# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_JLU-Liu-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C15.50 H24.50 Cu4 N3.50 O19.50 S3' _chemical_formula_sum 'C15.50 H24.50 Cu4 N3.50 O19.50 S3' _chemical_formula_weight 922.23 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 13.6542(19) _cell_length_b 13.6542(19) _cell_length_c 42.160(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7860(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 2.362 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 49628 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.40 _reflns_number_total 9858 _reflns_number_gt 9015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material 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^)+(0.0587P)^2^+2.1645P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(1) _refine_ls_number_reflns 9858 _refine_ls_number_parameters 344 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.55767(3) 0.51279(3) 0.279284(9) 0.02707(9) Uani 1 1 d . . . Cu2 Cu 0.72394(3) 0.42180(3) 0.236332(8) 0.02606(9) Uani 1 1 d . . . Cu3 Cu 0.32772(3) 0.54182(3) 0.270364(9) 0.03181(9) Uani 1 1 d . . . Cu4 Cu 0.63234(4) 0.84817(3) 0.253978(9) 0.03774(11) Uani 1 1 d . . . S1 S 0.71554(6) 0.38635(6) 0.308206(18) 0.03132(17) Uani 1 1 d . . . S2 S 0.46042(7) 0.69980(6) 0.30074(2) 0.03726(19) Uani 1 1 d . . . S3 S 0.68642(7) 0.64860(6) 0.21550(2) 0.03644(19) Uani 1 1 d . . . O1 O 0.2078(2) 0.5486(2) 0.29446(7) 0.0533(8) Uani 1 1 d . . . O2 O 0.10041(18) 0.4311(2) 0.28302(5) 0.0410(6) Uani 1 1 d . . . O3 O 0.59106(14) 0.40894(14) 0.2500 0.0222(5) Uani 1 2 d S . . O4 O 0.45389(15) 0.54611(15) 0.2500 0.0250(6) Uani 1 2 d S . . O5 O 0.6540(2) 0.4747(2) 0.31065(6) 0.0433(6) Uani 1 1 d . . . O6 O 0.77848(18) 0.3967(2) 0.28024(6) 0.0439(6) Uani 1 1 d . . . O7 O 0.6495(2) 0.3017(2) 0.30391(6) 0.0484(7) Uani 1 1 d . . . O8 O 0.7732(2) 0.3740(2) 0.33646(6) 0.0463(6) Uani 1 1 d . . . O9 O 0.5283(2) 0.61837(19) 0.30832(6) 0.0466(7) Uani 1 1 d . . . O10 O 0.3607(2) 0.6603(2) 0.29633(8) 0.0590(8) Uani 1 1 d . . . O11 O 0.4926(3) 0.7451(2) 0.27059(6) 0.0509(7) Uani 1 1 d . . . O12 O 0.4612(2) 0.7703(2) 0.32594(7) 0.0537(7) Uani 1 1 d . . . O13 O 0.7100(2) 0.57859(18) 0.24087(7) 0.0460(6) Uani 1 1 d . . . O14 O 0.6964(3) 0.7479(2) 0.22912(8) 0.0615(9) Uani 1 