# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Lang, Jian-Ping' _publ_contact_author_email jplang@suda.edu.cn _publ_section_title ; Single-Crystal-to-Single-Crystal Structural Transformations of Two Sandwich-like Cu(II) Pyrazolate Complexes and Their Excellent Catalytic Performances in MMA Polymerization ; loop_ _publ_author_name H.-X.Li Z.-G.Ren D.Liu Y.Chen J.-P.Lang Z.-P.Cheng X.Zhu ; B.F.Abrahams ; # Attachment '- JPLangCIF.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 774537' #TrackingRef '- JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H88 Cu7 N18 O32' _chemical_formula_sum 'C54 H88 Cu7 N18 O32' _chemical_formula_weight 1946.27 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.329(2) _cell_length_b 18.527(3) _cell_length_c 16.144(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.400(3) _cell_angle_gamma 90.00 _cell_volume 3907.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7367 _cell_measurement_theta_min 3.1173 _cell_measurement_theta_max 27.4816 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1994 _exptl_absorpt_coefficient_mu 1.962 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5075 _exptl_absorpt_correction_T_max 0.8280 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Corp.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15750 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6840 _reflns_number_gt 6066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0346P)^2^+3.8790P] 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 6840 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.0950 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.008 _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 0.10826(3) 0.60139(3) 0.23487(3) 0.02439(12) Uani 1 1 d . . . Cu2 Cu 0.15544(3) 0.42577(2) 0.23498(3) 0.02409(12) Uani 1 1 d . . . Cu3 Cu 0.29078(3) 0.53720(2) 0.14251(3) 0.02350(12) Uani 1 1 d . . . Cu4 Cu 0.0000 0.5000 0.0000 0.02118(15) Uani 1 2 d S . . O1 O 0.4329(3) 0.83440(19) 0.1559(2) 0.0592(10) Uani 1 1 d . . . O2 O 0.3060(3) 0.8787(2) 0.2041(3) 0.0825(13) Uani 1 1 d . . . O3 O -0.1647(2) 0.51937(19) 0.46514(18) 0.0466(8) Uani 1 1 d . . . O4 O -0.1129(3) 0.40828(19) 0.47771(19) 0.0494(8) Uani 1 1 d . . . O5 O 0.4659(2) 0.21356(16) 0.19362(19) 0.0454(8) Uani 1 1 d . . . O6 O 0.5477(3) 0.28364(19) 0.1240(2) 0.0608(10) Uani 1 1 d . . . O7 O 0.21445(18) 0.52449(13) 0.23678(14) 0.0224(6) Uani 1 1 d . . . O8 O -0.0137(2) 0.66356(15) 0.19006(16) 0.0335(7) Uani 1 1 d . . . O9 O -0.0065(2) 0.57767(16) 0.09887(16) 0.0362(7) Uani 1 1 d . . . O10 O 0.0422(2) 0.42691(16) 0.09652(15) 0.0344(7) Uani 1 1 d . . . O11 O 0.0700(2) 0.33962(15) 0.18889(16) 0.0319(6) Uani 1 1 d . . . O12 O 0.30983(19) 0.54204(14) 0.02217(15) 0.0272(6) Uani 1 1 d . . . O13 O 0.14817(19) 0.52320(15) 0.02031(15) 0.0294(6) Uani 1 1 d . . . O14 O 0.1906(2) 0.6287(2) 0.37911(17) 0.0512(9) Uani 1 1 d . . . O15 O 0.2670(2) 0.4330(2) 0.39046(18) 0.0571(10) Uani 1 1 d . . . H15A H 0.2775 0.4557 0.3487 0.086 Uiso 1 1 calc R . . O16 O 0.4431(2) 0.56495(17) 0.2625(2) 0.0536(9) Uani 1 1 d . . . H16A H 0.4554 0.6088 0.2687 0.080 Uiso 1 1 calc R . . N1 N 0.2753(2) 0.64238(17) 0.15140(17) 0.0243(7) Uani 1 1 d . . . N2 N 0.2044(2) 0.66893(17) 0.19608(17) 0.0244(7) Uani 1 1 d . . . N3 N 0.3494(3) 0.8280(2) 0.1775(2) 0.0462(10) Uani 1 1 d . . . N4 N 0.0269(2) 0.53427(17) 0.29328(18) 0.0231(7) Uani 1 1 d . . . N5 N 0.0557(2) 0.46175(17) 0.29997(18) 0.0246(7) Uani 1 1 d . . . N6 N -0.1144(3) 0.4687(2) 0.4447(2) 0.0346(8) Uani 1 1 d . . . N7 N 0.2763(2) 0.38863(17) 0.19624(18) 0.0249(7) Uani 1 1 d . . . N8 N 0.3310(2) 0.43426(17) 0.15410(18) 0.0241(7) Uani 1 1 d . . . N9 N 0.4768(3) 0.27209(19) 0.1600(2) 0.0366(8) Uani 1 1 d . . . C1 C 0.4219(3) 0.6854(2) 0.0919(3) 0.0416(11) Uani 1 1 d . . . H1A H 0.4197 0.6365 0.0703 0.062 Uiso 1 1 calc R . . H1B H 0.4864 0.6933 0.1308 0.062 Uiso 1 1 calc R . . H1C H 0.4156 0.7193 0.0454 0.062 Uiso 1 1 calc R . . C2 C 0.3358(3) 0.6964(2) 0.1371(2) 0.0283(9) Uani 1 1 d . . . C3 C 0.3033(3) 0.7586(2) 0.1732(2) 0.0306(9) Uani 1 1 d . . . C4 C 0.2203(3) 0.7389(2) 0.2101(2) 0.0291(9) Uani 1 1 d . . . C5 C 0.1635(3) 0.7817(2) 0.2633(3) 0.0423(11) Uani 1 1 d . . . H5A H 0.1031 0.7552 0.2708 0.063 Uiso 1 1 calc R . . H5B H 0.1430 0.8275 0.2360 0.063 Uiso 1 1 calc R . . H5C H 0.2071 0.7903 0.3180 0.063 Uiso 1 1 calc R . . C6 C -0.0848(3) 0.6180(2) 0.3530(3) 0.0408(11) Uani 1 1 d . . . H6A H -0.0599 0.6523 0.3163 0.061 Uiso 1 1 calc R . . H6B H -0.0648 0.6338 0.4112 0.061 Uiso 1 1 calc R . . H6C H -0.1588 0.6152 0.3377 0.061 Uiso 1 1 calc R . . C7 C -0.0403(3) 0.5461(2) 0.3435(2) 0.0268(9) Uani 1 1 d . . . C8 C -0.0538(3) 0.4800(2) 0.3834(2) 0.0265(9) Uani 1 1 d . . . C9 C 0.0092(3) 0.4288(2) 0.3554(2) 0.0265(9) Uani 1 1 d . . . C10 C 0.0340(3) 0.3531(2) 0.3817(2) 0.0373(10) Uani 1 1 d . . . H10A H 0.0659 0.3294 0.3400 0.056 Uiso 1 1 calc R . . H10B H -0.0283 0.3278 0.3864 0.056 Uiso 1 1 calc R . . H10C H 0.0808 0.3527 0.4360 0.056 Uiso 1 1 calc R . . C11 C 0.2818(4) 0.2634(2) 0.2490(3) 0.0454(12) Uani 1 1 d . . . H11A H 0.2223 0.2795 0.2700 0.068 Uiso 1 1 calc R . . H11B H 0.3345 0.2478 0.2959 0.068 Uiso 1 1 calc R . . H11C H 0.2628 0.2235 0.2101 0.068 Uiso 1 1 calc R . . C12 C 0.3215(3) 0.3240(2) 0.2041(2) 0.0270(9) Uani 1 1 d . . . C16 C -0.0507(3) 0.6313(2) 0.1220(3) 0.0320(9) Uani 1 1 d . . . C13 C 0.4056(3) 0.3281(2) 0.1645(2) 0.0268(9) Uani 1 1 d . . . C14 C 0.4094(3) 0.3987(2) 0.1339(2) 0.0263(9) Uani 1 1 d . . . C15 C 0.4856(3) 0.4330(2) 0.0902(3) 0.0425(11) Uani 1 1 d . . . H15B H 0.4770 0.4141 0.0331 0.064 Uiso 1 1 calc R . . H15C H 0.5542 0.4223 0.1208 0.064 Uiso 1 1 calc R . . H15D H 0.4752 0.4848 0.0880 0.064 Uiso 1 1 calc R . . C17 C -0.1509(3) 0.6584(3) 0.0706(3) 0.0532(13) Uani 1 1 d . . . H17A H -0.1435 0.7085 0.0554 0.080 Uiso 1 1 calc R . . H17B H -0.2039 0.6545 0.1038 0.080 Uiso 1 1 calc R . . H17C H -0.1697 0.6296 0.0197 0.080 Uiso 1 1 calc R . . C18 C 0.0264(3) 0.3631(2) 0.1175(2) 0.0305(9) Uani 1 1 d . . . C19 C -0.0421(4) 0.3127(3) 0.0590(3) 0.0473(12) Uani 1 1 d . . . H19A H -0.0751 0.3389 0.0089 0.071 Uiso 1 1 calc R . . H19B H -0.0938 0.2933 0.0874 0.071 Uiso 1 1 calc R . . H19C H -0.0017 0.2736 0.0428 0.071 Uiso 1 1 calc R . . C20 C 0.2196(3) 0.5324(2) -0.0187(2) 0.0272(9) Uani 1 1 d . . . C21 C 0.2029(3) 0.5327(3) -0.1138(2) 0.0432(11) Uani 1 1 d . . . H21A H 0.1308 0.5259 -0.1373 0.065 Uiso 1 1 calc R . . H21B H 0.2419 0.4938 -0.1324 0.065 Uiso 1 1 calc R . . H21C H 0.2254 0.5785 -0.1329 0.065 Uiso 1 1 calc R . . C23 C 0.2848(4) 0.6619(3) 0.4191(3) 0.0537(14) Uani 1 1 d . . . H23A H 0.2711 0.6972 0.4606 0.064 Uiso 1 1 calc R . . H23B H 0.3141 0.6877 0.3765 0.064 Uiso 1 1 calc R . . C24 C 0.3600(4) 0.6080(3) 0.4620(3) 0.0664(16) Uani 1 1 d . . . H24A H 0.3320 0.5833 0.5054 0.100 Uiso 1 1 calc R . . H24B H 0.4229 0.6323 0.4878 0.100 Uiso 1 1 calc R . . H24C H 0.3743 0.5731 0.4210 0.100 Uiso 1 1 calc R . . C25 C 0.3604(4) 0.4000(3) 0.4327(3) 0.0559(14) Uani 1 1 d . . . H25A H 0.4025 0.4360 0.4683 0.067 Uiso 1 1 calc R . . H25B H 0.3988 0.3829 0.3907 0.067 Uiso 1 1 calc R . . C26 C 0.3401(5) 0.3382(3) 0.4861(4) 0.0809(19) Uani 1 1 d . . . H26A H 0.3073 0.3557 0.5308 0.121 Uiso 1 1 calc R . . H26B H 0.4042 0.3149 0.5107 0.121 Uiso 1 1 calc R . . H26C H 0.2954 0.3038 0.4515 0.121 Uiso 1 1 calc R . . C27 C 0.5300(4) 0.5247(3) 0.3034(3) 0.0523(13) Uani 1 1 d . . . H27A H 0.5191 0.4735 0.2890 0.063 Uiso 1 1 calc R . . H27B H 0.5370 0.5294 0.3648 0.063 Uiso 1 1 calc R . . C28 C 0.6265(4) 0.5495(3) 0.2785(4) 0.0776(19) Uani 1 1 d . . . H28A H 0.6189 0.5467 0.2176 0.116 Uiso 1 1 calc R . . H28B H 0.6828 0.5189 0.3051 0.116 Uiso 1 1 calc R . . H28C H 0.6404 0.5990 0.2967 0.116 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 Cu1 0.0232(2) 0.0242(3) 0.0281(2) 0.00143(19) 0.01060(19) 0.0010(2) Cu2 0.0237(2) 0.0223(3) 0.0291(2) 0.00025(19) 0.01229(19) -0.0013(2) Cu3 0.0257(2) 0.0194(3) 0.0286(2) 0.00106(18) 0.01314(19) 0.0005(2) Cu4 0.0208(3) 0.0216(4) 0.0219(3) 0.0010(2) 0.0060(2) -0.0006(3) O1 0.061(2) 0.041(2) 0.080(2) 0.0002(18) 0.0237(19) -0.0232(19) O2 0.105(3) 0.026(2) 0.130(4) -0.019(2) 0.057(3) -0.013(2) O3 0.0424(18) 0.060(2) 0.0454(17) -0.0021(16) 0.0281(15) 0.0058(17) O4 0.057(2) 0.052(2) 0.0485(18) 0.0114(16) 0.0322(16) -0.0022(18) O5 0.0495(19) 0.0250(17) 0.063(2) 0.0041(15) 0.0156(16) 0.0112(15) O6 0.054(2) 0.043(2) 0.099(3) 0.0093(19) 0.048(2) 0.0193(18) O7 0.0225(13) 0.0204(14) 0.0269(13) -0.0004(10) 0.0113(11) -0.0009(11) O8 0.0310(15) 0.0332(17) 0.0372(15) 0.0043(13) 0.0092(12) 0.0028(13) O9 0.0360(16) 0.0422(19) 0.0293(14) -0.0005(13) 0.0038(12) -0.0027(15) O10 0.0352(16) 0.0375(18) 0.0302(14) -0.0024(13) 0.0057(12) -0.0090(14) O11 0.0324(15) 0.0314(16) 0.0339(15) -0.0038(12) 0.0114(12) -0.0080(13) O12 0.0261(14) 0.0275(15) 0.0302(14) -0.0019(11) 0.0111(11) -0.0012(12) O13 0.0239(14) 0.0386(17) 