# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1436 data_culn #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Chen, Xiao-Ming School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone '86-20-84186300 ext 2074' _publ_contact_author_fax '86-20-4189173' _publ_contact_author_email cedc03@zsu.edu.cn _publ_requested_joiurnal ' J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF as a supplemenatry data for a submission of a full paper to J. Chem. Soc., Dalton Trans. (Paper ref. 9/00647H). Jan. 26, 1998. ; #========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Structures of Carboxylate-Bridged Polynuclear Copper(II)-Lanthanide(III) Complexes [CuLn(pyridinioacetate) 5(H2O)5](ClO4)5(2H2O and [Cu3Nd2(pyridinioacetate)10(NO3)2 (H2O)8](ClO4)8(4H2O ; loop_ _publ_author_name _publ_author_address 'Yang, Yang-Yi' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Wu, Yu-Luan' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Long, La-Sheng' ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou 350002 P. R. China ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; #============================================================ data_complex_1.La _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H49 Cl5 Cu La N5 O37' _chemical_formula_weight 1511.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.950(8) _cell_length_b 11.286(2) _cell_length_c 27.859(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.70(3) _cell_angle_gamma 90.00 _cell_volume 11542(4) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6088 _exptl_absorpt_coefficient_mu 1.435 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'Siemens R3m' _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 120 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.0 _diffrn_reflns_number 8822 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8822 _reflns_number_gt 5359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0988P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000015(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8822 _refine_ls_number_parameters 811 _refine_ls_number_restraints 177 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1661 _refine_ls_wR_factor_gt 0.1410 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.456 _refine_ls_shift/su_mean 0.032 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.105852(6) 0.06466(2) 0.071817(8) 0.04089(7) Uani 1 d . . . Cu1 Cu 0.188708(12) -0.01540(4) 0.173162(17) 0.03745(13) Uani 1 d . . . O1W O 0.10638(10) 0.2911(3) 0.07395(15) 0.1003(16) Uani 1 d . . . H1WA H 0.1223 0.3223 0.1007 0.100 Uiso 1 d R . . H1WB H 0.0831 0.3564 0.0646 0.100 Uiso 1 d R . . O2W O 0.13011(9) 0.0917(3) -0.00795(12) 0.0781(12) Uani 1 d . . . H2WA H 0.1581 0.0982 0.0082 0.100 Uiso 1 d R . . H2WB H 0.1104 0.1198 -0.0350 0.100 Uiso 1 d R . . O3W O 0.05824(8) 0.1615(3) -0.00209(12) 0.0816(12) Uani 1 d . . . H3WA H 0.0307 0.1318 -0.0152 0.100 Uiso 1 d R . . H3WB H 0.0585 0.2397 -0.0147 0.100 Uiso 1 d R . . O4W O 0.06971(8) -0.1061(3) 0.01816(11) 0.0599(10) Uani 1 d . . . H4WA H 0.0432 -0.1342 0.0271 0.100 Uiso 1 d R . . H4WB H 0.0818 -0.1923 0.0179 0.100 Uiso 1 d R . . O5W O 0.23628(8) -0.0643(3) 0.23549(11) 0.0583(9) Uani 1 d . . . H5WA H 0.2487 -0.1478 0.2364 0.100 Uiso 1 d R . . H5WB H 0.2543 -0.0026 0.2317 0.100 Uiso 1 d R . . O12 O 0.17038(7) 0.1433(3) 0.09167(11) 0.0589(10) Uani 1 d . . . O11 O 0.22008(7) 0.1005(3) 0.14994(10) 0.0513(9) Uani 1 d . . . N1 N 0.26154(8) 0.2593(3) 0.11732(12) 0.0444(10) Uani 1 d . . . C11 C 0.20269(11) 0.1567(4) 0.11296(15) 0.0435(11) Uani 1 d . . . C12 C 0.22239(11) 0.2520(4) 0.09234(15) 0.0505(13) Uani 1 d . . . H12A H 0.2199 0.2362 0.0578 0.100 Uiso 1 d R . . H12B H 0.2111 0.3270 0.0950 0.100 Uiso 1 d R . . C13 C 0.28580(13) 0.2114(5) 0.09612(19) 0.0755(18) Uani 1 d . . . H13 H 0.2781 0.1688 0.0654 0.100 Uiso 1 d R . . C14 C 0.32251(14) 0.2146(6) 0.1201(2) 0.084(2) Uani 1 d . . . H14 H 0.3400 0.1840 0.1037 0.100 Uiso 1 d R . . C15 C 0.33408(14) 0.2679(6) 0.1640(2) 0.091(2) Uani 1 d . . . H15 H 0.3595 0.2718 0.1805 0.100 Uiso 1 d R . . C16 C 0.30847(15) 0.3180(6) 0.1847(2) 0.102(2) Uani 1 d . . . H16 H 0.3160 0.3496 0.2177 0.100 Uiso 1 d R . . C17 C 0.27229(14) 0.3123(6) 0.16109(18) 0.0794(18) Uani 1 d . . . H17 H 0.2551 0.3525 0.1754 0.100 Uiso 1 d R . . O21 O 0.15600(7) -0.1234(3) 0.19397(10) 0.0510(9) Uani 1 d . . . O22 O 0.10474(7) -0.1014(3) 0.13325(10) 0.0542(9) Uani 1 d . . . N2 N 0.06929(9) -0.2724(3) 0.17222(13) 0.0464(10) Uani 1 d . . . C21 C 0.12366(11) -0.1467(3) 0.17131(14) 0.0430(11) Uani 1 d . . . C22 C 0.10785(11) -0.2475(4) 0.19609(16) 0.0497(13) Uani 1 d . . . H22A H 0.1218 -0.3181 0.1953 0.100 Uiso 1 d R . . H22B H 0.1101 -0.2276 0.2302 0.100 Uiso 1 d R . . C23 C 0.06065(13) -0.3288(4) 0.12947(18) 0.0650(16) Uani 1 d . . . H23 H 0.0794 -0.3568 0.1148 0.100 Uiso 1 d R . . C24 C 0.02505(15) -0.3520(6) 0.1068(2) 0.089(2) Uani 1 d . . . H24 H 0.0190 -0.3860 0.0741 0.100 Uiso 1 d R . . C25 C -0.00143(14) -0.3211(5) 0.1279(2) 0.085(2) Uani 1 d . . . H25 H -0.0261 -0.3450 0.1134 0.100 Uiso 1 d R . . C26 C 0.00739(13) -0.2620(5) 0.1715(2) 0.0820(19) Uani 1 d . . . H26 H -0.0113 -0.2336 0.1863 0.100 Uiso 1 d R . . C27 C 0.04338(12) -0.2370(4) 0.19408(18) 0.0624(15) Uani 1 d . . . H27 H 0.0498 -0.1950 0.2251 0.100 Uiso 1 d R . . O31 O 0.19920(7) -0.1327(3) 0.12657(10) 0.0503(9) Uani 1 d . . . O32 O 0.14866(7) -0.1039(3) 0.06566(10) 0.0532(9) Uani 1 d . . . N3 N 0.16803(10) -0.2774(4) 0.00785(14) 0.0708(13) Uani 1 d . . . C31 C 0.17795(10) -0.1519(4) 0.08432(14) 0.0427(11) Uani 1 d . . . C32 C 0.19338(11) -0.2444(4) 0.05620(15) 0.0513(13) Uani 1 d . . . H32A H 0.2159 -0.2166 0.0506 0.100 Uiso 1 d R . . H32B H 0.1985 -0.3148 0.0761 0.100 Uiso 1 d R . . C33 C 0.16152(19) -0.3907(7) -0.0018(3) 0.141(3) Uani 1 d . . . H33 H 0.1705 -0.4498 0.0231 0.100 Uiso 1 d R . . C34 C 0.1400(2) -0.4185(10) -0.0493(4) 0.272(4) Uani 1 d . . . H34 H 0.1348 -0.4983 -0.0608 0.100 Uiso 1 d R . . C35 C 0.1231(2) -0.3421(10) -0.0798(3) 0.237(4) Uani 1 d . . . H35 H 0.1060 -0.3588 -0.1109 0.100 Uiso 1 d R . . C36 C 0.13133(18) -0.2267(10) -0.0707(2) 0.152(4) Uani 1 d . . . H36 H 0.1212 -0.1654 -0.0940 0.100 Uiso 1 d R . . C37 C 0.15407(15) -0.1937(7) -0.02536(18) 0.096(2) Uani 1 d . . . H37 H 0.1611 -0.1130 -0.0173 0.100 Uiso 1 d R . . O41 O 0.17464(7) 0.1106(3) 0.21512(10) 0.0473(8) Uani 1 d . . . O42 O 0.12138(8) 0.1408(3) 0.15983(10) 0.0559(9) Uani 1 d . . . N4 N 0.15819(9) 0.2621(3) 0.28253(12) 0.0495(10) Uani 1 d . . . C41 C 0.14374(11) 0.1574(4) 0.20028(15) 0.0443(12) Uani 1 d . . . C42 C 0.13070(11) 0.2394(4) 0.23560(15) 0.0531(14) Uani 1 d . . . H42A H 0.1239 0.3135 0.2189 0.100 Uiso 1 d R . . H42B H 0.1094 0.2059 0.2429 0.100 Uiso 1 d R . . C43 C 0.16874(15) 0.1747(5) 0.31460(18) 0.0770(18) Uani 1 d . . . H43 H 0.1570 0.0991 0.3072 0.100 Uiso 1 d R . . C44 C 0.1936(2) 0.1938(8) 0.3580(2) 0.127(3) Uani 1 d . . . H44 H 0.2018 0.1301 0.3809 0.100 Uiso 1 d R . . C45 C 0.20903(18) 0.2991(8) 0.3686(3) 0.132(3) Uani 1 d . . . H45 H 0.2262 0.3124 0.4000 0.100 Uiso 1 d R . . C46 C 0.19924(16) 0.3927(7) 0.3359(3) 0.115(2) Uani 1 d . . . H46 H 0.2108 0.4686 0.3430 0.100 Uiso 1 d R . . C47 C 0.17278(13) 0.3697(5) 0.2915(2) 0.0744(17) Uani 1 d . . . H47 H 0.1645 0.4314 0.2675 0.100 Uiso 1 d R . . O51 O 0.04472(7) 0.0608(3) 0.08873(12) 0.0606(10) Uani 1 d . . . O52 O 0.00937(8) -0.0839(3) 0.04990(12) 0.0598(10) Uani 1 d . . . N5 N -0.00606(9) 0.1485(3) 0.13027(13) 0.0529(11) Uani 1 d . . . C51 C 0.01610(11) 0.0018(4) 0.07752(16) 0.0490(13) Uani 1 d . . . C52 C -0.01362(12) 0.0385(5) 0.10224(18) 0.0632(16) Uani 1 d . . . H52A H -0.0361 0.0477 0.0773 0.100 Uiso 1 d R . . H52B H -0.0168 -0.0237 0.1243 0.100 Uiso 1 d R . . C53 C 0.01551(13) 0.1436(5) 0.17746(18) 0.0703(17) Uani 1 d . . . H53 H 0.0246 0.0693 0.1923 0.100 Uiso 1 d R . . C54 C 0.02477(14) 0.2452(6) 0.2032(2) 0.080(2) Uani 1 d . . . H54 H 0.0412 0.2443 0.2357 0.100 Uiso 1 d R . . C55 C 0.01059(18) 0.3522(6) 0.1826(3) 0.109(3) Uani 1 d . . . H55 H 0.0161 0.4247 0.2009 0.100 Uiso 1 d R . . C56 C -0.0118(2) 0.3513(6) 0.1365(3) 0.125(3) Uani 1 d . . . H56 H -0.0218 0.4244 0.1214 0.100 Uiso 1 d R . . C57 C -0.02004(18) 0.2501(5) 0.1117(2) 0.092(2) Uani 1 d . . . H57 H -0.0366 0.2489 0.0793 0.100 Uiso 1 d R . . Cl1 Cl 0.41852(4) 0.02543(13) 0.20243(5) 0.0723(4) Uani 1 d . . . O13 O 0.4175(2) -0.1014(5) 0.1981(2) 0.165(3) Uani 1 d U . . O14 O 0.39914(18) 0.0531(6) 0.2348(2) 0.212(3) Uani 1 d U . . O15 O 0.4056(3) 0.0671(6) 0.1570(3) 0.253(5) Uani 1 d U . . O16 O 0.45401(17) 0.0565(6) 0.2221(3) 0.193(3) Uani 1 d U . . Cl2 Cl 0.07779(4) 0.00471(12) -0.19316(5) 0.0728(4) Uiso 1 d . . . O23 O 0.09660(12) 0.0242(5) -0.22917(18) 0.1399(18) Uani 1 d U . . O24 O 0.07577(16) -0.1176(5) -0.1830(2) 0.153(2) Uani 1 d U . . O25 O 0.04165(14) 0.0432(5) -0.2110(2) 0.162(2) Uani 1 d U . . O26 O 0.0920(3) 0.0594(8) -0.1526(3) 0.273(4) Uani 1 d U . . Cl3 Cl 0.23767(4) 0.00019(12) -0.01186(5) 0.0772(4) Uiso 1 d D . . O33 O 0.26671(10) 0.0787(4) -0.01276(19) 0.147(2) Uani 1 