# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dr. Qi Shen' _publ_contact_author_email qshen@suda.edu.cn loop_ _publ_author_name 'Zhu Du' 'Yong Zhang' 'Ying-ming Yao' 'Qi Shen' #============================================================================== data_complexl _database_code_depnum_ccdc_archive 'CCDC 807555' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C160 H304 N32 O16 P8 Sm4, 8(C4 H8 O)' _chemical_formula_sum 'C192 H368 N32 O24 P8 Sm4' _chemical_formula_weight 4358.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 33.120(2) _cell_length_b 18.3460(11) _cell_length_c 41.000(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.620(2) _cell_angle_gamma 90.00 _cell_volume 23160(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 46648 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.6 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9216 _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.631 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58744 _diffrn_reflns_av_R_equivalents 0.0920 _diffrn_reflns_av_sigmaI/netI 0.1251 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.50 _reflns_number_total 21432 _reflns_number_gt 13964 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+121.5860P] 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 21432 _refine_ls_number_parameters 1132 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.1525 _refine_ls_R_factor_gt 0.0982 _refine_ls_wR_factor_ref 0.2048 _refine_ls_wR_factor_gt 0.1745 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.887049(16) 0.53515(3) 0.634803(13) 0.04636(15) Uani 1 1 d . . . Sm2 Sm 1.124068(17) 0.56043(3) 0.683081(14) 0.05020(16) Uani 1 1 d . . . P1 P 0.78111(10) 0.41077(18) 0.60124(9) 0.0740(9) Uani 1 1 d . . . P2 P 0.87255(11) 0.63016(18) 0.54353(8) 0.0718(8) Uani 1 1 d . . . P3 P 1.11752(9) 0.76821(14) 0.69716(7) 0.0535(7) Uani 1 1 d D . . P4 P 1.11912(9) 0.35088(15) 0.67431(8) 0.0630(8) Uani 1 1 d D . . O1 O 0.8635(2) 0.6485(3) 0.64988(16) 0.0551(16) Uani 1 1 d . . . O2 O 1.1229(2) 0.5678(4) 0.62587(18) 0.0587(17) Uani 1 1 d . . . O3 O 0.9268(2) 0.4244(3) 0.64137(16) 0.0536(16) Uani 1 1 d . . . O4 O 0.8008(2) 0.5686(4) 0.79206(17) 0.0580(17) Uani 1 1 d . . . O5 O 0.8189(2) 0.4624(4) 0.61154(19) 0.074(2) Uani 1 1 d . . . O6 O 0.8755(2) 0.5886(4) 0.57583(17) 0.071(2) Uani 1 1 d . . . O7 O 1.1105(2) 0.6883(3) 0.69603(17) 0.0614(18) Uani 1 1 d . A . O8 O 1.1095(2) 0.4266(3) 0.68198(17) 0.0565(17) Uani 1 1 d . B . N1 N 0.9643(2) 0.6272(4) 0.66153(18) 0.0442(17) Uani 1 1 d . . . N2 N 1.0293(2) 0.5707(4) 0.63442(18) 0.0433(17) Uani 1 1 d . . . N3 N 0.9068(2) 0.4697(4) 0.70825(18) 0.0443(17) Uani 1 1 d . . . N4 N 0.8483(2) 0.5446(4) 0.73653(18) 0.0426(17) Uani 1 1 d . . . N5 N 0.7768(3) 0.3684(5) 0.5640(2) 0.083(3) Uani 1 1 d . . . N6 N 0.7376(3) 0.4566(6) 0.5980(3) 0.099(4) Uani 1 1 d . . . N7 N 0.7831(3) 0.3425(6) 0.6280(3) 0.080(3) Uani 1 1 d . . . N8 N 0.8230(3) 0.6530(6) 0.5236(3) 0.090(3) Uani 1 1 d . . . N9 N 0.8923(3) 0.5805(5) 0.5199(2) 0.078(3) Uani 1 1 d . . . N10 N 0.8986(3) 0.7097(5) 0.5485(3) 0.077(3) Uani 1 1 d . . . N11 N 1.1108(5) 0.7921(9) 0.6559(3) 0.066(3) Uiso 0.50 1 d PD A 1 N11' N 1.0830(6) 0.8128(9) 0.6639(4) 0.066(3) Uiso 0.50 1 d PD A 2 N12 N 1.1682(6) 0.7874(9) 0.7213(4) 0.054(3) Uiso 0.50 1 d PD A 1 N12' N 1.1653(6) 0.7969(9) 0.7072(4) 0.054(3) Uiso 0.50 1 d PD A 2 N13 N 1.0830(6) 0.8122(9) 0.7095(4) 0.064(4) Uiso 0.50 1 d PD A 1 N13' N 1.1039(5) 0.8080(9) 0.7281(4) 0.064(4) Uiso 0.50 1 d PD A 2 N14 N 1.0741(5) 0.3000(9) 0.6655(5) 0.067(4) Uiso 0.50 1 d PD B 1 N14' N 1.0842(6) 0.2944(10) 0.6787(5) 0.067(4) Uiso 0.50 1 d PD B 2 N15 N 1.1207(8) 0.3455(16) 0.6335(4) 0.085(4) Uiso 0.50 1 d PD B 1 N15' N 1.1255(8) 0.3307(16) 0.6376(5) 0.085(4) Uiso 0.50 1 d PD B 2 N16 N 1.1703(5) 0.3331(10) 0.6966(4) 0.064(3) Uiso 0.50 1 d PD B 1 N16' N 1.1606(5) 0.3201(10) 0.7076(4) 0.064(3) Uiso 0.50 1 d PD B 2 C1 C 0.8760(3) 0.7173(5) 0.6542(2) 0.049(2) Uani 1 1 d . . . C2 C 0.8462(3) 0.7769(5) 0.6425(3) 0.056(3) Uani 1 1 d . . . C3 C 0.8630(4) 0.8470(6) 0.6487(3) 0.075(3) Uani 1 1 d . . . H3 H 0.8435 0.8861 0.6411 0.090 Uiso 1 1 calc R . . C4 C 0.9067(4) 0.8631(6) 0.6653(3) 0.077(3) Uani 1 1 d . . . C5 C 0.9348(4) 0.8044(6) 0.6756(3) 0.064(3) Uani 1 1 d . . . H5 H 0.9648 0.8133 0.6861 0.076 Uiso 1 1 calc R . . C6 C 0.9204(3) 0.7338(5) 0.6709(2) 0.050(2) Uani 1 1 d . . . C7 C 1.0964(3) 0.5794(5) 0.5930(3) 0.054(2) Uani 1 1 d . . . C8 C 1.1111(4) 0.6117(5) 0.5673(3) 0.061(3) Uani 1 1 d . . . C9 C 1.0804(4) 0.6235(6) 0.5342(3) 0.062(3) Uani 1 1 d . . . H9 H 1.0896 0.6450 0.5173 0.075 Uiso 1 1 calc R . . C10 C 1.0370(4) 0.6058(6) 0.5243(3) 0.066(3) Uani 1 1 d . . . C11 C 1.0236(3) 0.5718(6) 0.5486(3) 0.060(3) Uani 1 1 d . . . H11 H 0.9945 0.5572 0.5420 0.072 Uiso 1 1 calc R . . C12 C 1.0519(3) 0.5585(5) 0.5825(2) 0.047(2) Uani 1 1 d . . . C13 C 0.9531(3) 0.6744(5) 0.6864(2) 0.050(2) Uani 1 1 d . . . H13A H 0.9799 0.6970 0.7023 0.060 Uiso 1 1 calc R . . H13B H 0.9421 0.6431 0.7006 0.060 Uiso 1 1 calc R . . C14 C 0.9818(3) 0.6715(5) 0.6395(2) 0.047(2) Uani 1 1 d . . . H14A H 1.0070 0.6993 0.6546 0.057 Uiso 1 1 calc R . . H14B H 0.9597 0.7062 0.6256 0.057 Uiso 1 1 calc R . . C15 C 0.9952(3) 0.6234(5) 0.6153(2) 0.051(2) Uani 1 1 d . . . H15A H 0.9697 0.5969 0.5997 0.061 Uiso 1 1 calc R . . H15B H 1.0058 0.6542 0.6006 0.061 Uiso 1 1 calc R . . C16 C 0.9995(3) 0.5768(5) 0.6815(2) 0.049(2) Uani 1 1 d . . . H16A H 0.9899 0.5467 0.6970 0.059 Uiso 1 1 calc R . . H16B H 1.0249 0.6050 0.6962 0.059 Uiso 1 1 calc R . . C17 C 1.0124(3) 0.5277(5) 0.6567(2) 0.055(3) Uani 1 1 d . . . H17A H 1.0346 0.4929 0.6705 0.066 Uiso 1 1 calc R . . H17B H 0.9870 0.4998 0.6419 0.066 Uiso 1 1 calc R . . C18 C 1.0365(3) 0.5213(5) 0.6086(2) 0.051(2) Uani 1 1 d . . . H18A H 1.0093 0.4957 0.5958 0.062 Uiso 1 1 calc R . . H18B H 1.0580 0.4845 0.6213 0.062 Uiso 1 1 calc R . . C19 C 0.7968(3) 0.7626(6) 0.6239(3) 0.063(3) Uani 1 1 d . . . C20 C 0.7702(4) 0.8341(6) 0.6139(4) 0.092(4) Uani 1 1 d . . . H20A H 0.7801 0.8626 0.5983 0.138 Uiso 1 1 calc R . . H20B H 0.7742 0.8619 0.6350 0.138 Uiso 1 1 calc R . . H20C H 0.7397 0.8225 0.6021 0.138 Uiso 1 1 calc R . . C21 C 0.7801(3) 0.7195(6) 0.6479(3) 0.074(3) Uani 1 1 d . . . H21A H 0.7496 0.7083 0.6357 0.111 Uiso 1 1 calc R . . H21B H 0.7837 0.7481 0.6687 0.111 Uiso 1 1 calc R . . H21C H 0.7965 0.6745 0.6548 0.111 Uiso 1 1 calc R . . C22 C 0.7882(4) 0.7195(7) 0.5901(3) 0.079(3) Uani 1 1 d . . . H22A H 0.8056 0.6754 0.5953 0.118 Uiso 1 1 calc R . . H22B H 0.7959 0.7490 0.5736 0.118 Uiso 1 1 calc R . . H22C H 0.7577 0.7066 0.5798 0.118 Uiso 1 1 calc R . . C23 C 0.9223(4) 0.9430(6) 0.6741(4) 0.107(5) Uani 1 1 d . . . H23A H 0.9176 0.9585 0.6950 0.160 Uiso 1 1 calc R . . H23B H 0.9062 0.9744 0.6546 0.160 Uiso 1 1 calc R . . H23C H 0.9530 0.9461 0.6782 0.160 Uiso 1 1 calc R . . C24 C 1.1589(4) 0.6294(6) 0.5765(3) 0.065(3) Uani 1 1 d . . . C25 C 1.1680(4) 0.6591(8) 0.5449(3) 0.105(5) Uani 1 1 d . . . H25A H 1.1573 0.6249 0.5256 0.157 Uiso 1 1 calc R . . H25B H 1.1990 0.6656 0.5513 0.157 Uiso 1 1 calc R . . H25C H 1.1534 0.7055 0.5379 0.157 Uiso 1 1 calc R . . C26 C 1.1735(4) 0.6887(7) 0.6050(3) 0.086(4) Uani 1 1 d . . . H26A H 1.1598 0.7346 0.5952 0.129 Uiso 1 1 calc R . . H26B H 1.2048 0.6941 0.6132 0.129 Uiso 1 1 calc R . . H26C H 1.1651 0.6748 0.6244 0.129 Uiso 1 1 calc R . . C27 C 1.1868(4) 0.5605(6) 0.5900(3) 0.077(3) Uani 1 1 d . . . H27A H 1.1809 0.5405 0.6097 0.115 Uiso 1 1 calc R . . H27B H 1.2173 0.5732 0.5976 0.115 Uiso 1 1 calc R . . H27C H 1.1797 0.5246 0.5714 0.115 Uiso 1 1 calc R . . C28 C 1.0038(4) 0.6216(7) 0.4866(3) 0.091(4) Uani 1 1 d . . . H28A H 1.0005 0.6738 0.4830 0.136 Uiso 1 1 calc R . . H28B H 0.9759 0.6003 0.4839 0.136 Uiso 1 1 calc R . . H28C H 1.0142 0.6004 0.4695 0.136 Uiso 1 1 calc R . . C29 C 0.9288(3) 0.3579(5) 0.6546(3) 0.050(2) Uani 1 1 d . . . C30 C 0.9284(3) 0.2941(5) 0.6352(3) 0.056(3) Uani 1 1 d . . . C31 C 0.9295(4) 0.2277(6) 0.6510(3) 0.080(4) Uani 1 1 d . . . H31 H 0.9291 0.1858 0.6376 0.096 Uiso 1 1 calc R . . C32 C 0.9311(5) 0.2172(6) 0.6849(4) 0.088(4) Uani 1 1 d . . . C33 C 0.9340(4) 0.2811(6) 0.7050(3) 0.072(3) Uani 1 1 d . . . H33 H 0.9369 0.2773 0.7286 0.086 Uiso 1 1 calc R . . C34 C 0.9327(3) 0.3512(5) 0.6896(3) 0.054(2) Uani 1 1 d . . . C35 C 0.7670(3) 0.5650(5) 0.7629(3) 0.053(2) Uani 1 1 d . . . C36 C 0.7714(3) 0.5781(5) 0.7298(2) 0.047(2) Uani 1 1 d . . . C37 C 0.7367(3) 0.5755(5) 0.6982(3) 0.058(3) Uani 1 1 d . . . H37 H 0.7413 0.5835 0.6772 0.069 Uiso 1 1 calc R . . C38 C 0.6939(3) 0.5606(5) 0.6972(3) 0.058(3) Uani 1 1 d . . . C39 C 0.6895(3) 0.5492(5) 0.7286(3) 0.064(3) Uani 1 1 d . . . H39 H 0.6616 0.5379 0.7282 0.077 Uiso 1 1 calc R . . C40 C 0.7233(3) 0.5529(5) 0.7615(3) 0.057(3) Uani 1 1 d . . . C41 C 0.9423(3) 0.4152(5) 0.7146(3) 0.055(2) Uani 1 1 d . . . H41A H 0.9501 0.3961 0.7384 0.066 Uiso 1 1 calc R . . H41B H 0.9679 0.4406 0.7136 0.066 Uiso 1 1 calc R . . C42 C 0.8683(3) 0.4347(5) 0.7103(3) 0.054(2) Uani 1 1 d . . . H42A H 0.8762 0.4085 0.7326 0.065 Uiso 1 1 calc R . . H42B H 0.8569 0.3992 0.6913 0.065 Uiso 1 1 calc R . . C43 C 0.8330(3) 0.4912(5) 0.7077(3) 0.053(2) Uani 1 1 d . . . H43A H 0.8247 0.5167 0.6851 0.064 Uiso 1 1 calc R . . H43B H 0.8072 0.4662 0.7084 0.064 Uiso 1 1 calc R . . C44 C 0.9222(3) 0.5228(5) 0.7378(2) 0.050(2) Uani 1 1 d . . . H44A H 0.9485 0.5472 0.7377 0.060 Uiso 1 1 calc R . . H44B H 0.9296 0.4968 0.7602 0.060 Uiso 1 1 calc R . . C45 C 0.8877(3) 0.5790(5) 0.7346(2) 0.047(2) Uani 1 1 d . . . H45A H 0.8990 0.6149 0.7534 0.057 Uiso 1 1 calc R . . H45B H 0.8802 0.6046 0.7121 0.057 Uiso 1 1 calc R . . C46 C 0.8144(3) 0.6016(5) 0.7299(2) 0.051(2) Uani 1 1 d . . . H46A H 0.8099 0.6239 0.7071 0.061 Uiso 1 1 calc R . . H46B H 0.8257 0.6396 0.7477 0.061 Uiso 1 1 calc R . . C47 C 0.9274(4) 0.2988(6) 0.5973(3) 0.068(3) Uani 1 1 d . . . C48 C 0.9313(5) 0.2239(7) 0.5825(4) 0.120(6) Uani 1 1 d . . . H48A H 0.9089 0.1920 0.5844 0.180 Uiso 1 1 calc R . . H48B H 0.9597 0.2034 0.5957 0.180 Uiso 1 1 calc R . . H48C H 0.9278 0.2287 0.5581 0.180 Uiso 1 1 calc R . . C49 C 0.9659(4) 0.3449(7) 0.5973(3) 0.091(4) Uani 1 1 d . . . H49A H 0.9663 0.3465 0.5738 0.136 Uiso 1 1 calc R . . H49B H 0.9927 0.3236 0.6132 0.136 Uiso 1 1 calc R . . H49C H 0.9630 0.3940 0.6050 0.136 Uiso 1 1 calc R . . C50 C 0.8855(4) 0.3317(7) 0.5735(3) 0.089(4) Uani 1 1 d . . . H50A H 0.8798 0.3760 0.5840 0.134 Uiso 1 1 calc R . . H50B H 0.8620 0.2973 0.5701 0.134 Uiso 1 1 calc R . . H50C H 0.8874 0.3430 0.5510 0.134 Uiso 1 1 calc R . . C51 C 0.9343(6) 0.1427(6) 0.7014(4) 0.138(7) Uani 1 1 d . . . H51A H 0.9055 0.1264 0.6992 0.207 Uiso 1 1 calc R . . H51B H 0.9528 0.1453 0.7260 0.207 Uiso 1 1 calc R . . H51C H 0.9465 0.1086 0.6895 0.207 Uiso 1 1 calc R . . C52 C 0.7150(4) 0.5458(6) 0.7958(3) 0.067(3) Uani 1 1 d . . . C53 C 0.6665(4) 0.5306(7) 0.7888(4) 0.096(4) Uani 1 1 d . . . H53A H 0.6629 0.5211 0.8109 0.145 Uiso 1 1 calc R . . H53B H 0.6569 0.4885 0.7736 0.145 Uiso 1 1 calc R . . H53C H 0.6492 0.5727 0.7776 0.145 Uiso 1 1 calc R . . C54 C 0.7276(4) 0.6170(6) 0.8166(3) 0.081(3) Uani 1 1 d . . . H54A H 0.7585 0.6253 0.8233 0.121 Uiso 1 1 calc R . . H54B H 0.7205 0.6136 0.8375 0.121 Uiso 1 1 calc R . . H54C H 0.7116 0.6572 0.8022 0.121 Uiso 1 1 calc R . . C55 C 0.7421(4) 0.4823(6) 0.8179(3) 0.091(4) Uani 1 1 d . . . H55A H 0.7727 0.4933 0.8248 0.136 Uiso 1 1 calc R . . H55B H 0.7354 0.4379 0.8042 0.136 Uiso 1 1 calc R . . H55C H 0.7351 0.4759 0.8388 0.136 Uiso 1 1 calc R . . C56 C 0.6555(3) 0.5572(6) 0.6623(3) 0.082(4) Uani 1 1 d . . . H56A H 0.6287 0.5528 0.6667 0.123 Uiso 1 1 calc R . . H56B H 0.6587 0.5153 0.6490 0.123 Uiso 1 1 calc R . . H56C H 0.6546 0.6014 0.6490 0.123 Uiso 1 1 calc R . . C57 C 0.7863(4) 0.4101(7) 0.5374(3) 0.100(4) Uani 1 1 d . . . H57A H 0.7953 0.3772 0.5229 0.149 Uiso 1 1 calc R . . H57B H 0.8094 0.4447 0.5488 0.149 Uiso 1 1 calc R . . H57C H 0.7604 0.4362 0.5229 0.149 Uiso 1 1 calc R . . C58 C 0.7493(5) 0.3056(8) 0.5510(4) 0.135(6) Uani 1 1 d . . . H58A H 0.7220 0.3208 0.5332 0.203 Uiso 1 1 calc R . . H58B H 0.7437 0.2825 0.5702 0.203 Uiso 1 1 calc R . . H58C H 0.7637 0.2713 0.5409 0.203 Uiso 1 1 calc R . . C59 C 0.7376(4) 0.5352(8) 0.6000(4) 0.115(5) Uani 1 1 d . . . H59A H 0.7231 0.5552 0.5767 0.172 Uiso 1 1 calc R . . H59B H 0.7673 0.5527 0.6096 0.172 Uiso 1 1 calc R . . H59C H 0.7224 0.5503 0.6151 0.172 Uiso 1 1 calc R . . C60 C 0.6945(4) 0.4229(9) 0.5822(5) 0.149(7) Uani 1 1 d . . . H60A H 0.6763 0.4384 0.5948 0.224 Uiso 1 1 calc R . . H60B H 0.6974 0.3703 0.5834 0.224 Uiso 1 1 calc R . . H60C H 0.6813 0.4378 0.5578 0.224 Uiso 1 1 calc R . . C61 C 0.7627(5) 0.3442(8) 0.6537(3) 0.110(5) Uani 1 1 d . . . H61A H 0.7450 0.3009 0.6513 0.165 Uiso 1 1 calc R . . H61B H 0.7445 0.3872 0.6500 0.165 Uiso 1 1 calc R . . H61C H 0.7849 0.3456 0.6771 0.165 Uiso 1 1 calc R . . C62 C 0.8142(4) 0.2826(7) 0.6327(4) 0.099(4) Uani 1 1 d . . . H62A H 0.8364 0.2851 0.6561 0.148 Uiso 1 1 calc R . . H62B H 0.8277 0.2869 0.6155 0.148 Uiso 1 1 calc R . . H62C H 0.7991 0.2363 0.6297 0.148 Uiso 1 1 calc R . . C63 C 0.8094(5) 0.7107(10) 0.4960(4) 0.150(7) Uani 1 1 d . . . H63A H 0.8094 0.6908 0.4741 0.225 Uiso 1 1 calc R . . H63B H 0.8296 0.7513 0.5031 0.225 Uiso 1 1 calc R . . H63C H 0.7805 0.7275 0.4928 0.225 Uiso 1 1 calc R . . C64 C 0.7872(4) 0.6030(7) 0.5217(4) 0.111(5) Uani 1 1 d . . . H64A H 0.7611 0.6310 0.5182 0.167 Uiso 1 1 calc R . . H64B H 0.7951 0.5756 0.5434 0.167 Uiso 1 1 calc R . . H64C H 0.7819 0.5696 0.5022 0.167 Uiso 1 1 calc R . . C65 C 0.8827(5) 0.5980(9) 0.4839(3) 0.116(5) Uani 1 1 d . . . H65A H 0.9009 0.5689 0.4750 0.174 Uiso 1 1 calc R . . H65B H 0.8884 0.6493 0.4818 0.174 Uiso 1 1 calc R . . H65C H 0.8524 0.5877 0.4705 0.174 Uiso 1 1 calc R . . C66 C 0.9006(4) 0.5028(6) 0.5280(3) 0.089(4) Uani 1 1 d . . . H66A H 0.8734 0.4764 0.5197 0.133 Uiso 1 1 calc R . . H66B H 0.9147 0.4966 0.5532 0.133 Uiso 1 1 calc R . . H66C H 0.9194 0.4842 0.5166 0.133 Uiso 1 1 calc R . . C67 C 0.8856(5) 0.7680(7) 0.5653(3) 0.104(5) Uani 1 1 d . . . H67A H 0.9096 0.7816 0.5865 0.156 Uiso 1 1 calc R . . H67B H 0.8612 0.7526 0.5713 0.156 Uiso 1 1 calc R . . H67C H 0.8771 0.8096 0.5496 0.156 Uiso 1 1 calc R . . C68 C 0.9380(4) 0.7241(7) 0.5406(3) 0.097(4) Uani 1 1 d . . . H68A H 0.9315 0.7605 0.5222 0.145 Uiso 1 1 calc R . . H68B H 0.9473 0.6794 0.5329 0.145 Uiso 1 1 calc R . . H68C H 0.9609 0.7418 0.5616 0.145 Uiso 1 1 calc R . . C69 C 1.1287(7) 0.8588(11) 0.6470(6) 0.080(5) Uiso 0.50 1 d PD A 1 H69A H 1.1363 0.8499 0.6266 0.120 Uiso 0.50 1 calc PR A 1 H69B H 1.1544 0.8732 0.6667 0.120 Uiso 0.50 1 calc PR A 1 H69C H 1.1072 0.8973 0.6417 0.120 Uiso 0.50 1 calc PR A 1 C69' C 1.0647(8) 0.8846(11) 0.6699(6) 0.080(5) Uiso 0.50 1 d PD A 2 H69D H 1.0343 0.8878 0.6549 0.120 Uiso 0.50 1 calc PR A 2 H69E H 1.0806 0.9243 0.6645 0.120 Uiso 0.50 1 calc PR A 2 H69F H 1.0675 0.8879 0.6943 0.120 Uiso 0.50 1 calc PR A 2 C70 C 1.0787(7) 0.7508(13) 0.6264(6) 0.069(5) Uiso 0.50 1 d PD A 1 H70A H 1.0502 0.7731 0.6202 0.103 Uiso 0.50 1 calc PR A 1 H70B H 1.0774 0.7008 0.6336 0.103 Uiso 0.50 1 calc PR A 1 H70C H 1.0874 0.7517 0.6063 0.103 Uiso 0.50 1 calc PR A 1 C70' C 1.0732(8) 0.7761(13) 0.6299(6) 0.069(5) Uiso 0.50 1 d PD A 2 H70D H 1.0462 0.7949 0.6131 0.103 Uiso 0.50 1 calc PR A 2 H70E H 1.0705 0.7240 0.6328 0.103 Uiso 0.50 1 calc PR A 2 H70F H 1.0965 0.7850 0.6214 0.103 Uiso 0.50 1 calc PR A 2 C71 C 1.1821(9) 0.8370(14) 0.7504(6) 0.111(7) Uiso 0.50 1 d PD A 1 H71A H 1.1914 0.8096 0.7722 0.167 Uiso 0.50 1 calc PR A 1 H71B H 1.1582 0.8687 0.7493 0.167 Uiso 0.50 1 calc PR A 1 H71C H 1.2061 0.8662 0.7495 0.167 Uiso 0.50 1 calc PR A 1 C71' C 1.1777(9) 0.8741(12) 0.7057(8) 0.111(7) Uiso 0.50 1 d PD A 2 H71D H 1.1814 0.8979 0.7278 0.167 Uiso 0.50 1 calc PR A 2 H71E H 1.1552 0.8987 0.6867 0.167 Uiso 0.50 1 calc PR A 2 H71F H 1.2048 0.8762 0.7017 0.167 Uiso 0.50 1 calc PR A 2 C72 C 1.2000(10) 0.759(2) 0.7064(9) 0.078(5) Uiso 0.50 1 d PD A 1 H72A H 1.2076 0.7976 0.6935 0.118 Uiso 0.50 1 calc PR A 1 H72B H 1.1871 0.7188 0.6907 0.118 Uiso 0.50 1 calc PR A 1 H72C H 1.2259 0.7425 0.7253 0.118 Uiso 0.50 1 calc PR A 1 C72' C 1.2039(10) 0.750(2) 0.7140(9) 0.078(5) Uiso 0.50 1 d PD A 2 H72D H 1.2263 0.7772 0.7094 0.118 Uiso 0.50 1 calc PR A 2 H72E H 1.1959 0.7076 0.6988 0.118 Uiso 0.50 1 calc PR A 2 H72F H 1.2147 0.7343 0.7384 0.118 Uiso 0.50 1 calc PR A 2 C73 C 1.0744(10) 0.8900(11) 0.7060(8) 0.106(6) Uiso 0.50 1 d PD A 1 H73A H 1.0443 0.8981 0.6910 0.159 Uiso 0.50 1 calc PR A 1 H73B H 1.0932 0.9129 0.6956 0.159 Uiso 0.50 1 calc PR A 1 H73C H 1.0798 0.9109 0.7289 0.159 Uiso 0.50 1 calc PR A 1 C73' C 1.1403(8) 0.8056(15) 0.7642(6) 0.106(6) Uiso 0.50 1 d PD A 2 H73D H 1.1374 0.8466 0.7781 0.159 Uiso 0.50 1 calc PR A 2 H73E H 1.1682 0.8082 0.7615 0.159 Uiso 0.50 1 calc PR A 2 H73F H 1.1385 0.7605 0.7759 0.159 Uiso 0.50 1 calc PR A 2 C74 C 1.0814(8) 0.7839(14) 0.7438(6) 0.075(5) Uiso 0.50 1 d PD A 1 H74A H 1.1107 0.7748 0.7602 0.112 Uiso 0.50 1 calc PR A 1 H74B H 1.0648 0.7389 0.7395 0.112 Uiso 0.50 1 calc PR A 1 H74C H 1.0676 0.8198 0.7536 0.112 Uiso 0.50 1 calc PR A 1 C74' C 1.0646(7) 0.7912(14) 0.7350(7) 0.075(5) Uiso 0.50 1 d PD A 2 H74D H 1.0610 0.7387 0.7353 0.112 Uiso 0.50 1 calc PR A 2 H74E H 1.0396 0.8123 0.7167 0.112 Uiso 0.50 1 calc PR A 2 H74F H 1.0670 0.8113 0.7575 0.112 Uiso 0.50 1 calc PR A 2 C75 C 1.0582(9) 0.3060(16) 0.6954(7) 0.068(4) Uiso 0.50 1 d PD B 1 H75A H 1.0373 0.2677 0.6934 0.102 Uiso 0.50 1 calc PR B 1 H75B H 1.0445 0.3531 0.6945 0.102 Uiso 0.50 1 calc PR B 1 H75C H 1.0826 0.3011 0.7175 0.102 Uiso 0.50 1 calc PR B 1 C75' C 1.0466(8) 0.3148(16) 0.6881(7) 0.068(4) Uiso 0.50 1 d PD B 2 H75D H 1.0198 0.3016 0.6691 0.102 Uiso 0.50 1 calc PR B 2 H75E H 1.0469 0.3670 0.6921 0.102 Uiso 0.50 1 calc PR B 2 H75F H 1.0483 0.2893 0.7093 0.102 Uiso 0.50 1 calc PR B 2 C76 C 1.0728(9) 0.2232(11) 0.6547(7) 0.106(6) Uiso 0.50 1 d PD B 1 H76A H 1.0905 0.1941 0.6746 0.159 Uiso 0.50 1 calc PR B 1 H76B H 1.0839 0.2192 0.6360 0.159 Uiso 0.50 1 calc PR B 1 H76C H 1.0430 0.2059 0.6465 0.159 Uiso 0.50 1 calc PR B 1 C76' C 1.1064(9) 0.2379(14) 0.7060(7) 0.106(6) Uiso 0.50 1 d PD B 2 H76D H 1.0914 0.2338 0.7223 0.159 Uiso 0.50 1 calc PR B 2 H76E H 1.1363 0.2522 0.7187 0.159 Uiso 0.50 1 calc PR B 2 H76F H 1.1057 0.1912 0.6947 0.159 Uiso 0.50 1 calc PR B 2 C77 C 1.0819(9) 0.3376(16) 0.6017(7) 0.102(7) Uiso 0.50 1 d PD B 1 H77A H 1.0728 0.3851 0.5912 0.153 Uiso 0.50 1 calc PR B 1 H77B H 1.0588 0.3160 0.6077 0.153 Uiso 0.50 1 calc PR B 1 H77C H 1.0884 0.3063 0.5852 0.153 Uiso 0.50 1 calc PR B 1 C77' C 1.0982(9) 0.3659(16) 0.6052(7) 0.102(7) Uiso 0.50 1 d PD B 2 H77D H 1.1074 0.4160 0.6051 0.153 Uiso 0.50 1 calc PR B 2 H77E H 1.0682 0.3650 0.6036 0.153 Uiso 0.50 1 calc PR B 2 H77F H 1.1005 0.3402 0.5854 0.153 Uiso 0.50 1 calc PR B 2 C78 C 1.1514(11) 0.3815(18) 0.6207(9) 0.126(8) Uiso 0.50 1 d PD B 1 H78A H 1.1560 0.3513 0.6030 0.189 Uiso 0.50 1 calc PR B 1 H78B H 1.1788 0.3889 0.6401 0.189 Uiso 0.50 1 calc PR B 1 H78C H 1.1396 0.4283 0.6106 0.189 Uiso 0.50 1 calc PR B 1 C78' C 1.1689(9) 0.3449(18) 0.6355(9) 0.126(8) Uiso 0.50 1 d PD B 2 H78D H 1.1678 0.3333 0.6121 0.189 Uiso 0.50 1 calc PR B 2 H78E H 1.1906 0.3148 0.6525 0.189 Uiso 0.50 1 calc PR B 2 H78F H 1.1764 0.3959 0.6405 0.189 Uiso 0.50 1 calc PR B 2 C79 C 1.1914(12) 0.360(2) 0.7329(10) 0.078(5) Uiso 0.50 1 d P B 1 H79A H 1.1868 0.3258 0.7491 0.117 Uiso 0.50 1 calc PR B 1 H79B H 1.1789 0.4071 0.7351 0.117 Uiso 0.50 1 calc PR B 1 H79C H 1.2223 0.3661 0.7383 0.117 Uiso 0.50 1 calc PR B 1 C79' C 1.1959(12) 0.372(2) 0.7290(10) 0.078(5) Uiso 0.50 1 d P B 2 H79D H 1.2082 0.3544 0.7530 0.117 Uiso 0.50 1 calc PR B 2 H79E H 1.1837 0.4199 0.7284 0.117 Uiso 0.50 1 calc PR B 2 H79F H 1.2184 0.3735 0.7192 0.117 Uiso 0.50 1 calc PR B 2 C80 C 1.1926(11) 0.2711(15) 0.6870(9) 0.129(9) Uiso 0.50 1 d PD B 1 H80A H 1.2233 0.2724 0.7014 0.193 Uiso 0.50 1 calc PR B 1 H80B H 1.1889 0.2749 0.6625 0.193 Uiso 0.50 1 calc PR B 1 H80C H 1.1802 0.2256 0.6909 0.193 Uiso 0.50 1 calc PR B 1 C80' C 1.1794(10) 0.2459(13) 0.7081(9) 0.129(9) Uiso 0.50 1 d PD B 2 H80D H 1.2083 0.2503 0.7076 0.193 Uiso 0.50 1 calc PR B 2 H80E H 1.1611 0.2186 0.6878 0.193 Uiso 0.50 1 calc PR B 2 H80F H 1.1809 0.2206 0.7294 0.193 Uiso 0.50 1 calc PR B 2 O9 O 