# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Richard Jones' _publ_contact_author_email RAJONES@MAIL.UTEXAS.EDU _publ_section_title ; Anion Dependant Self-assembly and the First X-Ray Structure of a Neutral Homoleptic Lanthanide Salen Complex Tb4(Salen)6) ; loop_ _publ_author_name 'R Jones' 'Wai-Kwok Wong.' 'Xiaoping Yang.' data_complex-1 _database_code_depnum_ccdc_archive 'CCDC 680102' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H116 N12 O22 Tb4' _chemical_formula_weight 2497.75 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' Tb Tb -0.1723 4.1537 '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 13.537(2) _cell_length_b 14.101(3) _cell_length_c 15.774(3) _cell_angle_alpha 69.31(3) _cell_angle_beta 78.51(2) _cell_angle_gamma 63.05(3) _cell_volume 2508.1(11) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 2.862 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.7251 _exptl_absorpt_correction_T_max 0.8701 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14396 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0848 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8772 _reflns_number_gt 6178 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and Rfactors based on ALL data will be even larger. Hydrogen atoms of water molecules were not added. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+1.2517P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0050(2) _refine_ls_number_reflns 8772 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.21576(3) 0.79825(3) 0.24086(3) 0.01965(14) Uani 1 1 d . . . Tb2 Tb 0.44367(3) 0.53486(3) 0.38415(3) 0.01782(13) Uani 1 1 d . . . N1 N 0.2088(6) 0.8961(6) 0.3496(5) 0.0227(16) Uani 1 1 d . . . N2 N 0.3037(6) 0.9359(6) 0.1735(5) 0.0255(17) Uani 1 1 d . . . N3 N 0.2588(6) 0.6294(6) 0.1910(5) 0.0281(18) Uani 1 1 d . . . N4 N 0.0688(6) 0.7241(6) 0.2908(5) 0.0225(16) Uani 1 1 d . . . N5 N 0.5545(5) 0.4095(5) 0.2862(4) 0.0206(16) Uani 1 1 d . . . N6 N 0.6343(5) 0.5266(5) 0.3430(5) 0.0213(16) Uani 1 1 d . . . O1 O 0.2632(4) 0.6704(4) 0.3891(4) 0.0208(13) Uani 1 1 d . . . O2 O 0.1997(5) 0.8601(5) 0.0890(4) 0.0288(14) Uani 1 1 d . . . O3 O 0.4101(4) 0.6794(4) 0.2468(4) 0.0193(12) Uani 1 1 d . . . O4 O 0.0485(5) 0.9465(5) 0.2296(4) 0.0264(14) Uani 1 1 d . . . O5 O 0.3534(4) 0.4350(4) 0.3910(4) 0.0221(13) Uani 1 1 d . . . O6 O 0.4826(5) 0.6069(4) 0.4795(3) 0.0193(13) Uani 1 1 d . . . C1 C 0.1862(6) 0.6849(7) 0.4576(5) 0.0208(19) Uani 1 1 d . . . C2 C 0.1518(7) 0.6000(8) 0.5104(6) 0.028(2) Uani 1 1 d . . . H2A H 0.1845 0.5318 0.4986 0.033 Uiso 1 1 calc R . . C3 C 0.0720(7) 0.6155(8) 0.5784(6) 0.034(2) Uani 1 1 d . . . H3A H 0.0503 0.5584 0.6114 0.040 Uiso 1 1 calc R . . C4 C 0.0225(7) 0.7160(9) 0.5993(6) 0.037(2) Uani 1 1 d . . . H4A H -0.0329 0.7266 0.6451 0.045 Uiso 1 1 calc R . . C5 C 0.0562(7) 0.7976(8) 0.5521(6) 0.030(2) Uani 1 1 d . . . H5A H 0.0256 0.8632 0.5680 0.036 Uiso 1 1 calc R . . C6 C 0.1360(7) 0.7865(7) 0.4799(6) 0.027(2) Uani 1 1 d . . . C7 C 0.1658(7) 0.8810(7) 0.4302(6) 0.027(2) Uani 1 1 d . . . H7A H 0.1524 0.9328 0.4595 0.033 Uiso 1 1 calc R . . C8 C 0.2317(8) 0.9953(8) 0.3090(6) 0.034(2) Uani 1 1 d . . . H8A H 0.2484 1.0153 0.3555 0.041 Uiso 1 1 calc R . . H8B H 0.1677 1.0578 0.2777 0.041 Uiso 1 1 calc R . . C9 C 0.3311(8) 0.9666(8) 0.2423(6) 0.035(2) Uani 1 1 d . . . H9A H 0.3491 1.0304 0.2135 0.042 Uiso 1 1 calc R . . H9B H 0.3950 0.9050 0.2742 0.042 Uiso 1 1 calc R . . C10 C 0.3291(7) 0.9760(7) 0.0906(6) 0.027(2) Uani 1 1 d . . . H10A H 0.3640 1.0230 0.0799 0.033 Uiso 1 1 calc R . . C11 C 0.3118(7) 0.9590(7) 0.0119(6) 0.029(2) Uani 1 1 d . . . C12 C 0.3591(9) 1.0018(8) -0.0702(7) 0.041(3) Uani 1 1 d . . . H12A H 0.3998 1.0407 -0.0716 0.049 Uiso 1 1 calc R . . C13 C 0.3481(9) 0.9889(9) -0.1499(7) 0.045(3) Uani 1 1 d . . . H13A H 0.3830 1.0157 -0.2038 0.054 Uiso 1 1 calc R . . C14 C 0.2833(8) 0.9345(8) -0.1475(6) 0.037(2) Uani 1 1 d . . . H14A H 0.2734 0.9266 -0.2009 0.045 Uiso 1 1 calc R . . C15 C 0.2341(8) 0.8925(7) -0.0686(6) 0.033(2) Uani 1 1 d . . . H15A H 0.1911 0.8566 -0.0690 0.039 Uiso 1 1 calc R . . C16 C 0.2474(7) 0.9027(7) 0.0140(6) 0.027(2) Uani 1 1 d . . . C17 C 0.4585(7) 0.6785(7) 0.1639(6) 0.025(2) Uani 1 1 d . . . C18 C 0.5387(7) 0.7214(7) 0.1294(6) 0.026(2) Uani 1 1 d . . . H18A H 0.5579 0.7511 0.1643 0.031 Uiso 1 1 calc R . . C19 C 0.5895(8) 0.7204(8) 0.0447(6) 0.035(2) Uani 1 1 d . . . H19A H 0.6430 0.7486 0.0233 0.042 Uiso 1 1 calc R . . C20 C 0.5605(8) 0.6764(8) -0.0102(7) 0.042(3) Uani 1 1 d . . . H20A H 0.5941 0.6755 -0.0676 0.050 Uiso 1 1 calc R . . C21 C 0.4820(8) 0.6357(8) 0.0237(6) 0.035(2) Uani 1 1 d . . . H21A H 0.4631 0.6064 -0.0117 0.042 Uiso 1 1 calc R . . C22 C 0.4287(7) 0.6358(7) 0.1087(6) 0.026(2) Uani 1 1 d . . . C23 C 0.3411(7) 0.5963(7) 0.1364(6) 0.028(2) Uani 1 1 d . . . H23A H 0.3455 0.5429 0.1124 0.034 Uiso 1 1 calc R . . C24 C 0.1712(7) 0.5896(7) 0.2080(6) 0.030(2) Uani 1 1 d . . . H24A H 0.2040 0.5112 0.2116 0.036 Uiso 1 1 calc R . . H24B H 0.1210 0.6311 0.1586 0.036 Uiso 1 1 calc R . . C25 C 0.1082(7) 0.6055(7) 0.2964(6) 0.028(2) Uani 1 1 d . . . H25A H 0.0457 0.5863 0.3058 0.033 Uiso 1 1 calc R . . H25B H 0.1563 0.5576 0.3468 0.033 Uiso 1 1 calc R . . C26 C -0.0287(7) 0.7710(7) 0.3235(6) 0.027(2) Uani 1 1 d . . . H26A H -0.0696 0.7285 0.3457 0.033 Uiso 1 1 calc R . . C27 C -0.0828(7) 0.8843(7) 0.3298(6) 0.025(2) Uani 1 1 d . . . C28 C -0.1822(8) 0.9124(8) 0.3850(6) 0.036(2) Uani 1 1 d . . . H28A H -0.2097 0.8587 0.4146 0.043 Uiso 1 1 calc R . . C29 C -0.2375(8) 1.0147(8) 0.3954(7) 0.038(2) Uani 1 1 d . . . H29A H -0.3023 1.0310 0.4320 0.046 Uiso 1 1 calc R . . C30 C -0.1975(8) 1.0972(8) 0.3508(6) 0.035(2) Uani 1 1 d . . . H30A H -0.2353 1.1679 0.3583 0.042 Uiso 1 1 calc R . . C31 C -0.1015(7) 1.0724(7) 0.2960(6) 0.029(2) Uani 1 1 d . . . H31A H -0.0763 1.1278 0.2665 0.035 Uiso 1 1 calc R . . C32 C -0.0408(6) 0.9672(7) 0.2832(6) 0.024(2) Uani 1 1 d . . . C33 C 0.3582(7) 0.3526(7) 0.3687(6) 0.025(2) Uani 1 1 d . . . C34 C 0.2779(7) 0.3087(7) 0.4023(6) 0.025(2) Uani 1 1 d . . . H34A H 0.2204 0.3394 0.4414 0.030 Uiso 1 1 calc R . . C35 C 0.2826(8) 0.2228(8) 0.3790(7) 0.034(2) Uani 1 1 d . . . H35A H 0.2281 0.1962 0.4022 0.040 Uiso 1 1 calc R . . C36 C 0.3656(8) 0.1746(8) 0.3221(7) 0.038(2) Uani 1 1 d . . . H36A H 0.3687 0.1146 0.3079 0.045 Uiso 1 1 calc R . . C37 C 0.4453(8) 0.2161(8) 0.2859(7) 0.034(2) Uani 1 1 d . . . H37A H 0.5008 0.1848 0.2458 0.041 Uiso 1 1 calc R . . C38 C 0.4438(7) 0.3044(7) 0.3084(6) 0.025(2) Uani 1 1 d . . . C39 C 0.5351(7) 0.3359(7) 0.2706(6) 0.024(2) Uani 1 1 d . . . H39A H 0.5850 0.2990 0.2308 0.029 Uiso 1 1 calc R . . C40 C 0.6568(7) 0.4226(7) 0.2405(6) 0.026(2) Uani 1 1 d . . . H40A H 0.6378 0.4872 0.1868 0.031 Uiso 1 1 calc R . . H40B H 0.7063 0.3572 0.2216 0.031 Uiso 1 1 calc R . . C41 C 0.7142(7) 0.4371(7) 0.3051(6) 0.027(2) Uani 1 1 d . . . H41A H 0.7441 0.3679 0.3538 0.033 Uiso 1 1 calc R . . H41B H 0.7752 0.4556 0.2732 0.033 Uiso 1 1 calc R . . C42 C 0.6646(7) 0.5997(7) 0.3415(6) 0.024(2) Uani 1 1 d . . . H42A H 0.7338 0.5942 0.3142 0.029 Uiso 1 1 calc R . . C43 C 0.5988(7) 0.6934(7) 0.3799(5) 0.0202(19) Uani 1 1 d . . . C44 C 0.6286(7) 0.7830(7) 0.3515(6) 0.026(2) Uani 1 1 d . . . H44A H 0.6873 0.7819 0.3090 0.032 Uiso 1 1 calc R . . C45 C 0.5730(7) 0.8733(7) 0.3848(6) 0.026(2) Uani 1 1 d . . . H45A H 0.5941 0.9322 0.3656 0.032 Uiso 1 1 calc R . . C46 C 0.4853(7) 0.8741(7) 0.4476(6) 0.029(2) Uani 1 1 d . . . H46A H 0.4459 0.9353 0.4693 0.034 Uiso 1 1 calc R . . C47 C 0.4553(7) 0.7863(7) 0.4784(6) 0.0209(19) Uani 1 1 d . . . H47A H 0.3970 0.7882 0.5215 0.025 Uiso 1 1 calc R . . C48 C 0.5112(7) 0.6942(7) 0.4458(5) 0.0205(19) Uani 1 1 d . . . C49 C 0.1596(11) 0.6045(12) -0.0414(9) 0.095(5) Uani 1 1 d . . . H49A H 0.2090 0.6329 -0.0346 0.142 Uiso 1 1 calc R . . H49B H 0.2016 0.5299 -0.0451 0.142 Uiso 1 1 calc R . . H49C H 0.1077 0.6041 0.0099 0.142 Uiso 1 1 calc R . . O7 O 0.1025(7) 0.6719(7) -0.1200(6) 0.072(3) Uani 1 1 d . . . H7B H 0.0431 0.7194 -0.1079 0.108 Uiso 1 1 calc R . . C50 C -0.1439(14) 0.6744(16) 0.8592(12) 0.119(7) Uani 1 1 d . . . H50A H -0.1707 0.6395 0.9172 0.178 Uiso 1 1 calc R . . H50B H -0.1917 0.6921 0.8132 0.178 Uiso 1 1 calc R . . H50C H -0.1430 0.7416 0.8604 0.178 Uiso 1 1 calc R . . O8 O -0.0297(13) 0.5969(12) 0.8388(10) 0.148(5) Uani 1 1 d . . . H8C H 0.0090 0.6315 0.8174 0.222 Uiso 1 1 calc R . . C51 C 0.1367(11) 0.3098(12) 0.8621(11) 0.113(7) Uani 1 1 d . . . H51A H 0.0974 0.3262 0.9166 0.169 Uiso 1 1 calc R . . H51B H 0.2144 0.2866 0.8666 0.169 Uiso 1 1 calc R . . H51C H 0.1252 0.2510 0.8543 0.169 Uiso 1 1 calc R . . O9 O 0.0969(8) 