Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name M.J.Hudson M.G.B.Drew M.R.S.Foreman C.Hill N.Huet C.Madic ; T.G.A.Youngs ; data_1_b _database_code_CSD 202727 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 La2 N16 O20' _chemical_formula_weight 1212.52 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.126(14) _cell_length_b 9.638(17) _cell_length_c 14.08(2) _cell_angle_alpha 92.127(10) _cell_angle_beta 101.892(10) _cell_angle_gamma 100.306(10) _cell_volume 1059(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour 'pale orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.902 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 2.090 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.573 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3527 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 26.03 _reflns_number_total 3527 _reflns_number_gt 3244 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+4.4529P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3527 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.58217(3) 0.95285(3) 0.659201(16) 0.02317(10) Uani 1 d . . . N63 N 0.5777(6) 1.2688(4) 0.5162(3) 0.0346(9) Uani 1 d . . . O64 O 0.6332(7) 1.3563(4) 0.5837(3) 0.0659(14) Uani 1 d . . . O62 O 0.5443(4) 1.1356(3) 0.5291(2) 0.0299(7) Uani 1 d . . . O61 O 0.5460(5) 1.2996(4) 0.4298(2) 0.0403(8) Uani 1 d . . . O51 O 0.7952(5) 1.1893(4) 0.7191(3) 0.0448(9) Uani 1 d . . . O52 O 0.9319(6) 1.0246(5) 0.7629(3) 0.0536(10) Uani 1 d . . . N53 N 0.9230(5) 1.1525(5) 0.7706(3) 0.0331(9) Uani 1 d . . . O54 O 1.0268(6) 1.2390(5) 0.8285(3) 0.0624(12) Uani 1 d . . . O41 O 0.3373(4) 0.8193(4) 0.7346(2) 0.0384(8) Uani 1 d . . . O42 O 0.2385(5) 0.9043(4) 0.6000(3) 0.0435(9) Uani 1 d . . . N43 N 0.2098(5) 0.8308(5) 0.6694(3) 0.0351(9) Uani 1 d . . . O44 O 0.0654(5) 0.7752(6) 0.6744(4) 0.0657(13) Uani 1 d . . . N31 N 0.4378(5) 1.1489(4) 0.7318(3) 0.0332(9) Uani 1 d . . . N36 N 0.3326(6) 1.2144(5) 0.6697(3) 0.0402(10) Uani 1 d . . . C35 C 0.2912(7) 1.3316(6) 0.7038(4) 0.0409(12) Uani 1 d . . . C34 C 0.3549(7) 1.3844(6) 0.8016(4) 0.0416(13) Uani 1 d . . . N33 N 0.4539(6) 1.3169(5) 0.8621(3) 0.0392(10) Uani 1 d . . . C32 C 0.4908(6) 1.1989(5) 0.8233(3) 0.0317(10) Uani 1 d . . . C26 C 0.6005(6) 1.1195(5) 0.8908(3) 0.0320(10) Uani 1 d . . . C25 C 0.6595(7) 1.1679(6) 0.9880(4) 0.0425(13) Uani 1 d . . . H25 H 0.6342 1.2511 1.0118 0.051 Uiso 1 calc R . . C24 C 0.7567(7) 1.0894(6) 1.0485(4) 0.0431(13) Uani 1 d . . . H24 H 0.8016 1.1209 1.1134 0.052 Uiso 1 calc R . . C23 C 0.7863(6) 0.9649(6) 1.0120(3) 0.0359(11) Uani 1 d . . . H23 H 0.8484 0.9093 1.0522 0.043 Uiso 1 calc R . . C22 C 0.7222(6) 0.9226(5) 0.9137(3) 0.0275(9) Uani 1 d . . . N21 N 0.6338(5) 0.9994(4) 0.8532(3) 0.0269(8) Uani 1 d . . . N11 N 0.7033(5) 0.7615(4) 0.7731(3) 0.0286(8) Uani 1 d . . . C12 C 0.7261(6) 0.6387(5) 0.7343(3) 0.0320(10) Uani 1 d . . . H12 H 0.6957 0.6218 0.6670 0.038 Uiso 1 calc R . . C16 C 0.7487(6) 0.7867(5) 0.8708(3) 0.0280(9) Uani 1 d . . . C13 C 0.7914(7) 0.5363(6) 0.7874(4) 0.0399(12) Uani 1 d . . . H13 H 0.8064 0.4535 0.7570 0.048 Uiso 1 calc R . . C14 C 0.8333(8) 0.5610(6) 0.8867(4) 0.0468(14) Uani 1 d . . . H14 H 0.8743 0.4930 0.9252 0.056 Uiso 1 calc R . . C15 C 0.8150(8) 0.6857(6) 0.9292(4) 0.0448(13) Uani 1 d . . . H15 H 0.8462 0.7036 0.9965 0.054 Uiso 1 calc R . . C350 C 0.1739(9) 1.3994(8) 0.6323(5) 0.0648(19) Uani 1 d . . . H35A H 0.1501 1.3483 0.5697 0.078 Uiso 1 calc R . . H35B H 0.2273 1.4955 0.6277 0.078 Uiso 1 calc R . . H35C H 0.0688 1.3982 0.6536 0.078 Uiso 1 calc R . . C300 C 0.3159(9) 1.5162(6) 0.8426(5) 0.0578(17) Uani 1 d . . . H30A H 0.3656 1.5297 0.9110 0.069 Uiso 1 calc R . . H30B H 0.1940 1.5085 0.8324 0.069 Uiso 1 calc R . . H30C H 0.3628 1.5953 0.8106 0.069 Uiso 1 calc R . . O100 O 0.8013(5) 0.8955(5) 0.5636(3) 0.0524(11) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.02425(15) 0.02300(16) 0.02225(13) 0.00153(9) 0.00484(9) 0.00473(11) N63 0.043(2) 0.028(2) 0.030(2) -0.0020(16) -0.0009(17) 0.009(2) O64 0.104(4) 0.037(2) 0.040(2) -0.0098(17) -0.013(2) 0.006(3) O62 0.0385(18) 0.0235(18) 0.0274(15) 0.0027(12) 0.0045(13) 0.0085(15) O61 0.055(2) 0.0289(19) 0.0318(18) 0.0065(14) -0.0006(15) 0.0041(18) O51 0.0342(19) 0.044(2) 0.048(2) 0.0085(16) -0.0067(16) 0.0021(18) O52 0.061(3) 0.047(3) 0.058(2) 0.0087(19) 0.016(2) 0.020(2) N53 0.027(2) 0.037(3) 0.031(2) 0.0060(17) 0.0062(16) -0.0029(19) O54 0.053(2) 0.056(3) 0.056(3) 0.005(2) -0.012(2) -0.020(2) O41 0.0316(18) 0.047(2) 0.0367(18) 0.0120(15) 0.0057(14) 0.0068(17) O42 0.038(2) 0.050(2) 0.042(2) 0.0120(17) 0.0031(16) 0.0109(18) N43 0.027(2) 0.031(2) 0.047(2) 0.0024(18) 0.0106(18) 0.0029(19) O44 0.0240(19) 0.080(4) 0.094(3) 0.021(3) 0.018(2) 0.005(2) N31 0.033(2) 0.032(2) 0.039(2) 0.0034(17) 0.0117(17) 0.0127(19) N36 0.041(2) 0.042(3) 0.045(2) 0.0089(19) 0.0140(19) 0.022(2) C35 0.039(3) 0.029(3) 0.065(3) 0.015(2) 0.028(3) 0.012(2) C34 0.036(3) 0.027(3) 0.069(4) 0.004(2) 0.028(3) 0.002(2) N33 0.037(2) 0.028(2) 0.056(3) -0.0023(19) 0.019(2) 0.005(2) C32 0.031(2) 0.025(3) 0.042(3) -0.0012(19) 0.015(2) 0.007(2) C26 0.033(2) 0.031(3) 0.033(2) -0.0020(19) 0.0143(19) 0.001(2) C25 0.047(3) 0.041(3) 0.040(3) -0.013(2) 0.018(2) 0.002(3) C24 0.046(3) 0.053(4) 0.026(2) -0.009(2) 0.007(2) 0.003(3) C23 0.037(3) 0.038(3) 0.030(2) -0.001(2) 0.005(2) 0.005(2) C22 0.025(2) 0.035(3) 0.022(2) 0.0040(17) 0.0068(16) 0.003(2) N21 0.0254(18) 0.027(2) 0.0271(18) -0.0015(15) 0.0078(14) 0.0013(17) N11 0.0257(19) 0.033(2) 0.0269(19) -0.0001(15) 0.0021(15) 0.0092(18) C12 0.032(2) 0.028(3) 0.036(2) -0.0002(18) 0.0075(19) 0.006(2) C16 0.022(2) 0.029(3) 0.032(2) 0.0056(18) 0.0041(17) 0.001(2) C13 0.039(3) 0.029(3) 0.050(3) -0.001(2) 0.002(2) 0.011(2) C14 0.051(3) 0.034(3) 0.051(3) 0.010(2) -0.005(3) 0.013(3) C15 0.059(4) 0.041(3) 0.032(3) 0.006(2) -0.002(2) 0.015(3) C350 0.072(5) 0.058(4) 0.080(5) 0.023(3) 0.025(4) 0.039(4) C300 0.059(4) 0.028(3) 0.092(5) -0.003(3) 0.025(3) 0.013(3) O100 0.039(2) 0.085(3) 0.043(2) 0.007(2) 0.0129(16) 0.031(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 La1 O100 2.564(5) . ? La1 O51 2.597(5) . ? La1 O62 2.599(4) . ? La1 O41 2.607(5) . ? La1 O61 2.627(5) 2_676 ? La1 N31 2.672(5) . ? La1 N11 2.676(5) . ? La1 O62 2.685(5) 2_676 ? La1 N21 2.685(6) . ? La1 O42 2.694(6) . ? La1 O52 2.863(6) . ? N63 O64 1.201(6) . ? N63 O61 1.250(5) . ? N63 O62 1.292(6) . ? O62 La1 2.685(5) 2_676 ? O61 La1 2.627(5) 2_676 ? O51 N53 1.253(5) . ? O52 N53 1.250(6) . ? N53 O54 1.219(6) . ? O41 N43 1.259(5) . ? O42 N43 1.264(6) . ? N43 O44 1.217(6) . ? N31 C32 1.316(6) . ? N31 N36 1.348(6) . ? N36 C35 1.334(7) . ? C35 C34 1.409(9) . ? C35 C350 1.492(8) . ? C34 N33 1.319(7) . ? C34 C300 1.487(7) . ? N33 C32 1.351(6) . ? C32 C26 1.494(7) . ? C26 N21 1.349(6) . ? C26 C25 1.387(7) . ? C25 C24 1.381(8) . ? C24 C23 1.367(8) . ? C23 C22 1.393(7) . ? C22 N21 1.332(6) . ? C22 C16 1.491(7) . ? N11 C12 1.344(6) . ? N11 C16 1.349(6) . ? C12 C13 1.376(7) . ? C16 C15 1.407(7) . ? C13 C14 1.371(8) . ? C14 C15 1.368(8) . ? 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 O100 La1 O51 86.25(17) . . ? O100 La1 O62 81.43(14) . . ? O51 La1 O62 69.88(15) . . ? O100 La1 O41 138.83(16) . . ? O51 La1 O41 130.01(14) . . ? O62 La1 O41 124.98(13) . . ? O100 La1 O61 73.86(16) . 2_676 ? O51 La1 O61 160.08(13) . 2_676 ? O62 La1 O61 107.30(16) . 2_676 ? O41 La1 O61 68.45(14) . 2_676 ? O100 La1 N31 148.06(15) . . ? O51 La1 N31 66.88(18) . . ? O62 La1 N31 73.48(15) . . ? O41 La1 N31 72.97(17) . . ? O61 La1 N31 132.25(16) 2_676 . ? O100 La1 N11 82.28(15) . . ? O51 La1 N11 104.97(16) . . ? O62 La1 N11 163.21(11) . . ? O41 La1 N11 70.93(15) . . ? O61 La1 N11 71.83(16) 2_676 . ? N31 La1 N11 120.07(15) . . ? O100 La1 O62 64.43(15) . 2_676 ? O51 La1 O62 123.99(11) . 2_676 ? O62 La1 O62 59.79(16) . 2_676 ? O41 La1 O62 99.62(14) . 2_676 ? O61 La1 O62 47.72(10) 2_676 2_676 ? N31 La1 O62 116.06(12) . 2_676 ? N11 La1 O62 115.89(14) . 2_676 ? O100 La1 N21 126.43(13) . . ? O51 La1 N21 69.44(12) . . ? O62 La1 N21 127.72(14) . . ? O41 La1 N21 65.65(13) . . ? O61 La1 N21 121.84(12) 2_676 . ? N31 La1 N21 61.14(12) . . ? N11 La1 N21 60.88(14) . . ? O62 La1 N21 165.27(12) 2_676 . ? O100 La1 O42 127.75(15) . . ? O51 La1 O42 129.52(13) . . ? O62 La1 O42 79.02(11) . . ? O41 La1 O42 47.88(13) . . ? O61 La1 O42 66.78(12) 2_676 . ? N31 La1 O42 66.68(15) . . ? N11 La1 O42 114.60(13) . . ? O62 La1 O42 63.80(11) 2_676 . ? N21 La1 O42 103.55(11) . . ? O100 La1 O52 65.10(17) . . ? O51 La1 O52 45.70(12) . . ? O62 La1 O52 106.17(13) . . ? O41 La1 O52 123.07(15) . . ? O61 La1 O52 121.17(12) 2_676 . ? N31 La1 O52 103.04(15) . . ? N11 La1 O52 62.78(14) . . ? O62 La1 O52 129.06(11) 2_676 . ? N21 La1 O52 63.83(12) . . ? O42 La1 O52 167.11(12) . . ? O64 N63 O61 122.9(5) . . ? O64 N63 O62 121.6(4) . . ? O61 N63 O62 115.5(4) . . ? N63 O62 La1 143.1(3) . . ? N63 O62 La1 96.4(2) . 2_676 ? La1 O62 La1 120.21(16) . 2_676 ? N63 O61 La1 100.4(3) . 2_676 ? N53 O51 La1 104.2(3) . . ? N53 O52 La1 91.2(3) . . ? O54 N53 O52 123.1(5) . . ? O54 N53 O51 119.8(5) . . ? O52 N53 O51 117.0(4) . . ? N43 O41 La1 99.6(3) . . ? N43 O42 La1 95.3(3) . . ? O44 N43 O41 121.1(5) . . ? O44 N43 O42 121.9(4) . . ? O41 N43 O42 117.1(4) . . ? C32 N31 N36 119.6(4) . . ? C32 N31 La1 120.6(3) . . ? N36 N31 La1 118.7(3) . . ? C35 N36 N31 117.9(5) . . ? N36 C35 C34 120.9(5) . . ? N36 C35 C350 115.7(5) . . ? C34 C35 C350 123.4(5) . . ? N33 C34 C35 120.5(5) . . ? N33 C34 C300 116.5(5) . . ? C35 C34 C300 123.0(5) . . ? C34 N33 C32 115.8(5) . . ? N31 C32 N33 125.3(5) . . ? N31 C32 C26 118.0(4) . . ? N33 C32 C26 116.7(4) . . ? N21 C26 C25 122.9(5) . . ? N21 C26 C32 117.0(4) . . ? C25 C26 C32 120.1(5) . . ? C24 C25 C26 118.3(5) . . ? C23 C24 C25 119.4(5) . . ? C24 C23 C22 119.1(5) . . ? N21 C22 C23 122.5(4) . . ? N21 C22 C16 116.4(4) . . ? C23 C22 C16 121.1(4) . . ? C22 N21 C26 117.8(4) . . ? C22 N21 La1 121.7(3) . . ? C26 N21 La1 119.2(3) . . ? C12 N11 C16 117.8(4) . . ? C12 N11 La1 120.8(3) . . ? C16 N11 La1 121.4(3) . . ? N11 C12 C13 124.5(5) . . ? N11 C16 C15 120.5(4) . . ? N11 C16 C22 117.7(4) . . ? C15 C16 C22 121.8(4) . . ? C14 C13 C12 117.4(5) . . ? C15 C14 C13 120.0(5) . . ? C14 C15 C16 119.8(5) . . ? _refine_diff_density_max 0.816 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.104 #===END data_2 _database_code_CSD 202728 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Ce2 N16 O20 ' _chemical_formula_weight 1214.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.135(14) _cell_length_b 9.611(17) _cell_length_c 14.05(2) _cell_angle_alpha 92.297(10) _cell_angle_beta 101.364(10) _cell_angle_gamma 100.431(10) _cell_volume 1056(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 598 _exptl_absorpt_coefficient_mu 2.229 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.316 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3492 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0985 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3492 _reflns_number_gt 2226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1438P)^2^+3.8884P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3492 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1606 _refine_ls_R_factor_gt 0.0942 _refine_ls_wR_factor_ref 0.2524 _refine_ls_wR_factor_gt 0.2189 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.57810(11) 0.95153(9) 0.65891(7) 0.0519(4) Uani 1 d . . . N63 N 0.5845(17) 1.2684(14) 0.5174(10) 0.056(3) Uani 1 d . . . O64 O 0.6331(19) 1.3539(13) 0.5817(10) 0.083(4) Uani 1 d . . . O62 O 0.5458(13) 1.1346(10) 0.5290(7) 0.051(2) Uani 1 d . . . O61 O 0.5516(15) 1.2983(12) 0.4268(8) 0.067(3) Uani 1 d . . . O51 O 0.7913(16) 1.1811(13) 0.7168(9) 0.074(3) Uani 1 d . . . O52 O 0.939(2) 1.0212(14) 0.7637(10) 0.087(4) Uani 1 d . . . N53 N 0.9220(17) 1.1495(17) 0.7723(10) 0.063(4) Uani 1 d . . . O54 O 1.0221(18) 1.2391(16) 0.8273(11) 0.096(5) Uani 1 d . . . O41 O 0.3382(15) 0.8207(13) 0.7352(9) 0.069(3) Uani 1 d . . . O42 O 0.2375(14) 0.9048(12) 0.5982(8) 0.060(3) Uani 1 d . . . N43 N 0.2100(17) 0.8326(15) 0.6687(12) 0.064(4) Uani 1 d . . . O44 O 0.0635(14) 0.7723(15) 0.6741(11) 0.086(4) Uani 1 d . . . N31 N 0.4353(15) 1.1493(13) 0.7298(10) 0.054(3) Uani 1 d . . . N36 N 0.334(2) 1.2147(15) 0.6668(10) 0.067(4) Uani 1 d . . . C35 C 0.289(2) 1.3292(16) 0.7012(12) 0.055(4) Uani 1 d . . . C34 C 0.352(2) 1.3849(18) 0.8018(14) 0.067(5) Uani 1 d . . . N33 N 0.4471(18) 1.3143(13) 0.8577(10) 0.060(3) Uani 1 d . . . C32 C 0.4878(19) 1.1976(15) 0.8225(11) 0.050(4) Uani 1 d . . . C26 C 0.599(2) 1.1206(17) 0.8906(12) 0.058(4) Uani 1 d . . . C25 C 0.658(2) 1.1678(18) 0.9866(13) 0.064(4) Uani 1 d . . . H25 H 0.6319 1.2510 1.0107 0.077 Uiso 1 calc R . . C24 C 0.754(2) 1.0916(18) 1.0467(12) 0.065(5) Uani 1 d . . . H24 H 0.7983 1.1243 1.1115 0.078 Uiso 1 calc R . . C23 C 0.786(2) 0.965(2) 1.0104(12) 0.066(5) Uani 1 d . . . H23 H 0.8483 0.9096 1.0504 0.080 Uiso 1 calc R . . C22 C 0.720(2) 0.9235(17) 0.9102(12) 0.057(4) Uani 1 d . . . N21 N 0.6324(15) 1.0001(11) 0.8517(9) 0.047(3) Uani 1 d . . . N11 N 0.7022(15) 0.7597(11) 0.7734(9) 0.046(3) Uani 1 d . . . C12 C 0.722(2) 0.6367(16) 0.7319(12) 0.057(4) Uani 1 d . . . H12 H 0.6899 0.6204 0.6645 0.069 Uiso 1 calc R . . C13 C 0.749(2) 0.7851(16) 0.8723(10) 0.051(4) Uani 1 d . . . C14 C 0.786(2) 0.5354(17) 0.7838(13) 0.065(4) Uani 1 d . . . H14 H 0.7996 0.4519 0.7531 0.078 Uiso 1 calc R . . C15 C 0.832(2) 0.5615(18) 0.8857(14) 0.074(5) Uani 1 d . . . H15 H 0.8736 0.4938 0.9241 0.089 Uiso 1 calc R . . C16 C 0.814(2) 0.6864(17) 0.9279(13) 0.066(5) Uani 1 d . . . H16 H 0.8472 0.7049 0.9951 0.080 Uiso 1 calc R . . C350 C 0.170(3) 1.398(2) 0.6277(17) 0.098(7) Uani 1 d . . . H35A H 0.1253 1.3337 0.5703 0.118 Uiso 1 calc R . . H35B H 0.2328 1.4842 0.6105 0.118 Uiso 1 calc R . . H35C H 0.0779 1.4177 0.6558 0.118 Uiso 1 calc R . . C300 C 0.315(3) 1.5146(19) 0.8395(17) 0.093(6) Uani 1 d . . . H30A H 0.3612 1.5286 0.9084 0.111 Uiso 1 calc R . . H30B H 0.1940 1.5091 0.8275 0.111 Uiso 1 calc R . . H30C H 0.3667 1.5926 0.8078 0.111 Uiso 1 calc R . . O100 O 0.7966(14) 0.8942(13) 0.5657(9) 0.072(3) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.0528(5) 0.0504(6) 0.0517(6) 0.0017(4) 0.0103(4) 0.0091(4) N63 0.070(8) 0.047(8) 0.045(8) -0.019(6) 0.008(6) 0.003(6) O64 0.115(11) 0.049(7) 0.071(8) -0.009(6) -0.007(7) 0.008(7) O62 0.056(6) 0.045(6) 0.048(6) 0.000(4) 0.004(5) 0.009(4) O61 0.074(7) 0.061(7) 0.055(7) 0.010(5) -0.003(6) 0.003(6) O51 0.077(8) 0.074(8) 0.061(8) 0.015(6) 0.002(6) -0.002(6) O52 0.129(12) 0.067(8) 0.084(9) 0.015(7) 0.048(8) 0.042(8) N53 0.051(8) 0.082(11) 0.057(9) 0.018(8) 0.010(7) 0.017(8) O54 0.075(8) 0.089(10) 0.091(10) 0.021(8) -0.033(8) -0.016(8) O41 0.058(7) 0.074(8) 0.071(8) 0.007(6) 0.015(6) -0.002(6) O42 0.060(6) 0.067(7) 0.057(7) 