# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _publ_contact_author 'Igor O.Fritsky' _publ_contact_author_email KONTECKA@WCHUWR.CHEM.UNI.WROC.PL _publ_section_title ;New CuII [12]metallocrown-4 pentanuclear complex based on CuII-malonomono-hydroxamic acid unit ; _publ_contact_author_name 'Elzbieta Gumienna-Kontecka' loop_ _publ_author_name E.Gumienna-Kontecka I.A.Golenya N.M.Dudarenko A.Dobosz ; M.Haukka ; I.O.Fritsky J.Swiatek-Kozlowska data_1 _database_code_depnum_ccdc_archive 'CCDC 643467' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(ethylenediamine)diaquacopper(II) catena-bis(ethylenediamine) (aqua)copper(II)(mu-aqua)bis((triaqua)tetrakis(malonomonohydroxate) pentacopper(II)) hydrate ; _chemical_name_common ; bis(ethylenediamine)diaquacopper(ii) catena- bis(ethylenediamine) (aqua)copper(ii)(mu- aqua)bis((triaqua)tetrakis(malonomonohydroxate) pentacopper(ii)) hydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H32 Cu6 N8 O20, 11(H2 O)' _chemical_formula_sum 'C16 H54 Cu6 N8 O31' _chemical_formula_weight 1235.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 11.2883(4) _cell_length_b 13.0045(4) _cell_length_c 14.3048(6) _cell_angle_alpha 84.252(2) _cell_angle_beta 82.162(2) _cell_angle_gamma 88.661(2) _cell_volume 2069.75(13) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9047 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'bluish green' _exptl_crystal_colour plate _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 3.137 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5401 _exptl_absorpt_correction_T_max 0.7875 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; Two of the water molceules (O31 and O32) were refined with occupation factor 0.5. The position of H~2~O hydrogens were estimated with HYDROGEN (Nardelli, 1999) program. Water hydrogens were constrained to ride on their parent oxygens 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 =0.98-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41194 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0605 _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 -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9041 _reflns_number_gt 6300 _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 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1d (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^)+(0.0490P)^2^+2.7643P] 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 9041 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Cu1A Cu -0.16838(4) 0.30331(4) -0.21611(4) 0.01959(13) Uani 1 1 d . . . Cu1B Cu 0.11032(4) 0.15354(4) -0.03562(4) 0.01760(12) Uani 1 1 d . . . Cu1C Cu 0.02413(4) 0.39091(4) 0.17881(4) 0.02112(13) Uani 1 1 d . . . Cu1D Cu -0.26721(4) 0.53354(4) 0.00644(4) 0.01816(12) Uani 1 1 d . . . Cu2 Cu -0.06169(4) 0.35647(4) -0.02993(3) 0.01776(12) Uani 1 1 d . . . Cu3 Cu 0.0000 0.5000 -0.5000 0.0512(3) Uani 1 2 d S . . Cu4 Cu 0.5000 1.0000 0.0000 0.02830(19) Uani 1 2 d S . . O1A O 0.1317(4) -0.1183(3) -0.1450(3) 0.0527(11) Uani 1 1 d . . . O2A O 0.1407(2) 0.0170(2) -0.0683(2) 0.0230(7) Uani 1 1 d . . . O3A O -0.1107(2) 0.1629(2) -0.2435(2) 0.0235(7) Uani 1 1 d . . . O4A O -0.0329(2) 0.2925(2) -0.1460(2) 0.0183(6) Uani 1 1 d . . . O1C O -0.3012(3) 0.7805(2) 0.1481(2) 0.0242(7) Uani 1 1 d . . . O2C O -0.3396(2) 0.6474(2) 0.0727(2) 0.0209(6) Uani 1 1 d . . . O3C O -0.0817(2) 0.4949(2) 0.2399(2) 0.0210(6) Uani 1 1 d . . . O4C O -0.0790(3) 0.4181(2) 0.0848(2) 0.0259(7) Uani 1 1 d . . . O1B O 0.2905(3) 0.3072(3) 0.3312(3) 0.0424(9) Uani 1 1 d . . . O2B O 0.1310(3) 0.3706(2) 0.2717(2) 0.0246(7) Uani 1 1 d . . . O3B O 0.1898(2) 0.1342(2) 0.0781(2) 0.0225(6) Uani 1 1 d . . . O4B O 0.0745(2) 0.2841(2) 0.0095(2) 0.0213(6) Uani 1 1 d . . . O1D O -0.4666(3) 0.3630(3) -0.3435(3) 0.0520(11) Uani 1 1 d . . . O2D O -0.3028(3) 0.3049(2) -0.2858(2) 0.0275(7) Uani 1 1 d . . . O3D O -0.3684(2) 0.5406(2) -0.0942(2) 0.0202(6) Uani 1 1 d . . . O4D O -0.1668(2) 0.4558(2) -0.08251(19) 0.0193(6) Uani 1 1 d . . . O5 O -0.0331(3) 0.3828(2) -0.3454(2) 0.0281(7) Uani 1 1 d . . . H5D H 0.0045 0.4208 -0.3136 