# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_address ;Laboratorio de Rayos X y Materiales Moleculares Dpto. F\'isica Fundamental II. Facultad de F\'isica Universidad de La Laguna E-38204. La Laguna. Tenerife Spain ; _publ_contact_author_address ;Laboratorio de Rayos X y Materiales Moleculares Dpto. F\'isica Fundamental II. Facultad de F\'isica Universidad de La Laguna E-38204. La Laguna. Tenerife Spain ; _publ_contact_author_email caruiz@ull.es _publ_contact_author_fax +34922318320 _publ_contact_author_phone +34922318300 _publ_contact_author_name 'Professor Catalina Ruiz-Perez' loop_ _publ_author_name 'Oscar Fabelo' 'Laura Canadillas-Delgado' 'Jorge Pasan' 'Ana Labrador' 'Pau Diaz-Gallifa' 'Catalina Ruiz-Perez' # Attachment '- 1a.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 806345' #TrackingRef '- 1a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H45 Cu2 O40 Pr2' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour light_blue _diffrn_ambient_temperature 293(2) _chemical_formula_weight 1394.51 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.953(2) _cell_length_b 23.056(5) _cell_length_c 19.811(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.88(3) _cell_angle_gamma 90.00 _cell_volume 4929.0(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2764 _exptl_absorpt_coefficient_mu 3.194 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.7600 _exptl_absorpt_correction_T_max 0.8684 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7383 _diffrn_source synchrotron _diffrn_source_type 'ESRF-CRG BM16' _diffrn_radiation_monochromator 'Si 111' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9.6 _diffrn_radiation_detector 'ADSC Q210r CCD (binned mode)' _diffrn_measurement_device_type 'Single-axis HUBER diffractometer' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90569 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.92 _reflns_number_total 11573 _reflns_number_gt 9974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MxCube (ESRF, 2006)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+23.0827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00051(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11573 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1633 _refine_ls_wR_factor_gt 0.1544 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Cu1 Cu 0.08994(5) 0.17742(3) 0.89995(3) 0.02228(14) Uani 1 1 d . . . Cu2 Cu 0.30261(5) 0.17830(3) 0.65253(3) 0.02011(14) Uani 1 1 d . . . Pr1 Pr -0.46065(2) 0.146151(10) 0.400194(12) 0.01775(10) Uani 1 1 d . . . Pr2 Pr 0.85108(3) 0.145124(12) 1.147697(14) 0.02345(10) Uani 1 1 d . . . O1 O -0.3538(3) 0.21738(18) 0.47913(18) 0.0296(8) Uani 1 1 d . . . O2 O -0.3275(4) 0.31243(17) 0.49504(17) 0.0290(8) Uani 1 1 d . . . O3 O -0.4945(3) 0.29128(17) 0.59869(17) 0.0254(7) Uani 1 1 d . . . O4 O -0.4091(4) 0.35591(18) 0.6739(2) 0.0349(9) Uani 1 1 d . . . O5 O -0.0271(4) 0.27101(17) 0.82813(18) 0.0306(8) Uani 1 1 d . . . O6 O 0.0057(3) 0.17878(17) 0.80408(17) 0.0272(7) Uani 1 1 d . . . O7 O 0.1439(3) 0.20242(16) 0.68006(17) 0.0245(7) Uani 1 1 d . . . O8 O 0.0378(4) 0.12111(19) 0.6518(3) 0.0418(10) Uani 1 1 d . . . O9 O -0.3300(4) -0.03949(19) 0.4623(2) 0.0391(9) Uani 1 1 d . . . O10 O -0.2980(4) 0.01187(19) 0.5589(2) 0.0360(9) Uani 1 1 d . . . O11 O -0.2741(3) 0.09020(18) 0.4410(2) 0.0342(9) Uani 1 1 d . . . O12 O -0.1052(5) 0.1394(3) 0.4296(6) 0.116(4) Uani 1 1 d . . . O13 O 0.2473(3) 0.19603(17) 0.86812(18) 0.0264(7) Uani 1 1 d . . . O14 O 0.3614(4) 0.1207(2) 0.9084(3) 0.0464(11) Uani 1 1 d . . . O15 O 0.3856(3) 0.17996(17) 0.74821(17) 0.0265(7) Uani 1 1 d . . . O16 O 0.4094(4) 0.27233(19) 0.72333(19) 0.0344(9) Uani 1 1 d . . . O17 O 0.7951(4) 0.36132(18) 0.8786(2) 0.0345(9) Uani 1 1 d . . . O18 O 0.8813(3) 0.29553(17) 0.95243(17) 0.0262(7) Uani 1 1 d . . . O19 O 0.7398(4) 0.21654(18) 1.07177(19) 0.0319(8) Uani 1 1 d . . . O20 O 0.7246(3) 0.31244(17) 1.05720(17) 0.0271(7) Uani 1 1 d . . . O1W O -0.4765(4) 0.10304(17) 0.51878(19) 0.0289(8) Uani 1 1 d . . . O2W O -0.5152(4) 0.03975(18) 0.3888(2) 0.0359(9) Uani 1 1 d . . . O3W O -0.4802(5) 0.1095(2) 0.2781(2) 0.0502(12) Uani 1 1 d . . . O4W O -0.2802(4) 0.18752(19) 0.3468(2) 0.0366(9) Uani 1 1 d . . . O5W O 0.6605(5) 0.1778(2) 1.1968(3) 0.0554(14) Uani 1 1 d . . . O6W O 0.8716(9) 0.1085(3) 1.2685(3) 0.091(3) Uani 1 1 d . . . O7W O 0.9189(8) 0.0400(3) 1.1620(3) 0.080(2) Uani 1 1 d . . . O8W O 0.6693(6) 0.0825(3) 1.1021(4) 0.086(2) Uani 1 1 d . . . O9W O 0.8915(6) 0.1048(2) 1.0370(3) 0.0624(16) Uani 1 1 d . . . O10W O -0.0725(4) 0.18032(18) 0.93364(19) 0.0319(8) Uani 1 1 d . . . O11W O 0.1057(9) 0.0814(3) 0.9093(4) 0.094(3) Uani 1 1 d . . . O12W O 0.2686(4) 0.0829(2) 0.6516(2) 0.0391(9) Uani 1 1 d . . . O13W O 0.4706(3) 0.17821(17) 0.62167(19) 0.0291(8) Uani 1 1 d . . . O1X O -0.1685(6) 0.0622(3) 0.6680(3) 0.0688(16) Uani 1 1 d . . . O2X O -0.2584(7) 0.1263(4) 0.8574(4) 0.090(2) Uani 1 1 d . . . O3X O 0.6456(8) 0.1176(5) 0.7221(4) 0.116(3) Uani 1 1 d . . . O4X O 0.6059(10) 0.4356(4) 0.8073(5) 0.128(4) Uani 1 1 d . . . O5X O -0.7027(11) 0.0751(6) 0.1937(9) 0.176(6) Uani 1 1 d . . . O6X O 0.5849(13) 0.0632(7) 0.9297(14) 0.314(14) Uani 1 1 d . . . O7X O 0.4119(14) 0.1162(8) 1.0810(8) 0.203(7) Uani 1 1 d . . . C1 C -0.2482(4) 0.2508(2) 0.5865(2) 0.0206(9) Uani 1 1 d . . . C2 C -0.2808(4) 0.2802(2) 0.6431(2) 0.0205(9) Uani 1 1 d . . . C3 C -0.2077(4) 0.2739(2) 0.7069(2) 0.0235(9) Uani 1 1 d . . . H3 H -0.2280 0.2942 0.7440 0.028 Uiso 1 1 calc R . . C4 C -0.1044(4) 0.2377(2) 0.7167(2) 0.0204(9) Uani 1 1 d . . . C5 C -0.0726(4) 0.2082(2) 0.6603(2) 0.0207(9) Uani 1 1 d . . . C6 C -0.1442(4) 0.2150(2) 0.5957(2) 0.0222(9) Uani 1 1 d . . . H6 H -0.1225 0.1956 0.5583 0.027 Uiso 1 1 calc R . . C7 C -0.3169(4) 0.2602(2) 0.5149(2) 0.0208(9) Uani 1 1 d . . . C8 C -0.4011(4) 0.3122(2) 0.6376(2) 0.0234(9) Uani 1 1 d . . . C9 C -0.0358(4) 0.2289(2) 0.7878(2) 0.0214(9) Uani 1 1 d . . . C10 C 0.0449(4) 0.1734(2) 0.6658(2) 0.0222(9) Uani 1 1 d . . . C11 C -0.1268(4) -0.0037(2) 0.5015(3) 0.0248(9) Uani 1 1 d . . . C12 C -0.0780(5) 0.0465(2) 0.4764(3) 0.0318(11) Uani 1 1 d . . . C13 C 0.0492(5) 0.0495(2) 0.4754(3) 0.0329(12) Uani 1 1 d . . . H13 H 0.0821 0.0828 0.4590 0.040 Uiso 1 1 calc R . . C14 C -0.2611(4) -0.0098(2) 0.5082(3) 0.0274(10) Uani 1 1 d . . . C15 C -0.1584(5) 0.0958(3) 0.4471(4) 0.0472(17) Uani 1 1 d . . . C20 C 0.4632(4) 0.2089(2) 0.8915(2) 0.0210(9) Uani 1 1 d . . . C21 C 0.4914(4) 0.2403(2) 0.8359(2) 0.0209(9) Uani 1 1 d . . . C22 C 0.5917(4) 0.2780(2) 0.8453(2) 0.0226(9) Uani 1 1 d . . . H22 H 0.6089 0.2995 0.8084 0.027 Uiso 1 1 calc R . . C23 C 0.6668(4) 0.2841(2) 0.9089(2) 0.0208(9) Uani 1 1 d . . . C24 C 0.6389(4) 0.2529(2) 0.9653(2) 0.0199(9) Uani 1 1 d . . . C25 C 0.5365(4) 0.2157(2) 0.9556(2) 0.0226(9) Uani 1 1 d . . . H25 H 0.5172 0.1952 0.9928 0.027 Uiso 1 1 calc R . . C26 C 0.3495(5) 0.1712(2) 0.8882(2) 0.0240(9) Uani 1 1 d . . . C27 C 0.4221(4) 0.2308(2) 0.7642(2) 0.0216(9) Uani 1 1 d . . . C28 C 0.7873(4) 0.3170(2) 0.9142(2) 0.0227(9) Uani 1 1 d . . . C29 C 0.7083(4) 0.2609(2) 1.0364(2) 0.0216(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0182(3) 0.0335(3) 0.0140(3) 