Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address 'You Song.' ; Coordination Chemistry Institute and the State Key Laboratory of Coordination chemistry Nanjing University Nanjing 210093 P. R. China ; 'Kazuhito Hashimoto' ; Coordination Chemistry Institute and the State Key Laboratory of Coordination chemistry Nanjing University Nanjing 210093 P. R. China ; 'Xi-Li Li.' ; Coordination Chemistry Institute and the State Key Laboratory of Coordination chemistry Nanjing University Nanjing 210093 P. R. China ; 'Bao-Lin Liu.' ; Coordination Chemistry Institute and the State Key Laboratory of Coordination chemistry Nanjing University Nanjing 210093 P. R. China ; 'Shinichi Ohkoshi' ; Department of Chemistry School of Science The University of Tokyo 7-3-1 Hongo Bunkyo-ku Tokyo 113-0033 Japan ; 'Hiroko Tokoro' ; Department of Chemistry School of Science The University of Tokyo 7-3-1 Hongo Bunkyo-ku Tokyo 113-0033 Japan ; ; Zhaoxi Wang ; ; Department of Applied Chemistry School of Engineering The University of Tokyo 7-3-1 Hongo Bunkyo-ku Tokyo 113-8656 Japan ; 'Xiao-Zeng You.' ; Coordination Chemistry Institute and the State Key Laboratory of Coordination chemistry Nanjing University Nanjing 210093 P. R. China ; 'Peng Zhang.' '' _publ_contact_author_name 'You Song' _publ_contact_author_email YOUSONG@NJU.EDU.CN _publ_section_title ; 3D coordination metal-organic frameworks of octacyanometalate bridging between Cu4 magnetic units ; _publ_contact_author_address ; Coordination Chemistry Institute and the State Key Laboratory of Coordination chemistry Nanjing University Nanjing 210093 P. R. China ; _publ_contact_author_fax +862583314502 _publ_contact_author_phone +862583593739 # Attachment 'MoCu4.cif' data_MoCu4 _database_code_depnum_ccdc_archive 'CCDC 666244' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H24 Cu4 Mo N12 O4, 2(H2 O)' _chemical_formula_sum 'C16 H28 Cu4 Mo N12 O6' _chemical_formula_weight 834.60 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7166(13) _cell_length_b 10.1526(11) _cell_length_c 23.395(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.738(2) _cell_angle_gamma 90.00 _cell_volume 2782.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3878 _cell_measurement_theta_min 0.995 _cell_measurement_theta_max 27 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.992 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 3.501 _exptl_absorpt_correction_type multi_scan _exptl_absorpt_correction_T_min 0.321 _exptl_absorpt_correction_T_max 0.447 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _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 15657 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.1283 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6026 _reflns_number_gt 3878 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0538P)^2^] 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 6026 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1369 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.1530 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1772(8) 0.3469(10) 0.2195(4) 0.025(2) Uani 1 1 d . . . C2 C 0.1486(8) 0.5674(10) 0.1812(4) 0.027(2) Uani 1 1 d . . . C3 C 0.0655(7) 0.4177(9) 0.1031(4) 0.022(2) Uani 1 1 d . . . C4 C 0.1775(7) 0.2084(10) 0.1217(4) 0.024(2) Uani 1 1 d . . . C5 C 0.3803(8) 0.5211(10) 0.1657(4) 0.026(2) Uani 1 1 d . . . C6 C 0.2382(8) 0.5826(10) 0.0811(4) 0.028(2) Uani 1 1 d . . . C7 C 0.3067(7) 0.3481(9) 0.0580(4) 0.022(2) Uani 1 1 d . . . C8 C 0.3677(8) 0.2794(10) 0.1696(4) 0.026(2) Uani 1 1 d . . . C9 C 0.0510(8) 0.3702(10) 0.4319(4) 0.031(2) Uani 1 1 d . . . H9A H -0.0149 0.4085 0.4503 0.038 Uiso 1 1 calc R . . H9B H 0.1177 0.4223 0.4419 0.038 Uiso 1 