0.042 Uiso 1 1 d R . . H5E H 0.0225 0.3289 -0.3702 0.042 Uiso 1 1 d R . . O6 O -0.1069(3) 0.2475(2) 0.2772(2) 0.0315(7) Uani 1 1 d . . . H6D H -0.1185 0.1953 0.2452 0.047 Uiso 1 1 d R . . H6E H -0.0857 0.2075 0.3300 0.047 Uiso 1 1 d R . . O7 O -0.3965(3) 0.3831(2) 0.0839(2) 0.0308(7) Uani 1 1 d . . . H7D H -0.4677 0.4086 0.0884 0.046 Uiso 1 1 d R . . H7E H -0.3829 0.3639 0.1401 0.046 Uiso 1 1 d R . . O8 O -0.2360(3) 0.2305(2) 0.0054(2) 0.0371(8) Uani 1 1 d . . . H8D H -0.2019 0.1974 0.0562 0.056 Uiso 1 1 d R . . H8E H -0.2852 0.2765 0.0330 0.056 Uiso 1 1 d R . . O9 O 0.5367(3) 0.8098(2) -0.0321(3) 0.0379(8) Uani 1 1 d . . . H9D H 0.5738 0.7644 0.0027 0.057 Uiso 1 1 d R . . H9E H 0.4626 0.7931 -0.0214 0.057 Uiso 1 1 d R . . O1W O 0.0030(3) 0.1388(2) 0.4395(2) 0.0407(9) Uani 1 1 d . . . H11W H -0.0412 0.1046 0.4943 0.061 Uiso 1 1 d R . . H21W H 0.0030 0.0857 0.4008 0.061 Uiso 1 1 d R . . O2W O 0.4602(5) 0.1778(4) 0.3862(3) 0.099(2) Uani 1 1 d . . . H12W H 0.3788 0.2089 0.4002 0.148 Uiso 1 1 d R . . H22W H 0.4658 0.1489 0.4415 0.148 Uiso 1 1 d R . . O3W O 0.6635(3) 0.3400(3) 0.2647(3) 0.0508(10) Uani 1 1 d . . . H13W H 0.7398 0.3189 0.2667 0.076 Uiso 1 1 d R . . H23W H 0.6181 0.3320 0.3176 0.076 Uiso 1 1 d R . . O4W O 0.7166(5) 0.0486(4) 0.3706(4) 0.102(2) Uani 1 1 d . . . H14W H 0.6566 0.0817 0.3719 0.153 Uiso 1 1 d R . . H24W H 0.7125 -0.0157 0.3596 0.153 Uiso 1 1 d R . . O5W O 0.1300(3) 0.9547(3) 0.3945(2) 0.0411(9) Uani 1 1 d . . . H15W H 0.1029 0.9392 0.3443 0.062 Uiso 1 1 d R . . H25W H 0.2136 0.9606 0.3908 0.062 Uiso 1 1 d R . . O6W O 0.3545(3) 0.9771(3) 0.4382(3) 0.0632(13) Uani 1 1 d . . . H16W H 0.3635 1.0413 0.4209 0.095 Uiso 1 1 d R . . H26W H 0.3324 0.9691 0.4977 0.095 Uiso 1 1 d R . . O7W O 0.5042(3) 0.8034(2) 0.4298(2) 0.0360(8) Uani 1 1 d . . . H17W H 0.4424 0.7588 0.4120 0.054 Uiso 1 1 d R . . H27W H 0.4423 0.8544 0.4524 0.054 Uiso 1 1 d R . . O8W O 0.7187(3) 0.8522(3) 0.3207(2) 0.0394(8) Uani 1 1 d . . . H18W H 0.7098 0.8214 0.2620 0.059 Uiso 1 1 d R . . H28W H 0.6458 0.8375 0.3587 0.059 Uiso 1 1 d R . . O9W O 0.8785(3) 0.7582(2) 0.4306(2) 0.0423(9) Uani 1 1 d . . . H19W H 0.9029 0.8010 0.4647 0.064 Uiso 1 1 d R . . H29W H 0.8272 0.8009 0.4015 0.064 Uiso 1 1 d R . . O10W O 0.5327(11) 0.4215(9) 0.4082(7) 0.117(5) Uani 0.50 1 d P . . H110 H 0.5138 0.4830 0.3892 0.176 Uiso 0.50 1 d PR . . H510 H 0.4928 0.3917 0.4578 0.176 Uiso 0.50 1 d PR . . O11W O 0.5944(10) 0.1534(8) 0.2438(8) 0.102(4) Uani 0.50 1 d P . . H211 H 0.6659 0.1718 0.2449 0.153 Uiso 0.50 1 d PR . . H311 H 0.5468 0.1618 0.2939 0.153 Uiso 0.50 1 d PR . . N1A N 0.0144(3) 0.1905(2) -0.1370(2) 0.0171(7) Uani 1 1 d . . . N1D N -0.2320(3) 0.4227(2) -0.1522(2) 0.0181(7) Uani 1 1 d . . . N1B N 0.1110(3) 0.2949(3) 0.0986(2) 0.0195(7) Uani 1 1 d . . . N1C N -0.1614(3) 0.4987(2) 0.1016(2) 0.0199(8) Uani 1 1 d . . . N2 N 0.3528(3) 0.9544(3) 0.0868(3) 0.0333(10) Uani 1 1 d . . . H2NA H 0.2975 1.0076 0.0898 0.040 Uiso 1 1 calc R . . H2NB H 0.3192 0.8995 0.0646 0.040 Uiso 1 1 calc R . . N3 N 0.5803(3) 0.9845(3) 0.1173(3) 0.0323(9) Uani 1 1 d . . . H3NA H 0.6269 0.9255 0.1185 0.039 Uiso 1 1 calc R . . H3NB H 0.6284 1.0403 0.1185 0.039 Uiso 1 1 calc R . . N4 N 0.0713(5) 0.6150(3) -0.4424(3) 0.0575(14) Uani 1 1 d . . . H4NA H 0.0323 0.6764 -0.4566 0.069 Uiso 1 1 calc R . . H4NB H 0.0635 0.6013 -0.3776 0.069 Uiso 1 1 calc R . . N5 N 0.1723(5) 0.4546(4) -0.5350(3) 0.0608(15) Uani 1 1 d . . . H5NA H 0.1809 0.3852 -0.5170 0.073 Uiso 1 1 calc R . . H5NB H 0.1940 0.4658 -0.5995 0.073 Uiso 1 1 calc R . . C1A C 0.1025(4) -0.0274(3) -0.1325(3) 0.0229(9) Uani 1 1 d . . . C2A C 0.0168(4) 0.0228(3) -0.1974(3) 0.0228(9) Uani 1 1 d . . . H2A H 0.0559 0.0187 -0.2632 0.027 Uiso 1 1 calc R . . H2B H -0.0544 -0.0220 -0.1887 0.027 Uiso 1 1 calc R . . C3A C -0.0289(3) 0.1321(3) -0.1918(3) 0.0169(8) Uani 1 1 d . . . C1D C -0.3907(4) 0.3686(3) -0.2885(3) 0.0281(10) Uani 1 1 d . . . C2D C -0.4115(4) 0.4562(3) -0.2262(3) 0.0260(10) Uani 1 1 d . . . H2C H -0.4111 0.5208 -0.2691 0.031 Uiso 1 1 calc R . . H2D H -0.4937 0.4484 -0.1922 0.031 Uiso 1 1 calc R . . C3D C -0.3318(4) 