0.0000(2) -0.0004(2) -0.0026(2) Cu2 0.0154(3) 0.0321(3) 0.0117(2) -0.0015(2) -0.00079(19) 0.0016(2) Pr1 0.01381(15) 0.02485(15) 0.01469(14) 0.00107(8) 0.00276(9) 0.00154(8) Pr2 0.02014(16) 0.02965(17) 0.02054(16) 0.00090(9) 0.00341(11) -0.00358(9) O1 0.0255(18) 0.041(2) 0.0194(16) -0.0049(15) -0.0060(13) -0.0025(15) O2 0.0314(19) 0.038(2) 0.0160(16) 0.0005(14) -0.0006(14) 0.0025(15) O3 0.0164(16) 0.0368(19) 0.0223(16) -0.0038(14) 0.0014(13) 0.0018(13) O4 0.0233(19) 0.043(2) 0.038(2) -0.0139(17) 0.0020(17) 0.0048(15) O5 0.035(2) 0.038(2) 0.0163(16) -0.0068(14) -0.0040(14) -0.0044(16) O6 0.0243(18) 0.039(2) 0.0166(15) -0.0010(14) -0.0022(13) 0.0039(14) O7 0.0147(15) 0.0372(19) 0.0208(16) -0.0049(14) 0.0011(12) 0.0004(13) O8 0.026(2) 0.036(2) 0.063(3) -0.012(2) 0.0072(19) 0.0002(17) O9 0.0195(18) 0.047(2) 0.052(3) -0.0095(19) 0.0099(17) -0.0082(16) O10 0.0227(18) 0.050(2) 0.038(2) -0.0020(18) 0.0120(16) -0.0005(16) O11 0.0140(16) 0.036(2) 0.053(2) 0.0141(18) 0.0056(16) 0.0042(14) O12 0.023(3) 0.064(4) 0.260(11) 0.093(5) 0.020(4) 0.007(2) O13 0.0154(16) 0.040(2) 0.0229(17) 0.0020(14) 0.0021(13) -0.0045(14) O14 0.030(2) 0.038(2) 0.069(3) 0.014(2) 0.001(2) -0.0042(18) O15 0.0208(17) 0.042(2) 0.0149(15) -0.0042(14) -0.0028(12) -0.0019(14) O16 0.037(2) 0.046(2) 0.0168(17) 0.0057(15) -0.0042(15) -0.0024(17) O17 0.0226(19) 0.037(2) 0.043(2) 0.0115(17) 0.0032(17) -0.0045(15) O18 0.0149(15) 0.043(2) 0.0197(16) 0.0010(14) 0.0000(12) -0.0046(14) O19 0.0284(19) 0.044(2) 0.0201(17) 0.0051(15) -0.0055(14) 0.0004(16) O20 0.0260(18) 0.042(2) 0.0124(15) -0.0013(14) -0.0006(13) -0.0062(15) O1W 0.0280(18) 0.0336(19) 0.0266(18) 0.0029(15) 0.0091(14) 0.0005(15) O2W 0.034(2) 0.0317(19) 0.044(2) -0.0017(17) 0.0128(18) -0.0054(16) O3W 0.072(3) 0.052(3) 0.029(2) -0.0087(19) 0.015(2) -0.017(2) O4W 0.033(2) 0.042(2) 0.038(2) -0.0003(17) 0.0151(17) -0.0036(17) O5W 0.055(3) 0.046(3) 0.077(4) 0.011(2) 0.046(3) 0.004(2) O6W 0.173(8) 0.060(4) 0.041(3) 0.015(3) 0.020(4) -0.003(4) O7W 0.126(6) 0.044(3) 0.068(4) 0.005(3) 0.008(4) 0.012(3) O8W 0.056(4) 0.092(5) 0.111(6) -0.035(4) 0.013(4) -0.034(3) O9W 0.104(5) 0.050(3) 0.040(3) -0.009(2) 0.032(3) -0.015(3) O10W 0.0272(19) 0.046(2) 0.0230(17) 0.0035(16) 0.0059(14) -0.0030(16) O11W 0.151(8) 0.041(3) 0.085(5) 0.001(3) 0.008(5) -0.013(4) O12W 0.034(2) 0.042(2) 0.040(2) -0.0032(18) 0.0040(18) 0.0031(17) O13W 0.0209(17) 0.041(2) 0.0256(17) -0.0054(15) 0.0048(14) 0.0022(15) O1X 0.057(3) 0.086(4) 0.064(4) -0.003(3) 0.010(3) -0.024(3) O2X 0.059(4) 0.135(7) 0.072(4) -0.028(4) 0.003(3) -0.028(4) O3X 0.084(6) 0.183(9) 0.072(5) -0.008(6) -0.011(4) 0.067(6) O4X 0.163(10) 0.088(6) 0.104(6) -0.036(5) -0.057(6) 0.030(6) O5X 0.111(9) 0.124(9) 0.301(17) 0.081(11) 0.057(10) 0.043(7) O6X 0.118(10) 0.170(14) 0.70(4) 0.15(2) 0.187(18) 0.063(10) O7X 0.151(12) 0.247(17) 0.227(16) 0.102(14) 0.081(11) 0.060(12) C1 0.015(2) 0.033(2) 0.0124(19) -0.0001(17) -0.0004(15) -0.0018(17) C2 0.0136(19) 0.031(2) 0.016(2) -0.0022(17) 0.0017(16) 0.0027(17) C3 0.015(2) 0.039(3) 0.016(2) -0.0023(18) 0.0025(16) 0.0007(18) C4 0.0150(19) 0.035(2) 0.0105(18) -0.0008(16) -0.0013(15) -0.0018(17) C5 0.014(2) 0.032(2) 0.016(2) -0.0013(17) 0.0015(16) -0.0008(17) C6 0.017(2) 0.035(2) 0.0136(19) -0.0032(17) 0.0006(16) 0.0021(18) C7 0.0132(19) 0.036(2) 0.0130(19) -0.0014(17) 0.0023(15) 0.0007(17) C8 0.017(2) 0.033(2) 0.020(2) 0.0016(18) 0.0032(17) 0.0036(18) C9 0.0143(19) 0.039(3) 0.0100(18) -0.0011(17) -0.0006(15) -0.0022(18) C10 0.017(2) 0.033(2) 0.0155(19) -0.0011(17) 0.0011(16) 0.0027(18) C11 0.016(2) 0.031(2) 0.028(2) 0.0020(19) 0.0052(17) 0.0012(17) C12 0.016(2) 0.030(3) 0.050(3) 0.007(2) 0.006(2) 0.0013(18) C13 0.014(2) 0.035(3) 0.051(3) 0.009(2) 0.008(2) -0.0005(19) C14 0.017(2) 0.031(2) 0.035(3) 0.008(2) 0.0053(19) 0.0025(18) C15 0.019(3) 0.038(3) 0.087(5) 0.025(3) 0.013(3) 0.005(2) C20 0.015(2) 0.030(2) 0.017(2) -0.0008(17) -0.0002(16) -0.0015(17) C21 0.015(2) 0.033(2) 0.0131(19) -0.0008(17) -0.0019(15) -0.0007(17) C22 0.016(2) 0.037(3) 0.0140(19) 0.0011(17) 0.0006(16) -0.0045(18) C23 0.015(2) 0.031(2) 0.017(2) 0.0016(17) 0.0030(16) -0.0034(17) C24 0.015(2) 0.031(2) 0.0124(19) 0.0006(17) -0.0015(15) -0.0031(17) C25 0.018(2) 0.035(2) 0.014(2) 0.0023(17) 0.0012(16) -0.0063(18) C26 0.019(2) 0.034(2) 0.019(2) -0.0001(18) 0.0007(17) -0.0059(18) C27 0.0147(19) 0.038(3) 0.0117(19) -0.0008(17) 0.0018(15) 0.0010(18) C28 0.015(2) 0.032(2) 0.021(2) -0.0013(18) 0.0047(17) -0.0047(17) C29 0.0118(19) 0.040(3) 0.0118(19) 0.0019(17) -0.0002(15) -0.0025(18) _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 Cu1 O2 1.959(4) 4_666 ? Cu1 O6 1.964(3) . ? Cu1 O13 1.981(3) . ? Cu1 O10W 2.005(4) . ? Cu1 O11W 2.226(6) . ? Cu2 O20 1.947(3) 4_565 ? Cu2 O15 1.957(3) . ? Cu2 O7 1.989(3) . ? Cu2 O13W 2.036(4) . ? Cu2 O12W 2.231(5) . ? Pr1 O5 2.421(4) 4_565 ? Pr1 O1 2.426(4) . ? Pr1 O11 2.434(4) . ? Pr1 O2W 2.526(4) . ? Pr1 O3W 2.536(4) . ? Pr1 O18 2.548(4) 4_465 ? Pr1 O4W 2.579(4) . ? Pr1 O1W 2.584(4) . ? Pr1 O17 2.642(4) 4_465 ? Pr1 C28 2.947(5) 4_465 ? Pr2 O19 2.415(4) . ? Pr2 O16 2.439(4) 4_666 ? Pr2 O9W 2.490(5) . ? Pr2 O8W 2.500(6) . ? Pr2 O6W 2.511(6) . ? Pr2 O7W 2.537(6) . ? Pr2 O3 2.553(4) 4_766 ? Pr2 O5W 2.564(5) . ? Pr2 O4 2.589(4) 4_766 ? Pr2 C8 2.926(5) 4_766 ? O1 C7 1.242(6) . ? O2 C7 1.266(6) . ? O2 Cu1 1.959(3) 4_565 ? O3 C8 1.266(6) . ? O3 Pr2 2.553(3) 4_465 ? O4 C8 1.250(6) . ? O4 Pr2 2.589(4) 4_465 ? O5 C9 1.250(6) . ? O5 Pr1 2.421(4) 4_666 ? O6 C9 1.264(6) . ? O7 C10 1.264(6) . ? O8 C10 1.236(7) . ? O9 C14 1.276(7) . ? O10 C14 1.250(7) . ? O11 C15 1.259(7) . ? O12 C15 1.239(8) . ? O13 C26 1.260(6) . ? O14 C26 1.231(7) . ? O15 C27 1.262(6) . ? O16 C27 1.246(6) . ? O16 Pr2 2.439(4) 4_565 ? O17 C28 1.253(6) . ? O17 Pr1 2.642(4) 4_766 ? O18 C28 1.269(6) . ? O18 Pr1 2.548(4) 4_766 ? O19 C29 1.256(6) . ? O20 C29 1.260(6) . ? O20 Cu2 1.947(3) 4_666 ? C1 C6 1.394(7) . ? C1 C2 1.407(6) . ? C1 C7 1.503(6) . ? C2 C3 1.384(6) . ? C2 C8 1.498(6) . ? C3 C4 1.393(7) . ? C4 C5 1.402(6) . ? C4 C9 1.493(6) . ? C5 C6 1.391(6) . ? C5 C10 1.504(6) . ? C8 Pr2 2.926(5) 4_465 ? C11 C13 1.384(7) 3_556 ? C11 C12 1.401(7) . ? C11 C14 1.506(6) . ? C12 C13 1.399(7) . ? C12 C15 1.493(8) . ? C13 C11 1.384(7) 3_556 ? C20 C25 1.391(6) . ? C20 C21 1.395(6) . ? C20 C26 1.512(6) . ? C21 C22 1.388(6) . ? C21 C27 1.508(6) . ? C22 C23 1.389(6) . ? C23 C24 1.404(6) . ? C23 C28 1.511(6) . ? C24 C25 1.399(6) . ? C24 C29 1.492(6) . ? C28 Pr1 2.947(5) 4_766 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O6 172.22(17) 4_666 . ? O2 Cu1 O13 89.82(16) 4_666 . ? O6 Cu1 O13 88.79(15) . . ? O2 Cu1 O10W 88.03(16) 4_666 . ? O6 Cu1 O10W 91.42(16) . . ? O13 Cu1 O10W 165.58(17) . . ? O2 Cu1 O11W 91.3(2) 4_666 . ? O6 Cu1 O11W 96.5(2) . . ? O13 Cu1 O11W 100.5(3) . . ? O10W Cu1 O11W 93.8(3) . . ? O20 Cu2 O15 172.45(17) 4_565 . ? O20 Cu2 O7 88.65(15) 4_565 . ? O15 Cu2 O7 90.67(15) . . ? O20 Cu2 O13W 88.73(15) 4_565 . ? O15 Cu2 O13W 89.84(15) . . ? O7 Cu2 O13W 163.81(16) . . ? O20 Cu2 O12W 93.17(16) 4_565 . ? O15 Cu2 O12W 94.37(16) . . ? O7 Cu2 O12W 97.20(16) . . ? O13W Cu2 O12W 98.89(16) . . ? O5 Pr1 O1 84.79(13) 4_565 . ? O5 Pr1 O11 139.85(14) 4_565 . ? O1 Pr1 O11 81.96(14) . . ? O5 Pr1 O2W 132.13(14) 4_565 . ? O1 Pr1 O2W 142.74(14) . . ? O11 Pr1 O2W 71.77(14) . . ? O5 Pr1 O3W 74.50(15) 4_565 . ? O1 Pr1 O3W 142.45(15) . . ? O11 Pr1 O3W 93.95(18) . . ? O2W Pr1 O3W 67.10(15) . . ? O5 Pr1 O18 70.52(13) 4_565 4_465 ? O1 Pr1 O18 70.56(12) . 