0.015(6) 0.016(5) 0.021(5) N43 0.049(8) 0.061(9) 0.082(11) -0.009(8) 0.016(8) 0.008(7) O44 0.044(6) 0.089(9) 0.130(12) 0.028(8) 0.027(7) 0.013(6) N31 0.041(7) 0.061(8) 0.069(9) 0.005(7) 0.021(6) 0.021(6) N36 0.085(10) 0.068(9) 0.047(8) 0.012(7) 0.010(7) 0.016(8) C35 0.060(9) 0.054(9) 0.063(10) 0.017(8) 0.027(8) 0.026(7) C34 0.068(10) 0.053(10) 0.081(13) 0.011(9) 0.029(9) -0.002(8) N33 0.079(9) 0.038(7) 0.069(9) -0.003(6) 0.029(7) 0.014(6) C32 0.048(8) 0.046(8) 0.062(10) -0.002(7) 0.022(7) 0.017(6) C26 0.060(9) 0.061(10) 0.063(11) 0.009(8) 0.037(8) 0.013(8) C25 0.066(10) 0.053(10) 0.069(12) -0.014(8) 0.012(9) 0.007(8) C24 0.082(12) 0.058(10) 0.048(10) -0.020(8) 0.016(9) -0.002(9) C23 0.057(9) 0.098(14) 0.050(10) 0.030(9) 0.012(8) 0.024(9) C22 0.054(9) 0.056(9) 0.061(11) 0.016(8) 0.017(8) 0.000(7) N21 0.058(7) 0.036(6) 0.049(7) 0.005(5) 0.014(6) 0.011(5) N11 0.050(7) 0.034(6) 0.054(8) -0.002(5) 0.008(6) 0.009(5) C12 0.071(10) 0.051(9) 0.048(9) -0.007(7) 0.009(8) 0.013(8) C13 0.067(10) 0.057(9) 0.034(8) 0.000(7) 0.013(7) 0.019(7) C14 0.078(11) 0.048(9) 0.065(11) -0.003(8) 0.006(9) 0.014(8) C15 0.087(13) 0.050(10) 0.082(14) 0.013(9) -0.002(10) 0.024(9) C16 0.076(11) 0.052(10) 0.057(10) 0.004(8) -0.008(9) 0.001(8) C350 0.108(17) 0.091(15) 0.106(17) 0.011(12) 0.013(14) 0.059(13) C300 0.124(18) 0.048(11) 0.110(17) -0.004(10) 0.037(14) 0.017(11) O100 0.059(7) 0.084(8) 0.076(8) 0.007(6) 0.011(6) 0.027(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O100 2.528(12) . ? Ce1 O51 2.540(12) . ? Ce1 O41 2.566(11) . ? Ce1 O61 2.585(12) 2_676 ? Ce1 O62 2.595(10) . ? Ce1 N31 2.657(12) . ? Ce1 N21 2.664(12) . ? Ce1 O62 2.672(10) 2_676 ? Ce1 O42 2.682(12) . ? Ce1 N11 2.697(11) . ? Ce1 O52 2.959(17) . ? N63 O64 1.153(16) . ? N63 O62 1.292(16) . ? N63 O61 1.302(16) . ? O62 Ce1 2.672(10) 2_676 ? O61 Ce1 2.585(12) 2_676 ? O51 N53 1.280(17) . ? O52 N53 1.270(18) . ? N53 O54 1.203(19) . ? O41 N43 1.281(18) . ? O42 N43 1.265(17) . ? N43 O44 1.245(17) . ? N31 C32 1.325(19) . ? N31 N36 1.342(18) . ? N36 C35 1.32(2) . ? C35 C34 1.45(2) . ? C35 C350 1.52(2) . ? C34 N33 1.29(2) . ? C34 C300 1.44(3) . ? N33 C32 1.329(18) . ? C32 C26 1.50(2) . ? C26 N21 1.355(19) . ? C26 C25 1.37(2) . ? C25 C24 1.36(2) . ? C24 C23 1.39(2) . ? C23 C22 1.42(2) . ? C22 N21 1.317(19) . ? C22 C13 1.49(2) . ? N11 C12 1.346(18) . ? N11 C13 1.366(18) . ? C12 C14 1.36(2) . ? C13 C16 1.37(2) . ? C14 C15 1.41(2) . ? C15 C16 1.36(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O100 Ce1 O51 85.0(4) . . ? O100 Ce1 O41 138.9(4) . . ? O51 Ce1 O41 130.4(4) . . ? O100 Ce1 O61 75.0(4) . 2_676 ? O51 Ce1 O61 159.9(4) . 2_676 ? O41 Ce1 O61 67.8(4) . 2_676 ? O100 Ce1 O62 81.4(4) . . ? O51 Ce1 O62 69.9(4) . . ? O41 Ce1 O62 126.0(4) . . ? O61 Ce1 O62 107.9(3) 2_676 . ? O100 Ce1 N31 147.6(4) . . ? O51 Ce1 N31 67.8(4) . . ? O41 Ce1 N31 73.4(4) . . ? O61 Ce1 N31 131.6(4) 2_676 . ? O62 Ce1 N31 73.2(4) . . ? O100 Ce1 N21 125.1(4) . . ? O51 Ce1 N21 69.0(4) . . ? O41 Ce1 N21 66.0(4) . . ? O61 Ce1 N21 121.7(3) 2_676 . ? O62 Ce1 N21 127.5(3) . . ? N31 Ce1 N21 62.0(4) . . ? O100 Ce1 O62 65.1(4) . 2_676 ? O51 Ce1 O62 123.4(3) . 2_676 ? O41 Ce1 O62 100.4(4) . 2_676 ? O61 Ce1 O62 48.8(3) 2_676 2_676 ? O62 Ce1 O62 59.4(4) . 2_676 ? N31 Ce1 O62 115.3(4) . 2_676 ? N21 Ce1 O62 166.4(3) . 2_676 ? O100 Ce1 O42 127.7(4) . . ? O51 Ce1 O42 130.4(4) . . ? O41 Ce1 O42 49.1(4) . . ? O61 Ce1 O42 66.2(4) 2_676 . ? O62 Ce1 O42 78.9(3) . . ? N31 Ce1 O42 66.8(4) . . ? N21 Ce1 O42 105.1(4) . . ? O62 Ce1 O42 63.2(3) 2_676 . ? O100 Ce1 N11 81.3(4) . . ? O51 Ce1 N11 103.7(4) . . ? O41 Ce1 N11 71.3(4) . . ? O61 Ce1 N11 72.0(4) 2_676 . ? O62 Ce1 N11 162.0(3) . . ? N31 Ce1 N11 121.0(4) . . ? N21 Ce1 N11 60.9(3) . . ? O62 Ce1 N11 116.5(3) 2_676 . ? O42 Ce1 N11 116.0(3) . . ? O100 Ce1 O52 63.7(4) . . ? O51 Ce1 O52 45.6(4) . . ? O41 Ce1 O52 122.7(4) . . ? O61 Ce1 O52 120.6(4) 2_676 . ? O62 Ce1 O52 105.9(3) . . ? N31 Ce1 O52 104.2(4) . . ? N21 Ce1 O52 63.7(4) . . ? O62 Ce1 O52 128.3(3) 2_676 . ? O42 Ce1 O52 168.5(3) . . ? N11 Ce1 O52 61.6(4) . . ? O64 N63 O62 123.0(14) . . ? O64 N63 O61 123.2(14) . . ? O62 N63 O61 113.7(11) . . ? N63 O62 Ce1 142.2(9) . . ? N63 O62 Ce1 96.8(8) . 2_676 ? Ce1 O62 Ce1 120.6(4) . 2_676 ? N63 O61 Ce1 100.7(8) . 2_676 ? N53 O51 Ce1 107.6(10) . . ? N53 O52 Ce1 87.6(10) . . ? O54 N53 O52 123.4(15) . . ? O54 N53 O51 120.5(15) . . ? O52 N53 O51 116.1(15) . . ? N43 O41 Ce1 98.8(9) . . ? N43 O42 Ce1 93.7(8) . . ? O44 N43 O42 121.9(15) . . ? O44 N43 O41 119.9(15) . . ? O42 N43 O41 118.2(13) . . ? C32 N31 N36 121.2(12) . . ? C32 N31 Ce1 119.5(9) . . ? N36 N31 Ce1 118.3(10) . . ? C35 N36 N31 117.3(13) . . ? N36 C35 C34 121.4(14) . . ? N36 C35 C350 115.4(15) . . ? C34 C35 C350 123.2(15) . . ? N33 C34 C300 120.1(18) . . ? N33 C34 C35 117.1(16) . . ? C300 C34 C35 122.8(18) . . ? C34 N33 C32 120.6(15) . . ? N31 C32 N33 122.3(14) . . ? N31 C32 C26 119.5(12) . . ? N33 C32 C26 118.2(14) . . ? N21 C26 C25 122.8(15) . . ? N21 C26 C32 115.8(14) . . ? C25 C26 C32 121.4(14) . . ? C24 C25 C26 119.4(15) . . ? C25 C24 C23 119.6(15) . . ? C24 C23 C22 117.5(15) . . ? N21 C22 C23 122.7(16) . . ? N21 C22 C13 119.9(14) . . ? C23 C22 C13 117.4(14) . . ? C22 N21 C26 118.1(14) . . ? C22 N21 Ce1 121.0(10) . . ? C26 N21 Ce1 119.8(9) . . ? C12 N11 C13 119.1(12) . . ? C12 N11 Ce1 119.2(10) . . ? C13 N11 Ce1 121.7(9) . . ? N11 C12 C14 123.1(15) . . ? N11 C13 C16 120.0(14) . . ? N11 C13 C22 114.5(12) . . ? C16 C13 C22 125.5(14) . . ? C12 C14 C15 117.5(15) . . ? C16 C15 C14 119.5(15) . . ? C15 C16 C13 120.7(16) . . ? _refine_diff_density_max 1.705 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.180 #===END data_3 _database_code_CSD 202729 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H19 N9 O10.50 Pr' _chemical_formula_weight 658.32 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.248(16) _cell_length_b 12.976(18) _cell_length_c 12.967(15) _cell_angle_alpha 60.461(10) _cell_angle_beta 85.997(10) _cell_angle_gamma 89.330(10) _cell_volume 1350(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cuboid _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 654 _exptl_absorpt_coefficient_mu 1.870 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.432 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8514 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.1201 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.82 _reflns_number_total 4745 _reflns_number_gt 3939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1645P)^2^+4.4429P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.023(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4745 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.1015 _refine_ls_wR_factor_ref 0.2727 _refine_ls_wR_factor_gt 0.2605 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.72472(7) 0.72368(5) 0.93051(6) 0.0502(4) Uani 1 d . . . N11 N 0.5583(14) 0.9010(10) 0.8219(12) 0.066(3) Uani 1 d . . . C12 C 0.4686(18) 0.9010(15) 0.7445(16) 0.076(4) Uani 1 d . . . H12 H 0.4527 0.8309 0.7435 0.091 Uiso 1 calc R . . C13 C 0.398(2) 1.0029(17) 0.6656(17) 0.083(4) Uani 1 d . . . H13 H 0.3379 1.0016 0.6118 0.100 Uiso 1 calc R . . C14 C 0.421(2) 1.1025(18) 0.6700(19) 0.090(5) Uani 1 d . . . H14 H 0.3760 1.1714 0.6179 0.108 Uiso 1 calc R . . C15 C 0.508(2) 1.1047(14) 0.7492(14) 0.072(4) Uani 1 d . . . H15 H 0.5217 1.1740 0.7525 0.087 Uiso 1 calc R . . C16 C 0.5772(17) 1.0020(13) 0.8248(14) 0.067(3) Uani 1 d . . . C22 C 0.6761(15) 0.9957(12) 0.9151(13) 0.059(3) Uani 1 d . . . N21 N 0.7383(13) 0.8932(10) 0.9803(11) 0.060(3) Uani 1 d . . . C23 C 0.6878(18) 1.0907(13) 0.9385(15) 0.070(4) Uani 1 d . . . H23 H 0.6381 1.1601 0.8953 0.083 Uiso 1 calc R . . C24 C 0.7732(17) 1.0794(13) 1.0255(16) 0.070(4) Uani 1 d . . . H24 H 0.7839 1.1410 1.0419 0.084 Uiso 1 calc R . . C25 C 0.8437(18) 0.9727(14) 1.0888(16) 0.072(4) Uani 1 d . . . H25 H 0.9043 0.9632 1.1470 0.087 Uiso 1 calc R . . C26 C 0.8236(15) 0.8808(12) 1.0649(12) 0.058(3) Uani 1 d . . . C32 C 0.8966(16) 0.7655(12) 1.1345(13) 0.062(3) Uani 1 d . . . N31 N 0.8621(14) 0.6808(10) 1.1094(12) 0.066(3) Uani 1 d . . . N33 N 0.9847(13) 0.7598(10) 1.2120(10) 0.061(3) Uani 1 d . . . C34 C 1.0477(19) 0.6515(14) 1.2740(15) 0.074(4) Uani 1 d . . . C35 C 1.0068(17) 0.5604(14) 1.2528(13) 0.067(3) Uani 1 d . . . N36 N 0.9211(16) 0.5750(11) 1.1747(12) 0.072(3) Uani 1 d . . . C300 C 1.160(3) 0.641(2) 1.356(2) 0.116(9) Uani 1 d . . . H30A H 1.2540 0.6366 1.3232 0.139 Uiso 1 calc R . . H30B H 1.1397 0.5712 1.4319 0.139 Uiso 1 calc R . . H30C H 1.1570 0.7096 1.3668 0.139 Uiso 1 calc R . . C350 C 1.072(2) 0.4401(16) 1.3221(18) 0.085(5) Uani 1 d . . . H35A H 1.0823 0.4231 1.4021 0.102 Uiso 1 calc R . . H35B H 1.1657 0.4398 1.2851 0.102 Uiso 1 calc R . . H35C H 1.0099 0.3809 1.3230 0.102 Uiso 1 calc R . . N43 N 1.0375(15) 0.7459(13) 0.8643(13) 0.076(3) Uani 1 d . . . O42 O 0.9732(12) 0.8297(10) 0.8676(11) 0.074(3) Uani 1 d . . . O44 O 1.1677(15) 0.7556(17) 0.8341(16) 0.112(5) Uani 1 d . . . O41 O 0.9649(12) 0.6525(9) 0.8934(11) 0.075(3) Uani 1 d . . . N53 N 0.4347(15) 0.6534(11) 1.0629(12) 0.070(3) Uani 1 d . . . O52 O 0.4694(11) 0.6399(9) 0.9729(10) 0.070(2) Uani 1 d . . . O51 O 0.5362(11) 0.6932(9) 1.0929(10) 0.068(2) Uani 1 d . . . O54 O 0.3152(13) 0.6284(12) 1.1136(13) 0.090(4) Uani 1 d . . . N63 N 0.7149(17) 0.7516(14) 0.6924(13) 0.080(4) Uani 1 d . . . O61 O 0.7892(14) 0.8276(12) 0.7080(11) 0.085(3) Uani 1 d . . . O62 O 0.6498(13) 0.6696(10) 0.7819(11) 0.074(3) Uani 1 d . . . O64 O 0.7014(18) 0.7671(13) 0.5907(12) 0.100(4) Uani 1 d . . . O100 O 0.7270(13) 0.5123(9) 1.0496(10) 0.074(3) Uani 1 d . . . N100 N 0.671(3) 0.602(3) 1.387(2) 0.080(7) Uani 0.50 d P . . C101 C 0.637(3) 0.530(3) 1.376(2) 0.062(6) Uani 0.50 d P . . C102 C 0.573(4) 0.437(3) 1.355(3) 0.076(8) Uani 0.50 d P . . H10A H 0.5968 0.4562 1.2744 0.091 Uiso 0.50 calc PR . . H10B H 0.4699 0.4335 1.3704 0.091 Uiso 0.50 calc PR . . H10C H 0.6122 0.3613 1.4077 0.091 Uiso 0.50 calc PR . . O300 O 0.563(5) 0.467(4) 1.506(4) 0.147(14) Uiso 0.50 d P . . C202 C 1.120(3) 1.019(3) 0.653(3) 0.070(7) Uiso 0.50 d P . . H20A H 1.0926 0.9394 0.7120 0.084 Uiso 0.50 calc PR . . H20B H 1.1536 1.0613 0.6903 0.084 Uiso 0.50 calc PR . . H20C H 1.1959 1.0181 0.5989 0.084 Uiso 0.50 calc PR . . C201 C 0.996(4) 1.077(3) 0.588(3) 0.074(7) Uiso 0.50 d P . . N200 N 0.873(3) 1.123(3) 0.536(3) 0.082(7) Uiso 0.50 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0517(5) 0.0535(4) 0.0516(5) -0.0305(3) -0.0039(3) 0.0012(2) N11 0.065(7) 0.065(6) 0.067(8) -0.032(6) -0.009(5) 0.010(5) C12 0.063(10) 0.083(9) 0.084(11) -0.041(9) -0.016(8) 0.003(7) C13 0.080(12) 0.093(11) 0.077(11) -0.041(9) -0.013(8) 0.000(8) C14 0.085(13) 0.101(12) 0.087(13) -0.048(11) -0.019(9) 0.018(9) C15 0.087(11) 0.067(8) 0.056(9) -0.024(7) -0.013(7) 0.011(7) C16 0.068(9) 0.066(7) 0.066(9) -0.032(7) -0.001(7) 0.004(6) C22 0.053(8) 0.064(7) 0.062(8) -0.033(6) -0.004(6) 0.005(5) N21 0.059(7) 0.068(6) 0.057(7) -0.033(5) 0.004(5) -0.005(5) C23 0.079(10) 0.063(7) 0.070(10) -0.036(7) -0.007(7) 0.006(6) C24 0.059(9) 0.072(8) 0.088(11) -0.047(8) -0.008(7) 0.003(6) C25 0.072(10) 0.076(8) 0.082(11) -0.047(8) -0.014(7) -0.002(6) C26 0.060(8) 0.070(7) 0.048(7) -0.034(6) 0.006(5) 0.003(5) C32 0.075(9) 0.063(7) 0.062(8) -0.044(7) 0.007(6) -0.006(6) N31 0.066(8) 0.068(6) 0.066(8) -0.033(6) -0.012(5) 0.004(5) N33 0.065(7) 0.067(6) 0.043(6) -0.020(5) -0.011(5) 0.006(5) C34 0.082(11) 0.074(8) 0.062(9) -0.030(7) -0.011(7) 0.011(7) C35 0.070(9) 0.083(9) 0.049(8) -0.033(7) -0.011(6) 0.011(6) N36 0.083(9) 0.064(6) 0.071(8) -0.037(6) -0.003(6) 0.010(5) C300 0.15(2) 0.121(15) 0.115(17) -0.079(14) -0.083(15) 0.074(14) C350 0.083(12) 0.086(10) 0.085(12) -0.042(9) -0.008(9) 0.014(8) N43 0.066(9) 0.088(9) 0.077(9) -0.042(7) -0.005(6) 0.010(6) O42 0.072(7) 0.078(6) 0.086(8) -0.052(6) 0.005(5) 0.003(5) O44 0.058(9) 0.162(14) 0.136(13) -0.092(12) 0.014(7) 0.006(7) O41 0.076(7) 0.072(6) 0.079(7) -0.039(5) 0.006(5) 0.000(5) N53 0.076(9) 0.064(6) 0.074(8) -0.038(6) 0.006(6) 0.001(5) O52 0.064(6) 0.078(6) 0.072(7) -0.042(5) 0.002(5) -0.006(4) O51 0.062(6) 0.078(6) 0.074(7) -0.045(5) 0.001(5) -0.008(4) O54 0.064(8) 0.098(8) 0.108(10) -0.053(7) 0.021(6) -0.010(5) N63 0.085(10) 0.103(10) 0.068(9) -0.054(8) -0.017(7) 0.033(8) O61 0.083(8) 0.103(8) 0.071(7) -0.045(7) -0.008(6) 0.011(6) O62 0.088(8) 0.082(6) 0.066(7) -0.048(6) 0.002(5) -0.003(5) O64 0.126(12) 0.117(10) 0.059(7) -0.042(7) -0.030(7) 0.036(8) O100 0.088(7) 0.063(5) 0.070(7) -0.032(5) -0.014(5) 0.004(4) N100 0.09(2) 0.090(18) 0.047(15) -0.023(14) 0.014(12) -0.016(14) C101 0.064(16) 0.072(16) 0.032(13) -0.013(12) 0.009(10) 0.008(12) C102 0.08(2) 0.072(16) 0.07(2) -0.033(15) 0.002(15) -0.011(13) _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 Pr1 O100 2.394(10) . ? Pr1 O62 2.493(11) . ? Pr1 O41 2.501(12) . ? Pr1 O51 2.512(11) . ? Pr1 O52 2.520(11) . ? Pr1 N31 2.535(13) . ? Pr1 O61 2.538(13) . ? Pr1 O42 2.558(12) . ? Pr1 N11 2.582(12) . ? Pr1 N21 2.586(11) . ? N11 C16 1.344(19) . ? N11 C12 1.35(2) . ? C12 C13 1.40(3) . ? C13 C14 1.34(3) . ? C14 C15 1.36(3) . ? C15 C16 1.39(2) . ? C16 C22 1.51(2) . ? C22 N21 1.325(18) . ? C22 C23 1.415(19) . ? N21 C26 1.341(19) . ? C23 C24 1.37(2) . ? C24 C25 1.40(2) . ? C25 C26 1.39(2) . ? C26 C32 1.50(2) . ? C32 N33 1.311(19) . ? C32 N31 1.338(17) . ? N31 N36 1.341(18) . ? N33 C34 1.38(2) . ? C34 C35 1.40(2) . ? C34 C300 1.50(2) . ? C35 N36 1.27(2) . ? C35 C350 1.51(2) . ? N43 O44 1.228(19) . ? N43 O42 1.250(18) . ? N43 O41 1.263(18) . ? N53 O54 1.206(17) . ? N53 O51 1.250(16) . ? N53 O52 1.281(17) . ? N63 O62 1.242(19) . ? N63 O64 1.248(18) . ? N63 O61 1.31(2) . ? N100 C101 1.06(4) . ? C101 C102 1.49(5) . ? C202 C201 1.44(5) . ? C201 N200 1.34(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O100 Pr1 O62 80.8(4) . . ? O100 Pr1 O41 71.0(4) . . ? O62 Pr1 O41 82.7(4) . . ? O100 Pr1 O51 80.2(4) . . ? O62 Pr1 O51 116.3(4) . . ? O41 Pr1 O51 142.6(4) . . ? O100 Pr1 O52 70.3(4) . . ? O62 Pr1 O52 66.5(4) . . ? O41 Pr1 O52 133.5(4) . . ? O51 Pr1 O52 49.8(3) . . ? O100 Pr1 N31 74.0(4) . . ? O62 Pr1 N31 150.9(4) . . ? O41 Pr1 N31 75.5(4) . . ? O51 Pr1 N31 73.9(4) . . ? O52 Pr1 N31 116.5(4) . . ? O100 Pr1 O61 121.5(4) . . ? O62 Pr1 O61 51.3(4) . . ? O41 Pr1 O61 71.4(4) . . ? O51 Pr1 O61 145.9(4) . . ? O52 Pr1 O61 109.1(4) . . ? N31 Pr1 O61 134.3(4) . . ? O100 Pr1 O42 115.7(4) . . ? O62 Pr1 O42 111.2(4) . . ? O41 Pr1 O42 50.4(3) . . ? O51 Pr1 O42 131.8(3) . . ? O52 Pr1 O42 173.5(4) . . ? N31 Pr1 O42 68.6(4) . . ? O61 Pr1 O42 66.1(4) . . ? O100 Pr1 N11 143.6(4) . . ? O62 Pr1 N11 83.4(4) . . ? O41 Pr1 N11 138.8(4) . . ? O51 Pr1 N11 77.8(4) . . ? O52 Pr1 N11 73.3(4) . . ? N31 Pr1 N11 125.6(4) . . ? O61 Pr1 N11 69.6(4) . . ? O42 Pr1 N11 100.5(4) . . ? O100 Pr1 N21 133.0(4) . . ? O62 Pr1 N21 144.6(4) . . ? O41 Pr1 