# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email iplakatu@cc.uoi.gr _publ_contact_author_name 'John C. Plakatouras' _publ_author_name G.Kostakis data_1 _database_code_depnum_ccdc_archive 'CCDC 835270' #TrackingRef 'Konidaris.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C21 H36 Cu3 La2 N6 O27), 11(H2 O)' _chemical_formula_sum 'C42 H94 Cu6 La4 N12 O65' _chemical_formula_weight 2744.17 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' 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.291(2) _cell_length_b 13.235(3) _cell_length_c 15.436(3) _cell_angle_alpha 73.80(3) _cell_angle_beta 72.74(3) _cell_angle_gamma 79.37(3) _cell_volume 2102.3(7) _cell_formula_units_Z 1 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 35412 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description purple _exptl_crystal_colour plate _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 3.595 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5065 _exptl_absorpt_correction_T_max 0.6997 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The crystal under investigation was refined as a twin with a twin matrix [0.375 -0.420 0.625 0 -1 0 1.375 -0.420 -0.375] (PLATON, Spek, 2003) and BASF refined to 0.16136. The water molecules O13 and O14 were disordered over two sites with occupancy ratio of 0.51/0.49 and 0.83/0.17 respectively. O13A and O13B as well as O14A and O14B were refined with equal anisotropic displacement parameters. The water molecule O15 was partially lost and refined with occupancy of 0.5. The H~2~O hydrogen atoms were either located from the difference Fourier map or by using HYDROGEN program (Nardelli, 1999) and constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogens were positioned geometrically and were also constrained to ride on their parent atoms, with C---H =0.99 \%A, and U~iso~ = 1.2 U~eq~(parent atom). The highest peak is located 1.32 \%A from atom La1 and the deepest hole is located 0.95 \%A from atom La2. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_reflns_number 7436 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7436 _reflns_number_gt 6485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1b (Crystal Impact GbR, 2006)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+45.7688P] 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 7436 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.19297(5) 0.23685(4) 0.94324(4) 0.01227(15) Uani 1 1 d . . . O1W O 0.3212(7) 0.0849(6) 0.8736(5) 0.0230(16) Uani 1 1 d . . . H11W H 0.3457 0.1055 0.8153 0.035 Uiso 1 1 d R . . H21W H 0.3821 0.0396 0.8940 0.035 Uiso 1 1 d R . . O2W O -0.0201(7) 0.2567(8) 1.0591(5) 0.035(2) Uani 1 1 d . . . H12W H -0.0164 0.2648 1.1136 0.053 Uiso 1 1 d R . . H22W H -0.0947 0.2657 1.0594 0.053 Uiso 1 1 d R . . O3W O 0.2520(7) 0.2968(6) 0.7647(5) 0.0230(16) Uani 1 1 d . . . H13W H 0.2339 0.2765 0.7243 0.035 Uiso 1 1 d R . . H23W H 0.3241 0.3120 0.7441 0.035 Uiso 1 1 d R . . O4W O 0.1330(8) 0.4350(6) 0.8938(5) 0.0288(18) Uani 1 1 d . . . H14W H 0.1243 0.4781 0.9301 0.043 Uiso 1 1 d R . . H24W H 0.1271 0.4735 0.8421 0.043 Uiso 1 1 d R . . La2 La 0.49511(5) 0.26024(4) 1.38100(4) 0.01376(16) Uani 1 1 d . . . O5W O 0.3050(10) 0.3926(8) 1.4216(8) 0.052(3) Uani 1 1 d . . . H15W H 0.2380 0.4344 1.3954 0.077 Uiso 1 1 d R . . H25W H 0.2758 0.3756 1.4833 0.077 Uiso 1 1 d R . . O6W O 0.7043(7) 0.2811(6) 1.2529(5) 0.0249(17) Uani 1 1 d . . . H16W H 0.6990 0.3411 1.2102 0.037 Uiso 1 1 d R . . H26W H 0.7857 0.2591 1.2557 0.037 Uiso 1 1 d R . . O7W O 0.5603(10) 0.4120(6) 1.4207(8) 0.049(3) Uani 1 1 d . . . H17W H 0.5723 0.3950 1.4772 0.074 Uiso 1 1 d R . . H27W H 0.6302 0.4349 1.3871 0.074 Uiso 1 1 d R . . O8W O 0.4162(7) 0.1980(7) 1.5556(5) 0.0290(18) Uani 1 1 d . . . H18W H 0.3473 0.1690 1.5647 0.044 Uiso 1 1 d R . . H28W H 0.4486 0.1637 1.6075 0.044 Uiso 1 1 d R . . O9W O 0.5605(7) 0.0930(6) 1.3217(5) 0.0246(17) Uani 1 1 d . . . H19W H 0.5030 0.0669 1.3086 0.037 Uiso 1 1 d R . . H29W H 0.6201 0.1091 1.2701 0.037 Uiso 1 1 d R . . Cu1 Cu -0.23967(11) 0.21559(9) 0.76669(8) 0.0137(3) Uani 1 1 d . . . O1A O -0.1546(7) 0.5074(6) 0.7013(6) 0.0252(17) Uani 1 1 d . . . O2A O -0.2419(7) 0.3649(6) 0.7107(5) 0.0211(16) Uani 1 1 d . . . O3A O 0.0369(7) 0.1785(6) 0.8965(5) 0.0206(16) Uani 1 1 d . . . O4A O -0.2110(7) -0.0862(5) 0.9255(5) 0.0188(15) Uani 1 1 d . . . O5A O -0.3646(7) 0.1996(6) 0.7088(5) 0.0194(15) Uani 1 1 d . . . O6A O -0.4787(6) 0.0822(6) 0.7030(5) 0.0163(14) Uani 1 1 d . . . N1A N -0.1162(8) 0.2346(6) 0.8207(6) 0.0150(17) Uani 1 1 d . . . N2A N -0.2487(8) 0.0691(6) 0.8246(6) 0.0146(17) Uani 1 1 d . . . C1A C -0.1651(9) 0.4122(8) 0.7303(7) 0.018(2) Uani 1 1 d . . . C2A C -0.0847(10) 0.3422(8) 0.7919(8) 0.022(2) Uani 1 1 d . . . H2A1 H 0.0043 0.3434 0.7572 0.026 Uiso 1 1 calc R . . H2A2 H -0.0976 0.3698 0.8478 0.026 Uiso 1 1 calc R . . C3A C -0.0521(9) 0.1609(8) 0.8707(6) 0.014(2) Uani 1 1 d . . . C4A C -0.0833(9) 0.0477(8) 0.9021(7) 0.015(2) Uani 1 1 d . . . H4A1 H -0.0973 0.0279 0.9709 0.018 Uiso 1 1 calc R . . H4A2 H -0.0060 0.0043 0.8769 0.018 Uiso 1 1 calc R . . C5A C -0.1888(9) 0.0079(8) 0.8827(7) 0.017(2) Uani 1 1 d . . . C6A C -0.3501(10) 0.0252(8) 0.8079(7) 0.020(2) Uani 1 1 d . . . H6A1 H -0.4172 0.0088 0.8663 0.024 Uiso 1 1 calc R . . H6A2 H -0.3169 -0.0409 0.7865 0.024 Uiso 1 1 calc R . . C7A C -0.4008(9) 0.1075(8) 0.7337(7) 0.017(2) Uani 1 1 d . . . Cu2 Cu 0.34088(11) 0.58899(9) 1.03306(8) 0.0137(3) Uani 1 1 d . . . O1B O 0.2777(7) 0.7116(6) 0.9481(5) 0.0192(15) Uani 1 1 d . . . O2B O 0.2706(7) 0.8871(5) 0.9042(5) 0.0203(16) Uani 1 1 d . . . O3B O 0.5902(7) 0.7294(6) 1.0931(5) 0.0222(16) Uani 1 1 d . . . O4B O 0.4740(8) 0.3856(6) 1.2410(6) 0.033(2) Uani 1 1 d . . . O5B O 0.2434(7) 0.4924(6) 1.0151(5) 0.0219(16) Uani 1 1 d . . . O6B O 0.2029(8) 0.3232(6) 1.0654(5) 0.0251(17) Uani 1 1 d . . . N1B N 0.4311(8) 0.6858(6) 1.0522(6) 0.0163(17) Uani 1 1 d . . . N2B N 0.3945(8) 0.4703(6) 1.1200(6) 0.0173(18) Uani 1 1 d . . . C1B C 0.3132(9) 0.7986(8) 0.9463(6) 0.015(2) Uani 1 1 d . . . C2B C 0.4157(10) 0.7935(8) 0.9923(7) 0.016(2) Uani 1 1 d . . . H2B1 H 0.4947 0.8093 0.9442 0.020 Uiso 1 1 calc R . . H2B2 H 0.3934 0.8464 1.0305 0.020 Uiso 1 1 calc R . . C3B C 0.5173(9) 0.6649(7) 1.0991(6) 0.0125(19) Uani 1 1 d . . . C4B C 0.5287(9) 0.5581(8) 1.1687(7) 0.018(2) Uani 1 1 d . . . H4B1 H 0.6186 0.5315 1.1557 0.022 Uiso 1 1 calc R . . H4B2 H 0.5051 0.5730 1.2314 0.022 Uiso 1 1 calc R . . C5B C 0.4604(10) 0.4673(8) 1.1771(7) 0.018(2) Uani 1 1 d . . . C6B C 0.3286(10) 0.3793(7) 1.1371(7) 0.016(2) Uani 1 1 d . . . H6B1 H 0.2733 0.3662 1.2013 0.019 Uiso 1 1 calc R . . H6B2 H 0.3894 0.3157 1.1314 0.019 Uiso 1 1 calc R . . C7B C 0.2527(10) 0.3986(8) 1.0683(7) 0.017(2) Uani 1 1 d . . . Cu3 Cu 0.08550(11) -0.03322(10) 1.39672(8) 0.0166(3) Uani 1 1 d . . . O1C O -0.0102(7) 0.0656(6) 1.3145(5) 0.0204(15) Uani 1 1 d . . . O2C O -0.0455(7) 0.2369(6) 1.2481(5) 0.0215(16) Uani 1 1 d . . . O3C O 0.3124(7) 0.1758(6) 1.3935(5) 0.0212(16) Uani 1 1 d . . . O4C O 0.3270(7) -0.1815(6) 1.5553(5) 0.0200(15) Uani 1 1 d . . . O5C O 0.0132(7) -0.1566(6) 1.4011(5) 0.0262(17) Uani 1 1 d . . . O6C O 0.0106(9) -0.3284(7) 1.4678(6) 0.041(2) Uani 1 1 d . . . N1C N 0.1627(8) 0.0880(7) 1.3837(6) 0.0187(18) Uani 1 1 d . . . N2C N 0.1761(8) -0.1288(7) 1.4782(6) 0.0169(18) Uani 1 1 d . . . C1C C 0.0143(9) 0.1602(9) 1.2917(7) 0.020(2) Uani 1 1 d . . . C2C C 0.1264(10) 0.1818(8) 1.3173(7) 0.020(2) Uani 1 1 d . . . H2C1 H 0.1964 0.1973 1.2607 0.024 Uiso 1 1 calc R . . H2C2 H 0.1039 0.2437 1.3454 0.024 Uiso 1 1 calc R . . C3C C 0.2553(9) 0.0937(8) 1.4179(7) 0.016(2) Uani 1 1 d . . . C4C C 0.2948(9) 0.0024(8) 1.4922(7) 0.016(2) Uani 1 1 d . . . H4C1 H 0.3866 -0.0012 1.4791 0.019 Uiso 1 1 calc R . . H4C2 H 0.2591 0.0229 1.5525 0.019 Uiso 1 1 calc R . . C5C C 0.2653(9) -0.1092(8) 1.5082(6) 0.0135(19) Uani 1 1 d . . . C6C C 0.1529(10) -0.2389(9) 1.4984(7) 0.022(2) Uani 1 1 d . . . H6C1 H 0.1268 -0.2679 1.5668 0.026 Uiso 1 1 calc R . . H6C2 H 0.2302 -0.2818 1.4726 0.026 Uiso 1 1 calc R . . C7C C 0.0507(10) -0.2446(9) 1.4546(7) 0.025(2) Uani 1 1 d . . . O10W O 0.1781(7) 0.1894(8) 0.6639(6) 0.040(2) Uani 1 1 d . . . H110 H 0.1515 0.2051 0.6171 0.060 Uiso 1 1 d R . . H210 H 0.1214 0.1757 0.7132 0.060 Uiso 1 1 d R . . O11W O 0.8038(7) 0.0238(6) 1.2547(5) 0.0261(17) Uani 1 1 d . . . H111 H 0.8540 0.0515 1.2707 0.039 Uiso 1 1 d R . . H211 H 0.8067 0.0443 1.1973 0.039 Uiso 1 1 d R . . O12W O 0.1357(17) 0.4788(12) 1.5533(12) 0.133(8) Uani 1 1 d . . . H112 H 0.0655 0.4513 1.5789 0.200 Uiso 1 1 d R . . H212 H 0.1201 0.5415 1.5209 0.200 Uiso 1 1 d R . . O13A O 0.4081(15) 0.5968(12) 1.4053(11) 0.026(2) Uani 0.488(13) 1 d P A 1 H13A H 0.3508 0.5607 1.4373 0.039 Uiso 0.488(13) 1 d PR A 1 H13B H 0.3825 0.6431 1.3649 0.039 Uiso 0.488(13) 1 d PR A 1 O13B O 0.5191(14) 0.6326(12) 1.3673(10) 0.026(2) Uani 0.512(13) 1 d P A 2 H13C H 0.5265 0.6751 1.3976 0.039 Uiso 0.512(13) 1 d PR A 2 H13D H 0.5080 0.6694 1.3147 0.039 Uiso 0.512(13) 1 d PR A 2 O14A O 0.0317(13) 0.5591(8) 0.7560(9) 0.052(4) Uani 0.825(17) 1 d P B 3 H14A H -0.0241 0.5548 0.7299 0.078 Uiso 0.825(17) 1 d PR B 3 H14B H -0.0053 0.5880 0.8011 0.078 Uiso 0.825(17) 1 d PR B 3 O14B O 0.151(6) 0.549(4) 0.704(5) 0.052(4) Uani 0.175(17) 1 d P . 