1 calc R . . C10 C 0.0672(8) 0.2306(10) 0.4512(4) 0.029(2) Uani 1 1 d . . . H10A H 0.0910 0.2284 0.4910 0.035 Uiso 1 1 calc R . . H10B H -0.0038 0.1821 0.4472 0.035 Uiso 1 1 calc R . . C11 C 0.3914(9) 0.4718(10) 0.3831(4) 0.037(3) Uani 1 1 d . . . H11A H 0.3141 0.5053 0.3799 0.045 Uiso 1 1 calc R . . H11B H 0.4442 0.5445 0.3784 0.045 Uiso 1 1 calc R . . N10 N 0.4102(7) 0.4070(8) 0.4401(3) 0.034(2) Uani 1 1 d . . . H10C H 0.3721 0.4506 0.4673 0.040 Uiso 1 1 calc R . . H10D H 0.4850 0.4071 0.4494 0.040 Uiso 1 1 calc R . . C13 C 0.2558(8) -0.1128(10) 0.2532(5) 0.036(3) Uani 1 1 d . . . H13A H 0.2515 -0.1835 0.2810 0.044 Uiso 1 1 calc R . . H13B H 0.2423 -0.1495 0.2154 0.044 Uiso 1 1 calc R . . C14 C 0.1686(8) -0.0091(10) 0.2658(4) 0.031(2) Uani 1 1 d . . . H14A H 0.1599 0.0495 0.2333 0.037 Uiso 1 1 calc R . . H14B H 0.0954 -0.0499 0.2731 0.037 Uiso 1 1 calc R . . C15 C 0.3700(8) -0.1957(9) 0.4195(4) 0.026(2) Uani 1 1 d . . . H15A H 0.3923 -0.2100 0.3802 0.031 Uiso 1 1 calc R . . H15B H 0.4031 -0.2650 0.4429 0.031 Uiso 1 1 calc R . . C16 C 0.4111(7) -0.0631(9) 0.4399(4) 0.023(2) Uani 1 1 d . . . H16A H 0.4044 -0.0570 0.4811 0.028 Uiso 1 1 calc R . . H16B H 0.4907 -0.0511 0.4302 0.028 Uiso 1 1 calc R . . Cu1 Cu 0.35260(9) 0.22153(11) 0.43372(4) 0.0208(3) Uani 1 1 d . . . Cu2 Cu 0.18572(9) -0.01511(11) 0.41265(5) 0.0204(3) Uani 1 1 d . . . Cu3 Cu 0.37166(9) 0.08821(12) 0.31415(4) 0.0220(3) Uani 1 1 d . . . Cu4 Cu 0.13382(9) 0.22996(11) 0.33694(4) 0.0235(3) Uani 1 1 d . . . Mo1 Mo 0.23410(6) 0.40942(8) 0.13731(3) 0.01602(19) Uani 1 1 d . . . N1 N 0.1458(7) 0.3082(8) 0.2619(3) 0.032(2) Uani 1 1 d . . . N2 N 0.0997(8) 0.6486(9) 0.2036(4) 0.042(2) Uani 1 1 d . . . N3 N -0.0271(6) 0.4304(8) 0.0892(3) 0.030(2) Uani 1 1 d . . . N4 N 0.1521(8) 0.1030(9) 0.1120(4) 0.045(2) Uani 1 1 d . . . N5 N 0.4619(7) 0.5787(8) 0.1775(3) 0.0295(19) Uani 1 1 d . . . N6 N 0.2428(7) 0.6741(9) 0.0544(4) 0.038(2) Uani 1 1 d . . . N7 N 0.3383(6) 0.3110(8) 0.0146(3) 0.0246(18) Uani 1 1 d . . . N8 N 0.4353(7) 0.2105(10) 0.1884(4) 0.046(3) Uani 1 1 d . . . N9 N 0.0337(6) 0.3686(8) 0.3694(3) 0.029(2) Uani 1 1 d . . . H9C H 0.0515 0.4477 0.3546 0.035 Uiso 1 1 calc R . . H9D H -0.0399 0.3512 0.3608 0.035 Uiso 1 1 calc R . . C12 C 0.4117(9) 0.3679(9) 0.3390(4) 0.032(2) Uani 1 1 d . . . H12A H 0.3884 0.4002 0.3016 0.038 Uiso 1 1 calc R . . H12B H 0.4924 0.3467 0.3378 0.038 Uiso 1 1 calc R . . N11 N 0.3691(6) -0.0497(8) 0.2561(3) 0.031(2) Uani 1 1 d . . . H11C H 0.3857 -0.0148 0.2219 0.037 Uiso 1 1 calc R . . H11D H 0.4225 -0.1106 0.2646 0.037 Uiso 1 1 calc R . . N12 N 0.2434(6) -0.1968(7) 0.4240(3) 0.0277(19) Uani 1 1 d . . . H12C H 0.2231 -0.2267 0.4586 0.033 Uiso 1 1 calc R . . H12D H 0.2131 -0.2506 0.3972 0.033 Uiso 1 1 calc R . . O1 O 0.1530(5) 0.1729(6) 0.4162(2) 0.0193(14) Uani 1 1 d . . . O2 O 0.3491(5) 0.2554(6) 0.3525(2) 0.0210(14) Uani 1 1 d . . . O3 O 0.2054(5) 0.0633(6) 0.3145(2) 0.0214(14) Uani 1 1 d . . . O4 O 0.3441(4) 0.0336(6) 0.4134(2) 0.0202(14) Uani 1 1 d . . . O5 O 0.0979(6) 0.6462(8) 0.3319(3) 0.048(2) Uani 1 1 d . . . H5B H 0.0990 0.6499 0.2956 0.057 Uiso 1 1 d R . . H5A H 0.0496 0.7015 0.3442 0.057 Uiso 1 1 d R . . O6 O 0.3226(7) 0.9413(8) 0.0424(3) 0.064(3) Uani 1 1 d . . . H6A H 0.2769 0.9889 0.0613 0.077 Uiso 1 1 d R . . H6B H 0.3012 0.8616 0.0451 0.077 Uiso 1 1 d 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 C1 0.024(5) 0.028(6) 0.023(5) -0.007(5) -0.004(4) -0.005(4) C2 0.022(5) 0.035(7) 0.025(5) -0.003(5) 0.006(4) -0.005(4) C3 0.015(5) 0.026(6) 0.024(5) 0.003(4) 0.007(4) -0.001(4) C4 0.021(5) 0.028(6) 0.023(5) -0.001(5) 0.008(4) -0.007(4) C5 0.026(6) 0.028(6) 0.024(5) 0.001(4) 0.002(4) 0.004(4) C6 0.029(6) 0.025(6) 0.030(5) -0.001(5) 0.002(4) 