0.4061(9) 0.7871(7) 0.093(3) Uani 1 1 d . . . H9C H 0.0922 0.4601 0.7991 0.140 Uiso 1 1 calc R . . O1W O -0.0058(6) 0.8693(6) 0.0710(5) 0.0481(19) Uani 1 1 d . . . O2W O -0.0422(5) 0.8654(5) -0.0924(4) 0.0394(16) Uani 1 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 Tb1 0.0196(2) 0.0194(2) 0.0202(2) -0.00672(18) -0.00079(17) -0.00779(19) Tb2 0.0181(2) 0.0173(2) 0.0185(2) -0.00644(18) 0.00012(17) -0.00738(18) N1 0.029(4) 0.026(4) 0.020(4) -0.011(3) -0.001(3) -0.015(3) N2 0.029(4) 0.027(4) 0.024(4) -0.007(3) -0.003(3) -0.014(3) N3 0.031(4) 0.031(4) 0.032(4) -0.017(4) -0.001(4) -0.015(4) N4 0.019(4) 0.019(4) 0.026(4) -0.005(3) -0.002(3) -0.006(3) N5 0.022(4) 0.018(4) 0.015(4) -0.001(3) 0.002(3) -0.007(3) N6 0.023(4) 0.021(4) 0.024(4) -0.011(3) 0.000(3) -0.010(3) O1 0.022(3) 0.025(3) 0.015(3) -0.008(3) 0.002(2) -0.010(3) O2 0.035(4) 0.035(4) 0.019(3) -0.010(3) 0.001(3) -0.016(3) O3 0.018(3) 0.018(3) 0.015(3) -0.002(2) 0.002(2) -0.006(2) O4 0.021(3) 0.022(3) 0.033(4) -0.012(3) 0.002(3) -0.005(3) O5 0.022(3) 0.019(3) 0.026(3) -0.010(3) 0.000(3) -0.007(3) O6 0.030(3) 0.016(3) 0.017(3) -0.004(2) -0.002(2) -0.014(3) C1 0.017(4) 0.037(5) 0.012(4) -0.008(4) -0.003(3) -0.012(4) C2 0.023(5) 0.035(5) 0.026(5) -0.008(4) -0.003(4) -0.014(4) C3 0.023(5) 0.048(6) 0.033(6) -0.005(5) 0.002(4) -0.023(5) C4 0.022(5) 0.058(7) 0.026(5) -0.014(5) 0.011(4) -0.015(5) C5 0.021(5) 0.042(6) 0.025(5) -0.018(5) 0.002(4) -0.006(4) C6 0.018(5) 0.030(5) 0.031(5) -0.012(4) -0.008(4) -0.003(4) C7 0.029(5) 0.022(5) 0.026(5) -0.013(4) -0.006(4) 0.000(4) C8 0.053(7) 0.036(6) 0.023(5) -0.007(4) -0.002(5) -0.028(5) C9 0.042(6) 0.036(6) 0.040(6) -0.014(5) -0.007(5) -0.024(5) C10 0.029(5) 0.021(5) 0.036(6) -0.010(4) 0.004(4) -0.015(4) C11 0.030(5) 0.020(5) 0.025(5) -0.006(4) 0.003(4) -0.005(4) C12 0.051(7) 0.022(5) 0.038(6) 0.001(5) 0.000(5) -0.012(5) C13 0.053(7) 0.043(6) 0.019(5) -0.004(5) 0.006(5) -0.010(6) C14 0.041(6) 0.031(6) 0.022(5) -0.008(4) -0.006(4) 0.002(5) C15 0.035(6) 0.028(5) 0.020(5) -0.007(4) -0.002(4) -0.001(4) C16 0.028(5) 0.027(5) 0.014(5) -0.006(4) -0.002(4) -0.002(4) C17 0.020(5) 0.018(5) 0.024(5) 0.001(4) 0.002(4) -0.003(4) C18 0.019(5) 0.019(5) 0.032(5) -0.005(4) -0.002(4) -0.003(4) C19 0.031(6) 0.029(5) 0.029(6) 0.005(4) 0.004(4) -0.012(4) C20 0.043(6) 0.041(6) 0.026(6) -0.007(5) 0.009(5) -0.012(5) C21 0.030(5) 0.038(6) 0.028(5) -0.014(5) 0.000(4) -0.004(5) C22 0.027(5) 0.022(5) 0.024(5) -0.005(4) -0.004(4) -0.008(4) C23 0.031(5) 0.019(5) 0.030(5) -0.015(4) -0.008(4) 0.001(4) C24 0.033(5) 0.023(5) 0.040(6) -0.014(4) -0.007(4) -0.011(4) C25 0.020(5) 0.022(5) 0.039(6) -0.003(4) -0.009(4) -0.007(4) C26 0.028(5) 0.028(5) 0.030(5) -0.008(4) -0.001(4) -0.016(4) C27 0.016(5) 0.030(5) 0.030(5) -0.015(4) -0.001(4) -0.007(4) C28 0.038(6) 0.042(6) 0.032(6) -0.012(5) -0.003(5) -0.018(5) C29 0.028(5) 0.046(6) 0.044(6) -0.026(5) 0.008(5) -0.013(5) C30 0.030(5) 0.035(6) 0.038(6) -0.019(5) -0.001(4) -0.006(5) C31 0.032(5) 0.028(5) 0.034(6) -0.011(4) 0.000(4) -0.018(4) C32 0.012(4) 0.033(5) 0.023(5) -0.011(4) -0.001(4) -0.004(4) C33 0.026(5) 0.021(5) 0.025(5) -0.004(4) -0.009(4) -0.007(4) C34 0.032(5) 0.020(5) 0.028(5) -0.009(4) 0.002(4) -0.016(4) C35 0.029(6) 0.031(6) 0.043(6) -0.010(5) -0.004(5) -0.014(4) C36 0.046(6) 0.034(6) 0.051(7) -0.024(5) 0.000(5) -0.024(5) C37 0.033(6) 0.034(6) 0.042(6) -0.020(5) 0.001(4) -0.013(5) C38 0.025(5) 0.018(5) 0.033(5) -0.005(4) -0.007(4) -0.011(4) C39 0.024(5) 0.026(5) 0.017(5) -0.008(4) 0.000(4) -0.003(4) C40 0.017(5) 0.027(5) 0.032(5) -0.013(4) 0.003(4) -0.005(4) C41 0.025(5) 0.027(5) 0.030(5) -0.011(4) 0.004(4) -0.010(4) C42 0.015(4) 0.033(5) 0.025(5) -0.005(4) -0.002(4) -0.012(4) C43 0.022(5) 0.022(5) 0.019(5) -0.007(4) -0.002(4) -0.010(4) C44 0.026(5) 0.026(5) 0.025(5) -0.004(4) -0.003(4) -0.012(4) C45 0.035(5) 0.025(5) 0.023(5) -0.001(4) -0.004(4) -0.019(4) C46 0.033(5) 0.024(5) 0.029(5) -0.008(4) -0.006(4) -0.010(4) C47 0.023(5) 0.024(5) 0.021(5) -0.007(4) 0.001(4) -0.016(4) C48 0.029(5) 0.016(4) 0.016(4) -0.002(4) -0.006(4) -0.009(4) C49 0.068(10) 0.080(10) 0.059(9) -0.003(8) 0.008(8) 0.017(8) O7 0.073(6) 0.053(5) 0.055(5) -0.011(4) 0.000(5) -0.001(5) C50 0.081(13) 0.149(17) 0.092(13) 0.014(12) -0.003(10) -0.057(13) O8 0.142(13) 0.164(13) 0.182(15) -0.093(12) 0.030(11) -0.085(11) C51 0.054(9) 0.080(11) 0.119(14) 0.040(10) 0.025(9) -0.021(8) O9 0.087(7) 0.106(8) 0.094(8) -0.026(7) 0.004(6) -0.052(7) O1W 0.054(5) 0.052(5) 0.046(5) -0.011(4) -0.015(4) -0.026(4) O2W 0.044(4) 0.029(4) 0.039(4) -0.006(3) -0.002(3) -0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O2 2.260(6) . ? Tb1 O4 2.267(6) . ? Tb1 O1 2.387(5) . ? Tb1 O3 2.394(5) . ? Tb1 N1 2.519(6) . ? Tb1 N4 2.520(7) . ? Tb1 N2 2.539(7) . ? Tb1 N3 2.551(7) . ? Tb1 Tb2 3.858(2) . ? Tb2 O5 2.211(5) . ? Tb2 O1 2.330(6) . ? Tb2 O6 2.336(5) . ? Tb2 O3 2.343(5) . ? Tb2 O6 2.372(5) 2_666 ? Tb2 N6 2.492(7) . ? Tb2 N5 2.522(7) . ? Tb2 Tb2 3.8694(12) 2_666 ? N1 C7 1.277(11) . ? N1 C8 1.464(11) . ? N2 C10 1.274(11) . ? N2 C9 1.462(11) . ? N3 C23 1.278(11) . ? N3 C24 1.472(11) . ? N4 C26 1.274(11) . ? N4 C25 1.482(11) . ? N5 C39 1.290(11) . ? N5 C40 1.487(10) . ? N6 C42 1.263(10) . ? N6 C41 1.468(11) . ? O1 C1 1.346(9) . ? O2 C16 1.312(10) . ? O3 C17 1.341(10) . ? O4 C32 1.307(10) . ? O5 C33 1.299(10) . ? O6 C48 1.354(9) . ? O6 Tb2 2.372(5) 2_666 ? C1 C2 1.409(12) . ? C1 C6 1.420(12) . ? C2 C3 1.362(13) . ? C2 H2A 0.9300 . ? C3 C4 1.395(14) . ? C3 H3A 0.9300 . ? C4 C5 1.349(13) . ? C4 H4A 0.9300 . ? C5 C6 1.405(12) . ? C5 H5A 0.9300 . ? C6 C7 1.475(12) . ? C7 H7A 0.9300 . ? C8 C9 1.525(13) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.424(12) . ? C10 H10A 0.9300 . ? C11 C12 1.386(13) . ? C11 C16 1.411(13) . ? C12 C13 1.378(14) . ? C12 H12A 0.9300 . ? C13 C14 1.391(14) . ? C13 H13A 0.9300 . ? C14 C15 1.360(13) . ? C14 H14A 0.9300 . ? C15 C16 1.414(12) . ? C15 H15A 0.9300 . ? C17 C18 1.404(12) . ? C17 C22 1.419(12) . ? C18 C19 1.377(13) . ? C18 H18A 0.9300 . ? C19 C20 1.423(14) . ? C19 H19A 0.9300 . ? C20 C21 1.361(14) . ? C20 H20A 0.9300 . ? C21 C22 1.391(12) . ? C21 H21A 0.9300 . ? C22 C23 1.459(12) . ? C23 H23A 0.9300 . ? C24 C25 1.515(13) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.456(12) . ? C26 H26A 0.9300 . ? C27 C28 1.421(13) . ? C27 C32 1.434(12) . ? C28 C29 1.345(13) . ? C28 H28A 0.9300 . ? C29 C30 1.408(13) . ? C29 H29A 0.9300 . ? C30 C31 1.383(13) . ? C30 H30A 0.9300 . ? C31 C32 1.399(12) . ? C31 H31A 0.9300 . ? C33 C34 1.411(12) . ? C33 C38 1.419(12) . ? C34 C35 1.358(12) . ? C34 H34A 0.9300 . ? C35 C36 1.367(13) . ? C35 H35A 0.9300 . ? C36 C37 1.387(13) . ? C36 H36A 0.9300 . ? C37 C38 1.401(12) . ? C37 H37A 0.9300 . ? C38 C39 1.448(12) . ? C39 H39A 0.9300 . ? C40 C41 1.514(11) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.479(12) . ? C42 H42A 0.9300 . ? C43 C44 1.396(11) . ? C43 C48 1.412(12) . ? C44 C45 1.383(12) . ? C44 H44A 0.9300 . ? C45 C46 1.385(12) . ? C45 H45A 0.9300 . ? C46 C47 1.373(11) . ? C46 H46A 0.9300 . ? C47 C48 1.396(12) . ? C47 H47A 0.9300 . ? C49 O7 1.387(14) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? O7 H7B 0.8200 . ? C50 O8 1.48(2) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? O8 H8C 0.8200 . ? C51 O9 1.411(15) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? O9 H9C 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Tb1 O4 79.8(2) . . ? O2 Tb1 O1 159.2(2) . . ? O4 Tb1 O1 116.5(2) . . ? O2 Tb1 O3 99.2(2) . . ? O4 Tb1 O3 164.41(19) . . ? O1 Tb1 O3 68.63(18) . . ? O2 Tb1 N1 130.9(2) . . ? O4 Tb1 N1 72.7(2) . . ? O1 Tb1 N1 68.9(2) . . ? O3 Tb1 N1 97.2(2) . . ? O2 Tb1 N4 100.2(2) . . ? O4 Tb1 N4 72.4(2) . . ? O1 Tb1 N4 74.8(2) . . ? O3 Tb1 N4 122.8(2) . . ? N1 Tb1 N4 108.8(2) . . ? O2 Tb1 N2 72.1(2) . . ? O4 Tb1 N2 87.8(2) . . ? O1 Tb1 N2 118.9(2) . . ? O3 Tb1 N2 77.2(2) . . ? N1 Tb1 N2 67.1(2) . . ? N4 Tb1 N2 159.9(2) . . ? O2 Tb1 N3 73.1(2) . . ? O4 Tb1 N3 124.3(2) . . ? O1 Tb1 N3 86.6(2) . . ? O3 Tb1 N3 69.3(2) . . ? N1 Tb1 N3 155.2(2) . . ? N4 Tb1 N3 66.1(2) . . ? N2 Tb1 N3 126.1(2) . . ? O2 Tb1 Tb2 128.86(16) . . ? O4 Tb1 Tb2 150.94(15) . . ? O1 Tb1 Tb2 34.64(13) . . ? O3 Tb1 Tb2 35.04(12) . . ? N1 Tb1 Tb2 87.57(16) . . ? N4 Tb1 Tb2 95.12(15) . . ? N2 Tb1 Tb2 104.17(16) . . ? N3 Tb1 Tb2 69.39(16) . . ? O5 Tb2 O1 81.45(19) . . ? O5 Tb2 O6 138.68(19) . . ? O1 Tb2 O6 85.55(19) . . ? O5 Tb2 O3 109.34(19) . . ? O1 Tb2 O3 70.44(18) . . ? O6 Tb2 O3 102.74(18) . . ? O5 Tb2 O6 82.87(18) . 2_666 ? O1 Tb2 O6 118.63(19) . 2_666 ? O6 Tb2 O6 69.5(2) . 2_666 ? O3 Tb2 O6 166.40(18) . 