# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Bin Zhao' _publ_contact_author_email ZHAOBIN@NANKAI.EDU.CN _publ_section_title ; Unique two-fold interpenetration of 3D microporous 3d-4f heterometal-organic frameworks (HMOF) based on a rigid ligand ; loop_ _publ_author_name 'Bin Zhao' 'Jun Chen' 'Peng Cheng' 'Ming Fang' 'Jing Liang' 'Wei Shi' ; Ya Zuo ; # Attachment '3.cif' data_r70504a _database_code_depnum_ccdc_archive 'CCDC 692739' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H32 Cu1.50 Eu N6 O19' _chemical_formula_weight 1099.95 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.137(5) _cell_length_b 12.413(3) _cell_length_c 26.807(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.12(3) _cell_angle_gamma 90.00 _cell_volume 7903(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4388 _exptl_absorpt_coefficient_mu 2.464 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7564 _exptl_absorpt_correction_T_max 0.8273 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _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 23769 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6955 _reflns_number_gt 5947 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+78.0997P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6955 _refine_ls_number_parameters 605 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.104 _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 Eu1 Eu 0.626550(9) 0.215155(17) 0.545453(7) 0.01143(5) Uani 1 1 d . . . Cu1 Cu 0.25292(2) 0.20949(4) 0.365459(17) 0.01218(12) Uani 1 1 d . . . Cu2 Cu 1.0000 0.24862(7) 0.7500 0.01880(19) Uani 1 2 d S . . C1 C 0.38316(18) 0.1778(4) 0.43410(14) 0.0141(10) Uani 1 1 d . . . H1 H 0.3712 0.1250 0.4527 0.017 Uiso 1 1 calc R . . C2 C 0.43973(19) 0.1986(4) 0.44820(15) 0.0166(11) Uani 1 1 d . . . H2 H 0.4651 0.1621 0.4763 0.020 Uiso 1 1 calc R . . C3 C 0.45860(18) 0.2750(3) 0.41998(15) 0.0142(10) Uani 1 1 d . . . C4 C 0.41845(18) 0.3288(4) 0.37836(14) 0.0153(11) Uani 1 1 d . . . H4 H 0.4295 0.3814 0.3590 0.018 Uiso 1 1 calc R . . C5 C 0.36258(18) 0.3024(3) 0.36670(14) 0.0133(10) Uani 1 1 d . . . C6 C 0.31749(19) 0.3466(3) 0.32001(14) 0.0149(10) Uani 1 1 d . . . C7 C 0.32774(18) 0.4268(3) 0.28769(15) 0.0141(10) Uani 1 1 d . . . H7 H 0.3630 0.4589 0.2957 0.017 Uiso 1 1 calc R . . C8 C 0.28349(18) 0.4571(3) 0.24309(14) 0.0132(10) Uani 1 1 d . . . C9 C 0.23225(18) 0.4059(3) 0.23090(15) 0.0138(10) Uani 1 1 d . . . H9 H 0.2033 0.4220 0.1998 0.017 Uiso 1 1 calc R . . C10 C 0.22460(18) 0.3298(3) 0.26593(14) 0.0125(10) Uani 1 1 d . . . H10 H 0.1897 0.2967 0.2586 0.015 Uiso 1 1 calc R . . C11 C 0.52075(19) 0.3009(4) 0.43355(16) 0.0182(11) Uani 1 1 d . . . C12 C 0.29008(19) 0.5505(4) 0.20965(15) 0.0179(11) Uani 1 1 d . . . C13 C 0.2260(2) 0.0213(4) 0.42287(15) 0.0186(11) Uani 1 1 d . . . H13 H 0.2473 -0.0201 0.4075 0.022 Uiso 1 1 calc R . . C14 C 0.1991(2) -0.0290(3) 0.45398(15) 0.0168(11) Uani 1 1 d . . . H14 H 0.2039 -0.1025 0.4607 0.020 Uiso 1 1 calc R . . C15 C 0.16467(19) 0.0309(4) 0.47513(15) 0.0176(11) Uani 1 1 d . . . C16 C 0.16100(18) 0.1420(4) 0.46582(15) 0.0152(10) Uani 1 1 d . . . H16 H 0.1385 0.1844 0.4794 0.018 Uiso 1 1 calc R . . C17 C 0.19105(18) 0.1885(3) 0.43620(14) 0.0139(10) Uani 1 1 d . . . C18 C 0.19407(19) 0.3056(3) 0.42792(15) 0.0152(11) Uani 1 1 d . . . C19 C 0.1684(2) 0.3810(3) 0.45128(15) 0.0163(11) Uani 1 1 d . . . H19 H 0.1435 0.3590 0.4684 0.020 Uiso 1 1 calc R . . C20 C 0.18071(19) 0.4888(4) 0.44851(14) 0.0154(11) Uani 1 1 d . . . C21 C 0.21571(19) 0.5197(4) 0.42007(15) 0.0172(11) Uani 1 1 d . . . H21 H 0.2248 0.5918 0.4180 0.021 Uiso 1 1 calc R . . C22 C 0.2366(2) 0.4411(4) 0.39493(15) 0.0178(11) Uani 1 1 d . . . H22 H 0.2586 0.4618 0.3747 0.021 Uiso 1 1 calc R . . C23 C 0.1336(2) -0.0199(4) 0.50841(15) 0.0194(11) Uani 1 1 d . . . C24 C 0.15983(19) 0.5718(4) 0.47945(15) 0.0160(11) Uani 1 1 d . . . C25 C 0.88886(18) 0.3178(4) 0.74341(15) 0.0142(10) Uani 1 1 d . . . C26 C 0.83109(19) 0.3309(3) 0.72282(14) 0.0145(10) Uani 1 1 d . . . H26 H 0.8123 0.3732 0.7403 0.017 Uiso 1 1 calc R . . C27 C 0.80150(18) 0.2803(4) 0.67588(15) 0.0147(10) Uani 1 1 d . . . C28 C 0.8310(2) 0.2185(4) 0.65056(16) 0.0210(12) Uani 1 1 d . . . H28 H 0.8121 0.1846 0.6188 0.025 Uiso 1 1 calc R . . C29 C 0.8884(2) 0.2078(4) 0.67287(15) 0.0198(11) Uani 1 1 d . . . H29 H 0.9077 0.1657 0.6558 0.024 Uiso 1 1 calc R . . C30 C 0.73904(18) 0.2934(3) 0.65067(15) 0.0140(10) Uani 1 1 d . . . C31 C 1.07460(18) 0.3720(4) 0.70797(15) 0.0148(11) Uani 1 1 d . . . C32 C 1.09605(19) 0.4390(3) 0.67714(14) 0.0150(10) Uani 1 1 d . . . H32 H 1.1347 0.4479 0.6853 0.018 Uiso 1 1 calc R . . C33 C 1.05917(19) 0.4917(3) 0.63448(15) 0.0149(10) Uani 1 1 d . . . C34 C 1.00153(19) 0.4744(4) 0.62211(16) 0.0196(11) Uani 1 1 d . . . H34 H 0.9759 0.5081 0.5932 0.023 Uiso 1 1 calc R . . C35 C 0.98338(19) 0.4057(4) 0.65406(15) 0.0181(11) Uani 1 1 d . . . H35 H 0.9449 0.3941 0.6459 0.022 Uiso 1 1 calc R . . C36 C 1.08194(18) 0.5652(3) 0.60162(14) 0.0129(10) Uani 1 1 d . . . N1 N 0.34407(14) 0.2294(3) 0.39496(11) 0.0112(8) Uani 1 1 d . . . N2 N 0.26620(15) 0.3029(3) 0.30990(12) 0.0131(9) Uani 1 1 d . . . N3 N 0.22250(15) 0.1284(3) 0.41408(12) 0.0151(9) Uani 1 1 d . . . N4 N 0.22608(15) 0.3358(3) 0.39879(12) 0.0149(9) Uani 1 1 d . . . N5 N 0.91765(15) 0.2566(3) 0.71872(12) 0.0157(9) Uani 1 1 d . . . N6 N 1.01868(15) 0.3553(3) 0.69610(12) 0.0155(9) Uani 1 1 d . . . O1 O 0.24459(13) 0.5818(2) 0.17569(10) 0.0167(8) Uani 1 1 d . . . O2 O 0.33738(14) 0.5920(3) 0.21745(12) 0.0279(9) Uani 1 1 d . . . O3 O 0.53546(14) 0.3668(3) 0.40672(13) 0.0353(10) Uani 1 1 d . . . O4 O 0.55245(14) 0.2495(3) 0.47227(12) 0.0277(9) Uani 1 1 d . . . O5 O 0.17953(13) 0.6650(3) 0.48519(11) 0.0216(8) Uani 1 1 d . . . O6 O 0.12382(13) 0.5405(2) 0.49992(11) 0.0208(8) Uani 1 1 d . . . O7 O 0.09452(16) 0.0330(3) 0.51476(14) 0.0413(10) Uani 1 1 d . . . O8 O 0.14986(14) -0.1123(2) 0.52669(11) 0.0221(8) Uani 1 1 d . . . O9 O 0.60753(13) 0.3144(3) 0.61817(11) 0.0217(8) Uani 1 1 d . . . O10 O 0.71664(13) 0.2383(2) 0.60947(10) 0.0176(8) Uani 1 1 d . . . O11 O 0.71477(13) 0.3599(3) 0.67061(11) 0.0221(8) Uani 1 1 d . . . O12 O 1.04741(13) 0.6182(2) 0.56434(10) 0.0160(7) Uani 1 1 d U . . O13 O 1.13408(13) 0.5750(2) 0.61334(10) 0.0167(8) Uani 1 1 d . . . O14 O 1.0082(2) 0.1044(5) 0.7003(2) 0.0634(17) Uani 0.80 1 d PU . . O14' O 1.0000 0.0907(14) 0.7500 0.069(3) Uani 0.40 2 d SPU . . O15 O 0.0850(2) 0.2639(6) 0.2076(2) 0.0895(19) Uani 1 1 d U . . O16 O 0.9694(3) 0.2512(7) 0.1716(2) 0.0380(19) Uani 0.50 1 d PU . . O17 O 0.96007(17) 0.2506(3) 0.06783(15) 0.0458(12) Uani 1 1 d . . . O18 O 0.4341(4) 0.5536(7) 0.1910(3) 0.057(2) Uani 0.50 1 d PU . . O19 O 0.02615(18) 0.0547(3) 0.06436(16) 0.0495(12) Uani 1 1 d U . . O20 O 0.0917(4) 0.4248(8) 0.2911(3) 0.069(3) Uani 0.50 1 d PU . . O21 O 0.1132(7) 0.2596(14) 0.3136(6) 0.049(4) Uani 0.25 1 d PU . . O22 O 0.0523(7) 0.9644(14) 0.7068(7) 0.055(5) Uani 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01241(10) 0.01082(11) 0.00997(8) 0.00068(7) 0.00217(8) -0.00102(9) Cu1 0.0145(2) 0.0120(3) 0.0102(2) -0.00104(18) 0.00421(19) -0.0005(2) Cu2 0.0134(4) 0.0291(4) 0.0139(3) 0.000 0.0045(3) 0.000 C1 0.014(2) 0.016(2) 0.0093(16) 0.0038(15) 0.0005(16) 0.0042(18) C2 0.021(2) 0.016(2) 0.0129(17) -0.0009(16) 0.0042(17) 0.0056(19) C3 0.012(2) 0.012(2) 0.0153(18) -0.0018(16) 0.0007(16) -0.0021(18) C4 0.017(2) 0.017(2) 0.0105(17) 0.0023(16) 0.0031(16) -0.0008(19) C5 0.016(2) 0.013(2) 0.0091(16) -0.0037(15) 0.0025(16) 0.0030(18) C6 0.022(2) 0.011(2) 0.0116(17) -0.0011(15) 0.0056(17) 0.0055(19) C7 0.010(2) 0.016(2) 0.0155(18) 0.0022(16) 0.0040(16) 0.0007(18) C8 0.018(2) 0.011(2) 0.0095(16) -0.0004(15) 0.0025(16) -0.0001(18) C9 0.011(2) 0.016(2) 0.0121(17) 0.0003(16) 0.0017(16) 0.0035(18) C10 0.010(2) 0.013(2) 0.0154(17) -0.0008(15) 0.0049(16) 0.0012(17) C11 0.014(2) 0.019(2) 0.0193(19) -0.0017(17) 0.0025(18) 0.0015(19) C12 0.022(2) 0.016(2) 0.0189(18) -0.0009(16) 0.0119(17) -0.001(2) C13 0.026(2) 0.017(2) 0.0110(17) -0.0039(16) 0.0034(18) 0.006(2) C14 0.028(2) 0.005(2) 0.0157(18) 0.0008(15) 0.0044(18) 0.0018(19) C15 0.016(2) 0.020(2) 0.0137(18) -0.0004(17) 0.0016(17) 0.002(2) C16 0.012(2) 0.015(2) 0.0201(18) -0.0002(16) 0.0070(17) 0.0021(18) C17 0.018(2) 0.014(2) 0.0092(16) -0.0010(15) 0.0040(16) 0.0018(18) C18 0.019(2) 0.011(2) 0.0157(18) -0.0021(16) 0.0056(17) -0.0027(18) C19 0.024(2) 0.013(2) 0.0135(17) 0.0078(15) 0.0085(17) 0.0038(19) C20 0.017(2) 0.018(2) 0.0074(17) 0.0016(16) -0.0004(17) 0.0022(19) C21 0.025(2) 0.011(2) 0.0150(18) -0.0003(16) 0.0053(18) -0.0016(19) C22 0.024(2) 0.015(2) 0.0167(18) 0.0033(16) 0.0102(17) -0.001(2) C23 0.029(2) 0.015(2) 0.0161(18) -0.0004(16) 0.0102(18) -0.007(2) C24 0.013(2) 0.019(2) 0.0117(17) 0.0060(16) -0.0016(17) 0.0024(19) C25 0.012(2) 0.016(2) 0.0141(17) 0.0011(16) 0.0028(16) 0.0031(18) C26 0.020(2) 0.011(2) 0.0118(17) -0.0015(15) 0.0047(17) -0.0058(18) C27 0.016(2) 0.015(2) 0.0138(17) 0.0017(16) 0.0069(16) 0.0000(19) C28 0.020(2) 0.023(3) 0.0164(19) -0.0059(17) 0.0017(18) -0.003(2) C29 0.021(2) 0.023(2) 0.0126(18) -0.0103(17) 0.0029(17) -0.001(2) C30 0.014(2) 0.012(2) 0.0159(18) 0.0023(16) 0.0048(16) -0.0043(18) C31 0.011(2) 0.019(2) 0.0104(17) -0.0013(16) -0.0020(16) 0.0004(18) C32 0.014(2) 0.017(2) 0.0136(17) -0.0022(16) 0.0037(16) -0.0025(19) C33 0.019(2) 0.013(2) 0.0135(17) -0.0014(16) 0.0068(17) -0.0029(19) C34 0.018(2) 0.023(2) 0.0153(19) 0.0053(17) 0.0016(18) 0.005(2) C35 0.012(2) 0.026(2) 0.0180(18) 0.0050(17) 0.0062(17) 0.001(2) C36 0.018(2) 0.011(2) 0.0078(16) -0.0039(15) 0.0013(16) -0.0005(18) N1 0.0136(17) 0.0129(18) 0.0071(13) -0.0016(12) 0.0033(13) 0.0005(15) N2 0.0144(17) 0.0171(19) 0.0080(14) 0.0001(13) 0.0038(13) 0.0017(15) N3 0.0198(19) 0.0126(19) 0.0124(14) -0.0005(13) 0.0045(14) -0.0032(16) N4 0.0152(18) 0.0139(19) 0.0157(15) -0.0024(14) 0.0053(14) 0.0014(16) N5 0.0158(18) 0.020(2) 0.0135(14) -0.0010(14) 0.0079(14) 0.0041(16) N6 0.0150(18) 0.021(2) 0.0120(14) 0.0006(14) 0.0062(14) -0.0023(16) O1 0.0183(16) 0.0192(16) 0.0127(12) 0.0044(11) 0.0052(12) 0.0018(13) O2 0.0178(17) 0.038(2) 0.0284(15) 0.0165(14) 0.0077(14) 0.0035(16) O3 0.0179(18) 0.052(2) 0.0303(16) 0.0208(16) 0.0003(15) -0.0072(17) O4 0.0163(17) 0.0315(19) 0.0265(15) 0.0146(14) -0.0051(14) 0.0020(15) O5 0.0229(16) 0.0160(17) 0.0305(14) -0.0047(13) 0.0147(13) -0.0035(14) O6 0.0275(16) 0.0148(16) 0.0283(14) -0.0017(12) 0.0201(13) -0.0011(14) O7 0.053(2) 0.027(2) 0.0650(19) 0.0101(16) 0.0471(17) 0.0097(18) O8 0.0307(18) 0.0152(17) 0.0207(14) 0.0058(12) 0.0087(13) -0.0026(15) O9 0.0177(16) 0.0237(18) 0.0239(14) -0.0044(13) 0.0071(13) 0.0008(14) O10 0.0172(15) 0.0217(17) 0.0112(12) -0.0021(12) 0.0009(12) -0.0070(14) O11 0.0134(16) 0.0243(18) 0.0243(14) -0.0048(13) 0.0003(13) 0.0020(14) O12 0.0146(15) 0.0150(15) 0.0152(12) 0.0037(11) 0.0005(12) 0.0005(13) O13 0.0138(15) 0.0181(16) 0.0150(13) 0.0057(11) 0.0003(12) 0.0015(13) O14 0.045(3) 0.063(3) 0.079(3) 0.010(3) 0.016(3) -0.001(3) O14' 0.064(5) 0.055(5) 0.075(5) 0.000 0.004(4) 0.000 O15 0.062(3) 0.138(5) 0.074(3) -0.016(3) 0.030(2) -0.009(3) O16 0.037(3) 0.066(4) 0.014(2) 0.003(3) 0.013(2) -0.033(3) O17 0.036(2) 0.050(3) 0.047(2) 0.0097(19) 0.0083(18) -0.005(2) O18 0.053(4) 0.045(5) 0.085(4) 0.012(4) 0.038(4) 0.011(4) O19 0.047(2) 0.041(2) 0.064(2) -0.0063(19) 0.023(2) -0.009(2) O20 0.106(5) 0.049(5) 0.074(4) -0.002(4) 0.060(4) 0.002(4) O21 0.032(6) 0.048(7) 0.058(6) -0.012(5) 0.003(5) -0.006(5) O22 0.055(10) 0.047(11) 0.077(10) -0.011(8) 0.041(8) 0.004(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O4 2.260(3) . ? Eu1 O8 2.318(3) 3 ? Eu1 O10 2.369(3) . ? Eu1 O6 2.478(3) 3_545 ? Eu1 O13 2.480(3) 3_445 ? Eu1 O9 2.481(3) . ? Eu1 O5 2.486(3) 3_545 ? Eu1 O12 2.514(3) 3_445 ? Eu1 C24 2.822(5) 3_545 ? Eu1 C36 2.845(4) 3_445 ? Cu1 O1 1.943(3) 4_545 ? Cu1 N3 1.987(4) . ? Cu1 N2 2.000(3) . ? Cu1 N4 2.026(4) . ? Cu1 N1 2.179(4) . ? Cu2 O14' 1.960(18) . ? Cu2 N5 1.965(4) 2_756 ? Cu2 N5 1.965(4) . ? Cu2 N6 2.123(4) 2_756 ? Cu2 N6 2.123(4) . ? Cu2 O14 2.281(7) . ? Cu2 O14 2.281(7) 2_756 ? C1 N1 1.342(5) . ? C1 C2 1.371(6) . ? C2 C3 1.390(6) . ? C3 C4 1.405(6) . ? C3 C11 1.518(6) . ? C4 C5 1.375(6) . ? C5 N1 1.358(6) . ? C5 C6 1.491(5) . ? C6 N2 1.342(6) . ? C6 C7 1.398(6) . ? C7 C8 1.392(5) . ? C8 C9 1.376(6) . ? C8 C12 1.508(6) . ? C9 C10 1.389(6) . ? C10 N2 1.337(5) . ? C11 O3 1.224(6) . ? C11 O4 1.256(5) . ? C12 O2 1.249(6) . ? C12 O1 1.267(5) . ? C13 N3 1.348(6) . ? C13 C14 1.384(7) . ? C14 C15 1.394(7) . ? C15 C16 1.399(6) . ? C15 C23 1.503(7) . ? C16 C17 1.389(6) . ? C17 N3 1.357(6) . ? C17 C18 1.475(6) . ? C18 N4 1.345(6) . ? C18 C19 1.396(6) . ? C19 C20 1.381(6) . ? C20 C21 1.394(7) . ? C20 C24 1.520(6) . ? C21 C22 1.383(6) . ? C22 N4 1.345(6) . ? C23 O7 1.238(6) . ? C23 O8 1.262(5) . ? C24 O5 1.247(5) . ? C24 O6 1.264(6) . ? C24 Eu1 2.822(5) 3_455 ? C25 N5 1.362(6) . ? C25 C26 1.384(6) . ? C25 C31 1.487(5) 2_756 ? C26 C27 1.385(5) . ? C27 C28 1.388(7) . ? C27 C30 1.501(6) . ? C28 C29 1.376(6) . ? C29 N5 1.351(5) . ? C30 O11 1.246(6) . ? C30 O10 1.264(5) . ? C31 N6 1.352(6) . ? C31 C32 1.399(6) . ? C31 C25 1.487(5) 2_756 ? C32 C33 1.378(6) . ? C33 C34 1.393(6) . ? C33 C36 1.506(6) . ? C34 C35 1.388(6) . ? C35 N6 1.339(5) . ? C36 O13 1.250(5) . ? C36 O12 1.272(5) . ? C36 Eu1 2.845(4) 3 ? O1 Cu1 1.943(3) 4 ? O5 Eu1 2.486(3) 3_455 ? O6 Eu1 2.478(3) 3_455 ? O8 Eu1 2.318(3) 3_445 ? O12 Eu1 2.514(3) 3 ? O13 Eu1 2.480(3) 3 ? O14 O14' 1.424(7) . ? O14' O14 1.424(7) 2_756 ? 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 O4 Eu1 O8 80.34(11) . 3 ? O4 Eu1 O10 157.92(12) . . ? O8 Eu1 O10 78.20(10) 3 . ? O4 Eu1 O6 81.70(11) . 3_545 ? O8 Eu1 O6 132.03(11) 3 3_545 ? O10 Eu1 O6 109.19(10) . 3_545 ? O4 Eu1 O13 127.79(11) . 3_445 ? O8 Eu1 O13 147.49(9) 3 3_445 ? O10 Eu1 O13 74.23(10) . 3_445 ? O6 Eu1 O13 74.38(10) 3_545 3_445 ? O4 Eu1 O9 105.79(12) . . ? O8 Eu1 O9 80.75(11) 3 . ? O10 Eu1 O9 75.82(10) . . ? O6 Eu1 O9 147.14(11) 3_545 . ? O13 Eu1 O9 76.10(10) 3_445 . ? O4 Eu1 O5 87.01(12) . 3_545 ? O8 Eu1 O5 82.13(11) 3 3_545 ? O10 Eu1 O5 84.99(10) . 3_545 ? O6 Eu1 O5 52.78(10) 3_545 3_545 ? O13 Eu1 O5 111.89(10) 3_445 3_545 ? O9 Eu1 O5 156.48(10) . 3_545 ? O4 Eu1 O12 77.51(11) . 3_445 ? O8 Eu1 O12 139.33(11) 3 3_445 ? O10 Eu1 O12 122.95(9) . 3_445 ? O6 Eu1 O12 77.55(10) 3_545 3_445 ? O13 Eu1 O12 52.54(9) 3_445 3_445 ? O9 Eu1 O12 73.18(10) . 3_445 ? O5 Eu1 O12 129.69(10) 3_545 3_445 ? O4 Eu1 C24 84.50(12) . 3_545 ? O8 Eu1 C24 107.36(12) 3 3_545 ? O10 Eu1 C24 96.97(11) . 3_545 ? O6 Eu1 C24 26.58(12) 3_545 3_545 ? O13 Eu1 C24 92.91(11) 3_445 3_545 ? O9 Eu1 C24 168.08(11) . 3_545 ? O5 Eu1 C24 26.22(12) 3_545 3_545 ? O12 Eu1 C24 103.96(12) 3_445 3_545 ? O4 Eu1 C36 103.14(12) . 3_445 ? O8 Eu1 C36 152.93(12) 3 3_445 ? O10 Eu1 C36 98.33(11) . 3_445 ? O6 Eu1 C36 74.71(11) 3_545 3_445 ? O13 Eu1 C36 26.00(11) 3_445 3_445 ? O9 Eu1 C36 72.43(11) . 3_445 ? O5 Eu1 C36 124.61(11) 3_545 3_445 ? O12 Eu1 C36 26.54(10) 3_445 3_445 ? C24 Eu1 C36 99.71(13) 3_545 3_445 ? O1 Cu1 N3 92.88(14) 4_545 . ? O1 Cu1 N2 90.32(13) 4_545 . ? N3 Cu1 N2 167.41(15) . . ? O1 Cu1 N4 163.40(13) 4_545 . ? N3 Cu1 N4 81.22(15) . . ? N2 Cu1 N4 92.35(15) . . ? O1 Cu1 N1 94.18(13) 4_545 . ? N3 Cu1 N1 113.83(13) . . ? N2 Cu1 N1 78.03(13) . . ? N4 Cu1 N1 102.40(14) . . ? O14' Cu2 N5 92.88(11) . 2_756 ? O14' Cu2 N5 92.88(11) . . ? N5 Cu2 N5 174.2(2) 2_756 . ? O14' Cu2 N6 128.59(10) . 2_756 ? N5 Cu2 N6 96.62(14) 2_756 2_756 ? N5 Cu2 N6 79.75(14) . 2_756 ? O14' Cu2 N6 128.59(10) . . ? N5 Cu2 N6 79.75(14) 2_756 . ? N5 Cu2 N6 96.62(14) . . ? N6 Cu2 N6 102.8(2) 2_756 . ? O14' Cu2 O14 38.31(16) . . ? N5 Cu2 O14 90.26(18) 2_756 . ? N5 Cu2 O14 94.26(18) . . ? N6 Cu2 O14 165.9(2) 2_756 . ? N6 Cu2 O14 90.52(19) . . ? O14' Cu2 O14 38.31(16) . 2_756 ? N5 Cu2 O14 94.26(18) 2_756 2_756 ? N5 Cu2 O14 90.26(18) . 2_756 ? N6 Cu2 O14 90.52(19) 2_756 2_756 ? N6 Cu2 O14 165.86(19) . 2_756 ? O14 Cu2 O14 76.6(3) . 2_756 ? N1 C1 C2 123.6(4) . . ? C1 C2 C3 119.1(4) . . ? C2 C3 C4 118.2(4) . . ? C2 C3 C11 121.5(4) . . ? C4 C3 C11 120.3(4) . . ? C5 C4 C3 118.8(4) . . ? N1 C5 C4 122.9(4) . . ? N1 C5 C6 114.1(4) . . ? C4 C5 C6 122.8(4) . . ? N2 C6 C7 121.5(4) . . ? N2 C6 C5 115.9(4) . . ? C7 C6 C5 122.6(4) . . ? C8 C7 C6 117.9(4) . . ? C9 C8 C7 120.1(4) . . ? C9 C8 C12 119.4(4) . . ? C7 C8 C12 120.4(4) . . ? C8 C9 C10 118.7(4) . . ? N2 C10 C9 121.6(4) . . ? O3 C11 O4 126.4(4) . . ? O3 C11 C3 119.1(4) . . ? O4 C11 C3 114.5(4) . . ? O2 C12 O1 125.4(4) . . ? O2 C12 C8 120.1(4) . . ? O1 C12 C8 114.4(4) . . ? N3 C13 C14 122.3(4) . . ? C13 C14 C15 119.7(4) . . ? C14 C15 C16 117.8(4) . . ? C14 C15 C23 122.0(4) . . ? C16 C15 C23 120.1(4) . . ? C17 C16 C15 119.7(4) . . ? N3 C17 C16 121.7(4) . . ? N3 C17 C18 114.2(4) . . ? C16 C17 C18 124.1(4) . . ? N4 C18 C19 121.7(4) . . ? N4 C18 C17 115.6(4) . . ? C19 C18 C17 122.6(4) . . ? C20 C19 C18 118.8(4) . . ? C19 C20 C21 119.3(4) . . ? C19 C20 C24 120.3(4) . . ? C21 C20 C24 120.3(4) . . ? C22 C21 C20 118.7(4) . . ? N4 C22 C21 122.2(4) . . ? O7 C23 O8 126.8(5) . . ? O7 C23 C15 116.7(4) . . ? O8 C23 C15 116.5(4) . . ? O5 C24 O6 123.0(4) . . ? O5 C24 C20 120.1(4) . . ? O6 C24 C20 116.9(4) . . ? O5 C24 Eu1 61.7(2) . 