# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Tang, Wen-Xia' 'Gao, Song' 'Li, Dong-Feng' 'Okamura, Taka-aki' 'Sun, Wei-Yin' 'Ueyama, Norikazu' 'Zheng, Li-Min' _publ_contact_author_name ' Prof. Wen-Xia Tang' _publ_contact_author_address ; Coordination Chemistry Institute, Nanjing University Nanjing 210093 CHINA ; _publ_contact_author_email ' wxtang@netra.nju.edu.cn' _publ_contact_author_fax ' 86-25-3314502' _publ_contact_author_phone ' 86-25-3595706' _publ_section_title ; A novel Cu(II)-W(V) bimetallic ferromagnet, {[Cu(en)2]3[W(CN)8]2.H2O}oo (en = ethylenediamine), with cube-like W8Cu12 units from a coordinated anion template self-assembly reaction ; data_Cu3W2 _database_code_CSD 169196 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H50 Cu3 N28 O W2' _chemical_formula_weight 1353.28 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4759(12) _cell_length_b 14.7380(16) _cell_length_c 15.3325(17) _cell_angle_alpha 87.479(2) _cell_angle_beta 87.473(2) _cell_angle_gamma 88.683(2) _cell_volume 2362.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Dark-blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.903 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1314 _exptl_absorpt_coefficient_mu 6.238 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.276 _exptl_absorpt_correction_T_max 0.418 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14855 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.1065 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.00 _reflns_number_total 10407 _reflns_number_gt 7139 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0000P)^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_number_reflns 10407 _refine_ls_number_parameters 547 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _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 W1 W 0.00424(3) 0.74784(2) 0.243053(19) 0.02637(8) Uani 1 1 d . . . W2 W 0.46187(3) 0.23404(2) 0.25132(2) 0.03923(10) Uani 1 1 d . . . Cu1 Cu 0.50054(9) 0.79050(7) 0.25850(6) 0.0434(3) Uani 1 1 d . F . Cu2 Cu 0.0000 1.0000 0.5000 0.0366(3) Uani 1 2 d S . . Cu3 Cu 0.0000 0.5000 0.0000 0.0425(4) Uani 1 2 d S . . Cu4 Cu 0.0000 0.0000 0.0000 0.0532(4) Uani 1 2 d S . . Cu5 Cu 0.0000 0.5000 0.5000 0.1101(8) Uani 1 2 d SD . . C1 C 0.1924(7) 0.7685(5) 0.2918(5) 0.039(2) Uani 1 1 d . . . N1 N 0.2916(6) 0.7779(5) 0.3153(4) 0.0508(19) Uani 1 1 d . . . C2 C 0.1067(7) 0.6193(6) 0.2447(5) 0.042(2) Uani 1 1 d . . . N2 N 0.1583(8) 0.5514(5) 0.2492(5) 0.082(3) Uani 1 1 d . . . C3 C -0.0179(7) 0.8745(5) 0.3138(5) 0.040(2) Uani 1 1 d . . . N3 N -0.0295(7) 0.9370(5) 0.3512(4) 0.058(2) Uani 1 1 d . . . C4 C -0.0216(7) 0.7048(5) 0.3781(5) 0.042(2) Uani 1 1 d . . . N4 N -0.0396(8) 0.6779(5) 0.4489(5) 0.070(2) Uani 1 1 d . . . C5 C 0.0911(7) 0.8478(5) 0.1534(5) 0.0344(19) Uani 1 1 d . . . N5 N 0.1373(6) 0.8992(5) 0.1066(4) 0.0522(19) Uani 1 1 d . . . C6 C -0.1439(7) 0.6496(5) 0.2508(5) 0.041(2) Uani 1 1 d . . . N6 N -0.2250(6) 0.5973(5) 0.2577(5) 0.057(2) Uani 1 1 d . . . C7 C -0.1657(7) 0.8171(5) 0.1963(5) 