d DU A 1 O34 O 0.23272(18) 0.0027(6) 0.03737(16) 0.142(3) Uani 0.60 d PDU A 1 O35 O 0.24191(17) -0.1198(4) -0.0224(2) 0.096(2) Uani 0.60 d PDU A 1 O36 O 0.20532(16) 0.0398(7) -0.0451(3) 0.175(5) Uani 0.60 d PDU A 1 O34' O 0.2534(3) -0.0946(6) 0.0196(3) 0.237(8) Uani 0.40 d PDU A 2 O35' O 0.2252(4) -0.0436(9) -0.0608(2) 0.314(13) Uani 0.40 d PDU A 2 O36' O 0.20930(15) 0.0523(8) 0.0037(3) 0.133(5) Uani 0.40 d PDU A 2 Cl4 Cl 0.17770(4) 0.50689(14) 0.16046(6) 0.0830(5) Uani 1 d . . . O43 O 0.18450(17) 0.5621(4) 0.20812(19) 0.135(2) Uani 1 d . . . O44 O 0.17543(17) 0.3861(5) 0.1668(2) 0.176(2) Uani 1 d . . . O45 O 0.14889(16) 0.5682(8) 0.1313(3) 0.242(4) Uani 1 d . . . O46 O 0.20901(15) 0.5320(5) 0.1439(2) 0.136(2) Uani 1 d . . . Cl5 Cl 0.05920(6) 0.5358(2) -0.00146(7) 0.1484(10) Uani 1 d D . . O53 O 0.06020(19) 0.4547(5) -0.0390(2) 0.147(3) Uani 0.60 d PDU B 1 O54 O 0.02176(14) 0.5759(9) -0.0119(4) 0.258(7) Uani 0.60 d PDU B 1 O55 O 0.0787(2) 0.6434(5) -0.0005(4) 0.215(6) Uani 0.60 d PDU B 1 O56 O 0.0690(2) 0.4856(6) 0.04634(17) 0.131(3) Uani 0.60 d PDU B 1 O53' O 0.0459(2) 0.4513(7) 0.0274(3) 0.210(8) Uani 0.40 d PDU B 2 O54' O 0.0861(2) 0.6075(8) 0.0295(3) 0.240(9) Uani 0.40 d PDU B 2 O55' O 0.0304(2) 0.6075(8) -0.0281(4) 0.421(17) Uani 0.40 d PDU B 2 O56' O 0.0750(2) 0.4732(9) -0.0350(3) 0.289(13) Uani 0.40 d PDU B 2 O6W O 0.09604(13) 0.2480(5) -0.08239(18) 0.1409(19) Uani 1 d . . . H6WA H 0.0865 0.2882 -0.1128 0.100 Uiso 1 d R . . H6WB H 0.0853 0.3226 -0.0630 0.100 Uiso 1 d R . . O7W O 0.25560(10) -0.2919(3) 0.23107(17) 0.1027(16) Uani 1 d . . . H7WA H 0.2297 -0.3349 0.2303 0.100 Uiso 1 d R . . H7WB H 0.2494 -0.2198 0.2325 0.100 Uiso 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 La1 0.02969(11) 0.04867(13) 0.03990(11) 0.00589(11) 0.00069(9) -0.00402(11) Cu1 0.0332(2) 0.0414(3) 0.0365(2) 0.0026(2) 0.00664(19) -0.0031(2) O1W 0.088(3) 0.057(2) 0.123(3) 0.015(2) -0.032(2) 0.006(2) O2W 0.0595(19) 0.118(3) 0.0537(18) 0.0261(19) 0.0084(16) 0.003(2) O3W 0.0481(18) 0.093(2) 0.083(2) 0.0409(19) -0.0199(17) -0.0177(18) O4W 0.0486(16) 0.072(2) 0.0541(17) -0.0108(16) 0.0036(14) -0.0058(16) O5W 0.0419(15) 0.0673(19) 0.0600(17) 0.0142(16) 0.0025(14) 0.0107(15) O12 0.0312(14) 0.072(2) 0.0680(18) 0.0085(17) 0.0026(13) -0.0112(15) O11 0.0466(15) 0.0560(17) 0.0496(15) 0.0075(14) 0.0087(13) -0.0120(14) N1 0.0400(17) 0.047(2) 0.0466(18) 0.0034(16) 0.0124(15) -0.0097(16) C11 0.041(2) 0.045(2) 0.047(2) -0.0038(19) 0.0153(17) -0.0029(19) C12 0.046(2) 0.054(2) 0.050(2) 0.015(2) 0.0082(19) -0.015(2) C13 0.053(3) 0.103(4) 0.074(3) -0.029(3) 0.022(2) -0.008(3) C14 0.051(3) 0.121(5) 0.082(3) -0.027(3) 0.021(2) 0.001(3) C15 0.042(3) 0.140(5) 0.086(4) -0.021(4) 0.005(3) -0.027(3) C16 0.065(3) 0.166(6) 0.064(3) -0.049(4) -0.002(3) -0.023(4) C17 0.054(3) 0.121(4) 0.062(3) -0.034(3) 0.013(2) -0.012(3) O21 0.0386(14) 0.0538(17) 0.0596(16) 0.0076(15) 0.0104(13) -0.0125(14) O22 0.0488(16) 0.0614(18) 0.0508(16) 0.0139(14) 0.0094(13) -0.0057(15) N2 0.0403(18) 0.0404(18) 0.055(2) 0.0044(16) 0.0048(16) -0.0084(16) C21 0.049(2) 0.037(2) 0.045(2) 0.0043(18) 0.0149(18) 0.0002(19) C22 0.043(2) 0.046(2) 0.058(2) 0.015(2) 0.0103(19) -0.006(2) C23 0.055(3) 0.068(3) 0.068(3) 0.000(3) 0.010(2) -0.011(3) C24 0.075(4) 0.113(5) 0.067(3) -0.003(3) -0.006(3) -0.020(4) C25 0.051(3) 0.083(4) 0.108(4) 0.018(3) -0.007(3) -0.020(3) C26 0.046(2) 0.098(4) 0.109(4) 0.022(3) 0.033(3) 0.006(3) C27 0.057(3) 0.061(3) 0.077(3) -0.001(2) 0.033(2) -0.003(2) O31 0.0487(15) 0.0545(17) 0.0449(15) -0.0040(14) 0.0067(13) 0.0061(14) O32 0.0478(16) 0.0622(18) 0.0484(15) 0.0029(14) 0.0099(13) 0.0085(15) N3 0.047(2) 0.107(3) 0.061(2) -0.032(2) 0.0184(17) 0.004(2) C31 0.037(2) 0.048(2) 0.045(2) 0.0080(19) 0.0127(17) -0.0055(19) C32 0.049(2) 0.060(3) 0.044(2) -0.007(2) 0.0114(19) 0.000(2) C33 0.100(5) 0.126(5) 0.202(7) -0.099(5) 0.044(5) -0.009(4) C34 0.100(6) 0.404(9) 0.295(7) -0.301(6) 0.018(5) -0.034(7) C35 0.094(6) 0.414(11) 0.192(6) -0.233(6) 0.013(5) -0.049(7) C36 0.076(4) 0.324(12) 0.052(3) -0.030(5) 0.009(3) 0.021(6) C37 0.068(3) 0.175(6) 0.042(3) -0.006(4) 0.011(2) 0.007(4) O41 0.0356(14) 0.0502(16) 0.0506(15) -0.0014(14) 0.0008(12) -0.0018(13) O42 0.0493(16) 0.068(2) 0.0450(15) -0.0121(15) 0.0016(13) -0.0047(15) N4 0.0455(18) 0.065(2) 0.0406(17) -0.0085(17) 0.0145(15) -0.0014(18) C41 0.043(2) 0.044(2) 0.045(2) -0.0082(19) 0.0083(18) -0.0086(19) C42 0.035(2) 0.072(3) 0.047(2) -0.014(2) 0.0014(19) 0.004(2) C43 0.081(3) 0.086(4) 0.061(3) 0.014(3) 0.013(3) -0.004(3) C44 0.129(5) 0.197(8) 0.051(3) 0.023(4) 0.015(3) 0.049(5) C45 0.075(4) 0.211(8) 0.090(4) -0.052(5) -0.013(4) 0.022(5) C46 0.074(3) 0.137(5) 0.143(5) -0.084(4) 0.043(3) -0.034(4) C47 0.066(3) 0.074(3) 0.084(3) -0.022(3) 0.020(3) 0.006(3) O51 0.0280(13) 0.069(2) 0.083(2) -0.0075(17) 0.0117(14) -0.0104(14) O52 0.0421(15) 0.064(2) 0.0724(19) -0.0081(16) 0.0122(14) -0.0049(15) N5 0.0397(18) 0.064(2) 0.056(2) -0.0022(19) 0.0143(16) 0.0048(18) C51 0.041(2) 0.055(3) 0.049(2) 0.005(2) 0.0068(19) 0.006(2) C52 0.039(2) 0.080(3) 0.068(3) 0.004(3) 0.009(2) -0.007(2) C53 0.060(3) 0.079(4) 0.066(3) 0.007(3) 0.005(3) 0.008(3) C54 0.055(3) 0.109(5) 0.071(3) -0.014(3) 0.007(3) 0.005(3) C55 0.111(5) 0.096(4) 0.120(5) -0.046(4) 0.028(4) -0.006(4) C56 0.172(7) 0.070(4) 0.108(5) -0.010(4) -0.014(5) 0.035(4) C57 0.110(4) 0.078(4) 0.069(3) 0.014(3) -0.008(3) 0.025(4) Cl1 0.0675(7) 0.0776(8) 0.0690(7) -0.0157(7) 0.0122(6) -0.0006(7) O13 0.249(7) 0.094(3) 0.147(5) -0.026(3) 0.040(5) 0.009(4) O14 0.219(5) 0.223(6) 0.249(5) -0.126(4) 0.163(4) -0.060(5) O15 0.376(11) 0.176(6) 0.148(5) 0.054(5) -0.041(7) 0.062(7) O16 0.117(4) 0.214(7) 0.227(7) 0.026(6) 0.006(5) -0.046(4) O23 0.140(3) 0.153(4) 0.166(3) 0.062(3) 0.112(2) 0.053(3) O24 0.155(4) 0.102(3) 0.208(5) 0.037(4) 0.054(4) -0.016(3) O25 0.126(4) 0.193(5) 0.182(5) 0.074(4) 0.066(3) 0.066(4) O26 0.300(9) 0.330(9) 0.180(6) -0.102(6) 0.045(6) -0.163(7) O33 0.147(3) 0.148(4) 0.165(4) 0.006(3) 0.074(3) -0.066(3) O34 0.239(6) 0.109(5) 0.130(4) -0.063(4) 0.139(4) -0.080(5) O35 0.130(5) 0.058(4) 0.117(4) -0.015(3) 0.066(4) 0.006(4) O36 0.165(9) 0.106(7) 0.216(11) 0.025(7) -0.023(8) -0.006(6) O34' 0.190(13) 0.291(16) 0.251(15) 0.181(12) 0.095(12) 0.122(12) O35' 0.41(3) 0.296(17) 0.212(13) -0.198(11) 0.040(17) -0.02(2) O36' 0.082(6) 0.139(10) 0.185(11) -0.031(9) 0.049(7) 0.044(6) Cl4 0.0752(8) 0.0802(9) 0.0923(10) -0.0079(8) 0.0188(8) 0.0024(8) O43 0.177(5) 0.116(4) 0.103(3) -0.020(3) 0.021(3) 0.002(4) O44 0.265(5) 0.099(3) 0.215(5) -0.058(3) 0.153(4) -0.080(3) O45 0.120(4) 0.331(9) 0.227(7) -0.099(6) -0.044(5) 0.101(5) O46 0.144(4) 0.132(4) 0.150(4) 0.033(3) 0.072(3) 0.010(3) Cl5 0.160(2) 0.165(2) 0.1049(15) 0.0029(15) 0.0037(14) -0.0019(17) O53 0.099(5) 0.174(7) 0.138(6) -0.104(5) -0.022(5) 0.027(5) O54 0.189(9) 0.396(16) 0.181(11) 0.073(11) 0.034(8) 0.173(9) O55 0.376(15) 0.053(5) 0.243(11) 0.001(6) 0.130(10) 0.032(7) O56 0.205(8) 0.093(5) 0.083(5) 0.018(4) 0.015(5) 0.068(5) O53' 0.178(13) 0.178(12) 0.288(16) 0.150(11) 0.088(12) 0.046(11) O54' 0.195(11) 0.43(3) 0.126(9) -0.099(13) 0.108(7) -0.147(14) O55' 0.59(4) 0.235(12) 0.326(17) 0.242(11) -0.09(2) -0.02(2) O56' 0.42(3) 0.253(18) 0.202(15) -0.156(13) 0.101(17) -0.03(2) O6W 0.137(3) 0.164(4) 0.136(3) 0.087(3) 0.062(3) 0.062(3) O7W 0.074(2) 0.066(2) 0.153(4) 0.018(3) 0.000(3) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O51 2.482(3) . yes La1 O42 2.523(3) . yes La1 O12 2.531(3) . yes La1 O32 2.536(3) . yes La1 O22 2.546(3) . yes La1 O1W 2.556(4) . yes La1 O4W 2.606(3) . yes La1 O3W 2.610(3) . yes La1 O2W 2.630(3) . yes Cu1 O21 1.931(3) . yes Cu1 O31 1.964(3) . yes Cu1 O11 1.984(3) . yes Cu1 O41 1.998(3) . yes Cu1 O5W 2.233(3) . yes O12 C11 1.228(4) . ? O11 C11 1.247(5) . ? N1 C17 1.326(6) . ? N1 C13 1.328(6) . ? N1 C12 1.474(5) . ? C11 C12 1.505(6) . ? C13 C14 1.384(7) . ? C14 C15 1.335(8) . ? C15 C16 1.371(9) . ? C16 C17 1.366(7) . ? O21 C21 1.257(4) . ? O22 C21 1.230(4) . ? N2 C23 1.316(6) . ? N2 C27 1.342(6) . ? N2 C22 1.473(5) . ? C21 C22 1.530(6) . ? C23 C24 1.364(7) . ? C24 C25 1.333(9) . ? C25 C26 1.352(8) . ? C26 C27 1.380(6) . ? O31 C31 1.266(4) . ? O32 C31 1.227(5) . ? N3 C33 1.317(8) . ? N3 C37 1.334(8) . ? N3 C32 1.490(5) . ? C31 C32 1.509(6) . ? C33 C34 1.403(11) . ? C34 C35 1.266(15) . ? C35 C36 1.349(15) . ? C36 C37 1.387(8) . ? O41 C41 1.256(5) . ? O42 C41 1.241(4) . ? N4 C43 1.323(6) . ? N4 C47 1.332(6) . ? N4 C42 1.473(5) . ? C41 C42 1.522(6) . ? C43 C44 1.348(8) . ? C44 C45 1.324(12) . ? C45 C46 1.384(11) . ? C46 C47 1.405(8) . ? O51 C51 1.244(5) . ? O52 C51 1.222(5) . ? N5 C57 1.314(7) . ? N5 C53 1.362(6) . ? N5 C52 1.456(6) . ? C51 C52 1.521(7) . ? C53 C54 1.350(8) . ? C54 C55 1.387(9) . ? C55 C56 1.348(9) . ? C56 C57 1.329(9) . ? Cl1 O15 1.322(7) . ? Cl1 O14 1.337(7) . ? Cl1 O16 1.365(6) . ? Cl1 O13 1.437(6) . ? Cl2 O26 1.281(8) . ? Cl2 O23 1.388(5) . ? Cl2 O25 1.404(5) . ? Cl2 O24 1.415(5) . ? Cl3 O36' 1.390(6) . ? Cl3 O35 1.403(4) . ? Cl3 O36 1.410(5) . ? Cl3 O35' 1.414(6) . ? Cl3 O34' 1.415(6) . ? Cl3 O33 1.419(4) . ? Cl3 O34 1.431(5) . ? Cl4 O45 