4 H14C H 0.1802 0.5964 0.6594 0.078 Uiso 0.175(17) 1 d PR B 4 H14D H 0.1154 0.5003 0.7012 0.078 Uiso 0.175(17) 1 d PR B 4 O15W O 0.7626(17) 0.4987(13) 1.3460(12) 0.036(4) Uani 0.50 1 d P . . H15A H 0.7555 0.5340 1.2944 0.053 Uiso 0.50 1 d PR . . H25B H 0.7328 0.5363 1.3866 0.053 Uiso 0.50 1 d PR . . 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 0.0145(3) 0.0105(3) 0.0149(3) 0.0000(2) -0.0096(2) -0.0041(2) O1W 0.024(4) 0.017(4) 0.027(4) -0.006(3) -0.002(3) -0.007(3) O2W 0.019(4) 0.074(7) 0.019(4) -0.020(4) -0.009(3) -0.001(4) O3W 0.030(4) 0.023(4) 0.019(4) -0.002(3) -0.008(3) -0.010(3) O4W 0.051(5) 0.014(4) 0.026(4) -0.004(3) -0.022(4) 0.003(3) La2 0.0176(3) 0.0112(3) 0.0158(3) -0.0006(2) -0.0109(2) -0.0029(2) O5W 0.057(6) 0.042(6) 0.075(7) -0.037(5) -0.048(6) 0.031(5) O6W 0.019(4) 0.037(5) 0.017(4) 0.003(3) -0.007(3) -0.012(3) O7W 0.079(7) 0.017(4) 0.079(7) -0.006(4) -0.069(6) -0.001(4) O8W 0.017(4) 0.050(5) 0.015(4) 0.001(3) -0.006(3) -0.004(4) O9W 0.016(4) 0.029(4) 0.032(4) -0.017(3) 0.001(3) -0.006(3) Cu1 0.0162(6) 0.0123(6) 0.0148(6) -0.0008(5) -0.0076(5) -0.0046(5) O1A 0.026(4) 0.014(4) 0.038(5) -0.005(3) -0.013(4) -0.004(3) O2A 0.019(4) 0.022(4) 0.024(4) -0.002(3) -0.010(3) -0.004(3) O3A 0.023(4) 0.026(4) 0.021(4) -0.003(3) -0.015(3) -0.011(3) O4A 0.023(4) 0.014(4) 0.020(4) 0.006(3) -0.011(3) -0.009(3) O5A 0.018(4) 0.019(4) 0.024(4) -0.003(3) -0.009(3) -0.003(3) O6A 0.012(3) 0.025(4) 0.016(3) -0.009(3) -0.007(3) -0.001(3) N1A 0.015(4) 0.012(4) 0.017(4) -0.001(3) -0.005(3) -0.003(3) N2A 0.017(4) 0.011(4) 0.018(4) -0.002(3) -0.007(3) -0.006(3) C1A 0.015(5) 0.016(5) 0.023(5) -0.007(4) -0.003(4) -0.001(4) C2A 0.020(5) 0.023(6) 0.026(6) -0.006(5) -0.008(4) -0.009(4) C3A 0.014(5) 0.020(5) 0.010(4) -0.001(4) -0.003(4) -0.008(4) C4A 0.016(5) 0.015(5) 0.016(5) -0.003(4) -0.009(4) -0.001(4) C5A 0.015(5) 0.025(6) 0.019(5) -0.011(4) -0.010(4) -0.001(4) C6A 0.018(5) 0.024(6) 0.026(6) -0.009(4) -0.010(4) -0.006(4) C7A 0.017(5) 0.020(5) 0.017(5) -0.008(4) -0.005(4) -0.005(4) Cu2 0.0198(6) 0.0119(6) 0.0129(6) 0.0006(4) -0.0101(5) -0.0059(5) O1B 0.024(4) 0.018(4) 0.020(4) -0.003(3) -0.012(3) -0.007(3) O2B 0.026(4) 0.008(3) 0.030(4) -0.006(3) -0.009(3) -0.003(3) O3B 0.019(4) 0.020(4) 0.030(4) 0.004(3) -0.015(3) -0.010(3) O4B 0.037(5) 0.030(5) 0.036(5) 0.012(4) -0.029(4) -0.011(4) O5B 0.030(4) 0.015(4) 0.024(4) 0.002(3) -0.017(3) -0.007(3) O6B 0.040(5) 0.022(4) 0.020(4) -0.007(3) -0.010(3) -0.013(3) N1B 0.020(4) 0.012(4) 0.018(4) 0.000(3) -0.008(4) -0.004(3) N2B 0.019(4) 0.013(4) 0.022(4) -0.001(3) -0.010(4) -0.005(3) C1B 0.019(5) 0.021(5) 0.004(4) -0.005(4) 0.001(4) 0.000(4) C2B 0.026(6) 0.012(5) 0.013(5) -0.002(4) -0.009(4) -0.004(4) C3B 0.013(5) 0.013(5) 0.010(4) 0.001(4) 0.000(4) -0.007(4) C4B 0.015(5) 0.023(5) 0.015(5) 0.001(4) -0.007(4) -0.001(4) C5B 0.018(5) 0.013(5) 0.019(5) 0.002(4) -0.006(4) -0.003(4) C6B 0.021(5) 0.011(5) 0.019(5) 0.000(4) -0.010(4) -0.008(4) C7B 0.026(6) 0.016(5) 0.008(4) -0.002(4) -0.002(4) -0.006(4) Cu3 0.0133(6) 0.0224(7) 0.0177(6) -0.0032(5) -0.0089(5) -0.0050(5) O1C 0.020(4) 0.022(4) 0.023(4) -0.002(3) -0.012(3) -0.004(3) O2C 0.016(4) 0.030(4) 0.020(4) -0.002(3) -0.014(3) 0.004(3) O3C 0.017(4) 0.020(4) 0.029(4) -0.001(3) -0.013(3) -0.006(3) O4C 0.017(4) 0.020(4) 0.025(4) -0.001(3) -0.015(3) 0.001(3) O5C 0.027(4) 0.037(5) 0.021(4) -0.004(3) -0.011(3) -0.015(4) O6C 0.055(6) 0.037(5) 0.041(5) -0.010(4) -0.017(4) -0.026(5) N1C 0.016(4) 0.023(5) 0.018(4) 0.002(4) -0.010(4) -0.005(4) N2C 0.021(5) 0.016(4) 0.017(4) -0.002(3) -0.009(4) -0.005(3) C1C 0.011(5) 0.034(6) 0.014(5) -0.011(4) -0.004(4) 0.005(4) C2C 0.018(5) 0.020(5) 0.025(6) -0.002(4) -0.016(4) 0.003(4) C3C 0.012(5) 0.020(5) 0.017(5) -0.004(4) -0.004(4) -0.001(4) C4C 0.014(5) 0.017(5) 0.018(5) -0.001(4) -0.010(4) -0.001(4) C5C 0.011(5) 0.020(5) 0.011(4) -0.005(4) -0.002(4) -0.003(4) C6C 0.023(6) 0.024(6) 0.018(5) 0.002(4) -0.005(4) -0.011(4) C7C 0.024(6) 0.037(7) 0.017(5) 0.000(5) -0.005(4) -0.017(5) O10W 0.019(4) 0.080(7) 0.034(5) -0.036(5) -0.005(4) -0.009(4) O11W 0.021(4) 0.038(5) 0.026(4) -0.015(4) -0.009(3) -0.004(3) O12W 0.134(15) 0.067(10) 0.117(13) -0.010(9) 0.067(12) 0.005(10) O13A 0.032(6) 0.024(6) 0.021(5) 0.002(4) -0.013(5) -0.001(5) O13B 0.032(6) 0.024(6) 0.021(5) 0.002(4) -0.013(5) -0.001(5) O14A 0.072(9) 0.025(5) 0.077(9) 0.020(5) -0.065(8) -0.021(6) O14B 0.072(9) 0.025(5) 0.077(9) 0.020(5) -0.065(8) -0.021(6) O15W 0.039(10) 0.024(9) 0.038(10) -0.005(7) -0.005(8) -0.002(8) _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 O3A 2.406(7) . yes La1 O3B 2.440(7) 2_667 yes La1 O4A 2.442(7) 2_557 yes La1 O6B 2.501(7) . yes La1 O4W 2.541(7) . yes La1 O1W 2.551(7) . yes La1 O2W 2.555(8) . yes La1 O3W 2.559(7) . yes O1W H11W 0.8392 . ? O1W H21W 0.8964 . ? O2W H12W 0.8915 . ? O2W H22W 0.8269 . ? O3W H13W 0.8333 . ? O3W H23W 0.8217 . ? O4W H14W 0.8798 . ? O4W H24W 0.8323 . ? La2 O4B 2.374(8) . yes La2 O4C 2.433(7) 2_658 yes La2 O3C 2.456(7) . yes La2 O8W 2.519(7) . yes La2 O9W 2.531(7) . yes La2 O7W 2.540(8) . yes La2 O5W 2.549(9) . yes La2 O6W 2.594(7) . yes O5W H15W 0.9709 . ? O5W H25W 0.8867 . ? O6W H16W 0.8840 . ? O6W H26W 0.9221 . ? O7W H17W 0.8827 . ? O7W H27W 0.8611 . ? O8W H18W 0.8872 . ? O8W H28W 0.9442 . ? O9W H19W 0.8841 . ? O9W H29W 0.8796 . ? Cu1 N2A 1.902(8) . ? Cu1 N1A 1.907(8) . ? Cu1 O2A 1.922(7) . ? Cu1 O5A 1.948(7) . ? O1A C1A 1.230(12) . ? O2A C1A 1.303(12) . ? O3A C3A 1.265(12) . ? O4A C5A 1.269(13) . ? O4A La1 2.442(7) 2_557 ? O5A C7A 1.277(12) . ? O6A C7A 1.247(12) . ? N1A C3A 1.312(13) . ? N1A C2A 1.446(13) . ? N2A C5A 1.292(13) . ? N2A C6A 1.491(12) . ? C1A C2A 1.515(15) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3A C4A 1.513(13) . ? C4A C5A 1.522(13) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C6A C7A 1.513(15) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? Cu2 N2B 1.895(8) . ? Cu2 N1B 1.907(8) . ? Cu2 O1B 1.950(7) . ? Cu2 O5B 1.955(7) . ? O1B C1B 1.276(12) . ? O2B C1B 1.257(12) . ? O3B C3B 1.259(12) . ? O3B La1 2.440(7) 2_667 ? O4B C5B 1.265(13) . ? O5B C7B 1.289(12) . ? O6B C7B 1.249(13) . ? N1B C3B 1.325(13) . ? N1B C2B 1.478(12) . ? N2B C5B 1.300(13) . ? N2B C6B 1.453(12) . ? C1B C2B 1.510(14) . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C3B C4B 1.528(13) . ? C4B C5B 1.501(14) . ? C4B H4B1 0.9900 . ? C4B H4B2 0.9900 . ? C6B C7B 1.494(14) . ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? Cu3 N1C 1.898(9) . ? Cu3 N2C 1.905(8) . ? Cu3 O5C 1.932(8) . ? Cu3 O1C 1.963(7) . ? O1C C1C 1.262(13) . ? O2C C1C 1.254(13) . ? O3C C3C 1.276(12) . ? O4C C5C 1.264(12) . ? O4C La2 2.433(7) 2_658 ? O5C C7C 1.307(14) . ? O6C C7C 1.217(14) . ? N1C C3C 1.325(13) . ? N1C C2C 1.454(13) . ? N2C C5C 1.317(13) . ? N2C C6C 1.459(13) . ? C1C C2C 1.528(14) . ? C2C H2C1 0.9900 . ? C2C H2C2 0.9900 . ? C3C C4C 1.519(13) . ? C4C C5C 1.510(14) . ? C4C H4C1 0.9900 . ? C4C H4C2 0.9900 . ? C6C C7C 1.522(15) . ? C6C H6C1 0.9900 . ? C6C H6C2 0.9900 . ? O10W H110 0.8226 . ? O10W H210 0.8360 . ? O11W H111 0.8531 . ? O11W H211 0.8440 . ? O12W H112 0.8698 . ? O12W H212 0.8586 . ? O13A H13A 0.8264 . ? O13A H13B 0.8221 . ? O13B H13C 0.8539 . ? O13B H13D 0.8550 . ? O14A H14A 0.8605 . ? O14A H14B 0.8493 . ? O14A H14D 1.3549 . ? O14B O15W 1.25(7) 2_667 ? O14B H14C 0.8248 . ? O14B H14D 0.8375 . ? O15W O14B 1.25(7) 2_667 ? O15W H15A 0.8221 . ? O15W H25B 0.8603 . ? 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 O3A La1 O3B 147.4(3) . 2_667 ? O3A La1 O4A 97.8(2) . 2_557 ? O3B La1 O4A 93.9(2) 2_667 2_557 ? O3A La1 O6B 138.1(3) . . ? O3B La1 O6B 74.2(3) 2_667 . ? O4A La1 O6B 77.3(2) 2_557 . ? O3A La1 O4W 98.1(3) . . ? O3B La1 O4W 88.9(3) 2_667 . ? O4A La1 O4W 145.5(2) 2_557 . ? O6B La1 O4W 70.4(2) . . ? O3A La1 O1W 79.5(3) . . ? O3B La1 O1W 74.9(2) 2_667 . ? O4A La1 O1W 73.3(2) 2_557 . ? O6B La1 O1W 135.2(3) . . ? O4W La1 O1W 139.9(3) . . ? O3A La1 O2W 69.6(3) . . ? O3B La1 O2W 142.9(3) 2_667 . ? O4A La1 O2W 77.8(3) 2_557 . ? O6B La1 O2W 68.7(3) . . ? O4W La1 O2W 79.4(3) . . ? O1W La1 O2W 133.9(3) . . ? O3A La1 O3W 75.1(2) . . ? O3B La1 O3W 77.4(2) 2_667 . ? O4A La1 O3W 143.6(2) 2_557 . ? O6B La1 O3W 131.5(2) . . ? O4W La1 O3W 70.5(2) . . ? O1W La1 O3W 70.2(2) . . ? O2W La1 O3W 129.1(2) . . ? La1 O1W H11W 110.1 . . ? La1 O1W H21W 126.7 . . ? H11W O1W H21W 108.3 . . ? La1 O2W H12W 113.9 . . ? La1 O2W H22W 138.5 . . ? H12W O2W H22W 107.0 . . ? La1 O3W H13W 131.7 . . ? La1 O3W H23W 111.5 . . ? H13W O3W H23W 108.1 . . ? La1 O4W H14W 122.9 . . ? La1 O4W H24W 130.7 . . ? H14W O4W H24W 105.9 . . ? O4B La2 O4C 133.1(3) . 2_658 ? O4B La2 O3C 92.8(3) . . ? O4C La2 O3C 127.7(2) 2_658 . ? O4B La2 O8W 148.3(3) . . ? O4C La2 O8W 71.7(2) 2_658 . ? O3C La2 O8W 78.9(3) . . ? O4B La2 O9W 100.0(3) . . ? O4C La2 O9W 78.2(2) 2_658 . ? O3C La2 O9W 69.0(2) . . ? O8W La2 O9W 105.2(3) . . ? O4B La2 O7W 85.0(3) . . ? O4C La2 O7W 75.5(3) 2_658 . ? O3C La2 O7W 142.9(3) . . ? O8W La2 O7W 83.8(3) . . ? O9W La2 O7W 147.9(3) . . ? O4B La2 O5W 71.7(3) . . ? O4C La2 O5W 135.4(3) 2_658 . ? O3C La2 O5W 73.7(3) . . ? O8W La2 O5W 76.6(3) . . ? O9W La2 O5W 141.3(3) . . ? O7W La2 O5W 70.5(3) . . ? O4B La2 O6W 66.8(3) . . ? O4C La2 O6W 68.4(2) 2_658 . ? O3C La2 O6W 131.0(2) . . ? O8W La2 O6W 139.8(2) . . ? O9W La2 O6W 71.4(2) . . ? O7W La2 O6W 81.9(3) . . ? O5W La2 O6W 131.6(3) . . ? La2 O5W H15W 139.8 . . ? La2 O5W H25W 106.8 . . ? H15W O5W H25W 107.8 . . ? La2 O6W H16W 110.6 . . ? La2 O6W H26W 131.4 . . ? H16W O6W H26W 111.2 . . ? La2 O7W H17W 112.8 . . ? La2 O7W H27W 117.1 . . ? H17W O7W H27W 101.3 . . ? La2 O8W H18W 105.3 . . ? La2 O8W H28W 138.5 . . ? H18W O8W H28W 106.1 . . ? La2 O9W H19W 117.5 . . ? La2 O9W H29W 105.3 . . ? H19W O9W H29W 108.0 . . ? N2A Cu1 N1A 96.8(3) . . ? N2A Cu1 O2A 176.4(3) . . ? N1A Cu1 O2A 85.6(3) . . ? N2A Cu1 O5A 84.7(3) . . ? N1A Cu1 O5A 178.4(3) . . ? O2A Cu1 O5A 93.0(3) . . ? C1A O2A Cu1 115.0(6) . . ? C3A O3A La1 172.1(7) . . ? C5A O4A La1 148.2(6) . 