3_455 ? O6 C24 Eu1 61.4(2) . 3_455 ? C20 C24 Eu1 174.7(3) . 3_455 ? N5 C25 C26 121.8(4) . . ? N5 C25 C31 113.9(4) . 2_756 ? C26 C25 C31 124.3(4) . 2_756 ? C25 C26 C27 119.4(4) . . ? C26 C27 C28 118.8(4) . . ? C26 C27 C30 122.1(4) . . ? C28 C27 C30 119.1(4) . . ? C29 C28 C27 119.5(4) . . ? N5 C29 C28 122.2(4) . . ? O11 C30 O10 126.3(4) . . ? O11 C30 C27 117.8(4) . . ? O10 C30 C27 115.8(4) . . ? N6 C31 C32 121.6(4) . . ? N6 C31 C25 115.7(4) . 2_756 ? C32 C31 C25 122.7(4) . 2_756 ? C33 C32 C31 119.2(4) . . ? C32 C33 C34 119.3(4) . . ? C32 C33 C36 119.4(4) . . ? C34 C33 C36 121.3(4) . . ? C35 C34 C33 118.3(4) . . ? N6 C35 C34 123.0(4) . . ? O13 C36 O12 122.5(4) . . ? O13 C36 C33 118.7(3) . . ? O12 C36 C33 118.8(4) . . ? O13 C36 Eu1 60.4(2) . 3 ? O12 C36 Eu1 62.1(2) . 3 ? C33 C36 Eu1 175.9(3) . 3 ? C1 N1 C5 117.3(4) . . ? C1 N1 Cu1 130.0(3) . . ? C5 N1 Cu1 112.6(2) . . ? C10 N2 C6 120.0(4) . . ? C10 N2 Cu1 121.9(3) . . ? C6 N2 Cu1 117.9(2) . . ? C13 N3 C17 118.7(4) . . ? C13 N3 Cu1 126.6(3) . . ? C17 N3 Cu1 114.4(3) . . ? C22 N4 C18 119.1(4) . . ? C22 N4 Cu1 128.0(3) . . ? C18 N4 Cu1 112.9(3) . . ? C29 N5 C25 118.3(4) . . ? C29 N5 Cu2 123.3(3) . . ? C25 N5 Cu2 118.3(3) . . ? C35 N6 C31 118.5(4) . . ? C35 N6 Cu2 129.1(3) . . ? C31 N6 Cu2 112.4(3) . . ? C12 O1 Cu1 117.9(3) . 4 ? C11 O4 Eu1 158.9(3) . . ? C24 O5 Eu1 92.1(3) . 3_455 ? C24 O6 Eu1 92.1(3) . 3_455 ? C23 O8 Eu1 148.3(3) . 3_445 ? C30 O10 Eu1 138.2(3) . . ? C36 O12 Eu1 91.4(3) . 3 ? C36 O13 Eu1 93.6(2) . 3 ? O14' O14 Cu2 58.5(8) . . ? O14 O14' O14 166.3(15) 2_756 . ? O14 O14' Cu2 83.2(8) 2_756 . ? O14 O14' Cu2 83.2(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.571 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.150 # Attachment '2.cif' data_r70726c _database_code_depnum_ccdc_archive 'CCDC 692740' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H29.50 Cu1.50 N6 O17.75 Tb' _chemical_formula_weight 1084.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.064(9) _cell_length_b 12.361(5) _cell_length_c 26.806(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.194(13) _cell_angle_gamma 90.00 _cell_volume 7843(5) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4304 _exptl_absorpt_coefficient_mu 2.682 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6735 _exptl_absorpt_correction_T_max 0.7390 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 29041 _diffrn_reflns_av_R_equivalents 0.0959 _diffrn_reflns_av_sigmaI/netI 0.0916 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6879 _reflns_number_gt 5897 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+69.3469P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6879 _refine_ls_number_parameters 596 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1202 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.010 _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 0.126776(7) 0.285123(15) 0.045556(8) 0.01035(5) Uani 1 1 d . . . Cu1 Cu -0.24725(2) 0.29015(4) -0.13443(2) 0.01229(12) Uani 1 1 d . . . Cu2 Cu 0.5000 0.24934(7) 0.2500 0.01812(19) Uani 1 2 d S . . C1 C 0.51598(18) 0.0939(4) 0.34651(18) 0.0224(12) Uani 1 1 d . . . H1 H 0.5554 0.1057 0.3549 0.027 Uiso 1 1 calc R . . C2 C 0.49831(17) 0.0269(4) 0.37839(17) 0.0203(12) Uani 1 1 d . . . H2 H 0.5248 -0.0066 0.4082 0.024 Uiso 1 1 calc R . . C3 C 0.44049(16) 0.0085(4) 0.36632(17) 0.0150(10) Uani 1 1 d . . . C4 C 0.40348(17) 0.0620(3) 0.32279(17) 0.0153(11) Uani 1 1 d . . . H4 H 0.3638 0.0541 0.3145 0.018 Uiso 1 1 calc R . . C5 C 0.42486(16) 0.1259(4) 0.29213(16) 0.0154(11) Uani 1 1 d . . . C6 C 0.38913(17) 0.1817(3) 0.24343(16) 0.0136(10) Uani 1 1 d . . . C7 C 0.33031(16) 0.1688(3) 0.22289(17) 0.0147(10) Uani 1 1 d . . . H7 H 0.3109 0.1263 0.2410 0.018 Uiso 1 1 calc R . . C8 C 0.30115(17) 0.2193(3) 0.17564(17) 0.0136(10) Uani 1 1 d . . . C9 C 0.33051(18) 0.2801(4) 0.15055(19) 0.0205(12) Uani 1 1 d . . . H9 H 0.3111 0.3151 0.1181 0.025 Uiso 1 1 calc R . . C10 C 0.38844(19) 0.2900(4) 0.17273(18) 0.0220(12) Uani 1 1 d . . . H10 H 0.4084 0.3321 0.1550 0.026 Uiso 1 1 calc R . . C11 C 0.23766(17) 0.2071(3) 0.14998(18) 0.0158(11) Uani 1 1 d . . . C12 C 0.41782(17) -0.0658(4) 0.39828(17) 0.0161(11) Uani 1 1 d . . . C13 C -0.11722(16) 0.3218(3) -0.06533(17) 0.0147(10) Uani 1 1 d . . . H13 H -0.1297 0.3755 -0.0463 0.018 Uiso 1 1 calc R . . C14 C -0.06024(18) 0.3018(4) -0.05136(18) 0.0200(12) Uani 1 1 d . . . H14 H -0.0342 0.3404 -0.0231 0.024 Uiso 1 1 calc R . . C15 C -0.04112(18) 0.2234(3) -0.07949(17) 0.0158(11) Uani 1 1 d . . . C16 C -0.08087(16) 0.1709(3) -0.12085(16) 0.0130(10) Uani 1 1 d . . . H16 H -0.0695 0.1173 -0.1407 0.016 Uiso 1 1 calc R . . C17 C -0.13793(17) 0.1977(3) -0.13294(17) 0.0144(10) Uani 1 1 d . . . C18 C -0.18167(16) 0.1532(3) -0.17909(16) 0.0137(10) Uani 1 1 d . . . C19 C -0.17207(17) 0.0741(3) -0.21226(16) 0.0154(10) Uani 1 1 d . . . H19 H -0.1358 0.0421 -0.2045 0.019 Uiso 1 1 calc R . . C20 C -0.21599(17) 0.0425(3) -0.25660(17) 0.0157(10) Uani 1 1 d . . . C21 C -0.26771(17) 0.0948(3) -0.26895(17) 0.0158(11) Uani 1 1 d . . . H21 H -0.2974 0.0792 -0.3008 0.019 Uiso 1 1 calc R . . C22 C -0.27491(17) 0.1701(3) -0.23360(17) 0.0152(10) Uani 1 1 d . . . H22 H -0.3107 0.2041 -0.2411 0.018 Uiso 1 1 calc R . . C23 C -0.20921(18) -0.0501(3) -0.29009(17) 0.0163(11) Uani 1 1 d . . . C24 C 0.02081(18) 0.2001(4) -0.06576(18) 0.0190(11) Uani 1 1 d . . . C25 C 0.22648(18) -0.0205(4) -0.07679(17) 0.0176(11) Uani 1 1 d . . . H25 H 0.2486 0.0217 -0.0923 0.021 Uiso 1 1 calc R . . C26 C 0.19997(18) 0.0295(4) -0.04581(17) 0.0176(11) Uani 1 1 d . . . H26 H 0.2049 0.1049 -0.0390 0.021 Uiso 1 1 calc R . . C27 C 0.16594(17) -0.0299(3) -0.02449(17) 0.0170(11) Uani 1 1 d . . . C28 C 0.16133(18) -0.1404(3) -0.03406(17) 0.0178(11) Uani 1 1 d . . . H28 H 0.1381 -0.1834 -0.0201 0.021 Uiso 1 1 calc R . . C29 C 0.19048(17) -0.1872(3) -0.06378(17) 0.0146(10) Uani 1 1 d . . . C30 C 0.19303(17) -0.3057(3) -0.07195(17) 0.0143(10) Uani 1 1 d . . . C31 C 0.16816(17) -0.3809(3) -0.04915(17) 0.0167(11) Uani 1 1 d . . . H31 H 0.1427 -0.3582 -0.0317 0.020 Uiso 1 1 calc R . . C32 C 0.17997(16) -0.4901(3) -0.05143(17) 0.0140(10) Uani 1 1 d . . . C33 C 0.21494(18) -0.5207(4) -0.07967(17) 0.0193(11) Uani 1 1 d . . . H33 H 0.2247 -0.5946 -0.0814 0.023 Uiso 1 1 calc R . . C34 C 0.23546(18) -0.4423(4) -0.10525(18) 0.0191(11) Uani 1 1 d . . . H34 H 0.2573 -0.4641 -0.1265 0.023 Uiso 1 1 calc R . . C35 C 0.1341(2) 0.0220(4) 0.00854(19) 0.0230(12) Uani 1 1 d . . . C36 C 0.15882(16) -0.5713(3) -0.02051(16) 0.0139(10) Uani 1 1 d . . . N1 N -0.23405(14) 0.1968(3) -0.18982(14) 0.0132(9) Uani 1 1 d . . . N2 N -0.15595(14) 0.2695(3) -0.10438(13) 0.0128(9) Uani 1 1 d . . . N3 N 0.48090(14) 0.1441(3) 0.30396(14) 0.0184(9) Uani 1 1 d . . . N4 N 0.41716(14) 0.2425(3) 0.21824(14) 0.0159(9) Uani 1 1 d . . . N5 N 0.22208(13) -0.1282(3) -0.08594(14) 0.0139(9) Uani 1 1 d . . . N6 N 0.22563(14) -0.3365(3) -0.10121(14) 0.0138(9) Uani 1 1 d . . . O1 O 0.45194(11) -0.1181(2) 0.43619(11) 0.0161(7) Uani 1 1 d . . . O2 O 0.36500(11) -0.0753(2) 0.38714(12) 0.0182(8) Uani 1 1 d . . . O3 O 0.21333(12) 0.1412(3) 0.17018(13) 0.0255(9) Uani 1 1 d . . . O4 O 0.21563(12) 0.2621(2) 0.10937(12) 0.0180(8) Uani 1 1 d . . . O5 O 0.5078(2) 0.3935(6) 0.1992(3) 0.068(2) Uani 0.75 1 d P . . O5' O 0.5000 0.4045(10) 0.2500 0.062(4) Uani 0.50 2 d SP . . O6 O 0.15123(13) 0.1144(3) 0.02670(13) 0.0253(9) Uani 1 1 d . . . O7 O 0.09484(16) -0.0295(3) 0.01575(17) 0.0538(11) Uani 1 1 d . . . O8 O 0.12229(13) -0.5417(2) -0.00049(13) 0.0239(8) Uani 1 1 d . . . O9 O 0.17926(12) -0.6652(2) -0.01402(12) 0.0210(8) Uani 1 1 d . . . O10 O 0.10672(13) 0.1872(3) 0.11599(14) 0.0295(9) Uani 1 1 d . . . O11 O 0.05258(13) 0.2484(3) -0.02669(13) 0.0261(9) Uani 1 1 d . . . O12 O 0.03643(14) 0.1353(3) -0.09353(14) 0.0436(11) Uani 1 1 d . . . O13 O -0.16221(13) -0.0915(3) -0.28315(13) 0.0305(9) Uani 1 1 d . . . O14 O -0.25498(11) -0.0820(2) -0.32385(11) 0.0172(8) Uani 1 1 d . . . O15 O 0.02429(17) 0.0548(3) 0.06414(18) 0.0545(13) Uani 1 1 d . . . O16 O 0.0857(3) 0.2602(8) 0.2077(3) 0.046(2) Uani 0.50 1 d P . . O17 O 0.0838(8) 0.4206(16) 0.2865(7) 0.0629(8) Uani 0.25 1 d PU . . O18 O 0.0259(3) 0.2420(7) 0.3284(3) 0.0845(8) Uani 0.75 1 d PU . . O19 O 0.03951(17) 0.2521(4) 0.43090(19) 0.0563(14) Uani 1 1 d . . . O20 O 0.9345(4) 0.9465(8) 0.6907(5) 0.087(3) Uani 0.50 1 d P . . O21 O 0.5484(7) 0.5345(16) 0.2032(7) 0.062(4) Uani 0.25 1 d PU . . 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 0.01036(9) 0.00893(10) 0.01095(10) -0.00065(8) 0.00243(7) 0.00020(7) Cu1 0.0146(2) 0.0114(2) 0.0112(3) 0.0010(2) 0.00476(19) 0.00011(19) Cu2 0.0126(3) 0.0264(4) 0.0148(4) 0.000 0.0037(3) 0.000 C1 0.0149(19) 0.029(3) 0.023(2) 0.002(2) 0.0055(17) -0.0031(18) C2 0.0112(18) 0.033(3) 0.013(2) 0.004(2) -0.0008(16) 0.0016(18) C3 0.0149(18) 0.017(2) 0.014(2) -0.0017(18) 0.0061(16) -0.0022(16) C4 0.0125(18) 0.016(2) 0.016(2) -0.0041(18) 0.0021(16) -0.0015(16) C5 0.0143(18) 0.018(2) 0.012(2) -0.0016(18) 0.0015(16) -0.0033(17) C6 0.0182(19) 0.0086(19) 0.013(2) -0.0040(17) 0.0032(16) -0.0029(16) C7 0.0128(18) 0.014(2) 0.015(2) -0.0015(18) 0.0002(16) 0.0004(16) C8 0.0188(19) 0.008(2) 0.013(2) -0.0060(16) 0.0034(17) 0.0002(16) C9 0.020(2) 0.017(2) 0.024(2) 0.0044(19) 0.0072(18) 0.0004(17) C10 0.026(2) 0.022(2) 0.018(2) 0.0074(19) 0.0073(18) 0.0008(18) C11 0.0160(19) 0.008(2) 0.019(2) -0.0019(17) 0.0005(17) -0.0014(16) C12 0.0167(19) 0.017(2) 0.015(2) -0.0044(18) 0.0064(16) 0.0005(17) C13 0.0170(18) 0.012(2) 0.015(2) -0.0041(17) 0.0055(16) -0.0028(16) C14 0.021(2) 0.020(2) 0.016(2) -0.0022(19) 0.0014(18) -0.0058(18) C15 0.022(2) 0.013(2) 0.011(2) -0.0014(17) 0.0040(17) 0.0005(17) C16 0.0129(17) 0.015(2) 0.010(2) -0.0027(17) 0.0027(15) 0.0007(16) C17 0.0165(18) 0.011(2) 0.017(2) 0.0003(17) 0.0064(16) -0.0034(16) C18 0.0131(17) 0.014(2) 0.014(2) 0.0048(17) 0.0039(15) -0.0035(16) C19 0.0167(18) 0.018(2) 0.013(2) -0.0022(18) 0.0064(16) -0.0022(17) C20 0.0200(19) 0.013(2) 0.017(2) -0.0004(18) 0.0090(17) -0.0031(17) C21 0.0166(19) 0.016(2) 0.012(2) 0.0036(18) 0.0004(16) -0.0038(17) C22 0.0176(19) 0.010(2) 0.016(2) 0.0006(18) 0.0026(16) -0.0014(16) C23 0.025(2) 0.010(2) 0.013(2) -0.0001(17) 0.0053(17) -0.0018(17) C24 0.019(2) 0.023(2) 0.013(2) 0.0025(19) 0.0028(17) 0.0020(18) C25 0.022(2) 0.015(2) 0.013(2) 0.0004(18) 0.0026(17) -0.0053(17) C26 0.028(2) 0.011(2) 0.013(2) 0.0024(17) 0.0062(18) -0.0004(17) C27 0.0211(19) 0.013(2) 0.018(2) 0.0003(18) 0.0081(17) 0.0007(17) C28 0.025(2) 0.013(2) 0.018(2) 0.0022(18) 0.0100(17) -0.0032(17) C29 0.0190(19) 0.010(2) 0.015(2) -0.0017(17) 0.0057(17) -0.0044(16) C30 0.0180(19) 0.011(2) 0.016(2) -0.0004(17) 0.0075(16) -0.0011(16) C31 0.0213(19) 0.014(2) 0.018(2) -0.0035(18) 0.0107(17) -0.0009(17) C32 0.0153(18) 0.013(2) 0.014(2) -0.0008(17) 0.0051(16) 0.0003(16) C33 0.024(2) 0.016(2) 0.018(2) -0.0012(19) 0.0071(18) 0.0027(18) C34 0.023(2) 0.017(2) 0.019(2) -0.0020(19) 0.0084(17) 0.0022(18) C35 0.037(2) 0.009(2) 0.025(2) -0.0048(19) 0.014(2) 0.0036(19) C36 0.0166(18) 0.012(2) 0.013(2) -0.0070(17) 0.0054(16) -0.0041(16) N1 0.0138(15) 0.0140(18) 0.0134(18) 0.0002(14) 0.0068(13) -0.0018(13) N2 0.0159(15) 0.0131(18) 0.0109(17) 0.0057(14) 0.0066(13) 0.0015(14) N3 0.0129(15) 0.024(2) 0.0167(19) 0.0014(16) 0.0028(14) -0.0004(15) N4 0.0161(16) 0.0200(19) 0.0139(18) 0.0038(15) 0.0080(14) -0.0007(15) N5 0.0135(15) 0.0112(18) 0.0173(18) -0.0007(15) 0.0053(14) -0.0021(13) N6 0.0190(16) 0.0072(17) 0.0166(18) 0.0027(15) 0.0077(14) -0.0017(14) O1 0.0133(13) 0.0161(15) 0.0169(15) 0.0064(13) 0.0022(11) 0.0031(11) O2 0.0142(13) 0.0211(16) 0.0185(15) 0.0091(13) 0.0043(12) -0.0026(12) O3 0.0163(14) 0.0267(18) 0.0274(18) 0.0091(15) -0.0009(13) -0.0021(13) O4 0.0157(13) 0.0172(15) 0.0175(16) -0.0022(13) 0.0008(12) 0.0019(12) O5 0.042(3) 0.090(5) 0.064(4) -0.014(4) 0.008(3) 0.012(3) O5' 0.059(8) 0.038(7) 0.067(9) 0.000 -0.011(7) 0.000 O6 0.0284(16) 0.0174(17) 0.0286(18) -0.0050(14) 0.0073(14) 0.0030(13) O7 0.078(2) 0.028(2) 0.087(3) -0.0104(19) 0.0702(19) -0.0126(18) O8 0.0393(16) 0.0101(15) 0.0312(17) 0.0017(13) 0.0237(14) 0.0004(13) O9 0.0256(14) 0.0085(15) 0.0323(17) 0.0048(13) 0.0143(13) 0.0029(12) O10 0.0218(15) 0.0348(19) 0.0347(19) 0.0125(16) 0.0129(14) 0.0026(14) O11 0.0190(15) 0.0291(18) 0.0225(18) -0.0100(15) -0.0036(13) 0.0008(14) O12 0.0196(16) 0.068(3) 0.037(2) -0.032(2) 0.0012(15) 0.0078(17) O13 0.0199(15) 0.036(2) 0.0335(19) -0.0166(16) 0.0056(14) 0.0012(14) O14 0.0162(13) 0.0178(16) 0.0180(15) -0.0047(13) 0.0064(12) -0.0030(12) O15 0.054(2) 0.041(2) 0.073(3) -0.008(2) 0.027(2) -0.009(2) O16 0.019(3) 0.108(7) 0.013(3) -0.010(4) 0.008(3) 0.000(4) O17 0.0633(10) 0.0628(10) 0.0629(11) -0.0001(7) 0.0211(7) 0.0002(7) O18 0.0849(10) 0.0851(10) 0.0839(10) -0.0005(7) 0.0282(7) 0.0021(7) O19 0.044(2) 0.056(3) 0.062(3) -0.017(2) 0.009(2) 0.002(2) O20 0.087(5) 0.056(6) 0.159(8) -0.036(6) 0.098(5) -0.029(5) O21 0.072(7) 0.060(7) 0.068(7) 0.009(6) 0.042(5) 0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O11 2.247(3) . ? Tb1 O6 2.300(3) . ? Tb1 O4 2.337(3) . ? Tb1 O10 2.430(4) . ? Tb1 O8 2.455(3) 1_565 ? Tb1 O2 2.456(3) 4 ? Tb1 O9 2.457(3) 1_565 ? Tb1 O1 2.489(3) 4 ? Tb1 C36 2.804(4) 1_565 ? Tb1 C12 2.832(5) 4 ? Cu1 O14 1.947(3) 4_454 ? Cu1 N5 1.989(4) 3_455 ? Cu1 N1 1.992(4) . ? Cu1 N6 2.025(4) 3_455 ? Cu1 N2 2.177(3) . ? Cu2 O5' 1.918(13) . ? Cu2 N4 1.970(3) 2_655 ? Cu2 N4 1.970(3) . ? Cu2 N3 2.114(4) 2_655 ? Cu2 N3 2.114(4) . ? Cu2 O5 2.289(7) 2_655 ? Cu2 O5 2.289(7) . ? C1 N3 1.341(5) . ? C1 C2 1.364(7) . ? C1 H1 0.9500 . ? C2 C3 1.396(6) . ? C2 H2 0.9500 . ? C3 C4 1.395(6) . ? C3 C12 1.490(6) . ? C4 C5 1.370(6) . ? C4 H4 0.9500 . ? C5 N3 1.353(5) . ? C5 C6 1.488(6) . ? C6 N4 1.351(6) . ? C6 C7 1.403(5) . ? C7 C8 1.386(6) . ? C7 H7 0.9500 . ? C8 C9 1.372(7) . ? C8 C11 1.519(6) . ? C9 C10 1.382(6) . ? C9 H9 0.9500 . ? C10 N4 1.332(6) . ? C10 H10 0.9500 . ? C11 O3 1.243(6) . ? C11 O4 1.247(5) . ? C12 O2 1.263(5) . ? C12 O1 1.269(5) . ? C12 Tb1 2.832(5) 4_545 ? C13 N2 1.337(5) . ? C13 C14 1.375(6) . ? C13 H13 0.9500 . ? C14 C15 1.406(7) . ? C14 H14 0.9500 . ? C15 C16 1.384(5) . ? C15 C24 1.501(6) . ? C16 C17 1.399(6) . ? C16 H16 0.9500 . ? C17 N2 1.344(6) . ? C17 C18 1.464(5) . ? C18 N1 1.360(5) . ? C18 C19 1.395(6) . ? C19 C20 1.384(5) . ? C19 H19 0.9500 . ? C20 C21 1.388(6) . ? C20 C23 1.498(6) . ? C21 C22 1.382(6) . ? C21 H21 0.9500 . ? C22 N1 1.321(5) . ? C22 H22 0.9500 . ? C23 O13 1.241(5) . ? C23 O14 1.268(5) . ? C24 O11 1.240(5) . ? C24 O12 1.241(6) . ? C25 N5 1.352(6) . ? C25 C26 1.370(7) . ? C25 H25 0.9500 . ? C26 C27 1.383(6) . ? C26 H26 0.9500 . ? C27 C28 1.388(6) . ? C27 C35 1.515(7) . ? C28 C29 1.373(7) . ? C28 H28 0.9500 . ? C29 N5 1.350(6) . ? C29 C30 1.485(6) . ? C30 N6 1.360(6) . ? C30 C31 1.370(6) . ? C31 C32 1.387(6) . ? C31 H31 0.9500 . ? C32 C33 1.386(7) . ? C32 C36 1.505(6) . ? C33 C34 1.380(7) . ? C33 H33 0.9500 . ? C34 N6 1.343(6) . ? C34 H34 0.9500 . ? C35 O7 1.239(6) . ? C35 O6 1.261(5) . ? C36 O9 1.258(5) . ? C36 O8 1.258(5) . ? C36 Tb1 2.804(4) 1_545 ? N5 Cu1 1.989(4) 3_545 ? N6 Cu1 2.025(4) 3_545 ? O1 Tb1 2.489(3) 4_545 ? O2 Tb1 2.456(3) 4_545 ? O5 O5' 1.443(7) . ? O5' O5 1.443(7) 2_655 ? O8 Tb1 2.455(3) 1_545 ? O9 Tb1 2.457(3) 1_545 ? O14 Cu1 1.947(3) 4_444 ? 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 O11 Tb1 O6 80.20(11) . . ? O11 Tb1 O4 157.79(12) . . ? O6 Tb1 O4 77.90(11) . . ? O11 Tb1 O10 104.19(12) . . ? O6 Tb1 O10 81.49(13) . . ? O4 Tb1 O10 76.19(11) . . ? O11 Tb1 O8 81.65(12) . 1_565 ? O6 Tb1 O8 131.39(12) . 1_565 ? O4 Tb1 O8 110.45(10) . 1_565 ? O10 Tb1 O8 146.90(12) . 1_565 ? O11 Tb1 O2 128.40(11) . 4 ? O6 Tb1 O2 147.38(10) . 4 ? O4 Tb1 O2 73.64(10) . 4 ? O10 Tb1 O2 76.58(12) . 4 ? O8 Tb1 O2 74.67(11) 1_565 4 ? O11 Tb1 O9 87.62(12) . 1_565 ? O6 Tb1 O9 81.26(11) . 1_565 ? O4 Tb1 O9 85.48(11) . 1_565 ? O10 Tb1 O9 157.06(10) . 1_565 ? O8 Tb1 O9 53.23(10) 1_565 1_565 ? O2 Tb1 O9 111.62(10) 4 1_565 ? O11 Tb1 O1 77.39(11) . 4 ? O6 Tb1 O1 140.34(11) . 