390(9) 0.3574(5) 0.072(4) Uani 1 1 d . . . H20 H 0.0587 0.6911 0.3279 0.086 Uiso 1 1 calc R . . C21 C 0.1101(8) 0.7263(8) 0.4109(5) 0.062(3) Uani 1 1 d . . . H21 H 0.0931 0.6688 0.418 0.074 Uiso 1 1 calc R . . C22 C 0.4197(7) 0.9415(6) 0.7921(4) 0.040(2) Uani 1 1 d . . . C23 C 0.3652(8) 0.9911(7) 0.7778(5) 0.056(3) Uani 1 1 d . . . H23 H 0.3066 0.9666 0.7503 0.067 Uiso 1 1 calc R . . C24 C 0.3964(9) 1.0763(8) 0.8036(5) 0.061(3) Uani 1 1 d . . . H24 H 0.3582 1.1094 0.7934 0.074 Uiso 1 1 calc R . . C25 C 0.4804(8) 1.1153(7) 0.8435(4) 0.048(3) Uani 1 1 d . . . C26 C 0.5377(7) 1.0667(6) 0.8565(4) 0.045(3) Uani 1 1 d . . . H26 H 0.5976 1.0925 0.883 0.054 Uiso 1 1 calc R . . C27 C 0.5074(7) 0.9804(6) 0.8311(4) 0.040(2) Uani 1 1 d . . . H27 H 0.5469 0.9479 0.8404 0.048 Uiso 1 1 calc R . . C28 C 0.5102(8) 1.2051(7) 0.8732(4) 0.052(3) Uani 1 1 d . . . C29 C 0.5034(11) 1.2700(7) 0.8470(5) 0.077(4) Uani 1 1 d . . . H29 H 0.4781 1.2583 0.8084 0.092 Uiso 1 1 calc R . . C30 C 0.5343(12) 1.3549(8) 0.8773(6) 0.095(5) Uani 1 1 d . . . H30 H 0.5283 1.3995 0.8588 0.114 Uiso 1 1 calc R . . C31 C 0.5712(11) 1.3739(9) 0.9309(6) 0.087(5) Uani 1 1 d . . . H31 H 0.5917 1.4315 0.9504 0.104 Uiso 1 1 calc R . . C32 C 0.5793(10) 1.3118(10) 0.9568(6) 0.080(4) Uani 1 1 d . . . H32 H 0.6051 1.325 0.9954 0.096 Uiso 1 1 calc R . . C33 C 0.5503(9) 1.2269(8) 0.9283(5) 0.061(3) Uani 1 1 d . . . H33 H 0.5586 1.1836 0.9476 0.073 Uiso 1 1 calc R . . C34 C 0.6215(7) 0.8309(6) 0.7359(4) 0.033(2) Uani 1 1 d . . . C35 C 0.6330(7) 0.7862(6) 0.7803(4) 0.033(2) Uani 1 1 d . . . H35 H 0.6686 0.8234 0.8142 0.04 Uiso 1 1 calc R . . C36 C 0.6012(7) 0.6964(6) 0.7832(4) 0.032(2) Uani 1 1 d . . . C37 C 0.4930(7) 0.8551(7) 0.5844(4) 0.045(3) Uani 1 1 d . . . H37A H 0.5242 0.916 0.6025 0.067 Uiso 1 1 calc R . . H37B H 0.4226 0.8307 0.5909 0.067 Uiso 1 1 calc R . . H37C H 0.4948 0.8513 0.5444 0.067 Uiso 1 1 calc R . . C38 C 0.4987(8) 0.6786(6) 0.5767(4) 0.050(3) Uani 1 1 d . . . H38A H 0.5334 0.6429 0.5907 0.074 Uiso 1 1 calc R . . H38B H 0.5004 0.6767 0.5368 0.074 Uiso 1 1 calc R . . H38C H 0.4283 0.6563 0.5833 0.074 Uiso 1 1 calc R . . C39 C 0.6955(7) 0.8410(7) 0.5964(4) 0.052(3) Uani 1 1 d . . . H39A H 0.7361 0.8102 0.6109 0.078 Uiso 1 1 calc R . . H39B H 0.7264 0.9025 0.6133 0.078 Uiso 1 1 calc R . . H39C H 0.6927 0.8354 0.556 0.078 Uiso 1 1 calc R . . C40 C 0.3980(8) 0.5203(7) 0.7866(5) 0.055(3) Uani 1 1 d . . . H40A H 0.3676 0.5637 0.7842 0.082 Uiso 1 1 calc R . . H40B H 0.4389 0.5327 0.8232 0.082 Uiso 1 1 calc R . . H40C H 0.3444 0.4625 0.7813 0.082 Uiso 1 1 calc R . . C41 C 0.4016(8) 0.4949(7) 0.6618(4) 0.055(3) Uani 1 1 d . . . H41A H 0.3699 0.537 0.6576 0.082 Uiso 1 1 calc R . . H41B H 0.349 0.4368 0.6582 0.082 Uiso 1 1 calc R . . H41C H 0.4444 0.4952 0.633 0.082 Uiso 1 1 calc R . . C42 C 0.5375(8) 0.4433(6) 0.7364(5) 0.053(3) Uani 1 1 d . . . H42A H 0.58 0.4569 0.7726 0.079 Uiso 1 1 calc R . . H42B H 0.5791 0.444 0.7068 0.079 Uiso 1 1 calc R . . H42C H 0.4839 0.3856 0.7323 0.079 Uiso 1 1 calc R . . C43 C 0.6628(6) 0.9271(5) 0.7462(4) 0.031(2) Uani 1 1 d . . . C44 C 0.7452(7) 0.9755(6) 0.7886(4) 0.038(2) Uani 1 1 d . . . H44 H 0.7757 0.9459 0.8102 0.045 Uiso 1 1 calc R . . C45 C 0.7817(7) 1.0641(6) 0.7991(4) 0.041(2) Uani 1 1 d . . . H45 H 0.8361 1.094 0.8286 0.049 Uiso 1 1 calc R . . C46 C 0.7431(7) 1.1120(6) 0.7688(4) 0.036(2) Uani 1 1 d . . . C47 C 0.6651(8) 1.0658(6) 0.7264(4) 0.044(3) Uani 1 1 d . . . H47 H 0.6374 1.0964 0.704 0.053 Uiso 1 1 calc R . . C48 C 0.6251(7) 0.9754(6) 0.7151(4) 0.038(2) Uani 1 1 d . . . H48 H 0.5709 0.9462 0.6855 0.046 Uiso 1 1 calc R . . C49 C 0.7844(8) 1.2082(6) 0.7802(4) 0.045(3) Uani 1 1 d . . . C50 C 0.8867(9) 1.2570(7) 0.7972(4) 0.055(3) Uani 1 1 d . . . H50 H 0.9327 1.2285 0.8014 0.066 Uiso 1 1 calc R . . C51 C 0.9224(12) 1.3470(8) 0.8081(5) 0.074(4) Uani 1 1 d . . . H51 H 0.9926 1.3791 0.8203 0.089 Uiso 1 1 calc R . . C52 C 0.8605(14) 1.3896(8) 0.8019(6) 0.087(5) Uani 1 1 d . . . H52 H 0.8866 1.4512 0.8089 0.104 Uiso 1 1 calc R . . C53 C 0.7603(12) 1.3440(8) 0.7855(5) 0.075(4) Uani 1 1 d . . . H53 H 0.7161 1.3741 0.7811 0.09 Uiso 1 1 calc R . . C54 C 0.7203(10) 1.2522(7) 0.7748(5) 0.060(3) Uani 1 1 d . . . H54 H 0.6496 1.221 0.764 0.072 Uiso 1 1 calc R . . C55 C 0.6298(7) 0.6731(6) 0.8375(4) 0.038(2) Uani 1 1 d . . . C56 C 0.6777(7) 0.6149(6) 0.8404(4) 0.039(2) Uani 1 1 d . . . H56 H 0.6911 0.5886 0.8071 0.047 Uiso 1 1 calc R . . C57 C 0.7066(7) 0.5938(6) 0.8902(4) 0.042(3) Uani 1 1 d . . . H57 H 0.741 0.5549 0.8903 0.051 Uiso 1 1 calc R . . C58 C 0.6869(7) 0.6276(6) 0.9398(4) 0.038(2) Uani 1 1 d . . . C59 C 0.6353(8) 0.6829(7) 0.9369(4) 0.048(3) Uani 1 1 d . . . H59 H 0.6179 0.7056 0.9701 0.058 Uiso 1 1 calc R . . C60 C 0.6082(8) 0.7065(6) 0.8872(4) 0.045(3) Uani 1 1 d . . . H60 H 0.5745 0.7458 0.8873 0.054 Uiso 1 1 calc R . . C61 C 0.7183(8) 0.6066(6) 0.9933(4) 0.046(3) Uani 1 1 d . . . C62 C 0.8111(9) 0.6005(7) 1.0050(4) 0.055(3) Uani 1 1 d . . . H62 H 0.8558 0.6109 0.9782 0.066 Uiso 1 1 calc R . . C63 C 0.8408(11) 0.5795(9) 1.0545(5) 0.076(4) Uani 1 1 d . . . H63 H 0.9061 0.5775 1.0617 0.092 Uiso 1 1 calc R . . C64 C 0.7776(13) 0.5615(9) 1.0934(5) 0.084(4) Uani 1 1 d . . . H64 H 0.7972 0.5459 1.1272 0.101 Uiso 1 1 calc R . . C65 C 0.6856(12) 0.5667(10) 1.0820(5) 0.087(4) Uani 1 1 d . . . H65 H 0.6402 0.5533 1.1083 0.104 Uiso 1 1 calc R . . C66 C 0.6552(9) 0.5913(8) 1.0328(5) 0.067(4) Uani 1 1 d . . . H66 H 0.5918 0.5973 1.027 0.081 Uiso 1 1 calc R . . C67 C 0.7670(7) 0.5925(6) 0.6578(4) 0.036(2) Uani 1 1 d . . . C68 C 0.8116(6) 0.6199(6) 0.7139(4) 0.033(2) Uani 1 1 d . . . H68 H 0.8039 0.5726 0.733 0.039 Uiso 1 1 calc R . . C69 C 0.8657(6) 0.7020(6) 0.7491(4) 0.032(2) Uani 1 1 d . . . C70 C 0.9075(8) 0.7546(8) 0.5592(5) 0.069(4) Uani 1 1 d . . . H70A H 0.8873 0.8036 0.5697 0.103 Uiso 1 1 calc R . . H70B H 0.9273 0.7559 0.5221 0.103 Uiso 1 1 calc R . . H70C H 0.9648 0.7587 0.586 0.103 Uiso 1 1 calc R . . C71 C 0.8410(10) 0.5582(9) 0.5380(5) 0.079(4) Uani 1 1 d . . . H71A H 0.785 0.503 0.5374 0.118 Uiso 1 1 calc R . . H71B H 0.8986 0.5631 0.5649 0.118 Uiso 1 1 calc R . . H71C H 0.8611 0.5605 0.501 0.118 Uiso 1 1 calc R . . C72 C 0.6958(9) 0.6437(9) 0.5014(4) 0.071(4) Uani 1 1 d . . . H72A H 0.6372 0.5897 0.4996 0.107 Uiso 1 1 calc R . . H72B H 0.7212 0.644 0.4657 0.107 Uiso 1 1 calc R . . H72C H 0.6758 0.6933 0.5094 0.107 Uiso 1 1 calc R . . C73 C 1.0772(8) 0.8628(7) 0.7215(6) 0.069(4) Uani 1 1 d . . . H73A H 1.0984 0.8274 0.7449 0.103 Uiso 1 1 calc R . . H73B H 1.1323 0.9195 0.7249 0.103 Uiso 1 1 calc R . . H73C H 1.0606 0.8336 0.6827 0.103 Uiso 1 1 calc R . . C74 C 1.0080(9) 0.9452(7) 0.8151(5) 0.070(4) Uani 1 1 d . . . H74A H 1.0293 0.9125 0.8407 0.105 Uiso 1 1 calc R . . H74B H 0.9528 0.9598 0.8281 0.105 Uiso 1 1 calc R . . H74C H 1.0653 0.9987 0.8137 0.105 Uiso 1 1 calc R . . C75 C 0.9257(8) 0.9446(7) 0.6992(5) 0.056(3) Uani 1 1 d . . . H75A H 0.8663 0.9537 0.7107 0.084 Uiso 1 1 calc R . . H75B H 0.9091 0.9147 0.6605 0.084 Uiso 1 1 calc R . . H75C