Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof John Arnold' _publ_contact_author_address ; Department of Chemistry University of California Berkeley CA 94720 UNITED STATES OF AMERICA ; _publ_contact_author_email ARNOLD@BERKELEY.EDU _publ_section_title ; Synthesis and Characterization of Mono Diketiminatosamarium Amides and Hydrocarbyls ; loop_ _publ_author_name 'John Arnold' 'Chunming Cui.' 'Joseph A. R. Schmidt' 'Alexandr Shafir' data_NacSmCl2(THF)SmCl2Nac _database_code_depnum_ccdc_archive 'CCDC 244217' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C62 H88 Cl4 N4 O Sm2), 4.5(C7 H8)' _chemical_formula_sum 'C153.75 H204 Cl8 N8 O2 Sm4' _chemical_formula_weight 3081.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 23.7660(11) _cell_length_b 26.1434(12) _cell_length_c 26.7645(12) _cell_angle_alpha 90.00 _cell_angle_beta 110.8440(10) _cell_angle_gamma 90.00 _cell_volume 15541.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 6291 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 24.47 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6330 _exptl_absorpt_coefficient_mu 1.677 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6891 _exptl_absorpt_correction_T_max 0.7871 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 138(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method /w\2/q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 68628 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_sigmaI/netI 0.1253 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 24.69 _reflns_number_total 25619 _reflns_number_gt 13270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.052d' _computing_cell_refinement 'Bruker SAINT v5.10' _computing_data_reduction 'Bruker SAINT v5.10' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Associated with the samarium molecules are four and half toluenes of crystallization. Three of the toluenes are well behaved and show no signs of disorder. The remainin one and half molecules of toluene are disordered over three different sites. Further, two of these toluenes are disordeed over inversion centers. Hydrogen atoms were not predicted for these disordered molecules. ; _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^)+(0.0829P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25619 _refine_ls_number_parameters 1436 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1308 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1748 _refine_ls_wR_factor_gt 0.1556 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.36000(2) 0.292058(19) 0.83046(2) 0.02792(15) Uani 1 1 d . . . Sm2 Sm 0.32321(2) 0.289619(18) 0.962059(19) 0.02460(14) Uani 1 1 d . . . Sm11 Sm 0.76707(2) 0.301804(19) 0.58518(2) 0.02629(14) Uani 1 1 d . . . Sm12 Sm 0.80226(2) 0.30350(2) 0.45237(2) 0.02782(15) Uani 1 1 d . . . Cl1 Cl 0.38144(14) 0.22314(10) 0.91372(11) 0.0486(8) Uani 1 1 d . . . Cl2 Cl 0.25606(12) 0.29713(11) 0.85109(10) 0.0462(7) Uani 1 1 d . . . Cl3 Cl 0.38972(14) 0.35381(10) 0.91919(11) 0.0457(8) Uani 1 1 d . . . Cl4 Cl 0.38119(13) 0.24015(10) 1.04981(10) 0.0433(7) Uani 1 1 d . . . Cl11 Cl 0.73879(14) 0.36677(10) 0.49900(11) 0.0475(8) Uani 1 1 d . . . Cl12 Cl 0.74263(13) 0.23599(10) 0.49906(11) 0.0417(7) Uani 1 1 d . . . Cl13 Cl 0.86999(12) 0.30658(11) 0.56305(10) 0.0460(7) Uani 1 1 d . . . Cl14 Cl 0.74802(13) 0.25186(11) 0.36476(10) 0.0464(7) Uani 1 1 d . . . O1 O 0.4683(3) 0.2918(2) 0.8507(2) 0.0369(18) Uani 1 1 d . . . O101 O 0.6600(3) 0.3008(2) 0.5634(2) 0.0351(17) Uani 1 1 d . . . N1 N 0.3448(4) 0.3461(3) 0.7547(3) 0.031(2) Uani 1 1 d . . . N2 N 0.3485(3) 0.2333(3) 0.7607(3) 0.032(2) Uani 1 1 d . . . N3 N 0.3147(3) 0.3625(3) 1.0111(3) 0.0260(19) Uani 1 1 d . . . N4 N 0.2271(4) 0.2756(3) 0.9678(3) 0.037(2) Uani 1 1 d . . . N101 N 0.7799(4) 0.3542(3) 0.6618(3) 0.030(2) Uani 1 1 d . . . N102 N 0.7775(3) 0.2421(3) 0.6551(3) 0.0281(19) Uani 1 1 d . . . N103 N 0.8062(3) 0.3772(3) 0.4020(3) 0.035(2) Uani 1 1 d . . . N104 N 0.8988(3) 0.2950(3) 0.4439(3) 0.032(2) Uani 1 1 d . . . C1 C 0.3525(5) 0.3775(4) 0.6692(4) 0.050(3) Uani 1 1 d . . . H1A H 0.3442 0.4103 0.6829 0.074 Uiso 1 1 calc R . . H1B H 0.3206 0.3700 0.6348 0.074 Uiso 1 1 calc R . . H1C H 0.3913 0.3793 0.6641 0.074 Uiso 1 1 calc R . . C2 C 0.3546(4) 0.3356(4) 0.7086(4) 0.029(2) Uani 1 1 d . . . C3 C 0.3658(5) 0.2876(4) 0.6944(4) 0.035(3) Uani 1 1 d . . . H3A H 0.3808 0.2867 0.6659 0.042 Uiso 1 1 calc R . . C4 C 0.3591(4) 0.2398(4) 0.7142(4) 0.031(2) Uani 1 1 d . . . C5 C 0.3626(5) 0.1931(4) 0.6806(4) 0.045(3) Uani 1 1 d . . . H5A H 0.3572 0.1618 0.6986 0.067 Uiso 1 1 calc R . . H5B H 0.4019 0.1924 0.6765 0.067 Uiso 1 1 calc R . . H5C H 0.3307 0.1954 0.6453 0.067 Uiso 1 1 calc R . . C6 C 0.3309(5) 0.1828(4) 0.7731(4) 0.031(2) Uani 1 1 d . . . C7 C 0.2701(5) 0.1751(4) 0.7624(4) 0.038(3) Uani 1 1 d . . . C8 C 0.2524(5) 0.1276(4) 0.7771(5) 0.058(3) Uani 1 1 d . . . H8A H 0.2110 0.1210 0.7702 0.069 Uiso 1 1 calc R . . C9 C 0.2951(6) 0.0904(4) 0.8018(5) 0.065(4) Uani 1 1 d . . . H9A H 0.2831 0.0585 0.8118 0.078 Uiso 1 1 calc R . . C10 C 0.3545(5) 0.1003(4) 0.8115(5) 0.051(3) Uani 1 1 d . . . H10A H 0.3836 0.0749 0.8288 0.061 Uiso 1 1 calc R . . C11 C 0.3738(5) 0.1453(4) 0.7972(4) 0.036(3) Uani 1 1 d . . . C12 C 0.2219(4) 0.2142(4) 0.7346(4) 0.038(3) Uani 1 1 d . . . H12A H 0.2397 0.2486 0.7471 0.046 Uiso 1 1 calc R . . C13 C 0.1645(5) 0.2104(4) 0.7476(5) 0.057(3) Uani 1 1 d . . . H13A H 0.1749 0.2110 0.7865 0.086 Uiso 1 1 calc R . . H13B H 0.1436 0.1784 0.7332 0.086 Uiso 1 1 calc R . . H13C H 0.1381 0.2394 0.7316 0.086 Uiso 1 1 calc R . . C14 C 0.2055(5) 0.2132(4) 0.6733(4) 0.048(3) Uani 1 1 d . . . H14A H 0.2423 0.2157 0.6649 0.073 Uiso 1 1 calc R . . H14B H 0.1791 0.2422 0.6572 0.073 Uiso 1 1 calc R . . H14C H 0.1846 0.1812 0.6589 0.073 Uiso 1 1 calc R . . C15 C 0.4417(5) 0.1519(4) 0.8076(4) 0.044(3) Uani 1 1 d . . . H15A H 0.4477 0.1859 0.7932 0.053 Uiso 1 1 calc R . . C16 C 0.4789(5) 0.1507(5) 0.8668(4) 0.074(4) Uani 1 1 d . . . H16A H 0.5216 0.1549 0.8719 0.111 Uiso 1 1 calc R . . H16B H 0.4731 0.1179 0.8820 0.111 Uiso 1 1 calc R . . H16C H 0.4662 0.1786 0.8849 0.111 Uiso 1 1 calc R . . C17 C 0.4653(5) 0.1102(4) 0.7793(4) 0.064(4) Uani 1 1 d . . . H17A H 0.5083 0.1157 0.7867 0.096 Uiso 1 1 calc R . . H17B H 0.4433 0.1120 0.7407 0.096 Uiso 1 1 calc R . . H17C H 0.4594 0.0765 0.7926 0.096 Uiso 1 1 calc R . . C18 C 0.3221(5) 0.3958(4) 0.7613(4) 0.031(2) Uani 1 1 d . . . C19 C 0.3598(5) 0.4328(4) 0.7935(4) 0.037(3) Uani 1 1 d . . . C20 C 0.3361(6) 0.4799(4) 0.7989(5) 0.051(3) Uani 1 1 d . . . H20A H 0.3618 0.5054 0.8206 0.061 Uiso 1 1 calc R . . C21 C 0.2757(6) 0.4904(4) 0.7731(5) 0.050(3) Uani 1 1 d . . . H21A H 0.2599 0.5229 0.7769 0.060 Uiso 1 1 calc R . . C22 C 0.2388(5) 0.4531(4) 0.7420(4) 0.047(3) Uani 1 1 d . . . H22A H 0.1971 0.4602 0.7246 0.057 Uiso 1 1 calc R . . C23 C 0.2608(5) 0.4056(4) 0.7354(4) 0.035(3) Uani 1 1 d . . . C24 C 0.4281(5) 0.4236(4) 0.8207(4) 0.047(3) Uani 1 1 d . . . H24A H 0.4353 0.3862 0.8281 0.056 Uiso 1 1 calc R . . C25 C 0.4563(6) 0.4527(4) 0.8725(4) 0.060(4) Uani 1 1 d . . . H25A H 0.4370 0.4426 0.8978 0.090 Uiso 1 1 calc R . . H25B H 0.4508 0.4895 0.8654 0.090 Uiso 1 1 calc R . . H25C H 0.4994 0.4449 0.8877 0.090 Uiso 1 1 calc R . . C26 C 0.4602(5) 0.4405(5) 0.7826(4) 0.076(4) Uani 1 1 d . . . H26A H 0.5036 0.4347 0.7996 0.113 Uiso 1 1 calc R . . H26B H 0.4527 0.4770 0.7744 0.113 Uiso 1 1 calc R . . H26C H 0.4448 0.4206 0.7494 0.113 Uiso 1 1 calc R . . C27 C 0.2180(5) 0.3671(4) 0.6984(4) 0.048(3) Uani 1 1 d . . . H27A H 0.2405 0.3347 0.6987 0.057 Uiso 1 1 calc R . . C28 C 0.1912(6) 0.3872(6) 0.6403(4) 0.085(5) Uani 1 1 d . . . H28A H 0.2240 0.3953 0.6274 0.127 Uiso 1 1 calc R . . H28B H 0.1675 0.4181 0.6393 0.127 Uiso 1 1 calc R . . H28C H 0.1653 0.3609 0.6174 0.127 Uiso 1 1 calc R . . C29 C 0.1649(5) 0.3553(4) 0.7164(4) 0.048(3) Uani 1 1 d . . . H29A H 0.1801 0.3427 0.7533 0.072 Uiso 1 1 calc R . . H29B H 0.1392 0.3292 0.6930 0.072 Uiso 1 1 calc R . . H29C H 0.1413 0.3865 0.7144 0.072 Uiso 1 1 calc R . . C30 C 0.3001(5) 0.4037(3) 1.0894(4) 0.039(3) Uani 1 1 d . . . H30A H 0.3284 0.4284 1.0840 0.058 Uiso 1 1 calc R . . H30B H 0.3176 0.3887 1.1252 0.058 Uiso 1 1 calc R . . H30C H 0.2624 0.4210 1.0859 0.058 Uiso 1 1 calc R . . C31 C 0.2877(4) 0.3615(3) 1.0477(4) 0.026(2) Uani 1 1 d . . . C32 C 0.2473(4) 0.3229(4) 1.0503(4) 0.036(3) Uani 1 1 d . . . H32A H 0.2396 0.3218 1.0827 0.043 Uiso 1 1 calc R . . C33 C 0.2170(4) 0.2863(4) 1.0126(4) 0.036(3) Uani 1 1 d . . . C34 C 0.1659(5) 0.2595(4) 1.0258(4) 0.055(3) Uani 1 1 d . . . H34A H 0.1460 0.2344 0.9979 0.082 Uiso 1 1 calc R . . H34B H 0.1364 0.2851 1.0274 0.082 Uiso 1 1 calc R . . H34C H 0.1828 0.2422 1.0604 0.082 Uiso 1 1 calc R . . C35 C 0.1811(5) 0.2473(4) 0.9264(4) 0.041(3) Uani 1 1 d . . . C36 C 0.1890(6) 0.1955(5) 0.9204(5) 0.052(3) Uani 1 1 d . . . C37 C 0.1428(6) 0.1693(5) 0.8792(5) 0.059(4) Uani 1 1 d . . . H37A H 0.1460 0.1336 0.8743 0.071 Uiso 1 1 calc R . . C38 C 0.0937(7) 0.1956(6) 0.8468(6) 0.079(5) Uani 1 1 d . . . H38A H 0.0640 0.1777 0.8189 0.095 Uiso 1 1 calc R . . C39 C 0.0855(6) 0.2478(6) 0.8530(5) 0.069(4) Uani 1 1 d . . . H39A H 0.0499 0.2646 0.8310 0.083 Uiso 1 1 calc R . . C40 C 0.1302(5) 0.2744(5) 0.8918(4) 0.052(3) Uani 1 1 d . . . C41 C 0.2438(7) 0.1663(5) 0.9547(5) 0.066(4) Uani 1 1 d . . . H41A H 0.2750 0.1923 0.9733 0.080 Uiso 1 1 calc R . . C42 C 0.2320(9) 0.1363(7) 0.9972(8) 0.188(12) Uani 1 1 d . . . H42A H 0.2137 0.1586 1.0166 0.283 Uiso 1 1 calc R . . H42B H 0.2700 0.1226 1.0220 0.283 Uiso 1 1 calc R . . H42C H 0.2045 0.1081 0.9808 0.283 Uiso 1 1 calc R . . C43 C 0.2726(8) 0.1303(6) 0.9237(7) 0.133(8) Uani 1 1 d . . . H43A H 0.3077 0.1129 0.9492 0.199 Uiso 1 1 calc R . . H43B H 0.2852 0.1506 0.8987 0.199 Uiso 1 1 calc R . . H43C H 0.2429 0.1047 0.9037 0.199 Uiso 1 1 calc R . . C44 C 0.1212(5) 0.3306(5) 0.8979(5) 0.068(4) Uani 1 1 d . . . H44A H 0.1581 0.3441 0.9264 0.081 Uiso 1 1 calc R . . C45 C 0.0670(6) 0.3405(6) 0.9155(5) 0.088(5) Uani 1 1 d . . . H45A H 0.0726 0.3217 0.9487 0.132 Uiso 1 1 calc R . . H45B H 0.0300 0.3288 0.8875 0.132 Uiso 1 1 calc R . . H45C H 0.0639 0.3772 0.9216 0.132 Uiso 1 1 calc R . . C46 C 0.1135(6) 0.3591(5) 0.8455(5) 0.084(5) Uani 1 1 d . . . H46A H 0.1484 0.3524 0.8351 0.126 Uiso 1 1 calc R . . H46B H 0.1104 0.3959 0.8509 0.126 Uiso 1 1 calc R . . H46C H 0.0768 0.3472 0.8173 0.126 Uiso 1 1 calc R . . C47 C 0.3479(5) 0.4087(3) 1.0084(4) 0.032(3) Uani 1 1 d . . . C48 C 0.4086(5) 0.4140(4) 1.0403(4) 0.035(3) Uani 1 1 d . . . C49 C 0.4369(5) 0.4574(4) 1.0319(4) 0.045(3) Uani 1 1 d . . . H49A H 0.4780 0.4624 1.0536 0.054 Uiso 1 1 calc R . . C50 C 0.4091(6) 0.4940(4) 0.9936(5) 0.054(4) Uani 1 1 d . . . H50A H 0.4308 0.5230 0.9890 0.065 Uiso 1 1 calc R . . C51 C 0.3501(6) 0.4874(4) 0.9627(5) 0.049(3) Uani 1 1 d . . . H51A H 0.3308 0.5123 0.9364 0.059 Uiso 1 1 calc R . . C52 C 0.3170(5) 0.4446(4) 0.9688(4) 0.036(3) Uani 1 1 d . . . C53 C 0.4425(4) 0.3745(4) 1.0805(4) 0.037(3) Uani 1 1 d . . . H53A H 0.4133 0.3481 1.0835 0.044 Uiso 1 1 calc R . . C54 C 0.4893(5) 0.3484(4) 1.0621(5) 0.057(3) Uani 1 1 d . . . H54A H 0.4693 0.3334 1.0266 0.085 Uiso 1 1 calc R . . H54B H 0.5096 0.3214 1.0875 0.085 Uiso 1 1 calc R . . H54C H 0.5190 0.3737 1.0604 0.085 Uiso 1 1 calc R . . C55 C 0.4757(5) 0.3978(4) 1.1367(4) 0.059(4) Uani 1 1 d . . . H55A H 0.4465 0.4150 1.1493 0.088 Uiso 1 1 calc R . . H55B H 0.5056 0.4227 1.1346 0.088 Uiso 1 1 calc R . . H55C H 0.4959 0.3706 1.1618 0.088 Uiso 1 1 calc R . . C56 C 0.2520(5) 0.4373(4) 0.9331(4) 0.050(3) Uani 1 1 d . . . H56A H 0.2434 0.3998 0.9318 0.060 Uiso 1 1 calc R . . C57 C 0.2387(6) 0.4551(5) 0.8751(5) 0.069(4) Uani 1 1 d . . . H57A H 0.1960 0.4495 0.8541 0.103 Uiso 1 1 calc R . . H57B H 0.2635 0.4355 0.8595 0.103 Uiso 1 1 calc R . . H57C H 0.2481 0.4916 0.8750 0.103 Uiso 1 1 calc R . . C58 C 0.2100(6) 0.4632(5) 0.9568(5) 0.074(4) Uani 1 1 d . . . H58A H 0.2192 0.4513 0.9936 0.111 Uiso 1 1 calc R . . H58B H 0.1682 0.4546 0.9353 0.111 Uiso 1 1 calc R . . H58C H 0.2155 0.5003 0.9567 0.111 Uiso 1 1 calc R . . C59 C 0.5125(5) 0.2958(5) 0.9064(4) 0.062(4) Uani 1 1 d . . . H59A H 0.5084 0.3288 0.9230 0.074 Uiso 1 1 calc R . . H59B H 0.5077 0.2674 0.9290 0.074 Uiso 1 1 calc R . . C60 C 0.5702(6) 0.2926(6) 0.8981(5) 0.093(5) Uani 1 1 d . . . H60A H 0.5838 0.2565 0.9006 0.111 Uiso 1 1 calc R . . H60B H 0.6013 0.3127 0.9257 0.111 Uiso 1 1 calc R . . C61 C 0.5614(5) 0.3131(5) 0.8443(4) 0.060(4) Uani 1 1 d . . . H61A H 0.5915 0.2992 0.8303 0.072 Uiso 1 1 calc R . . H61B H 0.5635 0.3509 0.8448 0.072 Uiso 1 1 calc R . . C62 C 0.4984(4) 0.2945(4) 0.8118(4) 0.041(3) Uani 1 1 d . . . H62A H 0.4777 0.3188 0.7827 0.050 Uiso 1 1 calc R . . H62B H 0.4997 0.2605 0.7960 0.050 Uiso 1 1 calc R . . C101 C 0.7748(5) 0.3833(4) 0.7485(4) 0.053(3) Uani 1 1 d . . . H10B H 0.7830 0.4165 0.7354 0.079 Uiso 1 1 calc R . . H10C H 0.8068 0.3753 0.7825 0.079 Uiso 1 1 calc R . . H10D H 0.7360 0.3848 0.7537 0.079 Uiso 1 1 calc R . . C102 C 0.7724(4) 0.3419(4) 0.7076(4) 0.034(3) Uani 1 1 d . . . C103 C 0.7606(4) 0.2931(3) 0.7236(4) 0.030(2) Uani 1 1 d . . . H10E H 0.7454 0.2916 0.7519 0.036 Uiso 1 1 calc R . . C104 C 0.7692(4) 0.2465(4) 0.7014(4) 0.031(2) Uani 1 1 d . . . C105 C 0.7676(5) 0.1998(4) 0.7341(4) 0.040(3) Uani 1 1 d . . . H10F H 0.7741 0.1691 0.7158 0.060 Uiso 1 1 calc R . . H10G H 0.7283 0.1975 0.7381 0.060 Uiso 1 1 calc R . . H10H H 0.7993 0.2023 0.7694 0.060 Uiso 1 1 calc R . . C106 C 0.7952(4) 0.1929(4) 0.6391(4) 0.031(2) Uani 1 1 d . . . C107 C 0.8585(5) 0.1859(4) 0.6456(4) 0.034(3) Uani 1 1 d . . . C108 C 0.8720(6) 0.1409(5) 0.6263(5) 0.064(4) Uani 1 1 d . . . H10I H 0.9128 0.1340 0.6308 0.076 Uiso 1 1 calc R . . C109 C 0.8278(6) 0.1043(4) 0.6000(5) 0.063(4) Uani 1 1 d . . . H10J H 0.8391 0.0739 0.5867 0.075 Uiso 1 1 calc R . . C110 C 0.7696(5) 0.1120(4) 0.5935(5) 0.047(3) Uani 1 1 d . . . H11A H 0.7403 0.0874 0.5747 0.057 Uiso 1 1 calc R . . C111 C 0.7517(5) 0.1556(4) 0.6140(4) 0.038(3) Uani 1 1 d . . . C112 C 0.6854(5) 0.1610(4) 0.6066(4) 0.035(3) Uani 1 1 d . . . H11B H 0.6802 0.1942 0.6230 0.042 Uiso 1 1 calc R . . C113 C 0.6443(5) 0.1613(4) 0.5491(4) 0.053(3) Uani 1 1 d . . . H11C H 0.6562 0.1889 0.5301 0.080 Uiso 1 1 calc R . . H11D H 0.6028 0.1667 0.5471 0.080 Uiso 1 1 calc R . . H11E H 0.6472 0.1284 0.5326 0.080 Uiso 1 1 calc R . . C114 C 0.6654(5) 0.1165(4) 0.6364(4) 0.048(3) Uani 1 1 d . . . H11F H 0.6228 0.1206 0.6313 0.071 Uiso 1 1 calc R . . H11G H 0.6896 0.1177 0.6746 0.071 Uiso 1 1 calc R . . H11H H 0.6715 0.0835 0.6217 0.071 Uiso 1 1 calc R . . C115 C 0.9042(5) 0.2243(4) 0.6765(4) 0.042(3) Uani 1 1 d . . . H11I H 0.8874 0.2594 0.6660 0.050 Uiso 1 1 calc R . . C116 C 0.9206(5) 0.2180(4) 0.7370(4) 0.056(3) Uani 1 1 d . . . H11J H 0.8841 0.2210 0.7459 0.083 Uiso 1 1 calc R . . H11K H 0.9493 0.2447 0.7558 0.083 Uiso 1 1 calc R . . H11L H 0.9389 0.1843 0.7480 0.083 Uiso 1 1 calc R . . C117 C 0.9633(5) 0.2191(4) 0.6646(5) 0.056(3) Uani 1 1 d . . . H11M H 0.9543 0.2228 0.6261 0.084 Uiso 1 1 calc R . . H11N H 0.9811 0.1854 0.6763 0.084 Uiso 1 1 calc R . . H11O H 0.9917 0.2458 0.6838 0.084 Uiso 1 1 calc R . . C118 C 0.8027(5) 0.4047(3) 0.6579(4) 0.030(2) Uani 1 1 d . . . C119 C 0.7637(5) 0.4431(4) 0.6281(4) 0.038(3) Uani 1 1 d . . . C120 C 0.7866(6) 0.4916(4) 0.6269(5) 0.052(3) Uani 1 1 d . . . H12B H 0.7604 0.5180 0.6074 0.062 Uiso 1 1 calc R . . C121 C 0.8475(6) 0.5025(4) 0.6537(5) 0.059(4) Uani 1 1 d . . . H12C H 0.8628 0.5359 0.6530 0.071 Uiso 1 1 calc R . . C122 C 0.8853(6) 0.4634(4) 0.6816(4) 0.051(3) Uani 1 1 d . . . H12D H 0.9269 0.4704 0.6993 0.061 Uiso 1 1 calc R . . C123 C 0.8644(5) 0.4151(4) 0.6844(4) 0.040(3) Uani 1 1 d . . . C124 C 0.6973(4) 0.4342(4) 0.5988(4) 0.036(3) Uani 1 1 d . . . H12E H 0.6925 0.3972 0.5887 0.043 Uiso 1 1 calc R . . C125 C 0.6703(5) 0.4651(4) 0.5461(5) 0.060(4) Uani 1 1 d . . . H12F H 0.6942 0.4591 0.5235 0.091 Uiso 1 1 calc R . . H12G H 0.6709 0.5017 0.5545 0.091 Uiso 1 1 calc R . . H12H H 0.6287 0.4542 0.5272 0.091 Uiso 1 1 calc R . . C126 C 0.6600(6) 0.4437(5) 0.6335(6) 0.076(4) Uani 1 1 d . . . H12I H 0.6768 0.4241 0.6668 0.114 Uiso 1 1 calc R . . H12J H 0.6184 0.4328 0.6144 0.114 Uiso 1 1 calc R . . H12K H 0.6607 0.4802 0.6419 0.114 Uiso 1 1 calc R . . C127 C 0.9090(5) 0.3748(4) 0.7170(4) 0.045(3) Uani 1 1 d . . . H12L H 0.8865 0.3420 0.7147 0.055 Uiso 1 1 calc R . . C128 C 0.9374(6) 0.3902(6) 0.7773(5) 0.091(5) Uani 1 1 d . . . H12M H 0.9657 0.3636 0.7970 0.137 Uiso 1 1 calc R . . H12N H 0.9054 0.3938 0.7922 0.137 Uiso 1 1 calc R . . H12O H 0.9587 0.4228 0.7805 0.137 Uiso 1 1 calc R . . C129 C 0.9597(5) 0.3649(4) 0.6961(5) 0.058(3) Uani 1 1 d . . . H12P H 0.9426 0.3552 0.6583 0.087 Uiso 1 1 calc R . . H12Q H 0.9852 0.3371 0.7166 0.087 Uiso 1 1 calc R . . H12R H 0.9838 0.3960 0.6998 0.087 Uiso 1 1 calc R . . C130 C 0.8156(5) 0.4183(4) 0.3216(4) 0.044(3) Uani 1 1 d . . . H13D H 0.7860 0.4417 0.3269 0.066 Uiso 1 1 calc R . . H13E H 0.7983 0.4021 0.2864 0.066 Uiso 1 1 calc R . . H13F H 0.8518 0.4374 0.3237 0.066 Uiso 1 1 calc R . . C131 C 0.8318(5) 0.3777(4) 0.3643(4) 0.039(3) Uani 1 1 d . . . C132 C 0.8741(4) 0.3409(4) 0.3620(4) 0.036(3) Uani 1 1 d . . . H13G H 0.8801 0.3402 0.3288 0.044 Uiso 1 1 calc R . . C133 C 0.9089(4) 0.3053(4) 0.3988(4) 0.031(2) Uani 1 1 d . . . C134 C 0.9570(5) 0.2798(5) 0.3874(5) 0.063(4) Uani 1 1 d . . . H13H H 0.9777 0.2561 0.4166 0.094 Uiso 1 1 calc R . . H13I H 0.9857 0.3053 0.3841 0.094 Uiso 1 1 calc R . . H13J H 0.9402 0.2606 0.3538 0.094 Uiso 1 1 calc R . . C135 C 0.9462(5) 0.2668(4) 0.4853(4) 0.035(3) Uani 1 1 d . . . C136 C 0.9408(5) 0.2146(4) 0.4917(4) 0.043(3) Uani 1 1 d . . . C137 C 0.9869(5) 0.1899(4) 0.5334(4) 0.047(3) Uani 1 1 d . . . H13K H 0.9835 0.1543 0.5388 0.056 Uiso 1 1 calc R . . C138 C 1.0369(5) 0.2159(5) 0.5667(4) 0.043(3) Uani 1 1 d . . . H13L H 1.0684 0.1983 0.5934 0.052 Uiso 1 1 calc R . . C139 C 1.0395(5) 0.2679(5) 0.5600(4) 0.043(3) Uani 1 1 d . . . H13M H 1.0726 0.2864 0.5839 0.052 Uiso 1 1 calc R . . C140 C 0.9953(4) 0.2949(4) 0.5192(4) 0.036(3) Uani 1 1 d . . . C141 C 0.8879(5) 0.1831(4) 0.4552(5) 0.054(3) Uani 1 1 d . . . H14D H 0.8556 0.2081 0.4359 0.065 Uiso 1 1 calc R . . C142 C 0.8611(5) 0.1481(5) 0.4852(5) 0.069(4) Uani 1 1 d . . . H42D H 0.8275 0.1292 0.4597 0.103 Uiso 1 1 calc R . . H42E H 0.8466 0.1683 0.5090 0.103 Uiso 1 1 calc R . . H42F H 0.8919 0.1239 0.5064 0.103 Uiso 1 1 calc R . . C143 C 0.9031(7) 0.1544(6) 0.4134(6) 0.108(6) Uani 1 1 d . . . H14E H 0.8678 0.1349 0.3912 0.162 Uiso 1 1 calc R . . H14F H 0.9365 0.1309 0.4306 0.162 Uiso 1 1 calc R . . H14G H 0.9149 0.1786 0.3909 0.162 Uiso 1 1 calc R . . C144 C 1.0024(5) 0.3511(4) 0.5138(4) 0.047(3) Uani 1 1 d . . . H14H H 0.9649 0.3637 0.4854 0.057 Uiso 1 1 calc R . . C145 C 1.0549(6) 0.3641(4) 0.4961(5) 0.063(4) Uani 1 1 d . . . H14I H 1.0507 0.3453 0.4633 0.095 Uiso 1 1 calc R . . H14J H 1.0928 0.3544 0.5243 0.095 Uiso 1 1 calc R . . H14K H 1.0550 0.4009 0.4894 0.095 Uiso 1 1 calc R . . C146 C 1.0093(5) 0.3804(4) 0.5648(4) 0.052(3) Uani 1 1 d . . . H14L H 0.9755 0.3723 0.5763 0.078 Uiso 1 1 calc R . . H14M H 1.0097 0.4172 0.5580 0.078 Uiso 1 1 calc R . . H14N H 1.0472 0.3706 0.5929 0.078 Uiso 1 1 calc R . . C147 C 0.7703(5) 0.4216(4) 0.4046(4) 0.036(3) Uani 1 1 d . . . C148 C 0.7089(5) 0.4241(4) 0.3702(4) 0.039(3) Uani 1 1 d . . . C149 C 0.6758(5) 0.4668(5) 0.3769(5) 0.056(4) Uani 1 1 d . . . H14O H 0.6343 0.4695 0.3556 0.067 Uiso 1 1 calc R . . C150 C 0.7019(6) 0.5044(5) 0.4134(5) 0.062(4) Uani 1 1 d . . . H15B H 0.6789 0.5330 0.4168 0.074 Uiso 1 1 calc R . . C151 C 0.7629(5) 0.5005(4) 0.4456(5) 0.054(3) Uani 1 1 d . . . H15C H 0.7809 0.5269 0.4705 0.065 Uiso 1 1 calc R . . C152 C 0.7971(5) 0.4593(4) 0.4422(4) 0.038(3) Uani 1 1 d . . . C153 C 0.6776(5) 0.3825(5) 0.3315(4) 0.052(3) Uani 1 1 d . . . H15D H 0.7091 0.3585 0.3287 0.062 Uiso 1 1 calc R . . C154 C 0.6419(5) 0.4025(5) 0.2752(4) 0.066(4) Uani 1 1 d . . . H15E H 0.6687 0.4220 0.2617 0.099 Uiso 1 1 calc R . . H15F H 0.6093 0.4247 0.2766 0.099 Uiso 1 1 calc R . . H15G H 0.6249 0.3736 0.2513 0.099 Uiso 1 1 calc R . . C155 C 0.6355(5) 0.3521(4) 0.3528(4) 0.053(3) Uani 1 1 d . . . H15H H 0.6584 0.3394 0.3887 0.079 Uiso 1 1 calc R . . H15I H 0.6183 0.3232 0.3289 0.079 Uiso 1 1 calc R . . H15J H 0.6030 0.3745 0.3543 0.079 Uiso 1 1 calc R . . C156 C 0.8619(5) 0.4553(4) 0.4800(4) 0.044(3) Uani 1 1 d . . . H15K H 0.8734 0.4184 0.4814 0.052 Uiso 1 1 calc R . . C157 C 0.8731(6) 0.4719(5) 0.5369(5) 0.074(4) Uani 1 1 d . . . H15L H 0.8459 0.4533 0.5507 0.111 Uiso 1 1 calc R . . H15M H 0.8657 0.5087 0.5376 0.111 Uiso 1 1 calc R . . H15N H 0.9149 0.4645 0.5592 0.111 Uiso 1 1 calc R . . C158 C 0.9045(6) 0.4850(6) 0.4579(5) 0.093(5) Uani 1 1 d . . . H15O H 0.9461 0.4819 0.4830 0.140 Uiso 1 1 calc R . . H15P H 0.8930 0.5212 0.4537 0.140 Uiso 1 1 calc R . . H15Q H 0.9015 0.4708 0.4232 0.140 Uiso 1 1 calc R . . C159 C 0.6127(4) 0.3058(5) 0.5115(4) 0.063(4) Uani 1 1 d . . . H15R H 0.6195 0.3092 0.4788 0.076 Uiso 1 1 calc R . . C160 C 0.5561(6) 0.3048(8) 0.5157(5) 0.129(8) Uani 1 1 d . . . H16D H 0.5189 0.2973 0.4881 0.155 Uiso 1 1 calc R . . C161 C 0.5652(5) 0.3175(6) 0.5703(5) 0.073(4) Uani 1 1 d . . . H16E H 0.5359 0.2991 0.5824 0.087 Uiso 1 1 calc R . . H16F H 0.5603 0.3547 0.5741 0.087 Uiso 1 1 calc R . . C162 C 0.6280(5) 0.3013(4) 0.6020(4) 0.039(3) Uani 1 1 d . . . H16G H 0.6472 0.3257 0.6314 0.046 Uiso 1 1 calc R . . H16H H 0.6283 0.2668 0.6175 0.046 Uiso 1 1 calc R . . C201 C 0.5604(8) 0.3374(6) 0.7059(7) 0.096(5) Uiso 1 1 d . . . C202 C 0.5108(6) 0.3080(5) 0.6763(5) 0.068(4) Uiso 1 1 d . . . H20B H 0.4743 0.3243 0.6553 0.081 Uiso 1 1 calc R . . C203 C 0.5145(8) 0.2578(6) 0.6777(6) 0.098(5) Uiso 1 1 d . . . H20C H 0.4795 0.2404 0.6555 0.118 Uiso 1 1 calc R . . C204 C 0.5632(8) 0.2259(6) 0.7075(6) 0.106(6) Uiso 1 1 d . . . H20D H 0.5743 0.2025 0.6835 0.127 Uiso 1 1 calc R . . H20E H 0.5522 0.2052 0.7336 0.127 Uiso 1 1 calc R . . C205 C 0.6136(8) 0.2602(6) 0.7353(6) 0.104(5) Uiso 1 1 d . . . H20F H 0.6511 0.2443 0.7544 0.125 Uiso 1 1 calc R . . C206 C 0.6127(7) 0.3108(5) 0.7368(6) 0.081(4) Uiso 1 1 d . . . H20G H 0.6472 0.3291 0.7586 0.097 Uiso 1 1 calc R . . C207 C 0.5554(8) 0.3889(6) 0.7023(6) 0.118(6) Uiso 1 1 d . . . H20H H 0.5149 0.3982 0.6781 0.177 Uiso 1 1 calc R . . H20I H 0.5853 0.4026 0.6884 0.177 Uiso 1 1 calc R . . H20J H 0.5623 0.4033 0.7378 0.177 Uiso 1 1 calc R . . C301 C -0.1289(9) 0.5699(7) 0.8896(8) 0.035(5) Uiso 0.50 1 d P . . C302 C -0.1027(10) 0.5778(8) 0.8592(8) 0.042(6) Uiso 0.50 1 d P . . H302 H -0.0726 0.6036 0.8699 0.051 Uiso 0.50 1 calc PR . . C303 C -0.1102(11) 0.5557(8) 0.8136(9) 0.051(6) Uiso 0.50 1 d P . . H30D H -0.0870 0.5654 0.7927 0.061 Uiso 0.50 1 calc PR . . C304 C -0.1505(10) 0.5202(8) 0.7978(9) 0.051(6) Uiso 0.50 1 d P . . H30E H -0.1571 0.5034 0.7647 0.061 Uiso 0.50 1 calc PR . . C305 C -0.1860(11) 0.5055(9) 0.8304(10) 0.060(7) Uiso 0.50 1 d P . . H30F H -0.2170 0.4806 0.8189 0.072 Uiso 0.50 1 calc PR . . C306 C -0.1720(11) 0.5294(8) 0.8767(10) 0.054(7) Uiso 0.50 1 d P . . H30G H -0.1906 0.5196 0.9013 0.065 Uiso 0.50 1 calc PR . . C307 C -0.1167(12) 0.5877(9) 0.9367(10) 0.067(8) Uiso 0.50 1 d P . . H30H H -0.0869 0.6152 0.9430 0.100 Uiso 0.50 1 calc PR . . H30I H -0.1003 0.5603 0.9629 0.100 Uiso 0.50 1 calc PR . . H30J H -0.1535 0.6012 0.9404 0.100 Uiso 0.50 1 calc PR . . C401 C -0.3491(7) 0.4641(5) 0.8435(6) 0.074(4) Uiso 1 1 d . . . C402 C -0.3128(8) 0.4258(7) 0.8352(8) 0.125(7) Uiso 1 1 d . . . H40A H -0.3016 0.4250 0.8045 0.149 Uiso 1 1 calc R . . C403 C -0.2938(9) 0.3881(7) 0.8759(8) 0.131(7) Uiso 1 1 d . . . H40B H -0.2713 0.3598 0.8708 0.158 Uiso 1 1 calc R . . C404 C -0.3061(7) 0.3903(6) 0.9224(6) 0.090(5) Uiso 1 1 d . . . H40C H -0.2919 0.3647 0.9491 0.108 Uiso 1 1 calc R . . C405 C -0.3376(7) 0.4282(5) 0.9283(6) 0.087(5) Uiso 1 1 d . . . H40D H -0.3447 0.4318 0.9608 0.104 Uiso 1 1 calc R . . C406 C -0.3623(6) 0.4655(5) 0.8864(6) 0.077(4) Uiso 1 1 d . . . H40E H -0.3886 0.4913 0.8904 0.093 Uiso 1 1 calc R . . C407 C -0.3669(7) 0.5021(5) 0.8001(6) 0.093(5) Uiso 1 1 d . . . H40F H -0.3919 0.5285 0.8079 0.140 Uiso 1 1 calc R . . H40G H -0.3899 0.4852 0.7663 0.140 Uiso 1 1 calc R . . H40H H -0.3308 0.5180 0.7972 0.140 Uiso 1 1 calc R . . C501 C 0.0616(6) 0.5191(5) 0.7709(4) 0.204(11) Uiso 1 1 d GD . . C502 C 0.0731(5) 0.4846(4) 0.7361(5) 0.105(6) Uiso 1 1 d GD . . C503 C 0.0524(5) 0.4947(4) 0.6816(4) 0.089(5) Uiso 1 1 d GD . . C504 C 0.0202(6) 0.5392(5) 0.6618(4) 0.155(8) Uiso 1 1 d GD . . C505 C 0.0087(6) 0.5737(4) 0.6965(6) 0.187(10) Uiso 1 1 d GD . . C506 C 0.0294(7) 0.5636(5) 0.7511(6) 0.239(13) Uiso 1 1 d GD . . C507 C 0.068(2) 0.5021(11) 0.8276(7) 0.183(19) Uiso 0.50 1 d PD . . C57A C -0.0072(17) 0.5495(11) 0.6019(5) 0.158(17) Uiso 0.50 1 d PD . . C601 C 0.4910(6) 0.4869(5) 0.5260(5) 0.211(12) Uiso 1 1 d G . . C602 C 0.4760(6) 0.4769(5) 0.5707(5) 0.105(11) Uiso 0.50 1 d PG . . C603 C 0.4429(5) 0.4335(7) 0.5722(4) 0.089(10) Uiso 0.50 1 d PG . . C604 C 0.4250(6) 0.4000(5) 0.5291(5) 0.100(11) Uiso 0.50 1 d PG . . C605 C 0.4400(5) 0.4100(4) 0.4844(5) 0.082(9) Uiso 0.50 1 d PG . . C606 C 0.4731(5) 0.4535(5) 0.4829(5) 0.045(6) Uiso 0.50 1 d PG . . C701 C -0.0344(6) 0.4914(8) 0.0577(5) 0.110(12) Uiso 0.50 1 d PG . . C702 C 0.0073(7) 0.5227(7) 0.0701(5) 0.079(17) Uiso 0.25 1 d PG . . C703 C 0.0445(7) 0.5227(8) 0.0333(5) 0.113(12) Uiso 0.50 1 d PG . . C704 C 0.0124(7) 0.5029(9) -0.0102(5) 0.13(3) Uiso 0.25 1 d PG . . C705 C -0.0719(7) 0.4825(9) 0.0137(6) 0.16(3) Uiso 0.25 1 d PG . . 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 0.0252(3) 0.0405(3) 0.0172(3) -0.0014(2) 0.0064(2) -0.0027(3) Sm2 0.0218(3) 0.0323(3) 0.0190(3) 0.0011(2) 0.0064(2) -0.0053(2) Sm11 0.0227(3) 0.0346(3) 0.0212(3) 0.0027(2) 0.0074(2) -0.0002(2) Sm12 0.0191(3) 0.0421(3) 0.0205(3) 0.0025(2) 0.0049(2) 0.0011(2) Cl1 0.074(2) 0.0474(16) 0.0352(16) 0.0109(13) 0.0324(16) 0.0214(15) Cl2 0.0235(15) 0.088(2) 0.0247(15) 0.0039(15) 0.0055(12) 0.0024(14) Cl3 0.064(2) 0.0496(16) 0.0362(16) -0.0150(13) 0.0332(16) -0.0271(15) Cl4 0.054(2) 0.0466(16) 0.0255(15) 0.0053(12) 0.0099(14) 0.0065(14) Cl11 0.062(2) 0.0488(17) 0.0432(17) 0.0196(14) 0.0326(16) 0.0224(15) Cl12 0.0484(18) 0.0445(16) 0.0421(17) -0.0116(13) 0.0281(15) -0.0156(13) Cl13 0.0231(15) 0.091(2) 0.0251(15) 0.0013(15) 0.0102(12) -0.0062(14) Cl14 0.0383(18) 0.0655(19) 0.0269(15) -0.0047(14) 0.0013(13) -0.0061(14) O1 0.024(4) 0.062(5) 0.016(4) 0.001(3) -0.002(3) -0.005(4) O101 0.027(4) 0.059(5) 0.020(4) -0.003(3) 0.009(3) -0.001(3) N1 0.026(5) 0.037(5) 0.030(5) 0.001(4) 0.011(4) -0.003(4) N2 0.026(5) 0.041(5) 0.027(5) -0.007(4) 0.006(4) -0.005(4) N3 0.018(5) 0.030(4) 0.025(5) 0.010(4) 0.002(4) -0.010(4) N4 0.022(5) 0.040(5) 0.041(6) -0.005(4) 0.002(4) -0.014(4) N101 0.028(5) 0.032(5) 0.031(5) 0.001(4) 0.011(4) -0.003(4) N102 0.029(5) 0.033(5) 0.020(5) -0.005(4) 0.007(4) 0.000(4) N103 0.018(5) 0.050(5) 0.033(5) 0.009(4) 0.006(4) -0.005(4) N104 0.017(5) 0.056(6) 0.025(5) -0.006(4) 0.010(4) -0.002(4) C1 0.054(8) 0.054(7) 0.032(7) 0.008(6) 0.004(6) -0.008(6) C2 0.018(6) 0.050(7) 0.018(6) 0.001(5) 0.004(5) -0.002(5) C3 0.052(8) 0.044(7) 0.011(5) 0.002(5) 0.015(5) -0.011(6) C4 0.013(6) 0.055(7) 0.020(6) -0.016(5) 0.000(4) 0.006(5) C5 0.029(7) 0.070(8) 0.030(6) -0.009(6) 0.004(5) 0.001(6) C6 0.031(7) 0.043(6) 0.017(5) -0.005(5) 0.004(5) -0.002(5) C7 0.030(7) 0.053(7) 0.025(6) -0.004(5) 0.002(5) 0.001(5) C8 0.036(8) 0.051(8) 0.077(10) 0.004(7) 0.011(7) -0.012(6) C9 0.070(11) 0.039(7) 0.084(11) 0.018(7) 0.026(9) 0.003(7) C10 0.045(8) 0.037(7) 0.069(9) 0.009(6) 0.019(7) 0.016(6) C11 0.051(8) 0.041(7) 0.019(6) -0.006(5) 0.016(6) 0.000(6) C12 0.020(6) 0.050(7) 0.043(7) 0.010(6) 0.009(5) -0.003(5) C13 0.026(7) 0.068(8) 0.072(9) 0.008(7) 0.009(7) -0.004(6) C14 0.034(7) 0.067(8) 0.037(7) -0.003(6) 0.003(6) 0.000(6) C15 0.028(7) 0.056(7) 0.044(8) -0.006(6) 0.008(6) 0.009(6) C16 0.040(9) 0.127(12) 0.040(8) -0.025(8) -0.003(7) 0.018(8) C17 0.053(9) 0.082(9) 0.046(8) -0.022(7) 0.004(7) 0.014(7) C18 0.038(7) 0.035(6) 0.022(6) 0.005(5) 0.012(5) -0.010(5) C19 0.039(7) 0.035(6) 0.036(7) 0.007(5) 0.012(6) -0.002(5) C20 0.059(9) 0.042(7) 0.047(8) 0.000(6) 0.015(7) -0.013(6) C21 0.061(9) 0.045(7) 0.045(8) 0.017(6) 0.021(7) 0.012(7) C22 0.040(8) 0.056(8) 0.041(7) 0.020(6) 0.008(6) 0.001(6) C23 0.034(7) 0.042(7) 0.029(6) 0.004(5) 0.010(5) -0.002(5) C24 0.041(8) 0.045(7) 0.045(7) -0.006(6) 0.003(6) -0.012(6) C25 0.078(10) 0.057(8) 0.038(7) -0.007(6) 0.012(7) -0.031(7) C26 0.039(8) 0.150(13) 0.036(8) -0.016(8) 0.011(7) -0.008(9) C27 0.028(7) 0.066(8) 0.046(8) 0.008(6) 0.011(6) 0.005(6) C28 0.048(9) 0.152(14) 0.037(8) 0.017(9) -0.005(7) -0.035(9) C29 0.036(7) 0.053(7) 0.044(7) 0.008(6) 0.002(6) -0.004(6) C30 0.054(8) 0.038(6) 0.034(6) -0.006(5) 0.028(6) -0.011(5) C31 0.016(5) 0.035(6) 0.019(5) 0.007(4) -0.002(4) 0.002(4) C32 0.032(7) 0.038(6) 0.032(6) 0.012(5) 0.006(5) -0.008(5) C33 0.020(6) 0.051(7) 0.034(7) 0.007(6) 0.006(5) 0.000(5) C34 0.042(8) 0.097(9) 0.033(7) 0.005(7) 0.022(6) -0.032(7) C35 0.028(7) 0.067(8) 0.033(7) -0.009(6) 0.019(6) -0.020(6) C36 0.052(9) 0.065(9) 0.044(8) -0.007(7) 0.021(7) -0.026(7) C37 0.060(10) 0.072(9) 0.055(9) -0.021(7) 0.031(8) -0.039(8) C38 0.055(10) 0.115(13) 0.055(10) -0.026(9) 0.005(8) -0.051(10) C39 0.051(9) 0.114(12) 0.032(8) -0.009(8) 0.003(7) -0.033(9) C40 0.024(7) 0.094(10) 0.036(7) -0.002(7) 0.007(6) -0.032(7) C41 0.090(12) 0.046(8) 0.064(9) 0.001(7) 0.028(9) -0.031(8) C42 0.17(2) 0.21(2) 0.22(2) 0.17(2) 0.12(2) 0.106(18) C43 0.115(17) 0.090(12) 0.19(2) -0.067(13) 0.050(16) -0.036(11) C44 0.031(8) 0.090(11) 0.058(9) 0.020(8) -0.014(7) -0.006(7) C45 0.066(11) 0.143(14) 0.064(10) 0.012(10) 0.035(9) 0.004(10) C46 0.041(9) 0.114(12) 0.093(12) 0.015(10) 0.018(9) 0.018(8) C47 0.038(7) 0.025(5) 0.037(6) -0.001(5) 0.018(6) -0.003(5) C48 0.043(7) 0.039(6) 0.032(6) -0.008(5) 0.022(6) -0.016(5) C49 0.048(8) 0.054(7) 0.040(7) -0.011(6) 0.023(6) -0.026(6) C50 0.076(11) 0.040(7) 0.062(9) -0.010(7) 0.045(8) -0.018(7) C51 0.055(9) 0.045(7) 0.060(9) 0.011(6) 0.035(7) -0.001(6) C52 0.045(7) 0.028(6) 0.044(7) 0.014(5) 0.026(6) 0.002(5) C53 0.026(6) 0.055(7) 0.035(7) -0.012(5) 0.019(5) -0.017(5) C54 0.035(8) 0.091(9) 0.051(8) -0.005(7) 0.023(7) 0.008(7) C55 0.056(9) 0.077(9) 0.035(7) 0.002(6) 0.006(6) -0.025(7) C56 0.043(8) 0.053(7) 0.049(8) 0.030(6) 0.010(6) 0.010(6) C57 0.063(10) 0.073(9) 0.066(10) 0.020(8) 0.019(8) 0.007(7) C58 0.052(9) 0.119(12) 0.055(9) 0.025(8) 0.026(8) 0.017(8) C59 0.031(7) 0.130(12) 0.020(6) 0.007(7) 0.005(5) -0.011(7) C60 0.047(9) 0.176(16) 0.041(8) 0.035(10) -0.003(7) -0.017(10) C61 0.031(7) 0.105(10) 0.041(8) 0.003(7) 0.008(6) -0.004(7) C62 0.018(6) 0.079(8) 0.028(6) 0.006(6) 0.010(5) -0.007(6) C101 0.062(9) 0.056(7) 0.050(8) -0.019(6) 0.032(7) -0.009(6) C102 0.027(6) 0.045(7) 0.032(6) -0.005(5) 0.013(5) 0.003(5) C103 0.041(7) 0.030(6) 0.018(5) 0.000(4) 0.009(5) -0.011(5) C104 0.020(6) 0.041(6) 0.034(6) 0.011(5) 0.010(5) 0.001(5) C105 0.044(7) 0.050(7) 0.032(6) 0.012(5) 0.020(6) 0.007(6) C106 0.017(6) 0.039(6) 0.034(6) 0.010(5) 0.006(5) 0.011(5) C107 0.039(7) 0.047(7) 0.025(6) 0.000(5) 0.021(5) 0.015(5) C108 0.040(8) 0.070(9) 0.069(10) 0.000(8) 0.005(7) 0.011(7) C109 0.052(9) 0.040(7) 0.096(11) -0.022(7) 0.027(8) 0.006(7) C110 0.047(8) 0.037(7) 0.067(9) -0.015(6) 0.030(7) -0.005(6) C111 0.043(8) 0.036(6) 0.041(7) 0.003(5) 0.020(6) 0.003(5) C112 0.033(7) 0.032(6) 0.046(7) -0.004(5) 0.021(6) -0.006(5) C113 0.047(8) 0.070(8) 0.044(8) 0.004(7) 0.017(7) -0.016(6) C114 0.059(9) 0.047(7) 0.040(7) -0.006(6) 0.022(6) -0.012(6) C115 0.030(7) 0.056(7) 0.033(7) 0.006(6) 0.004(5) 0.005(6) C116 0.036(8) 0.074(8) 0.049(8) 0.005(7) 0.006(6) 0.002(6) C117 0.047(8) 0.091(9) 0.046(8) 0.002(7) 0.038(7) -0.010(7) C118 0.034(7) 0.029(6) 0.030(6) -0.007(5) 0.016(5) -0.011(5) C119 0.040(7) 0.030(6) 0.048(7) -0.008(5) 0.022(6) -0.004(5) C120 0.058(9) 0.042(7) 0.056(8) -0.007(6) 0.023(7) -0.001(6) C121 0.070(10) 0.043(7) 0.074(10) -0.010(7) 0.036(8) -0.011(7) C122 0.050(8) 0.061(8) 0.037(7) -0.010(6) 0.008(6) -0.012(7) C123 0.042(8) 0.041(7) 0.044(7) -0.006(5) 0.022(6) -0.015(6) C124 0.025(6) 0.036(6) 0.048(7) -0.009(5) 0.016(6) 0.002(5) C125 0.042(8) 0.051(8) 0.075(10) 0.018(7) 0.004(7) 0.016(6) C126 0.058(10) 0.075(9) 0.107(12) -0.030(9) 0.043(9) -0.015(8) C127 0.040(8) 0.052(7) 0.044(7) 0.003(6) 0.013(6) -0.005(6) C128 0.065(11) 0.158(15) 0.047(9) 0.021(10) 0.014(8) 0.025(10) C129 0.049(9) 0.068(8) 0.050(8) -0.005(7) 0.008(7) 0.006(7) C130 0.029(7) 0.063(7) 0.041(7) 0.017(6) 0.014(6) 0.000(6) C131 0.022(6) 0.058(7) 0.030(6) 0.011(5) 0.001(5) -0.018(5) C132 0.021(6) 0.075(8) 0.015(6) -0.005(5) 0.010(5) 0.000(6) C133 0.021(6) 0.059(7) 0.018(6) 0.001(5) 0.014(5) -0.005(5) C134 0.042(8) 0.106(10) 0.044(8) -0.007(7) 0.020(7) 0.008(7) C135 0.031(7) 0.053(7) 0.022(6) -0.002(5) 0.009(5) 0.004(5) C136 0.027(7) 0.061(8) 0.034(7) -0.007(6) 0.002(5) 0.002(6) C137 0.038(8) 0.064(8) 0.049(8) 0.003(6) 0.028(7) 0.010(6) C138 0.027(7) 0.083(9) 0.021(6) 0.007(6) 0.011(5) 0.015(6) C139 0.016(6) 0.071(8) 0.041(7) -0.002(6) 0.008(5) 0.004(6) C140 0.023(6) 0.051(7) 0.033(6) -0.006(5) 0.011(5) 0.014(5) C141 0.034(7) 0.061(8) 0.057(8) 0.001(7) 0.003(6) 0.004(6) C142 0.034(8) 0.095(10) 0.081(10) -0.012(8) 0.025(8) -0.006(7) C143 0.097(14) 0.171(16) 0.074(11) -0.058(11) 0.053(11) -0.057(12) C144 0.025(7) 0.059(8) 0.044(8) -0.012(6) -0.004(6) 0.004(6) C145 0.085(11) 0.073(9) 0.040(8) -0.005(7) 0.032(8) 0.002(8) C146 0.029(7) 0.078(9) 0.057(8) -0.011(7) 0.025(6) -0.006(6) C147 0.031(7) 0.050(7) 0.033(7) 0.024(5) 0.017(6) 0.004(6) C148 0.028(7) 0.055(7) 0.039(7) 0.027(6) 0.019(6) 0.007(6) C149 0.026(7) 0.067(9) 0.071(10) 0.035(8) 0.013(7) 0.007(7) C150 0.047(9) 0.055(8) 0.081(11) 0.040(8) 0.021(8) 0.019(7) C151 0.044(8) 0.043(7) 0.073(9) 0.024(6) 0.019(7) 0.003(6) C152 0.030(7) 0.038(6) 0.051(8) 0.007(6) 0.020(6) -0.001(5) C153 0.034(7) 0.073(9) 0.043(8) 0.026(7) 0.008(6) -0.007(6) C154 0.029(7) 0.110(11) 0.049(8) 0.031(8) 0.001(6) -0.007(7) C155 0.031(7) 0.068(8) 0.055(8) 0.005(7) 0.011(6) -0.011(6) C156 0.033(7) 0.051(7) 0.042(7) -0.001(6) 0.007(6) -0.004(6) C157 0.058(10) 0.109(11) 0.048(9) -0.008(8) 0.011(7) 0.007(8) C158 0.054(10) 0.155(14) 0.072(11) -0.013(10) 0.025(9) -0.019(10) C159 0.001(5) 0.149(12) 0.032(7) 0.001(8) -0.004(5) 0.005(7) C160 0.024(8) 0.31(3) 0.041(9) -0.058(12) -0.004(7) 0.031(12) C161 0.039(8) 0.120(12) 0.058(9) -0.008(9) 0.016(7) 0.014(8) C162 0.038(7) 0.053(7) 0.023(6) -0.003(5) 0.010(5) 0.000(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N2 2.357(7) . ? Sm1 N1 2.390(8) . ? Sm1 O1 2.434(7) . ? Sm1 Cl2 2.719(3) . ? Sm1 Cl3 2.748(3) . ? Sm1 Cl1 2.768(3) . ? Sm1 Sm2 3.9199(7) . ? Sm2 N3 2.362(8) . ? Sm2 N4 2.372(8) . ? Sm2 Cl4 2.605(3) . ? Sm2 Cl1 2.808(3) . ? Sm2 Cl3 2.815(2) . ? Sm2 Cl2 2.834(3) . ? Sm11 N102 2.382(7) . ? Sm11 N101 2.392(8) . ? Sm11 O101 2.400(7) . ? Sm11 Cl13 2.717(3) . ? Sm11 Cl11 2.748(3) . ? Sm11 Cl12 2.767(3) . ? Sm11 Sm12 3.9309(7) . ? Sm12 N103 2.371(8) . ? Sm12 N104 2.394(7) . ? Sm12 Cl14 2.614(3) . ? Sm12 Cl11 2.812(3) . ? Sm12 Cl12 2.819(2) . ? Sm12 Cl13 2.825(3) . ? O1 C62 1.460(10) . ? O1 C59 1.492(12) . ? O101 C159 1.449(12) . ? O101 C162 1.486(11) . ? N1 C2 1.364(11) . ? N1 C18 1.442(12) . ? N2 C4 1.365(11) . ? N2 C6 1.459(12) . ? N3 C31 1.347(11) . ? N3 C47 1.459(11) . ? N4 C33 1.333(12) . ? N4 C35 1.452(12) . ? N101 C102 1.341(11) . ? N101 C118 1.446(11) . ? N102 C104 1.328(11) . ? N102 C106 1.463(11) . ? N103 C131 1.351(12) . ? N103 C147 1.457(12) . ? N104 C133 1.341(11) . ? N104 C135 1.466(12) . ? C1 C2 1.508(12) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.366(13) . ? C3 C4 1.387(13) . ? C3 H3A 0.9500 . ? C4 C5 1.535(12) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.385(13) . ? C6 C11 1.396(13) . ? C7 C8 1.412(14) . ? C7 C12 1.517(13) . ? C8 C9 1.390(15) . ? C8 H8A 0.9500 . ? C9 C10 1.368(16) . ? C9 H9A 0.9500 . ? C10 C11 1.365(14) . ? C10 H10A 0.9500 . ? C11 C15 1.548(14) . ? C12 C13 1.528(13) . ? C12 C14 1.546(13) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.515(14) . ? C15 C17 1.541(13) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.390(13) . ? C18 C23 1.396(14) . ? C19 C20 1.382(14) . ? C19 C24 1.545(14) . ? C20 C21 1.380(15) . ? C20 H20A 0.9500 . ? C21 C22 1.377(15) . ? C21 H21A 0.9500 . ? C22 C23 1.384(14) . ? C22 H22A 0.9500 . ? C23 C27 1.520(14) . ? C24 C25 1.513(14) . ? C24 C26 1.541(14) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.536(13) . ? C27 C28 1.548(14) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.521(12) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.412(12) . ? C32 C33 1.391(13) . ? C32 H32A 0.9500 . ? C33 C34 1.549(13) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.386(15) . ? C35 C40 1.423(15) . ? C36 C37 1.425(15) . ? C36 C41 1.505(17) . ? C37 C38 1.365(18) . ? C37 H37A 0.9500 . ? C38 C39 1.397(17) . ? C38 H38A 0.9500 . ? C39 C40 1.380(15) . ? C39 H39A 0.9500 . ? C40 C44 1.501(17) . ? C41 C42 1.487(17) . ? C41 C43 1.565(18) . ? C41 H41A 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C46 1.541(16) . ? C44 C45 1.545(16) . ? C44 H44A 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.397(14) . ? C47 C52 1.410(13) . ? C48 C49 1.377(13) . ? C48 C53 1.503(14) . ? C49 C50 1.386(15) . ? C49 H49A 0.9500 . ? C50 C51 1.362(16) . ? C50 H50A 0.9500 . ? C51 C52 1.410(13) . ? C51 H51A 0.9500 . ? C52 C56 1.512(15) . ? C53 C54 1.529(13) . ? C53 C55 1.553(13) . ? C53 H53A 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C58 1.517(15) . ? C56 C57 1.542(14) . ? C56 H56A 1.0000 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.468(16) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.479(15) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.519(14) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C101 C102 1.524(12) . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C101 H10D 0.9800 . ? C102 C103 1.404(12) . ? C103 C104 1.402(12) . ? C103 H10E 0.9500 . ? C104 C105 1.510(12) . ? C105 H10F 0.9800 . ? C105 H10G 0.9800 . ? C105 H10H 0.9800 . ? C106 C111 1.408(13) . ? C106 C107 1.463(13) . ? C107 C108 1.370(14) . ? C107 C115 1.495(14) . ? C108 C109 1.410(15) . ? C108 H10I 0.9500 . ? C109 C110 1.346(15) . ? C109 H10J 0.9500 . ? C110 C111 1.394(13) . ? C110 H11A 0.9500 . ? C111 C112 1.521(13) . ? C112 C113 1.500(14) . ? C112 C114 1.577(12) . ? C112 H11B 1.0000 . ? C113 H11C 0.9800 . ? C113 H11D 0.9800 . ? C113 H11E 0.9800 . ? C114 H11F 0.9800 . ? C114 H11G 0.9800 . ? C114 H11H 0.9800 . ? C115 C116 1.533(14) . ? C115 C117 1.552(13) . ? C115 H11I 1.0000 . ? C116 H11J 0.9800 . ? C116 H11K 0.9800 . ? C116 H11L 0.9800 . ? C117 H11M 0.9800 . ? C117 H11N 0.9800 . ? C117 H11O 0.9800 . ? C118 C119 1.408(13) . ? C118 C123 1.409(14) . ? C119 C120 1.384(14) . ? C119 C124 1.509(14) . ? C120 C121 1.398(16) . ? C120 H12B 0.9500 . ? C121 C122 1.389(15) . ? C121 H12C 0.9500 . ? C122 C123 1.369(14) . ? C122 H12D 0.9500 . ? C123 C127 1.529(14) . ? C124 C126 1.517(14) . ? C124 C125 1.551(14) . ? C124 H12E 1.0000 . ? C125 H12F 0.9800 . ? C125 H12G 0.9800 . ? C125 H12H 0.9800 . ? C126 H12I 0.9800 . ? C126 H12J 0.9800 . ? C126 H12K 0.9800 . ? C127 C129 1.519(14) . ? C127 C128 1.564(15) . ? C127 H12L 1.0000 . ? C128 H12M 0.9800 . ? C128 H12N 0.9800 . ? C128 H12O 0.9800 . ? C129 H12P 0.9800 . ? C129 H12Q 0.9800 . ? C129 H12R 0.9800 . ? C130 C131 1.506(13) . ? C130 H13D 0.9800 . ? C130 H13E 0.9800 . ? C130 H13F 0.9800 . ? C131 C132 1.409(14) . ? C132 C133 1.392(13) . ? C132 H13G 0.9500 . ? C133 C134 1.448(13) . ? C134 H13H 0.9800 . ? C134 H13I 0.9800 . ? C134 H13J 0.9800 . ? C135 C136 1.388(14) . ? C135 C140 1.403(14) . ? C136 C137 1.410(14) . ? C136 C141 1.530(15) . ? C137 C138 1.384(15) . ? C137 H13K 0.9500 . ? C138 C139 1.377(14) . ? C138 H13L 0.9500 . ? C139 C140 1.407(13) . ? C139 H13M 0.9500 . ? C140 C144 1.492(14) . ? C141 C142 1.498(15) . ? C141 C143 1.497(15) . ? C141 H14D 1.0000 . ? C142 H42D 0.9800 . ? C142 H42E 0.9800 . ? C142 H42F 0.9800 . ? C143 H14E 0.9800 . ? C143 H14F 0.9800 . ? C143 H14G 0.9800 . ? C144 C145 1.522(14) . ? C144 C146 1.523(13) . ? C144 H14H 1.0000 . ? C145 H14I 0.9800 . ? C145 H14J 0.9800 . ? C145 H14K 0.9800 . ? C146 H14L 0.9800 . ? C146 H14M 0.9800 . ? C146 H14N 0.9800 . ? C147 C152 1.390(14) . ? C147 C148 1.424(14) . ? C148 C149 1.412(15) . ? C148 C153 1.504(15) . ? C149 C150 1.369(16) . ? C149 H14O 0.9500 . ? C150 C151 1.401(15) . ? C150 H15B 0.9500 . ? C151 C152 1.373(14) . ? C151 H15C 0.9500 . ? C152 C156 1.515(14) . ? C153 C154 1.534(14) . ? C153 C155 1.537(13) . ? C153 H15D 1.0000 . ? C154 H15E 0.9800 . ? C154 H15F 0.9800 . ? C154 H15G 0.9800 . ? C155 H15H 0.9800 . ? C155 H15I 0.9800 . ? C155 H15J 0.9800 . ? C156 C157 1.514(14) . ? C156 C158 1.552(15) . ? C156 H15K 1.0000 . ? C157 H15L 0.9800 . ? C157 H15M 0.9800 . ? C157 H15N 0.9800 . ? C158 H15O 0.9800 . ? C158 H15P 0.9800 . ? C158 H15Q 0.9800 . ? C159 C160 1.389(16) . ? C159 H15R 0.9500 . ? C160 C161 1.437(16) . ? C160 H16D 0.9500 . ? C161 C162 1.493(15) . ? C161 H16E 0.9900 . ? C161 H16F 0.9900 . ? C162 H16G 0.9900 . ? C162 H16H 0.9900 . ? C201 C207 1.354(19) . ? C201 C202 1.393(19) . ? C201 C206 1.406(19) . ? C202 C203 1.315(16) . ? C202 H20B 0.9500 . ? C203 C204 1.421(19) . ? C203 H20C 0.9500 . ? C204 C205 1.47(2) . ? C204 H20D 0.9900 . ? C204 H20E 0.9900 . ? C205 C206 1.323(18) . ? C205 H20F 0.9500 . ? C206 H20G 0.9500 . ? C207 H20H 0.9800 . ? C207 H20I 0.9800 . ? C207 H20J 0.9800 . ? C301 C302 1.21(3) . ? C301 C307 1.28(3) . ? C301 C306 1.43(3) . ? C302 C303 1.30(3) . ? C302 H302 0.9500 . ? C303 C304 1.29(3) . ? C303 H30D 0.9500 . ? C304 C305 1.46(3) . ? C304 H30E 0.9500 . ? C305 C306 1.32(3) . ? C305 H30F 0.9500 . ? C306 H30G 0.9500 . ? C307 H30H 0.9800 . ? C307 H30I 0.9800 . ? C307 H30J 0.9800 . ? C401 C406 1.295(16) . ? C401 C402 1.390(19) . ? C401 C407 1.471(17) . ? C402 C403 1.42(2) . ? C402 H40A 0.9500 . ? C403 C404 1.38(2) . ? C403 H40B 0.9500 . ? C404 C405 1.285(17) . ? C404 H40C 0.9500 . ? C405 C406 1.442(17) . ? C405 H40D 0.9500 . ? C406 H40E 0.9500 . ? C407 H40F 0.9800 . ? C407 H40G 0.9800 . ? C407 H40H 0.9800 . ? C501 C502 1.3900 . ? C501 C506 1.3900 . ? C501 C507 1.534(7) . ? C502 C503 1.3900 . ? C503 C504 1.3900 . ? C504 C505 1.3900 . ? C504 C57A 1.523(6) . ? C505 C506 1.3900 . ? C601 C602 1.3900 . ? C601 C606 1.3900 . ? C601 C601 1.74(3) 3_666 ? C601 C606 1.83(2) 3_666 ? C602 C603 1.3900 . ? C603 C604 1.3900 . ? C604 C605 1.3900 . ? C605 C606 1.3900 . ? C606 C601 1.83(2) 3_666 ? C701 C705 1.2202 . ? C701 C702 1.2362 . ? C701 C704 1.55(3) 3_565 ? C702 C703 1.5408 . ? C702 C704 1.65(3) 3_565 ? C703 C704 1.2526 . ? C703 C704 1.44(3) 3_565 ? C703 C705 1.61(4) 3_565 ? C704 C704 0.95(4) 3_565 ? C704 C703 1.44(4) 3_565 ? C704 C705 1.50(4) 3_565 ? C704 C701 1.55(3) 3_565 ? C704 C702 1.65(3) 3_565 ? C705 C704 1.50(4) 3_565 ? C705 C703 1.61(4) 3_565 ? 