0.0343(19) Uani 1 1 d . . . N7 N -0.2560(6) 0.8512(5) 0.1709(5) 0.059(2) Uani 1 1 d . . . C8 C -0.0008(7) 0.6984(5) 0.1132(5) 0.0362(19) Uani 1 1 d . . . N8 N -0.0010(6) 0.6689(4) 0.0458(4) 0.0523(19) Uani 1 1 d . . . C10 C 0.4673(9) 0.3812(7) 0.2371(6) 0.062(3) Uani 1 1 d . E . N10 N 0.4721(8) 0.4574(6) 0.2296(6) 0.099(3) Uani 1 1 d . . . C11 C 0.3659(8) 0.2669(6) 0.1330(6) 0.063(3) Uani 1 1 d . E . C13 C 0.6066(8) 0.1378(6) 0.2952(7) 0.072(3) Uani 1 1 d . E . C15 C 0.2754(8) 0.2811(6) 0.2938(6) 0.068(3) Uani 1 1 d . E . C16 C 0.5087(8) 0.2778(6) 0.3771(6) 0.057(3) Uani 1 1 d . E . N16 N 0.5311(9) 0.3015(6) 0.4456(5) 0.089(3) Uani 1 1 d . . . N17 N 0.5865(6) 0.7413(5) 0.3673(4) 0.063(2) Uani 1 1 d . . . H17C H 0.5295 0.7113 0.4028 0.076 Uiso 1 1 calc R . . H17D H 0.6502 0.7022 0.3524 0.076 Uiso 1 1 calc R . . C17 C 0.6381(9) 0.8175(8) 0.4131(6) 0.081(4) Uani 1 1 d . . . H17A H 0.6515 0.7998 0.4738 0.097 Uiso 1 1 calc R . . H17B H 0.7190 0.8362 0.3856 0.097 Uiso 1 1 calc R . . C18 C 0.5430(8) 0.8917(7) 0.4072(6) 0.071(3) Uani 1 1 d . . . H18A H 0.5760 0.9460 0.4308 0.086 Uiso 1 1 calc R . . H18B H 0.4657 0.8751 0.4407 0.086 Uiso 1 1 calc R . . N18 N 0.5149(6) 0.9088(4) 0.3145(5) 0.063(2) Uani 1 1 d . . . H18C H 0.5778 0.9412 0.2872 0.075 Uiso 1 1 calc R . . H18D H 0.4412 0.9410 0.3103 0.075 Uiso 1 1 calc R . . N19 N 0.4488(6) 0.8451(5) 0.1435(4) 0.062(2) Uani 1 1 d . . . H19E H 0.3807 0.8829 0.1502 0.075 Uiso 0.50 1 calc PR A 1 H19F H 0.5134 0.8758 0.1163 0.075 Uiso 0.50 1 calc PR A 1 H19G H 0.3663 0.8630 0.1498 0.075 Uiso 0.50 1 d PR A 2 H19H H 0.4947 0.8954 0.1320 0.075 Uiso 0.50 1 d PR A 2 N20 N 0.5038(7) 0.6730(5) 0.1990(5) 0.078(2) Uani 1 1 d . . . H20E H 0.5721 0.6395 0.2157 0.094 Uiso 0.50 1 calc PR B 1 H20F H 0.4331 0.6420 0.2156 0.094 Uiso 0.50 1 calc PR B 1 H20G H 0.5843 0.6529 0.1875 0.094 Uiso 0.50 1 d PR B 2 H20H H 0.4608 0.6301 0.2310 0.094 Uiso 0.50 1 d PR B 2 N21 N 0.1782(5) 0.9453(4) 0.5064(4) 0.0463(18) Uani 1 1 d . . . H21A H 0.2228 0.9567 0.4558 0.056 Uiso 1 1 calc R . . H21B H 0.2194 0.9696 0.5497 0.056 Uiso 1 1 calc R . . C21 C 0.1671(7) 0.8466(5) 0.5231(5) 0.043(2) Uani 1 1 d . . . H21C H 0.2465 0.8209 0.5445 0.052 Uiso 1 1 calc R . . H21D H 0.1488 0.8175 0.4697 0.052 Uiso 1 1 calc R . . C22 C -0.0611(7) 1.1682(5) 0.4103(5) 0.047(2) Uani 1 1 d . . . H22C H -0.0837 1.1452 0.3548 0.057 Uiso 1 1 calc R . . H22D H -0.0448 1.2326 0.4018 0.057 Uiso 1 1 calc R . . N22 N 0.0529(5) 1.1199(4) 0.4420(4) 0.0419(17) Uani 1 1 d . . . H22A H 0.0910 1.1536 0.4805 0.050 Uiso 1 1 calc R . . H22B H 0.1090 1.1102 0.3970 0.050 Uiso 1 1 calc R . . N23 N -0.1376(6) 0.4666(4) 0.0899(4) 0.0532(19) Uani 1 1 d . . . H23A H -0.1410 0.4058 0.0972 0.064 Uiso 1 1 calc R . . H23B H -0.1202 0.4895 0.1415 0.064 Uiso 1 1 calc R . . C23 C -0.2601(8) 0.5032(7) 0.0610(6) 0.071(3) Uani 1 1 d . . . H23C H -0.3295 0.4697 0.0901 0.085 Uiso 1 1 calc R . . H23D H -0.2699 0.5664 0.0754 0.085 Uiso 1 1 calc R . . C24 C 0.2635(8) 0.5049(6) 0.0328(7) 0.072(3) Uani 1 1 d . . . H24C H 0.2648 0.5683 0.0470 0.086 Uiso 