# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 Dear Depositor The following crystal structures have been deposited at the Cambridge Crystallographic Data Centre and allocated the deposition numbers CCDC 722460 - 722464 If we have any queries relating to these data then we will contact you later. Summary of Data CCDC 722460 --------------- Authors: Shantang Yue,Jing-Wei Dai,Zhao-Yang Li,Ying-Liang Liu, Ning Wang Journal: CrystEngComm (1350) Formula: C83 H64 Cu10 Eu4 N23 O32 Unit cell parameters: a 39.009(3) b 9.6104(6) c 30.547(2) beta 120.8650(10) space group C2/c Summary of Data CCDC 722461 --------------- Authors: Shantang Yue,Jing-Wei Dai,Zhao-Yang Li,Ying-Liang Liu, Ning Wang Journal: CrystEngComm (1350) Formula: C83 H64 Cu10 N23 O32 Tb4 Unit cell parameters: a 38.977(3) b 9.5906(6) c 30.516(2) beta 120.9940(10) space group C2/c Summary of Data CCDC 722462 --------------- Authors: Shantang Yue,Jing-Wei Dai,Zhao-Yang Li,Ying-Liang Liu, Ning Wang Journal: CrystEngComm (1350) Formula: C83 H64 Cu10 Gd4 N23 O32 Unit cell parameters: a 39.0134(19) b 9.6043(5) c 30.5304(15) beta 120.8860(10) space group C2/c Summary of Data CCDC 722463 --------------- Authors: Shantang Yue,Jing-Wei Dai,Zhao-Yang Li,Ying-Liang Liu, Ning Wang Journal: CrystEngComm (1350) Formula: C83 H64 Cu10 N23 O32 Sm4 Unit cell parameters: a 39.020(2) b 9.6088(5) c 30.5665(15) beta 120.8200(10) space group C2/c Summary of Data CCDC 722464 --------------- Authors: Shantang Yue,Jing-Wei Dai,Zhao-Yang Li,Ying-Liang Liu, Ning Wang Journal: CrystEngComm (1350) Formula: C83 H64 Cu10 N23 Nd4 O32 Unit cell parameters: a 17.6646(17) b 9.5625(9) c 30.623(3) beta 107.761(4) space group P21/c Any publication carrying these CCDC numbers will refer to the most recent set of deposited data; previous depositions carrying these numbers will not be retained. Please note, if data have not appeared in a journal publication 3 years after the date of deposition, and the CCDC cannot contact you to discuss the matter, then the CCDC will automatically include the data in the CSD as a Private Communication. Thank you for your help. Best wishes Data Acquisition Team -- Data Acquisition - the Cambridge Crystallographic Data Centre deposit@ccdc.cam.ac.uk http://www.ccdc.cam.ac.uk/deposit Telephone: (44) 01223 762910 Facsimile: (44) 01223 336033 Postal Address: CCDC, 12 Union Road, CAMBRIDGE CB2 1EZ, UK LEGAL NOTICE Unless expressly stated otherwise, information contained in this message is confidential. If this message is not intended for you, please inform deposit@ccdc.cam.ac.uk immediately. --CCDCCONTENTSEPARATOR Content-type: text/plain; charset=us-ascii; name="B905398K_ccdc_722460_722464_cif.txt" data_global _journal_name_full CrystEngComm #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_Cambridge 1350 #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author 'Shantang Yue' _publ_contact_author_name ; School of Chemistry and Environment South China Nomal University Guangzhou 510006 P. R. China ; _publ_contact_author_phone '86 20 39310178' _publ_contact_author_fax '86 20 39310178' _publ_contact_author_email yuesht@scnu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as supplmentary data for a manuscript submitted to 'CrystEngComm'. Shantang Yue ; _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; A series of novel 3D heterometallic 3d-4f heptanuclear complexes based on the linkages of Ln2(ina)6 chains and [Cu2(CN)] chains ; loop_ _publ_author_name 'Shantang Yue' 'Jing-Wei Dai' 'Zhao-Yang Li' 'Ying-Liang Liu' ; Ning Wang ; data_2 _database_code_depnum_ccdc_archive 'CCDC 722460' #==================================================================== #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C83 H64 Cu10 Eu4 N23 O32' _chemical_formula_sum 'C83 H64 Cu10 Eu4 N23 O32' _chemical_formula_weight 3138.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 ' C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 39.009(3) _cell_length_b 9.6104(6) _cell_length_c 30.547(2) _cell_angle_alpha 90.00 _cell_angle_beta 120.8650(10) _cell_angle_gamma 90.00 _cell_volume 9829.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6553 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.80 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6084.0 _exptl_absorpt_coefficient_mu 4.716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0762 _exptl_absorpt_correction_T_max 0.1641 _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 APEX-II area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24232 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8650 _reflns_number_gt 7038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'Apex2 (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-XP (Bruker, 2004)' _computing_publication_material SHELXL-97 _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. The cyanice groups are disordered with respect to the C and N termini. So the 'SIMU' and 'ISOR' were used in the restrain refinements for the partial C and N atoms. ; _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^)+(0.0302P)^2^+46.4712P] 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 8650 _refine_ls_number_parameters 685 _refine_ls_number_restraints 192 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.056 _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 C1 C 0.40064(17) 1.5317(6) 1.3699(2) 0.0342(14) Uani 1 1 d . . . C2 C 0.40989(17) 1.0316(6) 1.3786(2) 0.0331(13) Uani 1 1 d . . . C3 C 0.33331(16) 0.6194(6) 1.2422(2) 0.0328(9) Uani 1 1 d U . . H4 H 0.3457 0.5347 1.2559 0.039 Uiso 1 1 calc R . . C4 C 0.30247(16) 0.6227(6) 1.1919(2) 0.0314(8) Uani 1 1 d U . . H3 H 0.2944 0.5414 1.1727 0.038 Uiso 1 1 calc R . . C5 C 0.28357(17) 0.7474(5) 1.1703(2) 0.0297(7) Uani 1 1 d U . . C6 C 0.29719(16) 0.8643(6) 1.2006(2) 0.0335(8) Uani 1 1 d U . . H6 H 0.2856 0.9506 1.1876 0.040 Uiso 1 1 calc R . . C7 C 0.32808(17) 0.8522(6) 1.2503(2) 0.0353(9) Uani 1 1 d U . . H5 H 0.3369 0.9325 1.2701 0.042 Uiso 1 1 calc R . . C8 C 0.24898(16) 0.7540(6) 1.1162(2) 0.0276(8) Uani 1 1 d U . . C9 C 0.22505(17) 0.2366(6) 1.1418(2) 0.0336(9) Uani 1 1 d U . . C10 C 0.25020(17) 0.2023(6) 1.1975(2) 0.0350(7) Uani 1 1 d U . . C11 C 0.23829(17) 0.1035(6) 1.2195(2) 0.0375(8) Uani 1 1 d U . . H10 H 0.2141 0.0572 1.2000 0.045 Uiso 1 1 calc R . . C12 C 0.26233(17) 0.0737(7) 1.2705(2) 0.0389(9) Uani 1 1 d U . . H9 H 0.2535 0.0084 1.2850 0.047 Uiso 1 1 calc R . . C13 C 0.30922(19) 0.2250(6) 1.2786(2) 0.0406(10) Uani 1 1 d U . . H8 H 0.3340 0.2666 1.2989 0.049 Uiso 1 1 calc R . . C14 C 0.28707(18) 0.2628(6) 1.2281(2) 0.0379(8) Uani 1 1 d U . . H11 H 0.2968 0.3283 1.2147 0.045 Uiso 1 1 calc R . . C15 C 0.11290(18) 0.2259(6) 1.0295(3) 0.0402(10) Uani 1 1 d U . . C16 C 0.06813(18) 0.2401(6) 1.0044(3) 0.0441(8) Uani 1 1 d U . . C17 C 0.04394(18) 0.1261(7) 0.9912(3) 0.0469(9) Uani 1 1 d U . . H16 H 0.0550 0.0380 1.0016 0.056 Uiso 1 1 calc R . . C18 C 0.00301(18) 0.1416(7) 0.9623(3) 0.0486(11) Uani 1 1 d U . . H19 H -0.0127 0.0621 0.9538 0.058 Uiso 1 1 calc R . . C19 C 0.00823(18) 0.3734(7) 0.9634(3) 0.0526(11) Uani 1 1 d U . . H18 H -0.0038 0.4607 0.9560 0.063 Uiso 1 1 calc R . . C20 C 0.04993(18) 0.3674(7) 0.9924(3) 0.0498(9) Uani 1 1 d U . . H17 H 0.0650 0.4486 1.0033 0.060 Uiso 1 1 calc R . . C21 C 0.13743(18) 0.2473(6) 0.9433(2) 0.0344(9) Uani 1 1 d U . . C22 C 0.10073(18) 0.2721(6) 0.8918(2) 0.0372(8) Uani 1 1 d U . . C23 C 0.08042(18) 0.1625(7) 0.8596(2) 0.0401(9) Uani 1 1 d U . . H22 H 0.0898 0.0721 0.8693 0.048 Uiso 1 1 calc R . . C24 C 0.04667(18) 0.1864(7) 0.8135(2) 0.0422(10) Uani 1 1 d U . . H23 H 0.0330 0.1108 0.7928 0.051 Uiso 1 1 calc R . . C25 C 0.08656(18) 0.4047(7) 0.8744(2) 0.0410(9) Uani 1 1 d U . . H25 H 0.1000 0.4819 0.8942 0.049 Uiso 1 1 calc R . . C26 C 0.05221(18) 0.4218(7) 0.8272(2) 0.0434(10) Uani 1 1 d U . . H24 H 0.0425 0.5112 0.8161 0.052 Uiso 1 1 calc R . . C27 C 0.00941(19) 0.6857(7) 0.8861(3) 0.0544(11) Uani 1 1 d U . . H29 H -0.0089 0.6133 0.8717 0.065 Uiso 1 1 calc R . . C28 C 0.04809(18) 0.6548(7) 0.9221(2) 0.0508(10) Uani 1 1 d U . . H28 H 0.0555 0.5636 0.9332 0.061 Uiso 1 1 calc R . . C29 C 0.07614(19) 0.7614(6) 0.9420(3) 0.0446(8) Uani 1 1 d U . . C30 C 0.11927(18) 0.7275(6) 0.9785(2) 0.0393(10) Uani 1 1 d U . . C31 C 0.06373(18) 0.8882(7) 0.9224(2) 0.0479(10) Uani 1 1 d U . . H31 H 0.0819 0.9611 0.9326 0.057 Uiso 1 1 calc R . . C32 C 0.02389(18) 0.9115(7) 0.8870(2) 0.0499(11) Uani 1 1 d U . . H30 H 0.0161 1.0012 0.8743 0.060 Uiso 1 1 calc R . . C33 C -0.1560(2) 0.7830(8) 0.6111(3) 0.0557(19) Uani 1 1 d U . . C34 C -0.07144(16) 0.5336(6) 0.7743(2) 0.0288(12) Uani 1 1 d U . . C35 C -0.14259(17) 0.1813(6) 0.6770(2) 0.0339(9) Uani 1 1 d U . . H35 H -0.1268 0.1057 0.6951 0.041 Uiso 1 1 calc R . . C36 C -0.17800(16) 0.1571(6) 0.6324(2) 0.0328(8) Uani 1 1 d U . . H36 H -0.1856 0.0668 0.6202 0.039 Uiso 1 1 calc R . . C37 C -0.20234(17) 0.2688(6) 0.6056(2) 0.0316(7) Uani 1 1 d U . . C38 C -0.18840(16) 0.4008(6) 0.6230(2) 0.0346(8) Uani 1 1 d U . . H37 H -0.2033 0.4783 0.6051 0.042 Uiso 1 1 calc R . . C39 C -0.15174(16) 0.4167(6) 0.6677(2) 0.0361(9) Uani 1 1 d U . . H34 H -0.1421 0.5062 0.6787 0.043 Uiso 1 1 calc R . . C40 C -0.24406(17) 0.2442(6) 0.5617(2) 0.0308(9) Uani 1 1 d U . . C41 C -0.06276(17) 1.1574(6) 0.7881(2) 0.0326(14) Uani 1 1 d . . . C42 C -0.01716(18) 0.8120(7) 0.7387(3) 0.0581(18) Uani 0.50 1 d P . . Cu1 Cu 0.39150(2) 0.72053(8) 1.35042(3) 0.03624(19) Uani 1 1 d . . . Cu2 Cu 0.42290(2) 1.22155(8) 1.39136(3) 0.0401(2) Uani 1 1 d . . . Cu3 Cu -0.07269(3) 0.79381(10) 0.70433(4) 0.0633(3) Uani 1 1 d . . . Cu4 Cu -0.07732(2) 0.34161(7) 0.76800(3) 0.0401(2) Uani 1 1 d . . . Cu5 Cu -0.05670(2) 0.84152(7) 0.80090(3) 0.03762(19) Uani 1 1 d . . . Eu1 Eu 0.186322(7) 0.47155(3) 1.046023(9) 0.02182(8) Uani 1 1 d . . . Eu2 Eu 0.184249(7) 0.00762(3) 1.038524(9) 0.02417(8) Uani 1 1 d . . . N1 N 0.40621(15) 1.4134(6) 1.37912(19) 0.0443(13) Uani 1 1 d . . . N2 N 0.40327(15) 0.9144(6) 1.37054(19) 0.0435(13) Uani 1 1 d . . . N3 N 0.34616(14) 0.7323(5) 1.27196(17) 0.0319(11) Uani 1 1 d . . . N4 N 0.29711(16) 0.1327(6) 1.29976(18) 0.0461(14) Uani 1 1 d . . . N5 N -0.01516(15) 0.2635(5) 0.9459(2) 0.0478(15) Uani 1 1 d . . . N6 N 0.03260(15) 0.3142(6) 0.79717(18) 0.0436(13) Uani 1 1 d . . . N7 N -0.07007(17) 0.6530(7) 0.7782(2) 0.0560(16) Uani 1 1 d . . . N8 N -0.12991(14) 0.3098(5) 0.69542(18) 0.0350(12) Uani 1 1 d . . . N9 N -0.06127(15) 1.0404(7) 0.7913(2) 0.0507(15) Uani 1 1 d . . . N10 N -0.1250(2) 0.7895(8) 0.6469(3) 0.087(2) Uani 1 1 d . . . N11 N -0.00314(14) 0.8160(5) 0.8706(2) 0.0436(14) Uani 1 1 d . . . N13 N -0.01716(18) 0.8120(7) 0.7387(3) 0.0581(18) Uani 0.50 1 d P . . O1 O 0.23198(12) 0.6427(4) 1.09608(14) 0.0410(11) Uani 1 1 d . . . O2 O 0.23986(11) 0.8706(4) 1.09530(14) 0.0366(10) Uani 1 1 d . . . O3 O 0.22463(12) 0.3605(4) 1.12889(14) 0.0408(11) Uani 1 1 d . . . O4 O 0.20683(13) 0.1392(5) 1.11246(15) 0.0522(13) Uani 1 1 d . . . O5 O 0.12546(11) 0.1040(4) 1.03264(16) 0.0415(10) Uani 1 1 d . . . O6 O 0.13352(11) 0.3328(4) 1.04267(16) 0.0404(10) Uani 1 1 d . . . O7 O 0.12755(11) 0.6043(4) 0.99288(14) 0.0370(10) Uani 1 1 d . . . O8 O 0.14417(11) 0.8241(4) 0.99194(15) 0.0406(11) Uani 1 1 d . . . O9 O 0.14560(12) 0.1244(5) 0.95714(15) 0.0483(12) Uani 1 1 d . . . O10 O 0.15611(12) 0.3526(5) 0.96765(14) 0.0445(11) Uani 1 1 d . . . O11 O -0.26584(12) 0.3486(5) 0.54247(16) 0.0503(12) Uani 1 1 d . . . O12 O -0.25517(11) 0.1209(4) 0.55013(15) 0.0385(10) Uani 1 1 d . . . O1W O 0.20898(12) -0.0842(5) 0.98248(15) 0.0439(11) Uani 1 1 d . . . H1W H 0.1942 -0.1216 0.9577 0.066 Uiso 1 1 d R . . H2W H 0.2305 -0.0349 0.9873 0.066 Uiso 1 1 d R . . O2W O 0.16538(13) -0.1219(4) 1.09505(17) 0.0486(12) Uani 1 1 d . . . H4W H 0.1602 -0.2161 1.0915 0.073 Uiso 1 1 d R . . H3W H 0.1393 -0.0876 1.0792 0.073 Uiso 1 1 d R . . O3W O 0.20223(11) 0.6037(4) 0.98828(14) 0.0388(10) Uani 1 1 d . . . H6W H 0.2109 0.7068 0.9977 0.058 Uiso 1 1 d R . . H5W H 0.1907 0.6443 0.9589 0.058 Uiso 1 1 d R . . O4W O 0.16181(11) 0.5803(4) 1.09904(14) 0.0357(10) Uani 1 1 d . . . H8W H 0.1735 0.6021 1.1316 0.054 Uiso 1 1 d R . . H7W H 0.1453 0.5229 1.0977 0.054 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(3) 0.026(3) 0.031(3) 0.001(3) 0.008(3) 0.002(3) C2 0.027(3) 0.026(3) 0.038(3) -0.003(3) 0.010(3) -0.001(3) C3 0.0313(16) 0.0225(16) 0.0300(16) 0.0001(14) 0.0051(14) 0.0009(14) C4 0.0304(15) 0.0221(14) 0.0292(14) -0.0005(12) 0.0065(13) 0.0005(13) C5 0.0292(14) 0.0219(14) 0.0286(14) -0.0003(11) 0.0081(12) 0.0001(12) C6 0.0327(15) 0.0226(15) 0.0308(15) -0.0013(12) 0.0059(13) 0.0005(13) C7 0.0343(17) 0.0228(17) 0.0318(16) -0.0027(14) 0.0048(14) 0.0006(15) C8 0.0272(16) 0.0216(16) 0.0276(15) -0.0002(13) 0.0095(13) 0.0000(14) C9 0.0305(16) 0.0361(18) 0.0285(16) 0.0048(14) 0.0110(14) 0.0001(14) C10 0.0318(14) 0.0368(16) 0.0294(14) 0.0059(12) 0.0107(12) -0.0009(12) C11 0.0335(15) 0.0389(17) 0.0318(15) 0.0073(13) 0.0108(13) -0.0012(13) C12 0.0350(17) 0.0404(19) 0.0330(17) 0.0084(15) 0.0114(15) -0.0008(15) C13 0.0349(17) 0.0391(19) 0.0319(17) 0.0061(15) 0.0057(15) -0.0023(15) C14 0.0335(15) 0.0379(17) 0.0304(15) 0.0065(13) 0.0079(13) -0.0021(14) C15 0.0281(17) 0.0327(18) 0.053(2) 0.0071(16) 0.0164(16) 0.0004(15) C16 0.0299(15) 0.0337(16) 0.0569(19) 0.0076(14) 0.0138(14) -0.0002(13) C17 0.0308(16) 0.0343(17) 0.0600(19) 0.0089(15) 0.0120(15) -0.0011(14) C18 0.0312(17) 0.0345(19) 0.062(2) 0.0093(17) 0.0110(17) -0.0019(16) C19 0.0342(18) 0.0361(19) 0.063(2) 0.0075(17) 0.0075(17) 0.0011(16) C20 0.0328(16) 0.0353(17) 0.061(2) 0.0074(15) 0.0096(15) 0.0001(14) C21 0.0335(17) 0.0374(18) 0.0248(16) 0.0009(14) 0.0095(14) 0.0001(15) C22 0.0353(15) 0.0376(16) 0.0267(14) 0.0008(12) 0.0073(12) -0.0001(13) C23 0.0373(16) 0.0381(17) 0.0284(15) 0.0004(13) 0.0049(13) -0.0012(14) C24 0.0383(18) 0.0392(19) 0.0297(17) -0.0003(15) 0.0036(15) -0.0019(16) C25 0.0376(16) 0.0385(17) 0.0292(15) 0.0004(13) 0.0045(13) 0.0008(14) C26 0.0392(18) 0.0396(19) 0.0307(17) 0.0011(15) 0.0030(15) 0.0015(16) C27 0.0380(18) 0.0343(18) 0.055(2) 0.0096(16) -0.0020(16) -0.0027(16) C28 0.0361(16) 0.0318(17) 0.0523(18) 0.0099(14) -0.0005(14) -0.0025(14) C29 0.0330(15) 0.0281(15) 0.0474(17) 0.0083(13) 0.0024(13) -0.0018(13) C30 0.0303(17) 0.0260(17) 0.0435(19) 0.0069(15) 0.0060(15) -0.0007(15) C31 0.0346(16) 0.0286(16) 0.0494(18) 0.0089(14) -0.0008(14) -0.0026(14) C32 0.0358(18) 0.0290(18) 0.050(2) 0.0087(16) -0.0027(16) -0.0025(16) C33 0.055(2) 0.057(2) 0.054(2) 0.0020(10) 0.0270(13) -0.0004(10) C34 0.0291(15) 0.0259(15) 0.0293(15) 0.0000(10) 0.0133(10) -0.0008(10) C35 0.0287(16) 0.0280(17) 0.0363(17) 0.0005(15) 0.0105(14) 0.0008(15) C36 0.0282(15) 0.0277(15) 0.0358(15) 0.0001(13) 0.0117(13) 0.0003(13) C37 0.0276(14) 0.0278(14) 0.0351(14) -0.0004(12) 0.0129(12) 0.0006(12) C38 0.0293(15) 0.0278(15) 0.0372(15) -0.0003(13) 0.0103(13) 0.0005(13) C39 0.0304(17) 0.0277(17) 0.0381(17) -0.0006(15) 0.0089(15) -0.0001(15) C40 0.0271(16) 0.0283(16) 0.0341(16) -0.0008(14) 0.0137(14) 0.0008(14) C41 0.036(3) 0.014(3) 0.033(3) 0.007(2) 0.006(3) 0.004(3) C42 0.052(4) 0.073(5) 0.057(4) 0.001(4) 