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 N2 Sm1 N1 76.9(3) . . ? N2 Sm1 O1 89.4(2) . . ? N1 Sm1 O1 91.1(2) . . ? N2 Sm1 Cl2 109.6(2) . . ? N1 Sm1 Cl2 105.6(2) . . ? O1 Sm1 Cl2 156.92(15) . . ? N2 Sm1 Cl3 171.5(2) . . ? N1 Sm1 Cl3 107.50(19) . . ? O1 Sm1 Cl3 83.30(16) . . ? Cl2 Sm1 Cl3 76.62(8) . . ? N2 Sm1 Cl1 98.6(2) . . ? N1 Sm1 Cl1 175.02(19) . . ? O1 Sm1 Cl1 86.68(16) . . ? Cl2 Sm1 Cl1 77.79(8) . . ? Cl3 Sm1 Cl1 76.68(8) . . ? N2 Sm1 Sm2 134.54(19) . . ? N1 Sm1 Sm2 139.19(19) . . ? O1 Sm1 Sm2 110.89(14) . . ? Cl2 Sm1 Sm2 46.30(5) . . ? Cl3 Sm1 Sm2 45.89(5) . . ? Cl1 Sm1 Sm2 45.74(5) . . ? N3 Sm2 N4 79.2(3) . . ? N3 Sm2 Cl4 91.25(18) . . ? N4 Sm2 Cl4 94.5(2) . . ? N3 Sm2 Cl1 155.36(19) . . ? N4 Sm2 Cl1 125.3(2) . . ? Cl4 Sm2 Cl1 85.34(8) . . ? N3 Sm2 Cl3 85.28(18) . . ? N4 Sm2 Cl3 144.3(2) . . ? Cl4 Sm2 Cl3 118.03(9) . . ? Cl1 Sm2 Cl3 74.98(8) . . ? N3 Sm2 Cl2 113.50(19) . . ? N4 Sm2 Cl2 83.2(2) . . ? Cl4 Sm2 Cl2 154.06(9) . . ? Cl1 Sm2 Cl2 75.29(8) . . ? Cl3 Sm2 Cl2 73.74(8) . . ? N3 Sm2 Sm1 125.24(17) . . ? N4 Sm2 Sm1 126.0(2) . . ? Cl4 Sm2 Sm1 127.06(6) . . ? Cl1 Sm2 Sm1 44.93(5) . . ? Cl3 Sm2 Sm1 44.51(5) . . ? Cl2 Sm2 Sm1 43.93(5) . . ? N102 Sm11 N101 75.9(2) . . ? N102 Sm11 O101 89.3(2) . . ? N101 Sm11 O101 90.8(2) . . ? N102 Sm11 Cl13 110.60(19) . . ? N101 Sm11 Cl13 108.10(19) . . ? O101 Sm11 Cl13 155.05(16) . . ? N102 Sm11 Cl11 172.1(2) . . ? N101 Sm11 Cl11 106.50(19) . . ? O101 Sm11 Cl11 83.20(16) . . ? Cl13 Sm11 Cl11 76.04(8) . . ? N102 Sm11 Cl12 100.31(18) . . ? N101 Sm11 Cl12 173.91(19) . . ? O101 Sm11 Cl12 84.31(16) . . ? Cl13 Sm11 Cl12 77.61(8) . . ? Cl11 Sm11 Cl12 76.64(8) . . ? N102 Sm11 Sm12 136.20(17) . . ? N101 Sm11 Sm12 139.93(18) . . ? O101 Sm11 Sm12 109.21(15) . . ? Cl13 Sm11 Sm12 45.94(6) . . ? Cl11 Sm11 Sm12 45.68(5) . . ? Cl12 Sm11 Sm12 45.81(5) . . ? N103 Sm12 N104 77.9(3) . . ? N103 Sm12 Cl14 90.9(2) . . ? N104 Sm12 Cl14 92.89(19) . . ? N103 Sm12 Cl11 84.8(2) . . ? N104 Sm12 Cl11 141.25(19) . . ? Cl14 Sm12 Cl11 122.06(9) . . ? N103 Sm12 Cl12 152.6(2) . . ? N104 Sm12 Cl12 129.3(2) . . ? Cl14 Sm12 Cl12 84.79(8) . . ? Cl11 Sm12 Cl12 74.80(8) . . ? N103 Sm12 Cl13 116.7(2) . . ? N104 Sm12 Cl13 83.91(19) . . ? Cl14 Sm12 Cl13 150.54(9) . . ? Cl11 Sm12 Cl13 73.34(8) . . ? Cl12 Sm12 Cl13 75.03(8) . . ? N103 Sm12 Sm11 125.9(2) . . ? N104 Sm12 Sm11 127.12(19) . . ? Cl14 Sm12 Sm11 127.57(6) . . ? Cl11 Sm12 Sm11 44.36(5) . . ? Cl12 Sm12 Sm11 44.75(5) . . ? Cl13 Sm12 Sm11 43.72(5) . . ? Sm1 Cl1 Sm2 89.33(7) . . ? Sm1 Cl2 Sm2 89.77(8) . . ? Sm1 Cl3 Sm2 89.60(7) . . ? Sm11 Cl11 Sm12 89.97(7) . . ? Sm11 Cl12 Sm12 89.45(7) . . ? Sm11 Cl13 Sm12 90.35(8) . . ? C62 O1 C59 111.1(7) . . ? C62 O1 Sm1 126.1(5) . . ? C59 O1 Sm1 122.4(6) . . ? C159 O101 C162 104.5(7) . . ? C159 O101 Sm11 128.8(6) . . ? C162 O101 Sm11 126.3(5) . . ? C2 N1 C18 118.8(8) . . ? C2 N1 Sm1 128.9(6) . . ? C18 N1 Sm1 112.3(6) . . ? C4 N2 C6 118.7(8) . . ? C4 N2 Sm1 129.4(6) . . ? C6 N2 Sm1 111.8(5) . . ? C31 N3 C47 117.2(8) . . ? C31 N3 Sm2 123.1(6) . . ? C47 N3 Sm2 119.0(6) . . ? C33 N4 C35 117.8(8) . . ? C33 N4 Sm2 120.7(7) . . ? C35 N4 Sm2 120.7(6) . . ? C102 N101 C118 117.4(8) . . ? C102 N101 Sm11 129.1(6) . . ? C118 N101 Sm11 113.4(6) . . ? C104 N102 C106 120.2(8) . . ? C104 N102 Sm11 131.9(6) . . ? C106 N102 Sm11 107.9(5) . . ? C131 N103 C147 117.0(8) . . ? C131 N103 Sm12 123.5(7) . . ? C147 N103 Sm12 118.7(6) . . ? C133 N104 C135 116.5(8) . . ? C133 N104 Sm12 123.5(6) . . ? C135 N104 Sm12 118.7(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.3(9) . . ? N1 C2 C1 121.0(9) . . ? C3 C2 C1 115.7(9) . . ? C2 C3 C4 131.4(9) . . ? C2 C3 H3A 114.3 . . ? C4 C3 H3A 114.3 . . ? N2 C4 C3 122.9(8) . . ? N2 C4 C5 120.0(9) . . ? C3 C4 C5 117.0(9) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 121.9(10) . . ? C7 C6 N2 116.6(9) . . ? C11 C6 N2 121.4(9) . . ? C6 C7 C8 117.6(10) . . ? C6 C7 C12 123.6(10) . . ? C8 C7 C12 118.8(10) . . ? C9 C8 C7 120.6(11) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C10 C9 C8 119.2(11) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? C11 C10 C9 122.4(11) . . ? C11 C10 H10A 118.8 . . ? C9 C10 H10A 118.8 . . ? C10 C11 C6 118.3(11) . . ? C10 C11 C15 118.5(10) . . ? C6 C11 C15 123.2(9) . . ? C7 C12 C13 115.1(9) . . ? C7 C12 C14 111.8(9) . . ? C13 C12 C14 109.4(9) . . ? C7 C12 H12A 106.7 . . ? C13 C12 H12A 106.7 . . ? C14 C12 H12A 106.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C17 108.7(9) . . ? C16 C15 C11 111.7(9) . . ? C17 C15 C11 111.8(9) . . ? C16 C15 H15A 108.1 . . ? C17 C15 H15A 108.1 . . ? C11 C15 H15A 108.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.5(10) . . ? C19 C18 N1 121.2(9) . . ? C23 C18 N1 118.3(9) . . ? C20 C19 C18 119.3(11) . . ? C20 C19 C24 119.3(10) . . ? C18 C19 C24 121.4(9) . . ? C21 C20 C19 121.0(11) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C22 C21 C20 119.2(11) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C21 C22 C23 121.6(11) . . ? C21 C22 H22A 119.2 . . ? C23 C22 H22A 119.2 . . ? C22 C23 C18 118.5(10) . . ? C22 C23 C27 118.7(10) . . ? C18 C23 C27 122.7(9) . . ? C25 C24 C26 107.4(9) . . ? C25 C24 C19 113.7(10) . . ? C26 C24 C19 109.2(9) . . ? C25 C24 H24A 108.8 . . ? C26 C24 H24A 108.8 . . ? C19 C24 H24A 108.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 111.3(9) . . ? C23 C27 C28 111.8(9) . . ? C29 C27 C28 107.1(9) . . ? C23 C27 H27A 108.9 . . ? C29 C27 H27A 108.9 . . ? C28 C27 H27A 108.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 C32 123.8(9) . . ? N3 C31 C30 120.2(8) . . ? C32 C31 C30 116.1(9) . . ? C33 C32 C31 129.9(10) . . ? C33 C32 H32A 115.0 . . ? C31 C32 H32A 115.0 . . ? N4 C33 C32 125.7(9) . . ? N4 C33 C34 121.2(9) . . ? C32 C33 C34 113.0(9) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 122.1(11) . . ? C36 C35 N4 119.3(11) . . ? C40 C35 N4 118.5(10) . . ? C35 C36 C37 117.3(13) . . ? C35 C36 C41 123.3(11) . . ? C37 C36 C41 119.4(12) . . ? C38 C37 C36 120.0(13) . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C37 C38 C39 122.7(13) . . ? C37 C38 H38A 118.7 . . ? C39 C38 H38A 118.7 . . ? C40 C39 C38 118.6(14) . . ? C40 C39 H39A 120.7 . . ? C38 C39 H39A 120.7 . . ? C39 C40 C35 119.1(13) . . ? C39 C40 C44 118.3(13) . . ? C35 C40 C44 122.5(10) . . ? C42 C41 C36 112.0(13) . . ? C42 C41 C43 109.0(13) . . ? C36 C41 C43 115.4(12) . . ? C42 C41 H41A 106.6 . . ? C36 C41 H41A 106.6 . . ? C43 C41 H41A 106.6 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 C46 110.5(12) . . ? C40 C44 C45 111.3(11) . . ? C46 C44 C45 110.8(10) . . ? C40 C44 H44A 108.0 . . ? C46 C44 H44A 108.0 . . ? C45 C44 H44A 108.0 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C52 122.7(9) . . ? C48 C47 N3 120.8(9) . . ? C52 C47 N3 116.2(9) . . ? C49 C48 C47 116.2(10) . . ? C49 C48 C53 120.9(10) . . ? C47 C48 C53 122.9(8) . . ? C48 C49 C50 123.8(11) . . ? C48 C49 H49A 118.1 . . ? C50 C49 H49A 118.1 . . ? C51 C50 C49 118.6(11) . . ? C51 C50 H50A 120.7 . . ? C49 C50 H50A 120.7 . . ? C50 C51 C52 121.8(11) . . ? C50 C51 H51A 119.1 . . ? C52 C51 H51A 119.1 . . ? C51 C52 C47 116.9(11) . . ? C51 C52 C56 120.9(10) . . ? C47 C52 C56 122.2(9) . . ? C48 C53 C54 110.0(8) . . ? C48 C53 C55 112.5(9) . . ? C54 C53 C55 108.1(9) . . ? C48 C53 H53A 108.7 . . ? C54 C53 H53A 108.7 . . ? C55 C53 H53A 108.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C52 C56 C58 110.9(10) . . ? C52 C56 C57 113.3(9) . . ? C58 C56 C57 110.8(10) . . ? C52 C56 H56A 107.2 . . ? C58 C56 H56A 107.2 . . ? C57 C56 H56A 107.2 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 O1 102.0(9) . . ? C60 C59 H59A 111.4 . . ? O1 C59 H59A 111.4 . . ? C60 C59 H59B 111.4 . . ? O1 C59 H59B 111.4 . . ? H59A C59 H59B 109.2 . . ? C59 C60 C61 108.0(11) . . ? C59 C60 H60A 110.1 . . ? C61 C60 H60A 110.1 . . ? C59 C60 H60B 110.1 . . ? C61 C60 H60B 110.1 . . ? H60A C60 H60B 108.4 . . ? C60 C61 C62 102.2(9) . . ? C60 C61 H61A 111.3 . . ? C62 C61 H61A 111.3 . . ? C60 C61 H61B 111.3 . . ? C62 C61 H61B 111.3 . . ? H61A C61 H61B 109.2 . . ? O1 C62 C61 103.9(8) . . ? O1 C62 H62A 111.0 . . ? C61 C62 H62A 111.0 . . ? O1 C62 H62B 111.0 . . ? C61 C62 H62B 111.0 . . ? H62A C62 H62B 109.0 . . ? C102 C101 H10B 109.5 . . ? C102 C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C102 C101 H10D 109.5 . . ? H10B C101 H10D 109.5 . . ? H10C C101 H10D 109.5 . . ? N101 C102 C103 126.8(9) . . ? N101 C102 C101 120.3(9) . . ? C103 C102 C101 112.8(9) . . ? C104 C103 C102 126.0(9) . . ? C104 C103 H10E 117.0 . . ? C102 C103 H10E 117.0 . . ? N102 C104 C103 124.2(8) . . ? N102 C104 C105 120.8(9) . . ? C103 C104 C105 115.0(9) . . ? C104 C105 H10F 109.5 . . ? C104 C105 H10G 109.5 . . ? H10F C105 H10G 109.5 . . ? C104 C105 H10H 109.5 . . ? H10F C105 H10H 109.5 . . ? H10G C105 H10H 109.5 . . ? C111 C106 C107 121.4(9) . . ? C111 C106 N102 120.6(8) . . ? C107 C106 N102 117.8(8) . . ? C108 C107 C106 115.6(10) . . ? C108 C107 C115 124.4(10) . . ? C106 C107 C115 119.7(9) . . ? C107 C108 C109 122.6(12) . . ? C107 C108 H10I 118.7 . . ? C109 C108 H10I 118.7 . . ? C110 C109 C108 120.8(11) . . ? C110 C109 H10J 119.6 . . ? C108 C109 H10J 119.6 . . ? C109 C110 C111 121.0(11) . . ? C109 C110 H11A 119.5 . . ? C111 C110 H11A 119.5 . . ? C110 C111 C106 118.6(10) . . ? C110 C111 C112 118.2(10) . . ? C106 C111 C112 123.2(9) . . ? C113 C112 C111 113.6(9) . . ? C113 C112 C114 108.5(8) . . ? C111 C112 C114 110.4(9) . . ? C113 C112 H11B 108.0 . . ? C111 C112 H11B 108.0 . . ? C114 C112 H11B 108.0 . . ? C112 C113 H11C 109.5 . . ? C112 C113 H11D 109.5 . . ? H11C C113 H11D 109.5 . . ? C112 C113 H11E 109.5 . . ? H11C C113 H11E 109.5 . . ? H11D C113 H11E 109.5 . . ? C112 C114 H11F 109.5 . . ? C112 C114 H11G 109.5 . . ? H11F C114 H11G 109.5 . . ? C112 C114 H11H 109.5 . . ? H11F C114 H11H 109.5 . . ? H11G C114 H11H 109.5 . . ? C107 C115 C116 112.0(9) . . ? C107 C115 C117 111.0(9) . . ? C116 C115 C117 107.4(9) . . ? C107 C115 H11I 108.8 . . ? C116 C115 H11I 108.8 . . ? C117 C115 H11I 108.8 . . ? C115 C116 H11J 109.5 . . ? C115 C116 H11K 109.5 . . ? H11J C116 H11K 109.5 . . ? C115 C116 H11L 109.5 . . ? H11J C116 H11L 109.5 . . ? H11K C116 H11L 109.5 . . ? C115 C117 H11M 109.5 . . ? C115 C117 H11N 109.5 . . ? H11M C117 H11N 109.5 . . ? C115 C117 H11O 109.5 . . ? H11M C117 H11O 109.5 . . ? H11N C117 H11O 109.5 . . ? C119 C118 C123 120.4(9) . . ? C119 C118 N101 120.3(9) . . ? C123 C118 N101 119.4(9) . . ? C120 C119 C118 118.8(10) . . ? C120 C119 C124 118.4(10) . . ? C118 C119 C124 122.7(9) . . ? C119 C120 C121 121.2(12) . . ? C119 C120 H12B 119.4 . . ? C121 C120 H12B 119.4 . . ? C122 C121 C120 118.7(11) . . ? C122 C121 H12C 120.7 . . ? C120 C121 H12C 120.7 . . ? C123 C122 C121 122.1(12) . . ? C123 C122 H12D 119.0 . . ? C121 C122 H12D 119.0 . . ? C122 C123 C118 118.9(11) . . ? C122 C123 C127 118.4(10) . . ? C118 C123 C127 122.7(9) . . ? C119 C124 C126 112.8(9) . . ? C119 C124 C125 114.2(9) . . ? C126 C124 C125 109.2(9) . . ? C119 C124 H12E 106.7 . . ? C126 C124 H12E 106.7 . . ? C125 C124 H12E 106.7 . . ? C124 C125 H12F 109.5 . . ? C124 C125 H12G 109.5 . . ? H12F C125 H12G 109.5 . . ? C124 C125 H12H 109.5 . . ? H12F C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? C124 C126 H12I 109.5 . . ? C124 C126 H12J 109.5 . . ? H12I C126 H12J 109.5 . . ? C124 C126 H12K 109.5 . . ? H12I C126 H12K 109.5 . . ? H12J C126 H12K 109.5 . . ? C129 C127 C123 112.8(9) . . ? C129 C127 C128 108.5(10) . . ? C123 C127 C128 111.5(10) . . ? C129 C127 H12L 108.0 . . ? C123 C127 H12L 108.0 . . ? C128 C127 H12L 108.0 . . ? C127 C128 H12M 109.5 . . ? C127 C128 H12N 109.5 . . ? H12M C128 H12N 109.5 . . ? C127 C128 H12O 109.5 . . ? H12M C128 H12O 109.5 . . ? H12N C128 H12O 109.5 . . ? C127 C129 H12P 109.5 . . ? C127 C129 H12Q 109.5 . . ? H12P C129 H12Q 109.5 . . ? C127 C129 H12R 109.5 . . ? H12P C129 H12R 109.5 . . ? H12Q C129 H12R 109.5 . . ? C131 C130 H13D 109.5 . . ? C131 C130 H13E 109.5 . . ? H13D C130 H13E 109.5 . . ? C131 C130 H13F 109.5 . . ? H13D C130 H13F 109.5 . . ? H13E C130 H13F 109.5 . . ? N103 C131 C132 123.0(9) . . ? N103 C131 C130 120.8(10) . . ? C132 C131 C130 116.2(9) . . ? C133 C132 C131 132.8(9) . . ? C133 C132 H13G 113.6 . . ? C131 C132 H13G 113.6 . . ? N104 C133 C132 121.3(9) . . ? N104 C133 C134 120.3(10) . . ? C132 C133 C134 118.3(9) . . ? C133 C134 H13H 109.5 . . ? C133 C134 H13I 109.5 . . ? H13H C134 H13I 109.5 . . ? C133 C134 H13J 109.5 . . ? H13H C134 H13J 109.5 . . ? H13I C134 H13J 109.5 . . ? C136 C135 C140 121.8(10) . . ? C136 C135 N104 120.6(9) . . ? C140 C135 N104 117.6(9) . . ? C135 C136 C137 117.9(10) . . ? C135 C136 C141 122.7(10) . . ? C137 C136 C141 119.4(10) . . ? C138 C137 C136 122.2(11) . . ? C138 C137 H13K 118.9 . . ? C136 C137 H13K 118.9 . . ? C139 C138 C137 118.0(11) . . ? C139 C138 H13L 121.0 . . ? C137 C138 H13L 121.0 . . ? C138 C139 C140 122.7(11) . . ? C138 C139 H13M 118.7 . . ? C140 C139 H13M 118.7 . . ? C135 C140 C139 117.4(10) . . ? C135 C140 C144 123.4(9) . . ? C139 C140 C144 119.3(10) . . ? C142 C141 C143 110.8(11) . . ? C142 C141 C136 113.3(10) . . ? C143 C141 C136 112.6(10) . . ? C142 C141 H14D 106.5 . . ? C143 C141 H14D 106.5 . . ? C136 C141 H14D 106.5 . . ? C141 C142 H42D 109.5 . . ? C141 C142 H42E 109.5 . . ? H42D C142 H42E 109.5 . . ? C141 C142 H42F 109.5 . . ? H42D C142 H42F 109.5 . . ? H42E C142 H42F 109.5 . . ? C141 C143 H14E 109.5 . . ? C141 C143 H14F 109.5 . . ? H14E C143 H14F 109.5 . . ? C141 C143 H14G 109.5 . . ? H14E C143 H14G 109.5 . . ? H14F C143 H14G 109.5 . . ? C140 C144 C145 112.6(9) . . ? C140 C144 C146 112.9(10) . . ? C145 C144 C146 109.1(9) . . ? C140 C144 H14H 107.3 . . ? C145 C144 H14H 107.3 . . ? C146 C144 H14H 107.3 . . ? C144 C145 H14I 109.5 . . ? C144 C145 H14J 109.5 . . ? H14I C145 H14J 109.5 . . ? C144 C145 H14K 109.5 . . ? H14I C145 H14K 109.5 . . ? H14J C145 H14K 109.5 . . ? C144 C146 H14L 109.5 . . ? C144 C146 H14M 109.5 . . ? H14L C146 H14M 109.5 . . ? C144 C146 H14N 109.5 . . ? H14L C146 H14N 109.5 . . ? H14M C146 H14N 109.5 . . ? C152 C147 C148 122.4(10) . . ? C152 C147 N103 118.3(9) . . ? C148 C147 N103 119.3(10) . . ? C149 C148 C147 116.3(11) . . ? C149 C148 C153 119.9(11) . . ? C147 C148 C153 123.6(10) . . ? C150 C149 C148 121.8(12) . . ? C150 C149 H14O 119.1 . . ? C148 C149 H14O 119.1 . . ? C149 C150 C151 119.6(12) . . ? C149 C150 H15B 120.2 . . ? C151 C150 H15B 120.2 . . ? C152 C151 C150 121.6(12) . . ? C152 C151 H15C 119.2 . . ? C150 C151 H15C 119.2 . . ? C151 C152 C147 118.3(11) . . ? C151 C152 C156 119.7(11) . . ? C147 C152 C156 122.0(9) . . ? C148 C153 C154 113.3(9) . . ? C148 C153 C155 110.2(9) . . ? C154 C153 C155 109.5(9) . . ? C148 C153 H15D 107.9 . . ? C154 C153 H15D 107.9 . . ? C155 C153 H15D 107.9 . . ? C153 C154 H15E 109.5 . . ? C153 C154 H15F 109.5 . . ? H15E C154 H15F 109.5 . . ? C153 C154 H15G 109.5 . . ? H15E C154 H15G 109.5 . . ? H15F C154 H15G 109.5 . . ? C153 C155 H15H 109.5 . . ? C153 C155 H15I 109.5 . . ? H15H C155 H15I 109.5 . . ? C153 C155 H15J 109.5 . . ? H15H C155 H15J 109.5 . . ? H15I C155 H15J 109.5 . . ? C157 C156 C152 115.2(10) . . ? C157 C156 C158 109.5(10) . . ? C152 C156 C158 110.9(9) . . ? C157 C156 H15K 106.9 . . ? C152 C156 H15K 106.9 . . ? C158 C156 H15K 106.9 . . ? C156 C157 H15L 109.5 . . ? C156 C157 H15M 109.5 . . ? H15L C157 H15M 109.5 . . ? C156 C157 H15N 109.5 . . ? H15L C157 H15N 109.5 . . ? H15M C157 H15N 109.5 . . ? C156 C158 H15O 109.5 . . ? C156 C158 H15P 109.5 . . ? H15O C158 H15P 109.5 . . ? C156 C158 H15Q 109.5 . . ? H15O C158 H15Q 109.5 . . ? H15P C158 H15Q 109.5 . . ? C160 C159 O101 111.4(10) . . ? C160 C159 H15R 124.3 . . ? O101 C159 H15R 124.3 . . ? C159 C160 C161 106.2(12) . . ? C159 C160 H16D 126.9 . . ? C161 C160 H16D 126.9 . . ? C160 C161 C162 105.7(10) . . ? C160 C161 H16E 110.6 . . ? C162 C161 H16E 110.6 . . ? C160 C161 H16F 110.6 . . ? C162 C161 H16F 110.6 . . ? H16E C161 H16F 108.7 . . ? O101 C162 C161 105.2(8) . . ? O101 C162 H16G 110.7 . . ? C161 C162 H16G 110.7 . . ? O101 C162 H16H 110.7 . . ? C161 C162 H16H 110.7 . . ? H16G C162 H16H 108.8 . . ? C207 C201 C202 118.2(17) . . ? C207 C201 C206 124.8(17) . . ? C202 C201 C206 117.0(15) . . ? C203 C202 C201 119.9(16) . . ? C203 C202 H20B 120.0 . . ? C201 C202 H20B 120.0 . . ? C202 C203 C204 129.4(17) . . ? C202 C203 H20C 115.3 . . ? C204 C203 H20C 115.3 . . ? C203 C204 C205 106.3(15) . . ? C203 C204 H20D 110.5 . . ? C205 C204 H20D 110.5 . . ? C203 C204 H20E 110.5 . . ? C205 C204 H20E 110.5 . . ? H20D C204 H20E 108.7 . . ? C206 C205 C204 127.2(17) . . ? C206 C205 H20F 116.4 . . ? C204 C205 H20F 116.4 . . ? C205 C206 C201 119.8(16) . . ? C205 C206 H20G 120.1 . . ? C201 C206 H20G 120.1 . . ? C201 C207 H20H 109.5 . . ? C201 C207 H20I 109.5 . . ? H20H C207 H20I 109.5 . . ? C201 C207 H20J 109.5 . . ? H20H C207 H20J 109.5 . . ? H20I C207 H20J 109.5 . . ? C302 C301 C307 128(2) . . ? C302 C301 C306 118(2) . . ? C307 C301 C306 114(2) . . ? C301 C302 C303 129(2) . . ? C301 C302 H302 115.7 . . ? C303 C302 H302 115.7 . . ? C304 C303 C302 118(2) . . ? C304 C303 H30D 121.2 . . ? C302 C303 H30D 121.2 . . ? C303 C304 C305 121(2) . . ? C303 C304 H30E 119.7 . . ? C305 C304 H30E 119.7 . . ? C306 C305 C304 115(2) . . ? C306 C305 H30F 122.3 . . ? C304 C305 H30F 122.3 . . ? C305 C306 C301 120(2) . . ? C305 C306 H30G 120.1 . . ? C301 C306 H30G 120.1 . . ? C301 C307 H30H 109.5 . . ? C301 C307 H30I 109.5 . . ? H30H C307 H30I 109.5 . . ? C301 C307 H30J 109.5 . . ? H30H C307 H30J 109.5 . . ? H30I C307 H30J 109.5 . . ? C406 C401 C402 121.5(16) . . ? C406 C401 C407 126.1(14) . . ? C402 C401 C407 112.4(15) . . ? C401 C402 C403 115.0(18) . . ? C401 C402 H40A 122.5 . . ? C403 C402 H40A 122.5 . . ? C404 C403 C402 123.6(19) . . ? C404 C403 H40B 118.2 . . ? C402 C403 H40B 118.2 . . ? C405 C404 C403 117.6(17) . . ? C405 C404 H40C 121.2 . . ? C403 C404 H40C 121.2 . . ? C404 C405 C406 121.3(16) . . ? C404 C405 H40D 119.3 . . ? C406 C405 H40D 119.3 . . ? C401 C406 C405 120.7(14) . . ? C401 C406 H40E 119.6 . . ? C405 C406 H40E 119.6 . . ? C401 C407 H40F 109.5 . . ? C401 C407 H40G 109.5 . . ? H40F C407 H40G 109.5 . . ? C401 C407 H40H 109.5 . . ? H40F C407 H40H 109.5 . . ? H40G C407 H40H 109.5 . . ? C502 C501 C506 120.0 . . ? C502 C501 C507 120.0(6) . . ? C506 C501 C507 117.8(6) . . ? C501 C502 C503 120.0 . . ? C504 C503 C502 120.0 . . ? C505 C504 C503 120.0 . . ? C505 C504 C57A 118.5(6) . . ? C503 C504 C57A 121.4(6) . . ? C504 C505 C506 120.0 . . ? C505 C506 C501 120.0 . . ? C602 C601 C606 120.0 . . ? C602 C601 C601 167.7(13) . 3_666 ? C606 C601 C601 70.8(11) . 3_666 ? C602 C601 C606 123.1(17) . 3_666 ? C606 C601 C606 116.5(16) . 3_666 ? C601 C601 C606 45.8(9) 3_666 3_666 ? C603 C602 C601 120.0 . . ? C604 C603 C602 120.0 . . ? C603 C604 C605 120.0 . . ? C606 C605 C604 120.0 . . ? C605 C606 C601 120.0 . . ? C605 C606 C601 173.2(7) . 3_666 ? C601 C606 C601 63.5(11) . 3_666 ? C705 C701 C702 128.8 . . ? C705 C701 C704 64.4(10) . 3_565 ? C702 C701 C704 71.6(13) . 3_565 ? C701 C702 C703 114.5 . . ? C701 C702 C704 63.0(14) . 3_565 ? C703 C702 C704 53.4(13) . 3_565 ? C704 C703 C704 40.5(13) . 3_565 ? C704 C703 C702 107.3 . . ? C704 C703 C702 67.1(13) 3_565 . ? C704 C703 C705 61.6(14) . 3_565 ? C704 C703 C705 101.8(19) 3_565 3_565 ? C702 C703 C705 168.8(15) . 3_565 ? C704 C704 C703 80.2(18) 3_565 . ? C704 C704 C703 59(2) 3_565 3_565 ? C703 C704 C703 139.5(14) . 3_565 ? C704 C704 C705 151(2) 3_565 3_565 ? C703 C704 C705 71.2(14) . 3_565 ? C703 C704 C705 149(3) 3_565 3_565 ? C704 C704 C701 162(3) 3_565 3_565 ? C703 C704 C701 116.9(18) . 3_565 ? C703 C704 C701 103.4(17) 3_565 3_565 ? C705 C704 C701 47.2(11) 3_565 3_565 ? C704 C704 C702 118(3) 3_565 3_565 ? C703 C704 C702 160.2(16) . 3_565 ? C703 C704 C702 59.5(13) 3_565 3_565 ? C705 C704 C702 89.4(18) 3_565 3_565 ? C701 C704 C702 45.4(9) 3_565 3_565 ? C701 C705 C704 68.4(10) . 3_565 ? C701 C705 C703 114.1(10) . 3_565 ? C704 C705 C703 47.2(12) 3_565 3_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Sm1 Sm2 N3 -161.5(3) . . . . ? N1 Sm1 Sm2 N3 -30.8(4) . . . . ? O1 Sm1 Sm2 N3 87.5(3) . . . . ? Cl2 Sm1 Sm2 N3 -88.3(2) . . . . ? Cl3 Sm1 Sm2 N3 30.4(2) . . . . ? Cl1 Sm1 Sm2 N3 150.2(2) . . . . ? N2 Sm1 Sm2 N4 -58.1(4) . . . . ? N1 Sm1 Sm2 N4 72.6(4) . . . . ? O1 Sm1 Sm2 N4 -169.1(3) . . . . ? Cl2 Sm1 Sm2 N4 15.1(3) . . . . ? Cl3 Sm1 Sm2 N4 133.8(3) . . . . ? Cl1 Sm1 Sm2 N4 -106.4(3) . . . . ? N2 Sm1 Sm2 Cl4 74.0(3) . . . . ? N1 Sm1 Sm2 Cl4 -155.3(3) . . . . ? O1 Sm1 Sm2 Cl4 -37.06(18) . . . . ? Cl2 Sm1 Sm2 Cl4 147.17(12) . . . . ? Cl3 Sm1 Sm2 Cl4 -94.12(12) . . . . ? Cl1 Sm1 Sm2 Cl4 25.65(12) . . . . ? N2 Sm1 Sm2 Cl1 48.3(3) . . . . ? N1 Sm1 Sm2 Cl1 179.0(3) . . . . ? O1 Sm1 Sm2 Cl1 -62.72(19) . . . . ? Cl2 Sm1 Sm2 Cl1 121.52(13) . . . . ? Cl3 Sm1 Sm2 Cl1 -119.77(13) . . . . ? N2 Sm1 Sm2 Cl3 168.1(3) . . . . ? N1 Sm1 Sm2 Cl3 -61.2(3) . . . . ? O1 Sm1 Sm2 Cl3 57.05(19) . . . . ? Cl2 Sm1 Sm2 Cl3 -118.71(13) . . . . ? Cl1 Sm1 Sm2 Cl3 119.77(13) . . . . ? N2 Sm1 Sm2 Cl2 -73.2(3) . . . . ? N1 Sm1 Sm2 Cl2 57.5(3) . . . . ? O1 Sm1 Sm2 Cl2 175.77(19) . . . . ? Cl3 Sm1 Sm2 Cl2 118.71(13) . . . . ? Cl1 Sm1 Sm2 Cl2 -121.52(13) . . . . ? N102 Sm11 Sm12 N103 -165.0(3) . . . . ? N101 Sm11 Sm12 N103 -31.2(4) . . . . ? O101 Sm11 Sm12 N103 84.8(3) . . . . ? Cl13 Sm11 Sm12 N103 -92.6(2) . . . . ? Cl11 Sm11 Sm12 N103 25.8(3) . . . . ? Cl12 Sm11 Sm12 N103 145.7(2) . . . . ? N102 Sm11 Sm12 N104 -62.2(4) . . . . ? N101 Sm11 Sm12 N104 71.6(4) . . . . ? O101 Sm11 Sm12 N104 -172.4(3) . . . . ? Cl13 Sm11 Sm12 N104 10.3(3) . . . . ? Cl11 Sm11 Sm12 N104 128.7(3) . . . . ? Cl12 Sm11 Sm12 N104 -111.4(2) . . . . ? N102 Sm11 Sm12 Cl14 69.3(3) . . . . ? N101 Sm11 Sm12 Cl14 -156.9(3) . . . . ? O101 Sm11 Sm12 Cl14 -40.89(18) . . . . ? Cl13 Sm11 Sm12 Cl14 141.72(12) . . . . ? Cl11 Sm11 Sm12 Cl14 -99.85(12) . . . . ? Cl12 Sm11 Sm12 Cl14 20.09(11) . . . . ? N102 Sm11 Sm12 Cl11 169.1(3) . . . . ? N101 Sm11 Sm12 Cl11 -57.0(3) . . . . ? O101 Sm11 Sm12 Cl11 58.96(18) . . . . ? Cl13 Sm11 Sm12 Cl11 -118.43(13) . . . . ? Cl12 Sm11 Sm12 Cl11 119.94(13) . . . . ? N102 Sm11 Sm12 Cl12 49.2(3) . . . . ? N101 Sm11 Sm12 Cl12 -177.0(3) . . . . ? O101 Sm11 Sm12 Cl12 -60.98(18) . . . . ? Cl13 Sm11 Sm12 Cl12 121.63(12) . . . . ? Cl11 Sm11 Sm12 Cl12 -119.94(13) . . . . ? N102 Sm11 Sm12 Cl13 -72.4(3) . . . . ? N101 Sm11 Sm12 Cl13 61.4(3) . . . . ? O101 Sm11 Sm12 Cl13 177.39(18) . . . . ? Cl11 Sm11 Sm12 Cl13 118.43(13) . . . . ? Cl12 Sm11 Sm12 Cl13 -121.63(12) . . . . ? N2 Sm1 Cl1 Sm2 -147.4(2) . . . . ? N1 Sm1 Cl1 Sm2 -173(2) . . . . ? O1 Sm1 Cl1 Sm2 123.72(16) . . . . ? Cl2 Sm1 Cl1 Sm2 -39.10(8) . . . . ? Cl3 Sm1 Cl1 Sm2 39.83(8) . . . . ? N3 Sm2 Cl1 Sm1 -76.9(4) . . . . ? N4 Sm2 Cl1 Sm1 108.1(3) . . . . ? Cl4 Sm2 Cl1 Sm1 -159.72(9) . . . . ? Cl3 Sm2 Cl1 Sm1 -39.05(8) . . . . ? Cl2 Sm2 Cl1 Sm1 37.69(8) . . . . ? N2 Sm1 Cl2 Sm2 133.6(2) . . . . ? N1 Sm1 Cl2 Sm2 -145.1(2) . . . . ? O1 Sm1 Cl2 Sm2 -10.1(4) . . . . ? Cl3 Sm1 Cl2 Sm2 -40.34(8) . . . . ? Cl1 Sm1 Cl2 Sm2 38.66(8) . . . . ? N3 Sm2 Cl2 Sm1 117.10(19) . . . . ? N4 Sm2 Cl2 Sm1 -167.8(2) . . . . ? Cl4 Sm2 Cl2 Sm1 -81.5(2) . . . . ? Cl1 Sm2 Cl2 Sm1 -38.49(8) . . . . ? Cl3 Sm2 Cl2 Sm1 39.82(8) . . . . ? N2 Sm1 Cl3 Sm2 -97.1(13) . . . . ? N1 Sm1 Cl3 Sm2 143.1(2) . . . . ? O1 Sm1 Cl3 Sm2 -127.87(16) . . . . ? Cl2 Sm1 Cl3 Sm2 40.68(8) . . . . ? Cl1 Sm1 Cl3 Sm2 -39.71(8) . . . . ? N3 Sm2 Cl3 Sm1 -155.48(19) . . . . ? N4 Sm2 Cl3 Sm1 -91.3(4) . . . . ? Cl4 Sm2 Cl3 Sm1 115.62(9) . . . . ? Cl1 Sm2 Cl3 Sm1 39.39(8) . . . . ? Cl2 Sm2 Cl3 Sm1 -39.33(8) . . . . ? N102 Sm11 Cl11 Sm12 -107.6(13) . . . . ? N101 Sm11 Cl11 Sm12 145.7(2) . . . . ? O101 Sm11 Cl11 Sm12 -125.43(16) . . . . ? Cl13 Sm11 Cl11 Sm12 40.63(8) . . . . ? Cl12 Sm11 Cl11 Sm12 -39.69(8) . . . . ? N103 Sm12 Cl11 Sm11 -159.3(2) . . . . ? N104 Sm12 Cl11 Sm11 -96.0(3) . . . . ? Cl14 Sm12 Cl11 Sm11 112.87(10) . . . . ? Cl12 Sm12 Cl11 Sm11 39.21(8) . . . . ? Cl13 Sm12 Cl11 Sm11 -39.37(8) . . . . ? N102 Sm11 Cl12 Sm12 -147.82(19) . . . . ? N101 Sm11 Cl12 Sm12 161.4(18) . . . . ? O101 Sm11 Cl12 Sm12 123.92(16) . . . . ? Cl13 Sm11 Cl12 Sm12 -38.79(8) . . . . ? Cl11 Sm11 Cl12 Sm12 39.58(8) . . . . ? N103 Sm12 Cl12 Sm11 -82.2(5) . . . . ? N104 Sm12 Cl12 Sm11 106.4(2) . . . . ? Cl14 Sm12 Cl12 Sm11 -164.14(9) . . . . ? Cl11 Sm12 Cl12 Sm11 -38.89(8) . . . . ? Cl13 Sm12 Cl12 Sm11 37.52(8) . . . . ? N102 Sm11 Cl13 Sm12 135.18(19) . . . . ? N101 Sm11 Cl13 Sm12 -143.5(2) . . . . ? O101 Sm11 Cl13 Sm12 -5.9(4) . . . . ? Cl11 Sm11 Cl13 Sm12 -40.41(8) . . . . ? Cl12 Sm11 Cl13 Sm12 38.69(8) . . . . ? N103 Sm12 Cl13 Sm11 115.1(2) . . . . ? N104 Sm12 Cl13 Sm11 -171.8(2) . . . . ? Cl14 Sm12 Cl13 Sm11 -86.71(18) . . . . ? Cl11 Sm12 Cl13 Sm11 39.92(8) . . . . ? Cl12 Sm12 Cl13 Sm11 -38.35(8) . . . . ? N2 Sm1 O1 C62 44.2(7) . . . . ? N1 Sm1 O1 C62 -32.7(7) . . . . ? Cl2 Sm1 O1 C62 -169.7(6) . . . . ? Cl3 Sm1 O1 C62 -140.1(7) . . . . ? Cl1 Sm1 O1 C62 142.9(7) . . . . ? Sm2 Sm1 O1 C62 -177.5(7) . . . . ? N2 Sm1 O1 C59 -144.3(8) . . . . ? N1 Sm1 O1 C59 138.9(8) . . . . ? Cl2 Sm1 O1 C59 1.9(10) . . . . ? Cl3 Sm1 O1 C59 31.4(8) . . . . ? Cl1 Sm1 O1 C59 -45.6(8) . . . . ? Sm2 Sm1 O1 C59 -6.0(8) . . . . ? N102 Sm11 O101 C159 -146.1(9) . . . . ? N101 Sm11 O101 C159 138.0(9) . . . . ? Cl13 Sm11 O101 C159 -2.2(11) . . . . ? Cl11 Sm11 O101 C159 31.5(8) . . . . ? Cl12 Sm11 O101 C159 -45.7(8) . . . . ? Sm12 Sm11 O101 C159 -6.6(9) . . . . ? N102 Sm11 O101 C162 42.0(7) . . . . ? N101 Sm11 O101 C162 -33.9(7) . . . . ? Cl13 Sm11 O101 C162 -174.0(5) . . . . ? Cl11 Sm11 O101 C162 -140.4(7) . . . . ? Cl12 Sm11 O101 C162 142.4(6) . . . . ? Sm12 Sm11 O101 C162 -178.5(6) . . . . ? N2 Sm1 N1 C2 -23.3(8) . . . . ? O1 Sm1 N1 C2 65.8(8) . . . . ? Cl2 Sm1 N1 C2 -130.3(7) . . . . ? Cl3 Sm1 N1 C2 149.1(7) . . . . ? Cl1 Sm1 N1 C2 2(3) . . . . ? Sm2 Sm1 N1 C2 -169.6(6) . . . . ? N2 Sm1 N1 C18 156.6(7) . . . . ? O1 Sm1 N1 C18 -114.2(6) . . . . ? Cl2 Sm1 N1 C18 49.6(6) . . . . ? Cl3 Sm1 N1 C18 -30.9(6) . . . . ? Cl1 Sm1 N1 C18 -178(34) . . . . ? Sm2 Sm1 N1 C18 10.3(8) . . . . ? N1 Sm1 N2 C4 25.2(8) . . . . ? O1 Sm1 N2 C4 -66.1(8) . . . . ? Cl2 Sm1 N2 C4 127.3(7) . . . . ? Cl3 Sm1 N2 C4 -96.6(15) . . . . ? Cl1 Sm1 N2 C4 -152.6(8) . . . . ? Sm2 Sm1 N2 C4 174.6(6) . . . . ? N1 Sm1 N2 C6 -158.8(7) . . . . ? O1 Sm1 N2 C6 110.0(6) . . . . ? Cl2 Sm1 N2 C6 -56.6(6) . . . . ? Cl3 Sm1 N2 C6 79.4(15) . . . . ? Cl1 Sm1 N2 C6 23.4(6) . . . . ? Sm2 Sm1 N2 C6 -9.3(7) . . . . ? N4 Sm2 N3 C31 36.0(7) . . . . ? Cl4 Sm2 N3 C31 -58.3(7) . . . . ? Cl1 Sm2 N3 C31 -139.8(6) . . . . ? Cl3 Sm2 N3 C31 -176.3(7) . . . . ? Cl2 Sm2 N3 C31 113.7(7) . . . . ? Sm1 Sm2 N3 C31 162.8(6) . . . . ? N4 Sm2 N3 C47 -154.0(7) . . . . ? Cl4 Sm2 N3 C47 111.7(7) . . . . ? Cl1 Sm2 N3 C47 30.2(9) . . . . ? Cl3 Sm2 N3 C47 -6.3(6) . . . . ? Cl2 Sm2 N3 C47 -76.3(7) . . . . ? Sm1 Sm2 N3 C47 -27.2(7) . . . . ? N3 Sm2 N4 C33 -39.5(7) . . . . ? Cl4 Sm2 N4 C33 50.9(7) . . . . ? Cl1 Sm2 N4 C33 138.4(7) . . . . ? Cl3 Sm2 N4 C33 -105.4(7) . . . . ? Cl2 Sm2 N4 C33 -155.1(7) . . . . ? Sm1 Sm2 N4 C33 -165.5(6) . . . . ? N3 Sm2 N4 C35 151.1(8) . . . . ? Cl4 Sm2 N4 C35 -118.5(8) . . . . ? Cl1 Sm2 N4 C35 -31.0(8) . . . . ? Cl3 Sm2 N4 C35 85.2(8) . . . . ? Cl2 Sm2 N4 C35 35.6(7) . . . . ? Sm1 Sm2 N4 C35 25.1(8) . . . . ? N102 Sm11 N101 C102 -19.0(8) . . . . ? O101 Sm11 N101 C102 70.1(8) . . . . ? Cl13 Sm11 N101 C102 -126.4(8) . . . . ? Cl11 Sm11 N101 C102 153.2(8) . . . . ? Cl12 Sm11 N101 C102 33(2) . . . . ? Sm12 Sm11 N101 C102 -168.0(7) . . . . ? N102 Sm11 N101 C118 156.5(7) . . . . ? O101 Sm11 N101 C118 -114.5(6) . . . . ? Cl13 Sm11 N101 C118 49.0(7) . . . . ? Cl11 Sm11 N101 C118 -31.3(7) . . . . ? Cl12 Sm11 N101 C118 -151.7(16) . . . . ? Sm12 Sm11 N101 C118 7.5(8) . . . . ? N101 Sm11 N102 C104 21.5(8) . . . . ? O101 Sm11 N102 C104 -69.5(8) . . . . ? Cl13 Sm11 N102 C104 125.9(8) . . . . ? Cl11 Sm11 N102 C104 -87.2(16) . . . . ? Cl12 Sm11 N102 C104 -153.6(8) . . . . ? Sm12 Sm11 N102 C104 172.9(7) . . . . ? N101 Sm11 N102 C106 -159.7(6) . . . . ? O101 Sm11 N102 C106 109.3(6) . . . . ? Cl13 Sm11 N102 C106 -55.3(6) . . . . ? Cl11 Sm11 N102 C106 91.7(14) . . . . ? Cl12 Sm11 N102 C106 25.2(6) . . . . ? Sm12 Sm11 N102 C106 -8.3(7) . . . . ? N104 Sm12 N103 C131 36.6(7) . . . . ? Cl14 Sm12 N103 C131 -56.2(7) . . . . ? Cl11 Sm12 N103 C131 -178.3(7) . . . . ? Cl12 Sm12 N103 C131 -136.6(6) . . . . ? Cl13 Sm12 N103 C131 113.3(7) . . . . ? Sm11 Sm12 N103 C131 163.9(6) . . . . ? N104 Sm12 N103 C147 -154.7(8) . . . . ? Cl14 Sm12 N103 C147 112.6(7) . . . . ? Cl11 Sm12 N103 C147 -9.6(7) . . . . ? Cl12 Sm12 N103 C147 32.1(10) . . . . ? Cl13 Sm12 N103 C147 -78.0(7) . . . . ? Sm11 Sm12 N103 C147 -27.4(8) . . . . ? N103 Sm12 N104 C133 -40.9(8) . . . . ? Cl14 Sm12 N104 C133 49.4(7) . . . . ? Cl11 Sm12 N104 C133 -106.4(7) . . . . ? Cl12 Sm12 N104 C133 135.0(7) . . . . ? Cl13 Sm12 N104 C133 -160.0(8) . . . . ? Sm11 Sm12 N104 C133 -167.1(6) . . . . ? N103 Sm12 N104 C135 152.9(7) . . . . ? Cl14 Sm12 N104 C135 -116.8(7) . . . . ? Cl11 Sm12 N104 C135 87.4(7) . . . . ? Cl12 Sm12 N104 C135 -31.2(8) . . . . ? Cl13 Sm12 N104 C135 33.8(6) . . . . ? Sm11 Sm12 N104 C135 26.7(7) . . . . ? C18 N1 C2 C3 -168.2(9) . . . . ? Sm1 N1 C2 C3 11.8(14) . . . . ? C18 N1 C2 C1 10.7(13) . . . . ? Sm1 N1 C2 C1 -169.4(7) . . . . ? N1 C2 C3 C4 13.7(18) . . . . ? C1 C2 C3 C4 -165.2(11) . . . . ? C6 N2 C4 C3 168.5(9) . . . . ? Sm1 N2 C4 C3 -15.7(14) . . . . ? C6 N2 C4 C5 -10.0(13) . . . . ? Sm1 N2 C4 C5 165.8(6) . . . . ? C2 C3 C4 N2 -11.9(18) . . . . ? C2 C3 C4 C5 166.6(11) . . . . ? C4 N2 C6 C7 -99.7(10) . . . . ? Sm1 N2 C6 C7 83.8(9) . . . . ? C4 N2 C6 C11 83.7(11) . . . . ? Sm1 N2 C6 C11 -92.8(9) . . . . ? C11 C6 C7 C8 0.5(15) . . . . ? N2 C6 C7 C8 -176.1(9) . . . . ? C11 C6 C7 C12 -177.9(9) . . . . ? N2 C6 C7 C12 5.5(14) . . . . ? C6 C7 C8 C9 0.4(17) . . . . ? C12 C7 C8 C9 178.8(11) . . . . ? C7 C8 C9 C10 -0.1(19) . . . . ? C8 C9 C10 C11 -1(2) . . . . ? C9 C10 C11 C6 1.8(17) . . . . ? C9 C10 C11 C15 -177.3(11) . . . . ? C7 C6 C11 C10 -1.5(15) . . . . ? N2 C6 C11 C10 174.9(9) . . . . ? C7 C6 C11 C15 177.5(9) . . . . ? N2 C6 C11 C15 -6.0(14) . . . . ? C6 C7 C12 C13 -154.2(10) . . . . ? C8 C7 C12 C13 27.4(14) . . . . ? C6 C7 C12 C14 80.2(12) . . . . ? C8 C7 C12 C14 -98.2(12) . . . . ? C10 C11 C15 C16 -64.0(13) . . . . ? C6 C11 C15 C16 117.0(11) . . . . ? C10 C11 C15 C17 58.1(13) . . . . ? C6 C11 C15 C17 -120.9(11) . . . . ? C2 N1 C18 C19 -103.2(11) . . . . ? Sm1 N1 C18 C19 76.8(9) . . . . ? C2 N1 C18 C23 78.2(11) . . . . ? Sm1 N1 C18 C23 -101.8(8) . . . . ? C23 C18 C19 C20 -1.2(15) . . . . ? N1 C18 C19 C20 -179.7(9) . . . . ? C23 C18 C19 C24 -177.5(9) . . . . ? N1 C18 C19 C24 4.0(14) . . . . ? C18 C19 C20 C21 0.6(16) . . . . ? C24 C19 C20 C21 176.9(10) . . . . ? C19 C20 C21 C22 0.4(17) . . . . ? C20 C21 C22 C23 -0.7(16) . . . . ? C21 C22 C23 C18 0.1(15) . . . . ? C21 C22 C23 C27 -177.2(9) . . . . ? C19 C18 C23 C22 0.8(14) . . . . ? N1 C18 C23 C22 179.4(9) . . . . ? C19 C18 C23 C27 178.0(9) . . . . ? N1 C18 C23 C27 -3.4(14) . . . . ? C20 C19 C24 C25 32.2(14) . . . . ? C18 C19 C24 C25 -151.5(9) . . . . ? C20 C19 C24 C26 -87.7(12) . . . . ? C18 C19 C24 C26 88.6(12) . . . . ? C22 C23 C27 C29 -58.6(12) . . . . ? C18 C23 C27 C29 124.2(10) . . . . ? C22 C23 C27 C28 61.1(13) . . . . ? C18 C23 C27 C28 -116.1(11) . . . . ? C47 N3 C31 C32 170.9(9) . . . . ? Sm2 N3 C31 C32 -18.9(12) . . . . ? C47 N3 C31 C30 -9.2(12) . . . . ? Sm2 N3 C31 C30 161.0(6) . . . . ? N3 C31 C32 C33 -15.4(17) . . . . ? C30 C31 C32 C33 164.6(10) . . . . ? C35 N4 C33 C32 -162.9(10) . . . . ? Sm2 N4 C33 C32 27.4(14) . . . . ? C35 N4 C33 C34 13.5(14) . . . . ? Sm2 N4 C33 C34 -156.1(8) . . . . ? C31 C32 C33 N4 10.2(18) . . . . ? C31 C32 C33 C34 -166.4(10) . . . . ? C33 N4 C35 C36 -101.6(11) . . . . ? Sm2 N4 C35 C36 68.1(11) . . . . ? C33 N4 C35 C40 80.8(12) . . . . ? Sm2 N4 C35 C40 -109.6(9) . . . . ? C40 C35 C36 C37 -2.3(16) . . . . ? N4 C35 C36 C37 -179.9(9) . . . . ? C40 C35 C36 C41 177.0(10) . . . . ? N4 C35 C36 C41 -0.6(16) . . . . ? C35 C36 C37 C38 1.3(17) . . . . ? C41 C36 C37 C38 -178.0(12) . . . . ? C36 C37 C38 C39 -2(2) . . . . ? C37 C38 C39 C40 3(2) . . . . ? C38 C39 C40 C35 -4.1(17) . . . . ? C38 C39 C40 C44 179.5(12) . . . . ? C36 C35 C40 C39 3.8(16) . . . . ? N4 C35 C40 C39 -178.6(9) . . . . ? C36 C35 C40 C44 -180.0(10) . . . . ? N4 C35 C40 C44 -2.4(16) . . . . ? C35 C36 C41 C42 101.3(16) . . . . ? C37 C36 C41 C42 -79.4(16) . . . . ? C35 C36 C41 C43 -133.3(12) . . . . ? C37 C36 C41 C43 46.1(16) . . . . ? C39 C40 C44 C46 -59.7(14) . . . . ? C35 C40 C44 C46 124.1(11) . . . . ? C39 C40 C44 C45 63.9(15) . . . . ? C35 C40 C44 C45 -112.3(12) . . . . ? C31 N3 C47 C48 88.4(11) . . . . ? Sm2 N3 C47 C48 -82.2(10) . . . . ? C31 N3 C47 C52 -97.2(10) . . . . ? Sm2 N3 C47 C52 92.2(9) . . . . ? C52 C47 C48 C49 1.3(15) . . . . ? N3 C47 C48 C49 175.4(9) . . . . ? C52 C47 C48 C53 -176.7(9) . . . . ? N3 C47 C48 C53 -2.7(14) . . . . ? C47 C48 C49 C50 -1.5(15) . . . . ? C53 C48 C49 C50 176.6(9) . . . . ? C48 C49 C50 C51 0.8(17) . . . . ? C49 C50 C51 C52 0.1(17) . . . . ? C50 C51 C52 C47 -0.2(16) . . . . ? C50 C51 C52 C56 -178.4(11) . . . . ? C48 C47 C52 C51 -0.6(15) . . . . ? N3 C47 C52 C51 -174.8(9) . . . . ? C48 C47 C52 C56 177.6(10) . . . . ? N3 C47 C52 C56 3.4(14) . . . . ? C49 C48 C53 C54 -66.9(12) . . . . ? C47 C48 C53 C54 111.0(11) . . . . ? C49 C48 C53 C55 53.6(12) . . . . ? C47 C48 C53 C55 -128.4(10) . . . . ? C51 C52 C56 C58 -89.2(12) . . . . ? C47 C52 C56 C58 92.7(12) . . . . ? C51 C52 C56 C57 36.2(15) . . . . ? C47 C52 C56 C57 -141.9(10) . . . . ? C62 O1 C59 C60 -8.9(13) . . . . ? Sm1 O1 C59 C60 178.5(8) . . . . ? O1 C59 C60 C61 28.6(15) . . . . ? C59 C60 C61 C62 -37.0(15) . . . . ? C59 O1 C62 C61 -13.1(12) . . . . ? Sm1 O1 C62 C61 159.2(7) . . . . ? C60 C61 C62 O1 29.5(13) . . . . ? C118 N101 C102 C103 -168.6(10) . . . . ? Sm11 N101 C102 C103 6.8(15) . . . . ? C118 N101 C102 C101 13.0(14) . . . . ? Sm11 N101 C102 C101 -171.7(7) . . . . ? N101 C102 C103 C104 17.1(17) . . . . ? C101 C102 C103 C104 -164.4(10) . . . . ? C106 N102 C104 C103 170.6(9) . . . . ? Sm11 N102 C104 C103 -10.7(15) . . . . ? C106 N102 C104 C105 -10.4(13) . . . . ? Sm11 N102 C104 C105 168.3(7) . . . . ? C102 C103 C104 N102 -15.1(17) . . . . ? C102 C103 C104 C105 165.8(10) . . . . ? C104 N102 C106 C111 84.1(12) . . . . ? Sm11 N102 C106 C111 -94.9(9) . . . . ? C104 N102 C106 C107 -101.5(10) . . . . ? Sm11 N102 C106 C107 79.5(9) . . . . ? C111 C106 C107 C108 -0.7(14) . . . . ? N102 C106 C107 C108 -175.1(9) . . . . ? C111 C106 C107 C115 -174.9(9) . . . . ? N102 C106 C107 C115 10.7(13) . . . . ? C106 C107 C108 C109 2.4(17) . . . . ? C115 C107 C108 C109 176.2(11) . . . . ? C107 C108 C109 C110 -1(2) . . . . ? C108 C109 C110 C111 -2(2) . . . . ? C109 C110 C111 C106 3.5(17) . . . . ? C109 C110 C111 C112 -178.2(11) . . . . ? C107 C106 C111 C110 -2.1(15) . . . . ? N102 C106 C111 C110 172.1(9) . . . . ? C107 C106 C111 C112 179.7(9) . . . . ? N102 C106 C111 C112 -6.1(15) . . . . ? C110 C111 C112 C113 -59.5(13) . . . . ? C106 C111 C112 C113 118.7(11) . . . . ? C110 C111 C112 C114 62.6(12) . . . . ? C106 C111 C112 C114 -119.1(10) . . . . ? C108 C107 C115 C116 -96.7(13) . . . . ? C106 C107 C115 C116 76.9(12) . . . . ? C108 C107 C115 C117 23.4(14) . . . . ? C106 C107 C115 C117 -163.0(9) . . . . ? C102 N101 C118 C119 -103.7(11) . . . . ? Sm11 N101 C118 C119 80.3(9) . . . . ? C102 N101 C118 C123 75.9(12) . . . . ? Sm11 N101 C118 C123 -100.2(9) . . . . ? C123 C118 C119 C120 -2.1(15) . . . . ? N101 C118 C119 C120 177.5(9) . . . . ? C123 C118 C119 C124 180.0(9) . . . . ? N101 C118 C119 C124 -0.5(14) . . . . ? C118 C119 C120 C121 1.2(16) . . . . ? C124 C119 C120 C121 179.2(10) . . . . ? C119 C120 C121 C122 0.5(18) . . . . ? C120 C121 C122 C123 -1.4(18) . . . . ? C121 C122 C123 C118 0.5(17) . . . . ? C121 C122 C123 C127 -178.7(10) . . . . ? C119 C118 C123 C122 1.2(15) . . . . ? N101 C118 C123 C122 -178.3(9) . . . . ? C119 C118 C123 C127 -179.5(9) . . . . ? N101 C118 C123 C127 0.9(15) . . . . ? C120 C119 C124 C126 -90.1(12) . . . . ? C118 C119 C124 C126 87.9(12) . . . . ? C120 C119 C124 C125 35.3(13) . . . . ? C118 C119 C124 C125 -146.7(10) . . . . ? C122 C123 C127 C129 -60.6(13) . . . . ? C118 C123 C127 C129 120.2(11) . . . . ? C122 C123 C127 C128 61.8(13) . . . . ? C118 C123 C127 C128 -117.5(12) . . . . ? C147 N103 C131 C132 171.0(10) . . . . ? Sm12 N103 C131 C132 -20.1(13) . . . . ? C147 N103 C131 C130 -9.7(14) . . . . ? Sm12 N103 C131 C130 159.2(7) . . . . ? N103 C131 C132 C133 -16.2(18) . . . . ? C130 C131 C132 C133 164.5(11) . . . . ? C135 N104 C133 C132 -165.8(9) . . . . ? Sm12 N104 C133 C132 27.8(13) . . . . ? C135 N104 C133 C134 13.8(14) . . . . ? Sm12 N104 C133 C134 -152.7(8) . . . . ? C131 C132 C133 N104 11.6(18) . . . . ? C131 C132 C133 C134 -167.9(11) . . . . ? C133 N104 C135 C136 -100.3(11) . . . . ? Sm12 N104 C135 C136 66.8(11) . . . . ? C133 N104 C135 C140 82.4(11) . . . . ? Sm12 N104 C135 C140 -110.5(9) . . . . ? C140 C135 C136 C137 -0.6(15) . . . . ? N104 C135 C136 C137 -177.8(9) . . . . ? C140 C135 C136 C141 -179.8(10) . . . . ? N104 C135 C136 C141 3.0(16) . . . . ? C135 C136 C137 C138 -1.3(16) . . . . ? C141 C136 C137 C138 178.0(10) . . . . ? C136 C137 C138 C139 3.1(15) . . . . ? C137 C138 C139 C140 -3.3(15) . . . . ? C136 C135 C140 C139 0.5(15) . . . . ? N104 C135 C140 C139 177.8(8) . . . . ? C136 C135 C140 C144 -179.6(10) . . . . ? N104 C135 C140 C144 -2.3(14) . . . . ? C138 C139 C140 C135 1.5(15) . . . . ? C138 C139 C140 C144 -178.4(9) . . . . ? C135 C136 C141 C142 -133.2(11) . . . . ? C137 C136 C141 C142 47.7(15) . . . . ? C135 C136 C141 C143 100.1(14) . . . . ? C137 C136 C141 C143 -79.1(14) . . . . ? C135 C140 C144 C145 -112.1(11) . . . . ? C139 C140 C144 C145 67.8(13) . . . . ? C135 C140 C144 C146 123.8(11) . . . . ? C139 C140 C144 C146 -56.2(13) . . . . ? C131 N103 C147 C152 -97.7(11) . . . . ? Sm12 N103 C147 C152 92.8(9) . . . . ? C131 N103 C147 C148 84.6(11) . . . . ? Sm12 N103 C147 C148 -84.9(9) . . . . ? C152 C147 C148 C149 -1.2(14) . . . . ? N103 C147 C148 C149 176.4(8) . . . . ? C152 C147 C148 C153 -176.2(9) . . . . ? N103 C147 C148 C153 1.4(14) . . . . ? C147 C148 C149 C150 1.9(15) . . . . ? C153 C148 C149 C150 177.2(10) . . . . ? C148 C149 C150 C151 -1.0(17) . . . . ? C149 C150 C151 C152 -0.9(18) . . . . ? C150 C151 C152 C147 1.6(16) . . . . ? C150 C151 C152 C156 -176.6(10) . . . . ? C148 C147 C152 C151 -0.5(15) . . . . ? N103 C147 C152 C151 -178.2(9) . . . . ? C148 C147 C152 C156 177.6(9) . . . . ? N103 C147 C152 C156 0.0(14) . . . . ? C149 C148 C153 C154 53.0(13) . . . . ? C147 C148 C153 C154 -132.2(10) . . . . ? C149 C148 C153 C155 -70.1(12) . . . . ? C147 C148 C153 C155 104.7(11) . . . . ? C151 C152 C156 C157 39.4(14) . . . . ? C147 C152 C156 C157 -138.8(11) . . . . ? C151 C152 C156 C158 -85.7(13) . . . . ? C147 C152 C156 C158 96.1(12) . . . . ? C162 O101 C159 C160 -4.9(15) . . . . ? Sm11 O101 C159 C160 -178.2(10) . . . . ? O101 C159 C160 C161 20.1(19) . . . . ? C159 C160 C161 C162 -26.8(19) . . . . ? C159 O101 C162 C161 -11.6(11) . . . . ? Sm11 O101 C162 C161 161.9(7) . . . . ? C160 C161 C162 O101 23.6(15) . . . . ? C207 C201 C202 C203 178.2(14) . . . . ? C206 C201 C202 C203 -1(2) . . . . ? C201 C202 C203 C204 2(3) . . . . ? C202 C203 C204 C205 -4(2) . . . . ? C203 C204 C205 C206 6(2) . . . . ? C204 C205 C206 C201 -5(3) . . . . ? C207 C201 C206 C205 -176.7(16) . . . . ? C202 C201 C206 C205 2(2) . . . . ? C307 C301 C302 C303 172(3) . . . . ? C306 C301 C302 C303 4(4) . . . . ? C301 C302 C303 C304 -1(4) . . . . ? C302 C303 C304 C305 0(4) . . . . ? C303 C304 C305 C306 -3(3) . . . . ? C304 C305 C306 C301 6(3) . . . . ? C302 C301 C306 C305 -6(3) . . . . ? C307 C301 C306 C305 -176(2) . . . . ? C406 C401 C402 C403 2(3) . . . . ? C407 C401 C402 C403 179.6(15) . . . . ? C401 C402 C403 C404 -4(3) . . . . ? C402 C403 C404 C405 1(3) . . . . ? C403 C404 C405 C406 4(2) . . . . ? C402 C401 C406 C405 3(2) . . . . ? C407 C401 C406 C405 -174.4(14) . . . . ? C404 C405 C406 C401 -6(2) . . . . ? C506 C501 C502 C503 0.0 . . . . ? C507 C501 C502 C503 163(2) . . . . ? C501 C502 C503 C504 0.0 . . . . ? C502 C503 C504 C505 0.0 . . . . ? C502 C503 C504 C57A -175(2) . . . . ? C503 C504 C505 C506 0.0 . . . . ? C57A C504 C505 C506 176(2) . . . . ? C504 C505 C506 C501 0.0 . . . . ? C502 C501 C506 C505 0.0 . . . . ? C507 C501 C506 C505 -163(2) . . . . ? C606 C601 C602 C603 0.0 . . . . ? C601 C601 C602 C603 149(4) 3_666 . . . ? C606 C601 C602 C603 172.9(15) 3_666 . . . ? C601 C602 C603 C604 0.0 . . . . ? C602 C603 C604 C605 0.0 . . . . ? C603 C604 C605 C606 0.0 . . . . ? C604 C605 C606 C601 0.0 . . . . ? C604 C605 C606 C601 -119(11) . . . 