4_465 ? O11 Pr1 O18 137.31(13) . 4_465 ? O2W Pr1 O18 112.48(13) . 4_465 ? O3W Pr1 O18 127.67(16) . 4_465 ? O5 Pr1 O4W 68.93(14) 4_565 . ? O1 Pr1 O4W 72.25(13) . . ? O11 Pr1 O4W 70.94(14) . . ? O2W Pr1 O4W 120.56(13) . . ? O3W Pr1 O4W 71.17(15) . . ? O18 Pr1 O4W 126.39(13) 4_465 . ? O5 Pr1 O1W 141.20(13) 4_565 . ? O1 Pr1 O1W 76.97(13) . . ? O11 Pr1 O1W 71.21(13) . . ? O2W Pr1 O1W 69.89(13) . . ? O3W Pr1 O1W 136.98(15) . . ? O18 Pr1 O1W 71.18(12) 4_465 . ? O4W Pr1 O1W 133.71(13) . . ? O5 Pr1 O17 76.22(14) 4_565 4_465 ? O1 Pr1 O17 120.80(13) . 4_465 ? O11 Pr1 O17 142.04(13) . 4_465 ? O2W Pr1 O17 72.83(13) . 4_465 ? O3W Pr1 O17 84.61(16) . 4_465 ? O18 Pr1 O17 50.24(12) 4_465 4_465 ? O4W Pr1 O17 141.59(14) . 4_465 ? O1W Pr1 O17 84.16(14) . 4_465 ? O5 Pr1 C28 68.67(14) 4_565 4_465 ? O1 Pr1 C28 95.76(14) . 4_465 ? O11 Pr1 C28 150.24(13) . 4_465 ? O2W Pr1 C28 94.45(14) . 4_465 ? O3W Pr1 C28 104.99(17) . 4_465 ? O18 Pr1 C28 25.40(12) 4_465 4_465 ? O4W Pr1 C28 136.74(14) . 4_465 ? O1W Pr1 C28 79.33(13) . 4_465 ? O17 Pr1 C28 25.17(13) 4_465 4_465 ? O19 Pr2 O16 84.36(14) . 4_666 ? O19 Pr2 O9W 81.56(18) . . ? O16 Pr2 O9W 139.91(17) 4_666 . ? O19 Pr2 O8W 83.3(2) . . ? O16 Pr2 O8W 141.4(2) 4_666 . ? O9W Pr2 O8W 73.5(2) . . ? O19 Pr2 O6W 140.9(2) . . ? O16 Pr2 O6W 72.88(19) 4_666 . ? O9W Pr2 O6W 135.5(2) . . ? O8W Pr2 O6W 94.9(3) . . ? O19 Pr2 O7W 145.89(19) . . ? O16 Pr2 O7W 129.51(19) 4_666 . ? O9W Pr2 O7W 69.4(2) . . ? O8W Pr2 O7W 71.8(3) . . ? O6W Pr2 O7W 66.1(2) . . ? O19 Pr2 O3 70.62(13) . 4_766 ? O16 Pr2 O3 70.40(13) 4_666 4_766 ? O9W Pr2 O3 69.52(16) . 4_766 ? O8W Pr2 O3 137.1(2) . 4_766 ? O6W Pr2 O3 126.8(2) . 4_766 ? O7W Pr2 O3 113.0(2) . 4_766 ? O19 Pr2 O5W 71.27(16) . . ? O16 Pr2 O5W 71.43(17) 4_666 . ? O9W Pr2 O5W 136.4(2) . . ? O8W Pr2 O5W 70.0(2) . . ? O6W Pr2 O5W 71.5(2) . . ? O7W Pr2 O5W 118.7(2) . . ? O3 Pr2 O5W 127.68(14) 4_766 . ? O19 Pr2 O4 121.19(13) . 4_766 ? O16 Pr2 O4 74.58(14) 4_666 4_766 ? O9W Pr2 O4 81.13(19) . 4_766 ? O8W Pr2 O4 141.7(2) . 4_766 ? O6W Pr2 O4 83.3(2) . 4_766 ? O7W Pr2 O4 72.6(2) . 4_766 ? O3 Pr2 O4 50.65(11) 4_766 4_766 ? O5W Pr2 O4 142.26(18) . 4_766 ? O19 Pr2 C8 95.93(14) . 4_766 ? O16 Pr2 C8 68.38(14) 4_666 4_766 ? O9W Pr2 C8 76.00(18) . 4_766 ? O8W Pr2 C8 149.3(2) . 4_766 ? O6W Pr2 C8 104.2(2) . 4_766 ? O7W Pr2 C8 94.1(2) . 4_766 ? O3 Pr2 C8 25.57(12) 4_766 4_766 ? O5W Pr2 C8 138.81(16) . 4_766 ? O4 Pr2 C8 25.26(13) 4_766 4_766 ? C7 O1 Pr1 168.5(3) . . ? C7 O2 Cu1 114.5(3) . 4_565 ? C8 O3 Pr2 93.9(3) . 4_465 ? C8 O4 Pr2 92.6(3) . 4_465 ? C9 O5 Pr1 166.3(4) . 4_666 ? C9 O6 Cu1 110.5(3) . . ? C10 O7 Cu2 123.2(3) . . ? C15 O11 Pr1 138.7(4) . . ? C26 O13 Cu1 125.2(3) . . ? C27 O15 Cu2 109.6(3) . . ? C27 O16 Pr2 170.8(4) . 4_565 ? C28 O17 Pr1 91.2(3) . 4_766 ? C28 O18 Pr1 95.2(3) . 4_766 ? C29 O19 Pr2 164.8(3) . . ? C29 O20 Cu2 115.8(3) . 4_666 ? C6 C1 C2 119.7(4) . . ? C6 C1 C7 118.3(4) . . ? C2 C1 C7 121.9(4) . . ? C3 C2 C1 119.4(4) . . ? C3 C2 C8 118.8(4) . . ? C1 C2 C8 121.3(4) . . ? C2 C3 C4 121.2(4) . . ? C3 C4 C5 119.2(4) . . ? C3 C4 C9 118.5(4) . . ? C5 C4 C9 122.2(4) . . ? C6 C5 C4 120.0(4) . . ? C6 C5 C10 117.8(4) . . ? C4 C5 C10 121.9(4) . . ? C5 C6 C1 120.4(4) . . ? O1 C7 O2 125.2(4) . . ? O1 C7 C1 119.0(4) . . ? O2 C7 C1 115.7(4) . . ? O4 C8 O3 122.0(4) . . ? O4 C8 C2 120.2(4) . . ? O3 C8 C2 117.7(4) . . ? O4 C8 Pr2 62.1(3) . 4_465 ? O3 C8 Pr2 60.5(2) . 4_465 ? C2 C8 Pr2 167.3(3) . 4_465 ? O5 C9 O6 124.3(4) . . ? O5 C9 C4 118.0(4) . . ? O6 C9 C4 117.7(4) . . ? O8 C10 O7 125.8(5) . . ? O8 C10 C5 118.9(4) . . ? O7 C10 C5 115.1(4) . . ? C13 C11 C12 119.9(4) 3_556 . ? C13 C11 C14 116.9(4) 3_556 . ? C12 C11 C14 123.1(4) . . ? C13 C12 C11 119.2(5) . . ? C13 C12 C15 118.6(5) . . ? C11 C12 C15 122.1(5) . . ? C11 C13 C12 120.9(5) 3_556 . ? O10 C14 O9 123.6(5) . . ? O10 C14 C11 119.2(5) . . ? O9 C14 C11 117.1(5) . . ? O12 C15 O11 124.7(6) . . ? O12 C15 C12 116.9(5) . . ? O11 C15 C12 118.4(5) . . ? C25 C20 C21 119.4(4) . . ? C25 C20 C26 116.6(4) . . ? C21 C20 C26 123.8(4) . . ? C22 C21 C20 119.8(4) . . ? C22 C21 C27 118.4(4) . . ? C20 C21 C27 121.6(4) . . ? C21 C22 C23 121.1(4) . . ? C22 C23 C24 119.6(4) . . ? C22 C23 C28 119.2(4) . . ? C24 C23 C28 120.5(4) . . ? C25 C24 C23 118.9(4) . . ? C25 C24 C29 118.1(4) . . ? C23 C24 C29 122.9(4) . . ? C20 C25 C24 121.2(4) . . ? O14 C26 O13 124.9(5) . . ? O14 C26 C20 119.3(5) . . ? O13 C26 C20 115.6(4) . . ? O16 C27 O15 123.8(4) . . ? O16 C27 C21 118.9(4) . . ? O15 C27 C21 117.2(4) . . ? O17 C28 O18 121.8(4) . . ? O17 C28 C23 120.9(4) . . ? O18 C28 C23 117.1(4) . . ? O17 C28 Pr1 63.7(3) . 4_766 ? O18 C28 Pr1 59.4(2) . 4_766 ? C23 C28 Pr1 163.7(3) . 4_766 ? O19 C29 O20 125.1(4) . . ? O19 C29 C24 118.2(5) . . ? O20 C29 C24 116.5(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.92 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.972 _refine_diff_density_min -1.472 _refine_diff_density_rms 0.206 # Attachment '- 1b_100K.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 806346' #TrackingRef '- 1b_100K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H45 Cu2 O40 Pr2' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour light_blue _diffrn_ambient_temperature 100(2) _chemical_formula_weight 1394.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.906(2) _cell_length_b 20.212(4) _cell_length_c 19.769(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.22(3) _cell_angle_gamma 90.00 _cell_volume 4301.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2772 _exptl_absorpt_coefficient_mu 3.835 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.7320 _exptl_absorpt_correction_T_max 0.8513 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7513 _diffrn_source synchrotron _diffrn_source_type 'ESRF-CRG BM16' _diffrn_radiation_monochromator 'Si 111' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9.6 _diffrn_radiation_detector 'ADSC Q210r CCD (binned mode)' _diffrn_measurement_device_type 'Single-axis HUBER diffractometer' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 264668 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.80 _reflns_number_total 9480 _reflns_number_gt 8857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MxCube (ESRF, 2006)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+41.8932P] 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 9480 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1374 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 Pr1 Pr -0.46760(2) 0.126313(13) 0.345064(13) 0.00827(9) Uani 1 1 d . . . Pr2 Pr 0.83304(3) 0.123936(13) 1.082800(13) 0.00940(9) Uani 1 1 d . . . Cu1 Cu 0.07202(6) 0.17265(3) 0.83172(3) 0.00919(14) Uani 1 1 d . . . Cu2 Cu 0.28846(5) 0.17465(3) 0.58907(3) 0.00876(14) Uani 1 1 d . . . C1 C -0.2618(5) 0.2610(3) 0.5215(2) 0.0107(9) Uani 1 1 d . . . C2 C -0.2938(5) 0.2972(3) 0.5764(3) 0.0111(9) Uani 1 1 d . . . C3 C -0.2196(5) 0.2935(3) 0.6407(2) 0.0108(9) Uani 1 1 d . . . H3 H -0.2383 0.3194 0.6765 