# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Yingming Yao' _publ_contact_author_email YAOYM@SUDA.EDU.CN _publ_section_title ; Synthesis and characterization of amine bridged bis(phenolate) lanthanide aryloxides and their application in the polymerization of L-lactide ; loop_ _publ_author_name 'Yingming Yao.' 'Xiangyong Gu.' 'Kun Nie.' 'Qi Shen.' 'Yong Zhang.' # Attachment 'NieKun-dalton.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 763744' #TrackingRef 'NieKun-dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H79 N2 Nd O4' _chemical_formula_sum 'C50 H79 N2 Nd O4' _chemical_formula_weight 916.39 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 15.2696(6) _cell_length_b 16.8752(7) _cell_length_c 19.2287(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4954.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13280 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1940 _exptl_absorpt_coefficient_mu 1.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.483 _exptl_absorpt_correction_T_max 0.653 _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 14970 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8503 _reflns_number_gt 7930 _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. Because there are disordered atoms (C32-C34, C42, C43), which caused abnormal bond distances or thermal parameters, constraints are used during refinements. ; _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^)+(0.0503P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(14) _refine_ls_number_reflns 8503 _refine_ls_number_parameters 495 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.026386(16) 0.873014(14) 0.892647(13) 0.03131(8) Uani 1 1 d . . . O1 O -0.0509(2) 0.9544(2) 0.95974(19) 0.0408(9) Uani 1 1 d . . . O2 O 0.1569(2) 0.8317(2) 0.85495(19) 0.0397(9) Uani 1 1 d . . . O3 O -0.0680(3) 0.7811(2) 0.85937(19) 0.0446(9) Uani 1 1 d . . . O4 O 0.0780(3) 0.8218(2) 1.00743(19) 0.0533(11) Uani 1 1 d . . . N1 N 0.1319(3) 0.9981(2) 0.9097(2) 0.0312(9) Uani 1 1 d . . . N2 N 0.0075(3) 0.9827(3) 0.7924(2) 0.0437(11) Uani 1 1 d . . . C1 C -0.0580(3) 1.0307(3) 0.9762(3) 0.0343(12) Uani 1 1 d . . . C2 C -0.1398(4) 1.0672(3) 0.9872(3) 0.0383(12) Uani 1 1 d . . . C3 C -0.1411(4) 1.1495(3) 0.9987(3) 0.0398(13) Uani 1 1 d . . . H3 H -0.1958 1.1738 1.0055 0.048 Uiso 1 1 calc R . . C4 C -0.0679(4) 1.1966(3) 1.0006(3) 0.0392(13) Uani 1 1 d . . . C5 C 0.0135(4) 1.1588(3) 0.9928(3) 0.0382(12) Uani 1 1 d . . . H5 H 0.0654 1.1885 0.9961 0.046 Uiso 1 1 calc R . . C6 C 0.0182(4) 1.0759(3) 0.9800(2) 0.0336(11) Uani 1 1 d . . . C7 C 0.2324(3) 0.8603(3) 0.8298(3) 0.0343(11) Uani 1 1 d . . . C8 C 0.2798(4) 0.8213(3) 0.7763(3) 0.0384(12) Uani 1 1 d . . . C9 C 0.3557(3) 0.8568(3) 0.7518(3) 0.0414(13) Uani 1 1 d . . . H9 H 0.3869 0.8310 0.7163 0.050 Uiso 1 1 calc R . . C10 C 0.3886(4) 0.9290(3) 0.7770(3) 0.0410(13) Uani 1 1 d . A . C11 C 0.3422(3) 0.9632(3) 0.8303(3) 0.0362(12) Uani 1 1 d . . . H11 H 0.3631 1.0109 0.8493 0.043 Uiso 1 1 calc R . . C12 C 0.2668(3) 0.9310(3) 0.8573(3) 0.0343(11) Uani 1 1 d . . . C13 C 0.1069(3) 1.0371(3) 0.9762(3) 0.0343(12) Uani 1 1 d . . . H13A H 0.1511 1.0775 0.9867 0.041 Uiso 1 1 calc R . . H13B H 0.1100 0.9972 1.0132 0.041 Uiso 1 1 calc R . . C14 C 0.2232(3) 0.9677(3) 0.9200(3) 0.0343(12) Uani 1 1 d . . . H14A H 0.2220 0.9281 0.9573 0.041 Uiso 1 1 calc R . . H14B H 0.2598 1.0118 0.9361 0.041 Uiso 1 1 calc R . . C15 C 0.1302(4) 1.0544(3) 0.8508(3) 0.0405(13) Uani 1 1 d . . . H15A H 0.1736 1.0377 0.8162 0.049 Uiso 1 1 calc R . . H15B H 0.1473 1.1070 0.8676 0.049 Uiso 1 1 calc R . . C16 C 0.0415(4) 1.0603(3) 0.8161(3) 0.0475(14) Uani 1 1 d . . . H16A H -0.0003 1.0836 0.8490 0.057 Uiso 1 1 calc R . . H16B H 0.0459 1.0960 0.7760 0.057 Uiso 1 1 calc R . . C17 C -0.0860(5) 0.9955(5) 0.7734(4) 0.0672(19) Uani 1 1 d . . . H17A H -0.0906 1.0409 0.7427 0.101 Uiso 1 1 calc R . . H17B H -0.1199 1.0052 0.8152 0.101 Uiso 1 1 calc R . . H17C H -0.1084 0.9488 0.7500 0.101 Uiso 1 1 calc R . . C18 C 0.0563(5) 0.9528(4) 0.7326(3) 0.0586(17) Uani 1 1 d . . . H18A H 0.0515 0.9901 0.6944 0.088 Uiso 1 1 calc R . . H18B H 0.0323 0.9020 0.7185 0.088 Uiso 1 1 calc R . . H18C H 0.1174 0.9463 0.7452 0.088 Uiso 1 1 calc R . . C19 C -0.2246(4) 1.0190(4) 0.9915(3) 0.0479(14) Uani 1 1 d . . . C20 C -0.3043(4) 1.0701(4) 1.0073(4) 0.067(2) Uani 1 1 d . . . H20A H -0.3565 1.0372 1.0074 0.101 Uiso 1 1 calc R . . H20B H -0.3100 1.1109 0.9721 0.101 Uiso 1 1 calc R . . H20C H -0.2974 1.0946 1.0526 0.101 Uiso 1 1 calc R . . C21 C -0.2429(4) 0.9777(4) 0.9215(4) 0.0639(19) Uani 1 1 d . . . H21A H -0.1987 0.9376 0.9132 0.096 Uiso 1 1 calc R . . H21B H -0.2413 1.0166 0.8843 0.096 Uiso 1 1 calc R . . H21C H -0.3003 0.9531 0.9229 0.096 Uiso 1 1 calc R . . C22 C -0.2166(5) 0.9574(4) 1.0485(4) 0.0653(19) Uani 1 1 d . . . H22A H -0.1654 0.9248 1.0401 0.098 Uiso 1 1 calc R . . H22B H -0.2685 0.9243 1.0488 0.098 Uiso 1 1 calc R . . H22C H -0.2108 0.9837 1.0931 0.098 Uiso 1 1 calc R . . C23 C -0.0702(4) 1.2865(3) 1.0128(3) 0.0485(14) Uani 1 1 d . . . C24 C -0.1640(5) 1.3176(5) 1.0111(5) 0.086(3) Uani 1 1 d . . . H24A H -0.1970 1.2948 1.0493 0.129 Uiso 1 1 calc R . . H24B H -0.1912 1.3029 0.9673 0.129 Uiso 1 1 calc R . . H24C H -0.1635 1.3749 1.0154 0.129 Uiso 1 1 calc R . . C25 C -0.0262(7) 1.3046(4) 1.0809(4) 0.088(3) Uani 1 1 d . . . H25A H -0.0600 1.2820 1.1187 0.132 Uiso 1 1 calc R . . H25B H -0.0223 1.3616 1.0869 0.132 Uiso 1 1 calc R . . H25C H 0.0322 1.2821 1.0810 0.132 Uiso 1 1 calc R . . C26 C -0.0195(6) 1.3281(4) 0.9541(4) 0.074(2) Uani 1 1 d . . . H26A H -0.0228 1.3851 0.9604 0.110 Uiso 1 1 calc R . . H26B H -0.0450 1.3140 0.9096 0.110 Uiso 1 1 calc R . . H26C H 0.0413 1.3115 0.9552 0.110 Uiso 1 1 calc R . . C27 C 0.2495(4) 0.7396(3) 0.7481(3) 0.0475(14) Uani 1 1 d . . . C28 C 0.3114(5) 0.7084(4) 0.6900(4) 0.069(2) Uani 1 1 d . . . H28A H 0.2974 0.6536 0.6798 0.104 Uiso 1 1 calc R . . H28B H 0.3717 0.7122 0.7055 0.104 Uiso 1 1 calc R . . H28C H 0.3037 0.7401 0.6483 0.104 Uiso 1 1 calc R . . C29 C 0.2520(5) 0.6789(3) 0.8088(4) 0.0636(19) Uani 1 1 d . . . H29A H 0.2114 0.6952 0.8448 0.095 Uiso 1 1 calc R . . H29B H 0.3108 0.6765 0.8278 0.095 Uiso 1 1 calc R . . H29C H 0.2354 0.6270 0.7916 0.095 Uiso 1 1 calc R . . C30 C 0.1572(5) 0.7443(5) 0.7178(4) 0.069(2) Uani 1 1 d . . . H30A H 0.1164 0.7601 0.7539 0.104 Uiso 1 1 calc R . . H30B H 0.1404 0.6928 0.6998 0.104 Uiso 1 1 calc R . . H30C H 0.1560 0.7830 0.6805 0.104 Uiso 1 1 calc R . . C31 C 0.4745(4) 0.9650(3) 0.7487(3) 0.0484(13) Uani 1 1 d D . . C32 C 0.5420(9) 0.9630(9) 0.8091(7) 0.0669(18) Uani 0.50 1 d PD A 1 C32' C 0.5510(9) 0.9300(10) 0.7893(8) 0.0669(18) Uani 0.50 1 d PD A 2 C33 C 0.4594(11) 1.0533(9) 0.7335(10) 0.0669(18) Uani 0.50 1 d PD A 1 C33' C 0.4796(11) 1.0532(9) 0.7544(10) 0.0669(18) Uani 0.50 1 d PD A 2 C34 C 0.5130(9) 0.9211(8) 0.6874(7) 0.0669(18) Uani 0.50 1 d PD A 1 C34' C 0.4794(10) 0.9500(9) 0.6689(7) 0.0669(18) Uani 0.50 1 d PD A 2 C35 C -0.1203(3) 0.7181(3) 0.8488(3) 0.0386(12) Uani 1 1 d . . . C36 C -0.1163(3) 0.6519(3) 0.8931(3) 0.0403(11) Uani 1 1 d . B . C37 C -0.1699(4) 0.5883(4) 0.8815(3) 0.0495(15) Uani 1 1 d . . . H37 H -0.1665 0.5443 0.9114 0.059 Uiso 1 1 calc R . . C38 C -0.2293(4) 0.5868(4) 0.8270(4) 0.0568(17) Uani 1 1 d . . . H38 H -0.2648 0.5422 0.8191 0.068 Uiso 1 1 calc R . . C39 C -0.2347(4) 0.6518(4) 0.7851(4) 0.0569(17) Uani 1 1 d . . . H39 H -0.2758 0.6517 0.7487 0.068 Uiso 1 1 calc R . . C40 C -0.1820(4) 0.7182(4) 0.7939(3) 0.0437(13) Uani 1 1 d . D . C41 C -0.0469(4) 0.6527(4) 0.9514(3) 0.0603(18) Uani 1 1 d D . . C42 C 0.0396(8) 0.6257(11) 0.9166(7) 0.080(3) Uani 0.50 1 d PD B 1 C42' C -0.0361(12) 0.5757(9) 0.9933(9) 0.080(3) Uani 0.50 1 d PD B 2 C43 C -0.0733(11) 0.6036(11) 1.0142(8) 0.080(3) Uani 0.50 1 d PD B 1 C43' C -0.0985(10) 0.6948(10) 1.0092(7) 0.080(3) Uani 0.50 1 d PD B 2 C44 C -0.1861(5) 0.7913(6) 0.7466(4) 0.0805(13) Uani 1 1 d . . . H44 H -0.1733 0.8390 0.7748 0.097 Uiso 1 1 calc R C 1 C45 C -0.2768(5) 0.8012(5) 0.7130(4) 0.0805(13) Uani 1 1 d . D 1 H45A H -0.2822 0.8544 0.6942 0.121 Uiso 1 1 calc R D 1 H45B H -0.3219 0.7927 0.7477 0.121 Uiso 1 1 calc R D 1 H45C H -0.2835 0.7629 0.6757 0.121 Uiso 1 1 calc R D 1 C46 C -0.1200(5) 0.7855(5) 0.6898(4) 0.0805(13) Uani 1 1 d . D . H46A H -0.0627 0.7759 0.7097 0.121 Uiso 1 1 calc R . . H46B H -0.1191 0.8347 0.6637 0.121 Uiso 1 1 calc R . . H46C H -0.1354 0.7422 0.6590 0.121 Uiso 1 1 calc R . . C47 C 0.1553(7) 0.7784(5) 1.0240(4) 0.0835(13) Uani 1 1 d . . . H47A H 0.2035 0.8144 1.0356 0.100 Uiso 1 1 calc R . . H47B H 0.1733 0.7451 0.9847 0.100 Uiso 1 1 calc R . . C48 C 0.1313(7) 0.7286(5) 1.0851(4) 0.0835(13) Uani 1 1 d . . . H48A H 0.1089 0.6771 1.0699 0.100 Uiso 1 1 calc R . . H48B H 0.1824 0.7200 1.1150 0.100 Uiso 1 1 calc R . . C49 C 0.0636(6) 0.7729(4) 1.1223(4) 0.0835(13) Uani 1 1 d . . . H49A H 0.0878 0.7986 1.1637 0.100 Uiso 1 1 calc R . . H49B H 0.0156 0.7379 1.1364 0.100 Uiso 1 1 calc R . . C50 C 0.0325(7) 0.8332(4) 1.0709(4) 0.0835(13) Uani 1 1 d . . . H50A H -0.0307 0.8273 1.0634 0.100 Uiso 1 1 calc R . . H50B H 0.0436 0.8867 1.0887 0.100 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.03123(13) 0.02629(11) 0.03639(14) 0.00101(12) -0.00081(11) -0.00106(12) O1 0.037(2) 0.0300(17) 0.056(2) -0.0041(16) 0.0077(17) -0.0001(16) O2 0.035(2) 0.0317(19) 0.052(2) -0.0058(16) 0.0066(17) 0.0004(16) O3 0.043(2) 0.0384(19) 0.052(2) -0.0047(16) -0.0013(18) -0.0104(19) O4 0.077(3) 0.047(2) 0.036(2) -0.0014(17) -0.011(2) 0.017(2) N1 0.026(2) 0.028(2) 0.040(3) -0.0010(17) 0.0034(18) -0.0011(17) N2 0.043(3) 0.040(2) 0.048(3) 0.009(2) -0.010(2) -0.003(2) C1 0.037(3) 0.029(3) 0.037(3) 0.000(2) 0.008(2) 0.004(2) C2 0.034(3) 0.042(3) 0.039(3) -0.001(2) 0.002(2) -0.006(3) C3 0.033(3) 0.043(3) 0.044(3) -0.006(2) 0.007(2) 0.009(2) C4 0.041(3) 0.031(3) 0.046(3) -0.004(2) 0.002(3) 0.005(3) C5 0.038(3) 0.038(3) 0.039(3) -0.005(2) -0.001(2) -0.005(3) C6 0.030(3) 0.036(2) 0.035(3) -0.001(2) 0.006(2) 0.005(3) C7 0.032(2) 0.032(3) 0.039(3) 0.002(2) 0.000(2) 0.005(2) C8 0.045(3) 0.035(3) 0.035(3) -0.002(2) -0.002(2) -0.002(3) C9 0.041(3) 0.050(4) 0.034(3) -0.003(2) 0.006(2) 0.006(3) C10 0.038(3) 0.042(3) 0.044(3) 0.009(3) -0.001(2) 0.007(3) C11 0.033(3) 0.033(3) 0.042(3) -0.001(2) -0.003(2) -0.002(2) C12 0.031(3) 0.031(2) 0.040(3) -0.001(2) 0.002(2) 0.004(2) C13 0.031(3) 0.031(3) 0.042(3) -0.007(2) 0.004(2) -0.003(2) C14 0.028(3) 0.034(3) 0.041(3) 0.000(2) -0.003(2) 0.002(2) C15 0.039(3) 0.032(3) 0.051(3) 0.006(2) 0.000(3) -0.003(3) C16 0.048(4) 0.039(3) 0.056(4) 0.010(3) 0.007(3) -0.001(3) C17 0.059(4) 0.075(5) 0.068(4) 0.020(4) -0.011(4) 0.003(4) C18 0.067(4) 0.052(4) 0.056(4) 0.005(3) -0.004(3) 0.002(3) C19 0.036(3) 0.043(3) 0.064(4) 0.005(3) 0.001(3) -0.006(3) C20 0.032(3) 0.065(4) 0.105(6) -0.009(4) 0.013(3) -0.003(3) C21 0.040(3) 0.064(4) 0.087(5) -0.016(4) 0.000(3) -0.011(3) C22 0.049(4) 0.059(4) 0.087(5) 0.018(4) 0.019(4) -0.013(3) C23 0.051(3) 0.031(3) 0.063(4) -0.012(3) 0.007(3) 0.003(3) C24 0.068(5) 0.052(4) 0.139(8) -0.014(4) 0.017(5) 0.017(4) C25 0.130(7) 0.057(4) 0.075(5) -0.023(3) -0.009(5) 0.000(6) C26 0.086(5) 0.043(3) 0.093(5) -0.007(3) 0.015(5) -0.002(4) C27 0.053(3) 0.043(3) 0.047(4) -0.008(3) 0.006(3) 0.000(3) C28 0.089(5) 0.056(4) 0.062(5) -0.030(3) 0.015(4) 0.002(4) C29 0.070(5) 0.031(3) 0.090(5) 0.006(3) 0.013(4) 0.002(3) C30 0.063(5) 0.075(5) 0.069(5) -0.021(4) -0.007(4) -0.008(4) C31 0.040(3) 0.056(3) 0.049(3) 0.010(3) 0.007(3) 0.002(3) C32 0.046(4) 0.067(4) 0.088(5) 0.007(3) 0.020(3) 0.005(3) C32' 0.046(4) 0.067(4) 0.088(5) 0.007(3) 0.020(3) 0.005(3) C33 0.046(4) 0.067(4) 0.088(5) 0.007(3) 0.020(3) 0.005(3) C33' 0.046(4) 0.067(4) 0.088(5) 0.007(3) 0.020(3) 0.005(3) C34 0.046(4) 0.067(4) 0.088(5) 0.007(3) 0.020(3) 0.005(3) C34' 0.046(4) 0.067(4) 0.088(5) 0.007(3) 0.020(3) 0.005(3) C35 0.029(3) 0.038(3) 0.049(3) -0.014(2) 0.001(2) -0.003(2) C36 0.033(2) 0.036(2) 0.052(3) -0.007(3) -0.003(3) -0.007(2) C37 0.039(3) 0.050(3) 0.059(4) -0.008(3) 0.002(3) -0.011(3) C38 0.041(3) 0.058(4) 0.072(4) -0.021(4) -0.002(3) -0.013(3) C39 0.040(3) 0.069(4) 0.061(4) -0.025(3) -0.012(3) 0.002(3) C40 0.035(3) 0.048(3) 0.048(3) -0.011(3) -0.002(3) 0.004(3) C41 0.058(4) 0.072(4) 0.051(4) 0.010(3) -0.009(3) -0.020(3) C42 0.066(6) 0.094(6) 0.078(5) 0.017(5) -0.024(4) -0.004(5) C42' 0.066(6) 0.094(6) 0.078(5) 0.017(5) -0.024(4) -0.004(5) C43 0.066(6) 0.094(6) 0.078(5) 0.017(5) -0.024(4) -0.004(5) C43' 0.066(6) 0.094(6) 0.078(5) 0.017(5) -0.024(4) -0.004(5) C44 0.065(3) 0.092(3) 0.085(3) 0.013(3) -0.001(2) 0.011(3) C45 0.065(3) 0.092(3) 0.085(3) 0.013(3) -0.001(2) 0.011(3) C46 0.065(3) 0.092(3) 0.085(3) 0.013(3) -0.001(2) 0.011(3) C47 0.122(4) 0.069(2) 0.060(2) 0.0108(18) -0.015(2) 0.020(2) C48 0.122(4) 0.069(2) 0.060(2) 0.0108(18) -0.015(2) 0.020(2) C49 0.122(4) 0.069(2) 0.060(2) 0.0108(18) -0.015(2) 0.020(2) C50 0.122(4) 0.069(2) 0.060(2) 0.0108(18) -0.015(2) 0.020(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O3 2.212(4) . ? Nd1 O1 2.224(3) . ? Nd1 O2 2.232(4) . ? Nd1 O4 2.498(4) . ? Nd1 N1 2.676(4) . ? Nd1 N2 2.687(4) . ? O1 C1 1.331(6) . ? O2 C7 1.341(6) . ? O3 C35 1.346(6) . ? O4 C50 1.418(9) . ? O4 C47 1.426(9) . ? N1 C15 1.478(6) . ? N1 C13 1.489(6) . ? N1 C14 1.499(6) . ? N2 C18 1.460(8) . ? N2 C16 1.481(7) . ? N2 C17 1.490(8) . ? C1 C6 1.392(8) . ? C1 C2 1.408(8) . ? C2 C3 1.406(8) . ? C2 C19 1.531(8) . ? C3 C4 1.373(8) . ? C3 H3 0.9400 . ? C4 C5 1.406(8) . ? C4 C23 1.534(7) . ? C5 C6 1.422(7) . ? C5 H5 0.9400 . ? C6 C13 1.507(7) . ? C7 C12 1.407(7) . ? C7 C8 1.419(7) . ? C8 C9 1.387(8) . ? C8 C27 1.552(7) . ? C9 C10 1.404(8) . ? C9 H9 0.9400 . ? C10 C11 1.373(8) . ? C10 C31 1.545(8) . ? C11 C12 1.375(7) . ? C11 H11 0.9400 . ? C12 C14 1.509(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.514(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C22 1.516(9) . ? C19 C20 1.523(9) . ? C19 C21 1.540(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 C25 1.503(10) . ? C23 C24 1.526(10) . ? C23 C26 1.540(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? 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 C30 1.528(9) . ? C27 C29 1.553(9) . ? C27 C28 1.556(9) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 C33' 1.493(15) . ? C31 C34 1.513(13) . ? C31 C32' 1.525(14) . ? C31 C33 1.536(15) . ? C31 C32 1.553(14) . ? C31 C34' 1.558(13) . ? C35 C36 1.407(8) . ? C35 C40 1.415(8) . ? C36 C37 1.369(7) . ? C36 C41 1.543(8) . ? C37 C38 1.386(9) . ? C37 H37 0.9400 . ? C38 C39 1.363(9) . ? C38 H38 0.9400 . ? C39 C40 1.389(9) . ? C39 H39 0.9400 . ? C40 C44 1.534(10) . ? C41 C43 1.517(14) . ? C41 C43' 1.536(14) . ? C41 C42' 1.538(14) . ? C41 C42 1.550(13) . ? C44 C46 1.490(10) . ? C44 C45 1.537(11) . ? C44 H44 0.9900 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 C48 1.490(11) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 C49 1.463(12) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.494(9) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Nd1 O1 104.77(14) . . ? O3 Nd1 O2 105.59(14) . . ? O1 Nd1 O2 148.79(13) . . ? O3 Nd1 O4 102.61(15) . . ? O1 Nd1 O4 82.46(13) . . ? O2 Nd1 O4 84.10(15) . . ? O3 Nd1 N1 168.80(13) . . ? O1 Nd1 N1 76.19(12) . . ? O2 Nd1 N1 75.44(13) . . ? O4 Nd1 N1 88.58(14) . . ? O3 Nd1 N2 101.86(14) . . ? O1 Nd1 N2 86.19(14) . . ? O2 Nd1 N2 94.48(14) . . ? O4 Nd1 N2 154.94(14) . . ? N1 Nd1 N2 66.98(13) . . ? C1 O1 Nd1 141.2(3) . . ? C7 O2 Nd1 140.5(3) . . ? C35 O3 Nd1 170.0(4) . . ? C50 O4 C47 106.5(5) . . ? C50 O4 Nd1 124.0(4) . . ? C47 O4 Nd1 129.5(4) . . ? C15 N1 C13 111.7(4) . . ? C15 N1 C14 109.7(4) . . ? C13 N1 C14 106.0(4) . . ? C15 N1 Nd1 113.8(3) . . ? C13 N1 Nd1 107.4(3) . . ? C14 N1 Nd1 107.8(3) . . ? C18 N2 C16 111.7(5) . . ? C18 N2 C17 110.2(5) . . ? C16 N2 C17 106.4(5) . . ? C18 N2 Nd1 105.8(3) . . ? C16 N2 Nd1 110.6(3) . . ? C17 N2 Nd1 112.3(4) . . ? O1 C1 C6 118.3(4) . . ? O1 C1 C2 122.0(5) . . ? C6 C1 C2 119.6(5) . . ? C3 C2 C1 117.9(5) . . ? C3 C2 C19 120.3(5) . . ? C1 C2 C19 121.7(5) . . ? C4 C3 C2 124.4(5) . . ? C4 C3 H3 117.8 . . ? C2 C3 H3 117.8 . . ? C3 C4 C5 117.0(5) . . ? C3 C4 C23 124.0(5) . . ? C5 C4 C23 119.0(5) . . ? C4 C5 C6 120.6(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 120.4(5) . . ? C1 C6 C13 120.7(4) . . ? C5 C6 C13 118.7(5) . . ? O2 C7 C12 119.4(4) . . ? O2 C7 C8 122.1(4) . . ? C12 C7 C8 118.4(5) . . ? C9 C8 C7 118.1(5) . . ? C9 C8 C27 120.9(5) . . ? C7 C8 C27 120.9(5) . . ? C8 C9 C10 123.9(5) . . ? C8 C9 H9 118.1 . . ? C10 C9 H9 118.1 . . ? C11 C10 C9 115.9(5) . . ? C11 C10 C31 122.4(5) . . ? C9 C10 C31 121.6(5) . . ? C10 C11 C12 123.2(5) . . ? C10 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C11 C12 C7 120.3(5) . . ? C11 C12 C14 120.6(5) . . ? C7 C12 C14 118.9(4) . . ? N1 C13 C6 117.6(4) . . ? N1 C13 H13A 107.9 . . ? C6 C13 H13A 107.9 . . ? N1 C13 H13B 107.9 . . ? C6 C13 H13B 107.9 . . ? H13A C13 H13B 107.2 . . ? N1 C14 C12 116.4(4) . . ? N1 C14 H14A 108.2 . . ? C12 C14 H14A 108.2 . . ? N1 C14 H14B 108.2 . . ? C12 C14 H14B 108.2 . . ? H14A C14 H14B 107.3 . . ? N1 C15 C16 113.3(4) . . ? N1 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? N1 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N2 C16 C15 113.0(4) . . ? N2 C16 H16A 109.0 . . ? C15 C16 H16A 109.0 . . ? N2 C16 H16B 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C19 C20 107.9(6) . . ? C22 C19 C2 109.6(5) . . ? C20 C19 C2 112.7(5) . . ? C22 C19 C21 109.7(6) . . ? C20 C19 C21 106.6(5) . . ? C2 C19 C21 110.3(5) . . ? 