2_557 ? C7A O5A Cu1 115.1(6) . . ? C3A N1A C2A 119.5(8) . . ? C3A N1A Cu1 127.3(7) . . ? C2A N1A Cu1 112.8(6) . . ? C5A N2A C6A 117.2(8) . . ? C5A N2A Cu1 128.8(7) . . ? C6A N2A Cu1 113.5(6) . . ? O1A C1A O2A 124.0(10) . . ? O1A C1A C2A 120.0(9) . . ? O2A C1A C2A 116.0(9) . . ? N1A C2A C1A 110.5(8) . . ? N1A C2A H2A1 109.5 . . ? C1A C2A H2A1 109.5 . . ? N1A C2A H2A2 109.5 . . ? C1A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 108.1 . . ? O3A C3A N1A 123.4(9) . . ? O3A C3A C4A 115.9(9) . . ? N1A C3A C4A 120.7(8) . . ? C3A C4A C5A 125.5(8) . . ? C3A C4A H4A1 105.9 . . ? C5A C4A H4A1 105.9 . . ? C3A C4A H4A2 105.9 . . ? C5A C4A H4A2 105.9 . . ? H4A1 C4A H4A2 106.3 . . ? O4A C5A N2A 124.1(9) . . ? O4A C5A C4A 116.1(8) . . ? N2A C5A C4A 119.8(9) . . ? N2A C6A C7A 107.8(8) . . ? N2A C6A H6A1 110.1 . . ? C7A C6A H6A1 110.1 . . ? N2A C6A H6A2 110.1 . . ? C7A C6A H6A2 110.1 . . ? H6A1 C6A H6A2 108.5 . . ? O6A C7A O5A 124.0(9) . . ? O6A C7A C6A 117.9(9) . . ? O5A C7A C6A 118.0(8) . . ? N2B Cu2 N1B 95.4(3) . . ? N2B Cu2 O1B 177.2(3) . . ? N1B Cu2 O1B 85.3(3) . . ? N2B Cu2 O5B 85.3(3) . . ? N1B Cu2 O5B 178.1(4) . . ? O1B Cu2 O5B 93.9(3) . . ? C1B O1B Cu2 113.8(6) . . ? C3B O3B La1 146.2(7) . 2_667 ? C5B O4B La2 167.2(8) . . ? C7B O5B Cu2 113.3(6) . . ? C7B O6B La1 136.9(7) . . ? C3B N1B C2B 117.8(8) . . ? C3B N1B Cu2 128.4(7) . . ? C2B N1B Cu2 112.8(6) . . ? C5B N2B C6B 117.4(8) . . ? C5B N2B Cu2 128.4(7) . . ? C6B N2B Cu2 112.6(6) . . ? O2B C1B O1B 122.8(9) . . ? O2B C1B C2B 119.0(9) . . ? O1B C1B C2B 118.1(9) . . ? N1B C2B C1B 108.3(8) . . ? N1B C2B H2B1 110.0 . . ? C1B C2B H2B1 110.0 . . ? N1B C2B H2B2 110.0 . . ? C1B C2B H2B2 110.0 . . ? H2B1 C2B H2B2 108.4 . . ? O3B C3B N1B 124.3(9) . . ? O3B C3B C4B 116.0(8) . . ? N1B C3B C4B 119.7(8) . . ? C5B C4B C3B 123.3(8) . . ? C5B C4B H4B1 106.5 . . ? C3B C4B H4B1 106.5 . . ? C5B C4B H4B2 106.5 . . ? C3B C4B H4B2 106.5 . . ? H4B1 C4B H4B2 106.5 . . ? O4B C5B N2B 121.5(9) . . ? O4B C5B C4B 116.2(9) . . ? N2B C5B C4B 122.2(9) . . ? N2B C6B C7B 110.2(8) . . ? N2B C6B H6B1 109.6 . . ? C7B C6B H6B1 109.6 . . ? N2B C6B H6B2 109.6 . . ? C7B C6B H6B2 109.6 . . ? H6B1 C6B H6B2 108.1 . . ? O6B C7B O5B 124.0(9) . . ? O6B C7B C6B 118.4(9) . . ? O5B C7B C6B 117.6(9) . . ? N1C Cu3 N2C 96.2(4) . . ? N1C Cu3 O5C 176.0(4) . . ? N2C Cu3 O5C 85.1(3) . . ? N1C Cu3 O1C 83.9(3) . . ? N2C Cu3 O1C 179.0(4) . . ? O5C Cu3 O1C 94.9(3) . . ? C1C O1C Cu3 114.8(6) . . ? C3C O3C La2 150.3(6) . . ? C5C O4C La2 155.1(6) . 2_658 ? C7C O5C Cu3 115.0(6) . . ? C3C N1C C2C 116.6(8) . . ? C3C N1C Cu3 128.2(7) . . ? C2C N1C Cu3 114.6(6) . . ? C5C N2C C6C 117.6(8) . . ? C5C N2C Cu3 127.9(7) . . ? C6C N2C Cu3 114.0(6) . . ? O2C C1C O1C 124.6(9) . . ? O2C C1C C2C 118.1(10) . . ? O1C C1C C2C 117.3(9) . . ? N1C C2C C1C 107.8(9) . . ? N1C C2C H2C1 110.2 . . ? C1C C2C H2C1 110.2 . . ? N1C C2C H2C2 110.2 . . ? C1C C2C H2C2 110.2 . . ? H2C1 C2C H2C2 108.5 . . ? O3C C3C N1C 122.7(9) . . ? O3C C3C C4C 116.6(8) . . ? N1C C3C C4C 120.6(9) . . ? C5C C4C C3C 122.5(8) . . ? C5C C4C H4C1 106.7 . . ? C3C C4C H4C1 106.7 . . ? C5C C4C H4C2 106.7 . . ? C3C C4C H4C2 106.7 . . ? H4C1 C4C H4C2 106.6 . . ? O4C C5C N2C 122.2(9) . . ? O4C C5C C4C 116.2(8) . . ? N2C C5C C4C 121.5(9) . . ? N2C C6C C7C 109.2(9) . . ? N2C C6C H6C1 109.8 . . ? C7C C6C H6C1 109.8 . . ? N2C C6C H6C2 109.8 . . ? C7C C6C H6C2 109.8 . . ? H6C1 C6C H6C2 108.3 . . ? O6C C7C O5C 123.2(10) . . ? O6C C7C C6C 120.4(11) . . ? O5C C7C C6C 116.4(9) . . ? H110 O10W H210 112.2 . . ? H111 O11W H211 113.7 . . ? H112 O12W H212 107.9 . . ? H13A O13A H13B 108.6 . . ? H13C O13B H13D 107.8 . . ? H14A O14A H14B 106.9 . . ? H14A O14A H14D 89.2 . . ? H14B O14A H14D 162.2 . . ? O15W O14B H14C 76.0 2_667 . ? O15W O14B H14D 78.5 2_667 . ? H14C O14B H14D 125.0 . . ? O14B O15W H15A 80.8 2_667 . ? O14B O15W H25B 153.4 2_667 . ? H15A O15W H25B 109.8 . . ? 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 _geom_hbond_publ_flag O1W H11W O6A 0.84 2.25 2.921(10) 137.1 1_655 yes O2W H12W O2C 0.89 1.94 2.788(10) 158.0 . yes O2W H22W O1B 0.83 2.07 2.892(11) 176.6 2_567 yes O3W H13W O10W 0.83 1.95 2.755(11) 161.3 . yes O4W H14W O5B 0.88 2.20 2.857(10) 131.0 . yes O5W H15W O1A 0.97 1.91 2.814(12) 154.3 2_567 yes O5W H25W O12W 0.89 2.13 2.695(17) 120.8 . yes O6W H26W O2C 0.92 1.85 2.761(10) 170.4 1_655 yes O7W H17W O13A 0.88 1.93 2.781(17) 162.8 2_668 yes O7W H17W O13B 0.88 2.27 3.039(18) 146.0 2_668 yes O7W H27W O15W 0.86 1.72 2.55(2) 163.2 . yes O8W H18W O10W 0.89 2.09 2.715(11) 126.7 1_556 yes O8W H28W O6A 0.94 1.87 2.813(10) 172.9 1_656 yes O9W H19W O6A 0.88 2.10 2.805(10) 135.6 2_557 yes O9W H29W O11W 0.88 2.15 2.715(10) 121.4 . yes O9W H29W O6W 0.88 2.54 2.992(10) 112.5 . yes O10W H110 O5C 0.82 2.19 2.780(11) 128.8 2_557 yes O11W H111 O1C 0.85 1.91 2.727(10) 160.9 1_655 yes O11W H211 O2B 0.84 1.94 2.712(11) 151.5 2_667 yes O12W H112 O6C 0.87 2.33 2.95(2) 127.8 2_558 yes O12W H212 O6C 0.86 2.05 2.85(2) 156.2 1_565 yes O13A H13A O5W 0.83 2.47 3.054(19) 129.0 . yes O13A H13B O5A 0.82 2.08 2.825(17) 150.5 2_567 yes O13A H13B O2A 0.82 2.26 2.849(17) 128.5 2_567 yes O13B H13C O8W 0.85 2.26 3.096(18) 165.5 2_668 yes O13B H13D O5A 0.85 2.17 2.773(16) 127.0 2_567 yes O14A H14A O1A 0.86 1.91 2.741(13) 162.7 . yes O14B H14D O12W 0.84 2.32 2.80(6) 116.8 1_554 yes O15W H15A O3W 0.82 2.16 2.774(18) 131.0 2_667 yes _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.249 _refine_diff_density_min -1.262 _refine_diff_density_rms 0.215 # start Validation Reply Form _vrf_PUBL772_GLOBAL ; PROBLEM: Suspect O-H Bond in CIF: O14A -- H14D .. 1.35 Ang. RESPONSE: There is no O-H bond here. This is due to the disorder. ; # end Validation Reply Form #===END======================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 835271' #TrackingRef 'Konidaris.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C21 H36 Cu3 Nd2 N6 O27), 11(H2 O)' _chemical_formula_sum 'C42 H94 Cu6 N12 Nd4 O65' _chemical_formula_weight 2765.49 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.190(2) _cell_length_b 13.181(3) _cell_length_c 15.356(3) _cell_angle_alpha 73.70(3) _cell_angle_beta 72.87(3) _cell_angle_gamma 79.78(3) _cell_volume 2066.5(7) _cell_formula_units_Z 1 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 25641 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 4.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4669 _exptl_absorpt_correction_T_max 0.6680 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _publ_section_exptl_refinement ; The water molecules O13 and O14 were disordered over two sites with occupancy ratio of 0.54/0.46 and 0.77/0.23 respectively. The water molecule O15 was partially lost and refined with occupancy of 0.5. The H~2~O hydrogen atoms were either located from the difference Fourier map or by using HYDROGEN program (Nardelli, 1999) and constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogens were positioned geometrically and were also constrained to ride on their parent atoms, with C---H =0.99 \%A, and U~iso~ = 1.2 U~eq~(parent atom). The highest peak is located 0.66 \%A from atom H13A and the deepest hole is located 0.75 \%A from atom Nd2. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_reflns_number 36216 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.43 _reflns_number_total 9405 _reflns_number_gt 7334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1b (Crystal Impact GbR, 2006)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+2.1572P] 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 9405 _refine_ls_number_parameters 600 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Nd1 Nd 0.19171(2) 0.237251(18) 0.944036(17) 0.02718(7) Uani 1 1 d . . . O1W O 0.3189(3) 0.0891(3) 0.8761(3) 0.0410(8) Uani 1 1 d . . . H11W H 0.3456 0.1054 0.8156 0.061 Uiso 1 1 d R . . H21W H 0.3820 0.0394 0.8944 0.061 Uiso 1 1 d R . . O2W O -0.0181(3) 0.2513(4) 1.0597(3) 0.0537(10) Uani 1 1 d . . . H12W H -0.0162 0.2648 1.1137 0.081 Uiso 1 1 d R . . H22W H -0.0945 0.2656 1.0595 0.081 Uiso 1 1 d R . . O3W O 0.2493(3) 0.2949(3) 0.7687(2) 0.0370(8) Uani 1 1 d . . . H13W H 0.2336 0.2766 0.7246 0.056 Uiso 1 1 d R . . H23W H 0.3239 0.3121 0.7444 0.056 Uiso 1 1 d R . . O4W O 0.1294(4) 0.4303(3) 0.8965(3) 0.0488(9) Uani 1 1 d . . . H14W H 0.1243 0.4780 0.9301 0.073 Uiso 1 1 d R . . H24W H 0.1271 0.4734 0.8421 0.073 Uiso 1 1 d R . . Nd2 Nd 0.49393(2) 0.260067(18) 1.381356(17) 0.02845(7) Uani 1 1 d . . . O5W O 0.3047(4) 0.3864(4) 1.4237(4) 0.0757(15) Uani 1 1 d . . . H15W H 0.2378 0.4341 1.3955 0.113 Uiso 1 1 d R . . H25W H 0.2755 0.3753 1.4833 0.113 Uiso 1 1 d R . . O6W O 0.7002(3) 0.2861(3) 1.2539(2) 0.0405(8) Uani 1 1 d . . . H16W H 0.6987 0.3410 1.2102 0.061 Uiso 1 1 d R . . H26W H 0.7855 0.2590 1.2556 0.061 Uiso 1 1 d R . . O7W O 0.5569(5) 0.4097(3) 1.4189(4) 0.0678(14) Uani 1 1 d . . . H17W H 0.5721 0.3951 1.4776 0.102 Uiso 1 1 d R . . H27W H 0.6299 0.4350 1.3874 0.102 Uiso 1 1 d R . . O8W O 0.4181(3) 0.1983(3) 1.5526(2) 0.0476(9) Uani 1 1 d . . . H18W H 0.3473 0.1692 1.5646 0.071 Uiso 1 1 d R . . H28W H 0.4486 0.1639 1.6074 0.071 Uiso 1 1 d R . . O9W O 0.5589(3) 0.0992(3) 1.3196(3) 0.0405(8) Uani 1 1 d . . . H19W H 0.5031 0.0669 1.3088 0.061 Uiso 1 1 d R . . H29W H 0.6203 0.1091 1.2703 0.061 Uiso 1 1 d R . . Cu1 Cu -0.23933(5) 0.21302(4) 0.76816(4) 0.03030(13) Uani 1 1 d . . . O1A O -0.1553(4) 0.5076(3) 0.7020(3) 0.0462(9) Uani 1 1 d . . . O2A O -0.2431(3) 0.3637(3) 0.7096(2) 0.0394(8) Uani 1 1 d . . . O3A O 0.0394(3) 0.1781(3) 0.8978(2) 0.0368(8) Uani 1 1 d . . . O4A O -0.2126(3) -0.0904(3) 0.9272(2) 0.0387(8) Uani 1 1 d . . . O5A O -0.3667(3) 0.1977(3) 0.7101(2) 0.0379(8) Uani 1 1 d . . . O6A O -0.4790(3) 0.0791(3) 0.7015(2) 0.0351(7) Uani 1 1 d . . . N1A N -0.1144(4) 0.2335(3) 0.8220(3) 0.0353(9) Uani 1 1 d . . . N2A N -0.2496(4) 0.0657(3) 0.8260(3) 0.0373(9) Uani 1 1 d . . . C1A C -0.1667(5) 0.4109(4) 0.7308(4) 0.0411(12) Uani 1 1 d . . . C2A C -0.0841(5) 0.3419(4) 0.7925(4) 0.0408(12) Uani 1 1 d . . . H2A1 H 0.0054 0.3444 0.7571 0.049 Uiso 1 1 calc R . . H2A2 H -0.0968 0.3699 0.8484 0.049 Uiso 1 1 calc R . . C3A C -0.0508(4) 0.1605(4) 0.8719(3) 0.0312(10) Uani 1 1 d . . . C4A C -0.0838(4) 0.0470(4) 0.9031(3) 0.0316(10) Uani 1 1 d . . . H4A1 H -0.0062 0.0037 0.8780 0.038 Uiso 1 1 calc R . . H4A2 H -0.0979 0.0269 0.9723 0.038 Uiso 1 1 calc R . . C5A C -0.1893(4) 0.0063(4) 0.8841(3) 0.0361(11) Uani 1 1 d . . . C6A C -0.3512(4) 0.0205(4) 0.8087(3) 0.0358(11) Uani 1 1 d . . . H6A1 H -0.4189 0.0030 0.8673 0.043 Uiso 1 1 calc R . . H6A2 H -0.3171 -0.0453 0.7870 0.043 Uiso 1 1 calc R . . C7A C -0.4016(4) 0.1025(4) 0.7350(3) 0.0328(10) Uani 1 1 d . . . Cu2 Cu 0.34245(5) 0.58752(4) 1.03352(4) 0.02857(13) Uani 1 1 d . . . O1B O 0.2809(3) 0.7116(3) 0.9480(2) 0.0371(8) Uani 1 1 d . . . O2B O 0.2743(3) 0.8868(3) 0.9083(2) 0.0398(8) Uani 1 1 d . . . O3B O 0.5955(3) 0.7249(3) 1.0955(3) 0.0401(8) Uani 1 1 d . . . O4B O 0.4681(4) 0.3824(3) 1.2461(3) 0.0532(10) Uani 1 1 d . . . O5B O 0.2443(3) 0.4899(3) 1.0144(2) 0.0398(8) Uani 1 1 d . . . O6B O 0.2042(4) 0.3204(3) 1.0642(2) 0.0416(8) Uani 1 1 d . . . N1B N 0.4354(4) 0.6837(3) 1.0534(3) 0.0319(8) Uani 1 1 d . . . N2B N 0.3948(4) 0.4675(3) 1.1211(3) 0.0356(9) Uani 1 1 d . . . C1B C 0.3189(5) 0.7984(4) 0.9466(3) 0.0332(10) Uani 1 1 d . . . C2B C 0.4223(5) 0.7910(4) 0.9937(3) 0.0326(10) Uani 1 1 d . . . H2B1 H 0.5025 0.8063 0.9456 0.039 Uiso 1 1 calc R . . H2B2 H 0.4013 0.8438 1.0322 0.039 Uiso 1 1 calc R . . C3B C 0.5208(4) 0.6615(4) 1.1000(3) 0.0316(10) Uani 1 1 d . . . C4B C 0.5305(5) 0.5533(4) 1.1702(3) 0.0371(11) Uani 1 1 d . . . H4B1 H 0.6206 0.5258 1.1569 0.045 Uiso 1 1 calc R . . H4B2 H 0.5081 0.5680 1.2332 0.045 Uiso 1 1 calc R . . C5B C 0.4602(4) 0.4645(4) 1.1794(3) 0.0364(11) Uani 1 1 d . . . C6B C 0.3266(5) 0.3759(4) 1.1390(3) 0.0368(11) Uani 1 1 d . . . H6B1 H 0.2689 0.3642 1.2029 0.044 Uiso 1 1 calc R . . H6B2 H 0.3867 0.3114 1.1352 0.044 Uiso 1 1 calc R . . C7B C 0.2529(5) 0.3960(4) 1.0673(3) 0.0378(11) Uani 1 1 d . . . Cu3 Cu 0.08638(5) -0.03628(4) 1.39805(4) 0.02974(13) Uani 1 1 d . . . O1C O -0.0110(3) 0.0620(3) 1.3160(2) 0.0344(7) Uani 1 1 d . . . O2C O -0.0466(3) 0.2335(3) 1.2502(2) 0.0368(8) Uani 1 1 d . . . O3C O 0.3135(3) 0.1760(3) 1.3952(2) 0.0356(7) Uani 1 1 d . . . O4C O 0.3306(3) -0.1835(2) 1.5574(2) 0.0344(7) Uani 1 1 d . . . O5C O 0.0148(3) -0.1617(3) 1.4014(2) 0.0400(8) Uani 1 1 d . . . O6C O 0.0124(5) -0.3347(3) 1.4710(3) 0.0677(13) Uani 1 1 d . . . N1C N 0.1647(4) 0.0864(3) 1.3861(3) 0.0318(8) Uani 1 1 d . . . N2C N 0.1784(4) -0.1315(3) 1.4798(3) 0.0313(8) Uani 1 1 d . . . C1C C 0.0143(4) 0.1586(4) 1.2936(3) 0.0338(10) Uani 1 1 d . . . C2C C 0.1252(4) 0.1796(4) 1.3204(3) 0.0341(10) Uani 1 1 d . . . H2C1 H 0.1954 0.1972 1.2635 0.041 Uiso 1 1 calc R . . H2C2 H 0.1016 0.2409 1.3494 0.041 Uiso 1 1 calc R . . C3C C 0.2574(4) 0.0926(4) 1.4197(3) 0.0278(9) Uani 1 1 d . . . C4C C 0.2962(4) 0.0010(4) 1.4935(3) 0.0300(10) Uani 1 1 d . . . H4C1 H 0.2600 0.0211 1.5542 0.036 Uiso 1 1 calc R . . H4C2 H 0.3886 -0.0018 1.4807 0.036 Uiso 1 1 calc R . . C5C C 0.2676(4) -0.1113(4) 1.5100(3) 0.0293(9) Uani 1 1 d . . . C6C C 0.1540(5) -0.2417(4) 1.4995(3) 0.0385(11) Uani 1 1 d . . . H6C1 H 0.1271 -0.2709 1.5683 0.046 Uiso 1 1 calc R . . H6C2 H 0.2321 -0.2844 1.4742 0.046 Uiso 1 1 calc R . . C7C C 0.0525(5) -0.2493(4) 1.4554(3) 0.0416(12) Uani 1 1 d . . . O10W O 0.1809(3) 0.1842(3) 0.6659(2) 0.0432(8) Uani 1 1 d . . . H110 H 0.1517 0.2051 0.6170 0.065 Uiso 1 1 d R . . H210 H 0.1216 0.1756 0.7131 0.065 Uiso 1 1 d R . . O11W O 0.8014(3) 0.0288(3) 1.2518(2) 0.0387(8) Uani 1 1 d . . . H111 H 0.8536 0.0517 1.2706 0.058 Uiso 1 1 d R . . H211 H 0.8063 0.0445 1.1971 0.058 Uiso 1 1 d R . . O12W O 0.1329(6) 0.4707(5) 1.5532(4) 0.109(2) Uani 1 1 d . . . H112 H 0.0657 0.4514 1.5786 0.164 Uiso 1 1 d R . . H212 H 0.1203 0.5416 1.5206 0.164 Uiso 1 1 d R . . O13A O 0.4066(9) 0.5952(7) 1.4052(6) 0.0546(14) Uani 0.457(6) 1 d P A 1 H13A H 0.3513 0.5603 1.4383 0.082 Uiso 0.457(6) 1 d PR A 1 H13B H 0.3830 0.6426 1.3658 0.082 Uiso 0.457(6) 1 d PR A 1 O13B O 0.5199(8) 0.6312(6) 1.3668(5) 0.0546(14) Uani 0.543(6) 1 d P A 2 H13C H 0.5263 0.6747 1.3977 0.082 Uiso 0.543(6) 1 d PR A 2 H13D H 0.5078 0.6691 1.3148 0.082 Uiso 0.543(6) 1 d PR A 2 O14A O 0.0251(6) 0.5619(4) 0.7635(5) 0.066(3) Uani 0.739(11) 1 d P B 3 H14A H -0.0234 0.5548 0.7294 0.099 Uiso 0.739(11) 1 d PR B 3 H14B H -0.0045 0.5880 0.8006 0.099 Uiso 0.739(11) 1 d PR B 3 O14B O 0.1460(17) 0.5507(13) 0.7126(11) 0.058(6) Uani 0.261(11) 1 d P . 4 H14C H 0.1796 0.5988 0.6593 0.088 Uiso 0.261(11) 1 d PR B 4 H14D H 0.1149 0.5026 0.7012 0.088 Uiso 0.261(11) 1 d PR B 4 O15W O 0.7571(8) 0.5007(6) 1.3454(6) 0.060(2) Uani 0.50 1 d P . . H15A H 0.7553 0.5342 1.2944 0.090 Uiso 0.50 1 d PR . . H25B H 0.7327 0.5364 1.3866 0.090 Uiso 0.50 1 d PR . . 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 0.03001(13) 0.02296(12) 0.03233(13) -0.00336(10) -0.01520(10) -0.00561(9) O1W 0.0390(19) 0.0352(18) 0.049(2) -0.0132(16) -0.0087(16) -0.0037(15) O2W 0.0331(19) 0.092(3) 0.046(2) -0.031(2) -0.0109(16) -0.005(2) O3W 0.0440(19) 0.0365(18) 0.0330(17) -0.0038(14) -0.0122(15) -0.0137(15) O4W 0.076(3) 0.0280(18) 0.049(2) -0.0063(16) -0.032(2) 0.0017(18) Nd2 0.03188(14) 0.02373(12) 0.03301(13) -0.00351(10) -0.01597(10) -0.00381(10) O5W 0.073(3) 0.070(3) 0.112(4) -0.052(3) -0.061(3) 0.034(2) O6W 0.0329(18) 0.046(2) 0.0369(18) 0.0048(16) -0.0115(15) -0.0094(16) O7W 0.098(3) 0.0293(19) 0.106(4) -0.011(2) -0.079(3) -0.003(2) O8W 0.0354(19) 0.074(3) 0.0325(18) -0.0060(18) -0.0123(15) -0.0075(18) O9W 0.0368(19) 0.0396(19) 0.052(2) -0.0209(17) -0.0101(16) -0.0088(15) Cu1 0.0360(3) 0.0263(3) 0.0307(3) -0.0047(2) -0.0111(2) -0.0081(2) O1A 0.053(2) 0.0291(18) 0.061(2) -0.0067(17) -0.0236(19) -0.0053(16) O2A 0.0372(19) 0.0354(18) 0.047(2) -0.0009(16) -0.0194(16) -0.0086(15) O3A 0.0379(18) 0.0409(19) 0.0378(18) -0.0059(15) -0.0174(15) -0.0134(15) O4A 0.047(2) 0.0280(17) 0.0410(19) 0.0050(14) -0.0202(16) -0.0091(15) O5A 0.0386(19) 0.0378(18) 0.0433(19) -0.0123(15) -0.0133(15) -0.0109(15) O6A 0.0336(17) 0.0385(18) 0.0390(18) -0.0087(15) -0.0154(14) -0.0094(15) N1A 0.041(2) 0.029(2) 0.035(2) -0.0040(17) -0.0136(18) -0.0030(18) N2A 0.038(2) 0.036(2) 0.039(2) -0.0059(18) -0.0127(18) -0.0067(18) C1A 0.042(3) 0.038(3) 0.046(3) -0.013(2) -0.012(2) -0.006(2) C2A 0.044(3) 0.036(3) 0.046(3) -0.009(2) -0.017(2) -0.007(2) C3A 0.033(2) 0.034(2) 0.029(2) -0.0073(19) -0.0085(19) -0.007(2) C4A 0.032(2) 0.029(2) 0.035(2) -0.0072(19) -0.011(2) -0.0046(19) C5A 0.031(2) 0.043(3) 0.037(3) -0.015(2) -0.010(2) 0.000(2) C6A 0.032(2) 0.042(3) 0.039(3) -0.013(2) -0.013(2) -0.006(2) C7A 0.035(2) 0.034(2) 0.033(2) -0.011(2) -0.008(2) -0.008(2) Cu2 0.0358(3) 0.0242(3) 0.0294(3) -0.0019(2) -0.0155(2) -0.0082(2) O1B 0.050(2) 0.0293(17) 0.0382(18) -0.0023(14) -0.0222(16) -0.0097(15) O2B 0.052(2) 0.0273(17) 0.0438(19) -0.0041(15) -0.0224(17) -0.0026(15) O3B 0.0371(18) 0.0373(19) 0.053(2) -0.0064(16) -0.0203(16) -0.0137(15) O4B 0.053(2) 0.048(2) 0.057(2) 0.0164(19) -0.0338(19) -0.0129(19) O5B 0.051(2) 0.0353(18) 0.0399(19) -0.0037(15) -0.0219(16) -0.0145(16) O6B 0.061(2) 0.0318(18) 0.0404(19) -0.0085(15) -0.0190(17) -0.0184(17) N1B 0.033(2) 0.032(2) 0.033(2) -0.0040(17) -0.0134(17) -0.0099(17) N2B 0.037(2) 0.030(2) 0.037(2) -0.0004(17) -0.0100(18) -0.0068(17) C1B 0.039(3) 0.031(2) 0.026(2) -0.0055(19) -0.0053(19) -0.005(2) C2B 0.041(3) 0.027(2) 0.031(2) -0.0082(19) -0.008(2) -0.007(2) C3B 0.031(2) 0.035(2) 0.032(2) -0.012(2) -0.0083(19) -0.004(2) C4B 0.037(3) 0.041(3) 0.032(2) -0.004(2) -0.012(2) -0.003(2) C5B 0.030(2) 0.041(3) 0.037(3) -0.007(2) -0.014(2) 0.002(2) C6B 0.046(3) 0.027(2) 0.041(3) -0.005(2) -0.016(2) -0.009(2) C7B 0.046(3) 0.036(3) 0.033(2) -0.011(2) -0.007(2) -0.009(2) Cu3 0.0282(3) 0.0327(3) 0.0310(3) -0.0047(2) -0.0128(2) -0.0063(2) O1C 0.0358(18) 0.0370(18) 