0.3237(12) 0.571(2) 0.5320(9) 0.214(8) Uiso 0.50 1 d PD C 1 O9' O 0.3248(12) 0.602(2) 0.5848(10) 0.214(8) Uiso 0.50 1 d PD D 2 O10 O 0.5370(19) 0.308(3) 0.5299(14) 0.277(10) Uiso 0.50 1 d PD E 1 O10' O 0.5772(19) 0.381(3) 0.5440(13) 0.277(10) Uiso 0.50 1 d PD F 2 O11 O 0.8461(12) 0.855(2) 0.4619(12) 0.229(8) Uiso 0.50 1 d PD G 1 O11' O 0.8727(14) 0.855(2) 0.4728(12) 0.229(8) Uiso 0.50 1 d PD H 2 O12 O 0.986(2) 1.023(3) 0.6250(13) 0.295(11) Uiso 0.50 1 d PD I 1 O12' O 1.012(2) 1.042(3) 0.5999(17) 0.295(11) Uiso 0.50 1 d PD J 2 C81 C 0.3304(18) 0.495(2) 0.5301(14) 0.214(8) Uiso 0.50 1 d PD C 1 C81' C 0.3230(18) 0.609(3) 0.5490(12) 0.214(8) Uiso 0.50 1 d PD D 2 C82 C 0.3056(17) 0.490(3) 0.5534(14) 0.214(8) Uiso 0.50 1 d PD C 1 C82' C 0.3519(17) 0.544(3) 0.5517(15) 0.214(8) Uiso 0.50 1 d PD D 2 C83 C 0.3014(19) 0.533(3) 0.5828(13) 0.214(8) Uiso 0.50 1 d PD C 1 C83' C 0.3360(18) 0.477(3) 0.5635(14) 0.214(8) Uiso 0.50 1 d PD D 2 C84 C 0.3002(17) 0.587(3) 0.5550(13) 0.214(8) Uiso 0.50 1 d PD C 1 C84' C 0.3382(18) 0.527(2) 0.5932(13) 0.214(8) Uiso 0.50 1 d PD D 2 C85 C 0.5828(19) 0.320(4) 0.536(2) 0.277(10) Uiso 0.50 1 d PD E 1 C85' C 0.532(2) 0.357(5) 0.5313(19) 0.277(10) Uiso 0.50 1 d PD F 2 C86 C 0.585(2) 0.359(4) 0.5045(19) 0.277(10) Uiso 0.50 1 d PD E 1 C86' C 0.528(3) 0.322(4) 0.4963(19) 0.277(10) Uiso 0.50 1 d PD F 2 C87 C 0.547(2) 0.410(4) 0.501(2) 0.277(10) Uiso 0.50 1 d PD E 1 C87' C 0.550(2) 0.387(5) 0.4871(19) 0.277(10) Uiso 0.50 1 d PD F 2 C88 C 0.511(2) 0.361(4) 0.503(2) 0.277(10) Uiso 0.50 1 d PD E 1 C88' C 0.594(2) 0.394(4) 0.5163(18) 0.277(10) Uiso 0.50 1 d PD F 2 C89 C 0.853(2) 0.816(4) 0.4333(16) 0.229(8) Uiso 0.50 1 d PD G 1 C89' C 0.9091(17) 0.906(3) 0.4812(15) 0.229(8) Uiso 0.50 1 d PD H 2 C90 C 0.888(2) 0.852(3) 0.4241(14) 0.229(8) Uiso 0.50 1 d PD G 1 C90' C 0.9132(19) 0.899(3) 0.4460(16) 0.229(8) Uiso 0.50 1 d PD H 2 C91 C 0.895(2) 0.917(3) 0.4478(16) 0.229(8) Uiso 0.50 1 d PD G 1 C91' C 0.9127(19) 0.818(3) 0.4486(15) 0.229(8) Uiso 0.50 1 d PD H 2 C92 C 0.8777(19) 0.914(3) 0.4770(16) 0.229(8) Uiso 0.50 1 d PD G 1 C92' C 0.8647(19) 0.813(4) 0.4404(15) 0.229(8) Uiso 0.50 1 d PD H 2 C93 C 0.962(3) 0.962(4) 0.602(2) 0.295(11) Uiso 0.50 1 d PD I 1 C93' C 0.965(2) 1.031(4) 0.593(2) 0.295(11) Uiso 0.50 1 d PD J 2 C94 C 0.981(3) 0.933(4) 0.576(2) 0.295(11) Uiso 0.50 1 d PD I 1 C94' C 0.956(3) 0.954(5) 0.580(2) 0.295(11) Uiso 0.50 1 d PD J 2 C95 C 1.015(3) 0.992(5) 0.584(2) 0.295(11) Uiso 0.50 1 d PD I 1 C95' C 0.989(3) 0.916(4) 0.611(2) 0.295(11) Uiso 0.50 1 d PD J 2 C96 C 1.027(2) 1.031(5) 0.620(2) 0.295(11) Uiso 0.50 1 d PD I 1 C96' C 1.023(2) 0.963(3) 0.606(2) 0.295(11) Uiso 0.50 1 d PD J 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0456(3) 0.0460(3) 0.0482(3) -0.0022(2) 0.0182(2) -0.0018(2) Sm2 0.0523(3) 0.0488(3) 0.0559(3) -0.0065(2) 0.0275(3) -0.0055(2) P1 0.0554(18) 0.077(2) 0.087(2) -0.0111(17) 0.0230(17) -0.0165(15) P2 0.080(2) 0.082(2) 0.0554(18) 0.0080(15) 0.0266(16) 0.0136(17) P3 0.0559(16) 0.0469(15) 0.0566(17) -0.0009(12) 0.0195(14) -0.0053(12) P4 0.0581(17) 0.0488(16) 0.079(2) -0.0071(13) 0.0220(16) 0.0027(13) O1 0.054(4) 0.053(4) 0.057(4) -0.001(3) 0.019(3) 0.008(3) O2 0.048(4) 0.075(5) 0.058(5) -0.004(3) 0.025(4) -0.006(3) O3 0.060(4) 0.050(4) 0.056(4) -0.002(3) 0.026(3) -0.007(3) O4 0.048(4) 0.077(5) 0.050(4) 0.004(3) 0.018(3) 0.004(3) O5 0.054(4) 0.074(5) 0.086(5) -0.016(4) 0.016(4) -0.019(4) O6 0.088(5) 0.073(5) 0.054(4) 0.011(4) 0.027(4) 0.004(4) O7 0.072(5) 0.047(4) 0.060(4) -0.004(3) 0.018(4) -0.012(3) O8 0.060(4) 0.045(4) 0.070(5) -0.005(3) 0.030(4) -0.003(3) N1 0.041(4) 0.049(4) 0.045(4) 0.002(3) 0.018(4) 0.004(3) N2 0.036(4) 0.051(4) 0.049(5) -0.001(3) 0.022(4) 0.002(3) N3 0.044(4) 0.047(4) 0.043(4) -0.005(3) 0.018(4) -0.004(3) N4 0.043(4) 0.048(4) 0.045(4) -0.002(3) 0.026(4) -0.002(3) N5 0.103(8) 0.083(7) 0.062(6) -0.019(5) 0.029(6) -0.034(6) N6 0.054(6) 0.094(8) 0.141(10) -0.015(7) 0.026(6) -0.018(6) N7 0.076(7) 0.091(7) 0.089(7) -0.004(6) 0.048(6) -0.029(6) N8 0.067(7) 0.135(10) 0.069(7) 0.028(6) 0.025(6) 0.006(6) N9 0.099(8) 0.088(7) 0.048(6) -0.012(5) 0.031(5) 0.009(6) N10 0.077(7) 0.070(6) 0.094(7) 0.010(5) 0.044(6) -0.010(5) C1 0.057(6) 0.047(6) 0.054(6) -0.001(4) 0.032(5) 0.013(5) C2 0.058(6) 0.056(6) 0.062(7) 0.002(5) 0.031(5) 0.011(5) C3 0.084(9) 0.061(7) 0.085(9) 0.009(6) 0.038(7) 0.029(6) C4 0.080(9) 0.057(7) 0.110(10) 0.001(6) 0.053(8) -0.001(6) C5 0.062(7) 0.062(7) 0.080(8) -0.002(5) 0.041(6) 0.003(5) C6 0.055(6) 0.047(6) 0.058(6) 0.003(4) 0.033(5) 0.001(5) C7 0.050(6) 0.053(6) 0.062(7) -0.013(5) 0.023(5) -0.009(5) C8 0.074(7) 0.055(6) 0.066(7) -0.013(5) 0.040(6) -0.018(5) C9 0.078(8) 0.069(7) 0.057(7) -0.003(5) 0.044(6) -0.002(6) C10 0.079(8) 0.079(8) 0.048(7) -0.011(5) 0.033(6) 0.003(6) C11 0.048(6) 0.083(8) 0.045(6) -0.012(5) 0.011(5) 0.002(5) C12 0.057(6) 0.047(5) 0.052(6) -0.017(4) 0.035(5) -0.005(4) C13 0.055(6) 0.063(6) 0.041(5) -0.006(4) 0.027(5) 0.011(5) C14 0.063(6) 0.042(5) 0.041(5) 0.005(4) 0.024(5) 0.000(4) C15 0.043(5) 0.061(6) 0.051(6) -0.012(5) 0.020(5) -0.004(5) C16 0.038(5) 0.055(6) 0.055(6) 0.005(4) 0.018(5) 0.000(4) C17 0.071(7) 0.050(6) 0.053(6) 0.007(4) 0.032(5) -0.006(5) C18 0.044(5) 0.052(6) 0.061(6) -0.016(5) 0.023(5) -0.005(4) C19 0.062(7) 0.060(7) 0.073(8) 0.015(5) 0.032(6) 0.020(5) C20 0.077(9) 0.078(8) 0.121(11) 0.024(8) 0.036(8) 0.022(7) C21 0.064(7) 0.092(9) 0.079(8) 0.002(6) 0.041(6) 0.004(6) C22 0.065(7) 0.103(9) 0.070(8) -0.006(7) 0.026(6) 0.016(7) C23 0.096(10) 0.044(7) 0.197(16) 0.000(8) 0.073(11) -0.006(6) C24 0.070(7) 0.079(8) 0.054(7) -0.011(5) 0.032(6) -0.032(6) C25 0.104(10) 0.150(13) 0.081(9) -0.030(8) 0.057(8) -0.069(9) C26 0.092(9) 0.103(10) 0.067(8) -0.016(7) 0.033(7) -0.041(8) C27 0.064(7) 0.086(9) 0.092(9) -0.016(7) 0.043(7) -0.013(6) C28 0.084(9) 0.131(12) 0.061(8) 0.007(7) 0.032(7) 0.002(8) C29 0.047(6) 0.049(6) 0.064(7) -0.006(5) 0.032(5) -0.006(4) C30 0.065(7) 0.046(6) 0.074(7) -0.008(5) 0.043(6) -0.001(5) C31 0.122(11) 0.045(6) 0.105(10) -0.011(6) 0.080(9) -0.008(6) C32 0.139(12) 0.047(7) 0.107(10) 0.002(6) 0.078(10) -0.002(7) C33 0.091(9) 0.063(7) 0.077(8) 0.011(6) 0.049(7) 0.016(6) C34 0.060(6) 0.042(5) 0.065(7) 0.005(5) 0.031(5) 0.001(5) C35 0.062(7) 0.039(5) 0.069(7) -0.005(5) 0.038(6) 0.011(5) C36 0.038(5) 0.051(6) 0.049(6) 0.003(4) 0.011(5) 0.002(4) C37 0.062(7) 0.048(6) 0.068(7) 0.005(5) 0.029(6) 0.009(5) C38 0.045(6) 0.051(6) 0.075(8) 0.001(5) 0.016(6) 0.003(5) C39 0.040(6) 0.053(6) 0.101(9) 0.001(6) 0.025(6) 0.000(5) C40 0.051(6) 0.057(6) 0.069(7) -0.003(5) 0.031(6) 0.008(5) C41 0.046(6) 0.058(6) 0.061(7) -0.005(5) 0.020(5) -0.002(5) C42 0.045(6) 0.058(6) 0.057(6) -0.007(5) 0.016(5) -0.004(5) C43 0.037(5) 0.065(6) 0.062(6) -0.005(5) 0.023(5) -0.002(5) C44 0.047(5) 0.064(6) 0.038(5) -0.003(4) 0.014(4) -0.003(5) C45 0.049(6) 0.053(6) 0.040(5) -0.003(4) 0.017(5) 0.000(4) C46 0.058(6) 0.055(6) 0.052(6) -0.001(4) 0.035(5) 0.000(5) C47 0.093(9) 0.056(7) 0.071(8) -0.016(5) 0.048(7) -0.012(6) C48 0.196(17) 0.082(9) 0.118(12) -0.041(8) 0.099(12) -0.019(10) C49 0.112(11) 0.100(10) 0.085(9) -0.023(7) 0.064(8) -0.015(8) C50 0.097(10) 0.117(11) 0.055(8) -0.013(7) 0.031(7) -0.021(8) C51 0.27(2) 0.046(7) 0.141(14) 0.015(8) 0.127(15) -0.009(10) C52 0.068(7) 0.065(7) 0.082(8) -0.005(6) 0.045(6) -0.011(6) C53 0.090(9) 0.106(10) 0.130(12) -0.003(8) 0.083(9) -0.016(8) C54 0.090(9) 0.088(9) 0.088(9) -0.006(7) 0.060(8) 0.005(7) C55 0.117(11) 0.078(9) 0.102(10) 0.007(7) 0.070(9) -0.011(8) C56 0.060(7) 0.088(8) 0.076(8) -0.007(6) -0.001(6) 0.002(6) C57 0.111(11) 0.112(11) 0.069(9) 0.009(7) 0.025(8) -0.018(9) C58 0.143(14) 0.128(13) 0.129(13) -0.069(11) 0.044(11) -0.086(11) C59 0.081(10) 0.111(12) 0.148(14) -0.028(10) 0.038(10) -0.005(9) C60 0.060(9) 0.149(15) 0.23(2) -0.030(14) 0.037(11) -0.025(9) C61 0.131(13) 0.122(12) 0.098(11) -0.013(9) 0.065(10) -0.051(10) C62 0.093(10) 0.097(10) 0.108(11) 0.019(8) 0.039(9) -0.016(8) C63 0.112(13) 0.202(19) 0.127(14) 0.083(13) 0.033(11) 0.059(12) C64 0.084(10) 0.099(10) 0.115(12) 0.004(9) -0.005(9) -0.018(8) C65 0.130(13) 0.153(14) 0.075(10) -0.012(9) 0.050(9) -0.017(11) C66 0.098(10) 0.068(8) 0.113(11) -0.029(7) 0.055(8) -0.010(7) C67 0.141(13) 0.089(10) 0.097(10) -0.015(8) 0.061(10) 0.024(9) C68 0.092(10) 0.103(10) 0.105(11) 0.013(8) 0.048(9) 0.015(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1 2.380(6) . ? Sm1 O3 2.382(6) . ? Sm1 O5 2.489(6) . ? Sm1 O6 2.504(7) . ? Sm1 N1 2.920(7) . ? Sm2 O4 2.321(6) 2_756 ? Sm2 O2 2.336(6) . ? Sm2 O7 2.483(6) . ? Sm2 O8 2.500(6) . ? P1 O5 1.501(7) . ? P1 N6 1.631(11) . ? P1 N7 1.651(10) . ? P1 N5 1.671(9) . ? P2 O6 1.501(7) . ? P2 N8 1.595(10) . ? P2 N9 1.632(9) . ? P2 N10 1.668(9) . ? P3 O7 1.483(6) . ? P3 N12' 1.571(17) . ? P3 N13 1.624(17) . ? P3 N11' 1.640(17) . ? P3 N12 1.641(18) . ? P3 N13' 1.664(13) . ? P3 N11 1.682(13) . ? P4 O8 1.484(6) . ? P4 N14' 1.611(19) . ? P4 N16 1.634(14) . ? P4 N16' 1.639(14) . ? P4 N15' 1.640(16) . ? P4 N14 1.681(14) . ? P4 N15 1.697(15) . ? O1 C1 1.320(10) . ? O2 C7 1.329(11) . ? O3 C29 1.327(10) . ? O4 C35 1.304(11) . ? O4 Sm2 2.321(6) 2_756 ? N1 C16 1.479(10) . ? N1 C13 1.483(10) . ? N1 C14 1.483(10) . ? N2 C17 1.466(10) . ? N2 C15 1.475(11) . ? N2 C18 1.478(10) . ? N3 C42 1.457(11) . ? N3 C44 1.491(10) . ? N3 C41 1.494(11) . ? N4 C43 1.475(11) . ? N4 C45 1.477(10) . ? N4 C46 1.484(11) . ? N5 C58 1.444(13) . ? N5 C57 1.458(14) . ? N6 C59 1.443(15) . ? N6 C60 1.471(15) . ? N7 C61 1.447(14) . ? N7 C62 1.471(15) . ? N8 C64 1.480(15) . ? N8 C63 1.493(15) . ? N9 C65 1.426(14) . ? N9 C66 1.467(14) . ? N10 C67 1.424(13) . ? N10 C68 1.478(14) . ? N11 C69 1.463(16) . ? N11 C70 1.489(17) . ? N11' C70' 1.472(16) . ? N11' C69' 1.508(16) . ? N12 C71 1.437(17) . ? N12 C72 1.491(18) . ? N12' C72' 1.480(17) . ? N12' C71' 1.483(17) . ? N13 C73 1.453(17) . ? N13 C74 1.519(17) . ? N13' C74' 1.463(17) . ? N13' C73' 1.528(17) . ? N14 C76 1.472(17) . ? N14 C75 1.504(17) . ? N14' C75' 1.482(17) . ? N14' C76' 1.506(17) . ? N15 C78 1.460(18) . ? N15 C77 1.462(18) . ? N15' C77' 1.452(18) . ? N15' C78' 1.493(18) . ? N16 C79 1.48(4) . ? N16 C80 1.485(17) . ? N16' C80' 1.493(18) . ? N16' C79' 1.51(4) . ? C1 C6 1.408(13) . ? C1 C2 1.432(12) . ? C2 C3 1.386(14) . ? C2 C19 1.553(14) . ? C3 C4 1.385(15) . ? C3 H3 0.9400 . ? C4 C5 1.384(14) . ? C4 C23 1.551(14) . ? C5 C6 1.369(13) . ? C5 H5 0.9400 . ? C6 C13 1.503(12) . ? C7 C12 1.427(12) . ? C7 C8 1.442(13) . ? C8 C9 1.381(14) . ? C8 C24 1.520(14) . ? C9 C10 1.382(14) . ? C9 H9 0.9400 . ? C10 C11 1.382(14) . ? C10 C28 1.557(15) . ? C11 C12 1.381(13) . ? C11 H11 0.9400 . ? C12 C18 1.508(12) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.511(11) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.531(12) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C21 1.519(13) . ? C19 C22 1.528(14) . ? C19 C20 1.547(13) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.532(14) . ? C24 C26 1.539(14) . ? C24 C27 1.542(15) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 C34 1.394(13) . ? C29 C30 1.413(12) . ? C30 C31 1.375(13) . ? C30 C47 1.545(14) . ? C31 C32 1.387(15) . ? C31 H31 0.9400 . ? C32 C33 1.415(15) . ? C32 C51 1.510(15) . ? C33 C34 1.428(13) . ? C33 H33 0.9400 . ? C34 C41 1.513(12) . ? C35 C36 1.439(13) . ? C35 C40 1.442(13) . ? C36 C37 1.378(12) . ? C36 C46 1.489(12) . ? C37 C38 1.428(13) . ? C37 H37 0.9400 . ? C38 C39 1.367(14) . ? C38 C56 1.525(13) . ? C39 C40 1.401(14) . ? C39 H39 0.9400 . ? C40 C52 1.536(14) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 C43 1.535(12) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 C45 1.509(12) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C47 C50 1.499(16) . ? C47 C48 1.526(14) . ? C47 C49 1.528(15) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C49 H49C 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 H50C 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C52 C54 1.531(14) . ? C52 C55 1.544(15) . ? C52 C53 1.549(14) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C55 H55C 0.9700 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C56 H56C 0.9700 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C57 H57C 0.9700 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C58 H58C 0.9700 . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C59 H59C 0.9700 . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C60 H60C 0.9700 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C61 H61C 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C62 H62C 0.9700 . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C63 H63C 0.9700 . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C64 H64C 0.9700 . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C65 H65C 0.9700 . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C66 H66C 0.9700 . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C67 H67C 0.9700 . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C68 H68C 0.9700 . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C69 H69C 0.9700 . ? C69' H69D 0.9700 . ? C69' H69E 0.9700 . ? C69' H69F 0.9700 . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C70 H70C 0.9700 . ? C70' H70D 0.9700 . ? C70' H70E 0.9700 . ? C70' H70F 0.9700 . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C71 H71C 0.9700 . ? C71' H71D 0.9700 . ? C71' H71E 0.9700 . ? C71' H71F 0.9700 . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C72 H72C 0.9700 . ? C72' H72D 0.9700 . ? C72' H72E 0.9700 . ? C72' H72F 0.9700 . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C73 H73C 0.9700 . ? C73' H73D 0.9700 . ? C73' H73E 0.9700 . ? C73' H73F 0.9700 . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C74 H74C 0.9700 . ? C74' H74D 0.9700 . ? C74' H74E 0.9700 . ? C74' H74F 0.9700 . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C75 H75C 0.9700 . ? C75' H75D 0.9700 . ? C75' H75E 0.9700 . ? C75' H75F 0.9700 . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C76 H76C 0.9700 . ? C76' H76D 0.9700 . ? C76' H76E 0.9700 . ? C76' H76F 0.9700 . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C77 H77C 0.9700 . ? C77' H77D 0.9700 . ? C77' H77E 0.9700 . ? C77' H77F 0.9700 . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C78 H78C 0.9700 . ? C78' H78D 0.9700 . ? C78' H78E 0.9700 . ? C78' H78F 0.9700 . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C79 H79C 0.9700 . ? C79' H79D 0.9700 . ? C79' H79E 0.9700 . ? C79' H79F 0.9700 . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C80 H80C 0.9700 . ? C80' H80D 0.9700 . ? C80' H80E 0.9700 . ? C80' H80F 0.9700 . ? O9 C81 1.427(19) . ? O9 C84 1.46(2) . ? O9' C84' 1.439(19) . ? O9' C81' 1.46(2) . ? O10 C85 1.46(2) . ? O10 C88 1.47(2) . ? O10' C88' 1.45(2) . ? O10' C85' 1.47(2) . ? O11 C89 1.46(2) . ? O11 C92 1.48(2) . ? O11' C89' 1.47(2) . ? O11' C92' 1.47(2) . ? O12 C96 1.46(2) . ? O12 C93 1.48(2) . ? O12' C93' 1.47(2) . ? O12' C96' 1.49(2) . ? C81 C82 1.48(2) . ? C81' C82' 1.50(2) . ? C82 C83 1.48(2) . ? C82' C83' 1.49(2) . ? C83 C84 1.51(2) . ? C83' C84' 1.50(2) . ? C85 C86 1.49(2) . ? C85' C86' 1.53(2) . ? C86 C87 1.52(2) . ? C86' C87' 1.50(2) . ? C87 C88 1.51(2) . ? C87' C88' 1.51(2) . ? C89 C90 1.50(2) . ? C89' C90' 1.50(2) . ? C90 C91 1.51(2) . ? C90' C91' 1.49(2) . ? C91 C92 1.51(2) . ? C91' C92' 1.50(2) . ? C93 C94 1.51(2) . ? C93' C94' 1.51(2) . ? C94 C95 1.50(2) . ? C94' C95' 1.50(2) . ? C95 C96 1.54(2) . ? C95' C96' 1.50(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sm1 O3 159.4(2) . . ? O1 Sm1 O5 103.3(2) . . ? O3 Sm1 O5 88.3(2) . . ? O1 Sm1 O6 87.7(2) . . ? O3 Sm1 O6 109.0(2) . . ? O5 Sm1 O6 92.6(2) . . ? O1 Sm1 N1 73.9(2) . . ? O3 Sm1 N1 94.6(2) . . ? O5 Sm1 N1 177.1(2) . . ? O6 Sm1 N1 86.4(2) . . ? O4 Sm2 O2 93.2(2) 2_756 . ? O4 Sm2 O7 95.4(2) 2_756 . ? O2 Sm2 O7 102.9(2) . . ? O4 Sm2 O8 103.9(2) 2_756 . ? O2 Sm2 O8 96.1(2) . . ? O7 Sm2 O8 152.0(2) . . ? O5 P1 N6 108.5(5) . . ? O5 P1 N7 117.8(5) . . ? N6 P1 N7 105.2(6) . . ? O5 P1 N5 109.4(5) . . ? N6 P1 N5 113.0(6) . . ? N7 P1 N5 102.9(5) . . ? O6 P2 N8 107.8(5) . . ? O6 P2 N9 109.4(5) . . ? N8 P2 N9 113.8(5) . . ? O6 P2 N10 118.4(5) . . ? N8 P2 N10 102.7(6) . . ? N9 P2 N10 104.9(5) . . ? O7 P3 N12' 118.1(7) . . ? O7 P3 N13 112.3(7) . . ? N12' P3 N13 120.5(9) . . ? O7 P3 N11' 114.5(6) . . ? N12' P3 N11' 112.1(9) . . ? N13 P3 N11' 70.0(8) . . ? O7 P3 N12 110.2(6) . . ? N12' P3 N12 20.5(8) . . ? N13 P3 N12 112.7(9) . . ? N11' P3 N12 129.6(9) . . ? O7 P3 N13' 112.0(7) . . ? N12' P3 N13' 100.6(8) . . ? N13 P3 N13' 28.9(7) . . ? N11' P3 N13' 96.6(8) . . ? N12 P3 N13' 87.2(8) . . ? O7 P3 N11 105.4(6) . . ? N12' P3 N11 85.6(8) . . ? N13 P3 N11 109.7(9) . . ? N11' P3 N11 40.4(7) . . ? N12 P3 N11 106.0(8) . . ? N13' P3 N11 132.9(9) . . ? O8 P4 N14' 111.1(7) . . ? O8 P4 N16 109.1(7) . . ? N14' P4 N16 116.7(9) . . ? O8 P4 N16' 109.0(7) . . ? N14' P4 N16' 95.8(9) . . ? N16 P4 N16' 24.2(8) . . ? O8 P4 N15' 121.1(10) . . ? N14' P4 N15' 107.3(12) . . ? N16 P4 N15' 90.5(11) . . ? N16' P4 N15' 109.6(11) . . ? O8 P4 N14 108.8(7) . . ? N14' P4 N14 18.3(10) . . ? N16 P4 N14 131.6(9) . . ? N16' P4 N14 113.1(9) . . ? N15' P4 N14 94.7(12) . . ? O8 P4 N15 110.5(10) . . ? N14' P4 N15 110.9(12) . . ? N16 P4 N15 97.8(11) . . ? N16' P4 N15 118.7(11) . . ? N15' P4 N15 11.1(16) . . ? N14 P4 N15 96.0(11) . . ? C1 O1 Sm1 138.9(6) . . ? C7 O2 Sm2 142.0(6) . . ? C29 O3 Sm1 140.5(5) . . ? C35 O4 Sm2 145.0(6) . 