H 0.9815 1.0008 0.7023 0.084 Uiso 1 1 calc R . . C76 C 0.7145(7) 0.5003(6) 0.6376(4) 0.036(2) Uani 1 1 d . . . C77 C 0.6256(7) 0.4685(6) 0.5989(4) 0.041(2) Uani 1 1 d . . . H77 H 0.6027 0.5084 0.5833 0.049 Uiso 1 1 calc R . . C78 C 0.5706(7) 0.3808(7) 0.5829(4) 0.044(3) Uani 1 1 d . . . H78 H 0.5101 0.362 0.557 0.052 Uiso 1 1 calc R . . C79 C 0.6003(7) 0.3193(6) 0.6032(4) 0.040(2) Uani 1 1 d . . . C80 C 0.6916(8) 0.3511(7) 0.6390(4) 0.049(3) Uani 1 1 d . . . H80 H 0.7164 0.3106 0.6522 0.058 Uiso 1 1 calc R . . C81 C 0.7488(8) 0.4396(6) 0.6565(4) 0.043(3) Uani 1 1 d . . . H81 H 0.8107 0.4582 0.6811 0.051 Uiso 1 1 calc R . . C82 C 0.5423(8) 0.2263(7) 0.5861(4) 0.048(3) Uani 1 1 d . . . C83 C 0.4396(9) 0.1945(7) 0.5722(5) 0.067(3) Uani 1 1 d . . . H83 H 0.4048 0.2331 0.5726 0.08 Uiso 1 1 calc R . . C84 C 0.3841(10) 0.1028(9) 0.5571(6) 0.078(4) Uani 1 1 d . . . H84 H 0.3125 0.0812 0.5484 0.093 Uiso 1 1 calc R . . C85 C 0.4316(10) 0.0464(8) 0.5549(6) 0.075(4) Uani 1 1 d . . . H85 H 0.3938 -0.0143 0.5457 0.09 Uiso 1 1 calc R . . C86 C 0.5344(11) 0.0779(7) 0.5663(6) 0.073(4) Uani 1 1 d . . . H86 H 0.5685 0.0389 0.5636 0.088 Uiso 1 1 calc R . . C87 C 0.5906(9) 0.1672(7) 0.5821(5) 0.057(3) Uani 1 1 d . . . H87 H 0.6623 0.1878 0.5901 0.068 Uiso 1 1 calc R . . C88 C 0.9143(7) 0.6987(6) 0.8044(4) 0.035(2) Uani 1 1 d . . . C89 C 0.9614(7) 0.6412(6) 0.8113(4) 0.038(2) Uani 1 1 d . . . H89 H 0.9609 0.6021 0.7797 0.046 Uiso 1 1 calc R . . C90 C 1.0094(7) 0.6377(7) 0.8624(4) 0.044(3) Uani 1 1 d . . . H90 H 1.0403 0.5967 0.8651 0.053 Uiso 1 1 calc R . . C91 C 1.0120(7) 0.6944(7) 0.9096(4) 0.044(3) Uani 1 1 d . . . C92 C 0.9624(7) 0.7514(6) 0.9032(4) 0.043(3) Uani 1 1 d . . . H92 H 0.9606 0.7892 0.9349 0.051 Uiso 1 1 calc R . . C93 C 0.9163(7) 0.7540(6) 0.8522(4) 0.038(2) Uani 1 1 d . . . H93 H 0.8848 0.7946 0.8494 0.046 Uiso 1 1 calc R . . C94 C 1.0689(8) 0.6944(7) 0.9641(4) 0.046(3) Uani 1 1 d . . . C95 C 1.0784(8) 0.6201(8) 0.9764(5) 0.060(3) Uani 1 1 d . . . H95 H 1.0473 0.5673 0.9508 0.072 Uiso 1 1 calc R . . C96 C 1.1349(10) 0.6225(10) 1.0275(5) 0.072(4) Uani 1 1 d . . . H96 H 1.1432 0.5713 1.0353 0.087 Uiso 1 1 calc R . . C97 C 1.1773(10) 0.6962(10) 1.0654(5) 0.069(4) Uani 1 1 d . . . H97 H 1.2139 0.6972 1.0999 0.083 Uiso 1 1 calc R . . C98 C 1.1661(9) 0.7674(10) 1.0527(5) 0.071(4) Uani 1 1 d . . . H98 H 1.1954 0.8194 1.0792 0.085 Uiso 1 1 calc R . . C99 C 1.1134(8) 0.7691(8) 1.0027(4) 0.059(3) Uani 1 1 d . . . H99 H 1.1083 0.8216 0.9952 0.071 Uiso 1 1 calc R . . C100 C 0.791(3) 0.966(2) 0.9551(14) 0.277(17) Uiso 1 1 d D . . C101 C 0.746(3) 0.949(2) 1.0215(15) 0.274(16) Uiso 1 1 d D . . C102 C 0.844(2) 0.902(2) 1.0275(12) 0.238(14) Uiso 1 1 d D . . C103 C 0.776(3) 0.856(2) 1.0810(14) 0.277(17) Uiso 1 1 d D . . C104 C 0.881(4) 0.821(3) 1.094(2) 0.41(3) Uiso 1 1 d 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 Sm1 0.0363(3) 0.0332(3) 0.0314(3) 0.0069(2) 0.0059(2) 0.0133(2) Sm2 0.0358(3) 0.0317(3) 0.0291(3) 0.0054(2) 0.0028(2) 0.0139(2) Si1 0.0391(16) 0.0470(18) 0.0494(19) 0.0043(15) 0.0069(14) 0.0085(14) Si2 0.072(2) 0.0475(19) 0.0396(18) 0.0067(15) 0.0215(16) 0.0217(16) Si3 0.0415(15) 0.0382(16) 0.0311(15) 0.0117(13) 0.0052(12) 0.0157(13) Si4 0.0471(16) 0.0306(15) 0.0380(16) 0.0082(13) 0.0062(13) 0.0118(13) Si5 0.0552(18) 0.068(2) 0.0297(16) 0.0066(15) 0.0084(14) 0.0304(16) Si6 0.0384(15) 0.0360(16) 0.0479(18) 0.0025(14) -0.0007(13) 0.0086(13) N1 0.038(5) 0.033(5) 0.038(5) 0.003(4) 0.004(4) 0.011(4) N2 0.049(5) 0.039(5) 0.033(5) -0.003(4) 0.007(4) 0.016(4) N3 0.037(4) 0.025(4) 0.027(4) 0.005(3) 0.003(3) 0.011(3) N4 0.038(4) 0.024(4) 0.028(4) 0.005(3) 0.001(3) 0.013(3) N5 0.043(5) 0.042(5) 0.029(5) 0.003(4) 0.003(4) 0.018(4) N6 0.040(4) 0.033(5) 0.039(5) 0.005(4) 0.000(4) 0.018(4) C1 0.037(6) 0.044(7) 0.042(6) 0.000(5) 0.012(5) 0.023(5) C2 0.040(6) 0.037(6) 0.036(6) 0.006(5) 0.011(5) 0.010(5) C3 0.026(5) 0.043(6) 0.048(7) 0.012(5) 0.011(4) 0.016(4) C4 0.042(7) 0.092(10) 0.086(10) 0.027(8) 0.007(6) 0.024(7) C5 0.070(9) 0.080(10) 0.085(10) -0.025(8) 0.020(8) -0.004(7) C6 0.058(8) 0.065(9) 0.096(11) 0.028(8) 0.010(7) 0.004(6) C7 0.101(11) 0.079(10) 0.099(11) 0.020(8) 0.056(9) 0.043(8) C8 0.128(12) 0.060(8) 0.033(7) -0.014(6) 0.002(7) 0.015(8) C9 0.099(10) 0.061(8) 0.044(7) 0.012(6) 0.022(7) 0.024(7) C10 0.039(6) 0.046(7) 0.040(7) 0.009(5) -0.001(5) 0.011(5) C11 0.047(6) 0.041(6) 0.054(7) 0.006(5) 0.015(5) 0.022(5) C12 0.045(6) 0.056(7) 0.040(7) 0.014(6) 0.004(5) 0.024(5) C13 0.039(6) 0.042(6) 0.044(7) 0.004(5) 0.009(5) 0.014(5) C14 0.052(6) 0.032(6) 0.036(6) -0.004(5) 0.005(5) 0.009(5) C15 0.052(6) 0.041(6) 0.036(7) -0.001(5) -0.004(5) 0.017(5) C16 0.033(6) 0.054(7) 0.044(7) 0.011(6) 0.005(5) 0.008(5) C17 0.066(8) 0.051(8) 0.047(7) 0.005(6) 0.006(6) 0.013(6) C18 0.092(9) 0.054(8) 0.058(9) 0.026(7) -0.001(7) 0.025(7) C19 0.080(9) 0.093(11) 0.048(8) 0.029(8) 0.004(7) 0.022(8) C20 0.084(9) 0.067(9) 0.045(8) -0.003(7) -0.014(7) 0.015(7) C21 0.064(8) 0.050(7) 0.055(8) 0.008(6) -0.015(6) 0.009(6) C22 0.037(6) 0.031(6) 0.046(6) -0.005(5) 0.002(5) 0.009(5) C23 0.060(7) 0.045(7) 0.063(8) -0.007(6) -0.005(6) 0.028(6) C24 0.080(8) 0.057(8) 0.057(8) 0.002(6) -0.003(7) 0.043(7) C25 0.054(7) 0.045(7) 0.040(6) 0.000(5) 0.002(5) 0.017(6) C26 0.044(6) 0.039(6) 0.041(6) -0.002(5) -0.002(5) 0.007(5) C27 0.039(6) 0.047(7) 0.033(6) 0.004(5) 0.006(5) 0.016(5) C28 0.060(7) 0.041(7) 0.048(7) -0.002(6) 0.014(6) 0.014(5) C29 0.142(13) 0.035(7) 0.049(8) -0.002(6) 0.016(8) 0.032(8) C30 0.166(15) 0.046(8) 0.081(10) 0.020(8) 0.047(10) 0.038(9) C31 0.118(12) 0.051(8) 0.079(10) -0.007(8) 0.048(9) 0.014(8) C32 0.088(10) 0.077(10) 0.056(9) -0.015(8) 0.004(7) 0.021(8) C33 0.072(8) 0.055(8) 0.051(7) -0.006(6) 0.001(6) 0.025(6) C34 0.044(6) 0.031(6) 0.027(5) 0.005(4) 0.004(4) 0.017(4) C35 0.039(5) 0.030(5) 0.023(5) -0.004(4) 0.000(4) 0.008(4) C36 0.040(5) 0.035(6) 0.022(5) 0.005(4) 0.003(4) 0.015(4) C37 0.043(6) 0.051(7) 0.039(6) 0.013(5) 0.002(5) 0.016(5) C38 0.062(7) 0.046(7) 0.038(6) 0.004(5) -0.004(5) 0.020(5) C39 0.047(6) 0.073(8) 0.048(7) 0.034(6) 0.016(5) 0.027(6) C40 0.055(7) 0.045(7) 0.057(7) 0.009(6) 0.021(6) 0.007(5) C41 0.054(7) 0.046(7) 0.051(7) 0.004(6) -0.002(6) 0.008(5) C42 0.078(8) 0.037(6) 0.047(7) 0.006(5) 0.005(6) 0.026(6) C43 0.034(5) 0.024(5) 0.030(5) 0.001(4) 0.004(4) 0.010(4) C44 0.041(6) 0.034(6) 0.045(6) 0.008(5) 0.006(5) 0.022(5) C45 0.039(6) 0.036(6) 0.040(6) 0.001(5) -0.001(5) 0.010(5) C46 0.046(6) 0.031(6) 0.033(6) 0.005(5) 0.009(5) 0.016(5) C47 0.063(7) 0.029(6) 0.039(6) 0.008(5) 0.010(5) 0.015(5) C48 0.045(6) 0.040(6) 0.024(5) 0.003(5) -0.002(4) 0.013(5) C49 0.059(7) 0.032(6) 0.040(6) 0.011(5) 0.006(5) 0.010(6) C50 0.062(7) 0.046(7) 0.047(7) 0.002(6) 0.014(6) 0.008(6) C51 0.104(11) 0.039(8) 0.050(8) 0.002(6) -0.004(7) -0.001(8) C52 0.136(14) 0.033(8) 0.063(9) 0.012(7) -0.009(9) 0.003(9) C53 0.129(13) 0.045(8) 0.051(8) 0.006(6) -0.009(8) 0.039(8) C54 0.095(9) 0.031(7) 0.052(7) 0.003(5) 0.006(7) 0.023(6) C55 0.049(6) 0.028(5) 0.036(6) 0.004(5) 0.005(5) 0.015(5) C56 