1.373(7) . ? Cl4 O44 1.381(5) . ? Cl4 O46 1.408(6) . ? Cl4 O43 1.430(5) . ? Cl5 O53 1.397(5) . ? Cl5 O55' 1.410(7) . ? Cl5 O56 1.408(5) . ? Cl5 O54' 1.411(6) . ? Cl5 O55 1.417(6) . ? Cl5 O56' 1.420(7) . ? Cl5 O53' 1.422(7) . ? Cl5 O54 1.449(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O51 La1 O42 79.66(10) . . yes O51 La1 O12 149.77(10) . . yes O42 La1 O12 72.17(10) . . yes O51 La1 O32 130.19(10) . . yes O42 La1 O32 109.00(9) . . yes O12 La1 O32 71.15(10) . . yes O51 La1 O22 71.56(10) . . yes O42 La1 O22 68.72(10) . . yes O12 La1 O22 106.95(9) . . yes O32 La1 O22 67.24(10) . . yes O51 La1 O1W 90.89(12) . . yes O42 La1 O1W 68.80(12) . . yes O12 La1 O1W 69.07(11) . . yes O32 La1 O1W 138.61(12) . . yes O22 La1 O1W 136.21(12) . . yes O51 La1 O4W 73.41(10) . . yes O42 La1 O4W 140.23(10) . . yes O12 La1 O4W 136.40(10) . . yes O32 La1 O4W 70.08(9) . . yes O22 La1 O4W 75.22(9) . . yes O1W La1 O4W 138.82(10) . . yes O51 La1 O3W 70.36(11) . . yes O42 La1 O3W 124.63(11) . . yes O12 La1 O3W 117.60(11) . . yes O32 La1 O3W 126.03(11) . . yes O22 La1 O3W 135.44(10) . . yes O1W La1 O3W 66.38(11) . . yes O4W La1 O3W 72.49(11) . . yes O51 La1 O2W 134.98(10) . . yes O42 La1 O2W 137.41(10) . . yes O12 La1 O2W 67.49(10) . . yes O32 La1 O2W 70.26(11) . . yes O22 La1 O2W 136.26(11) . . yes O1W La1 O2W 84.33(13) . . yes O4W La1 O2W 81.21(11) . . yes O3W La1 O2W 66.77(11) . . yes O21 Cu1 O31 91.52(13) . . yes O21 Cu1 O11 177.01(11) . . yes O31 Cu1 O11 89.41(13) . . yes O21 Cu1 O41 89.21(13) . . yes O31 Cu1 O41 174.61(11) . . yes O11 Cu1 O41 89.60(12) . . yes O21 Cu1 O5W 93.74(11) . . yes O31 Cu1 O5W 95.05(11) . . yes O11 Cu1 O5W 89.01(11) . . yes O41 Cu1 O5W 90.24(11) . . yes C11 O12 La1 160.2(3) . . ? C11 O11 Cu1 111.7(3) . . ? C17 N1 C13 120.4(4) . . ? C17 N1 C12 119.8(4) . . ? C13 N1 C12 119.8(4) . . ? O12 C11 O11 126.2(4) . . ? O12 C11 C12 115.8(4) . . ? O11 C11 C12 118.0(3) . . ? N1 C12 C11 113.5(3) . . ? N1 C13 C14 120.1(5) . . ? C15 C14 C13 120.7(5) . . ? C14 C15 C16 118.0(5) . . ? C17 C16 C15 120.7(5) . . ? N1 C17 C16 120.1(5) . . ? C21 O21 Cu1 127.0(3) . . ? C21 O22 La1 141.2(3) . . ? C23 N2 C27 120.8(4) . . ? C23 N2 C22 119.5(4) . . ? C27 N2 C22 119.8(4) . . ? O22 C21 O21 128.9(4) . . ? O22 C21 C22 119.2(3) . . ? O21 C21 C22 111.9(3) . . ? N2 C22 C21 113.4(3) . . ? N2 C23 C24 120.2(5) . . ? C25 C24 C23 120.9(5) . . ? C24 C25 C26 118.9(5) . . ? C25 C26 C27 120.1(5) . . ? N2 C27 C26 119.1(5) . . ? C31 O31 Cu1 122.8(3) . . ? C31 O32 La1 146.1(3) . . ? C33 N3 C37 121.7(5) . . ? C33 N3 C32 118.1(5) . . ? C37 N3 C32 120.2(5) . . ? O32 C31 O31 127.8(4) . . ? O32 C31 C32 121.0(3) . . ? O31 C31 C32 111.2(3) . . ? N3 C32 C31 113.3(3) . . ? N3 C33 C34 116.3(8) . . ? C35 C34 C33 123.8(10) . . ? C34 C35 C36 118.5(8) . . ? C35 C36 C37 119.4(8) . . ? N3 C37 C36 119.2(8) . . ? C41 O41 Cu1 118.2(2) . . ? C41 O42 La1 150.6(3) . . ? C43 N4 C47 120.9(4) . . ? C43 N4 C42 119.6(4) . . ? C47 N4 C42 119.5(4) . . ? O42 C41 O41 127.0(4) . . ? O42 C41 C42 114.8(4) . . ? O41 C41 C42 118.2(3) . . ? N4 C42 C41 114.0(3) . . ? N4 C43 C44 120.5(6) . . ? C45 C44 C43 120.9(7) . . ? C44 C45 C46 120.5(6) . . ? C45 C46 C47 116.8(6) . . ? N4 C47 C46 120.2(5) . . ? C51 O51 La1 139.5(3) . . ? C57 N5 C53 119.9(4) . . ? C57 N5 C52 121.9(4) . . ? C53 N5 C52 118.2(4) . . ? O52 C51 O51 127.7(4) . . ? O52 C51 C52 116.1(4) . . ? O51 C51 C52 116.2(4) . . ? N5 C52 C51 114.0(4) . . ? C54 C53 N5 119.4(5) . . ? C53 C54 C55 119.8(5) . . ? C56 C55 C54 118.2(6) . . ? C57 C56 C55 120.6(6) . . ? N5 C57 C56 121.8(5) . . ? O15 Cl1 O14 115.4(6) . . ? O15 Cl1 O16 112.4(6) . . ? O14 Cl1 O16 109.0(5) . . ? O15 Cl1 O13 106.1(4) . . ? O14 Cl1 O13 106.4(4) . . ? O16 Cl1 O13 107.0(4) . . ? O26 Cl2 O23 112.5(5) . . ? O26 Cl2 O25 108.6(5) . . ? O23 Cl2 O25 109.3(3) . . ? O26 Cl2 O24 109.0(5) . . ? O23 Cl2 O24 111.3(4) . . ? O25 Cl2 O24 106.0(4) . . ? O36' Cl3 O35 127.8(5) . . ? O36' Cl3 O36 57.0(5) . . ? O35 Cl3 O36 107.2(4) . . ? O36' Cl3 O35' 110.6(6) . . ? O35 Cl3 O35' 59.3(5) . . ? O36 Cl3 O35' 56.9(6) . . ? O36' Cl3 O34' 111.5(6) . . ? O35 Cl3 O34' 49.2(4) . . ? O36 Cl3 O34' 143.8(5) . . ? O35' Cl3 O34' 108.5(6) . . ? O36' Cl3 O33 114.1(4) . . ? O35 Cl3 O33 117.9(3) . . ? O36 Cl3 O33 110.0(4) . . ? O35' Cl3 O33 105.9(6) . . ? O34' Cl3 O33 106.0(5) . . ? O36' Cl3 O34 52.6(5) . . ? O35 Cl3 O34 105.6(4) . . ? O36 Cl3 O34 108.6(5) . . ? O35' Cl3 O34 146.8(6) . . ? O34' Cl3 O34 63.8(5) . . ? O33 Cl3 O34 107.2(3) . . ? O45 Cl4 O44 120.5(4) . . ? O45 Cl4 O46 108.4(4) . . ? O44 Cl4 O46 109.0(4) . . ? O45 Cl4 O43 105.0(4) . . ? O44 Cl4 O43 108.3(3) . . ? O46 Cl4 O43 104.4(4) . . ? O53 Cl5 O55' 98.5(6) . . ? O53 Cl5 O56 113.1(4) . . ? O55' Cl5 O56 135.4(7) . . ? O53 Cl5 O54' 132.8(5) . . ? O55' Cl5 O54' 109.7(6) . . ? O56 Cl5 O54' 71.2(5) . . ? O53 Cl5 O55 117.6(5) . . ? O55' Cl5 O55 81.4(5) . . ? O56 Cl5 O55 108.4(5) . . ? O54' Cl5 O55 37.3(5) . . ? O53 Cl5 O56' 23.8(5) . . ? O55' Cl5 O56' 109.9(6) . . ? O56 Cl5 O56' 111.6(5) . . ? O54' Cl5 O56' 109.0(5) . . ? O55 Cl5 O56' 97.8(6) . . ? O53 Cl5 O53' 93.7(5) . . ? O55' Cl5 O53' 110.0(6) . . ? O56 Cl5 O53' 40.6(5) . . ? O54' Cl5 O53' 110.2(5) . . ? O55 Cl5 O53' 145.3(6) . . ? O56' Cl5 O53' 108.0(6) . . ? O53 Cl5 O54 105.4(5) . . ? O55' Cl5 O54 29.0(6) . . ? O56 Cl5 O54 109.0(6) . . ? O54' Cl5 O54 117.7(6) . . ? O55 Cl5 O54 102.5(5) . . ? O56' Cl5 O54 125.4(5) . . ? O53' Cl5 O54 81.4(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 H1WB O56 1.13 1.59 2.621(7) 148.4 . O1W H1WB O53' 1.13 1.86 2.952(9) 160.4 . O2W H2WA O36' 1.04 2.05 2.973(6) 146.5 . O2W H2WA O12 1.04 2.31 2.868(4) 111.9 . O2W H2WB O6W 0.97 1.94 2.779(6) 143.1 . O3W H3WA O52 1.07 1.67 2.718(4) 164.9 5 O3W H3WB O6W 0.95 2.64 3.106(6) 110.8 . O4W H4WA O52 1.14 1.67 2.668(5) 142.6 . O4W H4WB O55 1.08 1.92 2.909(7) 151.4 1_545 O5W H5WA O7W 1.05 1.66 2.683(5) 163.1 . O6W H6WA O15 0.95 2.11 2.935(9) 144.5 7 O6W H6WB O56' 1.13 1.95 3.063(10) 166.6 . O6W H6WB O53 1.13 1.98 3.098(8) 170.9 . O7W H7WA O43 1.09 2.03 3.087(7) 161.0 1_545 O6W H6WA O15 0.95 2.11 2.935(9) 144.5 7 O6W H6WB O56' 1.13 1.95 3.063(10) 166.6 . O6W H6WB O53 1.13 1.98 3.098(8) 170.9 . _diffrn_measured_fraction_theta_max 0.409 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.409 _refine_diff_density_max 1.886 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.113 #===========================================================END data_complex_1.Nd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H49 Cl5 Cu N5 Nd O37' _chemical_formula_weight 1516.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.51(2) _cell_length_b 11.172(3) _cell_length_c 27.557(14) _cell_angle_alpha 90.00 _cell_angle_beta 104.810(10) _cell_angle_gamma 90.00 _cell_volume 11166(9) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6112 _exptl_absorpt_coefficient_mu 1.648 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.583 _exptl_absorpt_correction_T_max 0.971 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 120 _diffrn_standards_decay_% 1.2 _diffrn_reflns_number 9967 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9788 _reflns_number_gt 6205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+50.6729P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000106(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9788 _refine_ls_number_parameters 786 _refine_ls_number_restraints 177 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1560 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.069 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.106208(7) 0.06300(3) 0.072663(9) 0.04120(7) Uani 1 d . . . Cu1 Cu 0.189062(15) -0.01399(5) 0.17361(2) 0.03802(16) Uani 1 d . . . O1W O 0.10610(12) 0.2829(4) 0.07353(17) 0.0905(17) Uani 1 d . . . H1WA H 0.1220 0.3141 0.1003 0.100 Uiso 1 d R . . H1WB H 0.0828 0.3482 0.0642 0.100 Uiso 1 d R . . O2W O 0.12955(11) 0.0902(4) -0.00553(13) 0.0728(14) Uani 1 d . . . H2WA H 0.1575 0.0966 0.0106 0.100 Uiso 1 d R . . H2WB H 0.1098 0.1183 -0.0326 0.100 Uiso 1 d R . . O3W O 0.05861(10) 0.1543(4) -0.00068(14) 0.0756(14) Uani 1 d . . . H3WA H 0.0310 0.1246 -0.0138 0.100 Uiso 1 d R . . H3WB H 0.0588 0.2325 -0.0133 0.100 Uiso 1 d R . . O4W O 0.07110(10) -0.1020(3) 0.01983(13) 0.0581(11) Uani 1 d . . . H4WA H 0.0446 -0.1301 0.0288 0.100 Uiso 1 d R . . H4WB H 0.0832 -0.1882 0.0196 0.100 Uiso 1 d R . . O5W O 0.23707(9) -0.0618(4) 0.23686(13) 0.0594(11) Uani 1 d . . . H5WA H 0.2495 -0.1453 0.2378 0.100 Uiso 1 d R . . H5WB H 0.2551 -0.0002 0.2331 0.100 Uiso 1 d R . . O12 O 0.16952(9) 0.1426(3) 0.09210(13) 0.0537(11) Uani 1 d . . . O11 O 0.22045(9) 0.1014(3) 0.15035(12) 0.0503(10) Uani 1 d . . . N1 N 0.26126(10) 0.2606(4) 0.11607(14) 0.0435(11) Uani 1 d . . . C11 C 0.20261(13) 0.1561(5) 0.11318(18) 0.0446(14) Uani 1 d . . . C12 C 0.22182(13) 0.2515(5) 0.09152(18) 0.0499(15) Uani 1 d . . . H12A H 0.2194 0.2357 0.0570 0.100 Uiso 1 d R . . H12B H 0.2105 0.3265 0.0941 0.100 Uiso 1 d R . . C13 C 0.28571(16) 0.2131(6) 0.0961(2) 0.069(2) Uani 1 d . . . H13 H 0.2781 0.1704 0.0654 0.100 Uiso 1 d R . . C14 C 0.32206(17) 0.2148(7) 0.1183(2) 