1 1 calc R . . H24D H 0.3396 0.4746 0.0548 0.086 Uiso 1 1 calc R . . N24 N 0.1486(6) 0.4622(4) 0.0723(4) 0.0500(18) Uani 1 1 d . . . H24A H 0.1347 0.4799 0.1274 0.060 Uiso 1 1 calc R . . H24B H 0.1586 0.4013 0.0738 0.060 Uiso 1 1 calc R . . N25 N 0.1094(6) 0.1010(5) 0.0400(4) 0.063(2) Uani 1 1 d . . . H25E H 0.1762 0.0776 0.0690 0.075 Uiso 0.50 1 calc PR C 1 H25F H 0.1392 0.1352 -0.0062 0.075 Uiso 0.50 1 calc PR C 1 H25G H 0.1914 0.0818 0.0415 0.075 Uiso 0.50 1 d PR C 2 H25H H 0.1053 0.1490 0.0018 0.075 Uiso 0.50 1 d PR C 2 N26 N -0.1241(6) 0.0392(5) 0.0952(4) 0.059(2) Uani 1 1 d . . . H26E H -0.1889 0.0722 0.0724 0.071 Uiso 0.50 1 calc PR D 1 H26F H -0.1565 -0.0095 0.1251 0.071 Uiso 0.50 1 calc PR D 1 H26G H -0.2044 0.0407 0.0764 0.071 Uiso 0.50 1 d PR D 2 H26H H -0.1206 -0.0002 0.1416 0.071 Uiso 0.50 1 d PR D 2 C9A C 0.6250(15) 0.2602(10) 0.1604(11) 0.030(4) Uiso 0.50 1 d P E 1 N9A N 0.7152(13) 0.2778(9) 0.1197(8) 0.041(3) Uiso 0.50 1 d P E 1 N11A N 0.2955(16) 0.2682(12) 0.0751(12) 0.060(5) Uiso 0.50 1 d P E 1 C12A C 0.4258(19) 0.1175(13) 0.1704(12) 0.056(5) Uiso 0.50 1 d P E 1 N12A N 0.4124(16) 0.0567(12) 0.1297(11) 0.081(5) Uiso 0.50 1 d P E 1 N13A N 0.6894(12) 0.0857(9) 0.3037(9) 0.032(3) Uiso 0.50 1 d P E 1 C14A C 0.3518(17) 0.1236(13) 0.3011(11) 0.046(5) Uiso 0.50 1 d P E 1 N14A N 0.2993(16) 0.0599(12) 0.3310(12) 0.085(6) Uiso 0.50 1 d P E 1 N15A N 0.1628(15) 0.2995(11) 0.2986(11) 0.056(5) Uiso 0.50 1 d P E 1 C9B C 0.645(3) 0.2750(17) 0.1994(16) 0.088(8) Uiso 0.50 1 d P E 2 N9B N 0.744(2) 0.2954(16) 0.1773(17) 0.144(9) Uiso 0.50 1 d P E 2 N11B N 0.3349(18) 0.3002(12) 0.0628(12) 0.069(6) Uiso 0.50 1 d P E 2 C12B C 0.515(2) 0.1293(15) 0.1659(14) 0.077(7) Uiso 0.50 1 d P E 2 N12B N 0.534(2) 0.0694(15) 0.1205(13) 0.120(7) Uiso 0.50 1 d P E 2 N13B N 0.6616(18) 0.0854(14) 0.3459(12) 0.090(7) Uiso 0.50 1 d P E 2 C14B C 0.3785(14) 0.1287(10) 0.3404(10) 0.027(4) Uiso 0.50 1 d P E 2 N14B N 0.3333(11) 0.0730(8) 0.3807(8) 0.033(3) Uiso 0.50 1 d P E 2 N15B N 0.1883(18) 0.3112(12) 0.3375(11) 0.068(5) Uiso 0.50 1 d P E 2 C19A C 0.4118(16) 0.7538(13) 0.0870(12) 0.044(5) Uiso 0.50 1 d P F 1 H19A H 0.3277 0.7321 0.1053 0.052 Uiso 0.50 1 calc PR F 1 H19B H 0.4134 0.7688 0.0247 0.052 Uiso 0.50 1 calc PR F 1 C20A C 0.5098(16) 0.6862(12) 0.1078(11) 0.045(5) Uiso 0.50 1 d P F 1 H20A H 0.4939 0.6298 0.0801 0.054 Uiso 0.50 1 calc PR F 1 H20B H 0.5934 0.7075 0.0876 0.054 Uiso 0.50 1 calc PR F 1 C19B C 0.459(2) 0.7927(14) 0.0772(13) 0.070(7) Uiso 0.50 1 d P F 2 H19C H 0.5427 0.7983 0.0484 0.084 Uiso 0.50 1 calc PR F 2 H19D H 0.3951 0.8104 0.0353 0.084 Uiso 0.50 1 calc PR F 2 C20B C 0.439(2) 0.6978(17) 0.1099(15) 0.084(7) Uiso 0.50 1 d P F 2 H20C H 0.4732 0.6571 0.0661 0.101 Uiso 0.50 1 calc PR F 2 H20D H 0.3481 0.6876 0.1175 0.101 Uiso 0.50 1 calc PR F 2 C25A C 0.019(2) 0.1605(15) 0.1026(14) 0.071(7) Uiso 0.50 1 d P G 1 H25A H 0.0699 0.1978 0.1380 0.085 Uiso 0.50 1 calc PR G 1 H25B H -0.0375 0.1997 0.0689 0.085 Uiso 0.50 1 calc PR G 1 C26A C -0.0500(18) 0.0964(13) 0.1552(11) 0.047(5) Uiso 0.50 1 d P G 