3_666 ? C602 C601 C606 C605 0.0 . . . . ? C601 C601 C606 C605 -173.4(11) 3_666 . . . ? C606 C601 C606 C605 -173.4(16) 3_666 . . . ? C602 C601 C606 C601 173.4(11) . . . 3_666 ? C606 C601 C606 C601 0.0(5) 3_666 . . 3_666 ? C705 C701 C702 C703 -46.4 . . . . ? C704 C701 C702 C703 -14.7(13) 3_565 . . . ? C705 C701 C702 C704 -31.7(13) . . . 3_565 ? C701 C702 C703 C704 21.1 . . . . ? C704 C702 C703 C704 4.8(15) 3_565 . . . ? C701 C702 C703 C704 16.4(15) . . . 3_565 ? C701 C702 C703 C705 21(11) . . . 3_565 ? C704 C702 C703 C705 5(9) 3_565 . . 3_565 ? C702 C703 C704 C704 -7(2) . . . 3_565 ? C705 C703 C704 C704 173(4) 3_565 . . 3_565 ? C704 C703 C704 C703 0.0(3) 3_565 . . 3_565 ? C702 C703 C704 C703 -7(2) . . . 3_565 ? C705 C703 C704 C703 173(4) 3_565 . . 3_565 ? C704 C703 C704 C705 -173(4) 3_565 . . 3_565 ? C702 C703 C704 C705 180(2) . . . 3_565 ? C704 C703 C704 C701 174(4) 3_565 . . 3_565 ? C702 C703 C704 C701 168(2) . . . 3_565 ? C705 C703 C704 C701 -12.3(4) 3_565 . . 3_565 ? C704 C703 C704 C702 -162(8) 3_565 . . 3_565 ? C702 C703 C704 C702 -169(6) . . . 3_565 ? C705 C703 C704 C702 11(4) 3_565 . . 3_565 ? C702 C701 C705 C704 33.6(16) . . . 3_565 ? C702 C701 C705 C703 45.6(17) . . . 3_565 ? C704 C701 C705 C703 12.0(4) 3_565 . . 3_565 ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.354 _refine_diff_density_min -1.817 _refine_diff_density_rms 0.136 #============================================ data_NacNacSmClNTMS2 _database_code_depnum_ccdc_archive 'CCDC 244218' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H59 Cl N3 Si2 Sm' _chemical_formula_sum 'C35 H59 Cl N3 Si2 Sm' _chemical_formula_weight 763.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 17.208(3) _cell_length_b 18.256(4) _cell_length_c 13.022(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.74(3) _cell_angle_gamma 90.00 _cell_volume 3973.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 24.74 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 1.630 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6319 _exptl_absorpt_correction_T_max 0.7920 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method /w\2/q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17450 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.57 _reflns_number_total 6694 _reflns_number_gt 5533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.052d' _computing_cell_refinement 'Bruker SAINT v5.10' _computing_data_reduction 'Bruker SAINT v5.10' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6694 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.785228(9) 0.574739(8) 0.329001(12) 0.01960(7) Uani 1 1 d . . . Cl1 Cl 0.88322(5) 0.63313(5) 0.49323(7) 0.0344(2) Uani 1 1 d . . . Si1 Si 0.59592(5) 0.57794(5) 0.18117(8) 0.0259(2) Uani 1 1 d . . . Si2 Si 0.63289(5) 0.70788(5) 0.32676(8) 0.0273(2) Uani 1 1 d . . . N1 N 0.86354(15) 0.52741(14) 0.2190(2) 0.0221(6) Uani 1 1 d . . . N2 N 0.78206(15) 0.45150(14) 0.3754(2) 0.0216(6) Uani 1 1 d . . . N3 N 0.66155(15) 0.62616(14) 0.2784(2) 0.0242(6) Uani 1 1 d . . . C1 C 1.00862(19) 0.4980(2) 0.2574(3) 0.0332(8) Uani 1 1 d . . . H1A H 1.0459 0.4664 0.3066 0.050 Uiso 1 1 calc R . . H1B H 1.0285 0.5485 0.2644 0.050 Uiso 1 1 calc R . . H1C H 1.0042 0.4810 0.1848 0.050 Uiso 1 1 calc R . . C2 C 0.92673(18) 0.49499(16) 0.2827(3) 0.0226(7) Uani 1 1 d . . . C3 C 0.92339(19) 0.45719(17) 0.3768(3) 0.0250(7) Uani 1 1 d . . . H3A H 0.9740 0.4492 0.4240 0.030 Uiso 1 1 calc R . . C4 C 0.85803(19) 0.42950(17) 0.4121(3) 0.0246(7) Uani 1 1 d . . . C5 C 0.8786(2) 0.3716(2) 0.4979(3) 0.0408(10) Uani 1 1 d . . . H5A H 0.8668 0.3229 0.4663 0.061 Uiso 1 1 calc R . . H5B H 0.8468 0.3797 0.5500 0.061 Uiso 1 1 calc R . . H5C H 0.9357 0.3748 0.5328 0.061 Uiso 1 1 calc R . . C6 C 0.87280(19) 0.55632(18) 0.1193(3) 0.0240(7) Uani 1 1 d . . . C7 C 0.90002(19) 0.62878(18) 0.1148(3) 0.0258(7) Uani 1 1 d . . . C8 C 0.9073(2) 0.65618(19) 0.0174(3) 0.0331(8) Uani 1 1 d . . . H8A H 0.9252 0.7051 0.0128 0.040 Uiso 1 1 calc R . . C9 C 0.8890(2) 0.6130(2) -0.0728(3) 0.0385(9) Uani 1 1 d . . . H9A H 0.8952 0.6321 -0.1382 0.046 Uiso 1 1 calc R . . C10 C 0.8619(2) 0.5429(2) -0.0677(3) 0.0357(9) Uani 1 1 d . . . H10A H 0.8491 0.5141 -0.1303 0.043 Uiso 1 1 calc R . . C11 C 0.8524(2) 0.51220(18) 0.0279(3) 0.0276(8) Uani 1 1 d . . . C12 C 0.9176(2) 0.67735(18) 0.2132(3) 0.0283(8) Uani 1 1 d . . . H12A H 0.9286 0.6443 0.2763 0.034 Uiso 1 1 calc R . . C13 C 0.8438(2) 0.72292(19) 0.2170(3) 0.0331(8) Uani 1 1 d . . . H13A H 0.8507 0.7446 0.2875 0.050 Uiso 1 1 calc R . . H13B H 0.7964 0.6914 0.2019 0.050 Uiso 1 1 calc R . . H13C H 0.8371 0.7620 0.1641 0.050 Uiso 1 1 calc R . . C14 C 0.9909(2) 0.7272(2) 0.2229(3) 0.0470(10) Uani 1 1 d . . . H14A H 1.0375 0.6974 0.2191 0.070 Uiso 1 1 calc R . . H14B H 1.0016 0.7531 0.2907 0.070 Uiso 1 1 calc R . . H14C H 0.9804 0.7629 0.1650 0.070 Uiso 1 1 calc R . . C15 C 0.8199(2) 0.43478(18) 0.0307(3) 0.0341(9) Uani 1 1 d . . . H15A H 0.7973 0.4310 0.0945 0.041 Uiso 1 1 calc R . . C16 C 0.8858(3) 0.3773(2) 0.0416(4) 0.0547(12) Uani 1 1 d . . . H16A H 0.9265 0.3858 0.1071 0.082 Uiso 1 1 calc R . . H16B H 0.9103 0.3807 -0.0189 0.082 Uiso 1 1 calc R . . H16C H 0.8627 0.3283 0.0434 0.082 Uiso 1 1 calc R . . C17 C 0.7521(3) 0.4182(2) -0.0665(3) 0.0464(11) Uani 1 1 d . . . H17A H 0.7127 0.4580 -0.0770 0.070 Uiso 1 1 calc R . . H17B H 0.7261 0.3721 -0.0555 0.070 Uiso 1 1 calc R . . H17C H 0.7740 0.4139 -0.1291 0.070 Uiso 1 1 calc R . . C18 C 0.71833(19) 0.40728(17) 0.3965(3) 0.0225(7) Uani 1 1 d . . . C19 C 0.69633(19) 0.34267(17) 0.3361(3) 0.0259(7) Uani 1 1 d . . . C20 C 0.6348(2) 0.30012(19) 0.3589(3) 0.0339(8) Uani 1 1 d . . . H20A H 0.6194 0.2562 0.3203 0.041 Uiso 1 1 calc R . . C21 C 0.5963(2) 0.3201(2) 0.4357(3) 0.0360(9) Uani 1 1 d . . . H21A H 0.5554 0.2898 0.4504 0.043 Uiso 1 1 calc R . . C22 C 0.6171(2) 0.38434(19) 0.4913(3) 0.0330(8) Uani 1 1 d . . . H22A H 0.5894 0.3982 0.5433 0.040 Uiso 1 1 calc R . . C23 C 0.6777(2) 0.42916(17) 0.4728(3) 0.0274(8) Uani 1 1 d . . . C24 C 0.7351(2) 0.32014(19) 0.2473(3) 0.0314(8) Uani 1 1 d . . . H24A H 0.7729 0.3598 0.2381 0.038 Uiso 1 1 calc R . . C25 C 0.6724(3) 0.3116(2) 0.1429(3) 0.0497(11) Uani 1 1 d . . . H25A H 0.6409 0.3567 0.1277 0.075 Uiso 1 1 calc R . . H25B H 0.6370 0.2705 0.1484 0.075 Uiso 1 1 calc R . . H25C H 0.6993 0.3020 0.0858 0.075 Uiso 1 1 calc R . . C26 C 0.7820(3) 0.2496(3) 0.2707(4) 0.0654(14) Uani 1 1 d . . . H26A H 0.8225 0.2545 0.3374 0.098 Uiso 1 1 calc R . . H26B H 0.8083 0.2391 0.2133 0.098 Uiso 1 1 calc R . . H26C H 0.7456 0.2093 0.2765 0.098 Uiso 1 1 calc R . . C27 C 0.6971(2) 0.5000(2) 0.5363(3) 0.0383(9) Uani 1 1 d . . . H27A H 0.7260 0.5326 0.4961 0.046 Uiso 1 1 calc R . . C28 C 0.6239(3) 0.5412(3) 0.5489(4) 0.0664(14) Uani 1 1 d . . . H28A H 0.6398 0.5895 0.5795 0.100 Uiso 1 1 calc R . . H28B H 0.5976 0.5137 0.5958 0.100 Uiso 1 1 calc R . . H28C H 0.5867 0.5471 0.4796 0.100 Uiso 1 1 calc R . . C29 C 0.7522(4) 0.4873(4) 0.6430(5) 0.131(3) Uani 1 1 d . . . H29A H 0.7642 0.5342 0.6800 0.197 Uiso 1 1 calc R . . H29B H 0.8020 0.4650 0.6342 0.197 Uiso 1 1 calc R . . H29C H 0.7264 0.4545 0.6844 0.197 Uiso 1 1 calc R . . C30 C 0.5277(2) 0.5151(2) 0.2321(3) 0.0459(10) Uani 1 1 d . . . H30A H 0.4947 0.4875 0.1731 0.069 Uiso 1 1 calc R . . H30B H 0.4932 0.5439 0.2667 0.069 Uiso 1 1 calc R . . H30C H 0.5597 0.4809 0.2832 0.069 Uiso 1 1 calc R . . C31 C 0.5317(2) 0.6349(2) 0.0750(3) 0.0402(9) Uani 1 1 d . . . H31A H 0.5034 0.6030 0.0177 0.060 Uiso 1 1 calc R . . H31B H 0.5653 0.6695 0.0475 0.060 Uiso 1 1 calc R . . H31C H 0.4927 0.6620 0.1042 0.060 Uiso 1 1 calc R . . C32 C 0.6589(2) 0.5198(2) 0.1132(3) 0.0469(11) Uani 1 1 d . . . H32A H 0.6241 0.4901 0.0584 0.070 Uiso 1 1 calc R . . H32B H 0.6932 0.4876 0.1651 0.070 Uiso 1 1 calc R . . H32C H 0.6924 0.5515 0.0808 0.070 Uiso 1 1 calc R . . C33 C 0.6318(2) 0.78627(19) 0.2339(3) 0.0428(10) Uani 1 1 d . . . H33A H 0.6853 0.7928 0.2215 0.064 Uiso 1 1 calc R . . H33B H 0.6158 0.8311 0.2649 0.064 Uiso 1 1 calc R . . H33C H 0.5935 0.7760 0.1667 0.064 Uiso 1 1 calc R . . C34 C 0.5311(2) 0.7011(2) 0.3561(3) 0.0398(9) Uani 1 1 d . . . H34A H 0.5335 0.6672 0.4152 0.060 Uiso 1 1 calc R . . H34B H 0.4925 0.6829 0.2934 0.060 Uiso 1 1 calc R . . H34C H 0.5144 0.7496 0.3750 0.060 Uiso 1 1 calc R . . C35 C 0.7037(2) 0.7352(2) 0.4537(3) 0.0390(9) Uani 1 1 d . . . H35A H 0.7573 0.7423 0.4416 0.059 Uiso 1 1 calc R . . H35B H 0.7056 0.6966 0.5065 0.059 Uiso 1 1 calc R . . H35C H 0.6854 0.7810 0.4794 0.059 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 Sm1 0.01854(10) 0.02012(10) 0.01903(11) 0.00069(7) 0.00226(7) 0.00090(7) Cl1 0.0323(5) 0.0317(5) 0.0318(5) -0.0072(4) -0.0072(4) 0.0044(4) Si1 0.0213(5) 0.0290(5) 0.0251(5) 0.0015(4) 0.0008(4) 0.0018(4) Si2 0.0224(5) 0.0293(5) 0.0310(5) -0.0015(4) 0.0078(4) 0.0041(4) N1 0.0205(14) 0.0226(14) 0.0221(15) 0.0011(11) 0.0029(12) -0.0012(11) N2 0.0214(15) 0.0231(14) 0.0194(14) 0.0014(11) 0.0031(11) -0.0020(11) N3 0.0211(14) 0.0245(14) 0.0259(15) 0.0027(12) 0.0032(12) 0.0012(11) C1 0.0238(18) 0.038(2) 0.039(2) 0.0042(17) 0.0093(16) 0.0075(16) C2 0.0207(17) 0.0194(16) 0.0264(18) -0.0031(14) 0.0034(14) -0.0014(13) C3 0.0196(17) 0.0237(17) 0.0280(19) -0.0002(14) -0.0016(14) 0.0012(14) C4 0.0245(18) 0.0240(17) 0.0214(17) 0.0011(14) -0.0022(14) -0.0033(14) C5 0.036(2) 0.044(2) 0.037(2) 0.0183(18) -0.0016(18) 0.0007(18) C6 0.0189(17) 0.0295(18) 0.0247(18) 0.0028(14) 0.0070(14) 0.0027(14) C7 0.0218(18) 0.0269(18) 0.0295(19) 0.0024(14) 0.0079(15) 0.0035(14) C8 0.035(2) 0.0275(19) 0.041(2) 0.0068(16) 0.0159(17) 0.0039(16) C9 0.050(2) 0.041(2) 0.030(2) 0.0082(17) 0.0196(18) 0.0099(19) C10 0.043(2) 0.038(2) 0.030(2) -0.0027(17) 0.0171(18) 0.0042(18) C11 0.0255(18) 0.0310(19) 0.0278(19) -0.0002(15) 0.0096(15) 0.0060(15) C12 0.0284(19) 0.0264(18) 0.0291(19) 0.0033(15) 0.0050(15) -0.0029(15) C13 0.039(2) 0.0297(19) 0.030(2) -0.0050(16) 0.0061(16) 0.0009(16) C14 0.037(2) 0.048(2) 0.052(3) 0.003(2) 0.003(2) -0.0124(19) C15 0.042(2) 0.031(2) 0.032(2) -0.0043(16) 0.0122(17) -0.0011(16) C16 0.058(3) 0.033(2) 0.072(3) -0.004(2) 0.014(2) 0.003(2) C17 0.056(3) 0.048(2) 0.033(2) -0.0109(18) 0.005(2) -0.015(2) C18 0.0205(17) 0.0230(17) 0.0201(17) 0.0055(13) -0.0027(14) -0.0006(13) C19 0.0243(18) 0.0250(17) 0.0258(18) 0.0036(14) 0.0007(14) -0.0004(14) C20 0.034(2) 0.0298(19) 0.035(2) -0.0010(16) 0.0023(17) -0.0123(16) C21 0.034(2) 0.038(2) 0.038(2) 0.0052(17) 0.0105(17) -0.0119(17) C22 0.033(2) 0.038(2) 0.031(2) 0.0035(16) 0.0122(16) -0.0053(17) C23 0.0282(19) 0.0295(19) 0.0225(18) 0.0041(14) 0.0024(15) -0.0027(15) C24 0.032(2) 0.0289(19) 0.034(2) -0.0025(16) 0.0103(16) -0.0090(16) C25 0.053(3) 0.062(3) 0.035(2) -0.009(2) 0.011(2) -0.011(2) C26 0.072(3) 0.068(3) 0.061(3) 0.008(3) 0.027(3) 0.033(3) C27 0.048(2) 0.040(2) 0.032(2) -0.0091(17) 0.0198(18) -0.0175(18) C28 0.067(3) 0.056(3) 0.071(3) -0.026(3) 0.007(3) 0.007(3) C29 0.125(5) 0.111(5) 0.104(5) -0.070(4) -0.079(4) 0.052(4) C30 0.041(2) 0.046(2) 0.046(3) 0.005(2) 0.0004(19) -0.0129(19) C31 0.036(2) 0.042(2) 0.035(2) 0.0052(18) -0.0065(17) 0.0055(18) C32 0.032(2) 0.053(3) 0.049(3) -0.021(2) -0.0039(19) 0.0093(19) C33 0.045(2) 0.031(2) 0.055(3) 0.0038(19) 0.015(2) 0.0068(18) C34 0.026(2) 0.051(2) 0.043(2) -0.0059(19) 0.0098(17) 0.0066(17) C35 0.033(2) 0.043(2) 0.040(2) -0.0125(18) 0.0076(17) 0.0043(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N3 2.276(3) . ? Sm1 N2 2.333(3) . ? Sm1 N1 2.352(3) . ? Sm1 Cl1 2.6154(11) . ? Sm1 C2 3.018(3) . ? Sm1 C4 3.021(3) . ? Sm1 Si1 3.3678(14) . ? Si1 N3 1.724(3) . ? Si1 C31 1.868(4) . ? Si1 C30 1.872(4) . ? Si1 C32 1.881(4) . ? Si2 N3 1.736(3) . ? Si2 C33 1.870(4) . ? Si2 C35 1.874(4) . ? Si2 C34 1.883(3) . ? N1 C2 1.339(4) . ? N1 C6 1.445(4) . ? N2 C4 1.342(4) . ? N2 C18 1.440(4) . ? C1 C2 1.523(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.419(4) . ? C3 C4 1.406(5) . ? C3 H3A 0.9500 . ? C4 C5 1.518(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.409(4) . ? C6 C11 1.411(5) . ? C7 C8 1.398(5) . ? C7 C12 1.528(5) . ? C8 C9 1.387(5) . ? C8 H8A 0.9500 . ? C9 C10 1.370(5) . ? C9 H9A 0.9500 . ? C10 C11 1.409(5) . ? C10 H10A 0.9500 . ? C11 C15 1.523(5) . ? C12 C13 1.528(5) . ? C12 C14 1.536(5) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.526(5) . ? C15 C17 1.535(5) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.401(5) . ? C18 C19 1.419(4) . ? C19 C20 1.400(5) . ? C19 C24 1.522(5) . ? C20 C21 1.374(5) . ? C20 H20A 0.9500 . ? C21 C22 1.380(5) . ? C21 H21A 0.9500 . ? C22 C23 1.391(5) . ? C22 H22A 0.9500 . ? C23 C27 1.528(5) . ? C24 C26 1.513(5) . ? C24 C25 1.529(5) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.503(6) . ? C27 C28 1.510(6) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? 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 113.27(9) . . ? N3 Sm1 N1 127.35(9) . . ? N2 Sm1 N1 81.69(9) . . ? N3 Sm1 Cl1 116.47(7) . . ? N2 Sm1 Cl1 103.39(7) . . ? N1 Sm1 Cl1 107.24(7) . . ? N3 Sm1 C2 152.19(9) . . ? N2 Sm1 C2 69.88(9) . . ? N1 Sm1 C2 25.18(9) . . ? Cl1 Sm1 C2 88.04(7) . . ? N3 Sm1 C4 138.21(9) . . ? N2 Sm1 C4 25.08(9) . . ? N1 Sm1 C4 69.33(9) . . ? Cl1 Sm1 C4 86.14(7) . . ? C2 Sm1 C4 50.40(9) . . ? N3 Sm1 Si1 27.89(7) . . ? N2 Sm1 Si1 94.92(7) . . ? N1 Sm1 Si1 105.94(7) . . ? Cl1 Sm1 Si1 143.96(3) . . ? C2 Sm1 Si1 127.66(6) . . ? C4 Sm1 Si1 118.85(6) . . ? N3 Si1 C31 115.36(15) . . ? N3 Si1 C30 114.16(16) . . ? C31 Si1 C30 107.03(18) . . ? N3 Si1 C32 106.43(15) . . ? C31 Si1 C32 105.77(18) . . ? C30 Si1 C32 107.5(2) . . ? N3 Si1 Sm1 38.13(9) . . ? C31 Si1 Sm1 139.01(13) . . ? C30 Si1 Sm1 112.93(13) . . ? C32 Si1 Sm1 70.84(12) . . ? N3 Si2 C33 112.53(15) . . ? N3 Si2 C35 111.57(15) . . ? C33 Si2 C35 105.74(18) . . ? N3 Si2 C34 112.05(15) . . ? C33 Si2 C34 108.30(18) . . ? C35 Si2 C34 106.26(17) . . ? C2 N1 C6 118.2(3) . . ? C2 N1 Sm1 106.45(19) . . ? C6 N1 Sm1 127.9(2) . . ? C4 N2 C18 119.0(3) . . ? C4 N2 Sm1 107.46(19) . . ? C18 N2 Sm1 131.0(2) . . ? Si1 N3 Si2 120.81(15) . . ? Si1 N3 Sm1 113.98(13) . . ? Si2 N3 Sm1 125.18(14) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.8(3) . . ? N1 C2 C1 120.4(3) . . ? C3 C2 C1 115.7(3) . . ? N1 C2 Sm1 48.37(15) . . ? C3 C2 Sm1 82.08(18) . . ? C1 C2 Sm1 149.1(2) . . ? C4 C3 C2 131.0(3) . . ? C4 C3 H3A 114.5 . . ? C2 C3 H3A 114.5 . . ? N2 C4 C3 124.2(3) . . ? N2 C4 C5 120.6(3) . . ? C3 C4 C5 115.2(3) . . ? N2 C4 Sm1 47.46(15) . . ? C3 C4 Sm1 82.14(19) . . ? C5 C4 Sm1 151.6(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 121.3(3) . . ? C7 C6 N1 119.3(3) . . ? C11 C6 N1 119.4(3) . . ? C8 C7 C6 118.4(3) . . ? C8 C7 C12 120.8(3) . . ? C6 C7 C12 120.8(3) . . ? C9 C8 C7 120.9(3) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C11 121.8(3) . . ? C9 C10 H10A 119.1 . . ? C11 C10 H10A 119.1 . . ? C10 C11 C6 117.4(3) . . ? C10 C11 C15 120.6(3) . . ? C6 C11 C15 121.9(3) . . ? C7 C12 C13 110.0(3) . . ? C7 C12 C14 114.0(3) . . ? C13 C12 C14 110.3(3) . . ? C7 C12 H12A 107.4 . . ? C13 C12 H12A 107.4 . . ? C14 C12 H12A 107.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 111.9(3) . . ? C11 C15 C17 112.0(3) . . ? C16 C15 C17 110.1(3) . . ? C11 C15 H15A 107.5 . . ? C16 C15 H15A 107.5 . . ? C17 C15 H15A 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 121.2(3) . . ? C23 C18 N2 120.5(3) . . ? C19 C18 N2 118.3(3) . . ? C20 C19 C18 117.3(3) . . ? C20 C19 C24 120.1(3) . . ? C18 C19 C24 122.6(3) . . ? C21 C20 C19 121.8(3) . . ? C21 C20 H20A 119.1 . . ? C19 C20 H20A 119.1 . . ? C20 C21 C22 119.9(3) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C21 C22 C23 121.3(3) . . ? C21 C22 H22A 119.3 . . ? C23 C22 H22A 119.3 . . ? C22 C23 C18 118.4(3) . . ? C22 C23 C27 118.7(3) . . ? C18 C23 C27 122.9(3) . . ? C26 C24 C19 112.7(3) . . ? C26 C24 C25 108.8(3) . . ? C19 C24 C25 111.1(3) . . ? C26 C24 H24A 108.0 . . ? C19 C24 H24A 108.0 . . ? C25 C24 H24A 108.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 109.6(4) . . ? C29 C27 C23 112.3(4) . . ? C28 C27 C23 113.6(3) . . ? C29 C27 H27A 107.0 . . ? C28 C27 H27A 107.0 . . ? C23 C27 H27A 107.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Sm1 Si1 N3 133.23(15) . . . . ? N1 Sm1 Si1 N3 -144.03(15) . . . . ? Cl1 Sm1 Si1 N3 12.35(15) . . . . ? C2 Sm1 Si1 N3 -158.47(16) . . . . ? C4 Sm1 Si1 N3 141.15(16) . . . . ? N3 Sm1 Si1 C31 65.9(2) . . . . ? N2 Sm1 Si1 C31 -160.9(2) . . . . ? N1 Sm1 Si1 C31 -78.2(2) . . . . ? Cl1 Sm1 Si1 C31 78.2(2) . . . . ? C2 Sm1 Si1 C31 -92.6(2) . . . . ? C4 Sm1 Si1 C31 -153.0(2) . . . . ? N3 Sm1 Si1 C30 -100.4(2) . . . . ? N2 Sm1 Si1 C30 32.80(16) . . . . ? N1 Sm1 Si1 C30 115.55(16) . . . . ? Cl1 Sm1 Si1 C30 -88.08(16) . . . . ? C2 Sm1 Si1 C30 101.11(17) . . . . ? C4 Sm1 Si1 C30 40.73(17) . . . . ? N3 Sm1 Si1 C32 158.1(2) . . . . ? N2 Sm1 Si1 C32 -68.68(17) . . . . ? N1 Sm1 Si1 C32 14.06(16) . . . . ? Cl1 Sm1 Si1 C32 170.44(15) . . . . ? C2 Sm1 Si1 C32 -0.37(17) . . . . ? C4 Sm1 Si1 C32 -60.76(17) . . . . ? N3 Sm1 N1 C2 -172.59(18) . . . . ? N2 Sm1 N1 C2 -59.6(2) . . . . ? Cl1 Sm1 N1 C2 41.9(2) . . . . ? C4 Sm1 N1 C2 -36.99(19) . . . . ? Si1 Sm1 N1 C2 -152.37(18) . . . . ? N3 Sm1 N1 C6 38.8(3) . . . . ? N2 Sm1 N1 C6 151.8(3) . . . . ? Cl1 Sm1 N1 C6 -106.7(2) . . . . ? C2 Sm1 N1 C6 -148.6(4) . . . . ? C4 Sm1 N1 C6 174.4(3) . . . . ? Si1 Sm1 N1 C6 59.0(2) . . . . ? N3 Sm1 N2 C4 -174.8(2) . . . . ? N1 Sm1 N2 C4 58.0(2) . . . . ? Cl1 Sm1 N2 C4 -47.8(2) . . . . ? C2 Sm1 N2 C4 35.0(2) . . . . ? Si1 Sm1 N2 C4 163.5(2) . . . . ? N3 Sm1 N2 C18 -13.5(3) . . . . ? N1 Sm1 N2 C18 -140.7(3) . . . . ? Cl1 Sm1 N2 C18 113.5(3) . . . . ? C2 Sm1 N2 C18 -163.7(3) . . . . ? C4 Sm1 N2 C18 161.3(4) . . . . ? Si1 Sm1 N2 C18 -35.3(3) . . . . ? C31 Si1 N3 Si2 39.5(2) . . . . ? C30 Si1 N3 Si2 -85.0(2) . . . . ? C32 Si1 N3 Si2 156.5(2) . . . . ? Sm1 Si1 N3 Si2 178.1(3) . . . . ? C31 Si1 N3 Sm1 -138.51(16) . . . . ? C30 Si1 N3 Sm1 96.89(19) . . . . ? C32 Si1 N3 Sm1 -21.6(2) . . . . ? C33 Si2 N3 Si1 -76.6(2) . . . . ? C35 Si2 N3 Si1 164.77(18) . . . . ? C34 Si2 N3 Si1 45.8(2) . . . . ? C33 Si2 N3 Sm1 101.3(2) . . . . ? C35 Si2 N3 Sm1 -17.4(2) . . . . ? C34 Si2 N3 Sm1 -136.40(18) . . . . ? N2 Sm1 N3 Si1 -52.21(16) . . . . ? N1 Sm1 N3 Si1 45.27(18) . . . . ? Cl1 Sm1 N3 Si1 -171.92(10) . . . . ? C2 Sm1 N3 Si1 38.5(3) . . . . ? C4 Sm1 N3 Si1 -55.5(2) . . . . ? N2 Sm1 N3 Si2 129.83(16) . . . . ? N1 Sm1 N3 Si2 -132.69(15) . . . . ? Cl1 Sm1 N3 Si2 10.11(19) . . . . ? C2 Sm1 N3 Si2 -139.45(16) . . . . ? C4 Sm1 N3 Si2 126.50(16) . . . . ? Si1 Sm1 N3 Si2 -178.0(3) . . . . ? C6 N1 C2 C3 -172.6(3) . . . . ? Sm1 N1 C2 C3 35.2(4) . . . . ? C6 N1 C2 C1 8.2(4) . . . . ? Sm1 N1 C2 C1 -144.0(3) . . . . ? C6 N1 C2 Sm1 152.2(3) . . . . ? N3 Sm1 C2 N1 12.7(3) . . . . ? N2 Sm1 C2 N1 114.7(2) . . . . ? Cl1 Sm1 C2 N1 -140.32(19) . . . . ? C4 Sm1 C2 N1 133.1(2) . . . . ? Si1 Sm1 C2 N1 34.3(2) . . . . ? N3 Sm1 C2 C3 -138.4(2) . . . . ? N2 Sm1 C2 C3 -36.47(18) . . . . ? N1 Sm1 C2 C3 -151.1(3) . . . . ? Cl1 Sm1 C2 C3 68.55(18) . . . . ? C4 Sm1 C2 C3 -18.06(17) . . . . ? Si1 Sm1 C2 C3 -116.84(17) . . . . ? N3 Sm1 C2 C1 93.2(5) . . . . ? N2 Sm1 C2 C1 -164.8(5) . . . . ? N1 Sm1 C2 C1 80.5(5) . . . . ? Cl1 Sm1 C2 C1 -59.8(4) . . . . ? C4 Sm1 C2 C1 -146.4(5) . . . . ? Si1 Sm1 C2 C1 114.8(4) . . . . ? N1 C2 C3 C4 17.1(6) . . . . ? C1 C2 C3 C4 -163.7(3) . . . . ? Sm1 C2 C3 C4 42.9(4) . . . . ? C18 N2 C4 C3 164.2(3) . . . . ? Sm1 N2 C4 C3 -31.9(4) . . . . ? C18 N2 C4 C5 -16.3(5) . . . . ? Sm1 N2 C4 C5 147.6(3) . . . . ? C18 N2 C4 Sm1 -163.9(3) . . . . ? C2 C3 C4 N2 -19.7(6) . . . . ? C2 C3 C4 C5 160.8(3) . . . . ? C2 C3 C4 Sm1 -42.8(4) . . . . ? N3 Sm1 C4 N2 7.2(3) . . . . ? N1 Sm1 C4 N2 -116.2(2) . . . . ? Cl1 Sm1 C4 N2 133.7(2) . . . . ? C2 Sm1 C4 N2 -135.6(2) . . . . ? Si1 Sm1 C4 N2 -18.9(2) . . . . ? N3 Sm1 C4 C3 161.07(18) . . . . ? N2 Sm1 C4 C3 153.8(3) . . . . ? N1 Sm1 C4 C3 37.64(19) . . . . ? Cl1 Sm1 C4 C3 -72.42(18) . . . . ? C2 Sm1 C4 C3 18.23(17) . . . . ? Si1 Sm1 C4 C3 134.94(17) . . . . ? N3 Sm1 C4 C5 -68.5(5) . . . . ? N2 Sm1 C4 C5 -75.8(5) . . . . ? N1 Sm1 C4 C5 168.0(5) . . . . ? Cl1 Sm1 C4 C5 58.0(5) . . . . ? C2 Sm1 C4 C5 148.6(5) . . . . ? Si1 Sm1 C4 C5 -94.7(5) . . . . ? C2 N1 C6 C7 -88.6(4) . . . . ? Sm1 N1 C6 C7 56.9(4) . . . . ? C2 N1 C6 C11 93.1(4) . . . . ? Sm1 N1 C6 C11 -121.4(3) . . . . ? C11 C6 C7 C8 -0.7(5) . . . . ? N1 C6 C7 C8 -179.0(3) . . . . ? C11 C6 C7 C12 176.7(3) . . . . ? N1 C6 C7 C12 -1.6(4) . . . . ? C6 C7 C8 C9 -0.6(5) . . . . ? C12 C7 C8 C9 -177.9(3) . . . . ? C7 C8 C9 C10 1.2(5) . . . . ? C8 C9 C10 C11 -0.6(6) . . . . ? C9 C10 C11 C6 -0.6(5) . . . . ? C9 C10 C11 C15 178.3(3) . . . . ? C7 C6 C11 C10 1.3(5) . . . . ? N1 C6 C11 C10 179.5(3) . . . . ? C7 C6 C11 C15 -177.7(3) . . . . ? N1 C6 C11 C15 0.6(5) . . . . ? C8 C7 C12 C13 83.9(4) . . . . ? C6 C7 C12 C13 -93.4(4) . . . . ? C8 C7 C12 C14 -40.7(4) . . . . ? C6 C7 C12 C14 142.0(3) . . . . ? C10 C11 C15 C16 84.8(4) . . . . ? C6 C11 C15 C16 -96.4(4) . . . . ? C10 C11 C15 C17 -39.4(5) . . . . ? C6 C11 C15 C17 139.5(3) . . . . ? C4 N2 C18 C23 105.0(4) . . . . ? Sm1 N2 C18 C23 -54.5(4) . . . . ? C4 N2 C18 C19 -77.1(4) . . . . ? Sm1 N2 C18 C19 123.4(3) . . . . ? C23 C18 C19 C20 -2.8(5) . . . . ? N2 C18 C19 C20 179.3(3) . . . . ? C23 C18 C19 C24 175.5(3) . . . . ? N2 C18 C19 C24 -2.5(5) . . . . ? C18 C19 C20 C21 0.8(5) . . . . ? C24 C19 C20 C21 -177.5(3) . . . . ? C19 C20 C21 C22 1.1(6) . . . . ? C20 C21 C22 C23 -1.2(6) . . . . ? C21 C22 C23 C18 -0.7(5) . . . . ? C21 C22 C23 C27 179.3(3) . . . . ? C19 C18 C23 C22 2.7(5) . . . . ? N2 C18 C23 C22 -179.4(3) . . . . ? C19 C18 C23 C27 -177.3(3) . . . . ? N2 C18 C23 C27 0.6(5) . . . . ? C20 C19 C24 C26 -66.8(4) . . . . ? C18 C19 C24 C26 115.0(4) . . . . ? C20 C19 C24 C25 55.6(4) . . . . ? C18 C19 C24 C25 -122.6(3) . . . . ? C22 C23 C27 C29 83.0(5) . . . . ? C18 C23 C27 C29 -96.9(5) . . . . ? C22 C23 C27 C28 -42.0(5) . . . . ? C18 C23 C27 C28 138.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 25.57 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.645 _refine_diff_density_min -1.680 _refine_diff_density_rms 0.089 #========================================= data_nacSmTMS2 _database_code_depnum_ccdc_archive 'CCDC 244219' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C41 H75 N4 Si4 Sm), 0.5(C7 H8)' _chemical_formula_sum 'C44.50 H79 N4 Si4 Sm' _chemical_formula_weight 932.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.686(2) _cell_length_b 11.708(2) _cell_length_c 20.510(4) _cell_angle_alpha 75.55(3) _cell_angle_beta 79.49(3) _cell_angle_gamma 68.51(3) _cell_volume 2515.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 23.04 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.294 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6673 _exptl_absorpt_correction_T_max 0.8602 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method /w\2/q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12827 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.55 _reflns_number_total 8108 _reflns_number_gt 7035 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.052' _computing_cell_refinement 'Bruker SAINT v5.10' _computing_data_reduction 'Bruker SAINT v5.10' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of toluene was located from a Fourier Difference map. It was found to be disordered across the inversion center at [1, 0.5, 0]. Hydrogen atoms positions were not calculated for this molecule. ; _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^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8108 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1083 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.689797(18) 0.235185(18) 0.741047(10) 0.01446(9) Uani 1 1 d . . . Si1 Si 0.51959(11) 0.53414(11) 0.77249(6) 0.0214(3) Uani 1 1 d . . . Si2 Si 0.37080(10) 0.42990(11) 0.71901(6) 0.0209(3) Uani 1 1 d . . . Si3 Si 0.54307(11) 0.02116(11) 0.79668(6) 0.0218(3) Uani 1 1 d . . . Si4 Si 0.65762(11) 0.02133(11) 0.65244(6) 0.0201(3) Uani 1 1 d . . . N1 N 0.8606(3) 0.2932(3) 0.67316(16) 0.0154(7) Uani 1 1 d . . . N2 N 0.8477(3) 0.1586(3) 0.82385(17) 0.0167(7) Uani 1 1 d . . . N3 N 0.5139(3) 0.4124(3) 0.74059(17) 0.0172(7) Uani 1 1 d . . . N4 N 0.6298(3) 0.0774(3) 0.72673(18) 0.0197(8) Uani 1 1 d . . . C1 C 0.9973(4) 0.4215(4) 0.6532(2) 0.0279(10) Uani 1 1 d . . . H1A H 1.0496 0.3814 0.6165 0.042 Uiso 1 1 calc R . . H1B H 1.0484 0.4403 0.6792 0.042 Uiso 1 1 calc R . . H1C H 0.9344 0.4994 0.6341 0.042 Uiso 1 1 calc R . . C2 C 0.9344(4) 0.3336(4) 0.6995(2) 0.0194(9) Uani 1 1 d . . . C3 C 0.9605(4) 0.2983(4) 0.7671(2) 0.0187(9) Uani 1 1 d . . . H3A H 1.0037 0.3442 0.7784 0.022 Uiso 1 1 calc R . . C4 C 0.9350(3) 0.2086(4) 0.8207(2) 0.0155(8) Uani 1 1 d . . . C5 C 1.0164(4) 0.1700(4) 0.8777(2) 0.0238(10) Uani 1 1 d . . . H5A H 1.0118 0.0909 0.9064 0.036 Uiso 1 1 calc R . . H5B H 0.9879 0.2352 0.9048 0.036 Uiso 1 1 calc R . . H5C H 1.1021 0.1591 0.8586 0.036 Uiso 1 1 calc R . . C6 C 0.8857(4) 0.2994(4) 0.6006(2) 0.0179(9) Uani 1 1 d . . . C7 C 0.8177(4) 0.4016(4) 0.5538(2) 0.0192(9) Uani 1 1 d . . . C8 C 0.8442(4) 0.3971(4) 0.4852(2) 0.0244(10) Uani 1 1 d . . . H8A H 0.7979 0.4646 0.4533 0.029 Uiso 1 1 calc R . . C9 C 0.9357(4) 0.2973(4) 0.4623(2) 0.0252(10) Uani 1 1 d . . . H9A H 0.9514 0.2961 0.4153 0.030 Uiso 1 1 calc R . . C10 C 1.0041(4) 0.1992(4) 0.5081(2) 0.0219(9) Uani 1 1 d . . . H10A H 1.0684 0.1317 0.4920 0.026 Uiso 1 1 calc R . . C11 C 0.9813(4) 0.1969(4) 0.5772(2) 0.0182(9) Uani 1 1 d . . . C12 C 0.7193(4) 0.5173(4) 0.5745(2) 0.0218(9) Uani 1 1 d . . . H12A H 0.7177 0.5089 0.6244 0.026 Uiso 1 1 calc R . . C13 C 0.5908(4) 0.5279(5) 0.5597(2) 0.0290(11) Uani 1 1 d . . . H13A H 0.5703 0.4544 0.5858 0.043 Uiso 1 1 calc R . . H13B H 0.5916 0.5323 0.5113 0.043 Uiso 1 1 calc R . . H13C H 0.5289 0.6038 0.5726 0.043 Uiso 1 1 calc R . . C14 C 0.7467(5) 0.6379(4) 0.5385(2) 0.0320(11) Uani 1 1 d . . . H14A H 0.8308 0.6288 0.5450 0.048 Uiso 1 1 calc R . . H14B H 0.6875 0.7088 0.5574 0.048 Uiso 1 1 calc R . . H14C H 0.7391 0.6530 0.4900 0.048 Uiso 1 1 calc R . . C15 C 1.0590(4) 0.0863(4) 0.6253(2) 0.0225(9) Uani 1 1 d . . . H15A H 1.0142 0.0873 0.6717 0.027 Uiso 1 1 calc R . . C16 C 1.0775(5) -0.0399(4) 0.6081(2) 0.0309(11) Uani 1 1 d . . . H16A H 0.9968 -0.0456 0.6056 0.046 Uiso 1 1 calc R . . H16B H 1.1201 -0.1082 0.6433 0.046 Uiso 1 1 calc R . . H16C H 1.1273 -0.0466 0.5644 0.046 Uiso 1 1 calc R . . C17 C 1.1854(4) 0.0969(5) 0.6275(3) 0.0417(13) Uani 1 1 d . . . H17A H 1.1734 0.1727 0.6439 0.063 Uiso 1 1 calc R . . H17B H 1.2294 0.1016 0.5819 0.063 Uiso 1 1 calc R . . H17C H 1.2341 0.0233 0.6580 0.063 Uiso 1 1 calc R . . C18 C 0.8395(4) 0.0587(4) 0.8816(2) 0.0174(9) Uani 1 1 d . . . C19 C 0.8889(4) -0.0668(4) 0.8714(2) 0.0190(9) Uani 1 1 d . . . C20 C 0.8732(4) -0.1612(4) 0.9252(2) 0.0238(10) Uani 1 1 d . . . H20A H 0.9071 -0.2458 0.9197 0.029 Uiso 1 1 calc R . . C21 C 0.8092(4) -0.1346(4) 0.9865(2) 0.0269(10) Uani 1 1 d . . . H21A H 0.7963 -0.1999 1.0219 0.032 Uiso 1 1 calc R . . C22 C 0.7645(4) -0.0130(4) 0.9959(2) 0.0239(10) Uani 1 1 d . . . H22A H 0.7213 0.0047 1.0382 0.029 Uiso 1 1 calc R . . C23 C 0.7811(4) 0.0849(4) 0.9445(2) 0.0198(9) Uani 1 1 d . . . C24 C 0.9643(4) -0.0992(4) 0.8051(2) 0.0217(9) Uani 1 1 d . . . H24A H 0.9204 -0.0359 0.7670 0.026 Uiso 1 1 calc R . . C25 C 1.0950(4) -0.0914(4) 0.7990(2) 0.0260(10) Uani 1 1 d . . . H25A H 1.0884 -0.0058 0.7997 0.039 Uiso 1 1 calc R . . H25B H 1.1407 -0.1137 0.7563 0.039 Uiso 1 1 calc R . . H25C H 1.1389 -0.1497 0.8370 0.039 Uiso 1 1 calc R . . C26 C 0.9779(4) -0.2301(4) 0.7951(2) 0.0295(11) Uani 1 1 d . . . H26A H 0.8959 -0.2380 0.8002 0.044 Uiso 1 1 calc R . . H26B H 1.0280 -0.2945 0.8290 0.044 Uiso 1 1 calc R . . H26C H 1.0184 -0.2408 0.7497 0.044 Uiso 1 1 calc R . . C27 C 0.7367(4) 0.2157(4) 0.9617(2) 0.0239(10) Uani 1 1 d . . . H27A H 0.7670 0.2720 0.9229 0.029 Uiso 1 1 calc R . . C28 C 0.5963(4) 0.2724(5) 0.9719(3) 0.0347(12) Uani 1 1 d . . . H28A H 0.5615 0.2797 0.9304 0.052 Uiso 1 1 calc R . . H28B H 0.5731 0.3557 0.9824 0.052 Uiso 1 1 calc R . . H28C H 0.5641 0.2184 1.0094 0.052 Uiso 1 1 calc R . . C29 C 0.7933(5) 0.2110(5) 1.0251(2) 0.0328(11) Uani 1 1 d . . . H29A H 0.7778 0.2966 1.0303 0.049 Uiso 1 1 calc R . . H29B H 0.8826 0.1666 1.0200 0.049 Uiso 1 1 calc R . . H29C H 0.7554 0.1670 1.0652 0.049 Uiso 1 1 calc R . . C30 C 0.6725(4) 0.4895(4) 0.8055(3) 0.0311(11) Uani 1 1 d . . . H30A H 0.7373 0.4866 0.7675 0.047 Uiso 1 1 calc R . . H30B H 0.6907 0.4070 0.8356 0.047 Uiso 1 1 calc R . . H30C H 0.6696 0.5517 0.8307 0.047 Uiso 1 1 calc R . . C31 C 0.5053(5) 0.6847(4) 0.7104(3) 0.0328(11) Uani 1 1 d . . . H31A H 0.5732 0.6707 0.6741 0.049 Uiso 1 1 calc R . . H31B H 0.5090 0.7470 0.7334 0.049 Uiso 1 1 calc R . . H31C H 0.4262 0.7154 0.6910 0.049 Uiso 1 1 calc R . . C32 C 0.4001(5) 0.5746(5) 0.8457(3) 0.0368(12) Uani 1 1 d . . . H32A H 0.3173 0.6024 0.8309 0.055 Uiso 1 1 calc R . . H32B H 0.4099 0.6420 0.8621 0.055 Uiso 1 1 calc R . . H32C H 0.4107 0.5006 0.8823 0.055 Uiso 1 1 calc R . . C33 C 0.2764(4) 0.5954(4) 0.6814(3) 0.0327(11) Uani 1 1 d . . . H33A H 0.3209 0.6254 0.6393 0.049 Uiso 1 1 calc R . . H33B H 0.2628 0.6497 0.7136 0.049 Uiso 1 1 calc R . . H33C H 0.1966 0.5969 0.6720 0.049 Uiso 1 1 calc R . . C34 C 0.2666(4) 0.3821(5) 0.7945(2) 0.0350(12) Uani 1 1 d . . . H34A H 0.3054 0.2936 0.8147 0.052 Uiso 1 1 calc R . . H34B H 0.1869 0.3943 0.7799 0.052 Uiso 1 1 calc R . . H34C H 0.2536 0.4335 0.8281 0.052 Uiso 1 1 calc R . . C35 C 0.3826(4) 0.3362(4) 0.6551(2) 0.0233(10) Uani 1 1 d . . . H35A H 0.4179 0.3724 0.6113 0.035 Uiso 1 1 calc R . . H35B H 0.3001 0.3372 0.6507 0.035 Uiso 1 1 calc R . . H35C H 0.4360 0.2496 0.6698 0.035 Uiso 1 1 calc R . . C36 C 0.5278(4) 0.1123(5) 0.8635(2) 0.0295(11) Uani 1 1 d . . . H36A H 0.4670 0.0946 0.9006 0.044 Uiso 1 1 calc R . . H36B H 0.5005 0.2021 0.8437 0.044 Uiso 1 1 calc R . . H36C H 0.6080 0.0876 0.8808 0.044 Uiso 1 1 calc R . . C37 C 0.3818(4) 0.0379(5) 0.7832(2) 0.0286(10) Uani 1 1 d . . . H37A H 0.3857 -0.0273 0.7599 0.043 Uiso 1 1 calc R . . H37B H 0.3433 0.1206 0.7555 0.043 Uiso 1 1 calc R . . H37C H 0.3325 0.0293 0.8270 0.043 Uiso 1 1 calc R . . C38 C 0.6150(4) -0.1484(4) 0.8359(2) 0.0313(11) Uani 1 1 d . . . H38A H 0.5580 -0.1734 0.8733 0.047 Uiso 1 1 calc R . . H38B H 0.6924 -0.1609 0.8532 0.047 Uiso 1 1 calc R . . H38C H 0.6320 -0.1997 0.8018 0.047 Uiso 1 1 calc R . . C39 C 0.5214(4) 0.0065(4) 0.6233(2) 0.0277(10) Uani 1 1 d . . . H39A H 0.4534 0.0869 0.6200 0.041 Uiso 1 1 calc R . . H39B H 0.4947 -0.0581 0.6558 0.041 Uiso 1 1 calc R . . H39C H 0.5449 -0.0169 0.5788 0.041 Uiso 1 1 calc R . . C40 C 0.7791(4) -0.1381(4) 0.6583(2) 0.0295(11) Uani 1 1 d . . . H40A H 0.8548 -0.1359 0.6712 0.044 Uiso 1 1 calc R . . H40B H 0.7965 -0.1627 0.6142 0.044 Uiso 1 1 calc R . . H40C H 0.7494 -0.1989 0.6924 0.044 Uiso 1 1 calc R . . C41 C 0.7080(4) 0.1332(5) 0.5807(2) 0.0324(11) Uani 1 1 d . . . H41A H 0.7852 0.1389 0.5894 0.049 Uiso 1 1 calc R . . H41B H 0.6439 0.2162 0.5766 0.049 Uiso 1 1 calc R . . H41C H 0.7212 0.1031 0.5385 0.049 Uiso 1 1 calc R . . C51 C 0.8413(12) 0.5366(13) 0.0199(7) 0.057(3) Uiso 0.50 1 d P . . C52 C 0.9291(6) 0.5278(6) 0.0479(3) 0.0541(16) Uiso 1 1 d . . . C53 C 1.0023(12) 0.5204(12) 0.0762(6) 0.053(3) Uiso 0.50 1 d P . . C54 C 1.1549(8) 0.4823(8) 0.0521(4) 0.082(2) Uiso 1 1 d . . . C55 C 1.0636(12) 0.4950(12) 0.0204(7) 0.053(3) Uiso 0.50 1 d P . . 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 0.01207(13) 0.01397(13) 0.01683(13) -0.00315(8) -0.00374(8) -0.00269(8) Si1 0.0204(6) 0.0164(6) 0.0256(7) -0.0075(5) -0.0068(5) 0.0002(5) Si2 0.0137(6) 0.0219(6) 0.0259(7) -0.0083(5) -0.0037(5) -0.0015(5) Si3 0.0185(6) 0.0244(6) 0.0247(6) -0.0064(5) -0.0046(5) -0.0075(5) Si4 0.0176(6) 0.0197(6) 0.0253(6) -0.0079(5) -0.0014(5) -0.0069(5) N1 0.0135(17) 0.0163(17) 0.0150(17) -0.0030(14) -0.0042(14) -0.0022(14) N2 0.0176(18) 0.0121(17) 0.0164(18) -0.0004(14) -0.0041(14) -0.0010(14) N3 0.0147(17) 0.0153(17) 0.0184(18) -0.0032(14) -0.0038(14) -0.0006(14) N4 0.0158(18) 0.0212(19) 0.0230(19) -0.0071(15) -0.0045(15) -0.0042(15) C1 0.031(3) 0.033(3) 0.027(3) 0.000(2) -0.008(2) -0.019(2) C2 0.018(2) 0.015(2) 0.025(2) -0.0049(17) -0.0043(18) -0.0034(17) C3 0.021(2) 0.023(2) 0.017(2) -0.0062(18) -0.0057(17) -0.0089(18) C4 0.0089(19) 0.014(2) 0.022(2) -0.0065(17) -0.0048(16) 0.0010(16) C5 0.021(2) 0.027(2) 0.024(2) -0.0034(19) -0.0070(19) -0.0087(19) C6 0.016(2) 0.023(2) 0.020(2) -0.0041(17) -0.0030(17) -0.0128(18) C7 0.018(2) 0.019(2) 0.022(2) -0.0020(17) -0.0045(17) -0.0082(18) C8 0.025(2) 0.027(2) 0.021(2) -0.0012(19) -0.0070(19) -0.010(2) C9 0.027(2) 0.030(3) 0.019(2) -0.0035(19) -0.0036(19) -0.010(2) C10 0.019(2) 0.026(2) 0.023(2) -0.0080(19) -0.0020(18) -0.0069(18) C11 0.013(2) 0.023(2) 0.023(2) -0.0040(18) -0.0027(17) -0.0105(17) C12 0.022(2) 0.023(2) 0.018(2) -0.0002(18) -0.0060(18) -0.0057(19) C13 0.019(2) 0.036(3) 0.028(3) -0.006(2) -0.0053(19) -0.005(2) C14 0.034(3) 0.026(3) 0.036(3) -0.003(2) -0.007(2) -0.011(2) C15 0.019(2) 0.024(2) 0.023(2) -0.0036(18) -0.0022(18) -0.0056(18) C16 0.034(3) 0.025(3) 0.029(3) -0.005(2) -0.007(2) -0.003(2) C17 0.024(3) 0.044(3) 0.056(4) 0.003(3) -0.019(2) -0.010(2) C18 0.013(2) 0.019(2) 0.021(2) -0.0028(17) -0.0090(17) -0.0036(17) C19 0.017(2) 0.018(2) 0.024(2) -0.0049(18) -0.0088(18) -0.0039(17) C20 0.024(2) 0.017(2) 0.029(2) -0.0026(19) -0.0085(19) -0.0044(18) C21 0.032(3) 0.027(3) 0.022(2) 0.0011(19) -0.007(2) -0.012(2) C22 0.023(2) 0.032(3) 0.016(2) -0.0016(19) -0.0038(18) -0.009(2) C23 0.019(2) 0.020(2) 0.021(2) -0.0038(18) -0.0064(18) -0.0060(18) C24 0.021(2) 0.018(2) 0.024(2) -0.0044(18) -0.0075(18) -0.0011(18) C25 0.023(2) 0.026(2) 0.028(2) -0.010(2) -0.0058(19) -0.0035(19) C26 0.029(3) 0.025(2) 0.033(3) -0.011(2) -0.005(2) -0.005(2) C27 0.029(2) 0.020(2) 0.020(2) -0.0031(18) -0.0033(19) -0.0050(19) C28 0.034(3) 0.029(3) 0.038(3) -0.016(2) -0.002(2) -0.002(2) C29 0.044(3) 0.032(3) 0.025(3) -0.010(2) -0.004(2) -0.013(2) C30 0.032(3) 0.025(3) 0.039(3) -0.010(2) -0.016(2) -0.003(2) C31 0.037(3) 0.020(2) 0.040(3) -0.005(2) -0.014(2) -0.004(2) C32 0.033(3) 0.034(3) 0.039(3) -0.020(2) -0.002(2) 0.001(2) C33 0.021(2) 0.030(3) 0.044(3) -0.013(2) -0.014(2) 0.003(2) C34 0.026(3) 0.050(3) 0.032(3) -0.015(2) 0.006(2) -0.016(2) C35 0.019(2) 0.024(2) 0.027(2) -0.0051(19) -0.0058(19) -0.0048(18) C36 0.020(2) 0.038(3) 0.032(3) -0.011(2) -0.007(2) -0.007(2) C37 0.025(2) 0.034(3) 0.028(3) -0.004(2) -0.005(2) -0.012(2) C38 0.033(3) 0.026(3) 0.035(3) -0.003(2) -0.003(2) -0.012(2) C39 0.029(3) 0.029(3) 0.032(3) -0.011(2) -0.006(2) -0.013(2) C40 0.027(3) 0.027(3) 0.032(3) -0.010(2) -0.002(2) -0.005(2) C41 0.030(3) 0.032(3) 0.038(3) -0.007(2) 0.000(2) -0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N4 2.299(3) . ? Sm1 N3 2.324(3) . ? Sm1 N1 2.428(3) . ? Sm1 N2 2.503(3) . ? Sm1 Si3 3.3953(15) . ? Si1 N3 1.736(4) . ? Si1 C31 1.871(5) . ? Si1 C30 1.873(5) . ? Si1 C32 1.880(5) . ? Si2 N3 1.735(3) . ? Si2 C35 1.865(4) . ? Si2 C33 1.887(5) . ? Si2 C34 1.890(5) . ? Si3 N4 1.733(4) . ? Si3 C38 1.877(5) . ? Si3 C36 1.884(5) . ? Si3 C37 1.887(4) . ? Si4 N4 1.738(4) . ? Si4 C41 1.875(5) . ? Si4 C40 1.877(5) . ? Si4 C39 1.877(4) . ? N1 C2 1.362(5) . ? N1 C6 1.453(5) . ? N2 C4 1.334(5) . ? N2 C18 1.460(5) . ? C1 C2 1.521(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.401(6) . ? C3 C4 1.390(6) . ? C3 H3A 0.9500 . ? C4 C5 1.518(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.411(6) . ? C6 C11 1.424(6) . ? C7 C8 1.395(6) . ? C7 C12 1.518(6) . ? C8 C9 1.380(6) . ? C8 H8A 0.9500 . ? C9 C10 1.379(6) . ? C9 H9A 0.9500 . ? C10 C11 1.389(6) . ? C10 H10A 0.9500 . ? C11 C15 1.518(6) . ? C12 C14 1.538(6) . ? C12 C13 1.540(6) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.534(6) . ? C15 C17 1.537(6) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.395(6) . ? C18 C19 1.422(6) . ? C19 C20 1.392(6) . ? C19 C24 1.532(6) . ? C20 C21 1.385(6) . ? C20 H20A 0.9500 . ? C21 C22 1.375(6) . ? C21 H21A 0.9500 . ? C22 C23 1.396(6) . ? C22 H22A 0.9500 . ? C23 C27 1.535(6) . ? C24 C26 1.543(6) . ? C24 C25 1.544(6) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.524(6) . ? C27 C29 1.544(6) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C51 C52 1.225(14) . ? C51 C55 1.254(17) 2_765 ? C51 C54 1.536(15) 2_765 ? C52 C53 1.085(13) . ? C52 C55 1.471(14) 2_765 ? C52 C55 1.509(14) . ? C53 C55 1.275(17) . ? C53 C54 1.682(14) . ? C54 C55 1.293(14) . ? C54 C51 1.537(15) 2_765 ? C55 C51 1.254(17) 2_765 ? C55 C52 1.471(14) 2_765 ? C55 C55 1.79(3) 2_765 ? 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 Sm1 N3 107.06(12) . . ? N4 Sm1 N1 123.85(12) . . ? N3 Sm1 N1 109.44(12) . . ? N4 Sm1 N2 112.36(12) . . ? N3 Sm1 N2 125.14(11) . . ? N1 Sm1 N2 78.00(11) . . ? N4 Sm1 Si3 27.81(9) . . ? N3 Sm1 Si3 96.78(9) . . ? N1 Sm1 Si3 148.91(8) . . ? N2 Sm1 Si3 100.69(8) . . ? N3 Si1 C31 116.0(2) . . ? N3 Si1 C30 110.05(19) . . ? C31 Si1 C30 104.3(2) . . ? N3 Si1 C32 113.7(2) . . ? C31 Si1 C32 106.3(2) . . ? C30 Si1 C32 105.6(2) . . ? N3 Si2 C35 112.71(18) . . ? N3 Si2 C33 115.0(2) . . ? C35 Si2 C33 104.9(2) . . ? N3 Si2 C34 112.5(2) . . ? C35 Si2 C34 107.0(2) . . ? C33 Si2 C34 103.9(2) . . ? N4 Si3 C38 115.0(2) . . ? N4 Si3 C36 106.9(2) . . ? C38 Si3 C36 106.2(2) . . ? N4 Si3 C37 116.1(2) . . ? C38 Si3 C37 104.8(2) . . ? C36 Si3 C37 107.2(2) . . ? N4 Si3 Sm1 38.24(12) . . ? C38 Si3 Sm1 126.42(16) . . ? C36 Si3 Sm1 68.64(16) . . ? C37 Si3 Sm1 128.12(16) . . ? N4 Si4 C41 109.4(2) . . ? N4 Si4 C40 112.4(2) . . ? C41 Si4 C40 109.1(2) . . ? N4 Si4 C39 116.18(19) . . ? C41 Si4 C39 104.0(2) . . ? C40 Si4 C39 105.2(2) . . ? C2 N1 C6 114.3(3) . . ? C2 N1 Sm1 122.1(3) . . ? C6 N1 Sm1 123.3(2) . . ? C4 N2 C18 117.7(3) . . ? C4 N2 Sm1 123.9(3) . . ? C18 N2 Sm1 118.3(2) . . ? Si2 N3 Si1 115.70(19) . . ? Si2 N3 Sm1 126.16(18) . . ? Si1 N3 Sm1 117.82(17) . . ? Si3 N4 Si4 120.7(2) . . ? Si3 N4 Sm1 113.95(17) . . ? Si4 N4 Sm1 125.28(18) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 125.0(4) . . ? N1 C2 C1 119.2(4) . . ? C3 C2 C1 115.8(4) . . ? C4 C3 C2 132.0(4) . . ? C4 C3 H3A 114.0 . . ? C2 C3 H3A 114.0 . . ? N2 C4 C3 124.9(4) . . ? N2 C4 C5 121.2(4) . . ? C3 C4 C5 113.9(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 120.1(4) . . ? C7 C6 N1 122.2(4) . . ? C11 C6 N1 117.7(4) . . ? C8 C7 C6 118.3(4) . . ? C8 C7 C12 118.5(4) . . ? C6 C7 C12 123.1(4) . . ? C9 C8 C7 121.8(4) . . ? C9 C8 H8A 119.1 . . ? C7 C8 H8A 119.1 . . ? C10 C9 C8 119.6(4) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C9 C10 C11 121.5(4) . . ? C9 C10 H10A 119.2 . . ? C11 C10 H10A 119.2 . . ? C10 C11 C6 118.6(4) . . ? C10 C11 C15 119.3(4) . . ? C6 C11 C15 122.1(4) . . ? C7 C12 C14 112.0(4) . . ? C7 C12 C13 110.7(4) . . ? C14 C12 C13 109.4(4) . . ? C7 C12 H12A 108.2 . . ? C14 C12 H12A 108.2 . . ? C13 C12 H12A 108.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 112.7(4) . . ? C11 C15 C17 111.5(4) . . ? C16 C15 C17 109.6(4) . . ? C11 C15 H15A 107.6 . . ? C16 C15 H15A 107.6 . . ? C17 C15 H15A 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.6(4) . . ? C23 C18 N2 121.3(4) . . ? C19 C18 N2 118.0(4) . . ? C20 C19 C18 117.9(4) . . ? C20 C19 C24 120.5(4) . . ? C18 C19 C24 121.5(4) . . ? C21 C20 C19 121.5(4) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C22 C21 C20 119.6(4) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? C21 C22 C23 121.3(4) . . ? C21 C22 H22A 119.3 . . ? C23 C22 H22A 119.3 . . ? C18 C23 C22 118.8(4) . . ? C18 C23 C27 123.8(4) . . ? C22 C23 C27 117.4(4) . . ? C19 C24 C26 113.7(4) . . ? C19 C24 C25 111.8(3) . . ? C26 C24 C25 108.1(4) . . ? C19 C24 H24A 107.6 . . ? C26 C24 H24A 107.6 . . ? C25 C24 H24A 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C23 112.9(4) . . ? C28 C27 C29 110.0(4) . . ? C23 C27 C29 110.3(4) . . ? C28 C27 H27A 107.8 . . ? C23 C27 H27A 107.8 . . ? C29 C27 H27A 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si3 C36 H36A 109.5 . . ? Si3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si3 C37 H37A 109.5 . . ? Si3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si3 C38 H38A 109.5 . . ? Si3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si4 C39 H39A 109.5 . . ? Si4 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si4 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si4 C40 H40A 109.5 . . ? Si4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si4 C41 H41A 109.5 . . ? Si4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C52 C51 C55 72.8(10) . 2_765 ? C52 C51 C54 126.8(11) . 2_765 ? C55 C51 C54 54.1(8) 2_765 2_765 ? C53 C52 C51 175.7(12) . . ? C53 C52 C55 129.7(10) . 2_765 ? C51 C52 C55 54.5(8) . 