N21 114.9(4) . . ? O51 Pr1 N21 69.1(3) . . ? O52 Pr1 N21 110.1(4) . . ? N31 Pr1 N21 63.9(4) . . ? O61 Pr1 N21 103.2(4) . . ? O42 Pr1 N21 67.8(3) . . ? N11 Pr1 N21 62.9(4) . . ? C16 N11 C12 118.3(13) . . ? C16 N11 Pr1 121.0(10) . . ? C12 N11 Pr1 119.6(10) . . ? N11 C12 C13 122.2(16) . . ? C14 C13 C12 117.8(17) . . ? C13 C14 C15 121.4(18) . . ? C14 C15 C16 118.8(16) . . ? N11 C16 C15 121.4(15) . . ? N11 C16 C22 115.8(12) . . ? C15 C16 C22 122.7(13) . . ? N21 C22 C23 121.5(13) . . ? N21 C22 C16 117.1(12) . . ? C23 C22 C16 120.9(12) . . ? C22 N21 C26 119.9(12) . . ? C22 N21 Pr1 121.1(9) . . ? C26 N21 Pr1 118.6(9) . . ? C24 C23 C22 119.3(14) . . ? C23 C24 C25 118.0(13) . . ? C26 C25 C24 120.1(15) . . ? N21 C26 C25 120.9(13) . . ? N21 C26 C32 118.9(11) . . ? C25 C26 C32 120.2(13) . . ? N33 C32 N31 128.4(14) . . ? N33 C32 C26 116.5(11) . . ? N31 C32 C26 115.1(13) . . ? C32 N31 N36 116.0(13) . . ? C32 N31 Pr1 122.3(10) . . ? N36 N31 Pr1 121.1(9) . . ? C32 N33 C34 113.9(12) . . ? N33 C34 C35 118.2(14) . . ? N33 C34 C300 117.1(15) . . ? C35 C34 C300 124.7(15) . . ? N36 C35 C34 123.1(14) . . ? N36 C35 C350 118.0(15) . . ? C34 C35 C350 118.9(15) . . ? C35 N36 N31 120.2(13) . . ? O44 N43 O42 120.1(15) . . ? O44 N43 O41 121.9(15) . . ? O42 N43 O41 118.0(14) . . ? O44 N43 Pr1 178.6(13) . . ? O42 N43 Pr1 60.3(8) . . ? O41 N43 Pr1 57.8(8) . . ? N43 O42 Pr1 94.6(9) . . ? N43 O41 Pr1 97.0(9) . . ? O54 N53 O51 123.9(14) . . ? O54 N53 O52 122.5(14) . . ? O51 N53 O52 113.6(12) . . ? O54 N53 Pr1 177.8(11) . . ? O51 N53 Pr1 56.6(7) . . ? O52 N53 Pr1 57.1(7) . . ? N53 O52 Pr1 97.6(8) . . ? N53 O51 Pr1 98.9(8) . . ? O62 N63 O64 121.8(17) . . ? O62 N63 O61 117.0(13) . . ? O64 N63 O61 120.9(17) . . ? O62 N63 Pr1 57.4(7) . . ? O64 N63 Pr1 175.6(11) . . ? O61 N63 Pr1 59.7(8) . . ? N63 O61 Pr1 93.9(9) . . ? N63 O62 Pr1 97.9(9) . . ? N100 C101 C102 173(4) . . ? N200 C201 C202 174(3) . . ? _refine_diff_density_max 2.600 _refine_diff_density_min -1.413 _refine_diff_density_rms 0.337 #===END data_4 _database_code_CSD 202730 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 N16 Nd2 O18' _chemical_formula_weight 1187.14 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.932(17) _cell_length_b 14.53(2) _cell_length_c 13.23(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.913(10) _cell_angle_gamma 90.00 _cell_volume 2000(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.972 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 2.666 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.693 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6657 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3811 _reflns_number_gt 3380 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+2.9419P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3811 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.172940(14) 0.050774(11) 0.129540(12) 0.02166(7) Uani 1 d . . . N11 N 0.1756(3) 0.22693(19) 0.1110(2) 0.0293(6) Uani 1 d . . . C12 C 0.1132(4) 0.2811(3) 0.1611(3) 0.0386(8) Uani 1 d . . . H12 H 0.0596 0.2530 0.1945 0.046 Uiso 1 calc R . . C13 C 0.1235(4) 0.3755(3) 0.1661(3) 0.0458(10) Uani 1 d . . . H13 H 0.0767 0.4099 0.2007 0.055 Uiso 1 calc R . . C14 C 0.2039(4) 0.4176(3) 0.1192(3) 0.0459(10) Uani 1 d . . . H14 H 0.2139 0.4812 0.1221 0.055 Uiso 1 calc R . . C15 C 0.2700(4) 0.3637(2) 0.0675(3) 0.0397(8) Uani 1 d . . . H15 H 0.3258 0.3909 0.0356 0.048 Uiso 1 calc R . . C16 C 0.2532(3) 0.2694(2) 0.0631(3) 0.0281(7) Uani 1 d . . . C22 C 0.3126(3) 0.2096(2) 0.0004(2) 0.0259(7) Uani 1 d . . . N21 N 0.2927(2) 0.11807(19) 0.0039(2) 0.0258(6) Uani 1 d . . . C23 C 0.3808(3) 0.2465(3) -0.0633(3) 0.0368(8) Uani 1 d . . . H23 H 0.3943 0.3096 -0.0643 0.044 Uiso 1 calc R . . C24 C 0.4281(4) 0.1887(3) -0.1246(3) 0.0418(9) Uani 1 d . . . H24 H 0.4743 0.2124 -0.1671 0.050 Uiso 1 calc R . . C25 C 0.4065(3) 0.0955(3) -0.1228(3) 0.0357(8) Uani 1 d . . . H25 H 0.4366 0.0555 -0.1646 0.043 Uiso 1 calc R . . C26 C 0.3390(3) 0.0627(2) -0.0574(3) 0.0265(7) Uani 1 d . . . N31 N 0.2551(3) -0.06465(19) 0.0152(2) 0.0283(6) Uani 1 d . . . C32 C 0.3123(3) -0.0371(2) -0.0541(3) 0.0260(7) Uani 1 d . . . N33 N 0.3469(3) -0.0916(2) -0.1225(2) 0.0346(7) Uani 1 d . . . C34 C 0.3209(3) -0.1802(3) -0.1181(3) 0.0369(8) Uani 1 d . . . C35 C 0.2638(3) -0.2128(2) -0.0419(3) 0.0339(8) Uani 1 d . . . N36 N 0.2325(3) -0.15543(19) 0.0230(2) 0.0325(6) Uani 1 d . . . C300 C 0.3528(5) -0.2419(3) -0.1966(4) 0.0595(13) Uani 1 d . . . H30A H 0.2748 -0.2647 -0.2461 0.071 Uiso 1 calc R . . H30B H 0.4036 -0.2926 -0.1600 0.071 Uiso 1 calc R . . H30C H 0.4005 -0.2080 -0.2342 0.071 Uiso 1 calc R . . C350 C 0.2382(4) -0.3124(3) -0.0294(4) 0.0488(10) Uani 1 d . . . H35A H 0.3184 -0.3447 -0.0035 0.059 Uiso 1 calc R . . H35B H 0.1893 -0.3373 -0.0969 0.059 Uiso 1 calc R . . H35C H 0.1906 -0.3191 0.0202 0.059 Uiso 1 calc R . . O41 O 0.3844(2) 0.11923(18) 0.2439(2) 0.0394(6) Uani 1 d . . . N43 N 0.4316(3) 0.0456(2) 0.2892(3) 0.0384(7) Uani 1 d . . . O42 O 0.3704(3) -0.02735(19) 0.2520(2) 0.0488(7) Uani 1 d . . . O44 O 0.5296(3) 0.0443(2) 0.3640(3) 0.0788(12) Uani 1 d . . . O51 O -0.0220(2) 0.0842(2) 0.1865(2) 0.0418(6) Uani 1 d . . . N53 N 0.0372(3) 0.0882(2) 0.2862(3) 0.0389(7) Uani 1 d . . . O52 O 0.1590(3) 0.0881(2) 0.3117(2) 0.0466(7) Uani 1 d . . . O54 O -0.0202(4) 0.0916(3) 0.3508(3) 0.0645(9) Uani 1 d . . . N63 N -0.0280(3) 0.12883(19) -0.1276(2) 0.0287(6) Uani 1 d . . . O61 O -0.1166(2) 0.10072(18) -0.20723(19) 0.0364(6) Uani 1 d . . . O62 O 0.0034(2) 0.07393(16) -0.04801(17) 0.0285(5) Uani 1 d . . . O64 O 0.0236(3) 0.20262(19) -0.1260(2) 0.0480(7) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02232(10) 0.02168(10) 0.02114(10) -0.00038(6) 0.00696(7) -0.00089(6) N11 0.0348(15) 0.0213(14) 0.0318(15) -0.0033(11) 0.0101(12) 0.0013(11) C12 0.043(2) 0.0323(19) 0.047(2) -0.0016(16) 0.0233(17) 0.0026(16) C13 0.055(2) 0.032(2) 0.056(3) -0.0037(18) 0.025(2) 0.0060(17) C14 0.060(2) 0.0216(18) 0.056(3) -0.0005(17) 0.018(2) 0.0042(17) C15 0.047(2) 0.0287(19) 0.047(2) 0.0011(16) 0.0194(17) -0.0041(16) C16 0.0275(15) 0.0250(16) 0.0298(17) 0.0001(13) 0.0061(13) -0.0025(13) C22 0.0219(14) 0.0287(16) 0.0248(16) 0.0013(13) 0.0038(12) -0.0019(12) N21 0.0260(13) 0.0256(13) 0.0253(13) -0.0007(11) 0.0070(11) 0.0006(11) C23 0.0381(18) 0.0321(18) 0.043(2) 0.0072(16) 0.0169(16) -0.0032(15) C24 0.043(2) 0.048(2) 0.041(2) 0.0113(18) 0.0230(17) 0.0007(17) C25 0.0354(18) 0.044(2) 0.0311(18) 0.0007(16) 0.0151(15) 0.0041(16) C26 0.0234(15) 0.0294(17) 0.0249(16) -0.0009(13) 0.0046(12) 0.0034(12) N31 0.0259(14) 0.0286(15) 0.0313(15) -0.0007(12) 0.0103(11) 0.0010(11) C32 0.0187(14) 0.0300(17) 0.0282(16) -0.0027(13) 0.0057(12) 0.0024(12) N33 0.0314(15) 0.0397(18) 0.0346(17) -0.0131(13) 0.0132(13) -0.0013(13) C34 0.0267(17) 0.038(2) 0.043(2) -0.0163(16) 0.0065(15) -0.0005(14) C35 0.0273(16) 0.0322(18) 0.0367(19) -0.0078(15) 0.0018(14) 0.0025(14) N36 0.0375(15) 0.0232(14) 0.0348(16) -0.0010(12) 0.0084(12) 0.0013(12) C300 0.060(3) 0.054(3) 0.077(3) -0.040(2) 0.040(3) -0.016(2) C350 0.053(2) 0.031(2) 0.059(3) -0.0078(19) 0.013(2) 0.0000(18) O41 0.0344(13) 0.0334(14) 0.0442(15) -0.0024(12) 0.0032(11) -0.0034(11) N43 0.0271(15) 0.0432(19) 0.0381(17) -0.0082(14) 0.0000(13) 0.0032(13) O42 0.0391(15) 0.0349(14) 0.0583(18) -0.0050(13) -0.0058(13) 0.0028(12) O44 0.052(2) 0.074(2) 0.077(3) -0.0125(19) -0.0299(18) 0.0097(17) O51 0.0287(12) 0.0552(17) 0.0425(16) -0.0064(13) 0.0124(11) 0.0002(12) N53 0.0509(19) 0.0324(16) 0.0427(19) -0.0066(14) 0.0282(16) -0.0077(14) O52 0.0420(15) 0.0646(19) 0.0333(14) -0.0107(13) 0.0118(12) -0.0047(14) O54 0.082(2) 0.071(2) 0.062(2) -0.0165(17) 0.0533(19) -0.0197(19) N63 0.0292(14) 0.0282(15) 0.0279(14) 0.0066(12) 0.0074(11) -0.0039(11) O61 0.0403(14) 0.0345(14) 0.0268(12) 0.0073(10) -0.0009(10) -0.0063(11) O62 0.0296(12) 0.0289(12) 0.0241(12) 0.0072(9) 0.0039(9) -0.0012(9) O64 0.0568(17) 0.0338(15) 0.0460(16) 0.0111(12) 0.0049(13) -0.0165(13) _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 O51 2.517(4) . ? Nd1 O52 2.519(5) . ? Nd1 O62 2.527(4) . ? Nd1 O42 2.534(4) . ? Nd1 O41 2.544(4) . ? Nd1 N11 2.573(5) . ? Nd1 O61 2.583(4) 3 ? Nd1 N31 2.597(4) . ? Nd1 N21 2.603(4) . ? Nd1 O62 2.624(4) 3 ? Nd1 N53 2.947(5) . ? Nd1 N43 2.964(5) . ? N11 C12 1.342(5) . ? N11 C16 1.353(4) . ? C12 C13 1.377(6) . ? C13 C14 1.366(6) . ? C14 C15 1.381(6) . ? C15 C16 1.381(5) . ? C16 C22 1.482(5) . ? C22 N21 1.351(5) . ? C22 C23 1.392(5) . ? N21 C26 1.346(4) . ? C23 C24 1.375(6) . ? C24 C25 1.375(6) . ? C25 C26 1.383(5) . ? C26 C32 1.483(5) . ? N31 C32 1.320(5) . ? N31 N36 1.352(4) . ? C32 N33 1.341(4) . ? N33 C34 1.324(6) . ? C34 C35 1.421(6) . ? C34 C300 1.491(5) . ? C35 N36 1.315(5) . ? C35 C350 1.493(6) . ? O41 N43 1.256(4) . ? N43 O44 1.215(5) . ? N43 O42 1.270(4) . ? O51 N53 1.279(5) . ? N53 O54 1.207(4) . ? N53 O52 1.269(5) . ? N63 O64 1.209(4) . ? N63 O61 1.259(4) . ? N63 O62 1.281(4) . ? O61 Nd1 2.583(4) 3 ? O62 Nd1 2.624(4) 3 ? 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 O51 Nd1 O52 50.69(9) . . ? O51 Nd1 O62 78.81(14) . . ? O52 Nd1 O62 128.12(13) . . ? O51 Nd1 O42 121.91(14) . . ? O52 Nd1 O42 77.02(13) . . ? O62 Nd1 O42 152.96(9) . . ? O51 Nd1 O41 116.41(14) . . ? O52 Nd1 O41 70.01(12) . . ? O62 Nd1 O41 140.65(9) . . ? O42 Nd1 O41 49.86(12) . . ? O51 Nd1 N11 82.66(10) . . ? O52 Nd1 N11 83.28(10) . . ? O62 Nd1 N11 78.78(8) . . ? O42 Nd1 N11 118.32(10) . . ? O41 Nd1 N11 68.46(10) . . ? O51 Nd1 O61 73.60(11) . 3 ? O52 Nd1 O61 73.20(12) . 3 ? O62 Nd1 O61 106.66(10) . 3 ? O42 Nd1 O61 67.94(12) . 3 ? O41 Nd1 O61 112.39(11) . 3 ? N11 Nd1 O61 153.79(10) . 3 ? O51 Nd1 N31 140.84(9) . . ? O52 Nd1 N31 146.04(10) . . ? O62 Nd1 N31 80.26(14) . . ? O42 Nd1 N31 72.76(14) . . ? O41 Nd1 N31 100.67(13) . . ? N11 Nd1 N31 124.82(11) . . ? O61 Nd1 N31 81.31(14) 3 . ? O51 Nd1 N21 139.24(10) . . ? O52 Nd1 N21 136.07(11) . . ? O62 Nd1 N21 74.08(15) . . ? O42 Nd1 N21 94.56(15) . . ? O41 Nd1 N21 71.90(14) . . ? N11 Nd1 N21 62.77(9) . . ? O61 Nd1 N21 143.40(9) 3 . ? N31 Nd1 N21 62.52(13) . . ? O51 Nd1 O62 70.94(12) . 3 ? O52 Nd1 O62 106.79(10) . 3 ? O62 Nd1 O62 58.26(10) . 3 ? O42 Nd1 O62 109.09(13) . 3 ? O41 Nd1 O62 158.89(8) . 3 ? N11 Nd1 O62 132.57(10) . 3 ? O61 Nd1 O62 48.69(10) 3 3 ? N31 Nd1 O62 69.91(13) . 3 ? N21 Nd1 O62 116.58(12) . 3 ? O51 Nd1 N53 25.56(9) . . ? O52 Nd1 N53 25.34(10) . . ? O62 Nd1 N53 104.18(16) . . ? O42 Nd1 N53 98.48(16) . . ? O41 Nd1 N53 94.10(15) . . ? N11 Nd1 N53 84.63(9) . . ? O61 Nd1 N53 69.15(11) 3 . ? N31 Nd1 N53 150.23(9) . . ? N21 Nd1 N53 147.24(10) . . ? O62 Nd1 N53 87.21(12) 3 . ? O51 Nd1 N43 120.11(15) . . ? O52 Nd1 N43 69.45(13) . . ? O62 Nd1 N43 158.70(9) . . ? O42 Nd1 N43 25.17(10) . . ? O41 Nd1 N43 24.90(9) . . ? N11 Nd1 N43 93.26(9) . . ? O61 Nd1 N43 89.25(11) 3 . ? N31 Nd1 N43 88.49(13) . . ? N21 Nd1 N43 84.70(15) . . ? O62 Nd1 N43 133.99(10) 3 . ? N53 Nd1 N43 94.58(16) . . ? C12 N11 C16 116.8(3) . . ? C12 N11 Nd1 120.9(2) . . ? C16 N11 Nd1 121.7(2) . . ? N11 C12 C13 124.2(4) . . ? C14 C13 C12 118.6(4) . . ? C13 C14 C15 118.6(4) . . ? C16 C15 C14 120.0(4) . . ? N11 C16 C15 121.8(3) . . ? N11 C16 C22 116.1(3) . . ? C15 C16 C22 122.0(3) . . ? N21 C22 C23 121.4(3) . . ? N21 C22 C16 117.1(3) . . ? C23 C22 C16 121.4(3) . . ? C26 N21 C22 118.3(3) . . ? C26 N21 Nd1 121.1(2) . . ? C22 N21 Nd1 120.6(2) . . ? C24 C23 C22 119.3(4) . . ? C23 C24 C25 119.6(3) . . ? C24 C25 C26 118.5(3) . . ? N21 C26 C25 122.8(3) . . ? N21 C26 C32 117.0(3) . . ? C25 C26 C32 120.2(3) . . ? C32 N31 N36 119.0(3) . . ? C32 N31 Nd1 122.1(2) . . ? N36 N31 Nd1 118.8(2) . . ? N31 C32 N33 125.5(3) . . ? N31 C32 C26 117.2(3) . . ? N33 C32 C26 117.3(3) . . ? C34 N33 C32 115.8(3) . . ? N33 C34 C35 120.1(3) . . ? N33 C34 C300 117.1(4) . . ? C35 C34 C300 122.8(4) . . ? N36 C35 C34 120.7(3) . . ? N36 C35 C350 116.6(3) . . ? C34 C35 C350 122.7(3) . . ? C35 N36 N31 118.6(3) . . ? N43 O41 Nd1 96.6(2) . . ? O44 N43 O41 122.1(3) . . ? O44 N43 O42 122.0(3) . . ? O41 N43 O42 115.9(3) . . ? O44 N43 Nd1 171.9(3) . . ? O41 N43 Nd1 58.49(16) . . ? O42 N43 Nd1 58.11(17) . . ? N43 O42 Nd1 96.7(2) . . ? N53 O51 Nd1 96.3(2) . . ? O54 N53 O52 122.9(4) . . ? O54 N53 O51 121.6(4) . . ? O52 N53 O51 115.5(3) . . ? O54 N53 Nd1 171.7(3) . . ? O52 N53 Nd1 58.16(18) . . ? O51 N53 Nd1 58.09(19) . . ? N53 O52 Nd1 96.5(2) . . ? O64 N63 O61 122.5(3) . . ? O64 N63 O62 122.2(3) . . ? O61 N63 O62 115.3(3) . . ? N63 O61 Nd1 99.21(19) . 3 ? N63 O62 Nd1 141.39(19) . . ? N63 O62 Nd1 96.61(19) . 3 ? Nd1 O62 Nd1 121.75(11) . 3 ? _refine_diff_density_max 0.850 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.092 #===END data_5 _database_code_CSD 202731 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H25 Gd N8 O15' _chemical_formula_weight 714.68 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.183(14) _cell_length_b 9.585(14) _cell_length_c 16.57(2) _cell_angle_alpha 82.415(10) _cell_angle_beta 82.379(10) _cell_angle_gamma 78.879(10) _cell_volume 1257(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.889 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 710 _exptl_absorpt_coefficient_mu 2.727 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.585 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3877 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.09 _reflns_number_total 3877 _reflns_number_gt 3460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+5.6420P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3877 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.74096(4) 0.93192(3) 0.777064(17) 0.02241(15) Uani 1 d . . . N11 N 0.6739(8) 0.7461(6) 0.6954(3) 0.0270(13) Uani 1 d . . . C12 C 0.6354(10) 0.6216(8) 0.7332(5) 0.0331(17) Uani 1 d . . . H12 H 0.6393 0.6032 0.7895 0.040 Uiso 1 calc R . . C13 C 0.5905(11) 0.5196(9) 0.6932(5) 0.0375(18) Uani 1 d . . . H13 H 0.5628 0.4356 0.7217 0.045 Uiso 1 calc R . . C14 C 0.5878(13) 0.5464(9) 0.6094(5) 0.045(2) Uani 1 d . . . H14 H 0.5568 0.4805 0.5805 0.054 Uiso 1 calc R . . C15 C 0.6312(11) 0.6710(9) 0.5689(5) 0.0358(18) Uani 1 d . . . H15 H 0.6326 0.6889 0.5123 0.043 Uiso 1 calc R . . C16 C 0.6734(9) 0.7709(7) 0.6136(4) 0.0250(14) Uani 1 d . . . N21 N 0.7809(8) 0.9854(6) 0.6208(3) 0.0241(12) Uani 1 d . . . C22 C 0.7253(9) 0.9060(7) 0.5727(4) 0.0253(14) Uani 1 d . . . C23 C 0.7141(10) 0.9488(9) 0.4897(4) 0.0322(16) Uani 1 d . . . H23 H 0.6731 0.8931 0.4579 0.039 Uiso 1 calc R . . C24 C 0.7644(10) 1.0747(9) 0.4552(4) 0.0332(17) Uani 1 d . . . H24 H 0.7567 1.1055 0.4000 0.040 Uiso 1 calc R . . C25 C 0.8264(10) 1.1544(9) 0.5036(4) 0.0327(17) Uani 1 d . . . H25 H 0.8624 1.2392 0.4817 0.039 Uiso 1 calc R . . C26 C 0.8336(9) 1.1056(8) 0.5845(4) 0.0271(15) Uani 1 d . . . C32 C 0.9015(8) 1.1868(7) 0.6393(4) 0.0230(14) Uani 1 d . . . N31 N 0.8967(8) 1.1407(6) 0.7182(3) 0.0263(13) Uani 1 d . . . N33 N 