data_global _publ_contact_author_email marius.andruh@dnt.ro _publ_contact_author_name 'Prof Marius Andruh' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author 'Prof Marius Andruh' _publ_contact_author_address ; University of Bucharest, Faculty of Chemistry, Inorganic Chemistry Laboratory, Str. Dumbrava Rosie 23, 70254-Bucharest, Romania ; #============================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; A rational synthetic route leading to 3d - 3d' - 4f heterospin systems: self-assembly processes involving heterobinuclear 3d - 4f complexes and hexacyanometallates ; #============================================================================== _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. and Camalli, M. (1994)., SIR92 program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. DIFABS - N. Walker and D. Stuart, Acta Crystallogr., Sect A 1983, 39, 158-166. Farrugia, L. J., ORTEP3 for Windows, J. Appl. Crystallogr. 1997, 30, 565. Flack H D (1983), Acta Cryst. A39, 876-881 Sheldrick, G. M. (1997). SHELXL97. Program for the refinement of Crystal Structures. University of G\"ottingen, Germany. Crysalis Red, Data Reduction for Kappa CCD XCALIBUR, Oxford Diffraction Version 1.170 14 release 25 11 2002 Stoe, X-RED, Data Reduction for STADI4 and IPDS, Revision 1.08. Stoe & Cie, Darmstadt, 1996, Germany. WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; loop_ _publ_author_name 'Marius Andruh' 'Bruno Bonnadieu' 'Jean-pierre Costes' #**************************************************************************** data_(1) _database_code_CSD 216452 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H20 Cu Fe Gd N8 O11' _chemical_formula_weight 885.13 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' Fe Fe 0.3463 0.8444 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.0095(6) _cell_length_b 14.9900(8) _cell_length_c 16.9710(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3309.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 3.116 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.264 _exptl_absorpt_correction_T_max 0.833 _exptl_special_details ; The data were collected on a Oxford Diffraction four circles Kappa CCD XCalibur. The crystal-to-detector distance was 50 mm. 936 frames (27 sec per frame) were obtained using phi, omegan scan techniques. Coverage of the unique set was over 99.1% complete to at least 23.21\%. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'KappaCCD Xcalibur' _diffrn_measurement_method 'omega, phi scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 27 _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 39578 _diffrn_reflns_av_R_equivalents 0.1060 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 23.21 _reflns_number_total 4719 _reflns_number_gt 4542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis Red, Vers 1.170 14 release 25 11 2002' _computing_data_reduction 'Crysalis Red, Vers 1.170 14 release 25 11 2002' _computing_cell_refinement 'Crysalis Red, Vers 1.170 14 release 25 11 2002' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _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^)+(0.0353P)^2^+3.7986P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.024(11) _refine_ls_number_reflns 4719 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0688 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Cu1 Cu 0.20546(4) -0.05184(4) 0.90805(4) 0.01756(15) Uani 1 1 d . . . Gd1 Gd 0.414075(17) 0.096404(15) 0.911816(15) 0.01540(9) Uani 1 1 d . . . Fe1 Fe 0.83700(5) 0.10053(5) 0.90667(4) 0.01468(16) Uani 1 1 d . . . N1 N 0.1348(3) -0.1139(3) 0.8207(3) 0.0197(11) Uani 1 1 d . . . N2 N 0.1261(3) -0.1102(3) 0.9930(3) 0.0199(10) Uani 1 1 d . . . N3 N 