0.033(4) -0.001(3) Cu1 0.0353(4) 0.0302(4) 0.0317(4) 0.0007(3) 0.0089(3) 0.0003(3) Cu2 0.0303(4) 0.0298(4) 0.0503(5) -0.0034(3) 0.0136(4) -0.0012(3) Cu3 0.0411(5) 0.0608(6) 0.0665(6) -0.0038(5) 0.0123(5) 0.0042(4) Cu4 0.0388(4) 0.0234(4) 0.0438(5) 0.0005(3) 0.0108(4) -0.0007(3) Cu5 0.0305(4) 0.0229(4) 0.0428(4) 0.0024(3) 0.0069(3) 0.0014(3) Eu1 0.01824(14) 0.01727(14) 0.01868(14) 0.00040(10) 0.00138(11) -0.00046(11) Eu2 0.02021(14) 0.01735(15) 0.02166(15) 0.00153(10) 0.00118(11) -0.00127(11) N1 0.035(3) 0.050(4) 0.035(3) -0.002(3) 0.008(2) -0.001(3) N2 0.038(3) 0.051(4) 0.034(3) 0.002(3) 0.013(2) 0.000(3) N3 0.029(3) 0.028(3) 0.026(3) 0.001(2) 0.005(2) -0.001(2) N4 0.051(3) 0.051(4) 0.030(3) 0.013(2) 0.016(3) 0.010(3) N5 0.028(3) 0.032(3) 0.067(4) 0.003(3) 0.012(3) -0.003(2) N6 0.033(3) 0.051(3) 0.026(3) 0.001(2) 0.000(2) 0.001(3) N7 0.043(3) 0.063(4) 0.058(4) 0.004(3) 0.023(3) 0.000(3) N8 0.031(3) 0.026(3) 0.038(3) 0.001(2) 0.010(2) 0.000(2) N9 0.039(3) 0.054(4) 0.044(3) 0.003(3) 0.010(3) 0.001(3) N10 0.081(5) 0.093(6) 0.087(6) 0.021(4) 0.043(5) 0.001(5) N11 0.023(3) 0.033(3) 0.054(3) 0.017(3) 0.005(2) 0.007(2) N13 0.052(4) 0.073(5) 0.057(4) 0.001(4) 0.033(4) -0.001(3) O1 0.037(2) 0.029(2) 0.032(2) -0.0022(18) 0.0001(19) -0.0122(19) O2 0.027(2) 0.028(2) 0.035(2) 0.0091(18) 0.0018(18) 0.0022(18) O3 0.040(2) 0.035(3) 0.032(2) 0.0139(18) 0.0076(19) 0.000(2) O4 0.053(3) 0.041(3) 0.034(2) -0.015(2) 0.001(2) 0.000(2) O5 0.028(2) 0.035(3) 0.051(3) -0.010(2) 0.013(2) -0.0026(19) O6 0.030(2) 0.032(2) 0.049(3) 0.0078(19) 0.012(2) -0.0055(19) O7 0.025(2) 0.026(2) 0.040(2) 0.0093(18) 0.0021(18) 0.0037(17) O8 0.027(2) 0.029(2) 0.046(3) -0.0047(19) 0.0044(19) -0.0097(19) O9 0.038(2) 0.044(3) 0.040(3) 0.012(2) 0.003(2) -0.004(2) O10 0.035(2) 0.052(3) 0.026(2) -0.016(2) 0.0012(18) -0.003(2) O11 0.035(2) 0.047(3) 0.042(3) -0.009(2) 0.001(2) 0.019(2) O12 0.028(2) 0.035(2) 0.039(2) -0.0034(19) 0.0074(18) -0.0089(19) O1W 0.032(2) 0.054(3) 0.038(2) -0.010(2) 0.0126(19) -0.007(2) O2W 0.057(3) 0.033(3) 0.066(3) 0.015(2) 0.039(3) 0.007(2) O3W 0.043(2) 0.034(2) 0.037(2) 0.0124(19) 0.018(2) 0.001(2) O4W 0.037(2) 0.040(2) 0.026(2) -0.0075(18) 0.0133(18) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.165(7) . ? C1 Cu1 1.886(6) 1_565 ? C2 N2 1.154(7) . ? C2 Cu2 1.881(6) . ? C3 N3 1.338(7) . ? C3 C4 1.381(7) . ? C3 H4 0.9300 . ? C4 C5 1.384(7) . ? C4 H3 0.9300 . ? C5 C6 1.378(7) . ? C5 C8 1.506(7) . ? C6 C7 1.376(7) . ? C6 H6 0.9300 . ? C7 N3 1.335(7) . ? C7 H5 0.9300 . ? C8 O1 1.242(6) . ? C8 O2 1.248(6) . ? C9 O4 1.237(7) . ? C9 O3 1.251(7) . ? C9 C10 1.502(8) . ? C10 C11 1.375(8) . ? C10 C14 1.379(8) . ? C11 C12 1.376(8) . ? C11 H10 0.9300 . ? C12 N4 1.310(8) . ? C12 H9 0.9300 . ? C13 N4 1.319(8) . ? C13 C14 1.376(8) . ? C13 H8 0.9300 . ? C14 H11 0.9300 . ? C15 O6 1.238(7) . ? C15 O5 1.255(7) . ? C15 C16 1.511(8) . ? C16 C17 1.365(8) . ? C16 C20 1.366(8) . ? C17 C18 1.380(8) . ? C17 H16 0.9300 . ? C18 N5 1.326(8) . ? C18 H19 0.9300 . ? C19 N5 1.317(8) . ? C19 C20 1.398(8) . ? C19 H18 0.9300 . ? C20 H17 0.9300 . ? C21 O9 1.240(7) . ? C21 O10 1.246(7) . ? C21 C22 1.506(8) . ? C22 C23 1.380(8) . ? C22 C25 1.383(8) . ? C23 C24 1.366(8) . ? C23 H22 0.9300 . ? C24 N6 1.333(8) . ? C24 H23 0.9300 . ? C25 C26 1.385(8) . ? C25 H25 0.9300 . ? C26 N6 1.332(8) . ? C26 H24 0.9300 . ? C27 N11 1.339(8) . ? C27 C28 1.369(8) . ? C27 H29 0.9300 . ? C28 C29 1.391(8) . ? C28 H28 0.9300 . ? C29 C31 1.333(8) . ? C29 C30 1.502(8) . ? C30 O7 1.247(7) . ? C30 O8 1.251(7) . ? C31 C32 1.382(8) . ? C31 H31 0.9300 . ? C32 N11 1.290(8) . ? C32 H30 0.9300 . ? C33 N10 1.143(10) . ? C34 N7 1.152(8) . ? C34 Cu4 1.857(6) . ? C35 N8 1.342(7) . ? C35 C36 1.374(7) . ? C35 H35 0.9300 . ? C36 C37 1.388(8) . ? C36 H36 0.9300 . ? C37 C38 1.375(8) . ? C37 C40 1.505(8) . ? C38 C39 1.389(7) . ? C38 H37 0.9300 . ? C39 N8 1.325(7) . ? C39 H34 0.9300 . ? C40 O12 1.249(6) . ? C40 O11 1.249(7) . ? C40 Eu1 3.251(6) 8_455 ? C41 N9 1.127(7) . ? C41 Cu4 1.865(6) 1_565 ? C42 N13 1.149(12) 2_556 ? C42 C42 1.149(12) 2_556 ? C42 Cu3 1.868(6) . ? Cu1 C1 1.886(6) 1_545 ? Cu1 N2 1.942(6) . ? Cu1 N3 2.130(4) . ? Cu2 N1 1.927(6) . ? Cu2 N5 2.122(5) 8_566 ? Cu3 N10 1.889(8) . ? Cu3 Cu5 2.7227(13) . ? Cu4 C41 1.865(6) 1_545 ? Cu4 N8 2.133(5) . ? Cu5 N7 1.915(7) . ? Cu5 N9 1.928(6) . ? Cu5 N11 2.096(5) . ? Eu1 O1 2.329(4) . ? Eu1 O10 2.352(4) . ? Eu1 O7 2.388(3) . ? Eu1 O12 2.392(4) 8_556 ? Eu1 O6 2.411(4) . ? Eu1 O3 2.429(4) . ? Eu1 O4W 2.494(4) . ? Eu1 O3W 2.496(4) . ? Eu1 C40 3.251(6) 8_556 ? Eu1 Eu2 4.4630(5) . ? Eu1 H7W 2.8092 . ? Eu2 O8 2.301(4) 1_545 ? Eu2 O4 2.331(4) . ? Eu2 O11 2.340(4) 8_556 ? Eu2 O2 2.363(4) 1_545 ? Eu2 O5 2.393(4) . ? Eu2 O9 2.422(4) . ? Eu2 O1W 2.517(4) . ? Eu2 O2W 2.525(4) . ? Eu2 H3W 2.7720 . ? N5 Cu2 2.122(5) 8_465 ? O2 Eu2 2.363(4) 1_565 ? O8 Eu2 2.301(4) 1_565 ? O11 Eu2 2.340(4) 8_455 ? O12 Eu1 2.392(4) 8_455 ? O1W H1W 0.7654 . ? O1W H2W 0.9083 . ? O2W H4W 0.9219 . ? O2W H3W 0.9335 . ? O3W H6W 1.0396 . ? O3W H5W 0.8644 . ? O4W H8W 0.8808 . ? O4W H7W 0.8334 . ? 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 N1 C1 Cu1 175.8(6) . 1_565 ? N2 C2 Cu2 177.1(6) . . ? N3 C3 C4 123.1(5) . . ? N3 C3 H4 118.5 . . ? C4 C3 H4 118.5 . . ? C3 C4 C5 119.9(5) . . ? C3 C4 H3 120.1 . . ? C5 C4 H3 120.1 . . ? C6 C5 C4 117.2(5) . . ? C6 C5 C8 121.5(5) . . ? C4 C5 C8 121.3(5) . . ? C7 C6 C5 119.3(5) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? N3 C7 C6 124.1(5) . . ? N3 C7 H5 117.9 . . ? C6 C7 H5 117.9 . . ? O1 C8 O2 125.5(5) . . ? O1 C8 C5 117.2(5) . . ? O2 C8 C5 117.3(5) . . ? O4 C9 O3 125.6(6) . . ? O4 C9 C10 116.9(5) . . ? O3 C9 C10 117.5(5) . . ? C11 C10 C14 117.2(5) . . ? C11 C10 C9 121.2(5) . . ? C14 C10 C9 121.5(5) . . ? C10 C11 C12 119.6(6) . . ? C10 C11 H10 120.2 . . ? C12 C11 H10 120.2 . . ? N4 C12 C11 123.2(6) . . ? N4 C12 H9 118.4 . . ? C11 C12 H9 118.4 . . ? N4 C13 C14 123.4(6) . . ? N4 C13 H8 118.3 . . ? C14 C13 H8 118.3 . . ? C13 C14 C10 119.0(6) . . ? C13 C14 H11 120.5 . . ? C10 C14 H11 120.5 . . ? O6 C15 O5 126.0(6) . . ? O6 C15 C16 118.6(6) . . ? O5 C15 C16 115.3(5) . . ? C17 C16 C20 117.0(6) . . ? C17 C16 C15 121.4(6) . . ? C20 C16 C15 121.5(6) . . ? C16 C17 C18 120.0(6) . . ? C16 C17 H16 120.0 . . ? C18 C17 H16 120.0 . . ? N5 C18 C17 123.7(6) . . ? N5 C18 H19 118.1 . . ? C17 C18 H19 118.1 . . ? N5 C19 C20 124.2(6) . . ? N5 C19 H18 117.9 . . ? C20 C19 H18 117.9 . . ? C16 C20 C19 118.9(6) . . ? C16 C20 H17 120.6 . . ? C19 C20 H17 120.6 . . ? O9 C21 O10 127.0(6) . . ? O9 C21 C22 116.5(5) . . ? O10 C21 C22 116.5(5) . . ? C23 C22 C25 117.3(5) . . ? C23 C22 C21 121.0(5) . . ? C25 C22 C21 121.7(5) . . ? C24 C23 C22 120.3(6) . . ? C24 C23 H22 119.9 . . ? C22 C23 H22 119.9 . . ? N6 C24 C23 122.3(6) . . ? N6 C24 H23 118.9 . . ? C23 C24 H23 118.9 . . ? C22 C25 C26 119.5(6) . . ? C22 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? N6 C26 C25 122.1(6) . . ? N6 C26 H24 119.0 . . ? C25 C26 H24 119.0 . . ? N11 C27 C28 122.7(6) . . ? N11 C27 H29 118.7 . . ? C28 C27 H29 118.7 . . ? C27 C28 C29 119.1(6) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C31 C29 C28 117.0(6) . . ? C31 C29 C30 122.8(6) . . ? C28 C29 C30 119.6(5) . . ? O7 C30 O8 124.9(5) . . ? O7 C30 C29 117.2(5) . . ? O8 C30 C29 117.9(5) . . ? C29 C31 C32 120.2(6) . . ? C29 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? N11 C32 C31 123.7(6) . . ? N11 C32 H30 118.1 . . ? C31 C32 H30 118.1 . . ? N7 C34 Cu4 175.6(6) . . ? N8 C35 C36 122.6(5) . . ? N8 C35 H35 118.7 . . ? C36 C35 H35 118.7 . . ? C35 C36 C37 119.2(5) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C38 C37 C36 118.1(5) . . ? C38 C37 C40 121.5(5) . . ? C36 C37 C40 120.2(5) . . ? C37 C38 C39 119.0(5) . . ? C37 C38 H37 120.5 . . ? C39 C38 H37 120.5 . . ? N8 C39 C38 122.9(6) . . ? N8 C39 H34 118.6 . . ? C38 C39 H34 118.6 . . ? O12 C40 O11 125.1(5) . . ? O12 C40 C37 117.5(5) . . ? O11 C40 C37 117.2(5) . . ? O12 C40 Eu1 37.9(3) . 8_455 ? O11 C40 Eu1 97.3(4) . 8_455 ? C37 C40 Eu1 132.2(4) . 8_455 ? N9 C41 Cu4 165.7(5) . 1_565 ? N13 C42 C42 0.0(12) 2_556 2_556 ? N13 C42 Cu3 174.2(4) 2_556 . ? C42 C42 Cu3 174.2(4) 2_556 . ? C1 Cu1 N2 148.0(2) 1_545 . ? C1 Cu1 N3 108.6(2) 1_545 . ? N2 Cu1 N3 103.30(19) . . ? C2 Cu2 N1 149.3(2) . . ? C2 Cu2 N5 107.8(2) . 8_566 ? N1 Cu2 N5 102.9(2) . 8_566 ? C42 Cu3 N10 155.8(3) . . ? C42 Cu3 Cu5 79.7(2) . . ? N10 Cu3 Cu5 123.2(3) . . ? C34 Cu4 C41 155.3(2) . 1_545 ? C34 Cu4 N8 104.6(2) . . ? C41 Cu4 N8 100.0(2) 1_545 . ? N7 Cu5 N9 153.7(2) . . ? N7 Cu5 N11 101.6(2) . . ? N9 Cu5 N11 103.7(2) . . ? N7 Cu5 Cu3 65.14(18) . . ? N9 Cu5 Cu3 92.93(17) . . ? N11 Cu5 Cu3 129.47(16) . . ? O1 Eu1 O10 145.77(16) . . ? O1 Eu1 O7 102.30(14) . . ? O10 Eu1 O7 76.27(14) . . ? O1 Eu1 O12 80.81(15) . 8_556 ? O10 Eu1 O12 80.75(14) . 8_556 ? O7 Eu1 O12 142.35(14) . 8_556 ? O1 Eu1 O6 140.13(15) . . ? O10 Eu1 O6 73.56(15) . . ? O7 Eu1 O6 76.43(13) . . ? O12 Eu1 O6 124.62(14) 8_556 . ? O1 Eu1 O3 76.81(14) . . ? O10 Eu1 O3 124.50(15) . . ? O7 Eu1 O3 143.73(15) . . ? O12 Eu1 O3 73.84(14) 8_556 . ? O6 Eu1 O3 81.76(14) . . ? O1 Eu1 O4W 72.32(14) . . ? O10 Eu1 O4W 134.90(14) . . ? O7 Eu1 O4W 70.32(13) . . ? O12 Eu1 O4W 142.67(13) 8_556 . ? O6 Eu1 O4W 69.86(14) . . ? O3 Eu1 O4W 75.13(14) . . ? O1 Eu1 O3W 73.80(14) . . ? O10 Eu1 O3W 72.80(15) . . ? O7 Eu1 O3W 75.39(13) . . ? O12 Eu1 O3W 69.49(13) 8_556 . ? O6 Eu1 O3W 140.16(13) . . ? O3 Eu1 O3W 135.80(13) . . ? O4W Eu1 O3W 124.25(14) . . ? O1 Eu1 C40 93.10(15) . 8_556 ? O10 Eu1 C40 77.57(14) . 8_556 ? O7 Eu1 C40 151.56(14) . 8_556 ? O12 Eu1 C40 18.72(14) 8_556 8_556 ? O6 Eu1 C40 106.51(14) . 8_556 ? O3 Eu1 C40 62.93(15) . 8_556 ? O4W Eu1 C40 137.82(13) . 8_556 ? O3W Eu1 C40 86.40(14) . 8_556 ? O1 Eu1 Eu2 136.64(10) . . ? O10 Eu1 Eu2 58.39(11) . . ? O7 Eu1 Eu2 120.88(9) . . ? O12 Eu1 Eu2 67.86(10) 8_556 . ? O6 Eu1 Eu2 56.83(10) . . ? O3 Eu1 Eu2 66.40(10) . . ? O4W Eu1 Eu2 116.69(9) . . ? O3W Eu1 Eu2 118.45(10) . . ? C40 Eu1 Eu2 50.36(10) 8_556 . ? O1 Eu1 H7W 88.4 . . ? O10 Eu1 H7W 121.7 . . ? O7 Eu1 H7W 70.3 . . ? O12 Eu1 H7W 147.1 8_556 . ? O6 Eu1 H7W 53.2 . . ? O3 Eu1 H7W 73.4 . . ? O4W Eu1 H7W 16.8 . . ? O3W Eu1 H7W 136.7 . . ? C40 Eu1 H7W 134.7 8_556 . ? Eu2 Eu1 H7W 101.8 . . ? O8 Eu2 O4 144.46(17) 1_545 . ? O8 Eu2 O11 140.16(16) 1_545 8_556 ? O4 Eu2 O11 74.87(17) . 8_556 ? O8 Eu2 O2 95.94(14) 1_545 1_545 ? O4 Eu2 O2 80.96(15) . 1_545 ? O11 Eu2 O2 82.24(14) 8_556 1_545 ? O8 Eu2 O5 85.94(14) 1_545 . ? O4 Eu2 O5 74.58(15) . . ? O11 Eu2 O5 121.02(16) 8_556 . ? O2 Eu2 O5 138.95(15) 1_545 . ? O8 Eu2 O9 81.54(14) 1_545 . ? O4 Eu2 O9 118.03(16) . . ? O11 Eu2 O9 80.94(14) 8_556 . ? O2 Eu2 O9 149.87(15) 1_545 . ? O5 Eu2 O9 71.07(15) . . ? O8 Eu2 O1W 71.73(15) 1_545 . ? O4 Eu2 O1W 139.74(15) . . ? O11 Eu2 O1W 69.09(16) 8_556 . ? O2 Eu2 O1W 77.05(14) 1_545 . ? O5 Eu2 O1W 140.50(13) . . ? O9 Eu2 O1W 73.65(15) . . ? O8 Eu2 O2W 72.62(15) 1_545 . ? O4 Eu2 O2W 72.69(16) . . ? O11 Eu2 O2W 141.51(15) 8_556 . ? O2 Eu2 O2W 72.75(14) 1_545 . ? O5 Eu2 O2W 68.76(15) . . ? O9 Eu2 O2W 133.15(15) . . ? O1W Eu2 O2W 129.80(15) . . ? O8 Eu2 Eu1 141.80(10) 1_545 . ? O4 Eu2 Eu1 54.60(11) . . ? O11 Eu2 Eu1 54.17(12) 8_556 . ? O2 Eu2 Eu1 122.22(9) 1_545 . ? O5 Eu2 Eu1 66.96(10) . . ? O9 Eu2 Eu1 64.85(11) . . ? O1W Eu2 Eu1 112.47(10) . . ? O2W Eu2 Eu1 117.47(10) . . ? O8 Eu2 H3W 68.8 1_545 . ? O4 Eu2 H3W 75.9 . . ? O11 Eu2 H3W 150.8 8_556 . ? O2 Eu2 H3W 92.3 1_545 . ? O5 Eu2 H3W 50.2 . . ? O9 Eu2 H3W 114.1 . . ? O1W Eu2 H3W 137.7 . . ? O2W Eu2 H3W 19.6 . . ? Eu1 Eu2 H3W 107.8 . . ? C1 N1 Cu2 169.6(5) . . ? C2 N2 Cu1 174.4(5) . . ? C7 N3 C3 116.4(5) . . ? C7 N3 Cu1 121.7(4) . . ? C3 N3 Cu1 121.8(4) . . ? C12 N4 C13 117.6(5) . . ? C19 N5 C18 115.5(5) . . ? C19 N5 Cu2 122.5(4) . 8_465 ? C18 N5 Cu2 121.9(4) . 8_465 ? C26 N6 C24 118.5(5) . . ? C34 N7 Cu5 165.8(6) . . ? C39 N8 C35 117.9(5) . . ? C39 N8 Cu4 120.9(4) . . ? C35 N8 Cu4 121.3(4) . . ? C41 N9 Cu5 176.8(6) . . ? C33 N10 Cu3 176.9(8) . . ? C32 N11 C27 116.8(5) . . ? C32 N11 Cu5 120.1(4) . . ? C27 N11 Cu5 117.5(4) . . ? C8 O1 Eu1 165.3(4) . . ? C8 O2 Eu2 142.1(4) . 1_565 ? C9 O3 Eu1 130.4(4) . . ? C9 O4 Eu2 154.5(5) . . ? C15 O5 Eu2 133.5(4) . . ? C15 O6 Eu1 150.6(4) . . ? C30 O7 Eu1 137.1(4) . . ? C30 O8 Eu2 159.9(4) . 1_565 ? C21 O9 Eu2 135.0(4) . . ? C21 O10 Eu1 146.8(4) . . ? C40 O11 Eu2 147.7(4) . 8_455 ? C40 O12 Eu1 123.4(4) . 8_455 ? Eu2 O1W H1W 118.7 . . ? Eu2 O1W H2W 110.6 . . ? H1W O1W H2W 124.7 . . ? Eu2 O2W H4W 121.7 . . ? Eu2 O2W H3W 95.3 . . ? H4W O2W H3W 99.9 . . ? Eu1 O3W H6W 117.0 . . ? Eu1 O3W H5W 141.2 . . ? H6W O3W H5W 77.2 . . ? Eu1 O4W H8W 133.2 . . ? Eu1 O4W H7W 103.6 . . ? H8W O4W H7W 98.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W O8 0.77 2.70 2.828(6) 92.0 1_545 O1W H1W O3W 0.77 2.76 3.024(6) 102.5 1_545 O1W H2W O12 0.91 2.37 3.157(6) 145.4 2_556 O1W H2W O3W 0.91 2.42 3.107(6) 132.3 7_557 O2W H4W O4W 0.92 1.97 2.871(6) 166.2 1_545 O2W H3W O5 0.93 2.22 2.780(6) 117.9 . O2W H3W N1 0.93 2.66 3.286(7) 124.6 4_537 O3W H6W O1W 1.04 2.05 3.024(6) 154.3 1_565 O4W H8W N4 0.88 1.83 2.701(6) 172.7 4_557 O4W H7W O6 0.83 2.36 2.809(6) 114.2 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.248 _refine_diff_density_min -1.102 _refine_diff_density_rms 0.121 data_3 _database_code_depnum_ccdc_archive 'CCDC 722461' #==================================================================== #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C83 H64 Cu10 N23 O32 Tb4' _chemical_formula_sum 'C83 H64 Cu10 N23 O32 Tb4' _chemical_formula_weight 3166.80 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 'C 2/c ' _symmetry_space_group_name_Hall '-C 2yc' 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 38.977(3) _cell_length_b 9.5906(6) _cell_length_c 30.516(2) _cell_angle_alpha 90.00 _cell_angle_beta 120.9940(10) _cell_angle_gamma 90.00 _cell_volume 9778.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6102 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.67 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6116.0 _exptl_absorpt_coefficient_mu 5.