Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Athanassios Boudalis' 'Belen Abarca' 'Rafael Ballesteros' 'Mimoun Chadlaoui' 'Vassilis Psycharis' 'Catherine P Raptopoulou' 'Yiannis Sanakis' _publ_contact_author_name 'Athanassios Boudalis' _publ_contact_author_address ; Institute of Materials Science NCSR Patriarchou Grigoriou & Neapoleos Aghia Paraskevi Attikis 15310 GREECE ; _publ_contact_author_email 'TBOU@IMS.DEMOKRITOS.GR ' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; A pentanuclear CuII cluster derived from the metal-assisted hydrolysis of pyCOpyCOpy: structural, magnetic and spectroscopic studies ; data_tb515b _database_code_depnum_ccdc_archive 'CCDC 644727' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H52 Cu5 N6 O24' _chemical_formula_weight 1390.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.108(12) _cell_length_b 10.539(9) _cell_length_c 10.636(10) _cell_angle_alpha 100.09(4) _cell_angle_beta 110.70(3) _cell_angle_gamma 95.96(3) _cell_volume 1331(2) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11 _cell_measurement_theta_max 27 _exptl_crystal_description parall _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 707 _exptl_absorpt_coefficient_mu 2.994 _exptl_absorpt_correction_type 'psi-scan empirical' _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; The crystals had poor diffraction ability and the data were collected in increasing 2theta shells. The data collection was terminated when about 50% of the collected shell data were unobserved. ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'P21 Nicolet upgraded by Crystal Logic' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -2.9 _diffrn_reflns_number 3850 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 59.12 _reflns_number_total 3850 _reflns_number_gt 3305 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1179P)^2^+4.3757P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3850 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2162 _refine_ls_wR_factor_gt 0.2059 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 0.0000 0.5000 0.5000 0.0401(4) Uani 1 2 d S . . Cu2 Cu 0.09398(9) 0.37245(9) 0.24495(11) 0.0383(4) Uani 1 1 d . . . Cu3 Cu 0.24882(9) 0.17781(11) 0.25058(13) 0.0465(4) Uani 1 1 d . . . O1 O 0.0129(4) 0.4986(4) 0.3182(5) 0.0391(12) Uani 1 1 d . . . O3 O 0.1711(4) 0.2858(4) 0.1293(5) 0.0379(12) Uani 1 1 d . . . N1 N 0.1192(5) 0.6539(6) 0.5585(7) 0.0412(15) Uani 1 1 d . . . N2 N 0.1443(5) 0.5220(6) 0.1896(7) 0.0383(14) Uani 1 1 d . . . N3 N 0.3806(5) 0.3054(6) 0.2725(7) 0.0458(16) Uani 1 1 d . . . O11 O -0.0009(4) 0.2126(5) 0.2272(6) 0.0452(13) Uani 1 1 d . . . O12 O 0.1085(5) 0.0632(5) 0.2151(7) 0.0577(16) Uani 1 1 d . . . O13 O 0.1388(6) 0.3621(6) 0.5669(7) 0.0640(17) Uani 1 1 d . . . O14 O 