# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Peter Junk' 'Marcus L. Cole' 'Glen Deacon' 'Craig M Forsyth' 'Dorian C. Polo' 'Jun Wang.' _publ_contact_author_name 'Peter Junk' _publ_contact_author_email PETER.JUNK@SCI.MONASH.EDU.AU _publ_section_title ; Steric control of the reduction of carbodiimides by samarium(II) and the synthesis of very crowded samarium(III) complexes ; # Attachment '2_5_.3PhMe.CIF' data_jun1ab _database_code_depnum_ccdc_archive 'CCDC 752057' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C63 H93 N6 Sm), 3(C7 H8)' _chemical_formula_sum 'C147 H210 N12 Sm2' _chemical_formula_weight 2445.97 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 46.3055(3) _cell_length_b 13.4519(2) _cell_length_c 25.1741(1) _cell_angle_alpha 90.00 _cell_angle_beta 121.213(1) _cell_angle_gamma 90.00 _cell_volume 13411.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 20896 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5200 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KAPPA CCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method 'thin slice phi and omega scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51421 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0730 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 55 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.36 _reflns_number_total 12230 _reflns_number_gt 8560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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^)+(0.0341P)^2^+48.3841P] 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 12230 _refine_ls_number_parameters 748 _refine_ls_number_restraints 125 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.037 _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 0.140256(5) 0.371131(16) 0.176521(10) 0.02240(7) Uani 1 1 d . A . N1 N 0.15848(9) 0.2066(3) 0.21985(18) 0.0312(9) Uani 1 1 d . . . N2 N 0.16197(10) 0.2508(3) 0.13594(19) 0.0345(9) Uani 1 1 d . . . N3 N 0.08414(8) 0.3346(3) 0.15317(17) 0.0263(8) Uani 1 1 d . . . N4 N 0.08736(8) 0.4316(3) 0.08128(16) 0.0270(8) Uani 1 1 d . . . N5 N 0.18895(8) 0.4305(2) 0.27547(16) 0.0244(8) Uani 1 1 d . . . N6 N 0.15751(8) 0.5469(2) 0.20295(17) 0.0246(8) Uani 1 1 d . . . C1 C 0.16591(11) 0.1848(3) 0.1776(2) 0.0342(11) Uani 1 1 d . A . H1 H 0.1743 0.1206 0.1771 0.041 Uiso 1 1 calc R . . C2 C 0.17160(17) 0.2225(4) 0.0905(3) 0.0631(18) Uani 0.60 1 d P A 1 H2 H 0.1502 0.2070 0.0507 0.076 Uiso 0.60 1 calc PR A 1 C2' C 0.17160(17) 0.2225(4) 0.0905(3) 0.0631(18) Uani 0.40 1 d PD A 2 H2' H 0.1930 0.1868 0.1199 0.076 Uiso 0.40 1 calc PR A 2 C3 C 0.18727(18) 0.3098(5) 0.0780(3) 0.075(2) Uani 0.60 1 d P A 1 H3A H 0.2085 0.3252 0.1174 0.089 Uiso 0.60 1 calc PR A 1 H3B H 0.1720 0.3671 0.0689 0.089 Uiso 0.60 1 calc PR A 1 C3' C 0.18727(18) 0.3098(5) 0.0780(3) 0.075(2) Uani 0.40 1 d PD A 2 H3'1 H 0.2037 0.3442 0.1169 0.089 Uiso 0.40 1 calc PR A 2 H3'2 H 0.1700 0.3578 0.0494 0.089 Uiso 0.40 1 calc PR A 2 C4 C 0.1958(3) 0.3069(10) 0.0271(6) 0.077(4) Uani 0.60 1 d PU A 1 H4A H 0.1752 0.2978 -0.0143 0.092 Uiso 0.60 1 calc PR A 1 H4B H 0.2075 0.3684 0.0270 0.092 Uiso 0.60 1 calc PR A 1 C4' C 0.2053(5) 0.2583(16) 0.0470(9) 0.088(5) Uani 0.40 1 d PDU A 2 H4'1 H 0.2120 0.3111 0.0281 0.106 Uiso 0.40 1 calc PR A 2 H4'2 H 0.2264 0.2278 0.0806 0.106 Uiso 0.40 1 calc PR A 2 C5 C 0.2186(3) 0.2185(9) 0.0449(6) 0.064(3) Uani 0.60 1 d PU A 1 H5A H 0.2396 0.2325 0.0849 0.077 Uiso 0.60 1 calc PR A 1 H5B H 0.2249 0.2088 0.0132 0.077 Uiso 0.60 1 calc PR A 1 C5' C 0.1862(5) 0.1783(13) -0.0027(9) 0.093(4) Uani 0.40 1 d PDU A 2 H5'1 H 0.2028 0.1438 -0.0097 0.112 Uiso 0.40 1 calc PR A 2 H5'2 H 0.1702 0.2129 -0.0419 0.112 Uiso 0.40 1 calc PR A 2 C6 C 0.2032(3) 0.1226(7) 0.0512(5) 0.057(2) Uani 0.60 1 d PU A 1 H6A H 0.2195 0.0671 0.0630 0.068 Uiso 0.60 1 calc PR A 1 H6B H 0.1825 0.1059 0.0113 0.068 Uiso 0.60 1 calc PR A 1 C6' C 0.1663(5) 0.0982(11) 0.0084(8) 0.086(5) Uani 0.40 1 d PDU A 2 H6'1 H 0.1811 0.0399 0.0284 0.103 Uiso 0.40 1 calc PR A 2 H6'2 H 0.1470 0.0763 -0.0322 0.103 Uiso 0.40 1 calc PR A 2 C7 C 0.1945(2) 0.1400(6) 0.1030(4) 0.046(2) Uani 0.60 1 d PU A 1 H7A H 0.1842 0.0787 0.1077 0.055 Uiso 0.60 1 calc PR A 1 H7B H 0.2157 0.1523 0.1429 0.055 Uiso 0.60 1 calc PR A 1 C7' C 0.1526(4) 0.1345(9) 0.0496(6) 0.061(4) Uani 0.40 1 d PDU A 2 H7'1 H 0.1285 0.1530 0.0224 0.073 Uiso 0.40 1 calc PR A 2 H7'2 H 0.1537 0.0788 0.0763 0.073 Uiso 0.40 1 calc PR A 2 C8 C 0.16571(11) 0.1309(3) 0.2665(2) 0.0339(10) Uani 1 1 d . . . H8 H 0.1615 0.0644 0.2460 0.041 Uiso 1 1 calc R . . C9 C 0.14228(13) 0.1411(4) 0.2919(2) 0.0455(13) Uani 1 1 d . . . H9A H 0.1185 0.1382 0.2571 0.055 Uiso 1 1 calc R . . H9B H 0.1460 0.2065 0.3126 0.055 Uiso 1 1 calc R . . C10 C 0.14877(16) 0.0584(5) 0.3381(3) 0.0639(18) Uani 1 1 d . . . H10A H 0.1337 0.0673 0.3547 0.077 Uiso 1 1 calc R . . H10B H 0.1434 -0.0065 0.3165 0.077 Uiso 1 1 calc R . . C11 C 0.18482(17) 0.0583(5) 0.3909(3) 0.0666(18) Uani 1 1 d . . . H11A H 0.1886 0.0008 0.4183 0.080 Uiso 1 1 calc R . . H11B H 0.1893 0.1197 0.4157 0.080 Uiso 1 1 calc R . . C12 C 0.20902(14) 0.0524(4) 0.3677(3) 0.0576(16) Uani 1 1 d . . . H12A H 0.2069 -0.0136 0.3486 0.069 Uiso 1 1 calc R . . H12B H 0.2324 0.0591 0.4033 0.069 Uiso 1 1 calc R . . C13 C 0.20229(12) 0.1332(4) 0.3200(2) 0.0444(12) Uani 1 1 d . . . H13A H 0.2073 0.1991 0.3405 0.053 Uiso 1 1 calc R . . H13B H 0.2174 0.1234 0.3036 0.053 Uiso 1 1 calc R . . C14 C 0.06894(10) 0.3834(3) 0.0997(2) 0.0286(10) Uani 1 1 d . A . H14 H 0.0450 0.3840 0.0746 0.034 Uiso 1 1 calc R . . C15 C 0.06316(10) 0.2821(3) 0.1703(2) 0.0302(11) Uani 1 1 d . A . C16 C 0.05230(11) 0.1856(3) 0.1486(2) 0.0392(12) Uani 1 1 d . . . C17 C 0.03228(14) 0.1372(4) 0.1666(3) 0.0604(16) Uani 1 1 d . A . H17 H 0.0244 0.0719 0.1519 0.072 Uiso 1 1 calc R . . C18 C 0.02373(15) 0.1829(5) 0.2056(3) 0.0690(19) Uani 1 1 d . . . H18 H 0.0101 0.1487 0.2178 0.083 Uiso 1 1 calc R A . C19 C 0.03479(13) 0.2776(5) 0.2270(3) 0.0560(16) Uani 1 1 d . A . H19 H 0.0287 0.3083 0.2539 0.067 Uiso 1 1 calc R . . C20 C 0.05465(11) 0.3288(4) 0.2099(2) 0.0378(12) Uani 1 1 d . . . C21 C 0.06043(12) 0.1331(4) 0.1043(3) 0.0479(13) Uani 1 1 d . A . H21 H 0.0775 0.1744 0.1012 0.057 Uiso 1 1 calc R . . C22 C 0.07575(19) 0.0290(5) 0.1267(3) 0.096(3) Uani 1 1 d . . . H22A H 0.0960 0.0340 0.1682 0.145 Uiso 1 1 calc R A . H22B H 0.0818 0.0009 0.0978 0.145 Uiso 1 1 calc R . . H22C H 0.0592 -0.0142 0.1284 0.145 Uiso 1 1 calc R . . C23 C 0.02891(13) 0.1278(4) 0.0399(3) 0.0581(15) Uani 1 1 d . . . H23A H 0.0343 0.0948 0.0114 0.087 Uiso 1 1 calc R A . H23B H 0.0207 0.1953 0.0249 0.087 Uiso 1 1 calc R . . H23C H 0.0114 0.0901 0.0418 0.087 Uiso 1 1 calc R . . C24 C 0.06716(12) 0.4331(4) 0.2338(3) 0.0428(13) Uani 1 1 d . A . H24 H 0.0686 0.4687 0.2004 0.051 Uiso 1 1 calc R . . C25 C 0.10226(14) 0.4306(5) 0.2896(3) 0.079(2) Uani 1 1 d . . . H25A H 0.1100 0.4986 0.3037 0.119 Uiso 1 1 calc R A . H25B H 0.1175 0.3985 0.2786 0.119 Uiso 1 1 calc R . . H25C H 0.1023 0.3930 0.3230 0.119 Uiso 1 1 calc R . . C26 C 0.04380(14) 0.4941(5) 0.2468(3) 0.0582(16) Uani 1 1 d . . . H26A H 0.0534 0.5606 0.2610 0.087 Uiso 1 1 calc R A . H26B H 0.0414 0.4613 0.2790 0.087 Uiso 1 1 calc R . . H26C H 0.0216 0.4998 0.2087 0.087 Uiso 1 1 calc R . . C27 C 0.06979(10) 0.4890(3) 0.0259(2) 0.0302(11) Uani 1 1 d . A . C28 C 0.06946(11) 0.4559(4) -0.0275(2) 0.0349(12) Uani 1 1 d . . . C29 C 0.05162(12) 0.5120(4) -0.0819(2) 0.0435(13) Uani 1 1 d . A . H29 H 0.0508 0.4903 -0.1186 0.052 Uiso 1 1 calc R . . C30 C 0.03530(12) 0.5980(4) -0.0832(3) 0.0486(14) Uani 1 1 d . . . H30 H 0.0229 0.6343 -0.1208 0.058 Uiso 1 1 calc R A . C31 C 0.03674(11) 0.6316(4) -0.0305(2) 0.0418(12) Uani 1 1 d . A . H31 H 0.0258 0.6921 -0.0319 0.050 Uiso 1 1 calc R . . C32 C 0.05394(10) 0.5790(3) 0.0252(2) 0.0331(11) Uani 1 1 d . . . C33 C 0.08682(12) 0.3594(4) -0.0267(2) 0.0433(12) Uani 1 1 d . A . H33 H 0.1074 0.3521 0.0156 0.052 Uiso 1 1 calc R . . C34 C 0.06392(17) 0.2705(4) -0.0375(3) 0.0669(18) Uani 1 1 d . . . H34A H 0.0757 0.2090 -0.0360 0.100 Uiso 1 1 calc R A . H34B H 0.0432 0.2765 -0.0783 0.100 Uiso 1 1 calc R . . H34C H 0.0581 0.2688 -0.0052 0.100 Uiso 1 1 calc R . . C35 C 0.09829(15) 0.3556(5) -0.0742(3) 0.0640(17) Uani 1 1 d . . . H35A H 0.1096 0.2921 -0.0704 0.096 Uiso 1 1 calc R A . H35B H 0.1140 0.4103 -0.0661 0.096 Uiso 1 1 calc R . . H35C H 0.0786 0.3621 -0.1163 0.096 Uiso 1 1 calc R . . C36 C 0.05470(10) 0.6193(3) 0.0827(2) 0.0340(11) Uani 1 1 d . A . H36 H 0.0739 0.5867 0.1199 0.041 Uiso 1 1 calc R . . C37 C 0.02230(12) 0.5954(4) 0.0823(3) 0.0450(13) Uani 1 1 d . . . H37A H 0.0240 0.6217 0.1201 0.068 Uiso 1 1 calc R A . H37B H 0.0192 0.5231 0.0807 0.068 Uiso 1 1 calc R . . H37C H 0.0030 0.6259 0.0458 0.068 Uiso 1 1 calc R . . C38 C 0.06061(12) 0.7327(3) 0.0898(3) 0.0432(13) Uani 1 1 d . . . H38A H 0.0814 0.7488 0.0905 0.065 Uiso 1 1 calc R A . H38B H 0.0626 0.7546 0.1287 0.065 Uiso 1 1 calc R . . H38C H 0.0415 0.7667 0.0548 0.065 Uiso 1 1 calc R . . C39 C 0.18508(10) 0.5227(3) 0.2556(2) 0.0251(10) Uani 1 1 d . A . H39 H 0.2019 0.5712 0.2789 0.030 Uiso 1 1 calc R . . C40 C 0.22006(10) 0.4017(3) 0.3296(2) 0.0252(10) Uani 1 1 d . A . C41 C 0.22240(11) 0.3992(3) 0.3876(2) 0.0328(11) Uani 1 1 d . . . C42 C 0.25247(11) 0.3669(4) 0.4391(2) 0.0401(11) Uani 1 1 d . A . H42 H 0.2541 0.3636 0.4783 0.048 Uiso 1 1 calc R . . C43 C 0.27988(12) 0.3396(4) 0.4349(2) 0.0409(12) Uani 1 1 d . . . H43 H 0.3003 0.3187 0.4708 0.049 Uiso 1 1 calc R A . C44 C 0.27704(11) 0.3431(3) 0.3778(2) 0.0378(12) Uani 1 1 d . A . H44 H 0.2961 0.3254 0.3750 0.045 Uiso 1 1 calc R . . C45 C 0.24751(10) 0.3715(3) 0.3241(2) 0.0277(9) Uani 1 1 d . . . C46 C 0.19370(13) 0.4348(4) 0.3955(2) 0.0473(14) Uani 1 1 d . A . H46 H 0.1731 0.4410 0.3531 0.057 Uiso 1 1 calc R . . C47 C 0.18551(16) 0.3621(5) 0.4322(3) 0.0664(17) Uani 1 1 d . . . H47A H 0.1669 0.3884 0.4358 0.100 Uiso 1 1 calc R A . H47B H 0.2055 0.3532 0.4737 0.100 Uiso 1 1 calc R . . H47C H 0.1789 0.2980 0.4106 0.100 Uiso 1 1 calc R . . C48 C 0.20164(17) 0.5367(5) 0.4248(3) 0.075(2) Uani 1 1 d . . . H48A H 0.1830 0.5592 0.4295 0.113 Uiso 1 1 calc R A . H48B H 0.2047 0.5834 0.3982 0.113 Uiso 1 1 calc R . . H48C H 0.2224 0.5337 0.4657 0.113 Uiso 1 1 calc R . . C49 C 0.24618(10) 0.3713(3) 0.2628(2) 0.0314(10) Uani 1 1 d . A . H49 H 0.2220 0.3775 0.2290 0.038 Uiso 1 1 calc R . . C50 C 0.25985(12) 0.2748(3) 0.2518(2) 0.0397(12) Uani 1 1 d . . . H50A H 0.2582 0.2781 0.2114 0.060 Uiso 1 1 calc R A . H50B H 0.2465 0.2185 0.2521 0.060 Uiso 1 1 calc R . . H50C H 0.2835 0.2662 0.2847 0.060 Uiso 1 1 calc R . . C51 C 0.26518(13) 0.4608(4) 0.2581(3) 0.0440(13) Uani 1 1 d . . . H51A H 0.2560 0.5221 0.2645 0.066 Uiso 1 1 calc R A . H51B H 0.2625 0.4620 0.2169 0.066 Uiso 1 1 calc R . . H51C H 0.2892 0.4554 0.2899 0.066 Uiso 1 1 calc R . . C52 C 0.15228(10) 0.6480(3) 0.1837(2) 0.0263(10) Uani 1 1 d . A . C53 C 0.14886(10) 0.7219(3) 0.2198(2) 0.0331(11) Uani 1 1 d . . . C54 C 0.14429(11) 0.8213(3) 0.1991(3) 0.0371(12) Uani 1 1 d . A . H54 H 0.1426 0.8723 0.2235 0.045 Uiso 1 1 calc R . . C55 C 0.14223(11) 0.8451(3) 0.1448(3) 0.0401(13) Uani 1 1 d . . . H55 H 0.1393 0.9125 0.1318 0.048 Uiso 1 1 calc R A . C56 C 0.14426(10) 0.7722(3) 0.1081(2) 0.0364(12) Uani 1 1 d . A . H56 H 0.1420 0.7897 0.0696 0.044 Uiso 1 1 calc R . . C57 C 0.14959(10) 0.6728(3) 0.1272(2) 0.0287(10) Uani 1 1 d . . . C58 C 0.14909(12) 0.7006(3) 0.2796(2) 0.0395(12) Uani 1 1 d . A . H58 H 0.1548 0.6287 0.2897 0.047 Uiso 1 1 calc R . . C59 C 0.11375(14) 0.7174(5) 0.2697(3) 0.0615(17) Uani 1 1 d . . . H59A H 0.1142 0.7027 0.3082 0.092 Uiso 1 1 calc R A . H59B H 0.0975 0.6734 0.2366 0.092 Uiso 1 1 calc R . . H59C H 0.1070 0.7868 0.2578 0.092 Uiso 1 1 calc R . . C60 C 0.17553(15) 0.7608(4) 0.3345(3) 0.0604(16) Uani 1 1 d . . . H60A H 0.1749 0.7434 0.3717 0.091 Uiso 1 1 calc R A . H60B H 0.1707 0.8319 0.3257 0.091 Uiso 1 1 calc R . . H60C H 0.1980 0.7461 0.3414 0.091 Uiso 1 1 calc R . . C61 C 0.15461(11) 0.5939(3) 0.0895(2) 0.0338(11) Uani 1 1 d . A . H61 H 0.1444 0.5308 0.0932 0.041 Uiso 1 1 calc R . . C62 C 0.19202(12) 0.5745(4) 0.1156(3) 0.0450(13) Uani 1 1 d . . . H62A H 0.1946 0.5230 0.0908 0.067 Uiso 1 1 calc R A . H62B H 0.2026 0.5521 0.1588 0.067 Uiso 1 1 calc R . . H62C H 0.2029 0.6359 0.1140 0.067 Uiso 1 1 calc R . . C63 C 0.13729(13) 0.6192(4) 0.0200(2) 0.0472(13) Uani 1 1 d . . . H63A H 0.1413 0.5655 -0.0017 0.071 Uiso 1 1 calc R A . H63B H 0.1465 0.6815 0.0149 0.071 Uiso 1 1 calc R . . H63C H 0.1129 0.6267 0.0026 0.071 Uiso 1 1 calc R . . C64 C 0.0937(2) -0.1536(6) -0.0762(3) 0.052(2) Uiso 0.60 1 d PD B 1 C64' C 0.0783(2) -0.1323(11) -0.1127(5) 0.078(5) Uiso 0.40 1 d PD C 2 C65 C 0.1203(3) -0.0828(7) -0.0435(4) 0.078(3) Uiso 0.60 1 d PD B 1 H65 H 0.1393 -0.0838 -0.0484 0.094 Uiso 0.60 1 calc PR B 1 C65' C 0.0679(3) -0.0479(10) -0.1502(6) 0.069(4) Uiso 0.40 1 d PD C 2 H65' H 0.0725 -0.0410 -0.1827 0.083 Uiso 0.40 1 calc PR C 2 C66 C 0.1186(3) -0.0135(7) -0.0052(4) 0.079(3) Uiso 0.60 1 d PD B 1 H66 H 0.1367 0.0323 0.0158 0.095 Uiso 0.60 1 calc PR B 1 C66' C 0.0514(3) 0.0226(11) -0.1398(7) 0.085(5) Uiso 0.40 1 d PD C 2 H66' H 0.0444 0.0797 -0.1657 0.103 Uiso 0.40 1 calc PR C 2 C67 C 0.0920(3) -0.0074(8) 0.0041(5) 0.088(4) Uiso 0.60 1 d PD B 1 H67 H 0.0916 0.0383 0.0324 0.106 Uiso 0.60 1 calc PR B 1 C67' C 0.0437(3) 0.0189(12) -0.0949(7) 0.099(6) Uiso 0.40 1 d PD C 2 H67' H 0.0317 0.0704 -0.0887 0.119 Uiso 0.40 1 calc PR C 2 C68 C 0.0664(3) -0.0713(8) -0.0301(6) 0.078(4) Uiso 0.60 1 d PD B 1 H68 H 0.0459 -0.0670 -0.0302 0.094 Uiso 0.60 1 calc PR B 1 C68' C 0.0544(3) -0.0630(11) -0.0599(8) 0.090(7) Uiso 0.40 1 d PD C 2 H68' H 0.0494 -0.0657 -0.0277 0.108 Uiso 0.40 1 calc PR C 2 C69 C 0.07049(15) -0.1397(5) -0.0632(3) 0.0710(18) Uiso 0.60 1 d PD B 1 H69 H 0.0530 -0.1880 -0.0807 0.085 Uiso 0.60 1 calc PR B 1 C69' C 0.07049(15) -0.1397(5) -0.0632(3) 0.0710(18) Uiso 0.40 1 d PD C 2 H69' H 0.0766 -0.1953 -0.0361 0.085 Uiso 0.40 1 calc PR C 2 C70 C 0.0969(2) -0.2208(7) -0.1143(4) 0.124(3) Uiso 0.60 1 d PD B 1 H70A H 0.0873 -0.2849 -0.1127 0.186 Uiso 0.60 1 calc PR B 1 H70B H 0.1209 -0.2294 -0.1001 0.186 Uiso 0.60 1 calc PR B 1 H70C H 0.0849 -0.1959 -0.1571 0.186 Uiso 0.60 1 calc PR B 1 C70' C 0.0969(2) -0.2208(7) -0.1143(4) 0.124(3) Uiso 0.40 1 d PD C 2 H70D H 0.1174 -0.2301 -0.0735 0.186 Uiso 0.40 1 calc PR C 2 H70E H 0.1032 -0.2112 -0.1456 0.186 Uiso 0.40 1 calc PR C 2 H70F H 0.0825 -0.2797 -0.1248 0.186 Uiso 0.40 1 calc PR C 2 C71 C 0.0366(3) 0.1175(10) -0.2045(5) 0.099(5) Uiso 0.50 1 d PD D -1 C72 C 0.0247(4) 0.2036(11) -0.2439(7) 0.101(5) Uiso 0.50 1 d PD D -1 H72 H 0.0359 0.2244 -0.2647 0.122 Uiso 0.50 1 calc PR D -1 C73 C -0.0020(5) 0.2548(9) -0.2518(10) 0.098(4) Uiso 0.50 1 d PD D -1 H73 H -0.0093 0.3113 -0.2783 0.118 Uiso 0.50 1 calc PR D -1 C74 C -0.0192(4) 0.2280(12) -0.2224(8) 0.113(6) Uiso 0.50 1 d PD D -1 H74 H -0.0379 0.2661 -0.2286 0.136 Uiso 0.50 1 calc PR D -1 C75 C -0.0093(4) 0.1487(12) -0.1855(7) 0.130(7) Uiso 0.50 1 d PD D -1 H75 H -0.0207 0.1289 -0.1649 0.156 Uiso 0.50 1 calc PR D -1 C76 C 0.0189(3) 0.0949(10) -0.1779(6) 0.086(4) Uiso 0.50 1 d PD D -1 H76 H 0.0258 0.0380 -0.1518 0.103 Uiso 0.50 1 calc PR D -1 C77 C 0.0653(4) 0.0600(11) -0.1941(7) 0.101(5) Uiso 0.50 1 d PD D -1 H77A H 0.0732 0.0188 -0.1569 0.151 Uiso 0.50 1 calc PR D -1 H77B H 0.0834 0.1049 -0.1882 0.151 Uiso 0.50 1 calc PR D -1 H77C H 0.0587 0.0172 -0.2301 0.151 Uiso 0.50 1 calc PR D -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01595(11) 0.02366(12) 0.02426(12) 0.00134(12) 0.00807(9) 0.00030(11) N1 0.036(2) 0.025(2) 0.033(2) -0.0010(17) 0.018(2) 0.0043(17) N2 0.040(2) 0.035(2) 0.040(3) -0.0070(19) 0.028(2) -0.0015(18) N3 0.0178(18) 0.0282(19) 0.034(2) 0.0024(16) 0.0139(18) -0.0015(15) N4 0.0157(18) 0.034(2) 0.023(2) 0.0022(17) 0.0044(17) -0.0001(16) N5 0.0183(18) 0.024(2) 0.024(2) 0.0012(16) 0.0058(17) 0.0008(15) N6 0.0165(19) 0.0229(19) 0.030(2) 0.0034(16) 0.0091(18) -0.0005(15) C1 0.028(3) 0.028(3) 0.044(3) -0.002(2) 0.017(2) 0.002(2) C2 0.093(5) 0.051(4) 0.075(5) -0.017(3) 0.064(4) -0.012(3) C2' 0.093(5) 0.051(4) 0.075(5) -0.017(3) 0.064(4) -0.012(3) C3 0.083(5) 0.099(5) 0.060(4) 0.007(4) 0.050(4) -0.012(4) C3' 0.083(5) 0.099(5) 0.060(4) 0.007(4) 0.050(4) -0.012(4) C4 0.079(8) 0.103(9) 0.060(7) 0.036(6) 0.044(6) 0.002(7) C4' 0.103(11) 0.125(13) 0.060(9) 0.026(9) 0.060(9) 0.005(10) C5 0.082(7) 0.086(7) 0.054(6) 0.012(5) 0.057(5) 0.004(6) C5' 0.111(9) 0.122(10) 0.075(8) -0.003(8) 0.068(7) 0.016(8) C6 0.062(5) 0.061(5) 0.065(6) 0.009(5) 0.045(5) 0.015(5) C6' 0.124(10) 0.070(9) 0.071(9) -0.004(7) 0.055(8) 0.021(8) C7 0.056(5) 0.045(5) 0.042(5) 0.004(4) 0.028(4) 0.009(4) C7' 0.096(9) 0.052(7) 0.049(7) -0.006(7) 0.048(7) 0.020(7) C8 0.036(3) 0.023(2) 0.037(3) 0.005(2) 0.015(2) 0.006(2) C9 0.051(3) 0.047(3) 0.044(3) 0.006(3) 0.028(3) 0.012(3) C10 0.082(5) 0.064(4) 0.064(4) 0.025(3) 0.051(4) 0.030(3) C11 0.091(5) 0.055(4) 0.051(4) 0.016(3) 0.035(4) 0.023(4) C12 0.048(3) 0.050(3) 0.049(4) 0.015(3) 0.006(3) 0.012(3) C13 0.040(3) 0.028(2) 0.049(3) 0.004(3) 0.011(3) 0.002(2) C14 0.018(2) 0.028(2) 0.033(3) 0.001(2) 0.008(2) 0.0021(19) C15 0.020(2) 0.034(3) 0.034(3) 0.007(2) 0.012(2) 0.0022(19) C16 0.023(2) 0.035(3) 0.049(3) 0.004(2) 0.011(2) -0.002(2) C17 0.045(3) 0.049(3) 0.076(4) 0.014(3) 0.023(3) -0.013(3) C18 0.052(4) 0.089(5) 0.070(5) 0.019(4) 0.035(4) -0.024(4) C19 0.040(3) 0.085(5) 0.050(4) 0.005(3) 0.029(3) -0.011(3) C20 0.022(2) 0.049(3) 0.041(3) 0.002(2) 0.015(2) -0.002(2) C21 0.027(3) 0.037(3) 0.064(4) -0.001(3) 0.012(3) 0.000(2) C22 0.089(5) 0.054(4) 0.084(6) -0.012(4) 0.000(4) 0.034(4) C23 0.038(3) 0.062(4) 0.064(4) 0.001(3) 0.020(3) 0.000(3) C24 0.031(3) 0.055(3) 0.046(3) -0.006(3) 0.023(3) 0.000(2) C25 0.033(3) 0.062(4) 0.100(6) -0.014(4) 0.005(4) 0.000(3) C26 0.042(3) 0.082(4) 0.054(4) -0.017(3) 0.027(3) 0.005(3) C27 0.017(2) 0.037(3) 0.028(3) 0.005(2) 0.005(2) -0.0051(19) C28 0.021(2) 0.045(3) 0.029(3) 0.007(2) 0.006(2) -0.005(2) C29 0.033(3) 0.063(4) 0.027(3) 0.008(3) 0.011(2) -0.004(3) C30 0.032(3) 0.058(4) 0.034(3) 0.018(3) 0.001(3) -0.006(2) C31 0.025(2) 0.042(3) 0.042(3) 0.013(3) 0.006(2) 0.004(2) C32 0.016(2) 0.037(3) 0.034(3) 0.007(2) 0.005(2) -0.004(2) C33 0.038(3) 0.058(3) 0.030(3) 0.001(3) 0.015(2) 0.004(3) C34 0.082(5) 0.048(4) 0.086(5) -0.005(3) 0.055(4) 0.001(3) C35 0.056(4) 0.098(5) 0.042(4) 0.005(3) 0.029(3) 0.012(3) C36 0.020(2) 0.037(3) 0.038(3) 0.007(2) 0.010(2) 0.006(2) C37 0.035(3) 0.042(3) 0.058(4) -0.001(3) 0.024(3) -0.004(2) C38 0.026(3) 0.034(3) 0.061(4) 0.002(3) 0.017(3) 0.000(2) C39 0.012(2) 0.028(2) 0.032(3) 0.001(2) 0.009(2) 0.0005(18) C40 0.022(2) 0.017(2) 0.028(3) -0.0020(17) 0.007(2) -0.0027(17) C41 0.025(2) 0.038(3) 0.027(3) 0.000(2) 0.007(2) -0.0011(19) C42 0.033(3) 0.051(3) 0.027(3) 0.000(3) 0.009(2) -0.004(3) C43 0.029(3) 0.045(3) 0.033(3) 0.005(2) 0.005(2) 0.006(2) C44 0.023(2) 0.044(3) 0.038(3) 0.000(2) 0.010(2) 0.008(2) C45 0.020(2) 0.025(2) 0.031(2) 0.004(2) 0.009(2) 0.000(2) C46 0.030(3) 0.077(4) 0.029(3) 0.000(3) 0.012(2) 0.006(3) C47 0.064(4) 0.086(5) 0.066(4) -0.007(4) 0.046(4) -0.006(4) C48 0.070(4) 0.067(4) 0.098(6) 0.002(4) 0.051(4) 0.028(4) C49 0.020(2) 0.037(2) 0.034(3) 0.006(2) 0.012(2) 0.003(2) C50 0.035(3) 0.043(3) 0.041(3) 0.002(2) 0.020(3) 0.001(2) C51 0.041(3) 0.041(3) 0.051(4) 0.006(3) 0.024(3) -0.002(2) C52 0.015(2) 0.019(2) 0.037(3) 0.0017(19) 0.008(2) -0.0012(16) C53 0.015(2) 0.029(3) 0.050(3) -0.001(2) 0.013(2) -0.0004(19) C54 0.026(3) 0.020(2) 0.061(4) 0.000(2) 0.019(3) 0.0012(19) C55 0.025(3) 0.022(3) 0.066(4) 0.011(2) 0.018(3) 0.0030(18) C56 0.016(2) 0.036(3) 0.049(3) 0.015(2) 0.010(2) 0.000(2) C57 0.014(2) 0.028(2) 0.037(3) 0.007(2) 0.008(2) -0.0023(18) C58 0.038(3) 0.027(2) 0.052(3) -0.003(2) 0.023(3) 0.001(2) C59 0.045(3) 0.080(4) 0.068(4) 0.012(3) 0.035(3) 0.015(3) C60 0.068(4) 0.043(3) 0.058(4) -0.009(3) 0.024(3) -0.007(3) C61 0.031(3) 0.031(2) 0.033(3) 0.005(2) 0.012(2) -0.008(2) C62 0.043(3) 0.034(3) 0.057(4) 0.004(3) 0.025(3) 0.008(2) C63 0.043(3) 0.056(3) 0.041(3) 0.007(3) 0.021(3) -0.014(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 N2 2.395(4) . ? Sm1 N3 2.399(3) . ? Sm1 N1 2.418(4) . ? Sm1 N5 2.471(3) . ? Sm1 N6 2.475(3) . ? Sm1 N4 2.514(3) . ? Sm1 C1 2.767(5) . ? Sm1 C14 2.838(4) . ? Sm1 C39 2.854(4) . ? N1 C1 1.310(6) . ? N1 C8 1.457(6) . ? N2 C1 1.312(6) . ? N2 C2 1.478(6) . ? N3 C14 1.325(5) . ? N3 C15 1.436(5) . ? N4 C14 1.331(5) . ? N4 C27 1.424(5) . ? N5 C39 1.314(5) . ? N5 C40 1.431(5) . ? N6 C39 1.319(5) . ? N6 C52 1.421(5) . ? C2 C7 1.452(10) . ? C2 C3 1.496(8) . ? C3 C4 1.523(13) . ? C4 C5 1.497(17) . ? C4' C5' 1.537(10) . ? C5 C6 1.521(15) . ? C5' C6' 1.537(10) . ? C6 C7 1.570(12) . ? C6' C7' 1.548(9) . ? C8 C13 1.523(6) . ? C8 C9 1.523(6) . ? C9 C10 1.524(7) . ? C10 C11 1.501(8) . ? C11 C12 1.511(8) . ? C12 C13 1.526(7) . ? C15 C16 1.396(6) . ? C15 C20 1.397(6) . ? C16 C17 1.388(7) . ? C16 C21 1.521(7) . ? C17 C18 1.379(9) . ? C18 C19 1.375(9) . ? C19 C20 1.385(7) . ? C20 C24 1.518(7) . ? C21 C23 1.521(7) . ? C21 C22 1.538(7) . ? C24 C25 1.500(7) . ? C24 C26 1.523(7) . ? C27 C28 1.410(7) . ? C27 C32 1.411(6) . ? C28 C29 1.398(7) . ? C28 C33 1.522(7) . ? C29 C30 1.373(7) . ? C30 C31 1.369(7) . ? C31 C32 1.393(6) . ? C32 C36 1.528(7) . ? C33 C34 1.527(7) . ? C33 C35 1.540(7) . ? C36 C37 1.530(6) . ? C36 C38 1.544(6) . ? C40 C41 1.407(6) . ? C40 C45 1.408(6) . ? C41 C42 1.392(6) . ? C41 C46 1.519(6) . ? C42 C43 1.377(6) . ? C43 C44 1.376(7) . ? C44 C45 1.388(6) . ? C45 C49 1.511(6) . ? C46 C48 1.510(8) . ? C46 C47 1.522(8) . ? C49 C50 1.530(6) . ? C49 C51 1.531(6) . ? C52 C57 1.403(6) . ? C52 C53 1.411(6) . ? C53 C54 1.410(6) . ? C53 C58 1.526(7) . ? C54 C55 1.358(7) . ? C55 C56 1.384(7) . ? C56 C57 1.398(6) . ? C57 C61 1.520(7) . ? C58 C60 1.521(7) . ? C58 C59 1.539(7) . ? C61 C62 1.523(6) . ? C61 C63 1.537(7) . ? C64 C69 1.289(9) . ? C64 C70 1.381(12) . ? C64 C65 1.433(11) . ? C64' C65' 1.394(15) . ? C65 C66 1.372(12) . ? C65' C66' 1.327(15) . ? C66 C67 1.370(12) . ? C66' C67' 1.348(15) . ? C67 C68 1.351(13) . ? C67' C68' 1.335(16) . ? C68 C69 1.319(11) . ? C71 C76 1.332(14) . ? C71 C72 1.437(15) . ? C71 C77 1.439(19) . ? C72 C73 1.334(16) . ? C73 C74 1.387(17) . ? C74 C75 1.330(15) . ? C75 C76 1.417(14) . ? 