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0675 _exptl_absorpt_correction_T_max 0.1464 _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 APEX-II area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19185 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8533 _reflns_number_gt 6969 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'Apex2 (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-XP (Bruker, 2004)' _computing_publication_material SHELXL-97 _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. The cyanice groups are disordered with respect to the C and N termini. So the 'SIMU' and 'ISOR' were used in the restrain refinements for the partial C and N atoms. ; _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^)+(0.0302P)^2^+46.4712P] 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 8533 _refine_ls_number_parameters 685 _refine_ls_number_restraints 192 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.084 _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 C1 C 0.40025(17) 1.5336(7) 1.3701(2) 0.0322(14) Uani 1 1 d . . . C2 C 0.40972(17) 1.0338(7) 1.3790(2) 0.0325(14) Uani 1 1 d . . . C3 C 0.33339(16) 0.6205(6) 1.2416(2) 0.0320(9) Uani 1 1 d U . . H4 H 0.3463 0.5363 1.2554 0.038 Uiso 1 1 calc R . . C4 C 0.30209(16) 0.6226(6) 1.1912(2) 0.0308(8) Uani 1 1 d U . . H3 H 0.2939 0.5409 1.1721 0.037 Uiso 1 1 calc R . . C5 C 0.28322(17) 0.7479(6) 1.1697(2) 0.0287(7) Uani 1 1 d U . . C6 C 0.29673(17) 0.8649(6) 1.2000(2) 0.0326(8) Uani 1 1 d U . . H6 H 0.2850 0.9512 1.1869 0.039 Uiso 1 1 calc R . . C7 C 0.32791(17) 0.8532(6) 1.2501(2) 0.0347(10) Uani 1 1 d U . . H5 H 0.3368 0.9335 1.2699 0.042 Uiso 1 1 calc R . . C8 C 0.24844(16) 0.7535(6) 1.1151(2) 0.0265(8) Uani 1 1 d U . . C9 C 0.22490(17) 0.2367(6) 1.1408(2) 0.0327(9) Uani 1 1 d U . . C10 C 0.24993(17) 0.2018(7) 1.1972(2) 0.0346(8) Uani 1 1 d U . . C11 C 0.23801(18) 0.1046(7) 1.2187(2) 0.0371(8) Uani 1 1 d U . . H10 H 0.2139 0.0579 1.1989 0.044 Uiso 1 1 calc R . . C12 C 0.26184(18) 0.0751(7) 1.2701(2) 0.0387(10) Uani 1 1 d U . . H9 H 0.2527 0.0105 1.2845 0.046 Uiso 1 1 calc R . . C13 C 0.30905(19) 0.2266(7) 1.2785(2) 0.0398(10) Uani 1 1 d U . . H8 H 0.3338 0.2689 1.2988 0.048 Uiso 1 1 calc R . . C14 C 0.28654(18) 0.2628(6) 1.2276(2) 0.0375(8) Uani 1 1 d U . . H11 H 0.2961 0.3281 1.2140 0.045 Uiso 1 1 calc R . . C15 C 0.11373(18) 0.2255(7) 1.0297(3) 0.0393(10) Uani 1 1 d U . . C16 C 0.06886(18) 0.2396(7) 1.0045(3) 0.0432(8) Uani 1 1 d U . . C17 C 0.04480(18) 0.1259(7) 0.9919(3) 0.0461(9) Uani 1 1 d U . . H16 H 0.0560 0.0378 1.0029 0.055 Uiso 1 1 calc R . . C18 C 0.00378(18) 0.1412(7) 0.9627(3) 0.0474(11) Uani 1 1 d U . . H19 H -0.0118 0.0610 0.9544 0.057 Uiso 1 1 calc R . . C19 C 0.00862(19) 0.3722(8) 0.9632(3) 0.0527(11) Uani 1 1 d U . . H18 H -0.0034 0.4597 0.9553 0.063 Uiso 1 1 calc R . . C20 C 0.05033(19) 0.3664(7) 0.9927(3) 0.0494(10) Uani 1 1 d U . . H17 H 0.0653 0.4480 1.0041 0.059 Uiso 1 1 calc R . . C21 C 0.13804(18) 0.2470(6) 0.9440(2) 0.0326(9) Uani 1 1 d U . . C22 C 0.10117(18) 0.2710(6) 0.8917(2) 0.0358(8) Uani 1 1 d U . . C23 C 0.08068(17) 0.1612(7) 0.8599(2) 0.0389(9) Uani 1 1 d U . . H22 H 0.0897 0.0705 0.8701 0.047 Uiso 1 1 calc R . . C24 C 0.04721(18) 0.1846(7) 0.8135(2) 0.0411(10) Uani 1 1 d U . . H23 H 0.0338 0.1091 0.7925 0.049 Uiso 1 1 calc R . . C25 C 0.08687(18) 0.4039(7) 0.8747(2) 0.0392(9) Uani 1 1 d U . . H25 H 0.1002 0.4810 0.8948 0.047 Uiso 1 1 calc R . . C26 C 0.05226(18) 0.4210(7) 0.8271(2) 0.0420(10) Uani 1 1 d U . . H24 H 0.0424 0.5104 0.8159 0.050 Uiso 1 1 calc R . . C27 C 0.00926(19) 0.6844(7) 0.8871(3) 0.0542(12) Uani 1 1 d U . . H29 H -0.0093 0.6122 0.8738 0.065 Uiso 1 1 calc R . . C28 C 0.04876(18) 0.6541(7) 0.9230(3) 0.0508(10) Uani 1 1 d U . . H28 H 0.0565 0.5628 0.9338 0.061 Uiso 1 1 calc R . . C29 C 0.07658(18) 0.7611(7) 0.9425(3) 0.0450(9) Uani 1 1 d U . . C30 C 0.11983(18) 0.7286(7) 0.9792(3) 0.0402(10) Uani 1 1 d U . . C31 C 0.06385(18) 0.8888(7) 0.9227(2) 0.0487(10) Uani 1 1 d U . . H31 H 0.0818 0.9627 0.9330 0.058 Uiso 1 1 calc R . . C32 C 0.02447(18) 0.9093(7) 0.8875(3) 0.0508(12) Uani 1 1 d U . . H30 H 0.0167 0.9985 0.8740 0.061 Uiso 1 1 calc R . . C33 C -0.1566(2) 0.7836(8) 0.6111(3) 0.056(2) Uani 1 1 d U . . C34 C -0.07150(17) 0.5320(7) 0.7748(2) 0.0317(14) Uani 1 1 d U . . C35 C -0.14296(17) 0.1814(6) 0.6768(2) 0.0336(9) Uani 1 1 d U . . H35 H -0.1273 0.1052 0.6949 0.040 Uiso 1 1 calc R . . C36 C -0.17854(16) 0.1566(6) 0.6320(2) 0.0326(8) Uani 1 1 d U . . H36 H -0.1863 0.0662 0.6199 0.039 Uiso 1 1 calc R . . C37 C -0.20263(17) 0.2694(6) 0.6053(2) 0.0316(7) Uani 1 1 d U . . C38 C -0.18822(16) 0.4022(6) 0.6232(2) 0.0341(8) Uani 1 1 d U . . H37 H -0.2028 0.4805 0.6054 0.041 Uiso 1 1 calc R . . C39 C -0.15173(16) 0.4160(7) 0.6680(2) 0.0356(10) Uani 1 1 d U . . H34 H -0.1421 0.5055 0.6794 0.043 Uiso 1 1 calc R . . C40 C -0.24466(17) 0.2465(6) 0.5617(2) 0.0304(9) Uani 1 1 d U . . C41 C -0.06303(18) 1.1558(6) 0.7880(2) 0.0329(15) Uani 1 1 d . . . C42 C -0.01702(17) 0.8102(7) 0.7389(3) 0.0541(18) Uani 0.50 1 d P . . Cu1 Cu 0.39116(2) 0.72326(8) 1.35020(3) 0.0368(2) Uani 1 1 d . . . Cu2 Cu 0.42302(2) 1.22431(8) 1.39201(3) 0.0411(2) Uani 1 1 d . . . Cu3 Cu -0.07286(3) 0.79210(11) 0.70472(4) 0.0641(3) Uani 1 1 d . . . Cu4 Cu -0.07724(2) 0.33956(8) 0.76813(3) 0.0423(2) Uani 1 1 d . . . Cu5 Cu -0.05667(2) 0.83926(8) 0.80132(3) 0.0390(2) Uani 1 1 d . . . Tb1 Tb 0.186238(7) 0.47171(3) 1.046261(9) 0.02145(8) Uani 1 1 d . . . Tb2 Tb 0.184506(7) 0.00739(3) 1.038351(9) 0.02387(8) Uani 1 1 d . . . N1 N 0.40613(15) 1.4164(7) 1.3795(2) 0.0461(14) Uani 1 1 d . . . N2 N 0.40306(16) 0.9163(7) 1.3706(2) 0.0469(15) Uani 1 1 d . . . N3 N 0.34579(14) 0.7336(5) 1.27122(18) 0.0318(12) Uani 1 1 d . . . N4 N 0.29682(16) 0.1338(6) 1.29975(19) 0.0441(14) Uani 1 1 d . . . N5 N -0.01488(15) 0.2615(6) 0.9459(2) 0.0504(16) Uani 1 1 d . . . N6 N 0.03306(15) 0.3130(6) 0.79748(19) 0.0429(14) Uani 1 1 d . . . N7 N -0.06984(17) 0.6504(7) 0.7786(2) 0.0595(17) Uani 1 1 d . . . N8 N -0.12961(14) 0.3085(5) 0.69559(19) 0.0363(13) Uani 1 1 d . . . N9 N -0.06126(16) 1.0384(7) 0.7917(2) 0.0542(17) Uani 1 1 d . . . N10 N -0.1254(2) 0.7876(9) 0.6468(3) 0.089(2) Uani 1 1 d . . . N11 N -0.00295(15) 0.8148(6) 0.8713(2) 0.0469(15) Uani 1 1 d . . . N13 N -0.01702(17) 0.8102(7) 0.7389(3) 0.0541(18) Uani 0.50 1 d P . . O1 O 0.23140(12) 0.6416(4) 1.09554(14) 0.0387(11) Uani 1 1 d . . . O2 O 0.23918(11) 0.8697(4) 1.09433(14) 0.0349(10) Uani 1 1 d . . . O3 O 0.22356(12) 0.3606(4) 1.12820(15) 0.0390(11) Uani 1 1 d . . . O4 O 0.20757(14) 0.1384(5) 1.11156(16) 0.0509(13) Uani 1 1 d . . . O5 O 0.12628(11) 0.1040(4) 1.03267(16) 0.0400(11) Uani 1 1 d . . . O6 O 0.13414(11) 0.3339(4) 1.04289(15) 0.0367(10) Uani 1 1 d . . . O7 O 0.12828(11) 0.6049(4) 0.99360(15) 0.0356(10) Uani 1 1 d . . . O8 O 0.14453(11) 0.8245(4) 0.99232(16) 0.0386(11) Uani 1 1 d . . . O9 O 0.14629(12) 0.1243(5) 0.95799(15) 0.0434(12) Uani 1 1 d . . . O10 O 0.15635(11) 0.3531(5) 0.96848(15) 0.0409(11) Uani 1 1 d . . . O11 O -0.26554(12) 0.3526(5) 0.54201(16) 0.0473(12) Uani 1 1 d . . . O12 O -0.25620(11) 0.1237(4) 0.55042(15) 0.0383(11) Uani 1 1 d . . . O1W O 0.20862(11) -0.0877(5) 0.98313(15) 0.0413(11) Uani 1 1 d . . . H1W H 0.1939 -0.1250 0.9584 0.062 Uiso 1 1 d R . . H2W H 0.2302 -0.0383 0.9880 0.062 Uiso 1 1 d R . . O2W O 0.16619(14) -0.1205(5) 1.09529(17) 0.0488(12) Uani 1 1 d . . . H4W H 0.1610 -0.2147 1.0917 0.073 Uiso 1 1 d R . . H3W H 0.1401 -0.0862 1.0794 0.073 Uiso 1 1 d R . . O3W O 0.20251(12) 0.6021(4) 0.98908(15) 0.0390(10) Uani 1 1 d . . . H6W H 0.2112 0.7053 0.9985 0.059 Uiso 1 1 d R . . H5W H 0.1910 0.6428 0.9597 0.059 Uiso 1 1 d R . . O4W O 0.16199(11) 0.5806(4) 1.09867(14) 0.0355(10) Uani 1 1 d . . . H8W H 0.1737 0.6023 1.1312 0.053 Uiso 1 1 d R . . H7W H 0.1455 0.5231 1.0973 0.053 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(3) 0.028(4) 0.030(3) 0.004(3) 0.008(3) 0.002(3) C2 0.025(3) 0.027(4) 0.036(3) -0.007(3) 0.009(3) -0.003(3) C3 0.0317(17) 0.0230(17) 0.0300(17) 0.0001(15) 0.0077(14) 0.0015(15) C4 0.0307(15) 0.0224(15) 0.0292(15) -0.0009(13) 0.0083(13) 0.0010(13) C5 0.0292(14) 0.0217(14) 0.0281(14) -0.0009(12) 0.0097(12) 0.0003(12) C6 0.0327(15) 0.0220(15) 0.0300(15) -0.0014(13) 0.0067(13) 0.0010(13) C7 0.0344(17) 0.0225(17) 0.0309(17) -0.0018(15) 0.0052(14) 0.0007(15) C8 0.0270(16) 0.0214(16) 0.0272(16) -0.0008(14) 0.0113(14) -0.0001(14) C9 0.0313(16) 0.0356(18) 0.0258(16) 0.0050(15) 0.0109(14) -0.0013(15) C10 0.0327(14) 0.0365(16) 0.0273(15) 0.0062(13) 0.0102(12) -0.0021(13) C11 0.0341(15) 0.0382(17) 0.0302(15) 0.0075(14) 0.0102(13) -0.0026(14) C12 0.0355(17) 0.0397(19) 0.0319(17) 0.0083(16) 0.0108(15) -0.0024(15) C13 0.0356(17) 0.0387(19) 0.0296(17) 0.0063(16) 0.0056(15) -0.0034(16) C14 0.0344(15) 0.0377(17) 0.0285(15) 0.0068(14) 0.0077(13) -0.0034(14) C15 0.0287(17) 0.0345(19) 0.051(2) 0.0068(17) 0.0175(16) -0.0023(15) C16 0.0303(15) 0.0356(17) 0.0541(18) 0.0068(15) 0.0149(14) -0.0023(13) C17 0.0313(16) 0.0364(18) 0.0568(19) 0.0079(16) 0.0128(15) -0.0031(14) C18 0.0317(17) 0.037(2) 0.058(2) 0.0087(18) 0.0120(17) -0.0039(16) C19 0.0354(18) 0.039(2) 0.061(2) 0.0057(18) 0.0087(17) -0.0006(17) C20 0.0337(16) 0.0374(18) 0.059(2) 0.0057(16) 0.0108(15) -0.0013(15) C21 0.0323(17) 0.0348(18) 0.0232(16) 0.0004(15) 0.0088(14) -0.0006(15) C22 0.0345(15) 0.0354(16) 0.0250(14) 0.0005(13) 0.0064(12) -0.0006(13) C23 0.0366(16) 0.0364(17) 0.0264(15) 0.0005(14) 0.0039(13) -0.0012(14) C24 0.0377(18) 0.0377(19) 0.0274(17) -0.0002(16) 0.0021(15) -0.0018(16) C25 0.0366(16) 0.0358(17) 0.0277(16) 0.0001(14) 0.0042(14) 0.0005(14) C26 0.0381(18) 0.0366(19) 0.0299(17) 0.0002(16) 0.0023(15) 0.0017(16) C27 0.0352(18) 0.0380(19) 0.054(2) 0.0132(17) -0.0025(17) -0.0058(16) C28 0.0335(16) 0.0359(18) 0.0511(19) 0.0124(16) -0.0009(15) -0.0050(14) C29 0.0305(15) 0.0330(17) 0.0466(18) 0.0104(14) 0.0022(14) -0.0041(13) C30 0.0279(17) 0.0310(19) 0.0432(19) 0.0088(16) 0.0051(15) -0.0036(15) C31 0.0331(16) 0.0337(18) 0.0486(19) 0.0108(15) -0.0009(15) -0.0042(15) C32 0.0346(18) 0.0342(19) 0.050(2) 0.0108(17) -0.0024(16) -0.0034(16) C33 0.055(2) 0.057(2) 0.055(2) 0.0020(10) 0.0273(13) -0.0003(10) C34 0.0319(16) 0.0287(16) 0.0319(16) 0.0002(10) 0.0146(11) -0.0006(10) C35 0.0285(16) 0.0272(17) 0.0363(17) -0.0004(15) 0.0103(15) 0.0010(15) C36 0.0277(15) 0.0274(16) 0.0360(16) -0.0007(14) 0.0115(13) 0.0007(13) C37 0.0265(14) 0.0281(15) 0.0354(15) -0.0010(13) 0.0124(12) 0.0009(12) C38 0.0276(15) 0.0282(16) 0.0374(16) -0.0010(14) 0.0102(13) 0.0014(13) C39 0.0283(16) 0.0283(17) 0.0385(18) -0.0014(15) 0.0088(15) 0.0013(15) C40 0.0255(16) 0.0289(17) 0.0344(17) -0.0008(15) 0.0136(14) 0.0009(14) C41 0.041(4) 0.010(3) 0.035(3) 0.008(3) 0.011(3) 0.003(3) C42 0.042(3) 0.071(5) 0.051(4) 0.001(4) 0.026(3) -0.001(3) Cu1 0.0352(4) 0.0328(4) 0.0314(4) 0.0003(3) 0.0093(3) 0.0002(3) Cu2 0.0291(4) 0.0331(5) 0.0508(5) -0.0032(4) 0.0132(4) -0.0008(3) Cu3 0.0412(5) 0.0620(7) 0.0673(7) -0.0032(5) 0.0123(5) 0.0043(5) Cu4 0.0398(4) 0.0275(4) 0.0445(5) 0.0001(4) 0.0110(4) -0.0009(4) Cu5 0.0299(4) 0.0273(4) 0.0431(5) 0.0024(4) 0.0069(3) 0.0011(3) Tb1 0.01766(13) 0.01764(14) 0.01820(13) 0.00025(11) 0.00148(10) -0.00022(10) Tb2 0.01982(14) 0.01796(15) 0.02087(14) 0.00134(11) 0.00123(11) -0.00145(11) N1 0.034(3) 0.053(4) 0.042(3) -0.003(3) 0.013(3) -0.003(3) N2 0.041(3) 0.059(4) 0.035(3) -0.001(3) 0.015(3) 0.001(3) N3 0.028(3) 0.030(3) 0.025(3) 0.001(2) 0.005(2) -0.001(2) N4 0.051(3) 0.049(4) 0.025(3) 0.015(3) 0.014(3) 0.013(3) N5 0.026(3) 0.033(3) 0.067(4) 0.005(3) 0.007(3) -0.004(2) N6 0.033(3) 0.051(4) 0.027(3) 0.004(3) 0.004(2) -0.002(3) N7 0.041(3) 0.072(5) 0.061(4) 0.003(4) 0.023(3) -0.003(3) N8 0.030(3) 0.025(3) 0.041(3) 0.000(2) 0.009(2) 0.002(2) N9 0.035(3) 0.068(5) 0.042(3) 0.003(3) 0.007(3) 0.000(3) N10 0.087(6) 0.100(6) 0.092(6) 0.022(5) 0.056(5) 0.004(5) N11 0.027(3) 0.031(3) 0.057(4) 0.017(3) 0.003(3) 0.004(2) N13 0.042(3) 0.071(5) 0.051(4) 0.001(4) 0.026(3) -0.001(3) O1 0.037(2) 0.032(2) 0.026(2) -0.0004(19) 0.0012(18) -0.0102(19) O2 0.028(2) 0.026(2) 0.031(2) 0.0087(18) 0.0011(18) 0.0019(18) O3 0.038(2) 0.033(3) 0.030(2) 0.0144(19) 0.0057(19) 0.0013(19) O4 0.056(3) 0.040(3) 0.030(2) -0.013(2) 0.003(2) 0.004(2) O5 0.026(2) 0.034(3) 0.048(3) -0.007(2) 0.011(2) 0.0009(19) O6 0.027(2) 0.033(2) 0.041(2) 0.004(2) 0.0103(19) -0.0062(19) O7 0.025(2) 0.028(2) 0.036(2) 0.0067(19) 0.0024(18) 0.0010(18) O8 0.027(2) 0.028(2) 0.040(2) -0.004(2) 0.0025(19) -0.0084(18) O9 0.036(2) 0.039(3) 0.032(2) 0.017(2) 0.0006(19) 0.001(2) O10 0.031(2) 0.051(3) 0.026(2) -0.013(2) 0.0039(18) 0.000(2) O11 0.035(2) 0.047(3) 0.038(3) -0.003(2) 0.003(2) 0.018(2) O12 0.027(2) 0.034(3) 0.040(2) -0.001(2) 0.0073(19) -0.0096(19) O1W 0.030(2) 0.050(3) 0.038(2) -0.009(2) 0.0138(19) -0.006(2) O2W 0.059(3) 0.036(3) 0.063(3) 0.013(2) 0.041(3) 0.005(2) O3W 0.047(3) 0.031(2) 0.036(2) 0.011(2) 0.020(2) 0.001(2) O4W 0.040(2) 0.040(3) 0.024(2) -0.0063(19) 0.0143(18) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.153(8) . ? C1 Cu1 1.892(6) 1_565 ? C2 N2 1.155(8) . ? C2 Cu2 1.885(6) . ? C3 N3 1.333(7) . ? C3 C4 1.387(7) . ? C3 H4 0.9300 . ? C4 C5 1.385(7) . ? C4 H3 0.9300 . ? C5 C6 1.375(8) . ? C5 C8 1.513(8) . ? C6 C7 1.383(8) . ? C6 H6 0.9300 . ? C7 N3 1.325(7) . ? C7 H5 0.9300 . ? C8 O1 1.241(6) . ? C8 O2 1.240(6) . ? C9 O4 1.234(7) . ? C9 O3 1.242(7) . ? C9 C10 1.515(8) . ? C10 C11 1.352(8) . ? C10 C14 1.369(8) . ? C11 C12 1.381(8) . ? C11 H10 0.9300 . ? C12 N4 1.313(8) . ? C12 H9 0.9300 . ? C13 N4 1.326(8) . ? C13 C14 1.379(8) . ? C13 H8 0.9300 . ? C14 H11 0.9300 . ? C15 O6 1.244(7) . ? C15 O5 1.249(7) . ? C15 C16 1.511(8) . ? C16 C17 1.359(8) . ? C16 C20 1.364(9) . ? C17 C18 1.380(8) . ? C17 H16 0.9300 . ? C18 N5 1.319(8) . ? C18 H19 0.9300 . ? C19 N5 1.322(8) . ? C19 C20 1.396(8) . ? C19 H18 0.9300 . ? C20 H17 0.9300 . ? C21 O9 1.237(7) . ? C21 O10 1.247(7) . ? C21 C22 1.517(8) . ? C22 C23 1.375(8) . ? C22 C25 1.381(8) . ? C23 C24 1.361(8) . ? C23 H22 0.9300 . ? C24 N6 1.335(8) . ? C24 H23 0.9300 . ? C25 C26 1.392(8) . ? C25 H25 0.9300 . ? C26 N6 1.325(8) . ? C26 H24 0.9300 . ? C27 N11 1.337(8) . ? C27 C28 1.384(8) . ? C27 H29 0.9300 . ? C28 C29 1.385(8) . ? C28 H28 0.9300 . ? C29 C31 1.343(8) . ? C29 C30 1.499(8) . ? C30 O7 1.249(7) . ? C30 O8 1.239(7) . ? C31 C32 1.360(8) . ? C31 H31 0.9300 . ? C32 N11 1.290(8) . ? C32 H30 0.9300 . ? C33 N10 1.142(10) . ? C34 N7 1.140(8) . ? C34 Cu4 1.858(7) . ? C35 N8 1.333(7) . ? C35 C36 1.376(8) . ? C35 H35 0.9300 . ? C36 C37 1.389(8) . ? C36 H36 0.9300 . ? C37 C38 1.386(8) . ? C37 C40 1.503(8) . ? C38 C39 1.381(8) . ? C38 H37 0.9300 . ? C39 N8 1.330(7) . ? C39 H34 0.9300 . ? C40 O12 1.245(7) . ? C40 O11 1.247(7) . ? C41 N9 1.130(8) . ? C41 Cu4 1.853(6) 1_565 ? C42 N13 1.137(11) 2_556 ? C42 C42 1.137(11) 2_556 ? C42 Cu3 1.876(6) . ? Cu1 C1 1.892(6) 1_545 ? Cu1 N2 1.932(7) . ? Cu1 N3 2.134(5) . ? Cu2 N1 1.927(6) . ? Cu2 N5 2.117(5) 8_566 ? Cu3 N10 1.894(9) . ? Cu3 Cu5 2.7159(14) . ? Cu4 C41 1.853(6) 1_545 ? Cu4 N8 2.122(5) . ? Cu5 N7 1.912(7) . ? Cu5 N9 1.927(7) . ? Cu5 N11 2.096(5) . ? Tb1 O1 2.299(4) . ? Tb1 O10 2.332(4) . ? Tb1 O7 2.362(4) . ? Tb1 O12 2.365(4) 8_556 ? Tb1 O6 2.380(4) . ? Tb1 O3 2.400(4) . ? Tb1 O4W 2.469(4) . ? Tb1 O3W 2.480(4) . ? Tb2 O8 2.286(4) 1_545 ? Tb2 O4 2.304(4) . ? Tb2 O11 2.320(4) 8_556 ? Tb2 O2 2.336(4) 1_545 ? Tb2 O5 2.373(4) . ? Tb2 O9 2.393(4) . ? Tb2 O1W 2.487(4) . ? Tb2 O2W 2.512(4) . ? N5 Cu2 2.117(5) 8_465 ? O2 Tb2 2.336(4) 1_565 ? O8 Tb2 2.286(4) 1_565 ? O11 Tb2 2.320(4) 8_455 ? O12 Tb1 2.365(4) 8_455 ? O1W H1W 0.7634 . ? O1W H2W 0.9070 . ? O2W H4W 0.9200 . ? O2W H3W 0.9316 . ? O3W H6W 1.0373 . ? O3W H5W 0.8624 . ? O4W H8W 0.8788 . ? O4W H7W 0.8322 . ? 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 N1 C1 Cu1 175.5(6) . 