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 . . ? C25 C23 C24 111.7(6) . . ? C25 C23 C4 109.0(5) . . ? C24 C23 C4 111.0(5) . . ? C25 C23 C26 108.7(6) . . ? C24 C23 C26 107.4(6) . . ? C4 C23 C26 109.1(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C30 C27 C8 111.3(5) . . ? C30 C27 C29 110.1(6) . . ? C8 C27 C29 108.4(5) . . ? C30 C27 C28 107.7(5) . . ? C8 C27 C28 111.8(5) . . ? C29 C27 C28 107.6(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33' C31 C34 121.7(10) . . ? C33' C31 C32' 108.0(10) . . ? C34 C31 C32' 84.9(9) . . ? C33' C31 C33 19.2(10) . . ? C34 C31 C33 112.6(10) . . ? C32' C31 C33 126.1(10) . . ? C33' C31 C10 114.2(8) . . ? C34 C31 C10 114.3(7) . . ? C32' C31 C10 108.6(7) . . ? C33 C31 C10 108.7(8) . . ? C33' C31 C32 86.2(9) . . ? C34 C31 C32 108.3(9) . . ? C32' C31 C32 25.9(7) . . ? C33 C31 C32 105.3(9) . . ? C10 C31 C32 106.9(7) . . ? C33' C31 C34' 103.4(9) . . ? C34 C31 C34' 29.8(6) . . ? C32' C31 C34' 113.8(9) . . ? C33 C31 C34' 88.7(9) . . ? C10 C31 C34' 108.9(7) . . ? C32 C31 C34' 134.5(9) . . ? O3 C35 C36 120.7(5) . . ? O3 C35 C40 120.5(5) . . ? C36 C35 C40 118.9(5) . . ? C37 C36 C35 119.9(5) . . ? C37 C36 C41 122.5(5) . . ? C35 C36 C41 117.6(5) . . ? C36 C37 C38 121.9(6) . . ? C36 C37 H37 119.1 . . ? C38 C37 H37 119.1 . . ? C39 C38 C37 118.2(6) . . ? C39 C38 H38 120.9 . . ? C37 C38 H38 120.9 . . ? C38 C39 C40 122.8(6) . . ? C38 C39 H39 118.6 . . ? C40 C39 H39 118.6 . . ? C39 C40 C35 118.4(6) . . ? C39 C40 C44 123.6(6) . . ? C35 C40 C44 118.1(6) . . ? C43 C41 C43' 62.7(9) . . ? C43 C41 C42' 31.9(8) . . ? C43' C41 C42' 93.8(9) . . ? C43 C41 C36 113.0(8) . . ? C43' C41 C36 100.2(7) . . ? C42' C41 C36 116.5(8) . . ? C43 C41 C42 114.2(10) . . ? C43' C41 C42 152.4(9) . . ? C42' C41 C42 83.5(10) . . ? C36 C41 C42 105.5(7) . . ? C46 C44 C40 110.7(7) . . ? C46 C44 C45 108.0(7) . . ? C40 C44 C45 111.9(7) . . ? C46 C44 H44 108.7 . . ? C40 C44 H44 108.7 . . ? C45 C44 H44 108.7 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O4 C47 C48 105.2(7) . . ? O4 C47 H47A 110.7 . . ? C48 C47 H47A 110.7 . . ? O4 C47 H47B 110.7 . . ? C48 C47 H47B 110.7 . . ? H47A C47 H47B 108.8 . . ? C49 C48 C47 105.7(7) . . ? C49 C48 H48A 110.6 . . ? C47 C48 H48A 110.6 . . ? C49 C48 H48B 110.6 . . ? C47 C48 H48B 110.6 . . ? H48A C48 H48B 108.7 . . ? C48 C49 C50 104.5(7) . . ? C48 C49 H49A 110.9 . . ? C50 C49 H49A 110.9 . . ? C48 C49 H49B 110.9 . . ? C50 C49 H49B 110.9 . . ? H49A C49 H49B 108.9 . . ? O4 C50 C49 108.7(7) . . ? O4 C50 H50A 109.9 . . ? C49 C50 H50A 109.9 . . ? O4 C50 H50B 109.9 . . ? C49 C50 H50B 109.9 . . ? H50A C50 H50B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.601 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.109 #===================================================end data_complex2 _database_code_depnum_ccdc_archive 'CCDC 763745' #TrackingRef 'NieKun-dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H79 N2 O4 Sm' _chemical_formula_sum 'C50 H79 N2 O4 Sm' _chemical_formula_weight 922.50 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 15.3534(14) _cell_length_b 16.8680(15) _cell_length_c 19.187(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4968.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 12813 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1948 _exptl_absorpt_coefficient_mu 1.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.460 _exptl_absorpt_correction_T_max 0.788 _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_me 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16070 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.1650 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8999 _reflns_number_gt 6447 _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. Because there are disordered atoms (C32-C34, C42, C43), which caused abnormal bond distances or thermal parameters, constraints are used during refinements. ; _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^)+(0.1290P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0186(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_number_reflns 8999 _refine_ls_number_parameters 454 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1219 _refine_ls_R_factor_gt 0.1032 _refine_ls_wR_factor_ref 0.2768 _refine_ls_wR_factor_gt 0.2604 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.02864(4) 0.87512(4) 0.89215(4) 0.0406(3) Uani 1 1 d . . . O1 O -0.0479(6) 0.9532(5) 0.9584(6) 0.045(3) Uani 1 1 d . . . O2 O 0.1563(7) 0.8330(6) 0.8555(7) 0.051(3) Uani 1 1 d . . . O3 O -0.0630(7) 0.7846(7) 0.8594(7) 0.057(3) Uani 1 1 d . . . O4 O 0.0787(9) 0.8203(7) 1.0033(7) 0.062(3) Uani 1 1 d . . . N1 N 0.1328(7) 0.9967(7) 0.9077(7) 0.041(3) Uani 1 1 d . . . N2 N 0.0137(9) 0.9895(9) 0.7856(9) 0.073(2) Uani 1 1 d D . . C1 C -0.0571(11) 1.0312(8) 0.9775(12) 0.054(5) Uani 1 1 d . . . C2 C -0.1371(9) 1.0657(9) 0.9879(8) 0.042(3) Uani 1 1 d . . . C3 C -0.1387(10) 1.1470(9) 1.0015(10) 0.049(4) Uani 1 1 d . . . H3 H -0.1926 1.1715 1.0105 0.059 Uiso 1 1 calc R . . C4 C -0.0641(13) 1.1928(11) 1.0022(10) 0.061(5) Uani 1 1 d . . . C5 C 0.0109(11) 1.1559(8) 0.9936(8) 0.042(4) Uani 1 1 d . . . H5 H 0.0620 1.1864 0.9963 0.051 Uiso 1 1 calc R . . C6 C 0.0197(11) 1.0752(9) 0.9808(9) 0.046(4) Uani 1 1 d . . . C7 C 0.2327(8) 0.8591(8) 0.8298(9) 0.040(3) Uani 1 1 d . . . C8 C 0.2792(9) 0.8213(9) 0.7758(9) 0.044(4) Uani 1 1 d . . . C9 C 0.3550(10) 0.8571(10) 0.7514(11) 0.058(5) Uani 1 1 d . . . H9 H 0.3850 0.8325 0.7146 0.070 Uiso 1 1 calc R . . C10 C 0.3886(10) 0.9262(10) 0.7780(10) 0.052(4) Uani 1 1 d . A . C11 C 0.3434(9) 0.9619(10) 0.8324(9) 0.046(4) Uani 1 1 d . . . H11 H 0.3665 1.0081 0.8526 0.056 Uiso 1 1 calc R . . C12 C 0.2658(9) 0.9318(9) 0.8577(10) 0.047(4) Uani 1 1 d . . . C13 C 0.1073(9) 1.0374(9) 0.9724(9) 0.044(4) Uani 1 1 d . . . H13A H 0.1508 1.0789 0.9807 0.053 Uiso 1 1 calc R . . H13B H 0.1135 0.9988 1.0103 0.053 Uiso 1 1 calc R . . C14 C 0.2224(9) 0.9685(8) 0.9196(8) 0.039(3) Uani 1 1 d . . . H14A H 0.2214 0.9295 0.9574 0.047 Uiso 1 1 calc R . . H14B H 0.2578 1.0134 0.9353 0.047 Uiso 1 1 calc R . . C15 C 0.1307(13) 1.0545(12) 0.8525(13) 0.073(2) Uani 1 1 d . . . H15A H 0.1731 1.0397 0.8166 0.088 Uiso 1 1 calc R . . H15B H 0.1478 1.1063 0.8712 0.088 Uiso 1 1 calc R . . C16 C 0.0432(12) 1.0608(11) 0.8205(13) 0.073(2) Uani 1 1 d . . . H16A H 0.0011 1.0745 0.8570 0.088 Uiso 1 1 calc R . . H16B H 0.0438 1.1044 0.7867 0.088 Uiso 1 1 calc R . . C17 C -0.0796(11) 1.0054(12) 0.7825(13) 0.073(2) Uani 1 1 d D . . H17A H -0.0926 1.0358 0.7409 0.110 Uiso 1 1 calc R . . H17B H -0.0970 1.0352 0.8234 0.110 Uiso 1 1 calc R . . H17C H -0.1112 0.9556 0.7811 0.110 Uiso 1 1 calc R . . C18 C 0.0512(12) 0.9518(11) 0.7258(11) 0.073(2) Uani 1 1 d D . . H18A H 0.0187 0.9041 0.7149 0.110 Uiso 1 1 calc R . . H18B H 0.1114 0.9381 0.7356 0.110 Uiso 1 1 calc R . . H18C H 0.0490 0.9878 0.6864 0.110 Uiso 1 1 calc R . . C19 C -0.2244(10) 1.0158(10) 0.9899(12) 0.058(5) Uani 1 1 d . . . C20 C -0.3014(11) 1.0659(12) 1.0081(13) 0.070(6) Uani 1 1 d . . . H20A H -0.3511 1.0321 1.0174 0.105 Uiso 1 1 calc R . . H20B H -0.3147 1.1009 0.9694 0.105 Uiso 1 1 calc R . . H20C H -0.2883 1.0972 1.0492 0.105 Uiso 1 1 calc R . . C21 C -0.2402(13) 0.9772(12) 0.9177(14) 0.079(7) Uani 1 1 d . . . H21A H -0.2871 0.9389 0.9212 0.119 Uiso 1 1 calc R . . H21B H -0.1875 0.9506 0.9024 0.119 Uiso 1 1 calc R . . H21C H -0.2558 1.0179 0.8842 0.119 Uiso 1 1 calc R . . C22 C -0.2145(14) 0.9545(11) 1.0468(12) 0.072(6) Uani 1 1 d . . . H22A H -0.2011 0.9808 1.0905 0.108 Uiso 1 1 calc R . . H22B H -0.1676 0.9184 1.0349 0.108 Uiso 1 1 calc R . . H22C H -0.2684 0.9250 1.0516 0.108 Uiso 1 1 calc R . . C23 C -0.0701(19) 1.2832(12) 1.0176(18) 0.098(4) Uani 1 1 d . . . C24 C -0.1562(16) 1.3174(13) 1.0132(17) 0.098(4) Uani 1 1 d . . . H24A H -0.1515 1.3743 1.0067 0.147 Uiso 1 1 calc R . . H24B H -0.1878 1.3066 1.0560 0.147 Uiso 1 1 calc R . . H24C H -0.1872 1.2944 0.9741 0.147 Uiso 1 1 calc R . . C25 C -0.0226(17) 1.2957(12) 1.0858(16) 0.098(4) Uani 1 1 d . . . H25A H -0.0356 1.3482 1.1037 0.147 Uiso 1 1 calc R . . H25B H 0.0396 1.2908 1.0783 0.147 Uiso 1 1 calc R . . H25C H -0.0414 1.2561 1.1193 0.147 Uiso 1 1 calc R . . C26 C -0.0221(18) 1.3267(12) 0.9578(16) 0.098(4) Uani 1 1 d . . . H26A H -0.0322 1.2989 0.9142 0.147 Uiso 1 1 calc R . . H26B H 0.0399 1.3279 0.9675 0.147 Uiso 1 1 calc R . . H26C H -0.0440 1.3805 0.9541 0.147 Uiso 1 1 calc R . . C27 C 0.2502(11) 0.7412(10) 0.7493(11) 0.058(5) Uani 1 1 d . . . C28 C 0.3077(14) 0.7113(13) 0.6854(14) 0.082(7) Uani 1 1 d . . . H28A H 0.2999 0.7469 0.6462 0.123 Uiso 1 1 calc R . . H28B H 0.2896 0.6583 0.6723 0.123 Uiso 1 1 calc R . . H28C H 0.3686 0.7106 0.6989 0.123 Uiso 1 1 calc R . . C29 C 0.2506(13) 0.6786(12) 0.8100(15) 0.084(8) Uani 1 1 d . . . H29A H 0.3100 0.6623 0.8196 0.126 Uiso 1 1 calc R . . H29B H 0.2164 0.6328 0.7964 0.126 Uiso 1 1 calc R . . H29C H 0.2256 0.7021 0.8516 0.126 Uiso 1 1 calc R . . C30 C 0.1569(14) 0.7439(13) 0.7182(12) 0.073(6) Uani 1 1 d . . . H30A H 0.1172 0.7663 0.7523 0.110 Uiso 1 1 calc R . . H30B H 0.1384 0.6906 0.7064 0.110 Uiso 1 1 calc R . . H30C H 0.1569 0.7765 0.6766 0.110 Uiso 1 1 calc R . . C31 C 0.4737(12) 0.9659(8) 0.7504(9) 0.054(4) Uani 1 1 d D . . C32 C 0.539(3) 0.952(8) 0.808(3) 0.100(8) Uani 0.50 1 d PD A 1 C32' C 0.549(3) 0.953(8) 0.799(3) 0.100(8) Uani 0.50 1 d PD A 2 C33 C 0.460(4) 1.0528(16) 0.736(5) 0.100(8) Uani 0.50 1 d PD A 1 C33' C 0.479(4) 1.0556(13) 0.752(5) 0.100(8) Uani 0.50 1 d PD A 2 C34 C 0.517(3) 0.917(2) 0.695(2) 0.100(8) Uani 0.50 1 d PD A 1 C34' C 0.485(3) 0.949(3) 0.6744(14) 0.100(8) Uani 0.50 1 d PD A 2 C35 C -0.1173(9) 0.7216(9) 0.8477(10) 0.049(4) Uani 1 1 d . . . C36 C -0.1152(10) 0.6538(9) 0.8906(11) 0.051(4) Uani 1 1 d . B . C37 C -0.1705(10) 0.5957(10) 0.8838(12) 0.057(5) Uani 1 1 d . . . H37 H -0.1725 0.5547 0.9170 0.068 Uiso 1 1 calc R . . C38 C -0.2294(11) 0.5953(11) 0.8235(11) 0.058(5) Uani 1 1 d . . . H38 H -0.2646 0.5511 0.8135 0.069 Uiso 1 1 calc R . . C39 C -0.2311(10) 0.6572(11) 0.7852(10) 0.054(4) Uani 1 1 d . . . H39 H -0.2721 0.6587 0.7489 0.065 Uiso 1 1 calc R . . C40 C -0.1769(10) 0.7223(11) 0.7930(10) 0.052(4) Uani 1 1 d . D . C41 C -0.0462(11) 0.6531(12) 0.9466(11) 0.070(6) Uani 1 1 d D . . C42 C 0.038(2) 0.635(4) 0.907(3) 0.116(11) Uani 0.50 1 d PD B 1 C42' C 0.042(2) 0.617(4) 0.940(3) 0.116(11) Uani 0.50 1 d PD B 2 C43 C -0.050(3) 0.585(3) 0.996(3) 0.116(11) Uani 0.50 1 d PD B 1 C43' C -0.092(3) 0.677(3) 1.0110(19) 0.116(11) Uani 0.50 1 d PD B 2 C44 C -0.1793(15) 0.7946(18) 0.7461(16) 0.099(5) Uani 1 1 d . . . H44 H -0.1522 0.8371 0.7743 0.118 Uiso 1 1 calc R C 1 C45 C -0.2658(14) 0.8271(16) 0.7259(15) 0.099(5) Uani 1 1 d . D 1 H45A H -0.2588 0.8809 0.7090 0.148 Uiso 1 1 calc R D 1 H45B H -0.3041 0.8271 0.7661 0.148 Uiso 1 1 calc R D 1 H45C H -0.2909 0.7945 0.6894 0.148 Uiso 1 1 calc R D 1 C46 C -0.1215(15) 0.7870(17) 0.6840(15) 0.099(5) Uani 1 1 d . D . H46A H -0.0611 0.7870 0.6988 0.148 Uiso 1 1 calc R . . H46B H -0.1315 0.8312 0.6527 0.148 Uiso 1 1 calc R . . H46C H -0.1342 0.7377 0.6599 0.148 Uiso 1 1 calc R . . C47 C 0.1567(19) 0.7755(14) 1.0202(12) 0.089(4) Uani 1 1 d . . . H47A H 0.2058 0.8109 1.0298 0.107 Uiso 1 1 calc R . . H47B H 0.1726 0.7397 0.9820 0.107 Uiso 1 1 calc R . . C48 C 0.1312(17) 0.7297(13) 1.0842(11) 0.089(4) Uani 1 1 d D . . H48A H 0.1822 0.7224 1.1143 0.107 Uiso 1 1 calc R . . H48B H 0.1094 0.6773 1.0709 0.107 Uiso 1 1 calc R . . C49 C 0.0610(16) 0.7748(13) 1.1233(11) 0.089(4) Uani 1 1 d D . . H49A H 0.0128 0.7399 1.1367 0.107 Uiso 1 1 calc R . . H49B H 0.0845 0.8006 1.1651 0.107 Uiso 1 1 calc R . . C50 C 0.0331(19) 0.8345(13) 1.0701(11) 0.089(4) Uani 1 1 d . . . H50A H -0.0300 0.8307 1.0629 0.107 Uiso 1 1 calc R . . H50B H 0.0463 0.8880 1.0869 0.107 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0415(4) 0.0387(4) 0.0418(4) 0.0028(3) 0.0000(3) -0.0005(3) O1 0.046(6) 0.042(5) 0.047(7) -0.012(5) 0.016(5) 0.005(4) O2 0.044(6) 0.041(5) 0.067(9) 0.005(5) -0.001(5) -0.005(5) O3 0.037(5) 0.060(6) 0.075(10) 0.000(6) -0.004(5) -0.010(5) O4 0.073(8) 0.062(7) 0.052(8) 0.006(6) -0.012(7) 0.010(6) N1 0.036(6) 0.042(6) 0.044(9) 0.000(5) -0.004(5) -0.014(5) N2 0.069(5) 0.063(4) 0.087(7) 0.010(4) -0.024(5) 0.003(4) C1 0.053(9) 0.020(6) 0.088(15) 0.005(7) 0.000(9) -0.010(6) C2 0.042(8) 0.053(8) 0.032(8) -0.007(7) 0.006(6) -0.005(7) C3 0.044(8) 0.044(8) 0.060(12) 0.004(7) 0.001(7) 0.002(7) C4 0.076(12) 0.067(11) 0.041(11) -0.021(9) 0.007(9) 0.003(10) C5 0.053(9) 0.041(7) 0.032(8) -0.005(6) 0.009(7) 0.013(7) C6 0.047(8) 0.043(7) 0.048(9) 0.004(6) -0.003(8) 0.020(8) C7 0.034(6) 0.039(8) 0.048(9) -0.006(6) 0.008(6) -0.003(6) C8 0.040(7) 0.051(8) 0.042(9) -0.003(7) -0.002(7) -0.002(7) C9 0.050(8) 0.061(11) 0.063(12) -0.012(8) -0.001(9) 0.013(8) C10 0.049(9) 0.052(9) 0.055(11) -0.003(8) -0.015(8) 0.008(8) C11 0.038(7) 0.061(9) 0.040(10) 0.010(8) 0.010(7) 0.011(7) C12 0.035(7) 0.046(8) 0.059(11) -0.002(7) 0.000(7) 0.001(7) C13 0.039(7) 0.045(7) 0.048(10) -0.019(7) 0.017(7) -0.007(7) C14 0.039(7) 0.040(7) 0.038(8) 0.007(6) -0.003(6) -0.015(6) C15 0.069(5) 0.063(4) 0.087(7) 0.010(4) -0.024(5) 0.003(4) C16 0.069(5) 0.063(4) 0.087(7) 0.010(4) -0.024(5) 0.003(4) C17 0.069(5) 0.063(4) 0.087(7) 0.010(4) -0.024(5) 0.003(4) C18 0.069(5) 0.063(4) 0.087(7) 0.010(4) -0.024(5) 0.003(4) C19 0.040(8) 0.052(9) 0.082(15) 0.007(9) 0.010(9) -0.011(7) C20 0.040(9) 0.069(11) 0.100(19) -0.004(11) 0.005(9) 0.003(9) C21 0.062(11) 0.071(12) 0.10(2) -0.017(12) 0.025(12) -0.018(10) C22 0.087(13) 0.068(11) 0.060(14) 0.036(10) 0.028(11) -0.002(11) C23 0.104(9) 0.058(6) 0.133(14) -0.008(7) -0.013(9) -0.007(6) C24 0.104(9) 0.058(6) 0.133(14) -0.008(7) -0.013(9) -0.007(6) C25 0.104(9) 0.058(6) 0.133(14) -0.008(7) -0.013(9) -0.007(6) C26 0.104(9) 0.058(6) 0.133(14) -0.008(7) -0.013(9) -0.007(6) C27 0.052(9) 0.055(9) 0.066(13) -0.024(9) 0.021(9) 0.002(8) C28 0.077(13) 0.083(13) 0.085(19) -0.024(13) 0.010(12) -0.013(11) C29 0.061(11) 0.070(12) 0.12(2) 0.011(13) 0.024(13) 0.007(10) C30 0.085(13) 0.088(13) 0.047(12) -0.016(10) -0.006(10) -0.028(12) C31 0.071(10) 0.038(7) 0.054(10) 0.008(7) 0.013(11) 0.002(8) C32 0.053(12) 0.108(11) 0.14(2) 0.043(12) 0.038(12) 0.025(10) C32' 0.053(12) 0.108(11) 0.14(2) 0.043(12) 0.038(12) 0.025(10) C33 0.053(12) 0.108(11) 0.14(2) 0.043(12) 0.038(12) 0.025(10) C33' 0.053(12) 0.108(11) 0.14(2) 0.043(12) 0.038(12) 0.025(10) C34 0.053(12) 0.108(11) 0.14(2) 0.043(12) 0.038(12) 0.025(10) C34' 0.053(12) 0.108(11) 0.14(2) 0.043(12) 0.038(12) 0.025(10) C35 0.036(7) 0.051(8) 0.058(12) -0.017(8) -0.001(7) -0.002(7) C36 0.043(7) 0.057(8) 0.053(10) 0.004(8) -0.004(8) -0.007(7) C37 0.041(8) 0.057(9) 0.073(14) -0.003(9) -0.008(9) -0.006(7) C38 0.051(9) 0.062(10) 0.060(13) -0.016(10) 0.009(9) -0.011(8) C39 0.042(8) 0.078(11) 0.042(10) -0.019(9) -0.007(8) 0.009(8) C40 0.039(7) 0.071(11) 0.045(10) -0.018(8) -0.010(7) 0.008(8) C41 0.055(10) 0.092(13) 0.064(13) -0.016(10) -0.004(9) -0.035(9) C42 0.076(14) 0.14(2) 0.13(3) 0.05(2) -0.035(17) -0.038(16) C42' 0.076(14) 0.14(2) 0.13(3) 0.05(2) -0.035(17) -0.038(16) C43 0.076(14) 0.14(2) 0.13(3) 0.05(2) -0.035(17) -0.038(16) C43' 0.076(14) 0.14(2) 0.13(3) 0.05(2) -0.035(17) -0.038(16) C44 0.077(8) 0.128(12) 0.090(12) 0.039(10) 0.000(8) 0.025(8) C45 0.077(8) 0.128(12) 0.090(12) 0.039(10) 0.000(8) 0.025(8) C46 0.077(8) 0.128(12) 0.090(12) 0.039(10) 0.000(8) 0.025(8) C47 0.139(11) 0.086(7) 0.043(7) 0.022(5) -0.004(7) 0.017(8) C48 0.139(11) 0.086(7) 0.043(7) 0.022(5) -0.004(7) 0.017(8) C49 0.139(11) 0.086(7) 0.043(7) 0.022(5) -0.004(7) 0.017(8) C50 0.139(11) 0.086(7) 0.043(7) 0.022(5) -0.004(7) 0.017(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 O3 2.170(11) . ? Sm1 O1 2.175(9) . ? Sm1 O2 2.200(11) . ? Sm1 O4 2.449(12) . ? Sm1 N1 2.618(11) . ? Sm1 N2 2.820(16) . ? O1 C1 1.373(17) . ? O2 C7 1.347(16) . ? O3 C35 1.368(18) . ? O4 C47 1.45(3) . ? O4 C50 1.48(3) . ? N1 C15 1.44(2) . ? N1 C13 1.471(19) . ? N1 C14 1.472(18) . ? N2 C18 1.433(17) . ? N2 C16 1.45(2) . ? N2 C17 1.458(15) . ? C1 C2 1.37(2) . ? C1 C6 1.39(2) . ? C2 C3 1.40(2) . ? C2 C19 1.58(2) . ? C3 C4 1.38(2) . ? C3 H3 0.9400 . ? C4 C5 1.32(2) . ? C4 C23 1.55(3) . ? C5 C6 1.39(2) . ? C5 H5 0.9400 . ? C6 C13 1.50(2) . ? C7 C8 1.41(2) . ? C7 C12 1.43(2) . ? C8 C9 1.39(2) . ? C8 C27 1.51(2) . ? C9 C10 1.37(2) . ? C9 H9 0.9400 . ? C10 C11 1.39(2) . ? C10 C31 1.56(2) . ? C11 C12 1.38(2) . ? C11 H11 0.9400 . ? C12 C14 1.49(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.48(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.49(2) . ? C19 C22 1.51(2) . ? C19 C21 1.55(3) . ? 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 C24 1.45(3) . ? C23 C25 1.51(4) . ? C23 C26 1.55(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? 