2_765 ? C53 C52 C55 56.0(8) . . ? C51 C52 C55 128.2(10) . . ? C55 C52 C55 73.7(9) 2_765 . ? C52 C53 C55 79.1(10) . . ? C52 C53 C54 128.6(11) . . ? C55 C53 C54 49.5(7) . . ? C55 C54 C51 51.7(8) . 2_765 ? C55 C54 C53 48.6(8) . . ? C51 C54 C53 100.4(8) 2_765 . ? C51 C55 C53 156.0(14) 2_765 . ? C51 C55 C54 74.2(10) 2_765 . ? C53 C55 C54 81.8(10) . . ? C51 C55 C52 52.7(8) 2_765 2_765 ? C53 C55 C52 151.1(12) . 2_765 ? C54 C55 C52 126.9(11) . 2_765 ? C51 C55 C52 159.0(13) 2_765 . ? C53 C55 C52 44.9(7) . . ? C54 C55 C52 126.7(11) . . ? C52 C55 C52 106.3(9) 2_765 . ? C51 C55 C55 106.8(13) 2_765 2_765 ? C53 C55 C55 97.0(12) . 2_765 ? C54 C55 C55 176.8(15) . 2_765 ? C52 C55 C55 54.1(7) 2_765 2_765 ? C52 C55 C55 52.2(7) . 2_765 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Sm1 Si3 N4 114.1(2) . . . . ? N1 Sm1 Si3 N4 -33.7(2) . . . . ? N2 Sm1 Si3 N4 -118.2(2) . . . . ? N4 Sm1 Si3 C38 84.9(3) . . . . ? N3 Sm1 Si3 C38 -161.0(2) . . . . ? N1 Sm1 Si3 C38 51.2(3) . . . . ? N2 Sm1 Si3 C38 -33.3(2) . . . . ? N4 Sm1 Si3 C36 179.7(2) . . . . ? N3 Sm1 Si3 C36 -66.19(18) . . . . ? N1 Sm1 Si3 C36 146.0(2) . . . . ? N2 Sm1 Si3 C36 61.57(18) . . . . ? N4 Sm1 Si3 C37 -84.7(3) . . . . ? N3 Sm1 Si3 C37 29.4(2) . . . . ? N1 Sm1 Si3 C37 -118.4(2) . . . . ? N2 Sm1 Si3 C37 157.1(2) . . . . ? N4 Sm1 N1 C2 -145.5(3) . . . . ? N3 Sm1 N1 C2 86.8(3) . . . . ? N2 Sm1 N1 C2 -36.5(3) . . . . ? Si3 Sm1 N1 C2 -127.3(3) . . . . ? N4 Sm1 N1 C6 40.6(3) . . . . ? N3 Sm1 N1 C6 -87.1(3) . . . . ? N2 Sm1 N1 C6 149.6(3) . . . . ? Si3 Sm1 N1 C6 58.8(4) . . . . ? N4 Sm1 N2 C4 149.4(3) . . . . ? N3 Sm1 N2 C4 -78.0(3) . . . . ? N1 Sm1 N2 C4 27.5(3) . . . . ? Si3 Sm1 N2 C4 175.8(3) . . . . ? N4 Sm1 N2 C18 -34.8(3) . . . . ? N3 Sm1 N2 C18 97.9(3) . . . . ? N1 Sm1 N2 C18 -156.7(3) . . . . ? Si3 Sm1 N2 C18 -8.4(3) . . . . ? C35 Si2 N3 Si1 156.5(2) . . . . ? C33 Si2 N3 Si1 36.3(3) . . . . ? C34 Si2 N3 Si1 -82.4(3) . . . . ? C35 Si2 N3 Sm1 -30.2(3) . . . . ? C33 Si2 N3 Sm1 -150.4(2) . . . . ? C34 Si2 N3 Sm1 90.9(3) . . . . ? C31 Si1 N3 Si2 -70.7(3) . . . . ? C30 Si1 N3 Si2 171.2(2) . . . . ? C32 Si1 N3 Si2 53.0(3) . . . . ? C31 Si1 N3 Sm1 115.4(2) . . . . ? C30 Si1 N3 Sm1 -2.7(3) . . . . ? C32 Si1 N3 Sm1 -120.9(2) . . . . ? N4 Sm1 N3 Si2 -10.1(2) . . . . ? N1 Sm1 N3 Si2 126.5(2) . . . . ? N2 Sm1 N3 Si2 -144.74(18) . . . . ? Si3 Sm1 N3 Si2 -36.6(2) . . . . ? N4 Sm1 N3 Si1 163.09(18) . . . . ? N1 Sm1 N3 Si1 -60.3(2) . . . . ? N2 Sm1 N3 Si1 28.4(2) . . . . ? Si3 Sm1 N3 Si1 136.63(17) . . . . ? C38 Si3 N4 Si4 65.6(3) . . . . ? C36 Si3 N4 Si4 -176.8(2) . . . . ? C37 Si3 N4 Si4 -57.3(3) . . . . ? Sm1 Si3 N4 Si4 -176.5(3) . . . . ? C38 Si3 N4 Sm1 -117.9(2) . . . . ? C36 Si3 N4 Sm1 -0.3(2) . . . . ? C37 Si3 N4 Sm1 119.3(2) . . . . ? C41 Si4 N4 Si3 162.2(2) . . . . ? C40 Si4 N4 Si3 -76.4(3) . . . . ? C39 Si4 N4 Si3 44.9(3) . . . . ? C41 Si4 N4 Sm1 -13.9(3) . . . . ? C40 Si4 N4 Sm1 107.4(2) . . . . ? C39 Si4 N4 Sm1 -131.3(2) . . . . ? N3 Sm1 N4 Si3 -71.5(2) . . . . ? N1 Sm1 N4 Si3 159.80(15) . . . . ? N2 Sm1 N4 Si3 69.5(2) . . . . ? N3 Sm1 N4 Si4 104.8(2) . . . . ? N1 Sm1 N4 Si4 -23.8(3) . . . . ? N2 Sm1 N4 Si4 -114.1(2) . . . . ? Si3 Sm1 N4 Si4 176.4(4) . . . . ? C6 N1 C2 C3 -156.3(4) . . . . ? Sm1 N1 C2 C3 29.3(5) . . . . ? C6 N1 C2 C1 22.2(5) . . . . ? Sm1 N1 C2 C1 -152.3(3) . . . . ? N1 C2 C3 C4 8.6(7) . . . . ? C1 C2 C3 C4 -169.9(4) . . . . ? C18 N2 C4 C3 175.5(4) . . . . ? Sm1 N2 C4 C3 -8.6(5) . . . . ? C18 N2 C4 C5 -4.6(5) . . . . ? Sm1 N2 C4 C5 171.3(3) . . . . ? C2 C3 C4 N2 -20.3(7) . . . . ? C2 C3 C4 C5 159.8(4) . . . . ? C2 N1 C6 C7 -96.0(4) . . . . ? Sm1 N1 C6 C7 78.4(4) . . . . ? C2 N1 C6 C11 84.9(4) . . . . ? Sm1 N1 C6 C11 -100.7(4) . . . . ? C11 C6 C7 C8 2.0(6) . . . . ? N1 C6 C7 C8 -177.1(4) . . . . ? C11 C6 C7 C12 -176.6(4) . . . . ? N1 C6 C7 C12 4.3(6) . . . . ? C6 C7 C8 C9 -1.2(6) . . . . ? C12 C7 C8 C9 177.4(4) . . . . ? C7 C8 C9 C10 -0.5(7) . . . . ? C8 C9 C10 C11 1.5(7) . . . . ? C9 C10 C11 C6 -0.7(6) . . . . ? C9 C10 C11 C15 179.7(4) . . . . ? C7 C6 C11 C10 -1.1(6) . . . . ? N1 C6 C11 C10 178.1(3) . . . . ? C7 C6 C11 C15 178.5(4) . . . . ? N1 C6 C11 C15 -2.4(6) . . . . ? C8 C7 C12 C14 -55.4(5) . . . . ? C6 C7 C12 C14 123.2(4) . . . . ? C8 C7 C12 C13 67.0(5) . . . . ? C6 C7 C12 C13 -114.4(4) . . . . ? C10 C11 C15 C16 -44.4(5) . . . . ? C6 C11 C15 C16 136.0(4) . . . . ? C10 C11 C15 C17 79.3(5) . . . . ? C6 C11 C15 C17 -100.3(5) . . . . ? C4 N2 C18 C23 79.8(5) . . . . ? Sm1 N2 C18 C23 -96.4(4) . . . . ? C4 N2 C18 C19 -102.5(4) . . . . ? Sm1 N2 C18 C19 81.4(4) . . . . ? C23 C18 C19 C20 2.3(6) . . . . ? N2 C18 C19 C20 -175.5(4) . . . . ? C23 C18 C19 C24 -174.0(4) . . . . ? N2 C18 C19 C24 8.2(6) . . . . ? C18 C19 C20 C21 1.3(6) . . . . ? C24 C19 C20 C21 177.7(4) . . . . ? C19 C20 C21 C22 -2.8(7) . . . . ? C20 C21 C22 C23 0.6(7) . . . . ? C19 C18 C23 C22 -4.4(6) . . . . ? N2 C18 C23 C22 173.3(4) . . . . ? C19 C18 C23 C27 173.8(4) . . . . ? N2 C18 C23 C27 -8.5(6) . . . . ? C21 C22 C23 C18 3.0(7) . . . . ? C21 C22 C23 C27 -175.4(4) . . . . ? C20 C19 C24 C26 20.4(6) . . . . ? C18 C19 C24 C26 -163.4(4) . . . . ? C20 C19 C24 C25 -102.4(5) . . . . ? C18 C19 C24 C25 73.8(5) . . . . ? C18 C23 C27 C28 111.6(5) . . . . ? C22 C23 C27 C28 -70.1(5) . . . . ? C18 C23 C27 C29 -124.8(4) . . . . ? C22 C23 C27 C29 53.5(5) . . . . ? C55 C51 C52 C53 -168(16) 2_765 . . . ? C54 C51 C52 C53 -170(15) 2_765 . . . ? C54 C51 C52 C55 -2.2(11) 2_765 . . 2_765 ? C55 C51 C52 C55 1.4(16) 2_765 . . . ? C54 C51 C52 C55 -0.8(19) 2_765 . . . ? C51 C52 C53 C55 170(16) . . . . ? C55 C52 C53 C55 2.6(17) 2_765 . . . ? C51 C52 C53 C54 169(15) . . . . ? C55 C52 C53 C54 1(2) 2_765 . . . ? C55 C52 C53 C54 -1.3(11) . . . . ? C52 C53 C54 C55 1.7(14) . . . . ? C52 C53 C54 C51 0.7(16) . . . 2_765 ? C55 C53 C54 C51 -0.9(10) . . . 2_765 ? C52 C53 C55 C51 -176(3) . . . 2_765 ? C54 C53 C55 C51 3(3) . . . 2_765 ? C52 C53 C55 C54 -178.7(11) . . . . ? C52 C53 C55 C52 -4(3) . . . 2_765 ? C54 C53 C55 C52 174(3) . . . 2_765 ? C54 C53 C55 C52 178.7(11) . . . . ? C52 C53 C55 C55 -1.7(11) . . . 2_765 ? C54 C53 C55 C55 177.0(15) . . . 2_765 ? C53 C54 C55 C51 -178.8(13) . . . 2_765 ? C51 C54 C55 C53 178.8(13) 2_765 . . . ? C51 C54 C55 C52 2.2(10) 2_765 . . 2_765 ? C53 C54 C55 C52 -176.7(17) . . . 2_765 ? C51 C54 C55 C52 177.7(17) 2_765 . . . ? C53 C54 C55 C52 -1.2(10) . . . . ? C51 C54 C55 C55 109(27) 2_765 . . 2_765 ? C53 C54 C55 C55 -69(27) . . . 2_765 ? C53 C52 C55 C51 175(4) . . . 2_765 ? C51 C52 C55 C51 -4(4) . . . 2_765 ? C55 C52 C55 C51 -2(3) 2_765 . . 2_765 ? C51 C52 C55 C53 -179.1(15) . . . . ? C55 C52 C55 C53 -177.9(14) 2_765 . . . ? C53 C52 C55 C54 1.6(13) . . . . ? C51 C52 C55 C54 -177.4(13) . . . . ? C55 C52 C55 C54 -176.3(18) 2_765 . . . ? C53 C52 C55 C52 177.9(14) . . . 2_765 ? C51 C52 C55 C52 -1.2(14) . . . 2_765 ? C55 C52 C55 C52 0.0 2_765 . . 2_765 ? C53 C52 C55 C55 177.9(14) . . . 2_765 ? C51 C52 C55 C55 -1.2(14) . . . 2_765 ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 25.55 _diffrn_measured_fraction_theta_full 0.862 _refine_diff_density_max 1.451 _refine_diff_density_min -2.273 _refine_diff_density_rms 0.120 #============================================ data_NACSmCpCl _database_code_depnum_ccdc_archive 'CCDC 244221' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H56 Cl N2 Sm' _chemical_formula_sum 'C39 H56 Cl N2 Sm' _chemical_formula_weight 738.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6492(4) _cell_length_b 12.0177(5) _cell_length_c 15.7839(6) _cell_angle_alpha 104.1520(10) _cell_angle_beta 97.11 _cell_angle_gamma 106.8410(10) _cell_volume 1832.99(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2678 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.40 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 766 _exptl_absorpt_coefficient_mu 1.702 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6292 _exptl_absorpt_correction_T_max 0.7843 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method /w\2/q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9258 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.40 _reflns_number_total 5844 _reflns_number_gt 5444 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.052d' _computing_cell_refinement 'Bruker SAINT v5.10' _computing_data_reduction 'Bruker SAINT v5.10' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One of the iso-propyl groups exhibited some positional disorder and was modeled with carbons in two appropriate locations. ; _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^)+(0.0477P)^2^+1.0160P] 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_extinction_coef ? _refine_ls_number_reflns 5844 _refine_ls_number_parameters 402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.804631(15) 0.787619(14) 0.738804(10) 0.01766(9) Uani 1 1 d . . . N1 N 0.6977(3) 0.7481(3) 0.8571(2) 0.0219(6) Uani 1 1 d . . . N2 N 0.7512(3) 0.9699(3) 0.78006(19) 0.0194(6) Uani 1 1 d . . . C1 C 0.7568(5) 0.8237(4) 1.0234(3) 0.0339(9) Uani 1 1 d . . . H1A H 0.7570 0.7411 1.0198 0.051 Uiso 1 1 calc R . . H1B H 0.6777 0.8351 1.0451 0.051 Uiso 1 1 calc R . . H1C H 0.8382 0.8830 1.0648 0.051 Uiso 1 1 calc R . . C2 C 0.7530(4) 0.8419(3) 0.9312(3) 0.0247(8) Uani 1 1 d . . . C3 C 0.8095(4) 0.9647(3) 0.9326(3) 0.0252(8) Uani 1 1 d . . . H3A H 0.8676 1.0161 0.9877 0.030 Uiso 1 1 calc R . . C4 C 0.7955(3) 1.0248(3) 0.8676(2) 0.0215(8) Uani 1 1 d . . . C5 C 0.8343(4) 1.1620(3) 0.9041(3) 0.0321(9) Uani 1 1 d . . . H5A H 0.7664 1.1891 0.8755 0.048 Uiso 1 1 calc R . . H5B H 0.9216 1.2007 0.8915 0.048 Uiso 1 1 calc R . . H5C H 0.8400 1.1848 0.9688 0.048 Uiso 1 1 calc R . . C6 C 0.6212(4) 0.6327(3) 0.8654(2) 0.0231(8) Uani 1 1 d . A . C7 C 0.6821(4) 0.5470(4) 0.8755(3) 0.0360(10) Uani 1 1 d . . . C8 C 0.6050(4) 0.4350(3) 0.8810(3) 0.0332(9) Uani 1 1 d . A . H8A H 0.6469 0.3771 0.8883 0.040 Uiso 1 1 calc R . . C9 C 0.4693(4) 0.4064(4) 0.8762(3) 0.0384(10) Uani 1 1 d . . . H9A H 0.4175 0.3293 0.8797 0.046 Uiso 1 1 calc R A . C10 C 0.4087(4) 0.4917(4) 0.8660(3) 0.0367(10) Uani 1 1 d . A . H10A H 0.3150 0.4724 0.8638 0.044 Uiso 1 1 calc R . . C11 C 0.4817(4) 0.6047(3) 0.8590(2) 0.0242(8) Uani 1 1 d . . . C12 C 0.8215(8) 0.5581(7) 0.8476(6) 0.0317(18) Uiso 0.50 1 d P A 1 H12B H 0.8253 0.5966 0.7981 0.038 Uiso 0.50 1 calc PR A 1 C13 C 0.9284(9) 0.6443(8) 0.9276(6) 0.042(2) Uiso 0.50 1 d P A 1 H13D H 1.0173 0.6501 0.9146 0.063 Uiso 0.50 1 calc PR A 1 H13E H 0.9187 0.6137 0.9794 0.063 Uiso 0.50 1 calc PR A 1 H13F H 0.9185 0.7250 0.9408 0.063 Uiso 0.50 1 calc PR A 1 C14 C 0.8508(10) 0.4414(9) 0.8170(7) 0.041(2) Uiso 0.50 1 d P A 1 H14D H 0.9347 0.4574 0.7953 0.061 Uiso 0.50 1 calc PR A 1 H14E H 0.7772 0.3830 0.7687 0.061 Uiso 0.50 1 calc PR A 1 H14F H 0.8598 0.4076 0.8672 0.061 Uiso 0.50 1 calc PR A 1 C12A C 0.8382(7) 0.5846(7) 0.9056(5) 0.0210(15) Uiso 0.50 1 d P A 2 H12A H 0.8778 0.6748 0.9188 0.025 Uiso 0.50 1 calc PR A 2 C13A C 0.8922(9) 0.5485(9) 0.9852(6) 0.042(2) Uiso 0.50 1 d P A 2 H13A H 0.9905 0.5756 0.9962 0.063 Uiso 0.50 1 calc PR A 2 H13B H 0.8571 0.4599 0.9723 0.063 Uiso 0.50 1 calc PR A 2 H13C H 0.8639 0.5869 1.0383 0.063 Uiso 0.50 1 calc PR A 2 C14A C 0.8838(9) 0.5234(8) 0.8227(6) 0.0359(19) Uiso 0.50 1 d P A 2 H14A H 0.9816 0.5448 0.8360 0.054 Uiso 0.50 1 calc PR A 2 H14B H 0.8565 0.5517 0.7725 0.054 Uiso 0.50 1 calc PR A 2 H14C H 0.8421 0.4349 0.8070 0.054 Uiso 0.50 1 calc PR A 2 C15 C 0.4094(4) 0.6931(4) 0.8447(3) 0.0309(9) Uani 1 1 d . A . H15A H 0.4676 0.7514 0.8185 0.037 Uiso 1 1 calc R . . C16 C 0.3918(6) 0.7672(5) 0.9323(4) 0.0623(15) Uani 1 1 d . . . H16A H 0.4798 0.8216 0.9684 0.093 Uiso 1 1 calc R A . H16B H 0.3488 0.7123 0.9650 0.093 Uiso 1 1 calc R . . H16C H 0.3355 0.8154 0.9203 0.093 Uiso 1 1 calc R . . C17 C 0.2742(4) 0.6299(5) 0.7783(4) 0.0469(12) Uani 1 1 d . . . H17A H 0.2393 0.6913 0.7635 0.070 Uiso 1 1 calc R A . H17B H 0.2104 0.5800 0.8052 0.070 Uiso 1 1 calc R . . H17C H 0.2864 0.5778 0.7237 0.070 Uiso 1 1 calc R . . C18 C 0.7286(3) 1.0414(3) 0.7223(2) 0.0198(7) Uani 1 1 d . . . C19 C 0.5955(4) 1.0365(3) 0.6930(2) 0.0246(8) Uani 1 1 d . . . C20 C 0.5752(4) 1.1016(4) 0.6338(3) 0.0311(9) Uani 1 1 d . . . H20A H 0.4869 1.1006 0.6138 0.037 Uiso 1 1 calc R . . C21 C 0.6798(4) 1.1678(4) 0.6034(3) 0.0332(9) Uani 1 1 d . . . H21A H 0.6626 1.2101 0.5622 0.040 Uiso 1 1 calc R . . C22 C 0.8093(4) 1.1723(3) 0.6327(3) 0.0293(9) Uani 1 1 d . . . H22A H 0.8807 1.2179 0.6115 0.035 Uiso 1 1 calc R . . C23 C 0.8366(4) 1.1102(3) 0.6935(2) 0.0236(8) Uani 1 1 d . . . C24 C 0.4798(4) 0.9667(4) 0.7272(3) 0.0280(8) Uani 1 1 d . . . H24A H 0.4991 0.8932 0.7359 0.034 Uiso 1 1 calc R . . C25 C 0.4692(5) 1.0409(4) 0.8181(3) 0.0433(11) Uani 1 1 d . . . H25A H 0.5503 1.0572 0.8625 0.065 Uiso 1 1 calc R . . H25B H 0.3906 0.9948 0.8365 0.065 Uiso 1 1 calc R . . H25C H 0.4597 1.1181 0.8136 0.065 Uiso 1 1 calc R . . C26 C 0.3441(4) 0.9219(4) 0.6622(3) 0.0399(11) Uani 1 1 d . . . H26A H 0.3524 0.8787 0.6030 0.060 Uiso 1 1 calc R . . H26B H 0.3161 0.9917 0.6583 0.060 Uiso 1 1 calc R . . H26C H 0.2771 0.8667 0.6836 0.060 Uiso 1 1 calc R . . C27 C 0.9811(4) 1.1178(4) 0.7243(3) 0.0289(9) Uani 1 1 d . . . H27A H 0.9845 1.0861 0.7772 0.035 Uiso 1 1 calc R . . C28 C 1.0791(5) 1.2496(4) 0.7539(4) 0.0495(12) Uani 1 1 d . . . H28A H 1.0493 1.2999 0.8006 0.074 Uiso 1 1 calc R . . H28B H 1.0810 1.2819 0.7026 0.074 Uiso 1 1 calc R . . H28C H 1.1692 1.2507 0.7774 0.074 Uiso 1 1 calc R . . C29 C 1.0264(4) 1.0380(4) 0.6520(3) 0.0418(11) Uani 1 1 d . . . H29A H 0.9661 0.9537 0.6358 0.063 Uiso 1 1 calc R . . H29B H 1.1181 1.0419 0.6745 0.063 Uiso 1 1 calc R . . H29C H 1.0243 1.0671 0.5992 0.063 Uiso 1 1 calc R . . C30 C 0.6085(4) 0.6608(3) 0.5931(2) 0.0264(8) Uani 1 1 d . . . C31 C 0.7081(4) 0.7336(3) 0.5599(2) 0.0281(8) Uani 1 1 d . . . C32 C 0.8199(4) 0.6904(3) 0.5647(2) 0.0257(8) Uani 1 1 d . . . C33 C 0.7861(4) 0.5903(3) 0.6002(2) 0.0249(8) Uani 1 1 d . . . C34 C 0.6555(4) 0.5714(3) 0.6179(2) 0.0268(8) Uani 1 1 d . . . C35 C 0.4684(4) 0.6659(4) 0.5935(3) 0.0409(11) Uani 1 1 d . . . H35A H 0.4029 0.5907 0.5524 0.061 Uiso 1 1 calc R . . H35B H 0.4600 0.7356 0.5744 0.061 Uiso 1 1 calc R . . H35C H 0.4514 0.6748 0.6540 0.061 Uiso 1 1 calc R . . C36 C 0.6938(5) 0.8283(4) 0.5147(3) 0.0387(10) Uani 1 1 d . . . H36A H 0.6653 0.7903 0.4499 0.058 Uiso 1 1 calc R . . H36B H 0.7803 0.8936 0.5282 0.058 Uiso 1 1 calc R . . H36C H 0.6267 0.8622 0.5367 0.058 Uiso 1 1 calc R . . C37 C 0.9428(5) 0.7279(4) 0.5270(3) 0.0387(10) Uani 1 1 d . . . H37A H 0.9413 0.6604 0.4768 0.058 Uiso 1 1 calc R . . H37B H 1.0231 0.7492 0.5735 0.058 Uiso 1 1 calc R . . H37C H 0.9443 0.7986 0.5062 0.058 Uiso 1 1 calc R . . C38 C 0.8719(4) 0.5105(4) 0.6051(3) 0.0349(9) Uani 1 1 d . . . H38A H 0.8763 0.4684 0.5445 0.052 Uiso 1 1 calc R . . H38C H 0.8324 0.4504 0.6349 0.052 Uiso 1 1 calc R . . H38D H 0.9626 0.5609 0.6389 0.052 Uiso 1 1 calc R . . C39 C 0.5706(4) 0.4662(4) 0.6443(3) 0.0342(9) Uani 1 1 d . . . H39C H 0.4996 0.4114 0.5930 0.051 Uiso 1 1 calc R . . H39D H 0.5301 0.4972 0.6934 0.051 Uiso 1 1 calc R . . H39A H 0.6270 0.4217 0.6637 0.051 Uiso 1 1 calc R . . Cl1 Cl 1.06094(9) 0.84318(10) 0.80032(7) 0.0364(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01573(11) 0.02117(13) 0.01793(12) 0.00541(8) 0.00284(8) 0.00945(8) N1 0.0208(14) 0.0236(16) 0.0264(17) 0.0124(14) 0.0057(13) 0.0103(13) N2 0.0177(13) 0.0193(15) 0.0230(16) 0.0071(13) 0.0054(12) 0.0076(12) C1 0.053(3) 0.026(2) 0.026(2) 0.0121(17) 0.0155(19) 0.0125(19) C2 0.0239(18) 0.027(2) 0.028(2) 0.0108(17) 0.0081(16) 0.0131(16) C3 0.0268(18) 0.0215(19) 0.025(2) 0.0062(16) 0.0014(16) 0.0063(15) C4 0.0211(17) 0.0206(19) 0.0241(19) 0.0073(15) 0.0076(15) 0.0072(14) C5 0.046(2) 0.022(2) 0.025(2) 0.0062(16) 0.0069(18) 0.0077(18) C6 0.0264(18) 0.0185(18) 0.0223(19) 0.0064(15) 0.0065(15) 0.0034(15) C7 0.027(2) 0.028(2) 0.061(3) 0.024(2) 0.0139(19) 0.0110(17) C8 0.039(2) 0.024(2) 0.043(2) 0.0184(19) 0.0103(19) 0.0129(18) C9 0.039(2) 0.026(2) 0.047(3) 0.016(2) 0.010(2) 0.0012(18) C10 0.027(2) 0.034(2) 0.051(3) 0.018(2) 0.0142(19) 0.0057(18) C11 0.0264(18) 0.026(2) 0.0205(18) 0.0062(16) 0.0080(15) 0.0087(16) C15 0.0257(19) 0.034(2) 0.038(2) 0.0154(19) 0.0105(17) 0.0118(17) C16 0.089(4) 0.064(4) 0.048(3) 0.008(3) 0.017(3) 0.053(3) C17 0.024(2) 0.054(3) 0.069(3) 0.027(3) 0.010(2) 0.015(2) C18 0.0234(17) 0.0192(18) 0.0183(17) 0.0042(14) 0.0044(14) 0.0103(14) C19 0.0277(19) 0.0252(19) 0.0240(19) 0.0053(16) 0.0057(16) 0.0150(16) C20 0.033(2) 0.037(2) 0.032(2) 0.0136(18) 0.0058(17) 0.0214(18) C21 0.046(2) 0.033(2) 0.031(2) 0.0176(18) 0.0090(19) 0.0218(19) C22 0.036(2) 0.030(2) 0.027(2) 0.0157(17) 0.0116(17) 0.0107(17) C23 0.0253(18) 0.0220(19) 0.0243(19) 0.0066(16) 0.0052(15) 0.0092(15) C24 0.0234(18) 0.031(2) 0.033(2) 0.0073(17) 0.0087(16) 0.0149(16) C25 0.040(2) 0.049(3) 0.042(3) 0.010(2) 0.021(2) 0.015(2) C26 0.023(2) 0.052(3) 0.048(3) 0.017(2) 0.0063(19) 0.017(2) C27 0.0208(18) 0.034(2) 0.034(2) 0.0176(18) 0.0082(16) 0.0059(16) C28 0.037(2) 0.044(3) 0.059(3) 0.025(2) 0.002(2) -0.004(2) C29 0.030(2) 0.058(3) 0.045(3) 0.018(2) 0.013(2) 0.022(2) C30 0.0253(18) 0.031(2) 0.0178(18) -0.0018(16) -0.0031(15) 0.0128(16) C31 0.038(2) 0.030(2) 0.0184(19) 0.0050(16) 0.0008(16) 0.0177(17) C32 0.035(2) 0.028(2) 0.0191(18) 0.0088(16) 0.0088(16) 0.0151(17) C33 0.032(2) 0.026(2) 0.0195(18) 0.0033(15) 0.0062(16) 0.0173(16) C34 0.031(2) 0.024(2) 0.0187(19) -0.0006(16) 0.0023(16) 0.0069(16) C35 0.031(2) 0.056(3) 0.031(2) -0.003(2) -0.0042(18) 0.024(2) C36 0.054(3) 0.036(2) 0.026(2) 0.0069(19) -0.0039(19) 0.021(2) C37 0.054(3) 0.039(2) 0.038(2) 0.017(2) 0.029(2) 0.026(2) C38 0.040(2) 0.037(2) 0.040(2) 0.016(2) 0.0142(19) 0.025(2) C39 0.036(2) 0.027(2) 0.027(2) -0.0012(17) 0.0071(18) -0.0001(17) Cl1 0.0185(4) 0.0485(6) 0.0429(6) 0.0111(5) 0.0021(4) 0.0157(4) _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 N1 2.378(3) . ? Sm1 N2 2.380(3) . ? Sm1 Cl1 2.6095(9) . ? Sm1 C30 2.688(4) . ? Sm1 C34 2.711(4) . ? Sm1 C31 2.729(4) . ? Sm1 C33 2.745(4) . ? Sm1 C32 2.755(4) . ? N1 C2 1.337(5) . ? N1 C6 1.437(4) . ? N2 C4 1.334(5) . ? N2 C18 1.441(4) . ? C1 C2 1.521(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.417(5) . ? C3 C4 1.409(5) . ? C3 H3A 0.9500 . ? C4 C5 1.518(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.397(5) . ? C6 C11 1.410(5) . ? C7 C8 1.388(5) . ? C7 C12A 1.567(8) . ? C7 C12 1.578(9) . ? C8 C9 1.373(6) . ? C8 H8A 0.9500 . ? C9 C10 1.389(6) . ? C9 H9A 0.9500 . ? C10 C11 1.395(5) . ? C10 H10A 0.9500 . ? C11 C15 1.522(5) . ? C12 C14 1.503(13) . ? C12 C13 1.512(12) . ? C12 H12B 1.0000 . ? C13 H13D 0.9800 . ? C13 H13E 0.9800 . ? C13 H13F 0.9800 . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? C12A C13A 1.527(11) . ? C12A C14A 1.543(11) . ? C12A H12A 1.0000 . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15 C16 1.516(6) . ? C15 C17 1.534(6) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.406(5) . ? C18 C19 1.415(5) . ? C19 C20 1.391(5) . ? C19 C24 1.517(5) . ? C20 C21 1.382(6) . ? C20 H20A 0.9500 . ? C21 C22 1.379(6) . ? C21 H21A 0.9500 . ? C22 C23 1.403(5) . ? C22 H22A 0.9500 . ? C23 C27 1.525(5) . ? C24 C25 1.529(6) . ? C24 C26 1.530(5) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.525(6) . ? C27 C28 1.541(6) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.410(6) . ? C30 C34 1.423(6) . ? C30 C35 1.512(5) . ? C31 C32 1.431(5) . ? C31 C36 1.516(5) . ? C32 C33 1.420(5) . ? C32 C37 1.501(6) . ? C33 C34 1.418(5) . ? C33 C38 1.512(5) . ? C34 C39 1.510(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38C 0.9800 . ? C38 H38D 0.9800 . ? C39 H39C 0.9800 . ? C39 H39D 0.9800 . ? C39 H39A 0.9800 . ? 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 Sm1 N2 82.20(10) . . ? N1 Sm1 Cl1 105.93(7) . . ? N2 Sm1 Cl1 107.42(7) . . ? N1 Sm1 C30 102.60(11) . . ? N2 Sm1 C30 99.83(11) . . ? Cl1 Sm1 C30 142.65(8) . . ? N1 Sm1 C34 94.76(11) . . ? N2 Sm1 C34 128.56(11) . . ? Cl1 Sm1 C34 122.46(9) . . ? C30 Sm1 C34 30.56(12) . . ? N1 Sm1 C31 131.97(11) . . ? N2 Sm1 C31 95.57(11) . . ? Cl1 Sm1 C31 120.14(9) . . ? C30 Sm1 C31 30.17(12) . . ? C34 Sm1 C31 50.16(12) . . ? N1 Sm1 C33 117.17(11) . . ? N2 Sm1 C33 145.16(11) . . ? Cl1 Sm1 C33 95.20(8) . . ? C30 Sm1 C33 49.77(11) . . ? C34 Sm1 C33 30.11(11) . . ? C31 Sm1 C33 49.71(11) . . ? N1 Sm1 C32 144.49(11) . . ? N2 Sm1 C32 120.08(10) . . ? Cl1 Sm1 C32 93.81(8) . . ? C30 Sm1 C32 49.80(11) . . ? C34 Sm1 C32 49.86(12) . . ? C31 Sm1 C32 30.25(11) . . ? C33 Sm1 C32 29.91(11) . . ? C2 N1 C6 118.5(3) . . ? C2 N1 Sm1 109.9(2) . . ? C6 N1 Sm1 128.3(2) . . ? C4 N2 C18 118.9(3) . . ? C4 N2 Sm1 110.3(2) . . ? C18 N2 Sm1 126.2(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 124.7(3) . . ? N1 C2 C1 121.2(3) . . ? C3 C2 C1 114.1(3) . . ? C4 C3 C2 132.0(4) . . ? C4 C3 H3A 114.0 . . ? C2 C3 H3A 114.0 . . ? N2 C4 C3 124.9(3) . . ? N2 C4 C5 120.2(3) . . ? C3 C4 C5 114.8(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 120.1(3) . . ? C7 C6 N1 121.0(3) . . ? C11 C6 N1 118.8(3) . . ? C8 C7 C6 119.7(4) . . ? C8 C7 C12A 117.3(4) . . ? C6 C7 C12A 121.1(4) . . ? C8 C7 C12 118.2(4) . . ? C6 C7 C12 118.8(4) . . ? C12A C7 C12 32.1(3) . . ? C9 C8 C7 121.2(4) . . ? C9 C8 H8A 119.4 . . ? C7 C8 H8A 119.4 . . ? C8 C9 C10 119.2(4) . . ? C8 C9 H9A 120.4 . . ? C10 C9 H9A 120.4 . . ? C9 C10 C11 121.7(4) . . ? C9 C10 H10A 119.1 . . ? C11 C10 H10A 119.1 . . ? C10 C11 C6 118.1(3) . . ? C10 C11 C15 119.6(3) . . ? C6 C11 C15 122.3(3) . . ? C14 C12 C13 109.6(7) . . ? C14 C12 C7 116.3(7) . . ? C13 C12 C7 106.6(7) . . ? C14 C12 H12B 108.0 . . ? C13 C12 H12B 108.0 . . ? C7 C12 H12B 108.0 . . ? C13A C12A C14A 108.8(6) . . ? C13A C12A C7 117.6(6) . . ? C14A C12A C7 104.7(6) . . ? C13A C12A H12A 108.5 . . ? C14A C12A H12A 108.5 . . ? C7 C12A H12A 108.5 . . ? C12A C13A H13A 109.5 . . ? C12A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? C12A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? C12A C14A H14A 109.5 . . ? C12A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C12A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C16 C15 C11 111.6(4) . . ? C16 C15 C17 110.6(4) . . ? C11 C15 C17 112.7(3) . . ? C16 C15 H15A 107.2 . . ? C11 C15 H15A 107.2 . . ? C17 C15 H15A 107.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 121.4(3) . . ? C23 C18 N2 120.1(3) . . ? C19 C18 N2 118.5(3) . . ? C20 C19 C18 117.5(3) . . ? C20 C19 C24 121.2(3) . . ? C18 C19 C24 121.3(3) . . ? C21 C20 C19 121.9(4) . . ? C21 C20 H20A 119.0 . . ? C19 C20 H20A 119.0 . . ? C22 C21 C20 120.1(4) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 120.7(4) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C22 C23 C18 118.4(3) . . ? C22 C23 C27 119.0(3) . . ? C18 C23 C27 122.6(3) . . ? C19 C24 C25 111.8(3) . . ? C19 C24 C26 113.7(3) . . ? C25 C24 C26 109.4(3) . . ? C19 C24 H24A 107.2 . . ? C25 C24 H24A 107.2 . . ? C26 C24 H24A 107.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 111.3(3) . . ? C23 C27 C28 112.3(3) . . ? C29 C27 C28 110.1(3) . . ? C23 C27 H27A 107.6 . . ? C29 C27 H27A 107.6 . . ? C28 C27 H27A 107.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C34 108.9(3) . . ? C31 C30 C35 126.3(4) . . ? C34 C30 C35 124.4(4) . . ? C31 C30 Sm1 76.5(2) . . ? C34 C30 Sm1 75.6(2) . . ? C35 C30 Sm1 119.5(2) . . ? C30 C31 C32 107.6(3) . . ? C30 C31 C36 126.8(4) . . ? C32 C31 C36 125.1(4) . . ? C30 C31 Sm1 73.3(2) . . ? C32 C31 Sm1 75.9(2) . . ? C36 C31 Sm1 123.3(3) . . ? C33 C32 C31 107.6(3) . . ? C33 C32 C37 124.1(3) . . ? C31 C32 C37 127.6(4) . . ? C33 C32 Sm1 74.7(2) . . ? C31 C32 Sm1 73.9(2) . . ? C37 C32 Sm1 124.3(3) . . ? C34 C33 C32 108.6(3) . . ? C34 C33 C38 127.5(4) . . ? C32 C33 C38 123.4(3) . . ? C34 C33 Sm1 73.6(2) . . ? C32 C33 Sm1 75.4(2) . . ? C38 C33 Sm1 123.3(3) . . ? C33 C34 C30 107.2(3) . . ? C33 C34 C39 127.6(4) . . ? C30 C34 C39 124.6(4) . . ? C33 C34 Sm1 76.3(2) . . ? C30 C34 Sm1 73.8(2) . . ? C39 C34 Sm1 122.6(2) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? C33 C38 H38D 109.5 . . ? H38A C38 H38D 109.5 . . ? H38C C38 H38D 109.5 . . ? C34 C39 H39C 109.5 . . ? C34 C39 H39D 109.5 . . ? H39C C39 H39D 109.5 . . ? C34 C39 H39A 109.5 . . ? H39C C39 H39A 109.5 . . ? H39D C39 H39A 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Sm1 N1 C2 -52.8(2) . . . . ? Cl1 Sm1 N1 C2 53.1(2) . . . . ? C30 Sm1 N1 C2 -151.2(2) . . . . ? C34 Sm1 N1 C2 178.9(2) . . . . ? C31 Sm1 N1 C2 -143.3(2) . . . . ? C33 Sm1 N1 C2 157.8(2) . . . . ? C32 Sm1 N1 C2 174.4(2) . . . . ? N2 Sm1 N1 C6 148.3(3) . . . . ? Cl1 Sm1 N1 C6 -105.8(3) . . . . ? C30 Sm1 N1 C6 49.9(3) . . . . ? C34 Sm1 N1 C6 20.0(3) . . . . ? C31 Sm1 N1 C6 57.8(3) . . . . ? C33 Sm1 N1 C6 -1.1(3) . . . . ? C32 Sm1 N1 C6 15.5(4) . . . . ? N1 Sm1 N2 C4 52.2(2) . . . . ? Cl1 Sm1 N2 C4 -52.1(2) . . . . ? C30 Sm1 N2 C4 153.7(2) . . . . ? C34 Sm1 N2 C4 142.1(2) . . . . ? C31 Sm1 N2 C4 -176.1(2) . . . . ? C33 Sm1 N2 C4 179.8(2) . . . . ? C32 Sm1 N2 C4 -157.3(2) . . . . ? N1 Sm1 N2 C18 -152.6(3) . . . . ? Cl1 Sm1 N2 C18 103.1(2) . . . . ? C30 Sm1 N2 C18 -51.1(3) . . . . ? C34 Sm1 N2 C18 -62.7(3) . . . . ? C31 Sm1 N2 C18 -20.9(3) . . . . ? C33 Sm1 N2 C18 -25.0(3) . . . . ? C32 Sm1 N2 C18 -2.1(3) . . . . ? C6 N1 C2 C3 -167.9(3) . . . . ? Sm1 N1 C2 C3 30.8(4) . . . . ? C6 N1 C2 C1 10.6(5) . . . . ? Sm1 N1 C2 C1 -150.6(3) . . . . ? N1 C2 C3 C4 18.1(6) . . . . ? C1 C2 C3 C4 -160.6(4) . . . . ? C18 N2 C4 C3 173.5(3) . . . . ? Sm1 N2 C4 C3 -29.2(4) . . . . ? C18 N2 C4 C5 -6.0(5) . . . . ? Sm1 N2 C4 C5 151.3(3) . . . . ? C2 C3 C4 N2 -19.1(6) . . . . ? C2 C3 C4 C5 160.4(4) . . . . ? C2 N1 C6 C7 -91.0(4) . . . . ? Sm1 N1 C6 C7 66.3(5) . . . . ? C2 N1 C6 C11 91.9(4) . . . . ? Sm1 N1 C6 C11 -110.8(3) . . . . ? C11 C6 C7 C8 -1.3(6) . . . . ? N1 C6 C7 C8 -178.3(4) . . . . ? C11 C6 C7 C12A -165.2(5) . . . . ? N1 C6 C7 C12A 17.8(7) . . . . ? C11 C6 C7 C12 157.8(5) . . . . ? N1 C6 C7 C12 -19.3(7) . . . . ? C6 C7 C8 C9 0.4(7) . . . . ? C12A C7 C8 C9 164.9(5) . . . . ? C12 C7 C8 C9 -158.8(5) . . . . ? C7 C8 C9 C10 -0.3(7) . . . . ? C8 C9 C10 C11 1.2(7) . . . . ? C9 C10 C11 C6 -2.0(6) . . . . ? C9 C10 C11 C15 177.9(4) . . . . ? C7 C6 C11 C10 2.1(6) . . . . ? N1 C6 C11 C10 179.2(3) . . . . ? C7 C6 C11 C15 -177.9(4) . . . . ? N1 C6 C11 C15 -0.8(5) . . . . ? C8 C7 C12 C14 8.1(10) . . . . ? C6 C7 C12 C14 -151.3(7) . . . . ? C12A C7 C12 C14 105.3(11) . . . . ? C8 C7 C12 C13 -114.5(6) . . . . ? C6 C7 C12 C13 86.2(7) . . . . ? C12A C7 C12 C13 -17.3(7) . . . . ? C8 C7 C12A C13A -36.7(8) . . . . ? C6 C7 C12A C13A 127.5(6) . . . . ? C12 C7 C12A C13A -136.9(11) . . . . ? C8 C7 C12A C14A 84.1(7) . . . . ? C6 C7 C12A C14A -111.6(6) . . . . ? C12 C7 C12A C14A -16.0(7) . . . . ? C10 C11 C15 C16 84.2(5) . . . . ? C6 C11 C15 C16 -95.8(5) . . . . ? C10 C11 C15 C17 -41.0(5) . . . . ? C6 C11 C15 C17 139.0(4) . . . . ? C4 N2 C18 C23 81.7(4) . . . . ? Sm1 N2 C18 C23 -71.7(4) . . . . ? C4 N2 C18 C19 -100.7(4) . . . . ? Sm1 N2 C18 C19 106.0(3) . . . . ? C23 C18 C19 C20 0.7(5) . . . . ? N2 C18 C19 C20 -177.0(3) . . . . ? C23 C18 C19 C24 -177.2(3) . . . . ? N2 C18 C19 C24 5.1(5) . . . . ? C18 C19 C20 C21 0.7(6) . . . . ? C24 C19 C20 C21 178.6(4) . . . . ? C19 C20 C21 C22 -1.1(6) . . . . ? C20 C21 C22 C23 0.0(6) . . . . ? C21 C22 C23 C18 1.3(6) . . . . ? C21 C22 C23 C27 -179.9(4) . . . . ? C19 C18 C23 C22 -1.7(5) . . . . ? N2 C18 C23 C22 175.9(3) . . . . ? C19 C18 C23 C27 179.6(3) . . . . ? N2 C18 C23 C27 -2.8(5) . . . . ? C20 C19 C24 C25 -95.9(4) . . . . ? C18 C19 C24 C25 81.9(4) . . . . ? C20 C19 C24 C26 28.6(5) . . . . ? C18 C19 C24 C26 -153.5(4) . . . . ? C22 C23 C27 C29 -75.7(4) . . . . ? C18 C23 C27 C29 103.0(4) . . . . ? C22 C23 C27 C28 48.3(5) . . . . ? C18 C23 C27 C28 -133.0(4) . . . . ? N1 Sm1 C30 C31 168.2(2) . . . . ? N2 Sm1 C30 C31 84.1(2) . . . . ? Cl1 Sm1 C30 C31 -52.6(3) . . . . ? C34 Sm1 C30 C31 -113.9(3) . . . . ? C33 Sm1 C30 C31 -76.7(2) . . . . ? C32 Sm1 C30 C31 -37.2(2) . . . . ? N1 Sm1 C30 C34 -77.8(2) . . . . ? N2 Sm1 C30 C34 -161.9(2) . . . . ? Cl1 Sm1 C30 C34 61.4(3) . . . . ? C31 Sm1 C30 C34 113.9(3) . . . . ? C33 Sm1 C30 C34 37.3(2) . . . . ? C32 Sm1 C30 C34 76.8(2) . . . . ? N1 Sm1 C30 C35 43.9(3) . . . . ? N2 Sm1 C30 C35 -40.2(3) . . . . ? Cl1 Sm1 C30 C35 -177.0(3) . . . . ? C34 Sm1 C30 C35 121.7(4) . . . . ? C31 Sm1 C30 C35 -124.4(4) . . . . ? C33 Sm1 C30 C35 159.0(4) . . . . ? C32 Sm1 C30 C35 -161.5(4) . . . . ? C34 C30 C31 C32 -0.6(4) . . . . ? C35 C30 C31 C32 -174.4(4) . . . . ? Sm1 C30 C31 C32 68.8(3) . . . . ? C34 C30 C31 C36 171.2(4) . . . . ? C35 C30 C31 C36 -2.6(6) . . . . ? Sm1 C30 C31 C36 -119.5(4) . . . . ? C34 C30 C31 Sm1 -69.4(3) . . . . ? C35 C30 C31 Sm1 116.8(4) . . . . ? N1 Sm1 C31 C30 -15.5(3) . . . . ? N2 Sm1 C31 C30 -100.0(2) . . . . ? Cl1 Sm1 C31 C30 146.13(19) . . . . ? C34 Sm1 C31 C30 37.2(2) . . . . ? C33 Sm1 C31 C30 76.9(2) . . . . ? C32 Sm1 C31 C30 113.6(3) . . . . ? N1 Sm1 C31 C32 -129.1(2) . . . . ? N2 Sm1 C31 C32 146.4(2) . . . . ? Cl1 Sm1 C31 C32 32.5(2) . . . . ? C30 Sm1 C31 C32 -113.6(3) . . . . ? C34 Sm1 C31 C32 -76.4(2) . . . . ? C33 Sm1 C31 C32 -36.7(2) . . . . ? N1 Sm1 C31 C36 107.9(3) . . . . ? N2 Sm1 C31 C36 23.4(3) . . . . ? Cl1 Sm1 C31 C36 -90.4(3) . . . . ? C30 Sm1 C31 C36 123.4(4) . . . . ? C34 Sm1 C31 C36 160.7(4) . . . . ? C33 Sm1 C31 C36 -159.6(4) . . . . ? C32 Sm1 C31 C36 -122.9(4) . . . . ? C30 C31 C32 C33 0.6(4) . . . . ? C36 C31 C32 C33 -171.4(4) . . . . ? Sm1 C31 C32 C33 67.6(3) . . . . ? C30 C31 C32 C37 171.8(4) . . . . ? C36 C31 C32 C37 -0.2(6) . . . . ? Sm1 C31 C32 C37 -121.2(4) . . . . ? C30 C31 C32 Sm1 -67.0(3) . . . . ? C36 C31 C32 Sm1 121.0(4) . . . . ? N1 Sm1 C32 C33 -30.7(3) . . . . ? N2 Sm1 C32 C33 -153.5(2) . . . . ? Cl1 Sm1 C32 C33 93.8(2) . . . . ? C30 Sm1 C32 C33 -76.9(2) . . . . ? C34 Sm1 C32 C33 -36.5(2) . . . . ? C31 Sm1 C32 C33 -114.0(3) . . . . ? N1 Sm1 C32 C31 83.2(3) . . . . ? N2 Sm1 C32 C31 -39.6(3) . . . . ? Cl1 Sm1 C32 C31 -152.2(2) . . . . ? C30 Sm1 C32 C31 37.1(2) . . . . ? C34 Sm1 C32 C31 77.4(2) . . . . ? C33 Sm1 C32 C31 114.0(3) . . . . ? N1 Sm1 C32 C37 -151.9(3) . . . . ? N2 Sm1 C32 C37 85.3(3) . . . . ? Cl1 Sm1 C32 C37 -27.3(3) . . . . ? C30 Sm1 C32 C37 162.0(4) . . . . ? C34 Sm1 C32 C37 -157.7(4) . . . . ? C31 Sm1 C32 C37 124.9(4) . . . . ? C33 Sm1 C32 C37 -121.2(4) . . . . ? C31 C32 C33 C34 -0.3(4) . . . . ? C37 C32 C33 C34 -171.9(4) . . . . ? Sm1 C32 C33 C34 66.7(3) . . . . ? C31 C32 C33 C38 172.4(4) . . . . ? C37 C32 C33 C38 0.8(6) . . . . ? Sm1 C32 C33 C38 -120.5(4) . . . . ? C31 C32 C33 Sm1 -67.1(3) . . . . ? C37 C32 C33 Sm1 121.4(4) . . . . ? N1 Sm1 C33 C34 45.7(3) . . . . ? N2 Sm1 C33 C34 -72.4(3) . . . . ? Cl1 Sm1 C33 C34 156.5(2) . . . . ? C30 Sm1 C33 C34 -37.9(2) . . . . ? C31 Sm1 C33 C34 -77.7(2) . . . . ? C32 Sm1 C33 C34 -114.9(3) . . . . ? N1 Sm1 C33 C32 160.5(2) . . . . ? N2 Sm1 C33 C32 42.5(3) . . . . ? Cl1 Sm1 C33 C32 -88.6(2) . . . . ? C30 Sm1 C33 C32 77.0(2) . . . . ? C34 Sm1 C33 C32 114.9(3) . . . . ? C31 Sm1 C33 C32 37.1(2) . . . . ? N1 Sm1 C33 C38 -78.9(3) . . . . ? N2 Sm1 C33 C38 163.1(3) . . . . ? Cl1 Sm1 C33 C38 32.0(3) . . . . ? C30 Sm1 C33 C38 -162.4(4) . . . . ? C34 Sm1 C33 C38 -124.5(4) . . . . ? C31 Sm1 C33 C38 157.7(4) . . . . ? C32 Sm1 C33 C38 120.6(4) . . . . ? C32 C33 C34 C30 0.0(4) . . . . ? C38 C33 C34 C30 -172.4(4) . . . . ? Sm1 C33 C34 C30 67.9(3) . . . . ? C32 C33 C34 C39 171.3(4) . . . . ? C38 C33 C34 C39 -1.0(7) . . . . ? Sm1 C33 C34 C39 -120.8(4) . . . . ? C32 C33 C34 Sm1 -67.9(3) . . . . ? C38 C33 C34 Sm1 119.7(4) . . . . ? C31 C30 C34 C33 0.4(4) . . . . ? C35 C30 C34 C33 174.3(3) . . . . ? Sm1 C30 C34 C33 -69.6(3) . . . . ? C31 C30 C34 C39 -171.3(3) . . . . ? C35 C30 C34 C39 2.7(6) . . . . ? Sm1 C30 C34 C39 118.8(4) . . . . ? C31 C30 C34 Sm1 70.0(3) . . . . ? C35 C30 C34 Sm1 -116.1(4) . . . . ? N1 Sm1 C34 C33 -140.3(2) . . . . ? N2 Sm1 C34 C33 135.9(2) . . . . ? Cl1 Sm1 C34 C33 -28.0(3) . . . . ? C30 Sm1 C34 C33 112.9(3) . . . . ? C31 Sm1 C34 C33 76.1(2) . . . . ? C32 Sm1 C34 C33 36.3(2) . . . . ? N1 Sm1 C34 C30 106.8(2) . . . . ? N2 Sm1 C34 C30 23.0(3) . . . . ? Cl1 Sm1 C34 C30 -140.88(19) . . . . ? C31 Sm1 C34 C30 -36.7(2) . . . . ? C33 Sm1 C34 C30 -112.9(3) . . . . ? C32 Sm1 C34 C30 -76.6(2) . . . . ? N1 Sm1 C34 C39 -14.2(3) . . . . ? N2 Sm1 C34 C39 -98.0(3) . . . . ? Cl1 Sm1 C34 C39 98.1(3) . . . . ? C30 Sm1 C34 C39 -121.1(4) . . . . ? C31 Sm1 C34 C39 -157.8(4) . . . . ? C33 Sm1 C34 C39 126.1(4) . . . . ? C32 Sm1 C34 C39 162.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.866 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.866 _refine_diff_density_max 0.956 _refine_diff_density_min -1.722 _refine_diff_density_rms 0.106 #==================================== data_NACSmClALMe4 _database_code_depnum_ccdc_archive 'CCDC 244222' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C40 H96 N12 CL6 Al2 Sm2), 4.5(C7 H8)' _chemical_formula_sum 'C155.50 H236 Al2 Cl6 N8 Sm4' _chemical_formula_weight 3085.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 16.0730(3) _cell_length_b 28.2943(3) _cell_length_c 34.5779(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.4430(10) _cell_angle_gamma 90.00 _cell_volume 15512.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.17 _cell_measurement_theta_max 22.03 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6404 _exptl_absorpt_coefficient_mu 1.656 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6452 _exptl_absorpt_correction_T_max 0.9218 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 69617 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0977 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.74 _reflns_number_total 26328 _reflns_number_gt 17281 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.052' _computing_cell_refinement 'Bruker SAINT v5.10' _computing_data_reduction 'Bruker SAINT v5.10' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms on the bridging methyl groups were included in positions observed from a difference Fourier map. They were allowed to refine, but were constrained to have C-H distances equal to 1. Three of the toluenes of crystallization were found to have disorder. One was disordered about the inversion center at [0.5, 0.5, 0.5]. Three of the remianng four toluenes have simple rotatio disorder, either by approximately 180 deg. or by an approximate 30 deg rotation. The benzene portion of these molecules was refined as a rigid hexagon. ; _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^)+(0.0381P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26328 _refine_ls_number_parameters 1605 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.935245(16) 0.272171(9) 0.400136(9) 0.01784(7) Uani 1 1 d . . . Sm2 Sm 0.730676(16) 0.286745(9) 0.445253(8) 0.01677(7) Uani 1 1 d . . . Sm3 Sm 0.612828(16) 0.034412(9) 0.365989(8) 0.01661(7) Uani 1 1 d . . . Sm4 Sm 0.725618(16) 0.063510(9) 0.277790(8) 0.01706(7) Uani 1 1 d . . . Cl1 Cl 0.87598(8) 0.33871(5) 0.44780(5) 0.0303(4) Uani 1 1 d . . . Cl2 Cl 0.85408(8) 0.21776(5) 0.44889(5) 0.0316(4) Uani 1 1 d . . . Cl3 Cl 0.76508(8) 0.28061(5) 0.36912(4) 0.0292(3) Uani 1 1 d . . . Cl4 Cl 0.62450(9) -0.00992(5) 0.29590(4) 0.0276(3) Uani 1 1 d . . . Cl5 Cl 0.60525(9) 0.10915(5) 0.31336(4) 0.0297(4) Uani 1 1 d . . . Cl6 Cl 0.77828(8) 0.05049(5) 0.35777(4) 0.0294(4) Uani 1 1 d . . . Al1 Al 0.55000(10) 0.15483(6) 0.45276(5) 0.0214(4) Uani 1 1 d . . . Al2 Al 0.95570(10) 0.17111(6) 0.29087(5) 0.0239(4) Uani 1 1 d . . . N1 N 1.0330(3) 0.32589(15) 0.38114(13) 0.0246(11) Uani 1 1 d . . . N2 N 1.0654(3) 0.23754(15) 0.42876(13) 0.0228(11) Uani 1 1 d . . . N3 N 0.6036(3) 0.32873(14) 0.42308(13) 0.0197(10) Uani 1 1 d . . . N4 N 0.6957(2) 0.31631(14) 0.50479(12) 0.0168(10) Uani 1 1 d . . . N5 N 0.4873(2) -0.00435(14) 0.37512(12) 0.0186(10) Uani 1 1 d . . . N6 N 0.6604(2) -0.01096(14) 0.42385(12) 0.0169(10) Uani 1 1 d . . . N7 N 0.6754(2) 0.10465(14) 0.21798(13) 0.0177(10) Uani 1 1 d . . . N8 N 0.7946(2) 0.02330(14) 0.23249(12) 0.0185(10) Uani 1 1 d . . . C1 C 0.9447(3) 0.21495(19) 0.33640(17) 0.0226(13) Uani 1 1 d D . . H101 H 0.947(3) 0.1951(15) 0.3597(9) 0.034 Uiso 1 1 d D . . H102 H 0.992(2) 0.2375(13) 0.3409(15) 0.034 Uiso 1 1 d D . . H103 H 0.8903(15) 0.2313(15) 0.3317(15) 0.034 Uiso 1 1 d D . . C2 C 0.8574(3) 0.12524(19) 0.28739(17) 0.0223(13) Uani 1 1 d D . . H201 H 0.874(3) 0.0965(10) 0.3024(13) 0.034 Uiso 1 1 d D . . H202 H 0.842(3) 0.1171(17) 0.2596(4) 0.034 Uiso 1 1 d D . . H203 H 0.810(2) 0.1398(15) 0.2972(14) 0.034 Uiso 1 1 d D . . C3 C 0.9415(4) 0.2056(2) 0.24031(17) 0.0366(16) Uani 1 1 d . . . H3A H 0.9876 0.2284 0.2407 0.055 Uiso 1 1 calc R . . H3B H 0.8875 0.2225 0.2364 0.055 Uiso 1 1 calc R . . H3C H 0.9422 0.1831 0.2188 0.055 Uiso 1 1 calc R . . C4 C 1.0637(3) 0.1363(2) 0.30362(19) 0.0381(16) Uani 1 1 d . . . H4A H 1.1108 0.1586 0.3053 0.057 Uiso 1 1 calc R . . H4B H 1.0678 0.1130 0.2831 0.057 Uiso 1 1 calc R . . H4C H 1.0660 0.1201 0.3288 0.057 Uiso 1 1 calc R . . C5 C 0.6291(3) 0.21026(19) 0.44930(16) 0.0180(12) Uani 1 1 d D . . H501 H 0.607(3) 0.2379(10) 0.4612(13) 0.027 Uiso 1 1 d D . . H502 H 0.636(3) 0.2157(17) 0.4220(5) 0.027 Uiso 1 1 d D . . H503 H 0.6828(16) 0.2002(16) 0.4647(12) 0.027 Uiso 1 1 d D . . C6 C 0.5787(3) 0.10408(19) 0.41537(18) 0.0226(13) Uani 1 1 d D . . H601 H 0.6385(9) 0.0996(17) 0.4139(15) 0.034 Uiso 1 1 d D . . H602 H 0.554(3) 0.1120(17) 0.3884(5) 0.034 Uiso 1 1 d D . . H603 H 0.557(3) 0.0739(9) 0.4237(15) 0.034 Uiso 1 1 d D . . C7 C 0.4317(3) 0.1743(2) 0.43416(19) 0.0408(17) Uani 1 1 d . . . H7A H 0.4156 0.1988 0.4516 0.061 Uiso 1 1 calc R . . H7B H 0.3944 0.1469 0.4342 0.061 Uiso 1 1 calc R . . H7C H 0.4267 0.1869 0.4075 0.061 Uiso 1 1 calc R . . C8 C 0.5718(4) 0.1303(2) 0.50699(17) 0.0396(17) Uani 1 1 d . . . H8A H 0.5580 0.1546 0.5250 0.059 Uiso 1 1 calc R . . H8B H 0.6315 0.1217 0.5139 0.059 Uiso 1 1 calc R . . H8C H 0.5368 0.1023 0.5089 0.059 Uiso 1 1 calc R . . C9 C 1.2123(3) 0.2088(2) 0.4301(2) 0.0401(17) Uani 1 1 d . . . H9A H 1.1967 0.1878 0.4503 0.060 Uiso 1 1 calc R . . H9B H 1.2603 0.2284 0.4415 0.060 Uiso 1 1 calc R . . H9C H 1.2278 0.1898 0.4087 0.060 Uiso 1 1 calc R . . C10 C 1.1383(3) 0.24009(19) 0.41448(18) 0.0267(14) Uani 1 1 d . . . C11 C 1.1518(3) 0.2723(2) 0.38542(18) 0.0321(15) Uani 1 1 d . . . H11A H 1.1977 0.2648 0.3724 0.039 Uiso 1 1 calc R . . C12 C 1.1092(4) 0.3134(2) 0.37262(17) 0.0287(14) Uani 1 1 d . . . C13 C 1.1546(4) 0.3468(2) 0.3478(2) 0.0444(18) Uani 1 1 d . . . H13A H 1.1196 0.3748 0.3406 0.067 Uiso 1 1 calc R . . H13B H 1.1645 0.3304 0.3240 0.067 Uiso 1 1 calc R . . H13C H 1.2088 0.3565 0.3631 0.067 Uiso 1 1 calc R . . C14 C 1.0044(3) 0.37393(19) 0.37279(18) 0.0288(15) Uani 1 1 d . . . C15 C 1.0372(4) 0.4107(2) 0.39839(18) 0.0331(16) Uani 1 1 d . . . C16 C 1.0093(4) 0.4563(2) 0.3897(2) 0.0448(19) Uani 1 1 d . . . H16A H 1.0306 0.4813 0.4067 0.054 Uiso 1 1 calc R . . C17 C 0.9511(4) 0.4662(2) 0.3567(2) 0.0428(18) Uani 1 1 d . . . H17A H 0.9333 0.4978 0.3509 0.051 Uiso 1 1 calc R . . C18 C 0.9191(4) 0.4301(2) 0.3322(2) 0.0380(17) Uani 1 1 d . . . H18A H 0.8789 0.4372 0.3096 0.046 Uiso 1 1 calc R . . C19 C 0.9435(4) 0.38353(19) 0.33950(18) 0.0286(15) Uani 1 1 d . . . C20 C 0.9060(3) 0.3449(2) 0.31129(17) 0.0295(15) Uani 1 1 d . . . H20A H 0.9016 0.3160 0.3275 0.035 Uiso 1 1 calc R . . C21 C 0.9652(4) 0.3322(2) 0.2818(2) 0.056(2) Uani 1 1 d . . . H21A H 1.0216 0.3251 0.2961 0.084 Uiso 1 1 calc R . . H21B H 0.9684 0.3589 0.2642 0.084 Uiso 1 1 calc R . . H21C H 0.9430 0.3045 0.2665 0.084 Uiso 1 1 calc R . . C22 C 0.8176(4) 0.3554(2) 0.2898(2) 0.0483(19) Uani 1 1 d . . . H22A H 0.7809 0.3634 0.3089 0.072 Uiso 1 1 calc R . . H22B H 0.7952 0.3275 0.2748 0.072 Uiso 1 1 calc R . . H22C H 0.8197 0.3821 0.2719 0.072 Uiso 1 1 calc R . . C23 C 1.1011(4) 0.4010(2) 0.43532(19) 0.0444(18) Uani 1 1 d . . . H23A H 1.1117 0.3662 0.4374 0.053 Uiso 1 1 calc R . . C24 C 1.1856(4) 0.4265(3) 0.4343(2) 0.072(3) Uani 1 1 d . . . H24A H 1.2084 0.4167 0.4110 0.109 Uiso 1 1 calc R . . H24B H 1.2258 0.4184 0.4579 0.109 Uiso 1 1 calc R . . H24C H 1.1764 0.4608 0.4335 0.109 Uiso 1 1 calc R . . C25 C 1.0671(4) 0.4176(2) 0.4720(2) 0.056(2) Uani 1 1 d . . . H25A H 1.0138 0.4015 0.4735 0.084 Uiso 1 1 calc R . . H25B H 1.0578 0.4518 0.4706 0.084 Uiso 1 1 calc R . . H25C H 1.1082 0.4100 0.4954 0.084 Uiso 1 1 calc R . . C26 C 1.0620(3) 0.2079(2) 0.46230(17) 0.0243(14) Uani 1 1 d . . . C27 C 1.0544(3) 0.1578(2) 0.45857(17) 0.0265(14) Uani 1 1 d . . . C28 C 1.0449(4) 0.1321(2) 0.49166(18) 0.0368(16) Uani 1 1 d . . . H28A H 1.0403 0.0987 0.4900 0.044 Uiso 1 1 calc R . . C29 C 1.0418(4) 0.1540(2) 0.52670(19) 0.0477(19) Uani 1 1 d . . . H29A H 1.0345 0.1356 0.5489 0.057 Uiso 1 1 calc R . . C30 C 1.0493(4) 0.2026(2) 0.53037(19) 0.0423(17) Uani 1 1 d . . . H30A H 1.0478 0.2171 0.5550 0.051 Uiso 1 1 calc R . . C31 C 1.0589(3) 0.2302(2) 0.49846(17) 0.0289(15) Uani 1 1 d . . . C32 C 1.0537(3) 0.13167(18) 0.41980(17) 0.0248(14) Uani 1 1 d . . . H32A H 1.0689 0.1547 0.4001 0.030 Uiso 1 1 calc R . . C33 C 1.1181(4) 0.0912(2) 0.4239(2) 0.0433(18) Uani 1 1 d . . . H33A H 1.1746 0.1038 0.4335 0.065 Uiso 1 1 calc R . . H33B H 1.1176 0.0762 0.3983 0.065 Uiso 1 1 calc R . . H33C H 1.1034 0.0678 0.4426 0.065 Uiso 1 1 calc R . . C34 C 0.9655(3) 0.11178(19) 0.40419(17) 0.0305(15) Uani 1 1 d . . . H34A H 0.9242 0.1376 0.4012 0.046 Uiso 1 1 calc R . . H34B H 0.9502 0.0884 0.4227 0.046 Uiso 1 1 calc R . . H34C H 0.9658 0.0968 0.3787 0.046 Uiso 1 1 calc R . . C35 C 1.0690(3) 0.2829(2) 0.50275(18) 0.0304(15) Uani 1 1 d . . . H35A H 1.0430 