1 H26A H -0.1085 0.1272 0.1955 0.057 Uiso 0.50 1 calc PR G 1 H26B H 0.0078 0.0580 0.1889 0.057 Uiso 0.50 1 calc PR G 1 C25B C 0.0634(19) 0.1330(17) 0.1174(15) 0.076(8) Uiso 0.50 1 d P G 2 H25C H 0.0814 0.1970 0.1202 0.091 Uiso 0.50 1 calc PR G 2 H25D H 0.1037 0.1004 0.1656 0.091 Uiso 0.50 1 calc PR G 2 C26B C -0.087(3) 0.118(2) 0.1239(19) 0.109(10) Uiso 0.50 1 d P G 2 H26C H -0.1169 0.1224 0.1844 0.131 Uiso 0.50 1 calc PR G 2 H26D H -0.1285 0.1671 0.0905 0.131 Uiso 0.50 1 calc PR G 2 N27A N 0.1802(13) 0.4891(18) 0.4510(18) 0.098(9) Uiso 0.50 1 d PD H 1 H27E H 0.1974 0.4321 0.4343 0.117 Uiso 0.50 1 calc PR H 1 H27F H 0.1923 0.5276 0.4043 0.117 Uiso 0.50 1 calc PR H 1 C27A C 0.257(5) 0.510(3) 0.516(3) 0.158(16) Uiso 0.50 1 d PD H 1 H27A H 0.3352 0.5357 0.4902 0.189 Uiso 0.50 1 calc PR H 1 H27B H 0.2805 0.4547 0.5485 0.189 Uiso 0.50 1 calc PR H 1 N27B N 0.1530(17) 0.470(2) 0.4240(15) 0.153(15) Uiso 0.50 1 d PD H 2 H27G H 0.1573 0.4090 0.4188 0.184 Uiso 0.50 1 calc PR H 2 H27H H 0.1423 0.4952 0.3703 0.184 Uiso 0.50 1 calc PR H 2 C27B C 0.270(3) 0.498(2) 0.4537(16) 0.165(14) Uiso 0.50 1 d PD H 2 H27C H 0.2961 0.5521 0.4199 0.199 Uiso 0.50 1 calc PR H 2 H27D H 0.3345 0.4508 0.4431 0.199 Uiso 0.50 1 calc PR H 2 C28A C 0.2013(18) 0.5751(13) 0.5793(12) 0.061(5) Uiso 0.50 1 d PD H 1 H28A H 0.2045 0.6362 0.5530 0.073 Uiso 0.50 1 calc PR H 1 H28B H 0.2520 0.5734 0.6308 0.073 Uiso 0.50 1 calc PR H 1 N28A N 0.0640(13) 0.5533(9) 0.6062(7) 0.056(4) Uiso 0.50 1 d PD H 1 H28E H 0.0189 0.6039 0.6198 0.067 Uiso 0.50 1 calc PR H 1 H28F H 0.0601 0.5132 0.6522 0.067 Uiso 0.50 1 calc PR H 1 C28B C 0.266(3) 0.518(3) 0.5476(16) 0.111(13) Uiso 0.50 1 d PD H 2 H28C H 0.2958 0.4647 0.5814 0.133 Uiso 0.50 1 calc PR H 2 H28D H 0.3220 0.5675 0.5570 0.133 Uiso 0.50 1 calc PR H 2 N28B N 0.1391(14) 0.5409(12) 0.5753(11) 0.088(6) Uiso 0.50 1 d PD H 2 H28G H 0.1328 0.6017 0.5781 0.105 Uiso 0.50 1 calc PR H 2 H28H H 0.1247 0.5170 0.6298 0.105 Uiso 0.50 1 calc PR H 2 O1W O 0.9375(14) 0.3627(11) 0.2504(10) 0.179(7) Uiso 0.60 1 d P . . H1WB H 0.9633 0.3809 0.2983 0.269 Uiso 0.60 1 d PR . . H1WA H 0.9965 0.3689 0.2108 0.269 Uiso 0.60 1 d PR . . O2W O 0.624(2) -0.0151(16) 0.0136(14) 0.160(9) Uiso 0.40 1 d P . . H2WB H 0.6830 -0.0149 -0.0262 0.240 Uiso 0.40 1 d PR . . H2WA H 0.5824 -0.0639 0.0125 0.240 Uiso 0.40 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.03056(17) 0.02369(17) 0.02485(17) -0.00341(13) 0.00022(12) 0.00129(13) W2 0.0395(2) 0.0354(2) 0.0416(2) 0.00751(16) 0.00450(16) -0.00424(16) Cu1 0.0426(6) 0.0402(6) 0.0479(6) -0.0076(5) -0.0072(5) 0.0072(5) Cu2 0.0320(7) 0.0332(8) 0.0436(8) 0.0009(6) 0.0044(6) 0.0019(6) Cu3 0.0480(9) 0.0434(9) 0.0361(8) -0.0089(7) 0.0037(7) 0.0002(7) Cu4 0.0752(11) 0.0466(10) 0.0367(9) 0.0024(7) 0.0094(8) -0.0091(8) Cu5 0.203(2) 0.0719(14) 0.0574(13) 0.0257(11) -0.0361(14) -0.0379(15) C1 0.046(5) 0.040(5) 0.032(5) 0.007(4) 0.002(4) -0.017(4) N1 0.040(4) 0.062(5) 0.051(5) 0.000(4) -0.005(4) -0.010(4) C2 0.055(5) 0.039(5) 0.030(5) 0.000(4) 0.000(4) 0.009(4) N2 0.123(7) 0.065(6) 