4 ? O4 Tb1 O1 122.73(10) . 4 ? O10 Tb1 O1 72.95(11) . 4 ? O8 Tb1 O1 76.80(11) 1_565 4 ? O2 Tb1 O1 53.02(9) 4 4 ? O9 Tb1 O1 129.49(10) 1_565 4 ? O11 Tb1 C36 84.91(12) . 1_565 ? O6 Tb1 C36 106.83(13) . 1_565 ? O4 Tb1 C36 97.91(11) . 1_565 ? O10 Tb1 C36 168.80(12) . 1_565 ? O8 Tb1 C36 26.64(12) 1_565 1_565 ? O2 Tb1 C36 92.70(12) 4 1_565 ? O9 Tb1 C36 26.62(11) 1_565 1_565 ? O1 Tb1 C36 103.30(11) 4 1_565 ? O11 Tb1 C12 103.32(12) . 4 ? O6 Tb1 C12 153.43(13) . 4 ? O4 Tb1 C12 97.92(11) . 4 ? O10 Tb1 C12 72.08(13) . 4 ? O8 Tb1 C12 74.87(12) 1_565 4 ? O2 Tb1 C12 26.44(10) 4 4 ? O9 Tb1 C12 124.90(11) 1_565 4 ? O1 Tb1 C12 26.61(10) 4 4 ? C36 Tb1 C12 99.73(13) 1_565 4 ? O14 Cu1 N5 93.09(14) 4_454 3_455 ? O14 Cu1 N1 89.94(14) 4_454 . ? N5 Cu1 N1 167.31(13) 3_455 . ? O14 Cu1 N6 163.08(12) 4_454 3_455 ? N5 Cu1 N6 81.19(15) 3_455 3_455 ? N1 Cu1 N6 92.42(15) . 3_455 ? O14 Cu1 N2 94.72(12) 4_454 . ? N5 Cu1 N2 113.74(13) 3_455 . ? N1 Cu1 N2 78.23(13) . . ? N6 Cu1 N2 102.16(13) 3_455 . ? O5' Cu2 N4 92.47(11) . 2_655 ? O5' Cu2 N4 92.47(11) . . ? N4 Cu2 N4 175.1(2) 2_655 . ? O5' Cu2 N3 127.99(11) . 2_655 ? N4 Cu2 N3 79.96(14) 2_655 2_655 ? N4 Cu2 N3 96.97(14) . 2_655 ? O5' Cu2 N3 127.99(11) . . ? N4 Cu2 N3 96.97(14) 2_655 . ? N4 Cu2 N3 79.96(14) . . ? N3 Cu2 N3 104.0(2) 2_655 . ? O5' Cu2 O5 38.88(17) . 2_655 ? N4 Cu2 O5 93.47(18) 2_655 2_655 ? N4 Cu2 O5 90.37(18) . 2_655 ? N3 Cu2 O5 165.6(2) 2_655 2_655 ? N3 Cu2 O5 89.4(2) . 2_655 ? O5' Cu2 O5 38.88(17) . . ? N4 Cu2 O5 90.37(18) 2_655 . ? N4 Cu2 O5 93.47(18) . . ? N3 Cu2 O5 89.4(2) 2_655 . ? N3 Cu2 O5 165.6(2) . . ? O5 Cu2 O5 77.8(3) 2_655 . ? N3 C1 C2 123.8(4) . . ? N3 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C1 C2 C3 118.7(4) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 118.1(4) . . ? C4 C3 C12 119.9(4) . . ? C2 C3 C12 122.0(4) . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N3 C5 C4 122.4(4) . . ? N3 C5 C6 114.1(4) . . ? C4 C5 C6 123.5(4) . . ? N4 C6 C7 121.3(4) . . ? N4 C6 C5 115.8(3) . . ? C7 C6 C5 122.9(4) . . ? C8 C7 C6 118.5(4) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C9 C8 C7 119.2(4) . . ? C9 C8 C11 118.9(4) . . ? C7 C8 C11 121.9(4) . . ? C8 C9 C10 119.6(4) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N4 C10 C9 122.0(5) . . ? N4 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? O3 C11 O4 126.7(4) . . ? O3 C11 C8 117.3(4) . . ? O4 C11 C8 116.0(4) . . ? O2 C12 O1 121.3(4) . . ? O2 C12 C3 119.3(4) . . ? O1 C12 C3 119.4(4) . . ? O2 C12 Tb1 59.9(2) . 4_545 ? O1 C12 Tb1 61.5(2) . 4_545 ? C3 C12 Tb1 176.9(3) . 4_545 ? N2 C13 C14 123.2(4) . . ? N2 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C15 119.0(4) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 118.1(4) . . ? C16 C15 C24 121.4(4) . . ? C14 C15 C24 120.5(4) . . ? C15 C16 C17 119.1(4) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? N2 C17 C16 122.3(4) . . ? N2 C17 C18 115.5(4) . . ? C16 C17 C18 122.1(4) . . ? N1 C18 C19 120.0(3) . . ? N1 C18 C17 115.6(4) . . ? C19 C18 C17 124.3(4) . . ? C20 C19 C18 119.3(4) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 119.4(4) . . ? C19 C20 C23 121.0(4) . . ? C21 C20 C23 119.6(4) . . ? C22 C21 C20 118.2(4) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? N1 C22 C21 122.7(4) . . ? N1 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? O13 C23 O14 124.7(4) . . ? O13 C23 C20 121.0(4) . . ? O14 C23 C20 114.3(4) . . ? O11 C24 O12 125.1(4) . . ? O11 C24 C15 116.1(4) . . ? O12 C24 C15 118.8(4) . . ? N5 C25 C26 121.8(4) . . ? N5 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C27 119.9(4) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 118.1(4) . . ? C26 C27 C35 122.1(4) . . ? C28 C27 C35 119.8(4) . . ? C29 C28 C27 119.6(4) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? N5 C29 C28 121.9(4) . . ? N5 C29 C30 114.1(4) . . ? C28 C29 C30 123.9(4) . . ? N6 C30 C31 121.0(4) . . ? N6 C30 C29 115.1(4) . . ? C31 C30 C29 123.7(4) . . ? C30 C31 C32 120.4(4) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C33 C32 C31 118.1(4) . . ? C33 C32 C36 121.3(4) . . ? C31 C32 C36 120.4(4) . . ? C34 C33 C32 119.1(4) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? N6 C34 C33 122.4(4) . . ? N6 C34 H34 118.8 . . ? C33 C34 H34 118.8 . . ? O7 C35 O6 126.3(5) . . ? O7 C35 C27 118.2(4) . . ? O6 C35 C27 115.6(4) . . ? O9 C36 O8 122.0(4) . . ? O9 C36 C32 119.4(4) . . ? O8 C36 C32 118.6(4) . . ? O9 C36 Tb1 61.1(2) . 1_545 ? O8 C36 Tb1 61.0(2) . 1_545 ? C32 C36 Tb1 174.7(3) . 1_545 ? C22 N1 C18 120.1(4) . . ? C22 N1 Cu1 122.4(3) . . ? C18 N1 Cu1 117.2(3) . . ? C13 N2 C17 118.1(4) . . ? C13 N2 Cu1 129.6(3) . . ? C17 N2 Cu1 112.1(2) . . ? C1 N3 C5 117.5(4) . . ? C1 N3 Cu2 129.3(3) . . ? C5 N3 Cu2 113.1(3) . . ? C10 N4 C6 119.3(4) . . ? C10 N4 Cu2 123.5(3) . . ? C6 N4 Cu2 117.1(3) . . ? C29 N5 C25 118.5(4) . . ? C29 N5 Cu1 115.0(3) . 3_545 ? C25 N5 Cu1 126.3(3) . 3_545 ? C34 N6 C30 118.7(4) . . ? C34 N6 Cu1 128.4(3) . 3_545 ? C30 N6 Cu1 112.9(3) . 3_545 ? C12 O1 Tb1 91.9(2) . 4_545 ? C12 O2 Tb1 93.6(2) . 4_545 ? C11 O4 Tb1 138.3(3) . . ? O5' O5 Cu2 56.5(6) . . ? O5 O5' O5 169.2(12) 2_655 . ? O5 O5' Cu2 84.6(6) 2_655 . ? O5 O5' Cu2 84.6(6) . . ? C35 O6 Tb1 146.6(3) . . ? C36 O8 Tb1 92.3(3) . 1_545 ? C36 O9 Tb1 92.3(3) . 1_545 ? C24 O11 Tb1 160.9(3) . . ? C23 O14 Cu1 118.2(3) . 4_444 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C1 C2 C3 0.2(8) . . . . ? C1 C2 C3 C4 -1.5(7) . . . . ? C1 C2 C3 C12 178.3(4) . . . . ? C2 C3 C4 C5 3.1(7) . . . . ? C12 C3 C4 C5 -176.8(4) . . . . ? C3 C4 C5 N3 -3.5(7) . . . . ? C3 C4 C5 C6 176.8(4) . . . . ? N3 C5 C6 N4 -0.4(6) . . . . ? C4 C5 C6 N4 179.4(4) . . . . ? N3 C5 C6 C7 176.5(4) . . . . ? C4 C5 C6 C7 -3.7(7) . . . . ? N4 C6 C7 C8 0.4(7) . . . . ? C5 C6 C7 C8 -176.3(4) . . . . ? C6 C7 C8 C9 0.0(6) . . . . ? C6 C7 C8 C11 178.4(4) . . . . ? C7 C8 C9 C10 -0.1(7) . . . . ? C11 C8 C9 C10 -178.5(4) . . . . ? C8 C9 C10 N4 -0.2(7) . . . . ? C9 C8 C11 O3 171.4(4) . . . . ? C7 C8 C11 O3 -7.0(6) . . . . ? C9 C8 C11 O4 -6.1(6) . . . . ? C7 C8 C11 O4 175.4(4) . . . . ? C4 C3 C12 O2 -3.6(6) . . . . ? C2 C3 C12 O2 176.5(4) . . . . ? C4 C3 C12 O1 176.5(4) . . . . ? C2 C3 C12 O1 -3.3(7) . . . . ? C4 C3 C12 Tb1 71(5) . . . 4_545 ? C2 C3 C12 Tb1 -109(5) . . . 4_545 ? N2 C13 C14 C15 0.6(7) . . . . ? C13 C14 C15 C16 1.0(7) . . . . ? C13 C14 C15 C24 179.4(4) . . . . ? C14 C15 C16 C17 0.1(7) . . . . ? C24 C15 C16 C17 -178.2(4) . . . . ? C15 C16 C17 N2 -3.0(7) . . . . ? C15 C16 C17 C18 174.1(4) . . . . ? N2 C17 C18 N1 5.4(6) . . . . ? C16 C17 C18 N1 -171.8(4) . . . . ? N2 C17 C18 C19 -176.8(4) . . . . ? C16 C17 C18 C19 5.9(7) . . . . ? N1 C18 C19 C20 1.5(6) . . . . ? C17 C18 C19 C20 -176.2(4) . . . . ? C18 C19 C20 C21 3.9(7) . . . . ? C18 C19 C20 C23 -173.6(4) . . . . ? C19 C20 C21 C22 -5.9(7) . . . . ? C23 C20 C21 C22 171.6(4) . . . . ? C20 C21 C22 N1 2.5(7) . . . . ? C19 C20 C23 O13 -9.6(7) . . . . ? C21 C20 C23 O13 173.0(4) . . . . ? C19 C20 C23 O14 168.7(4) . . . . ? C21 C20 C23 O14 -8.8(6) . . . . ? C16 C15 C24 O11 -177.2(4) . . . . ? C14 C15 C24 O11 4.6(7) . . . . ? C16 C15 C24 O12 2.7(7) . . . . ? C14 C15 C24 O12 -175.5(5) . . . . ? N5 C25 C26 C27 -2.4(6) . . . . ? C25 C26 C27 C28 2.1(6) . . . . ? C25 C26 C27 C35 -177.9(4) . . . . ? C26 C27 C28 C29 0.3(6) . . . . ? C35 C27 C28 C29 -179.7(4) . . . . ? C27 C28 C29 N5 -2.6(6) . . . . ? C27 C28 C29 C30 173.7(4) . . . . ? N5 C29 C30 N6 -1.3(5) . . . . ? C28 C29 C30 N6 -177.9(4) . . . . ? N5 C29 C30 C31 174.2(4) . . . . ? C28 C29 C30 C31 -2.4(6) . . . . ? N6 C30 C31 C32 5.9(6) . . . . ? C29 C30 C31 C32 -169.3(4) . . . . ? C30 C31 C32 C33 -3.4(6) . . . . ? C30 C31 C32 C36 172.0(4) . . . . ? C31 C32 C33 C34 -1.5(6) . . . . ? C36 C32 C33 C34 -176.8(4) . . . . ? C32 C33 C34 N6 4.2(6) . . . . ? C26 C27 C35 O7 163.3(4) . . . . ? C28 C27 C35 O7 -16.7(6) . . . . ? C26 C27 C35 O6 -17.6(6) . . . . ? C28 C27 C35 O6 162.4(4) . . . . ? C33 C32 C36 O9 10.0(6) . . . . ? C31 C32 C36 O9 -165.2(4) . . . . ? C33 C32 C36 O8 -172.2(4) . . . . ? C31 C32 C36 O8 12.6(6) . . . . ? C33 C32 C36 Tb1 104(3) . . . 1_545 ? C31 C32 C36 Tb1 -71(3) . . . 1_545 ? C21 C22 N1 C18 2.9(7) . . . . ? C21 C22 N1 Cu1 -171.6(3) . . . . ? C19 C18 N1 C22 -4.9(6) . . . . ? C17 C18 N1 C22 173.0(4) . . . . ? C19 C18 N1 Cu1 169.9(3) . . . . ? C17 C18 N1 Cu1 -12.2(5) . . . . ? O14 Cu1 N1 C22 -80.0(3) 4_454 . . . ? N5 Cu1 N1 C22 23.9(9) 3_455 . . . ? N6 Cu1 N1 C22 83.3(3) 3_455 . . . ? N2 Cu1 N1 C22 -174.8(4) . . . . ? O14 Cu1 N1 C18 105.4(3) 4_454 . . . ? N5 Cu1 N1 C18 -150.7(6) 3_455 . . . ? N6 Cu1 N1 C18 -91.4(3) 3_455 . . . ? N2 Cu1 N1 C18 10.5(3) . . . . ? C14 C13 N2 C17 -3.4(7) . . . . ? C14 C13 N2 Cu1 -178.4(3) . . . . ? C16 C17 N2 C13 4.5(6) . . . . ? C18 C17 N2 C13 -172.7(4) . . . . ? C16 C17 N2 Cu1 -179.6(3) . . . . ? C18 C17 N2 Cu1 3.1(5) . . . . ? O14 Cu1 N2 C13 79.1(4) 4_454 . . . ? N5 Cu1 N2 C13 -16.4(4) 3_455 . . . ? N1 Cu1 N2 C13 168.0(4) . . . . ? N6 Cu1 N2 C13 -102.0(4) 3_455 . . . ? O14 Cu1 N2 C17 -96.2(3) 4_454 . . . ? N5 Cu1 N2 C17 168.3(3) 3_455 . . . ? N1 Cu1 N2 C17 -7.2(3) . . . . ? N6 Cu1 N2 C17 82.7(3) 3_455 . . . ? C2 C1 N3 C5 -0.5(7) . . . . ? C2 C1 N3 Cu2 -179.7(4) . . . . ? C4 C5 N3 C1 2.2(7) . . . . ? C6 C5 N3 C1 -178.1(4) . . . . ? C4 C5 N3 Cu2 -178.5(3) . . . . ? C6 C5 N3 Cu2 1.2(5) . . . . ? O5' Cu2 N3 C1 -96.8(4) . . . . ? N4 Cu2 N3 C1 1.8(4) 2_655 . . . ? N4 Cu2 N3 C1 177.9(4) . . . . ? N3 Cu2 N3 C1 83.2(4) 2_655 . . . ? O5 Cu2 N3 C1 -91.6(4) 2_655 . . . ? O5 Cu2 N3 C1 -118.3(7) . . . . ? O5' Cu2 N3 C5 84.0(3) . . . . ? N4 Cu2 N3 C5 -177.4(3) 2_655 . . . ? N4 Cu2 N3 C5 -1.3(3) . . . . ? N3 Cu2 N3 C5 -96.0(3) 2_655 . . . ? O5 Cu2 N3 C5 89.2(3) 2_655 . . . ? O5 Cu2 N3 C5 62.5(8) . . . . ? C9 C10 N4 C6 0.7(7) . . . . ? C9 C10 N4 Cu2 177.4(4) . . . . ? C7 C6 N4 C10 -0.7(7) . . . . ? C5 C6 N4 C10 176.2(4) . . . . ? C7 C6 N4 Cu2 -177.7(3) . . . . ? C5 C6 N4 Cu2 -0.8(5) . . . . ? O5' Cu2 N4 C10 56.1(4) . . . . ? N4 Cu2 N4 C10 -123.9(4) 2_655 . . . ? N3 Cu2 N4 C10 -72.7(4) 2_655 . . . ? N3 Cu2 N4 C10 -175.8(4) . . . . ? O5 Cu2 N4 C10 94.9(4) 2_655 . . . ? O5 Cu2 N4 C10 17.1(4) . . . . ? O5' Cu2 N4 C6 -127.1(3) . . . . ? N4 Cu2 N4 C6 52.9(3) 2_655 . . . ? N3 Cu2 N4 C6 104.2(3) 2_655 . . . ? N3 Cu2 N4 C6 1.1(3) . . . . ? O5 Cu2 N4 C6 -88.2(4) 2_655 . . . ? O5 Cu2 N4 C6 -166.0(4) . . . . ? C28 C29 N5 C25 2.4(6) . . . . ? C30 C29 N5 C25 -174.3(3) . . . . ? C28 C29 N5 Cu1 -172.7(3) . . . 3_545 ? C30 C29 N5 Cu1 10.6(4) . . . 3_545 ? C26 C25 N5 C29 0.1(6) . . . . ? C26 C25 N5 Cu1 174.7(3) . . . 3_545 ? C33 C34 N6 C30 -1.8(6) . . . . ? C33 C34 N6 Cu1 179.0(3) . . . 3_545 ? C31 C30 N6 C34 -3.3(6) . . . . ? C29 C30 N6 C34 172.3(3) . . . . ? C31 C30 N6 Cu1 176.0(3) . . . 3_545 ? C29 C30 N6 Cu1 -8.3(4) . . . 3_545 ? O2 C12 O1 Tb1 3.5(4) . . . 4_545 ? C3 C12 O1 Tb1 -176.6(4) . . . 4_545 ? O1 C12 O2 Tb1 -3.5(4) . . . 4_545 ? C3 C12 O2 Tb1 176.6(4) . . . 4_545 ? O3 C11 O4 Tb1 -1.4(8) . . . . ? C8 C11 O4 Tb1 175.9(3) . . . . ? O11 Tb1 O4 C11 -79.4(6) . . . . ? O6 Tb1 O4 C11 -69.8(4) . . . . ? O10 Tb1 O4 C11 14.3(4) . . . . ? O8 Tb1 O4 C11 160.3(4) 1_565 . . . ? O2 Tb1 O4 C11 94.1(4) 4 . . . ? O9 Tb1 O4 C11 -151.8(4) 1_565 . . . ? O1 Tb1 O4 C11 73.2(5) 4 . . . ? C36 Tb1 O4 C11 -175.4(4) 1_565 . . . ? C12 Tb1 O4 C11 83.6(5) 4 . . . ? N4 Cu2 O5 O5' -93.5(2) 2_655 . . . ? N4 Cu2 O5 O5' 89.6(2) . . . . ? N3 Cu2 O5 O5' -173.43(19) 2_655 . . . ? N3 Cu2 O5 O5' 27.4(8) . . . . ? O5 Cu2 O5 O5' 0.000(2) 2_655 . . . ? Cu2 O5 O5' O5 0.001(12) . . . 2_655 ? N4 Cu2 O5' O5 -92.5(2) 2_655 . . 2_655 ? N4 Cu2 O5' O5 87.5(2) . . . 2_655 ? N3 Cu2 O5' O5 -171.6(2) 2_655 . . 2_655 ? N3 Cu2 O5' O5 8.4(2) . . . 2_655 ? O5 Cu2 O5' O5 180.000(2) . . . 2_655 ? N4 Cu2 O5' O5 87.5(2) 2_655 . . . ? N4 Cu2 O5' O5 -92.5(2) . . . . ? N3 Cu2 O5' O5 8.4(2) 2_655 . . . ? N3 Cu2 O5' O5 -171.6(2) . . . . ? O5 Cu2 O5' O5 180.000(3) 2_655 . . . ? O7 C35 O6 Tb1 -39.9(9) . . . . ? C27 C35 O6 Tb1 141.1(5) . . . . ? O11 Tb1 O6 C35 -33.1(6) . . . . ? O4 Tb1 O6 C35 150.6(6) . . . . ? O10 Tb1 O6 C35 73.0(6) . . . . ? O8 Tb1 O6 C35 -102.7(6) 1_565 . . . ? O2 Tb1 O6 C35 121.0(6) 4 . . . ? O9 Tb1 O6 C35 -122.1(6) 1_565 . . . ? O1 Tb1 O6 C35 23.2(7) 4 . . . ? C36 Tb1 O6 C35 -114.6(6) 1_565 . . . ? C12 Tb1 O6 C35 67.2(7) 4 . . . ? O9 C36 O8 Tb1 3.7(4) . . . 1_545 ? C32 C36 O8 Tb1 -174.0(3) . . . 1_545 ? O8 C36 O9 Tb1 -3.7(4) . . . 1_545 ? C32 C36 O9 Tb1 174.0(3) . . . 1_545 ? O12 C24 O11 Tb1 -30.5(14) . . . . ? C15 C24 O11 Tb1 149.4(8) . . . . ? O6 Tb1 O11 C24 -1.6(11) . . . . ? O4 Tb1 O11 C24 8.1(13) . . . . ? O10 Tb1 O11 C24 -80.1(11) . . . . ? O8 Tb1 O11 C24 133.1(11) 1_565 . . . ? O2 Tb1 O11 C24 -164.1(10) 4 . . . ? O9 Tb1 O11 C24 80.0(11) 1_565 . . . ? O1 Tb1 O11 C24 -148.6(11) 4 . . . ? C36 Tb1 O11 C24 106.5(11) 1_565 . . . ? C12 Tb1 O11 C24 -154.7(11) 4 . . . ? O13 C23 O14 Cu1 3.4(6) . . . 4_444 ? C20 C23 O14 Cu1 -174.7(3) . . . 4_444 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.706 _refine_diff_density_min -1.342 _refine_diff_density_rms 0.173 # Attachment '1.cif' data_r70726d _database_code_depnum_ccdc_archive 'CCDC 692741' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H31.50 Cu1.50 Gd N6 O18.75' _chemical_formula_weight 1100.73 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.1360(17) _cell_length_b 12.4100(9) _cell_length_c 26.8552(13) _cell_angle_alpha 90.00 _cell_angle_beta 109.110(3) _cell_angle_gamma 90.00 _cell_volume 7915.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8826 _cell_measurement_theta_min 1.6380 _cell_measurement_theta_max 27.9163 _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.2400 _exptl_crystal_size_mid 0.1600 _exptl_crystal_size_min 0.1400 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4376 _exptl_absorpt_coefficient_mu 2.550 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8184 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ???? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 29444 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.10 _reflns_number_total 7040 _reflns_number_gt 6527 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+81.8916P] 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 0.000071(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7040 _refine_ls_number_parameters 606 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.088 _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 Gd1 Gd 0.373315(6) 0.215076(12) 0.454617(5) 0.01026(4) Uani 1 1 d . . . Cu1 Cu 0.747173(15) 0.20973(3) 0.634592(14) 0.01215(9) Uani 1 1 d . . . Cu2 Cu 0.0000 0.25069(5) 0.2500 0.01845(13) Uani 1 2 d S . . C1 C 0.68209(12) 0.3472(3) 0.67989(11) 0.0136(7) Uani 1 1 d . . . C2 C 0.67234(12) 0.4265(3) 0.71227(12) 0.0144(7) Uani 1 1 d . . . H2 H 0.6370 0.4581 0.7044 0.017 Uiso 1 1 d R . . C3 C 0.71620(12) 0.4577(3) 0.75676(11) 0.0140(7) Uani 1 1 d . . . C4 C 0.76766(12) 0.4055(3) 0.76892(12) 0.0155(7) Uani 1 1 d . . . H4 H 0.7965 0.4210 0.8000 0.019 Uiso 1 1 d R . . C5 C 0.77512(13) 0.3302(3) 0.73414(12) 0.0162(7) Uani 1 1 d . . . H5 H 0.8100 0.2969 0.7417 0.019 Uiso 1 1 d R . . C6 C 0.63770(13) 0.3029(3) 0.63308(12) 0.0147(7) Uani 1 1 d . . . C7 C 0.58129(12) 0.3286(3) 0.62118(12) 0.0149(7) Uani 1 1 d . . . H7 H 0.5701 0.3802 0.6409 0.018 Uiso 1 1 d R . . C8 C 0.54152(13) 0.2768(3) 0.57975(12) 0.0167(8) Uani 1 1 d . . . C9 C 0.56005(13) 0.1990(3) 0.55164(12) 0.0192(8) Uani 1 1 d . . . H9 H 0.5344 0.1615 0.5241 0.023 Uiso 1 1 d R . . C10 C 0.61714(13) 0.1787(3) 0.56535(12) 0.0181(8) Uani 1 1 d . . . H10 H 0.6293 0.1270 0.5464 0.022 Uiso 1 1 d R . . C11 C 0.70948(13) 0.5506(3) 0.79013(12) 0.0172(8) Uani 1 1 d . . . C12 C 0.47902(13) 0.3008(3) 0.56614(12) 0.0190(8) Uani 1 1 d . . . C13 C 0.11093(12) 0.3191(3) 0.25670(12) 0.0139(7) Uani 1 1 d . . . C14 C 0.16934(12) 0.3311(3) 0.27709(12) 0.0151(7) Uani 1 1 d . . . H14 H 0.1883 0.3721 0.2593 0.018 Uiso 1 1 d R . . C15 C 0.19858(13) 0.2806(3) 0.32439(12) 0.0149(7) Uani 1 1 d . . . C16 C 0.16885(14) 0.2196(3) 0.34945(13) 0.0197(8) Uani 1 1 d . . . H16 H 0.1877 0.1855 0.3812 0.024 Uiso 1 1 d R . . C17 C 0.11158(14) 0.2093(3) 0.32715(13) 0.0212(8) Uani 1 1 d . . . H17 H 0.0921 0.1673 0.3441 0.025 Uiso 1 1 d R . . C18 C 0.07491(12) 0.3736(3) 0.20762(12) 0.0152(7) Uani 1 1 d . . . C19 C 0.09612(12) 0.4388(3) 0.17700(12) 0.0152(7) Uani 1 1 d . . . H19 H 0.1348 0.4479 0.1853 0.018 Uiso 1 1 d R . . C20 C 0.05917(12) 0.4912(3) 0.13366(12) 0.0161(7) Uani 1 1 d . . . C21 C 0.00175(13) 0.4740(3) 0.12189(13) 0.0212(8) Uani 1 1 d . . . H21 H -0.0240 0.5081 0.0932 0.025 Uiso 1 1 d R . . C22 C -0.01622(13) 0.4055(3) 0.15351(13) 0.0226(9) Uani 1 1 d . . . H22 H -0.0546 0.3930 