# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' #TrackingRef 'sg3325.cif' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry University of Ottawa Ottawa, Ontario k1n 6n5 Canada ; _publ_contact_author_name 'Sandro Gambarotta' _publ_contact_author_email sandro.gambarotta@uottawa.ca _publ_section_title ; samarium complexes of a sigma-/pi-pyrrolide/arene based macrocyclic ligand. ; loop_ _publ_author_name 'Sandro Gambarotta' 'Sougandi Ilango' 'Balamurugan Vidjayacoumar' data_sg3303 _database_code_depnum_ccdc_archive 'CCDC 763508' #TrackingRef '329_web_deposit_cif_file_0_BVidjayacoumar_1264555817.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 Cl N2 Sm' _chemical_formula_weight 634.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 19.09(3) _cell_length_b 14.994(11) _cell_length_c 10.206(11) _cell_angle_alpha 90.00 _cell_angle_beta 109.89(13) _cell_angle_gamma 90.00 _cell_volume 2747(6) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 191 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 24.73 _exptl_crystal_description plate _exptl_crystal_colour reddish-orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 2.258 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6609 _exptl_absorpt_correction_T_max 0.8057 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 9947 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 24.77 _reflns_number_total 2307 _reflns_number_gt 2105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2000)' _computing_cell_refinement 'SMART, Bruker (2000)' _computing_data_reduction 'XPREP, Bruker (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2000)' _computing_publication_material 'SHELXTL, Bruker (2000)' _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^)+(0.0469P)^2^]' _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 2307 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 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 0.5000 0.788826(18) 0.7500 0.02316(12) Uani 1 2 d S . . Cl1 Cl 0.5000 0.96345(11) 0.7500 0.0685(7) Uani 1 2 d S . . N1 N 0.61009(18) 0.7093(2) 0.7521(3) 0.0261(7) Uani 1 1 d . . . C1 C 0.6076(2) 0.7657(3) 0.5159(4) 0.0300(9) Uani 1 1 d . . . C2 C 0.6181(3) 0.7229(3) 0.3871(5) 0.0403(11) Uani 1 1 d . . . H2A H 0.5911 0.6669 0.3665 0.060 Uiso 1 1 calc R . . H2B H 0.6706 0.7120 0.4054 0.060 Uiso 1 1 calc R . . H2C H 0.5991 0.7628 0.3081 0.060 Uiso 1 1 calc R . . C3 C 0.6482(2) 0.8559(3) 0.5420(5) 0.0409(11) Uani 1 1 d . . . H3A H 0.6418 0.8845 0.6223 0.061 Uiso 1 1 calc R . . H3B H 0.6277 0.8937 0.4608 0.061 Uiso 1 1 calc R . . H3C H 0.7009 0.8464 0.5592 0.061 Uiso 1 1 calc R . . C4 C 0.6393(2) 0.7060(3) 0.6442(4) 0.0277(9) Uani 1 1 d . . . C5 C 0.6968(2) 0.6468(3) 0.6744(4) 0.0316(9) Uani 1 1 d . . . H5A H 0.7254 0.6330 0.6182 0.038 Uiso 1 1 calc R . . C6 C 0.7050(2) 0.6098(3) 0.8068(4) 0.0313(9) Uani 1 1 d . . . H6A H 0.7399 0.5664 0.8545 0.038 Uiso 1 1 calc R . . C7 C 0.6527(2) 0.6491(3) 0.8521(4) 0.0245(8) Uani 1 1 d . . . C8 C 0.6344(2) 0.6276(3) 0.9828(4) 0.0277(9) Uani 1 1 d . . . C9 C 0.7070(2) 0.6142(3) 1.1091(4) 0.0397(11) Uani 1 1 d . . . H9A H 0.7366 0.6683 1.1246 0.060 Uiso 1 1 calc R . . H9B H 0.7353 0.5652 1.0902 0.060 Uiso 1 1 calc R . . H9C H 0.6945 0.6008 1.1915 0.060 Uiso 1 1 calc R . . C10 C 0.5901(2) 0.5400(3) 0.9608(5) 0.0389(10) Uani 1 1 d . . . H10A H 0.5444 0.5463 0.8820 0.058 Uiso 1 1 calc R . . H10B H 0.5784 0.5262 1.0438 0.058 Uiso 1 1 calc R . . H10C H 0.6197 0.4921 0.9425 0.058 Uiso 1 1 calc R . . C11 C 0.5911(2) 0.7062(3) 1.0108(4) 0.0245(9) Uani 1 1 d . . . C12 C 0.5175(2) 0.6991(3) 1.0050(4) 0.0263(9) Uani 1 1 d . . . H12A H 0.4951 0.6393 1.0030 0.032 Uiso 1 1 calc R . . C13 C 0.4753(2) 0.7773(3) 1.0125(4) 0.0278(9) Uani 1 1 d . . . C14 C 0.5115(2) 0.8579(3) 1.0381(4) 0.0311(9) Uani 1 1 d . . . H14A H 0.4840 0.9123 1.0463 0.037 Uiso 1 1 calc R . . C15 C 0.5869(2) 0.8643(3) 1.0489(4) 0.0344(10) Uani 1 1 d . . . H15A H 0.6110 0.9199 1.0676 0.041 Uiso 1 1 calc R . . C16 C 0.6253(2) 0.7909(3) 1.0326(4) 0.0301(9) Uani 1 1 d . . . H16A H 0.6749 0.7967 1.0360 0.036 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 0.02743(18) 0.02364(18) 0.01845(17) 0.000 0.00785(11) 0.000 Cl1 0.146(2) 0.0253(9) 0.0327(9) 0.000 0.0286(11) 0.000 N1 0.0263(17) 0.0297(18) 0.0216(17) 0.0012(13) 0.0075(13) 0.0028(14) C1 0.033(2) 0.037(3) 0.024(2) 0.0028(17) 0.0144(17) 0.0039(18) C2 0.038(3) 0.058(3) 0.027(2) 0.003(2) 0.0139(19) 0.010(2) C3 0.034(2) 0.046(3) 0.041(3) 0.009(2) 0.011(2) -0.001(2) C4 0.027(2) 0.033(2) 0.022(2) -0.0020(16) 0.0072(16) -0.0025(18) C5 0.031(2) 0.039(2) 0.027(2) -0.0078(17) 0.0128(17) -0.0026(19) C6 0.028(2) 0.033(2) 0.031(2) 0.0042(17) 0.0080(17) 0.0032(18) C7 0.0208(19) 0.027(2) 0.0223(19) 0.0015(16) 0.0033(15) -0.0013(16) C8 0.024(2) 0.032(2) 0.025(2) 0.0048(17) 0.0049(16) -0.0006(17) C9 0.034(2) 0.053(3) 0.029(2) 0.010(2) 0.0065(19) 0.007(2) C10 0.037(2) 0.030(2) 0.051(3) 0.008(2) 0.016(2) 0.0002(19) C11 0.025(2) 0.035(2) 0.0114(17) 0.0038(15) 0.0034(14) -0.0021(17) C12 0.033(2) 0.029(2) 0.0163(19) 0.0027(15) 0.0074(16) -0.0037(17) C13 0.036(2) 0.035(2) 0.0149(18) 0.0001(16) 0.0111(16) 0.0031(18) C14 0.041(2) 0.034(2) 0.0192(19) -0.0061(17) 0.0111(17) 0.000(2) C15 0.043(3) 0.036(2) 0.024(2) -0.0088(18) 0.0119(18) -0.011(2) C16 0.032(2) 0.040(2) 0.0161(19) -0.0060(17) 0.0060(16) -0.0099(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N1 2.410(5) . ? Sm1 N1 2.410(5) 2_656 ? Sm1 Cl1 2.618(3) . ? Sm1 C12 2.847(5) 2_656 ? Sm1 C12 2.847(5) . ? Sm1 C13 2.879(5) 2_656 ? Sm1 C13 2.879(5) . ? Sm1 C11 2.915(5) 2_656 ? Sm1 C11 2.915(5) . ? Sm1 C14 3.054(5) 2_656 ? Sm1 C14 3.054(5) . ? Sm1 C16 3.057(7) 2_656 ? N1 C4 1.394(5) . ? N1 C7 1.398(5) . ? C1 C13 1.519(7) 2_656 ? C1 C4 1.530(6) . ? C1 C2 1.536(6) . ? C1 C3 1.536(6) . ? C4 C5 1.363(6) . ? C5 C6 1.419(6) . ? C6 C7 1.368(6) . ? C7 C8 1.524(6) . ? C8 C11 1.521(6) . ? C8 C10 1.537(6) . ? C8 C9 1.551(6) . ? C11 C12 1.390(6) . ? C11 C16 1.410(5) . ? C12 C13 1.439(6) . ? C13 C14 1.373(6) . ? C13 C1 1.519(7) 2_656 ? C14 C15 1.408(7) . ? C15 C16 1.364(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 N1 Sm1 N1 120.70(18) . 2_656 ? N1 Sm1 Cl1 119.65(9) . . ? N1 Sm1 Cl1 119.65(9) 2_656 . ? N1 Sm1 C12 66.75(16) . 2_656 ? N1 Sm1 C12 85.83(15) 2_656 2_656 ? Cl1 Sm1 C12 118.20(9) . 2_656 ? N1 Sm1 C12 85.83(15) . . ? N1 Sm1 C12 66.75(16) 2_656 . ? Cl1 Sm1 C12 118.20(9) . . ? C12 Sm1 C12 123.60(17) 2_656 . ? N1 Sm1 C13 63.90(15) . 2_656 ? N1 Sm1 C13 112.36(15) 2_656 2_656 ? Cl1 Sm1 C13 93.45(8) . 2_656 ? C12 Sm1 C13 29.11(12) 2_656 2_656 ? C12 Sm1 C13 144.77(12) . 2_656 ? N1 Sm1 C13 112.36(15) . . ? N1 Sm1 C13 63.90(15) 2_656 . ? Cl1 Sm1 C13 93.45(8) . . ? C12 Sm1 C13 144.77(12) 2_656 . ? C12 Sm1 C13 29.11(12) . . ? C13 Sm1 C13 173.10(16) 2_656 . ? N1 Sm1 C11 92.61(16) . 2_656 ? N1 Sm1 C11 62.20(14) 2_656 2_656 ? Cl1 Sm1 C11 115.17(9) . 2_656 ? C12 Sm1 C11 27.90(13) 2_656 2_656 ? C12 Sm1 C11 118.80(14) . 2_656 ? C13 Sm1 C11 50.26(14) 2_656 2_656 ? C13 Sm1 C11 126.02(14) . 2_656 ? N1 Sm1 C11 62.21(14) . . ? N1 Sm1 C11 92.61(16) 2_656 . ? Cl1 Sm1 C11 115.17(9) . . ? C12 Sm1 C11 118.80(14) 2_656 . ? C12 Sm1 C11 27.90(13) . . ? C13 Sm1 C11 126.03(14) 2_656 . ? C13 Sm1 C11 50.26(14) . . ? C11 Sm1 C11 129.66(17) 2_656 . ? N1 Sm1 C14 87.32(15) . 2_656 ? N1 Sm1 C14 112.46(16) 2_656 2_656 ? Cl1 Sm1 C14 70.19(9) . 2_656 ? C12 Sm1 C14 48.11(13) 2_656 2_656 ? C12 Sm1 C14 171.16(12) . 2_656 ? C13 Sm1 C14 26.55(11) 2_656 2_656 ? C13 Sm1 C14 159.28(12) . 2_656 ? C11 Sm1 C14 55.93(14) 2_656 2_656 ? C11 Sm1 C14 148.05(13) . 2_656 ? N1 Sm1 C14 112.46(16) . . ? N1 Sm1 C14 87.32(15) 2_656 . ? Cl1 Sm1 C14 70.18(9) . . ? C12 Sm1 C14 171.16(12) 2_656 . ? C12 Sm1 C14 48.11(13) . . ? C13 Sm1 C14 159.28(12) 2_656 . ? C13 Sm1 C14 26.55(11) . . ? C11 Sm1 C14 148.05(13) 2_656 . ? C11 Sm1 C14 55.93(14) . . ? C14 Sm1 C14 140.37(17) 2_656 . ? N1 Sm1 C16 114.41(15) . 2_656 ? N1 Sm1 C16 66.21(15) 2_656 2_656 ? Cl1 Sm1 C16 89.43(8) . 2_656 ? C12 Sm1 C16 48.03(13) 2_656 2_656 ? C12 Sm1 C16 132.70(14) . 2_656 ? C13 Sm1 C16 56.36(16) 2_656 2_656 ? C13 Sm1 C16 123.73(16) . 2_656 ? C11 Sm1 C16 27.18(11) 2_656 2_656 ? C11 Sm1 C16 153.90(12) . 2_656 ? C14 Sm1 C16 46.46(14) 2_656 2_656 ? C14 Sm1 C16 133.01(14) . 2_656 ? C4 N1 C7 105.3(3) . . ? C4 N1 Sm1 126.3(3) . . ? C7 N1 Sm1 128.0(3) . . ? C13 C1 C4 108.3(3) 2_656 . ? C13 C1 C2 108.3(4) 2_656 . ? C4 C1 C2 111.1(4) . . ? C13 C1 C3 111.4(4) 2_656 . ? C4 C1 C3 109.7(4) . . ? C2 C1 C3 108.1(4) . . ? C5 C4 N1 110.6(4) . . ? C5 C4 C1 128.9(4) . . ? N1 C4 C1 120.4(4) . . ? C4 C5 C6 106.9(4) . . ? C7 C6 C5 107.2(4) . . ? C6 C7 N1 110.0(4) . . ? C6 C7 C8 128.0(4) . . ? N1 C7 C8 121.7(3) . . ? C11 C8 C7 107.6(3) . . ? C11 C8 C10 112.5(3) . . ? C7 C8 C10 109.3(3) . . ? C11 C8 C9 109.5(3) . . ? C7 C8 C9 110.4(3) . . ? C10 C8 C9 107.6(3) . . ? C12 C11 C16 118.8(4) . . ? C12 C11 C8 122.7(4) . . ? C16 C11 C8 118.4(4) . . ? C12 C11 Sm1 73.3(2) . . ? C16 C11 Sm1 82.1(2) . . ? C8 C11 Sm1 110.6(2) . . ? C11 C12 C13 120.8(4) . . ? C11 C12 Sm1 78.8(2) . . ? C13 C12 Sm1 76.7(2) . . ? C14 C13 C12 118.1(4) . . ? C14 C13 C1 124.2(4) . 2_656 ? C12 C13 C1 117.6(4) . 2_656 ? C14 C13 Sm1 83.8(2) . . ? C12 C13 Sm1 74.2(2) . . ? C1 C13 Sm1 108.6(3) 2_656 . ? C13 C14 C15 120.7(4) . . ? C13 C14 Sm1 69.6(2) . . ? C15 C14 Sm1 80.6(3) . . ? C16 C15 C14 120.8(4) . . ? C15 C16 C11 120.5(4) . . ? C15 C16 Sm1 81.0(3) . . ? C11 C16 Sm1 70.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Sm1 N1 C4 111.6(3) 2_656 . . . ? Cl1 Sm1 N1 C4 -68.4(3) . . . . ? C12 Sm1 N1 C4 42.0(3) 2_656 . . . ? C12 Sm1 N1 C4 171.4(3) . . . . ? C13 Sm1 N1 C4 10.0(3) 2_656 . . . ? C13 Sm1 N1 C4 -176.4(3) . . . . ? C11 Sm1 N1 C4 52.7(3) 2_656 . . . ? C11 Sm1 N1 C4 -173.0(3) . . . . ? C14 Sm1 N1 C4 -3.0(3) 2_656 . . . ? C14 Sm1 N1 C4 -147.6(3) . . . . ? C16 Sm1 N1 C4 35.9(3) 2_656 . . . ? N1 Sm1 N1 C7 -60.1(3) 2_656 . . . ? Cl1 Sm1 N1 C7 119.9(3) . . . . ? C12 Sm1 N1 C7 -129.8(3) 2_656 . . . ? C12 Sm1 N1 C7 -0.3(3) . . . . ? C13 Sm1 N1 C7 -161.7(3) 2_656 . . . ? C13 Sm1 N1 C7 11.9(3) . . . . ? C11 Sm1 N1 C7 -119.0(3) 2_656 . . . ? C11 Sm1 N1 C7 15.3(3) . . . . ? C14 Sm1 N1 C7 -174.7(3) 2_656 . . . ? C14 Sm1 N1 C7 40.7(3) . . . . ? C16 Sm1 N1 C7 -135.9(3) 2_656 . . . ? C7 N1 C4 C5 0.3(4) . . . . ? Sm1 N1 C4 C5 -172.9(3) . . . . ? C7 N1 C4 C1 -178.5(3) . . . . ? Sm1 N1 C4 C1 8.3(5) . . . . ? C13 C1 C4 C5 148.0(4) 2_656 . . . ? C2 C1 C4 C5 29.2(6) . . . . ? C3 C1 C4 C5 -90.2(5) . . . . ? C13 C1 C4 N1 -33.4(5) 2_656 . . . ? C2 C1 C4 N1 -152.3(4) . . . . ? C3 C1 C4 N1 88.3(5) . . . . ? N1 C4 C5 C6 0.2(5) . . . . ? C1 C4 C5 C6 178.9(4) . . . . ? C4 C5 C6 C7 -0.7(5) . . . . ? C5 C6 C7 N1 0.9(5) . . . . ? C5 C6 C7 C8 174.9(4) . . . . ? C4 N1 C7 C6 -0.8(4) . . . . ? Sm1 N1 C7 C6 172.3(3) . . . . ? C4 N1 C7 C8 -175.2(3) . . . . ? Sm1 N1 C7 C8 -2.1(5) . . . . ? C6 C7 C8 C11 162.6(4) . . . . ? N1 C7 C8 C11 -24.0(5) . . . . ? C6 C7 C8 C10 -75.0(5) . . . . ? N1 C7 C8 C10 98.4(4) . . . . ? C6 C7 C8 C9 43.2(6) . . . . ? N1 C7 C8 C9 -143.4(4) . . . . ? C7 C8 C11 C12 115.5(4) . . . . ? C10 C8 C11 C12 -4.9(5) . . . . ? C9 C8 C11 C12 -124.5(4) . . . . ? C7 C8 C11 C16 -59.5(4) . . . . ? C10 C8 C11 C16 -179.9(3) . . . . ? C9 C8 C11 C16 60.6(5) . . . . ? C7 C8 C11 Sm1 32.6(3) . . . . ? C10 C8 C11 Sm1 -87.9(3) . . . . ? C9 C8 C11 Sm1 152.6(3) . . . . ? N1 Sm1 C11 C12 -145.1(3) . . . . ? N1 Sm1 C11 C12 -21.4(2) 2_656 . . . ? Cl1 Sm1 C11 C12 103.2(2) . . . . ? C12 Sm1 C11 C12 -108.1(3) 2_656 . . . ? C13 Sm1 C11 C12 -141.7(2) 2_656 . . . ? C13 Sm1 C11 C12 30.9(2) . . . . ? C11 