1_565 ? N2 C2 Cu2 176.7(6) . . ? N3 C3 C4 123.0(5) . . ? N3 C3 H4 118.5 . . ? C4 C3 H4 118.5 . . ? C3 C4 C5 119.2(5) . . ? C3 C4 H3 120.4 . . ? C5 C4 H3 120.4 . . ? C6 C5 C4 117.6(5) . . ? C6 C5 C8 121.8(5) . . ? C4 C5 C8 120.6(5) . . ? C7 C6 C5 119.5(5) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? N3 C7 C6 123.4(6) . . ? N3 C7 H5 118.3 . . ? C6 C7 H5 118.3 . . ? O1 C8 O2 126.0(5) . . ? O1 C8 C5 116.9(5) . . ? O2 C8 C5 117.0(5) . . ? O4 C9 O3 125.9(6) . . ? O4 C9 C10 116.5(5) . . ? O3 C9 C10 117.6(5) . . ? C11 C10 C14 117.7(6) . . ? C11 C10 C9 121.4(5) . . ? C14 C10 C9 120.8(6) . . ? C12 C11 C10 119.6(6) . . ? C12 C11 H10 120.2 . . ? C10 C11 H10 120.2 . . ? N4 C12 C11 123.1(6) . . ? N4 C12 H9 118.4 . . ? C11 C12 H9 118.4 . . ? N4 C13 C14 122.7(6) . . ? N4 C13 H8 118.7 . . ? C14 C13 H8 118.7 . . ? C13 C14 C10 119.4(6) . . ? C13 C14 H11 120.3 . . ? C10 C14 H11 120.3 . . ? O6 C15 O5 126.5(6) . . ? O6 C15 C16 118.0(6) . . ? O5 C15 C16 115.3(6) . . ? C17 C16 C20 116.5(6) . . ? C17 C16 C15 121.4(6) . . ? C20 C16 C15 122.0(6) . . ? C16 C17 C18 119.9(6) . . ? C16 C17 H16 120.0 . . ? C18 C17 H16 120.0 . . ? N5 C18 C17 124.6(6) . . ? N5 C18 H19 117.7 . . ? C17 C18 H19 117.7 . . ? N5 C19 C20 124.2(7) . . ? N5 C19 H18 117.9 . . ? C20 C19 H18 117.9 . . ? C16 C20 C19 119.2(6) . . ? C16 C20 H17 120.4 . . ? C19 C20 H17 120.4 . . ? O9 C21 O10 127.0(5) . . ? O9 C21 C22 116.4(5) . . ? O10 C21 C22 116.6(5) . . ? C23 C22 C25 117.8(5) . . ? C23 C22 C21 121.2(6) . . ? C25 C22 C21 121.0(5) . . ? C24 C23 C22 120.3(6) . . ? C24 C23 H22 119.9 . . ? C22 C23 H22 119.9 . . ? N6 C24 C23 121.9(6) . . ? N6 C24 H23 119.1 . . ? C23 C24 H23 119.1 . . ? C22 C25 C26 119.1(6) . . ? C22 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? N6 C26 C25 121.6(6) . . ? N6 C26 H24 119.2 . . ? C25 C26 H24 119.2 . . ? N11 C27 C28 121.7(6) . . ? N11 C27 H29 119.1 . . ? C28 C27 H29 119.1 . . ? C27 C28 C29 119.4(6) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C31 C29 C28 117.1(6) . . ? C31 C29 C30 122.6(6) . . ? C28 C29 C30 119.8(6) . . ? O7 C30 O8 124.8(6) . . ? O7 C30 C29 116.9(5) . . ? O8 C30 C29 118.3(5) . . ? C29 C31 C32 119.5(6) . . ? C29 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? N11 C32 C31 125.2(6) . . ? N11 C32 H30 117.4 . . ? C31 C32 H30 117.4 . . ? N7 C34 Cu4 176.6(6) . . ? N8 C35 C36 123.8(6) . . ? N8 C35 H35 118.1 . . ? C36 C35 H35 118.1 . . ? C35 C36 C37 118.6(6) . . ? C35 C36 H36 120.7 . . ? C37 C36 H36 120.7 . . ? C38 C37 C36 118.0(5) . . ? C38 C37 C40 121.3(5) . . ? C36 C37 C40 120.4(5) . . ? C37 C38 C39 118.7(6) . . ? C37 C38 H37 120.7 . . ? C39 C38 H37 120.7 . . ? N8 C39 C38 123.7(6) . . ? N8 C39 H34 118.2 . . ? C38 C39 H34 118.2 . . ? O12 C40 O11 125.9(5) . . ? O12 C40 C37 117.2(5) . . ? O11 C40 C37 116.8(5) . . ? N9 C41 Cu4 166.5(6) . 1_565 ? N13 C42 C42 0.0(8) 2_556 2_556 ? N13 C42 Cu3 174.3(4) 2_556 . ? C42 C42 Cu3 174.3(4) 2_556 . ? C1 Cu1 N2 147.5(2) 1_545 . ? C1 Cu1 N3 108.4(2) 1_545 . ? N2 Cu1 N3 103.9(2) . . ? C2 Cu2 N1 148.9(2) . . ? C2 Cu2 N5 107.8(2) . 8_566 ? N1 Cu2 N5 103.3(2) . 8_566 ? C42 Cu3 N10 155.2(3) . . ? C42 Cu3 Cu5 80.0(2) . . ? N10 Cu3 Cu5 123.5(3) . . ? C34 Cu4 C41 155.5(3) . 1_545 ? C34 Cu4 N8 104.5(2) . . ? C41 Cu4 N8 100.0(2) 1_545 . ? N7 Cu5 N9 153.8(3) . . ? N7 Cu5 N11 101.8(2) . . ? N9 Cu5 N11 103.4(2) . . ? N7 Cu5 Cu3 65.2(2) . . ? N9 Cu5 Cu3 92.75(18) . . ? N11 Cu5 Cu3 129.70(18) . . ? O1 Tb1 O10 145.51(16) . . ? O1 Tb1 O7 101.76(14) . . ? O10 Tb1 O7 76.69(14) . . ? O1 Tb1 O12 81.57(15) . 8_556 ? O10 Tb1 O12 80.13(14) . 8_556 ? O7 Tb1 O12 142.58(15) . 8_556 ? O1 Tb1 O6 140.38(15) . . ? O10 Tb1 O6 73.58(15) . . ? O7 Tb1 O6 77.00(14) . . ? O12 Tb1 O6 123.52(15) 8_556 . ? O1 Tb1 O3 77.53(14) . . ? O10 Tb1 O3 124.12(15) . . ? O7 Tb1 O3 143.46(15) . . ? O12 Tb1 O3 73.91(15) 8_556 . ? O6 Tb1 O3 81.05(14) . . ? O1 Tb1 O4W 72.32(15) . . ? O10 Tb1 O4W 135.11(14) . . ? O7 Tb1 O4W 70.20(14) . . ? O12 Tb1 O4W 142.91(13) 8_556 . ? O6 Tb1 O4W 70.13(14) . . ? O3 Tb1 O4W 75.03(14) . . ? O1 Tb1 O3W 73.49(14) . . ? O10 Tb1 O3W 72.82(15) . . ? O7 Tb1 O3W 75.52(14) . . ? O12 Tb1 O3W 69.74(14) 8_556 . ? O6 Tb1 O3W 140.46(14) . . ? O3 Tb1 O3W 136.03(14) . . ? O4W Tb1 O3W 124.35(14) . . ? O8 Tb2 O4 144.74(17) 1_545 . ? O8 Tb2 O11 139.76(17) 1_545 8_556 ? O4 Tb2 O11 74.87(18) . 8_556 ? O8 Tb2 O2 95.28(14) 1_545 1_545 ? O4 Tb2 O2 81.12(15) . 1_545 ? O11 Tb2 O2 82.24(14) 8_556 1_545 ? O8 Tb2 O5 86.05(15) 1_545 . ? O4 Tb2 O5 74.88(15) . . ? O11 Tb2 O5 121.66(16) 8_556 . ? O2 Tb2 O5 138.78(15) 1_545 . ? O8 Tb2 O9 82.07(15) 1_545 . ? O4 Tb2 O9 117.67(16) . . ? O11 Tb2 O9 80.93(14) 8_556 . ? O2 Tb2 O9 150.05(16) 1_545 . ? O5 Tb2 O9 71.04(16) . . ? O8 Tb2 O1W 71.22(15) 1_545 . ? O4 Tb2 O1W 139.63(16) . . ? O11 Tb2 O1W 69.15(16) 8_556 . ? O2 Tb2 O1W 76.55(14) 1_545 . ? O5 Tb2 O1W 140.75(14) . . ? O9 Tb2 O1W 74.36(15) . . ? O8 Tb2 O2W 72.76(16) 1_545 . ? O4 Tb2 O2W 72.76(17) . . ? O11 Tb2 O2W 141.23(15) 8_556 . ? O2 Tb2 O2W 72.26(15) 1_545 . ? O5 Tb2 O2W 68.87(15) . . ? O9 Tb2 O2W 133.54(15) . . ? O1W Tb2 O2W 129.11(15) . . ? C1 N1 Cu2 169.9(6) . . ? C2 N2 Cu1 174.5(6) . . ? C7 N3 C3 117.3(5) . . ? C7 N3 Cu1 120.8(4) . . ? C3 N3 Cu1 121.9(4) . . ? C12 N4 C13 117.3(5) . . ? C19 N5 C18 114.7(6) . . ? C19 N5 Cu2 122.6(4) . 8_465 ? C18 N5 Cu2 122.6(4) . 8_465 ? C26 N6 C24 119.3(5) . . ? C34 N7 Cu5 166.1(6) . . ? C39 N8 C35 117.0(5) . . ? C39 N8 Cu4 120.9(4) . . ? C35 N8 Cu4 122.0(4) . . ? C41 N9 Cu5 177.3(6) . . ? C33 N10 Cu3 178.2(8) . . ? C32 N11 C27 116.6(5) . . ? C32 N11 Cu5 120.5(4) . . ? C27 N11 Cu5 117.1(4) . . ? C8 O1 Tb1 165.2(4) . . ? C8 O2 Tb2 142.9(4) . 1_565 ? C9 O3 Tb1 130.9(4) . . ? C9 O4 Tb2 156.0(5) . . ? C15 O5 Tb2 133.9(4) . . ? C15 O6 Tb1 150.1(4) . . ? C30 O7 Tb1 137.7(4) . . ? C30 O8 Tb2 159.8(5) . 1_565 ? C21 O9 Tb2 135.6(4) . . ? C21 O10 Tb1 147.2(4) . . ? C40 O11 Tb2 145.0(4) . 8_455 ? C40 O12 Tb1 125.4(4) . 8_455 ? Tb2 O1W H1W 119.2 . . ? Tb2 O1W H2W 109.8 . . ? H1W O1W H2W 124.6 . . ? Tb2 O2W H4W 121.3 . . ? Tb2 O2W H3W 95.2 . . ? H4W O2W H3W 99.9 . . ? Tb1 O3W H6W 116.9 . . ? Tb1 O3W H5W 140.9 . . ? H6W O3W H5W 77.1 . . ? Tb1 O4W H8W 133.2 . . ? Tb1 O4W H7W 103.5 . . ? H8W O4W H7W 98.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W O8 0.76 2.66 2.784(6) 91.6 1_545 O1W H1W O3W 0.76 2.74 2.997(6) 102.2 1_545 O1W H2W O12 0.91 2.46 3.249(6) 145.8 2_556 O1W H2W O3W 0.91 2.42 3.116(6) 133.6 7_557 O2W H4W O4W 0.92 1.97 2.876(6) 166.8 1_545 O2W H3W O5 0.93 2.20 2.765(6) 117.8 . O2W H3W N1 0.93 2.67 3.301(7) 125.2 4_537 O3W H6W O1W 1.04 2.03 2.997(6) 154.0 1_565 O4W H8W N4 0.88 1.83 2.706(6) 172.8 4_557 O4W H7W O6 0.83 2.34 2.787(6) 113.9 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.321 _refine_diff_density_min -1.145 _refine_diff_density_rms 0.123 data_4 _database_code_depnum_ccdc_archive 'CCDC 722462' #==================================================================== #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C83 H64 Cu10 Gd4 N23 O32' _chemical_formula_sum 'C83 H64 Cu10 Gd4 N23 O32' _chemical_formula_weight 3160.08 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 39.0134(19) _cell_length_b 9.6043(5) _cell_length_c 30.5304(15) _cell_angle_alpha 90.00 _cell_angle_beta 120.8860(10) _cell_angle_gamma 90.00 _cell_volume 9817.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6334 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.63 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6100.0 _exptl_absorpt_coefficient_mu 4.868 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0724 _exptl_absorpt_correction_T_max 0.1564 _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 APEX-II area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24354 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8633 _reflns_number_gt 6953 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'Apex2 (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-XP (Bruker, 2004)' _computing_publication_material SHELXL-97 _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. The cyanice groups are disordered with respect to the C and N termini. So the 'SIMU' and 'ISOR' were used in the restrain refinements for the partial C and N atoms. ; _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^)+(0.0308P)^2^+55.6824P] 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 8633 _refine_ls_number_parameters 685 _refine_ls_number_restraints 192 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.041 _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 C1 C 0.40058(18) 1.5314(6) 1.3697(2) 0.0323(14) Uani 1 1 d . . . C2 C 0.40961(17) 1.0303(6) 1.3785(2) 0.0329(14) Uani 1 1 d . . . C3 C 0.33331(17) 0.6205(6) 1.2413(2) 0.0308(9) Uani 1 1 d U . . H4 H 0.3462 0.5361 1.2547 0.037 Uiso 1 1 calc R . . C4 C 0.30211(16) 0.6236(6) 1.1914(2) 0.0294(8) Uani 1 1 d U . . H3 H 0.2938 0.5423 1.1721 0.035 Uiso 1 1 calc R . . C5 C 0.28338(17) 0.7487(5) 1.1703(2) 0.0282(7) Uani 1 1 d U . . C6 C 0.29683(17) 0.8651(6) 1.2002(2) 0.0311(8) Uani 1 1 d U . . H6 H 0.2854 0.9515 1.1871 0.037 Uiso 1 1 calc R . . C7 C 0.32778(17) 0.8525(6) 1.2504(2) 0.0328(10) Uani 1 1 d U . . H5 H 0.3363 0.9323 1.2705 0.039 Uiso 1 1 calc R . . C8 C 0.24856(17) 0.7551(5) 1.1159(2) 0.0268(9) Uani 1 1 d U . . C9 C 0.22465(18) 0.2380(6) 1.1416(2) 0.0320(9) Uani 1 1 d U . . C10 C 0.24995(18) 0.2029(6) 1.1975(2) 0.0339(7) Uani 1 1 d U . . C11 C 0.23810(18) 0.1054(6) 1.2193(2) 0.0358(8) Uani 1 1 d U . . H10 H 0.2140 0.0590 1.1998 0.043 Uiso 1 1 calc R . . C12 C 0.26242(18) 0.0758(6) 1.2711(2) 0.0370(10) Uani 1 1 d U . . H9 H 0.2535 0.0113 1.2858 0.044 Uiso 1 1 calc R . . C13 C 0.3096(2) 0.2275(6) 1.2783(2) 0.0400(10) Uani 1 1 d U . . H8 H 0.3344 0.2690 1.2982 0.048 Uiso 1 1 calc R . . C14 C 0.28689(18) 0.2643(6) 1.2276(2) 0.0369(9) Uani 1 1 d U . . H11 H 0.2963 0.3296 1.2138 0.044 Uiso 1 1 calc R . . C15 C 0.11328(18) 0.2270(6) 1.0293(3) 0.0396(10) Uani 1 1 d U . . C16 C 0.06826(19) 0.2411(6) 1.0045(3) 0.0429(8) Uani 1 1 d U . . C17 C 0.04423(18) 0.1272(7) 0.9917(3) 0.0453(9) Uani 1 1 d U . . H16 H 0.0554 0.0392 1.0024 0.054 Uiso 1 1 calc R . . C18 C 0.00310(19) 0.1428(7) 0.9628(3) 0.0467(11) Uani 1 1 d U . . H19 H -0.0127 0.0635 0.9550 0.056 Uiso 1 1 calc R . . C19 C 0.00853(19) 0.3746(7) 0.9630(3) 0.0507(11) Uani 1 1 d U . . H18 H -0.0033 0.4622 0.9556 0.061 Uiso 1 1 calc R . . C20 C 0.04995(19) 0.3673(7) 0.9919(3) 0.0483(10) Uani 1 1 d U . . H17 H 0.0651 0.4485 1.0025 0.058 Uiso 1 1 calc R . . C21 C 0.13766(18) 0.2486(6) 0.9436(2) 0.0336(9) Uani 1 1 d U . . C22 C 0.10073(19) 0.2723(6) 0.8918(2) 0.0363(8) Uani 1 1 d U . . C23 C 0.08048(18) 0.1618(6) 0.8603(2) 0.0386(9) Uani 1 1 d U . . H22 H 0.0895 0.0713 0.8705 0.046 Uiso 1 1 calc R . . C24 C 0.04671(19) 0.1865(7) 0.8136(2) 0.0405(10) Uani 1 1 d U . . H23 H 0.0331 0.1112 0.7928 0.049 Uiso 1 1 calc R . . C25 C 0.08677(18) 0.4061(6) 0.8743(2) 0.0390(9) Uani 1 1 d U . . H25 H 0.1005 0.4831 0.8940 0.047 Uiso 1 1 calc R . . C26 C 0.05241(19) 0.4234(7) 0.8276(2) 0.0415(10) Uani 1 1 d U . . H24 H 0.0425 0.5128 0.8167 0.050 Uiso 1 1 calc R . . C27 C 0.0093(2) 0.6857(7) 0.8863(3) 0.0523(12) Uani 1 1 d U . . H29 H -0.0091 0.6134 0.8726 0.063 Uiso 1 1 calc R . . C28 C 0.04846(19) 0.6549(7) 0.9221(3) 0.0490(10) Uani 1 1 d U . . H28 H 0.0561 0.5636 0.9328 0.059 Uiso 1 1 calc R . . C29 C 0.07617(19) 0.7611(6) 0.9420(3) 0.0438(9) Uani 1 1 d U . . C30 C 0.11948(18) 0.7289(6) 0.9789(2) 0.0396(10) Uani 1 1 d U . . C31 C 0.06348(19) 0.8896(6) 0.9230(2) 0.0467(10) Uani 1 1 d U . . H31 H 0.0815 0.9632 0.9338 0.056 Uiso 1 1 calc R . . C32 C 0.02412(19) 0.9119(7) 0.8878(3) 0.0486(12) Uani 1 1 d U . . H30 H 0.0164 1.0018 0.8752 0.058 Uiso 1 1 calc R . . C33 C -0.1561(3) 0.7829(8) 0.6105(3) 0.058(2) Uani 1 1 d U . . C34 C -0.07176(17) 0.5354(6) 0.7744(2) 0.0269(12) Uani 1 1 d U . . C35 C -0.14295(17) 0.1812(6) 0.6766(2) 0.0320(9) Uani 1 1 d U . . H35 H -0.1275 0.1050 0.6949 0.038 Uiso 1 1 calc R . . C36 C -0.17824(16) 0.1574(6) 0.6321(2) 0.0306(8) Uani 1 1 d U . . H36 H -0.1857 0.0670 0.6199 0.037 Uiso 1 1 calc R . . C37 C -0.20274(17) 0.2687(6) 0.6052(2) 0.0296(7) Uani 1 1 d U . . C38 C -0.18845(16) 0.4003(6) 0.6229(2) 0.0321(8) Uani 1 1 d U . . H37 H -0.2033 0.4779 0.6049 0.038 Uiso 1 1 calc R . . C39 C -0.15206(16) 0.4172(6) 0.6674(2) 0.0335(10) Uani 1 1 d U . . H34 H -0.1428 0.5070 0.6785 0.040 Uiso 1 1 calc R . . C40 C -0.24423(17) 0.2444(6) 0.5620(2) 0.0288(9) Uani 1 1 d U . . C41 C -0.06278(17) 1.1586(6) 0.7879(2) 0.0302(14) Uani 1 1 d . . . C42 C -0.01712(18) 0.8122(7) 0.7385(2) 0.0548(18) Uani 0.50 1 d P . . Cu1 Cu 0.39138(2) 0.72126(7) 1.35020(3) 0.03515(19) Uani 1 1 d . . . Cu2 Cu 0.42288(2) 1.22213(7) 1.39142(3) 0.0388(2) Uani 1 1 d . . . Cu3 Cu -0.07276(3) 0.79413(10) 0.70420(4) 0.0623(3) Uani 1 1 d . . . Cu4 Cu -0.07740(2) 0.34189(7) 0.76778(3) 0.0387(2) Uani 1 1 d . . . Cu5 Cu -0.05672(2) 0.84196(7) 0.80084(3) 0.0369(2) Uani 1 1 d . . . Gd1 Gd 0.186149(8) 0.47275(3) 1.045999(9) 0.02120(8) Uani 1 1 d . . . Gd2 Gd 0.184174(8) 0.00864(3) 1.038549(10) 0.02324(8) Uani 1 1 d . . . N1 N 0.40619(15) 1.4142(6) 1.3791(2) 0.0431(14) Uani 1 1 d . . . N2 N 0.40319(16) 0.9142(6) 1.37049(19) 0.0437(14) Uani 1 1 d . . . N3 N 0.34601(15) 0.7327(5) 1.27143(18) 0.0327(12) Uani 1 1 d . . . N4 N 0.29740(17) 0.1349(6) 1.30010(19) 0.0452(14) Uani 1 1 d . . . N5 N -0.01504(15) 0.2645(5) 0.9456(2) 0.0468(16) Uani 1 1 d . . . N6 N 0.03280(15) 0.3147(6) 0.79721(19) 0.0427(14) Uani 1 1 d . . . N7 N -0.06988(17) 0.6540(6) 0.7782(2) 0.0558(17) Uani 1 1 d . . . N8 N -0.12961(14) 0.3096(5) 0.69518(18) 0.0337(12) Uani 1 1 d . . . N9 N -0.06096(16) 1.0411(7) 0.7916(2) 0.0509(16) Uani 1 1 d . . . N10 N -0.1252(2) 0.7888(8) 0.6463(3) 0.086(2) Uani 1 1 d . . . N11 N -0.00322(15) 0.8162(5) 0.8707(2) 0.0442(15) Uani 1 1 d . . . N13 N -0.01712(18) 0.8122(7) 0.7385(2) 0.0548(18) Uani 0.50 1 d P . . O1 O 0.23157(12) 0.6440(4) 1.09592(15) 0.0391(11) Uani 1 1 d . . . O2 O 0.23909(11) 0.8710(4) 1.09492(14) 0.0349(10) Uani 1 1 d . . . O3 O 0.22408(12) 0.3607(4) 1.12850(14) 0.0391(11) Uani 1 1 d . . . O4 O 0.20675(14) 0.1399(4) 1.11251(15) 0.0497(13) Uani 1 1 d . . . O5 O 0.12571(12) 0.1051(4) 1.03310(16) 0.0396(11) Uani 1 1 d . . . O6 O 0.13363(11) 0.3346(4) 1.04298(16) 0.0370(10) Uani 1 1 d . . . O7 O 0.12780(11) 0.6056(4) 0.99326(15) 0.0363(10) Uani 1 1 d . . . O8 O 0.14425(12) 0.8262(4) 0.99225(16) 0.0386(11) Uani 1 1 d . . . O9 O 0.14557(12) 0.1256(4) 0.95775(15) 0.0433(12) Uani 1 1 d . . . O10 O 0.15614(12) 0.3536(4) 0.96786(14) 0.0414(11) Uani 1 1 d . . . O11 O -0.26614(12) 0.3478(4) 0.54230(16) 0.0443(12) Uani 1 1 d . . . O12 O -0.25549(11) 0.1210(4) 0.55005(15) 0.0371(10) Uani 1 1 d . . . O1W O 0.20877(12) -0.0834(4) 0.98288(15) 0.0410(11) Uani 1 1 d . . . H1W H 0.1940 -0.1208 0.9581 0.061 Uiso 1 1 d R . . H2W H 0.2303 -0.0341 0.9877 0.061 Uiso 1 1 d R . . O2W O 0.16538(14) -0.1200(4) 1.09504(17) 0.0495(12) Uani 1 1 d . . . H4W H 0.1602 -0.2143 1.0915 0.074 Uiso 1 1 d R . . H3W H 0.1393 -0.0858 1.0792 0.074 Uiso 1 1 d R . . O3W O 0.20229(12) 0.6052(4) 0.98878(15) 0.0407(11) Uani 1 1 d . . . H6W H 0.2110 0.7083 0.9982 0.061 Uiso 1 1 d R . . H5W H 0.1908 0.6458 0.9594 0.061 Uiso 1 1 d R . . O4W O 0.16173(12) 0.5809(4) 1.09887(14) 0.0342(10) Uani 1 1 d . . . H8W H 0.1734 0.6027 1.1314 0.051 Uiso 1 1 d R . . H7W H 0.1452 0.5235 1.0975 0.051 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.031(3) 0.025(3) 0.032(3) 0.000(2) 0.010(3) 0.003(3) C2 0.025(3) 0.027(3) 0.038(3) -0.005(3) 0.010(3) -0.005(3) C3 0.0304(17) 0.0209(15) 0.0272(16) 0.0000(14) 0.0048(14) 0.0024(14) C4 0.0294(15) 0.0207(14) 0.0265(14) -0.0004(12) 0.0059(13) 0.0016(12) C5 0.0281(14) 0.0209(13) 