0.9635(9) 1.3040(7) 0.6045(4) 0.0320(14) Uani 1 d . . . C34 C 1.0213(10) 1.3764(8) 0.6528(5) 0.0302(16) Uani 1 d . . . C300 C 1.0878(12) 1.5073(8) 0.6170(5) 0.0382(19) Uani 1 d . . . H30A H 1.0817 1.5210 0.5589 0.046 Uiso 1 calc R . . H30B H 1.2023 1.4970 0.6275 0.046 Uiso 1 calc R . . H30C H 1.0223 1.5886 0.6413 0.046 Uiso 1 calc R . . C35 C 1.0178(10) 1.3296(8) 0.7376(5) 0.0315(16) Uani 1 d . . . C350 C 1.0802(15) 1.4073(10) 0.7959(5) 0.052(2) Uani 1 d . . . H35A H 1.0221 1.5046 0.7930 0.063 Uiso 1 calc R . . H35B H 1.1982 1.4057 0.7818 0.063 Uiso 1 calc R . . H35C H 1.0608 1.3617 0.8506 0.063 Uiso 1 calc R . . N36 N 0.9557(8) 1.2129(7) 0.7695(4) 0.0306(13) Uani 1 d . . . O100 O 0.6945(7) 1.0667(6) 0.8895(3) 0.0302(11) Uani 1 d . . . O200 O 0.4817(7) 0.8750(6) 0.8467(3) 0.0346(12) Uani 1 d . . . O300 O 0.7937(7) 0.7292(6) 0.8805(3) 0.0368(12) Uani 1 d . . . O51 O 0.5527(7) 1.1573(7) 0.7393(3) 0.0406(14) Uani 1 d . . . N53 N 0.4481(8) 1.1492(7) 0.6908(4) 0.0287(13) Uani 1 d . . . O54 O 0.3877(10) 1.2562(7) 0.6484(5) 0.0580(19) Uani 1 d . . . O52 O 0.4199(12) 1.0297(8) 0.6842(4) 0.066(2) Uani 1 d . . . O62 O 1.0397(8) 0.8981(6) 0.8265(3) 0.0389(13) Uani 1 d . . . O61 O 1.0095(7) 0.7966(6) 0.7216(3) 0.0362(12) Uani 1 d . . . N63 N 1.1057(8) 0.8217(7) 0.7714(4) 0.0308(14) Uani 1 d . . . O64 O 1.2537(8) 0.7691(8) 0.7642(4) 0.0545(17) Uani 1 d . . . N73 N 0.4754(10) 1.4085(8) 0.9193(4) 0.0458(18) Uani 1 d . . . O71 O 0.6180(10) 1.3563(7) 0.8871(4) 0.0591(19) Uani 1 d . . . O72 O 0.3812(11) 1.3289(9) 0.9580(5) 0.069(2) Uani 1 d . . . O74 O 0.4279(11) 1.5389(8) 0.9121(5) 0.072(2) Uani 1 d . . . O400 O 0.3241(8) 1.0602(7) 0.9538(3) 0.0434(14) Uani 1 d . . . O500 O 0.9922(8) 1.1377(7) 0.9530(4) 0.0455(14) Uani 1 d . . . O600 O 1.0715(8) 0.6179(7) 0.9632(4) 0.0494(16) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0231(2) 0.0237(2) 0.0207(2) -0.00163(13) -0.00219(13) -0.00539(16) N11 0.025(3) 0.028(3) 0.027(3) -0.002(2) -0.003(2) -0.003(3) C12 0.032(4) 0.031(4) 0.034(4) -0.002(3) 0.000(3) -0.003(4) C13 0.041(5) 0.034(4) 0.043(4) -0.003(3) -0.005(3) -0.020(4) C14 0.057(6) 0.038(5) 0.049(5) -0.008(4) -0.015(4) -0.022(5) C15 0.041(5) 0.038(4) 0.033(4) -0.005(3) -0.013(3) -0.011(4) C16 0.023(3) 0.022(3) 0.030(3) -0.002(3) -0.001(3) -0.004(3) N21 0.029(3) 0.025(3) 0.017(2) 0.003(2) -0.005(2) -0.002(3) C22 0.028(4) 0.027(3) 0.023(3) -0.004(3) -0.007(3) -0.006(3) C23 0.034(4) 0.040(4) 0.027(4) -0.002(3) -0.005(3) -0.018(4) C24 0.034(4) 0.041(4) 0.025(3) 0.002(3) -0.005(3) -0.012(4) C25 0.038(4) 0.033(4) 0.029(4) 0.002(3) -0.003(3) -0.015(4) C26 0.026(4) 0.025(3) 0.030(3) -0.003(3) -0.005(3) -0.003(3) C32 0.017(3) 0.025(3) 0.028(3) -0.003(3) -0.002(2) -0.004(3) N31 0.029(3) 0.027(3) 0.024(3) -0.002(2) -0.003(2) -0.008(3) N33 0.034(4) 0.029(3) 0.034(3) 0.003(3) -0.007(3) -0.011(3) C34 0.030(4) 0.029(4) 0.033(4) 0.000(3) -0.006(3) -0.008(3) C300 0.051(5) 0.024(4) 0.040(4) -0.001(3) -0.004(4) -0.011(4) C35 0.034(4) 0.026(4) 0.036(4) -0.002(3) -0.005(3) -0.008(3) C350 0.085(7) 0.046(5) 0.037(4) -0.005(4) -0.013(4) -0.033(5) N36 0.032(3) 0.032(3) 0.030(3) 0.001(2) -0.006(2) -0.010(3) O100 0.034(3) 0.031(3) 0.026(2) -0.007(2) -0.003(2) -0.005(2) O200 0.024(3) 0.041(3) 0.039(3) -0.004(2) 0.001(2) -0.010(3) O300 0.034(3) 0.033(3) 0.038(3) 0.009(2) -0.005(2) -0.002(3) O51 0.030(3) 0.053(4) 0.039(3) -0.006(3) -0.016(2) 0.002(3) N53 0.026(3) 0.027(3) 0.033(3) -0.004(2) -0.004(2) -0.004(3) O54 0.063(5) 0.042(4) 0.069(5) 0.005(3) -0.040(4) 0.005(4) O52 0.113(7) 0.052(4) 0.046(4) -0.004(3) -0.020(4) -0.037(5) O62 0.045(3) 0.037(3) 0.036(3) -0.004(2) -0.010(2) -0.006(3) O61 0.031(3) 0.044(3) 0.037(3) -0.015(2) -0.002(2) -0.007(3) N63 0.020(3) 0.030(3) 0.041(3) 0.000(3) -0.006(2) -0.002(3) O64 0.026(3) 0.060(4) 0.079(5) -0.018(4) -0.013(3) 0.001(3) N73 0.051(5) 0.045(4) 0.038(4) -0.002(3) 0.003(3) -0.007(4) O71 0.064(5) 0.043(4) 0.062(4) -0.006(3) 0.017(4) -0.008(4) O72 0.074(5) 0.064(5) 0.070(5) -0.016(4) 0.022(4) -0.032(5) O74 0.082(6) 0.040(4) 0.079(5) -0.002(4) 0.013(4) 0.010(4) O400 0.038(3) 0.052(4) 0.038(3) -0.007(3) -0.003(2) -0.003(3) O500 0.037(3) 0.047(3) 0.056(4) -0.005(3) -0.015(3) -0.010(3) O600 0.051(4) 0.043(3) 0.054(4) -0.002(3) -0.017(3) 0.000(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 Gd1 O100 2.355(5) . ? Gd1 O200 2.401(6) . ? Gd1 O300 2.427(6) . ? Gd1 O61 2.457(6) . ? Gd1 O51 2.459(6) . ? Gd1 N11 2.553(7) . ? Gd1 N21 2.563(6) . ? Gd1 N31 2.592(7) . ? Gd1 O62 2.628(7) . ? N11 C12 1.346(10) . ? N11 C16 1.346(9) . ? C12 C13 1.381(11) . ? C13 C14 1.380(12) . ? C14 C15 1.376(12) . ? C15 C16 1.402(10) . ? C16 C22 1.490(10) . ? N21 C22 1.345(9) . ? N21 C26 1.347(10) . ? C22 C23 1.393(10) . ? C23 C24 1.378(11) . ? C24 C25 1.380(11) . ? C25 C26 1.365(10) . ? C26 C32 1.493(10) . ? C32 N31 1.322(9) . ? C32 N33 1.351(9) . ? N31 N36 1.351(8) . ? N33 C34 1.311(10) . ? C34 C35 1.417(10) . ? C34 C300 1.485(11) . ? C35 N36 1.334(10) . ? C35 C350 1.489(11) . ? O51 N53 1.268(8) . ? N53 O54 1.223(9) . ? N53 O52 1.233(9) . ? O62 N63 1.246(9) . ? O61 N63 1.287(8) . ? N63 O64 1.215(9) . ? N73 O74 1.230(10) . ? N73 O72 1.247(11) . ? N73 O71 1.255(10) . ? 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 O100 Gd1 O200 77.3(2) . . ? O100 Gd1 O300 83.9(2) . . ? O200 Gd1 O300 69.5(2) . . ? O100 Gd1 O61 126.83(19) . . ? O200 Gd1 O61 136.1(2) . . ? O300 Gd1 O61 76.9(2) . . ? O100 Gd1 O51 72.5(2) . . ? O200 Gd1 O51 80.6(2) . . ? O300 Gd1 O51 145.4(2) . . ? O61 Gd1 O51 137.6(2) . . ? O100 Gd1 N11 153.0(2) . . ? O200 Gd1 N11 76.0(2) . . ? O300 Gd1 N11 83.5(2) . . ? O61 Gd1 N11 72.8(2) . . ? O51 Gd1 N11 106.4(2) . . ? O100 Gd1 N21 136.1(2) . . ? O200 Gd1 N21 120.9(2) . . ? O300 Gd1 N21 138.62(19) . . ? O61 Gd1 N21 69.98(19) . . ? O51 Gd1 N21 72.15(18) . . ? N11 Gd1 N21 63.8(2) . . ? O100 Gd1 N31 79.2(2) . . ? O200 Gd1 N31 143.95(19) . . ? O300 Gd1 N31 134.2(2) . . ? O61 Gd1 N31 79.9(2) . . ? O51 Gd1 N31 66.4(2) . . ? N11 Gd1 N31 125.91(19) . . ? N21 Gd1 N31 63.25(19) . . ? O100 Gd1 O62 76.61(19) . . ? O200 Gd1 O62 131.2(2) . . ? O300 Gd1 O62 67.29(19) . . ? O61 Gd1 O62 50.22(19) . . ? O51 Gd1 O62 128.0(2) . . ? N11 Gd1 O62 119.58(19) . . ? N21 Gd1 O62 106.43(19) . . ? N31 Gd1 O62 67.4(2) . . ? O100 Gd1 N63 101.46(19) . . ? O200 Gd1 N63 139.64(19) . . ? O300 Gd1 N63 70.22(19) . . ? O61 Gd1 N63 25.37(18) . . ? O51 Gd1 N63 138.3(2) . . ? N11 Gd1 N63 96.5(2) . . ? N21 Gd1 N63 88.27(18) . . ? N31 Gd1 N63 71.9(2) . . ? O62 Gd1 N63 24.86(18) . . ? C12 N11 C16 118.2(6) . . ? C12 N11 Gd1 120.8(5) . . ? C16 N11 Gd1 120.9(5) . . ? N11 C12 C13 123.7(7) . . ? C14 C13 C12 117.9(7) . . ? C15 C14 C13 119.6(8) . . ? C14 C15 C16 119.6(7) . . ? N11 C16 C15 121.0(7) . . ? N11 C16 C22 117.1(6) . . ? C15 C16 C22 121.8(6) . . ? C22 N21 C26 117.2(6) . . ? C22 N21 Gd1 120.6(4) . . ? C26 N21 Gd1 121.4(4) . . ? N21 C22 C23 121.9(7) . . ? N21 C22 C16 116.3(6) . . ? C23 C22 C16 121.8(6) . . ? C24 C23 C22 119.2(7) . . ? C23 C24 C25 119.2(7) . . ? C26 C25 C24 118.2(7) . . ? N21 C26 C25 124.2(7) . . ? N21 C26 C32 115.4(6) . . ? C25 C26 C32 120.4(7) . . ? N31 C32 N33 124.2(6) . . ? N31 C32 C26 118.6(6) . . ? N33 C32 C26 117.2(6) . . ? C32 N31 N36 119.8(6) . . ? C32 N31 Gd1 119.8(5) . . ? N36 N31 Gd1 119.9(4) . . ? C34 N33 C32 117.3(6) . . ? N33 C34 C35 119.8(7) . . ? N33 C34 C300 118.8(7) . . ? C35 C34 C300 121.4(7) . . ? N36 C35 C34 120.9(7) . . ? N36 C35 C350 116.5(7) . . ? C34 C35 C350 122.5(7) . . ? C35 N36 N31 118.0(6) . . ? N53 O51 Gd1 115.3(5) . . ? O54 N53 O52 122.1(7) . . ? O54 N53 O51 120.1(7) . . ? O52 N53 O51 117.7(7) . . ? N63 O62 Gd1 92.7(4) . . ? N63 O61 Gd1 99.8(4) . . ? O64 N63 O62 123.1(7) . . ? O64 N63 O61 119.6(7) . . ? O62 N63 O61 117.3(6) . . ? O64 N63 Gd1 174.4(6) . . ? O62 N63 Gd1 62.4(4) . . ? O61 N63 Gd1 54.8(3) . . ? O74 N73 O72 119.8(9) . . ? O74 N73 O71 119.8(8) . . ? O72 N73 O71 120.4(8) . . ? _refine_diff_density_max 1.632 _refine_diff_density_min -1.780 _refine_diff_density_rms 0.188 #===END data_6 _database_code_CSD 202732 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H13 Er N8 O12 ' _chemical_formula_weight 664.60 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.652(13) _cell_length_b 10.803(17) _cell_length_c 14.55(2) _cell_angle_alpha 95.914(10) _cell_angle_beta 101.427(10) _cell_angle_gamma 95.431(10) _cell_volume 1165(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow-brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 646 _exptl_absorpt_coefficient_mu 3.679 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.386 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3598 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.09 _reflns_number_total 3598 _reflns_number_gt 3111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1250P)^2^+3.5478P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0060(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3598 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1793 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.18113(5) 0.11144(3) 0.24355(3) 0.0400(2) Uani 1 d . . . N53 N 0.5117(13) 0.2645(8) 0.2643(8) 0.051(2) Uani 1 d . . . O51 O 0.3632(10) 0.3093(6) 0.2492(6) 0.0556(19) Uani 1 d . . . O54 O 0.6564(13) 0.3294(9) 0.2748(10) 0.077(3) Uani 1 d . . . O52 O 0.5065(10) 0.1491(6) 0.2738(6) 0.0522(18) Uani 1 d . . . N43 N -0.0030(13) 0.5673(9) 0.2008(9) 0.060(3) Uani 1 d . . . O42 O -0.0421(14) 0.6722(8) 0.1934(8) 0.079(3) Uani 1 d . . . O41 O -0.005(2) 0.4925(12) 0.1310(10) 0.119(5) Uani 1 d . . . O44 O 0.0291(18) 0.5296(12) 0.2788(11) 0.098(4) Uani 1 d . . . N63 N -0.1609(13) -0.0336(8) 0.2072(9) 0.055(2) Uani 1 d . . . O64 O -0.3066(14) -0.0978(10) 0.1937(10) 0.085(3) Uani 1 d . . . O61 O -0.0801(11) 0.0164(8) 0.2875(6) 0.060(2) Uani 1 d . . . O62 O -0.0849(12) -0.0110(8) 0.1404(6) 0.064(2) Uani 1 d . . . N11 N 0.2130(14) 0.2159(8) 0.4068(7) 0.054(2) Uani 1 d . . . C12 C 0.205(2) 0.3402(11) 0.4287(12) 0.074(4) Uani 1 d . . . H12 H 0.1979 0.3898 0.3798 0.089 Uiso 1 calc R . . C13 C 0.207(2) 0.3973(13) 0.5157(12) 0.082(4) Uani 1 d . . . H13 H 0.2017 0.4831 0.5256 0.099 Uiso 1 calc R . . C14 C 0.217(2) 0.3261(13) 0.5903(10) 0.072(4) Uani 1 d . . . H14 H 0.2135 0.3626 0.6505 0.087 Uiso 1 calc R . . C15 C 0.2314(17) 0.2014(12) 0.5731(9) 0.059(3) Uani 1 d . . . H15 H 0.2429 0.1523 0.6224 0.071 Uiso 1 calc R . . C16 C 0.2290(13) 0.1475(10) 0.4814(8) 0.046(2) Uani 1 d . . . C22 C 0.2552(14) 0.0146(10) 0.4609(8) 0.046(2) Uani 1 d . . . N21 N 0.2704(11) -0.0211(7) 0.3725(5) 0.0385(16) Uani 1 d . . . C26 C 0.2962(12) -0.1419(9) 0.3480(7) 0.0381(19) Uani 1 d . . . C25 C 0.3028(15) -0.2282(10) 0.4121(8) 0.052(2) Uani 1 d . . . H25 H 0.3205 -0.3102 0.3935 0.062 Uiso 1 calc R . . C24 C 0.2838(17) -0.1950(11) 0.5013(9) 0.058(3) Uani 1 d . . . H24 H 0.2873 -0.2528 0.5446 0.069 Uiso 1 calc R . . C23 C 0.2584(18) -0.0698(12) 0.5259(10) 0.059(3) Uani 1 d . . . H23 H 0.2437 -0.0437 0.5866 0.071 Uiso 1 calc R . . C32 C 0.3204(12) -0.1735(8) 0.2512(7) 0.039(2) Uani 1 d . . . N31 N 0.2731(11) -0.0927(7) 0.1912(6) 0.0403(17) Uani 1 d . . . N36 N 0.2903(13) -0.1191(8) 0.1009(7) 0.049(2) Uani 1 d . . . C35 C 0.3500(16) -0.2260(10) 0.0756(9) 0.051(3) Uani 1 d . . . C34 C 0.3996(14) -0.3104(9) 0.1434(9) 0.051(3) Uani 1 d . . . N33 N 0.3814(13) -0.2850(8) 0.2307(7) 0.046(2) Uani 1 d . . . C350 C 0.375(2) -0.2471(14) -0.0234(9) 0.068(3) Uani 1 d . . . H35A H 0.3394 -0.1776 -0.0558 0.081 Uiso 1 calc R . . H35B H 0.3031 -0.3227 -0.0551 0.081 Uiso 1 calc R . . H35C H 0.4993 -0.2545 -0.0231 0.081 Uiso 1 calc R . . C300 C 0.477(2) -0.4267(12) 0.1198(11) 0.069(4) Uani 1 d . . . H30A H 0.5132 -0.4650 0.1761 0.083 Uiso 1 calc R . . H30B H 0.5795 -0.4072 0.0928 0.083 Uiso 1 calc R . . H30C H 0.3886 -0.4835 0.0751 0.083 Uiso 1 calc R . . O100 O -0.0182(10) 0.2611(7) 0.2193(6) 0.0548(18) Uani 1 d . . . O200 O 0.2155(12) 0.1260(7) 0.0914(6) 0.0585(19) Uani 1 d . . . O300 O 0.131(2) 0.3181(11) 0.0055(9) 0.099(4) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0397(3) 0.0385(3) 0.0428(4) 0.00589(18) 0.0108(2) 0.00446(18) N53 0.042(5) 0.044(5) 0.067(7) 0.012(4) 0.015(4) -0.004(4) O51 0.047(4) 0.038(3) 0.084(6) 0.007(3) 0.015(4) 0.011(3) O54 0.053(5) 0.060(5) 0.123(9) 0.018(5) 0.033(6) -0.003(4) O52 0.050(4) 0.039(4) 0.069(5) 0.012(3) 0.010(4) 0.007(3) N43 0.051(6) 0.054(5) 0.080(8) 0.014(5) 0.025(5) 0.003(4) O42 0.086(6) 0.043(4) 0.111(8) 0.016(4) 0.019(6) 0.016(4) O41 0.140(12) 0.101(9) 0.106(11) -0.043(7) 0.028(9) 0.019(8) O44 0.104(9) 0.085(7) 0.116(11) 0.044(7) 0.030(8) 0.014(6) N63 0.045(5) 0.039(4) 0.085(8) 0.012(4) 0.019(5) -0.001(4) O64 0.057(6) 0.076(6) 0.114(10) 0.003(6) 0.013(6) -0.018(5) O61 0.054(5) 0.077(5) 0.051(5) 0.013(4) 0.015(4) -0.004(4) O62 0.057(5) 0.076(5) 0.050(5) -0.011(4) 0.006(4) -0.003(4) N11 0.065(6) 0.043(4) 0.055(6) 0.000(4) 0.017(5) 0.015(4) C12 0.091(10) 0.042(6) 0.089(11) 0.002(6) 0.020(8) 0.009(6) C13 0.112(12) 0.053(7) 0.079(11) -0.011(6) 0.016(9) 0.023(7) C14 0.088(9) 0.080(8) 0.046(8) -0.017(6) 0.013(7) 0.026(7) C15 0.057(7) 0.072(7) 0.047(7) -0.001(5) 0.013(5) 0.008(5) C16 0.039(5) 0.054(5) 0.041(6) 0.002(4) 0.001(4) 0.007(4) C22 0.039(5) 0.050(5) 0.049(7) 0.008(4) 0.005(4) 0.004(4) N21 0.046(4) 0.048(4) 0.021(4) 0.004(3) 0.006(3) 0.004(3) C26 0.035(5) 0.042(4) 0.036(5) 0.004(4) 0.006(4) 0.004(4) C25 0.058(6) 0.049(5) 0.050(7) 0.013(4) 0.012(5) 0.012(5) C24 0.064(7) 0.059(6) 0.052(7) 0.023(5) 0.009(5) 0.008(5) C23 0.064(7) 0.067(7) 0.054(8) 0.011(5) 0.024(6) 0.015(6) C32 0.028(4) 0.040(5) 0.045(6) 0.005(4) 0.003(4) -0.004(3) N31 0.041(4) 0.036(4) 0.040(5) 0.002(3) 0.005(3) 0.000(3) N36 0.052(5) 0.048(5) 0.052(6) 0.010(4) 0.016(4) 0.015(4) C35 0.051(6) 0.049(5) 0.050(7) -0.013(4) 0.016(5) -0.002(4) C34 0.046(6) 0.040(5) 0.068(8) 0.002(4) 0.020(5) 0.000(4) N33 0.054(5) 0.039(4) 0.045(5) 0.011(3) 0.009(4) 0.005(4) C350 0.074(8) 0.077(8) 0.056(8) 0.000(6) 0.024(7) 0.020(7) C300 0.079(9) 0.055(7) 0.078(10) -0.001(6) 0.027(8) 0.018(6) O100 0.052(4) 0.044(4) 0.069(5) 0.007(3) 0.010(4) 0.016(3) O200 0.076(5) 0.059(4) 0.045(5) 0.011(3) 0.021(4) 0.009(4) O300 0.149(11) 0.083(7) 0.076(8) 0.031(6) 0.026(8) 0.034(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O200 2.300(8) . ? Er1 O100 2.331(7) . ? Er1 O61 2.391(8) . ? Er1 O51 2.423(8) . ? Er1 O52 2.428(9) . ? Er1 O62 2.453(9) . ? Er1 N31 2.469(8) . ? Er1 N11 2.478(10) . ? Er1 N21 2.504(8) . ? N53 O54 1.226(13) . ? N53 O52 1.266(11) . ? N53 O51 1.266(12) . ? N43 O42 1.209(13) . ? N43 O41 1.228(16) . ? N43 O44 1.233(17) . ? N63 O64 1.225(13) . ? N63 O61 1.250(14) . ? N63 O62 1.260(14) . ? N11 C12 1.357(15) . ? N11 C16 1.367(15) . ? C12 C13 1.35(2) . ? C13 C14 1.39(2) . ? C14 C15 1.364(18) . ? C15 C16 1.396(15) . ? C16 C22 1.478(15) . ? C22 N21 1.336(14) . ? C22 C23 1.379(17) . ? N21 C26 1.360(12) . ? C26 C25 1.383(14) . ? C26 C32 1.467(14) . ? C25 C24 1.350(17) . ? C24 C23 1.405(18) . ? C32 N31 1.321(13) . ? C32 N33 1.359(13) . ? N31 N36 1.351(12) . ? N36 C35 1.326(13) . ? C35 C34 1.432(17) . ? C35 C350 1.489(16) . ? C34 N33 1.309(15) . ? C34 C300 1.476(15) . ? 