2_756 ? P1 O5 Sm1 172.1(5) . . ? P2 O6 Sm1 171.3(5) . . ? P3 O7 Sm2 154.4(4) . . ? P4 O8 Sm2 150.2(4) . . ? C16 N1 C13 109.3(7) . . ? C16 N1 C14 105.8(7) . . ? C13 N1 C14 110.6(7) . . ? C16 N1 Sm1 104.5(5) . . ? C13 N1 Sm1 100.9(5) . . ? C14 N1 Sm1 125.0(5) . . ? C17 N2 C15 107.0(7) . . ? C17 N2 C18 108.4(7) . . ? C15 N2 C18 108.4(7) . . ? C42 N3 C44 106.6(7) . . ? C42 N3 C41 110.2(7) . . ? C44 N3 C41 106.5(7) . . ? C43 N4 C45 106.8(6) . . ? C43 N4 C46 107.9(7) . . ? C45 N4 C46 108.2(7) . . ? C58 N5 C57 115.0(10) . . ? C58 N5 P1 122.6(9) . . ? C57 N5 P1 118.0(8) . . ? C59 N6 C60 115.1(11) . . ? C59 N6 P1 121.9(9) . . ? C60 N6 P1 120.3(10) . . ? C61 N7 C62 114.5(11) . . ? C61 N7 P1 123.6(10) . . ? C62 N7 P1 120.5(8) . . ? C64 N8 C63 112.8(11) . . ? C64 N8 P2 121.2(9) . . ? C63 N8 P2 122.7(9) . . ? C65 N9 C66 114.0(10) . . ? C65 N9 P2 120.3(9) . . ? C66 N9 P2 119.3(8) . . ? C67 N10 C68 114.8(10) . . ? C67 N10 P2 118.7(9) . . ? C68 N10 P2 126.0(9) . . ? C69 N11 C70 117.2(17) . . ? C69 N11 P3 123.7(13) . . ? C70 N11 P3 118.2(14) . . ? C70' N11' C69' 126.4(18) . . ? C70' N11' P3 113.7(14) . . ? C69' N11' P3 119.8(14) . . ? C71 N12 C72 120(2) . . ? C71 N12 P3 125.5(17) . . ? C72 N12 P3 113.5(18) . . ? C72' N12' C71' 109(2) . . ? C72' N12' P3 125(2) . . ? C71' N12' P3 125.3(16) . . ? C73 N13 C74 110.8(19) . . ? C73 N13 P3 126.4(16) . . ? C74 N13 P3 112.9(14) . . ? C74' N13' C73' 104.4(18) . . ? C74' N13' P3 124.4(15) . . ? C73' N13' P3 112.8(15) . . ? C76 N14 C75 109.5(19) . . ? C76 N14 P4 121.4(16) . . ? C75 N14 P4 109.5(15) . . ? C75' N14' C76' 101.9(19) . . ? C75' N14' P4 125.0(17) . . ? C76' N14' P4 110.6(16) . . ? C78 N15 C77 103(2) . . ? C78 N15 P4 127(2) . . ? C77 N15 P4 123(2) . . ? C77' N15' C78' 99(2) . . ? C77' N15' P4 119.3(19) . . ? C78' N15' P4 118(2) . . ? C79 N16 C80 115(2) . . ? C79 N16 P4 120.2(19) . . ? C80 N16 P4 121.3(18) . . ? C80' N16' C79' 109(2) . . ? C80' N16' P4 122.9(17) . . ? C79' N16' P4 120.0(18) . . ? O1 C1 C6 119.4(8) . . ? O1 C1 C2 122.9(9) . . ? C6 C1 C2 117.8(9) . . ? C3 C2 C1 117.7(10) . . ? C3 C2 C19 121.8(9) . . ? C1 C2 C19 120.5(9) . . ? C4 C3 C2 124.4(10) . . ? C4 C3 H3 117.8 . . ? C2 C3 H3 117.8 . . ? C5 C4 C3 116.5(10) . . ? C5 C4 C23 122.4(11) . . ? C3 C4 C23 121.0(11) . . ? C6 C5 C4 122.2(11) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C1 121.3(9) . . ? C5 C6 C13 117.9(9) . . ? C1 C6 C13 120.7(8) . . ? O2 C7 C12 119.0(9) . . ? O2 C7 C8 122.1(9) . . ? C12 C7 C8 118.9(9) . . ? C9 C8 C7 117.2(9) . . ? C9 C8 C24 122.2(9) . . ? C7 C8 C24 120.6(10) . . ? C8 C9 C10 124.2(10) . . ? C8 C9 H9 117.9 . . ? C10 C9 H9 117.9 . . ? C11 C10 C9 118.0(10) . . ? C11 C10 C28 120.3(10) . . ? C9 C10 C28 121.7(10) . . ? C12 C11 C10 121.9(10) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C7 119.7(9) . . ? C11 C12 C18 120.8(9) . . ? C7 C12 C18 119.4(9) . . ? N1 C13 C6 117.1(7) . . ? N1 C13 H13A 108.0 . . ? C6 C13 H13A 108.0 . . ? N1 C13 H13B 108.0 . . ? C6 C13 H13B 108.0 . . ? H13A C13 H13B 107.3 . . ? N1 C14 C15 110.9(7) . . ? N1 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.0 . . ? N2 C15 C14 112.6(7) . . ? N2 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? N2 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? N1 C16 C17 110.9(7) . . ? N1 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N2 C17 C16 111.1(7) . . ? N2 C17 H17A 109.4 . . ? C16 C17 H17A 109.4 . . ? N2 C17 H17B 109.4 . . ? C16 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N2 C18 C12 114.6(7) . . ? N2 C18 H18A 108.6 . . ? C12 C18 H18A 108.6 . . ? N2 C18 H18B 108.6 . . ? C12 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C21 C19 C22 109.2(9) . . ? C21 C19 C20 107.8(9) . . ? C22 C19 C20 107.6(9) . . ? C21 C19 C2 109.7(9) . . ? C22 C19 C2 110.1(8) . . ? C20 C19 C2 112.4(9) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C4 C23 H23A 109.5 . . ? C4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 C24 C25 112.1(9) . . ? C8 C24 C26 110.2(9) . . ? C25 C24 C26 106.6(9) . . ? C8 C24 C27 110.2(9) . . ? C25 C24 C27 108.6(10) . . ? C26 C24 C27 109.1(9) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C10 C28 H28A 109.5 . . ? C10 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C10 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C34 118.3(8) . . ? O3 C29 C30 122.7(9) . . ? C34 C29 C30 119.0(9) . . ? C31 C30 C29 118.4(10) . . ? C31 C30 C47 120.7(9) . . ? C29 C30 C47 120.9(9) . . ? C30 C31 C32 125.4(10) . . ? C30 C31 H31 117.3 . . ? C32 C31 H31 117.3 . . ? C31 C32 C33 116.0(10) . . ? C31 C32 C51 122.9(11) . . ? C33 C32 C51 120.8(12) . . ? C32 C33 C34 120.2(10) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C29 C34 C33 120.8(9) . . ? C29 C34 C41 122.9(8) . . ? C33 C34 C41 115.7(9) . . ? O4 C35 C36 120.4(9) . . ? O4 C35 C40 123.7(9) . . ? C36 C35 C40 115.9(9) . . ? C37 C36 C35 122.7(9) . . ? C37 C36 C46 118.6(9) . . ? C35 C36 C46 118.5(8) . . ? C36 C37 C38 120.7(10) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C39 C38 C37 116.7(10) . . ? C39 C38 C56 122.5(10) . . ? C37 C38 C56 120.8(10) . . ? C38 C39 C40 125.2(10) . . ? C38 C39 H39 117.4 . . ? C40 C39 H39 117.4 . . ? C39 C40 C35 118.7(9) . . ? C39 C40 C52 121.8(9) . . ? C35 C40 C52 119.5(9) . . ? N3 C41 C34 116.5(8) . . ? N3 C41 H41A 108.2 . . ? C34 C41 H41A 108.2 . . ? N3 C41 H41B 108.2 . . ? C34 C41 H41B 108.2 . . ? H41A C41 H41B 107.3 . . ? N3 C42 C43 111.0(7) . . ? N3 C42 H42A 109.4 . . ? C43 C42 H42A 109.4 . . ? N3 C42 H42B 109.4 . . ? C43 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? N4 C43 C42 111.3(7) . . ? N4 C43 H43A 109.4 . . ? C42 C43 H43A 109.4 . . ? N4 C43 H43B 109.4 . . ? C42 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? N3 C44 C45 110.6(7) . . ? N3 C44 H44A 109.5 . . ? C45 C44 H44A 109.5 . . ? N3 C44 H44B 109.5 . . ? C45 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? N4 C45 C44 111.1(7) . . ? N4 C45 H45A 109.4 . . ? C44 C45 H45A 109.4 . . ? N4 C45 H45B 109.4 . . ? C44 C45 H45B 109.4 . . ? H45A C45 H45B 108.0 . . ? N4 C46 C36 117.1(7) . . ? N4 C46 H46A 108.0 . . ? C36 C46 H46A 108.0 . . ? N4 C46 H46B 108.0 . . ? C36 C46 H46B 108.0 . . ? H46A C46 H46B 107.3 . . ? C50 C47 C48 107.3(11) . . ? C50 C47 C49 110.5(10) . . ? C48 C47 C49 107.9(10) . . ? C50 C47 C30 110.3(9) . . ? C48 C47 C30 112.0(10) . . ? C49 C47 C30 108.8(9) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C32 C51 H51A 109.5 . . ? C32 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C32 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C54 C52 C40 109.5(9) . . ? C54 C52 C55 109.6(10) . . ? C40 C52 C55 109.9(9) . . ? C54 C52 C53 107.9(9) . . ? C40 C52 C53 111.7(10) . . ? C55 C52 C53 108.1(10) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C38 C56 H56A 109.5 . . ? C38 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C38 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N5 C57 H57A 109.5 . . ? N5 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N5 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N5 C58 H58A 109.5 . . ? N5 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? N5 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N6 C59 H59A 109.5 . . ? N6 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? N6 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N6 C60 H60A 109.5 . . ? N6 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N6 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N7 C61 H61A 109.5 . . ? N7 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N7 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N7 C62 H62A 109.5 . . ? N7 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N7 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N8 C63 H63A 109.5 . . ? N8 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N8 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N8 C64 H64A 109.5 . . ? N8 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N8 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N9 C65 H65A 109.5 . . ? N9 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N9 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N9 C66 H66A 109.5 . . ? N9 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N9 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N10 C67 H67A 109.5 . . ? N10 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N10 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N10 C68 H68A 109.5 . . ? N10 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? N10 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N11' C69' H69D 109.5 . . ? N11' C69' H69E 109.5 . . ? H69D C69' H69E 109.5 . . ? N11' C69' H69F 109.5 . . ? H69D C69' H69F 109.5 . . ? H69E C69' H69F 109.5 . . ? N11' C70' H70D 109.5 . . ? N11' C70' H70E 109.5 . . ? H70D C70' H70E 109.5 . . ? N11' C70' H70F 109.5 . . ? H70D C70' H70F 109.5 . . ? H70E C70' H70F 109.5 . . ? N12' C71' H71D 109.5 . . ? N12' C71' H71E 109.5 . . ? H71D C71' H71E 109.5 . . ? N12' C71' H71F 109.5 . . ? H71D C71' H71F 109.5 . . ? H71E C71' H71F 109.5 . . ? N12' C72' H72D 109.5 . . ? N12' C72' H72E 109.5 . . ? H72D C72' H72E 109.5 . . ? N12' C72' H72F 109.5 . . ? H72D C72' H72F 109.5 . . ? H72E C72' H72F 109.5 . . ? N13' C73' H73D 109.5 . . ? N13' C73' H73E 109.5 . . ? H73D C73' H73E 109.5 . . ? N13' C73' H73F 109.5 . . ? H73D C73' H73F 109.5 . . ? H73E C73' H73F 109.5 . . ? N13' C74' H74D 109.5 . . ? N13' C74' H74E 109.5 . . ? H74D C74' H74E 109.5 . . ? N13' C74' H74F 109.5 . . ? H74D C74' H74F 109.5 . . ? H74E C74' H74F 109.5 . . ? N14' C75' H75D 109.5 . . ? N14' C75' H75E 109.5 . . ? H75D C75' H75E 109.5 . . ? N14' C75' H75F 109.5 . . ? H75D C75' H75F 109.5 . . ? H75E C75' H75F 109.5 . . ? N14' C76' H76D 109.5 . . ? N14' C76' H76E 109.5 . . ? H76D C76' H76E 109.5 . . ? N14' C76' H76F 109.5 . . ? H76D C76' H76F 109.5 . . ? H76E C76' H76F 109.5 . . ? N15' C77' H77D 109.5 . . ? N15' C77' H77E 109.5 . . ? H77D C77' H77E 109.5 . . ? N15' C77' H77F 109.5 . . ? H77D C77' H77F 109.5 . . ? H77E C77' H77F 109.5 . . ? N15' C78' H78D 109.5 . . ? N15' C78' H78E 109.5 . . ? H78D C78' H78E 109.5 . . ? N15' C78' H78F 109.5 . . ? H78D C78' H78F 109.5 . . ? H78E C78' H78F 109.5 . . ? N16' C79' H79D 109.5 . . ? N16' C79' H79E 109.5 . . ? H79D C79' H79E 109.5 . . ? N16' C79' H79F 109.5 . . ? H79D C79' H79F 109.5 . . ? H79E C79' H79F 109.5 . . ? N16' C80' H80D 109.5 . . ? N16' C80' H80E 109.5 . . ? H80D C80' H80E 109.5 . . ? N16' C80' H80F 109.5 . . ? H80D C80' H80F 109.5 . . ? H80E C80' H80F 109.5 . . ? C81 O9 C84 111(4) . . ? C84' O9' C81' 103(4) . . ? C85 O10 C88 108(5) . . ? C88' O10' C85' 114(6) . . ? C89 O11 C92 114(4) . . ? C89' O11' C92' 114(5) . . ? C96 O12 C93 107(6) . . ? C93' O12' C96' 96(6) . . ? O9 C81 C82 83(3) . . ? O9' C81' C82' 94(4) . . ? C81 C82 C83 138(5) . . ? C83' C82' C81' 113(4) . . ? C82 C83 C84 74(4) . . ? C82' C83' C84' 81(4) . . ? O9 C84 C83 119(4) . . ? O9' C84' C83' 118(4) . . ? O10 C85 C86 108(6) . . ? O10' C85' C86' 100(5) . . ? C85 C86 C87 95(6) . . ? C87' C86' C85' 92(6) . . ? C88 C87 C86 106(6) . . ? C86' C87' C88' 106(7) . . ? O10 C88 C87 101(6) . . ? O10' C88' C87' 95(5) . . ? O11 C89 C90 110(5) . . ? O11' C89' C90' 95(4) . . ? C89 C90 C91 98(5) . . ? C91' C90' C89' 90(4) . . ? C90 C91 C92 118(5) . . ? C90' C91' C92' 95(5) . . ? O11 C92 C91 97(4) . . ? O11' C92' C91' 86(4) . . ? O12 C93 C94 117(6) . . ? O12' C93' C94' 105(6) . . ? C95 C94 C93 93(6) . . ? C95' C94' C93' 99(6) . . ? C94 C95 C96 117(7) . . ? C94' C95' C96' 88(6) . . ? O12 C96 C95 99(5) . . ? O12' C96' C95' 115(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 O3 Sm1 O1 C1 80.7(11) . . . . ? O5 Sm1 O1 C1 -156.3(9) . . . . ? O6 Sm1 O1 C1 -64.1(9) . . . . ? N1 Sm1 O1 C1 22.8(8) . . . . ? O4 Sm2 O2 C7 -165.3(9) 2_756 . . . ? O7 Sm2 O2 C7 -69.0(10) . . . . ? O8 Sm2 O2 C7 90.3(9) . . . . ? O1 Sm1 O3 C29 75.8(11) . . . . ? O5 Sm1 O3 C29 -49.5(9) . . . . ? O6 Sm1 O3 C29 -141.7(9) . . . . ? N1 Sm1 O3 C29 130.5(9) . . . . ? N6 P1 O5 Sm1 132(3) . . . . ? N7 P1 O5 Sm1 13(4) . . . . ? N5 P1 O5 Sm1 -104(4) . . . . ? O1 Sm1 O5 P1 -125(4) . . . . ? O3 Sm1 O5 P1 38(4) . . . . ? O6 Sm1 O5 P1 147(4) . . . . ? N1 Sm1 O5 P1 -143(4) . . . . ? N8 P2 O6 Sm1 -114(3) . . . . ? N9 P2 O6 Sm1 122(3) . . . . ? N10 P2 O6 Sm1 2(3) . . . . ? O1 Sm1 O6 P2 50(3) . . . . ? O3 Sm1 O6 P2 -117(3) . . . . ? O5 Sm1 O6 P2 154(3) . . . . ? N1 Sm1 O6 P2 -24(3) . . . . ? N12' P3 O7 Sm2 -38.7(13) . . . . ? N13 P3 O7 Sm2 174.0(10) . . . . ? N11' P3 O7 Sm2 96.6(11) . . . . ? N12 P3 O7 Sm2 -59.5(11) . . . . ? N13' P3 O7 Sm2 -154.7(10) . . . . ? N11 P3 O7 Sm2 54.6(11) . . . . ? O4 Sm2 O7 P3 46.8(10) 2_756 . . . ? O2 Sm2 O7 P3 -47.7(10) . . . . ? O8 Sm2 O7 P3 -179.4(7) . . . . ? N14' P4 O8 Sm2 -172.5(10) . . . . ? N16 P4 O8 Sm2 57.5(11) . . . . ? N16' P4 O8 Sm2 83.2(11) . . . . ? N15' P4 O8 Sm2 -45.3(14) . . . . ? N14 P4 O8 Sm2 -153.1(9) . . . . ? N15 P4 O8 Sm2 -49.0(13) . . . . ? O4 Sm2 O8 P4 -46.1(9) 2_756 . . . ? O2 Sm2 O8 P4 48.7(8) . . . . ? O7 Sm2 O8 P4 -178.5(6) . . . . ? O1 Sm1 N1 C16 142.6(5) . . . . ? O3 Sm1 N1 C16 -19.9(5) . . . . ? O5 Sm1 N1 C16 161(4) . . . . ? O6 Sm1 N1 C16 -128.7(5) . . . . ? O1 Sm1 N1 C13 29.2(5) . . . . ? O3 Sm1 N1 C13 -133.4(5) . . . . ? O5 Sm1 N1 C13 48(4) . . . . ? O6 Sm1 N1 C13 117.9(5) . . . . ? O1 Sm1 N1 C14 -95.8(6) . . . . ? O3 Sm1 N1 C14 101.7(6) . . . . ? O5 Sm1 N1 C14 -77(4) . . . . ? O6 Sm1 N1 C14 -7.1(6) . . . . ? O5 P1 N5 C58 167.5(11) . . . . ? N6 P1 N5 C58 -71.5(13) . . . . ? N7 P1 N5 C58 41.5(13) . . . . ? O5 P1 N5 C57 -37.2(11) . . . . ? N6 P1 N5 C57 83.8(10) . . . . ? N7 P1 N5 C57 -163.3(9) . . . . ? O5 P1 N6 C59 8.2(13) . . . . ? N7 P1 N6 C59 135.2(12) . . . . ? N5 P1 N6 C59 -113.2(12) . . . . ? O5 P1 N6 C60 168.9(12) . . . . ? N7 P1 N6 C60 -64.1(13) . . . . ? N5 P1 N6 C60 47.4(14) . . . . ? O5 P1 N7 C61 96.9(10) . . . . ? N6 P1 N7 C61 -24.2(11) . . . . ? N5 P1 N7 C61 -142.7(10) . . . . ? O5 P1 N7 C62 -68.8(11) . . . . ? N6 P1 N7 C62 170.1(9) . . . . ? N5 P1 N7 C62 51.6(10) . . . . ? O6 P2 N8 C64 -38.6(12) . . . . ? N9 P2 N8 C64 82.9(11) . . . . ? N10 P2 N8 C64 -164.3(10) . . . . ? O6 P2 N8 C63 163.5(12) . . . . ? N9 P2 N8 C63 -75.1(14) . . . . ? N10 P2 N8 C63 37.8(13) . . . . ? O6 P2 N9 C65 162.6(10) . . . . ? N8 P2 N9 C65 42.1(12) . . . . ? N10 P2 N9 C65 -69.4(11) . . . . ? O6 P2 N9 C66 12.6(10) . . . . ? N8 P2 N9 C66 -108.0(9) . . . . ? N10 P2 N9 C66 140.5(9) . . . . ? O6 P2 N10 C67 -63.6(11) . . . . ? N8 P2 N10 C67 54.9(10) . . . . ? N9 P2 N10 C67 174.1(9) . . . . ? O6 P2 N10 C68 108.8(10) . . . . ? N8 P2 N10 C68 -132.7(10) . . . . ? N9 P2 N10 C68 -13.5(11) . . . . ? O7 P3 N11 C69 -158.2(16) . . . . ? N12' P3 N11 C69 -40.3(18) . . . . ? N13 P3 N11 C69 80.6(18) . . . . ? N11' P3 N11 C69 92(2) . . . . ? N12 P3 N11 C69 -41.3(19) . . . . ? N13' P3 N11 C69 60(2) . . . . ? O7 P3 N11 C70 33.1(17) . . . . ? N12' P3 N11 C70 151.0(17) . . . . ? N13 P3 N11 C70 -88.0(17) . . . . ? N11' P3 N11 C70 -76.7(18) . . . . ? N12 P3 N11 C70 150.0(16) . . . . ? N13' P3 N11 C70 -108.6(17) . . . . ? O7 P3 N11' C70' -41.2(17) . . . . ? N12' P3 N11' C70' 96.8(17) . . . . ? N13 P3 N11' C70' -147.4(18) . . . . ? N12 P3 N11' C70' 109.2(17) . . . . ? N13' P3 N11' C70' -159.0(16) . . . . ? N11 P3 N11' C70' 44.0(15) . . . . ? O7 P3 N11' C69' 138.8(15) . . . . ? N12' P3 N11' C69' -83.2(18) . . . . ? N13 P3 N11' C69' 32.6(16) . . . . ? N12 P3 N11' C69' -70.8(19) . . . . ? N13' P3 N11' C69' 21.1(18) . . . . ? N11 P3 N11' C69' -136(2) . . . . ? O7 P3 N12 C71 -126.1(19) . . . . ? N12' P3 N12 C71 117(4) . . . . ? N13 P3 N12 C71 0(2) . . . . ? N11' P3 N12 C71 83(2) . . . . ? N13' P3 N12 C71 -14(2) . . . . ? N11 P3 N12 C71 120(2) . . . . ? O7 P3 N12 C72 64.7(19) . . . . ? N12' P3 N12 C72 -52(3) . . . . ? N13 P3 N12 C72 -169.0(18) . . . . ? N11' P3 N12 C72 -87(2) . . . . ? N13' P3 N12 C72 177.1(19) . . . . ? N11 P3 N12 C72 -49(2) . . . . ? O7 P3 N12' C72' 3(2) . . . . ? N13 P3 N12' C72' 148(2) . . . . ? N11' P3 N12' C72' -133(2) . . . . ? N12 P3 N12' C72' 75(3) . . . . ? N13' P3 N12' C72' 125(2) . . . . ? N11 P3 N12' C72' -102(2) . . . . ? O7 P3 N12' C71' 172.7(17) . . . . ? N13 P3 N12' C71' -43(2) . . . . ? N11' P3 N12' C71' 36(2) . . . . ? N12 P3 N12' C71' -115(4) . . . . ? N13' P3 N12' C71' -65(2) . . . . ? N11 P3 N12' C71' 68(2) . . . . ? O7 P3 N13 C73 -165.2(19) . . . . ? N12' P3 N13 C73 48(2) . . . . ? N11' P3 N13 C73 -56(2) . . . . ? N12 P3 N13 C73 70(2) . . . . ? N13' P3 N13 C73 100(3) . . . . ? N11 P3 N13 C73 -48(2) . . . . ? O7 P3 N13 C74 52.7(17) . . . . ? N12' P3 N13 C74 -93.7(16) . . . . ? N11' P3 N13 C74 161.8(18) . . . . ? N12 P3 N13 C74 -72.5(17) . . . . ? N13' P3 N13 C74 -42.6(18) . . . . ? N11 P3 N13 C74 169.6(15) . . . . ? O7 P3 N13' C74' -44(2) . . . . ? N12' P3 N13' C74' -169.8(18) . . . . ? N13 P3 N13' C74' 53(2) . . . . ? N11' P3 N13' C74' 76.2(19) . . . . ? N12 P3 N13' C74' -154.2(19) . . . . ? N11 P3 N13' C74' 96(2) . . . . ? O7 P3 N13' C73' 84.3(16) . . . . ? N12' P3 N13' C73' -41.9(17) . . . . ? N13 P3 N13' C73' -179(3) . . . . ? N11' P3 N13' C73' -155.9(16) . . . . ? N12 P3 N13' C73' -26.3(16) . . . . ? N11 P3 N13' C73' -135.7(16) . . . . ? O8 P4 N14 C76 176.1(17) . . . . ? N14' P4 N14 C76 -83(4) . . . . ? N16 P4 N14 C76 -44(2) . . . . ? N16' P4 N14 C76 -63(2) . . . . ? N15' P4 N14 C76 51(2) . . . . ? N15 P4 N14 C76 62(2) . . . . ? O8 P4 N14 C75 -54.8(16) . . . . ? N14' P4 N14 C75 46(3) . . . . ? N16 P4 N14 C75 85.1(18) . . . . ? N16' P4 N14 C75 66.5(17) . . . . ? N15' P4 N14 C75 -179.9(17) . . . . ? N15 P4 N14 C75 -168.9(17) . . . . ? O8 P4 N14' C75' 2(2) . . . . ? N16 P4 N14' C75' 127.5(19) . . . . ? N16' P4 N14' C75' 115(2) . . . . ? N15' P4 N14' C75' -133(2) . . . . ? N14 P4 N14' C75' -85(4) . . . . ? N15 P4 N14' C75' -122(2) . . . . ? O8 P4 N14' C76' -120.6(15) . . . . ? N16 P4 N14' C76' 5(2) . . . . ? N16' P4 N14' C76' -7.6(17) . . . . ? N15' P4 N14' C76' 105.0(18) . . . . ? N14 P4 N14' C76' 153(4) . . . . ? N15 P4 N14' C76' 116.1(18) . . . . ? O8 P4 N15 C78 64(3) . . . . ? N14' P4 N15 C78 -173(3) . . . . ? N16 P4 N15 C78 -50(3) . . . . ? N16' P4 N15 C78 -63(3) . . . . ? N15' P4 N15 C78 -99(9) . . . . ? N14 P4 N15 C78 176(3) . . . . ? O8 P4 N15 C77 -83(3) . . . . ? N14' P4 N15 C77 41(3) . . . . ? N16 P4 N15 C77 163(2) . . . . ? N16' P4 N15 C77 150(2) . . . . ? N15' P4 N15 C77 114(11) . . . . ? N14 P4 N15 C77 30(3) . . . . ? O8 P4 N15' C77' -38(3) . . . . ? N14' P4 N15' C77' 91(2) . . . . ? N16 P4 N15' C77' -151(2) . . . . ? N16' P4 N15' C77' -166(2) . . . . ? N14 P4 N15' C77' 77(2) . . . . ? N15 P4 N15' C77' -20(8) . . . . ? O8 P4 N15' C78' 82(2) . . . . ? N14' P4 N15' C78' -149(2) . . . . ? N16 P4 N15' C78' -31(2) . . . . ? N16' P4 N15' C78' -46(3) . . . . ? N14 P4 N15' C78' -163(2) . . . . ? N15 P4 N15' C78' 100(10) . . . . ? O8 P4 N16 C79 39(2) . . . . ? N14' P4 N16 C79 -88(2) . . . . ? N16' P4 N16 C79 -55(3) . . . . ? N15' P4 N16 C79 162(2) . . . . ? N14 P4 N16 C79 -101(2) . . . . ? N15 P4 N16 C79 154(2) . . . . ? O8 P4 N16 C80 -162.2(19) . . . . ? N14' P4 N16 C80 71(2) . . . . ? N16' P4 N16 C80 104(3) . . . . ? N15' P4 N16 C80 -39(2) . . . . ? N14 P4 N16 C80 58(2) . . . . ? N15 P4 N16 C80 -47(2) . . . . ? O8 P4 N16' C80' -179(2) . . . . ? N14' P4 N16' C80' 67(2) . . . . ? N16 P4 N16' C80' -84(3) . . . . ? N15' P4 N16' C80' -44(2) . . . . ? N14 P4 N16' C80' 60(2) . . . . ? N15 P4 N16' C80' -51(3) . . . . ? O8 P4 N16' C79' -32(2) . . . . ? N14' P4 N16' C79' -147(2) . . . . ? N16 P4 N16' C79' 62(3) . . . . ? N15' P4 N16' C79' 102(2) . . . . ? N14 P4 N16' C79' -153(2) . . . . ? N15 P4 N16' C79' 95(2) . . . . ? Sm1 O1 C1 C6 -40.0(13) . . . . ? Sm1 O1 C1 C2 139.9(8) . . . . ? O1 C1 C2 C3 179.5(9) . . . . ? C6 C1 C2 C3 -0.6(14) . . . . ? O1 C1 C2 C19 0.1(14) . . . . ? C6 C1 C2 C19 180.0(8) . . . . ? C1 C2 C3 C4 0.2(17) . . . . ? C19 C2 C3 C4 179.6(11) . . . . ? C2 C3 C4 C5 1.3(18) . . . . ? C2 C3 C4 C23 -174.6(11) . . . . ? C3 C4 C5 C6 -2.4(17) . . . . ? C23 C4 C5 C6 173.4(11) . . . . ? C4 C5 C6 C1 2.1(16) . . . . ? C4 C5 C6 C13 -173.6(10) . . . . ? O1 C1 C6 C5 179.4(8) . . . . ? C2 C1 C6 C5 -0.5(14) . . . . ? O1 C1 C6 C13 -5.0(13) . . . . ? C2 C1 C6 C13 175.1(8) . . . . ? Sm2 O2 C7 C12 -30.2(14) . . . . ? Sm2 O2 C7 C8 150.6(8) . . . . ? O2 C7 C8 C9 -177.8(9) . . . . ? C12 C7 C8 C9 2.9(13) . . . . ? O2 C7 C8 C24 4.0(14) . . . . ? C12 C7 C8 C24 -175.3(9) . . . . ? C7 C8 C9 C10 -0.6(15) . . . . ? C24 C8 C9 C10 177.5(10) . . . . ? C8 C9 C10 C11 -2.4(16) . . . . ? C8 C9 C10 C28 179.2(10) . . . . ? C9 C10 C11 C12 3.1(15) . . . . ? C28 C10 C11 C12 -178.4(9) . . . . ? C10 C11 C12 C7 -0.9(14) . . . . ? C10 C11 C12 C18 180.0(9) . . . . ? O2 C7 C12 C11 178.5(8) . . . . ? C8 C7 C12 C11 -2.2(13) . . . . ? O2 C7 C12 C18 -2.3(12) . . . . ? C8 C7 C12 C18 177.0(8) . . . . ? C16 N1 C13 C6 174.8(8) . . . . ? C14 N1 C13 C6 58.7(10) . . . . ? Sm1 N1 C13 C6 -75.4(8) . . . . ? C5 C6 C13 N1 -110.3(10) . . . . ? C1 C6 C13 N1 73.9(11) . . . . ? C16 N1 C14 C15 59.2(9) . . . . ? C13 N1 C14 C15 177.4(7) . . . . ? Sm1 N1 C14 C15 -61.8(9) . . . . ? C17 N2 C15 C14 57.0(9) . . . . ? C18 N2 C15 C14 173.8(7) . . . . ? N1 C14 C15 N2 -60.4(10) . . . . ? C13 N1 C16 C17 -179.4(7) . . . . ? C14 N1 C16 C17 -60.3(9) . . . . ? Sm1 N1 C16 C17 73.3(7) . . . . ? C15 N2 C17 C16 -57.2(9) . . . . ? C18 N2 C17 C16 -173.9(7) . . . . ? N1 C16 C17 N2 62.3(10) . . . . ? C17 N2 C18 C12 177.2(8) . . . . ? C15 N2 C18 C12 61.3(9) . . . . ? C11 C12 C18 N2 -102.6(10) . . . . ? C7 C12 C18 N2 78.2(10) . . . . ? C3 C2 C19 C21 -120.3(11) . . . . ? C1 C2 C19 C21 59.1(12) . . . . ? C3 C2 C19 C22 119.5(11) . . . . ? C1 C2 C19 C22 -61.1(12) . . . . ? C3 C2 C19 C20 -0.4(14) . . . . ? C1 C2 C19 C20 179.0(9) . . . . ? C9 C8 C24 C25 -1.4(15) . . . . ? C7 C8 C24 C25 176.6(10) . . . . ? C9 C8 C24 C26 117.1(11) . . . . ? C7 C8 C24 C26 -64.8(13) . . . . ? C9 C8 C24 C27 -122.4(11) . . . . ? C7 C8 C24 C27 55.6(12) . . . . ? Sm1 O3 C29 C34 -53.1(13) . . . . ? Sm1 O3 C29 C30 128.9(9) . . . . ? O3 C29 C30 C31 -178.4(10) . . . . ? C34 C29 C30 C31 3.6(15) . . . . ? O3 C29 C30 C47 2.4(15) . . . . ? C34 C29 C30 C47 -175.6(9) . . . . ? C29 C30 C31 C32 -0.3(19) . . . . ? C47 C30 C31 C32 178.9(12) . . . . ? C30 C31 C32 C33 -3(2) . . . . ? C30 C31 C32 C51 -177.1(14) . . . . ? C31 C32 C33 C34 3.6(18) . . . . ? C51 C32 C33 C34 177.5(13) . . . . ? O3 C29 C34 C33 178.7(9) . . . . ? C30 C29 C34 C33 -3.2(15) . . . . ? O3 C29 C34 C41 -10.6(14) . . . . ? C30 C29 C34 C41 167.5(9) . . . . ? C32 C33 C34 C29 -0.4(17) . . . . ? C32 C33 C34 C41 -171.8(10) . . . . ? Sm2 O4 C35 C36 -23.7(15) 2_756 . . . ? Sm2 O4 C35 C40 160.6(7) 2_756 . . . ? O4 C35 C36 C37 -179.5(8) . . . . ? C40 C35 C36 C37 -3.5(13) . . . . ? O4 C35 C36 C46 -4.8(13) . . . . ? C40 C35 C36 C46 171.2(8) . . . . ? C35 C36 C37 C38 1.2(14) . . . . ? C46 C36 C37 C38 -173.5(8) . . . . ? C36 C37 C38 C39 -0.3(14) . . . . ? C36 C37 C38 C56 -179.7(9) . . . . ? C37 C38 C39 C40 1.9(15) . . . . ? C56 C38 C39 C40 -178.7(9) . . . . ? C38 C39 C40 C35 -4.3(15) . . . . ? C38 C39 C40 C52 174.6(10) . . . . ? O4 C35 C40 C39 -179.3(8) . . . . ? C36 C35 C40 C39 4.8(13) . . . . ? O4 C35 C40 C52 1.8(14) . . . . ? C36 C35 C40 C52 -174.1(8) . . . . ? C42 N3 C41 C34 59.4(10) . . . . ? C44 N3 C41 C34 174.7(8) . . . . ? C29 C34 C41 N3 70.7(12) . . . . ? C33 C34 C41 N3 -118.2(10) . . . . ? C44 N3 C42 C43 59.0(9) . . . . ? C41 N3 C42 C43 174.2(7) . . . . ? C45 N4 C43 C42 57.7(9) . . . . ? C46 N4 C43 C42 173.7(7) . . . . ? N3 C42 C43 N4 -60.7(10) . . . . ? C42 N3 C44 C45 -60.2(9) . . . . ? C41 N3 C44 C45 -177.9(7) . . . . ? C43 N4 C45 C44 -59.0(9) . . . . ? C46 N4 C45 C44 -174.8(7) . . . . ? N3 C44 C45 N4 62.3(9) . . . . ? C43 N4 C46 C36 63.4(10) . . . . ? C45 N4 C46 C36 178.6(8) . . . . ? C37 C36 C46 N4 -108.1(10) . . . . ? C35 C36 C46 N4 77.0(11) . . . . ? C31 C30 C47 C50 115.1(12) . . . . ? C29 C30 C47 C50 -65.7(13) . . . . ? C31 C30 C47 C48 -4.3(16) . . . . ? C29 C30 C47 C48 174.8(11) . . . . ? C31 C30 C47 C49 -123.5(11) . . . . ? C29 C30 C47 C49 55.6(13) . . . . ? C39 C40 C52 C54 -116.6(11) . . . . ? C35 C40 C52 C54 62.3(12) . . . . ? C39 C40 C52 C55 122.9(11) . . . . ? C35 C40 C52 C55 -58.2(12) . . . . ? C39 C40 C52 C53 3.0(14) . . . . ? C35 C40 C52 C53 -178.2(9) . . . . ? C84 O9 C81 C82 2(5) . . . . ? C84' O9' C81' C82' -20(5) . . . . ? O9 C81 C82 C83 -37(8) . . . . ? O9' C81' C82' C83' 54(5) . . . . ? C81 C82 C83 C84 46(8) . . . . ? C81' C82' C83' C84' -55(5) . . . . ? C81 O9 C84 C83 23(7) . . . . ? C82 C83 C84 O9 -30(6) . . . . ? C81' O9' C84' C83' -14(7) . . . . ? C82' C83' C84' O9' 39(5) . . . . ? C88 O10 C85 C86 -21(10) . . . . ? C88' O10' C85' C86' 25(10) . . . . ? O10 C85 C86 C87 41(8) . . . . ? O10' C85' C86' C87' -46(8) . . . . ? C85 C86 C87 C88 -47(7) . . . . ? C85' C86' C87' C88' 58(7) . . . . ? C85 O10 C88 C87 -10(9) . . . . ? C86 C87 C88 O10 37(8) . . . . ? C85' O10' C88' C87' 9(9) . . . . ? C86' C87' C88' O10' -42(7) . . . . ? C92 O11 C89 C90 -6(8) . . . . ? C92' O11' C89' C90' 12(7) . . . . ? O11 C89 C90 C91 -6(7) . . . . ? O11' C89' C90' C91' -49(5) . . . . ? C89 C90 C91 C92 17(8) . . . . ? C89' C90' C91' C92' 76(4) . . . . ? C89 O11 C92 C91 14(7) . . . . ? C90 C91 C92 O11 -20(7) . . . . ? C89' O11' C92' C91' 31(6) . . . . ? C90' C91' C92' O11' -63(5) . . . . ? C96 O12 C93 C94 -10(12) . . . . ? C96' O12' C93' C94' -25(9) . . . . ? O12 C93 C94 C95 -6(11) . . . . ? O12' C93' C94' C95' 56(9) . . . . ? C93 C94 C95 C96 21(11) . . . . ? C93' C94' C95' C96' -55(7) . . . . ? C93 O12 C96 C95 20(10) . . . . ? C94 C95 C96 O12 -28(12) . . . . ? C93' O12' C96' C95' -13(11) . . . . ? C94' C95' C96' O12' 44(10) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.980 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.104 #===END #============================================================================== data_3 #(Complex 3) _database_code_depnum_ccdc_archive 'CCDC 807556' #TrackingRef '- revised.CIF' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H108 N8 O4 Sm2, C4 H8 O' _chemical_formula_sum 'C74 H116 N8 O5 Sm2' _chemical_formula_weight 1498.