0.082(2) Uani 1 d . . . H14 H 0.3396 0.1841 0.1020 0.100 Uiso 1 d R . . C15 C 0.33355(16) 0.2719(7) 0.1629(2) 0.082(2) Uani 1 d . . . H15 H 0.3590 0.2758 0.1794 0.100 Uiso 1 d R . . C16 C 0.30836(18) 0.3217(7) 0.1832(2) 0.094(3) Uani 1 d . . . H16 H 0.3159 0.3534 0.2162 0.100 Uiso 1 d R . . C17 C 0.27193(16) 0.3169(6) 0.1595(2) 0.073(2) Uani 1 d . . . H17 H 0.2547 0.3571 0.1738 0.100 Uiso 1 d R . . O21 O 0.15603(9) -0.1217(3) 0.19444(12) 0.0499(10) Uani 1 d . . . O22 O 0.10454(9) -0.0995(3) 0.13309(12) 0.0510(11) Uani 1 d . . . N2 N 0.06885(11) -0.2697(4) 0.17174(15) 0.0459(12) Uani 1 d . . . C21 C 0.12353(13) -0.1455(4) 0.17084(17) 0.0425(14) Uani 1 d . . . C22 C 0.10750(14) -0.2444(5) 0.19644(19) 0.0529(16) Uani 1 d . . . H22A H 0.1214 -0.3151 0.1957 0.100 Uiso 1 d R . . H22B H 0.1097 -0.2246 0.2306 0.100 Uiso 1 d R . . C23 C 0.05976(16) -0.3269(5) 0.1290(2) 0.0645(18) Uani 1 d . . . H23 H 0.0785 -0.3550 0.1144 0.100 Uiso 1 d R . . C24 C 0.0232(2) -0.3478(7) 0.1058(3) 0.094(3) Uani 1 d . . . H24 H 0.0172 -0.3817 0.0732 0.100 Uiso 1 d R . . C25 C -0.00292(17) -0.3146(7) 0.1280(3) 0.087(3) Uani 1 d . . . H25 H -0.0276 -0.3384 0.1135 0.100 Uiso 1 d R . . C26 C 0.00660(17) -0.2561(6) 0.1711(3) 0.082(2) Uani 1 d . . . H26 H -0.0120 -0.2277 0.1859 0.100 Uiso 1 d R . . C27 C 0.04294(15) -0.2334(6) 0.1935(2) 0.0643(18) Uani 1 d . . . H27 H 0.0494 -0.1915 0.2244 0.100 Uiso 1 d R . . O31 O 0.19936(9) -0.1315(3) 0.12723(12) 0.0496(10) Uani 1 d . . . O32 O 0.14870(9) -0.1015(3) 0.06603(12) 0.0510(10) Uani 1 d . . . N3 N 0.16745(13) -0.2780(5) 0.00818(17) 0.0695(16) Uani 1 d . . . C31 C 0.17806(13) -0.1503(4) 0.08474(16) 0.0421(14) Uani 1 d . . . C32 C 0.19287(14) -0.2429(5) 0.05622(18) 0.0517(16) Uani 1 d . . . H32A H 0.2154 -0.2151 0.0506 0.100 Uiso 1 d R . . H32B H 0.1979 -0.3134 0.0761 0.100 Uiso 1 d R . . C33 C 0.1592(2) -0.3894(7) -0.0024(3) 0.120(3) Uani 1 d . . . H33 H 0.1682 -0.4485 0.0225 0.100 Uiso 1 d R . . C34 C 0.1377(3) -0.4201(11) -0.0470(4) 0.268(5) Uani 1 d . . . H34 H 0.1325 -0.4999 -0.0586 0.100 Uiso 1 d R . . C35 C 0.1229(3) -0.3490(12) -0.0797(4) 0.231(5) Uani 1 d . . . H35 H 0.1058 -0.3657 -0.1107 0.100 Uiso 1 d R . . C36 C 0.1298(2) -0.2278(12) -0.0715(3) 0.144(5) Uani 1 d . . . H36 H 0.1196 -0.1665 -0.0948 0.100 Uiso 1 d R . . C37 C 0.15374(18) -0.1934(8) -0.0257(2) 0.089(3) Uani 1 d . . . H37 H 0.1608 -0.1127 -0.0176 0.100 Uiso 1 d R . . O41 O 0.17471(9) 0.1123(3) 0.21447(12) 0.0482(10) Uani 1 d . . . O42 O 0.12087(9) 0.1401(3) 0.15889(12) 0.0543(11) Uani 1 d . . . N4 N 0.15736(11) 0.2640(4) 0.28155(14) 0.0485(12) Uani 1 d . . . C41 C 0.14307(13) 0.1570(5) 0.19968(18) 0.0439(14) Uani 1 d . . . C42 C 0.12966(14) 0.2399(5) 0.23380(19) 0.0568(17) Uani 1 d . . . H42A H 0.1229 0.3140 0.2171 0.100 Uiso 1 d R . . H42B H 0.1083 0.2064 0.2411 0.100 Uiso 1 d R . . C43 C 0.16821(17) 0.1784(7) 0.3141(2) 0.074(2) Uani 1 d . . . H43 H 0.1565 0.1029 0.3067 0.100 Uiso 1 d R . . C44 C 0.1938(2) 0.2009(9) 0.3586(2) 0.123(4) Uani 1 d . . . H44 H 0.2020 0.1371 0.3815 0.100 Uiso 1 d R . . C45 C 0.2087(2) 0.3073(10) 0.3683(3) 0.137(4) Uani 1 d . . . H45 H 0.2259 0.3207 0.3996 0.100 Uiso 1 d R . . C46 C 0.1983(2) 0.3960(8) 0.3342(3) 0.117(3) Uani 1 d . . . H46 H 0.2099 0.4719 0.3414 0.100 Uiso 1 d R . . C47 C 0.17199(16) 0.3730(6) 0.2896(2) 0.074(2) Uani 1 d . . . H47 H 0.1637 0.4346 0.2656 0.100 Uiso 1 d R . . O51 O 0.04622(9) 0.0622(3) 0.08991(14) 0.0567(11) Uani 1 d . . . O52 O 0.01011(10) -0.0808(3) 0.04972(14) 0.0613(12) Uani 1 d . . . N5 N -0.00538(12) 0.1524(4) 0.12995(16) 0.0559(14) Uani 1 d . . . C51 C 0.01716(13) 0.0050(5) 0.07859(18) 0.0474(15) Uani 1 d . . . C52 C -0.01307(15) 0.0430(5) 0.1021(2) 0.0623(19) Uani 1 d . . . H52A H -0.0356 0.0522 0.0771 0.100 Uiso 1 d R . . H52B H -0.0162 -0.0192 0.1241 0.100 Uiso 1 d R . . C53 C 0.01582(17) 0.1526(6) 0.1772(2) 0.069(2) Uani 1 d . . . H53 H 0.0249 0.0782 0.1920 0.100 Uiso 1 d R . . C54 C 0.02481(17) 0.2534(7) 0.2030(2) 0.085(2) Uani 1 d . . . H54 H 0.0412 0.2525 0.2355 0.100 Uiso 1 d R . . C55 C 0.0109(2) 0.3571(7) 0.1829(3) 0.110(3) Uani 1 d . . . H55 H 0.0164 0.4296 0.2013 0.100 Uiso 1 d R . . C56 C -0.0109(3) 0.3576(7) 0.1339(3) 0.127(4) Uani 1 d . . . H56 H -0.0210 0.4307 0.1189 0.100 Uiso 1 d R . . C57 C -0.0182(2) 0.2530(7) 0.1092(3) 0.096(3) Uani 1 d . . . H57 H -0.0348 0.2518 0.0768 0.100 Uiso 1 d R . . Cl1 Cl 0.41844(5) 0.03071(15) 0.20175(6) 0.0727(5) Uani 1 d . . . O13 O 0.4182(2) -0.0960(6) 0.1983(2) 0.161(3) Uani 1 d U . . O14 O 0.3992(2) 0.0573(8) 0.2341(3) 0.230(3) Uani 1 d U . . O15 O 0.4063(3) 0.0696(8) 0.1552(3) 0.213(6) Uani 1 d U . . O16 O 0.4554(2) 0.0576(8) 0.2219(4) 0.198(4) Uani 1 d U . . Cl2 Cl 0.07729(4) 0.00163(16) -0.19283(6) 0.0727(5) Uani 1 d . . . O23 O 0.09674(15) 0.0215(6) -0.2277(2) 0.141(2) Uani 1 d U . . O24 O 0.07501(18) -0.1198(6) -0.1829(3) 0.149(3) Uani 1 d U . . O25 O 0.04119(16) 0.0394(7) -0.2114(3) 0.161(3) Uani 1 d U . . O26 O 0.0915(3) 0.0539(9) -0.1509(3) 0.214(5) Uani 1 d U . . Cl3 Cl 0.23758(4) -0.00072(15) -0.01260(6) 0.0737(4) Uiso 1 d D . . O33 O 0.26716(11) 0.0782(4) -0.0131(2) 0.135(2) Uani 1 d DU A 1 O34 O 0.2315(2) 0.0036(7) 0.03623(17) 0.140(3) Uani 0.60 d PDU A 1 O35 O 0.2424(2) -0.1217(4) -0.0225(3) 0.094(3) Uani 0.60 d PDU A 1 O36 O 0.20528(17) 0.0393(7) -0.0476(3) 0.165(6) Uani 0.60 d PDU A 1 O34' O 0.2530(3) -0.0990(6) 0.0182(4) 0.256(11) Uani 0.40 d PDU A 2 O35' O 0.2227(4) -0.0386(10) -0.0625(2) 0.254(13) Uani 0.40 d PDU A 2 O36' O 0.21009(16) 0.0542(8) 0.0057(3) 0.125(6) Uani 0.40 d PDU A 2 Cl4 Cl 0.17624(5) 0.50818(18) 0.15885(7) 0.0844(6) Uani 1 d . . . O43 O 0.1840(2) 0.5609(5) 0.2064(2) 0.141(3) Uani 1 d . . . O44 O 0.1739(2) 0.3864(6) 0.1649(3) 0.190(3) Uani 1 d . . . O45 O 0.1486(2) 0.5714(10) 0.1296(3) 0.228(4) Uani 1 d . . . O46 O 0.20727(18) 0.5301(6) 0.1418(3) 0.160(3) Uani 1 d . . . Cl5 Cl 0.05856(7) 0.5320(2) 0.00107(9) 0.1662(14) Uani 1 d D . . O53 O 0.0602(2) 0.4553(6) -0.0375(2) 0.169(4) Uani 0.60 d PDU B 1 O54 O 0.02042(14) 0.5734(8) -0.0099(4) 0.180(4) Uani 0.60 d PDU B 1 O55 O 0.0779(2) 0.6431(5) 0.0029(4) 0.180(4) Uani 0.60 d PDU B 1 O56 O 0.0685(3) 0.4786(7) 0.0488(2) 0.180(4) Uani 0.60 d PDU B 1 O53' O 0.0461(3) 0.4556(8) 0.0346(3) 0.250(7) Uani 0.40 d PDU B 2 O54' O 0.0877(2) 0.6034(8) 0.0305(4) 0.250(7) Uani 0.40 d PDU B 2 O55' O 0.0306(2) 0.6065(8) -0.0279(4) 0.250(7) Uani 0.40 d PDU B 2 O56' O 0.0732(2) 0.4592(8) -0.0316(3) 0.250(7) Uani 0.40 d PDU B 2 O6W O 0.09718(16) 0.2455(6) -0.0799(2) 0.157(3) Uani 1 d . . . H6WA H 0.0877 0.2857 -0.1103 0.100 Uiso 1 d R . . H6WB H 0.0864 0.3202 -0.0605 0.100 Uiso 1 d R . . O7W O 0.25490(13) -0.2904(4) 0.23080(19) 0.103(2) Uani 1 d . . . H7WA H 0.2290 -0.3334 0.2300 0.100 Uiso 1 d R . . H7WB H 0.2487 -0.2183 0.2323 0.100 Uiso 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 Nd1 0.03319(12) 0.04674(15) 0.03980(12) 0.00466(13) 0.00225(10) -0.00334(14) Cu1 0.0348(3) 0.0415(3) 0.0366(3) 0.0028(2) 0.0072(2) -0.0026(3) O1W 0.082(3) 0.054(2) 0.106(3) 0.005(2) -0.029(3) 0.007(2) O2W 0.063(2) 0.100(3) 0.053(2) 0.021(2) 0.0102(18) 0.004(2) O3W 0.050(2) 0.082(3) 0.079(3) 0.033(2) -0.011(2) -0.013(2) O4W 0.0470(19) 0.064(2) 0.061(2) -0.0121(19) 0.0096(16) -0.0106(18) O5W 0.0492(19) 0.068(2) 0.058(2) 0.0148(19) 0.0079(16) 0.013(2) O12 0.0397(17) 0.058(2) 0.060(2) 0.0037(18) 0.0065(15) -0.0109(18) O11 0.0433(18) 0.057(2) 0.0484(18) 0.0115(16) 0.0071(15) -0.0076(17) N1 0.041(2) 0.044(2) 0.046(2) 0.0023(18) 0.0111(17) -0.0110(19) C11 0.044(2) 0.044(3) 0.051(3) 0.000(2) 0.021(2) -0.008(2) C12 0.044(3) 0.053(3) 0.052(3) 0.008(2) 0.012(2) -0.018(3) C13 0.062(3) 0.080(4) 0.065(3) -0.021(3) 0.017(3) -0.002(3) C14 0.051(3) 0.118(6) 0.082(4) -0.018(4) 0.025(3) 0.004(4) C15 0.040(3) 0.123(6) 0.077(4) -0.015(4) 0.003(3) -0.014(4) C16 0.067(4) 0.145(6) 0.064(4) -0.041(4) 0.005(3) -0.023(4) C17 0.055(3) 0.107(5) 0.057(3) -0.031(3) 0.013(3) -0.005(4) O21 0.0496(18) 0.050(2) 0.0514(18) 0.0074(16) 0.0145(15) -0.0083(17) O22 0.055(2) 0.051(2) 0.0453(18) 0.0091(16) 0.0084(15) -0.0067(17) N2 0.041(2) 0.044(2) 0.053(2) 0.0049(19) 0.0115(18) -0.007(2) C21 0.045(2) 0.037(3) 0.047(2) 0.002(2) 0.014(2) -0.009(2) C22 0.044(3) 0.056(3) 0.059(3) 0.011(3) 0.012(2) -0.010(3) C23 0.071(3) 0.065(4) 0.063(3) -0.009(3) 0.028(3) -0.014(3) C24 0.092(5) 0.088(5) 0.087(5) -0.002(4) -0.003(4) -0.029(4) C25 0.041(3) 0.092(5) 0.120(5) 0.016(4) 0.008(3) -0.010(4) C26 0.058(3) 0.083(5) 0.113(5) 0.016(4) 0.040(3) 0.002(3) C27 0.064(3) 0.067(4) 0.070(3) 0.001(3) 0.031(3) -0.007(3) O31 0.0519(19) 0.051(2) 0.0449(17) -0.0014(16) 0.0099(15) 0.0035(18) O32 0.0534(19) 0.052(2) 0.0460(18) 0.0008(16) 0.0106(15) 0.0012(18) N3 0.055(3) 0.096(4) 0.060(3) -0.028(3) 0.020(2) -0.007(3) C31 0.045(3) 0.044(3) 0.037(2) 0.004(2) 0.010(2) 0.000(2) C32 0.048(3) 0.058(3) 0.048(3) -0.004(3) 0.011(2) 0.004(3) C33 0.114(6) 0.095(5) 0.148(6) -0.072(5) 0.028(5) -0.014(5) C34 0.105(7) 0.395(10) 0.292(8) -0.297(7) 0.031(6) -0.063(8) C35 0.094(7) 0.398(13) 0.188(7) -0.225(7) 0.014(6) -0.039(8) C36 0.084(5) 0.290(13) 0.057(4) -0.002(6) 0.016(4) 