Sm1 C11 C12 -76.8(2) 2_656 . . . ? C14 Sm1 C11 C12 -164.2(2) 2_656 . . . ? C14 Sm1 C11 C12 63.5(2) . . . . ? C16 Sm1 C11 C12 -55.9(4) 2_656 . . . ? N1 Sm1 C11 C16 91.6(3) . . . . ? N1 Sm1 C11 C16 -144.8(2) 2_656 . . . ? Cl1 Sm1 C11 C16 -20.1(3) . . . . ? C12 Sm1 C11 C16 128.6(3) 2_656 . . . ? C12 Sm1 C11 C16 -123.3(4) . . . . ? C13 Sm1 C11 C16 95.0(3) 2_656 . . . ? C13 Sm1 C11 C16 -92.4(3) . . . . ? C11 Sm1 C11 C16 159.9(3) 2_656 . . . ? C14 Sm1 C11 C16 72.5(3) 2_656 . . . ? C14 Sm1 C11 C16 -59.8(3) . . . . ? C16 Sm1 C11 C16 -179.19(11) 2_656 . . . ? N1 Sm1 C11 C8 -25.8(2) . . . . ? N1 Sm1 C11 C8 97.8(3) 2_656 . . . ? Cl1 Sm1 C11 C8 -137.5(2) . . . . ? C12 Sm1 C11 C8 11.2(3) 2_656 . . . ? C12 Sm1 C11 C8 119.3(4) . . . . ? C13 Sm1 C11 C8 -22.4(3) 2_656 . . . ? C13 Sm1 C11 C8 150.2(3) . . . . ? C11 Sm1 C11 C8 42.5(2) 2_656 . . . ? C14 Sm1 C11 C8 -44.9(4) 2_656 . . . ? C14 Sm1 C11 C8 -177.2(3) . . . . ? C16 Sm1 C11 C8 63.4(4) 2_656 . . . ? C16 C11 C12 C13 3.9(5) . . . . ? C8 C11 C12 C13 -171.1(3) . . . . ? Sm1 C11 C12 C13 -66.9(3) . . . . ? C16 C11 C12 Sm1 70.8(3) . . . . ? C8 C11 C12 Sm1 -104.1(3) . . . . ? N1 Sm1 C12 C11 30.5(2) . . . . ? N1 Sm1 C12 C11 156.6(3) 2_656 . . . ? Cl1 Sm1 C12 C11 -91.1(2) . . . . ? C12 Sm1 C12 C11 88.9(2) 2_656 . . . ? C13 Sm1 C12 C11 60.3(3) 2_656 . . . ? C13 Sm1 C12 C11 -125.7(4) . . . . ? C11 Sm1 C12 C11 121.2(3) 2_656 . . . ? C14 Sm1 C12 C11 69.9(8) 2_656 . . . ? C14 Sm1 C12 C11 -94.9(3) . . . . ? C16 Sm1 C12 C11 150.3(2) 2_656 . . . ? N1 Sm1 C12 C13 156.2(2) . . . . ? N1 Sm1 C12 C13 -77.7(3) 2_656 . . . ? Cl1 Sm1 C12 C13 34.6(3) . . . . ? C12 Sm1 C12 C13 -145.4(3) 2_656 . . . ? C13 Sm1 C12 C13 -174.00(15) 2_656 . . . ? C11 Sm1 C12 C13 -113.1(3) 2_656 . . . ? C11 Sm1 C12 C13 125.7(4) . . . . ? C14 Sm1 C12 C13 -164.4(6) 2_656 . . . ? C14 Sm1 C12 C13 30.8(2) . . . . ? C16 Sm1 C12 C13 -84.0(3) 2_656 . . . ? C11 C12 C13 C14 -5.8(5) . . . . ? Sm1 C12 C13 C14 -73.9(3) . . . . ? C11 C12 C13 C1 171.1(3) . . . 2_656 ? Sm1 C12 C13 C1 103.1(3) . . . 2_656 ? C11 C12 C13 Sm1 68.0(3) . . . . ? N1 Sm1 C13 C14 95.8(3) . . . . ? N1 Sm1 C13 C14 -149.8(3) 2_656 . . . ? Cl1 Sm1 C13 C14 -28.3(2) . . . . ? C12 Sm1 C13 C14 176.7(2) 2_656 . . . ? C12 Sm1 C13 C14 121.6(4) . . . . ? C13 Sm1 C13 C14 151.7(2) 2_656 . . . ? C11 Sm1 C13 C14 -153.1(2) 2_656 . . . ? C11 Sm1 C13 C14 92.0(3) . . . . ? C14 Sm1 C13 C14 -65.1(5) 2_656 . . . ? C16 Sm1 C13 C14 -119.9(3) 2_656 . . . ? N1 Sm1 C13 C12 -25.8(3) . . . . ? N1 Sm1 C13 C12 88.6(3) 2_656 . . . ? Cl1 Sm1 C13 C12 -149.9(2) . . . . ? C12 Sm1 C13 C12 55.2(4) 2_656 . . . ? C13 Sm1 C13 C12 30.1(2) 2_656 . . . ? C11 Sm1 C13 C12 85.3(3) 2_656 . . . ? C11 Sm1 C13 C12 -29.6(2) . . . . ? C14 Sm1 C13 C12 173.3(3) 2_656 . . . ? C14 Sm1 C13 C12 -121.6(4) . . . . ? C16 Sm1 C13 C12 118.5(2) 2_656 . . . ? N1 Sm1 C13 C1 -140.1(3) . . . 2_656 ? N1 Sm1 C13 C1 -25.7(2) 2_656 . . 2_656 ? Cl1 Sm1 C13 C1 95.8(3) . . . 2_656 ? C12 Sm1 C13 C1 -59.2(4) 2_656 . . 2_656 ? C12 Sm1 C13 C1 -114.4(4) . . . 2_656 ? C13 Sm1 C13 C1 -84.2(3) 2_656 . . 2_656 ? C11 Sm1 C13 C1 -29.0(3) 2_656 . . 2_656 ? C11 Sm1 C13 C1 -144.0(3) . . . 2_656 ? C14 Sm1 C13 C1 58.9(5) 2_656 . . 2_656 ? C14 Sm1 C13 C1 124.1(4) . . . 2_656 ? C16 Sm1 C13 C1 4.1(3) 2_656 . . 2_656 ? C12 C13 C14 C15 3.5(6) . . . . ? C1 C13 C14 C15 -173.2(4) 2_656 . . . ? Sm1 C13 C14 C15 -64.9(4) . . . . ? C12 C13 C14 Sm1 68.4(3) . . . . ? C1 C13 C14 Sm1 -108.3(4) 2_656 . . . ? N1 Sm1 C14 C13 -95.4(3) . . . . ? N1 Sm1 C14 C13 26.9(3) 2_656 . . . ? Cl1 Sm1 C14 C13 149.8(3) . . . . ? C12 Sm1 C14 C13 -12.4(8) 2_656 . . . ? C12 Sm1 C14 C13 -33.8(3) . . . . ? C13 Sm1 C14 C13 -170.7(2) 2_656 . . . ? C11 Sm1 C14 C13 43.7(4) 2_656 . . . ? C11 Sm1 C14 C13 -68.1(3) . . . . ? C14 Sm1 C14 C13 149.8(3) 2_656 . . . ? C16 Sm1 C14 C13 80.3(3) 2_656 . . . ? N1 Sm1 C14 C15 32.5(3) . . . . ? N1 Sm1 C14 C15 154.8(3) 2_656 . . . ? Cl1 Sm1 C14 C15 -82.3(3) . . . . ? C12 Sm1 C14 C15 115.5(7) 2_656 . . . ? C12 Sm1 C14 C15 94.0(3) . . . . ? C13 Sm1 C14 C15 -42.9(5) 2_656 . . . ? C13 Sm1 C14 C15 127.9(4) . . . . ? C11 Sm1 C14 C15 171.6(2) 2_656 . . . ? C11 Sm1 C14 C15 59.8(3) . . . . ? C14 Sm1 C14 C15 -82.3(3) 2_656 . . . ? C16 Sm1 C14 C15 -151.8(3) 2_656 . . . ? C13 C14 C15 C16 0.8(6) . . . . ? Sm1 C14 C15 C16 -58.6(4) . . . . ? C14 C15 C16 C11 -2.9(6) . . . . ? C14 C15 C16 Sm1 58.4(4) . . . . ? C12 C11 C16 C15 0.5(6) . . . . ? C8 C11 C16 C15 175.7(3) . . . . ? Sm1 C11 C16 C15 66.5(4) . . . . ? C12 C11 C16 Sm1 -66.0(3) . . . . ? C8 C11 C16 Sm1 109.2(3) . . . . ? N1 Sm1 C16 C15 158.0(3) . . . . ? N1 Sm1 C16 C15 -87.6(3) 2_656 . . . ? Cl1 Sm1 C16 C15 35.0(3) . . . . ? C12 Sm1 C16 C15 164.3(2) 2_656 . . . ? C12 Sm1 C16 C15 -95.1(3) . . . . ? C13 Sm1 C16 C15 128.8(3) 2_656 . . . ? C13 Sm1 C16 C15 -59.5(3) . . . . ? C11 Sm1 C16 C15 -163.8(3) 2_656 . . . ? C11 Sm1 C16 C15 -126.9(4) . . . . ? C14 Sm1 C16 C15 96.8(3) 2_656 . . . ? C14 Sm1 C16 C15 -27.7(2) . . . . ? C16 Sm1 C16 C15 34.9(3) 2_656 . . . ? N1 Sm1 C16 C11 -75.1(3) . . . . ? N1 Sm1 C16 C11 39.3(3) 2_656 . . . ? Cl1 Sm1 C16 C11 161.9(2) . . . . ? C12 Sm1 C16 C11 -68.8(3) 2_656 . . . ? C12 Sm1 C16 C11 31.7(2) . . . . ? C13 Sm1 C16 C11 -104.4(3) 2_656 . . . ? C13 Sm1 C16 C11 67.3(2) . . . . ? C11 Sm1 C16 C11 -37.0(5) 2_656 . . . ? C14 Sm1 C16 C11 -136.3(2) 2_656 . . . ? C14 Sm1 C16 C11 99.1(3) . . . . ? C16 Sm1 C16 C11 161.8(2) 2_656 . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 24.77 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.152 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.109 # attachment 'sg3325.cif' data_sg3325 _database_code_depnum_ccdc_archive 'CCDC 763509' #TrackingRef 'sg3325.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H43 N2 O Sm' _chemical_formula_weight 670.07 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 P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.408(3) _cell_length_b 17.835(5) _cell_length_c 18.082(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.807(5) _cell_angle_gamma 90.00 _cell_volume 3027.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 202(2) _cell_measurement_reflns_used 457 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.95 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 1.970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5894 _exptl_absorpt_correction_T_max 0.7565 _exptl_absorpt_process_details multi-scan _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 202(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 14492 _diffrn_reflns_av_R_equivalents 0.1323 _diffrn_reflns_av_sigmaI/netI 0.1433 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 23.44 _reflns_number_total 4395 _reflns_number_gt 2656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2000)' _computing_cell_refinement 'SMART, Bruker (2000)' _computing_data_reduction 'XPREP, Bruker (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2000)' _computing_publication_material 'SHELXTL, Bruker (2000)' _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^)+(0.0976P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4395 _refine_ls_number_parameters 369 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1313 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.1955 _refine_ls_wR_factor_gt 0.1640 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 0.76042(10) 0.2500 0.22641(5) 0.0239(3) Uani 1 2 d S . . N1 N 0.7363(12) 0.1070(6) 0.2332(6) 0.032(3) Uani 1 1 d . . . C1 C 0.9293(19) 0.2500 0.3337(10) 0.027(5) Uani 1 2 d S . . C2 C 0.9596(12) 0.1825(8) 0.3700(7) 0.026(3) Uani 1 1 d . . . C3 C 1.0124(16) 0.1839(9) 0.4441(8) 0.041(4) Uani 1 1 d . . . H3A H 1.0280 0.1380 0.4700 0.049 Uiso 1 1 calc R . . C4 C 1.042(2) 0.2500 0.4799(12) 0.051(6) Uani 1 2 d S . . H4 H 1.0825 0.2500 0.5294 0.062 Uiso 1 2 calc SR . . C5 C 0.9462(14) 0.1070(7) 0.3272(8) 0.030(3) Uani 1 1 d . . . C6 C 1.0992(15) 0.0757(9) 0.3214(8) 0.042(4) Uani 1 1 d . . . H6A H 1.1559 0.1116 0.2949 0.064 Uiso 1 1 calc R . . H6B H 1.0944 0.0280 0.2945 0.064 Uiso 1 1 calc R . . H6C H 1.1438 0.0676 0.3713 0.064 Uiso 1 1 calc R . . C7 C 0.8615(15) 0.0470(8) 0.3706(7) 0.036(4) Uani 1 1 d . . . H7A H 0.7641 0.0648 0.3757 0.054 Uiso 1 1 calc R . . H7B H 0.9090 0.0392 0.4199 0.054 Uiso 1 1 calc R . . H7C H 0.8585 -0.0005 0.3432 0.054 Uiso 1 1 calc R . . C8 C 0.8810(13) 0.1187(8) 0.2501(7) 0.026(3) Uani 1 1 d . . . C9 C 0.9437(13) 0.1407(8) 0.1857(7) 0.027(3) Uani 1 1 d . . . H9A H 1.0482 0.1472 0.1806 0.033 Uiso 1 1 calc R . . C10 C 0.8391(14) 0.1422(8) 0.1281(7) 0.029(3) Uani 1 1 d . . . H10A H 0.8538 0.1496 0.0743 0.035 Uiso 1 1 calc R . . C11 C 0.7132(14) 0.1192(8) 0.1587(7) 0.029(3) Uani 1 1 d . . . C12 C 0.5618(13) 0.1092(8) 0.1199(7) 0.031(4) Uani 1 1 d . . . C13 C 0.5727(16) 0.1001(9) 0.0352(8) 0.048(4) Uani 1 1 d . . . H13A H 0.4771 0.0937 0.0110 0.072 Uiso 1 1 calc R . . H13B H 0.6308 0.0560 0.0255 0.072 Uiso 1 1 calc R . . H13C H 0.6171 0.1450 0.0154 0.072 Uiso 1 1 calc R . . C14 C 0.4948(16) 0.0395(9) 0.1500(9) 0.049(4) Uani 1 1 d . . . H14A H 0.3996 0.0325 0.1255 0.073 Uiso 1 1 calc R . . H14B H 0.4870 0.0451 0.2035 0.073 Uiso 1 1 calc R . . H14C H 0.5542 -0.0041 0.1405 0.073 Uiso 1 1 calc R . . C15 C 0.4807(14) 0.1801(8) 0.1357(7) 0.030(3) Uani 1 1 d . . . C16 C 0.533(2) 0.2500 0.1140(10) 0.030(5) Uani 1 2 d S . . H16 H 0.6100 0.2500 0.0824 0.036 Uiso 1 2 calc SR . . C17 C 0.3571(15) 0.1832(9) 0.1747(7) 0.041(4) Uani 1 1 d . . . H17A H 0.3148 0.1372 0.1878 0.049 Uiso 1 1 calc R . . C18 C 0.2915(19) 0.2500 0.1957(11) 0.032(5) Uani 1 2 d S . . H18 H 0.2079 0.2500 0.2224 0.039 Uiso 1 2 calc SR . . O1 O 0.5764(13) 0.2500 0.3167(6) 0.031(3) Uani 1 2 d S . . C19 C 0.535(2) 0.1852(10) 0.3600(9) 0.067(5) Uani 1 1 d . . . H19A H 0.6153 0.1686 0.3942 0.080 Uiso 1 1 calc R . . H19B H 0.5060 0.1429 0.3268 0.080 Uiso 1 1 calc R . . C20 C 0.414(2) 0.2099(11) 0.4018(11) 0.085(7) Uani 1 1 d . . . H20A H 0.3237 0.1907 0.3781 0.102 Uiso 1 1 calc R . . H20B H 0.4252 0.1907 0.4532 0.102 Uiso 1 1 calc R . . Sm2 Sm 0.81076(10) 0.2500 0.74420(5) 0.0259(4) Uani 1 2 d S . . N2 N 0.7830(11) 0.1063(6) 0.7473(6) 0.027(3) Uani 1 1 d . . . C21 C 1.0917(19) 0.2500 1.0019(10) 0.031(4) Uani 1 2 d S . . H21 H 1.1317 0.2500 1.0515 0.037 Uiso 1 2 calc SR . . C22 C 1.0631(15) 0.1826(9) 0.9664(7) 0.040(4) Uani 1 1 d . . . H22A H 1.0886 0.1368 0.9906 0.049 Uiso 1 1 calc R . . C23 C 0.9973(14) 0.1815(8) 0.8957(7) 0.029(3) Uani 1 1 d . . . C24 C 0.9617(19) 0.2500 0.8591(10) 0.031(4) Uani 1 2 d S . . C25 C 0.9723(15) 0.1072(8) 0.8523(8) 0.037(4) Uani 1 1 d . . . C26 C 0.8689(16) 0.0574(9) 0.8943(8) 0.045(4) Uani 1 1 d . . . H26A H 0.7760 0.0822 0.8946 0.068 Uiso 1 1 calc R . . H26B H 0.9077 0.0499 0.9454 0.068 Uiso 1 1 calc R . . H26C H 0.8578 0.0088 0.8694 0.068 Uiso 1 1 calc R . . C27 C 1.1163(16) 0.0631(9) 0.8555(8) 0.051(4) Uani 1 1 d . . . H27A H 1.1869 0.0918 0.8298 0.076 Uiso 1 1 calc R . . H27B H 1.1015 0.0143 0.8313 0.076 Uiso 1 1 calc R . . H27C H 1.1507 0.0557 0.9073 0.076 Uiso 1 1 calc R . . C28 C 0.9200(14) 0.1167(8) 0.7748(7) 0.026(3) Uani 1 1 d . . . C29 C 1.0046(15) 0.1396(8) 0.7156(8) 0.037(4) Uani 1 1 d . . . H29A H 1.1107 0.1450 0.7183 0.045 Uiso 1 1 calc R . . C30 C 0.9139(15) 0.1403(7) 0.6509(8) 0.030(3) Uani 1 1 d . . . H30A H 0.9422 0.1477 0.5990 0.035 Uiso 1 1 calc R . . C31 C 0.7775(13) 0.1187(8) 0.6728(7) 0.024(3) Uani 1 1 d . . . C32 C 0.6377(14) 0.1085(8) 0.6242(7) 0.029(3) Uani 1 1 d . . . C33 C 0.6758(19) 0.0944(9) 0.5417(8) 0.056(5) Uani 1 1 d . . . H33A H 0.5879 0.0877 0.5102 0.084 Uiso 1 1 calc R . . H33B H 0.7346 0.0492 0.5395 0.084 Uiso 