0.055(5) -0.007(5) -0.006(5) 0.054(6) C3 0.052(5) 0.028(5) 0.040(5) 0.002(4) -0.002(4) 0.009(4) N3 0.089(6) 0.037(5) 0.049(5) -0.016(4) -0.014(4) 0.010(4) C4 0.064(6) 0.029(5) 0.033(5) -0.005(4) -0.001(4) -0.001(4) N4 0.121(7) 0.049(5) 0.038(5) -0.001(4) 0.013(5) -0.010(5) C5 0.045(5) 0.029(5) 0.030(4) 0.003(4) -0.005(4) -0.003(4) N5 0.059(5) 0.045(5) 0.051(5) 0.009(4) 0.001(4) -0.001(4) C6 0.048(5) 0.032(5) 0.042(5) -0.008(4) -0.010(4) 0.021(4) N6 0.055(5) 0.046(5) 0.071(5) -0.006(4) 0.003(4) -0.017(4) C7 0.041(5) 0.023(4) 0.037(5) 0.001(4) 0.012(4) 0.003(4) N7 0.045(4) 0.061(5) 0.070(5) -0.012(4) -0.011(4) 0.014(4) C8 0.049(5) 0.033(5) 0.026(4) -0.003(4) 0.001(4) 0.003(4) N8 0.075(5) 0.042(5) 0.039(4) -0.013(4) 0.003(4) 0.010(4) C10 0.075(7) 0.049(6) 0.061(6) -0.005(5) 0.005(5) -0.004(6) N10 0.101(7) 0.044(6) 0.150(9) -0.003(6) 0.013(6) -0.013(6) C11 0.066(7) 0.066(7) 0.056(6) -0.001(5) -0.004(5) 0.011(5) C13 0.047(6) 0.047(6) 0.125(9) 0.013(6) -0.031(6) -0.013(5) C15 0.066(7) 0.051(6) 0.083(7) 0.018(6) 0.025(6) 0.013(5) C16 0.056(6) 0.057(7) 0.058(6) 0.008(5) 0.000(5) -0.004(5) N16 0.128(8) 0.086(7) 0.054(6) -0.005(5) -0.006(6) -0.016(6) N17 0.056(5) 0.069(6) 0.062(5) 0.002(4) 0.000(4) 0.038(5) C17 0.057(7) 0.144(12) 0.045(6) -0.022(7) -0.008(5) -0.020(7) C18 0.059(6) 0.083(8) 0.075(8) -0.043(6) 0.004(6) -0.017(6) N18 0.053(5) 0.049(5) 0.087(6) -0.020(4) 0.008(4) -0.013(4) N19 0.055(5) 0.079(6) 0.052(5) 0.007(4) -0.002(4) -0.008(4) N20 0.075(6) 0.061(6) 0.101(7) -0.033(5) -0.010(5) 0.010(5) N21 0.033(4) 0.047(5) 0.056(4) 0.013(4) 0.004(3) 0.007(3) C21 0.040(5) 0.037(5) 0.053(5) -0.005(4) -0.002(4) 0.009(4) C22 0.055(5) 0.051(6) 0.036(5) 0.003(4) -0.001(4) -0.001(5) N22 0.038(4) 0.035(4) 0.053(4) 0.000(3) 0.002(3) -0.005(3) N23 0.082(5) 0.038(4) 0.039(4) -0.007(3) 0.014(4) -0.001(4) C23 0.043(6) 0.070(7) 0.096(8) 0.018(7) 0.021(6) 0.008(5) C24 0.058(7) 0.059(7) 0.101(9) -0.018(6) -0.017(6) -0.001(5) N24 0.062(5) 0.042(4) 0.048(4) -0.017(4) -0.006(4) 0.008(4) N25 0.075(5) 0.061(5) 0.051(5) 0.003(4) 0.006(4) -0.003(4) N26 0.070(5) 0.058(5) 0.048(5) 0.013(4) 0.014(4) -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 W1 C6 2.143(9) . ? W1 C4 2.146(8) . ? W1 C8 2.153(8) . ? W1 C2 2.155(8) . ? W1 C5 2.159(7) . ? W1 C7 2.166(7) . ? W1 C1 2.171(8) . ? W1 C3 2.203(8) . ? W2 C12B 2.12(2) . ? W2 C14A 2.113(19) . ? W2 C15 2.142(8) . ? W2 C9B 2.13(3) . ? W2 C11 2.144(9) . ? W2 C16 2.141(10) . ? W2 C13 2.161(9) . ? W2 C10 2.172(10) . ? W2 C9A 2.187(16) . ? W2 C14B 2.193(16) . ? W2 C12A 2.21(2) . ? Cu1 N18 1.989(7) . ? Cu1 N20 1.991(7) . ? Cu1 N19 1.997(6) . ? Cu1 N17 2.029(6) . ? Cu1 N1 2.329(6) . ? Cu2 N22 2.021(5) . ? Cu2 N22 2.021(5) 2_576 ? Cu2 N21 2.021(5) 2_576 ? Cu2 N21 2.021(5) . ? Cu3 N24 2.005(6) 2_565 ? Cu3 N24 2.005(6) . ? Cu3 N23 2.004(6) . ? Cu3 N23 2.004(6) 2_565 ? Cu4 N26 2.007(6) . ? Cu4 N26 2.007(6) 2 ? Cu4 N25 2.031(7) . ? Cu4 N25 2.031(7) 2 ? Cu5 N28A 1.987(8) . ? Cu5 N28A 1.987(8) 2_566 ? Cu5 N27B 1.994(9) 2_566 ? Cu5 N27B 1.994(9) . ? Cu5 N27A 2.007(9) . ? Cu5 N27A 2.007(9) 