0.0349(17) -0.0073(14) -0.0156(14) -0.0063(15) O2C 0.0317(17) 0.0414(19) 0.0362(18) -0.0057(15) -0.0136(14) 0.0007(15) O3C 0.0320(17) 0.0315(17) 0.0452(19) -0.0040(15) -0.0156(15) -0.0075(14) O4C 0.0370(18) 0.0310(17) 0.0367(17) -0.0027(14) -0.0172(15) -0.0030(14) O5C 0.045(2) 0.046(2) 0.0364(18) -0.0044(16) -0.0190(16) -0.0171(16) O6C 0.097(3) 0.054(3) 0.069(3) 0.009(2) -0.047(3) -0.047(3) N1C 0.028(2) 0.031(2) 0.037(2) -0.0033(17) -0.0156(17) -0.0015(16) N2C 0.035(2) 0.031(2) 0.0303(19) -0.0025(16) -0.0142(16) -0.0070(17) C1C 0.030(2) 0.041(3) 0.030(2) -0.008(2) -0.0110(19) 0.002(2) C2C 0.031(2) 0.033(2) 0.038(3) -0.004(2) -0.014(2) -0.001(2) C3C 0.024(2) 0.032(2) 0.029(2) -0.0090(19) -0.0071(18) -0.0026(18) C4C 0.029(2) 0.031(2) 0.032(2) -0.0049(19) -0.0135(19) -0.0054(19) C5C 0.027(2) 0.030(2) 0.028(2) -0.0049(18) -0.0059(18) -0.0034(18) C6C 0.052(3) 0.034(3) 0.033(2) 0.000(2) -0.013(2) -0.021(2) C7C 0.050(3) 0.044(3) 0.035(3) 0.001(2) -0.016(2) -0.023(3) O10W 0.0374(19) 0.061(2) 0.0370(18) -0.0172(17) -0.0087(15) -0.0118(17) O11W 0.0381(19) 0.044(2) 0.0404(18) -0.0142(16) -0.0156(15) -0.0041(16) O12W 0.104(5) 0.087(4) 0.115(5) -0.013(4) -0.002(4) -0.019(4) O13A 0.076(4) 0.042(3) 0.046(3) -0.006(3) -0.026(3) 0.002(3) O13B 0.076(4) 0.042(3) 0.046(3) -0.006(3) -0.026(3) 0.002(3) O14A 0.086(6) 0.032(3) 0.099(5) 0.007(3) -0.070(5) -0.014(3) O14B 0.068(14) 0.060(10) 0.053(10) 0.012(8) -0.029(9) -0.040(9) O15W 0.058(5) 0.036(4) 0.069(6) 0.011(4) -0.008(4) -0.014(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 O3A 2.347(3) . yes Nd1 O4A 2.382(3) 2_557 yes Nd1 O3B 2.385(3) 2_667 yes Nd1 O6B 2.443(3) . yes Nd1 O4W 2.474(3) . yes Nd1 O1W 2.492(4) . yes Nd1 O3W 2.499(3) . yes Nd1 O2W 2.505(4) . yes O1W H11W 0.8636 . ? O1W H21W 0.9250 . ? O2W H12W 0.9021 . ? O2W H22W 0.8425 . ? O3W H13W 0.8507 . ? O3W H23W 0.8514 . ? O4W H14W 0.9035 . ? O4W H24W 0.8729 . ? Nd2 O4B 2.303(4) . yes Nd2 O4C 2.369(3) 2_658 yes Nd2 O3C 2.400(3) . yes Nd2 O8W 2.454(3) . yes Nd2 O7W 2.467(4) . yes Nd2 O9W 2.470(3) . yes Nd2 O5W 2.495(4) . yes Nd2 O6W 2.553(3) . yes O5W H15W 1.0069 . ? O5W H25W 0.8559 . ? O6W H16W 0.8394 . ? O6W H26W 0.9626 . ? O7W H17W 0.9271 . ? O7W H27W 0.8872 . ? O8W H18W 0.8890 . ? O8W H28W 0.9655 . ? O9W H19W 0.8908 . ? O9W H29W 0.8554 . ? Cu1 N2A 1.904(4) . ? Cu1 N1A 1.911(4) . ? Cu1 O2A 1.936(3) . ? Cu1 O5A 1.954(3) . ? O1A C1A 1.242(6) . ? O2A C1A 1.300(6) . ? O3A C3A 1.267(6) . ? O4A C5A 1.293(6) . ? O4A Nd1 2.382(3) 2_557 ? O5A C7A 1.300(5) . ? O6A C7A 1.248(5) . ? N1A C3A 1.297(6) . ? N1A C2A 1.443(6) . ? N2A C5A 1.280(6) . ? N2A C6A 1.492(6) . ? C1A C2A 1.521(7) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3A C4A 1.513(6) . ? C4A C5A 1.512(6) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C6A C7A 1.497(7) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? Cu2 N2B 1.896(4) . ? Cu2 N1B 1.912(4) . ? Cu2 O1B 1.950(3) . ? Cu2 O5B 1.963(3) . ? O1B C1B 1.281(6) . ? O2B C1B 1.239(6) . ? O3B C3B 1.258(5) . ? O3B Nd1 2.385(3) 2_667 ? O4B C5B 1.275(6) . ? O5B C7B 1.281(6) . ? O6B C7B 1.235(6) . ? N1B C3B 1.302(6) . ? N1B C2B 1.463(6) . ? N2B C5B 1.302(6) . ? N2B C6B 1.460(6) . ? C1B C2B 1.513(7) . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C3B C4B 1.536(7) . ? C4B C5B 1.475(7) . ? C4B H4B1 0.9900 . ? C4B H4B2 0.9900 . ? C6B C7B 1.503(7) . ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? Cu3 N2C 1.905(4) . ? Cu3 N1C 1.912(4) . ? Cu3 O5C 1.942(3) . ? Cu3 O1C 1.962(3) . ? O1C C1C 1.282(6) . ? O2C C1C 1.242(6) . ? O3C C3C 1.271(5) . ? O4C C5C 1.268(5) . ? O4C Nd2 2.369(3) 2_658 ? O5C C7C 1.302(6) . ? O6C C7C 1.221(6) . ? N1C C3C 1.311(6) . ? N1C C2C 1.449(6) . ? N2C C5C 1.311(6) . ? N2C C6C 1.456(6) . ? C1C C2C 1.508(6) . ? C2C H2C1 0.9900 . ? C2C H2C2 0.9900 . ? C3C C4C 1.506(6) . ? C4C C5C 1.506(6) . ? C4C H4C1 0.9900 . ? C4C H4C2 0.9900 . ? C6C C7C 1.514(7) . ? C6C H6C1 0.9900 . ? C6C H6C2 0.9900 . ? O10W H110 0.8628 . ? O10W H210 0.8221 . ? O11W H111 0.8518 . ? O11W H211 0.7941 . ? O12W H112 0.7882 . ? O12W H212 0.9359 . ? O13A H13A 0.7984 . ? O13A H13B 0.8061 . ? O13B H13C 0.8648 . ? O13B H13D 0.8491 . ? O14A H14A 0.8892 . ? O14A H14B 0.7143 . ? O14A H14D 1.4527 . ? O14B O15W 1.39(2) 2_667 ? O14B H14C 0.9081 . ? O14B H14D 0.8554 . ? O15W O14B 1.39(2) 2_667 ? O15W H15A 0.7871 . ? O15W H25B 0.8463 . ? 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 O3A Nd1 O4A 98.51(12) . 2_557 ? O3A Nd1 O3B 146.29(12) . 2_667 ? O4A Nd1 O3B 94.57(12) 2_557 2_667 ? O3A Nd1 O6B 139.04(12) . . ? O4A Nd1 O6B 76.37(12) 2_557 . ? O3B Nd1 O6B 74.30(12) 2_667 . ? O3A Nd1 O4W 97.79(13) . . ? O4A Nd1 O4W 145.12(13) 2_557 . ? O3B Nd1 O4W 88.61(13) 2_667 . ? O6B Nd1 O4W 71.11(12) . . ? O3A Nd1 O1W 79.41(12) . . ? O4A Nd1 O1W 73.14(12) 2_557 . ? O3B Nd1 O1W 74.89(12) 2_667 . ? O6B Nd1 O1W 134.15(12) . . ? O4W Nd1 O1W 140.43(12) . . ? O3A Nd1 O3W 74.61(11) . . ? O4A Nd1 O3W 143.06(12) 2_557 . ? O3B Nd1 O3W 76.28(12) 2_667 . ? O6B Nd1 O3W 132.17(11) . . ? O4W Nd1 O3W 71.31(12) . . ? O1W Nd1 O3W 69.92(12) . . ? O3A Nd1 O2W 69.71(12) . . ? O4A Nd1 O2W 77.32(14) 2_557 . ? O3B Nd1 O2W 143.84(12) 2_667 . ? O6B Nd1 O2W 69.53(12) . . ? O4W Nd1 O2W 79.78(14) . . ? O1W Nd1 O2W 133.00(13) . . ? O3W Nd1 O2W 129.84(12) . . ? Nd1 O1W H11W 114.5 . . ? Nd1 O1W H21W 131.3 . . ? H11W O1W H21W 102.9 . . ? Nd1 O2W H12W 114.9 . . ? Nd1 O2W H22W 138.4 . . ? H12W O2W H22W 103.6 . . ? Nd1 O3W H13W 135.9 . . ? Nd1 O3W H23W 114.1 . . ? H13W O3W H23W 102.4 . . ? Nd1 O4W H14W 125.7 . . ? Nd1 O4W H24W 132.3 . . ? H14W O4W H24W 99.9 . . ? O4B Nd2 O4C 134.18(12) . 2_658 ? O4B Nd2 O3C 92.12(13) . . ? O4C Nd2 O3C 127.50(11) 2_658 . ? O4B Nd2 O8W 147.51(15) . . ? O4C Nd2 O8W 71.74(12) 2_658 . ? O3C Nd2 O8W 78.75(12) . . ? O4B Nd2 O7W 84.84(15) . . ? O4C Nd2 O7W 76.34(12) 2_658 . ? O3C Nd2 O7W 142.38(15) . . ? O8W Nd2 O7W 83.95(15) . . ? O4B Nd2 O9W 99.11(14) . . ? O4C Nd2 O9W 78.47(12) 2_658 . ? O3C Nd2 O9W 69.51(11) . . ? O8W Nd2 O9W 106.46(13) . . ? O7W Nd2 O9W 148.01(14) . . ? O4B Nd2 O5W 71.54(17) . . ? O4C Nd2 O5W 135.63(13) 2_658 . ? O3C Nd2 O5W 72.83(14) . . ? O8W Nd2 O5W 75.98(16) . . ? O7W Nd2 O5W 70.66(16) . . ? O9W Nd2 O5W 140.78(13) . . ? O4B Nd2 O6W 67.39(13) . . ? O4C Nd2 O6W 68.61(11) 2_658 . ? O3C Nd2 O6W 131.95(12) . . ? O8W Nd2 O6W 139.87(11) . . ? O7W Nd2 O6W 81.03(16) . . ? O9W Nd2 O6W 71.58(12) . . ? O5W Nd2 O6W 131.56(15) . . ? Nd2 O5W H15W 140.3 . . ? Nd2 O5W H25W 111.1 . . ? H15W O5W H25W 106.3 . . ? Nd2 O6W H16W 115.1 . . ? Nd2 O6W H26W 130.8 . . ? H16W O6W H26W 110.7 . . ? Nd2 O7W H17W 115.4 . . ? Nd2 O7W H27W 120.4 . . ? H17W O7W H27W 95.2 . . ? Nd2 O8W H18W 107.6 . . ? Nd2 O8W H28W 141.0 . . ? H18W O8W H28W 102.9 . . ? Nd2 O9W H19W 121.1 . . ? Nd2 O9W H29W 111.1 . . ? H19W O9W H29W 108.0 . . ? N2A Cu1 N1A 97.62(17) . . ? N2A Cu1 O2A 175.36(16) . . ? N1A Cu1 O2A 86.35(15) . . ? N2A Cu1 O5A 84.59(16) . . ? N1A Cu1 O5A 177.78(15) . . ? O2A Cu1 O5A 91.46(14) . . ? C1A O2A Cu1 113.3(3) . . ? C3A O3A Nd1 171.3(3) . . ? C5A O4A Nd1 146.8(3) . 2_557 ? C7A O5A Cu1 114.0(3) . . ? C3A N1A C2A 120.4(4) . . ? C3A N1A Cu1 126.9(3) . . ? C2A N1A Cu1 112.4(3) . . ? C5A N2A C6A 117.9(4) . . ? C5A N2A Cu1 127.5(4) . . ? C6A N2A Cu1 114.2(3) . . ? O1A C1A O2A 124.1(5) . . ? O1A C1A C2A 118.6(4) . . ? O2A C1A C2A 117.3(4) . . ? N1A C2A C1A 110.5(4) . . ? N1A C2A H2A1 109.5 . . ? C1A C2A H2A1 109.5 . . ? N1A C2A H2A2 109.5 . . ? C1A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 108.1 . . ? O3A C3A N1A 123.7(4) . . ? O3A C3A C4A 116.2(4) . . ? N1A C3A C4A 120.1(4) . . ? C5A C4A C3A 126.6(4) . . ? C5A C4A H4A1 105.7 . . ? C3A C4A H4A1 105.7 . . ? C5A C4A H4A2 105.7 . . ? C3A C4A H4A2 105.7 . . ? H4A1 C4A H4A2 106.1 . . ? N2A C5A O4A 122.7(4) . . ? N2A C5A C4A 120.2(4) . . ? O4A C5A C4A 117.0(4) . . ? N2A C6A C7A 107.5(4) . . ? N2A C6A H6A1 110.2 . . ? C7A C6A H6A1 110.2 . . ? N2A C6A H6A2 110.2 . . ? C7A C6A H6A2 110.2 . . ? H6A1 C6A H6A2 108.5 . . ? O6A C7A O5A 121.7(4) . . ? O6A C7A C6A 119.4(4) . . ? O5A C7A C6A 118.8(4) . . ? N2B Cu2 N1B 95.34(17) . . ? N2B Cu2 O1B 177.24(17) . . ? N1B Cu2 O1B 85.21(15) . . ? N2B Cu2 O5B 84.91(16) . . ? N1B Cu2 O5B 179.00(17) . . ? O1B Cu2 O5B 94.50(14) . . ? C1B O1B Cu2 113.6(3) . . ? C3B O3B Nd1 147.3(3) . 2_667 ? C5B O4B Nd2 167.2(4) . . ? C7B O5B Cu2 113.6(3) . . ? C7B O6B Nd1 137.2(3) . . ? C3B N1B C2B 117.9(4) . . ? C3B N1B Cu2 128.1(3) . . ? C2B N1B Cu2 112.9(3) . . ? C5B N2B C6B 117.0(4) . . ? C5B N2B Cu2 127.9(3) . . ? C6B N2B Cu2 113.2(3) . . ? O2B C1B O1B 122.6(5) . . ? O2B C1B C2B 119.4(4) . . ? O1B C1B C2B 117.9(4) . . ? N1B C2B C1B 108.7(4) . . ? N1B C2B H2B1 110.0 . . ? C1B C2B H2B1 110.0 . . ? N1B C2B H2B2 110.0 . . ? C1B C2B H2B2 110.0 . . ? H2B1 C2B H2B2 108.3 . . ? O3B C3B N1B 124.7(4) . . ? O3B C3B C4B 115.4(4) . . ? N1B C3B C4B 119.9(4) . . ? C5B C4B C3B 123.7(4) . . ? C5B C4B H4B1 106.4 . . ? C3B C4B H4B1 106.4 . . ? C5B C4B H4B2 106.4 . . ? C3B C4B H4B2 106.4 . . ? H4B1 C4B H4B2 106.5 . . ? O4B C5B N2B 120.5(5) . . ? O4B C5B C4B 117.3(4) . . ? N2B C5B C4B 122.2(4) . . ? N2B C6B C7B 109.2(4) . . ? N2B C6B H6B1 109.8 . . ? C7B C6B H6B1 109.8 . . ? N2B C6B H6B2 109.8 . . ? C7B C6B H6B2 109.8 . . ? H6B1 C6B H6B2 108.3 . . ? O6B C7B O5B 124.8(5) . . ? O6B C7B C6B 117.3(4) . . ? O5B C7B C6B 117.9(4) . . ? N2C Cu3 N1C 95.59(16) . . ? N2C Cu3 O5C 85.17(15) . . ? N1C Cu3 O5C 175.87(16) . . ? N2C Cu3 O1C 178.93(16) . . ? N1C Cu3 O1C 84.58(15) . . ? O5C Cu3 O1C 94.73(14) . . ? C1C O1C Cu3 114.0(3) . . ? C3C O3C Nd2 149.8(3) . . ? C5C O4C Nd2 155.4(3) . 