0.6022(3) 0.1266(3) 0.9170(3) 0.0228(10) Uani 1 1 d . . . N4 N 0.8164(4) 0.0147(3) 1.0712(3) 0.0315(13) Uani 1 1 d . . . N5 N 0.8915(4) 0.2749(3) 0.9940(3) 0.0266(12) Uani 1 1 d . . . N6 N 1.0716(3) 0.0675(3) 0.8997(3) 0.0250(11) Uani 1 1 d . . . N7 N 0.8439(4) 0.1725(4) 0.7369(3) 0.0376(13) Uani 1 1 d . . . N8 N 0.7837(4) -0.0768(4) 0.8229(3) 0.0354(13) Uani 1 1 d . . . O1 O 0.3066(3) 0.0008(3) 0.8352(2) 0.0163(8) Uani 1 1 d . . . O2 O 0.2982(3) 0.0070(2) 0.9862(2) 0.0174(8) Uani 1 1 d . . . O3 O 0.4731(3) 0.0649(3) 0.7702(2) 0.0224(9) Uani 1 1 d . . . O4 O 0.4698(3) 0.0580(3) 1.0522(2) 0.0245(9) Uani 1 1 d . . . C1 C 0.0274(4) -0.1466(4) 0.8315(4) 0.0286(15) Uani 1 1 d . . . H1A H 0.0091 -0.1854 0.7864 0.034 Uiso 1 1 calc R . . H1B H -0.0199 -0.0949 0.8312 0.034 Uiso 1 1 calc R . . C2 C 0.0124(4) -0.1980(4) 0.9066(4) 0.0263(12) Uani 1 1 d . . . H2A H 0.0642 -0.2462 0.9091 0.032 Uiso 1 1 calc R . . H2B H -0.0564 -0.2263 0.9055 0.032 Uiso 1 1 calc R . . C3 C 0.0210(4) -0.1420(4) 0.9798(4) 0.0266(14) Uani 1 1 d . . . H3A H -0.0257 -0.0901 0.9752 0.032 Uiso 1 1 calc R . . H3B H -0.0014 -0.1777 1.0258 0.032 Uiso 1 1 calc R . . C4 C 0.1642(5) -0.1261(4) 1.0616(3) 0.0252(14) Uani 1 1 d . . . H4 H 0.1228 -0.1598 1.0968 0.030 Uiso 1 1 calc R . . C5 C 0.2643(4) -0.0977(4) 1.0908(3) 0.0199(11) Uani 1 1 d . . . C6 C 0.2967(5) -0.1362(4) 1.1622(4) 0.0303(15) Uani 1 1 d . . . H6 H 0.2546 -0.1792 1.1876 0.036 Uiso 1 1 calc R . . C7 C 0.3890(5) -0.1122(4) 1.1954(3) 0.0325(15) Uani 1 1 d . . . H7 H 0.4108 -0.1391 1.2432 0.039 Uiso 1 1 calc R . . C8 C 0.4503(5) -0.0487(4) 1.1592(3) 0.0290(15) Uani 1 1 d . . . H8 H 0.5148 -0.0328 1.1814 0.035 Uiso 1 1 calc R . . C9 C 0.4166(4) -0.0083(3) 1.0897(3) 0.0219(11) Uani 1 1 d . . . C10 C 0.3240(4) -0.0323(4) 1.0537(3) 0.0195(12) Uani 1 1 d . . . C11 C 0.3317(4) -0.0317(3) 0.7655(3) 0.0166(12) Uani 1 1 d . . . C12 C 0.4221(4) -0.0016(3) 0.7292(3) 0.0191(12) Uani 1 1 d . . . C13 C 0.4545(4) -0.0340(4) 0.6570(3) 0.0232(13) Uani 1 1 d . . . H13 H 0.5166 -0.0127 0.6344 0.028 Uiso 1 1 calc R . . C14 C 0.3957(4) -0.0982(4) 0.6172(3) 0.0252(13) Uani 1 1 d . . . H14 H 0.4181 -0.1217 0.5681 0.030 Uiso 1 1 calc R . . C15 C 0.3051(5) -0.1265(4) 0.6503(3) 0.0255(14) Uani 1 1 d . . . H15 H 0.2636 -0.1682 0.6226 0.031 Uiso 1 1 calc R . . C16 C 0.2723(4) -0.0952(4) 0.7245(3) 0.0188(11) Uani 1 1 d . . . C17 C 0.1737(4) -0.1257(4) 0.7531(3) 0.0195(13) Uani 1 1 d . . . H17 H 0.1331 -0.1586 0.7167 0.023 Uiso 1 1 calc R . . C18 C 0.5547(4) 0.0980(5) 1.0942(4) 0.0325(14) Uani 1 1 d . . . H18A H 0.6116 0.0553 1.0973 0.049 Uiso 1 1 calc R . . H18B H 0.5326 0.1141 1.1475 0.049 Uiso 1 1 calc R . . H18C H 0.5776 0.1517 1.0662 0.049 Uiso 1 1 calc R . . C19 C 0.5645(4) 0.0995(5) 0.7327(3) 0.0293(14) Uani 1 1 d . . . H19A H 0.5468 0.1227 0.6804 0.044 Uiso 1 1 calc R . . H19B H 0.6153 0.0517 0.7274 0.044 Uiso 1 1 calc R . . H19C H 0.5932 0.1477 0.7649 0.044 Uiso 1 1 calc R . . C20 C 0.6897(4) 0.1204(3) 0.9130(4) 0.0174(11) Uani 1 1 d . . . C21 C 0.8265(4) 0.0463(4) 1.0091(3) 0.0195(12) Uani 1 1 d . . . C22 C 0.8699(4) 0.2116(4) 0.9587(3) 0.0196(12) Uani 1 1 d . . . C23 C 0.9850(4) 0.0810(3) 0.9025(3) 0.0128(10) Uani 1 1 d . . . C24 C 0.8419(4) 0.1495(4) 0.8011(4) 0.0243(13) Uani 1 1 d . . . C25 C 0.8052(4) -0.0120(4) 0.8546(4) 0.0231(13) Uani 1 1 d . . . O4W O 0.7778(3) 0.1595(3) 1.1814(3) 0.0330(10) Uani 1 1 d . . . O1W O 0.4491(3) 0.2364(3) 0.8370(2) 0.0279(9) Uani 1 1 d . . . O2W O 0.4901(3) -0.0511(2) 0.9118(3) 0.0285(8) Uani 1 1 d . . . O3W O 0.2537(3) 0.1709(3) 0.8802(3) 0.0345(11) Uani 1 1 d . . . O5W O 0.7536(3) 0.1618(3) 0.5912(3) 0.0451(11) Uani 1 1 d . . . O6W O 0.6504(3) -0.1590(3) 0.9433(3) 0.0467(13) Uani 1 1 d . . . O7W O 0.6444(5) 0.3083(4) 