1 d . . . O15 O 0.5861(2) 0.6330(3) 0.20483(7) 0.0601(9) Uani 1 1 d . . . O16 O 0.7533(2) 0.6403(3) 0.18881(8) 0.0608(8) Uani 1 1 d . . . O17 O 0.7004(3) 0.8130(3) 0.29256(8) 0.0631(5) Uani 1 1 d U . . N1 N -0.06726(19) 0.63829(18) 0.46926(6) 0.0274(5) Uani 1 1 d . . . N2 N -0.0877(2) 0.46912(18) 0.47213(6) 0.0281(5) Uani 1 1 d . . . N3 N 0.7866(3) 0.7146(3) 0.32377(10) 0.0631(5) Uani 1 1 d DU . . C1 C -0.0900(2) 0.5578(2) 0.48476(7) 0.0294(6) Uani 1 1 d . . . H1 H -0.1088 0.5636 0.5059 0.080 Uiso 1 1 calc . . . C2 C -0.0384(2) 0.6309(2) 0.43897(7) 0.0293(6) Uani 1 1 d . . . H2 H -0.0236 0.6874 0.4276 0.080 Uiso 1 1 calc . . . C3 C -0.0303(2) 0.5408(2) 0.42445(7) 0.0270(6) Uani 1 1 d . . . C4 C -0.0577(3) 0.4606(2) 0.44218(7) 0.0300(6) Uani 1 1 d . . . H4 H -0.0552 0.3988 0.4330 0.080 Uiso 1 1 calc . . . C5 C 0.0087(2) 0.5305(2) 0.39205(7) 0.0263(6) Uani 1 1 d . . . C6 C 0.0834(3) 0.5915(3) 0.38171(9) 0.0429(9) Uani 1 1 d . . . H6 H 0.1079 0.6396 0.3952 0.080 Uiso 1 1 calc . . . C7 C 0.1207(3) 0.5816(3) 0.35221(9) 0.0472(10) Uani 1 1 d . . . H7 H 0.1702 0.6237 0.3456 0.080 Uiso 1 1 calc . . . C8 C 0.0867(2) 0.5098(2) 0.33139(7) 0.0296(6) Uani 1 1 d . . . C9 C 0.0112(2) 0.4500(3) 0.34120(7) 0.0334(7) Uani 1 1 d . . . H9 H -0.0136 0.4024 0.3276 0.080 Uiso 1 1 calc . . . C10 C -0.0277(2) 0.4612(3) 0.37136(7) 0.0333(7) Uani 1 1 d . . . H10 H -0.0792 0.4213 0.3778 0.080 Uiso 1 1 calc . . . C11 C 0.1350(2) 0.4949(3) 0.30046(7) 0.0325(7) Uani 1 1 d . . . C12 C 0.7448(4) 0.7355(4) 0.29733(13) 0.0631(5) Uani 1 1 d U A . H12 H 0.7482 0.6900 0.2810 0.080 Uiso 1 1 calc . . . C13 C 0.8229(8) 0.8056(7) 0.3435(2) 0.0631(5) Uani 0.50 1 d PDU A 1 H13A H 0.8481 0.7839 0.3635 0.080 Uiso 0.50 1 calc P B 1 H13B H 0.7692 0.8497 0.3469 0.080 Uiso 0.50 1 calc P C 1 H13C H 0.8737 0.8388 0.3320 0.080 Uiso 0.50 1 calc P D 1 C13' C 0.7677(8) 0.7745(8) 0.3522(2) 0.0631(5) Uani 0.50 1 d PDU A 2 H13D H 0.8040 0.7486 0.3698 0.080 Uiso 0.50 1 calc P E 2 H13E H 0.6990 0.7731 0.3570 0.080 Uiso 0.50 1 calc P F 2 H13F H 0.7877 0.8408 0.3483 0.080 Uiso 0.50 1 calc P G 2 C14 C 0.8300(8) 0.6205(7) 0.3333(3) 0.0631(5) Uani 0.50 1 d PDU A 1 H14A H 0.8655 0.6287 0.3527 0.080 Uiso 0.50 1 calc P H 1 H14B H 0.8739 0.5983 0.3170 0.080 Uiso 0.50 1 calc P I 1 H14C H 0.7790 0.5730 0.3362 0.080 Uiso 0.50 1 calc P J 1 