0.4735(3) -0.1534(3) 0.0190(9) Uani 1 1 d . . . C3B C 0.1717(4) 0.2133(3) 0.1259(3) 0.0214(9) Uani 1 1 d . . . C2B C 0.2250(4) 0.2110(3) 0.2173(3) 0.0282(10) Uani 1 1 d . . . H2E H 0.3114 0.1955 0.2020 0.034 Uiso 1 1 calc R . . H2F H 0.1898 0.1511 0.2592 0.034 Uiso 1 1 calc R . . C1B C 0.2149(4) 0.3029(3) 0.2763(3) 0.0280(10) Uani 1 1 d . . . C3C C -0.1570(4) 0.5323(3) 0.1832(3) 0.0185(9) Uani 1 1 d . . . C2C C -0.2417(4) 0.6168(3) 0.2150(3) 0.0209(9) Uani 1 1 d . . . H11G H -0.1988 0.6615 0.2511 0.025 Uiso 1 1 calc R . . H11H H -0.3082 0.5844 0.2597 0.025 Uiso 1 1 calc R . . C1C C -0.2961(3) 0.6863(3) 0.1388(3) 0.0181(9) Uani 1 1 d . . . C4 C 0.1990(7) 0.6228(4) -0.4819(4) 0.0604(18) Uani 1 1 d . . . H4A H 0.2427 0.6611 -0.4411 0.072 Uiso 1 1 calc R . . H4B H 0.2078 0.6600 -0.5463 0.072 Uiso 1 1 calc R . . C5 C 0.2483(7) 0.5148(5) -0.4860(4) 0.068(2) Uani 1 1 d . . . H5A H 0.3308 0.5169 -0.5201 0.082 Uiso 1 1 calc R . . H5B H 0.2511 0.4818 -0.4209 0.082 Uiso 1 1 calc R . . C6 C 0.3868(5) 0.9239(6) 0.1811(5) 0.070(2) Uani 1 1 d . . . H6A H 0.3189 0.9375 0.2300 0.084 Uiso 1 1 calc R . . H6B H 0.4043 0.8488 0.1873 0.084 Uiso 1 1 calc R . . C7 C 0.4885(5) 0.9784(7) 0.1969(4) 0.085(3) Uani 1 1 d . . . H7A H 0.5211 0.9434 0.2528 0.102 Uiso 1 1 calc R . . H7B H 0.4637 1.0492 0.2115 0.102 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1A 0.0222(3) 0.0187(3) 0.0208(3) -0.0079(2) -0.0103(2) 0.0081(2) Cu1B 0.0187(3) 0.0162(2) 0.0194(3) -0.0047(2) -0.0068(2) 0.0063(2) Cu1C 0.0251(3) 0.0218(3) 0.0199(3) -0.0089(2) -0.0121(2) 0.0112(2) Cu1D 0.0193(3) 0.0185(3) 0.0191(3) -0.0075(2) -0.0088(2) 0.0088(2) Cu2 0.0197(3) 0.0178(2) 0.0180(3) -0.0069(2) -0.0083(2) 0.0088(2) Cu3 0.1022(9) 0.0289(5) 0.0245(5) -0.0082(4) -0.0137(5) 0.0160(5) Cu4 0.0216(4) 0.0239(4) 0.0399(5) 0.0004(4) -0.0095(3) 0.0060(3) O1A 0.086(3) 0.0309(19) 0.055(2) -0.0252(18) -0.050(2) 0.0326(19) O2A 0.0270(16) 0.0158(14) 0.0292(17) -0.0073(13) -0.0114(13) 0.0048(12) O3A 0.0280(16) 0.0216(15) 0.0249(17) -0.0111(13) -0.0131(13) 0.0091(13) O4A 0.0204(14) 0.0147(13) 0.0219(16) -0.0054(12) -0.0087(12) 0.0079(11) O1C 0.0293(16) 0.0191(15) 0.0249(17) -0.0054(13) -0.0050(13) 0.0063(13) O2C 0.0212(15) 0.0218(14) 0.0219(16) -0.0092(13) -0.0078(12) 0.0097(12) O3C 0.0253(15) 0.0202(14) 0.0200(16) -0.0064(12) -0.0100(13) 0.0071(12) O4C 0.0318(17) 0.0265(16) 0.0240(17) -0.0159(13) -0.0144(14) 0.0211(13) O1B 0.050(2) 0.041(2) 0.045(2) -0.0202(17) -0.0350(19) 0.0242(17) O2B 0.0321(17) 0.0257(16) 0.0195(16) -0.0075(13) -0.0131(13) 0.0099(14) O3B 0.0258(16) 0.0202(15) 0.0236(16) -0.0069(13) -0.0091(13) 0.0104(12) O4B 0.0266(15) 0.0226(15) 0.0190(16) -0.0111(12) -0.0139(13) 0.0130(12) O1D 0.052(2) 0.053(2) 0.067(3) -0.042(2) -0.046(2) 0.0307(19) O2D 0.0269(16) 0.0284(16) 0.0328(19) -0.0140(14) -0.0177(14) 0.0119(14) O3D 0.0187(14) 0.0227(15) 0.0210(16) -0.0071(12) -0.0066(12) 0.0079(12) O4D 0.0202(14) 0.0209(14) 0.0209(16) -0.0101(12) -0.0123(12) 0.0057(12) O5 0.0388(18) 0.0247(16) 0.0222(17) -0.0047(13) -0.0080(14) 0.0054(14) O6 0.0403(19) 0.0242(16) 0.0331(19) -0.0095(14) -0.0125(15) 0.0089(14) O7 0.0247(16) 0.0421(19) 0.0267(18) -0.0079(15) -0.0069(14) 0.0169(14) O8 0.046(2) 0.0321(18) 0.032(2) -0.0033(15) -0.0075(16) 0.0179(16) O9 0.0295(18) 0.0242(17) 0.063(2) -0.0020(16) -0.0204(17) 0.0077(14) O1W 0.059(2) 0.0328(18) 0.032(2) -0.0053(15) -0.0119(17) 0.0052(17) O2W 0.161(5) 0.095(4) 0.053(3) -0.036(3) -0.057(3) 0.106(4) O3W 0.048(2) 0.071(3) 0.035(2) -0.0032(19) -0.0151(18) 0.025(2) O4W 0.160(6) 0.058(3) 0.097(4) 0.010(3) -0.052(4) -0.052(3) O5W 0.041(2) 0.051(2) 0.038(2) -0.0223(17) -0.0171(17) 0.0116(17) O6W 0.058(3) 0.080(3) 0.067(3) -0.048(2) -0.037(2) 0.034(2) O7W 0.0372(19) 0.0377(19) 0.038(2) -0.0187(16) -0.0121(16) 0.0082(15) O8W 0.0373(19) 0.051(2) 0.035(2) -0.0221(17) -0.0103(16) 0.0072(17) O9W 0.057(2) 0.0324(18) 0.041(2) -0.0145(16) -0.0120(18) 0.0142(17) O10W 0.152(11) 0.116(9) 0.067(7) 0.013(6) 0.014(7) 0.082(8) O11W 0.096(8) 0.102(8) 0.107(9) -0.039(7) 0.019(7) -0.026(7) N1A 0.0188(17) 0.0138(16) 0.0190(18) -0.0045(14) -0.0024(14) 0.0070(14) N1D 