0.0271(13) 0.0007(12) 0.0089(11) -0.0042(13) O14 0.0439(19) 0.075(3) 0.0339(16) -0.0031(16) 0.0067(14) -0.0286(18) O15 0.047(2) 0.086(3) 0.0372(17) 0.0124(17) 0.0051(15) 0.0195(19) O16 0.0400(18) 0.0300(18) 0.081(2) -0.0042(16) -0.0114(17) 0.0011(15) N1 0.0265(17) 0.0244(18) 0.0234(15) -0.0004(13) 0.0083(13) 0.0000(14) N2 0.0268(17) 0.0217(18) 0.0262(16) -0.0006(13) 0.0085(13) 0.0014(14) N3 0.062(3) 0.028(2) 0.049(2) -0.0012(17) 0.012(2) -0.012(2) N4 0.0198(16) 0.0237(18) 0.0265(15) -0.0003(13) 0.0058(13) -0.0010(14) N5 0.0226(16) 0.0254(18) 0.0263(16) 0.0012(13) 0.0063(13) -0.0002(14) N6 0.0289(19) 0.049(2) 0.0290(17) -0.0022(17) 0.0128(15) -0.0039(18) N7 0.0249(17) 0.0214(18) 0.0308(16) 0.0009(13) 0.0117(13) -0.0002(14) N8 0.0254(17) 0.0187(17) 0.0302(16) 0.0000(13) 0.0102(13) -0.0025(14) N9 0.038(2) 0.029(2) 0.045(2) -0.0051(16) 0.0116(17) 0.0052(17) C1 0.045(3) 0.039(3) 0.047(2) -0.001(2) 0.023(2) -0.014(2) C2 0.031(2) 0.025(2) 0.030(2) 0.0039(16) 0.0082(17) -0.0035(18) C3 0.037(2) 0.019(2) 0.036(2) 0.0020(17) 0.0086(18) -0.0049(19) C4 0.033(2) 0.018(2) 0.034(2) -0.0028(16) 0.0009(17) 0.0002(18) C5 0.045(3) 0.034(3) 0.050(3) -0.012(2) 0.014(2) 0.006(2) C6 0.039(3) 0.045(3) 0.044(2) 0.004(2) 0.024(2) 0.006(2) C7 0.0203(19) 0.034(2) 0.0275(19) -0.0035(16) 0.0074(16) -0.0020(18) C8 0.0212(19) 0.036(2) 0.0242(18) -0.0018(16) 0.0086(15) -0.0058(18) C9 0.024(2) 0.030(2) 0.0255(18) 0.0001(16) 0.0051(16) -0.0071(18) C10 0.049(3) 0.031(2) 0.036(2) 0.0029(18) 0.018(2) -0.005(2) C11 0.045(3) 0.029(3) 0.064(3) 0.012(2) 0.015(2) 0.004(2) C12 0.028(2) 0.022(2) 0.032(2) -0.0019(16) 0.0099(16) -0.0013(18) C16 0.026(2) 0.029(2) 0.043(2) 0.0124(19) 0.0110(18) -0.0004(19) C13 0.028(2) 0.020(2) 0.033(2) -0.0078(16) 0.0075(16) 0.0068(17) C14 0.027(2) 0.022(2) 0.0310(19) -0.0033(16) 0.0095(16) 0.0018(17) C15 0.039(3) 0.031(3) 0.066(3) 0.006(2) 0.034(2) 0.008(2) C17 0.039(3) 0.057(3) 0.059(3) 0.014(3) -0.001(2) 0.007(3) C18 0.025(2) 0.040(3) 0.031(2) -0.0074(18) 0.0143(17) -0.0055(19) C19 0.053(3) 0.049(3) 0.041(2) -0.011(2) 0.011(2) -0.019(3) C20 0.033(2) 0.018(2) 0.032(2) 0.0016(16) 0.0099(18) 0.0011(18) C21 0.046(3) 0.058(3) 0.027(2) -0.001(2) 0.0123(19) -0.004(2) C23 0.046(3) 0.060(3) 0.052(3) -0.003(2) 0.003(2) -0.023(3) C24 0.048(3) 0.076(4) 0.070(4) -0.003(3) -0.001(3) -0.007(3) C25 0.040(3) 0.062(4) 0.062(3) 0.010(3) 0.001(2) 0.009(3) C26 0.072(4) 0.075(5) 0.088(4) 0.021(4) -0.002(4) -0.002(4) C27 0.046(3) 0.041(3) 0.063(3) 0.004(2) -0.005(2) 0.008(2) C28 0.048(3) 0.043(3) 0.138(6) -0.010(3) 0.008(4) 0.012(3) _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 N2 1.979(3) . ? Cu1 N4 2.004(3) . ? Cu1 O7 2.004(2) . ? Cu1 O8 2.007(3) . ? Cu1 O14 2.423(3) . ? Cu2 N7 1.964(3) . ? Cu2 N5 1.966(3) . ? Cu2 O7 1.989(2) . ? Cu2 O11 2.016(3) . ? Cu2 O10 2.437(2) . ? Cu3 N1 1.968(3) . ? Cu3 N8 1.980(3) . ? Cu3 O7 2.005(2) . ? Cu3 O12 2.010(2) . ? Cu4 O13 1.984(3) . ? Cu4 O13 1.984(3) 3_565 ? Cu4 O10 2.057(3) 3_565 ? Cu4 O10 2.057(3) . ? Cu4 O9 2.163(3) 3_565 ? Cu4 O9 2.163(3) . ? O1 N3 1.236(5) . ? O2 N3 1.225(5) . ? O3 N6 1.236(4) . ? O4 N6 1.237(4) . ? O5 N9 1.234(4) . ? O6 N9 1.222(4) . ? O8 C16 1.263(5) . ? O9 C16 1.249(5) . ? O10 C18 1.259(5) . ? O11 C18 1.261(4) . ? O12 C20 1.265(4) . ? O13 C20 1.253(4) . ? O14 C23 1.432(5) . ? O15 C25 1.433(5) . ? O15 H15A 0.8300 . ? O16 C27 1.425(5) . ? O16 H16A 0.8300 . ? N1 C2 1.334(5) . ? N1 N2 1.387(4) . ? N2 C4 1.326(5) . ? N3 C3 1.421(5) . ? N4 C7 1.339(5) . ? N4 N5 1.396(4) . ? N5 C9 1.333(5) . ? N6 C8 1.411(5) . ? N7 C12 1.336(5) . ? N7 N8 1.380(4) . ? N8 C14 1.329(5) . ? N9 C13 1.418(5) . ? C1 C2 1.491(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C3 1.397(5) . ? C3 C4 1.404(6) . ? C4 C5 1.483(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.479(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.412(5) . ? C8 C9 1.400(5) . ? C9 C10 1.483(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.489(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 C13 1.398(5) . ? C16 C17 1.512(5) . ? C13 C14 1.402(5) . ? C14 C15 1.489(5) . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C15 H15D 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C19 1.502(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 C21 1.507(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C23 C24 1.486(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.490(7) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 C28 1.494(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? 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 N2 Cu1 N4 170.28(12) . . ? N2 Cu1 O7 87.41(11) . . ? N4 Cu1 O7 89.89(11) . . ? N2 Cu1 O8 93.00(12) . . ? N4 Cu1 O8 92.88(12) . . ? O7 Cu1 O8 158.87(10) . . ? N2 Cu1 O14 88.48(11) . . ? N4 Cu1 O14 82.05(11) . . ? O7 Cu1 O14 87.08(11) . . ? O8 Cu1 O14 114.05(12) . . ? N7 Cu2 N5 166.55(12) . . ? N7 Cu2 O7 88.85(12) . . ? N5 Cu2 O7 89.29(12) . . ? N7 Cu2 O11 92.54(12) . . ? N5 Cu2 O11 94.18(12) . . ? O7 Cu2 O11 157.89(10) . . ? N7 Cu2 O10 96.25(11) . . ? N5 Cu2 O10 97.19(11) . . ? O7 Cu2 O10 100.18(10) . . ? O11 Cu2 O10 57.73(10) . . ? N1 Cu3 N8 167.80(12) . . ? N1 Cu3 O7 89.11(11) . . ? N8 Cu3 O7 89.05(11) . . ? N1 Cu3 O12 93.52(11) . . ? N8 Cu3 O12 92.92(11) . . ? O7 Cu3 O12 156.76(10) . . ? O13 Cu4 O13 180.00(14) . 3_565 ? O13 Cu4 O10 95.57(11) . 3_565 ? O13 Cu4 O10 84.43(11) 3_565 3_565 ? O13 Cu4 O10 84.43(11) . . ? O13 Cu4 O10 95.57(11) 3_565 . ? O10 Cu4 O10 180.00(12) 3_565 . ? O13 Cu4 O9 94.72(11) . 3_565 ? O13 Cu4 O9 85.28(11) 3_565 3_565 ? O10 Cu4 O9 85.64(11) 3_565 3_565 ? O10 Cu4 O9 94.36(11) . 3_565 ? O13 Cu4 O9 85.28(11) . . ? O13 Cu4 O9 94.72(11) 3_565 . ? O10 Cu4 O9 94.36(11) 3_565 . ? O10 Cu4 O9 85.64(11) . . ? O9 Cu4 O9 180.00(15) 3_565 . ? Cu2 O7 Cu1 112.17(12) . . ? Cu2 O7 Cu3 110.83(11) . . ? Cu1 O7 Cu3 111.57(11) . . ? C16 O8 Cu1 101.0(2) . . ? C16 O9 Cu4 147.1(3) . . ? C18 O10 Cu4 141.9(2) . . ? C18 O10 Cu2 81.4(2) . . ? Cu4 O10 Cu2 136.68(13) . . ? C18 O11 Cu2 100.9(2) . . ? C20 O12 Cu3 102.1(2) . . ? C20 O13 Cu4 141.0(2) . . ? C23 O14 Cu1 135.5(3) . . ? C25 O15 H15A 109.5 . . ? C27 O16 H16A 109.5 . . ? C2 N1 N2 108.7(3) . . ? C2 N1 Cu3 130.9(3) . . ? N2 N1 Cu3 118.8(2) . . ? C4 N2 N1 109.4(3) . . ? C4 N2 Cu1 131.0(3) . . ? N1 N2 Cu1 119.4(2) . . ? O2 N3 O1 122.6(4) . . ? O2 N3 C3 118.8(4) . . ? O1 N3 C3 118.5(4) . . ? C7 N4 N5 108.5(3) . . ? C7 N4 Cu1 132.2(3) . . ? N5 N4 Cu1 117.9(2) . . ? C9 N5 N4 109.6(3) . . ? C9 N5 Cu2 131.0(3) . . ? N4 N5 Cu2 119.3(2) . . ? O3 N6 O4 122.4(3) . . ? O3 N6 C8 119.3(4) . . ? O4 N6 C8 118.3(4) . . ? C12 N7 N8 108.9(3) . . ? C12 N7 Cu2 131.9(3) . . ? N8 N7 Cu2 119.3(2) . . ? C14 N8 N7 109.6(3) . . ? C14 N8 Cu3 131.7(3) . . ? N7 N8 Cu3 118.5(2) . . ? O6 N9 O5 122.2(4) . . ? O6 N9 C13 118.9(4) . . ? O5 N9 C13 118.8(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 107.4(3) . . ? N1 C2 C1 122.2(4) . . ? C3 C2 C1 130.5(4) . . ? C2 C3 C4 107.3(3) . . ? C2 C3 N3 126.9(4) . . ? C4 C3 N3 125.7(4) . . ? N2 C4 C3 107.1(4) . . ? N2 C4 C5 122.5(4) . . ? C3 C4 C5 130.0(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 C8 107.1(3) . . ? N4 C7 C6 122.7(4) . . ? C8 C7 C6 130.1(3) . . ? C9 C8 N6 126.0(4) . . ? C9 C8 C7 107.6(3) . . ? N6 C8 C7 126.3(4) . . ? N5 C9 C8 107.1(3) . . ? N5 C9 C10 121.2(4) . . ? C8 C9 C10 131.5(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N7 C12 C13 107.2(3) . . ? N7 C12 C11 121.7(4) . . ? C13 C12 C11 131.1(4) . . ? O9 C16 O8 120.7(4) . . ? O9 C16 C17 121.2(4) . . ? O8 C16 C17 118.1(4) . . ? C12 C13 C14 107.4(3) . . ? C12 C13 N9 126.1(4) . . ? C14 C13 N9 126.5(4) . . ? N8 C14 C13 107.0(3) . . ? N8 C14 C15 123.2(3) . . ? C13 C14 C15 129.8(4) . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C15 H15D 109.5 . . ? H15B C15 H15D 109.5 . . ? H15C C15 H15D 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O10 C18 O11 119.9(3) . . ? O10 C18 C19 121.8(4) . . ? O11 C18 C19 118.3(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O13 C20 O12 119.7(3) . . ? O13 C20 C21 122.6(3) . . ? O12 C20 C21 117.7(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O14 C23 C24 111.8(4) . . ? O14 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? O14 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O15 C25 C26 111.3(4) . . ? O15 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? O15 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O16 C27 C28 112.2(4) . . ? O16 C27 H27A 109.2 . . ? C28 C27 H27A 109.2 . . ? O16 C27 H27B 109.2 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? 