0.000(4) C7 0.008(4) 0.029(6) 0.027(5) 0.005(4) -0.009(4) -0.002(4) C8 0.029(6) 0.028(6) 0.021(5) 0.010(4) 0.009(4) -0.005(4) C9 0.036(6) 0.037(7) 0.022(5) -0.012(5) 0.006(4) 0.019(5) C10 0.025(5) 0.033(6) 0.029(5) 0.006(5) 0.006(4) 0.003(4) C11 0.055(7) 0.023(6) 0.034(6) -0.005(5) 0.014(5) -0.013(5) N10 0.040(5) 0.030(5) 0.030(5) -0.004(4) -0.001(4) -0.005(4) C13 0.032(6) 0.034(7) 0.043(6) -0.015(5) 0.003(5) -0.010(5) C14 0.022(5) 0.040(7) 0.030(5) -0.008(5) -0.004(4) -0.003(4) C15 0.032(6) 0.019(6) 0.028(5) 0.011(4) 0.007(4) 0.004(4) C16 0.014(5) 0.026(6) 0.029(5) 0.007(4) -0.002(4) 0.003(4) Cu1 0.0264(6) 0.0203(6) 0.0159(6) -0.0004(5) 0.0037(5) -0.0027(5) Cu2 0.0151(6) 0.0219(7) 0.0243(6) 0.0018(5) -0.0014(5) -0.0009(5) Cu3 0.0170(6) 0.0257(7) 0.0233(6) -0.0047(5) 0.0012(5) 0.0019(5) Cu4 0.0266(6) 0.0265(7) 0.0174(6) 0.0032(5) 0.0066(5) 0.0083(5) Mo1 0.0135(4) 0.0201(4) 0.0145(4) 0.0011(3) 0.0019(3) -0.0005(3) N1 0.039(5) 0.028(5) 0.028(5) 0.012(4) 0.007(4) 0.009(4) N2 0.050(6) 0.036(6) 0.042(6) -0.003(5) 0.010(5) 0.003(5) N3 0.015(4) 0.036(6) 0.040(5) -0.002(4) -0.004(4) -0.003(4) N4 0.057(7) 0.037(6) 0.042(6) 0.003(5) 0.004(5) -0.016(5) N5 0.026(5) 0.034(5) 0.028(4) -0.001(4) -0.005(4) -0.001(4) N6 0.044(6) 0.032(6) 0.038(5) 0.010(4) 0.012(4) 0.011(4) N7 0.030(5) 0.031(5) 0.013(4) -0.008(4) 0.003(3) 0.003(4) N8 0.030(5) 0.055(7) 0.053(6) 0.014(5) -0.006(5) 0.017(5) N9 0.033(5) 0.031(5) 0.025(4) 0.002(4) 0.000(4) 0.014(4) C12 0.048(7) 0.023(6) 0.024(5) 0.004(4) 0.004(5) -0.004(5) N11 0.025(5) 0.041(6) 0.027(4) -0.015(4) 0.008(4) 0.001(4) N12 0.034(5) 0.021(5) 0.028(4) 0.005(4) -0.005(4) -0.007(4) O1 0.019(3) 0.023(4) 0.017(3) 0.004(3) 0.009(3) 0.004(3) O2 0.027(4) 0.021(4) 0.015(3) 0.001(3) 0.005(3) -0.005(3) O3 0.016(3) 0.028(4) 0.020(3) -0.005(3) 0.001(3) 0.004(3) O4 0.009(3) 0.025(4) 0.026(3) 0.002(3) -0.002(3) 0.002(2) O5 0.046(5) 0.054(6) 0.044(5) -0.002(4) 0.007(4) 0.004(4) O6 0.078(7) 0.048(6) 0.069(6) -0.005(5) 0.038(5) 0.000(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 C1 N1 1.133(11) . ? C1 Mo1 2.140(10) . ? C2 N2 1.136(12) . ? C2 Mo1 2.159(10) . ? C3 N3 1.135(10) . ? C3 Mo1 2.124(9) . ? C4 N4 1.133(12) . ? C4 Mo1 2.175(10) . ? C5 N5 1.152(11) . ? C5 Mo1 2.152(10) . ? C6 N6 1.122(12) . ? C6 Mo1 2.196(10) . ? C7 N7 1.148(11) . ? C7 Mo1 2.144(9) . ? C8 N8 1.140(11) . ? C8 Mo1 2.175(10) . ? C9 N9 1.473(11) . ? C9 C10 1.499(13) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O1 1.431(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.497(13) . ? C11 N10 1.500(12) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N10 Cu1 2.005(8) . ? N10 H10C 0.9000 . ? N10 H10D 0.9000 . ? C13 N11 1.474(11) . ? C13 C14 1.500(13) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O3 1.418(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N12 1.488(11) . ? C15 C16 1.505(13) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O4 1.398(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? Cu1 O2 1.930(6) . ? Cu1 N7 1.931(7) 4_566 ? Cu1 O4 1.969(6) . ? Cu1 O1 2.420(6) . ? Cu2 O4 1.921(5) . ? Cu2 N3 1.939(8) 2_545 ? Cu2 O1 1.949(6) . ? Cu2 N12 1.981(8) . ? Cu2 O3 2.444(6) . ? Cu3 O2 1.940(6) . ? Cu3 N11 1.950(7) . ? Cu3 N5 1.960(8) 2_645 ? Cu3 O3 1.964(6) . ? Cu3 O4 2.412(6) . ? Cu4 N1 1.934(8) . ? Cu4 O1 1.952(5) . ? Cu4 O3 1.963(6) . ? Cu4 N9 1.989(7) . ? Cu4 O2 2.557(6) . ? N3 Cu2 1.939(7) 2 ? N5 Cu3 1.960(8) 2_655 ? N7 Cu1 1.931(7) 4_565 ? N9 H9C 0.9000 . ? N9 H9D 0.9000 . ? C12 O2 1.397(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? N11 H11C 0.9000 . ? N11 H11D 0.9000 . ? N12 H12C 0.9000 . ? N12 H12D 0.9000 . ? O5 H5B 0.8501 . ? O5 H5A 0.8500 . ? O6 H6A 0.8499 . ? O6 H6B 0.8500 . ? 