0.5952(8) 0.147(4) 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 0.0142(3) 0.0184(3) 0.0200(3) -0.0021(3) 0.0002(3) -0.0038(2) Gd1 0.00930(13) 0.01561(13) 0.02130(14) -0.00258(13) -0.00036(11) 0.00026(9) Fe1 0.0084(3) 0.0157(3) 0.0199(4) -0.0037(4) 0.0000(3) -0.0004(3) N1 0.012(2) 0.018(3) 0.029(3) -0.002(2) -0.0041(19) -0.0020(19) N2 0.018(2) 0.015(2) 0.027(3) -0.001(2) 0.0013(19) 0.001(2) N3 0.012(2) 0.027(2) 0.029(3) -0.001(2) -0.004(2) -0.0058(17) N4 0.028(3) 0.034(3) 0.032(4) 0.005(3) -0.005(2) 0.001(2) N5 0.026(3) 0.027(3) 0.027(3) -0.005(2) -0.002(2) -0.002(2) N6 0.013(2) 0.030(3) 0.032(3) -0.003(2) 0.003(2) 0.0046(18) N7 0.057(4) 0.035(3) 0.022(3) 0.002(3) 0.006(3) 0.001(3) N8 0.033(3) 0.029(3) 0.044(3) -0.013(3) -0.008(2) 0.003(2) O1 0.0141(19) 0.024(2) 0.011(2) -0.0023(16) 0.0022(14) -0.0026(15) O2 0.0170(19) 0.017(2) 0.018(2) 0.0014(16) 0.0002(15) 0.0051(15) O3 0.020(2) 0.027(2) 0.021(2) -0.0006(18) 0.0045(16) -0.0075(16) O4 0.019(2) 0.027(2) 0.028(2) -0.0054(19) -0.0085(17) -0.0032(17) C1 0.012(3) 0.033(4) 0.040(4) -0.013(3) -0.002(2) -0.006(3) C2 0.016(3) 0.024(3) 0.038(3) -0.005(3) -0.002(3) -0.005(2) C3 0.015(3) 0.025(3) 0.040(4) 0.000(3) 0.003(2) -0.008(3) C4 0.032(3) 0.017(3) 0.026(4) 0.000(2) 0.007(3) -0.006(2) C5 0.021(3) 0.022(3) 0.017(3) 0.005(4) 0.004(2) 0.007(2) C6 0.034(3) 0.026(3) 0.031(4) 0.001(3) 0.011(3) 0.008(3) C7 0.036(4) 0.040(4) 0.021(3) 0.006(3) -0.004(3) 0.014(3) C8 0.026(3) 0.033(4) 0.028(3) -0.003(3) -0.007(3) 0.013(3) C9 0.021(3) 0.022(3) 0.024(3) -0.002(3) 0.002(3) 0.007(2) C10 0.023(3) 0.024(3) 0.012(3) -0.005(2) -0.003(2) 0.004(3) C11 0.020(3) 0.011(3) 0.019(3) 0.000(2) -0.002(2) 0.005(2) C12 0.016(3) 0.020(3) 0.021(3) 0.003(2) -0.002(2) 0.003(2) C13 0.020(3) 0.029(3) 0.021(3) 0.003(3) 0.004(2) 0.008(3) C14 0.032(3) 0.021(3) 0.022(3) -0.005(3) 0.005(2) 0.005(3) C15 0.031(3) 0.026(3) 0.019(3) -0.003(3) -0.006(2) 0.008(2) C16 0.021(3) 0.012(3) 0.023(3) -0.002(3) -0.006(2) 0.005(3) C17 0.012(2) 0.019(3) 0.028(3) -0.005(2) -0.006(2) 0.003(2) C18 0.019(3) 0.051(4) 0.027(3) -0.006(4) -0.002(2) -0.009(3) C19 0.014(3) 0.047(4) 0.027(3) -0.002(3) 0.008(2) -0.008(3) C20 0.014(3) 0.016(3) 0.023(3) -0.002(3) -0.001(2) 0.0002(18) C21 0.010(2) 0.019(3) 0.030(4) -0.007(3) -0.003(2) 0.002(2) C22 0.014(2) 0.020(3) 0.024(3) 0.001(3) 0.000(2) 0.005(2) C23 0.014(3) 0.014(3) 0.010(3) 0.006(2) 0.003(2) 0.0008(18) C24 0.017(3) 0.025(3) 0.031(4) -0.003(3) -0.001(2) -0.002(2) C25 0.012(3) 0.028(4) 0.029(4) -0.001(3) -0.001(2) 0.000(2) O4W 0.033(2) 0.022(2) 0.045(3) 0.007(2) 0.0027(19) -0.0059(18) O1W 0.025(2) 0.021(2) 0.038(3) 0.0054(19) 0.0035(17) 0.0012(17) O2W 0.0237(19) 0.0217(19) 0.040(2) -0.001(2) 0.000(2) 0.0053(15) O3W 0.017(2) 0.020(2) 0.066(3) 0.001(2) -0.0109(18) -0.0001(16) O5W 0.047(3) 0.040(3) 0.048(3) 0.001(3) -0.005(3) -0.003(2) O6W 0.032(3) 0.040(3) 0.068(3) 0.012(2) -0.005(2) 0.004(2) O7W 0.071(5) 0.039(3) 0.330(13) -0.041(6) -0.065(7) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.971(4) . ? Cu1 N1 1.977(4) . ? Cu1 N2 1.978(4) . ? Cu1 O2 1.999(4) . ? Cu1 Gd1 3.5083(6) . ? Gd1 O2 2.379(4) . ? Gd1 O1 2.388(4) . ? Gd1 O2W 2.422(4) . ? Gd1 O3W 2.426(4) . ? Gd1 N3 2.491(4) . ? Gd1 O1W 2.495(4) . ? Gd1 N5 2.522(5) 4_457 ? Gd1 O4 2.555(4) . ? Gd1 O3 2.567(4) . ? Fe1 C21 1.924(6) . ? Fe1 C22 1.933(6) . ? Fe1 C24 1.938(7) . ? Fe1 C20 1.942(5) . ? Fe1 C23 1.948(5) . ? Fe1 C25 1.949(6) . ? N1 C17 1.267(7) . ? N1 C1 1.491(7) . ? N2 C4 1.286(7) . ? N2 C3 1.465(7) . ? N3 C20 1.144(6) . ? N4 C21 1.163(7) . ? N5 C22 1.157(7) . ? N5 Gd1 2.522(5) 4_557 ? N6 C23 1.146(6) . ? N7 C24 1.143(7) . ? N8 C25 1.145(8) . ? O1 C11 1.320(6) . ? O2 C10 1.332(7) . ? O3 C12 1.385(7) . ? O3 C19 1.445(6) . ? O4 C9 1.369(7) . ? O4 C18 1.445(7) . ? C1 C2 1.502(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.503(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.457(8) . ? C4 H4 0.9500 . ? C5 C10 1.400(8) . ? C5 C6 1.408(8) . ? C6 C7 1.375(9) . ? C6 H6 0.9500 . ? C7 C8 1.385(9) . ? C7 H7 0.9500 . ? C8 C9 1.396(8) . ? C8 H8 0.9500 . ? C9 C10 1.397(8) . ? C11 C12 1.402(8) . ? C11 C16 1.408(8) . ? C12 C13 1.384(8) . ? C13 C14 1.403(8) . ? C13 H13 0.9500 . ? C14 C15 1.373(8) . ? C14 H14 0.9500 . ? C15 C16 1.411(8) . ? C15 H15 0.9500 . ? C16 C17 1.446(8) . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 O1 Cu1 N1 91.62(17) . . ? O1 Cu1 N2 169.55(17) . . ? N1 Cu1 N2 95.49(17) . . ? O1 Cu1 O2 80.58(13) . . ? N1 Cu1 O2 170.47(17) . . ? N2 Cu1 O2 91.55(17) . . ? O1 Cu1 Gd1 40.65(10) . . ? N1 Cu1 Gd1 132.19(14) . . ? N2 Cu1 Gd1 132.14(13) . . ? O2 Cu1 Gd1 40.62(11) . . ? O2 Gd1 O1 65.17(11) . . ? O2 Gd1 O2W 75.20(12) . . ? O1 Gd1 O2W 72.01(13) . . ? O2 Gd1 O3W 80.31(13) . . ? O1 Gd1 O3W 69.62(13) . . ? O2W Gd1 O3W 140.43(13) . . ? O2 Gd1 N3 134.93(14) . . ? O1 Gd1 N3 134.75(14) . . ? O2W Gd1 N3 76.41(13) . . ? O3W Gd1 N3 140.28(14) . . ? O2 Gd1 O1W 149.25(12) . . ? O1 Gd1 O1W 109.55(13) . . ? O2W Gd1 O1W 133.90(13) . . ? O3W Gd1 O1W 69.97(13) . . ? N3 Gd1 O1W 71.66(14) . . ? O2 Gd1 N5 91.20(14) . 4_457 ? O1 Gd1 N5 137.39(14) . 4_457 ? O2W Gd1 N5 138.23(15) . 4_457 ? O3W Gd1 N5 71.84(14) . 4_457 ? N3 Gd1 N5 87.29(15) . 4_457 ? O1W Gd1 N5 72.55(15) . 4_457 ? O2 Gd1 O4 63.79(12) . . ? O1 Gd1 O4 122.61(12) . . ? O2W Gd1 O4 71.27(14) . . ? O3W Gd1 O4 123.62(14) . . ? N3 Gd1 O4 74.30(14) . . ? O1W Gd1 O4 127.72(13) . . ? N5 Gd1 O4 67.33(14) 4_457 . ? O2 Gd1 O3 125.64(12) . . ? O1 Gd1 O3 63.55(11) . . ? O2W Gd1 O3 73.13(14) . . ? O3W Gd1 O3 97.74(14) . . ? N3 Gd1 O3 76.86(14) . . ? O1W Gd1 O3 67.90(13) . . ? N5 Gd1 O3 140.24(14) 4_457 . ? O4 Gd1 O3 138.29(11) . . ? O2 Gd1 Cu1 33.16(9) . . ? O1 Gd1 Cu1 32.53(8) . . ? O2W Gd1 Cu1 74.78(9) . . ? O3W Gd1 Cu1 67.80(10) . . ? N3 Gd1 Cu1 151.17(10) . . ? O1W Gd1 Cu1 131.68(9) . . ? N5 Gd1 Cu1 113.96(11) 4_457 . ? O4 Gd1 Cu1 95.38(9) . . ? O3 Gd1 Cu1 95.61(8) . . ? C21 Fe1 C22 88.1(2) . . ? C21 Fe1 C24 176.5(2) . . ? C22 Fe1 C24 95.1(2) . . ? C21 Fe1 C20 86.8(2) . . ? C22 Fe1 C20 93.5(2) . . ? C24 Fe1 C20 91.5(2) . . ? C21 Fe1 C23 92.3(2) . . ? C22 Fe1 C23 85.9(2) . . ? C24 Fe1 C23 89.5(2) . . ? C20 Fe1 C23 178.9(2) . . ? C21 Fe1 C25 91.7(2) . . ? C22 Fe1 C25 179.4(2) . . ? C24 Fe1 C25 85.1(2) . . ? C20 Fe1 C25 87.0(2) . . ? C23 Fe1 C25 93.6(2) . . ? C17 N1 C1 116.1(5) . . ? C17 N1 Cu1 124.0(4) . . ? C1 N1 Cu1 119.9(4) . . ? C4 N2 C3 116.0(5) . . ? C4 N2 Cu1 122.7(4) . . ? C3 N2 Cu1 121.3(4) . . ? C20 N3 Gd1 163.9(4) . . ? C22 N5 Gd1 169.7(4) . 4_557 ? C11 O1 Cu1 125.4(3) . . ? C11 O1 Gd1 124.4(3) . . ? Cu1 O1 Gd1 106.81(15) . . ? C10 O2 Cu1 121.9(3) . . ? C10 O2 Gd1 123.1(3) . . ? Cu1 O2 Gd1 106.22(15) . . ? C12 O3 C19 115.6(4) . . ? C12 O3 Gd1 117.3(3) . . ? C19 O3 Gd1 126.3(3) . . ? C9 O4 C18 117.3(5) . . ? C9 O4 Gd1 117.0(3) . . ? C18 O4 Gd1 125.7(4) . . ? N1 C1 C2 113.3(5) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C1 C2 C3 113.9(5) . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2B 108.8 . . ? C3 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? N2 C3 C2 112.2(5) . . ? N2 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N2 C4 C5 126.7(5) . . ? N2 C4 H4 116.6 . . ? C5 C4 H4 116.6 . . ? C10 C5 C6 120.5(5) . . ? C10 C5 C4 123.2(5) . . ? C6 C5 C4 116.2(5) . . ? C7 C6 C5 120.5(6) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 120.1(6) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 119.4(6) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? O4 C9 C8 123.3(5) . . ? O4 C9 C10 114.7(5) . . ? C8 C9 