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 N7 Cu2 O7 Cu1 160.52(13) . . . . ? N5 Cu2 O7 Cu1 -32.81(13) . . . . ? O11 Cu2 O7 Cu1 66.6(3) . . . . ? O10 Cu2 O7 Cu1 64.37(12) . . . . ? N7 Cu2 O7 Cu3 35.08(13) . . . . ? N5 Cu2 O7 Cu3 -158.25(13) . . . . ? O11 Cu2 O7 Cu3 -58.8(3) . . . . ? O10 Cu2 O7 Cu3 -61.07(13) . . . . ? N2 Cu1 O7 Cu2 -160.64(13) . . . . ? N4 Cu1 O7 Cu2 28.71(13) . . . . ? O8 Cu1 O7 Cu2 -69.0(3) . . . . ? O14 Cu1 O7 Cu2 110.75(12) . . . . ? N2 Cu1 O7 Cu3 -35.61(13) . . . . ? N4 Cu1 O7 Cu3 153.74(13) . . . . ? O8 Cu1 O7 Cu3 56.0(3) . . . . ? O14 Cu1 O7 Cu3 -124.22(12) . . . . ? N1 Cu3 O7 Cu2 158.62(13) . . . . ? N8 Cu3 O7 Cu2 -33.44(13) . . . . ? O12 Cu3 O7 Cu2 61.7(3) . . . . ? N1 Cu3 O7 Cu1 32.84(13) . . . . ? N8 Cu3 O7 Cu1 -159.22(13) . . . . ? O12 Cu3 O7 Cu1 -64.0(3) . . . . ? N2 Cu1 O8 C16 100.5(2) . . . . ? N4 Cu1 O8 C16 -87.2(2) . . . . ? O7 Cu1 O8 C16 10.0(4) . . . . ? O14 Cu1 O8 C16 -169.8(2) . . . . ? O13 Cu4 O9 C16 131.7(5) . . . . ? O13 Cu4 O9 C16 -48.3(5) 3_565 . . . ? O10 Cu4 O9 C16 36.4(5) 3_565 . . . ? O10 Cu4 O9 C16 -143.6(5) . . . . ? O13 Cu4 O10 C18 -137.0(4) . . . . ? O9 Cu4 O10 C18 -42.7(4) 3_565 . . . ? O9 Cu4 O10 C18 137.3(4) . . . . ? O13 Cu4 O10 Cu2 43.58(19) . . . . ? O13 Cu4 O10 Cu2 -136.42(19) 3_565 . . . ? O9 Cu4 O10 Cu2 137.91(19) 3_565 . . . ? O9 Cu4 O10 Cu2 -42.09(19) . . . . ? N7 Cu2 O10 C18 87.9(2) . . . . ? N5 Cu2 O10 C18 -91.5(2) . . . . ? O7 Cu2 O10 C18 177.9(2) . . . . ? O11 Cu2 O10 C18 -1.1(2) . . . . ? N7 Cu2 O10 Cu4 -92.4(2) . . . . ? N5 Cu2 O10 Cu4 88.1(2) . . . . ? O7 Cu2 O10 Cu4 -2.5(2) . . . . ? O11 Cu2 O10 Cu4 178.5(2) . . . . ? N7 Cu2 O11 C18 -94.7(2) . . . . ? N5 Cu2 O11 C18 97.0(2) . . . . ? O7 Cu2 O11 C18 -1.5(4) . . . . ? O10 Cu2 O11 C18 1.1(2) . . . . ? N1 Cu3 O12 C20 -93.6(2) . . . . ? N8 Cu3 O12 C20 96.7(2) . . . . ? O7 Cu3 O12 C20 2.3(4) . . . . ? O10 Cu4 O13 C20 -47.3(4) 3_565 . . . ? O10 Cu4 O13 C20 132.7(4) . . . . ? O9 Cu4 O13 C20 38.7(4) 3_565 . . . ? O9 Cu4 O13 C20 -141.3(4) . . . . ? N2 Cu1 O14 C23 -15.7(4) . . . . ? N4 Cu1 O14 C23 162.1(5) . . . . ? O7 Cu1 O14 C23 71.8(4) . . . . ? O8 Cu1 O14 C23 -108.3(4) . . . . ? N8 Cu3 N1 C2 67.1(7) . . . . ? O7 Cu3 N1 C2 148.5(3) . . . . ? O12 Cu3 N1 C2 -54.6(3) . . . . ? N8 Cu3 N1 N2 -96.6(6) . . . . ? O7 Cu3 N1 N2 -15.2(2) . . . . ? O12 Cu3 N1 N2 141.7(2) . . . . ? C2 N1 N2 C4 -0.2(4) . . . . ? Cu3 N1 N2 C4 166.9(2) . . . . ? C2 N1 N2 Cu1 -175.8(2) . . . . ? Cu3 N1 N2 Cu1 -8.7(3) . . . . ? O7 Cu1 N2 C4 -147.2(3) . . . . ? O8 Cu1 N2 C4 54.0(3) . . . . ? O14 Cu1 N2 C4 -60.0(3) . . . . ? O7 Cu1 N2 N1 27.3(2) . . . . ? O8 Cu1 N2 N1 -131.5(2) . . . . ? O14 Cu1 N2 N1 114.5(2) . . . . ? O7 Cu1 N4 C7 153.5(3) . . . . ? O8 Cu1 N4 C7 -47.4(3) . . . . ? O14 Cu1 N4 C7 66.5(3) . . . . ? O7 Cu1 N4 N5 -11.2(2) . . . . ? O8 Cu1 N4 N5 147.9(2) . . . . ? O14 Cu1 N4 N5 -98.2(2) . . . . ? C7 N4 N5 C9 -1.6(4) . . . . ? Cu1 N4 N5 C9 166.5(2) . . . . ? C7 N4 N5 Cu2 -179.4(2) . . . . ? Cu1 N4 N5 Cu2 -11.3(3) . . . . ? N7 Cu2 N5 C9 -68.1(7) . . . . ? O7 Cu2 N5 C9 -150.2(3) . . . . ? O11 Cu2 N5 C9 51.7(3) . . . . ? O10 Cu2 N5 C9 109.7(3) . . . . ? N7 Cu2 N5 N4 109.2(5) . . . . ? O7 Cu2 N5 N4 27.1(2) . . . . ? O11 Cu2 N5 N4 -131.1(2) . . . . ? O10 Cu2 N5 N4 -73.1(2) . . . . ? N5 Cu2 N7 C12 71.4(7) . . . . ? O7 Cu2 N7 C12 153.5(3) . . . . ? O11 Cu2 N7 C12 -48.5(3) . . . . ? O10 Cu2 N7 C12 -106.4(3) . . . . ? N5 Cu2 N7 N8 -106.9(6) . . . . ? O7 Cu2 N7 N8 -24.7(2) . . . . ? O11 Cu2 N7 N8 133.2(2) . . . . ? O10 Cu2 N7 N8 75.4(2) . . . . ? C12 N7 N8 C14 1.1(4) . . . . ? Cu2 N7 N8 C14 179.8(2) . . . . ? C12 N7 N8 Cu3 -174.0(2) . . . . ? Cu2 N7 N8 Cu3 4.6(3) . . . . ? N1 Cu3 N8 C14 -74.4(7) . . . . ? O7 Cu3 N8 C14 -155.7(3) . . . . ? O12 Cu3 N8 C14 47.4(3) . . . . ? N1 Cu3 N8 N7 99.5(6) . . . . ? O7 Cu3 N8 N7 18.1(2) . . . . ? O12 Cu3 N8 N7 -138.7(2) . . . . ? N2 N1 C2 C3 0.0(4) . . . . ? Cu3 N1 C2 C3 -165.0(3) . . . . ? N2 N1 C2 C1 178.6(3) . . . . ? Cu3 N1 C2 C1 13.7(5) . . . . ? N1 C2 C3 C4 0.2(4) . . . . ? C1 C2 C3 C4 -178.3(4) . . . . ? N1 C2 C3 N3 176.1(4) . . . . ? C1 C2 C3 N3 -2.4(7) . . . . ? O2 N3 C3 C2 173.1(4) . . . . ? O1 N3 C3 C2 -8.4(6) . . . . ? O2 N3 C3 C4 -11.6(6) . . . . ? O1 N3 C3 C4 166.8(4) . . . . ? N1 N2 C4 C3 0.3(4) . . . . ? Cu1 N2 C4 C3 175.2(2) . . . . ? N1 N2 C4 C5 -174.1(3) . . . . ? Cu1 N2 C4 C5 0.9(6) . . . . ? C2 C3 C4 N2 -0.3(4) . . . . ? N3 C3 C4 N2 -176.3(4) . . . . ? C2 C3 C4 C5 173.5(4) . . . . ? N3 C3 C4 C5 -2.5(7) . . . . ? N5 N4 C7 C8 0.5(4) . . . . ? Cu1 N4 C7 C8 -165.3(2) . . . . ? N5 N4 C7 C6 178.6(3) . . . . ? Cu1 N4 C7 C6 12.8(5) . . . . ? O3 N6 C8 C9 178.2(3) . . . . ? O4 N6 C8 C9 0.1(6) . . . . ? O3 N6 C8 C7 2.8(6) . . . . ? O4 N6 C8 C7 -175.3(4) . . . . ? N4 C7 C8 C9 0.7(4) . . . . ? C6 C7 C8 C9 -177.2(4) . . . . ? N4 C7 C8 N6 176.8(3) . . . . ? C6 C7 C8 N6 -1.1(6) . . . . ? N4 N5 C9 C8 2.0(4) . . . . ? Cu2 N5 C9 C8 179.4(2) . . . . ? N4 N5 C9 C10 -173.6(3) . . . . ? Cu2 N5 C9 C10 3.9(5) . . . . ? N6 C8 C9 N5 -177.8(3) . . . . ? C7 C8 C9 N5 -1.6(4) . . . . ? N6 C8 C9 C10 -2.9(6) . . . . ? C7 C8 C9 C10 173.3(4) . . . . ? N8 N7 C12 C13 -1.3(4) . . . . ? Cu2 N7 C12 C13 -179.7(2) . . . . ? N8 N7 C12 C11 178.4(3) . . . . ? Cu2 N7 C12 C11 0.0(6) . . . . ? Cu4 O9 C16 O8 -172.1(3) . . . . ? Cu4 O9 C16 C17 9.4(8) . . . . ? Cu1 O8 C16 O9 -3.2(4) . . . . ? Cu1 O8 C16 C17 175.3(3) . . . . ? N7 C12 C13 C14 1.0(4) . . . . ? C11 C12 C13 C14 -178.6(4) . . . . ? N7 C12 C13 N9 178.1(3) . . . . ? C11 C12 C13 N9 -1.6(7) . . . . ? O6 N9 C13 C12 -179.2(4) . . . . ? O5 N9 C13 C12 0.0(6) . . . . ? O6 N9 C13 C14 -2.7(6) . . . . ? O5 N9 C13 C14 176.5(4) . . . . ? N7 N8 C14 C13 -0.4(4) . . . . ? Cu3 N8 C14 C13 173.9(2) . . . . ? N7 N8 C14 C15 -178.1(3) . . . . ? Cu3 N8 C14 C15 -3.8(5) . . . . ? C12 C13 C14 N8 -0.4(4) . . . . ? N9 C13 C14 N8 -177.4(3) . . . . ? C12 C13 C14 C15 177.1(4) . . . . ? N9 C13 C14 C15 0.1(6) . . . . ? Cu4 O10 C18 O11 -177.8(3) . . . . ? Cu2 O10 C18 O11 1.7(3) . . . . ? Cu4 O10 C18 C19 3.4(7) . . . . ? Cu2 O10 C18 C19 -177.1(4) . . . . ? Cu2 O11 C18 O10 -2.1(4) . . . . ? Cu2 O11 C18 C19 176.7(3) . . . . ? Cu4 O13 C20 O12 -174.7(3) . . . . ? Cu4 O13 C20 C21 5.3(7) . . . . ? Cu3 O12 C20 O13 -0.1(4) . . . . ? Cu3 O12 C20 C21 179.9(3) . . . . ? Cu1 O14 C23 C24 -106.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.669 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.072 #===END #========================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 774538' #TrackingRef '- JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H80 Cu7 N18 O32' _chemical_formula_sum 'C48 H80 Cu7 N18 O32' _chemical_formula_weight 1866.15 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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3 c' _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 18.778(3) _cell_length_b 18.778(3) _cell_length_c 35.187(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10745(3) _cell_formula_units_Z 6 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8902 _cell_measurement_theta_min 3.1533 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Block _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5718 _exptl_absorpt_coefficient_mu 2.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.585 _exptl_absorpt_correction_T_max 0.652 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 33533 _diffrn_reflns_av_R_equivalents 0.1012 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 25.34 _reflns_number_total 2188 _reflns_number_gt 1993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0478P)^2^+263.0658P] 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 2188 _refine_ls_number_parameters 190 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0944 _refine_ls_wR_factor_ref 0.1887 _refine_ls_wR_factor_gt 0.1839 _refine_ls_goodness_of_fit_ref 1.194 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 0.58845(6) 0.36973(6) 0.22789(3) 0.0421(3) Uani 1 1 d . . . Cu2 Cu 0.6667 0.3333 0.3333 0.0345(5) Uani 1 6 d S . . O1 O 0.2477(4) 0.1018(5) 0.2081(2) 0.082(2) Uani 1 1 d . . . O2 O 0.2786(5) 0.0056(5) 0.2034(3) 0.091(3) Uani 1 1 d . . . O3 O 0.5278(3) 0.4030(3) 0.26446(18) 0.0493(15) Uani 1 1 d . A . O4 O 0.6000(4) 0.3629(3) 0.29674(15) 0.0463(14) Uani 1 1 d . A . O5 O 0.6667 0.3333 0.2111(3) 0.041(2) Uani 1 3 d SD . . H5 H 0.6667 0.3333 0.1869(7) 0.061 Uiso 1 3 d SD . . N1 N 0.4960(4) 0.2550(4) 0.22534(18) 0.0390(15) Uani 1 1 d . A . N2 N 0.5155(4) 0.1931(4) 0.22109(19) 0.0458(17) Uani 1 1 d . . . N3 N 0.2985(5) 0.0786(6) 0.2089(2) 0.065(2) Uani 1 1 d . . . C1 C 0.3729(6) 0.2711(6) 0.2249(3) 0.061(3) Uani 1 1 d . A . H1A H 0.4140 0.3298 0.2236 0.091 Uiso 1 1 calc R . . H1B H 0.3429 0.2593 0.2490 0.091 Uiso 1 1 calc R . . H1C H 0.3342 0.2568 0.2037 0.091 Uiso 1 1 calc R . . C2 C 0.4150(5) 0.2213(5) 0.2224(2) 0.047(2) Uani 1 1 d . . . C3 C 0.3820(5) 0.1379(5) 0.2152(2) 0.051(2) Uani 1 1 d . A . C4 C 0.4473(6) 0.1222(5) 0.2143(2) 0.051(2) Uani 1 1 d . A . C5 C 0.4495(8) 0.0461(6) 0.2048(3) 0.081(4) Uani 1 1 d . . . H5A H 0.5049 0.0552 0.2095 0.122 Uiso 1 1 calc R A . H5B H 0.4353 0.0324 0.1780 0.122 Uiso 1 1 calc R . . H5C H 0.4099 0.0007 0.2207 0.122 Uiso 1 1 calc R . . C6 C 0.5493(5) 0.3879(5) 0.2959(3) 0.046(2) Uani 1 1 d . . . C7 C 0.5116(6) 0.3991(6) 