C14' C 0.8608(8) 0.6301(8) 0.3209(3) 0.0631(5) Uani 0.50 1 d PDU A 2 H14D H 0.8991 0.6263 0.3399 0.080 Uiso 0.50 1 calc P K 2 H14E H 0.9031 0.6419 0.3031 0.080 Uiso 0.50 1 calc P L 2 H14F H 0.8263 0.5696 0.3178 0.080 Uiso 0.50 1 calc P M 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.03309(19) 0.02670(18) 0.02141(17) 0.00004(13) -0.00036(14) 0.00115(15) Cu2 0.02228(17) 0.03265(19) 0.02326(17) 0.00344(14) 0.00496(13) 0.00078(15) Cu3 0.03052(19) 0.0348(2) 0.03016(19) 0.00278(16) 0.01170(15) -0.00068(16) Cu4 0.0625(3) 0.0285(2) 0.02218(18) -0.00123(15) -0.00388(18) 0.01462(19) S1 0.0321(4) 0.0403(4) 0.0215(3) 0.0064(3) -0.0032(3) -0.0042(3) S2 0.0523(5) 0.0272(4) 0.0323(4) -0.0031(3) 0.0120(4) -0.0021(4) S3 0.0385(4) 0.0307(4) 0.0402(4) 0.0010(3) 0.0171(4) 0.0032(3) O1 0.0492(16) 0.0563(17) 0.0544(17) -0.0102(14) 0.0319(14) -0.0135(14) O2 0.0360(13) 0.0633(17) 0.0236(11) -0.0079(11) 0.0023(9) -0.0040(12) O3 0.0232(8) 0.0232(8) 0.0203(13) 0.0034(8) 0.0034(8) 0.0020(11) O4 0.0257(8) 0.0257(8) 0.0235(13) 0.0026(8) 0.0026(8) 0.0009(11) O5 0.0467(14) 0.0542(16) 0.0289(11) -0.0094(11) -0.0103(10) 0.0089(12) O6 0.0280(11) 0.0769(19) 0.0268(11) 0.0138(12) 0.0017(9) -0.0009(12) O7 0.0647(18) 0.0474(15) 0.0332(13) 0.0157(11) -0.0150(12) -0.0223(13) O8 0.0452(14) 0.0647(18) 0.0289(12) 0.0085(12) -0.0113(11) -0.0051(13) O9 0.0745(19) 0.0350(13) 0.0302(12) -0.0058(10) -0.0046(12) 0.0075(13) O10 0.0559(17) 0.0473(16) 0.074(2) -0.0249(15) 0.0309(16) -0.0086(14) O11 0.078(2) 0.0403(14) 0.0345(13) 0.0064(11) 0.0024(13) -0.0140(14) O12 0.077(2) 0.0372(14) 0.0465(15) -0.0132(12) 0.0159(15) -0.0091(14) O13 0.0560(16) 0.0313(12) 0.0507(15) 0.0010(11) -0.0093(13) 0.0027(11) O14 0.090(2) 0.0287(13) 0.066(2) -0.0084(13) 0.0288(18) 0.0041(14) O15 0.0410(15) 0.105(3) 0.0340(14) 0.0061(16) 0.0084(12) 0.0136(16) O16 0.0600(18) 0.0638(19) 0.0586(18) -0.0101(15) 0.0330(15) -0.0096(15) O17 0.0643(6) 0.0629(6) 0.0622(6) 0.0011(4) -0.0026(4) 0.0033(4) N1 0.0332(13) 0.0226(12) 0.0265(12) -0.0042(10) 0.0074(10) -0.0014(10) N2 0.0463(15) 0.0193(11) 0.0187(11) -0.0021(9) -0.0018(10) -0.0012(11) N3 0.0643(6) 0.0629(6) 0.0622(6) 0.0011(4) -0.0026(4) 0.0033(4) C1 0.0364(16) 0.0247(14) 0.0271(14) -0.0033(11) 0.0047(12) -0.0026(12) C2 0.0346(16) 0.0243(14) 0.0292(14) -0.0052(11) 0.0072(12) -0.0065(13) C3 