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 O200 Er1 O100 86.4(3) . . ? O200 Er1 O61 125.6(3) . . ? O100 Er1 O61 77.2(3) . . ? O200 Er1 O51 74.0(3) . . ? O100 Er1 O51 73.7(3) . . ? O61 Er1 O51 143.6(3) . . ? O200 Er1 O52 81.3(3) . . ? O100 Er1 O52 126.5(3) . . ? O61 Er1 O52 147.9(3) . . ? O51 Er1 O52 52.8(2) . . ? O200 Er1 O62 74.1(3) . . ? O100 Er1 O62 77.7(3) . . ? O61 Er1 O62 52.0(3) . . ? O51 Er1 O62 137.9(3) . . ? O52 Er1 O62 144.3(3) . . ? O200 Er1 N31 75.5(3) . . ? O100 Er1 N31 148.9(3) . . ? O61 Er1 N31 93.0(3) . . ? O51 Er1 N31 123.0(3) . . ? O52 Er1 N31 75.9(3) . . ? O62 Er1 N31 73.2(3) . . ? O200 Er1 N11 148.3(3) . . ? O100 Er1 N11 78.8(3) . . ? O61 Er1 N11 78.3(3) . . ? O51 Er1 N11 75.0(3) . . ? O52 Er1 N11 85.3(3) . . ? O62 Er1 N11 128.4(3) . . ? N31 Er1 N11 128.6(3) . . ? O200 Er1 N21 138.8(3) . . ? O100 Er1 N21 134.3(3) . . ? O61 Er1 N21 70.0(3) . . ? O51 Er1 N21 117.8(3) . . ? O52 Er1 N21 78.1(3) . . ? O62 Er1 N21 104.2(3) . . ? N31 Er1 N21 65.1(3) . . ? N11 Er1 N21 64.3(3) . . ? O200 Er1 N53 75.4(3) . . ? O100 Er1 N53 100.2(3) . . ? O61 Er1 N53 158.0(3) . . ? O51 Er1 N53 26.4(3) . . ? O52 Er1 N53 26.4(3) . . ? O62 Er1 N53 149.4(3) . . ? N31 Er1 N53 99.4(3) . . ? N11 Er1 N53 79.8(3) . . ? N21 Er1 N53 98.9(3) . . ? O200 Er1 N63 100.2(3) . . ? O100 Er1 N63 76.8(3) . . ? O61 Er1 N63 25.8(3) . . ? O51 Er1 N63 150.3(3) . . ? O52 Er1 N63 156.5(3) . . ? O62 Er1 N63 26.2(3) . . ? N31 Er1 N63 81.7(3) . . ? N11 Er1 N63 103.5(3) . . ? N21 Er1 N63 86.1(3) . . ? N53 Er1 N63 174.9(3) . . ? O54 N53 O52 120.3(10) . . ? O54 N53 O51 122.6(9) . . ? O52 N53 O51 117.0(8) . . ? O54 N53 Er1 178.6(9) . . ? O52 N53 Er1 58.6(5) . . ? O51 N53 Er1 58.4(5) . . ? N53 O51 Er1 95.2(5) . . ? N53 O52 Er1 94.9(6) . . ? O42 N43 O41 121.5(14) . . ? O42 N43 O44 120.6(13) . . ? O41 N43 O44 117.8(13) . . ? O64 N63 O61 122.3(12) . . ? O64 N63 O62 122.1(13) . . ? O61 N63 O62 115.6(9) . . ? O64 N63 Er1 178.2(10) . . ? O61 N63 Er1 56.4(5) . . ? O62 N63 Er1 59.3(5) . . ? N63 O61 Er1 97.8(6) . . ? N63 O62 Er1 94.5(7) . . ? C12 N11 C16 115.3(11) . . ? C12 N11 Er1 124.0(9) . . ? C16 N11 Er1 120.6(7) . . ? C13 C12 N11 125.1(14) . . ? C12 C13 C14 119.1(12) . . ? C15 C14 C13 118.4(11) . . ? C14 C15 C16 119.8(12) . . ? N11 C16 C15 122.2(10) . . ? N11 C16 C22 116.3(9) . . ? C15 C16 C22 121.4(10) . . ? N21 C22 C23 121.1(10) . . ? N21 C22 C16 115.2(9) . . ? C23 C22 C16 123.6(11) . . ? C22 N21 C26 118.9(8) . . ? C22 N21 Er1 121.1(6) . . ? C26 N21 Er1 118.4(6) . . ? N21 C26 C25 121.3(9) . . ? N21 C26 C32 116.2(8) . . ? C25 C26 C32 122.6(9) . . ? C24 C25 C26 120.9(10) . . ? C25 C24 C23 117.3(10) . . ? C22 C23 C24 120.4(11) . . ? N31 C32 N33 126.3(9) . . ? N31 C32 C26 116.5(8) . . ? N33 C32 C26 117.1(8) . . ? C32 N31 N36 118.5(8) . . ? C32 N31 Er1 121.6(6) . . ? N36 N31 Er1 119.7(6) . . ? C35 N36 N31 118.7(9) . . ? N36 C35 C34 120.6(10) . . ? N36 C35 C350 116.4(11) . . ? C34 C35 C350 122.9(10) . . ? N33 C34 C35 120.5(9) . . ? N33 C34 C300 117.1(11) . . ? C35 C34 C300 122.4(11) . . ? C34 N33 C32 115.4(9) . . ? _refine_diff_density_max 1.502 _refine_diff_density_min -1.561 _refine_diff_density_rms 0.209 data_7 _database_code_CSD 202733 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H15 N8 O11 Y' _chemical_formula_weight 572.26 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.212(11) _cell_length_b 10.887(14) _cell_length_c 12.361(14) _cell_angle_alpha 104.701(10) _cell_angle_beta 98.626(10) _cell_angle_gamma 107.551(10) _cell_volume 1108(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 2.706 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.452 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3745 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.14 _reflns_number_total 3745 _reflns_number_gt 2830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1528P)^2^+2.1748P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3745 _refine_ls_number_parameters 326 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1118 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.2226 _refine_ls_wR_factor_gt 0.1981 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.13085(8) 0.31946(7) 0.22138(5) 0.0372(3) Uani 1 d . . . N11 N 0.3106(7) 0.1985(6) 0.1611(5) 0.0411(13) Uani 1 d . . . C12 C 0.2766(10) 0.0682(8) 0.1499(7) 0.0509(19) Uani 1 d . . . H12 H 0.1755 0.0185 0.1511 0.061 Uiso 1 calc R . . C13 C 0.3807(11) 0.0018(9) 0.1365(7) 0.056(2) Uani 1 d . . . H13 H 0.3531 -0.0896 0.1308 0.068 Uiso 1 calc R . . C14 C 0.5280(11) 0.0768(9) 0.1318(7) 0.055(2) Uani 1 d . . . H14 H 0.6035 0.0365 0.1257 0.067 Uiso 1 calc R . . C15 C 0.5651(10) 0.2087(9) 0.1360(6) 0.0521(19) Uani 1 d . . . H15 H 0.6629 0.2576 0.1285 0.063 Uiso 1 calc R . . C16 C 0.4527(8) 0.2688(8) 0.1517(5) 0.0420(16) Uani 1 d . . . C22 C 0.4898(9) 0.4127(8) 0.1641(6) 0.0412(16) Uani 1 d . . . N21 N 0.3862(7) 0.4682(6) 0.2048(5) 0.0407(14) Uani 1 d . . . C23 C 0.6208(10) 0.4929(10) 0.1387(7) 0.059(2) Uani 1 d . . . H23 H 0.6897 0.4543 0.1091 0.070 Uiso 1 calc R . . C24 C 0.6488(11) 0.6271(10) 0.1569(8) 0.061(2) Uani 1 d . . . H24 H 0.7345 0.6793 0.1370 0.073 Uiso 1 calc R . . C25 C 0.5524(10) 0.6850(9) 0.2038(7) 0.055(2) Uani 1 d . . . H25 H 0.5729 0.7777 0.2202 0.066 Uiso 1 calc R . . C26 C 0.4217(9) 0.6013(8) 0.2268(6) 0.0418(16) Uani 1 d . . . C32 C 0.3116(9) 0.6580(7) 0.2790(6) 0.0408(16) Uani 1 d . . . N33 N 0.3493(8) 0.7936(7) 0.3179(6) 0.0489(16) Uani 1 d . . . C34 C 0.2502(10) 0.8389(8) 0.3659(6) 0.0494(19) Uani 1 d . . . C35 C 0.1053(10) 0.7464(8) 0.3691(6) 0.0451(17) Uani 1 d . . . N36 N 0.0757(8) 0.6145(7) 0.3301(5) 0.0477(15) Uani 1 d . . . N31 N 0.1826(7) 0.5686(6) 0.2855(5) 0.0406(13) Uani 1 d . . . C300 C 0.2931(15) 0.9865(9) 0.4227(9) 0.076(3) Uani 1 d . . . H30A H 0.3899 1.0349 0.4078 0.091 Uiso 1 calc R . . H30B H 0.3057 1.0047 0.5044 0.091 Uiso 1 calc R . . H30C H 0.2115 1.0155 0.3927 0.091 Uiso 1 calc R . . C350 C -0.0178(14) 0.7891(11) 0.4164(8) 0.073(3) Uani 1 d . . . H35A H -0.1026 0.7102 0.4137 0.087 Uiso 1 calc R . . H35B H -0.0567 0.8374 0.3711 0.087 Uiso 1 calc R . . H35C H 0.0265 0.8471 0.4949 0.087 Uiso 1 calc R . . O54 O -0.1726(10) -0.0512(8) 0.1998(8) 0.093(3) Uani 1 d . . . O52 O -0.0841(8) 0.1047(6) 0.1220(5) 0.0658(17) Uani 1 d . . . N53 N -0.0758(9) 0.0542(7) 0.2023(7) 0.0596(19) Uani 1 d . . . N63 N -0.0213(9) 0.3263(8) 0.0048(6) 0.060(2) Uani 1 d . . . O64 O -0.0908(10) 0.3181(10) -0.0896(6) 0.101(3) Uani 1 d . . . O62 O -0.0683(8) 0.3604(7) 0.0951(6) 0.0634(16) Uani 1 d . . . O200 O -0.0360(7) 0.3602(6) 0.3349(5) 0.0588(15) Uani 1 d . . . O61 O 0.1031(7) 0.3010(8) 0.0206(5) 0.0670(17) Uani 1 d . . . O51 O 0.0405(7) 0.1232(6) 0.2894(5) 0.0548(14) Uani 1 d . . . N43 N 0.3516(8) 0.6889(7) 0.5767(5) 0.0476(16) Uani 1 d . . . O41 O 0.2925(8) 0.5750(6) 0.5875(5) 0.0629(16) Uani 1 d . . . O42 O 0.4707(8) 0.7143(7) 0.5425(6) 0.0691(17) Uani 1 d . . . O44 O 0.2846(7) 0.7734(6) 0.5995(5) 0.0554(14) Uani 1 d . . . O100 O 0.2973(7) 0.3770(6) 0.4016(4) 0.0486(13) Uani 1 d D . . H1 H 0.387(5) 0.360(8) 0.413(6) 0.04(2) Uiso 1 d D . . H2 H 0.297(11) 0.449(6) 0.459(5) 0.06(3) Uiso 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0351(4) 0.0384(4) 0.0386(4) 0.0127(3) 0.0089(3) 0.0133(3) N11 0.036(3) 0.040(4) 0.045(3) 0.011(3) 0.011(2) 0.013(3) C12 0.050(5) 0.041(5) 0.062(5) 0.016(4) 0.021(4) 0.014(4) C13 0.064(6) 0.047(5) 0.057(5) 0.009(4) 0.023(4) 0.020(4) C14 0.060(6) 0.058(6) 0.053(5) 0.010(4) 0.014(4) 0.034(4) C15 0.040(4) 0.065(6) 0.045(4) 0.007(4) 0.011(3) 0.019(4) C16 0.038(4) 0.049(5) 0.029(3) 0.004(3) 0.004(3) 0.010(3) C22 0.039(4) 0.042(4) 0.036(3) 0.007(3) 0.007(3) 0.012(3) N21 0.045(4) 0.037(3) 0.035(3) 0.011(2) 0.005(2) 0.011(3) C23 0.048(5) 0.067(6) 0.061(5) 0.025(4) 0.020(4) 0.014(4) C24 0.052(5) 0.059(6) 0.064(5) 0.022(4) 0.025(4) 0.004(4) C25 0.053(5) 0.044(5) 0.062(5) 0.020(4) 0.016(4) 0.003(4) C26 0.044(4) 0.039(4) 0.038(4) 0.011(3) 0.008(3) 0.011(3) C32 0.045(4) 0.036(4) 0.037(3) 0.014(3) 0.002(3) 0.011(3) N33 0.052(4) 0.039(4) 0.051(4) 0.013(3) 0.006(3) 0.012(3) C34 0.063(5) 0.042(4) 0.040(4) 0.014(3) 0.000(3) 0.021(4) C35 0.055(5) 0.045(4) 0.041(4) 0.013(3) 0.008(3) 0.026(4) N36 0.053(4) 0.049(4) 0.045(3) 0.015(3) 0.012(3) 0.025(3) N31 0.040(3) 0.042(4) 0.040(3) 0.012(3) 0.010(2) 0.017(3) C300 0.097(8) 0.040(5) 0.078(6) 0.010(4) -0.001(5) 0.024(5) C350 0.101(9) 0.061(6) 0.060(5) 0.010(5) 0.020(5) 0.042(6) O54 0.074(5) 0.056(5) 0.153(8) 0.049(5) 0.037(5) 0.010(4) O52 0.059(4) 0.054(4) 0.069(4) 0.023(3) -0.005(3) 0.006(3) N53 0.053(5) 0.042(4) 0.085(5) 0.022(4) 0.020(4) 0.014(3) N63 0.047(4) 0.062(5) 0.057(4) 0.028(4) -0.006(3) 0.003(3) O64 0.099(6) 0.127(7) 0.064(4) 0.052(5) -0.015(4) 0.020(5) O62 0.059(4) 0.063(4) 0.067(4) 0.021(3) 0.005(3) 0.025(3) O200 0.063(4) 0.055(4) 0.079(4) 0.027(3) 0.045(3) 0.032(3) O61 0.050(4) 0.099(5) 0.052(3) 0.029(3) 0.016(3) 0.022(3) O51 0.057(4) 0.051(3) 0.063(3) 0.023(3) 0.023(3) 0.020(3) N43 0.048(4) 0.052(4) 0.038(3) 0.011(3) 0.011(3) 0.013(3) O41 0.078(5) 0.048(4) 0.070(4) 0.015(3) 0.035(3) 0.026(3) O42 0.061(4) 0.075(5) 0.088(5) 0.040(4) 0.029(3) 0.029(3) O44 0.061(4) 0.050(3) 0.061(3) 0.017(3) 0.020(3) 0.027(3) O100 0.047(3) 0.054(3) 0.043(3) 0.005(2) 0.006(2) 0.025(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 O200 2.296(6) . ? Y1 O100 2.323(6) . ? Y1 O61 2.406(6) . ? Y1 O52 2.433(6) . ? Y1 O62 2.447(6) . ? Y1 O51 2.453(6) . ? Y1 N31 2.495(7) . ? Y1 N11 2.493(7) . ? Y1 N21 2.493(7) . ? Y1 N63 2.859(7) . ? Y1 N53 2.868(8) . ? N11 C12 1.322(10) . ? N11 C16 1.342(9) . ? C12 C13 1.370(12) . ? C13 C14 1.375(13) . ? C14 C15 1.358(12) . ? C15 C16 1.394(11) . ? C16 C22 1.461(11) . ? C22 N21 1.366(10) . ? C22 C23 1.391(11) . ? N21 C26 1.330(10) . ? C23 C24 1.356(14) . ? C24 C25 1.353(14) . ? C25 C26 1.390(11) . ? C26 C32 1.482(11) . ? C32 N31 1.318(10) . ? C32 N33 1.346(10) . ? N33 C34 1.309(11) . ? C34 C35 1.422(12) . ? C34 C300 1.481(12) . ? C35 N36 1.320(10) . ? C35 C350 1.491(13) . ? N36 N31 1.358(9) . ? O54 N53 1.212(10) . ? O52 N53 1.254(9) . ? N53 O51 1.276(9) . ? N63 O64 1.212(9) . ? N63 O61 1.255(10) . ? N63 O62 1.266(10) . ? N43 O42 1.214(9) . ? N43 O44 1.253(9) . ? N43 O41 1.246(9) . ? 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 O200 Y1 O100 80.8(2) . . ? O200 Y1 O61 128.0(2) . . ? O100 Y1 O61 148.0(2) . . ? O200 Y1 O52 84.1(3) . . ? O100 Y1 O52 126.0(2) . . ? O61 Y1 O52 76.1(2) . . ? O200 Y1 O62 76.4(3) . . ? O100 Y1 O62 149.6(2) . . ? O61 Y1 O62 51.9(2) . . ? O52 Y1 O62 71.5(2) . . ? O200 Y1 O51 72.8(2) . . ? O100 Y1 O51 74.1(2) . . ? O61 Y1 O51 123.3(2) . . ? O52 Y1 O51 51.9(2) . . ? O62 Y1 O51 116.9(2) . . ? O200 Y1 N31 71.7(2) . . ? O100 Y1 N31 81.6(2) . . ? O61 Y1 N31 94.2(2) . . ? O52 Y1 N31 140.2(2) . . ? O62 Y1 N31 72.4(2) . . ? O51 Y1 N31 139.4(2) . . ? O200 Y1 N11 150.3(2) . . ? O100 Y1 N11 81.7(2) . . ? O61 Y1 N11 76.4(2) . . ? O52 Y1 N11 86.9(2) . . ? O62 Y1 N11 127.0(2) . . ? O51 Y1 N11 79.4(2) . . ? N31 Y1 N11 128.8(2) . . ? O200 Y1 N21 132.2(2) . . ? O100 Y1 N21 76.5(2) . . ? O61 Y1 N21 73.3(2) . . ? O52 Y1 N21 142.5(2) . . ? O62 Y1 N21 104.6(2) . . ? O51 Y1 N21 136.7(2) . . ? N31 Y1 N21 63.8(2) . . ? N11 Y1 N21 65.3(2) . . ? O200 Y1 N63 102.3(3) . . ? O100 Y1 N63 163.5(2) . . ? O61 Y1 N63 25.8(2) . . ? O52 Y1 N63 70.5(2) . . ? O62 Y1 N63 26.2(2) . . ? O51 Y1 N63 122.4(2) . . ? N31 Y1 N63 84.1(2) . . ? N11 Y1 N63 101.3(2) . . ? N21 Y1 N63 89.9(2) . . ? O200 Y1 N53 75.6(2) . . ? O100 Y1 N53 100.4(2) . . ? O61 Y1 N53 100.3(2) . . ? O52 Y1 N53 25.7(2) . . ? O62 Y1 N53 93.2(2) . . ? O51 Y1 N53 26.3(2) . . ? N31 Y1 N53 146.5(2) . . ? N11 Y1 N53 84.1(2) . . ? N21 Y1 N53 149.4(2) . . ? N63 Y1 N53 96.1(2) . . ? C12 N11 C16 118.2(7) . . ? C12 N11 Y1 121.5(5) . . ? C16 N11 Y1 119.9(5) . . ? N11 C12 C13 124.2(8) . . ? C12 C13 C14 116.7(8) . . ? C15 C14 C13 121.1(8) . . ? C14 C15 C16 118.3(8) . . ? N11 C16 C15 121.3(8) . . ? N11 C16 C22 118.1(7) . . ? C15 C16 C22 120.5(7) . . ? N21 C22 C23 120.0(7) . . ? N21 C22 C16 115.5(6) . . ? C23 C22 C16 124.5(8) . . ? C26 N21 C22 117.7(6) . . ? C26 N21 Y1 121.8(5) . . ? C22 N21 Y1 120.2(5) . . ? C24 C23 C22 120.4(9) . . ? C25 C24 C23 120.1(8) . . ? C24 C25 C26 117.8(8) . . ? N21 C26 C25 123.7(8) . . ? N21 C26 C32 115.6(7) . . ? C25 C26 C32 120.7(7) . . ? N31 C32 N33 124.7(7) . . ? N31 C32 C26 115.9(6) . . ? N33 C32 C26 119.4(7) . . ? C34 N33 C32 117.1(7) . . ? N33 C34 C35 120.3(7) . . ? N33 C34 C300 119.8(9) . . ? C35 C34 C300 119.9(9) . . ? N36 C35 C34 119.5(7) . . ? N36 C35 C350 116.6(8) . . ? C34 C35 C350 123.8(8) . . ? C35 N36 N31 119.7(7) . . ? C32 N31 N36 118.5(7) . . ? C32 N31 Y1 122.3(5) . . ? N36 N31 Y1 119.2(5) . . ? N53 O52 Y1 96.9(5) . . ? O54 N53 O52 123.0(9) . . ? O54 N53 O51 121.6(8) . . ? O52 N53 O51 115.4(7) . . ? O54 N53 Y1 173.2(7) . . ? O52 N53 Y1 57.4(4) . . ? O51 N53 Y1 58.4(4) . . ? O64 N63 O61 122.5(9) . . ? O64 N63 O62 122.8(9) . . ? O61 N63 O62 114.7(6) . . ? O64 N63 Y1 174.8(7) . . ? O61 N63 Y1 56.5(4) . . ? O62 N63 Y1 58.4(4) . . ? N63 O62 Y1 95.4(5) . . ? N63 O61 Y1 97.7(5) . . ? N53 O51 Y1 95.3(4) . . ? O42 N43 O44 121.8(7) . . ? O42 N43 O41 119.3(7) . . ? O44 N43 O41 118.9(7) . . ? _refine_diff_density_max 0.834 _refine_diff_density_min -1.549 _refine_diff_density_rms 0.128 data_8 _database_code_CSD 202734 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 N16 O18 Y2' _chemical_formula_weight 1076.48 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' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.886(16) _cell_length_b 14.401(18) _cell_length_c 13.191(18) _cell_angle_alpha 90.00 _cell_angle_beta 108.511(10) _cell_angle_gamma 90.00 _cell_volume 1961(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cuboid _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 3.045 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.571 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6642 _diffrn_reflns_av_R_equivalents 0.0883 _diffrn_reflns_av_sigmaI/netI 0.0855 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.19 _reflns_number_total 3811 _reflns_number_gt 2483 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0042(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3811 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1259 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.2307 _refine_ls_wR_factor_gt 0.2013 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.17298(6) 0.05068(4) 0.12457(5) 0.0350(3) Uani 1 d . . . N11 N 0.1687(6) 0.2227(4) 0.1103(4) 0.0402(14) Uani 1 d . . . C12 C 0.1057(8) 0.2770(5) 0.1594(6) 0.0462(18) Uani 1 d . . . H12 H 