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 C30 1.55(3) . ? C27 C29 1.57(3) . ? C27 C28 1.59(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 C34' 1.50(2) . ? C31 C34 1.498(19) . ? C31 C32' 1.51(2) . ? C31 C33 1.505(19) . ? C31 C32 1.51(2) . ? C31 C33' 1.52(2) . ? C35 C40 1.39(2) . ? C35 C36 1.41(2) . ? C36 C37 1.30(2) . ? C36 C41 1.51(2) . ? C37 C38 1.47(3) . ? C37 H37 0.9400 . ? C38 C39 1.28(2) . ? C38 H38 0.9400 . ? C39 C40 1.39(2) . ? C39 H39 0.9400 . ? C40 C44 1.52(3) . ? C41 C43' 1.477(19) . ? C41 C42' 1.488(19) . ? C41 C43 1.494(19) . ? C41 C42 1.53(2) . ? C44 C45 1.49(3) . ? C44 C46 1.49(4) . ? C44 H44 0.9900 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 C48 1.50(3) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 C49 1.518(17) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.50(3) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Sm1 O1 104.2(4) . . ? O3 Sm1 O2 104.9(4) . . ? O1 Sm1 O2 149.7(4) . . ? O3 Sm1 O4 101.0(5) . . ? O1 Sm1 O4 83.7(4) . . ? O2 Sm1 O4 82.9(5) . . ? O3 Sm1 N1 168.7(4) . . ? O1 Sm1 N1 77.8(4) . . ? O2 Sm1 N1 75.2(4) . . ? O4 Sm1 N1 90.2(4) . . ? O3 Sm1 N2 102.6(5) . . ? O1 Sm1 N2 88.0(5) . . ? O2 Sm1 N2 93.5(4) . . ? O4 Sm1 N2 156.2(4) . . ? N1 Sm1 N2 66.2(4) . . ? C1 O1 Sm1 142.4(10) . . ? C7 O2 Sm1 142.0(8) . . ? C35 O3 Sm1 171.3(12) . . ? C47 O4 C50 106.4(16) . . ? C47 O4 Sm1 130.5(12) . . ? C50 O4 Sm1 123.0(11) . . ? C15 N1 C13 107.3(14) . . ? C15 N1 C14 110.7(13) . . ? C13 N1 C14 105.6(12) . . ? C15 N1 Sm1 115.6(10) . . ? C13 N1 Sm1 107.4(8) . . ? C14 N1 Sm1 109.6(8) . . ? C18 N2 C16 127.8(17) . . ? C18 N2 C17 116.3(18) . . ? C16 N2 C17 100.0(15) . . ? C18 N2 Sm1 104.2(11) . . ? C16 N2 Sm1 102.0(12) . . ? C17 N2 Sm1 103.6(12) . . ? O1 C1 C2 122.4(14) . . ? O1 C1 C6 115.8(14) . . ? C2 C1 C6 121.6(12) . . ? C1 C2 C3 117.3(14) . . ? C1 C2 C19 122.4(13) . . ? C3 C2 C19 120.2(14) . . ? C4 C3 C2 122.4(15) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C5 C4 C3 117.3(15) . . ? C5 C4 C23 122.5(19) . . ? C3 C4 C23 120.1(18) . . ? C4 C5 C6 124.7(17) . . ? C4 C5 H5 117.6 . . ? C6 C5 H5 117.6 . . ? C5 C6 C1 116.5(15) . . ? C5 C6 C13 121.6(16) . . ? C1 C6 C13 121.9(12) . . ? O2 C7 C8 124.2(13) . . ? O2 C7 C12 116.9(13) . . ? C8 C7 C12 118.9(12) . . ? C9 C8 C7 118.3(14) . . ? C9 C8 C27 121.4(15) . . ? C7 C8 C27 120.2(13) . . ? C10 C9 C8 123.9(17) . . ? C10 C9 H9 118.0 . . ? C8 C9 H9 118.0 . . ? C9 C10 C11 117.3(17) . . ? C9 C10 C31 123.6(16) . . ? C11 C10 C31 119.1(14) . . ? C12 C11 C10 122.4(16) . . ? C12 C11 H11 118.8 . . ? C10 C11 H11 118.8 . . ? C11 C12 C7 119.2(15) . . ? C11 C12 C14 120.8(14) . . ? C7 C12 C14 119.6(13) . . ? N1 C13 C6 122.0(15) . . ? N1 C13 H13A 106.8 . . ? C6 C13 H13A 106.8 . . ? N1 C13 H13B 106.8 . . ? C6 C13 H13B 106.8 . . ? H13A C13 H13B 106.7 . . ? N1 C14 C12 115.3(13) . . ? N1 C14 H14A 108.5 . . ? C12 C14 H14A 108.5 . . ? N1 C14 H14B 108.5 . . ? C12 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? N1 C15 C16 112.0(17) . . ? N1 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N1 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? N2 C16 C15 114.5(17) . . ? N2 C16 H16A 108.6 . . ? C15 C16 H16A 108.6 . . ? N2 C16 H16B 108.6 . . ? C15 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C22 107.4(17) . . ? C20 C19 C21 108.8(17) . . ? C22 C19 C21 112.0(16) . . ? C20 C19 C2 112.0(14) . . ? C22 C19 C2 107.3(16) . . ? C21 C19 C2 109.5(15) . . ? 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 . . ? C24 C23 C25 116(3) . . ? C24 C23 C26 102(2) . . ? C25 C23 C26 110(2) . . ? C24 C23 C4 116(2) . . ? C25 C23 C4 106(2) . . ? C26 C23 C4 107(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C27 C30 112.0(15) . . ? C8 C27 C29 110.5(18) . . ? C30 C27 C29 107.9(16) . . ? C8 C27 C28 112.3(15) . . ? C30 C27 C28 103.0(17) . . ? C29 C27 C28 110.9(16) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C34' C31 C34 32(2) . . ? C34' C31 C32' 119(4) . . ? C34 C31 C32' 91(5) . . ? C34' C31 C33 92(4) . . ? C34 C31 C33 118(4) . . ? C32' C31 C33 111(6) . . ? C34' C31 C32 127(4) . . ? C34 C31 C32 98(5) . . ? C32' C31 C32 9(5) . . ? C33 C31 C32 112(6) . . ? C34' C31 C33' 102(4) . . ? C34 C31 C33' 123(4) . . ? C32' C31 C33' 95(6) . . ? C33 C31 C33' 16(5) . . ? C32 C31 C33' 96(6) . . ? C34' C31 C10 110(2) . . ? C34 C31 C10 112(2) . . ? C32' C31 C10 112(3) . . ? C33 C31 C10 111(3) . . ? C32 C31 C10 104(3) . . ? C33' C31 C10 118(3) . . ? O3 C35 C40 121.1(16) . . ? O3 C35 C36 121.4(15) . . ? C40 C35 C36 117.5(15) . . ? C37 C36 C35 122.5(17) . . ? C37 C36 C41 121.5(17) . . ? C35 C36 C41 116.0(14) . . ? C36 C37 C38 118.9(18) . . ? C36 C37 H37 120.6 . . ? C38 C37 H37 120.6 . . ? C39 C38 C37 117.5(16) . . ? C39 C38 H38 121.2 . . ? C37 C38 H38 121.2 . . ? C38 C39 C40 125.0(17) . . ? C38 C39 H39 117.5 . . ? C40 C39 H39 117.5 . . ? C39 C40 C35 118.0(18) . . ? C39 C40 C44 123.9(18) . . ? C35 C40 C44 118.0(18) . . ? C43' C41 C42' 128(3) . . ? C43' C41 C43 70(4) . . ? C42' C41 C43 77(3) . . ? C43' C41 C36 105(2) . . ? C42' C41 C36 125(3) . . ? C43 C41 C36 115(2) . . ? C43' C41 C42 151(3) . . ? C42' C41 C42 27(3) . . ? C43 C41 C42 101(3) . . ? C36 C41 C42 104(3) . . ? C45 C44 C46 111(2) . . ? C45 C44 C40 118(2) . . ? C46 C44 C40 113(2) . . ? C45 C44 H44 104.4 . . ? C46 C44 H44 104.4 . . ? C40 C44 H44 104.4 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O4 C47 C48 104(2) . . ? O4 C47 H47A 111.0 . . ? C48 C47 H47A 111.0 . . ? O4 C47 H47B 111.0 . . ? C48 C47 H47B 111.0 . . ? H47A C47 H47B 109.0 . . ? C47 C48 C49 109.4(18) . . ? C47 C48 H48A 109.8 . . ? C49 C48 H48A 109.8 . . ? C47 C48 H48B 109.8 . . ? C49 C48 H48B 109.8 . . ? H48A C48 H48B 108.3 . . ? C50 C49 C48 101.8(18) . . ? C50 C49 H49A 111.4 . . ? C48 C49 H49A 111.4 . . ? C50 C49 H49B 111.4 . . ? C48 C49 H49B 111.4 . . ? H49A C49 H49B 109.3 . . ? O4 C50 C49 110.2(18) . . ? O4 C50 H50A 109.6 . . ? C49 C50 H50A 109.6 . . ? O4 C50 H50B 109.6 . . ? C49 C50 H50B 109.6 . . ? H50A C50 H50B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.391 _refine_diff_density_min -1.202 _refine_diff_density_rms 0.180 #===================================================end data_complex3 _database_code_depnum_ccdc_archive 'CCDC 763746' #TrackingRef 'NieKun-dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sy _chemical_melting_point ? _chemical_formula_moiety 'C50 H79 N2 O4 Yb' _chemical_formula_sum 'C50 H79 N2 O4 Yb' _chemical_formula_weight 945.19 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 15.604(3) _cell_length_b 16.456(3) _cell_length_c 19.273(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4948.9(15) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10382 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1980 _exptl_absorpt_coefficient_mu 1.931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.469 _exptl_absorpt_correction_T_max 0.680 _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 14662 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0921 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8865 _reflns_number_gt 8018 _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. Because there are disordered atoms (C32-C34, C42, C43), which caused abnormal bond distances or thermal parameters, constraints are used during refinements. ; _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^)+(0.0431P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(14) _refine_ls_number_reflns 8865 _refine_ls_number_parameters 478 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.04422(2) 0.87562(2) 0.889193(14) 0.02564(9) Uani 1 1 d . . . O1 O -0.0369(4) 0.9488(3) 0.9493(2) 0.0314(12) Uani 1 1 d . . . O2 O 0.1636(3) 0.8278(3) 0.8563(2) 0.0309(12) Uani 1 1 d . . . O3 O -0.0426(4) 0.7895(3) 0.8525(3) 0.0360(12) Uani 1 1 d . . . O4 O 0.0810(4) 0.8218(3) 0.9986(2) 0.0359(13) Uani 1 1 d . . . N1 N 0.1387(4) 0.9963(4) 0.9141(3) 0.0290(15) Uani 1 1 d . . . N2 N 0.0407(6) 0.9691(4) 0.7870(3) 0.0422(17) Uani 1 1 d . . . C1 C -0.0430(7) 1.0269(5) 0.9722(4) 0.0336(18) Uani 1 1 d . . . C2 C -0.1291(6) 1.0617(5) 0.9810(4) 0.0302(17) Uani 1 1 d . . . C3 C -0.1338(6) 1.1432(5) 0.9991(4) 0.036(2) Uani 1 1 d . . . H3 H -0.1881 1.1667 1.0058 0.043 Uiso 1 1 calc R . . C4 C -0.0599(5) 1.1925(5) 1.0080(4) 0.0303(18) Uani 1 1 d . . . C5 C 0.0196(6) 1.1543(5) 1.0016(4) 0.034(2) Uani 1 1 d . . . H5 H 0.0697 1.1846 1.0092 0.041 Uiso 1 1 calc R . . C6 C 0.0265(5) 1.0726(5) 0.9841(4) 0.031(2) Uani 1 1 d . . . C7 C 0.2389(5) 0.8553(4) 0.8331(4) 0.0306(18) Uani 1 1 d . . . C8 C 0.2872(5) 0.8141(5) 0.7792(4) 0.0317(18) Uani 1 1 d . . . C9 C 0.3600(6) 0.8528(5) 0.7559(4) 0.036(2) Uani 1 1 d . . . H9 H 0.3911 0.8267 0.7206 0.044 Uiso 1 1 calc R . . C10 C 0.3921(6) 0.9269(5) 0.7797(4) 0.036(2) Uani 1 1 d . A . C11 C 0.3470(6) 0.9609(5) 0.8339(4) 0.039(2) Uani 1 1 d . . . H11 H 0.3684 1.0088 0.8540 0.047 Uiso 1 1 calc R . . C12 C 0.2731(5) 0.9289(5) 0.8604(4) 0.0306(18) Uani 1 1 d . . . C13 C 0.1152(6) 1.0323(5) 0.9818(4) 0.034(2) Uani 1 1 d . . . H13A H 0.1584 1.0730 0.9941 0.041 Uiso 1 1 calc R . . H13B H 0.1171 0.9895 1.0171 0.041 Uiso 1 1 calc R . . C14 C 0.2285(5) 0.9667(5) 0.9239(4) 0.0318(18) Uani 1 1 d . . . H14A H 0.2282 0.9262 0.9612 0.038 Uiso 1 1 calc R . . H14B H 0.2634 1.0126 0.9399 0.038 Uiso 1 1 calc R . . C15 C 0.1343(6) 1.0588(5) 0.8577(4) 0.0364(19) Uani 1 1 d . . . H15A H 0.0887 1.0977 0.8688 0.044 Uiso 1 1 calc R . . H15B H 0.1886 1.0888 0.8564 0.044 Uiso 1 1 calc R . . C16 C 0.1178(7) 1.0241(7) 0.7890(4) 0.051(3) Uani 1 1 d . . . H16A H 0.1684 0.9933 0.7742 0.061 Uiso 1 1 calc R . . H16B H 0.1094 1.0685 0.7557 0.061 Uiso 1 1 calc R . . C17 C -0.0381(8) 1.0172(6) 0.7870(4) 0.057(3) Uani 1 1 d . . . H17A H -0.0396 1.0513 0.8281 0.085 Uiso 1 1 calc R . . H17B H -0.0873 0.9811 0.7872 0.085 Uiso 1 1 calc R . . H17C H -0.0398 1.0511 0.7459 0.085 Uiso 1 1 calc R . . C18 C 0.0494(8) 0.9240(6) 0.7226(4) 0.056(3) Uani 1 1 d . . . H18A H 0.0592 0.9615 0.6846 0.085 Uiso 1 1 calc R . . H18B H -0.0027 0.8934 0.7140 0.085 Uiso 1 1 calc R . . H18C H 0.0974 0.8868 0.7262 0.085 Uiso 1 1 calc R . . C19 C -0.2103(5) 1.0096(5) 0.9754(5) 0.038(2) Uani 1 1 d . . . C20 C -0.2915(6) 1.0592(6) 0.9909(5) 0.053(3) Uani 1 1 d . . . H20A H -0.2886 1.0803 1.0379 0.080 Uiso 1 1 calc R . . H20B H -0.3415 1.0245 0.9863 0.080 Uiso 1 1 calc R . . H20C H -0.2957 1.1040 0.9584 0.080 Uiso 1 1 calc R . . C21 C -0.2213(6) 0.9764(5) 0.9000(5) 0.048(2) Uani 1 1 d . . . H21A H -0.2141 1.0205 0.8671 0.072 Uiso 1 1 calc R . . H21B H -0.2781 0.9532 0.8948 0.072 Uiso 1 1 calc R . . H21C H -0.1785 0.9349 0.8911 0.072 Uiso 1 1 calc R . . C22 C -0.2038(6) 0.9394(5) 1.0281(5) 0.048(2) Uani 1 1 d . . . H22A H -0.1492 0.9120 1.0225 0.072 Uiso 1 1 calc R . . H22B H -0.2500 0.9011 1.0200 0.072 Uiso 1 1 calc R . . H22C H -0.2082 0.9608 1.0748 0.072 Uiso 1 1 calc R . . C23 C -0.0718(10) 1.2814(6) 1.0261(6) 0.079(2) Uani 1 1 d . . . C24 C -0.1183(9) 1.3262(6) 0.9706(6) 0.079(2) Uani 1 1 d . . . H24A H -0.1697 1.2966 0.9580 0.119 Uiso 1 1 calc R . . H24B H -0.0816 1.3315 0.9302 0.119 Uiso 1 1 calc R . . H24C H -0.1339 1.3798 0.9873 0.119 Uiso 1 1 calc R . . C25 C -0.1175(9) 1.2909(6) 1.0926(6) 0.079(2) Uani 1 1 d . . . H25A H -0.0766 1.2891 1.1305 0.119 Uiso 1 1 calc R . . H25B H -0.1587 1.2473 1.0979 0.119 Uiso 1 1 calc R . . H25C H -0.1472 1.3427 1.0932 0.119 Uiso 1 1 calc R . . C26 C 0.0105(9) 1.3252(6) 1.0360(6) 0.079(2) Uani 1 1 d . . . H26A H 0.0001 1.3833 1.0357 0.119 Uiso 1 1 calc R . . H26B H 0.0495 1.3113 0.9987 0.119 Uiso 1 1 calc R . . H26C H 0.0355 1.3096 1.0801 0.119 Uiso 1 1 calc R . . C27 C 0.2609(6) 0.7312(5) 0.7535(4) 0.039(2) Uani 1 1 d . . . C28 C 0.3208(8) 0.6985(6) 0.6982(5) 0.068(3) Uani 1 1 d . . . H28A H 0.3164 0.7317 0.6568 0.102 Uiso 1 1 calc R . . H28B H 0.3051 0.6429 0.6871 0.102 Uiso 1 1 calc R . . H28C H 0.3793 0.6998 0.7153 0.102 Uiso 1 1 calc R . . C29 C 0.2639(7) 0.6714(5) 0.8150(4) 0.057(3) Uani 1 1 d . . . H29A H 0.2432 0.6186 0.8002 0.085 Uiso 1 1 calc R . . H29B H 0.2280 0.6916 0.8523 0.085 Uiso 1 1 calc R . . H29C H 0.3225 0.6664 0.8314 0.085 Uiso 1 1 calc R . . C30 C 0.1698(7) 0.7298(6) 0.7214(5) 0.060(3) Uani 1 1 d . . . H30A H 0.1673 0.7677 0.6829 0.090 Uiso 1 1 calc R . . H30B H 0.1282 0.7455 0.7563 0.090 Uiso 1 1 calc R . . H30C H 0.1569 0.6755 0.7050 0.090 Uiso 1 1 calc R . . C31 C 0.4768(5) 0.9656(5) 0.7523(4) 0.043(2) Uani 1 1 d D . . C32 C 0.5348(14) 0.9712(17) 0.8163(9) 0.068(3) Uani 0.50 1 d PD A 1 C32' C 0.5508(13) 0.9534(17) 0.8010(10) 0.068(3) Uani 0.50 1 d PD A 2 C33 C 0.4656(18) 1.0495(11) 0.7219(10) 0.068(3) Uani 0.50 1 d PD A 1 C33' C 0.4611(18) 1.0581(10) 0.7503(11) 0.068(3) Uani 0.50 1 d PD A 2 C34 C 0.5232(14) 0.9097(11) 0.7001(10) 0.068(3) Uani 0.50 1 d PD A 1 C34' C 0.4876(14) 0.9472(13) 0.6753(8) 0.068(3) Uani 0.50 1 d PD A 2 C35 C -0.1063(5) 0.7336(5) 0.8459(4) 0.039(2) Uani 1 1 d . . . C36 C -0.1094(5) 0.6638(5) 0.8896(4) 0.0379(18) Uani 1 1 d . B . C37 C -0.1738(5) 0.6087(5) 0.8816(4) 0.046(2) Uani 1 1 d . . . H37 H -0.1767 0.5632 0.9110 0.055 Uiso 1 1 calc R . . C38 C -0.2355(5) 0.6191(8) 0.8300(5) 0.059(3) Uani 1 1 d . . . H38 H -0.2793 0.5803 0.8246 0.071 Uiso 1 1 calc R . . C39 C -0.2329(6) 0.6845(6) 0.7877(5) 0.051(3) Uani 1 1 d . . . H39 H -0.2757 0.6907 0.7538 0.061 Uiso 1 1 calc R . . C40 C -0.1693(6) 0.7424(6) 0.7929(4) 0.042(2) Uani 1 1 d . D . C41 C -0.0362(7) 0.6485(5) 0.9413(4) 0.048(2) Uani 1 1 d D . . C42 C 0.0428(10) 0.6154(12) 0.9066(8) 0.054(3) Uani 0.50 1 d PD B 1 C42' C -0.0516(13) 0.5900(13) 1.0028(11) 0.054(3) Uani 0.50 1 d PD B 2 C43 C -0.0794(11) 0.6123(15) 1.0060(10) 0.054(3) Uani 0.50 1 d PD B 1 C43' C -0.0607(12) 0.7322(10) 0.9662(10) 0.054(3) Uani 0.50 1 d PD B 2 C44 C -0.1639(7) 0.8143(7) 0.7435(5) 0.0608(16) Uani 1 1 d . . . H44 H -0.1242 0.8548 0.7637 0.073 Uiso 1 1 calc R C 1 C45 C -0.2502(7) 0.8547(6) 0.7336(5) 0.0608(16) Uani 1 1 d . D 1 H45A H -0.2910 0.8151 0.7164 0.091 Uiso 1 1 calc R D 1 H45B H -0.2448 0.8987 0.7004 0.091 Uiso 1 1 calc R D 1 H45C H -0.2700 0.8761 0.7776 0.091 Uiso 1 1 calc R D 1 C46 C -0.1275(7) 0.7872(6) 0.6719(5) 0.0608(16) Uani 1 1 d . D . H46A H -0.0739 0.7584 0.6788 0.091 Uiso 1 1 calc R . . H46B H -0.1175 0.8346 0.6432 0.091 Uiso 1 1 calc R . . H46C H -0.1683 0.7516 0.6492 0.091 Uiso 1 1 calc R . . C47 C 0.1579(7) 0.7764(6) 1.0171(4) 0.0506(13) Uani 1 1 d . . . H47A H 0.2034 0.8131 1.0326 0.061 Uiso 1 1 calc R . . H47B H 0.1789 0.7449 0.9774 0.061 Uiso 1 1 calc R . . C48 C 0.1298(7) 0.7210(6) 1.0752(4) 0.0506(13) Uani 1 1 d . . . H48A H 0.1775 0.7091 1.1067 0.061 Uiso 1 1 calc R . . H48B H 0.1069 0.6698 1.0571 0.061 Uiso 1 1 calc R . . C49 C 0.0602(6) 0.7700(5) 1.1119(4) 0.0506(13) Uani 1 1 d . . . H49A H 0.0141 0.7341 1.1277 0.061 Uiso 1 1 calc R . . H49B H 0.0841 0.7982 1.1523 0.061 Uiso 1 1 calc R . . C50 C 0.0266(7) 0.8300(6) 1.0606(4) 0.0506(13) Uani 1 1 d . . . H50A H -0.0334 0.8181 1.0492 0.061 Uiso 1 1 calc R . . H50B H 0.0301 0.8853 1.0792 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02518(14) 0.02422(14) 0.02751(14) 0.00022(15) 0.00005(13) -0.00141(17) O1 0.032(3) 0.023(2) 0.040(3) -0.003(2) 0.004(3) -0.001(3) O2 0.024(3) 0.032(3) 0.037(3) -0.008(2) 0.009(2) 0.002(3) O3 0.032(3) 0.032(3) 0.044(3) 0.002(2) -0.006(3) 0.001(3) O4 0.040(3) 0.044(3) 0.024(2) 0.003(3) 0.000(2) 0.005(3) N1 0.025(3) 0.029(3) 0.033(3) 0.001(3) 0.005(3) 0.005(3) N2 0.057(5) 0.040(4) 0.030(3) 0.008(3) -0.007(4) -0.012(5) C1 0.034(4) 0.033(4) 0.034(4) 0.001(3) -0.003(4) 0.007(5) C2 0.025(4) 0.035(4) 0.030(4) 0.001(4) 0.006(3) -0.006(4) C3 0.029(4) 0.039(5) 0.039(4) -0.001(4) 0.009(4) 0.002(4) C4 0.029(5) 0.031(4) 0.031(4) -0.004(3) 0.006(3) -0.003(4) C5 0.036(5) 0.032(4) 0.035(4) -0.007(4) 0.008(4) -0.007(4) C6 0.024(5) 0.034(4) 0.035(4) -0.008(4) 0.002(3) -0.002(4) C7 0.030(4) 0.029(4) 0.033(3) -0.002(3) 0.001(3) -0.002(4) C8 0.029(4) 0.031(4) 0.035(4) -0.002(4) 0.000(3) 0.008(4) C9 0.037(5) 0.048(5) 0.024(3) -0.009(4) 0.007(3) 0.009(4) C10 0.028(5) 0.038(5) 0.041(4) 0.001(4) 0.006(4) 0.006(4) C11 0.039(5) 0.037(5) 0.041(4) -0.009(4) 0.004(4) -0.016(4) C12 0.030(4) 0.028(4) 0.034(4) -0.006(3) 0.003(3) 0.005(4) C13 0.038(5) 0.031(4) 0.032(4) -0.011(4) -0.007(4) -0.010(4) C14 0.025(4) 0.035(4) 0.035(4) 0.000(4) -0.001(3) -0.007(4) C15 0.030(4) 0.028(4) 0.051(4) -0.002(4) 0.010(4) 0.002(4) C16 0.042(6) 0.066(7) 0.043(5) 0.019(5) 0.001(4) 0.017(6) C17 0.075(8) 0.048(5) 0.047(5) 0.016(4) 0.013(6) 0.022(7) C18 0.063(7) 0.066(6) 0.040(4) 0.000(5) 0.004(5) 0.016(7) C19 0.017(4) 0.034(5) 0.061(5) 0.001(4) 0.003(4) 0.006(4) C20 0.026(5) 0.047(6) 0.087(7) -0.001(5) 0.010(5) -0.006(5) C21 0.033(5) 0.040(5) 0.070(6) -0.001(5) -0.018(5) -0.009(4) C22 0.037(5) 0.039(5) 0.069(6) 0.015(5) 0.011(5) 0.001(5) C23 0.106(6) 0.036(3) 0.095(4) -0.011(3) 0.002(4) 0.014(3) C24 0.106(6) 0.036(3) 0.095(4) -0.011(3) 0.002(4) 0.014(3) C25 0.106(6) 0.036(3) 0.095(4) -0.011(3) 0.002(4) 0.014(3) C26 0.106(6) 0.036(3) 0.095(4) -0.011(3) 0.002(4) 0.014(3) C27 0.039(5) 0.034(5) 0.045(5) -0.013(4) 0.007(4) 0.004(4) C28 0.085(9) 0.048(6) 0.070(6) -0.019(5) 0.033(7) -0.005(7) C29 0.069(7) 0.042(5) 0.060(6) -0.004(5) 0.009(5) -0.004(6) C30 0.052(6) 0.050(6) 0.077(7) -0.018(6) -0.001(6) -0.007(6) C31 0.031(5) 0.057(6) 0.040(4) 0.006(4) 0.011(4) -0.010(5) C32 0.051(5) 0.075(6) 0.077(7) 0.022(5) 0.032(6) -0.007(5) C32' 0.051(5) 0.075(6) 0.077(7) 0.022(5) 0.032(6) -0.007(5) C33 0.051(5) 0.075(6) 0.077(7) 0.022(5) 0.032(6) -0.007(5) C33' 0.051(5) 0.075(6) 0.077(7) 0.022(5) 0.032(6) -0.007(5) C34 0.051(5) 0.075(6) 0.077(7) 0.022(5) 0.032(6) -0.007(5) C34' 0.051(5) 0.075(6) 0.077(7) 0.022(5) 0.032(6) -0.007(5) C35 0.019(4) 0.042(5) 0.056(5) -0.019(4) -0.001(4) -0.005(4) C36 0.034(4) 0.044(4) 0.036(4) -0.012(4) 0.009(4) -0.008(4) C37 0.035(4) 0.048(6) 0.055(5) -0.022(5) 0.019(4) -0.009(4) C38 0.023(4) 0.084(8) 0.070(6) -0.035(7) 0.006(4) -0.016(6) C39 0.023(5) 0.055(6) 0.075(6) -0.020(6) -0.013(5) -0.004(5) C40 0.034(5) 0.044(5) 0.047(5) -0.016(4) -0.004(4) 0.007(5) C41 0.063(6) 0.045(5) 0.037(4) 0.006(4) -0.012(5) -0.026(5) C42 0.031(6) 0.067(7) 0.064(5) 0.021(5) -0.023(5) 0.003(6) C42' 0.031(6) 0.067(7) 0.064(5) 0.021(5) -0.023(5) 0.003(6) C43 0.031(6) 0.067(7) 0.064(5) 0.021(5) -0.023(5) 0.003(6) C43' 0.031(6) 0.067(7) 0.064(5) 0.021(5) -0.023(5) 0.003(6) C44 0.054(4) 0.059(4) 0.070(3) -0.011(3) -0.017(3) 0.014(3) C45 0.054(4) 0.059(4) 0.070(3) -0.011(3) -0.017(3) 0.014(3) C46 0.054(4) 0.059(4) 0.070(3) -0.011(3) -0.017(3) 0.014(3) C47 0.066(4) 0.049(3) 0.036(2) 0.004(2) -0.007(2) 0.013(3) C48 0.066(4) 0.049(3) 0.036(2) 0.004(2) -0.007(2) 0.013(3) C49 0.066(4) 0.049(3) 0.036(2) 0.004(2) -0.007(2) 0.013(3) C50 0.066(4) 0.049(3) 0.036(2) 0.004(2) -0.007(2) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O3 2.084(6) . ? Yb1 O1 2.096(5) . ? Yb1 O2 2.120(5) . ? Yb1 O4 2.358(5) . ? Yb1 N2 2.500(6) . ? Yb1 N1 2.519(7) . ? O1 C1 1.363(9) . ? O2 C7 1.336(9) . ? O3 C35 1.360(9) . ? O4 C47 1.458(11) . ? O4 C50 1.471(10) . ? N1 C13 1.479(9) . ? N1 C14 1.495(10) . ? N1 C15 1.498(9) . ? N2 C18 1.452(10) . ? N2 C17 1.463(13) . ? N2 C16 1.508(13) . ? C1 C6 1.339(12) . ? C1 C2 1.472(13) . ? C2 C3 1.388(11) . ? C2 C19 1.532(11) . ? C3 C4 1.421(11) . ? C3 H3 0.9400 . ? C4 C5 1.395(12) . ? C4 C23 1.516(12) . ? C5 C6 1.390(11) . ? C5 H5 0.9400 . ? C6 C13 1.536(12) . ? C7 C12 1.424(10) . ? C7 C8 1.452(10) . ? C8 C9 1.377(11) . ? C8 C27 1.509(11) . ? C9 C10 1.396(11) . ? C9 H9 0.9400 . ? C10 C11 1.378(11) . ? C10 C31 1.558(11) . ? C11 C12 1.367(11) . ? C11 H11 0.9400 . ? C12 C14 1.540(10) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.465(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.537(12) . ? C19 C22 1.541(11) . ? C19 C21 1.563(12) . ? 