0.2974 0.4772 0.036 Uiso 1 1 calc R . . C36 C 1.1630(3) 0.2966(2) 0.5100(2) 0.049(2) Uani 1 1 d . . . H36A H 1.1907 0.2831 0.4894 0.074 Uiso 1 1 calc R . . H36B H 1.1898 0.2843 0.5356 0.074 Uiso 1 1 calc R . . H36C H 1.1683 0.3311 0.5099 0.074 Uiso 1 1 calc R . . C37 C 1.0249(4) 0.3043(2) 0.53449(18) 0.0413(17) Uani 1 1 d . . . H37A H 0.9648 0.2962 0.5292 0.062 Uiso 1 1 calc R . . H37B H 1.0314 0.3387 0.5346 0.062 Uiso 1 1 calc R . . H37C H 1.0501 0.2916 0.5601 0.062 Uiso 1 1 calc R . . C38 C 0.4559(3) 0.3564(2) 0.42212(17) 0.0361(16) Uani 1 1 d . . . H38A H 0.4575 0.3601 0.3941 0.054 Uiso 1 1 calc R . . H38B H 0.4455 0.3872 0.4334 0.054 Uiso 1 1 calc R . . H38C H 0.4106 0.3344 0.4257 0.054 Uiso 1 1 calc R . . C39 C 0.5404(3) 0.33681(18) 0.44271(17) 0.0223(13) Uani 1 1 d . . . C40 C 0.5467(3) 0.33012(18) 0.48320(16) 0.0244(14) Uani 1 1 d . . . H40A H 0.4943 0.3294 0.4925 0.029 Uiso 1 1 calc R . . C41 C 0.6170(3) 0.32433(18) 0.51183(16) 0.0210(13) Uani 1 1 d . . . C42 C 0.6011(3) 0.3291(2) 0.55344(16) 0.0307(15) Uani 1 1 d . . . H42A H 0.6542 0.3249 0.5716 0.046 Uiso 1 1 calc R . . H42B H 0.5606 0.3050 0.5586 0.046 Uiso 1 1 calc R . . H42C H 0.5781 0.3606 0.5572 0.046 Uiso 1 1 calc R . . C43 C 0.7633(3) 0.31842(18) 0.53892(15) 0.0188(12) Uani 1 1 d . . . C44 C 0.8059(3) 0.36145(18) 0.54728(17) 0.0234(13) Uani 1 1 d . . . C45 C 0.8670(3) 0.3641(2) 0.58107(18) 0.0325(15) Uani 1 1 d . . . H45A H 0.8963 0.3930 0.5873 0.039 Uiso 1 1 calc R . . C46 C 0.8857(3) 0.3256(2) 0.60553(18) 0.0353(16) Uani 1 1 d . . . H46A H 0.9270 0.3282 0.6285 0.042 Uiso 1 1 calc R . . C47 C 0.8445(3) 0.2838(2) 0.59659(17) 0.0293(14) Uani 1 1 d . . . H47A H 0.8579 0.2575 0.6135 0.035 Uiso 1 1 calc R . . C48 C 0.7832(3) 0.27886(18) 0.56320(16) 0.0235(13) Uani 1 1 d . . . C49 C 0.7384(3) 0.23157(19) 0.55617(16) 0.0264(14) Uani 1 1 d . . . H49A H 0.6934 0.2347 0.5327 0.032 Uiso 1 1 calc R . . C50 C 0.6965(4) 0.2159(2) 0.59145(18) 0.0419(17) Uani 1 1 d . . . H50A H 0.6561 0.2401 0.5967 0.063 Uiso 1 1 calc R . . H50B H 0.7399 0.2119 0.6147 0.063 Uiso 1 1 calc R . . H50C H 0.6669 0.1859 0.5853 0.063 Uiso 1 1 calc R . . C51 C 0.8000(4) 0.1933(2) 0.54777(19) 0.0412(17) Uani 1 1 d . . . H51A H 0.8260 0.2027 0.5252 0.062 Uiso 1 1 calc R . . H51B H 0.7696 0.1634 0.5420 0.062 Uiso 1 1 calc R . . H51C H 0.8440 0.1892 0.5708 0.062 Uiso 1 1 calc R . . C52 C 0.7862(4) 0.4048(2) 0.52175(19) 0.0351(16) Uani 1 1 d . . . H52A H 0.7615 0.3936 0.4949 0.042 Uiso 1 1 calc R . . C53 C 0.8633(4) 0.4353(2) 0.5178(2) 0.0496(19) Uani 1 1 d . . . H53A H 0.9058 0.4158 0.5080 0.074 Uiso 1 1 calc R . . H53B H 0.8872 0.4484 0.5435 0.074 Uiso 1 1 calc R . . H53C H 0.8462 0.4612 0.4994 0.074 Uiso 1 1 calc R . . C54 C 0.7201(4) 0.4357(2) 0.5364(3) 0.072(3) Uani 1 1 d . . . H54A H 0.6702 0.4167 0.5385 0.108 Uiso 1 1 calc R . . H54B H 0.7043 0.4617 0.5178 0.108 Uiso 1 1 calc R . . H54C H 0.7435 0.4487 0.5621 0.108 Uiso 1 1 calc R . . C55 C 0.5947(3) 0.34308(19) 0.38208(16) 0.0225(13) Uani 1 1 d . . . C56 C 0.5498(3) 0.3148(2) 0.35232(17) 0.0260(14) Uani 1 1 d . . . C57 C 0.5489(3) 0.3285(2) 0.31336(18) 0.0352(16) Uani 1 1 d . . . H57A H 0.5201 0.3096 0.2926 0.042 Uiso 1 1 calc R . . C58 C 0.5898(4) 0.3694(2) 0.30484(18) 0.0381(17) Uani 1 1 d . . . H58A H 0.5881 0.3787 0.2783 0.046 Uiso 1 1 calc R . . C59 C 0.6328(4) 0.3965(2) 0.3346(2) 0.0386(17) Uani 1 1 d . . . H59A H 0.6606 0.4243 0.3281 0.046 Uiso 1 1 calc R . . C60 C 0.6368(3) 0.38439(19) 0.37327(17) 0.0265(14) Uani 1 1 d . . . C61 C 0.6843(3) 0.41464(19) 0.40543(19) 0.0339(16) Uani 1 1 d . . . H61A H 0.7031 0.3931 0.4281 0.041 Uiso 1 1 calc R . . C62 C 0.6275(4) 0.4514(2) 0.4196(2) 0.058(2) Uani 1 1 d . . . H62A H 0.5772 0.4359 0.4263 0.087 Uiso 1 1 calc R . . H62B H 0.6105 0.4747 0.3989 0.087 Uiso 1 1 calc R . . H62C H 0.6580 0.4673 0.4429 0.087 Uiso 1 1 calc R . . C63 C 0.7650(4) 0.4378(2) 0.3950(2) 0.054(2) Uani 1 1 d . . . H63A H 0.8011 0.4134 0.3864 0.081 Uiso 1 1 calc R . . H63B H 0.7955 0.4539 0.4182 0.081 Uiso 1 1 calc R . . H63C H 0.7494 0.4608 0.3739 0.081 Uiso 1 1 calc R . . C64 C 0.5032(3) 0.26935(19) 0.36016(17) 0.0278(14) Uani 1 1 d . . . H64A H 0.5080 0.2656 0.3892 0.033 Uiso 1 1 calc R . . C65 C 0.4088(3) 0.2714(2) 0.34276(19) 0.0405(17) Uani 1 1 d . . . H65A H 0.3815 0.2419 0.3485 0.061 Uiso 1 1 calc R . . H65B H 0.4023 0.2757 0.3143 0.061 Uiso 1 1 calc R . . H65C H 0.3825 0.2980 0.3544 0.061 Uiso 1 1 calc R . . C66 C 0.5424(3) 0.22583(19) 0.34437(17) 0.0330(15) Uani 1 1 d . . . H66A H 0.5115 0.1975 0.3501 0.050 Uiso 1 1 calc R . . H66B H 0.6015 0.2231 0.3569 0.050 Uiso 1 1 calc R . . H66C H 0.5395 0.2289 0.3159 0.050 Uiso 1 1 calc R . . C67 C 0.3753(3) -0.0235(2) 0.41474(17) 0.0315(15) Uani 1 1 d . . . H67A H 0.3395 -0.0186 0.3893 0.047 Uiso 1 1 calc R . . H67B H 0.3589 -0.0013 0.4339 0.047 Uiso 1 1 calc R . . H67C H 0.3685 -0.0559 0.4236 0.047 Uiso 1 1 calc R . . C68 C 0.4675(3) -0.01507(18) 0.41078(17) 0.0230(13) Uani 1 1 d . . . C69 C 0.5252(3) -0.02136(18) 0.44473(16) 0.0227(13) Uani 1 1 d . . . H69A H 0.5015 -0.0233 0.4681 0.027 Uiso 1 1 calc R . . C70 C 0.6142(3) -0.02538(17) 0.45008(16) 0.0187(12) Uani 1 1 d . . . C71 C 0.6530(3) -0.04850(19) 0.48836(16) 0.0280(14) Uani 1 1 d . . . H71A H 0.7144 -0.0501 0.4899 0.042 Uiso 1 1 calc R . . H71B H 0.6303 -0.0805 0.4896 0.042 Uiso 1 1 calc R . . H71C H 0.6395 -0.0298 0.5104 0.042 Uiso 1 1 calc R . . C72 C 0.7509(3) -0.01927(17) 0.43151(16) 0.0187(13) Uani 1 1 d . . . C73 C 0.8043(3) 0.01017(18) 0.45775(15) 0.0193(13) Uani 1 1 d . . . C74 C 0.8912(3) 0.00379(19) 0.46070(17) 0.0254(14) Uani 1 1 d . . . H74A H 0.9286 0.0224 0.4787 0.030 Uiso 1 1 calc R . . C75 C 0.9232(3) -0.02904(19) 0.43797(18) 0.0313(15) Uani 1 1 d . . . H75A H 0.9826 -0.0324 0.4400 0.038 Uiso 1 1 calc R . . C76 C 0.8704(3) -0.05741(19) 0.41214(18) 0.0297(15) Uani 1 1 d . . . H76A H 0.8938 -0.0797 0.3964 0.036 Uiso 1 1 calc R . . C77 C 0.7835(3) -0.05351(17) 0.40905(16) 0.0200(13) Uani 1 1 d . . . C78 C 0.7255(3) -0.08627(18) 0.38174(16) 0.0232(13) Uani 1 1 d . . . H78A H 0.6731 -0.0680 0.3717 0.028 Uiso 1 1 calc R . . C79 C 0.7627(3) -0.1022(2) 0.34617(17) 0.0357(16) Uani 1 1 d . . . H79A H 0.7224 -0.1228 0.3298 0.054 Uiso 1 1 calc R . . H79B H 0.8151 -0.1196 0.3549 0.054 Uiso 1 1 calc R . . H79C H 0.7745 -0.0745 0.3310 0.054 Uiso 1 1 calc R . . C80 C 0.6992(4) -0.1285(2) 0.40409(19) 0.0430(17) Uani 1 1 d . . . H80A H 0.6616 -0.1489 0.3861 0.065 Uiso 1 1 calc R . . H80B H 0.6696 -0.1174 0.4250 0.065 Uiso 1 1 calc R . . H80C H 0.7494 -0.1464 0.4156 0.065 Uiso 1 1 calc R . . C81 C 0.7722(3) 0.04981(18) 0.48127(16) 0.0226(13) Uani 1 1 d . . . H81A H 0.7092 0.0480 0.4769 0.027 Uiso 1 1 calc R . . C82 C 0.8035(3) 0.0454(2) 0.52533(16) 0.0309(15) Uani 1 1 d . . . H82A H 0.7871 0.0145 0.5345 0.046 Uiso 1 1 calc R . . H82B H 0.7783 0.0704 0.5392 0.046 Uiso 1 1 calc R . . H82C H 0.8650 0.0484 0.5306 0.046 Uiso 1 1 calc R . . C83 C 0.7969(3) 0.09831(18) 0.46680(16) 0.0237(13) Uani 1 1 d . . . H83A H 0.7763 0.1011 0.4386 0.036 Uiso 1 1 calc R . . H83B H 0.8584 0.1015 0.4718 0.036 Uiso 1 1 calc R . . H83C H 0.7717 0.1233 0.4808 0.036 Uiso 1 1 calc R . . C84 C 0.4222(3) -0.01134(18) 0.34107(15) 0.0198(13) Uani 1 1 d . . . C85 C 0.4189(3) -0.05624(19) 0.32270(16) 0.0223(13) Uani 1 1 d . . . C86 C 0.3569(3) -0.0643(2) 0.29037(17) 0.0296(15) Uani 1 1 d . . . H86A H 0.3535 -0.0943 0.2779 0.036 Uiso 1 1 calc R . . C87 C 0.3000(3) -0.0294(2) 0.27613(18) 0.0341(16) Uani 1 1 d . . . H87A H 0.2580 -0.0355 0.2540 0.041 Uiso 1 1 calc R . . C88 C 0.3043(3) 0.0141(2) 0.29407(16) 0.0268(14) Uani 1 1 d . . . H88A H 0.2646 0.0378 0.2842 0.032 Uiso 1 1 calc R . . C89 C 0.3655(3) 0.02430(18) 0.32645(16) 0.0226(13) Uani 1 1 d . . . C90 C 0.3647(3) 0.07320(19) 0.34507(17) 0.0287(15) Uani 1 1 d . . . H90A H 0.4125 0.0748 0.3676 0.034 Uiso 1 1 calc R . . C91 C 0.2816(4) 0.0822(2) 0.3612(2) 0.0447(18) Uani 1 1 d . . . H91A H 0.2835 0.1136 0.3732 0.067 Uiso 1 1 calc R . . H91B H 0.2750 0.0581 0.3808 0.067 Uiso 1 1 calc R . . H91C H 0.2338 0.0805 0.3396 0.067 Uiso 1 1 calc R . . C92 C 0.3767(4) 0.1125(2) 0.3165(2) 0.0425(18) Uani 1 1 d . . . H92A H 0.4297 0.1074 0.3065 0.064 Uiso 1 1 calc R . . H92B H 0.3788 0.1430 0.3299 0.064 Uiso 1 1 calc R . . H92C H 0.3296 0.1123 0.2946 0.064 Uiso 1 1 calc R . . C93 C 0.4788(3) -0.09626(19) 0.33865(17) 0.0268(14) Uani 1 1 d . . . H93A H 0.5293 -0.0816 0.3550 0.032 Uiso 1 1 calc R . . C94 C 0.4377(4) -0.1288(2) 0.3653(2) 0.0478(19) Uani 1 1 d . . . H94A H 0.4774 -0.1539 0.3755 0.072 Uiso 1 1 calc R . . H94B H 0.3867 -0.1429 0.3503 0.072 Uiso 1 1 calc R . . H94C H 0.4227 -0.1105 0.3872 0.072 Uiso 1 1 calc R . . C95 C 0.5096(4) -0.1251(2) 0.30671(18) 0.0349(16) Uani 1 1 d . . . H95A H 0.5366 -0.1040 0.2899 0.052 Uiso 1 1 calc R . . H95B H 0.4616 -0.1410 0.2909 0.052 Uiso 1 1 calc R . . H95C H 0.5504 -0.1487 0.3187 0.052 Uiso 1 1 calc R . . C96 C 0.8879(3) 0.01725(19) 0.18231(17) 0.0299(15) Uani 1 1 d . . . H96A H 0.9066 -0.0114 0.1972 0.045 Uiso 1 1 calc R . . H96B H 0.9359 0.0387 0.1827 0.045 Uiso 1 1 calc R . . H96C H 0.8653 0.0087 0.1552 0.045 Uiso 1 1 calc R . . C97 C 0.8201(3) 0.04147(18) 0.20064(16) 0.0212(13) Uani 1 1 d . . . C98 C 0.7871(3) 0.08247(18) 0.18218(16) 0.0228(13) Uani 1 1 d . . . H98A H 0.8182 0.0948 0.1633 0.027 Uiso 1 1 calc R . . C99 C 0.7143(3) 0.10917(18) 0.18683(16) 0.0212(13) Uani 1 1 d . . . C100 C 0.6818(3) 0.1418(2) 0.15344(16) 0.0317(15) Uani 1 1 d . . . H10A H 0.6316 0.1583 0.1591 0.048 Uiso 1 1 calc R . . H10B H 0.6670 0.1234 0.1293 0.048 Uiso 1 1 calc R . . H10C H 0.7254 0.1649 0.1502 0.048 Uiso 1 1 calc R . . C101 C 0.5976(3) 0.13107(18) 0.21851(15) 0.0198(13) Uani 1 1 d . . . C102 C 0.5998(3) 0.17978(18) 0.22699(15) 0.0214(13) Uani 1 1 d . . . C103 C 0.5240(3) 0.20160(19) 0.23072(16) 0.0284(14) Uani 1 1 d . . . H10D H 0.5237 0.2346 0.2359 0.034 Uiso 1 1 calc R . . C104 C 0.4490(4) 0.1768(2) 0.22712(17) 0.0320(15) Uani 1 1 d . . . H10E H 0.3984 0.1925 0.2305 0.038 Uiso 1 1 calc R . . C105 C 0.4476(3) 0.1296(2) 0.21869(17) 0.0280(14) Uani 1 1 d . . . H10F H 0.3956 0.1130 0.2158 0.034 Uiso 1 1 calc R . . C106 C 0.5217(3) 0.10501(19) 0.21418(16) 0.0226(13) Uani 1 1 d . . . C107 C 0.5197(3) 0.05297(19) 0.20449(17) 0.0256(14) Uani 1 1 d . . . H10G H 0.5746 0.0392 0.2174 0.031 Uiso 1 1 calc R . . C108 C 0.5138(4) 0.0451(2) 0.16054(19) 0.0485(19) Uani 1 1 d . . . H10H H 0.5133 0.0112 0.1550 0.073 Uiso 1 1 calc R . . H10I H 0.5625 0.0597 0.1515 0.073 Uiso 1 1 calc R . . H10J H 0.4618 0.0595 0.1468 0.073 Uiso 1 1 calc R . . C109 C 0.4498(3) 0.0258(2) 0.2198(2) 0.0405(17) Uani 1 1 d . . . H10K H 0.4529 -0.0077 0.2129 0.061 Uiso 1 1 calc R . . H10L H 0.3948 0.0385 0.2080 0.061 Uiso 1 1 calc R . . H10M H 0.4569 0.0290 0.2484 0.061 Uiso 1 1 calc R . . C110 C 0.6806(3) 0.20904(18) 0.23330(16) 0.0254(14) Uani 1 1 d . . . H11B H 0.7272 0.1882 0.2275 0.031 Uiso 1 1 calc R . . C111 C 0.7037(3) 0.22512(19) 0.27600(16) 0.0303(15) Uani 1 1 d . . . H11C H 0.7072 0.1975 0.2933 0.045 Uiso 1 1 calc R . . H11D H 0.6603 0.2468 0.2824 0.045 Uiso 1 1 calc R . . H11E H 0.7582 0.2414 0.2796 0.045 Uiso 1 1 calc R . . C112 C 0.6757(4) 0.2516(2) 0.20542(19) 0.0408(17) Uani 1 1 d . . . H11F H 0.6611 0.2406 0.1783 0.061 Uiso 1 1 calc R . . H11G H 0.7305 0.2676 0.2089 0.061 Uiso 1 1 calc R . . H11H H 0.6325 0.2736 0.2113 0.061 Uiso 1 1 calc R . . C113 C 0.8187(3) -0.02510(18) 0.24347(16) 0.0211(13) Uani 1 1 d . . . C114 C 0.8950(3) -0.03582(19) 0.26751(16) 0.0240(13) Uani 1 1 d . . . C115 C 0.9125(4) -0.0831(2) 0.27737(18) 0.0313(15) Uani 1 1 d . . . H11I H 0.9638 -0.0911 0.2939 0.038 Uiso 1 1 calc R . . C116 C 0.8558(4) -0.1185(2) 0.26330(18) 0.0362(16) Uani 1 1 d . . . H11J H 0.8684 -0.1505 0.2703 0.043 Uiso 1 1 calc R . . C117 C 0.7815(4) -0.10742(19) 0.23931(17) 0.0283(14) Uani 1 1 d . . . H11K H 0.7432 -0.1320 0.2299 0.034 Uiso 1 1 calc R . . C118 C 0.7610(3) -0.06124(19) 0.22847(16) 0.0241(14) Uani 1 1 d . . . C119 C 0.6796(3) -0.04979(19) 0.20067(17) 0.0256(14) Uani 1 1 d . . . H11L H 0.6620 -0.0172 0.2071 0.031 Uiso 1 1 calc R . . C120 C 0.6923(4) -0.0496(2) 0.15788(18) 0.0391(17) Uani 1 1 d . . . H12A H 0.6390 -0.0418 0.1410 0.059 Uiso 1 1 calc R . . H12B H 0.7111 -0.0810 0.1509 0.059 Uiso 1 1 calc R . . H12C H 0.7350 -0.0261 0.1543 0.059 Uiso 1 1 calc R . . C121 C 0.6068(4) -0.0836(2) 0.2052(2) 0.0463(18) Uani 1 1 d . . . H12D H 0.5562 -0.0744 0.1869 0.069 Uiso 1 1 calc R . . H12E H 0.5952 -0.0820 0.2321 0.069 Uiso 1 1 calc R . . H12F H 0.6226 -0.1160 0.1994 0.069 Uiso 1 1 calc R . . C122 C 0.9616(3) 0.0009(2) 0.28253(17) 0.0284(14) Uani 1 1 d . . . H12G H 0.9417 0.0322 0.2713 0.034 Uiso 1 1 calc R . . C123 C 0.9737(3) 0.0048(2) 0.32740(16) 0.0349(16) Uani 1 1 d . . . H12H H 0.9196 0.0124 0.3355 0.052 Uiso 1 1 calc R . . H12I H 1.0145 0.0298 0.3362 0.052 Uiso 1 1 calc R . . H12J H 0.9947 -0.0253 0.3391 0.052 Uiso 1 1 calc R . . C124 C 1.0468(3) -0.0101(2) 0.26958(19) 0.0380(17) Uani 1 1 d . . . H12K H 1.0390 -0.0121 0.2409 0.057 Uiso 1 1 calc R . . H12L H 1.0685 -0.0403 0.2810 0.057 Uiso 1 1 calc R . . H12M H 1.0871 0.0151 0.2786 0.057 Uiso 1 1 calc R . . C125 C 0.2309(6) 0.2388(3) 0.1702(3) 0.072(3) Uani 1 1 d . . . C126 C 0.2906(4) 0.2709(2) 0.1868(3) 0.051(2) Uani 1 1 d . . . H12N H 0.3255 0.2869 0.1713 0.062 Uiso 1 1 calc R . . C127 C 0.2982(5) 0.2790(3) 0.2257(3) 0.065(2) Uani 1 1 d . . . H12O H 0.3396 0.3012 0.2369 0.078 Uiso 1 1 calc R . . C128 C 0.2493(7) 0.2570(4) 0.2511(3) 0.101(4) Uani 1 1 d . . . H12P H 0.2563 0.2628 0.2785 0.121 Uiso 1 1 calc R . . C129 C 0.1960(7) 0.2290(5) 0.2335(4) 0.123(5) Uani 1 1 d . . . H12Q H 0.1595 0.2151 0.2492 0.148 Uiso 1 1 calc R . . C130 C 0.1817(5) 0.2152(3) 0.1948(4) 0.099(4) Uani 1 1 d . . . H13D H 0.1418 0.1915 0.1852 0.119 Uiso 1 1 calc R . . C131 C 0.2190(6) 0.2302(3) 0.1295(3) 0.118(4) Uani 1 1 d . . . H13E H 0.2585 0.2495 0.1175 0.177 Uiso 1 1 calc R . . H13F H 0.1610 0.2384 0.1178 0.177 Uiso 1 1 calc R . . H13G H 0.2291 0.1967 0.1248 0.177 Uiso 1 1 calc R . . C132 C 0.9490(6) 0.1651(5) 0.6488(3) 0.117(5) Uani 1 1 d . . . C133 C 0.9384(6) 0.1203(4) 0.6248(2) 0.080(3) Uani 1 1 d . . . H13H H 0.9745 0.1110 0.6070 0.097 Uiso 1 1 calc R . . C134 C 0.8682(8) 0.0940(5) 0.6320(3) 0.127(5) Uani 1 1 d . . . H13J H 0.8602 0.0664 0.6162 0.152 Uiso 1 1 calc R . . C135 C 0.8161(6) 0.0975(4) 0.6528(3) 0.103(4) Uani 1 1 d . . . H13K H 0.7716 0.0759 0.6544 0.124 Uiso 1 1 calc R . . C136 C 0.8336(7) 0.1419(4) 0.6760(3) 0.085(3) Uani 1 1 d . . . H13L H 0.7969 0.1486 0.6942 0.102 Uiso 1 1 calc R . . C137 C 0.8943(5) 0.1731(3) 0.6741(2) 0.063(2) Uani 1 1 d . . . H13M H 0.8995 0.2005 0.6902 0.075 Uiso 1 1 calc R . . C138 C 1.0148(6) 0.1938(5) 0.6465(3) 0.174(7) Uani 1 1 d . . . H13N H 1.0133 0.2208 0.6642 0.261 Uiso 1 1 calc R . . H13O H 1.0113 0.2052 0.6195 0.261 Uiso 1 1 calc R . . H13P H 1.0676 0.1763 0.6541 0.261 Uiso 1 1 calc R . . C139 C 0.3995(6) 0.2692(4) 0.5527(3) 0.086(3) Uani 1 1 d U . . C140 C 0.4421(6) 0.2477(4) 0.5838(4) 0.110(3) Uani 1 1 d U . . H14A H 0.4581 0.2156 0.5819 0.132 Uiso 1 1 calc R . . C141 C 0.4615(6) 0.2688(4) 0.6152(3) 0.099(3) Uani 1 1 d U . . H14B H 0.4937 0.2521 0.6364 0.119 Uiso 1 1 calc R . . C142 C 0.4399(5) 0.3142(4) 0.6217(3) 0.081(2) Uani 1 1 d U . . H14C H 0.4572 0.3282 0.6467 0.097 Uiso 1 1 calc R . . C143 C 0.3926(5) 0.3401(3) 0.5918(3) 0.081(2) Uani 1 1 d U . . H14D H 0.3743 0.3715 0.5954 0.097 Uiso 1 1 calc R . . C144 C 0.3727(4) 0.3148(3) 0.5534(3) 0.075(2) Uani 1 1 d U . . H14E H 0.3429 0.3297 0.5307 0.091 Uiso 1 1 calc R . . C145 C 0.3886(8) 0.2361(5) 0.5215(4) 0.192(6) Uani 1 1 d U . . H14G H 0.4152 0.2061 0.5307 0.288 Uiso 1 1 calc R . . H14H H 0.4148 0.2483 0.4998 0.288 Uiso 1 1 calc R . . H14I H 0.3283 0.2310 0.5124 0.288 Uiso 1 1 calc R . . C146 C 0.8359(5) 0.5808(2) 0.3761(2) 0.0510(19) Uani 1 1 d . . . C147 C 0.9118(5) 0.5972(2) 0.3690(3) 0.063(2) Uani 1 1 d . . . H14J H 0.9530 0.6068 0.3904 0.076 Uiso 1 1 calc R . . C148 C 0.9298(5) 0.6002(3) 0.3323(4) 0.075(3) Uani 1 1 d . . . H14K H 0.9828 0.6123 0.3281 0.090 Uiso 1 1 calc R . . C149 C 0.8711(6) 0.5857(3) 0.3012(3) 0.079(3) Uani 1 1 d . . . H14L H 0.8833 0.5878 0.2752 0.095 Uiso 1 1 calc R . . C150 C 0.7939(5) 0.5679(3) 0.3075(2) 0.065(2) Uani 1 1 d . . . H15A H 0.7531 0.5573 0.2863 0.078 Uiso 1 1 calc R . . C151 C 0.7786(4) 0.5662(3) 0.3446(2) 0.052(2) Uani 1 1 d . . . H15B H 0.7257 0.5544 0.3491 0.062 Uiso 1 1 calc R . . C152 C 0.8163(6) 0.5775(3) 0.4169(2) 0.097(3) Uani 1 1 d . . . H15C H 0.8644 0.5893 0.4355 0.146 Uiso 1 1 calc R . . H15D H 0.8054 0.5445 0.4229 0.146 Uiso 1 1 calc R . . H15E H 0.7663 0.5966 0.4188 0.146 Uiso 1 1 calc R . . C153 C 0.5405(10) 0.4839(6) 0.5554(5) 0.076(5) Uiso 0.50 1 d P . . C154 C 0.5554(7) 0.5181(4) 0.5265(4) 0.110(4) Uiso 1 1 d . . . C155 C 0.5684(10) 0.5551(5) 0.4900(5) 0.064(4) Uiso 0.50 1 d P . . C156 C 0.5239(8) 0.5495(4) 0.4590(4) 0.129(4) Uiso 1 1 d . . . C157 C 0.5207(10) 0.5167(5) 0.4968(6) 0.063(5) Uiso 0.50 1 d P . . 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 0.01337(14) 0.02147(16) 0.01991(17) -0.00039(13) 0.00641(12) -0.00145(11) Sm2 0.01322(14) 0.02032(15) 0.01767(16) -0.00008(13) 0.00524(12) 0.00163(11) Sm3 0.01474(14) 0.02051(15) 0.01559(16) 0.00098(13) 0.00550(12) -0.00099(12) Sm4 0.01627(15) 0.02204(16) 0.01384(16) 0.00081(13) 0.00536(12) 0.00043(12) Cl1 0.0213(7) 0.0302(8) 0.0422(10) -0.0155(7) 0.0141(7) -0.0067(6) Cl2 0.0224(7) 0.0307(8) 0.0460(10) 0.0199(8) 0.0179(7) 0.0113(6) Cl3 0.0181(7) 0.0526(10) 0.0170(8) 0.0000(7) 0.0035(6) 0.0064(6) Cl4 0.0382(8) 0.0256(8) 0.0211(8) -0.0046(7) 0.0112(7) -0.0091(6) Cl5 0.0386(9) 0.0287(8) 0.0262(9) 0.0093(7) 0.0184(7) 0.0147(7) Cl6 0.0161(7) 0.0545(10) 0.0175(8) 0.0076(7) 0.0026(6) -0.0036(6) Al1 0.0178(9) 0.0244(9) 0.0230(10) -0.0037(8) 0.0060(8) -0.0038(7) Al2 0.0216(9) 0.0270(10) 0.0246(11) -0.0038(8) 0.0084(8) -0.0031(7) N1 0.025(3) 0.024(3) 0.027(3) 0.000(2) 0.011(2) -0.004(2) N2 0.022(3) 0.029(3) 0.020(3) -0.005(2) 0.010(2) -0.004(2) N3 0.023(3) 0.021(3) 0.016(3) 0.001(2) 0.004(2) 0.0022(19) N4 0.015(2) 0.020(2) 0.015(3) -0.004(2) 0.003(2) 0.0001(18) N5 0.017(2) 0.026(3) 0.014(3) -0.001(2) 0.004(2) 0.0018(19) N6 0.011(2) 0.022(2) 0.018(3) 0.001(2) 0.004(2) 0.0027(18) N7 0.013(2) 0.021(2) 0.019(3) -0.002(2) 0.003(2) 0.0035(18) N8 0.016(2) 0.024(3) 0.015(3) 0.002(2) 0.003(2) -0.0029(19) C1 0.022(3) 0.022(3) 0.025(4) 0.001(3) 0.007(3) -0.004(2) C2 0.024(3) 0.020(3) 0.023(4) -0.004(3) 0.006(3) -0.002(2) C3 0.044(4) 0.038(4) 0.031(4) -0.002(3) 0.015(3) -0.007(3) C4 0.029(3) 0.042(4) 0.047(4) -0.001(3) 0.014(3) -0.002(3) C5 0.020(3) 0.018(3) 0.016(3) 0.000(3) 0.004(3) 0.003(2) C6 0.017(3) 0.023(3) 0.030(4) -0.003(3) 0.010(3) -0.001(2) C7 0.022(3) 0.056(4) 0.044(4) -0.016(4) 0.004(3) 0.003(3) C8 0.039(4) 0.051(4) 0.030(4) 0.002(3) 0.009(3) -0.020(3) C9 0.017(3) 0.044(4) 0.061(5) -0.006(4) 0.010(3) 0.003(3) C10 0.019(3) 0.027(3) 0.034(4) -0.005(3) 0.005(3) 0.000(2) C11 0.019(3) 0.041(4) 0.040(4) -0.009(3) 0.016(3) -0.007(3) C12 0.032(3) 0.030(3) 0.027(4) -0.007(3) 0.014(3) -0.013(3) C13 0.043(4) 0.039(4) 0.059(5) -0.009(4) 0.030(4) -0.016(3) C14 0.029(3) 0.025(3) 0.037(4) -0.006(3) 0.020(3) -0.012(3) C15 0.037(4) 0.036(4) 0.033(4) -0.007(3) 0.025(3) -0.014(3) C16 0.061(5) 0.026(4) 0.057(5) -0.013(4) 0.039(4) -0.016(3) C17 0.047(4) 0.024(4) 0.065(5) 0.003(4) 0.032(4) -0.003(3) C18 0.043(4) 0.036(4) 0.041(4) 0.008(3) 0.023(3) -0.006(3) C19 0.033(4) 0.023(3) 0.035(4) 0.001(3) 0.021(3) -0.011(3) C20 0.038(4) 0.028(3) 0.022(4) 0.005(3) 0.005(3) -0.003(3) C21 0.061(5) 0.064(5) 0.046(5) -0.013(4) 0.020(4) -0.002(4) C22 0.045(4) 0.050(4) 0.046(5) 0.014(4) -0.001(4) -0.002(3) C23 0.060(5) 0.041(4) 0.035(4) -0.009(3) 0.017(4) -0.026(3) C24 0.050(5) 0.108(7) 0.060(6) -0.012(5) 0.011(4) -0.031(5) C25 0.063(5) 0.068(5) 0.039(5) -0.015(4) 0.016(4) -0.031(4) C26 0.013(3) 0.036(4) 0.023(4) 0.000(3) 0.000(3) 0.003(2) C27 0.016(3) 0.034(4) 0.028(4) 0.004(3) 0.001(3) 0.005(2) C28 0.042(4) 0.037(4) 0.031(4) 0.006(3) 0.004(3) 0.008(3) C29 0.071(5) 0.051(5) 0.021(4) 0.014(4) 0.008(4) 0.010(4) C30 0.047(4) 0.055(5) 0.022(4) -0.004(4) 0.000(3) 0.009(3) C31 0.015(3) 0.046(4) 0.023(4) -0.003(3) -0.004(3) 0.008(3) C32 0.023(3) 0.025(3) 0.027(4) 0.001(3) 0.007(3) 0.002(2) C33 0.042(4) 0.039(4) 0.052(5) 0.002(4) 0.019(4) 0.014(3) C34 0.027(3) 0.030(3) 0.036(4) 0.004(3) 0.008(3) -0.003(3) C35 0.019(3) 0.045(4) 0.027(4) -0.008(3) 0.003(3) 0.002(3) C36 0.024(4) 0.062(5) 0.059(5) -0.023(4) 0.000(3) -0.007(3) C37 0.034(4) 0.051(4) 0.038(4) -0.008(4) 0.004(3) 0.004(3) C38 0.026(3) 0.052(4) 0.029(4) 0.002(3) -0.001(3) 0.023(3) C39 0.018(3) 0.020(3) 0.030(4) -0.005(3) 0.006(3) 0.007(2) C40 0.013(3) 0.038(4) 0.023(4) -0.004(3) 0.007(3) 0.003(2) C41 0.018(3) 0.024(3) 0.022(3) -0.007(3) 0.003(3) -0.006(2) C42 0.021(3) 0.051(4) 0.022(4) -0.002(3) 0.008(3) 0.002(3) C43 0.015(3) 0.029(3) 0.013(3) -0.009(3) 0.004(2) 0.002(2) C44 0.018(3) 0.027(3) 0.026(4) -0.002(3) 0.008(3) 0.005(2) C45 0.023(3) 0.039(4) 0.037(4) -0.013(3) 0.010(3) -0.010(3) C46 0.024(3) 0.052(4) 0.027(4) -0.011(4) -0.004(3) -0.002(3) C47 0.029(3) 0.038(4) 0.019(3) -0.002(3) -0.005(3) 0.001(3) C48 0.021(3) 0.027(3) 0.023(3) -0.002(3) 0.006(3) 0.004(2) C49 0.034(3) 0.032(3) 0.012(3) 0.001(3) -0.001(3) -0.007(3) C50 0.046(4) 0.048(4) 0.033(4) 0.007(4) 0.009(3) -0.007(3) C51 0.057(4) 0.028(4) 0.040(4) 0.003(3) 0.009(4) 0.008(3) C52 0.038(4) 0.028(4) 0.038(4) -0.007(3) -0.001(3) -0.012(3) C53 0.071(5) 0.032(4) 0.050(5) -0.007(4) 0.025(4) -0.012(3) C54 0.044(5) 0.037(4) 0.138(9) 0.002(5) 0.022(5) 0.005(3) C55 0.021(3) 0.029(3) 0.018(3) 0.008(3) 0.006(3) 0.014(3) C56 0.017(3) 0.037(4) 0.023(4) 0.002(3) 0.004(3) 0.012(3) C57 0.028(3) 0.058(4) 0.019(4) 0.003(3) 0.001(3) 0.015(3) C58 0.031(4) 0.065(5) 0.020(4) 0.020(4) 0.010(3) 0.019(3) C59 0.031(4) 0.045(4) 0.041(5) 0.021(4) 0.010(3) 0.013(3) C60 0.024(3) 0.028(3) 0.029(4) 0.006(3) 0.008(3) 0.010(3) C61 0.030(3) 0.025(3) 0.048(4) 0.007(3) 0.014(3) 0.005(3) C62 0.054(5) 0.046(4) 0.074(6) -0.014(4) 0.013(4) 0.006(4) C63 0.052(5) 0.054(5) 0.058(5) 0.016(4) 0.014(4) -0.016(4) C64 0.021(3) 0.036(4) 0.024(4) 0.001(3) -0.001(3) 0.004(3) C65 0.029(4) 0.049(4) 0.040(4) -0.001(4) -0.004(3) 0.000(3) C66 0.030(3) 0.043(4) 0.025(4) -0.007(3) 0.002(3) 0.000(3) C67 0.011(3) 0.056(4) 0.028(4) -0.001(3) 0.005(3) -0.006(3) C68 0.016(3) 0.026(3) 0.029(4) -0.004(3) 0.009(3) -0.002(2) C69 0.017(3) 0.039(4) 0.013(3) 0.002(3) 0.005(3) -0.004(2) C70 0.024(3) 0.016(3) 0.016(3) -0.002(3) 0.003(3) 0.002(2) C71 0.032(3) 0.036(4) 0.017(3) 0.007(3) 0.005(3) -0.003(3) C72 0.019(3) 0.017(3) 0.020(3) 0.008(3) 0.003(3) 0.004(2) C73 0.022(3) 0.021(3) 0.015(3) 0.003(3) 0.002(3) -0.001(2) C74 0.019(3) 0.028(3) 0.027(4) 0.005(3) -0.003(3) 0.004(2) C75 0.017(3) 0.035(4) 0.041(4) 0.006(3) 0.000(3) 0.008(3) C76 0.025(3) 0.028(3) 0.035(4) 0.000(3) 0.003(3) 0.013(3) C77 0.020(3) 0.018(3) 0.022(3) 0.008(3) 0.003(3) 0.006(2) C78 0.026(3) 0.022(3) 0.021(3) -0.002(3) 0.004(3) 0.006(2) C79 0.033(4) 0.039(4) 0.035(4) -0.009(3) 0.005(3) 0.003(3) C80 0.050(4) 0.032(4) 0.047(5) -0.009(3) 0.009(4) -0.007(3) C81 0.018(3) 0.027(3) 0.023(3) -0.001(3) 0.004(3) 0.003(2) C82 0.032(3) 0.037(4) 0.024(4) -0.005(3) 0.003(3) -0.001(3) C83 0.019(3) 0.030(3) 0.021(3) -0.004(3) 0.001(3) -0.001(2) C84 0.021(3) 0.028(3) 0.013(3) -0.002(3) 0.009(3) -0.010(2) C85 0.018(3) 0.031(3) 0.019(3) -0.003(3) 0.008(3) -0.005(2) C86 0.027(3) 0.031(4) 0.031(4) -0.006(3) 0.005(3) -0.005(3) C87 0.028(3) 0.046(4) 0.025(4) -0.003(3) -0.008(3) -0.008(3) C88 0.020(3) 0.035(4) 0.023(4) -0.001(3) -0.003(3) 0.004(3) C89 0.013(3) 0.030(3) 0.026(4) 0.001(3) 0.007(3) 0.000(2) C90 0.020(3) 0.035(4) 0.030(4) -0.008(3) -0.001(3) 0.007(3) C91 0.032(4) 0.050(4) 0.055(5) -0.003(4) 0.014(3) 0.013(3) C92 0.033(4) 0.029(4) 0.065(5) 0.003(4) 0.009(4) -0.001(3) C93 0.029(3) 0.029(3) 0.022(4) -0.004(3) 0.004(3) -0.008(3) C94 0.059(5) 0.039(4) 0.050(5) 0.013(4) 0.021(4) 0.006(3) C95 0.035(4) 0.032(4) 0.040(4) -0.011(3) 0.012(3) 0.007(3) C96 0.028(3) 0.038(4) 0.026(4) 0.001(3) 0.015(3) 0.008(3) C97 0.015(3) 0.023(3) 0.026(4) -0.003(3) 0.004(3) 0.002(2) C98 0.021(3) 0.031(3) 0.018(3) 0.005(3) 0.009(3) -0.002(2) C99 0.023(3) 0.022(3) 0.017(3) 0.002(3) 0.001(3) 0.001(2) C100 0.038(4) 0.041(4) 0.018(3) 0.010(3) 0.009(3) 0.014(3) C101 0.025(3) 0.024(3) 0.010(3) 0.003(3) 0.005(2) 0.007(2) C102 0.023(3) 0.028(3) 0.011(3) 0.005(3) -0.001(3) 0.007(2) C103 0.037(4) 0.026(3) 0.023(4) -0.002(3) 0.004(3) 0.013(3) C104 0.026(3) 0.041(4) 0.028(4) 0.000(3) 0.004(3) 0.011(3) C105 0.022(3) 0.031(4) 0.030(4) 0.003(3) 0.002(3) 0.003(3) C106 0.018(3) 0.029(3) 0.018(3) 0.002(3) -0.005(3) 0.004(2) C107 0.019(3) 0.032(3) 0.024(4) -0.001(3) -0.003(3) 0.003(2) C108 0.056(5) 0.047(4) 0.040(5) -0.019(4) 0.002(4) 0.001(3) C109 0.022(3) 0.040(4) 0.057(5) 0.002(4) 0.001(3) -0.005(3) C110 0.032(3) 0.021(3) 0.025(4) 0.003(3) 0.012(3) -0.003(3) C111 0.033(3) 0.029(3) 0.030(4) -0.004(3) 0.008(3) 0.005(3) C112 0.051(4) 0.029(4) 0.044(5) 0.009(3) 0.011(4) -0.005(3) C113 0.022(3) 0.023(3) 0.022(3) 0.001(3) 0.013(3) 0.006(2) C114 0.024(3) 0.028(3) 0.021(3) -0.001(3) 0.007(3) 0.006(3) C115 0.030(3) 0.038(4) 0.028(4) 0.000(3) 0.011(3) 0.011(3) C116 0.050(4) 0.026(4) 0.035(4) 0.005(3) 0.017(3) 0.011(3) C117 0.036(4) 0.019(3) 0.033(4) -0.003(3) 0.015(3) 0.004(3) C118 0.024(3) 0.033(3) 0.020(3) -0.006(3) 0.018(3) 0.004(3) C119 0.025(3) 0.021(3) 0.034(4) -0.007(3) 0.014(3) -0.001(2) C120 0.037(4) 0.041(4) 0.039(4) -0.002(3) 0.006(3) 0.011(3) C121 0.034(4) 0.052(4) 0.054(5) -0.015(4) 0.009(3) -0.016(3) C122 0.019(3) 0.035(4) 0.031(4) -0.001(3) 0.001(3) 0.006(3) C123 0.032(4) 0.045(4) 0.024(4) -0.016(3) -0.005(3) 0.010(3) C124 0.025(3) 0.043(4) 0.046(5) -0.004(3) 0.005(3) 0.009(3) C125 0.074(6) 0.065(6) 0.063(6) -0.005(5) -0.026(5) 0.014(5) C126 0.045(4) 0.031(4) 0.075(6) 0.008(4) -0.003(4) 0.003(3) C127 0.065(6) 0.045(5) 0.089(8) -0.003(5) 0.028(6) 0.013(4) C128 0.078(8) 0.113(9) 0.096(9) -0.010(8) -0.028(7) 0.046(7) C129 0.067(8) 0.193(14) 0.101(10) 0.053(10) -0.013(7) -0.006(8) C130 0.058(6) 0.091(7) 0.137(10) 0.023(8) -0.021(7) -0.058(5) C131 0.123(9) 0.115(9) 0.112(10) -0.021(8) 0.007(8) 0.031(7) C132 0.078(7) 0.179(12) 0.103(9) 0.111(9) 0.040(7) 0.075(8) C133 0.104(8) 0.121(8) 0.024(5) 0.013(5) 0.031(5) 0.093(7) C134 0.118(10) 0.210(14) 0.057(7) 0.080(8) 0.027(7) 0.111(10) C135 0.080(8) 0.132(10) 0.096(9) 0.041(8) 0.009(7) 0.040(7) C136 0.120(9) 0.088(8) 0.045(6) -0.010(6) 0.006(6) 0.043(6) C137 0.064(6) 0.094(7) 0.034(5) 0.015(5) 0.019(5) 0.035(5) C138 0.041(6) 0.307(18) 0.172(13) 0.179(13) 0.011(7) 0.043(8) C139 0.054(5) 0.134(7) 0.074(5) -0.038(6) 0.026(4) -0.050(5) C140 0.070(5) 0.140(7) 0.121(7) -0.002(6) 0.022(6) -0.046(5) C141 0.070(5) 0.131(7) 0.099(6) 0.008(6) 0.022(5) -0.041(5) C142 0.062(5) 0.115(6) 0.074(5) -0.020(5) 0.035(4) -0.033(5) C143 0.043(4) 0.104(6) 0.103(6) 0.002(5) 0.032(4) -0.020(4) C144 0.025(4) 0.121(6) 0.081(5) 0.025(5) 0.011(4) -0.021(4) C145 0.196(11) 0.225(12) 0.180(12) -0.114(10) 0.107(10) -0.074(10) C146 0.053(5) 0.053(5) 0.043(5) -0.011(4) -0.002(4) 0.009(4) C147 0.042(5) 0.042(5) 0.097(8) -0.024(5) -0.015(5) -0.001(4) C148 0.046(5) 0.039(5) 0.147(10) -0.022(6) 0.037(6) -0.010(4) C149 0.116(8) 0.061(6) 0.072(7) 0.005(5) 0.052(6) 0.010(6) C150 0.062(5) 0.094(6) 0.038(5) -0.007(5) 0.005(4) -0.010(5) C151 0.029(4) 0.076(5) 0.047(5) -0.005(5) -0.002(4) -0.008(4) C152 0.135(9) 0.100(7) 0.052(6) -0.005(6) 0.000(6) 0.006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N1 2.355(4) . ? Sm1 N2 2.374(4) . ? Sm1 C1 2.759(6) . ? Sm1 Cl2 2.7633(14) . ? Sm1 Cl1 2.7719(14) . ? Sm1 Cl3 2.7795(13) . ? Sm1 Sm2 3.8856(4) . ? Sm1 H101 2.61(5) . ? Sm1 H102 2.57(5) . ? Sm2 N4 2.373(4) . ? Sm2 N3 2.379(4) . ? Sm2 C5 2.728(5) . ? Sm2 Cl1 2.7489(13) . ? Sm2 Cl2 2.7710(13) . ? Sm2 Cl3 2.7829(14) . ? Sm2 H501 2.56(5) . ? Sm2 H502 2.57(5) . ? Sm3 N5 2.362(4) . ? Sm3 N6 2.394(4) . ? Sm3 C6 2.722(6) . ? Sm3 Cl6 2.7582(13) . ? Sm3 Cl4 2.7624(14) . ? Sm3 Cl5 2.7796(14) . ? Sm3 Sm4 3.8832(4) . ? Sm3 H601 2.47(5) . ? Sm3 H602 2.56(5) . ? Sm3 H603 2.57(5) . ? Sm4 N8 2.355(4) . ? Sm4 N7 2.395(4) . ? Sm4 C2 2.723(5) . ? Sm4 Cl4 2.7719(13) . ? Sm4 Cl5 2.7756(13) . ? Sm4 Cl6 2.7806(14) . ? Sm4 H201 2.57(5) . ? Sm4 H202 2.56(5) . ? Sm4 H203 2.58(5) . ? Al1 C8 1.976(6) . ? Al1 C7 1.983(5) . ? Al1 C6 2.035(6) . ? Al1 C5 2.035(6) . ? Al2 C4 1.982(6) . ? Al2 C3 1.983(6) . ? Al2 C2 2.033(6) . ? Al2 C1 2.035(6) . ? N1 C12 1.353(7) . ? N1 C14 1.448(7) . ? N2 C10 1.346(6) . ? N2 C26 1.440(7) . ? N3 C39 1.331(6) . ? N3 C55 1.459(6) . ? N4 C41 1.346(6) . ? N4 C43 1.467(6) . ? N5 C68 1.357(7) . ? N5 C84 1.455(6) . ? N6 C70 1.327(6) . ? N6 C72 1.454(6) . ? N7 C99 1.337(6) . ? N7 C101 1.460(6) . ? N8 C97 1.339(6) . ? N8 C113 1.456(6) . ? C1 H101 0.979(5) . ? C1 H102 0.980(5) . ? C1 H103 0.979(5) . ? C2 H201 0.979(5) . ? C2 H202 0.979(5) . ? C2 H203 0.980(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H501 0.980(5) . ? C5 H502 0.980(5) . ? C5 H503 0.980(5) . ? C6 H601 0.980(5) . ? C6 H602 0.981(5) . ? C6 H603 0.980(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.510(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.400(8) . ? C11 C12 1.384(8) . ? C11 H11A 0.9500 . ? C12 C13 1.538(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.409(8) . ? C14 C15 1.410(8) . ? C15 C16 1.384(8) . ? C15 C23 1.526(9) . ? C16 C17 1.380(9) . ? C16 H16A 0.9500 . ? C17 C18 1.371(8) . ? C17 H17A 0.9500 . ? C18 C19 1.385(8) . ? C18 H18A 0.9500 . ? C19 C20 1.523(8) . ? C20 C22 1.522(8) . ? C20 C21 1.545(8) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.534(8) . ? C23 C24 1.544(8) . ? C23 H23A 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C31 1.409(7) . ? C26 C27 1.425(8) . ? C27 C28 1.386(8) . ? C27 C32 1.530(8) . ? C28 C29 1.369(8) . ? C28 H28A 0.9500 . ? C29 C30 1.385(8) . ? C29 H29A 0.9500 . ? C30 C31 1.380(8) . ? C30 H30A 0.9500 . ? C31 C35 1.505(8) . ? C32 C33 1.534(7) . ? C32 C34 1.539(7) . ? C32 H32A 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C37 1.525(7) . ? C35 C36 1.540(7) . ? C35 H35A 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.529(7) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.400(7) . ? C40 C41 1.385(7) . ? C40 H40A 0.9500 . ? C41 C42 1.508(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.404(7) . ? C43 C48 1.404(7) . ? C44 C45 1.400(8) . ? C44 C52 1.513(8) . ? C45 C46 1.381(8) . ? C45 H45A 0.9500 . ? C46 C47 1.365(7) . ? C46 H46A 0.9500 . ? C47 C48 1.397(7) . ? C47 H47A 0.9500 . ? C48 C49 1.520(7) . ? C49 C51 1.527(7) . ? C49 C50 1.552(7) . ? C49 H49A 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C54 1.525(8) . ? C52 C53 1.535(8) . ? C52 H52A 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.406(8) . ? C55 C60 1.408(7) . ? C56 C57 1.399(8) . ? C56 C64 1.534(7) . ? C57 C58 1.386(8) . ? C57 H57A 0.9500 . ? C58 C59 1.375(8) . ? C58 H58A 0.9500 . ? C59 C60 1.372(8) . ? C59 H59A 0.9500 . ? C60 C61 1.508(8) . ? C61 C62 1.518(8) . ? C61 C63 1.547(8) . ? C61 H61A 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C66 1.525(7) . ? C64 C65 1.538(7) . ? C64 H64A 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.529(7) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.383(7) . ? C69 C70 1.416(7) . ? C69 H69A 0.9500 . ? C70 C71 1.516(7) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C77 1.396(7) . ? C72 C73 1.413(7) . ? C73 C74 1.395(7) . ? C73 C81 1.524(7) . ? C74 C75 1.371(7) . ? C74 H74A 0.9500 . ? C75 C76 1.383(8) . ? C75 H75A 0.9500 . ? C76 C77 1.389(7) . ? C76 H76A 0.9500 . ? C77 C78 1.527(7) . ? C78 C80 1.520(7) . ? C78 C79 1.522(7) . ? C78 H78A 1.0000 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.529(7) . ? C81 C83 1.535(7) . ? C81 H81A 1.0000 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 C89 1.397(7) . ? C84 C85 1.418(7) . ? C85 C86 1.389(7) . ? C85 C93 1.529(7) . ? C86 C87 1.380(7) . ? C86 H86A 0.9500 . ? C87 C88 1.376(7) . ? C87 H87A 0.9500 . ? C88 C89 1.394(7) . ? C88 H88A 0.9500 . ? C89 C90 1.527(7) . ? C90 C92 1.521(8) . ? C90 C91 1.550(7) . ? C90 H90A 1.0000 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 C95 1.519(7) . ? C93 C94 1.527(7) . ? C93 H93A 1.0000 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 C97 1.512(7) . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 C98 1.387(7) . ? C98 C99 1.424(7) . ? C98 H98A 0.9500 . ? C99 C100 1.503(7) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? C101 C102 1.408(7) . ? C101 C106 1.412(7) . ? C102 C103 1.391(7) . ? C102 C110 1.526(7) . ? C103 C104 1.383(7) . ? C103 H10D 0.9500 . ? C104 C105 1.365(7) . ? C104 H10E 0.9500 . ? C105 C106 1.409(7) . ? C105 H10F 0.9500 . ? C106 C107 1.509(7) . ? C107 C108 1.523(8) . ? C107 C109 1.526(7) . ? C107 H10G 1.0000 . ? C108 H10H 0.9800 . ? C108 H10I 0.9800 . ? C108 H10J 0.9800 . ? C109 H10K 0.9800 . ? C109 H10L 0.9800 . ? C109 H10M 0.9800 . ? C110 C111 1.531(7) . ? C110 C112 1.536(7) . ? C110 H11B 1.0000 . ? C111 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C113 C114 1.397(7) . ? C113 C118 1.420(7) . ? C114 C115 1.398(7) . ? C114 C122 1.521(7) . ? C115 C116 1.388(8) . ? C115 H11I 0.9500 . ? C116 C117 1.375(8) . ? C116 H11J 0.9500 . ? C117 C118 1.384(7) . ? C117 H11K 0.9500 . ? C118 C119 1.526(7) . ? C119 C120 1.527(8) . ? C119 C121 1.540(7) . ? C119 H11L 1.0000 . ? C120 H12A 0.9800 . ? C120 H12B 0.9800 . ? C120 H12C 0.9800 . ? C121 H12D 0.9800 . ? C121 H12E 0.9800 . ? C121 H12F 0.9800 . ? C122 C123 1.536(7) . ? C122 C124 1.540(7) . ? C122 H12G 1.0000 . ? C123 H12H 0.9800 . ? C123 H12I 0.9800 . ? C123 H12J 0.9800 . ? C124 H12K 0.9800 . ? C124 H12L 0.9800 . ? C124 H12M 0.9800 . ? C125 C126 1.377(10) . ? C125 C131 1.411(12) . ? C125 C130 1.419(12) . ? C126 C127 1.350(10) . ? C126 H12N 0.9500 . ? C127 C128 1.416(13) . ? C127 H12O 0.9500 . ? C128 C129 1.248(13) . ? C128 H12P 0.9500 . ? C129 C130 1.376(14) . ? C129 H12Q 0.9500 . ? C130 H13D 0.9500 . ? C131 H13E 0.9800 . ? C131 H13F 0.9800 . ? C131 H13G 0.9800 . ? C132 C138 1.346(14) . ? C132 C137 1.358(11) . ? C132 C133 1.510(15) . ? C133 C134 1.406(15) . ? C133 H13H 0.9500 . ? C134 C135 1.196(12) . ? C134 H13J 0.9500 . ? C135 C136 1.490(13) . ? C135 H13K 0.9500 . ? C136 C137 1.326(11) . ? C136 H13L 0.9500 . ? C137 H13M 0.9500 . ? C138 H13N 0.9800 . ? C138 H13O 0.9800 . ? C138 H13P 0.9800 . ? C139 C140 1.325(14) . ? C139 C144 1.360(12) . ? C139 C145 1.418(13) . ? C140 C141 1.233(13) . ? C140 H14A 0.9500 . ? C141 C142 1.358(12) . ? C141 H14B 0.9500 . ? C142 C143 1.389(12) . ? C142 H14C 0.9500 . ? C143 C144 1.495(12) . ? C143 H14D 0.9500 . ? C144 H14E 0.9500 . ? C145 H14G 0.9800 . ? C145 H14H 0.9800 . ? C145 H14I 0.9800 . ? C146 C147 1.364(10) . ? C146 C151 1.372(9) . ? C146 C152 1.496(10) . ? C147 C148 1.348(11) . ? C147 H14J 0.9500 . ? C148 C149 1.374(11) . ? C148 H14K 0.9500 . ? C149 C150 1.390(10) . ? C149 H14L 0.9500 . ? C150 C151 1.343(9) . ? C150 H15A 0.9500 . ? C151 H15B 0.9500 . ? C152 H15C 0.9800 . ? C152 H15D 0.9800 . ? C152 H15E 0.9800 . ? C153 C156 1.431(18) 3_666 ? C153 C154 1.438(18) . ? C153 C157 1.91(3) 3_666 ? C154 C157 1.088(19) . ? C154 C157 1.671(19) 3_666 ? C154 C155 1.681(18) . ? C155 C156 1.196(17) . ? C155 C157 1.373(19) . ? C156 C153 1.431(18) 3_666 ? C156 C157 1.610(19) . ? C157 C157 1.20(3) 3_666 ? C157 C154 1.671(19) 3_666 ? C157 C153 1.91(3) 3_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sm1 N2 78.48(15) . . ? N1 Sm1 C1 91.67(15) . . ? N2 Sm1 C1 86.02(16) . . ? N1 Sm1 Cl2 158.89(12) . . ? N2 Sm1 Cl2 89.29(11) . . ? C1 Sm1 Cl2 104.71(12) . . ? N1 Sm1 Cl1 92.14(11) . . ? N2 Sm1 Cl1 113.43(11) . . ? C1 Sm1 Cl1 160.55(12) . . ? Cl2 Sm1 Cl1 76.88(4) . . ? N1 Sm1 Cl3 119.73(11) . . ? N2 Sm1 Cl3 160.11(11) . . ? C1 Sm1 Cl3 85.52(12) . . ? Cl2 Sm1 Cl3 75.53(4) . . ? Cl1 Sm1 Cl3 76.03(4) . . ? N1 Sm1 Sm2 133.66(10) . . ? N2 Sm1 Sm2 128.48(10) . . ? C1 Sm1 Sm2 122.97(11) . . ? Cl2 Sm1 Sm2 45.48(3) . . ? Cl1 Sm1 Sm2 45.02(3) . . ? Cl3 Sm1 Sm2 45.72(3) . . ? N1 Sm1 H101 106.2(8) . . ? N2 Sm1 H101 75.1(9) . . ? C1 Sm1 H101 20.76(12) . . ? Cl2 Sm1 H101 86.8(6) . . ? Cl1 Sm1 H101 161.2(10) . . ? Cl3 Sm1 H101 91.1(11) . . ? Sm2 Sm1 H101 116.3(10) . . ? N1 Sm1 H102 71.7(4) . . ? N2 Sm1 H102 76.9(10) . . ? C1 Sm1 H102 20.80(13) . . ? Cl2 Sm1 H102 122.5(6) . . ? Cl1 Sm1 H102 159.2(9) . . ? Cl3 Sm1 H102 100.3(8) . . ? Sm2 Sm1 H102 142.5(5) . . ? H101 Sm1 H102 35.7(9) . . ? N4 Sm2 N3 77.92(14) . . ? N4 Sm2 C5 90.37(15) . . ? N3 Sm2 C5 85.60(15) . . ? N4 Sm2 Cl1 95.99(10) . . ? N3 Sm2 Cl1 115.05(10) . . ? C5 Sm2 Cl1 159.23(11) . . ? N4 Sm2 Cl2 118.58(10) . . ? N3 Sm2 Cl2 159.54(11) . . ? C5 Sm2 Cl2 82.46(11) . . ? Cl1 Sm2 Cl2 77.13(4) . . ? N4 Sm2 Cl3 162.67(10) . . ? N3 Sm2 Cl3 91.12(11) . . ? C5 Sm2 Cl3 102.27(12) . . ? Cl1 Sm2 Cl3 76.35(4) . . ? Cl2 Sm2 Cl3 75.35(4) . . ? N4 Sm2 Sm1 136.21(9) . . ? N3 Sm2 Sm1 131.46(10) . . ? C5 Sm2 Sm1 119.29(11) . . ? Cl1 Sm2 Sm1 45.51(3) . . ? Cl2 Sm2 Sm1 45.32(3) . . ? Cl3 Sm2 Sm1 45.65(3) . . ? N4 Sm2 H501 72.5(6) . . ? N3 Sm2 H501 71.4(9) . . ? C5 Sm2 H501 21.04(12) . . ? Cl1 Sm2 H501 165.8(10) . . ? Cl2 Sm2 H501 100.7(6) . . ? Cl3 Sm2 H501 117.0(8) . . ? Sm1 Sm2 H501 140.31(18) . . ? N4 Sm2 H502 109.5(5) . . ? N3 Sm2 H502 81.7(11) . . ? C5 Sm2 H502 21.04(12) . . ? Cl1 Sm2 H502 152.3(8) . . ? Cl2 Sm2 H502 81.2(11) . . ? Cl3 Sm2 H502 81.7(3) . . ? Sm1 Sm2 H502 106.8(8) . . ? H501 Sm2 H502 37.1(8) . . ? N5 Sm3 N6 78.58(14) . . ? N5 Sm3 C6 89.30(15) . . ? N6 Sm3 C6 86.20(16) . . ? N5 Sm3 Cl6 161.66(10) . . ? N6 Sm3 Cl6 89.62(10) . . ? C6 Sm3 Cl6 104.03(12) . . ? N5 Sm3 Cl4 95.10(11) . . ? N6 Sm3 Cl4 115.55(10) . . ? C6 Sm3 Cl4 158.25(13) . . ? Cl6 Sm3 Cl4 77.23(4) . . ? N5 Sm3 Cl5 119.61(10) . . ? N6 Sm3 Cl5 158.22(10) . . ? C6 Sm3 Cl5 82.42(13) . . ? Cl6 Sm3 Cl5 75.31(4) . . ? Cl4 Sm3 Cl5 76.88(4) . . ? N5 Sm3 Sm4 136.25(10) . . ? N6 Sm3 Sm4 130.06(9) . . ? C6 Sm3 Sm4 120.49(12) . . ? Cl6 Sm3 Sm4 45.72(3) . . ? Cl4 Sm3 Sm4 45.54(3) . . ? Cl5 Sm3 Sm4 45.61(3) . . ? N5 Sm3 H601 108.0(6) . . ? N6 Sm3 H601 81.1(11) . . ? C6 Sm3 H601 21.04(16) . . ? Cl6 Sm3 H601 83.6(3) . . ? Cl4 Sm3 H601 154.2(10) . . ? Cl5 Sm3 H601 81.7(12) . . ? Sm4 Sm3 H601 108.7(9) . . ? N5 Sm3 H602 89.4(11) . . ? N6 Sm3 H602 106.9(3) . . ? C6 Sm3 H602 21.11(12) . . ? Cl6 Sm3 H602 107.6(11) . . ? Cl4 Sm3 H602 137.4(2) . . ? Cl5 Sm3 H602 64.3(6) . . ? Sm4 Sm3 H602 107.4(8) . . ? H601 Sm3 H602 35.6(9) . . ? N5 Sm3 H603 71.7(7) . . ? N6 Sm3 H603 71.9(9) . . ? C6 Sm3 H603 21.08(13) . . ? Cl6 Sm3 H603 118.2(9) . . ? Cl4 Sm3 H603 163.8(11) . . ? Cl5 Sm3 H603 101.1(5) . . ? Sm4 Sm3 H603 141.56(18) . . ? H601 Sm3 H603 36.4(9) . . ? H602 Sm3 H603 36.8(8) . . ? N8 Sm4 N7 77.83(14) . . ? N8 Sm4 C2 87.10(15) . . ? N7 Sm4 C2 86.49(16) . . ? N8 Sm4 Cl4 98.38(10) . . ? N7 Sm4 Cl4 115.61(10) . . ? C2 Sm4 Cl4 157.86(13) . . ? N8 Sm4 Cl5 163.31(10) . . ? N7 Sm4 Cl5 89.76(10) . . ? C2 Sm4 Cl5 103.42(12) . . ? Cl4 Sm4 Cl5 76.79(4) . . ? N8 Sm4 Cl6 119.85(10) . . ? N7 Sm4 Cl6 158.08(10) . . ? C2 Sm4 Cl6 81.95(13) . . ? Cl4 Sm4 Cl6 76.71(4) . . ? Cl5 Sm4 Cl6 75.02(4) . . ? N8 Sm4 Sm3 138.70(10) . . ? N7 Sm4 Sm3 130.29(9) . . ? C2 Sm4 Sm3 119.61(12) . . ? Cl4 Sm4 Sm3 45.34(3) . . ? Cl5 Sm4 Sm3 45.69(3) . . ? Cl6 Sm4 Sm3 45.25(3) . . ? N8 Sm4 H201 83.3(11) . . ? N7 Sm4 H201 105.8(5) . . ? C2 Sm4 H201 21.06(12) . . ? Cl4 Sm4 H201 138.0(3) . . ? Cl5 Sm4 H201 111.1(11) . . ? Cl6 Sm4 H201 66.7(8) . . ? Sm3 Sm4 H201 110.1(10) . . ? N8 Sm4 H202 71.4(8) . . ? N7 Sm4 H202 69.9(7) . . ? C2 Sm4 H202 21.08(12) . . ? Cl4 Sm4 H202 167.6(11) . . ? Cl5 Sm4 H202 115.0(10) . . ? Cl6 Sm4 H202 101.9(4) . . ? Sm3 Sm4 H202 140.4(3) . . ? H201 Sm4 H202 36.2(9) . . ? N8 Sm4 H203 107.1(4) . . ? N7 Sm4 H203 84.6(12) . . ? C2 Sm4 H203 21.07(12) . . ? Cl4 Sm4 H203 150.6(9) . . ? Cl5 Sm4 H203 82.4(2) . . ? Cl6 Sm4 H203 78.0(11) . . ? Sm3 Sm4 H203 105.4(8) . . ? H201 Sm4 H203 36.1(9) . . ? H202 Sm4 H203 36.5(9) . . ? Sm2 Cl1 Sm1 89.47(4) . . ? Sm1 Cl2 Sm2 89.19(4) . . ? Sm1 Cl3 Sm2 88.62(4) . . ? Sm3 Cl4 Sm4 89.12(4) . . ? Sm4 Cl5 Sm3 88.70(4) . . ? Sm3 Cl6 Sm4 89.03(4) . . ? C8 Al1 C7 114.7(3) . . ? C8 Al1 C6 109.3(3) . . ? C7 Al1 C6 107.2(2) . . ? C8 Al1 C5 108.1(2) . . ? C7 Al1 C5 110.0(2) . . ? C6 Al1 C5 107.3(2) . . ? C4 Al2 C3 114.3(3) . . ? C4 Al2 C2 109.9(2) . . ? C3 Al2 C2 106.6(3) . . ? C4 Al2 C1 108.4(3) . . ? C3 Al2 C1 111.7(2) . . ? C2 Al2 C1 105.6(2) . . ? C12 N1 C14 118.0(4) . . ? C12 N1 Sm1 124.2(3) . . ? C14 N1 Sm1 117.2(3) . . ? C10 N2 C26 118.5(4) . . ? C10 N2 Sm1 125.8(4) . . ? C26 N2 Sm1 115.4(3) . . ? C39 N3 C55 119.1(4) . . ? C39 N3 Sm2 127.5(4) . . ? C55 N3 Sm2 113.2(3) . . ? C41 N4 C43 116.2(4) . . ? C41 N4 Sm2 125.4(3) . . ? C43 N4 Sm2 117.6(3) . . ? C68 N5 C84 117.4(4) . . ? C68 N5 Sm3 123.9(3) . . ? C84 N5 Sm3 118.1(3) . . ? C70 N6 C72 118.7(4) . . ? C70 N6 Sm3 126.7(3) . . ? C72 N6 Sm3 114.3(3) . . ? C99 N7 C101 118.4(4) . . ? C99 N7 Sm4 127.3(3) . . ? C101 N7 Sm4 114.0(3) . . ? C97 N8 C113 118.1(4) . . ? C97 N8 Sm4 127.1(3) . . ? C113 N8 Sm4 114.5(3) . . ? Al2 C1 Sm1 177.5(3) . . ? Al2 C1 H101 107(3) . . ? Sm1 C1 H101 71(3) . . ? Al2 C1 H102 111(3) . . ? Sm1 C1 H102 68(3) . . ? H101 C1 H102 109(4) . . ? Al2 C1 H103 110(3) . . ? Sm1 C1 H103 72(3) . . ? H101 C1 H103 109(4) . . ? H102 C1 H103 111(4) . . ? Al2 C2 Sm4 176.4(3) . . ? Al2 C2 H201 111(3) . . ? Sm4 C2 H201 71(3) . . ? Al2 C2 H202 106(3) . . ? Sm4 C2 H202 70(3) . . ? H201 C2 H202 109(4) . . ? Al2 C2 H203 111(3) . . ? Sm4 C2 H203 71(3) . . ? H201 C2 H203 109(4) . . ? H202 C2 H203 111(4) . . ? Al2 C3 H3A 109.5 . . ? Al2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Al2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Al2 C4 H4A 109.5 . . ? Al2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Al2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Al1 C5 Sm2 177.9(3) . . ? Al1 C5 H501 108(3) . . ? Sm2 C5 H501 70(3) . . ? Al1 C5 H502 110(3) . . ? Sm2 C5 H502 70(3) . . ? H501 C5 H502 113(4) . . ? Al1 C5 H503 104(3) . . ? Sm2 C5 H503 77(3) . . ? H501 C5 H503 111(4) . . ? H502 C5 H503 110(4) . . ? Al1 C6 Sm3 178.1(3) . . ? Al1 C6 H601 117(3) . . ? Sm3 C6 H601 65(3) . . ? Al1 C6 H602 110(3) . . ? Sm3 C6 H602 70(3) . . ? H601 C6 H602 103(4) . . ? Al1 C6 H603 108(3) . . ? Sm3 C6 H603 71(3) . . ? H601 C6 H603 107(4) . . ? H602 C6 H603 112(4) . . ? Al1 C7 H7A 109.5 . . ? Al1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Al1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Al1 C8 H8A 109.5 . . ? Al1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Al1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 123.0(5) . . ? N2 C10 C9 121.2(5) . . ? C11 C10 C9 115.7(5) . . ? C12 C11 C10 130.5(5) . . ? C12 C11 H11A 114.7 . . ? C10 C11 H11A 114.7 . . ? N1 C12 C11 124.6(5) . . ? N1 C12 C13 119.4(5) . . ? C11 C12 C13 116.0(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 120.6(5) . . ? C19 C14 N1 119.9(5) . . ? C15 C14 N1 119.5(6) . . ? C16 C15 C14 118.4(6) . . ? C16 C15 C23 119.9(6) . . ? C14 C15 C23 121.6(6) . . ? C17 C16 C15 121.4(6) . . ? C17 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? C18 C17 C16 119.5(6) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C19 122.0(6) . . ? C17 C18 H18A 119.0 . . ? C19 C18 H18A 119.0 . . ? C18 C19 C14 118.0(6) . . ? C18 C19 C20 119.7(6) . . ? C14 C19 C20 122.2(5) . . ? C22 C20 C19 114.3(5) . . ? C22 C20 C21 110.5(5) . . ? C19 C20 C21 111.6(5) . . ? C22 C20 H20A 106.7 . . ? C19 C20 H20A 106.7 . . ? C21 C20 H20A 106.