2_666 ? O5 Tb2 N6 138.2(2) . . ? O1 Tb2 N6 137.8(2) . . ? O6 Tb2 N6 71.6(2) . . ? O3 Tb2 N6 80.4(2) . . ? O6 Tb2 N6 86.5(2) 2_666 . ? O5 Tb2 N5 73.1(2) . . ? O1 Tb2 N5 136.0(2) . . ? O6 Tb2 N5 136.4(2) . . ? O3 Tb2 N5 84.7(2) . . ? O6 Tb2 N5 93.5(2) 2_666 . ? N6 Tb2 N5 67.4(2) . . ? O5 Tb2 Tb1 90.28(14) . . ? O1 Tb2 Tb1 35.62(13) . . ? O6 Tb2 Tb1 101.43(13) . . ? O3 Tb2 Tb1 35.92(13) . . ? O6 Tb2 Tb1 154.25(14) 2_666 . ? N6 Tb2 Tb1 114.22(16) . . ? N5 Tb2 Tb1 108.25(15) . . ? O5 Tb2 Tb2 112.17(14) . 2_666 ? O1 Tb2 Tb2 104.29(13) . 2_666 ? O6 Tb2 Tb2 35.03(13) . 2_666 ? O3 Tb2 Tb2 136.80(13) . 2_666 ? O6 Tb2 Tb2 34.42(12) 2_666 2_666 ? N6 Tb2 Tb2 76.80(15) . 2_666 ? N5 Tb2 Tb2 118.33(15) . 2_666 ? Tb1 Tb2 Tb2 132.20(3) . 2_666 ? C7 N1 C8 117.5(7) . . ? C7 N1 Tb1 125.2(6) . . ? C8 N1 Tb1 115.5(5) . . ? C10 N2 C9 118.6(7) . . ? C10 N2 Tb1 128.4(6) . . ? C9 N2 Tb1 113.0(5) . . ? C23 N3 C24 119.7(7) . . ? C23 N3 Tb1 121.4(6) . . ? C24 N3 Tb1 117.2(5) . . ? C26 N4 C25 117.0(7) . . ? C26 N4 Tb1 127.4(6) . . ? C25 N4 Tb1 114.7(5) . . ? C39 N5 C40 115.7(7) . . ? C39 N5 Tb2 129.2(6) . . ? C40 N5 Tb2 115.1(5) . . ? C42 N6 C41 116.7(7) . . ? C42 N6 Tb2 125.7(6) . . ? C41 N6 Tb2 117.0(5) . . ? C1 O1 Tb2 131.7(5) . . ? C1 O1 Tb1 118.5(5) . . ? Tb2 O1 Tb1 109.7(2) . . ? C16 O2 Tb1 140.4(5) . . ? C17 O3 Tb2 130.0(5) . . ? C17 O3 Tb1 112.1(5) . . ? Tb2 O3 Tb1 109.0(2) . . ? C32 O4 Tb1 133.0(5) . . ? C33 O5 Tb2 144.5(5) . . ? C48 O6 Tb2 121.5(5) . . ? C48 O6 Tb2 120.7(4) . 2_666 ? Tb2 O6 Tb2 110.5(2) . 2_666 ? O1 C1 C2 121.6(8) . . ? O1 C1 C6 121.3(7) . . ? C2 C1 C6 117.1(8) . . ? C3 C2 C1 121.6(9) . . ? C3 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C2 C3 C4 120.9(9) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C5 C4 C3 119.0(9) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? C4 C5 C6 122.0(9) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 119.3(8) . . ? C5 C6 C7 118.6(8) . . ? C1 C6 C7 122.2(8) . . ? N1 C7 C6 124.1(8) . . ? N1 C7 H7A 117.9 . . ? C6 C7 H7A 117.9 . . ? N1 C8 C9 107.1(8) . . ? N1 C8 H8A 110.3 . . ? C9 C8 H8A 110.3 . . ? N1 C8 H8B 110.3 . . ? C9 C8 H8B 110.3 . . ? H8A C8 H8B 108.6 . . ? N2 C9 C8 109.0(7) . . ? N2 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? N2 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C11 129.3(8) . . ? N2 C10 H10A 115.3 . . ? C11 C10 H10A 115.3 . . ? C12 C11 C16 119.1(9) . . ? C12 C11 C10 118.0(9) . . ? C16 C11 C10 122.9(8) . . ? C13 C12 C11 122.4(10) . . ? C13 C12 H12A 118.8 . . ? C11 C12 H12A 118.8 . . ? C12 C13 C14 118.2(9) . . ? C12 C13 H13A 120.9 . . ? C14 C13 H13A 120.9 . . ? C15 C14 C13 121.4(9) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? C14 C15 C16 120.9(10) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? O2 C16 C11 122.7(8) . . ? O2 C16 C15 119.2(8) . . ? C11 C16 C15 118.1(8) . . ? O3 C17 C18 120.6(8) . . ? O3 C17 C22 121.0(7) . . ? C18 C17 C22 118.5(8) . . ? C19 C18 C17 121.2(9) . . ? C19 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? C18 C19 C20 120.2(9) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C21 C20 C19 118.1(9) . . ? C21 C20 H20A 121.0 . . ? C19 C20 H20A 121.0 . . ? C20 C21 C22 123.3(9) . . ? C20 C21 H21A 118.4 . . ? C22 C21 H21A 118.4 . . ? C21 C22 C17 118.7(8) . . ? C21 C22 C23 118.8(8) . . ? C17 C22 C23 122.4(8) . . ? N3 C23 C22 124.9(8) . . ? N3 C23 H23A 117.5 . . ? C22 C23 H23A 117.5 . . ? N3 C24 C25 109.0(7) . . ? N3 C24 H24A 109.9 . . ? C25 C24 H24A 109.9 . . ? N3 C24 H24B 109.9 . . ? C25 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? N4 C25 C24 107.9(7) . . ? N4 C25 H25A 110.1 . . ? C24 C25 H25A 110.1 . . ? N4 C25 H25B 110.1 . . ? C24 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? N4 C26 C27 126.8(8) . . ? N4 C26 H26A 116.6 . . ? C27 C26 H26A 116.6 . . ? C28 C27 C32 119.4(8) . . ? C28 C27 C26 117.3(8) . . ? C32 C27 C26 123.3(8) . . ? C29 C28 C27 121.5(9) . . ? C29 C28 H28A 119.2 . . ? C27 C28 H28A 119.2 . . ? C28 C29 C30 120.1(9) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C31 C30 C29 119.5(9) . . ? C31 C30 H30A 120.2 . . ? C29 C30 H30A 120.2 . . ? C30 C31 C32 122.6(8) . . ? C30 C31 H31A 118.7 . . ? C32 C31 H31A 118.7 . . ? O4 C32 C31 121.4(8) . . ? O4 C32 C27 121.8(8) . . ? C31 C32 C27 116.9(8) . . ? O5 C33 C34 121.5(8) . . ? O5 C33 C38 121.0(8) . . ? C34 C33 C38 117.5(8) . . ? C35 C34 C33 121.6(9) . . ? C35 C34 H34A 119.2 . . ? C33 C34 H34A 119.2 . . ? C34 C35 C36 121.4(9) . . ? C34 C35 H35A 119.3 . . ? C36 C35 H35A 119.3 . . ? C35 C36 C37 119.2(9) . . ? C35 C36 H36A 120.4 . . ? C37 C36 H36A 120.4 . . ? C36 C37 C38 121.2(9) . . ? C36 C37 H37A 119.4 . . ? C38 C37 H37A 119.4 . . ? C37 C38 C33 119.1(8) . . ? C37 C38 C39 116.1(8) . . ? C33 C38 C39 124.8(8) . . ? N5 C39 C38 127.0(8) . . ? N5 C39 H39A 116.5 . . ? C38 C39 H39A 116.5 . . ? N5 C40 C41 109.6(7) . . ? N5 C40 H40A 109.8 . . ? C41 C40 H40A 109.8 . . ? N5 C40 H40B 109.8 . . ? C41 C40 H40B 109.8 . . ? H40A C40 H40B 108.2 . . ? N6 C41 C40 109.5(7) . . ? N6 C41 H41A 109.8 . . ? C40 C41 H41A 109.8 . . ? N6 C41 H41B 109.8 . . ? C40 C41 H41B 109.8 . . ? H41A C41 H41B 108.2 . . ? N6 C42 C43 125.1(8) . . ? N6 C42 H42A 117.4 . . ? C43 C42 H42A 117.4 . . ? C44 C43 C48 119.0(8) . . ? C44 C43 C42 117.7(8) . . ? C48 C43 C42 123.3(7) . . ? C45 C44 C43 121.7(8) . . ? C45 C44 H44A 119.1 . . ? C43 C44 H44A 119.1 . . ? C44 C45 C46 118.5(8) . . ? C44 C45 H45A 120.8 . . ? C46 C45 H45A 120.8 . . ? C47 C46 C45 121.3(8) . . ? C47 C46 H46A 119.3 . . ? C45 C46 H46A 119.3 . . ? C46 C47 C48 120.8(8) . . ? C46 C47 H47A 119.6 . . ? C48 C47 H47A 119.6 . . ? O6 C48 C47 119.7(7) . . ? O6 C48 C43 121.6(7) . . ? C47 C48 C43 118.7(7) . . ? O7 C49 H49A 109.5 . . ? O7 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O7 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C49 O7 H7B 109.5 . . ? O8 C50 H50A 109.5 . . ? O8 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O8 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C50 O8 H8C 109.5 . . ? O9 C51 H51A 109.5 . . ? O9 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O9 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C51 O9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.741 _refine_diff_density_min -1.696 _refine_diff_density_rms 0.307 data_complex-2 _database_code_depnum_ccdc_archive 'CCDC 680103' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H52 N8 O14 Tb2' _chemical_formula_weight 1306.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 12.267(3) _cell_length_b 10.542(2) _cell_length_c 20.449(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.33(3) _cell_angle_gamma 90.00 _cell_volume 2573.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 2.800 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.6327 _exptl_absorpt_correction_T_max 0.8500 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7747 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4448 _reflns_number_gt 3165 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and Rfactors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+1.2517P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0066(2) _refine_ls_number_reflns 4448 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.666921(16) 0.74888(2) 0.216313(10) 0.02465(10) Uani 1 1 d . . . N1 N 0.7481(4) 0.9605(4) 0.2336(2) 0.0422(11) Uani 1 1 d . . . N2 N 0.5651(4) 0.9003(4) 0.1291(2) 0.0459(12) Uani 1 1 d . . . O1 O 0.8269(3) 0.7275(3) 0.28710(18) 0.0454(11) Uani 1 1 d . . . O2 O 0.5191(3) 0.6483(3) 0.15941(18) 0.0439(9) Uani 1 1 d . . . O3 O 0.5207(3) 0.8636(3) 0.25589(19) 0.0466(9) Uani 1 1 d . . . N3 N 0.5235(4) 0.7960(5) 0.3076(2) 0.0403(11) Uani 1 1 d . . . O4 O 0.6001(3) 0.7138(4) 0.32131(19) 0.0470(10) Uani 1 1 d . . . O5 O 0.4552(3) 0.8117(4) 0.34270(19) 0.0501(10) Uani 1 1 d . . . C1 C 0.9223(4) 0.7834(5) 0.3085(3) 0.0387(13) Uani 1 1 d . . . C2 C 1.0153(4) 0.7172(6) 0.3431(3) 0.0438(15) Uani 1 1 d . . . H2A H 1.0074 0.6311 0.3509 0.053 Uiso 1 1 calc R . . C3 C 1.1188(5) 0.7719(6) 0.3666(3) 0.0500(16) Uani 1 1 d . . . H3A H 1.1796 0.7227 0.3879 0.060 Uiso 1 1 calc R . . C4 C 1.1318(5) 0.9017(7) 0.3581(3) 0.0606(17) Uani 1 1 d . . . H4A H 1.2007 0.9402 0.3749 0.073 Uiso 1 1 calc R . . C5 C 1.0422(5) 0.9721(6) 0.3248(3) 0.0542(16) Uani 1 1 d . . . H5A H 1.0514 1.0585 0.3184 0.065 Uiso 1 1 calc R . . C6 C 0.9368(4) 0.9161(5) 0.3000(3) 0.0407(13) Uani 1 1 d . . . C7 C 0.8469(5) 0.9966(5) 0.2651(3) 0.0446(14) Uani 1 1 d . . . H7A H 0.8616 1.0831 0.2653 0.053 Uiso 1 1 calc R . . C8 C 0.6733(4) 1.0618(5) 0.1998(3) 0.0458(14) Uani 1 1 d . . . H8A H 0.7148 1.1403 0.2005 0.055 Uiso 1 1 calc R . . H8B H 0.6133 1.0758 0.2227 0.055 Uiso 1 1 calc R . . C9 C 0.6253(5) 1.0200(5) 0.1277(3) 0.0506(15) Uani 1 1 d . . . H9A H 0.5746 1.0842 0.1039 0.061 Uiso 1 1 calc R . . H9B H 0.6853 1.0083 