0.0312(15) 0.0285(14) 0.0212(13) -0.0011(11) 0.0033(11) 0.0005(12) C4 0.0468(18) 0.0244(14) 0.0187(13) 0.0000(11) 0.0033(12) 0.0006(13) C5 0.0327(15) 0.0252(14) 0.0211(13) -0.0011(11) 0.0040(11) -0.0002(12) C6 0.0444(19) 0.044(2) 0.0399(18) -0.0161(16) 0.0104(16) -0.0201(16) C7 0.051(2) 0.046(2) 0.045(2) -0.0121(17) 0.0197(17) -0.0238(18) C8 0.0289(14) 0.0364(16) 0.0234(14) -0.0032(12) 0.0080(12) 0.0018(13) C9 0.0326(16) 0.0438(18) 0.0238(14) -0.0073(13) 0.0034(12) -0.0066(15) C10 0.0351(17) 0.0393(18) 0.0255(14) -0.0042(12) 0.0063(12) -0.0096(14) C11 0.0263(15) 0.0459(18) 0.0253(14) 0.0031(13) 0.0076(12) 0.0039(14) C12 0.0643(6) 0.0629(6) 0.0622(6) 0.0011(4) -0.0026(4) 0.0033(4) C13 0.0643(6) 0.0629(6) 0.0622(6) 0.0011(4) -0.0026(4) 0.0033(4) C13' 0.0643(6) 0.0629(6) 0.0622(6) 0.0011(4) -0.0026(4) 0.0033(4) C14 0.0643(6) 0.0629(6) 0.0622(6) 0.0011(4) -0.0026(4) 0.0033(4) C14' 0.0643(6) 0.0629(6) 0.0622(6) 0.0011(4) -0.0026(4) 0.0033(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 Cu1 O9 1.933(3) . ? Cu1 O4 1.934(2) . ? Cu1 O3 1.9347(19) . ? Cu1 O5 1.937(2) . ? Cu1 Cu1 2.8192(9) 8_665 ? Cu2 O3 1.9117(17) . ? Cu2 O7 1.987(3) 8_665 ? Cu2 N1 2.020(3) 3_654 ? Cu2 O6 2.025(2) . ? Cu2 O13 2.158(3) . ? Cu2 Cu2 3.0412(8) 8_665 ? Cu3 O4 1.9258(18) . ? Cu3 O1 1.930(3) . ? Cu3 O10 2.005(3) . ? Cu3 O11 2.047(3) 8_665 ? Cu3 O15 2.105(3) 8_665 ? Cu3 Cu3 3.0488(8) 8_665 ? Cu4 O2 1.918(2) 8_665 ? Cu4 O14 1.933(3) . ? Cu4 O17 1.934(3) . ? Cu4 N2 2.028(3) 5 ? S1 O8 1.438(2) . ? S1 O6 1.466(2) . ? S1 O5 1.473(3) . ? S1 O7 1.477(3) . ? S2 O12 1.434(3) . ? S2 O10 1.477(3) . ? S2 O11 1.481(3) . ? S2 O9 1.483(3) . ? S3 O16 1.453(3) . ? S3 O15 1.458(3) . ? S3 O13 1.470(3) . ? S3 O14 1.479(3) . ? O1 C11 1.260(4) . ? O2 C11 1.234(4) . ? O2 Cu4 1.918(2) 8_665 ? O3 Cu2 1.9118(17) 8_665 ? O3 Cu1 1.9347(19) 8_665 ? O4 Cu3 1.9258(18) 8_665 ? O4 Cu1 1.934(2) 8_665 ? O7 Cu2 1.987(3) 8_665 ? O11 Cu3 2.047(3) 8_665 ? O15 Cu3 2.105(3) 8_665 ? O17 C12 1.237(6) . ? N1 C1 1.316(4) . ? N1 C2 1.340(4) . ? N1 Cu2 2.020(3) 4_465 ? N2 C1 1.323(4) . ? N2 C4 1.333(4) . ? N2 Cu4 2.028(3) 5_545 ? N3 C12 1.284(6) . ? N3 C14 1.471(10) . ? N3 C13' 1.473(10) . ? N3 C14' 1.540(10) . ? N3 C13 1.574(10) . ? C1 H1 0.9300 . ? C2 C3 1.379(4) . ? C2 H2 0.9300 . ? C3 C4 1.377(4) . ? C3 C5 1.473(4) . ? C4 H4 0.9300 . ? C5 