0.1450 0.027 Uiso 1 1 d R . . C23 C 0.26159(13) 0.2939(3) 0.34941(12) 0.0169(8) Uani 1 1 d . . . C24 C 0.08198(12) 0.5659(3) 0.10130(11) 0.0147(7) Uani 1 1 d . . . C25 C 0.30658(12) -0.1941(3) 0.57210(11) 0.0141(7) Uani 1 1 d . . . C26 C 0.33183(13) -0.1190(3) 0.54889(12) 0.0167(7) Uani 1 1 d . . . H26 H 0.3567 -0.1410 0.5317 0.020 Uiso 1 1 d R . . C27 C 0.31959(12) -0.0105(3) 0.55159(12) 0.0150(7) Uani 1 1 d . . . C28 C 0.28442(13) 0.0193(3) 0.57957(12) 0.0171(8) Uani 1 1 d . . . H28 H 0.2746 0.0912 0.5811 0.021 Uiso 1 1 d R . . C29 C 0.26425(13) -0.0581(3) 0.60513(12) 0.0176(8) Uani 1 1 d . . . H29 H 0.2431 -0.0368 0.6260 0.021 Uiso 1 1 calc R . . C30 C 0.30919(13) -0.3123(3) 0.56390(12) 0.0149(7) Uani 1 1 d . . . C31 C 0.33875(13) -0.3593(3) 0.53424(12) 0.0185(8) Uani 1 1 d . . . H31 H 0.3613 -0.3171 0.5206 0.022 Uiso 1 1 d R . . C32 C 0.33446(13) -0.4694(3) 0.52478(12) 0.0186(8) Uani 1 1 d . . . C33 C 0.30050(13) -0.5297(3) 0.54623(12) 0.0174(8) Uani 1 1 d . . . H33 H 0.2958 -0.6033 0.5398 0.021 Uiso 1 1 d R . . C34 C 0.27389(13) -0.4786(3) 0.57711(12) 0.0161(8) Uani 1 1 d . . . H34 H 0.2524 -0.5194 0.5924 0.019 Uiso 1 1 d R . . C35 C 0.34072(13) 0.0710(3) 0.52057(12) 0.0162(8) Uani 1 1 d . . . C36 C 0.36608(15) -0.5214(3) 0.49168(13) 0.0237(8) Uani 1 1 d . . . N1 N 0.73390(10) 0.3031(2) 0.68985(10) 0.0132(6) Uani 1 1 d . . . N2 N 0.65575(10) 0.2302(2) 0.60470(10) 0.0149(6) Uani 1 1 d . . . N3 N 0.08275(10) 0.2582(2) 0.28142(10) 0.0170(6) Uani 1 1 d . . . N4 N 0.01909(10) 0.3561(2) 0.19592(10) 0.0170(7) Uani 1 1 d . . . N5 N 0.27403(10) -0.1641(2) 0.60104(10) 0.0147(6) Uani 1 1 d . . . N6 N 0.27788(10) -0.3719(2) 0.58600(10) 0.0137(6) Uani 1 1 d . . . O1 O 0.75519(9) 0.58210(18) 0.82388(8) 0.0181(5) Uani 1 1 d . . . O2 O 0.66238(10) 0.5909(2) 0.78321(10) 0.0296(7) Uani 1 1 d . . . O3 O 0.46419(10) 0.3658(3) 0.59394(11) 0.0419(8) Uani 1 1 d . . . O4 O 0.44739(10) 0.2517(2) 0.52708(10) 0.0296(7) Uani 1 1 d . . . O5 O 0.28393(9) 0.23798(19) 0.39068(8) 0.0184(6) Uani 1 1 d . . . O6 O 0.28598(9) 0.3587(2) 0.32906(10) 0.0263(6) Uani 1 1 d . . . O7 O 0.13446(8) 0.57474(19) 0.11274(8) 0.0183(6) Uani 1 1 d . . . O8 O 0.04801(9) 0.61841(18) 0.06421(8) 0.0178(5) Uani 1 1 d . . . O9 O 0.31987(9) 0.16395(19) 0.51385(9) 0.0219(6) Uani 1 1 d . . . O10 O 0.37708(9) 0.04073(18) 0.50045(9) 0.0218(6) Uani 1 1 d . . . O11 O 0.40537(13) -0.4694(2) 0.48458(12) 0.0545(8) Uani 1 1 d . . . O12 O 0.34905(10) -0.61342(19) 0.47349(9) 0.0244(6) Uani 1 1 d . . . O13 O 0.39298(10) 0.3130(2) 0.38325(10) 0.0294(7) Uani 1 1 d . . . O14 O -0.0081(2) 0.1052(4) 0.29943(19) 0.0649(7) Uani 0.75 1 d PU . . O19 O 0.52462(13) 0.4444(3) 0.06368(15) 0.0583(10) Uani 1 1 d . . . O15 O 0.46063(13) 0.7513(3) 0.56861(14) 0.0542(10) Uani 1 1 d . . . O16 O 0.4143(2) 0.2378(6) 0.2926(2) 0.093(2) Uani 0.75 1 d P . . O17 O 0.9740(2) 0.7610(6) 0.17239(19) 0.101(2) Uani 0.75 1 d P . . O18 O 0.0661(3) 0.9454(6) 0.3094(4) 0.094(2) Uani 0.50 1 d P . . O20 O 0.4128(6) 0.0785(12) 0.2112(5) 0.0558(8) Uani 0.25 1 d PU . . O21 O 0.9481(5) 0.9606(10) 0.2933(5) 0.048(3) Uani 0.25 1 d P . . O22 O 0.8882(5) 0.7405(11) 0.1904(5) 0.0491(8) Uani 0.25 1 d PU . . O14' O 0.0000 0.0921(8) 0.2500 0.065(3) Uani 0.50 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01030(6) 0.00958(7) 0.01014(7) -0.00052(5) 0.00231(5) 0.00079(5) Cu1 0.01426(16) 0.01220(18) 0.01058(16) 0.00129(14) 0.00485(13) 0.00031(14) Cu2 0.0132(2) 0.0279(3) 0.0145(2) 0.000 0.00500(19) 0.000 C1 0.0136(13) 0.0154(16) 0.0117(13) -0.0012(12) 0.0043(11) -0.0043(12) C2 0.0126(13) 0.0161(16) 0.0159(14) 0.0011(12) 0.0064(11) -0.0006(12) C3 0.0188(13) 0.0124(15) 0.0130(13) -0.0010(12) 0.0083(11) -0.0032(12) C4 0.0167(13) 0.0176(16) 0.0113(13) 0.0008(12) 0.0031(11) -0.0040(13) C5 0.0136(13) 0.0182(16) 0.0157(14) -0.0001(13) 0.0031(11) -0.0001(13) C6 0.0177(13) 0.0149(16) 0.0122(14) -0.0012(12) 0.0057(11) -0.0028(12) C7 0.0156(13) 0.0148(15) 0.0123(14) -0.0013(12) 0.0018(11) -0.0010(12) C8 0.0185(14) 0.0184(17) 0.0134(14) 0.0007(12) 0.0056(12) -0.0023(13) C9 0.0196(15) 0.0222(18) 0.0149(14) -0.0030(13) 0.0045(12) -0.0057(13) C10 0.0215(14) 0.0181(16) 0.0158(14) -0.0051(13) 0.0079(12) -0.0066(13) C11 0.0220(14) 0.0158(16) 0.0158(14) -0.0021(13) 0.0089(12) -0.0015(13) C12 0.0146(14) 0.0238(18) 0.0148(15) 0.0022(13) -0.0003(12) -0.0005(13) C13 0.0148(13) 0.0135(15) 0.0135(14) -0.0008(12) 0.0047(11) -0.0021(12) C14 0.0155(13) 0.0144(16) 0.0153(14) 0.0015(12) 0.0050(11) -0.0016(12) C15 0.0156(14) 0.0123(15) 0.0149(14) -0.0034(12) 0.0024(12) 0.0020(12) C16 0.0235(15) 0.0181(17) 0.0171(15) 0.0052(13) 0.0060(13) 0.0022(13) C17 0.0227(15) 0.0234(18) 0.0190(15) 0.0087(14) 0.0090(12) 0.0015(14) C18 0.0149(13) 0.0172(16) 0.0124(14) -0.0008(12) 0.0030(11) -0.0005(12) C19 0.0119(13) 0.0181(16) 0.0143(14) 0.0002(13) 0.0026(11) -0.0015(12) C20 0.0151(13) 0.0192(17) 0.0149(14) -0.0001(13) 0.0063(11) -0.0006(13) C21 0.0143(14) 0.0262(18) 0.0200(16) 0.0071(14) 0.0015(12) 0.0006(14) C22 0.0095(13) 0.037(2) 0.0193(16) 0.0056(15) 0.0025(12) -0.0025(14) C23 0.0180(14) 0.0130(16) 0.0172(15) -0.0033(13) 0.0024(12) 0.0017(12) C24 0.0160(13) 0.0162(16) 0.0104(13) 0.0001(12) 0.0023(11) 0.0003(12) C25 0.0177(13) 0.0146(16) 0.0103(13) -0.0006(12) 0.0048(11) -0.0005(12) C26 0.0205(14) 0.0155(16) 0.0156(14) -0.0043(13) 0.0080(12) -0.0005(13) C27 0.0169(13) 0.0151(16) 0.0129(14) -0.0007(12) 0.0046(11) -0.0030(12) C28 0.0211(14) 0.0137(16) 0.0171(15) -0.0003(13) 0.0071(12) 0.0035(13) C29 0.0228(14) 0.0162(16) 0.0175(14) -0.0008(13) 0.0114(12) 0.0011(13) C30 0.0175(13) 0.0142(16) 0.0125(14) 0.0003(12) 0.0043(11) -0.0017(12) C31 0.0256(15) 0.0146(16) 0.0184(15) 0.0015(13) 0.0113(12) -0.0020(13) C32 0.0239(15) 0.0161(16) 0.0146(14) -0.0016(13) 0.0047(12) -0.0009(13) C33 0.0247(15) 0.0102(15) 0.0151(14) 0.0009(12) 0.0035(12) -0.0016(13) C34 0.0186(14) 0.0129(16) 0.0147(14) 0.0015(12) 0.0025(12) -0.0055(12) C35 0.0180(14) 0.0155(16) 0.0145(14) -0.0022(13) 0.0045(12) -0.0037(13) C36 0.0404(18) 0.0151(17) 0.0198(15) 0.0012(13) 0.0154(14) 0.0062(15) N1 0.0149(11) 0.0144(13) 0.0104(11) -0.0004(10) 0.0044(9) -0.0011(10) N2 0.0169(11) 0.0158(14) 0.0124(12) 0.0007(10) 0.0055(10) -0.0024(10) N3 0.0174(12) 0.0204(14) 0.0157(12) 0.0030(11) 0.0088(10) -0.0017(11) N4 0.0130(11) 0.0243(15) 0.0130(12) 0.0021(11) 0.0031(10) -0.0039(11) N5 0.0167(11) 0.0114(13) 0.0166(12) 0.0015(11) 0.0062(10) -0.0007(10) N6 0.0163(11) 0.0109(13) 0.0132(11) 0.0027(10) 0.0039(10) -0.0002(10) O1 0.0192(10) 0.0187(12) 0.0158(10) -0.0062(9) 0.0047(8) -0.0029(9) O2 0.0195(11) 0.0345(14) 0.0325(13) -0.0159(11) 0.0053(10) 0.0028(11) O3 0.0197(12) 0.067(2) 0.0336(14) -0.0266(14) 0.0009(11) 0.0074(13) O4 0.0171(11) 0.0318(14) 0.0310(13) -0.0163(12) -0.0043(10) -0.0022(11) O5 0.0167(10) 0.0212(12) 0.0142(10) -0.0008(9) 0.0009(8) 0.0055(9) O6 0.0186(11) 0.0254(13) 0.0295(12) 0.0091(11) 0.0005(10) -0.0036(10) O7 0.0122(9) 0.0234(12) 0.0176(10) 0.0058(9) 0.0027(8) -0.0021(9) O8 0.0137(9) 0.0203(12) 0.0177(10) 0.0061(9) 0.0027(8) 0.0000(9) O9 0.0232(10) 0.0146(12) 0.0325(12) 0.0063(10) 0.0152(9) 0.0027(9) O10 0.0321(11) 0.0134(11) 0.0289(11) 0.0010(9) 0.0222(9) 0.0016(10) O11 0.0842(16) 0.0283(16) 0.0835(17) -0.0156(14) 0.0718(13) -0.0151(14) O12 0.0293(12) 0.0152(12) 0.0258(12) -0.0056(10) 0.0050(10) 0.0063(10) O13 0.0256(11) 0.0336(14) 0.0317(13) 0.0073(11) 0.0132(10) 0.0005(11) O14 0.0640(9) 0.0659(9) 0.0650(9) -0.0007(7) 0.0213(6) 0.0010(7) O19 0.0564(17) 0.0375(18) 0.090(2) 0.0135(17) 0.0365(16) 0.0099(15) O15 0.0410(16) 0.056(2) 0.063(2) 0.0118(17) 0.0133(15) -0.0055(16) O16 0.039(2) 0.186(7) 0.052(3) -0.018(4) 0.013(2) -0.011(3) O17 0.111(3) 0.154(5) 0.048(3) 0.020(3) 0.040(2) 0.088(3) O18 0.092(4) 0.062(5) 0.172(6) 0.052(4) 0.104(4) 0.037(4) O20 0.0566(10) 0.0556(10) 0.0559(11) 0.0001(7) 0.0190(7) 0.0002(7) O21 0.052(6) 0.033(6) 0.076(7) 0.015(6) 0.043(5) 0.017(5) O22 0.0489(10) 0.0491(10) 0.0494(10) -0.0002(7) 0.0161(7) 0.0000(7) O14' 0.063(6) 0.034(5) 0.070(7) 0.000 -0.020(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O4 2.256(2) . ? Gd1 O12 2.315(2) 1_565 ? Gd1 O5 2.356(2) . ? Gd1 O13 2.453(3) . ? Gd1 O7 2.472(2) 4_545 ? Gd1 O10 2.476(2) . ? Gd1 O9 2.477(2) . ? Gd1 O8 2.502(2) 4_545 ? Gd1 C24 2.837(3) 4_545 ? Cu1 O1 1.949(2) 4_646 ? Cu1 N1 1.995(3) . ? Cu1 N6 1.996(3) 3 ? Cu1 N5 2.029(3) 3 ? Cu1 N2 2.187(3) . ? Cu2 O14' 1.969(9) . ? Cu2 N3 1.974(2) 2 ? Cu2 N3 1.974(2) . ? Cu2 N4 2.123(3) 2 ? Cu2 N4 2.123(3) . ? Cu2 O14 2.290(5) 2 ? Cu2 O14 2.290(5) . ? C1 N1 1.356(4) . ? C1 C2 1.387(5) . ? C1 C6 1.486(4) . ? C2 C3 1.389(4) . ? C3 C4 1.386(4) . ? C3 C11 1.504(5) . ? C4 C5 1.377(5) . ? C5 N1 1.340(4) . ? C6 N2 1.352(4) . ? C6 C7 1.385(4) . ? C7 C8 1.387(4) . ? C8 C9 1.396(5) . ? C8 C12 1.521(4) . ? C9 C10 1.383(4) . ? C10 N2 1.340(4) . ? C11 O2 1.242(4) . ? C11 O1 1.270(4) . ? C12 O3 1.237(5) . ? C12 O4 1.248(4) . ? C13 N3 1.350(4) . ? C13 C14 1.397(4) . ? C13 C18 1.494(4) . ? C14 C15 1.391(4) . ? C15 C16 1.384(5) . ? C15 C23 1.513(4) . ? C16 C17 1.372(5) . ? C17 N3 1.349(4) . ? C18 N4 1.351(4) . ? C18 C19 1.379(5) . ? C19 C20 1.390(4) . ? C20 C21 1.389(4) . ? C20 C24 1.507(5) . ? C21 C22 1.378(5) . ? C22 N4 1.342(4) . ? C23 O6 1.242(4) . ? C23 O5 1.272(4) . ? C24 O7 1.257(4) . ? C24 O8 1.261(3) . ? C24 Gd1 2.837(3) 4 ? C25 N5 1.352(4) . ? C25 C26 1.386(5) . ? C25 C30 1.487(4) . ? C26 C27 1.388(5) . ? C27 C28 1.385(5) . ? C27 C35 1.513(5) . ? C28 C29 1.371(5) . ? C29 N5 1.350(4) . ? C30 N6 1.351(4) . ? C30 C31 1.383(5) . ? C31 C32 1.388(5) . ? C32 C33 1.393(5) . ? C32 C36 1.517(5) . ? C33 C34 1.379(5) . ? C34 N6 1.342(4) . ? C35 O9 1.256(4) . ? C35 O10 1.261(4) . ? C36 O11 1.246(5) . ? C36 O12 1.260(4) . ? N5 Cu1 2.029(3) 3_445 ? N6 Cu1 1.996(3) 3_445 ? O1 Cu1 1.949(2) 4_656 ? O7 Gd1 2.472(2) 4 ? O8 Gd1 2.502(2) 4 ? O12 Gd1 2.315(2) 1_545 ? O14 O14' 1.417(5) . ? O14' O14 1.417(5) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Gd1 O12 80.12(9) . 1_565 ? O4 Gd1 O5 157.72(9) . . ? O12 Gd1 O5 77.99(8) 1_565 . ? O4 Gd1 O13 104.70(9) . . ? O12 Gd1 O13 81.39(9) 1_565 . ? O5 Gd1 O13 76.04(8) . . ? O4 Gd1 O7 128.19(8) . 4_545 ? O12 Gd1 O7 147.60(7) 1_565 4_545 ? O5 Gd1 O7 73.96(7) . 4_545 ? O13 Gd1 O7 76.42(8) . 4_545 ? O4 Gd1 O10 81.99(9) . . ? O12 Gd1 O10 131.64(8) 1_565 . ? O5 Gd1 O10 109.86(8) . . ? O13 Gd1 O10 146.82(8) . . ? O7 Gd1 O10 74.28(8) 4_545 . ? O4 Gd1 O9 88.03(9) . . ? O12 Gd1 O9 81.83(9) 1_565 . ? O5 Gd1 O9 84.87(8) . . ? O13 Gd1 O9 156.79(8) . . ? O7 Gd1 O9 111.09(8) 4_545 . ? O10 Gd1 O9 52.95(8) . . ? O4 Gd1 O8 77.70(8) . 4_545 ? O12 Gd1 O8 140.10(8) 1_565 4_545 ? O5 Gd1 O8 122.60(7) . 4_545 ? O13 Gd1 O8 72.84(8) . 4_545 ? O7 Gd1 O8 52.61(7) 4_545 4_545 ? O10 Gd1 O8 77.14(8) . 4_545 ? O9 Gd1 O8 129.61(7) . 4_545 ? O4 Gd1 C24 103.29(9) . 4_545 ? O12 Gd1 C24 153.38(9) 1_565 4_545 ? O5 Gd1 C24 98.13(8) . 4_545 ? O13 Gd1 C24 72.17(9) . 4_545 ? O7 Gd1 C24 26.26(7) 4_545 4_545 ? O10 Gd1 C24 74.67(8) . 4_545 ? O9 Gd1 C24 124.38(9) . 4_545 ? O8 Gd1 C24 26.36(7) 4_545 4_545 ? O1 Cu1 N1 90.13(10) 4_646 . ? O1 Cu1 N6 92.99(10) 4_646 3 ? N1 Cu1 N6 167.34(10) . 3 ? O1 Cu1 N5 163.33(9) 4_646 3 ? N1 Cu1 N5 92.49(11) . 3 ? N6 Cu1 N5 81.10(11) 3 3 ? O1 Cu1 N2 94.53(10) 4_646 . ? N1 Cu1 N2 78.12(10) . . ? N6 Cu1 N2 113.81(10) 3 . ? N5 Cu1 N2 102.12(10) 3 . ? O14' Cu2 N3 92.69(9) . 2 ? O14' Cu2 N3 92.69(8) . . ? N3 Cu2 N3 174.61(17) 2 . ? O14' Cu2 N4 128.03(8) . 2 ? N3 Cu2 N4 79.69(10) 2 2 ? N3 Cu2 N4 96.96(10) . 2 ? O14' Cu2 N4 128.03(8) . . ? N3 Cu2 N4 96.96(10) 2 . ? N3 Cu2 N4 79.69(10) . . ? N4 Cu2 N4 103.94(16) 2 . ? O14' Cu2 O14 37.95(13) . 2 ? N3 Cu2 O14 94.07(14) 2 2 ? N3 Cu2 O14 90.18(15) . 2 ? N4 Cu2 O14 164.94(16) 2 2 ? N4 Cu2 O14 90.34(15) . 2 ? O14' Cu2 O14 37.95(13) . . ? N3 Cu2 O14 90.18(15) 2 . ? N3 Cu2 O14 94.07(14) . . ? N4 Cu2 O14 90.34(15) 2 . ? N4 Cu2 O14 164.94(16) . . ? O14 Cu2 O14 75.9(3) 2 . ? N1 C1 C2 121.2(3) . . ? N1 C1 C6 115.1(3) . . ? C2 C1 C6 123.7(3) . . ? C1 C2 C3 118.9(3) . . ? C4 C3 C2 119.3(3) . . ? C4 C3 C11 119.7(3) . . ? C2 C3 C11 120.9(3) . . ? C5 C4 C3 118.8(3) . . ? N1 C5 C4 122.3(3) . . ? N2 C6 C7 122.1(3) . . ? N2 C6 C1 115.2(3) . . ? C7 C6 C1 122.6(3) . . ? C6 C7 C8 119.5(3) . . ? C7 C8 C9 118.3(3) . . ? C7 C8 C12 121.2(3) . . ? C9 C8 C12 120.4(3) . . ? C10 C9 C8 118.9(3) . . ? N2 C10 C9 122.9(3) . . ? O2 C11 O1 125.4(3) . . ? O2 C11 C3 120.5(3) . . ? O1 C11 C3 114.2(3) . . ? O3 C12 O4 126.2(3) . . ? O3 C12 C8 118.3(3) . . ? O4 C12 C8 115.5(3) . . ? N3 C13 C14 121.3(3) . . ? N3 C13 C18 115.1(3) . . ? C14 C13 C18 123.6(3) . . ? C15 C14 C13 118.9(3) . . ? C16 C15 C14 118.9(3) . . ? C16 C15 C23 119.8(3) . . ? C14 C15 C23 121.3(3) . . ? C17 C16 C15 119.7(3) . . ? N3 C17 C16 122.0(3) . . ? N4 C18 C19 122.0(3) . . ? N4 C18 C13 114.5(3) . . ? C19 C18 C13 123.4(3) . . ? C18 C19 C20 119.4(3) . . ? C21 C20 C19 118.6(3) . . ? C21 C20 C24 121.8(3) . . ? C19 C20 C24 119.6(3) . . ? C22 C21 C20 118.7(3) . . ? N4 C22 C21 123.1(3) . . ? O6 C23 O5 126.6(3) . . ? O6 C23 C15 118.1(3) . . ? O5 C23 C15 115.3(3) . . ? O7 C24 O8 122.2(3) . . ? O7 C24 C20 118.7(3) . . ? O8 C24 C20 119.1(3) . . ? O7 C24 Gd1 60.45(16) . 4 ? O8 C24 Gd1 61.81(17) . 4 ? C20 C24 Gd1 176.7(2) . 4 ? N5 C25 C26 121.7(3) . . ? N5 C25 C30 114.9(3) . . ? C26 C25 C30 123.2(3) . . ? C25 C26 C27 119.2(3) . . ? C28 C27 C26 118.7(3) . . ? C28 C27 C35 121.4(3) . . ? C26 C27 C35 119.7(3) . . ? C29 C28 C27 119.4(3) . . ? N5 C29 C28 122.4(3) . . ? N6 C30 C31 121.4(3) . . ? N6 C30 C25 114.5(3) . . ? C31 C30 C25 124.0(3) . . ? C30 C31 C32 119.8(3) . . ? C31 C32 C33 118.3(3) . . ? C31 C32 C36 120.1(3) . . ? C33 C32 C36 121.6(3) . . ? C34 C33 C32 119.0(3) . . ? N6 C34 C33 122.5(3) . . ? O9 C35 O10 122.6(3) . . ? O9 C35 C27 119.2(3) . . ? O10 C35 C27 118.1(3) . . ? O11 C36 O12 126.6(4) . . ? O11 C36 C32 117.6(3) . . ? O12 C36 C32 115.8(3) . . ? C5 N1 C1 119.2(3) . . ? C5 N1 Cu1 122.5(2) . . ? C1 N1 Cu1 118.13(19) . . ? C10 N2 C6 118.2(3) . . ? C10 N2 Cu1 129.6(2) . . ? C6 N2 Cu1 112.13(18) . . ? C17 N3 C13 119.2(3) . . ? C17 N3 Cu2 123.0(2) . . ? C13 N3 Cu2 117.72(19) . . ? C22 N4 C18 118.1(3) . . ? C22 N4 Cu2 128.9(2) . . ? C18 N4 Cu2 113.0(2) . . ? C29 N5 C25 118.4(3) . . ? C29 N5 Cu1 128.3(2) . 3_445 ? C25 N5 Cu1 113.2(2) . 3_445 ? C34 N6 C30 118.8(3) . . ? C34 N6 Cu1 126.5(2) . 3_445 ? C30 N6 Cu1 114.5(2) . 3_445 ? C11 O1 Cu1 117.9(2) . 4_656 ? C12 O4 Gd1 160.4(2) . . ? C23 O5 Gd1 138.1(2) . . ? C24 O7 Gd1 93.29(18) . 4 ? C24 O8 Gd1 91.83(18) . 4 ? C35 O9 Gd1 92.2(2) . . ? C35 O10 Gd1 92.16(19) . . ? C36 O12 Gd1 146.8(2) . 1_545 ? O14' O14 Cu2 58.7(4) . . ? O14 O14' O14 166.8(9) . 2 ? O14 O14' Cu2 83.4(4) . . ? O14 O14' Cu2 83.4(4) 2 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -2.5(5) . . . . ? C6 C1 C2 C3 176.3(3) . . . . ? C1 C2 C3 C4 -2.9(5) . . . . ? C1 C2 C3 C11 173.9(3) . . . . ? C2 C3 C4 C5 5.2(5) . . . . ? C11 C3 C4 C5 -171.7(3) . . . . ? C3 C4 C5 N1 -2.2(5) . . . . ? N1 C1 C6 N2 -4.4(4) . . . . ? C2 C1 C6 N2 176.7(3) . . . . ? N1 C1 C6 C7 171.5(3) . . . . ? C2 C1 C6 C7 -7.4(5) . . . . ? N2 C6 C7 C8 1.6(5) . . . . ? C1 C6 C7 C8 -174.0(3) . . . . ? C6 C7 C8 C9 0.6(5) . . . . ? C6 C7 C8 C12 178.6(3) . . . . ? C7 C8 C9 C10 -1.5(5) . . . . ? C12 C8 C9 C10 -179.5(3) . . . . ? C8 C9 C10 N2 0.2(5) . . . . ? C4 C3 C11 O2 -172.5(3) . . . . ? C2 C3 C11 O2 10.7(5) . . . . ? C4 C3 C11 O1 8.3(4) . . . . ? C2 C3 C11 O1 -168.5(3) . . . . ? C7 C8 C12 O3 -2.0(5) . . . . ? C9 C8 C12 O3 175.9(3) . . . . ? C7 C8 C12 O4 177.9(3) . . . . ? C9 C8 C12 O4 -4.1(5) . . . . ? N3 C13 C14 C15 -1.3(5) . . . . ? C18 C13 C14 C15 177.1(3) . . . . ? C13 C14 C15 C16 0.5(5) . . . . ? C13 C14 C15 C23 -177.8(3) . . . . ? C14 C15 C16 C17 0.5(5) . . . . ? C23 C15 C16 C17 178.9(3) . . . . ? C15 C16 C17 N3 -0.8(5) . . . . ? N3 C13 C18 N4 1.7(4) . . . . ? C14 C13 C18 N4 -176.8(3) . . . . ? N3 C13 C18 C19 -179.8(3) . . . . ? C14 C13 C18 C19 1.7(5) . . . . ? N4 C18 C19 C20 2.1(5) . . . . ? C13 C18 C19 C20 -176.3(3) . . . . ? C18 C19 C20 C21 -1.4(5) . . . . ? C18 C19 C20 C24 177.6(3) . . . . ? C19 C20 C21 C22 -0.2(5) . . . . ? C24 C20 C21 C22 -179.3(3) . . . . ? C20 C21 C22 N4 1.4(6) . . . . ? C16 C15 C23 O6 -172.0(3) . . . . ? C14 C15 C23 O6 6.3(5) . . . . ? C16 C15 C23 O5 6.3(5) . . . . ? C14 C15 C23 O5 -175.4(3) . . . . ? C21 C20 C24 O7 -177.2(3) . . . . ? C19 C20 C24 O7 3.7(5) . . . . ? C21 C20 C24 O8 3.7(5) . . . . ? C19 C20 C24 O8 -175.4(3) . . . . ? C21 C20 C24 Gd1 109(3) . . . 4 ? C19 C20 C24 Gd1 -70(4) . . . 