1 1 calc R . . H33C H 0.7286 0.1375 0.5241 0.084 Uiso 1 1 calc R . . C34 C 0.5603(16) 0.0413(9) 0.6510(9) 0.049(4) Uani 1 1 d . . . H34A H 0.5352 0.0497 0.7021 0.073 Uiso 1 1 calc R . . H34B H 0.6218 -0.0030 0.6493 0.073 Uiso 1 1 calc R . . H34C H 0.4734 0.0331 0.6191 0.073 Uiso 1 1 calc R . . C35 C 0.5495(15) 0.1799(7) 0.6261(7) 0.031(3) Uani 1 1 d . . . C36 C 0.4059(14) 0.1811(9) 0.6402(8) 0.038(4) Uani 1 1 d . . . H36A H 0.3546 0.1357 0.6456 0.046 Uiso 1 1 calc R . . C37 C 0.339(2) 0.2500 0.6462(11) 0.040(5) Uani 1 2 d S . . H37 H 0.2409 0.2500 0.6550 0.048 Uiso 1 2 calc SR . . C38 C 0.615(2) 0.2500 0.6123(10) 0.035(5) Uani 1 2 d S . . H38 H 0.7060 0.2500 0.5928 0.042 Uiso 1 2 calc SR . . O2 O 0.6004(12) 0.2500 0.8115(7) 0.042(4) Uani 1 2 d SD . . C39 C 0.517(2) 0.1880(12) 0.8394(14) 0.108(6) Uani 1 1 d D . . H39A H 0.4839 0.1557 0.7970 0.130 Uiso 1 1 calc R . . H39B H 0.5794 0.1572 0.8734 0.130 Uiso 1 1 calc R . . C40 C 0.394(2) 0.2110(11) 0.8778(13) 0.108(6) Uani 1 1 d D . . H40A H 0.3054 0.1916 0.8521 0.130 Uiso 1 1 calc R . . H40B H 0.4009 0.1916 0.9292 0.130 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 0.0182(6) 0.0208(7) 0.0330(6) 0.000 0.0042(5) 0.000 N1 0.029(7) 0.025(8) 0.044(8) -0.013(6) 0.019(6) -0.001(5) C1 0.019(11) 0.022(13) 0.039(12) 0.000 -0.003(9) 0.000 C2 0.010(7) 0.032(10) 0.035(8) 0.009(6) 0.007(6) 0.003(6) C3 0.045(10) 0.048(12) 0.030(9) 0.002(7) 0.005(7) 0.003(8) C4 0.061(17) 0.06(2) 0.030(12) 0.000 0.002(11) 0.000 C5 0.028(8) 0.011(9) 0.052(9) 0.002(6) 0.016(7) 0.001(6) C6 0.031(9) 0.043(11) 0.053(9) -0.002(8) 0.006(7) 0.023(7) C7 0.034(9) 0.043(11) 0.031(8) 0.007(7) 0.007(6) 0.007(7) C8 0.013(8) 0.033(9) 0.033(8) -0.006(6) 0.003(6) -0.001(6) C9 0.011(7) 0.029(9) 0.042(8) 0.000(7) 0.010(7) 0.001(6) C10 0.029(8) 0.038(10) 0.023(7) -0.009(6) 0.018(6) 0.000(7) C11 0.024(8) 0.028(9) 0.037(9) -0.006(7) 0.010(7) -0.002(6) C12 0.019(8) 0.035(10) 0.039(8) -0.009(7) -0.001(6) -0.013(7) C13 0.044(10) 0.049(12) 0.050(10) -0.013(8) 0.001(8) -0.002(8) C14 0.038(10) 0.041(11) 0.067(11) -0.009(8) 0.007(8) -0.001(8) C15 0.022(8) 0.044(10) 0.024(8) 0.003(7) -0.007(6) -0.002(7) C16 0.025(11) 0.037(15) 0.029(11) 0.000 0.004(9) 0.000 C17 0.029(9) 0.053(12) 0.039(9) 0.005(7) -0.002(7) -0.009(8) C18 0.022(11) 0.009(12) 0.066(14) 0.000 0.015(10) 0.000 O1 0.031(8) 0.052(10) 0.012(6) 0.000 0.013(5) 0.000 C19 0.101(15) 0.043(12) 0.061(11) 0.022(9) 0.044(10) 0.014(10) C20 0.066(13) 0.091(17) 0.104(15) 0.015(12) 0.054(11) -0.003(10) Sm2 0.0192(6) 0.0240(7) 0.0350(7) 0.000 0.0050(5) 0.000 N2 0.024(7) 0.015(7) 0.041(7) -0.013(5) 0.004(5) 0.004(5) C21 0.018(8) 0.053(12) 0.024(8) 0.000 0.011(6) 0.000 C22 0.039(9) 0.054(12) 0.028(8) 0.010(7) 0.002(7) 0.000(8) C23 0.021(8) 0.025(9) 0.043(9) 0.000(7) 0.011(7) -0.001(6) C24 0.018(8) 0.053(12) 0.024(8) 0.000 0.011(6) 0.000 C25 0.026(8) 0.035(11) 0.052(10) 0.008(7) 0.001(7) 0.003(7) C26 0.049(10) 0.046(11) 0.039(9) 0.016(8) -0.004(7) -0.008(8) C27 0.045(10) 0.046(12) 0.058(10) -0.012(8) -0.018(8) 0.009(8) C28 0.020(8) 0.032(9) 0.027(8) -0.002(6) 0.009(6) -0.003(6) C29 0.030(9) 0.025(10) 0.059(10) 0.002(7) 0.016(8) 0.004(7) C30 0.037(9) 0.017(9) 0.036(8) -0.003(6) 0.019(7) -0.003(6) C31 0.019(8) 0.027(9) 0.025(8) 0.003(6) 0.001(6) 0.004(6) C32 0.032(8) 0.027(10) 0.028(8) 0.004(6) 0.000(6) 0.004(7) C33 0.081(13) 0.041(12) 0.045(10) -0.019(8) -0.008(9) 0.015(9) C34 0.046(10) 0.024(10) 0.076(12) 0.007(8) 0.000(8) -0.008(8) C35 0.044(9) 0.012(9) 0.036(8) -0.002(6) -0.003(7) -0.003(7) C36 0.017(8) 0.051(11) 0.048(9) -0.002(8) 0.012(7) -0.010(7) C37 0.027(12) 0.039(16) 0.056(14) 0.000 0.011(10) 0.000 C38 0.019(11) 0.038(15) 0.046(13) 0.000 -0.008(9) 0.000 O2 0.015(7) 0.060(11) 0.056(9) 0.000 0.025(6) 0.000 C39 0.101(13) 0.081(12) 0.155(15) 0.017(10) 0.097(11) 0.009(9) C40 0.101(13) 0.081(12) 0.155(15) 0.017(10) 0.097(11) 0.009(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 C1 2.425(17) . ? Sm1 O1 2.457(11) . ? Sm1 N1 2.564(11) . ? Sm1 N1 2.564(11) 4_565 ? Sm1 C8 2.626(14) 4_565 ? Sm1 C8 2.626(14) . ? Sm1 C11 2.658(13) . ? Sm1 C11 2.658(13) 4_565 ? Sm1 C9 2.736(13) 4_565 ? Sm1 C9 2.736(13) . ? Sm1 C10 2.753(12) . ? Sm1 C10 2.753(12) 4_565 ? N1 C11 1.367(16) . ? N1 C8 1.391(16) . ? C1 C2 1.391(15) . ? C1 C2 1.391(15) 4_565 ? C2 C3 1.398(18) . ? C2 C5 1.554(19) . ? C3 C4 1.364(17) . ? C3 H3A 0.9500 . ? C4 C3 1.364(17) 4_565 ? C4 H4 0.9500 . ? C5 C8 1.499(18) . ? C5 C6 1.554(18) . ? C5 C7 1.575(18) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.397(17) . ? C9 C10 1.385(17) . ? C9 H9A 1.0000 . ? C10 C11 1.402(17) . ? C10 H10A 1.0000 . ? C11 C12 1.556(18) . ? C12 C14 1.51(2) . ? C12 C15 1.51(2) . ? C12 C13 1.550(18) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.401(18) . ? C15 C16 1.407(16) . ? C16 C15 1.407(16) 4_565 ? C16 H16 0.9500 . ? C17 C18 1.405(18) . ? C17 H17A 0.9500 . ? C18 C17 1.405(18) 4_565 ? C18 H18 0.9500 . ? O1 C19 1.464(16) . ? O1 C19 1.464(16) 4_565 ? C19 C20 1.47(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C20 1.43(4) 4_565 ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? Sm2 O2 2.392(11) . ? Sm2 C24 2.437(18) . ? Sm2 N2 2.577(11) . ? Sm2 N2 2.577(11) 4_565 ? Sm2 C28 2.634(14) . ? Sm2 C28 2.634(14) 4_565 ? Sm2 C31 2.683(13) . ? Sm2 C31 2.683(13) 4_565 ? Sm2 C29 2.757(14) . ? Sm2 C29 2.757(14) 4_565 ? Sm2 C30 2.799(13) . ? Sm2 C30 2.799(13) 4_565 ? N2 C28 1.363(16) . ? N2 C31 1.364(15) . ? C21 C22 1.381(17) . ? C21 C22 1.381(17) 4_565 ? C21 H21 0.9500 . ? C22 C23 1.383(18) . ? C22 H22A 0.9500 . ? C23 C24 1.419(16) . ? C23 C25 1.550(19) . ? C24 C23 1.419(16) 4_565 ? C25 C28 1.465(18) . ? C25 C26 1.551(19) . ? C25 C27 1.563(19) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.435(18) . ? C29 C30 1.401(19) . ? C29 H29A 1.0000 . ? C30 C31 1.421(17) . ? C30 H30A 1.0000 . ? C31 C32 1.543(18) . ? C32 C34 1.500(19) . ? C32 C35 1.521(19) . ? C32 C33 1.578(19) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.392(18) . ? C35 C38 1.423(16) . ? C36 C37 1.387(17) . ? C36 H36A 0.9500 . ? C37 C36 1.387(17) 4_565 ? C37 H37 0.9500 . ? C38 C35 1.423(16) 4_565 ? C38 H38 0.9500 . ? O2 C39 1.47(2) . ? O2 C39 1.47(2) 4_565 ? C39 C40 1.446(16) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C40 1.39(4) 4_565 ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sm1 O1 85.5(5) . . ? C1 Sm1 N1 91.0(3) . . ? O1 Sm1 N1 84.2(2) . . ? C1 Sm1 N1 91.0(3) . 4_565 ? O1 Sm1 N1 84.2(2) . 4_565 ? N1 Sm1 N1 168.1(5) . 4_565 ? C1 Sm1 C8 67.4(3) . 4_565 ? O1 Sm1 C8 102.0(3) . 4_565 ? N1 Sm1 C8 156.7(4) . 4_565 ? N1 Sm1 C8 31.1(4) 4_565 4_565 ? C1 Sm1 C8 67.4(3) . . ? O1 Sm1 C8 102.0(3) . . ? N1 Sm1 C8 31.1(4) . . ? N1 Sm1 C8 156.7(4) 4_565 . ? C8 Sm1 C8 126.3(6) 4_565 . ? C1 Sm1 C11 116.7(3) . . ? O1 Sm1 C11 101.7(3) . . ? N1 Sm1 C11 30.3(4) . . ? N1 Sm1 C11 151.9(4) 4_565 . ? C8 Sm1 C11 156.3(4) 4_565 . ? C8 Sm1 C11 49.4(4) . . ? C1 Sm1 C11 116.7(3) . 4_565 ? O1 Sm1 C11 101.7(3) . 4_565 ? N1 Sm1 C11 151.9(4) . 4_565 ? N1 Sm1 C11 30.3(4) 4_565 4_565 ? C8 Sm1 C11 49.4(4) 4_565 4_565 ? C8 Sm1 C11 156.3(4) . 4_565 ? C11 Sm1 C11 122.7(6) . 4_565 ? C1 Sm1 C9 79.9(4) . 4_565 ? O1 Sm1 C9 131.5(3) . 4_565 ? N1 Sm1 C9 141.4(4) . 4_565 ? N1 Sm1 C9 50.5(4) 4_565 4_565 ? C8 Sm1 C9 30.1(4) 4_565 4_565 ? C8 Sm1 C9 114.0(4) . 4_565 ? C11 Sm1 C9 126.2(4) . 4_565 ? C11 Sm1 C9 48.7(4) 4_565 4_565 ? C1 Sm1 C9 79.9(4) . . ? O1 Sm1 C9 131.5(3) . . ? N1 Sm1 C9 50.5(4) . . ? N1 Sm1 C9 141.4(4) 4_565 . ? C8 Sm1 C9 114.0(4) 4_565 . ? C8 Sm1 C9 30.1(4) . . ? C11 Sm1 C9 48.7(4) . . ? C11 Sm1 C9 126.2(4) 4_565 . ? C9 Sm1 C9 90.9(5) 4_565 . ? C1 Sm1 C10 109.1(4) . . ? O1 Sm1 C10 131.3(3) . . ? N1 Sm1 C10 50.6(4) . . ? N1 Sm1 C10 138.9(4) 4_565 . ? C8 Sm1 C10 126.6(4) 4_565 . ? C8 Sm1 C10 49.5(4) . . ? C11 Sm1 C10 30.0(4) . . ? C11 Sm1 C10 111.1(4) 4_565 . ? C9 Sm1 C10 97.0(4) 4_565 . ? C9 Sm1 C10 29.2(4) . . ? C1 Sm1 C10 109.1(4) . 4_565 ? O1 Sm1 C10 131.3(3) . 4_565 ? N1 Sm1 C10 138.9(4) . 4_565 ? N1 Sm1 C10 50.6(4) 4_565 4_565 ? C8 Sm1 C10 49.5(4) 4_565 4_565 ? C8 Sm1 C10 126.6(4) . 4_565 ? C11 Sm1 C10 111.1(4) . 4_565 ? C11 Sm1 C10 30.0(4) 4_565 4_565 ? C9 Sm1 C10 29.2(4) 4_565 4_565 ? C9 Sm1 C10 97.0(4) . 4_565 ? C10 Sm1 C10 88.6(6) . 4_565 ? C11 N1 C8 106.4(11) . . ? C11 N1 Sm1 78.7(8) . . ? C8 N1 Sm1 76.9(7) . . ? C2 C1 C2 119.8(17) . 4_565 ? C2 C1 Sm1 118.7(8) . . ? C2 C1 Sm1 118.7(8) 4_565 . ? C1 C2 C3 119.0(14) . . ? C1 C2 C5 120.5(12) . . ? C3 C2 C5 120.3(12) . . ? C4 C3 C2 121.1(16) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C3 120(2) . 4_565 ? C3 C4 H4 120.2 . . ? C3 C4 H4 120.2 4_565 . ? C8 C5 C6 108.2(11) . . ? C8 C5 C2 111.0(11) . . ? C6 C5 C2 107.5(11) . . ? C8 C5 C7 111.6(11) . . ? C6 C5 C7 106.9(11) . . ? C2 C5 C7 111.5(11) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 108.6(11) . . ? N1 C8 C5 121.2(11) . . ? C9 C8 C5 130.1(12) . . ? N1 C8 Sm1 72.0(7) . . ? C9 C8 Sm1 79.3(8) . . ? C5 C8 Sm1 114.9(8) . . ? C10 C9 C8 108.3(12) . . ? C10 C9 Sm1 76.0(7) . . ? C8 C9 Sm1 70.6(8) . . ? C10 C9 H9A 125.6 . . ? C8 C9 H9A 125.6 . . ? Sm1 C9 H9A 125.6 . . ? C9 C10 C11 105.9(11) . . ? C9 C10 Sm1 74.7(7) . . ? C11 C10 Sm1 71.3(7) . . ? C9 C10 H10A 126.7 . . ? C11 C10 H10A 126.7 . . ? Sm1 C10 H10A 126.7 . . ? N1 C11 C10 110.6(11) . . ? N1 C11 C12 120.4(11) . . ? C10 C11 C12 128.9(12) . . ? N1 C11 Sm1 71.1(7) . . ? C10 C11 Sm1 78.7(8) . . ? C12 C11 Sm1 115.4(8) . . ? C14 C12 C15 113.0(12) . . ? C14 C12 C13 109.1(12) . . ? C15 C12 C13 109.9(12) . . ? C14 C12 C11 108.9(12) . . ? C15 C12 C11 106.1(10) . . ? C13 C12 C11 109.8(11) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 115.0(14) . . ? C17 C15 C12 125.0(13) . . ? C16 C15 C12 119.8(12) . . ? C15 C16 C15 124.9(18) . 4_565 ? C15 C16 Sm1 93.6(9) . . ? C15 C16 Sm1 93.6(9) 4_565 . ? C15 C16 H16 117.5 . . ? C15 C16 H16 117.5 4_565 . ? Sm1 C16 H16 82.3 . . ? C15 C17 C18 124.4(15) . . ? C15 C17 H17A 117.8 . . ? C18 C17 H17A 117.8 . . ? C17 C18 C17 115.9(18) . 4_565 ? C17 C18 H18 122.1 . . ? C17 C18 H18 122.1 4_565 . ? C19 O1 C19 104.4(15) . 4_565 ? C19 O1 Sm1 125.4(8) . . ? C19 O1 Sm1 125.4(8) 4_565 . ? O1 C19 C20 106.2(14) . . ? O1 C19 H19A 110.5 . . ? C20 C19 H19A 110.5 . . ? O1 C19 H19B 110.5 . . ? C20 C19 H19B 110.5 . . ? H19A C19 H19B 108.7 . . ? C20 C20 C19 107.5(10) 4_565 . ? C20 C20 H20A 110.2 4_565 . ? C19 C20 H20A 110.2 . . ? C20 C20 H20B 110.2 4_565 . ? C19 C20 H20B 110.2 . . ? H20A C20 H20B 108.5 . . ? O2 Sm2 C24 91.2(5) . . ? O2 Sm2 N2 84.3(2) . . ? C24 Sm2 N2 92.0(2) . . ? O2 Sm2 N2 84.3(2) . 4_565 ? C24 Sm2 N2 92.0(2) . 4_565 ? N2 Sm2 N2 167.9(5) . 4_565 ? O2 Sm2 C28 102.6(3) . . ? C24 Sm2 C28 67.9(3) . . ? N2 Sm2 C28 30.3(3) . . ? N2 Sm2 C28 158.7(4) 4_565 . ? O2 Sm2 C28 102.6(3) . 4_565 ? C24 Sm2 C28 67.9(3) . 4_565 ? N2 Sm2 C28 158.7(4) . 4_565 ? N2 Sm2 C28 30.3(3) 4_565 4_565 ? C28 Sm2 C28 129.0(6) . 4_565 ? O2 Sm2 C31 99.9(3) . . ? C24 Sm2 C31 116.9(3) . . ? N2 Sm2 C31 30.0(3) . . ? N2 Sm2 C31 150.5(4) 4_565 . ? C28 Sm2 C31 49.0(4) . . ? C28 Sm2 C31 157.0(4) 4_565 . ? O2 Sm2 C31 99.9(3) . 4_565 ? C24 Sm2 C31 116.9(3) . 4_565 ? N2 Sm2 C31 150.5(4) . 4_565 ? N2 Sm2 C31 30.0(3) 4_565 4_565 ? C28 Sm2 C31 157.0(4) . 4_565 ? C28 Sm2 C31 49.0(4) 4_565 4_565 ? C31 Sm2 C31 121.6(5) . 4_565 ? O2 Sm2 C29 132.5(3) . . ? C24 Sm2 C29 78.7(4) . . ? N2 Sm2 C29 50.4(4) . . ? N2 Sm2 C29 141.6(4) 4_565 . ? C28 Sm2 C29 30.8(4) . . ? C28 Sm2 C29 115.5(4) 4_565 . ? C31 Sm2 C29 48.9(4) . . ? C31 Sm2 C29 126.2(4) 4_565 . ? O2 Sm2 C29 132.5(3) . 4_565 ? C24 Sm2 C29 78.7(4) . 4_565 ? N2 Sm2 C29 141.6(4) . 4_565 ? N2 Sm2 C29 50.4(4) 4_565 4_565 ? C28 Sm2 C29 115.5(4) . 