C10 1.380(4) . ? C5 C6 1.387(5) . ? C6 C7 1.351(5) . ? C6 H6 0.9300 . ? C7 C8 1.395(5) . ? C7 H7 0.9300 . ? C8 C9 1.379(5) . ? C8 C11 1.475(4) . ? C9 C10 1.386(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C13' H13D 0.9600 . ? C13' H13E 0.9600 . ? C13' H13F 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Cu1 O4 94.41(11) . . ? O9 Cu1 O3 178.19(10) . . ? O4 Cu1 O3 86.43(9) . . ? O9 Cu1 O5 84.76(11) . . ? O4 Cu1 O5 175.59(9) . . ? O3 Cu1 O5 94.52(10) . . ? O9 Cu1 Cu1 137.59(8) . 8_665 ? O4 Cu1 Cu1 43.20(6) . 8_665 ? O3 Cu1 Cu1 43.23(6) . 8_665 ? O5 Cu1 Cu1 137.59(8) . 8_665 ? O3 Cu2 O7 92.59(8) . 8_665 ? O3 Cu2 N1 176.54(8) . 3_654 ? O7 Cu2 N1 84.02(11) 8_665 3_654 ? O3 Cu2 O6 93.32(8) . . ? O7 Cu2 O6 139.67(14) 8_665 . ? N1 Cu2 O6 89.76(10) 3_654 . ? O3 Cu2 O13 88.90(10) . . ? O7 Cu2 O13 123.13(12) 8_665 . ? N1 Cu2 O13 92.32(11) 3_654 . ? O6 Cu2 O13 96.86(12) . . ? O3 Cu2 Cu2 37.31(7) . 8_665 ? O7 Cu2 Cu2 83.55(8) 8_665 8_665 ? N1 Cu2 Cu2 142.46(7) 3_654 8_665 ? O6 Cu2 Cu2 77.49(8) . 8_665 ? O13 Cu2 Cu2 123.91(8) . 8_665 ? O4 Cu3 O1 173.04(10) . . ? O4 Cu3 O10 91.04(9) . . ? O1 Cu3 O10 82.20(12) . . ? O4 Cu3 O11 93.77(8) . 8_665 ? O1 Cu3 O11 92.43(13) . 8_665 ? O10 Cu3 O11 139.02(15) . 8_665 ? O4 Cu3 O15 91.08(12) . 8_665 ? O1 Cu3 O15 89.68(14) . 8_665 ? O10 Cu3 O15 109.94(14) . 8_665 ? O11 Cu3 O15 110.63(13) 8_665 8_665 ? O4 Cu3 Cu3 37.67(7) . 8_665 ? O1 Cu3 Cu3 139.86(10) . 8_665 ? O10 Cu3 Cu3 72.84(9) . 8_665 ? O11 Cu3 Cu3 86.74(8) 8_665 8_665 ? O15 Cu3 Cu3 128.00(11) 8_665 8_665 ? O2 Cu4 O14 91.30(14) 8_665 . ? O2 Cu4 O17 172.85(13) 8_665 . ? O14 Cu4 O17 93.61(15) . . ? O2 Cu4 N2 88.28(11) 8_665 5 ? O14 Cu4 N2 169.06(13) . 5 ? O17 Cu4 N2 85.92(13) . 5 ? O8 S1 O6 110.88(15) . . ? O8 S1 O5 110.49(17) . . ? O6 S1 O5 108.15(17) . . ? O8 S1 O7 110.14(16) . . ? O6 S1 O7 109.54(18) . . ? O5 S1 O7 107.56(18) . . ? O12 S2 O10 110.21(18) . . ? O12 S2 O11 110.68(17) . . ? O10 S2 O11 108.6(2) . . ? O12 S2 O9 109.81(18) . . ? O10 S2 O9 109.28(18) . . ? O11 S2 O9 108.24(18) . . ? O16 S3 O15 109.86(19) . . ? O16 S3 O13 112.0(2) . . ? O15 S3 O13 109.60(18) . . ? O16 S3 O14 108.31(19) . . ? O15 S3 O14 109.9(2) . . ? O13 S3 O14 107.07(18) . . ? C11 O1 Cu3 138.3(3) . . ? C11 O2 Cu4 131.6(2) . 8_665 ? Cu2 O3 Cu2 105.38(13) . 8_665 ? Cu2 O3 Cu1 118.79(2) . 