0.0261(14) -0.0003(11) 0.0071(12) 0.0007(11) C6 0.0306(15) 0.0217(14) 0.0276(15) -0.0008(12) 0.0054(13) 0.0006(12) C7 0.0322(17) 0.0224(16) 0.0286(16) -0.0018(14) 0.0047(14) 0.0007(14) C8 0.0268(16) 0.0206(15) 0.0255(16) -0.0002(13) 0.0081(14) 0.0002(13) C9 0.0315(17) 0.0336(17) 0.0268(16) 0.0032(14) 0.0119(14) 0.0008(14) C10 0.0329(15) 0.0348(15) 0.0281(15) 0.0043(12) 0.0114(13) 0.0001(12) C11 0.0341(16) 0.0369(16) 0.0304(16) 0.0060(13) 0.0122(13) -0.0003(13) C12 0.0353(18) 0.0384(18) 0.0316(17) 0.0073(15) 0.0130(15) -0.0001(15) C13 0.0368(18) 0.0373(18) 0.0307(17) 0.0054(15) 0.0063(15) -0.0025(15) C14 0.0350(16) 0.0359(16) 0.0292(16) 0.0054(13) 0.0088(14) -0.0020(14) C15 0.0258(17) 0.0320(17) 0.053(2) 0.0069(16) 0.0151(16) -0.0018(15) C16 0.0273(15) 0.0330(15) 0.0565(19) 0.0068(14) 0.0129(14) -0.0018(13) C17 0.0281(16) 0.0337(16) 0.059(2) 0.0077(15) 0.0113(15) -0.0024(14) C18 0.0284(18) 0.0343(18) 0.060(2) 0.0077(17) 0.0106(17) -0.0030(16) C19 0.0316(18) 0.0353(18) 0.062(2) 0.0068(17) 0.0076(17) -0.0010(16) C20 0.0303(16) 0.0344(16) 0.060(2) 0.0067(15) 0.0091(15) -0.0016(14) C21 0.0321(18) 0.0347(17) 0.0250(16) -0.0002(14) 0.0081(14) -0.0009(15) C22 0.0338(16) 0.0353(15) 0.0267(15) -0.0001(12) 0.0061(13) -0.0010(13) C23 0.0352(17) 0.0363(16) 0.0278(15) -0.0008(13) 0.0043(13) -0.0020(14) C24 0.0365(19) 0.0376(18) 0.0284(17) -0.0017(15) 0.0030(15) -0.0029(16) C25 0.0356(17) 0.0357(16) 0.0290(15) 0.0004(13) 0.0045(14) 0.0001(14) C26 0.0371(19) 0.0364(18) 0.0310(17) 0.0011(15) 0.0030(15) 0.0012(16) C27 0.0353(19) 0.0353(18) 0.053(2) 0.0097(16) -0.0009(17) -0.0032(16) C28 0.0336(17) 0.0331(16) 0.0509(18) 0.0092(14) 0.0006(15) -0.0024(14) C29 0.0306(16) 0.0300(15) 0.0469(17) 0.0073(13) 0.0027(14) -0.0010(13) C30 0.0283(18) 0.0281(17) 0.0440(19) 0.0062(15) 0.0052(16) -0.0003(15) C31 0.0322(17) 0.0305(16) 0.0485(18) 0.0073(14) 0.0001(15) -0.0008(14) C32 0.0333(19) 0.0311(18) 0.050(2) 0.0071(16) -0.0017(16) -0.0001(16) C33 0.057(2) 0.059(2) 0.056(2) 0.0014(10) 0.0282(13) -0.0002(10) C34 0.0267(15) 0.0239(15) 0.0274(15) -0.0003(9) 0.0119(10) -0.0003(10) C35 0.0246(17) 0.0262(16) 0.0349(17) -0.0001(14) 0.0080(14) -0.0005(14) C36 0.0236(15) 0.0260(14) 0.0342(15) -0.0002(12) 0.0090(13) -0.0003(12) C37 0.0227(14) 0.0262(13) 0.0336(14) -0.0003(11) 0.0100(12) 0.0003(11) C38 0.0241(15) 0.0264(14) 0.0357(15) -0.0003(13) 0.0082(13) 0.0011(12) C39 0.0249(17) 0.0265(16) 0.0370(17) -0.0007(14) 0.0071(14) 0.0012(14) C40 0.0224(16) 0.0266(16) 0.0327(16) -0.0008(14) 0.0106(14) 0.0007(14) C41 0.036(4) 0.012(3) 0.026(3) 0.007(2) 0.004(3) 0.005(2) C42 0.048(4) 0.068(4) 0.048(4) -0.003(3) 0.024(4) -0.002(3) Cu1 0.0347(4) 0.0284(4) 0.0309(4) -0.0001(3) 0.0087(3) 0.0000(3) Cu2 0.0295(4) 0.0278(4) 0.0492(5) -0.0031(3) 0.0130(4) -0.0015(3) Cu3 0.0401(6) 0.0606(6) 0.0643(6) -0.0034(5) 0.0112(5) 0.0041(4) Cu4 0.0366(5) 0.0223(4) 0.0423(5) 0.0005(3) 0.0096(4) -0.0009(3) Cu5 0.0291(4) 0.0227(4) 0.0423(5) 0.0020(3) 0.0064(4) 0.0008(3) Gd1 0.01723(14) 0.01668(13) 0.01841(14) 0.00054(10) 0.00104(11) -0.00043(10) Gd2 0.01904(15) 0.01667(14) 0.02109(14) 0.00128(10) 0.00104(11) -0.00072(11) N1 0.033(3) 0.046(4) 0.039(3) -0.004(3) 0.011(3) -0.001(3) N2 0.041(3) 0.047(4) 0.033(3) 0.001(3) 0.012(3) -0.003(3) N3 0.030(3) 0.029(3) 0.028(3) 0.003(2) 0.006(2) 0.000(2) N4 0.052(4) 0.051(3) 0.028(3) 0.013(3) 0.018(3) 0.012(3) N5 0.023(3) 0.033(3) 0.064(4) 0.007(3) 0.007(3) 0.001(2) N6 0.032(3) 0.052(3) 0.026(3) 0.003(2) 0.002(2) 0.001(3) N7 0.043(4) 0.056(4) 0.058(4) 0.000(3) 0.019(3) -0.001(3) N8 0.025(3) 0.027(3) 0.034(3) -0.002(2) 0.005(2) -0.001(2) N9 0.036(3) 0.060(4) 0.039(3) 0.001(3) 0.006(3) 0.004(3) N10 0.083(6) 0.085(6) 0.094(6) 0.012(5) 0.049(5) -0.001(4) N11 0.023(3) 0.035(3) 0.053(4) 0.017(3) 0.004(3) 0.006(2) N13 0.048(4) 0.068(4) 0.048(4) -0.003(3) 0.024(4) -0.002(3) O1 0.036(2) 0.028(2) 0.030(2) 0.0008(17) 0.0004(19) -0.0107(19) O2 0.026(2) 0.027(2) 0.030(2) 0.0076(17) -0.0013(18) 0.0029(17) O3 0.036(3) 0.036(2) 0.026(2) 0.0139(18) 0.0023(19) 0.0016(19) O4 0.052(3) 0.042(3) 0.028(2) -0.015(2) 0.001(2) 0.000(2) O5 0.027(2) 0.034(2) 0.049(3) -0.004(2) 0.013(2) -0.0003(19) O6 0.025(2) 0.030(2) 0.044(3) 0.0043(18) 0.0087(19) -0.0056(18) O7 0.024(2) 0.026(2) 0.039(2) 0.0078(18) 0.0026(19) 0.0018(17) O8 0.027(2) 0.028(2) 0.042(3) -0.0055(18) 0.004(2) -0.0073(18) O9 0.034(3) 0.042(3) 0.030(2) 0.0143(19) -0.0009(19) -0.003(2) O10 0.033(2) 0.048(3) 0.023(2) -0.0154(19) -0.0005(19) -0.002(2) O11 0.029(2) 0.041(3) 0.039(3) -0.006(2) 0.000(2) 0.017(2) O12 0.027(2) 0.034(2) 0.039(2) 0.0005(19) 0.0081(19) -0.0062(18) O1W 0.033(2) 0.050(3) 0.033(2) -0.008(2) 0.012(2) -0.006(2) O2W 0.062(3) 0.034(2) 0.062(3) 0.013(2) 0.039(3) 0.007(2) O3W 0.045(3) 0.037(2) 0.038(2) 0.014(2) 0.020(2) 0.002(2) O4W 0.036(2) 0.036(2) 0.028(2) -0.0078(18) 0.0146(19) -0.0034(19) _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 C1 N1 1.154(7) . ? C1 Cu1 1.895(6) 1_565 ? C2 N2 1.142(7) . ? C2 Cu2 1.899(6) . ? C3 N3 1.336(7) . ? C3 C4 1.378(7) . ? C3 H4 0.9300 . ? C4 C5 1.381(7) . ? C4 H3 0.9300 . ? C5 C6 1.367(7) . ? C5 C8 1.514(7) . ? C6 C7 1.385(7) . ? C6 H6 0.9300 . ? C7 N3 1.332(7) . ? C7 H5 0.9300 . ? C8 O1 1.239(6) . ? C8 O2 1.243(6) . ? C9 O4 1.235(7) . ? C9 O3 1.241(7) . ? C9 C10 1.506(8) . ? C10 C11 1.361(8) . ? C10 C14 1.382(8) . ? C11 C12 1.393(8) . ? C11 H10 0.9300 . ? C12 N4 1.315(8) . ? C12 H9 0.9300 . ? C13 N4 1.336(8) . ? C13 C14 1.377(8) . ? C13 H8 0.9300 . ? C14 H11 0.9300 . ? C15 O6 1.238(7) . ? C15 O5 1.249(7) . ? C15 C16 1.520(9) . ? C16 C20 1.359(8) . ? C16 C17 1.360(8) . ? C17 C18 1.386(8) . ? C17 H16 0.9300 . ? C18 N5 1.327(8) . ? C18 H19 0.9300 . ? C19 N5 1.321(8) . ? C19 C20 1.389(9) . ? C19 H18 0.9300 . ? C20 H17 0.9300 . ? C21 O10 1.240(7) . ? C21 O9 1.241(7) . ? C21 C22 1.513(8) . ? C22 C23 1.376(8) . ? C22 C25 1.390(8) . ? C23 C24 1.377(8) . ? C23 H22 0.9300 . ? C24 N6 1.335(8) . ? C24 H23 0.9300 . ? C25 C26 1.377(8) . ? C25 H25 0.9300 . ? C26 N6 1.344(8) . ? C26 H24 0.9300 . ? C27 N11 1.340(8) . ? C27 C28 1.380(8) . ? C27 H29 0.9300 . ? C28 C29 1.380(8) . ? C28 H28 0.9300 . ? C29 C31 1.345(8) . ? C29 C30 1.505(8) . ? C30 O7 1.247(7) . ? C30 O8 1.253(7) . ? C31 C32 1.365(8) . ? C31 H31 0.9300 . ? C32 N11 1.298(8) . ? C32 H30 0.9300 . ? C33 N10 1.137(10) . ? C34 N7 1.143(8) . ? C34 Cu4 1.870(6) . ? C35 N8 1.346(7) . ? C35 C36 1.369(7) . ? C35 H35 0.9300 . ? C36 C37 1.388(7) . ? C36 H36 0.9300 . ? C37 C38 1.376(8) . ? C37 C40 1.490(8) . ? C38 C39 1.381(7) . ? C38 H37 0.9300 . ? C39 N8 1.338(7) . ? C39 H34 0.9300 . ? C40 O11 1.245(6) . ? C40 O12 1.251(6) . ? C41 N9 1.132(7) . ? C41 Cu4 1.855(5) 1_565 ? C42 N13 1.146(12) 2_556 ? C42 C42 1.146(12) 2_556 ? C42 Cu3 1.872(6) . ? Cu1 C1 1.895(6) 1_545 ? Cu1 N2 1.933(6) . ? Cu1 N3 2.135(5) . ? Cu2 N1 1.928(6) . ? Cu2 N5 2.123(5) 8_566 ? Cu3 N10 1.898(8) . ? Cu3 Cu5 2.7225(14) . ? Cu4 C41 1.855(5) 1_545 ? Cu4 N8 2.127(5) . ? Cu5 N7 1.907(6) . ? Cu5 N9 1.928(6) . ? Cu5 N11 2.097(5) . ? Gd1 O1 2.323(4) . ? Gd1 O10 2.346(4) . ? Gd1 O7 2.375(4) . ? Gd1 O12 2.392(4) 8_556 ? Gd1 O6 2.403(4) . ? Gd1 O3 2.422(4) . ? Gd1 O4W 2.484(4) . ? Gd1 O3W 2.489(4) . ? Gd2 O8 2.288(4) 1_545 ? Gd2 O4 2.329(4) . ? Gd2 O11 2.333(4) 8_556 ? Gd2 O2 2.348(3) 1_545 ? Gd2 O5 2.387(4) . ? Gd2 O9 2.409(4) . ? Gd2 O1W 2.503(4) . ? Gd2 O2W 2.518(4) . ? N5 Cu2 2.123(5) 8_465 ? O2 Gd2 2.348(3) 1_565 ? O8 Gd2 2.288(4) 1_565 ? O11 Gd2 2.333(4) 8_455 ? O12 Gd1 2.392(4) 8_455 ? O1W H1W 0.7649 . ? O1W H2W 0.9083 . ? O2W H4W 0.9214 . ? O2W H3W 0.9334 . ? O3W H6W 1.0389 . ? O3W H5W 0.8638 . ? O4W H8W 0.8802 . ? O4W H7W 0.8333 . ? 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 N1 C1 Cu1 176.1(6) . 1_565 ? N2 C2 Cu2 176.7(6) . . ? N3 C3 C4 123.3(5) . . ? N3 C3 H4 118.4 . . ? C4 C3 H4 118.4 . . ? C3 C4 C5 119.3(5) . . ? C3 C4 H3 120.3 . . ? C5 C4 H3 120.3 . . ? C6 C5 C4 118.0(5) . . ? C6 C5 C8 121.4(5) . . ? C4 C5 C8 120.6(5) . . ? C5 C6 C7 119.0(5) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? N3 C7 C6 123.8(5) . . ? N3 C7 H5 118.1 . . ? C6 C7 H5 118.1 . . ? O1 C8 O2 125.2(5) . . ? O1 C8 C5 117.2(5) . . ? O2 C8 C5 117.6(5) . . ? O4 C9 O3 125.6(6) . . ? O4 C9 C10 116.3(5) . . ? O3 C9 C10 118.0(5) . . ? C11 C10 C14 117.9(6) . . ? C11 C10 C9 121.3(5) . . ? C14 C10 C9 120.8(6) . . ? C10 C11 C12 119.5(6) . . ? C10 C11 H10 120.3 . . ? C12 C11 H10 120.3 . . ? N4 C12 C11 122.9(6) . . ? N4 C12 H9 118.5 . . ? C11 C12 H9 118.5 . . ? N4 C13 C14 122.9(6) . . ? N4 C13 H8 118.5 . . ? C14 C13 H8 118.5 . . ? C13 C14 C10 119.2(6) . . ? C13 C14 H11 120.4 . . ? C10 C14 H11 120.4 . . ? O6 C15 O5 126.9(6) . . ? O6 C15 C16 118.1(5) . . ? O5 C15 C16 115.1(5) . . ? C20 C16 C17 116.8(6) . . ? C20 C16 C15 121.7(6) . . ? C17 C16 C15 121.4(6) . . ? C16 C17 C18 119.9(6) . . ? C16 C17 H16 120.1 . . ? C18 C17 H16 120.1 . . ? N5 C18 C17 123.7(6) . . ? N5 C18 H19 118.2 . . ? C17 C18 H19 118.2 . . ? N5 C19 C20 123.9(6) . . ? N5 C19 H18 118.1 . . ? C20 C19 H18 118.1 . . ? C16 C20 C19 119.7(6) . . ? C16 C20 H17 120.1 . . ? C19 C20 H17 120.1 . . ? O10 C21 O9 127.0(5) . . ? O10 C21 C22 116.9(5) . . ? O9 C21 C22 116.1(5) . . ? C23 C22 C25 118.3(5) . . ? C23 C22 C21 120.7(5) . . ? C25 C22 C21 121.0(5) . . ? C22 C23 C24 119.4(6) . . ? C22 C23 H22 120.3 . . ? C24 C23 H22 120.3 . . ? N6 C24 C23 122.4(6) . . ? N6 C24 H23 118.8 . . ? C23 C24 H23 118.8 . . ? C26 C25 C22 119.3(6) . . ? C26 C25 H25 120.3 . . ? C22 C25 H25 120.3 . . ? N6 C26 C25 121.8(6) . . ? N6 C26 H24 119.1 . . ? C25 C26 H24 119.1 . . ? N11 C27 C28 122.3(6) . . ? N11 C27 H29 118.8 . . ? C28 C27 H29 118.8 . . ? C27 C28 C29 119.3(6) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C31 C29 C28 117.2(6) . . ? C31 C29 C30 122.3(6) . . ? C28 C29 C30 120.1(5) . . ? O7 C30 O8 125.2(6) . . ? O7 C30 C29 116.6(5) . . ? O8 C30 C29 118.2(5) . . ? C29 C31 C32 120.0(6) . . ? C29 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? N11 C32 C31 124.5(6) . . ? N11 C32 H30 117.8 . . ? C31 C32 H30 117.8 . . ? N7 C34 Cu4 177.1(6) . . ? N8 C35 C36 123.1(5) . . ? N8 C35 H35 118.5 . . ? C36 C35 H35 118.5 . . ? C35 C36 C37 119.7(5) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 117.3(5) . . ? C38 C37 C40 121.9(5) . . ? C36 C37 C40 120.6(5) . . ? C37 C38 C39 120.0(5) . . ? C37 C38 H37 120.0 . . ? C39 C38 H37 120.0 . . ? N8 C39 C38 122.7(5) . . ? N8 C39 H34 118.6 . . ? C38 C39 H34 118.6 . . ? O11 C40 O12 124.3(5) . . ? O11 C40 C37 117.8(5) . . ? O12 C40 C37 117.7(5) . . ? N9 C41 Cu4 166.3(5) . 1_565 ? N13 C42 C42 0.0(10) 2_556 2_556 ? N13 C42 Cu3 174.0(5) 2_556 . ? C42 C42 Cu3 174.0(5) 2_556 . ? C1 Cu1 N2 147.8(2) 1_545 . ? C1 Cu1 N3 108.5(2) 1_545 . ? N2 Cu1 N3 103.6(2) . . ? C2 Cu2 N1 149.2(2) . . ? C2 Cu2 N5 107.5(2) . 8_566 ? N1 Cu2 N5 103.3(2) . 8_566 ? C42 Cu3 N10 155.5(3) . . ? C42 Cu3 Cu5 79.7(2) . . ? N10 Cu3 Cu5 123.5(3) . . ? C41 Cu4 C34 155.3(2) 1_545 . ? C41 Cu4 N8 100.0(2) 1_545 . ? C34 Cu4 N8 104.7(2) . . ? N7 Cu5 N9 154.0(2) . . ? N7 Cu5 N11 101.5(2) . . ? N9 Cu5 N11 103.4(2) . . ? N7 Cu5 Cu3 65.0(2) . . ? N9 Cu5 Cu3 93.12(18) . . ? N11 Cu5 Cu3 129.63(18) . . ? O1 Gd1 O10 145.79(16) . . ? O1 Gd1 O7 101.98(14) . . ? O10 Gd1 O7 76.60(14) . . ? O1 Gd1 O12 81.22(15) . 8_556 ? O10 Gd1 O12 80.44(14) . 8_556 ? O7 Gd1 O12 142.48(15) . 8_556 ? O1 Gd1 O6 139.86(16) . . ? O10 Gd1 O6 73.80(16) . . ? O7 Gd1 O6 76.64(14) . . ? O12 Gd1 O6 124.35(14) 8_556 . ? O1 Gd1 O3 77.24(14) . . ? O10 Gd1 O3 124.08(15) . . ? O7 Gd1 O3 143.62(16) . . ? O12 Gd1 O3 73.84(15) 8_556 . ? O6 Gd1 O3 81.27(14) . . ? O1 Gd1 O4W 72.27(15) . . ? O10 Gd1 O4W 134.99(14) . . ? O7 Gd1 O4W 70.24(14) . . ? O12 Gd1 O4W 142.77(13) 8_556 . ? O6 Gd1 O4W 69.63(14) . . ? O3 Gd1 O4W 75.13(14) . . ? O1 Gd1 O3W 73.51(15) . . ? O10 Gd1 O3W 73.11(15) . . ? O7 Gd1 O3W 75.50(14) . . ? O12 Gd1 O3W 69.61(14) 8_556 . ? O6 Gd1 O3W 140.64(14) . . ? O3 Gd1 O3W 135.83(14) . . ? O4W Gd1 O3W 124.20(14) . . ? O8 Gd2 O4 144.34(18) 1_545 . ? O8 Gd2 O11 140.17(17) 1_545 8_556 ? O4 Gd2 O11 75.00(17) . 8_556 ? O8 Gd2 O2 95.59(14) 1_545 1_545 ? O4 Gd2 O2 81.11(15) . 1_545 ? O11 Gd2 O2 82.78(14) 8_556 1_545 ? O8 Gd2 O5 86.05(15) 1_545 . ? O4 Gd2 O5 74.32(15) . . ? O11 Gd2 O5 120.93(15) 8_556 . ? O2 Gd2 O5 138.52(15) 1_545 . ? O8 Gd2 O9 81.66(14) 1_545 . ? O4 Gd2 O9 117.84(16) . . ? O11 Gd2 O9 80.88(14) 8_556 . ? O2 Gd2 O9 150.31(16) 1_545 . ? O5 Gd2 O9 71.03(16) . . ? O8 Gd2 O1W 71.74(15) 1_545 . ? O4 Gd2 O1W 139.79(16) . . ? O11 Gd2 O1W 69.13(16) 8_556 . ? O2 Gd2 O1W 77.01(14) 1_545 . ? O5 Gd2 O1W 140.84(14) . . ? O9 Gd2 O1W 74.06(15) . . ? O8 Gd2 O2W 72.66(16) 1_545 . ? O4 Gd2 O2W 72.53(17) . . ? O11 Gd2 O2W 141.57(15) 8_556 . ? O2 Gd2 O2W 72.46(15) 1_545 . ? O5 Gd2 O2W 68.56(15) . . ? O9 Gd2 O2W 132.98(15) . . ? O1W Gd2 O2W 129.77(15) . . ? C1 N1 Cu2 169.5(6) . . ? C2 N2 Cu1 174.3(6) . . ? C7 N3 C3 116.5(5) . . ? C7 N3 Cu1 121.1(4) . . ? C3 N3 Cu1 122.3(4) . . ? C12 N4 C13 117.6(5) . . ? C19 N5 C18 115.2(5) . . ? C19 N5 Cu2 123.1(4) . 8_465 ? C18 N5 Cu2 121.7(4) . 8_465 ? C24 N6 C26 118.7(5) . . ? C34 N7 Cu5 166.2(6) . . ? C39 N8 C35 117.1(5) . . ? C39 N8 Cu4 120.9(4) . . ? C35 N8 Cu4 121.9(4) . . ? C41 N9 Cu5 177.8(6) . . ? C33 N10 Cu3 177.2(9) . . ? C32 N11 C27 116.5(5) . . ? C32 N11 Cu5 120.6(4) . . ? C27 N11 Cu5 117.6(4) . . ? C8 O1 Gd1 165.5(4) . . ? C8 O2 Gd2 143.2(4) . 1_565 ? C9 O3 Gd1 131.1(4) . . ? C9 O4 Gd2 154.5(5) . . ? C15 O5 Gd2 132.9(4) . . ? C15 O6 Gd1 149.3(5) . . ? C30 O7 Gd1 137.3(4) . . ? C30 O8 Gd2 160.0(5) . 1_565 ? C21 O9 Gd2 135.5(4) . . ? C21 O10 Gd1 146.9(4) . . ? C40 O11 Gd2 147.4(5) . 8_455 ? C40 O12 Gd1 123.7(4) . 8_455 ? Gd2 O1W H1W 118.7 . . ? Gd2 O1W H2W 110.5 . . ? H1W O1W H2W 124.7 . . ? Gd2 O2W H4W 121.6 . . ? Gd2 O2W H3W 95.4 . . ? H4W O2W H3W 99.9 . . ? Gd1 O3W H6W 117.3 . . ? Gd1 O3W H5W 141.0 . . ? H6W O3W H5W 77.1 . . ? Gd1 O4W H8W 133.2 . . ? Gd1 O4W H7W 103.7 . . ? H8W O4W H7W 98.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W O8 0.76 2.68 2.813(6) 91.9 1_545 O1W H1W O3W 0.76 2.76 3.015(6) 102.4 1_545 O1W H2W O12 0.91 2.38 3.174(6) 145.5 2_556 O1W H2W O3W 0.91 2.44 3.122(6) 132.0 7_557 O2W H4W O4W 0.92 1.98 2.881(6) 166.3 1_545 O2W H3W O5 0.93 2.20 2.764(6) 117.8 . O2W H3W N1 0.93 2.66 3.284(7) 124.6 4_537 O3W H6W O1W 1.04 2.05 3.015(6) 154.1 1_565 O4W H8W N4 0.88 1.82 2.697(6) 173.1 4_557 O4W H7W O6 0.83 2.34 2.791(5) 114.1 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.151 _refine_diff_density_min -1.042 _refine_diff_density_rms 0.124 data_5 _database_code_depnum_ccdc_archive 'CCDC 722463' #==================================================================== #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C83 H64 Cu10 N23 O32 Sm4' _chemical_formula_sum 'C83 H64 Cu10 N23 O32 Sm4' _chemical_formula_weight 3132.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 39.020(2) _cell_length_b 9.6088(5) _cell_length_c 30.5665(15) _cell_angle_alpha 90.00 _cell_angle_beta 120.8200(10) _cell_angle_gamma 90.00 _cell_volume 9842.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5521 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.82 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6068.0 _exptl_absorpt_coefficient_mu 4.