2_658 ? C7C O5C Cu3 114.9(3) . . ? C3C N1C C2C 117.6(4) . . ? C3C N1C Cu3 128.6(3) . . ? C2C N1C Cu3 113.2(3) . . ? C5C N2C C6C 118.2(4) . . ? C5C N2C Cu3 128.1(3) . . ? C6C N2C Cu3 113.2(3) . . ? O2C C1C O1C 123.1(4) . . ? O2C C1C C2C 119.6(4) . . ? O1C C1C C2C 117.3(4) . . ? N1C C2C C1C 109.6(4) . . ? N1C C2C H2C1 109.7 . . ? C1C C2C H2C1 109.7 . . ? N1C C2C H2C2 109.7 . . ? C1C C2C H2C2 109.7 . . ? H2C1 C2C H2C2 108.2 . . ? O3C C3C N1C 122.3(4) . . ? O3C C3C C4C 117.8(4) . . ? N1C C3C C4C 119.9(4) . . ? C3C C4C C5C 123.7(4) . . ? C3C C4C H4C1 106.4 . . ? C5C C4C H4C1 106.4 . . ? C3C C4C H4C2 106.4 . . ? C5C C4C H4C2 106.4 . . ? H4C1 C4C H4C2 106.5 . . ? O4C C5C N2C 122.5(4) . . ? O4C C5C C4C 116.5(4) . . ? N2C C5C C4C 121.0(4) . . ? N2C C6C C7C 110.4(4) . . ? N2C C6C H6C1 109.6 . . ? C7C C6C H6C1 109.6 . . ? N2C C6C H6C2 109.6 . . ? C7C C6C H6C2 109.6 . . ? H6C1 C6C H6C2 108.1 . . ? O6C C7C O5C 124.4(5) . . ? O6C C7C C6C 119.6(5) . . ? O5C C7C C6C 116.0(4) . . ? H110 O10W H210 108.6 . . ? H111 O11W H211 118.0 . . ? H112 O12W H212 106.7 . . ? H13A O13A H13B 111.9 . . ? H13C O13B H13D 106.4 . . ? H14A O14A H14B 116.4 . . ? H14A O14A H14D 79.9 . . ? H14B O14A H14D 163.5 . . ? O15W O14B H14C 70.5 2_667 . ? O15W O14B H14D 72.6 2_667 . ? H14C O14B H14D 112.0 . . ? O14B O15W H15A 76.4 2_667 . ? O14B O15W H25B 149.9 2_667 . ? H15A O15W H25B 114.0 . . ? 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 _geom_hbond_publ_flag O1W H11W O6A 0.86 2.26 2.973(5) 139.7 1_655 yes O2W H12W O2C 0.90 1.96 2.794(5) 153.9 . yes O2W H22W O1B 0.84 2.09 2.926(5) 174.1 2_567 yes O3W H13W O10W 0.85 1.96 2.758(5) 156.5 . yes O4W H14W O5B 0.90 2.17 2.841(5) 130.4 . yes O5W H15W O1A 1.01 1.90 2.834(6) 153.3 2_567 yes O5W H25W O12W 0.86 2.08 2.668(8) 125.6 . yes O6W H26W O2C 0.96 1.83 2.782(5) 169.3 1_655 yes O7W H17W O13A 0.93 1.93 2.831(9) 164.9 2_668 yes O7W H17W O13B 0.93 2.26 3.060(9) 144.3 2_668 yes O7W H27W O15W 0.89 1.67 2.537(9) 166.8 . yes O8W H18W O10W 0.89 2.06 2.717(5) 129.4 1_556 yes O8W H28W O6A 0.97 1.86 2.814(5) 169.8 1_656 yes O9W H19W O6A 0.89 2.05 2.788(5) 140.1 2_557 yes O9W H29W O11W 0.86 2.09 2.701(5) 127.6 . yes O9W H29W O6W 0.86 2.57 2.939(5) 107.5 . yes O10W H110 O5C 0.86 2.16 2.774(5) 128.0 2_557 yes O11W H111 O1C 0.85 1.88 2.712(5) 163.8 1_655 yes O11W H211 O2B 0.79 2.00 2.713(5) 149.1 2_667 yes O12W H112 O6C 0.79 2.29 2.785(7) 121.8 2_558 yes O12W H212 O6C 0.94 1.96 2.819(8) 151.7 1_565 yes O13A H13A O5W 0.80 2.52 3.073(10) 127.4 . yes O13A H13B O5A 0.81 2.11 2.847(9) 153.0 2_567 yes O13A H13B O2A 0.81 2.23 2.786(9) 126.6 2_567 yes O13B H13C O8W 0.86 2.27 3.112(9) 166.0 2_668 yes O13B H13D O5A 0.85 2.17 2.783(8) 128.7 2_567 yes O14A H14A O1A 0.89 1.89 2.739(6) 158.1 . yes O14B H14D O12W 0.86 2.37 2.974(18) 128.0 1_554 yes O15W H15A O3W 0.79 2.19 2.773(8) 131.7 2_667 yes _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.350 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.139 # start Validation Reply Form _vrf_PUBL772_GLOBAL ; PROBLEM: Suspect O-H Bond in CIF: O14A -- H14D .. 1.45 Ang. RESPONSE: There is no O-H bond here. This is due to the disorder. ; # end Validation Reply Form #===END======================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 835272' #TrackingRef 'Konidaris.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C21 H36 Cu3 Gd2 N6 O27), 11(H2 O)' _chemical_formula_sum 'C42 H94 Cu6 Gd4 N12 O65' _chemical_formula_weight 2817.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0485(3) _cell_length_b 13.1016(3) _cell_length_c 15.4028(3) _cell_angle_alpha 73.203(2) _cell_angle_beta 72.574(2) _cell_angle_gamma 79.917(2) _cell_volume 2026.92(8) _cell_formula_units_Z 1 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 8962 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 4.893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4138 _exptl_absorpt_correction_T_max 0.6226 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The water molecules O13 and O14 were disordered over two sites with occupancy ratio of 0.59/0.41 and 0.57/0.43 respectively. The water molecule O15 was partially lost and refined with occupancy of 0.5. The H~2~O hydrogen atoms were either located from the difference Fourier map or by using HYDROGEN program (Nardelli, 1999) and constrained to ride on their parent atom, with U~iso~ = 1.5 U~eq~(parent atom). Other hydrogens were positioned geometrically and were also constrained to ride on their parent atoms, with C---H =0.99 \%A, and U~iso~ = 1.2 U~eq~(parent atom). The highest peak is located 0.75 \%A from atom Gd2 and the deepest hole is located 0.74 \%A from atom Gd2. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_reflns_number 39481 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.53 _reflns_number_total 9260 _reflns_number_gt 7268 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1b (Crystal Impact GbR, 2006)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+8.4378P] 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 9260 _refine_ls_number_parameters 606 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 Gd1 Gd 0.19250(2) 0.236282(19) 0.942835(17) 0.01641(7) Uani 1 1 d . . . O1W O 0.3185(4) 0.0919(3) 0.8763(3) 0.0268(8) Uani 1 1 d . . . H11W H 0.3455 0.1056 0.8157 0.040 Uiso 1 1 d R . . H21W H 0.3819 0.0396 0.8945 0.040 Uiso 1 1 d R . . O2W O -0.0144(4) 0.2467(4) 1.0593(3) 0.0353(10) Uani 1 1 d . . . H12W H -0.0162 0.2645 1.1138 0.053 Uiso 1 1 d R . . H22W H -0.0945 0.2653 1.0596 0.053 Uiso 1 1 d R . . O3W O 0.2485(4) 0.2945(3) 0.7708(3) 0.0244(8) Uani 1 1 d . . . H13W H 0.2334 0.2766 0.7249 0.037 Uiso 1 1 d R . . H23W H 0.3237 0.3121 0.7447 0.037 Uiso 1 1 d R . . O4W O 0.1274(4) 0.4257(3) 0.8970(3) 0.0323(10) Uani 1 1 d . . . H14W H 0.1241 0.4779 0.9303 0.049 Uiso 1 1 d R . . H24W H 0.1269 0.4733 0.8423 0.049 Uiso 1 1 d R . . Gd2 Gd 0.49418(2) 0.260835(19) 1.381817(17) 0.01745(7) Uani 1 1 d . . . O5W O 0.3112(5) 0.3872(4) 1.4234(4) 0.0532(14) Uani 1 1 d . . . H15W H 0.2377 0.4341 1.3955 0.080 Uiso 1 1 d R . . H25W H 0.2754 0.3753 1.4833 0.080 Uiso 1 1 d R . . O6W O 0.6983(4) 0.2885(3) 1.2542(3) 0.0311(9) Uani 1 1 d . . . H16W H 0.6985 0.3412 1.2101 0.047 Uiso 1 1 d R . . H26W H 0.7853 0.2592 1.2555 0.047 Uiso 1 1 d R . . O7W O 0.5658(6) 0.4073(3) 1.4115(4) 0.0657(19) Uani 1 1 d . . . H17W H 0.5722 0.3953 1.4766 0.099 Uiso 1 1 d R . . H27W H 0.6300 0.4352 1.3865 0.099 Uiso 1 1 d R . . O8W O 0.4194(4) 0.2008(4) 1.5500(3) 0.0337(10) Uani 1 1 d . . . H18W H 0.3474 0.1691 1.5647 0.051 Uiso 1 1 d R . . H28W H 0.4486 0.1638 1.6075 0.051 Uiso 1 1 d R . . O9W O 0.5568(4) 0.1038(3) 1.3213(3) 0.0280(9) Uani 1 1 d . . . H19W H 0.5035 0.0672 1.3086 0.042 Uiso 1 1 d R . . H29W H 0.6207 0.1094 1.2701 0.042 Uiso 1 1 d R . . Cu1 Cu -0.24083(6) 0.21392(5) 0.76792(4) 0.01842(14) Uani 1 1 d . . . O1A O -0.1564(4) 0.5114(3) 0.6998(3) 0.0307(9) Uani 1 1 d . . . O2A O -0.2446(3) 0.3658(3) 0.7104(3) 0.0252(8) Uani 1 1 d . . . O3A O 0.0396(3) 0.1805(3) 0.8985(3) 0.0225(8) Uani 1 1 d . . . O4A O -0.2159(4) -0.0909(3) 0.9320(3) 0.0259(9) Uani 1 1 d . . . O5A O -0.3661(3) 0.1973(3) 0.7078(3) 0.0225(8) Uani 1 1 d . . . O6A O -0.4769(3) 0.0766(3) 0.6985(3) 0.0226(8) Uani 1 1 d . . . N1A N -0.1177(4) 0.2349(3) 0.8238(3) 0.0211(9) Uani 1 1 d . . . N2A N -0.2499(4) 0.0649(3) 0.8259(3) 0.0204(9) Uani 1 1 d . . . C1A C -0.1679(5) 0.4141(4) 0.7296(4) 0.0244(12) Uani 1 1 d . . . C2A C -0.0858(5) 0.3448(4) 0.7932(4) 0.0264(12) Uani 1 1 d . . . H2A1 H 0.0054 0.3471 0.7585 0.032 Uiso 1 1 calc R . . H2A2 H -0.1000 0.3734 0.8487 0.032 Uiso 1 1 calc R . . C3A C -0.0529(5) 0.1618(4) 0.8735(3) 0.0198(11) Uani 1 1 d . . . C4A C -0.0845(5) 0.0464(4) 0.9061(4) 0.0201(11) Uani 1 1 d . . . H4A1 H -0.0994 0.0263 0.9753 0.024 Uiso 1 1 calc R . . H4A2 H -0.0051 0.0035 0.8813 0.024 Uiso 1 1 calc R . . C5A C -0.1908(5) 0.0040(4) 0.8871(4) 0.0206(11) Uani 1 1 d . . . C6A C -0.3499(5) 0.0198(4) 0.8075(4) 0.0225(11) Uani 1 1 d . . . H6A1 H -0.4194 0.0013 0.8658 0.027 Uiso 1 1 calc R . . H6A2 H -0.3143 -0.0462 0.7861 0.027 Uiso 1 1 calc R . . C7A C -0.4008(5) 0.1029(4) 0.7323(4) 0.0206(11) Uani 1 1 d . . . Cu2 Cu 0.34677(6) 0.58482(5) 1.03151(4) 0.01757(14) Uani 1 1 d . . . O1B O 0.2855(4) 0.7108(3) 0.9456(2) 0.0227(8) Uani 1 1 d . . . O2B O 0.2792(4) 0.8877(3) 0.9071(3) 0.0271(9) Uani 1 1 d . . . O3B O 0.5969(3) 0.7237(3) 1.0993(3) 0.0258(9) Uani 1 1 d . . . O4B O 0.4633(4) 0.3769(3) 1.2480(3) 0.0376(11) Uani 1 1 d . . . O5B O 0.2480(4) 0.4873(3) 1.0110(3) 0.0247(8) Uani 1 1 d . . . O6B O 0.2071(4) 0.3157(3) 1.0607(3) 0.0275(9) Uani 1 1 d . . . N1B N 0.4392(4) 0.6814(3) 1.0534(3) 0.0206(9) Uani 1 1 d . . . N2B N 0.3966(4) 0.4630(3) 1.1198(3) 0.0221(10) Uani 1 1 d . . . C1B C 0.3235(5) 0.7980(4) 0.9455(3) 0.0198(11) Uani 1 1 d . . . C2B C 0.4265(5) 0.7895(4) 0.9944(4) 0.0193(11) Uani 1 1 d . . . H2B1 H 0.5084 0.8060 0.9471 0.023 Uiso 1 1 calc R . . H2B2 H 0.4037 0.8417 1.0334 0.023 Uiso 1 1 calc R . . C3B C 0.5228(5) 0.6585(4) 1.1026(4) 0.0210(11) Uani 1 1 d . . . C4B