0.054(6) 0.040(6) 0.031(6) 0.011(5) 0.011(5) 0.023(5) C57 0.055(6) 0.037(6) 0.042(7) 0.011(5) 0.004(5) 0.025(5) C58 0.052(6) 0.032(6) 0.026(6) 0.007(5) 0.003(5) 0.010(5) C59 0.065(7) 0.053(7) 0.033(6) 0.008(5) 0.012(5) 0.029(6) C60 0.056(7) 0.040(6) 0.042(7) 0.004(5) 0.003(5) 0.024(5) C61 0.055(7) 0.042(6) 0.031(6) 0.011(5) -0.003(5) 0.007(5) C62 0.075(8) 0.063(8) 0.035(7) 0.015(6) 0.008(6) 0.032(6) C63 0.089(10) 0.099(11) 0.046(8) 0.019(8) 0.001(7) 0.042(8) C64 0.125(13) 0.099(11) 0.041(8) 0.020(8) 0.005(9) 0.055(10) C65 0.107(12) 0.108(12) 0.052(9) 0.038(8) 0.036(8) 0.035(10) C66 0.068(8) 0.090(10) 0.056(8) 0.040(7) 0.023(7) 0.031(7) C67 0.041(6) 0.050(7) 0.026(6) 0.004(5) 0.002(4) 0.029(5) C68 0.035(5) 0.035(6) 0.031(6) 0.005(5) 0.001(4) 0.017(4) C69 0.031(5) 0.035(6) 0.027(5) 0.000(4) -0.005(4) 0.012(4) C70 0.059(8) 0.091(10) 0.054(8) 0.016(7) 0.017(6) 0.023(7) C71 0.102(10) 0.118(12) 0.041(7) 0.011(8) 0.024(7) 0.068(9) C72 0.081(9) 0.106(11) 0.033(7) 0.013(7) 0.009(6) 0.042(8) C73 0.044(7) 0.055(8) 0.103(11) 0.020(7) 0.013(7) 0.012(6) C74 0.077(8) 0.048(7) 0.065(8) -0.003(6) -0.009(7) 0.010(6) C75 0.053(7) 0.048(7) 0.060(8) 0.017(6) 0.002(6) 0.010(5) C76 0.057(6) 0.032(6) 0.020(5) 0.000(4) 0.001(5) 0.020(5) C77 0.055(6) 0.039(6) 0.033(6) -0.008(5) 0.000(5) 0.028(5) C78 0.045(6) 0.051(7) 0.031(6) -0.005(5) -0.009(5) 0.021(5) C79 0.048(6) 0.039(6) 0.038(6) 0.001(5) 0.002(5) 0.025(5) C80 0.056(7) 0.059(8) 0.033(6) -0.007(5) -0.008(5) 0.033(6) C81 0.054(6) 0.043(7) 0.032(6) 0.004(5) -0.004(5) 0.023(5) C82 0.047(7) 0.044(7) 0.047(7) 0.006(5) -0.001(5) 0.013(6) C83 0.069(9) 0.044(7) 0.077(9) 0.004(6) 0.003(7) 0.014(6) C84 0.062(8) 0.070(10) 0.083(10) 0.006(8) -0.009(7) 0.011(8) C85 0.066(9) 0.044(8) 0.102(11) 0.005(7) -0.006(8) 0.012(7) C86 0.092(10) 0.036(7) 0.091(10) 0.016(7) 0.009(8) 0.024(7) C87 0.059(7) 0.040(7) 0.069(8) 0.010(6) 0.007(6) 0.017(6) C88 0.038(5) 0.035(6) 0.030(6) 0.002(5) 0.004(4) 0.014(5) C89 0.041(6) 0.038(6) 0.026(6) -0.006(5) -0.007(4) 0.011(5) C90 0.047(6) 0.042(6) 0.040(7) 0.004(5) -0.002(5) 0.015(5) C91 0.036(6) 0.049(7) 0.039(7) 0.004(5) 0.004(5) 0.008(5) C92 0.050(6) 0.042(6) 0.038(7) -0.004(5) 0.007(5) 0.023(5) C93 0.040(6) 0.043(6) 0.033(6) 0.005(5) -0.002(5) 0.019(5) C94 0.049(6) 0.056(7) 0.029(6) 0.008(6) 0.002(5) 0.015(6) C95 0.062(7) 0.074(9) 0.046(7) 0.020(6) -0.003(6) 0.029(6) C96 0.080(9) 0.088(10) 0.059(9) 0.025(8) 0.009(7) 0.041(8) C97 0.080(9) 0.097(11) 0.033(7) 0.011(8) -0.006(6) 0.040(8) C98 0.065(8) 0.087(10) 0.050(8) -0.007(7) -0.008(6) 0.026(7) C99 0.062(7) 0.068(8) 0.036(7) 0.003(6) -0.009(6) 0.019(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sm1 N3 2.317(7) . ? Sm1 N2 2.380(8) . ? Sm1 N1 2.411(7) . ? Sm1 N4 2.464(7) . ? Sm1 C36 2.590(9) . ? Sm1 C34 2.623(9) . ? Sm1 C35 2.644(9) . ? Sm1 C2 2.772(10) . ? Sm1 C3 2.784(9) . ? Sm1 C1 2.803(10) . ? Sm1 Si4 3.343(3) . ? Sm2 N6 2.303(7) . ? Sm2 N5 2.320(7) . ? Sm2 N4 2.407(7) . ? Sm2 N3 2.488(7) . ? Sm2 C67 2.694(9) . ? Sm2 C34 2.697(9) . ? Sm2 C35 2.726(9) . ? Sm2 C36 2.730(8) . ? Sm2 C68 2.742(9) . ? Sm2 C69 2.763(9) . ? Sm2 Si3 3.294(3) . ? Si1 N1 1.758(8) . ? Si1 C4 1.838(11) . ? Si1 C5 1.852(12) . ? Si1 C6 1.881(12) . ? Si2 N2 1.759(8) . ? Si2 C7 1.837(13) . ? Si2 C9 1.859(11) . ? Si2 C8 1.871(12) . ? Si3 N3 1.728(7) . ? Si3 C37 1.855(9) . ? Si3 C38 1.867(10) . ? Si3 C39 1.880(9) . ? Si4 N4 1.738(7) . ? Si4 C42 1.838(10) . ? Si4 C41 1.860(10) . ? Si4 C40 1.874(10) . ? Si5 N5 1.732(8) . ? Si5 C70 1.859(11) . ? Si5 C71 1.894(12) . ? Si5 C72 1.901(11) . ? Si6 N6 1.720(8) . ? Si6 C75 1.848(10) . ? Si6 C73 1.862(11) . ? Si6 C74 1.868(11) . ? N1 C1 1.328(12) . ? N2 C3 1.353(12) . ? N3 C34 1.447(9) . ? N4 C36 1.417(9) . ? N5 C67 1.420(9) . ? N6 C69 1.390(9) . ? C1 C2 1.430(13) . ? C1 C10 1.521(14) . ? C2 C3 1.424(13) . ? C3 C22 1.508(13) . ? C10 C11 1.378(13) . ? C10 C15 1.386(14) . ? C11 C12 1.394(14) . ? C12 C13 1.377(14) . ? C13 C14 1.401(13) . ? C13 C16 1.483(14) . ? C14 C15 1.365(14) . ? C16 C17 1.358(14) . ? C16 C21 1.374(15) . ? C17 C18 1.390(15) . ? C18 C19 1.338(17) . ? C19 C20 1.356(17) . ? C20 C21 1.381(16) . ? C22 C23 1.388(14) . ? C22 C27 1.395(13) . ? C23 C24 1.380(15) . ? C24 C25 1.371(15) . ? C25 C26 1.396(14) . ? C25 C28 1.479(14) . ? C26 C27 1.395(13) . ? C28 C29 1.362(15) . ? C28 C33 1.368(11) . ? C29 C30 1.413(16) . ? C30 C31 1.323(15) . ? C31 C32 1.321(18) . ? C32 C33 1.401(16) . ? C34 C35 1.427(12) . ? C34 C43 1.484(12) . ? C35 C36 1.421(12) . ? C36 C55 1.497(13) . ? C43 C48 1.388(12) . ? C43 C44 1.415(13) . ? C44 C45 1.366(13) . ? C45 C46 1.380(13) . ? C46 C47 1.373(13) . ? C46 C49 1.483(13) . ? C47 C48 1.393(13) . ? C49 C54 1.379(15) . ? C49 C50 1.387(14) . ? C50 C51 1.390(16) . ? C51 C52 1.335(19) . ? C52 C53 1.353(19) . ? C53 C54 1.416(15) . ? C55 C60 1.387(13) . ? C55 C56 1.389(13) . ? C56 C57 1.383(13) . ? C57 C58 1.375(13) . ? C58 C59 1.385(14) . ? C58 C61 1.473(13) . ? C59 C60 1.394(14) . ? C61 C66 1.375(14) . ? C61 C62 1.379(15) . ? C62 C63 1.380(15) . ? C63 C64 1.364(18) . ? C64 C65 1.359(19) . ? C65 C66 1.406(17) . ? C67 C68 1.408(12) . ? C67 C76 1.450(13) . ? C68 C69 1.431(12) . ? C69 C88 1.484(13) . ? C76 C81 1.389(13) . ? C76 C77 1.402(13) . ? C77 C78 1.378(13) . ? C78 C79 1.380(13) . ? C79 C80 1.389(13) . ? C79 C82 1.463(14) . ? C80 C81 1.400(14) . ? C82 C83 1.365(15) . ? C82 C87 1.400(14) . ? C83 C84 1.433(16) . ? C84 C85 1.352(17) . ? C85 C86 1.361(17) . ? C86 C87 1.403(15) . ? C88 C89 1.381(13) . ? C88 C93 1.394(13) . ? C89 C90 1.390(13) . ? C90 C91 1.394(14) . ? C91 C92 1.400(14) . ? C91 C94 1.500(14) . ? C92 C93 1.373(13) . ? C94 C95 1.369(15) . ? C94 C99 1.373(15) . ? C95 C96 1.416(16) . ? C96 C97 1.350(17) . ? C97 C98 1.332(17) . ? C98 C99 1.389(16) . ? C100 C101 1.82(3) . ? C101 C102 1.84(3) . ? C102 C103 1.79(3) . ? C103 C104 1.82(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 N3 Sm1 N2 121.4(3) . . ? N3 Sm1 N1 116.6(2) . . ? N2 Sm1 N1 79.1(3) . . ? N3 Sm1 N4 75.1(2) . . ? N2 Sm1 N4 135.7(3) . . ? N1 Sm1 N4 133.8(2) . . ? N3 Sm1 C36 77.67(19) . . ? N2 Sm1 C36 106.1(2) . . ? N1 Sm1 C36 160.1(2) . . ? N4 Sm1 C36 32.4(2) . . ? N3 Sm1 C34 33.34(19) . . ? N2 Sm1 C34 97.1(2) . . ? N1 Sm1 C34 139.45(19) . . ? N4 Sm1 C34 75.6(2) . . ? C36 Sm1 C34 59.9(3) . . ? N3 Sm1 C35 59.39(19) . . ? N2 Sm1 C35 93.38(19) . . ? N1 Sm1 C35 167.9(2) . . ? N4 Sm1 C35 57.78(19) . . ? C36 Sm1 C35 31.5(3) . . ? C34 Sm1 C35 31.4(3) . . ? N3 Sm1 C2 85.4(3) . . ? N2 Sm1 C2 56.4(3) . . ? N1 Sm1 C2 55.6(3) . . ? N4 Sm1 C2 160.5(2) . . ? C36 Sm1 C2 143.2(2) . . ? C34 Sm1 C2 88.44(19) . . ? C35 Sm1 C2 112.3(2) . . ? N3 Sm1 C3 98.2(3) . . ? N2 Sm1 C3 29.1(3) . . ? N1 Sm1 C3 72.6(3) . . ? N4 Sm1 C3 153.2(3) . . ? C36 Sm1 C3 121.2(2) . . ? C34 Sm1 C3 84.72(19) . . ? C35 Sm1 C3 96.25(19) . . ? C2 Sm1 C3 29.7(3) . . ? N3 Sm1 C1 95.4(3) . . ? N2 Sm1 C1 73.3(3) . . ? N1 Sm1 C1 28.2(3) . . ? N4 Sm1 C1 150.4(3) . . ? C36 Sm1 C1 171.6(2) . . ? C34 Sm1 C1 111.7(2) . . ? C35 Sm1 C1 140.3(2) . . ? C2 Sm1 C1 29.7(3) . . ? C3 Sm1 C1 54.6(3) . . ? N3 