4 ? N5 C25 C26 C27 -5.6(4) . . . . ? C30 C25 C26 C27 169.4(3) . . . . ? C25 C26 C27 C28 2.9(4) . . . . ? C25 C26 C27 C35 -172.1(3) . . . . ? C26 C27 C28 C29 2.1(4) . . . . ? C35 C27 C28 C29 177.0(3) . . . . ? C27 C28 C29 N5 -4.9(4) . . . . ? N5 C25 C30 N6 0.9(4) . . . . ? C26 C25 C30 N6 -174.4(3) . . . . ? N5 C25 C30 C31 178.1(3) . . . . ? C26 C25 C30 C31 2.7(4) . . . . ? N6 C30 C31 C32 2.9(4) . . . . ? C25 C30 C31 C32 -174.0(3) . . . . ? C30 C31 C32 C33 -0.6(4) . . . . ? C30 C31 C32 C36 179.2(3) . . . . ? C31 C32 C33 C34 -1.8(4) . . . . ? C36 C32 C33 C34 178.4(3) . . . . ? C32 C33 C34 N6 2.3(4) . . . . ? C28 C27 C35 O9 -10.2(4) . . . . ? C26 C27 C35 O9 164.6(3) . . . . ? C28 C27 C35 O10 172.9(3) . . . . ? C26 C27 C35 O10 -12.3(4) . . . . ? C31 C32 C36 O11 17.1(5) . . . . ? C33 C32 C36 O11 -163.1(3) . . . . ? C31 C32 C36 O12 -162.0(3) . . . . ? C33 C32 C36 O12 17.8(4) . . . . ? C4 C5 N1 C1 -3.2(5) . . . . ? C4 C5 N1 Cu1 171.3(2) . . . . ? C2 C1 N1 C5 5.6(5) . . . . ? C6 C1 N1 C5 -173.4(3) . . . . ? C2 C1 N1 Cu1 -169.2(2) . . . . ? C6 C1 N1 Cu1 11.9(4) . . . . ? O1 Cu1 N1 C5 80.1(3) 4_646 . . . ? N6 Cu1 N1 C5 -24.3(6) 3 . . . ? N5 Cu1 N1 C5 -83.5(3) 3 . . . ? N2 Cu1 N1 C5 174.7(3) . . . . ? O1 Cu1 N1 C1 -105.3(2) 4_646 . . . ? N6 Cu1 N1 C1 150.3(4) 3 . . . ? N5 Cu1 N1 C1 91.1(2) 3 . . . ? N2 Cu1 N1 C1 -10.7(2) . . . . ? C9 C10 N2 C6 2.0(5) . . . . ? C9 C10 N2 Cu1 178.5(2) . . . . ? C7 C6 N2 C10 -2.9(5) . . . . ? C1 C6 N2 C10 173.1(3) . . . . ? C7 C6 N2 Cu1 -180.0(2) . . . . ? C1 C6 N2 Cu1 -4.1(3) . . . . ? O1 Cu1 N2 C10 -79.8(3) 4_646 . . . ? N1 Cu1 N2 C10 -168.9(3) . . . . ? N6 Cu1 N2 C10 15.5(3) 3 . . . ? N5 Cu1 N2 C10 101.0(3) 3 . . . ? O1 Cu1 N2 C6 97.0(2) 4_646 . . . ? N1 Cu1 N2 C6 7.8(2) . . . . ? N6 Cu1 N2 C6 -167.8(2) 3 . . . ? N5 Cu1 N2 C6 -82.2(2) 3 . . . ? C16 C17 N3 C13 0.0(5) . . . . ? C16 C17 N3 Cu2 -177.0(3) . . . . ? C14 C13 N3 C17 1.0(5) . . . . ? C18 C13 N3 C17 -177.5(3) . . . . ? C14 C13 N3 Cu2 178.2(2) . . . . ? C18 C13 N3 Cu2 -0.3(4) . . . . ? O14' Cu2 N3 C17 -55.4(3) . . . . ? N3 Cu2 N3 C17 124.6(3) 2 . . . ? N4 Cu2 N3 C17 73.4(3) 2 . . . ? N4 Cu2 N3 C17 176.4(3) . . . . ? O14 Cu2 N3 C17 -93.3(3) 2 . . . ? O14 Cu2 N3 C17 -17.4(3) . . . . ? O14' Cu2 N3 C13 127.5(2) . . . . ? N3 Cu2 N3 C13 -52.5(2) 2 . . . ? N4 Cu2 N3 C13 -103.7(2) 2 . . . ? N4 Cu2 N3 C13 -0.7(2) . . . . ? O14 Cu2 N3 C13 89.6(3) 2 . . . ? O14 Cu2 N3 C13 165.5(3) . . . . ? C21 C22 N4 C18 -0.8(5) . . . . ? C21 C22 N4 Cu2 178.9(3) . . . . ? C19 C18 N4 C22 -1.0(5) . . . . ? C13 C18 N4 C22 177.5(3) . . . . ? C19 C18 N4 Cu2 179.3(3) . . . . ? C13 C18 N4 Cu2 -2.2(3) . . . . ? O14' Cu2 N4 C22 96.6(3) . . . . ? N3 Cu2 N4 C22 -2.3(3) 2 . . . ? N3 Cu2 N4 C22 -178.1(3) . . . . ? N4 Cu2 N4 C22 -83.4(3) 2 . . . ? O14 Cu2 N4 C22 91.8(3) 2 . . . ? O14 Cu2 N4 C22 115.5(6) . . . . ? O14' Cu2 N4 C18 -83.7(2) . . . . ? N3 Cu2 N4 C18 177.3(2) 2 . . . ? N3 Cu2 N4 C18 1.6(2) . . . . ? N4 Cu2 N4 C18 96.3(2) 2 . . . ? O14 Cu2 N4 C18 -88.5(2) 2 . . . ? O14 Cu2 N4 C18 -64.9(6) . . . . ? C28 C29 N5 C25 2.4(4) . . . . ? C28 C29 N5 Cu1 -179.0(2) . . . 3_445 ? C26 C25 N5 C29 2.9(4) . . . . ? C30 C25 N5 C29 -172.5(2) . . . . ? C26 C25 N5 Cu1 -175.8(2) . . . 3_445 ? C30 C25 N5 Cu1 8.8(3) . . . 3_445 ? C33 C34 N6 C30 0.0(4) . . . . ? C33 C34 N6 Cu1 -174.3(2) . . . 3_445 ? C31 C30 N6 C34 -2.6(4) . . . . ? C25 C30 N6 C34 174.6(2) . . . . ? C31 C30 N6 Cu1 172.4(2) . . . 3_445 ? C25 C30 N6 Cu1 -10.4(3) . . . 3_445 ? O2 C11 O1 Cu1 -4.2(5) . . . 4_656 ? C3 C11 O1 Cu1 174.9(2) . . . 4_656 ? O3 C12 O4 Gd1 31.2(10) . . . . ? C8 C12 O4 Gd1 -148.8(6) . . . . ? O12 Gd1 O4 C12 0.9(8) 1_565 . . . ? O5 Gd1 O4 C12 -9.8(9) . . . . ? O13 Gd1 O4 C12 79.2(8) . . . . ? O7 Gd1 O4 C12 163.4(7) 4_545 . . . ? O10 Gd1 O4 C12 -133.9(8) . . . . ? O9 Gd1 O4 C12 -81.1(8) . . . . ? O8 Gd1 O4 C12 147.6(8) 4_545 . . . ? C24 Gd1 O4 C12 154.0(8) 4_545 . . . ? O6 C23 O5 Gd1 1.9(6) . . . . ? C15 C23 O5 Gd1 -176.1(2) . . . . ? O4 Gd1 O5 C23 80.3(4) . . . . ? O12 Gd1 O5 C23 69.5(3) 1_565 . . . ? O13 Gd1 O5 C23 -14.5(3) . . . . ? O7 Gd1 O5 C23 -94.1(3) 4_545 . . . ? O10 Gd1 O5 C23 -160.3(3) . . . . ? O9 Gd1 O5 C23 152.2(3) . . . . ? O8 Gd1 O5 C23 -73.1(3) 4_545 . . . ? C24 Gd1 O5 C23 -83.7(3) 4_545 . . . ? O8 C24 O7 Gd1 2.7(3) . . . 4 ? C20 C24 O7 Gd1 -176.3(3) . . . 4 ? O7 C24 O8 Gd1 -2.7(3) . . . 4 ? C20 C24 O8 Gd1 176.4(3) . . . 4 ? O10 C35 O9 Gd1 2.5(3) . . . . ? C27 C35 O9 Gd1 -174.3(2) . . . . ? O4 Gd1 O9 C35 -82.78(18) . . . . ? O12 Gd1 O9 C35 -163.07(18) 1_565 . . . ? O5 Gd1 O9 C35 118.36(18) . . . . ? O13 Gd1 O9 C35 152.9(2) . . . . ? O7 Gd1 O9 C35 47.75(18) 4_545 . . . ? O10 Gd1 O9 C35 -1.33(16) . . . . ? O8 Gd1 O9 C35 -10.5(2) 4_545 . . . ? C24 Gd1 O9 C35 22.0(2) 4_545 . . . ? O9 C35 O10 Gd1 -2.5(3) . . . . ? C27 C35 O10 Gd1 174.3(2) . . . . ? O4 Gd1 O10 C35 94.92(18) . . . . ? O12 Gd1 O10 C35 25.8(2) 1_565 . . . ? O5 Gd1 O10 C35 -65.60(18) . . . . ? O13 Gd1 O10 C35 -160.41(17) . . . . ? O7 Gd1 O10 C35 -131.59(18) 4_545 . . . ? O9 Gd1 O10 C35 1.33(16) . . . . ? O8 Gd1 O10 C35 174.06(18) 4_545 . . . ? C24 Gd1 O10 C35 -158.86(18) 4_545 . . . ? O11 C36 O12 Gd1 40.4(6) . . . 1_545 ? C32 C36 O12 Gd1 -140.6(3) . . . 1_545 ? N3 Cu2 O14 O14' 94.15(17) 2 . . . ? N3 Cu2 O14 O14' -89.16(17) . . . . ? N4 Cu2 O14 O14' 173.84(16) 2 . . . ? N4 Cu2 O14 O14' -24.4(6) . . . . ? O14 Cu2 O14 O14' 0.000(1) 2 . . . ? Cu2 O14 O14' O14 0.000(5) . . . 2 ? N3 Cu2 O14' O14 -86.8(2) 2 . . . ? N3 Cu2 O14' O14 93.2(2) . . . . ? N4 Cu2 O14' O14 -7.8(2) 2 . . . ? N4 Cu2 O14' O14 172.2(2) . . . . ? O14 Cu2 O14' O14 180.0 2 . . . ? N3 Cu2 O14' O14 93.2(2) 2 . . 2 ? N3 Cu2 O14' O14 -86.8(2) . . . 2 ? N4 Cu2 O14' O14 172.2(2) 2 . . 2 ? N4 Cu2 O14' O14 -7.8(2) . . . 2 ? O14 Cu2 O14' O14 180.000(1) . . . 2 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.876 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.128 # Attachment '5.cif' data_r71208d _database_code_depnum_ccdc_archive 'CCDC 731499' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26.50 Cu1.50 N6 O16.25 Yb' _chemical_formula_weight 1071.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.814(5) _cell_length_b 12.254(3) _cell_length_c 26.883(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.30(3) _cell_angle_gamma 90.00 _cell_volume 7715(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4224 _exptl_absorpt_coefficient_mu 3.312 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6193 _exptl_absorpt_correction_T_max 0.8789 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 27905 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6687 _reflns_number_gt 5622 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+47.8652P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6687 _refine_ls_number_parameters 596 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.169078(8) 0.466684(14) 0.046088(7) 0.01543(5) Uani 1 1 d . . . Cu1 Cu 0.0000 0.50757(6) 0.2500 0.02274(18) Uani 1 2 d SD . . Cu2 Cu 0.36335(2) 0.46266(4) -0.13416(2) 0.01917(13) Uani 1 1 d . . . C1 C 0.0813(2) 0.6595(4) 0.34686(18) 0.0300(12) Uani 1 1 d . . . H1 H 0.0520 0.6522 0.3610 0.036 Uiso 1 1 calc R . . C2 C 0.1306(2) 0.7277(4) 0.37836(17) 0.0282(11) Uani 1 1 d . . . H2 H 0.1277 0.7609 0.4085 0.034 Uiso 1 1 calc R . . C3 C 0.17739(19) 0.7449(4) 0.36734(16) 0.0228(10) Uani 1 1 d . . . C4 C 0.1712(2) 0.6905(3) 0.32360(16) 0.0208(10) Uani 1 1 d . . . H4 H 0.2016 0.6913 0.3107 0.025 Uiso 1 1 calc R . . C5 C 0.11897(19) 0.6271(3) 0.29264(16) 0.0194(10) Uani 1 1 d . . . C6 C 0.10605(18) 0.5709(3) 0.24403(16) 0.0184(10) Uani 1 1 d . . . C7 C 0.1446(2) 0.5817(4) 0.22310(16) 0.0228(10) Uani 1 1 d . . . H7 H 0.1791 0.6182 0.2376 0.027 Uiso 1 1 calc R . . C8 C 0.1265(2) 0.5307(3) 0.17568(17) 0.0207(11) Uani 1 1 d . . . C9 C 0.0712(2) 0.4714(4) 0.15075(19) 0.0267(12) Uani 1 1 d . . . H9 H 0.0639 0.4404 0.1176 0.032 Uiso 1 1 calc R . . C10 C 0.0351(2) 0.4627(4) 0.1732(2) 0.0308(13) Uani 1 1 d . . . H10 H 0.0003 0.4265 0.1600 0.037 Uiso 1 1 calc R . . C11 C 0.2317(2) 0.8199(4) 0.39888(17) 0.0245(11) Uani 1 1 d . . . C12 C 0.1648(2) 0.5435(4) 0.15013(17) 0.0257(11) Uani 1 1 d . . . C13 C 0.3004(2) 0.4306(4) -0.06466(18) 0.0265(11) Uani 1 1 d . . . H13 H 0.3291 0.3818 -0.0472 0.032 Uiso 1 1 calc R . . C14 C 0.2582(2) 0.4506(4) -0.05001(17) 0.0251(11) Uani 1 1 d . . . H14 H 0.2562 0.4154 -0.0201 0.030 Uiso 1 1 calc R . . C15 C 0.2109(2) 0.5283(4) -0.07812(19) 0.0255(11) Uani 1 1 d . . . C16 C 0.2091(2) 0.5816(4) -0.12004(17) 0.0239(11) Uani 1 1 d . . . H16 H 0.1806 0.6300 -0.1385 0.029 Uiso 1 1 calc R . . C17 C 0.2547(2) 0.5553(4) -0.13187(17) 0.0216(11) Uani 1 1 d . . . C18 C 0.25175(19) 0.6009(3) -0.17875(16) 0.0206(10) Uani 1 1 d . . . C19 C 0.2091(2) 0.6785(3) -0.21156(16) 0.0205(10) Uani 1 1 d . . . H19 H 0.1816 0.7057 -0.1983 0.025 Uiso 1 1 calc R . . C20 C 0.20796(19) 0.7096(4) -0.25638(17) 0.0212(11) Uani 1 1 d . . . C21 C 0.24801(19) 0.6571(3) -0.26884(17) 0.0217(10) Uani 1 1 d . . . H21 H 0.2492 0.6673 -0.3027 0.026 Uiso 1 1 calc R . . C22 C 0.2914(2) 0.5830(4) -0.23368(16) 0.0226(10) Uani 1 1 d . . . H22 H 0.3185 0.5537 -0.2469 0.027 Uiso 1 1 calc R . . C23 C 0.1613(2) 0.5510(4) -0.06417(17) 0.0233(11) Uani 1 1 d . . . C24 C 0.1673(2) 0.8016(4) -0.29003(19) 0.0273(12) Uani 1 1 d . . . C25 C 0.4109(2) 0.6968(4) -0.10450(17) 0.0248(11) Uani 1 1 d . . . H25 H 0.3741 0.7209 -0.1228 0.030 Uiso 1 1 calc R . . C26 C 0.4579(2) 0.7742(4) -0.07833(17) 0.0239(11) Uani 1 1 d . . . H26 H 0.4485 0.8478 -0.0794 0.029 Uiso 1 1 calc R . . C27 C 0.52078(18) 0.7431(3) -0.04964(15) 0.0191(10) Uani 1 1 d D . . C28 C 0.5348(2) 0.6331(3) -0.04718(16) 0.0210(10) Uani 1 1 d . . . H28 H 0.5722 0.6085 -0.0320 0.025 Uiso 1 1 calc R . . C29 C 0.48632(19) 0.5574(3) -0.07037(16) 0.0183(10) Uani 1 1 d . . . C30 C 0.4965(2) 0.4386(4) -0.06234(17) 0.0227(10) Uani 1 1 d . . . C31 C 0.5548(2) 0.3902(3) -0.03227(17) 0.0246(11) Uani 1 1 d . . . H31 H 0.5866 0.4352 -0.0201 0.029 Uiso 1 1 calc R . . C32 C 0.5601(2) 0.2775(3) -0.02303(17) 0.0276(12) Uani 1 1 d D . . C33 C 0.5029(2) 0.2193(3) -0.04652(16) 0.0252(12) Uani 1 1 d . . . H33 H 0.5028 0.1443 -0.0413 0.030 Uiso 1 1 calc R . . C34 C 0.4456(2) 0.2714(4) -0.07771(16) 0.0242(11) Uani 1 1 d . . . H34 H 0.4133 0.2281 -0.0911 0.029 Uiso 1 1 calc R . . C35 C 0.57289(18) 0.8235(3) -0.01829(16) 0.0198(10) Uani 1 1 d D . . C36 C 0.6212(2) 0.2228(4) 0.00949(19) 0.0342(14) Uani 1 1 d D . . N1 N 0.42449(16) 0.5890(3) -0.10023(14) 0.0212(9) Uani 1 1 d . . . N2 N 0.44201(16) 0.3797(3) -0.08577(13) 0.0205(9) Uani 1 1 d . . . N3 N 0.30011(17) 0.4817(3) -0.10445(14) 0.0231(9) Uani 1 1 d . . . N4 N 0.29464(16) 0.5574(3) -0.18924(13) 0.0196(9) Uani 1 1 d . . . N5 N 0.05399(16) 0.5124(3) 0.21816(14) 0.0246(9) Uani 1 1 d D . . N6 N 0.07357(16) 0.6107(3) 0.30425(14) 0.0234(9) Uani 1 1 d . . . O1 O 0.62140(17) 0.1313(2) 0.02576(13) 0.0437(9) Uani 1 1 d . . . O2 O 0.6700(2) 0.2737(3) 0.0206(2) 0.0734(18) Uani 1 1 d . . . O3 O 0.62950(14) 0.7950(2) 0.00113(13) 0.0274(8) Uani 1 1 d . . . O4 O 0.55932(14) 0.9175(2) -0.01072(13) 0.0287(8) Uani 1 1 d . . . O5 O 0.18038(14) 0.8352(2) -0.32375(11) 0.0249(8) Uani 1 1 d . . . O6 O 0.12608(15) 0.8422(3) -0.28382(13) 0.0428(9) Uani 1 1 d . . . O7 O 0.11524(17) 0.6084(4) -0.09419(14) 0.0547(12) Uani 1 1 d . . . O8 O 0.17170(15) 0.5054(3) -0.02321(13) 0.0396(9) Uani 1 1 d . . . O9 O 0.25496(19) 0.5735(4) 0.10755(19) 0.0795(14) Uani 1 1 d . . . O10 O 0.14403(15) 0.4890(3) 0.10822(12) 0.0293(8) Uani 1 1 d . . . O11 O 0.21040(16) 0.6053(3) 0.17083(13) 0.0459(9) Uani 1 1 d . . . O12 O 0.27399(13) 0.8303(3) 0.38813(11) 0.0287(8) Uani 1 1 d . . . O13 O 0.23547(14) 0.8714(3) 0.43673(12) 0.0298(8) Uani 1 1 d . . . O14 O 0.0000 0.3463(7) 0.2500 0.102(3) Uani 1 2 d SU . . O15 O -0.0576(4) 0.3641(12) 0.2004(4) 0.106(4) Uani 0.50 1 d PU . . O16 O 0.1334(6) 0.0168(14) 0.2990(5) 0.043(3) Uani 0.25 1 d PU . . O17 O 0.0673(10) 0.983(2) 0.2282(10) 0.060(5) Uani 0.20 1 d PU . . O18 O 0.0455(6) 0.8536(11) 0.2363(6) 0.049(4) Uani 0.25 1 d P . . O19 O 1.0109(9) 0.0133(17) 0.1643(7) 0.068(5) Uani 0.25 1 d PU . . O20 O 0.9415(6) 0.0147(10) 0.1710(5) 0.041(3) Uani 0.30 1 d PU . . O21 O 0.2956(4) 0.6925(7) 0.0551(4) 0.075(3) Uani 0.50 1 d P . . O22 O 0.1392(3) 0.0011(7) 0.4292(3) 0.0424(18) Uani 0.50 1 d PU . . 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 0.02498(10) 0.01239(8) 0.01534(9) 0.00087(6) 0.01532(7) 0.00114(7) Cu1 0.0270(4) 0.0250(4) 0.0226(4) 0.000 0.0169(3) 0.000 Cu2 0.0301(3) 0.0173(2) 0.0164(2) -0.00163(18) 0.0163(2) -0.0020(2) C1 0.034(2) 0.044(3) 0.024(2) -0.0054(19) 0.0249(18) -0.009(2) C2 0.035(2) 0.040(3) 0.019(2) -0.0082(19) 0.0219(18) -0.006(2) C3 0.035(2) 0.026(2) 0.0176(18) -0.0027(16) 0.0219(17) -0.0034(19) C4 0.031(2) 0.023(2) 0.0136(19) -0.0019(16) 0.0138(17) -0.0031(19) C5 0.024(2) 0.020(2) 0.0201(19) 0.0008(16) 0.0150(17) -0.0034(18) C6 0.024(2) 0.020(2) 0.0176(19) 0.0014(16) 0.0157(17) 0.0013(18) C7 0.036(2) 0.022(2) 0.0204(19) -0.0004(16) 0.0237(17) -0.0028(19) C8 0.035(2) 0.016(2) 0.016(2) 0.0022(15) 0.0151(18) 0.0043(19) C9 0.039(3) 0.024(2) 0.024(2) -0.0065(17) 0.0194(19) 0.002(2) C10 0.035(3) 0.029(2) 0.032(3) -0.0151(19) 0.016(2) -0.009(2) C11 0.036(2) 0.027(2) 0.018(2) 0.0015(17) 0.0187(18) 0.000(2) C12 0.043(3) 0.023(2) 0.019(2) 0.0058(17) 0.0220(19) 0.006(2) C13 0.039(3) 0.023(2) 0.022(2) 0.0034(18) 0.017(2) -0.002(2) C14 0.039(3) 0.024(2) 0.020(2) -0.0001(17) 0.0192(19) -0.002(2) C15 0.030(2) 0.027(2) 0.027(2) -0.0008(18) 0.0198(19) 0.002(2) C16 0.034(2) 0.026(2) 0.018(2) 0.0015(17) 0.0179(18) 0.000(2) C17 0.032(2) 0.019(2) 0.020(2) -0.0023(16) 0.0171(18) -0.0038(19) C18 0.027(2) 0.021(2) 0.0222(19) -0.0018(16) 0.0202(17) -0.0034(18) C19 0.031(2) 0.022(2) 0.0143(19) 0.0011(16) 0.0157(17) -0.0044(19) C20 0.024(2) 0.021(2) 0.022(2) -0.0019(17) 0.0127(18) -0.0054(19) C21 0.033(2) 0.0169(19) 0.023(2) -0.0030(16) 0.0203(18) -0.0062(18) C22 0.034(2) 0.026(2) 0.0177(19) -0.0022(16) 0.0220(17) -0.0022(19) C23 0.031(2) 0.025(2) 0.021(2) 0.0015(17) 0.0178(18) -0.0002(19) C24 0.028(3) 0.029(2) 0.026(2) 0.0032(19) 0.011(2) 0.006(2) C25 0.036(2) 0.018(2) 0.027(2) 0.0012(17) 0.0200(19) 0.0024(19) C26 0.037(3) 0.017(2) 0.023(2) -0.0009(17) 0.0173(19) 0.0029(19) C27 0.028(2) 0.019(2) 0.0153(19) -0.0022(16) 0.0139(17) -0.0020(18) C28 0.028(2) 0.021(2) 0.018(2) 0.0037(16) 0.0139(18) 0.0001(19) C29 0.026(2) 0.0161(19) 0.0184(19) 0.0021(16) 0.0142(17) 0.0017(18) C30 0.038(2) 0.020(2) 0.0189(19) -0.0022(16) 0.0206(18) -0.0042(19) C31 0.038(2) 0.0146(19) 0.028(2) 0.0028(17) 0.0199(19) 0.0022(19) C32 0.053(3) 0.014(2) 0.023(2) -0.0036(17) 0.021(2) -0.004(2) C33 0.052(3) 0.0118(19) 0.015(2) 0.0004(16) 0.015(2) -0.002(2) C34 0.043(3) 0.020(2) 0.0146(19) -0.0026(16) 0.0166(18) -0.015(2) C35 0.032(2) 0.0146(19) 0.0186(19) 0.0053(16) 0.0164(17) -0.0037(18) C36 0.053(3) 0.018(2) 0.029(3) -0.0047(19) 0.010(2) 0.003(2) N1 0.0331(19) 0.0167(17) 0.0212(17) -0.0020(14) 0.0191(15) -0.0011(16) N2 0.0366(19) 0.0159(17) 0.0184(16) -0.0001(13) 0.0217(14) -0.0017(16) N3 0.036(2) 0.0227(18) 0.0189(17) 0.0022(14) 0.0196(15) -0.0039(17) N4 0.030(2) 0.0192(17) 0.0150(17) 0.0007(14) 0.0141(15) -0.0036(16) N5 0.033(2) 0.0231(18) 0.0245(18) -0.0040(15) 0.0186(16) -0.0037(17) N6 0.0296(19) 0.0268(19) 0.0234(17) -0.0021(15) 0.0218(15) -0.0041(16) O1 0.090(2) 0.0121(14) 0.0477(18) 0.0123(13) 0.0483(17) 0.0218(16) O2 0.047(3) 0.026(2) 0.129(4) 0.009(3) 0.005(3) 0.004(2) O3 0.0338(18) 0.0142(14) 0.0385(17) -0.0019(13) 0.0178(14) -0.0034(14) O4 0.0375(17) 0.0172(15) 0.0426(17) -0.0111(13) 0.0285(14) -0.0029(14) O5 0.0460(18) 0.0203(15) 0.0184(14) 0.0068(12) 0.0239(13) 0.0020(14) O6 0.0554(19) 0.045(2) 0.0472(18) 0.0204(15) 0.0431(15) 0.0185(17) O7 0.055(2) 0.088(3) 0.0361(17) 0.0247(19) 0.0367(15) 0.036(2) O8 0.0622(19) 0.0370(18) 0.0413(17) 0.0187(14) 0.0463(14) 0.0129(17) O9 0.066(2) 0.094(3) 0.104(3) -0.066(2) 0.064(2) -0.048(2) O10 0.0460(18) 0.0301(16) 0.0209(15) -0.0016(13) 0.0235(14) 0.0088(15) O11 0.080(2) 0.043(2) 0.0388(16) -0.0164(14) 0.0517(15) -0.0208(18) O12 0.0387(17) 0.0354(17) 0.0256(14) -0.0109(13) 0.0290(13) -0.0159(15) O13 0.0444(17) 0.0328(17) 0.0270(14) -0.0124(13) 0.0317(13) -0.0108(15) O14 0.201(9) 0.049(5) 0.088(5) 0.000 0.092(6) 0.000 O15 0.110(6) 0.170(12) 0.076(5) 0.021(6) 0.081(4) 0.045(7) O16 0.042(6) 0.076(7) 0.022(5) 0.022(5) 0.025(4) 0.008(5) O17 0.053(7) 0.063(8) 0.070(8) 0.000(6) 0.028(6) 0.009(6) O18 0.051(8) 0.041(7) 0.075(8) 0.051(6) 0.047(6) 0.034(6) O19 0.084(7) 0.075(7) 0.059(7) -0.001(6) 0.040(5) -0.005(6) O20 0.046(6) 0.033(5) 0.040(5) -0.001(4) 0.008(4) -0.023(5) O21 0.083(7) 0.026(4) 0.122(8) 0.008(5) 0.043(6) -0.008(4) O22 0.043(3) 0.067(4) 0.035(3) 0.008(3) 0.037(2) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O8 1.944(3) . ? Yb1 O10 1.984(3) . ? Yb1 O1 2.311(3) 3_455 ? Yb1 O3 2.463(3) 3_445 ? Yb1 O12 2.503(3) 4_545 ? Yb1 O13 2.542(3) 4_545 ? Yb1 O9 2.580(4) . ? Yb1 O4 2.714(3) 3_445 ? Yb1 C35 3.007(4) 3_445 ? Yb1 C11 3.013(5) 4_545 ? Cu1 N5 1.814(4) 2 ? Cu1 N5 1.814(4) . ? Cu1 O14 1.977(9) . ? Cu1 N6 2.302(4) . ? Cu1 N6 2.302(4) 2 ? Cu1 O15 2.378(14) . ? Cu1 O15 2.378(14) 2 ? Cu2 N3 1.996(4) . ? Cu2 O5 2.021(3) 4_544 ? Cu2 N1 2.149(4) . ? Cu2 N4 2.186(4) . ? Cu2 N2 2.204(4) . ? C1 N6 1.249(6) . ? C1 C2 1.492(7) . ? C1 H1 0.9300 . ? C2 C3 1.308(7) . ? C2 H2 0.9300 . ? C3 C4 1.316(6) . ? C3 C11 1.619(6) . ? C4 C5 1.504(6) . ? C4 H4 0.9300 . ? C5 N6 1.280(6) . ? C5 C6 1.417(6) . ? C6 C7 1.266(6) . ? C6 N5 1.440(6) . ? C7 C8 1.356(6) . ? C7 H7 0.9300 . ? C8 C12 1.354(7) . ? C8 C9 1.500(7) . ? C9 C10 1.240(8) . ? C9 H9 0.9300 . ? C10 N5 1.295(6) . ? C10 H10 0.9300 . ? C11 O13 1.175(5) . ? C11 O12 1.184(6) . ? C11 Yb1 3.013(5) 4 ? C12 O10 1.264(5) . ? C12 O11 1.322(6) . ? C13 N3 1.238(6) . ? C13 C14 1.257(7) . ? C13 H13 0.9300 . ? C14 C15 1.507(7) . ? C14 H14 0.9300 . ? C15 C16 1.291(6) . ? C15 C23 1.428(7) . ? C16 C17 1.313(7) . ? C16 H16 0.9300 . ? C17 C18 1.358(6) . ? C17 N3 1.442(6) . ? C18 N4 1.302(6) . ? C18 C19 1.479(6) . ? C19 C20 1.256(6) . ? C19 H19 0.9300 . ? C20 C21 1.317(7) . ? C20 C24 1.581(6) . ? C21 C22 1.484(6) . ? C21 H21 0.9300 . ? C22 N4 1.212(5) . ? C22 H22 0.9300 . ? C23 O8 1.185(5) . ? C23 O7 1.356(6) . ? C24 O5 1.136(6) . ? C24 O6 1.199(6) . ? C25 N1 1.358(6) . ? C25 C26 1.487(6) . ? C25 H25 0.9300 . ? C26 C27 1.543(6) . ? C26 H26 0.9300 . ? C27 C28 1.389(6) . ? C27 C35 1.622(5) . ? C28 C29 1.484(6) . ? C28 H28 0.9300 . ? C29 C30 1.482(6) . ? C29 N1 1.528(6) . ? C30 N2 1.478(6) . ? C30 C31 1.523(6) . ? C31 C32 1.403(6) . ? C31 H31 0.9300 . ? C32 C33 1.526(7) . ? C32 C36 1.623(6) . ? C33 C34 1.530(7) . ? C33 H33 0.9300 . ? C34 N2 1.342(5) . ? C34 H34 0.9300 . ? C35 O4 1.236(5) . ? C35 O3 1.372(5) . ? C35 Yb1 3.007(4) 3 ? C36 O1 1.203(6) . ? C36 O2 1.307(7) . ? O1 Yb1 2.311(3) 3_545 ? O3 Yb1 2.463(3) 3 ? O4 Yb1 2.714(3) 3 ? O5 Cu2 2.021(3) 4_554 ? O12 Yb1 2.503(3) 4 ? O13 Yb1 2.542(3) 4 ? O14 O15 1.616(10) 2 ? O17 O18 1.71(3) . ? O19 O20 1.79(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Yb1 O10 153.14(14) . . ? O8 Yb1 O1 74.77(14) . 