0.040(7) C37 0.077(4) 0.151(7) 0.037(3) 0.003(4) 0.011(3) 0.014(5) O41 0.0403(17) 0.056(2) 0.0464(17) -0.0072(16) 0.0067(14) -0.0028(17) O42 0.0493(19) 0.065(2) 0.0454(18) -0.0086(18) 0.0055(15) -0.0031(19) N4 0.047(2) 0.058(3) 0.042(2) -0.004(2) 0.0135(17) 0.006(2) C41 0.039(2) 0.043(3) 0.053(3) -0.001(2) 0.016(2) -0.004(2) C42 0.044(3) 0.072(4) 0.052(3) -0.016(3) 0.007(2) 0.000(3) C43 0.079(4) 0.093(5) 0.054(3) 0.004(3) 0.022(3) -0.003(4) C44 0.121(6) 0.198(9) 0.046(4) 0.012(5) 0.013(4) 0.056(6) C45 0.078(5) 0.239(10) 0.079(5) -0.068(6) -0.009(4) 0.024(6) C46 0.072(4) 0.137(6) 0.145(6) -0.092(5) 0.034(4) -0.038(4) C47 0.062(3) 0.072(4) 0.088(4) -0.024(3) 0.022(3) 0.000(3) O51 0.0345(17) 0.060(2) 0.071(2) -0.004(2) 0.0067(16) -0.0027(18) O52 0.0473(19) 0.063(2) 0.071(2) -0.010(2) 0.0115(17) -0.0094(19) N5 0.052(2) 0.063(3) 0.053(2) 0.004(2) 0.014(2) 0.012(2) C51 0.039(2) 0.051(3) 0.052(3) 0.023(2) 0.011(2) 0.003(3) C52 0.047(3) 0.063(4) 0.075(4) 0.006(3) 0.013(3) -0.004(3) C53 0.065(4) 0.075(4) 0.063(3) 0.009(3) 0.007(3) 0.007(3) C54 0.060(4) 0.122(6) 0.067(4) -0.031(4) 0.005(3) 0.006(4) C55 0.107(6) 0.080(5) 0.134(6) -0.037(5) 0.018(5) 0.000(5) C56 0.168(8) 0.068(5) 0.113(6) -0.005(5) -0.021(6) 0.032(6) C57 0.118(6) 0.077(5) 0.076(4) 0.007(4) -0.007(4) 0.031(5) Cl1 0.0719(9) 0.0764(11) 0.0687(9) -0.0170(8) 0.0161(7) 0.0010(8) O13 0.253(8) 0.104(5) 0.119(5) -0.017(4) 0.037(5) 0.018(5) O14 0.226(5) 0.245(8) 0.283(6) -0.147(5) 0.182(4) -0.073(6) O15 0.181(14) 0.162(7) 0.143(7) 0.043(6) -0.026(8) 0.065(8) O16 0.119(5) 0.238(9) 0.222(8) 0.033(7) 0.014(5) -0.053(6) Cl2 0.0698(9) 0.0717(10) 0.0806(9) 0.0049(8) 0.0268(7) -0.0010(9) O23 0.157(3) 0.131(5) 0.178(4) 0.052(3) 0.126(3) 0.042(4) O24 0.137(5) 0.102(4) 0.207(6) 0.058(4) 0.043(4) -0.007(4) O25 0.106(4) 0.188(6) 0.207(6) 0.064(5) 0.071(4) 0.055(4) O26 0.221(10) 0.276(9) 0.139(5) -0.108(5) 0.051(6) -0.141(8) O33 0.153(4) 0.134(5) 0.137(4) -0.010(4) 0.070(3) -0.060(4) O34 0.235(7) 0.109(6) 0.124(5) -0.050(4) 0.137(4) -0.082(6) O35 0.156(6) 0.036(4) 0.111(5) 0.000(4) 0.071(4) 0.021(4) O36 0.157(10) 0.085(7) 0.225(13) 0.001(8) -0.004(10) 0.002(7) O34' 0.193(16) 0.31(2) 0.29(2) 0.159(18) 0.114(15) 0.128(17) O35' 0.28(3) 0.259(19) 0.222(16) -0.115(13) 0.008(18) -0.01(2) O36' 0.084(8) 0.127(11) 0.162(12) -0.050(10) 0.027(8) 0.020(8) Cl4 0.0785(10) 0.0847(12) 0.0869(11) -0.0074(10) 0.0157(9) 0.0046(10) O43 0.184(6) 0.109(4) 0.119(4) -0.025(4) 0.021(4) -0.010(5) O44 0.205(6) 0.169(4) 0.251(6) -0.055(4) 0.122(5) -0.091(4) O45 0.123(5) 0.341(11) 0.175(7) -0.076(7) -0.045(5) 0.093(6) O46 0.166(5) 0.136(5) 0.214(5) 0.061(4) 0.115(4) 0.038(4) Cl5 0.147(2) 0.220(3) 0.1179(19) -0.007(2) 0.0076(18) 0.011(2) O53 0.097(6) 0.245(8) 0.136(5) -0.157(5) -0.020(5) 0.039(6) O54 0.245(8) 0.134(5) 0.144(5) 0.040(4) 0.015(6) 0.076(5) O55 0.245(8) 0.134(5) 0.144(5) 0.040(4) 0.015(6) 0.076(5) O56 0.245(8) 0.134(5) 0.144(5) 0.040(4) 0.015(6) 0.076(5) O53' 0.248(15) 0.268(13) 0.156(8) 0.102(8) 0.076(9) 0.048(11) O54' 0.248(15) 0.268(13) 0.156(8) 0.102(8) 0.076(9) 0.048(11) O55' 0.248(15) 0.268(13) 0.156(8) 0.102(8) 0.076(9) 0.048(11) O56' 0.248(15) 0.268(13) 0.156(8) 0.102(8) 0.076(9) 0.048(11) O6W 0.128(4) 0.191(5) 0.161(4) 0.106(4) 0.053(4) 0.065(4) O7W 0.084(3) 0.058(3) 0.150(4) 0.023(3) 0.001(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O51 2.416(4) . yes Nd1 O42 2.454(3) . yes Nd1 O1W 2.457(4) . yes Nd1 O12 2.464(4) . yes Nd1 O32 2.470(4) . yes Nd1 O22 2.475(3) . yes Nd1 O4W 2.505(4) . yes Nd1 O2W 2.543(4) . yes Nd1 O3W 2.543(4) . yes Cu1 O21 1.918(4) . yes Cu1 O31 1.938(4) . yes Cu1 O11 1.961(4) . yes Cu1 O41 1.964(4) . yes Cu1 O5W 2.228(3) . yes O12 C11 1.238(5) . ? O11 C11 1.233(5) . ? N1 C13 1.299(7) . ? N1 C17 1.321(7) . ? N1 C12 1.465(6) . ? C11 C12 1.494(7) . ? C13 C14 1.345(8) . ? C14 C15 1.354(9) . ? C15 C16 1.336(10) . ? C16 C17 1.356(8) . ? O21 C21 1.255(5) . ? O22 C21 1.214(5) . ? N2 C23 1.306(7) . ? N2 C27 1.328(7) . ? N2 C22 1.463(6) . ? C21 C22 1.516(7) . ? C23 C24 1.376(9) . ? C24 C25 1.333(11) . ? C25 C26 1.321(10) . ? C26 C27 1.369(8) . ? O31 C31 1.255(5) . ? O32 C31 1.219(6) . ? N3 C33 1.298(9) . ? N3 C37 1.336(9) . ? N3 C32 1.473(6) . ? C31 C32 1.490(7) . ? C33 C34 1.332(12) . ? C34 C35 1.221(18) . ? C35 C36 1.386(18) . ? C36 C37 1.404(9) . ? O41 C41 1.256(6) . ? O42 C41 1.230(5) . ? N4 C43 1.304(8) . ? N4 C47 1.330(8) . ? N4 C42 1.478(6) . ? C41 C42 1.496(8) . ? C43 C44 1.373(9) . ? C44 C45 1.312(14) . ? C45 C46 1.351(13) . ? C46 C47 1.391(9) . ? O51 C51 1.233(6) . ? O52 C51 1.230(6) . ? N5 C57 1.297(8) . ? N5 C53 1.340(7) . ? N5 C52 1.434(7) . ? C51 C52 1.503(8) . ? C53 C54 1.329(9) . ? C54 C55 1.333(11) . ? C55 C56 1.388(11) . ? C56 C57 1.345(11) . ? Cl1 O14 1.316(8) . ? Cl1 O15 1.321(9) . ? Cl1 O16 1.388(7) . ? Cl1 O13 1.418(7) . ? Cl2 O26 1.283(8) . ? Cl2 O23 1.366(6) . ? Cl2 O25 1.385(6) . ? Cl2 O24 1.391(6) . ? Cl3 O36' 1.399(6) . ? Cl3 O35 1.400(5) . ? Cl3 O35' 1.411(6) . ? Cl3 O36 1.415(6) . ? Cl3 O34' 1.418(6) . ? Cl3 O33 1.420(4) . ? Cl3 O34 1.422(5) . ? Cl4 O45 1.340(8) . ? Cl4 O44 1.376(7) . ? Cl4 O46 1.384(7) . ? Cl4 O43 1.399(6) . ? Cl5 O53 1.379(6) . ? Cl5 O56 1.404(6) . ? Cl5 O55' 1.414(7) . ? Cl5 O53' 1.420(7) . ? Cl5 O56' 1.423(7) . ? Cl5 O54' 1.427(7) . ? Cl5 O55 1.431(6) . ? Cl5 O54 1.460(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O51 Nd1 O42 78.48(12) . . yes O51 Nd1 O1W 89.89(15) . . yes O42 Nd1 O1W 68.92(14) . . yes O51 Nd1 O12 148.58(12) . . yes O42 Nd1 O12 72.41(12) . . yes O1W Nd1 O12 68.94(14) . . yes O51 Nd1 O32 131.52(12) . . yes O42 Nd1 O32 110.10(11) . . yes O1W Nd1 O32 138.37(14) . . yes O12 Nd1 O32 71.35(12) . . yes O51 Nd1 O22 71.32(12) . . yes O42 Nd1 O22 69.14(12) . . yes O1W Nd1 O22 136.60(14) . . yes O12 Nd1 O22 107.91(11) . . yes O32 Nd1 O22 68.39(12) . . yes O51 Nd1 O4W 74.56(13) . . yes O42 Nd1 O4W 140.86(12) . . yes O1W Nd1 O4W 137.71(13) . . yes O12 Nd1 O4W 136.61(12) . . yes O32 Nd1 O4W 70.28(12) . . yes O22 Nd1 O4W 75.59(12) . . yes O51 Nd1 O2W 134.99(12) . . yes O42 Nd1 O2W 137.58(13) . . yes O1W Nd1 O2W 83.73(16) . . yes O12 Nd1 O2W 67.63(12) . . yes O32 Nd1 O2W 69.97(13) . . yes O22 Nd1 O2W 136.97(13) . . yes O4W Nd1 O2W 80.74(13) . . yes O51 Nd1 O3W 69.99(13) . . yes O42 Nd1 O3W 124.53(13) . . yes O1W Nd1 O3W 66.68(13) . . yes O12 Nd1 O3W 118.03(13) . . yes O32 Nd1 O3W 125.09(13) . . yes O22 Nd1 O3W 134.06(12) . . yes O4W Nd1 O3W 71.05(13) . . yes O2W Nd1 O3W 66.59(14) . . yes O21 Cu1 O31 91.45(15) . . yes O21 Cu1 O11 176.81(14) . . yes O31 Cu1 O11 89.56(15) . . yes O21 Cu1 O41 89.23(15) . . yes O31 Cu1 O41 173.88(13) . . yes O11 Cu1 O41 89.45(15) . . yes O21 Cu1 O5W 94.04(14) . . yes O31 Cu1 O5W 95.51(14) . . yes O11 Cu1 O5W 88.87(14) . . yes O41 Cu1 O5W 90.51(14) . . yes C11 O12 Nd1 160.3(3) . . yes C11 O11 Cu1 110.7(3) . . yes C13 N1 C17 119.8(5) . . ? C13 N1 C12 121.0(4) . . ? C17 N1 C12 119.2(5) . . ? O11 C11 O12 126.6(5) . . ? O11 C11 C12 118.1(4) . . ? O12 C11 C12 115.3(4) . . ? N1 C12 C11 113.5(4) . . ? N1 C13 C14 123.0(6) . . ? C13 C14 C15 118.1(6) . . ? C16 C15 C14 118.8(6) . . ? C15 C16 C17 121.0(6) . . ? N1 C17 C16 119.3(6) . . ? C21 O21 Cu1 126.5(3) . . yes C21 O22 Nd1 140.9(3) . . yes C23 N2 C27 120.2(5) . . ? C23 N2 C22 120.9(5) . . ? C27 N2 C22 118.9(4) . . ? O22 C21 O21 129.4(5) . . ? O22 C21 C22 119.4(4) . . ? O21 C21 C22 111.2(4) . . ? N2 C22 C21 112.8(4) . . ? N2 C23 C24 120.0(6) . . ? C25 C24 C23 120.2(7) . . ? C26 C25 C24 119.2(6) . . ? C25 C26 C27 120.4(7) . . ? N2 C27 C26 119.9(6) . . ? C31 O31 Cu1 122.8(3) . . yes C31 O32 Nd1 146.3(3) . . yes C33 N3 C37 119.7(6) . . ? C33 N3 C32 121.3(6) . . ? C37 N3 C32 119.0(5) . . ? O32 C31 O31 127.7(5) . . ? O32 C31 C32 120.4(4) . . ? O31 C31 C32 112.0(4) . . ? N3 C32 C31 114.6(4) . . ? N3 C33 C34 120.5(9) . . ? C35 C34 C33 124.5(12) . . ? C34 C35 C36 119.0(10) . . ? C35 C36 C37 117.6(9) . . ? N3 C37 C36 118.5(9) . . ? C41 O41 Cu1 118.3(3) . . yes C41 O42 Nd1 150.5(3) . . yes C43 N4 C47 120.9(5) . . ? C43 N4 C42 120.2(5) . . ? C47 N4 C42 118.8(5) . . ? O42 C41 O41 126.8(5) . . ? O42 C41 C42 114.3(4) . . ? O41 C41 C42 118.9(4) . . ? N4 C42 C41 113.6(4) . . ? N4 C43 C44 120.3(7) . . ? C45 C44 C43 120.8(8) . . ? C44 C45 C46 119.4(7) . . ? C45 C46 C47 119.5(8) . . ? N4 C47 C46 119.1(6) . . ? C51 O51 Nd1 139.5(4) . . yes C57 N5 C53 119.2(5) . . ? C57 N5 C52 120.1(5) . . ? C53 N5 C52 120.6(5) . . ? O52 C51 O51 126.7(5) . . ? O52 C51 C52 115.9(5) . . ? O51 C51 C52 117.4(5) . . ? N5 C52 C51 113.6(5) . . ? C54 C53 N5 121.9(6) . . ? C53 C54 C55 119.6(6) . . ? C54 C55 C56 118.6(7) . . ? C57 C56 C55 118.8(7) . . ? N5 C57 C56 121.7(7) . . ? O14 Cl1 O15 118.1(7) . . ? O14 Cl1 O16 110.0(5) . . ? O15 Cl1 O16 112.3(7) . . ? O14 Cl1 O13 106.0(5) . . ? O15 Cl1 O13 105.6(5) . . ? O16 Cl1 O13 103.4(5) . . ? O26 Cl2 O23 112.8(5) . . ? O26 Cl2 O25 109.6(6) . . ? O23 Cl2 O25 109.7(4) . . ? O26 Cl2 O24 107.3(5) . . ? O23 Cl2 O24 111.6(4) . . ? O25 Cl2 O24 105.4(4) . . ? O35 Cl3 O36 107.7(4) . . ? O36' Cl3 O34' 110.5(6) . . ? O35' Cl3 O34' 110.5(6) . . ? O36' Cl3 O33 112.4(4) . . ? O35 Cl3 O33 117.3(4) . . ? O35' Cl3 O33 107.0(6) . . ? O36 Cl3 O33 109.4(4) . . ? O34' Cl3 O33 106.6(5) . . ? O35 Cl3 O34 106.0(4) . . ? O36 Cl3 O34 108.5(5) . . ? O33 Cl3 O34 107.6(4) . . ? O45 Cl4 O44 122.0(5) . . ? O45 Cl4 O46 106.9(5) . . ? O44 Cl4 O46 107.6(5) . . ? O45 Cl4 O43 106.6(5) . . ? O44 Cl4 O43 107.9(4) . . ? O46 Cl4 O43 104.7(5) . . ? O53 Cl5 O56 113.9(5) . . ? O55' Cl5 O53' 113.7(6) . . ? O55' Cl5 O56' 109.2(6) . . ? O53' Cl5 O56' 108.2(6) . . ? O55' Cl5 O54' 109.9(6) . . ? O53' Cl5 O54' 107.3(6) . . ? O56' Cl5 O54' 108.5(6) . . ? O53 Cl5 O55 116.3(6) . . ? O56 Cl5 O55 108.9(5) . . ? O53 Cl5 O54 105.9(5) . . ? O56 Cl5 O54 109.8(6) . . ? O55 Cl5 O54 101.1(5) . . ? 