Sm1 Si4 99.86(18) . . ? N2 Sm1 Si4 131.0(2) . . ? N1 Sm1 Si4 106.69(19) . . ? N4 Sm1 Si4 30.26(16) . . ? C36 Sm1 Si4 55.2(2) . . ? C34 Sm1 Si4 105.83(19) . . ? C35 Sm1 Si4 85.41(19) . . ? C2 Sm1 Si4 161.4(2) . . ? C3 Sm1 Si4 159.9(2) . . ? C1 Sm1 Si4 131.7(2) . . ? N3 Sm1 Sm2 38.23(17) . . ? N2 Sm1 Sm2 137.53(19) . . ? N1 Sm1 Sm2 139.86(18) . . ? N4 Sm1 Sm2 37.20(16) . . ? C36 Sm1 Sm2 45.05(18) . . ? C34 Sm1 Sm2 44.34(19) . . ? C35 Sm1 Sm2 44.99(19) . . ? C2 Sm1 Sm2 123.44(18) . . ? C3 Sm1 Sm2 128.80(18) . . ? C1 Sm1 Sm2 130.15(19) . . ? Si4 Sm1 Sm2 64.97(5) . . ? N6 Sm2 N5 85.3(3) . . ? N6 Sm2 N4 124.7(3) . . ? N5 Sm2 N4 121.4(3) . . ? N6 Sm2 N3 129.9(2) . . ? N5 Sm2 N3 128.2(2) . . ? N4 Sm2 N3 73.1(2) . . ? N6 Sm2 C67 79.3(2) . . ? N5 Sm2 C67 31.81(19) . . ? N4 Sm2 C67 99.3(2) . . ? N3 Sm2 C67 149.3(2) . . ? N6 Sm2 C34 101.6(2) . . ? N5 Sm2 C34 154.09(18) . . ? N4 Sm2 C34 75.11(18) . . ? N3 Sm2 C34 32.09(19) . . ? C67 Sm2 C34 173.8(3) . . ? N6 Sm2 C35 92.04(19) . . ? N5 Sm2 C35 175.23(19) . . ? N4 Sm2 C35 57.19(18) . . ? N3 Sm2 C35 56.43(19) . . ? C67 Sm2 C35 143.7(3) . . ? C34 Sm2 C35 30.5(3) . . ? N6 Sm2 C36 100.34(19) . . ? N5 Sm2 C36 146.61(19) . . ? N4 Sm2 C36 31.21(19) . . ? N3 Sm2 C36 72.27(19) . . ? C67 Sm2 C36 116.5(3) . . ? C34 Sm2 C36 57.3(3) . . ? C35 Sm2 C36 30.2(3) . . ? N6 Sm2 C68 57.97(19) . . ? N5 Sm2 C68 57.68(18) . . ? N4 Sm2 C68 94.35(18) . . ? N3 Sm2 C68 167.39(19) . . ? C67 Sm2 C68 30.0(3) . . ? C34 Sm2 C68 146.2(3) . . ? C35 Sm2 C68 117.6(3) . . ? C36 Sm2 C68 97.4(3) . . ? N6 Sm2 C69 30.14(18) . . ? N5 Sm2 C69 76.90(19) . . ? N4 Sm2 C69 104.37(18) . . ? N3 Sm2 C69 152.86(19) . . ? C67 Sm2 C69 57.5(3) . . ? C34 Sm2 C69 120.8(3) . . ? C35 Sm2 C69 98.8(3) . . ? C36 Sm2 C69 91.5(3) . . ? C68 Sm2 C69 30.1(3) . . ? N6 Sm2 Si3 130.59(19) . . ? N5 Sm2 Si3 98.20(19) . . ? N4 Sm2 Si3 95.21(17) . . ? N3 Sm2 Si3 30.97(16) . . ? C67 Sm2 Si3 125.72(19) . . ? C34 Sm2 Si3 58.32(19) . . ? C35 Sm2 Si3 86.53(19) . . ? C36 Sm2 Si3 102.45(19) . . ? C68 Sm2 Si3 155.42(19) . . ? C69 Sm2 Si3 159.48(18) . . ? N6 Sm2 Sm1 135.30(19) . . ? N5 Sm2 Sm1 139.07(19) . . ? N4 Sm2 Sm1 38.22(16) . . ? N3 Sm2 Sm1 35.18(15) . . ? C67 Sm2 Sm1 133.0(2) . . ? C34 Sm2 Sm1 42.82(19) . . ? C35 Sm2 Sm1 43.29(19) . . ? C36 Sm2 Sm1 42.16(19) . . ? C68 Sm2 Sm1 132.36(18) . . ? C69 Sm2 Sm1 133.70(18) . . ? Si3 Sm2 Sm1 61.79(5) . . ? N1 Si1 C4 109.1(5) . . ? N1 Si1 C5 115.3(5) . . ? C4 Si1 C5 110.1(7) . . ? N1 Si1 C6 106.3(5) . . ? C4 Si1 C6 108.8(6) . . ? C5 Si1 C6 106.9(7) . . ? N2 Si2 C7 107.5(5) . . ? N2 Si2 C9 104.9(5) . . ? C7 Si2 C9 111.8(6) . . ? N2 Si2 C8 116.0(5) . . ? C7 Si2 C8 109.0(7) . . ? C9 Si2 C8 107.6(6) . . ? N3 Si3 C37 121.0(3) . . ? N3 Si3 C38 102.1(3) . . ? C37 Si3 C38 106.2(5) . . ? N3 Si3 C39 110.5(3) . . ? C37 Si3 C39 106.3(4) . . ? C38 Si3 C39 110.4(5) . . ? N3 Si3 Sm2 47.8(2) . . ? C37 Si3 Sm2 166.3(3) . . ? C38 Si3 Sm2 85.5(3) . . ? C39 Si3 Sm2 75.2(3) . . ? N4 Si4 C42 119.0(3) . . ? N4 Si4 C41 104.2(3) . . ? C42 Si4 C41 107.1(5) . . ? N4 Si4 C40 107.5(3) . . ? C42 Si4 C40 109.2(5) . . ? C41 Si4 C40 109.5(5) . . ? N4 Si4 Sm1 45.6(2) . . ? C42 Si4 Sm1 164.3(3) . . ? C41 Si4 Sm1 82.6(3) . . ? C40 Si4 Sm1 77.8(3) . . ? N5 Si5 C70 109.0(4) . . ? N5 Si5 C71 113.3(4) . . ? C70 Si5 C71 108.2(6) . . ? N5 Si5 C72 111.9(3) . . ? C70 Si5 C72 106.9(6) . . ? C71 Si5 C72 107.3(6) . . ? N6 Si6 C75 107.2(3) . . ? N6 Si6 C73 110.1(4) . . ? C75 Si6 C73 108.3(5) . . ? N6 Si6 C74 118.9(4) . . ? C75 Si6 C74 106.3(5) . . ? C73 Si6 C74 105.6(6) . . ? C1 N1 Si1 125.3(7) . . ? C1 N1 Sm1 92.5(6) . . ? Si1 N1 Sm1 142.1(4) . . ? C3 N2 Si2 124.3(7) . . ? C3 N2 Sm1 92.3(6) . . ? Si2 N2 Sm1 143.4(5) . . ? C34 N3 Si3 137.9(5) . . ? C34 N3 Sm1 85.0(3) . . ? Si3 N3 Sm1 131.9(4) . . ? C34 N3 Sm2 81.9(4) . . ? Si3 N3 Sm2 101.2(3) . . ? Sm1 N3 Sm2 106.6(3) . . ? C36 N4 Si4 127.0(5) . . ? C36 N4 Sm2 87.1(3) . . ? Si4 N4 Sm2 139.0(4) . . ? C36 N4 Sm1 78.7(4) . . ? Si4 N4 Sm1 104.1(3) . . ? Sm2 N4 Sm1 104.6(2) . . ? C67 N5 Si5 121.7(5) . . ? C67 N5 Sm2 88.8(4) . . ? Si5 N5 Sm2 149.4(4) . . ? C69 N6 Si6 127.8(5) . . ? C69 N6 Sm2 93.5(4) . . ? Si6 N6 Sm2 138.3(4) . . ? N1 C1 C2 124.2(9) . . ? N1 C1 C10 122.0(9) . . ? C2 C1 C10 113.6(9) . . ? N1 C1 Sm1 59.2(5) . . ? C2 C1 Sm1 73.9(5) . . ? C10 C1 Sm1 143.9(6) . . ? C3 C2 C1 127.7(9) . . ? C3 C2 Sm1 75.6(5) . . ? C1 C2 Sm1 76.3(6) . . ? N2 C3 C2 124.6(9) . . ? N2 C3 C22 119.8(9) . . ? C2 C3 C22 115.6(8) . . ? N2 C3 Sm1 58.6(5) . . ? C2 C3 Sm1 74.7(5) . . ? C22 C3 Sm1 146.2(6) . . ? C11 C10 C15 118.8(10) . . ? C11 C10 C1 121.6(9) . . ? C15 C10 C1 119.5(9) . . ? C10 C11 C12 119.4(10) . . ? C13 C12 C11 122.8(10) . . ? C12 C13 C14 116.2(9) . . ? C12 C13 C16 121.3(10) . . ? C14 C13 C16 122.4(9) . . ? C15 C14 C13 121.7(10) . . ? C14 C15 C10 121.0(10) . . ? C17 C16 C21 117.1(10) . . ? C17 C16 C13 122.0(10) . . ? C21 C16 C13 120.9(10) . . ? C16 C17 C18 121.8(11) . . ? C19 C18 C17 119.0(11) . . ? C18 C19 C20 121.6(12) . . ? C19 C20 C21 118.5(12) . . ? C16 C21 C20 121.9(11) . . ? C23 C22 C27 118.7(9) . . ? C23 C22 C3 120.9(9) . . ? C27 C22 C3 120.4(9) . . ? C24 C23 C22 119.7(10) . . ? C25 C24 C23 122.8(11) . . ? C24 C25 C26 117.7(10) . . ? C24 C25 C28 122.5(10) . . ? C26 C25 C28 119.8(10) . . ? C27 C26 C25 120.4(10) . . ? C26 C27 C22 120.6(9) . . ? C29 C28 C33 117.2(9) . . ? C29 C28 C25 122.1(10) . . ? C33 C28 C25 120.6(9) . . ? C28 C29 C30 119.7(12) . . ? C31 C30 C29 121.9(11) . . ? C32 C31 C30 119.2(12) . . ? C31 C32 C33 120.9(13) . . ? C28 C33 C32 121.1(11) . . ? C35 C34 N3 118.8(7) . . ? C35 C34 C43 119.4(8) . . ? N3 C34 C43 121.8(7) . . ? C35 C34 Sm1 75.1(5) . . ? N3 C34 Sm1 61.6(3) . . ? C43 C34 Sm1 134.8(6) . . ? C35 C34 Sm2 75.9(5) . . ? N3 C34 Sm2 66.0(3) . . ? C43 C34 Sm2 131.3(6) . . ? Sm1 C34 Sm2 92.8(3) . . ? C36 C35 C34 132.1(8) . . ? C36 C35 Sm1 72.1(5) . . ? C34 C35 Sm1 73.5(5) . . ? C36 C35 Sm2 75.1(5) . . ? C34 C35 Sm2 73.6(5) . . ? Sm1 C35 Sm2 91.7(3) . . ? N4 C36 C35 121.2(7) . . ? N4 C36 C55 121.0(7) . . ? C35 C36 C55 117.1(8) . . ? N4 C36 Sm1 68.9(3) . . ? C35 C36 Sm1 76.4(5) . . ? C55 C36 Sm1 136.5(6) . . ? N4 C36 Sm2 61.7(3) . . ? C35 C36 Sm2 74.7(5) . . ? C55 C36 Sm2 130.1(6) . . ? Sm1 C36 Sm2 92.8(3) . . ? C48 C43 C44 115.7(8) . . ? C48 C43 C34 123.2(8) . . ? C44 C43 C34 121.2(8) . . ? C45 C44 C43 121.4(9) . . ? C44 C45 C46 122.8(9) . . ? C47 C46 C45 116.3(9) . . ? C47 C46 C49 121.4(9) . . ? C45 C46 C49 122.3(9) . . ? C46 C47 C48 122.2(9) . . ? C43 C48 C47 121.6(9) . . ? C54 C49 C50 117.7(10) . . ? C54 C49 C46 120.0(10) . . ? C50 C49 C46 122.3(10) . . ? C49 C50 C51 120.6(12) . . ? C52 C51 C50 121.6(14) . . ? C51 C52 C53 119.3(13) . . ? C52 C53 C54 121.0(13) . . ? C49 C54 C53 119.7(12) . . ? C60 C55 C56 116.4(9) . . ? C60 C55 C36 122.3(9) . . ? C56 C55 C36 121.3(8) . . ? C57 C56 C55 122.2(9) . . ? C58 C57 C56 121.7(9) . . ? C57 C58 C59 116.4(9) . . ? C57 C58 C61 122.4(9) . . ? C59 C58 C61 121.2(9) . . ? C58 C59 C60 122.4(9) . . ? C55 C60 C59 120.8(9) . . ? C66 C61 C62 117.9(10) . . ? C66 C61 C58 120.9(10) . . ? C62 C61 C58 