4_565 ? C28 Sm2 C29 30.8(4) 4_565 4_565 ? C31 Sm2 C29 126.2(4) . 4_565 ? C31 Sm2 C29 48.9(4) 4_565 4_565 ? C29 Sm2 C29 91.2(6) . 4_565 ? O2 Sm2 C30 129.7(3) . . ? C24 Sm2 C30 107.9(4) . . ? N2 Sm2 C30 50.1(4) . . ? N2 Sm2 C30 138.4(4) 4_565 . ? C28 Sm2 C30 49.4(4) . . ? C28 Sm2 C30 127.7(4) 4_565 . ? C31 Sm2 C30 30.0(4) . . ? C31 Sm2 C30 110.7(4) 4_565 . ? C29 Sm2 C30 29.2(4) . . ? C29 Sm2 C30 97.2(4) 4_565 . ? O2 Sm2 C30 129.7(3) . 4_565 ? C24 Sm2 C30 107.9(4) . 4_565 ? N2 Sm2 C30 138.4(4) . 4_565 ? N2 Sm2 C30 50.1(4) 4_565 4_565 ? C28 Sm2 C30 127.7(4) . 4_565 ? C28 Sm2 C30 49.4(4) 4_565 4_565 ? C31 Sm2 C30 110.7(4) . 4_565 ? C31 Sm2 C30 30.0(4) 4_565 4_565 ? C29 Sm2 C30 97.2(4) . 4_565 ? C29 Sm2 C30 29.2(4) 4_565 4_565 ? C30 Sm2 C30 88.7(5) . 4_565 ? C28 N2 C31 108.1(11) . . ? C28 N2 Sm2 77.2(7) . . ? C31 N2 Sm2 79.3(7) . . ? C22 C21 C22 121.1(18) . 4_565 ? C22 C21 H21 119.5 . . ? C22 C21 H21 119.5 4_565 . ? C21 C22 C23 120.2(15) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C22 C23 C24 119.7(14) . . ? C22 C23 C25 121.5(13) . . ? C24 C23 C25 118.5(12) . . ? C23 C24 C23 118.9(17) . 4_565 ? C23 C24 Sm2 120.2(8) . . ? C23 C24 Sm2 120.2(8) 4_565 . ? C28 C25 C23 114.5(12) . . ? C28 C25 C26 110.7(11) . . ? C23 C25 C26 108.7(12) . . ? C28 C25 C27 109.2(12) . . ? C23 C25 C27 108.0(11) . . ? C26 C25 C27 105.4(13) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 C28 C29 108.9(11) . . ? N2 C28 C25 125.6(11) . . ? C29 C28 C25 125.4(13) . . ? N2 C28 Sm2 72.5(7) . . ? C29 C28 Sm2 79.3(8) . . ? C25 C28 Sm2 114.0(9) . . ? C30 C29 C28 106.8(13) . . ? C30 C29 Sm2 77.0(8) . . ? C28 C29 Sm2 69.9(8) . . ? C30 C29 H29A 126.2 . . ? C28 C29 H29A 126.2 . . ? Sm2 C29 H29A 126.2 . . ? C29 C30 C31 106.0(12) . . ? C29 C30 Sm2 73.7(8) . . ? C31 C30 Sm2 70.5(7) . . ? C29 C30 H30A 126.7 . . ? C31 C30 H30A 126.7 . . ? Sm2 C30 H30A 126.7 . . ? N2 C31 C30 110.1(11) . . ? N2 C31 C32 121.2(11) . . ? C30 C31 C32 128.7(11) . . ? N2 C31 Sm2 70.7(7) . . ? C30 C31 Sm2 79.5(8) . . ? C32 C31 Sm2 116.4(8) . . ? C34 C32 C35 112.6(12) . . ? C34 C32 C31 108.9(11) . . ? C35 C32 C31 109.6(11) . . ? C34 C32 C33 108.8(13) . . ? C35 C32 C33 108.3(11) . . ? C31 C32 C33 108.6(11) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C38 117.0(14) . . ? C36 C35 C32 123.7(13) . . ? C38 C35 C32 119.3(13) . . ? C37 C36 C35 118.5(15) . . ? C37 C36 H36A 120.8 . . ? C35 C36 H36A 120.8 . . ? C36 C37 C36 124.8(19) . 4_565 ? C36 C37 H37 117.6 . . ? C36 C37 H37 117.6 4_565 . ? C35 C38 C35 123.1(18) . 4_565 ? C35 C38 Sm2 96.4(9) . . ? C35 C38 Sm2 96.4(9) 4_565 . ? C35 C38 H38 118.4 . . ? C35 C38 H38 118.4 4_565 . ? Sm2 C38 H38 76.4 . . ? C39 O2 C39 98.0(15) . 4_565 ? C39 O2 Sm2 131.0(8) . . ? C39 O2 Sm2 131.0(8) 4_565 . ? C40 C39 O2 114.5(15) . . ? C40 C39 H39A 108.6 . . ? O2 C39 H39A 108.6 . . ? C40 C39 H39B 108.6 . . ? O2 C39 H39B 108.6 . . ? H39A C39 H39B 107.6 . . ? C40 C40 C39 106.5(11) 4_565 . ? C40 C40 H40A 110.4 4_565 . ? C39 C40 H40A 110.4 . . ? C40 C40 H40B 110.4 4_565 . ? C39 C40 H40B 110.4 . . ? H40A C40 H40B 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Sm1 N1 C11 -149.5(8) . . . . ? O1 Sm1 N1 C11 125.2(7) . . . . ? N1 Sm1 N1 C11 111(2) 4_565 . . . ? C8 Sm1 N1 C11 -127.8(10) 4_565 . . . ? C8 Sm1 N1 C11 -110.0(10) . . . . ? C11 Sm1 N1 C11 21.1(9) 4_565 . . . ? C9 Sm1 N1 C11 -74.5(9) 4_565 . . . ? C9 Sm1 N1 C11 -73.5(7) . . . . ? C10 Sm1 N1 C11 -35.3(7) . . . . ? C10 Sm1 N1 C11 -28.3(9) 4_565 . . . ? C1 Sm1 N1 C8 -39.4(8) . . . . ? O1 Sm1 N1 C8 -124.8(8) . . . . ? N1 Sm1 N1 C8 -139(2) 4_565 . . . ? C8 Sm1 N1 C8 -17.8(10) 4_565 . . . ? C11 Sm1 N1 C8 110.0(10) . . . . ? C11 Sm1 N1 C8 131.1(9) 4_565 . . . ? C9 Sm1 N1 C8 35.5(10) 4_565 . . . ? C9 Sm1 N1 C8 36.5(7) . . . . ? C10 Sm1 N1 C8 74.7(8) . . . . ? C10 Sm1 N1 C8 81.7(9) 4_565 . . . ? O1 Sm1 C1 C2 80.5(12) . . . . ? N1 Sm1 C1 C2 -3.7(12) . . . . ? N1 Sm1 C1 C2 164.6(12) 4_565 . . . ? C8 Sm1 C1 C2 -174.6(14) 4_565 . . . ? C8 Sm1 C1 C2 -24.5(11) . . . . ? C11 Sm1 C1 C2 -20.3(14) . . . . ? C11 Sm1 C1 C2 -178.7(11) 4_565 . . . ? C9 Sm1 C1 C2 -145.9(13) 4_565 . . . ? C9 Sm1 C1 C2 -53.1(12) . . . . ? C10 Sm1 C1 C2 -51.9(13) . . . . ? C10 Sm1 C1 C2 -147.2(12) 4_565 . . . ? O1 Sm1 C1 C2 -80.5(12) . . . 4_565 ? N1 Sm1 C1 C2 -164.6(12) . . . 4_565 ? N1 Sm1 C1 C2 3.7(12) 4_565 . . 4_565 ? C8 Sm1 C1 C2 24.5(11) 4_565 . . 4_565 ? C8 Sm1 C1 C2 174.6(14) . . . 4_565 ? C11 Sm1 C1 C2 178.7(11) . . . 4_565 ? C11 Sm1 C1 C2 20.3(14) 4_565 . . 4_565 ? C9 Sm1 C1 C2 53.1(12) 4_565 . . 4_565 ? C9 Sm1 C1 C2 145.9(13) . . . 4_565 ? C10 Sm1 C1 C2 147.2(12) . . . 4_565 ? C10 Sm1 C1 C2 51.9(13) 4_565 . . 4_565 ? C2 C1 C2 C3 4(2) 4_565 . . . ? Sm1 C1 C2 C3 -157.0(10) . . . . ? C2 C1 C2 C5 -171.5(10) 4_565 . . . ? Sm1 C1 C2 C5 27.7(17) . . . . ? C1 C2 C3 C4 -4(2) . . . . ? C5 C2 C3 C4 171.7(15) . . . . ? C2 C3 C4 C3 3(3) . . . 4_565 ? C1 C2 C5 C8 -7.5(17) . . . . ? C3 C2 C5 C8 177.3(11) . . . . ? C1 C2 C5 C6 110.6(14) . . . . ? C3 C2 C5 C6 -64.6(15) . . . . ? C1 C2 C5 C7 -132.6(14) . . . . ? C3 C2 C5 C7 52.2(15) . . . . ? C11 N1 C8 C9 2.2(14) . . . . ? Sm1 N1 C8 C9 -71.7(10) . . . . ? C11 N1 C8 C5 -177.5(12) . . . . ? Sm1 N1 C8 C5 108.7(11) . . . . ? C11 N1 C8 Sm1 73.8(9) . . . . ? C6 C5 C8 N1 145.2(12) . . . . ? C2 C5 C8 N1 -97.2(14) . . . . ? C7 C5 C8 N1 27.9(17) . . . . ? C6 C5 C8 C9 -34.3(19) . . . . ? C2 C5 C8 C9 83.3(17) . . . . ? C7 C5 C8 C9 -151.6(14) . . . . ? C6 C5 C8 Sm1 -131.5(10) . . . . ? C2 C5 C8 Sm1 -13.8(12) . . . . ? C7 C5 C8 Sm1 111.2(10) . . . . ? C1 Sm1 C8 N1 136.5(9) . . . . ? O1 Sm1 C8 N1 56.6(7) . . . . ? N1 Sm1 C8 N1 160.1(11) 4_565 . . . ? C8 Sm1 C8 N1 171.4(5) 4_565 . . . ? C11 Sm1 C8 N1 -38.6(7) . . . . ? C11 Sm1 C8 N1 -118.2(11) 4_565 . . . ? C9 Sm1 C8 N1 -156.6(7) 4_565 . . . ? C9 Sm1 C8 N1 -113.8(11) . . . . ? C10 Sm1 C8 N1 -78.4(8) . . . . ? C10 Sm1 C8 N1 -125.9(7) 4_565 . . . ? C1 Sm1 C8 C9 -109.7(9) . . . . ? O1 Sm1 C8 C9 170.4(7) . . . . ? N1 Sm1 C8 C9 113.8(11) . . . . ? N1 Sm1 C8 C9 -86.1(11) 4_565 . . . ? C8 Sm1 C8 C9 -74.9(10) 4_565 . . . ? C11 Sm1 C8 C9 75.2(8) . . . . ? C11 Sm1 C8 C9 -4.4(15) 4_565 . . . ? C9 Sm1 C8 C9 -42.9(8) 4_565 . . . ? C10 Sm1 C8 C9 35.4(7) . . . . ? C10 Sm1 C8 C9 -12.1(9) 4_565 . . . ? C1 Sm1 C8 C5 19.8(9) . . . . ? O1 Sm1 C8 C5 -60.1(9) . . . . ? N1 Sm1 C8 C5 -116.8(12) . . . . ? N1 Sm1 C8 C5 43.3(14) 4_565 . . . ? C8 Sm1 C8 C5 54.6(12) 4_565 . . . ? C11 Sm1 C8 C5 -155.3(11) . . . . ? C11 Sm1 C8 C5 125.0(11) 4_565 . . . ? C9 Sm1 C8 C5 86.6(9) 4_565 . . . ? C9 Sm1 C8 C5 129.5(13) . . . . ? C10 Sm1 C8 C5 164.9(11) . . . . ? C10 Sm1 C8 C5 117.4(9) 4_565 . . . ? N1 C8 C9 C10 -0.5(15) . . . . ? C5 C8 C9 C10 179.0(13) . . . . ? Sm1 C8 C9 C10 -67.3(10) . . . . ? N1 C8 C9 Sm1 66.7(9) . . . . ? C5 C8 C9 Sm1 -113.7(15) . . . . ? C1 Sm1 C9 C10 177.6(8) . . . . ? O1 Sm1 C9 C10 102.9(8) . . . . ? N1 Sm1 C9 C10 77.8(8) . . . . ? N1 Sm1 C9 C10 -103.7(9) 4_565 . . . ? C8 Sm1 C9 C10 -122.8(8) 4_565 . . . ? C8 Sm1 C9 C10 115.5(12) . . . . ? C11 Sm1 C9 C10 37.7(8) . . . . ? C11 Sm1 C9 C10 -66.7(9) 4_565 . . . ? C9 Sm1 C9 C10 -102.9(8) 4_565 . . . ? C10 Sm1 C9 C10 -74.2(9) 4_565 . . . ? C1 Sm1 C9 C8 62.0(8) . . . . ? O1 Sm1 C9 C8 -12.6(10) . . . . ? N1 Sm1 C9 C8 -37.8(7) . . . . ? N1 Sm1 C9 C8 140.8(8) 4_565 . . . ? C8 Sm1 C9 C8 121.6(9) 4_565 . . . ? C11 Sm1 C9 C8 -77.8(8) . . . . ? C11 Sm1 C9 C8 177.8(7) 4_565 . . . ? C9 Sm1 C9 C8 141.6(6) 4_565 . . . ? C10 Sm1 C9 C8 -115.5(12) . . . . ? C10 Sm1 C9 C8 170.2(8) 4_565 . . . ? C8 C9 C10 C11 -1.3(15) . . . . ? Sm1 C9 C10 C11 -64.9(9) . . . . ? C8 C9 C10 Sm1 63.7(9) . . . . ? C1 Sm1 C10 C9 -2.5(9) . . . . ? O1 Sm1 C10 C9 -103.7(8) . . . . ? N1 Sm1 C10 C9 -77.4(8) . . . . ? N1 Sm1 C10 C9 112.6(8) 4_565 . . . ? C8 Sm1 C10 C9 73.1(9) 4_565 . . . ? C8 Sm1 C10 C9 -36.5(7) . . . . ? C11 Sm1 C10 C9 -113.1(12) . . . . ? C11 Sm1 C10 C9 127.4(8) 4_565 . . . ? C9 Sm1 C10 C9 79.1(9) 4_565 . . . ? C10 Sm1 C10 C9 107.2(7) 4_565 . . . ? C1 Sm1 C10 C11 110.6(8) . . . . ? O1 Sm1 C10 C11 9.4(10) . . . . ? N1 Sm1 C10 C11 35.7(7) . . . . ? N1 Sm1 C10 C11 -134.3(8) 4_565 . . . ? C8 Sm1 C10 C11 -173.8(8) 4_565 . . . ? C8 Sm1 C10 C11 76.6(9) . . . . ? C11 Sm1 C10 C11 -119.4(10) 4_565 . . . ? C9 Sm1 C10 C11 -167.7(8) 4_565 . . . ? C9 Sm1 C10 C11 113.1(12) . . . . ? C10 Sm1 C10 C11 -139.7(7) 4_565 . . . ? C8 N1 C11 C10 -3.0(15) . . . . ? Sm1 N1 C11 C10 69.5(10) . . . . ? C8 N1 C11 C12 178.6(12) . . . . ? Sm1 N1 C11 C12 -108.9(11) . . . . ? C8 N1 C11 Sm1 -72.5(8) . . . . ? C9 C10 C11 N1 2.7(16) . . . . ? Sm1 C10 C11 N1 -64.6(9) . . . . ? C9 C10 C11 C12 -179.0(13) . . . . ? Sm1 C10 C11 C12 113.6(14) . . . . ? C9 C10 C11 Sm1 67.3(9) . . . . ? C1 Sm1 C11 N1 34.7(9) . . . . ? O1 Sm1 C11 N1 -56.2(7) . . . . ? N1 Sm1 C11 N1 -155.9(10) 4_565 . . . ? C8 Sm1 C11 N1 129.0(10) 4_565 . . . ? C8 Sm1 C11 N1 39.7(7) . . . . ? C11 Sm1 C11 N1 -168.4(5) 4_565 . . . ? C9 Sm1 C11 N1 131.8(7) 4_565 . . . ? C9 Sm1 C11 N1 79.9(8) . . . . ? C10 Sm1 C11 N1 116.6(11) . . . . ? C10 Sm1 C11 N1 160.5(7) 4_565 . . . ? C1 Sm1 C11 C10 -82.0(9) . . . . ? O1 Sm1 C11 C10 -172.8(8) . . . . ? N1 Sm1 C11 C10 -116.6(11) . . . . ? N1 Sm1 C11 C10 87.4(11) 4_565 . . . ? C8 Sm1 C11 C10 12.4(15) 4_565 . . . ? C8 Sm1 C11 C10 -76.9(9) . . . . ? C11 Sm1 C11 C10 75.0(10) 4_565 . . . ? C9 Sm1 C11 C10 15.2(10) 4_565 . . . ? C9 Sm1 C11 C10 -36.7(7) . . . . ? C10 Sm1 C11 C10 43.9(8) 4_565 . . . ? C1 Sm1 C11 C12 150.1(9) . . . . ? O1 Sm1 C11 C12 59.3(9) . . . . ? N1 Sm1 C11 C12 115.5(12) . . . . ? N1 Sm1 C11 C12 -40.5(13) 4_565 . . . ? C8 Sm1 C11 C12 -115.5(11) 4_565 . . . ? C8 Sm1 C11 C12 155.2(11) . . . . ? C11 Sm1 C11 C12 -52.9(12) 4_565 . . . ? C9 Sm1 C11 C12 -112.7(9) 4_565 . . . ? C9 Sm1 C11 C12 -164.6(11) . . . . ? C10 Sm1 C11 C12 -127.9(13) . . . . ? C10 Sm1 C11 C12 -84.0(9) 4_565 . . . ? N1 C11 C12 C14 -41.9(17) . . . . ? C10 C11 C12 C14 140.0(15) . . . . ? Sm1 C11 C12 C14 -124.0(10) . . . . ? N1 C11 C12 C15 80.0(15) . . . . ? C10 C11 C12 C15 -98.1(16) . . . . ? Sm1 C11 C12 C15 -2.1(13) . . . . ? N1 C11 C12 C13 -161.3(13) . . . . ? C10 C11 C12 C13 21(2) . . . . ? Sm1 C11 C12 C13 116.6(11) . . . . ? C14 C12 C15 C17 0.8(18) . . . . ? C13 C12 C15 C17 122.9(13) . . . . ? C11 C12 C15 C17 -118.5(13) . . . . ? C14 C12 C15 C16 177.2(13) . . . . ? C13 C12 C15 C16 -60.7(16) . . . . ? C11 C12 C15 C16 58.0(16) . . . . ? C17 C15 C16 C15 7(2) . . . 4_565 ? C12 C15 C16 C15 -169.4(11) . . . 4_565 ? C17 C15 C16 Sm1 104.3(10) . . . . ? C12 C15 C16 Sm1 -72.5(12) . . . . ? O1 Sm1 C16 C15 -62.7(9) . . . . ? N1 Sm1 C16 C15 21.7(9) . . . . ? N1 Sm1 C16 C15 -147.0(10) 4_565 . . . ? C8 Sm1 C16 C15 -164.4(8) 4_565 . . . ? C8 Sm1 C16 C15 39.1(11) . . . . ? C11 Sm1 C16 C15 41.8(8) . . . . ? C11 Sm1 C16 C15 -167.1(11) 4_565 . . . ? C9 Sm1 C16 C15 165.0(9) 4_565 . . . ? C9 Sm1 C16 C15 69.7(10) . . . . ? C10 Sm1 C16 C15 71.3(9) . . . . ? C10 Sm1 C16 C15 163.3(10) 4_565 . . . ? O1 Sm1 C16 C15 62.7(9) . . . 4_565 ? N1 Sm1 C16 C15 147.0(10) . . . 4_565 ? N1 Sm1 C16 C15 -21.7(9) 4_565 . . 4_565 ? C8 Sm1 C16 C15 -39.1(11) 4_565 . . 4_565 ? C8 Sm1 C16 C15 164.4(8) . . . 4_565 ? C11 Sm1 C16 C15 167.1(11) . . . 4_565 ? C11 Sm1 C16 C15 -41.8(8) 4_565 . . 4_565 ? C9 Sm1 C16 C15 -69.7(10) 4_565 . . 4_565 ? C9 Sm1 C16 C15 -165.0(9) . . . 4_565 ? C10 Sm1 C16 C15 -163.3(10) . . . 4_565 ? C10 Sm1 C16 C15 -71.3(9) 4_565 . . 4_565 ? C16 C15 C17 C18 -4(2) . . . . ? C12 C15 C17 C18 173.0(15) . . . . ? C15 C17 C18 C17 0(3) . . . 