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 H1WB O56 1.12 1.57 2.597(9) 149.4 . O1W H1WB O53' 1.12 1.85 2.950(10) 167.2 . O2W H2WA O36' 1.03 2.07 2.985(7) 146.9 . O2W H2WA O12 1.03 2.23 2.787(5) 111.8 . O2W H2WB O6W 0.96 1.91 2.724(7) 141.7 . O3W H3WA O52 1.06 1.68 2.714(5) 164.5 5 O3W H3WB O6W 0.94 2.61 3.085(8) 111.8 . O4W H4WA O52 1.13 1.64 2.633(6) 143.3 . O4W H4WB O55 1.06 1.94 2.907(7) 149.7 1_545 O5W H5WA O7W 1.04 1.65 2.656(6) 161.0 . O6W H6WA O15 0.94 2.08 2.906(11) 146.0 7 O6W H6WB O56' 1.12 1.87 2.982(10) 171.6 . O6W H6WB O53 1.12 1.99 3.099(9) 169.7 . O7W H7WA O43 1.08 2.03 3.062(9) 159.6 1_545 O6W H6WA O15 0.94 2.08 2.906(11) 146.0 7 O6W H6WB O56' 1.12 1.87 2.982(10) 171.6 . O6W H6WB O53 1.12 1.99 3.099(9) 169.7 . _diffrn_measured_fraction_theta_max 0.471 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.471 _refine_diff_density_max 1.049 _refine_diff_density_min -1.155 _refine_diff_density_rms 0.126 #===========================================================END data_complex_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H94 Cl10 Cu3 N12 Nd2 O78' _chemical_formula_weight 3185.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.410(4) _cell_length_b 14.992(6) _cell_length_c 18.447(7) _cell_angle_alpha 73.380(10) _cell_angle_beta 72.140(10) _cell_angle_gamma 88.900(10) _cell_volume 2869.8(19) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedral _exptl_crystal_colour 'deep blue' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1599 _exptl_absorpt_coefficient_mu 1.789 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4682 _exptl_absorpt_correction_T_max 0.6158 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'Siemens R3' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 120 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.5 _diffrn_reflns_number 11282 _diffrn_reflns_av_R_equivalents 0.0127 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11263 _reflns_number_gt 8654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' __refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+4.3474P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11263 _refine_ls_number_parameters 826 _refine_ls_number_restraints 95 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1344 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 2.738 _refine_ls_shift/su_mean 0.040 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.017608(19) 0.152799(14) 0.325763(11) 0.02975(5) Uani 1 d . . . Cu1 Cu 0.15276(4) 0.31863(3) 0.12860(3) 0.03180(12) Uani 1 d . . . Cu2 Cu 0.0000 0.5000 0.0000 0.04105(19) Uani 1 d S . . O1W O 0.1565(3) 0.0884(2) 0.40273(17) 0.0515(9) Uani 1 d . . . H1WA H 0.2263 0.1263 0.3912 0.100 Uiso 1 d R . . H1WB H 0.1609 0.0287 0.4372 0.100 Uiso 1 d R . . O2W O -0.0152(3) -0.0175(2) 0.35312(19) 0.0525(9) Uani 1 d . . . H2WA H -0.0720 -0.0617 0.3930 0.100 Uiso 1 d R . . H2WB H 0.0454 -0.0576 0.3356 0.100 Uiso 1 d R . . O3W O -0.2112(3) 0.1314(2) 0.35774(19) 0.0591(10) Uani 1 d . . . H3WA H -0.2578 0.0955 0.3965 0.100 Uiso 1 d R . . H3WB H -0.2383 0.1397 0.3169 0.100 Uiso 1 d R . . O61 O -0.0553(3) 0.2261(2) 0.43867(16) 0.0464(8) Uani 1 d . . . O62 O -0.1017(3) 0.0788(2) 0.47874(16) 0.0467(8) Uani 1 d . . . O63 O -0.1265(4) 0.1553(3) 0.56461(18) 0.0707(12) Uani 1 d . . . N6 N -0.0946(3) 0.1535(3) 0.49548(19) 0.0416(10) Uani 1 d . . . O11 O 0.2376(3) 0.3767(2) 0.18293(16) 0.0425(8) Uani 1 d . . . O12 O 0.1856(3) 0.26715(19) 0.30068(16) 0.0419(8) Uani 1 d . . . C11 C 0.2331(3) 0.3441(3) 0.2543(2) 0.0348(10) Uani 1 d . . . C12 C 0.2985(4) 0.4088(3) 0.2809(2) 0.0466(12) Uani 1 d . . . H12A H 0.2768 0.4712 0.2611 0.100 Uiso 1 d R . . H12B H 0.3859 0.4078 0.2573 0.100 Uiso 1 d R . . N1 N 0.2706(3) 0.3861(2) 0.36757(19) 0.0390(9) Uani 1 d . . . C13 C 0.1553(4) 0.3622(3) 0.4166(3) 0.0492(13) Uani 1 d . . . H13A H 0.0898 0.3576 0.3950 0.100 Uiso 1 d R . . C14 C 0.1292(5) 0.3439(4) 0.4969(3) 0.0602(15) Uani 1 d . . . H14A H 0.0465 0.3252 0.5322 0.100 Uiso 1 d R . . C15 C 0.2231(6) 0.3528(4) 0.5258(3) 0.0654(16) Uani 1 d . . . H15A H 0.2071 0.3407 0.5821 0.100 Uiso 1 d R . . C16 C 0.3398(6) 0.3791(4) 0.4750(3) 0.0719(16) Uani 1 d . . . H16A H 0.4059 0.3868 0.4952 0.100 Uiso 1 d R . . C17 C 0.3625(5) 0.3940(4) 0.3963(3) 0.0587(14) Uani 1 d . . . H17A H 0.4454 0.4102 0.3607 0.100 Uiso 1 d R . . O21 O 0.0166(3) 0.40057(19) 0.15145(15) 0.0390(7) Uani 1 d . . . O22 O -0.0398(3) 0.3068(2) 0.27431(16) 0.0448(8) Uani 1 d . . . C21 C -0.0471(3) 0.3783(3) 0.2233(2) 0.0346(10) Uani 1 d . . . C22 C -0.1375(4) 0.4458(3) 0.2488(2) 0.0448(12) Uani 1 d . . . H22A H -0.2024 0.4472 0.2256 0.100 Uiso 1 d R . . H22B H -0.0967 0.5073 0.2298 0.100 Uiso 1 d R . . N2 N -0.1910(3) 0.4193(2) 0.3362(2) 0.0381(9) Uani 1 d . . . C23 C -0.2859(4) 0.3555(3) 0.3741(3) 0.0536(14) Uani 1 d . . . H23A H -0.3242 0.3288 0.3447 0.100 Uiso 1 d R . . C24 C -0.3288(5) 0.3283(4) 0.4567(3) 0.0661(18) Uani 1 d . . . H24A H -0.3975 0.2825 0.4847 0.100 Uiso 1 d R . . C25 C -0.2748(5) 0.3656(4) 0.4979(3) 0.0709(18) Uani 1 d . . . H25A H -0.3047 0.3467 0.5551 0.100 Uiso 1 d R . . C26 C -0.1795(6) 0.4290(4) 0.4584(3) 0.0684(16) Uani 1 d . . . H26A H -0.1395 0.4554 0.4871 0.100 Uiso 1 d R . . C27 C -0.1388(4) 0.4565(3) 0.3771(3) 0.0515(13) Uani 1 d . . . H27A H -0.0714 0.5034 0.3491 0.100 Uiso 1 d R . . O31 O 0.0559(3) 0.2494(2) 0.08751(17) 0.0473(8) Uani 1 d . . . O32 O -0.0330(3) 0.1538(2) 0.20842(16) 0.0476(8) Uani 1 d . . . C31 C -0.0100(4) 0.1795(3) 0.1352(2) 0.0408(11) Uani 1 d . . . C32 C -0.0706(5) 0.1216(3) 0.1003(3) 0.0568(14) Uani 1 d . . . H32A H -0.0157 0.1210 0.0493 0.100 Uiso 1 d R . . H32B H -0.1444 0.1488 0.0926 0.100 Uiso 1 d R . . N3 N -0.1013(3) 0.0266(2) 0.1524(2) 0.0450(10) Uani 1 d . . . C33 C -0.0137(6) -0.0324(4) 0.1487(4) 0.0737(19) Uani 1 d . . . H33A H 0.0654 -0.0127 0.1089 0.100 Uiso 1 d R . . C34 C -0.0324(7) -0.1201(4) 0.1995(5) 0.099(2) Uani 1 d . . . H34A H 0.0329 -0.1616 0.1978 0.100 Uiso 1 d R . . C35 C -0.1454(7) -0.1468(5) 0.2522(4) 0.101(2) Uani 1 d . . . H35A H -0.1621 -0.2091 0.2879 0.100 Uiso 1 d R . . C36 C -0.2348(6) -0.0888(5) 0.2560(4) 0.092(2) Uani 1 d . . . H36A H -0.3156 -0.1093 0.2937 0.100 Uiso 1 d R . . C37 C -0.2112(5) 0.0013(4) 0.2056(3) 0.0664(17) Uani 1 d . . . H37A H -0.2740 0.0448 0.2093 0.100 Uiso 1 d R . . O41 O 0.2790(3) 0.2301(2) 0.11588(18) 0.0511(9) Uani 1 d . . . O42 O 0.1961(3) 0.1184(2) 0.22983(18) 0.0484(9) Uani 1 d . . . C41 C 0.2774(4) 0.1542(3) 0.1668(2) 0.0396(10) Uani 1 d . . . C42 C 0.3924(4) 0.1031(3) 0.1436(3) 0.0442(12) Uani 1 d . . . H42A H 0.4640 0.1453 0.1277 0.100 Uiso 1 d R . . H42B H 0.3932 0.0827 0.0986 0.100 Uiso 1 d R . . N4 N 0.3990(3) 0.0220(2) 0.2090(2) 0.0387(9) Uani 1 d . . . C43 C 0.3847(5) -0.0647(3) 0.2053(3) 0.0624(15) Uani 1 d . . . H43A H 0.3680 -0.0746 0.1602 0.100 Uiso 1 d R . . C44 C 0.3940(6) -0.1389(4) 0.2659(4) 0.078(2) Uani 1 d . . . H44A H 0.3843 -0.2014 0.2636 0.100 Uiso 1 d R . . C45 C 0.4172(5) -0.1241(4) 0.3296(3) 0.0678(17) Uani 1 d . . . H45A H 0.4260 -0.1763 0.3715 0.100 Uiso 1 d R . . C46 C 0.4282(5) -0.0359(4) 0.3344(3) 0.0662(16) Uani 1 d . . . H46A H 0.4424 -0.0252 0.3800 0.100 Uiso 1 d R . . C47 C 0.4183(4) 0.0363(3) 0.2733(3) 0.0488(12) Uani 1 d . . . H47A H 0.4251 0.0989 0.2759 0.100 Uiso 1 d R . . O51 O 0.2495(2) 0.4175(2) 0.01568(15) 0.0412(8) Uani 1 d . . . O52 O 0.1439(3) 0.4650(2) -0.06962(17) 0.0469(8) Uani 1 d . . . C51 C 0.2379(4) 0.4374(3) -0.0499(2) 0.0324(10) Uani 1 d . . . C52 C 0.3466(4) 0.4324(4) -0.1208(3) 0.0572(14) Uani 1 d . . . H52A H 0.3725 0.4942 -0.1567 0.100 Uiso 1 d R . . H52B H 0.3207 0.3957 -0.1489 0.100 Uiso 1 d R . . N5 N 0.4511(3) 0.3911(3) -0.0964(2) 0.0448(10) Uani 1 d . . . C53 C 0.5328(5) 0.4445(3) -0.0873(3) 0.0544(14) Uani 1 d . . . H53A H 0.5241 0.5103 -0.0966 0.100 Uiso 1 d R . . C54 C 0.6299(5) 0.4055(4) -0.0644(3) 0.0672(17) Uani 1 d . . . H54A H 0.6899 0.4442 -0.0580 0.100 Uiso 1 d R . . C55 C 0.6414(4) 0.3131(4) -0.0506(3) 0.0641(17) Uani 1 d . . . H55A H 0.7098 0.2859 -0.0347 0.100 Uiso 1 d R . . C56 C 0.5554(4) 0.2582(4) -0.0595(3) 0.0578(15) Uani 1 d . . . H56A H 0.5623 0.1922 -0.0495 0.100 Uiso 1 d R . . C57 C 0.4608(4) 0.2984(3) -0.0824(3) 0.0541(14) Uani 1 d . . . H57A H 0.3998 0.2606 -0.0887 0.100 Uiso 1 d R . . Cl1 Cl 0.35203(11) 0.11470(9) 0.50992(7) 0.0586(3) Uani 1 d D . . O13 O 0.2314(4) 0.1288(3) 0.5561(3) 0.1037(18) Uani 1 d D . . O14 