2_566 ? Cu5 N28B 2.018(9) 2_566 ? Cu5 N28B 2.018(9) . ? C1 N1 1.128(8) . ? C2 N2 1.128(8) . ? C3 N3 1.107(8) . ? C4 N4 1.148(8) . ? C5 N5 1.123(8) . ? C6 N6 1.158(9) . ? C7 N7 1.137(8) . ? C8 N8 1.138(8) . ? C10 N10 1.127(10) . ? C11 N11A 1.178(18) . ? C11 N11B 1.218(18) . ? C13 N13A 1.154(13) . ? C13 N13B 1.225(18) . ? C15 N15B 1.196(17) . ? C15 N15A 1.204(16) . ? C16 N16 1.157(10) . ? N17 C17 1.476(11) . ? C17 C18 1.464(11) . ? C18 N18 1.474(10) . ? N19 C19B 1.30(2) . ? N19 C19A 1.693(19) . ? N20 C20A 1.403(17) . ? N20 C20B 1.58(2) . ? N21 C21 1.472(9) . ? C21 C22 1.488(9) 2_576 ? C22 N22 1.467(8) . ? C22 C21 1.488(9) 2_576 ? N23 C23 1.460(9) . ? C23 C24 1.450(11) 2_565 ? C24 C23 1.450(11) 2_565 ? C24 N24 1.466(10) . ? N25 C25B 1.36(2) . ? N25 C25A 1.59(2) . ? N26 C26B 1.33(3) . ? N26 C26A 1.52(2) . ? C9A N9A 1.139(17) . ? C12A N12A 1.13(2) . ? C14A N14A 1.16(2) . ? C9B N9B 1.12(3) . ? C12B N12B 1.16(2) . ? C14B N14B 1.108(17) . ? C19A C20A 1.45(2) . ? C19B C20B 1.48(3) . ? C25A C26A 1.41(3) . ? C25B C26B 1.60(3) . ? N27A C27A 1.37(4) . ? C27A C28A 1.479(10) . ? N27B C27B 1.41(4) . ? C27B C28B 1.480(10) . ? C28A N28A 1.52(2) . ? C28B N28B 1.42(3) . ? 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 C6 W1 C4 73.1(3) . . ? C6 W1 C8 75.1(3) . . ? C4 W1 C8 141.8(3) . . ? C6 W1 C2 76.2(3) . . ? C4 W1 C2 79.0(3) . . ? C8 W1 C2 73.4(3) . . ? C6 W1 C5 141.0(3) . . ? C4 W1 C5 144.6(3) . . ? C8 W1 C5 72.0(3) . . ? C2 W1 C5 112.7(3) . . ? C6 W1 C7 73.6(3) . . ? C4 W1 C7 111.0(3) . . ? C8 W1 C7 78.9(3) . . ? C2 W1 C7 143.2(3) . . ? C5 W1 C7 80.1(3) . . ? C6 W1 C1 140.2(3) . . ? C4 W1 C1 78.0(3) . . ? C8 W1 C1 116.3(3) . . ? C2 W1 C1 71.9(3) . . ? C5 W1 C1 74.8(3) . . ? C7 W1 C1 143.8(3) . . ? C6 W1 C3 120.7(3) . . ? C4 W1 C3 75.0(3) . . ? C8 W1 C3 141.0(3) . . ? C2 W1 C3 142.0(3) . . ? C5 W1 C3 76.7(3) . . ? C7 W1 C3 73.3(3) . . ? C1 W1 C3 75.9(3) . . ? C12B W2 C14A 76.8(7) . . ? C12B W2 C15 129.5(7) . . ? C14A W2 C15 69.9(5) . . ? C12B W2 C9B 77.2(9) . . ? C14A W2 C9B 145.3(8) . . ? C15 W2 C9B 144.7(7) . . ? C12B W2 C11 74.3(6) . . ? C14A W2 C11 100.0(6) . . ? C15 W2 C11 75.3(3) . . ? C9B W2 C11 94.6(7) . . ? C12B W2 C16 138.8(6) . . ? C14A W2 C16 94.8(6) . . ? C15 W2 C16 81.9(4) . . ? C9B W2 C16 89.9(7) . . ? C11 W2 C16 146.4(3) . . ? C12B W2 C13 63.5(6) . . ? C14A W2 C13 77.7(5) . . ? C15 W2 C13 138.3(4) . . ? C9B W2 C13 70.4(7) . . ? C11 W2 C13 137.3(4) . . ? C16 W2 C13 75.3(4) . . ? C12B W2 C10 132.8(6) . . ? C14A W2 C10 144.2(5) . . ? C15 W2 C10 74.7(3) . . ? C9B W2 C10 70.0(7) . . ? C11 W2 C10 75.5(4) . . ? C16 W2 C10 74.9(3) . . ? C13 W2 C10 129.7(3) . . ? C12B W2 C9A 63.6(7) . . ? C14A W2 C9A 139.1(6) . . ? C15 W2 C9A 144.9(4) . . ? C9B W2 C9A 18.3(7) . . ? C11 W2 C9A 79.3(5) . . ? C16 W2 C9A 108.2(5) . . ? C13 W2 C9A 76.3(5) . . ? C10 W2 C9A 75.8(5) . . ? C12B W2 C14B 87.3(7) . . ? C14A W2 C14B 18.1(5) . . ? C15 W2 C14B 72.3(4) . . ? C9B W2 C14B 139.2(7) . . ? C11 W2 C14B 117.4(5) . . ? C16 W2 C14B 77.3(5) . . ? C13 W2 C14B 68.9(4) . . ? C10 W2 C14B 139.1(4) . . ? C9A W2 C14B 