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C15 C23 C25 110.9(6) . . ? C15 C23 C24 111.8(5) . . ? C25 C23 C24 108.0(5) . . ? C15 C23 H23A 108.7 . . ? C25 C23 H23A 108.7 . . ? C24 C23 H23A 108.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C31 C26 C27 120.7(6) . . ? C31 C26 N2 117.7(5) . . ? C27 C26 N2 121.4(5) . . ? C28 C27 C26 117.8(6) . . ? C28 C27 C32 118.9(5) . . ? C26 C27 C32 123.2(5) . . ? C29 C28 C27 121.2(6) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? C28 C29 C30 121.0(6) . . ? C28 C29 H29A 119.5 . . ? C30 C29 H29A 119.5 . . ? C31 C30 C29 120.5(6) . . ? C31 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? C30 C31 C26 118.7(6) . . ? C30 C31 C35 120.4(6) . . ? C26 C31 C35 120.9(6) . . ? C27 C32 C33 111.8(5) . . ? C27 C32 C34 111.0(4) . . ? C33 C32 C34 109.2(5) . . ? C27 C32 H32A 108.2 . . ? C33 C32 H32A 108.2 . . ? C34 C32 H32A 108.2 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 C37 114.1(5) . . ? C31 C35 C36 110.6(5) . . ? C37 C35 C36 110.0(5) . . ? C31 C35 H35A 107.3 . . ? C37 C35 H35A 107.3 . . ? C36 C35 H35A 107.3 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N3 C39 C40 123.4(5) . . ? N3 C39 C38 121.2(5) . . ? C40 C39 C38 115.3(5) . . ? C41 C40 C39 130.3(5) . . ? C41 C40 H40A 114.8 . . ? C39 C40 H40A 114.8 . . ? N4 C41 C40 124.9(5) . . ? N4 C41 C42 120.0(5) . . ? C40 C41 C42 115.1(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 120.8(5) . . ? C44 C43 N4 118.2(5) . . ? C48 C43 N4 120.9(4) . . ? C45 C44 C43 118.1(5) . . ? C45 C44 C52 119.7(5) . . ? C43 C44 C52 122.2(5) . . ? C46 C45 C44 121.4(5) . . ? C46 C45 H45A 119.3 . . ? C44 C45 H45A 119.3 . . ? C47 C46 C45 119.7(6) . . ? C47 C46 H46A 120.1 . . ? C45 C46 H46A 120.1 . . ? C46 C47 C48 121.6(6) . . ? C46 C47 H47A 119.2 . . ? C48 C47 H47A 119.2 . . ? C47 C48 C43 118.3(5) . . ? C47 C48 C49 118.2(5) . . ? C43 C48 C49 123.4(5) . . ? C48 C49 C51 110.5(5) . . ? C48 C49 C50 112.4(5) . . ? C51 C49 C50 109.0(5) . . ? C48 C49 H49A 108.3 . . ? C51 C49 H49A 108.3 . . ? C50 C49 H49A 108.3 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C44 C52 C54 111.3(5) . . ? C44 C52 C53 114.4(5) . . ? C54 C52 C53 108.8(5) . . ? C44 C52 H52A 107.4 . . ? C54 C52 H52A 107.4 . . ? C53 C52 H52A 107.4 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 C60 121.4(5) . . ? C56 C55 N3 120.6(5) . . ? C60 C55 N3 117.9(5) . . ? C57 C56 C55 118.0(5) . . ? C57 C56 C64 118.3(5) . . ? C55 C56 C64 123.7(5) . . ? C58 C57 C56 120.3(6) . . ? C58 C57 H57A 119.8 . . ? C56 C57 H57A 119.8 . . ? C59 C58 C57 120.3(6) . . ? C59 C58 H58A 119.8 . . ? C57 C58 H58A 119.8 . . ? C60 C59 C58 121.8(6) . . ? C60 C59 H59A 119.1 . . ? C58 C59 H59A 119.1 . . ? C59 C60 C55 118.1(6) . . ? C59 C60 C61 121.0(6) . . ? C55 C60 C61 121.0(5) . . ? C60 C61 C62 111.6(5) . . ? C60 C61 C63 114.3(5) . . ? C62 C61 C63 110.9(5) . . ? C60 C61 H61A 106.5 . . ? C62 C61 H61A 106.5 . . ? C63 C61 H61A 106.5 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C66 C64 C56 111.8(4) . . ? C66 C64 C65 109.3(5) . . ? C56 C64 C65 112.2(5) . . ? C66 C64 H64A 107.8 . . ? C56 C64 H64A 107.8 . . ? C65 C64 H64A 107.8 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C68 C67 H67A 109.5 . . ? C68 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C68 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N5 C68 C69 125.1(5) . . ? N5 C68 C67 119.4(5) . . ? C69 C68 C67 115.4(5) . . ? C68 C69 C70 130.1(5) . . ? C68 C69 H69A 115.0 . . ? C70 C69 H69A 115.0 . . ? N6 C70 C69 123.5(5) . . ? N6 C70 C71 122.2(5) . . ? C69 C70 C71 114.3(5) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C77 C72 C73 121.5(5) . . ? C77 C72 N6 117.8(5) . . ? C73 C72 N6 120.4(4) . . ? C74 C73 C72 117.7(5) . . ? C74 C73 C81 118.6(5) . . ? C72 C73 C81 123.6(4) . . ? C75 C74 C73 120.8(5) . . ? C75 C74 H74A 119.6 . . ? C73 C74 H74A 119.6 . . ? C74 C75 C76 121.0(5) . . ? C74 C75 H75A 119.5 . . ? C76 C75 H75A 119.5 . . ? C75 C76 C77 120.5(5) . . ? C75 C76 H76A 119.8 . . ? C77 C76 H76A 119.8 . . ? C76 C77 C72 118.5(5) . . ? C76 C77 C78 120.3(5) . . ? C72 C77 C78 121.2(4) . . ? C80 C78 C79 110.9(5) . . ? C80 C78 C77 110.8(5) . . ? C79 C78 C77 113.5(4) . . ? C80 C78 H78A 107.1 . . ? C79 C78 H78A 107.1 . . ? C77 C78 H78A 107.1 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C78 C80 H80A 109.5 . . ? C78 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C78 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C73 C81 C82 112.8(4) . . ? C73 C81 C83 110.9(4) . . ? C82 C81 C83 109.7(4) . . ? C73 C81 H81A 107.8 . . ? C82 C81 H81A 107.8 . . ? C83 C81 H81A 107.8 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C89 C84 C85 120.7(5) . . ? C89 C84 N5 122.3(5) . . ? C85 C84 N5 117.0(5) . . ? C86 C85 C84 118.5(5) . . ? C86 C85 C93 119.6(5) . . ? C84 C85 C93 121.8(5) . . ? C87 C86 C85 121.0(5) . . ? C87 C86 H86A 119.5 . . ? C85 C86 H86A 119.5 . . ? C88 C87 C86 119.9(5) . . ? C88 C87 H87A 120.1 . . ? C86 C87 H87A 120.1 . . ? C87 C88 C89 121.6(5) . . ? C87 C88 H88A 119.2 . . ? C89 C88 H88A 119.2 . . ? C88 C89 C84 118.3(5) . . ? C88 C89 C90 118.2(5) . . ? C84 C89 C90 123.5(5) . . ? C92 C90 C89 112.2(5) . . ? C92 C90 C91 108.8(5) . . ? C89 C90 C91 111.6(5) . . ? C92 C90 H90A 108.1 . . ? C89 C90 H90A 108.1 . . ? C91 C90 H90A 108.1 . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C90 C92 H92A 109.5 . . ? C90 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C90 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C95 C93 C94 109.9(5) . . ? C95 C93 C85 113.3(5) . . ? C94 C93 C85 110.8(5) . . ? C95 C93 H93A 107.5 . . ? C94 C93 H93A 107.5 . . ? C85 C93 H93A 107.5 . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C93 C95 H95A 109.5 . . ? C93 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C93 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C97 C96 H96A 109.5 . . ? C97 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C97 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? N8 C97 C98 123.6(5) . . ? N8 C97 C96 120.7(5) . . ? C98 C97 C96 115.7(5) . . ? C97 C98 C99 130.6(5) . . ? C97 C98 H98A 114.7 . . ? C99 C98 H98A 114.7 . . ? N7 C99 C98 122.8(5) . . ? N7 C99 C100 121.8(5) . . ? C98 C99 C100 115.3(5) . . ? C99 C100 H10A 109.5 . . ? C99 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C99 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C102 C101 C106 121.6(5) . . ? C102 C101 N7 120.8(4) . . ? C106 C101 N7 117.3(4) . . ? C103 C102 C101 117.5(5) . . ? C103 C102 C110 119.0(5) . . ? C101 C102 C110 123.5(5) . . ? C104 C103 C102 122.0(5) . . ? C104 C103 H10D 119.0 . . ? C102 C103 H10D 119.0 . . ? C105 C104 C103 119.9(5) . . ? C105 C104 H10E 120.1 . . ? C103 C104 H10E 120.1 . . ? C104 C105 C106 121.5(5) . . ? C104 C105 H10F 119.2 . . ? C106 C105 H10F 119.2 . . ? C105 C106 C101 117.4(5) . . ? C105 C106 C107 121.3(5) . . ? C101 C106 C107 121.3(5) . . ? C106 C107 C108 111.0(5) . . ? C106 C107 C109 113.9(5) . . ? C108 C107 C109 110.2(5) . . ? C106 C107 H10G 107.1 . . ? C108 C107 H10G 107.1 . . ? C109 C107 H10G 107.1 . . ? C107 C108 H10H 109.5 . . ? C107 C108 H10I 109.5 . . ? H10H C108 H10I 109.5 . . ? C107 C108 H10J 109.5 . . ? H10H C108 H10J 109.5 . . ? H10I C108 H10J 109.5 . . ? C107 C109 H10K 109.5 . . ? C107 C109 H10L 109.5 . . ? H10K C109 H10L 109.5 . . ? C107 C109 H10M 109.5 . . ? H10K C109 H10M 109.5 . . ? H10L C109 H10M 109.5 . . ? C102 C110 C111 111.4(4) . . ? C102 C110 C112 112.4(5) . . ? C111 C110 C112 110.6(4) . . ? C102 C110 H11B 107.4 . . ? C111 C110 H11B 107.4 . . ? C112 C110 H11B 107.4 . . ? C110 C111 H11C 109.5 . . ? C110 C111 H11D 109.5 . . ? H11C C111 H11D 109.5 . . ? C110 C111 H11E 109.5 . . ? H11C C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? C110 C112 H11F 109.5 . . ? C110 C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? C110 C112 H11H 109.5 . . ? H11F C112 H11H 109.5 . . ? H11G C112 H11H 109.5 . . ? C114 C113 C118 121.2(5) . . ? C114 C113 N8 122.0(5) . . ? C118 C113 N8 116.9(5) . . ? C113 C114 C115 118.3(5) . . ? C113 C114 C122 123.7(5) . . ? C115 C114 C122 117.9(5) . . ? C116 C115 C114 120.8(5) . . ? C116 C115 H11I 119.6 . . ? C114 C115 H11I 119.6 . . ? C117 C116 C115 120.1(5) . . ? C117 C116 H11J 120.0 . . ? C115 C116 H11J 120.0 . . ? C116 C117 C118 121.6(5) . . ? C116 C117 H11K 119.2 . . ? C118 C117 H11K 119.2 . . ? C117 C118 C113 118.0(5) . . ? C117 C118 C119 120.8(5) . . ? C113 C118 C119 121.2(5) . . ? C118 C119 C120 112.0(4) . . ? C118 C119 C121 113.1(5) . . ? C120 C119 C121 108.9(5) . . ? C118 C119 H11L 107.5 . . ? C120 C119 H11L 107.5 . . ? C121 C119 H11L 107.5 . . ? C119 C120 H12A 109.5 . . ? C119 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? C119 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C119 C121 H12D 109.5 . . ? C119 C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? C119 C121 H12F 109.5 . . ? H12D C121 H12F 109.5 . . ? H12E C121 H12F 109.5 . . ? C114 C122 C123 111.1(5) . . ? C114 C122 C124 111.9(5) . . ? C123 C122 C124 109.7(5) . . ? C114 C122 H12G 108.0 . . ? C123 C122 H12G 108.0 . . ? C124 C122 H12G 108.0 . . ? C122 C123 H12H 109.5 . . ? C122 C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? C122 C123 H12J 109.5 . . ? H12H C123 H12J 109.5 . . ? H12I C123 H12J 109.5 . . ? C122 C124 H12K 109.5 . . ? C122 C124 H12L 109.5 . . ? H12K C124 H12L 109.5 . . ? C122 C124 H12M 109.5 . . ? H12K C124 H12M 109.5 . . ? H12L C124 H12M 109.5 . . ? C126 C125 C131 120.1(10) . . ? C126 C125 C130 118.6(9) . . ? C131 C125 C130 121.3(9) . . ? C127 C126 C125 118.0(8) . . ? C127 C126 H12N 121.0 . . ? C125 C126 H12N 121.0 . . ? C126 C127 C128 125.0(9) . . ? C126 C127 H12O 117.5 . . ? C128 C127 H12O 117.5 . . ? C129 C128 C127 112.5(11) . . ? C129 C128 H12P 123.7 . . ? C127 C128 H12P 123.7 . . ? C128 C129 C130 130.2(12) . . ? C128 C129 H12Q 114.9 . . ? C130 C129 H12Q 114.9 . . ? C129 C130 C125 115.4(8) . . ? C129 C130 H13D 122.3 . . ? C125 C130 H13D 122.3 . . ? C125 C131 H13E 109.5 . . ? C125 C131 H13F 109.5 . . ? H13E C131 H13F 109.5 . . ? C125 C131 H13G 109.5 . . ? H13E C131 H13G 109.5 . . ? H13F C131 H13G 109.5 . . ? C138 C132 C137 122.4(15) . . ? C138 C132 C133 119.5(11) . . ? C137 C132 C133 117.9(11) . . ? C134 C133 C132 111.6(8) . . ? C134 C133 H13H 124.2 . . ? C132 C133 H13H 124.2 . . ? C135 C134 C133 136.4(15) . . ? C135 C134 H13J 111.8 . . ? C133 C134 H13J 111.8 . . ? C134 C135 C136 107.7(13) . . ? C134 C135 H13K 126.1 . . ? C136 C135 H13K 126.1 . . ? C137 C136 C135 127.6(10) . . ? C137 C136 H13L 116.2 . . ? C135 C136 H13L 116.2 . . ? C136 C137 C132 118.7(11) . . ? C136 C137 H13M 120.6 . . ? C132 C137 H13M 120.6 . . ? C132 C138 H13N 109.5 . . ? C132 C138 H13O 109.5 . . ? H13N C138 H13O 109.5 . . ? C132 C138 H13P 109.5 . . ? H13N C138 H13P 109.5 . . ? H13O C138 H13P 109.5 . . ? C140 C139 C144 122.8(11) . . ? C140 C139 C145 107.4(13) . . ? C144 C139 C145 129.8(13) . . ? C141 C140 C139 121.1(14) . . ? C141 C140 H14A 119.4 . . ? C139 C140 H14A 119.4 . . ? C140 C141 C142 124.6(13) . . ? C140 C141 H14B 117.7 . . ? C142 C141 H14B 117.7 . . ? C141 C142 C143 120.0(10) . . ? C141 C142 H14C 120.0 . . ? C143 C142 H14C 120.0 . . ? C142 C143 C144 114.7(9) . . ? C142 C143 H14D 122.6 . . ? C144 C143 H14D 122.6 . . ? C139 C144 C143 116.7(9) . . ? C139 C144 H14E 121.7 . . ? C143 C144 H14E 121.7 . . ? C139 C145 H14G 109.5 . . ? C139 C145 H14H 109.5 . . ? H14G C145 H14H 109.5 . . ? C139 C145 H14I 109.5 . . ? H14G C145 H14I 109.5 . . ? H14H C145 H14I 109.5 . . ? C147 C146 C151 117.5(7) . . ? C147 C146 C152 121.6(8) . . ? C151 C146 C152 120.8(7) . . ? C148 C147 C146 121.9(8) . . ? C148 C147 H14J 119.0 . . ? C146 C147 H14J 119.0 . . ? C147 C148 C149 119.5(8) . . ? C147 C148 H14K 120.2 . . ? C149 C148 H14K 120.2 . . ? C148 C149 C150 120.0(8) . . ? C148 C149 H14L 120.0 . . ? C150 C149 H14L 120.0 . . ? C151 C150 C149 118.2(8) . . ? C151 C150 H15A 120.9 . . ? C149 C150 H15A 120.9 . . ? C150 C151 C146 122.9(7) . . ? C150 C151 H15B 118.6 . . ? C146 C151 H15B 118.6 . . ? C146 C152 H15C 109.5 . . ? C146 C152 H15D 109.5 . . ? H15C C152 H15D 109.5 . . ? C146 C152 H15E 109.5 . . ? H15C C152 H15E 109.5 . . ? H15D C152 H15E 109.5 . . ? C156 C153 C154 113.3(14) 3_666 . ? C156 C153 C157 55.5(9) 3_666 3_666 ? C154 C153 C157 57.9(8) . 3_666 ? C157 C154 C153 120.9(15) . . ? C157 C154 C157 45.6(14) . 3_666 ? C153 C154 C157 75.3(10) . 3_666 ? C157 C154 C155 54.5(10) . . ? C153 C154 C155 175.3(13) . . ? C157 C154 C155 100.1(12) 3_666 . ? C156 C155 C157 77.3(13) . . ? C156 C155 C154 117.5(14) . . ? C157 C155 C154 40.2(9) . . ? C155 C156 C153 133.7(15) . 3_666 ? C155 C156 C157 56.3(11) . . ? C153 C156 C157 77.5(11) 3_666 . ? C154 C157 C157 94(2) . 3_666 ? C154 C157 C155 85.3(14) . . ? C157 C157 C155 179(3) 3_666 . ? C154 C157 C156 131.7(15) . . ? C157 C157 C156 134(2) 3_666 . ? C155 C157 C156 46.4(9) . . ? C154 C157 C154 134.4(14) . 3_666 ? C157 C157 C154 40.5(13) 3_666 3_666 ? C155 C157 C154 140.3(17) . 3_666 ? C156 C157 C154 93.9(13) . 3_666 ? C154 C157 C153 178.4(16) . 3_666 ? C157 C157 C153 87.3(19) 3_666 3_666 ? C155 C157 C153 93.5(14) . 3_666 ? C156 C157 C153 47.1(8) . 3_666 ? C154 C157 C153 46.8(8) 3_666 3_666 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Sm1 Sm2 N4 -63.9(2) . . . . ? N2 Sm1 Sm2 N4 50.07(19) . . . . ? C1 Sm1 Sm2 N4 164.3(2) . . . . ? Cl2 Sm1 Sm2 N4 86.59(15) . . . . ? Cl1 Sm1 Sm2 N4 -35.57(15) . . . . ? Cl3 Sm1 Sm2 N4 -155.42(15) . . . . ? N1 Sm1 Sm2 N3 57.3(2) . . . . ? N2 Sm1 Sm2 N3 171.28(18) . . . . ? C1 Sm1 Sm2 N3 -74.52(19) . . . . ? Cl2 Sm1 Sm2 N3 -152.20(14) . . . . ? Cl1 Sm1 Sm2 N3 85.64(14) . . . . ? Cl3 Sm1 Sm2 N3 -34.21(14) . . . . ? N1 Sm1 Sm2 C5 169.6(2) . . . . ? N2 Sm1 Sm2 C5 -76.50(18) . . . . ? C1 Sm1 Sm2 C5 37.70(19) . . . . ? Cl2 Sm1 Sm2 C5 -39.98(14) . . . . ? Cl1 Sm1 Sm2 C5 -162.14(14) . . . . ? Cl3 Sm1 Sm2 C5 78.01(14) . . . . ? N1 Sm1 Sm2 Cl1 -28.31(16) . . . . ? N2 Sm1 Sm2 Cl1 85.64(14) . . . . ? C1 Sm1 Sm2 Cl1 -160.16(15) . . . . ? Cl2 Sm1 Sm2 Cl1 122.16(7) . . . . ? Cl3 Sm1 Sm2 Cl1 -119.85(6) . . . . ? N1 Sm1 Sm2 Cl2 -150.47(16) . . . . ? N2 Sm1 Sm2 Cl2 -36.52(14) . . . . ? C1 Sm1 Sm2 Cl2 77.67(15) . . . . ? Cl1 Sm1 Sm2 Cl2 -122.16(7) . . . . ? Cl3 Sm1 Sm2 Cl2 117.99(6) . . . . ? N1 Sm1 Sm2 Cl3 91.54(16) . . . . ? N2 Sm1 Sm2 Cl3 -154.51(14) . . . . ? C1 Sm1 Sm2 Cl3 -40.31(15) . . . . ? Cl2 Sm1 Sm2 Cl3 -117.99(6) . . . . ? Cl1 Sm1 Sm2 Cl3 119.85(6) . . . . ? N5 Sm3 Sm4 N8 -67.8(2) . . . . ? N6 Sm3 Sm4 N8 52.50(19) . . . . ? C6 Sm3 Sm4 N8 165.7(2) . . . . ? Cl6 Sm3 Sm4 N8 86.18(15) . . . . ? Cl4 Sm3 Sm4 N8 -35.45(15) . . . . ? Cl5 Sm3 Sm4 N8 -156.49(15) . . . . ? N5 Sm3 Sm4 N7 55.32(19) . . . . ? N6 Sm3 Sm4 N7 175.61(18) . . . . ? C6 Sm3 Sm4 N7 -71.15(19) . . . . ? Cl6 Sm3 Sm4 N7 -150.71(13) . . . . ? Cl4 Sm3 Sm4 N7 87.65(13) . . . . ? Cl5 Sm3 Sm4 N7 -33.39(13) . . . . ? N5 Sm3 Sm4 C2 168.2(2) . . . . ? N6 Sm3 Sm4 C2 -71.48(19) . . . . ? C6 Sm3 Sm4 C2 41.76(19) . . . . ? Cl6 Sm3 Sm4 C2 -37.80(14) . . . . ? Cl4 Sm3 Sm4 C2 -159.43(14) . . . . ? Cl5 Sm3 Sm4 C2 79.53(14) . . . . ? N5 Sm3 Sm4 Cl4 -32.33(15) . . . . ? N6 Sm3 Sm4 Cl4 87.95(13) . . . . ? C6 Sm3 Sm4 Cl4 -158.80(14) . . . . ? Cl6 Sm3 Sm4 Cl4 121.63(6) . . . . ? Cl5 Sm3 Sm4 Cl4 -121.04(6) . . . . ? N5 Sm3 Sm4 Cl5 88.71(15) . . . . ? N6 Sm3 Sm4 Cl5 -151.01(13) . . . . ? C6 Sm3 Sm4 Cl5 -37.76(15) . . . . ? Cl6 Sm3 Sm4 Cl5 -117.33(6) . . . . ? Cl4 Sm3 Sm4 Cl5 121.04(6) . . . . ? N5 Sm3 Sm4 Cl6 -153.97(15) . . . . ? N6 Sm3 Sm4 Cl6 -33.68(13) . . . . ? C6 Sm3 Sm4 Cl6 79.56(14) . . . . ? Cl4 Sm3 Sm4 Cl6 -121.63(6) . . . . ? Cl5 Sm3 Sm4 Cl6 117.33(6) . . . . ? N4 Sm2 Cl1 Sm1 156.13(10) . . . . ? N3 Sm2 Cl1 Sm1 -124.43(12) . . . . ? C5 Sm2 Cl1 Sm1 49.0(3) . . . . ? Cl2 Sm2 Cl1 Sm1 38.13(4) . . . . ? Cl3 Sm2 Cl1 Sm1 -39.66(4) . . . . ? N1 Sm1 Cl1 Sm2 159.92(11) . . . . ? N2 Sm1 Cl1 Sm2 -121.71(11) . . . . ? C1 Sm1 Cl1 Sm2 58.7(4) . . . . ? Cl2 Sm1 Cl1 Sm2 -38.30(4) . . . . ? Cl3 Sm1 Cl1 Sm2 39.79(4) . . . . ? N1 Sm1 Cl2 Sm2 98.1(3) . . . . ? N2 Sm1 Cl2 Sm2 152.23(11) . . . . ? C1 Sm1 Cl2 Sm2 -122.08(12) . . . . ? Cl1 Sm1 Cl2 Sm2 37.95(4) . . . . ? Cl3 Sm1 Cl2 Sm2 -40.76(4) . . . . ? N4 Sm2 Cl2 Sm1 -128.13(11) . . . . ? N3 Sm2 Cl2 Sm1 90.8(3) . . . . ? C5 Sm2 Cl2 Sm1 145.58(12) . . . . ? Cl1 Sm2 Cl2 Sm1 -38.28(4) . . . . ? Cl3 Sm2 Cl2 Sm1 40.74(4) . . . . ? N1 Sm1 Cl3 Sm2 -123.61(13) . . . . ? N2 Sm1 Cl3 Sm2 81.9(3) . . . . ? C1 Sm1 Cl3 Sm2 147.01(12) . . . . ? Cl2 Sm1 Cl3 Sm2 40.56(4) . . . . ? Cl1 Sm1 Cl3 Sm2 -39.22(4) . . . . ? N4 Sm2 Cl3 Sm1 104.9(3) . . . . ? N3 Sm2 Cl3 Sm1 155.08(10) . . . . ? C5 Sm2 Cl3 Sm1 -119.18(12) . . . . ? Cl1 Sm2 Cl3 Sm1 39.54(4) . . . . ? Cl2 Sm2 Cl3 Sm1 -40.47(4) . . . . ? N5 Sm3 Cl4 Sm4 158.20(10) . . . . ? N6 Sm3 Cl4 Sm4 -122.03(10) . . . . ? C6 Sm3 Cl4 Sm4 57.2(3) . . . . ? Cl6 Sm3 Cl4 Sm4 -38.68(4) . . . . ? Cl5 Sm3 Cl4 Sm4 38.95(4) . . . . ? N8 Sm4 Cl4 Sm3 157.24(10) . . . . ? N7 Sm4 Cl4 Sm3 -122.30(11) . . . . ? C2 Sm4 Cl4 Sm3 54.2(3) . . . . ? Cl5 Sm4 Cl4 Sm3 -39.03(4) . . . . ? Cl6 Sm4 Cl4 Sm3 38.41(4) . . . . ? N8 Sm4 Cl5 Sm3 113.6(4) . . . . ? N7 Sm4 Cl5 Sm3 155.18(10) . . . . ? C2 Sm4 Cl5 Sm3 -118.49(13) . . . . ? Cl4 Sm4 Cl5 Sm3 38.76(4) . . . . ? Cl6 Sm4 Cl5 Sm3 -40.78(4) . . . . ? N5 Sm3 Cl5 Sm4 -127.32(12) . . . . ? N6 Sm3 Cl5 Sm4 88.7(3) . . . . ? C6 Sm3 Cl5 Sm4 147.83(12) . . . . ? Cl6 Sm3 Cl5 Sm4 41.11(4) . . . . ? Cl4 Sm3 Cl5 Sm4 -38.90(4) . . . . ? N5 Sm3 Cl6 Sm4 105.4(3) . . . . ? N6 Sm3 Cl6 Sm4 154.88(10) . . . . ? C6 Sm3 Cl6 Sm4 -119.13(13) . . . . ? Cl4 Sm3 Cl6 Sm4 38.54(4) . . . . ? Cl5 Sm3 Cl6 Sm4 -41.02(4) . . . . ? N8 Sm4 Cl6 Sm3 -130.60(11) . . . . ? N7 Sm4 Cl6 Sm3 88.6(3) . . . . ? C2 Sm4 Cl6 Sm3 147.44(12) . . . . ? Cl4 Sm4 Cl6 Sm3 -38.48(4) . . . . ? Cl5 Sm4 Cl6 Sm3 41.16(4) . . . . ? N2 Sm1 N1 C12 34.0(4) . . . . ? C1 Sm1 N1 C12 -51.6(5) . . . . ? Cl2 Sm1 N1 C12 89.8(5) . . . . ? Cl1 Sm1 N1 C12 147.5(4) . . . . ? Cl3 Sm1 N1 C12 -137.4(4) . . . . ? Sm2 Sm1 N1 C12 167.1(4) . . . . ? N2 Sm1 N1 C14 -155.1(4) . . . . ? C1 Sm1 N1 C14 119.3(4) . . . . ? Cl2 Sm1 N1 C14 -99.3(5) . . . . ? Cl1 Sm1 N1 C14 -41.6(4) . . . . ? Cl3 Sm1 N1 C14 33.5(4) . . . . ? Sm2 Sm1 N1 C14 -22.0(5) . . . . ? N1 Sm1 N2 C10 -31.1(4) . . . . ? C1 Sm1 N2 C10 61.5(4) . . . . ? Cl2 Sm1 N2 C10 166.3(4) . . . . ? Cl1 Sm1 N2 C10 -118.4(4) . . . . ? Cl3 Sm1 N2 C10 126.5(4) . . . . ? Sm2 Sm1 N2 C10 -168.6(4) . . . . ? N1 Sm1 N2 C26 154.9(4) . . . . ? C1 Sm1 N2 C26 -112.5(4) . . . . ? Cl2 Sm1 N2 C26 -7.7(3) . . . . ? Cl1 Sm1 N2 C26 67.6(4) . . . . ? Cl3 Sm1 N2 C26 -47.5(5) . . . . ? Sm2 Sm1 N2 C26 17.4(4) . . . . ? N4 Sm2 N3 C39 -28.1(4) . . . . ? C5 Sm2 N3 C39 63.2(4) . . . . ? Cl1 Sm2 N3 C39 -119.1(4) . . . . ? Cl2 Sm2 N3 C39 117.6(4) . . . . ? Cl3 Sm2 N3 C39 165.5(4) . . . . ? Sm1 Sm2 N3 C39 -170.8(4) . . . . ? N4 Sm2 N3 C55 157.1(4) . . . . ? C5 Sm2 N3 C55 -111.6(4) . . . . ? Cl1 Sm2 N3 C55 66.1(4) . . . . ? Cl2 Sm2 N3 C55 -57.2(5) . . . . ? Cl3 Sm2 N3 C55 -9.4(3) . . . . ? Sm1 Sm2 N3 C55 14.3(4) . . . . ? N3 Sm2 N4 C41 30.4(4) . . . . ? C5 Sm2 N4 C41 -55.0(4) . . . . ? Cl1 Sm2 N4 C41 144.8(4) . . . . ? Cl2 Sm2 N4 C41 -136.6(4) . . . . ? Cl3 Sm2 N4 C41 82.2(5) . . . . ? Sm1 Sm2 N4 C41 169.4(3) . . . . ? N3 Sm2 N4 C43 -160.8(4) . . . . ? C5 Sm2 N4 C43 113.8(4) . . . . ? Cl1 Sm2 N4 C43 -46.4(3) . . . . ? Cl2 Sm2 N4 C43 32.2(4) . . . . ? Cl3 Sm2 N4 C43 -109.0(4) . . . . ? Sm1 Sm2 N4 C43 -21.7(4) . . . . ? N6 Sm3 N5 C68 33.6(4) . . . . ? C6 Sm3 N5 C68 -52.7(4) . . . . ? Cl6 Sm3 N5 C68 84.5(5) . . . . ? Cl4 Sm3 N5 C68 148.6(4) . . . . ? Cl5 Sm3 N5 C68 -133.6(4) . . . . ? Sm4 Sm3 N5 C68 171.2(3) . . . . ? N6 Sm3 N5 C84 -155.3(4) . . . . ? C6 Sm3 N5 C84 118.4(4) . . . . ? Cl6 Sm3 N5 C84 -104.4(4) . . . . ? Cl4 Sm3 N5 C84 -40.3(3) . . . . ? Cl5 Sm3 N5 C84 37.5(4) . . . . ? Sm4 Sm3 N5 C84 -17.7(4) . . . . ? N5 Sm3 N6 C70 -26.8(4) . . . . ? C6 Sm3 N6 C70 63.3(4) . . . . ? Cl6 Sm3 N6 C70 167.4(4) . . . . ? Cl4 Sm3 N6 C70 -117.0(4) . . . . ? Cl5 Sm3 N6 C70 121.8(4) . . . . ? Sm4 Sm3 N6 C70 -169.2(3) . . . . ? N5 Sm3 N6 C72 158.8(3) . . . . ? C6 Sm3 N6 C72 -111.2(3) . . . . ? Cl6 Sm3 N6 C72 -7.1(3) . . . . ? Cl4 Sm3 N6 C72 68.5(3) . . . . ? Cl5 Sm3 N6 C72 -52.7(5) . . . . ? Sm4 Sm3 N6 C72 16.3(4) . . . . ? N8 Sm4 N7 C99 -26.6(4) . . . . ? C2 Sm4 N7 C99 61.1(4) . . . . ? Cl4 Sm4 N7 C99 -120.2(4) . . . . ? Cl5 Sm4 N7 C99 164.6(4) . . . . ? Cl6 Sm4 N7 C99 119.2(4) . . . . ? Sm3 Sm4 N7 C99 -172.2(4) . . . . ? N8 Sm4 N7 C101 159.9(3) . . . . ? C2 Sm4 N7 C101 -112.3(3) . . . . ? Cl4 Sm4 N7 C101 66.4(3) . . . . ? Cl5 Sm4 N7 C101 -8.8(3) . . . . ? Cl6 Sm4 N7 C101 -54.2(5) . . . . ? Sm3 Sm4 N7 C101 14.4(4) . . . . ? N7 Sm4 N8 C97 31.6(4) . . . . ? C2 Sm4 N8 C97 -55.4(4) . . . . ? Cl4 Sm4 N8 C97 146.1(4) . . . . ? Cl5 Sm4 N8 C97 74.4(6) . . . . ? Cl6 Sm4 N8 C97 -134.4(4) . . . . ? Sm3 Sm4 N8 C97 170.8(3) . . . . ? N7 Sm4 N8 C113 -155.2(3) . . . . ? C2 Sm4 N8 C113 117.8(3) . . . . ? Cl4 Sm4 N8 C113 -40.6(3) . . . . ? Cl5 Sm4 N8 C113 -112.4(4) . . . . ? Cl6 Sm4 N8 C113 38.8(4) . . . . ? Sm3 Sm4 N8 C113 -16.0(4) . . . . ? C4 Al2 C1 Sm1 -16(6) . . . . ? C3 Al2 C1 Sm1 -143(6) . . . . ? C2 Al2 C1 Sm1 101(6) . . . . ? N1 Sm1 C1 Al2 93(6) . . . . ? N2 Sm1 C1 Al2 14(6) . . . . ? Cl2 Sm1 C1 Al2 -74(6) . . . . ? Cl1 Sm1 C1 Al2 -166(6) . . . . ? Cl3 Sm1 C1 Al2 -148(6) . . . . ? Sm2 Sm1 C1 Al2 -120(6) . . . . ? C4 Al2 C2 Sm4 -94(4) . . . . ? C3 Al2 C2 Sm4 30(5) . . . . ? C1 Al2 C2 Sm4 149(4) . . . . ? N8 Sm4 C2 Al2 40(4) . . . . ? N7 Sm4 C2 Al2 -38(4) . . . . ? Cl4 Sm4 C2 Al2 145(4) . . . . ? Cl5 Sm4 C2 Al2 -127(4) . . . . ? Cl6 Sm4 C2 Al2 160(4) . . . . ? Sm3 Sm4 C2 Al2 -173(4) . . . . ? C8 Al1 C5 Sm2 -93(8) . . . . ? C7 Al1 C5 Sm2 33(8) . . . . ? C6 Al1 C5 Sm2 149(8) . . . . ? N4 Sm2 C5 Al1 47(8) . . . . ? N3 Sm2 C5 Al1 -31(8) . . . . ? Cl1 Sm2 C5 Al1 155(8) . . . . ? Cl2 Sm2 C5 Al1 166(8) . . . . ? Cl3 Sm2 C5 Al1 -121(8) . . . . ? Sm1 Sm2 C5 Al1 -167(8) . . . . ? C8 Al1 C6 Sm3 65(10) . . . . ? C7 Al1 C6 Sm3 -60(10) . . . . ? C5 Al1 C6 Sm3 -178(100) . . . . ? N5 Sm3 C6 Al1 10(10) . . . . ? N6 Sm3 C6 Al1 -69(10) . . . . ? Cl6 Sm3 C6 Al1 -158(10) . . . . ? Cl4 Sm3 C6 Al1 112(10) . . . . ? Cl5 Sm3 C6 Al1 130(10) . . . . ? Sm4 Sm3 C6 Al1 156(10) . . . . ? C26 N2 C10 C11 -171.4(5) . . . . ? Sm1 N2 C10 C11 14.8(8) . . . . ? C26 N2 C10 C9 6.6(8) . . . . ? Sm1 N2 C10 C9 -167.2(4) . . . . ? N2 C10 C11 C12 17.9(10) . . . . ? C9 C10 C11 C12 -160.2(6) . . . . ? C14 N1 C12 C11 167.3(6) . . . . ? Sm1 N1 C12 C11 -21.9(8) . . . . ? C14 N1 C12 C13 -11.3(8) . . . . ? Sm1 N1 C12 C13 159.6(4) . . . . ? C10 C11 C12 N1 -14.0(10) . . . . ? C10 C11 C12 C13 164.6(6) . . . . ? C12 N1 C14 C19 102.9(6) . . . . ? Sm1 N1 C14 C19 -68.6(6) . . . . ? C12 N1 C14 C15 -77.9(7) . . . . ? Sm1 N1 C14 C15 110.6(5) . . . . ? C19 C14 C15 C16 -1.1(8) . . . . ? N1 C14 C15 C16 179.7(5) . . . . ? C19 C14 C15 C23 178.0(5) . . . . ? N1 C14 C15 C23 -1.2(8) . . . . ? C14 C15 C16 C17 -0.4(9) . . . . ? C23 C15 C16 C17 -179.5(5) . . . . ? C15 C16 C17 C18 1.0(9) . . . . ? C16 C17 C18 C19 -0.2(9) . . . . ? C17 C18 C19 C14 -1.2(9) . . . . ? C17 C18 C19 C20 -179.9(5) . . . . ? C15 C14 C19 C18 1.9(8) . . . . ? N1 C14 C19 C18 -178.9(5) . . . . ? C15 C14 C19 C20 -179.5(5) . . . . ? N1 C14 C19 C20 -0.3(8) . . . . ? C18 C19 C20 C22 -28.7(7) . . . . ? C14 C19 C20 C22 152.7(5) . . . . ? C18 C19 C20 C21 97.5(6) . . . . ? C14 C19 C20 C21 -81.1(7) . . . . ? C16 C15 C23 C25 58.0(7) . . . . ? C14 C15 C23 C25 -121.1(6) . . . . ? C16 C15 C23 C24 -62.6(8) . . . . ? C14 C15 C23 C24 118.3(6) . . . . ? C10 N2 C26 C31 107.9(6) . . . . ? Sm1 N2 C26 C31 -77.6(5) . . . . ? C10 N2 C26 C27 -77.6(6) . . . . ? Sm1 N2 C26 C27 96.9(5) . . . . ? C31 C26 C27 C28 -0.7(7) . . . . ? N2 C26 C27 C28 -175.0(5) . . . . ? C31 C26 C27 C32 177.5(5) . . . . ? N2 C26 C27 C32 3.2(7) . . . . ? C26 C27 C28 C29 0.8(8) . . . . ? C32 C27 C28 C29 -177.5(5) . . . . ? C27 C28 C29 C30 -0.8(10) . . . . ? C28 C29 C30 C31 0.8(10) . . . . ? C29 C30 C31 C26 -0.8(9) . . . . ? C29 C30 C31 C35 -178.6(5) . . . . ? C27 C26 C31 C30 0.7(8) . . . . ? N2 C26 C31 C30 175.2(5) . . . . ? C27 C26 C31 C35 178.6(5) . . . . ? N2 C26 C31 C35 -6.9(7) . . . . ? C28 C27 C32 C33 -53.4(7) . . . . ? C26 C27 C32 C33 128.4(5) . . . . ? C28 C27 C32 C34 68.8(6) . . . . ? C26 C27 C32 C34 -109.4(6) . . . . ? C30 C31 C35 C37 -29.7(7) . . . . ? C26 C31 C35 C37 152.5(5) . . . . ? C30 C31 C35 C36 94.9(6) . . . . ? C26 C31 C35 C36 -82.9(6) . . . . ? C55 N3 C39 C40 -171.4(5) . . . . ? Sm2 N3 C39 C40 14.1(8) . . . . ? C55 N3 C39 C38 6.0(7) . . . . ? Sm2 N3 C39 C38 -168.6(4) . . . . ? N3 C39 C40 C41 15.0(9) . . . . ? C38 C39 C40 C41 -162.5(5) . . . . ? C43 N4 C41 C40 171.0(5) . . . . ? Sm2 N4 C41 C40 -20.0(7) . . . . ? C43 N4 C41 C42 -7.1(7) . . . . ? Sm2 N4 C41 C42 161.9(4) . . . . ? C39 C40 C41 N4 -11.6(10) . . . . ? C39 C40 C41 C42 166.6(6) . . . . ? C41 N4 C43 C44 -93.6(6) . . . . ? Sm2 N4 C43 C44 96.5(5) . . . . ? C41 N4 C43 C48 84.7(6) . . . . ? Sm2 N4 C43 C48 -85.2(5) . . . . ? C48 C43 C44 C45 -1.8(8) . . . . ? N4 C43 C44 C45 176.5(4) . . . . ? C48 C43 C44 C52 180.0(5) . . . . ? N4 C43 C44 C52 -1.8(7) . . . . ? C43 C44 C45 C46 0.4(8) . . . . ? C52 C44 C45 C46 178.7(5) . . . . ? C44 C45 C46 C47 0.6(9) . . . . ? C45 C46 C47 C48 -0.3(9) . . . . ? C46 C47 C48 C43 -1.0(8) . . . . ? C46 C47 C48 C49 -178.1(5) . . . . ? C44 C43 C48 C47 2.1(8) . . . . ? N4 C43 C48 C47 -176.1(5) . . . . ? C44 C43 C48 C49 179.0(5) . . . . ? N4 C43 C48 C49 0.7(8) . . . . ? C47 C48 C49 C51 -66.5(7) . . . . ? C43 C48 C49 C51 116.6(6) . . . . ? C47 C48 C49 C50 55.5(7) . . . . ? C43 C48 C49 C50 -121.4(6) . . . . ? C45 C44 C52 C54 -86.1(7) . . . . ? C43 C44 C52 C54 92.2(7) . . . . ? C45 C44 C52 C53 37.7(7) . . . . ? C43 C44 C52 C53 -144.0(5) . . . . ? C39 N3 C55 C56 -80.8(6) . . . . ? Sm2 N3 C55 C56 94.5(5) . . . . ? C39 N3 C55 C60 103.0(6) . . . . ? Sm2 N3 C55 C60 -81.7(5) . . . . ? C60 C55 C56 C57 0.9(8) . . . . ? N3 C55 C56 C57 -175.2(4) . . . . ? C60 C55 C56 C64 179.7(5) . . . . ? N3 C55 C56 C64 3.7(7) . . . . ? C55 C56 C57 C58 -1.4(8) . . . . ? C64 C56 C57 C58 179.7(5) . . . . ? C56 C57 C58 C59 1.1(8) . . . . ? C57 C58 C59 C60 -0.2(9) . . . . ? C58 C59 C60 C55 -0.4(8) . . . . ? C58 C59 C60 C61 -179.9(5) . . . . ? C56 C55 C60 C59 0.0(8) . . . . ? N3 C55 C60 C59 176.2(5) . . . . ? C56 C55 C60 C61 179.6(5) . . . . ? N3 C55 C60 C61 -4.3(7) . . . . ? C59 C60 C61 C62 91.5(7) . . . . ? C55 C60 C61 C62 -88.0(6) . . . . ? C59 C60 C61 C63 -35.4(7) . . . . ? C55 C60 C61 C63 145.1(5) . . . . ? C57 C56 C64 C66 64.1(6) . . . . ? C55 C56 C64 C66 -114.7(6) . . . . ? C57 C56 C64 C65 -59.0(7) . . . . ? C55 C56 C64 C65 122.1(6) . . . . ? C84 N5 C68 C69 164.0(5) . . . . ? Sm3 N5 C68 C69 -24.8(7) . . . . ? C84 N5 C68 C67 -12.9(7) . . . . ? Sm3 N5 C68 C67 158.3(4) . . . . ? N5 C68 C69 C70 -10.4(10) . . . . ? C67 C68 C69 C70 166.6(5) . . . . ? C72 N6 C70 C69 -176.6(5) . . . . ? Sm3 N6 C70 C69 9.1(7) . . . . ? C72 N6 C70 C71 2.4(7) . . . . ? Sm3 N6 C70 C71 -171.9(3) . . . . ? C68 C69 C70 N6 19.3(9) . . . . ? C68 C69 C70 C71 -159.8(6) . . . . ? C70 N6 C72 C77 108.5(6) . . . . ? Sm3 N6 C72 C77 -76.6(5) . . . . ? C70 N6 C72 C73 -78.4(6) . . . . ? Sm3 N6 C72 C73 96.5(5) . . . . ? C77 C72 C73 C74 -0.3(8) . . . . ? N6 C72 C73 C74 -173.1(5) . . . . ? C77 C72 C73 C81 176.5(5) . . . . ? N6 C72 C73 C81 3.7(8) . . . . ? C72 C73 C74 C75 1.9(8) . . . . ? C81 C73 C74 C75 -175.2(5) . . . . ? C73 C74 C75 C76 -1.4(8) . . . . ? C74 C75 C76 C77 -0.7(9) . . . . ? C75 C76 C77 C72 2.2(8) . . . . ? C75 C76 C77 C78 -177.5(5) . . . . ? C73 C72 C77 C76 -1.7(8) . . . . ? N6 C72 C77 C76 171.3(5) . . . . ? C73 C72 C77 C78 178.0(5) . . . . ? N6 C72 C77 C78 -9.0(7) . . . . ? C76 C77 C78 C80 95.7(6) . . . . ? C72 C77 C78 C80 -84.1(6) . . . . ? C76 C77 C78 C79 -29.9(7) . . . . ? C72 C77 C78 C79 150.4(5) . . . . ? C74 C73 C81 C82 -58.0(6) . . . . ? C72 C73 C81 C82 125.2(5) . . . . ? C74 C73 C81 C83 65.5(6) . . . . ? C72 C73 C81 C83 -111.3(5) . . . . ? C68 N5 C84 C89 90.6(6) . . . . ? Sm3 N5 C84 C89 -81.1(5) . . . . ? C68 N5 C84 C85 -90.1(6) . . . . ? Sm3 N5 C84 C85 98.2(4) . . . . ? C89 C84 C85 C86 -1.4(8) . . . . ? N5 C84 C85 C86 179.3(4) . . . . ? C89 C84 C85 C93 -178.5(5) . . . . ? N5 C84 C85 C93 2.1(7) . . . . ? C84 C85 C86 C87 0.5(8) . . . . ? C93 C85 C86 C87 177.7(5) . . . . ? C85 C86 C87 C88 -0.1(9) . . . . ? C86 C87 C88 C89 0.5(9) . . . . ? C87 C88 C89 C84 -1.3(8) . . . . ? C87 C88 C89 C90 -178.8(5) . . . . ? C85 C84 C89 C88 1.8(8) . . . . ? N5 C84 C89 C88 -178.9(5) . . . . ? C85 C84 C89 C90 179.1(5) . . . . ? N5 C84 C89 C90 -1.5(8) . . . . ? C88 C89 C90 C92 -60.6(6) . . . . ? C84 C89 C90 C92 122.0(6) . . . . ? C88 C89 C90 C91 61.8(7) . . . . ? C84 C89 C90 C91 -115.6(6) . . . . ? C86 C85 C93 C95 42.1(7) . . . . ? C84 C85 C93 C95 -140.8(5) . . . . ? C86 C85 C93 C94 -82.0(6) . . . . ? C84 C85 C93 C94 95.1(6) . . . . ? C113 N8 C97 C98 165.4(5) . . . . ? Sm4 N8 C97 C98 -21.5(7) . . . . ? C113 N8 C97 C96 -14.1(7) . . . . ? Sm4 N8 C97 C96 159.0(4) . . . . ? N8 C97 C98 C99 -12.0(9) . . . . ? C96 C97 C98 C99 167.5(6) . . . . ? C101 N7 C99 C98 -175.4(5) . . . . ? Sm4 N7 C99 C98 11.4(7) . . . . ? C101 N7 C99 C100 2.2(7) . . . . ? Sm4 N7 C99 C100 -171.0(4) . . . . ? C97 C98 C99 N7 17.2(9) . . . . ? C97 C98 C99 C100 -160.6(6) . . . . ? C99 N7 C101 C102 -77.1(6) . . . . ? Sm4 N7 C101 C102 96.9(5) . . . . ? C99 N7 C101 C106 109.2(6) . . . . ? Sm4 N7 C101 C106 -76.8(5) . . . . ? C106 C101 C102 C103 -0.4(8) . . . . ? N7 C101 C102 C103 -173.9(5) . . . . ? C106 C101 C102 C110 177.8(5) . . . . ? N7 C101 C102 C110 4.4(8) . . . . ? C101 C102 C103 C104 1.3(8) . . . . ? C110 C102 C103 C104 -177.1(5) . . . . ? C102 C103 C104 C105 -1.7(9) . . . . ? C103 C104 C105 C106 1.1(9) . . . . ? C104 C105 C106 C101 -0.3(8) . . . . ? C104 C105 C106 C107 -179.4(5) . . . . ? C102 C101 C106 C105 0.0(8) . . . . ? N7 C101 C106 C105 173.6(5) . . . . ? C102 C101 C106 C107 179.1(5) . . . . ? N7 C101 C106 C107 -7.3(8) . . . . ? C105 C106 C107 C108 95.8(6) . . . . ? C101 C106 C107 C108 -83.3(6) . . . . ? C105 C106 C107 C109 -29.2(8) . . . . ? C101 C106 C107 C109 151.7(5) . . . . ? C103 C102 C110 C111 66.8(6) . . . . ? C101 C102 C110 C111 -111.4(6) . . . . ? C103 C102 C110 C112 -58.0(7) . . . . ? C101 C102 C110 C112 123.8(6) . . . . ? C97 N8 C113 C114 87.4(6) . . . . ? Sm4 N8 C113 C114 -86.5(5) . . . . ? C97 N8 C113 C118 -92.4(6) . . . . ? Sm4 N8 C113 C118 93.7(5) . . . . ? C118 C113 C114 C115 -1.6(8) . . . . ? N8 C113 C114 C115 178.6(5) . . . . ? C118 C113 C114 C122 176.3(5) . . . . ? N8 C113 C114 C122 -3.5(8) . . . . ? C113 C114 C115 C116 0.6(8) . . . . ? C122 C114 C115 C116 -177.4(5) . . . . ? C114 C115 C116 C117 0.1(9) . . . . ? C115 C116 C117 C118 0.2(9) . . . . ? C116 C117 C118 C113 -1.1(8) . . . . ? C116 C117 C118 C119 177.8(5) . . . . ? C114 C113 C118 C117 1.9(8) . . . . ? N8 C113 C118 C117 -178.3(5) . . . . ? C114 C113 C118 C119 -177.1(5) . . . . ? N8 C113 C118 C119 2.7(7) . . . . ? C117 C118 C119 C120 -90.7(6) . . . . ? C113 C118 C119 C120 88.2(6) . . . . ? C117 C118 C119 C121 32.8(7) . . . . ? C113 C118 C119 C121 -148.3(5) . . . . ? C113 C114 C122 C123 115.9(6) . . . . ? C115 C114 C122 C123 -66.2(6) . . . . ? C113 C114 C122 C124 -121.1(6) . . . . ? C115 C114 C122 C124 56.8(7) . . . . ? C131 C125 C126 C127 178.2(8) . . . . ? C130 C125 C126 C127 -1.3(11) . . . . ? C125 C126 C127 C128 0.0(12) . . . . ? C126 C127 C128 C129 -1.1(14) . . . . ? C127 C128 C129 C130 4.0(19) . . . . ? C128 C129 C130 C125 -5(2) . . . . ? C126 C125 C130 C129 3.5(14) . . . . ? C131 C125 C130 C129 -176.0(10) . . . . ? C138 C132 C133 C134 177.9(8) . . . . ? C137 C132 C133 C134 2.3(11) . . . . ? C132 C133 C134 C135 -2.1(15) . . . . ? C133 C134 C135 C136 0.5(16) . . . . ? C134 C135 C136 C137 1.0(14) . . . . ? C135 C136 C137 C132 -0.5(14) . . . . ? C138 C132 C137 C136 -176.8(9) . . . . ? C133 C132 C137 C136 -1.3(12) . . . . ? C144 C139 C140 C141 -1.6(16) . . . . ? C145 C139 C140 C141 179.0(10) . . . . ? C139 C140 C141 C142 2.1(16) . . . . ? C140 C141 C142 C143 0.2(15) . . . . ? C141 C142 C143 C144 -2.6(11) . . . . ? C140 C139 C144 C143 -1.0(12) . . . . ? C145 C139 C144 C143 178.3(9) . . . . ? C142 C143 C144 C139 2.9(10) . . . . ? C151 C146 C147 C148 1.4(11) . . . . ? C152 C146 C147 C148 180.0(8) . . . . ? C146 C147 C148 C149 -1.0(13) . . . . ? C147 C148 C149 C150 -0.2(13) . . . . ? C148 C149 C150 C151 1.0(13) . . . . ? C149 C150 C151 C146 -0.6(13) . . . . ? C147 C146 C151 C150 -0.6(12) . . . . ? C152 C146 C151 C150 -179.1(8) . . . . ? C156 C153 C154 C157 -2(2) 3_666 . . . ? C157 C153 C154 C157 -1.3(19) 3_666 . . . ? C156 C153 C154 C157 -0.3(12) 3_666 . . 3_666 ? C156 C153 C154 C155 -16(15) 3_666 . . . ? C157 C153 C154 C155 -16(14) 3_666 . . . ? C157 C154 C155 C156 1.7(17) . . . . ? C153 C154 C155 C156 17(15) . . . . ? C157 C154 C155 C156 1.5(16) 3_666 . . . ? C153 C154 C155 C157 15(14) . . . . ? C157 C154 C155 C157 -0.2(17) 3_666 . . . ? C157 C155 C156 C153 -1(2) . . . 3_666 ? C154 C155 C156 C153 -2(3) . . . 3_666 ? C154 C155 C156 C157 -1.1(11) . . . . ? C153 C154 C157 C157 2(3) . . . 3_666 ? C155 C154 C157 C157 -180(2) . . . 3_666 ? C153 C154 C157 C155 -178.5(13) . . . . ? C157 C154 C157 C155 180(2) 3_666 . . . ? C153 C154 C157 C156 180.0(14) . . . . ? C157 C154 C157 C156 178(3) 3_666 . . . ? C155 C154 C157 C156 -1.5(15) . . . . ? C153 C154 C157 C154 2(3) . . . 3_666 ? C157 C154 C157 C154 0.000(6) 3_666 . . 3_666 ? C155 C154 C157 C154 -180(2) . . . 3_666 ? C153 C154 C157 C153 138(54) . . . 3_666 ? C157 C154 C157 C153 136(56) 3_666 . . 3_666 ? C155 C154 C157 C153 -44(55) . . . 3_666 ? C156 C155 C157 C154 -178.5(15) . . . . ? C156 C155 C157 C157 -159(100) . . . 3_666 ? C154 C155 C157 C157 19(100) . . . 3_666 ? C154 C155 C157 C156 178.5(15) . . . . ? C156 C155 C157 C154 1(2) . . . 3_666 ? C154 C155 C157 C154 180(3) . . . 3_666 ? C156 C155 C157 C153 0.4(12) . . . 3_666 ? C154 C155 C157 C153 178.9(16) . . . 3_666 ? C155 C156 C157 C154 2(2) . . . . ? C153 C156 C157 C154 -178(2) 3_666 . . . ? C155 C156 C157 C157 180(3) . . . 3_666 ? C153 C156 C157 C157 -1(3) 3_666 . . 3_666 ? C153 C156 C157 C155 179.5(16) 3_666 . . . ? C155 C156 C157 C154 -179.2(14) . . . 3_666 ? C153 C156 C157 C154 0.2(10) 3_666 . . 3_666 ? C155 C156 C157 C153 -179.5(16) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.888 _diffrn_reflns_theta_full 25.74 _diffrn_measured_fraction_theta_full 0.888 _refine_diff_density_max 1.078 _refine_diff_density_min -1.205 _refine_diff_density_rms 0.115 #===================================== data_NACSmCpCH2SiMe3 _database_code_depnum_ccdc_archive 'CCDC 244223' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H68 N2 Si Sm, 0.5(C6 H12)' _chemical_formula_sum 'C49 H75 N2 Si Sm' _chemical_formula_weight 870.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 16.573(3) _cell_length_b 22.284(5) _cell_length_c 12.794(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4725.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6764 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 24.49 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1836 _exptl_absorpt_coefficient_mu 1.300 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6736 _exptl_absorpt_correction_T_max 0.9031 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method /w\2/q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20176 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4200 _reflns_number_gt 3218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.052d' _computing_cell_refinement 'Bruker SAINT v5.10' _computing_data_reduction 'Bruker SAINT v5.10' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A half molecule of hexane is present in the asymmetric unit. The hexane is disordered across the inversion center at [0.5, 0.5, 1]. This disorder results in some unsual bond lengths and angles. ; _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^)+(0.0520P)^2^+3.7095P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4200 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0997 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.578610(15) 0.2500 0.45211(2) 0.02491(12) Uani 1 2 d S . . Si1 Si 0.56843(10) 0.2500 0.14208(14) 0.0444(5) Uani 1 2 d S . . N1 N 0.68932(19) 0.31893(15) 0.4623(3) 0.0298(8) Uani 1 1 d . . . C1 C 0.5131(3) 0.2500 0.6449(4) 0.0308(14) Uani 1 2 d S . . C2 C 0.4790(2) 0.3018(2) 0.5971(3) 0.0339(10) Uani 1 1 d . . . C3 C 0.4248(2) 0.2816(2) 0.5187(3) 0.0345(10) Uani 1 1 d . . . C4 C 0.5670(4) 0.2500 0.7385(5) 0.055(2) Uani 1 2 d S . . H4A H 0.5818 0.2914 0.7561 0.083 Uiso 0.50 1 calc PR . . H4B H 0.6160 0.2269 0.7231 0.083 Uiso 0.50 1 calc PR . . H4C H 0.5387 0.2317 0.7977 0.083 Uiso 0.50 1 calc PR . . C5 C 0.4914(3) 0.3656(2) 0.6327(4) 0.0533(13) Uani 1 1 d . . . H5A H 0.5416 0.3684 0.6729 0.080 Uiso 1 1 calc R . . H5B H 0.4459 0.3780 0.6766 0.080 Uiso 1 1 calc R . . H5C H 0.4948 0.3920 0.5715 0.080 Uiso 1 1 calc R . . C6 C 0.3665(3) 0.3190(3) 0.4568(4) 0.0536(14) Uani 1 1 d . . . H6A H 0.3765 0.3132 0.3820 0.080 Uiso 1 1 calc R . . H6B H 0.3738 0.3615 0.4746 0.080 Uiso 1 1 calc R . . H6C H 0.3112 0.3068 0.4734 0.080 Uiso 1 1 calc R . . C7 C 0.7490(2) 0.3076(2) 0.3952(3) 0.0340(10) Uani 1 1 d . . . C8 C 0.7690(3) 0.2500 0.3591(5) 0.0356(14) Uani 1 2 d S . . H8 H 0.8024 0.2500 0.2987 0.043 Uiso 1 2 calc SR . . C9 C 0.8018(3) 0.3579(2) 0.3537(4) 0.0494(13) Uani 1 1 d . . . H9A H 0.8045 0.3903 0.4054 0.074 Uiso 1 1 calc R . . H9B H 0.7787 0.3734 0.2885 0.074 Uiso 1 1 calc R . . H9C H 0.8562 0.3425 0.3403 0.074 Uiso 1 1 calc R . . C10 C 0.6828(2) 0.3782(2) 0.5078(4) 0.0364(11) Uani 1 1 d . . . C11 C 0.6437(3) 0.4245(2) 0.4537(4) 0.0433(11) Uani 1 1 d . . . C12 C 0.6338(3) 0.4811(2) 0.5056(5) 0.0558(14) Uani 1 1 d . . . C13 C 0.6636(3) 0.4897(2) 0.6049(5) 0.0593(15) Uani 1 1 d . . . C14 C 0.7027(3) 0.4433(2) 0.6575(4) 0.0563(14) Uani 1 1 d . . . C15 C 0.7127(3) 0.3868(2) 0.6094(4) 0.0445(12) Uani 1 1 d . . . C16 C 0.6110(3) 0.4175(2) 0.3439(4) 0.0467(12) Uani 1 1 d . . . H16 H 0.6283 0.3773 0.3174 0.056 Uiso 1 1 calc R . . C17 C 0.5193(3) 0.4193(3) 0.3422(4) 0.0626(15) Uani 1 1 d . . . H17A H 0.5002 0.4129 0.2706 0.094 Uiso 1 1 calc R . . H17B H 0.5007 0.4585 0.3672 0.094 Uiso 1 1 calc R . . H17C H 0.4980 0.3877 0.3877 0.094 Uiso 1 1 calc R . . C18 C 0.6446(4) 0.4655(3) 0.2689(5) 0.0786(19) Uani 1 1 d . . . H18A H 0.6250 0.4577 0.1979 0.118 Uiso 1 1 calc R . . H18B H 0.7037 0.4640 0.2695 0.118 Uiso 1 1 calc R . . H18C H 0.6266 0.5053 0.2916 0.118 Uiso 1 1 calc R . . C19 C 0.7580(3) 0.3382(2) 0.6659(4) 0.0548(14) Uani 1 1 d . . . H19 H 0.7337 0.2990 0.6448 0.066 Uiso 1 1 calc R . . C20 C 0.7539(4) 0.3419(3) 0.7854(4) 0.0684(16) Uani 1 1 d . . . H20A H 0.7804 0.3066 0.8158 0.103 Uiso 1 1 calc R . . H20B H 0.6973 0.3429 0.8077 0.103 Uiso 1 1 calc R . . H20C H 0.7813 0.3783 0.8093 0.103 Uiso 1 1 calc R . . C21 C 0.8470(3) 0.3371(3) 0.6329(5) 0.0771(19) Uani 1 1 d . . . H21A H 0.8757 0.3063 0.6729 0.116 Uiso 1 1 calc R . . H21B H 0.8714 0.3764 0.6464 0.116 Uiso 1 1 calc R . . H21C H 0.8507 0.3279 0.5581 0.116 Uiso 1 1 calc R . . C22 C 0.5241(3) 0.2500 0.2734(5) 0.0399(16) Uani 1 2 d S . . H22A H 0.4879 0.2147 0.2725 0.048 Uiso 0.50 1 calc PR . . H22B H 0.4879 0.2853 0.2725 0.048 Uiso 0.50 1 calc PR . . C23 C 0.6366(5) 0.3154(3) 0.1190(5) 0.095(2) Uani 1 1 d . . . H23A H 0.6587 0.3132 0.0480 0.143 Uiso 1 1 calc R . . H23B H 0.6809 0.3146 0.1697 0.143 Uiso 1 1 calc R . . H23C H 0.6061 0.3528 0.1270 0.143 Uiso 1 1 calc R . . C24 C 0.4936(6) 0.2728(4) 0.0378(7) 0.058(3) Uiso 0.50 1 d P . . H24A H 0.5202 0.2725 -0.0306 0.087 Uiso 0.50 1 calc PR . . H24B H 0.4734 0.3132 0.0528 0.087 Uiso 0.50 1 calc PR . . H24C H 0.4484 0.2444 0.0372 0.087 Uiso 0.50 1 calc PR . . C30 C 0.6410(8) 0.4765(6) 0.9512(9) 0.181(5) Uiso 1 1 d . . . H30A H 0.6799 0.4818 0.8943 0.272 Uiso 1 1 calc R . . H30B H 0.6572 0.4422 0.9944 0.272 Uiso 1 1 calc R . . H30C H 0.6397 0.5128 0.9943 0.272 Uiso 1 1 calc R . . C31 C 0.5750(8) 0.4674(7) 0.9152(12) 0.199(6) Uiso 1 1 d . . . H31A H 0.5745 0.4257 0.8886 0.239 Uiso 1 1 calc R . . H31B H 0.5689 0.4941 0.8538 0.239 Uiso 1 1 calc R . . C32 C 0.5030(8) 0.4751(4) 0.9801(10) 0.162(4) Uiso 1 1 d . . . H32A H 0.4546 0.4675 0.9367 0.194 Uiso 1 1 calc R . . H32B H 0.5038 0.4446 1.0364 0.194 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 Sm1 0.01715(16) 0.03351(18) 0.02407(18) 0.000 0.00182(13) 0.000 Si1 0.0276(9) 0.0805(14) 0.0253(10) 0.000 0.0008(8) 0.000 N1 0.0266(18) 0.0345(19) 0.028(2) -0.0024(16) 0.0022(15) -0.0029(15) C1 0.016(3) 0.058(4) 0.018(3) 0.000 0.004(2) 0.000 C2 0.025(2) 0.047(3) 0.030(2) -0.007(2) 0.0124(19) 0.0007(19) C3 0.019(2) 0.055(3) 0.030(2) 0.0005(19) 0.0056(17) 0.0040(18) C4 0.032(4) 0.111(7) 0.023(4) 0.000 0.003(3) 0.000 C5 0.054(3) 0.052(3) 0.053(3) -0.015(3) 0.019(3) 0.001(2) C6 0.036(3) 0.079(4) 0.046(3) 0.015(3) 0.011(2) 0.025(3) C7 0.024(2) 0.053(3) 0.026(2) 0.001(2) -0.0032(18) -0.0069(19) C8 0.024(3) 0.057(4) 0.026(3) 0.000 0.008(3) 0.000 C9 0.036(3) 0.057(3) 0.055(3) 0.004(3) 0.009(2) -0.013(2) C10 0.024(2) 0.041(3) 0.044(3) -0.003(2) 0.006(2) -0.0089(19) C11 0.036(2) 0.041(3) 0.053(3) -0.001(2) 0.009(2) -0.008(2) C12 0.057(3) 0.043(3) 0.067(4) -0.009(3) 0.006(3) -0.009(3) C13 0.059(3) 0.044(3) 0.075(4) -0.021(3) 0.005(3) -0.011(3) C14 0.048(3) 0.056(3) 0.066(4) -0.019(3) 0.005(3) -0.014(3) C15 0.033(3) 0.054(3) 0.047(3) -0.010(2) 0.001(2) -0.011(2) C16 0.051(3) 0.038(3) 0.051(3) 0.007(2) 0.003(3) 0.000(2) C17 0.052(3) 0.083(4) 0.053(3) -0.004(3) -0.004(3) 0.012(3) C18 0.104(5) 0.059(4) 0.073(4) 0.019(3) 0.011(4) -0.019(4) C19 0.055(3) 0.057(3) 0.052(3) -0.014(3) -0.015(3) -0.008(3) C20 0.079(4) 0.074(4) 0.053(4) -0.013(3) -0.013(3) -0.017(3) C21 0.057(4) 0.112(5) 0.063(4) -0.026(4) -0.014(3) 0.014(4) C22 0.021(3) 0.065(5) 0.034(4) 0.000 0.001(3) 0.000 C23 0.132(6) 0.095(5) 0.059(4) 0.007(4) 0.043(4) -0.017(5) _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 N1 2.397(3) . ? Sm1 N1 2.397(3) 7_565 ? Sm1 C22 2.458(6) . ? Sm1 C1 2.694(5) . ? Sm1 C2 2.738(4) . ? Sm1 C2 2.738(4) 7_565 ? Sm1 C3 2.779(4) 7_565 ? Sm1 C3 2.779(4) . ? Si1 C22 1.834(6) . ? Si1 C23 1.869(6) 7_565 ? Si1 C23 1.869(6) . ? Si1 C24 1.891(10) 7_565 ? Si1 C24 1.891(10) . ? N1 C7 1.334(5) . ? N1 C10 1.447(5) . ? C1 C2 1.423(5) 7_565 ? C1 C2 1.423(5) . ? C1 C4 1.494(8) . ? C2 C3 1.419(6) . ? C2 C5 1.508(6) . ? C3 C3 1.410(9) 7_565 ? C3 C6 1.501(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.404(5) . ? C7 C9 1.518(6) . ? C8 C7 1.404(5) 7_565 ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.402(6) . ? C10 C15 1.405(7) . ? C11 C12 1.433(7) . ? C11 C16 1.514(6) . ? C12 C13 1.377(8) . ? C13 C14 1.393(8) . ? C14 C15 1.411(7) . ? C15 C19 1.502(7) . ? C16 C17 1.520(7) . ? C16 C18 1.542(7) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.532(7) . ? C19 C21 1.535(7) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C30 C31 1.204(14) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.465(15) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C32 1.227(18) 5_667 ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? 