4_565 ? C1 Sm1 O1 C19 -75.9(13) . . . . ? N1 Sm1 O1 C19 15.6(13) . . . . ? N1 Sm1 O1 C19 -167.3(13) 4_565 . . . ? C8 Sm1 O1 C19 -141.6(13) 4_565 . . . ? C8 Sm1 O1 C19 -10.1(14) . . . . ? C11 Sm1 O1 C19 40.5(14) . . . . ? C11 Sm1 O1 C19 167.8(13) 4_565 . . . ? C9 Sm1 O1 C19 -148.1(12) 4_565 . . . ? C9 Sm1 O1 C19 -3.6(15) . . . . ? C10 Sm1 O1 C19 35.7(15) . . . . ? C10 Sm1 O1 C19 172.6(12) 4_565 . . . ? C1 Sm1 O1 C19 75.9(13) . . . 4_565 ? N1 Sm1 O1 C19 167.3(13) . . . 4_565 ? N1 Sm1 O1 C19 -15.6(13) 4_565 . . 4_565 ? C8 Sm1 O1 C19 10.1(14) 4_565 . . 4_565 ? C8 Sm1 O1 C19 141.6(13) . . . 4_565 ? C11 Sm1 O1 C19 -167.8(13) . . . 4_565 ? C11 Sm1 O1 C19 -40.5(14) 4_565 . . 4_565 ? C9 Sm1 O1 C19 3.6(15) 4_565 . . 4_565 ? C9 Sm1 O1 C19 148.1(12) . . . 4_565 ? C10 Sm1 O1 C19 -172.6(12) . . . 4_565 ? C10 Sm1 O1 C19 -35.7(15) 4_565 . . 4_565 ? C19 O1 C19 C20 28(3) 4_565 . . . ? Sm1 O1 C19 C20 -175.7(11) . . . . ? O1 C19 C20 C20 -17.4(16) . . . 4_565 ? O2 Sm2 N2 C28 -127.2(7) . . . . ? C24 Sm2 N2 C28 -36.2(8) . . . . ? N2 Sm2 N2 C28 -146(2) 4_565 . . . ? C28 Sm2 N2 C28 -17.0(10) 4_565 . . . ? C31 Sm2 N2 C28 111.6(10) . . . . ? C31 Sm2 N2 C28 132.8(8) 4_565 . . . ? C29 Sm2 N2 C28 37.4(7) . . . . ? C29 Sm2 N2 C28 38.1(9) 4_565 . . . ? C30 Sm2 N2 C28 75.6(8) . . . . ? C30 Sm2 N2 C28 84.1(8) 4_565 . . . ? O2 Sm2 N2 C31 121.2(8) . . . . ? C24 Sm2 N2 C31 -147.8(8) . . . . ? N2 Sm2 N2 C31 103(2) 4_565 . . . ? C28 Sm2 N2 C31 -111.6(10) . . . . ? C28 Sm2 N2 C31 -128.6(10) 4_565 . . . ? C31 Sm2 N2 C31 21.3(8) 4_565 . . . ? C29 Sm2 N2 C31 -74.2(8) . . . . ? C29 Sm2 N2 C31 -73.4(9) 4_565 . . . ? C30 Sm2 N2 C31 -35.9(7) . . . . ? C30 Sm2 N2 C31 -27.5(9) 4_565 . . . ? C22 C21 C22 C23 -4(3) 4_565 . . . ? C21 C22 C23 C24 1(2) . . . . ? C21 C22 C23 C25 176.1(13) . . . . ? C22 C23 C24 C23 1(2) . . . 4_565 ? C25 C23 C24 C23 -173.8(10) . . . 4_565 ? C22 C23 C24 Sm2 -169.5(10) . . . . ? C25 C23 C24 Sm2 15.4(17) . . . . ? O2 Sm2 C24 C23 85.3(12) . . . . ? N2 Sm2 C24 C23 1.0(12) . . . . ? N2 Sm2 C24 C23 169.7(12) 4_565 . . . ? C28 Sm2 C24 C23 -17.7(11) . . . . ? C28 Sm2 C24 C23 -171.6(13) 4_565 . . . ? C31 Sm2 C24 C23 -16.4(14) . . . . ? C31 Sm2 C24 C23 -173.0(10) 4_565 . . . ? C29 Sm2 C24 C23 -47.9(12) . . . . ? C29 Sm2 C24 C23 -141.4(13) 4_565 . . . ? C30 Sm2 C24 C23 -47.4(13) . . . . ? C30 Sm2 C24 C23 -141.9(11) 4_565 . . . ? O2 Sm2 C24 C23 -85.3(12) . . . 4_565 ? N2 Sm2 C24 C23 -169.7(12) . . . 4_565 ? N2 Sm2 C24 C23 -1.0(12) 4_565 . . 4_565 ? C28 Sm2 C24 C23 171.6(13) . . . 4_565 ? C28 Sm2 C24 C23 17.7(11) 4_565 . . 4_565 ? C31 Sm2 C24 C23 173.0(10) . . . 4_565 ? C31 Sm2 C24 C23 16.4(14) 4_565 . . 4_565 ? C29 Sm2 C24 C23 141.4(13) . . . 4_565 ? C29 Sm2 C24 C23 47.9(12) 4_565 . . 4_565 ? C30 Sm2 C24 C23 141.9(11) . . . 4_565 ? C30 Sm2 C24 C23 47.4(13) 4_565 . . 4_565 ? C22 C23 C25 C28 -171.8(12) . . . . ? C24 C23 C25 C28 3.1(18) . . . . ? C22 C23 C25 C26 63.9(16) . . . . ? C24 C23 C25 C26 -121.2(14) . . . . ? C22 C23 C25 C27 -50.0(17) . . . . ? C24 C23 C25 C27 125.0(14) . . . . ? C31 N2 C28 C29 2.3(14) . . . . ? Sm2 N2 C28 C29 -71.7(10) . . . . ? C31 N2 C28 C25 -178.5(13) . . . . ? Sm2 N2 C28 C25 107.5(13) . . . . ? C31 N2 C28 Sm2 74.0(8) . . . . ? C23 C25 C28 N2 -103.1(15) . . . . ? C26 C25 C28 N2 20(2) . . . . ? C27 C25 C28 N2 135.7(14) . . . . ? C23 C25 C28 C29 76.0(17) . . . . ? C26 C25 C28 C29 -160.7(14) . . . . ? C27 C25 C28 C29 -45.2(19) . . . . ? C23 C25 C28 Sm2 -17.9(14) . . . . ? C26 C25 C28 Sm2 105.3(12) . . . . ? C27 C25 C28 Sm2 -139.1(10) . . . . ? O2 Sm2 C28 N2 54.3(7) . . . . ? C24 Sm2 C28 N2 140.4(8) . . . . ? N2 Sm2 C28 N2 161.2(11) 4_565 . . . ? C28 Sm2 C28 N2 172.1(5) 4_565 . . . ? C31 Sm2 C28 N2 -38.0(6) . . . . ? C31 Sm2 C28 N2 -112.5(11) 4_565 . . . ? C29 Sm2 C28 N2 -113.9(11) . . . . ? C29 Sm2 C28 N2 -154.9(6) 4_565 . . . ? C30 Sm2 C28 N2 -77.9(7) . . . . ? C30 Sm2 C28 N2 -123.5(7) 4_565 . . . ? O2 Sm2 C28 C29 168.2(8) . . . . ? C24 Sm2 C28 C29 -105.7(9) . . . . ? N2 Sm2 C28 C29 113.9(11) . . . . ? N2 Sm2 C28 C29 -84.9(12) 4_565 . . . ? C28 Sm2 C28 C29 -73.9(10) 4_565 . . . ? C31 Sm2 C28 C29 76.0(8) . . . . ? C31 Sm2 C28 C29 1.5(15) 4_565 . . . ? C29 Sm2 C28 C29 -40.9(8) 4_565 . . . ? C30 Sm2 C28 C29 36.1(8) . . . . ? C30 Sm2 C28 C29 -9.5(10) 4_565 . . . ? O2 Sm2 C28 C25 -67.6(10) . . . . ? C24 Sm2 C28 C25 18.5(9) . . . . ? N2 Sm2 C28 C25 -121.9(12) . . . . ? N2 Sm2 C28 C25 39.3(15) 4_565 . . . ? C28 Sm2 C28 C25 50.2(12) 4_565 . . . ? C31 Sm2 C28 C25 -159.8(11) . . . . ? C31 Sm2 C28 C25 125.7(11) 4_565 . . . ? C29 Sm2 C28 C25 124.2(14) . . . . ? C29 Sm2 C28 C25 83.3(10) 4_565 . . . ? C30 Sm2 C28 C25 160.3(11) . . . . ? C30 Sm2 C28 C25 114.6(9) 4_565 . . . ? N2 C28 C29 C30 -1.7(15) . . . . ? C25 C28 C29 C30 179.1(13) . . . . ? Sm2 C28 C29 C30 -68.9(10) . . . . ? N2 C28 C29 Sm2 67.2(9) . . . . ? C25 C28 C29 Sm2 -112.0(14) . . . . ? O2 Sm2 C29 C30 97.8(9) . . . . ? C24 Sm2 C29 C30 179.0(9) . . . . ? N2 Sm2 C29 C30 76.8(9) . . . . ? N2 Sm2 C29 C30 -102.2(9) 4_565 . . . ? C28 Sm2 C29 C30 113.5(12) . . . . ? C28 Sm2 C29 C30 -122.3(8) 4_565 . . . ? C31 Sm2 C29 C30 37.2(7) . . . . ? C31 Sm2 C29 C30 -65.8(9) 4_565 . . . ? C29 Sm2 C29 C30 -102.7(8) 4_565 . . . ? C30 Sm2 C29 C30 -74.1(9) 4_565 . . . ? O2 Sm2 C29 C28 -15.7(11) . . . . ? C24 Sm2 C29 C28 65.5(8) . . . . ? N2 Sm2 C29 C28 -36.7(7) . . . . ? N2 Sm2 C29 C28 144.3(8) 4_565 . . . ? C28 Sm2 C29 C28 124.1(10) 4_565 . . . ? C31 Sm2 C29 C28 -76.3(9) . . . . ? C31 Sm2 C29 C28 -179.3(7) 4_565 . . . ? C29 Sm2 C29 C28 143.7(7) 4_565 . . . ? C30 Sm2 C29 C28 -113.5(12) . . . . ? C30 Sm2 C29 C28 172.4(8) 4_565 . . . ? C28 C29 C30 C31 0.5(15) . . . . ? Sm2 C29 C30 C31 -63.5(9) . . . . ? C28 C29 C30 Sm2 64.1(9) . . . . ? O2 Sm2 C30 C29 -108.4(9) . . . . ? C24 Sm2 C30 C29 -1.0(9) . . . . ? N2 Sm2 C30 C29 -78.2(9) . . . . ? N2 Sm2 C30 C29 113.8(9) 4_565 . . . ? C28 Sm2 C30 C29 -38.1(8) . . . . ? C28 Sm2 C30 C29 74.5(9) 4_565 . . . ? C31 Sm2 C30 C29 -114.1(12) . . . . ? C31 Sm2 C30 C29 128.1(8) 4_565 . . . ? C29 Sm2 C30 C29 79.4(9) 4_565 . . . ? C30 Sm2 C30 C29 107.4(8) 4_565 . . . ? O2 Sm2 C30 C31 5.7(10) . . . . ? C24 Sm2 C30 C31 113.0(8) . . . . ? N2 Sm2 C30 C31 35.9(7) . . . . ? N2 Sm2 C30 C31 -132.1(7) 4_565 . . . ? C28 Sm2 C30 C31 76.0(8) . . . . ? C28 Sm2 C30 C31 -171.4(7) 4_565 . . . ? C31 Sm2 C30 C31 -117.8(9) 4_565 . . . ? C29 Sm2 C30 C31 114.1(11) . . . . ? C29 Sm2 C30 C31 -166.5(7) 4_565 . . . ? C30 Sm2 C30 C31 -138.5(6) 4_565 . . . ? C28 N2 C31 C30 -2.0(14) . . . . ? Sm2 N2 C31 C30 70.6(10) . . . . ? C28 N2 C31 C32 177.7(12) . . . . ? Sm2 N2 C31 C32 -109.8(11) . . . . ? C28 N2 C31 Sm2 -72.6(8) . . . . ? C29 C30 C31 N2 0.9(15) . . . . ? Sm2 C30 C31 N2 -64.9(9) . . . . ? C29 C30 C31 C32 -178.7(13) . . . . ? Sm2 C30 C31 C32 115.5(14) . . . . ? C29 C30 C31 Sm2 65.8(9) . . . . ? O2 Sm2 C31 N2 -59.7(7) . . . . ? C24 Sm2 C31 N2 36.7(9) . . . . ? N2 Sm2 C31 N2 -155.6(10) 4_565 . . . ? C28 Sm2 C31 N2 38.4(7) . . . . ? C28 Sm2 C31 N2 133.4(11) 4_565 . . . ? C31 Sm2 C31 N2 -167.9(5) 4_565 . . . ? C29 Sm2 C31 N2 79.6(8) . . . . ? C29 Sm2 C31 N2 132.5(7) 4_565 . . . ? C30 Sm2 C31 N2 115.8(11) . . . . ? C30 Sm2 C31 N2 160.9(7) 4_565 . . . ? O2 Sm2 C31 C30 -175.5(8) . . . . ? C24 Sm2 C31 C30 -79.1(9) . . . . ? N2 Sm2 C31 C30 -115.8(11) . . . . ? N2 Sm2 C31 C30 88.6(10) 4_565 . . . ? C28 Sm2 C31 C30 -77.4(8) . . . . ? C28 Sm2 C31 C30 17.6(14) 4_565 . . . ? C31 Sm2 C31 C30 76.3(9) 4_565 . . . ? C29 Sm2 C31 C30 -36.2(7) . . . . ? C29 Sm2 C31 C30 16.7(9) 4_565 . . . ? C30 Sm2 C31 C30 45.1(7) 4_565 . . . ? O2 Sm2 C31 C32 56.3(9) . . . . ? C24 Sm2 C31 C32 152.8(9) . . . . ? N2 Sm2 C31 C32 116.1(12) . . . . ? N2 Sm2 C31 C32 -39.5(13) 4_565 . . . ? C28 Sm2 C31 C32 154.5(11) . . . . ? C28 Sm2 C31 C32 -110.5(12) 4_565 . . . ? C31 Sm2 C31 C32 -51.8(11) 4_565 . . . ? C29 Sm2 C31 C32 -164.3(11) . . . . ? C29 Sm2 C31 C32 -111.4(9) 4_565 . . . ? C30 Sm2 C31 C32 -128.1(13) . . . . ? C30 Sm2 C31 C32 -83.0(9) 4_565 . . . ? N2 C31 C32 C34 -38.9(17) . . . . ? C30 C31 C32 C34 140.7(14) . . . . ? Sm2 C31 C32 C34 -121.5(11) . . . . ? N2 C31 C32 C35 84.6(14) . . . . ? C30 C31 C32 C35 -95.8(16) . . . . ? Sm2 C31 C32 C35 2.1(13) . . . . ? N2 C31 C32 C33 -157.3(12) . . . . ? C30 C31 C32 C33 22.3(18) . . . . ? Sm2 C31 C32 C33 120.2(10) . . . . ? C34 C32 C35 C36 -9.2(18) . . . . ? C31 C32 C35 C36 -130.5(13) . . . . ? C33 C32 C35 C36 111.2(15) . . . . ? C34 C32 C35 C38 171.4(13) . . . . ? C31 C32 C35 C38 50.0(17) . . . . ? C33 C32 C35 C38 -68.2(17) . . . . ? C38 C35 C36 C37 -5(2) . . . . ? C32 C35 C36 C37 175.1(14) . . . . ? C35 C36 C37 C36 -1(3) . . . 4_565 ? C36 C35 C38 C35 13(3) . . . 4_565 ? C32 C35 C38 C35 -168.0(11) . . . 4_565 ? C36 C35 C38 Sm2 114.6(11) . . . . ? C32 C35 C38 Sm2 -66.0(13) . . . . ? O2 Sm2 C38 C35 -62.2(10) . . . . ? N2 Sm2 C38 C35 22.2(10) . . . . ? N2 Sm2 C38 C35 -146.7(10) 4_565 . . . ? C28 Sm2 C38 C35 39.4(11) . . . . ? C28 Sm2 C38 C35 -163.9(9) 4_565 . . . ? C31 Sm2 C38 C35 41.2(9) . . . . ? C31 Sm2 C38 C35 -165.7(12) 4_565 . . . ? C29 Sm2 C38 C35 70.4(11) . . . . ? C29 Sm2 C38 C35 165.1(10) 4_565 . . . ? C30 Sm2 C38 C35 71.3(9) . . . . ? C30 Sm2 C38 C35 164.2(11) 4_565 . . . ? O2 Sm2 C38 C35 62.2(10) . . . 4_565 ? N2 Sm2 C38 C35 146.7(10) . . . 4_565 ? N2 Sm2 C38 C35 -22.2(10) 4_565 . . 4_565 ? C28 Sm2 C38 C35 163.9(9) . . . 4_565 ? C28 Sm2 C38 C35 -39.4(11) 4_565 . . 4_565 ? C31 Sm2 C38 C35 165.7(12) . . . 4_565 ? C31 Sm2 C38 C35 -41.2(9) 4_565 . . 4_565 ? C29 Sm2 C38 C35 -165.1(10) . . . 4_565 ? C29 Sm2 C38 C35 -70.4(11) 4_565 . . 4_565 ? C30 Sm2 C38 C35 -164.2(11) . . . 4_565 ? C30 Sm2 C38 C35 -71.3(10) 4_565 . . 4_565 ? C24 Sm2 O2 C39 -89.2(19) . . . . ? N2 Sm2 O2 C39 2.7(18) . . . . ? N2 Sm2 O2 C39 178.9(19) 4_565 . . . ? C28 Sm2 O2 C39 -21.6(19) . . . . ? C28 Sm2 O2 C39 -156.8(18) 4_565 . . . ? C31 Sm2 O2 C39 28.4(19) . . . . ? C31 Sm2 O2 C39 153.2(18) 4_565 . . . ? C29 Sm2 O2 C39 -13(2) . . . . ? C29 Sm2 O2 C39 -165.0(17) 4_565 . . . ? C30 Sm2 O2 C39 26(2) . . . . ? C30 Sm2 O2 C39 156.1(17) 4_565 . . . ? C24 Sm2 O2 C39 89.2(19) . . . 4_565 ? N2 Sm2 O2 C39 -178.9(19) . . . 4_565 ? N2 Sm2 O2 C39 -2.7(18) 4_565 . . 4_565 ? C28 Sm2 O2 C39 156.8(18) . . . 4_565 ? C28 Sm2 O2 C39 21.6(19) 4_565 . . 4_565 ? C31 Sm2 O2 C39 -153.2(18) . . . 4_565 ? C31 Sm2 O2 C39 -28.4(19) 4_565 . . 4_565 ? C29 Sm2 O2 C39 165.0(17) . . . 4_565 ? C29 Sm2 O2 C39 13(2) 4_565 . . 4_565 ? C30 Sm2 O2 C39 -156.1(17) . . . 4_565 ? C30 Sm2 O2 C39 -26(2) 4_565 . . 4_565 ? C39 O2 C39 C40 1(4) 4_565 . . . ? Sm2 O2 C39 C40 -179.7(16) . . . . ? O2 C39 C40 C40 -1(2) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 23.44 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 3.361 _refine_diff_density_min -1.272 _refine_diff_density_rms 0.193 #===END # Attachment '331_web_deposit_cif_file_2_BVidjayacoumar_1264555817.cif' data_sg3418 _database_code_depnum_ccdc_archive 'CCDC 763510' #TrackingRef '331_web_deposit_cif_file_2_BVidjayacoumar_1264555817.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H73 N4 Sm' _chemical_formula_weight 1048.61 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.057(3) _cell_length_b 16.189(3) _cell_length_c 25.081(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.507(2) _cell_angle_gamma 90.00 _cell_volume 5267.