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 N3 113.44(12) . . ? N2 Sm1 N1 56.53(13) . . ? N3 Sm1 N1 90.20(12) . . ? N2 Sm1 N5 106.43(12) . . ? N3 Sm1 N5 128.31(12) . . ? N1 Sm1 N5 85.32(12) . . ? N2 Sm1 N6 127.73(12) . . ? N3 Sm1 N6 114.80(11) . . ? N1 Sm1 N6 139.91(12) . . ? N5 Sm1 N6 54.63(11) . . ? N2 Sm1 N4 103.21(13) . . ? N3 Sm1 N4 55.69(12) . . ? N1 Sm1 N4 131.75(12) . . ? N5 Sm1 N4 141.80(11) . . ? N6 Sm1 N4 88.09(11) . . ? N2 Sm1 C1 28.29(13) . . ? N3 Sm1 C1 102.82(12) . . ? N1 Sm1 C1 28.25(13) . . ? N5 Sm1 C1 96.90(12) . . ? N6 Sm1 C1 141.78(12) . . ? N4 Sm1 C1 120.21(13) . . ? N2 Sm1 C14 110.25(13) . . ? N3 Sm1 C14 27.73(12) . . ? N1 Sm1 C14 111.81(12) . . ? N5 Sm1 C14 143.12(12) . . ? N6 Sm1 C14 103.13(11) . . ? N4 Sm1 C14 27.97(11) . . ? C1 Sm1 C14 113.67(13) . . ? N2 Sm1 C39 117.77(12) . . ? N3 Sm1 C39 128.39(11) . . ? N1 Sm1 C39 112.43(12) . . ? N5 Sm1 C39 27.38(11) . . ? N6 Sm1 C39 27.50(11) . . ? N4 Sm1 C39 115.54(11) . . ? C1 Sm1 C39 119.13(12) . . ? C14 Sm1 C39 127.06(11) . . ? C1 N1 C8 116.9(4) . . ? C1 N1 Sm1 90.9(3) . . ? C8 N1 Sm1 152.2(3) . . ? C1 N2 C2 118.1(4) . . ? C1 N2 Sm1 91.8(3) . . ? C2 N2 Sm1 150.0(3) . . ? C14 N3 C15 117.6(3) . . ? C14 N3 Sm1 94.9(2) . . ? C15 N3 Sm1 147.4(3) . . ? C14 N4 C27 117.4(3) . . ? C14 N4 Sm1 89.7(3) . . ? C27 N4 Sm1 152.8(3) . . ? C39 N5 C40 119.3(3) . . ? C39 N5 Sm1 92.8(3) . . ? C40 N5 Sm1 144.6(3) . . ? C39 N6 C52 119.0(4) . . ? C39 N6 Sm1 92.5(2) . . ? C52 N6 Sm1 148.0(3) . . ? N1 C1 N2 120.8(4) . . ? N1 C1 Sm1 60.9(2) . . ? N2 C1 Sm1 59.9(2) . . ? C7 C2 N2 120.6(6) . . ? C7 C2 C3 105.4(6) . . ? N2 C2 C3 109.5(5) . . ? C2 C3 C4 121.4(8) . . ? C5 C4 C3 102.7(8) . . ? C4 C5 C6 114.1(9) . . ? C4' C5' C6' 119.3(15) . . ? C5 C6 C7 107.2(8) . . ? C5' C6' C7' 113.2(12) . . ? C2 C7 C6 114.0(7) . . ? N1 C8 C13 112.6(4) . . ? N1 C8 C9 111.0(4) . . ? C13 C8 C9 109.6(4) . . ? C8 C9 C10 110.6(4) . . ? C11 C10 C9 111.5(5) . . ? C10 C11 C12 111.4(5) . . ? C11 C12 C13 112.1(5) . . ? C8 C13 C12 111.2(4) . . ? N3 C14 N4 119.7(4) . . ? N3 C14 Sm1 57.4(2) . . ? N4 C14 Sm1 62.4(2) . . ? C16 C15 C20 121.3(4) . . ? C16 C15 N3 120.1(4) . . ? C20 C15 N3 118.5(4) . . ? C17 C16 C15 118.3(5) . . ? C17 C16 C21 118.8(5) . . ? C15 C16 C21 122.9(4) . . ? C18 C17 C16 120.8(5) . . ? C19 C18 C17 120.4(5) . . ? C18 C19 C20 120.8(6) . . ? C19 C20 C15 118.5(5) . . ? C19 C20 C24 121.0(5) . . ? C15 C20 C24 120.5(4) . . ? C23 C21 C16 109.7(4) . . ? C23 C21 C22 110.7(5) . . ? C16 C21 C22 113.4(5) . . ? C25 C24 C20 110.9(4) . . ? C25 C24 C26 110.9(5) . . ? C20 C24 C26 114.6(4) . . ? C28 C27 C32 120.6(4) . . ? C28 C27 N4 118.8(4) . . ? C32 C27 N4 120.6(4) . . ? C29 C28 C27 118.2(5) . . ? C29 C28 C33 120.9(5) . . ? C27 C28 C33 120.8(4) . . ? C30 C29 C28 121.0(5) . . ? C31 C30 C29 120.4(5) . . ? C30 C31 C32 121.5(5) . . ? C31 C32 C27 118.1(5) . . ? C31 C32 C36 119.6(4) . . ? C27 C32 C36 122.3(4) . . ? C28 C33 C34 110.7(4) . . ? C28 C33 C35 114.2(4) . . ? C34 C33 C35 108.9(5) . . ? C32 C36 C37 112.2(4) . . ? C32 C36 C38 112.1(4) . . ? C37 C36 C38 108.8(4) . . ? N5 C39 N6 119.1(4) . . ? N5 C39 Sm1 59.9(2) . . ? N6 C39 Sm1 60.0(2) . . ? C41 C40 C45 120.5(4) . . ? C41 C40 N5 119.5(4) . . ? C45 C40 N5 119.9(4) . . ? C42 C41 C40 118.4(4) . . ? C42 C41 C46 119.8(4) . . ? C40 C41 C46 121.7(4) . . ? C43 C42 C41 121.9(5) . . ? C42 C43 C44 118.5(4) . . ? C43 C44 C45 122.7(4) . . ? C44 C45 C40 117.8(4) . . ? C44 C45 C49 119.5(4) . . ? C40 C45 C49 122.7(4) . . ? C48 C46 C41 110.0(4) . . ? C48 C46 C47 111.2(5) . . ? C41 C46 C47 112.8(5) . . ? C45 C49 C50 112.6(4) . . ? C45 C49 C51 110.8(4) . . ? C50 C49 C51 110.1(4) . . ? C57 C52 C53 120.3(4) . . ? C57 C52 N6 119.0(4) . . ? C53 C52 N6 120.7(4) . . ? C54 C53 C52 118.4(5) . . ? C54 C53 C58 117.8(4) . . ? C52 C53 C58 123.8(4) . . ? C55 C54 C53 120.9(5) . . ? C54 C55 C56 120.8(4) . . ? C55 C56 C57 120.6(5) . . ? C56 C57 C52 118.9(4) . . ? C56 C57 C61 120.6(4) . . ? C52 C57 C61 120.3(4) . . ? C60 C58 C53 112.8(4) . . ? C60 C58 C59 110.9(5) . . ? C53 C58 C59 110.4(4) . . ? C57 C61 C62 111.0(4) . . ? C57 C61 C63 113.4(4) . . ? C62 C61 C63 109.6(4) . . ? C69 C64 C70 132.5(9) . . ? C69 C64 C65 109.8(8) . . ? C70 C64 C65 117.6(9) . . ? C66 C65 C64 120.6(10) . . ? C66' C65' C64' 118.7(14) . . ? C67 C66 C65 123.0(11) . . ? C65' C66' C67' 124.6(16) . . ? C68 C67 C66 115.0(11) . . ? C68' C67' C66' 114.6(16) . . ? C69 C68 C67 118.7(11) . . ? C64 C69 C68 132.3(9) . . ? C76 C71 C72 114.5(14) . . ? C76 C71 C77 122.3(15) . . ? C72 C71 C77 123.1(14) . . ? C73 C72 C71 120.8(16) . . ? C72 C73 C74 121.9(15) . . ? C75 C74 C73 119.8(15) . . ? C74 C75 C76 117.6(16) . . ? C71 C76 C75 125.3(14) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.989 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.090 # Attachment '3.hexane.CIF' data_jun9rsq _database_code_depnum_ccdc_archive 'CCDC 752058' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C69 H93 N6 Sm, C6 H14' _chemical_formula_sum 'C75 H107 N6 Sm' _chemical_formula_weight 1243.02 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 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.4627(1) _cell_length_b 42.0049(5) _cell_length_c 13.4222(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.980(1) _cell_angle_gamma 90.00 _cell_volume 6873.41(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 33035 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2644 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KAPPA CCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method 'thin slice phi and omega scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54490 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_sigmaI/netI 0.1012 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 23069 _reflns_number_gt 17648 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material CIFTAB _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^)+(0.0920P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.035(12) _refine_ls_number_reflns 23069 _refine_ls_number_parameters 1369 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1448 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.413 0.320 0.845 496.0 110 2 0.413 0.820 0.155 496.0 112 _platon_squeeze_details ; ? ; 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 0.02262(3) 0.182339(9) 0.41691(3) 0.02910(11) Uani 1 1 d . . . Sm2 Sm -0.23620(3) -0.041629(9) -0.21587(3) 0.03043(11) Uani 1 1 d . . . N1 N -0.1106(5) 0.17220(15) 0.5241(5) 0.0311(17) Uani 1 1 d . . . N2 N -0.1538(5) 0.15485(17) 0.3570(5) 0.0323(17) Uani 1 1 d . . . N3 N 0.1647(5) 0.14515(17) 0.5036(5) 0.0318(16) Uani 1 1 d . . . N4 N 0.1526(5) 0.15448(17) 0.3330(5) 0.0343(17) Uani 1 1 d . . . N5 N 0.0910(5) 0.23567(17) 0.4777(5) 0.0324(16) Uani 1 1 d . . . N6 N -0.0225(5) 0.23183(15) 0.3176(5) 0.0299(16) Uani 1 1 d . . . N7 N -0.0595(5) -0.01584(17) -0.1522(5) 0.0320(16) Uani 1 1 d . . . N8 N -0.0997(6) -0.03166(19) -0.3176(5) 0.042(2) Uani 1 1 d . . . N9 N -0.3664(5) -0.01442(16) -0.1308(5) 0.0292(15) Uani 1 1 d . . . N10 N -0.3781(5) -0.00326(16) -0.2981(5) 0.0308(17) Uani 1 1 d . . . N11 N -0.1983(5) -0.09267(16) -0.1270(5) 0.0305(16) Uani 1 1 d . . . N12 N -0.3038(6) -0.09302(18) -0.2881(5) 0.0371(17) Uani 1 1 d . . . C1 C -0.1798(7) 0.1577(2) 0.4472(6) 0.037(2) Uani 1 1 d . . . H1 H -0.2476 0.1495 0.4577 0.044 Uiso 1 1 calc R . . C2 C -0.1522(6) 0.1765(2) 0.6139(6) 0.031(2) Uani 1 1 d . . . C3 C -0.2448(7) 0.1958(2) 0.6138(6) 0.042(2) Uani 1 1 d . . . C4 C -0.2870(7) 0.1975(2) 0.7018(7) 0.047(3) Uani 1 1 d . . . H4 H -0.3509 0.2099 0.7012 0.057 Uiso 1 1 calc R . . C5 C -0.2391(6) 0.1818(3) 0.7897(6) 0.049(3) Uani 1 1 d . . . C6 C -0.1462(7) 0.1642(2) 0.7889(7) 0.040(2) Uani 1 1 d . . . H6 H -0.1110 0.1538 0.8497 0.048 Uiso 1 1 calc R . . C7 C -0.1023(6) 0.1610(2) 0.7031(6) 0.035(2) Uani 1 1 d . . . C8 C -0.2955(7) 0.2143(2) 0.5202(7) 0.048(2) Uani 1 1 d . . . H8A H -0.2555 0.2099 0.4661 0.071 Uiso 1 1 calc R . . H8B H -0.2918 0.2371 0.5359 0.071 Uiso 1 1 calc R . . H8C H -0.3723 0.2079 0.4975 0.071 Uiso 1 1 calc R . . C9 C -0.2889(8) 0.1834(3) 0.8847(7) 0.065(3) Uani 1 1 d . . . H9A H -0.3536 0.1972 0.8714 0.097 Uiso 1 1 calc R . . H9B H -0.2345 0.1919 0.9418 0.097 Uiso 1 1 calc R . . H9C H -0.3104 0.1619 0.9018 0.097 Uiso 1 1 calc R . . C10 C 0.0004(7) 0.1412(2) 0.7066(7) 0.041(2) Uani 1 1 d . . . H10A H 0.0247 0.1323 0.7750 0.061 Uiso 1 1 calc R . . H10B H 0.0585 0.1547 0.6900 0.061 Uiso 1 1 calc R . . H10C H -0.0158 0.1238 0.6569 0.061 Uiso 1 1 calc R . . C11 C -0.2335(6) 0.1387(2) 0.2811(5) 0.028(2) Uani 1 1 d . . . C12 C -0.2866(6) 0.1556(2) 0.1958(7) 0.036(2) Uani 1 1 d . . . C13 C -0.3646(6) 0.1402(2) 0.1209(6) 0.034(2) Uani 1 1 d . . . H13 H -0.3984 0.1516 0.0616 0.041 Uiso 1 1 calc R . . C14 C -0.3930(6) 0.1093(2) 0.1308(6) 0.034(2) Uani 1 1 d . . . C15 C -0.3420(7) 0.0922(2) 0.2155(7) 0.036(2) Uani 1 1 d . . . H15 H -0.3608 0.0705 0.2223 0.043 Uiso 1 1 calc R . . C16 C -0.2607(7) 0.1070(2) 0.2928(7) 0.035(2) Uani 1 1 d . . . C17 C -0.2579(7) 0.1895(2) 0.1808(7) 0.047(3) Uani 1 1 d . . . H17A H -0.2018 0.1966 0.2389 0.071 Uiso 1 1 calc R . . H17B H -0.3236 0.2028 0.1753 0.071 Uiso 1 1 calc R . . H17C H -0.2296 0.1914 0.1182 0.071 Uiso 1 1 calc R . . C18 C -0.4765(7) 0.0927(2) 0.0493(7) 0.050(3) Uani 1 1 d . . . H18A H -0.4860 0.0707 0.0704 0.075 Uiso 1 1 calc R . . H18B H -0.4508 0.0927 -0.0149 0.075 Uiso 1 1 calc R . . H18C H -0.5468 0.1039 0.0398 0.075 Uiso 1 1 calc R . . C19 C -0.2023(8) 0.0868(2) 0.3814(7) 0.039(2) Uani 1 1 d . . . H19A H -0.2340 0.0654 0.3757 0.059 Uiso 1 1 calc R . . H19B H -0.2111 0.0965 0.4457 0.059 Uiso 1 1 calc R . . H19C H -0.1241 0.0855 0.3800 0.059 Uiso 1 1 calc R . . C20 C 0.1962(6) 0.1389(2) 0.4166(7) 0.031(2) Uani 1 1 d . . . H20 H 0.2503 0.1231 0.4149 0.037 Uiso 1 1 calc R . . C21 C 0.2130(6) 0.1261(2) 0.5914(7) 0.035(2) Uani 1 1 d . . . C22 C 0.2752(7) 0.1431(2) 0.6772(7) 0.043(2) Uani 1 1 d . . . C23 C 0.3178(7) 0.1255(2) 0.7634(7) 0.046(2) Uani 1 1 d . . . H23 H 0.3603 0.1359 0.8213 0.055 Uiso 1 1 calc R . . C24 C 0.2995(8) 0.0933(3) 0.7666(8) 0.049(3) Uani 1 1 d . . . H24 H 0.3289 0.0818 0.8269 0.058 Uiso 1 1 calc R . . C25 C 0.2407(7) 0.0779(2) 0.6857(7) 0.041(2) Uani 1 1 d . . . H25 H 0.2299 0.0556 0.6903 0.050 Uiso 1 1 calc R . . C26 C 0.1952(7) 0.0935(2) 0.5960(7) 0.034(2) Uani 1 1 d . . . C27 C 0.2943(8) 0.1781(3) 0.6711(7) 0.053(3) Uani 1 1 d . . . H27 H 0.2347 0.1869 0.6167 0.063 Uiso 1 1 calc R . . C28 C 0.3996(15) 0.1839(4) 0.6405(15) 0.145(7) Uani 1 1 d . . . H28A H 0.4114 0.2069 0.6363 0.218 Uiso 1 1 calc R . . H28B H 0.3979 0.1741 0.5739 0.218 Uiso 1 1 calc R . . H28C H 0.4594 0.1745 0.6910 0.218 Uiso 1 1 calc R . . C29 C 0.2909(14) 0.1958(4) 0.7708(12) 0.110(5) Uani 1 1 d . . . H29A H 0.2224 0.1906 0.7924 0.164 Uiso 1 1 calc R . . H29B H 0.2945 0.2188 0.7597 0.164 Uiso 1 1 calc R . . H29C H 0.3534 0.1892 0.8239 0.164 Uiso 1 1 calc R . . C30 C 0.1243(7) 0.07484(19) 0.5091(6) 0.035(2) Uani 1 1 d . . . H30 H 0.0864 0.0906 0.4579 0.043 Uiso 1 1 calc R . . C31 C 0.1936(9) 0.0534(2) 0.4558(8) 0.055(3) Uani 1 1 d . . . H31A H 0.1457 0.0418 0.4005 0.082 Uiso 1 1 calc R . . H31B H 0.2341 0.0382 0.5049 0.082 Uiso 1 1 calc R . . H31C H 0.2455 0.0664 0.4278 0.082 Uiso 1 1 calc R . . C32 C 0.0352(7) 0.0551(2) 0.5446(7) 0.041(2) Uani 1 1 d . . . H32A H -0.0086 0.0437 0.4864 0.061 Uiso 1 1 calc R . . H32B H -0.0125 0.0693 0.5739 0.061 Uiso 1 1 calc R . . H32C H 0.0699 0.0397 0.5962 0.061 Uiso 1 1 calc R . . C33 C 0.1905(6) 0.14702(19) 0.2412(6) 0.0300(19) Uani 1 1 d . . . C34 C 0.1151(7) 0.1346(2) 0.1576(6) 0.034(2) Uani 1 1 d . . . C35 C 0.1490(7) 0.1290(2) 0.0676(7) 0.039(2) Uani 1 1 d . . . H35 H 0.0981 0.1209 0.0106 0.047 Uiso 1 1 calc R . . C36 C 0.2564(7) 0.1351(2) 0.0590(7) 0.041(2) Uani 1 1 d . . . H36 H 0.2790 0.1307 -0.0030 0.050 Uiso 1 1 calc R . . C37 C 0.3310(7) 0.1477(2) 0.1420(7) 0.044(2) Uani 1 1 d . . . H37 H 0.4041 0.1521 0.1356 0.053 Uiso 1 1 calc R . . C38 C 0.2998(7) 0.1539(2) 0.2344(7) 0.034(2) Uani 1 1 d . . . C39 C 0.0008(7) 0.1242(2) 0.1701(7) 0.040(2) Uani 1 1 d . . . H39 H -0.0225 0.1389 0.2204 0.048 Uiso 1 1 calc R . . C40 C 0.0030(7) 0.0913(2) 0.2119(7) 0.046(2) Uani 1 1 d . . . H40A H 0.0564 0.0902 0.2766 0.069 Uiso 1 1 calc R . . H40B H 0.0240 0.0763 0.1633 0.069 Uiso 1 1 calc R . . H40C H -0.0699 0.0857 0.2231 0.069 Uiso 1 1 calc R . . C41 C -0.0839(7) 0.1270(2) 0.0694(7) 0.044(2) Uani 1 1 d . . . H41A H -0.0846 0.1489 0.0440 0.066 Uiso 1 1 calc R . . H41B H -0.1568 0.1215 0.0809 0.066 Uiso 1 1 calc R . . H41C H -0.0642 0.1124 0.0192 0.066 Uiso 1 1 calc R . . C42 C 0.3842(7) 0.1687(2) 0.3182(7) 0.038(2) Uani 1 1 d . . . H42 H 0.3444 0.1776 0.3694 0.046 Uiso 1 1 calc R . . C43 C 0.4494(7) 0.1962(2) 0.2833(8) 0.055(3) Uani 1 1 d . . . H43A H 0.5011 0.2049 0.3421 0.083 Uiso 1 1 calc R . . H43B H 0.3987 0.2130 0.2523 0.083 Uiso 1 1 calc R . . H43C H 0.4900 0.1883 0.2331 0.083 Uiso 1 1 calc R . . C44 C 0.4662(7) 0.1432(2) 0.3737(8) 0.051(3) Uani 1 1 d . . . H44A H 0.5195 0.1534 0.4283 0.077 Uiso 1 1 calc R . . H44B H 0.5047 0.1334 0.3249 0.077 Uiso 1 1 calc R . . H44C H 0.4258 0.1268 0.4027 0.077 Uiso 1 1 calc R . . C45 C 0.0334(6) 0.2496(2) 0.3939(6) 0.0315(19) Uani 1 1 d . . . H45 H 0.0321 0.2721 0.3885 0.038 Uiso 1 1 calc R . . C46 C 0.1516(7) 0.2563(2) 0.5540(7) 0.037(2) Uani 1 1 d . . . C47 C 0.1081(8) 0.2638(2) 0.6405(7) 0.043(2) Uani 1 1 d . . . C48 C 0.1671(8) 0.2856(3) 0.7120(7) 0.050(3) Uani 1 1 d . . . H48 H 0.1391 0.2918 0.7697 0.061 Uiso 1 1 calc R . . C49 C 0.2648(9) 0.2976(3) 0.6975(8) 0.053(3) Uani 1 1 d . . . H49 H 0.3041 0.3119 0.7467 0.064 Uiso 1 1 calc R . . C50 C 0.3069(8) 0.2900(2) 0.6169(8) 0.051(2) Uani 1 1 d . . . H50 H 0.3749 0.2992 0.6106 0.062 Uiso 1 1 calc R . . C51 C 0.2540(7) 0.2690(2) 0.5413(7) 0.042(2) Uani 1 1 d . . . C52 C 0.0026(8) 0.2510(3) 0.6575(7) 0.052(3) Uani 1 1 d . . . H52 H -0.0160 0.2322 0.6112 0.063 Uiso 1 1 calc R . . C53 C 0.0046(10) 0.2394(3) 0.7639(8) 0.076(4) Uani 1 1 d . . . H53A H -0.0676 0.2308 0.7676 0.114 Uiso 1 1 calc R . . H53B H 0.0223 0.2572 0.8118 0.114 Uiso 1 1 calc R . . H53C H 0.0602 0.2227 0.7817 0.114 Uiso 1 1 calc R . . C54 C -0.0889(9) 0.2756(3) 0.6245(10) 0.084(4) Uani 1 1 d . . . H54A H -0.1586 0.2669 0.6349 0.125 Uiso 1 1 calc R . . H54B H -0.0950 0.2808 0.5523 0.125 Uiso 1 1 calc R . . H54C H -0.0714 0.2950 0.6653 0.125 Uiso 1 1 calc R . . C55 C 0.3030(7) 0.2623(2) 0.4505(7) 0.042(2) Uani 1 1 d . . . H55 H 0.2687 0.2423 0.4176 0.051 Uiso 1 1 calc R . . C56 C 0.4269(8) 0.2572(3) 0.4780(10) 0.070(3) Uani 1 1 d . . . H56A H 0.4541 0.2526 0.4161 0.104 Uiso 1 1 calc R . . H56B H 0.4438 0.2393 0.5255 0.104 Uiso 1 1 calc R . . H56C H 0.4624 0.2766 0.5100 0.104 Uiso 1 1 calc R . . C57 C 0.2798(8) 0.2888(2) 0.3729(8) 0.054(3) Uani 1 1 d . . . H57A H 0.3128 0.2836 0.3147 0.081 Uiso 1 1 calc R . . H57B H 0.3112 0.3087 0.4041 0.081 Uiso 1 1 calc R . . H57C H 0.2003 0.2913 0.3497 0.081 Uiso 1 1 calc R . . C58 C -0.0793(6) 0.24821(19) 0.2284(7) 0.032(2) Uani 1 1 d . . . C59 C -0.1671(7) 0.2696(2) 0.2344(7) 0.039(2) Uani 1 1 d . . . C60 C -0.2207(8) 0.2843(2) 0.1441(8) 0.049(3) Uani 1 1 d . . . H60 H -0.2782 0.2990 0.1462 0.058 Uiso 1 1 calc R . . C61 C -0.1922(7) 0.2780(2) 0.0527(8) 0.052(3) Uani 1 1 d . . . H61 H -0.2303 0.2882 -0.0075 0.062 Uiso 1 1 calc R . . C62 C -0.1075(8) 0.2568(2) 0.0477(8) 0.050(2) Uani 1 1 d . . . H62 H -0.0891 0.2523 -0.0161 0.060 Uiso 1 1 calc R . . C63 C -0.0487(7) 0.2418(2) 0.1371(7) 0.036(2) Uani 1 1 d . . . C64 C -0.2056(8) 0.2761(2) 0.3333(8) 0.046(2) Uani 1 1 d . . . H64 H -0.1658 0.2615 0.3875 0.055 Uiso 1 1 calc R . . C65 C -0.3303(8) 0.2700(3) 0.3189(9) 0.061(3) Uani 1 1 d . . . H65A H -0.3534 0.2740 0.3832 0.091 Uiso 1 1 calc R . . H65B H -0.3464 0.2479 0.2980 0.091 Uiso 1 1 calc R . . H65C H -0.3700 0.2843 0.2662 0.091 Uiso 1 1 calc R . . C66 C -0.1814(9) 0.3107(2) 0.3679(9) 0.062(3) Uani 1 1 d . . . H66A H -0.2060 0.3143 0.4317 0.093 Uiso 1 1 calc R . . H66B H -0.2204 0.3252 0.3154 0.093 Uiso 1 1 calc R . . H66C H -0.1024 0.3147 0.3786 0.093 Uiso 1 1 calc R . . C67 C 0.0433(7) 0.2185(2) 0.1315(7) 0.044(2) Uani 1 1 d . . . H67 H 0.0332 0.1990 0.1710 0.053 Uiso 1 1 calc R . . C68 C 0.1533(8) 0.2337(3) 0.1793(8) 0.055(3) Uani 1 1 d . . . H68A H 0.1536 0.2396 0.2500 0.082 Uiso 1 1 calc R . . H68B H 0.1643 0.2529 0.1408 0.082 Uiso 1 1 calc R . . H68C H 0.2126 0.2185 0.1777 0.082 Uiso 1 1 calc R . . C69 C 0.0470(9) 0.2089(3) 0.0221(7) 0.056(3) Uani 1 1 d . . . H69A H -0.0221 0.1986 -0.0095 0.084 Uiso 1 1 calc R . . H69B H 0.1080 0.1941 0.0230 0.084 Uiso 1 1 calc R . . H69C H 0.0575 0.2279 -0.0170 0.084 Uiso 1 1 calc R . . C70 C -0.0306(7) -0.0187(2) -0.2402(7) 0.036(2) Uani 1 1 d . . . H70 H 0.0394 -0.0116 -0.2483 0.043 Uiso 1 1 calc R . . C71 C 0.0220(6) -0.0014(2) -0.0728(6) 0.031(2) Uani 1 1 d . . . C72 C 0.0717(7) -0.0195(2) 0.0139(7) 0.034(2) Uani 1 1 d . . . C73 C 0.1510(6) -0.0047(2) 0.0901(7) 0.034(2) Uani 1 1 d . . . H73 H 0.1854 -0.0169 0.1475 0.041 Uiso 1 1 calc R . . C74 C 0.1803(6) 0.0267(2) 0.0843(6) 0.036(2) Uani 1 1 d . . . C75 C 0.1321(7) 0.0436(2) -0.0003(7) 0.039(2) Uani 1 1 d . . . H75 H 0.1536 0.0652 -0.0054 0.047 Uiso 1 1 calc R . . C76 C 0.0521(7) 0.0308(2) -0.0803(6) 0.032(2) Uani 1 1 d . . . C77 C 0.0391(8) -0.0535(2) 0.0243(7) 0.044(3) Uani 1 1 d . . . H77A H 0.0803 -0.0622 0.0888 0.066 Uiso 1 1 calc R . . H77B H 0.0554 -0.0660 -0.0324 0.066 Uiso 1 1 calc R . . H77C H -0.0396 -0.0546 0.0234 0.066 Uiso 1 1 calc R . . C78 C 0.2637(7) 0.0417(3) 0.1681(7) 0.050(3) Uani 1 1 d . . . H78A H 0.2747 0.0640 0.1507 0.075 Uiso 1 1 calc R . . H78B H 0.3333 0.0302 0.1762 0.075 Uiso 1 1 calc R . . H78C H 0.2374 0.0408 0.2319 0.075 Uiso 1 1 calc R . . C79 C -0.0005(8) 0.0513(2) -0.1682(8) 0.048(3) Uani 1 1 d . . . H79A H 0.0308 0.0727 -0.1592 0.073 Uiso 1 1 calc R . . H79B H -0.0797 0.0524 -0.1714 0.073 Uiso 1 1 calc R . . H79C H 0.0129 0.0421 -0.2317 0.073 Uiso 1 1 calc R . . C80 C -0.0579(7) -0.0351(2) -0.4097(6) 0.038(2) Uani 1 1 d . . . C81 C -0.1072(8) -0.0194(2) -0.4984(7) 0.044(2) Uani 1 1 d . . . C82 C -0.0632(8) -0.0217(2) -0.5840(7) 0.050(2) Uani 1 1 d . . . H82 H -0.0980 -0.0109 -0.6443 0.060 Uiso 1 1 calc R . . C83 C 0.0314(7) -0.0395(4) -0.5845(6) 0.059(3) Uani 1 1 d . . . C84 C 0.0749(8) -0.0565(3) -0.4960(8) 0.067(3) Uani 1 1 d . . . H84 H 0.1369 -0.0697 -0.4954 0.081 Uiso 1 1 calc R . . C85 C 0.0322(7) -0.0550(2) -0.4101(7) 0.047(3) Uani 1 1 d . . . C86 C -0.2093(8) 0.0003(3) -0.4990(8) 0.052(3) Uani 1 1 d . . . H86A H -0.2284 -0.0007 -0.4318 0.079 Uiso 1 1 calc R . . H86B H -0.2701 -0.0080 -0.5506 0.079 Uiso 1 1 calc R . . H86C H -0.1953 0.0225 -0.5150 0.079 Uiso 1 1 calc R . . C87 C 0.0790(9) -0.0411(5) -0.6798(8) 0.101(5) Uani 1 1 d . . . H87A H 0.0359 -0.0275 -0.7327 0.151 Uiso 1 1 calc R . . H87B H 0.0767 -0.0631 -0.7042 0.151 Uiso 1 1 calc R . . H87C H 0.1552 -0.0336 -0.6639 0.151 Uiso 1 1 calc R . . C88 C 0.0805(9) -0.0753(3) -0.3175(8) 0.066(3) Uani 1 1 d . . . H88A H 0.1434 -0.0873 -0.3309 0.099 Uiso 1 1 calc R . . H88B H 0.0246 -0.0902 -0.3039 0.099 Uiso 1 1 calc R . . H88C H 0.1043 -0.0615 -0.2581 0.099 Uiso 1 1 calc R . . C89 C -0.4083(6) 0.0025(2) -0.2133(7) 