0.0527 0.2478 0.1929 0.055 Uiso 1 calc R . . C13 C 0.1123(8) 0.3722(5) 0.1649(7) 0.051(2) Uani 1 d . . . H13 H 0.0633 0.4064 0.1981 0.061 Uiso 1 calc R . . C14 C 0.1938(9) 0.4141(6) 0.1196(7) 0.058(2) Uani 1 d . . . H14 H 0.2034 0.4783 0.1242 0.070 Uiso 1 calc R . . C15 C 0.2625(8) 0.3638(5) 0.0668(6) 0.0499(19) Uani 1 d . . . H15 H 0.3181 0.3925 0.0356 0.060 Uiso 1 calc R . . C16 C 0.2448(6) 0.2671(5) 0.0624(6) 0.0348(15) Uani 1 d . . . C22 C 0.3054(7) 0.2078(5) -0.0009(5) 0.0386(16) Uani 1 d . . . N21 N 0.2884(6) 0.1175(4) 0.0032(4) 0.0366(13) Uani 1 d . . . C23 C 0.3727(8) 0.2453(5) -0.0655(6) 0.0468(18) Uani 1 d . . . H23 H 0.3840 0.3092 -0.0671 0.056 Uiso 1 calc R . . C24 C 0.4219(8) 0.1891(6) -0.1263(6) 0.052(2) Uani 1 d . . . H24 H 0.4678 0.2141 -0.1685 0.062 Uiso 1 calc R . . C25 C 0.4023(8) 0.0935(5) -0.1243(6) 0.0448(18) Uani 1 d . . . H25 H 0.4343 0.0532 -0.1649 0.054 Uiso 1 calc R . . C26 C 0.3325(7) 0.0605(5) -0.0589(6) 0.0371(16) Uani 1 d . . . C32 C 0.3087(7) -0.0412(5) -0.0522(6) 0.0422(17) Uani 1 d . . . N31 N 0.2489(6) -0.0660(4) 0.0152(5) 0.0405(14) Uani 1 d . . . N33 N 0.3452(6) -0.0951(5) -0.1201(5) 0.0459(16) Uani 1 d . . . C34 C 0.3210(7) -0.1841(6) -0.1145(6) 0.0472(19) Uani 1 d . . . C35 C 0.2646(7) -0.2174(5) -0.0380(6) 0.0460(18) Uani 1 d . . . N36 N 0.2271(6) -0.1578(4) 0.0239(5) 0.0432(15) Uani 1 d . . . O61 O -0.1220(5) 0.0956(4) -0.2037(4) 0.0459(13) Uani 1 d . . . N63 N -0.0305(6) 0.1272(4) -0.1259(4) 0.0392(14) Uani 1 d . . . O62 O 0.0045(5) 0.0724(3) -0.0443(4) 0.0410(12) Uani 1 d . . . O64 O 0.0195(6) 0.2007(4) -0.1284(4) 0.0557(15) Uani 1 d . . . C300 C 0.3562(11) -0.2491(7) -0.1893(8) 0.075(3) Uani 1 d . . . H30A H 0.4130 -0.2181 -0.2210 0.090 Uiso 1 calc R . . H30B H 0.2790 -0.2683 -0.2443 0.090 Uiso 1 calc R . . H30C H 0.3991 -0.3026 -0.1505 0.090 Uiso 1 calc R . . C350 C 0.2389(10) -0.3168(5) -0.0223(8) 0.065(3) Uani 1 d . . . H35A H 0.3193 -0.3483 0.0110 0.078 Uiso 1 calc R . . H35B H 0.1957 -0.3449 -0.0903 0.078 Uiso 1 calc R . . H35C H 0.1849 -0.3215 0.0226 0.078 Uiso 1 calc R . . O51 O 0.1670(6) 0.0839(4) 0.3038(4) 0.0553(14) Uani 1 d . . . N53 N 0.0443(7) 0.0852(4) 0.2803(5) 0.0465(16) Uani 1 d . . . O52 O -0.0155(5) 0.0809(4) 0.1800(4) 0.0457(12) Uani 1 d . . . O54 O -0.0107(7) 0.0896(5) 0.3449(5) 0.0708(19) Uani 1 d . . . O41 O 0.3797(5) 0.1217(4) 0.2360(4) 0.0514(14) Uani 1 d . . . N43 N 0.4295(7) 0.0480(4) 0.2788(5) 0.0467(16) Uani 1 d . . . O42 O 0.3681(5) -0.0257(4) 0.2396(4) 0.0530(14) Uani 1 d . . . O44 O 0.5286(7) 0.0463(5) 0.3525(6) 0.084(2) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0362(5) 0.0354(4) 0.0325(4) -0.0003(3) 0.0098(3) -0.0001(3) N11 0.041(4) 0.038(3) 0.039(3) -0.004(2) 0.009(3) 0.003(3) C12 0.045(5) 0.047(4) 0.050(4) 0.004(3) 0.019(4) 0.004(4) C13 0.060(6) 0.034(4) 0.065(5) -0.006(3) 0.030(4) 0.012(4) C14 0.077(7) 0.039(4) 0.057(5) 0.000(4) 0.019(5) 0.011(4) C15 0.053(5) 0.044(4) 0.054(5) -0.002(4) 0.019(4) -0.013(4) C16 0.023(4) 0.032(3) 0.045(4) 0.004(3) 0.006(3) 0.001(3) C22 0.044(4) 0.032(4) 0.040(4) -0.001(3) 0.014(3) 0.002(3) N21 0.040(4) 0.033(3) 0.037(3) 0.006(2) 0.012(3) 0.003(2) C23 0.044(5) 0.041(4) 0.058(5) 0.010(3) 0.019(4) 0.003(3) C24 0.055(5) 0.058(5) 0.048(4) 0.018(4) 0.025(4) 0.002(4) C25 0.046(5) 0.052(5) 0.038(4) 0.004(3) 0.016(3) 0.010(4) C26 0.028(4) 0.046(4) 0.037(3) 0.003(3) 0.010(3) -0.001(3) C32 0.041(4) 0.050(4) 0.033(3) -0.009(3) 0.008(3) 0.004(3) N31 0.041(4) 0.035(3) 0.044(3) -0.001(2) 0.011(3) 0.006(3) N33 0.034(4) 0.054(4) 0.049(4) -0.014(3) 0.014(3) 0.001(3) C34 0.037(4) 0.051(5) 0.052(4) -0.020(4) 0.013(4) -0.002(3) C35 0.036(4) 0.042(4) 0.056(5) 0.001(3) 0.008(4) 0.004(3) N36 0.050(4) 0.036(3) 0.043(3) -0.003(3) 0.014(3) 0.002(3) O61 0.044(3) 0.046(3) 0.038(3) 0.004(2) 0.000(2) 0.002(2) N63 0.038(4) 0.043(4) 0.034(3) 0.001(3) 0.008(3) -0.001(3) O62 0.047(3) 0.041(3) 0.031(2) 0.005(2) 0.007(2) -0.002(2) O64 0.061(4) 0.046(3) 0.055(3) 0.008(2) 0.011(3) -0.018(3) C300 0.079(7) 0.074(6) 0.081(7) -0.040(5) 0.039(6) -0.010(5) C350 0.083(7) 0.032(4) 0.077(6) -0.008(4) 0.019(5) 0.009(4) O51 0.049(4) 0.069(4) 0.043(3) -0.011(3) 0.008(3) -0.004(3) N53 0.058(5) 0.042(3) 0.044(4) -0.011(3) 0.023(3) -0.005(3) O52 0.043(3) 0.051(3) 0.041(3) -0.007(2) 0.011(2) 0.000(2) O54 0.086(5) 0.078(4) 0.068(4) -0.018(3) 0.052(4) -0.024(4) O41 0.051(4) 0.040(3) 0.054(3) -0.001(2) 0.004(3) -0.002(3) N43 0.042(4) 0.048(4) 0.042(3) -0.003(3) 0.002(3) 0.008(3) O42 0.045(3) 0.043(3) 0.058(3) -0.009(3) -0.002(3) -0.001(3) O44 0.062(5) 0.078(5) 0.079(5) -0.006(3) -0.025(4) 0.005(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 O62 2.414(5) . ? Y1 O52 2.427(6) . ? Y1 O51 2.434(6) . ? Y1 O42 2.445(6) . ? Y1 O41 2.484(6) . ? Y1 N11 2.484(7) . ? Y1 O61 2.491(6) 3 ? Y1 N31 2.519(6) . ? Y1 N21 2.520(6) . ? Y1 O62 2.588(5) 3 ? Y1 N53 2.874(7) . ? Y1 N43 2.887(7) . ? N11 C12 1.336(9) . ? N11 C16 1.351(9) . ? C12 C13 1.373(11) . ? C13 C14 1.358(12) . ? C14 C15 1.379(12) . ? C15 C16 1.405(10) . ? C16 C22 1.487(10) . ? C22 N21 1.317(9) . ? C22 C23 1.397(10) . ? N21 C26 1.351(9) . ? C23 C24 1.363(11) . ? C24 C25 1.394(11) . ? C25 C26 1.401(10) . ? C26 C32 1.496(10) . ? C32 N31 1.307(10) . ? C32 N33 1.337(9) . ? N31 N36 1.355(8) . ? N33 C34 1.315(11) . ? C34 C35 1.420(11) . ? C34 C300 1.495(11) . ? C35 N36 1.335(9) . ? C35 C350 1.486(11) . ? O61 N63 1.266(8) . ? O61 Y1 2.491(6) 3 ? N63 O64 1.196(8) . ? N63 O62 1.291(7) . ? O62 Y1 2.588(5) 3 ? O51 N53 1.271(9) . ? N53 O54 1.188(8) . ? N53 O52 1.278(8) . ? O41 N43 1.243(8) . ? N43 O44 1.202(8) . ? N43 O42 1.273(8) . ? 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 O62 Y1 O52 77.7(2) . . ? O62 Y1 O51 128.6(2) . . ? O52 Y1 O51 52.10(18) . . ? O62 Y1 O42 152.48(19) . . ? O52 Y1 O42 123.0(2) . . ? O51 Y1 O42 76.8(2) . . ? O62 Y1 O41 140.59(17) . . ? O52 Y1 O41 116.2(2) . . ? O51 Y1 O41 69.1(2) . . ? O42 Y1 O41 51.1(2) . . ? O62 Y1 N11 79.04(17) . . ? O52 Y1 N11 81.18(19) . . ? O51 Y1 N11 82.6(2) . . ? O42 Y1 N11 119.17(19) . . ? O41 Y1 N11 68.03(18) . . ? O62 Y1 O61 106.94(17) . 3 ? O52 Y1 O61 72.72(19) . 3 ? O51 Y1 O61 71.4(2) . 3 ? O42 Y1 O61 68.0(2) . 3 ? O41 Y1 O61 112.38(18) . 3 ? N11 Y1 O61 150.93(19) . 3 ? O62 Y1 N31 81.3(2) . . ? O52 Y1 N31 139.03(19) . . ? O51 Y1 N31 143.4(2) . . ? O42 Y1 N31 71.2(2) . . ? O41 Y1 N31 102.3(2) . . ? N11 Y1 N31 128.6(2) . . ? O61 Y1 N31 80.4(2) 3 . ? O62 Y1 N21 75.5(2) . . ? O52 Y1 N21 139.74(19) . . ? O51 Y1 N21 135.6(2) . . ? O42 Y1 N21 93.2(2) . . ? O41 Y1 N21 71.2(2) . . ? N11 Y1 N21 64.65(18) . . ? O61 Y1 N21 144.31(18) 3 . ? N31 Y1 N21 64.5(2) . . ? O62 Y1 O62 57.43(19) . 3 ? O52 Y1 O62 69.72(19) . 3 ? O51 Y1 O62 106.59(18) . 3 ? O42 Y1 O62 109.54(18) . 3 ? O41 Y1 O62 160.48(17) . 3 ? N11 Y1 O62 131.19(18) . 3 ? O61 Y1 O62 49.86(16) 3 3 ? N31 Y1 O62 69.3(2) . 3 ? N21 Y1 O62 117.38(19) . 3 ? O62 Y1 N53 103.7(2) . . ? O52 Y1 N53 26.20(18) . . ? O51 Y1 N53 26.06(18) . . ? O42 Y1 N53 99.1(2) . . ? O41 Y1 N53 93.5(2) . . ? N11 Y1 N53 83.10(19) . . ? O61 Y1 N53 67.83(19) 3 . ? N31 Y1 N53 148.0(2) . . ? N21 Y1 N53 147.44(19) . . ? O62 Y1 N53 86.64(19) 3 . ? O62 Y1 N43 159.0(2) . . ? O52 Y1 N43 120.8(2) . . ? O51 Y1 N43 68.7(2) . . ? O42 Y1 N43 25.98(17) . . ? O41 Y1 N43 25.36(16) . . ? N11 Y1 N43 93.29(18) . . ? O61 Y1 N43 89.32(19) 3 . ? N31 Y1 N43 88.6(2) . . ? N21 Y1 N43 83.5(2) . . ? O62 Y1 N43 135.14(17) 3 . ? N53 Y1 N43 94.6(2) . . ? C12 N11 C16 115.8(6) . . ? C12 N11 Y1 123.2(5) . . ? C16 N11 Y1 120.5(4) . . ? N11 C12 C13 125.7(7) . . ? C14 C13 C12 116.8(7) . . ? C13 C14 C15 121.6(8) . . ? C14 C15 C16 116.9(8) . . ? N11 C16 C15 123.1(7) . . ? N11 C16 C22 116.0(6) . . ? C15 C16 C22 120.8(6) . . ? N21 C22 C23 120.9(7) . . ? N21 C22 C16 116.8(6) . . ? C23 C22 C16 122.3(6) . . ? C22 N21 C26 119.6(6) . . ? C22 N21 Y1 120.5(5) . . ? C26 N21 Y1 119.9(4) . . ? C24 C23 C22 120.7(7) . . ? C23 C24 C25 118.9(7) . . ? C24 C25 C26 117.6(7) . . ? N21 C26 C25 122.2(7) . . ? N21 C26 C32 117.3(6) . . ? C25 C26 C32 120.4(7) . . ? N31 C32 N33 128.0(7) . . ? N31 C32 C26 116.1(6) . . ? N33 C32 C26 115.8(7) . . ? C32 N31 N36 117.5(6) . . ? C32 N31 Y1 122.2(5) . . ? N36 N31 Y1 120.3(4) . . ? C34 N33 C32 114.8(7) . . ? N33 C34 C35 120.6(7) . . ? N33 C34 C300 118.3(8) . . ? C35 C34 C300 121.1(8) . . ? N36 C35 C34 120.1(7) . . ? N36 C35 C350 115.2(7) . . ? C34 C35 C350 124.6(7) . . ? C35 N36 N31 118.7(6) . . ? N63 O61 Y1 100.8(4) . 3 ? O64 N63 O61 122.9(6) . . ? O64 N63 O62 123.2(6) . . ? O61 N63 O62 113.9(6) . . ? N63 O62 Y1 141.8(4) . . ? N63 O62 Y1 95.3(4) . 3 ? Y1 O62 Y1 122.57(19) . 3 ? N53 O51 Y1 96.7(4) . . ? O54 N53 O51 123.7(7) . . ? O54 N53 O52 122.5(8) . . ? O51 N53 O52 113.8(6) . . ? O54 N53 Y1 173.1(5) . . ? O51 N53 Y1 57.3(3) . . ? O52 N53 Y1 57.0(4) . . ? N53 O52 Y1 96.8(4) . . ? N43 O41 Y1 95.8(4) . . ? O44 N43 O41 122.4(7) . . ? O44 N43 O42 122.1(7) . . ? O41 N43 O42 115.5(6) . . ? O44 N43 Y1 171.7(7) . . ? O41 N43 Y1 58.9(4) . . ? O42 N43 Y1 57.2(4) . . ? N43 O42 Y1 96.8(4) . . ? _refine_diff_density_max 1.861 _refine_diff_density_min -1.513 _refine_diff_density_rms 0.152 #===END data_1 _database_code_CSD 206177 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H115 N27 O20.50 Y2' _chemical_formula_weight 1972.82 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 34.86(4) _cell_length_b 14.790(17) _cell_length_c 40.64(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.108(10) _cell_angle_gamma 90.00 _cell_volume 20789(41) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17907 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 26.22 _exptl_crystal_description parallelopiped _exptl_crystal_colour white _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8256 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.346 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 10 min.' _diffrn_standards_number n/a _diffrn_standards_decay_% none _diffrn_reflns_number 55610 _diffrn_reflns_av_R_equivalents 0.2170 _diffrn_reflns_av_sigmaI/netI 0.3179 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.22 _reflns_number_total 17907 _reflns_number_gt 5119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00027(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 17907 _refine_ls_number_parameters 1173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2879 _refine_ls_R_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.2678 _refine_ls_wR_factor_gt 0.2028 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.841 _refine_ls_shift/su_max 0.075 _refine_ls_shift/su_mean 0.005 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.38644(3) 0.72700(5) 0.11274(2) 0.0698(3) Uani 1 d . . . N11 N 0.4335(2) 0.6040(5) 0.1323(2) 0.069(2) Uani 1 d . . . N12 N 0.4278(2) 0.5448(5) 0.1550(2) 0.076(2) Uani 1 d . . . C13 C 0.4539(4) 0.4826(6) 0.1643(3) 0.082(3) Uani 1 d . . . C14 C 0.4900(3) 0.4852(6) 0.1549(3) 0.074(3) Uani 1 d . . . N15 N 0.4956(2) 0.5435(5) 0.1298(2) 0.083(2) Uani 1 d . . . C16 C 0.4689(3) 0.6021(6) 0.1205(2) 0.064(2) Uani 1 d . . . C22 C 0.4737(4) 0.6598(7) 0.0927(3) 0.090(3) Uani 1 d . . . N21 N 0.4445(2) 0.7189(5) 0.0837(2) 0.073(2) Uani 1 d . . . C26 C 0.4474(3) 0.7731(7) 0.0572(3) 0.084(3) Uani 1 d . . . C25 C 0.4798(4) 0.7707(6) 0.0410(3) 0.092(3) Uani 1 d . . . H25 H 0.4819 0.8092 0.0232 0.110 Uiso 1 calc R . . C24 C 0.5079(3) 0.7138(7) 0.0509(3) 0.096(3) Uani 1 d . . . H24 H 0.5289 0.7099 0.0390 0.115 Uiso 1 calc R . . C23 C 0.5070(4) 0.6591(7) 0.0787(3) 0.105(4) Uani 1 d . . . H23 H 0.5281 0.6241 0.0872 0.126 Uiso 1 calc R . . N31 N 0.3866(2) 0.8349(4) 0.06698(19) 0.065(2) Uani 1 d . . . C32 C 0.4163(3) 0.8375(6) 0.0481(3) 0.086(3) Uani 1 d . . . N33 N 0.4195(3) 0.8959(6) 0.0230(2) 0.097(3) Uani 1 d . . . C35 C 0.3618(3) 0.9570(6) 0.0375(3) 0.066(3) Uani 1 d . . . C34 C 0.3909(4) 0.9553(7) 0.0172(3) 0.090(3) Uani 1 d . . . N36 N 0.3596(2) 0.9017(5) 0.0608(2) 0.078(2) Uani 1 d . . . C17 C 0.4441(3) 0.4112(7) 0.1875(3) 0.096(3) Uani 1 d . . . C18 C 0.4751(5) 0.3438(11) 0.1981(5) 0.175(8) Uani 1 d . . . H18A H 0.4751 0.3332 0.2217 0.210 Uiso 1 calc R . . H18B H 0.4679 0.2873 0.1869 0.210 Uiso 1 calc R . . C19 C 0.5077(5) 0.3615(11) 0.1935(4) 0.152(7) Uani 1 d . . . H19A H 0.5196 0.3034 0.1902 0.182 Uiso 1 calc R . . H19B H 0.5200 0.3837 0.2146 0.182 Uiso 1 calc R . . C20 C 0.5223(4) 0.4247(8) 0.1673(3) 0.111(4) Uani 1 d . . . C171 C 0.4090(4) 0.3566(8) 0.1701(3) 0.142(5) Uani 1 d . . . H17A H 0.3993 0.3857 0.1496 0.170 Uiso 1 calc R . . H17B H 0.3890 0.3541 0.1843 0.170 Uiso 1 calc R . . H17C H 0.4172 0.2963 0.1656 0.170 Uiso 1 calc R . . C172 C 0.4295(3) 0.4524(7) 0.2176(3) 0.119(4) Uani 1 d . . . H17D H 0.4501 0.4848 0.2303 0.143 Uiso 1 calc R . . H17E H 0.4204 0.4053 0.2310 0.143 Uiso 1 calc R . . H17F H 0.4086 0.4932 0.2106 0.143 Uiso 1 calc R . . C201 C 0.5563(3) 0.4770(8) 0.1829(3) 0.132(5) Uani 1 d . . . H20A H 0.5705 0.4998 0.1660 0.159 Uiso 1 calc R . . H20B H 0.5726 0.4382 0.1975 0.159 Uiso 1 calc R . . H20C H 0.5476 0.5266 0.1953 0.159 Uiso 1 calc R . . C202 C 0.5355(4) 0.3760(9) 0.1378(4) 0.183(7) Uani 1 d . . . H20D H 0.5167 0.3315 0.1297 0.219 Uiso 1 calc R . . H20E H 0.5599 0.3470 0.1444 0.219 Uiso 1 calc R . . H20F H 0.5384 0.4190 0.1205 0.219 Uiso 1 calc R . . C37 C 0.3899(5) 1.0149(11) -0.0117(4) 0.143(6) Uani 1 d . . . C38 C 0.3699(5) 1.0971(11) -0.0065(5) 0.178(7) Uani 1 d . . . H38A H 0.3840 1.1300 0.0118 0.213 Uiso 1 calc R . . H38B H 0.3689 1.1345 -0.0262 0.213 Uiso 1 calc R . . C39 C 0.3316(5) 1.0803(9) 0.0007(4) 0.142(5) Uani 1 d . . . H39A H 0.3174 1.0484 -0.0178 0.170 Uiso 1 calc R . . H39B H 0.3187 1.1374 0.0033 0.170 Uiso 1 calc R . . C40 C 0.3315(4) 1.0254(9) 0.0316(4) 0.117(4) Uani 1 d . . . C371 C 0.4321(4) 1.0583(8) -0.0092(3) 0.133(5) Uani 1 d . . . H37A H 0.4506 1.0120 -0.0123 0.160 Uiso 1 calc R . . H37B H 0.4385 1.0855 0.0122 0.160 Uiso 1 calc R . . H37C H 0.4326 1.1036 -0.0261 0.160 Uiso 1 calc R . . C372 C 0.3847(5) 0.9663(11) -0.0417(4) 0.209(9) Uani 1 d . . . H37D H 0.4023 0.9162 -0.0404 0.251 Uiso 1 calc R . . H37E H 0.3896 1.0053 -0.0596 0.251 Uiso 1 calc R . . H37F H 0.3586 0.9443 -0.0456 0.251 Uiso 1 calc R . . C401 C 0.3316(4) 1.0821(8) 0.0623(4) 0.150(5) Uani 1 d . . . H40A H 0.3105 1.1241 0.0593 0.179 Uiso 1 calc R . . H40B H 0.3555 1.1148 0.0662 0.179 Uiso 1 calc R . . H40C H 0.3289 1.0437 0.0809 0.179 Uiso 1 calc R . . C402 C 0.2923(4) 0.9780(9) 0.0267(4) 0.173(7) Uani 1 d . . . H40D H 0.2943 0.9234 0.0143 0.208 Uiso 1 calc R . . H40E H 0.2735 1.0172 0.0149 0.208 Uiso 1 calc R . . H40F H 0.2846 0.9635 0.0480 0.208 Uiso 1 calc R . . N41 N 0.3474(3) 0.6182(5) 0.1408(2) 0.086(3) Uani 1 d . . . N42 N 0.3227(3) 0.5569(6) 0.1249(2) 0.093(3) Uani 1 d . . . C43 C 0.3075(3) 0.4953(7) 0.1398(4) 0.096(4) Uani 1 d . . . C44 C 0.3093(4) 0.5017(8) 0.1733(4) 0.107(4) Uani 1 d . . . N45 N 0.3303(3) 0.5605(6) 