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 721 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 23.28 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2188 _exptl_absorpt_coefficient_mu 1.159 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8013 _exptl_absorpt_correction_T_max 0.8454 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 17054 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 23.28 _reflns_number_total 7446 _reflns_number_gt 6893 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2000)' _computing_cell_refinement 'SMART, Bruker (2000)' _computing_data_reduction 'XPREP, Bruker (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2000)' _computing_publication_material 'SHELXTL, Bruker (2000)' _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^)+(0.0366P)^2^]' _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 0.006(10) _refine_ls_number_reflns 7446 _refine_ls_number_parameters 622 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 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 0.050965(13) 0.434467(13) 0.460686(11) 0.02526(8) Uani 1 1 d . . . N1 N -0.0796(3) 0.4640(3) 0.38452(17) 0.0276(10) Uani 1 1 d . . . N2 N 0.2117(3) 0.3670(3) 0.44586(18) 0.0302(10) Uani 1 1 d . . . C1 C -0.0755(4) 0.5255(3) 0.3467(2) 0.0290(12) Uani 1 1 d . . . C2 C -0.1682(4) 0.5352(3) 0.3171(2) 0.0380(14) Uani 1 1 d . . . H2A H -0.1847 0.5738 0.2895 0.046 Uiso 1 1 calc R . . C3 C -0.2348(4) 0.4767(4) 0.3356(2) 0.0377(14) Uani 1 1 d . . . H3A H -0.3045 0.4685 0.3226 0.045 Uiso 1 1 calc R . . C4 C -0.1805(4) 0.4341(3) 0.3755(2) 0.0286(12) Uani 1 1 d . . . C5 C -0.2201(4) 0.3630(3) 0.4075(2) 0.0298(12) Uani 1 1 d . . . C6 C -0.3026(4) 0.3954(4) 0.4423(3) 0.0452(15) Uani 1 1 d . . . H6A H -0.2722 0.4372 0.4669 0.068 Uiso 1 1 calc R . . H6B H -0.3276 0.3500 0.4625 0.068 Uiso 1 1 calc R . . H6C H -0.3596 0.4194 0.4192 0.068 Uiso 1 1 calc R . . C7 C -0.2728(4) 0.2969(3) 0.3688(2) 0.0410(14) Uani 1 1 d . . . H7A H -0.2233 0.2756 0.3462 0.061 Uiso 1 1 calc R . . H7B H -0.3302 0.3217 0.3466 0.061 Uiso 1 1 calc R . . H7C H -0.2977 0.2521 0.3896 0.061 Uiso 1 1 calc R . . C8 C -0.1303(4) 0.3219(3) 0.4412(2) 0.0277(12) Uani 1 1 d . . . C9 C -0.1217(4) 0.3187(4) 0.4963(2) 0.0284(14) Uani 1 1 d . . . H9A H -0.1750 0.3402 0.5144 0.034 Uiso 1 1 calc R . . C10 C -0.0348(4) 0.2838(3) 0.5260(2) 0.0321(13) Uani 1 1 d . . . H10A H -0.0297 0.2816 0.5637 0.039 Uiso 1 1 calc R . . C11 C 0.0432(5) 0.2529(4) 0.4989(2) 0.0280(15) Uani 1 1 d . . . H11A H 0.1014 0.2294 0.5187 0.034 Uiso 1 1 calc R . . C12 C 0.0386(5) 0.2551(4) 0.4441(2) 0.0320(18) Uani 1 1 d . . . C13 C -0.0489(4) 0.2883(3) 0.4149(2) 0.0270(12) Uani 1 1 d . . . H13A H -0.0541 0.2886 0.3772 0.032 Uiso 1 1 calc R . . C14 C 0.1336(4) 0.2277(4) 0.4170(2) 0.0318(12) Uani 1 1 d . . . C15 C 0.1193(5) 0.2371(4) 0.3567(2) 0.0448(15) Uani 1 1 d . . . H15A H 0.1815 0.2195 0.3421 0.067 Uiso 1 1 calc R . . H15B H 0.1055 0.2945 0.3475 0.067 Uiso 1 1 calc R . . H15C H 0.0618 0.2033 0.3417 0.067 Uiso 1 1 calc R . . C16 C 0.1571(5) 0.1370(4) 0.4313(3) 0.0526(17) Uani 1 1 d . . . H16A H 0.2167 0.1191 0.4145 0.079 Uiso 1 1 calc R . . H16B H 0.0981 0.1031 0.4185 0.079 Uiso 1 1 calc R . . H16C H 0.1714 0.1314 0.4699 0.079 Uiso 1 1 calc R . . C17 C 0.2215(4) 0.2811(4) 0.4420(3) 0.0350(15) Uani 1 1 d . . . C18 C 0.3228(5) 0.2596(4) 0.4571(3) 0.0551(18) Uani 1 1 d . . . H18A H 0.3507 0.2060 0.4583 0.066 Uiso 1 1 calc R . . C19 C 0.3761(5) 0.3331(5) 0.4702(3) 0.060(2) Uani 1 1 d . . . H19A H 0.4466 0.3374 0.4826 0.072 Uiso 1 1 calc R . . C20 C 0.3087(4) 0.3977(4) 0.4619(2) 0.0398(15) Uani 1 1 d . . . C21 C 0.3347(4) 0.4878(4) 0.4696(2) 0.0394(14) Uani 1 1 d . . . C22 C 0.3873(5) 0.5029(4) 0.5270(3) 0.0547(17) Uani 1 1 d . . . H22A H 0.4492 0.4694 0.5331 0.082 Uiso 1 1 calc R . . H22B H 0.3404 0.4880 0.5527 0.082 Uiso 1 1 calc R . . H22C H 0.4056 0.5608 0.5312 0.082 Uiso 1 1 calc R . . C23 C 0.4113(5) 0.5157(5) 0.4316(3) 0.064(2) Uani 1 1 d . . . H23A H 0.3819 0.5068 0.3948 0.096 Uiso 1 1 calc R . . H23B H 0.4745 0.4840 0.4387 0.096 Uiso 1 1 calc R . . H23C H 0.4263 0.5739 0.4372 0.096 Uiso 1 1 calc R . . C24 C 0.2371(4) 0.5390(4) 0.4582(2) 0.0362(14) Uani 1 1 d . . . C25 C 0.1922(5) 0.5843(4) 0.4964(2) 0.0399(15) Uani 1 1 d . . . H25A H 0.2244 0.5870 0.5318 0.048 Uiso 1 1 calc R . . C26 C 0.1003(5) 0.6255(4) 0.4824(3) 0.0352(17) Uani 1 1 d . . . H26A H 0.0729 0.6586 0.5082 0.042 Uiso 1 1 calc R . . C27 C 0.0485(5) 0.6194(4) 0.4322(3) 0.0358(17) Uani 1 1 d . . . H27A H -0.0156 0.6458 0.4245 0.043 Uiso 1 1 calc R . . C28 C 0.0895(4) 0.5742(3) 0.3918(2) 0.0302(12) Uani 1 1 d . . . C29 C 0.1835(4) 0.5359(3) 0.4055(2) 0.0276(12) Uani 1 1 d . . . H29A H 0.2132 0.5064 0.3789 0.033 Uiso 1 1 calc R . . C30 C 0.0287(4) 0.5641(3) 0.3372(2) 0.0313(12) Uani 1 1 d . . . C31 C 0.0104(5) 0.6498(4) 0.3108(2) 0.0459(16) Uani 1 1 d . . . H31A H 0.0761 0.6741 0.3049 0.069 Uiso 1 1 calc R . . H31B H -0.0242 0.6853 0.3342 0.069 Uiso 1 1 calc R . . H31C H -0.0320 0.6438 0.2767 0.069 Uiso 1 1 calc R . . C32 C 0.0809(4) 0.5089(4) 0.2991(2) 0.0379(14) Uani 1 1 d . . . H32A H 0.0927 0.4547 0.3151 0.057 Uiso 1 1 calc R . . H32B H 0.1463 0.5331 0.2926 0.057 Uiso 1 1 calc R . . H32C H 0.0369 0.5037 0.2654 0.057 Uiso 1 1 calc R . . N3 N 0.0471(3) 0.4603(2) 0.55286(16) 0.0264(10) Uani 1 1 d . . . N4 N 0.2643(3) 0.6562(3) 0.69523(17) 0.0310(10) Uani 1 1 d . . . H4A H 0.2393 0.6426 0.7247 0.037 Uiso 1 1 calc R . . C34 C 0.0424(4) 0.4172(3) 0.6374(2) 0.0259(12) Uani 1 1 d . . . H34A H 0.0203 0.4096 0.6715 0.031 Uiso 1 1 calc R . . C33 C -0.0076(4) 0.4630(3) 0.5963(2) 0.0261(12) Uani 1 1 d . . . C35 C 0.1328(4) 0.3833(3) 0.61989(19) 0.0238(11) Uani 1 1 d . . . C36 C 0.1334(4) 0.4126(3) 0.5691(2) 0.0280(12) Uani 1 1 d . . . H36A H 0.1862 0.4018 0.5475 0.034 Uiso 1 1 calc R . . C37 C 0.2101(4) 0.3274(3) 0.6513(2) 0.0282(12) Uani 1 1 d . . . C38 C 0.2902(4) 0.2971(4) 0.6148(2) 0.0387(14) Uani 1 1 d . . . H38A H 0.3288 0.3439 0.6035 0.058 Uiso 1 1 calc R . . H38B H 0.2550 0.2699 0.5835 0.058 Uiso 1 1 calc R . . H38C H 0.3370 0.2584 0.6345 0.058 Uiso 1 1 calc R . . C39 C 0.1514(4) 0.2508(3) 0.6681(2) 0.0394(14) Uani 1 1 d . . . H39A H 0.1007 0.2676 0.6914 0.059 Uiso 1 1 calc R . . H39B H 0.1997 0.2125 0.6872 0.059 Uiso 1 1 calc R . . H39C H 0.1169 0.2240 0.6364 0.059 Uiso 1 1 calc R . . C40 C 0.2683(4) 0.3730(3) 0.6985(2) 0.0249(12) Uani 1 1 d . . . C41 C 0.2863(4) 0.3391(3) 0.7498(2) 0.0299(12) Uani 1 1 d . . . H41A H 0.2571 0.2877 0.7568 0.036 Uiso 1 1 calc R . . C42 C 0.3457(4) 0.3793(3) 0.7902(2) 0.0372(14) Uani 1 1 d . . . H42A H 0.3566 0.3554 0.8245 0.045 Uiso 1 1 calc R . . C43 C 0.3894(4) 0.4543(3) 0.7809(2) 0.0359(14) Uani 1 1 d . . . H43A H 0.4316 0.4805 0.8088 0.043 Uiso 1 1 calc R . . C44 C 0.3720(4) 0.4919(3) 0.7311(2) 0.0327(13) Uani 1 1 d . . . C45 C 0.3108(4) 0.4501(3) 0.6913(2) 0.0310(13) Uani 1 1 d . . . H45A H 0.2972 0.4754 0.6575 0.037 Uiso 1 1 calc R . . C46 C 0.4261(4) 0.5728(3) 0.7178(3) 0.0401(14) Uani 1 1 d . . . C47 C 0.4629(6) 0.6230(4) 0.7677(3) 0.059(2) Uani 1 1 d . . . H47A H 0.4043 0.6382 0.7861 0.089 Uiso 1 1 calc R . . H47B H 0.4974 0.6725 0.7572 0.089 Uiso 1 1 calc R . . H47C H 0.5106 0.5902 0.7914 0.089 Uiso 1 1 calc R . . C48 C 0.5202(5) 0.5489(4) 0.6889(3) 0.061(2) Uani 1 1 d . . . H48A H 0.5561 0.5985 0.6799 0.091 Uiso 1 1 calc R . . H48B H 0.4971 0.5187 0.6563 0.091 Uiso 1 1 calc R . . H48C H 0.5665 0.5144 0.7123 0.091 Uiso 1 1 calc R . . C49 C 0.3550(4) 0.6270(3) 0.6806(2) 0.0342(13) Uani 1 1 d . . . C50 C 0.3667(4) 0.6620(3) 0.6320(2) 0.0386(14) Uani 1 1 d . . . H50A H 0.4222 0.6537 0.6118 0.046 Uiso 1 1 calc R . . C51 C 0.2795(4) 0.7133(3) 0.6176(2) 0.0377(14) Uani 1 1 d . . . H51A H 0.2670 0.7442 0.5859 0.045 Uiso 1 1 calc R . . C52 C 0.2173(4) 0.7102(3) 0.6573(2) 0.0288(12) Uani 1 1 d . . . C53 C 0.1200(4) 0.7561(3) 0.6659(2) 0.0309(12) Uani 1 1 d . . . C54 C 0.1459(5) 0.8179(3) 0.7121(2) 0.0438(15) Uani 1 1 d . . . H54A H 0.1992 0.8554 0.7031 0.066 Uiso 1 1 calc R . . H54B H 0.1702 0.7880 0.7447 0.066 Uiso 1 1 calc R . . H54C H 0.0846 0.8491 0.7178 0.066 Uiso 1 1 calc R . . C55 C 0.0819(4) 0.8052(4) 0.6156(2) 0.0427(14) Uani 1 1 d . . . H55A H 0.1345 0.8443 0.6079 0.064 Uiso 1 1 calc R . . H55B H 0.0195 0.8347 0.6214 0.064 Uiso 1 1 calc R . . H55C H 0.0675 0.7676 0.5855 0.064 Uiso 1 1 calc R . . C56 C 0.0349(4) 0.6941(3) 0.6776(2) 0.0285(12) Uani 1 1 d . . . C57 C -0.0152(4) 0.6980(4) 0.7233(2) 0.0366(13) Uani 1 1 d . . . H57A H 0.0035 0.7384 0.7496 0.044 Uiso 1 1 calc R . . C58 C -0.0941(5) 0.6412(3) 0.7303(2) 0.0344(13) Uani 1 1 d . . . H58A H -0.1267 0.6422 0.7619 0.041 Uiso 1 1 calc R . . C59 C -0.1237(4) 0.5840(3) 0.6907(2) 0.0325(13) Uani 1 1 d . . . H59A H -0.1782 0.5476 0.6952 0.039 Uiso 1 1 calc R . . C60 C -0.0753(4) 0.5790(3) 0.6448(2) 0.0259(11) Uani 1 1 d . . . C61 C 0.0051(4) 0.6337(3) 0.6400(2) 0.0299(12) Uani 1 1 d . . . H61A H 0.0412 0.6294 0.6098 0.036 Uiso 1 1 calc R . . C62 C -0.1027(4) 0.5156(3) 0.5997(2) 0.0297(12) Uani 1 1 d . . . C63 C -0.1930(4) 0.4605(4) 0.6121(3) 0.0409(14) Uani 1 1 d . . . H63A H -0.2092 0.4214 0.5830 0.061 Uiso 1 1 calc R . . H63B H -0.2529 0.4946 0.6157 0.061 Uiso 1 1 calc R . . H63C H -0.1739 0.4307 0.6453 0.061 Uiso 1 1 calc R . . C64 C -0.1348(4) 0.5602(3) 0.5472(2) 0.0383(14) Uani 1 1 d . . . H64A H -0.0789 0.5952 0.5384 0.057 Uiso 1 1 calc R . . H64B H -0.1952 0.5938 0.5507 0.057 Uiso 1 1 calc R . . H64C H -0.1510 0.5200 0.5188 0.057 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 0.02309(12) 0.02984(12) 0.02243(12) 0.0000(2) 0.00079(8) -0.00137(19) N1 0.023(2) 0.028(2) 0.031(2) 0.002(2) -0.0027(19) 0.0030(19) N2 0.020(2) 0.043(3) 0.027(3) 0.002(2) 0.004(2) -0.003(2) C1 0.032(3) 0.023(3) 0.031(3) 0.000(2) 0.000(2) 0.000(2) C2 0.036(3) 0.038(3) 0.037(3) 0.006(3) -0.010(3) 0.006(3) C3 0.022(3) 0.047(3) 0.043(4) 0.006(3) -0.003(3) 0.002(3) C4 0.029(3) 0.026(3) 0.030(3) -0.003(2) 0.003(2) 0.002(2) C5 0.026(3) 0.030(3) 0.033(3) -0.004(2) 0.002(2) -0.002(2) C6 0.025(3) 0.051(4) 0.060(4) 0.005(3) 0.005(3) 0.009(3) C7 0.037(3) 0.033(3) 0.050(4) -0.001(3) -0.009(3) -0.005(3) C8 0.029(3) 0.025(3) 0.029(3) 0.002(3) 0.007(2) -0.012(2) C9 0.023(3) 0.034(4) 0.031(4) -0.005(3) 0.015(3) 0.001(3) C10 0.041(3) 0.034(3) 0.021(3) 0.007(3) 0.001(3) 0.000(3) C11 0.028(4) 0.025(3) 0.031(3) 0.005(3) -0.001(3) -0.002(3) C12 0.026(4) 0.030(3) 0.041(5) -0.001(3) 0.009(4) -0.003(3) C13 0.034(3) 0.025(3) 0.022(3) 0.001(2) 0.004(2) -0.003(2) C14 0.031(3) 0.034(3) 0.031(3) 0.000(3) 0.007(2) 0.008(3) C15 0.043(4) 0.051(4) 0.042(4) -0.001(3) 0.012(3) 0.011(3) C16 0.040(4) 0.035(3) 0.084(5) -0.004(3) 0.013(3) 0.007(3) C17 0.027(3) 0.031(3) 0.049(4) -0.004(3) 0.013(3) -0.004(3) C18 0.036(4) 0.053(4) 0.075(5) 0.002(4) 0.002(3) 0.016(3) C19 0.030(4) 0.068(5) 0.079(5) 0.014(4) -0.002(4) -0.005(4) C20 0.029(3) 0.062(4) 0.029(3) 0.003(3) 0.007(3) 0.003(3) C21 0.029(3) 0.049(4) 0.039(3) 0.005(3) -0.001(3) -0.012(3) C22 0.046(4) 0.064(4) 0.050(4) 0.003(3) -0.011(3) -0.005(3) C23 0.026(3) 0.077(5) 0.088(6) 0.034(4) 0.006(3) 0.001(3) C24 0.035(3) 0.048(4) 0.025(3) 0.002(3) 0.004(3) -0.021(3) C25 0.041(3) 0.044(4) 0.035(3) 0.000(3) 0.001(3) -0.021(3) C26 0.046(5) 0.036(3) 0.025(4) -0.005(3) 0.009(3) -0.002(3) C27 0.033(4) 0.026(3) 0.050(4) 0.005(3) 0.012(3) -0.004(3) C28 0.034(3) 0.027(3) 0.030(3) 0.001(2) 0.005(2) -0.008(3) C29 0.031(3) 0.030(3) 0.023(3) 0.002(2) 0.006(2) -0.006(2) C30 0.032(3) 0.032(3) 0.029(3) 0.007(2) -0.001(2) -0.003(3) C31 0.053(4) 0.041(3) 0.042(4) 0.016(3) -0.001(3) -0.010(3) C32 0.036(3) 0.060(4) 0.019(3) 0.003(3) 0.006(3) -0.006(3) N3 0.027(2) 0.031(2) 0.021(2) 0.0004(18) 0.0022(19) -0.0047(19) N4 0.032(3) 0.030(2) 0.031(3) 0.007(2) 0.006(2) -0.004(2) C34 0.027(3) 0.025(3) 0.026(3) 0.001(2) 0.005(2) -0.001(2) C33 0.027(3) 0.025(3) 0.026(3) -0.004(2) 0.004(2) -0.004(2) C35 0.028(3) 0.018(3) 0.025(3) 0.001(2) 0.001(2) -0.009(2) C36 0.021(3) 0.031(3) 0.031(3) -0.004(2) 0.003(2) 0.004(2) C37 0.028(3) 0.022(3) 0.034(3) 0.003(2) 0.003(2) -0.003(2) C38 0.034(3) 0.043(3) 