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.0159(7) _cell_length_b 19.9480(10) _cell_length_c 28.2760(16) _cell_angle_alpha 90.00 _cell_angle_beta 102.694(2) _cell_angle_gamma 90.00 _cell_volume 7712.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 34038 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 1.558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.626 _exptl_absorpt_correction_T_max 0.851 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39337 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 14277 _reflns_number_gt 11773 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+7.4333P] 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 14277 _refine_ls_number_parameters 783 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1332 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.36113(2) 0.196864(15) 0.609899(10) 0.03423(10) Uani 1 1 d . . . Sm2 Sm 0.69315(2) -0.047507(15) 0.705975(11) 0.03769(10) Uani 1 1 d . . . O1 O 0.2119(3) 0.1557(2) 0.59623(13) 0.0407(10) Uani 1 1 d . . . O2 O 0.3781(3) 0.2681(2) 0.66953(14) 0.0451(10) Uani 1 1 d . . . O3 O 0.6674(3) -0.0471(2) 0.77932(16) 0.0538(12) Uani 1 1 d . . . O4 O 0.6450(3) -0.1450(2) 0.67099(15) 0.0449(10) Uani 1 1 d . . . O5 O 0.028(2) 0.6387(18) 0.5246(10) 0.245(6) Uiso 0.50 1 d PD A 1 O5' O 0.122(3) 0.7424(13) 0.5322(11) 0.245(6) Uiso 0.50 1 d PD B 2 N1 N 0.2850(3) 0.2160(2) 0.52252(16) 0.0370(11) Uani 1 1 d . . . N2 N 0.3580(3) 0.3145(2) 0.57033(16) 0.0382(11) Uani 1 1 d . . . N3 N 0.8586(4) -0.0361(2) 0.76439(19) 0.0466(13) Uani 1 1 d . . . N4 N 0.8447(3) -0.1020(2) 0.68901(17) 0.0405(12) Uani 1 1 d . . . N5 N 0.4397(3) 0.0918(2) 0.62963(18) 0.0393(12) Uani 1 1 d . . . N6 N 0.5351(3) 0.1683(2) 0.60433(17) 0.0370(11) Uani 1 1 d . . . N7 N 0.6602(4) 0.0732(2) 0.69583(17) 0.0391(11) Uani 1 1 d . . . N8 N 0.6429(3) 0.0127(2) 0.62711(16) 0.0393(11) Uani 1 1 d . . . C1 C 0.1378(4) 0.1338(3) 0.5608(2) 0.0391(14) Uani 1 1 d . . . C2 C 0.0439(4) 0.1194(3) 0.5690(2) 0.0431(15) Uani 1 1 d . . . C3 C -0.0270(5) 0.0963(3) 0.5299(2) 0.0513(17) Uani 1 1 d . . . H3 H -0.0888 0.0851 0.5353 0.062 Uiso 1 1 calc R . . C4 C -0.0116(5) 0.0890(4) 0.4835(3) 0.0565(18) Uani 1 1 d . . . C5 C 0.0789(5) 0.1066(3) 0.4758(2) 0.0526(17) Uani 1 1 d . . . H5 H 0.0907 0.1034 0.4444 0.063 Uiso 1 1 calc R . . C6 C 0.1529(4) 0.1289(3) 0.5135(2) 0.0420(14) Uani 1 1 d . . . C7 C 0.3554(4) 0.3312(3) 0.6795(2) 0.0407(14) Uani 1 1 d . . . C8 C 0.3250(4) 0.3458(3) 0.7233(2) 0.0469(16) Uani 1 1 d . . . C9 C 0.3048(5) 0.4129(4) 0.7309(2) 0.0534(18) Uani 1 1 d . . . H9 H 0.2849 0.4239 0.7596 0.064 Uiso 1 1 calc R . . C10 C 0.3120(5) 0.4642(4) 0.6990(3) 0.0554(18) Uani 1 1 d . . . C11 C 0.3400(5) 0.4475(3) 0.6569(3) 0.0496(16) Uani 1 1 d . . . H11 H 0.3438 0.4815 0.6343 0.059 Uiso 1 1 calc R . . C12 C 0.3627(4) 0.3822(3) 0.6465(2) 0.0424(14) Uani 1 1 d . . . C13 C 0.2480(5) 0.1497(3) 0.5021(2) 0.0462(15) Uani 1 1 d . . . H13A H 0.2973 0.1155 0.5146 0.055 Uiso 1 1 calc R . . H13B H 0.2400 0.1511 0.4668 0.055 Uiso 1 1 calc R . . C14 C 0.2118(4) 0.2693(3) 0.5165(2) 0.0419(14) Uani 1 1 d . . . H14A H 0.1500 0.2519 0.5222 0.050 Uiso 1 1 calc R . . H14B H 0.2000 0.2872 0.4834 0.050 Uiso 1 1 calc R . . C15 C 0.2519(4) 0.3252(3) 0.5537(2) 0.0457(15) Uani 1 1 d . . . H15A H 0.2391 0.3694 0.5385 0.055 Uiso 1 1 calc R . . H15B H 0.2199 0.3230 0.5812 0.055 Uiso 1 1 calc R . . C16 C 0.3690(4) 0.2394(3) 0.5030(2) 0.0419(14) Uani 1 1 d . . . H16A H 0.3497 0.2446 0.4678 0.050 Uiso 1 1 calc R . . H16B H 0.4228 0.2071 0.5106 0.050 Uiso 1 1 calc R . . C17 C 0.4010(5) 0.3076(3) 0.5274(2) 0.0447(15) Uani 1 1 d . . . H17A H 0.4725 0.3097 0.5372 0.054 Uiso 1 1 calc R . . H17B H 0.3785 0.3442 0.5046 0.054 Uiso 1 1 calc R . . C18 C 0.4050(5) 0.3697(3) 0.6024(2) 0.0427(14) Uani 1 1 d . . . H18A H 0.3994 0.4111 0.5833 0.051 Uiso 1 1 calc R . . H18B H 0.4748 0.3595 0.6133 0.051 Uiso 1 1 calc R . . C19 C 0.0202(5) 0.1317(3) 0.6183(3) 0.0517(17) Uani 1 1 d . . . C20 C -0.0870(5) 0.1142(4) 0.6189(3) 0.071(2) Uani 1 1 d . . . H20A H -0.1306 0.1413 0.5949 0.107 Uiso 1 1 calc R . . H20B H -0.0989 0.1233 0.6508 0.107 Uiso 1 1 calc R . . H20C H -0.0987 0.0671 0.6112 0.107 Uiso 1 1 calc R . . C21 C 0.0333(6) 0.2064(4) 0.6308(3) 0.067(2) Uani 1 1 d . . . H21A H 0.1001 0.2196 0.6313 0.101 Uiso 1 1 calc R . . H21B H 0.0192 0.2143 0.6624 0.101 Uiso 1 1 calc R . . H21C H -0.0112 0.2325 0.6066 0.101 Uiso 1 1 calc R . . C22 C 0.0860(5) 0.0895(4) 0.6580(3) 0.066(2) Uani 1 1 d . . . H22A H 0.0722 0.0423 0.6517 0.100 Uiso 1 1 calc R . . H22B H 0.0733 0.1013 0.6894 0.100 Uiso 1 1 calc R . . H22C H 0.1541 0.0984 0.6581 0.100 Uiso 1 1 calc R . . C23 C -0.0933(6) 0.0638(4) 0.4434(3) 0.076(2) Uani 1 1 d . . . H23A H -0.1180 0.0218 0.4531 0.115 Uiso 1 1 calc R . . H23B H -0.0688 0.0570 0.4142 0.115 Uiso 1 1 calc R . . H23C H -0.1457 0.0966 0.4370 0.115 Uiso 1 1 calc R . . C24 C 0.3106(5) 0.2911(4) 0.7594(2) 0.0552(18) Uani 1 1 d . . . C25 C 0.2758(7) 0.3198(5) 0.8026(3) 0.081(3) Uani 1 1 d . . . H25A H 0.3226 0.3527 0.8189 0.122 Uiso 1 1 calc R . . H25B H 0.2701 0.2839 0.8250 0.122 Uiso 1 1 calc R . . H25C H 0.2126 0.3410 0.7915 0.122 Uiso 1 1 calc R . . C26 C 0.4050(5) 0.2509(4) 0.7781(3) 0.070(2) Uani 1 1 d . . . H26A H 0.4321 0.2368 0.7510 0.104 Uiso 1 1 calc R . . H26B H 0.3904 0.2117 0.7956 0.104 Uiso 1 1 calc R . . H26C H 0.4522 0.2788 0.7997 0.104 Uiso 1 1 calc R . . C27 C 0.2314(5) 0.2419(4) 0.7341(3) 0.066(2) Uani 1 1 d . . . H27A H 0.1716 0.2663 0.7209 0.098 Uiso 1 1 calc R . . H27B H 0.2193 0.2090 0.7573 0.098 Uiso 1 1 calc R . . H27C H 0.2534 0.2193 0.7080 0.098 Uiso 1 1 calc R . . C28 C 0.2882(6) 0.5367(4) 0.7096(3) 0.077(2) Uani 1 1 d . . . H28A H 0.3379 0.5662 0.7020 0.116 Uiso 1 1 calc R . . H28B H 0.2868 0.5412 0.7436 0.116 Uiso 1 1 calc R . . H28C H 0.2249 0.5488 0.6898 0.116 Uiso 1 1 calc R . . C29 C 0.7074(8) -0.0486(4) 0.8267(3) 0.0816(12) Uani 1 1 d . . . C30 C 0.6558(8) -0.0703(4) 0.8614(3) 0.0816(12) Uani 1 1 d . . . C31 C 0.7077(8) -0.0739(4) 0.9104(3) 0.0816(12) Uani 1 1 d . . . H31 H 0.6750 -0.0896 0.9339 0.098 Uiso 1 1 calc R . . C32 C 0.8041(8) -0.0553(4) 0.9248(3) 0.0816(12) Uani 1 1 d . . . C33 C 0.8520(8) -0.0313(4) 0.8918(3) 0.0816(12) Uani 1 1 d . . . H33 H 0.9173 -0.0172 0.9019 0.098 Uiso 1 1 calc R . . C34 C 0.8052(8) -0.0273(4) 0.8426(3) 0.0816(12) Uani 1 1 d . . . C35 C 0.6746(4) -0.2003(3) 0.6516(2) 0.0415(14) Uani 1 1 d . . . C36 C 0.6164(5) -0.2594(3) 0.6429(2) 0.0449(15) Uani 1 1 d . . . C37 C 0.6562(5) -0.3158(3) 0.6251(2) 0.0483(16) Uani 1 1 d . . . H37 H 0.6179 -0.3549 0.6196 0.058 Uiso 1 1 calc R . . C38 C 0.7485(5) -0.3177(3) 0.6150(2) 0.0507(17) Uani 1 1 d . . . C39 C 0.8026(5) -0.2587(3) 0.6224(2) 0.0458(15) Uani 1 1 d . . . H39 H 0.8654 -0.2579 0.6157 0.055 Uiso 1 1 calc R . . C40 C 0.7667(4) -0.2014(3) 0.6394(2) 0.0398(14) Uani 1 1 d . . . C41 C 0.8600(5) 0.0038(4) 0.8084(3) 0.068(2) Uani 1 1 d . . . H41A H 0.8319 0.0480 0.7988 0.082 Uiso 1 1 calc R . . H41B H 0.9281 0.0104 0.8255 0.082 Uiso 1 1 calc R . . C42 C 0.8948(6) -0.1045(3) 0.7766(2) 0.060(2) Uani 1 1 d . . . H42A H 0.8584 -0.1253 0.7986 0.071 Uiso 1 1 calc R . . H42B H 0.9642 -0.1031 0.7928 0.071 Uiso 1 1 calc R . . C43 C 0.8815(5) -0.1448(3) 0.7304(2) 0.0558(18) Uani 1 1 d . . . H43A H 0.9442 -0.1644 0.7277 0.067 Uiso 1 1 calc R . . H43B H 0.8353 -0.1814 0.7312 0.067 Uiso 1 1 calc R . . C44 C 0.9201(5) -0.0047(4) 0.7344(3) 0.064(2) Uani 1 1 d . . . H44A H 0.9882 -0.0027 0.7526 0.077 Uiso 1 1 calc R . . H44B H 0.8977 0.0411 0.7259 0.077 Uiso 1 1 calc R . . C45 C 0.9132(6) -0.0464(4) 0.6886(3) 0.068(2) Uani 1 1 d . . . H45A H 0.8901 -0.0183 0.6599 0.082 Uiso 1 1 calc R . . H45B H 0.9778 -0.0640 0.6873 0.082 Uiso 1 1 calc R . . C46 C 0.8284(4) -0.1380(3) 0.6423(2) 0.0434(15) Uani 1 1 d . . . H46A H 0.8922 -0.1501 0.6359 0.052 Uiso 1 1 calc R . . H46B H 0.7966 -0.1074 0.6165 0.052 Uiso 1 1 calc R . . C47 C 0.5502(10) -0.0899(6) 0.8463(4) 0.106(4) Uani 1 1 d . . . C48 C 0.5042(11) -0.1107(5) 0.8898(4) 0.150(6) Uani 1 1 d . . . H48A H 0.5395 -0.1488 0.9064 0.225 Uiso 1 1 calc R . . H48B H 0.4362 -0.1227 0.8777 0.225 Uiso 1 1 calc R . . H48C H 0.5085 -0.0734 0.9122 0.225 Uiso 1 1 calc R . . C49 C 0.4906(8) -0.0296(7) 0.8238(4) 0.126(4) Uani 1 1 d . . . H49A H 0.4942 0.0053 0.8480 0.189 Uiso 1 1 calc R . . H49B H 0.4229 -0.0429 0.8120 0.189 Uiso 1 1 calc R . . H49C H 0.5166 -0.0128 0.7970 0.189 Uiso 1 1 calc R . . C50 C 0.5364(11) -0.1492(6) 0.8106(4) 0.156(6) Uani 1 1 d . . . H50A H 0.5597 -0.1367 0.7819 0.234 Uiso 1 1 calc R . . H50B H 0.4676 -0.1608 0.8014 0.234 Uiso 1 1 calc R . . H50C H 0.5733 -0.1875 0.8260 0.234 Uiso 1 1 calc R . . C51 C 0.8572(12) -0.0598(8) 0.9791(3) 0.193(8) Uani 1 1 d . . . H51A H 0.9269 -0.0649 0.9816 0.290 Uiso 1 1 calc R . . H51B H 0.8326 -0.0981 0.9939 0.290 Uiso 1 1 calc R . . H51C H 0.8451 -0.0191 0.9957 0.290 Uiso 1 1 calc R . . C52 C 0.5121(5) -0.2616(4) 0.6528(3) 0.0598(19) Uani 1 1 d . . . C53 C 0.4607(6) -0.3281(4) 0.6382(4) 0.093(3) Uani 1 1 d . . . H53A H 0.4948 -0.3636 0.6586 0.140 Uiso 1 1 calc R . . H53B H 0.4609 -0.3375 0.6046 0.140 Uiso 1 1 calc R . . H53C H 0.3938 -0.3254 0.6421 0.140 Uiso 1 1 calc R . . C54 C 0.5158(6) -0.2520(4) 0.7060(3) 0.074(2) Uani 1 1 d . . . H54A H 0.4498 -0.2510 0.7114 0.110 Uiso 1 1 calc R . . H54B H 0.5485 -0.2101 0.7168 0.110 Uiso 1 1 calc R . . H54C H 0.5515 -0.2889 0.7242 0.110 Uiso 1 1 calc R . . C55 C 0.4499(5) -0.2058(4) 0.6227(3) 0.078(3) Uani 1 1 d . . . H55A H 0.3830 -0.2088 0.6266 0.117 Uiso 1 1 calc R . . H55B H 0.4511 -0.2113 0.5887 0.117 Uiso 1 1 calc R . . H55C H 0.4767 -0.1623 0.6338 0.117 Uiso 1 1 calc R . . C56 C 0.7894(6) -0.3810(3) 0.5972(3) 0.063(2) Uani 1 1 d . . . H56A H 0.7910 -0.4166 0.6208 0.095 Uiso 1 1 calc R . . H56B H 0.8551 -0.3725 0.5929 0.095 Uiso 1 1 calc R . . H56C H 0.7480 -0.3945 0.5665 0.095 Uiso 1 1 calc R . . C57 C 0.5294(4) 0.1103(3) 0.62604(19) 0.0331(12) Uani 1 1 d . . . C58 C 0.4161(5) 0.0278(3) 0.6492(3) 0.0532(18) Uani 1 1 d . . . H58 H 0.4766 0.0008 0.6588 0.064 Uiso 1 1 calc R . . C59 C 0.3421(6) -0.0107(4) 0.6116(3) 0.078(3) Uani 1 1 d . . . H59A H 0.2814 0.0144 0.6035 0.118 Uiso 1 1 calc R . . H59B H 0.3301 -0.0541 0.6246 0.118 Uiso 1 1 calc R . . H59C H 0.3676 -0.0168 0.5826 0.118 Uiso 1 1 calc R . . C60 C 0.3717(7) 0.0383(5) 0.6932(3) 0.093(3) Uani 1 1 d . . . H60A H 0.4186 0.0610 0.7185 0.140 Uiso 1 1 calc R . . H60B H 0.3551 -0.0048 0.7051 0.140 Uiso 1 1 calc R . . H60C H 0.3131 0.0654 0.6841 0.140 Uiso 1 1 calc R . . C61 C 0.6320(4) 0.1932(3) 0.6004(2) 0.0476(16) Uani 1 1 d . . . H61 H 0.6821 0.1610 0.6170 0.057 Uiso 1 1 calc R . . C62 C 0.6388(5) 0.1979(4) 0.5471(3) 0.064(2) Uani 1 1 d . . . H62A H 0.6203 0.1552 0.5312 0.096 Uiso 1 1 calc R . . H62B H 0.7054 0.2087 0.5453 0.096 Uiso 1 1 calc R . . H62C H 0.5950 0.2327 0.5311 0.096 Uiso 1 1 calc R . . C63 C 0.6527(5) 0.2612(3) 0.6252(3) 0.0606(19) Uani 1 1 d . . . H63A H 0.6116 0.2950 0.6061 0.091 Uiso 1 1 calc R . . H63B H 0.7209 0.2728 0.6279 0.091 Uiso 1 1 calc R . . H63C H 0.6388 0.2590 0.6573 0.091 Uiso 1 1 calc R . . C64 C 0.6160(4) 0.0659(3) 0.6494(2) 0.0344(13) Uani 1 1 d . . . C65 C 0.6451(5) 0.1343(3) 0.7227(2) 0.0472(16) Uani 1 1 d . . . H65 H 0.5942 0.1623 0.7020 0.057 Uiso 1 1 calc R . . C66 C 0.6134(6) 0.1173(4) 0.7695(2) 0.066(2) Uani 1 1 d . . . H66A H 0.5468 0.1006 0.7618 0.098 Uiso 1 1 calc R . . H66B H 0.6168 0.1573 0.7893 0.098 Uiso 1 1 calc R . . H66C H 0.6565 0.0832 0.7870 0.098 Uiso 1 1 calc R . . C67 C 0.7416(5) 0.1730(3) 0.7342(3) 0.065(2) Uani 1 1 d . . . H67A H 0.7864 0.1515 0.7609 0.098 Uiso 1 1 calc R . . H67B H 0.7295 0.2187 0.7431 0.098 Uiso 1 1 calc R . . H67C H 0.7701 0.1734 0.7059 0.098 Uiso 1 1 calc R . . C68 C 0.6045(5) 0.0032(3) 0.5746(2) 0.0430(15) Uani 1 1 d . . . H68 H 0.5515 0.0361 0.5633 0.052 Uiso 1 1 calc R . . C69 C 0.5641(5) -0.0665(3) 0.5634(2) 0.0482(16) Uani 1 1 d . . . H69A H 0.6145 -0.0992 0.5760 0.072 Uiso 1 1 calc R . . H69B H 0.5429 -0.0720 0.5286 0.072 Uiso 1 1 calc R . . H69C H 0.5089 -0.0732 0.5784 0.072 Uiso 1 1 calc R . . C70 C 0.6866(5) 0.0161(4) 0.5478(2) 0.0539(17) Uani 1 1 d . . . H70A H 0.7142 0.0602 0.5563 0.081 Uiso 1 1 calc R . . H70B H 0.6604 0.0138 0.5132 0.081 Uiso 1 1 calc R . . H70C H 0.7372 -0.0176 0.5572 0.081 Uiso 1 1 calc R . . C71 C 0.085(3) 0.6827(15) 0.5637(15) 0.245(6) Uiso 0.50 1 d PD A 1 C71' C 0.214(2) 0.716(2) 0.5471(17) 0.245(6) Uiso 0.50 1 d PD B 2 C72 C 0.173(3) 0.638(2) 0.5828(15) 0.245(6) Uiso 0.50 1 d PD A 1 C72' C 0.209(3) 0.640(2) 0.5517(17) 0.245(6) Uiso 0.50 1 d PD B 2 C73 C 0.136(3) 0.5654(18) 0.5774(16) 0.245(6) Uiso 0.50 1 d PD A 1 C73' C 0.104(3) 0.6233(18) 0.5526(17) 0.245(6) Uiso 0.50 1 d PD B 2 C74 C 0.033(3) 0.5697(17) 0.5417(15) 0.245(6) Uiso 0.50 1 d PD A 1 C74' C 0.059(2) 0.686(2) 0.5226(17) 0.245(6) Uiso 0.50 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02886(17) 0.03482(18) 0.03755(18) 0.00150(13) 0.00411(12) 0.00203(12) Sm2 0.03375(18) 0.03486(18) 0.04162(19) 0.00385(13) 0.00215(13) 0.00386(13) O1 0.033(2) 0.050(2) 0.037(2) -0.0039(19) 0.0028(17) -0.0056(18) O2 0.044(3) 0.047(3) 0.044(2) 0.002(2) 0.0090(19) 0.004(2) O3 0.061(3) 0.056(3) 0.046(3) 0.004(2) 0.015(2) -0.007(2) O4 0.036(2) 0.039(2) 0.058(3) -0.002(2) 0.0055(19) -0.0022(19) N1 0.037(3) 0.040(3) 0.034(3) -0.004(2) 0.007(2) 0.005(2) N2 0.034(3) 0.044(3) 0.036(3) 0.001(2) 0.007(2) 0.003(2) N3 0.046(3) 0.038(3) 0.050(3) -0.005(2) -0.004(2) -0.002(2) N4 0.038(3) 0.037(3) 0.044(3) 0.006(2) 0.003(2) -0.002(2) N5 0.031(3) 0.029(3) 0.057(3) 0.011(2) 0.006(2) 0.003(2) N6 0.035(3) 0.032(3) 0.043(3) 0.006(2) 0.005(2) 0.000(2) N7 0.044(3) 0.032(3) 0.038(3) -0.001(2) 0.000(2) 0.006(2) N8 0.039(3) 0.040(3) 0.036(3) 0.000(2) 0.002(2) 0.006(2) C1 0.034(3) 0.035(3) 0.043(3) -0.001(3) -0.001(3) -0.002(3) C2 0.034(3) 0.038(3) 0.055(4) 0.000(3) 0.003(3) -0.004(3) C3 0.036(4) 0.046(4) 0.065(4) 0.003(3) -0.003(3) -0.011(3) C4 0.053(5) 0.054(4) 0.054(4) -0.007(3) -0.010(3) -0.001(3) C5 0.054(4) 0.053(4) 0.049(4) -0.014(3) 0.006(3) 0.006(3) C6 0.041(4) 0.042(3) 0.041(3) -0.005(3) 0.005(3) -0.005(3) C7 0.028(3) 0.044(4) 0.047(4) -0.007(3) 0.001(3) 0.002(3) C8 0.037(3) 0.060(4) 0.045(4) -0.016(3) 0.010(3) -0.010(3) C9 0.042(4) 0.066(5) 0.053(4) -0.019(4) 0.012(3) -0.006(3) C10 0.038(4) 0.058(4) 0.069(5) -0.023(4) 0.009(3) 0.001(3) C11 0.040(4) 0.043(4) 0.060(4) 0.000(3) -0.002(3) -0.001(3) C12 0.035(3) 0.047(4) 0.044(3) -0.004(3) 0.005(3) -0.004(3) C13 0.049(4) 0.050(4) 0.036(3) -0.008(3) 0.003(3) 0.004(3) C14 0.040(4) 0.043(4) 0.040(3) 0.003(3) 0.002(3) 0.003(3) C15 0.042(4) 0.045(4) 0.047(4) -0.002(3) 0.004(3) 0.007(3) C16 0.044(4) 0.046(4) 0.037(3) -0.004(3) 0.010(3) 0.004(3) C17 0.044(4) 0.048(4) 0.043(4) 0.007(3) 0.012(3) 0.000(3) C18 0.045(4) 0.035(3) 0.047(4) -0.004(3) 0.006(3) -0.004(3) C19 0.034(4) 0.052(4) 0.069(5) 0.001(3) 0.011(3) -0.006(3) C20 0.044(4) 0.092(6) 0.078(5) 0.006(5) 0.013(4) -0.006(4) C21 0.057(5) 0.072(5) 0.076(5) -0.021(4) 0.021(4) -0.001(4) C22 0.045(4) 0.094(6) 0.057(4) 0.014(4) 0.005(3) -0.006(4) C23 0.058(5) 0.074(5) 0.082(6) -0.013(5) -0.017(4) -0.014(4) C24 0.046(4) 0.071(5) 0.051(4) -0.010(4) 0.016(3) -0.011(4) C25 0.094(7) 0.096(6) 0.063(5) -0.029(5) 0.038(5) -0.028(5) C26 0.054(5) 0.091(6) 0.062(5) 0.016(4) 0.008(4) -0.013(4) C27 0.051(5) 0.075(5) 0.073(5) -0.007(4) 0.019(4) -0.016(4) C28 0.080(6) 0.060(5) 0.095(6) -0.027(5) 0.025(5) 0.006(4) C29 0.131(4) 0.059(2) 0.055(2) 0.0029(18) 0.020(2) 0.033(2) C30 0.131(4) 0.059(2) 0.055(2) 0.0029(18) 0.020(2) 0.033(2) C31 0.131(4) 0.059(2) 0.055(2) 0.0029(18) 0.020(2) 0.033(2) C32 0.131(4) 0.059(2) 0.055(2) 0.0029(18) 0.020(2) 0.033(2) C33 0.131(4) 0.059(2) 0.055(2) 0.0029(18) 0.020(2) 0.033(2) C34 0.131(4) 0.059(2) 0.055(2) 0.0029(18) 0.020(2) 0.033(2) C35 0.039(4) 0.033(3) 0.048(4) 0.005(3) 0.000(3) 0.004(3) C36 0.047(4) 0.036(3) 0.048(4) -0.001(3) 0.001(3) -0.004(3) C37 0.062(5) 0.033(3) 0.046(4) 0.004(3) 0.003(3) -0.008(3) C38 0.070(5) 0.043(4) 0.038(3) 0.004(3) 0.009(3) 0.007(3) C39 0.048(4) 0.049(4) 0.040(3) 0.005(3) 0.009(3) 0.009(3) C40 0.040(3) 0.040(3) 0.037(3) 0.011(3) 0.002(3) 0.002(3) C41 0.051(4) 0.068(5) 0.072(5) -0.021(4) -0.015(4) 0.015(4) C42 0.070(5) 0.046(4) 0.053(4) -0.004(3) -0.010(3) 0.020(4) C43 0.067(5) 0.049(4) 0.047(4) 0.002(3) 0.002(3) 0.020(4) C44 0.043(4) 0.052(4) 0.094(6) -0.002(4) 0.005(4) -0.008(3) C45 0.065(5) 0.070(5) 0.070(5) -0.014(4) 0.013(4) -0.033(4) C46 0.037(3) 0.045(4) 0.051(4) 0.002(3) 0.015(3) 0.005(3) C47 0.158(11) 0.092(7) 0.087(7) 0.010(6) 0.067(7) -0.023(7) C48 0.271(17) 0.098(8) 0.131(9) -0.019(7) 0.152(11) -0.053(10) C49 0.077(7) 0.192(14) 0.118(9) 0.027(9) 0.041(6) -0.021(8) C50 0.243(16) 0.138(10) 0.123(9) -0.057(8) 0.119(10) -0.123(11) C51 0.29(2) 0.223(16) 0.047(6) -0.002(8) -0.005(8) 0.125(15) C52 0.041(4) 0.051(4) 0.086(5) 0.003(4) 0.011(4) -0.001(3) C53 0.067(6) 0.061(5) 0.153(9) -0.003(6) 0.028(6) -0.024(4) C54 0.052(5) 0.081(6) 0.094(6) 0.014(5) 0.030(4) -0.002(4) C55 0.035(4) 0.073(5) 0.119(7) 0.023(5) 0.003(4) -0.001(4) C56 0.096(6) 0.042(4) 0.055(4) 0.003(3) 0.021(4) 0.012(4) C57 0.032(3) 0.031(3) 0.035(3) -0.002(2) 0.002(2) 0.001(2) C58 0.034(4) 0.049(4) 0.073(5) 0.025(4) 0.004(3) 0.005(3) C59 0.062(5) 0.053(5) 0.116(7) -0.010(5) 0.010(5) -0.009(4) C60 0.087(7) 0.127(8) 0.068(5) 0.026(6) 0.022(5) -0.030(6) C61 0.033(3) 0.046(4) 0.063(4) 0.011(3) 0.007(3) 0.006(3) C62 0.048(4) 0.075(5) 0.074(5) 0.026(4) 0.025(4) 0.008(4) C63 0.045(4) 0.044(4) 0.088(5) 0.005(4) 0.004(4) -0.006(3) C64 0.028(3) 0.035(3) 0.039(3) 0.002(3) 0.004(2) -0.002(2) C65 0.047(4) 0.040(3) 0.045(4) -0.009(3) -0.011(3) 0.010(3) C66 0.072(5) 