C10 121.9(5) . . ? O2 C10 C9 118.7(5) . . ? O2 C10 C5 123.8(5) . . ? C9 C10 C5 117.5(5) . . ? O1 C11 C12 118.8(5) . . ? O1 C11 C16 123.8(5) . . ? C12 C11 C16 117.5(5) . . ? C13 C12 O3 123.4(5) . . ? C13 C12 C11 122.1(5) . . ? O3 C12 C11 114.5(5) . . ? C12 C13 C14 120.1(5) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 118.9(5) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 121.5(6) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C11 C16 C15 119.9(5) . . ? C11 C16 C17 122.4(5) . . ? C15 C16 C17 117.6(5) . . ? N1 C17 C16 127.9(5) . . ? N1 C17 H17 116.1 . . ? C16 C17 H17 116.1 . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O3 C19 H19A 109.5 . . ? O3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 Fe1 175.9(4) . . ? N4 C21 Fe1 177.5(5) . . ? N5 C22 Fe1 175.6(5) . . ? N6 C23 Fe1 178.5(5) . . ? N7 C24 Fe1 175.3(5) . . ? N8 C25 Fe1 177.8(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.21 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.044 _refine_diff_density_min -0.813 _refine_diff_density_rms 0.098 #====END data_(2) _database_code_CSD 216453 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H17 Co Cu Gd N8 O10.50' _chemical_formula_weight 877.19 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M ' P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.945(3) _cell_length_b 15.010(3) _cell_length_c 16.955(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3294.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1708 _exptl_absorpt_coefficient_mu 3.192 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.197 _exptl_absorpt_correction_T_max 0.666 _exptl_special_details ; The data were collected on a Oxford Diffraction four circles Kappa CCD XCalibur. The crystal-to-detector distance was 50 mm. 460 frames (40 sec per frame) were obtained using phi, omegan scan techniques. Coverage of the unique set was over 99.5% complete to at least 26.37\%. ; _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'KappaCCD Xcalibur' _diffrn_measurement_method 'omega, phi scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 27 _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 25146 _diffrn_reflns_av_R_equivalents 0.1117 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6719 _reflns_number_gt 5717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis Red, Vers 1.170 14 release 25 11 2002' _computing_data_reduction 'Crysalis Red, Vers 1.170 14 release 25 11 2002' _computing_cell_refinement 'Crysalis Red, Vers 1.170 14 release 25 11 2002' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _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^)+(0.0808P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.024(18) _refine_ls_number_reflns 6719 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.91311(3) 0.59808(3) 0.91271(2) 0.02196(12) Uani 1 1 d . . . Cu1 Cu 0.70484(6) 0.44838(7) 0.90901(7) 0.0238(2) Uani 1 1 d . . . Co1 Co 1.33530(7) 0.60032(7) 0.90845(6) 0.0200(2) Uani 1 1 d . . . N1 N 0.6262(5) 0.3909(5) 0.9941(4) 0.0255(15) Uani 1 1 d . . . N2 N 0.6329(5) 0.3863(5) 0.8219(4) 0.0219(15) Uani 1 1 d . . . N3 N 1.1027(5) 0.6284(5) 0.9173(5) 0.0299(15) Uani 1 1 d . . . N4 N 1.2834(6) 0.4255(6) 0.8252(5) 0.039(2) Uani 1 1 d . . . N5 N 1.3439(7) 0.6725(6) 0.7413(5) 0.042(2) Uani 1 1 d . . . N6 N 1.5679(5) 0.5669(5) 0.9007(4) 0.0285(16) Uani 1 1 d . . . N7 N 1.3883(6) 0.7727(5) 0.9927(5) 0.0349(18) Uani 1 1 d . . . N8 N 1.3152(6) 0.5170(5) 1.0698(5) 0.0356(19) Uani 1 1 d . . . O1 O 0.7970(4) 0.5077(4) 0.9864(3) 0.0236(13) Uani 1 1 d . . . O2 O 0.8044(4) 0.5031(4) 0.8367(3) 0.0247(13) Uani 1 1 d . . . O3 O 0.9691(4) 0.5604(4) 1.0536(4) 0.0280(13) Uani 1 1 d . . . O4 O 0.9730(4) 0.5663(4) 0.7714(4) 0.0284(13) Uani 1 