0.2247(4) 0.3296(5) 0.4247(6) 0.0495(14) Uani 1 1 d . . . O15 O 0.3321(5) 0.0563(6) 0.3444(7) 0.0622(17) Uani 1 1 d . . . O16 O 0.3459(7) -0.0225(7) 0.1463(9) 0.085(2) Uani 1 1 d . . . C1 C 0.1873(7) 0.7071(8) 0.6870(10) 0.051(2) Uani 1 1 d . . . H1 H 0.1807 0.6703 0.7578 0.067 Uiso 1 1 calc R . . C2 C 0.2687(8) 0.8170(9) 0.7193(10) 0.061(2) Uani 1 1 d . . . H2 H 0.3193 0.8504 0.8094 0.079 Uiso 1 1 calc R . . C3 C 0.2720(8) 0.8738(8) 0.6155(11) 0.061(2) Uani 1 1 d . . . H3 H 0.3221 0.9508 0.6354 0.080 Uiso 1 1 calc R . . C4 C 0.2023(7) 0.8188(8) 0.4817(10) 0.054(2) Uani 1 1 d . . . H4 H 0.2057 0.8566 0.4102 0.070 Uiso 1 1 calc R . . C5 C 0.1260(6) 0.7050(7) 0.4548(9) 0.0416(18) Uani 1 1 d . . . C6 C 0.0453(6) 0.6298(7) 0.3117(8) 0.0401(18) Uani 1 1 d . . . O2 O -0.0480(4) 0.6913(5) 0.2661(6) 0.0425(13) Uani 1 1 d . . . HO2 H -0.069(8) 0.695(10) 0.321(10) 0.055 Uiso 1 1 d . . . C7 C 0.0995(6) 0.6277(7) 0.2076(8) 0.0387(17) Uani 1 1 d . . . C8 C 0.1072(7) 0.7244(8) 0.1333(9) 0.0470(19) Uani 1 1 d . . . H8 H 0.0759 0.7987 0.1446 0.061 Uiso 1 1 calc R . . C9 C 0.1611(7) 0.7075(7) 0.0450(9) 0.048(2) Uani 1 1 d . . . H9 H 0.1679 0.7719 -0.0026 0.063 Uiso 1 1 calc R . . C10 C 0.2065(7) 0.5946(8) 0.0243(9) 0.0471(19) Uani 1 1 d . . . H10 H 0.2423 0.5813 -0.0372 0.061 Uiso 1 1 calc R . . C11 C 0.1949(6) 0.5023(7) 0.1024(8) 0.0419(18) Uani 1 1 d . . . C12 C 0.2364(6) 0.3711(7) 0.0918(9) 0.0440(19) Uani 1 1 d . . . O4 O 0.2342(5) 0.3238(5) -0.0399(6) 0.0471(13) Uani 1 1 d . . . HO4 H 0.160(8) 0.321(9) -0.106(10) 0.061 Uiso 1 1 d . . . C13 C 0.3581(7) 0.3892(7) 0.1907(9) 0.048(2) Uani 1 1 d . . . C14 C 0.4414(7) 0.4842(10) 0.1910(12) 0.067(3) Uani 1 1 d . . . H14 H 0.4258 0.5407 0.1313 0.087 Uiso 1 1 calc R . . C15 C 0.5468(8) 0.4901(11) 0.2830(15) 0.094(4) Uani 1 1 d . . . H15 H 0.6035 0.5534 0.2868 0.123 Uiso 1 1 calc R . . C16 C 0.5712(8) 0.4069(10) 0.3687(13) 0.076(3) Uani 1 1 d . . . H16 H 0.6433 0.4113 0.4299 0.098 Uiso 1 1 calc R . . C17 C 0.4839(7) 0.3144(9) 0.3613(11) 0.064(3) Uani 1 1 d . . . H17 H 0.4982 0.2571 0.4202 0.083 Uiso 1 1 calc R . . C21 C 0.0203(8) 0.0981(8) 0.2096(10) 0.056(2) Uani 1 1 d . . . C22 C -0.0787(8) -0.0106(8) 0.1726(16) 0.088(4) Uani 1 1 d . . . H22A H -0.1451 0.0158 0.1180 0.114 Uiso 1 1 calc R . . H22B H -0.0852 -0.0271 0.2557 0.114 Uiso 1 1 calc R . . H22C H -0.0681 -0.0889 0.1209 0.114 Uiso 1 1 calc R . . C23 C 0.1975(8) 0.3046(8) 0.5221(9) 0.050(2) Uani 1 1 d . . . C24 C 0.2429(12) 0.1945(12) 0.5865(13) 0.087(4) Uani 1 1 d . . . H24A H 0.2948 0.1636 0.5488 0.113 Uiso 1 1 calc R . . H24B H 0.1831 0.1239 0.5669 0.113 Uiso 1 1 calc R . . H24C H 0.2797 0.2263 0.6846 0.113 Uiso 1 1 calc R . . C25 C 0.3630(7) -0.0243(8) 0.2692(11) 0.056(2) Uani 1 1 d . . . C26 C 0.4219(9) -0.1245(10) 0.3352(14) 0.082(3) Uani 1 