0.035(2) Uani 1 1 d . . . H89 H -0.4603 0.0188 -0.2100 0.042 Uiso 1 1 calc R . . C90 C -0.4030(7) -0.0083(2) -0.0380(6) 0.034(2) Uani 1 1 d . . . C91 C -0.3283(7) 0.0037(2) 0.0464(7) 0.037(2) Uani 1 1 d . . . C92 C -0.3617(7) 0.0081(2) 0.1378(7) 0.037(2) Uani 1 1 d . . . H92 H -0.3102 0.0152 0.1959 0.045 Uiso 1 1 calc R . . C93 C -0.4701(7) 0.0023(2) 0.1455(7) 0.047(2) Uani 1 1 d . . . H93 H -0.4924 0.0055 0.2083 0.057 Uiso 1 1 calc R . . C94 C -0.5431(7) -0.0079(2) 0.0622(7) 0.043(2) Uani 1 1 d . . . H94 H -0.6175 -0.0107 0.0670 0.051 Uiso 1 1 calc R . . C95 C -0.5129(7) -0.0143(2) -0.0304(7) 0.037(2) Uani 1 1 d . . . C96 C -0.2120(7) 0.0128(2) 0.0373(7) 0.039(2) Uani 1 1 d . . . H96 H -0.1897 -0.0018 -0.0138 0.046 Uiso 1 1 calc R . . C97 C -0.2139(7) 0.0465(2) -0.0041(7) 0.047(2) Uani 1 1 d . . . H97A H -0.1399 0.0526 -0.0108 0.070 Uiso 1 1 calc R . . H97B H -0.2395 0.0611 0.0429 0.070 Uiso 1 1 calc R . . H97C H -0.2637 0.0475 -0.0709 0.070 Uiso 1 1 calc R . . C98 C -0.1250(8) 0.0097(3) 0.1385(7) 0.048(2) Uani 1 1 d . . . H98A H -0.0528 0.0157 0.1266 0.071 Uiso 1 1 calc R . . H98B H -0.1227 -0.0124 0.1626 0.071 Uiso 1 1 calc R . . H98C H -0.1448 0.0238 0.1900 0.071 Uiso 1 1 calc R . . C99 C -0.6005(7) -0.0263(2) -0.1205(7) 0.042(2) Uani 1 1 d . . . H99 H -0.5624 -0.0351 -0.1732 0.050 Uiso 1 1 calc R . . C100 C -0.6775(7) -0.0004(2) -0.1691(7) 0.050(2) Uani 1 1 d . . . H10D H -0.7303 -0.0092 -0.2270 0.074 Uiso 1 1 calc R . . H10E H -0.6354 0.0167 -0.1930 0.074 Uiso 1 1 calc R . . H10F H -0.7168 0.0082 -0.1190 0.074 Uiso 1 1 calc R . . C101 C -0.6674(7) -0.0536(2) -0.0837(8) 0.051(3) Uani 1 1 d . . . H10G H -0.6172 -0.0706 -0.0530 0.077 Uiso 1 1 calc R . . H10H H -0.7203 -0.0622 -0.1419 0.077 Uiso 1 1 calc R . . H10I H -0.7066 -0.0453 -0.0330 0.077 Uiso 1 1 calc R . . C102 C -0.4211(7) 0.0159(2) -0.3859(7) 0.038(2) Uani 1 1 d . . . C103 C -0.3993(7) 0.0497(2) -0.3844(7) 0.039(2) Uani 1 1 d . . . C104 C -0.4434(7) 0.0674(2) -0.4721(7) 0.045(2) Uani 1 1 d . . . H104 H -0.4318 0.0897 -0.4720 0.055 Uiso 1 1 calc R . . C105 C -0.5031(8) 0.0530(3) -0.5582(8) 0.049(3) Uani 1 1 d . . . H105 H -0.5313 0.0652 -0.6173 0.059 Uiso 1 1 calc R . . C106 C -0.5215(7) 0.0203(3) -0.5575(8) 0.048(3) Uani 1 1 d . . . H106 H -0.5617 0.0105 -0.6174 0.057 Uiso 1 1 calc R . . C107 C -0.4836(7) 0.0021(2) -0.4736(7) 0.035(2) Uani 1 1 d . . . C108 C -0.3277(7) 0.0664(2) -0.2938(7) 0.041(2) Uani 1 1 d . . . H108 H -0.2920 0.0498 -0.2444 0.049 Uiso 1 1 calc R . . C109 C -0.3976(8) 0.0886(2) -0.2385(8) 0.057(3) Uani 1 1 d . . . H10J H -0.4554 0.0761 -0.2174 0.085 Uiso 1 1 calc R . . H10K H -0.4308 0.1055 -0.2851 0.085 Uiso 1 1 calc R . . H10L H -0.3502 0.0981 -0.1784 0.085 Uiso 1 1 calc R . . C110 C -0.2356(8) 0.0870(2) -0.3257(7) 0.049(2) Uani 1 1 d . . . H11A H -0.1908 0.0735 -0.3606 0.074 Uiso 1 1 calc R . . H11B H -0.1891 0.0963 -0.2649 0.074 Uiso 1 1 calc R . . H11C H -0.2692 0.1040 -0.3717 0.074 Uiso 1 1 calc R . . C111 C -0.5107(8) -0.0333(3) -0.4756(8) 0.058(3) Uani 1 1 d . . . H111 H -0.4556 -0.0438 -0.4205 0.069 Uiso 1 1 calc R . . C112 C -0.6223(13) -0.0377(4) -0.4497(17) 0.148(8) Uani 1 1 d . . . H11D H -0.6244 -0.0264 -0.3861 0.222 Uiso 1 1 calc R . . H11E H -0.6359 -0.0604 -0.4413 0.222 Uiso 1 1 calc R . . H11F H -0.6789 -0.0290 -0.5048 0.222 Uiso 1 1 calc R . . C113 C -0.5032(13) -0.0492(3) -0.5743(10) 0.105(5) Uani 1 1 d . . . H11G H -0.5214 -0.0719 -0.5709 0.158 Uiso 1 1 calc R . . H11H H -0.4285 -0.0471 -0.5859 0.158 Uiso 1 1 calc R . . H11I H -0.5550 -0.0391 -0.6304 0.158 Uiso 1 1 calc R . . C114 C -0.2550(6) -0.1083(2) -0.2041(7) 0.034(2) Uani 1 1 d . . . H114 H -0.2616 -0.1308 -0.2003 0.041 Uiso 1 1 calc R . . C115 C -0.1461(7) -0.1113(2) -0.0391(7) 0.039(2) Uani 1 1 d . . . C116 C -0.0613(7) -0.1328(2) -0.0441(8) 0.043(2) Uani 1 1 d . . . C117 C -0.0182(9) -0.1501(3) 0.0448(9) 0.056(3) Uani 1 1 d . . . H117 H 0.0373 -0.1654 0.0423 0.067 Uiso 1 1 calc R . . C118 C -0.0506(9) -0.1463(3) 0.1309(9) 0.065(3) Uani 1 1 d . . . H118 H -0.0184 -0.1588 0.1886 0.078 Uiso 1 1 calc R . . C119 C -0.1302(9) -0.1247(3) 0.1385(8) 0.058(3) Uani 1 1 d . . . H119 H -0.1520 -0.1219 0.2017 0.069 Uiso 1 1 calc R . . C120 C -0.1793(7) -0.1068(2) 0.0545(7) 0.041(2) Uani 1 1 d . . . C121 C -0.0187(7) -0.1383(2) -0.1406(8) 0.048(3) Uani 1 1 d . . . H121 H -0.0540 -0.1223 -0.1921 0.058 Uiso 1 1 calc R . . C122 C -0.0478(8) -0.1709(2) -0.1844(8) 0.056(3) Uani 1 1 d . . . H12A H -0.0198 -0.1734 -0.2470 0.084 Uiso 1 1 calc R . . H12B H -0.1277 -0.1735 -0.1999 0.084 Uiso 1 1 calc R . . H12C H -0.0148 -0.1871 -0.1349 0.084 Uiso 1 1 calc R . . C123 C 0.1092(8) -0.1328(3) -0.1201(9) 0.054(3) Uani 1 1 d . . . H12D H 0.1354 -0.1364 -0.1831 0.081 Uiso 1 1 calc R . . H12E H 0.1457 -0.1478 -0.0678 0.081 Uiso 1 1 calc R . . H12F H 0.1260 -0.1110 -0.0965 0.081 Uiso 1 1 calc R . . C124 C -0.2731(9) -0.0840(2) 0.0621(7) 0.051(3) Uani 1 1 d . . . H124 H -0.2625 -0.0649 0.0208 0.061 Uiso 1 1 calc R . . C125 C -0.3829(10) -0.0983(4) 0.0108(10) 0.085(4) Uani 1 1 d . . . H12G H -0.4419 -0.0833 0.0161 0.127 Uiso 1 1 calc R . . H12H H -0.3944 -0.1183 0.0444 0.127 Uiso 1 1 calc R . . H12I H -0.3832 -0.1023 -0.0611 0.127 Uiso 1 1 calc R . . C126 C -0.2685(12) -0.0719(3) 0.1701(8) 0.077(4) Uani 1 1 d . . . H12J H -0.3303 -0.0575 0.1703 0.116 Uiso 1 1 calc R . . H12K H -0.1994 -0.0604 0.1941 0.116 Uiso 1 1 calc R . . H12L H -0.2727 -0.0899 0.2154 0.116 Uiso 1 1 calc R . . C127 C -0.3697(7) -0.1111(2) -0.3668(7) 0.036(2) Uani 1 1 d . . . C128 C -0.4717(7) -0.1233(2) -0.3578(8) 0.047(2) Uani 1 1 d . . . C129 C -0.5341(7) -0.1411(2) -0.4386(9) 0.061(3) Uani 1 1 d . . . H129 H -0.6020 -0.1500 -0.4313 0.073 Uiso 1 1 calc R . . C130 C -0.4981(10) -0.1457(3) -0.5289(9) 0.061(3) Uani 1 1 d . . . H130 H -0.5428 -0.1570 -0.5834 0.073 Uiso 1 1 calc R . . C131 C -0.3983(10) -0.1339(3) -0.5396(8) 0.061(3) Uani 1 1 d . . . H131 H -0.3735 -0.1372 -0.6012 0.073 Uiso 1 1 calc R . . C132 C -0.3315(8) -0.1166(2) -0.4572(8) 0.047(2) Uani 1 1 d . . . C133 C -0.5154(8) -0.1193(2) -0.2623(9) 0.059(3) Uani 1 1 d . . . H133 H -0.4716 -0.1023 -0.2201 0.070 Uiso 1 1 calc R . . C134 C -0.5009(10) -0.1510(3) -0.1996(11) 0.090(4) Uani 1 1 d . . . H13A H -0.5296 -0.1482 -0.1375 0.135 Uiso 1 1 calc R . . H13B H -0.4228 -0.1565 -0.1813 0.135 Uiso 1 1 calc R . . H13C H -0.5411 -0.1681 -0.2408 0.135 Uiso 1 1 calc R . . C135 C -0.6391(8) -0.1092(3) -0.2842(11) 0.084(4) Uani 1 1 d . . . H13D H -0.6633 -0.1068 -0.2197 0.126 Uiso 1 1 calc R . . H13E H -0.6834 -0.1256 -0.3256 0.126 Uiso 1 1 calc R . . H13F H -0.6481 -0.0889 -0.3211 0.126 Uiso 1 1 calc R . . C136 C -0.2162(8) -0.1060(3) -0.4669(7) 0.056(3) Uani 1 1 d . . . H136 H -0.1927 -0.0878 -0.4193 0.068 Uiso 1 1 calc R . . C137 C -0.1344(9) -0.1335(3) -0.4380(9) 0.071(3) Uani 1 1 d . . . H13G H -0.0610 -0.1264 -0.4436 0.106 Uiso 1 1 calc R . . H13H H -0.1568 -0.1515 -0.4841 0.106 Uiso 1 1 calc R . . H13I H -0.1333 -0.1401 -0.3678 0.106 Uiso 1 1 calc R . . C138 C -0.2126(10) -0.0952(3) -0.5767(7) 0.072(3) Uani 1 1 d . . . H13J H -0.2631 -0.0773 -0.5962 0.107 Uiso 1 1 calc R . . H13K H -0.2344 -0.1130 -0.6240 0.107 Uiso 1 1 calc R . . H13L H -0.1379 -0.0885 -0.5794 0.107 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 0.02186(19) 0.0325(2) 0.0332(2) 0.0006(2) 0.00632(16) 0.00056(18) Sm2 0.0238(2) 0.0345(2) 0.0336(2) 0.0006(2) 0.00733(17) 0.00044(18) N1 0.030(4) 0.039(5) 0.025(4) 0.002(3) 0.008(3) -0.004(3) N2 0.024(4) 0.040(5) 0.034(4) -0.005(3) 0.010(3) 0.000(3) N3 0.019(3) 0.040(4) 0.036(4) 0.005(3) 0.002(3) -0.004(3) N4 0.025(4) 0.043(5) 0.033(4) 0.001(4) 0.002(3) 0.001(3) N5 0.027(4) 0.034(4) 0.035(4) -0.005(3) 0.005(3) -0.008(3) N6 0.029(4) 0.022(4) 0.038(4) 0.000(3) 0.005(3) -0.002(3) N7 0.031(4) 0.040(4) 0.026(4) -0.002(3) 0.007(3) -0.006(3) N8 0.027(4) 0.067(6) 0.030(4) -0.007(4) 0.003(3) -0.012(4) N9 0.029(4) 0.032(4) 0.029(4) 0.003(3) 0.013(3) 0.004(3) N10 0.025(4) 0.034(4) 0.035(4) -0.002(3) 0.008(3) -0.002(3) N11 0.023(3) 0.033(4) 0.034(4) 0.000(3) 0.003(3) -0.005(3) N12 0.032(4) 0.037(4) 0.038(4) 0.003(4) -0.002(3) 0.000(3) C1 0.036(5) 0.049(6) 0.028(5) -0.005(4) 0.010(4) -0.001(4) C2 0.020(4) 0.042(6) 0.030(4) -0.004(4) 0.002(3) 0.002(4) C3 0.029(4) 0.065(7) 0.031(5) -0.006(4) 0.002(4) -0.004(4) C4 0.025(4) 0.071(7) 0.046(6) -0.015(5) 0.007(4) 0.003(4) C5 0.038(5) 0.073(7) 0.040(6) -0.007(6) 0.018(5) -0.009(6) C6 0.027(4) 0.055(6) 0.037(5) -0.012(4) 0.008(4) -0.012(4) C7 0.027(4) 0.042(5) 0.038(5) -0.006(4) 0.009(4) -0.004(4) C8 0.037(5) 0.055(6) 0.049(6) 0.003(5) 0.004(4) 0.012(4) C9 0.053(6) 0.099(8) 0.048(5) 0.002(7) 0.022(5) 0.011(7) C10 0.038(5) 0.043(6) 0.040(5) 0.005(4) 0.005(4) 0.004(4) C11 0.020(4) 0.043(6) 0.022(5) -0.009(4) 0.011(4) -0.004(4) C12 0.018(4) 0.043(6) 0.048(6) 0.002(5) 0.010(4) -0.006(4) C13 0.020(4) 0.054(6) 0.027(5) 0.004(4) -0.001(4) 0.000(4) C14 0.025(4) 0.039(5) 0.042(5) 0.003(4) 0.013(4) -0.003(4) C15 0.035(5) 0.034(5) 0.039(5) -0.004(4) 0.010(4) -0.006(4) C16 0.022(4) 0.042(6) 0.042(5) -0.007(4) 0.009(4) -0.003(4) C17 0.034(5) 0.059(8) 0.046(5) 0.012(5) 0.003(4) -0.002(4) C18 0.032(5) 0.065(7) 0.050(6) -0.022(5) -0.002(4) -0.013(4) C19 0.045(5) 0.032(5) 0.042(5) 0.000(4) 0.012(4) -0.001(4) C20 0.019(4) 0.032(5) 0.044(5) 0.001(4) 0.009(4) -0.004(3) C21 0.023(4) 0.040(6) 0.043(5) 0.010(4) 0.011(4) 0.015(4) C22 0.031(5) 0.049(6) 0.046(6) 0.002(5) 0.000(4) 0.006(4) C23 0.032(5) 0.061(7) 0.040(5) 0.006(5) 0.001(4) 0.004(4) C24 0.038(5) 0.057(7) 0.047(6) 0.024(5) -0.002(5) 0.007(5) C25 0.042(5) 0.044(6) 0.038(5) 0.014(4) 0.008(5) 0.004(4) C26 0.028(4) 0.038(6) 0.039(5) 0.004(4) 0.012(4) -0.005(4) C27 0.056(6) 0.039(7) 0.052(6) 0.009(5) -0.014(5) -0.011(5) C28 0.167(16) 0.072(10) 0.22(2) 0.011(13) 0.089(15) -0.048(12) C29 0.144(14) 0.073(11) 0.115(13) -0.025(9) 0.033(11) -0.014(9) C30 0.039(5) 0.024(5) 0.040(5) 0.009(4) 0.002(4) 0.010(4) C31 0.068(7) 0.051(7) 0.048(6) -0.002(5) 0.017(5) 0.009(5) C32 0.033(5) 0.039(5) 0.047(5) 0.004(4) 0.003(4) -0.012(4) C33 0.023(4) 0.034(5) 0.038(5) -0.001(4) 0.018(4) 0.006(3) C34 0.033(5) 0.039(5) 0.032(5) -0.007(4) 0.012(4) -0.005(4) C35 0.030(4) 0.045(6) 0.042(5) -0.011(4) 0.010(4) 0.000(4) C36 0.041(5) 0.052(6) 0.037(5) -0.004(4) 0.019(4) 0.006(4) C37 0.026(5) 0.063(7) 0.045(6) -0.002(5) 0.009(4) 0.000(4) C38 0.029(5) 0.031(5) 0.044(5) 0.004(4) 0.015(4) 0.003(4) C39 0.028(4) 0.048(6) 0.044(5) -0.022(5) 0.011(4) -0.006(4) C40 0.035(5) 0.059(7) 0.046(6) -0.005(5) 0.014(4) -0.015(4) C41 0.023(4) 0.048(6) 0.061(6) -0.007(5) 0.009(4) 0.001(4) C42 0.026(4) 0.044(6) 0.044(5) 0.000(4) 0.005(4) 0.001(4) C43 0.026(5) 0.074(8) 0.064(7) 0.000(5) 0.004(5) -0.009(4) C44 0.028(5) 0.047(6) 0.079(8) 0.005(5) 0.010(5) 0.005(4) C45 0.024(4) 0.031(5) 0.039(5) 0.004(4) 0.005(4) -0.003(4) C46 0.033(5) 0.028(5) 0.045(6) -0.002(4) -0.003(4) -0.003(4) C47 0.040(5) 0.053(6) 0.035(5) -0.007(5) 0.004(4) -0.008(4) C48 0.051(6) 0.064(7) 0.037(5) -0.006(5) 0.009(5) -0.018(5) C49 0.059(7) 0.048(7) 0.046(6) 0.000(5) -0.006(5) -0.017(5) C50 0.041(5) 0.049(6) 0.061(7) -0.005(5) 0.004(5) -0.008(5) C51 0.031(5) 0.044(6) 0.047(5) 0.004(5) 0.000(4) -0.008(4) C52 0.061(6) 0.059(7) 0.043(6) -0.016(5) 0.024(5) -0.020(5) C53 0.080(8) 0.100(10) 0.053(7) -0.016(7) 0.026(6) -0.042(7) C54 0.052(7) 0.110(11) 0.085(9) -0.024(8) 0.006(6) -0.012(7) C55 0.027(4) 0.058(6) 0.039(5) -0.012(5) 0.001(4) -0.013(4) C56 0.040(6) 0.071(8) 0.095(9) -0.016(7) 0.010(6) 0.003(5) C57 0.058(6) 0.048(6) 0.058(6) -0.006(5) 0.017(5) -0.010(5) C58 0.026(4) 0.023(5) 0.043(5) 0.010(4) -0.005(4) -0.003(3) C59 0.028(5) 0.042(6) 0.045(6) 0.008(5) 0.000(4) -0.002(4) C60 0.032(5) 0.052(6) 0.060(7) 0.011(5) 0.004(5) -0.001(4) C61 0.034(5) 0.058(7) 0.055(6) 0.014(5) -0.009(5) -0.012(5) C62 0.053(6) 0.046(6) 0.051(6) 0.000(5) 0.008(5) -0.009(5) C63 0.038(5) 0.028(5) 0.038(5) -0.001(4) -0.001(4) -0.010(4) C64 0.034(5) 0.056(7) 0.049(6) 0.006(5) 0.011(5) 0.000(5) C65 0.037(6) 0.072(8) 0.077(8) 0.018(7) 0.019(6) 0.013(6) C66 0.061(7) 0.053(7) 0.079(8) 0.013(6) 0.029(6) 0.012(5) C67 0.040(5) 0.047(6) 0.045(6) 0.002(5) 0.007(4) 0.004(4) C68 0.043(6) 0.069(7) 0.051(6) 0.005(6) 0.007(5) 0.015(5) C69 0.073(7) 0.051(7) 0.046(6) -0.003(5) 0.016(5) 0.001(5) C70 0.023(4) 0.039(6) 0.047(6) 0.003(4) 0.009(4) -0.005(4) C71 0.023(5) 0.038(6) 0.033(5) -0.011(4) 0.009(4) 0.000(3) C72 0.029(5) 0.042(6) 0.033(5) 0.002(4) 0.012(4) -0.001(4) C73 0.019(4) 0.046(6) 0.039(5) -0.005(4) 0.008(4) 0.004(4) C74 0.015(4) 0.060(7) 0.034(5) -0.010(4) 0.006(3) 0.003(4) C75 0.033(5) 0.040(5) 0.047(6) -0.005(4) 0.017(4) -0.006(4) C76 0.029(4) 0.036(6) 0.031(5) 0.002(4) 0.009(4) -0.003(4) C77 0.045(5) 0.048(7) 0.038(5) -0.002(4) 0.008(4) -0.008(4) C78 0.028(4) 0.068(7) 0.053(6) -0.024(5) 0.007(4) -0.001(4) C79 0.046(6) 0.041(6) 0.054(6) 0.007(5) 0.001(5) 0.002(4) C80 0.035(4) 0.050(7) 0.033(5) -0.009(4) 0.015(4) -0.018(4) C81 0.041(5) 0.054(6) 0.043(6) 0.006(5) 0.019(5) -0.010(5) C82 0.053(6) 0.059(7) 0.039(5) 0.002(5) 0.012(5) -0.005(5) C83 0.040(6) 0.104(10) 0.032(6) -0.007(7) 0.005(5) -0.004(7) C84 0.034(5) 0.113(10) 0.056(7) -0.001(6) 0.014(5) 0.013(6) C85 0.028(5) 0.073(7) 0.040(5) -0.006(5) 0.003(4) 0.000(4) C86 0.054(6) 0.059(7) 0.048(6) 0.016(5) 0.018(5) 0.017(5) C87 0.062(7) 0.203(15) 0.046(6) -0.010(10) 0.030(6) 0.010(10) C88 0.052(6) 0.097(9) 0.045(6) -0.010(6) 0.002(5) 0.018(6) C89 0.020(4) 0.038(6) 0.049(6) -0.006(5) 0.011(4) -0.003(4) C90 0.035(5) 0.034(5) 0.038(5) 0.003(4) 0.014(4) 0.009(4) C91 0.023(4) 0.050(6) 0.039(5) 0.004(4) 0.009(4) 0.004(4) C92 0.031(4) 0.043(6) 0.040(5) -0.004(4) 0.013(4) 0.005(4) C93 0.043(5) 0.059(7) 0.045(6) -0.002(5) 0.021(5) 0.001(5) C94 0.026(5) 0.054(6) 0.051(6) -0.005(5) 0.014(4) -0.002(4) C95 0.027(4) 0.043(6) 0.042(5) -0.002(4) 0.010(4) 0.004(4) C96 0.035(5) 0.049(6) 0.034(5) -0.004(4) 0.012(4) 0.002(4) C97 0.036(5) 0.055(6) 0.053(6) 0.005(5) 0.016(4) -0.010(4) C98 0.041(5) 0.062(7) 0.036(5) -0.010(5) 0.001(4) 0.003(5) C99 0.025(4) 0.058(6) 0.044(5) -0.011(5) 0.011(4) -0.003(4) C100 0.033(5) 0.060(7) 0.051(6) 0.005(5) -0.002(4) -0.001(5) C101 0.040(5) 0.053(7) 0.062(7) -0.008(5) 0.014(5) -0.001(4) C102 0.025(4) 0.049(6) 0.038(5) 0.000(5) 0.002(4) 0.003(4) C103 0.021(4) 0.050(6) 0.045(6) 0.009(5) 0.008(4) 0.005(4) C104 0.041(5) 0.045(6) 0.048(6) 0.009(5) 0.004(5) 0.005(4) C105 0.041(5) 0.053(7) 0.049(6) 0.022(5) 0.001(5) 0.007(5) C106 0.032(5) 0.061(7) 0.046(6) -0.010(5) -0.001(4) -0.007(5) C107 0.030(5) 0.037(6) 0.039(5) 0.006(4) 0.005(4) 0.002(4) C108 0.034(5) 0.051(6) 0.038(5) 0.002(4) 0.010(4) -0.008(4) C109 0.056(6) 0.049(7) 0.069(7) -0.005(5) 0.022(6) 0.001(5) C110 0.052(6) 0.041(6) 0.049(6) 0.002(5) -0.002(5) -0.017(4) C111 0.055(6) 0.065(9) 0.042(6) -0.004(5) -0.016(5) -0.007(5) C112 0.123(13) 0.069(11) 0.28(2) -0.001(14) 0.094(15) -0.048(10) C113 0.155(14) 0.057(9) 0.091(10) -0.018(7) -0.005(10) -0.011(8) C114 0.030(4) 0.026(5) 0.049(5) -0.006(4) 0.011(4) 0.001(4) C115 0.039(5) 0.029(5) 0.042(5) 0.005(4) -0.008(4) -0.005(4) C116 0.034(5) 0.038(6) 0.053(6) -0.001(5) 0.002(5) 0.004(4) C117 0.046(6) 0.053(7) 0.063(7) 0.023(6) -0.001(5) 0.025(5) C118 0.058(7) 0.069(8) 0.060(7) 0.036(6) -0.007(6) 0.006(6) C119 0.064(7) 0.065(7) 0.043(6) 0.018(5) 0.008(5) 0.025(6) C120 0.039(5) 0.033(5) 0.051(6) 0.011(4) 0.009(4) 0.000(4) C121 0.032(5) 0.046(6) 0.060(7) 0.000(5) -0.003(5) 0.009(4) C122 0.055(6) 0.041(6) 0.066(7) -0.006(5) -0.001(5) 0.006(5) C123 0.047(6) 0.047(7) 0.067(7) -0.011(6) 0.010(5) 0.006(5) C124 0.067(7) 0.050(7) 0.040(6) 0.024(5) 0.019(5) 0.013(5) C125 0.055(7) 0.118(11) 0.086(9) -0.002(8) 0.023(7) 0.010(7) C126 0.138(12) 0.047(7) 0.058(7) 0.007(6) 0.048(7) 0.026(7) C127 0.035(5) 0.022(5) 0.044(5) 0.003(4) -0.009(4) 0.000(4) C128 0.039(5) 0.030(5) 0.067(7) -0.020(5) -0.004(5) -0.001(4) C129 0.023(5) 0.049(7) 0.102(9) -0.021(6) -0.010(5) -0.001(4) C130 0.061(7) 0.055(8) 0.056(7) -0.019(6) -0.015(6) -0.003(6) C131 0.068(7) 0.052(7) 0.055(7) 0.001(5) -0.006(6) -0.006(6) C132 0.048(6) 0.036(6) 0.051(6) -0.015(5) -0.005(5) -0.009(4) C133 0.039(5) 0.041(6) 0.096(9) -0.014(6) 0.015(6) -0.006(5) C134 0.066(8) 0.090(10) 0.116(11) 0.003(8) 0.025(8) -0.020(7) C135 0.038(6) 0.099(10) 0.113(11) -0.039(8) 0.010(7) 0.003(6) C136 0.053(6) 0.078(8) 0.035(5) -0.010(5) 0.003(5) -0.022(6) C137 0.054(7) 0.098(10) 0.059(7) 0.016(7) 0.009(6) -0.016(6) C138 0.094(9) 0.088(9) 0.035(6) -0.007(6) 0.019(6) -0.028(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N1 2.449(6) . ? Sm1 N4 2.453(7) . ? Sm1 N3 2.464(7) . ? Sm1 N2 2.466(7) . ? Sm1 N6 2.470(6) . ? Sm1 N5 2.474(7) . ? Sm1 C20 2.832(8) . ? Sm1 C1 2.832(9) . ? Sm1 C45 2.846(9) . ? Sm2 N8 2.429(7) . ? Sm2 N7 2.443(7) . ? Sm2 N12 2.444(7) . ? Sm2 N11 2.451(7) . ? Sm2 N9 2.451(6) . ? Sm2 N10 2.476(7) . ? Sm2 C70 2.819(8) . ? Sm2 C114 2.820(9) . ? Sm2 C89 2.839(9) . ? N1 C1 1.345(11) . ? N1 C2 1.420(9) . ? N2 C1 1.321(10) . ? N2 C11 1.438(10) . ? N3 C20 1.333(10) . ? N3 C21 1.448(10) . ? N4 C20 1.315(11) . ? N4 C33 1.444(10) . ? N5 C45 1.336(10) . ? N5 C46 1.432(11) . ? N6 C45 1.339(10) . ? N6 C58 1.434(10) . ? N7 C70 1.311(10) . ? N7 C71 1.444(10) . ? N8 C70 1.321(11) . ? N8 C80 1.444(10) . ? N9 C89 1.327(11) . ? N9 C90 1.436(10) . ? N10 C89 1.294(10) . ? N10 C102 1.436(11) . ? N11 C114 1.304(10) . ? N11 C115 1.453(11) . ? N12 C114 1.330(11) . ? N12 C127 1.416(11) . ? C2 C7 1.392(11) . ? C2 C3 1.410(11) . ? C3 C4 1.391(12) . ? C3 C8 1.500(12) . ? C4 C5 1.374(13) . ? C5 C6 1.377(13) . ? C5 C9 1.532(11) . ? C6 C7 1.380(11) . ? C7 C10 1.519(12) . ? C11 C16 1.387(14) . ? C11 C12 1.392(12) . ? C12 C13 1.404(12) . ? C12 C17 1.494(13) . ? C13 C14 1.356(12) . ? C14 C15 1.384(12) . ? C14 C18 1.516(12) . ? C15 C16 1.435(12) . ? C16 C19 1.519(12) . ? C21 C26 1.393(12) . ? C21 C22 1.438(13) . ? C22 C23 1.383(13) . ? C22 C27 1.491(14) . ? C23 C24 1.374(14) . ? C24 C25 1.343(14) . ? C25 C26 1.384(12) . ? C26 C30 1.525(12) . ? C27 C28 1.474(17) . ? C27 C29 1.540(17) . ? C30 C31 1.524(12) . ? C30 C32 1.539(11) . ? C33 C34 1.406(12) . ? C33 C38 1.413(10) . ? C34 C35 1.380(11) . ? C34 C39 1.533(11) . ? C35 C36 1.392(11) . ? C36 C37 1.399(12) . ? C37 C38 1.399(12) . ? C38 C42 1.507(12) . ? C39 C40 1.490(13) . ? C39 C41 1.537(12) . ? C42 C43 1.540(12) . ? C42 C44 1.560(12) . ? C46 C47 1.415(13) . ? C46 C51 1.426(12) . ? C47 C48 1.417(13) . ? C47 C52 1.481(13) . ? C48 C49 1.368(14) . ? C49 C50 1.336(15) . ? C50 C51 1.402(13) . ? C51 C55 1.499(13) . ? C52 C53 1.505(14) . ? C52 C54 1.536(16) . ? C55 C57 1.513(13) . ? C55 C56 1.526(12) . ? C58 C63 1.383(12) . ? C58 C59 1.431(12) . ? C59 C60 1.402(13) . ? C59 C64 1.527(13) . ? C60 C61 1.372(14) . ? C61 C62 1.395(14) . ? C62 C63 1.418(13) . ? C63 C67 1.520(12) . ? C64 C66 1.537(14) . ? C64 C65 1.546(13) . ? C67 C68 1.527(13) . ? C67 C69 1.533(13) . ? C71 C76 1.412(13) . ? C71 C72 1.420(13) . ? C72 C73 1.409(12) . ? C72 C77 1.500(12) . ? C73 C74 1.375(12) . ? C74 C75 1.369(12) . ? C74 C78 1.503(12) . ? C75 C76 1.412(12) . ? C76 C79 1.498(12) . ? C80 C81 1.390(13) . ? C80 C85 1.400(13) . ? C81 C82 1.375(12) . ? C81 C86 1.516(13) . ? C82 C83 1.397(14) . ? C83 C84 1.397(15) . ? C83 C87 1.519(12) . ? C84 C85 1.367(13) . ? C85 C88 1.525(14) . ? C90 C91 1.402(12) . ? C90 C95 1.417(11) . ? C91 C92 1.386(11) . ? C91 C96 1.528(11) . ? C92 C93 1.398(12) . ? C93 C94 1.355(13) . ? C94 C95 1.399(12) . ? C95 C99 1.536(12) . ? C96 C97 1.519(13) . ? C96 C98 1.558(12) . ? C99 C100 1.506(13) . ? C99 C101 1.560(13) . ? C102 C107 1.397(12) . ? C102 C103 1.442(13) . ? C103 C104 1.404(13) . ? C103 C108 1.523(12) . ? C104 C105 1.377(14) . ? C105 C106 1.390(14) . ? C106 C107 1.363(13) . ? C107 C111 1.525(13) . ? C108 C109 1.564(12) . ? C108 C110 1.567(12) . ? C111 C113 1.503(16) . ? C111 C112 1.514(16) . ? C115 C116 1.402(13) . ? C115 C120 1.416(13) . ? C116 C117 1.405(14) . ? C116 C121 1.516(14) . ? C117 C118 1.312(16) . ? C118 C119 1.365(15) . ? C119 C120 1.387(13) . ? C120 C124 1.532(13) . ? C121 C122 1.506(13) . ? C121 C123 1.577(13) . ? C124 C125 1.521(16) . ? C124 C126 1.526(14) . ? C127 C128 1.400(13) . ? C127 C132 1.411(13) . ? C128 C129 1.410(13) . ? C128 C133 1.502(15) . ? C129 C130 1.390(16) . ? C130 C131 1.373(16) . ? C131 C132 1.437(13) . ? C132 C136 1.535(13) . ? C133 C134 1.567(16) . ? C133 C135 1.567(14) . ? C136 C137 1.535(16) . ? C136 C138 1.552(13) . ? 