0.074(5) 0.049(4) -0.012(4) 0.009(4) 0.019(4) C67 0.071(5) 0.047(4) 0.068(5) -0.019(4) -0.006(4) -0.005(4) C68 0.046(4) 0.041(3) 0.038(3) 0.001(3) -0.002(3) 0.008(3) C69 0.047(4) 0.053(4) 0.042(3) -0.010(3) 0.004(3) -0.004(3) C70 0.061(5) 0.058(4) 0.045(4) 0.000(3) 0.016(3) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O2 2.178(4) . ? Sm1 O1 2.201(4) . ? Sm1 N5 2.376(4) . ? Sm1 N1 2.496(4) . ? Sm1 N6 2.542(5) . ? Sm1 N2 2.596(5) . ? Sm1 C57 2.878(5) . ? Sm2 O3 2.182(4) . ? Sm2 O4 2.218(4) . ? Sm2 N7 2.458(5) . ? Sm2 N8 2.494(5) . ? Sm2 N4 2.524(5) . ? Sm2 N3 2.544(5) . ? Sm2 C64 2.845(6) . ? O1 C1 1.348(6) . ? O2 C7 1.344(7) . ? O3 C29 1.334(9) . ? O4 C35 1.338(7) . ? O5 C74 1.456(18) . ? O5 C71 1.493(19) . ? O5' C71' 1.362(18) . ? O5' C74' 1.416(19) . ? N1 C14 1.461(7) . ? N1 C16 1.482(7) . ? N1 C13 1.490(7) . ? N2 C15 1.473(7) . ? N2 C17 1.476(7) . ? N2 C18 1.485(7) . ? N3 C42 1.470(8) . ? N3 C41 1.474(9) . ? N3 C44 1.474(9) . ? N4 C43 1.450(8) . ? N4 C45 1.469(8) . ? N4 C46 1.477(8) . ? N5 C57 1.336(7) . ? N5 C58 1.458(8) . ? N6 C57 1.321(7) . ? N6 C61 1.474(8) . ? N7 C64 1.332(7) . ? N7 C65 1.474(7) . ? N8 C64 1.330(7) . ? N8 C68 1.477(7) . ? C1 C6 1.401(8) . ? C1 C2 1.415(8) . ? C2 C3 1.392(8) . ? C2 C19 1.523(9) . ? C3 C4 1.382(9) . ? C3 H3 0.9400 . ? C4 C5 1.379(10) . ? C4 C23 1.510(9) . ? C5 C6 1.387(8) . ? C5 H5 0.9400 . ? C6 C13 1.497(9) . ? C7 C12 1.399(8) . ? C7 C8 1.425(8) . ? C8 C9 1.394(9) . ? C8 C24 1.537(10) . ? C9 C10 1.383(10) . ? C9 H9 0.9400 . ? C10 C11 1.375(9) . ? C10 C28 1.527(10) . ? C11 C12 1.389(9) . ? C11 H11 0.9400 . ? C12 C18 1.514(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.550(8) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.546(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C21 1.532(10) . ? C19 C22 1.538(9) . ? C19 C20 1.546(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.525(9) . ? C24 C27 1.536(9) . ? C24 C26 1.538(10) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 C30 1.410(13) . ? C29 C34 1.410(13) . ? C30 C31 1.418(11) . ? C30 C47 1.500(15) . ? C31 C32 1.374(13) . ? C31 H31 0.9400 . ? C32 C33 1.350(12) . ? C32 C51 1.556(12) . ? C33 C34 1.404(11) . ? C33 H33 0.9400 . ? C34 C41 1.494(12) . ? C35 C40 1.407(8) . ? C35 C36 1.425(8) . ? C36 C37 1.398(9) . ? C36 C52 1.549(9) . ? C37 C38 1.386(9) . ? C37 H37 0.9400 . ? C38 C39 1.392(9) . ? C38 C56 1.517(9) . ? C39 C40 1.377(8) . ? C39 H39 0.9400 . ? C40 C46 1.524(8) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 C43 1.509(9) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 C45 1.526(10) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C47 C49 1.521(15) . ? C47 C50 1.540(14) . ? C47 C48 1.564(11) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C49 H49C 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 H50C 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C52 C54 1.506(10) . ? C52 C53 1.522(10) . ? C52 C55 1.548(10) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C55 H55C 0.9700 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C56 H56C 0.9700 . ? C57 C64 1.529(7) . ? C58 C59 1.520(10) . ? C58 C60 1.524(11) . ? C58 H58 0.9900 . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C59 H59C 0.9700 . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C60 H60C 0.9700 . ? C61 C63 1.526(9) . ? C61 C62 1.533(9) . ? C61 H61 0.9900 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C62 H62C 0.9700 . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C63 H63C 0.9700 . ? C65 C66 1.523(9) . ? C65 C67 1.530(9) . ? C65 H65 0.9900 . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C66 H66C 0.9700 . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C67 H67C 0.9700 . ? C68 C69 1.510(8) . ? C68 C70 1.530(9) . ? C68 H68 0.9900 . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C69 H69C 0.9700 . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C70 H70C 0.9700 . ? C71 C72 1.522(19) . ? C71' C72' 1.533(19) . ? C72 C73 1.539(19) . ? C72' C73' 1.52(2) . ? C73 C74 1.569(19) . ? C73' C74' 1.563(19) . ? 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 O2 Sm1 O1 108.49(15) . . ? O2 Sm1 N5 115.32(16) . . ? O1 Sm1 N5 94.92(16) . . ? O2 Sm1 N1 128.09(15) . . ? O1 Sm1 N1 72.54(15) . . ? N5 Sm1 N1 116.26(16) . . ? O2 Sm1 N6 104.57(15) . . ? O1 Sm1 N6 142.45(15) . . ? N5 Sm1 N6 54.23(15) . . ? N1 Sm1 N6 100.39(15) . . ? O2 Sm1 N2 74.49(15) . . ? O1 Sm1 N2 109.65(15) . . ? N5 Sm1 N2 149.49(16) . . ? N1 Sm1 N2 58.14(15) . . ? N6 Sm1 N2 95.83(15) . . ? O2 Sm1 C57 108.83(15) . . ? O1 Sm1 C57 121.21(15) . . ? N5 Sm1 C57 27.37(15) . . ? N1 Sm1 C57 113.96(15) . . ? N6 Sm1 C57 27.31(15) . . ? N2 Sm1 C57 123.13(15) . . ? O3 Sm2 O4 109.22(16) . . ? O3 Sm2 N7 92.38(16) . . ? O4 Sm2 N7 140.90(15) . . ? O3 Sm2 N8 140.79(17) . . ? O4 Sm2 N8 91.43(15) . . ? N7 Sm2 N8 54.17(15) . . ? O3 Sm2 N4 120.27(16) . . ? O4 Sm2 N4 73.98(15) . . ? N7 Sm2 N4 122.98(16) . . ? N8 Sm2 N4 97.00(15) . . ? O3 Sm2 N3 72.56(18) . . ? O4 Sm2 N3 120.84(15) . . ? N7 Sm2 N3 96.25(16) . . ? N8 Sm2 N3 125.12(17) . . ? N4 Sm2 N3 58.47(16) . . ? O3 Sm2 C64 114.23(17) . . ? O4 Sm2 C64 113.93(15) . . ? N7 Sm2 C64 27.88(15) . . ? N8 Sm2 C64 27.87(15) . . ? N4 Sm2 C64 117.86(16) . . ? N3 Sm2 C64 118.25(16) . . ? C1 O1 Sm1 143.0(4) . . ? C7 O2 Sm1 141.6(4) . . ? C29 O3 Sm2 146.4(6) . . ? C35 O4 Sm2 144.5(4) . . ? C74 O5 C71 109(2) . . ? C71' O5' C74' 104.9(19) . . ? C14 N1 C16 108.7(5) . . ? C14 N1 C13 115.2(5) . . ? C16 N1 C13 111.9(4) . . ? C14 N1 Sm1 111.3(3) . . ? C16 N1 Sm1 102.4(3) . . ? C13 N1 Sm1 106.5(3) . . ? C15 N2 C17 108.5(5) . . ? C15 N2 C18 111.7(5) . . ? C17 N2 C18 111.3(5) . . ? C15 N2 Sm1 100.9(4) . . ? C17 N2 Sm1 107.4(3) . . ? C18 N2 Sm1 116.4(3) . . ? C42 N3 C41 111.2(5) . . ? C42 N3 C44 108.2(6) . . ? C41 N3 C44 110.9(6) . . ? C42 N3 Sm2 106.7(4) . . ? C41 N3 Sm2 116.0(4) . . ? C44 N3 Sm2 103.3(4) . . ? C43 N4 C45 109.6(5) . . ? C43 N4 C46 113.2(5) . . ? C45 N4 C46 109.4(5) . . ? C43 N4 Sm2 105.3(4) . . ? C45 N4 Sm2 104.8(4) . . ? C46 N4 Sm2 114.1(3) . . ? C57 N5 C58 124.5(5) . . ? C57 N5 Sm1 97.7(3) . . ? C58 N5 Sm1 136.8(4) . . ? C57 N6 C61 118.7(5) . . ? C57 N6 Sm1 90.7(3) . . ? C61 N6 Sm1 147.3(4) . . ? C64 N7 C65 120.7(5) . . ? C64 N7 Sm2 92.4(3) . . ? C65 N7 Sm2 142.5(4) . . ? C64 N8 C68 120.0(5) . . ? C64 N8 Sm2 90.9(3) . . ? C68 N8 Sm2 143.8(4) . . ? O1 C1 C6 118.6(5) . . ? O1 C1 C2 122.4(5) . . ? C6 C1 C2 118.9(5) . . ? C3 C2 C1 117.6(6) . . ? C3 C2 C19 121.3(6) . . ? C1 C2 C19 121.0(5) . . ? C4 C3 C2 123.8(6) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C5 C4 C3 117.6(6) . . ? C5 C4 C23 122.5(7) . . ? C3 C4 C23 119.9(7) . . ? C4 C5 C6 121.3(6) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 120.7(6) . . ? C5 C6 C13 118.3(6) . . ? C1 C6 C13 120.9(5) . . ? O2 C7 C12 119.0(5) . . ? O2 C7 C8 120.2(6) . . ? C12 C7 C8 120.8(6) . . ? C9 C8 C7 116.1(6) . . ? C9 C8 C24 121.2(6) . . ? C7 C8 C24 122.7(6) . . ? C10 C9 C8 124.3(6) . . ? C10 C9 H9 117.8 . . ? C8 C9 H9 117.8 . . ? C11 C10 C9 117.5(6) . . ? C11 C10 C28 120.9(7) . . ? C9 C10 C28 121.6(7) . . ? C10 C11 C12 122.3(7) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C11 C12 C7 119.1(6) . . ? C11 C12 C18 118.6(6) . . ? C7 C12 C18 122.0(6) . . ? N1 C13 C6 114.4(5) . . ? N1 C13 H13A 108.7 . . ? C6 C13 H13A 108.7 . . ? N1 C13 H13B 108.7 . . ? C6 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? N1 C14 C15 107.7(5) . . ? N1 C14 H14A 110.2 . . ? C15 C14 H14A 110.2 . . ? N1 C14 H14B 110.2 . . ? C15 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? N2 C15 C14 107.6(5) . . ? N2 C15 H15A 110.2 . . ? C14 C15 H15A 110.2 . . ? N2 C15 H15B 110.2 . . ? C14 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? N1 C16 C17 106.8(5) . . ? N1 C16 H16A 110.4 . . ? C17 C16 H16A 110.4 . . ? N1 C16 H16B 110.4 . . ? C17 C16 H16B 110.4 . . ? H16A C16 H16B 108.6 . . ? N2 C17 C16 108.5(5) . . ? N2 C17 H17A 110.0 . . ? C16 C17 H17A 110.0 . . ? N2 C17 H17B 110.0 . . ? C16 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? N2 C18 C12 115.0(5) . . ? N2 C18 H18A 108.5 . . ? C12 C18 H18A 108.5 . . ? N2 C18 H18B 108.5 . . ? C12 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? C2 C19 C21 109.2(6) . . ? C2 C19 C22 111.4(6) . . ? C21 C19 C22 110.0(6) . . ? C2 C19 C20 112.3(6) . . ? C21 C19 C20 106.5(6) . . ? C22 C19 C20 107.3(6) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C4 C23 H23A 109.5 . . ? C4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C27 106.7(6) . . ? C25 C24 C8 112.2(6) . . ? C27 C24 C8 109.4(6) . . ? C25 C24 C26 108.7(6) . . ? C27 C24 C26 107.8(6) . . ? C8 C24 C26 111.8(6) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C10 C28 H28A 109.5 . . ? C10 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C10 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C30 122.6(10) . . ? O3 C29 C34 118.6(8) . . ? C30 C29 C34 118.8(8) . . ? C29 C30 C31 117.7(10) . . ? C29 C30 C47 120.4(8) . . ? C31 C30 C47 121.8(9) . . ? C32 C31 C30 122.3(9) . . ? C32 C31 H31 118.8 . . ? C30 C31 H31 118.8 . . ? C33 C32 C31 119.9(9) . . ? C33 C32 C51 120.0(11) . . ? C31 C32 C51 120.1(10) . . ? C32 C33 C34 120.6(10) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C33 C34 C29 120.6(9) . . ? C33 C34 C41 118.0(9) . . ? C29 C34 C41 121.3(7) . . ? O4 C35 C40 119.8(5) . . ? O4 C35 C36 122.4(6) . . ? C40 C35 C36 117.8(6) . . ? C37 C36 C35 118.0(6) . . ? C37 C36 C52 120.6(6) . . ? C35 C36 C52 121.3(6) . . ? C38 C37 C36 124.1(6) . . ? C38 C37 H37 118.0 . . ? C36 C37 H37 118.0 . . ? C37 C38 C39 116.6(6) . . ? C37 C38 C56 121.9(6) . . ? C39 C38 C56 121.5(7) . . ? C40 C39 C38 121.8(6) . . ? C40 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? C39 C40 C35 121.6(6) . . ? C39 C40 C46 117.4(6) . . ? C35 C40 C46 121.0(5) . . ? N3 C41 C34 114.2(7) . . ? N3 C41 H41A 108.7 . . ? C34 C41 H41A 108.7 . . ? N3 C41 H41B 108.7 . . ? C34 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? N3 C42 C43 108.7(5) . . ? N3 C42 H42A 109.9 . . ? C43 C42 H42A 109.9 . . ? N3 C42 H42B 109.9 . . ? C43 C42 H42B 109.9 . . ? H42A C42 H42B 108.3 . . ? N4 C43 C42 109.9(5) . . ? N4 C43 H43A 109.7 . . ? C42 C43 H43A 109.7 . . ? N4 C43 H43B 109.7 . . ? C42 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? N3 C44 C45 108.7(6) . . ? N3 C44 H44A 109.9 . . ? C45 C44 H44A 109.9 . . ? N3 C44 H44B 109.9 . . ? C45 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? N4 C45 C44 108.9(6) . . ? N4 C45 H45A 109.9 . . ? C44 C45 H45A 109.9 . . ? N4 C45 H45B 109.9 . . ? C44 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? N4 C46 C40 115.2(5) . . ? N4 C46 H46A 108.5 . . ? C40 C46 H46A 108.5 . . ? N4 C46 H46B 108.5 . . ? C40 C46 H46B 108.5 . . ? H46A C46 H46B 107.5 . . ? C30 C47 C49 109.3(8) . . ? C30 C47 C50 111.2(10) . . ? C49 C47 C50 110.8(11) . . ? C30 C47 C48 113.3(10) . . ? C49 C47 C48 104.8(10) . . ? C50 C47 C48 107.3(8) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C32 C51 H51A 109.5 . . ? C32 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C32 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C54 C52 C53 107.0(7) . . ? C54 C52 C55 110.6(7) . . ? C53 C52 C55 107.5(6) . . ? C54 C52 C36 110.5(6) . . ? C53 C52 C36 112.6(6) . . ? C55 C52 C36 108.6(6) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C38 C56 H56A 109.5 . . ? C38 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C38 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N6 C57 N5 115.5(5) . . ? N6 C57 C64 125.8(5) . . ? N5 C57 C64 118.6(5) . . ? N6 C57 Sm1 62.0(3) . . ? N5 C57 Sm1 54.9(3) . . ? C64 C57 Sm1 163.9(4) . . ? N5 C58 C59 110.7(6) . . ? N5 C58 C60 110.9(6) . . ? C59 C58 C60 107.6(6) . . ? N5 C58 H58 109.2 . . ? C59 C58 H58 109.2 . . ? C60 C58 H58 109.2 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N6 C61 C63 110.5(5) . . ? N6 C61 C62 110.6(5) . . ? C63 C61 C62 110.6(6) . . ? N6 C61 H61 108.3 . . ? C63 C61 H61 108.3 . . ? C62 C61 H61 108.3 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N8 C64 N7 115.8(5) . . ? N8 C64 C57 122.6(5) . . ? N7 C64 C57 121.0(5) . . ? N8 C64 Sm2 61.2(3) . . ? N7 C64 Sm2 59.7(3) . . ? C57 C64 Sm2 150.5(4) . . ? N7 C65 C66 111.5(5) . . ? N7 C65 C67 107.9(5) . . ? C66 C65 C67 109.9(6) . . ? N7 C65 H65 109.2 . . ? C66 C65 H65 109.2 . . ? C67 C65 H65 109.2 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N8 C68 C69 111.5(5) . . ? N8 C68 C70 109.2(5) . . ? C69 C68 C70 109.8(5) . . ? N8 C68 H68 108.8 . . ? C69 C68 H68 108.8 . . ? C70 C68 H68 108.8 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O5 C71 C72 100.3(18) . . ? O5' C71' C72' 111(2) . . ? C71 C72 C73 106.6(19) . . ? C73' C72' C71' 106(2) . . ? C72 C73 C74 104.7(18) . . ? C72' C73' C74' 95.2(19) . . ? O5 C74 C73 103.6(19) . . ? O5' C74' C73' 112(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 O2 Sm1 O1 C1 145.2(6) . . . . ? N5 Sm1 O1 C1 -96.0(6) . . . . ? N1 Sm1 O1 C1 20.0(6) . . . . ? N6 Sm1 O1 C1 -64.3(7) . . . . ? N2 Sm1 O1 C1 65.6(6) . . . . ? C57 Sm1 O1 C1 -87.9(6) . . . . ? O1 Sm1 O2 C7 -78.1(6) . . . . ? N5 Sm1 O2 C7 176.9(6) . . . . ? N1 Sm1 O2 C7 3.8(7) . . . . ? N6 Sm1 O2 C7 120.0(6) . . . . ? N2 Sm1 O2 C7 27.9(6) . . . . ? C57 Sm1 O2 C7 148.2(6) . . . . ? O4 Sm2 O3 C29 109.5(8) . . . . ? N7 Sm2 O3 C29 -103.7(8) . . . . ? N8 Sm2 O3 C29 -132.6(8) . . . . ? N4 Sm2 O3 C29 27.2(9) . . . . ? N3 Sm2 O3 C29 -7.9(8) . . . . ? C64 Sm2 O3 C29 -121.7(8) . . . . ? O3 Sm2 O4 C35 -117.8(6) . . . . ? N7 Sm2 O4 C35 122.3(6) . . . . ? N8 Sm2 O4 C35 96.2(6) . . . . ? N4 Sm2 O4 C35 -0.7(6) . . . . ? N3 Sm2 O4 C35 -37.1(7) . . . . ? C64 Sm2 O4 C35 113.1(6) . . . . ? O2 Sm1 N1 C14 -26.8(4) . . . . ? O1 Sm1 N1 C14 73.3(4) . . . . ? N5 Sm1 N1 C14 160.2(4) . . . . ? N6 Sm1 N1 C14 -144.7(4) . . . . ? N2 Sm1 N1 C14 -54.3(4) . . . . ? C57 Sm1 N1 C14 -169.6(4) . . . . ? O2 Sm1 N1 C16 89.2(4) . . . . ? O1 Sm1 N1 C16 -170.7(4) . . . . ? N5 Sm1 N1 C16 -83.8(4) . . . . ? N6 Sm1 N1 C16 -28.7(3) . . . . ? N2 Sm1 N1 C16 61.7(3) . . . . ? C57 Sm1 N1 C16 -53.6(4) . . . . ? O2 Sm1 N1 C13 -153.1(3) . . . . ? O1 Sm1 N1 C13 -53.0(3) . . . . ? N5 Sm1 N1 C13 33.8(4) . . . . ? N6 Sm1 N1 C13 88.9(4) . . . . ? N2 Sm1 N1 C13 179.4(4) . . . . ? C57 Sm1 N1 C13 64.0(4) . . . . ? O2 Sm1 N2 C15 -98.2(3) . . . . ? O1 Sm1 N2 C15 6.3(4) . . . . ? N5 Sm1 N2 C15 148.1(4) . . . . ? N1 Sm1 N2 C15 59.7(3) . . . . ? N6 Sm1 N2 C15 158.3(3) . . . . ? C57 Sm1 N2 C15 159.2(3) . . . . ? O2 Sm1 N2 C17 148.4(4) . . . . ? O1 Sm1 N2 C17 -107.1(4) . . . . ? N5 Sm1 N2 C17 34.6(5) . . . . ? N1 Sm1 N2 C17 -53.8(3) . . . . ? N6 Sm1 N2 C17 44.8(4) . . . . ? C57 Sm1 N2 C17 45.7(4) . . . . ? O2 Sm1 N2 C18 22.8(4) . . . . ? O1 Sm1 N2 C18 127.3(4) . . . . ? N5 Sm1 N2 C18 -90.9(5) . . . . ? N1 Sm1 N2 C18 -179.3(4) . . . . ? N6 Sm1 N2 C18 -80.7(4) . . . . ? C57 Sm1 N2 C18 -79.8(4) . . . . ? O3 Sm2 N3 C42 89.2(4) . . . . ? O4 Sm2 N3 C42 -13.2(5) . . . . ? N7 Sm2 N3 C42 179.7(4) . . . . ? N8 Sm2 N3 C42 -130.3(4) . . . . ? N4 Sm2 N3 C42 -55.2(4) . . . . ? C64 Sm2 N3 C42 -162.2(4) . . . . ? O3 Sm2 N3 C41 -35.3(5) . . . . ? O4 Sm2 N3 C41 -137.7(5) . . . . ? N7 Sm2 N3 C41 55.2(5) . . . . ? N8 Sm2 N3 C41 105.2(5) . . . . ? N4 Sm2 N3 C41 -179.7(5) . . . . ? C64 Sm2 N3 C41 73.3(5) . . . . ? O3 Sm2 N3 C44 -156.8(4) . . . . ? O4 Sm2 N3 C44 100.8(4) . . . . ? N7 Sm2 N3 C44 -66.3(4) . . . . ? N8 Sm2 N3 C44 -16.3(5) . . . . ? N4 Sm2 N3 C44 58.8(4) . . . . ? C64 Sm2 N3 C44 -48.2(4) . . . . ? O3 Sm2 N4 C43 17.1(4) . . . . ? O4 Sm2 N4 C43 -86.1(4) . . . . ? N7 Sm2 N4 C43 133.0(4) . . . . ? N8 Sm2 N4 C43 -175.6(4) . . . . ? N3 Sm2 N4 C43 57.2(4) . . . . ? C64 Sm2 N4 C43 164.9(4) . . . . ? O3 Sm2 N4 C45 -98.4(4) . . . . ? O4 Sm2 N4 C45 158.4(4) . . . . ? N7 Sm2 N4 C45 17.5(5) . . . . ? N8 Sm2 N4 C45 68.9(4) . . . . ? N3 Sm2 N4 C45 -58.3(4) . . . . ? C64 Sm2 N4 C45 49.4(4) . . . . ? O3 Sm2 N4 C46 142.0(4) . . . . ? O4 Sm2 N4 C46 38.7(4) . . . . ? N7 Sm2 N4 C46 -102.2(4) . . . . ? N8 Sm2 N4 C46 -50.8(4) . . . . ? N3 Sm2 N4 C46 -178.0(4) . . . . ? C64 Sm2 N4 C46 -70.3(4) . . . . ? O2 Sm1 N5 C57 -82.1(4) . . . . ? O1 Sm1 N5 C57 164.8(3) . . . . ? N1 Sm1 N5 C57 91.8(4) . . . . ? N6 Sm1 N5 C57 8.0(3) . . . . ? N2 Sm1 N5 C57 20.6(5) . . . . ? O2 Sm1 N5 C58 86.4(6) . . . . ? O1 Sm1 N5 C58 -26.7(6) . . . . ? N1 Sm1 N5 C58 -99.6(6) . . . . ? N6 Sm1 N5 C58 176.5(7) . . . . ? N2 Sm1 N5 C58 -170.9(5) . . . . ? C57 Sm1 N5 C58 168.5(8) . . . . ? O2 Sm1 N6 C57 102.9(3) . . . . ? O1 Sm1 N6 C57 -48.2(4) . . . . ? N5 Sm1 N6 C57 -8.0(3) . . . . ? N1 Sm1 N6 C57 -123.0(3) . . . . ? N2 Sm1 N6 C57 178.4(3) . . . . ? O2 Sm1 N6 C61 -52.5(7) . . . . ? O1 Sm1 N6 C61 156.4(6) . . . . ? N5 Sm1 N6 C61 -163.4(8) . . . . ? N1 Sm1 N6 C61 81.6(7) . . . . ? N2 Sm1 N6 C61 23.0(7) . . . . ? C57 Sm1 N6 C61 -155.4(9) . . . . ? O3 Sm2 N7 C64 -143.1(3) . . . . ? O4 Sm2 N7 C64 -18.1(5) . . . . ? N8 Sm2 N7 C64 14.8(3) . . . . ? N4 Sm2 N7 C64 88.0(4) . . . . ? N3 Sm2 N7 C64 144.2(3) . . . . ? O3 Sm2 N7 C65 10.4(6) . . . . ? O4 Sm2 N7 C65 135.4(6) . . . . ? N8 Sm2 N7 C65 168.3(7) . . . . ? N4 Sm2 N7 C65 -118.5(6) . . . . ? N3 Sm2 N7 C65 -62.3(6) . . . . ? C64 Sm2 N7 C65 153.5(8) . . . . ? O3 Sm2 N8 C64 21.7(5) . . . . ? O4 Sm2 N8 C64 145.1(3) . . . . ? N7 Sm2 N8 C64 -14.8(3) . . . . ? N4 Sm2 N8 C64 -140.8(3) . . . . ? N3 Sm2 N8 C64 -84.7(4) . . . . ? O3 Sm2 N8 C68 -128.4(6) . . . . ? O4 Sm2 N8 C68 -4.9(6) . . . . ? N7 Sm2 N8 C68 -164.9(7) . . . . ? N4 Sm2 N8 C68 69.1(6) . . . . ? N3 Sm2 N8 C68 125.2(6) . . . . ? C64 Sm2 N8 C68 -150.1(8) . . . . ? Sm1 O1 C1 C6 5.8(9) . . . . ? Sm1 O1 C1 C2 -170.5(4) . . . . ? O1 C1 C2 C3 -179.2(5) . . . . ? C6 C1 C2 C3 4.5(9) . . . . ? O1 C1 C2 C19 3.4(9) . . . . ? C6 C1 C2 C19 -172.9(6) . . . . ? C1 C2 C3 C4 -2.2(10) . . . . ? C19 C2 C3 C4 175.1(6) . . . . ? C2 C3 C4 C5 -1.0(10) . . . . ? C2 C3 C4 C23 -179.7(6) . . . . ? C3 C4 C5 C6 2.0(10) . . . . ? C23 C4 C5 C6 -179.4(7) . . . . ? C4 C5 C6 C1 0.3(10) . . . . ? C4 C5 C6 C13 -177.7(6) . . . . ? O1 C1 C6 C5 179.9(6) . . . . ? C2 C1 C6 C5 -3.6(9) . . . . ? O1 C1 C6 C13 -2.2(9) . . . . ? C2 C1 C6 C13 174.3(6) . . . . ? Sm1 O2 C7 C12 -40.8(9) . . . . ? Sm1 O2 C7 C8 139.6(5) . . . . ? O2 C7 C8 C9 178.8(5) . . . . ? C12 C7 C8 C9 -0.7(8) . . . . ? O2 C7 C8 C24 -3.8(9) . . . . ? C12 C7 C8 C24 176.7(6) . . . . ? C7 C8 C9 C10 0.3(10) . . . . ? C24 C8 C9 C10 -177.1(6) . . . . ? C8 C9 C10 C11 0.8(10) . . . . ? C8 C9 C10 C28 179.7(7) . . . . ? C9 C10 C11 C12 -1.5(10) . . . . ? C28 C10 C11 C12 179.5(6) . . . . ? C10 C11 C12 C7 1.2(9) . . . . ? C10 C11 C12 C18 -172.4(6) . . . . ? O2 C7 C12 C11 -179.6(5) . . . . ? C8 C7 C12 C11 -0.1(9) . . . . ? O2 C7 C12 C18 -6.2(8) . . . . ? C8 C7 C12 C18 173.3(5) . . . . ? C14 N1 C13 C6 -44.9(7) . . . . ? C16 N1 C13 C6 -169.8(5) . . . . ? Sm1 N1 C13 C6 79.1(5) . . . . ? C5 C6 C13 N1 130.8(6) . . . . ? C1 C6 C13 N1 -47.1(8) . . . . ? C16 N1 C14 C15 -72.5(6) . . . . ? C13 N1 C14 C15 161.0(5) . . . . ? Sm1 N1 C14 C15 39.6(6) . . . . ? C17 N2 C15 C14 51.1(6) . . . . ? C18 N2 C15 C14 174.1(5) . . . . ? Sm1 N2 C15 C14 -61.6(5) . . . . ? N1 C14 C15 N2 17.2(7) . . . . ? C14 N1 C16 C17 52.3(6) . . . . ? C13 N1 C16 C17 -179.2(5) . . . . ? Sm1 N1 C16 C17 -65.5(5) . . . . ? C15 N2 C17 C16 -71.2(6) . . . . ? C18 N2 C17 C16 165.5(5) . . . . ? Sm1 N2 C17 C16 37.0(5) . . . . ? N1 C16 C17 N2 16.6(6) . . . . ? C15 N2 C18 C12 56.4(7) . . . . ? C17 N2 C18 C12 177.8(5) . . . . ? Sm1 N2 C18 C12 -58.7(6) . . . . ? C11 C12 C18 N2 -131.9(6) . . . . ? C7 C12 C18 N2 54.7(8) . . . . ? C3 C2 C19 C21 -116.6(7) . . . . ? C1 C2 C19 C21 60.6(8) . . . . ? C3 C2 C19 C22 121.7(7) . . . . ? C1 C2 C19 C22 -61.0(8) . . . . ? C3 C2 C19 C20 1.3(9) . . . . ? C1 C2 C19 C20 178.6(6) . . . . ? C9 C8 C24 C25 -1.5(9) . . . . ? C7 C8 C24 C25 -178.7(6) . . . . ? C9 C8 C24 C27 116.7(7) . . . . ? C7 C8 C24 C27 -60.6(8) . . . . ? C9 C8 C24 C26 -123.9(7) . . . . ? C7 C8 C24 C26 58.8(8) . . . . ? Sm2 O3 C29 C30 -157.3(6) . . . . ? Sm2 O3 C29 C34 23.1(13) . . . . ? O3 C29 C30 C31 176.0(7) . . . . ? C34 C29 C30 C31 -4.4(11) . . . . ? O3 C29 C30 C47 -2.9(13) . . . . ? C34 C29 C30 C47 176.7(8) . . . . ? C29 C30 C31 C32 2.0(12) . . . . ? C47 C30 C31 C32 -179.2(9) . . . . ? C30 C31 C32 C33 1.3(12) . . . . ? C30 C31 C32 C51 179.5(8) . . . . ? C31 C32 C33 C34 -2.1(12) . . . . ? C51 C32 C33 C34 179.7(8) . . . . ? C32 C33 C34 C29 -0.4(12) . . . . ? C32 C33 C34 C41 176.2(7) . . . . ? O3 C29 C34 C33 -176.6(6) . . . . ? C30 C29 C34 C33 3.8(12) . . . . ? O3 