0.1045 0.061 Uiso 1 1 calc R . . C10 C 0.4646(5) 0.8931(6) 0.0932(3) 0.0484(15) Uani 1 1 d . . . H10A H 0.4376 0.9638 0.0673 0.058 Uiso 1 1 calc R . . C11 C 0.3888(4) 0.7863(6) 0.0887(3) 0.0410(13) Uani 1 1 d . . . C12 C 0.2811(5) 0.8015(7) 0.0476(3) 0.0551(16) Uani 1 1 d . . . H12A H 0.2632 0.8769 0.0239 0.066 Uiso 1 1 calc R . . C13 C 0.2009(5) 0.7074(7) 0.0414(3) 0.0624(18) Uani 1 1 d . . . H13A H 0.1307 0.7181 0.0128 0.075 Uiso 1 1 calc R . . C14 C 0.2267(5) 0.5960(7) 0.0788(3) 0.0570(17) Uani 1 1 d . . . H14A H 0.1727 0.5331 0.0763 0.068 Uiso 1 1 calc R . . C15 C 0.3324(4) 0.5791(6) 0.1195(3) 0.0434(13) Uani 1 1 d . . . H15A H 0.3484 0.5047 0.1443 0.052 Uiso 1 1 calc R . . C16 C 0.4169(4) 0.6722(5) 0.1244(3) 0.0407(13) Uani 1 1 d . . . N1' N 0.5933(3) 0.6396(4) 0.0209(2) 0.0396(10) Uani 1 1 d . . . O1' O 0.7420(3) 0.7156(3) 0.12991(18) 0.0402(9) Uani 1 1 d . . . H1'B H 0.7224 0.6334 0.1153 0.048 Uiso 1 1 calc R . . C1' C 0.8016(4) 0.7605(4) 0.0906(3) 0.0342(12) Uani 1 1 d . . . C2' C 0.9054(4) 0.8200(5) 0.1155(3) 0.0428(13) Uani 1 1 d . . . H2'A H 0.9319 0.8284 0.1618 0.051 Uiso 1 1 calc R . . C3' C 0.9678(5) 0.8657(5) 0.0740(3) 0.0474(14) Uani 1 1 d . . . H3'A H 1.0365 0.9037 0.0923 0.057 Uiso 1 1 calc R . . C4' C 0.9305(5) 0.8565(6) 0.0033(3) 0.0493(15) Uani 1 1 d . . . H4'A H 0.9737 0.8895 -0.0245 0.059 Uiso 1 1 calc R . . C5' C 0.8316(5) 0.7996(6) -0.0234(3) 0.0448(14) Uani 1 1 d . . . H5'A H 0.8072 0.7917 -0.0698 0.054 Uiso 1 1 calc R . . C6' C 0.7645(4) 0.7515(5) 0.0193(3) 0.0373(12) Uani 1 1 d . . . C7' C 0.6626(4) 0.6891(6) -0.0110(3) 0.0427(13) Uani 1 1 d . . . H7'A H 0.6442 0.6833 -0.0576 0.051 Uiso 1 1 calc R . . C8' C 0.4946(4) 0.5677(5) -0.0130(3) 0.0425(13) Uani 1 1 d . . . H8'B H 0.4886 0.5681 -0.0612 0.064 Uiso 1 1 calc R . . H8'C H 0.4276 0.6064 -0.0043 0.064 Uiso 1 1 calc R . . C17 C 0.7531(5) 0.4521(6) 0.2875(3) 0.0525(15) Uani 1 1 d . . . H17A H 0.7361 0.3641 0.2783 0.079 Uiso 1 1 calc R . . H17B H 0.7378 0.4742 0.3301 0.079 Uiso 1 1 calc R . . H17C H 0.8309 0.4670 0.2890 0.079 Uiso 1 1 calc R . . O6 O 0.6853(3) 0.5283(3) 0.23555(18) 0.0412(9) Uani 1 1 d . . . H6C H 0.6265 0.4910 0.2196 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02969(15) 0.02470(16) 0.01816(14) 0.00106(10) 0.00266(10) 0.00143(10) N1 0.060(3) 0.033(3) 0.034(2) 0.000(2) 0.011(2) 0.003(2) N2 0.061(3) 0.040(3) 0.034(2) 0.001(2) 0.005(2) 0.006(2) O1 0.039(2) 0.040(3) 0.050(3) 0.0048(17) -0.0055(19) -0.0044(16) O2 0.041(2) 0.041(2) 0.044(2) 0.0008(18) -0.0021(17) 0.0014(17) O3 0.056(2) 0.042(2) 0.042(2) 0.0077(19) 0.0115(18) 0.0079(18) N3 0.044(3) 0.041(3) 0.036(3) -0.009(2) 0.009(2) -0.002(2) O4 0.053(2) 0.051(2) 0.038(2) 0.0044(19) 0.0110(18) 0.0163(19) O5 0.050(2) 0.053(3) 0.051(2) -0.014(2) 0.0204(19) -0.002(2) C1 0.037(3) 0.051(4) 0.025(3) -0.004(2) 0.000(2) -0.001(2) C2 0.037(3) 0.058(4) 0.029(3) 0.011(3) -0.007(2) -0.018(3) C3 0.044(3) 0.069(5) 0.035(3) -0.005(3) 0.005(3) 0.001(3) C4 0.046(4) 0.068(5) 0.064(4) -0.001(4) 0.004(3) -0.016(3) C5 0.059(4) 0.042(4) 0.058(4) -0.004(3) 0.005(3) -0.011(3) C6 0.051(3) 0.036(3) 0.034(3) 0.003(3) 0.009(2) -0.004(3) C7 0.059(4) 0.037(3) 0.038(3) -0.006(3) 0.012(3) -0.009(3) C8 0.059(3) 0.034(3) 0.046(3) 0.002(3) 0.014(3) 0.001(3) C9 0.073(4) 0.032(3) 0.044(3) 0.003(3) 0.008(3) 0.003(3) C10 0.062(4) 0.050(4) 0.032(3) 0.006(3) 0.008(3) 0.019(3) C11 0.041(3) 0.048(4) 0.034(3) -0.002(3) 0.007(2) 0.003(3) C12 0.058(4) 0.064(4) 0.041(3) -0.001(3) 0.007(3) 0.019(3) C13 0.039(3) 0.094(5) 0.048(4) 0.001(4) -0.003(3) 0.012(3) C14 0.039(3) 0.085(5) 0.046(4) 0.005(4) 0.007(3) 0.005(3) C15 0.044(3) 0.050(4) 0.037(3) 0.003(3) 0.010(2) 0.005(3) C16 0.044(3) 0.045(4) 0.031(3) -0.004(3) 0.004(2) 0.009(3) N1' 0.042(2) 0.040(3) 0.036(2) -0.003(2) 0.008(2) -0.007(2) O1' 0.049(2) 0.034(2) 0.039(2) -0.0001(17) 0.0143(18) -0.0035(16) C1' 0.041(3) 0.030(3) 0.033(3) 0.003(2) 0.011(2) 0.005(2) C2' 0.047(3) 0.040(4) 0.041(3) -0.002(3) 0.008(3) 0.000(3) C3' 0.047(3) 0.044(4) 0.051(4) -0.002(3) 0.011(3) -0.010(3) C4' 0.054(3) 0.052(4) 0.044(3) 0.003(3) 0.013(3) -0.014(3) C5' 0.052(3) 0.050(3) 0.034(3) 0.000(3) 0.014(3) -0.007(3) C6' 0.043(3) 0.034(3) 0.033(3) 0.000(2) 0.006(2) 0.003(2) C7' 0.052(3) 0.038(3) 0.035(3) 0.004(3) 0.004(2) -0.006(3) C8' 0.049(3) 0.044(3) 0.034(3) -0.002(3) 0.008(2) -0.008(3) C17 0.054(4) 0.044(4) 0.054(4) 0.014(3) 0.003(3) 0.005(3) O6 0.042(2) 0.031(2) 0.045(2) 0.0042(17) -0.0008(16) -0.0008(16) _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 Tb1 O1 2.165(3) . ? Tb1 O2 2.190(3) . ? Tb1 O1' 2.201(4) . ? Tb1 O6 2.360(3) . ? Tb1 N1 2.435(5) . ? Tb1 O3 2.450(4) . ? Tb1 O4 2.496(4) . ? Tb1 N2 2.502(4) . ? Tb1 N3 2.887(5) . ? N1 C7 1.292(6) . ? N1 C8 1.472(7) . ? N2 C10 1.283(7) . ? N2 C9 1.467(7) . ? O1 C1 1.293(6) . ? O2 C16 1.316(6) . ? O3 N3 1.268(5) . ? N3 O5 1.235(5) . ? N3 O4 1.261(6) . ? C1 C2 1.385(8) . ? C1 C6 1.426(7) . ? C2 C3 1.377(8) . ? C2 H2A 0.9300 . ? C3 C4 1.392(8) . ? C3 H3A 0.9300 . ? C4 C5 1.370(8) . ? C4 H4A 0.9300 . ? C5 C6 1.406(7) . ? C5 H5A 0.9300 . ? C6 C7 1.442(7) . ? C7 H7A 0.9300 . ? C8 C9 1.522(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.449(8) . ? C10 H10A 0.9300 . ? C11 C12 1.402(8) . ? C11 C16 1.408(8) . ? C12 C13 1.383(10) . ? C12 H12A 0.9300 . ? C13 C14 1.398(9) . ? C13 H13A 0.9300 . ? C14 C15 1.381(7) . ? C14 H14A 0.9300 . ? C15 C16 1.414(7) . ? C15 H15A 0.9300 . ? N1' C7' 1.293(6) . ? N1' C8' 1.460(6) . ? O1' C1' 1.295(6) . ? O1' H1'B 0.9300 . ? C1' C2' 1.405(7) . ? C1' C6' 1.426(7) . ? C2' C3' 1.357(7) . ? C2' H2'A 0.9300 . ? C3' C4' 1.414(7) . ? C3' H3'A 0.9300 . ? C4' C5' 1.351(7) . ? C4' H4'A 0.9300 . ? C5' C6' 1.424(7) . ? C5' H5'A 0.9300 . ? C6' C7' 1.422(7) . ? C7' H7'A 0.9300 . ? C8' C8' 1.519(10) 3_665 ? C8' H8'B 0.9700 . ? C8' H8'C 0.9700 . ? C17 O6 1.435(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? O6 H6C 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O2 144.77(13) . . ? O1 Tb1 O1' 92.15(14) . . ? O2 Tb1 O1' 86.84(14) . . ? O1 Tb1 O6 75.46(13) . . ? O2 Tb1 O6 69.33(12) . . ? O1' Tb1 O6 86.28(13) . . ? O1 Tb1 N1 73.82(14) . . ? O2 Tb1 N1 141.40(14) . . ? O1' Tb1 N1 91.72(14) . . ? O6 Tb1 N1 149.11(14) . . ? O1 Tb1 O3 116.76(13) . . ? O2 Tb1 O3 80.50(13) . . ? O1' Tb1 O3 144.85(13) . . ? O6 Tb1 O3 118.69(12) . . ? N1 Tb1 O3 78.80(14) . . ? O1 Tb1 O4 80.56(14) . . ? O2 Tb1 O4 89.40(14) . . ? O1' Tb1 O4 161.47(14) . . ? O6 Tb1 O4 75.42(12) . . ? N1 Tb1 O4 102.42(14) . . ? O3 Tb1 O4 51.57(12) . . ? O1 Tb1 N2 140.33(15) . . ? O2 Tb1 N2 73.37(15) . . ? O1' Tb1 N2 76.25(14) . . ? O6 Tb1 N2 139.46(13) . . ? N1 Tb1 N2 68.86(15) . . ? O3 Tb1 N2 68.73(14) . . ? O4 Tb1 N2 119.90(14) . . ? O1 Tb1 N3 100.32(14) . . ? O2 Tb1 N3 82.72(13) . . ? O1' Tb1 N3 167.52(13) . . ? O6 Tb1 N3 96.35(13) . . ? N1 Tb1 N3 92.19(14) . . ? O3 Tb1 N3 25.87(12) . . ? O4 Tb1 N3 25.81(12) . . ? N2 Tb1 N3 94.15(14) . . ? C7 N1 C8 115.6(5) . . ? C7 N1 Tb1 130.3(4) . . ? C8 N1 Tb1 114.0(3) . . ? C10 N2 C9 117.5(5) . . ? C10 N2 Tb1 128.8(4) . . ? C9 N2 Tb1 113.1(3) . . ? C1 O1 Tb1 142.0(3) . . ? C16 O2 Tb1 139.8(3) . . ? N3 O3 Tb1 96.7(3) . . ? O5 N3 O4 122.3(5) . . ? O5 N3 O3 121.2(5) . . ? O4 N3 O3 116.6(4) . . ? O5 N3 Tb1 174.8(3) . . ? O4 N3 Tb1 59.5(2) . . ? O3 N3 Tb1 57.4(2) . . ? N3 O4 Tb1 94.7(3) . . ? O1 C1 C2 121.2(5) . . ? O1 C1 C6 122.3(5) . . ? C2 C1 C6 116.5(5) . . ? C3 C2 C1 123.5(6) . . ? C3 C2 H2A 118.3 . . ? C1 C2 H2A 118.3 . . ? C2 C3 C4 119.4(6) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 119.6(6) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 121.1(6) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C5 C6 C1 119.9(5) . . ? C5 C6 C7 117.8(5) . . ? C1 C6 C7 122.3(5) . . ? N1 C7 C6 126.6(5) . . ? N1 C7 H7A 116.7 . . ? C6 C7 H7A 116.7 . . ? N1 C8 C9 107.8(4) . . ? N1 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? N1 C8 H8B 110.2 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? N2 C9 C8 108.3(5) . . ? N2 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? N2 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? N2 C10 C11 126.9(5) . . ? N2 C10 H10A 116.6 . . ? C11 C10 H10A 116.6 . . ? C12 C11 C16 119.6(6) . . ? C12 C11 C10 116.8(6) . . ? C16 C11 C10 123.6(5) . . ? C13 C12 C11 121.7(6) . . ? C13 C12 H12A 119.2 . . ? C11 C12 H12A 119.2 . . ? C12 C13 C14 119.1(6) . . ? C12 C13 H13A 120.4 . . ? C14 C13 H13A 120.4 . . ? C15 C14 C13 120.0(6) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C16 121.7(6) . . ? C14 C15 H15A 119.2 . . ? C16 C15 H15A 119.2 . . ? O2 C16 C11 122.3(5) . . ? O2 C16 C15 119.8(5) . . ? C11 C16 C15 117.9(5) . . ? C7' N1' C8' 122.7(4) . . ? C1' O1' Tb1 147.3(3) . . ? C1' O1' H1'B 106.4 . . ? Tb1 O1' H1'B 106.4 . . ? O1' C1' C2' 122.1(5) . . ? O1' C1' C6' 121.2(5) . . ? C2' C1' C6' 116.8(5) . . ? C3' C2' C1' 121.7(5) . . ? C3' C2' H2'A 119.2 . . ? C1' C2' H2'A 119.2 . . ? C2' C3' C4' 121.3(5) . . ? C2' C3' H3'A 119.4 . . ? C4' C3' H3'A 119.4 . . ? C5' C4' C3' 119.5(5) . . ? C5' C4' H4'A 120.2 . . ? C3' C4' H4'A 120.2 . . ? C4' C5' C6' 120.1(5) . . ? C4' C5' H5'A 120.0 . . ? C6' C5' H5'A 120.0 . . ? C7' C6' C5' 118.1(5) . . ? C7' C6' C1' 121.1(5) . . ? C5' C6' C1' 120.7(5) . . ? N1' C7' C6' 125.5(5) . . ? N1' C7' H7'A 117.2 . . ? C6' C7' H7'A 117.2 . . ? N1' C8' C8' 109.0(5) . 