1 d . . . H26A H 0.4630 -0.0875 0.4317 0.106 Uiso 1 1 calc R . . H26B H 0.4719 -0.1507 0.2920 0.106 Uiso 1 1 calc R . . H26C H 0.3686 -0.1996 0.3240 0.106 Uiso 1 1 calc R . . OW1 O 0.3712(7) 0.1251(8) 0.9563(10) 0.092(2) Uani 1 1 d . . . OW2 O 0.5769(9) 0.2416(11) 0.9767(12) 0.125(3) 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 0.0476(9) 0.0265(8) 0.0496(9) 0.0161(7) 0.0191(7) 0.0058(6) Cu2 0.0423(6) 0.0207(5) 0.0555(7) 0.0156(5) 0.0191(5) 0.0080(4) Cu3 0.0468(7) 0.0319(6) 0.0652(8) 0.0214(6) 0.0193(6) 0.0150(5) O1 0.046(3) 0.018(2) 0.058(3) 0.018(2) 0.020(2) 0.007(2) O3 0.041(3) 0.020(2) 0.057(3) 0.015(2) 0.020(2) 0.006(2) N1 0.050(4) 0.031(3) 0.048(4) 0.013(3) 0.020(3) 0.011(3) N2 0.042(3) 0.025(3) 0.051(4) 0.017(3) 0.017(3) 0.008(3) N3 0.041(4) 0.037(3) 0.058(4) 0.015(3) 0.013(3) 0.011(3) O11 0.052(3) 0.024(3) 0.064(3) 0.015(2) 0.024(3) 0.008(2) O12 0.061(4) 0.027(3) 0.095(5) 0.026(3) 0.032(3) 0.019(3) O13 0.083(4) 0.061(4) 0.079(4) 0.043(3) 0.047(4) 0.042(4) O14 0.050(3) 0.044(3) 0.060(4) 0.023(3) 0.021(3) 0.013(3) O15 0.067(4) 0.043(3) 0.088(5) 0.032(3) 0.029(4) 0.027(3) O16 0.110(6) 0.057(4) 0.103(6) 0.030(4) 0.051(5) 0.021(4) C1 0.048(5) 0.044(5) 0.060(6) 0.015(4) 0.016(4) 0.010(4) C2 0.057(5) 0.045(5) 0.065(6) 0.002(5) 0.014(5) -0.003(4) C3 0.055(5) 0.035(4) 0.083(7) 0.009(5) 0.019(5) -0.003(4) C4 0.063(5) 0.030(4) 0.065(6) 0.011(4) 0.021(5) -0.002(4) C5 0.040(4) 0.025(4) 0.062(5) 0.014(3) 0.019(4) 0.008(3) C6 0.050(4) 0.020(3) 0.049(4) 0.015(3) 0.012(4) 0.012(3) O2 0.048(3) 0.032(3) 0.061(4) 0.024(3) 0.027(3) 0.018(2) C7 0.047(4) 0.024(4) 0.046(4) 0.014(3) 0.015(4) 0.008(3) C8 0.053(5) 0.036(4) 0.062(5) 0.027(4) 0.023(4) 0.019(4) C9 0.058(5) 0.029(4) 0.063(5) 0.025(4) 0.022(4) 0.011(4) C10 0.055(5) 0.042(4) 0.053(5) 0.025(4) 0.022(4) 0.011(4) C11 0.045(4) 0.033(4) 0.054(5) 0.019(3) 0.021(4) 0.011(3) C12 0.043(4) 0.030(4) 0.060(5) 0.020(4) 0.014(4) 0.011(3) O4 0.051(3) 0.038(3) 0.052(3) 0.011(3) 0.019(3) 0.011(2) C13 0.043(4) 0.031(4) 0.062(5) 0.009(4) 0.014(4) 0.002(3) C14 0.047(5) 0.057(6) 0.097(8) 0.037(5) 0.018(5) 0.005(4) C15 0.048(6) 0.064(7) 0.142(12) 0.035(8) 0.003(7) -0.011(5) C16 0.041(5) 0.069(6) 0.105(9) 0.025(6) 0.009(5) 0.012(5) C17 0.053(5) 0.054(5) 0.070(6) 0.019(5) 0.003(5) 0.017(4) C21 0.060(5) 0.024(4) 0.078(6) 0.016(4) 0.016(5) 0.010(4) C22 0.052(5) 0.028(4) 0.184(13) 0.025(6) 0.046(7) 0.003(4) C23 0.064(5) 0.034(4) 0.052(5) 0.014(4) 0.019(4) 0.017(4) C24 0.131(10) 0.074(7) 0.090(8) 0.054(7) 0.055(8) 0.052(7) C25 0.053(5) 0.038(5) 0.074(6) 0.025(5) 0.015(5) 0.010(4) C26 0.075(7) 0.051(6) 0.118(9) 0.031(6) 0.025(7) 0.031(5) OW1 0.091(5) 0.074(5) 0.124(7) 0.030(5) 0.049(5) 0.023(4) OW2 0.116(8) 0.112(8) 0.153(10) 0.032(7) 0.064(7) 0.003(6) _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 