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 C1 Mo1 176.7(9) . . ? N2 C2 Mo1 177.4(9) . . ? N3 C3 Mo1 173.0(8) . . ? N4 C4 Mo1 176.8(9) . . ? N5 C5 Mo1 175.4(8) . . ? N6 C6 Mo1 176.8(9) . . ? N7 C7 Mo1 175.1(8) . . ? N8 C8 Mo1 177.3(8) . . ? N9 C9 C10 107.7(8) . . ? N9 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? N9 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? O1 C10 C9 107.6(7) . . ? O1 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? O1 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? C12 C11 N10 106.3(8) . . ? C12 C11 H11A 110.5 . . ? N10 C11 H11A 110.5 . . ? C12 C11 H11B 110.5 . . ? N10 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? C11 N10 Cu1 107.5(6) . . ? C11 N10 H10C 110.2 . . ? Cu1 N10 H10C 110.2 . . ? C11 N10 H10D 110.2 . . ? Cu1 N10 H10D 110.2 . . ? H10C N10 H10D 108.5 . . ? N11 C13 C14 107.5(8) . . ? N11 C13 H13A 110.2 . . ? C14 C13 H13A 110.2 . . ? N11 C13 H13B 110.2 . . ? C14 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? O3 C14 C13 108.7(7) . . ? O3 C14 H14A 109.9 . . ? C13 C14 H14A 109.9 . . ? O3 C14 H14B 109.9 . . ? C13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? N12 C15 C16 107.4(7) . . ? N12 C15 H15A 110.2 . . ? C16 C15 H15A 110.2 . . ? N12 C15 H15B 110.2 . . ? C16 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? O4 C16 C15 108.2(7) . . ? O4 C16 H16A 110.1 . . ? C15 C16 H16A 110.1 . . ? O4 C16 H16B 110.1 . . ? C15 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? O2 Cu1 N7 173.8(3) . 4_566 ? O2 Cu1 O4 86.2(2) . . ? N7 Cu1 O4 93.8(3) 4_566 . ? O2 Cu1 N10 84.7(3) . . ? N7 Cu1 N10 97.0(3) 4_566 . ? O4 Cu1 N10 160.7(3) . . ? O2 Cu1 O1 82.0(2) . . ? N7 Cu1 O1 92.1(3) 4_566 . ? O4 Cu1 O1 73.5(2) . . ? N10 Cu1 O1 121.9(3) . . ? O4 Cu2 N3 178.2(3) . 2_545 ? O4 Cu2 O1 86.5(2) . . ? N3 Cu2 O1 95.2(3) 2_545 . ? O4 Cu2 N12 84.9(3) . . ? N3 Cu2 N12 93.6(3) 2_545 . ? O1 Cu2 N12 166.7(3) . . ? O4 Cu2 O3 79.7(2) . . ? N3 Cu2 O3 100.0(3) 2_545 . ? O1 Cu2 O3 75.0(2) . . ? N12 Cu2 O3 113.1(3) . . ? O2 Cu3 N11 161.7(3) . . ? O2 Cu3 N5 97.9(3) . 2_645 ? N11 Cu3 N5 92.3(3) . 2_645 ? O2 Cu3 O3 88.3(2) . . ? N11 Cu3 O3 84.5(3) . . ? N5 Cu3 O3 168.2(3) 2_645 . ? O2 Cu3 O4 74.6(2) . . ? N11 Cu3 O4 120.2(3) . . ? N5 Cu3 O4 92.2(3) 2_645 . ? O3 Cu3 O4 79.7(2) . . ? N1 Cu4 O1 167.2(3) . . ? N1 Cu4 O3 94.3(3) . . ? O1 Cu4 O3 87.3(2) . . ? N1 Cu4 N9 96.1(3) . . ? O1 Cu4 N9 84.7(3) . . ? O3 Cu4 N9 165.5(3) . . ? N1 Cu4 O2 90.3(3) . . ? O1 Cu4 O2 78.1(2) . . ? O3 Cu4 O2 72.6(2) . . ? N9 Cu4 O2 117.4(3) . . ? C3 Mo1 C1 93.0(3) . . ? C3 Mo1 C7 93.6(3) . . ? C1 Mo1 C7 145.4(4) . . ? C3 Mo1 C5 145.9(4) . . ? C1 Mo1 C5 97.7(3) . . ? C7 Mo1 C5 95.6(3) . . ? C3 Mo1 C2 73.5(3) . . ? C1 Mo1 C2 69.0(4) . . ? C7 Mo1 C2 145.1(4) . . ? C5 Mo1 C2 80.4(3) . . ? C3 Mo1 C4 72.1(4) . . ? C1 Mo1 C4 77.0(3) . . ? C7 Mo1 C4 72.9(3) . . ? C5 Mo1 C4 141.8(4) . . ? C2 Mo1 C4 129.4(3) . . ? C3 Mo1 C8 144.7(4) . . ? C1 Mo1 C8 74.9(3) . . ? C7 Mo1 C8 80.3(3) . . ? C5 Mo1 C8 69.3(4) . . ? C2 Mo1 C8 128.5(4) . . ? C4 Mo1 C8 72.9(4) . . ? C3 Mo1 C6 76.7(3) . . ? C1 Mo1 C6 141.7(4) . . ? C7 Mo1 C6 72.7(3) . . ? C5 Mo1 C6 74.9(3) . . ? C2 Mo1 C6 72.8(3) . . ? C4 Mo1 C6 131.3(3) . . ? C8 Mo1 C6 132.3(3) . . ? C1 N1 Cu4 164.9(8) . . ? C3 N3 Cu2 162.0(8) . 2 ? C5 N5 Cu3 150.6(8) . 2_655 ? C7 N7 Cu1 162.8(7) . 