0.0208(18) 0.0191(17) 0.0176(19) -0.0059(14) -0.0121(15) 0.0049(14) N1B 0.0229(18) 0.0233(18) 0.0155(18) -0.0052(15) -0.0127(15) 0.0076(15) N1C 0.0207(18) 0.0196(17) 0.022(2) -0.0089(15) -0.0074(15) 0.0110(14) N2 0.029(2) 0.024(2) 0.047(3) 0.0009(18) -0.0077(19) 0.0093(17) N3 0.026(2) 0.028(2) 0.044(3) -0.0044(19) -0.0113(18) 0.0070(17) N4 0.113(5) 0.035(3) 0.024(2) -0.002(2) -0.012(3) 0.015(3) N5 0.114(5) 0.037(3) 0.033(3) -0.002(2) -0.016(3) 0.008(3) C1A 0.025(2) 0.021(2) 0.023(2) -0.0046(19) -0.0057(19) 0.0056(18) C2A 0.025(2) 0.018(2) 0.028(3) -0.0091(18) -0.0100(19) 0.0044(18) C3A 0.016(2) 0.0168(19) 0.018(2) -0.0042(17) -0.0017(17) 0.0048(16) C1D 0.030(2) 0.032(2) 0.026(3) -0.008(2) -0.012(2) 0.005(2) C2D 0.024(2) 0.029(2) 0.030(3) -0.011(2) -0.015(2) 0.0078(19) C3D 0.021(2) 0.018(2) 0.019(2) -0.0032(17) -0.0048(17) 0.0028(17) C3B 0.020(2) 0.020(2) 0.025(2) -0.0032(18) -0.0022(18) 0.0025(17) C2B 0.034(3) 0.027(2) 0.027(3) -0.007(2) -0.017(2) 0.014(2) C1B 0.034(3) 0.030(2) 0.024(2) -0.006(2) -0.016(2) 0.012(2) C3C 0.021(2) 0.018(2) 0.016(2) -0.0017(17) -0.0034(17) 0.0022(17) C2C 0.024(2) 0.022(2) 0.018(2) -0.0067(18) -0.0052(18) 0.0075(18) C1C 0.015(2) 0.021(2) 0.018(2) -0.0035(17) 0.0014(17) 0.0033(17) C4 0.110(6) 0.042(3) 0.031(3) -0.006(3) -0.019(4) 0.005(4) C5 0.119(6) 0.056(4) 0.031(3) -0.005(3) -0.015(4) 0.016(4) C6 0.046(4) 0.101(5) 0.055(4) 0.043(4) -0.012(3) -0.017(4) C7 0.041(4) 0.178(8) 0.034(4) -0.020(4) -0.002(3) 0.035(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 Cu1A O2D 1.924(3) . ? Cu1A O4A 1.935(3) . ? Cu1A N1D 1.954(3) . ? Cu1A O3A 1.982(3) . ? Cu1A O5 2.396(3) . ? Cu1B O4B 1.892(3) . ? Cu1B O2A 1.893(3) . ? Cu1B N1A 1.942(3) . ? Cu1B O3B 1.955(3) . ? Cu1B O1C 2.613(3) 2_565 ? Cu1C O4C 1.898(3) . ? Cu1C O2B 1.909(3) . ? Cu1C N1B 1.939(3) . ? Cu1C O3C 1.975(3) . ? Cu1C O6 2.585(3) . ? Cu1C O4D 2.731(3) 2_565 ? Cu1D O4D 1.933(3) . ? Cu1D O2C 1.942(3) . ? Cu1D N1C 1.944(3) . ? Cu1D O3D 1.950(3) . ? Cu2 O4C 1.882(3) . ? Cu2 O4D 1.902(3) . ? Cu2 O4B 1.905(3) . ? Cu2 O4A 1.916(3) . ? Cu2 O8 2.554(3) . ? Cu2 Cu1C 3.7316(7) 2_565 ? Cu3 N4 2.012(5) 2_564 ? Cu3 N4 2.012(5) . ? Cu3 N5 2.030(5) . ? Cu3 N5 2.030(5) 2_564 ? Cu3 O5 2.546(3) . ? Cu4 N2 1.998(4) . ? Cu4 N2 1.998(4) 2_675 ? Cu4 N3 2.003(4) 2_675 ? Cu4 N3 2.003(4) . ? Cu4 O9 2.574(3) . ? O1A C1A 1.244(5) . ? O2A C1A 1.260(5) . ? O3A C3A 1.291(5) . ? O4A N1A 1.419(4) . ? O1C C1C 1.245(5) . ? O2C C1C 1.274(5) . ? O3C C3C 1.307(5) . ? O4C N1C 1.402(4) . ? O1B C1B 1.241(5) . ? O2B C1B 1.282(5) . ? O3B C3B 1.288(5) . ? O4B N1B 1.412(4) . ? O1D C1D 1.248(5) . ? O2D C1D 1.280(5) . ? O3D C3D 1.298(5) . ? O4D N1D 1.422(4) . ? O5 H5D 0.8599 . ? O5 H5E 0.9908 . ? O6 H6D 0.8773 . ? O6 H6E 0.9294 . ? O7 H7D 0.8596 . ? O7 H7E 0.8500 . ? O8 H8D 0.9302 . ? O8 H8E 0.8913 . ? O9 H9D 0.8710 . ? O9 H9E 0.8583 . ? O1W H11W 0.9462 . ? O1W H21W 0.9272 . ? O2W H12W 0.9984 . ? O2W H22W 0.8510 . ? O3W H13W 0.9013 . ? O3W H23W 0.8530 . ? O4W H14W 0.7930 . ? O4W H24W 0.8696 . ? O5W H15W 0.8616 . ? O5W H25W 0.9421 . ? O6W H16W 0.8500 . ? O6W H26W 0.8500 . ? O7W H17W 0.9925 . ? O7W H27W 0.9958 . ? O8W H18W 0.9830 . ? O8W H28W 0.9350 . ? O9W H19W 0.8500 . ? O9W H29W 0.9068 . ? O10W H110 0.8504 . ? O10W H510 0.8499 . ? O11W H211 0.8500 . ? O11W H311 0.8505 . ? N1A C3A 1.293(5) . ? N1D C3D 1.294(5) . ? N1B C3B 1.305(5) . ? N1C C3C 1.294(5) . ? N2 C6 1.467(7) . ? N2 H2NA 0.9200 . ? N2 H2NB 0.9200 . ? N3 C7 1.429(7) . ? N3 H3NA 0.9200 . ? N3 H3NB 0.9200 . ? N4 C4 1.476(8) . ? N4 H4NA 0.9200 . ? N4 H4NB 0.9200 . ? N5 C5 1.466(8) . ? N5 H5NA 0.9200 . ? N5 H5NB 0.9200 . ? C1A C2A 1.523(6) . ? C2A C3A 1.507(5) . ? C2A H2A 0.9900 . ? C2A H2B 0.9900 . ? C1D C2D 1.510(6) . ? C2D C3D 1.501(5) . ? C2D H2C 0.9900 . ? C2D H2D 0.9900 . ? C3B C2B 1.510(6) . ? C2B C1B 1.525(6) . ? C2B H2E 0.9900 . ? C2B H2F 0.9900 . ? C3C C2C 1.503(5) . ? C2C C1C 1.531(5) . ? C2C H11G 0.9900 . ? C2C H11H 0.9900 . ? C4 C5 1.501(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.419(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? 