0.3312(3) 0.063(3) Uani 1 1 d . A . H7A H 0.5453 0.4555 0.3405 0.095 Uiso 1 1 calc R . . H7B H 0.5086 0.3605 0.3508 0.095 Uiso 1 1 calc R . . H7C H 0.4560 0.3886 0.3256 0.095 Uiso 1 1 calc R . . O6 O 0.5679(18) 0.364(2) 0.1563(10) 0.091(10) Uani 0.54(6) 1 d PDU A 1 H6 H 0.590(10) 0.335(12) 0.162(6) 0.137 Uiso 0.54(6) 1 d PD A 1 C8 C 0.610(3) 0.420(3) 0.1288(14) 0.090(11) Uani 0.54(6) 1 d PDU A 1 H8A H 0.6565 0.4689 0.1402 0.136 Uiso 0.54(6) 1 calc PR A 1 H8B H 0.5739 0.4354 0.1158 0.136 Uiso 0.54(6) 1 calc PR A 1 H8C H 0.6316 0.3959 0.1104 0.136 Uiso 0.54(6) 1 calc PR A 1 O6A O 0.550(2) 0.387(3) 0.1653(11) 0.097(11) Uani 0.46(6) 1 d PDU A 2 H6A H 0.511(13) 0.344(10) 0.155(2) 0.145 Uiso 0.46(6) 1 d PD A 2 C8A C 0.591(4) 0.438(4) 0.1311(18) 0.103(13) Uani 0.46(6) 1 d PDU A 2 H8A1 H 0.6482 0.4795 0.1374 0.155 Uiso 0.46(6) 1 calc PR A 2 H8A2 H 0.5615 0.4659 0.1229 0.155 Uiso 0.46(6) 1 calc PR A 2 H8A3 H 0.5915 0.4032 0.1105 0.155 Uiso 0.46(6) 1 calc PR A 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 0.0368(6) 0.0402(6) 0.0503(6) -0.0017(4) -0.0029(4) 0.0200(5) Cu2 0.0336(8) 0.0336(8) 0.0361(12) 0.000 0.000 0.0168(4) O1 0.036(4) 0.086(6) 0.101(6) -0.002(4) -0.014(4) 0.013(4) O2 0.065(5) 0.052(5) 0.116(7) -0.016(4) -0.015(5) -0.002(4) O3 0.047(3) 0.045(3) 0.059(4) 0.002(3) 0.003(3) 0.025(3) O4 0.053(4) 0.041(3) 0.045(3) 0.001(2) 0.006(3) 0.023(3) O5 0.040(3) 0.040(3) 0.041(5) 0.000 0.000 0.0202(16) N1 0.036(4) 0.039(4) 0.041(4) -0.002(3) -0.003(3) 0.018(3) N2 0.043(4) 0.042(4) 0.046(4) -0.005(3) -0.005(3) 0.016(3) N3 0.040(5) 0.072(6) 0.055(5) 0.001(4) -0.007(4) 0.008(4) C1 0.043(5) 0.054(6) 0.083(7) -0.013(5) -0.004(5) 0.023(5) C2 0.039(5) 0.056(6) 0.036(4) 0.001(4) -0.003(4) 0.017(4) C3 0.044(5) 0.044(5) 0.048(5) -0.001(4) -0.014(4) 0.009(4) C4 0.055(6) 0.042(5) 0.044(5) -0.001(4) -0.008(4) 0.015(4) C5 0.093(9) 0.041(6) 0.099(9) -0.019(5) -0.037(7) 0.026(6) C6 0.048(5) 0.027(4) 0.058(6) -0.002(4) 0.011(4) 0.014(4) C7 0.067(7) 0.049(6) 0.067(6) 0.002(5) 0.018(5) 0.025(5) O6 0.071(12) 0.089(16) 0.063(12) 0.028(10) -0.027(9) 0.002(9) C8 0.068(15) 0.093(17) 0.065(11) 0.021(11) 0.003(11) 0.007(11) O6A 0.065(13) 0.100(18) 0.067(12) 0.019(11) -0.006(10) -0.003(11) C8A 0.074(16) 0.103(19) 0.066(12) 0.018(13) -0.008(13) -0.007(13) _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 N2 1.973(7) 3_665 ? Cu1 N1 1.981(7) . ? Cu1 O5 1.994(3) . ? Cu1 O3 2.014(6) . ? Cu1 O6A 2.39(4) . ? Cu2 O4 2.056(6) 32 ? Cu2 O4 2.056(6) 33_545 ? Cu2 O4 2.056(6) 2_655 ? Cu2 O4 2.056(6) 3_665 ? Cu2 O4 2.056(6) . ? Cu2 O4 2.056(6) 31_655 ? O1 N3 1.231(11) . ? O2 N3 1.243(11) . ? O3 C6 1.259(11) . ? O4 C6 1.254(10) . ? O5 Cu1 1.994(3) 3_665 ? O5 Cu1 1.994(3) 2_655 ? O5 H5 0.85(2) . ? N1 C2 1.328(10) . ? N1 N2 1.392(9) . ? N2 C4 1.329(11) . ? N2 Cu1 1.973(7) 2_655 ? N3 C3 1.414(11) . ? C1 C2 1.500(13) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.389(12) . ? C3 C4 1.398(13) . ? C4 C5 1.488(13) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.497(12) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? O6 C8 1.36(4) . ? O6 H6 0.8500(15) . ? O6 H6A 0.9(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O6A C8A 1.49(5) . ? O6A H6A 0.8500(11) . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? 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 N2 Cu1 N1 170.3(3) 3_665 . ? N2 Cu1 O5 88.3(2) 3_665 . ? N1 Cu1 O5 90.54(19) . . ? N2 Cu1 O3 92.3(3) 3_665 . ? N1 Cu1 O3 92.4(3) . . ? O5 Cu1 O3 157.4(3) . . ? N2 Cu1 O6A 83.6(9) 3_665 . ? N1 Cu1 O6A 86.9(9) . . ? O5 Cu1 O6A 95.4(15) . . ? O3 Cu1 O6A 107.1(15) . . ? O4 Cu2 O4 85.0(2) 32 33_545 ? O4 Cu2 O4 180.0(2) 32 2_655 ? O4 Cu2 O4 95.1(2) 33_545 2_655 ? O4 Cu2 O4 95.1(2) 32 3_665 ? O4 Cu2 O4 179.997(1) 33_545 3_665 ? O4 Cu2 O4 84.9(2) 2_655 3_665 ? O4 Cu2 O4 95.1(2) 32 . ? O4 Cu2 O4 95.1(2) 33_545 . ? O4 Cu2 O4 84.9(2) 2_655 . ? O4 Cu2 O4 84.9(2) 3_665 . ? O4 Cu2 O4 84.9(2) 32 31_655 ? O4 Cu2 O4 84.9(2) 33_545 31_655 ? O4 Cu2 O4 95.1(2) 2_655 31_655 ? O4 Cu2 O4 95.1(2) 3_665 31_655 ? O4 Cu2 O4 179.997(1) . 31_655 ? C6 O3 Cu1 101.3(5) . . ? C6 O4 Cu2 142.5(6) . . ? Cu1 O5 Cu1 111.6(2) 3_665 2_655 ? Cu1 O5 Cu1 111.6(2) 3_665 . ? Cu1 O5 Cu1 111.6(2) 2_655 . ? Cu1 O5 H5 107.2(3) 3_665 . ? Cu1 O5 H5 107.2(3) 2_655 . ? Cu1 O5 H5 107.2(3) . . ? C2 N1 N2 108.1(7) . . ? C2 N1 Cu1 134.0(6) . . ? N2 N1 Cu1 117.3(5) . . ? C4 N2 N1 109.3(7) . . ? C4 N2 Cu1 130.9(6) . 2_655 ? N1 N2 Cu1 119.7(5) . 2_655 ? O1 N3 O2 121.9(9) . . ? O1 N3 C3 118.3(9) . . ? O2 N3 C3 119.8(10) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.1(8) . . ? N1 C2 C1 122.2(8) . . ? C3 C2 C1 129.6(8) . . ? C2 C3 C4 107.4(8) . . ? C2 C3 N3 127.6(9) . . ? C4 C3 N3 125.0(9) . . ? N2 C4 C3 107.0(8) . . ? N2 C4 C5 121.7(9) . . ? C3 C4 C5 131.1(9) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O4 C6 O3 119.6(8) . . ? O4 C6 C7 122.3(9) . . ? O3 C6 C7 118.1(8) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C8 O6 H6 113(4) . . ? C8 O6 H6A 113(9) . . ? H6 O6 H6A 125(10) . . ? C8A O6A Cu1 138(2) . . ? C8A O6A H6A 102(4) . . ? Cu1 O6A H6A 116(10) . . ? O6A C8A H8A1 109.5 . . ? O6A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? O6A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.744 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.091 #===END #========================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 774539' #TrackingRef '- JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H62 Cu7 N20 O26, 4(C2 H3 N)' _chemical_formula_sum 'C54 H74 Cu7 N24 O26' _chemical_formula_weight 1920.22 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' _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 11.638(2) _cell_length_b 13.075(3) _cell_length_c 13.262(3) _cell_angle_alpha 100.86(3) _cell_angle_beta 93.47(3) _cell_angle_gamma 104.97(3) _cell_volume 1901.8(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7802 _cell_measurement_theta_min 3.1493 _cell_measurement_theta_max 27.5010 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 977 _exptl_absorpt_coefficient_mu 2.011 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3783 _exptl_absorpt_correction_T_max 0.8242 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Corp.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17561 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8590 _reflns_number_gt 5779 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0588P)^2^+1.9555P] 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 8590 _refine_ls_number_parameters 494 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Cu2 Cu 0.47316(5) -0.02781(5) 0.18930(5) 0.02891(17) Uani 1 1 d . . . Cu3 Cu 0.69598(5) -0.10550(5) 0.27344(5) 0.02896(17) Uani 1 1 d . . . Cu1 Cu 0.41858(5) -0.26580(5) 0.24862(5) 0.02873(17) Uani 1 1 d . . . Cu4 Cu 0.5000 0.0000 0.5000 0.0248(2) Uani 1 2 d S . . O1 O -0.0697(4) -0.3187(5) 0.0614(4) 0.0691(14) Uani 1 1 d . . . O2 O -0.0382(5) -0.1510(4) 0.0494(5) 0.0847(18) Uani 1 1 d . . . O3 O 0.8344(4) 0.3453(4) 0.1223(4) 0.0675(14) Uani 1 1 d . . . O4 O 0.9859(4) 0.2895(4) 0.1645(4) 0.0726(15) Uani 1 1 d . . . O5 O 0.8307(4) -0.4812(4) 0.3657(4) 0.0655(14) Uani 1 1 d . . . O6 O 0.6565(5) -0.5615(5) 0.3981(6) 0.092(2) Uani 1 1 d . . . O7 O 0.5351(3) -0.1551(3) 0.1918(3) 0.0289(8) Uani 1 1 d D . . O10 O 0.4203(3) 0.1057(3) 0.2384(3) 0.0330(8) Uani 1 1 d . . . O11 O 0.4848(3) 0.0483(3) 0.3693(3) 0.0297(8) Uani 1 1 d . . . O12 O 0.8325(3) -0.0459(3) 0.3863(3) 0.0390(9) Uani 1 1 d . . . O13 O 0.6629(3) -0.0410(3) 0.4462(3) 0.0338(8) Uani 1 1 d . . . O8 O 0.3115(3) -0.3143(3) 0.3539(3) 0.0310(8) Uani 1 1 d . . . O9 O 0.4088(3) -0.1462(3) 0.4156(3) 0.0331(8) Uani 1 1 d . . . N1 N 0.2870(4) -0.2259(3) 0.1771(3) 0.0309(10) Uani 1 1 d . . . N2 N 0.3109(4) -0.1232(3) 0.1549(3) 0.0297(9) Uani 1 1 d . . . N3 N -0.0028(5) -0.2263(5) 0.0709(5) 0.0570(15) Uani 1 1 d . . . N4 N 0.6348(4) 0.0572(4) 0.1762(3) 0.0334(10) Uani 1 1 d . . . N5 N 0.7316(4) 0.0237(4) 0.2129(3) 0.0309(10) Uani 1 1 d . . . N6 N 0.8770(5) 0.2768(4) 0.1512(4) 0.0511(13) Uani 1 1 d . . . N7 N 0.6708(4) -0.2534(3) 0.2969(3) 0.0307(10) Uani 1 1 d . . . N8 N 0.5540(4) -0.3142(3) 0.3016(3) 0.0279(9) Uani 1 1 d . . . N9 N 0.7245(5) -0.4867(4) 0.3709(4) 0.0509(14) Uani 1 1 d . . . N10 N 0.3825(5) -0.4249(4) 0.1016(4) 0.0485(13) Uani 1 1 d . . . N11 N 0.6302(5) -0.2507(5) 0.0172(4) 0.0533(14) Uani 1 1 d . . . N12 N 0.8357(7) -0.2974(7) 0.5942(6) 0.099(2) Uiso 1 1 d . . . C1 C 0.1176(5) -0.3909(5) 0.1558(5) 0.0434(14) Uani 1 1 d . . . H1A H 0.1785 -0.4187 0.1870 0.065 Uiso 1 1 calc R . . H1B H 0.0865 -0.4356 0.0867 0.065 Uiso 1 1 calc R . . H1C H 0.0520 -0.3935 0.1991 0.065 Uiso 1 1 calc R . . C2 C 0.1715(5) -0.2779(4) 0.1476(4) 0.0335(12) Uani 1 1 d . . . C3 C 0.1207(5) -0.2051(5) 0.1077(4) 0.0386(13) Uani 1 1 d . . . C4 C 0.2092(5) -0.1096(5) 0.1133(4) 0.0346(12) Uani 1 1 d . . . C5 C 0.2064(5) -0.0078(5) 0.0789(5) 