1 d . . . O5 O 0.9900(4) 0.4513(4) 0.9131(4) 0.0324(13) Uani 1 1 d . . . C1 C 0.5200(7) 0.3580(7) 0.9811(5) 0.031(2) Uani 1 1 d . . . H1A H 0.4724 0.4093 0.9766 0.037 Uiso 1 1 calc R . . H1B H 0.4982 0.3220 1.0272 0.037 Uiso 1 1 calc R . . C2 C 0.5125(6) 0.3019(6) 0.9074(6) 0.0304(18) Uani 1 1 d . . . H2A H 0.5652 0.2543 0.9101 0.036 Uiso 1 1 calc R . . H2B H 0.4438 0.2729 0.9063 0.036 Uiso 1 1 calc R . . C3 C 0.5271(7) 0.3529(7) 0.8319(6) 0.033(2) Uani 1 1 d . . . H3A H 0.5097 0.3136 0.7869 0.039 Uiso 1 1 calc R . . H3B H 0.4786 0.4038 0.8311 0.039 Uiso 1 1 calc R . . C4 C 0.6730(6) 0.3751(6) 0.7544(5) 0.0257(19) Uani 1 1 d . . . H4 H 0.6322 0.3430 0.7175 0.031 Uiso 1 1 calc R . . C5 C 0.7729(6) 0.4047(6) 0.7260(5) 0.0247(16) Uani 1 1 d . . . C6 C 0.8067(7) 0.3721(7) 0.6513(5) 0.033(2) Uani 1 1 d . . . H6 H 0.7663 0.3292 0.6239 0.039 Uiso 1 1 calc R . . C7 C 0.8970(7) 0.4022(7) 0.6189(5) 0.035(2) Uani 1 1 d . . . H7 H 0.9199 0.3787 0.5699 0.042 Uiso 1 1 calc R . . C8 C 0.9561(7) 0.4675(7) 0.6574(5) 0.030(2) Uani 1 1 d . . . H8 H 1.0178 0.4893 0.6340 0.036 Uiso 1 1 calc R . . C9 C 0.9232(6) 0.5003(6) 0.7304(5) 0.0243(17) Uani 1 1 d . . . C10 C 0.8319(6) 0.4685(5) 0.7663(5) 0.0218(16) Uani 1 1 d . . . C11 C 0.8249(6) 0.4679(6) 1.0547(5) 0.0249(17) Uani 1 1 d . . . C12 C 0.9165(6) 0.4925(5) 1.0914(5) 0.0265(16) Uani 1 1 d . . . C13 C 0.9512(7) 0.4514(7) 1.1602(5) 0.032(2) Uani 1 1 d . . . H13 H 1.0162 0.4670 1.1822 0.038 Uiso 1 1 calc R . . C14 C 0.8911(8) 0.3888(8) 1.1954(5) 0.043(3) Uani 1 1 d . . . H14 H 0.9135 0.3613 1.2428 0.052 Uiso 1 1 calc R . . C15 C 0.7976(8) 0.3650(7) 1.1625(6) 0.034(2) Uani 1 1 d . . . H15 H 0.7552 0.3224 1.1883 0.041 Uiso 1 1 calc R . . C16 C 0.7647(5) 0.4025(6) 1.0921(5) 0.0257(16) Uani 1 1 d . . . C17 C 0.6642(7) 0.3737(6) 1.0624(6) 0.031(2) Uani 1 1 d . . . H17 H 0.6230 0.3388 1.0970 0.037 Uiso 1 1 calc R . . C18 C 1.0541(6) 0.6000(7) 1.0951(6) 0.037(2) Uani 1 1 d . . . H18A H 1.0345 0.6100 1.1503 0.055 Uiso 1 1 calc R . . H18B H 1.0719 0.6571 1.0705 0.055 Uiso 1 1 calc R . . H18C H 1.1139 0.5601 1.0930 0.055 Uiso 1 1 calc R . . C19 C 1.0674(6) 0.5988(8) 0.7330(5) 0.035(2) Uani 1 1 d . . . C20 C 1.1903(5) 0.6218(5) 0.9140(6) 0.0229(15) Uani 1 1 d . . . C21 C 1.3039(6) 0.4904(6) 0.8572(6) 0.0284(19) Uani 1 1 d . . . C22 C 1.3395(7) 0.6491(7) 0.8057(6) 0.034(2) Uani 1 1 d . . . C23 C 1.4821(5) 0.5823(5) 0.9047(4) 0.0181(15) Uani 1 1 d . . . C24 C 1.3659(6) 0.7094(6) 0.9579(5) 0.0276(18) Uani 1 1 d . . . C25 C 1.3249(6) 0.5478(6) 1.0092(5) 0.0236(17) Uani 1 1 d . . . O1W O 0.7502(5) 0.6713(5) 0.8806(4) 0.0399(17) Uani 1 1 d . . . O3W O 0.9470(5) 0.7377(4) 0.8381(4) 0.0337(15) Uani 1 1 d . . . O4W O 0.2755(5) 0.6588(5) 1.1819(4) 0.0397(16) Uani 1 1 d . . . O5W O 0.2551(5) 0.6611(5) 1.5936(5) 0.0450(16) Uani 1 1 d . . . O6W O 0.1515(5) 0.3406(5) 1.9451(5) 0.0503(19) Uani 1 1 d . . . O7W O 0.8529(8) 0.3132(7) 1.9159(14) 0.065(6) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01684(17) 0.0253(2) 0.02372(19) -0.00222(19) -0.00013(15) 0.00000(14) Cu1 0.0216(4) 0.0293(5) 0.0206(5) -0.0015(5) 0.0005(4) -0.0039(4) Co1 0.0155(4) 0.0225(5) 0.0222(5) -0.0032(6) -0.0006(4) -0.0005(4) N1 0.023(3) 0.019(4) 0.034(4) 0.000(3) 0.003(3) 0.001(3) N2 0.021(3) 0.022(4) 0.023(3) -0.003(3) -0.004(3) -0.001(3) N3 0.024(3) 0.031(4) 0.035(4) -0.007(3) 0.000(3) -0.011(3) N4 0.036(4) 0.034(5) 0.046(5) -0.009(4) -0.002(4) 0.001(3) N5 0.057(5) 0.039(5) 0.030(4) 0.002(4) -0.001(4) -0.009(4) N6 0.024(3) 0.035(4) 0.027(4) -0.007(3) 0.006(3) 0.004(3) N7 0.032(4) 0.034(5) 0.038(4) -0.006(4) -0.003(3) 0.003(3) N8 0.035(4) 0.033(4) 0.039(5) 0.002(4) -0.005(3) 0.002(3) O1 0.022(3) 0.026(3) 0.023(3) 0.000(2) 0.001(2) 0.000(2) O2 0.020(3) 0.043(4) 0.011(3) 