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0815 _exptl_absorpt_correction_T_max 0.1745 _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 APEX-II area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24415 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8660 _reflns_number_gt 6800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'Apex2 (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-XP (Bruker, 2004)' _computing_publication_material SHELXL-97 _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. The cyanice groups are disordered with respect to the C and N termini. So the 'SIMU' and 'ISOR' were used in the restrain refinements for the partial C and N atoms. ; _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^)+(0.0349P)^2^+46.0500P] 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 8660 _refine_ls_number_parameters 685 _refine_ls_number_restraints 192 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.054 _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 C1 C 0.40093(19) 1.5296(6) 1.3700(2) 0.0335(15) Uani 1 1 d . . . C2 C 0.40958(18) 1.0290(6) 1.3782(2) 0.0328(15) Uani 1 1 d . . . C3 C 0.33329(18) 0.6194(6) 1.2419(2) 0.0324(9) Uani 1 1 d U . . H4 H 0.3460 0.5349 1.2554 0.039 Uiso 1 1 calc R . . C4 C 0.30236(18) 0.6220(6) 1.1922(2) 0.0313(8) Uani 1 1 d U . . H3 H 0.2939 0.5402 1.1733 0.038 Uiso 1 1 calc R . . C5 C 0.28381(19) 0.7476(6) 1.1705(2) 0.0303(7) Uani 1 1 d U . . C6 C 0.29754(18) 0.8630(6) 1.2011(2) 0.0339(8) Uani 1 1 d U . . H6 H 0.2860 0.9495 1.1885 0.041 Uiso 1 1 calc R . . C7 C 0.32859(19) 0.8504(6) 1.2509(2) 0.0359(10) Uani 1 1 d U . . H5 H 0.3376 0.9305 1.2707 0.043 Uiso 1 1 calc R . . C8 C 0.24935(18) 0.7538(6) 1.1166(2) 0.0288(9) Uani 1 1 d U . . C9 C 0.2253(2) 0.2371(7) 1.1419(2) 0.0350(9) Uani 1 1 d U . . C10 C 0.2505(2) 0.2005(7) 1.1977(2) 0.0364(8) Uani 1 1 d U . . C11 C 0.2384(2) 0.1022(7) 1.2190(2) 0.0384(9) Uani 1 1 d U . . H10 H 0.2144 0.0553 1.1993 0.046 Uiso 1 1 calc R . . C12 C 0.2624(2) 0.0731(7) 1.2705(2) 0.0395(10) Uani 1 1 d U . . H9 H 0.2534 0.0083 1.2849 0.047 Uiso 1 1 calc R . . C13 C 0.3096(2) 0.2239(7) 1.2786(3) 0.0426(10) Uani 1 1 d U . . H8 H 0.3346 0.2644 1.2986 0.051 Uiso 1 1 calc R . . C14 C 0.2870(2) 0.2616(7) 1.2279(2) 0.0394(9) Uani 1 1 d U . . H11 H 0.2965 0.3277 1.2144 0.047 Uiso 1 1 calc R . . C15 C 0.1126(2) 0.2246(7) 1.0293(3) 0.0402(10) Uani 1 1 d U . . C16 C 0.0679(2) 0.2392(7) 1.0039(3) 0.0447(9) Uani 1 1 d U . . C17 C 0.0438(2) 0.1262(7) 0.9912(3) 0.0474(10) Uani 1 1 d U . . H16 H 0.0548 0.0379 1.0018 0.057 Uiso 1 1 calc R . . C18 C 0.0026(2) 0.1435(7) 0.9620(3) 0.0492(11) Uani 1 1 d U . . H19 H -0.0134 0.0646 0.9538 0.059 Uiso 1 1 calc R . . C19 C 0.0081(2) 0.3752(7) 0.9632(3) 0.0528(12) Uani 1 1 d U . . H18 H -0.0037 0.4627 0.9564 0.063 Uiso 1 1 calc R . . C20 C 0.0494(2) 0.3666(7) 0.9915(3) 0.0500(10) Uani 1 1 d U . . H17 H 0.0646 0.4475 1.0022 0.060 Uiso 1 1 calc R . . C21 C 0.1371(2) 0.2461(7) 0.9431(2) 0.0355(10) Uani 1 1 d U . . C22 C 0.1006(2) 0.2722(7) 0.8914(2) 0.0382(8) Uani 1 1 d U . . C23 C 0.0801(2) 0.1631(7) 0.8596(2) 0.0414(9) Uani 1 1 d U . . H22 H 0.0891 0.0726 0.8696 0.050 Uiso 1 1 calc R . . C24 C 0.0467(2) 0.1864(7) 0.8134(2) 0.0436(11) Uani 1 1 d U . . H23 H 0.0333 0.1109 0.7925 0.052 Uiso 1 1 calc R . . C25 C 0.0866(2) 0.4035(7) 0.8746(2) 0.0411(9) Uani 1 1 d U . . H25 H 0.0999 0.4801 0.8948 0.049 Uiso 1 1 calc R . . C26 C 0.0524(2) 0.4219(7) 0.8272(2) 0.0431(11) Uani 1 1 d U . . H24 H 0.0431 0.5118 0.8161 0.052 Uiso 1 1 calc R . . C27 C 0.0091(2) 0.6854(7) 0.8864(3) 0.0574(12) Uani 1 1 d U . . H29 H -0.0093 0.6130 0.8728 0.069 Uiso 1 1 calc R . . C28 C 0.0482(2) 0.6555(7) 0.9222(3) 0.0543(10) Uani 1 1 d U . . H28 H 0.0557 0.5642 0.9329 0.065 Uiso 1 1 calc R . . C29 C 0.0760(2) 0.7601(7) 0.9420(3) 0.0487(9) Uani 1 1 d U . . C30 C 0.1190(2) 0.7259(7) 0.9783(3) 0.0438(11) Uani 1 1 d U . . C31 C 0.0635(2) 0.8889(7) 0.9227(3) 0.0513(10) Uani 1 1 d U . . H31 H 0.0815 0.9625 0.9338 0.062 Uiso 1 1 calc R . . C32 C 0.0240(2) 0.9111(7) 0.8865(3) 0.0527(12) Uani 1 1 d U . . H30 H 0.0165 0.9999 0.8727 0.063 Uiso 1 1 calc R . . C33 C -0.1559(3) 0.7837(9) 0.6115(3) 0.060(2) Uani 1 1 d U . . C34 C -0.07173(18) 0.5352(7) 0.7744(2) 0.0308(14) Uani 1 1 d U . . C35 C -0.14256(19) 0.1822(7) 0.6772(2) 0.0367(10) Uani 1 1 d U . . H35 H -0.1268 0.1065 0.6954 0.044 Uiso 1 1 calc R . . C36 C -0.17779(18) 0.1573(7) 0.6329(2) 0.0351(8) Uani 1 1 d U . . H36 H -0.1853 0.0668 0.6211 0.042 Uiso 1 1 calc R . . C37 C -0.20225(19) 0.2687(6) 0.6059(2) 0.0338(8) Uani 1 1 d U . . C38 C -0.18805(18) 0.4016(6) 0.6237(2) 0.0362(8) Uani 1 1 d U . . H37 H -0.2028 0.4793 0.6059 0.043 Uiso 1 1 calc R . . C39 C -0.15176(18) 0.4168(7) 0.6682(2) 0.0374(10) Uani 1 1 d U . . H34 H -0.1423 0.5064 0.6794 0.045 Uiso 1 1 calc R . . C40 C -0.24364(19) 0.2441(6) 0.5620(2) 0.0322(9) Uani 1 1 d U . . C41 C -0.06287(19) 1.1582(6) 0.7879(2) 0.0321(15) Uani 1 1 d . . . C42 C -0.01678(19) 0.8124(7) 0.7386(3) 0.0579(19) Uani 0.50 1 d P . . Cu1 Cu 0.39160(2) 0.71936(8) 1.35052(3) 0.0363(2) Uani 1 1 d . . . Cu2 Cu 0.42285(2) 1.22028(8) 1.39116(3) 0.0401(2) Uani 1 1 d . . . Cu3 Cu -0.07261(3) 0.79439(11) 0.70436(4) 0.0650(3) Uani 1 1 d . . . Cu4 Cu -0.07728(3) 0.34225(8) 0.76807(3) 0.0410(2) Uani 1 1 d . . . Cu5 Cu -0.05665(2) 0.84211(8) 0.80087(3) 0.0386(2) Uani 1 1 d . . . Sm1 Sm 0.186437(9) 0.47079(3) 1.045975(11) 0.02327(9) Uani 1 1 d . . . Sm2 Sm 0.184206(9) 0.00724(3) 1.038596(11) 0.02536(9) Uani 1 1 d . . . N1 N 0.40617(16) 1.4123(6) 1.3791(2) 0.0441(14) Uani 1 1 d . . . N2 N 0.40331(17) 0.9130(6) 1.3707(2) 0.0430(14) Uani 1 1 d . . . N3 N 0.34616(15) 0.7314(5) 1.27192(19) 0.0320(12) Uani 1 1 d . . . N4 N 0.29704(18) 0.1316(6) 1.2999(2) 0.0466(15) Uani 1 1 d . . . N5 N -0.01509(17) 0.2643(5) 0.9455(2) 0.0491(16) Uani 1 1 d . . . N6 N 0.03248(16) 0.3157(6) 0.79710(19) 0.0448(15) Uani 1 1 d . . . N7 N -0.07018(18) 0.6542(7) 0.7781(2) 0.0578(17) Uani 1 1 d . . . N8 N -0.12972(15) 0.3097(5) 0.6956(2) 0.0365(13) Uani 1 1 d . . . N9 N -0.06103(17) 1.0408(7) 0.7917(2) 0.0521(16) Uani 1 1 d . . . N10 N -0.1250(3) 0.7879(8) 0.6465(3) 0.088(3) Uani 1 1 d . . . N11 N -0.00331(16) 0.8156(6) 0.8705(2) 0.0467(15) Uani 1 1 d . . . N13 N -0.01678(19) 0.8124(7) 0.7386(3) 0.0579(19) Uani 0.50 1 d P . . O1 O 0.23223(13) 0.6436(4) 1.09639(15) 0.0408(11) Uani 1 1 d . . . O2 O 0.23994(12) 0.8706(4) 1.09564(15) 0.0385(11) Uani 1 1 d . . . O3 O 0.22520(13) 0.3598(4) 1.12938(15) 0.0418(11) Uani 1 1 d . . . O4 O 0.20643(15) 0.1397(5) 1.11272(17) 0.0557(14) Uani 1 1 d . . . O5 O 0.12515(13) 0.1028(5) 1.03267(17) 0.0441(12) Uani 1 1 d . . . O6 O 0.13328(13) 0.3322(4) 1.04255(17) 0.0405(11) Uani 1 1 d . . . O7 O 0.12727(12) 0.6031(4) 0.99257(15) 0.0380(11) Uani 1 1 d . . . O8 O 0.14415(13) 0.8210(4) 0.99182(17) 0.0409(11) Uani 1 1 d . . . O9 O 0.14520(13) 0.1235(5) 0.95670(16) 0.0486(13) Uani 1 1 d . . . O10 O 0.15606(13) 0.3508(5) 0.96746(16) 0.0459(12) Uani 1 1 d . . . O11 O -0.26553(14) 0.3466(5) 0.54278(17) 0.0531(14) Uani 1 1 d . . . O12 O -0.25456(12) 0.1209(4) 0.54998(16) 0.0396(11) Uani 1 1 d . . . O1W O 0.20912(13) -0.0834(5) 0.98236(16) 0.0459(12) Uani 1 1 d . . . H1W H 0.1944 -0.1207 0.9576 0.069 Uiso 1 1 d R . . H2W H 0.2307 -0.0340 0.9872 0.069 Uiso 1 1 d R . . O2W O 0.16534(15) -0.1246(5) 1.09502(19) 0.0534(13) Uani 1 1 d . . . H4W H 0.1602 -0.2188 1.0914 0.080 Uiso 1 1 d R . . H3W H 0.1393 -0.0903 1.0791 0.080 Uiso 1 1 d R . . O3W O 0.20217(13) 0.6041(4) 0.98767(16) 0.0416(11) Uani 1 1 d . . . H6W H 0.2109 0.7073 0.9971 0.062 Uiso 1 1 d R . . H5W H 0.1907 0.6448 0.9583 0.062 Uiso 1 1 d R . . O4W O 0.16185(13) 0.5796(4) 1.09920(15) 0.0367(10) Uani 1 1 d . . . H8W H 0.1735 0.6014 1.1318 0.055 Uiso 1 1 d R . . H7W H 0.1453 0.5222 1.0979 0.055 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.031(4) 0.028(4) 0.033(4) 0.000(3) 0.010(3) 0.001(3) C2 0.029(4) 0.021(3) 0.043(4) -0.003(3) 0.015(3) -0.005(3) C3 0.0340(18) 0.0251(17) 0.0273(17) 0.0005(15) 0.0080(15) 0.0016(15) C4 0.0334(17) 0.0247(15) 0.0268(15) 0.0001(13) 0.0089(13) 0.0014(14) C5 0.0327(16) 0.0247(14) 0.0262(15) 0.0002(12) 0.0098(13) 0.0010(13) C6 0.0351(17) 0.0257(15) 0.0282(16) -0.0007(13) 0.0070(13) 0.0015(14) C7 0.0364(19) 0.0261(17) 0.0294(17) -0.0018(15) 0.0055(15) 0.0018(16) C8 0.0314(18) 0.0246(16) 0.0254(16) 0.0005(14) 0.0110(14) 0.0009(15) C9 0.0345(18) 0.0364(18) 0.0279(17) 0.0031(15) 0.0114(15) -0.0006(15) C10 0.0356(16) 0.0372(16) 0.0288(16) 0.0044(13) 0.0109(13) -0.0014(13) C11 0.0367(17) 0.0390(17) 0.0307(16) 0.0057(14) 0.0109(14) -0.0013(14) C12 0.0378(19) 0.0402(19) 0.0316(18) 0.0068(16) 0.0113(16) -0.0010(16) C13 0.0388(19) 0.0393(19) 0.0321(18) 0.0045(16) 0.0054(16) -0.0034(16) C14 0.0373(17) 0.0381(17) 0.0302(16) 0.0048(14) 0.0082(14) -0.0030(14) C15 0.0272(18) 0.0333(18) 0.055(2) 0.0060(17) 0.0171(17) -0.0019(16) C16 0.0292(17) 0.0344(16) 0.059(2) 0.0060(15) 0.0139(15) -0.0021(14) C17 0.0303(17) 0.0354(17) 0.061(2) 0.0078(16) 0.0122(16) -0.0032(15) C18 0.0310(19) 0.0361(19) 0.063(2) 0.0085(18) 0.0111(18) -0.0041(17) C19 0.0332(19) 0.0366(19) 0.065(2) 0.0047(18) 0.0080(18) -0.0002(17) C20 0.0318(18) 0.0358(17) 0.063(2) 0.0052(16) 0.0099(16) -0.0013(15) C21 0.0350(19) 0.0383(18) 0.0252(17) -0.0012(16) 0.0097(15) -0.0008(16) C22 0.0369(18) 0.0387(16) 0.0267(16) -0.0011(14) 0.0074(13) -0.0011(14) C23 0.0386(18) 0.0396(17) 0.0286(16) -0.0009(15) 0.0048(14) -0.0022(15) C24 0.040(2) 0.0410(19) 0.0298(18) -0.0013(16) 0.0031(16) -0.0029(17) C25 0.0389(18) 0.0389(17) 0.0286(16) -0.0012(15) 0.0051(14) -0.0003(15) C26 0.040(2) 0.0391(19) 0.0300(18) -0.0006(16) 0.0036(16) 0.0004(17) C27 0.037(2) 0.0378(19) 0.058(2) 0.0115(18) -0.0038(18) -0.0062(17) C28 0.0358(19) 0.0359(17) 0.056(2) 0.0109(16) -0.0020(16) -0.0058(15) C29 0.0333(18) 0.0327(16) 0.052(2) 0.0088(15) 0.0012(15) -0.0051(14) C30 0.031(2) 0.0308(18) 0.048(2) 0.0073(17) 0.0045(16) -0.0041(16) C31 0.0348(19) 0.0329(17) 0.053(2) 0.0090(16) -0.0014(16) -0.0054(15) C32 0.036(2) 0.0329(19) 0.054(2) 0.0091(18) -0.0026(17) -0.0049(17) C33 0.060(2) 0.061(2) 0.059(2) 0.0014(10) 0.0295(14) -0.0003(10) C34 0.0310(16) 0.0280(16) 0.0311(16) 0.0001(10) 0.0142(11) -0.0008(10) C35 0.0321(19) 0.0313(18) 0.0372(19) -0.0013(16) 0.0109(15) 0.0008(16) C36 0.0312(17) 0.0307(16) 0.0365(17) -0.0014(14) 0.0124(14) 0.0005(14) C37 0.0305(16) 0.0307(15) 0.0356(16) -0.0012(13) 0.0137(13) 0.0008(13) C38 0.0318(17) 0.0306(16) 0.0375(17) -0.0013(14) 0.0115(14) 0.0014(14) C39 0.0324(19) 0.0306(18) 0.0383(19) -0.0015(16) 0.0103(15) 0.0009(16) C40 0.0295(18) 0.0310(17) 0.0345(18) -0.0008(15) 0.0152(15) 0.0011(15) C41 0.038(4) 0.011(3) 0.035(4) 0.007(3) 0.009(3) 0.001(3) C42 0.049(4) 0.073(5) 0.053(5) -0.003(4) 0.027(4) -0.002(3) Cu1 0.0370(5) 0.0300(4) 0.0311(4) 0.0005(3) 0.0097(4) 0.0005(3) Cu2 0.0316(5) 0.0296(4) 0.0494(5) -0.0031(4) 0.0138(4) -0.0013(3) Cu3 0.0424(6) 0.0626(7) 0.0684(7) -0.0034(5) 0.0129(5) 0.0043(5) Cu4 0.0404(5) 0.0245(4) 0.0444(5) 0.0005(4) 0.0120(4) -0.0009(4) Cu5 0.0321(5) 0.0246(4) 0.0435(5) 0.0024(3) 0.0082(4) 0.0011(3) Sm1 0.01994(16) 0.01939(16) 0.01959(16) 0.00040(12) 0.00229(12) -0.00058(12) Sm2 0.02159(17) 0.01900(16) 0.02200(16) 0.00183(12) 0.00145(13) -0.00123(12) N1 0.036(3) 0.042(4) 0.042(3) -0.003(3) 0.011(3) 0.000(3) N2 0.043(4) 0.047(4) 0.030(3) 0.001(3) 0.013(3) -0.002(3) N3 0.030(3) 0.027(3) 0.029(3) -0.001(2) 0.008(2) -0.001(2) N4 0.052(4) 0.050(4) 0.028(3) 0.014(3) 0.014(3) 0.017(3) N5 0.029(3) 0.032(3) 0.065(4) 0.010(3) 0.008(3) -0.001(2) N6 0.037(3) 0.055(4) 0.024(3) 0.004(3) 0.002(3) 0.002(3) N7 0.042(4) 0.060(4) 0.061(4) 0.007(3) 0.019(3) 0.004(3) N8 0.030(3) 0.027(3) 0.040(3) 0.000(2) 0.009(3) -0.001(2) N9 0.038(4) 0.063(5) 0.041(4) -0.003(3) 0.010(3) -0.002(3) N10 0.087(7) 0.088(6) 0.095(6) 0.023(5) 0.051(6) 0.004(5) N11 0.027(3) 0.035(3) 0.056(4) 0.019(3) 0.005(3) 0.001(3) N13 0.049(4) 0.073(5) 0.053(5) -0.003(4) 0.027(4) -0.002(3) O1 0.040(3) 0.029(2) 0.031(2) -0.0007(19) 0.002(2) -0.011(2) O2 0.032(3) 0.027(2) 0.037(3) 0.011(2) 0.004(2) 0.0043(19) O3 0.045(3) 0.036(3) 0.028(2) 0.013(2) 0.008(2) 0.002(2) O4 0.058(3) 0.047(3) 0.032(3) -0.016(2) 0.002(2) 0.001(3) O5 0.031(3) 0.037(3) 0.052(3) -0.008(2) 0.013(2) 0.001(2) O6 0.028(2) 0.039(3) 0.046(3) 0.005(2) 0.013(2) -0.006(2) O7 0.025(2) 0.030(2) 0.037(2) 0.010(2) -0.0004(19) 0.0038(19) O8 0.030(3) 0.028(2) 0.046(3) -0.003(2) 0.006(2) -0.006(2) O9 0.038(3) 0.045(3) 0.035(3) 0.019(2) -0.002(2) -0.001(2) O10 0.035(3) 0.055(3) 0.027(2) -0.017(2) 0.001(2) -0.001(2) O11 0.038(3) 0.054(3) 0.040(3) -0.010(2) 0.001(2) 0.020(2) O12 0.032(3) 0.034(3) 0.042(3) -0.001(2) 0.011(2) -0.007(2) O1W 0.040(3) 0.055(3) 0.037(3) -0.008(2) 0.015(2) -0.005(2) O2W 0.065(4) 0.038(3) 0.070(3) 0.014(3) 0.043(3) 0.005(2) O3W 0.045(3) 0.037(3) 0.039(3) 0.013(2) 0.019(2) 0.002(2) O4W 0.041(3) 0.041(3) 0.025(2) -0.009(2) 0.015(2) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.153(8) . ? C1 Cu1 1.895(6) 1_565 ? C2 N2 1.139(8) . ? C2 Cu2 1.896(6) . ? C3 N3 1.334(7) . ? C3 C4 1.373(8) . ? C3 H4 0.9300 . ? C4 C5 1.389(8) . ? C4 H3 0.9300 . ? C5 C6 1.371(8) . ? C5 C8 1.502(8) . ? C6 C7 1.381(8) . ? C6 H6 0.9300 . ? C7 N3 1.319(7) . ? C7 H5 0.9300 . ? C8 O1 1.235(7) . ? C8 O2 1.251(7) . ? C9 O3 1.240(7) . ? C9 O4 1.240(7) . ? C9 C10 1.510(9) . ? C10 C11 1.362(9) . ? C10 C14 1.372(9) . ? C11 C12 1.388(8) . ? C11 H10 0.9300 . ? C12 N4 1.305(8) . ? C12 H9 0.9300 . ? C13 N4 1.335(8) . ? C13 C14 1.382(9) . ? C13 H8 0.9300 . ? C14 H11 0.9300 . ? C15 O6 1.245(7) . ? C15 O5 1.251(7) . ? C15 C16 1.512(9) . ? C16 C17 1.355(9) . ? C16 C20 1.372(9) . ? C17 C18 1.395(9) . ? C17 H16 0.9300 . ? C18 N5 1.311(8) . ? C18 H19 0.9300 . ? C19 N5 1.322(8) . ? C19 C20 1.386(9) . ? C19 H18 0.9300 . ? C20 H17 0.9300 . ? C21 O9 1.235(7) . ? C21 O10 1.245(7) . ? C21 C22 1.512(9) . ? C22 C25 1.366(9) . ? C22 C23 1.373(9) . ? C23 C24 1.362(9) . ? C23 H22 0.9300 . ? C24 N6 1.348(8) . ? C24 H23 0.9300 . ? C25 C26 1.390(8) . ? C25 H25 0.9300 . ? C26 N6 1.325(8) . ? C26 H24 0.9300 . ? C27 N11 1.339(8) . ? C27 C28 1.378(9) . ? C27 H29 0.9300 . ? C28 C29 1.373(9) . ? C28 H28 0.9300 . ? C29 C31 1.351(9) . ? C29 C30 1.498(9) . ? C30 O7 1.242(7) . ? C30 O8 1.246(7) . ? C31 C32 1.377(9) . ? C31 H31 0.9300 . ? C32 N11 1.298(8) . ? C32 H30 0.9300 . ? C33 N10 1.131(11) . ? C34 N7 1.148(8) . ? C34 Cu4 1.865(6) . ? C35 N8 1.334(8) . ? C35 C36 1.369(8) . ? C35 H35 0.9300 . ? C36 C37 1.390(8) . ? C36 H36 0.9300 . ? C37 C38 1.387(8) . ? C37 C40 1.498(9) . ? C38 C39 1.379(8) . ? C38 H37 0.9300 . ? C39 N8 1.328(8) . ? C39 H34 0.9300 . ? C40 O11 1.238(7) . ? C40 O12 1.248(7) . ? C41 N9 1.133(8) . ? C41 Cu4 1.861(6) 1_565 ? C42 N13 1.125(13) 2_556 ? C42 C42 1.125(13) 2_556 ? C42 Cu3 1.880(6) . ? Cu1 C1 1.895(6) 1_545 ? Cu1 N2 1.940(6) . ? Cu1 N3 2.136(5) . ? Cu2 N1 1.928(6) . ? Cu2 N5 2.127(6) 8_566 ? Cu3 N10 1.898(9) . ? Cu3 Cu5 2.7236(14) . ? Cu4 C41 1.861(6) 1_545 ? Cu4 N8 2.132(5) . ? Cu5 N7 1.909(7) . ? Cu5 N9 1.925(7) . ? Cu5 N11 2.094(5) . ? Sm1 O1 2.346(4) . ? Sm1 O10 2.362(4) . ? Sm1 O7 2.398(4) . ? Sm1 O12 2.409(4) 8_556 ? Sm1 O6 2.422(4) . ? Sm1 O3 2.444(4) . ? Sm1 O4W 2.502(4) . ? Sm1 O3W 2.513(4) . ? Sm2 O8 2.324(4) 1_545 ? Sm2 O4 2.344(4) . ? Sm2 O11 2.362(5) 8_556 ? Sm2 O2 2.368(4) 1_545 ? Sm2 O5 2.400(4) . ? Sm2 O9 2.435(4) . ? Sm2 O1W 2.524(4) . ? Sm2 O2W 2.534(4) . ? N5 Cu2 2.127(6) 8_465 ? O2 Sm2 2.368(4) 1_565 ? O8 Sm2 2.324(4) 1_565 ? O11 Sm2 2.362(4) 8_455 ? O12 Sm1 2.409(4) 8_455 ? O1W H1W 0.7661 . ? O1W H2W 0.9086 . ? O2W H4W 0.9218 . ? O2W H3W 0.9341 . ? O3W H6W 1.0395 . ? O3W H5W 0.8651 . ? O4W H8W 0.8817 . ? O4W H7W 0.8335 . ? 