C 0.5295(5) 0.5505(4) 1.1733(4) 0.0249(12) Uani 1 1 d . . . H4B1 H 0.6208 0.5231 1.1624 0.030 Uiso 1 1 calc R . . H4B2 H 0.5030 0.5652 1.2362 0.030 Uiso 1 1 calc R . . C5B C 0.4597(5) 0.4602(4) 1.1807(4) 0.0235(12) Uani 1 1 d . . . C6B C 0.3258(5) 0.3730(4) 1.1387(4) 0.0247(12) Uani 1 1 d . . . H6B1 H 0.2650 0.3634 1.2018 0.030 Uiso 1 1 calc R . . H6B2 H 0.3849 0.3068 1.1377 0.030 Uiso 1 1 calc R . . C7B C 0.2546(5) 0.3925(4) 1.0651(4) 0.0219(11) Uani 1 1 d . . . Cu3 Cu 0.08617(6) -0.03628(5) 1.39917(4) 0.01970(14) Uani 1 1 d . . . O1C O -0.0106(3) 0.0625(3) 1.3157(3) 0.0245(8) Uani 1 1 d . . . O2C O -0.0469(4) 0.2358(3) 1.2498(3) 0.0291(9) Uani 1 1 d . . . O3C O 0.3131(3) 0.1787(3) 1.3977(3) 0.0236(8) Uani 1 1 d . . . O4C O 0.3303(3) -0.1847(3) 1.5603(3) 0.0227(8) Uani 1 1 d . . . O5C O 0.0177(4) -0.1643(3) 1.4002(3) 0.0278(9) Uani 1 1 d . . . O6C O 0.0187(5) -0.3388(3) 1.4673(3) 0.0419(11) Uani 1 1 d . . . N1C N 0.1619(4) 0.0873(3) 1.3893(3) 0.0211(9) Uani 1 1 d . . . N2C N 0.1789(4) -0.1323(3) 1.4811(3) 0.0204(9) Uani 1 1 d . . . C1C C 0.0136(5) 0.1599(5) 1.2946(4) 0.0242(12) Uani 1 1 d . . . C2C C 0.1239(5) 0.1819(4) 1.3227(4) 0.0238(12) Uani 1 1 d . . . H2C1 H 0.1964 0.2002 1.2665 0.029 Uiso 1 1 calc R . . H2C2 H 0.0986 0.2433 1.3517 0.029 Uiso 1 1 calc R . . C3C C 0.2567(5) 0.0945(4) 1.4224(4) 0.0183(10) Uani 1 1 d . . . C4C C 0.2954(5) 0.0023(4) 1.4968(4) 0.0207(11) Uani 1 1 d . . . H4C1 H 0.2573 0.0218 1.5574 0.025 Uiso 1 1 calc R . . H4C2 H 0.3889 0.0002 1.4845 0.025 Uiso 1 1 calc R . . C5C C 0.2668(5) -0.1113(4) 1.5127(3) 0.0172(10) Uani 1 1 d . . . C6C C 0.1569(6) -0.2439(4) 1.4999(4) 0.0248(12) Uani 1 1 d . . . H6C1 H 0.1275 -0.2744 1.5686 0.030 Uiso 1 1 calc R . . H6C2 H 0.2375 -0.2855 1.4754 0.030 Uiso 1 1 calc R . . C7C C 0.0576(6) -0.2521(5) 1.4535(4) 0.0294(13) Uani 1 1 d . . . O10W O 0.1809(3) 0.1849(3) 0.6667(3) 0.0265(9) Uani 1 1 d . . . H110 H 0.1517 0.2049 0.6174 0.040 Uiso 1 1 d R . . H210 H 0.1216 0.1755 0.7134 0.040 Uiso 1 1 d R . . O11W O 0.8008(3) 0.0299(3) 1.2507(3) 0.0247(8) Uani 1 1 d . . . H111 H 0.8531 0.0522 1.2709 0.037 Uiso 1 1 d R . . H211 H 0.8058 0.0451 1.1975 0.037 Uiso 1 1 d R . . O12W O 0.1346(5) 0.4686(4) 1.5576(4) 0.0641(15) Uani 1 1 d . . . H112 H 0.0659 0.4514 1.5785 0.096 Uiso 1 1 d R . . H212 H 0.1204 0.5416 1.5205 0.096 Uiso 1 1 d R . . O13A O 0.4071(12) 0.5943(9) 1.4048(7) 0.048(4) Uani 0.408(11) 1 d P A 1 H13A H 0.3509 0.5595 1.4388 0.072 Uiso 0.408(11) 1 d PR A 1 H13B H 0.3826 0.6419 1.3664 0.072 Uiso 0.408(11) 1 d PR A 1 O13B O 0.5193(7) 0.6289(5) 1.3704(5) 0.030(2) Uani 0.592(11) 1 d P A 2 H13C H 0.5272 0.6740 1.3976 0.044 Uiso 0.592(11) 1 d PR A 2 H13D H 0.5087 0.6683 1.3146 0.044 Uiso 0.592(11) 1 d PR A 2 O14A O 0.0194(9) 0.5618(6) 0.7699(7) 0.054(4) Uani 0.573(12) 1 d P B 3 H14A H -0.0241 0.5549 0.7297 0.082 Uiso 0.573(12) 1 d PR B 3 H14B H -0.0052 0.5881 0.8008 0.082 Uiso 0.573(12) 1 d PR B 3 O14B O 0.1473(10) 0.5495(7) 0.7120(6) 0.031(3) Uani 0.427(12) 1 d P . 4 H14C H 0.1805 0.5988 0.6595 0.046 Uiso 0.427(12) 1 d PR B 4 H14D H 0.1158 0.5027 0.7013 0.046 Uiso 0.427(12) 1 d PR B 4 O15W O 0.7601(10) 0.4989(8) 1.3372(8) 0.057(3) Uani 0.50 1 d P . . H15A H 0.7553 0.5336 1.2949 0.085 Uiso 0.50 1 d PR . . H25B H 0.7327 0.5358 1.3870 0.085 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01836(14) 0.01290(12) 0.02098(14) -0.00105(10) -0.01130(10) -0.00399(9) O1W 0.025(2) 0.0199(19) 0.032(2) -0.0043(16) -0.0067(17) -0.0010(16) O2W 0.020(2) 0.064(3) 0.027(2) -0.020(2) -0.0075(17) -0.002(2) O3W 0.029(2) 0.023(2) 0.024(2) -0.0029(16) -0.0093(16) -0.0112(16) O4W 0.053(3) 0.0137(19) 0.036(2) -0.0016(16) -0.028(2) 0.0031(18) Gd2 0.02183(14) 0.01327(13) 0.02001(14) -0.00094(10) -0.01230(10) -0.00244(10) O5W 0.059(3) 0.051(3) 0.068(3) -0.036(3) -0.045(3) 0.035(3) O6W 0.023(2) 0.038(2) 0.028(2) 0.0049(18) -0.0083(17) -0.0096(18) O7W 0.100(4) 0.018(2) 0.116(5) -0.009(3) -0.095(4) 0.002(2) O8W 0.023(2) 0.058(3) 0.019(2) -0.0052(19) -0.0096(16) -0.0019(19) O9W 0.023(2) 0.031(2) 0.034(2) -0.0171(18) -0.0013(17) -0.0090(17) Cu1 0.0211(3) 0.0165(3) 0.0189(3) -0.0013(2) -0.0080(3) -0.0055(2) O1A 0.035(2) 0.020(2) 0.040(2) -0.0032(17) -0.0165(19) -0.0049(17) O2A 0.025(2) 0.021(2) 0.030(2) -0.0001(16) -0.0132(17) -0.0048(16) O3A 0.0203(19) 0.025(2) 0.027(2) -0.0054(16) -0.0115(16) -0.0084(15) O4A 0.032(2) 0.0170(19) 0.029(2) 0.0055(16) -0.0169(17) -0.0051(16) O5A 0.023(2) 0.0213(19) 0.026(2) -0.0046(15) -0.0106(16) -0.0057(15) O6A 0.021(2) 0.0230(19) 0.028(2) -0.0057(16) -0.0104(16) -0.0059(15) N1A 0.023(2) 0.017(2) 0.025(2) -0.0045(18) -0.0099(19) -0.0019(18) N2A 0.020(2) 0.021(2) 0.022(2) -0.0033(18) -0.0089(18) -0.0028(18) C1A 0.025(3) 0.026(3) 0.025(3) -0.007(2) -0.007(2) -0.006(2) C2A 0.025(3) 0.023(3) 0.035(3) -0.004(2) -0.012(2) -0.008(2) C3A 0.018(3) 0.022(3) 0.018(3) -0.007(2) -0.002(2) 0.000(2) C4A 0.022(3) 0.014(2) 0.027(3) -0.003(2) -0.011(2) -0.003(2) C5A 0.025(3) 0.020(3) 0.019(3) -0.007(2) -0.007(2) 0.001(2) C6A 0.022(3) 0.024(3) 0.026(3) -0.006(2) -0.010(2) -0.006(2) C7A 0.025(3) 0.021(3) 0.020(3) -0.007(2) -0.007(2) -0.006(2) Cu2 0.0228(3) 0.0143(3) 0.0185(3) -0.0003(2) -0.0107(3) -0.0065(2) O1B 0.030(2) 0.0175(18) 0.0233(19) -0.0009(15) -0.0146(16) -0.0042(16) O2B 0.036(2) 0.019(2) 0.028(2) -0.0028(16) -0.0153(18) 0.0003(17) O3B 0.024(2) 0.023(2) 0.037(2) -0.0040(17) -0.0174(17) -0.0084(16) O4B 0.038(2) 0.036(2) 0.037(2) 0.0131(19) -0.024(2) -0.012(2) O5B 0.029(2) 0.022(2) 0.028(2) -0.0030(16) -0.0141(17) -0.0063(16) O6B 0.040(2) 0.0200(19) 0.027(2) -0.0040(16) -0.0118(18) -0.0143(17) N1B 0.022(2) 0.021(2) 0.021(2) 0.0010(18) -0.0113(19) -0.0092(18) N2B 0.022(2) 0.016(2) 0.027(2) -0.0006(18) -0.0076(19) -0.0059(18) C1B 0.023(3) 0.021(3) 0.017(3) -0.006(2) -0.005(2) -0.003(2) C2B 0.025(3) 0.015(2) 0.019(3) -0.005(2) -0.003(2) -0.006(2) C3B 0.017(3) 0.023(3) 0.022(3) -0.007(2) -0.001(2) -0.005(2) C4B 0.023(3) 0.026(3) 0.027(3) -0.004(2) -0.013(2) 0.001(2) C5B 0.022(3) 0.025(3) 0.022(3) 0.000(2) -0.011(2) 0.001(2) C6B 0.027(3) 0.019(3) 0.029(3) -0.002(2) -0.009(2) -0.009(2) C7B 0.025(3) 0.020(3) 0.022(3) -0.006(2) -0.005(2) -0.003(2) Cu3 0.0173(3) 0.0234(3) 0.0205(3) -0.0033(3) -0.0088(3) -0.0044(3) O1C 0.025(2) 0.027(2) 0.026(2) -0.0064(16) -0.0137(16) -0.0028(16) O2C 0.022(2) 0.038(2) 0.025(2) -0.0014(17) -0.0108(17) -0.0003(17) O3C 0.0173(19) 0.0183(19) 0.036(2) -0.0014(16) -0.0120(16) -0.0030(15) O4C 0.0197(19) 0.0220(19) 0.028(2) 0.0000(16) -0.0134(16) -0.0031(15) O5C 0.030(2) 0.033(2) 0.026(2) -0.0028(17) -0.0150(17) -0.0128(18) O6C 0.055(3) 0.036(3) 0.042(3) 0.001(2) -0.023(2) -0.026(2) N1C 0.021(2) 0.019(2) 0.023(2) 0.0006(18) -0.0116(19) -0.0025(18) N2C 0.022(2) 0.022(2) 0.019(2) -0.0004(18) -0.0090(18) -0.0066(18) C1C 0.022(3) 0.036(3) 0.015(3) -0.006(2) -0.009(2) 0.002(2) C2C 0.019(3) 0.026(3) 0.023(3) -0.002(2) -0.006(2) 0.000(2) C3C 0.014(3) 0.019(3) 0.021(3) -0.005(2) -0.003(2) -0.002(2) C4C 0.020(3) 0.023(3) 0.021(3) 0.000(2) -0.011(2) -0.004(2) C5C 0.018(3) 0.017(2) 0.015(2) -0.0012(19) -0.003(2) -0.005(2) C6C 0.033(3) 0.024(3) 0.019(3) -0.003(2) -0.007(2) -0.012(2) C7C 0.030(3) 0.035(3) 0.024(3) 0.001(2) -0.008(2) -0.019(3) O10W 0.022(2) 0.038(2) 0.021(2) -0.0099(17) -0.0037(16) -0.0070(17) O11W 0.025(2) 0.028(2) 0.025(2) -0.0086(16) -0.0089(16) -0.0042(16) O12W 0.053(3) 0.054(3) 0.077(4) -0.005(3) -0.011(3) -0.013(3) O13A 0.056(9) 0.044(7) 0.029(6) -0.001(5) -0.015(6) 0.025(6) O13B 0.038(5) 0.025(4) 0.031(4) -0.005(3) -0.016(3) -0.006(3) O14A 0.072(7) 0.022(4) 0.085(7) 0.007(4) -0.061(6) -0.010(4) O14B 0.040(7) 0.024(5) 0.026(5) 0.002(4) -0.007(5) -0.016(5) O15W 0.053(7) 0.047(6) 0.056(6) 0.011(5) -0.008(5) -0.018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O3A 2.295(3) . yes Gd1 O4A 2.327(3) 2_557 yes Gd1 O3B 2.331(4) 2_667 yes Gd1 O6B 2.394(4) . yes Gd1 O4W 2.417(4) . yes Gd1 O1W 2.431(4) . yes Gd1 O3W 2.449(4) . yes Gd1 O2W 2.457(4) . yes O1W H11W 0.8645 . ? O1W H21W 0.9362 . ? O2W H12W 0.9274 . ? O2W H22W 0.8754 . ? O3W H13W 0.8745 . ? O3W H23W 0.8475 . ? O4W H14W 0.9571 . ? O4W H24W 0.8916 . ? Gd2 O4B 2.259(4) . yes Gd2 O4C 2.323(3) 2_658 yes Gd2 O3C 2.351(3) . yes Gd2 O7W 2.402(4) . yes Gd2 O8W 2.404(4) . yes Gd2 O9W 2.409(4) . yes Gd2 O5W 2.430(4) . yes Gd2 O6W 2.510(4) . yes O5W H15W 1.0502 . ? O5W H25W 0.8665 . ? O6W H16W 0.8166 . ? O6W H26W 0.9744 . ? O7W H17W 0.9920 . ? O7W H27W 0.7954 . ? O8W H18W 0.9007 . ? O8W H28W 0.9956 . ? O9W H19W 0.9151 . ? O9W H29W 0.8814 . ? Cu1 N2A 1.905(4) . ? Cu1 N1A 1.907(4) . ? Cu1 O2A 1.929(4) . ? Cu1 O5A 1.952(3) . ? O1A C1A 1.239(6) . ? O2A C1A 1.285(6) . ? O3A C3A 1.277(6) . ? O4A C5A 1.269(6) . ? O4A Gd1 2.327(3) 2_557 ? O5A C7A 1.277(6) . ? O6A C7A 1.250(6) . ? N1A C3A 1.296(6) . ? N1A C2A 1.451(7) . ? N2A C5A 1.305(6) . ? N2A C6A 1.470(6) . ? C1A C2A 1.528(7) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3A C4A 1.517(7) . ? C4A C5A 1.517(7) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C6A C7A 1.513(7) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? Cu2 N2B 1.894(4) . ? Cu2 N1B 1.914(4) . ? Cu2 O1B 1.954(3) . ? Cu2 O5B 1.963(4) . ? O1B C1B 1.283(6) . ? O2B C1B 1.242(6) . ? O3B C3B 1.264(6) . ? O3B Gd1 2.331(4) 2_667 ? O4B C5B 1.274(6) . ? O5B C7B 1.283(6) . ? O6B C7B 1.240(6) . ? N1B C3B 1.307(6) . ? N1B C2B 1.454(6) . ? N2B C5B 1.314(7) . ? N2B C6B 1.441(6) . ? C1B C2B 1.515(7) . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C3B C4B 1.521(7) . ? C4B C5B 1.482(8) . ? C4B H4B1 0.9900 . ? C4B H4B2 0.9900 . ? C6B C7B 1.505(7) . ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? Cu3 N1C 1.897(4) . ? Cu3 N2C 1.906(4) . ? Cu3 O5C 1.951(4) . ? Cu3 O1C 1.961(4) . ? O1C C1C 1.278(7) . ? O2C C1C 1.249(6) . ? O3C C3C 1.267(6) . ? O4C C5C 1.272(6) . ? O4C Gd2 2.323(3) 2_658 ? O5C C7C 1.299(7) . ? O6C C7C 1.223(7) . ? N1C C3C 1.322(6) . ? N1C C2C 1.451(6) . ? N2C C5C 1.307(6) . ? N2C C6C 1.455(7) . ? C1C C2C 1.507(7) . ? C2C H2C1 0.9900 . ? C2C H2C2 0.9900 . ? C3C C4C 1.506(7) . ? C4C C5C 1.511(7) . ? C4C H4C1 0.9900 . ? C4C H4C2 0.9900 . ? C6C C7C 1.510(7) . ? C6C H6C1 0.9900 . ? C6C H6C2 0.9900 . ? O10W H110 0.8672 . ? O10W H210 0.8109 . ? O11W H111 0.8585 . ? O11W H211 0.7720 . ? O12W H112 0.7763 . ? O12W H212 0.9752 . ? O13A H13A 0.7967 . ? O13A H13B 0.7974 . ? O13B H13C 0.8446 . ? O13B H13D 0.8950 . ? O14A H14A 0.9208 . ? O14A H14B 0.6363 . ? O14B O15W 1.268(14) 2_667 ? O14B H14C 0.8994 . ? O14B H14D 0.8326 . ? O15W O14B 1.268(14) 2_667 ? O15W H15A 0.6898 . ? O15W H25B 0.9685 . ? 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 O3A Gd1 O4A 99.59(13) . 2_557 ? O3A Gd1 O3B 146.03(13) . 2_667 ? O4A Gd1 O3B 94.83(13) 2_557 2_667 ? O3A Gd1 O6B 138.94(14) . . ? O4A Gd1 O6B 75.81(13) 2_557 . ? O3B Gd1 O6B 74.45(13) 2_667 . ? O3A Gd1 O4W 96.16(13) . . ? O4A Gd1 O4W 145.27(14) 2_557 . ? O3B Gd1 O4W 88.94(14) 2_667 . ? O6B Gd1 O4W 72.01(13) . . ? O3A Gd1 O1W 80.35(13) . . ? O4A Gd1 O1W 72.79(13) 2_557 . ? O3B Gd1 O1W 74.81(13) 2_667 . ? O6B Gd1 O1W 133.37(13) . . ? O4W Gd1 O1W 140.78(14) . . ? O3A Gd1 O3W 74.26(12) . . ? O4A Gd1 O3W 142.73(13) 2_557 . ? O3B Gd1 O3W 75.66(12) 2_667 . ? O6B Gd1 O3W 132.62(12) . . ? O4W Gd1 O3W 71.53(13) . . ? O1W Gd1 O3W 69.94(12) . . ? O3A Gd1 O2W 69.85(13) . . ? O4A Gd1 O2W 77.05(14) 2_557 . ? O3B Gd1 O2W 143.82(13) 2_667 . ? O6B Gd1 O2W 69.37(13) . . ? O4W Gd1 O2W 79.69(15) . . ? O1W Gd1 O2W 132.83(14) . . ? O3W Gd1 O2W 130.60(13) . . ? Gd1 O1W H11W 117.0 . . ? Gd1 O1W H21W 132.5 . . ? H11W O1W H21W 101.4 . . ? Gd1 O2W H12W 117.7 . . ? Gd1 O2W H22W 137.9 . . ? H12W O2W H22W 98.6 . . ? Gd1 O3W H13W 137.2 . . ? Gd1 O3W H23W 115.5 . . ? H13W O3W H23W 99.6 . . ? Gd1 O4W H14W 126.8 . . ? Gd1 O4W H24W 134.7 . . ? H14W O4W H24W 95.1 . . ? O4B Gd2 O4C 135.48(14) . 2_658 ? O4B Gd2 O3C 89.68(13) . . ? O4C Gd2 O3C 127.75(12) 2_658 . ? O4B Gd2 O7W 86.57(16) . . ? O4C Gd2 O7W 75.66(14) 2_658 . ? O3C Gd2 O7W 144.16(18) . . ? O4B Gd2 O8W 147.36(16) . . ? O4C Gd2 O8W 72.24(13) 2_658 . ? O3C Gd2 O8W 78.86(13) . . ? O7W Gd2 O8W 85.35(18) . . ? O4B Gd2 O9W 96.88(15) . . ? O4C Gd2 O9W 78.41(13) 2_658 . ? O3C Gd2 O9W 69.92(13) . . ? O7W Gd2 O9W 145.91(17) . . ? O8W Gd2 O9W 107.36(14) . . ? O4B Gd2 O5W 71.67(17) . . ? O4C Gd2 O5W 135.28(14) 2_658 . ? O3C Gd2 O5W 73.67(15) . . ? O7W Gd2 O5W 71.33(18) . . ? O8W Gd2 O5W 75.78(16) . . ? O9W Gd2 O5W 141.85(14) . . ? O4B Gd2 O6W 67.81(14) . . ? O4C Gd2 O6W 68.79(13) 2_658 . ? O3C Gd2 O6W 132.09(13) . . ? O7W Gd2 O6W 78.61(19) . . ? O8W Gd2 O6W 140.40(12) . . ? O9W Gd2 O6W 71.56(13) . . ? O5W Gd2 O6W 130.29(17) . . ? Gd2 O5W H15W 139.5 . . ? Gd2 O5W H25W 113.8 . . ? H15W O5W H25W 101.6 . . ? Gd2 O6W H16W 117.3 . . ? Gd2 O6W H26W 129.8 . . ? H16W O6W H26W 110.3 . . ? Gd2 O7W H17W 114.8 . . ? Gd2 O7W H27W 129.7 . . ? H17W O7W H27W 95.8 . . ? Gd2 O8W H18W 108.9 . . ? Gd2 O8W H28W 142.5 . . ? H18W O8W H28W 98.9 . . ? Gd2 O9W H19W 125.6 . . ? Gd2 O9W H29W 115.6 . . ? H19W O9W H29W 101.5 . . ? N2A Cu1 N1A 97.15(18) . . ? N2A Cu1 O2A 175.90(17) . . ? N1A Cu1 O2A 86.07(16) . . ? N2A Cu1 O5A 84.77(16) . . ? N1A Cu1 O5A 178.04(17) . . ? O2A Cu1 O5A 92.02(15) . . ? C1A O2A Cu1 114.6(3) . . ? C3A O3A Gd1 172.5(3) . . ? C5A O4A Gd1 147.4(3) . 2_557 ? C7A O5A Cu1 114.2(3) . . ? C3A N1A C2A 120.0(4) . . ? C3A N1A Cu1 127.2(4) . . ? C2A N1A Cu1 112.2(3) . . ? C5A N2A C6A 117.8(4) . . ? C5A N2A Cu1 128.0(4) . . ? C6A N2A Cu1 113.6(3) . . ? O1A C1A O2A 124.5(5) . . ? O1A C1A C2A 118.9(5) . . ? O2A C1A C2A 116.7(5) . . ? N1A C2A C1A 110.3(4) . . ? N1A C2A H2A1 109.6 . . ? C1A C2A H2A1 109.6 . . ? N1A C2A H2A2 109.6 . . ? C1A C2A H2A2 109.6 . . ? H2A1 C2A H2A2 108.1 . . ? O3A C3A N1A 123.5(5) . . ? O3A C3A C4A 115.7(4) . . ? N1A C3A C4A 120.8(4) . . ? C3A C4A C5A 125.9(4) . . ? C3A C4A H4A1 105.9 . . ? C5A C4A H4A1 105.9 . . ? C3A C4A H4A2 105.9 . . ? C5A C4A H4A2 105.9 . . ? H4A1 C4A H4A2 106.2 . . ? O4A C5A N2A 123.7(5) . . ? O4A C5A C4A 116.9(4) . . ? N2A C5A C4A 119.4(5) . . ? N2A C6A C7A 108.2(4) . . ? N2A C6A H6A1 110.1 . . ? C7A C6A H6A1 110.1 . . ? N2A C6A H6A2 110.1 . . ? C7A C6A H6A2 110.1 . . ? H6A1 C6A H6A2 108.4 . . ? O6A C7A O5A 123.0(5) . . ? O6A C7A C6A 118.6(4) . . ? O5A C7A C6A 118.3(4) . . ? N2B Cu2 N1B 95.49(18) . . ? N2B Cu2 O1B 176.64(18) . . ? N1B Cu2 O1B 85.41(16) . . ? N2B Cu2 O5B 84.81(16) . . ? N1B Cu2 O5B 178.55(19) . . ? O1B Cu2 O5B 94.21(15) . . ? C1B O1B Cu2 113.1(3) . . ? C3B O3B Gd1 146.2(4) . 2_667 ? C5B O4B Gd2 163.4(4) . . ? C7B O5B Cu2 113.2(3) . . ? C7B O6B Gd1 138.2(3) . . ? C3B N1B C2B 118.3(4) . . ? C3B N1B Cu2 128.1(4) . . ? C2B N1B Cu2 112.8(3) . . ? C5B N2B C6B 116.7(4) . . ? C5B N2B Cu2 127.4(4) . . ? C6B N2B Cu2 113.4(3) . . ? O2B C1B O1B 122.5(5) . . ? O2B C1B C2B 119.5(4) . . ? O1B C1B C2B 118.0(4) . . ? N1B C2B C1B 109.1(4) . . ? N1B C2B H2B1 109.9 . . ? C1B C2B H2B1 109.9 . . ? N1B C2B H2B2 109.9 . . ? C1B C2B H2B2 109.9 . . ? H2B1 C2B H2B2 108.3 . . ? O3B C3B N1B 123.8(5) . . ? O3B C3B C4B 115.9(4) . . ? N1B C3B C4B 120.2(4) . . ? C5B C4B C3B 123.6(4) . . ? C5B C4B H4B1 106.4 . . ? C3B C4B H4B1 106.4 . . ? C5B C4B H4B2 106.4 . . ? C3B C4B H4B2 106.4 . . ? H4B1 C4B H4B2 106.5 . . ? O4B C5B N2B 119.6(5) . . ? O4B C5B C4B 118.1(5) . . ? N2B C5B C4B 122.3(5) . . ? N2B C6B C7B 109.3(4) . . ? N2B C6B H6B1 109.8 . . ? C7B C6B H6B1 109.8 . . ? N2B C6B H6B2 109.8 . . ? C7B C6B H6B2 109.8 . . ? H6B1 C6B H6B2 108.3 . . ? O6B C7B O5B 124.7(5) . . ? O6B C7B C6B 117.6(5) . . ? O5B C7B C6B 117.7(4) . . ? N1C Cu3 N2C 95.55(18) . . ? N1C Cu3 O5C 175.60(19) . . ? N2C Cu3 O5C 85.04(17) . . ? N1C Cu3 O1C 84.60(16) . . ? N2C Cu3 O1C 179.53(18) . . ? O5C Cu3 O1C 94.84(15) . . ? C1C O1C Cu3 113.8(3) . . ? C3C O3C Gd2 149.3(3) . . ? C5C O4C Gd2 155.0(3) . 2_658 ? C7C O5C Cu3 114.4(3) . . ? C3C N1C C2C 116.5(4) . . ? C3C N1C Cu3 128.9(4) . . ? C2C N1C Cu3 113.6(3) . . ? C5C N2C C6C 118.0(4) . . ? C5C N2C Cu3 128.1(4) . . ? C6C N2C Cu3 113.4(3) . . ? O2C C1C O1C 123.3(5) . . ? O2C C1C C2C 119.3(5) . . ? O1C C1C C2C 117.4(4) . . ? N1C C2C C1C 109.1(4) . . ? N1C C2C H2C1 109.9 . . ? C1C C2C H2C1 109.9 . . ? N1C C2C H2C2 109.9 . . ? C1C C2C H2C2 109.9 . . ? H2C1 C2C H2C2 108.3 . . ? O3C C3C N1C 122.7(5) . . ? O3C C3C C4C 117.7(4) . . ? N1C C3C C4C 119.5(4) . . ? C3C C4C C5C 123.2(4) . . ? C3C C4C H4C1 106.5 . . ? C5C C4C H4C1 106.5 . . ? C3C C4C H4C2 106.5 . . ? C5C C4C H4C2 106.5 . . ? H4C1 C4C H4C2 106.5 . . ? O4C C5C N2C 122.0(5) . . ? O4C C5C C4C 116.6(4) . . ? N2C C5C C4C 121.4(4) . . ? N2C C6C C7C 110.1(4) . . ? N2C C6C H6C1 109.6 . . ? C7C C6C H6C1 109.6 . . ? N2C C6C H6C2 109.6 . . ? C7C C6C H6C2 109.6 . . ? H6C1 C6C H6C2 108.2 . . ? O6C C7C O5C 123.4(5) . . ? O6C C7C C6C 119.8(5) . . ? O5C C7C C6C 116.8(5) . . ? H110 O10W H210 109.1 . . ? H111 O11W H211 120.0 . . ? H112 O12W H212 102.2 . . ? H13A O13A H13B 111.4 . . ? H13C O13B H13D 104.6 . . ? H14A O14A H14B 122.2 . . ? O15W O14B H14C 73.2 2_667 . ? O15W O14B H14D 74.6 2_667 . ? H14C O14B H14D 112.9 . . ? O14B O15W H15A 85.3 2_667 . ? O14B O15W H25B 146.2 2_667 . ? H15A O15W H25B 110.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1W H11W O6A 0.86 2.29 3.016(5) 141.1 1_655 yes O2W H12W O2C 0.93 1.95 2.812(5) 153.3 . yes O2W H22W O1B 0.88 2.10 2.969(5) 171.6 2_567 yes O3W H13W O10W 0.87 1.94 2.761(5) 155.8 . yes O4W H14W O5B 0.96 2.14 2.847(5) 129.2 . yes O5W H15W O1A 1.05 1.85 2.826(6) 152.5 2_567 yes O5W H25W O12W 0.87 2.07 2.710(8) 129.6 . yes O6W H26W O2C 0.97 1.81 2.764(5) 167.3 1_655 yes O7W H17W O13A 0.99 1.95 2.927(12) 167.0 2_668 yes O7W H17W O13B 0.99 2.22 3.121(9) 150.3 2_668 yes O7W H27W O15W 0.80 1.65 2.449(11) 176.9 . yes O8W H18W O10W 0.90 2.05 2.712(5) 128.9 1_556 yes O8W H28W O6A 1.00 1.84 2.821(5) 168.0 1_656 yes O9W H19W O6A 0.92 2.00 2.788(5) 143.9 2_557 yes O9W H29W O11W 0.88 2.06 2.707(5) 129.7 . yes O9W H29W O6W 0.88 2.56 2.877(5) 102.2 . yes O10W H110 O5C 0.87 2.14 2.769(5) 128.7 2_557 yes O11W H111 O1C 0.86 1.87 2.708(5) 164.0 1_655 yes O11W H211 O2B 0.77 2.01 2.700(5) 148.3 2_667 yes O12W H112 O6C 0.78 2.24 2.772(7) 126.2 2_558 yes O12W H212 O6C 0.98 1.89 2.801(7) 153.8 1_565 yes O13A H13A O5W 0.80 2.46 2.991(15) 124.9 . yes O13A H13B O5A 0.80 2.09 2.823(11) 152.3 2_567 yes O13A H13B O2A 0.80 2.22 2.773(12) 126.7 2_567 yes O13B H13C O8W 0.84 2.25 3.089(8) 169.8 2_668 yes O13B H13D O5A 0.89 2.17 2.791(7) 126.0 2_567 yes O14A H14A O1A 0.92 1.88 2.737(8) 154.6 . yes O14B H14D O12W 0.83 2.32 2.916(11) 128.5 1_554 yes O15W H15A O3W 0.69 2.19 2.740(10) 138.5 2_667 yes _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.984 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.162