0.013 Uiso 1 1 calc R . . C4 C -0.1179(5) 0.2512(3) 0.6514(2) 0.0106(9) Uani 1 1 d . . . C5 C -0.0859(5) 0.2144(3) 0.5969(2) 0.0104(9) Uani 1 1 d . . . C6 C -0.1577(5) 0.2199(3) 0.5318(3) 0.0120(9) Uani 1 1 d . . . H6 H -0.1360 0.1961 0.4952 0.014 Uiso 1 1 calc R . . C7 C -0.3321(4) 0.2683(3) 0.4500(2) 0.0097(9) Uani 1 1 d . . . C8 C -0.4160(5) 0.3329(3) 0.5716(2) 0.0108(9) Uani 1 1 d . . . C9 C -0.0515(4) 0.2412(3) 0.7227(2) 0.0101(9) Uani 1 1 d . . . C10 C 0.0299(5) 0.1722(3) 0.6059(2) 0.0102(9) Uani 1 1 d . . . C11 C -0.1264(5) -0.0139(3) 0.4871(3) 0.0116(9) Uani 1 1 d . . . C12 C -0.0776(4) 0.0340(2) 0.4478(2) 0.0099(9) Uani 1 1 d . . . C13 C 0.0490(5) 0.0470(3) 0.4607(3) 0.0118(9) Uani 1 1 d . . . H13 H 0.0826 0.0782 0.4343 0.014 Uiso 1 1 calc R . . C14 C -0.2617(5) -0.0320(3) 0.4751(3) 0.0117(9) Uani 1 1 d . . . C15 C -0.1598(5) 0.0741(3) 0.3942(3) 0.0119(9) Uani 1 1 d . . . C20 C 0.4494(5) 0.2057(3) 0.8265(2) 0.0105(9) Uani 1 1 d . . . C21 C 0.4792(5) 0.2430(3) 0.7718(3) 0.0119(9) Uani 1 1 d . . . C22 C 0.5816(5) 0.2857(3) 0.7830(3) 0.0128(10) Uani 1 1 d . . . H22 H 0.5992 0.3119 0.7471 0.015 Uiso 1 1 calc R . . C23 C 0.6571(4) 0.2897(3) 0.8462(3) 0.0112(9) Uani 1 1 d . . . C24 C 0.6273(4) 0.2516(3) 0.9008(2) 0.0092(9) Uani 1 1 d . . . C25 C 0.5252(5) 0.2099(3) 0.8909(3) 0.0114(9) Uani 1 1 d . . . H25 H 0.5067 0.1845 0.9272 0.014 Uiso 1 1 calc R . . C27 C 0.4096(5) 0.2348(3) 0.7007(3) 0.0118(9) Uani 1 1 d . . . C28 C 0.7768(5) 0.3284(3) 0.8537(2) 0.0108(9) Uani 1 1 d . . . C29 C 0.6957(4) 0.2584(3) 0.9728(2) 0.0097(9) Uani 1 1 d . . . O1 O -0.3664(3) 0.21728(19) 0.41589(18) 0.0122(7) Uani 1 1 d . . . O2 O -0.3465(4) 0.32689(19) 0.42729(18) 0.0128(7) Uani 1 1 d . . . O3 O -0.5088(3) 0.30793(18) 0.53358(18) 0.0110(7) Uani 1 1 d . . . O4 O -0.4263(4) 0.38292(19) 0.6079(2) 0.0138(7) Uani 1 1 d . . . O5 O -0.0445(4) 0.28809(19) 0.76432(18) 0.0142(7) Uani 1 1 d . . . O6 O -0.0091(3) 0.18401(19) 0.73727(18) 0.0132(7) Uani 1 1 d . . . O7 O 0.1310(3) 0.20651(19) 0.61441(18) 0.0122(7) Uani 1 1 d . . . O8 O 0.0239(4) 0.11182(19) 0.6021(2) 0.0159(8) Uani 1 1 d . . . O9 O -0.3065(3) -0.06637(19) 0.42413(19) 0.0141(7) Uani 1 1 d . . . O10 O -0.3239(3) -0.01214(19) 0.52025(19) 0.0151(7) Uani 1 1 d . . . O11 O -0.2754(3) 0.07446(19) 0.39646(19) 0.0128(7) Uani 1 1 d . . . O12 O -0.1088(4) 0.1058(2) 0.3516(2) 0.0188(8) Uani 1 1 d . . . O13 O 0.2315(3) 0.19662(18) 0.80321(17) 0.0112(7) Uani 1 1 d . . . O14 O 0.3388(4) 0.1070(2) 0.8436(2) 0.0184(8) Uani 1 1 d . . . O15 O 0.3676(3) 0.17725(19) 0.68455(18) 0.0121(7) Uani 1 1 d . . . O16 O 0.4012(3) 0.2831(2) 0.66028(19) 0.0147(7) Uani 1 1 d . . . O17 O 0.7851(4) 0.38107(19) 0.8212(2) 0.0152(8) Uani 1 1 d . . . O18 O 0.8708(3) 0.30260(19) 0.89071(18) 0.0127(7) Uani 1 1 d . . . O19 O 0.7242(3) 0.20695(19) 1.00757(18) 0.0130(7) Uani 1 1 d . . . O20 O 0.7129(3) 0.31714(18) 0.99410(18) 0.0122(7) Uani 1 1 d . . . O1W O -0.4879(3) 0.08937(19) 0.46614(19) 0.0137(7) Uani 1 1 d . . . O2W O -0.4948(4) 0.00112(19) 0.3450(2) 0.0191(8) Uani 1 1 d . . . O3W O -0.4883(5) 0.0793(2) 0.2268(2) 0.0257(10) Uani 1 1 d . . . O4W O -0.2920(3) 0.17205(18) 0.28557(18) 0.0124(7) Uani 1 1 d . . . O5W O 0.6568(4) 0.1626(2) 1.14459(19) 0.0155(8) Uani 1 1 d . . . O6W O 0.8660(6) 0.0763(2) 1.2043(2) 0.0383(13) Uani 1 1 d . . . O7W O 0.8750(4) 0.00202(19) 1.0795(2) 0.0197(8) Uani 1 1 d . . . O8W O 0.6398(4) 0.0620(2) 1.0380(2) 0.0242(9) Uani 1 1 d . . . O9W O 0.8834(4) 0.0806(2) 0.9700(2) 0.0189(8) Uani 1 1 d . . . O10W O -0.0919(4) 0.1738(2) 0.8664(2) 0.0165(8) Uani 1 1 d . . . O11W O 0.0556(4) 0.0647(2) 0.8067(2) 0.0220(9) Uani 1 1 d . . . O13W O 0.4593(3) 0.18074(19) 0.55983(18) 0.0128(7) Uani 1 1 d . . . C26 C 0.3318(5) 0.1648(3) 0.8231(2) 0.0107(9) Uani 1 1 d . . . O1X O 0.7488(4) -0.0257(2) 0.9138(2) 0.0239(9) Uani 1 1 d . . . O2X O 0.8088(4) 0.0596(2) 0.6234(3) 0.0289(10) Uani 1 1 d . . . O3X O 0.6157(4) -0.0754(2) 1.0124(2) 0.0259(9) Uani 1 1 d . . . O4X O 0.5478(5) 0.0366(2) 0.8371(3) 0.0341(11) Uani 1 1 d . . . O5X O 0.1931(5) 0.0470(3) 0.7090(2) 0.0315(11) Uani 1 1 d . . . O6X O 0.6279(5) 0.1248(3) 0.6641(3) 0.0428(14) Uani 1 1 d . . . O7X O 0.8443(5) -0.0035(3) 0.7430(3) 0.0463(15) Uani 1 1 d . . . O8X O 0.7289(5) 0.1083(3) 0.7925(3) 0.0370(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.00666(15) 0.01416(15) 0.00387(14) 0.00059(9) 0.00052(10) 0.00046(9) Pr2 0.00999(16) 0.01354(15) 0.00480(15) 0.00061(9) 0.00159(10) -0.00001(9) Cu1 0.0085(3) 0.0157(3) 0.0032(3) 0.0001(2) 0.0003(2) -0.0005(2) Cu2 0.0080(3) 0.0154(3) 0.0026(3) -0.0002(2) 0.0000(2) 0.0002(2) C1 0.008(2) 0.017(2) 0.007(2) 0.0034(18) -0.0007(17) -0.0016(18) C2 0.010(2) 0.015(2) 0.008(2) 0.0005(18) 0.0020(18) -0.0003(18) C3 0.010(2) 0.016(2) 0.007(2) -0.0005(18) 0.0028(18) -0.0028(18) C4 0.009(2) 0.019(2) 0.003(2) -0.0016(18) -0.0018(17) -0.0043(18) C5 0.010(2) 0.015(2) 0.007(2) -0.0004(18) 0.0015(17) -0.0026(18) C6 0.012(2) 0.018(2) 0.006(2) -0.0014(18) 0.0022(18) -0.0005(19) C7 0.007(2) 0.017(2) 0.006(2) 0.0003(17) 0.0029(17) -0.0002(18) C8 0.011(2) 0.016(2) 0.006(2) 0.0021(17) 0.0034(18) -0.0004(18) C9 0.007(2) 0.021(2) 0.003(2) -0.0015(18) 0.0033(17) -0.0034(18) C10 0.009(2) 0.019(2) 0.002(2) -0.0014(17) -0.0009(17) 0.0003(18) C11 0.009(2) 0.015(2) 0.011(2) -0.0005(18) 0.0029(18) -0.0010(18) C12 0.006(2) 0.016(2) 0.008(2) 0.0020(18) 0.0007(17) 0.0019(17) C13 0.007(2) 0.017(2) 0.012(2) 0.0000(18) 0.0032(18) -0.0019(18) C14 0.010(2) 0.016(2) 0.010(2) 0.0031(18) 0.0020(18) 0.0004(18) C15 0.011(2) 0.016(2) 0.009(2) 0.0004(18) 0.0026(18) 0.0002(18) C20 0.011(2) 0.016(2) 0.005(2) -0.0009(18) 0.0008(17) 0.0010(18) C21 0.008(2) 0.017(2) 0.010(2) -0.0006(19) 0.0015(18) 0.0021(18) C22 0.010(2) 0.021(3) 0.007(2) 0.0013(19) 0.0023(18) 0.0006(19) C23 0.006(2) 0.018(2) 0.010(2) -0.0011(19) 0.0022(18) 0.0001(18) C24 0.006(2) 0.017(2) 0.005(2) -0.0008(17) -0.0002(17) 0.0005(17) C25 0.012(2) 0.017(2) 0.007(2) 0.0003(18) 0.0032(18) -0.0004(19) C27 0.010(2) 0.020(2) 0.007(2) 0.0026(18) 0.0040(18) 0.0010(19) C28 0.009(2) 0.018(2) 0.005(2) -0.0016(18) 0.0004(17) 0.0003(18) C29 0.005(2) 0.018(2) 0.007(2) 0.0010(18) 0.0018(17) 0.0018(17) O1 0.0085(16) 0.0198(19) 0.0075(16) -0.0028(14) -0.0011(13) -0.0022(14) O2 0.0160(18) 0.0184(18) 0.0037(15) 0.0012(13) 0.0009(13) 0.0004(14) O3 0.0090(16) 0.0160(17) 0.0075(16) 0.0006(13) -0.0004(13) -0.0003(13) O4 0.0117(18) 0.0180(18) 0.0122(18) -0.0027(14) 0.0034(14) -0.0004(14) O5 0.0153(18) 0.0194(18) 0.0073(16) -0.0033(14) 0.0005(14) -0.0033(14) O6 0.0135(18) 0.0186(18) 0.0071(16) -0.0005(14) 0.0001(13) 0.0037(14) O7 0.0100(17) 0.0195(18) 0.0070(16) -0.0026(13) 0.0014(13) -0.0021(14) O8 0.0139(19) 0.0164(18) 0.0164(19) -0.0034(15) -0.0009(15) 0.0004(15) O9 0.0104(17) 0.0176(18) 0.0127(17) -0.0011(14) -0.0026(14) -0.0002(14) O10 0.0101(18) 0.0212(19) 0.0147(18) 0.0017(15) 0.0037(14) -0.0004(14) O11 0.0055(16) 0.0203(19) 0.0125(17) 0.0036(14) 0.0009(13) -0.0002(13) O12 0.0099(18) 0.027(2) 0.020(2) 0.0124(17) 0.0044(15) 0.0017(15) O13 0.0084(16) 0.0196(18) 0.0057(16) 0.0007(13) 0.0015(13) 0.0002(13) O14 0.018(2) 0.0152(19) 0.021(2) 0.0025(15) 0.0008(16) -0.0019(15) O15 0.0106(17) 0.0204(19) 0.0053(16) -0.0001(13) 