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 N4 141.2(2) . . ? N1 Sm1 N3 96.9(2) . . ? N4 Sm1 N3 55.7(2) . . ? N1 Sm1 N2 56.1(2) . . ? N4 Sm1 N2 104.8(2) . . ? N3 Sm1 N2 111.2(2) . . ? N1 Sm1 N6 110.9(2) . . ? N4 Sm1 N6 104.6(2) . . ? N3 Sm1 N6 148.1(2) . . ? N2 Sm1 N6 97.5(2) . . ? N1 Sm1 N5 101.1(2) . . ? N4 Sm1 N5 111.6(2) . . ? N3 Sm1 N5 104.7(2) . . ? N2 Sm1 N5 139.0(2) . . ? N6 Sm1 N5 56.0(2) . . ? N1 Sm1 C20 120.0(2) . . ? N4 Sm1 C20 27.6(2) . . ? N3 Sm1 C20 28.1(2) . . ? N2 Sm1 C20 109.1(2) . . ? N6 Sm1 C20 129.1(2) . . ? N5 Sm1 C20 111.9(2) . . ? N1 Sm1 C1 28.3(2) . . ? N4 Sm1 C1 125.8(2) . . ? N3 Sm1 C1 106.0(2) . . ? N2 Sm1 C1 27.8(2) . . ? N6 Sm1 C1 105.9(2) . . ? N5 Sm1 C1 122.6(2) . . ? C20 Sm1 C1 117.9(2) . . ? N1 Sm1 C45 106.8(2) . . ? N4 Sm1 C45 111.9(2) . . ? N3 Sm1 C45 129.4(2) . . ? N2 Sm1 C45 119.2(2) . . ? N6 Sm1 C45 28.1(2) . . ? N5 Sm1 C45 28.0(2) . . ? C20 Sm1 C45 125.9(2) . . ? C1 Sm1 C45 116.2(2) . . ? N8 Sm2 N7 55.6(2) . . ? N8 Sm2 N12 98.8(2) . . ? N7 Sm2 N12 137.9(2) . . ? N8 Sm2 N11 109.7(2) . . ? N7 Sm2 N11 98.6(2) . . ? N12 Sm2 N11 55.7(2) . . ? N8 Sm2 N9 142.2(2) . . ? N7 Sm2 N9 105.4(2) . . ? N12 Sm2 N9 112.9(2) . . ? N11 Sm2 N9 105.1(2) . . ? N8 Sm2 N10 99.0(2) . . ? N7 Sm2 N10 112.1(2) . . ? N12 Sm2 N10 104.0(2) . . ? N11 Sm2 N10 146.5(2) . . ? N9 Sm2 N10 54.8(2) . . ? N8 Sm2 C70 27.9(2) . . ? N7 Sm2 C70 27.7(2) . . ? N12 Sm2 C70 120.2(2) . . ? N11 Sm2 C70 105.5(2) . . ? N9 Sm2 C70 126.9(2) . . ? N10 Sm2 C70 108.0(2) . . ? N8 Sm2 C114 106.2(2) . . ? N7 Sm2 C114 120.0(2) . . ? N12 Sm2 C114 28.1(2) . . ? N11 Sm2 C114 27.5(2) . . ? N9 Sm2 C114 111.5(2) . . ? N10 Sm2 C114 127.7(2) . . ? C70 Sm2 C114 115.7(2) . . ? N8 Sm2 C89 120.9(3) . . ? N7 Sm2 C89 109.5(2) . . ? N12 Sm2 C89 112.5(2) . . ? N11 Sm2 C89 129.4(2) . . ? N9 Sm2 C89 27.8(2) . . ? N10 Sm2 C89 27.1(2) . . ? C70 Sm2 C89 119.1(2) . . ? C114 Sm2 C89 125.2(2) . . ? C1 N1 C2 114.9(6) . . ? C1 N1 Sm1 91.9(5) . . ? C2 N1 Sm1 152.7(5) . . ? C1 N2 C11 115.4(7) . . ? C1 N2 Sm1 91.7(5) . . ? C11 N2 Sm1 152.9(5) . . ? C20 N3 C21 117.1(7) . . ? C20 N3 Sm1 91.5(5) . . ? C21 N3 Sm1 150.5(5) . . ? C20 N4 C33 117.9(7) . . ? C20 N4 Sm1 92.4(5) . . ? C33 N4 Sm1 149.3(5) . . ? C45 N5 C46 116.7(7) . . ? C45 N5 Sm1 91.7(5) . . ? C46 N5 Sm1 151.5(6) . . ? C45 N6 C58 117.4(7) . . ? C45 N6 Sm1 91.8(5) . . ? C58 N6 Sm1 150.7(5) . . ? C70 N7 C71 114.9(7) . . ? C70 N7 Sm2 92.3(5) . . ? C71 N7 Sm2 152.8(5) . . ? C70 N8 C80 115.0(7) . . ? C70 N8 Sm2 92.7(5) . . ? C80 N8 Sm2 152.0(5) . . ? C89 N9 C90 119.1(7) . . ? C89 N9 Sm2 92.6(5) . . ? C90 N9 Sm2 148.0(5) . . ? C89 N10 C102 119.3(7) . . ? C89 N10 Sm2 92.3(5) . . ? C102 N10 Sm2 147.3(5) . . ? C114 N11 C115 116.7(7) . . ? C114 N11 Sm2 92.2(5) . . ? C115 N11 Sm2 151.1(5) . . ? C114 N12 C127 117.7(7) . . ? C114 N12 Sm2 91.8(5) . . ? C127 N12 Sm2 150.3(6) . . ? N2 C1 N1 120.3(8) . . ? N2 C1 Sm1 60.5(4) . . ? N1 C1 Sm1 59.8(4) . . ? C7 C2 C3 119.3(7) . . ? C7 C2 N1 119.6(7) . . ? C3 C2 N1 121.1(7) . . ? C4 C3 C2 118.8(8) . . ? C4 C3 C8 121.1(8) . . ? C2 C3 C8 120.0(7) . . ? C5 C4 C3 122.1(8) . . ? C4 C5 C6 117.9(7) . . ? C4 C5 C9 121.0(9) . . ? C6 C5 C9 121.1(9) . . ? C5 C6 C7 122.6(9) . . ? C6 C7 C2 119.3(8) . . ? C6 C7 C10 120.3(8) . . ? C2 C7 C10 120.4(7) . . ? C16 C11 C12 119.7(8) . . ? C16 C11 N2 121.4(8) . . ? C12 C11 N2 118.8(9) . . ? C11 C12 C13 119.6(9) . . ? C11 C12 C17 120.8(8) . . ? C13 C12 C17 119.5(8) . . ? C14 C13 C12 121.7(8) . . ? C13 C14 C15 119.6(8) . . ? C13 C14 C18 121.6(8) . . ? C15 C14 C18 118.8(8) . . ? C14 C15 C16 120.1(8) . . ? C11 C16 C15 119.2(8) . . ? C11 C16 C19 122.4(8) . . ? C15 C16 C19 118.3(8) . . ? N4 C20 N3 120.2(7) . . ? N4 C20 Sm1 59.9(4) . . ? N3 C20 Sm1 60.4(4) . . ? C26 C21 C22 121.2(8) . . ? C26 C21 N3 122.4(8) . . ? C22 C21 N3 116.2(8) . . ? C23 C22 C21 117.0(9) . . ? C23 C22 C27 122.3(9) . . ? C21 C22 C27 120.7(8) . . ? C24 C23 C22 121.0(9) . . ? C25 C24 C23 121.0(9) . . ? C24 C25 C26 122.2(9) . . ? C25 C26 C21 117.5(9) . . ? C25 C26 C30 119.4(8) . . ? C21 C26 C30 123.0(8) . . ? C28 C27 C22 109.9(11) . . ? C28 C27 C29 110.5(11) . . ? C22 C27 C29 113.2(9) . . ? C31 C30 C26 111.6(7) . . ? C31 C30 C32 110.0(7) . . ? C26 C30 C32 112.3(7) . . ? C34 C33 C38 121.2(7) . . ? C34 C33 N4 118.6(6) . . ? C38 C33 N4 120.1(7) . . ? C35 C34 C33 119.1(7) . . ? C35 C34 C39 120.5(8) . . ? C33 C34 C39 120.1(7) . . ? C34 C35 C36 121.0(8) . . ? C35 C36 C37 119.7(8) . . ? C36 C37 C38 121.0(8) . . ? C37 C38 C33 117.9(8) . . ? C37 C38 C42 117.3(7) . . ? C33 C38 C42 124.7(7) . . ? C40 C39 C34 111.1(7) . . ? C40 C39 C41 110.9(7) . . ? C34 C39 C41 111.5(7) . . ? C38 C42 C43 114.4(8) . . ? C38 C42 C44 111.0(7) . . ? C43 C42 C44 109.1(7) . . ? N5 C45 N6 120.3(8) . . ? N5 C45 Sm1 60.3(4) . . ? N6 C45 Sm1 60.2(4) . . ? C47 C46 C51 121.3(8) . . ? C47 C46 N5 119.0(8) . . ? C51 C46 N5 119.6(8) . . ? C46 C47 C48 117.8(8) . . ? C46 C47 C52 123.3(8) . . ? C48 C47 C52 118.9(8) . . ? C49 C48 C47 119.6(9) . . ? C50 C49 C48 122.5(10) . . ? C49 C50 C51 122.1(9) . . ? C50 C51 C46 116.6(9) . . ? C50 C51 C55 119.9(8) . . ? C46 C51 C55 123.5(8) . . ? C47 C52 C53 115.1(9) . . ? C47 C52 C54 110.0(9) . . ? C53 C52 C54 110.9(9) . . ? C51 C55 C57 111.6(8) . . ? C51 C55 C56 113.1(8) . . ? C57 C55 C56 107.9(8) . . ? C63 C58 C59 121.9(8) . . ? C63 C58 N6 117.8(7) . . ? C59 C58 N6 120.3(8) . . ? C60 C59 C58 117.5(9) . . ? C60 C59 C64 119.6(9) . . ? C58 C59 C64 123.0(8) . . ? C61 C60 C59 121.5(9) . . ? C60 C61 C62 120.4(9) . . ? C61 C62 C63 120.4(9) . . ? C58 C63 C62 118.3(8) . . ? C58 C63 C67 121.3(8) . . ? C62 C63 C67 120.4(8) . . ? C59 C64 C66 110.7(8) . . ? C59 C64 C65 110.5(9) . . ? C66 C64 C65 108.8(8) . . ? C63 C67 C68 109.3(8) . . ? C63 C67 C69 112.9(8) . . ? C68 C67 C69 108.0(8) . . ? N7 C70 N8 119.3(7) . . ? N7 C70 Sm2 60.0(4) . . ? N8 C70 Sm2 59.4(4) . . ? C76 C71 C72 119.5(8) . . ? C76 C71 N7 120.4(8) . . ? C72 C71 N7 120.0(9) . . ? C73 C72 C71 118.7(8) . . ? C73 C72 C77 120.9(9) . . ? C71 C72 C77 120.4(8) . . ? C74 C73 C72 122.4(9) . . ? C75 C74 C73 118.0(8) . . ? C75 C74 C78 121.1(9) . . ? C73 C74 C78 120.8(8) . . ? C74 C75 C76 123.4(8) . . ? C71 C76 C75 117.9(8) . . ? C71 C76 C79 121.8(8) . . ? C75 C76 C79 120.3(8) . . ? C81 C80 C85 119.5(8) . . ? C81 C80 N8 120.7(8) . . ? C85 C80 N8 119.7(8) . . ? C82 C81 C80 120.0(9) . . ? C82 C81 C86 120.9(9) . . ? C80 C81 C86 119.1(8) . . ? C81 C82 C83 121.7(9) . . ? C84 C83 C82 116.7(8) . . ? C84 C83 C87 122.9(11) . . ? C82 C83 C87 120.3(10) . . ? C85 C84 C83 122.9(10) . . ? C84 C85 C80 118.9(9) . . ? C84 C85 C88 120.3(9) . . ? C80 C85 C88 120.7(8) . . ? N10 C89 N9 119.9(8) . . ? N10 C89 Sm2 60.6(4) . . ? N9 C89 Sm2 59.6(4) . . ? C91 C90 C95 119.7(7) . . ? C91 C90 N9 119.2(7) . . ? C95 C90 N9 121.1(8) . . ? C92 C91 C90 119.5(7) . . ? C92 C91 C96 120.1(8) . . ? C90 C91 C96 120.4(7) . . ? C91 C92 C93 120.9(8) . . ? C94 C93 C92 119.2(8) . . ? C93 C94 C95 122.4(8) . . ? C94 C95 C90 118.2(8) . . ? C94 C95 C99 119.0(7) . . ? C90 C95 C99 122.8(7) . . ? C97 C96 C91 108.6(7) . . ? C97 C96 C98 110.6(8) . . ? C91 C96 C98 114.2(7) . . ? C100 C99 C95 113.0(8) . . ? C100 C99 C101 109.6(7) . . ? C95 C99 C101 109.3(8) . . ? C107 C102 N10 120.3(8) . . ? C107 C102 C103 119.4(8) . . ? N10 C102 C103 120.2(8) . . ? C104 C103 C102 118.0(9) . . ? C104 C103 C108 119.2(9) . . ? C102 C103 C108 122.8(8) . . ? C105 C104 C103 121.3(9) . . ? C104 C105 C106 119.2(9) . . ? C107 C106 C105 122.1(9) . . ? C106 C107 C102 119.9(9) . . ? C106 C107 C111 119.8(8) . . ? C102 C107 C111 120.3(8) . . ? C103 C108 C109 111.2(7) . . ? C103 C108 C110 112.1(7) . . ? C109 C108 C110 108.2(8) . . ? C113 C111 C112 112.1(12) . . ? C113 C111 C107 113.3(9) . . ? C112 C111 C107 109.0(10) . . ? N11 C114 N12 120.3(8) . . ? N11 C114 Sm2 60.3(5) . . ? N12 C114 Sm2 60.0(5) . . ? C116 C115 C120 119.4(8) . . ? C116 C115 N11 121.6(9) . . ? C120 C115 N11 119.0(8) . . ? C115 C116 C117 116.9(9) . . ? C115 C116 C121 122.7(9) . . ? C117 C116 C121 120.4(9) . . ? C118 C117 C116 123.6(10) . . ? C117 C118 C119 120.5(10) . . ? C118 C119 C120 120.4(10) . . ? C119 C120 C115 119.3(8) . . ? C119 C120 C124 119.9(8) . . ? C115 C120 C124 120.7(8) . . ? C122 C121 C116 111.9(9) . . ? C122 C121 C123 110.7(8) . . ? C116 C121 C123 110.5(8) . . ? C125 C124 C126 114.5(10) . . ? C125 C124 C120 110.5(9) . . ? C126 C124 C120 113.2(9) . . ? C128 C127 C132 119.3(8) . . ? C128 C127 N12 121.9(9) . . ? C132 C127 N12 118.8(8) . . ? C127 C128 C129 119.6(10) . . ? C127 C128 C133 121.9(8) . . ? C129 C128 C133 118.5(9) . . ? C130 C129 C128 121.2(10) . . ? C131 C130 C129 120.4(10) . . ? C130 C131 C132 119.6(11) . . ? C127 C132 C131 120.0(9) . . ? C127 C132 C136 121.0(8) . . ? C131 C132 C136 119.0(9) . . ? C128 C133 C134 109.9(9) . . ? C128 C133 C135 112.8(10) . . ? C134 C133 C135 109.2(9) . . ? C137 C136 C132 110.1(9) . . ? C137 C136 C138 108.1(9) . . ? C132 C136 C138 112.2(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.219 _refine_diff_density_min -1.203 _refine_diff_density_rms 0.099 # Attachment '4.CIF' data_jun11 _database_code_depnum_ccdc_archive 'CCDC 752059' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H99 N6 Sm' _chemical_formula_sum 'C70 H99 N6 Sm' _chemical_formula_weight 1174.90 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 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 12.5418(2) _cell_length_b 13.3499(2) _cell_length_c 21.3672(4) _cell_angle_alpha 77.583(1) _cell_angle_beta 82.913(1) _cell_angle_gamma 63.814(1) _cell_volume 3133.62(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8752 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 26.17 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1246 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 X8 Apex CCD' _diffrn_measurement_method 'thin slice phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30274 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14016 _reflns_number_gt 11413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 v2.0' _computing_cell_refinement 'Bruker Apex2 v2.0' _computing_data_reduction 'Bruker Apex2 v2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+4.8908P] 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 14016 _refine_ls_number_parameters 758 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.033 _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 0.765870(16) 0.646600(16) 0.747430(9) 0.017 Uani 1 1 d . . . N1 N 0.5683(3) 0.7940(3) 0.74237(15) 0.029 Uani 1 1 d . . . N2 N 0.5938(3) 0.6141(3) 0.77813(15) 0.029 Uani 1 1 d . . . N3 N 0.8352(3) 0.7277(2) 0.81872(13) 0.021 Uani 1 1 d . . . N4 N 0.8717(2) 0.5415(2) 0.84957(13) 0.022 Uani 1 1 d . A . N5 N 0.8843(2) 0.6618(2) 0.64517(13) 0.019 Uani 1 1 d . . . N6 N 0.7749(2) 0.5602(2) 0.65399(12) 0.018 Uani 1 1 d . . . C1 C 0.5199(3) 0.7240(3) 0.76887(18) 0.031 Uani 1 1 d . . . C2 C 0.4989(3) 0.9187(3) 0.73052(19) 0.034 Uani 1 1 d . . . H2 H 0.4377 0.9404 0.7659 0.041 Uiso 1 1 calc R . . C3 C 0.5820(4) 0.9736(3) 0.7299(2) 0.037 Uani 1 1 d . . . H3A H 0.6462 0.9473 0.6971 0.045 Uiso 1 1 calc R . . H3B H 0.6192 0.9488 0.7721 0.045 Uiso 1 1 calc R . . C4 C 0.5188(4) 1.1034(4) 0.7156(2) 0.050 Uani 1 1 d . . . H4A H 0.4604 1.1306 0.7508 0.060 Uiso 1 1 calc R . . H4B H 0.5777 1.1347 0.7135 0.060 Uiso 1 1 calc R . . C5 C 0.4552(4) 1.1458(4) 0.6527(2) 0.054 Uani 1 1 d . . . H5A H 0.4109 1.2295 0.6461 0.065 Uiso 1 1 calc R . . H5B H 0.5143 1.1260 0.6169 0.065 Uiso 1 1 calc R . . C6 C 0.3700(4) 1.0937(4) 0.6530(2) 0.055 Uani 1 1 d . . . H6A H 0.3321 1.1194 0.6109 0.066 Uiso 1 1 calc R . . H6B H 0.3067 1.1189 0.6864 0.066 Uiso 1 1 calc R . . C7 C 0.4367(4) 0.9632(4) 0.6664(2) 0.047 Uani 1 1 d . . . H7A H 0.3796 0.9303 0.6668 0.057 Uiso 1 1 calc R . . H7B H 0.4965 0.9383 0.6314 0.057 Uiso 1 1 calc R . . C8 C 0.5574(3) 0.5233(3) 0.80486(18) 0.030 Uani 1 1 d . . . H8 H 0.5003 0.5460 0.8418 0.036 Uiso 1 1 calc R . . C9 C 0.4990(3) 0.4958(3) 0.75673(18) 0.031 Uani 1 1 d . . . H9A H 0.5541 0.4754 0.7194 0.037 Uiso 1 1 calc R . . H9B H 0.4264 0.5640 0.7413 0.037 Uiso 1 1 calc R . . C10 C 0.4658(4) 0.3978(3) 0.78610(19) 0.036 Uani 1 1 d . . . H10A H 0.4048 0.4207 0.8208 0.044 Uiso 1 1 calc R . . H10B H 0.4315 0.3801 0.7529 0.044 Uiso 1 1 calc R . . C11 C 0.5736(4) 0.2935(4) 0.8128(2) 0.042 Uani 1 1 d . . . H11A H 0.6300 0.2648 0.7771 0.051 Uiso 1 1 calc R . . H11B H 0.5490 0.2334 0.8347 0.051 Uiso 1 1 calc R . . C12 C 0.6353(4) 0.3194(4) 0.8597(2) 0.046 Uani 1 1 d . . . H12A H 0.7088 0.2512 0.8738 0.055 Uiso 1 1 calc R . . H12B H 0.5826 0.3388 0.8980 0.055 Uiso 1 1 calc R . . C13 C 0.6665(4) 0.4178(3) 0.82925(19) 0.036 Uani 1 1 d . . . H13A H 0.7041 0.4344 0.8613 0.043 Uiso 1 1 calc R . . H13B H 0.7245 0.3958 0.7932 0.043 Uiso 1 1 calc R . . C14 C 0.3875(4) 0.7687(4) 0.7872(2) 0.040 Uani 1 1 d . . . H14A H 0.3429 0.8306 0.7524 0.047 Uiso 1 1 calc R . . H14B H 0.3629 0.7069 0.7898 0.047 Uiso 1 1 calc R . . C15 C 0.3513(4) 0.8129(4) 0.8499(2) 0.041 Uani 1 1 d . . . C16 C 0.4219(5) 0.7669(4) 0.9020(2) 0.055 Uani 1 1 d . . . H16 H 0.4997 0.7082 0.8987 0.067 Uiso 1 1 calc R . . C17 C 0.3811(6) 0.8053(5) 0.9592(2) 0.074 Uani 1 1 d . . . H17 H 0.4319 0.7739 0.9946 0.089 Uiso 1 1 calc R . . C18 C 0.2680(6) 0.8883(6) 0.9657(3) 0.078 Uani 1 1 d . . . H18 H 0.2391 0.9124 1.0057 0.094 Uiso 1 1 calc R . . C19 C 0.1981(5) 0.9353(6) 0.9135(3) 0.090 Uani 1 1 d . . . H19 H 0.1204 0.9943 0.9162 0.108 Uiso 1 1 calc R . . C20 C 0.2409(4) 0.8965(5) 0.8574(3) 0.075 Uani 1 1 d . . . H20 H 0.1909 0.9298 0.8216 0.090 Uiso 1 1 calc R . . C21 C 0.8774(3) 0.6321(3) 0.86076(16) 0.022 Uani 1 1 d . . . H21 H 0.9115 0.6288 0.8989 0.027 Uiso 1 1 calc R . . C22 C 0.8483(3) 0.8239(3) 0.82883(16) 0.024 Uani 1 1 d . . . C31C C 0.7641(4) 0.9006(3) 0.86601(18) 0.035 Uani 1 1 d . . . C24 C 0.7793(4) 0.9955(3) 0.8713(2) 0.042 Uani 1 1 d . . . H24 H 0.7236 1.0475 0.8966 0.051 Uiso 1 1 calc R . . C25 C 0.8721(4) 1.0161(4) 0.8410(2) 0.049 Uani 1 1 d . . . H25 H 0.8809 1.0812 0.8456 0.059 Uiso 1 1 calc R . . C26 C 0.9526(4) 0.9418(4) 0.8038(2) 0.045 Uani 1 1 d . . . H26 H 1.0158 0.9574 0.7820 0.054 Uiso 1 1 calc R . . C27 C 0.9435(3) 0.8445(3) 0.79729(18) 0.030 Uani 1 1 d . . . C28 C 0.6591(4) 0.8823(4) 0.9016(2) 0.051 Uani 1 1 d . . . H28 H 0.6484 0.8246 0.8832 0.061 Uiso 1 1 calc R . . C29 C 0.6879(6) 0.8347(5) 0.9722(3) 0.092 Uani 1 1 d . . . H29A H 0.7631 0.7661 0.9758 0.137 Uiso 1 1 calc R . . H29B H 0.6241 0.8159 0.9945 0.137 Uiso 1 1 calc R . . H29C H 0.6949 0.8915 0.9917 0.137 Uiso 1 1 calc R . . C30 C 0.5417(5) 0.9886(4) 0.8974(3) 0.064 Uani 1 1 d . . . H30A H 0.5222 1.0206 0.8522 0.096 Uiso 1 1 calc R . . H30B H 0.5489 1.0446 0.9175 0.096 Uiso 1 1 calc R . . H30C H 0.4785 0.9689 0.9196 0.096 Uiso 1 1 calc R . . C31 C 1.0384(3) 0.7603(3) 0.75966(19) 0.032 Uani 1 1 d . . . H31 H 0.9993 0.7236 0.7403 0.039 Uiso 1 1 calc R . . C32 C 1.1319(4) 0.6670(3) 0.8053(2) 0.042 Uani 1 1 d . . . H32A H 1.1924 0.6121 0.7810 0.063 Uiso 1 1 calc R . . H32B H 1.0936 0.6284 0.8378 0.063 Uiso 1 1 calc R . . H32C H 1.1695 0.7010 0.8264 0.063 Uiso 1 1 calc R . . C33 C 1.0998(4) 0.8123(4) 0.7052(2) 0.045 Uani 1 1 d . . . H33A H 1.1588 0.7526 0.6831 0.067 Uiso 1 1 calc R . . H33B H 1.1395 0.8486 0.7227 0.067 Uiso 1 1 calc R . . H33C H 1.0405 0.8691 0.6747 0.067 Uiso 1 1 calc R . . C34 C 0.9142(3) 0.4401(3) 0.89768(19) 0.033 Uani 1 1 d . . . C35 C 1.0233(5) 0.3502(4) 0.8898(2) 0.025 Uani 0.71 1 d P A 1 C35' C 1.0012(13) 0.3384(11) 0.8643(6) 0.033 Uani 0.29 1 d P A 2 C36 C 1.0629(5) 0.2524(5) 0.9360(3) 0.036 Uani 0.71 1 d P A 1 H36 H 1.1361 0.1903 0.9287 0.044 Uiso 0.71 1 calc PR A 1 C36' C 1.0315(14) 0.2301(13) 0.9013(8) 0.056 Uani 0.29 1 d P A 2 H36' H 1.0922 0.1659 0.8861 0.068 Uiso 0.29 1 calc PR A 2 C37 C 0.9980(6) 0.2434(5) 0.9924(3) 0.040 Uani 0.71 1 d P A 1 H37 H 1.0255 0.1749 1.0230 0.048 Uiso 0.71 1 calc PR A 1 C37' C 0.9748(16) 0.2154(13) 0.9590(9) 0.066 Uani 0.29 1 d P A 2 H37' H 0.9953 0.1414 0.9834 0.079 Uiso 0.29 1 calc PR A 2 C38 C 0.8951(6) 0.3325(5) 1.0039(3) 0.035 Uani 0.71 1 d P A 1 H38 H 0.8531 0.3293 1.0439 0.042 Uiso 0.71 1 calc PR A 1 C38' C 0.8871(13) 0.3093(14) 0.9818(6) 0.042 Uani 0.29 1 d P A 2 H38' H 0.8446 0.2929 1.0195 0.050 Uiso 0.29 1 calc PR A 2 C39 C 0.8509(4) 0.4306(3) 0.95570(19) 0.036 Uani 1 1 d . A . C40 C 1.0969(5) 0.3551(5) 0.8282(3) 0.030 Uani 0.71 1 d PU A 1 H40 H 1.0836 0.4359 0.8134 0.036 Uiso 0.71 1 calc PR A 1 C40' C 1.0773(13) 0.3504(12) 0.8065(7) 0.031 Uani 0.29 1 d PU A 2 H40' H 1.0263 0.4172 0.7750 0.037 Uiso 0.29 1 calc PR A 2 C41 C 1.2292(5) 0.2847(6) 0.8350(3) 0.038 Uani 0.71 1 d PU A 1 H41A H 1.2571 0.3074 0.8680 0.057 Uiso 0.71 1 calc PR A 1 H41B H 1.2703 0.2968 0.7940 0.057 Uiso 0.71 1 calc PR A 1 H41C H 1.2459 0.2042 0.8473 0.057 Uiso 0.71 1 calc PR A 1 C41' C 1.1717(14) 0.3775(15) 0.8262(8) 0.055 Uani 0.29 1 d PU A 2 H41D H 1.1339 0.4440 0.8471 0.083 Uiso 0.29 1 calc PR A 2 H41E H 1.2179 0.3936 0.7881 0.083 Uiso 0.29 1 calc PR A 2 H41F H 1.2246 0.3125 0.8561 0.083 Uiso 0.29 1 calc PR A 2 C42 C 1.0513(6) 0.3234(7) 0.7781(3) 0.053 Uani 0.71 1 d PU A 1 H42A H 1.0982 0.3270 0.7381 0.080 Uiso 0.71 1 calc PR A 1 H42B H 0.9678 0.3762 0.7708 0.080 Uiso 0.71 1 calc PR A 1 H42C H 1.0580 0.2461 0.7923 0.080 Uiso 0.71 1 calc PR A 1 C42' C 1.1338(15) 0.2502(13) 0.7728(7) 0.048 Uani 0.29 1 d PU A 2 H42D H 1.1800 0.2672 0.7351 0.072 Uiso 0.29 1 calc PR A 2 H42E H 1.0718 0.2343 0.7594 0.072 Uiso 0.29 1 calc PR A 2 H42F H 1.1865 0.1838 0.8021 0.072 Uiso 0.29 1 calc PR A 2 C43 C 0.7435(4) 0.5260(4) 0.97707(18) 0.037 Uani 1 1 d . . . H43 H 0.7217 0.5932 0.9415 0.044 Uiso 1 1 calc R A . C44 C 0.6378(4) 0.4967(4) 0.9923(2) 0.050 Uani 1 1 d . A . H44A H 0.5691 0.5613 1.0058 0.075 Uiso 1 1 calc R . . H44B H 0.6576 0.4305 1.0270 0.075 Uiso 1 1 calc R . . H44C H 0.6186 0.4793 0.9541 0.075 Uiso 1 1 calc R . . C45 C 0.7670(6) 0.5594(5) 1.0362(2) 0.084 Uani 1 1 d . A . H45A H 0.6950 0.6224 1.0487 0.126 Uiso 1 1 calc R . . H45B H 0.8318 0.5831 1.0263 0.126 Uiso 1 1 calc R . . H45C H 0.7894 0.4943 1.0716 0.126 Uiso 1 1 calc R . . C46 C 0.8433(3) 0.6040(3) 0.61903(16) 0.019 Uani 1 1 d . . . H46 H 0.8632 0.5945 0.5757 0.023 Uiso 1 1 calc R . . C47 C 0.9631(3) 0.7024(3) 0.60612(16) 0.021 Uani 1 1 d . . . C48 C 1.0816(3) 0.6278(3) 0.59424(16) 0.026 Uani 1 1 d . . . C49 C 1.1579(4) 0.6693(4) 0.55706(18) 0.035 Uani 1 1 d . . . H49 H 1.2377 0.6183 0.5489 0.042 Uiso 1 1 calc R . . C50 C 1.1192(4) 0.7826(4) 0.5321(2) 0.044 Uani 1 1 d . . . H50 H 1.1722 0.8103 0.5075 0.052 Uiso 1 1 calc R . . C51 C 1.0044(4) 0.8549(4) 0.54285(19) 0.040 Uani 1 1 d . . . H51 H 0.9780 0.9331 0.5247 0.048 Uiso 1 1 calc R . . C52 C 0.9239(3) 0.8183(3) 0.57979(18) 0.029 Uani 1 1 d . . . C53 C 1.1329(3) 0.5009(3) 0.62001(17) 0.028 Uani 1 1 d . . . H53 H 1.0680 0.4832 0.6443 0.034 Uiso 1 1 calc R . . C54 C 1.2317(4) 0.4662(4) 0.6659(2) 0.055 Uani 1 1 d . . . H54A H 1.2009 0.5095 0.7009 0.082 Uiso 1 1 calc R . . H54B H 1.2969 0.4818 0.6429 0.082 Uiso 1 1 calc R . . H54C H 1.2611 0.3849 0.6835 0.082 Uiso 1 1 calc R . . C55 C 1.1787(5) 0.4328(4) 0.5664(2) 0.058 Uani 1 1 d . . . H55A H 1.2103 0.3516 0.5846 0.088 Uiso 1 1 calc R . . H55B H 1.2420 0.4495 0.5417 0.088 Uiso 1 1 calc R . . H55C H 1.1136 0.4531 0.5382 0.088 Uiso 1 1 calc R . . C56 C 0.7985(4) 0.9052(3) 0.5881(2) 0.036 Uani 1 1 d . . . H56 H 0.7541 0.8669 0.6179 0.044 Uiso 1 1 calc R . . C57 C 0.7963(4) 1.0009(3) 0.6181(2) 0.049 Uani 1 1 d . . . H57A H 0.7139 1.0567 0.6229 0.073 Uiso 1 1 calc R . . H57B H 0.8416 1.0380 0.5903 0.073 Uiso 1 1 calc R . . H57C H 0.8321 0.9691 0.6603 0.073 Uiso 1 1 calc R . . C58 C 0.7363(4) 0.9531(4) 0.5234(2) 0.054 Uani 1 1 d . . . H58A H 0.6544 1.0088 0.5297 0.081 Uiso 1 1 calc R . . H58B H 0.7356 0.8911 0.5061 0.081 Uiso 1 1 calc R . . H58C H 0.7793 0.9899 0.4932 0.081 Uiso 1 1 calc R . . C59 C 0.7221(3) 0.5059(3) 0.62537(15) 0.021 Uani 1 1 d . . . C60 C 0.6089(3) 0.5701(3) 0.59832(16) 0.024 Uani 1 1 d . . . C61 C 0.5555(3) 0.5133(3) 0.57583(17) 0.029 Uani 1 1 d . . . H61 H 0.4804 0.5558 0.5565 0.035 Uiso 1 1 calc R . . C62 C 0.6086(4) 0.3977(3) 0.58087(18) 0.034 Uani 1 1 d . . . H62 H 0.5696 0.3605 0.5662 0.041 Uiso 1 1 calc R . . C63 C 0.7181(4) 0.3360(3) 0.60710(18) 0.034 Uani 1 1 d . . . H63 H 0.7546 0.2559 0.6103 0.041 Uiso 1 1 calc R . . C64 C 0.7774(3) 0.3876(3) 0.62918(17) 0.026 Uani 1 1 d . . . C65 C 0.5463(3) 0.6983(3) 0.59311(17) 0.026 Uani 1 1 d . . . H65 H 0.5704 0.7181 0.6299 0.032 Uiso 1 1 calc R . . C66 C 0.4110(3) 0.7438(4) 0.5964(2) 0.041 Uani 1 1 d . . . H66A H 0.3753 0.8264 0.5931 0.062 Uiso 1 1 calc R . . H66B H 0.3859 0.7095 0.6374 0.062 Uiso 1 1 calc R . . H66C H 0.3851 0.7247 0.5610 0.062 Uiso 1 1 calc R . . C67 C 0.5844(4) 0.7576(3) 0.5313(2) 0.040 Uani 1 1 d . . . H67A H 0.5432 0.8399 0.5291 0.060 Uiso 1 1 calc R . . H67B H 0.5639 0.7376 0.4944 0.060 Uiso 1 1 calc R . . H67C H 0.6704 0.7333 0.5307 0.060 Uiso 1 1 calc R . . C68 C 0.9012(4) 0.3160(3) 0.6546(2) 0.039 Uani 1 1 d . . . H68 H 0.9197 0.3622 0.6791 0.046 Uiso 1 1 calc R . . C69 C 0.9099(5) 0.2084(4) 0.7005(3) 0.072 Uani 1 1 d . . . H69A H 0.9910 0.1651 0.7160 0.109 Uiso 1 1 calc R . . H69B H 0.8906 0.1621 0.6780 0.109 Uiso 1 1 calc R . . H69C H 0.8539 