121.2(9) . . ? C61 C62 C63 121.8(11) . . ? C64 C63 C62 120.8(13) . . ? C65 C64 C63 117.8(12) . . ? C64 C65 C66 122.4(12) . . ? C61 C66 C65 119.2(12) . . ? C68 C67 N5 121.6(8) . . ? C68 C67 C76 118.3(8) . . ? N5 C67 C76 119.4(7) . . ? C68 C67 Sm2 76.9(5) . . ? N5 C67 Sm2 59.4(3) . . ? C76 C67 Sm2 131.4(6) . . ? C67 C68 C69 135.3(9) . . ? C67 C68 Sm2 73.1(5) . . ? C69 C68 Sm2 75.7(5) . . ? N6 C69 C68 122.6(7) . . ? N6 C69 C88 121.4(7) . . ? C68 C69 C88 115.6(8) . . ? N6 C69 Sm2 56.3(3) . . ? C68 C69 Sm2 74.2(5) . . ? C88 C69 Sm2 144.4(6) . . ? C81 C76 C77 117.2(9) . . ? C81 C76 C67 121.7(9) . . ? C77 C76 C67 121.1(8) . . ? C78 C77 C76 121.6(9) . . ? C77 C78 C79 122.2(9) . . ? C78 C79 C80 115.9(9) . . ? C78 C79 C82 122.3(9) . . ? C80 C79 C82 121.7(9) . . ? C79 C80 C81 123.2(10) . . ? C76 C81 C80 119.6(9) . . ? C83 C82 C87 117.9(10) . . ? C83 C82 C79 121.0(10) . . ? C87 C82 C79 121.1(9) . . ? C82 C83 C84 119.9(12) . . ? C85 C84 C83 121.4(12) . . ? C84 C85 C86 119.0(12) . . ? C85 C86 C87 120.9(12) . . ? C82 C87 C86 120.8(11) . . ? C89 C88 C93 116.2(9) . . ? C89 C88 C69 121.8(8) . . ? C93 C88 C69 122.0(9) . . ? C88 C89 C90 123.2(9) . . ? C89 C90 C91 119.9(10) . . ? C90 C91 C92 117.3(9) . . ? C90 C91 C94 120.1(10) . . ? C92 C91 C94 122.6(10) . . ? C93 C92 C91 121.6(9) . . ? C92 C93 C88 121.8(9) . . ? C95 C94 C99 118.5(10) . . ? C95 C94 C91 120.8(10) . . ? C99 C94 C91 120.7(10) . . ? C94 C95 C96 119.6(12) . . ? C97 C96 C95 121.4(13) . . ? C98 C97 C96 117.9(12) . . ? C97 C98 C99 123.1(13) . . ? C94 C99 C98 119.5(12) . . ? C100 C101 C102 81.0(16) . . ? C103 C102 C101 82.2(17) . . ? C102 C103 C104 83.3(17) . . ? #===END data_(6)-may1101 _database_code_depnum_ccdc_archive 'CCDC 768772' #TrackingRef 'MFL-Dalton-feb2010[1].cif' _audit_creation_date 2010-02-24T11:18:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C52 H81 N4 Si4 Sm, 0.5(C8), 0.5(C6)' _chemical_formula_sum 'C59 H81 N4 Si4 Sm' _chemical_formula_weight 1109.00 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 16.0256(6) _cell_length_b 18.5440(9) _cell_length_c 20.9627(7) _cell_angle_alpha 90 _cell_angle_beta 104.300(2) _cell_angle_gamma 90 _cell_volume 6036.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 45938 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour Black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.686 _exptl_absorpt_correction_T_max 0.840 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_unetI/netI 0.0482 _diffrn_reflns_number 27143 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 23 _diffrn_reflns_theta_full 23 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 8331 _reflns_number_gt 6791 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There are two regions of poorly defined residual density presumably due to uncharacterized solvate molecules. This was modeled by including seven isotropic carbon atoms in the refinement. 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^)+(0.0280P)^2^+12.4551P] 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_number_reflns 8331 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.057 _refine_ls_R_factor_gt 0.041 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.661 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Sm Sm 0.255391(14) 0.348793(14) 0.262677(12) 0.04062(10) Uani 1 1 d . A 1 Si1 Si 0.04335(9) 0.27105(8) 0.28869(7) 0.0514(4) Uani 1 1 d . A 1 Si2 Si 0.31387(7) 0.38725(7) 0.43752(6) 0.0388(3) Uani 1 1 d . A 1 Si3 Si 0.18802(8) 0.35747(8) 0.07534(6) 0.0460(3) Uani 1 1 d . A 1 Si4 Si 0.39420(9) 0.22989(8) 0.24432(8) 0.0553(4) Uani 1 1 d . A 1 N1 N 0.1109(2) 0.3418(2) 0.27809(17) 0.0406(9) Uani 1 1 d . A 1 N2 N 0.2662(2) 0.4207(2) 0.36055(16) 0.0350(9) Uani 1 1 d . A 1 N3 N 0.2351(2) 0.3888(2) 0.15350(17) 0.0409(9) Uani 1 1 d . A 1 N4 N 0.3918(2) 0.3239(2) 0.24363(19) 0.0466(10) Uani 1 1 d . A 1 C1 C 0.0921(3) 0.4097(3) 0.2615(2) 0.0385(11) Uani 1 1 d . A 1 C2 C 0.1495(2) 0.4693(3) 0.2775(2) 0.0357(10) Uani 1 1 d . A 1 H2 H 0.1368 0.5092 0.2482 0.043 Uiso 1 1 calc R A 1 C3 C 0.2229(3) 0.4776(3) 0.3308(2) 0.0358(11) Uani 1 1 d . A 1 C4 C 0.1012(4) 0.2228(3) 0.3641(3) 0.0778(19) Uani 1 1 d . A 1 H4A H 0.1566 0.2053 0.3583 0.117 Uiso 1 1 calc R A 1 H4B H 0.0665 0.1819 0.372 0.117 Uiso 1 1 calc R A 1 H4C H 0.1113 0.2558 0.4017 0.117 Uiso 1 1 calc R A 1 C5 C 0.0272(4) 0.2045(3) 0.2203(3) 0.0670(16) Uani 1 1 d . A 1 H5A H -0.0066 0.1637 0.2299 0.101 Uiso 1 1 calc R A 1 H5B H 0.0833 0.1873 0.2158 0.101 Uiso 1 1 calc R A 1 H5C H -0.0037 0.2275 0.1791 0.101 Uiso 1 1 calc R A 1 C6 C -0.0626(3) 0.3022(4) 0.3006(3) 0.0738(18) Uani 1 1 d . A 1 H6A H -0.0949 0.2607 0.311 0.111 Uiso 1 1 calc R A 1 H6B H -0.0956 0.3253 0.2601 0.111 Uiso 1 1 calc R A 1 H6C H -0.053 0.3369 0.3369 0.111 Uiso 1 1 calc R A 1 C7 C 0.0057(3) 0.4298(3) 0.2171(2) 0.0431(12) Uani 1 1 d . A 1 C8 C -0.0407(3) 0.4885(3) 0.2303(3) 0.0561(14) Uani 1 1 d . A 1 H8 H -0.0185 0.5169 0.2684 0.067 Uiso 1 1 calc R A 1 C9 C -0.1201(3) 0.5061(4) 0.1879(3) 0.0708(18) Uani 1 1 d . A 1 H9 H -0.1519 0.546 0.1978 0.085 Uiso 1 1 calc R A 1 C10 C -0.1527(3) 0.4659(4) 0.1316(3) 0.0719(19) Uani 1 1 d . A 1 C11 C -0.1062(4) 0.4085(4) 0.1186(3) 0.0710(18) Uani 1 1 d . A 1 H11 H -0.1279 0.3809 0.0798 0.085 Uiso 1 1 calc R A 1 C12 C -0.0281(3) 0.3894(3) 0.1604(2) 0.0559(14) Uani 1 1 d . A 1 H12 H 0.0025 0.3488 0.1506 0.067 Uiso 1 1 calc R A 1 C13 C -0.2389(4) 0.4860(5) 0.0860(4) 0.114(3) Uani 1 1 d . A 1 H13A H -0.2793 0.4457 0.0834 0.171 Uiso 0.5 1 calc PR A 1 H13B H -0.2312 0.4964 0.042 0.171 Uiso 0.5 1 calc PR A 1 H13C H -0.262 0.5287 0.1033 0.171 Uiso 0.5 1 calc PR A 1 H13D H -0.2357 0.5349 0.0691 0.171 Uiso 0.5 1 calc PR A 1 H13E H -0.2838 0.4842 0.1105 0.171 Uiso 0.5 1 calc PR A 1 H13F H -0.253 0.4519 0.0492 0.171 Uiso 0.5 1 calc PR A 1 C14 C 0.2526(3) 0.5548(3) 0.3529(2) 0.0369(11) Uani 1 1 d . A 1 C15 C 0.2074(3) 0.6143(3) 0.3044(2) 0.0465(12) Uani 1 1 d . A 1 H15A H 0.2194 0.6064 0.2608 0.056 Uiso 1 1 calc R A 1 H15B H 0.1444 0.6114 0.2989 0.056 Uiso 1 1 calc R A 1 C16 C 0.2401(3) 0.6900(3) 0.3306(3) 0.0576(14) Uani 1 1 d . A 1 H16 H 0.2108 0.7276 0.2986 0.069 Uiso 1 1 calc R A 1 C17 C 0.2186(4) 0.7022(3) 0.3966(3) 0.0624(15) Uani 1 1 d . A 1 H17A H 0.1555 0.6999 0.391 0.075 Uiso 1 1 calc R A 1 H17B H 0.2386 0.7506 0.4137 0.075 Uiso 1 1 calc R A 1 C18 C 0.2628(3) 0.6443(3) 0.4457(2) 0.0506(13) Uani 1 1 d . A 1 H18 H 0.2488 0.6523 0.4891 0.061 Uiso 1 1 calc R A 1 C19 C 0.2312(3) 0.5698(3) 0.4193(2) 0.0445(12) Uani 1 1 d . A 1 H19A H 0.1682 0.5667 0.4137 0.053 Uiso 1 1 calc R A 1 H19B H 0.2587 0.5326 0.4515 0.053 Uiso 1 1 calc R A 1 C20 C 0.3505(3) 0.5626(3) 0.3612(2) 0.0396(11) Uani 1 1 d . A 1 H20A H 0.381 0.5253 0.392 0.048 Uiso 1 1 calc R A 1 H20B H 0.3642 0.555 0.3181 0.048 Uiso 1 1 calc R A 1 C21 C 0.3817(3) 0.6374(3) 0.3876(2) 0.0496(13) Uani 1 1 d . A 1 H21 H 0.4454 0.6407 0.3934 0.06 Uiso 1 1 calc R A 1 C22 C 0.3602(3) 0.6497(3) 0.4542(2) 0.0499(12) Uani 1 1 d . A 1 H22A H 0.3897 0.613 0.4862 0.06 Uiso 1 1 calc R A 1 H22B H 0.3807 0.6979 