0.001(2) 0.000(2) -0.003(2) O3 0.026(3) 0.031(3) 0.027(3) -0.002(3) -0.009(2) -0.001(3) O4 0.027(3) 0.030(3) 0.029(3) -0.003(3) 0.003(2) -0.009(2) O5 0.027(3) 0.029(3) 0.041(3) -0.001(3) -0.002(3) -0.001(2) C1 0.028(4) 0.032(5) 0.033(5) -0.003(4) 0.001(4) -0.007(4) C2 0.022(3) 0.032(5) 0.038(5) -0.013(5) -0.002(4) -0.005(3) C3 0.029(5) 0.031(5) 0.038(5) -0.006(4) -0.003(4) -0.005(4) C4 0.018(4) 0.033(5) 0.026(4) 0.000(4) -0.004(3) 0.000(3) C5 0.029(4) 0.019(4) 0.026(4) -0.004(4) -0.001(3) 0.000(4) C6 0.030(4) 0.050(6) 0.018(4) -0.009(4) -0.003(3) 0.005(4) C7 0.045(5) 0.043(5) 0.016(4) 0.004(4) 0.006(3) 0.014(5) C8 0.026(4) 0.037(5) 0.027(5) 0.003(4) 0.005(3) 0.007(4) C9 0.023(4) 0.030(5) 0.020(4) 0.001(3) 0.003(3) 0.003(3) C10 0.025(4) 0.021(4) 0.019(4) 0.000(3) -0.005(3) -0.003(3) C11 0.027(4) 0.029(5) 0.019(4) -0.005(3) 0.001(3) 0.003(4) C12 0.026(3) 0.026(4) 0.028(4) -0.010(4) 0.003(4) 0.001(3) C13 0.025(4) 0.047(6) 0.023(4) -0.004(4) -0.007(3) 0.011(4) C14 0.050(6) 0.057(7) 0.022(4) 0.013(4) -0.010(4) 0.015(5) C15 0.043(5) 0.032(5) 0.027(5) 0.003(4) 0.003(4) 0.001(4) C16 0.027(4) 0.023(4) 0.028(4) -0.002(5) 0.004(3) 0.009(3) C17 0.044(5) 0.016(4) 0.033(5) -0.002(3) 0.002(4) 0.006(4) C18 0.027(4) 0.050(6) 0.033(5) -0.013(6) 0.002(4) -0.004(4) C19 0.027(4) 0.047(6) 0.031(4) 0.001(5) 0.014(3) -0.011(4) C20 0.019(3) 0.023(4) 0.027(4) -0.002(4) 0.000(3) 0.001(3) C21 0.029(4) 0.025(5) 0.030(5) -0.006(4) 0.006(3) 0.002(3) C22 0.025(4) 0.039(6) 0.038(6) -0.001(4) -0.004(4) 0.003(4) C23 0.018(3) 0.024(4) 0.012(3) 0.007(3) 0.005(3) 0.009(3) C24 0.023(4) 0.034(5) 0.026(4) -0.001(4) 0.006(3) 0.003(4) C25 0.018(4) 0.023(5) 0.029(5) -0.009(4) 0.003(3) -0.002(3) O1W 0.026(3) 0.033(4) 0.061(4) -0.001(3) -0.015(3) -0.005(3) O3W 0.029(3) 0.034(4) 0.039(4) 0.001(3) 0.004(3) -0.001(3) O4W 0.038(4) 0.034(4) 0.047(4) 0.004(3) 0.003(3) -0.008(3) O5W 0.049(4) 0.043(4) 0.043(4) 0.003(4) -0.006(4) 0.000(3) O6W 0.042(4) 0.043(5) 0.065(5) 0.007(4) -0.008(3) 0.005(3) O7W 0.010(5) 0.002(5) 0.184(18) 0.013(9) -0.023(9) -0.004(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 Gd1 O1 2.379(6) . ? Gd1 O2 2.381(6) . ? Gd1 O5 2.418(6) . ? Gd1 O1W 2.439(6) . ? Gd1 O3W 2.488(7) . ? Gd1 N3 2.498(6) . ? Gd1 N7 2.537(8) 4_467 ? Gd1 O3 2.559(6) . ? Gd1 O4 2.563(6) . ? Gd1 Cu1 3.5102(11) . ? Cu1 O2 1.959(6) . ? Cu1 N1 1.966(7) . ? Cu1 N2 1.979(7) . ? Cu1 O1 1.984(6) . ? Co1 C24 1.882(9) . ? Co1 C25 1.885(9) . ? Co1 C22 1.891(10) . ? Co1 C20 1.907(7) . ? Co1 C21 1.909(9) . ? Co1 C23 1.921(7) . ? N1 C17 1.285(11) . ? N1 C1 1.477(11) . ? N2 C4 1.268(11) . ? N2 C3 1.469(11) . ? N3 C20 1.139(10) . ? N4 C21 1.146(12) . ? N5 C22 1.148(12) . ? N6 C23 1.136(9) . ? N7 C24 1.155(11) . ? N7 Gd1 2.537(8) 4_567 ? N8 C25 1.134(12) . ? O1 C11 1.353(10) . ? O2 C10 1.350(10) . ? O3 C12 1.384(11) . ? O3 C18 1.436(10) . ? O4 C9 1.371(10) . ? O4 C19 1.468(9) . ? C1 C2 1.509(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.503(14) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.450(11) . ? C4 H4 0.9500 . ? C5 C10 1.402(11) . ? C5 C6 1.427(12) . ? C6 C7 1.369(13) . ? C6 H6 0.9500 . ? C7 C8 1.404(14) . ? C7 H7 0.9500 . ? C8 C9 1.398(12) . ? C8 H8 0.9500 . ? C9 C10 1.412(11) . ? C11 C12 1.389(12) . ? C11 C16 1.404(12) . ? C12 C13 1.394(13) . ? C13 C14 1.358(15) . ? C13 H13 0.9500 . ? C14 C15 1.380(14) . ? C14 H14 0.9500 . ? C15 C16 1.386(13) . ? C15 H15 0.9500 . ? C16 C17 1.460(12) . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 O1 Gd1 O2 64.49(17) . . ? O1 Gd1 O5 74.9(2) . . ? O2 Gd1 O5 72.5(2) . . ? O1 Gd1 O1W 80.1(2) . . ? O2 Gd1 O1W 68.8(2) . . ? O5 Gd1 O1W 140.1(2) . . ? O1 Gd1 O3W 149.21(19) . . ? O2 Gd1 O3W 109.5(2) . . ? O5 Gd1 O3W 134.2(2) . . ? O1W Gd1 O3W 70.1(2) . . ? O1 Gd1 N3 135.1(2) . . ? O2 Gd1 N3 135.0(2) . . ? O5 Gd1 N3 76.2(2) . . ? O1W Gd1 N3 140.8(2) . . ? O3W Gd1 N3 71.9(2) . . ? O1 Gd1 N7 91.4(2) . 