0.038(3) -0.004(3) -0.001(3) 0.009(3) C39 0.038(3) 0.031(3) 0.045(4) 0.005(3) -0.009(3) -0.002(3) C40 0.017(3) 0.020(3) 0.037(3) 0.001(2) 0.001(2) 0.000(2) C41 0.035(3) 0.029(3) 0.027(3) 0.007(2) 0.008(2) -0.002(2) C42 0.042(3) 0.038(4) 0.031(3) 0.002(3) 0.001(3) 0.007(3) C43 0.037(3) 0.032(3) 0.036(3) -0.005(2) -0.005(3) 0.004(3) C44 0.024(3) 0.033(3) 0.040(3) 0.001(3) -0.003(3) 0.000(2) C45 0.028(3) 0.031(3) 0.033(3) 0.010(2) -0.003(2) 0.002(2) C46 0.028(3) 0.030(3) 0.060(4) 0.002(3) -0.004(3) -0.007(3) C47 0.061(4) 0.027(3) 0.082(5) -0.003(3) -0.029(4) -0.009(3) C48 0.030(3) 0.037(4) 0.115(6) 0.012(4) 0.004(4) -0.004(3) C49 0.025(3) 0.026(3) 0.050(4) -0.004(3) -0.001(3) -0.004(2) C50 0.040(3) 0.032(3) 0.046(4) 0.004(3) 0.018(3) -0.002(3) C51 0.049(4) 0.027(3) 0.037(3) 0.003(2) 0.008(3) -0.006(3) C52 0.032(3) 0.023(3) 0.030(3) 0.000(2) -0.002(2) -0.008(2) C53 0.033(3) 0.025(3) 0.034(3) -0.002(2) 0.001(2) -0.006(2) C54 0.049(4) 0.030(3) 0.053(4) -0.005(3) 0.006(3) -0.010(3) C55 0.039(3) 0.034(3) 0.054(4) 0.010(3) 0.003(3) -0.003(3) C56 0.033(3) 0.026(3) 0.026(3) 0.000(2) 0.001(2) 0.006(2) C57 0.039(3) 0.035(3) 0.033(3) -0.001(3) -0.008(3) 0.004(3) C58 0.038(4) 0.040(3) 0.026(3) 0.004(3) 0.008(3) 0.009(3) C59 0.029(3) 0.026(3) 0.042(3) 0.004(3) 0.005(3) 0.002(2) C60 0.024(3) 0.019(3) 0.035(3) 0.002(2) 0.003(2) 0.002(2) C61 0.031(3) 0.030(3) 0.031(3) 0.000(2) 0.008(2) 0.001(2) C62 0.027(3) 0.025(3) 0.036(3) 0.001(2) -0.003(2) -0.003(2) C63 0.028(3) 0.042(3) 0.053(4) -0.010(3) 0.006(3) -0.008(3) C64 0.035(3) 0.040(3) 0.038(3) 0.003(3) -0.008(3) 0.004(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 N3 2.355(4) . ? Sm1 N2 2.431(5) . ? Sm1 N1 2.459(4) . ? Sm1 C36 2.831(5) . ? Sm1 C29 2.854(5) . ? Sm1 C13 2.876(5) . ? Sm1 C28 2.925(5) . ? Sm1 C12 2.935(6) . ? Sm1 C24 2.968(5) . ? Sm1 C8 2.983(5) . ? N1 C1 1.381(7) . ? N1 C4 1.397(6) . ? N2 C20 1.378(7) . ? N2 C17 1.401(8) . ? C1 C2 1.356(7) . ? C1 C30 1.539(7) . ? C2 C3 1.400(8) . ? C3 C4 1.349(7) . ? C4 C5 1.527(7) . ? C5 C8 1.518(7) . ? C5 C7 1.551(7) . ? C5 C6 1.553(8) . ? C8 C9 1.376(8) . ? C8 C13 1.421(7) . ? C9 C10 1.404(8) . ? C10 C11 1.382(8) . ? C11 C12 1.369(9) . ? C12 C13 1.392(8) . ? C12 C14 1.546(8) . ? C14 C15 1.511(8) . ? C14 C17 1.514(8) . ? C14 C16 1.535(8) . ? C17 C18 1.379(8) . ? C18 C19 1.398(10) . ? C19 C20 1.368(9) . ? C20 C21 1.504(9) . ? C21 C24 1.520(8) . ? C21 C23 1.524(8) . ? C21 C22 1.543(8) . ? C24 C25 1.389(8) . ? C24 C29 1.424(7) . ? C25 C26 1.383(9) . ? C26 C27 1.365(8) . ? C27 C28 1.403(8) . ? C28 C29 1.383(8) . ? C28 C30 1.513(7) . ? C30 C32 1.524(8) . ? C30 C31 1.543(7) . ? N3 C33 1.369(6) . ? N3 C36 1.389(6) . ? N4 C49 1.363(7) . ? N4 C52 1.384(6) . ? C34 C33 1.374(7) . ? C34 C35 1.417(7) . ? C33 C62 1.517(7) . ? C35 C36 1.361(7) . ? C35 C37 1.509(7) . ? C37 C40 1.523(7) . ? C37 C39 1.541(7) . ? C37 C38 1.545(7) . ? C40 C45 1.387(7) . ? C40 C41 1.395(7) . ? C41 C42 1.368(8) . ? C42 C43 1.372(8) . ? C43 C44 1.386(8) . ? C44 C45 1.382(7) . ? C44 C46 1.541(7) . ? C46 C49 1.520(8) . ? C46 C47 1.523(9) . ? C46 C48 1.545(9) . ? C49 C50 1.368(8) . ? C50 C51 1.422(8) . ? C51 C52 1.353(7) . ? C52 C53 1.509(7) . ? C53 C55 1.526(8) . ? C53 C54 1.539(8) . ? C53 C56 1.548(7) . ? C56 C61 1.383(7) . ? C56 C57 1.385(8) . ? C57 C58 1.407(8) . ? C58 C59 1.380(8) . ? C59 C60 1.378(8) . ? C60 C61 1.389(7) . ? C60 C62 1.538(7) . ? C62 C64 1.519(7) . ? C62 C63 1.538(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Sm1 N2 110.17(15) . . ? N3 Sm1 N1 129.62(14) . . ? N2 Sm1 N1 120.20(15) . . ? N3 Sm1 C36 29.28(14) . . ? N2 Sm1 C36 81.36(15) . . ? N1 Sm1 C36 157.70(14) . . ? N3 Sm1 C29 117.09(14) . . ? N2 Sm1 C29 66.62(15) . . ? N1 Sm1 C29 85.22(14) . . ? C36 Sm1 C29 110.61(15) . . ? N3 Sm1 C13 118.59(14) . . ? N2 Sm1 C13 85.95(15) . . ? N1 Sm1 C13 66.84(14) . . ? C36 Sm1 C13 112.72(14) . . ? C29 Sm1 C13 123.49(15) . . ? N3 Sm1 C28 117.82(14) . . ? N2 Sm1 C28 92.75(15) . . ? N1 Sm1 C28 62.70(14) . . ? C36 Sm1 C28 126.29(14) . . ? C29 Sm1 C28 27.66(15) . . ? C13 Sm1 C28 120.06(14) . . ? N3 Sm1 C12 107.94(15) . . ? N2 Sm1 C12 64.44(17) . . ? N1 Sm1 C12 93.42(16) . . ? C36 Sm1 C12 91.23(15) . . ? C29 Sm1 C12 121.79(16) . . ? C13 Sm1 C12 27.70(16) . . ? C28 Sm1 C12 133.77(16) . . ? N3 Sm1 C24 91.63(14) . . ? N2 Sm1 C24 61.96(16) . . ? N1 Sm1 C24 111.72(15) . . ? C36 Sm1 C24 82.44(15) . . ? C29 Sm1 C24 28.22(15) . . ? C13 Sm1 C24 142.71(15) . . ? C28 Sm1 C24 49.48(15) . . ? C12 Sm1 C24 126.38(18) . . ? N3 Sm1 C8 99.47(14) . . ? N2 Sm1 C8 112.52(15) . . ? N1 Sm1 C8 61.55(14) . . ? C36 Sm1 C8 106.84(14) . . ? C29 Sm1 C8 141.72(14) . . ? C13 Sm1 C8 27.99(14) . . ? C28 Sm1 C8 124.19(14) . . ? C12 Sm1 C8 48.90(16) . . ? C24 Sm1 C8 168.85(14) . . ? C1 N1 C4 104.4(4) . . ? C1 N1 Sm1 126.6(3) . . ? C4 N1 Sm1 128.1(3) . . ? C20 N2 C17 106.9(5) . . ? C20 N2 Sm1 125.0(4) . . ? C17 N2 Sm1 123.0(3) . . ? C2 C1 N1 110.9(5) . . ? C2 C1 C30 128.2(5) . . ? N1 C1 C30 120.3(4) . . ? C1 C2 C3 106.9(5) . . ? C4 C3 C2 107.3(5) . . ? C3 C4 N1 110.5(5) . . ? C3 C4 C5 126.4(5) . . ? N1 C4 C5 123.0(4) . . ? C8 C5 C4 109.6(4) . . ? C8 C5 C7 107.8(4) . . ? C4 C5 C7 110.1(4) . . ? C8 C5 C6 112.1(5) . . ? C4 C5 C6 109.8(4) . . ? C7 C5 C6 107.3(5) . . ? C9 C8 C13 118.1(5) . . ? C9 C8 C5 123.1(5) . . ? C13 C8 C5 118.8(5) . . ? C9 C8 Sm1 83.4(3) . . ? C13 C8 Sm1 71.8(3) . . ? C5 C8 Sm1 111.8(3) . . ? C8 C9 C10 121.2(5) . . ? C11 C10 C9 118.7(5) . . ? C12 C11 C10 122.3(6) . . ? C11 C12 C13 118.5(6) . . ? C11 C12 C14 119.2(5) . . ? C13 C12 C14 122.1(5) . . ? C11 C12 Sm1 83.6(4) . . ? C13 C12 Sm1 73.8(3) . . ? C14 C12 Sm1 108.2(4) . . ? C12 C13 C8 121.1(5) . . ? C12 C13 Sm1 78.5(3) . . ? C8 C13 Sm1 80.2(3) . . ? C15 C14 C17 111.0(5) . . ? C15 C14 C16 109.2(5) . . ? C17 C14 C16 109.1(5) . . ? C15 C14 C12 113.4(5) . . ? C17 C14 C12 105.2(5) . . ? C16 C14 C12 108.8(5) . . ? C18 C17 N2 108.9(5) . . ? C18 C17 C14 128.9(6) . . ? N2 C17 C14 121.6(5) . . ? C17 C18 C19 106.6(6) . . ? C20 C19 C18 108.7(6) . . ? C19 C20 N2 108.8(6) . . ? C19 C20 C21 126.1(5) . . ? N2 C20 C21 125.1(5) . . ? C20 C21 C24 109.4(4) . . ? C20 C21 C23 111.2(6) . . ? C24 C21 C23 108.5(5) . . ? C20 C21 C22 110.1(5) . . ? C24 C21 C22 111.3(5) . . ? C23 C21 C22 106.4(5) . . ? C25 C24 C29 117.2(5) . . ? C25 C24 C21 124.7(5) . . ? C29 C24 C21 117.9(5) . . ? C25 C24 Sm1 82.9(3) . . ? C29 C24 Sm1 71.4(3) . . ? C21 C24 Sm1 110.9(3) . . ? C26 C25 C24 120.1(6) . . ? C27 C26 C25 121.6(7) . . ? C26 C27 C28 121.0(7) . . ? C29 C28 C27 117.0(5) . . ? C29 C28 C30 122.5(5) . . ? C27 C28 C30 120.4(5) . . ? C29 C28 Sm1 73.3(3) . . ? C27 C28 Sm1 82.6(3) . . ? C30 C28 Sm1 110.1(3) . . ? C28 C29 C24 123.0(5) . . ? C28 C29 Sm1 79.0(3) . . ? C24 C29 Sm1 80.4(3) . . ? C28 C30 C32 113.8(4) . . ? C28 C30 C1 106.6(4) . . ? C32 C30 C1 108.9(4) . . ? C28 C30 C31 109.3(4) . . ? C32 C30 C31 108.5(5) . . ? C1 C30 C31 109.6(4) . . ? C33 N3 C36 105.3(4) . . ? C33 N3 Sm1 149.1(3) . . ? C36 N3 Sm1 94.7(3) . . ? C49 N4 C52 111.4(4) . . ? C33 C34 C35 108.5(4) . . ? N3 C33 C34 109.5(4) . . ? N3 C33 C62 124.5(5) . . ? C34 C33 C62 125.7(5) . . ? C36 C35 C34 104.4(4) . . ? C36 C35 C37 128.6(5) . . ? C34 C35 C37 127.0(4) . . ? C35 C36 N3 112.2(5) . . ? C35 C36 Sm1 154.3(4) . . ? N3 C36 Sm1 56.0(2) . . ? C35 C37 C40 111.1(4) . . ? C35 C37 C39 107.5(4) . . ? C40 C37 C39 113.3(4) . . ? C35 C37 C38 109.8(4) . . ? C40 C37 C38 107.7(4) . . ? C39 C37 C38 107.3(4) . . ? C45 C40 C41 116.5(5) . . ? C45 C40 C37 120.5(5) . . ? C41 C40 C37 123.0(5) . . ? C42 C41 C40 121.2(5) . . ? C41 C42 C43 120.5(5) . . ? C42 C43 C44 120.8(5) . . ? C45 C44 C43 117.3(5) . . ? C45 C44 C46 120.1(5) . . ? C43 C44 C46 122.4(5) . . ? C44 C45 C40 123.7(5) . . ? C49 C46 C47 108.1(5) . . ? C49 C46 C44 111.2(4) . . ? C47 C46 C44 112.7(5) . . ? C49 C46 C48 108.6(5) . . ? C47 C46 C48 108.9(5) . . ? C44 C46 C48 107.2(4) . . ? N4 C49 C50 106.5(5) . . ? N4 C49 C46 121.5(5) . . ? C50 C49 C46 131.7(5) . . ? C49 C50 C51 107.4(5) . . ? C52 C51 C50 108.8(5) . . ? C51 C52 N4 105.8(5) . . ? C51 C52 C53 132.3(5) . . ? N4 C52 C53 121.8(4) . . ? C52 C53 C55 109.7(4) . . ? C52 C53 C54 108.1(4) . . ? C55 C53 C54 108.0(5) . . ? C52 C53 C56 110.0(4) . . ? C55 C53 C56 108.7(4) . . ? C54 C53 C56 112.4(4) . . ? C61 C56 C57 118.2(5) . . ? C61 C56 C53 118.9(4) . . ? C57 C56 C53 122.9(5) . . ? C56 C57 C58 119.6(5) . . ? C59 C58 C57 119.9(5) . . ? C60 C59 C58 121.6(5) . . ? C59 C60 C61 117.1(5) . . ? C59 C60 C62 124.3(4) . . ? C61 C60 C62 118.5(4) . . ? C56 C61 C60 123.4(5) . . ? C33 C62 C64 111.4(5) . . ? C33 C62 C60 106.9(4) . . ? C64 C62 C60 109.9(4) . . ? C33 C62 C63 109.7(4) . . ? C64 C62 C63 108.0(4) . . ? C60 C62 C63 111.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Sm1 N1 C1 106.2(4) . . . . ? N2 Sm1 N1 C1 -74.7(4) . . . . ? C36 Sm1 N1 C1 121.3(5) . . . . ? C29 Sm1 N1 C1 -15.4(4) . . . . ? C13 Sm1 N1 C1 -145.0(4) . . . . ? C28 Sm1 N1 C1 1.5(4) . . . . ? C12 Sm1 N1 C1 -137.0(4) . . . . ? C24 Sm1 N1 C1 -5.4(4) . . . . ? C8 Sm1 N1 C1 -175.6(4) . . . . ? N3 Sm1 N1 C4 -60.6(4) . . . . ? N2 Sm1 N1 C4 118.4(4) . . . . ? C36 Sm1 N1 C4 -45.6(6) . . . . ? C29 Sm1 N1 C4 177.8(4) . . . . ? C13 Sm1 N1 C4 48.1(4) . . . . ? C28 Sm1 N1 C4 -165.4(4) . . . . ? C12 Sm1 N1 C4 56.1(4) . . . . ? C24 Sm1 N1 C4 -172.3(4) . . . . ? C8 Sm1 N1 C4 17.5(4) . . . . ? N3 Sm1 N2 C20 -56.2(5) . . . . ? N1 Sm1 N2 C20 124.6(4) . . . . ? C36 Sm1 N2 C20 -61.5(4) . . . . ? C29 Sm1 N2 C20 55.5(4) . . . . ? C13 Sm1 N2 C20 -175.2(4) . . . . ? C28 Sm1 N2 C20 64.8(4) . . . . ? C12 Sm1 N2 C20 -157.1(5) . . . . ? C24 Sm1 N2 C20 24.5(4) . . . . ? C8 Sm1 N2 C20 -166.2(4) . . . . ? N3 Sm1 N2 C17 95.1(5) . . . . ? N1 Sm1 N2 C17 -84.1(5) . . . . ? C36 Sm1 N2 C17 89.8(5) . . . . ? C29 Sm1 N2 C17 -153.2(5) . . . . ? C13 Sm1 N2 C17 -23.9(5) . . . . ? C28 Sm1 N2 C17 -143.9(5) . . . . ? C12 Sm1 N2 C17 -5.8(4) . . . . ? C24 Sm1 N2 C17 175.8(5) . . . . ? C8 Sm1 N2 C17 -14.9(5) . . . . ? C4 N1 C1 C2 1.8(6) . . . . ? Sm1 N1 C1 C2 -167.6(4) . . . . ? C4 N1 C1 C30 -169.7(4) . . . . ? Sm1 N1 C1 C30 21.0(6) . . . . ? N1 C1 C2 C3 -1.2(6) . . . . ? C30 C1 C2 C3 169.3(5) . . . . ? C1 C2 C3 C4 0.2(7) . . . . ? C2 C3 C4 N1 0.9(6) . . . . ? C2 C3 C4 C5 -179.1(5) . . . . ? C1 N1 C4 C3 -1.6(6) . . . . ? Sm1 N1 C4 C3 167.5(4) . . . . ? C1 N1 C4 C5 178.4(5) . . . . ? Sm1 N1 C4 C5 -12.4(7) . . . . ? C3 C4 C5 C8 169.5(5) . . . . ? N1 C4 C5 C8 -10.6(7) . . . . ? C3 C4 C5 C7 51.1(7) . . . . ? N1 C4 C5 C7 -129.0(5) . . . . ? C3 C4 C5 C6 -66.9(7) . . . . ? N1 C4 C5 C6 113.0(5) . . . . ? C4 C5 C8 C9 118.8(6) . . . . ? C7 C5 C8 C9 -121.3(6) . . . . ? C6 C5 C8 C9 -3.5(7) . . . . ? C4 C5 C8 C13 -58.4(6) . . . . ? C7 C5 C8 C13 61.5(6) . . . . ? C6 C5 C8 C13 179.4(4) . . . . ? C4 C5 C8 Sm1 22.2(5) . . . . ? C7 C5 C8 Sm1 142.1(4) . . . . ? C6 C5 C8 Sm1 -100.0(4) . . . . ? N3 Sm1 C8 C9 -13.6(4) . . . . ? N2 Sm1 C8 C9 103.0(3) . . . . ? N1 Sm1 C8 C9 -143.7(4) . . . . ? C36 Sm1 C8 C9 15.6(4) . . . . ? C29 Sm1 C8 C9 -176.6(3) . . . . ? C13 Sm1 C8 C9 122.5(5) . . . . ? C28 Sm1 C8 C9 -146.8(3) . . . . ? C12 Sm1 C8 C9 92.0(4) . . . . ? C24 Sm1 C8 C9 161.2(7) . . . . ? N3 Sm1 C8 C13 -136.0(3) . . . . ? N2 Sm1 C8 C13 -19.4(3) . . . . ? N1 Sm1 C8 C13 93.8(3) . . . . ? C36 Sm1 C8 C13 -106.9(3) . . . . ? C29 Sm1 C8 C13 60.9(4) . . . . ? C28 Sm1 C8 C13 90.7(3) . . . . ? C12 Sm1 C8 C13 -30.4(3) . . . . ? C24 Sm1 C8 C13 38.7(10) . . . . ? N3 Sm1 C8 C5 109.5(3) . . . . ? N2 Sm1 C8 C5 -133.9(3) . . . . ? N1 Sm1 C8 C5 -20.7(3) . . . . ? C36 Sm1 C8 C5 138.6(3) . . . . ? C29 Sm1 C8 C5 -53.6(4) . . . . ? C13 Sm1 C8 C5 -114.5(5) . . . . ? C28 Sm1 C8 C5 -23.8(4) . . . . ? C12 