0.0440(15) Uani 1 1 d . . . H5A H 0.2862 0.0438 0.0949 0.066 Uiso 1 1 calc R . . H5B H 0.1488 0.0240 0.1151 0.066 Uiso 1 1 calc R . . H5C H 0.1824 -0.0242 0.0042 0.066 Uiso 1 1 calc R . . C6 C 0.5939(5) 0.2053(5) 0.1022(5) 0.0475(16) Uani 1 1 d . . . H6A H 0.5108 0.1625 0.1003 0.071 Uiso 1 1 calc R . . H6B H 0.6119 0.2100 0.0317 0.071 Uiso 1 1 calc R . . H6C H 0.6050 0.2783 0.1437 0.071 Uiso 1 1 calc R . . C7 C 0.6773(5) 0.1512(4) 0.1499(4) 0.0359(13) Uani 1 1 d . . . C8 C 0.7995(5) 0.1801(4) 0.1680(4) 0.0368(13) Uani 1 1 d . . . C9 C 0.8319(5) 0.0966(4) 0.2062(4) 0.0351(12) Uani 1 1 d . . . C10 C 0.9520(5) 0.0821(5) 0.2333(5) 0.0474(15) Uani 1 1 d . . . H10A H 0.9422 0.0144 0.2576 0.071 Uiso 1 1 calc R . . H10B H 0.9975 0.1430 0.2880 0.071 Uiso 1 1 calc R . . H10C H 0.9952 0.0792 0.1721 0.071 Uiso 1 1 calc R . . C11 C 0.8786(5) -0.2647(5) 0.3212(5) 0.0444(15) Uani 1 1 d . . . H11A H 0.8958 -0.1947 0.3004 0.067 Uiso 1 1 calc R . . H11B H 0.9069 -0.3160 0.2719 0.067 Uiso 1 1 calc R . . H11C H 0.9197 -0.2554 0.3904 0.067 Uiso 1 1 calc R . . C12 C 0.7477(4) -0.3070(4) 0.3224(4) 0.0332(12) Uani 1 1 d . . . C13 C 0.6795(5) -0.4026(4) 0.3463(4) 0.0336(12) Uani 1 1 d . . . C14 C 0.5590(5) -0.4047(4) 0.3322(4) 0.0316(12) Uani 1 1 d . . . C15 C 0.4500(5) -0.4881(5) 0.3432(5) 0.0480(16) Uani 1 1 d . . . H15A H 0.3791 -0.4642 0.3273 0.072 Uiso 1 1 calc R . . H15B H 0.4530 -0.4991 0.4143 0.072 Uiso 1 1 calc R . . H15C H 0.4458 -0.5563 0.2954 0.072 Uiso 1 1 calc R . . C18 C 0.4431(4) 0.1176(4) 0.3349(4) 0.0305(11) Uani 1 1 d . . . C19 C 0.4240(5) 0.2144(4) 0.4061(5) 0.0413(14) Uani 1 1 d . . . H19A H 0.4234 0.2019 0.4767 0.062 Uiso 1 1 calc R . . H19B H 0.3473 0.2255 0.3834 0.062 Uiso 1 1 calc R . . H19C H 0.4890 0.2788 0.4046 0.062 Uiso 1 1 calc R . . C20 C 0.7731(5) -0.0268(4) 0.4618(5) 0.0377(13) Uani 1 1 d . . . C21 C 0.8373(6) 0.0083(6) 0.5692(5) 0.0533(17) Uani 1 1 d . . . H21A H 0.7974 0.0546 0.6125 0.080 Uiso 1 1 calc R . . H21B H 0.9204 0.0487 0.5672 0.080 Uiso 1 1 calc R . . H21C H 0.8361 -0.0557 0.5980 0.080 Uiso 1 1 calc R . . C16 C 0.3313(5) -0.2302(4) 0.4239(4) 0.0300(11) Uani 1 1 d . . . C17 C 0.2591(5) -0.2343(5) 0.5145(4) 0.0406(14) Uani 1 1 d . . . H17A H 0.2038 -0.3068 0.5058 0.061 Uiso 1 1 calc R . . H17B H 0.2134 -0.1807 0.5180 0.061 Uiso 1 1 calc R . . H17C H 0.3131 -0.2181 0.5785 0.061 Uiso 1 1 calc R . . C22 C 0.3590(5) -0.4636(5) 0.0173(5) 0.0376(13) Uani 1 1 d . . . C23 C 0.3286(6) -0.5118(5) -0.0922(5) 0.0464(15) Uani 1 1 d . . . H23A H 0.2712 -0.4792 -0.1220 0.070 Uiso 1 1 calc R . . H23B H 0.2928 -0.5900 -0.1015 0.070 Uiso 1 1 calc R . . H23C H 0.4012 -0.4985 -0.1271 0.070 Uiso 1 1 calc R . . C24 C 0.6823(5) -0.2676(5) -0.0499(5) 0.0398(13) Uani 1 1 d . . . C25 C 0.7473(6) -0.2878(5) -0.1376(5) 0.0479(15) Uani 1 1 d . . . H25A H 0.7157 -0.2617 -0.1951 0.072 Uiso 1 1 calc R . . H25B H 0.7380 -0.3657 -0.1588 0.072 Uiso 1 1 calc R . . H25C H 0.8324 -0.2495 -0.1185 0.072 Uiso 1 1 calc R . . C26 C 0.8685(7) -0.3713(6) 0.6062(6) 0.0648(19) Uiso 1 1 d . . . C27 C 0.9092(7) -0.4606(7) 0.6200(7) 0.077(2) Uiso 1 1 d . . . H27A H 0.8561 -0.5270 0.5763 0.116 Uiso 1 1 calc R . . H27B H 0.9093 -0.4664 0.6926 0.116 Uiso 1 1 calc R . . H27C H 0.9907 -0.4509 0.6006 0.116 Uiso 1 1 calc R . . H7 H 0.545(6) -0.179(5) 0.131(2) 0.06(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu2 0.0308(3) 0.0318(3) 0.0278(4) 0.0081(3) 0.0022(3) 0.0138(3) Cu3 0.0276(3) 0.0298(3) 0.0311(4) 0.0079(3) 0.0008(3) 0.0104(3) Cu1 0.0285(3) 0.0313(3) 0.0289(4) 0.0078(3) 0.0021(3) 0.0119(3) Cu4 0.0303(4) 0.0235(4) 0.0214(5) 0.0041(3) -0.0001(3) 0.0098(4) O1 0.043(3) 0.083(4) 0.078(4) 0.028(3) -0.006(2) 0.006(3) O2 0.061(3) 0.073(4) 0.117(5) 0.004(3) -0.033(3) 0.034(3) O3 0.068(3) 0.050(3) 0.101(4) 0.041(3) 0.023(3) 0.023(3) O4 0.042(3) 0.080(4) 0.104(4) 0.047(3) 0.014(3) 0.009(3) O5 0.055(3) 0.068(3) 0.090(4) 0.029(3) 0.008(3) 0.038(3) O6 0.063(3) 0.071(4) 0.167(6) 0.073(4) 0.012(4) 0.028(3) O7 0.0298(19) 0.0298(19) 0.027(2) 0.0037(16) -0.0007(16) 0.0107(16) O10 0.040(2) 0.033(2) 0.032(2) 0.0082(16) 0.0026(16) 0.0192(17) O11 0.040(2) 0.0264(18) 0.027(2) 0.0082(15) 0.0022(16) 0.0154(16) O12 0.034(2) 0.045(2) 0.038(2) 0.0077(18) -0.0026(17) 0.0120(18) O13 0.036(2) 0.034(2) 0.033(2) 0.0035(16) 0.0034(16) 0.0136(17) O8 0.0329(19) 0.0300(19) 0.031(2) 0.0067(16) 0.0038(16) 0.0095(16) O9 0.039(2) 0.031(2) 0.030(2) 0.0058(16) 0.0050(16) 0.0110(17) N1 0.034(2) 0.032(2) 0.030(2) 0.0053(19) 0.0011(19) 0.015(2) N2 0.031(2) 0.033(2) 0.027(2) 0.0036(19) -0.0021(18) 0.014(2) N3 0.047(3) 0.064(4) 0.059(4) 0.007(3) -0.012(3) 0.021(3) N4 0.031(2) 0.039(3) 0.035(3) 0.014(2) 0.0035(19) 0.015(2) N5 0.024(2) 0.036(2) 0.034(3) 0.011(2) 0.0026(18) 0.0098(19) N6 0.051(3) 0.049(3) 0.057(4) 0.019(3) 0.013(3) 0.013(3) N7 0.030(2) 0.033(2) 0.031(3) 0.0062(19) 0.0002(19) 0.013(2) N8 0.028(2) 0.026(2) 0.030(2) 0.0051(18) -0.0002(18) 0.0083(18) N9 0.057(3) 0.051(3) 0.057(4) 0.022(3) 0.002(3) 0.028(3) N10 0.049(3) 0.048(3) 0.045(3) -0.003(3) 0.001(3) 0.016(3) N11 0.057(3) 0.069(4) 0.046(3) 0.021(3) 0.013(3) 0.031(3) C1 0.035(3) 0.045(4) 0.044(4) 0.008(3) -0.006(3) 0.003(3) C2 0.028(3) 0.038(3) 0.031(3) 0.002(2) 0.001(2) 0.009(2) C3 0.029(3) 0.050(4) 0.034(3) -0.002(3) -0.007(2) 0.017(3) C4 0.037(3) 0.044(3) 0.028(3) 0.003(2) -0.001(2) 0.024(3) C5 0.049(3) 0.040(3) 0.046(4) 0.008(3) -0.011(3) 0.021(3) C6 0.052(4) 0.053(4) 0.050(4) 0.031(3) 0.009(3) 0.022(3) C7 0.045(3) 0.036(3) 0.032(3) 0.012(2) 0.009(3) 0.016(3) C8 0.037(3) 0.034(3) 0.041(3) 0.014(3) 0.014(3) 0.006(3) C9 0.031(3) 0.040(3) 0.037(3) 0.009(3) 0.008(2) 0.011(3) C10 0.039(3) 0.050(4) 0.060(4) 0.021(3) 0.013(3) 0.015(3) C11 0.041(3) 0.053(4) 0.048(4) 0.014(3) 0.004(3) 0.027(3) C12 0.030(3) 0.037(3) 0.034(3) 0.004(2) 0.000(2) 0.014(2) C13 0.038(3) 0.033(3) 0.035(3) 0.010(2) 0.002(2) 0.018(3) C14 0.042(3) 0.025(3) 0.026(3) 0.003(2) -0.002(2) 0.010(2) C15 0.045(3) 0.034(3) 0.067(5) 0.021(3) 0.002(3) 0.010(3) C18 0.030(3) 0.033(3) 0.029(3) 0.009(2) 0.003(2) 0.009(2) C19 0.054(4) 0.031(3) 0.043(4) 0.006(3) 0.007(3) 0.019(3) C20 0.042(3) 0.025(3) 0.045(4) 0.009(3) -0.002(3) 0.007(3) C21 0.051(4) 0.063(4) 0.039(4) 0.007(3) -0.009(3) 0.010(3) C16 0.036(3) 0.030(3) 0.028(3) 0.009(2) -0.002(2) 0.014(2) C17 0.050(3) 0.039(3) 0.036(3) 0.010(3) 0.013(3) 0.014(3) C22 0.039(3) 0.035(3) 0.040(4) 0.006(3) 0.006(3) 0.014(3) C23 0.061(4) 0.041(3) 0.036(4) 0.000(3) 0.000(3) 0.019(3) C24 0.038(3) 0.043(3) 0.042(4) 0.013(3) 0.003(3) 0.016(3) C25 0.050(4) 0.055(4) 0.039(4) 0.006(3) 0.009(3) 0.019(3) _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 Cu2 N2 1.948(4) . ? Cu2 N4 1.959(4) . ? Cu2 O7 1.982(3) . ? Cu2 O10 2.006(3) . ? Cu2 O11 2.387(4) . ? Cu2 C18 2.552(5) . ? Cu3 N5 1.965(4) . ? Cu3 N7 1.966(4) . ? Cu3 O7 1.990(4) . ? Cu3 O12 2.001(4) . ? Cu3 O13 2.378(4) . ? Cu3 C20 2.527(6) . ? Cu1 N8 1.982(4) . ? Cu1 N1 1.985(4) . ? Cu1 O7 2.006(4) . ? Cu1 O8 2.011(3) . ? Cu4 O11 1.967(3) 2_656 ? Cu4 O11 1.967(3) . ? Cu4 O9 2.009(4) 2_656 ? Cu4 O9 2.009(4) . ? Cu4 O13 2.222(3) . ? Cu4 O13 2.222(3) 2_656 ? O1 N3 1.235(7) . ? O2 N3 1.233(7) . ? O3 N6 1.236(6) . ? O4 N6 1.233(6) . ? O5 N9 1.226(6) . ? O6 N9 1.216(7) . ? O7 H7 0.84(2) . ? O10 C18 1.263(6) . ? O11 C18 1.274(6) . ? O12 C20 1.274(7) . ? O13 C20 1.246(6) . ? O8 C16 1.259(6) . ? O9 C16 1.256(6) . ? N1 C2 1.337(7) . ? N1 N2 1.389(6) . ? N2 C4 1.344(6) . ? N3 C3 1.429(7) . ? N4 C7 1.321(7) . ? N4 N5 1.402(5) . ? N5 C9 1.323(6) . ? N6 C8 1.415(7) . ? N7 C12 1.335(6) . ? N7 N8 1.399(6) . ? N8 C14 1.334(6) . ? N9 C13 1.414(7) . ? N10 C22 1.123(7) . ? N11 C24 1.127(7) . ? N12 C26 1.160(9) . ? C1 C2 1.476(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.407(7) . ? C3 C4 1.384(8) . ? C4 C5 1.494(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.513(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.368(8) . ? C8 C9 1.409(7) . ? C9 C10 1.490(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.483(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.401(7) . ? C13 C14 1.397(7) . ? C14 C15 1.479(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C18 C19 1.503(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.498(8) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C16 C17 1.508(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C22 C23 1.452(9) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.445(8) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.407(10) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 N2 Cu2 N4 161.78(19) . . ? N2 Cu2 O7 89.85(16) . . ? N4 Cu2 O7 89.36(16) . . ? N2 Cu2 O10 94.40(16) . . ? N4 Cu2 O10 92.35(17) . . ? O7 Cu2 O10 160.62(15) . . ? N2 Cu2 O11 104.12(15) . . ? N4 Cu2 O11 93.86(16) . . ? O7 Cu2 O11 101.81(13) . . ? O10 Cu2 O11 58.81(13) . . ? N2 Cu2 C18 101.01(17) . . ? N4 Cu2 C18 93.10(18) . . ? O7 Cu2 C18 131.46(16) . . ? O10 Cu2 C18 29.17(14) . . ? O11 Cu2 C18 29.65(13) . . ? N5 Cu3 N7 164.15(18) . . ? N5 Cu3 O7 89.01(16) . . ? N7 Cu3 O7 87.93(16) . . ? N5 Cu3 O12 94.70(17) . . ? N7 Cu3 O12 92.31(17) . . ? O7 Cu3 O12 164.73(15) . . ? N5 Cu3 O13 104.58(16) . . ? N7 Cu3 O13 91.22(16) . . ? O7 Cu3 O13 105.66(14) . . ? O12 Cu3 O13 59.07(14) . . ? N5 Cu3 C20 102.27(18) . . ? N7 Cu3 C20 90.84(18) . . ? O7 Cu3 C20 134.85(17) . . ? O12 Cu3 C20 29.89(16) . . ? O13 Cu3 C20 29.22(15) . . ? N8 Cu1 N1 172.46(18) . . ? N8 Cu1 O7 89.20(15) . . ? N1 Cu1 O7 88.20(16) . . ? N8 Cu1 O8 95.13(15) . . ? N1 Cu1 O8 90.32(16) . . ? O7 Cu1 O8 153.72(15) . . ? O11 Cu4 O11 180.000(1) 2_656 . ? O11 Cu4 O9 84.29(14) 2_656 2_656 ? O11 Cu4 O9 95.71(14) . 