4_565 ? C9 N9 Cu4 108.2(5) . . ? C9 N9 H9C 110.1 . . ? Cu4 N9 H9C 110.1 . . ? C9 N9 H9D 110.1 . . ? Cu4 N9 H9D 110.1 . . ? H9C N9 H9D 108.4 . . ? O2 C12 C11 109.3(8) . . ? O2 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? O2 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? C13 N11 Cu3 110.5(6) . . ? C13 N11 H11C 109.6 . . ? Cu3 N11 H11C 109.6 . . ? C13 N11 H11D 109.6 . . ? Cu3 N11 H11D 109.6 . . ? H11C N11 H11D 108.1 . . ? C15 N12 Cu2 108.8(5) . . ? C15 N12 H12C 109.9 . . ? Cu2 N12 H12C 109.9 . . ? C15 N12 H12D 109.9 . . ? Cu2 N12 H12D 109.9 . . ? H12C N12 H12D 108.3 . . ? C10 O1 Cu2 124.4(5) . . ? C10 O1 Cu4 110.5(5) . . ? Cu2 O1 Cu4 105.7(3) . . ? C10 O1 Cu1 120.3(5) . . ? Cu2 O1 Cu1 91.0(2) . . ? Cu4 O1 Cu1 101.5(2) . . ? C12 O2 Cu1 111.4(5) . . ? C12 O2 Cu3 122.4(5) . . ? Cu1 O2 Cu3 107.4(3) . . ? C12 O2 Cu4 124.8(6) . . ? Cu1 O2 Cu4 97.5(2) . . ? Cu3 O2 Cu4 89.2(2) . . ? C14 O3 Cu4 122.3(5) . . ? C14 O3 Cu3 110.7(5) . . ? Cu4 O3 Cu3 108.5(3) . . ? C14 O3 Cu2 123.7(6) . . ? Cu4 O3 Cu2 89.1(2) . . ? Cu3 O3 Cu2 98.7(2) . . ? C16 O4 Cu2 111.1(5) . . ? C16 O4 Cu1 123.2(5) . . ? Cu2 O4 Cu1 107.3(3) . . ? C16 O4 Cu3 120.5(5) . . ? Cu2 O4 Cu3 101.1(2) . . ? Cu1 O4 Cu3 90.2(2) . . ? H5B O5 H5A 109.1 . . ? H6A O6 H6B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.460 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.193 # Attachment 'WCu4.cif' data_WCu4 _database_code_depnum_ccdc_archive 'CCDC 666245' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H24 Cu4 N12 O4 W, 2(H2 O)' _chemical_formula_sum 'C16 H28 Cu4 N12 O6 W' _chemical_formula_weight 922.51 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7493(6) _cell_length_b 10.1924(5) _cell_length_c 23.4293(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.7220(10) _cell_angle_gamma 90.00 _cell_volume 2805.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 7.122 _exptl_absorpt_correction_type multi_scan _exptl_absorpt_correction_T_min 0.105 _exptl_absorpt_correction_T_max 0.194 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _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 15890 _diffrn_reflns_av_R_equivalents 0.0937 _diffrn_reflns_av_sigmaI/netI 0.0870 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6085 _reflns_number_gt 4595 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^] 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 6085 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _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 C1 C 0.1766(5) 0.3460(6) 0.2195(2) 0.0292(14) Uani 1 1 d . . . C2 C 0.1515(5) 0.5692(6) 0.1810(2) 0.0287(15) Uani 1 1 d . . . C3 C 0.0648(5) 0.4204(6) 0.1035(2) 0.0267(14) Uani 1 1 d . . . C4 C 0.1768(5) 0.2115(7) 0.1212(2) 0.0305(15) Uani 1 1 d . . . C5 C 0.3786(5) 0.5218(6) 0.1656(2) 0.0275(14) Uani 1 1 d . . . C6 C 0.2393(5) 0.5821(7) 0.0825(2) 0.0305(15) Uani 1 1 d . . . C7 C 0.3063(5) 0.3484(6) 0.0576(2) 0.0274(14) Uani 1 1 d . . . C8 C 0.3656(6) 0.2797(7) 0.1684(2) 0.0326(15) Uani 1 1 d . . . C9 C 0.0510(6) 0.3705(7) 0.4330(2) 0.0422(18) Uani 1 1 d . . . H9A H -0.0154 0.4075 0.4512 0.051 Uiso 1 1 calc R . . H9B H 0.1168 0.4234 0.4432 0.051 Uiso 1 1 calc R . . C10 C 0.0685(5) 0.2319(6) 0.4518(2) 0.0321(15) Uani 1 1 d . . . H10A H 0.0934 0.2297 0.4914 0.039 Uiso 1 1 calc R . . H10B H -0.0022 0.1833 0.4484 0.039 Uiso 1 1 calc R . . C11 C 0.3927(7) 0.4690(7) 0.3840(3) 0.049(2) Uani 1 1 d . . . H11A H 0.4446 0.5422 0.3795 0.058 Uiso 1 1 calc R . . H11B H 0.3153 0.5013 0.3808 0.058 Uiso 1 1 calc R . . N10 N 0.4117(5) 0.4044(5) 0.44052(19) 0.0400(14) Uani 1 1 d . . . H10C H 0.3743 0.4480 0.4679 0.048 Uiso 1 1 calc R . . H10D H 0.4863 0.4038 0.4496 0.048 Uiso 1 1 calc R . . C13 C 0.2575(7) -0.1091(8) 0.2531(3) 0.057(2) Uani 1 1 d . . . H13A H 0.2535 -0.1806 0.2804 0.069 Uiso 1 1 calc R . . H13B H 0.2442 -0.1448 0.2152 0.069 Uiso 1 1 calc R . . C14 C 0.1683(6) -0.0087(7) 0.2662(2) 0.0402(18) Uani 1 1 d . . . H14A H 0.1568 0.0489 0.2337 0.048 Uiso 1 1 calc R . . H14B H 0.0966 -0.0517 0.2743 0.048 Uiso 1 1 calc R . . C15 C 0.3680(5) -0.1960(6) 0.4186(2) 0.0330(16) Uani 1 1 d . . . H15A H 0.3884 -0.2084 0.3789 0.040 Uiso 1 1 calc R . . H15B