0.0012(13) -0.0002(14) O16 0.0107(17) 0.026(2) 0.0070(16) 0.0030(14) -0.0004(13) -0.0016(15) O17 0.0137(19) 0.0196(19) 0.0125(18) 0.0035(14) 0.0025(15) -0.0013(14) O18 0.0115(17) 0.0196(18) 0.0067(16) 0.0003(14) 0.0008(13) -0.0004(14) O19 0.0113(17) 0.0182(18) 0.0088(16) 0.0019(14) -0.0008(13) 0.0006(14) O20 0.0137(18) 0.0170(18) 0.0061(16) -0.0008(13) 0.0019(13) 0.0001(14) O1W 0.0130(18) 0.0162(18) 0.0131(18) 0.0017(14) 0.0053(14) 0.0004(14) O2W 0.024(2) 0.0149(19) 0.0167(19) 0.0004(15) -0.0019(16) -0.0018(16) O3W 0.039(3) 0.023(2) 0.017(2) -0.0063(16) 0.0107(18) -0.0107(19) O4W 0.0152(18) 0.0170(18) 0.0054(16) -0.0009(13) 0.0024(13) -0.0003(14) O5W 0.0153(19) 0.0198(19) 0.0119(18) 0.0010(14) 0.0033(14) -0.0008(15) O6W 0.078(4) 0.026(2) 0.011(2) 0.0046(17) 0.005(2) 0.018(2) O7W 0.030(2) 0.0148(19) 0.0135(19) 0.0009(15) 0.0011(16) 0.0016(16) O8W 0.020(2) 0.023(2) 0.029(2) -0.0055(18) 0.0024(18) -0.0019(16) O9W 0.028(2) 0.021(2) 0.0088(17) 0.0001(15) 0.0039(15) -0.0038(16) O10W 0.0164(19) 0.0203(19) 0.0140(18) 0.0017(15) 0.0064(15) -0.0012(15) O11W 0.036(2) 0.019(2) 0.0090(18) 0.0017(15) -0.0003(16) 0.0004(17) O13W 0.0114(17) 0.0194(18) 0.0082(16) -0.0007(14) 0.0030(13) -0.0007(14) C26 0.011(2) 0.017(2) 0.004(2) -0.0005(18) 0.0020(17) 0.0009(18) O1X 0.019(2) 0.021(2) 0.031(2) -0.0045(17) 0.0032(18) -0.0001(16) O2X 0.023(2) 0.028(2) 0.035(3) -0.0025(19) 0.0029(19) -0.0062(18) O3X 0.025(2) 0.024(2) 0.027(2) 0.0035(18) -0.0017(18) -0.0045(18) O4X 0.027(2) 0.028(2) 0.044(3) -0.010(2) -0.006(2) 0.0028(19) O5X 0.039(3) 0.035(3) 0.024(2) -0.0011(19) 0.013(2) 0.000(2) O6X 0.033(3) 0.063(4) 0.032(3) 0.006(2) 0.002(2) 0.010(2) O7X 0.038(3) 0.077(4) 0.023(3) -0.011(3) 0.003(2) -0.027(3) O8X 0.033(3) 0.048(3) 0.029(3) -0.002(2) 0.002(2) -0.012(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 Pr1 O5 2.412(4) 4_565 ? Pr1 O11 2.417(4) . ? Pr1 O1 2.462(4) . ? Pr1 O3W 2.500(4) . ? Pr1 O2W 2.548(4) . ? Pr1 O18 2.549(4) 4_465 ? Pr1 O1W 2.551(4) . ? Pr1 O4W 2.574(4) . ? Pr1 O17 2.667(4) 4_465 ? Pr1 C28 2.965(5) 4_465 ? Pr2 O19 2.423(4) . ? Pr2 O16 2.462(4) 4_666 ? Pr2 O8W 2.488(4) . ? Pr2 O7W 2.509(4) . ? Pr2 O3 2.521(4) 4_766 ? Pr2 O9W 2.538(4) . ? Pr2 O6W 2.559(4) . ? Pr2 O5W 2.559(4) . ? Pr2 O4 2.595(4) 4_766 ? Pr2 C8 2.915(5) 4_766 ? Cu2 O20 1.933(4) 4_565 ? Cu2 O15 1.946(4) . ? Cu2 O7 1.973(4) . ? Cu2 O13W 2.041(4) . ? Cu2 O9 2.217(4) 3_556 ? Cu1 O6 1.947(4) . ? Cu1 O2 1.955(4) 4_666 ? Cu1 O13 1.973(4) . ? Cu1 O10W 2.015(4) . ? Cu1 O11W 2.237(4) . ? C1 C6 1.395(7) . ? C1 C2 1.400(7) . ? C1 C7 1.503(7) . ? C2 C3 1.394(7) . ? C2 C8 1.505(7) . ? C3 C4 1.389(7) . ? C4 C5 1.400(7) . ? C4 C9 1.492(6) . ? C5 C6 1.400(7) . ? C5 C10 1.510(7) . ? C7 O1 1.256(6) . ? C7 O2 1.267(6) . ? C8 O4 1.257(6) . ? C8 O3 1.264(6) . ? C8 Pr2 2.915(5) 4_465 ? C9 O5 1.250(6) . ? C9 O6 1.260(7) . ? C10 O8 1.224(6) . ? C10 O7 1.290(6) . ? C11 C13 1.394(7) 3_556 ? C11 C12 1.400(7) . ? C11 C14 1.501(7) . ? C12 C13 1.389(7) . ? C12 C15 1.509(7) . ? C13 C11 1.394(7) 3_556 ? C14 O9 1.257(6) . ? C14 O10 1.270(6) . ? C15 O12 1.257(6) . ? C15 O11 1.268(6) . ? C20 C21 1.399(7) . ? C20 C25 1.405(7) . ? C20 C26 1.518(7) . ? C21 C22 1.399(7) . ? C21 C27 1.496(7) . ? C22 C23 1.384(7) . ? C23 C24 1.407(7) . ? C23 C28 1.509(7) . ? C24 C25 1.384(7) . ? C24 C29 1.504(6) . ? C27 O16 1.256(6) . ? C27 O15 1.272(7) . ? C28 O17 1.254(6) . ? C28 O18 1.272(6) . ? C28 Pr1 2.965(5) 4_766 ? C29 O19 1.258(6) . ? C29 O20 1.263(6) . ? O2 Cu1 1.955(4) 4_565 ? O3 Pr2 2.521(4) 4_465 ? O4 Pr2 2.595(4) 4_465 ? O5 Pr1 2.412(4) 4_666 ? O9 Cu2 2.217(4) 3_556 ? O13 C26 1.274(6) . ? O14 C26 1.236(7) . ? O16 Pr2 2.462(4) 4_565 ? O17 Pr1 2.667(4) 4_766 ? O18 Pr1 2.549(4) 4_766 ? O20 Cu2 1.933(4) 4_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Pr1 O11 140.86(13) 4_565 . ? O5 Pr1 O1 85.26(13) 4_565 . ? O11 Pr1 O1 78.77(13) . . ? O5 Pr1 O3W 71.59(14) 4_565 . ? O11 Pr1 O3W 99.81(15) . . ? O1 Pr1 O3W 141.33(13) . . ? O5 Pr1 O2W 133.17(13) 4_565 . ? O11 Pr1 O2W 70.27(13) . . ? O1 Pr1 O2W 141.56(13) . . ? O3W Pr1 O2W 68.21(14) . . ? O5 Pr1 O18 69.09(12) 4_565 4_465 ? O11 Pr1 O18 134.27(12) . 4_465 ? O1 Pr1 O18 69.52(12) . 4_465 ? O3W Pr1 O18 125.56(14) . 4_465 ? O2W Pr1 O18 118.23(13) . 4_465 ? O5 Pr1 O1W 139.27(12) 4_565 . ? O11 Pr1 O1W 71.25(12) . . ? O1 Pr1 O1W 77.50(12) . . ? O3W Pr1 O1W 139.26(13) . . ? O2W Pr1 O1W 71.46(13) . . ? O18 Pr1 O1W 70.34(12) 4_465 . ? O5 Pr1 O4W 69.22(12) 4_565 . ? O11 Pr1 O4W 71.90(12) . . ? O1 Pr1 O4W 72.13(12) . . ? O3W Pr1 O4W 70.84(13) . . ? O2W Pr1 O4W 116.84(13) . . ? O18 Pr1 O4W 124.52(12) 4_465 . ? O1W Pr1 O4W 135.79(12) . . ? O5 Pr1 O17 71.85(13) 4_565 4_465 ? O11 Pr1 O17 146.56(12) . 4_465 ? O1 Pr1 O17 119.38(12) . 4_465 ? O3W Pr1 O17 82.90(14) . 4_465 ? O2W Pr1 O17 80.22(13) . 4_465 ? O18 Pr1 O17 49.96(12) 4_465 4_465 ? O1W Pr1 O17 84.93(12) . 4_465 ? O4W Pr1 O17 138.14(12) . 4_465 ? O5 Pr1 C28 65.57(13) 4_565 4_465 ? O11 Pr1 C28 150.41(13) . 4_465 ? O1 Pr1 C28 94.40(13) . 4_465 ? O3W Pr1 C28 103.09(15) . 4_465 ? O2W Pr1 C28 101.31(14) . 4_465 ? O18 Pr1 C28 25.25(13) 4_465 4_465 ? O1W Pr1 C28 79.17(13) . 4_465 ? O4W Pr1 C28 133.69(13) . 4_465 ? O17 Pr1 C28 25.01(13) 4_465 4_465 ? O19 Pr2 O16 85.57(13) . 4_666 ? O19 Pr2 O8W 79.99(14) . . ? O16 Pr2 O8W 139.38(13) 4_666 . ? O19 Pr2 O7W 137.51(13) . . ? O16 Pr2 O7W 136.68(13) 4_666 . ? O8W Pr2 O7W 69.16(15) . . ? O19 Pr2 O3 71.52(12) . 4_766 ? O16 Pr2 O3 70.52(12) 4_666 4_766 ? O8W Pr2 O3 136.88(13) . 4_766 ? O7W Pr2 O3 112.80(13) . 4_766 ? O19 Pr2 O9W 81.56(13) . . ? O16 Pr2 O9W 136.38(13) 4_666 . ? O8W Pr2 O9W 78.69(14) . . ? O7W Pr2 O9W 64.65(13) . . ? O3 Pr2 O9W 65.87(12) 4_766 . ? O19 Pr2 O6W 144.87(15) . . ? O16 Pr2 O6W 73.73(15) 4_666 . ? O8W Pr2 O6W 97.39(18) . . ? O7W Pr2 O6W 69.92(14) . . ? O3 Pr2 O6W 124.46(17) 4_766 . ? O9W Pr2 O6W 132.68(14) . . ? O19 Pr2 O5W 75.52(12) . . ? O16 Pr2 O5W 69.20(12) 4_666 . ? O8W Pr2 O5W 70.47(14) . . ? O7W Pr2 O5W 117.81(13) . . ? O3 Pr2 O5W 129.04(12) 4_766 . ? O9W Pr2 O5W 144.11(13) . . ? O6W Pr2 O5W 70.74(16) . . ? O19 Pr2 O4 122.37(12) . 4_766 ? O16 Pr2 O4 74.13(12) 4_666 4_766 ? O8W Pr2 O4 144.48(13) . 4_766 ? O7W Pr2 O4 76.68(13) . 4_766 ? O3 Pr2 O4 50.93(12) 4_766 4_766 ? O9W Pr2 O4 78.18(13) . 4_766 ? O6W Pr2 O4 79.31(17) . 4_766 ? O5W Pr2 O4 137.61(12) . 4_766 ? O19 Pr2 C8 96.86(14) . 4_766 ? O16 Pr2 C8 68.01(13) 4_666 4_766 ? O8W Pr2 C8 151.07(14) . 4_766 ? O7W Pr2 C8 96.59(15) . 4_766 ? O3 Pr2 C8 25.61(13) 4_766 4_766 ? O9W Pr2 C8 72.42(14) . 4_766 ? O6W Pr2 C8 101.06(18) . 4_766 ? O5W Pr2 C8 136.97(13) . 4_766 ? O4 Pr2 C8 25.53(13) 4_766 4_766 ? O20 Cu2 O15 173.45(16) 4_565 . ? O20 Cu2 O7 88.03(15) 4_565 . ? O15 Cu2 O7 90.79(15) . . ? O20 Cu2 O13W 89.21(15) 4_565 . ? O15 Cu2 O13W 89.42(15) . . ? O7 Cu2 O13W 157.48(16) . . ? O20 Cu2 O9 90.15(15) 4_565 3_556 ? O15 Cu2 O9 96.13(15) . 3_556 ? O7 Cu2 O9 116.71(15) . 3_556 ? O13W Cu2 O9 85.64(15) . 3_556 ? O6 Cu1 O2 172.95(16) . 