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 N1 C1 Cu1 176.0(6) . 1_565 ? N2 C2 Cu2 176.8(6) . . ? N3 C3 C4 123.6(6) . . ? N3 C3 H4 118.2 . . ? C4 C3 H4 118.2 . . ? C3 C4 C5 119.4(6) . . ? C3 C4 H3 120.3 . . ? C5 C4 H3 120.3 . . ? C6 C5 C4 116.8(6) . . ? C6 C5 C8 122.3(5) . . ? C4 C5 C8 120.8(5) . . ? C5 C6 C7 119.7(6) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? N3 C7 C6 123.8(6) . . ? N3 C7 H5 118.1 . . ? C6 C7 H5 118.1 . . ? O1 C8 O2 124.8(6) . . ? O1 C8 C5 117.8(5) . . ? O2 C8 C5 117.4(5) . . ? O3 C9 O4 126.1(6) . . ? O3 C9 C10 117.8(6) . . ? O4 C9 C10 116.1(6) . . ? C11 C10 C14 118.1(6) . . ? C11 C10 C9 121.1(6) . . ? C14 C10 C9 120.8(6) . . ? C10 C11 C12 118.9(6) . . ? C10 C11 H10 120.5 . . ? C12 C11 H10 120.5 . . ? N4 C12 C11 123.7(6) . . ? N4 C12 H9 118.2 . . ? C11 C12 H9 118.2 . . ? N4 C13 C14 122.6(7) . . ? N4 C13 H8 118.7 . . ? C14 C13 H8 118.7 . . ? C10 C14 C13 119.2(6) . . ? C10 C14 H11 120.4 . . ? C13 C14 H11 120.4 . . ? O6 C15 O5 126.2(6) . . ? O6 C15 C16 118.3(6) . . ? O5 C15 C16 115.4(6) . . ? C17 C16 C20 116.6(7) . . ? C17 C16 C15 121.4(6) . . ? C20 C16 C15 122.0(6) . . ? C16 C17 C18 119.4(7) . . ? C16 C17 H16 120.3 . . ? C18 C17 H16 120.3 . . ? N5 C18 C17 123.9(6) . . ? N5 C18 H19 118.0 . . ? C17 C18 H19 118.0 . . ? N5 C19 C20 122.7(7) . . ? N5 C19 H18 118.6 . . ? C20 C19 H18 118.6 . . ? C16 C20 C19 120.3(7) . . ? C16 C20 H17 119.9 . . ? C19 C20 H17 119.9 . . ? O9 C21 O10 126.8(6) . . ? O9 C21 C22 116.8(6) . . ? O10 C21 C22 116.4(6) . . ? C25 C22 C23 117.6(6) . . ? C25 C22 C21 121.8(6) . . ? C23 C22 C21 120.6(6) . . ? C24 C23 C22 120.6(7) . . ? C24 C23 H22 119.7 . . ? C22 C23 H22 119.7 . . ? N6 C24 C23 121.9(6) . . ? N6 C24 H23 119.1 . . ? C23 C24 H23 119.1 . . ? C22 C25 C26 119.7(6) . . ? C22 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? N6 C26 C25 122.2(6) . . ? N6 C26 H24 118.9 . . ? C25 C26 H24 118.9 . . ? N11 C27 C28 122.0(7) . . ? N11 C27 H29 119.0 . . ? C28 C27 H29 119.0 . . ? C29 C28 C27 120.1(7) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C31 C29 C28 116.7(6) . . ? C31 C29 C30 122.9(6) . . ? C28 C29 C30 120.0(6) . . ? O7 C30 O8 124.2(6) . . ? O7 C30 C29 117.3(6) . . ? O8 C30 C29 118.5(6) . . ? C29 C31 C32 120.0(7) . . ? C29 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? N11 C32 C31 123.9(6) . . ? N11 C32 H30 118.1 . . ? C31 C32 H30 118.1 . . ? N7 C34 Cu4 176.5(6) . . ? N8 C35 C36 123.2(6) . . ? N8 C35 H35 118.4 . . ? C36 C35 H35 118.4 . . ? C35 C36 C37 119.3(6) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C38 C37 C36 117.4(6) . . ? C38 C37 C40 121.8(6) . . ? C36 C37 C40 120.5(6) . . ? C39 C38 C37 119.1(6) . . ? C39 C38 H37 120.4 . . ? C37 C38 H37 120.4 . . ? N8 C39 C38 123.1(6) . . ? N8 C39 H34 118.5 . . ? C38 C39 H34 118.5 . . ? O11 C40 O12 124.5(6) . . ? O11 C40 C37 117.7(6) . . ? O12 C40 C37 117.6(5) . . ? N9 C41 Cu4 166.6(6) . 1_565 ? N13 C42 C42 0.0(11) 2_556 2_556 ? N13 C42 Cu3 173.8(6) 2_556 . ? C42 C42 Cu3 173.8(6) 2_556 . ? C1 Cu1 N2 147.9(3) 1_545 . ? C1 Cu1 N3 108.7(2) 1_545 . ? N2 Cu1 N3 103.3(2) . . ? C2 Cu2 N1 149.2(3) . . ? C2 Cu2 N5 108.1(2) . 8_566 ? N1 Cu2 N5 102.7(2) . 8_566 ? C42 Cu3 N10 155.4(3) . . ? C42 Cu3 Cu5 79.9(2) . . ? N10 Cu3 Cu5 123.6(3) . . ? C41 Cu4 C34 155.7(3) 1_545 . ? C41 Cu4 N8 99.7(2) 1_545 . ? C34 Cu4 N8 104.6(2) . . ? N7 Cu5 N9 153.8(3) . . ? N7 Cu5 N11 101.5(2) . . ? N9 Cu5 N11 103.7(2) . . ? N7 Cu5 Cu3 65.1(2) . . ? N9 Cu5 Cu3 93.14(18) . . ? N11 Cu5 Cu3 129.55(18) . . ? O1 Sm1 O10 146.07(17) . . ? O1 Sm1 O7 102.45(15) . . ? O10 Sm1 O7 76.12(15) . . ? O1 Sm1 O12 80.73(16) . 8_556 ? O10 Sm1 O12 80.92(15) . 8_556 ? O7 Sm1 O12 142.22(15) . 8_556 ? O1 Sm1 O6 139.90(16) . . ? O10 Sm1 O6 73.44(16) . . ? O7 Sm1 O6 75.96(15) . . ? O12 Sm1 O6 125.19(15) 8_556 . ? O1 Sm1 O3 76.55(14) . . ? O10 Sm1 O3 124.56(16) . . ? O7 Sm1 O3 143.80(15) . . ? O12 Sm1 O3 73.91(15) 8_556 . ? O6 Sm1 O3 82.18(15) . . ? O1 Sm1 O4W 72.17(15) . . ? O10 Sm1 O4W 134.81(15) . . ? O7 Sm1 O4W 70.42(14) . . ? O12 Sm1 O4W 142.63(14) 8_556 . ? O6 Sm1 O4W 69.67(15) . . ? O3 Sm1 O4W 75.09(14) . . ? O1 Sm1 O3W 74.00(15) . . ? O10 Sm1 O3W 72.90(16) . . ? O7 Sm1 O3W 75.34(14) . . ? O12 Sm1 O3W 69.39(14) 8_556 . ? O6 Sm1 O3W 139.88(15) . . ? O3 Sm1 O3W 135.78(15) . . ? O4W Sm1 O3W 124.23(14) . . ? O8 Sm2 O4 144.32(18) 1_545 . ? O8 Sm2 O11 140.29(17) 1_545 8_556 ? O4 Sm2 O11 74.87(19) . 8_556 ? O8 Sm2 O2 95.77(15) 1_545 1_545 ? O4 Sm2 O2 81.02(16) . 1_545 ? O11 Sm2 O2 82.29(15) 8_556 1_545 ? O8 Sm2 O5 86.05(15) 1_545 . ? O4 Sm2 O5 74.37(16) . . ? O11 Sm2 O5 121.02(17) 8_556 . ? O2 Sm2 O5 138.75(16) 1_545 . ? O8 Sm2 O9 81.46(15) 1_545 . ? O4 Sm2 O9 118.14(17) . . ? O11 Sm2 O9 81.21(15) 8_556 . ? O2 Sm2 O9 149.99(16) 1_545 . ? O5 Sm2 O9 71.13(17) . . ? O8 Sm2 O1W 71.79(16) 1_545 . ? O4 Sm2 O1W 139.90(17) . . ? O11 Sm2 O1W 69.09(17) 8_556 . ? O2 Sm2 O1W 77.37(15) 1_545 . ? O5 Sm2 O1W 140.41(15) . . ? O9 Sm2 O1W 73.38(16) . . ? O8 Sm2 O2W 72.28(16) 1_545 . ? O4 Sm2 O2W 72.91(18) . . ? O11 Sm2 O2W 141.54(16) 8_556 . ? O2 Sm2 O2W 72.50(16) 1_545 . ? O5 Sm2 O2W 68.90(16) . . ? O9 Sm2 O2W 133.04(16) . . ? O1W Sm2 O2W 129.69(16) . . ? C1 N1 Cu2 169.0(6) . . ? C2 N2 Cu1 173.7(5) . . ? C7 N3 C3 116.5(5) . . ? C7 N3 Cu1 121.3(4) . . ? C3 N3 Cu1 122.2(4) . . ? C12 N4 C13 117.4(6) . . ? C18 N5 C19 116.2(6) . . ? C18 N5 Cu2 121.7(5) . 8_465 ? C19 N5 Cu2 122.0(4) . 8_465 ? C26 N6 C24 118.0(5) . . ? C34 N7 Cu5 165.7(6) . . ? C39 N8 C35 117.6(5) . . ? C39 N8 Cu4 120.6(4) . . ? C35 N8 Cu4 121.7(4) . . ? C41 N9 Cu5 177.8(7) . . ? C33 N10 Cu3 178.8(9) . . ? C32 N11 C27 116.8(6) . . ? C32 N11 Cu5 119.6(4) . . ? C27 N11 Cu5 117.9(5) . . ? C8 O1 Sm1 165.9(4) . . ? C8 O2 Sm2 142.4(4) . 1_565 ? C9 O3 Sm1 129.7(4) . . ? C9 O4 Sm2 153.4(5) . . ? C15 O5 Sm2 133.1(4) . . ? C15 O6 Sm1 150.2(5) . . ? C30 O7 Sm1 136.8(4) . . ? C30 O8 Sm2 159.4(5) . 1_565 ? C21 O9 Sm2 134.5(4) . . ? C21 O10 Sm1 146.8(4) . . ? C40 O11 Sm2 148.3(5) . 8_455 ? C40 O12 Sm1 122.4(4) . 8_455 ? Sm2 O1W H1W 118.5 . . ? Sm2 O1W H2W 110.9 . . ? H1W O1W H2W 124.7 . . ? Sm2 O2W H4W 122.1 . . ? Sm2 O2W H3W 95.1 . . ? H4W O2W H3W 99.8 . . ? Sm1 O3W H6W 117.0 . . ? Sm1 O3W H5W 141.5 . . ? H6W O3W H5W 77.2 . . ? Sm1 O4W H8W 133.2 . . ? Sm1 O4W H7W 103.7 . . ? H8W O4W H7W 98.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W O8 0.77 2.71 2.847(6) 92.4 1_545 O1W H1W O3W 0.77 2.76 3.027(6) 102.7 1_545 O1W H2W O12 0.91 2.34 3.126(6) 145.0 2_556 O1W H2W O3W 0.91 2.42 3.100(6) 131.9 7_557 O2W H4W O4W 0.92 1.95 2.852(6) 166.0 1_545 O2W H3W O5 0.93 2.23 2.793(6) 118.2 . O2W H3W N1 0.93 2.66 3.285(7) 124.7 4_537 O3W H6W O1W 1.04 2.05 3.027(6) 154.6 1_565 O4W H8W N4 0.88 1.82 2.695(6) 172.5 4_557 O4W H7W O6 0.83 2.37 2.813(6) 114.3 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.324 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.125 #============================================================ # Attachment 'revised_CIFs1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 722464' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C83 H64 Cu10 N23 Nd4 O32' _chemical_formula_sum 'C83 H64 Cu10 N23 Nd4 O32' _chemical_formula_weight 3108.04 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' Cu Cu 0.3201 1.2651 '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' Nd Nd -0.1943 3.0179 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.6646(17) _cell_length_b 9.5625(9) _cell_length_c 30.623(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.761(4) _cell_angle_gamma 90.00 _cell_volume 4926.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4762 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 25.26 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3018.0 _exptl_absorpt_coefficient_mu 4.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2494 _exptl_absorpt_correction_T_max 0.3084 _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 APEX-II area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24238 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8664 _reflns_number_gt 6621 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'Apex2 (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-XP (Bruker, 2004)' _computing_publication_material SHELXL-97 _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. The cyanice groups are disordered with respect to the C and N termini. So the 'SIMU' and 'ISOR' were used in the restrain refinements for the partial C and N atoms. ; _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^)+(0.0373P)^2^+22.9901P] 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 8664 _refine_ls_number_parameters 685 _refine_ls_number_restraints 186 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C28 C 0.3067(4) 0.6171(8) 0.0741(3) 0.0351(10) Uani 1 1 d U . . H28 H 0.2899 0.7065 0.0787 0.042 Uiso 1 1 calc R . . C29 C 0.3783(4) 0.6022(8) 0.0641(2) 0.0345(9) Uani 1 1 d U . . H29 H 0.4090 0.6802 0.0630 0.041 Uiso 1 1 calc R . . C25 C 0.4029(4) 0.4706(8) 0.0560(3) 0.0334(8) Uani 1 1 d U . . C26 C 0.3544(4) 0.3574(8) 0.0573(2) 0.0332(9) Uani 1 1 d U . . H26 H 0.3681 0.2675 0.0509 0.040 Uiso 1 1 calc R . . C27 C 0.2853(4) 0.3817(8) 0.0681(2) 0.0333(10) Uani 1 1 d U . . H27 H 0.2533 0.3054 0.0692 0.040 Uiso 1 1 calc R . . C24 C 0.4849(4) 0.4477(8) 0.0521(3) 0.0327(9) Uani 1 1 d U . . C3 C 1.1266(4) 0.3523(8) 0.0994(3) 0.0371(19) Uani 1 1 d . . . C23 C 0.7705(5) 0.4074(9) 0.1665(3) 0.0463(11) Uani 1 1 d U . . C30 C 0.5410(4) 0.4370(8) 0.1607(3) 0.0347(10) Uani 1 1 d U . . C5 C 1.2029(4) 0.7406(7) 0.2205(3) 0.0279(17) Uani 1 1 d . . . C36 C 0.3224(4) 0.0527(8) 0.1560(3) 0.0327(10) Uani 1 1 d U . . H36 H 0.2900 0.1304 0.1544 0.039 Uiso 1 1 calc R . . C40 C 0.3583(4) -0.1680(8) 0.1804(3) 0.0335(10) Uani 1 1 d U . . H40 H 0.3506 -0.2480 0.1958 0.040 Uiso 1 1 calc R . . C19 C 0.9071(4) 0.2991(9) 0.1965(3) 0.0489(11) Uani 1 1 d U . . H19 H 0.8839 0.2121 0.1972 0.059 Uiso 1 1 calc R . . C18 C 0.9883(4) 0.3100(9) 0.2074(3) 0.0494(12) Uani 1 1 d U . . H18 H 1.0182 0.2286 0.2153 0.059 Uiso 1 1 calc R . . C20 C 0.8603(5) 0.4147(9) 0.1847(3) 0.0483(10) Uani 1 1 d U . . C32 C 0.5093(4) 0.2558(8) 0.2114(3) 0.0375(9) Uani 1 1 d U . . H32 H 0.5527 0.2033 0.2098 0.045 Uiso 1 1 calc R . . C31 C 0.4896(4) 0.3771(8) 0.1872(3) 0.0359(8) Uani 1 1 d U . . C35 C 0.4208(4) 0.4443(8) 0.1879(3) 0.0367(9) Uani 1 1 d U . . H35 H 0.4039 0.5242 0.1703 0.044 Uiso 1 1 calc R . . C34 C 0.3777(4) 0.3932(8) 0.2146(3) 0.0376(10) Uani 1 1 d U . . H34 H 0.3312 0.4393 0.2144 0.045 Uiso 1 1 calc R . . C33 C 0.4635(4) 0.2118(8) 0.2387(3) 0.0387(10) Uani 1 1 d U . . H33 H 0.4784 0.1311 0.2562 0.046 Uiso 1 1 calc R . . C12 C 0.7277(5) 0.4433(9) 0.0566(3) 0.0431(10) Uani 1 1 d U . . C13 C 0.8004(5) 0.4606(9) 0.0408(3) 0.0439(9) Uani 1 1 d U . . C17 C 0.8381(5) 0.5880(9) 0.0443(3) 0.0461(10) Uani 1 1 d U . . H17 H 0.8181 0.6659 0.0552 0.055 Uiso 1 1 calc R . . C22 C 0.9820(5) 0.5417(9) 0.1995(3) 0.0533(12) Uani 1 1 d U . . H22 H 1.0071 0.6281 0.2017 0.064 Uiso 1 1 calc R . . C21 C 0.8991(5) 0.5385(9) 0.1878(3) 0.0516(11) Uani 1 1 d U . . H21 H 0.8704 0.6216 0.1821 0.062 Uiso 1 1 calc R . . C14 C 0.8313(5) 0.3521(9) 0.0231(3) 0.0438(10) Uani 1 1 d U . . H14 H 0.8063 0.2654 0.0192 0.053 Uiso 1 1 calc R . . C15 C 0.8991(5) 0.3702(9) 0.0110(3) 0.0440(11) Uani 1 1 d U . . H15 H 0.9198 0.2942 -0.0006 0.053 Uiso 1 1 calc R . . C6 C 0.9452(5) 0.1055(10) 0.1052(4) 0.0641(14) Uani 1 1 d U . . H6 H 0.9576 0.1872 0.0924 0.077 Uiso 1 1 calc R . . C9 C 0.8658(5) 0.0795(10) 0.1004(4) 0.0643(13) Uani 1 1 d U . . H9 H 0.8269 0.1414 0.0840 0.077 Uiso 1 1 calc R . . C7 C 0.9824(5) -0.0797(11) 0.1468(4) 0.0711(14) Uani 1 1 d U . . H7 H 1.0227 -0.1358 0.1651 0.085 Uiso 1 1 calc R . . C8 C 0.9054(5) -0.1142(11) 0.1438(4) 0.0689(13) Uani 1 1 d U . . H8 H 0.8952 -0.1932 0.1588 0.083 Uiso 1 1 calc R . . C10 C 0.8454(5) -0.0346(10) 0.1193(4) 0.0646(13) Uani 1 1 d U . . C37 C 0.3815(4) 0.0595(8) 0.1350(3) 0.0322(9) Uani 1 1 d U . . H37 H 0.3873 0.1394 0.1190 0.039 Uiso 1 1 calc R . . C39 C 0.4197(4) -0.1687(8) 0.1612(3) 0.0329(9) Uani 1 1 d U . . H39 H 0.4523 -0.2466 0.1640 0.039 Uiso 1 1 calc R . . C11 C 0.7600(5) -0.0709(10) 0.1124(4) 0.0626(14) Uani 1 1 d U . . C38 C 0.4314(4) -0.0519(7) 0.1379(3) 0.0318(8) Uani 1 1 d U . . C41 C 0.4987(4) -0.0483(8) 0.1168(3) 0.0312(9) Uani 1 1 d U . . C2 C 1.1438(5) -0.2725(8) 0.1010(3) 0.0338(18) Uani 1 1 d . . . C4 C 1.1863(4) 0.1191(9) 0.2151(2) 0.0326(17) Uani 1 1 d . . . C16 C 0.9061(5) 0.5982(10) 0.0311(3) 0.0477(11) Uani 1 1 d U . . H16 H 0.9317 0.6842 0.0337 0.057 Uiso 1 1 calc R . . C1 C 1.3087(6) -0.0033(11) 0.0211(3) 0.056(2) Uani 1 1 d U . . Cu2 Cu 1.15696(6) 0.53681(10) 0.09702(4) 0.0448(3) Uani 1 1 d . . . Cu3 Cu 1.11080(6) 0.03753(10) 0.11189(4) 0.0470(3) Uani 1 1 d . . . Cu1 Cu 1.15062(5) 0.43497(10) 0.21805(4) 0.0401(3) Uani 1 1 d . . . Cu5 Cu 0.21623(5) -0.06630(9) 0.20816(3) 0.0356(2) Uani 1 1 d . . . Cu4 Cu 1.14392(7) 0.01232(16) 0.03062(5) 0.0792(4) Uani 1 1 d . . . N10 N 0.2614(4) 0.5082(7) 0.0772(2) 0.0387(16) Uani 1 1 d . . . N12 N 0.3099(3) -0.0610(6) 0.1784(2) 0.0307(14) Uani 1 1 d . . . N7 N 1.0264(4) 0.4278(7) 0.2075(3) 0.0482(19) Uani 1 1 d . . . N9 N 1.0029(4) 0.0245(7) 0.1263(3) 0.0495(19) Uani 1 1 d . . . N11 N 0.3992(4) 0.2807(8) 0.2407(2) 0.0476(18) Uani 1 1 d . . . N8 N 0.9362(4) 0.4909(9) 0.0151(2) 0.052(2) Uani 1 1 d . . . N6 N 1.1876(4) 0.6266(10) 0.2218(3) 0.060(2) Uani 1 1 d . . . N3 N 1.1375(4) -0.1572(10) 0.1046(3) 0.065(2) Uani 1 1 d . . . N5 N 1.1751(3) 0.2374(7) 0.2201(2) 0.0405(16) Uani 1 1 d . . . N4 N 1.1212(4) 0.2345(9) 0.1017(2) 0.053(2) Uani 1 1 d . . . N2 N 1.0337(4) 0.0053(11) 0.0072(3) 0.060(2) Uani 0.50 1 d P . . C2' C 1.0337(4) 0.0053(11) 0.0072(3) 0.060(2) Uani 0.50 1 d P . . N1 N 1.2474(6) 0.0079(12) 0.0263(3) 0.098(3) Uani 1 1 d . . . Nd1 Nd 0.62092(2) 0.20076(4) 0.094748(13) 0.02291(11) Uani 1 1 d . . . Nd2 Nd 0.63202(2) -0.33390(4) 0.116374(13) 0.02327(11) Uani 1 1 d . . . O9 O 0.5032(3) 0.3260(5) 0.04287(16) 0.0313(11) Uani 1 1 d . . . O10 O 0.5302(3) 0.5504(5) 0.05928(16) 0.0353(12) Uani 1 1 d . . . O3 O 0.7048(3) 0.5504(7) 0.0716(2) 0.0607(18) Uani 1 1 d . . . O1 O 0.7412(3) 0.2907(5) 0.15183(18) 0.0373(12) Uani 1 1 d . . . O11 O 0.5473(3) 0.5660(5) 0.15987(17) 0.0338(12) Uani 1 1 d . . . O12 O 0.5747(3) 0.3530(5) 0.14092(16) 0.0355(12) Uani 1 1 d . . . O2 O 0.7334(3) 0.5184(6) 0.16664(19) 0.0416(13) Uani 1 1 d . . . O4 O 0.6974(3) 0.3255(6) 0.0532(2) 0.0512(16) Uani 1 1 d . . . O6 O 0.7474(3) -0.1872(6) 0.12638(19) 0.0440(14) Uani 1 1 d . . . O5 O 0.7080(3) 0.0153(5) 0.09281(18) 0.0388(13) Uani 1 1 d . . . O7 O 0.5396(3) -0.1541(5) 0.11994(18) 0.0385(13) Uani 1 1 d . . . O8 O 0.5088(3) 0.0638(5) 0.09757(18) 0.0351(12) Uani 1 1 d . . . O2W O 0.5791(3) 