2_656 ? O11 Cu4 O9 95.71(14) 2_656 . ? O11 Cu4 O9 84.29(14) . . ? O9 Cu4 O9 180.00(15) 2_656 . ? O11 Cu4 O13 94.34(13) 2_656 . ? O11 Cu4 O13 85.66(13) . . ? O9 Cu4 O13 94.01(14) 2_656 . ? O9 Cu4 O13 85.99(14) . . ? O11 Cu4 O13 85.66(13) 2_656 2_656 ? O11 Cu4 O13 94.34(13) . 2_656 ? O9 Cu4 O13 85.99(14) 2_656 2_656 ? O9 Cu4 O13 94.01(14) . 2_656 ? O13 Cu4 O13 180.000(1) . 2_656 ? Cu2 O7 Cu3 108.85(17) . . ? Cu2 O7 Cu1 109.97(16) . . ? Cu3 O7 Cu1 112.50(17) . . ? Cu2 O7 H7 107(4) . . ? Cu3 O7 H7 107(4) . . ? Cu1 O7 H7 112(5) . . ? C18 O10 Cu2 100.1(3) . . ? C18 O11 Cu4 138.0(3) . . ? C18 O11 Cu2 82.4(3) . . ? Cu4 O11 Cu2 136.92(16) . . ? C20 O12 Cu3 98.6(3) . . ? C20 O13 Cu4 148.1(4) . . ? C20 O13 Cu3 82.0(3) . . ? Cu4 O13 Cu3 127.50(16) . . ? C16 O8 Cu1 103.1(3) . . ? C16 O9 Cu4 140.3(3) . . ? C2 N1 N2 109.3(4) . . ? C2 N1 Cu1 132.4(4) . . ? N2 N1 Cu1 118.2(3) . . ? C4 N2 N1 109.0(4) . . ? C4 N2 Cu2 132.3(4) . . ? N1 N2 Cu2 118.7(3) . . ? O1 N3 O2 122.7(6) . . ? O1 N3 C3 119.1(5) . . ? O2 N3 C3 118.2(6) . . ? C7 N4 N5 108.4(4) . . ? C7 N4 Cu2 133.4(4) . . ? N5 N4 Cu2 117.7(3) . . ? C9 N5 N4 108.4(4) . . ? C9 N5 Cu3 133.4(3) . . ? N4 N5 Cu3 117.9(3) . . ? O4 N6 O3 121.8(5) . . ? O4 N6 C8 118.5(5) . . ? O3 N6 C8 119.7(5) . . ? C12 N7 N8 109.3(4) . . ? C12 N7 Cu3 131.7(4) . . ? N8 N7 Cu3 118.5(3) . . ? C14 N8 N7 108.5(4) . . ? C14 N8 Cu1 132.3(4) . . ? N7 N8 Cu1 118.6(3) . . ? O6 N9 O5 122.2(5) . . ? O6 N9 C13 118.6(5) . . ? O5 N9 C13 119.2(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 106.2(5) . . ? N1 C2 C1 123.3(5) . . ? C3 C2 C1 130.5(5) . . ? C4 C3 C2 108.7(5) . . ? C4 C3 N3 126.2(5) . . ? C2 C3 N3 125.0(6) . . ? N2 C4 C3 106.7(5) . . ? N2 C4 C5 121.7(5) . . ? C3 C4 C5 131.5(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 C8 108.6(5) . . ? N4 C7 C6 120.6(5) . . ? C8 C7 C6 130.7(5) . . ? C7 C8 C9 107.3(5) . . ? C7 C8 N6 125.3(5) . . ? C9 C8 N6 127.4(5) . . ? N5 C9 C8 107.2(4) . . ? N5 C9 C10 122.0(5) . . ? C8 C9 C10 130.7(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N7 C12 C13 106.8(4) . . ? N7 C12 C11 122.0(5) . . ? C13 C12 C11 131.2(5) . . ? C14 C13 C12 108.0(4) . . ? C14 C13 N9 126.1(5) . . ? C12 C13 N9 125.6(5) . . ? N8 C14 C13 107.4(5) . . ? N8 C14 C15 122.2(5) . . ? C13 C14 C15 130.3(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O10 C18 O11 118.7(5) . . ? O10 C18 C19 119.6(4) . . ? O11 C18 C19 121.7(5) . . ? O10 C18 Cu2 50.7(2) . . ? O11 C18 Cu2 68.0(3) . . ? C19 C18 Cu2 169.9(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O13 C20 O12 120.1(5) . . ? O13 C20 C21 121.0(5) . . ? O12 C20 C21 118.8(5) . . ? O13 C20 Cu3 68.7(3) . . ? O12 C20 Cu3 51.5(3) . . ? C21 C20 Cu3 168.7(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O8 C16 O9 119.3(5) . . ? O8 C16 C17 118.2(5) . . ? O9 C16 C17 122.6(5) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N10 C22 C23 178.9(6) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N11 C24 C25 178.4(7) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N12 C26 C27 179.4(9) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? 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 O7 H7 N11 0.84(2) 2.06(3) 2.843(7) 155(6) . _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.796 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.146 #===END #========================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 774540' #TrackingRef '- JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H68 Cu7 N20 O28, C5 H6 O, 2(C Cl3 H)' _chemical_formula_sum 'C55 H76 Cl6 Cu7 N20 O29' _chemical_formula_weight 2136.89 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' Cl Cl 0.1484 0.1585 '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 13.717(7) _cell_length_b 14.320(9) _cell_length_c 14.657(3) _cell_angle_alpha 62.48(6) _cell_angle_beta 62.25(6) _cell_angle_gamma 80.88(8) _cell_volume 2253.6(19) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7731 _cell_measurement_theta_min 3.0182 _cell_measurement_theta_max 27.4662 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1086 _exptl_absorpt_coefficient_mu 1.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5354 _exptl_absorpt_correction_T_max 0.7050 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Corp.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17662 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.1558 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.36 _reflns_number_total 9773 _reflns_number_gt 6016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1327P)^2^+5.0518P] 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 9773 _refine_ls_number_parameters 526 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1939 _refine_ls_R_factor_gt 0.1357 _refine_ls_wR_factor_ref 0.3702 _refine_ls_wR_factor_gt 0.3239 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.193 _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 Cl1 Cl 1.1038(6) 0.1986(6) 0.8848(7) 0.161(3) Uiso 1 1 d . . . Cu1 Cu 0.25091(12) 0.79784(11) 0.54207(12) 0.0436(4) Uani 1 1 d . . . Cu2 Cu 0.25051(12) 0.87293(12) 0.28987(12) 0.0447(4) Uani 1 1 d . . . Cu3 Cu 0.33567(12) 1.04342(11) 0.33172(12) 0.0430(4) Uani 1 1 d . . . Cu4 Cu 0.0000 1.0000 0.5000 0.0439(5) Uani 1 2 d S . . O1 O 0.0771(10) 0.3876(8) 0.6510(10) 0.086(4) Uani 1 1 d . . . O2 O 0.1132(13) 0.4285(10) 0.4789(11) 0.111(5) Uani 1 1 d . . . O3 O 0.4317(8) 0.9388(8) 0.7570(8) 0.066(3) Uani 1 1 d . . . O4 O 0.4214(9) 1.1058(9) 0.6609(9) 0.073(3) Uani 1 1 d . . . O5 O 0.4661(10) 1.1775(9) -0.1997(8) 0.082(3) Uani 1 1 d . . . O6 O 0.5399(12) 1.2776(12) -0.1724(9) 0.116(5) Uani 1 1 d . . . O7 O 0.3320(6) 0.8907(6) 0.3669(6) 0.0402(17) Uani 1 1 d . . . O8 O 0.1252(7) 0.7595(7) 0.7033(7) 0.050(2) Uani 1 1 d . . . O9 O 0.0777(7) 0.8988(6) 0.5841(7) 0.050(2) Uani 1 1 d . . . O10 O 0.1343(7) 0.8705(7) 0.2435(7) 0.051(2) Uani 1 1 d . . . O11 O 0.0670(7) 0.9147(7) 0.3863(7) 0.055(2) Uani 1 1 d . . . O12 O 0.2913(7) 1.1910(6) 0.3077(7) 0.0460(19) Uani 1 1 d . . . O13 O 0.1437(7) 1.0827(6) 0.3985(7) 0.051(2) Uani 1 1 d . . . O14 O 0.3826(7) 0.6763(7) 0.5737(8) 0.059(2) Uani 1 1 d . . . N1 N 0.1959(9) 0.6970(8) 0.5158(9) 0.052(3) Uani 1 1 d . . . N2 N 0.2159(8) 0.7253(7) 0.4022(8) 0.043(2) Uani 1 1 d . . . N3 N 0.1122(10) 0.4521(9) 0.5489(11) 0.060(3) Uani 1 1 d . . . N4 N 0.3293(7) 1.0057(7) 0.1544(8) 0.039(2) Uani 1 1 d . . . N5 N 0.3701(8) 1.0751(8) 0.1725(8) 0.046(2) Uani 1 1 d . . . N6 N 0.4800(9) 1.2035(11) -0.1350(11) 0.065(3) Uani 1 1 d . . . N7 N 0.3392(7) 1.0046(8) 0.4786(8) 0.040(2) Uani 1 1 d . . . N8 N 0.3149(8) 0.8985(7) 0.5609(7) 0.038(2) Uani 1 1 d . . . N9 N 0.4053(10) 1.0107(11) 0.6851(10) 0.063(3) Uani 1 1 d . . . N10 N 0.5477(9) 0.6150(10) 0.4946(10) 0.062(3) Uani 1 1 d . . . C28 C 0.253(5) 0.468(4) -0.038(5) 0.142(19) Uiso 0.50 1 d PD . . C1 C 0.1866(11) 0.6384(10) 0.4021(11) 0.051(3) Uani 1 1 d . . . C2 C 0.2000(13) 0.6405(12) 0.2918(12) 0.069(4) Uani 1 1 d . . . H2A H 0.1278 0.6352 0.2971 0.104 Uiso 1 1 calc R . . H2B H 0.2410 0.5816 0.2814 0.104 Uiso 1 1 calc R . . H2C H 0.2398 0.7062 0.2267 0.104 Uiso 1 1 calc R . . C3 C 0.1511(10) 0.5561(10) 0.5122(11) 0.052(3) Uani 1 1 d . . . C4 C 0.1559(11) 0.5960(11) 0.5814(12) 0.056(3) Uani 1 1 d . . . C5 C 0.1236(13) 0.5421(10) 0.7097(10) 0.065(4) Uani 1 1 d . . . H5A H 0.1565 0.5830 0.7271 0.097 Uiso 1 1 calc R . . H5B H 0.1498 0.4718 0.7308 0.097 Uiso 1 1 calc R . . H5C H 0.0438 0.5373 0.7529 0.097 Uiso 1 1 calc R . . C6 C 0.4313(11) 1.1561(10) 0.0719(10) 0.051(3) Uani 1 1 d . . . C7 C 0.4895(11) 1.2421(10) 0.0597(10) 0.055(3) Uani 1 1 d . . . H7A H 0.4816 1.2278 0.1344 0.082 Uiso 1 1 calc R . . H7B H 0.4581 1.3082 0.0293 0.082 Uiso 1 1 calc R . . H7C H 0.5672 1.2469 0.0075 0.082 Uiso 1 1 calc R . . C8 C 0.4235(10) 1.1360(10) -0.0113(10) 0.053(3) Uani 1 1 d . . . C9 C 0.3607(10) 1.0452(10) 0.0425(9) 0.046(3) Uani 1 1 d . . . C10 C 0.3278(12) 0.9865(11) -0.0036(10) 0.062(4) Uani 1 1 d . . . H10A H 0.3228 0.9111 0.0443 0.092 Uiso 1 1 calc R . . H10B H 0.3829 1.0032 -0.0819 0.092 Uiso 1 1 calc R . . H10C H 0.2567 1.0076 -0.0027 0.092 Uiso 1 1 calc R . . C11 C 0.3331(9) 0.8889(10) 0.6484(10) 0.041(3) Uani 1 1 d . . . C12 C 0.3148(12) 0.7847(11) 0.7514(10) 0.061(4) Uani 1 1 d . . . H12A