C29 C34 C41 6.9(12) . . . . ? C30 C29 C34 C41 -172.7(7) . . . . ? Sm2 O4 C35 C40 -14.8(10) . . . . ? Sm2 O4 C35 C36 164.7(5) . . . . ? O4 C35 C36 C37 -176.4(5) . . . . ? C40 C35 C36 C37 3.1(8) . . . . ? O4 C35 C36 C52 3.6(9) . . . . ? C40 C35 C36 C52 -176.9(6) . . . . ? C35 C36 C37 C38 -0.5(9) . . . . ? C52 C36 C37 C38 179.6(6) . . . . ? C36 C37 C38 C39 -1.4(9) . . . . ? C36 C37 C38 C56 178.1(6) . . . . ? C37 C38 C39 C40 0.7(9) . . . . ? C56 C38 C39 C40 -178.9(6) . . . . ? C38 C39 C40 C35 2.1(9) . . . . ? C38 C39 C40 C46 -175.1(5) . . . . ? O4 C35 C40 C39 175.5(5) . . . . ? C36 C35 C40 C39 -4.0(8) . . . . ? O4 C35 C40 C46 -7.3(8) . . . . ? C36 C35 C40 C46 173.1(5) . . . . ? C42 N3 C41 C34 -55.3(8) . . . . ? C44 N3 C41 C34 -175.7(6) . . . . ? Sm2 N3 C41 C34 66.9(7) . . . . ? C33 C34 C41 N3 131.2(7) . . . . ? C29 C34 C41 N3 -52.2(10) . . . . ? C41 N3 C42 C43 173.9(6) . . . . ? C44 N3 C42 C43 -64.0(7) . . . . ? Sm2 N3 C42 C43 46.6(7) . . . . ? C45 N4 C43 C42 58.3(8) . . . . ? C46 N4 C43 C42 -179.3(6) . . . . ? Sm2 N4 C43 C42 -53.9(6) . . . . ? N3 C42 C43 N4 4.5(8) . . . . ? C42 N3 C44 C45 59.8(7) . . . . ? C41 N3 C44 C45 -177.9(6) . . . . ? Sm2 N3 C44 C45 -53.1(6) . . . . ? C43 N4 C45 C44 -61.9(8) . . . . ? C46 N4 C45 C44 173.4(6) . . . . ? Sm2 N4 C45 C44 50.7(6) . . . . ? N3 C44 C45 N4 2.1(8) . . . . ? C43 N4 C46 C40 51.6(7) . . . . ? C45 N4 C46 C40 174.2(6) . . . . ? Sm2 N4 C46 C40 -68.8(5) . . . . ? C39 C40 C46 N4 -130.6(6) . . . . ? C35 C40 C46 N4 52.1(7) . . . . ? C29 C30 C47 C49 -62.0(11) . . . . ? C31 C30 C47 C49 119.2(9) . . . . ? C29 C30 C47 C50 60.6(12) . . . . ? C31 C30 C47 C50 -118.2(9) . . . . ? C29 C30 C47 C48 -178.4(8) . . . . ? C31 C30 C47 C48 2.8(14) . . . . ? C37 C36 C52 C54 116.0(7) . . . . ? C35 C36 C52 C54 -63.9(8) . . . . ? C37 C36 C52 C53 -3.5(10) . . . . ? C35 C36 C52 C53 176.5(7) . . . . ? C37 C36 C52 C55 -122.5(7) . . . . ? C35 C36 C52 C55 57.5(8) . . . . ? C61 N6 C57 N5 178.0(5) . . . . ? Sm1 N6 C57 N5 12.9(5) . . . . ? C61 N6 C57 C64 1.8(8) . . . . ? Sm1 N6 C57 C64 -163.3(5) . . . . ? C61 N6 C57 Sm1 165.1(5) . . . . ? C58 N5 C57 N6 175.5(5) . . . . ? Sm1 N5 C57 N6 -13.9(5) . . . . ? C58 N5 C57 C64 -7.9(8) . . . . ? Sm1 N5 C57 C64 162.6(4) . . . . ? C58 N5 C57 Sm1 -170.5(7) . . . . ? O2 Sm1 C57 N6 -85.3(3) . . . . ? O1 Sm1 C57 N6 147.9(3) . . . . ? N5 Sm1 C57 N6 165.7(5) . . . . ? N1 Sm1 C57 N6 64.5(3) . . . . ? N2 Sm1 C57 N6 -1.9(4) . . . . ? O2 Sm1 C57 N5 108.9(3) . . . . ? O1 Sm1 C57 N5 -17.8(4) . . . . ? N1 Sm1 C57 N5 -101.2(4) . . . . ? N6 Sm1 C57 N5 -165.7(5) . . . . ? N2 Sm1 C57 N5 -167.7(3) . . . . ? O2 Sm1 C57 C64 37.8(14) . . . . ? O1 Sm1 C57 C64 -88.9(13) . . . . ? N5 Sm1 C57 C64 -71.1(13) . . . . ? N1 Sm1 C57 C64 -172.3(13) . . . . ? N6 Sm1 C57 C64 123.2(14) . . . . ? N2 Sm1 C57 C64 121.2(13) . . . . ? C57 N5 C58 C59 -120.8(6) . . . . ? Sm1 N5 C58 C59 73.0(8) . . . . ? C57 N5 C58 C60 119.8(7) . . . . ? Sm1 N5 C58 C60 -46.4(8) . . . . ? C57 N6 C61 C63 -120.9(6) . . . . ? Sm1 N6 C61 C63 30.7(9) . . . . ? C57 N6 C61 C62 116.3(6) . . . . ? Sm1 N6 C61 C62 -92.1(8) . . . . ? C68 N8 C64 N7 -174.8(5) . . . . ? Sm2 N8 C64 N7 25.2(5) . . . . ? C68 N8 C64 C57 14.2(8) . . . . ? Sm2 N8 C64 C57 -145.9(5) . . . . ? C68 N8 C64 Sm2 160.1(6) . . . . ? C65 N7 C64 N8 172.8(5) . . . . ? Sm2 N7 C64 N8 -25.6(5) . . . . ? C65 N7 C64 C57 -16.0(8) . . . . ? Sm2 N7 C64 C57 145.6(5) . . . . ? C65 N7 C64 Sm2 -161.6(6) . . . . ? N6 C57 C64 N8 -99.5(7) . . . . ? N5 C57 C64 N8 84.4(7) . . . . ? Sm1 C57 C64 N8 146.2(11) . . . . ? N6 C57 C64 N7 89.9(7) . . . . ? N5 C57 C64 N7 -86.2(7) . . . . ? Sm1 C57 C64 N7 -24.4(16) . . . . ? N6 C57 C64 Sm2 172.2(5) . . . . ? N5 C57 C64 Sm2 -3.9(10) . . . . ? Sm1 C57 C64 Sm2 57.9(17) . . . . ? O3 Sm2 C64 N8 -165.2(3) . . . . ? O4 Sm2 C64 N8 -38.7(4) . . . . ? N7 Sm2 C64 N8 153.7(5) . . . . ? N4 Sm2 C64 N8 45.2(4) . . . . ? N3 Sm2 C64 N8 112.4(3) . . . . ? O3 Sm2 C64 N7 41.2(4) . . . . ? O4 Sm2 C64 N7 167.6(3) . . . . ? N8 Sm2 C64 N7 -153.7(5) . . . . ? N4 Sm2 C64 N7 -108.5(3) . . . . ? N3 Sm2 C64 N7 -41.3(4) . . . . ? O3 Sm2 C64 C57 -59.1(8) . . . . ? O4 Sm2 C64 C57 67.4(8) . . . . ? N7 Sm2 C64 C57 -100.3(8) . . . . ? N8 Sm2 C64 C57 106.1(8) . . . . ? N4 Sm2 C64 C57 151.2(7) . . . . ? N3 Sm2 C64 C57 -141.6(7) . . . . ? C64 N7 C65 C66 127.3(6) . . . . ? Sm2 N7 C65 C66 -21.5(9) . . . . ? C64 N7 C65 C67 -112.0(6) . . . . ? Sm2 N7 C65 C67 99.2(7) . . . . ? C64 N8 C68 C69 -130.2(6) . . . . ? Sm2 N8 C68 C69 14.6(9) . . . . ? C64 N8 C68 C70 108.3(6) . . . . ? Sm2 N8 C68 C70 -106.8(7) . . . . ? C74 O5 C71 C72 41(4) . . . . ? C74' O5' C71' C72' -5(5) . . . . ? O5 C71 C72 C73 -33(4) . . . . ? O5' C71' C72' C73' -17(6) . . . . ? C71 C72 C73 C74 15(5) . . . . ? C71' C72' C73' C74' 28(5) . . . . ? C71 O5 C74 C73 -31(4) . . . . ? C72 C73 C74 O5 9(5) . . . . ? C71' O5' C74' C73' 26(5) . . . . ? C72' C73' C74' O5' -34(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.812 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.096 #===END #============================================================================== data_4 #(Complex 4) _database_code_depnum_ccdc_archive 'CCDC 807557' #TrackingRef '- revised.CIF' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C69 H102 N6 O4 Sm2, 5.5(C4 H8 O)' _chemical_formula_sum 'C91 H146 N6 O9.50 Sm2' _chemical_formula_weight 1776.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.8914(16) _cell_length_b 14.8306(15) _cell_length_c 41.133(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.820(3) _cell_angle_gamma 90.00 _cell_volume 9019.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 30721 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3736 _exptl_absorpt_coefficient_mu 1.347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.451 _exptl_absorpt_correction_T_max 0.933 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62228 _diffrn_reflns_av_R_equivalents 0.1113 _diffrn_reflns_av_sigmaI/netI 0.1166 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.50 _reflns_number_total 16663 _reflns_number_gt 12146 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+80.0861P] 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 16663 _refine_ls_number_parameters 918 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.1394 _refine_ls_R_factor_gt 0.1039 _refine_ls_wR_factor_ref 0.2320 _refine_ls_wR_factor_gt 0.2115 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.003 _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 0.62356(3) 0.56609(4) 0.689299(13) 0.03440(17) Uani 1 1 d . . . Sm2 Sm 0.49271(4) 0.53063(4) 0.616203(13) 0.03629(17) Uani 1 1 d . . . O1 O 0.4645(4) 0.5218(4) 0.67188(17) 0.0360(16) Uani 1 1 d . . . O2 O 0.7287(4) 0.6760(5) 0.69784(18) 0.0408(18) Uani 1 1 d . . . O3 O 0.5488(4) 0.6638(5) 0.64757(17) 0.0387(17) Uani 1 1 d . . . O4 O 0.3985(5) 0.4144(5) 0.60753(18) 0.0446(18) Uani 1 1 d . . . N1 N 0.5808(5) 0.4443(6) 0.7292(2) 0.037(2) Uani 1 1 d . . . N2 N 0.6826(5) 0.5643(6) 0.7534(2) 0.0337(19) Uani 1 1 d . . . N3 N 0.5324(6) 0.6504(6) 0.5748(2) 0.040(2) Uani 1 1 d . . . N4 N 0.3944(6) 0.5559(6) 0.5578(2) 0.045(2) Uani 1 1 d . . . N5 N 0.7095(6) 0.4606(6) 0.6636(2) 0.041(2) Uani 1 1 d . . . N6 N 0.6276(6) 0.4569(6) 0.6075(2) 0.039(2) Uani 1 1 d . . . C1 C 0.3989(7) 0.4750(7) 0.6849(3) 0.042(3) Uani 1 1 d . . . C2 C 0.3046(7) 0.4985(8) 0.6810(3) 0.041(3) Uani 1 1 d . . . C3 C 0.2455(8) 0.4481(9) 0.6970(3) 0.052(3) Uani 1 1 d . . . H3 H 0.1833 0.4641 0.6939 0.062 Uiso 1 1 calc R . . C4 C 0.2710(8) 0.3761(9) 0.7171(3) 0.054(3) Uani 1 1 d . . . C5 C 0.3627(7) 0.3535(8) 0.7212(3) 0.047(3) Uani 1 1 d . . . H5 H 0.3827 0.3049 0.7353 0.056 Uiso 1 1 calc R . . C6 C 0.4241(6) 0.3996(7) 0.7055(2) 0.035(2) Uani 1 1 d . . . C7 C 0.8124(7) 0.6717(7) 0.7136(3) 0.040(3) Uani 1 1 d . . . C8 C 0.8918(7) 0.6907(7) 0.6978(3) 0.042(3) Uani 1 1 d . . . C9 C 0.9751(7) 0.6697(8) 0.7155(3) 0.049(3) Uani 1 1 d . . . H9 H 1.0279 0.6793 0.7051 0.059 Uiso 1 1 calc R . . C10 C 0.9866(7) 0.6354(8) 0.7478(3) 0.045(3) Uani 1 1 d . . . C11 C 0.9113(7) 0.6302(8) 0.7634(3) 0.044(3) Uani 1 1 d . . . H11 H 0.9176 0.6147 0.7860 0.053 Uiso 1 1 calc R . . C12 C 0.8246(7) 0.6471(7) 0.7472(3) 0.038(3) Uani 1 1 d . . . C13 C 0.5225(7) 0.3736(8) 0.7114(3) 0.041(3) Uani 1 1 d . . . H13A H 0.5282 0.3171 0.7243 0.049 Uiso 1 1 calc R . . H13B H 0.5446 0.3616 0.6901 0.049 Uiso 1 1 calc R . . C14 C 0.6679(7) 0.4020(7) 0.7425(3) 0.039(2) Uani 1 1 d . . . H14A H 0.6965 0.3728 0.7247 0.047 Uiso 1 1 calc R . . H14B H 0.6574 0.3555 0.7589 0.047 Uiso 1 1 calc R . . C15 C 0.7320(7) 0.4790(8) 0.7591(3) 0.047(3) Uani 1 1 d . . . H15A H 0.7461 0.4677 0.7829 0.056 Uiso 1 1 calc R . . H15B H 0.7893 0.4810 0.7492 0.056 Uiso 1 1 calc R . . C16 C 0.5411(7) 0.4850(8) 0.7569(3) 0.042(3) Uani 1 1 d . . . H16A H 0.5344 0.4387 0.7738 0.050 Uiso 1 1 calc R . . H16B H 0.4804 0.5096 0.7492 0.050 Uiso 1 1 calc R . . C17 C 0.6026(7) 0.5597(7) 0.7712(3) 0.040(3) Uani 1 1 d . . . H17A H 0.5699 0.6179 0.7693 0.049 Uiso 1 1 calc R . . H17B H 0.6215 0.5477 0.7947 0.049 Uiso 1 1 calc R . . C18 C 0.7434(7) 0.6364(9) 0.7656(3) 0.052(3) Uani 1 1 d . . . H18A H 0.7647 0.6247 0.7889 0.062 Uiso 1 1 calc R . . H18B H 0.7093 0.6938 0.7643 0.062 Uiso 1 1 calc R . . C19 C 0.2626(7) 0.5817(8) 0.6616(3) 0.047(3) Uani 1 1 d . . . C20 C 0.2445(9) 0.6548(9) 0.6866(3) 0.061(3) Uani 1 1 d . . . H20A H 0.3020 0.6742 0.6986 0.091 Uiso 1 1 calc R . . H20B H 0.2054 0.6302 0.7020 0.091 Uiso 1 1 calc R . . H20C H 0.2146 0.7065 0.6750 0.091 Uiso 1 1 calc R . . C21 C 0.3183(7) 0.6232(8) 0.6362(3) 0.049(3) Uani 1 1 d . . . H21A H 0.2851 0.6741 0.6254 0.074 Uiso 1 1 calc R . . H21B H 0.3287 0.5776 0.6199 0.074 Uiso 1 1 calc R . . H21C H 0.3765 0.6443 0.6472 0.074 Uiso 1 1 calc R . . C22 C 0.1704(8) 0.5559(10) 0.6420(4) 0.070(4) Uani 1 1 d . . . H22A H 0.1488 0.6059 0.6275 0.105 Uiso 1 1 calc R . . H22B H 0.1261 0.5434 0.6572 0.105 Uiso 1 1 calc R . . H22C H 0.1782 0.5020 0.6288 0.105 Uiso 1 1 calc R . . C23 C 0.2019(9) 0.3218(11) 0.7346(4) 0.079(5) Uani 1 1 d . . . H23A H 0.1764 0.2731 0.7202 0.118 Uiso 1 1 calc R . . H23B H 0.1531 0.3619 0.7397 0.118 Uiso 1 1 calc R . . H23C H 0.2323 0.2960 0.7549 0.118 Uiso 1 1 calc R . . C24 C 0.8851(7) 0.7296(8) 0.6636(3) 0.045(3) Uani 1 1 d . . . C25 C 0.9772(8) 0.7527(9) 0.6532(3) 0.059(3) Uani 1 1 d . . . H25A H 1.0093 0.7937 0.6692 0.089 Uiso 1 1 calc R . . H25B H 0.9690 0.7820 0.6316 0.089 Uiso 1 1 calc R . . H25C H 1.0126 0.6974 0.6519 0.089 Uiso 1 1 calc R . . C26 C 0.8298(8) 0.8184(8) 0.6628(3) 0.051(3) Uani 1 1 d . . . H26A H 0.8620 0.8624 0.6776 0.076 Uiso 1 1 calc R . . H26B H 0.7703 0.8062 0.6697 0.076 Uiso 1 1 calc R . . H26C H 0.8222 0.8427 0.6405 0.076 Uiso 1 1 calc R . . C27 C 0.8369(8) 0.6645(10) 0.6380(3) 0.059(3) Uani 1 1 d . . . H27A H 0.8271 0.6946 0.6167 0.089 Uiso 1 1 calc R . . H27B H 0.7785 0.6467 0.6447 0.089 Uiso 1 1 calc R . . H27C H 0.8744 0.6108 0.6364 0.089 Uiso 1 1 calc R . . C28 C 1.0801(8) 0.6071(9) 0.7634(3) 0.060(3) Uani 1 1 d . . . H28A H 1.0925 0.6346 0.7851 0.089 Uiso 1 1 calc R . . H28B H 1.1256 0.6272 0.7496 0.089 Uiso 1 1 calc R . . H28C H 1.0825 0.5413 0.7654 0.089 Uiso 1 1 calc R . . C29 C 0.5729(7) 0.7518(8) 0.6421(3) 0.043(3) Uani 1 1 d . . . C30 C 0.5576(7) 0.8244(7) 0.6631(3) 0.041(3) Uani 1 1 d . . . C31 C 0.5876(8) 0.9070(9) 0.6542(3) 0.053(3) Uani 1 1 d . . . H31 H 0.5809 0.9553 0.6689 0.063 Uiso 1 1 calc R . . C32 C 0.6261(8) 0.9281(8) 0.6267(3) 0.055(3) Uani 1 1 d . . . C33 C 0.6335(7) 0.8585(9) 0.6049(3) 0.053(3) Uani 1 1 d . . . H33 H 0.6575 0.8706 0.5850 0.064 Uiso 1 1 calc R . . C34 C 0.6069(7) 0.7714(8) 0.6115(3) 0.044(3) Uani 1 1 d . . . C35 C 0.3730(8) 0.3606(8) 0.5822(3) 0.048(3) Uani 1 1 d . . . C36 C 0.3830(8) 0.2628(8) 0.5847(3) 0.053(3) Uani 1 1 d . . . C37 C 0.3560(9) 0.2144(9) 0.5558(3) 0.061(4) Uani 1 1 d . . . H37 H 0.3618 0.1506 0.5568 0.073 Uiso 1 1 calc R . . C38 C 0.3218(10) 0.2516(10) 0.5264(3) 0.066(4) Uani 1 1 d . . . C39 C 0.3088(8) 0.3451(10) 0.5253(3) 0.060(4) Uani 1 1 d . . . H39 H 0.2822 0.3722 0.5056 0.072 Uiso 1 1 calc R . . C40 C 0.3335(7) 0.3989(9) 0.5523(3) 0.049(3) Uani 1 1 d . . . C41 C 0.6176(7) 0.7002(8) 0.5872(3) 0.048(3) Uani 1 1 d . . . H41A H 0.6625 0.6559 0.5972 0.058 Uiso 1 1 calc R . . H41B H 0.6426 0.7277 0.5683 0.058 Uiso 1 1 calc R . . C42 C 0.5436(8) 0.5996(9) 0.5440(3) 0.049(3) Uani 1 1 d . . . H42A H 0.5991 0.5623 0.5473 0.058 Uiso 1 1 calc R . . H42B H 0.5494 0.6424 0.5259 0.058 Uiso 1 1 calc R . . C43 C 0.4611(7) 0.5396(8) 0.5355(3) 0.046(3) Uani 1 1 d . . . H43A H 0.4341 0.5520 0.5128 0.056 Uiso 1 1 calc R . . H43B H 0.4798 0.4755 0.5368 0.056 Uiso 1 1 calc R . . C44 C 0.4528(7) 0.7113(8) 0.5686(3) 0.045(3) Uani 1 1 d . . . H44A H 0.4640 0.7579 0.5523 0.054 Uiso 1 1 calc R . . H44B H 0.4416 0.7418 0.5891 0.054 Uiso 1 1 calc R . . C45 C 0.3701(8) 0.6532(8) 0.5555(3) 0.048(3) Uani 1 1 d . . . H45A H 0.3195 0.6653 0.5684 0.058 Uiso 1 1 calc R . . H45B H 0.3503 0.6691 0.5323 0.058 Uiso 1 1 calc R . . C46 C 0.3139(7) 0.4986(8) 0.5511(3) 0.046(3) Uani 1 1 d . . . H46A H 0.2829 0.5139 0.5292 0.056 Uiso 1 1 calc R . . H46B H 0.2717 0.5126 0.5673 0.056 Uiso 1 1 calc R . . C47 C 0.5048(7) 0.8176(8) 0.6928(3) 0.044(3) Uani 1 1 d . . . C48 C 0.5459(11) 0.8815(9) 0.7208(3) 0.072(4) Uani 1 1 d . . . H48A H 0.6092 0.8650 0.7274 0.108 Uiso 1 1 calc R . . H48B H 0.5116 0.8755 0.7396 0.108 Uiso 1 1 calc R . . H48C H 0.5427 0.9440 0.7130 0.108 Uiso 1 1 calc R . . C49 C 0.5028(7) 0.7248(8) 0.7096(3) 0.043(3) Uani 1 1 d . . . H49A H 0.4795 0.6793 0.6935 0.065 Uiso 1 1 calc R . . H49B H 0.4635 0.7278 0.7271 0.065 Uiso 1 1 calc R . . H49C H 0.5642 0.7082 0.7190 0.065 Uiso 1 1 calc R . . C50 C 0.4080(8) 0.8478(9) 0.6809(3) 0.061(4) Uani 1 1 d . . . H50A H 0.4088 0.9099 0.6729 0.091 Uiso 1 1 calc R . . H50B H 0.3712 0.8448 0.6992 0.091 Uiso 1 1 calc R . . H50C H 0.3820 0.8081 0.6632 0.091 Uiso 1 1 calc R . . C51 C 0.6621(10) 1.0220(9) 0.6204(4) 0.084(5) Uani 1 1 d . . . H51A H 0.6292 1.0670 0.6318 0.126 Uiso 1 1 calc R . . H51B H 0.6538 1.0345 0.5968 0.126 Uiso 1 1 calc R . . H51C H 0.7267 1.0250 0.6285 0.126 Uiso 1 1 calc R . . C52 C 0.4124(10) 0.2174(9) 0.6173(4) 0.064(4) Uani 1 1 d . . . C53 C 0.4108(11) 0.1130(10) 0.6148(4) 0.083(5) Uani 1 1 d . . . H53A H 0.3507 0.0931 0.6053 0.124 Uiso 1 1 calc R . . H53B H 0.4247 0.0870 0.6367 0.124 Uiso 1 1 calc R . . H53C H 0.4560 0.0931 0.6009 0.124 Uiso 1 1 calc R . . C54 C 0.3463(10) 0.2459(8) 0.6399(4) 0.077(5) Uani 1 1 d . . . H54A H 0.3502 0.3113 0.6432 0.116 Uiso 1 1 calc R . . H54B H 0.3605 0.2154 0.6610 0.116 Uiso 1 1 calc R . . H54C H 0.2850 0.2298 0.6304 0.116 Uiso 1 1 calc R . . C55 C 0.5117(10) 0.2463(9) 0.6294(4) 0.069(4) Uani 1 1 d . . . H55A H 0.5509 0.2310 0.6127 0.103 Uiso 1 1 calc R . . H55B H 0.5325 0.2146 0.6498 0.103 Uiso 1 1 calc R . . H55C H 0.5137 0.3115 0.6333 0.103 Uiso 1 1 calc R . . C56 C 0.2938(12) 0.1929(10) 0.4963(4) 0.085(5) Uani 1 1 d . . . H56A H 0.3466 0.1815 0.4848 0.128 Uiso 1 1 calc R . . H56B H 0.2472 0.2241 0.4817 0.128 Uiso 1 1 calc R . . H56C H 0.2698 0.1354 0.5033 0.128 Uiso 1 1 calc R . . C57 C 0.6442(6) 0.4769(6) 0.6395(3) 0.032(2) Uani 1 1 d . . . C58 C 0.7927(7) 0.4083(7) 0.6613(3) 0.038(2) Uani 1 1 d . . . H58 H 0.8113 0.4175 0.6390 0.046 Uiso 1 1 calc R . . C59 C 0.7784(7) 0.3061(7) 0.6664(3) 0.045(3) Uani 1 1 d . . . H59A H 0.7616 0.2954 0.6887 0.054 Uiso 1 1 calc R . . H59B H 0.7283 0.2841 0.6504 0.054 Uiso 1 1 calc R . . C60 C 0.8647(8) 0.2546(8) 0.6621(3) 0.053(3) Uani 1 1 d . . . H60A H 0.8788 0.2619 0.6393 0.063 Uiso 1 1 calc R . . H60B H 0.8554 0.1896 0.6660 0.063 Uiso 1 1 calc R . . C61 C 0.9453(8) 0.2891(9) 0.6861(3) 0.059(3) Uani 1 1 d . . . H61A H 1.0012 0.2572 0.6819 0.070 Uiso 1 1 calc R . . H61B H 0.9341 0.2762 0.7089 0.070 Uiso 1 1 calc R . . C62 C 0.9579(7) 0.3924(8) 0.6818(3) 0.052(3) Uani 1 1 d . . . H62A H 1.0076 0.4145 0.6980 0.062 Uiso 1 1 calc R . . H62B H 0.9739 0.4053 0.6596 0.062 Uiso 1 1 calc R . . C63 C 0.8705(7) 0.4396(8) 0.6868(3) 0.043(3) Uani 1 1 d . . . H63A H 0.8785 0.5056 0.6849 0.051 Uiso 1 1 calc R . . H63B H 0.8551 0.4266 0.7090 0.051 Uiso 1 1 calc R . . C64 C 0.6855(7) 0.3976(8) 0.5900(3) 0.041(3) Uani 1 1 d . . . H64 H 0.7127 0.3506 0.6056 0.049 Uiso 1 1 calc R . . C65 C 0.6289(8) 0.3497(9) 0.5610(3) 0.052(3) Uani 1 1 d . . . H65A H 0.5775 0.3174 0.5689 0.063 Uiso 1 1 calc R . . H65B H 0.6043 0.3948 0.5445 0.063 Uiso 1 1 calc R . . C66 C 0.6893(10) 0.2828(10) 0.5454(4) 0.069(4) Uani 1 1 d . . . H66A H 0.7095 0.2352 0.5616 0.083 Uiso 1 1 calc R . . H66B H 0.6538 0.2535 0.5265 0.083 Uiso 1 1 calc R . . C67 C 0.7709(9) 0.3276(11) 0.5342(4) 0.073(4) Uani 1 1 d . . . H67A H 0.8107 0.2810 0.5264 0.088 Uiso 1 1 calc R . . H67B H 0.7511 0.3682 0.5156 0.088 Uiso 1 1 calc R . . C68 C 0.8233(8) 0.3809(10) 0.5610(4) 0.066(4) Uani 1 1 d . . . H68A H 0.8731 0.4130 0.5519 0.079 Uiso 1 1 calc R . . H68B H 0.8506 0.3390 0.5781 0.079 Uiso 1 1 calc R . . C69 C 0.7634(7) 0.4512(8) 0.5769(3) 0.048(3) Uani 1 1 d . . . H69A H 0.7998 0.4832 0.5950 0.058 Uiso 1 1 calc R . . H69B H 0.7386 0.4961 0.5604 0.058 Uiso 1 1 calc R . . O5 O 0.926(3) -0.073(3) 0.5710(13) 0.207(10) Uiso 0.50 1 d PD A 1 O5' O 0.858(3) -0.055(3) 0.5701(13) 0.207(10) Uiso 0.50 1 d PD B 2 O6 O 0.092(3) 0.169(3) 0.5868(11) 0.162(6) Uiso 0.50 1 d PD C 1 O6' O 0.114(3) 0.194(3) 0.6054(10) 0.162(6) Uiso 0.50 1 d PD D 2 O7 O 0.272(4) 0.819(4) 0.5802(14) 0.215(9) Uiso 0.50 1 d PD E 1 O7' O 0.193(3) 0.838(3) 0.5930(12) 0.215(9) Uiso 0.50 1 d PD F 2 O8 O 0.4239(19) 0.578(2) 0.8061(8) 0.116(4) Uiso 0.50 1 d PD G 1 O8' O 0.4321(19) 0.563(2) 0.8294(7) 0.116(4) Uiso 0.50 1 d PD H 2 O9 O 1.061(6) 0.579(4) 0.5453(17) 0.255(11) Uiso 0.50 1 d PD I 1 O9' O 1.026(4) 0.610(5) 0.5132(14) 0.255(11) Uiso 0.50 1 d PD J 2 O10 O 0.524(2) 1.013(2) 0.4726(9) 0.142(8) Uiso 0.50 1 d PD . 2 C70 C 0.930(5) -0.050(5) 0.5367(14) 0.207(10) Uiso 0.50 1 d PD A 1 C70' C 0.873(5) -0.026(5) 0.5372(13) 0.207(10) Uiso 0.50 1 d PD B 2 C71 C 0.896(5) 0.044(5) 0.5285(17) 0.207(10) Uiso 0.50 1 d PD A 1 C71' C 0.829(5) 0.060(4) 0.5453(17) 0.207(10) Uiso 0.50 1 d PD B 2 C72 C 0.868(5) 0.085(6) 0.5592(17) 0.207(10) Uiso 0.50 1 d PD A 1 C72' C 0.859(5) 0.090(5) 0.5796(18) 0.207(10) Uiso 0.50 1 d PD B 2 C73 C 0.902(7) 0.014(4) 0.5841(19) 0.207(10) Uiso 0.50 1 d PD A 1 C73' C 0.901(6) 0.006(5) 0.5952(18) 0.207(10) Uiso 0.50 1 d PD B 2 C74 C 0.092(4) 0.215(4) 0.5558(12) 0.162(6) Uiso 0.50 1 d PD C 1 C74' C 0.119(4) 0.205(4) 0.5702(11) 0.162(6) Uiso 0.50 1 d PD D 2 C75 C 0.101(5) 0.308(4) 0.5707(15) 0.162(6) Uiso 0.50 1 d PD C 1 C75' C 0.066(4) 0.286(4) 0.5556(14) 0.162(6) Uiso 0.50 1 d PD D 2 C76 C 0.085(5) 0.315(4) 0.6059(15) 0.162(6) Uiso 0.50 1 d PD C 1 C76' C 0.100(5) 0.344(4) 0.5843(14) 0.162(6) Uiso 0.50 1 d PD D 2 C77 C 0.044(4) 0.223(4) 0.6090(13) 0.162(6) Uiso 0.50 1 d PD C 1 C77' C 0.087(5) 0.286(3) 0.6131(15) 0.162(6) Uiso 0.50 1 d PD D 2 C78 C 0.228(5) 0.876(5) 0.6028(14) 0.215(9) Uiso 0.50 1 d PD E 1 C78' C 0.274(4) 0.899(4) 0.5929(14) 0.215(9) Uiso 0.50 1 d PD F 2 C79 C 0.182(5) 0.953(4) 0.5839(18) 0.215(9) Uiso 0.50 1 d PD E 1 C79' C 0.248(5) 0.944(4) 0.5601(17) 0.215(9) Uiso 0.50 1 d PD F 2 C80 C 0.211(5) 0.947(5) 0.5507(16) 0.215(9) Uiso 0.50 1 d PD E 1 C80' C 0.211(6) 0.864(5) 0.5397(13) 0.215(9) Uiso 0.50 1 d PD F 2 C81 C 0.281(5) 0.873(5) 0.5515(17) 0.215(9) Uiso 0.50 1 d PD E 1 C81' C 0.193(5) 0.789(4) 0.5623(15) 0.215(9) Uiso 0.50 1 d PD F 2 C82 C 0.330(2) 0.588(3) 0.7928(10) 0.116(4) Uiso 0.50 1 d PD G 1 C82' C 0.396(3) 0.595(3) 0.7966(9) 0.116(4) Uiso 0.50 1 d PD H 2 C83 C 0.283(3) 0.511(3) 0.8073(11) 0.116(4) Uiso 0.50 1 d PD G 1 C83' C 0.316(3) 0.532(3) 0.7887(11) 0.116(4) Uiso 0.50 1 d PD H 2 C84 C 0.353(3) 0.441(3) 0.8182(11) 0.116(4) Uiso 0.50 1 d PD G 1 C84' C 0.342(3) 0.446(3) 0.8064(9) 0.116(4) Uiso 0.50 1 d PD H 2 C85 C 0.436(3) 0.498(3) 0.8284(10) 0.116(4) Uiso 0.50 1 d PD G 1 C85' C 0.379(3) 0.488(3) 0.8390(9) 0.116(4) Uiso 0.50 1 d PD H 2 C86 C 1.063(7) 0.674(5) 0.536(2) 0.255(11) Uiso 0.50 1 d PD I 1 C86' C 1.076(7) 0.625(7) 0.5457(19) 0.255(11) Uiso 0.50 1 d PD J 2 C87 C 0.971(6) 0.715(6) 0.531(2) 0.255(11) Uiso 0.50 1 d PD I 1 C87' C 0.994(8) 0.628(8) 0.564(2) 0.255(11) Uiso 0.50 1 d PD J 2 C88 C 0.917(8) 0.639(7) 0.543(3) 0.255(11) Uiso 0.50 1 d PD I 1 C88' C 0.922(8) 0.674(5) 0.541(3) 0.255(11) Uiso 0.50 1 d PD J 2 C89 C 0.987(7) 0.589(7) 0.565(3) 0.255(11) Uiso 0.50 1 d PD I 1 C89' C 0.933(5) 0.595(6) 0.5196(19) 0.255(11) Uiso 0.50 1 d PD J 2 C90 C 0.558(4) 1.057(3) 0.5038(12) 0.142(8) Uiso 0.50 1 d PD . 