3_455 ? O10 Yb1 O1 78.50(13) . 3_455 ? O8 Yb1 O3 82.65(13) . 3_445 ? O10 Yb1 O3 110.22(13) . 3_445 ? O1 Yb1 O3 122.66(12) 3_455 3_445 ? O8 Yb1 O12 130.54(13) . 4_545 ? O10 Yb1 O12 75.99(12) . 4_545 ? O1 Yb1 O12 151.08(11) 3_455 4_545 ? O3 Yb1 O12 79.44(11) 3_445 4_545 ? O8 Yb1 O13 87.81(13) . 4_545 ? O10 Yb1 O13 116.26(12) . 4_545 ? O1 Yb1 O13 144.81(12) 3_455 4_545 ? O3 Yb1 O13 83.87(11) 3_445 4_545 ? O12 Yb1 O13 44.81(10) 4_545 4_545 ? O8 Yb1 O9 102.00(16) . . ? O10 Yb1 O9 79.24(15) . . ? O1 Yb1 O9 87.63(15) 3_455 . ? O3 Yb1 O9 149.14(14) 3_445 . ? O12 Yb1 O9 74.48(14) 4_545 . ? O13 Yb1 O9 66.04(13) 4_545 . ? O8 Yb1 O4 81.96(13) . 3_445 ? O10 Yb1 O4 88.22(12) . 3_445 ? O1 Yb1 O4 73.77(11) 3_455 3_445 ? O3 Yb1 O4 51.02(10) 3_445 3_445 ? O12 Yb1 O4 118.45(10) 4_545 3_445 ? O13 Yb1 O4 134.57(10) 4_545 3_445 ? O9 Yb1 O4 159.39(13) . 3_445 ? O8 Yb1 C35 82.08(14) . 3_445 ? O10 Yb1 C35 98.91(13) . 3_445 ? O1 Yb1 C35 97.26(12) 3_455 3_445 ? O3 Yb1 C35 26.77(11) 3_445 3_445 ? O12 Yb1 C35 99.92(11) 4_545 3_445 ? O13 Yb1 C35 110.56(11) 4_545 3_445 ? O9 Yb1 C35 174.36(14) . 3_445 ? O4 Yb1 C35 24.26(10) 3_445 3_445 ? O8 Yb1 C11 109.59(14) . 4_545 ? O10 Yb1 C11 95.82(13) . 4_545 ? O1 Yb1 C11 155.32(13) 3_455 4_545 ? O3 Yb1 C11 81.92(11) 3_445 4_545 ? O12 Yb1 C11 22.43(11) 4_545 4_545 ? O13 Yb1 C11 22.42(11) 4_545 4_545 ? O9 Yb1 C11 67.69(15) . 4_545 ? O4 Yb1 C11 130.47(11) 3_445 4_545 ? C35 Yb1 C11 107.38(12) 3_445 4_545 ? N5 Cu1 N5 176.3(2) 2 . ? N5 Cu1 O14 91.87(12) 2 . ? N5 Cu1 O14 91.87(12) . . ? N5 Cu1 N6 103.76(15) 2 . ? N5 Cu1 N6 74.11(15) . . ? O14 Cu1 N6 123.31(10) . . ? N5 Cu1 N6 74.11(15) 2 2 ? N5 Cu1 N6 103.77(15) . 2 ? O14 Cu1 N6 123.31(10) . 2 ? N6 Cu1 N6 113.38(19) . 2 ? N5 Cu1 O15 83.6(3) 2 . ? N5 Cu1 O15 99.2(3) . . ? O14 Cu1 O15 42.3(3) . . ? N6 Cu1 O15 164.9(3) . . ? N6 Cu1 O15 81.2(3) 2 . ? N5 Cu1 O15 99.2(3) 2 2 ? N5 Cu1 O15 83.6(3) . 2 ? O14 Cu1 O15 42.3(3) . 2 ? N6 Cu1 O15 81.2(3) . 2 ? N6 Cu1 O15 164.9(3) 2 2 ? O15 Cu1 O15 84.6(6) . 2 ? N3 Cu2 O5 88.10(14) . 4_544 ? N3 Cu2 N1 106.50(15) . . ? O5 Cu2 N1 165.38(14) 4_544 . ? N3 Cu2 N4 70.64(14) . . ? O5 Cu2 N4 82.93(13) 4_544 . ? N1 Cu2 N4 100.84(14) . . ? N3 Cu2 N2 118.53(14) . . ? O5 Cu2 N2 100.41(13) 4_544 . ? N1 Cu2 N2 73.66(13) . . ? N4 Cu2 N2 170.12(14) . . ? N6 C1 C2 129.6(4) . . ? N6 C1 H1 115.2 . . ? C2 C1 H1 115.2 . . ? C3 C2 C1 125.8(4) . . ? C3 C2 H2 117.1 . . ? C1 C2 H2 117.1 . . ? C2 C3 C4 105.7(4) . . ? C2 C3 C11 128.4(4) . . ? C4 C3 C11 125.9(4) . . ? C3 C4 C5 125.6(4) . . ? C3 C4 H4 117.2 . . ? C5 C4 H4 117.2 . . ? N6 C5 C6 101.5(4) . . ? N6 C5 C4 127.7(4) . . ? C6 C5 C4 130.7(4) . . ? C7 C6 C5 112.7(4) . . ? C7 C6 N5 121.7(4) . . ? C5 C6 N5 125.5(4) . . ? C6 C7 C8 107.8(4) . . ? C6 C7 H7 126.1 . . ? C8 C7 H7 126.1 . . ? C12 C8 C7 110.8(4) . . ? C12 C8 C9 121.4(4) . . ? C7 C8 C9 127.8(4) . . ? C10 C9 C8 121.7(4) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C9 C10 N5 108.5(5) . . ? C9 C10 H10 125.8 . . ? N5 C10 H10 125.8 . . ? O13 C11 O12 109.3(4) . . ? O13 C11 C3 124.9(4) . . ? O12 C11 C3 125.8(4) . . ? O13 C11 Yb1 55.6(2) . 4 ? O12 C11 Yb1 53.8(2) . 4 ? C3 C11 Yb1 177.5(3) . 4 ? O10 C12 O11 135.9(5) . . ? O10 C12 C8 104.1(4) . . ? O11 C12 C8 120.0(4) . . ? N3 C13 C14 113.9(5) . . ? N3 C13 H13 123.1 . . ? C14 C13 H13 123.1 . . ? C13 C14 C15 123.9(4) . . ? C13 C14 H14 118.1 . . ? C15 C14 H14 118.1 . . ? C16 C15 C23 110.2(4) . . ? C16 C15 C14 123.7(5) . . ? C23 C15 C14 126.1(4) . . ? C15 C16 C17 107.6(4) . . ? C15 C16 H16 126.2 . . ? C17 C16 H16 126.2 . . ? C16 C17 C18 109.8(4) . . ? C16 C17 N3 128.4(4) . . ? C18 C17 N3 121.6(4) . . ? N4 C18 C17 103.7(4) . . ? N4 C18 C19 127.6(4) . . ? C17 C18 C19 128.7(4) . . ? C20 C19 C18 123.5(4) . . ? C20 C19 H19 118.3 . . ? C18 C19 H19 118.3 . . ? C19 C20 C21 108.5(4) . . ? C19 C20 C24 125.0(4) . . ? C21 C20 C24 126.5(4) . . ? C20 C21 C22 125.9(4) . . ? C20 C21 H21 117.0 . . ? C22 C21 H21 117.0 . . ? N4 C22 C21 125.7(4) . . ? N4 C22 H22 117.1 . . ? C21 C22 H22 117.1 . . ? O8 C23 O7 132.8(5) . . ? O8 C23 C15 102.1(4) . . ? O7 C23 C15 125.1(4) . . ? O5 C24 O6 116.3(5) . . ? O5 C24 C20 114.8(4) . . ? O6 C24 C20 128.9(4) . . ? N1 C25 C26 116.5(4) . . ? N1 C25 H25 121.8 . . ? C26 C25 H25 121.8 . . ? C25 C26 C27 125.8(4) . . ? C25 C26 H26 117.1 . . ? C27 C26 H26 117.1 . . ? C28 C27 C26 117.4(4) . . ? C28 C27 C35 114.9(4) . . ? C26 C27 C35 127.7(3) . . ? C27 C28 C29 115.5(4) . . ? C27 C28 H28 122.3 . . ? C29 C28 H28 122.3 . . ? C30 C29 C28 118.5(4) . . ? C30 C29 N1 114.8(4) . . ? C28 C29 N1 126.6(4) . . ? N2 C30 C29 109.2(4) . . ? N2 C30 C31 127.6(4) . . ? C29 C30 C31 123.1(4) . . ? C32 C31 C30 119.6(4) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 111.5(4) . . ? C31 C32 C36 121.2(4) . . ? C33 C32 C36 127.3(4) . . ? C32 C33 C34 126.9(4) . . ? C32 C33 H33 116.6 . . ? C34 C33 H33 116.6 . . ? N2 C34 C33 120.1(4) . . ? N2 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? O4 C35 O3 118.4(4) . . ? O4 C35 C27 116.0(4) . . ? O3 C35 C27 125.7(3) . . ? O4 C35 Yb1 64.5(2) . 3 ? O3 C35 Yb1 53.95(18) . 3 ? C27 C35 Yb1 176.4(3) . 3 ? O1 C36 O2 118.0(5) . . ? O1 C36 C32 118.1(4) . . ? O2 C36 C32 123.8(4) . . ? C25 N1 C29 118.0(4) . . ? C25 N1 Cu2 123.0(3) . . ? C29 N1 Cu2 119.1(2) . . ? C34 N2 C30 114.3(4) . . ? C34 N2 Cu2 123.4(3) . . ? C30 N2 Cu2 122.3(3) . . ? C13 N3 C17 122.5(4) . . ? C13 N3 Cu2 120.4(4) . . ? C17 N3 Cu2 117.0(3) . . ? C22 N4 C18 108.4(4) . . ? C22 N4 Cu2 126.0(3) . . ? C18 N4 Cu2 125.5(3) . . ? C10 N5 C6 132.5(4) . . ? C10 N5 Cu1 109.2(3) . . ? C6 N5 Cu1 118.2(3) . . ? C1 N6 C5 105.5(4) . . ? C1 N6 Cu1 133.9(3) . . ? C5 N6 Cu1 120.6(3) . . ? C36 O1 Yb1 147.2(4) . 3_545 ? C35 O3 Yb1 99.3(2) . 3 ? C35 O4 Yb1 91.3(3) . 3 ? C24 O5 Cu2 119.0(3) . 4_554 ? C23 O8 Yb1 159.9(4) . . ? C12 O10 Yb1 132.4(3) . . ? C11 O12 Yb1 103.8(3) . 4 ? C11 O13 Yb1 102.0(3) . 4 ? O15 O14 Cu1 82.2(6) 2 . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.004 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.151 # Attachment '6.cif' data_r80219a _database_code_depnum_ccdc_archive 'CCDC 731500' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26 Cu1.50 Lu N6 O16' _chemical_formula_weight 1068.91 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' O O 0.0106 0.0060 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.830(8) _cell_length_b 12.258(3) _cell_length_c 26.898(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.41(3) _cell_angle_gamma 90.00 _cell_volume 7722(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4212 _exptl_absorpt_coefficient_mu 3.444 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6827 _exptl_absorpt_correction_T_max 0.7702 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 21921 _diffrn_reflns_av_R_equivalents 0.1484 _diffrn_reflns_av_sigmaI/netI 0.1594 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6732 _reflns_number_gt 4461 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6732 _refine_ls_number_parameters 569 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1112 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1400 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.005 _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 Lu1 Lu 0.372992(10) 0.216990(17) 0.954530(8) 0.01752(6) Uani 1 1 d . . . Cu1 Cu 0.74694(3) 0.21319(5) 1.13417(2) 0.01972(17) Uani 1 1 d . . . Cu2 Cu 0.5000 -0.24022(8) 0.7500 0.0267(3) Uani 1 2 d S . . C1 C 0.6352(3) 0.3067(4) 1.13175(18) 0.0204(14) Uani 1 1 d . . . C2 C 0.5798(2) 0.3329(4) 1.12068(18) 0.0157(5) Uani 1 1 d U . . H2 H 0.5687 0.3849 1.1406 0.019 Uiso 1 1 calc R . . C3 C 0.5389(3) 0.2798(4) 1.0783(2) 0.0227(15) Uani 1 1 d . . . C4 C 0.5589(3) 0.2037(5) 1.0508(2) 0.0252(16) Uani 1 1 d . . . H4 H 0.5333 0.1672 1.0224 0.030 Uiso 1 1 calc R . . C5 C 0.6150(2) 0.1818(4) 1.06470(19) 0.0183(14) Uani 1 1 d . . . H5 H 0.6271 0.1279 1.0465 0.022 Uiso 1 1 calc R . . C6 C 0.6813(2) 0.3510(4) 1.17955(19) 0.0196(14) Uani 1 1 d . . . C7 C 0.6712(2) 0.4286(4) 1.2124(2) 0.0204(14) Uani 1 1 d . . . H7 H 0.6353 0.4606 1.2044 0.025 Uiso 1 1 calc R . . C8 C 0.7146(2) 0.4578(4) 1.2570(2) 0.0233(14) Uani 1 1 d . . . C9 C 0.7665(3) 0.4061(4) 1.2693(2) 0.0246(15) Uani 1 1 d . . . H9 H 0.7950 0.4205 1.3011 0.030 Uiso 1 1 calc R . . C10 C 0.7761(3) 0.3333(4) 1.2346(2) 0.0226(15) Uani 1 1 d . . . H10 H 0.8118 0.3009 1.2419 0.027 Uiso 1 1 calc R . . C11 C 0.7079(3) 0.5505(4) 1.29211(19) 0.0230(14) Uani 1 1 d . . . C12 C 0.4755(2) 0.3010(4) 1.0655(2) 0.0204(14) Uani 1 1 d . . . C13 C 0.4248(2) -0.1228(4) 0.7928(2) 0.0208(14) Uani 1 1 d . . . C14 C 0.4030(3) -0.0590(4) 0.8240(2) 0.0285(15) Uani 1 1 d . . . H14 H 0.3637 -0.0522 0.8160 0.034 Uiso 1 1 calc R . . C15 C 0.4397(2) -0.0053(4) 0.86707(19) 0.0197(14) Uani 1 1 d . . . C16 C 0.4979(3) -0.0222(5) 0.8791(2) 0.0321(17) Uani 1 1 d . . . H16 H 0.5242 0.0112 0.9082 0.039 Uiso 1 1 calc R . . C17 C 0.5153(3) -0.0897(5) 0.8468(2) 0.0311(16) Uani 1 1 d . . . H17 H 0.5543 -0.1024 0.8551 0.037 Uiso 1 1 calc R . . C18 C 0.3868(2) -0.1772(4) 0.7442(2) 0.0243(14) Uani 1 1 d . . . C19 C 0.4163(2) 0.0703(5) 0.8995(2) 0.0255(15) Uani 1 1 d . . . C20 C 0.3084(2) -0.3115(4) 1.06324(19) 0.0187(13) Uani 1 1 d . . . C21 C 0.3382(3) -0.3591(4) 1.0336(2) 0.0237(15) Uani 1 1 d . . . H21 H 0.3610 -0.3173 1.0196 0.028 Uiso 1 1 calc R . . C22 C 0.3330(2) -0.4734(4) 1.0251(2) 0.0234(14) Uani 1 1 d . . . C23 C 0.2999(3) -0.5314(5) 1.0467(2) 0.0255(15) Uani 1 1 d . . . H23 H 0.2953 -0.6062 1.0409 0.031 Uiso 1 1 calc R . . C24 C 0.2727(3) -0.4783(4) 1.07773(19) 0.0229(14) Uani 1 1 d . . . H24 H 0.2509 -0.5188 1.0933 0.027 Uiso 1 1 calc R . . C25 C 0.3068(2) -0.1918(5) 1.0709(2) 0.0208(14) Uani 1 1 d . . . C26 C 0.3331(3) -0.1158(4) 1.0476(2) 0.0292(14) Uani 1 1 d . . . H26 H 0.3585 -0.1384 1.0309 0.035 Uiso 1 1 calc R . . C27 C 0.3206(2) -0.0076(4) 1.04990(19) 0.0223(14) Uani 1 1 d . . . C28 C 0.2859(3) 0.0258(4) 1.0787(2) 0.0298(16) Uani 1 1 d . . . H28 H 0.2768 0.0991 1.0800 0.036 Uiso 1 1 calc R . . C29 C 0.2654(3) -0.0516(4) 1.1052(2) 0.0316(15) Uani 1 1 d . . . H29 H 0.2442 -0.0296 1.1261 0.038 Uiso 1 1 calc R . . C30 C 0.1721(3) 0.3328(4) 0.7773(2) 0.0231(14) Uani 1 1 d . . . H30 H 0.1919 0.3740 0.7601 0.028 Uiso 1 1 calc R . . C31 C 0.2009(2) 0.2815(4) 0.8241(2) 0.0188(14) Uani 1 1 d . . . C32 C 0.1694(3) 0.2217(5) 0.8486(2) 0.0311(17) Uani 1 1 d . . . H32 H 0.1878 0.1855 0.8800 0.037 Uiso 1 1 calc R . . C33 C 0.1120(3) 0.2159(5) 0.8269(2) 0.0288(16) Uani 1 1 d . . . H33 H 0.0914 0.1768 0.8442 0.035 Uiso 1 1 calc R . . C34 C 0.2638(3) 0.2914(4) 0.8497(2) 0.0203(14) Uani 1 1 d . . . C35 C 0.3627(3) 0.4699(5) 0.9904(2) 0.0464(19) Uani 1 1 d . . . C36 C 0.3416(3) 0.0742(4) 1.0187(2) 0.0246(15) Uani 1 1 d . . . N1 N 0.6538(2) 0.2340(4) 1.10329(17) 0.0228(12) Uani 1 1 d . . . N2 N 0.7334(2) 0.3088(4) 1.18966(16) 0.0203(12) Uani 1 1 d . . . N3 N 0.4801(2) -0.1377(4) 0.80469(17) 0.0260(13) Uani 1 1 d . . . N4 N 0.4157(2) -0.2351(4) 0.71850(17) 0.0231(12) Uani 1 1 d . . . N5 N 0.2773(2) -0.3695(3) 1.08571(17) 0.0223(12) Uani 1 1 d . . . N6 N 0.2758(2) -0.1599(3) 1.10106(16) 0.0203(12) Uani 1 1 d . . . O1 O 0.45127(17) 0.1218(3) 0.93799(14) 0.0276(11) Uani 1 1 d . . . O2 O 0.36561(19) 0.0823(3) 0.88869(15) 0.0319(5) Uani 1 1 d U . . O3 O 0.31983(17) 0.1674(3) 1.01040(14) 0.0283(10) Uani 1 1 d . . . O4 O 0.37811(18) 0.0442(3) 0.99860(15) 0.0321(10) Uani 1 1 d . . . O5 O 0.44374(19) 0.2543(4) 1.02423(16) 0.0330(12) Uani 1 1 d . . . O6 O 0.45905(18) 0.3593(4) 1.09541(15) 0.0370(13) Uani 1 1 d . . . O7 O 0.28601(19) 0.2380(3) 0.89189(14) 0.0278(11) Uani 1 1 d . . . O8 O 0.3984(2) 0.3261(4) 0.8958(2) 0.0686(17) Uani 1 1 d . . . O9 O 0.3445(2) 0.3802(3) 0.97441(16) 0.0404(13) Uani 1 1 d . . . O10 O 0.4020(2) 0.5229(4) 0.9817(2) 0.0791(14) Uani 1 1 d . . . O11 O 0.6608(2) 0.5903(4) 1.28498(17) 0.0446(14) Uani 1 1 d . . . O12 O 0.75554(18) 0.5851(3) 1.32418(14) 0.0269(11) Uani 1 1 d . . . O13 O 0.5000 -0.4039(8) 0.7500 0.089(6) Uani 1 2 d SP . . O14 O 0.2904(2) 0.3547(4) 0.82887(16) 0.0395(13) Uani 1 1 d . . . O15 O 0.0078(5) 0.0622(8) 0.0504(5) 0.092(4) Uani 0.50 1 d P . . O16 O 0.0127(5) 1.0133(8) 0.1716(3) 0.056(3) Uani 0.50 1 d P . . O17 O 0.0115(5) 0.2337(7) 0.3230(4) 0.061(4) Uani 0.50 1 d P . . O18 O 0.0385(4) 0.2542(7) 0.4269(3) 0.0382(6) Uani 0.50 1 d PU . . O19 O 0.0889(5) 0.2635(9) 0.2721(5) 0.066(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.01864(12) 0.01624(11) 0.01704(10) -0.00083(8) 0.00505(8) 0.00047(9) Cu1 0.0208(3) 0.0201(3) 0.0181(3) 0.0026(2) 0.0063(2) 0.0015(3) Cu2 0.0227(5) 0.0341(5) 0.0257(4) 0.000 0.0116(3) 0.000 C1 0.034(3) 0.019(2) 0.006(2) -0.0005(19) 0.0043(19) -0.003(2) C2 0.0159(7) 0.0153(7) 0.0155(7) 0.0000(6) 0.0050(5) 0.0001(6) C3 0.028(3) 0.019(3) 0.018(2) -0.006(2) 0.003(2) -0.005(2) C4 0.021(3) 0.032(3) 0.019(2) 0.004(2) 0.001(2) -0.001(3) C5 0.018(3) 0.022(3) 0.010(2) -0.003(2) -0.0027(19) -0.005(2) C6 0.019(3) 0.020(3) 0.016(2) 0.003(2) 0.001(2) 0.005(2) C7 0.005(3) 0.023(3) 0.028(3) 0.004(2) -0.001(2) -0.003(2) C8 0.023(3) 0.023(3) 0.026(2) 0.002(2) 0.010(2) -0.002(2) C9 0.027(3) 0.028(3) 0.013(2) 0.003(2) 0.000(2) -0.005(3) C10 0.021(3) 0.028(3) 0.013(2) 0.002(2) -0.002(2) 0.002(3) C11 0.028(3) 0.026(3) 0.015(2) -0.002(2) 0.0082(19) 0.003(2) C12 0.020(3) 0.025(3) 0.015(2) 0.006(2) 0.003(2) 0.006(2) C13 0.013(3) 0.017(2) 0.030(3) -0.003(2) 0.005(2) -0.002(2) C14 0.032(3) 0.026(3) 0.033(3) 0.007(2) 0.019(2) 0.006(2) C15 0.012(3) 0.025(3) 0.019(2) 0.004(2) 0.0021(19) 0.006(2) C16 0.013(3) 0.043(3) 0.036(3) -0.006(3) 0.002(2) -0.004(3) C17 0.020(3) 0.042(3) 0.034(3) -0.018(3) 0.012(2) -0.007(3) C18 0.027(3) 0.018(2) 0.033(2) 0.005(2) 0.017(2) -0.006(2) C19 0.010(3) 0.033(3) 0.036(3) 0.004(2) 0.011(2) 0.005(2) C20 0.013(3) 0.027(3) 0.015(2) 0.006(2) 0.0050(18) 0.000(2) C21 0.031(3) 0.018(2) 0.019(2) -0.004(2) 0.005(2) -0.014(2) C22 0.020(3) 0.025(3) 0.024(2) 0.005(2) 0.007(2) -0.009(2) C23 0.036(3) 0.021(3) 0.014(2) 0.005(2) 0.002(2) -0.001(3) C24 0.027(3) 0.026(3) 0.016(2) 0.004(2) 0.007(2) -0.009(2) C25 0.016(3) 0.030(3) 0.012(2) 0.002(2) -0.002(2) -0.005(2) C26 0.046(3) 0.015(2) 0.037(2) -0.008(2) 0.027(2) -0.006(2) C27 0.026(3) 0.023(3) 0.022(2) 0.004(2) 0.0122(19) 0.000(2) C28 0.045(4) 0.016(3) 0.031(3) 0.001(2) 0.017(2) 0.007(3) C29 0.035(3) 0.025(3) 0.045(3) 0.005(2) 0.026(2) 