H 0.2473 0.7838 0.8168 0.092 Uiso 1 1 calc R . . H12B H 0.3766 0.7746 0.7691 0.092 Uiso 1 1 calc R . . H12C H 0.3084 0.7283 0.7349 0.092 Uiso 1 1 calc R . . C13 C 0.3681(9) 0.9874(11) 0.6235(10) 0.045(3) Uani 1 1 d . . . C14 C 0.3681(9) 1.0622(11) 0.5159(10) 0.045(3) Uani 1 1 d . . . C15 C 0.3969(11) 1.1788(10) 0.4506(11) 0.057(3) Uani 1 1 d . . . H15A H 0.4263 1.2002 0.3689 0.085 Uiso 1 1 calc R . . H15B H 0.4520 1.1962 0.4653 0.085 Uiso 1 1 calc R . . H15C H 0.3312 1.2155 0.4752 0.085 Uiso 1 1 calc R . . C16 C 0.0575(11) 0.8280(11) 0.6848(12) 0.056(3) Uani 1 1 d . . . C17 C -0.0457(12) 0.8276(11) 0.7937(11) 0.067(4) Uani 1 1 d . . . H17A H -0.0856 0.7587 0.8402 0.100 Uiso 1 1 calc R . . H17B H -0.0935 0.8808 0.7700 0.100 Uiso 1 1 calc R . . H17C H -0.0219 0.8431 0.8384 0.100 Uiso 1 1 calc R . . C18 C 0.0573(12) 0.8939(10) 0.3154(11) 0.054(3) Uani 1 1 d . . . C19 C -0.0615(11) 0.8931(13) 0.3251(13) 0.066(4) Uani 1 1 d . . . H19A H -0.0616 0.9449 0.2532 0.099 Uiso 1 1 calc R . . H19B H -0.1137 0.9103 0.3869 0.099 Uiso 1 1 calc R . . H19C H -0.0825 0.8235 0.3412 0.099 Uiso 1 1 calc R . . C20 C 0.1858(11) 1.1751(9) 0.3562(9) 0.043(3) Uani 1 1 d . . . C21 C 0.1145(13) 1.2659(11) 0.3648(13) 0.067(4) Uani 1 1 d . . . H21A H 0.1542 1.3172 0.3635 0.101 Uiso 1 1 calc R . . H21B H 0.0468 1.2394 0.4361 0.101 Uiso 1 1 calc R . . H21C H 0.0969 1.2993 0.3002 0.101 Uiso 1 1 calc R . . C22 C 0.4608(11) 0.6683(10) 0.4918(13) 0.055(3) Uani 1 1 d . . . H22 H 0.4586 0.7032 0.4205 0.066 Uiso 1 1 calc R . . C23 C 0.5548(13) 0.5513(13) 0.6044(15) 0.080(5) Uani 1 1 d . . . H23A H 0.6119 0.5835 0.6044 0.120 Uiso 1 1 calc R . . H23B H 0.5728 0.4804 0.6126 0.120 Uiso 1 1 calc R . . H23C H 0.4844 0.5481 0.6680 0.120 Uiso 1 1 calc R . . C24 C 0.6405(12) 0.6160(12) 0.3905(13) 0.078(5) Uani 1 1 d . . . H24A H 0.6248 0.6579 0.3253 0.117 Uiso 1 1 calc R . . H24B H 0.6517 0.5443 0.3992 0.117 Uiso 1 1 calc R . . H24C H 0.7066 0.6464 0.3779 0.117 Uiso 1 1 calc R . . C25 C 0.9717(17) 0.2158(13) 0.9020(13) 0.114(7) Uiso 1 1 d D . . Cl2 Cl 0.8904(10) 0.3110(9) 0.9313(10) 0.105(3) Uiso 0.50 1 d P . . Cl2A Cl 0.9429(16) 0.3151(16) 0.9537(17) 0.192(8) Uiso 0.50 1 d P . . Cl3 Cl 0.8906(6) 0.0894(6) 1.0452(7) 0.159(3) Uiso 1 1 d D . . C29 C 0.314(3) 0.505(3) 0.091(3) 0.075(9) Uiso 0.50 1 d PD A 1 O15 O 0.304(2) 0.463(2) 0.029(3) 0.120(10) Uiso 0.50 1 d PD A 1 C27 C 0.266(2) 0.386(2) -0.080(3) 0.065(7) Uiso 0.50 1 d PD A 1 C30 C 0.389(3) 0.464(3) 0.149(3) 0.108(13) Uiso 0.50 1 d PD . . C27A C 0.115(4) 0.481(5) -0.011(5) 0.063(14) Uiso 0.25 1 d PD A . C28A C 0.204(3) 0.475(4) 0.026(5) 0.056(13) Uiso 0.25 1 d PD . . 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 0.0515(9) 0.0442(8) 0.0435(8) -0.0187(7) -0.0289(7) 0.0056(6) Cu2 0.0518(9) 0.0491(9) 0.0439(8) -0.0223(7) -0.0285(7) 0.0052(7) Cu3 0.0518(9) 0.0452(8) 0.0434(8) -0.0186(7) -0.0312(7) 0.0049(6) Cu4 0.0435(12) 0.0494(12) 0.0471(11) -0.0235(10) -0.0265(10) 0.0094(9) O1 0.115(10) 0.055(7) 0.082(8) -0.009(6) -0.052(7) -0.021(6) O2 0.188(14) 0.083(9) 0.101(9) -0.059(8) -0.073(10) 0.002(9) O3 0.091(7) 0.069(6) 0.063(6) -0.026(5) -0.056(6) 0.000(5) O4 0.093(8) 0.084(8) 0.078(7) -0.051(7) -0.050(6) 0.007(6) O5 0.103(9) 0.090(8) 0.050(6) -0.028(6) -0.029(6) -0.011(7) O6 0.133(12) 0.144(12) 0.048(6) -0.020(7) -0.022(7) -0.074(10) O7 0.039(4) 0.047(5) 0.043(4) -0.024(4) -0.022(4) 0.004(3) O8 0.063(6) 0.051(5) 0.044(5) -0.022(4) -0.031(4) 0.012(4) O9 0.070(6) 0.047(5) 0.047(5) -0.022(4) -0.038(5) 0.016(4) O10 0.057(6) 0.063(6) 0.051(5) -0.031(5) -0.034(5) 0.008(4) O11 0.063(6) 0.061(6) 0.059(5) -0.031(5) -0.037(5) 0.005(4) O12 0.050(5) 0.043(5) 0.054(5) -0.022(4) -0.030(4) 0.002(4) O13 0.050(5) 0.040(5) 0.051(5) -0.012(4) -0.020(4) -0.005(4) O14 0.046(6) 0.064(6) 0.067(6) -0.029(5) -0.026(5) 0.005(4) N1 0.080(8) 0.047(6) 0.049(6) -0.027(5) -0.041(6) 0.011(5) N2 0.055(6) 0.037(5) 0.043(5) -0.019(4) -0.027(5) 0.007(4) N3 0.059(7) 0.056(7) 0.076(8) -0.024(7) -0.042(7) 0.002(6) N4 0.039(5) 0.045(5) 0.041(5) -0.017(4) -0.024(4) 0.000(4) N5 0.049(6) 0.064(7) 0.039(5) -0.032(5) -0.025(5) 0.014(5) N6 0.041(7) 0.085(10) 0.063(8) -0.036(7) -0.019(6) 0.012(6) N7 0.038(5) 0.053(6) 0.035(5) -0.020(4) -0.019(4) 0.005(4) N8 0.044(5) 0.045(5) 0.029(4) -0.016(4) -0.021(4) 0.008(4) N9 0.063(8) 0.092(10) 0.056(7) -0.041(7) -0.038(6) 0.014(7) N10 0.049(7) 0.073(8) 0.068(8) -0.036(7) -0.026(6) 0.015(6) C1 0.063(8) 0.041(7) 0.061(8) -0.020(6) -0.041(7) 0.011(6) C2 0.097(12) 0.068(10) 0.058(8) -0.032(8) -0.038(8) -0.009(8) C3 0.044(7) 0.046(7) 0.056(8) -0.015(6) -0.023(6) 0.003(5) C4 0.058(8) 0.056(8) 0.067(9) -0.029(7) -0.039(7) 0.013(6) C5 0.098(12) 0.036(7) 0.045(7) -0.007(6) -0.030(8) -0.002(7) C6 0.056(8) 0.056(8) 0.041(6) -0.014(6) -0.027(6) -0.002(6) C7 0.062(9) 0.052(8) 0.032(6) -0.007(5) -0.013(6) -0.015(6) C8 0.049(8) 0.057(8) 0.043(7) -0.008(6) -0.026(6) -0.001(6) C9 0.057(8) 0.053(7) 0.032(5) -0.020(5) -0.023(6) 0.007(6) C10 0.098(11) 0.058(8) 0.047(7) -0.026(7) -0.044(8) 0.007(8) C11 0.029(6) 0.051(7) 0.043(6) -0.021(5) -0.019(5) 0.012(5) C12 0.084(10) 0.069(9) 0.041(7) -0.026(7) -0.032(7) 0.000(8) C13 0.038(7) 0.069(8) 0.044(6) -0.033(6) -0.025(6) 0.014(6) C14 0.030(6) 0.067(8) 0.052(7) -0.031(6) -0.027(6) 0.019(5) C15 0.062(9) 0.050(8) 0.046(7) -0.014(6) -0.016(6) -0.017(6) C16 0.066(9) 0.061(9) 0.062(8) -0.030(7) -0.042(7) 0.001(7) C17 0.075(11) 0.055(9) 0.053(8) -0.023(7) -0.020(8) 0.014(7) C18 0.071(9) 0.043(7) 0.050(7) -0.022(6) -0.027(7) 0.004(6) C19 0.049(8) 0.102(12) 0.080(10) -0.062(10) -0.037(8) 0.018(8) C20 0.062(8) 0.043(7) 0.035(6) -0.021(5) -0.027(6) 0.007(6) C21 0.089(11) 0.051(8) 0.082(10) -0.037(8) -0.053(9) 0.025(8) C22 0.051(8) 0.051(8) 0.073(9) -0.030(7) -0.035(8) 0.012(6) C23 0.075(11) 0.082(12) 0.098(13) -0.048(11) -0.049(10) 0.027(9) C24 0.057(10) 0.066(10) 0.080(11) -0.023(9) -0.021(9) 0.021(7) _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 Cl1 C25 1.70(2) . ? Cu1 N8 1.980(9) . ? Cu1 N1 1.984(10) . ? Cu1 O8 2.041(9) . ? Cu1 O7 2.062(8) . ? Cu1 O14 2.355(9) . ? Cu2 N2 1.944(10) . ? Cu2 N4 1.972(10) . ? Cu2 O10 2.014(8) . ? Cu2 O7 2.029(7) . ? Cu2 O11 2.384(9) . ? Cu2 C18 2.486(15) . ? Cu3 N7 1.982(9) . ? Cu3 N5 1.985(9) . ? Cu3 O7 2.005(8) . ? Cu3 O12 2.016(8) . ? Cu3 O13 2.418(9) . ? Cu4 O9 1.959(8) 2_576 ? Cu4 O9 1.959(8) . ? Cu4 O13 1.971(8) 2_576 ? Cu4 O13 1.971(8) . ? Cu4 O11 2.284(8) . ? Cu4 O11 2.284(8) 2_576 ? O1 N3 1.232(15) . ? O2 N3 1.213(14) . ? O3 N9 1.240(14) . ? O4 N9 1.267(15) . ? O5 N6 1.261(14) . ? O6 N6 1.193(15) . ? O8 C16 1.264(15) . ? O9 C16 1.269(15) . ? O10 C18 1.232(15) . ? O11 C18 1.270(14) . ? O12 C20 1.284(14) . ? O13 C20 1.272(13) . ? O14 C22 1.222(15) . ? N1 C4 1.338(16) . ? N1 N2 1.413(12) . ? N2 C1 1.367(15) . ? N3 C3 1.428(16) . ? N4 C9 1.326(13) . ? N4 N5 1.388(12) . ? N5 C6 1.341(15) . ? N6 C8 1.460(16) . ? N7 C14 1.363(14) . ? N7 N8 1.402(12) . ? N8 C11 1.360(13) . ? N9 C13 1.396(14) . ? N10 C22 1.317(15) . ? N10 C24 1.458(17) . ? N10 C23 1.480(19) . ? C28 O15 1.41(5) . ? C28 C27 1.522(10) . ? C1 C3 1.387(17) . ? C1 C2 1.526(17) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.402(18) . ? C4 C5 1.523(17) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C8 1.426(17) . ? C6 C7 1.470(16) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C9 1.353(17) . ? C9 C10 1.515(16) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C13 1.389(17) . ? C11 C12 1.501(16) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C14 1.440(16) . ? C14 C15 1.497(17) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.562(18) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C19 1.570(17) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 C21 1.516(16) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22 0.9400 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 Cl2 1.70(2) . ? C25 Cl2A 1.81(3) . ? C25 Cl3 1.968(10) . ? C29 O15 1.37(4) . ? C29 C30 1.514(10) . ? O15 C28A 1.375(10) . ? C27A C28A 1.522(10) . ? 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 N8 Cu1 N1 176.5(4) . . ? N8 Cu1 O8 88.2(4) . . ? N1 Cu1 O8 95.1(4) . . ? N8 Cu1 O7 87.5(3) . . ? N1 Cu1 O7 90.1(4) . . ? O8 Cu1 O7 154.1(3) . . ? N8 Cu1 O14 91.4(3) . . ? N1 Cu1 O14 86.6(4) . . ? O8 Cu1 O14 103.8(3) . . ? O7 Cu1 O14 101.8(3) . . ? N2 Cu2 N4 162.3(4) . . ? N2 Cu2 O10 92.7(4) . . ? N4 Cu2 O10 95.2(4) . . ? N2 Cu2 O7 88.7(4) . . ? N4 Cu2 O7 88.2(3) . . ? O10 Cu2 O7 163.5(3) . . ? N2 Cu2 O11 91.4(4) . . ? N4 Cu2 O11 106.2(4) . . ? O10 Cu2 O11 59.6(3) . . ? O7 Cu2 O11 104.0(3) . . ? N2 Cu2 C18 91.7(4) . . ? N4 Cu2 C18 102.9(4) . . ? O10 Cu2 C18 29.5(3) . . ? O7 Cu2 C18 134.1(4) . . ? O11 Cu2 C18 30.1(3) . . ? N7 Cu3 N5 166.2(4) . . ? N7 Cu3 O7 90.5(4) . . ? N5 Cu3 O7 86.4(4) . . ? N7 Cu3 O12 94.6(4) . . ? N5 Cu3 O12 92.3(4) . . ? O7 Cu3 O12 162.6(3) . . ? N7 Cu3 O13 94.9(3) . . ? N5 Cu3 O13 98.9(4) . . ? O7 Cu3 O13 104.3(3) . . ? O12 Cu3 O13 58.8(3) . . ? O9 Cu4 O9 180.0(5) 2_576 . ? O9 Cu4 O13 84.6(4) 2_576 2_576 ? O9 Cu4 O13 95.4(4) . 