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 Sm1 N1 79.73(16) . 7_565 ? N1 Sm1 C22 109.38(13) . . ? N1 Sm1 C22 109.38(13) 7_565 . ? N1 Sm1 C1 104.98(11) . . ? N1 Sm1 C1 104.98(11) 7_565 . ? C22 Sm1 C1 134.70(18) . . ? N1 Sm1 C2 98.90(12) . . ? N1 Sm1 C2 134.02(12) 7_565 . ? C22 Sm1 C2 114.12(15) . . ? C1 Sm1 C2 30.36(11) . . ? N1 Sm1 C2 134.02(12) . 7_565 ? N1 Sm1 C2 98.90(12) 7_565 7_565 ? C22 Sm1 C2 114.12(15) . 7_565 ? C1 Sm1 C2 30.36(11) . 7_565 ? C2 Sm1 C2 49.84(19) . 7_565 ? N1 Sm1 C3 148.02(12) . 7_565 ? N1 Sm1 C3 121.54(12) 7_565 7_565 ? C22 Sm1 C3 87.04(16) . 7_565 ? C1 Sm1 C3 49.44(14) . 7_565 ? C2 Sm1 C3 49.15(13) . 7_565 ? C2 Sm1 C3 29.79(12) 7_565 7_565 ? N1 Sm1 C3 121.54(12) . . ? N1 Sm1 C3 148.02(12) 7_565 . ? C22 Sm1 C3 87.04(16) . . ? C1 Sm1 C3 49.44(14) . . ? C2 Sm1 C3 29.79(12) . . ? C2 Sm1 C3 49.15(13) 7_565 . ? C3 Sm1 C3 29.39(19) 7_565 . ? C22 Si1 C23 112.8(2) . 7_565 ? C22 Si1 C23 112.8(2) . . ? C23 Si1 C23 102.6(5) 7_565 . ? C22 Si1 C24 112.6(4) . 7_565 ? C23 Si1 C24 94.3(4) 7_565 7_565 ? C23 Si1 C24 119.6(4) . 7_565 ? C22 Si1 C24 112.6(4) . . ? C23 Si1 C24 119.6(4) 7_565 . ? C23 Si1 C24 94.3(4) . . ? C7 N1 C10 119.2(3) . . ? C7 N1 Sm1 114.3(3) . . ? C10 N1 Sm1 123.3(2) . . ? C2 C1 C2 108.3(5) 7_565 . ? C2 C1 C4 125.6(3) 7_565 . ? C2 C1 C4 125.6(3) . . ? C2 C1 Sm1 76.5(3) 7_565 . ? C2 C1 Sm1 76.5(3) . . ? C4 C1 Sm1 119.5(4) . . ? C3 C2 C1 107.4(4) . . ? C3 C2 C5 126.7(4) . . ? C1 C2 C5 125.5(4) . . ? C3 C2 Sm1 76.7(2) . . ? C1 C2 Sm1 73.1(3) . . ? C5 C2 Sm1 121.3(3) . . ? C3 C3 C2 108.4(3) 7_565 . ? C3 C3 C6 123.7(3) 7_565 . ? C2 C3 C6 127.2(4) . . ? C3 C3 Sm1 75.30(9) 7_565 . ? C2 C3 Sm1 73.5(2) . . ? C6 C3 Sm1 124.7(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C8 124.1(4) . . ? N1 C7 C9 120.8(4) . . ? C8 C7 C9 115.1(4) . . ? C7 C8 C7 132.2(5) 7_565 . ? C7 C8 H8 113.9 7_565 . ? C7 C8 H8 113.9 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 121.3(4) . . ? C11 C10 N1 120.6(4) . . ? C15 C10 N1 118.1(4) . . ? C10 C11 C12 118.2(5) . . ? C10 C11 C16 123.2(4) . . ? C12 C11 C16 118.7(5) . . ? C13 C12 C11 120.6(5) . . ? C12 C13 C14 120.6(5) . . ? C13 C14 C15 120.4(5) . . ? C10 C15 C14 119.0(5) . . ? C10 C15 C19 121.6(4) . . ? C14 C15 C19 119.4(5) . . ? C11 C16 C17 111.6(4) . . ? C11 C16 C18 112.1(4) . . ? C17 C16 C18 109.5(5) . . ? C11 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C18 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 C20 114.8(5) . . ? C15 C19 C21 111.1(5) . . ? C20 C19 C21 108.6(4) . . ? C15 C19 H19 107.3 . . ? C20 C19 H19 107.3 . . ? C21 C19 H19 107.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 Sm1 134.8(3) . . ? Si1 C22 H22A 103.5 . . ? Sm1 C22 H22A 103.5 . . ? Si1 C22 H22B 103.5 . . ? Sm1 C22 H22B 103.5 . . ? H22A C22 H22B 105.3 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C30 C31 C32 120.3(16) . . ? C30 C31 H31A 107.3 . . ? C32 C31 H31A 107.2 . . ? C30 C31 H31B 107.2 . . ? C32 C31 H31B 107.2 . . ? H31A C31 H31B 106.9 . . ? C32 C32 C31 113.9(17) 5_667 . ? C32 C32 H32A 108.8 5_667 . ? C31 C32 H32A 108.8 . . ? C32 C32 H32B 108.8 5_667 . ? C31 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Sm1 N1 C7 49.6(3) 7_565 . . . ? C22 Sm1 N1 C7 -57.4(3) . . . . ? C1 Sm1 N1 C7 152.6(3) . . . . ? C2 Sm1 N1 C7 -177.0(3) . . . . ? C2 Sm1 N1 C7 142.1(3) 7_565 . . . ? C3 Sm1 N1 C7 -174.8(3) 7_565 . . . ? C3 Sm1 N1 C7 -156.2(3) . . . . ? N1 Sm1 N1 C10 -150.9(3) 7_565 . . . ? C22 Sm1 N1 C10 102.1(3) . . . . ? C1 Sm1 N1 C10 -47.9(3) . . . . ? C2 Sm1 N1 C10 -17.5(3) . . . . ? C2 Sm1 N1 C10 -58.4(4) 7_565 . . . ? C3 Sm1 N1 C10 -15.3(4) 7_565 . . . ? C3 Sm1 N1 C10 3.3(4) . . . . ? N1 Sm1 C1 C2 -165.1(2) . . . 7_565 ? N1 Sm1 C1 C2 -81.9(3) 7_565 . . 7_565 ? C22 Sm1 C1 C2 56.5(2) . . . 7_565 ? C2 Sm1 C1 C2 113.0(5) . . . 7_565 ? C3 Sm1 C1 C2 37.0(3) 7_565 . . 7_565 ? C3 Sm1 C1 C2 76.0(3) . . . 7_565 ? N1 Sm1 C1 C2 81.9(3) . . . . ? N1 Sm1 C1 C2 165.1(2) 7_565 . . . ? C22 Sm1 C1 C2 -56.5(2) . . . . ? C2 Sm1 C1 C2 -113.0(5) 7_565 . . . ? C3 Sm1 C1 C2 -76.0(3) 7_565 . . . ? C3 Sm1 C1 C2 -37.0(3) . . . . ? N1 Sm1 C1 C4 -41.57(9) . . . . ? N1 Sm1 C1 C4 41.57(9) 7_565 . . . ? C22 Sm1 C1 C4 180.0 . . . . ? C2 Sm1 C1 C4 -123.5(2) . . . . ? C2 Sm1 C1 C4 123.5(2) 7_565 . . . ? C3 Sm1 C1 C4 160.50(13) 7_565 . . . ? C3 Sm1 C1 C4 -160.50(13) . . . . ? C2 C1 C2 C3 -0.9(6) 7_565 . . . ? C4 C1 C2 C3 -173.4(5) . . . . ? Sm1 C1 C2 C3 69.7(3) . . . . ? C2 C1 C2 C5 172.6(3) 7_565 . . . ? C4 C1 C2 C5 0.1(8) . . . . ? Sm1 C1 C2 C5 -116.8(4) . . . . ? C2 C1 C2 Sm1 -70.6(4) 7_565 . . . ? C4 C1 C2 Sm1 116.9(5) . . . . ? N1 Sm1 C2 C3 142.4(3) . . . . ? N1 Sm1 C2 C3 -133.3(3) 7_565 . . . ? C22 Sm1 C2 C3 26.4(3) . . . . ? C1 Sm1 C2 C3 -113.1(4) . . . . ? C2 Sm1 C2 C3 -75.6(3) 7_565 . . . ? C3 Sm1 C2 C3 -36.1(3) 7_565 . . . ? N1 Sm1 C2 C1 -104.5(3) . . . . ? N1 Sm1 C2 C1 -20.2(3) 7_565 . . . ? C22 Sm1 C2 C1 139.5(2) . . . . ? C2 Sm1 C2 C1 37.5(3) 7_565 . . . ? C3 Sm1 C2 C1 77.0(3) 7_565 . . . ? C3 Sm1 C2 C1 113.1(4) . . . . ? N1 Sm1 C2 C5 17.3(4) . . . . ? N1 Sm1 C2 C5 101.5(4) 7_565 . . . ? C22 Sm1 C2 C5 -98.7(4) . . . . ? C1 Sm1 C2 C5 121.8(5) . . . . ? C2 Sm1 C2 C5 159.3(3) 7_565 . . . ? C3 Sm1 C2 C5 -161.2(4) 7_565 . . . ? C3 Sm1 C2 C5 -125.1(5) . . . . ? C1 C2 C3 C3 0.6(4) . . . 7_565 ? C5 C2 C3 C3 -172.9(4) . . . 7_565 ? Sm1 C2 C3 C3 67.82(10) . . . 7_565 ? C1 C2 C3 C6 171.4(4) . . . . ? C5 C2 C3 C6 -2.0(7) . . . . ? Sm1 C2 C3 C6 -121.3(4) . . . . ? C1 C2 C3 Sm1 -67.2(3) . . . . ? C5 C2 C3 Sm1 119.3(4) . . . . ? N1 Sm1 C3 C3 -159.79(12) . . . 7_565 ? N1 Sm1 C3 C3 -33.8(2) 7_565 . . 7_565 ? C22 Sm1 C3 C3 89.2(4) . . . 7_565 ? C1 Sm1 C3 C3 -77.03(10) . . . 7_565 ? C2 Sm1 C3 C3 -114.7(2) . . . 7_565 ? C2 Sm1 C3 C3 -36.62(16) 7_565 . . 7_565 ? N1 Sm1 C3 C2 -45.0(3) . . . . ? N1 Sm1 C3 C2 81.0(3) 7_565 . . . ? C22 Sm1 C3 C2 -156.0(3) . . . . ? C1 Sm1 C3 C2 37.7(2) . . . . ? C2 Sm1 C3 C2 78.1(3) 7_565 . . . ? C3 Sm1 C3 C2 114.7(2) 7_565 . . . ? N1 Sm1 C3 C6 79.1(4) . . . . ? N1 Sm1 C3 C6 -154.9(4) 7_565 . . . ? C22 Sm1 C3 C6 -31.9(4) . . . . ? C1 Sm1 C3 C6 161.9(5) . . . . ? C2 Sm1 C3 C6 124.2(5) . . . . ? C2 Sm1 C3 C6 -157.7(5) 7_565 . . . ? C3 Sm1 C3 C6 -121.1(4) 7_565 . . . ? C10 N1 C7 C8 169.5(4) . . . . ? Sm1 N1 C7 C8 -30.1(6) . . . . ? C10 N1 C7 C9 -9.4(6) . . . . ? Sm1 N1 C7 C9 151.0(3) . . . . ? N1 C7 C8 C7 -15.9(10) . . . 7_565 ? C9 C7 C8 C7 163.0(5) . . . 7_565 ? C7 N1 C10 C11 83.6(5) . . . . ? Sm1 N1 C10 C11 -74.9(5) . . . . ? C7 N1 C10 C15 -99.7(5) . . . . ? Sm1 N1 C10 C15 101.7(4) . . . . ? C15 C10 C11 C12 -1.0(7) . . . . ? N1 C10 C11 C12 175.6(4) . . . . ? C15 C10 C11 C16 179.5(4) . . . . ? N1 C10 C11 C16 -3.9(6) . . . . ? C10 C11 C12 C13 1.4(7) . . . . ? C16 C11 C12 C13 -179.1(5) . . . . ? C11 C12 C13 C14 -1.0(8) . . . . ? C12 C13 C14 C15 0.2(8) . . . . ? C11 C10 C15 C14 0.2(6) . . . . ? N1 C10 C15 C14 -176.4(4) . . . . ? C11 C10 C15 C19 -177.1(4) . . . . ? N1 C10 C15 C19 6.3(6) . . . . ? C13 C14 C15 C10 0.2(7) . . . . ? C13 C14 C15 C19 177.6(5) . . . . ? C10 C11 C16 C17 111.6(5) . . . . ? C12 C11 C16 C17 -67.8(6) . . . . ? C10 C11 C16 C18 -125.1(5) . . . . ? C12 C11 C16 C18 55.4(6) . . . . ? C10 C15 C19 C20 -154.0(4) . . . . ? C14 C15 C19 C20 28.7(7) . . . . ? C10 C15 C19 C21 82.3(5) . . . . ? C14 C15 C19 C21 -95.0(6) . . . . ? C23 Si1 C22 Sm1 57.8(3) 7_565 . . . ? C23 Si1 C22 Sm1 -57.8(3) . . . . ? C24 Si1 C22 Sm1 163.1(3) 7_565 . . . ? C24 Si1 C22 Sm1 -163.1(3) . . . . ? N1 Sm1 C22 Si1 42.80(9) . . . . ? N1 Sm1 C22 Si1 -42.81(9) 7_565 . . . ? C1 Sm1 C22 Si1 180.0 . . . . ? C2 Sm1 C22 Si1 152.51(10) . . . . ? C2 Sm1 C22 Si1 -152.51(10) 7_565 . . . ? C3 Sm1 C22 Si1 -165.29(9) 7_565 . . . ? C3 Sm1 C22 Si1 165.29(9) . . . . ? C30 C31 C32 C32 56(3) . . . 5_667 ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.649 _refine_diff_density_min -1.100 _refine_diff_density_rms 0.094 #=============================================== data_NacNacSmNTMS22 _database_code_depnum_ccdc_archive 'CCDC 245593' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Nacnac)Sm(NHAr)2 _chemical_melting_point ? _chemical_formula_moiety '2(C65 H101 N4 Sm), 1.5(C5H12)' _chemical_formula_sum 'C69 H100.75 N4 Sm' _chemical_formula_weight 1136.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 25.2973(6) _cell_length_b 13.4722(4) _cell_length_c 39.0529(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.4630(10) _cell_angle_gamma 90.00 _cell_volume 13088.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 30.69 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4838 _exptl_absorpt_coefficient_mu 0.937 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8063 _exptl_absorpt_correction_T_max 0.9121 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 57944 _diffrn_reflns_av_R_equivalents 0.0859 _diffrn_reflns_av_sigmaI/netI 0.1205 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.82 _reflns_number_total 22186 _reflns_number_gt 13402 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.052' _computing_cell_refinement 'Bruker SAINT v5.10' _computing_data_reduction 'Bruker SAINT v5.10' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A significant number of carbon atoms within the second molecule were found to be disordered over two positions. Where recommened, the carbon atoms were split into two equal occupancy atoms and refined isotropically. Hydrogen atoms were included on these disordered atoms, where appropriate. This disorder resulted in a number of unusual bond distances and thermal parameters within the molecules. Two molecules of disordered solvent were also located during the refinement. These regions of electron density are presumed to be disordered pentane molecules and have been refined with isotropic carbon atoms in the regions of dominant electron density. No attempt was made to include hydrogen atoms on these solvent molecules. In addition, one of the solvent molecules is disordered across the inversion center at [0.5, 0.5, 0.5]. ; _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^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22186 _refine_ls_number_parameters 1344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1163 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1374 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.152147(11) 0.66290(2) 0.356785(8) 0.01811(9) Uani 1 1 d . . . N11 N 0.14514(18) 0.5399(3) 0.31016(12) 0.0207(11) Uani 1 1 d . . . N12 N 0.20311(18) 0.5304(3) 0.38696(13) 0.0230(12) Uani 1 1 d . . . N13 N 0.21929(18) 0.7568(3) 0.34300(13) 0.0251(12) Uani 1 1 d . . . H13A H 0.2379 0.7112 0.3343 0.030 Uiso 1 1 calc R . . N14 N 0.08878(18) 0.6882(3) 0.39171(13) 0.0239(12) Uani 1 1 d . . . H14A H 0.0834 0.6357 0.4041 0.029 Uiso 1 1 calc R . . C1 C 0.1907(3) 0.4274(5) 0.27421(16) 0.0364(17) Uani 1 1 d . . . H1A H 0.1552 0.4259 0.2592 0.055 Uiso 1 1 calc R . . H1B H 0.2036 0.3594 0.2792 0.055 Uiso 1 1 calc R . . H1C H 0.2159 0.4633 0.2624 0.055 Uiso 1 1 calc R . . C2 C 0.1868(2) 0.4798(4) 0.30825(16) 0.0249(14) Uani 1 1 d . . . C3 C 0.2286(2) 0.4575(4) 0.33590(16) 0.0278(15) Uani 1 1 d . . . H3A H 0.2591 0.4282 0.3290 0.033 Uiso 1 1 calc R . . C4 C 0.2335(2) 0.4706(4) 0.37174(17) 0.0256(15) Uani 1 1 d . . . C5 C 0.2770(2) 0.4067(5) 0.39355(16) 0.0352(17) Uani 1 1 d . . . H5A H 0.2703 0.4024 0.4175 0.053 Uiso 1 1 calc R . . H5B H 0.3123 0.4368 0.3937 0.053 Uiso 1 1 calc R . . H5C H 0.2763 0.3400 0.3835 0.053 Uiso 1 1 calc R . . C6 C 0.0998(2) 0.5383(4) 0.28124(15) 0.0230(14) Uani 1 1 d . . . C7 C 0.0963(2) 0.6049(4) 0.25348(16) 0.0249(15) Uani 1 1 d . . . C8 C 0.0492(2) 0.6046(5) 0.22809(17) 0.0322(16) Uani 1 1 d . . . H8A H 0.0461 0.6497 0.2091 0.039 Uiso 1 1 calc R . . C9 C 0.0074(3) 0.5407(5) 0.22993(17) 0.0356(17) Uani 1 1 d . . . H9A H -0.0244 0.5424 0.2127 0.043 Uiso 1 1 calc R . . C10 C 0.0122(3) 0.4742(5) 0.25725(17) 0.0388(18) Uani 1 1 d . . . H10A H -0.0166 0.4297 0.2583 0.047 Uiso 1 1 calc R . . C11 C 0.0579(2) 0.4702(4) 0.28337(16) 0.0277(15) Uani 1 1 d . . . C12 C 0.1407(2) 0.6774(5) 0.24943(16) 0.0334(16) Uani 1 1 d . . . H12A H 0.1687 0.6739 0.2710 0.040 Uiso 1 1 calc R . . C13 C 0.1204(3) 0.7847(5) 0.24529(19) 0.048(2) Uani 1 1 d . . . H13B H 0.0977 0.7985 0.2625 0.072 Uiso 1 1 calc R . . H13C H 0.0994 0.7940 0.2218 0.072 Uiso 1 1 calc R . . H13D H 0.1511 0.8302 0.2488 0.072 Uiso 1 1 calc R . . C14 C 0.1673(3) 0.6503(6) 0.2185(2) 0.060(2) Uani 1 1 d . . . H14B H 0.1840 0.5846 0.2224 0.090 Uiso 1 1 calc R . . H14C H 0.1949 0.6997 0.2162 0.090 Uiso 1 1 calc R . . H14D H 0.1401 0.6492 0.1972 0.090 Uiso 1 1 calc R . . C15 C 0.0612(3) 0.3940(5) 0.31229(17) 0.0352(17) Uani 1 1 d . . . H15A H 0.0933 0.4104 0.3304 0.042 Uiso 1 1 calc R . . C16 C 0.0699(3) 0.2904(5) 0.2982(2) 0.060(2) Uani 1 1 d . . . H16A H 0.1005 0.2919 0.2859 0.089 Uiso 1 1 calc R . . H16B H 0.0375 0.2696 0.2820 0.089 Uiso 1 1 calc R . . H16C H 0.0774 0.2432 0.3176 0.089 Uiso 1 1 calc R . . C17 C 0.0122(3) 0.3943(5) 0.32974(19) 0.052(2) Uani 1 1 d . . . H17A H 0.0065 0.4614 0.3381 0.078 Uiso 1 1 calc R . . H17B H 0.0179 0.3481 0.3494 0.078 Uiso 1 1 calc R . . H17C H -0.0195 0.3737 0.3129 0.078 Uiso 1 1 calc R . . C18 C 0.2057(2) 0.5249(4) 0.42404(16) 0.0247(15) Uani 1 1 d . . . C19 C 0.1648(2) 0.4740(4) 0.43700(16) 0.0227(14) Uani 1 1 d . . . C20 C 0.1668(2) 0.4712(5) 0.47282(17) 0.0321(16) Uani 1 1 d . . . H20A H 0.1390 0.4380 0.4817 0.039 Uiso 1 1 calc R . . C21 C 0.2079(2) 0.5151(5) 0.49585(17) 0.0331(16) Uani 1 1 d . . . H21A H 0.2090 0.5107 0.5203 0.040 Uiso 1 1 calc R . . C22 C 0.2474(2) 0.5658(4) 0.48265(17) 0.0315(16) Uani 1 1 d . . . H22A H 0.2753 0.5973 0.4985 0.038 Uiso 1 1 calc R . . C23 C 0.2481(2) 0.5726(4) 0.44744(16) 0.0259(15) Uani 1 1 d . . . C24 C 0.1205(2) 0.4189(4) 0.41250(17) 0.0287(15) Uani 1 1 d . . . H24A H 0.1115 0.4592 0.3907 0.034 Uiso 1 1 calc R . . C25 C 0.0691(2) 0.4061(5) 0.42696(19) 0.046(2) Uani 1 1 d . . . H25A H 0.0587 0.4700 0.4357 0.069 Uiso 1 1 calc R . . H25B H 0.0751 0.3577 0.4460 0.069 Uiso 1 1 calc R . . H25C H 0.0404 0.3824 0.4085 0.069 Uiso 1 1 calc R . . C26 C 0.1409(3) 0.3181(4) 0.40236(18) 0.0416(19) Uani 1 1 d . . . H26A H 0.1741 0.3274 0.3931 0.062 Uiso 1 1 calc R . . H26B H 0.1136 0.2873 0.3845 0.062 Uiso 1 1 calc R . . H26C H 0.1481 0.2752 0.4229 0.062 Uiso 1 1 calc R . . C27 C 0.2933(2) 0.6268(5) 0.43525(18) 0.0371(17) Uani 1 1 d . . . H27A H 0.2901 0.6147 0.4097 0.044 Uiso 1 1 calc R . . C28 C 0.2917(3) 0.7381(5) 0.4409(2) 0.052(2) Uani 1 1 d . . . H28A H 0.2586 0.7653 0.4272 0.078 Uiso 1 1 calc R . . H28B H 0.3228 0.7691 0.4334 0.078 Uiso 1 1 calc R . . H28C H 0.2928 0.7519 0.4656 0.078 Uiso 1 1 calc R . . C29 C 0.3485(3) 0.5859(6) 0.4535(2) 0.062(2) Uani 1 1 d . . . H29A H 0.3476 0.5132 0.4531 0.092 Uiso 1 1 calc R . . H29B H 0.3561 0.6091 0.4777 0.092 Uiso 1 1 calc R . . H29C H 0.3766 0.6096 0.4413 0.092 Uiso 1 1 calc R . . C30 C 0.2508(2) 0.8427(4) 0.33937(15) 0.0212(13) Uani 1 1 d . . . C31 C 0.2319(2) 0.9376(4) 0.34710(15) 0.0201(14) Uani 1 1 d . . . C32 C 0.2654(2) 1.0193(4) 0.34594(16) 0.0258(15) Uani 1 1 d . . . H32A H 0.2529 1.0823 0.3520 0.031 Uiso 1 1 calc R . . C33 C 0.3157(2) 1.0150(4) 0.33654(15) 0.0247(14) Uani 1 1 d . . . C34 C 0.3323(2) 0.9220(4) 0.32765(15) 0.0241(14) Uani 1 1 d . . . H34A H 0.3661 0.9167 0.3204 0.029 Uiso 1 1 calc R . . C35 C 0.3021(2) 0.8357(4) 0.32867(15) 0.0246(14) Uani 1 1 d . . . C36 C 0.1773(2) 0.9542(4) 0.35779(18) 0.0290(16) Uani 1 1 d . . . C37 C 0.1758(3) 0.9051(5) 0.39286(17) 0.0371(18) Uani 1 1 d . . . H37A H 0.2013 0.9386 0.4111 0.056 Uiso 1 1 calc R . . H37B H 0.1857 0.8350 0.3919 0.056 Uiso 1 1 calc R . . H37C H 0.1394 0.9103 0.3981 0.056 Uiso 1 1 calc R . . C38 C 0.1322(2) 0.9157(5) 0.32897(18) 0.0378(18) Uani 1 1 d . . . H38A H 0.0979 0.9179 0.3372 0.057 Uiso 1 1 calc R . . H38B H 0.1400 0.8472 0.3231 0.057 Uiso 1 1 calc R . . H38C H 0.1299 0.9576 0.3083 0.057 Uiso 1 1 calc R . . C39 C 0.1646(3) 1.0644(4) 0.36274(19) 0.044(2) Uani 1 1 d . . . H39A H 0.1898 1.0912 0.3826 0.066 Uiso 1 1 calc R . . H39B H 0.1278 1.0707 0.3671 0.066 Uiso 1 1 calc R . . H39C H 0.1679 1.1014 0.3417 0.066 Uiso 1 1 calc R . . C40 C 0.3506(3) 1.1088(5) 0.3379(2) 0.0383(18) Uani 1 1 d . . . C41 C 0.3673(3) 1.1417(5) 0.3758(2) 0.059(2) Uani 1 1 d . . . H41A H 0.3890 1.2022 0.3768 0.089 Uiso 1 1 calc R . . H41B H 0.3885 1.0891 0.3892 0.089 Uiso 1 1 calc R . . H41C H 0.3351 1.1549 0.3858 0.089 Uiso 1 1 calc R . . C42 C 0.3188(3) 1.1924(5) 0.3170(2) 0.054(2) Uani 1 1 d . . . H42A H 0.3412 1.2521 0.3183 0.081 Uiso 1 1 calc R . . H42B H 0.2864 1.2067 0.3267 0.081 Uiso 1 1 calc R . . H42C H 0.3084 1.1719 0.2926 0.081 Uiso 1 1 calc R . . C43 C 0.4015(3) 1.0912(5) 0.3227(2) 0.054(2) Uani 1 1 d . . . H43A H 0.4228 1.1524 0.3244 0.081 Uiso 1 1 calc R . . H43B H 0.3915 1.0718 0.2982 0.081 Uiso 1 1 calc R . . H43C H 0.4229 1.0383 0.3358 0.081 Uiso 1 1 calc R . . C44 C 0.3250(2) 0.7362(4) 0.31735(16) 0.0265(15) Uani 1 1 d . . . C45 C 0.2880(2) 0.6881(5) 0.28679(18) 0.0428(19) Uani 1 1 d . . . H45A H 0.2544 0.6681 0.2940 0.064 Uiso 1 1 calc R . . H45B H 0.3057 0.6296 0.2791 0.064 Uiso 1 1 calc R . . H45C H 0.2801 0.7357 0.2676 0.064 Uiso 1 1 calc R . . C46 C 0.3378(2) 0.6648(5) 0.34865(18) 0.0398(18) Uani 1 1 d . . . H46A H 0.3048 0.6512 0.3577 0.060 Uiso 1 1 calc R . . H46B H 0.3644 0.6953 0.3670 0.060 Uiso 1 1 calc R . . H46C H 0.3521 0.6025 0.3412 0.060 Uiso 1 1 calc R . . C47 C 0.3801(2) 0.7509(5) 0.30489(17) 0.0341(17) Uani 1 1 d . . . H47A H 0.3752 0.7964 0.2850 0.051 Uiso 1 1 calc R . . H47B H 0.3930 0.6867 0.2980 0.051 Uiso 1 1 calc R . . H47C H 0.4065 0.7788 0.3240 0.051 Uiso 1 1 calc R . . C48 C 0.0572(2) 0.7695(4) 0.39726(15) 0.0198(14) Uani 1 1 d . . . C49 C 0.0623(2) 0.8213(4) 0.42935(15) 0.0233(14) Uani 1 1 d . . . C50 C 0.0395(2) 0.9157(4) 0.42995(17) 0.0287(15) Uani 1 1 d . . . H50A H 0.0442 0.9504 0.4515 0.034 Uiso 1 1 calc R . . C51 C 0.0105(3) 0.9610(4) 0.40085(17) 0.0292(16) Uani 1 1 d . A . C52 C -0.0014(2) 0.9030(4) 0.37093(16) 0.0279(16) Uani 1 1 d . . . H52A H -0.0245 0.9297 0.3511 0.033 Uiso 1 1 calc R . . C53 C 0.0190(2) 0.8074(4) 0.36874(15) 0.0197(14) Uani 1 1 d . . . C54 C 0.0912(2) 0.7762(5) 0.46431(16) 0.0304(16) Uani 1 1 d . . . C55 C 0.0858(3) 0.8417(5) 0.49569(17) 0.053(2) Uani 1 1 d . . . H55A H 0.1008 0.8067 0.5173 0.079 Uiso 1 1 calc R . . H55B H 0.0478 0.8563 0.4953 0.079 Uiso 1 1 calc R . . H55C H 0.1055 0.9039 0.4945 0.079 Uiso 1 1 calc R . . C56 C 0.0650(3) 0.6760(5) 0.47051(17) 0.0383(18) Uani 1 1 d . . . H56A H 0.0855 0.6444 0.4914 0.058 Uiso 1 1 calc R . . H56B H 0.0649 0.6327 0.4503 0.058 Uiso 1 1 calc R . . H56C H 0.0279 0.6873 0.4738 0.058 Uiso 1 1 calc R . . C57 C 0.1526(2) 0.7630(5) 0.46588(17) 0.0340(17) Uani 1 1 d . . . H57A H 0.1695 0.7412 0.4893 0.051 Uiso 1 1 calc R . . H57B H 0.1684 0.8265 0.4606 0.051 Uiso 1 1 calc R . . H57C H 0.1588 0.7132 0.4488 0.051 Uiso 1 1 calc R . . C58 C -0.0113(3) 1.0672(4) 0.40163(17) 0.0315(16) Uani 1 1 d . . . C59 C 0.0068(4) 1.1302(5) 0.3747(2) 0.084(3) Uani 1 1 d . A . H59A H -0.0068 1.1025 0.3515 0.126 Uiso 1 1 calc R . . H59B H 0.0462 1.1317 0.3787 0.126 Uiso 1 1 calc R . . H59C H -0.0070 1.1977 0.3760 0.126 Uiso 1 1 calc R . . C60 C -0.0744(5) 1.0679(10) 0.3806(4) 0.041(4) Uiso 0.50 1 d P A 1 H60A H -0.0764 1.0367 0.3578 0.061 Uiso 0.50 1 calc PR A 1 H60B H -0.0873 1.1365 0.3776 0.061 Uiso 0.50 1 calc PR A 1 H60C H -0.0969 1.0309 0.3941 0.061 Uiso 0.50 1 calc PR A 1 C61 C -0.0123(7) 1.1059(12) 0.4361(4) 0.060(5) Uiso 0.50 1 d P A 1 H61A H -0.0342 1.0625 0.4480 0.090 Uiso 0.50 1 calc PR A 1 H61B H -0.0277 1.1728 0.4341 0.090 Uiso 0.50 1 calc PR A 1 H61C H 0.0245 1.1086 0.4494 0.090 Uiso 0.50 1 calc PR A 1 C60A C 0.0251(6) 1.1288(11) 0.4346(4) 0.057(5) Uiso 0.50 1 d P A 2 H60D H 0.0625 1.1321 0.4313 0.086 Uiso 0.50 1 calc PR A 2 H60E H 0.0233 1.0944 0.4564 0.086 Uiso 0.50 1 calc PR A 2 H60F H 0.0108 1.1962 0.4354 0.086 Uiso 0.50 1 calc PR A 2 C61A C -0.0645(7) 1.0679(12) 0.4098(5) 0.068(5) Uiso 0.50 1 d P A 2 H61D H -0.0859 1.0148 0.3969 0.102 Uiso 0.50 1 calc PR A 2 H61E H -0.0816 1.1321 0.4033 0.102 Uiso 0.50 1 calc PR A 2 H61F H -0.0622 1.0572 0.4349 0.102 Uiso 0.50 1 calc PR A 2 C62 C -0.0055(2) 0.7407(4) 0.33801(16) 0.0226(14) Uani 1 1 d . . . C63 C -0.0373(2) 0.6570(5) 0.35215(18) 0.0372(17) Uani 1 1 d . . . H63A H -0.0677 0.6857 0.3611 0.056 Uiso 1 1 calc R . . H63B H -0.0137 0.6219 0.3709 0.056 Uiso 1 1 calc R . . H63C H -0.0508 0.6103 0.3333 0.056 Uiso 1 1 calc R . . C64 C -0.0452(3) 0.7978(5) 0.31006(17) 0.0399(18) Uani 1 1 d . . . H64A H -0.0265 0.8531 0.3011 0.060 Uiso 1 1 calc R . . H64B H -0.0749 0.8237 0.3205 0.060 Uiso 1 1 calc R . . H64C H -0.0595 0.7528 0.2909 0.060 Uiso 1 1 calc R . . C65 C 0.0353(2) 0.6925(5) 0.31798(16) 0.0307(16) Uani 1 1 d . . . H65A H 0.0614 0.7425 0.3136 0.046 Uiso 1 1 calc R . . H65B H 0.0162 0.6661 0.2958 0.046 Uiso 1 1 calc R . . H65C H 0.0541 0.6384 0.3319 0.046 Uiso 1 1 calc R . . Sm2 Sm 0.340284(11) 0.34837(2) 0.099268(8) 0.02018(9) Uani 1 1 d . . . N21 N 0.3224(2) 0.4748(4) 0.05419(15) 0.0432(16) Uani 1 1 d . B . N22 N 0.29539(18) 0.4702(3) 0.12640(14) 0.0270(13) Uani 1 1 d . B . N23 N 0.26757(18) 0.2543(3) 0.07936(13) 0.0286(13) Uani 1 1 d . . . H23A H 0.2493 0.2915 0.0628 0.034 Uiso 1 1 calc R . . N24 N 0.41983(17) 0.3284(3) 0.13958(12) 0.0195(11) Uani 1 1 d . . . H24B H 0.4284 0.3802 0.1532 0.023 Uiso 1 1 calc R . . C101 C 0.2234(3) 0.5890(6) 0.1325(2) 0.074(3) Uani 1 1 d . B . H10F H 0.2073 0.5426 0.1470 0.111 Uiso 1 1 calc R . . H10G H 0.1949 0.6248 0.1170 0.111 Uiso 1 1 calc R . . H10H H 0.2461 0.6366 0.1476 0.111 Uiso 1 1 calc R . . C102 C 0.2786(3) 0.5327(6) 0.0501(2) 0.057(2) Uani 1 1 d . . . C103 C 0.2478(3) 0.5502(5) 0.0758(2) 0.049(2) Uani 1 1 d . B . H10B H 0.2139 0.5801 0.0673 0.059 Uiso 1 1 calc R . . C104 C 0.2573(3) 0.5322(5) 0.1110(2) 0.0395(18) Uani 1 1 d . . . C105 C 0.2653(6) 0.6085(11) 0.0215(4) 0.045(4) Uiso 0.50 1 d P B 1 H10C H 0.2632 0.6745 0.0318 0.067 Uiso 0.50 1 calc PR B 1 H10D H 0.2306 0.5921 0.0070 0.067 Uiso 0.50 1 calc PR B 1 H10E H 0.2933 0.6082 0.0072 0.067 Uiso 0.50 1 calc PR B 1 C05A C 0.2548(6) 0.5653(10) 0.0099(4) 0.037(4) Uiso 0.50 1 d P B 2 H05A H 0.2315 0.5125 -0.0017 0.055 Uiso 0.50 1 calc PR B 2 H05B H 0.2847 0.5761 -0.0025 0.055 Uiso 0.50 1 calc PR B 2 H05C H 0.2340 0.6267 0.0098 0.055 Uiso 0.50 1 calc PR B 2 C106 C 0.3563(3) 0.4842(6) 0.0279(2) 0.055(2) Uani 1 1 d . . . C107 C 0.3488(3) 0.4201(8) -0.0012(2) 0.072(3) Uani 1 1 d . B . C108 C 0.3849(6) 0.4542(12) -0.0229(4) 0.038(4) Uiso 0.50 1 d P B 1 H10I H 0.3788 0.4298 -0.0461 0.046 Uiso 0.50 1 calc PR B 1 C109 C 0.4282(7) 0.5191(14) -0.0137(5) 0.045(5) Uiso 0.50 1 d P B 1 H10K H 0.4538 0.5253 -0.0286 0.054 Uiso 0.50 1 calc PR B 1 C110 C 0.4332(4) 0.5621(7) 0.0097(3) 0.089(4) Uani 0.50 1 d P B 1 C08A C 0.3839(6) 0.4060(13) -0.0273(4) 0.050(5) Uiso 0.50 1 d P B 2 H08A H 0.3813 0.3529 -0.0435 0.060 Uiso 0.50 1 calc PR B 2 C09A C 0.4217(7) 0.4830(13) -0.0244(5) 0.050(5) Uiso 0.50 1 d P B 2 H09A H 0.4419 0.4910 -0.0425 0.059 Uiso 0.50 1 calc PR B 2 C10A C 0.4332(4) 0.5621(7) 0.0097(3) 0.089(4) Uani 0.50 1 d P B 2 H10J H 0.4615 0.6094 0.0125 0.106 Uiso 0.50 1 calc PR B 2 C111 C 0.3981(3) 0.5537(6) 0.0339(3) 0.066(3) Uani 1 1 d . B . C112 C 0.3036(6) 0.3689(13) -0.0088(4) 0.046(4) Uiso 0.50 1 d P B 1 H11A H 0.2853 0.3690 0.0118 0.055 Uiso 0.50 1 calc PR B 1 C113 C 0.2639(7) 0.4064(14) -0.0408(5) 0.070(6) Uiso 0.50 1 d P B 1 H11B H 0.2530 0.4744 -0.0366 0.106 Uiso 0.50 1 calc PR B 1 H11C H 0.2322 0.3633 -0.0450 0.106 Uiso 0.50 1 calc PR B 1 H11D H 0.2814 0.4053 -0.0613 0.106 Uiso 0.50 1 calc PR B 1 C114 C 0.3209(7) 0.2644(15) -0.0153(5) 0.055(5) Uiso 0.50 1 d P B 1 H11E H 0.3473 0.2417 0.0047 0.083 Uiso 0.50 1 calc PR B 1 H11F H 0.3371 0.2632 -0.0363 0.083 Uiso 0.50 1 calc PR B 1 H11G H 0.2895 0.2203 -0.0186 0.083 Uiso 0.50 1 calc PR B 1 C115 C 0.4153(6) 0.6176(11) 0.0748(4) 0.041(4) Uiso 0.50 1 d P B 1 H11H H 0.4063 0.5744 0.0938 0.050 Uiso 0.50 1 calc PR B 1 C116 C 0.4666(4) 0.6373(7) 0.0811(3) 0.101(4) Uani 0.50 1 d P B 1 H11I H 0.4778 0.6541 0.1058 0.151 Uiso 0.50 1 calc PR B 1 H11J H 0.4738 0.6935 0.0667 0.151 Uiso 0.50 1 calc PR B 1 H11K H 0.4866 0.5790 0.0755 0.151 Uiso 0.50 1 calc PR B 1 C117 C 0.3816(6) 0.7129(12) 0.0726(5) 0.064(5) Uiso 0.50 1 d P B 1 H11L H 0.3883 0.7466 0.0952 0.095 Uiso 0.50 1 calc PR B 1 H11M H 0.3434 0.6961 0.0663 0.095 Uiso 0.50 1 calc PR B 1 H11N H 0.3917 0.7569 0.0548 0.095 Uiso 0.50 1 calc PR B 1 C12A C 0.3078(6) 0.3157(13) -0.0088(4) 0.033(4) Uiso 0.50 1 d P B 2 H12B H 0.2905 0.3098 0.0122 0.040 Uiso 0.50 1 calc PR B 2 C13A C 0.2617(7) 0.3380(13) -0.0389(4) 0.062(5) Uiso 0.50 1 d P B 2 H13E H 0.2365 0.2821 -0.0421 0.093 Uiso 0.50 1 calc PR B 2 H13F H 0.2761 0.3482 -0.0603 0.093 Uiso 0.50 1 calc PR B 2 H13G H 0.2429 0.3982 -0.0336 0.093 Uiso 0.50 1 calc PR B 2 C14A C 0.3314(7) 0.2148(14) -0.0130(5) 0.067(6) Uiso 0.50 1 d P B 2 H14E H 0.3071 0.1634 -0.0073 0.101 Uiso 0.50 1 calc PR B 2 H14F H 0.3663 0.2090 0.0025 0.101 Uiso 0.50 1 calc PR B 2 H14G H 0.3362 0.2063 -0.0372 0.101 Uiso 0.50 1 calc PR B 2 C15A C 0.3993(6) 0.6207(11) 0.0567(5) 0.043(4) Uiso 0.50 1 d P B 2 H15B H 0.3761 0.5983 0.0734 0.051 Uiso 0.50 1 calc PR B 2 C16A C 0.4666(4) 0.6373(7) 0.0811(3) 0.101(4) Uani 0.50 1 d P B 2 H16D H 0.4815 0.5726 0.0893 0.151 Uiso 0.50 1 calc PR B 2 H16E H 0.4654 0.6805 0.1011 0.151 Uiso 0.50 1 calc PR B 2 H16F H 0.4892 0.6677 0.0661 0.151 Uiso 0.50 1 calc PR B 2 C17A C 0.3788(8) 0.7250(14) 0.0427(5) 0.093(7) Uiso 0.50 1 d P B 2 H17D H 0.3394 0.7242 0.0366 0.139 Uiso 0.50 1 calc PR B 2 H17E H 0.3940 0.7412 0.0220 0.139 Uiso 0.50 1 calc PR B 2 H17F H 0.3900 0.7751 0.0608 0.139 Uiso 0.50 1 calc PR B 2 C118 C 0.3060(2) 0.4668(5) 0.16434(19) 0.0357(18) Uani 1 1 d . . . C119 C 0.3455(3) 0.5287(5) 0.1831(2) 0.055(2) Uani 1 1 d . B . C120 C 0.3552(4) 0.5234(7) 0.2198(3) 0.072(3) Uani 1 1 d . . . H12C H 0.3807 0.5666 0.2330 0.086 Uiso 1 1 calc R B . C121 C 0.3279(4) 0.4564(8) 0.2364(3) 0.079(3) Uani 1 1 d . B . H12D H 0.3356 0.4516 0.2610 0.095 Uiso 1 1 calc R . . C122 C 0.2903(3) 0.3975(7) 0.2180(2) 0.061(2) Uani 1 1 d . . . H12E H 0.2712 0.3532 0.2302 0.073 Uiso 1 1 calc R B . C123 C 0.2781(3) 0.3985(6) 0.18173(19) 0.0413(19) Uani 1 1 d . B . C124 C 0.3740(3) 0.6041(6) 0.1644(3) 0.081(3) Uani 0.50 1 d P B 1 H124 H 0.3591 0.6038 0.1389 0.097 Uiso 0.50 1 calc PR B 1 C24A C 0.3740(3) 0.6041(6) 0.1644(3) 0.081(3) Uani 0.50 1 d P B 2 H24C H 0.3679 0.5680 0.1417 0.097 Uiso 0.50 1 calc PR B 2 C125 C 0.4351(3) 0.5945(6) 0.1709(2) 0.075(3) Uani 1 1 d . . . H12F H 0.4452 0.5362 0.1585 0.112 Uiso 1 1 calc R B 1 H12G H 0.4486 0.5870 0.1959 0.112 Uiso 1 1 calc R B 1 H12H H 0.4507 0.6542 0.1624 0.112 Uiso 1 1 calc R B 1 C126 C 0.3614(5) 0.7118(9) 0.1822(4) 0.034(3) Uiso 0.50 1 d P B 1 H12I H 0.3734 0.7086 0.2074 0.051 Uiso 0.50 1 calc PR B 1 H12J H 0.3227 0.7251 0.1769 0.051 Uiso 0.50 1 calc PR B 1 H12K H 0.3806 0.7651 0.1725 0.051 Uiso 0.50 1 calc PR B 1 C26A C 0.3592(14) 0.700(3) 0.1496(9) 0.220(16) Uiso 0.50 1 d P B 2 H26D H 0.3704 0.7054 0.1269 0.331 Uiso 0.50 1 calc PR B 2 H26E H 0.3769 0.7519 0.1651 0.331 Uiso 0.50 1 calc PR B 2 H26F H 0.3201 0.7083 0.1465 0.331 Uiso 0.50 1 calc PR B 2 C127 C 0.2349(2) 0.3299(6) 0.16388(19) 0.047(2) Uani 1 1 d . . . H12L H 0.2327 0.3394 0.1383 0.056 Uiso 1 1 calc R B . C128 C 0.2475(4) 0.2214(7) 0.1714(3) 0.093(3) Uani 1 1 d . B . H12M H 0.2828 0.2057 0.1657 0.140 Uiso 1 1 calc R . . H12N H 0.2200 0.1802 0.1572 0.140 Uiso 1 1 calc R . . H12O H 0.2481 0.2079 0.1961 0.140 Uiso 1 1 calc R . . C129 C 0.1798(3) 0.3551(8) 0.1718(2) 0.103(4) Uani 1 1 d . B . H12P H 0.1715 0.4248 0.1660 0.154 Uiso 1 1 calc R . . H12Q H 0.1798 0.3442 0.1966 0.154 Uiso 1 1 calc R . . H12R H 0.1527 0.3125 0.1579 0.154 Uiso 1 1 calc R . . C130 C 0.2345(2) 0.1684(4) 0.07851(16) 0.0275(15) Uani 1 1 d . . . C131 C 0.1775(2) 0.1724(4) 0.06799(16) 0.0263(15) Uani 1 1 d . . . C132 C 0.1476(2) 0.0896(5) 0.07365(16) 0.0314(16) Uani 1 1 d . . . H13H H 0.1096 0.0936 0.0673 0.038 Uiso 1 1 calc R . . C133 C 0.1696(2) 0.0022(5) 0.08788(17) 0.0322(16) Uani 1 1 d . . . C134 C 0.2257(2) -0.0032(5) 0.09477(16) 0.0305(16) Uani 1 1 d . . . H13I H 0.2421 -0.0636 0.1036 0.037 Uiso 1 1 calc R . . C135 C 0.2584(2) 0.0752(4) 0.08935(16) 0.0255(15) Uani 1 1 d . . . C136 C 0.1472(2) 0.2633(5) 0.04991(18) 0.0376(18) Uani 1 1 d . . . C137 C 0.1699(3) 0.2950(5) 0.01756(19) 0.047(2) Uani 1 1 d . . . H13J H 0.2077 0.3136 0.0245 0.071 Uiso 1 1 calc R . . H13K H 0.1494 0.3519 0.0065 0.071 Uiso 1 1 calc R . . H13L H 0.1668 0.2397 0.0010 0.071 Uiso 1 1 calc R . . C138 C 0.1469(3) 0.3517(5) 0.0748(2) 0.054(2) Uani 1 1 d . . . H13M H 0.1839 0.3709 0.0845 0.081 Uiso 1 1 calc R . . H13N H 0.1283 0.3327 0.0937 0.081 Uiso 1 1 calc R . . H13O H 0.1281 0.4078 0.0620 0.081 Uiso 1 1 calc R . . C139 C 0.0872(2) 0.2415(5) 0.03607(19) 0.050(2) Uani 1 1 d . . . H13P H 0.0692 0.2259 0.0556 0.075 Uiso 1 1 calc R . . H13Q H 0.0840 0.1849 0.0201 0.075 Uiso 1 1 calc R . . H13R H 0.0703 0.2999 0.0237 0.075 Uiso 1 1 calc R . . C140 C 0.1366(3) -0.0889(5) 0.09536(19) 0.0426(19) Uani 1 1 d . . . C141 C 0.1449(4) -0.1089(8) 0.1341(2) 0.114(4) Uani 1 1 d . . . H14H H 0.1830 -0.1225 0.1430 0.171 Uiso 1 1 calc R . . H14I H 0.1234 -0.1664 0.1385 0.171 Uiso 1 1 calc R . . H14J H 0.1337 -0.0507 0.1461 0.171 Uiso 1 1 calc R . . C142 C 0.0769(3) -0.0737(6) 0.0817(3) 0.085(3) Uani 1 1 d . . . H14K H 0.0647 -0.0136 0.0921 0.127 Uiso 1 1 calc R . . H14L H 0.0568 -0.1311 0.0879 0.127 Uiso 1 1 calc R . . H14M H 0.0708 -0.0666 0.0563 0.127 Uiso 1 1 calc R . . C143 C 0.1544(3) -0.1788(5) 0.0761(2) 0.056(2) Uani 1 1 d . . . H14N H 0.1918 -0.1952 0.0860 0.084 Uiso 1 1 calc R . . H14O H 0.1514 -0.1629 0.0514 0.084 Uiso 1 1 calc R . . H14P H 0.1313 -0.2357 0.0787 0.084 Uiso 1 1 calc R . . C144 C 0.3202(3) 0.0552(5) 0.0945(2) 0.044(2) Uani 1 1 d . . . C145 C 0.3491(3) 0.1037(6) 0.1281(2) 0.073(3) Uani 1 1 d . . . H14Q H 0.3880 0.0953 0.1300 0.110 Uiso 1 1 calc R . . H14R H 0.3375 0.0723 0.1481 0.110 Uiso 1 1 calc R . . H14S H 0.3404 0.1746 0.1277 0.110 Uiso 1 1 calc R . . C146 C 0.3332(3) -0.0564(5) 0.0972(3) 0.081(3) Uani 1 1 d . . . H14T H 0.3712 -0.0666 0.0961 0.122 Uiso 1 1 calc R . . H14U H 0.3107 -0.0916 0.0779 0.122 Uiso 1 1 calc R . . H14V H 0.3259 -0.0820 0.1194 0.122 Uiso 1 1 calc R . . C147 C 0.3426(3) 0.0925(5) 0.0631(2) 0.056(2) Uani 1 1 d . . . H14W H 0.3820 0.0917 0.0686 0.085 Uiso 1 1 calc R . . H14X H 0.3301 0.1605 0.0576 0.085 Uiso 1 1 calc R . . H14Y H 0.3301 0.0494 0.0431 0.085 Uiso 1 1 calc R . . C148 C 0.4562(2) 0.2506(4) 0.14627(15) 0.0189(14) Uani 1 1 d . . . C149 C 0.4676(2) 0.1982(4) 0.17902(15) 0.0204(14) Uani 1 1 d . . . C150 C 0.4906(2) 0.1049(4) 0.17958(16) 0.0245(15) Uani 1 1 d . . . H15C H 0.4955 0.0689 0.2008 0.029 Uiso 1 1 calc R . . C151 C 0.5070(2) 0.0602(4) 0.15124(17) 0.0281(16) Uani 1 1 d . C . C152 C 0.5052(2) 0.1202(4) 0.12226(16) 0.0260(15) Uani 1 1 d . . . H15D H 0.5198 0.0954 0.1032 0.031 Uiso 1 1 calc R . . C153 C 0.4829(2) 0.2152(4) 0.11964(15) 0.0182(13) Uani 1 1 d . . . C154 C 0.4558(2) 0.2424(5) 0.21337(16) 0.0336(17) Uani 1 1 d . . . C155 C 0.3947(2) 0.2428(6) 0.21383(18) 0.050(2) Uani 1 1 d . . . H15E H 0.3807 0.1751 0.2105 0.075 Uiso 1 1 calc R . . H15F H 0.3763 0.2853 0.1950 0.075 Uiso 1 1 calc R . . H15G H 0.3886 0.2684 0.2363 0.075 Uiso 1 1 calc R . . C156 C 0.4790(3) 0.3473(5) 0.21859(18) 0.048(2) Uani 1 1 d . . . H15H H 0.5182 0.3446 0.2203 0.072 Uiso 1 1 calc R . . H15I H 0.4705 0.3756 0.2401 0.072 Uiso 1 1 calc R . . H15J H 0.4634 0.3890 0.1988 0.072 Uiso 1 1 calc R . . C157 C 0.4827(3) 0.1829(6) 0.24515(17) 0.057(2) Uani 1 1 d . . . H15K H 0.5212 0.1761 0.2447 0.086 Uiso 1 1 calc R . . H15L H 0.4663 0.1170 0.2446 0.086 Uiso 1 1 calc R . . H15M H 0.4780 0.2176 0.2664 0.086 Uiso 1 1 calc R . . C158 C 0.5271(3) -0.0474(4) 0.15347(19) 0.0398(19) Uani 1 1 d . . . C159 C 0.5348(7) -0.0889(12) 0.1215(4) 0.049(4) Uiso 0.50 1 d P C 1 H15N H 0.5625 -0.0512 0.1125 0.073 Uiso 0.50 1 calc PR C 1 H15O H 0.5010 -0.0860 0.1046 0.073 Uiso 0.50 1 calc PR C 1 H15P H 0.5462 -0.1582 0.1251 0.073 Uiso 0.50 1 calc PR C 1 C160 C 0.4783(5) -0.1127(10) 0.1678(4) 0.036(4) Uiso 0.50 1 d P C 1 H16G H 0.4755 -0.0906 0.1913 0.054 Uiso 0.50 1 calc PR C 1 H16H H 0.4872 -0.1835 0.1682 0.054 Uiso 0.50 1 calc PR C 1 H16I H 0.4439 -0.1017 0.1521 0.054 Uiso 0.50 1 calc PR C 1 C59A C 0.5618(7) -0.0664(12) 0.1210(4) 0.049(4) Uiso 0.50 1 d P C 2 H59D H 0.5916 -0.0191 0.1232 0.073 Uiso 0.50 1 calc PR C 2 H59E H 0.5379 -0.0569 0.0985 0.073 Uiso 0.50 1 calc PR C 2 H59F H 0.5760 -0.1343 0.1224 0.073 Uiso 0.50 1 calc PR C 2 C60B C 0.4841(7) -0.1143(13) 0.1487(5) 0.068(6) Uiso 0.50 1 d P C 2 H60G H 0.4656 -0.1122 0.1244 0.102 Uiso 0.50 1 calc PR C 2 H60H H 0.4590 -0.0962 0.1640 0.102 Uiso 0.50 1 calc PR C 2 H60I H 0.4977 -0.1816 0.1544 0.102 Uiso 0.50 1 calc PR C 2 C161 C 0.5721(3) -0.0612(5) 0.18481(19) 0.053(2) Uani 1 1 d . C . H16J H 0.6025 -0.0183 0.1823 0.079 Uiso 1 1 calc R . . H16K H 0.5838 -0.1306 0.1861 0.079 Uiso 1 1 calc R . . H16L H 0.5590 -0.0434 0.2061 0.079 Uiso 1 1 calc R . . C162 C 0.4930(2) 0.2854(4) 0.08962(15) 0.0243(14) Uani 1 1 d . . . C163 C 0.4416(2) 0.3221(5) 0.06637(16) 0.0315(16) Uani 1 1 d . . . H16M H 0.4265 0.3772 0.0778 0.047 Uiso 1 1 calc R . . H16N H 0.4154 0.2678 0.0622 0.047 Uiso 1 1 calc R . . H16O H 0.4499 0.3447 0.0441 0.047 Uiso 1 1 calc R . . C164 C 0.5271(3) 0.2341(5) 0.06557(18) 0.048(2) Uani 1 1 d . . . H16P H 0.5075 0.1764 0.0544 0.071 Uiso 1 1 calc R . . H16Q H 0.5613 0.2123 0.0794 0.071 Uiso 1 1 calc R . . H16R H 0.5339 0.2810 0.0477 0.071 Uiso 1 1 calc R . . C165 C 0.5250(2) 0.3754(4) 0.10594(17) 0.0341(17) Uani 1 1 d . . . H16S H 0.5071 0.4042 0.1239 0.051 Uiso 1 1 calc R . . H16T H 0.5269 0.4251 0.0879 0.051 Uiso 1 1 calc R . . H16U H 0.5614 0.3545 0.1165 0.051 Uiso 1 1 calc R . . C201 C 0.3201(7) -0.0650(12) 0.2147(4) 0.167(6) Uiso 1 1 d . . . C202 C 0.2835(9) -0.0232(14) 0.2257(5) 0.206(8) Uiso 1 1 d . . . C203 C 0.2305(6) -0.0028(10) 0.2263(3) 0.126(5) Uiso 1 1 d . . . C204 C 0.2018(8) 0.0493(13) 0.2434(5) 0.191(7) Uiso 1 1 d . . . C205 C 0.1483(6) 0.0839(11) 0.2400(4) 0.154(5) Uiso 1 1 d . . . C206 C 0.4647(6) 0.3457(10) 0.4710(4) 0.155(6) Uiso 1 1 d . . . C207 C 0.5055(8) 0.4223(13) 0.4783(4) 0.176(6) Uiso 1 1 d . . . C208 C 0.5331(7) 0.5199(18) 0.4971(6) 0.250(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01450(16) 0.01578(16) 0.02453(19) -0.00164(15) 0.00484(13) -0.00036(14) N11 0.020(3) 0.019(3) 0.023(3) 0.002(2) 0.003(2) 0.006(2) N12 0.023(3) 0.022(3) 0.025(3) -0.001(2) 0.007(2) -0.001(2) N13 0.027(3) 0.015(3) 0.036(3) -0.004(2) 0.014(3) 0.000(2) N14 0.023(3) 0.012(3) 0.038(3) 0.000(2) 0.010(2) 0.002(2) C1 0.036(4) 0.043(4) 0.031(4) -0.005(3) 0.008(3) 0.016(3) C2 0.027(3) 0.025(3) 0.025(4) -0.002(3) 0.009(3) -0.003(3) C3 0.026(4) 0.027(4) 0.033(4) 0.003(3) 0.014(3) 0.010(3) C4 0.021(3) 0.024(3) 0.033(4) 0.006(3) 0.005(3) 0.006(3) C5 0.033(4) 0.037(4) 0.035(4) -0.001(3) 0.003(3) 0.013(3) C6 0.030(4) 0.021(3) 0.018(4) -0.007(3) 0.004(3) 0.000(3) C7 0.023(3) 0.024(3) 0.028(4) -0.003(3) 0.004(3) 0.003(3) C8 0.034(4) 0.033(4) 0.027(4) -0.004(3) -0.002(3) 0.001(3) C9 0.037(4) 0.034(4) 0.031(4) -0.003(3) -0.007(3) -0.006(3) C10 0.038(4) 0.041(4) 0.034(4) -0.005(4) -0.002(4) -0.019(3) C11 0.037(4) 0.022(3) 0.025(4) -0.001(3) 0.007(3) -0.008(3) C12 0.031(4) 0.043(4) 0.024(4) 0.009(3) 0.000(3) -0.007(3) C13 0.064(5) 0.033(4) 0.045(5) 0.001(4) 0.004(4) -0.015(4) C14 0.060(5) 0.068(6) 0.061(6) 0.004(5) 0.035(5) -0.004(5) C15 0.039(4) 0.032(4) 0.032(4) 0.002(3) 0.001(3) -0.015(3) C16 0.081(6) 0.027(4) 0.075(6) 0.016(4) 0.029(5) 0.006(4) C17 0.066(6) 0.045(5) 0.047(5) 0.004(4) 0.016(4) -0.008(4) C18 0.023(3) 0.020(3) 0.030(4) 0.004(3) 0.002(3) 0.009(3) C19 0.019(3) 0.022(3) 0.026(4) 0.006(3) 0.000(3) 0.010(3) C20 0.026(4) 0.035(4) 0.034(4) 0.014(3) 0.004(3) 0.001(3) C21 0.035(4) 0.040(4) 0.022(4) 0.004(3) 0.001(3) 0.008(3) C22 0.024(4) 0.036(4) 0.032(4) -0.001(3) -0.005(3) 0.005(3) C23 0.023(3) 0.026(3) 0.028(4) 0.000(3) 0.001(3) -0.004(3) C24 0.022(3) 0.029(4) 0.033(4) 0.000(3) 0.000(3) -0.004(3) C25 0.030(4) 0.055(5) 0.058(5) -0.011(4) 0.017(4) -0.022(4) C26 0.047(4) 0.026(4) 0.052(5) -0.005(3) 0.011(4) -0.005(3) C27 0.023(4) 0.047(4) 0.039(4) -0.002(3) 0.001(3) -0.008(3) C28 0.042(5) 0.044(5) 0.071(6) 0.007(4) 0.013(4) -0.009(4) C29 0.027(4) 0.081(6) 0.077(7) 0.003(5) 0.008(4) -0.004(4) C30 0.016(3) 0.018(3) 0.030(4) -0.001(3) 0.005(3) -0.006(3) C31 0.019(3) 0.021(3) 0.021(4) 0.001(3) 0.005(3) -0.005(3) C32 0.029(4) 0.016(3) 0.033(4) 0.002(3) 0.009(3) 0.003(3) C33 0.021(3) 0.025(3) 0.028(4) 0.003(3) 0.005(3) -0.002(3) C34 0.017(3) 0.027(4) 0.029(4) 0.003(3) 0.008(3) -0.003(3) C35 0.019(3) 0.025(3) 0.030(4) 0.002(3) 0.003(3) 0.000(3) C36 0.012(3) 0.025(4) 0.052(5) -0.006(3) 0.013(3) 0.000(3) C37 0.040(4) 0.036(4) 0.043(5) -0.010(3) 0.028(4) -0.012(3) C38 0.013(3) 0.038(4) 0.062(5) 0.004(4) 0.007(3) -0.001(3) C39 0.032(4) 0.025(4) 0.081(6) -0.007(4) 0.026(4) 0.004(3) C40 0.035(4) 0.024(4) 0.061(5) 0.002(4) 0.021(4) -0.010(3) C41 0.057(5) 0.045(5) 0.076(6) -0.022(4) 0.012(5) -0.028(4) C42 0.048(5) 0.030(4) 0.088(7) 0.012(4) 0.022(5) -0.010(4) C43 0.033(4) 0.040(4) 0.096(7) 0.005(4) 0.029(4) -0.013(4) C44 0.021(3) 0.030(4) 0.031(4) -0.007(3) 0.012(3) 0.001(3) C45 0.028(4) 0.049(5) 0.052(5) -0.015(4) 0.009(4) -0.006(3) C46 0.025(4) 0.035(4) 0.062(5) 0.006(4) 0.014(3) 0.007(3) C47 0.023(4) 0.032(4) 0.050(5) -0.004(3) 0.014(3) 0.006(3) C48 0.017(3) 0.018(3) 0.029(4) 0.000(3) 0.014(3) 0.001(3) C49 0.021(3) 0.026(4) 0.023(4) 0.008(3) 0.005(3) 0.004(3) C50 0.035(4) 0.025(4) 0.030(4) -0.005(3) 0.015(3) 0.005(3) C51 0.038(4) 0.020(3) 0.035(4) -0.003(3) 0.020(3) -0.001(3) C52 0.026(4) 0.032(4) 0.029(4) 0.009(3) 0.011(3) 0.009(3) C53 