Sm1 C8 C5 -144.9(4) . . . . ? C24 Sm1 C8 C5 -75.7(9) . . . . ? C13 C8 C9 C10 0.5(8) . . . . ? C5 C8 C9 C10 -176.7(5) . . . . ? Sm1 C8 C9 C10 -64.8(6) . . . . ? C8 C9 C10 C11 0.3(9) . . . . ? C9 C10 C11 C12 0.1(10) . . . . ? C10 C11 C12 C13 -1.4(10) . . . . ? C10 C11 C12 C14 173.6(5) . . . . ? C10 C11 C12 Sm1 66.3(6) . . . . ? N3 Sm1 C12 C11 -4.5(4) . . . . ? N2 Sm1 C12 C11 99.8(4) . . . . ? N1 Sm1 C12 C11 -138.2(4) . . . . ? C36 Sm1 C12 C11 20.0(4) . . . . ? C29 Sm1 C12 C11 135.3(4) . . . . ? C13 Sm1 C12 C11 -122.2(6) . . . . ? C28 Sm1 C12 C11 167.2(3) . . . . ? C24 Sm1 C12 C11 101.5(4) . . . . ? C8 Sm1 C12 C11 -91.4(4) . . . . ? N3 Sm1 C12 C13 117.7(3) . . . . ? N2 Sm1 C12 C13 -138.0(4) . . . . ? N1 Sm1 C12 C13 -16.0(3) . . . . ? C36 Sm1 C12 C13 142.2(3) . . . . ? C29 Sm1 C12 C13 -102.5(3) . . . . ? C28 Sm1 C12 C13 -70.6(4) . . . . ? C24 Sm1 C12 C13 -136.3(3) . . . . ? C8 Sm1 C12 C13 30.8(3) . . . . ? N3 Sm1 C12 C14 -123.1(4) . . . . ? N2 Sm1 C12 C14 -18.8(3) . . . . ? N1 Sm1 C12 C14 103.2(4) . . . . ? C36 Sm1 C12 C14 -98.6(4) . . . . ? C29 Sm1 C12 C14 16.7(4) . . . . ? C13 Sm1 C12 C14 119.2(5) . . . . ? C28 Sm1 C12 C14 48.6(5) . . . . ? C24 Sm1 C12 C14 -17.1(4) . . . . ? C8 Sm1 C12 C14 149.9(4) . . . . ? C11 C12 C13 C8 2.2(9) . . . . ? C14 C12 C13 C8 -172.6(5) . . . . ? Sm1 C12 C13 C8 -71.0(4) . . . . ? C11 C12 C13 Sm1 73.2(6) . . . . ? C14 C12 C13 Sm1 -101.6(5) . . . . ? C9 C8 C13 C12 -1.8(8) . . . . ? C5 C8 C13 C12 175.5(5) . . . . ? Sm1 C8 C13 C12 70.1(5) . . . . ? C9 C8 C13 Sm1 -71.8(5) . . . . ? C5 C8 C13 Sm1 105.5(4) . . . . ? N3 Sm1 C13 C12 -73.5(4) . . . . ? N2 Sm1 C13 C12 37.3(3) . . . . ? N1 Sm1 C13 C12 162.6(4) . . . . ? C36 Sm1 C13 C12 -41.6(4) . . . . ? C29 Sm1 C13 C12 95.7(3) . . . . ? C28 Sm1 C13 C12 128.1(3) . . . . ? C24 Sm1 C13 C12 66.7(4) . . . . ? C8 Sm1 C13 C12 -124.8(5) . . . . ? N3 Sm1 C13 C8 51.3(3) . . . . ? N2 Sm1 C13 C8 162.1(3) . . . . ? N1 Sm1 C13 C8 -72.6(3) . . . . ? C36 Sm1 C13 C8 83.2(3) . . . . ? C29 Sm1 C13 C8 -139.5(3) . . . . ? C28 Sm1 C13 C8 -107.1(3) . . . . ? C12 Sm1 C13 C8 124.8(5) . . . . ? C24 Sm1 C13 C8 -168.5(3) . . . . ? C11 C12 C14 C15 -177.4(6) . . . . ? C13 C12 C14 C15 -2.6(8) . . . . ? Sm1 C12 C14 C15 -84.6(5) . . . . ? C11 C12 C14 C17 -55.9(8) . . . . ? C13 C12 C14 C17 118.9(6) . . . . ? Sm1 C12 C14 C17 36.9(5) . . . . ? C11 C12 C14 C16 60.9(8) . . . . ? C13 C12 C14 C16 -124.3(6) . . . . ? Sm1 C12 C14 C16 153.8(4) . . . . ? C20 N2 C17 C18 1.8(7) . . . . ? Sm1 N2 C17 C18 -153.9(4) . . . . ? C20 N2 C17 C14 -170.3(5) . . . . ? Sm1 N2 C17 C14 34.0(8) . . . . ? C15 C14 C17 C18 -96.4(8) . . . . ? C16 C14 C17 C18 24.0(9) . . . . ? C12 C14 C17 C18 140.6(7) . . . . ? C15 C14 C17 N2 74.0(7) . . . . ? C16 C14 C17 N2 -165.6(6) . . . . ? C12 C14 C17 N2 -49.1(7) . . . . ? N2 C17 C18 C19 -0.3(8) . . . . ? C14 C17 C18 C19 171.1(6) . . . . ? C17 C18 C19 C20 -1.4(8) . . . . ? C18 C19 C20 N2 2.5(8) . . . . ? C18 C19 C20 C21 -178.1(6) . . . . ? C17 N2 C20 C19 -2.6(7) . . . . ? Sm1 N2 C20 C19 152.4(4) . . . . ? C17 N2 C20 C21 178.0(5) . . . . ? Sm1 N2 C20 C21 -26.9(7) . . . . ? C19 C20 C21 C24 -177.8(6) . . . . ? N2 C20 C21 C24 1.4(7) . . . . ? C19 C20 C21 C23 62.4(8) . . . . ? N2 C20 C21 C23 -118.4(6) . . . . ? C19 C20 C21 C22 -55.2(8) . . . . ? N2 C20 C21 C22 124.0(6) . . . . ? C20 C21 C24 C25 113.1(6) . . . . ? C23 C21 C24 C25 -125.4(6) . . . . ? C22 C21 C24 C25 -8.8(8) . . . . ? C20 C21 C24 C29 -62.2(6) . . . . ? C23 C21 C24 C29 59.3(7) . . . . ? C22 C21 C24 C29 176.0(5) . . . . ? C20 C21 C24 Sm1 17.2(5) . . . . ? C23 C21 C24 Sm1 138.7(4) . . . . ? C22 C21 C24 Sm1 -104.6(5) . . . . ? N3 Sm1 C24 C25 -33.7(4) . . . . ? N2 Sm1 C24 C25 -145.7(4) . . . . ? N1 Sm1 C24 C25 100.6(4) . . . . ? C36 Sm1 C24 C25 -61.5(4) . . . . ? C29 Sm1 C24 C25 121.9(5) . . . . ? C13 Sm1 C24 C25 -179.5(3) . . . . ? C28 Sm1 C24 C25 92.5(4) . . . . ? C12 Sm1 C24 C25 -147.5(3) . . . . ? C8 Sm1 C24 C25 151.5(7) . . . . ? N3 Sm1 C24 C29 -155.6(3) . . . . ? N2 Sm1 C24 C29 92.4(4) . . . . ? N1 Sm1 C24 C29 -21.3(4) . . . . ? C36 Sm1 C24 C29 176.6(3) . . . . ? C13 Sm1 C24 C29 58.6(4) . . . . ? C28 Sm1 C24 C29 -29.4(3) . . . . ? C12 Sm1 C24 C29 90.6(4) . . . . ? C8 Sm1 C24 C29 29.6(10) . . . . ? N3 Sm1 C24 C21 90.8(4) . . . . ? N2 Sm1 C24 C21 -21.3(3) . . . . ? N1 Sm1 C24 C21 -134.9(3) . . . . ? C36 Sm1 C24 C21 62.9(4) . . . . ? C29 Sm1 C24 C21 -113.6(5) . . . . ? C13 Sm1 C24 C21 -55.0(5) . . . . ? C28 Sm1 C24 C21 -143.0(4) . . . . ? C12 Sm1 C24 C21 -23.0(4) . . . . ? C8 Sm1 C24 C21 -84.0(9) . . . . ? C29 C24 C25 C26 -1.4(8) . . . . ? C21 C24 C25 C26 -176.7(5) . . . . ? Sm1 C24 C25 C26 -66.2(5) . . . . ? C24 C25 C26 C27 3.7(10) . . . . ? C25 C26 C27 C28 -3.3(11) . . . . ? C26 C27 C28 C29 0.7(9) . . . . ? C26 C27 C28 C30 176.7(6) . . . . ? C26 C27 C28 Sm1 67.7(6) . . . . ? N3 Sm1 C28 C29 95.9(3) . . . . ? N2 Sm1 C28 C29 -18.7(3) . . . . ? N1 Sm1 C28 C29 -141.5(4) . . . . ? C36 Sm1 C28 C29 62.6(4) . . . . ? C13 Sm1 C28 C29 -105.6(3) . . . . ? C12 Sm1 C28 C29 -75.2(4) . . . . ? C24 Sm1 C28 C29 30.0(3) . . . . ? C8 Sm1 C28 C29 -138.4(3) . . . . ? N3 Sm1 C28 C27 -25.3(4) . . . . ? N2 Sm1 C28 C27 -139.8(4) . . . . ? N1 Sm1 C28 C27 97.3(4) . . . . ? C36 Sm1 C28 C27 -58.5(4) . . . . ? C29 Sm1 C28 C27 -121.1(5) . . . . ? C13 Sm1 C28 C27 133.2(4) . . . . ? C12 Sm1 C28 C27 163.7(4) . . . . ? C24 Sm1 C28 C27 -91.1(4) . . . . ? C8 Sm1 C28 C27 100.4(4) . . . . ? N3 Sm1 C28 C30 -145.0(3) . . . . ? N2 Sm1 C28 C30 100.5(4) . . . . ? N1 Sm1 C28 C30 -22.4(3) . . . . ? C36 Sm1 C28 C30 -178.3(3) . . . . ? C29 Sm1 C28 C30 119.2(5) . . . . ? C13 Sm1 C28 C30 13.5(4) . . . . ? C12 Sm1 C28 C30 44.0(4) . . . . ? C24 Sm1 C28 C30 149.2(4) . . . . ? C8 Sm1 C28 C30 -19.3(4) . . . . ? C27 C28 C29 C24 1.5(8) . . . . ? C30 C28 C29 C24 -174.4(5) . . . . ? Sm1 C28 C29 C24 -70.8(5) . . . . ? C27 C28 C29 Sm1 72.3(5) . . . . ? C30 C28 C29 Sm1 -103.6(5) . . . . ? C25 C24 C29 C28 -1.2(8) . . . . ? C21 C24 C29 C28 174.4(5) . . . . ? Sm1 C24 C29 C28 70.1(5) . . . . ? C25 C24 C29 Sm1 -71.3(4) . . . . ? C21 C24 C29 Sm1 104.3(4) . . . . ? N3 Sm1 C29 C28 -98.8(3) . . . . ? N2 Sm1 C29 C28 159.6(4) . . . . ? N1 Sm1 C29 C28 33.7(3) . . . . ? C36 Sm1 C29 C28 -130.1(3) . . . . ? C13 Sm1 C29 C28 91.8(3) . . . . ? C12 Sm1 C29 C28 124.8(3) . . . . ? C24 Sm1 C29 C28 -126.5(5) . . . . ? C8 Sm1 C29 C28 62.4(4) . . . . ? N3 Sm1 C29 C24 27.7(4) . . . . ? N2 Sm1 C29 C24 -73.9(3) . . . . ? N1 Sm1 C29 C24 160.2(3) . . . . ? C36 Sm1 C29 C24 -3.6(4) . . . . ? C13 Sm1 C29 C24 -141.7(3) . . . . ? C28 Sm1 C29 C24 126.5(5) . . . . ? C12 Sm1 C29 C24 -108.7(3) . . . . ? C8 Sm1 C29 C24 -171.1(3) . . . . ? C29 C28 C30 C32 -0.5(7) . . . . ? C27 C28 C30 C32 -176.3(5) . . . . ? Sm1 C28 C30 C32 -83.0(5) . . . . ? C29 C28 C30 C1 119.6(5) . . . . ? C27 C28 C30 C1 -56.1(6) . . . . ? Sm1 C28 C30 C1 37.1(5) . . . . ? C29 C28 C30 C31 -122.0(5) . . . . ? C27 C28 C30 C31 62.2(7) . . . . ? Sm1 C28 C30 C31 155.4(4) . . . . ? C2 C1 C30 C28 149.8(6) . . . . ? N1 C1 C30 C28 -40.4(6) . . . . ? C2 C1 C30 C32 -86.9(7) . . . . ? N1 C1 C30 C32 82.9(6) . . . . ? C2 C1 C30 C31 31.6(8) . . . . ? N1 C1 C30 C31 -158.6(5) . . . . ? N2 Sm1 N3 C33 -141.4(6) . . . . ? N1 Sm1 N3 C33 37.7(7) . . . . ? C36 Sm1 N3 C33 -130.7(8) . . . . ? C29 Sm1 N3 C33 145.3(6) . . . . ? C13 Sm1 N3 C33 -44.8(7) . . . . ? C28 Sm1 N3 C33 114.0(6) . . . . ? C12 Sm1 N3 C33 -72.7(7) . . . . ? C24 Sm1 N3 C33 158.0(7) . . . . ? C8 Sm1 N3 C33 -23.0(7) . . . . ? N2 Sm1 N3 C36 -10.7(3) . . . . ? N1 Sm1 N3 C36 168.4(3) . . . . ? C29 Sm1 N3 C36 -84.0(3) . . . . ? C13 Sm1 N3 C36 85.9(3) . . . . ? C28 Sm1 N3 C36 -115.3(3) . . . . ? C12 Sm1 N3 C36 57.9(3) . . . . ? C24 Sm1 N3 C36 -71.3(3) . . . . ? C8 Sm1 N3 C36 107.6(3) . . . . ? C36 N3 C33 C34 -1.2(5) . . . . ? Sm1 N3 C33 C34 127.2(6) . . . . ? C36 N3 C33 C62 173.3(5) . . . . ? Sm1 N3 C33 C62 -58.3(9) . . . . ? C35 C34 C33 N3 -0.2(6) . . . . ? C35 C34 C33 C62 -174.6(5) . . . . ? C33 C34 C35 C36 1.5(6) . . . . ? C33 C34 C35 C37 -178.6(5) . . . . ? C34 C35 C36 N3 -2.3(6) . . . . ? C37 C35 C36 N3 177.8(4) . . . . ? C34 C35 C36 Sm1 -59.3(9) . . . . ? C37 C35 C36 Sm1 120.8(8) . . . . ? C33 N3 C36 C35 2.2(6) . . . . ? Sm1 N3 C36 C35 -154.0(4) . . . . ? C33 N3 C36 Sm1 156.2(4) . . . . ? N3 Sm1 C36 C35 69.6(8) . . . . ? N2 Sm1 C36 C35 -120.6(9) . . . . ? N1 Sm1 C36 C35 45.4(10) . . . . ? C29 Sm1 C36 C35 178.5(8) . . . . ? C13 Sm1 C36 C35 -38.7(9) . . . . ? C28 Sm1 C36 C35 152.3(8) . . . . ? C12 Sm1 C36 C35 -56.7(8) . . . . ? C24 Sm1 C36 C35 176.7(9) . . . . ? C8 Sm1 C36 C35 -9.6(9) . . . . ? N2 Sm1 C36 N3 169.8(3) . . . . ? N1 Sm1 C36 N3 -24.2(5) . . . . ? C29 Sm1 C36 N3 108.9(3) . . . . ? C13 Sm1 C36 N3 -108.3(3) . . . . ? C28 Sm1 C36 N3 82.8(3) . . . . ? C12 Sm1 C36 N3 -126.3(3) . . . . ? C24 Sm1 C36 N3 107.2(3) . . . . ? C8 Sm1 C36 N3 -79.2(3) . . . . ? C36 C35 C37 C40 112.5(6) . . . . ? C34 C35 C37 C40 -67.4(6) . . . . ? C36 C35 C37 C39 -122.9(6) . . . . ? C34 C35 C37 C39 57.2(6) . . . . ? C36 C35 C37 C38 -6.5(7) . . . . ? C34 C35 C37 C38 173.6(5) . . . . ? C35 C37 C40 C45 -48.1(6) . . . . ? C39 C37 C40 C45 -169.4(5) . . . . ? C38 C37 C40 C45 72.1(6) . . . . ? C35 C37 C40 C41 135.1(5) . . . . ? C39 C37 C40 C41 13.9(7) . . . . ? C38 C37 C40 C41 -104.7(6) . . . . ? C45 C40 C41 C42 -2.0(8) . . . . ? C37 C40 C41 C42 174.9(5) . . . . ? C40 C41 C42 C43 -0.2(8) . . . . ? C41 C42 C43 C44 1.8(8) . . . . ? C42 C43 C44 C45 -1.1(8) . . . . ? C42 C43 C44 C46 -175.3(5) . . . . ? C43 C44 C45 C40 -1.3(8) . . . . ? C46 C44 C45 C40 173.1(5) . . . . ? C41 C40 C45 C44 2.8(8) . . . . ? C37 C40 C45 C44 -174.2(5) . . . . ? C45 C44 C46 C49 41.4(7) . . . . ? C43 C44 C46 C49 -144.5(5) . . . . ? C45 C44 C46 C47 163.0(5) . . . . ? C43 C44 C46 C47 -22.9(7) . . . . ? C45 C44 C46 C48 -77.1(6) . . . . ? C43 C44 C46 C48 97.0(7) . . . . ? C52 N4 C49 C50 -0.6(6) . . . . ? C52 N4 C49 C46 174.4(4) . . . . ? C47 C46 C49 N4 -63.2(7) . . . . ? C44 C46 C49 N4 61.0(7) . . . . ? C48 C46 C49 N4 178.8(5) . . . . ? C47 C46 C49 C50 110.4(7) . . . . ? C44 C46 C49 C50 -125.4(6) . . . . ? C48 C46 C49 C50 -7.7(8) . . . . ? N4 C49 C50 C51 -0.2(6) . . . . ? C46 C49 C50 C51 -174.5(5) . . . . ? C49 C50 C51 C52 1.0(6) . . . . ? C50 C51 C52 N4 -1.3(6) . . . . ? C50 C51 C52 C53 174.7(5) . . . . ? C49 N4 C52 C51 1.2(6) . . . . ? C49 N4 C52 C53 -175.3(4) . . . . ? C51 C52 C53 C55 9.2(8) . . . . ? N4 C52 C53 C55 -175.4(4) . . . . ? C51 C52 C53 C54 -108.3(6) . . . . ? N4 C52 C53 C54 67.1(6) . . . . ? C51 C52 C53 C56 128.7(6) . . . . ? N4 C52 C53 C56 -55.9(6) . . . . ? C52 C53 C56 C61 -58.1(6) . . . . ? C55 C53 C56 C61 62.0(6) . . . . ? C54 C53 C56 C61 -178.6(5) . . . . ? C52 C53 C56 C57 123.9(5) . . . . ? C55 C53 C56 C57 -115.9(5) . . . . ? C54 C53 C56 C57 3.5(7) . . . . ? C61 C56 C57 C58 -0.1(7) . . . . ? C53 C56 C57 C58 177.9(5) . . . . ? C56 C57 C58 C59 -2.4(8) . . . . ? C57 C58 C59 C60 2.2(8) . . . . ? C58 C59 C60 C61 0.3(7) . . . . ? C58 C59 C60 C62 178.7(5) . . . . ? C57 C56 C61 C60 2.8(8) . . . . ? C53 C56 C61 C60 -175.2(5) . . . . ? C59 C60 C61 C56 -2.9(7) . . . . ? C62 C60 C61 C56 178.6(5) . . . . ? N3 C33 C62 C64 4.3(7) . . . . ? C34 C33 C62 C64 177.9(5) . . . . ? N3 C33 C62 C60 -115.7(5) . . . . ? C34 C33 C62 C60 57.8(6) . . . . ? N3 C33 C62 C63 123.8(5) . . . . ? C34 C33 C62 C63 -62.6(7) . . . . ? C59 C60 C62 C33 -118.1(5) . . . . ? C61 C60 C62 C33 60.2(6) . . . . ? C59 C60 C62 C64 120.8(5) . . . . ? C61 C60 C62 C64 -60.9(6) . . . . ? C59 C60 C62 C63 1.5(7) . . . . ? C61 C60 C62 C63 179.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.885 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.073