0.002(3) C30 0.024(3) 0.025(3) 0.021(2) -0.007(2) 0.008(2) -0.001(2) C31 0.017(3) 0.020(3) 0.019(2) -0.002(2) 0.0049(19) 0.011(2) C32 0.035(3) 0.030(3) 0.029(3) 0.007(2) 0.012(2) 0.007(3) C33 0.028(3) 0.034(3) 0.029(3) 0.001(2) 0.015(2) -0.007(3) C34 0.025(3) 0.017(2) 0.013(2) -0.006(2) -0.001(2) 0.010(2) C35 0.078(4) 0.026(3) 0.047(3) 0.011(3) 0.035(3) 0.018(3) C36 0.041(3) 0.012(2) 0.022(2) -0.008(2) 0.013(2) -0.008(2) N1 0.018(2) 0.029(2) 0.025(2) 0.0023(19) 0.0116(17) 0.000(2) N2 0.016(2) 0.027(2) 0.0179(19) 0.0071(18) 0.0056(16) 0.000(2) N3 0.023(3) 0.033(3) 0.025(2) 0.002(2) 0.0118(17) 0.007(2) N4 0.019(2) 0.028(2) 0.024(2) -0.0037(19) 0.0079(17) 0.004(2) N5 0.027(3) 0.014(2) 0.025(2) 0.0007(18) 0.0076(18) -0.001(2) N6 0.029(3) 0.017(2) 0.0144(18) 0.0055(17) 0.0068(17) 0.007(2) O1 0.014(2) 0.038(2) 0.0292(18) -0.0122(17) 0.0054(15) -0.0002(18) O2 0.0318(7) 0.0323(7) 0.0315(7) -0.0011(6) 0.0103(5) 0.0004(6) O3 0.030(2) 0.0240(19) 0.0379(18) 0.0072(16) 0.0204(15) 0.0012(17) O4 0.051(2) 0.0117(17) 0.0460(18) 0.0079(15) 0.0334(15) 0.0067(17) O5 0.011(2) 0.051(2) 0.029(2) -0.020(2) -0.0043(17) 0.002(2) O6 0.012(2) 0.066(3) 0.0298(19) -0.019(2) 0.0024(16) -0.001(2) O7 0.025(2) 0.034(2) 0.0182(18) 0.0065(17) -0.0011(16) 0.0152(19) O8 0.042(3) 0.083(3) 0.083(3) 0.061(3) 0.024(2) 0.004(3) O9 0.065(3) 0.0176(19) 0.034(2) -0.0027(18) 0.010(2) 0.016(2) O10 0.134(3) 0.031(2) 0.124(3) -0.004(2) 0.112(2) -0.001(2) O11 0.032(3) 0.055(3) 0.046(2) -0.030(2) 0.0117(19) 0.000(2) O12 0.025(2) 0.029(2) 0.0269(18) -0.0150(16) 0.0087(15) -0.0060(18) O13 0.020(7) 0.020(5) 0.196(14) 0.000 -0.007(9) 0.000 O14 0.032(3) 0.046(3) 0.034(2) 0.013(2) 0.0028(19) -0.001(2) O15 0.063(6) 0.029(5) 0.218(10) -0.010(6) 0.092(6) -0.010(5) O16 0.077(6) 0.061(6) 0.042(4) -0.009(4) 0.036(4) -0.009(5) O17 0.096(8) 0.029(5) 0.066(6) -0.008(4) 0.035(5) -0.006(5) O18 0.0379(7) 0.0386(8) 0.0382(8) -0.0003(6) 0.0129(5) 0.0002(6) O19 0.040(6) 0.060(6) 0.113(7) 0.000(6) 0.045(5) -0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 O5 2.150(4) . ? Lu1 O9 2.246(4) . ? Lu1 O7 2.270(4) . ? Lu1 O8 2.312(5) . ? Lu1 O2 2.384(4) . ? Lu1 O3 2.385(4) . ? Lu1 O4 2.410(4) . ? Lu1 O1 2.432(4) . ? Cu1 O12 1.942(4) 4_647 ? Cu1 N5 1.987(5) 3 ? Cu1 N2 2.012(5) . ? Cu1 N6 2.038(5) 3 ? Cu1 N1 2.197(5) . ? Cu2 N4 1.980(5) 2_656 ? Cu2 N4 1.980(5) . ? Cu2 O13 2.006(9) . ? Cu2 N3 2.114(5) 2_656 ? Cu2 N3 2.114(5) . ? C1 C2 1.346(8) . ? C1 N1 1.353(7) . ? C1 C6 1.511(7) . ? C2 C3 1.408(7) . ? C2 H2 0.9300 . ? C3 C4 1.382(8) . ? C3 C12 1.517(9) . ? C4 C5 1.345(8) . ? C4 H4 0.9300 . ? C5 N1 1.323(7) . ? C5 H5 0.9300 . ? C6 N2 1.335(7) . ? C6 C7 1.377(8) . ? C7 C8 1.368(7) . ? C7 H7 0.9300 . ? C8 C9 1.374(8) . ? C8 C11 1.522(8) . ? C9 C10 1.368(8) . ? C9 H9 0.9300 . ? C10 N2 1.350(7) . ? C10 H10 0.9300 . ? C11 O11 1.224(8) . ? C11 O12 1.282(7) . ? C12 O6 1.243(7) . ? C12 O5 1.265(6) . ? C13 N3 1.317(7) . ? C13 C14 1.382(8) . ? C13 C18 1.492(7) . ? C14 C15 1.379(7) . ? C14 H14 0.9300 . ? C15 C16 1.387(9) . ? C15 C19 1.515(8) . ? C16 C17 1.372(9) . ? C16 H16 0.9300 . ? C17 N3 1.317(7) . ? C17 H17 0.9300 . ? C18 N4 1.350(8) . ? C18 C30 1.387(8) 4_546 ? C19 O2 1.204(7) . ? C19 O1 1.274(6) . ? C20 N5 1.333(7) . ? C20 C21 1.383(8) . ? C20 C25 1.484(8) . ? C21 C22 1.419(7) . ? C21 H21 0.9300 . ? C22 C23 1.355(9) . ? C22 C35 1.536(9) 1_545 ? C23 C24 1.396(9) . ? C23 H23 0.9300 . ? C24 N5 1.349(7) . ? C24 H24 0.9300 . ? C25 N6 1.350(8) . ? C25 C26 1.397(8) . ? C26 C27 1.368(7) . ? C26 H26 0.9300 . ? C27 C28 1.396(9) . ? C27 C36 1.508(8) . ? C28 C29 1.382(8) . ? C28 H28 0.9300 . ? C29 N6 1.363(7) . ? C29 H29 0.9300 . ? C30 C31 1.375(7) . ? C30 C18 1.387(8) 4_556 ? C30 H30 0.9300 . ? C31 C32 1.389(9) . ? C31 C34 1.487(8) . ? C32 C33 1.349(9) . ? C32 H32 0.9300 . ? C33 N4 1.330(7) 4_556 ? C33 H33 0.9300 . ? C34 O14 1.266(8) . ? C34 O7 1.267(6) . ? C35 O9 1.212(7) . ? C35 O10 1.256(9) . ? C35 C22 1.536(9) 1_565 ? C36 O3 1.252(6) . ? C36 O4 1.255(8) . ? N4 C33 1.330(7) 4_546 ? N5 Cu1 1.987(5) 3_445 ? N6 Cu1 2.038(4) 3_445 ? O12 Cu1 1.942(4) 4_657 ? 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 O5 Lu1 O9 80.42(16) . . ? O5 Lu1 O7 157.45(16) . . ? O9 Lu1 O7 77.19(15) . . ? O5 Lu1 O8 98.26(19) . . ? O9 Lu1 O8 80.02(19) . . ? O7 Lu1 O8 80.53(17) . . ? O5 Lu1 O2 129.36(16) . . ? O9 Lu1 O2 147.34(14) . . ? O7 Lu1 O2 73.01(15) . . ? O8 Lu1 O2 82.18(18) . . ? O5 Lu1 O3 88.15(16) . . ? O9 Lu1 O3 78.05(16) . . ? O7 Lu1 O3 84.68(15) . . ? O8 Lu1 O3 155.78(17) . . ? O2 Lu1 O3 111.68(14) . . ? O5 Lu1 O4 82.17(15) . . ? O9 Lu1 O4 129.45(16) . . ? O7 Lu1 O4 110.27(14) . . ? O8 Lu1 O4 149.62(18) . . ? O2 Lu1 O4 74.63(13) . . ? O3 Lu1 O4 54.25(14) . . ? O5 Lu1 O1 77.91(15) . . ? O9 Lu1 O1 143.67(17) . . ? O7 Lu1 O1 122.68(14) . . ? O8 Lu1 O1 74.70(18) . . ? O2 Lu1 O1 53.15(14) . . ? O3 Lu1 O1 129.52(13) . . ? O4 Lu1 O1 75.73(14) . . ? O12 Cu1 N5 93.31(18) 4_647 3 ? O12 Cu1 N2 89.88(17) 4_647 . ? N5 Cu1 N2 167.72(19) 3 . ? O12 Cu1 N6 162.33(18) 4_647 3 ? N5 Cu1 N6 80.64(18) 3 3 ? N2 Cu1 N6 92.82(18) . 3 ? O12 Cu1 N1 94.63(18) 4_647 . ? N5 Cu1 N1 113.12(18) 3 . ? N2 Cu1 N1 78.39(18) . . ? N6 Cu1 N1 103.02(18) 3 . ? N4 Cu2 N4 176.4(3) 2_656 . ? N4 Cu2 O13 91.80(14) 2_656 . ? N4 Cu2 O13 91.80(14) . . ? N4 Cu2 N3 79.72(19) 2_656 2_656 ? N4 Cu2 N3 98.11(19) . 2_656 ? O13 Cu2 N3 126.48(13) . 2_656 ? N4 Cu2 N3 98.11(19) 2_656 . ? N4 Cu2 N3 79.72(19) . . ? O13 Cu2 N3 126.48(13) . . ? N3 Cu2 N3 107.0(3) 2_656 . ? C2 C1 N1 123.3(5) . . ? C2 C1 C6 122.2(5) . . ? N1 C1 C6 114.4(5) . . ? C1 C2 C3 118.5(5) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 117.0(5) . . ? C4 C3 C12 121.6(5) . . ? C2 C3 C12 121.3(5) . . ? C5 C4 C3 120.6(5) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? N1 C5 C4 122.7(5) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? N2 C6 C7 120.6(5) . . ? N2 C6 C1 116.3(5) . . ? C7 C6 C1 123.0(5) . . ? C8 C7 C6 119.0(5) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C7 C8 C9 119.5(5) . . ? C7 C8 C11 121.6(5) . . ? C9 C8 C11 118.8(5) . . ? C10 C9 C8 120.0(5) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? N2 C10 C9 119.4(6) . . ? N2 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? O11 C11 O12 126.4(5) . . ? O11 C11 C8 119.8(5) . . ? O12 C11 C8 113.5(5) . . ? O6 C12 O5 125.8(6) . . ? O6 C12 C3 119.4(5) . . ? O5 C12 C3 114.8(5) . . ? N3 C13 C14 121.2(5) . . ? N3 C13 C18 117.0(5) . . ? C14 C13 C18 121.8(5) . . ? C15 C14 C13 119.9(6) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 118.1(5) . . ? C14 C15 C19 120.2(5) . . ? C16 C15 C19 121.7(5) . . ? C17 C16 C15 117.7(5) . . ? C17 C16 H16 121.1 . . ? C15 C16 H16 121.1 . . ? N3 C17 C16 123.8(6) . . ? N3 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? N4 C18 C30 119.9(5) . 4_546 ? N4 C18 C13 113.3(5) . . ? C30 C18 C13 126.6(5) 4_546 . ? O2 C19 O1 120.8(5) . . ? O2 C19 C15 120.3(5) . . ? O1 C19 C15 118.9(5) . . ? N5 C20 C21 122.5(5) . . ? N5 C20 C25 114.7(5) . . ? C21 C20 C25 122.7(5) . . ? C20 C21 C22 118.2(5) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? C23 C22 C21 119.0(6) . . ? C23 C22 C35 120.4(5) . 1_545 ? C21 C22 C35 120.5(5) . 1_545 ? C22 C23 C24 119.6(5) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? N5 C24 C23 121.6(5) . . ? N5 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? N6 C25 C26 121.3(5) . . ? N6 C25 C20 114.6(5) . . ? C26 C25 C20 124.0(5) . . ? C27 C26 C25 118.7(6) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C26 C27 C28 120.0(5) . . ? C26 C27 C36 119.6(5) . . ? C28 C27 C36 120.3(5) . . ? C29 C28 C27 119.0(5) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? N6 C29 C28 120.9(6) . . ? N6 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C31 C30 C18 119.8(5) . 4_556 ? C31 C30 H30 120.1 . . ? C18 C30 H30 120.1 4_556 . ? C30 C31 C32 118.1(5) . . ? C30 C31 C34 122.3(5) . . ? C32 C31 C34 119.6(5) . . ? C33 C32 C31 120.2(5) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? N4 C33 C32 121.5(6) 4_556 . ? N4 C33 H33 119.2 4_556 . ? C32 C33 H33 119.2 . . ? O14 C34 O7 125.3(6) . . ? O14 C34 C31 117.9(5) . . ? O7 C34 C31 116.8(5) . . ? O9 C35 O10 128.7(7) . . ? O9 C35 C22 115.3(6) . 1_565 ? O10 C35 C22 116.0(5) . 1_565 ? O3 C36 O4 121.4(5) . . ? O3 C36 C27 119.8(6) . . ? O4 C36 C27 118.6(5) . . ? C5 N1 C1 117.7(5) . . ? C5 N1 Cu1 129.9(4) . . ? C1 N1 Cu1 112.2(3) . . ? C6 N2 C10 121.1(5) . . ? C6 N2 Cu1 117.6(3) . . ? C10 N2 Cu1 121.2(4) . . ? C17 N3 C13 119.2(5) . . ? C17 N3 Cu2 128.5(4) . . ? C13 N3 Cu2 112.3(3) . . ? C33 N4 C18 120.4(5) 4_546 . ? C33 N4 Cu2 122.0(4) 4_546 . ? C18 N4 Cu2 117.6(3) . . ? C20 N5 C24 119.1(5) . . ? C20 N5 Cu1 115.4(3) . 3_445 ? C24 N5 Cu1 125.3(4) . 3_445 ? C25 N6 C29 119.5(5) . . ? C25 N6 Cu1 113.3(3) . 3_445 ? C29 N6 Cu1 127.1(4) . 3_445 ? C19 O1 Lu1 90.9(3) . . ? C19 O2 Lu1 95.1(4) . . ? C36 O3 Lu1 92.8(4) . . ? C36 O4 Lu1 91.5(3) . . ? C12 O5 Lu1 162.2(4) . . ? C34 O7 Lu1 138.4(4) . . ? C35 O9 Lu1 141.5(5) . . ? C11 O12 Cu1 117.2(4) . 4_657 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 2.0(8) . . . . ? C6 C1 C2 C3 -173.8(5) . . . . ? C1 C2 C3 C4 -0.1(8) . . . . ? C1 C2 C3 C12 176.8(5) . . . . ? C2 C3 C4 C5 0.5(8) . . . . ? C12 C3 C4 C5 -176.3(5) . . . . ? C3 C4 C5 N1 -2.9(9) . . . . ? C2 C1 C6 N2 172.1(5) . . . . ? N1 C1 C6 N2 -4.0(7) . . . . ? C2 C1 C6 C7 -6.2(8) . . . . ? N1 C1 C6 C7 177.7(5) . . . . ? N2 C6 C7 C8 -3.2(8) . . . . ? C1 C6 C7 C8 175.0(5) . . . . ? C6 C7 C8 C9 -2.8(8) . . . . ? C6 C7 C8 C11 174.1(5) . . . . ? C7 C8 C9 C10 6.1(9) . . . . ? C11 C8 C9 C10 -170.9(5) . . . . ? C8 C9 C10 N2 -3.4(9) . . . . ? C7 C8 C11 O11 10.3(9) . . . . ? C9 C8 C11 O11 -172.7(6) . . . . ? C7 C8 C11 O12 -163.8(5) . . . . ? C9 C8 C11 O12 13.2(7) . . . . ? C4 C3 C12 O6 170.7(5) . . . . ? C2 C3 C12 O6 -6.1(8) . . . . ? C4 C3 C12 O5 -8.2(8) . . . . ? C2 C3 C12 O5 175.0(5) . . . . ? N3 C13 C14 C15 3.1(8) . . . . ? C18 C13 C14 C15 -176.5(5) . . . . ? C13 C14 C15 C16 -3.3(8) . . . . ? C13 C14 C15 C19 176.3(5) . . . . ? C14 C15 C16 C17 1.2(9) . . . . ? C19 C15 C16 C17 -178.3(5) . . . . ? C15 C16 C17 N3 1.2(9) . . . . ? N3 C13 C18 N4 -0.3(7) . . . . ? C14 C13 C18 N4 179.3(5) . . . . ? N3 C13 C18 C30 -175.8(5) . . . 4_546 ? C14 C13 C18 C30 3.8(9) . . . 4_546 ? C14 C15 C19 O2 1.6(8) . . . . ? C16 C15 C19 O2 -178.9(6) . . . . ? C14 C15 C19 O1 -177.5(5) . . . . ? C16 C15 C19 O1 1.9(8) . . . . ? N5 C20 C21 C22 2.9(8) . . . . ? C25 C20 C21 C22 -174.7(5) . . . . ? C20 C21 C22 C23 -0.8(8) . . . . ? C20 C21 C22 C35 177.1(5) . . . 1_545 ? C21 C22 C23 C24 -1.4(8) . . . . ? C35 C22 C23 C24 -179.3(5) 1_545 . . . ? C22 C23 C24 N5 1.8(8) . . . . ? N5 C20 C25 N6 2.3(6) . . . . ? C21 C20 C25 N6 -179.9(5) . . . . ? N5 C20 C25 C26 -175.4(5) . . . . ? C21 C20 C25 C26 2.5(8) . . . . ? N6 C25 C26 C27 -8.8(8) . . . . ? C20 C25 C26 C27 168.7(5) . . . . ? C25 C26 C27 C28 5.2(8) . . . . ? C25 C26 C27 C36 -171.4(5) . . . . ? C26 C27 C28 C29 0.9(8) . . . . ? C36 C27 C28 C29 177.4(5) . . . . ? C27 C28 C29 N6 -3.7(8) . . . . ? C18 C30 C31 C32 -0.7(8) 4_556 . . . ? C18 C30 C31 C34 -178.4(5) 4_556 . . . ? C30 C31 C32 C33 -0.7(8) . . . . ? C34 C31 C32 C33 177.1(5) . . . . ? C31 C32 C33 N4 1.3(9) . . . 4_556 ? C30 C31 C34 O14 4.3(8) . . . . ? C32 C31 C34 O14 -173.4(5) . . . . ? C30 C31 C34 O7 -178.0(5) . . . . ? C32 C31 C34 O7 4.3(7) . . . . ? C26 C27 C36 O3 163.1(5) . . . . ? C28 C27 C36 O3 -13.5(8) . . . . ? C26 C27 C36 O4 -12.0(8) . . . . ? C28 C27 C36 O4 171.5(5) . . . . ? C4 C5 N1 C1 4.5(8) . . . . ? C4 C5 N1 Cu1 179.2(4) . . . . ? C2 C1 N1 C5 -4.1(8) . . . . ? C6 C1 N1 C5 172.0(5) . . . . ? C2 C1 N1 Cu1 -179.7(4) . . . . ? C6 C1 N1 Cu1 -3.6(6) . . . . ? O12 Cu1 N1 C5 -79.1(5) 4_647 . . . ? N5 Cu1 N1 C5 16.5(5) 3 . . . ? N2 Cu1 N1 C5 -168.0(5) . . . . ? N6 Cu1 N1 C5 101.7(5) 3 . . . ? O12 Cu1 N1 C1 95.8(4) 4_647 . . . ? N5 Cu1 N1 C1 -168.6(3) 3 . . . ? N2 Cu1 N1 C1 6.9(4) . . . . ? N6 Cu1 N1 C1 -83.4(4) 3 . . . ? C7 C6 N2 C10 6.1(8) . . . . ? C1 C6 N2 C10 -172.3(5) . . . . ? C7 C6 N2 Cu1 -171.1(4) . . . . ? C1 C6 N2 Cu1 10.5(6) . . . . ? C9 C10 N2 C6 -2.8(8) . . . . ? C9 C10 N2 Cu1 174.3(4) . . . . ? O12 Cu1 N2 C6 -104.2(4) 4_647 . . . ? N5 Cu1 N2 C6 150.6(7) 3 . . . ? N6 Cu1 N2 C6 93.2(4) 3 . . . ? N1 Cu1 N2 C6 -9.5(4) . . . . ? O12 Cu1 N2 C10 78.6(4) 4_647 . . . ? N5 Cu1 N2 C10 -26.6(11) 3 . . . ? N6 Cu1 N2 C10 -84.0(4) 3 . . . ? N1 Cu1 N2 C10 173.3(4) . . . . ? C16 C17 N3 C13 -1.4(9) . . . . ? C16 C17 N3 Cu2 178.3(5) . . . . ? C14 C13 N3 C17 -0.7(8) . . . . ? C18 C13 N3 C17 178.8(5) . . . . ? C14 C13 N3 Cu2 179.5(4) . . . . ? C18 C13 N3 Cu2 -0.9(6) . . . . ? N4 Cu2 N3 C17 -1.4(5) 2_656 . . . ? N4 Cu2 N3 C17 -178.4(5) . . . . ? O13 Cu2 N3 C17 97.0(5) . . . . ? N3 Cu2 N3 C17 -83.0(5) 2_656 . . . ? N4 Cu2 N3 C13 178.4(4) 2_656 . . . ? N4 Cu2 N3 C13 1.3(4) . . . . ? O13 Cu2 N3 C13 -83.3(4) . . . . ? N3 Cu2 N3 C13 96.7(4) 2_656 . . . ? C30 C18 N4 C33 -1.0(8) 4_546 . . 4_546 ? C13 C18 N4 C33 -176.8(5) . . . 4_546 ? C30 C18 N4 Cu2 177.3(4) 4_546 . . . ? C13 C18 N4 Cu2 1.5(6) . . . . ? N4 Cu2 N4 C33 123.5(4) 2_656 . . 4_546 ? O13 Cu2 N4 C33 -56.5(4) . . . 4_546 ? N3 Cu2 N4 C33 70.7(5) 2_656 . . 4_546 ? N3 Cu2 N4 C33 176.7(5) . . . 4_546 ? N4 Cu2 N4 C18 -54.8(4) 2_656 . . . ? O13 Cu2 N4 C18 125.2(4) . . . . ? N3 Cu2 N4 C18 -107.5(4) 2_656 . . . ? N3 Cu2 N4 C18 -1.5(4) . . . . ? C21 C20 N5 C24 -2.6(7) . . . . ? C25 C20 N5 C24 175.2(4) . . . . ? C21 C20 N5 Cu1 172.1(4) . . . 3_445 ? C25 C20 N5 Cu1 -10.1(5) . . . 3_445 ? C23 C24 N5 C20 0.2(7) . . . . ? C23 C24 N5 Cu1 -173.9(4) . . . 3_445 ? C26 C25 N6 C29 6.1(8) . . . . ? C20 C25 N6 C29 -171.7(5) . . . . ? C26 C25 N6 Cu1 -176.0(4) . . . 3_445 ? C20 C25 N6 Cu1 6.2(5) . . . 3_445 ? C28 C29 N6 C25 0.3(8) . . . . ? C28 C29 N6 Cu1 -177.3(4) . . . 3_445 ? O2 C19 O1 Lu1 -2.7(6) . . . . ? C15 C19 O1 Lu1 176.4(4) . . . . ? O5 Lu1 O1 C19 167.7(4) . . . . ? O9 Lu1 O1 C19 -137.7(3) . . . . ? O7 Lu1 O1 C19 -22.4(4) . . . . ? O8 Lu1 O1 C19 -90.2(4) . . . . ? O2 Lu1 O1 C19 1.5(3) . . . . ? O3 Lu1 O1 C19 90.3(3) . . . . ? O4 Lu1 O1 C19 82.8(3) . . . . ? O1 C19 O2 Lu1 2.8(6) . . . . ? C15 C19 O2 Lu1 -176.3(5) . . . . ? O5 Lu1 O2 C19 -19.1(4) . . . . ? O9 Lu1 O2 C19 132.6(4) . . . . ? O7 Lu1 O2 C19 157.6(4) . . . . ? O8 Lu1 O2 C19 75.1(4) . . . . ? O3 Lu1 O2 C19 -125.5(4) . . . . ? O4 Lu1 O2 C19 -85.1(4) . . . . ? O1 Lu1 O2 C19 -1.6(3) . . . . ? O4 C36 O3 Lu1 0.5(5) . . . . ? C27 C36 O3 Lu1 -174.5(4) . . . . ? O5 Lu1 O3 C36 -81.9(3) . . . . ? O9 Lu1 O3 C36 -162.5(3) . . . . ? O7 Lu1 O3 C36 119.5(3) . . . . ? O8 Lu1 O3 C36 171.9(4) . . . . ? O2 Lu1 O3 C36 50.1(3) . . . . ? O4 Lu1 O3 C36 -0.3(3) . . . . ? O1 Lu1 O3 C36 -9.3(4) . . . . ? O3 C36 O4 Lu1 -0.5(5) . . . . ? C27 C36 O4 Lu1 174.5(4) . . . . ? O5 Lu1 O4 C36 93.6(3) . . . . ? O9 Lu1 O4 C36 22.9(4) . . . . ? O7 Lu1 O4 C36 -66.9(3) . . . . ? O8 Lu1 O4 C36 -173.4(4) . . . . ? O2 Lu1 O4 C36 -131.8(3) . . . . ? O3 Lu1 O4 C36 0.3(3) . . . . ? O1 Lu1 O4 C36 173.1(3) . . . . ? O6 C12 O5 Lu1 27.9(18) . . . . ? C3 C12 O5 Lu1 -153.3(12) . . . . ? O9 Lu1 O5 C12 5.7(14) . . . . ? O7 Lu1 O5 C12 -1.1(17) . . . . ? O8 Lu1 O5 C12 84.1(14) . . . . ? O2 Lu1 O5 C12 170.7(13) . . . . ? O3 Lu1 O5 C12 -72.4(14) . . . . ? O4 Lu1 O5 C12 -126.6(14) . . . . ? O1 Lu1 O5 C12 156.4(14) . . . . ? O14 C34 O7 Lu1 1.8(9) . . . . ? C31 C34 O7 Lu1 -175.7(4) . . . . ? O5 Lu1 O7 C34 82.7(7) . . . . ? O9 Lu1 O7 C34 75.8(5) . . . . ? O8 Lu1 O7 C34 -6.0(5) . . . . ? O2 Lu1 O7 C34 -90.7(5) . . . . ? O3 Lu1 O7 C34 154.7(5) . . . . ? O4 Lu1 O7 C34 -156.6(5) . . . . ? O1 Lu1 O7 C34 -70.9(6) . . . . ? O10 C35 O9 Lu1 34.9(11) . . . . ? C22 C35 O9 Lu1 -146.0(5) 1_565 . . . ? O5 Lu1 O9 C35 39.7(7) . . . . ? O7 Lu1 O9 C35 -143.0(7) . . . . ? O8 Lu1 O9 C35 -60.5(7) . . . . ? O2 Lu1 O9 C35 -118.5(7) . . . . ? O3 Lu1 O9 C35 129.8(7) . . . . ? O4 Lu1 O9 C35 111.2(7) . . . . ? O1 Lu1 O9 C35 -14.3(8) . . . . ? O11 C11 O12 Cu1 0.1(8) . . . 4_657 ? C8 C11 O12 Cu1 173.7(3) . . . 