0.2286 0.7369 0.109 Uiso 1 1 calc R . . C70 C 0.9913(4) 0.2887(6) 0.6000(3) 0.086 Uani 1 1 d . . . H70A H 1.0709 0.2428 0.6171 0.129 Uiso 1 1 calc R . . H70B H 0.9884 0.3593 0.5733 0.129 Uiso 1 1 calc R . . H70C H 0.9732 0.2462 0.5741 0.129 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 0.017 0.018 0.018 -0.005 0.001 -0.007 N1 0.024 0.026 0.037 -0.008 -0.001 -0.008 N2 0.027 0.033 0.033 -0.011 0.005 -0.017 N3 0.027 0.019 0.016 -0.003 0.000 -0.010 N4 0.021 0.019 0.021 0.003 -0.001 -0.008 N5 0.019 0.018 0.018 -0.001 0.000 -0.008 N6 0.016 0.021 0.016 -0.006 0.001 -0.008 C1 0.019 0.043 0.032 -0.017 0.004 -0.011 C2 0.027 0.031 0.036 -0.015 -0.004 0.000 C3 0.042 0.029 0.035 -0.010 -0.001 -0.008 C4 0.059 0.032 0.051 -0.010 -0.005 -0.011 C5 0.055 0.029 0.060 -0.006 -0.009 0.000 C6 0.046 0.041 0.059 -0.001 -0.019 -0.001 C7 0.046 0.044 0.047 -0.008 -0.013 -0.012 C8 0.031 0.040 0.025 -0.012 0.009 -0.021 C9 0.030 0.035 0.032 -0.009 0.000 -0.017 C10 0.040 0.047 0.036 -0.008 -0.001 -0.030 C11 0.055 0.039 0.043 -0.003 -0.005 -0.030 C12 0.058 0.044 0.042 0.002 -0.016 -0.028 C13 0.041 0.045 0.030 -0.003 -0.006 -0.028 C14 0.028 0.044 0.050 -0.020 0.004 -0.016 C15 0.036 0.050 0.043 -0.014 0.007 -0.025 C16 0.064 0.058 0.041 -0.001 -0.001 -0.027 C17 0.100 0.093 0.038 -0.005 -0.005 -0.052 C18 0.095 0.123 0.051 -0.049 0.038 -0.073 C19 0.050 0.133 0.100 -0.084 0.021 -0.027 C20 0.030 0.114 0.076 -0.063 0.005 -0.007 C21 0.019 0.030 0.018 -0.005 0.001 -0.010 C22 0.029 0.024 0.019 0.001 -0.007 -0.011 C31C 0.048 0.032 0.022 -0.007 -0.002 -0.015 C24 0.065 0.026 0.036 -0.012 -0.011 -0.014 C25 0.056 0.026 0.072 -0.010 -0.019 -0.019 C26 0.040 0.033 0.068 0.000 -0.013 -0.022 C27 0.030 0.027 0.035 -0.001 -0.009 -0.013 C28 0.064 0.037 0.048 -0.018 0.024 -0.019 C29 0.107 0.064 0.052 0.001 0.034 -0.004 C30 0.064 0.061 0.062 -0.028 0.029 -0.023 C31 0.024 0.035 0.042 -0.006 0.000 -0.016 C32 0.026 0.035 0.050 0.002 0.004 -0.005 C33 0.043 0.062 0.039 0.001 -0.004 -0.035 C34 0.025 0.026 0.039 0.010 -0.003 -0.011 C35 0.026 0.026 0.019 0.003 -0.008 -0.009 C35' 0.039 0.030 0.025 0.010 -0.018 -0.013 C36 0.032 0.028 0.039 0.002 -0.001 -0.007 C36' 0.030 0.035 0.064 0.011 0.014 0.009 C37 0.050 0.026 0.031 0.009 -0.002 -0.010 C37' 0.065 0.018 0.069 0.015 0.013 0.009 C38 0.048 0.034 0.020 0.005 -0.005 -0.017 C38' 0.029 0.062 0.020 0.020 0.001 -0.019 C39 0.028 0.036 0.036 0.010 -0.003 -0.013 C40 0.025 0.031 0.033 -0.008 0.002 -0.010 C40' 0.031 0.031 0.031 -0.006 -0.001 -0.014 C41 0.022 0.056 0.032 -0.012 0.003 -0.011 C41' 0.040 0.065 0.047 -0.019 0.017 -0.011 C42 0.045 0.081 0.032 -0.016 0.000 -0.024 C42' 0.054 0.049 0.035 -0.024 -0.003 -0.010 C43 0.050 0.040 0.022 0.001 0.000 -0.025 C44 0.049 0.051 0.048 -0.014 0.022 -0.021 C45 0.156 0.082 0.045 -0.001 -0.016 -0.082 C46 0.015 0.017 0.019 -0.002 -0.003 -0.002 C47 0.020 0.022 0.018 -0.002 -0.001 -0.009 C48 0.028 0.030 0.019 -0.002 0.001 -0.014 C49 0.026 0.047 0.030 -0.003 0.006 -0.017 C50 0.043 0.055 0.039 0.007 0.003 -0.034 C51 0.047 0.033 0.040 0.011 -0.005 -0.024 C52 0.030 0.026 0.030 0.004 -0.005 -0.015 C53 0.020 0.030 0.027 -0.006 0.006 -0.005 C54 0.056 0.046 0.055 0.003 -0.027 -0.013 C55 0.070 0.044 0.047 -0.018 -0.006 -0.006 C56 0.034 0.021 0.049 0.002 -0.006 -0.010 C57 0.046 0.027 0.071 -0.007 0.000 -0.015 C58 0.048 0.039 0.065 0.012 -0.023 -0.014 C59 0.022 0.027 0.016 -0.005 0.002 -0.014 C60 0.021 0.032 0.017 -0.005 0.001 -0.012 C61 0.026 0.043 0.022 -0.007 -0.001 -0.018 C62 0.041 0.048 0.027 -0.008 -0.004 -0.031 C63 0.046 0.030 0.031 -0.008 -0.002 -0.019 C64 0.030 0.025 0.025 -0.006 -0.003 -0.014 C65 0.018 0.032 0.027 -0.010 -0.003 -0.006 C66 0.025 0.042 0.050 -0.015 -0.005 -0.004 C67 0.037 0.034 0.042 -0.002 -0.004 -0.011 C68 0.040 0.023 0.051 -0.010 -0.020 -0.006 C69 0.084 0.037 0.091 0.015 -0.045 -0.022 C70 0.028 0.121 0.088 -0.027 -0.013 -0.007 _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 2.373(3) . ? Sm1 N1 2.386(3) . ? Sm1 N3 2.473(3) . ? Sm1 N6 2.480(3) . ? Sm1 N4 2.500(3) . ? Sm1 N5 2.509(3) . ? Sm1 C1 2.799(4) . ? Sm1 C21 2.873(3) . ? Sm1 C46 2.884(3) . ? N1 C1 1.323(5) . ? N1 C2 1.479(5) . ? N2 C1 1.331(5) . ? N2 C8 1.460(4) . ? N3 C21 1.321(4) . ? N3 C22 1.426(4) . ? N4 C21 1.315(4) . ? N4 C34 1.439(4) . ? N5 C46 1.333(4) . ? N5 C47 1.429(4) . ? N6 C46 1.316(4) . ? N6 C59 1.433(4) . ? C1 C14 1.528(5) . ? C2 C3 1.514(5) . ? C2 C7 1.532(5) . ? C3 C4 1.531(6) . ? C4 C5 1.517(6) . ? C5 C6 1.510(6) . ? C6 C7 1.541(6) . ? C8 C13 1.511(5) . ? C8 C9 1.522(5) . ? C9 C10 1.530(5) . ? C10 C11 1.510(6) . ? C11 C12 1.516(5) . ? C12 C13 1.525(5) . ? C14 C15 1.518(6) . ? C15 C20 1.358(6) . ? C15 C16 1.367(6) . ? C16 C17 1.379(7) . ? C17 C18 1.375(8) . ? C18 C19 1.364(8) . ? C19 C20 1.362(7) . ? C22 C27 1.403(5) . ? C22 C31C 1.409(5) . ? C31C C24 1.391(5) . ? C31C C28 1.526(6) . ? C24 C25 1.367(6) . ? C25 C26 1.376(6) . ? C26 C27 1.389(5) . ? C27 C31 1.516(6) . ? C28 C30 1.524(6) . ? C28 C29 1.527(7) . ? C31 C33 1.528(5) . ? C31 C32 1.533(5) . ? C34 C35 1.387(7) . ? C34 C39 1.400(5) . ? C34 C35' 1.569(16) . ? C35 C36 1.385(7) . ? C35 C40 1.519(8) . ? C35' C36' 1.399(18) . ? C35' C40' 1.49(2) . ? C36 C37 1.383(8) . ? C36' C37' 1.37(2) . ? C37 C38 1.355(9) . ? C37' C38' 1.39(2) . ? C38 C39 1.415(6) . ? C38' C39 1.470(16) . ? C39 C43 1.493(6) . ? C40 C42 1.486(8) . ? C40 C41 1.511(8) . ? C40' C42' 1.50(2) . ? C40' C41' 1.51(2) . ? C43 C44 1.521(6) . ? C43 C45 1.529(6) . ? C47 C48 1.405(5) . ? C47 C52 1.405(5) . ? C48 C49 1.395(5) . ? C48 C53 1.520(5) . ? C49 C50 1.370(6) . ? C50 C51 1.358(6) . ? C51 C52 1.399(5) . ? C52 C56 1.504(5) . ? C53 C55 1.515(6) . ? C53 C54 1.520(5) . ? C56 C57 1.537(6) . ? C56 C58 1.541(5) . ? C59 C64 1.404(5) . ? C59 C60 1.414(5) . ? C60 C61 1.393(5) . ? C60 C65 1.520(5) . ? C61 C62 1.371(5) . ? C62 C63 1.369(5) . ? C63 C64 1.388(5) . ? C64 C68 1.515(5) . ? C65 C67 1.526(5) . ? C65 C66 1.526(5) . ? C68 C70 1.506(7) . ? C68 C69 1.523(6) . ? 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 56.34(10) . . ? N2 Sm1 N3 119.28(10) . . ? N1 Sm1 N3 94.62(10) . . ? N2 Sm1 N6 84.27(10) . . ? N1 Sm1 N6 101.55(10) . . ? N3 Sm1 N6 156.31(9) . . ? N2 Sm1 N4 95.98(10) . . ? N1 Sm1 N4 123.92(10) . . ? N3 Sm1 N4 54.52(9) . . ? N6 Sm1 N4 125.16(9) . . ? N2 Sm1 N5 135.81(9) . . ? N1 Sm1 N5 112.15(10) . . ? N3 Sm1 N5 103.30(9) . . ? N6 Sm1 N5 54.53(8) . . ? N4 Sm1 N5 119.47(9) . . ? N2 Sm1 C1 28.32(11) . . ? N1 Sm1 C1 28.16(11) . . ? N3 Sm1 C1 107.05(10) . . ? N6 Sm1 C1 95.16(10) . . ? N4 Sm1 C1 110.40(10) . . ? N5 Sm1 C1 130.07(10) . . ? N2 Sm1 C21 108.95(10) . . ? N1 Sm1 C21 110.59(10) . . ? N3 Sm1 C21 27.32(9) . . ? N6 Sm1 C21 147.43(9) . . ? N4 Sm1 C21 27.22(9) . . ? N5 Sm1 C21 114.53(9) . . ? C1 Sm1 C21 110.58(10) . . ? N2 Sm1 C46 109.71(10) . . ? N1 Sm1 C46 107.64(10) . . ? N3 Sm1 C46 130.59(9) . . ? N6 Sm1 C46 27.08(8) . . ? N4 Sm1 C46 128.23(9) . . ? N5 Sm1 C46 27.51(8) . . ? C1 Sm1 C46 113.27(10) . . ? C21 Sm1 C46 136.14(9) . . ? C1 N1 C2 122.3(3) . . ? C1 N1 Sm1 93.5(2) . . ? C2 N1 Sm1 143.3(2) . . ? C1 N2 C8 124.2(3) . . ? C1 N2 Sm1 93.9(2) . . ? C8 N2 Sm1 141.6(2) . . ? C21 N3 C22 119.6(3) . . ? C21 N3 Sm1 93.4(2) . . ? C22 N3 Sm1 147.0(2) . . ? C21 N4 C34 118.0(3) . . ? C21 N4 Sm1 92.38(19) . . ? C34 N4 Sm1 149.3(2) . . ? C46 N5 C47 116.9(3) . . ? C46 N5 Sm1 92.1(2) . . ? C47 N5 Sm1 150.9(2) . . ? C46 N6 C59 120.1(3) . . ? C46 N6 Sm1 93.8(2) . . ? C59 N6 Sm1 144.7(2) . . ? N1 C1 N2 115.7(3) . . ? N1 C1 C14 121.2(4) . . ? N2 C1 C14 123.2(4) . . ? N1 C1 Sm1 58.31(19) . . ? N2 C1 Sm1 57.74(18) . . ? C14 C1 Sm1 174.1(3) . . ? N1 C2 C3 108.9(3) . . ? N1 C2 C7 112.4(3) . . ? C3 C2 C7 108.4(3) . . ? C2 C3 C4 112.8(3) . . ? C5 C4 C3 111.2(4) . . ? C6 C5 C4 110.6(4) . . ? C5 C6 C7 110.2(4) . . ? C2 C7 C6 111.9(4) . . ? N2 C8 C13 108.2(3) . . ? N2 C8 C9 113.6(3) . . ? C13 C8 C9 108.7(3) . . ? C8 C9 C10 111.8(3) . . ? C11 C10 C9 110.8(3) . . ? C10 C11 C12 111.3(4) . . ? C11 C12 C13 111.1(3) . . ? C8 C13 C12 111.5(3) . . ? C15 C14 C1 115.7(3) . . ? C20 C15 C16 117.2(5) . . ? C20 C15 C14 119.7(4) . . ? C16 C15 C14 122.9(4) . . ? C15 C16 C17 120.4(5) . . ? C18 C17 C16 121.0(5) . . ? C19 C18 C17 118.5(5) . . ? C20 C19 C18 119.3(6) . . ? C15 C20 C19 123.5(5) . . ? N4 C21 N3 119.6(3) . . ? N4 C21 Sm1 60.40(17) . . ? N3 C21 Sm1 59.26(17) . . ? C27 C22 C31C 120.4(3) . . ? C27 C22 N3 118.2(3) . . ? C31C C22 N3 121.3(3) . . ? C24 C31C C22 118.3(4) . . ? C24 C31C C28 119.1(4) . . ? C22 C31C C28 122.7(3) . . ? C25 C24 C31C 121.8(4) . . ? C24 C25 C26 119.5(4) . . ? C25 C26 C27 121.6(4) . . ? C26 C27 C22 118.5(4) . . ? C26 C27 C31 120.2(4) . . ? C22 C27 C31 121.2(3) . . ? C30 C28 C31C 114.7(4) . . ? C30 C28 C29 108.4(4) . . ? C31C C28 C29 109.1(4) . . ? C27 C31 C33 114.7(3) . . ? C27 C31 C32 109.6(3) . . ? C33 C31 C32 109.4(3) . . ? C35 C34 C39 117.2(4) . . ? C35 C34 N4 121.0(4) . . ? C39 C34 N4 121.8(4) . . ? C39 C34 C35' 125.3(6) . . ? N4 C34 C35' 108.4(5) . . ? C36 C35 C34 120.6(5) . . ? C36 C35 C40 119.3(5) . . ? C34 C35 C40 120.0(4) . . ? C36' C35' C40' 118.1(14) . . ? C36' C35' C34 115.7(12) . . ? C40' C35' C34 123.7(10) . . ? C37 C36 C35 121.3(6) . . ? C37' C36' C35' 120.9(15) . . ? C38 C37 C36 119.8(5) . . ? C36' C37' C38' 119.7(14) . . ? C37 C38 C39 119.2(5) . . ? C37' C38' C39 129.0(12) . . ? C34 C39 C38 121.6(4) . . ? C34 C39 C38' 108.3(7) . . ? C34 C39 C43 124.3(3) . . ? C38 C39 C43 113.4(4) . . ? C38' C39 C43 125.5(7) . . ? C42 C40 C41 111.0(5) . . ? C42 C40 C35 109.2(5) . . ? C41 C40 C35 114.7(5) . . ? C35' C40' C42' 115.8(12) . . ? C35' C40' C41' 107.8(12) . . ? C42' C40' C41' 110.1(13) . . ? C39 C43 C44 111.9(3) . . ? C39 C43 C45 111.7(4) . . ? C44 C43 C45 108.5(4) . . ? N6 C46 N5 119.2(3) . . ? N6 C46 Sm1 59.07(17) . . ? N5 C46 Sm1 60.37(18) . . ? C48 C47 C52 118.7(3) . . ? C48 C47 N5 120.8(3) . . ? C52 C47 N5 120.5(3) . . ? C49 C48 C47 120.0(3) . . ? C49 C48 C53 117.0(3) . . ? C47 C48 C53 123.1(3) . . ? C50 C49 C48 120.9(4) . . ? C51 C50 C49 119.4(4) . . ? C50 C51 C52 122.3(4) . . ? C51 C52 C47 118.7(4) . . ? C51 C52 C56 118.0(3) . . ? C47 C52 C56 123.3(3) . . ? C55 C53 C48 111.6(3) . . ? C55 C53 C54 110.0(4) . . ? C48 C53 C54 110.7(3) . . ? C52 C56 C57 110.8(3) . . ? C52 C56 C58 110.5(4) . . ? C57 C56 C58 110.9(3) . . ? C64 C59 C60 119.8(3) . . ? C64 C59 N6 120.2(3) . . ? C60 C59 N6 119.8(3) . . ? C61 C60 C59 118.4(3) . . ? C61 C60 C65 120.1(3) . . ? C59 C60 C65 121.4(3) . . ? C62 C61 C60 121.6(3) . . ? C63 C62 C61 119.6(3) . . ? C62 C63 C64 121.7(4) . . ? C63 C64 C59 118.9(3) . . ? C63 C64 C68 119.5(3) . . ? C59 C64 C68 121.7(3) . . ? C60 C65 C67 110.9(3) . . ? C60 C65 C66 112.9(3) . . ? C67 C65 C66 109.3(3) . . ? C70 C68 C64 110.3(4) . . ? C70 C68 C69 111.1(4) . . ? C64 C68 C69 112.2(4) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.972 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.106 # Attachment '5.PhMe.CIF' data_jun12b _database_code_depnum_ccdc_archive 'CCDC 752060' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C63 H93 N6 Sm, C7 H8' _chemical_formula_sum 'C70 H101 N6 Sm' _chemical_formula_weight 1176.92 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 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 13.1079(3) _cell_length_b 13.5130(3) _cell_length_c 18.4697(4) _cell_angle_alpha 90.134(1) _cell_angle_beta 92.806(1) _cell_angle_gamma 101.948(1) _cell_volume 3196.51(12) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6540 _cell_measurement_theta_min 4.87 _cell_measurement_theta_max 59.75 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1250 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 X8 Apex CCD' _diffrn_measurement_method 'thin slice phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42022 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14643 _reflns_number_gt 13164 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 v2.0' _computing_cell_refinement 'Bruker Apex2 v2.0' _computing_data_reduction 'Bruker Apex2 v2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0084P)^2^+2.1818P] 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 14643 _refine_ls_number_parameters 695 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 0.830400(11) 0.740700(11) 0.740620(7) 0.019 Uani 1 1 d . . . N1 N 0.84502(19) 0.56822(18) 0.74132(13) 0.026 Uani 1 1 d . . . N2 N 0.68144(19) 0.60207(18) 0.73167(13) 0.026 Uani 1 1 d . . . N3 N 0.94437(17) 0.82099(17) 0.64252(11) 0.018 Uani 1 1 d . . . N4 N 0.76725(17) 0.80041(17) 0.62745(12) 0.018 Uani 1 1 d . . . N5 N 0.92849(18) 0.85793(17) 0.83448(12) 0.020 Uani 1 1 d . . . N6 N 0.77071(18) 0.76475(18) 0.86244(12) 0.022 Uani 1 1 d . . . C1 C 0.7412(2) 0.5363(2) 0.73716(15) 0.026 Uani 1 1 d . . . H1 H 0.7113 0.4661 0.7382 0.031 Uiso 1 1 calc R . . C2 C 0.5681(2) 0.5666(2) 0.72781(16) 0.027 Uani 1 1 d . . . H2 H 0.5483 0.5208 0.6846 0.033 Uiso 1 1 calc R . . C3 C 0.5260(2) 0.5093(3) 0.79491(18) 0.037 Uani 1 1 d . . . H3A H 0.5545 0.4472 0.8000 0.044 Uiso 1 1 calc R . . H3B H 0.5488 0.5521 0.8387 0.044 Uiso 1 1 calc R . . C4 C 0.4069(3) 0.4810(3) 0.78874(19) 0.044 Uani 1 1 d . . . H4A H 0.3844 0.4343 0.7469 0.052 Uiso 1 1 calc R . . H4B H 0.3809 0.4453 0.8331 0.052 Uiso 1 1 calc R . . C5 C 0.3601(3) 0.5739(3) 0.7789(2) 0.049 Uani 1 1 d . . . H5A H 0.3778 0.6181 0.8224 0.058 Uiso 1 1 calc R . . H5B H 0.2831 0.5531 0.7733 0.058 Uiso 1 1 calc R . . C6 C 0.4013(3) 0.6319(3) 0.7126(2) 0.055 Uani 1 1 d . . . H6A H 0.3740 0.6949 0.7091 0.066 Uiso 1 1 calc R . . H6B H 0.3763 0.5905 0.6685 0.066 Uiso 1 1 calc R . . C7 C 0.5202(3) 0.6581(3) 0.7168(2) 0.046 Uani 1 1 d . . . H7A H 0.5448 0.6917 0.6714 0.055 Uiso 1 1 calc R . . H7B H 0.5445 0.7066 0.7573 0.055 Uiso 1 1 calc R . . C8 C 0.9045(2) 0.4889(2) 0.75213(15) 0.025 Uani 1 1 d . . . H8 H 0.8629 0.4354 0.7823 0.030 Uiso 1 1 calc R . . C9 C 0.9247(2) 0.4390(2) 0.68154(15) 0.026 Uani 1 1 d . . . H9A H 0.8572 0.4093 0.6559 0.031 Uiso 1 1 calc R . . H9B H 0.9640 0.4909 0.6499 0.031 Uiso 1 1 calc R . . C10 C 0.9865(3) 0.3564(2) 0.69535(18) 0.033 Uani 1 1 d . . . H10A H 0.9434 0.3003 0.7217 0.040 Uiso 1 1 calc R . . H10B H 1.0024 0.3291 0.6483 0.040 Uiso 1 1 calc R . . C11 C 1.0881(3) 0.3956(2) 0.73943(17) 0.033 Uani 1 1 d . . . H11A H 1.1358 0.4443 0.7102 0.039 Uiso 1 1 calc R . . H11B H 1.1223 0.3385 0.7514 0.039 Uiso 1 1 calc R . . C12 C 1.0679(3) 0.4475(2) 0.80943(16) 0.032 Uani 1 1 d . . . H12A H 1.0277 0.3967 0.8414 0.039 Uiso 1 1 calc R . . H12B H 1.1354 0.4770 0.8352 0.039 Uiso 1 1 calc R . . C13 C 1.0077(2) 0.5303(2) 0.79389(16) 0.030 Uani 1 1 d . . . H13A H 1.0504 0.5839 0.7653 0.036 Uiso 1 1 calc R . . H13B H 0.9939 0.5610 0.8402 0.036 Uiso 1 1 calc R . . C14 C 0.8614(2) 0.8306(2) 0.60175(14) 0.018 Uani 1 1 d . . . H14 H 0.8689 0.8586 0.5547 0.021 Uiso 1 1 calc R . . C15 C 1.0449(2) 0.8650(2) 0.61735(13) 0.017 Uani 1 1 d . . . C16 C 1.0807(2) 0.9704(2) 0.61918(14) 0.019 Uani 1 1 d . . . C17 C 1.1789(2) 1.0104(2) 0.59372(15) 0.024 Uani 1 1 d . . . H17 H 1.2034 1.0817 0.5940 0.029 Uiso 1 1 calc R . . C18 C 1.2413(2) 0.9487(2) 0.56815(15) 0.025 Uani 1 1 d . . . H18 H 1.3076 0.9774 0.5504 0.030 Uiso 1 1 calc R . . C19 C 1.2067(2) 0.8451(2) 0.56858(15) 0.025 Uani 1 1 d . . . H19 H 1.2505 0.8028 0.5520 0.030 Uiso 1 1 calc R . . C20 C 1.1088(2) 0.8013(2) 0.59285(14) 0.022 Uani 1 1 d . . . C21 C 1.0168(2) 1.0424(2) 0.64742(14) 0.020 Uani 1 1 d . . . H21 H 0.9550 1.0013 0.6708 0.024 Uiso 1 1 calc R . . C22 C 1.0794(2) 1.1152(2) 0.70454(15) 0.026 Uani 1 1 d . . . H22A H 1.0360 1.1605 0.7218 0.040 Uiso 1 1 calc R . . H22B H 1.1414 1.1552 0.6832 0.040 Uiso 1 1 calc R . . H22C H 1.1009 1.0766 0.7453 0.040 Uiso 1 1 calc R . . C23 C 0.9764(2) 1.1013(2) 0.58565(16) 0.028 Uani 1 1 d . . . H23A H 0.9354 1.1471 0.6053 0.041 Uiso 1 1 calc R . . H23B H 0.9323 1.0538 0.5511 0.041 Uiso 1 1 calc R . . H23C H 1.0357 1.1406 0.5609 0.041 Uiso 1 1 calc R . . C24 C 1.0698(2) 0.6877(2) 0.58967(15) 0.023 Uani 1 1 d . . . H24 H 1.0187 0.6694 0.6284 0.028 Uiso 1 1 calc R . . C25 C 1.1558(3) 0.6280(2) 0.60300(18) 0.034 Uani 1 1 d . . . H25A H 1.1254 0.5554 0.6000 0.052 Uiso 1 1 calc R . . H25B H 1.1894 0.6449 0.6513 0.052 Uiso 1 1 calc R . . H25C H 1.2078 0.6454 0.5663 0.052 Uiso 1 1 calc R . . C26 C 1.0121(3) 0.6559(2) 0.51703(17) 0.036 Uani 1 1 d . . . H26A H 0.9875 0.5823 0.5156 0.054 Uiso 1 1 calc R . . H26B H 1.0595 0.6762 0.4778 0.054 Uiso 1 1 calc R . . H26C H 0.9522 0.6887 0.5110 0.054 Uiso 1 1 calc R . . C27 C 0.6769(2) 0.7941(2) 0.58081(14) 0.021 Uani 1 1 d . . . C28 C 0.6074(2) 0.8589(2) 0.59448(15) 0.024 Uani 1 1 d . . . C29 C 0.5155(2) 0.8483(3) 0.55212(17) 0.035 Uani 1 1 d . . . H29 H 0.4688 0.8917 0.5608 0.042 Uiso 1 1 calc R . . C30 C 0.4906(3) 0.7761(3) 0.49761(18) 0.041 Uani 1 1 d . . . H30 H 0.4274 0.7701 0.4689 0.050 Uiso 1 1 calc R . . C31 C 0.5577(2) 0.7130(3) 0.48506(17) 0.035 Uani 1 1 d . . . H31 H 0.5398 0.6632 0.4476 0.042 Uiso 1 1 calc R . . C32 C 0.6510(2) 0.7199(2) 0.52563(15) 0.025 Uani 1 1 d . . . C33 C 0.6336(2) 0.9374(2) 0.65478(16) 0.029 Uani 1 1 d . . . H33 H 0.6750 0.9097 0.6938 0.035 Uiso 1 1 calc R . . C34 C 0.7020(3) 1.0336(3) 0.62770(18) 0.039 Uani 1 1 d . . . H34A H 0.7186 1.0836 0.6673 0.059 Uiso 1 1 calc R . . H34B H 0.6646 1.0609 0.5878 0.059 Uiso 1 1 calc R . . H34C H 0.7667 1.0184 0.6106 0.059 Uiso 1 1 calc R . . C35 C 0.5375(3) 0.9621(3) 0.68880(19) 0.042 Uani 1 1 d . . . H35A H 0.5599 1.0129 0.7274 0.063 Uiso 1 1 calc R . . H35B H 0.4963 0.9005 0.7091 0.063 Uiso 1 1 calc R . . H35C H 0.4948 0.9887 0.6516 0.063 Uiso 1 1 calc R . . C36 C 0.7190(2) 0.6438(2) 0.51099(16) 0.027 Uani 1 1 d . . . H36 H 0.7833 0.6613 0.5438 0.032 Uiso 1 1 calc R . . C37 C 0.7530(3) 0.6491(3) 0.43304(16) 0.036 Uani 1 1 d . . . H37A H 0.7966 0.5995 0.4256 0.054 Uiso 1 1 calc R . . H37B H 0.7931 0.7172 0.4238 0.054 Uiso 1 1 calc R . . H37C H 0.6912 0.6342 0.3996 0.054 Uiso 1 1 calc R . . C38 C 0.6634(3) 0.5357(3) 0.52790(19) 0.043 Uani 1 1 d . . . H38A H 0.6416 0.5329 0.5780 0.064 Uiso 1 1 calc R . . H38B H 0.7112 0.4896 0.5218 0.064 Uiso 1 1 calc R . . H38C H 0.6019 0.5154 0.4947 0.064 Uiso 1 1 calc R . . C39 C 0.8597(2) 0.8240(2) 0.88382(15) 0.022 Uani 1 1 d . . . H39 H 0.8746 0.8422 0.9335 0.026 Uiso 1 1 calc R . . C40 C 1.0148(2) 0.9362(2) 0.85684(14) 0.022 Uani 1 1 d . . . C41 C 0.9980(2) 1.0297(2) 0.88293(14) 0.023 Uani 1 1 d . . . C42 C 1.0842(2) 1.1039(2) 0.90371(15) 0.028 Uani 1 1 d . . . H42 H 1.0739 1.1669 0.9216 0.033 Uiso 1 1 calc R . . C43 C 1.1848(2) 1.0889(2) 0.89920(16) 0.031 Uani 1 1 d . . . H43 H 1.2427 1.1405 0.9146 0.037 Uiso 1 1 calc R . . C44 C 1.2003(2) 0.9982(2) 0.87212(16) 0.030 Uani 1 1 d . . . H44 H 1.2695 0.9881 0.8686 0.036 Uiso 1 1 calc R . . C45 C 1.1168(2) 0.9216(2) 0.84992(15) 0.025 Uani 1 1 d . . . C46 C 0.8883(2) 1.0503(2) 0.88562(15) 0.026 Uani 1 1 d . . . H46 H 0.8445 0.9897 0.9079 0.031 Uiso 1 1 calc R . . C47 C 0.8397(2) 1.0597(3) 0.80957(16) 0.032 Uani 1 1 d . . . H47A H 0.7691 1.0723 0.8133 0.049 Uiso 1 1 calc R . . H47B H 0.8361 0.9967 0.7822 0.049 Uiso 1 1 calc R . . H47C H 0.8827 1.1160 0.7845 0.049 Uiso 1 1 calc R . . C48 C 0.8813(3) 1.1411(3) 0.93271(18) 0.038 Uani 1 1 d . . . H48A H 0.8088 1.1494 0.9320 0.057 Uiso 1 1 calc R . . H48B H 0.9255 1.2021 0.9138 0.057 Uiso 1 1 calc R . . H48C H 0.9052 1.1302 0.9826 0.057 Uiso 1 1 calc R . . C49 C 1.1382(2) 0.8219(2) 0.82176(16) 0.029 Uani 1 1 d . . . H49 H 1.0733 0.7850 0.7950 0.035 Uiso 1 1 calc R . . C50 C 1.1623(3) 0.7560(3) 0.88424(18) 0.040 Uani 1 1 d . . . H50A H 1.1758 0.6925 0.8650 0.060 Uiso 1 1 calc R . . H50B H 1.1025 0.7413 0.9152 0.060 Uiso 1 1 calc R . . H50C H 1.2240 0.7917 0.9127 0.060 Uiso 1 1 calc R . . C51 C 1.2263(3) 0.8388(3) 0.76886(17) 0.039 Uani 1 1 d . . . H51A H 1.2091 0.8808 0.7288 0.059 Uiso 1 1 calc R . . H51B H 1.2346 0.7734 0.7497 0.059 Uiso 1 1 calc R . . H51C H 1.2916 0.8729 0.7942 0.059 Uiso 1 1 calc R . . C52 C 0.7007(2) 0.7204(2) 0.91690(15) 0.023 Uani 1 1 d . . . C53 C 0.6163(2) 0.7652(2) 0.93217(15) 0.027 Uani 1 1 d . . . C54 C 0.5479(3) 0.7190(3) 0.98372(17) 0.037 Uani 1 1 d . . . H54 H 0.4902 0.7479 0.9947 0.044 Uiso 1 1 calc R . . C55 C 0.5619(3) 0.6336(3) 1.01869(18) 0.042 Uani 1 1 d . . . H55 H 0.5141 0.6037 1.0534 0.050 Uiso 1 1 calc R . . C56 C 0.6455(3) 0.5904(3) 1.00361(17) 0.038 Uani 1 1 d . . . H56 H 0.6553 0.5315 1.0287 0.046 Uiso 1 1 calc R . . C57 C 0.7155(2) 0.6324(2) 0.95203(16) 0.029 Uani 1 1 d . . . C58 C 0.5988(2) 0.8625(2) 0.89850(16) 0.030 Uani 1 1 d . . . H58 H 0.6453 0.8777 0.8569 0.036 Uiso 1 1 calc R . . C59 C 0.6291(3) 0.9506(3) 0.95335(17) 0.036 Uani 1 1 d . . . H59A H 0.6175 1.0131 0.9306 0.054 Uiso 1 1 calc R . . H59B H 0.7029 0.9587 0.9689 0.054 Uiso 1 1 calc R . . H59C H 0.5861 0.9364 0.9955 0.054 Uiso 1 1 calc R . . C60 C 0.4868(3) 0.8578(3) 0.86980(19) 0.042 Uani 1 1 d . . . H60A H 0.4812 0.9229 0.8485 0.063 Uiso 1 1 calc R . . H60B H 0.4396 0.8432 0.9097 0.063 Uiso 1 1 calc R . . H60C H 0.4676 0.8043 0.8327 0.063 Uiso 1 1 calc R . . C61 C 0.8058(3) 0.5827(2) 0.93603(15) 0.029 Uani 1 1 d . . . H61 H 0.8282 0.6042 0.8865 0.035 Uiso 1 1 calc R . . C62 C 0.8999(3) 0.6197(3) 0.98916(17) 0.039 Uani 1 1 d . . . H62A H 0.9176 0.6938 0.9896 0.058 Uiso 1 1 calc R . . H62B H 0.9597 0.5932 0.9739 0.058 Uiso 1 1 calc R . . H62C H 0.8824 0.5957 1.0379 0.058 Uiso 1 1 calc R . . C63 C 0.7767(3) 0.4674(3) 0.9350(2) 0.045 Uani 1 1 d . . . H63A H 0.8381 0.4401 0.9241 0.067 Uiso 1 1 calc R . . H63B H 0.7210 0.4445 0.8977 0.067 Uiso 1 1 calc R . . H63C H 0.7525 0.4435 0.9825 0.067 Uiso 1 1 calc R . . C64 C 0.4712(3) 0.2071(2) 0.76002(18) 0.035 Uani 1 1 d . . . C65 C 0.5502(3) 0.2351(3) 0.71204(19) 0.045 Uani 1 1 d . . . H65 H 0.5324 0.2408 0.6620 0.053 Uiso 1 1 calc R . . C66 C 0.6538(3) 0.2548(2) 0.7357(2) 0.045 Uani 1 1 d . . . H66 H 0.7067 0.2725 0.7018 0.054 Uiso 1 1 calc R . . C67 C 0.6808(3) 0.2491(2) 0.8076(2) 0.042 Uani 1 1 d . . . H67 H 0.7521 0.2639 0.8241 0.051 Uiso 1 1 calc R . . C68 C 0.6039(3) 0.2217(3) 0.8560(2) 0.041 Uani 1 1 d . . . H68 H 0.6222 0.2174 0.9061 0.050 Uiso 1 1 calc R . . C69 C 0.5006(3) 0.2004(3) 0.83230(18) 0.038 Uani 1 1 d . . . H69 H 0.4484 0.1807 0.8664 0.046 Uiso 1 1 calc R . . C70 C 0.3582(3) 0.1832(3) 0.7347(2) 0.060 Uani 1 1 d . . . H70A H 0.3506 0.2087 0.6855 0.090 Uiso 1 1 calc R . . H70B H 0.3179 0.2155 0.7675 0.090 Uiso 1 1 calc R . . H70C H 0.3321 0.1098 0.7346 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.020 0.019 0.017 0.001 0.003 0.003 N1 0.024 0.022 0.030 0.000 0.004 0.004 N2 0.023 0.023 0.031 -0.001 0.007 0.000 N3 0.020 0.017 0.017 0.002 0.004 0.003 N4 0.018 0.020 0.017 0.002 0.001 0.004 N5 0.019 0.021 0.019 0.001 0.003 0.003 N6 0.023 0.025 0.017 0.003 0.004 0.002 C1 0.027 0.026 0.023 0.000 0.004 -0.003 C2 0.024 0.029 0.026 0.000 0.003 -0.001 C3 0.027 0.043 0.036 0.008 0.007 -0.006 C4 0.035 0.049 0.039 0.003 0.008 -0.011 C5 0.023 0.056 0.061 -0.012 0.014 -0.006 C6 0.033 0.054 0.083 0.019 0.010 0.015 C7 0.032 0.041 0.067 0.018 0.016 0.011 C8 0.028 0.021 0.025 0.003 0.005 0.001 C9 0.031 0.023 0.024 0.000 -0.002 0.005 C10 0.039 0.025 0.037 -0.004 -0.004 0.011 C11 0.035 0.025 0.040 0.002 0.000 0.012 C12 0.031 0.037 0.028 0.006 -0.001 0.003 C13 0.034 0.030 0.025 -0.002 0.004 0.006 C14 0.023 0.015 0.016 0.000 0.002 0.004 C15 0.019 0.020 0.013 0.001 0.000 0.004 C16 0.022 0.020 0.014 0.002 -0.001 0.006 C17 0.023 0.024 0.023 0.002 -0.001 0.001 C18 0.017 0.035 0.022 0.000 0.005 0.001 C19 0.025 0.027 0.023 0.002 0.004 0.008 C20 0.024 0.025 0.018 0.002 0.000 0.007 C21 0.022 0.016 0.022 0.001 0.002 0.002 C22 0.032 0.024 0.022 -0.002 0.002 0.003 C23 0.028 0.028 0.027 0.001 0.000 0.008 C24 0.028 0.020 0.024 0.002 0.003 0.011 C25 0.035 0.030 0.043 0.005 0.005 0.015 C26 0.046 0.022 0.039 -0.001 -0.006 0.008 C27 0.020 0.025 0.018 0.005 0.001 0.005 C28 0.025 0.027 0.022 0.004 0.002 0.009 C29 0.027 0.051 0.031 -0.003 0.001 0.017 C30 0.029 0.063 0.034 -0.004 -0.009 0.016 C31 0.030 0.044 0.029 -0.010 -0.006 0.009 C32 0.021 0.032 0.021 0.001 0.002 0.004 C33 0.031 0.033 0.027 0.000 0.002 0.014 C34 0.039 0.041 0.036 -0.008 0.008 0.004 C35 0.046 0.042 0.041 -0.006 0.017 0.009 C36 0.028 0.025 0.026 -0.005 0.000 0.005 C37 0.041 0.038 0.031 0.001 0.010 0.010 C38 0.055 0.036 0.040 0.005 0.014 0.011 C39 0.024 0.023 0.018 0.000 0.000 0.007 C40 0.023 0.028 0.014 0.001 0.001 0.005 C41 0.023 0.028 0.017 -0.001 0.003 0.002 C42 0.031 0.031 0.020 -0.004 -0.002 0.004 C43 0.027 0.033 0.028 -0.004 -0.002 -0.005 C44 0.019 0.041 0.027 -0.003 -0.001 0.003 C45 0.025 0.031 0.019 -0.001 0.002 0.006 C46 0.029 0.027 0.024 -0.002 0.003 0.007 C47 0.032 0.038 0.029 -0.002 -0.001 0.013 C48 0.037 0.038 0.039 -0.009 0.004 0.011 C49 0.020 0.037 0.031 -0.011 -0.006 0.009 C50 0.046 0.031 0.045 -0.002 0.006 0.010 C51 0.035 0.061 0.028 -0.009 0.000 0.021 C52 0.024 0.026 0.018 0.000 0.002 0.001 C53 0.028 0.033 0.021 0.000 0.006 0.004 C54 0.031 0.048 0.033 0.004 0.014 0.006 C55 0.040 0.047 0.037 0.009 0.021 0.003 C56 0.049 0.036 0.027 0.008 0.011 0.000 C57 0.035 0.029 0.021 -0.002 0.007 0.000 C58 0.028 0.040 0.023 0.003 0.007 0.009 C59 0.031 0.042 0.036 -0.001 0.002 0.008 C60 0.033 0.050 0.044 -0.002 -0.005 0.012 C61 0.042 0.026 0.017 0.002 0.004 0.004 C62 0.045 0.043 0.029 0.004 -0.002 0.012 C63 0.059 0.031 0.045 0.001 0.008 0.011 C64 0.038 0.027 0.038 0.000 -0.002 0.002 C65 0.064 0.034 0.032 0.002 0.011 0.000 C66 0.046 0.022 0.066 -0.005 0.026 -0.001 C67 0.035 0.025 0.067 -0.005 0.001 0.006 C68 0.043 0.042 0.039 0.000 -0.005 0.010 C69 0.037 0.044 0.034 0.002 0.006 0.008 C70 0.046 0.062 0.063 0.005 -0.012 -0.008 _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(2) . ? Sm1 N2 2.409(2) . ? Sm1 N4 2.413(2) . ? Sm1 N6 2.461(2) . ? Sm1 N5 2.468(2) . ? Sm1 N3 2.509(2) . ? Sm1 C1 2.766(3) . ? Sm1 C39 2.849(3) . ? Sm1 C14 2.851(3) . ? N1 C1 1.338(4) . ? N1 C8 1.459(4) . ? N2 C1 1.302(4) . ? N2 C2 1.461(4) . ? N3 C14 1.321(3) . ? N3 C15 1.429(3) . ? N4 C14 1.328(3) . ? N4 C27 1.418(3) . ? N5 C39 1.328(3) . ? N5 C40 1.423(4) . ? N6 C39 1.313(4) . ? N6 C52 1.442(3) . ? C2 C7 1.508(4) . ? C2 C3 1.528(4) . ? C3 C4 1.527(4) . ? C4 C5 1.515(5) . ? C5 C6 1.516(5) . ? C6 C7 1.524(5) . ? C8 C13 1.523(4) . ? C8 C9 1.526(4) . ? C9 C10 1.524(4) . ? C10 C11 1.522(4) . ? C11 C12 1.530(4) . ? C12 C13 1.518(4) . ? C15 C16 1.404(4) . ? C15 C20 1.408(4) . ? C16 C17 1.394(4) . ? C16 C21 1.517(4) . ? C17 C18 1.380(4) . ? C18 C19 1.380(4) . ? C19 C20 1.393(4) . ? C20 C24 1.514(4) . ? C21 C22 1.526(4) . ? C21 C23 1.527(4) . ? C24 C26 1.523(4) . ? C24 C25 1.528(4) . ? C27 C32 1.407(4) . ? C27 C28 1.417(4) . ? C28 C29 1.385(4) . ? C28 C33 1.513(4) . ? C29 C30 1.379(4) . ? C30 C31 1.373(4) . ? C31 C32 1.389(4) . ? C32 C36 1.526(4) . ? C33 C34 1.519(4) . ? C33 C35 1.531(4) . ? C36 C37 1.526(4) . ? C36 C38 1.532(4) . ? C40 C45 1.403(4) . ? C40 C41 1.415(4) . ? C41 C42 1.384(4) . ? C41 C46 1.523(4) . ? C42 C43 1.381(4) . ? C43 C44 1.380(4) . ? C44 C45 1.387(4) . ? C45 C49 1.527(4) . ? C46 C48 1.523(4) . ? C46 C47 1.530(4) . ? C49 C50 1.520(5) . ? C49 C51 1.531(4) . ? C52 C57 1.401(4) . ? C52 C53 1.405(4) . ? C53 C54 1.398(4) . ? C53 C58 1.511(4) . ? C54 C55 1.365(5) . ? C55 C56 1.383(5) . ? C56 C57 1.394(4) . ? C57 C61 1.518(4) . ? C58 C60 1.525(4) . ? C58 C59 1.537(4) . ? C61 C63 1.525(4) . ? C61 C62 1.535(4) . ? C64 C69 1.380(5) . ? C64 C65 1.389(5) . ? C64 C70 1.500(5) . ? C65 C66 1.378(5) . ? C66 C67 1.364(5) . ? C67 C68 1.374(5) . ? C68 C69 1.374(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sm1 N2 56.94(8) . . ? N1 Sm1 N4 115.71(8) . . ? N2 Sm1 N4 87.63(8) . . ? N1 Sm1 N6 102.61(8) . . ? N2 Sm1 N6 84.25(8) . . ? N4 Sm1 N6 127.31(8) . . ? N1 Sm1 N5 119.31(8) . . ? N2 Sm1 N5 138.33(8) . . ? N4 Sm1 N5 121.90(8) . . ? N6 Sm1 N5 54.88(7) . . ? N1 Sm1 N3 105.38(7) . . ? N2 Sm1 N3 128.97(8) . . ? N4 Sm1 N3 55.25(7) . . ? N6 Sm1 N3 144.98(8) . . ? N5 Sm1 N3 92.69(7) . . ? N1 Sm1 C1 28.90(8) . . ? N2 Sm1 C1 28.06(8) . . ? N4 Sm1 C1 103.35(8) . . ? N6 Sm1 C1 92.99(8) . . ? N5 Sm1 C1 134.14(8) . . ? N3 Sm1 C1 121.44(7) . . ? N1 Sm1 C39 110.61(8) . . ? N2 Sm1 C39 110.69(8) . . ? N4 Sm1 C39 132.72(8) . . ? N6 Sm1 C39 27.41(7) . . ? N5 Sm1 C39 27.76(7) . . ? N3 Sm1 C39 120.17(8) . . ? C1 Sm1 C39 112.88(8) . . ? N1 Sm1 C14 112.81(8) . . ? N2 Sm1 C14 109.10(8) . . ? N4 Sm1 C14 27.64(7) . . ? N6 Sm1 C14 143.94(8) . . ? N5 Sm1 C14 109.29(8) . . ? N3 Sm1 C14 27.61(7) . . ? C1 Sm1 C14 114.73(8) . . ? C39 Sm1 C14 132.20(8) . . ? C1 N1 C8 115.2(3) . . ? C1 N1 Sm1 91.89(19) . . ? C8 N1 Sm1 152.16(19) . . ? C1 N2 C2 119.3(3) . . ? C1 N2 Sm1 91.43(18) . . ? C2 N2 Sm1 149.1(2) . . ? C14 N3 C15 117.9(2) . . ? C14 N3 Sm1 90.77(16) . . ? C15 N3 Sm1 150.81(18) . . ? C14 N4 C27 120.0(2) . . ? C14 N4 Sm1 94.90(17) . . ? C27 N4 Sm1 143.25(17) . . ? C39 N5 C40 117.0(2) . . ? C39 N5 Sm1 92.27(17) . . ? C40 N5 Sm1 150.76(16) . . ? C39 N6 C52 118.3(2) . . ? C39 N6 Sm1 92.99(16) . . ? C52 N6 Sm1 144.66(18) . . ? N2 C1 N1 119.7(3) . . ? N2 C1 Sm1 60.50(16) . . ? N1 C1 Sm1 59.21(16) . . ? N2 C2 C7 107.3(3) . . ? N2 C2 C3 113.8(3) . . ? C7 C2 C3 110.2(3) . . ? C4 C3 C2 110.5(3) . . ? C5 C4 C3 111.2(3) . . ? C4 C5 C6 110.6(3) . . ? C5 C6 C7 110.9(3) . . ? C2 C7 C6 112.8(3) . . ? N1 C8 C13 110.5(2) . . ? N1 C8 C9 113.3(2) . . ? C13 C8 C9 109.8(2) . . ? C10 C9 C8 111.6(2) . . ? C11 C10 C9 111.9(3) . . ? C10 C11 C12 110.9(3) . . ? C13 C12 C11 111.3(3) . . ? C12 C13 C8 111.2(3) . . ? N3 C14 N4 119.1(2) . . ? N3 C14 Sm1 61.62(14) . . ? N4 C14 Sm1 57.46(14) . . ? C16 C15 C20 120.4(2) . . ? C16 C15 N3 120.3(2) . . ? C20 C15 N3 119.2(2) . . ? C17 C16 C15 118.6(2) . . ? C17 C16 C21 118.6(3) . . ? C15 C16 C21 122.7(2) . . ? C18 C17 C16 121.3(3) . . ? C19 C18 C17 119.6(3) . . ? C18 C19 C20 121.3(3) . . ? C19 C20 C15 118.7(3) . . ? C19 C20 C24 120.7(2) . . ? C15 C20 C24 120.5(2) . . ? C16 C21 C22 111.4(2) . . ? C16 C21 C23 111.1(2) . . ? C22 C21 C23 110.3(2) . . ? C20 C24 C26 110.3(2) . . ? C20 C24 C25 113.7(3) . . ? C26 C24 C25 109.6(2) . . ? C32 C27 C28 119.8(3) . . ? C32 C27 N4 121.3(2) . . ? C28 C27 N4 118.7(2) . . ? C29 C28 C27 118.8(3) . . ? C29 C28 C33 121.0(3) . . ? C27 C28 C33 120.1(3) . . ? C30 C29 C28 121.3(3) . . ? C31 C30 C29 119.6(3) . . ? C30 C31 C32 121.8(3) . . ? C31 C32 C27 118.6(3) . . ? C31 C32 C36 118.8(3) . . ? C27 C32 C36 122.5(3) . . ? C28 C33 C34 110.3(2) . . ? C28 C33 C35 113.6(3) . . ? C34 C33 C35 109.9(3) . . ? C37 C36 C32 111.7(3) . . ? C37 C36 C38 110.0(2) . . ? C32 C36 C38 111.6(3) . . ? N6 C39 N5 118.6(2) . . ? N6 C39 Sm1 59.59(14) . . ? N5 C39 Sm1 59.97(14) . . ? C45 C40 C41 120.1(3) . . ? C45 C40 N5 119.5(2) . . ? C41 C40 N5 120.3(2) . . ? C42 C41 C40 118.3(3) . . ? C42 C41 C46 120.5(3) . . ? C40 C41 C46 121.2(3) . . ? C43 C42 C41 121.9(3) . . ? C44 C43 C42 119.3(3) . . ? C43 C44 C45 121.2(3) . . ? C44 C45 C40 119.1(3) . . ? C44 C45 C49 119.1(3) . . ? C40 C45 C49 121.7(3) . . ? C41 C46 C48 114.1(3) . . ? C41 C46 C47 111.7(2) . . ? C48 C46 C47 110.6(3) . . ? C50 C49 C45 110.8(2) . . ? C50 C49 C51 110.6(3) . . ? C45 C49 C51 112.0(3) . . ? C57 C52 C53 121.1(3) . . ? C57 C52 N6 119.9(3) . . ? C53 C52 N6 119.0(3) . . ? C54 C53 C52 117.8(3) . . ? C54 C53 C58 118.6(3) . . ? C52 C53 C58 123.5(3) . . ? C55 C54 C53 121.7(3) . . ? C54 C55 C56 120.1(3) . . ? C55 C56 C57 120.7(3) . . ? C56 C57 C52 118.6(3) . . ? C56 C57 C61 119.5(3) . . ? C52 C57 C61 121.8(3) . . ? C53 C58 C60 113.9(3) . . ? C53 C58 C59 110.6(3) . . ? C60 C58 C59 108.5(3) . . ? C57 C61 C63 113.5(3) . . ? C57 C61 C62 111.3(2) . . ? C63 C61 C62 110.2(3) . . ? C69 C64 C65 117.4(3) . . ? C69 C64 C70 120.8(3) . . ? C65 C64 C70 121.8(3) . . ? C66 C65 C64 121.3(3) . . ? C67 C66 C65 120.2(3) . . ? C66 C67 C68 119.5(4) . . ? C67 C68 C69 120.3(3) . . ? C68 C69 C64 121.3(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.404 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.091 # Attachment '7.PhMe.CIF' data_jun4b_0m _database_code_depnum_ccdc_archive 'CCDC 752061' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C71 H97 N6 Sm, C7 H8' _chemical_formula_sum 'C78 H105 N6 Sm' _chemical_formula_weight 1277.03 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' O O 0.0106 0.0060 '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 16.7889(6) _cell_length_b 17.8233(7) _cell_length_c 25.0661(11) _cell_angle_alpha 90.00 _cell_angle_beta 109.1180(10) _cell_angle_gamma 90.00 _cell_volume 7086.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5141 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 29.99 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2708 _exptl_absorpt_coefficient_mu 0.874 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 X8 Apex CCD' _diffrn_measurement_method 'thin slice phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57931 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16264 _reflns_number_gt 13374 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 v2.0' _computing_cell_refinement 'Bruker Apex2 v2.0' _computing_data_reduction 'Bruker Apex2 v2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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^)+(0.0151P)^2^+4.8918P] 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 16264 _refine_ls_number_parameters 767 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 0.263607(9) 0.616488(8) 0.227193(6) 0.01632(4) Uani 1 1 d . . . N1 N 0.12710(15) 0.60201(13) 0.24254(10) 0.0222(5) Uani 1 1 d . . . N2 N 0.13194(15) 0.63162(13) 0.15463(10) 0.0227(6) Uani 1 1 d . . . N3 N 0.35024(15) 0.52627(12) 0.19057(10) 0.0187(5) Uani 1 1 d . . . N4 N 0.29528(15) 0.49020(12) 0.25854(10) 0.0187(5) Uani 1 1 d . . . N5 N 0.27569(15) 0.73526(13) 0.27876(10) 0.0215(5) Uani 1 1 d . . . N6 N 0.38555(14) 0.70135(13) 0.24973(10) 0.0190(5) Uani 1 1 d . . . C1 C 0.08620(17) 0.61794(16) 0.18895(13) 0.0208(6) Uani 1 1 d . . . C2 C 0.08817(19) 0.65792(17) 0.09714(12) 0.0238(7) Uani 1 1 d . . . H2 H 0.0399 0.6898 0.0985 0.029 Uiso 1 1 calc R . . C3 C 0.0519(2) 0.59497(17) 0.05467(13) 0.0270(7) Uani 1 1 d . . . H3A H 0.0981 0.5613 0.0532 0.032 Uiso 1 1 calc R . . H3B H 0.0116 0.5650 0.0672 0.032 Uiso 1 1 calc R . . C4 C 0.0070(2) 0.62625(19) -0.00417(14) 0.0337(8) Uani 1 1 d . . . H4A H -0.0444 0.6532 -0.0038 0.040 Uiso 1 1 calc R . . H4B H -0.0109 0.5840 -0.0311 0.040 Uiso 1 1 calc R . . C5 C 0.0621(2) 0.67961(19) -0.02464(14) 0.0349(8) Uani 1 1 d . . . H5A H 0.1078 0.6508 -0.0320 0.042 Uiso 1 1 calc R . . H5B H 0.0276 0.7032 -0.0605 0.042 Uiso 1 1 calc R . . C6 C 0.1005(2) 0.74064(18) 0.01888(14) 0.0327(8) Uani 1 1 d . . . H6A H 0.1407 0.7707 0.0063 0.039 Uiso 1 1 calc R . . H6B H 0.0553 0.7746 0.0216 0.039 Uiso 1 1 calc R . . C7 C 0.14624(19) 0.70722(17) 0.07688(13) 0.0265(7) Uani 1 1 d . . . H7A H 0.1947 0.6771 0.0749 0.032 Uiso 1 1 calc R . . H7B H 0.1683 0.7483 0.1043 0.032 Uiso 1 1 calc R . . C8 C 0.07824(19) 0.59265(16) 0.28111(13) 0.0234(7) Uani 1 1 d . . . H8 H 0.0243 0.5666 0.2600 0.028 Uiso 1 1 calc R . . C9 C 0.0561(2) 0.66823(17) 0.30169(15) 0.0322(8) Uani 1 1 d . . . H9A H 0.1086 0.6957 0.3217 0.039 Uiso 1 1 calc R . . H9B H 0.0234 0.6987 0.2688 0.039 Uiso 1 1 calc R . . C10 C 0.0046(2) 0.65760(19) 0.34126(15) 0.0378(9) Uani 1 1 d . . . H10A H -0.0058 0.7072 0.3555 0.045 Uiso 1 1 calc R . . H10B H -0.0507 0.6354 0.3199 0.045 Uiso 1 1 calc R . . C11 C 0.0488(2) 0.6072(2) 0.39108(15) 0.0375(8) Uani 1 1 d . . . H11A H 0.0111 0.5979 0.4136 0.045 Uiso 1 1 calc R . . H11B H 0.1003 0.6324 0.4157 0.045 Uiso 1 1 calc R . . C12 C 0.0726(2) 0.53262(19) 0.37038(15) 0.0394(9) Uani 1 1 d . . . H12A H 0.0206 0.5047 0.3499 0.047 Uiso 1 1 calc R . . H12B H 0.1052 0.5021 0.4033 0.047 Uiso 1 1 calc R . . C13 C 0.1250(2) 0.54429(19) 0.33133(14) 0.0327(8) Uani 1 1 d . . . H13A H 0.1791 0.5686 0.3526 0.039 Uiso 1 1 calc R . . H13B H 0.1379 0.4950 0.3179 0.039 Uiso 1 1 calc R . . C14 C -0.00557(19) 0.62111(17) 0.16710(13) 0.0248(7) Uani 1 1 d . . . C15 C -0.08057(19) 0.62308(16) 0.14939(13) 0.0243(7) Uani 1 1 d . . . C16 C -0.17050(18) 0.62855(15) 0.12619(13) 0.0220(6) Uani 1 1 d . . . C17 C -0.2216(2) 0.61489(19) 0.15891(15) 0.0345(8) Uani 1 1 d . . . H17 H -0.1971 0.6001 0.1972 0.041 Uiso 1 1 calc R . . C18 C -0.3080(2) 0.6227(2) 0.13583(18) 0.0415(9) Uani 1 1 d . . . H18 H -0.3426 0.6138 0.1585 0.050 Uiso 1 1 calc R . . C19 C -0.3440(2) 0.6431(2) 0.08060(17) 0.0414(9) Uani 1 1 d . . . H19 H -0.4035 0.6479 0.0649 0.050 Uiso 1 1 calc R . . C20 C -0.2940(2) 0.6565(2) 0.04782(16) 0.0411(9) Uani 1 1 d . . . H20 H -0.3191 0.6710 0.0095 0.049 Uiso 1 1 calc R . . C21 C -0.2075(2) 0.64909(17) 0.07017(13) 0.0281(7) Uani 1 1 d . . . H21 H -0.1733 0.6581 0.0472 0.034 Uiso 1 1 calc R . . C22 C 0.33562(17) 0.47335(15) 0.22293(12) 0.0191(6) Uani 1 1 d . . . H22 H 0.3540 0.4234 0.2206 0.023 Uiso 1 1 calc R . . C23 C 0.40233(18) 0.50771(15) 0.15749(12) 0.0191(6) Uani 1 1 d . . . C24 C 0.49026(19) 0.49960(15) 0.18309(13) 0.0210(6) Uani 1 1 d . . . C25 C 0.5387(2) 0.48168(16) 0.14909(14) 0.0261(7) Uani 1 1 d . . . H25 H 0.5976 0.4740 0.1661 0.031 Uiso 1 1 calc R . . C26 C 0.5027(2) 0.47484(17) 0.09112(14) 0.0296(7) Uani 1 1 d . . . H26 H 0.5371 0.4637 0.0686 0.036 Uiso 1 1 calc R . . C27 C 0.4172(2) 0.48428(16) 0.06611(14) 0.0275(7) Uani 1 1 d . . . H27 H 0.3928 0.4798 0.0263 0.033 Uiso 1 1 calc R . . C28 C 0.36583(19) 0.50040(15) 0.09858(12) 0.0206(6) Uani 1 1 d . . . C29 C 0.53179(19) 0.50954(16) 0.24633(13) 0.0235(7) Uani 1 1 d . . . H29 H 0.4932 0.5404 0.2605 0.028 Uiso 1 1 calc R . . C30 C 0.6164(2) 0.55126(18) 0.26093(14) 0.0317(8) Uani 1 1 d . . . H30A H 0.6079 0.5995 0.2411 0.048 Uiso 1 1 calc R . . H30B H 0.6565 0.5209 0.2492 0.048 Uiso 1 1 calc R . . H30C H 0.6388 0.5599 0.3018 0.048 Uiso 1 1 calc R . . C31 C 0.5463(2) 0.43447(18) 0.27808(14) 0.0339(8) Uani 1 1 d . . . H31A H 0.5728 0.4436 0.3186 0.051 Uiso 1 1 calc R . . H31B H 0.5834 0.4028 0.2645 0.051 Uiso 1 1 calc R . . H31C H 0.4922 0.4091 0.2714 0.051 Uiso 1 1 calc R . . C32 C 0.2712(2) 0.50574(17) 0.07136(13) 0.0268(7) Uani 1 1 d . . . H32 H 0.2502 0.5433 0.0933 0.032 Uiso 1 1 calc R . . C33 C 0.2426(2) 0.53154(19) 0.00982(14) 0.0381(9) Uani 1 1 d . . . H33A H 0.2683 0.5802 0.0072 0.057 Uiso 1 1 calc R . . H33B H 0.1810 0.5364 -0.0041 0.057 Uiso 1 1 calc R . . H33C H 0.2601 0.4946 -0.0131 0.057 Uiso 1 1 calc R . . C34 C 0.2309(2) 0.43015(18) 0.07617(14) 0.0316(8) Uani 1 1 d . . . H34A H 0.1695 0.4339 0.0588 0.047 Uiso 1 1 calc R . . H34B H 0.2447 0.4166 0.1161 0.047 Uiso 1 1 calc R . . H34C H 0.2525 0.3915 0.0567 0.047 Uiso 1 1 calc R . . C35 C 0.27230(19) 0.43111(15) 0.28921(13) 0.0202(6) Uani 1 1 d . . . C36 C 0.3208(2) 0.42071(16) 0.34624(13) 0.0261(7) Uani 1 1 d . . . C37 C 0.2958(2) 0.36558(17) 0.37711(15) 0.0353(8) Uani 1 1 d . . . H37 H 0.3279 0.3576 0.4156 0.042 Uiso 1 1 calc R . . C38 C 0.2249(2) 0.32268(18) 0.35219(16) 0.0386(9) Uani 1 1 d . . . H38 H 0.2080 0.2860 0.3738 0.046 Uiso 1 1 calc R . . C39 C 0.1788(2) 0.33282(17) 0.29628(15) 0.0318(8) Uani 1 1 d . . . H39 H 0.1306 0.3024 0.2795 0.038 Uiso 1 1 calc R . . C40 C 0.20120(18) 0.38678(16) 0.26362(13) 0.0226(6) Uani 1 1 d . . . C41 C 0.3976(2) 0.46962(18) 0.37467(14) 0.0333(8) Uani 1 1 d . . . H41 H 0.4207 0.4861 0.3445 0.040 Uiso 1 1 calc R . . C42 C 0.3716(3) 0.5397(2) 0.3985(2) 0.0657(14) Uani 1 1 d . . . H42A H 0.3264 0.5650 0.3689 0.099 Uiso 1 1 calc R . . H42B H 0.4201 0.5734 0.4125 0.099 Uiso 1 1 calc R . . H42C H 0.3513 0.5261 0.4297 0.099 Uiso 1 1 calc R . . C43 C 0.4684(3) 0.4295(2) 0.41928(18) 0.0586(12) Uani 1 1 d . . . H43A H 0.5153 0.4643 0.4353 0.088 Uiso 1 1 calc R . . H43B H 0.4877 0.3869 0.4021 0.088 Uiso 1 1 calc R . . H43C H 0.4478 0.4113 0.4493 0.088 Uiso 1 1 calc R . . C44 C 0.14864(18) 0.39465(16) 0.20192(13) 0.0255(7) Uani 1 1 d . . . H44 H 0.1707 0.4385 0.1861 0.031 Uiso 1 1 calc R . . C45 C 0.0551(2) 0.40900(19) 0.19315(16) 0.0388(9) Uani 1 1 d . . . H45A H 0.0242 0.4139 0.1527 0.058 Uiso 1 1 calc R . . H45B H 0.0493 0.4554 0.2126 0.058 Uiso 1 1 calc R . . H45C H 0.0321 0.3669 0.2086 0.058 Uiso 1 1 calc R . . C46 C 0.1574(2) 0.32476(17) 0.16893(14) 0.0317(8) Uani 1 1 d . . . H46A H 0.1232 0.3308 0.1291 0.048 Uiso 1 1 calc R . . H46B H 0.1379 0.2807 0.1845 0.048 Uiso 1 1 calc R . . H46C H 0.2166 0.3180 0.1720 0.048 Uiso 1 1 calc R . . C47 C 0.34887(18) 0.75155(15) 0.27285(12) 0.0192(6) Uani 1 1 d . . . H47 H 0.3749 0.7987 0.2850 0.023 Uiso 1 1 calc R . . C48 C 0.23729(19) 0.79267(16) 0.30255(14) 0.0244(7) Uani 1 1 d . . . C49 C 0.2596(2) 0.79955(18) 0.36121(15) 0.0316(8) Uani 1 1 d . . . C50 C 0.2228(2) 0.8577(2) 0.38241(17) 0.0443(10) Uani 1 1 d . . . H50 H 0.2375 0.8633 0.4222 0.053 Uiso 1 1 calc R . . C51 C 0.1660(2) 0.9069(2) 0.34791(18) 0.0485(11) Uani 1 1 d . . . H51 H 0.1429 0.9465 0.3635 0.058 Uiso 1 1 calc R . . C52 C 0.1433(2) 0.89794(19) 0.29042(17) 0.0399(9) Uani 1 1 d . . . H52 H 0.1035 0.9315 0.2665 0.048 Uiso 1 1 calc R . . C53 C 0.1770(2) 0.84070(17) 0.26625(15) 0.0285(7) Uani 1 1 d . . . C54 C 0.3232(2) 0.74886(19) 0.40192(14) 0.0333(8) Uani 1 1 d . . . H54 H 0.3402 0.7095 0.3793 0.040 Uiso 1 1 calc R . . C55 C 0.4026(2) 0.7927(2) 0.43511(15) 0.0414(9) Uani 1 1 d . . . H55A H 0.4430 0.7586 0.4609 0.062 Uiso 1 1 calc R . . H55B H 0.3873 0.8326 0.4569 0.062 Uiso 1 1 calc R . . H55C H 0.4280 0.8149 0.4088 0.062 Uiso 1 1 calc R . . C56 C 0.2866(3) 0.7090(2) 0.44285(16) 0.0479(10) Uani 1 1 d . . . H56A H 0.3296 0.6764 0.4680 0.072 Uiso 1 1 calc R . . H56B H 0.2378 0.6788 0.4214 0.072 Uiso 1 1 calc R . . H56C H 0.2688 0.7465 0.4653 0.072 Uiso 1 1 calc R . . C57 C 0.1491(2) 0.83362(17) 0.20276(15) 0.0312(8) Uani 1 1 d . . . H57 H 0.1742 0.7864 0.1936 