4_666 ? O6 Cu1 O13 89.02(15) . . ? O2 Cu1 O13 89.41(15) 4_666 . ? O6 Cu1 O10W 91.93(16) . . ? O2 Cu1 O10W 87.81(16) 4_666 . ? O13 Cu1 O10W 164.89(16) . . ? O6 Cu1 O11W 83.98(15) . . ? O2 Cu1 O11W 103.06(15) 4_666 . ? O13 Cu1 O11W 102.66(16) . . ? O10W Cu1 O11W 92.43(17) . . ? C6 C1 C2 119.8(4) . . ? C6 C1 C7 118.4(4) . . ? C2 C1 C7 121.7(5) . . ? C3 C2 C1 119.8(5) . . ? C3 C2 C8 117.6(4) . . ? C1 C2 C8 122.0(4) . . ? C4 C3 C2 120.4(5) . . ? C3 C4 C5 120.1(4) . . ? C3 C4 C9 118.9(4) . . ? C5 C4 C9 120.8(5) . . ? C4 C5 C6 119.6(5) . . ? C4 C5 C10 121.0(4) . . ? C6 C5 C10 119.2(4) . . ? C1 C6 C5 120.2(5) . . ? O1 C7 O2 124.6(5) . . ? O1 C7 C1 119.1(4) . . ? O2 C7 C1 116.1(4) . . ? O4 C8 O3 121.6(5) . . ? O4 C8 C2 120.6(5) . . ? O3 C8 C2 117.6(4) . . ? O4 C8 Pr2 62.9(3) . 4_465 ? O3 C8 Pr2 59.5(3) . 4_465 ? C2 C8 Pr2 166.3(3) . 4_465 ? O5 C9 O6 124.3(5) . . ? O5 C9 C4 119.2(5) . . ? O6 C9 C4 116.4(4) . . ? O8 C10 O7 125.5(5) . . ? O8 C10 C5 121.3(5) . . ? O7 C10 C5 113.2(4) . . ? C13 C11 C12 120.3(5) 3_556 . ? C13 C11 C14 117.6(4) 3_556 . ? C12 C11 C14 122.1(5) . . ? C13 C12 C11 119.0(5) . . ? C13 C12 C15 119.2(4) . . ? C11 C12 C15 121.7(4) . . ? C12 C13 C11 120.7(5) . 3_556 ? O9 C14 O10 123.7(5) . . ? O9 C14 C11 120.5(4) . . ? O10 C14 C11 115.7(4) . . ? O12 C15 O11 124.7(5) . . ? O12 C15 C12 117.8(4) . . ? O11 C15 C12 117.5(4) . . ? C21 C20 C25 119.4(5) . . ? C21 C20 C26 124.0(4) . . ? C25 C20 C26 116.4(4) . . ? C20 C21 C22 119.2(5) . . ? C20 C21 C27 121.4(5) . . ? C22 C21 C27 119.2(5) . . ? C23 C22 C21 121.5(5) . . ? C22 C23 C24 118.9(5) . . ? C22 C23 C28 120.0(5) . . ? C24 C23 C28 120.7(4) . . ? C25 C24 C23 120.3(4) . . ? C25 C24 C29 117.1(4) . . ? C23 C24 C29 122.4(4) . . ? C24 C25 C20 120.6(5) . . ? O16 C27 O15 124.4(5) . . ? O16 C27 C21 119.1(5) . . ? O15 C27 C21 116.5(4) . . ? O17 C28 O18 121.7(5) . . ? O17 C28 C23 121.5(5) . . ? O18 C28 C23 116.7(5) . . ? O17 C28 Pr1 64.1(3) . 4_766 ? O18 C28 Pr1 58.7(3) . 4_766 ? C23 C28 Pr1 163.9(3) . 4_766 ? O19 C29 O20 125.8(5) . . ? O19 C29 C24 118.8(5) . . ? O20 C29 C24 115.2(4) . . ? C7 O1 Pr1 170.5(3) . . ? C7 O2 Cu1 111.0(3) . 4_565 ? C8 O3 Pr2 94.9(3) . 4_465 ? C8 O4 Pr2 91.6(3) . 4_465 ? C9 O5 Pr1 163.4(3) . 4_666 ? C9 O6 Cu1 114.9(3) . . ? C10 O7 Cu2 123.5(3) . . ? C14 O9 Cu2 127.6(3) . 3_556 ? C15 O11 Pr1 142.0(3) . . ? C26 O13 Cu1 122.7(3) . . ? C27 O15 Cu2 110.7(3) . . ? C27 O16 Pr2 166.7(3) . 4_565 ? C28 O17 Pr1 90.9(3) . 4_766 ? C28 O18 Pr1 96.0(3) . 4_766 ? C29 O19 Pr2 164.1(3) . . ? C29 O20 Cu2 114.9(3) . 4_666 ? O14 C26 O13 125.7(5) . . ? O14 C26 C20 119.5(5) . . ? O13 C26 C20 114.6(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.80 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.201 _refine_diff_density_min -3.244 _refine_diff_density_rms 0.222 data_1b _database_code_depnum_ccdc_archive 'CCDC 853196' #TrackingRef '- 1b_293K.cif' _ccdc_journal_manuscript_code ? _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H45 Cu1 O40 Pr2' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour light_blue _diffrn_ambient_temperature 293(2) _chemical_formula_weight 1394.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.920(2) _cell_length_b 20.369(4) _cell_length_c 19.792(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.59(3) _cell_angle_gamma 90.00 _cell_volume 4340.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2764 _exptl_absorpt_coefficient_mu 3.633 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.7340 _exptl_absorpt_correction_T_max 0.8525 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.73880 _diffrn_source synchrotron _diffrn_source_type 'ESRF-CRG BM16' _diffrn_radiation_monochromator 'Si 111' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9.6 _diffrn_radiation_detector 'ADSC Q210r CCD (binned mode)' _diffrn_measurement_device_type 'Single-axis HUBER diffractometer' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36832 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9522 _reflns_number_gt 8815 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MxCube (ESRF, 2006)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+6.8835P] 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 9522 _refine_ls_number_parameters 621 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Pr1 Pr -0.462756(17) 0.127530(9) 0.345159(10) 0.02606(9) Uani 1 1 d . . . Pr2 Pr 0.839379(19) 0.126351(9) 1.081239(10) 0.02905(9) Uani 1 1 d . . . Cu1 Cu 0.07855(4) 0.17338(2) 0.83025(2) 0.02835(12) Uani 1 1 d . . . Cu2 Cu 0.29507(4) 0.17310(2) 0.58911(2) 0.02753(12) Uani 1 1 d . . . C1 C -0.2559(3) 0.26067(19) 0.51998(17) 0.0291(7) Uani 1 1 d . . . C2 C -0.2879(3) 0.29665(18) 0.57495(18) 0.0296(7) Uani 1 1 d . . . C3 C -0.2139(3) 0.29288(19) 0.63881(18) 0.0297(7) Uani 1 1 d . . . H3 H -0.2324 0.3185 0.6746 0.036 Uiso 1 1 calc R . . C4 C -0.1118(3) 0.25086(19) 0.64974(16) 0.0289(7) Uani 1 1 d . . . C5 C -0.0798(3) 0.21468(19) 0.59537(18) 0.0297(7) Uani 1 1 d . . . C6 C -0.1524(3) 0.2202(2) 0.53054(18) 0.0323(7) Uani 1 1 d . . . H6 H -0.1312 0.1964 0.4941 0.039 Uiso 1 1 calc R . . C7 C -0.3266(3) 0.26787(18) 0.44879(18) 0.0291(7) Uani 1 1 d . . . C8 C -0.4104(3) 0.33130(19) 0.56951(18) 0.0306(7) Uani 1 1 d . . . C9 C -0.0445(3) 0.2414(2) 0.72115(17) 0.0296(7) Uani 1 1 d . . . C10 C 0.0344(3) 0.17169(19) 0.60493(18) 0.0304(7) Uani 1 1 d . . . C11 C -0.1270(3) -0.01263(18) 0.48738(19) 0.0310(7) Uani 1 1 d . . . C12 C -0.0773(3) 0.03424(19) 0.44890(19) 0.0324(7) Uani 1 1 d . . . C13 C 0.0494(3) 0.04653(19) 0.46142(19) 0.0329(7) Uani 1 1 d . . . H13 H 0.0828 0.0777 0.4353 0.039 Uiso 1 1 calc R . . C14 C -0.2622(3) -0.03017(18) 0.47661(19) 0.0327(7) Uani 1 1 d . . . C15 C -0.1576(4) 0.0747(2) 0.3958(2) 0.0369(8) Uani 1 1 d . . . C20 C 0.4558(3) 0.20737(19) 0.82613(17) 0.0291(7) Uani 1 1 d . . . C21 C 0.4855(3) 0.24385(19) 0.77114(17) 0.0287(7) Uani 1 1 d . . . C22 C 0.5879(3) 0.2860(2) 0.78210(18) 0.0316(7) Uani 1 1 d . . . H22 H 0.6064 0.3114 0.7461 0.038 Uiso 1 1 calc R . . C23 C 0.6626(3) 0.29044(19) 0.84591(18) 0.0293(7) Uani 1 1 d . . . C24 C 0.6329(3) 0.25304(19) 0.90045(17) 0.0282(7) Uani 1 1 d . . . C25 C 0.5306(3) 0.21225(19) 0.89026(18) 0.0306(7) Uani 1 1 d . . . H25 H 0.5113 0.1877 0.9267 0.037 Uiso 1 1 calc R . . C27 C 0.4165(3) 0.23419(19) 0.70004(18) 0.0297(7) Uani 1 1 d . . . C28 C 0.7835(3) 0.32807(19) 0.85324(19) 0.0312(7) Uani 1 1 d . . . C29 C 0.7018(3) 0.26004(19) 0.97244(17) 0.0284(7) Uani 1 1 d . . . O1 O -0.3607(3) 0.21790(15) 0.41440(14) 0.0358(6) Uani 1 1 d . . . O2 O -0.3430(3) 0.32583(14) 0.42641(13) 0.0357(6) Uani 1 1 d . . . O3 O -0.5032(2) 0.30586(14) 0.53162(13) 0.0326(5) Uani 1 1 d . . . O4 O -0.4211(3) 0.38131(15) 0.60519(17) 0.0392(7) Uani 1 1 d . . . O5 O -0.0380(3) 0.28839(16) 0.76223(14) 0.0402(6) Uani 1 1 d . . . O6 O -0.0019(3) 0.18529(15) 0.73615(13) 0.0371(6) Uani 1 1 d . . . O7 O 0.1362(2) 0.20441(14) 0.61331(14) 0.0344(6) Uani 1 1 d . . . O8 O 0.0245(3) 0.11220(16) 0.60178(18) 0.0455(7) Uani 1 1 d . . . O9 O -0.3083(3) -0.06429(14) 0.42520(15) 0.0383(6) Uani 1 1 d . . . O10 O -0.3236(3) -0.01061(16) 0.52169(15) 0.0419(6) Uani 1 1 d . . . O11 O -0.2738(2) 0.07505(15) 0.39640(15) 0.0377(6) Uani 1 1 d . . . O12 O -0.1070(3) 0.1073(2) 0.3543(2) 0.0619(10) Uani 1 1 d . . . O13 O 0.2392(2) 0.19737(14) 0.80368(14) 0.0336(5) Uani 1 1 d . . . O14 O 0.3486(3) 0.10862(16) 0.84093(19) 0.0481(8) Uani 1 1 d . . . O15 O 0.3746(3) 0.17749(14) 0.68504(13) 0.0345(6) Uani 1 1 d . . . O16 O 0.4076(3) 0.28115(15) 0.65864(14) 0.0384(6) Uani 1 1 d . . . O17 O 0.7922(3) 0.38029(14) 0.82240(18) 0.0405(7) Uani 1 1 d . . . O18 O 0.8772(2) 0.30050(14) 0.88895(14) 0.0331(5) Uani 1 1 d . . . O19 O 0.7293(3) 0.20909(14) 1.00728(14) 0.0361(6) Uani 1 1 d . . . O20 O 0.7218(3) 0.31769(13) 0.99350(13) 0.0331(5) Uani 1 1 d . . . O1W O -0.4876(3) 0.08899(14) 0.46484(14) 0.0357(6) Uani 1 1 d . . . O2W O -0.5009(4) 0.00282(16) 0.34465(18) 0.0541(8) Uani 1 1 d . . . O3W O -0.4842(5) 0.0785(2) 0.2270(2) 0.0723(12) Uani 1 1 d . . . O4W O -0.2869(3) 0.17131(14) 0.28436(14) 0.0355(6) Uani 1 1 d . . . O5W O 0.6624(3) 0.16429(16) 1.14216(16) 0.0430(7) Uani 1 1 d . . . O6W O 0.8834(5) 0.07940(19) 1.20146(19) 0.0693(12) Uani 1 1 d . . . O7W O 0.8863(4) 0.00413(17) 1.07865(18) 0.0555(9) Uani 1 1 d . . . O8W O 0.6452(3) 0.0622(2) 1.0382(2) 0.0681(11) Uani 1 1 d . . . O9W O 0.8807(4) 0.08321(17) 0.96671(17) 0.0550(9) Uani 1 1 d . . . O10W O -0.0898(3) 0.17247(15) 0.86130(15) 0.0408(6) Uani 1 1 d . . . O11W O 0.0702(5) 0.06607(19) 0.8088(2) 0.0811(14) Uani 1 1 d . . . O13W O 0.4666(3) 0.17776(14) 0.56217(15) 0.0370(6) Uani 1 1 d . . . C26 C 0.3401(4) 0.16653(19) 0.82229(19) 0.0318(7) Uani 1 1 d . . . O1X O 0.7484(5) -0.0228(2) 0.9071(3) 0.0918(16) Uani 1 1 d . . . O2X O 0.8093(5) 0.0610(2) 0.6317(2) 0.0792(12) Uani 1 1 d . . . O3X O 0.6146(4) -0.0760(2) 1.0108(3) 0.0815(13) Uani 1 1 d . . . O4X O 0.5596(5) 0.0440(3) 0.8171(4) 0.113(2) Uani 1 1 d . . . O5X O 0.1914(5) 0.0443(3) 0.7074(2) 0.0946(18) Uani 1 1 d . . . O6X O 0.6504(18) 0.1251(8) 0.6789(15) 0.384(15) Uani 1 1 d . . . O7X O 0.8632(6) -0.0211(3) 0.7458(3) 0.114(2) Uani 1 1 d . . . O8X O 0.7318(10) 0.1215(7) 0.7669(8) 0.267(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.02273(14) 0.03147(13) 0.02367(13) 0.00103(6) 0.00298(9) 0.00113(6) Pr2 0.02921(14) 0.03176(14) 0.02638(14) 0.00088(6) 0.00516(10) -0.00123(7) Cu1 0.0271(2) 0.0359(2) 0.0214(2) 0.00036(16) 0.00226(17) -0.00093(16) Cu2 0.0257(2) 0.0354(2) 0.0208(2) -0.00068(15) 0.00170(16) 0.00072(16) C1 0.0253(16) 0.0384(18) 0.0230(15) -0.0016(13) 0.0022(13) -0.0024(14) C2 0.0267(17) 0.0351(18) 0.0271(16) -0.0009(14) 0.0051(13) 0.0011(14) C3 0.0252(16) 0.0388(18) 0.0249(16) -0.0031(14) 0.0037(13) -0.0006(14) C4 0.0267(16) 0.0411(18) 0.018 -0.0030(13) 0.0009(12) -0.0014(14) C5 0.0252(16) 0.0372(18) 0.0262(16) -0.0007(14) 0.0032(13) -0.0002(14) C6 0.0307(17) 0.044(2) 0.0235(16) -0.0038(14) 0.0065(14) 0.0013(15) C7 0.0238(15) 0.0402(19) 0.0233(15) -0.0004(13) 0.0040(13) 0.0006(14) C8 0.0286(17) 0.0379(19) 0.0257(16) 0.0050(14) 0.0054(13) 0.0015(14) C9 0.0242(16) 0.0434(19) 0.0211(15) -0.0017(14) 0.0034(12) -0.0035(14) C10 0.0282(17) 0.041(2) 0.0220(15) -0.0028(13) 0.0033(13) 0.0033(14) C11 0.0239(16) 0.0340(17) 0.0347(18) -0.0011(14) 0.0035(13) 0.0009(13) C12 0.0261(17) 0.0377(18) 0.0332(18) 0.0016(14) 0.0046(14) 0.0027(14) C13 0.0260(17) 0.0371(18) 0.0359(18) 0.0054(15) 0.0061(14) 0.0017(14) C14 0.0265(17) 0.0348(18) 0.0367(19) 0.0069(15) 0.0049(14) 0.0024(14) C15 0.0291(18) 0.041(2) 0.040(2) 0.0057(16) 0.0053(15) 0.0016(15) C20 0.0256(16) 0.0373(18) 0.0239(16) -0.0004(13) 0.0024(13) -0.0019(14) C21 0.0241(16) 0.0402(18) 0.0207(15) 0.0017(14) 0.0010(12) 0.0017(14) C22 0.0262(16) 0.043(2) 0.0253(16) 0.0026(14) 0.0030(13) -0.0020(14) C23 0.0236(16) 0.0373(18) 0.0270(16) 0.0002(14) 0.0038(13) -0.0021(14) C24 0.0230(15) 0.0381(18) 0.0225(15) 0.0000(13) 0.0012(12) 0.0001(13) C25 0.0272(16) 0.0408(19) 0.0232(16) 0.0026(14) 0.0023(13) -0.0037(14) C27 0.0245(15) 0.042(2) 0.0225(15) 0.0005(14) 0.0030(13) 0.0018(14) C28 0.0269(17) 0.0396(19) 0.0279(17) -0.0036(14) 0.0068(14) -0.0043(14) C29 0.0225(15) 0.0409(19) 0.0218(15) 0.0011(13) 0.0038(12) 0.0004(14) O1 0.0333(13) 0.0443(15) 0.0274(13) -0.0049(11) -0.0024(10) -0.0041(11) O2 0.0425(15) 0.0410(15) 0.0225(12) 0.0002(10) 0.0024(11) 0.0015(12) O3 0.0263(12) 0.0399(14) 0.0308(13) -0.0018(11) 0.0020(10) 0.0011(10) O4 0.0310(15) 0.0431(16) 0.0430(17) -0.0100(12) 0.0043(13) 0.0012(11) O5 0.0420(15) 0.0505(16) 0.0257(13) -0.0091(12) -0.0015(11) -0.0040(13) O6 0.0371(14) 0.0474(16) 0.0246(12) 0.0001(11) -0.0010(11) 0.0073(12) O7 0.0256(12) 0.0446(15) 0.0339(13) -0.0027(11) 0.0073(10) 0.0008(11) O8 0.0388(16) 0.0392(15) 0.057(2) -0.0072(14) 0.0051(14) 0.0034(13) O9 0.0322(14) 0.0354(14) 0.0440(15) -0.0004(12) -0.0033(12) -0.0009(11) O10 0.0270(13) 0.0552(18) 0.0437(16) -0.0005(13) 0.0070(11) -0.0015(12) O11 0.0225(12) 0.0443(15) 0.0454(16) 0.0117(12) 0.0027(11) 0.0038(11) O12 0.0317(16) 0.088(3) 0.067(2) 0.044(2) 0.0105(15) 0.0064(16) O13 0.0266(12) 0.0421(14) 0.0319(13) 0.0027(11) 0.0048(10) -0.0011(11) O14 0.0388(16) 0.0405(16) 0.062(2) 0.0088(15) -0.0010(15) -0.0047(13) O15 0.0344(14) 0.0434(15) 0.0243(12) -0.0004(10) 0.0011(10) -0.0024(11) O16 0.0400(15) 0.0470(16) 0.0263(13) 0.0056(11) -0.0006(11) 0.0007(12) O17 0.0290(15) 0.0419(16) 0.0502(18) 0.0092(13) 0.0052(13) -0.0026(11) O18 0.0226(12) 0.0423(14) 0.0332(13) 0.0014(11) 0.0014(10) -0.0021(10) O19 0.0354(14) 0.0413(15) 0.0291(13) 0.0034(11) -0.0017(11) 0.0007(11) O20 0.0365(14) 0.0385(14) 0.0235(12) -0.0013(10) 0.0027(10) -0.0022(11) O1W 0.0333(14) 0.0406(15) 0.0348(14) 0.0067(11) 0.0105(11) 0.0040(11) O2W 0.059(2) 0.0392(16) 0.057(2) -0.0002(14) -0.0111(16) -0.0031(15) O3W 0.111(4) 0.065(2) 0.046(2) -0.0160(17) 0.026(2) -0.026(2) O4W 0.0345(14) 0.0419(15) 0.0308(13) 0.0005(11) 0.0069(11) 0.0007(11) O5W 0.0411(16) 0.0492(17) 0.0411(16) 0.0034(13) 0.0140(13) 0.0027(13) O6W 0.119(4) 0.054(2) 0.0369(18) 0.0093(15) 0.017(2) 0.017(2) O7W 0.078(3) 0.0412(17) 0.0479(19) 0.0035(14) 0.0122(17) 0.0084(17) O8W 0.0448(19) 0.059(2) 0.097(3) -0.019(2) 0.004(2) -0.0126(16) O9W 0.081(3) 0.0509(18) 0.0360(16) -0.0041(14) 0.0173(16) -0.0141(17) O10W 0.0415(16) 0.0461(16) 0.0374(15) 0.0005(12) 0.0141(12) -0.0045(13) O11W 0.150(5) 0.045(2) 0.051(2) 0.0064(16) 0.024(2) 0.012(2) O13W 0.0345(14) 0.0406(15) 0.0373(14) -0.0029(11) 0.0102(11) -0.0016(11) C26 0.0292(18) 0.0369(19) 0.0287(17) -0.0027(14) 0.0031(14) -0.0026(15) O1X 0.074(3) 0.068(3) 0.128(4) -0.032(3) 0.001(3) 0.006(2) O2X 0.073(3) 0.081(3) 0.083(3) -0.005(2) 0.012(2) -0.020(2) O3X 0.070(3) 0.077(3) 0.091(3) 0.008(2) -0.008(2) -0.001(2) O4X 0.075(3) 0.071(3) 0.184(6) -0.052(4) -0.008(4) 0.014(2) O5X 0.124(5) 0.090(4) 0.079(3) 0.001(2) 0.042(3) 0.011(3) O6X 0.238(19) 0.199(16) 0.78(5) 0.04(2) 0.26(2) 0.046(12) O7X 0.109(4) 0.136(5) 0.086(4) -0.006(3) -0.020(3) -0.046(4) O8X 0.104(7) 0.297(16) 0.42(2) -0.262(17) 0.094(10) -0.080(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O11 2.394(3) . ? Pr1 O5 2.419(3) 4_565 ? Pr1 O1 2.449(3) . ? Pr1 O3W 2.518(4) . ? Pr1 O18 2.542(3) 4_465 ? Pr1 O1W 2.552(3) . ? Pr1 O2W 2.574(3) . ? Pr1 O4W 2.589(3) . ? Pr1 O17 2.643(3) 4_465 ? Pr1 C28 2.944(4) 4_465 ? Pr2 O19 2.417(3) . ? Pr2 O16 2.464(3) 4_666 ? Pr2 O8W 2.515(4) . ? Pr2 O3 2.528(3) 4_766 ? Pr2 O6W 2.535(4) . ? Pr2 O9W 2.541(3) . ? Pr2 O7W 2.544(3) . ? Pr2 O5W 2.562(3) . ? Pr2 O4 2.585(3) 4_766 ? Pr2 C8 2.911(4) 4_766 ? Cu1 O6 1.937(3) . ? Cu1 O2 1.953(3) 4_666 ? Cu1 O13 1.975(3) . ? Cu1 O10W 2.033(3) . ? Cu1 O11W 2.226(4) . ? Cu2 O20 1.937(3) 4_565 ? Cu2 O15 1.954(3) . ? Cu2 O7 