0.4715 0.06 Uiso 1 1 calc R A 1 C23 C 0.3373(3) 0.6950(3) 0.3389(3) 0.0586(14) Uani 1 1 d . A 1 H23A H 0.3512 0.6875 0.2959 0.07 Uiso 1 1 calc R A 1 H23B H 0.3581 0.7434 0.3554 0.07 Uiso 1 1 calc R A 1 C24 C 0.3545(3) 0.2964(3) 0.4222(3) 0.0572(14) Uani 1 1 d . A 1 H24A H 0.3761 0.2714 0.4642 0.086 Uiso 1 1 calc R A 1 H24B H 0.4013 0.3017 0.4 0.086 Uiso 1 1 calc R A 1 H24C H 0.3076 0.2684 0.3943 0.086 Uiso 1 1 calc R A 1 C25 C 0.2305(3) 0.3793(3) 0.4848(2) 0.0564(14) Uani 1 1 d . A 1 H25A H 0.2553 0.3558 0.5271 0.085 Uiso 1 1 calc R A 1 H25B H 0.1823 0.3503 0.4597 0.085 Uiso 1 1 calc R A 1 H25C H 0.2098 0.4274 0.4925 0.085 Uiso 1 1 calc R A 1 C26 C 0.4089(3) 0.4345(3) 0.4908(2) 0.0517(13) Uani 1 1 d . A 1 H26A H 0.4548 0.4378 0.4675 0.078 Uiso 1 1 calc R A 1 H26B H 0.4297 0.4073 0.5317 0.078 Uiso 1 1 calc R A 1 H26C H 0.3919 0.4831 0.501 0.078 Uiso 1 1 calc R A 1 C27 C 0.2853(3) 0.4481(3) 0.1686(2) 0.0370(11) Uani 1 1 d . A 1 C28 C 0.3657(3) 0.4488(3) 0.2151(2) 0.0399(11) Uani 1 1 d . A 1 H28 H 0.3855 0.4949 0.2321 0.048 Uiso 1 1 calc R A 1 C29 C 0.4218(3) 0.3893(3) 0.2404(2) 0.0424(11) Uani 1 1 d . A 1 C30 C 0.2755(3) 0.3498(3) 0.0317(3) 0.0630(15) Uani 1 1 d . A 1 H30A H 0.2959 0.3981 0.0239 0.095 Uiso 1 1 calc R A 1 H30B H 0.2535 0.3254 -0.0106 0.095 Uiso 1 1 calc R A 1 H30C H 0.3233 0.3219 0.0586 0.095 Uiso 1 1 calc R A 1 C31 C 0.1432(4) 0.2669(3) 0.0862(3) 0.0651(16) Uani 1 1 d . A 1 H31A H 0.1889 0.2363 0.1123 0.098 Uiso 1 1 calc R A 1 H31B H 0.1201 0.2448 0.043 0.098 Uiso 1 1 calc R A 1 H31C H 0.0971 0.272 0.109 0.098 Uiso 1 1 calc R A 1 C32 C 0.0991(3) 0.4110(3) 0.0214(2) 0.0647(16) Uani 1 1 d . A 1 H32A H 0.0786 0.3863 -0.0209 0.097 Uiso 1 1 calc R A 1 H32B H 0.1204 0.459 0.014 0.097 Uiso 1 1 calc R A 1 H32C H 0.0515 0.4157 0.0428 0.097 Uiso 1 1 calc R A 1 C33 C 0.2532(3) 0.5190(3) 0.1382(2) 0.0398(11) Uani 1 1 d . A 1 C34 C 0.1659(3) 0.5360(3) 0.1257(2) 0.0416(11) Uani 1 1 d . A 1 H34 H 0.1274 0.5018 0.1364 0.05 Uiso 1 1 calc R A 1 C35 C 0.1340(3) 0.6008(3) 0.0984(2) 0.0453(12) Uani 1 1 d . A 1 H35 H 0.0741 0.6104 0.0909 0.054 Uiso 1 1 calc R A 1 C36 C 0.1874(3) 0.6523(3) 0.0814(2) 0.0523(13) Uani 1 1 d . A 1 C37 C 0.2738(4) 0.6363(3) 0.0936(3) 0.0638(16) Uani 1 1 d . A 1 H37 H 0.3118 0.6706 0.0823 0.077 Uiso 1 1 calc R A 1 C38 C 0.3070(3) 0.5715(3) 0.1218(2) 0.0518(13) Uani 1 1 d . A 1 H38 H 0.3671 0.5626 0.1301 0.062 Uiso 1 1 calc R A 1 C39 C 0.1513(4) 0.7229(3) 0.0501(3) 0.0742(18) Uani 1 1 d . A 1 H39A H 0.1236 0.7489 0.08 0.111 Uiso 0.5 1 calc PR A 1 H39B H 0.1088 0.7132 0.0086 0.111 Uiso 0.5 1 calc PR A 1 H39C H 0.1981 0.7523 0.0414 0.111 Uiso 0.5 1 calc PR A 1 H39D H 0.1634 0.7274 0.0067 0.111 Uiso 0.5 1 calc PR A 1 H39E H 0.1782 0.7631 0.0781 0.111 Uiso 0.5 1 calc PR A 1 H39F H 0.0889 0.724 0.0452 0.111 Uiso 0.5 1 calc PR A 1 C40 C 0.5194(3) 0.4060(3) 0.2660(2) 0.0402(11) Uani 1 1 d . A 1 C41 C 0.5441(4) 0.4852(4) 0.2576(4) 0.093(2) Uani 1 1 d . A 1 H41A H 0.5128 0.5171 0.2816 0.111 Uiso 1 1 calc R A 1 H41B H 0.5271 0.4984 0.2104 0.111 Uiso 1 1 calc R A 1 C42 C 0.6437(4) 0.4965(4) 0.2848(4) 0.088(2) Uani 1 1 d . A 1 H42 H 0.6592 0.5478 0.2789 0.105 Uiso 1 1 calc R A 1 C43 C 0.6873(4) 0.4484(5) 0.2470(3) 0.099(3) Uani 1 1 d . A 1 H43A H 0.6686 0.4609 0.1997 0.118 Uiso 1 1 calc R A 1 H43B H 0.7503 0.4561 0.2615 0.118 Uiso 1 1 calc R A 1 C44 C 0.6682(4) 0.3718(5) 0.2556(5) 0.097(3) Uani 1 1 d . A 1 H44 H 0.7003 0.3408 0.2307 0.116 Uiso 1 1 calc R A 1 C45 C 0.5696(3) 0.3591(4) 0.2298(4) 0.091(2) Uani 1 1 d . A 1 H45A H 0.5519 0.3701 0.1822 0.109 Uiso 1 1 calc R A 1 H45B H 0.5564 0.3078 0.2358 0.109 Uiso 1 1 calc R A 1 C46 C 0.5462(4) 0.3911(6) 0.3388(3) 0.108(3) Uani 1 1 d . A 1 H46A H 0.5294 0.3414 0.3475 0.13 Uiso 1 1 calc R A 1 H46B H 0.5163 0.4249 0.3623 0.13 Uiso 1 1 calc R A 1 C47 C 0.6468(5) 0.4002(8) 0.3653(3) 0.126(4) Uani 1 1 d . A 1 H47 H 0.6653 0.3882 0.4132 0.151 Uiso 1 1 calc R A 1 C48 C 0.6906(4) 0.3512(5) 0.3260(6) 0.128(4) Uani 1 1 d . A 1 H48A H 0.7538 0.3541 0.3436 0.154 Uiso 1 1 calc R A 1 H48B H 0.6727 0.3007 0.3304 0.154 Uiso 1 1 calc R A 1 C49 C 0.6665(5) 0.4776(6) 0.3537(4) 0.116(3) Uani 1 1 d . A 1 H49A H 0.6346 0.5091 0.3775 0.139 Uiso 1 1 calc R A 1 H49B H 0.7288 0.4864 0.3718 0.139 Uiso 1 1 calc R A 1 C50 C 0.4069(4) 0.2014(3) 0.1618(3) 0.0710(17) Uani 1 1 d . A 1 H50A H 0.3638 0.2261 0.1273 0.106 Uiso 1 1 calc R A 1 H50B H 0.3986 0.1491 0.1569 0.106 Uiso 1 1 calc R A 1 H50C H 0.4647 0.214 0.1578 0.106 Uiso 1 1 calc R A 1 C51 C 0.4838(4) 0.1878(4) 0.3083(3) 0.084(2) Uani 1 1 d . A 1 H51A H 0.4763 0.1353 0.3077 0.127 Uiso 1 1 calc R A 1 H51B H 0.4829 0.2065 0.3518 0.127 Uiso 1 1 calc R A 1 H51C H 0.5392 0.1995 0.2988 0.127 Uiso 1 1 calc R A 1 C52 C 0.2888(3) 0.2103(3) 0.2595(3) 0.0639(15) Uani 1 1 d . A 1 H52A H 0.2922 0.1855 0.3019 0.077 Uiso 1 1 calc R A 1 H52B H 0.2494 0.1844 0.2228 0.077 Uiso 1 1 calc R A 1 C53 C 0.4694(7) 0.8415(6) 0.4762(5) 0.145(4) Uiso 1 1 d . B 2 C54 C 0.4977(9) 0.9084(8) 0.5188(7) 0.185(5) Uiso 1 1 d . B 2 C55 C 0.4939(9) 0.9678(9) 0.4719(7) 0.200(6) Uiso 1 1 d . . 2 C58 C -0.0520(14) 0.5662(16) 0.4129(12) 0.306(11) Uiso 1 1 d . C 2 C56 C 0.0358(13) 0.5277(14) 0.5191(14) 0.276(10) Uiso 1 1 d . . 2 C57 C 0.0179(14) 0.6019(15) 0.4905(11) 0.288(9) Uiso 1 1 d . C 2 C59 C -0.0385(16) 0.4909(18) 0.4211(15) 0.337(13) Uiso 1 1 d . . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm 0.03187(14) 0.04731(17) 0.04062(15) -0.00110(12) 0.00504(10) 0.00031(11) Si1 0.0411(7) 0.0572(10) 0.0513(8) 0.0083(7) 0.0029(6) -0.0151(7) Si2 0.0305(6) 0.0458(8) 0.0367(7) 0.0081(6) 0.0019(5) 0.0013(6) Si3 0.0408(7) 0.0557(10) 0.0388(7) -0.0097(6) 0.0044(6) -0.0025(6) Si4 0.0479(8) 0.0410(9) 0.0747(10) 0.0000(7) 0.0108(7) 0.0089(7) N1 0.0325(19) 0.045(3) 0.042(2) 0.0059(18) 0.0040(16) -0.0049(18) N2 0.0284(18) 0.039(2) 0.0339(19) 0.0058(17) 0.0006(15) 0.0005(16) N3 0.038(2) 0.040(2) 0.043(2) -0.0040(18) 0.0067(17) -0.0055(18) N4 0.041(2) 0.042(3) 0.054(2) 0.0026(19) 0.0069(19) 0.0044(19) C1 0.028(2) 0.051(3) 0.036(2) -0.001(2) 0.0075(19) 0.000(2) C2 0.028(2) 0.044(3) 0.032(2) 0.005(2) 0.0028(19) -0.004(2) C3 0.028(2) 0.049(3) 0.030(2) 0.003(2) 0.0076(19) 0.000(2) C4 0.079(4) 0.069(4) 0.078(4) 0.027(3) 0.004(3) -0.031(3) C5 0.056(3) 0.065(4) 0.074(4) -0.004(3) 0.004(3) -0.020(3) C6 0.055(3) 0.089(5) 0.081(4) 0.005(4) 0.025(3) -0.024(3) C7 0.029(2) 0.053(3) 0.044(3) 0.014(2) 0.003(2) -0.001(2) C8 0.035(3) 0.059(4) 0.068(4) 0.011(3) 0.001(2) -0.001(3) C9 0.035(3) 0.075(5) 0.099(5) 0.030(4) 0.011(3) 0.012(3) C10 0.032(3) 0.105(6) 0.069(4) 0.036(4) -0.006(3) -0.009(3) C11 0.047(3) 0.109(6) 0.048(3) 0.011(3) -0.006(3) -0.018(4) C12 0.043(3) 0.070(4) 0.047(3) 0.004(3) -0.002(2) -0.006(3) C13 0.040(3) 0.196(9) 0.094(5) 0.066(6) -0.008(3) 0.006(4) C14 0.031(2) 0.042(3) 0.034(2) 0.004(2) 0.0013(19) 0.003(2) C15 0.046(3) 0.042(3) 0.044(3) 0.005(2) -0.004(2) 0.004(2) C16 0.064(3) 0.042(3) 0.053(3) 0.006(2) -0.010(3) 0.008(3) C17 0.059(3) 0.050(4) 0.066(4) -0.011(3) -0.008(3) 0.017(3) C18 0.049(3) 0.054(3) 0.044(3) -0.007(2) 