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 C25 1.475(16) . ? C23 C26 1.485(17) . ? C23 C24 1.488(15) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? 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 C28 1.517(12) . ? C27 C29 1.542(12) . ? C27 C30 1.549(13) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 C32' 1.501(16) . ? C31 C33 1.510(15) . ? C31 C34' 1.524(14) . ? C31 C32 1.532(16) . ? C31 C33' 1.542(16) . ? C31 C34 1.544(15) . ? C35 C36 1.425(12) . ? C35 C40 1.426(11) . ? C36 C37 1.363(11) . ? C36 C41 1.537(12) . ? C37 C38 1.394(12) . ? C37 H37 0.9400 . ? C38 C39 1.351(14) . ? C38 H38 0.9400 . ? C39 C40 1.380(12) . ? C39 H39 0.9400 . ? C40 C44 1.521(13) . ? C41 C42 1.505(15) . ? C41 C43' 1.507(15) . ? C41 C43 1.537(16) . ? C41 C42' 1.546(15) . ? C44 C45 1.512(13) . ? C44 C46 1.558(13) . ? C44 H44 0.9900 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 C48 1.510(12) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 C49 1.526(12) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.492(10) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Yb1 O1 100.7(2) . . ? O3 Yb1 O2 102.6(2) . . ? O1 Yb1 O2 155.4(2) . . ? O3 Yb1 O4 101.9(2) . . ? O1 Yb1 O4 82.43(19) . . ? O2 Yb1 O4 85.09(19) . . ? O3 Yb1 N2 97.8(2) . . ? O1 Yb1 N2 94.0(2) . . ? O2 Yb1 N2 90.7(3) . . ? O4 Yb1 N2 160.3(2) . . ? O3 Yb1 N1 168.76(19) . . ? O1 Yb1 N1 78.2(2) . . ? O2 Yb1 N1 80.5(2) . . ? O4 Yb1 N1 89.1(2) . . ? N2 Yb1 N1 71.2(2) . . ? C1 O1 Yb1 139.7(6) . . ? C7 O2 Yb1 138.3(5) . . ? C35 O3 Yb1 165.1(5) . . ? C47 O4 C50 108.9(6) . . ? C47 O4 Yb1 127.7(5) . . ? C50 O4 Yb1 123.4(5) . . ? C13 N1 C14 104.5(6) . . ? C13 N1 C15 110.6(6) . . ? C14 N1 C15 111.0(6) . . ? C13 N1 Yb1 109.8(5) . . ? C14 N1 Yb1 108.4(5) . . ? C15 N1 Yb1 112.1(5) . . ? C18 N2 C17 110.8(8) . . ? C18 N2 C16 104.7(8) . . ? C17 N2 C16 110.3(7) . . ? C18 N2 Yb1 110.9(5) . . ? C17 N2 Yb1 110.6(5) . . ? C16 N2 Yb1 109.4(5) . . ? C6 C1 O1 122.0(9) . . ? C6 C1 C2 120.1(7) . . ? O1 C1 C2 117.9(9) . . ? C3 C2 C1 116.9(8) . . ? C3 C2 C19 121.0(8) . . ? C1 C2 C19 122.0(7) . . ? C2 C3 C4 122.6(8) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C5 C4 C3 117.0(7) . . ? C5 C4 C23 124.4(9) . . ? C3 C4 C23 118.6(9) . . ? C6 C5 C4 121.7(8) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C1 C6 C5 121.5(8) . . ? C1 C6 C13 118.7(7) . . ? C5 C6 C13 119.7(8) . . ? O2 C7 C12 119.6(7) . . ? O2 C7 C8 122.6(7) . . ? C12 C7 C8 117.8(7) . . ? C9 C8 C7 116.5(7) . . ? C9 C8 C27 122.4(7) . . ? C7 C8 C27 121.0(7) . . ? C8 C9 C10 126.4(7) . . ? C8 C9 H9 116.8 . . ? C10 C9 H9 116.8 . . ? C11 C10 C9 114.8(8) . . ? C11 C10 C31 121.6(8) . . ? C9 C10 C31 123.4(7) . . ? C12 C11 C10 123.9(8) . . ? C12 C11 H11 118.0 . . ? C10 C11 H11 118.0 . . ? C11 C12 C7 120.4(7) . . ? C11 C12 C14 121.4(7) . . ? C7 C12 C14 118.0(7) . . ? N1 C13 C6 115.0(6) . . ? N1 C13 H13A 108.5 . . ? C6 C13 H13A 108.5 . . ? N1 C13 H13B 108.5 . . ? C6 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? N1 C14 C12 117.0(6) . . ? N1 C14 H14A 108.1 . . ? C12 C14 H14A 108.1 . . ? N1 C14 H14B 108.1 . . ? C12 C14 H14B 108.1 . . ? H14A C14 H14B 107.3 . . ? C16 C15 N1 113.3(7) . . ? C16 C15 H15A 108.9 . . ? N1 C15 H15A 108.9 . . ? C16 C15 H15B 108.9 . . ? N1 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C15 C16 N2 113.4(7) . . ? C15 C16 H16A 108.9 . . ? N2 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? N2 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C2 C19 C20 111.8(7) . . ? C2 C19 C22 108.6(7) . . ? C20 C19 C22 108.9(8) . . ? C2 C19 C21 110.6(7) . . ? C20 C19 C21 106.0(8) . . ? C22 C19 C21 110.9(7) . . ? 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 . . ? C25 C23 C26 104.7(11) . . ? C25 C23 C24 109.7(11) . . ? C26 C23 C24 105.9(10) . . ? C25 C23 C4 111.2(9) . . ? C26 C23 C4 113.0(10) . . ? C24 C23 C4 111.9(9) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C27 C28 112.5(8) . . ? C8 C27 C29 108.4(7) . . ? C28 C27 C29 107.2(8) . . ? C8 C27 C30 113.2(7) . . ? C28 C27 C30 106.3(8) . . ? C29 C27 C30 109.0(8) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32' C31 C33 117.0(19) . . ? C32' C31 C34' 119.7(13) . . ? C33 C31 C34' 79.4(12) . . ? C32' C31 C32 18.4(13) . . ? C33 C31 C32 109.1(14) . . ? C34' C31 C32 136.9(13) . . ? C32' C31 C33' 105.7(14) . . ? C33 C31 C33' 21.5(11) . . ? C34' C31 C33' 100.9(12) . . ? C32 C31 C33' 93.2(16) . . ? C32' C31 C34 88.1(13) . . ? C33 C31 C34 110.2(11) . . ? C34' C31 C34 36.4(10) . . ? C32 C31 C34 106.5(12) . . ? C33' C31 C34 130.3(12) . . ? C32' C31 C10 112.7(12) . . ? C33 C31 C10 114.0(12) . . ? C34' C31 C10 110.1(10) . . ? C32 C31 C10 104.6(11) . . ? C33' C31 C10 106.0(11) . . ? C34 C31 C10 112.0(10) . . ? O3 C35 C36 121.0(7) . . ? O3 C35 C40 120.0(8) . . ? C36 C35 C40 118.9(8) . . ? C37 C36 C35 119.6(8) . . ? C37 C36 C41 120.9(8) . . ? C35 C36 C41 119.3(7) . . ? C36 C37 C38 120.6(9) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C39 C38 C37 120.5(9) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 121.9(9) . . ? C38 C39 H39 119.0 . . ? C40 C39 H39 119.0 . . ? C39 C40 C35 118.5(9) . . ? C39 C40 C44 122.1(9) . . ? C35 C40 C44 119.4(9) . . ? C42 C41 C43' 132.9(13) . . ? C42 C41 C36 112.3(8) . . ? C43' C41 C36 82.4(9) . . ? C42 C41 C43 125.4(12) . . ? C43' C41 C43 89.1(13) . . ? C36 C41 C43 105.2(9) . . ? C42 C41 C42' 104.0(12) . . ? C43' C41 C42' 106.6(12) . . ? C36 C41 C42' 118.9(11) . . ? C43 C41 C42' 21.4(11) . . ? C45 C44 C40 111.8(10) . . ? C45 C44 C46 109.8(8) . . ? C40 C44 C46 110.5(8) . . ? C45 C44 H44 108.2 . . ? C40 C44 H44 108.2 . . ? C46 C44 H44 108.2 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O4 C47 C48 104.6(8) . . ? O4 C47 H47A 110.8 . . ? C48 C47 H47A 110.8 . . ? O4 C47 H47B 110.8 . . ? C48 C47 H47B 110.8 . . ? H47A C47 H47B 108.9 . . ? C47 C48 C49 103.3(7) . . ? C47 C48 H48A 111.1 . . ? C49 C48 H48A 111.1 . . ? C47 C48 H48B 111.1 . . ? C49 C48 H48B 111.1 . . ? H48A C48 H48B 109.1 . . ? C50 C49 C48 107.1(7) . . ? C50 C49 H49A 110.3 . . ? C48 C49 H49A 110.3 . . ? C50 C49 H49B 110.3 . . ? C48 C49 H49B 110.3 . . ? H49A C49 H49B 108.5 . . ? O4 C50 C49 105.9(7) . . ? O4 C50 H50A 110.6 . . ? C49 C50 H50A 110.6 . . ? O4 C50 H50B 110.6 . . ? C49 C50 H50B 110.6 . . ? H50A C50 H50B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.731 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.112 #===================================================end data_complex4 _database_code_depnum_ccdc_archive 'CCDC 763747' #TrackingRef 'NieKun-dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H77 N2 Nd O5' _chemical_formula_sum 'C49 H77 N2 Nd O5' _chemical_formula_weight 918.37 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x, -y+1/2, z' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z-1/2' '-x, y-1/2, -z' 'x-1/2, y, -z-1/2' _cell_length_a 21.889(2) _cell_length_b 20.6138(18) _cell_length_c 10.7149(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4834.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 17789 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1940 _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.394 _exptl_absorpt_correction_T_max 0.543 _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 20198 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4607 _reflns_number_gt 4255 _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. Because there are disordered atoms (C17-C19, C9-C11), which caused abnormal bond distances or thermal parameters, constraints are used during refinements. ; _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^)+(0.0671P)^2^+5.9045P] 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 4607 _refine_ls_number_parameters 276 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1240 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.680995(13) 0.2500 0.70252(3) 0.03185(14) Uani 1 2 d S . . O1 O 0.65838(13) 0.14557(14) 0.6682(3) 0.0374(6) Uani 1 1 d . . . O2 O 0.7500(2) 0.2500 0.8558(5) 0.0661(14) Uani 1 2 d S . . O3 O 0.7865(2) 0.2500 0.5979(5) 0.0728(16) Uani 1 2 d S . . O4 O 0.67592(19) 0.2500 0.4580(4) 0.0429(10) Uani 1 2 d S . . N1 N 0.5597(2) 0.2500 0.6628(4) 0.0309(10) Uani 1 2 d S . . N2 N 0.6123(3) 0.2500 0.9143(5) 0.0592(17) Uani 1 2 d SD . . C1 C 0.61090(18) 0.10571(19) 0.6831(4) 0.0327(9) Uani 1 1 d . . . C2 C 0.61746(19) 0.04260(19) 0.7336(4) 0.0337(9) Uani 1 1 d . . . C3 C 0.56425(19) 0.0061(2) 0.7502(4) 0.0371(9) Uani 1 1 d . . . H3 H 0.5682 -0.0355 0.7853 0.045 Uiso 1 1 calc R . . C4 C 0.5059(2) 0.0269(2) 0.7188(4) 0.0396(10) Uani 1 1 d . A . C5 C 0.50177(19) 0.08812(19) 0.6654(4) 0.0369(9) Uani 1 1 d . . . H5 H 0.4633 0.1037 0.6407 0.044 Uiso 1 1 calc R . . C6 C 0.55252(18) 0.12689(19) 0.6476(4) 0.0337(9) Uani 1 1 d . . . C7 C 0.54482(19) 0.19202(18) 0.5852(4) 0.0361(9) Uani 1 1 d . . . H7A H 0.5707 0.1929 0.5107 0.043 Uiso 1 1 calc R . . H7B H 0.5023 0.1959 0.5573 0.043 Uiso 1 1 calc R . . C8 C 0.5201(3) 0.2500 0.7778(6) 0.0416(14) Uani 1 2 d S . . C9 C 0.5503(4) 0.2844(5) 0.8873(9) 0.0499(14) Uani 0.50 1 d P . . C10 C 0.6091(5) 0.1892(4) 0.9717(9) 0.0499(14) Uani 0.50 1 d PD . . C11 C 0.6395(5) 0.3025(4) 0.9988(9) 0.0499(14) Uani 0.50 1 d PD . . C12 C 0.68039(19) 0.0144(2) 0.7632(5) 0.0395(10) Uani 1 1 d . . . C13 C 0.6768(2) -0.0538(3) 0.8216(6) 0.0548(13) Uani 1 1 d . . . H13A H 0.6488 -0.0531 0.8918 0.082 Uiso 1 1 calc R . . H13B H 0.7170 -0.0668 0.8501 0.082 Uiso 1 1 calc R . . H13C H 0.6622 -0.0845 0.7597 0.082 Uiso 1 1 calc R . . C14 C 0.7167(2) 0.0091(3) 0.6422(5) 0.0589(13) Uani 1 1 d . . . H14A H 0.6962 -0.0206 0.5859 0.088 Uiso 1 1 calc R . . H14B H 0.7574 -0.0070 0.6603 0.088 Uiso 1 1 calc R . . H14C H 0.7196 0.0515 0.6035 0.088 Uiso 1 1 calc R . . C15 C 0.7153(2) 0.0567(2) 0.8568(5) 0.0528(12) Uani 1 1 d . . . H15A H 0.7214 0.0996 0.8217 0.079 Uiso 1 1 calc R . . H15B H 0.7546 0.0371 0.8746 0.079 Uiso 1 1 calc R . . H15C H 0.6919 0.0602 0.9334 0.079 Uiso 1 1 calc R . . C16 C 0.4482(2) -0.0146(2) 0.7412(5) 0.0495(11) Uani 1 1 d D . . C17 C 0.4647(7) -0.0863(6) 0.7147(13) 0.0765(16) Uani 0.50 1 d PD A 1 C17' C 0.4635(7) -0.0850(6) 0.7786(14) 0.0765(16) Uani 0.50 1 d PD A 2 C18 C 0.3992(9) -0.0104(17) 0.638(2) 0.0765(16) Uani 0.50 1 d PD A 1 C18' C 0.4079(9) -0.0079(17) 0.626(2) 0.0765(16) Uani 0.50 1 d PD A 2 C19 C 0.4256(6) -0.0057(7) 0.8725(12) 0.0765(16) Uani 0.50 1 d PD A 1 C19' C 0.4111(6) 0.0210(7) 0.8430(13) 0.0765(16) Uani 0.50 1 d PD A 2 C20 C 0.7965(3) 0.2500 0.9349(6) 0.0461(15) Uani 1 2 d S . . C21 C 0.8224(2) 0.1927(3) 0.9783(5) 0.0512(12) Uani 1 1 d . . . H21 H 0.8063 0.1529 0.9510 0.061 Uiso 1 1 calc R . . C22 C 0.8713(2) 0.1926(2) 1.0609(4) 0.0506(12) Uani 1 1 d . . . H22 H 0.8882 0.1528 1.0869 0.061 Uiso 1 1 calc R . . C23 C 0.8956(3) 0.2500 1.1055(6) 0.0428(14) Uani 1 2 d S . . C24 C 0.9484(4) 0.2500 1.1969(6) 0.060(2) Uani 1 2 d S . . H24A H 0.9578 0.2057 1.2211 0.090 Uiso 0.50 1 calc PR . . H24B H 0.9373 0.2749 1.2704 0.090 Uiso 0.50 1 calc PR . . H24C H 0.9840 0.2694 1.1579 0.090 Uiso 0.50 1 calc PR . . C25 C 0.8255(3) 0.3060(4) 0.6044(8) 0.086(2) Uani 1 1 d . . . H25A H 0.8367 0.3158 0.6910 0.103 Uiso 1 1 calc R . . H25B H 0.8055 0.3441 0.5679 0.103 Uiso 1 1 calc R . . C26 C 0.8805(3) 0.2865(4) 0.5297(8) 0.102(3) Uani 1 1 d . . . H26A H 0.9180 0.3032 0.5681 0.123 Uiso 1 1 calc R . . H26B H 0.8776 0.3032 0.4443 0.123 Uiso 1 1 calc R . . C27 C 0.6888(3) 0.3061(3) 0.3822(6) 0.0677(16) Uani 1 1 d . . . H27A H 0.7064 0.3408 0.4334 0.081 Uiso 1 1 calc R . . H27B H 0.6511 0.3223 0.3437 0.081 Uiso 1 1 calc R . . C28 C 0.7327(4) 0.2855(3) 0.2850(5) 0.0799(19) Uani 1 1 d . . . H28A H 0.7202 0.3021 0.2031 0.096 Uiso 1 1 calc R . . H28B H 0.7736 0.3021 0.3039 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02389(19) 0.0351(2) 0.0365(2) 0.000 0.00013(11) 0.000 O1 0.0293(14) 0.0372(15) 0.0458(15) 0.0022(13) -0.0004(13) -0.0016(12) O2 0.037(3) 0.103(4) 0.058(3) 0.000 -0.017(2) 0.000 O3 0.033(3) 0.108(5) 0.077(4) 0.000 0.014(3) 0.000 O4 0.052(3) 0.043(2) 0.034(2) 0.000 0.0071(18) 0.000 N1 0.026(2) 0.031(2) 0.036(2) 0.000 -0.0054(19) 0.000 N2 0.035(3) 0.108(5) 0.035(3) 0.000 0.000(2) 0.000 C1 0.033(2) 0.032(2) 0.034(2) -0.0031(17) 0.0007(16) -0.0012(17) C2 0.037(2) 0.0305(19) 0.033(2) -0.0034(17) -0.0008(17) 0.0034(17) C3 0.042(2) 0.030(2) 0.039(2) -0.0015(17) 0.001(2) -0.0022(17) C4 0.038(2) 0.036(2) 0.045(2) -0.0026(18) 0.0013(18) -0.0043(19) C5 0.031(2) 0.033(2) 0.047(2) -0.0022(19) -0.0025(18) -0.0019(17) C6 0.032(2) 0.035(2) 0.034(2) -0.0028(17) -0.0023(16) -0.0002(16) C7 0.032(2) 0.032(2) 0.044(2) -0.0016(18) -0.0094(17) -0.0016(17) C8 0.035(3) 0.046(3) 0.044(3) 0.000 0.006(3) 0.000 C9 0.045(4) 0.053(3) 0.051(3) -0.003(3) 0.003(3) 0.006(2) C10 0.045(4) 0.053(3) 0.051(3) -0.003(3) 0.003(3) 0.006(2) C11 0.045(4) 0.053(3) 0.051(3) -0.003(3) 0.003(3) 0.006(2) C12 0.038(2) 0.037(2) 0.044(2) 0.002(2) 0.0000(17) 0.0011(18) C13 0.053(3) 0.038(3) 0.073(3) 0.005(2) -0.011(2) 0.009(2) C14 0.041(3) 0.077(4) 0.058(3) -0.001(3) 0.005(2) 0.019(3) C15 0.050(3) 0.052(3) 0.057(3) 0.003(2) -0.020(2) 0.002(2) C16 0.042(3) 0.049(3) 0.058(3) 0.005(2) 0.003(2) -0.009(2) C17 0.063(3) 0.082(3) 0.085(4) 0.018(3) -0.006(3) -0.034(3) C17' 0.063(3) 0.082(3) 0.085(4) 0.018(3) -0.006(3) -0.034(3) C18 0.063(3) 0.082(3) 0.085(4) 0.018(3) -0.006(3) -0.034(3) C18' 0.063(3) 0.082(3) 0.085(4) 0.018(3) -0.006(3) -0.034(3) C19 0.063(3) 0.082(3) 0.085(4) 0.018(3) -0.006(3) -0.034(3) C19' 0.063(3) 0.082(3) 0.085(4) 0.018(3) -0.006(3) -0.034(3) C20 0.030(3) 0.068(4) 0.040(3) 0.000 -0.001(3) 0.000 C21 0.043(3) 0.059(3) 0.052(3) 0.001(3) -0.008(2) -0.013(2) C22 0.043(3) 0.057(3) 0.051(3) 0.012(2) -0.004(2) -0.002(2) C23 0.029(3) 0.068(4) 0.031(3) 0.000 0.000(2) 0.000 C24 0.047(4) 0.090(6) 0.045(4) 0.000 -0.012(3) 0.000 C25 0.053(4) 0.117(6) 0.088(5) -0.001(4) 0.016(3) -0.015(3) C26 0.043(3) 0.150(7) 0.114(5) 0.014(5) 0.008(4) -0.003(4) C27 0.092(4) 0.053(3) 0.058(3) 0.017(3) 0.022(3) 0.006(3) C28 0.097(5) 0.084(4) 0.058(3) 0.003(3) 0.024(3) -0.018(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 Nd1 O2 2.232(5) . ? Nd1 O1 2.239(3) 3 ? Nd1 O1 2.239(3) . ? Nd1 O3 2.568(5) . ? Nd1 O4 2.622(4) . ? Nd1 N1 2.688(4) . ? Nd1 N2 2.721(5) . ? O1 C1 1.334(5) . ? O2 C20 1.325(8) . ? O3 C25 1.438(8) . ? O3 C25 1.438(8) 3 ? O4 C27 1.441(6) . ? O4 C27 1.441(6) 3 ? N1 C7 1.492(5) 3 ? N1 C7 1.492(5) . ? N1 C8 1.507(8) . ? N2 C10 1.399(8) 3 ? N2 C10 1.399(8) . ? N2 C11 1.532(8) . ? N2 C11 1.532(8) 3 ? N2 C9 1.560(10) 3 ? N2 C9 1.560(10) . ? C1 C6 1.403(6) . ? C1 C2 1.416(6) . ? C2 C3 1.398(6) . ? C2 C12 1.528(6) . ? C3 C4 1.389(6) . ? C3 H3 0.9400 . ? C4 C5 1.388(6) . ? C4 C16 1.546(6) . ? C5 C6 1.382(6) . ? C5 H5 0.9400 . ? C6 C7 1.509(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.522(11) . ? C8 C9 1.522(11) 3 ? C9 C9 1.418(19) 3 ? C9 C10 1.665(14) 3 ? C10 C11 0.746(11) 3 ? C10 C9 1.665(14) 3 ? C11 C10 0.746(11) 3 ? C12 C14 1.524(7) . ? C12 C15 1.534(6) . ? C12 C13 1.541(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C19 1.502(13) . ? C16 C18' 1.527(16) . ? C16 C18 1.539(15) . ? C16 C17' 1.542(13) . ? C16 C19' 1.545(14) . ? C16 C17 1.546(14) . ? C20 C21 1.390(6) 3 ? C20 C21 1.390(6) . ? C21 C22 1.390(7) . ? C21 H21 0.9400 . ? C22 C23 1.383(6) . ? C22 H22 0.9400 . ? C23 C22 1.383(6) 3 ? C23 C24 1.515(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.501(9) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 C26 1.504(16) 3 ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.480(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C28 1.463(13) 3 ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nd1 O1 105.70(7) . 