0.018(3) 0.021(3) 0.022(4) 0.003(3) 0.008(3) 0.001(3) C54 0.027(4) 0.038(4) 0.026(4) 0.000(3) 0.004(3) 0.011(3) C55 0.075(6) 0.060(5) 0.025(4) -0.005(4) 0.014(4) 0.029(4) C56 0.033(4) 0.045(4) 0.040(4) 0.017(3) 0.016(3) 0.017(3) C57 0.025(4) 0.043(4) 0.031(4) -0.003(3) -0.002(3) 0.003(3) C58 0.036(4) 0.022(3) 0.042(5) 0.004(3) 0.019(3) 0.000(3) C59 0.144(9) 0.030(5) 0.099(8) 0.010(5) 0.079(7) 0.014(5) C62 0.016(3) 0.023(3) 0.029(4) -0.001(3) 0.004(3) 0.000(3) C63 0.021(3) 0.035(4) 0.056(5) -0.001(4) 0.008(3) -0.007(3) C64 0.033(4) 0.045(4) 0.040(5) 0.001(4) 0.001(3) 0.003(3) C65 0.017(3) 0.034(4) 0.039(4) -0.012(3) 0.002(3) -0.002(3) Sm2 0.01360(16) 0.02058(17) 0.0253(2) 0.00351(15) 0.00083(14) 0.00077(14) N21 0.023(3) 0.059(4) 0.046(4) 0.039(3) 0.005(3) 0.009(3) N22 0.015(3) 0.023(3) 0.039(4) 0.000(2) -0.004(2) -0.001(2) N23 0.023(3) 0.025(3) 0.033(3) 0.003(2) -0.008(2) 0.000(2) N24 0.017(3) 0.014(3) 0.026(3) -0.006(2) 0.001(2) 0.001(2) C101 0.052(5) 0.062(6) 0.110(8) -0.010(5) 0.019(5) 0.031(5) C102 0.024(4) 0.069(6) 0.076(6) 0.053(5) 0.005(4) 0.015(4) C103 0.018(4) 0.053(5) 0.073(6) 0.029(4) 0.002(4) 0.012(3) C104 0.026(4) 0.025(4) 0.065(6) 0.003(4) 0.002(4) 0.001(3) C106 0.031(4) 0.073(6) 0.063(6) 0.055(5) 0.015(4) 0.016(4) C107 0.025(4) 0.148(9) 0.042(6) 0.049(6) 0.003(4) 0.002(5) C110 0.080(7) 0.068(7) 0.134(11) 0.049(7) 0.062(7) 0.012(6) C10A 0.080(7) 0.068(7) 0.134(11) 0.049(7) 0.062(7) 0.012(6) C111 0.049(5) 0.052(5) 0.110(8) 0.045(5) 0.048(5) 0.017(4) C116 0.115(9) 0.058(7) 0.141(11) 0.012(6) 0.057(8) 0.014(6) C16A 0.115(9) 0.058(7) 0.141(11) 0.012(6) 0.057(8) 0.014(6) C118 0.025(4) 0.030(4) 0.048(5) -0.017(4) -0.002(3) 0.016(3) C119 0.047(5) 0.027(4) 0.079(7) -0.019(4) -0.017(5) 0.012(4) C120 0.059(6) 0.064(6) 0.075(8) -0.045(6) -0.034(5) 0.021(5) C121 0.072(7) 0.106(9) 0.058(7) -0.031(6) 0.007(6) 0.042(6) C122 0.037(5) 0.111(7) 0.035(5) -0.018(5) 0.007(4) 0.019(5) C123 0.029(4) 0.063(5) 0.036(5) -0.007(4) 0.017(4) 0.016(4) C124 0.057(6) 0.041(5) 0.122(9) 0.003(5) -0.043(6) -0.010(5) C24A 0.057(6) 0.041(5) 0.122(9) 0.003(5) -0.043(6) -0.010(5) C125 0.068(6) 0.069(6) 0.078(7) -0.008(5) -0.012(5) 0.010(5) C127 0.023(4) 0.080(6) 0.037(5) 0.000(4) 0.007(3) -0.006(4) C128 0.080(7) 0.082(8) 0.112(9) 0.022(6) 0.000(7) -0.017(6) C129 0.026(4) 0.195(12) 0.091(8) -0.035(8) 0.020(5) -0.001(6) C130 0.027(3) 0.024(4) 0.030(4) -0.004(3) 0.003(3) -0.006(3) C131 0.023(3) 0.029(4) 0.026(4) -0.005(3) 0.001(3) 0.004(3) C132 0.018(3) 0.039(4) 0.038(4) -0.012(3) 0.007(3) -0.002(3) C133 0.030(4) 0.031(4) 0.037(4) -0.010(3) 0.011(3) -0.015(3) C134 0.029(4) 0.030(4) 0.030(4) 0.000(3) -0.001(3) -0.011(3) C135 0.023(3) 0.019(3) 0.031(4) -0.004(3) -0.003(3) -0.002(3) C136 0.023(4) 0.038(4) 0.045(5) -0.011(4) -0.011(3) 0.006(3) C137 0.029(4) 0.048(5) 0.056(5) 0.003(4) -0.013(4) -0.003(4) C138 0.040(4) 0.045(5) 0.070(6) -0.021(4) -0.008(4) 0.021(4) C139 0.031(4) 0.053(5) 0.060(6) -0.004(4) -0.007(4) 0.003(4) C140 0.042(4) 0.038(4) 0.050(5) -0.010(4) 0.014(4) -0.021(4) C141 0.163(11) 0.137(10) 0.049(7) 0.003(6) 0.038(7) -0.090(9) C142 0.037(5) 0.059(6) 0.162(10) -0.006(6) 0.027(6) -0.031(4) C143 0.049(5) 0.046(5) 0.072(6) 0.002(4) 0.004(4) -0.022(4) C144 0.022(4) 0.030(4) 0.074(6) 0.012(4) -0.009(4) -0.006(3) C145 0.053(5) 0.067(6) 0.080(7) 0.025(5) -0.038(5) -0.033(5) C146 0.030(4) 0.032(5) 0.174(10) 0.023(5) 0.000(6) 0.003(4) C147 0.022(4) 0.043(5) 0.105(7) 0.008(5) 0.015(4) 0.000(3) C148 0.011(3) 0.022(3) 0.023(4) -0.002(3) 0.002(3) -0.006(3) C149 0.005(3) 0.032(4) 0.024(4) 0.000(3) 0.000(3) -0.001(3) C150 0.012(3) 0.033(4) 0.027(4) 0.010(3) -0.002(3) -0.004(3) C151 0.015(3) 0.028(4) 0.036(4) 0.001(3) -0.010(3) -0.001(3) C152 0.021(3) 0.030(4) 0.026(4) -0.006(3) 0.000(3) 0.001(3) C153 0.010(3) 0.020(3) 0.022(4) -0.001(3) -0.005(3) 0.000(2) C154 0.026(4) 0.054(5) 0.021(4) 0.009(3) 0.004(3) 0.016(3) C155 0.028(4) 0.090(6) 0.036(5) 0.013(4) 0.015(4) 0.013(4) C156 0.042(4) 0.063(5) 0.033(4) -0.015(4) -0.007(3) 0.013(4) C157 0.064(5) 0.086(6) 0.023(4) 0.014(4) 0.010(4) 0.028(5) C158 0.036(4) 0.020(4) 0.055(5) 0.003(3) -0.014(4) 0.002(3) C161 0.051(5) 0.047(5) 0.058(6) 0.013(4) 0.002(4) 0.019(4) C162 0.025(3) 0.032(4) 0.018(4) 0.004(3) 0.009(3) 0.002(3) C163 0.028(4) 0.042(4) 0.025(4) 0.009(3) 0.006(3) 0.005(3) C164 0.053(5) 0.058(5) 0.040(5) 0.017(4) 0.031(4) 0.020(4) C165 0.030(4) 0.037(4) 0.036(4) 0.010(3) 0.007(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N13 2.260(4) . ? Sm1 N14 2.311(5) . ? Sm1 N12 2.384(5) . ? Sm1 N11 2.445(5) . ? N11 C2 1.341(7) . ? N11 C6 1.456(7) . ? N12 C4 1.327(7) . ? N12 C18 1.439(7) . ? N13 C30 1.427(7) . ? N13 H13A 0.8800 . ? N14 C48 1.394(6) . ? N14 H14A 0.8800 . ? C1 C2 1.524(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.400(8) . ? C3 C4 1.394(8) . ? C3 H3A 0.9500 . ? C4 C5 1.528(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.398(8) . ? C6 C11 1.416(8) . ? C7 C8 1.405(8) . ? C7 C12 1.518(8) . ? C8 C9 1.376(8) . ? C8 H8A 0.9500 . ? C9 C10 1.382(9) . ? C9 H9A 0.9500 . ? C10 C11 1.398(8) . ? C10 H10A 0.9500 . ? C11 C15 1.517(8) . ? C12 C14 1.530(9) . ? C12 C13 1.532(9) . ? C12 H12A 1.0000 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13 H13D 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C15 C17 1.521(9) . ? C15 C16 1.532(9) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.410(8) . ? C18 C23 1.428(8) . ? C19 C20 1.392(8) . ? C19 C24 1.527(8) . ? C20 C21 1.378(8) . ? C20 H20A 0.9500 . ? C21 C22 1.386(8) . ? C21 H21A 0.9500 . ? C22 C23 1.381(8) . ? C22 H22A 0.9500 . ? C23 C27 1.507(8) . ? C24 C25 1.520(8) . ? C24 C26 1.529(8) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.517(9) . ? C27 C29 1.548(9) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.418(7) . ? C30 C35 1.437(7) . ? C31 C32 1.394(7) . ? C31 C36 1.530(7) . ? C32 C33 1.389(8) . ? C32 H32A 0.9500 . ? C33 C34 1.385(8) . ? C33 C40 1.536(8) . ? C34 C35 1.395(7) . ? C34 H34A 0.9500 . ? C35 C44 1.555(8) . ? C36 C37 1.527(9) . ? C36 C39 1.539(8) . ? C36 C38 1.541(8) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.529(9) . ? C40 C42 1.531(9) . ? C40 C43 1.532(9) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.521(8) . ? C44 C46 1.543(8) . ? C44 C47 1.571(8) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.420(8) . ? C48 C53 1.430(8) . ? C49 C50 1.399(8) . ? C49 C54 1.550(8) . ? C50 C51 1.378(8) . ? C50 H50A 0.9500 . ? C51 C52 1.392(8) . ? C51 C58 1.536(8) . ? C52 C53 1.397(8) . ? C52 H52A 0.9500 . ? C53 C62 1.537(8) . ? C54 C55 1.537(8) . ? C54 C56 1.542(8) . ? C54 C57 1.554(8) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C61A 1.440(16) . ? C58 C61 1.447(16) . ? C58 C59 1.487(9) . ? C58 C60 1.658(14) . ? C58 C60A 1.660(16) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C60A H60D 0.9800 . ? C60A H60E 0.9800 . ? C60A H60F 0.9800 . ? C61A H61D 0.9800 . ? C61A H61E 0.9800 . ? C61A H61F 0.9800 . ? C62 C63 1.545(8) . ? C62 C65 1.546(8) . ? C62 C64 1.548(8) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? Sm2 N23 2.253(5) . ? Sm2 N24 2.334(4) . ? Sm2 N22 2.354(5) . ? Sm2 N21 2.432(5) . ? N21 C102 1.341(8) . ? N21 C106 1.456(9) . ? N22 C104 1.333(8) . ? N22 C118 1.458(8) . ? N23 C130 1.425(7) . ? N23 H23A 0.8800 . ? N24 C148 1.389(7) . ? N24 H24B 0.8800 . ? C101 C104 1.512(10) . ? C101 H10F 0.9800 . ? C101 H10G 0.9800 . ? C101 H10H 0.9800 . ? C102 C103 1.398(10) . ? C102 C105 1.506(15) . ? C102 C05A 1.638(15) . ? C103 C104 1.374(9) . ? C103 H10B 0.9500 . ? C105 H10C 0.9800 . ? C105 H10D 0.9800 . ? C105 H10E 0.9800 . ? C05A H05A 0.9800 . ? C05A H05B 0.9800 . ? C05A H05C 0.9800 . ? C106 C111 1.401(11) . ? C106 C107 1.415(12) . ? C107 C112 1.322(17) . ? C107 C108 1.429(17) . ? C107 C08A 1.480(18) . ? C107 C12A 1.742(18) . ? C108 C109 1.40(2) . ? C108 H10I 0.9500 . ? C109 C110 1.072(18) . ? C109 H10K 0.9500 . ? C110 C111 1.412(11) . ? C08A C09A 1.40(2) . ? C08A H08A 0.9500 . ? C09A H09A 0.9500 . ? C111 C15A 1.264(16) . ? C111 C115 1.798(18) . ? C112 C114 1.51(2) . ? C112 C113 1.54(2) . ? C112 H11A 1.0000 . ? C113 H11B 0.9800 . ? C113 H11C 0.9800 . ? C113 H11D 0.9800 . ? C114 H11E 0.9800 . ? C114 H11F 0.9800 . ? C114 H11G 0.9800 . ? C115 C116 1.303(16) . ? C115 C117 1.53(2) . ? C115 H11H 1.0000 . ? C116 H11I 0.9800 . ? C116 H11J 0.9800 . ? C116 H11K 0.9800 . ? C117 H11L 0.9800 . ? C117 H11M 0.9800 . ? C117 H11N 0.9800 . ? C12A C14A 1.51(2) . ? C12A C13A 1.53(2) . ? C12A H12B 1.0000 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C13A H13G 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C14A H14G 0.9800 . ? C15A C17A 1.56(2) . ? C15A H15B 1.0000 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C118 C119 1.401(9) . ? C118 C123 1.406(9) . ? C119 C120 1.410(11) . ? C119 C124 1.509(12) . ? C120 C121 1.368(12) . ? C120 H12C 0.9500 . ? C121 C122 1.342(11) . ? C121 H12D 0.9500 . ? C122 C123 1.393(9) . ? C122 H12E 0.9500 . ? C123 C127 1.503(9) . ? C124 C125 1.526(11) . ? C124 C126 1.663(15) . ? C124 H124 1.0000 . ? C125 H12F 0.9800 . ? C125 H12G 0.9800 . ? C125 H12H 0.9800 . ? C126 H12I 0.9800 . ? C126 H12J 0.9800 . ? C126 H12K 0.9800 . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 0.9800 . ? C127 C128 1.513(10) . ? C127 C129 1.519(9) . ? C127 H12L 1.0000 . ? C128 H12M 0.9800 . ? C128 H12N 0.9800 . ? C128 H12O 0.9800 . ? C129 H12P 0.9800 . ? C129 H12Q 0.9800 . ? C129 H12R 0.9800 . ? C130 C135 1.424(8) . ? C130 C131 1.426(8) . ? C131 C132 1.388(8) . ? C131 C136 1.545(8) . ? C132 C133 1.376(8) . ? C132 H13H 0.9500 . ? C133 C134 1.398(8) . ? C133 C140 1.542(8) . ? C134 C135 1.382(8) . ? C134 H13I 0.9500 . ? C135 C144 1.562(8) . ? C136 C138 1.538(9) . ? C136 C137 1.539(9) . ? C136 C139 1.545(8) . ? C137 H13J 0.9800 . ? C137 H13K 0.9800 . ? C137 H13L 0.9800 . ? C138 H13M 0.9800 . ? C138 H13N 0.9800 . ? C138 H13O 0.9800 . ? C139 H13P 0.9800 . ? C139 H13Q 0.9800 . ? C139 H13R 0.9800 . ? C140 C141 1.515(10) . ? C140 C142 1.520(9) . ? C140 C143 1.535(9) . ? C141 H14H 0.9800 . ? C141 H14I 0.9800 . ? C141 H14J 0.9800 . ? C142 H14K 0.9800 . ? C142 H14L 0.9800 . ? C142 H14M 0.9800 . ? C143 H14N 0.9800 . ? C143 H14O 0.9800 . ? C143 H14P 0.9800 . ? C144 C147 1.525(10) . ? C144 C145 1.528(10) . ? C144 C146 1.538(9) . ? C145 H14Q 0.9800 . ? C145 H14R 0.9800 . ? C145 H14S 0.9800 . ? C146 H14T 0.9800 . ? C146 H14U 0.9800 . ? C146 H14V 0.9800 . ? C147 H14W 0.9800 . ? C147 H14X 0.9800 . ? C147 H14Y 0.9800 . ? C148 C153 1.420(8) . ? C148 C149 1.443(8) . ? C149 C150 1.385(8) . ? C149 C154 1.545(8) . ? C150 C151 1.388(8) . ? C150 H15C 0.9500 . ? C151 C152 1.384(8) . ? C151 C158 1.534(8) . ? C152 C153 1.395(8) . ? C152 H15D 0.9500 . ? C153 C162 1.563(8) . ? C154 C157 1.530(8) . ? C154 C156 1.530(9) . ? C154 C155 1.547(8) . ? C155 H15E 0.9800 . ? C155 H15F 0.9800 . ? C155 H15G 0.9800 . ? C156 H15H 0.9800 . ? C156 H15I 0.9800 . ? C156 H15J 0.9800 . ? C157 H15K 0.9800 . ? C157 H15L 0.9800 . ? C157 H15M 0.9800 . ? C158 C60B 1.399(18) . ? C158 C159 1.414(16) . ? C158 C161 1.524(9) . ? C158 C59A 1.687(17) . ? C158 C160 1.691(15) . ? C159 H15N 0.9800 . ? C159 H15O 0.9800 . ? C159 H15P 0.9800 . ? C160 H16G 0.9800 . ? C160 H16H 0.9800 . ? C160 H16I 0.9800 . ? C59A H59D 0.9800 . ? C59A H59E 0.9800 . ? C59A H59F 0.9800 . ? C60B H60G 0.9800 . ? C60B H60H 0.9800 . ? C60B H60I 0.9800 . ? C161 H16J 0.9800 . ? C161 H16K 0.9800 . ? C161 H16L 0.9800 . ? C162 C163 1.526(8) . ? C162 C165 1.531(8) . ? C162 C164 1.549(8) . ? C163 H16M 0.9800 . ? C163 H16N 0.9800 . ? C163 H16O 0.9800 . ? C164 H16P 0.9800 . ? C164 H16Q 0.9800 . ? C164 H16R 0.9800 . ? C165 H16S 0.9800 . ? C165 H16T 0.9800 . ? C165 H16U 0.9800 . ? C201 C202 1.22(2) . ? C202 C203 1.37(2) . ? C203 C204 1.284(18) . ? C204 C205 1.413(19) . ? C206 C207 1.45(2) . ? C207 C208 1.60(2) . ? C207 C208 1.68(2) 3_666 ? C208 C207 1.68(2) 3_666 ? C208 C208 1.81(4) 3_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N13 Sm1 N14 133.62(16) . . ? N13 Sm1 N12 100.05(16) . . ? N14 Sm1 N12 100.92(16) . . ? N13 Sm1 N11 99.10(16) . . ? N14 Sm1 N11 125.13(15) . . ? N12 Sm1 N11 79.64(15) . . ? C2 N11 C6 117.6(5) . . ? C2 N11 Sm1 120.0(4) . . ? C6 N11 Sm1 121.8(3) . . ? C4 N12 C18 119.7(5) . . ? C4 N12 Sm1 122.6(4) . . ? C18 N12 Sm1 117.2(3) . . ? C30 N13 Sm1 159.3(4) . . ? C30 N13 H13A 100.3 . . ? Sm1 N13 H13A 100.3 . . ? C48 N14 Sm1 133.3(4) . . ? C48 N14 H14A 113.4 . . ? Sm1 N14 H14A 113.4 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N11 C2 C3 125.2(6) . . ? N11 C2 C1 120.3(5) . . ? C3 C2 C1 114.4(5) . . ? C4 C3 C2 131.7(6) . . ? C4 C3 H3A 114.1 . . ? C2 C3 H3A 114.1 . . ? N12 C4 C3 124.9(5) . . ? N12 C4 C5 120.6(6) . . ? C3 C4 C5 114.4(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 121.2(6) . . ? C7 C6 N11 121.5(5) . . ? C11 C6 N11 117.1(5) . . ? C6 C7 C8 118.2(6) . . ? C6 C7 C12 123.3(5) . . ? C8 C7 C12 118.5(6) . . ? C9 C8 C7 121.8(6) . . ? C9 C8 H8A 119.1 . . ? C7 C8 H8A 119.1 . . ? C8 C9 C10 119.0(6) . . ? C8 C9 H9A 120.5 . . ? C10 C9 H9A 120.5 . . ? C9 C10 C11 122.2(6) . . ? C9 C10 H10A 118.9 . . ? C11 C10 H10A 118.9 . . ? C10 C11 C6 117.5(6) . . ? C10 C11 C15 119.7(6) . . ? C6 C11 C15 122.8(6) . . ? C7 C12 C14 111.6(6) . . ? C7 C12 C13 112.2(5) . . ? C14 C12 C13 109.2(6) . . ? C7 C12 H12A 107.9 . . ? C14 C12 H12A 107.9 . . ? C13 C12 H12A 107.9 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C13 H13D 109.5 . . ? H13B C13 H13D 109.5 . . ? H13C C13 H13D 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C14 H14D 109.5 . . ? H14B C14 H14D 109.5 . . ? H14C C14 H14D 109.5 . . ? C11 C15 C17 113.1(6) . . ? C11 C15 C16 110.0(5) . . ? C17 C15 C16 110.2(5) . . ? C11 C15 H15A 107.8 . . ? C17 C15 H15A 107.8 . . ? C16 C15 H15A 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.2(6) . . ? C19 C18 N12 118.9(5) . . ? C23 C18 N12 120.8(5) . . ? C20 C19 C18 118.6(6) . . ? C20 C19 C24 120.3(6) . . ? C18 C19 C24 121.0(5) . . ? C21 C20 C19 122.0(6) . . ? C21 C20 H20A 119.0 . . ? C19 C20 H20A 119.0 . . ? C20 C21 C22 118.6(6) . . ? C20 C21 H21A 120.7 . . ? C22 C21 H21A 120.7 . . ? C23 C22 C21 122.9(6) . . ? C23 C22 H22A 118.6 . . ? C21 C22 H22A 118.6 . . ? C22 C23 C18 117.7(6) . . ? C22 C23 C27 119.6(6) . . ? C18 C23 C27 122.7(6) . . ? C25 C24 C19 113.7(5) . . ? C25 C24 C26 110.3(5) . . ? C19 C24 C26 110.5(5) . . ? C25 C24 H24A 107.3 . . ? C19 C24 H24A 107.3 . . ? C26 C24 H24A 107.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 113.0(6) . . ? C23 C27 C29 110.8(6) . . ? C28 C27 C29 109.3(6) . . ? C23 C27 H27A 107.8 . . ? C28 C27 H27A 107.8 . . ? C29 C27 H27A 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 N13 119.6(5) . . ? C31 C30 C35 118.6(5) . . ? N13 C30 C35 121.8(5) . . ? C32 C31 C30 118.4(5) . . ? C32 C31 C36 118.5(5) . . ? C30 C31 C36 123.1(5) . . ? C33 C32 C31 124.5(5) . . ? C33 C32 H32A 117.7 . . ? C31 C32 H32A 117.7 . . ? C34 C33 C32 115.9(5) . . ? C34 C33 C40 123.7(5) . . ? C32 C33 C40 120.3(5) . . ? C33 C34 C35 123.7(5) . . ? C33 C34 H34A 118.1 . . ? C35 C34 H34A 118.1 . . ? C34 C35 C30 118.7(5) . . ? C34 C35 C44 118.5(5) . . ? C30 C35 C44 122.7(5) . . ? C37 C36 C31 110.7(5) . . ? C37 C36 C39 105.3(5) . . ? C31 C36 C39 113.3(5) . . ? C37 C36 C38 111.9(5) . . ? C31 C36 C38 109.8(5) . . ? C39 C36 C38 105.7(5) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? 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 . . ? C41 C40 C42 109.2(6) . . ? C41 C40 C43 108.4(6) . . ? C42 C40 C43 107.7(6) . . ? C41 C40 C33 109.2(5) . . ? C42 C40 C33 110.1(5) . . ? C43 C40 C33 112.2(5) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C46 111.5(5) . . ? C45 C44 C35 112.5(5) . . ? C46 C44 C35 110.3(5) . . ? C45 C44 C47 105.3(5) . . ? C46 C44 C47 104.7(5) . . ? C35 C44 C47 112.1(5) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N14 C48 C49 124.1(5) . . ? N14 C48 C53 119.0(5) . . ? C49 C48 C53 116.9(5) . . ? C50 C49 C48 119.4(5) . . ? C50 C49 C54 118.1(5) . . ? C48 C49 C54 122.5(5) . . ? C51 C50 C49 123.2(6) . . ? C51 C50 H50A 118.4 . . ? C49 C50 H50A 118.4 . . ? C50 C51 C52 116.5(6) . . ? C50 C51 C58 122.3(6) . . ? C52 C51 C58 121.0(6) . . ? C51 C52 C53 122.8(6) . . ? C51 C52 H52A 118.6 . . ? C53 C52 H52A 118.6 . . ? C52 C53 C48 119.2(5) . . ? C52 C53 C62 119.0(5) . . ? C48 C53 C62 121.3(5) . . ? C55 C54 C56 105.9(5) . . ? C55 C54 C49 112.4(5) . . ? C56 C54 C49 109.5(5) . . ? C55 C54 C57 105.5(5) . . ? C56 C54 C57 110.5(5) . . ? C49 C54 C57 112.8(5) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C61A C58 C61 67.4(9) . . ? C61A C58 C59 125.1(9) . . ? C61 C58 C59 120.8(9) . . ? C61A C58 C51 111.3(8) . . ? C61 C58 C51 114.9(8) . . ? C59 C58 C51 111.1(5) . . ? C61A C58 C60 41.7(8) . . ? C61 C58 C60 106.2(9) . . ? C59 C58 C60 92.3(7) . . ? C51 C58 C60 108.2(7) . . ? C61A C58 C60A 103.5(10) . . ? C61 C58 C60A 36.9(8) . . ? C59 C58 C60A 93.8(8) . . ? C51 C58 C60A 109.3(7) . . ? C60 C58 C60A 136.7(9) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? C58 C61 H61A 109.5 . . ? C58 C61 H61B 109.5 . . ? C58 C61 H61C 109.5 . . ? C58 C60A H60D 109.5 . . ? C58 C60A H60E 109.5 . . ? H60D C60A H60E 109.5 . . ? C58 C60A H60F 109.5 . . ? H60D C60A H60F 109.5 . . ? H60E C60A H60F 109.5 . . ? C58 C61A H61D 109.5 . . ? C58 C61A H61E 109.5 . . ? H61D C61A H61E 109.5 . . ? C58 C61A H61F 109.5 . . ? H61D C61A H61F 109.5 . . ? H61E C61A H61F 109.5 . . ? C53 C62 C63 108.1(5) . . ? C53 C62 C65 115.4(5) . . ? C63 C62 C65 108.2(5) . . ? C53 C62 C64 112.3(5) . . ? C63 C62 C64 107.5(5) . . ? C65 C62 C64 105.0(5) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 C65 H65A 109.5 . . ? C62 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C62 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N23 Sm2 N24 135.86(16) . . ? N23 Sm2 N22 96.73(16) . . ? N24 Sm2 N22 101.77(16) . . ? N23 Sm2 N21 96.40(18) . . ? N24 Sm2 N21 126.37(16) . . ? N22 Sm2 N21 78.24(19) . . ? C102 N21 C106 116.5(5) . . ? C102 N21 Sm2 122.3(4) . . ? C106 N21 Sm2 121.0(4) . . ? C104 N22 C118 117.5(6) . . ? C104 N22 Sm2 127.1(5) . . ? C118 N22 Sm2 114.9(3) . . ? C130 N23 Sm2 154.7(4) . . ? C130 N23 H23A 102.6 . . ? Sm2 N23 H23A 102.6 . . ? C148 N24 Sm2 132.4(4) . . ? C148 N24 H24B 113.8 . . ? Sm2 N24 H24B 113.8 . . ? C104 C101 H10F 109.5 . . ? C104 C101 H10G 109.5 . . ? H10F C101 H10G 109.5 . . ? C104 C101 H10H 109.5 . . ? H10F C101 H10H 109.5 . . ? H10G C101 H10H 109.5 . . ? N21 C102 C103 124.8(7) . . ? N21 C102 C105 123.4(8) . . ? C103 C102 C105 109.8(8) . . ? N21 C102 C05A 114.9(8) . . ? C103 C102 C05A 119.2(7) . . ? C105 C102 C05A 27.4(7) . . ? C104 C103 C102 132.0(6) . . ? C104 C103 H10B 114.0 . . ? C102 C103 H10B 114.0 . . ? N22 C104 C103 122.8(7) . . ? N22 C104 C101 120.3(7) . . ? C103 C104 C101 116.9(6) . . ? C102 C105 H10C 109.5 . . ? C102 C105 H10D 109.5 . . ? C102 C105 H10E 109.5 . . ? C102 C05A H05A 109.5 . . ? C102 C05A H05B 109.5 . . ? H05A C05A H05B 109.5 . . ? C102 C05A H05C 109.5 . . ? H05A C05A H05C 109.5 . . ? H05B C05A H05C 109.5 . . ? C111 C106 C107 121.9(8) . . ? C111 C106 N21 117.7(9) . . ? C107 C106 N21 120.3(7) . . ? C112 C107 C106 118.9(10) . . ? C112 C107 C108 131.0(13) . . ? C106 C107 C108 105.9(10) . . ? C112 C107 C08A 112.5(13) . . ? C106 C107 C08A 128.5(10) . . ? C108 C107 C08A 26.6(8) . . ? C112 C107 C12A 22.5(8) . . ? C106 C107 C12A 128.2(8) . . ? C108 C107 C12A 125.8(11) . . ? C08A C107 C12A 101.2(11) . . ? C109 C108 C107 127.3(15) . . ? C109 C108 H10I 116.3 . . ? C107 C108 H10I 116.3 . . ? C110 C109 C108 121(2) . . ? C110 C109 H10K 119.3 . . ? C108 C109 H10K 119.3 . . ? C109 C110 C111 122.5(16) . . ? C09A C08A C107 109.6(15) . . ? C09A C08A H08A 125.2 . . ? C107 C08A H08A 125.2 . . ? C08A C09A H09A 118.4 . . ? C15A C111 C106 120.9(10) . . ? C15A C111 C110 118.5(11) . . ? C106 C111 C110 119.3(10) . . ? C15A C111 C115 20.1(9) . . ? C106 C111 C115 121.4(8) . . ? C110 C111 C115 118.5(9) . . ? C107 C112 C114 105.0(13) . . ? C107 C112 C113 114.8(14) . . ? C114 C112 C113 109.6(14) . . ? C107 C112 H11A 109.1 . . ? C114 C112 H11A 109.1 . . ? C113 C112 H11A 109.1 . . ? C116 C115 C117 111.3(13) . . ? C116 C115 C111 109.6(12) . . ? C117 C115 C111 107.9(12) . . ? C116 C115 H11H 109.3 . . ? C117 C115 H11H 109.3 . . ? C111 C115 H11H 109.3 . . ? C14A C12A C13A 110.8(14) . . ? C14A C12A C107 120.8(12) . . ? C13A C12A C107 108.5(12) . . ? C14A C12A H12B 105.1 . . ? C13A C12A H12B 105.1 . . ? C107 C12A H12B 105.1 . . ? C12A C13A H13E 109.5 . . ? C12A C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C12A C13A H13G 109.5 . . ? H13E C13A H13G 109.5 . . ? H13F C13A H13G 109.5 . . ? C12A C14A H14E 109.5 . . ? C12A C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C12A C14A H14G 109.5 . . ? H14E C14A H14G 109.5 . . ? H14F C14A H14G 109.5 . . ? C111 C15A C17A 115.6(15) . . ? C111 C15A H15B 107.6 . . ? C17A C15A H15B 107.6 . . ? C15A C17A H17D 109.5 . . ? C15A C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? C15A C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C119 C118 C123 120.5(7) . . ? C119 C118 N22 119.7(7) . . ? C123 C118 N22 119.7(6) . . ? C118 C119 C120 118.5(8) . . ? C118 C119 C124 120.4(8) . . ? C120 C119 C124 120.9(8) . . ? C121 C120 C119 120.3(8) . . ? C121 C120 H12C 119.9 . . ? C119 C120 H12C 119.9 . . ? C122 C121 C120 120.4(10) . . ? C122 C121 H12D 119.8 . . ? C120 C121 H12D 119.8 . . ? C121 C122 C123 122.9(9) . . ? C121 C122 H12E 118.6 . . ? C123 C122 H12E 118.6 . . ? C122 C123 C118 117.3(7) . . ? C122 C123 C127 118.3(7) . . ? C118 C123 C127 124.4(7) . . ? C119 C124 C125 115.0(7) . . ? C119 C124 C126 104.0(9) . . ? C125 C124 C126 105.7(7) . . ? C119 C124 H124 110.6 . . ? C125 C124 H124 110.6 . . ? C126 C124 H124 110.6 . . ? C124 C125 H12F 109.5 . . ? C124 C125 H12G 109.5 . . ? H12F C125 H12G 109.5 . . ? C124 C125 H12H 109.5 . . ? H12F C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? H26D C26A H26E 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? C123 C127 C128 113.2(6) . . ? C123 C127 C129 112.7(7) . . ? C128 C127 C129 110.2(7) . . ? C123 C127 H12L 106.8 . . ? C128 C127 H12L 106.8 . . ? C129 C127 H12L 106.8 . . ? C127 C128 H12M 109.5 . . ? C127 C128 H12N 109.5 . . ? H12M C128 H12N 109.5 . . ? C127 C128 H12O 109.5 . . ? H12M C128 H12O 109.5 . . ? H12N C128 H12O 109.5 . . ? C127 C129 H12P 109.5 . . ? C127 C129 H12Q 109.5 . . ? H12P C129 H12Q 109.5 . . ? C127 C129 H12R 109.5 . . ? H12P C129 H12R 109.5 . . ? H12Q C129 H12R 109.5 . . ? C135 C130 N23 119.5(5) . . ? C135 C130 C131 118.2(5) . . ? N23 C130 C131 122.3(5) . . ? C132 C131 C130 118.4(5) . . ? C132 C131 C136 118.0(5) . . ? C130 C131 C136 123.6(5) . . ? C133 C132 C131 124.0(6) . . ? C133 C132 H13H 118.0 . . ? C131 C132 H13H 118.0 . . ? C132 C133 C134 116.4(6) . . ? C132 C133 C140 124.4(6) . . ? C134 C133 C140 119.2(6) . . ? C135 C134 C133 123.1(6) . . ? C135 C134 H13I 118.4 . . ? C133 C134 H13I 118.4 . . ? C134 C135 C130 119.0(6) . . ? C134 C135 C144 117.5(5) . . ? C130 C135 C144 123.5(5) . . ? C138 C136 C137 110.4(6) . . ? C138 C136 C139 104.4(5) . . ? C137 C136 C139 104.7(6) . . ? C138 C136 C131 112.6(6) . . ? C137 C136 C131 111.6(5) . . ? C139 C136 C131 112.6(6) . . ? C136 C137 H13J 109.5 . . ? C136 C137 H13K 109.5 . . ? H13J C137 H13K 109.5 . . ? C136 C137 H13L 109.5 . . ? H13J C137 H13L 109.5 . . ? H13K C137 H13L 109.5 . . ? C136 C138 H13M 109.5 . . ? C136 C138 H13N 109.5 . . ? H13M C138 H13N 109.5 . . ? C136 C138 H13O 109.5 . . ? H13M C138 H13O 109.5 . . ? H13N C138 H13O 109.5 . . ? C136 C139 H13P 109.5 . . ? C136 C139 H13Q 109.5 . . ? H13P C139 H13Q 109.5 . . ? C136 C139 H13R 109.5 . . ? H13P C139 H13R 109.5 . . ? H13Q C139 H13R 109.5 . . ? C141 C140 C142 108.9(7) . . ? C141 C140 C143 110.4(7) . . ? C142 C140 C143 107.2(6) . . ? C141 C140 C133 110.5(6) . . ? C142 C140 C133 111.3(6) . . ? C143 C140 C133 108.6(6) . . ? C140 C141 H14H 109.5 . . ? C140 C141 H14I 109.5 . . ? H14H C141 H14I 109.5 . . ? C140 C141 H14J 109.5 . . ? H14H C141 H14J 109.5 . . ? H14I C141 H14J 109.5 . . ? C140 C142 H14K 109.5 . . ? C140 C142 H14L 109.5 . . ? H14K C142 H14L 109.5 . . ? C140 C142 H14M 109.5 . . ? H14K C142 H14M 109.5 . . ? H14L C142 H14M 109.5 . . ? C140 C143 H14N 109.5 . . ? C140 C143 H14O 109.5 . . ? H14N C143 H14O 109.5 . . ? C140 C143 H14P 109.5 . . ? H14N C143 H14P 109.5 . . ? H14O C143 H14P 109.5 . . ? C147 C144 C145 111.1(6) . . ? C147 C144 C146 105.8(7) . . ? C145 C144 C146 107.2(6) . . ? C147 C144 C135 110.4(5) . . ? C145 C144 C135 110.4(6) . . ? C146 C144 C135 111.9(5) . . ? C144 C145 H14Q 109.5 . . ? C144 C145 H14R 109.5 . . ? H14Q C145 H14R 109.5 . . ? C144 C145 H14S 109.5 . . ? H14Q C145 H14S 109.5 . . ? H14R C145 H14S 109.5 . . ? C144 C146 H14T 109.5 . . ? C144 C146 H14U 109.5 . . ? H14T C146 H14U 109.5 . . ? C144 C146 H14V 109.5 . . ? H14T C146 H14V 109.5 . . ? H14U C146 H14V 109.5 . . ? C144 C147 H14W 109.5 . . ? C144 C147 H14X 109.5 . . ? H14W C147 H14X 109.5 . . ? C144 C147 H14Y 109.5 . . ? H14W C147 H14Y 109.5 . . ? H14X C147 H14Y 109.5 . . ? N24 C148 C153 120.1(5) . . ? N24 C148 C149 123.6(5) . . ? C153 C148 C149 116.2(5) . . ? C150 C149 C148 118.2(5) . . ? C150 C149 C154 118.9(5) . . ? C148 C149 C154 122.9(5) . . ? C149 C150 C151 124.6(6) . . ? C149 C150 H15C 117.7 . . ? C151 C150 H15C 117.7 . . ? C152 C151 C150 115.4(6) . . ? C152 C151 C158 124.0(6) . . ? C150 C151 C158 120.6(6) . . ? C151 C152 C153 123.3(6) . . ? C151 C152 H15D 118.4 . . ? C153 C152 H15D 118.4 . . ? C152 C153 C148 119.6(5) . . ? C152 C153 C162 119.4(5) . . ? C148 C153 C162 120.6(5) . . ? C157 C154 C156 105.8(6) . . ? C157 C154 C149 112.0(5) . . ? C156 C154 C149 109.9(5) . . ? C157 C154 C155 106.9(6) . . ? C156 C154 C155 110.8(6) . . ? C149 C154 C155 111.2(5) . . ? C154 C155 H15E 109.5 . . ? C154 C155 H15F 109.5 . . ? H15E C155 H15F 109.5 . . ? C154 C155 H15G 109.5 . . ? H15E C155 H15G 109.5 . . ? H15F C155 H15G 109.5 . . ? C154 C156 H15H 109.5 . . ? C154 C156 H15I 109.5 . . ? H15H C156 H15I 109.5 . . ? C154 C156 H15J 109.5 . . ? H15H C156 H15J 109.5 . . ? H15I C156 H15J 109.5 . . ? C154 C157 H15K 109.5 . . ? C154 C157 H15L 109.5 . . ? H15K C157 H15L 109.5 . . ? C154 C157 H15M 109.5 . . ? H15K C157 H15M 109.5 . . ? H15L C157 H15M 109.5 . . ? C60B C158 C159 81.7(10) . . ? C60B C158 C161 118.5(9) . . ? C159 C158 C161 117.3(9) . . ? C60B C158 C151 111.1(9) . . ? C159 C158 C151 114.9(9) . . ? C161 C158 C151 110.6(5) . . ? C60B C158 C59A 107.4(10) . . ? C159 C158 C59A 26.1(8) . . ? C161 C158 C59A 99.8(7) . . ? C151 C158 C59A 108.3(7) . . ? C60B C158 C160 27.4(9) . . ? C159 C158 C160 108.2(9) . . ? C161 C158 C160 98.9(7) . . ? C151 C158 C160 104.8(7) . . ? C59A C158 C160 132.8(9) . . ? C158 C159 H15N 109.5 . . ? C158 C159 H15O 109.5 . . ? C158 C159 H15P 109.5 . . ? C158 C160 H16G 109.5 . . ? C158 C160 H16H 109.5 . . ? C158 C160 H16I 109.5 . . ? C158 C59A H59D 109.5 . . ? C158 C59A H59E 109.5 . . ? H59D C59A H59E 109.5 . . ? C158 C59A H59F 109.5 . . ? H59D C59A H59F 109.5 . . ? H59E C59A H59F 109.5 . . ? C158 C60B H60G 109.5 . . ? C158 C60B H60H 109.5 . . ? H60G C60B H60H 109.5 . . ? C158 C60B H60I 109.5 . . ? H60G C60B H60I 109.5 . . ? H60H C60B H60I 109.5 . . ? C158 C161 H16J 109.5 . . ? C158 C161 H16K 109.5 . . ? H16J C161 H16K 109.5 . . ? C158 C161 H16L 109.5 . . ? H16J C161 H16L 109.5 . . ? H16K C161 H16L 109.5 . . ? C163 C162 C165 108.7(5) . . ? C163 C162 C164 107.0(5) . . ? C165 C162 C164 107.2(5) . . ? C163 C162 C153 113.9(5) . . ? C165 C162 C153 108.2(5) . . ? C164 C162 C153 111.7(5) . . ? C162 C163 H16M 109.5 . . ? C162 C163 H16N 109.5 . . ? H16M C163 H16N 109.5 . . ? C162 C163 H16O 109.5 . . ? H16M C163 H16O 109.5 . . ? H16N C163 H16O 109.5 . . ? C162 C164 H16P 109.5 . . ? C162 C164 H16Q 109.5 . . ? H16P C164 H16Q 109.5 . . ? C162 C164 H16R 109.5 . . ? H16P C164 H16R 109.5 . . ? H16Q C164 H16R 109.5 . . ? C162 C165 H16S 109.5 . . ? C162 C165 H16T 109.5 . . ? H16S C165 H16T 109.5 . . ? C162 C165 H16U 109.5 . . ? H16S C165 H16U 109.5 . . ? H16T C165 H16U 109.5 . . ? C201 C202 C203 154(2) . . ? C204 C203 C202 140.0(18) . . ? C203 C204 C205 139.0(18) . . ? C206 C207 C208 155(2) . . ? C206 C207 C208 88.6(15) . 3_666 ? C208 C207 C208 66.9(15) . 3_666 ? C207 C208 C207 113.2(15) . 3_666 ? C207 C208 C208 58.6(13) . 3_666 ? C207 C208 C208 54.5(12) 3_666 3_666 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N13 Sm1 N11 C2 63.2(4) . . . . ? N14 Sm1 N11 C2 -131.6(4) . . . . ? N12 Sm1 N11 C2 -35.5(4) . . . . ? N13 Sm1 N11 C6 -108.0(4) . . . . ? N14 Sm1 N11 C6 57.2(4) . . . . ? N12 Sm1 N11 C6 153.3(4) . . . . ? N13 Sm1 N12 C4 -62.6(5) . . . . ? N14 Sm1 N12 C4 159.0(4) . . . . ? N11 Sm1 N12 C4 35.0(4) . . . . ? N13 Sm1 N12 C18 109.3(4) . . . . ? N14 Sm1 N12 C18 -29.1(4) . . . . ? N11 Sm1 N12 C18 -153.2(4) . . . . ? N14 Sm1 N13 C30 -15.8(12) . . . . ? N12 Sm1 N13 C30 -131.6(11) . . . . ? N11 Sm1 N13 C30 147.4(11) . . . . ? N13 Sm1 N14 C48 40.8(6) . . . . ? N12 Sm1 N14 C48 156.2(5) . . . . ? N11 Sm1 N14 C48 -118.9(5) . . . . ? C6 N11 C2 C3 -167.3(5) . . . . ? Sm1 N11 C2 C3 21.1(8) . . . . ? C6 N11 C2 C1 11.3(8) . . . . ? Sm1 N11 C2 C1 -160.3(4) . . . . ? N11 C2 C3 C4 15.4(11) . . . . ? C1 C2 C3 C4 -163.3(6) . . . . ? C18 N12 C4 C3 169.2(6) . . . . ? Sm1 N12 C4 C3 -19.1(8) . . . . ? C18 N12 C4 C5 -8.9(8) . . . . ? Sm1 N12 C4 C5 162.8(4) . . . . ? C2 C3 C4 N12 -17.4(11) . . . . ? C2 C3 C4 C5 160.8(6) . . . . ? C2 N11 C6 C7 -93.2(7) . . . . ? Sm1 N11 C6 C7 78.2(6) . . . . ? C2 N11 C6 C11 90.3(7) . . . . ? Sm1 N11 C6 C11 -98.3(5) . . . . ? C11 C6 C7 C8 1.8(9) . . . . ? N11 C6 C7 C8 -174.5(5) . . . . ? C11 C6 C7 C12 -178.3(6) . . . . ? N11 C6 C7 C12 5.4(9) . . . . ? C6 C7 C8 C9 -0.4(9) . . . . ? C12 C7 C8 C9 179.7(6) . . . . ? C7 C8 C9 C10 -0.9(10) . . . . ? C8 C9 C10 C11 0.7(10) . . . . ? C9 C10 C11 C6 0.7(10) . . . . ? C9 C10 C11 C15 -178.7(6) . . . . ? C7 C6 C11 C10 -2.0(9) . . . . ? N11 C6 C11 C10 174.5(5) . . . . ? C7 C6 C11 C15 177.4(6) . . . . ? N11 C6 C11 C15 -6.1(8) . . . . ? C6 C7 C12 C14 111.2(7) . . . . ? C8 C7 C12 C14 -68.9(8) . . . . ? C6 C7 C12 C13 -125.8(6) . . . . ? C8 C7 C12 C13 54.1(8) . . . . ? C10 C11 C15 C17 -51.0(8) . . . . ? C6 C11 C15 C17 129.6(6) . . . . ? C10 C11 C15 C16 72.7(8) . . . . ? C6 C11 C15 C16 -106.7(7) . . . . ? C4 N12 C18 C19 -101.3(6) . . . . ? Sm1 N12 C18 C19 86.6(5) . . . . ? C4 N12 C18 C23 80.6(7) . . . . ? Sm1 N12 C18 C23 -91.5(5) . . . . ? C23 C18 C19 C20 -0.2(8) . . . . ? N12 C18 C19 C20 -178.3(5) . . . . ? C23 C18 C19 C24 -177.4(5) . . . . ? N12 C18 C19 C24 4.4(8) . . . . ? C18 C19 C20 C21 -1.1(9) . . . . ? C24 C19 C20 C21 176.1(5) . . . . ? C19 C20 C21 C22 1.9(9) . . . . ? C20 C21 C22 C23 -1.3(9) . . . . ? C21 C22 C23 C18 0.1(9) . . . . ? C21 C22 C23 C27 -178.3(6) . . . . ? C19 C18 C23 C22 0.6(8) . . . . ? N12 C18 C23 C22 178.8(5) . . . . ? C19 C18 C23 C27 179.0(5) . . . . ? N12 C18 C23 C27 -2.8(9) . . . . ? C20 C19 C24 C25 27.1(8) . . . . ? C18 C19 C24 C25 -155.7(6) . . . . ? C20 C19 C24 C26 -97.6(7) . . . . ? C18 C19 C24 C26 79.6(7) . . . . ? C22 C23 C27 C28 -69.7(8) . . . . ? C18 C23 C27 C28 111.9(7) . . . . ? C22 C23 C27 C29 53.4(8) . . . . ? C18 C23 C27 C29 -125.0(7) . . . . ? Sm1 N13 C30 C31 -6.6(14) . . . . ? Sm1 N13 C30 C35 172.1(8) . . . . ? N13 C30 C31 C32 175.1(5) . . . . ? C35 C30 C31 C32 -3.7(8) . . . . ? N13 C30 C31 C36 -2.9(8) . . . . ? C35 C30 C31 C36 178.3(5) . . . . ? C30 C31 C32 C33 2.2(9) . . . . ? C36 C31 C32 C33 -179.7(6) . . . . ? C31 C32 C33 C34 0.5(9) . . . . ? C31 C32 C33 C40 -176.9(6) . . . . ? C32 C33 C34 C35 -1.8(9) . . . . ? C40 C33 C34 C35 175.5(6) . . . . ? C33 C34 C35 C30 0.3(9) . . . . ? C33 C34 C35 C44 178.9(6) . . . . ? C31 C30 C35 C34 2.5(8) . . . . ? N13 C30 C35 C34 -176.2(5) . . . . ? C31 C30 C35 C44 -176.1(5) . . . . ? N13 C30 C35 C44 5.2(9) . . . . ? C32 C31 C36 C37 -112.7(6) . . . . ? C30 C31 C36 C37 65.3(7) . . . . ? C32 C31 C36 C39 5.4(8) . . . . ? C30 C31 C36 C39 -176.6(6) . . . . ? C32 C31 C36 C38 123.3(6) . . . . ? C30 C31 C36 C38 -58.7(7) . . . . ? C34 C33 C40 C41 -110.8(7) . . . . ? C32 C33 C40 C41 66.3(8) . . . . ? C34 C33 C40 C42 129.3(7) . . . . ? C32 C33 C40 C42 -53.6(8) . . . . ? C34 C33 C40 C43 9.3(9) . . . . ? C32 C33 C40 C43 -173.5(6) . . . . ? C34 C35 C44 C45 -120.4(6) . . . . ? C30 C35 C44 C45 58.2(8) . . . . ? C34 C35 C44 C46 114.3(6) . . . . ? C30 C35 C44 C46 -67.1(7) . . . . ? C34 C35 C44 C47 -1.9(8) . . . . ? C30 C35 C44 C47 176.6(5) . . . . ? Sm1 N14 C48 C49 -114.3(6) . . . . ? Sm1 N14 C48 C53 62.3(7) . . . . ? N14 C48 C49 C50 163.3(5) . . . . ? C53 C48 C49 C50 -13.4(8) . . . . ? N14 C48 C49 C54 -18.3(8) . . . . ? C53 C48 C49 C54 165.0(5) . . . . ? C48 C49 C50 C51 2.0(9) . . . . ? C54 C49 C50 C51 -176.5(6) . . . . ? C49 C50 C51 C52 8.1(9) . . . . ? C49 C50 C51 C58 -176.1(5) . . . . ? C50 C51 C52 C53 -6.5(9) . . . . ? C58 C51 C52 C53 177.7(5) . . . . ? C51 C52 C53 C48 -5.1(9) . . . . ? C51 C52 C53 C62 166.9(5) . . . . ? N14 C48 C53 C52 -162.0(5) . . . . ? C49 C48 C53 C52 14.9(8) . . . . ? N14 C48 C53 C62 26.3(8) . . . . ? C49 C48 C53 C62 -156.9(5) . . . . ? C50 C49 C54 C55 4.9(8) . . . . ? C48 C49 C54 C55 -173.5(6) . . . . ? C50 C49 C54 C56 122.4(6) . . . . ? C48 C49 C54 C56 -56.1(7) . . . . ? C50 C49 C54 C57 -114.2(6) . . . . ? C48 C49 C54 C57 67.4(7) . . . . ? C50 C51 C58 C61A -90.4(11) . . . . ? C52 C51 C58 C61A 85.3(10) . . . . ? C50 C51 C58 C61 -16.2(11) . . . . ? C52 C51 C58 C61 159.4(9) . . . . ? C50 C51 C58 C59 125.4(7) . . . . ? C52 C51 C58 C59 -58.9(9) . . . . ? C50 C51 C58 C60 -134.7(8) . . . . ? C52 C51 C58 C60 40.9(9) . . . . ? C50 C51 C58 C60A 23.3(10) . . . . ? C52 C51 C58 C60A -161.1(8) . . . . ? C52 C53 C62 C63 -109.5(6) . . . . ? C48 C53 C62 C63 62.2(7) . . . . ? C52 C53 C62 C65 129.2(6) . . . . ? C48 C53 C62 C65 -59.0(7) . . . . ? C52 C53 C62 C64 8.9(7) . . . . ? C48 C53 C62 C64 -179.3(5) . . . . ? N23 Sm2 N21 C102 63.2(6) . . . . ? N24 Sm2 N21 C102 -128.4(6) . . . . ? N22 Sm2 N21 C102 -32.3(6) . . . . ? N23 Sm2 N21 C106 -110.4(6) . . . . ? N24 Sm2 N21 C106 58.0(7) . . . . ? N22 Sm2 N21 C106 154.0(6) . . . . ? N23 Sm2 N22 C104 -63.7(5) . . . . ? N24 Sm2 N22 C104 156.6(5) . . . . ? N21 Sm2 N22 C104 31.5(5) . . . . ? N23 Sm2 N22 C118 107.6(4) . . . . ? N24 Sm2 N22 C118 -32.2(4) . . . . ? N21 Sm2 N22 C118 -157.3(4) . . . . ? N24 Sm2 N23 C130 5.1(11) . . . . ? N22 Sm2 N23 C130 -109.5(9) . . . . ? N21 Sm2 N23 C130 171.7(9) . . . . ? N23 Sm2 N24 C148 43.6(6) . . . . ? N22 Sm2 N24 C148 156.3(5) . . . . ? N21 Sm2 N24 C148 -119.7(5) . . . . ? C106 N21 C102 C103 -165.7(8) . . . . ? Sm2 N21 C102 C103 20.4(11) . . . . ? C106 N21 C102 C105 -3.4(14) . . . . ? Sm2 N21 C102 C105 -177.2(8) . . . . ? C106 N21 C102 C05A 26.6(11) . . . . ? Sm2 N21 C102 C05A -147.3(7) . . . . ? N21 C102 C103 C104 13.6(14) . . . . ? C105 C102 C103 C104 -150.8(9) . . . . ? C05A C102 C103 C104 -179.3(9) . . . . ? C118 N22 C104 C103 172.5(6) . . . . ? Sm2 N22 C104 C103 -16.4(9) . . . . ? C118 N22 C104 C101 -5.5(9) . . . . ? Sm2 N22 C104 C101 165.5(5) . . . . ? C102 C103 C104 N22 -16.9(13) . . . . ? C102 C103 C104 C101 161.2(8) . . . . ? C102 N21 C106 C111 90.5(8) . . . . ? Sm2 N21 C106 C111 -95.5(7) . . . . ? C102 N21 C106 C107 -93.6(9) . . . . ? Sm2 N21 C106 C107 80.4(8) . . . . ? C111 C106 C107 C112 -168.1(11) . . . . ? N21 C106 C107 C112 16.1(14) . . . . ? C111 C106 C107 C108 -8.8(12) . . . . ? N21 C106 C107 C108 175.4(8) . . . . ? C111 C106 C107 C08A 7.1(15) . . . . ? N21 C106 C107 C08A -168.7(10) . . . . ? C111 C106 C107 C12A 167.2(9) . . . . ? N21 C106 C107 C12A -8.6(13) . . . . ? C112 C107 C108 C109 170.8(17) . . . . ? C106 C107 C108 C109 15.0(19) . . . . ? C08A C107 C108 C109 -136(3) . . . . ? C12A C107 C108 C109 -161.1(15) . . . . ? C107 C108 C109 C110 -13(3) . . . . ? C108 C109 C110 C111 3(3) . . . . ? C112 C107 C08A C09A 161.6(14) . . . . ? C106 C107 C08A C09A -13.9(19) . . . . ? C108 C107 C08A C09A 22.2(18) . . . . ? C12A C107 C08A C09A -178.1(12) . . . . ? C107 C106 C111 C15A 168.6(11) . . . . ? N21 C106 C111 C15A -15.5(14) . . . . ? C107 C106 C111 C110 1.6(12) . . . . ? N21 C106 C111 C110 177.4(7) . . . . ? C107 C106 C111 C115 -167.8(9) . . . . ? N21 C106 C111 C115 8.0(11) . . . . ? C109 C110 C111 C15A -164.9(17) . . . . ? C109 C110 C111 C106 2(2) . . . . ? C109 C110 C111 C115 172.1(16) . . . . ? C106 C107 C112 C114 -133.2(11) . . . . ? C108 C107 C112 C114 73.5(19) . . . . ? C08A C107 C112 C114 50.8(16) . . . . ? C12A C107 C112 C114 -12(2) . . . . ? C106 C107 C112 C113 106.4(14) . . . . ? C108 C107 C112 C113 -47(2) . . . . ? C08A C107 C112 C113 -69.5(18) . . . . ? C12A C107 C112 C113 -133(3) . . . . ? C15A C111 C115 C116 -116(3) . . . . ? C106 C111 C115 C116 148.9(10) . . . . ? C110 C111 C115 C116 -20.6(15) . . . . ? C15A C111 C115 C117 5(3) . . . . ? C106 C111 C115 C117 -89.7(12) . . . . ? C110 C111 C115 C117 100.9(12) . . . . ? C112 C107 C12A C14A 168(4) . . . . ? C106 C107 C12A C14A -118.8(14) . . . . ? C108 C107 C12A C14A 56.4(17) . . . . ? C08A C107 C12A C14A 45.4(15) . . . . ? C112 C107 C12A C13A 39(2) . . . . ? C106 C107 C12A C13A 111.7(12) . . . . ? C108 C107 C12A C13A -73.1(16) . . . . ? C08A C107 C12A C13A -84.1(14) . . . . ? C106 C111 C15A C17A -99.6(15) . . . . ? C110 C111 C15A C17A 67.6(17) . . . . ? C115 C111 C15A C17A 163(4) . . . . ? C104 N22 C118 C119 -91.6(7) . . . . ? Sm2 N22 C118 C119 96.2(6) . . . . ? C104 N22 C118 C123 91.1(7) . . . . ? Sm2 N22 C118 C123 -81.1(6) . . . . ? C123 C118 C119 C120 -2.3(10) . . . . ? N22 C118 C119 C120 -179.6(6) . . . . ? C123 C118 C119 C124 -178.1(7) . . . . ? N22 C118 C119 C124 4.7(9) . . . . ? C118 C119 C120 C121 2.5(11) . . . . ? C124 C119 C120 C121 178.2(8) . . . . ? C119 C120 C121 C122 -2.3(13) . . . . ? C120 C121 C122 C123 2.0(13) . . . . ? C121 C122 C123 C118 -1.8(11) . . . . ? C121 C122 C123 C127 -179.4(7) . . . . ? C119 C118 C123 C122 1.9(9) . . . . ? N22 C118 C123 C122 179.2(6) . . . . ? C119 C118 C123 C127 179.4(6) . . . . ? N22 C118 C123 C127 -3.3(9) . . . . ? C118 C119 C124 C125 -123.1(8) . . . . ? C120 C119 C124 C125 61.3(11) . . . . ? C118 C119 C124 C126 121.9(8) . . . . ? C120 C119 C124 C126 -53.8(10) . . . . ? C122 C123 C127 C128 -61.1(9) . . . . ? C118 C123 C127 C128 121.5(8) . . . . ? C122 C123 C127 C129 64.9(9) . . . . ? C118 C123 C127 C129 -112.6(8) . . . . ? Sm2 N23 C130 C135 -27.9(13) . . . . ? Sm2 N23 C130 C131 150.4(7) . . . . ? C135 C130 C131 C132 9.4(9) . . . . ? N23 C130 C131 C132 -168.9(5) . . . . ? C135 C130 C131 C136 -169.3(6) . . . . ? N23 C130 C131 C136 12.4(9) . . . . ? C130 C131 C132 C133 -2.1(10) . . . . ? C136 C131 C132 C133 176.7(6) . . . . ? C131 C132 C133 C134 -4.0(10) . . . . ? C131 C132 C133 C140 177.9(6) . . . . ? C132 C133 C134 C135 2.8(10) . . . . ? C140 C133 C134 C135 -179.0(6) . . . . ? C133 C134 C135 C130 4.5(10) . . . . ? C133 C134 C135 C144 -173.8(6) . . . . ? N23 C130 C135 C134 167.8(5) . . . . ? C131 C130 C135 C134 -10.5(9) . . . . ? N23 C130 C135 C144 -14.0(9) . . . . ? C131 C130 C135 C144 167.6(6) . . . . ? C132 C131 C136 C138 109.7(7) . . . . ? C130 C131 C136 C138 -71.5(8) . . . . ? C132 C131 C136 C137 -125.5(6) . . . . ? C130 C131 C136 C137 53.3(8) . . . . ? C132 C131 C136 C139 -8.0(9) . . . . ? C130 C131 C136 C139 170.7(6) . . . . ? C132 C133 C140 C141 -115.4(8) . . . . ? C134 C133 C140 C141 66.6(9) . . . . ? C132 C133 C140 C142 5.7(10) . . . . ? C134 C133 C140 C142 -172.3(7) . . . . ? C132 C133 C140 C143 123.5(7) . . . . ? C134 C133 C140 C143 -54.5(8) . . . . ? C134 C135 C144 C147 130.0(6) . . . . ? C130 C135 C144 C147 -48.2(9) . . . . ? C134 C135 C144 C145 -106.8(7) . . . . ? C130 C135 C144 C145 75.0(8) . . . . ? C134 C135 C144 C146 12.5(9) . . . . ? C130 C135 C144 C146 -165.7(7) . . . . ? Sm2 N24 C148 C153 59.0(7) . . . . ? Sm2 N24 C148 C149 -118.0(5) . . . . ? N24 C148 C149 C150 160.0(5) . . . . ? C153 C148 C149 C150 -17.0(7) . . . . ? N24 C148 C149 C154 -20.8(8) . . . . ? C153 C148 C149 C154 162.2(5) . . . . ? C148 C149 C150 C151 4.5(8) . . . . ? C154 C149 C150 C151 -174.7(5) . . . . ? C149 C150 C151 C152 7.6(8) . . . . ? C149 C150 C151 C158 -174.1(5) . . . . ? C150 C151 C152 C153 -7.1(8) . . . . ? C158 C151 C152 C153 174.8(5) . . . . ? C151 C152 C153 C148 -5.8(8) . . . . ? C151 C152 C153 C162 167.5(5) . . . . ? N24 C148 C153 C152 -159.5(5) . . . . ? C149 C148 C153 C152 17.7(7) . . . . ? N24 C148 C153 C162 27.3(8) . . . . ? C149 C148 C153 C162 -155.5(5) . . . . ? C150 C149 C154 C157 12.0(8) . . . . ? C148 C149 C154 C157 -167.2(6) . . . . ? C150 C149 C154 C156 129.3(5) . . . . ? C148 C149 C154 C156 -49.9(7) . . . . ? C150 C149 C154 C155 -107.5(6) . . . . ? C148 C149 C154 C155 73.3(7) . . . . ? C152 C151 C158 C60B -101.6(11) . . . . ? C150 C151 C158 C60B 80.3(11) . . . . ? C152 C151 C158 C159 -11.2(11) . . . . ? C150 C151 C158 C159 170.8(9) . . . . ? C152 C151 C158 C161 124.5(7) . . . . ? C150 C151 C158 C161 -53.5(8) . . . . ? C152 C151 C158 C59A 16.1(10) . . . . ? C150 C151 C158 C59A -162.0(8) . . . . ? C152 C151 C158 C160 -129.7(8) . . . . ? C150 C151 C158 C160 52.2(8) . . . . ? C152 C153 C162 C163 122.8(6) . . . . ? C148 C153 C162 C163 -64.0(7) . . . . ? C152 C153 C162 C165 -116.2(6) . . . . ? C148 C153 C162 C165 57.0(7) . . . . ? C152 C153 C162 C164 1.5(7) . . . . ? C148 C153 C162 C164 174.7(5) . . . . ? C201 C202 C203 C204 178(4) . . . . ? C202 C203 C204 C205 165(2) . . . . ? C206 C207 C208 C207 -8(4) . . . 3_666 ? C208 C207 C208 C207 -0.008(2) 3_666 . . 3_666 ? C206 C207 C208 C208 -8(4) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 25.82 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 1.145 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.109