0.0959(6) 0.01525(18) 0.0460(14) Uani 1 1 d . . . H3W H 0.6157 0.0924 0.0046 0.069 Uiso 1 1 d R . . H4W H 0.5398 0.1125 -0.0062 0.069 Uiso 1 1 d R . . O1W O 0.6570(3) 0.0768(5) 0.17500(17) 0.0403(13) Uani 1 1 d . . . H2W H 0.6999 0.1137 0.1869 0.060 Uiso 1 1 d R . . H1W H 0.6654 -0.0068 0.1782 0.060 Uiso 1 1 d R . . O4W O 0.5971(3) -0.2086(6) 0.04008(17) 0.0506(16) Uani 1 1 d . . . H7W H 0.5760 -0.2467 0.0156 0.076 Uiso 1 1 d R . . H8W H 0.6142 -0.1348 0.0332 0.076 Uiso 1 1 d R . . O3W O 0.6767(3) -0.2219(5) 0.19510(16) 0.0355(12) Uani 1 1 d . . . H5W H 0.7183 -0.2635 0.2076 0.053 Uiso 1 1 d R . . H6W H 0.6520 -0.2276 0.2139 0.053 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C28 0.0302(19) 0.029(2) 0.044(2) 0.0045(18) 0.0079(18) 0.0013(17) C29 0.0300(18) 0.0281(19) 0.043(2) 0.0049(16) 0.0080(16) 0.0006(16) C25 0.0296(17) 0.0276(18) 0.0414(19) 0.0057(15) 0.0085(15) 0.0000(15) C26 0.0297(18) 0.0273(19) 0.042(2) 0.0059(16) 0.0095(16) -0.0004(15) C27 0.0299(19) 0.027(2) 0.042(2) 0.0060(18) 0.0101(17) -0.0009(17) C24 0.0292(19) 0.027(2) 0.040(2) 0.0060(17) 0.0083(17) -0.0001(17) C3 0.036(4) 0.018(4) 0.062(6) 0.005(4) 0.022(4) -0.005(3) C23 0.027(2) 0.029(2) 0.084(3) 0.004(2) 0.017(2) 0.0009(18) C30 0.032(2) 0.036(2) 0.042(2) 0.0074(17) 0.0196(18) 0.0018(18) C5 0.034(4) 0.007(3) 0.048(5) 0.002(3) 0.019(3) -0.008(3) C36 0.030(2) 0.027(2) 0.046(2) 0.0052(17) 0.0181(18) 0.0047(17) C40 0.0319(19) 0.028(2) 0.046(2) 0.0064(17) 0.0197(17) 0.0048(17) C19 0.0285(19) 0.030(2) 0.087(3) 0.003(2) 0.015(2) 0.0012(17) C18 0.029(2) 0.030(2) 0.087(3) 0.003(2) 0.015(2) 0.0017(19) C20 0.0279(18) 0.030(2) 0.086(3) 0.0035(19) 0.0160(19) 0.0010(16) C32 0.0353(19) 0.038(2) 0.044(2) 0.0087(17) 0.0182(17) 0.0014(17) C31 0.0335(18) 0.037(2) 0.043(2) 0.0078(16) 0.0194(16) 0.0014(16) C35 0.0339(19) 0.038(2) 0.044(2) 0.0079(17) 0.0200(17) 0.0013(17) C34 0.034(2) 0.039(2) 0.045(2) 0.0077(18) 0.0200(18) 0.0010(18) C33 0.037(2) 0.038(2) 0.045(2) 0.0098(18) 0.0174(18) 0.0008(18) C12 0.039(2) 0.047(2) 0.054(2) 0.000(2) 0.0293(19) -0.0019(19) C13 0.039(2) 0.047(2) 0.056(2) -0.0007(18) 0.0293(18) -0.0020(17) C17 0.041(2) 0.048(2) 0.059(2) -0.0013(19) 0.0288(19) -0.0030(18) C22 0.031(2) 0.032(2) 0.093(3) 0.004(2) 0.013(2) 0.0013(19) C21 0.0299(19) 0.031(2) 0.091(3) 0.004(2) 0.014(2) 0.0014(17) C14 0.040(2) 0.047(2) 0.055(2) -0.0008(19) 0.0294(18) -0.0009(18) C15 0.040(2) 0.047(2) 0.055(2) -0.001(2) 0.029(2) 0.000(2) C6 0.030(2) 0.057(3) 0.109(4) 0.041(3) 0.027(2) 0.006(2) C9 0.030(2) 0.058(3) 0.109(4) 0.041(2) 0.026(2) 0.006(2) C7 0.034(2) 0.063(3) 0.115(4) 0.044(3) 0.020(2) 0.006(2) C8 0.032(2) 0.061(3) 0.113(4) 0.044(2) 0.022(2) 0.005(2) C10 0.030(2) 0.058(3) 0.109(3) 0.041(2) 0.026(2) 0.0060(19) C37 0.0297(18) 0.0266(19) 0.045(2) 0.0051(16) 0.0183(16) 0.0043(15) C39 0.0308(18) 0.0272(19) 0.046(2) 0.0059(16) 0.0191(16) 0.0048(15) C11 0.028(2) 0.057(3) 0.107(4) 0.040(3) 0.027(2) 0.006(2) C38 0.0295(17) 0.0267(18) 0.044(2) 0.0051(15) 0.0187(15) 0.0042(14) C41 0.0288(19) 0.027(2) 0.043(2) 0.0048(17) 0.0186(17) 0.0032(16) C2 0.042(5) 0.006(4) 0.053(5) -0.004(3) 0.015(4) 0.006(3) C4 0.023(4) 0.039(5) 0.038(4) 0.000(4) 0.013(3) 0.000(3) C16 0.042(2) 0.049(2) 0.060(2) -0.001(2) 0.028(2) -0.004(2) C1 0.055(3) 0.057(3) 0.056(3) -0.0023(10) 0.0183(12) 0.0008(10) Cu2 0.0421(6) 0.0290(6) 0.0653(7) 0.0029(5) 0.0192(5) 0.0025(5) Cu3 0.0291(5) 0.0307(6) 0.0842(8) 0.0009(5) 0.0217(5) -0.0010(4) Cu1 0.0296(5) 0.0265(5) 0.0623(7) 0.0000(4) 0.0114(5) -0.0008(4) Cu5 0.0322(5) 0.0280(5) 0.0519(6) 0.0008(4) 0.0207(5) 0.0014(4) Cu4 0.0357(6) 0.0821(10) 0.1181(12) -0.0221(9) 0.0208(7) -0.0065(7) N10 0.033(4) 0.028(4) 0.057(4) 0.005(3) 0.017(3) -0.001(3) N12 0.027(3) 0.032(4) 0.039(4) 0.001(3) 0.019(3) 0.000(3) N7 0.026(3) 0.027(4) 0.088(6) -0.002(4) 0.013(4) 0.004(3) N9 0.029(4) 0.048(5) 0.073(5) 0.025(4) 0.017(3) -0.002(3) N11 0.047(4) 0.058(5) 0.045(4) 0.008(4) 0.024(3) -0.011(4) N8 0.033(4) 0.073(6) 0.062(5) 0.007(4) 0.033(4) 0.000(4) N6 0.031(4) 0.092(7) 0.058(5) -0.002(5) 0.016(4) 0.010(4) N3 0.036(4) 0.096(8) 0.063(5) 0.000(5) 0.014(4) 0.000(5) N5 0.024(3) 0.041(4) 0.055(4) -0.002(3) 0.011(3) 0.000(3) N4 0.038(4) 0.066(6) 0.059(5) 0.002(4) 0.020(4) 0.003(4) N2 0.043(4) 0.076(6) 0.060(6) -0.002(5) 0.014(5) -0.001(5) C2' 0.043(4) 0.076(6) 0.060(6) -0.002(5) 0.014(5) -0.001(5) N1 0.082(7) 0.111(9) 0.093(8) -0.045(6) 0.012(6) -0.011(6) Nd1 0.01875(19) 0.0212(2) 0.0323(2) 0.00035(16) 0.01306(16) -0.00027(15) Nd2 0.01881(19) 0.0228(2) 0.0321(2) -0.00209(16) 0.01360(16) -0.00127(15) O9 0.027(3) 0.031(3) 0.035(3) 0.004(2) 0.008(2) 0.004(2) O10 0.031(3) 0.035(3) 0.037(3) -0.001(2) 0.006(2) -0.010(2) O3 0.043(3) 0.081(5) 0.072(4) -0.023(4) 0.038(3) 0.005(3) O1 0.024(3) 0.033(3) 0.052(3) -0.004(2) 0.006(2) -0.003(2) O11 0.038(3) 0.024(3) 0.050(3) 0.000(2) 0.029(3) -0.001(2) O12 0.032(3) 0.042(3) 0.036(3) -0.003(2) 0.017(2) 0.011(2) O2 0.028(3) 0.033(3) 0.060(4) -0.002(3) 0.008(3) 0.007(2) O4 0.038(3) 0.062(4) 0.061(4) 0.016(3) 0.025(3) -0.013(3) O6 0.031(3) 0.039(3) 0.063(4) 0.007(3) 0.016(3) -0.010(3) O5 0.027(3) 0.035(3) 0.056(3) -0.004(3) 0.016(3) 0.003(2) O7 0.036(3) 0.027(3) 0.064(4) 0.008(3) 0.031(3) 0.012(2) O8 0.022(3) 0.033(3) 0.053(3) 0.010(2) 0.016(2) -0.002(2) O2W 0.034(3) 0.062(4) 0.043(3) -0.008(3) 0.014(3) 0.002(3) O1W 0.049(3) 0.025(3) 0.044(3) 0.006(2) 0.009(3) -0.004(2) O4W 0.082(4) 0.035(3) 0.034(3) -0.001(2) 0.016(3) -0.024(3) O3W 0.030(3) 0.043(3) 0.036(3) -0.004(2) 0.013(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C28 N10 1.334(9) . ? C28 C29 1.394(10) . ? C28 H28 0.9300 . ? C29 C25 1.378(10) . ? C29 H29 0.9300 . ? C25 C26 1.388(10) . ? C25 C24 1.507(10) . ? C26 C27 1.378(10) . ? C26 H26 0.9300 . ? C27 N10 1.338(9) . ? C27 H27 0.9300 . ? C24 O10 1.243(8) . ? C24 O9 1.262(8) . ? C3 N4 1.135(10) . ? C3 Cu2 1.851(8) . ? C23 O2 1.249(9) . ? C23 O1 1.254(9) . ? C23 C20 1.514(10) . ? C30 O11 1.240(8) . ? C30 O12 1.259(8) . ? C30 C31 1.503(10) . ? C5 N6 1.127(10) . ? C5 Cu5 1.913(7) 1_665 ? C36 N12 1.340(9) . ? C36 C37 1.384(9) . ? C36 H36 0.9300 . ? C40 N12 1.323(9) . ? C40 C39 1.382(9) . ? C40 H40 0.9300 . ? C19 C20 1.361(11) . ? C19 C18 1.375(10) . ? C19 H19 0.9300 . ? C18 N7 1.312(10) . ? C18 H18 0.9300 . ? C20 C21 1.357(11) . ? C32 C31 1.364(10) . ? C32 C33 1.394(10) . ? C32 H32 0.9300 . ? C31 C35 1.381(10) . ? C35 C34 1.366(9) . ? C35 H35 0.9300 . ? C34 N11 1.326(10) . ? C34 H34 0.9300 . ? C33 N11 1.331(10) . ? C33 H33 0.9300 . ? C12 O4 1.239(9) . ? C12 O3 1.240(9) . ? C12 C13 1.514(10) . ? C13 C14 1.360(11) . ? C13 C17 1.377(11) . ? C17 C16 1.382(10) . ? C17 H17 0.9300 . ? C22 N7 1.321(10) . ? C22 C21 1.398(11) . ? C22 H22 0.9300 . ? C21 H21 0.9300 . ? C14 C15 1.368(10) . ? C14 H14 0.9300 . ? C15 N8 1.315(11) . ? C15 H15 0.9300 . ? C6 N9 1.286(10) . ? C6 C9 1.386(11) . ? C6 H6 0.9300 . ? C9 C10 1.336(11) . ? C9 H9 0.9300 . ? C7 N9 1.287(10) . ? C7 C8 1.374(11) . ? C7 H7 0.9300 . ? C8 C10 1.334(12) . ? C8 H8 0.9300 . ? C10 C11 1.498(11) . ? C37 C38 1.368(9) . ? C37 H37 0.9300 . ? C39 C38 1.375(10) . ? C39 H39 0.9300 . ? C11 O6 1.237(10) . ? C11 O5 1.244(9) . ? C38 C41 1.516(9) . ? C41 O7 1.230(8) . ? C41 O8 1.262(8) . ? C2 N3 1.117(10) . ? C2 Cu2 1.847(7) 1_545 ? C4 N5 1.167(10) . ? C4 Cu5 1.881(8) 1_655 ? C16 N8 1.317(11) . ? C16 H16 0.9300 . ? C1 N1 1.145(12) . ? Cu2 C2 1.847(7) 1_565 ? Cu2 N10 2.129(6) 1_655 ? Cu3 N4 1.927(9) . ? Cu3 N3 1.951(10) . ? Cu3 N9 2.087(6) . ? Cu3 Cu4 2.7355(19) . ? Cu1 N5 1.934(7) . ? Cu1 N6 1.937(10) . ? Cu1 N7 2.119(6) . ? Cu5 C4 1.881(8) 1_455 ? Cu5 C5 1.913(7) 1_445 ? Cu5 N12 2.119(5) . ? Cu4 N2 1.859(7) . ? Cu4 N1 1.874(11) . ? N10 Cu2 2.129(6) 1_455 ? N2 C2' 1.142(15) 3_755 ? N2 N2 1.142(15) 3_755 ? Nd1 O12 2.343(5) . ? Nd1 O5 2.360(5) . ? Nd1 O8 2.398(4) . ? Nd1 O4 2.431(5) . ? Nd1 O1 2.459(5) . ? Nd1 O9 2.503(5) . ? Nd1 O2W 2.526(5) . ? Nd1 O1W 2.626(5) . ? Nd2 O10 2.366(5) 1_545 ? Nd2 O7 2.396(5) . ? Nd2 O3 2.415(5) 1_545 ? Nd2 O6 2.415(5) . ? Nd2 O2 2.427(5) 1_545 ? Nd2 O11 2.479(4) 1_545 ? Nd2 O4W 2.529(5) . ? Nd2 O3W 2.534(5) . ? O10 Nd2 2.366(5) 1_565 ? O3 Nd2 2.415(5) 1_565 ? O11 Nd2 2.479(4) 1_565 ? O2 Nd2 2.427(5) 1_565 ? O2W H3W 0.8089 . ? O2W H4W 0.8139 . ? O1W H2W 0.8147 . ? O1W H1W 0.8143 . ? O4W H7W 0.8144 . ? O4W H8W 0.8196 . ? O3W H5W 0.8202 . ? O3W H6W 0.8224 . ? 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 N10 C28 C29 122.6(7) . . ? N10 C28 H28 118.7 . . ? C29 C28 H28 118.7 . . ? C25 C29 C28 119.3(7) . . ? C25 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C25 C26 118.4(7) . . ? C29 C25 C24 120.8(7) . . ? C26 C25 C24 120.4(7) . . ? C27 C26 C25 118.3(7) . . ? C27 C26 H26 120.8 . . ? C25 C26 H26 120.8 . . ? N10 C27 C26 124.1(7) . . ? N10 C27 H27 117.9 . . ? C26 C27 H27 117.9 . . ? O10 C24 O9 125.0(7) . . ? O10 C24 C25 116.9(7) . . ? O9 C24 C25 118.0(6) . . ? N4 C3 Cu2 168.3(7) . . ? O2 C23 O1 126.7(7) . . ? O2 C23 C20 116.8(7) . . ? O1 C23 C20 116.4(7) . . ? O11 C30 O12 124.6(7) . . ? O11 C30 C31 117.5(7) . . ? O12 C30 C31 117.9(7) . . ? N6 C5 Cu5 170.4(8) . 1_665 ? N12 C36 C37 122.8(7) . . ? N12 C36 H36 118.6 . . ? C37 C36 H36 118.6 . . ? N12 C40 C39 124.3(7) . . ? N12 C40 H40 117.8 . . ? C39 C40 H40 117.8 . . ? C20 C19 C18 120.5(8) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? N7 C18 C19 124.2(8) . . ? N7 C18 H18 117.9 . . ? C19 C18 H18 117.9 . . ? C21 C20 C19 116.0(7) . . ? C21 C20 C23 121.1(7) . . ? C19 C20 C23 122.9(7) . . ? C31 C32 C33 119.0(7) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C32 C31 C35 117.8(7) . . ? C32 C31 C30 121.5(7) . . ? C35 C31 C30 120.7(7) . . ? C34 C35 C31 119.9(7) . . ? C34 C35 H35 120.1 . . ? C31 C35 H35 120.1 . . ? N11 C34 C35 122.8(7) . . ? N11 C34 H34 118.6 . . ? C35 C34 H34 118.6 . . ? N11 C33 C32 122.5(7) . . ? N11 C33 H33 118.7 . . ? C32 C33 H33 118.7 . . ? O4 C12 O3 126.9(7) . . ? O4 C12 C13 117.4(7) . . ? O3 C12 C13 115.7(8) . . ? C14 C13 C17 117.6(7) . . ? C14 C13 C12 121.8(8) . . ? C17 C13 C12 120.6(7) . . ? C13 C17 C16 118.8(8) . . ? C13 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? N7 C22 C21 123.1(8) . . ? N7 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? C20 C21 C22 120.3(8) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C13 C14 C15 120.2(8) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? N8 C15 C14 122.4(8) . . ? N8 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? N9 C6 C9 124.5(8) . . ? N9 C6 H6 117.7 . . ? C9 C6 H6 117.7 . . ? C10 C9 C6 119.9(8) . . ? C10 C9 H9 120.1 . . ? C6 C9 H9 120.1 . . ? N9 C7 C8 124.9(9) . . ? N9 C7 H7 117.5 . . ? C8 C7 H7 117.5 . . ? C10 C8 C7 120.1(9) . . ? C10 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C10 C9 115.8(8) . . ? C8 C10 C11 122.7(8) . . ? C9 C10 C11 121.4(8) . . ? C38 C37 C36 119.8(7) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C38 C39 C40 118.6(7) . . ? C38 C39 H39 120.7 . . ? C40 C39 H39 120.7 . . ? O6 C11 O5 125.3(8) . . ? O6 C11 C10 116.1(8) . . ? O5 C11 C10 118.6(8) . . ? C37 C38 C39 118.0(6) . . ? C37 C38 C41 121.9(6) . . ? C39 C38 C41 120.1(6) . . ? O7 C41 O8 124.9(6) . . ? O7 C41 C38 117.8(6) . . ? O8 C41 C38 117.3(6) . . ? N3 C2 Cu2 177.9(9) . 1_545 ? N5 C4 Cu5 173.7(6) . 1_655 ? N8 C16 C17 122.7(8) . . ? N8 C16 H16 118.7 . . ? C17 C16 H16 118.7 . . ? C2 Cu2 C3 153.4(3) 1_565 . ? C2 Cu2 N10 106.5(3) 1_565 1_655 ? C3 Cu2 N10 100.1(3) . 1_655 ? N4 Cu3 N3 151.1(3) . . ? N4 Cu3 N9 103.4(3) . . ? N3 Cu3 N9 103.6(3) . . ? N4 Cu3 Cu4 83.2(2) . . ? N3 Cu3 Cu4 71.6(2) . . ? N9 Cu3 Cu4 130.5(2) . . ? N5 Cu1 N6 148.6(3) . . ? N5 Cu1 N7 100.6(3) . . ? N6 Cu1 N7 110.8(3) . . ? C4 Cu5 C5 146.3(3) 1_455 1_445 ? C4 Cu5 N12 108.0(3) 1_455 . ? C5 Cu5 N12 105.5(3) 1_445 . ? N2 Cu4 N1 154.3(4) . . ? N2 Cu4 Cu3 82.3(3) . . ? N1 Cu4 Cu3 123.4(3) . . ? C28 N10 C27 117.2(6) . . ? C28 N10 Cu2 120.7(5) . 1_455 ? C27 N10 Cu2 122.1(5) . 1_455 ? C40 N12 C36 116.5(6) . . ? C40 N12 Cu5 122.7(5) . . ? C36 N12 Cu5 120.8(5) . . ? C18 N7 C22 115.6(7) . . ? C18 N7 Cu1 122.3(5) . . ? C22 N7 Cu1 122.0(5) . . ? C6 N9 C7 114.4(7) . . ? C6 N9 Cu3 119.6(6) . . ? C7 N9 Cu3 124.1(6) . . ? C34 N11 C33 117.7(7) . . ? C15 N8 C16 118.3(7) . . ? C5 N6 Cu1 173.4(8) . . ? C2 N3 Cu3 171.2(8) . . ? C4 N5 Cu1 171.1(7) . . ? C3 N4 Cu3 174.0(7) . . ? C2' N2 N2 0.0(14) 3_755 3_755 ? C2' N2 Cu4 177.0(13) 3_755 . ? N2 N2 Cu4 177.0(13) 3_755 . ? C1 N1 Cu4 174.6(9) . . ? O12 Nd1 O5 146.28(18) . . ? O12 Nd1 O8 82.75(17) . . ? O5 Nd1 O8 98.19(17) . . ? O12 Nd1 O4 111.3(2) . . ? O5 Nd1 O4 83.41(19) . . ? O8 Nd1 O4 152.06(19) . . ? O12 Nd1 O1 74.84(17) . . ? O5 Nd1 O1 81.48(17) . . ? O8 Nd1 O1 135.21(17) . . ? O4 Nd1 O1 72.71(18) . . ? O12 Nd1 O9 73.20(16) . . ? O5 Nd1 O9 139.91(17) . . ? O8 Nd1 O9 75.44(16) . . ? O4 Nd1 O9 85.40(17) . . ? O1 Nd1 O9 130.89(16) . . ? O12 Nd1 O2W 140.82(17) . . ? O5 Nd1 O2W 71.26(18) . . ? O8 Nd1 O2W 79.41(17) . . ? O4 Nd1 O2W 74.69(19) . . ? O1 Nd1 O2W 139.38(16) . . ? O9 Nd1 O2W 68.67(17) . . ? O12 Nd1 O1W 75.24(17) . . ? O5 Nd1 O1W 73.17(17) . . ? O8 Nd1 O1W 71.76(16) . . ? O4 Nd1 O1W 134.12(17) . . ? O1 Nd1 O1W 65.30(16) . . ? O9 Nd1 O1W 136.65(15) . . ? O2W Nd1 O1W 129.72(17) . . ? O10 Nd2 O7 89.67(18) 1_545 . ? O10 Nd2 O3 77.46(19) 1_545 1_545 ? O7 Nd2 O3 147.4(2) . 1_545 ? O10 Nd2 O6 141.93(18) 1_545 . ? O7 Nd2 O6 97.90(18) . . ? O3 Nd2 O6 76.3(2) 1_545 . ? O10 Nd2 O2 116.38(18) 1_545 1_545 ? O7 Nd2 O2 140.33(18) . 1_545 ? O3 Nd2 O2 71.1(2) 1_545 1_545 ? O6 Nd2 O2 80.02(18) . 1_545 ? O10 Nd2 O11 76.64(17) 1_545 1_545 ? O7 Nd2 O11 73.82(16) . 1_545 ? O3 Nd2 O11 129.88(19) 1_545 1_545 ? O6 Nd2 O11 141.29(18) . 1_545 ? O2 Nd2 O11 83.35(17) 1_545 1_545 ? O10 Nd2 O4W 67.82(17) 1_545 . ? O7 Nd2 O4W 74.00(18) . . ? O3 Nd2 O4W 73.4(2) 1_545 . ? O6 Nd2 O4W 78.51(18) . . ? O2 Nd2 O4W 141.88(19) 1_545 . ? O11 Nd2 O4W 131.45(18) 1_545 . ? O10 Nd2 O3W 147.85(16) 1_545 . ? O7 Nd2 O3W 70.86(17) . . ? O3 Nd2 O3W 131.93(18) 1_545 . ? O6 Nd2 O3W 68.15(17) . . ? O2 Nd2 O3W 71.75(17) 1_545 . ? O11 Nd2 O3W 73.50(16) 1_545 . ? O4W Nd2 O3W 126.59(17) . . ? C24 O9 Nd1 121.3(4) . . ? C24 O10 Nd2 143.5(5) . 1_565 ? C12 O3 Nd2 151.6(6) . 1_565 ? C23 O1 Nd1 137.6(5) . . ? C30 O11 Nd2 117.8(4) . 1_565 ? C30 O12 Nd1 171.5(5) . . ? C23 O2 Nd2 141.2(6) . 1_565 ? C12 O4 Nd1 134.2(5) . . ? C11 O6 Nd2 135.5(5) . . ? C11 O5 Nd1 151.3(6) . . ? C41 O7 Nd2 168.2(5) . . ? C41 O8 Nd1 135.8(5) . . ? Nd1 O2W H3W 111.8 . . ? Nd1 O2W H4W 128.9 . . ? H3W O2W H4W 105.8 . . ? Nd1 O1W H2W 98.6 . . ? Nd1 O1W H1W 122.7 . . ? H2W O1W H1W 105.1 . . ? Nd2 O4W H7W 123.6 . . ? Nd2 O4W H8W 129.7 . . ? H7W O4W H8W 104.5 . . ? Nd2 O3W H5W 102.3 . . ? Nd2 O3W H6W 124.0 . . ? H5W O3W H6W 103.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2W H4W O4W 0.81 2.50 3.241(8) 152.5 3_655 O1W H2W O1 0.81 2.24 2.747(7) 120.5 . O1W H1W O3W 0.81 2.11 2.921(7) 170.1 . O4W H7W O9 0.81 2.05 2.847(7) 165.2 3_655 O4W H8W O2W 0.82 2.31 3.002(8) 142.1 . O4W H8W O5 0.82 2.51 3.017(7) 121.4 . O3W H5W N5 0.82 2.43 3.099(8) 139.3 2_745 O3W H5W O2 0.82 2.49 2.909(7) 113.0 1_545 O3W H6W N11 0.82 1.88 2.696(8) 173.0 2_645 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.727 _refine_diff_density_min -1.868 _refine_diff_density_rms 0.144 --CCDCCONTENTSEPARATOR--