0.1921(2) 0.081(2) Uani 1 d . . . C46 C 0.3489(3) 0.6147(7) 0.1723(4) 0.094(3) Uani 1 d . . . N51 N 0.39863(19) 0.7309(4) 0.17369(17) 0.0628(18) Uani 1 d . . . C53 C 0.3831(3) 0.6766(7) 0.2266(3) 0.098(3) Uani 1 d . . . H53 H 0.3681 0.6406 0.2388 0.117 Uiso 1 calc R . . C52 C 0.3772(3) 0.6755(6) 0.1935(3) 0.075(3) Uani 1 d . . . C55 C 0.4320(3) 0.7900(6) 0.2253(3) 0.081(3) Uani 1 d . . . H55 H 0.4504 0.8285 0.2363 0.098 Uiso 1 calc R . . C54 C 0.4108(3) 0.7303(7) 0.2424(3) 0.102(4) Uani 1 d . . . H54 H 0.4158 0.7273 0.2654 0.123 Uiso 1 calc R . . C56 C 0.4240(3) 0.7887(5) 0.1906(3) 0.068(3) Uani 1 d . . . N61 N 0.4337(3) 0.8458(5) 0.1368(3) 0.089(3) Uani 1 d . . . C62 C 0.4437(3) 0.8488(6) 0.1702(3) 0.079(3) Uani 1 d . . . N63 N 0.4697(2) 0.9079(5) 0.18591(19) 0.071(2) Uani 1 d . . . C64 C 0.4840(3) 0.9674(6) 0.1686(3) 0.079(3) Uani 1 d . . . C65 C 0.4725(3) 0.9709(5) 0.1336(3) 0.067(3) Uani 1 d . . . N66 N 0.4480(2) 0.9070(5) 0.1190(2) 0.073(2) Uani 1 d . . . C47 C 0.2811(4) 0.4235(8) 0.1166(4) 0.118(4) Uani 1 d . . . C48 C 0.2585(5) 0.3718(11) 0.1391(5) 0.162(7) Uani 1 d . . . H48A H 0.2327 0.3977 0.1363 0.195 Uiso 1 calc R . . H48B H 0.2559 0.3109 0.1301 0.195 Uiso 1 calc R . . C49 C 0.2683(6) 0.3629(11) 0.1710(5) 0.179(7) Uani 1 d . . . H49A H 0.2864 0.3128 0.1737 0.214 Uiso 1 calc R . . H49B H 0.2452 0.3429 0.1799 0.214 Uiso 1 calc R . . C50 C 0.2853(5) 0.4350(11) 0.1934(4) 0.143(6) Uani 1 d . . . C471 C 0.3120(4) 0.3661(9) 0.1013(4) 0.152(6) Uani 1 d . . . H47A H 0.3322 0.3491 0.1184 0.183 Uiso 1 calc R . . H47B H 0.3227 0.4012 0.0848 0.183 Uiso 1 calc R . . H47C H 0.3000 0.3127 0.0912 0.183 Uiso 1 calc R . . C472 C 0.2536(4) 0.4674(9) 0.0907(4) 0.170(6) Uani 1 d . . . H47D H 0.2386 0.4219 0.0781 0.205 Uiso 1 calc R . . H47E H 0.2677 0.5022 0.0763 0.205 Uiso 1 calc R . . H47F H 0.2366 0.5065 0.1011 0.205 Uiso 1 calc R . . C501 C 0.3123(5) 0.3960(9) 0.2217(4) 0.172(7) Uani 1 d . . . H50A H 0.3309 0.4409 0.2300 0.206 Uiso 1 calc R . . H50B H 0.3253 0.3444 0.2141 0.206 Uiso 1 calc R . . H50C H 0.2977 0.3779 0.2392 0.206 Uiso 1 calc R . . C502 C 0.2563(5) 0.4847(11) 0.2081(5) 0.193(8) Uani 1 d . . . H50D H 0.2401 0.5165 0.1911 0.232 Uiso 1 calc R . . H50E H 0.2687 0.5273 0.2239 0.232 Uiso 1 calc R . . H50F H 0.2409 0.4436 0.2192 0.232 Uiso 1 calc R . . C67 C 0.5158(3) 1.0269(6) 0.1852(3) 0.081(3) Uani 1 d . . . C68 C 0.5376(3) 1.0710(7) 0.1575(3) 0.109(4) Uani 1 d . . . H68A H 0.5541 1.1194 0.1671 0.130 Uiso 1 calc R . . H68B H 0.5539 1.0259 0.1488 0.130 Uiso 1 calc R . . C69 C 0.5086(4) 1.1099(9) 0.1284(4) 0.159(6) Uani 1 d . . . H69A H 0.4912 1.1517 0.1375 0.191 Uiso 1 calc R . . H69B H 0.5230 1.1437 0.1136 0.191 Uiso 1 calc R . . C70 C 0.4853(3) 1.0402(7) 0.1091(3) 0.098(3) Uani 1 d . . . C671 C 0.5430(3) 0.9780(6) 0.2083(3) 0.100(4) Uani 1 d . . . H67A H 0.5617 1.0194 0.2192 0.120 Uiso 1 calc R . . H67B H 0.5560 0.9334 0.1966 0.120 Uiso 1 calc R . . H67C H 0.5295 0.9487 0.2245 0.120 Uiso 1 calc R . . C672 C 0.4942(3) 1.0955(6) 0.2040(3) 0.102(4) Uani 1 d . . . H67D H 0.4777 1.0642 0.2174 0.122 Uiso 1 calc R . . H67E H 0.4789 1.1338 0.1885 0.122 Uiso 1 calc R . . H67F H 0.5125 1.1316 0.2179 0.122 Uiso 1 calc R . . C701 C 0.4489(3) 1.0827(7) 0.0914(3) 0.115(4) Uani 1 d . . . H70A H 0.4324 1.1012 0.1074 0.138 Uiso 1 calc R . . H70B H 0.4356 1.0394 0.0765 0.138 Uiso 1 calc R . . H70C H 0.4556 1.1345 0.0791 0.138 Uiso 1 calc R . . C702 C 0.5083(4) 0.9870(9) 0.0844(3) 0.146(5) Uani 1 d . . . H70D H 0.5267 1.0266 0.0762 0.175 Uiso 1 calc R . . H70E H 0.4906 0.9648 0.0662 0.175 Uiso 1 calc R . . H70F H 0.5216 0.9371 0.0958 0.175 Uiso 1 calc R . . N71 N 0.3743(2) 0.6107(4) 0.06828(18) 0.069(2) Uani 1 d . . . N72 N 0.3999(2) 0.5484(5) 0.0634(2) 0.075(2) Uani 1 d . . . C73 C 0.3933(3) 0.4894(6) 0.0389(3) 0.080(3) Uani 1 d . . . C74 C 0.3569(3) 0.4877(6) 0.0197(3) 0.080(3) Uani 1 d . . . N75 N 0.3294(2) 0.5471(5) 0.0246(2) 0.084(2) Uani 1 d . . . C76 C 0.3380(3) 0.6106(7) 0.0483(3) 0.082(3) Uani 1 d . . . C82 C 0.3076(3) 0.6748(6) 0.0566(3) 0.083(3) Uani 1 d . . . C83 C 0.2709(4) 0.6736(7) 0.0400(3) 0.103(4) Uani 1 d . . . H83 H 0.2646 0.6338 0.0225 0.124 Uiso 1 calc R . . C84 C 0.2437(4) 0.7314(8) 0.0495(3) 0.108(4) Uani 1 d . . . H84 H 0.2183 0.7300 0.0393 0.129 Uiso 1 calc R . . C85 C 0.2547(3) 0.7896(6) 0.0738(3) 0.084(3) Uani 1 d . . . H85 H 0.2374 0.8319 0.0803 0.101 Uiso 1 calc R . . C86 C 0.2951(4) 0.7858(7) 0.0903(3) 0.098(3) Uani 1 d . . . N92 N 0.3059(4) 0.8479(6) 0.1195(2) 0.114(3) Uani 1 d . . . C93 C 0.2793(3) 0.9104(6) 0.1262(3) 0.070(3) Uani 1 d . . . C94 C 0.2912(3) 0.9623(7) 0.1505(3) 0.093(3) Uani 1 d . . . C95 C 0.3309(4) 0.9638(7) 0.1655(3) 0.104(4) Uani 1 d . . . C97 C 0.2625(5) 1.0242(10) 0.1611(4) 0.151(6) Uani 1 d . . . C98 C 0.2820(5) 1.0812(11) 0.1905(5) 0.170(7) Uani 1 d . . . H98A H 0.2671 1.1365 0.1908 0.204 Uiso 1 calc R . . H98B H 0.2783 1.0484 0.2105 0.204 Uiso 1 calc R . . C99 C 0.3171(5) 1.1044(11) 0.1934(5) 0.192(9) Uani 1 d . . . H99A H 0.3231 1.1358 0.2144 0.230 Uiso 1 calc R . . H99B H 0.3206 1.1471 0.1759 0.230 Uiso 1 calc R . . C100 C 0.3467(4) 1.0270(9) 0.1921(4) 0.120(4) Uiso 1 d . . . C102 C 0.3763(5) 1.0757(10) 0.1791(4) 0.189(7) Uiso 1 d . . . H10A H 0.4002 1.0431 0.1834 0.227 Uiso 1 calc R . . H10B H 0.3791 1.1340 0.1895 0.227 Uiso 1 calc R . . H10C H 0.3696 1.0833 0.1556 0.227 Uiso 1 calc R . . C971 C 0.2295(4) 0.9707(9) 0.1708(4) 0.168(6) Uiso 1 d . . . H97A H 0.2308 0.9100 0.1626 0.201 Uiso 1 calc R . . H97B H 0.2056 0.9980 0.1615 0.201 Uiso 1 calc R . . H97C H 0.2308 0.9695 0.1945 0.201 Uiso 1 calc R . . C972 C 0.2514(5) 1.0888(11) 0.1335(5) 0.214(8) Uiso 1 d . . . H97D H 0.2741 1.1079 0.1243 0.256 Uiso 1 calc R . . H97E H 0.2389 1.1405 0.1417 0.256 Uiso 1 calc R . . H97F H 0.2340 1.0597 0.1166 0.256 Uiso 1 calc R . . C101 C 0.3590(5) 0.9836(10) 0.2229(4) 0.190(7) Uiso 1 d . . . H10D H 0.3867 0.9862 0.2273 0.228 Uiso 1 calc R . . H10E H 0.3508 0.9216 0.2218 0.228 Uiso 1 calc R . . H10F H 0.3478 1.0138 0.2403 0.228 Uiso 1 calc R . . N81 N 0.3217(2) 0.7307(5) 0.0830(2) 0.076(2) Uani 1 d . . . C77 C 0.4221(4) 0.4211(8) 0.0353(3) 0.099(4) Uani 1 d . . . C78 C 0.4067(4) 0.3458(7) 0.0130(3) 0.116(4) Uani 1 d . . . H78A H 0.4281 0.3088 0.0077 0.139 Uiso 1 calc R . . H78B H 0.3900 0.3081 0.0247 0.139 Uiso 1 calc R . . C79 C 0.3861(5) 0.3760(9) -0.0162(4) 0.159(7) Uani 1 d . . . H79A H 0.3806 0.3254 -0.0312 0.191 Uiso 1 calc R . . H79B H 0.4016 0.4193 -0.0267 0.191 Uiso 1 calc R . . C80 C 0.3478(4) 0.4207(8) -0.0098(3) 0.101(4) Uani 1 d . . . C771 C 0.4554(4) 0.4625(9) 0.0228(4) 0.164(6) Uani 1 d . . . H77A H 0.4477 0.5185 0.0120 0.196 Uiso 1 calc R . . H77B H 0.4652 0.4224 0.0072 0.196 Uiso 1 calc R . . H77C H 0.4752 0.4738 0.0409 0.196 Uiso 1 calc R . . C772 C 0.4398(4) 0.3855(8) 0.0695(4) 0.149(6) Uani 1 d . . . H77D H 0.4635 0.3543 0.0672 0.179 Uiso 1 calc R . . H77E H 0.4220 0.3447 0.0780 0.179 Uiso 1 calc R . . H77F H 0.4450 0.4353 0.0845 0.179 Uiso 1 calc R . . C801 C 0.3139(4) 0.3664(7) 0.0025(3) 0.142(5) Uani 1 d . . . H80A H 0.2905 0.3780 -0.0119 0.171 Uiso 1 calc R . . H80B H 0.3107 0.3850 0.0247 0.171 Uiso 1 calc R . . H80C H 0.3197 0.3030 0.0024 0.171 Uiso 1 calc R . . C802 C 0.3284(4) 0.4776(7) -0.0406(3) 0.134(5) Uani 1 d . . . H80D H 0.3163 0.4371 -0.0572 0.161 Uiso 1 calc R . . H80E H 0.3478 0.5125 -0.0496 0.161 Uiso 1 calc R . . H80F H 0.3092 0.5173 -0.0335 0.161 Uiso 1 calc R . . N91 N 0.3432(2) 0.8465(4) 0.13192(19) 0.066(2) Uani 1 d . . . N96 N 0.3546(3) 0.9042(5) 0.1557(2) 0.085(3) Uani 1 d . . . Y2 Y 0.63046(3) 0.74821(6) 0.14710(3) 0.0956(4) Uani 1 d . . . N103 N 0.6730(8) 0.7046(15) 0.2061(6) 0.229(11) Uani 1 d . . . O102 O 0.6907(3) 0.7296(7) 0.1833(3) 0.133(3) Uani 1 d . . . O101 O 0.6424(4) 0.6638(8) 0.1994(4) 0.173(5) Uani 1 d . . . O104 O 0.6977(4) 0.6771(11) 0.2312(4) 0.238(7) Uani 1 d . . . N113 N 0.6405(5) 0.9137(12) 0.1732(5) 0.182(9) Uani 1 d . . . O114 O 0.6460(3) 0.9945(8) 0.1866(3) 0.199(5) Uani 1 d . . . O112 O 0.6252(3) 0.8569(7) 0.1904(3) 0.154(4) Uani 1 d . . . O111 O 0.6511(4) 0.9030(8) 0.1478(3) 0.166(5) Uani 1 d . . . N123 N 0.5506(5) 0.7645(9) 0.1497(4) 0.139(5) Uani 1 d . . . O121 O 0.5705(3) 0.7126(6) 0.1685(2) 0.130(3) Uani 1 d . . . O122 O 0.5662(3) 0.8140(6) 0.1312(3) 0.145(4) Uani 1 d . . . O124 O 0.5140(3) 0.7712(7) 0.1498(3) 0.187(5) Uani 1 d . . . N133 N 0.6144(5) 0.5817(10) 0.1169(5) 0.168(7) Uani 1 d . . . O134 O 0.6085(3) 0.5066(8) 0.1018(3) 0.203(5) Uani 1 d . . . O131 O 0.5990(3) 0.6496(7) 0.1051(3) 0.162(4) Uani 1 d . . . O132 O 0.6390(3) 0.5857(7) 0.1402(3) 0.148(4) Uani 1 d . . . N143 N 0.6680(4) 0.7788(8) 0.0905(4) 0.123(4) Uani 1 d . . . O141 O 0.6825(2) 0.7355(5) 0.1138(2) 0.121(3) Uani 1 d . . . O142 O 0.6352(3) 0.8048(6) 0.0900(2) 0.149(4) Uani 1 d . . . O144 O 0.6875(3) 0.7885(7) 0.0667(3) 0.157(4) Uani 1 d . . . N163 N 0.3593(5) 0.7310(9) -0.0149(4) 0.138(5) Uani 1 d . . . O162 O 0.3399(3) 0.7765(7) -0.0011(3) 0.151(4) Uani 1 d . . . O164 O 0.3881(3) 0.6863(7) -0.0051(3) 0.161(4) Uani 1 d . . . O161 O 0.3481(4) 0.7157(7) -0.0447(4) 0.191(5) Uani 1 d . . . O100 O 0.4730(5) 0.7518(10) -0.0482(5) 0.152(6) Uiso 0.50 d P . . O200 O 0.2296(5) 0.6782(10) 0.1447(4) 0.141(6) Uiso 0.50 d P . . O300 O 0.6038(4) 0.2301(8) 0.2320(4) 0.109(4) Uiso 0.50 d P . . O400 O 0.7110(5) 0.7714(10) 0.3032(5) 0.157(6) Uiso 0.50 d P . . O500 O 0.6397(6) 1.2303(12) 0.2058(6) 0.186(8) Uiso 0.50 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0733(7) 0.0656(5) 0.0694(7) -0.0001(4) 0.0043(5) 0.0001(4) N11 0.052(6) 0.080(5) 0.075(6) 0.001(4) 0.010(5) 0.001(4) N12 0.069(6) 0.081(5) 0.082(6) 0.008(4) 0.019(5) -0.003(4) C13 0.092(10) 0.073(7) 0.079(8) 0.003(5) 0.005(7) -0.011(6) C14 0.070(9) 0.075(6) 0.078(8) 0.007(5) 0.012(6) -0.009(5) N15 0.068(7) 0.093(6) 0.090(7) 0.003(5) 0.014(5) -0.004(5) C16 0.057(8) 0.068(6) 0.066(7) -0.003(5) 0.006(6) 0.001(5) C22 0.094(10) 0.085(7) 0.088(9) 0.003(6) 0.007(8) -0.009(7) N21 0.083(6) 0.070(4) 0.069(6) 0.003(4) 0.013(5) -0.002(4) C26 0.081(9) 0.093(7) 0.081(8) -0.008(6) 0.026(7) -0.006(7) C25 0.093(9) 0.072(6) 0.109(9) 0.008(6) 0.011(8) -0.006(6) C24 0.096(10) 0.106(8) 0.090(9) -0.006(7) 0.029(7) -0.009(7) C23 0.102(11) 0.105(8) 0.106(11) 0.013(7) 0.009(9) -0.010(7) N31 0.059(6) 0.067(4) 0.068(6) 0.011(4) 0.003(5) 0.017(4) C32 0.077(9) 0.080(7) 0.100(10) -0.008(6) 0.000(7) 0.003(6) N33 0.104(8) 0.094(6) 0.092(8) 0.013(5) 0.013(6) 0.000(5) C35 0.069(8) 0.067(6) 0.064(8) 0.002(5) 0.014(6) 0.003(5) C34 0.123(11) 0.082(7) 0.064(8) 0.021(6) 0.005(8) -0.003(7) N36 0.065(6) 0.095(5) 0.073(6) 0.012(5) 0.005(5) -0.009(4) C17 0.099(10) 0.099(8) 0.093(9) 0.004(7) 0.020(8) 0.013(7) C18 0.155(17) 0.156(14) 0.22(2) 0.070(12) 0.047(17) 0.038(13) C19 0.111(14) 0.176(14) 0.163(16) 0.057(12) -0.003(13) -0.016(12) C20 0.121(12) 0.102(8) 0.105(11) 0.011(7) -0.009(9) 0.007(8) C171 0.187(15) 0.131(10) 0.112(11) 0.013(8) 0.033(11) -0.034(9) C172 0.129(12) 0.121(9) 0.110(11) 0.010(7) 0.020(9) 0.012(7) C201 0.114(11) 0.156(11) 0.122(12) 0.010(8) -0.006(9) -0.023(9) C202 0.174(17) 0.157(13) 0.21(2) -0.011(12) -0.020(15) 0.049(11) C37 0.148(16) 0.125(12) 0.150(16) 0.025(10) -0.005(12) -0.008(10) C38 0.158(18) 0.160(15) 0.22(2) 0.066(13) 0.052(15) 0.011(13) C39 0.118(14) 0.145(12) 0.163(16) 0.033(10) 0.021(11) 0.014(9) C40 0.125(13) 0.118(10) 0.106(12) 0.003(8) 0.007(9) -0.003(9) C371 0.140(13) 0.137(10) 0.124(12) 0.014(8) 0.024(10) 0.018(9) C372 0.25(2) 0.233(19) 0.142(17) 0.005(15) 0.008(16) -0.081(16) C401 0.149(14) 0.137(11) 0.162(16) 0.023(10) 0.018(12) 0.012(9) C402 0.112(13) 0.171(13) 0.23(2) 0.049(12) 0.013(13) 0.010(10) N41 0.093(7) 0.091(5) 0.071(7) 0.010(5) 0.001(6) -0.011(5) N42 0.099(7) 0.086(6) 0.091(7) -0.005(5) 0.000(6) -0.008(5) C43 0.099(10) 0.084(8) 0.106(11) 0.002(7) 0.019(8) -0.016(6) C44 0.119(11) 0.105(9) 0.099(11) 0.017(8) 0.023(9) -0.007(7) N45 0.074(6) 0.087(5) 0.080(7) -0.005(5) 0.001(5) 0.003(4) C46 0.093(10) 0.096(8) 0.095(11) 0.005(7) 0.014(8) -0.004(6) N51 0.048(4) 0.073(4) 0.070(5) 0.001(4) 0.016(4) -0.011(4) C53 0.113(11) 0.101(8) 0.083(10) -0.003(6) 0.027(8) -0.010(6) C52 0.076(8) 0.077(6) 0.071(8) -0.003(5) 0.006(6) 0.007(5) C55 0.074(8) 0.071(6) 0.097(10) -0.003(5) 0.005(7) -0.014(5) C54 0.116(10) 0.100(7) 0.088(9) -0.015(7) -0.002(8) 0.001(7) C56 0.076(7) 0.062(5) 0.064(7) 0.003(5) 0.004(6) -0.005(5) N61 0.105(8) 0.075(5) 0.083(7) -0.010(5) 0.000(6) 0.004(5) C62 0.070(8) 0.076(6) 0.095(10) 0.001(6) 0.016(7) 0.002(5) N63 0.074(6) 0.071(5) 0.069(6) 0.001(4) 0.008(5) -0.007(4) C64 0.085(8) 0.070(6) 0.080(9) -0.002(5) 0.001(7) 0.003(5) C65 0.055(7) 0.064(5) 0.082(8) -0.003(5) 0.010(6) -0.006(4) N66 0.053(6) 0.086(5) 0.082(6) 0.011(5) 0.015(5) 0.003(4) C47 0.110(11) 0.102(9) 0.139(13) 0.008(8) -0.002(10) -0.021(8) C48 0.157(16) 0.160(13) 0.165(18) 0.003(13) -0.001(15) -0.048(11) C49 0.184(19) 0.164(14) 0.19(2) -0.016(16) 0.018(17) -0.064(12) C50 0.148(16) 0.143(13) 0.136(15) -0.002(11) 0.014(13) 0.020(11) C471 0.145(14) 0.138(11) 0.173(16) -0.022(10) 0.021(12) -0.022(10) C472 0.151(15) 0.170(13) 0.182(18) 0.016(12) -0.011(13) -0.010(11) C501 0.174(17) 0.158(13) 0.192(18) 0.044(12) 0.056(14) -0.026(11) C502 0.162(18) 0.183(16) 0.24(2) 0.022(14) 0.037(16) -0.034(13) C67 0.090(9) 0.074(6) 0.081(8) -0.018(5) 0.014(7) 0.000(6) C68 0.092(10) 0.122(8) 0.113(11) -0.001(7) 0.020(9) -0.003(7) C69 0.173(16) 0.161(12) 0.137(14) 0.018(10) -0.008(12) -0.042(11) C70 0.089(10) 0.105(8) 0.100(10) -0.002(7) 0.014(8) -0.001(7) C671 0.081(9) 0.096(7) 0.119(10) 0.005(6) -0.008(7) -0.002(6) C672 0.079(9) 0.112(8) 0.111(10) 0.000(7) 0.003(7) -0.014(6) C701 0.125(11) 0.105(8) 0.114(11) 0.020(7) 0.011(9) 0.006(7) C702 0.124(13) 0.165(12) 0.152(14) 0.001(10) 0.029(11) -0.030(9) N71 0.075(6) 0.061(4) 0.072(6) -0.009(3) 0.016(5) -0.004(4) N72 0.080(6) 0.071(5) 0.074(6) -0.004(4) 0.008(5) 0.000(4) C73 0.068(8) 0.079(7) 0.093(9) -0.011(6) 0.009(6) 0.003(5) C74 0.061(8) 0.082(6) 0.098(9) -0.018(5) 0.011(7) -0.006(5) N75 0.086(7) 0.093(5) 0.073(6) -0.014(4) 0.004(5) -0.001(5) C76 0.060(8) 0.104(7) 0.082(9) 0.006(6) 0.009(6) -0.006(6) C82 0.085(9) 0.082(7) 0.083(9) 0.007(6) 0.013(7) 0.003(6) C83 0.073(9) 0.119(9) 0.112(10) -0.002(7) -0.007(8) -0.006(7) C84 0.100(10) 0.120(8) 0.099(10) 0.005(7) -0.003(8) 0.012(8) C85 0.075(8) 0.097(7) 0.082(8) -0.005(6) 0.017(6) 0.002(5) C86 0.093(10) 0.106(8) 0.087(9) 0.007(6) -0.015(7) -0.002(7) N92 0.140(11) 0.105(7) 0.092(8) -0.008(5) -0.004(7) -0.051(7) C93 0.061(7) 0.067(6) 0.082(8) -0.022(5) 0.012(6) 0.023(5) C94 0.075(9) 0.094(7) 0.113(11) -0.002(7) 0.028(8) 0.029(6) C95 0.105(11) 0.101(8) 0.097(10) -0.002(6) -0.018(8) 0.006(7) C97 0.182(17) 0.143(12) 0.125(13) -0.015(10) 0.006(12) 0.030(11) C98 0.145(17) 0.176(14) 0.192(19) -0.054(13) 0.029(15) 0.004(12) C99 0.132(16) 0.203(17) 0.24(2) -0.082(14) 