N1 1.972(7) . ? Cu1 N1 1.972(7) 2_566 ? Cu1 O1 1.997(6) . ? Cu1 O1 1.997(6) 2_566 ? Cu1 O13 2.435(6) 2_566 ? Cu1 O13 2.435(6) . ? Cu2 N2 1.910(6) . ? Cu2 O11 1.926(5) . ? Cu2 O1 2.005(5) . ? Cu2 O3 2.011(5) . ? Cu2 O14 2.223(6) . ? Cu2 Cu3 3.025(2) . ? Cu3 O15 1.949(6) . ? Cu3 O3 1.956(5) . ? Cu3 O12 1.968(6) . ? Cu3 N3 1.993(7) . ? Cu3 O14 2.360(6) . ? O1 C6 1.425(8) . ? O3 C12 1.381(9) . ? N1 C1 1.321(11) . ? N1 C5 1.335(10) . ? N2 C11 1.319(10) . ? N2 C7 1.327(9) . ? N3 C13 1.328(11) . ? N3 C17 1.331(11) . ? O11 C21 1.263(9) . ? O12 C21 1.235(10) . ? O13 C23 1.200(10) . ? O14 C23 1.267(11) . ? O15 C25 1.260(12) . ? O16 C25 1.250(12) . ? C1 C2 1.394(12) . ? C1 H1 0.9300 . ? C2 C3 1.356(14) . ? C2 H2 0.9300 . ? C3 C4 1.371(13) . ? C3 H3 0.9300 . ? C4 C5 1.397(11) . ? C4 H4 0.9300 . ? C5 C6 1.525(11) . ? C6 O2 1.416(9) . ? C6 C7 1.511(11) . ? O2 HO2 0.73(9) . ? C7 C8 1.411(11) . ? C8 C9 1.359(12) . ? C8 H8 0.9300 . ? C9 C10 1.402(11) . ? C9 H9 0.9300 . ? C10 C11 1.415(11) . ? C10 H10 0.9300 . ? C11 C12 1.538(10) . ? C12 O4 1.392(10) . ? C12 C13 1.539(11) . ? O4 HO4 0.97(10) . ? C13 C14 1.402(12) . ? C14 C15 1.370(13) . ? C14 H14 0.9300 . ? C15 C16 1.354(16) . ? C15 H15 0.9300 . ? C16 C17 1.395(14) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C21 C22 1.524(12) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.518(13) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.501(13) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 180.0(3) . 2_566 ? N1 Cu1 O1 81.3(2) . . ? N1 Cu1 O1 98.7(2) 2_566 . ? N1 Cu1 O1 98.7(2) . 2_566 ? N1 Cu1 O1 81.3(2) 2_566 2_566 ? O1 Cu1 O1 180.000(1) . 2_566 ? N1 Cu1 O13 90.2(3) . 2_566 ? N1 Cu1 O13 89.8(3) 2_566 2_566 ? O1 Cu1 O13 86.4(2) . 2_566 ? O1 Cu1 O13 93.6(2) 2_566 2_566 ? N1 Cu1 O13 89.8(3) . . ? N1 Cu1 O13 90.2(3) 2_566 . ? O1 Cu1 O13 93.6(2) . . ? O1 Cu1 O13 86.4(2) 2_566 . ? O13 Cu1 O13 180.000(1) 2_566 . ? N2 Cu2 O11 156.8(3) . . ? N2 Cu2 O1 81.9(2) . . ? O11 Cu2 O1 98.0(2) . . ? N2 Cu2 O3 81.2(2) . . ? O11 Cu2 O3 94.3(2) . . ? O1 Cu2 O3 161.1(2) . . ? N2 Cu2 O14 112.4(2) . . ? O11 Cu2 O14 89.8(2) . . ? O1 Cu2 O14 107.7(2) . . ? O3 Cu2 O14 86.5(2) . . ? N2 Cu2 Cu3 109.63(19) . . ? O11 Cu2 Cu3 78.89(17) . . ? O1 Cu2 Cu3 157.76(16) . . ? O3 Cu2 Cu3 39.62(14) . . ? O14 Cu2 Cu3 50.66(16) . . ? O15 Cu3 O3 170.1(3) . . ? O15 Cu3 O12 90.4(3) . . ? O3 Cu3 O12 91.4(2) . . ? O15 Cu3 N3 96.1(3) . . ? O3 Cu3 N3 82.1(2) . . ? O12 Cu3 N3 173.5(2) . . ? O15 Cu3 O14 105.6(3) . . ? O3 Cu3 O14 84.1(2) . . ? O12 Cu3 O14 91.5(2) . . ? N3 Cu3 O14 87.7(2) . . ? O15 Cu3 Cu2 148.7(2) . . ? O3 Cu3 Cu2 40.99(16) . . ? O12 Cu3 Cu2 78.09(17) . . ? N3 Cu3 Cu2 96.77(19) . . ? O14 Cu3 Cu2 46.77(14) . . ? C6 O1 Cu1 108.9(4) . . ? C6 O1 Cu2 112.9(5) . . ? Cu1 O1 Cu2 120.8(2) . . ? C12 O3 Cu3 116.1(4) . . ? C12 