3_665 ? N1' C8' H8'B 109.9 . . ? C8' C8' H8'B 109.9 3_665 . ? N1' C8' H8'C 109.9 . . ? C8' C8' H8'C 109.9 3_665 . ? H8'B C8' H8'C 108.3 . . ? O6 C17 H17A 109.5 . . ? O6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C17 O6 Tb1 133.8(3) . . ? C17 O6 H6C 109.5 . . ? Tb1 O6 H6C 111.4 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.948 _refine_diff_density_min -1.136 _refine_diff_density_rms 0.099 data_complex-3 _database_code_depnum_ccdc_archive 'CCDC 680104' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H52 Cl2 N6 O8 Tb2' _chemical_formula_weight 1253.72 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.122(3) _cell_length_b 10.038(2) _cell_length_c 19.478(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.71(3) _cell_angle_gamma 90.00 _cell_volume 2492.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 2.980 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.6471 _exptl_absorpt_correction_T_max 0.8185 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7324 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4399 _reflns_number_gt 3796 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and Rfactors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+1.2517P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0049(2) _refine_ls_number_reflns 4399 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.655316(16) 0.808861(19) 0.211423(10) 0.01773(10) Uani 1 1 d . . . Cl1 Cl 0.54177(9) 0.87155(12) 0.30270(6) 0.0304(3) Uani 1 1 d . . . N1 N 0.7447(3) 1.0234(4) 0.2455(2) 0.0298(9) Uani 1 1 d . . . N2 N 0.5681(3) 0.9925(4) 0.1341(2) 0.0261(9) Uani 1 1 d . . . O1 O 0.8105(3) 0.7613(4) 0.27784(18) 0.0335(8) Uani 1 1 d . . . O2 O 0.5128(3) 0.7188(3) 0.14043(17) 0.0290(7) Uani 1 1 d . . . O1' O 0.7206(3) 0.7745(4) 0.11838(17) 0.0331(8) Uani 1 1 d . . . H1L H 0.6752 0.7204 0.1005 0.050 Uiso 1 1 calc R . . N1' N 0.5949(3) 0.6410(4) 0.0132(2) 0.0268(9) Uani 1 1 d . . . C1 C 0.9038(4) 0.8114(5) 0.3008(3) 0.0288(11) Uani 1 1 d . . . C2 C 0.9913(4) 0.7278(6) 0.3230(3) 0.0366(12) Uani 1 1 d . . . H2A H 0.9821 0.6359 0.3204 0.044 Uiso 1 1 calc R . . C3 C 1.0903(5) 0.7786(7) 0.3486(3) 0.0501(16) Uani 1 1 d . . . H3A H 1.1473 0.7213 0.3621 0.060 Uiso 1 1 calc R . . C4 C 1.1054(5) 0.9159(8) 0.3543(3) 0.0585(18) Uani 1 1 d . . . H4A H 1.1721 0.9497 0.3733 0.070 Uiso 1 1 calc R . . C5 C 1.0241(4) 1.0002(6) 0.3325(3) 0.0465(14) Uani 1 1 d . . . H5A H 1.0354 1.0917 0.3358 0.056 Uiso 1 1 calc R . . C6 C 0.9229(4) 0.9509(5) 0.3050(3) 0.0321(11) Uani 1 1 d . . . C7 C 0.8406(4) 1.0471(5) 0.2791(2) 0.0331(12) Uani 1 1 d . . . H7A H 0.8587 1.1363 0.2876 0.040 Uiso 1 1 calc R . . C8 C 0.6770(4) 1.1379(5) 0.2195(3) 0.0326(12) Uani 1 1 d . . . H8A H 0.7180 1.2192 0.2262 0.039 Uiso 1 1 calc R . . H8B H 0.6228 1.1457 0.2456 0.039 Uiso 1 1 calc R . . C9 C 0.6276(4) 1.1174(5) 0.1420(3) 0.0333(12) Uani 1 1 d . . . H9A H 0.5813 1.1912 0.1239 0.040 Uiso 1 1 calc R . . H9B H 0.6816 1.1128 0.1156 0.040 Uiso 1 1 calc R . . C10 C 0.4797(4) 0.9943(5) 0.0894(3) 0.0301(11) Uani 1 1 d . . . H10A H 0.4626 1.0725 0.0636 0.036 Uiso 1 1 calc R . . C11 C 0.4033(4) 0.8883(5) 0.0746(2) 0.0309(11) Uani 1 1 d . . . C12 C 0.3045(4) 0.9210(6) 0.0326(3) 0.0413(13) Uani 1 1 d . . . H12A H 0.2944 1.0046 0.0114 0.050 Uiso 1 1 calc R . . C13 C 0.2216(4) 0.8326(6) 0.0218(3) 0.0443(14) Uani 1 1 d . . . H13A H 0.1567 0.8561 -0.0067 0.053 Uiso 1 1 calc R . . C14 C 0.2360(4) 0.7084(6) 0.0537(3) 0.0414(14) Uani 1 1 d . . . H14A H 0.1803 0.6488 0.0475 0.050 Uiso 1 1 calc R . . C15 C 0.3340(4) 0.6731(5) 0.0951(3) 0.0318(12) Uani 1 1 d . . . H15A H 0.3423 0.5901 0.1169 0.038 Uiso 1 1 calc R . . C16 C 0.4208(4) 0.7588(5) 0.1050(2) 0.0268(10) Uani 1 1 d . . . C1' C 0.7895(4) 0.7822(5) 0.0807(2) 0.0249(10) Uani 1 1 d . . . C2' C 0.8863(4) 0.8492(5) 0.1050(3) 0.0339(12) Uani 1 1 d . . . H2'A H 0.9025 0.8882 0.1496 0.041 Uiso 1 1 calc R . . C3' C 0.9560(5) 0.8568(7) 0.0629(3) 0.0499(16) Uani 1 1 d . . . H3'A H 1.0191 0.9017 0.0795 0.060 Uiso 1 1 calc R . . C4' C 0.9357(5) 0.7992(7) -0.0045(3) 0.060(2) Uani 1 1 d . . . H4'A H 0.9846 0.8050 -0.0320 0.072 Uiso 1 1 calc R . . C5' C 0.8433(5) 0.7349(7) -0.0289(3) 0.0482(15) Uani 1 1 d . . . H5'A H 0.8289 0.6974 -0.0738 0.058 Uiso 1 1 calc R . . C6' C 0.7688(4) 0.7237(5) 0.0122(3) 0.0309(11) Uani 1 1 d . . . C7' C 0.6727(4) 0.6566(5) -0.0173(3) 0.0302(11) Uani 1 1 d . . . H7'A H 0.6647 0.6207 -0.0622 0.036 Uiso 1 1 calc R . . C8' C 0.5006(4) 0.5658(5) -0.0200(2) 0.0279(10) Uani 1 1 d . . . H8'A H 0.5002 0.5477 -0.0690 0.042 Uiso 1 1 calc R . . H8'B H 0.4386 0.6176 -0.0188 0.042 Uiso 1 1 calc R . . O3 O 0.6466(3) 0.5815(3) 0.2403(2) 0.0372(8) Uani 1 1 d . . . H3B H 0.5879 0.5795 0.2481 0.045 Uiso 1 1 calc R . . C17 C 0.7162(5) 0.4986(6) 0.2906(3) 0.0474(15) Uani 1 1 d . . . H17A H 0.6874 0.4106 0.2894 0.071 Uiso 1 1 calc R . . H17B H 0.7247 0.5354 0.3371 0.071 Uiso 1 1 calc R . . H17C H 0.7832 0.4946 0.2788 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01850(15) 0.01765(14) 0.01734(14) -0.00125(8) 0.00485(9) 0.00048(8) Cl1 0.0325(7) 0.0325(6) 0.0292(6) -0.0032(5) 0.0129(5) 0.0013(5) N1 0.037(3) 0.024(2) 0.030(2) -0.0031(18) 0.0108(19) -0.0032(18) N2 0.026(2) 0.026(2) 0.026(2) 0.0013(17) 0.0075(18) -0.0006(17) O1 0.0253(19) 0.0336(19) 0.039(2) -0.0005(17) 0.0017(15) -0.0025(17) O2 0.0253(19) 0.0291(17) 0.0308(18) -0.0025(15) 0.0031(15) -0.0005(15) O1' 0.033(2) 0.0386(19) 0.0306(18) -0.0105(16) 0.0138(16) -0.0068(16) N1' 0.027(2) 0.028(2) 0.026(2) -0.0014(18) 0.0063(17) -0.0053(18) C1 0.028(3) 0.040(3) 0.019(2) -0.001(2) 0.006(2) 0.003(2) C2 0.031(3) 0.045(3) 0.031(3) 0.000(2) 0.002(2) 0.006(3) C3 0.028(3) 0.081(5) 0.041(3) 0.000(3) 0.008(3) 0.016(3) C4 0.035(4) 0.080(5) 0.054(4) -0.003(4) -0.003(3) -0.008(3) C5 0.032(3) 0.051(4) 0.051(3) -0.002(3) 0.000(3) -0.012(3) C6 0.028(3) 0.039(3) 0.028(3) -0.001(2) 0.004(2) -0.002(2) C7 0.036(3) 0.032(3) 0.031(3) -0.005(2) 0.008(2) -0.010(2) C8 0.039(3) 0.024(3) 0.036(3) -0.001(2) 0.012(2) 0.002(2) C9 0.037(3) 0.026(3) 0.038(3) 0.005(2) 0.009(2) -0.001(2) C10 0.031(3) 0.028(3) 0.030(3) 0.007(2) 0.006(2) 0.004(2) C11 0.030(3) 0.036(3) 0.026(2) 0.003(2) 0.005(2) 0.001(2) C12 0.033(3) 0.050(3) 0.036(3) 0.007(3) 0.000(2) 0.005(3) C13 0.025(3) 0.064(4) 0.038(3) -0.001(3) -0.004(2) 0.006(3) C14 0.025(3) 0.057(4) 0.042(3) -0.008(3) 0.008(3) -0.005(3) C15 0.033(3) 0.035(3) 0.029(3) -0.003(2) 0.010(2) -0.003(2) C16 0.022(3) 0.035(3) 0.024(2) -0.005(2) 0.007(2) -0.001(2) C1' 0.025(3) 0.025(2) 0.026(2) 0.003(2) 0.009(2) 0.003(2) C2' 0.035(3) 0.037(3) 0.030(3) -0.002(2) 0.007(2) -0.006(2) C3' 0.034(3) 0.072(4) 0.043(3) -0.007(3) 0.009(3) -0.022(3) C4' 0.041(4) 0.105(6) 0.041(3) -0.017(3) 0.022(3) -0.032(4) C5' 0.046(4) 0.072(4) 0.032(3) -0.015(3) 0.021(3) -0.016(3) C6' 0.028(3) 0.040(3) 0.026(3) -0.002(2) 0.009(2) -0.004(2) C7' 0.038(3) 0.030(3) 0.023(2) -0.002(2) 0.010(2) -0.002(2) C8' 0.028(3) 0.033(3) 0.022(2) -0.003(2) 0.006(2) -0.006(2) O3 0.0261(19) 0.0226(17) 0.058(2) 0.0105(17) 0.0006(17) 0.0004(15) C17 0.052(4) 0.038(3) 0.050(4) 0.012(3) 0.009(3) 0.002(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 Tb1 O1 2.191(4) . ? Tb1 O1' 2.207(3) . ? Tb1 O2 2.237(3) . ? Tb1 O3 2.360(3) . ? Tb1 N1 2.467(4) . ? Tb1 N2 2.482(4) . ? Tb1 Cl1 2.6518(13) . ? N1 C7 1.296(6) . ? N1 C8 1.467(6) . ? N2 C10 1.274(6) . ? N2 C9 1.465(6) . ? O1 C1 1.301(7) . ? O2 C16 1.304(6) . ? O1' C1' 1.295(6) . ? O1' H1L 0.8200 . ? N1' C7' 1.307(6) . ? N1' C8' 1.463(6) . ? C1 C2 1.406(7) . ? C1 C6 1.421(7) . ? C2 C3 1.374(8) . ? C2 H2A 0.9300 . ? C3 C4 1.393(10) . ? C3 H3A 0.9300 . ? C4 C5 1.349(9) . ? C4 H4A 0.9300 . ? C5 C6 1.399(7) . ? C5 H5A 0.9300 . ? C6 C7 1.448(7) . ? C7 H7A 0.9300 . ? C8 C9 1.510(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.444(7) . ? C10 H10A 0.9300 . ? C11 C12 1.398(7) . ? C11 C16 1.424(7) . ? C12 C13 1.382(8) . ? C12 H12A 0.9300 . ? C13 C14 1.386(8) . ? C13 H13A 0.9300 . ? C14 C15 1.393(8) . ? C14 H14A 0.9300 . ? C15 C16 1.403(7) . ? C15 H15A 0.9300 . ? C1' C2' 1.417(7) . ? C1' C6' 1.424(7) . ? C2' C3' 