2 C91 C 0.529(4) 0.984(4) 0.5257(12) 0.142(8) Uiso 0.50 1 d PD . 2 C92 C 0.468(4) 0.908(3) 0.5112(12) 0.142(8) Uiso 0.50 1 d PD . 2 C93 C 0.458(3) 0.942(3) 0.4765(12) 0.142(8) Uiso 0.50 1 d PD . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0315(3) 0.0328(3) 0.0391(3) 0.0006(2) 0.0050(2) 0.0023(2) Sm2 0.0335(3) 0.0371(3) 0.0381(3) 0.0012(2) 0.0035(2) 0.0041(2) O1 0.040(4) 0.022(4) 0.047(4) 0.003(3) 0.008(3) -0.002(3) O2 0.031(4) 0.043(5) 0.049(5) 0.001(4) 0.009(3) 0.006(3) O3 0.040(4) 0.038(4) 0.039(4) 0.009(3) 0.010(3) 0.001(3) O4 0.048(4) 0.044(5) 0.041(4) -0.002(4) 0.003(3) -0.007(4) N1 0.032(4) 0.031(5) 0.049(5) 0.002(4) 0.006(4) 0.004(4) N2 0.034(4) 0.025(5) 0.041(5) 0.003(4) 0.002(4) 0.004(4) N3 0.040(5) 0.036(5) 0.045(5) -0.002(4) 0.004(4) 0.006(4) N4 0.049(5) 0.030(5) 0.060(6) -0.004(4) 0.023(5) 0.001(4) N5 0.044(5) 0.030(5) 0.049(6) 0.006(4) 0.006(4) 0.005(4) N6 0.042(5) 0.037(5) 0.040(5) -0.003(4) 0.013(4) 0.010(4) C1 0.052(7) 0.036(6) 0.036(6) -0.015(5) 0.003(5) -0.006(5) C2 0.031(5) 0.047(7) 0.048(7) -0.008(5) 0.009(5) 0.001(5) C3 0.037(6) 0.073(10) 0.047(7) 0.001(6) 0.014(5) -0.011(6) C4 0.044(7) 0.068(9) 0.049(7) 0.004(6) 0.008(6) -0.013(6) C5 0.046(6) 0.041(7) 0.052(7) 0.007(5) 0.000(5) -0.004(5) C6 0.033(5) 0.038(6) 0.032(6) 0.003(5) 0.000(4) -0.003(4) C7 0.038(6) 0.031(6) 0.049(7) -0.001(5) 0.003(5) 0.007(5) C8 0.037(6) 0.025(6) 0.063(8) 0.004(5) 0.004(5) 0.004(4) C9 0.038(6) 0.033(7) 0.076(9) -0.008(6) 0.008(6) -0.012(5) C10 0.040(6) 0.034(6) 0.061(8) 0.000(6) 0.006(5) -0.005(5) C11 0.046(6) 0.039(7) 0.045(7) -0.003(5) -0.004(5) -0.001(5) C12 0.036(6) 0.028(6) 0.051(7) -0.011(5) 0.005(5) -0.005(4) C13 0.047(6) 0.042(7) 0.033(6) 0.001(5) -0.001(5) 0.002(5) C14 0.039(6) 0.026(6) 0.052(7) 0.002(5) 0.004(5) 0.000(4) C15 0.046(6) 0.063(8) 0.032(6) 0.007(5) 0.006(5) 0.026(6) C16 0.042(6) 0.049(7) 0.036(6) -0.003(5) 0.010(5) -0.003(5) C17 0.042(6) 0.034(6) 0.045(7) -0.002(5) 0.006(5) 0.001(5) C18 0.040(6) 0.062(9) 0.056(8) -0.002(6) 0.016(6) -0.012(6) C19 0.026(5) 0.056(8) 0.059(8) -0.012(6) 0.003(5) -0.003(5) C20 0.062(8) 0.056(9) 0.068(9) -0.004(7) 0.023(7) 0.004(6) C21 0.043(6) 0.053(8) 0.054(7) 0.012(6) 0.014(5) 0.012(5) C22 0.040(7) 0.068(10) 0.099(12) 0.008(8) -0.002(7) 0.003(6) C23 0.058(9) 0.087(12) 0.096(11) 0.016(9) 0.028(8) -0.024(8) C24 0.035(6) 0.059(8) 0.041(7) -0.005(6) 0.000(5) -0.010(5) C25 0.038(6) 0.064(9) 0.079(9) 0.011(7) 0.020(6) 0.001(6) C26 0.051(7) 0.042(7) 0.062(8) -0.002(6) 0.018(6) 0.005(5) C27 0.054(8) 0.075(10) 0.051(8) 0.000(7) 0.013(6) -0.008(7) C28 0.041(7) 0.050(8) 0.086(10) -0.008(7) 0.003(6) -0.002(6) C29 0.027(5) 0.041(7) 0.060(7) 0.012(6) 0.005(5) 0.006(5) C30 0.040(6) 0.026(6) 0.058(7) 0.002(5) 0.012(5) -0.005(5) C31 0.042(6) 0.045(8) 0.072(9) 0.006(6) 0.008(6) 0.000(5) C32 0.050(7) 0.034(7) 0.081(9) 0.014(7) 0.008(7) -0.003(5) C33 0.039(6) 0.054(8) 0.068(8) 0.014(7) 0.015(6) 0.008(6) C34 0.043(6) 0.033(6) 0.055(7) 0.009(5) 0.000(5) -0.003(5) C35 0.053(7) 0.052(8) 0.039(7) 0.005(6) 0.005(5) -0.001(6) C36 0.056(7) 0.033(7) 0.070(9) -0.004(6) 0.012(6) -0.009(5) C37 0.071(9) 0.043(8) 0.070(10) -0.010(7) 0.015(7) -0.011(6) C38 0.085(10) 0.054(9) 0.059(9) -0.016(7) 0.011(7) -0.015(7) C39 0.055(8) 0.075(10) 0.048(8) -0.013(7) 0.004(6) -0.026(7) C40 0.041(6) 0.055(8) 0.049(7) -0.004(6) 0.005(5) 0.003(5) C41 0.043(6) 0.046(7) 0.054(7) 0.006(6) 0.002(5) -0.004(5) C42 0.050(7) 0.060(8) 0.035(6) 0.001(6) 0.001(5) 0.000(6) C43 0.047(6) 0.048(7) 0.043(7) -0.011(5) -0.001(5) 0.006(5) C44 0.043(6) 0.038(7) 0.056(7) 0.001(5) 0.009(5) 0.011(5) C45 0.046(7) 0.062(9) 0.035(6) 0.005(6) -0.006(5) 0.001(6) C46 0.045(6) 0.051(8) 0.043(7) 0.000(5) 0.005(5) 0.006(5) C47 0.040(6) 0.043(7) 0.048(7) -0.003(5) -0.001(5) 0.016(5) C48 0.102(11) 0.051(9) 0.067(9) -0.022(7) 0.027(8) -0.026(8) C49 0.043(6) 0.043(7) 0.042(7) 0.000(5) 0.002(5) 0.002(5) C50 0.047(7) 0.055(9) 0.081(10) 0.001(7) 0.010(7) 0.012(6) C51 0.084(11) 0.041(9) 0.135(15) -0.005(9) 0.050(10) -0.006(7) C52 0.076(9) 0.036(8) 0.078(10) 0.013(7) 0.005(8) -0.006(6) C53 0.099(12) 0.048(9) 0.095(12) 0.003(8) -0.014(9) -0.014(8) C54 0.087(10) 0.025(7) 0.129(14) -0.003(8) 0.052(10) -0.013(7) C55 0.085(10) 0.047(9) 0.069(9) -0.005(7) -0.014(8) 0.001(7) C56 0.115(13) 0.060(10) 0.083(11) -0.008(8) 0.017(10) -0.017(9) C57 0.026(5) 0.020(5) 0.051(7) 0.002(4) 0.004(4) -0.002(4) C58 0.038(6) 0.034(6) 0.043(6) 0.006(5) 0.008(5) 0.011(5) C59 0.037(6) 0.037(7) 0.061(8) 0.003(5) 0.004(5) 0.012(5) C60 0.060(8) 0.041(7) 0.059(8) 0.000(6) 0.012(6) 0.007(6) C61 0.043(7) 0.058(9) 0.071(9) -0.003(7) -0.009(6) 0.014(6) C62 0.039(6) 0.054(8) 0.060(8) 0.003(6) -0.002(6) -0.003(5) C63 0.043(6) 0.032(6) 0.053(7) 0.004(5) 0.006(5) 0.006(5) C64 0.050(6) 0.037(6) 0.035(6) -0.002(5) -0.002(5) 0.004(5) C65 0.054(7) 0.055(8) 0.045(7) -0.011(6) -0.006(6) 0.005(6) C66 0.075(10) 0.067(10) 0.064(9) -0.027(7) 0.008(7) 0.008(7) C67 0.056(8) 0.098(12) 0.068(9) -0.032(9) 0.013(7) 0.026(8) C68 0.048(7) 0.077(11) 0.078(10) 0.001(8) 0.026(7) 0.015(7) C69 0.046(6) 0.055(8) 0.044(7) -0.002(6) 0.008(5) 0.014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O2 2.259(7) . ? Sm1 N5 2.350(9) . ? Sm1 O3 2.415(7) . ? Sm1 O1 2.480(7) . ? Sm1 C57 2.489(10) . ? Sm1 N1 2.571(9) . ? Sm1 N2 2.679(8) . ? Sm1 Sm2 3.4237(8) . ? Sm2 O4 2.224(7) . ? Sm2 N6 2.351(8) . ? Sm2 O1 2.381(7) . ? Sm2 O3 2.451(7) . ? Sm2 C57 2.475(9) . ? Sm2 N3 2.579(9) . ? Sm2 N4 2.686(10) . ? O1 C1 1.359(13) . ? O2 C7 1.336(12) . ? O3 C29 1.378(13) . ? O4 C35 1.332(14) . ? N1 C16 1.474(13) . ? N1 C14 1.486(12) . ? N1 C13 1.495(13) . ? N2 C18 1.451(14) . ? N2 C15 1.468(13) . ? N2 C17 1.473(13) . ? N3 C44 1.488(13) . ? N3 C42 1.498(14) . ? N3 C41 1.503(14) . ? N4 C43 1.452(14) . ? N4 C46 1.470(14) . ? N4 C45 1.487(14) . ? N5 C57 1.328(13) . ? N5 C58 1.474(12) . ? N6 C57 1.342(13) . ? N6 C64 1.478(13) . ? C1 C6 1.426(15) . ? C1 C2 1.438(14) . ? C2 C3 1.379(15) . ? C2 C19 1.560(16) . ? C3 C4 1.376(17) . ? C3 H3 0.9500 . ? C4 C5 1.397(16) . ? C4 C23 1.550(16) . ? C5 C6 1.364(15) . ? C5 H5 0.9500 . ? C6 C13 1.506(14) . ? C7 C12 1.422(15) . ? C7 C8 1.442(15) . ? C8 C9 1.397(15) . ? C8 C24 1.515(16) . ? C9 C10 1.413(17) . ? C9 H9 0.9500 . ? C10 C11 1.358(15) . ? C10 C28 1.521(15) . ? C11 C12 1.403(14) . ? C11 H11 0.9500 . ? C12 C18 1.507(14) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.589(16) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.511(15) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C21 1.536(16) . ? C19 C20 1.539(16) . ? C19 C22 1.556(16) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.524(15) . ? C24 C27 1.540(16) . ? C24 C26 1.552(16) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.417(16) . ? C29 C34 1.444(16) . ? C30 C31 1.369(15) . ? C30 C47 1.529(15) . ? C31 C32 1.365(17) . ? C31 H31 0.9500 . ? C32 C33 1.378(18) . ? C32 C51 1.526(17) . ? C33 C34 1.387(16) . ? C33 H33 0.9500 . ? C34 C41 1.475(16) . ? C35 C40 1.417(16) . ? C35 C36 1.460(17) . ? C36 C37 1.405(17) . ? C36 C52 1.517(18) . ? C37 C38 1.374(19) . ? C37 H37 0.9500 . ? C38 C39 1.400(19) . ? C38 C56 1.529(19) . ? C39 C40 1.378(16) . ? C39 H39 0.9500 . ? C40 C46 1.508(17) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.524(15) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.547(15) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C50 1.533(15) . ? C47 C49 1.544(16) . ? C47 C48 1.560(16) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C54 1.493(19) . ? C52 C53 1.550(18) . ? C52 C55 1.563(18) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C58 C63 1.538(15) . ? C58 C59 1.549(15) . ? C58 H58 1.0000 . ? C59 C60 1.524(15) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.548(16) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.555(17) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.514(15) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.548(15) . ? C64 C69 1.555(16) . ? C64 H64 1.0000 . ? C65 C66 1.530(16) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.50(2) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.496(19) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.564(16) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? O5 C70 1.46(2) . ? O5 C73 1.46(2) . ? O5' C73' 1.46(2) . ? O5' C70' 1.46(2) . ? O6 C74 1.45(2) . ? O6 C77 1.46(2) . ? O6' C77' 1.46(2) . ? O6' C74' 1.47(2) . ? O7 C81 1.44(2) . ? O7 C78 1.46(2) . ? O7' C81' 1.46(2) . ? O7' C78' 1.51(2) . ? O8 C82 1.453(19) . ? O8 C85 1.499(19) . ? O8' C85' 1.447(19) . ? O8' C82' 1.467(19) . ? O9 C89 1.46(2) . ? O9 C86 1.47(2) . ? O9' C89' 1.46(2) . ? O9' C86' 1.46(2) . ? O10 C91 0.80(6) 3_676 ? O10 C92 1.34(6) 3_676 ? O10 C93 1.467(19) . ? O10 C90 1.472(19) . ? C70 C71 1.51(2) . ? C70' C71' 1.49(2) . ? C71 C72 1.50(2) . ? C71' C72' 1.50(2) . ? C72 C73 1.51(2) . ? C72' C73' 1.51(2) . ? C74 C75 1.52(2) . ? C74' C75' 1.52(2) . ? C75 C76 1.50(2) . ? C75' C76' 1.50(2) . ? C76 C77 1.50(2) . ? C76' C77' 1.50(2) . ? C78 C79 1.51(2) . ? C78' C79' 1.52(2) . ? C79 C80 1.49(2) . ? C79' C80' 1.52(2) . ? C80 C81 1.52(2) . ? C80' C81' 1.50(2) . ? C82 C83 1.50(2) . ? C82' C83' 1.52(2) . ? C83 C84 1.51(2) . ? C83' C84' 1.50(2) . ? C84 C85 1.52(2) . ? C84' C85' 1.52(2) . ? C86 C87 1.50(2) . ? C86' C87' 1.51(2) . ? C87 C88 1.50(2) . ? C87' C88' 1.50(2) . ? C88 C89 1.50(2) . ? C88' C89' 1.50(2) . ? C90 C92 0.86(6) 3_676 ? C90 C93 0.87(6) 3_676 ? C90 C91 1.50(2) . ? C90 C91 1.77(7) 3_676 ? C91 O10 0.80(6) 3_676 ? C91 C93 1.12(7) 3_676 ? C91 C92 1.52(2) . ? C91 C90 1.77(7) 3_676 ? C92 C90 0.86(6) 3_676 ? C92 O10 1.34(6) 3_676 ? C92 C93 1.50(2) . ? C93 C90 0.87(6) 3_676 ? C93 C91 1.12(7) 3_676 ? 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 O2 Sm1 N5 98.4(3) . . ? O2 Sm1 O3 86.0(2) . . ? N5 Sm1 O3 108.1(3) . . ? O2 Sm1 O1 148.9(2) . . ? N5 Sm1 O1 104.2(3) . . ? O3 Sm1 O1 67.0(2) . . ? O2 Sm1 C57 111.1(3) . . ? N5 Sm1 C57 31.7(3) . . ? O3 Sm1 C57 79.9(3) . . ? O1 Sm1 C57 80.1(3) . . ? O2 Sm1 N1 128.9(3) . . ? N5 Sm1 N1 90.5(3) . . ? O3 Sm1 N1 138.3(2) . . ? O1 Sm1 N1 72.4(2) . . ? C57 Sm1 N1 102.5(3) . . ? O2 Sm1 N2 73.4(3) . . ? N5 Sm1 N2 107.6(3) . . ? O3 Sm1 N2 140.8(2) . . ? O1 Sm1 N2 118.2(2) . . ? C57 Sm1 N2 138.3(3) . . ? N1 Sm1 N2 56.1(3) . . ? O2 Sm1 Sm2 124.00(18) . . ? N5 Sm1 Sm2 77.7(2) . . ? O3 Sm1 Sm2 45.72(18) . . ? O1 Sm1 Sm2 44.05(16) . . ? C57 Sm1 Sm2 46.2(2) . . ? N1 Sm1 Sm2 107.10(19) . . ? N2 Sm1 Sm2 161.62(18) . . ? O4 Sm2 N6 98.6(3) . . ? O4 Sm2 O1 86.1(2) . . ? N6 Sm2 O1 111.9(3) . . ? O4 Sm2 O3 151.4(2) . . ? N6 Sm2 O3 102.2(3) . . ? O1 Sm2 O3 68.0(2) . . ? O4 Sm2 C57 109.9(3) . . ? N6 Sm2 C57 32.2(3) . . ? O1 Sm2 C57 82.4(3) . . ? O3 Sm2 C57 79.5(3) . . ? O4 Sm2 N3 128.1(3) . . ? N6 Sm2 N3 87.3(3) . . ? O1 Sm2 N3 139.0(3) . . ? O3 Sm2 N3 72.7(3) . . ? C57 Sm2 N3 102.0(3) . . ? O4 Sm2 N4 72.5(3) . . ? N6 Sm2 N4 108.3(3) . . ? O1 Sm2 N4 136.7(2) . . ? O3 Sm2 N4 118.3(2) . . ? C57 Sm2 N4 139.9(3) . . ? N3 Sm2 N4 57.1(3) . . ? O4 Sm2 Sm1 122.84(19) . . ? N6 Sm2 Sm1 78.3(2) . . ? O1 Sm2 Sm1 46.42(16) . . ? O3 Sm2 Sm1 44.85(16) . . ? C57 Sm2 Sm1 46.6(2) . . ? N3 Sm2 Sm1 108.9(2) . . ? N4 Sm2 Sm1 163.04(19) . . ? C1 O1 Sm2 128.7(6) . . ? C1 O1 Sm1 136.7(6) . . ? Sm2 O1 Sm1 89.5(2) . . ? C7 O2 Sm1 129.1(7) . . ? C29 O3 Sm1 125.2(6) . . ? C29 O3 Sm2 139.1(7) . . ? Sm1 O3 Sm2 89.4(2) . . ? C35 O4 Sm2 134.8(7) . . ? C16 N1 C14 107.4(8) . . ? C16 N1 C13 113.7(8) . . ? C14 N1 C13 108.4(8) . . ? C16 N1 Sm1 111.0(6) . . ? C14 N1 Sm1 105.1(6) . . ? C13 N1 Sm1 110.8(6) . . ? C18 N2 C15 107.4(9) . . ? C18 N2 C17 111.8(8) . . ? C15 N2 C17 107.4(8) . . ? C18 N2 Sm1 116.8(7) . . ? C15 N2 Sm1 105.4(6) . . ? C17 N2 Sm1 107.4(6) . . ? C44 N3 C42 109.1(8) . . ? C44 N3 C41 112.5(9) . . ? C42 N3 C41 111.1(9) . . ? C44 N3 Sm2 106.9(6) . . ? C42 N3 Sm2 105.6(7) . . ? C41 N3 Sm2 111.3(6) . . ? C43 N4 C46 112.9(9) . . ? C43 N4 C45 107.4(9) . . ? C46 N4 C45 111.2(9) . . ? C43 N4 Sm2 101.7(7) . . ? C46 N4 Sm2 115.7(7) . . ? C45 N4 Sm2 107.3(6) . . ? C57 N5 C58 126.4(9) . . ? C57 N5 Sm1 80.0(6) . . ? C58 N5 Sm1 152.4(7) . . ? C57 N6 C64 124.0(8) . . ? C57 N6 Sm2 79.0(5) . . ? C64 N6 Sm2 155.4(7) . . ? O1 C1 C6 119.0(9) . . ? O1 C1 C2 124.7(10) . . ? C6 C1 C2 116.1(10) . . ? C3 C2 C1 119.0(11) . . ? C3 C2 C19 115.6(10) . . ? C1 C2 C19 125.2(10) . . ? C4 C3 C2 124.1(11) . . ? C4 C3 H3 117.9 . . ? C2 C3 H3 117.9 . . ? C3 C4 C5 117.1(11) . . ? C3 C4 C23 122.1(11) . . ? C5 C4 C23 120.8(12) . . ? C6 C5 C4 121.5(11) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C1 122.1(10) . . ? C5 C6 C13 119.3(10) . . ? C1 C6 C13 118.5(9) . . ? O2 C7 C12 119.2(10) . . ? O2 C7 C8 122.7(10) . . ? C12 C7 C8 118.0(9) . . ? C9 C8 C7 116.7(11) . . ? C9 C8 C24 121.7(10) . . ? C7 C8 C24 121.7(9) . . ? C8 C9 C10 124.7(11) . . ? C8 C9 H9 117.6 . . ? C10 C9 H9 117.6 . . ? C11 C10 C9 116.8(11) . . ? C11 C10 C28 123.4(11) . . ? C9 C10 C28 119.8(11) . . ? C10 C11 C12 122.0(11) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C7 120.7(10) . . ? C11 C12 C18 119.5(11) . . ? C7 C12 C18 119.8(10) . . ? N1 C13 C6 113.4(9) . . ? N1 C13 H13A 108.9 . . ? C6 C13 H13A 108.9 . . ? N1 C13 H13B 108.9 . . ? C6 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? N1 C14 C15 108.0(8) . . ? N1 C14 H14A 110.1 . . ? C15 C14 H14A 110.1 . . ? N1 C14 H14B 110.1 . . ? C15 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? N2 C15 C14 106.7(8) . . ? N2 C15 H15A 110.4 . . ? C14 C15 H15A 110.4 . . ? N2 C15 H15B 110.4 . . ? C14 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? N1 C16 C17 108.8(8) . . ? N1 C16 H16A 109.9 . . ? C17 C16 H16A 109.9 . . ? N1 C16 H16B 109.9 . . ? C17 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? N2 C17 C16 109.2(9) . . ? N2 C17 H17A 109.8 . . ? C16 C17 H17A 109.8 . . ? N2 C17 H17B 109.8 . . ? C16 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? N2 C18 C12 114.2(10) . . ? N2 C18 H18A 108.7 . . ? C12 C18 H18A 108.7 . . ? N2 C18 H18B 108.7 . . ? C12 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C21 C19 C20 108.8(10) . . ? C21 C19 C22 105.1(10) . . ? C20 C19 C22 107.8(10) . . ? C21 C19 C2 116.7(9) . . ? C20 C19 C2 107.9(10) . . ? C22 C19 C2 110.3(10) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C4 C23 H23A 109.5 . . ? C4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 C24 C25 112.6(9) . . ? C8 C24 C27 111.7(10) . . ? C25 C24 C27 108.1(10) . . ? C8 C24 C26 108.6(9) . . ? C25 C24 C26 107.2(10) . . ? C27 C24 C26 108.3(10) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C10 C28 H28A 109.5 . . ? C10 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C10 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C30 123.8(10) . . ? O3 C29 C34 117.3(10) . . ? C30 C29 C34 118.6(10) . . ? C31 C30 C29 115.8(11) . . ? C31 C30 C47 119.2(11) . . ? C29 C30 C47 124.8(10) . . ? C32 C31 C30 127.6(13) . . ? C32 C31 H31 116.2 . . ? C30 C31 H31 116.2 . . ? C31 C32 C33 116.2(12) . . ? C31 C32 C51 122.7(13) . . ? C33 C32 C51 121.1(12) . . ? C32 C33 C34 121.7(12) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C33 C34 C29 119.7(11) . . ? C33 C34 C41 118.7(11) . . ? C29 C34 C41 121.6(10) . . ? O4 C35 C40 119.4(11) . . ? O4 C35 C36 121.4(10) . . ? C40 C35 C36 119.2(11) . . ? C37 C36 C35 115.5(12) . . ? C37 C36 C52 122.8(12) . . ? C35 C36 C52 121.4(11) . . ? C38 C37 C36 125.4(13) . . ? C38 C37 H37 117.3 . . ? C36 C37 H37 117.3 . . ? C37 C38 C39 117.4(12) . . ? C37 C38 C56 121.4(14) . . ? C39 C38 C56 121.1(14) . . ? C40 C39 C38 121.7(13) . . ? C40 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? C39 C40 C35 120.6(13) . . ? C39 C40 C46 120.7(12) . . ? C35 C40 C46 118.6(11) . . ? C34 C41 N3 115.3(9) . . ? C34 C41 H41A 108.4 . . ? N3 C41 H41A 108.4 . . ? C34 C41 H41B 108.4 . . ? N3 C41 H41B 108.4 . . ? H41A C41 H41B 107.5 . . ? N3 C42 C43 108.7(9) . . ? N3 C42 H42A 109.9 . . ? C43 C42 H42A 109.9 . . ? N3 C42 H42B 109.9 . . ? C43 C42 H42B 109.9 . . ? H42A C42 H42B 108.3 . . ? N4 C43 C42 110.5(9) . . ? N4 C43 H43A 109.6 . . ? C42 C43 H43A 109.6 . . ? N4 C43 H43B 109.6 . . ? C42 C43 H43B 109.6 . . ? H43A C43 H43B 108.1 . . ? N3 C44 C45 107.8(9) . . ? N3 C44 H44A 110.1 . . ? C45 C44 H44A 110.1 . . ? N3 C44 H44B 110.1 . . ? C45 C44 H44B 110.1 . . ? H44A C44 H44B 108.5 . . ? N4 C45 C44 109.9(9) . . ? N4 C45 H45A 109.7 . . ? C44 C45 H45A 109.7 . . ? N4 C45 H45B 109.7 . . ? C44 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? N4 C46 C40 114.2(9) . . ? N4 C46 H46A 108.7 . . ? C40 C46 H46A 108.7 . . ? N4 C46 H46B 108.7 . . ? C40 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? C30 C47 C50 106.3(9) . . ? C30 C47 C49 117.2(9) . . ? C50 C47 C49 109.6(10) . . ? C30 C47 C48 110.8(10) . . ? C50 C47 C48 109.2(10) . . ? C49 C47 C48 103.7(10) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C32 C51 H51A 109.5 . . ? C32 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C32 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C54 C52 C36 106.4(12) . . ? C54 C52 C53 108.5(12) . . ? C36 C52 C53 112.7(12) . . ? C54 C52 C55 113.0(13) . . ? C36 C52 C55 108.8(11) . . ? C53 C52 C55 107.5(12) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C38 C56 H56A 109.5 . . ? C38 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C38 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N5 C57 N6 136.6(9) . . ? N5 C57 Sm2 154.3(8) . . ? N6 C57 Sm2 68.8(5) . . ? N5 C57 Sm1 68.4(6) . . ? N6 C57 Sm1 153.9(7) . . ? Sm2 C57 Sm1 87.2(3) . . ? N5 C58 C63 111.6(9) . . ? N5 C58 C59 112.0(8) . . ? C63 C58 C59 107.9(9) . . ? N5 C58 H58 108.4 . . ? C63 C58 H58 108.4 . . ? C59 C58 H58 108.4 . . ? C60 C59 C58 110.1(9) . . ? C60 C59 H59A 109.6 . . ? C58 C59 H59A 109.6 . . ? C60 C59 H59B 109.6 . . ? C58 C59 H59B 109.6 . . ? H59A C59 H59B 108.2 . . ? C59 C60 C61 111.1(10) . . ? C59 C60 H60A 109.4 . . ? C61 C60 H60A 109.4 . . ? C59 C60 H60B 109.4 . . ? C61 C60 H60B 109.4 . . ? H60A C60 H60B 108.0 . . ? C60 C61 C62 110.4(10) . . ? C60 C61 H61A 109.6 . . ? C62 C61 H61A 109.6 . . ? C60 C61 H61B 109.6 . . ? C62 C61 H61B 109.6 . . ? H61A C61 H61B 108.1 . . ? C63 C62 C61 108.8(10) . . ? C63 C62 H62A 109.9 . . ? C61 C62 H62A 109.9 . . ? C63 C62 H62B 109.9 . . ? C61 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? C62 C63 C58 111.0(9) . . ? C62 C63 H63A 109.4 . . ? C58 C63 H63A 109.4 . . ? C62 C63 H63B 109.4 . . ? C58 C63 H63B 109.4 . . ? H63A C63 H63B 108.0 . . ? N6 C64 C65 110.7(9) . . ? N6 C64 C69 111.6(9) . . ? C65 C64 C69 109.2(9) . . ? N6 C64 H64 108.5 . . ? C65 C64 H64 108.5 . . ? C69 C64 H64 108.5 . . ? C66 C65 C64 109.0(10) . . ? C66 C65 H65A 109.9 . . ? C64 C65 H65A 109.9 . . ? C66 C65 H65B 109.9 . . ? C64 C65 H65B 109.9 . . ? H65A C65 H65B 108.3 . . ? C67 C66 C65 112.2(12) . . ? C67 C66 H66A 109.2 . . ? C65 C66 H66A 109.2 . . ? C67 C66 H66B 109.2 . . ? C65 C66 H66B 109.2 . . ? H66A C66 H66B 107.9 . . ? C68 C67 C66 112.2(11) . . ? C68 C67 H67A 109.2 . . ? C66 C67 H67A 109.2 . . ? C68 C67 H67B 109.2 . . ? C66 C67 H67B 109.2 . . ? H67A C67 H67B 107.9 . . ? C67 C68 C69 112.7(10) . . ? C67 C68 H68A 109.1 . . ? C69 C68 H68A 109.1 . . ? C67 C68 H68B 109.1 . . ? C69 C68 H68B 109.1 . . ? H68A C68 H68B 107.8 . . ? C64 C69 C68 106.9(10) . . ? C64 C69 H69A 110.3 . . ? C68 C69 H69A 110.3 . . ? C64 C69 H69B 110.3 . . ? C68 C69 H69B 110.3 . . ? H69A C69 H69B 108.6 . . ? C70 O5 C73 101(5) . . ? C73' O5' C70' 112(6) . . ? C74 O6 C77 110(4) . . ? C77' O6' C74' 99(4) . . ? C81 O7 C78 108(5) . . ? C81' O7' C78' 103(3) . . ? C82 O8 C85 111(3) . . ? C85' O8' C82' 110(3) . . ? C89 O9 C86 96(7) . . ? C89' O9' C86' 104(7) . . ? C91 O10 C92 87(5) 3_676 3_676 ? C91 O10 C93 49(5) 3_676 . ? C92 O10 C93 127(4) 3_676 . ? C91 O10 C90 98(6) 3_676 . ? C92 O10 C90 35(3) 3_676 . ? C93 O10 C90 113(3) . . ? O5 C70 C71 113(5) . . ? O5' C70' C71' 86(2) . . ? C72 C71 C70 107(6) . . ? C70' C71' C72' 112(5) . . ? C71 C72 C73 101(6) . . ? C71' C72' C73' 103(5) . . ? O5 C73 C72 116(6) . . ? O5' C73' C72' 95(5) . . ? O6 C74 C75 95(4) . . ? O6' C74' C75' 113(4) . . ? C76 C75 C74 116(5) . . ? C76' C75' C74' 92(5) . . ? C75 C76 C77 98(5) . . ? C75' C76' C77' 103(5) . . ? O6 C77 C76 102(4) . . ? O6' C77' C76' 107(5) . . ? O7 C78 C79 109(4) . . ? O7' C78' C79' 98(2) . . ? C80 C79 C78 105(3) . . ? C78' C79' C80' 100(2) . . ? C79 C80 C81 107(4) . . ? C81' C80' C79' 109(3) . . ? O7 C81 C80 107(5) . . ? O7' C81' C80' 101(4) . . ? O8 C82 C83 104(3) . . ? O8' C82' C83' 101(3) . . ? C82 C83 C84 108(3) . . ? C84' C83' C82' 105(4) . . ? C83 C84 C85 102(3) . . ? C83' C84' C85' 97(3) . . ? O8 C85 C84 104(3) . . ? O8' C85' C84' 103(3) . . ? O9 C86 C87 111(8) . . ? O9' C86' C87' 97(7) . . ? C86 C87 C88 100(8) . . ? C88' C87' C86' 105(9) . . ? C89 C88 C87 102(9) . . ? C89' C88' C87' 84(2) . . ? O9 C89 C88 103(9) . . ? O9' C89' C88' 99(7) . . ? C92 C90 C93 121(9) 3_676 3_676 ? C92 C90 O10 64(4) 3_676 . ? C93 C90 O10 136(6) 3_676 . ? C92 C90 C91 136(7) 3_676 . ? C93 C90 C91 47(4) 3_676 . ? O10 C90 C91 96(3) . . ? C92 C90 C91 59(4) 3_676 3_676 ? C93 C90 C91 113(7) 3_676 3_676 ? O10 C90 C91 26(2) . 