3 ? O2 Nd1 O1 105.70(7) . . ? O1 Nd1 O1 148.02(15) 3 . ? O2 Nd1 O3 73.26(19) . . ? O1 Nd1 O3 97.31(8) 3 . ? O1 Nd1 O3 97.31(8) . . ? O2 Nd1 O4 139.80(17) . . ? O1 Nd1 O4 80.01(8) 3 . ? O1 Nd1 O4 80.01(8) . . ? O3 Nd1 O4 66.54(16) . . ? O2 Nd1 N1 141.73(17) . . ? O1 Nd1 N1 75.86(7) 3 . ? O1 Nd1 N1 75.86(7) . . ? O3 Nd1 N1 145.01(16) . . ? O4 Nd1 N1 78.47(14) . . ? O2 Nd1 N2 76.15(18) . . ? O1 Nd1 N2 90.85(8) 3 . ? O1 Nd1 N2 90.85(8) . . ? O3 Nd1 N2 149.41(18) . . ? O4 Nd1 N2 144.05(15) . . ? N1 Nd1 N2 65.58(15) . . ? C1 O1 Nd1 138.1(3) . . ? C20 O2 Nd1 172.4(5) . . ? C25 O3 C25 106.9(7) . 3 ? C25 O3 Nd1 120.8(3) . . ? C25 O3 Nd1 120.8(3) 3 . ? C27 O4 C27 106.7(5) . 3 ? C27 O4 Nd1 123.7(3) . . ? C27 O4 Nd1 123.7(3) 3 . ? C7 N1 C7 106.5(4) 3 . ? C7 N1 C8 109.2(3) 3 . ? C7 N1 C8 109.2(3) . . ? C7 N1 Nd1 107.7(2) 3 . ? C7 N1 Nd1 107.7(2) . . ? C8 N1 Nd1 116.1(3) . . ? C10 N2 C10 127.4(9) 3 . ? C10 N2 C11 29.0(5) 3 . ? C10 N2 C11 113.2(7) . . ? C10 N2 C11 113.2(7) 3 3 ? C10 N2 C11 29.0(5) . 3 ? C11 N2 C11 90.0(8) . 3 ? C10 N2 C9 116.4(7) 3 3 ? C10 N2 C9 68.3(6) . 3 ? C11 N2 C9 140.2(6) . 3 ? C11 N2 C9 97.2(6) 3 3 ? C10 N2 C9 68.3(6) 3 . ? C10 N2 C9 116.4(7) . . ? C11 N2 C9 97.2(6) . . ? C11 N2 C9 140.2(6) 3 . ? C9 N2 C9 54.1(7) 3 . ? C10 N2 Nd1 113.3(5) 3 . ? C10 N2 Nd1 113.3(5) . . ? C11 N2 Nd1 106.2(5) . . ? C11 N2 Nd1 106.2(5) 3 . ? C9 N2 Nd1 109.1(4) 3 . ? C9 N2 Nd1 109.1(4) . . ? O1 C1 C6 119.0(4) . . ? O1 C1 C2 122.2(4) . . ? C6 C1 C2 118.8(4) . . ? C3 C2 C1 117.3(4) . . ? C3 C2 C12 121.3(4) . . ? C1 C2 C12 121.3(4) . . ? C4 C3 C2 124.7(4) . . ? C4 C3 H3 117.7 . . ? C2 C3 H3 117.7 . . ? C5 C4 C3 116.2(4) . . ? C5 C4 C16 121.0(4) . . ? C3 C4 C16 122.9(4) . . ? C6 C5 C4 122.0(4) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C1 121.0(4) . . ? C5 C6 C7 119.1(4) . . ? C1 C6 C7 119.9(4) . . ? N1 C7 C6 116.2(3) . . ? N1 C7 H7A 108.2 . . ? C6 C7 H7A 108.2 . . ? N1 C7 H7B 108.2 . . ? C6 C7 H7B 108.2 . . ? H7A C7 H7B 107.4 . . ? N1 C8 C9 112.4(5) . . ? N1 C8 C9 112.4(5) . 3 ? C9 C8 C9 55.5(8) . 3 ? C9 C9 C8 62.2(4) 3 . ? C9 C9 N2 63.0(4) 3 . ? C8 C9 N2 108.0(6) . . ? C9 C9 C10 109.1(5) 3 3 ? C8 C9 C10 155.1(8) . 3 ? N2 C9 C10 51.3(4) . 3 ? C11 C10 N2 85.4(10) 3 . ? C11 C10 C9 145.7(11) 3 3 ? N2 C10 C9 60.5(5) . 3 ? C10 C11 N2 65.5(8) 3 . ? C14 C12 C2 108.7(4) . . ? C14 C12 C15 109.7(4) . . ? C2 C12 C15 111.6(4) . . ? C14 C12 C13 107.9(4) . . ? C2 C12 C13 112.6(4) . . ? C15 C12 C13 106.2(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C16 C18' 124.0(13) . . ? C19 C16 C18 115.7(12) . . ? C18' C16 C18 9.0(15) . . ? C19 C16 C17' 86.8(8) . . ? C18' C16 C17' 115.0(15) . . ? C18 C16 C17' 113.0(14) . . ? C19 C16 C19' 26.9(6) . . ? C18' C16 C19' 103.1(14) . . ? C18 C16 C19' 96.5(14) . . ? C17' C16 C19' 112.2(8) . . ? C19 C16 C4 110.3(6) . . ? C18' C16 C4 107.2(8) . . ? C18 C16 C4 115.3(8) . . ? C17' C16 C4 112.6(6) . . ? C19' C16 C4 106.0(6) . . ? C19 C16 C17 111.4(8) . . ? C18' C16 C17 94.2(15) . . ? C18 C16 C17 94.9(16) . . ? C17' C16 C17 25.6(6) . . ? C19' C16 C17 134.9(8) . . ? C4 C16 C17 108.0(6) . . ? O2 C20 C21 121.8(3) . 3 ? O2 C20 C21 121.8(3) . . ? C21 C20 C21 116.4(6) 3 . ? C22 C21 C20 121.9(5) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C23 C22 C21 121.0(5) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C22 117.8(6) 3 . ? C22 C23 C24 121.1(3) 3 . ? C22 C23 C24 121.1(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 C25 C26 103.5(6) . . ? O3 C25 H25A 111.1 . . ? C26 C25 H25A 111.1 . . ? O3 C25 H25B 111.1 . . ? C26 C25 H25B 111.1 . . ? H25A C25 H25B 109.0 . . ? C25 C26 C26 105.6(4) . 3 ? C25 C26 H26A 110.6 . . ? C26 C26 H26A 110.6 3 . ? C25 C26 H26B 110.6 . . ? C26 C26 H26B 110.6 3 . ? H26A C26 H26B 108.8 . . ? O4 C27 C28 107.1(5) . . ? O4 C27 H27A 110.3 . . ? C28 C27 H27A 110.3 . . ? O4 C27 H27B 110.3 . . ? C28 C27 H27B 110.3 . . ? H27A C27 H27B 108.6 . . ? C28 C28 C27 106.7(3) 3 . ? C28 C28 H28A 110.4 3 . ? C27 C28 H28A 110.4 . . ? C28 C28 H28B 110.4 3 . ? C27 C28 H28B 110.4 . . ? H28A C28 H28B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.333 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.098 #===================================================end data_complex5 _database_code_depnum_ccdc_archive 'CCDC 763748' #TrackingRef 'NieKun-dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H77 N2 O5 Sm' _chemical_formula_sum 'C49 H77 N2 O5 Sm' _chemical_formula_weight 924.48 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 orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x, -y+1/2, z' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z-1/2' '-x, y-1/2, -z' 'x-1/2, y, -z-1/2' _cell_length_a 21.8277(13) _cell_length_b 20.6671(13) _cell_length_c 10.6996(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4826.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14821 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1948 _exptl_absorpt_coefficient_mu 1.261 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.526 _exptl_absorpt_correction_T_max 0.777 _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 17609 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4578 _reflns_number_gt 4093 _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. Because there are disordered atoms (C17-C19, C9-C11), which caused abnormal bond distances or thermal parameters, constraints are used during refinements. ; _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^+4.1805P] 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 consrt _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4578 _refine_ls_number_parameters 276 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1207 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.679720(12) 0.2500 0.70429(3) 0.03026(13) Uani 1 2 d S . . O1 O 0.65842(13) 0.14683(14) 0.6704(3) 0.0352(6) Uani 1 1 d . . . O2 O 0.7481(2) 0.2500 0.8557(4) 0.0613(14) Uani 1 2 d S . . O3 O 0.7847(2) 0.2500 0.5998(5) 0.0716(17) Uani 1 2 d S . . O4 O 0.67506(19) 0.2500 0.4619(4) 0.0424(11) Uani 1 2 d S . . N1 N 0.5593(2) 0.2500 0.6641(4) 0.0298(10) Uani 1 2 d S . . N2 N 0.6124(2) 0.2500 0.9142(5) 0.0552(17) Uani 1 2 d SD . . C1 C 0.61087(18) 0.1063(2) 0.6836(3) 0.0308(9) Uani 1 1 d . . . C2 C 0.61772(18) 0.0430(2) 0.7341(4) 0.0318(9) Uani 1 1 d . . . C3 C 0.56482(19) 0.0063(2) 0.7504(4) 0.0358(10) Uani 1 1 d . . . H3 H 0.5689 -0.0352 0.7855 0.043 Uiso 1 1 calc R . . C4 C 0.5060(2) 0.0271(2) 0.7178(4) 0.0373(10) Uani 1 1 d . A . C5 C 0.50148(18) 0.0881(2) 0.6653(4) 0.0357(10) Uani 1 1 d . . . H5 H 0.4627 0.1035 0.6410 0.043 Uiso 1 1 calc R . . C6 C 0.55230(18) 0.1272(2) 0.6475(4) 0.0323(9) Uani 1 1 d . . . C7 C 0.54456(18) 0.1922(2) 0.5853(4) 0.0341(9) Uani 1 1 d . . . H7A H 0.5707 0.1933 0.5109 0.041 Uiso 1 1 calc R . . H7B H 0.5020 0.1960 0.5571 0.041 Uiso 1 1 calc R . . C8 C 0.5197(3) 0.2500 0.7783(6) 0.0402(15) Uani 1 2 d S . . C9 C 0.5502(4) 0.2846(5) 0.8862(9) 0.0525(16) Uani 0.50 1 d P . . C10 C 0.6089(5) 0.1889(4) 0.9739(10) 0.0525(16) Uani 0.50 1 d PD . . C11 C 0.6388(5) 0.3014(5) 0.9954(10) 0.0525(16) Uani 0.50 1 d PD . . C12 C 0.68122(19) 0.0151(2) 0.7633(5) 0.0392(10) Uani 1 1 d . . . C13 C 0.6776(2) -0.0529(3) 0.8224(6) 0.0530(13) Uani 1 1 d . . . H13A H 0.6615 -0.0832 0.7616 0.079 Uiso 1 1 calc R . . H13B H 0.6509 -0.0516 0.8947 0.079 Uiso 1 1 calc R . . H13C H 0.7183 -0.0665 0.8479 0.079 Uiso 1 1 calc R . . C14 C 0.7173(2) 0.0106(3) 0.6418(5) 0.0588(14) Uani 1 1 d . . . H14A H 0.6966 -0.0187 0.5849 0.088 Uiso 1 1 calc R . . H14B H 0.7581 -0.0056 0.6591 0.088 Uiso 1 1 calc R . . H14C H 0.7201 0.0531 0.6040 0.088 Uiso 1 1 calc R . . C15 C 0.7158(2) 0.0576(2) 0.8580(4) 0.0493(12) Uani 1 1 d . . . H15A H 0.7562 0.0396 0.8726 0.074 Uiso 1 1 calc R . . H15B H 0.6932 0.0588 0.9361 0.074 Uiso 1 1 calc R . . H15C H 0.7197 0.1011 0.8250 0.074 Uiso 1 1 calc R . . C16 C 0.4481(2) -0.0150(2) 0.7405(5) 0.0480(12) Uani 1 1 d D . . C17 C 0.4653(7) -0.0862(6) 0.7141(12) 0.0719(17) Uani 0.50 1 d PD A 1 C17' C 0.4634(6) -0.0846(6) 0.7746(13) 0.0719(17) Uani 0.50 1 d PD A 2 C18 C 0.3991(8) -0.0052(16) 0.6391(17) 0.0719(17) Uani 0.50 1 d PD A 1 C18' C 0.4079(8) -0.0120(16) 0.6233(17) 0.0719(17) Uani 0.50 1 d PD A 2 C19 C 0.4253(6) -0.0062(7) 0.8723(11) 0.0719(17) Uani 0.50 1 d PD A 1 C19' C 0.4109(6) 0.0203(7) 0.8441(12) 0.0719(17) Uani 0.50 1 d PD A 2 C20 C 0.7948(3) 0.2500 0.9348(6) 0.0462(17) Uani 1 2 d S . . C21 C 0.8209(2) 0.1924(3) 0.9785(5) 0.0500(13) Uani 1 1 d . . . H21 H 0.8049 0.1526 0.9515 0.060 Uiso 1 1 calc R . . C22 C 0.8702(2) 0.1930(3) 1.0610(4) 0.0494(12) Uani 1 1 d . . . H22 H 0.8871 0.1535 1.0875 0.059 Uiso 1 1 calc R . . C23 C 0.8947(3) 0.2500 1.1047(5) 0.0405(15) Uani 1 2 d S . . C24 C 0.9471(3) 0.2500 1.1968(6) 0.058(2) Uani 1 2 d S . . H24A H 0.9829 0.2306 1.1583 0.087 Uiso 0.50 1 calc PR . . H24B H 0.9356 0.2253 1.2702 0.087 Uiso 0.50 1 calc PR . . H24C H 0.9564 0.2941 1.2210 0.087 Uiso 0.50 1 calc PR . . C25 C 0.8240(3) 0.3059(4) 0.6072(7) 0.085(2) Uani 1 1 d . . . H25A H 0.8356 0.3150 0.6939 0.102 Uiso 1 1 calc R . . H25B H 0.8040 0.3442 0.5717 0.102 Uiso 1 1 calc R . . C26 C 0.8792(3) 0.2863(4) 0.5304(7) 0.103(3) Uani 1 1 d . . . H26A H 0.8759 0.3030 0.4449 0.124 Uiso 1 1 calc R . . H26B H 0.9170 0.3030 0.5680 0.124 Uiso 1 1 calc R . . C27 C 0.6874(3) 0.3062(3) 0.3862(5) 0.0658(16) Uani 1 1 d . . . H27A H 0.7051 0.3409 0.4371 0.079 Uiso 1 1 calc R . . H27B H 0.6496 0.3221 0.3476 0.079 Uiso 1 1 calc R . . C28 C 0.7317(3) 0.2848(3) 0.2886(5) 0.0759(19) Uani 1 1 d . . . H28A H 0.7192 0.3012 0.2065 0.091 Uiso 1 1 calc R . . H28B H 0.7727 0.3012 0.3074 0.091 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02401(18) 0.0347(2) 0.0321(2) 0.000 -0.00033(11) 0.000 O1 0.0280(14) 0.0350(17) 0.0425(15) 0.0018(13) -0.0015(13) -0.0019(12) O2 0.037(2) 0.096(4) 0.050(3) 0.000 -0.017(2) 0.000 O3 0.037(3) 0.114(5) 0.065(3) 0.000 0.012(2) 0.000 O4 0.055(3) 0.040(3) 0.032(2) 0.000 0.0070(19) 0.000 N1 0.027(2) 0.028(3) 0.035(2) 0.000 -0.0037(19) 0.000 N2 0.035(3) 0.098(5) 0.033(3) 0.000 -0.005(2) 0.000 C1 0.030(2) 0.032(2) 0.0311(19) -0.0049(17) 0.0021(16) -0.0001(17) C2 0.033(2) 0.034(2) 0.0290(19) -0.0037(18) 0.0002(16) 0.0001(18) C3 0.042(2) 0.029(2) 0.037(2) -0.0002(18) 0.001(2) -0.0011(18) C4 0.034(2) 0.036(3) 0.041(2) -0.0031(19) 0.0008(18) -0.0047(19) C5 0.029(2) 0.037(3) 0.041(2) -0.002(2) -0.0025(18) -0.0015(18) C6 0.033(2) 0.033(2) 0.031(2) -0.0040(17) -0.0026(16) -0.0009(17) C7 0.030(2) 0.035(2) 0.037(2) -0.0003(18) -0.0080(17) -0.0011(17) C8 0.033(3) 0.049(4) 0.039(3) 0.000 0.000(3) 0.000 C9 0.047(4) 0.058(4) 0.053(3) 0.000(3) 0.013(3) 0.004(2) C10 0.047(4) 0.058(4) 0.053(3) 0.000(3) 0.013(3) 0.004(2) C11 0.047(4) 0.058(4) 0.053(3) 0.000(3) 0.013(3) 0.004(2) C12 0.036(2) 0.036(3) 0.045(2) 0.002(2) -0.0040(18) 0.0048(19) C13 0.051(3) 0.036(3) 0.071(3) 0.003(3) -0.011(2) 0.010(2) C14 0.042(3) 0.079(4) 0.055(3) -0.004(3) 0.004(2) 0.021(3) C15 0.053(3) 0.041(3) 0.053(3) 0.000(2) -0.021(2) 0.003(2) C16 0.042(2) 0.044(3) 0.058(3) 0.002(2) 0.006(2) -0.013(2) C17 0.057(3) 0.083(4) 0.075(3) 0.012(3) -0.004(3) -0.028(3) C17' 0.057(3) 0.083(4) 0.075(3) 0.012(3) -0.004(3) -0.028(3) C18 0.057(3) 0.083(4) 0.075(3) 0.012(3) -0.004(3) -0.028(3) C18' 0.057(3) 0.083(4) 0.075(3) 0.012(3) -0.004(3) -0.028(3) C19 0.057(3) 0.083(4) 0.075(3) 0.012(3) -0.004(3) -0.028(3) C19' 0.057(3) 0.083(4) 0.075(3) 0.012(3) -0.004(3) -0.028(3) C20 0.031(3) 0.071(5) 0.037(3) 0.000 -0.002(3) 0.000 C21 0.041(3) 0.056(3) 0.053(3) 0.000(3) -0.006(2) -0.011(2) C22 0.039(2) 0.063(3) 0.047(2) 0.014(2) -0.003(2) -0.001(2) C23 0.031(3) 0.059(4) 0.031(3) 0.000 -0.003(3) 0.000 C24 0.047(4) 0.085(6) 0.042(4) 0.000 -0.011(3) 0.000 C25 0.052(3) 0.125(7) 0.079(4) 0.001(5) 0.016(3) -0.020(3) C26 0.044(3) 0.162(8) 0.103(5) 0.016(5) 0.006(3) -0.004(4) C27 0.086(4) 0.057(4) 0.055(3) 0.015(3) 0.017(3) 0.006(3) C28 0.097(5) 0.078(4) 0.053(3) 0.000(3) 0.024(3) -0.020(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 2.202(4) . ? Sm1 O1 2.212(3) . ? Sm1 O1 2.212(3) 3 ? Sm1 O3 2.550(5) . ? Sm1 O4 2.595(4) . ? Sm1 N1 2.663(4) . ? Sm1 N2 2.684(5) . ? O1 C1 1.341(5) . ? O2 C20 1.326(7) . ? O3 C25 1.441(8) . ? O3 C25 1.441(8) 3 ? O4 C27 1.442(6) . ? O4 C27 1.442(6) 3 ? N1 C7 1.497(5) . ? N1 C7 1.497(5) 3 ? N1 C8 1.497(8) . ? N2 C10 1.418(8) 3 ? N2 C10 1.418(8) . ? N2 C11 1.488(8) . ? N2 C11 1.488(8) 3 ? N2 C9 1.563(11) 3 ? N2 C9 1.563(11) . ? C1 C6 1.404(6) . ? C1 C2 1.423(6) . ? C2 C3 1.393(6) . ? C2 C12 1.534(6) . ? C3 C4 1.399(6) . ? C3 H3 0.9400 . ? C4 C5 1.384(6) . ? C4 C16 1.553(6) . ? C5 C6 1.386(6) . ? C5 H5 0.9400 . ? C6 C7 1.508(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.513(12) . ? C8 C9 1.513(11) 3 ? C9 C9 1.43(2) 3 ? C9 C10 1.680(15) 3 ? C10 C11 0.721(12) 3 ? C10 C9 1.680(15) 3 ? C11 C10 0.721(12) 3 ? C12 C14 1.523(7) . ? C12 C15 1.538(6) . ? C12 C13 1.542(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C19 1.507(13) . ? C16 C17' 1.521(13) . ? C16 C18' 1.532(15) . ? C16 C18 1.538(15) . ? C16 C17 1.545(14) . ? C16 C19' 1.556(13) . ? C20 C21 1.400(6) 3 ? C20 C21 1.400(6) . ? C21 C22 1.390(6) . ? C21 H21 0.9400 . ? C22 C23 1.377(6) . ? C22 H22 0.9400 . ? C23 C22 1.377(6) 3 ? C23 C24 1.509(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.514(9) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 C26 1.502(16) 3 ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.490(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C28 1.437(13) 3 ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Sm1 O1 105.25(7) . . ? O2 Sm1 O1 105.25(7) . 3 ? O1 Sm1 O1 149.08(15) . 3 ? O2 Sm1 O3 73.37(18) . . ? O1 Sm1 O3 96.72(8) . . ? O1 Sm1 O3 96.72(8) 3 . ? O2 Sm1 O4 139.61(16) . . ? O1 Sm1 O4 80.09(8) . . ? O1 Sm1 O4 80.09(8) 3 . ? O3 Sm1 O4 66.23(15) . . ? O2 Sm1 N1 141.94(17) . . ? O1 Sm1 N1 76.47(7) . . ? O1 Sm1 N1 76.47(7) 3 . ? O3 Sm1 N1 144.68(16) . . ? O4 Sm1 N1 78.45(14) . . ? O2 Sm1 N2 75.83(17) . . ? O1 Sm1 N2 91.27(8) . . ? O1 Sm1 N2 91.27(8) 3 . ? O3 Sm1 N2 149.20(17) . . ? O4 Sm1 N2 144.56(14) . . ? N1 Sm1 N2 66.11(15) . . ? C1 O1 Sm1 138.4(3) . . ? C20 O2 Sm1 172.3(4) . . ? C25 O3 C25 106.5(7) . 3 ? C25 O3 Sm1 120.7(3) . . ? C25 O3 Sm1 120.7(3) 3 . ? C27 O4 C27 107.3(6) . 3 ? C27 O4 Sm1 123.7(3) . . ? C27 O4 Sm1 123.7(3) 3 . ? C7 N1 C7 105.9(4) . 3 ? C7 N1 C8 109.6(3) . . ? C7 N1 C8 109.6(3) 3 . ? C7 N1 Sm1 107.7(2) . . ? C7 N1 Sm1 107.7(2) 3 . ? C8 N1 Sm1 116.0(3) . . ? C10 N2 C10 126.0(10) 3 . ? C10 N2 C11 28.6(5) 3 . ? C10 N2 C11 113.2(7) . . ? C10 N2 C11 113.2(7) 3 3 ? C10 N2 C11 28.6(5) . 3 ? C11 N2 C11 91.1(9) . 3 ? C10 N2 C9 116.5(7) 3 3 ? C10 N2 C9 68.4(6) . 3 ? C11 N2 C9 140.7(7) . 3 ? C11 N2 C9 97.0(6) 3 3 ? C10 N2 C9 68.4(6) 3 . ? C10 N2 C9 116.5(7) . . ? C11 N2 C9 97.0(6) . . ? C11 N2 C9 140.7(7) 3 . ? C9 N2 C9 54.4(8) 3 . ? C10 N2 Sm1 114.0(5) 3 . ? C10 N2 Sm1 114.0(5) . . ? C11 N2 Sm1 106.1(5) . . ? C11 N2 Sm1 106.1(5) 3 . ? C9 N2 Sm1 108.3(4) 3 . ? C9 N2 Sm1 108.3(4) . . ? O1 C1 C6 118.9(4) . . ? O1 C1 C2 122.2(4) . . ? C6 C1 C2 118.9(4) . . ? C3 C2 C1 117.5(4) . . ? C3 C2 C12 121.2(4) . . ? C1 C2 C12 121.2(4) . . ? C2 C3 C4 124.2(4) . . ? C2 C3 H3 117.9 . . ? C4 C3 H3 117.9 . . ? C5 C4 C3 116.6(4) . . ? C5 C4 C16 121.1(4) . . ? C3 C4 C16 122.3(4) . . ? C4 C5 C6 122.0(4) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 120.8(4) . . ? C5 C6 C7 119.4(4) . . ? C1 C6 C7 119.9(4) . . ? N1 C7 C6 116.0(3) . . ? N1 C7 H7A 108.3 . . ? C6 C7 H7A 108.3 . . ? N1 C7 H7B 108.3 . . ? C6 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? N1 C8 C9 111.6(5) . . ? N1 C8 C9 111.6(5) . 3 ? C9 C8 C9 56.4(8) . 3 ? C9 C9 C8 61.8(4) 3 . ? C9 C9 N2 62.8(4) 3 . ? C8 C9 N2 108.2(7) . . ? C9 C9 C10 109.1(5) 3 3 ? C8 C9 C10 156.4(8) . 3 ? N2 C9 C10 51.7(4) . 3 ? C11 C10 N2 81.2(10) 3 . ? C11 C10 C9 141.1(12) 3 3 ? N2 C10 C9 59.9(5) . 3 ? C10 C11 N2 70.3(9) 3 . ? C14 C12 C2 108.4(4) . . ? C14 C12 C15 110.1(4) . . ? C2 C12 C15 111.3(4) . . ? C14 C12 C13 108.7(4) . . ? C2 C12 C13 112.3(4) . . ? C15 C12 C13 106.0(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C16 C17' 87.8(8) . . ? C19 C16 C18' 124.8(10) . . ? C17' C16 C18' 111.1(13) . . ? C19 C16 C18 114.4(9) . . ? C17' C16 C18 116.5(14) . . ? C18' C16 C18 10.9(16) . . ? C19 C16 C17 111.5(8) . . ? C17' C16 C17 24.5(6) . . ? C18' C16 C17 91.6(13) . . ? C18 C16 C17 99.5(13) . . ? C19 C16 C4 110.4(6) . . ? C17' C16 C4 112.9(6) . . ? C18' C16 C4 108.4(11) . . ? C18 C16 C4 112.5(11) . . ? C17 C16 C4 107.9(6) . . ? C19 C16 C19' 26.4(7) . . ? C17' C16 C19' 112.7(8) . . ? C18' C16 C19' 105.3(10) . . ? C18 C16 C19' 94.4(10) . . ? C17 C16 C19' 134.7(8) . . ? C4 C16 C19' 105.9(6) . . ? O2 C20 C21 121.8(3) . 3 ? O2 C20 C21 121.8(3) . . ? C21 C20 C21 116.4(6) 3 . ? C22 C21 C20 121.3(5) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C23 C22 C21 121.6(5) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C22 117.7(6) . 3 ? C22 C23 C24 121.1(3) . . ? C22 C23 C24 121.1(3) 3 . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 C25 C26 103.3(6) . . ? O3 C25 H25A 111.1 . . ? C26 C25 H25A 111.1 . . ? O3 C25 H25B 111.1 . . ? C26 C25 H25B 111.1 . . ? H25A C25 H25B 109.1 . . ? C26 C26 C25 105.5(4) 3 . ? C26 C26 H26A 110.6 3 . ? C25 C26 H26A 110.6 . . ? C26 C26 H26B 110.6 3 . ? C25 C26 H26B 110.6 . . ? H26A C26 H26B 108.8 . . ? O4 C27 C28 106.0(5) . . ? O4 C27 H27A 110.5 . . ? C28 C27 H27A 110.5 . . ? O4 C27 H27B 110.5 . . ? C28 C27 H27B 110.5 . . ? H27A C27 H27B 108.7 . . ? C28 C28 C27 107.3(3) 3 . ? C28 C28 H28A 110.3 3 . ? C27 C28 H28A 110.3 . . ? C28 C28 H28B 110.3 3 . ? C27 C28 H28B 110.3 . . ? H28A C28 H28B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.004 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.097 #===================================================end data_complex6 _database_code_depnum_ccdc_archive 'CCDC 763749' #TrackingRef 'NieKun-dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H69 N2 O4 Y,C7 H8' _chemical_formula_sum 'C52 H77 N2 O4 Y' _chemical_formula_weight 883.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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 14.5340(12) _cell_length_b 21.4857(15) _cell_length_c 16.2519(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.143(2) _cell_angle_gamma 90.00 _cell_volume 5023.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 19986 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 1.203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.610 _exptl_absorpt_correction_T_max 0.811 _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 25721 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.1042 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9314 _reflns_number_gt 6470 _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. Because there are disordered atoms (C24-C26), which caused abnormal bond distances or thermal parameters, constraints are used during refinements. ; _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^)+(0.1055P)^2^+4.8132P] 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 SHELXL _refine_ls_extinction_coef 0.0022(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9314 _refine_ls_number_parameters 490 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_gt 0.0923 _refine_ls_wR_factor_ref 0.2376 _refine_ls_wR_factor_gt 0.2127 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.75440(4) 0.42622(2) 0.77039(3) 0.0378(2) Uani 1 1 d . . . O1 O 0.7151(3) 0.40731(17) 0.8902(2) 0.0471(10) Uani 1 1 d . . . O2 O 0.7568(3) 0.40705(17) 0.6403(2) 0.0465(10) Uani 1 1 d . . . O3 O 0.8140(3) 0.51514(17) 0.7860(3) 0.0545(11) Uani 1 1 d . . . O4 O 0.5945(3) 0.4469(2) 0.7305(3) 0.0597(12) Uani 1 1 d . . . N1 N 0.7408(3) 0.3090(2) 0.7674(3) 0.0427(11) Uani 1 1 d . . . N2 N 0.9137(4) 0.3805(2) 0.8101(3) 0.0499(12) Uani 1 1 d . . . C1 C 0.7036(4) 0.3608(3) 0.9428(3) 0.0419(13) Uani 1 1 d . . . C2 C 0.7099(4) 0.3695(3) 1.0295(4) 0.0432(13) Uani 1 1 d . . . C3 C 0.6974(4) 0.3174(3) 1.0784(4) 0.0448(14) Uani 1 1 d . . . H3 H 0.7012 0.3231 1.1361 0.054 Uiso 1 1 calc R . . C4 C 0.6798(4) 0.2580(3) 1.0470(4) 0.0435(14) Uani 1 1 d . A . C5 C 0.6751(4) 0.2506(3) 0.9622(4) 0.0447(14) Uani 1 1 d . . . H5 H 0.6647 0.2107 0.9390 0.054 Uiso 1 1 calc R . . C6 C 0.6854(4) 0.3008(2) 0.9105(4) 0.0424(13) Uani 1 1 d . . . C7 C 0.7789(4) 0.3614(3) 0.5905(3) 0.0405(13) Uani 1 1 d . . . C8 C 0.8175(4) 0.3724(2) 0.5163(3) 0.0398(13) Uani 1 1 d . . . C9 C 0.8415(4) 0.3212(3) 0.4718(4) 0.0437(14) Uani 1 1 d . . . H9 H 0.8670 0.3287 0.4227 0.052 Uiso 1 1 calc R . . C10 C 0.8303(4) 0.2598(3) 0.4950(4) 0.0453(14) Uani 1 1 d . . . C11 C 0.7886(4) 0.2500(3) 0.5663(4) 0.0479(15) Uani 1 1 d . . . H11 H 0.7784 0.2090 0.5831 0.058 Uiso 1 1 calc R . . C12 C 0.7621(4) 0.2990(3) 0.6128(4) 0.0483(15) Uani 1 1 d . . . C13 C 0.6664(5) 0.2910(3) 0.8170(4) 0.0502(15) Uani 1 1 d . . . H13A H 0.6524 0.2469 0.8067 0.060 Uiso 1 1 calc R . . H13B H 0.6102 0.3145 0.7956 0.060 Uiso 1 1 calc R . . C14 C 0.7062(5) 0.2868(3) 0.6813(4) 0.0513(16) Uani 1 1 d . . . H14A H 0.6973 0.2417 0.6842 0.062 Uiso 1 1 calc R . . H14B H 0.6446 0.3052 0.6649 0.062 Uiso 1 1 calc R . . C15 C 0.8301(5) 0.2790(3) 0.7996(4) 0.0563(17) Uani 1 1 d . . . H15A H 0.8312 0.2369 0.7764 0.068 Uiso 1 1 calc R . . H15B H 0.8349 0.2751 0.8602 0.068 Uiso 1 1 calc R . . C16 C 0.9139(6) 0.3153(3) 0.7782(5) 0.072(2) Uani 1 1 d . . . H16A H 0.9712 0.2944 0.8027 0.086 Uiso 1 1 calc R . . H16B H 0.9125 0.3160 0.7178 0.086 Uiso 1 1 calc R . . C17 C 0.9462(6) 0.3863(5) 0.8978(5) 0.100(3) Uani 1 1 d . . . H17A H 0.9040 0.3647 0.9291 0.150 Uiso 1 1 calc R . . H17B H 0.9488 0.4300 0.9131 0.150 Uiso 1 1 calc R . . H17C H 1.0078 0.3683 0.9101 0.150 Uiso 1 1 calc R . . C18 C 0.9817(5) 0.4146(4) 0.7663(5) 0.078(2) Uani 1 1 d . . . H18A H 0.9743 0.4590 0.7736 0.117 Uiso 1 1 calc R . . H18B H 0.9707 0.4046 0.7075 0.117 Uiso 1 1 calc R . . H18C H 1.0444 0.4023 0.7892 0.117 Uiso 1 1 calc R . . C19 C 0.7257(5) 0.4349(3) 1.0692(4) 0.0499(15) Uani 1 1 d . . . C20 C 0.8174(5) 0.4630(3) 1.0485(4) 0.0603(18) Uani 1 1 d . . . H20A H 0.8144 0.4667 0.9887 0.090 Uiso 1 1 calc R . . H20B H 0.8688 0.4361 1.0700 0.090 Uiso 1 1 calc R . . H20C H 0.8265 0.5038 1.0737 0.090 Uiso 1 1 calc R . . C21 C 0.6437(6) 0.4765(3) 1.0354(5) 0.070(2) Uani 1 1 d . . . H21A H 0.6403 0.4801 0.9755 0.106 Uiso 1 1 calc R . . H21B H 0.6523 0.5175 1.0604 0.106 Uiso 1 1 calc R . . H21C H 0.5866 0.4583 1.0488 0.106 Uiso 1 1 calc R . . C22 C 0.7329(6) 0.4331(3) 1.1642(4) 0.069(2) Uani 1 1 d . . . H22A H 0.7462 0.4746 1.1864 0.103 Uiso 1 1 calc R . . H22B H 0.7825 0.4050 1.1866 0.103 Uiso 1 1 calc R . . H22C H 0.6746 0.4186 1.1798 0.103 Uiso 1 1 calc R . . C23 C 0.6664(4) 0.2004(3) 1.1029(4) 0.0487(15) Uani 1 1 d D . . C24 C 0.6795(12) 0.2157(7) 1.1961(9) 0.064(4) Uiso 0.50 1 d P A 1 C24' C 0.6348(15) 0.2236(9) 1.1826(9) 0.090(6) Uiso 0.50 1 d PD A 2 C25 C 0.7416(9) 0.1535(6) 1.0879(10) 0.060(4) Uiso 0.50 1 d PD A 1 C25' C 0.7593(14) 0.1648(9) 1.1257(13) 0.091(6) Uiso 0.50 1 d P A 2 C26 C 0.5708(7) 0.1736(6) 1.0772(9) 0.050(3) Uiso 0.50 1 d PD A 1 C26' C 0.5947(11) 0.1559(8) 1.0612(11) 0.080(5) Uiso 0.50 1 d PD A 2 C27 C 0.8274(4) 0.4391(3) 0.4841(4) 0.0468(14) Uani 1 1 d . . . C28 C 0.7312(5) 0.4693(3) 0.4692(4) 0.0649(19) Uani 1 1 d . . . H28A H 0.7365 0.5112 0.4479 0.097 Uiso 1 1 calc R . . H28B H 0.7056 0.4711 0.5211 0.097 Uiso 1 1 calc R . . H28C H 0.6905 0.4449 0.4291 0.097 Uiso 1 1 calc R . . C29 C 0.8907(5) 0.4786(3) 0.5482(4) 0.0556(17) Uani 1 1 d . . . H29A H 0.9512 0.4589 0.5603 0.083 Uiso 1 1 calc R . . H29B H 0.8629 0.4819 0.5989 0.083 Uiso 1 1 calc R . . H29C H 0.8978 0.5199 0.5257 0.083 Uiso 1 1 calc R . . C30 C 0.8690(6) 0.4409(3) 0.4036(4) 0.0647(19) Uani 1 1 d . . . H30A H 0.8272 0.4206 0.3600 0.097 Uiso 1 1 calc R . . H30B H 0.9283 0.4195 0.4112 0.097 Uiso 1 1 calc R . . H30C H 0.8781 0.4839 0.3882 0.097 Uiso 1 1 calc R . . C31 C 0.8571(5) 0.2031(3) 0.4439(4) 0.0528(16) Uani 1 1 d . . . C32 C 0.9250(6) 0.1612(3) 0.4996(5) 0.074(2) Uani 1 1 d . . . H32A H 0.9397 0.1249 0.4683 0.112 Uiso 1 1 calc R . . H32B H 0.8966 0.1479 0.5473 0.112 Uiso 1 1 calc R . . H32C H 0.9815 0.1841 0.5185 0.112 Uiso 1 1 calc R . . C33 C 0.7701(5) 0.1665(3) 0.4131(4) 0.0596(17) Uani 1 1 d . . . H33A H 0.7245 0.1938 0.3823 0.089 Uiso 1 1 calc R . . H33B H 0.7447 0.1490 0.4602 0.089 Uiso 1 1 calc R . . H33C H 0.7853 0.1331 0.3772 0.089 Uiso 1 1 calc R . . C34 C 0.9028(5) 0.2249(3) 0.3700(5) 0.071(2) Uani 1 1 d . . . H34A H 0.9248 0.1891 0.3421 0.107 Uiso 1 1 calc R . . H34B H 0.9548 0.2520 0.3893 0.107 Uiso 1 1 calc R . . H34C H 0.8577 0.2475 0.3314 0.107 Uiso 1 1 calc R . . C35 C 0.8679(4) 0.5653(2) 0.8046(4) 0.0467(14) Uani 1 1 d . . . C36 C 0.9262(5) 0.5866(3) 0.7503(4) 0.0596(17) Uani 1 1 d . . . H36 H 0.9266 0.5665 0.6990 0.072 Uiso 1 1 calc R . . C37 C 0.9838(5) 0.6374(3) 0.7709(5) 0.0649(19) Uani 1 1 d . . . H37 H 1.0227 0.6511 0.7330 0.078 Uiso 1 1 calc R . . C38 C 0.9855(4) 0.6679(3) 0.8444(5) 0.0569(17) Uani 1 1 d . . . C39 C 0.9267(5) 0.6472(3) 0.8984(4) 0.0627(19) Uani 1 1 d . . . H39 H 0.9256 0.6680 0.9491 0.075 Uiso 1 1 calc R . . C40 C 0.8690(4) 0.5959(3) 0.8789(4) 0.0512(15) Uani 1 1 d . . . H40 H 0.8304 0.5821 0.9170 0.061 Uiso 1 1 calc R . . C41 C 1.0480(5) 0.7238(4) 0.8676(6) 0.093(3) Uani 1 1 d . . . H41A H 1.0836 0.7327 0.8228 0.140 Uiso 1 1 calc R . . H41B H 1.0900 0.7148 0.9180 0.140 Uiso 1 1 calc R . . H41C H 1.0101 0.7597 0.8767 0.140 Uiso 1 1 calc R . . C42 C 0.5486(5) 0.4510(5) 0.6456(5) 0.0853(12) Uani 1 1 d . . . H42A H 0.5504 0.4938 0.6249 0.102 Uiso 1 1 calc R . . H42B H 0.5785 0.4235 0.6093 0.102 Uiso 1 1 calc R . . C43 C 0.4550(5) 0.4318(4) 0.6490(5) 0.0853(12) Uani 1 1 d . . . H43A H 0.4489 0.3868 0.6407 0.102 Uiso 1 1 calc R . . H43B H 0.4124 0.4527 0.6055 0.102 Uiso 1 1 calc R . . C44 C 0.4331(5) 0.4491(5) 0.7317(5) 0.0853(12) Uani 1 1 d . . . H44A H 0.3939 0.4174 0.7527 0.102 Uiso 1 1 calc R . . H44B H 0.4007 0.4892 0.7295 0.102 Uiso 1 1 calc R . . C45 C 0.5243(5) 0.4533(5) 0.7850(5) 0.0853(12) Uani 1 1 d . . . H45A H 0.5307 0.4935 0.8138 0.102 Uiso 1 1 calc R . . H45B H 0.5306 0.4200 0.8267 0.102 Uiso 1 1 calc R . . C46 C 1.0008(11) 0.1532(5) 0.8921(10) 0.150(2) Uani 1 1 d D . . C47 C 0.9129(10) 0.1320(5) 0.8968(9) 0.150(2) Uani 1 1 d D . . H47 H 0.8947 0.1349 0.9499 0.180 Uiso 1 1 calc R . . C48 C 0.8476(10) 0.1076(5) 0.8377(9) 0.150(2) Uani 1 1 d D . . H48 H 0.7889 0.0922 0.8454 0.180 Uiso 1 1 calc R . . C49 C 0.8850(10) 0.1097(5) 0.7622(9) 0.150(2) Uani 1 1 d D . . H49 H 0.8480 0.0956 0.7136 0.180 Uiso 1 1 calc R . . C50 C 0.9737(10) 0.1316(5) 0.7557(9) 0.150(2) Uani 1 1 d D . . H50 H 0.9906 0.1307 0.7020 0.180 Uiso 1 1 calc R . . C51 C 1.0403(10) 0.1544(5) 0.8173(9) 0.150(2) Uani 1 1 d D . . H51 H 1.1003 0.1681 0.8108 0.180 Uiso 1 1 calc R . . C52 C 1.0644(10) 0.1798(5) 0.9496(8) 0.150(2) Uani 1 1 d . . . H52A H 1.0667 0.1576 1.0018 0.225 Uiso 1 1 calc R . . H52B H 1.0475 0.2228 0.9573 0.225 Uiso 1 1 calc R . . H52C H 1.1249 0.1781 0.9310 0.225 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0411(3) 0.0317(3) 0.0411(3) 0.0012(2) 0.0072(2) -0.0022(2) O1 0.064(3) 0.0324(19) 0.047(2) 0.0034(18) 0.014(2) -0.0017(18) O2 0.058(3) 0.038(2) 0.045(2) 0.0000(18) 0.0152(19) -0.0012(18) O3 0.055(3) 0.038(2) 0.070(3) -0.006(2) 0.011(2) -0.0090(19) O4 0.040(2) 0.086(3) 0.054(3) 0.002(2) 0.009(2) 0.001(2) N1 0.057(3) 0.031(2) 0.041(3) -0.001(2) 0.012(2) -0.005(2) N2 0.051(3) 0.044(3) 0.054(3) -0.003(2) 0.005(2) -0.001(2) C1 0.044(3) 0.042(3) 0.041(3) 0.000(3) 0.010(3) -0.002(2) C2 0.047(3) 0.037(3) 0.047(3) -0.003(3) 0.012(3) -0.002(2) C3 0.044(3) 0.047(3) 0.044(3) 0.001(3) 0.008(3) -0.002(3) C4 0.044(3) 0.041(3) 0.046(3) 0.008(3) 0.010(3) 0.001(2) C5 0.059(4) 0.032(3) 0.045(3) 0.001(3) 0.015(3) -0.007(3) C6 0.051(4) 0.033(3) 0.045(3) 0.002(3) 0.012(3) -0.006(2) C7 0.044(3) 0.039(3) 0.037(3) -0.001(2) 0.004(3) -0.004(2) C8 0.043(3) 0.036(3) 0.039(3) 0.001(2) 0.001(2) -0.003(2) C9 0.039(3) 0.050(3) 0.041(3) -0.001(3) 0.005(3) -0.006(3) C10 0.051(4) 0.042(3) 0.042(3) -0.006(3) 0.007(3) -0.002(3) C11 0.063(4) 0.035(3) 0.045(3) -0.003(3) 0.007(3) -0.006(3) C12 0.060(4) 0.047(3) 0.040(3) 0.000(3) 0.013(3) -0.013(3) C13 0.066(4) 0.036(3) 0.052(4) -0.003(3) 0.023(3) -0.016(3) C14 0.069(4) 0.038(3) 0.047(3) -0.011(3) 0.010(3) -0.018(3) C15 0.077(5) 0.039(3) 0.056(4) 0.010(3) 0.019(3) 0.013(3) C16 0.087(6) 0.061(4) 0.069(5) 0.002(4) 0.014(4) 0.020(4) C17 0.079(6) 0.160(9) 0.056(5) -0.014(5) -0.007(4) 0.057(6) C18 0.054(5) 0.092(6) 0.088(6) 0.005(5) 0.013(4) 0.016(4) C19 0.066(4) 0.041(3) 0.045(3) -0.003(3) 0.015(3) -0.002(3) C20 0.076(5) 0.049(4) 0.058(4) -0.012(3) 0.014(3) -0.018(3) C21 0.092(6) 0.046(4) 0.074(5) -0.010(4) 0.016(4) 0.015(4) C22 0.099(6) 0.061(4) 0.048(4) -0.014(3) 0.017(4) -0.015(4) C23 0.053(4) 0.048(3) 0.046(3) 0.010(3) 0.011(3) -0.007(3) C27 0.050(4) 0.048(3) 0.042(3) 0.003(3) 0.007(3) -0.009(3) C28 0.069(5) 0.055(4) 0.067(4) 0.024(4) -0.001(4) 0.003(3) C29 0.066(4) 0.045(3) 0.058(4) 0.001(3) 0.014(3) -0.016(3) C30 0.092(5) 0.056(4) 0.048(4) 0.009(3) 0.016(4) -0.014(4) C31 0.061(4) 0.043(3) 0.054(4) -0.009(3) 0.007(3) -0.003(3) C32 0.082(6) 0.054(4) 0.086(5) -0.013(4) 0.007(4) 0.011(4) C33 0.072(5) 0.052(4) 0.055(4) -0.022(3) 0.009(3) -0.008(3) C34 0.081(5) 0.059(4) 0.080(5) -0.020(4) 0.037(4) -0.008(4) C35 0.047(4) 0.032(3) 0.062(4) 0.003(3) 0.009(3) -0.006(2) C36 0.068(5) 0.051(4) 0.063(4) -0.010(3) 0.020(4) -0.009(3) C37 0.057(4) 0.048(4) 0.094(6) -0.005(4) 0.028(4) -0.008(3) C38 0.040(4) 0.041(3) 0.088(5) 0.004(4) 0.001(3) -0.004(3) C39 0.078(5) 0.047(4) 0.058(4) -0.009(3) -0.010(4) 0.003(3) C40 0.057(4) 0.044(3) 0.054(4) 0.002(3) 0.015(3) -0.008(3) C41 0.058(5) 0.070(5) 0.147(8) -0.013(5) -0.007(5) -0.019(4) C42 0.055(2) 0.113(3) 0.087(3) -0.005(3) 0.005(2) 0.004(2) C43 0.055(2) 0.113(3) 0.087(3) -0.005(3) 0.005(2) 0.004(2) C44 0.055(2) 0.113(3) 0.087(3) -0.005(3) 0.005(2) 0.004(2) C45 0.055(2) 0.113(3) 0.087(3) -0.005(3) 0.005(2) 0.004(2) C46 0.192(7) 0.076(3) 0.175(5) 0.014(3) 0.003(5) 0.037(3) C47 0.192(7) 0.076(3) 0.175(5) 0.014(3) 0.003(5) 0.037(3) C48 0.192(7) 0.076(3) 0.175(5) 0.014(3) 0.003(5) 0.037(3) C49 0.192(7) 0.076(3) 0.175(5) 0.014(3) 0.003(5) 0.037(3) C50 0.192(7) 0.076(3) 0.175(5) 0.014(3) 0.003(5) 0.037(3) C51 0.192(7) 0.076(3) 0.175(5) 0.014(3) 0.003(5) 0.037(3) C52 0.192(7) 0.076(3) 0.175(5) 0.014(3) 0.003(5) 0.037(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O3 2.098(4) . ? Y1 O1 2.144(4) . ? Y1 O2 2.159(4) . ? Y1 O4 2.365(4) . ? Y1 N2 2.514(5) . ? Y1 N1 2.526(5) . ? O1 C1 1.341(7) . ? O2 C7 1.340(6) . ? O3 C35 1.342(6) . ? O4 C42 1.447(9) . ? O4 C45 1.449(9) . ? N1 C15 1.477(8) . ? N1 C13 1.489(7) . ? N1 C14 1.496(7) . ? N2 C17 1.442(8) . ? N2 C18 1.491(9) . ? N2 C16 1.493(8) . ? C1 C6 1.404(8) . ? C1 C2 1.411(8) . ? C2 C3 1.399(8) . ? C2 C19 1.550(8) . ? C3 C4 1.385(8) . ? C3 H3 0.9400 . ? C4 C5 1.379(8) . ? C4 C23 1.563(8) . ? C5 C6 1.389(7) . ? C5 H5 0.9400 . ? C6 C13 1.520(8) . ? C7 C12 1.419(8) . ? C7 C8 1.420(8) . ? C8 C9 1.388(8) . ? C8 C27 1.538(8) . ? C9 C10 1.390(8) . ? C9 H9 0.9400 . ? C10 C11 1.397(8) . ? C10 C31 1.554(8) . ? C11 C12 1.381(8) . ? C11 H11 0.9400 . ? C12 C14 1.492(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.527(10) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C21 1.528(9) . ? C19 C22 1.534(9) . ? C19 C20 1.542(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 C26' 1.503(9) . ? C23 C26 1.508(8) . ? C23 C24' 1.519(9) . ? C23 C25 1.531(9) . ? C23 C24 1.536(16) . ? C23 C25' 1.55(2) . ? C27 C30 1.517(9) . ? C27 C28 1.530(9) . ? C27 C29 1.544(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 C33 1.514(9) . ? C31 C34 1.526(9) . ? C31 C32 1.534(9) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 C40 1.372(9) . ? C35 C36 1.385(9) . ? C36 C37 1.386(9) . ? C36 H36 0.9400 . ? C37 C38 1.360(10) . ? C37 H37 0.9400 . ? C38 C39 1.383(10) . ? C38 C41 1.521(9) . ? C39 C40 1.394(9) . ? C39 H39 0.9400 . ? C40 H40 0.9400 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 C43 1.430(11) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 C44 1.472(11) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 C45 1.480(10) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 C52 1.346(17) . ? C46 C47 1.369(9) . ? C46 C51 1.416(9) . ? C47 C48 1.357(9) . ? C47 H47 0.9400 . ? C48 C49 1.412(9) . ? C48 H48 0.9400 . ? C49 C50 1.389(9) . ? C49 H49 0.9400 . ? C50 C51 1.380(9) . ? C50 H50 0.9400 . ? C51 H51 0.9400 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? 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 O3 Y1 O1 102.78(16) . . ? O3 Y1 O2 103.20(16) . . ? O1 Y1 O2 153.70(15) . . ? O3 Y1 O4 103.59(17) . . ? O1 Y1 O4 84.66(15) . . ? O2 Y1 O4 85.37(15) . . ? O3 Y1 N2 88.61(16) . . ? O1 Y1 N2 92.66(16) . . ? O2 Y1 N2 91.99(16) . . ? O4 Y1 N2 167.80(16) . . ? O3 Y1 N1 160.03(16) . . ? O1 Y1 N1 78.37(14) . . ? O2 Y1 N1 78.63(14) . . ? O4 Y1 N1 96.38(16) . . ? N2 Y1 N1 71.42(15) . . ? C1 O1 Y1 142.5(3) . . ? C7 O2 Y1 140.4(3) . . ? C35 O3 Y1 167.6(4) . . ? C42 O4 C45 108.0(5) . . ? C42 O4 Y1 125.1(4) . . ? C45 O4 Y1 126.8(4) . . ? C15 N1 C13 111.3(5) . . ? C15 N1 C14 110.8(5) . . ? C13 N1 C14 104.4(4) . . ? C15 N1 Y1 111.5(3) . . ? C13 N1 Y1 108.0(3) . . ? C14 N1 Y1 110.5(3) . . ? C17 N2 C18 106.4(6) . . ? C17 N2 C16 114.1(6) . . ? C18 N2 C16 105.1(6) . . ? C17 N2 Y1 112.4(4) . . ? C18 N2 Y1 109.5(4) . . ? C16 N2 Y1 109.0(4) . . ? O1 C1 C6 118.7(5) . . ? O1 C1 C2 122.9(5) . . ? C6 C1 C2 118.5(5) . . ? C3 C2 C1 117.8(5) . . ? C3 C2 C19 120.9(5) . . ? C1 C2 C19 121.2(5) . . ? C4 C3 C2 124.0(5) . . ? C4 C3 H3 118.0 . . ? C2 C3 H3 118.0 . . ? C5 C4 C3 117.1(5) . . ? C5 C4 C23 119.8(5) . . ? C3 C4 C23 123.1(5) . . ? C4 C5 C6 121.4(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 121.2(5) . . ? C5 C6 C13 118.6(5) . . ? C1 C6 C13 119.9(5) . . ? O2 C7 C12 118.2(5) . . ? O2 C7 C8 123.3(5) . . ? C12 C7 C8 118.5(5) . . ? C9 C8 C7 118.0(5) . . ? C9 C8 C27 121.1(5) . . ? C7 C8 C27 120.8(5) . . ? C8 C9 C10 124.3(5) . . ? C8 C9 H9 117.8 . . ? C10 C9 H9 117.8 . . ? C9 C10 C11 116.7(5) . . ? C9 C10 C31 123.4(5) . . ? C11 C10 C31 119.8(5) . . ? C12 C11 C10 121.8(5) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C7 120.6(5) . . ? C11 C12 C14 119.8(5) . . ? C7 C12 C14 119.2(5) . . ? N1 C13 C6 117.5(5) . . ? N1 C13 H13A 107.9 . . ? C6 C13 H13A 107.9 . . ? N1 C13 H13B 107.9 . . ? C6 C13 H13B 107.9 . . ? H13A C13 H13B 107.2 . . ? C12 C14 N1 119.7(5) . . ? C12 C14 H14A 107.4 . . ? N1 C14 H14A 107.4 . . ? C12 C14 H14B 107.4 . . ? N1 C14 H14B 107.4 . . ? H14A C14 H14B 106.9 . . ? N1 C15 C16 112.6(5) . . ? N1 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? N1 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? N2 C16 C15 111.0(6) . . ? N2 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? N2 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C22 108.3(6) . . ? C21 C19 C20 110.3(5) . . ? C22 C19 C20 106.9(6) . . ? C21 C19 C2 108.6(5) . . ? C22 C19 C2 112.4(5) . . ? C20 C19 C2 110.3(5) . . ? 