0.008(16) 0.007(14) N81 0.063(6) 0.070(4) 0.092(6) -0.004(4) 0.003(5) 0.008(4) C77 0.087(10) 0.112(9) 0.099(10) -0.013(7) 0.009(8) -0.011(7) C78 0.086(10) 0.118(9) 0.147(13) -0.043(9) 0.025(9) 0.010(7) C79 0.173(17) 0.144(11) 0.146(15) -0.036(10) -0.038(13) 0.032(10) C80 0.098(10) 0.108(8) 0.095(10) -0.009(7) 0.008(8) -0.005(7) C771 0.153(15) 0.152(12) 0.191(18) -0.020(11) 0.040(13) -0.016(11) C772 0.154(14) 0.122(10) 0.167(16) -0.036(9) -0.002(12) 0.028(8) C801 0.166(14) 0.119(9) 0.137(13) -0.022(8) 0.001(11) -0.023(9) C802 0.168(14) 0.099(8) 0.135(12) -0.019(8) 0.020(10) -0.009(8) N91 0.060(6) 0.077(5) 0.060(6) -0.013(4) 0.004(4) -0.016(4) N96 0.088(7) 0.085(6) 0.080(7) -0.001(5) 0.000(5) 0.012(5) Y2 0.0933(8) 0.0931(6) 0.0996(8) 0.0027(5) 0.0083(6) 0.0029(5) N103 0.31(4) 0.23(2) 0.14(2) 0.009(16) 0.01(2) -0.02(2) O102 0.104(7) 0.177(8) 0.117(8) 0.008(7) 0.010(6) 0.015(6) O101 0.195(14) 0.185(11) 0.138(11) 0.024(8) 0.022(10) 0.022(8) O104 0.198(14) 0.363(18) 0.161(13) 0.050(13) 0.050(11) 0.073(12) N113 0.161(17) 0.150(15) 0.22(3) -0.062(17) -0.021(17) 0.007(11) O114 0.184(11) 0.198(10) 0.215(13) -0.029(9) 0.029(9) -0.014(8) O112 0.162(11) 0.136(9) 0.164(11) -0.011(7) 0.018(8) 0.000(7) O111 0.234(14) 0.136(8) 0.138(11) -0.018(7) 0.062(10) -0.015(7) N123 0.159(16) 0.124(10) 0.131(13) -0.016(8) 0.004(11) -0.011(10) O121 0.110(7) 0.146(7) 0.137(8) 0.009(6) 0.024(6) 0.002(5) O122 0.120(9) 0.151(8) 0.158(10) 0.004(6) -0.007(7) 0.028(6) O124 0.136(9) 0.198(10) 0.222(13) -0.071(8) 0.003(9) 0.020(9) N133 0.185(19) 0.111(11) 0.21(2) -0.022(12) 0.054(14) -0.032(12) O134 0.223(13) 0.167(9) 0.229(14) -0.021(9) 0.071(10) -0.032(8) O131 0.151(10) 0.144(9) 0.189(11) -0.034(8) 0.018(8) -0.006(7) O132 0.136(10) 0.123(7) 0.184(12) -0.005(7) 0.012(8) 0.007(6) N143 0.094(11) 0.115(8) 0.154(14) 0.006(8) -0.010(10) -0.007(7) O141 0.113(7) 0.128(6) 0.124(7) 0.017(5) 0.021(5) 0.015(5) O142 0.163(10) 0.180(8) 0.103(7) 0.019(6) 0.007(8) 0.019(7) O144 0.158(11) 0.168(8) 0.149(10) -0.006(7) 0.037(8) -0.021(7) N163 0.157(16) 0.135(11) 0.114(12) -0.004(9) -0.021(11) -0.007(9) O162 0.142(10) 0.159(9) 0.151(10) -0.017(7) 0.015(7) 0.000(7) O164 0.151(10) 0.172(8) 0.153(10) 0.009(7) -0.005(8) 0.007(7) O161 0.189(12) 0.195(10) 0.190(13) -0.006(9) 0.026(10) 0.010(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 Y1 N81 2.426(8) . ? Y1 N31 2.451(8) . ? Y1 N51 2.461(8) . ? Y1 N21 2.470(9) . ? Y1 N41 2.476(9) . ? Y1 N71 2.493(7) . ? Y1 N11 2.511(7) . ? Y1 N91 2.507(8) . ? Y1 N61 2.522(8) . ? N11 N12 1.305(10) . ? N11 C16 1.377(12) . ? N12 C13 1.315(12) . ? C13 C14 1.358(14) . ? C13 C17 1.485(15) . ? C14 N15 1.367(12) . ? C14 C20 1.477(15) . ? N15 C16 1.293(11) . ? C16 C22 1.442(14) . ? C22 C23 1.353(15) . ? C22 N21 1.358(13) . ? N21 C26 1.355(13) . ? C26 C25 1.378(14) . ? C26 C32 1.456(14) . ? C25 C24 1.315(13) . ? C24 C23 1.395(15) . ? N31 C32 1.363(13) . ? N31 N36 1.367(10) . ? C32 N33 1.352(14) . ? N33 C34 1.329(14) . ? C35 N36 1.261(11) . ? C35 C34 1.386(15) . ? C35 C40 1.462(16) . ? C34 C37 1.465(18) . ? C17 C18 1.493(17) . ? C17 C172 1.510(15) . ? C17 C171 1.559(15) . ? C18 C19 1.204(17) . ? C19 C20 1.548(19) . ? C20 C201 1.490(15) . ? C20 C202 1.521(19) . ? C37 C372 1.41(2) . ? C37 C38 1.43(2) . ? C37 C371 1.597(19) . ? C38 C39 1.423(18) . ? C39 C40 1.494(18) . ? C40 C401 1.503(18) . ? C40 C402 1.525(17) . ? N41 C46 1.275(14) . ? N41 N42 1.356(11) . ? N42 C43 1.246(13) . ? C43 C44 1.362(16) . ? C43 C47 1.627(16) . ? C44 N45 1.318(14) . ? C44 C50 1.58(2) . ? N45 C46 1.356(14) . ? C46 C52 1.521(14) . ? N51 C56 1.355(10) . ? N51 C52 1.424(12) . ? C53 C52 1.337(13) . ? C53 C54 1.349(14) . ? C55 C54 1.390(14) . ? C55 C56 1.406(13) . ? C56 C62 1.444(13) . ? N61 N66 1.298(11) . ? N61 C62 1.358(13) . ? C62 N63 1.361(12) . ? N63 C64 1.266(12) . ? C64 C65 1.431(13) . ? C64 C67 1.507(13) . ? C65 N66 1.360(11) . ? C65 C70 1.534(15) . ? C47 C472 1.482(17) . ? C47 C48 1.49(2) . ? C47 C471 1.560(18) . ? C48 C49 1.306(19) . ? C49 C50 1.48(2) . ? C50 C502 1.44(2) . ? C50 C501 1.508(19) . ? C67 C671 1.442(13) . ? C67 C672 1.522(14) . ? C67 C68 1.577(15) . ? C68 C69 1.566(16) . ? C69 C70 1.475(16) . ? C70 C701 1.517(15) . ? C70 C702 1.570(16) . ? N71 N72 1.313(10) . ? N71 C76 1.418(12) . ? N72 C73 1.323(12) . ? C73 C74 1.406(13) . ? C73 C77 1.444(15) . ? C74 N75 1.333(12) . ? C74 C80 1.557(15) . ? N75 C76 1.352(12) . ? C76 C82 1.492(14) . ? C82 C83 1.371(13) . ? C82 N81 1.393(12) . ? C83 C84 1.369(15) . ? C84 C85 1.330(14) . ? C85 C86 1.482(14) . ? C86 N81 1.297(13) . ? C86 N92 1.511(13) . ? N92 N91 1.338(11) . ? N92 C93 1.360(13) . ? C93 C94 1.276(14) . ? C94 C95 1.444(15) . ? C94 C97 1.461(18) . ? C95 N96 1.302(14) . ? C95 C100 1.483(16) . ? C97 C971 1.49(2) . ? C97 C972 1.49(2) . ? C97 C98 1.55(2) . ? C98 C99 1.264(18) . ? C99 C100 1.546(19) . ? C100 C102 1.410(19) . ? C100 C101 1.426(18) . ? C77 C771 1.458(17) . ? C77 C78 1.492(15) . ? C77 C772 1.543(17) . ? C78 C79 1.382(16) . ? C79 C80 1.538(18) . ? C80 C801 1.562(16) . ? C80 C802 1.589(16) . ? N91 N96 1.315(10) . ? Y2 O141 2.401(9) . ? Y2 O131 2.403(11) . ? Y2 O121 2.418(10) . ? Y2 O102 2.427(10) . ? Y2 O112 2.407(13) . ? Y2 O111 2.399(13) . ? Y2 O132 2.443(10) . ? Y2 O122 2.453(10) . ? Y2 O101 2.455(15) . ? Y2 O142 2.493(10) . ? N103 O101 1.23(2) . ? N103 O102 1.23(2) . ? N103 O104 1.32(2) . ? N113 O111 1.15(2) . ? N113 O112 1.26(2) . ? N113 O114 1.32(2) . ? N123 O122 1.223(15) . ? N123 O121 1.236(15) . ? N123 O124 1.281(16) . ? N133 O132 1.198(17) . ? N133 O131 1.209(16) . ? N133 O134 1.273(17) . ? N143 O142 1.205(14) . ? N143 O141 1.200(13) . ? N143 O144 1.255(15) . ? N163 O162 1.149(16) . ? N163 O164 1.225(15) . ? N163 O161 1.248(16) . ? O300 O500 1.74(3) 1_545 ? O500 O300 1.74(3) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N81 Y1 N31 72.3(3) . . ? N81 Y1 N51 122.4(3) . . ? N31 Y1 N51 137.0(2) . . ? N81 Y1 N21 122.0(3) . . ? N31 Y1 N21 65.8(3) . . ? N51 Y1 N21 115.7(3) . . ? N81 Y1 N41 73.3(3) . . ? N31 Y1 N41 145.7(3) . . ? N51 Y1 N41 65.7(3) . . ? N21 Y1 N41 136.0(3) . . ? N81 Y1 N71 65.8(3) . . ? N31 Y1 N71 85.2(3) . . ? N51 Y1 N71 137.6(2) . . ? N21 Y1 N71 72.2(3) . . ? N41 Y1 N71 80.3(3) . . ? N81 Y1 N11 134.8(2) . . ? N31 Y1 N11 130.4(3) . . ? N51 Y1 N11 71.0(2) . . ? N21 Y1 N11 64.8(3) . . ? N41 Y1 N11 76.0(3) . . ? N71 Y1 N11 77.0(3) . . ? N81 Y1 N91 65.2(3) . . ? N31 Y1 N91 80.5(3) . . ? N51 Y1 N91 72.9(2) . . ? N21 Y1 N91 137.9(2) . . ? N41 Y1 N91 86.0(3) . . ? N71 Y1 N91 131.1(3) . . ? N11 Y1 N91 143.7(3) . . ? N81 Y1 N61 134.5(3) . . ? N31 Y1 N61 77.2(3) . . ? N51 Y1 N61 64.5(3) . . ? N21 Y1 N61 71.6(3) . . ? N41 Y1 N61 130.1(4) . . ? N71 Y1 N61 143.7(3) . . ? N11 Y1 N61 90.7(3) . . ? N91 Y1 N61 77.1(3) . . ? N12 N11 C16 116.8(7) . . ? N12 N11 Y1 124.1(7) . . ? C16 N11 Y1 118.9(6) . . ? N11 N12 C13 120.8(9) . . ? N12 C13 C14 122.0(10) . . ? N12 C13 C17 118.2(12) . . ? C14 C13 C17 119.6(10) . . ? C13 C14 N15 116.8(9) . . ? C13 C14 C20 125.3(11) . . ? N15 C14 C20 117.7(12) . . ? C16 N15 C14 118.4(9) . . ? N15 C16 N11 123.8(9) . . ? N15 C16 C22 118.3(11) . . ? N11 C16 C22 117.1(10) . . ? C23 C22 N21 122.9(11) . . ? C23 C22 C16 121.0(12) . . ? N21 C22 C16 115.9(12) . . ? C26 N21 C22 118.0(10) . . ? C26 N21 Y1 119.8(7) . . ? C22 N21 Y1 122.2(8) . . ? N21 C26 C25 120.7(10) . . ? N21 C26 C32 117.6(11) . . ? C25 C26 C32 121.6(12) . . ? C24 C25 C26 119.6(11) . . ? C25 C24 C23 121.9(12) . . ? C22 C23 C24 116.3(12) . . ? C32 N31 N36 115.5(8) . . ? C32 N31 Y1 121.3(6) . . ? N36 N31 Y1 122.9(7) . . ? N33 C32 N31 125.7(10) . . ? N33 C32 C26 118.7(12) . . ? N31 C32 C26 115.5(11) . . ? C34 N33 C32 115.1(11) . . ? N36 C35 C34 123.7(9) . . ? N36 C35 C40 117.6(12) . . ? C34 C35 C40 118.7(11) . . ? N33 C34 C35 119.7(10) . . ? N33 C34 C37 118.8(14) . . ? C35 C34 C37 121.4(13) . . ? C35 N36 N31 120.0(9) . . ? C13 C17 C18 116.2(12) . . ? C13 C17 C172 110.8(10) . . ? C18 C17 C172 109.9(12) . . ? C13 C17 C171 108.0(10) . . ? C18 C17 C171 106.5(12) . . ? C172 C17 C171 104.7(11) . . ? C19 C18 C17 118.2(17) . . ? C18 C19 C20 129.4(17) . . ? C14 C20 C201 111.4(11) . . ? C14 C20 C202 108.0(11) . . ? C201 C20 C202 106.1(13) . . ? C14 C20 C19 107.5(12) . . ? C201 C20 C19 109.5(12) . . ? C202 C20 C19 114.5(13) . . ? C372 C37 C38 123.3(17) . . ? C372 C37 C34 112.0(14) . . ? C38 C37 C34 110.8(16) . . ? C372 C37 C371 106.3(17) . . ? C38 C37 C371 96.3(14) . . ? C34 C37 C371 105.2(12) . . ? C39 C38 C37 111.6(15) . . ? C38 C39 C40 111.6(14) . . ? C35 C40 C39 115.9(13) . . ? C35 C40 C401 108.7(11) . . ? C39 C40 C401 113.2(13) . . ? C35 C40 C402 108.7(11) . . ? C39 C40 C402 103.8(13) . . ? C401 C40 C402 105.9(14) . . ? C46 N41 N42 113.3(10) . . ? C46 N41 Y1 122.1(8) . . ? N42 N41 Y1 124.6(8) . . ? C43 N42 N41 122.8(10) . . ? N42 C43 C44 117.6(11) . . ? N42 C43 C47 116.3(13) . . ? C44 C43 C47 125.2(13) . . ? N45 C44 C43 125.5(12) . . ? N45 C44 C50 113.8(14) . . ? C43 C44 C50 120.7(13) . . ? C44 N45 C46 108.5(10) . . ? N41 C46 N45 131.1(11) . . ? N41 C46 C52 119.2(12) . . ? N45 C46 C52 109.6(12) . . ? C56 N51 C52 115.7(8) . . ? C56 N51 Y1 123.0(6) . . ? C52 N51 Y1 121.2(6) . . ? C52 C53 C54 119.8(11) . . ? C53 C52 N51 122.4(9) . . ? C53 C52 C46 125.9(11) . . ? N51 C52 C46 111.7(10) . . ? C54 C55 C56 116.2(9) . . ? C53 C54 C55 122.0(11) . . ? N51 C56 C55 123.5(9) . . ? N51 C56 C62 115.1(9) . . ? C55 C56 C62 121.3(9) . . ? N66 N61 C62 117.8(8) . . ? N66 N61 Y1 123.2(7) . . ? C62 N61 Y1 119.0(7) . . ? N61 C62 N63 124.3(10) . . ? N61 C62 C56 118.1(10) . . ? N63 C62 C56 117.5(11) . . ? C64 N63 C62 118.1(9) . . ? N63 C64 C65 119.7(9) . . ? N63 C64 C67 118.4(10) . . ? C65 C64 C67 121.6(10) . . ? N66 C65 C64 119.5(9) . . ? N66 C65 C70 113.5(10) . . ? C64 C65 C70 127.0(9) . . ? N61 N66 C65 120.3(9) . . ? C472 C47 C48 108.4(14) . . ? C472 C47 C471 111.9(14) . . ? C48 C47 C471 114.2(13) . . ? C472 C47 C43 113.2(11) . . ? C48 C47 C43 106.7(13) . . ? C471 C47 C43 102.4(11) . . ? C49 C48 C47 124.5(17) . . ? C48 C49 C50 125.2(18) . . ? C502 C50 C49 112.2(18) . . ? C502 C50 C501 106.4(16) . . ? C49 C50 C501 111.0(16) . . ? C502 C50 C44 109.9(14) . . ? C49 C50 C44 109.1(15) . . ? C501 C50 C44 108.1(14) . . ? C671 C67 C64 112.7(9) . . ? C671 C67 C672 109.5(9) . . ? C64 C67 C672 103.4(9) . . ? C671 C67 C68 109.7(10) . . ? C64 C67 C68 108.3(9) . . ? C672 C67 C68 113.2(9) . . ? C69 C68 C67 111.6(10) . . ? C70 C69 C68 113.9(11) . . ? C69 C70 C701 109.6(11) . . ? C69 C70 C65 107.8(11) . . ? C701 C70 C65 106.9(10) . . ? C69 C70 C702 113.6(12) . . ? C701 C70 C702 111.7(11) . . ? C65 C70 C702 107.0(9) . . ? N72 N71 C76 119.1(8) . . ? N72 N71 Y1 122.5(6) . . ? C76 N71 Y1 118.4(6) . . ? N71 N72 C73 121.3(8) . . ? N72 C73 C74 119.3(9) . . ? N72 C73 C77 118.7(10) . . ? C74 C73 C77 121.5(10) . . ? N75 C74 C73 121.6(9) . . ? N75 C74 C80 116.9(10) . . ? C73 C74 C80 121.4(10) . . ? C74 N75 C76 117.5(9) . . ? N75 C76 N71 120.9(9) . . ? N75 C76 C82 120.2(10) . . ? N71 C76 C82 118.5(10) . . ? C83 C82 N81 127.2(10) . . ? C83 C82 C76 121.6(11) . . ? N81 C82 C76 111.2(10) . . ? C84 C83 C82 119.4(11) . . ? C85 C84 C83 117.8(12) . . ? C84 C85 C86 118.9(10) . . ? N81 C86 C85 125.9(10) . . ? N81 C86 N92 116.5(10) . . ? C85 C86 N92 117.6(11) . . ? N91 N92 C93 126.2(8) . . ? N91 N92 C86 115.0(10) . . ? C93 N92 C86 117.5(10) . . ? C94 C93 N92 113.6(9) . . ? C93 C94 C95 122.4(10) . . ? C93 C94 C97 116.0(12) . . ? C95 C94 C97 121.5(13) . . ? N96 C95 C94 118.3(10) . . ? N96 C95 C100 117.1(12) . . ? C94 C95 C100 124.6(13) . . ? C94 C97 C971 108.9(13) . . ? C94 C97 C972 107.5(15) . . ? C971 C97 C972 113.8(16) . . ? C94 C97 C98 108.5(14) . . ? C971 C97 C98 111.5(16) . . ? C972 C97 C98 106.3(15) . . ? C99 C98 C97 123(2) . . ? C98 C99 C100 116.0(17) . . ? C102 C100 C101 113.8(15) . . ? C102 C100 C95 105.8(14) . . ? C101 C100 C95 113.6(12) . . ? C102 C100 C99 99.0(14) . . ? C101 C100 C99 115.6(16) . . ? C95 C100 C99 107.7(12) . . ? C86 N81 C82 110.8(9) . . ? C86 N81 Y1 123.2(7) . . ? C82 N81 Y1 125.9(7) . . ? C73 C77 C771 109.6(11) . . ? C73 C77 C78 112.4(10) . . ? C771 C77 C78 110.2(12) . . ? C73 C77 C772 110.7(11) . . ? C771 C77 C772 102.0(12) . . ? C78 C77 C772 111.4(11) . . ? C79 C78 C77 112.9(12) . . ? C78 C79 C80 111.3(14) . . ? C79 C80 C74 107.9(10) . . ? C79 C80 C801 122.6(12) . . ? C74 C80 C801 99.8(10) . . ? C79 C80 C802 112.9(12) . . ? C74 C80 C802 107.2(9) . . ? C801 C80 C802 104.9(11) . . ? N92 N91 N96 117.3(8) . . ? N92 N91 Y1 119.2(6) . . ? N96 N91 Y1 123.3(7) . . ? C95 N96 N91 121.2(9) . . ? O141 Y2 O131 82.1(4) . . ? O141 Y2 O121 158.7(3) . . ? O131 Y2 O121 77.5(4) . . ? O141 Y2 O102 71.1(4) . . ? O131 Y2 O102 130.3(4) . . ? O121 Y2 O102 118.6(4) . . ? O141 Y2 O112 126.6(3) . . ? O131 Y2 O112 148.8(4) . . ? O121 Y2 O112 74.7(3) . . ? O102 Y2 O112 76.7(4) . . ? O141 Y2 O111 80.5(4) . . ? O131 Y2 O111 134.2(4) . . ? O121 Y2 O111 118.4(4) . . ? O102 Y2 O111 82.3(4) . . ? O112 Y2 O111 53.4(4) . . ? O141 Y2 O132 75.4(4) . . ? O131 Y2 O132 51.2(3) . . ? O121 Y2 O132 87.1(4) . . ? O102 Y2 O132 81.3(4) . . ? O112 Y2 O132 139.6(4) . . ? O111 Y2 O132 154.2(4) . . ? O141 Y2 O122 127.6(4) . . ? O131 Y2 O122 74.5(4) . . ? O121 Y2 O122 51.7(3) . . ? O102 Y2 O122 153.9(4) . . ? O112 Y2 O122 77.2(4) . . ? O111 Y2 O122 83.5(4) . . ? O132 Y2 O122 118.7(4) . . ? O141 Y2 O101 112.9(4) . . ? O131 Y2 O101 108.6(4) . . ? O121 Y2 O101 68.9(4) . . ? O102 Y2 O101 51.4(4) . . ? O112 Y2 O101 74.2(4) . . ? O111 Y2 O101 117.2(4) . . ? O132 Y2 O101 65.7(4) . . ? O122 Y2 O101 118.8(5) . . ? O141 Y2 O142 50.2(3) . . ? O131 Y2 O142 67.7(4) . . ? O121 Y2 O142 124.6(4) . . ? O102 Y2 O142 116.8(4) . . ? O112 Y2 O142 118.5(3) . . ? O111 Y2 O142 68.6(4) . . ? O132 Y2 O142 101.6(4) . . ? O122 Y2 O142 77.6(4) . . ? O101 Y2 O142 162.4(4) . . ? O101 N103 O102 119(3) . . ? O101 N103 O104 119(3) . . ? O102 N103 O104 110(3) . . ? N103 O102 Y2 90.7(15) . . ? N103 O101 Y2 89.5(17) . . ? O111 N113 O112 128(2) . . ? O111 N113 O114 117(2) . . ? O112 N113 O114 115(2) . . ? N113 O112 Y2 87.9(13) . . ? N113 O111 Y2 90.7(14) . . ? O122 N123 O121 119.5(17) . . ? O122 N123 O124 118.4(17) . . ? O121 N123 O124 122.0(17) . . ? N123 O121 Y2 94.9(10) . . ? N123 O122 Y2 93.6(11) . . ? O132 N133 O131 120.8(17) . . ? O132 N133 O134 118.6(19) . . ? O131 N133 O134 120(2) . . ? O132 N133 Y2 61.4(9) . . ? O131 N133 Y2 59.6(10) . . ? O134 N133 Y2 176.4(13) . . ? N133 O131 Y2 94.7(12) . . ? N133 O132 Y2 93.0(11) . . ? O142 N143 O141 119.3(16) . . ? O142 N143 O144 123.5(16) . . ? O141 N143 O144 116.9(15) . . ? O142 N143 Y2 62.0(9) . . ? O141 N143 Y2 57.6(8) . . ? O144 N143 Y2 174.5(12) . . ? N143 O141 Y2 97.5(10) . . ? N143 O142 Y2 92.7(10) . . ? O162 N163 O164 131.8(18) . . ? O162 N163 O161 116.5(18) . . ? O164 N163 O161 111.3(17) . . ? _refine_diff_density_max 0.428 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.061