H 0.4011 -0.2667 0.4409 0.040 Uiso 1 1 calc R . . C16 C 0.4107(5) -0.0670(5) 0.4396(2) 0.0275(14) Uani 1 1 d . . . H16A H 0.4041 -0.0619 0.4808 0.033 Uiso 1 1 calc R . . H16B H 0.4902 -0.0560 0.4299 0.033 Uiso 1 1 calc R . . Cu1 Cu 0.35266(6) 0.21973(8) 0.43388(3) 0.02574(18) Uani 1 1 d . . . Cu2 Cu 0.18504(6) -0.01438(7) 0.41279(3) 0.02461(17) Uani 1 1 d . . . Cu3 Cu 0.37147(6) 0.08749(8) 0.31434(3) 0.02755(18) Uani 1 1 d . . . Cu4 Cu 0.13513(6) 0.23099(8) 0.33721(3) 0.02920(19) Uani 1 1 d . . . W1 W 0.233980(19) 0.41020(2) 0.137293(8) 0.01924(7) Uani 1 1 d . . . N1 N 0.1481(5) 0.3075(5) 0.26257(19) 0.0347(14) Uani 1 1 d . . . N2 N 0.1021(5) 0.6503(6) 0.2037(2) 0.0529(17) Uani 1 1 d . . . N3 N -0.0268(5) 0.4349(5) 0.0882(2) 0.0383(14) Uani 1 1 d . . . N4 N 0.1473(6) 0.1065(6) 0.1117(2) 0.0527(17) Uani 1 1 d . . . N5 N 0.4611(5) 0.5768(6) 0.1781(2) 0.0370(14) Uani 1 1 d . . . N6 N 0.2425(5) 0.6742(6) 0.0542(2) 0.0463(16) Uani 1 1 d . . . N7 N 0.3388(4) 0.3140(5) 0.01463(18) 0.0326(13) Uani 1 1 d . . . N8 N 0.4342(5) 0.2096(6) 0.1868(2) 0.0545(18) Uani 1 1 d . . . N9 N 0.0345(5) 0.3680(5) 0.37002(18) 0.0400(15) Uani 1 1 d . . . H9C H 0.0518 0.4470 0.3552 0.048 Uiso 1 1 calc R . . H9D H -0.0387 0.3501 0.3613 0.048 Uiso 1 1 calc R . . C12 C 0.4142(6) 0.3668(6) 0.3398(2) 0.0370(17) Uani 1 1 d . . . H12A H 0.3922 0.3996 0.3024 0.044 Uiso 1 1 calc R . . H12B H 0.4946 0.3451 0.3392 0.044 Uiso 1 1 calc R . . N11 N 0.3682(5) -0.0494(6) 0.2560(2) 0.0435(15) Uani 1 1 d . . . H11C H 0.3852 -0.0144 0.2219 0.052 Uiso 1 1 calc R . . H11D H 0.4209 -0.1107 0.2644 0.052 Uiso 1 1 calc R . . N12 N 0.2428(4) -0.1957(5) 0.42426(19) 0.0331(13) Uani 1 1 d . . . H12C H 0.2239 -0.2246 0.4592 0.040 Uiso 1 1 calc R . . H12D H 0.2112 -0.2497 0.3981 0.040 Uiso 1 1 calc R . . O1 O 0.1532(3) 0.1742(4) 0.41626(14) 0.0250(9) Uani 1 1 d . . . O2 O 0.3499(3) 0.2541(4) 0.35296(14) 0.0260(9) Uani 1 1 d . . . O3 O 0.2059(3) 0.0657(4) 0.31484(14) 0.0268(10) Uani 1 1 d . . . O4 O 0.3435(3) 0.0324(4) 0.41311(14) 0.0233(9) Uani 1 1 d . . . O5 O 0.0982(4) 0.6460(5) 0.33246(18) 0.0546(14) Uani 1 1 d . . . H5B H 0.0990 0.6501 0.2962 0.066 Uiso 1 1 d R . . H5A H 0.0499 0.7013 0.3445 0.066 Uiso 1 1 d R . . O6 O 0.3191(5) 0.9440(5) 0.0408(2) 0.0778(19) Uani 1 1 d . . . H6A H 0.2735 0.9915 0.0597 0.093 Uiso 1 1 d R . . H6B H 0.2978 0.8646 0.0436 0.093 Uiso 1 1 d 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 C1 0.035(4) 0.025(4) 0.028(3) 0.006(3) 0.001(3) 0.009(3) C2 0.033(4) 0.034(4) 0.019(3) 0.002(3) 0.005(2) 0.000(3) C3 0.022(3) 0.030(4) 0.029(3) -0.004(3) 0.006(3) 0.005(3) C4 0.030(4) 0.037(4) 0.025(3) 0.000(3) 0.005(3) 0.002(3) C5 0.030(4) 0.033(4) 0.019(3) 0.005(3) 0.004(3) 0.001(3) C6 0.032(4) 0.037(4) 0.023(3) -0.003(3) 0.002(3) 0.001(3) C7 0.031(4) 0.027(4) 0.024(3) 0.000(3) -0.003(3) -0.001(3) C8 0.036(4) 0.031(4) 0.031(3) -0.001(3) 0.004(3) 0.000(3) C9 0.056(5) 0.046(5) 0.025(3) -0.006(3) 0.002(3) 0.017(4) C10 0.034(4) 0.040(4) 0.023(3) 0.001(3) 0.007(3) 0.013(3) C11 0.078(6) 0.031(4) 0.038(4) 0.001(3) 0.011(4) -0.007(4) N10 0.052(4) 0.036(3) 0.032(3) -0.007(3) 0.009(2) -0.013(3) C13 0.058(6) 0.063(6) 0.052(4) -0.026(4) 0.008(4) -0.010(5) C14 0.036(4) 0.051(5) 0.033(4) -0.014(3) -0.013(3) 0.000(4) C15 0.036(4) 0.033(4) 0.029(3) -0.001(3) -0.001(3) 0.006(3) C16 0.031(4) 0.024(4) 0.028(3) 0.002(3) -0.002(3) 0.003(3) Cu1 0.0335(4) 0.0266(4) 0.0172(3) 0.0002(3) 0.0031(3) -0.0037(4) Cu2 0.0228(4) 0.0258(4) 0.0252(4) 0.0027(3) -0.0030(3) -0.0010(3) Cu3 0.0249(4) 0.0303(4) 0.0274(4) -0.0045(3) 0.0009(3) 0.0035(4) Cu4 0.0361(5) 0.0326(5) 0.0190(4) 0.0063(3) 0.0063(3) 0.0094(4) W1 0.01893(13) 0.02414(14) 0.01466(11) 0.00158(10) 0.00113(8) -0.00088(11) N1 0.043(4) 0.036(3) 0.026(3) 