142.2(5) . . ? C12B W2 C12A 25.2(6) . . ? C14A W2 C12A 58.7(7) . . ? C15 W2 C12A 104.4(6) . . ? C9B W2 C12A 101.2(9) . . ? C11 W2 C12A 64.6(5) . . ? C16 W2 C12A 146.6(5) . . ? C13 W2 C12A 79.0(5) . . ? C10 W2 C12A 138.5(5) . . ? C9A W2 C12A 85.6(6) . . ? C14B W2 C12A 73.8(6) . . ? N18 Cu1 N20 174.5(3) . . ? N18 Cu1 N19 95.1(3) . . ? N20 Cu1 N19 85.1(3) . . ? N18 Cu1 N17 83.1(3) . . ? N20 Cu1 N17 95.7(3) . . ? N19 Cu1 N17 169.3(3) . . ? N18 Cu1 N1 90.1(3) . . ? N20 Cu1 N1 95.3(3) . . ? N19 Cu1 N1 94.2(2) . . ? N17 Cu1 N1 96.3(3) . . ? N22 Cu2 N22 180.000(1) . 2_576 ? N22 Cu2 N21 83.8(2) . 2_576 ? N22 Cu2 N21 96.2(2) 2_576 2_576 ? N22 Cu2 N21 96.2(2) . . ? N22 Cu2 N21 83.8(2) 2_576 . ? N21 Cu2 N21 180.000(2) 2_576 . ? N24 Cu3 N24 180.0(4) 2_565 . ? N24 Cu3 N23 83.2(3) 2_565 . ? N24 Cu3 N23 96.8(3) . . ? N24 Cu3 N23 96.8(3) 2_565 2_565 ? N24 Cu3 N23 83.2(3) . 2_565 ? N23 Cu3 N23 180.0(4) . 2_565 ? N26 Cu4 N26 180.0(4) . 2 ? N26 Cu4 N25 84.6(3) . . ? N26 Cu4 N25 95.4(3) 2 . ? N26 Cu4 N25 95.4(3) . 2 ? N26 Cu4 N25 84.6(3) 2 2 ? N25 Cu4 N25 180.0(5) . 2 ? N28A Cu5 N28A 180.000(2) . 2_566 ? N28A Cu5 N27B 73.2(8) . 2_566 ? N28A Cu5 N27B 106.8(9) 2_566 2_566 ? N28A Cu5 N27B 106.8(9) . . ? N28A Cu5 N27B 73.2(8) 2_566 . ? N27B Cu5 N27B 180.000(4) 2_566 . ? N28A Cu5 N27A 89.7(9) . . ? N28A Cu5 N27A 90.3(9) 2_566 . ? N27B Cu5 N27A 162.8(12) 2_566 . ? N27B Cu5 N27A 17.2(12) . . ? N28A Cu5 N27A 90.3(9) . 2_566 ? N28A Cu5 N27A 89.7(9) 2_566 2_566 ? N27B Cu5 N27A 17.2(12) 2_566 2_566 ? N27B Cu5 N27A 162.8(12) . 2_566 ? N27A Cu5 N27A 180.000(2) . 2_566 ? N28A Cu5 N28B 153.5(5) . 2_566 ? N28A Cu5 N28B 26.5(5) 2_566 2_566 ? N27B Cu5 N28B 80.3(9) 2_566 2_566 ? N27B Cu5 N28B 99.7(9) . 2_566 ? N27A Cu5 N28B 116.8(9) . 2_566 ? N27A Cu5 N28B 63.2(9) 2_566 2_566 ? N28A Cu5 N28B 26.5(5) . . ? N28A Cu5 N28B 153.5(5) 2_566 . ? N27B Cu5 N28B 99.7(9) 2_566 . ? N27B Cu5 N28B 80.3(9) . . ? N27A Cu5 N28B 63.2(9) . . ? N27A Cu5 N28B 116.8(9) 2_566 . ? N28B Cu5 N28B 180.000(2) 2_566 . ? N1 C1 W1 178.1(7) . . ? C1 N1 Cu1 139.2(6) . . ? N2 C2 W1 176.9(7) . . ? N3 C3 W1 178.3(7) . . ? N4 C4 W1 176.1(8) . . ? N5 C5 W1 179.3(7) . . ? N6 C6 W1 177.8(7) . . ? N7 C7 W1 178.0(8) . . ? N8 C8 W1 177.1(7) . . ? N10 C10 W2 179.0(10) . . ? N11A C11 N11B 31.4(11) . . ? N11A C11 W2 164.2(13) . . ? N11B C11 W2 164.3(13) . . ? N13A C13 N13B 33.9(10) . . ? N13A C13 W2 168.3(12) . . ? N13B C13 W2 157.5(13) . . ? N15B C15 N15A 33.6(10) . . ? N15B C15 W2 162.3(13) . . ? N15A C15 W2 164.0(13) . . ? N16 C16 W2 178.4(9) . . ? C17 N17 Cu1 109.2(6) . . ? C18 C17 N17 106.4(8) . . ? C17 C18 N18 108.4(7) . . ? C18 N18 Cu1 109.0(6) . . ? C19B N19 C19A 25.8(11) . . ? C19B N19 Cu1 116.7(10) . . ? C19A N19 Cu1 103.5(7) . . ? C20A N20 C20B 28.6(9) . . ? C20A N20 Cu1 111.7(9) . . ? C20B N20 Cu1 103.5(10) . . ? C21 N21 Cu2 108.1(4) . . ? N21 C21 C22 107.6(6) . 2_576 ? N22 C22 C21 107.8(6) . 