1.368(8) . ? C2' H2'A 0.9300 . ? C3' C4' 1.400(8) . ? C3' H3'A 0.9300 . ? C4' C5' 1.356(8) . ? C4' H4'A 0.9300 . ? C5' C6' 1.406(7) . ? C5' H5'A 0.9300 . ? C6' C7' 1.424(7) . ? C7' H7'A 0.9300 . ? C8' C8' 1.536(9) 3_665 ? C8' H8'A 0.9700 . ? C8' H8'B 0.9700 . ? O3 C17 1.436(6) . ? O3 H3B 0.8200 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O1' 87.92(13) . . ? O1 Tb1 O2 143.23(13) . . ? O1' Tb1 O2 81.93(13) . . ? O1 Tb1 O3 74.88(12) . . ? O1' Tb1 O3 95.47(13) . . ? O2 Tb1 O3 71.08(12) . . ? O1 Tb1 N1 73.47(14) . . ? O1' Tb1 N1 96.03(13) . . ? O2 Tb1 N1 142.55(13) . . ? O3 Tb1 N1 145.79(13) . . ? O1 Tb1 N2 138.66(13) . . ? O1' Tb1 N2 80.26(13) . . ? O2 Tb1 N2 74.18(12) . . ? O3 Tb1 N2 145.25(12) . . ? N1 Tb1 N2 68.66(13) . . ? O1 Tb1 Cl1 104.31(10) . . ? O1' Tb1 Cl1 167.53(10) . . ? O2 Tb1 Cl1 89.42(9) . . ? O3 Tb1 Cl1 90.15(10) . . ? N1 Tb1 Cl1 85.37(9) . . ? N2 Tb1 Cl1 88.78(9) . . ? C7 N1 C8 117.8(4) . . ? C7 N1 Tb1 129.7(3) . . ? C8 N1 Tb1 112.4(3) . . ? C10 N2 C9 115.8(4) . . ? C10 N2 Tb1 129.7(3) . . ? C9 N2 Tb1 114.5(3) . . ? C1 O1 Tb1 141.8(3) . . ? C16 O2 Tb1 137.4(3) . . ? C1' O1' Tb1 156.2(3) . . ? C1' O1' H1L 109.5 . . ? Tb1 O1' H1L 93.9 . . ? C7' N1' C8' 122.1(4) . . ? O1 C1 C2 120.6(5) . . ? O1 C1 C6 122.7(5) . . ? C2 C1 C6 116.7(5) . . ? C3 C2 C1 121.5(6) . . ? C3 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C2 C3 C4 120.0(6) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 120.6(6) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C4 C5 C6 120.4(6) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 120.6(5) . . ? C5 C6 C7 117.4(5) . . ? C1 C6 C7 122.0(5) . . ? N1 C7 C6 127.5(5) . . ? N1 C7 H7A 116.3 . . ? C6 C7 H7A 116.3 . . ? N1 C8 C9 108.6(4) . . ? N1 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? N1 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 108.3 . . ? N2 C9 C8 108.2(4) . . ? N2 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? N2 C9 H9B 110.1 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? N2 C10 C11 127.1(5) . . ? N2 C10 H10A 116.5 . . ? C11 C10 H10A 116.5 . . ? C12 C11 C16 119.5(5) . . ? C12 C11 C10 116.6(5) . . ? C16 C11 C10 123.6(4) . . ? C13 C12 C11 121.7(5) . . ? C13 C12 H12A 119.1 . . ? C11 C12 H12A 119.1 . . ? C12 C13 C14 119.4(5) . . ? C12 C13 H13A 120.3 . . ? C14 C13 H13A 120.3 . . ? C13 C14 C15 119.8(5) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C14 C15 C16 122.1(5) . . ? C14 C15 H15A 119.0 . . ? C16 C15 H15A 119.0 . . ? O2 C16 C15 120.2(5) . . ? O2 C16 C11 122.6(4) . . ? C15 C16 C11 117.2(5) . . ? O1' C1' C2' 122.1(4) . . ? O1' C1' C6' 120.2(4) . . ? C2' C1' C6' 117.7(4) . . ? C3' C2' C1' 120.1(5) . . ? C3' C2' H2'A 120.0 . . ? C1' C2' H2'A 120.0 . . ? C2' C3' C4' 122.2(5) . . ? C2' C3' H3'A 118.9 . . ? C4' C3' H3'A 118.9 . . ? C5' C4' C3' 118.7(5) . . ? C5' C4' H4'A 120.6 . . ? C3' C4' H4'A 120.6 . . ? C4' C5' C6' 121.6(5) . . ? C4' C5' H5'A 119.2 . . ? C6' C5' H5'A 119.2 . . ? C5' C6' C1' 119.7(5) . . ? C5' C6' C7' 118.5(5) . . ? C1' C6' C7' 121.7(4) . . ? N1' C7' C6' 125.9(4) . . ? N1' C7' H7'A 117.1 . . ? C6' C7' H7'A 117.1 . . ? N1' C8' C8' 109.2(5) . 3_665 ? N1' C8' H8'A 109.8 . . ? C8' C8' H8'A 109.8 3_665 . ? N1' C8' H8'B 109.8 . . ? C8' C8' H8'B 109.8 3_665 . ? H8'A C8' H8'B 108.3 . . ? C17 O3 Tb1 131.6(3) . . ? C17 O3 H3B 109.5 . . ? Tb1 O3 H3B 99.8 . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.447 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.139 data_complex-4 _database_code_depnum_ccdc_archive 'CCDC 680105' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H52 Cl2 N6 Nd2 O8' _chemical_formula_weight 1224.36 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' Cl Cl 0.1484 0.1585 '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 P2(1)/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 13.124(3) _cell_length_b 10.173(2) _cell_length_c 19.757(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.76(3) _cell_angle_gamma 90.00 _cell_volume 2550.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 2.175 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.6955 _exptl_absorpt_correction_T_max 0.8118 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7774 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4493 _reflns_number_gt 3784 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and Rfactors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+1.2517P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0036(2) _refine_ls_number_reflns 4493 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.658714(14) 0.798918(17) 0.215349(9) 0.02296(8) Uani 1 1 d . . . Cl1 Cl 0.53483(7) 0.86785(9) 0.30410(5) 0.0318(2) Uani 1 1 d . . . N1 N 0.7484(2) 1.0246(3) 0.24506(15) 0.0298(7) Uani 1 1 d . . . N2 N 0.5669(2) 0.9860(3) 0.13285(15) 0.0278(7) Uani 1 1 d . . . O1 O 0.82323(19) 0.7693(2) 0.28622(13) 0.0332(6) Uani 1 1 d . . . O2 O 0.51134(19) 0.7131(2) 0.13778(13) 0.0288(6) Uani 1 1 d . . . O1' O 0.72731(19) 0.7655(2) 0.11963(13) 0.0320(6) Uani 1 1 d . . . H1L H 0.6820 0.7115 0.1019 0.048 Uiso 1 1 calc R . . N1' N 0.5950(2) 0.6403(3) 0.01330(15) 0.0275(7) Uani 1 1 d . . . C1 C 0.9165(3) 0.8246(4) 0.30588(18) 0.0288(8) Uani 1 1 d . . . C2 C 1.0082(3) 0.7494(4) 0.3313(2) 0.0389(10) Uani 1 1 d . . . H2A H 1.0022 0.6585 0.3335 0.047 Uiso 1 1 calc R . . C3 C 1.1059(3) 0.8051(5) 0.3528(2) 0.0470(11) Uani 1 1 d . . . H3A H 1.1645 0.7514 0.3685 0.056 Uiso 1 1 calc R . . C4 C 1.1192(3) 0.9401(5) 0.3516(2) 0.0540(12) Uani 1 1 d . . . H4A H 1.1856 0.9777 0.3673 0.065 Uiso 1 1 calc R . . C5 C 1.0315(3) 1.0171(4) 0.3265(2) 0.0479(11) Uani 1 1 d . . . H5A H 1.0394 1.1078 0.3250 0.057 Uiso 1 1 calc R . . C6 C 0.9302(3) 0.9622(4) 0.3032(2) 0.0345(9) Uani 1 1 d . . . C7 C 0.8441(3) 1.0527(4) 0.27592(19) 0.0345(9) Uani 1 1 d . . . H7A H 0.8602 1.1417 0.2815 0.041 Uiso 1 1 calc R . . C8 C 0.6771(3) 1.1342(4) 0.2176(2) 0.0341(9) Uani 1 1 d . . . H8A H 0.7161 1.2162 0.2233 0.041 Uiso 1 1 calc R . . H8B H 0.6230 1.1407 0.2430 0.041 Uiso 1 1 calc R . . C9 C 0.6269(3) 1.1095(4) 0.1406(2) 0.0348(9) Uani 1 1 d . . . H9A H 0.5802 1.1817 0.1213 0.042 Uiso 1 1 calc R . . H9B H 0.6811 1.1038 0.1153 0.042 Uiso 1 1 calc R . . C10 C 0.4772(3) 0.9866(4) 0.08838(19) 0.0314(8) Uani 1 1 d . . . H10A H 0.4592 1.0633 0.0624 0.038 Uiso 1 1 calc R . . C11 C 0.3999(3) 0.8814(4) 0.07370(18) 0.0306(8) Uani 1 1 d . . . C12 C 0.2996(3) 0.9131(4) 0.0319(2) 0.0415(10) Uani 1 1 d . . . H12A H 0.2887 0.9958 0.0113 0.050 Uiso 1 1 calc R . . C13 C 0.2173(3) 0.8267(5) 0.0205(2) 0.0472(11) Uani 1 1 d . . . H13A H 0.1519 0.8496 -0.0082 0.057 Uiso 1 1 calc R . . C14 C 0.2331(3) 0.7036(4) 0.0525(2) 0.0444(10) Uani 1 1 d . . . H14A H 0.1771 0.6452 0.0464 0.053 Uiso 1 1 calc R . . C15 C 0.3302(3) 0.6678(4) 0.0928(2) 0.0340(9) Uani 1 1 d . . . H15A H 0.3388 0.5854 0.1139 0.041 Uiso 1 1 calc R . . C16 C 0.4180(3) 0.7534(4) 0.10316(18) 0.0278(8) Uani 1 1 d . . . C1' C 0.7909(3) 0.7808(3) 0.07997(18) 0.0258(8) Uani 1 1 d . . . C2' C 0.8864(3) 0.8497(4) 0.1025(2) 0.0341(9) Uani 1 1 d . . . H2'A H 0.9048 0.8860 0.1471 0.041 Uiso 1 1 calc R . . C3' C 0.9527(3) 0.8640(5) 0.0597(2) 0.0486(11) Uani 1 1 d . . . H3'A H 1.0156 0.9098 0.0758 0.058 Uiso 1 1 calc R . . C4' C 0.9280(3) 0.8110(5) -0.0079(2) 0.0543(13) Uani 1 1 d . . . H4'A H 0.9743 0.8211 -0.0362 0.065 Uiso 1 1 calc R . . C5' C 0.8364(3) 0.7451(5) -0.0320(2) 0.0445(10) Uani 1 1 d . . . H5'A H 0.8197 0.7107 -0.0771 0.053 Uiso 1 1 calc R . . C6' C 0.7656(3) 0.7278(3) 0.01098(18) 0.0273(8) Uani 1 1 d . . . C7' C 0.6700(3) 0.6601(3) -0.01785(18) 0.0278(8) Uani 1 1 d . . . H7'A H 0.6599 0.6269 -0.0629 0.033 Uiso 1 1 calc R . . C8' C 0.4993(3) 0.5651(3) -0.01966(18) 0.0287(8) Uani 1 1 d . . . H8'A H 0.4969 0.5480 -0.0683 0.043 Uiso 1 1 calc R . . H8'B H 0.4372 0.6154 -0.0180 0.043 Uiso 1 1 calc R . . O3 O 0.6546(2) 0.5637(2) 0.24814(15) 0.0412(7) Uani 1 1 d . . . H3B H 0.6408 0.5288 0.2094 0.049 Uiso 1 1 calc R . . C17 C 0.7329(4) 0.4868(4) 0.2964(2) 0.0496(11) Uani 1 1 d . . . H17A H 0.7080 0.3982 0.2974 0.074 Uiso 1 1 calc R . . H17B H 0.7457 0.5244 0.3424 0.074 Uiso 1 1 calc R . . H17C H 0.7972 0.4865 0.2817 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02396(11) 0.02222(11) 0.02318(12) -0.00141(8) 0.00689(8) 0.00008(8) Cl1 0.0331(5) 0.0341(5) 0.0308(5) -0.0037(4) 0.0126(4) 0.0022(4) N1 0.0339(18) 0.0259(16) 0.0298(17) -0.0040(13) 0.0083(14) 0.0010(13) N2 0.0301(17) 0.0257(16) 0.0279(17) 0.0018(13) 0.0080(14) 0.0011(13) O1 0.0282(15) 0.0317(14) 0.0365(15) 0.0033(12) 0.0025(12) 0.0005(11) O2 0.0278(13) 0.0267(13) 0.0302(14) -0.0023(11) 0.0042(11) -0.0010(11) O1' 0.0338(14) 0.0372(14) 0.0281(14) -0.0075(11) 