3_676 ? C91 C90 C91 85(4) . 3_676 ? O10 C91 C93 99(7) 3_676 3_676 ? O10 C91 C90 112(7) 3_676 . ? C93 C91 C90 35(3) 3_676 . ? O10 C91 C92 61(4) 3_676 . ? C93 C91 C92 143(5) 3_676 . ? C90 C91 C92 120(4) . . ? O10 C91 C90 55(4) 3_676 3_676 ? C93 C91 C90 114(5) 3_676 3_676 ? C90 C91 C90 95(4) . 3_676 ? C92 C91 C90 29(2) . 3_676 ? C90 C92 O10 81(5) 3_676 3_676 ? C90 C92 C93 30(5) 3_676 . ? O10 C92 C93 100(4) 3_676 . ? C90 C92 C91 92(5) 3_676 . ? O10 C92 C91 31(3) 3_676 . ? C93 C92 C91 96(4) . . ? C90 C93 C91 98(6) 3_676 3_676 ? C90 C93 O10 110(5) 3_676 . ? C91 C93 O10 32(3) 3_676 . ? C90 C93 C92 30(5) 3_676 . ? C91 C93 C92 114(4) 3_676 . ? O10 C93 C92 111(3) . . ? 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 O2 Sm1 Sm2 O4 174.5(3) . . . . ? N5 Sm1 Sm2 O4 82.6(3) . . . . ? O3 Sm1 Sm2 O4 -146.4(3) . . . . ? O1 Sm1 Sm2 O4 -43.4(3) . . . . ? C57 Sm1 Sm2 O4 87.0(4) . . . . ? N1 Sm1 Sm2 O4 -4.0(3) . . . . ? N2 Sm1 Sm2 O4 -26.4(6) . . . . ? O2 Sm1 Sm2 N6 81.7(3) . . . . ? N5 Sm1 Sm2 N6 -10.2(3) . . . . ? O3 Sm1 Sm2 N6 120.9(3) . . . . ? O1 Sm1 Sm2 N6 -136.2(3) . . . . ? C57 Sm1 Sm2 N6 -5.7(4) . . . . ? N1 Sm1 Sm2 N6 -96.8(3) . . . . ? N2 Sm1 Sm2 N6 -119.2(6) . . . . ? O2 Sm1 Sm2 O1 -142.1(3) . . . . ? N5 Sm1 Sm2 O1 126.0(3) . . . . ? O3 Sm1 Sm2 O1 -103.0(3) . . . . ? C57 Sm1 Sm2 O1 130.4(4) . . . . ? N1 Sm1 Sm2 O1 39.4(3) . . . . ? N2 Sm1 Sm2 O1 17.0(6) . . . . ? O2 Sm1 Sm2 O3 -39.1(3) . . . . ? N5 Sm1 Sm2 O3 -131.0(3) . . . . ? O1 Sm1 Sm2 O3 103.0(3) . . . . ? C57 Sm1 Sm2 O3 -126.6(4) . . . . ? N1 Sm1 Sm2 O3 142.4(3) . . . . ? N2 Sm1 Sm2 O3 119.9(6) . . . . ? O2 Sm1 Sm2 C57 87.5(4) . . . . ? N5 Sm1 Sm2 C57 -4.4(4) . . . . ? O3 Sm1 Sm2 C57 126.6(4) . . . . ? O1 Sm1 Sm2 C57 -130.4(4) . . . . ? N1 Sm1 Sm2 C57 -91.0(4) . . . . ? N2 Sm1 Sm2 C57 -113.4(6) . . . . ? O2 Sm1 Sm2 N3 -1.3(3) . . . . ? N5 Sm1 Sm2 N3 -93.2(3) . . . . ? O3 Sm1 Sm2 N3 37.9(3) . . . . ? O1 Sm1 Sm2 N3 140.8(3) . . . . ? C57 Sm1 Sm2 N3 -88.7(4) . . . . ? N1 Sm1 Sm2 N3 -179.8(3) . . . . ? N2 Sm1 Sm2 N3 157.8(6) . . . . ? O2 Sm1 Sm2 N4 -33.1(7) . . . . ? N5 Sm1 Sm2 N4 -125.0(7) . . . . ? O3 Sm1 Sm2 N4 6.0(7) . . . . ? O1 Sm1 Sm2 N4 109.0(7) . . . . ? C57 Sm1 Sm2 N4 -120.6(7) . . . . ? N1 Sm1 Sm2 N4 148.4(7) . . . . ? N2 Sm1 Sm2 N4 126.0(8) . . . . ? O4 Sm2 O1 C1 -13.1(8) . . . . ? N6 Sm2 O1 C1 -110.7(8) . . . . ? O3 Sm2 O1 C1 154.5(8) . . . . ? C57 Sm2 O1 C1 -123.8(8) . . . . ? N3 Sm2 O1 C1 136.7(8) . . . . ? N4 Sm2 O1 C1 46.0(9) . . . . ? Sm1 Sm2 O1 C1 -157.7(9) . . . . ? O4 Sm2 O1 Sm1 144.6(3) . . . . ? N6 Sm2 O1 Sm1 47.0(3) . . . . ? O3 Sm2 O1 Sm1 -47.8(2) . . . . ? C57 Sm2 O1 Sm1 33.9(3) . . . . ? N3 Sm2 O1 Sm1 -65.6(4) . . . . ? N4 Sm2 O1 Sm1 -156.3(3) . . . . ? O2 Sm1 O1 C1 -124.7(9) . . . . ? N5 Sm1 O1 C1 99.8(9) . . . . ? O3 Sm1 O1 C1 -156.3(9) . . . . ? C57 Sm1 O1 C1 120.5(9) . . . . ? N1 Sm1 O1 C1 13.9(9) . . . . ? N2 Sm1 O1 C1 -19.6(10) . . . . ? Sm2 Sm1 O1 C1 154.4(10) . . . . ? O2 Sm1 O1 Sm2 80.9(5) . . . . ? N5 Sm1 O1 Sm2 -54.6(3) . . . . ? O3 Sm1 O1 Sm2 49.3(2) . . . . ? C57 Sm1 O1 Sm2 -33.9(3) . . . . ? N1 Sm1 O1 Sm2 -140.5(3) . . . . ? N2 Sm1 O1 Sm2 -174.0(2) . . . . ? N5 Sm1 O2 C7 -55.7(9) . . . . ? O3 Sm1 O2 C7 -163.4(8) . . . . ? O1 Sm1 O2 C7 167.6(7) . . . . ? C57 Sm1 O2 C7 -85.8(9) . . . . ? N1 Sm1 O2 C7 41.7(9) . . . . ? N2 Sm1 O2 C7 50.3(8) . . . . ? Sm2 Sm1 O2 C7 -136.5(8) . . . . ? O2 Sm1 O3 C29 -8.3(8) . . . . ? N5 Sm1 O3 C29 -105.9(8) . . . . ? O1 Sm1 O3 C29 155.9(8) . . . . ? C57 Sm1 O3 C29 -120.7(8) . . . . ? N1 Sm1 O3 C29 141.8(7) . . . . ? N2 Sm1 O3 C29 48.9(9) . . . . ? Sm2 Sm1 O3 C29 -156.7(8) . . . . ? O2 Sm1 O3 Sm2 148.4(2) . . . . ? N5 Sm1 O3 Sm2 50.8(3) . . . . ? O1 Sm1 O3 Sm2 -47.4(2) . . . . ? C57 Sm1 O3 Sm2 36.1(2) . . . . ? N1 Sm1 O3 Sm2 -61.4(4) . . . . ? N2 Sm1 O3 Sm2 -154.4(3) . . . . ? O4 Sm2 O3 C29 -133.3(9) . . . . ? N6 Sm2 O3 C29 91.1(9) . . . . ? O1 Sm2 O3 C29 -160.0(9) . . . . ? C57 Sm2 O3 C29 114.1(9) . . . . ? N3 Sm2 O3 C29 7.9(9) . . . . ? N4 Sm2 O3 C29 -27.6(10) . . . . ? Sm1 Sm2 O3 C29 150.5(10) . . . . ? O4 Sm2 O3 Sm1 76.3(5) . . . . ? N6 Sm2 O3 Sm1 -59.3(3) . . . . ? O1 Sm2 O3 Sm1 49.6(2) . . . . ? C57 Sm2 O3 Sm1 -36.4(3) . . . . ? N3 Sm2 O3 Sm1 -142.5(3) . . . . ? N4 Sm2 O3 Sm1 -178.0(2) . . . . ? N6 Sm2 O4 C35 -61.5(10) . . . . ? O1 Sm2 O4 C35 -173.1(10) . . . . ? O3 Sm2 O4 C35 162.2(9) . . . . ? C57 Sm2 O4 C35 -92.7(10) . . . . ? N3 Sm2 O4 C35 31.7(11) . . . . ? N4 Sm2 O4 C35 45.0(10) . . . . ? Sm1 Sm2 O4 C35 -143.2(9) . . . . ? O2 Sm1 N1 C16 65.1(7) . . . . ? N5 Sm1 N1 C16 166.3(7) . . . . ? O3 Sm1 N1 C16 -75.3(7) . . . . ? O1 Sm1 N1 C16 -88.9(6) . . . . ? C57 Sm1 N1 C16 -164.2(6) . . . . ? N2 Sm1 N1 C16 55.2(6) . . . . ? Sm2 Sm1 N1 C16 -116.5(6) . . . . ? O2 Sm1 N1 C14 -50.7(7) . . . . ? N5 Sm1 N1 C14 50.5(6) . . . . ? O3 Sm1 N1 C14 168.8(5) . . . . ? O1 Sm1 N1 C14 155.3(7) . . . . ? C57 Sm1 N1 C14 80.0(6) . . . . ? N2 Sm1 N1 C14 -60.6(6) . . . . ? Sm2 Sm1 N1 C14 127.7(6) . . . . ? O2 Sm1 N1 C13 -167.7(6) . . . . ? N5 Sm1 N1 C13 -66.5(6) . . . . ? O3 Sm1 N1 C13 51.9(8) . . . . ? O1 Sm1 N1 C13 38.3(6) . . . . ? C57 Sm1 N1 C13 -36.9(7) . . . . ? N2 Sm1 N1 C13 -177.6(7) . . . . ? Sm2 Sm1 N1 C13 10.8(6) . . . . ? O2 Sm1 N2 C18 7.0(7) . . . . ? N5 Sm1 N2 C18 100.7(7) . . . . ? O3 Sm1 N2 C18 -54.1(9) . . . . ? O1 Sm1 N2 C18 -141.7(7) . . . . ? C57 Sm1 N2 C18 110.3(8) . . . . ? N1 Sm1 N2 C18 179.0(8) . . . . ? Sm2 Sm1 N2 C18 -155.0(6) . . . . ? O2 Sm1 N2 C15 -112.2(7) . . . . ? N5 Sm1 N2 C15 -18.5(7) . . . . ? O3 Sm1 N2 C15 -173.3(6) . . . . ? O1 Sm1 N2 C15 99.1(7) . . . . ? C57 Sm1 N2 C15 -8.9(8) . . . . ? N1 Sm1 N2 C15 59.8(6) . . . . ? Sm2 Sm1 N2 C15 85.8(8) . . . . ? O2 Sm1 N2 C17 133.5(7) . . . . ? N5 Sm1 N2 C17 -132.8(6) . . . . ? O3 Sm1 N2 C17 72.4(7) . . . . ? O1 Sm1 N2 C17 -15.2(7) . . . . ? C57 Sm1 N2 C17 -123.2(6) . . . . ? N1 Sm1 N2 C17 -54.5(6) . . . . ? Sm2 Sm1 N2 C17 -28.5(10) . . . . ? O4 Sm2 N3 C44 73.7(7) . . . . ? N6 Sm2 N3 C44 172.5(7) . . . . ? O1 Sm2 N3 C44 -66.6(8) . . . . ? O3 Sm2 N3 C44 -83.8(7) . . . . ? C57 Sm2 N3 C44 -158.7(7) . . . . ? N4 Sm2 N3 C44 58.6(6) . . . . ? Sm1 Sm2 N3 C44 -110.8(6) . . . . ? O4 Sm2 N3 C42 -42.3(7) . . . . ? N6 Sm2 N3 C42 56.4(6) . . . . ? O1 Sm2 N3 C42 177.3(6) . . . . ? O3 Sm2 N3 C42 160.1(7) . . . . ? C57 Sm2 N3 C42 85.2(7) . . . . ? N4 Sm2 N3 C42 -57.4(6) . . . . ? Sm1 Sm2 N3 C42 133.1(6) . . . . ? O4 Sm2 N3 C41 -163.1(6) . . . . ? N6 Sm2 N3 C41 -64.3(7) . . . . ? O1 Sm2 N3 C41 56.6(8) . . . . ? O3 Sm2 N3 C41 39.4(7) . . . . ? C57 Sm2 N3 C41 -35.5(7) . . . . ? N4 Sm2 N3 C41 -178.2(8) . . . . ? Sm1 Sm2 N3 C41 12.4(7) . . . . ? O4 Sm2 N4 C43 -108.5(7) . . . . ? N6 Sm2 N4 C43 -15.0(7) . . . . ? O1 Sm2 N4 C43 -172.3(6) . . . . ? O3 Sm2 N4 C43 100.4(7) . . . . ? C57 Sm2 N4 C43 -8.1(9) . . . . ? N3 Sm2 N4 C43 59.1(6) . . . . ? Sm1 Sm2 N4 C43 95.6(8) . . . . ? O4 Sm2 N4 C46 14.2(7) . . . . ? N6 Sm2 N4 C46 107.7(7) . . . . ? O1 Sm2 N4 C46 -49.7(8) . . . . ? O3 Sm2 N4 C46 -136.9(7) . . . . ? C57 Sm2 N4 C46 114.6(7) . . . . ? N3 Sm2 N4 C46 -178.2(8) . . . . ? Sm1 Sm2 N4 C46 -141.7(6) . . . . ? O4 Sm2 N4 C45 138.9(7) . . . . ? N6 Sm2 N4 C45 -127.6(7) . . . . ? O1 Sm2 N4 C45 75.0(7) . . . . ? O3 Sm2 N4 C45 -12.2(7) . . . . ? C57 Sm2 N4 C45 -120.7(7) . . . . ? N3 Sm2 N4 C45 -53.5(6) . . . . ? Sm1 Sm2 N4 C45 -17.0(11) . . . . ? O2 Sm1 N5 C57 -117.0(6) . . . . ? O3 Sm1 N5 C57 -28.6(6) . . . . ? O1 Sm1 N5 C57 41.5(6) . . . . ? N1 Sm1 N5 C57 113.5(6) . . . . ? N2 Sm1 N5 C57 167.8(5) . . . . ? Sm2 Sm1 N5 C57 6.1(5) . . . . ? O2 Sm1 N5 C58 47.0(15) . . . . ? O3 Sm1 N5 C58 135.5(14) . . . . ? O1 Sm1 N5 C58 -154.4(14) . . . . ? C57 Sm1 N5 C58 164.1(18) . . . . ? N1 Sm1 N5 C58 -82.5(15) . . . . ? N2 Sm1 N5 C58 -28.1(15) . . . . ? Sm2 Sm1 N5 C58 170.1(15) . . . . ? O4 Sm2 N6 C57 -114.1(6) . . . . ? O1 Sm2 N6 C57 -24.9(6) . . . . ? O3 Sm2 N6 C57 46.1(6) . . . . ? N3 Sm2 N6 C57 117.8(6) . . . . ? N4 Sm2 N6 C57 171.7(5) . . . . ? Sm1 Sm2 N6 C57 7.8(5) . . . . ? O4 Sm2 N6 C64 46.8(17) . . . . ? O1 Sm2 N6 C64 136.0(17) . . . . ? O3 Sm2 N6 C64 -153.0(17) . . . . ? C57 Sm2 N6 C64 161(2) . . . . ? N3 Sm2 N6 C64 -81.3(17) . . . . ? N4 Sm2 N6 C64 -27.4(18) . . . . ? Sm1 Sm2 N6 C64 168.8(17) . . . . ? Sm2 O1 C1 C6 111.3(9) . . . . ? Sm1 O1 C1 C6 -35.1(14) . . . . ? Sm2 O1 C1 C2 -72.3(12) . . . . ? Sm1 O1 C1 C2 141.3(8) . . . . ? O1 C1 C2 C3 -176.6(10) . . . . ? C6 C1 C2 C3 -0.1(15) . . . . ? O1 C1 C2 C19 -0.6(17) . . . . ? C6 C1 C2 C19 175.9(10) . . . . ? C1 C2 C3 C4 0.9(18) . . . . ? C19 C2 C3 C4 -175.5(11) . . . . ? C2 C3 C4 C5 -0.2(19) . . . . ? C2 C3 C4 C23 179.7(12) . . . . ? C3 C4 C5 C6 -1.3(18) . . . . ? C23 C4 C5 C6 178.8(12) . . . . ? C4 C5 C6 C1 2.1(18) . . . . ? C4 C5 C6 C13 178.7(11) . . . . ? O1 C1 C6 C5 175.4(10) . . . . ? C2 C1 C6 C5 -1.3(15) . . . . ? O1 C1 C6 C13 -1.3(14) . . . . ? C2 C1 C6 C13 -178.0(9) . . . . ? Sm1 O2 C7 C12 -60.4(12) . . . . ? Sm1 O2 C7 C8 119.4(10) . . . . ? O2 C7 C8 C9 -170.0(10) . . . . ? C12 C7 C8 C9 9.7(15) . . . . ? O2 C7 C8 C24 8.8(16) . . . . ? C12 C7 C8 C24 -171.5(10) . . . . ? C7 C8 C9 C10 -2.8(17) . . . . ? C24 C8 C9 C10 178.4(11) . . . . ? C8 C9 C10 C11 -6.0(17) . . . . ? C8 C9 C10 C28 174.4(11) . . . . ? C9 C10 C11 C12 7.8(17) . . . . ? C28 C10 C11 C12 -172.6(11) . . . . ? C10 C11 C12 C7 -0.8(17) . . . . ? C10 C11 C12 C18 177.4(11) . . . . ? O2 C7 C12 C11 171.5(9) . . . . ? C8 C7 C12 C11 -8.3(15) . . . . ? O2 C7 C12 C18 -6.7(15) . . . . ? C8 C7 C12 C18 173.5(10) . . . . ? C16 N1 C13 C6 43.3(12) . . . . ? C14 N1 C13 C6 162.7(9) . . . . ? Sm1 N1 C13 C6 -82.4(9) . . . . ? C5 C6 C13 N1 -112.7(12) . . . . ? C1 C6 C13 N1 64.1(12) . . . . ? C16 N1 C14 C15 -60.8(10) . . . . ? C13 N1 C14 C15 176.0(8) . . . . ? Sm1 N1 C14 C15 57.5(9) . . . . ? C18 N2 C15 C14 -174.5(8) . . . . ? C17 N2 C15 C14 65.0(10) . . . . ? Sm1 N2 C15 C14 -49.3(9) . . . . ? N1 C14 C15 N2 -3.1(11) . . . . ? C14 N1 C16 C17 64.2(11) . . . . ? C13 N1 C16 C17 -175.8(9) . . . . ? Sm1 N1 C16 C17 -50.2(10) . . . . ? C18 N2 C17 C16 178.7(9) . . . . ? C15 N2 C17 C16 -63.7(11) . . . . ? Sm1 N2 C17 C16 49.3(9) . . . . ? N1 C16 C17 N2 -1.9(12) . . . . ? C15 N2 C18 C12 65.0(12) . . . . ? C17 N2 C18 C12 -177.3(10) . . . . ? Sm1 N2 C18 C12 -53.1(12) . . . . ? C11 C12 C18 N2 -114.7(12) . . . . ? C7 C12 C18 N2 63.5(14) . . . . ? C3 C2 C19 C21 -163.5(11) . . . . ? C1 C2 C19 C21 20.4(16) . . . . ? C3 C2 C19 C20 73.7(12) . . . . ? C1 C2 C19 C20 -102.4(12) . . . . ? C3 C2 C19 C22 -43.8(14) . . . . ? C1 C2 C19 C22 140.1(11) . . . . ? C9 C8 C24 C25 -6.9(16) . . . . ? C7 C8 C24 C25 174.4(11) . . . . ? C9 C8 C24 C27 115.0(12) . . . . ? C7 C8 C24 C27 -63.7(14) . . . . ? C9 C8 C24 C26 -125.5(11) . . . . ? C7 C8 C24 C26 55.8(13) . . . . ? Sm1 O3 C29 C30 -72.5(12) . . . . ? Sm2 O3 C29 C30 144.7(9) . . . . ? Sm1 O3 C29 C34 114.2(9) . . . . ? Sm2 O3 C29 C34 -28.6(14) . . . . ? O3 C29 C30 C31 178.7(10) . . . . ? C34 C29 C30 C31 -8.1(15) . . . . ? O3 C29 C30 C47 -6.1(17) . . . . ? C34 C29 C30 C47 167.1(10) . . . . ? C29 C30 C31 C32 3.7(19) . . . . ? C47 C30 C31 C32 -171.7(11) . . . . ? C30 C31 C32 C33 1.7(19) . . . . ? C30 C31 C32 C51 -176.2(13) . . . . ? C31 C32 C33 C34 -2.6(18) . . . . ? C51 C32 C33 C34 175.4(12) . . . . ? C32 C33 C34 C29 -1.9(17) . . . . ? C32 C33 C34 C41 -179.5(11) . . . . ? O3 C29 C34 C33 -178.9(9) . . . . ? C30 C29 C34 C33 7.4(16) . . . . ? O3 C29 C34 C41 -1.4(15) . . . . ? C30 C29 C34 C41 -175.1(10) . . . . ? Sm2 O4 C35 C40 -58.0(15) . . . . ? Sm2 O4 C35 C36 123.5(10) . . . . ? O4 C35 C36 C37 -178.2(11) . . . . ? C40 C35 C36 C37 3.3(17) . . . . ? O4 C35 C36 C52 7.3(18) . . . . ? C40 C35 C36 C52 -171.3(11) . . . . ? C35 C36 C37 C38 0(2) . . . . ? C52 C36 C37 C38 174.3(13) . . . . ? C36 C37 C38 C39 -3(2) . . . . ? C36 C37 C38 C56 -179.7(13) . . . . ? C37 C38 C39 C40 3(2) . . . . ? C56 C38 C39 C40 179.9(13) . . . . ? C38 C39 C40 C35 -0.2(19) . . . . ? C38 C39 C40 C46 -176.4(12) . . . . ? O4 C35 C40 C39 178.3(11) . . . . ? C36 C35 C40 C39 -3.1(17) . . . . ? O4 C35 C40 C46 -5.5(16) . . . . ? C36 C35 C40 C46 173.1(10) . . . . ? C33 C34 C41 N3 -123.3(11) . . . . ? C29 C34 C41 N3 59.2(14) . . . . ? C44 N3 C41 C34 40.9(13) . . . . ? C42 N3 C41 C34 163.6(10) . . . . ? Sm2 N3 C41 C34 -79.0(10) . . . . ? C44 N3 C42 C43 -63.9(12) . . . . ? C41 N3 C42 C43 171.5(9) . . . . ? Sm2 N3 C42 C43 50.6(10) . . . . ? C46 N4 C43 C42 -179.0(9) . . . . ? C45 N4 C43 C42 58.0(12) . . . . ? Sm2 N4 C43 C42 -54.5(10) . . . . ? N3 C42 C43 N4 5.1(13) . . . . ? C42 N3 C44 C45 55.4(11) . . . . ? C41 N3 C44 C45 179.1(9) . . . . ? Sm2 N3 C44 C45 -58.4(9) . . . . ? C43 N4 C45 C44 -66.1(11) . . . . ? C46 N4 C45 C44 169.9(9) . . . . ? Sm2 N4 C45 C44 42.5(10) . . . . ? N3 C44 C45 N4 7.9(12) . . . . ? C43 N4 C46 C40 57.7(13) . . . . ? C45 N4 C46 C40 178.6(9) . . . . ? Sm2 N4 C46 C40 -58.8(11) . . . . ? C39 C40 C46 N4 -121.6(12) . . . . ? C35 C40 C46 N4 62.2(14) . . . . ? C31 C30 C47 C50 79.1(13) . . . . ? C29 C30 C47 C50 -96.0(13) . . . . ? C31 C30 C47 C49 -158.0(11) . . . . ? C29 C30 C47 C49 26.9(15) . . . . ? C31 C30 C47 C48 -39.4(14) . . . . ? C29 C30 C47 C48 145.5(12) . . . . ? C37 C36 C52 C54 -117.7(14) . . . . ? C35 C36 C52 C54 56.4(15) . . . . ? C37 C36 C52 C53 1.1(19) . . . . ? C35 C36 C52 C53 175.2(12) . . . . ? C37 C36 C52 C55 120.3(13) . . . . ? C35 C36 C52 C55 -65.6(16) . . . . ? C58 N5 C57 N6 -0.3(19) . . . . ? Sm1 N5 C57 N6 170.6(13) . . . . ? C58 N5 C57 Sm2 169.9(12) . . . . ? Sm1 N5 C57 Sm2 -19.2(16) . . . . ? C58 N5 C57 Sm1 -170.9(10) . . . . ? C64 N6 C57 N5 4.9(19) . . . . ? Sm2 N6 C57 N5 175.4(13) . . . . ? C64 N6 C57 Sm2 -170.6(10) . . . . ? C64 N6 C57 Sm1 164.7(12) . . . . ? Sm2 N6 C57 Sm1 -24.7(15) . . . . ? O4 Sm2 C57 N5 -99.0(17) . . . . ? N6 Sm2 C57 N5 -173(2) . . . . ? O1 Sm2 C57 N5 -16.0(16) . . . . ? O3 Sm2 C57 N5 53.0(16) . . . . ? N3 Sm2 C57 N5 122.6(16) . . . . ? N4 Sm2 C57 N5 174.9(15) . . . . ? Sm1 Sm2 C57 N5 17.8(15) . . . . ? O4 Sm2 C57 N6 73.8(6) . . . . ? O1 Sm2 C57 N6 156.8(6) . . . . ? O3 Sm2 C57 N6 -134.2(6) . . . . ? N3 Sm2 C57 N6 -64.6(6) . . . . ? N4 Sm2 C57 N6 -12.4(8) . . . . ? Sm1 Sm2 C57 N6 -169.4(7) . . . . ? O4 Sm2 C57 Sm1 -116.8(3) . . . . ? N6 Sm2 C57 Sm1 169.4(7) . . . . ? O1 Sm2 C57 Sm1 -33.8(2) . . . . ? O3 Sm2 C57 Sm1 35.2(2) . . . . ? N3 Sm2 C57 Sm1 104.8(3) . . . . ? N4 Sm2 C57 Sm1 157.0(3) . . . . ? O2 Sm1 C57 N5 70.9(6) . . . . ? O3 Sm1 C57 N5 152.5(6) . . . . ? O1 Sm1 C57 N5 -139.3(6) . . . . ? N1 Sm1 C57 N5 -69.9(6) . . . . ? N2 Sm1 C57 N5 -17.6(8) . . . . ? Sm2 Sm1 C57 N5 -171.8(7) . . . . ? O2 Sm1 C57 N6 -94.4(16) . . . . ? N5 Sm1 C57 N6 -165.3(19) . . . . ? O3 Sm1 C57 N6 -12.8(16) . . . . ? O1 Sm1 C57 N6 55.5(16) . . . . ? N1 Sm1 C57 N6 124.8(16) . . . . ? N2 Sm1 C57 N6 177.2(14) . . . . ? Sm2 Sm1 C57 N6 23.0(14) . . . . ? O2 Sm1 C57 Sm2 -117.4(3) . . . . ? N5 Sm1 C57 Sm2 171.8(7) . . . . ? O3 Sm1 C57 Sm2 -35.7(2) . . . . ? O1 Sm1 C57 Sm2 32.5(2) . . . . ? N1 Sm1 C57 Sm2 101.8(3) . . . . ? N2 Sm1 C57 Sm2 154.2(3) . . . . ? C57 N5 C58 C63 152.1(10) . . . . ? Sm1 N5 C58 C63 -8.2(19) . . . . ? C57 N5 C58 C59 -86.7(12) . . . . ? Sm1 N5 C58 C59 112.9(14) . . . . ? N5 C58 C59 C60 177.2(9) . . . . ? C63 C58 C59 C60 -59.6(12) . . . . ? C58 C59 C60 C61 57.6(13) . . . . ? C59 C60 C61 C62 -55.9(14) . . . . ? C60 C61 C62 C63 56.7(14) . . . . ? C61 C62 C63 C58 -61.1(13) . . . . ? N5 C58 C63 C62 -174.0(9) . . . . ? C59 C58 C63 C62 62.5(12) . . . . ? C57 N6 C64 C65 151.0(10) . . . . ? Sm2 N6 C64 C65 -6(2) . . . . ? C57 N6 C64 C69 -87.2(12) . . . . ? Sm2 N6 C64 C69 115.5(16) . . . . ? N6 C64 C65 C66 -174.9(10) . . . . ? C69 C64 C65 C66 61.9(13) . . . . ? C64 C65 C66 C67 -57.1(15) . . . . ? C65 C66 C67 C68 53.4(17) . . . . ? C66 C67 C68 C69 -54.2(17) . . . . ? N6 C64 C69 C68 176.3(9) . . . . ? C65 C64 C69 C68 -61.0(12) . . . . ? C67 C68 C69 C64 57.6(15) . . . . ? C73 O5 C70 C71 -9(8) . . . . ? C73' O5' C70' C71' -57(6) . . . . ? O5 C70 C71 C72 0(9) . . . . ? O5' C70' C71' C72' 41(7) . . . . ? C70 C71 C72 C73 8(9) . . . . ? C70' C71' C72' C73' -16(9) . . . . ? C70 O5 C73 C72 14(10) . . . . ? C71 C72 C73 O5 -14(11) . . . . ? C70' O5' C73' C72' 52(7) . . . . ? C71' C72' C73' O5' -18(8) . . . . ? C77 O6 C74 C75 36(6) . . . . ? C77' O6' C74' C75' -19(7) . . . . ? O6 C74 C75 C76 -13(7) . . . . ? O6' C74' C75' C76' 42(6) . . . . ? C74 C75 C76 C77 -13(8) . . . . ? C74' C75' C76' C77' -47(5) . . . . ? C74 O6 C77 C76 -48(6) . . . . ? C75 C76 C77 O6 33(6) . . . . ? C74' O6' C77' C76' -13(6) . . . . ? C75' C76' C77' O6' 41(6) . . . . ? C81 O7 C78 C79 19(9) . . . . ? C81' O7' C78' C79' 55(4) . . . . ? O7 C78 C79 C80 -8(9) . . . . ? O7' C78' C79' C80' -41(6) . . . . ? C78 C79 C80 C81 -5(9) . . . . ? C78' C79' C80' C81' 16(9) . . . . ? C78 O7 C81 C80 -22(9) . . . . ? C79 C80 C81 O7 17(10) . . . . ? C78' O7' C81' C80' -44(6) . . . . ? C79' C80' C81' O7' 17(9) . . . . ? C85 O8 C82 C83 -1(5) . . . . ? C85' O8' C82' C83' 1(5) . . . . ? O8 C82 C83 C84 -20(5) . . . . ? O8' C82' C83' C84' -31(5) . . . . ? C82 C83 C84 C85 33(5) . . . . ? C82' C83' C84' C85' 46(4) . . . . ? C82 O8 C85 C84 21(5) . . . . ? C83 C84 C85 O8 -32(4) . . . . ? C82' O8' C85' C84' 28(5) . . . . ? C83' C84' C85' O8' -45(4) . . . . ? C89 O9 C86 C87 -35(10) . . . . ? C89' O9' C86' C87' -8(11) . . . . ? O9 C86 C87 C88 6(11) . . . . ? O9' C86' C87' C88' -36(11) . . . . ? C86 C87 C88 C89 26(10) . . . . ? C86' C87' C88' C89' 62(9) . . . . ? C86 O9 C89 C88 50(9) . . . . ? C87 C88 C89 O9 -50(10) . . . . ? C86' O9' C89' C88' 49(9) . . . . ? C87' C88' C89' O9' -64(9) . . . . ? C91 O10 C90 C92 -73(5) 3_676 . . 3_676 ? C93 O10 C90 C92 -121(6) . . . 3_676 ? C91 O10 C90 C93 35(10) 3_676 . . 3_676 ? C92 O10 C90 C93 108(12) 3_676 . . 3_676 ? C93 O10 C90 C93 -13(12) . . . 3_676 ? C91 O10 C90 C91 66(7) 3_676 . . . ? C92 O10 C90 C91 139(8) 3_676 . . . ? C93 O10 C90 C91 18(5) . . . . ? C92 O10 C90 C91 73(5) 3_676 . . 3_676 ? C93 O10 C90 C91 -49(5) . . . 3_676 ? C92 C90 C91 O10 -20(8) 3_676 . . 3_676 ? C93 C90 C91 O10 73(7) 3_676 . . 3_676 ? O10 C90 C91 O10 -78(7) . . . 3_676 ? C91 C90 C91 O10 -54(5) 3_676 . . 3_676 ? C92 C90 C91 C93 -92(10) 3_676 . . 3_676 ? O10 C90 C91 C93 -151(8) . . . 3_676 ? C91 C90 C91 C93 -127(8) 3_676 . . 3_676 ? C92 C90 C91 C92 49(11) 3_676 . . . ? C93 C90 C91 C92 142(8) 3_676 . . . ? O10 C90 C91 C92 -9(6) . . . . ? C91 C90 C91 C92 15(4) 3_676 . . . ? C92 C90 C91 C90 35(7) 3_676 . . 3_676 ? C93 C90 C91 C90 127(8) 3_676 . . 3_676 ? O10 C90 C91 C90 -24(3) . . . 3_676 ? C91 C90 C91 C90 0.000(6) 3_676 . . 3_676 ? O10 C91 C92 C90 69(6) 3_676 . . 3_676 ? C93 C91 C92 C90 5(11) 3_676 . . 3_676 ? C90 C91 C92 C90 -32(9) . . . 3_676 ? C93 C91 C92 O10 -64(9) 3_676 . . 3_676 ? C90 C91 C92 O10 -101(8) . . . 3_676 ? C90 C91 C92 O10 -69(6) 3_676 . . 3_676 ? O10 C91 C92 C93 99(5) 3_676 . . . ? C93 C91 C92 C93 34(11) 3_676 . . . ? C90 C91 C92 C93 -2(7) . . . . ? C90 C91 C92 C93 30(5) 3_676 . . . ? C91 O10 C93 C90 -71(8) 3_676 . . 3_676 ? C92 O10 C93 C90 -28(8) 3_676 . . 3_676 ? C90 O10 C93 C90 10(9) . . . 3_676 ? C92 O10 C93 C91 43(6) 3_676 . . 3_676 ? C90 O10 C93 C91 81(7) . . . 3_676 ? C91 O10 C93 C92 -103(7) 3_676 . . . ? C92 O10 C93 C92 -60(6) 3_676 . . . ? C90 O10 C93 C92 -22(6) . . . . ? O10 C92 C93 C90 -51(8) 3_676 . . 3_676 ? C91 C92 C93 C90 -82(9) . . . 3_676 ? C90 C92 C93 C91 60(9) 3_676 . . 3_676 ? O10 C92 C93 C91 10(6) 3_676 . . 3_676 ? C91 C92 C93 C91 -22(8) . . . 3_676 ? C90 C92 C93 O10 95(9) 3_676 . . . ? O10 C92 C93 O10 45(6) 3_676 . . . ? C91 C92 C93 O10 13(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.301 _refine_diff_density_min -1.522 _refine_diff_density_rms 0.153 #===END