O 0.3650(4) 0.1617(4) 0.4298(2) 0.1128(18) Uani 1 d D . . O15 O 0.4394(4) 0.1523(3) 0.5334(3) 0.1107(16) Uani 1 d D . . O16 O 0.3591(4) 0.0183(3) 0.5210(3) 0.109(2) Uani 1 d D . . Cl2 Cl 0.29826(11) -0.00001(9) 0.97682(7) 0.0590(3) Uani 1 d D . . O23 O 0.2778(4) -0.0470(4) 1.0572(2) 0.126(2) Uani 1 d D . . O24 O 0.3885(4) 0.0720(4) 0.9522(4) 0.154(3) Uani 1 d D . . O25 O 0.3359(4) -0.0628(3) 0.9324(3) 0.1083(15) Uani 1 d D . . O26 O 0.1862(3) 0.0343(3) 0.9677(2) 0.0902(14) Uani 1 d D . . Cl3 Cl -0.36831(11) 0.27487(9) 0.19515(7) 0.0596(3) Uani 1 d D . . O33 O -0.3602(6) 0.1909(4) 0.2527(4) 0.105(2) Uani 0.60 d PD A 1 O34 O -0.3952(9) 0.3464(4) 0.2349(5) 0.145(4) Uani 0.60 d PD A 1 O35 O -0.4704(5) 0.2666(7) 0.1711(5) 0.182(3) Uani 0.60 d PD A 1 O36 O -0.2548(6) 0.3019(9) 0.1380(6) 0.219(7) Uani 0.60 d PD A 1 O33B O -0.3593(9) 0.1979(4) 0.1641(5) 0.105(2) Uani 0.40 d PD A 2 O34B O -0.4760(8) 0.2766(8) 0.2537(6) 0.145(4) Uani 0.40 d PD A 2 O35B O -0.3687(10) 0.3484(6) 0.1255(5) 0.182(3) Uani 0.40 d PD A 2 O36B O -0.2546(6) 0.2920(11) 0.2049(7) 0.219(7) Uani 0.40 d PD A 2 Cl4 Cl 0.40027(12) 0.37482(9) 0.68171(7) 0.0646(4) Uani 1 d D . . O43 O 0.4657(8) 0.3522(6) 0.6139(4) 0.160(3) Uani 0.60 d PD B 1 O44 O 0.2695(5) 0.3643(6) 0.6960(5) 0.109(3) Uani 0.60 d PD B 1 O45 O 0.4201(8) 0.4610(4) 0.6926(5) 0.112(3) Uani 0.60 d PD B 1 O46 O 0.4198(7) 0.3057(5) 0.7488(4) 0.129(3) Uani 0.60 d PD B 1 O43B O 0.4226(12) 0.2977(5) 0.6513(5) 0.160(3) Uani 0.40 d PD B 2 O44B O 0.2767(6) 0.3720(9) 0.7277(7) 0.109(3) Uani 0.40 d PD B 2 O45B O 0.4248(11) 0.4551(5) 0.6122(5) 0.112(3) Uani 0.40 d PD B 2 O46B O 0.4856(7) 0.3850(8) 0.7199(5) 0.129(3) Uani 0.40 d PD B 2 Cl5 Cl 0.13560(13) 0.64542(10) 0.29271(9) 0.0725(4) Uani 1 d D . . O53 O 0.0735(7) 0.6245(8) 0.2445(4) 0.155(4) Uani 0.50 d PD C 1 O54 O 0.1011(9) 0.5724(6) 0.3664(4) 0.139(3) Uani 0.50 d PD C 1 O55 O 0.2641(5) 0.6475(7) 0.2574(7) 0.160(4) Uani 0.50 d PD C 1 O56 O 0.1026(10) 0.7294(4) 0.3107(6) 0.153(5) Uani 0.50 d PD C 1 O53B O 0.1283(10) 0.5837(5) 0.2477(5) 0.155(4) Uani 0.50 d PD C 2 O54B O 0.1826(7) 0.5983(7) 0.3519(4) 0.139(3) Uani 0.50 d PD C 2 O55B O 0.2089(9) 0.7256(5) 0.2389(6) 0.160(4) Uani 0.50 d PD C 2 O56B O 0.0148(6) 0.6731(6) 0.3192(7) 0.153(5) Uani 0.50 d PD C 2 O4W O 0.0972(3) 0.6020(2) 0.0008(2) 0.0569(10) Uani 1 d . . . H4WA H 0.0751 0.6298 0.0377 0.100 Uiso 1 d R . . H4WB H 0.1621 0.6284 -0.0414 0.100 Uiso 1 d R . . O5W O 0.0340(4) 0.6997(3) 0.1010(3) 0.1041(15) Uani 1 d . . . H5WA H 0.0040 0.6491 0.1418 0.100 Uiso 1 d R . . H5WB H -0.0429 0.7203 0.1075 0.100 Uiso 1 d R . . O6W O -0.1879(5) 0.7676(4) 0.0999(5) 0.170(3) Uani 1 d U . . H6WA H -0.1779 0.7519 0.0538 0.100 Uiso 1 d R . . H6WB H -0.2158 0.7480 0.1565 0.100 Uiso 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 Nd1 0.03578(10) 0.02669(9) 0.02464(8) -0.00162(7) -0.01202(7) 0.00321(8) Cu1 0.0372(2) 0.0307(2) 0.0249(2) -0.00274(17) -0.01138(17) 0.00693(19) Cu2 0.0358(3) 0.0447(4) 0.0481(4) -0.0181(3) -0.0172(3) 0.0126(3) O1W 0.0558(16) 0.0437(17) 0.0506(15) 0.0100(13) -0.0323(13) -0.0045(14) O2W 0.0659(19) 0.0330(15) 0.0579(17) -0.0079(13) -0.0230(15) -0.0003(14) O3W 0.0449(16) 0.075(2) 0.0480(17) 0.0000(16) -0.0183(14) -0.0075(16) O61 0.0602(18) 0.0367(15) 0.0326(14) -0.0033(12) -0.0073(13) 0.0015(14) O62 0.0593(17) 0.0377(15) 0.0367(14) -0.0006(12) -0.0151(13) -0.0024(14) O63 0.095(3) 0.073(2) 0.0299(15) -0.0105(16) -0.0033(17) 0.011(2) N6 0.0458(19) 0.0445(19) 0.0305(16) -0.0070(14) -0.0105(14) 0.0091(16) O11 0.0502(15) 0.0414(15) 0.0334(13) -0.0036(12) -0.0161(12) -0.0022(13) O12 0.0515(15) 0.0350(14) 0.0361(13) -0.0007(11) -0.0182(12) -0.0064(13) C11 0.0332(18) 0.036(2) 0.0319(18) -0.0061(15) -0.0096(15) 0.0062(16) C12 0.056(2) 0.049(2) 0.0349(19) -0.0069(17) -0.0188(18) -0.016(2) N1 0.0444(18) 0.0354(17) 0.0384(16) -0.0093(14) -0.0157(14) -0.0034(15) C13 0.048(2) 0.051(2) 0.049(2) -0.015(2) -0.0147(19) -0.003(2) C14 0.067(3) 0.060(3) 0.050(2) -0.023(2) -0.005(2) -0.005(3) C15 0.105(4) 0.060(3) 0.038(2) -0.018(2) -0.027(2) 0.009(3) C16 0.092(3) 0.078(4) 0.068(3) -0.030(2) -0.049(2) 0.014(3) C17 0.055(2) 0.071(3) 0.063(3) -0.027(2) -0.029(2) -0.002(2) O21 0.0438(15) 0.0391(15) 0.0281(12) -0.0040(11) -0.0087(11) 0.0110(12) O22 0.0527(16) 0.0356(15) 0.0357(14) -0.0005(12) -0.0093(13) 0.0161(13) C21 0.0354(18) 0.0314(19) 0.0373(18) -0.0073(15) -0.0147(15) 0.0069(16) C22 0.051(2) 0.041(2) 0.037(2) -0.0050(17) -0.0117(18) 0.0192(19) N2 0.0366(16) 0.0340(17) 0.0421(17) -0.0097(14) -0.0118(14) 0.0095(14) C23 0.038(2) 0.054(3) 0.062(3) -0.013(2) -0.012(2) 0.002(2) C24 0.048(3) 0.063(3) 0.061(3) 0.006(3) -0.002(2) -0.004(3) C25 0.079(4) 0.078(4) 0.047(3) -0.016(3) -0.010(3) 0.025(3) C26 0.093(4) 0.064(3) 0.066(3) -0.037(2) -0.033(3) 0.023(3) C27 0.053(3) 0.043(2) 0.061(3) -0.019(2) -0.019(2) 0.010(2) O31 0.0612(17) 0.0398(16) 0.0417(14) -0.0059(12) -0.0226(13) -0.0034(14) O32 0.0607(17) 0.0517(17) 0.0344(13) -0.0078(12) -0.0250(12) -0.0007(15) C31 0.050(2) 0.041(2) 0.0393(19) -0.0133(16) -0.0230(17) 0.0105(18) C32 0.081(3) 0.050(3) 0.045(2) -0.010(2) -0.032(2) -0.007(2) N3 0.055(2) 0.0426(18) 0.0421(17) -0.0181(14) -0.0170(15) 0.0011(17) C33 0.070(4) 0.068(3) 0.077(3) -0.032(3) -0.004(3) 0.013(3) C34 0.121(5) 0.047(3) 0.139(6) -0.032(3) -0.052(4) 0.026(3) C35 0.133(5) 0.057(4) 0.113(5) 0.006(3) -0.065(4) -0.019(4) C36 0.073(4) 0.114(5) 0.068(4) 0.000(4) -0.016(3) -0.040(4) C37 0.044(3) 0.089(4) 0.065(3) -0.022(3) -0.016(2) 0.002(3) O41 0.0535(17) 0.0471(17) 0.0450(16) -0.0043(13) -0.0143(13) 0.0222(14) O42 0.0419(15) 0.0520(17) 0.0468(16) -0.0127(13) -0.0101(13) 0.0169(14) C41 0.042(2) 0.043(2) 0.0436(19) -0.0199(16) -0.0210(16) 0.0174(17) C42 0.043(2) 0.045(2) 0.040(2) -0.0076(18) -0.0132(17) 0.0181(19) N4 0.0333(16) 0.0407(18) 0.0423(17) -0.0111(14) -0.0137(13) 0.0109(14) C43 0.068(3) 0.053(3) 0.079(3) -0.026(2) -0.035(2) 0.018(2) C44 0.084(4) 0.047(3) 0.099(4) -0.013(3) -0.031(3) 0.011(3) C45 0.068(3) 0.054(3) 0.066(3) 0.007(3) -0.023(3) 0.013(3) C46 0.070(3) 0.079(4) 0.052(3) -0.012(2) -0.030(2) 0.027(3) C47 0.051(2) 0.050(2) 0.052(2) -0.0164(19) -0.0242(19) 0.012(2) O51 0.0366(14) 0.0506(17) 0.0267(13) 0.0010(12) -0.0080(11) 0.0039(13) O52 0.0453(15) 0.0596(17) 0.0412(14) -0.0184(13) -0.0191(12) 0.0228(14) C51 0.0382(19) 0.0283(18) 0.0253(17) -0.0022(14) -0.0076(15) 0.0040(16) C52 0.051(2) 0.081(3) 0.034(2) -0.009(2) -0.0156(19) 0.032(2) N5 0.0408(18) 0.053(2) 0.0364(17) -0.0111(15) -0.0092(15) 0.0160(16) C53 0.061(3) 0.049(3) 0.046(2) -0.011(2) -0.011(2) 0.006(2) C54 0.054(3) 0.074(3) 0.071(3) -0.018(3) -0.019(2) -0.011(3) C55 0.041(2) 0.083(4) 0.065(3) -0.011(3) -0.022(2) 0.011(3) C56 0.050(3) 0.049(3) 0.070(3) -0.012(2) -0.019(2) 0.018(2) C57 0.046(2) 0.057(3) 0.062(3) -0.020(2) -0.018(2) 0.002(2) Cl1 0.0579(6) 0.0541(7) 0.0634(7) -0.0082(5) -0.0265(5) -0.0081(6) O13 0.075(3) 0.085(3) 0.125(4) -0.029(3) 0.003(3) 0.000(2) O14 0.127(3) 0.135(4) 0.067(2) -0.001(3) -0.040(2) -0.048(3) O15 0.108(2) 0.109(3) 0.130(3) -0.007(3) -0.082(2) -0.034(3) O16 0.084(3) 0.063(3) 0.154(4) -0.024(3) -0.005(3) -0.006(2) Cl2 0.0497(6) 0.0749(8) 0.0616(6) -0.0281(6) -0.0234(5) 0.0129(6) O23 0.102(3) 0.203(6) 0.066(3) -0.018(3) -0.037(2) 0.041(4) O24 0.102(4) 0.127(4) 0.216(6) -0.054(4) -0.021(4) -0.038(4) O25 0.097(3) 0.137(3) 0.132(3) -0.092(3) -0.049(2) 0.056(3) O26 0.075(2) 0.121(3) 0.090(3) -0.045(2) -0.037(2) 0.046(2) Cl3 0.0583(6) 0.0607(7) 0.0606(6) -0.0145(6) -0.0223(5) -0.0072(6) O33 0.097(4) 0.084(4) 0.137(5) -0.008(4) -0.064(4) 0.017(3) O34 0.141(7) 0.112(6) 0.177(7) -0.080(5) -0.011(6) 0.011(5) O35 0.238(6) 0.131(7) 0.260(6) -0.039(5) -0.211(5) 0.004(5) O36 0.125(7) 0.251(12) 0.141(9) 0.042(10) 0.064(8) -0.012(8) O33B 0.097(4) 0.084(4) 0.137(5) -0.008(4) -0.064(4) 0.017(3) O34B 0.141(7) 0.112(6) 0.177(7) -0.080(5) -0.011(6) 0.011(5) O35B 0.238(6) 0.131(7) 0.260(6) -0.039(5) -0.211(5) 0.004(5) O36B 0.125(7) 0.251(12) 0.141(9) 0.042(10) 0.064(8) -0.012(8) Cl4 0.0725(7) 0.0743(8) 0.0587(6) -0.0320(6) -0.0267(6) 0.0214(6) O43 0.163(6) 0.259(7) 0.082(4) -0.100(4) -0.031(4) 0.093(6) O44 0.084(4) 0.112(4) 0.129(7) -0.049(5) -0.021(4) 0.015(3) O45 0.138(6) 0.068(4) 0.110(5) -0.009(4) -0.024(5) -0.025(4) O46 0.180(6) 0.135(7) 0.099(4) -0.040(4) -0.081(4) 0.077(5) O43B 0.163(6) 0.259(7) 0.082(4) -0.100(4) -0.031(4) 0.093(6) O44B 0.084(4) 0.112(4) 0.129(7) -0.049(5) -0.021(4) 0.015(3) O45B 0.138(6) 0.068(4) 0.110(5) -0.009(4) -0.024(5) -0.025(4) O46B 0.180(6) 0.135(7) 0.099(4) -0.040(4) -0.081(4) 0.077(5) Cl5 0.0692(8) 0.0672(8) 0.0770(8) -0.0212(7) -0.0167(7) -0.0019(7) O53 0.170(7) 0.194(8) 0.111(4) -0.011(5) -0.087(5) -0.057(6) O54 0.180(8) 0.136(6) 0.132(4) -0.017(4) -0.115(5) 0.024(6) O55 0.120(6) 0.112(7) 0.182(8) -0.029(7) 0.036(6) -0.039(6) O56 0.143(8) 0.087(6) 0.176(8) -0.027(6) 0.014(7) 0.019(5) O53B 0.170(7) 0.194(8) 0.111(4) -0.011(5) -0.087(5) -0.057(6) O54B 0.180(8) 0.136(6) 0.132(4) -0.017(4) -0.115(5) 0.024(6) O55B 0.120(6) 0.112(7) 0.182(8) -0.029(7) 0.036(6) -0.039(6) O56B 0.143(8) 0.087(6) 0.176(8) -0.027(6) 0.014(7) 