0.0133(12) -0.0089(12) N1' 0.0283(16) 0.0255(16) 0.0298(17) -0.0018(13) 0.0095(14) -0.0069(13) C1 0.027(2) 0.039(2) 0.0202(19) -0.0038(16) 0.0051(16) 0.0003(16) C2 0.034(2) 0.046(2) 0.038(2) 0.0169(19) 0.0127(19) 0.0140(19) C3 0.021(2) 0.073(3) 0.046(3) 0.005(2) 0.0078(19) 0.011(2) C4 0.032(2) 0.062(3) 0.061(3) -0.003(2) -0.002(2) -0.008(2) C5 0.038(2) 0.043(3) 0.056(3) -0.007(2) 0.001(2) -0.011(2) C6 0.035(2) 0.035(2) 0.033(2) -0.0022(17) 0.0071(18) 0.0006(17) C7 0.037(2) 0.028(2) 0.037(2) -0.0079(17) 0.0065(18) -0.0080(17) C8 0.037(2) 0.023(2) 0.041(2) -0.0035(17) 0.0091(19) -0.0006(16) C9 0.037(2) 0.0250(19) 0.043(2) 0.0050(17) 0.0109(19) -0.0013(17) C10 0.031(2) 0.032(2) 0.030(2) 0.0099(17) 0.0069(18) 0.0074(17) C11 0.0258(19) 0.037(2) 0.027(2) -0.0022(16) 0.0037(16) 0.0016(16) C12 0.037(2) 0.046(2) 0.037(2) 0.001(2) 0.0020(19) 0.006(2) C13 0.027(2) 0.064(3) 0.046(3) -0.004(2) 0.0007(19) 0.006(2) C14 0.029(2) 0.052(3) 0.051(3) -0.011(2) 0.009(2) -0.005(2) C15 0.028(2) 0.038(2) 0.037(2) -0.0066(18) 0.0088(18) -0.0031(17) C16 0.026(2) 0.035(2) 0.0226(19) -0.0056(16) 0.0069(16) 0.0005(16) C1' 0.0292(19) 0.0229(19) 0.0268(19) 0.0033(15) 0.0098(16) 0.0021(15) C2' 0.037(2) 0.035(2) 0.029(2) -0.0022(17) 0.0066(18) -0.0078(18) C3' 0.036(2) 0.066(3) 0.043(3) -0.003(2) 0.010(2) -0.022(2) C4' 0.041(3) 0.089(4) 0.040(3) -0.005(2) 0.023(2) -0.024(3) C5' 0.042(3) 0.063(3) 0.032(2) -0.006(2) 0.016(2) -0.011(2) C6' 0.0269(19) 0.029(2) 0.027(2) 0.0012(15) 0.0086(16) -0.0027(15) C7' 0.036(2) 0.0269(18) 0.0221(19) -0.0029(15) 0.0095(16) -0.0011(16) C8' 0.032(2) 0.030(2) 0.0245(19) -0.0030(16) 0.0084(16) -0.0069(16) O3 0.0377(15) 0.0269(14) 0.0534(18) -0.0010(13) 0.0013(13) -0.0014(12) C17 0.067(3) 0.033(2) 0.045(3) 0.011(2) 0.008(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1 2.274(3) . ? Nd1 O2 2.311(3) . ? Nd1 O1' 2.317(2) . ? Nd1 O3 2.484(3) . ? Nd1 N1 2.578(3) . ? Nd1 N2 2.594(3) . ? Nd1 Cl1 2.7681(10) . ? N1 C7 1.281(5) . ? N1 C8 1.468(5) . ? N2 C10 1.278(5) . ? N2 C9 1.469(5) . ? O1 C1 1.313(4) . ? O2 C16 1.308(4) . ? O1' C1' 1.292(4) . ? O1' H1L 0.8200 . ? N1' C7' 1.303(4) . ? N1' C8' 1.473(4) . ? C1 C2 1.406(5) . ? C1 C6 1.414(5) . ? C2 C3 1.366(6) . ? C2 H2A 0.9300 . ? C3 C4 1.385(6) . ? C3 H3A 0.9300 . ? C4 C5 1.376(6) . ? C4 H4A 0.9300 . ? C5 C6 1.407(5) . ? C5 H5A 0.9300 . ? C6 C7 1.451(5) . ? C7 H7A 0.9300 . ? C8 C9 1.516(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.452(5) . ? C10 H10A 0.9300 . ? C11 C12 1.402(5) . ? C11 C16 1.421(5) . ? C12 C13 1.365(6) . ? C12 H12A 0.9300 . ? C13 C14 1.394(6) . ? C13 H13A 0.9300 . ? C14 C15 1.369(6) . ? C14 H14A 0.9300 . ? C15 C16 1.417(5) . ? C15 H15A 0.9300 . ? C1' C2' 1.405(5) . ? C1' C6' 1.424(5) . ? C2' C3' 1.368(5) . ? C2' H2'A 0.9300 . ? C3' C4' 1.399(6) . ? C3' H3'A 0.9300 . ? C4' C5' 1.352(6) . ? C4' H4'A 0.9300 . ? C5' C6' 1.422(5) . ? C5' H5'A 0.9300 . ? C6' C7' 1.417(5) . ? C7' H7'A 0.9300 . ? C8' C8' 1.534(7) 3_665 ? C8' H8'A 0.9700 . ? C8' H8'B 0.9700 . ? O3 C17 1.442(5) . ? O3 H3B 0.8200 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nd1 O2 149.42(9) . . ? O1 Nd1 O1' 88.72(9) . . ? O2 Nd1 O1' 80.62(9) . . ? O1 Nd1 O3 77.99(9) . . ? O2 Nd1 O3 74.85(9) . . ? O1' Nd1 O3 96.33(9) . . ? O1 Nd1 N1 70.81(9) . . ? O2 Nd1 N1 138.05(9) . . ? O1' Nd1 N1 93.82(9) . . ? O3 Nd1 N1 146.89(9) . . ? O1 Nd1 N2 134.44(9) . . ? O2 Nd1 N2 71.60(9) . . ? O1' Nd1 N2 79.02(9) . . ? O3 Nd1 N2 146.45(9) . . ? N1 Nd1 N2 66.53(10) . . ? O1 Nd1 Cl1 105.20(7) . . ? O2 Nd1 Cl1 89.33(6) . . ? O1' Nd1 Cl1 165.27(7) . . ? O3 Nd1 Cl1 91.35(7) . . ? N1 Nd1 Cl1 86.44(6) . . ? N2 Nd1 Cl1 87.62(6) . . ? C7 N1 C8 117.5(3) . . ? C7 N1 Nd1 130.0(3) . . ? C8 N1 Nd1 112.4(2) . . ? C10 N2 C9 116.3(3) . . ? C10 N2 Nd1 129.4(2) . . ? C9 N2 Nd1 114.3(2) . . ? C1 O1 Nd1 142.4(2) . . ? C16 O2 Nd1 137.9(2) . . ? C1' O1' Nd1 157.3(2) . . ? C1' O1' H1L 109.5 . . ? Nd1 O1' H1L 93.2 . . ? C7' N1' C8' 122.2(3) . . ? O1 C1 C2 121.4(4) . . ? O1 C1 C6 122.1(3) . . ? C2 C1 C6 116.5(4) . . ? C3 C2 C1 122.3(4) . . ? C3 C2 H2A 118.8 . . ? C1 C2 H2A 118.8 . . ? C2 C3 C4 121.2(4) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C5 C4 C3 118.2(4) . . ? C5 C4 H4A 120.9 . . ? C3 C4 H4A 120.9 . . ? C4 C5 C6 121.8(4) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C5 C6 C1 119.9(4) . . ? C5 C6 C7 116.9(4) . . ? C1 C6 C7 123.2(3) . . ? N1 C7 C6 127.7(4) . . ? N1 C7 H7A 116.1 . . ? C6 C7 H7A 116.1 . . ? N1 C8 C9 108.5(3) . . ? N1 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? N1 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? N2 C9 C8 109.3(3) . . ? N2 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? N2 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C11 127.5(3) . . ? N2 C10 H10A 116.3 . . ? C11 C10 H10A 116.3 . . ? C12 C11 C16 119.1(3) . . ? C12 C11 C10 116.8(3) . . ? C16 C11 C10 123.9(3) . . ? C13 C12 C11 122.3(4) . . ? C13 C12 H12A 118.9 . . ? C11 C12 H12A 118.9 . . ? C12 C13 C14 118.9(4) . . ? C12 C13 H13A 120.6 . . ? C14 C13 H13A 120.6 . . ? C15 C14 C13 120.8(4) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C14 C15 C16 121.5(4) . . ? C14 C15 H15A 119.3 . . ? C16 C15 H15A 119.3 . . ? O2 C16 C15 120.1(3) . . ? O2 C16 C11 122.6(3) . . ? C15 C16 C11 117.3(3) . . ? O1' C1' C2' 122.0(3) . . ? O1' C1' C6' 120.3(3) . . ? C2' C1' C6' 117.7(3) . . ? C3' C2' C1' 120.9(4) . . ? C3' C2' H2'A 119.5 . . ? C1' C2' H2'A 119.5 . . ? C2' C3' C4' 121.3(4) . . ? C2' C3' H3'A 119.4 . . ? C4' C3' H3'A 119.4 . . ? C5' C4' C3' 119.8(4) . . ? C5' C4' H4'A 120.1 . . ? C3' C4' H4'A 120.1 . . ? C4' C5' C6' 120.6(4) . . ? C4' C5' H5'A 119.7 . . ? C6' C5' H5'A 119.7 . . ? C7' C6' C5' 117.8(3) . . ? C7' C6' C1' 122.4(3) . . ? C5' C6' C1' 119.7(3) . . ? N1' C7' C6' 125.7(3) . . ? N1' C7' H7'A 117.2 . . ? C6' C7' H7'A 117.2 . . ? N1' C8' C8' 109.0(4) . 3_665 ? N1' C8' H8'A 109.9 . . ? C8' C8' H8'A 109.9 3_665 . ? N1' C8' H8'B 109.9 . . ? C8' C8' H8'B 109.9 3_665 . ? H8'A C8' H8'B 108.3 . . ? C17 O3 Nd1 129.5(2) . . ? C17 O3 H3B 109.5 . . ? Nd1 O3 H3B 100.8 . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.994 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.085 data_complex-5 _database_code_depnum_ccdc_archive 'CCDC 680106' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H52 Cl2 N6 O8 Yb2' _chemical_formula_weight 1281.96 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.104(3) _cell_length_b 10.018(2) _cell_length_c 19.463(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.51(3) _cell_angle_gamma 90.00 _cell_volume 2484.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 3.908 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5087 _exptl_absorpt_correction_T_max 0.7993 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7331 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4354 _reflns_number_gt 3867 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and Rfactors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+1.2517P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0055(3) _refine_ls_number_reflns 4354 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0712 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.654671(13) 0.810187(17) 0.210624(9) 0.01758(9) Uani 1 1 d . . . Cl1 Cl 0.54324(9) 0.87235(11) 0.30259(6) 0.0251(2) Uani 1 1 d . . . N1 N 0.7442(3) 1.0229(3) 0.24565(19) 0.0239(8) Uani 1 1 d . . . N2 N 0.5683(3) 0.9938(4) 0.13437(18) 0.0219(8) Uani 1 1 d . . . O1 O 0.8076(3) 0.7610(3) 0.27575(18) 0.0284(7) Uani 1 1 d . . . O2 O 0.5131(2) 0.7217(3) 0.14168(16) 0.0241(7) Uani 1 1 d . . . O1' O 0.7196(3) 0.7750(3) 0.11804(17) 0.0293(7) Uani 1 1 d . . . H1L H 0.6744 0.7208 0.0999 0.044 Uiso 1 1 calc R . . N1' N 0.5951(3) 0.6404(4) 0.01286(19) 0.0235(8) Uani 1 1 d . . . C1 C 0.9009(4) 0.8089(4) 0.2990(2) 0.0244(10) Uani 1 1 d . . . C2 C 0.9883(4) 0.7243(6) 0.3219(3) 0.0327(11) Uani 1 1 d . . . H2A H 0.9780 0.6324 0.3190 0.039 Uiso 1 1 calc R . . C3 C 1.0864(4) 0.7715(7) 0.3478(3) 0.0459(14) Uani 1 1 d . . . H3A H 1.1423 0.7125 0.3609 0.055 Uiso 1 1 calc R . . C4 C 1.1038(4) 0.9084(7) 0.3548(3) 0.0535(16) Uani 1 1 d . . . H4A H 1.1710 0.9405 0.3742 0.064 Uiso 1 1 calc R . . C5 C 1.0229(4) 0.9951(6) 0.3335(3) 0.0454(14) Uani 1 1 d . . . H5A H 1.0355 1.0864 0.3381 0.054 Uiso 1 1 calc R . . C6 C 0.9209(4) 0.9491(5) 0.3047(2) 0.0279(10) Uani 1 1 d . . . C7 C 0.8396(3) 1.0459(5) 0.2795(2) 0.0280(10) Uani 1 1 d . . . H7A H 0.8578 1.1349 0.2886 0.034 Uiso 1 1 calc R . . C8 C 0.6775(4) 1.1381(5) 0.2204(2) 0.0291(10) Uani 1 1 d . . . H8A H 0.7191 1.2192 0.2274 0.035 Uiso 1 1 calc R . . H8B H 0.6232 1.1459 0.2465 0.035 Uiso 1 1 calc R . . C9 C 0.6284(4) 1.1185(4) 0.1424(2) 0.0290(10) Uani 1 1 d . . . H9A H 0.5824 1.1929 0.1245 0.035 Uiso 1 1 calc R . . H9B H 0.6826 1.1139 0.1161 0.035 Uiso 1 1 calc R . . C10 C 0.4808(4) 0.9961(5) 0.0898(2) 0.0279(10) Uani 1 1 d . . . H10A H 0.4642 1.0743 0.0638 0.033 Uiso 1 1 calc R . . C11 C 0.4036(4) 0.8896(5) 0.0749(2) 0.0264(10) Uani 1 1 d . . . C12 C 0.3049(4) 0.9216(6) 0.0325(3) 0.0362(12) Uani 1 1 d . . . H12A H 0.2950 1.0051 0.0111 0.043 Uiso 1 1 calc R . . C13 C 0.2217(4) 0.8333(6) 0.0213(3) 0.0411(13) Uani 1 1 d . . . H13A H 0.1570 0.8561 -0.0076 0.049 Uiso 1 1 calc R . . C14 C 0.2370(4) 0.7098(6) 0.0542(3) 0.0382(13) Uani 1 1 d . . . H14A H 0.1812 0.6503 0.0486 0.046 Uiso 1 1 calc R . . C15 C 0.3343(4) 0.6741(5) 0.0954(3) 0.0277(11) Uani 1 1 d . . . H15A H 0.3424 0.5906 0.1168 0.033 Uiso 1 1 calc R . . C16 C 0.4209(3) 0.7600(5) 0.1057(2) 0.0237(10) Uani 1 1 d . . . C1' C 0.7893(4) 0.7829(4) 0.0809(2) 0.0224(9) Uani 1 1 d . . . C2' C 0.8862(4) 0.8503(5) 0.1051(3) 0.0308(11) Uani 1 1 d . . . H2'A H 0.9017 0.8903 0.1494 0.037 Uiso 1 1 calc R . . C3' C 0.9567(4) 0.8568(7) 0.0635(3) 0.0452(14) Uani 1 1 d . . . H3'A H 1.0199 0.9012 0.0804 0.054 Uiso 1 1 calc R . . C4' C 0.9370(5) 0.7987(7) -0.0036(3) 0.059(2) Uani 1 1 d . . . H4'A H 0.9866 0.8041 -0.0307 0.071 Uiso 1 1 calc R . . C5' C 0.8445(5) 0.7345(7) -0.0288(3) 0.0468(15) Uani 1 1 d . . . H5'A H 0.8304 0.6977 -0.0739 0.056 Uiso 1 1 calc R . . C6' C 0.7695(4) 0.7227(5) 0.0125(2) 0.0269(10) Uani 1 1 d . . . C7' C 0.6730(4) 0.6561(5) -0.0171(2) 0.0262(10) Uani 1 1 d . . . H7'A H 0.6652 0.6205 -0.0622 0.031 Uiso 1 1 calc R . . C8' C 0.5010(3) 0.5655(4) -0.0198(2) 0.0236(9) Uani 1 1 d . . . H8'A H 0.5005 0.5473 -0.0688 0.035 Uiso 1 1 calc R . . H8'B H 0.4392 0.6178 -0.0185 0.035 Uiso 1 1 calc R . . O3 O 0.6449(2) 0.5840(3) 0.23859(19) 0.0321(8) Uani 1 1 d . . . H3B H 0.5861 0.5827 0.2464 0.038 Uiso 1 1 calc R . . C17 C 0.7137(4) 0.5009(5) 0.2888(3) 0.0410(13) Uani 1 1 d . . . H17A H 0.6846 0.4127 0.2874 0.062 Uiso 1 1 calc R . . H17B H 0.7216 0.5376 0.3353 0.062 Uiso 1 1 calc R . . H17C H 0.7810 0.4966 0.2773 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01722(13) 0.01775(12) 0.01798(13) -0.00147(7) 0.00452(8) 0.00035(7) Cl1 0.0265(6) 0.0272(5) 0.0243(5) -0.0024(5) 0.0111(4) 0.0017(5) N1 0.030(2) 0.0166(17) 0.026(2) -0.0027(15) 0.0084(17) -0.0020(15) N2 0.023(2) 0.0219(18) 0.0210(19) 0.0034(15) 0.0057(16) 0.0010(15) O1 0.0192(17) 0.0260(17) 0.0374(19) 0.0017(15) 0.0016(14) 0.0012(14) O2 0.0195(17) 0.0260(15) 0.0246(16) -0.0017(13) 0.0007(13) -0.0045(13) O1' 0.0305(18) 0.0338(17) 0.0271(17) -0.0096(15) 0.0138(15) -0.0086(15) N1' 0.022(2) 0.0232(18) 0.025(2) 0.0026(16) 0.0057(16) -0.0043(16) C1 0.018(2) 0.039(3) 0.017(2) -0.0017(18) 0.0057(18) 0.0023(19) C2 0.025(3) 0.042(3) 0.029(3) -0.001(2) 0.003(2) 0.008(2) C3 0.025(3) 0.075(4) 0.036(3) 0.003(3) 0.003(2) 0.016(3) C4 0.025(3) 0.076(5) 0.053(4) 0.002(3) -0.006(3) -0.005(3) C5 0.032(3) 0.051(3) 0.047(3) -0.003(3) -0.004(2) -0.015(3) C6 0.025(2) 0.034(3) 0.023(2) -0.003(2) 0.0026(19) -0.002(2) C7 0.031(3) 0.026(2) 0.027(2) -0.0035(19) 0.008(2) -0.0096(19) C8 0.033(3) 0.021(2) 0.033(3) -0.003(2) 0.007(2) 0.000(2) C9 0.035(3) 0.021(2) 0.032(3) 0.005(2) 0.010(2) -0.002(2) C10 0.031(3) 0.028(2) 0.026(2) 0.006(2) 0.009(2) 0.006(2) C11 0.026(2) 0.032(2) 0.022(2) 0.000(2) 0.0068(19) 0.001(2) C12 0.028(3) 0.046(3) 0.032(3) 0.006(2) 0.001(2) 0.004(2) C13 0.020(3) 0.064(4) 0.033(3) 0.002(3) -0.006(2) 0.007(2) C14 0.020(3) 0.059(4) 0.035(3) -0.010(3) 0.003(2) -0.008(2) C15 0.025(3) 0.035(3) 0.024(2) -0.004(2) 0.006(2) -0.005(2) C16 0.019(2) 0.032(2) 0.020(2) -0.007(2) 0.0049(18) 0.000(2) C1' 0.026(2) 0.020(2) 0.021(2) 0.0028(18) 0.0062(19) 0.0038(18) C2' 0.031(3) 0.036(3) 0.024(3) -0.002(2) 0.004(2) -0.005(2) C3' 0.028(3) 0.069(4) 0.038(3) -0.004(3) 0.007(2) -0.019(3) C4' 0.036(3) 0.112(6) 0.038(3) -0.018(3) 0.025(3) -0.029(3) C5' 0.040(3) 0.076(4) 0.028(3) -0.015(3) 0.016(2) -0.018(3) C6' 0.029(3) 0.034(2) 0.020(2) -0.001(2) 0.009(2) -0.001(2) C7' 0.031(3) 0.028(2) 0.021(2) -0.0018(19) 0.010(2) -0.002(2) C8' 0.024(2) 0.029(2) 0.017(2) -0.0009(19) 0.0039(18) -0.0062(19) O3 0.0214(17) 0.0188(16) 0.051(2) 0.0094(15) -0.0022(15) -0.0002(13) C17 0.044(3) 0.031(3) 0.046(3) 0.010(2) 0.006(3) -0.002(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 Yb1 O1 2.163(3) . ? Yb1 O1' 2.193(3) . ? Yb1 O2 2.206(3) . ? Yb1 O3 2.341(3) . ? Yb1 N1 2.451(4) . ? Yb1 N2 2.466(4) . ? Yb1 Cl1 2.6354(12) . ? N1 C7 1.290(6) . ? N1 C8 1.461(6) . ? N2 C10 1.266(6) . ? N2 C9 1.466(6) . ? O1 C1 1.293(6) . ? O2 C16 1.304(5) . ? O1' C1' 1.293(5) . ? O1' H1L 0.8200 . ? N1' C7' 1.298(6) . ? N1' C8' 1.456(5) . ? C1 C2 1.410(7) . ? C1 C6 1.428(6) . ? C2 C3 1.352(8) . ? C2 H2A 0.9300 . ? C3 C4 1.391(9) . ? C3 H3A 0.9300 . ? C4 C5 1.359(8) . ? C4 H4A 0.9300 . ? C5 C6 1.402(7) . ? C5 H5A 0.9300 . ? C6 C7 1.440(7) . ? C7 H7A 0.9300 . ? C8 C9 1.516(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.453(7) . ? C10 H10A 0.9300 . ? C11 C12 1.399(7) . ? C11 C16 1.426(7) . ? C12 C13 1.381(8) . ? C12 H12A 0.9300 . ? C13 C14 1.385(8) . ? C13 H13A 0.9300 . ? C14 C15 1.386(7) . ? C14 H14A 0.9300 . ? C15 C16 1.401(7) . ? C15 H15A 0.9300 . ? C1' C2' 1.418(7) . ? C1' C6' 1.429(6) . ? C2' C3' 1.364(7) . ? C2' H2'A 0.9300 . ? C3' C4' 1.398(8) . ? C3' H3'A 0.9300 . ? C4' C5' 1.358(8) . ? C4' H4'A 0.9300 . ? C5' C6' 1.413(7) . ? C5' H5'A 0.9300 . ? C6' C7' 1.427(7) . ? C7' H7'A 0.9300 . ? C8' C8' 1.525(8) 3_665 ? C8' H8'A 0.9700 . ? C8' H8'B 0.9700 . ? O3 C17 1.431(6) . ? O3 H3B 0.8200 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O1' 87.76(13) . . ? O1 Yb1 O2 142.88(12) . . ? O1' Yb1 O2 82.43(12) . . ? O1 Yb1 O3 74.73(11) . . ? O1' Yb1 O3 95.07(13) . . ? O2 Yb1 O3 70.64(11) . . ? O1 Yb1 N1 73.59(13) . . ? O1' Yb1 N1 96.65(12) . . ? O2 Yb1 N1 142.98(12) . . ? O3 Yb1 N1 145.64(12) . . ? O1 Yb1 N2 139.00(12) . . ? O1' Yb1 N2 80.60(12) . . ? O2 Yb1 N2 74.41(12) . . ? O3 Yb1 N2 145.04(12) . . ? N1 Yb1 N2 68.99(12) . . ? O1 Yb1 Cl1 103.90(9) . . ? O1' Yb1 Cl1 168.15(9) . . ? O2 Yb1 Cl1 89.27(9) . . ? O3 Yb1 Cl1 90.10(9) . . ? N1 Yb1 Cl1 84.88(9) . . ? N2 Yb1 Cl1 89.05(8) . . ? C7 N1 C8 117.5(4) . . ? C7 N1 Yb1 129.9(3) . . ? C8 N1 Yb1 112.6(3) . . ? C10 N2 C9 115.8(4) . . ? C10 N2 Yb1 129.9(3) . . ? C9 N2 Yb1 114.3(3) . . ? C1 O1 Yb1 142.3(3) . . ? C16 O2 Yb1 138.6(3) . . ? C1' O1' Yb1 155.5(3) . . ? C1' O1' H1L 109.5 . . ? Yb1 O1' H1L 94.6 . . ? C7' N1' C8' 122.7(4) . . ? O1 C1 C2 121.3(4) . . ? O1 C1 C6 122.2(4) . . ? C2 C1 C6 116.5(4) . . ? C3 C2 C1 122.6(5) . . ? C3 C2 H2A 118.7 . . ? C1 C2 H2A 118.7 . . ? C2 C3 C4 120.1(5) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C5 C4 C3 120.1(5) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 121.0(6) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C1 119.6(5) . . ? C5 C6 C7 118.4(5) . . ? C1 C6 C7 121.9(4) . . ? N1 C7 C6 127.2(4) . . ? N1 C7 H7A 116.4 . . ? C6 C7 H7A 116.4 . . ? N1 C8 C9 108.4(4) . . ? N1 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? N1 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? N2 C9 C8 108.0(4) . . ? N2 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? N2 C9 H9B 110.1 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? N2 C10 C11 126.9(4) . . ? N2 C10 H10A 116.6 . . ? C11 C10 H10A 116.6 . . ? C12 C11 C16 119.4(4) . . ? C12 C11 C10 117.0(4) . . ? C16 C11 C10 123.4(4) . . ? C13 C12 C11 122.2(5) . . ? C13 C12 H12A 118.9 . . ? C11 C12 H12A 118.9 . . ? C12 C13 C14 118.4(5) . . ? C12 C13 H13A 120.8 . . ? C14 C13 H13A 120.8 . . ? C13 C14 C15 120.8(5) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C14 C15 C16 122.0(5) . . ? C14 C15 H15A 119.0 . . ? C16 C15 H15A 119.0 . . ? O2 C16 C15 120.9(4) . . ? O2 C16 C11 122.0(4) . . ? C15 C16 C11 117.0(4) . . ? O1' C1' C2' 122.6(4) . . ? O1' C1' C6' 119.8(4) . . ? C2' C1' C6' 117.7(4) . . ? C3' C2' C1' 120.2(5) . . ? C3' C2' H2'A 119.9 . . ? C1' C2' H2'A 119.9 . . ? C2' C3' C4' 122.1(5) . . ? C2' C3' H3'A 118.9 . . ? C4' C3' H3'A 118.9 . . ? C5' C4' C3' 119.3(5) . . ? C5' C4' H4'A 120.4 . . ? C3' C4' H4'A 120.4 . . ? C4' C5' C6' 121.0(5) . . ? C4' C5' H5'A 119.5 . . ? C6' C5' H5'A 119.5 . . ? C5' C6' C7' 118.5(4) . . ? C5' C6' C1' 119.7(5) . . ? C7' C6' C1' 121.7(4) . . ? N1' C7' C6' 126.2(4) . . ? N1' C7' H7'A 116.9 . . ? C6' C7' H7'A 116.9 . . ? N1' C8' C8' 109.7(4) . 3_665 ? N1' C8' H8'A 109.7 . . ? C8' C8' H8'A 109.7 3_665 . ? N1' C8' H8'B 109.7 . . ? C8' C8' H8'B 109.7 3_665 . ? H8'A C8' H8'B 108.2 . . ? C17 O3 Yb1 131.4(3) . . ? C17 O3 H3B 109.5 . . ? Yb1 O3 H3B 99.4 . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.026 _refine_diff_density_min -1.292 _refine_diff_density_rms 0.146