0.037 Uiso 1 1 calc R . . C58 C 0.1817(2) 0.8988(2) 0.17616(17) 0.0470(10) Uani 1 1 d . . . H58A H 0.1632 0.8924 0.1351 0.070 Uiso 1 1 calc R . . H58B H 0.2434 0.8999 0.1910 0.070 Uiso 1 1 calc R . . H58C H 0.1594 0.9461 0.1853 0.070 Uiso 1 1 calc R . . C59 C 0.0533(2) 0.82742(19) 0.17653(16) 0.0408(9) Uani 1 1 d . . . H59A H 0.0382 0.8222 0.1355 0.061 Uiso 1 1 calc R . . H59B H 0.0269 0.8727 0.1853 0.061 Uiso 1 1 calc R . . H59C H 0.0335 0.7834 0.1920 0.061 Uiso 1 1 calc R . . C60 C 0.46659(18) 0.71918(15) 0.24580(12) 0.0192(6) Uani 1 1 d . . . C61 C 0.53679(18) 0.72962(15) 0.29470(13) 0.0221(6) Uani 1 1 d . . . C62 C 0.61370(19) 0.74776(17) 0.28787(14) 0.0278(7) Uani 1 1 d . . . H62 H 0.6618 0.7549 0.3204 0.033 Uiso 1 1 calc R . . C63 C 0.6220(2) 0.75555(17) 0.23529(14) 0.0278(7) Uani 1 1 d . . . H63 H 0.6748 0.7690 0.2318 0.033 Uiso 1 1 calc R . . C64 C 0.55294(19) 0.74366(16) 0.18754(14) 0.0244(7) Uani 1 1 d . . . H64 H 0.5591 0.7481 0.1513 0.029 Uiso 1 1 calc R . . C65 C 0.47450(18) 0.72524(15) 0.19165(13) 0.0201(6) Uani 1 1 d . . . C66 C 0.5332(2) 0.71906(17) 0.35402(13) 0.0275(7) Uani 1 1 d . . . H66 H 0.4734 0.7264 0.3523 0.033 Uiso 1 1 calc R . . C67 C 0.5869(2) 0.7758(2) 0.39576(15) 0.0475(10) Uani 1 1 d . . . H67A H 0.5818 0.7670 0.4331 0.071 Uiso 1 1 calc R . . H67B H 0.5676 0.8266 0.3831 0.071 Uiso 1 1 calc R . . H67C H 0.6460 0.7702 0.3980 0.071 Uiso 1 1 calc R . . C68 C 0.5595(3) 0.6398(2) 0.37587(17) 0.0620(13) Uani 1 1 d . . . H68A H 0.5561 0.6346 0.4140 0.093 Uiso 1 1 calc R . . H68B H 0.6176 0.6306 0.3769 0.093 Uiso 1 1 calc R . . H68C H 0.5218 0.6033 0.3507 0.093 Uiso 1 1 calc R . . C69 C 0.39908(19) 0.71587(16) 0.13853(12) 0.0224(7) Uani 1 1 d . . . H69 H 0.3606 0.6782 0.1469 0.027 Uiso 1 1 calc R . . C70 C 0.3504(2) 0.78989(17) 0.12327(14) 0.0293(7) Uani 1 1 d . . . H70A H 0.3015 0.7829 0.0892 0.044 Uiso 1 1 calc R . . H70B H 0.3873 0.8286 0.1164 0.044 Uiso 1 1 calc R . . H70C H 0.3312 0.8055 0.1545 0.044 Uiso 1 1 calc R . . C71 C 0.4215(2) 0.68716(18) 0.08812(14) 0.0308(8) Uani 1 1 d . . . H71A H 0.3700 0.6821 0.0555 0.046 Uiso 1 1 calc R . . H71B H 0.4492 0.6382 0.0972 0.046 Uiso 1 1 calc R . . H71C H 0.4598 0.7227 0.0791 0.046 Uiso 1 1 calc R . . C72 C 0.2205(3) 0.4537(2) 0.54074(18) 0.0482(10) Uani 1 1 d . . . C73 C 0.2107(3) 0.4047(3) 0.49804(19) 0.0675(14) Uani 1 1 d . . . H73 H 0.2241 0.4201 0.4657 0.081 Uiso 1 1 calc R . . C74 C 0.1823(4) 0.3340(3) 0.5003(2) 0.106(2) Uani 1 1 d . . . H74 H 0.1737 0.3016 0.4688 0.128 Uiso 1 1 calc R . . C75 C 0.1659(3) 0.3086(3) 0.5464(3) 0.0822(17) Uani 1 1 d . . . H75 H 0.1481 0.2583 0.5481 0.099 Uiso 1 1 calc R . . C76 C 0.1751(3) 0.3563(3) 0.5905(2) 0.0597(12) Uani 1 1 d . . . H76 H 0.1630 0.3397 0.6230 0.072 Uiso 1 1 calc R . . C77 C 0.2022(3) 0.4288(2) 0.58774(18) 0.0567(12) Uani 1 1 d . . . H77 H 0.2083 0.4621 0.6184 0.068 Uiso 1 1 calc R . . C78 C 0.2504(4) 0.5331(3) 0.5381(3) 0.111(2) Uani 1 1 d . . . H78A H 0.2830 0.5354 0.5121 0.167 Uiso 1 1 calc R . . H78B H 0.2860 0.5489 0.5759 0.167 Uiso 1 1 calc R . . H78C H 0.2015 0.5666 0.5247 0.167 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 0.01505(8) 0.01548(7) 0.01832(7) -0.00115(6) 0.00534(6) -0.00061(6) N1 0.0174(13) 0.0268(14) 0.0236(13) -0.0004(11) 0.0084(11) -0.0003(10) N2 0.0192(14) 0.0250(14) 0.0227(13) 0.0017(10) 0.0051(11) 0.0010(10) N3 0.0193(13) 0.0193(12) 0.0193(13) 0.0003(10) 0.0089(11) -0.0015(10) N4 0.0196(13) 0.0191(12) 0.0193(13) 0.0011(10) 0.0091(11) -0.0005(10) N5 0.0206(14) 0.0232(13) 0.0244(14) -0.0057(10) 0.0124(11) -0.0049(10) N6 0.0155(13) 0.0203(12) 0.0223(13) -0.0022(10) 0.0076(11) -0.0029(10) C1 0.0163(15) 0.0179(13) 0.0289(16) -0.0028(13) 0.0083(13) -0.0006(12) C2 0.0186(16) 0.0287(16) 0.0219(16) 0.0027(13) 0.0037(13) 0.0007(13) C3 0.0215(17) 0.0286(17) 0.0290(17) -0.0014(13) 0.0055(14) -0.0017(13) C4 0.0269(19) 0.041(2) 0.0287(18) -0.0017(15) 0.0025(15) -0.0009(15) C5 0.033(2) 0.044(2) 0.0255(18) 0.0038(15) 0.0054(16) 0.0013(16) C6 0.032(2) 0.0340(18) 0.0322(19) 0.0081(15) 0.0102(16) -0.0018(15) C7 0.0217(17) 0.0309(17) 0.0256(17) 0.0003(13) 0.0060(14) -0.0029(13) C8 0.0183(16) 0.0264(16) 0.0276(17) -0.0024(13) 0.0107(14) -0.0013(12) C9 0.034(2) 0.0256(17) 0.041(2) -0.0043(15) 0.0184(17) 0.0012(14) C10 0.040(2) 0.0362(19) 0.045(2) -0.0046(17) 0.0254(19) 0.0082(16) C11 0.036(2) 0.048(2) 0.035(2) -0.0042(17) 0.0209(17) 0.0002(17) C12 0.049(2) 0.042(2) 0.033(2) 0.0076(16) 0.0220(19) 0.0081(17) C13 0.035(2) 0.0366(19) 0.0295(18) 0.0053(15) 0.0146(16) 0.0098(15) C14 0.0226(17) 0.0246(15) 0.0275(17) -0.0009(13) 0.0085(14) -0.0017(13) C15 0.0247(18) 0.0233(15) 0.0256(16) -0.0001(13) 0.0091(14) 0.0006(13) C16 0.0153(15) 0.0220(15) 0.0288(17) -0.0038(12) 0.0076(13) 0.0007(12) C17 0.0260(18) 0.0384(19) 0.040(2) 0.0074(17) 0.0120(16) 0.0013(16) C18 0.027(2) 0.039(2) 0.065(3) -0.0012(19) 0.0246(19) -0.0015(16) C19 0.0177(18) 0.046(2) 0.057(3) -0.0161(19) 0.0074(18) 0.0056(15) C20 0.032(2) 0.051(2) 0.032(2) -0.0115(17) -0.0019(17) 0.0140(17) C21 0.0268(18) 0.0343(17) 0.0237(16) -0.0059(14) 0.0091(14) 0.0035(14) C22 0.0161(15) 0.0177(14) 0.0223(15) -0.0001(12) 0.0048(13) 0.0010(11) C23 0.0213(16) 0.0151(13) 0.0226(15) 0.0018(11) 0.0096(13) -0.0007(11) C24 0.0230(17) 0.0159(14) 0.0254(16) 0.0017(12) 0.0099(14) -0.0006(12) C25 0.0207(17) 0.0283(16) 0.0302(18) -0.0006(14) 0.0095(14) -0.0006(13) C26 0.032(2) 0.0285(17) 0.0361(19) -0.0030(14) 0.0220(16) -0.0010(14) C27 0.037(2) 0.0256(16) 0.0237(16) -0.0021(13) 0.0146(15) -0.0039(14) C28 0.0259(17) 0.0158(14) 0.0213(15) 0.0003(11) 0.0094(13) -0.0014(12) C29 0.0207(17) 0.0229(15) 0.0259(16) 0.0026(13) 0.0062(14) 0.0036(12) C30 0.0283(19) 0.0300(17) 0.0344(19) -0.0005(14) 0.0070(16) -0.0008(14) C31 0.034(2) 0.0315(18) 0.0332(19) 0.0058(15) 0.0063(16) 0.0000(15) C32 0.0285(19) 0.0282(17) 0.0218(16) -0.0017(13) 0.0058(14) 0.0041(13) C33 0.047(2) 0.038(2) 0.0249(18) 0.0022(15) 0.0052(17) 0.0065(17) C34 0.0237(19) 0.042(2) 0.0265(18) -0.0045(15) 0.0053(15) -0.0071(15) C35 0.0226(16) 0.0171(14) 0.0238(16) 0.0018(12) 0.0115(13) 0.0033(12) C36 0.0323(19) 0.0215(15) 0.0278(17) -0.0012(13) 0.0145(15) 0.0025(13) C37 0.053(2) 0.0281(18) 0.0291(18) 0.0072(14) 0.0189(18) 0.0033(16) C38 0.056(3) 0.0267(18) 0.044(2) 0.0067(16) 0.032(2) -0.0036(17) C39 0.037(2) 0.0230(16) 0.044(2) -0.0029(15) 0.0243(18) -0.0053(14) C40 0.0222(16) 0.0185(14) 0.0305(17) -0.0012(13) 0.0134(14) 0.0011(13) C41 0.031(2) 0.0359(19) 0.0294(19) 0.0005(15) 0.0050(16) 0.0026(15) C42 0.042(3) 0.054(3) 0.096(4) -0.038(3) 0.015(3) -0.005(2) C43 0.048(3) 0.060(3) 0.053(3) 0.004(2) -0.002(2) 0.006(2) C44 0.0194(16) 0.0225(16) 0.0344(18) -0.0012(13) 0.0084(14) -0.0010(12) C45 0.0237(19) 0.038(2) 0.055(2) -0.0118(17) 0.0127(18) -0.0005(15) C46 0.0272(19) 0.0313(18) 0.037(2) -0.0059(15) 0.0107(16) -0.0007(14) C47 0.0192(16) 0.0184(14) 0.0190(15) -0.0013(11) 0.0050(13) -0.0032(12) C48 0.0234(17) 0.0223(15) 0.0343(18) -0.0064(13) 0.0188(15) -0.0065(13) C49 0.0305(19) 0.0356(18) 0.0353(19) -0.0158(15) 0.0198(16) -0.0088(15) C50 0.043(2) 0.055(2) 0.042(2) -0.0272(19) 0.0234(19) -0.0108(19) C51 0.045(2) 0.045(2) 0.066(3) -0.026(2) 0.032(2) -0.0014(19) C52 0.029(2) 0.035(2) 0.063(3) -0.0123(18) 0.0245(19) -0.0009(15) C53 0.0255(18) 0.0235(16) 0.042(2) -0.0078(14) 0.0186(16) -0.0041(13) C54 0.041(2) 0.0362(19) 0.0274(18) -0.0096(15) 0.0169(17) -0.0095(16) C55 0.044(2) 0.049(2) 0.037(2) -0.0084(17) 0.0224(19) -0.0136(18) C56 0.060(3) 0.054(2) 0.035(2) -0.0112(18) 0.023(2) -0.027(2) C57 0.032(2) 0.0239(16) 0.040(2) -0.0013(14) 0.0144(17) 0.0040(14) C58 0.049(2) 0.044(2) 0.056(3) 0.0045(19) 0.028(2) -0.0014(18) C59 0.041(2) 0.0327(19) 0.048(2) 0.0020(17) 0.0137(19) 0.0031(16) C60 0.0190(16) 0.0155(13) 0.0250(16) -0.0021(12) 0.0097(13) -0.0024(11) C61 0.0194(16) 0.0205(15) 0.0276(17) -0.0043(12) 0.0093(14) -0.0029(12) C62 0.0182(17) 0.0300(17) 0.0331(19) -0.0037(14) 0.0055(15) -0.0049(13) C63 0.0206(17) 0.0269(16) 0.0373(19) -0.0019(14) 0.0115(15) -0.0058(13) C64 0.0270(18) 0.0208(15) 0.0295(17) 0.0003(13) 0.0149(15) -0.0014(13) C65 0.0189(16) 0.0176(14) 0.0248(16) -0.0010(12) 0.0087(13) 0.0001(11) C66 0.0217(17) 0.0342(18) 0.0261(17) -0.0071(14) 0.0073(14) -0.0066(14) C67 0.039(2) 0.069(3) 0.035(2) -0.0232(19) 0.0123(19) -0.021(2) C68 0.110(4) 0.046(2) 0.041(2) 0.0095(19) 0.039(3) 0.007(2) C69 0.0231(17) 0.0210(15) 0.0233(16) -0.0012(12) 0.0076(14) -0.0062(12) C70 0.0239(18) 0.0279(17) 0.0329(19) -0.0011(14) 0.0050(15) -0.0027(13) C71 0.034(2) 0.0325(18) 0.0280(18) -0.0019(14) 0.0127(16) -0.0038(15) C72 0.049(3) 0.043(2) 0.051(3) 0.0070(19) 0.015(2) -0.0015(19) C73 0.106(4) 0.058(3) 0.049(3) 0.011(2) 0.040(3) 0.023(3) C74 0.201(7) 0.053(3) 0.053(3) -0.019(3) 0.024(4) 0.013(4) C75 0.102(4) 0.045(3) 0.091(4) 0.000(3) 0.020(4) -0.024(3) C76 0.059(3) 0.062(3) 0.069(3) 0.021(3) 0.037(3) 0.009(2) C77 0.076(3) 0.055(3) 0.039(2) -0.007(2) 0.019(2) 0.018(2) C78 0.141(6) 0.070(4) 0.122(6) 0.020(4) 0.040(5) -0.034(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 N2 2.374(2) . ? Sm1 N4 2.386(2) . ? Sm1 N5 2.454(2) . ? Sm1 N6 2.458(2) . ? Sm1 N1 2.459(2) . ? Sm1 N3 2.534(2) . ? Sm1 C1 2.814(3) . ? Sm1 C22 2.840(3) . ? Sm1 C47 2.843(3) . ? N1 C1 1.324(4) . ? N1 C8 1.468(4) . ? N2 C1 1.350(4) . ? N2 C2 1.464(4) . ? N3 C22 1.318(3) . ? N3 C23 1.427(4) . ? N4 C22 1.320(3) . ? N4 C35 1.429(3) . ? N5 C47 1.317(4) . ? N5 C48 1.439(4) . ? N6 C47 1.323(3) . ? N6 C60 1.432(3) . ? C1 C14 1.457(4) . ? C2 C7 1.518(4) . ? C2 C3 1.529(4) . ? C3 C4 1.525(4) . ? C4 C5 1.528(4) . ? C5 C6 1.526(4) . ? C6 C7 1.526(4) . ? C8 C13 1.516(4) . ? C8 C9 1.531(4) . ? C9 C10 1.526(4) . ? C10 C11 1.520(5) . ? C11 C12 1.527(5) . ? C12 C13 1.530(4) . ? C14 C15 1.191(4) . ? C15 C16 1.432(4) . ? C16 C21 1.386(4) . ? C16 C17 1.389(4) . ? C17 C18 1.381(4) . ? C18 C19 1.366(5) . ? C19 C20 1.375(5) . ? C20 C21 1.381(4) . ? C23 C28 1.407(4) . ? C23 C24 1.411(4) . ? C24 C25 1.393(4) . ? C24 C29 1.519(4) . ? C25 C26 1.384(4) . ? C26 C27 1.376(4) . ? C27 C28 1.396(4) . ? C28 C32 1.513(4) . ? C29 C31 1.535(4) . ? C29 C30 1.538(4) . ? C32 C33 1.529(4) . ? C32 C34 1.530(4) . ? C35 C40 1.400(4) . ? C35 C36 1.406(4) . ? C36 C37 1.397(4) . ? C36 C41 1.526(4) . ? C37 C38 1.379(5) . ? C38 C39 1.373(5) . ? C39 C40 1.392(4) . ? C40 C44 1.515(4) . ? C41 C42 1.510(5) . ? C41 C43 1.518(5) . ? C44 C46 1.529(4) . ? C44 C45 1.534(4) . ? C48 C49 1.399(4) . ? C48 C53 1.408(4) . ? C49 C50 1.398(4) . ? C49 C54 1.511(5) . ? C50 C51 1.373(5) . ? C51 C52 1.374(5) . ? C52 C53 1.398(4) . ? C53 C57 1.510(5) . ? C54 C56 1.532(4) . ? C54 C55 1.533(4) . ? C57 C58 1.528(4) . ? C57 C59 1.529(5) . ? C60 C61 1.407(4) . ? C60 C65 1.411(4) . ? C61 C62 1.395(4) . ? C61 C66 1.520(4) . ? C62 C63 1.377(4) . ? C63 C64 1.383(4) . ? C64 C65 1.393(4) . ? C65 C69 1.517(4) . ? C66 C67 1.521(4) . ? C66 C68 1.528(5) . ? C69 C71 1.521(4) . ? C69 C70 1.533(4) . ? C72 C73 1.349(6) . ? C72 C77 1.385(5) . ? C72 C78 1.511(6) . ? C73 C74 1.356(7) . ? C74 C75 1.351(7) . ? C75 C76 1.362(6) . ? C76 C77 1.379(6) . ? 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 N4 114.25(8) . . ? N2 Sm1 N5 101.61(8) . . ? N4 Sm1 N5 132.01(8) . . ? N2 Sm1 N6 127.07(8) . . ? N4 Sm1 N6 115.20(8) . . ? N5 Sm1 N6 55.19(8) . . ? N2 Sm1 N1 56.63(8) . . ? N4 Sm1 N1 88.17(8) . . ? N5 Sm1 N1 85.91(8) . . ? N6 Sm1 N1 141.05(8) . . ? N2 Sm1 N3 107.19(8) . . ? N4 Sm1 N3 55.11(7) . . ? N5 Sm1 N3 141.28(8) . . ? N6 Sm1 N3 86.56(7) . . ? N1 Sm1 N3 131.70(8) . . ? N2 Sm1 C1 28.58(8) . . ? N4 Sm1 C1 102.57(8) . . ? N5 Sm1 C1 93.85(8) . . ? N6 Sm1 C1 141.41(8) . . ? N1 Sm1 C1 28.05(8) . . ? N3 Sm1 C1 123.47(8) . . ? N2 Sm1 C22 111.98(8) . . ? N4 Sm1 C22 27.54(8) . . ? N5 Sm1 C22 146.30(8) . . ? N6 Sm1 C22 103.22(8) . . ? N1 Sm1 C22 109.98(8) . . ? N3 Sm1 C22 27.65(7) . . ? C1 Sm1 C22 114.30(8) . . ? N2 Sm1 C47 115.60(8) . . ? N4 Sm1 C47 129.62(8) . . ? N5 Sm1 C47 27.57(8) . . ? N6 Sm1 C47 27.70(8) . . ? N1 Sm1 C47 113.47(8) . . ? N3 Sm1 C47 114.22(8) . . ? C1 Sm1 C47 117.81(8) . . ? C22 Sm1 C47 127.69(8) . . ? C1 N1 C8 118.5(2) . . ? C1 N1 Sm1 91.09(17) . . ? C8 N1 Sm1 149.94(19) . . ? C1 N2 C2 118.6(2) . . ? C1 N2 Sm1 94.15(18) . . ? C2 N2 Sm1 146.31(19) . . ? C22 N3 C23 117.7(2) . . ? C22 N3 Sm1 89.23(17) . . ? C23 N3 Sm1 153.05(17) . . ? C22 N4 C35 119.0(2) . . ? C22 N4 Sm1 95.76(17) . . ? C35 N4 Sm1 143.31(18) . . ? C47 N5 C48 116.8(2) . . ? C47 N5 Sm1 92.88(17) . . ? C48 N5 Sm1 149.42(19) . . ? C47 N6 C60 118.0(2) . . ? C47 N6 Sm1 92.56(17) . . ? C60 N6 Sm1 149.28(18) . . ? N1 C1 N2 118.1(3) . . ? N1 C1 C14 121.5(3) . . ? N2 C1 C14 120.4(3) . . ? N1 C1 Sm1 60.86(15) . . ? N2 C1 Sm1 57.27(14) . . ? C14 C1 Sm1 177.3(2) . . ? N2 C2 C7 110.1(2) . . ? N2 C2 C3 114.0(2) . . ? C7 C2 C3 110.2(3) . . ? C4 C3 C2 111.3(3) . . ? C3 C4 C5 113.0(3) . . ? C6 C5 C4 111.4(3) . . ? C7 C6 C5 111.5(3) . . ? C2 C7 C6 111.5(3) . . ? N1 C8 C13 111.2(2) . . ? N1 C8 C9 111.8(2) . . ? C13 C8 C9 109.7(3) . . ? C10 C9 C8 111.2(3) . . ? C11 C10 C9 112.3(3) . . ? C10 C11 C12 110.3(3) . . ? C11 C12 C13 111.6(3) . . ? C8 C13 C12 111.0(3) . . ? C15 C14 C1 179.4(4) . . ? C14 C15 C16 177.0(3) . . ? C21 C16 C17 119.1(3) . . ? C21 C16 C15 119.5(3) . . ? C17 C16 C15 121.4(3) . . ? C18 C17 C16 120.1(3) . . ? C19 C18 C17 120.4(3) . . ? C18 C19 C20 119.9(3) . . ? C19 C20 C21 120.5(3) . . ? C20 C21 C16 119.9(3) . . ? N3 C22 N4 119.6(3) . . ? N3 C22 Sm1 63.12(15) . . ? N4 C22 Sm1 56.70(14) . . ? C28 C23 C24 119.9(3) . . ? C28 C23 N3 119.5(3) . . ? C24 C23 N3 120.6(3) . . ? C25 C24 C23 118.6(3) . . ? C25 C24 C29 120.3(3) . . ? C23 C24 C29 121.1(3) . . ? C26 C25 C24 121.4(3) . . ? C27 C26 C25 119.9(3) . . ? C26 C27 C28 120.8(3) . . ? C27 C28 C23 119.4(3) . . ? C27 C28 C32 120.5(3) . . ? C23 C28 C32 120.0(3) . . ? C24 C29 C31 112.3(2) . . ? C24 C29 C30 112.2(3) . . ? C31 C29 C30 108.7(3) . . ? C28 C32 C33 114.2(3) . . ? C28 C32 C34 109.6(2) . . ? C33 C32 C34 110.1(3) . . ? C40 C35 C36 120.9(3) . . ? C40 C35 N4 120.6(3) . . ? C36 C35 N4 118.4(3) . . ? C37 C36 C35 118.5(3) . . ? C37 C36 C41 120.3(3) . . ? C35 C36 C41 121.2(3) . . ? C38 C37 C36 120.6(3) . . ? C39 C38 C37 120.2(3) . . ? C38 C39 C40 121.4(3) . . ? C39 C40 C35 118.3(3) . . ? C39 C40 C44 119.0(3) . . ? C35 C40 C44 122.7(3) . . ? C42 C41 C43 110.9(3) . . ? C42 C41 C36 110.3(3) . . ? C43 C41 C36 114.4(3) . . ? C40 C44 C46 110.5(3) . . ? C40 C44 C45 112.8(3) . . ? C46 C44 C45 109.5(3) . . ? N5 C47 N6 119.0(3) . . ? N5 C47 Sm1 59.56(15) . . ? N6 C47 Sm1 59.74(14) . . ? C49 C48 C53 121.0(3) . . ? C49 C48 N5 119.7(3) . . ? C53 C48 N5 119.3(3) . . ? C50 C49 C48 117.7(3) . . ? C50 C49 C54 119.3(3) . . ? C48 C49 C54 123.0(3) . . ? C51 C50 C49 122.4(4) . . ? C50 C51 C52 118.9(3) . . ? C51 C52 C53 121.8(4) . . ? C52 C53 C48 118.1(3) . . ? C52 C53 C57 119.2(3) . . ? C48 C53 C57 122.7(3) . . ? C49 C54 C56 112.3(3) . . ? C49 C54 C55 111.0(3) . . ? C56 C54 C55 109.9(3) . . ? C53 C57 C58 111.4(3) . . ? C53 C57 C59 112.3(3) . . ? C58 C57 C59 110.1(3) . . ? C61 C60 C65 120.8(3) . . ? C61 C60 N6 120.9(3) . . ? C65 C60 N6 118.3(3) . . ? C62 C61 C60 118.0(3) . . ? C62 C61 C66 118.9(3) . . ? C60 C61 C66 123.1(3) . . ? C63 C62 C61 121.9(3) . . ? C62 C63 C64 119.6(3) . . ? C63 C64 C65 121.1(3) . . ? C64 C65 C60 118.6(3) . . ? C64 C65 C69 119.9(3) . . ? C60 C65 C69 121.4(3) . . ? C61 C66 C67 112.7(3) . . ? C61 C66 C68 111.5(3) . . ? C67 C66 C68 109.4(3) . . ? C65 C69 C71 113.8(3) . . ? C65 C69 C70 110.4(2) . . ? C71 C69 C70 109.8(3) . . ? C73 C72 C77 117.7(4) . . ? C73 C72 C78 121.9(5) . . ? C77 C72 C78 120.4(4) . . ? C72 C73 C74 121.5(5) . . ? C75 C74 C73 121.3(5) . . ? C74 C75 C76 119.0(5) . . ? C75 C76 C77 119.8(4) . . ? C76 C77 C72 120.7(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.574 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.083 # Attachment '8.C6D6.CIF' data_mono _database_code_depnum_ccdc_archive 'CCDC 752062' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C77 H97 N6 Sm, C6 D6' _chemical_formula_sum 'C83 H97 D6 N6 Sm' _chemical_formula_weight 1341.10 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' D D 0.0000 0.0000 '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 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 12.6946(2) _cell_length_b 24.0285(4) _cell_length_c 24.4564(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.565(1) _cell_angle_gamma 90.00 _cell_volume 7281.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9059 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 30.03 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2820 _exptl_absorpt_coefficient_mu 0.853 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 X8 Apex CCD' _diffrn_measurement_method 'thin slice phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 102410 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16724 _reflns_number_gt 15474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 v2.0' _computing_cell_refinement 'Bruker Apex2 v2.0' _computing_data_reduction 'Bruker Apex2 v2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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^)+(0.0039P)^2^+28.1954P] 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 16724 _refine_ls_number_parameters 787 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.320 _refine_ls_restrained_S_all 1.323 _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 0.187468(16) 0.668607(8) 0.284712(9) 0.01576(6) Uani 1 1 d . . . N1 N 0.2179(3) 0.59346(14) 0.35421(15) 0.0228(7) Uani 1 1 d . . . N2 N 0.2613(3) 0.57744(15) 0.26937(16) 0.0268(8) Uani 1 1 d . . . N3 N 0.2850(3) 0.72535(13) 0.22857(14) 0.0175(7) Uani 1 1 d . . . N4 N 0.3349(3) 0.73283(14) 0.32385(14) 0.0177(7) Uani 1 1 d . . . N5 N 0.0308(3) 0.71647(14) 0.30738(14) 0.0175(7) Uani 1 1 d . . . N6 N 0.0037(3) 0.66488(14) 0.22569(13) 0.0183(7) Uani 1 1 d . . . C1 C 0.2560(3) 0.55920(17) 0.32048(19) 0.0245(9) Uani 1 1 d . . . C2 C 0.2226(3) 0.57289(17) 0.40975(18) 0.0225(9) Uani 1 1 d . . . C3 C 0.3106(3) 0.58718(18) 0.45230(19) 0.0258(9) Uani 1 1 d . . . C4 C 0.3195(4) 0.56458(19) 0.50554(19) 0.0273(9) Uani 1 1 d . . . H4 H 0.3794 0.5744 0.5345 0.033 Uiso 1 1 calc R . . C5 C 0.2425(4) 0.52784(19) 0.51709(19) 0.0279(10) Uani 1 1 d . . . C6 C 0.1551(4) 0.51517(18) 0.47461(19) 0.0275(9) Uani 1 1 d . . . H6 H 0.1011 0.4909 0.4824 0.033 Uiso 1 1 calc R . . C7 C 0.1432(3) 0.53666(18) 0.42062(19) 0.0250(9) Uani 1 1 d . . . C8 C 0.3963(4) 0.6258(2) 0.4406(2) 0.0384(12) Uani 1 1 d . . . H8A H 0.4257 0.6109 0.4098 0.058 Uiso 1 1 calc R . . H8B H 0.4542 0.6292 0.4742 0.058 Uiso 1 1 calc R . . H8C H 0.3647 0.6626 0.4303 0.058 Uiso 1 1 calc R . . C9 C 0.2555(4) 0.5020(2) 0.5745(2) 0.0376(11) Uani 1 1 d . . . H9A H 0.1901 0.5087 0.5887 0.056 Uiso 1 1 calc R . . H9B H 0.3176 0.5188 0.6000 0.056 Uiso 1 1 calc R . . H9C H 0.2671 0.4619 0.5719 0.056 Uiso 1 1 calc R . . C10 C 0.0499(4) 0.5198(2) 0.3752(2) 0.0334(11) Uani 1 1 d . . . H10A H 0.0141 0.5531 0.3568 0.050 Uiso 1 1 calc R . . H10B H -0.0015 0.4982 0.3914 0.050 Uiso 1 1 calc R . . H10C H 0.0758 0.4969 0.3477 0.050 Uiso 1 1 calc R . . C11 C 0.2977(4) 0.53806(17) 0.2336(2) 0.0272(10) Uani 1 1 d . . . C12 C 0.4060(4) 0.52115(19) 0.2443(2) 0.0363(12) Uani 1 1 d . . . C13 C 0.4336(4) 0.4793(2) 0.2099(3) 0.0443(14) Uani 1 1 d . . . H13 H 0.5064 0.4669 0.2168 0.053 Uiso 1 1 calc R . . C14 C 0.3597(5) 0.4552(2) 0.1666(3) 0.0501(16) Uani 1 1 d . . . C15 C 0.2556(4) 0.4757(2) 0.1553(3) 0.0421(13) Uani 1 1 d . . . H15 H 0.2047 0.4613 0.1241 0.050 Uiso 1 1 calc R . . C16 C 0.2230(4) 0.51670(19) 0.1882(2) 0.0337(11) Uani 1 1 d . . . C17 C 0.4893(4) 0.5453(2) 0.2909(2) 0.0431(13) Uani 1 1 d . . . H17A H 0.4763 0.5853 0.2938 0.065 Uiso 1 1 calc R . . H17B H 0.5612 0.5394 0.2833 0.065 Uiso 1 1 calc R . . H17C H 0.4851 0.5270 0.3262 0.065 Uiso 1 1 calc R . . C18 C 0.3910(6) 0.4079(3) 0.1326(4) 0.084(3) Uani 1 1 d . . . H18A H 0.3631 0.3728 0.1442 0.126 Uiso 1 1 calc R . . H18B H 0.4698 0.4059 0.1389 0.126 Uiso 1 1 calc R . . H18C H 0.3603 0.4143 0.0928 0.126 Uiso 1 1 calc R . . C19 C 0.1087(4) 0.5374(2) 0.1747(3) 0.0478(14) Uani 1 1 d . . . H19A H 0.0777 0.5342 0.2080 0.072 Uiso 1 1 calc R . . H19B H 0.0660 0.5151 0.1442 0.072 Uiso 1 1 calc R . . H19C H 0.1076 0.5765 0.1631 0.072 Uiso 1 1 calc R . . C20 C 0.2891(4) 0.50346(18) 0.3386(2) 0.0274(9) Uani 1 1 d . . . C21 C 0.3172(3) 0.45837(18) 0.35665(19) 0.0262(9) Uani 1 1 d . . . C22 C 0.3495(3) 0.40395(17) 0.37734(19) 0.0248(9) Uani 1 1 d . . . C23 C 0.3216(4) 0.3842(2) 0.4257(2) 0.0324(10) Uani 1 1 d . . . H23 H 0.2838 0.4076 0.4462 0.039 Uiso 1 1 calc R . . C24 C 0.3486(4) 0.3308(2) 0.4437(2) 0.0407(12) Uani 1 1 d . . . H24 H 0.3292 0.3173 0.4766 0.049 Uiso 1 1 calc R . . C25 C 0.4036(4) 0.2969(2) 0.4142(2) 0.0405(13) Uani 1 1 d . . . H25 H 0.4215 