0.003(2) 0.014(3) C19 0.034(2) 0.053(3) 0.045(3) -0.001(2) 0.006(2) 0.007(2) C20 0.034(2) 0.043(3) 0.042(3) 0.004(2) 0.011(2) 0.002(2) C21 0.041(3) 0.050(3) 0.051(3) 0.004(2) 0.000(2) -0.005(2) C22 0.051(3) 0.045(3) 0.045(3) -0.005(2) -0.004(2) 0.000(2) C23 0.071(4) 0.042(3) 0.053(3) 0.004(2) -0.002(3) -0.009(3) C24 0.062(3) 0.045(3) 0.060(3) 0.011(3) 0.007(3) 0.009(3) C25 0.047(3) 0.071(4) 0.051(3) 0.012(3) 0.012(2) 0.000(3) C26 0.037(3) 0.060(4) 0.049(3) 0.011(2) -0.006(2) 0.000(2) C27 0.037(2) 0.044(3) 0.030(2) 0.000(2) 0.010(2) 0.006(2) C28 0.037(2) 0.042(3) 0.041(3) -0.003(2) 0.009(2) 0.000(2) C29 0.042(3) 0.048(3) 0.036(3) -0.003(2) 0.008(2) 0.003(2) C30 0.057(3) 0.083(5) 0.050(3) -0.010(3) 0.015(3) 0.002(3) C31 0.061(3) 0.063(4) 0.069(4) -0.016(3) 0.013(3) -0.015(3) C32 0.053(3) 0.085(5) 0.047(3) -0.017(3) -0.004(3) 0.006(3) C33 0.037(2) 0.049(3) 0.031(2) -0.002(2) 0.003(2) -0.006(2) C34 0.045(3) 0.044(3) 0.033(2) 0.005(2) 0.005(2) -0.001(2) C35 0.048(3) 0.053(3) 0.032(2) 0.002(2) 0.003(2) 0.006(2) C36 0.063(3) 0.047(3) 0.043(3) 0.009(2) 0.007(2) 0.001(3) C37 0.065(4) 0.059(4) 0.066(4) 0.017(3) 0.014(3) -0.015(3) C38 0.043(3) 0.054(4) 0.057(3) 0.009(3) 0.009(2) -0.006(3) C39 0.095(5) 0.056(4) 0.069(4) 0.020(3) 0.012(3) 0.002(3) C40 0.030(2) 0.048(3) 0.041(3) -0.005(2) 0.005(2) 0.002(2) C41 0.046(3) 0.071(5) 0.147(7) -0.004(4) -0.004(4) -0.011(3) C42 0.057(4) 0.070(5) 0.125(7) -0.014(4) 0.003(4) -0.004(3) C43 0.068(4) 0.151(8) 0.079(5) -0.015(5) 0.021(4) -0.051(5) C44 0.051(4) 0.095(6) 0.143(7) -0.057(5) 0.021(4) 0.009(4) C45 0.044(3) 0.099(6) 0.132(6) -0.060(5) 0.027(4) -0.006(3) C46 0.040(3) 0.226(10) 0.054(4) 0.009(5) 0.005(3) -0.007(4) C47 0.063(5) 0.255(13) 0.047(4) 0.032(6) -0.009(3) -0.022(7) C48 0.036(4) 0.118(8) 0.223(11) 0.069(7) 0.018(5) 0.011(4) C49 0.059(4) 0.184(10) 0.102(6) -0.073(7) 0.016(4) -0.008(5) C50 0.067(4) 0.056(4) 0.091(4) -0.021(3) 0.021(3) 0.002(3) C51 0.075(4) 0.063(4) 0.109(5) 0.017(4) 0.011(4) 0.021(3) C52 0.057(3) 0.059(4) 0.073(4) 0.015(3) 0.012(3) -0.003(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sm N3 2.350(4) . ? Sm N4 2.363(4) . ? Sm N2 2.417(4) . ? Sm N1 2.420(4) . ? Sm C52 2.627(6) . ? Sm C27 2.825(4) . ? Sm C1 2.845(4) . ? Sm C2 2.869(4) . ? Sm C3 2.896(5) . ? Sm C28 2.904(5) . ? Sm C29 2.917(5) . ? Sm Si4 3.2220(15) . ? Si1 N1 1.749(4) . ? Si1 C4 1.853(6) . ? Si1 C5 1.861(6) . ? Si1 C6 1.868(6) . ? Si2 N2 1.721(3) . ? Si2 C25 1.856(5) . ? Si2 C24 1.862(5) . ? Si2 C26 1.869(5) . ? Si3 N3 1.726(4) . ? Si3 C30 1.860(5) . ? Si3 C31 1.863(6) . ? Si3 C32 1.871(5) . ? Si4 N4 1.743(4) . ? Si4 C52 1.831(6) . ? Si4 C50 1.867(6) . ? Si4 C51 1.876(6) . ? N1 C1 1.322(6) . ? N2 C3 1.330(6) . ? N3 C27 1.355(6) . ? N4 C29 1.313(6) . ? C1 C2 1.424(6) . ? C1 C7 1.511(6) . ? C2 C3 1.418(6) . ? C2 H2 0.95 . ? C3 C14 1.543(6) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 C8 1.384(7) . ? C7 C12 1.396(7) . ? C8 C9 1.400(7) . ? C8 H8 0.95 . ? C9 C10 1.384(9) . ? C9 H9 0.95 . ? C10 C11 1.367(9) . ? C10 C13 1.519(7) . ? C11 C12 1.385(7) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C13 H13D 0.98 . ? C13 H13E 0.98 . ? C13 H13F 0.98 . ? C14 C19 1.538(6) . ? C14 C20 1.542(6) . ? C14 C15 1.553(6) . ? C15 C16 1.552(7) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 C17 1.523(8) . ? C16 C23 1.527(7) . ? C16 H16 1 . ? C17 C18 1.533(7) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 C19 1.527(7) . ? C18 C22 1.530(7) . ? C18 H18 1 . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.531(7) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C23 1.525(7) . ? C21 C22 1.535(7) . ? C21 H21 1 . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C28 1.411(6) . ? C27 C33 1.496(6) . ? C28 C29 1.438(6) . ? C28 H28 0.95 . ? C29 C40 1.555(6) . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 C34 1.394(6) . ? C33 C38 1.396(7) . ? C34 C35 1.374(7) . ? C34 H34 0.95 . ? C35 C36 1.386(7) . ? C35 H35 0.95 . ? C36 C37 1.377(7) . ? C36 C39 1.515(7) . ? C37 C38 1.386(7) . ? C37 H37 0.95 . ? C38 H38 0.95 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C39 H39D 0.98 . ? C39 H39E 0.98 . ? C39 H39F 0.98 . ? C40 C46 1.506(7) . ? C40 C45 1.510(7) . ? C40 C41 1.542(8) . ? C41 C42 1.569(8) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 C49 1.443(11) . ? C42 C43 1.479(10) . ? C42 H42 1 . ? C43 C44 1.472(11) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C44 C48 1.479(12) . ? C44 C45 1.556(8) . ? C44 H44 1 . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? C46 C47 1.579(9) . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? C47 C49 1.502(13) . ? C47 C48 1.511(13) . ? C47 H47 1 . ? C48 H48A 0.99 . ? C48 H48B 0.99 . ? C49 H49A 0.99 . ? C49 H49B 0.99 . ? C50 H50A 0.98 . ? C50 H50B 0.98 . ? C50 H50C 0.98 . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C52 H52A 0.99 . ? C52 H52B 0.99 . ? C53 C54 1.529(16) . ? C54 C55 1.468(18) . ? C55 C55 1.65(3) 3_676 ? C58 C59 1.42(3) . ? C56 C59 1.29(3) 3_566 ? C56 C57 1.50(3) . ? C56 C56 1.60(4) 3_566 ? C59 C56 1.29(3) 3_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Sm N4 78.96(13) . . ? N3 Sm N2 128.05(13) . . ? N4 Sm N2 112.10(12) . . ? N3 Sm N1 103.89(12) . . ? N4 Sm N1 165.47(14) . . ? N2 Sm N1 77.67(12) . . ? N3 Sm C52 105.29(16) . . ? N4 Sm C52 66.54(16) . . ? N2 Sm C52 126.03(15) . . ? N1 Sm C52 99.11(15) . . ? N3 Sm C27 28.50(12) . . ? N4 Sm C27 71.70(13) . . ? N2 Sm C27 104.13(12) . . ? N1 Sm C27 117.48(12) . . ? C52 Sm C27 123.31(15) . . ? N3 Sm C1 87.73(13) . . ? N4 Sm C1 164.50(14) . . ? N2 Sm C1 70.19(12) . . ? N1 Sm C1 27.61(13) . . ? C52 Sm C1 125.49(15) . . ? C27 Sm C1 92.82(13) . . ? N3 Sm C2 85.21(13) . . ? N4 Sm C2 140.11(13) . . ? N2 Sm C2 53.03(11) . . ? N1 Sm C2 54.29(13) . . ? C52 Sm C2 153.34(14) . . ? C27 Sm C2 76.96(12) . . ? C1 Sm C2 28.86(12) . . ? N3 Sm C3 102.82(13) . . ? N4 Sm C3 122.08(13) . . ? N2 Sm C3 27.13(11) . . ? N1 Sm C3 71.58(12) . . ? C52 Sm C3 151.79(15) . . ? C27 Sm C3 83.61(12) . . ? C1 Sm C3 53.11(12) . . ? C2 Sm C3 28.47(11) . . ? N3 Sm C28 54.12(12) . . ? N4 Sm C28 53.11(13) . . ? N2 Sm C28 90.98(12) . . ? N1 Sm C28 139.84(13) . . ? C52 Sm C28 118.09(15) . . ? C27 Sm C28 28.48(12) . . ? C1 Sm C28 112.33(13) . . ? C2 Sm C28 88.05(13) . . ? C3 Sm C28 80.86(12) . . ? N3 Sm C29 71.02(12) . . ? N4 Sm C29 26.21(14) . . ? N2 Sm C29 96.75(12) . . ? N1 Sm C29 168.02(14) . . ? C52 Sm C29 92.75(15) . . ? C27 Sm C29 53.17(12) . . ? C1 Sm C29 140.48(14) . . ? C2 Sm C29 113.89(13) . . ? C3 Sm C29 98.58(13) . . ? C28 Sm C29 28.62(13) . . ? N3 Sm Si4 91.90(10) . . ? N4 Sm Si4 31.91(11) . . ? N2 Sm Si4 124.90(8) . . ? N1 Sm Si4 133.70(10) . . ? C52 Sm Si4 34.63(12) . . ? C27 Sm Si4 96.99(9) . . ? C1 Sm Si4 158.67(10) . . ? C2 Sm Si4 172.01(9) . . ? C3 Sm Si4 146.81(8) . . ? C28 Sm Si4 84.22(9) . . ? C29 Sm Si4 58.12(10) . . ? N1 Si1 C4 106.0(2) . . ? N1 Si1 C5 111.8(2) . . ? C4 Si1 C5 106.4(3) . . ? N1 Si1 C6 113.4(3) . . ? C4 Si1 C6 108.4(3) . . ? C5 Si1 C6 110.5(3) . . ? N2 Si2 C25 108.5(2) . . ? N2 Si2 C24 104.9(2) . . ? C25 