0.019(5) O4W 0.0542(18) 0.0522(18) 0.0644(19) -0.0237(15) -0.0125(15) 0.0002(15) O5W 0.104(3) 0.124(3) 0.121(3) -0.079(2) -0.047(2) 0.027(3) O6W 0.143(4) 0.108(5) 0.266(7) -0.022(5) -0.106(5) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O22 2.394(3) . yes Nd1 O32 2.402(3) . yes Nd1 O42 2.412(3) . yes Nd1 O12 2.441(3) . yes Nd1 O1W 2.449(3) . yes Nd1 O2W 2.469(3) . yes Nd1 O3W 2.499(3) . yes Nd1 O61 2.539(3) . yes Nd1 O62 2.638(3) . yes Cu1 O41 1.946(3) . yes Cu1 O11 1.956(3) . yes Cu1 O31 1.971(3) . yes Cu1 O21 1.980(3) . yes Cu1 O51 2.154(3) . yes Cu2 O4W 1.912(3) . yes Cu2 O4W 1.912(3) 2_565 yes Cu2 O52 1.918(3) 2_565 yes Cu2 O52 1.918(3) . yes O61 N6 1.249(4) . ? O62 N6 1.255(5) . ? O63 N6 1.222(5) . ? O11 C11 1.252(5) . ? O12 C11 1.238(4) . ? C11 C12 1.505(6) . ? C12 N1 1.467(5) . ? N1 C17 1.333(6) . ? N1 C13 1.334(5) . ? C13 C14 1.364(7) . ? C14 C15 1.359(8) . ? C15 C16 1.360(8) . ? C16 C17 1.346(7) . ? O21 C21 1.250(4) . ? O22 C21 1.229(4) . ? C21 C22 1.498(6) . ? C22 N2 1.472(5) . ? N2 C27 1.329(6) . ? N2 C23 1.329(5) . ? C23 C24 1.387(7) . ? C24 C25 1.347(9) . ? C25 C26 1.332(8) . ? C26 C27 1.363(7) . ? O31 C31 1.238(5) . ? O32 C31 1.238(5) . ? C31 C32 1.504(7) . ? C32 N3 1.450(6) . ? N3 C37 1.316(6) . ? N3 C33 1.321(7) . ? C33 C34 1.354(8) . ? C34 C35 1.341(10) . ? C35 C36 1.326(10) . ? C36 C37 1.379(9) . ? O41 C41 1.247(5) . ? O42 C41 1.226(5) . ? C41 C42 1.516(6) . ? C42 N4 1.468(5) . ? N4 C43 1.337(6) . ? N4 C47 1.343(6) . ? C43 C44 1.363(8) . ? C44 C45 1.356(9) . ? C45 C46 1.361(8) . ? C46 C47 1.353(7) . ? O51 C51 1.208(5) . ? O52 C51 1.261(5) . ? C51 C52 1.521(6) . ? C52 N5 1.466(6) . ? N5 C53 1.319(7) . ? N5 C57 1.348(6) . ? C53 C54 1.368(8) . ? C54 C55 1.346(8) . ? C55 C56 1.369(8) . ? C56 C57 1.347(7) . ? Cl1 O15 1.387(4) . ? Cl1 O16 1.405(4) . ? Cl1 O14 1.407(4) . ? Cl1 O13 1.428(4) . ? Cl2 O24 1.381(5) . ? Cl2 O23 1.395(4) . ? Cl2 O25 1.396(4) . ? Cl2 O26 1.409(4) . ? Cl3 O34B 1.370(7) . ? Cl3 O36 1.375(6) . ? Cl3 O35 1.386(6) . ? Cl3 O36B 1.402(7) . ? Cl3 O33B 1.416(7) . ? Cl3 O33 1.419(5) . ? Cl3 O35B 1.435(7) . ? Cl3 O34 1.443(6) . ? Cl4 O43 1.377(6) . ? Cl4 O45 1.396(6) . ? Cl4 O44B 1.399(6) . ? Cl4 O46B 1.399(7) . ? Cl4 O43B 1.410(7) . ? Cl4 O44 1.436(5) . ? Cl4 O45B 1.442(6) . ? Cl4 O46 1.443(6) . ? Cl5 O54B 1.373(6) . ? Cl5 O53 1.395(7) . ? Cl5 O56 1.407(6) . ? Cl5 O55 1.407(6) . ? Cl5 O55B 1.406(6) . ? Cl5 O56B 1.411(6) . ? Cl5 O53B 1.427(7) . ? Cl5 O54 1.428(6) . ? 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 O22 Nd1 O32 73.74(11) . . yes O22 Nd1 O42 110.41(10) . . yes O32 Nd1 O42 70.57(11) . . yes O22 Nd1 O12 70.30(11) . . yes O32 Nd1 O12 113.67(9) . . yes O42 Nd1 O12 72.61(11) . . yes O22 Nd1 O1W 134.08(11) . . yes O32 Nd1 O1W 142.92(11) . . yes O42 Nd1 O1W 75.64(11) . . yes O12 Nd1 O1W 68.63(10) . . yes O22 Nd1 O2W 149.24(12) . . yes O32 Nd1 O2W 81.69(11) . . yes O42 Nd1 O2W 77.40(10) . . yes O12 Nd1 O2W 138.30(10) . . yes O1W Nd1 O2W 76.40(11) . . yes O22 Nd1 O3W 76.32(11) . . yes O32 Nd1 O3W 69.94(11) . . yes O42 Nd1 O3W 135.81(12) . . yes O12 Nd1 O3W 143.09(11) . . yes O1W Nd1 O3W 132.00(10) . . yes O2W Nd1 O3W 78.06(11) . . yes O22 Nd1 O61 71.25(10) . . yes O32 Nd1 O61 137.74(11) . . yes O42 Nd1 O61 144.82(11) . . yes O12 Nd1 O61 75.45(10) . . yes O1W Nd1 O61 79.34(11) . . yes O2W Nd1 O61 120.04(10) . . yes O3W Nd1 O61 79.35(11) . . yes O22 Nd1 O62 112.35(9) . . yes O32 Nd1 O62 131.82(10) . . yes O42 Nd1 O62 136.01(10) . . yes O12 Nd1 O62 113.05(10) . . yes O1W Nd1 O62 67.60(10) . . yes O2W Nd1 O62 71.32(10) . . yes O3W Nd1 O62 65.95(10) . . yes O61 Nd1 O62 48.75(9) . . yes O41 Cu1 O11 90.93(14) . . yes O41 Cu1 O31 89.03(14) . . yes O11 Cu1 O31 172.65(11) . . yes O41 Cu1 O21 174.68(11) . . yes O11 Cu1 O21 88.68(13) . . yes O31 Cu1 O21 90.68(13) . . yes O41 Cu1 O51 92.51(12) . . yes O11 Cu1 O51 90.78(12) . . yes O31 Cu1 O51 96.57(12) . . yes O21 Cu1 O51 92.80(11) . . yes O4W Cu2 O4W 180.0 . 2_565 yes O4W Cu2 O52 90.69(14) . 2_565 yes O4W Cu2 O52 89.31(14) 2_565 2_565 yes O4W Cu2 O52 89.31(14) . . yes O4W Cu2 O52 90.69(14) 2_565 . yes O52 Cu2 O52 180.0 2_565 . yes N6 O61 Nd1 99.0(2) . . ? N6 O62 Nd1 94.1(2) . . ? O63 N6 O61 121.5(4) . . ? O63 N6 O62 121.2(3) . . ? O61 N6 O62 117.3(3) . . ? C11 O11 Cu1 124.8(3) . . ? C11 O12 Nd1 140.2(3) . . ? O12 C11 O11 127.2(4) . . ? O12 C11 C12 120.4(4) . . ? O11 C11 C12 112.4(3) . . ? N1 C12 C11 114.6(3) . . ? C17 N1 C13 120.4(4) . . ? C17 N1 C12 118.4(4) . . ? C13 N1 C12 121.1(4) . . ? N1 C13 C14 120.9(5) . . ? C15 C14 C13 118.4(5) . . ? C14 C15 C16 120.0(5) . . ? C17 C16 C15 119.8(6) . . ? N1 C17 C16 120.3(5) . . ? C21 O21 Cu1 113.1(2) . . ? C21 O22 Nd1 157.0(3) . . ? O22 C21 O21 125.3(4) . . ? O22 C21 C22 117.9(3) . . ? O21 C21 C22 116.8(3) . . ? N2 C22 C21 111.2(3) . . ? C27 N2 C23 120.2(4) . . ? C27 N2 C22 118.9(4) . . ? C23 N2 C22 120.8(4) . . ? N2 C23 C24 119.0(5) . . ? C25 C24 C23 120.5(5) . . ? C26 C25 C24 119.2(5) . . ? C25 C26 C27 120.1(6) . . ? N2 C27 C26 121.0(5) . . ? C31 O31 Cu1 117.6(3) . . ? C31 O32 Nd1 150.8(3) . . ? O32 C31 O31 126.8(4) . . ? O32 C31 C32 116.9(4) . . ? O31 C31 C32 116.3(4) . . ? N3 C32 C31 110.8(4) . . ? C37 N3 C33 120.5(4) . . ? C37 N3 C32 121.0(4) . . ? C33 N3 C32 118.4(4) . . ? N3 C33 C34 121.9(5) . . ? C35 C34 C33 117.5(7) . . ? C36 C35 C34 121.3(6) . . ? C35 C36 C37 119.7(6) . . ? N3 C37 C36 119.0(5) . . ? C41 O41 Cu1 124.3(3) . . ? C41 O42 Nd1 142.8(3) . . ? O42 C41 O41 128.1(4) . . ? O42 C41 C42 119.1(4) . . ? O41 C41 C42 112.8(3) . . ? N4 C42 C41 112.3(3) . . ? C43 N4 C47 120.5(4) . . ? C43 N4 C42 120.6(4) . . ? C47 N4 C42 118.9(4) . . ? N4 C43 C44 119.6(6) . . ? C45 C44 C43 119.7(6) . . ? C44 C45 C46 120.6(5) . . ? C47 C46 C45 118.2(6) . . ? N4 C47 C46 121.4(5) . . ? C51 O51 Cu1 133.9(3) . . ? C51 O52 Cu2 123.8(3) . . ? O51 C51 O52 127.9(4) . . ? O51 C51 C52 119.8(4) . . ? O52 C51 C52 112.3(3) . . ? N5 C52 C51 111.9(4) . . ? C53 N5 C57 121.1(4) . . ? C53 N5 C52 119.8(4) . . ? C57 N5 C52 119.1(4) . . ? N5 C53 C54 119.6(5) . . ? C55 C54 C53 120.1(6) . . ? C54 C55 C56 119.8(5) . . ? C57 C56 C55 118.9(5) . . ? C56 C57 N5 120.5(5) . . ? O15 Cl1 O16 112.4(3) . . ? O15 Cl1 O14 109.9(3) . . ? O16 Cl1 O14 110.4(3) . . ? O15 Cl1 O13 109.3(3) . . ? O16 Cl1 O13 107.7(3) . . ? O14 Cl1 O13 107.0(3) . . ? O24 Cl2 O23 109.5(4) . . ? O24 Cl2 O25 110.0(3) . . ? O23 Cl2 O25 109.0(3) . . ? O24 Cl2 O26 110.9(3) . . ? O23 Cl2 O26 108.2(3) . . ? O25 Cl2 O26 109.1(3) . . ? O34B Cl3 O36 161.3(8) . . ? O34B Cl3 O35 68.7(6) . . ? O36 Cl3 O35 118.8(6) . . ? O34B Cl3 O36B 119.9(7) . . ? O36 Cl3 O36B 51.2(6) . . ? O35 Cl3 O36B 169.6(6) . . ? O34B Cl3 O33B 116.2(6) . . ? O36 Cl3 O33B 82.3(7) . . ? O35 Cl3 O33B 70.4(6) . . ? O36B Cl3 O33B 108.1(7) . . ? O34B Cl3 O33 81.7(6) . . ? O36 Cl3 O33 109.3(5) . . ? O35 Cl3 O33 109.8(5) . . ? O36B Cl3 O33 78.5(6) . . ? O33B Cl3 O33 68.9(5) . . ? O34B Cl3 O35B 106.7(6) . . ? O36 Cl3 O35B 65.0(6) . . ? O35 Cl3 O35B 67.0(6) . . ? O36B Cl3 O35B 103.6(6) . . ? O33B Cl3 O35B 99.4(6) . . ? O33 Cl3 O35B 168.0(6) . . ? O34B Cl3 O34 55.1(6) . . ? O36 Cl3 O34 106.3(6) . . ? O35 Cl3 O34 104.7(6) . . ? O36B Cl3 O34 78.0(7) . . ? O33B Cl3 O34 171.4(5) . . ? O33 Cl3 O34 107.3(5) . . ? O35B Cl3 O34 84.7(6) . . ? O43 Cl4 O45 122.3(5) . . ? O43 Cl4 O44B 137.6(7) . . ? O45 Cl4 O44B 88.7(6) . . ? O43 Cl4 O46B 106.5(6) . . ? O45 Cl4 O46B 60.4(6) . . ? O44B Cl4 O46B 114.4(6) . . ? O43 Cl4 O43B 39.1(5) . . ? O45 Cl4 O43B 159.6(6) . . ? O44B Cl4 O43B 111.4(7) . . ? O46B Cl4 O43B 111.3(7) . . ? O43 Cl4 O44 111.3(6) . . ? O45 Cl4 O44 104.8(5) . . ? O44B Cl4 O44 26.7(7) . . ? O46B Cl4 O44 141.0(5) . . ? O43B Cl4 O44 92.7(7) . . ? O43 Cl4 O45B 69.0(5) . . ? O45 Cl4 O45B 63.6(5) . . ? O44B Cl4 O45B 108.2(7) . . ? O46B Cl4 O45B 106.1(6) . . ? O43B Cl4 O45B 104.8(5) . . ? O44 Cl4 O45B 96.2(6) . . ? O43 Cl4 O46 107.5(5) . . ? O45 Cl4 O46 105.6(5) . . ? O44B Cl4 O46 88.2(6) . . ? O46B Cl4 O46 54.4(5) . . ? O43B Cl4 O46 79.7(5) . . ? O44 Cl4 O46 103.8(5) . . ? O45B Cl4 O46 159.3(6) . . ? O54B Cl5 O53 138.1(7) . . ? O54B Cl5 O56 103.7(7) . . ? O53 Cl5 O56 112.6(7) . . ? O54B Cl5 O55 73.2(6) . . ? O53 Cl5 O55 110.5(6) . . ? O56 Cl5 O55 110.8(6) . . ? O54B Cl5 O55B 114.2(6) . . ? O53 Cl5 O55B 99.9(7) . . ? O56 Cl5 O55B 65.0(6) . . ? O55 Cl5 O55B 56.3(6) . . ? O54B Cl5 O56B 115.2(6) . . ? O53 Cl5 O56B 74.3(6) . . ? O56 Cl5 O56B 53.3(6) . . ? O55 Cl5 O56B 162.5(6) . . ? O55B Cl5 O56B 106.7(5) . . ? O54B Cl5 O53B 107.5(6) . . ? O53 Cl5 O53B 35.9(6) . . ? O56 Cl5 O53B 148.0(7) . . ? O55 Cl5 O53B 85.1(7) . . ? O55B Cl5 O53B 107.0(6) . . ? O56B Cl5 O53B 105.6(6) . . ? O54B Cl5 O54 39.3(5) . . ? O53 Cl5 O54 107.6(6) . . ? O56 Cl5 O54 107.1(6) . . ? O55 Cl5 O54 108.0(6) . . ? O55B Cl5 O54 152.1(7) . . ? O56B Cl5 O54 85.6(6) . . ? O53B Cl5 O54 93.0(5) . . ? 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 O5W H5WA O53 0.88 2.21 2.735(9) 118.0 . O5W H5WB O6W 0.91 1.82 2.715(8) 169.1 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.170 _refine_diff_density_min -1.270 _refine_diff_density_rms 0.110 #_eof #End of Crystallographic Information File