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 O2D Cu1A O4A 176.44(12) . . ? O2D Cu1A N1D 91.40(12) . . ? O4A Cu1A N1D 91.61(12) . . ? O2D Cu1A O3A 95.95(11) . . ? O4A Cu1A O3A 80.66(11) . . ? N1D Cu1A O3A 163.61(13) . . ? O2D Cu1A O5 95.22(12) . . ? O4A Cu1A O5 86.03(11) . . ? N1D Cu1A O5 101.91(12) . . ? O3A Cu1A O5 92.01(11) . . ? O4B Cu1B O2A 174.24(13) . . ? O4B Cu1B N1A 89.38(12) . . ? O2A Cu1B N1A 94.10(12) . . ? O4B Cu1B O3B 81.48(11) . . ? O2A Cu1B O3B 94.70(12) . . ? N1A Cu1B O3B 170.02(12) . . ? O4B Cu1B O1C 93.67(11) . 2_565 ? O2A Cu1B O1C 90.93(11) . 2_565 ? N1A Cu1B O1C 89.71(12) . 2_565 ? O3B Cu1B O1C 94.85(11) . 2_565 ? O4C Cu1C O2B 177.07(13) . . ? O4C Cu1C N1B 87.91(12) . . ? O2B Cu1C N1B 93.10(12) . . ? O4C Cu1C O3C 81.18(11) . . ? O2B Cu1C O3C 97.74(11) . . ? N1B Cu1C O3C 169.04(12) . . ? O4C Cu1C O6 95.17(12) . . ? O2B Cu1C O6 87.52(11) . . ? N1B Cu1C O6 93.16(12) . . ? O3C Cu1C O6 88.87(11) . . ? O4C Cu1C O4D 87.26(11) . 2_565 ? O2B Cu1C O4D 90.02(10) . 2_565 ? N1B Cu1C O4D 88.10(12) . 2_565 ? O3C Cu1C O4D 90.34(10) . 2_565 ? O6 Cu1C O4D 177.30(9) . 2_565 ? O4D Cu1D O2C 161.81(12) . . ? O4D Cu1D N1C 90.55(12) . . ? O2C Cu1D N1C 92.20(12) . . ? O4D Cu1D O3D 81.09(11) . . ? O2C Cu1D O3D 98.05(11) . . ? N1C Cu1D O3D 168.84(12) . . ? O4C Cu2 O4D 91.43(11) . . ? O4C Cu2 O4B 88.02(11) . . ? O4D Cu2 O4B 164.71(12) . . ? O4C Cu2 O4A 176.16(12) . . ? O4D Cu2 O4A 91.49(11) . . ? O4B Cu2 O4A 88.51(11) . . ? O4C Cu2 O8 99.70(12) . . ? O4D Cu2 O8 88.45(11) . . ? O4B Cu2 O8 106.70(11) . . ? O4A Cu2 O8 82.87(11) . . ? O4C Cu2 Cu1C 93.53(9) . 2_565 ? O4D Cu2 Cu1C 44.73(8) . 2_565 ? O4B Cu2 Cu1C 120.05(9) . 2_565 ? O4A Cu2 Cu1C 86.80(8) . 2_565 ? O8 Cu2 Cu1C 131.73(7) . 2_565 ? N4 Cu3 N4 180.00(15) 2_564 . ? N4 Cu3 N5 95.1(2) 2_564 . ? N4 Cu3 N5 84.9(2) . . ? N4 Cu3 N5 84.9(2) 2_564 2_564 ? N4 Cu3 N5 95.1(2) . 2_564 ? N5 Cu3 N5 180.000(1) . 2_564 ? N4 Cu3 O5 85.58(14) 2_564 . ? N4 Cu3 O5 94.42(14) . . ? N5 Cu3 O5 94.89(15) . . ? N5 Cu3 O5 85.11(15) 2_564 . ? N2 Cu4 N2 180.0(2) . 2_675 ? N2 Cu4 N3 94.87(16) . 2_675 ? N2 Cu4 N3 85.13(16) 2_675 2_675 ? N2 Cu4 N3 85.13(16) . . ? N2 Cu4 N3 94.87(16) 2_675 . ? N3 Cu4 N3 180.0(2) 2_675 . ? N2 Cu4 O9 87.86(13) . . ? N2 Cu4 O9 92.14(13) 2_675 . ? N3 Cu4 O9 86.46(13) 2_675 . ? N3 Cu4 O9 93.54(13) . . ? C1A O2A Cu1B 128.8(3) . . ? C3A O3A Cu1A 110.5(2) . . ? N1A O4A Cu2 114.7(2) . . ? N1A O4A Cu1A 112.4(2) . . ? Cu2 O4A Cu1A 112.92(13) . . ? C1C O2C Cu1D 124.4(2) . . ? C3C O3C Cu1C 110.1(2) . . ? N1C O4C Cu2 121.3(2) . . ? N1C O4C Cu1C 114.2(2) . . ? Cu2 O4C Cu1C 123.96(14) . . ? C1B O2B Cu1C 127.7(3) . . ? C3B O3B Cu1B 110.5(2) . . ? N1B O4B Cu1B 114.3(2) . . ? N1B O4B Cu2 121.4(2) . . ? Cu1B O4B Cu2 117.18(13) . . ? C1D O2D Cu1A 130.2(3) . . ? C3D O3D Cu1D 109.9(2) . . ? N1D O4D Cu2 116.3(2) . . ? N1D O4D Cu1D 111.4(2) . . ? Cu2 O4D Cu1D 116.32(14) . . ? Cu1A O5 Cu3 149.09(13) . . ? Cu1A O5 H5D 98.1 . . ? Cu3 O5 H5D 95.8 . . ? Cu1A O5 H5E 108.2 . . ? Cu3 O5 H5E 93.2 . . ? H5D O5 H5E 108.7 . . ? Cu1C O6 H6D 113.5 . . ? Cu1C O6 H6E 124.7 . . ? H6D O6 H6E 95.8 . . ? H7D O7 H7E 106.8 . . ? Cu2 O8 H8D 90.3 . . ? Cu2 O8 H8E 93.2 . . ? H8D O8 H8E 102.7 . . ? Cu4 O9 H9D 124.9 . . ? Cu4 O9 H9E 95.3 . . ? H9D O9 H9E 105.8 . . ? H11W O1W H21W 97.3 . . ? H12W O2W H22W 97.8 . . ? H13W O3W H23W 114.9 . . ? H14W O4W H24W 117.0 . . ? H15W O5W H25W 116.8 . . ? H16W O6W H26W 108.9 . . ? H17W O7W H27W 91.3 . . ? H18W O8W H28W 103.2 . . ? H19W O9W H29W 98.0 . . ? H110 O10W H510 118.9 . . ? H211 O11W H311 114.6 . . ? C3A N1A O4A 111.8(3) . . ? C3A N1A Cu1B 129.6(3) . . ? O4A N1A Cu1B 117.9(2) . . ? C3D N1D O4D 110.8(3) . . ? C3D N1D Cu1A 131.8(3) . . ? O4D N1D Cu1A 117.0(2) . . ? C3B N1B O4B 110.1(3) . . ? C3B N1B Cu1C 127.0(3) . . ? O4B N1B Cu1C 118.6(2) . . ? C3C N1C O4C 111.7(3) . . ? C3C N1C Cu1D 131.5(3) . . ? O4C N1C Cu1D 116.6(2) . . ? C6 N2 Cu4 108.1(3) . . ? C6 N2 H2NA 110.1 . . ? Cu4 N2 H2NA 110.1 . . ? C6 N2 H2NB 110.1 . . ? Cu4 N2 H2NB 110.1 . . ? H2NA N2 H2NB 108.4 . . ? C7 N3 Cu4 107.5(3) . . ? C7 N3 H3NA 110.2 . . ? Cu4 N3 H3NA 110.2 . . ? C7 N3 H3NB 110.2 . . ? Cu4 N3 H3NB 110.2 . . ? H3NA N3 H3NB 108.5 . . ? C4 N4 Cu3 108.1(3) . . ? C4 N4 H4NA 110.1 . . ? Cu3 N4 H4NA 110.1 . . ? C4 N4 H4NB 110.1 . . ? Cu3 N4 H4NB 110.1 . . ? H4NA N4 H4NB 108.4 . . ? C5 N5 Cu3 108.1(4) . . ? C5 N5 H5NA 110.1 . . ? Cu3 N5 H5NA 110.1 . . ? C5 N5 H5NB 110.1 . . ? Cu3 N5 H5NB 110.1 . . ? H5NA N5 H5NB 108.4 . . ? O1A C1A O2A 120.8(4) . . ? O1A C1A C2A 115.4(4) . . ? O2A C1A C2A 123.8(4) . . ? C3A C2A C1A 122.8(3) . . ? C3A C2A H2A 106.6 . . ? C1A C2A H2A 106.6 . . ? C3A C2A H2B 106.6 . . ? C1A C2A H2B 106.6 . . ? H2A C2A H2B 106.6 . . ? O3A C3A N1A 123.1(3) . . ? O3A C3A C2A 117.3(3) . . ? N1A C3A C2A 119.7(3) . . ? O1D C1D O2D 122.2(4) . . ? O1D C1D C2D 114.5(4) . . ? O2D C1D C2D 123.3(4) . . ? C3D C2D C1D 122.3(4) . . ? C3D C2D H2C 106.8 . . ? C1D C2D H2C 106.8 . . ? C3D C2D H2D 106.8 . . ? C1D C2D H2D 106.8 . . ? H2C C2D H2D 106.6 . . ? N1D C3D O3D 123.3(4) . . ? N1D C3D C2D 119.9(4) . . ? O3D C3D C2D 116.8(3) . . ? O3B C3B N1B 123.3(4) . . ? O3B C3B C2B 117.8(4) . . ? N1B C3B C2B 118.9(4) . . ? C3B C2B C1B 122.0(4) . . ? C3B C2B H2E 106.8 . . ? C1B C2B H2E 106.8 . . ? C3B C2B H2F 106.8 . . ? C1B C2B H2F 106.8 . . ? H2E C2B H2F 106.7 . . ? O1B C1B O2B 121.7(4) . . ? O1B C1B C2B 116.4(4) . . ? O2B C1B C2B 121.9(4) . . ? N1C C3C O3C 122.3(4) . . ? N1C C3C C2C 119.5(3) . . ? O3C C3C C2C 118.2(3) . . ? C3C C2C C1C 117.7(3) . . ? C3C C2C H11G 107.9 . . ? C1C C2C H11G 107.9 . . ? C3C C2C H11H 107.9 . . ? C1C C2C H11H 107.9 . . ? H11G C2C H11H 107.2 . . ? O1C C1C O2C 122.6(4) . . ? O1C C1C C2C 116.6(4) . . ? O2C C1C C2C 120.7(3) . . ? N4 C4 C5 107.7(5) . . ? N4 C4 H4A 110.2 . . ? C5 C4 H4A 110.2 . . ? N4 C4 H4B 110.2 . . ? C5 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? N5 C5 C4 109.6(6) . . ? N5 C5 H5A 109.8 . . ? C4 C5 H5A 109.8 . . ? N5 C5 H5B 109.8 . . ? C4 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? C7 C6 N2 111.7(5) . . ? C7 C6 H6A 109.3 . . ? N2 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? N2 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C6 C7 N3 112.7(6) . . ? C6 C7 H7A 109.1 . . ? N3 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? N3 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4B Cu1B O2A C1A 124.4(11) . . . . ? N1A Cu1B O2A C1A -2.7(4) . . . . ? O3B Cu1B O2A C1A 172.6(4) . . . . ? O1C Cu1B O2A C1A -92.5(4) 2_565 . . . ? O2D Cu1A O3A C3A -169.5(3) . . . . ? O4A Cu1A O3A C3A 9.4(3) . . . . ? N1D Cu1A O3A C3A -53.3(6) . . . . ? O5 Cu1A O3A C3A 95.0(3) . . . . ? O4C Cu2 O4A N1A 59.2(19) . . . . ? O4D Cu2 O4A N1A -161.3(2) . . . . ? O4B Cu2 O4A N1A 34.0(2) . . . . ? O8 Cu2 O4A N1A -73.0(2) . . . . ? Cu1C Cu2 O4A N1A 154.2(2) 2_565 . . . ? O4C Cu2 O4A Cu1A -170.2(18) . . . . ? O4D Cu2 O4A Cu1A -30.65(15) . . . . ? O4B Cu2 O4A Cu1A 164.64(15) . . . . ? O8 Cu2 O4A Cu1A 57.61(14) . . . . ? Cu1C Cu2 O4A Cu1A -75.15(12) 2_565 . . . ? O2D Cu1A O4A N1A 7(2) . . . . ? N1D Cu1A O4A N1A 154.0(2) . . . . ? O3A Cu1A O4A N1A -11.5(2) . . . . ? O5 Cu1A O4A N1A -104.2(2) . . . . ? O2D Cu1A O4A Cu2 -125(2) . . . . ? N1D Cu1A O4A Cu2 22.23(16) . . . . ? O3A Cu1A O4A Cu2 -143.24(16) . . . . ? O5 Cu1A O4A Cu2 124.06(14) . . . . ? O4D Cu1D O2C C1C -83.9(5) . . . . ? N1C Cu1D O2C C1C 14.6(3) . . . . ? O3D Cu1D O2C C1C -169.9(3) . . . . ? O4C Cu1C O3C C3C -5.0(3) . . . . ? O2B Cu1C O3C C3C 172.2(3) . . . . ? N1B Cu1C O3C C3C 0.4(8) . . . . ? O6 Cu1C O3C C3C -100.4(3) . . . . ? O4D Cu1C O3C C3C 82.2(3) 2_565 . . . ? O4D Cu2 O4C N1C 6.7(3) . . . . ? O4B Cu2 O4C N1C 171.4(3) . . . . ? O4A Cu2 O4C N1C 146.2(17) . . . . ? O8 Cu2 O4C N1C -82.0(3) . . . . ? Cu1C Cu2 O4C N1C 51.4(3) 2_565 . . . ? O4D Cu2 O4C Cu1C -164.9(2) . . . . ? O4B Cu2 O4C Cu1C -0.2(2) . . . . ? O4A Cu2 O4C Cu1C -25(2) . . . . ? O8 Cu2 O4C Cu1C 106.45(19) . . . . ? Cu1C Cu2 O4C Cu1C -120.15(18) 2_565 . . . ? O2B Cu1C O4C N1C -63(3) . . . . ? N1B Cu1C O4C N1C -173.0(3) . . . . ? O3C Cu1C O4C N1C 5.9(2) . . . . ? O6 Cu1C O4C N1C 94.0(3) . . . . ? O4D Cu1C O4C N1C -84.8(3) 2_565 . . . ? O2B Cu1C O4C Cu2 109(2) . . . . ? N1B Cu1C O4C Cu2 -1.0(2) . . . . ? O3C Cu1C O4C Cu2 178.0(2) . . . . ? O6 Cu1C O4C Cu2 -93.95(19) . . . . ? O4D Cu1C