0.2599 0.4267 0.049 Uiso 1 1 calc R . . C26 C 0.4329(4) 0.3163(2) 0.3666(2) 0.0381(12) Uani 1 1 d . . . H26 H 0.4714 0.2928 0.3466 0.046 Uiso 1 1 calc R . . C27 C 0.4066(4) 0.36982(19) 0.3480(2) 0.0304(10) Uani 1 1 d . . . H27 H 0.4272 0.3833 0.3153 0.036 Uiso 1 1 calc R . . C28 C 0.3480(3) 0.74702(16) 0.27372(16) 0.0161(7) Uani 1 1 d . . . H28 H 0.4027 0.7728 0.2700 0.019 Uiso 1 1 calc R . . C29 C 0.2982(3) 0.74505(17) 0.17541(15) 0.0164(8) Uani 1 1 d . . . C30 C 0.2711(3) 0.80024(17) 0.15826(17) 0.0194(8) Uani 1 1 d . . . C31 C 0.2837(3) 0.81761(18) 0.10576(17) 0.0232(9) Uani 1 1 d . . . H31 H 0.2656 0.8548 0.0941 0.028 Uiso 1 1 calc R . . C32 C 0.3218(3) 0.78202(19) 0.07036(18) 0.0250(9) Uani 1 1 d . . . H32 H 0.3300 0.7945 0.0347 0.030 Uiso 1 1 calc R . . C33 C 0.3478(3) 0.72818(18) 0.08713(18) 0.0236(9) Uani 1 1 d . . . H33 H 0.3743 0.7038 0.0627 0.028 Uiso 1 1 calc R . . C34 C 0.3364(3) 0.70862(17) 0.13882(17) 0.0199(8) Uani 1 1 d . . . C35 C 0.2330(3) 0.84326(17) 0.19559(18) 0.0229(9) Uani 1 1 d . . . H35 H 0.2180 0.8234 0.2290 0.027 Uiso 1 1 calc R . . C36 C 0.1292(4) 0.8723(2) 0.1661(2) 0.0361(11) Uani 1 1 d . . . H36A H 0.1079 0.8994 0.1916 0.054 Uiso 1 1 calc R . . H36B H 0.0718 0.8446 0.1552 0.054 Uiso 1 1 calc R . . H36C H 0.1413 0.8915 0.1327 0.054 Uiso 1 1 calc R . . C37 C 0.3219(4) 0.88587(19) 0.2164(2) 0.0335(10) Uani 1 1 d . . . H37A H 0.2964 0.9133 0.2402 0.050 Uiso 1 1 calc R . . H37B H 0.3406 0.9048 0.1843 0.050 Uiso 1 1 calc R . . H37C H 0.3858 0.8669 0.2381 0.050 Uiso 1 1 calc R . . C38 C 0.3720(4) 0.64982(18) 0.1564(2) 0.0278(10) Uani 1 1 d . . . H38 H 0.3348 0.6383 0.1867 0.033 Uiso 1 1 calc R . . C39 C 0.3431(5) 0.6078(2) 0.1089(2) 0.0460(14) Uani 1 1 d . . . H39A H 0.2648 0.6076 0.0945 0.069 Uiso 1 1 calc R . . H39B H 0.3670 0.5707 0.1228 0.069 Uiso 1 1 calc R . . H39C H 0.3790 0.6182 0.0787 0.069 Uiso 1 1 calc R . . C40 C 0.4915(5) 0.6494(2) 0.1804(3) 0.0489(14) Uani 1 1 d . . . H40A H 0.5148 0.6115 0.1919 0.073 Uiso 1 1 calc R . . H40B H 0.5080 0.6742 0.2130 0.073 Uiso 1 1 calc R . . H40C H 0.5296 0.6624 0.1520 0.073 Uiso 1 1 calc R . . C41 C 0.4092(3) 0.75640(16) 0.37072(16) 0.0183(8) Uani 1 1 d . . . C42 C 0.3690(3) 0.79264(18) 0.40658(17) 0.0217(8) Uani 1 1 d . . . C43 C 0.4407(3) 0.81536(18) 0.45207(17) 0.0243(9) Uani 1 1 d . . . H43 H 0.4142 0.8398 0.4765 0.029 Uiso 1 1 calc R . . C44 C 0.5499(4) 0.80321(19) 0.46273(19) 0.0278(9) Uani 1 1 d . . . H44 H 0.5978 0.8192 0.4940 0.033 Uiso 1 1 calc R . . C45 C 0.5883(3) 0.76753(18) 0.42730(19) 0.0255(9) Uani 1 1 d . . . H45 H 0.6633 0.7593 0.4345 0.031 Uiso 1 1 calc R . . C46 C 0.5197(3) 0.74323(17) 0.38120(18) 0.0217(8) Uani 1 1 d . . . C47 C 0.2524(3) 0.8110(2) 0.39324(19) 0.0296(10) Uani 1 1 d . . . H47 H 0.2085 0.7801 0.3723 0.035 Uiso 1 1 calc R . . C48 C 0.2410(5) 0.8613(3) 0.3547(2) 0.0586(18) Uani 1 1 d . . . H48A H 0.1655 0.8735 0.3457 0.088 Uiso 1 1 calc R . . H48B H 0.2633 0.8512 0.3201 0.088 Uiso 1 1 calc R . . H48C H 0.2867 0.8916 0.3734 0.088 Uiso 1 1 calc R . . C49 C 0.2063(4) 0.8242(2) 0.4444(2) 0.0347(11) Uani 1 1 d . . . H49A H 0.1307 0.8356 0.4322 0.052 Uiso 1 1 calc R . . H49B H 0.2478 0.8545 0.4657 0.052 Uiso 1 1 calc R . . H49C H 0.2109 0.7911 0.4682 0.052 Uiso 1 1 calc R . . C50 C 0.5680(3) 0.70391(18) 0.34440(19) 0.0258(9) Uani 1 1 d . . . H50 H 0.5075 0.6853 0.3177 0.031 Uiso 1 1 calc R . . C51 C 0.6361(4) 0.7356(2) 0.3104(2) 0.0327(11) Uani 1 1 d . . . H51A H 0.6663 0.7094 0.2872 0.049 Uiso 1 1 calc R . . H51B H 0.6949 0.7550 0.3359 0.049 Uiso 1 1 calc R . . H51C H 0.5907 0.7629 0.2863 0.049 Uiso 1 1 calc R . . C52 C 0.6370(4) 0.6588(2) 0.3794(2) 0.0340(11) Uani 1 1 d . . . H52A H 0.6668 0.6341 0.3546 0.051 Uiso 1 1 calc R . . H52B H 0.5922 0.6371 0.3996 0.051 Uiso 1 1 calc R . . H52C H 0.6962 0.6763 0.4064 0.051 Uiso 1 1 calc R . . C53 C -0.0337(3) 0.69494(16) 0.26285(16) 0.0180(8) Uani 1 1 d . . . H53 H -0.1092 0.7011 0.2572 0.022 Uiso 1 1 calc R . . C54 C -0.0215(3) 0.74908(17) 0.34265(16) 0.0180(8) Uani 1 1 d . . . C55 C -0.0277(3) 0.72838(17) 0.39530(17) 0.0208(8) Uani 1 1 d . . . C56 C -0.0778(3) 0.76066(19) 0.42963(18) 0.0263(9) Uani 1 1 d . . . H56 H -0.0821 0.7469 0.4655 0.032 Uiso 1 1 calc R . . C57 C -0.1212(3) 0.81188(19) 0.41293(19) 0.0277(10) Uani 1 1 d . . . H57 H -0.1543 0.8334 0.4371 0.033 Uiso 1 1 calc R . . C58 C -0.1160(3) 0.83171(19) 0.36066(18) 0.0256(9) Uani 1 1 d . . . H58 H -0.1469 0.8669 0.3489 0.031 Uiso 1 1 calc R . . C59 C -0.0666(3) 0.80140(17) 0.32465(18) 0.0214(8) Uani 1 1 d . . . C60 C 0.0185(3) 0.67256(18) 0.41727(17) 0.0213(8) Uani 1 1 d . . . H60 H 0.0446 0.6533 0.3865 0.026 Uiso 1 1 calc R . . C61 C -0.0658(4) 0.6350(2) 0.4353(2) 0.0372(12) Uani 1 1 d . . . H61A H -0.0325 0.5994 0.4488 0.056 Uiso 1 1 calc R . . H61B H -0.1259 0.6285 0.4032 0.056 Uiso 1 1 calc R . . H61C H -0.0929 0.6533 0.4654 0.056 Uiso 1 1 calc R . . C62 C 0.1149(4) 0.6805(2) 0.4664(2) 0.0356(11) Uani 1 1 d . . . H62A H 0.1442 0.6441 0.4799 0.053 Uiso 1 1 calc R . . H62B H 0.0915 0.7003 0.4967 0.053 Uiso 1 1 calc R . . H62C H 0.1707 0.7023 0.4540 0.053 Uiso 1 1 calc R . . C63 C -0.0685(4) 0.8253(2) 0.2669(2) 0.0351(11) Uani 1 1 d . . . H63 H -0.0102 0.8071 0.2515 0.042 Uiso 1 1 calc R . . C64 C -0.1774(5) 0.8138(2) 0.2271(2) 0.0501(15) Uani 1 1 d . . . H64A H -0.1768 0.8289 0.1899 0.075 Uiso 1 1 calc R . . H64B H -0.2352 0.8315 0.2417 0.075 Uiso 1 1 calc R . . H64C H -0.1899 0.7735 0.2242 0.075 Uiso 1 1 calc R . . C65 C -0.0509(4) 0.8883(2) 0.2677(3) 0.0478(15) Uani 1 1 d . . . H65A H -0.0520 0.9015 0.2297 0.072 Uiso 1 1 calc R . . H65B H 0.0190 0.8972 0.2922 0.072 Uiso 1 1 calc R . . H65C H -0.1085 0.9067 0.2819 0.072 Uiso 1 1 calc R . . C66 C -0.0785(3) 0.64608(17) 0.18004(17) 0.0202(8) Uani 1 1 d . . . C67 C -0.1485(3) 0.60253(17) 0.18720(18) 0.0226(9) Uani 1 1 d . . . C68 C -0.2342(4) 0.5892(2) 0.1432(2) 0.0337(11) Uani 1 1 d . . . H68 H -0.2829 0.5606 0.1482 0.040 Uiso 1 1 calc R . . C69 C -0.2499(4) 0.6165(2) 0.0928(2) 0.0408(13) Uani 1 1 d . . . H69 H -0.3095 0.6073 0.0634 0.049 Uiso 1 1 calc R . . C70 C -0.1784(4) 0.6575(2) 0.0851(2) 0.0383(12) Uani 1 1 d . . . H70 H -0.1883 0.6754 0.0497 0.046 Uiso 1 1 calc R . . C71 C -0.0924(4) 0.6732(2) 0.12761(18) 0.0288(9) Uani 1 1 d . . . C72 C -0.1326(3) 0.57032(18) 0.24191(19) 0.0240(9) Uani 1 1 d . . . H72 H -0.0574 0.5774 0.2635 0.029 Uiso 1 1 calc R . . C73 C -0.2098(4) 0.5897(2) 0.2777(2) 0.0395(12) Uani 1 1 d . . . H73A H -0.1973 0.5680 0.3125 0.059 Uiso 1 1 calc R . . H73B H -0.2844 0.5843 0.2570 0.059 Uiso 1 1 calc R . . H73C H -0.1974 0.6292 0.2867 0.059 Uiso 1 1 calc R . . C74 C -0.1448(4) 0.5081(2) 0.2321(3) 0.0425(13) Uani 1 1 d . . . H74A H -0.0948 0.4957 0.2092 0.064 Uiso 1 1 calc R . . H74B H -0.2191 0.4998 0.2125 0.064 Uiso 1 1 calc R . . H74C H -0.1286 0.4887 0.2681 0.064 Uiso 1 1 calc R . . C75 C -0.0154(4) 0.7177(2) 0.1163(2) 0.0351(11) Uani 1 1 d . . . H75 H 0.0314 0.7288 0.1530 0.042 Uiso 1 1 calc R . . C76 C -0.0747(5) 0.7697(2) 0.0896(2) 0.0400(12) Uani 1 1 d . . . H76A H -0.1209 0.7840 0.1137 0.060 Uiso 1 1 calc R . . H76B H -0.1192 0.7602 0.0528 0.060 Uiso 1 1 calc R . . H76C H -0.0220 0.7982 0.0853 0.060 Uiso 1 1 calc R . . C77 C 0.0576(4) 0.6941(2) 0.0799(2) 0.0421(13) Uani 1 1 d . . . H77A H 0.1080 0.7229 0.0733 0.063 Uiso 1 1 calc R . . H77B H 0.0135 0.6817 0.0440 0.063 Uiso 1 1 calc R . . H77C H 0.0984 0.6624 0.0991 0.063 Uiso 1 1 calc R . . C80 C 0.0256(7) 0.5551(3) -0.0090(4) 0.099(3) Uiso 1 1 d D . . D80 H 0.0443 0.5928 -0.0135 0.119 Uiso 1 1 calc R . . C79 C -0.0513(8) 0.5427(3) 0.0194(4) 0.118(4) Uiso 1 1 d D . . D79 H -0.0896 0.5725 0.0317 0.141 Uiso 1 1 calc R . . C81 C -0.0779(9) 0.4874(4) 0.0320(5) 0.162(5) Uiso 1 1 d D . . D81 H -0.1283 0.4797 0.0546 0.195 Uiso 1 1 calc R . . C87 C 0.4061(13) 0.5092(8) -0.0424(8) 0.239(9) Uiso 1 1 d D . . D87 H 0.3451 0.5194 -0.0706 0.286 Uiso 1 1 calc R . . C85 C 0.3982(11) 0.5036(8) 0.0141(10) 0.241(9) Uiso 1 1 d D . . D85 H 0.3298 0.5019 0.0239 0.289 Uiso 1 1 calc R . . C86 C 0.494(2) 0.5008(9) 0.0555(4) 0.247(9) Uiso 1 1 d D . . D86 H 0.4909 0.5058 0.0936 0.296 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 0.01510(9) 0.01290(9) 0.02016(10) 0.00204(8) 0.00582(7) 0.00119(8) N1 0.0274(18) 0.0177(17) 0.0259(19) 0.0054(14) 0.0114(15) 0.0050(14) N2 0.035(2) 0.0170(17) 0.034(2) 0.0032(15) 0.0187(17) 0.0062(15) N3 0.0192(16) 0.0152(16) 0.0184(17) 0.0008(13) 0.0050(13) -0.0001(13) N4 0.0161(15) 0.0180(16) 0.0195(17) 0.0010(13) 0.0050(13) -0.0001(13) N5 0.0156(15) 0.0187(17) 0.0184(17) 0.0014(13) 0.0040(13) 0.0017(13) N6 0.0197(15) 0.0182(16) 0.0170(16) -0.0006(14) 0.0036(13) -0.0028(13) C1 0.025(2) 0.017(2) 0.034(2) 0.0061(18) 0.0120(19) 0.0024(16) C2 0.024(2) 0.017(2) 0.027(2) 0.0047(17) 0.0089(17) 0.0062(16) C3 0.023(2) 0.023(2) 0.034(2) 0.0044(18) 0.0102(18) 0.0032(17) C4 0.026(2) 0.026(2) 0.029(2) 0.0011(19) 0.0029(18) 0.0022(18) C5 0.033(2) 0.024(2) 0.028(2) 0.0074(18) 0.0112(19) 0.0067(18) C6 0.027(2) 0.023(2) 0.034(3) 0.0072(19) 0.0095(19) -0.0005(17) C7 0.024(2) 0.021(2) 0.032(2) 0.0044(18) 0.0088(18) 0.0042(17) C8 0.032(3) 0.045(3) 0.037(3) 0.003(2) 0.008(2) -0.014(2) C9 0.050(3) 0.034(3) 0.029(3) 0.010(2) 0.008(2) 0.002(2) C10 0.027(2) 0.037(3) 0.036(3) 0.004(2) 0.005(2) -0.004(2) C11 0.036(2) 0.014(2) 0.038(3) 0.0043(18) 0.021(2) 0.0043(17) C12 0.039(3) 0.022(2) 0.056(3) 0.004(2) 0.027(2) 0.002(2) C13 0.040(3) 0.027(3) 0.075(4) -0.002(3) 0.033(3) 0.007(2) C14 0.056(4) 0.023(3) 0.082(5) -0.018(3) 0.039(3) -0.004(2) C15 0.047(3) 0.025(3) 0.062(4) -0.014(2) 0.027(3) -0.011(2) C16 0.038(3) 0.019(2) 0.051(3) 0.001(2) 0.024(2) 0.0009(19) C17 0.035(3) 0.043(3) 0.056(4) 0.004(3) 0.019(3) 0.001(2) C18 0.074(5) 0.050(4) 0.138(8) -0.053(5) 0.045(5) 0.002(4) C19 0.045(3) 0.044(3) 0.057(4) -0.005(3) 0.018(3) 0.010(3) C20 0.030(2) 0.021(2) 0.035(3) 0.0059(19) 0.0140(19) 0.0040(18) C21 0.025(2) 0.022(2) 0.032(2) 0.0009(18) 0.0067(18) 0.0008(17) C22 0.023(2) 0.018(2) 0.030(2) 0.0032(18) -0.0009(18) 0.0003(16) C23 0.034(2) 0.029(2) 0.033(3) 0.005(2) 0.006(2) 0.003(2) C24 0.043(3) 0.036(3) 0.041(3) 0.020(2) 0.005(2) 0.001(2) C25 0.036(3) 0.021(2) 0.059(4) 0.015(2) -0.002(2) 0.005(2) C26 0.036(3) 0.024(2) 0.052(3) 0.002(2) 0.005(2) 0.011(2) C27 0.028(2) 0.026(2) 0.036(3) 0.007(2) 0.003(2) 0.0071(18) C28 0.0146(17) 0.0179(19) 0.0151(19) 0.0011(15) 0.0013(14) 0.0003(14) C29 0.0137(17) 0.023(2) 0.0105(18) -0.0002(15) -0.0020(14) -0.0034(15) C30 0.0196(19) 0.019(2) 0.018(2) -0.0002(16) 0.0025(15) -0.0016(15) C31 0.026(2) 0.021(2) 0.020(2) 0.0039(16) 0.0012(17) -0.0002(16) C32 0.027(2) 0.032(2) 0.017(2) 0.0006(17) 0.0063(17) -0.0068(18) C33 0.023(2) 0.027(2) 0.022(2) -0.0059(17) 0.0078(17) -0.0043(17) C34 0.0176(18) 0.019(2) 0.024(2) -0.0036(16) 0.0062(16) -0.0024(15) C35 0.028(2) 0.017(2) 0.024(2) -0.0004(16) 0.0072(17) 0.0011(16) C36 0.034(3) 0.029(3) 0.044(3) -0.005(2) 0.005(2) 0.007(2) C37 0.036(3) 0.026(2) 0.038(3) -0.005(2) 0.006(2) 0.000(2) C38 0.038(2) 0.017(2) 0.032(2) 0.0009(18) 0.017(2) 0.0028(18) C39 0.068(4) 0.025(3) 0.051(3) -0.008(2) 0.025(3) -0.004(3) C40 0.047(3) 0.035(3) 0.067(4) 0.004(3) 0.017(3) 0.002(2) C41 0.0198(19) 0.0183(19) 0.0171(19) 0.0034(15) 0.0048(15) -0.0040(15) C42 0.022(2) 0.024(2) 0.020(2) 0.0030(17) 0.0055(16) -0.0011(16) C43 0.028(2) 0.027(2) 0.018(2) -0.0003(17) 0.0026(17) -0.0026(17) C44 0.027(2) 0.032(2) 0.022(2) 0.0032(18) -0.0013(18) -0.0063(19) C45 0.0167(19) 0.029(2) 0.029(2) 0.0081(19) 0.0008(17) -0.0016(17) C46 0.0198(19) 0.020(2) 0.026(2) 0.0059(17) 0.0066(17) -0.0017(16) C47 0.022(2) 0.039(3) 0.026(2) -0.012(2) 0.0020(18) 0.0047(19) C48 0.060(4) 0.081(5) 0.037(3) 0.014(3) 0.014(3) 0.041(4) C49 0.028(2) 0.043(3) 0.036(3) -0.010(2) 0.012(2) 0.001(2) C50 0.020(2) 0.026(2) 0.033(2) 0.0009(19) 0.0093(18) -0.0007(17) C51 0.030(2) 0.035(3) 0.037(3) 0.004(2) 0.016(2) -0.001(2) C52 0.022(2) 0.032(3) 0.050(3) 0.006(2) 0.013(2) 0.0068(19) C53 0.0170(18) 0.0187(19) 0.018(2) 0.0042(15) 0.0039(15) 0.0016(15) C54 0.0124(17) 0.022(2) 0.019(2) -0.0014(16) 0.0015(15) 0.0016(15) C55 0.0206(19) 0.022(2) 0.019(2) -0.0022(16) 0.0032(16) 0.0024(16) C56 0.028(2) 0.035(2) 0.016(2) -0.0032(18) 0.0056(17) 0.0048(19) C57 0.026(2) 0.031(2) 0.027(2) -0.0093(19) 0.0066(18) 0.0083(18) C58 0.025(2) 0.021(2) 0.031(2) -0.0010(19) 0.0061(18) 0.0056(18) C59 0.0184(19) 0.020(2) 0.026(2) 0.0025(17) 0.0057(16) 0.0014(16) C60 0.0216(19) 0.025(2) 0.0183(19) 0.0024(17) 0.0070(16) 0.0045(17) C61 0.028(2) 0.039(3) 0.047(3) 0.006(2) 0.013(2) 0.008(2) C62 0.035(3) 0.035(3) 0.031(3) -0.002(2) -0.006(2) 0.013(2) C63 0.040(3) 0.029(2) 0.043(3) 0.016(2) 0.024(2) 0.015(2) C64 0.078(4) 0.046(3) 0.018(3) 0.007(2) -0.007(3) 0.008(3) C65 0.041(3) 0.035(3) 0.069(4) 0.024(3) 0.016(3) 0.004(2) C66 0.0214(19) 0.021(2) 0.018(2) -0.0017(16) 0.0043(16) -0.0006(16) C67 0.022(2) 0.021(2) 0.025(2) -0.0005(17) 0.0050(17) -0.0003(16) C68 0.031(2) 0.029(3) 0.039(3) 0.001(2) 0.003(2) -0.011(2) C69 0.039(3) 0.045(3) 0.032(3) 0.001(2) -0.007(2) -0.016(2) C70 0.044(3) 0.043(3) 0.022(2) 0.003(2) -0.007(2) -0.017(2) C71 0.034(2) 0.028(2) 0.023(2) -0.0010(19) 0.0037(18) -0.010(2) C72 0.020(2) 0.023(2) 0.030(2) 0.0057(18) 0.0057(17) -0.0019(16) C73 0.041(3) 0.043(3) 0.040(3) 0.015(2) 0.021(2) 0.008(2) C74 0.038(3) 0.022(2) 0.067(4) 0.003(2) 0.008(3) -0.009(2) C75 0.043(3) 0.037(3) 0.021(2) 0.003(2) -0.002(2) -0.021(2) C76 0.061(3) 0.033(3) 0.029(3) 0.000(2) 0.017(2) -0.005(2) C77 0.031(3) 0.046(3) 0.049(3) 0.012(3) 0.006(2) -0.006(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 N2 2.443(3) . ? Sm1 N1 2.452(3) . ? Sm1 N3 2.453(3) . ? Sm1 N4 2.453(3) . ? Sm1 N5 2.463(3) . ? Sm1 N6 2.464(3) . ? Sm1 C53 2.814(4) . ? Sm1 C28 2.831(4) . ? Sm1 C1 2.847(4) . ? N1 C1 1.329(5) . ? N1 C2 1.434(5) . ? N2 C1 1.340(6) . ? N2 C11 1.432(5) . ? N3 C28 1.321(5) . ? N3 C29 1.427(5) . ? N4 C28 1.318(5) . ? N4 C41 1.434(5) . ? N5 C53 1.317(5) . ? N5 C54 1.431(5) . ? N6 C53 1.327(5) . ? N6 C66 1.426(5) . ? C1 C20 1.444(6) . ? C2 C3 1.394(6) . ? C2 C7 1.401(6) . ? C3 C4 1.393(6) . ? C3 C8 1.504(6) . ? C4 C5 1.391(6) . ? C5 C6 1.379(7) . ? C5 C9 1.510(6) . ? C6 C7 1.395(6) . ? C7 C10 1.493(6) . ? C11 C16 1.391(7) . ? C11 C12 1.402(6) . ? C12 C13 1.404(7) . ? C12 C17 1.494(8) . ? C13 C14 1.379(9) . ? C14 C15 1.381(8) . ? C14 C18 1.512(7) . ? C15 C16 1.392(6) . ? C16 C19 1.502(7) . ? C20 C21 1.194(6) . ? C21 C22 1.430(6) . ? C22 C23 1.389(6) . ? C22 C27 1.393(6) . ? C23 C24 1.377(7) . ? C24 C25 1.374(8) . ? C25 C26 1.378(8) . ? C26 C27 1.382(6) . ? C29 C30 1.411(6) . ? C29 C34 1.411(5) . ? C30 C31 1.392(6) . ? C30 C35 1.526(5) . ? C31 C32 1.378(6) . ? C32 C33 1.375(6) . ? C33 C34 1.385(6) . ? C34 C38 1.517(6) . ? C35 C36 1.526(6) . ? C35 C37 1.527(6) . ? C38 C40 1.502(7) . ? C38 C39 1.523(7) . ? C41 C46 1.406(5) . ? C41 C42 1.408(6) . ? C42 C43 1.386(6) . ? C42 C47 1.511(6) . ? C43 C44 1.385(6) . ? C44 C45 1.381(6) . ? C45 C46 1.394(6) . ? C46 C50 1.523(6) . ? C47 C48 1.520(8) . ? C47 C49 1.526(6) . ? C50 C51 1.527(6) . ? C50 C52 1.533(6) . ? C54 C55 1.398(6) . ? C54 C59 1.412(6) . ? C55 C56 1.394(5) . ? C55 C60 1.515(6) . ? C56 C57 1.373(6) . ? C57 C58 1.379(6) . ? C58 C59 1.392(6) . ? C59 C63 1.522(6) . ? C60 C62 1.528(6) . ? C60 C61 1.536(6) . ? C63 C65 1.530(7) . ? C63 C64 1.533(8) . ? C66 C67 1.408(6) . ? C66 C71 1.415(6) . ? C67 C68 1.391(6) . ? C67 C72 1.521(6) . ? C68 C69 1.373(7) . ? C69 C70 1.379(7) . ? C70 C71 1.386(6) . ? C71 C75 1.514(6) . ? C72 C74 1.516(6) . ? C72 C73 1.522(6) . ? C75 C77 1.527(7) . ? C75 C76 1.529(7) . ? C80 C79 1.349(7) . ? C80 C81 1.401(6) 3_565 ? C79 C81 1.420(8) . ? C81 C80 1.401(6) 3_565 ? C87 C86 1.393(7) 3_665 ? C87 C85 1.413(8) . ? C85 C86 1.407(8) . ? C86 C87 1.393(7) 3_665 ? 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 55.84(12) . . ? N2 Sm1 N3 98.92(11) . . ? N1 Sm1 N3 140.77(11) . . ? N2 Sm1 N4 109.78(12) . . ? N1 Sm1 N4 101.60(12) . . ? N3 Sm1 N4 55.51(11) . . ? N2 Sm1 N5 143.97(11) . . ? N1 Sm1 N5 101.60(11) . . ? N3 Sm1 N5 113.41(11) . . ? N4 Sm1 N5 101.73(11) . . ? N2 Sm1 N6 102.91(12) . . ? N1 Sm1 N6 111.45(11) . . ? N3 Sm1 N6 102.79(11) . . ? N4 Sm1 N6 142.75(11) . . ? N5 Sm1 N6 55.98(11) . . ? N2 Sm1 C53 124.94(12) . . ? N1 Sm1 C53 107.31(11) . . ? N3 Sm1 C53 111.91(11) . . ? N4 Sm1 C53 125.27(11) . . ? N5 Sm1 C53 27.91(11) . . ? N6 Sm1 C53 28.13(11) . . ? N2 Sm1 C28 105.90(11) . . ? N1 Sm1 C28 123.22(11) . . ? N3 Sm1 C28 27.80(11) . . ? N4 Sm1 C28 27.72(11) . . ? N5 Sm1 C28 110.11(11) . . ? N6 Sm1 C28 125.31(11) . . ? C53 Sm1 C28 122.78(11) . . ? N2 Sm1 C1 28.04(12) . . ? N1 Sm1 C1 27.80(12) . . ? N3 Sm1 C1 121.83(11) . . ? N4 Sm1 C1 107.74(12) . . ? N5 Sm1 C1 124.75(11) . . ? N6 Sm1 C1 109.50(12) . . ? C53 Sm1 C1 119.47(11) . . ? C28 Sm1 C1 117.75(11) . . ? C1 N1 C2 115.4(3) . . ? C1 N1 Sm1 92.9(3) . . ? C2 N1 Sm1 151.4(3) . . ? C1 N2 C11 116.2(4) . . ? C1 N2 Sm1 92.9(2) . . ? C11 N2 Sm1 150.7(3) . . ? C28 N3 C29 117.5(3) . . ? C28 N3 Sm1 92.2(2) . . ? C29 N3 Sm1 150.2(3) . . ? C28 N4 C41 116.6(3) . . ? C28 N4 Sm1 92.3(2) . . ? C41 N4 Sm1 150.9(2) . . ? C53 N5 C54 115.3(3) . . ? C53 N5 Sm1 91.0(2) . . ? C54 N5 Sm1 153.4(3) . . ? C53 N6 C66 113.5(3) . . ? C53 N6 Sm1 90.8(2) . . ? C66 N6 Sm1 155.3(3) . . ? N1 C1 N2 118.4(4) . . ? N1 C1 C20 120.3(4) . . ? N2 C1 C20 121.4(4) . . ? N1 C1 Sm1 59.4(2) . . ? N2 C1 Sm1 59.0(2) . . ? C20 C1 Sm1 179.1(3) . . ? C3 C2 C7 120.3(4) . . ? C3 C2 N1 118.9(4) . . ? C7 C2 N1 120.7(4) . . ? C4 C3 C2 119.4(4) . . ? C4 C3 C8 120.2(4) . . ? C2 C3 C8 120.4(4) . . ? C5 C4 C3 121.3(4) . . ? C6 C5 C4 118.2(4) . . ? C6 C5 C9 121.1(4) . . ? C4 C5 C9 120.7(4) . . ? C5 C6 C7 122.4(4) . . ? C6 C7 C2 118.4(4) . . ? C6 C7 C10 120.6(4) . . ? C2 C7 C10 121.0(4) . . ? C16 C11 C12 120.8(4) . . ? C16 C11 N2 118.5(4) . . ? C12 C11 N2 120.8(5) . . ? C11 C12 C13 117.3(5) . . ? C11 C12 C17 122.1(4) . . ? C13 C12 C17 120.5(5) . . ? C14 C13 C12 122.9(5) . . ? C13 C14 C15 117.8(5) . . ? C13 C14 C18 121.4(6) . . ? C15 C14 C18 120.7(6) . . ? C14 C15 C16 121.8(5) . . ? C11 C16 C15 119.1(5) . . ? C11 C16 C19 120.8(4) . . ? C15 C16 C19 120.1(5) . . ? C21 C20 C1 176.4(5) . . ? C20 C21 C22 179.0(6) . . ? C23 C22 C27 119.7(4) . . ? C23 C22 C21 120.4(4) . . ? C27 C22 C21 119.8(4) . . ? C24 C23 C22 119.9(5) . . ? C25 C24 C23 120.3(5) . . ? C24 C25 C26 120.2(4) . . ? C25 C26 C27 120.3(5) . . ? C26 C27 C22 119.5(5) . . ? N4 C28 N3 120.0(3) . . ? N4 C28 Sm1 60.0(2) . . ? N3 C28 Sm1 60.0(2) . . ? C30 C29 C34 119.3(4) . . ? C30 C29 N3 120.9(3) . . ? C34 C29 N3 119.8(4) . . ? C31 C30 C29 119.1(4) . . ? C31 C30 C35 117.6(4) . . ? C29 C30 C35 123.2(4) . . ? C32 C31 C30 121.3(4) . . ? C33 C32 C31 119.4(4) . . ? C32 C33 C34 121.7(4) . . ? C33 C34 C29 119.1(4) . . ? C33 C34 C38 119.4(4) . . ? C29 C34 C38 121.4(4) . . ? C36 C35 C30 112.4(4) . . ? C36 C35 C37 110.5(4) . . ? C30 C35 C37 110.2(3) . . ? C40 C38 C34 109.2(4) . . ? C40 C38 C39 110.4(4) . . ? C34 C38 C39 113.2(4) . . ? C46 C41 C42 120.5(4) . . ? C46 C41 N4 120.9(4) . . ? C42 C41 N4 118.5(3) . . ? C43 C42 C41 118.7(4) . . ? C43 C42 C47 119.9(4) . . ? C41 C42 C47 121.1(4) . . ? C44 C43 C42 121.5(4) . . ? C45 C44 C43 119.2(4) . . ? C44 C45 C46 121.6(4) . . ? C45 C46 C41 118.4(4) . . ? C45 C46 C50 118.5(4) . . ? C41 C46 C50 123.1(4) . . ? C42 C47 C48 108.9(4) . . ? C42 C47 C49 114.6(4) . . ? C48 C47 C49 109.9(4) . . ? C46 C50 C51 111.1(4) . . ? C46 C50 C52 111.3(4) . . ? C51 C50 C52 109.6(4) . . ? N5 C53 N6 122.0(4) . . ? N5 C53 Sm1 61.1(2) . . ? N6 C53 Sm1 61.1(2) . . ? C55 C54 C59 120.2(4) . . ? C55 C54 N5 119.1(3) . . ? C59 C54 N5 120.6(4) . . ? C56 C55 C54 118.8(4) . . ? C56 C55 C60 118.1(4) . . ? C54 C55 C60 123.1(3) . . ? C57 C56 C55 121.7(4) . . ? C56 C57 C58 119.3(4) . . ? C57 C58 C59 121.6(4) . . ? C58 C59 C54 118.5(4) . . ? C58 C59 C63 118.2(4) . . ? C54 C59 C63 123.3(4) . . ? C55 C60 C62 110.5(4) . . ? C55 C60 C61 112.4(3) . . ? C62 C60 C61 109.7(4) . . ? C59 C63 C65 112.8(4) . . ? C59 C63 C64 110.5(4) . . ? C65 C63 C64 107.3(4) . . ? C67 C66 C71 119.9(4) . . ? C67 C66 N6 120.8(4) . . ? C71 C66 N6 119.3(4) . . ? C68 C67 C66 118.9(4) . . ? C68 C67 C72 119.7(4) . . ? C66 C67 C72 121.4(4) . . ? C69 C68 C67 121.4(4) . . ? C68 C69 C70 119.5(5) . . ? C69 C70 C71 121.8(5) . . ? C70 C71 C66 118.4(4) . . ? C70 C71 C75 119.3(4) . . ? C66 C71 C75 122.2(4) . . ? C74 C72 C67 111.9(4) . . ? C74 C72 C73 109.6(4) . . ? C67 C72 C73 111.8(4) . . ? C71 C75 C77 110.0(4) . . ? C71 C75 C76 112.2(4) . . ? C77 C75 C76 111.1(4) . . ? C79 C80 C81 120.4(7) . 3_565 ? C80 C79 C81 123.4(7) . . ? C80 C81 C79 116.0(7) 3_565 . ? C86 C87 C85 118.0(9) 3_665 . ? C86 C85 C87 118.3(8) . . ? C87 C86 C85 122.1(9) 3_665 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.469 _refine_diff_density_min -4.103 _refine_diff_density_rms 0.098