0.013(2) 0.012(2) 0.004(3) N2 0.062(5) 0.046(4) 0.052(4) -0.017(3) 0.021(3) 0.010(4) N3 0.031(3) 0.041(4) 0.043(3) -0.003(3) -0.005(2) 0.006(3) N4 0.065(5) 0.035(4) 0.058(4) -0.006(3) 0.009(3) -0.011(4) N5 0.028(3) 0.049(4) 0.034(3) -0.003(3) 0.000(2) -0.009(3) N6 0.063(4) 0.038(4) 0.038(3) 0.009(3) 0.008(3) 0.004(3) N7 0.038(3) 0.043(4) 0.018(2) -0.001(2) 0.005(2) -0.005(3) N8 0.051(4) 0.054(4) 0.058(4) 0.011(3) 0.006(3) 0.024(4) N9 0.059(4) 0.034(3) 0.027(3) 0.006(2) 0.004(2) 0.019(3) C12 0.051(5) 0.032(4) 0.028(3) 0.006(3) 0.012(3) -0.007(4) N11 0.041(4) 0.050(4) 0.040(3) -0.008(3) 0.006(3) 0.002(3) N12 0.035(3) 0.032(3) 0.031(3) 0.002(2) -0.008(2) -0.005(3) O1 0.024(2) 0.032(3) 0.0189(19) 0.0036(18) 0.0031(16) 0.008(2) O2 0.034(2) 0.025(2) 0.0193(19) 0.0001(17) 0.0064(16) -0.003(2) O3 0.027(2) 0.033(3) 0.0202(19) -0.0041(18) -0.0007(16) 0.005(2) O4 0.023(2) 0.025(2) 0.023(2) 0.0041(18) 0.0014(16) 0.0012(19) O5 0.064(4) 0.054(3) 0.046(3) -0.016(3) 0.010(2) 0.000(3) O6 0.102(5) 0.048(4) 0.085(4) 0.000(3) 0.050(3) -0.002(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 C1 N1 1.137(6) . ? C1 W1 2.151(6) . ? C2 N2 1.145(7) . ? C2 W1 2.154(6) . ? C3 N3 1.140(7) . ? C3 W1 2.133(6) . ? C4 N4 1.145(8) . ? C4 W1 2.165(7) . ? C5 N5 1.155(7) . ? C5 W1 2.143(6) . ? C6 N6 1.150(7) . ? C6 W1 2.173(7) . ? C7 N7 1.136(6) . ? C7 W1 2.156(6) . ? C8 N8 1.157(8) . ? C8 W1 2.159(7) . ? C9 N9 1.486(7) . ? C9 C10 1.493(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O1 1.432(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N10 1.493(7) . ? C11 C12 1.493(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N10 Cu1 2.011(5) . ? N10 H10C 0.9000 . ? N10 H10D 0.9000 . ? C13 N11 1.438(9) . ? C13 C14 1.499(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O3 1.435(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N12 1.478(7) . ? C15 C16 1.490(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O4 1.423(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? Cu1 O2 1.928(3) . ? Cu1 N7 1.932(4) 4_566 ? Cu1 O4 1.973(4) . ? Cu1 O1 2.419(4) . ? Cu2 O4 1.922(4) . ? Cu2 N3 1.929(6) 2_545 ? Cu2 O1 1.960(4) . ? Cu2 N12 1.986(5) . ? Cu2 O3 2.451(3) . ? Cu3 O2 1.942(4) . ? Cu3 N11 1.953(5) . ? Cu3 O3 1.958(4) . ? Cu3 N5 1.976(5) 2_645 ? Cu3 O4 2.408(3) . ? Cu4 N1 1.923(5) . ? Cu4 O1 1.949(3) . ? Cu4 O3 1.953(4) . ? Cu4 N9 1.991(5) . ? Cu4 O2 2.557(4) . ? N3 Cu2 1.929(5) 2 ? N5 Cu3 1.976(5) 2_655 ? N7 Cu1 1.932(4) 4_565 ? N9 H9C 0.9000 . ? N9 H9D 0.9000 . ? C12 O2 1.411(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? N11 H11C 0.9000 . ? N11 H11D 0.9000 . ? N12 H12C 0.9000 . ? N12 H12D 0.9000 . ? O5 H5B 0.8500 . ? O5 H5A 0.8499 . ? O6 H6A 0.8500 . ? O6 H6B 0.8499 . ? 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 C1 W1 177.4(6) . . ? N2 C2 W1 176.3(6) . . ? N3 C3 W1 174.3(5) . . ? N4 C4 W1 178.8(6) . . ? N5 C5 W1 175.0(5) . . ? N6 C6 W1 178.9(5) . . ? N7 C7 W1 176.4(5) . . ? N8 C8 W1 177.6(6) . . ? N9 C9 C10 107.1(5) . . ? N9 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? N9 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.6 . . ? O1 C10 C9 108.1(5) . . ? O1 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O1 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? N10 C11 C12 106.5(6) . . ? N10 C11 H11A 110.4 . . ? C12 C11 H11A 110.4 . . ? N10 C11 H11B 110.4 . . ? C12 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? C11 N10 Cu1 107.3(4) . . ? C11 N10 H10C 110.3 . . ? Cu1 N10 H10C 110.3 . . ? C11 N10 H10D 110.3 . . ? Cu1 N10 H10D 110.3 . . ? H10C N10 H10D 108.5 . . ? N11 C13 C14 109.6(6) . . ? N11 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? N11 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? O3 C14 C13 108.3(5) . . ? O3 C14 H14A 110.0 . . ? C13 C14 H14A 110.0 . . ? O3 C14 H14B 110.0 . . ? C13 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? N12 C15 C16 107.4(5) . . ? N12 C15 H15A 110.2 . . ? C16 C15 H15A 110.2 . . ? N12 C15 H15B 110.2 . . ? C16 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? O4 C16 C15 107.5(4) . . ? O4 C16 H16A 110.2 . . ? C15 C16 H16A 110.2 . . ? O4 C16 H16B 110.2 . . ? C15 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? O2 Cu1 N7 174.21(19) . 