O4C Cu2 87.23(19) 2_565 . . . ? O4C Cu1C O2B C1B -119(2) . . . . ? N1B Cu1C O2B C1B -8.9(4) . . . . ? O3C Cu1C O2B C1B 172.7(4) . . . . ? O6 Cu1C O2B C1B 84.1(4) . . . . ? O4D Cu1C O2B C1B -97.0(4) 2_565 . . . ? O4B Cu1B O3B C3B 3.8(3) . . . . ? O2A Cu1B O3B C3B -171.8(3) . . . . ? N1A Cu1B O3B C3B -20.1(9) . . . . ? O1C Cu1B O3B C3B 96.8(3) 2_565 . . . ? O2A Cu1B O4B N1B 43.5(13) . . . . ? N1A Cu1B O4B N1B 170.7(2) . . . . ? O3B Cu1B O4B N1B -5.2(2) . . . . ? O1C Cu1B O4B N1B -99.6(2) 2_565 . . . ? O2A Cu1B O4B Cu2 -107.6(11) . . . . ? N1A Cu1B O4B Cu2 19.68(18) . . . . ? O3B Cu1B O4B Cu2 -156.29(18) . . . . ? O1C Cu1B O4B Cu2 109.35(16) 2_565 . . . ? O4C Cu2 O4B N1B 1.9(3) . . . . ? O4D Cu2 O4B N1B 90.0(5) . . . . ? O4A Cu2 O4B N1B -179.7(3) . . . . ? O8 Cu2 O4B N1B -97.6(3) . . . . ? Cu1C Cu2 O4B N1B 94.8(3) 2_565 . . . ? O4C Cu2 O4B Cu1B 150.78(18) . . . . ? O4D Cu2 O4B Cu1B -121.1(4) . . . . ? O4A Cu2 O4B Cu1B -30.86(17) . . . . ? O8 Cu2 O4B Cu1B 51.25(18) . . . . ? Cu1C Cu2 O4B Cu1B -116.30(13) 2_565 . . . ? O4A Cu1A O2D C1D 151.7(19) . . . . ? N1D Cu1A O2D C1D 4.2(4) . . . . ? O3A Cu1A O2D C1D 169.6(4) . . . . ? O5 Cu1A O2D C1D -97.8(4) . . . . ? O4D Cu1D O3D C3D 14.5(3) . . . . ? O2C Cu1D O3D C3D 176.1(3) . . . . ? N1C Cu1D O3D C3D -27.3(8) . . . . ? O4C Cu2 O4D N1D -151.5(2) . . . . ? O4B Cu2 O4D N1D 120.8(4) . . . . ? O4A Cu2 O4D N1D 31.0(2) . . . . ? O8 Cu2 O4D N1D -51.8(2) . . . . ? Cu1C Cu2 O4D N1D 115.0(3) 2_565 . . . ? O4C Cu2 O4D Cu1D -17.19(16) . . . . ? O4B Cu2 O4D Cu1D -104.9(4) . . . . ? O4A Cu2 O4D Cu1D 165.30(15) . . . . ? O8 Cu2 O4D Cu1D 82.47(15) . . . . ? Cu1C Cu2 O4D Cu1D -110.76(16) 2_565 . . . ? O2C Cu1D O4D N1D -105.4(4) . . . . ? N1C Cu1D O4D N1D 155.8(2) . . . . ? O3D Cu1D O4D N1D -16.7(2) . . . . ? O2C Cu1D O4D Cu2 118.2(3) . . . . ? N1C Cu1D O4D Cu2 19.46(16) . . . . ? O3D Cu1D O4D Cu2 -153.12(16) . . . . ? O2D Cu1A O5 Cu3 26.2(3) . . . . ? O4A Cu1A O5 Cu3 -157.2(3) . . . . ? N1D Cu1A O5 Cu3 -66.4(3) . . . . ? O3A Cu1A O5 Cu3 122.3(3) . . . . ? N4 Cu3 O5 Cu1A -71.5(3) 2_564 . . . ? N4 Cu3 O5 Cu1A 108.5(3) . . . . ? N5 Cu3 O5 Cu1A -166.3(3) . . . . ? N5 Cu3 O5 Cu1A 13.7(3) 2_564 . . . ? Cu2 O4A N1A C3A 142.6(3) . . . . ? Cu1A O4A N1A C3A 11.8(4) . . . . ? Cu2 O4A N1A Cu1B -28.2(3) . . . . ? Cu1A O4A N1A Cu1B -159.09(16) . . . . ? O4B Cu1B N1A C3A -163.6(4) . . . . ? O2A Cu1B N1A C3A 11.8(4) . . . . ? O3B Cu1B N1A C3A -140.0(7) . . . . ? O1C Cu1B N1A C3A 102.7(4) 2_565 . . . ? O4B Cu1B N1A O4A 5.3(3) . . . . ? O2A Cu1B N1A O4A -179.3(2) . . . . ? O3B Cu1B N1A O4A 29.0(9) . . . . ? O1C Cu1B N1A O4A -88.3(2) 2_565 . . . ? Cu2 O4D N1D C3D 152.5(3) . . . . ? Cu1D O4D N1D C3D 16.1(4) . . . . ? Cu2 O4D N1D Cu1A -20.8(3) . . . . ? Cu1D O4D N1D Cu1A -157.21(16) . . . . ? O2D Cu1A N1D C3D 5.2(4) . . . . ? O4A Cu1A N1D C3D -172.9(4) . . . . ? O3A Cu1A N1D C3D -111.6(5) . . . . ? O5 Cu1A N1D C3D 100.8(4) . . . . ? O2D Cu1A N1D O4D 176.8(3) . . . . ? O4A Cu1A N1D O4D -1.3(3) . . . . ? O3A Cu1A N1D O4D 60.0(5) . . . . ? O5 Cu1A N1D O4D -87.6(3) . . . . ? Cu1B O4B N1B C3B 5.6(4) . . . . ? Cu2 O4B N1B C3B 155.4(3) . . . . ? Cu1B O4B N1B Cu1C -152.77(17) . . . . ? Cu2 O4B N1B Cu1C -3.1(4) . . . . ? O4C Cu1C N1B C3B -152.1(3) . . . . ? O2B Cu1C N1B C3B 30.6(4) . . . . ? O3C Cu1C N1B C3B -157.5(6) . . . . ? O6 Cu1C N1B C3B -57.1(3) . . . . ? O4D Cu1C N1B C3B 120.5(3) 2_565 . . . ? O4C Cu1C N1B O4B 2.2(3) . . . . ? O2B Cu1C N1B O4B -175.0(3) . . . . ? O3C Cu1C N1B O4B -3.1(9) . . . . ? O6 Cu1C N1B O4B 97.3(3) . . . . ? O4D Cu1C N1B O4B -85.1(3) 2_565 . . . ? Cu2 O4C N1C C3C -178.1(3) . . . . ? Cu1C O4C N1C C3C -5.8(4) . . . . ? Cu2 O4C N1C Cu1D 6.1(4) . . . . ? Cu1C O4C N1C Cu1D 178.39(16) . . . . ? O4D Cu1D N1C C3C 170.3(4) . . . . ? O2C Cu1D N1C C3C 8.3(4) . . . . ? O3D Cu1D N1C C3C -148.5(6) . . . . ? O4D Cu1D N1C O4C -14.9(3) . . . . ? O2C Cu1D N1C O4C -176.9(3) . . . . ? O3D Cu1D N1C O4C 26.3(9) . . . . ? N2 Cu4 N2 C6 162(100) 2_675 . . . ? N3 Cu4 N2 C6 173.2(4) 2_675 . . . ? N3 Cu4 N2 C6 -6.8(4) . . . . ? O9 Cu4 N2 C6 87.0(4) . . . . ? N2 Cu4 N3 C7 -15.3(5) . . . . ? N2 Cu4 N3 C7 164.7(5) 