1.981(3) . ? Cu2 O13W 2.033(3) . ? Cu2 O9 2.242(3) 3_556 ? C1 C6 1.387(5) . ? C1 C2 1.403(5) . ? C1 C7 1.497(5) . ? C2 C3 1.384(5) . ? C2 C8 1.501(5) . ? C3 C4 1.393(5) . ? C4 C5 1.396(5) . ? C4 C9 1.493(5) . ? C5 C6 1.396(5) . ? C5 C10 1.509(5) . ? C7 O1 1.246(5) . ? C7 O2 1.263(5) . ? C8 O4 1.256(5) . ? C8 O3 1.266(5) . ? C8 Pr2 2.911(4) 4_465 ? C9 O5 1.250(5) . ? C9 O6 1.252(5) . ? C10 O8 1.217(5) . ? C10 O7 1.283(5) . ? C11 C12 1.387(5) . ? C11 C13 1.391(5) 3_556 ? C11 C14 1.499(5) . ? C12 C13 1.387(5) . ? C12 C15 1.499(5) . ? C13 C11 1.391(5) 3_556 ? C14 O9 1.266(5) . ? C14 O10 1.266(5) . ? C15 O12 1.254(5) . ? C15 O11 1.271(5) . ? C20 C25 1.394(5) . ? C20 C21 1.400(5) . ? C20 C26 1.503(5) . ? C21 C22 1.398(5) . ? C21 C27 1.494(5) . ? C22 C23 1.387(5) . ? C23 C24 1.403(5) . ? C23 C28 1.513(5) . ? C24 C25 1.379(5) . ? C24 C29 1.503(5) . ? C27 O16 1.253(5) . ? C27 O15 1.259(5) . ? C28 O17 1.238(5) . ? C28 O18 1.273(5) . ? C28 Pr1 2.944(4) 4_766 ? C29 O20 1.253(5) . ? C29 O19 1.254(5) . ? O2 Cu1 1.953(3) 4_565 ? O3 Pr2 2.528(3) 4_465 ? O4 Pr2 2.585(3) 4_465 ? O5 Pr1 2.419(3) 4_666 ? O9 Cu2 2.242(3) 3_556 ? O13 C26 1.269(5) . ? O14 C26 1.235(5) . ? O16 Pr2 2.464(3) 4_565 ? O17 Pr1 2.643(3) 4_766 ? O18 Pr1 2.542(3) 4_766 ? O20 Cu2 1.937(3) 4_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Pr1 O5 140.80(10) . 4_565 ? O11 Pr1 O1 79.57(10) . . ? O5 Pr1 O1 85.36(11) 4_565 . ? O11 Pr1 O3W 99.01(14) . . ? O5 Pr1 O3W 71.45(13) 4_565 . ? O1 Pr1 O3W 141.34(12) . . ? O11 Pr1 O18 134.93(10) . 4_465 ? O5 Pr1 O18 69.38(10) 4_565 4_465 ? O1 Pr1 O18 69.53(9) . 4_465 ? O3W Pr1 O18 125.64(14) . 4_465 ? O11 Pr1 O1W 71.74(10) . . ? O5 Pr1 O1W 140.42(10) 4_565 . ? O1 Pr1 O1W 79.66(9) . . ? O3W Pr1 O1W 137.09(12) . . ? O18 Pr1 O1W 71.07(9) 4_465 . ? O11 Pr1 O2W 71.84(11) . . ? O5 Pr1 O2W 131.27(11) 4_565 . ? O1 Pr1 O2W 143.33(10) . . ? O3W Pr1 O2W 67.37(13) . . ? O18 Pr1 O2W 116.78(11) 4_465 . ? O1W Pr1 O2W 70.00(11) . . ? O11 Pr1 O4W 72.36(9) . . ? O5 Pr1 O4W 68.62(10) 4_565 . ? O1 Pr1 O4W 72.40(9) . . ? O3W Pr1 O4W 70.49(12) . . ? O18 Pr1 O4W 124.43(9) 4_465 . ? O1W Pr1 O4W 137.64(9) . . ? O2W Pr1 O4W 118.04(11) . . ? O11 Pr1 O17 145.27(10) . 4_465 ? O5 Pr1 O17 72.97(11) 4_565 4_465 ? O1 Pr1 O17 119.60(9) . 4_465 ? O3W Pr1 O17 83.28(14) . 4_465 ? O18 Pr1 O17 50.11(9) 4_465 4_465 ? O1W Pr1 O17 83.03(10) . 4_465 ? O2W Pr1 O17 77.37(11) . 4_465 ? O4W Pr1 O17 138.58(10) . 4_465 ? O11 Pr1 C28 150.07(10) . 4_465 ? O5 Pr1 C28 66.60(10) 4_565 4_465 ? O1 Pr1 C28 94.77(10) . 4_465 ? O3W Pr1 C28 103.28(14) . 4_465 ? O18 Pr1 C28 25.50(10) 4_465 4_465 ? O1W Pr1 C28 78.33(10) . 4_465 ? O2W Pr1 C28 98.65(12) . 4_465 ? O4W Pr1 C28 134.20(10) . 4_465 ? O17 Pr1 C28 24.86(10) 4_465 4_465 ? O19 Pr2 O16 84.94(10) . 4_666 ? O19 Pr2 O8W 81.42(13) . . ? O16 Pr2 O8W 139.30(12) 4_666 . ? O19 Pr2 O3 71.69(9) . 4_766 ? O16 Pr2 O3 70.67(9) 4_666 4_766 ? O8W Pr2 O3 137.89(13) . 4_766 ? O19 Pr2 O6W 145.99(12) . . ? O16 Pr2 O6W 73.41(12) 4_666 . ? O8W Pr2 O6W 98.01(16) . . ? O3 Pr2 O6W 122.39(14) 4_766 . ? O19 Pr2 O9W 81.10(11) . . ? O16 Pr2 O9W 137.64(11) 4_666 . ? O8W Pr2 O9W 77.49(14) . . ? O3 Pr2 O9W 66.98(10) 4_766 . ? O6W Pr2 O9W 132.29(13) . . ? O19 Pr2 O7W 138.73(11) . . ? O16 Pr2 O7W 136.04(11) 4_666 . ? O8W Pr2 O7W 69.28(13) . . ? O3 Pr2 O7W 111.99(11) 4_766 . ? O6W Pr2 O7W 69.05(12) . . ? O9W Pr2 O7W 64.99(11) . . ? O19 Pr2 O5W 74.73(10) . . ? O16 Pr2 O5W 69.54(10) 4_666 . ? O8W Pr2 O5W 69.90(12) . . ? O3 Pr2 O5W 129.30(10) 4_766 . ? O6W Pr2 O5W 73.26(13) . . ? O9W Pr2 O5W 141.66(12) . . ? O7W Pr2 O5W 118.35(12) . . ? O19 Pr2 O4 122.64(10) . 4_766 ? O16 Pr2 O4 74.94(10) 4_666 4_766 ? O8W Pr2 O4 143.25(12) . 4_766 ? O3 Pr2 O4 51.02(9) 4_766 4_766 ? O6W Pr2 O4 77.12(14) . 4_766 ? O9W Pr2 O4 79.51(12) . 4_766 ? O7W Pr2 O4 75.14(12) . 4_766 ? O5W Pr2 O4 138.75(11) . 4_766 ? O19 Pr2 C8 97.12(11) . 4_766 ? O16 Pr2 C8 68.43(10) 4_666 4_766 ? O8W Pr2 C8 151.22(12) . 4_766 ? O3 Pr2 C8 25.71(10) 4_766 4_766 ? O6W Pr2 C8 98.79(14) . 4_766 ? O9W Pr2 C8 73.91(11) . 4_766 ? O7W Pr2 C8 95.37(12) . 4_766 ? O5W Pr2 C8 137.72(10) . 4_766 ? O4 Pr2 C8 25.54(10) 4_766 4_766 ? O20 Cu2 O15 171.61(12) 4_565 . ? O20 Cu2 O7 88.22(12) 4_565 . ? O15 Cu2 O7 90.92(12) . . ? O20 Cu2 O13W 89.32(12) 4_565 . ? O15 Cu2 O13W 88.44(12) . . ? O7 Cu2 O13W 158.54(12) . . ? O20 Cu2 O9 89.84(11) 4_565 3_556 ? O15 Cu2 O9 98.07(11) . 3_556 ? O7 Cu2 O9 115.24(11) . 3_556 ? O13W Cu2 O9 86.06(11) . 3_556 ? O6 Cu1 O2 172.25(13) . 4_666 ? O6 Cu1 O13 89.62(12) . . ? O2 Cu1 O13 89.57(12) 4_666 . ? O6 Cu1 O10W 90.22(13) . . ? O2 Cu1 O10W 88.72(13) 4_666 . ? O13 Cu1 O10W 166.10(12) . . ? O6 Cu1 O11W 86.67(14) . . ? O2 Cu1 O11W 101.04(14) 4_666 . ? O13 Cu1 O11W 101.66(16) . . ? O10W Cu1 O11W 92.21(17) . . ? C6 C1 C2 119.7(3) . . ? C6 C1 C7 118.7(3) . . ? C2 C1 C7 121.5(3) . . ? C3 C2 C1 119.8(3) . . ? C3 C2 C8 118.0(3) . . ? C1 C2 C8 121.6(3) . . ? C2 C3 C4 120.4(3) . . ? C3 C4 C5 120.1(3) . . ? C3 C4 C9 118.7(3) . . ? C5 C4 C9 121.0(3) . . ? C6 C5 C4 119.3(3) . . ? C6 C5 C10 119.5(3) . . ? C4 C5 C10 121.2(3) . . ? C1 C6 C5 120.7(3) . . ? O1 C7 O2 124.0(3) . . ? O1 C7 C1 119.6(3) . . ? O2 C7 C1 116.3(3) . . ? O4 C8 O3 121.7(3) . . ? O4 C8 C2 120.4(3) . . ? O3 C8 C2 117.7(3) . . ? O4 C8 Pr2 62.5(2) . 4_465 ? O3 C8 Pr2 59.99(19) . 4_465 ? C2 C8 Pr2 166.2(2) . 4_465 ? O5 C9 O6 124.5(3) . . ? O5 C9 C4 118.9(4) . . ? O6 C9 C4 116.6(3) . . ? O8 C10 O7 126.2(4) . . ? O8 C10 C5 120.5(3) . . ? O7 C10 C5 113.2(3) . . ? C12 C11 C13 119.7(3) . 3_556 ? C12 C11 C14 123.5(3) . . ? C13 C11 C14 116.8(3) 3_556 . ? C13 C12 C11 119.7(3) . . ? C13 C12 C15 118.4(3) . . ? C11 C12 C15 121.8(3) . . ? C12 C13 C11 120.6(3) . 3_556 ? O9 C14 O10 123.5(3) . . ? O9 C14 C11 119.7(3) . . ? O10 C14 C11 116.7(3) . . ? O12 C15 O11 123.6(4) . . ? O12 C15 C12 118.7(3) . . ? O11 C15 C12 117.7(3) . . ? C25 C20 C21 119.6(3) . . ? C25 C20 C26 116.5(3) . . ? C21 C20 C26 123.8(3) . . ? C22 C21 C20 119.2(3) . . ? C22 C21 C27 119.5(3) . . ? C20 C21 C27 121.1(3) . . ? C23 C22 C21 121.0(3) . . ? C22 C23 C24 119.2(3) . . ? C22 C23 C28 119.5(3) . . ? C24 C23 C28 120.8(3) . . ? C25 C24 C23 120.0(3) . . ? C25 C24 C29 117.5(3) . . ? C23 C24 C29 122.3(3) . . ? C24 C25 C20 120.9(3) . . ? O16 C27 O15 124.1(3) . . ? O16 C27 C21 119.2(3) . . ? O15 C27 C21 116.7(3) . . ? O17 C28 O18 122.2(3) . . ? O17 C28 C23 121.7(3) . . ? O18 C28 C23 115.9(3) . . ? O17 C28 Pr1 63.8(2) . 4_766 ? O18 C28 Pr1 59.30(18) . 4_766 ? C23 C28 Pr1 164.8(3) . 4_766 ? O20 C29 O19 125.5(3) . . ? O20 C29 C24 115.9(3) . . ? O19 C29 C24 118.6(3) . . ? C7 O1 Pr1 170.4(3) . . ? C7 O2 Cu1 111.3(2) . 4_565 ? C8 O3 Pr2 94.3(2) . 4_465 ? C8 O4 Pr2 91.9(2) . 4_465 ? C9 O5 Pr1 163.6(3) . 4_666 ? C9 O6 Cu1 115.7(2) . . ? C10 O7 Cu2 125.2(2) . . ? C14 O9 Cu2 128.2(2) . 3_556 ? C15 O11 Pr1 142.2(3) . . ? C26 O13 Cu1 124.6(2) . . ? C27 O15 Cu2 110.9(2) . . ? C27 O16 Pr2 166.6(3) . 4_565 ? C28 O17 Pr1 91.3(2) . 4_766 ? C28 O18 Pr1 95.2(2) . 4_766 ? C29 O19 Pr2 163.5(3) . . ? C29 O20 Cu2 115.9(2) . 4_666 ? O14 C26 O13 125.3(4) . . ? O14 C26 C20 119.5(3) . . ? O13 C26 C20 115.0(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 4.775 _refine_diff_density_min -1.225 _refine_diff_density_rms 0.147