8_665 ? Cu2 O3 Cu1 110.405(19) 8_665 8_665 ? Cu2 O3 Cu1 110.405(19) . . ? Cu2 O3 Cu1 118.79(2) 8_665 . ? Cu1 O3 Cu1 93.54(12) 8_665 . ? Cu3 O4 Cu3 104.67(14) 8_665 . ? Cu3 O4 Cu1 111.33(2) 8_665 8_665 ? Cu3 O4 Cu1 118.22(2) . 8_665 ? Cu3 O4 Cu1 118.22(2) 8_665 . ? Cu3 O4 Cu1 111.33(2) . . ? Cu1 O4 Cu1 93.60(13) 8_665 . ? S1 O5 Cu1 124.00(15) . . ? S1 O6 Cu2 122.42(15) . . ? S1 O7 Cu2 122.79(15) . 8_665 ? S2 O9 Cu1 123.53(15) . . ? S2 O10 Cu3 124.77(16) . . ? S2 O11 Cu3 116.91(17) . 8_665 ? S3 O13 Cu2 126.86(16) . . ? S3 O14 Cu4 144.9(2) . . ? S3 O15 Cu3 126.08(19) . 8_665 ? C12 O17 Cu4 125.8(4) . . ? C1 N1 C2 118.7(3) . . ? C1 N1 Cu2 125.7(2) . 4_465 ? C2 N1 Cu2 115.5(2) . 4_465 ? C1 N2 C4 117.9(3) . . ? C1 N2 Cu4 122.6(2) . 5_545 ? C4 N2 Cu4 119.5(2) . 5_545 ? C12 N3 C14 127.5(6) . . ? C12 N3 C13' 120.3(6) . . ? C14 N3 C13' 109.6(7) . . ? C12 N3 C14' 112.9(6) . . ? C14 N3 C14' 26.1(5) . . ? C13' N3 C14' 126.6(7) . . ? C12 N3 C13 115.0(5) . . ? C14 N3 C13 114.8(6) . . ? C13' N3 C13 35.8(5) . . ? C14' N3 C13 115.2(6) . . ? N1 C1 N2 124.0(3) . . ? N1 C1 H1 118.0 . . ? N2 C1 H1 118.0 . . ? N1 C2 C3 120.9(3) . . ? N1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 116.5(3) . . ? C4 C3 C5 121.7(3) . . ? C2 C3 C5 121.7(3) . . ? N2 C4 C3 121.9(3) . . ? N2 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C10 C5 C6 118.6(3) . . ? C10 C5 C3 121.4(3) . . ? C6 C5 C3 120.0(3) . . ? C7 C6 C5 120.4(3) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 121.7(3) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C9 C8 C7 118.4(3) . . ? C9 C8 C11 121.2(3) . . ? C7 C8 C11 120.3(3) . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C5 C10 C9 121.2(3) . . ? C5 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? O2 C11 O1 126.4(3) . . ? O2 C11 C8 116.9(3) . . ? O1 C11 C8 116.7(3) . . ? O17 C12 N3 123.3(5) . . ? O17 C12 H12 118.3 . . ? N3 C12 H12 118.3 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C13' H13D 109.5 . . ? N3 C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? N3 C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C14' H14D 109.5 . . ? N3 C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? N3 C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.907 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.080 _database_code_depnum_ccdc_archive 'CCDC 947183'