2_675 . . . ? N3 Cu4 N3 C7 -1(100) 2_675 . . . ? O9 Cu4 N3 C7 -102.8(5) . . . . ? N4 Cu3 N4 C4 172(100) 2_564 . . . ? N5 Cu3 N4 C4 17.4(4) . . . . ? N5 Cu3 N4 C4 -162.6(4) 2_564 . . . ? O5 Cu3 N4 C4 111.9(3) . . . . ? N4 Cu3 N5 C5 -169.7(4) 2_564 . . . ? N4 Cu3 N5 C5 10.3(4) . . . . ? N5 Cu3 N5 C5 49(100) 2_564 . . . ? O5 Cu3 N5 C5 -83.7(4) . . . . ? Cu1B O2A C1A O1A 179.7(3) . . . . ? Cu1B O2A C1A C2A -2.1(6) . . . . ? O1A C1A C2A C3A 179.5(4) . . . . ? O2A C1A C2A C3A 1.2(7) . . . . ? Cu1A O3A C3A N1A -5.7(5) . . . . ? Cu1A O3A C3A C2A 174.6(3) . . . . ? O4A N1A C3A O3A -3.9(5) . . . . ? Cu1B N1A C3A O3A 165.6(3) . . . . ? O4A N1A C3A C2A 175.8(3) . . . . ? Cu1B N1A C3A C2A -14.7(6) . . . . ? C1A C2A C3A O3A -173.0(4) . . . . ? C1A C2A C3A N1A 7.3(6) . . . . ? Cu1A O2D C1D O1D 174.3(4) . . . . ? Cu1A O2D C1D C2D -5.5(7) . . . . ? O1D C1D C2D C3D 178.2(4) . . . . ? O2D C1D C2D C3D -2.0(7) . . . . ? O4D N1D C3D O3D -3.9(5) . . . . ? Cu1A N1D C3D O3D 168.1(3) . . . . ? O4D N1D C3D C2D 175.9(3) . . . . ? Cu1A N1D C3D C2D -12.2(6) . . . . ? Cu1D O3D C3D N1D -10.0(5) . . . . ? Cu1D O3D C3D C2D 170.2(3) . . . . ? C1D C2D C3D N1D 10.6(6) . . . . ? C1D C2D C3D O3D -169.6(4) . . . . ? Cu1B O3B C3B N1B -1.7(5) . . . . ? Cu1B O3B C3B C2B 179.0(3) . . . . ? O4B N1B C3B O3B -2.5(5) . . . . ? Cu1C N1B C3B O3B 153.7(3) . . . . ? O4B N1B C3B C2B 176.8(4) . . . . ? Cu1C N1B C3B C2B -27.0(5) . . . . ? O3B C3B C2B C1B 176.5(4) . . . . ? N1B C3B C2B C1B -2.8(7) . . . . ? Cu1C O2B C1B O1B 168.6(3) . . . . ? Cu1C O2B C1B C2B -13.5(6) . . . . ? C3B C2B C1B O1B -157.9(4) . . . . ? C3B C2B C1B O2B 24.1(7) . . . . ? O4C N1C C3C O3C 1.4(5) . . . . ? Cu1D N1C C3C O3C 176.4(3) . . . . ? O4C N1C C3C C2C -178.1(3) . . . . ? Cu1D N1C C3C C2C -3.2(6) . . . . ? Cu1C O3C C3C N1C 3.4(5) . . . . ? Cu1C O3C C3C C2C -177.1(3) . . . . ? N1C C3C C2C C1C -22.1(6) . . . . ? O3C C3C C2C C1C 158.3(4) . . . . ? Cu1D O2C C1C O1C 142.9(3) . . . . ? Cu1D O2C C1C C2C -41.2(5) . . . . ? C3C C2C C1C O1C -137.5(4) . . . . ? C3C C2C C1C O2C 46.3(5) . . . . ? Cu3 N4 C4 C5 -41.2(5) . . . . ? Cu3 N5 C5 C4 -36.0(6) . . . . ? N4 C4 C5 N5 51.8(6) . . . . ? Cu4 N2 C6 C7 28.5(7) . . . . ? N2 C6 C7 N3 -44.0(9) . . . . ? Cu4 N3 C7 C6 36.1(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 O5 H5D O3C 0.86 1.90 2.755(4) 177.7 2_565 O5 H5E O9W 0.99 1.77 2.759(4) 171.9 2_665 O6 H6D O1A 0.88 1.85 2.697(4) 161.1 2 O6 H6E O1W 0.93 2.09 2.996(5) 165.1 . O7 H7D O3D 0.86 1.94 2.802(4) 176.5 2_465 O7 H7E O3W 0.85 1.92 2.761(5) 170.8 1_455 O8 H8D O1A 0.93 1.81 2.734(5) 172.2 2 O8 H8E O7 0.89 1.98 2.864(4) 175.4 . O9 H9D O2C 0.87 2.04 2.908(4) 173.8 1_655 O9 H9E O8 0.86 2.56 3.410(5) 171.0 2_565 O1W H11W O5W 0.95 1.87 2.812(5) 176.4 2_566 O1W H21W O5W 0.93 2.20 2.846(5) 125.8 1_545 O2W H12W O1B 1.00 1.89 2.667(5) 132.8 . O2W H22W O7W 0.85 2.07 2.752(5) 136.3 2_666 O3W H13W O6 0.90 1.96 2.852(5) 169.4 1_655 O3W H23W O10W 0.85 1.97 2.656(11) 137.0 . O4W H14W O11W 0.79 2.17 2.673(13) 122.0 . O4W H14W O2W 0.79 2.51 3.304(8) 175.8 . O4W H24W O8W 0.87 1.85 2.718(6) 171.9 1_545 O5W H15W O3A 0.86 2.05 2.803(4) 145.9 2_565 O5W H25W O6W 0.94 1.84 2.721(5) 155.0 . O6W H16W O2W 0.85 2.09 2.881(8) 155.1 1_565 O6W H26W O4W 0.85 1.88 2.733(7) 179.9 2_666 O7W H17W O1D 0.99 1.94 2.667(4) 127.8 2_565 O7W H27W O6W 1.00 1.87 2.792(5) 153.0 . O8W H18W O1C 0.98 1.78 2.763(4) 173.0 1_655 O8W H28W O7W 0.93 1.81 2.747(5) 177.2 . O9W H19W O1W 0.85 2.07 2.880(5) 160.2 2_666 O9W H29W O8W 0.91 1.86 2.740(5) 161.7 . O10W H110 O1D 0.85 2.12 2.972(11) 179.3 2_565 O11W H211 O1A 0.85 2.64 3.261(12) 130.7 2_655 O11W H311 O2W 0.85 1.56 2.411(12) 179.5 . N2 H2NA O3B 0.92 2.03 2.944(4) 171.4 1_565 N2 H2NB O8 0.92 2.33 3.243(5) 174.6 2_565 N3 H3NA O1C 0.92 2.06 2.963(5) 165.8 1_655 N3 H3NB O11W 0.92 2.42 3.003(11) 121.7 1_565 N4 H4NA O1W 0.92 2.46 3.293(5) 151.0 2_565 N4 H4NB O3C 0.92 2.26 3.116(5) 155.3 2_565 N5 H5NA O9W 0.92 2.20 3.038(6) 151.7 2_665 N5 H5NB O2B 0.92 2.51 3.168(5) 129.0 1_554 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.050 _refine_diff_density_min -1.097 _refine_diff_density_rms 0.119