2_576 ? C22 N22 Cu2 108.9(4) . . ? C23 N23 Cu3 109.2(5) . . ? C24 C23 N23 108.6(7) 2_565 . ? C23 C24 N24 107.4(8) 2_565 . ? C24 N24 Cu3 108.3(5) . . ? C25B N25 C25A 23.8(12) . . ? C25B N25 Cu4 111.4(11) . . ? C25A N25 Cu4 106.4(9) . . ? C26B N26 C26A 27.1(13) . . ? C26B N26 Cu4 108.9(13) . . ? C26A N26 Cu4 106.8(8) . . ? N9A C9A W2 173.2(16) . . ? N12A C12A W2 177.1(19) . . ? N14A C14A W2 175.0(17) . . ? N9B C9B W2 176(3) . . ? N12B C12B W2 175(2) . . ? N14B C14B W2 175.4(15) . . ? C20A C19A N19 104.6(12) . . ? N20 C20A C19A 106.3(13) . . ? N19 C19B C20B 108.3(16) . . ? C19B C20B N20 113.9(18) . . ? C26A C25A N25 104.6(15) . . ? C25A C26A N26 107.9(15) . . ? N25 C25B C26B 107.9(18) . . ? N26 C26B C25B 114.8(19) . . ? C27A N27A Cu5 106(2) . . ? N27A C27A C28A 116(3) . . ? C27B N27B Cu5 115.1(16) . . ? N27B C27B C28B 114(2) . . ? C27A C28A N28A 112(3) . . ? C28A N28A Cu5 103.0(9) . . ? N28B C28B C27B 110(2) . . ? C28B N28B Cu5 116.1(16) . . ? 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 N(17) H(17C) N(16) 0.90(3) 2.38(2) 3.116(10) 138(6) 2_666 N(17) H(17D) N(6) 0.90(1) 2.47(8) 3.325(10) 156(7) 1_655 N(18) H(18C) N(13A) 0.90(1) 2.48(1) 3.213(14) 138(7) 1_565 N(18) H(18C) N(13B) 0.90(1) 2.53(4) 3.12(2) 123(1) 1_565 N(18) H(18D) N(14A) 0.90(2) 2.29(5) 3.145(18) 157(3) 1_565 N(18) H(18D) N(14B) 0.90(2) 2.49(1) 3.216(13) 137(8) 1_565 N(19) H(19E) N(12A) 0.90(1) 2.59(4) 3.132(19) 119(1) 1_565 N(19) H(19F) N(7) 0.90(1) 2.60(3) 3.143(9) 119(2) 1_655 N(19) H(19G) N(5) 0.90(2) 2.55(5) 3.407(9) 158(1) 1_555 N(19) H(19H) N(12A) 0.90(1) 2.51(1) 3.132(19) 126(7) 1_565 N(19) H(19H) N(12B) 0.90(1) 2.60(1) 3.44(2) 155(5) 1_565 N(20) H(20E) N(6) 0.90(1) 2.31(2) 3.181(10) 162(2) 1_655 N(20) H(20G) N(6) 0.90(1) 2.42(1) 3.181(10) 142(3) 1_655 N(20) H(20H) N(10) 0.90(1) 2.54(6) 3.214(12) 131(5) 1_555 N(21) H(21A) N(14A) 0.90(1) 2.50(6) 3.331(19) 152(6) 1_565 N(21) H(21A) N(14B) 0.90(1) 2.32(4) 3.073(13) 140(5) 1_565 N(21) H(21B) N(13A) 0.90(1) 2.57(3) 3.289(15) 137(1) 2_666 N(21) H(21B) N(13B) 0.90(1) 2.18(3) 2.89(2) 134(5) 2_666 N(22) H(22B) N(14A) 0.90(4) 2.31(7) 3.159(18) 155(6) 1_565 N(22) H(22B) N(14B) 0.90(5) 2.40(5) 3.116(13) 136(1) 1_565 N(23) H(23A) O(1W) 0.90(1) 2.57(1) 2.967(17) 107(3) 1_455 N(23) H(23A) N(9A) 0.90(1) 2.44(4) 3.218(15) 144(2) 1_455 N(23) H(23A) N(9B) 0.90(1) 2.32(1) 3.07(2) 140(1) 1_455 N(23) H(23B) O(1W) 0.90(1) 2.53(1) 2.967(17) 110(3) 1_455 N(23) H(23B) N(6) 0.90(1) 2.62(6) 3.364(10) 139(5) 1_555 N(24) H(24A) N(2) 0.90(1) 2.21(1) 3.072(10) 160(3) 1_555 N(24) H(24B) N(11A) 0.90(1) 2.40(3) 3.215(19) 150(1) 1_555 N(24) H(24B) N(11B) 0.90(1) 2.35(1) 3.053(19) 134(7) 1_555 N(26) H(26F) N(7) 0.90(1) 2.38(7) 3.269(10) 166(3) 1_545 N(27A) H(27E) N(15B) 0.90(1) 2.37(4) 3.21(3) 153(7) 1_555 N(27A) H(27F) N(2) 0.90(1) 2.42(9) 3.21(3) 144(5) 1_555 N(27B) H(27G) N(15A) 0.90(1) 2.50(1) 3.23(3) 137(5) 1_555 N(27B) H(27G) N(15B) 0.90(1) 1.96(1) 2.75(3) 145(1) 1_555 N(27B) H(27G) N(4) 0.90(1) 2.62(6) 3.08(3) 112(1) 2_566 N(27B) H(27H) N(2) 0.90(1) 2.00(1) 2.89(3) 168(1) 1_555 N(28A) H(28H) N(6) 0.90(1) 2.59(6) 3.443(14) 157(3) 2_566 _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 2.013 _refine_diff_density_min -1.576 _refine_diff_density_rms 0.156