O3 Cu2 114.8(4) . . ? Cu3 O3 Cu2 99.4(2) . . ? C1 N1 C5 120.5(7) . . ? C1 N1 Cu1 125.5(6) . . ? C5 N1 Cu1 113.9(5) . . ? C11 N2 C7 122.3(6) . . ? C11 N2 Cu2 117.2(5) . . ? C7 N2 Cu2 117.5(5) . . ? C13 N3 C17 119.7(8) . . ? C13 N3 Cu3 114.2(5) . . ? C17 N3 Cu3 126.1(6) . . ? C21 O11 Cu2 126.8(6) . . ? C21 O12 Cu3 126.6(5) . . ? C23 O13 Cu1 140.0(6) . . ? C23 O14 Cu2 117.5(5) . . ? C23 O14 Cu3 127.1(5) . . ? Cu2 O14 Cu3 82.6(2) . . ? C25 O15 Cu3 114.4(6) . . ? N1 C1 C2 121.7(9) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 118.0(9) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? C2 C3 C4 120.7(8) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 118.6(9) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 120.2(8) . . ? N1 C5 C6 114.7(6) . . ? C4 C5 C6 125.1(8) . . ? O2 C6 O1 111.1(6) . . ? O2 C6 C7 107.1(6) . . ? O1 C6 C7 108.9(6) . . ? O2 C6 C5 110.5(6) . . ? O1 C6 C5 108.5(6) . . ? C7 C6 C5 110.8(6) . . ? C6 O2 HO2 104(8) . . ? N2 C7 C8 119.6(7) . . ? N2 C7 C6 113.5(6) . . ? C8 C7 C6 126.9(6) . . ? C9 C8 C7 119.1(7) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C10 121.2(7) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C9 C10 C11 116.1(8) . . ? C9 C10 H10 122.0 . . ? C11 C10 H10 122.0 . . ? N2 C11 C10 121.6(7) . . ? N2 C11 C12 114.3(6) . . ? C10 C11 C12 124.0(7) . . ? O3 C12 O4 112.6(6) . . ? O3 C12 C11 107.2(6) . . ? O4 C12 C11 111.2(6) . . ? O3 C12 C13 109.4(6) . . ? O4 C12 C13 106.1(7) . . ? C11 C12 C13 110.4(6) . . ? C12 O4 HO4 109(6) . . ? N3 C13 C14 121.8(8) . . ? N3 C13 C12 115.8(7) . . ? C14 C13 C12 122.4(8) . . ? C15 C14 C13 117.0(10) . . ? C15 C14 H14 121.5 . . ? C13 C14 H14 121.5 . . ? C16 C15 C14 122.2(10) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C17 117.3(9) . . ? C15 C16 H16 121.3 . . ? C17 C16 H16 121.3 . . ? N3 C17 C16 122.0(9) . . ? N3 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? O12 C21 O11 129.0(8) . . ? O12 C21 C22 116.5(7) . . ? O11 C21 C22 114.5(8) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O13 C23 O14 124.6(8) . . ? O13 C23 C24 118.0(9) . . ? O14 C23 C24 117.5(8) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O16 C25 O15 122.7(8) . . ? O16 C25 C26 121.1(10) . . ? O15 C25 C26 116.2(10) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 59.12 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.740 _refine_diff_density_min -1.322 _refine_diff_density_rms 0.150 # start Validation Reply Form # PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 59.12 Deg. # RESPONSE: see _exptl_special_details above # PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.94 # RESPONSE: see _exptl_special_details above # RESPONSE: It corresponds to a solvate water molecule for which no # H-atoms were included in the refinement. # end Validation Reply Form