4_566 ? O2 Cu1 O4 86.17(15) . . ? N7 Cu1 O4 93.68(19) 4_566 . ? O2 Cu1 N10 84.69(18) . . ? N7 Cu1 N10 97.1(2) 4_566 . ? O4 Cu1 N10 160.46(19) . . ? O2 Cu1 O1 82.12(14) . . ? N7 Cu1 O1 92.28(17) 4_566 . ? O4 Cu1 O1 73.89(14) . . ? N10 Cu1 O1 121.7(2) . . ? O4 Cu2 N3 178.7(2) . 2_545 ? O4 Cu2 O1 86.65(16) . . ? N3 Cu2 O1 94.5(2) 2_545 . ? O4 Cu2 N12 84.32(18) . . ? N3 Cu2 N12 94.6(2) 2_545 . ? O1 Cu2 N12 166.42(18) . . ? O4 Cu2 O3 79.19(14) . . ? N3 Cu2 O3 100.70(17) 2_545 . ? O1 Cu2 O3 74.55(13) . . ? N12 Cu2 O3 113.49(17) . . ? O2 Cu3 N11 161.6(2) . . ? O2 Cu3 O3 87.76(16) . . ? N11 Cu3 O3 84.99(19) . . ? O2 Cu3 N5 98.2(2) . 2_645 ? N11 Cu3 N5 91.9(2) . 2_645 ? O3 Cu3 N5 168.9(2) . 2_645 ? O2 Cu3 O4 74.68(14) . . ? N11 Cu3 O4 120.29(19) . . ? O3 Cu3 O4 79.64(13) . . ? N5 Cu3 O4 92.79(16) 2_645 . ? N1 Cu4 O1 167.3(2) . . ? N1 Cu4 O3 93.84(19) . . ? O1 Cu4 O3 87.54(15) . . ? N1 Cu4 N9 96.9(2) . . ? O1 Cu4 N9 84.24(17) . . ? O3 Cu4 N9 165.0(2) . . ? N1 Cu4 O2 90.26(18) . . ? O1 Cu4 O2 78.14(14) . . ? O3 Cu4 O2 72.26(14) . . ? N9 Cu4 O2 117.99(19) . . ? C3 W1 C5 145.1(2) . . ? C3 W1 C1 92.6(2) . . ? C5 W1 C1 98.1(2) . . ? C3 W1 C2 73.6(2) . . ? C5 W1 C2 79.2(2) . . ? C1 W1 C2 69.8(2) . . ? C3 W1 C7 93.9(2) . . ? C5 W1 C7 96.0(2) . . ? C1 W1 C7 144.9(2) . . ? C2 W1 C7 144.8(2) . . ? C3 W1 C8 144.6(2) . . ? C5 W1 C8 70.2(2) . . ? C1 W1 C8 75.0(2) . . ? C2 W1 C8 128.9(2) . . ? C7 W1 C8 79.8(2) . . ? C3 W1 C4 72.3(2) . . ? C5 W1 C4 142.5(2) . . ? C1 W1 C4 76.8(2) . . ? C2 W1 C4 130.2(2) . . ? C7 W1 C4 72.6(2) . . ? C8 W1 C4 72.7(2) . . ? C3 W1 C6 77.0(2) . . ? C5 W1 C6 74.1(2) . . ? C1 W1 C6 141.8(2) . . ? C2 W1 C6 72.0(2) . . ? C7 W1 C6 73.1(2) . . ? C8 W1 C6 132.1(2) . . ? C4 W1 C6 131.5(2) . . ? C1 N1 Cu4 167.1(5) . . ? C3 N3 Cu2 160.8(5) . 2 ? C5 N5 Cu3 151.9(6) . 2_655 ? C7 N7 Cu1 162.9(5) . 4_565 ? C9 N9 Cu4 108.9(4) . . ? C9 N9 H9C 109.9 . . ? Cu4 N9 H9C 109.9 . . ? C9 N9 H9D 109.9 . . ? Cu4 N9 H9D 109.9 . . ? H9C N9 H9D 108.3 . . ? O2 C12 C11 108.7(5) . . ? O2 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? O2 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.3 . . ? C13 N11 Cu3 110.2(4) . . ? C13 N11 H11C 109.6 . . ? Cu3 N11 H11C 109.6 . . ? C13 N11 H11D 109.6 . . ? Cu3 N11 H11D 109.6 . . ? H11C N11 H11D 108.1 . . ? C15 N12 Cu2 109.2(4) . . ? C15 N12 H12C 109.8 . . ? Cu2 N12 H12C 109.8 . . ? C15 N12 H12D 109.8 . . ? Cu2 N12 H12D 109.8 . . ? H12C N12 H12D 108.3 . . ? C10 O1 Cu4 111.2(3) . . ? C10 O1 Cu2 124.1(3) . . ? Cu4 O1 Cu2 105.69(17) . . ? C10 O1 Cu1 120.1(3) . . ? Cu4 O1 Cu1 101.49(15) . . ? Cu2 O1 Cu1 90.60(14) . . ? C12 O2 Cu1 111.1(3) . . ? C12 O2 Cu3 122.4(3) . . ? Cu1 O2 Cu3 107.37(19) . . ? C12 O2 Cu4 125.0(4) . . ? Cu1 O2 Cu4 97.43(15) . . ? Cu3 O2 Cu4 89.22(14) . . ? C14 O3 Cu4 122.8(3) . . ? C14 O3 Cu3 110.6(3) . . ? Cu4 O3 Cu3 109.29(19) . . ? C14 O3 Cu2 122.3(4) . . ? Cu4 O3 Cu2 89.31(13) . . ? Cu3 O3 Cu2 98.89(14) . . ? C16 O4 Cu2 110.9(3) . . ? C16 O4 Cu1 123.6(3) . . ? Cu2 O4 Cu1 106.92(18) . . ? C16 O4 Cu3 120.3(3) . . ? Cu2 O4 Cu3 101.43(14) . . ? Cu1 O4 Cu3 90.23(14) . . ? H5A O5 H5B 108.4 . . ? H6A O6 H6B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.178 _refine_diff_density_min -2.201 _refine_diff_density_rms 0.193