4_467 ? O2 Gd1 N7 136.4(2) . 4_467 ? O5 Gd1 N7 138.3(2) . 4_467 ? O1W Gd1 N7 71.8(2) . 4_467 ? O3W Gd1 N7 72.5(2) . 4_467 ? N3 Gd1 N7 88.0(2) . 4_467 ? O1 Gd1 O3 64.09(19) . . ? O2 Gd1 O3 122.7(2) . . ? O5 Gd1 O3 71.3(2) . . ? O1W Gd1 O3 123.5(2) . . ? O3W Gd1 O3 127.7(2) . . ? N3 Gd1 O3 74.5(2) . . ? N7 Gd1 O3 67.4(2) 4_467 . ? O1 Gd1 O4 125.15(19) . . ? O2 Gd1 O4 63.99(18) . . ? O5 Gd1 O4 73.0(2) . . ? O1W Gd1 O4 97.9(2) . . ? O3W Gd1 O4 68.2(2) . . ? N3 Gd1 O4 76.5(2) . . ? N7 Gd1 O4 140.5(2) 4_467 . ? O3 Gd1 O4 138.20(17) . . ? O1 Gd1 Cu1 32.76(14) . . ? O2 Gd1 Cu1 32.15(14) . . ? O5 Gd1 Cu1 74.52(13) . . ? O1W Gd1 Cu1 67.69(16) . . ? O3W Gd1 Cu1 131.74(14) . . ? N3 Gd1 Cu1 150.68(17) . . ? N7 Gd1 Cu1 113.78(17) 4_467 . ? O3 Gd1 Cu1 95.32(14) . . ? O4 Gd1 Cu1 95.53(13) . . ? O2 Cu1 N1 169.8(3) . . ? O2 Cu1 N2 92.3(3) . . ? N1 Cu1 N2 95.6(3) . . ? O2 Cu1 O1 80.2(2) . . ? N1 Cu1 O1 91.4(3) . . ? N2 Cu1 O1 171.0(3) . . ? O2 Cu1 Gd1 40.31(17) . . ? N1 Cu1 Gd1 131.8(2) . . ? N2 Cu1 Gd1 132.6(2) . . ? O1 Cu1 Gd1 40.45(17) . . ? C24 Co1 C25 88.6(4) . . ? C24 Co1 C22 93.9(4) . . ? C25 Co1 C22 176.9(4) . . ? C24 Co1 C20 92.2(3) . . ? C25 Co1 C20 87.5(4) . . ? C22 Co1 C20 90.5(4) . . ? C24 Co1 C21 179.3(4) . . ? C25 Co1 C21 92.0(4) . . ? C22 Co1 C21 85.5(4) . . ? C20 Co1 C21 87.7(3) . . ? C24 Co1 C23 85.9(3) . . ? C25 Co1 C23 92.4(3) . . ? C22 Co1 C23 89.8(3) . . ? C20 Co1 C23 178.1(4) . . ? C21 Co1 C23 94.2(3) . . ? C17 N1 C1 115.1(8) . . ? C17 N1 Cu1 123.5(6) . . ? C1 N1 Cu1 121.3(6) . . ? C4 N2 C3 116.2(7) . . ? C4 N2 Cu1 122.9(6) . . ? C3 N2 Cu1 121.0(6) . . ? C20 N3 Gd1 163.9(6) . . ? C24 N7 Gd1 169.5(7) . 4_567 ? C11 O1 Cu1 121.9(5) . . ? C11 O1 Gd1 122.2(5) . . ? Cu1 O1 Gd1 106.8(3) . . ? C10 O2 Cu1 124.4(5) . . ? C10 O2 Gd1 123.6(5) . . ? Cu1 O2 Gd1 107.5(2) . . ? C12 O3 C18 117.1(7) . . ? C12 O3 Gd1 117.1(5) . . ? C18 O3 Gd1 125.7(6) . . ? C9 O4 C19 114.0(7) . . ? C9 O4 Gd1 117.8(5) . . ? C19 O4 Gd1 127.2(5) . . ? N1 C1 C2 111.7(7) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? C3 C2 C1 114.4(7) . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? N2 C3 C2 112.9(7) . . ? N2 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? N2 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? N2 C4 C5 128.7(8) . . ? N2 C4 H4 115.7 . . ? C5 C4 H4 115.7 . . ? C10 C5 C6 120.0(8) . . ? C10 C5 C4 122.2(8) . . ? C6 C5 C4 117.6(8) . . ? C7 C6 C5 120.3(9) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 120.6(8) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C9 C8 C7 119.4(8) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? O4 C9 C8 124.1(8) . . ? O4 C9 C10 114.8(7) . . ? C8 C9 C10 121.2(8) . . ? O2 C10 C5 123.4(7) . . ? O2 C10 C9 118.1(7) . . ? C5 C10 C9 118.5(8) . . ? O1 C11 C12 119.6(8) . . ? O1 C11 C16 123.2(8) . . ? C12 C11 C16 117.2(8) . . ? O3 C12 C11 114.1(8) . . ? O3 C12 C13 123.7(8) . . ? C11 C12 C13 122.2(8) . . ? C14 C13 C12 119.3(8) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 120.3(9) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 120.8(9) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 120.1(8) . . ? C15 C16 C17 116.7(8) . . ? C11 C16 C17 123.1(8) . . ? N1 C17 C16 126.3(9) . . ? N1 C17 H17 116.8 . . ? C16 C17 H17 116.8 . . ? O3 C18 H18A 109.5 . . ? O3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C20 Co1 175.2(7) . . ? N4 C21 Co1 178.3(9) . . ? N5 C22 Co1 174.9(9) . . ? N6 C23 Co1 176.0(8) . . ? N7 C24 Co1 174.8(8) . . ? N8 C25 Co1 177.7(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.366 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.184 #====END