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 . . ? C26' C23 C26 23.0(8) . . ? C26' C23 C24' 108.6(12) . . ? C26 C23 C24' 89.0(10) . . ? C26' C23 C25 88.5(10) . . ? C26 C23 C25 110.8(9) . . ? C24' C23 C25 131.3(11) . . ? C26' C23 C24 124.2(10) . . ? C26 C23 C24 109.6(9) . . ? C24' C23 C24 25.6(8) . . ? C25 C23 C24 107.9(10) . . ? C26' C23 C25' 108.6(12) . . ? C26 C23 C25' 128.0(10) . . ? C24' C23 C25' 108.5(12) . . ? C25 C23 C25' 25.3(8) . . ? C24 C23 C25' 83.6(11) . . ? C26' C23 C4 112.1(8) . . ? C26 C23 C4 109.1(7) . . ? C24' C23 C4 108.3(9) . . ? C25 C23 C4 106.1(7) . . ? C24 C23 C4 113.3(7) . . ? C25' C23 C4 110.7(9) . . ? C30 C27 C28 108.6(5) . . ? C30 C27 C8 112.7(5) . . ? C28 C27 C8 108.8(5) . . ? C30 C27 C29 107.2(5) . . ? C28 C27 C29 108.5(5) . . ? C8 C27 C29 110.9(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C34 109.6(5) . . ? C33 C31 C32 109.0(6) . . ? C34 C31 C32 109.3(6) . . ? C33 C31 C10 108.8(5) . . ? C34 C31 C10 110.6(5) . . ? C32 C31 C10 109.5(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O3 C35 C40 121.0(6) . . ? O3 C35 C36 120.8(6) . . ? C40 C35 C36 118.1(5) . . ? C35 C36 C37 120.6(6) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C38 C37 C36 121.8(7) . . ? C38 C37 H37 119.1 . . ? C36 C37 H37 119.1 . . ? C37 C38 C39 117.7(6) . . ? C37 C38 C41 122.4(7) . . ? C39 C38 C41 119.9(7) . . ? C38 C39 C40 121.2(6) . . ? C38 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C35 C40 C39 120.6(6) . . ? C35 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 O4 105.0(7) . . ? C43 C42 H42A 110.8 . . ? O4 C42 H42A 110.8 . . ? C43 C42 H42B 110.8 . . ? O4 C42 H42B 110.8 . . ? H42A C42 H42B 108.8 . . ? C42 C43 C44 107.0(7) . . ? C42 C43 H43A 110.3 . . ? C44 C43 H43A 110.3 . . ? C42 C43 H43B 110.3 . . ? C44 C43 H43B 110.3 . . ? H43A C43 H43B 108.6 . . ? C43 C44 C45 105.0(7) . . ? C43 C44 H44A 110.7 . . ? C45 C44 H44A 110.7 . . ? C43 C44 H44B 110.7 . . ? C45 C44 H44B 110.7 . . ? H44A C44 H44B 108.8 . . ? O4 C45 C44 106.6(7) . . ? O4 C45 H45A 110.4 . . ? C44 C45 H45A 110.4 . . ? O4 C45 H45B 110.4 . . ? C44 C45 H45B 110.4 . . ? H45A C45 H45B 108.6 . . ? C52 C46 C47 131.1(16) . . ? C52 C46 C51 105.4(14) . . ? C47 C46 C51 123.4(17) . . ? C48 C47 C46 130.8(17) . . ? C48 C47 H47 114.6 . . ? C46 C47 H47 114.6 . . ? C47 C48 C49 106.6(14) . . ? C47 C48 H48 126.7 . . ? C49 C48 H48 126.7 . . ? C50 C49 C48 123.5(15) . . ? C50 C49 H49 118.2 . . ? C48 C49 H49 118.2 . . ? C51 C50 C49 128.9(16) . . ? C51 C50 H50 115.5 . . ? C49 C50 H50 115.5 . . ? C50 C51 C46 106.7(15) . . ? C50 C51 H51 126.7 . . ? C46 C51 H51 126.7 . . ? C46 C52 H52A 109.5 . . ? C46 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C46 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.866 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.101 #===================================================end data_complex7 _database_code_depnum_ccdc_archive 'CCDC 763750' #TrackingRef 'NieKun-dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H77 N2 Nd O6' _chemical_formula_sum 'C49 H77 N2 Nd O6' _chemical_formula_weight 934.37 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x, -y+1/2, z' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z-1/2' '-x, y-1/2, -z' 'x-1/2, y, -z-1/2' _cell_length_a 21.9718(14) _cell_length_b 20.6271(13) _cell_length_c 10.7530(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4873.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13879 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1972 _exptl_absorpt_coefficient_mu 1.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.563 _exptl_absorpt_correction_T_max 0.738 _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 15115 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4645 _reflns_number_gt 4142 _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 'CrystalStructure 3.7.0' _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. Because there are disordered atoms (O3, C9-C11, C17-C19, C20-C26), which caused abnormal bond distances or thermal parameters, constraints are used during refinements. ; _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^)+(0.0718P)^2^+8.6103P] 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 SHELXL _refine_ls_extinction_coef 0.0062(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4645 _refine_ls_number_parameters 266 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1512 _refine_ls_wR_factor_gt 0.1460 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.195 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.679831(16) 0.2500 0.69438(4) 0.03362(19) Uani 1 2 d S . . O1 O 0.65717(16) 0.14516(17) 0.6622(4) 0.0399(8) Uani 1 1 d . . . O2 O 0.7491(3) 0.2500 0.8451(6) 0.0637(17) Uani 1 2 d S . . O3 O 0.9359(5) 0.2813(5) 1.1865(10) 0.084(3) Uiso 0.50 1 d PD . . O4 O 0.7846(3) 0.2500 0.5861(7) 0.073(2) Uani 1 2 d S . . O5 O 0.6729(2) 0.2500 0.4515(5) 0.0450(13) Uani 1 2 d S . . N1 N 0.5583(3) 0.2500 0.6597(6) 0.0348(13) Uani 1 2 d S . . N2 N 0.6130(3) 0.2500 0.9075(6) 0.060(2) Uani 1 2 d SD . . C1 C 0.6099(2) 0.1056(3) 0.6784(5) 0.0389(12) Uani 1 1 d . . . C2 C 0.6160(3) 0.0425(3) 0.7295(5) 0.0407(12) Uani 1 1 d . . . C3 C 0.5641(3) 0.0064(3) 0.7504(6) 0.0546(16) Uani 1 1 d . . . H3 H 0.5681 -0.0349 0.7865 0.066 Uiso 1 1 calc R . . C4 C 0.5053(3) 0.0289(3) 0.7198(6) 0.0511(15) Uani 1 1 d . A . C5 C 0.5008(3) 0.0883(3) 0.6674(5) 0.0470(13) Uani 1 1 d . . . H5 H 0.4622 0.1040 0.6451 0.056 Uiso 1 1 calc R . . C6 C 0.5517(2) 0.1268(3) 0.6455(5) 0.0402(12) Uani 1 1 d . . . C7 C 0.5442(2) 0.1921(2) 0.5822(5) 0.0397(12) Uani 1 1 d . . . H7A H 0.5705 0.1930 0.5086 0.048 Uiso 1 1 calc R . . H7B H 0.5021 0.1958 0.5531 0.048 Uiso 1 1 calc R . . C8 C 0.5202(3) 0.2500 0.7754(8) 0.0445(18) Uani 1 2 d S . . C9 C 0.5506(5) 0.2842(6) 0.8827(12) 0.0532(19) Uani 0.50 1 d P . . C10 C 0.6100(6) 0.1881(5) 0.9662(12) 0.0532(19) Uani 0.50 1 d PD . . C11 C 0.6406(6) 0.3022(6) 0.9882(11) 0.0532(19) Uani 0.50 1 d PD . . C12 C 0.6802(3) 0.0145(3) 0.7574(6) 0.0487(14) Uani 1 1 d . . . C13 C 0.6764(4) -0.0539(3) 0.8163(7) 0.071(2) Uani 1 1 d . . . H13A H 0.6593 -0.0840 0.7564 0.107 Uiso 1 1 calc R . . H13B H 0.6506 -0.0524 0.8894 0.107 Uiso 1 1 calc R . . H13C H 0.7168 -0.0682 0.8398 0.107 Uiso 1 1 calc R . . C14 C 0.7147(3) 0.0087(4) 0.6362(7) 0.0660(18) Uani 1 1 d . . . H14A H 0.7181 0.0512 0.5980 0.099 Uiso 1 1 calc R . . H14B H 0.6931 -0.0203 0.5806 0.099 Uiso 1 1 calc R . . H14C H 0.7551 -0.0083 0.6523 0.099 Uiso 1 1 calc R . . C15 C 0.7146(3) 0.0570(3) 0.8497(7) 0.0610(17) Uani 1 1 d . . . H15A H 0.7552 0.0397 0.8621 0.092 Uiso 1 1 calc R . . H15B H 0.6931 0.0577 0.9284 0.092 Uiso 1 1 calc R . . H15C H 0.7175 0.1008 0.8172 0.092 Uiso 1 1 calc R . . C16 C 0.4470(3) -0.0124(4) 0.7473(7) 0.072(2) Uani 1 1 d D . . C17 C 0.4646(8) -0.0847(8) 0.734(2) 0.103(3) Uani 0.50 1 d PD A 1 C17' C 0.4589(9) -0.0760(9) 0.8138(18) 0.103(3) Uani 0.50 1 d PD A 2 C18 C 0.4016(13) -0.015(2) 0.642(2) 0.103(3) Uani 0.50 1 d PD A 1 C18' C 0.4093(14) -0.011(2) 0.627(2) 0.103(3) Uani 0.50 1 d PD A 2 C19 C 0.4230(9) 0.0036(11) 0.8744(15) 0.103(3) Uani 0.50 1 d PD A 1 C19' C 0.4070(9) 0.0297(9) 0.8311(19) 0.103(3) Uani 0.50 1 d PD A 2 C20 C 0.7945(4) 0.2500 0.9270(9) 0.0537(12) Uiso 1 2 d SD . . C21 C 0.8214(7) 0.1978(6) 0.9845(14) 0.0537(12) Uiso 0.50 1 d PD . . C22 C 0.8699(6) 0.2057(6) 1.0655(12) 0.0537(12) Uiso 0.50 1 d PD . . C23 C 0.8890(5) 0.2679(4) 1.0960(11) 0.0537(12) Uiso 0.50 1 d PD . . C24 C 0.8656(6) 0.3242(6) 1.0466(12) 0.0537(12) Uiso 0.50 1 d PD . . C25 C 0.8179(7) 0.3132(6) 0.9567(14) 0.0537(12) Uiso 0.50 1 d PD . . C26 C 0.9706(9) 0.2277(8) 1.2372(19) 0.099(6) Uiso 0.50 1 d PD . . C27 C 0.8229(3) 0.3057(5) 0.5947(9) 0.085(3) Uani 1 1 d . . . H27A H 0.8308 0.3171 0.6817 0.102 Uiso 1 1 calc R . . H27B H 0.8044 0.3430 0.5528 0.102 Uiso 1 1 calc R . . C28 C 0.8800(3) 0.2857(5) 0.5312(11) 0.113(4) Uani 1 1 d . . . H28A H 0.8809 0.3024 0.4458 0.136 Uiso 1 1 calc R . . H28B H 0.9156 0.3024 0.5759 0.136 Uiso 1 1 calc R . . C29 C 0.6854(3) 0.3062(3) 0.3755(7) 0.069(2) Uani 1 1 d . . . H29A H 0.7014 0.3417 0.4266 0.082 Uiso 1 1 calc R . . H29B H 0.6481 0.3211 0.3342 0.082 Uiso 1 1 calc R . . C30 C 0.7317(4) 0.2853(4) 0.2809(7) 0.081(2) Uani 1 1 d . . . H30A H 0.7209 0.3018 0.1984 0.097 Uiso 1 1 calc R . . H30B H 0.7721 0.3018 0.3032 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0271(3) 0.0401(3) 0.0337(3) 0.000 -0.00020(15) 0.000 O1 0.0340(18) 0.0396(19) 0.046(2) 0.0045(16) -0.0013(16) -0.0025(15) O2 0.043(3) 0.102(5) 0.046(3) 0.000 -0.020(3) 0.000 O4 0.036(3) 0.111(6) 0.072(5) 0.000 0.012(3) 0.000 O5 0.053(3) 0.049(3) 0.033(3) 0.000 0.008(2) 0.000 N1 0.025(3) 0.044(3) 0.035(3) 0.000 0.002(2) 0.000 N2 0.032(3) 0.114(6) 0.033(4) 0.000 -0.002(3) 0.000 C1 0.042(3) 0.039(3) 0.036(3) -0.003(2) 0.003(2) -0.006(2) C2 0.047(3) 0.042(3) 0.033(3) -0.002(2) -0.001(2) -0.001(2) C3 0.077(5) 0.042(3) 0.045(3) 0.001(3) 0.006(3) -0.012(3) C4 0.051(3) 0.054(3) 0.049(3) -0.007(3) 0.004(3) -0.020(3) C5 0.039(3) 0.052(3) 0.050(3) -0.003(3) -0.002(2) -0.014(2) C6 0.038(3) 0.045(3) 0.038(3) -0.005(2) 0.000(2) -0.006(2) C7 0.031(2) 0.045(3) 0.043(3) -0.001(2) -0.006(2) -0.003(2) C8 0.030(4) 0.061(5) 0.042(4) 0.000 0.004(3) 0.000 C9 0.042(4) 0.068(4) 0.050(4) -0.002(4) 0.014(4) 0.004(3) C10 0.042(4) 0.068(4) 0.050(4) -0.002(4) 0.014(4) 0.004(3) C11 0.042(4) 0.068(4) 0.050(4) -0.002(4) 0.014(4) 0.004(3) C12 0.060(4) 0.042(3) 0.043(3) 0.001(3) 0.002(3) 0.001(3) C13 0.095(6) 0.040(3) 0.079(5) 0.006(3) -0.002(4) 0.014(3) C14 0.058(4) 0.076(4) 0.064(4) 0.002(4) 0.007(4) 0.018(3) C15 0.064(4) 0.059(4) 0.060(4) 0.005(3) -0.015(3) 0.008(3) C16 0.077(5) 0.073(5) 0.067(5) -0.003(4) 0.015(4) -0.040(4) C17 0.092(5) 0.128(6) 0.088(6) 0.011(5) 0.009(5) -0.066(5) C17' 0.092(5) 0.128(6) 0.088(6) 0.011(5) 0.009(5) -0.066(5) C18 0.092(5) 0.128(6) 0.088(6) 0.011(5) 0.009(5) -0.066(5) C18' 0.092(5) 0.128(6) 0.088(6) 0.011(5) 0.009(5) -0.066(5) C19 0.092(5) 0.128(6) 0.088(6) 0.011(5) 0.009(5) -0.066(5) C19' 0.092(5) 0.128(6) 0.088(6) 0.011(5) 0.009(5) -0.066(5) C27 0.057(4) 0.110(7) 0.088(6) 0.012(5) 0.011(4) -0.014(4) C28 0.045(4) 0.149(8) 0.145(9) 0.032(7) 0.009(5) -0.006(4) C29 0.088(5) 0.056(4) 0.062(4) 0.015(3) 0.018(4) 0.005(3) C30 0.093(6) 0.088(5) 0.062(5) 0.000(4) 0.024(4) -0.017(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 Nd1 O2 2.223(6) . ? Nd1 O1 2.246(3) 3 ? Nd1 O1 2.246(3) . ? Nd1 O4 2.580(6) . ? Nd1 O5 2.616(5) . ? Nd1 N1 2.695(6) . ? Nd1 N2 2.722(7) . ? O1 C1 1.333(6) . ? O2 C20 1.330(10) . ? O3 C26 0.955(18) 3 ? O3 O3 1.29(2) 3 ? O3 C23 1.444(13) . ? O3 C26 1.449(14) . ? O3 C23 1.743(13) 3 ? O4 C27 1.428(9) . ? O4 C27 1.428(9) 3 ? O5 C29 1.445(7) . ? O5 C29 1.445(7) 3 ? N1 C7 1.489(6) . ? N1 C7 1.489(6) 3 ? N1 C8 1.500(10) . ? N2 C10 1.425(8) 3 ? N2 C10 1.425(8) . ? N2 C11 1.510(9) . ? N2 C11 1.510(9) 3 ? N2 C9 1.564(13) 3 ? N2 C9 1.564(13) . ? C1 C6 1.396(7) . ? C1 C2 1.419(8) . ? C2 C3 1.381(8) . ? C2 C12 1.553(8) . ? C3 C4 1.412(9) . ? C3 H3 0.9400 . ? C4 C5 1.352(9) . ? C4 C16 1.567(8) . ? C5 C6 1.392(7) . ? C5 H5 0.9400 . ? C6 C7 1.518(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.509(15) . ? C8 C9 1.509(14) 3 ? C9 C9 1.41(3) 3 ? C9 C10 1.683(18) 3 ? C10 C11 0.740(15) 3 ? C10 C9 1.683(18) 3 ? C11 C10 0.740(14) 3 ? C12 C14 1.513(9) . ? C12 C15 1.526(9) . ? C12 C13 1.548(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C19 1.502(16) . ? C16 C18 1.508(17) . ? C16 C17' 1.518(16) . ? C16 C18' 1.538(17) . ? C16 C17 1.547(16) . ? C16 C19' 1.529(17) . ? C20 C21 1.374(13) 3 ? C20 C21 1.374(13) . ? C20 C25 1.438(12) . ? C20 C25 1.438(12) 3 ? C21 C25 0.38(2) 3 ? C21 C24 1.264(18) 3 ? C21 C22 1.387(14) . ? C21 C23 2.036(16) 3 ? C22 C24 0.657(14) 3 ? C22 C23 0.760(13) 3 ? C22 C23 1.388(14) . ? C22 C25 1.683(18) 3 ? C22 C22 1.83(2) 3 ? C23 C23 0.739(18) 3 ? C23 C22 0.760(13) 3 ? C23 C24 1.377(13) . ? C23 O3 1.743(13) 3 ? C23 C21 2.036(16) 3 ? C23 C24 2.039(15) 3 ? C24 C22 0.657(14) 3 ? C24 C21 1.264(18) 3 ? C24 C25 1.444(14) . ? C24 C23 2.039(15) 3 ? C25 C21 0.38(2) 3 ? C25 C22 1.683(18) 3 ? C26 C26 0.92(3) 3 ? C26 O3 0.955(18) 3 ? C27 C28 1.487(11) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C28 1.475(19) 3 ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.503(10) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 C30 1.456(16) 3 ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nd1 O1 105.32(9) . 3 ? O2 Nd1 O1 105.32(9) . . ? O1 Nd1 O1 148.66(18) 3 . ? O2 Nd1 O4 73.6(2) . . ? O1 Nd1 O4 97.37(10) 3 . ? O1 Nd1 O4 97.37(10) . . ? O2 Nd1 O5 140.1(2) . . ? O1 Nd1 O5 80.39(10) 3 . ? O1 Nd1 O5 80.39(10) . . ? O4 Nd1 O5 66.5(2) . . ? O2 Nd1 N1 141.2(2) . . ? O1 Nd1 N1 76.06(9) 3 . ? O1 Nd1 N1 76.06(9) . . ? O4 Nd1 N1 145.2(2) . . ? O5 Nd1 N1 78.71(17) . . ? O2 Nd1 N2 75.9(2) . . ? O1 Nd1 N2 90.59(10) 3 . ? O1 Nd1 N2 90.59(10) . . ? O4 Nd1 N2 149.5(2) . . ? O5 Nd1 N2 144.00(18) . . ? N1 Nd1 N2 65.29(19) . . ? C1 O1 Nd1 137.9(3) . . ? C20 O2 Nd1 174.7(6) . . ? C26 O3 O3 78.9(13) 3 3 ? C26 O3 C23 156.6(17) 3 . ? O3 O3 C23 79.0(6) 3 . ? C26 O3 C26 38.6(15) 3 . ? O3 O3 C26 40.3(8) 3 . ? C23 O3 C26 118.9(11) . . ? C26 O3 C23 132.7(16) 3 3 ? O3 O3 C23 54.4(5) 3 3 ? C23 O3 C23 24.6(6) . 3 ? C26 O3 C23 94.4(10) . 3 ? C27 O4 C27 107.3(8) . 3 ? C27 O4 Nd1 119.8(4) . . ? C27 O4 Nd1 119.8(4) 3 . ? C29 O5 C29 106.7(7) . 3 ? C29 O5 Nd1 123.6(4) . . ? C29 O5 Nd1 123.6(4) 3 . ? C7 N1 C7 106.6(6) . 3 ? C7 N1 C8 110.3(4) . . ? C7 N1 C8 110.3(4) 3 . ? C7 N1 Nd1 106.5(3) . . ? C7 N1 Nd1 106.5(3) 3 . ? C8 N1 Nd1 116.0(4) . . ? C10 N2 C10 127.1(12) 3 . ? C10 N2 C11 29.0(6) 3 . ? C10 N2 C11 113.7(9) . . ? C10 N2 C11 113.7(9) 3 3 ? C10 N2 C11 29.0(6) . 3 ? C11 N2 C11 90.9(11) . 3 ? C10 N2 C9 116.0(8) 3 3 ? C10 N2 C9 68.4(8) . 3 ? C11 N2 C9 140.5(8) . 3 ? C11 N2 C9 97.4(7) 3 3 ? C10 N2 C9 68.4(8) 3 . ? C10 N2 C9 116.0(8) . . ? C11 N2 C9 97.4(7) . . ? C11 N2 C9 140.5(8) 3 . ? C9 N2 C9 53.6(10) 3 . ? C10 N2 Nd1 113.4(6) 3 . ? C10 N2 Nd1 113.4(6) . . ? C11 N2 Nd1 105.5(6) . . ? C11 N2 Nd1 105.5(6) 3 . ? C9 N2 Nd1 109.2(5) 3 . ? C9 N2 Nd1 109.2(5) . . ? O1 C1 C6 119.3(5) . . ? O1 C1 C2 122.5(5) . . ? C6 C1 C2 118.2(5) . . ? C3 C2 C1 118.6(5) . . ? C3 C2 C12 121.1(5) . . ? C1 C2 C12 120.3(5) . . ? C2 C3 C4 122.7(6) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? C5 C4 C3 117.5(5) . . ? C5 C4 C16 120.8(6) . . ? C3 C4 C16 121.7(6) . . ? C4 C5 C6 122.0(6) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 120.9(5) . . ? C5 C6 C7 119.7(5) . . ? C1 C6 C7 119.4(4) . . ? N1 C7 C6 116.0(4) . . ? N1 C7 H7A 108.3 . . ? C6 C7 H7A 108.3 . . ? N1 C7 H7B 108.3 . . ? C6 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? N1 C8 C9 112.7(7) . . ? N1 C8 C9 112.7(7) . 3 ? C9 C8 C9 55.8(10) . 3 ? C9 C9 C8 62.1(5) 3 . ? C9 C9 N2 63.2(5) 3 . ? C8 C9 N2 107.9(8) . . ? C9 C9 C10 109.8(6) 3 3 ? C8 C9 C10 155.5(9) . 3 ? N2 C9 C10 51.9(5) . 3 ? C11 C10 N2 81.8(10) 3 . ? C11 C10 C9 141.5(13) 3 3 ? N2 C10 C9 59.7(6) . 3 ? C10 C11 N2 69.2(9) 3 . ? C14 C12 C15 110.9(6) . . ? C14 C12 C13 107.9(5) . . ? C15 C12 C13 106.6(6) . . ? C14 C12 C2 108.5(5) . . ? C15 C12 C2 111.2(5) . . ? C13 C12 C2 111.7(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C16 C18 117.3(18) . . ? C19 C16 C17' 79.8(13) . . ? C18 C16 C17' 115.6(19) . . ? C19 C16 C18' 125(2) . . ? C18 C16 C18' 9.4(18) . . ? C17' C16 C18' 120(2) . . ? C19 C16 C17 112.6(13) . . ? C18 C16 C17 93(2) . . ? C17' C16 C17 33.5(9) . . ? C18' C16 C17 94(2) . . ? C19 C16 C19' 30.3(11) . . ? C18 C16 C19' 95(2) . . ? C17' C16 C19' 108.2(12) . . ? C18' C16 C19' 100(2) . . ? C17 C16 C19' 138.2(12) . . ? C19 C16 C4 109.8(8) . . ? C18 C16 C4 114.9(11) . . ? C17' C16 C4 114.7(9) . . ? C18' C16 C4 105.8(10) . . ? C17 C16 C4 107.6(8) . . ? C19' C16 C4 105.8(8) . . ? O2 C20 C21 128.3(6) . 3 ? O2 C20 C21 128.3(6) . . ? C21 C20 C21 103.0(12) 3 . ? O2 C20 C25 114.5(6) . . ? C21 C20 C25 15.5(8) 3 . ? C21 C20 C25 117.2(9) . . ? O2 C20 C25 114.5(6) . 3 ? C21 C20 C25 117.2(9) 3 3 ? C21 C20 C25 15.5(8) . 3 ? C25 C20 C25 130.2(13) . 3 ? C25 C21 C24 111(4) 3 3 ? C25 C21 C20 92(3) 3 . ? C24 C21 C20 148.2(13) 3 . ? C25 C21 C22 135(4) 3 . ? C24 C21 C22 28.2(7) 3 . ? C20 C21 C22 121.4(12) . . ? C25 C21 C23 144(4) 3 3 ? C24 C21 C23 41.6(7) 3 3 ? C20 C21 C23 107.9(9) . 3 ? C22 C21 C23 13.6(7) . 3 ? C24 C22 C23 152(3) 3 3 ? C24 C22 C21 65.4(16) 3 . ? C23 C22 C21 141.1(18) 3 . ? C24 C22 C23 170(2) 3 . ? C23 C22 C23 21.8(9) 3 . ? C21 C22 C23 119.2(12) . . ? C24 C22 C25 57.8(15) 3 3 ? C23 C22 C25 147.2(18) 3 3 ? C21 C22 C25 9.2(9) . 3 ? C23 C22 C25 125.7(11) . 3 ? C24 C22 C22 160.0(17) 3 3 ? C23 C22 C22 44.3(13) 3 3 ? C21 C22 C22 96.7(7) . 3 ? C23 C22 C22 22.5(7) . 