4_657 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.106 _refine_diff_density_min -1.580 _refine_diff_density_rms 0.254 # Attachment '41.cif' data_r80620d _database_code_depnum_ccdc_archive 'CCDC 731501' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26 Cu1.50 Ho N6 O16' _chemical_formula_weight 1058.87 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.922(5) _cell_length_b 12.285(3) _cell_length_c 26.811(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.21(3) _cell_angle_gamma 90.00 _cell_volume 7752(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4180 _exptl_absorpt_coefficient_mu 2.925 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7997 _exptl_absorpt_correction_T_max 0.9438 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 22052 _diffrn_reflns_av_R_equivalents 0.2251 _diffrn_reflns_av_sigmaI/netI 0.2338 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6802 _reflns_number_gt 3735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6802 _refine_ls_number_parameters 569 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.1480 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.1791 _refine_ls_wR_factor_gt 0.1433 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.003 _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 Ho1 Ho 0.126858(17) 1.21580(4) 1.045772(14) 0.01693(10) Uani 1 1 d . . . Cu1 Cu 0.25280(4) 0.71195(10) 0.86547(4) 0.0191(3) Uani 1 1 d . . . Cu2 Cu 0.0000 0.75475(15) 1.2500 0.0254(5) Uani 1 2 d S . . C1 C 0.5230(4) 0.8000(8) 0.9341(3) 0.028(3) Uani 1 1 d . . . C2 C 0.3845(4) 0.6798(8) 0.9346(3) 0.028(3) Uani 1 1 d . . . H2 H 0.3722 0.6263 0.9528 0.034 Uiso 1 1 calc R . . C3 C 0.4429(4) 0.7014(9) 0.9493(3) 0.031(3) Uani 1 1 d . . . H3 H 0.4689 0.6648 0.9772 0.037 Uiso 1 1 calc R . . C4 C 0.4599(3) 0.7783(8) 0.9210(3) 0.016(2) Uani 1 1 d . . . C5 C 0.4209(4) 0.8311(8) 0.8794(3) 0.0218(4) Uani 1 1 d U . . H5 H 0.4326 0.8829 0.8598 0.026 Uiso 1 1 calc R . . C6 C 0.3625(4) 0.8050(8) 0.8669(3) 0.0219(3) Uani 1 1 d U . . C7 C 0.3190(3) 0.8491(8) 0.8207(3) 0.020(2) Uani 1 1 d . . . C8 C 0.3289(3) 0.9269(8) 0.7874(3) 0.0167(8) Uani 1 1 d U . . H8 H 0.3649 0.9575 0.7948 0.020 Uiso 1 1 calc R . . C9 C 0.2862(4) 0.9580(8) 0.7442(3) 0.021(2) Uani 1 1 d . . . C10 C 0.2334(3) 0.9078(8) 0.7318(3) 0.016(2) Uani 1 1 d . . . H10 H 0.2044 0.9248 0.7006 0.019 Uiso 1 1 calc R . . C11 C 0.2245(4) 0.8322(8) 0.7664(3) 0.0210(8) Uani 1 1 d U . . H11 H 0.1888 0.8006 0.7593 0.025 Uiso 1 1 calc R . . C12 C 0.2919(4) 1.0520(8) 0.7087(3) 0.020(2) Uani 1 1 d . . . C13 C 0.1595(4) 1.0717(8) 0.9818(3) 0.024(3) Uani 1 1 d . . . C14 C 0.2351(4) 0.9417(8) 0.8954(3) 0.023(2) Uani 1 1 d . . . H14 H 0.2565 0.9618 0.8743 0.027 Uiso 1 1 calc R . . C15 C 0.2154(4) 1.0232(9) 0.9204(3) 0.0259(8) Uani 1 1 d U . . H15 H 0.2252 1.0957 0.9184 0.031 Uiso 1 1 calc R . . C16 C 0.1791(4) 0.9906(9) 0.9494(3) 0.024(3) Uani 1 1 d . . . C17 C 0.1675(4) 0.8811(8) 0.9532(3) 0.0213(4) Uani 1 1 d U . . H17 H 0.1433 0.8585 0.9712 0.026 Uiso 1 1 calc R . . C18 C 0.1932(4) 0.8046(8) 0.9288(3) 0.0212(5) Uani 1 1 d U . . C19 C 0.1903(3) 0.6873(8) 0.9366(3) 0.018(2) Uani 1 1 d . . . C20 C 0.1620(4) 0.6425(8) 0.9669(3) 0.0206(6) Uani 1 1 d U . . H20 H 0.1403 0.6856 0.9816 0.025 Uiso 1 1 calc R . . C21 C 0.1664(4) 0.5265(8) 0.9760(3) 0.019(2) Uani 1 1 d . . . C22 C 0.1992(4) 0.4696(9) 0.9538(3) 0.0249(4) Uani 1 1 d U . . H22 H 0.2037 0.3950 0.9595 0.030 Uiso 1 1 calc R . . C23 C 0.2265(4) 0.5216(8) 0.9222(3) 0.0250(5) Uani 1 1 d U . . H23 H 0.2477 0.4803 0.9064 0.030 Uiso 1 1 calc R . . C24 C 0.1363(5) 0.4749(10) 1.0099(4) 0.036(3) Uani 1 1 d . . . C25 C 0.2368(4) 1.2896(10) 1.1491(3) 0.033(3) Uani 1 1 d . . . C26 C 0.3887(4) 1.3196(8) 1.2439(3) 0.022(3) Uani 1 1 d . . . C27 C 0.3286(4) 1.3316(8) 1.2233(3) 0.024(2) Uani 1 1 d . . . H27 H 0.3092 1.3730 1.2409 0.028 Uiso 1 1 calc R . . C28 C 0.3001(4) 1.2797(8) 1.1762(3) 0.023(2) Uani 1 1 d . . . C29 C 0.3301(4) 1.2226(8) 1.1513(3) 0.027(3) Uani 1 1 d . . . H29 H 0.3113 1.1885 1.1193 0.032 Uiso 1 1 calc R . . C30 C 0.3876(4) 1.2147(9) 1.1726(3) 0.0285(8) Uani 1 1 d U . . H30 H 0.4071 1.1759 1.1543 0.034 Uiso 1 1 calc R . . C31 C 0.0817(4) 1.0682(8) 1.1009(3) 0.019(2) Uani 1 1 d . . . C32 C 0.0759(4) 0.8745(9) 1.2082(3) 0.026(3) Uani 1 1 d . . . C33 C 0.0973(4) 0.9389(8) 1.1759(3) 0.021(2) Uani 1 1 d . . . H33 H 0.1363 0.9452 1.1832 0.025 Uiso 1 1 calc R . . C34 C 0.0602(4) 0.9929(9) 1.1334(3) 0.0242(8) Uani 1 1 d U . . C35 C 0.0018(4) 0.9760(9) 1.1211(3) 0.030(3) Uani 1 1 d . . . H35 H -0.0241 1.0088 1.0917 0.036 Uiso 1 1 calc R . . C36 C -0.0162(4) 0.9110(9) 1.1530(3) 0.031(3) Uani 1 1 d . . . H36 H -0.0552 0.9018 1.1453 0.038 Uiso 1 1 calc R . . N1 N 0.2257(3) 0.8392(7) 0.8996(3) 0.021(2) Uani 1 1 d . . . N2 N 0.2228(3) 0.6280(6) 0.9144(2) 0.020(2) Uani 1 1 d . . . N3 N 0.3454(3) 0.7333(7) 0.8951(3) 0.0219(4) Uani 1 1 d U . . N4 N 0.2675(3) 0.8036(6) 0.8107(3) 0.021(2) Uani 1 1 d . . . N5 N 0.0198(3) 0.8573(7) 1.1965(2) 0.025(2) Uani 1 1 d . . . N6 N 0.4170(3) 1.2596(7) 1.2183(3) 0.027(2) Uani 1 1 d . . . O1 O 0.2450(2) 1.0834(6) 0.6757(2) 0.0251(18) Uani 1 1 d . . . O2 O 0.3389(3) 1.0922(7) 0.7165(2) 0.041(2) Uani 1 1 d . . . O3 O 0.5380(3) 0.8607(8) 0.9052(3) 0.058(3) Uani 1 1 d . . . O4 O 0.5549(3) 0.7532(6) 0.9749(2) 0.037(2) Uani 1 1 d . . . O5 O 0.1540(3) 0.3831(6) 1.0262(3) 0.046(2) Uani 1 1 d . . . O6 O 0.0968(4) 0.5278(7) 1.0189(3) 0.086(3) Uani 1 1 d . . . O7 O 0.1225(3) 1.0435(6) 1.0009(2) 0.0327(19) Uani 1 1 d . . . O8 O 0.1796(3) 1.1663(6) 0.9885(2) 0.0295(18) Uani 1 1 d . . . O9 O 0.2149(2) 1.2396(5) 1.1086(2) 0.0241(18) Uani 1 1 d . . . O10 O 0.2122(3) 1.3586(7) 1.1713(3) 0.040(2) Uani 1 1 d . . . O11 O 0.0493(3) 1.1183(6) 1.0646(2) 0.0270(18) Uani 1 1 d . . . O12 O 0.1353(3) 1.0781(5) 1.1122(2) 0.0267(18) Uani 1 1 d . . . O13 O 0.1043(3) 1.3186(9) 1.1102(3) 0.073(3) Uani 1 1 d . . . O14 O 0.0812(9) 0.2613(19) 0.2011(6) 0.089(8) Uani 0.50 1 d P . . O15 O 1.0186(7) 0.4448(14) 0.0606(5) 0.0504(8) Uani 0.50 1 d PU . . O16 O 0.0096(8) 0.6078(18) 1.1987(7) 0.090(5) Uani 0.70 1 d PU . . O17 O 0.9821(9) 0.264(2) 0.1725(8) 0.0204(8) Uani 0.25 1 d PU . . O18 O 0.9614(4) 0.2485(11) 0.0701(4) 0.072(4) Uani 0.75 1 d P . . O16' O 0.0000 0.594(2) 1.2500 0.091(5) Uani 0.60 2 d SPU . . 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 Ho1 0.01614(17) 0.0158(2) 0.01780(18) 0.0012(2) 0.00418(14) -0.0007(2) Cu1 0.0180(5) 0.0197(6) 0.0192(5) -0.0020(5) 0.0054(4) 0.0012(6) Cu2 0.0213(7) 0.0300(11) 0.0256(7) 0.000 0.0086(6) 0.000 C1 0.036(5) 0.020(6) 0.022(4) 0.011(4) 0.003(4) 0.012(5) C2 0.034(5) 0.022(6) 0.029(5) 0.000(4) 0.010(4) 0.005(5) C3 0.032(5) 0.039(7) 0.022(4) -0.002(5) 0.009(4) 0.011(6) C4 0.016(4) 0.014(5) 0.016(4) 0.008(4) 0.003(3) -0.001(4) C5 0.0218(6) 0.0220(6) 0.0218(6) -0.0001(5) 0.0073(5) 0.0000(5) C6 0.0218(5) 0.0220(5) 0.0218(5) -0.0001(4) 0.0073(4) 0.0000(4) C7 0.012(4) 0.017(5) 0.031(4) -0.019(4) 0.009(3) -0.001(4) C8 0.0166(9) 0.0168(10) 0.0168(10) -0.0004(7) 0.0058(6) 0.0002(7) C9 0.027(4) 0.012(5) 0.030(4) -0.007(4) 0.018(4) 0.000(5) C10 0.016(4) 0.017(5) 0.014(3) 0.002(4) 0.005(3) 0.002(4) C11 0.0208(9) 0.0213(10) 0.0211(10) -0.0002(7) 0.0069(6) 0.0000(7) C12 0.018(4) 0.011(5) 0.026(4) -0.003(4) 0.000(4) 0.000(4) C13 0.018(4) 0.018(5) 0.031(5) -0.007(4) 0.001(4) 0.006(5) C14 0.030(5) 0.016(5) 0.027(4) -0.005(4) 0.015(4) 0.002(5) C15 0.0261(9) 0.0258(10) 0.0258(10) 0.0003(7) 0.0087(6) -0.0003(7) C16 0.028(4) 0.032(6) 0.016(4) -0.003(4) 0.010(3) 0.010(5) C17 0.0211(6) 0.0212(6) 0.0215(6) -0.0002(5) 0.0071(5) -0.0003(5) C18 0.0211(6) 0.0212(6) 0.0214(6) -0.0002(5) 0.0070(5) -0.0003(5) C19 0.018(4) 0.021(6) 0.020(4) 0.002(4) 0.011(3) 0.003(4) C20 0.0207(7) 0.0206(7) 0.0206(7) 0.0000(5) 0.0069(5) 0.0001(5) C21 0.020(4) 0.010(5) 0.024(4) -0.001(4) 0.003(3) -0.003(4) C22 0.0251(6) 0.0246(6) 0.0248(6) 0.0001(5) 0.0080(5) 0.0001(5) C23 0.0252(6) 0.0248(6) 0.0248(6) 0.0000(5) 0.0080(5) 0.0000(5) C24 0.047(6) 0.036(7) 0.029(5) -0.013(5) 0.016(4) -0.005(6) C25 0.031(5) 0.040(6) 0.017(4) 0.004(5) -0.005(4) -0.016(6) C26 0.016(4) 0.027(6) 0.022(4) 0.002(4) 0.004(3) 0.000(4) C27 0.019(4) 0.031(6) 0.025(4) 0.009(4) 0.013(3) -0.002(5) C28 0.028(5) 0.015(5) 0.020(4) 0.005(4) 0.003(4) 0.011(5) C29 0.039(5) 0.015(5) 0.021(4) -0.010(4) 0.003(4) -0.008(5) C30 0.0286(9) 0.0286(10) 0.0286(10) 0.0002(7) 0.0098(6) 0.0000(7) C31 0.014(4) 0.023(6) 0.013(4) 0.004(4) -0.006(3) -0.001(4) C32 0.011(4) 0.036(7) 0.022(4) 0.003(5) -0.005(4) -0.008(5) C33 0.020(4) 0.022(6) 0.019(4) 0.002(4) 0.005(3) -0.006(5) C34 0.0241(9) 0.0238(10) 0.0241(10) -0.0001(7) 0.0072(6) 0.0000(7) C35 0.017(4) 0.049(7) 0.021(4) 0.010(5) 0.003(3) -0.013(5) C36 0.018(4) 0.045(7) 0.032(5) 0.011(5) 0.010(4) 0.007(5) N1 0.025(4) 0.017(4) 0.024(3) -0.006(3) 0.013(3) 0.006(4) N2 0.030(4) 0.003(4) 0.019(3) 0.000(3) -0.002(3) 0.001(4) N3 0.0219(6) 0.0221(6) 0.0218(6) 0.0000(5) 0.0072(5) -0.0001(5) N4 0.039(4) 0.005(4) 0.019(3) -0.002(3) 0.011(3) 0.006(4) N5 0.017(3) 0.041(6) 0.014(3) 0.002(4) 0.002(3) -0.006(4) N6 0.024(4) 0.027(5) 0.028(4) 0.007(4) 0.006(3) 0.003(4) O1 0.020(3) 0.031(4) 0.021(3) 0.005(3) 0.003(2) -0.011(3) O2 0.024(4) 0.048(5) 0.042(4) 0.019(4) 0.000(3) 0.005(4) O3 0.036(4) 0.092(7) 0.038(4) 0.036(4) 0.000(3) -0.032(5) O4 0.020(3) 0.053(6) 0.031(3) 0.006(3) 0.000(3) 0.012(4) O5 0.054(5) 0.023(4) 0.044(4) 0.014(4) -0.009(4) -0.012(4) O6 0.155(6) 0.028(5) 0.130(6) 0.013(5) 0.122(5) 0.009(6) O7 0.044(4) 0.021(4) 0.044(3) -0.007(3) 0.030(3) -0.010(4) O8 0.037(3) 0.023(4) 0.035(3) -0.014(3) 0.020(3) -0.007(4) O9 0.019(3) 0.034(4) 0.017(3) -0.001(3) 0.003(2) -0.016(3) O10 0.027(4) 0.041(5) 0.043(4) -0.014(4) -0.002(3) 0.002(4) O11 0.026(3) 0.031(4) 0.019(3) 0.008(3) 0.002(3) -0.016(3) O12 0.022(3) 0.023(4) 0.035(3) 0.012(3) 0.008(3) -0.003(3) O13 0.044(4) 0.106(8) 0.090(5) -0.056(5) 0.048(3) -0.024(5) O14 0.102(14) 0.12(2) 0.045(9) -0.019(11) 0.021(10) 0.035(14) O15 0.0505(10) 0.0502(10) 0.0506(10) -0.0001(7) 0.0167(7) 0.0001(7) O16 0.061(7) 0.084(7) 0.080(7) 0.009(6) -0.038(7) -0.012(6) O17 0.0206(10) 0.0204(10) 0.0202(11) 0.0001(7) 0.0067(7) 0.0001(7) O18 0.036(5) 0.114(12) 0.063(6) -0.037(7) 0.013(5) 0.023(7) O16' 0.060(8) 0.077(8) 0.082(8) 0.000 -0.050(7) 0.000 _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 Ho1 O4 2.189(6) 3_455 ? Ho1 O5 2.278(8) 1_565 ? Ho1 O9 2.303(5) . ? Ho1 O13 2.353(8) . ? Ho1 O8 2.405(7) . ? Ho1 O12 2.414(6) . ? Ho1 O7 2.419(7) . ? Ho1 O11 2.464(7) . ? Ho1 C13 2.766(10) . ? Ho1 C31 2.799(9) . ? Cu1 O1 1.937(7) 4_546 ? Cu1 N4 1.978(8) . ? Cu1 N2 1.997(8) . ? Cu1 N1 2.037(8) . ? Cu1 N3 2.194(7) . ? Cu2 N6 1.962(7) 4_547 ? Cu2 N6 1.962(7) 3_445 ? Cu2 O16' 1.97(3) . ? Cu2 N5 2.086(8) . ? Cu2 N5 2.086(8) 2_557 ? Cu2 O16 2.33(2) . ? Cu2 O16 2.33(2) 2_557 ? C1 O3 1.220(12) . ? C1 O4 1.260(10) . ? C1 C4 1.516(13) . ? C2 N3 1.351(11) . ? C2 C3 1.401(13) . ? C3 C4 1.364(14) . ? C4 C5 1.378(11) . ? C5 C6 1.418(12) . ? C6 N3 1.321(12) . ? C6 C7 1.457(11) . ? C7 N4 1.343(11) . ? C7 C8 1.386(13) . ? C8 C9 1.346(11) . ? C9 C10 1.391(12) . ? C9 C12 1.533(13) . ? C10 C11 1.381(12) . ? C11 N4 1.357(10) . ? C12 O2 1.224(11) . ? C12 O1 1.271(10) . ? C13 O7 1.240(12) . ? C13 O8 1.256(12) . ? C13 C16 1.505(14) . ? C14 N1 1.292(12) . ? C14 C15 1.382(14) . ? C15 C16 1.430(14) . ? C16 C17 1.387(14) . ? C17 C18 1.413(13) . ? C18 N1 1.365(12) . ? C18 C19 1.462(14) . ? C19 C20 1.356(13) . ? C19 N2 1.363(12) . ? C20 C21 1.444(13) . ? C21 C22 1.355(13) . ? C21 C24 1.496(14) . ? C22 C23 1.401(14) . ? C23 N2 1.322(12) . ? C24 O5 1.237(13) . ? C24 O6 1.267(14) . ? C25 O9 1.211(11) . ? C25 O10 1.299(13) . ? C25 C28 1.510(13) . ? C26 N6 1.354(12) . ? C26 C27 1.422(12) . ? C26 C32 1.462(12) 4_557 ? C27 C28 1.385(12) . ? C28 C29 1.351(14) . ? C29 C30 1.360(13) . ? C30 N6 1.322(11) . ? C31 O11 1.210(9) . ? C31 O12 1.274(10) . ? C31 C34 1.486(14) . ? C32 N5 1.347(11) . ? C32 C33 1.399(13) . ? C32 C26 1.462(12) 4_547 ? C33 C34 1.379(12) . ? C34 C35 1.399(13) . ? C35 C36 1.350(14) . ? C36 N5 1.382(11) . ? N6 Cu2 1.962(7) 3 ? O1 Cu1 1.937(7) 4_556 ? O4 Ho1 2.189(6) 3_545 ? O5 Ho1 2.278(8) 1_545 ? O16 O16' 1.48(2) . ? O16' O16 1.48(2) 2_557 ? 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 O4 Ho1 O5 80.3(3) 3_455 1_565 ? O4 Ho1 O9 156.8(3) 3_455 . ? O5 Ho1 O9 76.7(2) 1_565 . ? O4 Ho1 O13 101.5(3) 3_455 . ? O5 Ho1 O13 81.1(3) 1_565 . ? O9 Ho1 O13 78.2(2) . . ? O4 Ho1 O8 87.8(2) 3_455 . ? O5 Ho1 O8 79.4(3) 1_565 . ? O9 Ho1 O8 84.8(2) . . ? O13 Ho1 O8 156.6(3) . . ? O4 Ho1 O12 129.4(2) 3_455 . ? O5 Ho1 O12 147.3(2) 1_565 . ? O9 Ho1 O12 73.7(2) . . ? O13 Ho1 O12 79.5(3) . . ? O8 Ho1 O12 111.1(2) . . ? O4 Ho1 O7 82.1(2) 3_455 . ? O5 Ho1 O7 130.0(3) 1_565 . ? O9 Ho1 O7 110.5(2) . . ? O13 Ho1 O7 148.5(3) . . ? O8 Ho1 O7 53.5(2) . . ? O12 Ho1 O7 74.5(2) . . ? O4 Ho1 O11 78.8(2) 3_455 . ? O5 Ho1 O11 142.9(3) 1_565 . ? O9 Ho1 O11 122.3(2) . . ? O13 Ho1 O11 73.5(3) . . ? O8 Ho1 O11 129.7(2) . . ? O12 Ho1 O11 52.6(2) . . ? O7 Ho1 O11 76.6(2) . . ? O4 Ho1 C13 85.4(3) 3_455 . ? O5 Ho1 C13 105.4(3) 1_565 . ? O9 Ho1 C13 97.5(2) . . ? O13 Ho1 C13 171.4(3) . . ? O8 Ho1 C13 27.0(3) . . ? O12 Ho1 C13 92.1(3) . . ? O7 Ho1 C13 26.6(3) . . ? O11 Ho1 C13 103.1(3) . . ? O4 Ho1 C31 103.8(2) 3_455 . ? O5 Ho1 C31 155.1(3) 1_565 . ? O9 Ho1 C31 98.5(2) . . ? O13 Ho1 C31 74.0(3) . . ? O8 Ho1 C31 124.9(3) . . ? O12 Ho1 C31 27.0(2) . . ? O7 Ho1 C31 74.7(3) . . ? O11 Ho1 C31 25.6(2) . . ? C13 Ho1 C31 99.4(3) . . ? O1 Cu1 N4 89.7(3) 4_546 . ? O1 Cu1 N2 92.3(3) 4_546 . ? N4 Cu1 N2 169.2(3) . . ? O1 Cu1 N1 163.3(3) 4_546 . ? N4 Cu1 N1 93.8(3) . . ? N2 Cu1 N1 81.3(3) . . ? O1 Cu1 N3 94.6(3) 4_546 . ? N4 Cu1 N3 76.8(3) . . ? N2 Cu1 N3 113.6(3) . . ? N1 Cu1 N3 102.1(3) . . ? N6 Cu2 N6 176.5(5) 4_547 3_445 ? N6 Cu2 O16' 91.7(3) 4_547 . ? N6 Cu2 O16' 91.7(3) 3_445 . ? N6 Cu2 N5 80.0(3) 4_547 . ? N6 Cu2 N5 97.9(3) 3_445 . ? O16' Cu2 N5 127.1(2) . . ? N6 Cu2 N5 97.9(3) 4_547 2_557 ? N6 Cu2 N5 80.0(3) 3_445 2_557 ? O16' Cu2 N5 127.1(2) . 2_557 ? N5 Cu2 N5 105.7(5) . 2_557 ? N6 Cu2 O16 88.9(5) 4_547 . ? N6 Cu2 O16 93.8(5) 3_445 . ? O16' Cu2 O16 39.2(5) . . ? N5 Cu2 O16 88.2(6) . . ? N5 Cu2 O16 165.3(6) 2_557 . ? N6 Cu2 O16 93.8(5) 4_547 2_557 ? N6 Cu2 O16 88.9(5) 3_445 2_557 ? O16' Cu2 O16 39.2(5) . 2_557 ? N5 Cu2 O16 165.3(6) . 2_557 ? N5 Cu2 O16 88.2(6) 2_557 2_557 ? O16 Cu2 O16 78.4(11) . 2_557 ? O3 C1 O4 126.3(9) . . ? O3 C1 C4 118.1(8) . . ? O4 C1 C4 115.6(9) . . ? N3 C2 C3 123.0(9) . . ? C4 C3 C2 117.3(8) . . ? C3 C4 C5 120.7(8) . . ? C3 C4 C1 118.8(7) . . ? C5 C4 C1 120.5(8) . . ? C4 C5 C6 118.8(9) . . ? N3 C6 C5 121.1(8) . . ? N3 C6 C7 116.3(8) . . ? C5 C6 C7 122.5(8) . . ? N4 C7 C8 121.4(7) . . ? N4 C7 C6 114.3(8) . . ? C8 C7 C6 124.3(8) . . ? C9 C8 C7 119.4(8) . . ? C8 C9 C10 119.9(9) . . ? C8 C9 C12 122.6(8) . . ? C10 C9 C12 117.4(7) . . ? C11 C10 C9 119.1(7) . . ? N4 C11 C10 120.4(8) . . ? O2 C12 O1 127.3(9) . . ? O2 C12 C9 118.4(7) . . ? O1 C12 C9 114.1(8) . . ? O7 C13 O8 121.0(9) . . ? O7 C13 C16 118.7(9) . . ? O8 C13 C16 120.3(9) . . ? O7 C13 Ho1 60.9(5) . . ? O8 C13 Ho1 60.3(5) . . ? C16 C13 Ho1 177.2(6) . . ? N1 C14 C15 124.0(9) . . ? C14 C15 C16 116.8(10) . . ? C17 C16 C15 119.7(9) . . ? C17 C16 C13 119.0(9) . . ? C15 C16 C13 120.9(9) . . ? C16 C17 C18 118.3(9) . . ? N1 C18 C17 120.2(9) . . ? N1 C18 C19 117.1(8) . . ? C17 C18 C19 122.5(8) . . ? C20 C19 N2 123.1(9) . . ? C20 C19 C18 123.1(9) . . ? N2 C19 C18 113.6(8) . . ? C19 C20 C21 118.4(9) . . ? C22 C21 C20 117.3(9) . . ? C22 C21 C24 123.0(9) . . ? C20 C21 C24 119.7(9) . . ? C21 C22 C23 120.9(10) . . ? N2 C23 C22 121.7(10) . . ? O5 C24 O6 127.5(11) . . ? O5 C24 C21 114.2(10) . . ? O6 C24 C21 118.3(10) . . ? O9 C25 O10 126.8(9) . . ? O9 C25 C28 118.9(10) . . ? O10 C25 C28 114.1(8) . . ? N6 C26 C27 121.2(8) . . ? N6 C26 C32 115.6(8) . 4_557 ? C27 C26 C32 123.1(9) . 4_557 ? C28 C27 C26 117.6(9) . . ? C29 C28 C27 119.4(8) . . ? C29 C28 C25 117.6(8) . . ? C27 C28 C25 122.9(9) . . ? C28 C29 C30 120.3(8) . . ? N6 C30 C29 123.1(10) . . ? O11 C31 O12 120.9(9) . . ? O11 C31 C34 120.9(8) . . ? O12 C31 C34 118.2(7) . . ? O11 C31 Ho1 61.6(5) . . ? O12 C31 Ho1 59.4(5) . . ? C34 C31 Ho1 176.4(6) . . ? N5 C32 C33 121.5(8) . . ? N5 C32 C26 114.4(8) . 4_547 ? C33 C32 C26 124.2(8) . 4_547 ? C34 C33 C32 119.7(8) . . ? C33 C34 C35 119.1(9) . . ? C33 C34 C31 120.7(8) . . ? C35 C34 C31 120.2(8) . . ? C36 C35 C34 118.4(8) . . ? C35 C36 N5 123.9(9) . . ? C14 N1 C18 120.9(9) . . ? C14 N1 Cu1 127.7(7) . . ? C18 N1 Cu1 111.4(6) . . ? C23 N2 C19 118.6(8) . . ? C23 N2 Cu1 126.4(7) . . ? C19 N2 Cu1 114.6(6) . . ? C6 N3 C2 119.1(8) . . ? C6 N3 Cu1 111.9(5) . . ? C2 N3 Cu1 128.9(7) . . ? C7 N4 C11 119.6(8) . . ? C7 N4 Cu1 119.1(5) . . ? C11 N4 Cu1 120.7(6) . . ? C32 N5 C36 117.2(8) . . ? C32 N5 Cu2 113.4(6) . . ? C36 N5 Cu2 129.3(6) . . ? C30 N6 C26 118.3(8) . . ? C30 N6 Cu2 124.9(7) . 3 ? C26 N6 Cu2 116.6(5) . 3 ? C12 O1 Cu1 116.8(6) . 4_556 ? C1 O4 Ho1 162.2(7) . 3_545 ? C24 O5 Ho1 143.7(8) . 1_545 ? C13 O7 Ho1 92.5(6) . . ? C13 O8 Ho1 92.8(6) . . ? C25 O9 Ho1 139.6(7) . . ? C31 O11 Ho1 92.8(6) . . ? C31 O12 Ho1 93.5(5) . . ? O16' O16 Cu2 57.2(12) . . ? O16 O16' O16 167(3) . 2_557 ? O16 O16' Cu2 83.6(13) . . ? O16 O16' Cu2 83.6(13) 2_557 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.412 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.227