Si2 C24 110.4(3) . . ? N2 Si2 C26 119.9(2) . . ? C25 Si2 C26 107.8(2) . . ? C24 Si2 C26 105.0(2) . . ? N3 Si3 C30 106.7(2) . . ? N3 Si3 C31 106.2(2) . . ? C30 Si3 C31 110.6(3) . . ? N3 Si3 C32 119.0(2) . . ? C30 Si3 C32 107.3(3) . . ? C31 Si3 C32 107.0(3) . . ? N4 Si4 C52 100.4(2) . . ? N4 Si4 C50 106.4(3) . . ? C52 Si4 C50 114.9(3) . . ? N4 Si4 C51 115.7(3) . . ? C52 Si4 C51 111.7(3) . . ? C50 Si4 C51 107.8(3) . . ? N4 Si4 Sm 45.76(13) . . ? C52 Si4 Sm 54.62(19) . . ? C50 Si4 Sm 122.7(2) . . ? C51 Si4 Sm 129.0(2) . . ? C1 N1 Si1 129.8(3) . . ? C1 N1 Sm 94.4(3) . . ? Si1 N1 Sm 134.4(2) . . ? C3 N2 Si2 141.6(3) . . ? C3 N2 Sm 96.9(3) . . ? Si2 N2 Sm 121.28(19) . . ? C27 N3 Si3 126.1(3) . . ? C27 N3 Sm 95.6(3) . . ? Si3 N3 Sm 137.8(2) . . ? C29 N4 Si4 156.5(4) . . ? C29 N4 Sm 101.2(3) . . ? Si4 N4 Sm 102.33(19) . . ? N1 C1 C2 125.9(4) . . ? N1 C1 C7 120.7(4) . . ? C2 C1 C7 113.2(4) . . ? N1 C1 Sm 58.0(2) . . ? C2 C1 Sm 76.5(2) . . ? C7 C1 Sm 143.5(3) . . ? C3 C2 C1 129.2(4) . . ? C3 C2 Sm 76.8(3) . . ? C1 C2 Sm 74.6(3) . . ? C3 C2 H2 115.4 . . ? C1 C2 H2 115.4 . . ? Sm C2 H2 125.1 . . ? N2 C3 C2 121.2(4) . . ? N2 C3 C14 120.7(4) . . ? C2 C3 C14 118.1(4) . . ? N2 C3 Sm 56.0(2) . . ? C2 C3 Sm 74.7(3) . . ? C14 C3 Sm 146.5(3) . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 118.5(4) . . ? C8 C7 C1 121.8(4) . . ? C12 C7 C1 119.7(5) . . ? C7 C8 C9 120.4(6) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 120.6(6) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 118.7(5) . . ? C11 C10 C13 121.5(7) . . ? C9 C10 C13 119.8(7) . . ? C10 C11 C12 121.7(6) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C7 120.2(6) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C13 H13D 109.5 . . ? H13A C13 H13D 141.1 . . ? H13B C13 H13D 56.3 . . ? H13C C13 H13D 56.3 . . ? C10 C13 H13E 109.5 . . ? H13A C13 H13E 56.3 . . ? H13B C13 H13E 141.1 . . ? H13C C13 H13E 56.3 . . ? H13D C13 H13E 109.5 . . ? C10 C13 H13F 109.5 . . ? H13A C13 H13F 56.3 . . ? H13B C13 H13F 56.3 . . ? H13C C13 H13F 141.1 . . ? H13D C13 H13F 109.5 . . ? H13E C13 H13F 109.5 . . ? C19 C14 C20 109.2(3) . . ? C19 C14 C3 108.6(4) . . ? C20 C14 C3 110.5(4) . . ? C19 C14 C15 107.0(4) . . ? C20 C14 C15 107.7(4) . . ? C3 C14 C15 113.8(3) . . ? C16 C15 C14 110.4(4) . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C23 109.9(4) . . ? C17 C16 C15 108.9(5) . . ? C23 C16 C15 109.9(4) . . ? C17 C16 H16 109.4 . . ? C23 C16 H16 109.4 . . ? C15 C16 H16 109.4 . . ? C16 C17 C18 109.6(4) . . ? C16 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? C16 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? C19 C18 C22 109.7(4) . . ? C19 C18 C17 109.5(4) . . ? C22 C18 C17 108.7(4) . . ? C19 C18 H18 109.6 . . ? C22 C18 H18 109.6 . . ? C17 C18 H18 109.6 . . ? C18 C19 C14 111.4(4) . . ? C18 C19 H19A 109.4 . . ? C14 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? C14 C19 H19B 109.4 . . ? H19A C19 H19B 108 . . ? C21 C20 C14 111.0(4) . . ? C21 C20 H20A 109.4 . . ? C14 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? C14 C20 H20B 109.4 . . ? H20A C20 H20B 108 . . ? C23 C21 C20 109.6(4) . . ? C23 C21 C22 109.5(4) . . ? C20 C21 C22 109.7(4) . . ? C23 C21 H21 109.4 . . ? C20 C21 H21 109.4 . . ? C22 C21 H21 109.4 . . ? C18 C22 C21 109.6(4) . . ? C18 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? C18 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C21 C23 C16 109.1(4) . . ? C21 C23 H23A 109.9 . . ? C16 C23 H23A 109.9 . . ? C21 C23 H23B 109.9 . . ? C16 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 C28 123.8(4) . . ? N3 C27 C33 119.6(4) . . ? C28 C27 C33 116.5(4) . . ? N3 C27 Sm 55.9(2) . . ? C28 C27 Sm 78.8(3) . . ? C33 C27 Sm 140.5(3) . . ? C27 C28 C29 128.9(4) . . ? C27 C28 Sm 72.7(3) . . ? C29 C28 Sm 76.2(3) . . ? C27 C28 H28 115.6 . . ? C29 C28 H28 115.6 . . ? Sm C28 H28 128.4 . . ? N4 C29 C28 121.7(4) . . ? N4 C29 C40 121.0(4) . . ? C28 C29 C40 117.3(4) . . ? N4 C29 Sm 52.6(2) . . ? C28 C29 Sm 75.2(3) . . ? C40 C29 Sm 151.3(3) . . ? Si3 C30 H30A 109.5 . . ? Si3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C38 116.6(5) . . ? C34 C33 C27 120.1(4) . . ? C38 C33 C27 123.3(4) . . ? C35 C34 C33 122.0(5) . . ? C35 C34 H34 119 . . ? C33 C34 H34 119 . . ? C34 C35 C36 121.2(5) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C37 C36 C35 117.5(5) . . ? C37 C36 C39 121.7(5) . . ? C35 C36 C39 120.8(5) . . ? C36 C37 C38 121.8(5) . . ? C36 C37 H37 119.1 . . ? C38 C37 H37 119.1 . . ? C37 C38 C33 120.9(5) . . ? C37 C38 H38 119.5 . . ? C33 C38 H38 119.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C39 H39D 109.5 . . ? H39A C39 H39D 141.1 . . ? H39B C39 H39D 56.3 . . ? H39C C39 H39D 56.3 . . ? C36 C39 H39E 109.5 . . ? H39A C39 H39E 56.3 . . ? H39B C39 H39E 141.1 . . ? H39C C39 H39E 56.3 . . ? H39D C39 H39E 109.5 . . ? C36 C39 H39F 109.5 . . ? H39A C39 H39F 56.3 . . ? H39B C39 H39F 56.3 . . ? H39C C39 H39F 141.1 . . ? H39D C39 H39F 109.5 . . ? H39E C39 H39F 109.5 . . ? C46 C40 C45 110.4(5) . . ? C46 C40 C41 105.9(5) . . ? C45 C40 C41 107.9(5) . . ? C46 C40 C29 108.9(4) . . ? C45 C40 C29 109.1(4) . . ? C41 C40 C29 114.5(4) . . ? C40 C41 C42 110.6(5) . . ? C40 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C49 C42 C43 110.7(6) . . ? C49 C42 C41 108.3(7) . . ? C43 C42 C41 107.4(6) . . ? C49 C42 H42 110.1 . . ? C43 C42 H42 110.1 . . ? C41 C42 H42 110.1 . . ? C44 C43 C42 112.1(6) . . ? C44 C43 H43A 109.2 . . ? C42 C43 H43A 109.2 . . ? C44 C43 H43B 109.2 . . ? C42 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? C43 C44 C48 111.4(6) . . ? C43 C44 C45 109.1(7) . . ? C48 C44 C45 106.4(7) . . ? C43 C44 H44 109.9 . . ? C48 C44 H44 109.9 . . ? C45 C44 H44 109.9 . . ? C40 C45 C44 111.1(5) . . ? C40 C45 H45A 109.4 . . ? C44 C45 H45A 109.4 . . ? C40 C45 H45B 109.4 . . ? C44 C45 H45B 109.4 . . ? H45A C45 H45B 108 . . ? C40 C46 C47 110.3(5) . . ? C40 C46 H46A 109.6 . . ? C47 C46 H46A 109.6 . . ? C40 C46 H46B 109.6 . . ? C47 C46 H46B 109.6 . . ? H46A C46 H46B 108.1 . . ? C49 C47 C48 110.0(7) . . ? C49 C47 C46 106.4(8) . . ? C48 C47 C46 108.4(8) . . ? C49 C47 H47 110.6 . . ? C48 C47 H47 110.6 . . ? C46 C47 H47 110.6 . . ? C44 C48 C47 110.9(6) . . ? C44 C48 H48A 109.5 . . ? C47 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 108 . . ? C42 C49 C47 112.5(6) . . ? C42 C49 H49A 109.1 . . ? C47 C49 H49A 109.1 . . ? C42 C49 H49B 109.1 . . ? C47 C49 H49B 109.1 . . ? H49A C49 H49B 107.8 . . ? Si4 C50 H50A 109.5 . . ? Si4 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si4 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Si4 C51 H51A 109.5 . . ? Si4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si4 C52 Sm 90.7(2) . . ? Si4 C52 H52A 113.5 . . ? Sm C52 H52A 113.5 . . ? Si4 C52 H52B 113.5 . . ? Sm C52 H52B 113.5 . . ? H52A C52 H52B 110.8 . . ? C55 C54 C53 105.1(11) . . ? C54 C55 C55 95.0(14) . 3_676 ? C59 C58 C57 102(2) . . ? C59 C56 C57 126(3) 3_566 . ? C59 C56 C56 99(3) 3_566 3_566 ? C57 C56 C56 110(3) . 3_566 ? C56 C57 C58 92(2) . . ? C56 C59 C58 110(3) 3_566 . ? #===END