3 ? C25 C22 C22 103.5(6) 3 3 ? C23 C23 C22 135.7(13) 3 3 ? C23 C23 C24 147.5(7) 3 . ? C22 C23 C24 12.8(13) 3 . ? C23 C23 C22 22.5(7) 3 . ? C22 C23 C22 113.1(19) 3 . ? C24 C23 C22 125.2(11) . . ? C23 C23 O3 101.0(6) 3 . ? C22 C23 O3 123.1(16) 3 . ? C24 C23 O3 111.4(9) . . ? C22 C23 O3 123.4(10) . . ? C23 C23 O3 54.4(5) 3 3 ? C22 C23 O3 169.1(16) 3 3 ? C24 C23 O3 158.0(9) . 3 ? C22 C23 O3 76.8(8) . 3 ? O3 C23 O3 46.6(9) . 3 ? C23 C23 C21 110.3(4) 3 3 ? C22 C23 C21 25.4(12) 3 3 ? C24 C23 C21 37.6(7) . 3 ? C22 C23 C21 87.8(9) . 3 ? O3 C23 C21 148.4(8) . 3 ? O3 C23 C21 164.2(8) 3 3 ? C23 C23 C24 21.2(5) 3 3 ? C22 C23 C24 114.6(15) 3 3 ? C24 C23 C24 126.3(11) . 3 ? C22 C23 C24 3.2(8) . 3 ? O3 C23 C24 122.2(8) . 3 ? O3 C23 C24 75.6(6) 3 3 ? C21 C23 C24 89.2(6) 3 3 ? C22 C24 C21 86.4(18) 3 3 ? C22 C24 C23 14.9(14) 3 . ? C21 C24 C23 100.8(11) 3 . ? C22 C24 C25 99.5(19) 3 . ? C21 C24 C25 14.4(9) 3 . ? C23 C24 C25 113.4(11) . . ? C22 C24 C23 6.8(17) 3 3 ? C21 C24 C23 89.8(10) 3 3 ? C23 C24 C23 11.2(3) . 3 ? C25 C24 C23 102.2(9) . 3 ? C21 C25 C20 73(3) 3 . ? C21 C25 C24 55(3) 3 . ? C20 C25 C24 123.4(11) . . ? C21 C25 C22 35(3) 3 3 ? C20 C25 C22 100.7(9) . 3 ? C24 C25 C22 22.7(6) . 3 ? C26 C26 O3 101.1(13) 3 3 ? C26 C26 O3 40.3(8) 3 . ? O3 C26 O3 60.8(15) 3 . ? O4 C27 C28 104.1(8) . . ? O4 C27 H27A 110.9 . . ? C28 C27 H27A 110.9 . . ? O4 C27 H27B 110.9 . . ? C28 C27 H27B 110.9 . . ? H27A C27 H27B 108.9 . . ? C28 C28 C27 106.1(5) 3 . ? C28 C28 H28A 110.5 3 . ? C27 C28 H28A 110.5 . . ? C28 C28 H28B 110.5 3 . ? C27 C28 H28B 110.5 . . ? H28A C28 H28B 108.7 . . ? O5 C29 C30 106.3(6) . . ? O5 C29 H29A 110.5 . . ? C30 C29 H29A 110.5 . . ? O5 C29 H29B 110.5 . . ? C30 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? C30 C30 C29 106.7(4) 3 . ? C30 C30 H30A 110.4 3 . ? C29 C30 H30A 110.4 . . ? C30 C30 H30B 110.4 3 . ? C29 C30 H30B 110.4 . . ? H30A C30 H30B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.964 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.191 #===================================================end data_complex8 _database_code_depnum_ccdc_archive 'CCDC 763751' #TrackingRef 'NieKun-dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H77 N2 O6 Sm' _chemical_formula_sum 'C49 H77 N2 O6 Sm' _chemical_formula_weight 940.48 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 orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x, -y+1/2, z' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z-1/2' '-x, y-1/2, -z' 'x-1/2, y, -z-1/2' _cell_length_a 21.9170(12) _cell_length_b 20.6367(10) _cell_length_c 10.7274(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4851.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 12998 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1980 _exptl_absorpt_coefficient_mu 1.257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.397 _exptl_absorpt_correction_T_max 0.528 _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 16286 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4610 _reflns_number_gt 4259 _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. Because there are disordered atoms (O3, C9-C11, C17-C19, C20-C26), which caused abnormal bond distances or thermal parameters, constraints are used during refinements. ; _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^)+(0.0485P)^2^+16.5227P] 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 4610 _refine_ls_number_parameters 265 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.678379(16) 0.2500 0.69626(3) 0.02958(14) Uani 1 2 d S . . O1 O 0.65701(16) 0.14625(17) 0.6637(3) 0.0357(8) Uani 1 1 d . . . O2 O 0.7470(3) 0.2500 0.8446(5) 0.0587(17) Uani 1 2 d S . . O3 O 0.9350(5) 0.2797(5) 1.1879(10) 0.080(3) Uiso 0.50 1 d PD . . O4 O 0.7827(3) 0.2500 0.5889(6) 0.0683(19) Uani 1 2 d S . . O5 O 0.6718(3) 0.2500 0.4552(5) 0.0434(13) Uani 1 2 d S . . N1 N 0.5585(3) 0.2500 0.6608(6) 0.0335(13) Uani 1 2 d S . . N2 N 0.6124(3) 0.2500 0.9078(6) 0.057(2) Uani 1 2 d SD . . C1 C 0.6101(3) 0.1064(3) 0.6794(5) 0.0360(12) Uani 1 1 d . . . C2 C 0.6167(3) 0.0427(3) 0.7309(5) 0.0408(13) Uani 1 1 d . . . C3 C 0.5634(3) 0.0068(3) 0.7503(5) 0.0528(16) Uani 1 1 d . . . H3 H 0.5671 -0.0346 0.7861 0.063 Uiso 1 1 calc R . . C4 C 0.5049(3) 0.0287(3) 0.7197(6) 0.0522(16) Uani 1 1 d . A . C5 C 0.5007(3) 0.0884(3) 0.6665(5) 0.0461(14) Uani 1 1 d . . . H5 H 0.4620 0.1040 0.6433 0.055 Uiso 1 1 calc R . . C6 C 0.5514(2) 0.1273(3) 0.6451(5) 0.0375(12) Uani 1 1 d . . . C7 C 0.5432(2) 0.1923(3) 0.5832(5) 0.0387(12) Uani 1 1 d . . . H7A H 0.5686 0.1933 0.5081 0.046 Uiso 1 1 calc R . . H7B H 0.5006 0.1961 0.5565 0.046 Uiso 1 1 calc R . . C8 C 0.5193(3) 0.2500 0.7747(7) 0.0404(18) Uani 1 2 d S . . C9 C 0.5495(6) 0.2846(6) 0.8823(12) 0.053(2) Uani 0.50 1 d P . . C10 C 0.6102(6) 0.1886(5) 0.9689(13) 0.053(2) Uani 0.50 1 d PD . . C11 C 0.6406(6) 0.3023(6) 0.9882(12) 0.053(2) Uani 0.50 1 d PD . . C12 C 0.6805(3) 0.0153(3) 0.7582(6) 0.0475(14) Uani 1 1 d . . . C13 C 0.6771(4) -0.0534(3) 0.8162(7) 0.074(2) Uani 1 1 d . . . H13A H 0.7180 -0.0686 0.8348 0.111 Uiso 1 1 calc R . . H13B H 0.6578 -0.0828 0.7576 0.111 Uiso 1 1 calc R . . H13C H 0.6533 -0.0518 0.8924 0.111 Uiso 1 1 calc R . . C14 C 0.7155(4) 0.0099(4) 0.6357(6) 0.068(2) Uani 1 1 d . . . H14A H 0.7187 0.0524 0.5976 0.102 Uiso 1 1 calc R . . H14B H 0.6941 -0.0192 0.5798 0.102 Uiso 1 1 calc R . . H14C H 0.7561 -0.0069 0.6518 0.102 Uiso 1 1 calc R . . C15 C 0.7149(3) 0.0571(3) 0.8500(6) 0.0583(17) Uani 1 1 d . . . H15A H 0.7196 0.1004 0.8160 0.087 Uiso 1 1 calc R . . H15B H 0.7549 0.0385 0.8651 0.087 Uiso 1 1 calc R . . H15C H 0.6924 0.0594 0.9277 0.087 Uiso 1 1 calc R . . C16 C 0.4472(4) -0.0129(4) 0.7456(7) 0.076(2) Uani 1 1 d D . . C17 C 0.4653(9) -0.0851(8) 0.7350(19) 0.099(3) Uani 0.50 1 d PD A 1 C17' C 0.4606(9) -0.0770(8) 0.8092(17) 0.099(3) Uani 0.50 1 d PD A 2 C18 C 0.4010(12) -0.015(2) 0.642(2) 0.099(3) Uani 0.50 1 d PD A 1 C18' C 0.4097(13) -0.011(2) 0.624(2) 0.099(3) Uani 0.50 1 d PD A 2 C19 C 0.4238(10) -0.0002(10) 0.8753(14) 0.099(3) Uani 0.50 1 d PD A 1 C19' C 0.4079(9) 0.0297(9) 0.8356(17) 0.099(3) Uani 0.50 1 d PD A 2 C20 C 0.7930(4) 0.2500 0.9264(8) 0.0492(11) Uiso 1 2 d SD . . C21 C 0.8200(7) 0.1989(6) 0.9819(13) 0.0492(11) Uiso 0.50 1 d PD . . C22 C 0.8682(6) 0.2054(6) 1.0655(12) 0.0492(11) Uiso 0.50 1 d PD . . C23 C 0.8876(5) 0.2674(4) 1.0977(10) 0.0492(11) Uiso 0.50 1 d PD . . C24 C 0.8633(6) 0.3238(6) 1.0475(12) 0.0492(11) Uiso 0.50 1 d PD . . C25 C 0.8155(7) 0.3134(6) 0.9575(13) 0.0492(11) Uiso 0.50 1 d PD . . C26 C 0.9694(9) 0.2276(7) 1.2358(17) 0.092(6) Uiso 0.50 1 d PD . . C27 C 0.8214(3) 0.3056(5) 0.5981(8) 0.082(3) Uani 1 1 d . . . H27A H 0.8292 0.3167 0.6855 0.099 Uiso 1 1 calc R . . H27B H 0.8030 0.3430 0.5564 0.099 Uiso 1 1 calc R . . C28 C 0.8781(4) 0.2858(5) 0.5352(10) 0.115(4) Uani 1 1 d . . . H28A H 0.9138 0.3025 0.5801 0.138 Uiso 1 1 calc R . . H28B H 0.8791 0.3025 0.4497 0.138 Uiso 1 1 calc R . . C29 C 0.6849(4) 0.3060(3) 0.3794(6) 0.0633(19) Uani 1 1 d . . . H29A H 0.7016 0.3411 0.4309 0.076 Uiso 1 1 calc R . . H29B H 0.6476 0.3216 0.3388 0.076 Uiso 1 1 calc R . . C30 C 0.7304(4) 0.2852(4) 0.2845(6) 0.074(2) Uani 1 1 d . . . H30A H 0.7191 0.3017 0.2020 0.089 Uiso 1 1 calc R . . H30B H 0.7710 0.3017 0.3057 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0253(2) 0.0338(2) 0.0296(2) 0.000 -0.00080(15) 0.000 O1 0.0312(18) 0.0340(18) 0.042(2) 0.0031(16) -0.0010(16) -0.0049(16) O2 0.035(3) 0.098(5) 0.043(3) 0.000 -0.021(3) 0.000 O4 0.029(3) 0.116(6) 0.060(4) 0.000 0.010(3) 0.000 O5 0.058(4) 0.042(3) 0.031(3) 0.000 0.007(3) 0.000 N1 0.024(3) 0.041(3) 0.035(3) 0.000 0.000(3) 0.000 N2 0.032(4) 0.108(6) 0.030(3) 0.000 -0.004(3) 0.000 C1 0.042(3) 0.036(3) 0.030(2) -0.007(2) 0.000(2) -0.005(2) C2 0.055(4) 0.037(3) 0.030(3) -0.003(2) 0.002(3) -0.004(3) C3 0.081(5) 0.039(3) 0.038(3) -0.001(3) 0.007(3) -0.019(3) C4 0.058(4) 0.053(4) 0.045(3) -0.004(3) 0.003(3) -0.021(3) C5 0.043(3) 0.055(4) 0.041(3) -0.009(3) -0.001(3) -0.014(3) C6 0.038(3) 0.041(3) 0.034(3) -0.004(2) -0.002(2) -0.008(2) C7 0.029(3) 0.047(3) 0.040(3) 0.000(2) -0.006(2) -0.004(2) C8 0.027(4) 0.057(5) 0.038(4) 0.000 0.005(3) 0.000 C9 0.044(5) 0.060(4) 0.055(4) -0.004(4) 0.020(4) 0.005(3) C10 0.044(5) 0.060(4) 0.055(4) -0.004(4) 0.020(4) 0.005(3) C11 0.044(5) 0.060(4) 0.055(4) -0.004(4) 0.020(4) 0.005(3) C12 0.065(4) 0.034(3) 0.044(3) 0.001(3) 0.001(3) 0.010(3) C13 0.107(7) 0.037(3) 0.079(5) 0.008(3) 0.004(5) 0.013(4) C14 0.070(5) 0.080(5) 0.054(4) -0.002(4) 0.010(4) 0.026(4) C15 0.067(4) 0.053(4) 0.055(4) 0.004(3) -0.015(3) 0.009(3) C16 0.088(6) 0.080(5) 0.060(4) -0.003(4) 0.017(4) -0.057(5) C17 0.100(5) 0.118(6) 0.078(5) 0.007(5) 0.014(5) -0.067(5) C17' 0.100(5) 0.118(6) 0.078(5) 0.007(5) 0.014(5) -0.067(5) C18 0.100(5) 0.118(6) 0.078(5) 0.007(5) 0.014(5) -0.067(5) C18' 0.100(5) 0.118(6) 0.078(5) 0.007(5) 0.014(5) -0.067(5) C19 0.100(5) 0.118(6) 0.078(5) 0.007(5) 0.014(5) -0.067(5) C19' 0.100(5) 0.118(6) 0.078(5) 0.007(5) 0.014(5) -0.067(5) C27 0.052(4) 0.117(7) 0.078(5) 0.013(5) 0.007(4) -0.020(5) C28 0.047(4) 0.161(10) 0.137(8) 0.034(7) 0.013(5) -0.011(5) C29 0.085(5) 0.053(4) 0.052(4) 0.018(3) 0.015(4) 0.006(4) C30 0.087(6) 0.084(5) 0.052(4) 0.002(4) 0.022(4) -0.013(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 2.189(5) . ? Sm1 O1 2.219(3) . ? Sm1 O1 2.219(3) 3 ? Sm1 O4 2.560(6) . ? Sm1 O5 2.590(5) . ? Sm1 N1 2.656(6) . ? Sm1 N2 2.691(7) . ? O1 C1 1.328(6) . ? O2 C20 1.336(10) . ? O3 C26 0.926(18) 3 ? O3 O3 1.22(2) 3 ? O3 C26 1.409(14) . ? O3 C23 1.443(12) . ? O3 C23 1.721(13) 3 ? O4 C27 1.431(9) . ? O4 C27 1.431(9) 3 ? O5 C29 1.442(7) . ? O5 C29 1.442(7) 3 ? N1 C7 1.491(6) . ? N1 C7 1.491(6) 3 ? N1 C8 1.494(9) . ? N2 C10 1.428(8) 3 ? N2 C10 1.428(8) . ? N2 C11 1.513(9) . ? N2 C11 1.513(9) 3 ? N2 C9 1.577(14) 3 ? N2 C9 1.577(14) . ? C1 C6 1.406(8) . ? C1 C2 1.434(7) . ? C2 C3 1.399(8) . ? C2 C12 1.536(9) . ? C3 C4 1.398(10) . ? C3 H3 0.9400 . ? C4 C5 1.363(9) . ? C4 C16 1.553(9) . ? C5 C6 1.390(8) . ? C5 H5 0.9400 . ? C6 C7 1.507(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.511(15) . ? C8 C9 1.511(15) 3 ? C9 C9 1.43(3) 3 ? C9 C10 1.713(19) 3 ? C10 C11 0.725(16) 3 ? C10 C9 1.713(19) 3 ? C11 C10 0.725(16) 3 ? C12 C15 1.511(9) . ? C12 C14 1.526(9) . ? C12 C13 1.550(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C18 1.504(17) . ? C16 C19 1.506(15) . ? C16 C17' 1.518(16) . ? C16 C18' 1.544(17) . ? C16 C17 1.546(16) . ? C16 C19' 1.563(16) . ? C20 C21 1.348(12) 3 ? C20 C21 1.348(12) . ? C20 C25 1.437(12) . ? C20 C25 1.437(12) 3 ? C21 C25 0.38(2) 3 ? C21 C24 1.272(18) 3 ? C21 C22 1.392(14) . ? C22 C24 0.641(14) 3 ? C22 C23 0.785(13) 3 ? C22 C23 1.392(13) . ? C22 C25 1.681(18) 3 ? C22 C22 1.84(2) 3 ? C23 C23 0.717(18) 3 ? C23 C22 0.785(13) 3 ? C23 C24 1.388(13) . ? C23 O3 1.721(13) 3 ? C23 C24 2.028(15) 3 ? C24 C22 0.641(14) 3 ? C24 C21 1.272(18) 3 ? C24 C25 1.442(14) . ? C24 C23 2.028(15) 3 ? C25 C21 0.38(2) 3 ? C25 C22 1.681(18) 3 ? C26 C26 0.92(3) 3 ? C26 O3 0.926(18) 3 ? C27 C28 1.471(11) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C28 1.48(2) 3 ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.489(10) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 C30 1.451(15) 3 ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Sm1 O1 105.02(9) . . ? O2 Sm1 O1 105.02(9) . 3 ? O1 Sm1 O1 149.49(18) . 3 ? O2 Sm1 O4 73.3(2) . . ? O1 Sm1 O4 96.76(10) . . ? O1 Sm1 O4 96.76(10) 3 . ? O2 Sm1 O5 139.8(2) . . ? O1 Sm1 O5 80.29(10) . . ? O1 Sm1 O5 80.29(10) 3 . ? O4 Sm1 O5 66.5(2) . . ? O2 Sm1 N1 141.6(2) . . ? O1 Sm1 N1 76.63(9) . . ? O1 Sm1 N1 76.63(9) 3 . ? O4 Sm1 N1 145.0(2) . . ? O5 Sm1 N1 78.58(18) . . ? O2 Sm1 N2 75.9(2) . . ? O1 Sm1 N2 91.10(10) . . ? O1 Sm1 N2 91.10(10) 3 . ? O4 Sm1 N2 149.2(2) . . ? O5 Sm1 N2 144.32(19) . . ? N1 Sm1 N2 65.74(19) . . ? C1 O1 Sm1 137.8(3) . . ? C20 O2 Sm1 174.5(6) . . ? C26 O3 O3 80.6(13) 3 3 ? C26 O3 C26 40.2(16) 3 . ? O3 O3 C26 40.4(8) 3 . ? C26 O3 C23 158.6(17) 3 . ? O3 O3 C23 79.9(6) 3 . ? C26 O3 C23 119.8(11) . . ? C26 O3 C23 135.5(16) 3 3 ? O3 O3 C23 55.6(5) 3 3 ? C26 O3 C23 95.7(10) . 3 ? C23 O3 C23 24.2(6) . 3 ? C27 O4 C27 106.6(8) . 3 ? C27 O4 Sm1 119.9(4) . . ? C27 O4 Sm1 119.9(4) 3 . ? C29 O5 C29 106.6(6) . 3 ? C29 O5 Sm1 123.5(4) . . ? C29 O5 Sm1 123.5(4) 3 . ? C7 N1 C7 106.0(5) . 3 ? C7 N1 C8 109.1(4) . . ? C7 N1 C8 109.1(4) 3 . ? C7 N1 Sm1 107.6(3) . . ? C7 N1 Sm1 107.6(3) 3 . ? C8 N1 Sm1 116.9(4) . . ? C10 N2 C10 125.2(12) 3 . ? C10 N2 C11 28.3(6) 3 . ? C10 N2 C11 112.7(9) . . ? C10 N2 C11 112.7(9) 3 3 ? C10 N2 C11 28.3(6) . 3 ? C11 N2 C11 90.9(12) . 3 ? C10 N2 C9 116.8(8) 3 3 ? C10 N2 C9 69.3(8) . 3 ? C11 N2 C9 141.2(8) . 3 ? C11 N2 C9 97.6(7) 3 3 ? C10 N2 C9 69.3(8) 3 . ? C10 N2 C9 116.8(8) . . ? C11 N2 C9 97.6(7) . . ? C11 N2 C9 141.2(8) 3 . ? C9 N2 C9 53.9(10) 3 . ? C10 N2 Sm1 113.9(6) 3 . ? C10 N2 Sm1 113.9(6) . . ? C11 N2 Sm1 105.1(6) . . ? C11 N2 Sm1 105.1(6) 3 . ? C9 N2 Sm1 108.9(5) 3 . ? C9 N2 Sm1 108.9(5) . . ? O1 C1 C6 119.0(5) . . ? O1 C1 C2 122.5(5) . . ? C6 C1 C2 118.4(5) . . ? C3 C2 C1 117.2(6) . . ? C3 C2 C12 122.5(5) . . ? C1 C2 C12 120.2(5) . . ? C4 C3 C2 124.1(6) . . ? C4 C3 H3 117.9 . . ? C2 C3 H3 117.9 . . ? C5 C4 C3 116.9(6) . . ? C5 C4 C16 121.2(7) . . ? C3 C4 C16 121.8(6) . . ? C4 C5 C6 122.5(6) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 120.7(5) . . ? C5 C6 C7 119.4(5) . . ? C1 C6 C7 119.9(5) . . ? N1 C7 C6 116.0(4) . . ? N1 C7 H7A 108.3 . . ? C6 C7 H7A 108.3 . . ? N1 C7 H7B 108.3 . . ? C6 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? N1 C8 C9 111.9(6) . . ? N1 C8 C9 111.9(6) . 3 ? C9 C8 C9 56.5(10) . 3 ? C9 C9 C8 61.8(5) 3 . ? C9 C9 N2 63.0(5) 3 . ? C8 C9 N2 107.6(8) . . ? C9 C9 C10 108.8(6) 3 3 ? C8 C9 C10 155.2(9) . 3 ? N2 C9 C10 51.3(5) . 3 ? C11 C10 N2 82.3(11) 3 . ? C11 C10 C9 141.8(13) 3 3 ? N2 C10 C9 59.4(6) . 3 ? C10 C11 N2 69.3(10) 3 . ? C15 C12 C14 110.6(6) . . ? C15 C12 C2 111.6(5) . . ? C14 C12 C2 108.6(5) . . ? C15 C12 C13 106.6(5) . . ? C14 C12 C13 107.7(5) . . ? C2 C12 C13 111.6(6) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C19 117.3(16) . . ? C18 C16 C17' 115.9(18) . . ? C19 C16 C17' 78.5(12) . . ? C18 C16 C18' 10.6(17) . . ? C19 C16 C18' 126.7(18) . . ? C17' C16 C18' 120.1(19) . . ? C18 C16 C17 95(2) . . ? C19 C16 C17 108.8(12) . . ? C17' C16 C17 31.0(8) . . ? C18' C16 C17 95(2) . . ? C18 C16 C4 115.7(10) . . ? C19 C16 C4 110.3(8) . . ? C17' C16 C4 113.8(9) . . ? C18' C16 C4 105.8(10) . . ? C17 C16 C4 108.0(9) . . ? C18 C16 C19' 96(2) . . ? C19 C16 C19' 31.2(10) . . ? C17' C16 C19' 108.6(11) . . ? C18' C16 C19' 102.6(19) . . ? C17 C16 C19' 136.7(11) . . ? C4 C16 C19' 104.4(8) . . ? O2 C20 C21 128.4(6) . 3 ? O2 C20 C21 128.4(6) . . ? C21 C20 C21 102.9(12) 3 . ? O2 C20 C25 114.3(6) . . ? C21 C20 C25 15.2(8) 3 . ? C21 C20 C25 117.3(9) . . ? O2 C20 C25 114.3(6) . 3 ? C21 C20 C25 117.3(9) 3 3 ? C21 C20 C25 15.2(8) . 3 ? C25 C20 C25 131.0(12) . 3 ? C25 C21 C24 109(3) 3 3 ? C25 C21 C20 96(3) 3 . ? C24 C21 C20 149.4(13) 3 . ? C25 C21 C22 135(4) 3 . ? C24 C21 C22 27.4(7) 3 . ? C20 C21 C22 122.9(11) . . ? C24 C22 C23 154(3) 3 3 ? C24 C22 C23 171(3) 3 . ? C23 C22 C23 21.1(8) 3 . ? C24 C22 C21 65.8(17) 3 . ? C23 C22 C21 139.7(18) 3 . ? C23 C22 C21 118.7(12) . . ? C24 C22 C25 57.5(16) 3 3 ? C23 C22 C25 147.2(17) 3 3 ? C23 C22 C25 126.3(11) . 3 ? C21 C22 C25 9.1(8) . 3 ? C24 C22 C22 159.9(17) 3 3 ? C23 C22 C22 44.2(13) 3 3 ? C23 C22 C22 23.2(7) . 3 ? C21 C22 C22 95.5(7) . 3 ? C25 C22 C22 103.3(6) 3 3 ? C23 C23 C22 135.8(13) 3 3 ? C23 C23 C24 147.0(7) 3 . ? C22 C23 C24 11.9(12) 3 . ? C23 C23 C22 23.2(7) 3 . ? C22 C23 C22 112.6(19) 3 . ? C24 C23 C22 123.9(10) . . ? C23 C23 O3 100.1(6) 3 . ? C22 C23 O3 124.0(15) 3 . ? C24 C23 O3 112.8(9) . . ? C22 C23 O3 123.2(9) . . ? C23 C23 O3 55.6(5) 3 3 ? C22 C23 O3 168.2(15) 3 3 ? C24 C23 O3 157.3(9) . 3 ? C22 C23 O3 78.8(8) . 3 ? O3 C23 O3 44.5(8) . 3 ? C23 C23 C24 21.9(5) 3 3 ? C22 C23 C24 114.0(14) 3 3 ? C24 C23 C24 125.1(11) . 3 ? C22 C23 C24 2.7(8) . 3 ? O3 C23 C24 122.0(8) . 3 ? O3 C23 C24 77.5(6) 3 3 ? C22 C24 C21 86.8(18) 3 3 ? C22 C24 C23 14.6(15) 3 . ? C21 C24 C23 101.0(11) 3 . ? C22 C24 C25 100.5(19) 3 . ? C21 C24 C25 14.3(9) 3 . ? C23 C24 C25 114.4(11) . . ? C22 C24 C23 5.9(17) 3 3 ? C21 C24 C23 90.0(10) 3 3 ? C23 C24 C23 11.1(3) . 3 ? C25 C24 C23 103.3(9) . 3 ? C21 C25 C20 69(3) 3 . ? C21 C25 C24 56(3) 3 . ? C20 C25 C24 122.7(11) . . ? C21 C25 C22 36(3) 3 3 ? C20 C25 C22 100.7(9) . 3 ? C24 C25 C22 22.0(6) . 3 ? C26 C26 O3 99.4(13) 3 3 ? C26 C26 O3 40.4(8) 3 . ? O3 C26 O3 59.0(15) 3 . ? O4 C27 C28 104.3(8) . . ? O4 C27 H27A 110.9 . . ? C28 C27 H27A 110.9 . . ? O4 C27 H27B 110.9 . . ? C28 C27 H27B 110.9 . . ? H27A C27 H27B 108.9 . . ? C27 C28 C28 106.1(5) . 3 ? C27 C28 H28A 110.5 . . ? C28 C28 H28A 110.5 3 . ? C27 C28 H28B 110.5 . . ? C28 C28 H28B 110.5 3 . ? H28A C28 H28B 108.7 . . ? O5 C29 C30 106.6(5) . . ? O5 C29 H29A 110.4 . . ? C30 C29 H29A 110.4 . . ? O5 C29 H29B 110.4 . . ? C30 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? C30 C30 C29 106.8(4) 3 . ? C30 C30 H30A 110.4 3 . ? C29 C30 H30A 110.4 . . ? C30 C30 H30B 110.4 3 . ? C29 C30 H30B 110.4 . . ? H30A C30 H30B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.065 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.099 #==================================================END OF CIF