2_576 ? O9 Cu4 O13 95.4(4) 2_576 . ? O9 Cu4 O13 84.6(4) . . ? O13 Cu4 O13 180.0(5) 2_576 . ? O9 Cu4 O11 95.1(3) 2_576 . ? O9 Cu4 O11 84.9(3) . . ? O13 Cu4 O11 95.1(3) 2_576 . ? O13 Cu4 O11 84.9(3) . . ? O9 Cu4 O11 84.9(3) 2_576 2_576 ? O9 Cu4 O11 95.1(3) . 2_576 ? O13 Cu4 O11 84.9(3) 2_576 2_576 ? O13 Cu4 O11 95.1(3) . 2_576 ? O11 Cu4 O11 180.000(1) . 2_576 ? Cu3 O7 Cu2 108.0(4) . . ? Cu3 O7 Cu1 110.5(3) . . ? Cu2 O7 Cu1 109.5(3) . . ? C16 O8 Cu1 102.8(8) . . ? C16 O9 Cu4 139.7(9) . . ? C18 O10 Cu2 97.1(8) . . ? C18 O11 Cu4 146.9(9) . . ? C18 O11 Cu2 79.4(8) . . ? Cu4 O11 Cu2 130.3(4) . . ? C20 O12 Cu3 100.1(7) . . ? C20 O13 Cu4 140.4(9) . . ? C20 O13 Cu3 82.1(7) . . ? Cu4 O13 Cu3 136.0(4) . . ? C22 O14 Cu1 119.4(9) . . ? C4 N1 N2 108.4(10) . . ? C4 N1 Cu1 132.8(9) . . ? N2 N1 Cu1 117.9(8) . . ? C1 N2 N1 107.3(9) . . ? C1 N2 Cu2 132.5(8) . . ? N1 N2 Cu2 119.1(7) . . ? O2 N3 O1 120.7(13) . . ? O2 N3 C3 119.4(13) . . ? O1 N3 C3 119.9(12) . . ? C9 N4 N5 108.0(9) . . ? C9 N4 Cu2 134.8(8) . . ? N5 N4 Cu2 117.0(7) . . ? C6 N5 N4 110.5(9) . . ? C6 N5 Cu3 130.1(8) . . ? N4 N5 Cu3 119.4(7) . . ? O6 N6 O5 122.0(13) . . ? O6 N6 C8 120.6(13) . . ? O5 N6 C8 117.3(13) . . ? C14 N7 N8 109.9(9) . . ? C14 N7 Cu3 131.8(8) . . ? N8 N7 Cu3 118.2(7) . . ? C11 N8 N7 107.8(9) . . ? C11 N8 Cu1 132.1(8) . . ? N7 N8 Cu1 119.8(6) . . ? O3 N9 O4 119.5(11) . . ? O3 N9 C13 120.0(13) . . ? O4 N9 C13 120.2(12) . . ? C22 N10 C24 121.7(13) . . ? C22 N10 C23 121.1(12) . . ? C24 N10 C23 117.3(12) . . ? O15 C28 C27 122(4) . . ? N2 C1 C3 108.5(11) . . ? N2 C1 C2 121.3(11) . . ? C3 C1 C2 130.1(12) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 C4 107.0(12) . . ? C1 C3 N3 126.2(13) . . ? C4 C3 N3 126.7(12) . . ? N1 C4 C3 108.8(12) . . ? N1 C4 C5 121.3(12) . . ? C3 C4 C5 130.0(13) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N5 C6 C8 103.8(11) . . ? N5 C6 C7 124.6(11) . . ? C8 C6 C7 131.6(12) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C6 109.5(11) . . ? C9 C8 N6 127.1(12) . . ? C6 C8 N6 123.4(12) . . ? N4 C9 C8 108.2(11) . . ? N4 C9 C10 120.2(11) . . ? C8 C9 C10 131.6(11) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N8 C11 C13 108.7(10) . . ? N8 C11 C12 121.6(10) . . ? C13 C11 C12 129.7(10) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 N9 127.2(12) . . ? C11 C13 C14 107.6(10) . . ? N9 C13 C14 125.0(12) . . ? N7 C14 C13 105.8(11) . . ? N7 C14 C15 124.2(11) . . ? C13 C14 C15 129.9(11) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O8 C16 O9 121.6(13) . . ? O8 C16 C17 116.1(12) . . ? O9 C16 C17 122.0(13) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O10 C18 O11 123.9(13) . . ? O10 C18 C19 118.7(11) . . ? O11 C18 C19 117.3(11) . . ? O10 C18 Cu2 53.5(7) . . ? O11 C18 Cu2 70.5(7) . . ? C19 C18 Cu2 170.9(9) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O13 C20 O12 119.1(11) . . ? O13 C20 C21 121.6(12) . . ? O12 C20 C21 119.2(11) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O14 C22 N10 125.7(14) . . ? O14 C22 H22 117.1 . . ? N10 C22 H22 117.1 . . ? N10 C23 H23A 109.5 . . ? N10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N10 C24 H24A 109.5 . . ? N10 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N10 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Cl1 C25 Cl2 127.0(13) . . ? Cl1 C25 Cl2A 97.4(13) . . ? Cl2 C25 Cl2A 30.8(8) . . ? Cl1 C25 Cl3 102.1(10) . . ? Cl2 C25 Cl3 100.3(10) . . ? Cl2A C25 Cl3 101.6(11) . . ? O15 C29 C30 123(3) . . ? C29 O15 C28A 114(3) . . ? C29 O15 C28 146(3) . . ? C28A O15 C28 38(3) . . ? O15 C28A C27A 161(5) . . ? 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 N7 Cu3 O7 Cu2 150.9(4) . . . . ? N5 Cu3 O7 Cu2 -42.5(4) . . . . ? O12 Cu3 O7 Cu2 43.8(12) . . . . ? O13 Cu3 O7 Cu2 55.8(4) . . . . ? N7 Cu3 O7 Cu1 31.2(4) . . . . ? N5 Cu3 O7 Cu1 -162.3(4) . . . . ? O12 Cu3 O7 Cu1 -76.0(11) . . . . ? O13 Cu3 O7 Cu1 -64.0(4) . . . . ? N2 Cu2 O7 Cu3 -156.1(4) . . . . ? N4 Cu2 O7 Cu3 41.3(4) . . . . ? O10 Cu2 O7 Cu3 -61.0(13) . . . . ? O11 Cu2 O7 Cu3 -65.0(4) . . . . ? C18 Cu2 O7 Cu3 -65.0(6) . . . . ? N2 Cu2 O7 Cu1 -35.7(4) . . . . ? N4 Cu2 O7 Cu1 161.7(4) . . . . ? O10 Cu2 O7 Cu1 59.3(13) . . . . ? O11 Cu2 O7 Cu1 55.4(4) . . . . ? C18 Cu2 O7 Cu1 55.4(6) . . . . ? N8 Cu1 O7 Cu3 -35.0(4) . . . . ? N1 Cu1 O7 Cu3 147.5(4) . . . . ? O8 Cu1 O7 Cu3 45.7(8) . . . . ? O14 Cu1 O7 Cu3 -126.0(4) . . . . ? N8 Cu1 O7 Cu2 -153.9(4) . . . . ? N1 Cu1 O7 Cu2 28.6(4) . . . . ? O8 Cu1 O7 Cu2 -73.1(8) . . . . ? O14 Cu1 O7 Cu2 115.2(4) . . . . ? N8 Cu1 O8 C16 86.6(8) . . . . ? N1 Cu1 O8 C16 -94.7(8) . . . . ? O7 Cu1 O8 C16 6.0(12) . . . . ? O14 Cu1 O8 C16 177.6(7) . . . . ? O9 Cu4 O9 C16 -144(100) 2_576 . . . ? O13 Cu4 O9 C16 -26.8(13) 2_576 . . . ? O13 Cu4 O9 C16 153.2(13) . . . . ? O11 Cu4 O9 C16 -121.4(13) . . . . ? O11 Cu4 O9 C16 58.6(13) 2_576 . . . ? N2 Cu2 O10 C18 88.7(8) . . . . ? N4 Cu2 O10 C18 -107.1(8) . . . . ? O7 Cu2 O10 C18 -5.7(16) . . . . ? O11 Cu2 O10 C18 -1.3(7) . . . . ? O9 Cu4 O11 C18 -21.1(16) 2_576 . . . ? O9 Cu4 O11 C18 158.9(16) . . . . ? O13 Cu4 O11 C18 63.9(16) 2_576 . . . ? O13 Cu4 O11 C18 -116.1(16) . . . . ? O11 Cu4 O11 C18 -162(100) 2_576 . . . ? O9 Cu4 O11 Cu2 128.5(5) 2_576 . . . ? O9 Cu4 O11 Cu2 -51.5(5) . . . . ? O13 Cu4 O11 Cu2 -146.4(5) 2_576 . . . ? O13 Cu4 O11 Cu2 33.6(5) . . . . ? O11 Cu4 O11 Cu2 -13(100) 2_576 . . . ? N2 Cu2 O11 C18 -91.0(8) . . . . ? N4 Cu2 O11 C18 87.8(7) . . . . ? O10 Cu2 O11 C18 1.3(7) . . . . ? O7 Cu2 O11 C18 180.0(7) . . . . ? N2 Cu2 O11 Cu4 105.2(5) . . . . ? N4 Cu2 O11 Cu4 -75.9(6) . . . . ? O10 Cu2 O11 Cu4 -162.4(7) . . . . ? O7 Cu2 O11 Cu4 16.3(6) . . . . ? C18 Cu2 O11 Cu4 -163.7(10) . . . . ? N7 Cu3 O12 C20 -92.2(7) . . . . ? N5 Cu3 O12 C20 99.8(7) . . . . ? O7 Cu3 O12 C20 14.4(14) . . . . ? O13 Cu3 O12 C20 0.7(6) . . . . ? O9 Cu4 O13 C20 52.5(12) 2_576 . . . ? O9 Cu4 O13 C20 -127.5(12) . . . . ? O13 Cu4 O13 C20 83(100) 2_576 . . . ? O11 Cu4 O13 C20 147.2(12) . . . . ? O11 Cu4 O13 C20 -32.8(12) 2_576 . . . ? O9 Cu4 O13 Cu3 -147.3(6) 2_576 . . . ? O9 Cu4 O13 Cu3 32.7(6) . . . . ? O13 Cu4 O13 Cu3 -117(100) 2_576 . . . ? O11 Cu4 O13 Cu3 -52.6(6) . . . . ? O11 Cu4 O13 Cu3 127.4(6) 2_576 . . . ? N7 Cu3 O13 C20 91.7(7) . . . . ? N5 Cu3 O13 C20 -88.0(7) . . . . ? O7 Cu3 O13 C20 -176.5(6) . . . . ? O12 Cu3 O13 C20 -0.7(6) . . . . ? N7 Cu3 O13 Cu4 -75.7(6) . . . . ? N5 Cu3 O13 Cu4 104.6(6) . . . . ? O7 Cu3 O13 Cu4 16.1(7) . . . . ? O12 Cu3 O13 Cu4 -168.1(7) . . . . ? N8 Cu1 O14 C22 -102.8(9) . . . . ? N1 Cu1 O14 C22 74.3(10) . . . . ? O8 Cu1 O14 C22 168.7(9) . . . . ? O7 Cu1 O14 C22 -15.0(10) . . . . ? N8 Cu1 N1 C4 115(6) . . . . ? O8 Cu1 N1 C4 -44.6(13) . . . . ? O7 Cu1 N1 C4 160.8(13) . . . . ? O14 Cu1 N1 C4 59.0(13) . . . . ? N8 Cu1 N1 N2 -53(7) . . . . ? O8 Cu1 N1 N2 147.5(8) . . . . ? O7 Cu1 N1 N2 -7.1(8) . . . . ? O14 Cu1 N1 N2 -108.9(8) . . . . ? C4 N1 N2 C1 0.0(14) . . . . ? Cu1 N1 N2 C1 170.7(8) . . . . ? C4 N1 N2 Cu2 169.6(8) . . . . ? Cu1 N1 N2 Cu2 -19.7(11) . . . . ? N4 Cu2 N2 C1 -79.1(17) . . . . ? O10 Cu2 N2 C1 37.6(11) . . . . ? O7 Cu2 N2 C1 -158.9(11) . . . . ? O11 Cu2 N2 C1 97.2(11) . . . . ? C18 Cu2 N2 C1 67.0(12) . . . . ? N4 Cu2 N2 N1 114.5(13) . . . . ? O10 Cu2 N2 N1 -128.9(9) . . . . ? O7 Cu2 N2 N1 34.7(8) . . . . ? O11 Cu2 N2 N1 -69.3(8) . . . . ? C18 Cu2 N2 N1 -99.4(9) . . . . ? N2 Cu2 N4 C9 72.5(17) . . . . ? O10 Cu2 N4 C9 -43.8(12) . . . . ? O7 Cu2 N4 C9 152.4(12) . . . . ? O11 Cu2 N4 C9 -103.5(12) . . . . ? C18 Cu2 N4 C9 -72.6(12) . . . . ? N2 Cu2 N4 N5 -102.4(13) . . . . ? O10 Cu2 N4 N5 141.3(7) . . . . ? O7 Cu2 N4 N5 -22.5(7) . . . . ? O11 Cu2 N4 N5 81.5(7) . . . . ? C18 Cu2 N4 N5 112.5(8) . . . . ? C9 N4 N5 C6 -2.7(13) . . . . ? Cu2 N4 N5 C6 173.5(8) . . . . ? C9 N4 N5 Cu3 178.3(8) . . . . ? Cu2 N4 N5 Cu3 -5.5(10) . . . . ? N7 Cu3 N5 C6 -71(2) . . . . ? O7 Cu3 N5 C6 -148.2(11) . . . . ? O12 Cu3 N5 C6 49.2(11) . . . . ? O13 Cu3 N5 C6 107.9(11) . . . . ? N7 Cu3 N5 N4 108.0(18) . . . . ? O7 Cu3 N5 N4 30.5(8) . . . . ? O12 Cu3 N5 N4 -132.1(8) . . . . ? O13 Cu3 N5 N4 -73.4(8) . . . . ? N5 Cu3 N7 C14 85(2) . . . . ? O7 Cu3 N7 C14 162.3(10) . . . . ? O12 Cu3 N7 C14 -34.3(10) . . . . ? O13 Cu3 N7 C14 -93.3(10) . . . . ? N5 Cu3 N7 N8 -90.2(19) . . . . ? O7 Cu3 N7 N8 -13.2(8) . . . . ? O12 Cu3 N7 N8 150.1(8) . . . . ? O13 Cu3 N7 N8 91.2(8) . . . . ? C14 N7 N8 C11 -2.5(12) . . . . ? Cu3 N7 N8 C11 174.0(7) . . . . ? C14 N7 N8 Cu1 171.8(7) . . . . ? Cu3 N7 N8 Cu1 -11.7(10) . . . . ? N1 Cu1 N8 C11 -112(6) . . . . ? O8 Cu1 N8 C11 47.1(10) . . . . ? O7 Cu1 N8 C11 -158.5(10) . . . . ? O14 Cu1 N8 C11 -56.7(10) . . . . ? N1 Cu1 N8 N7 75(7) . . . . ? O8 Cu1 N8 N7 -125.7(8) . . . . ? O7 Cu1 N8 N7 28.8(8) . . . . ? O14 Cu1 N8 N7 130.6(8) . . . . ? N1 N2 C1 C3 -1.3(14) . . . . ? Cu2 N2 C1 C3 -168.9(9) . . . . ? N1 N2 C1 C2 -178.7(12) . . . . ? Cu2 N2 C1 C2 13.7(19) . . . . ? N2 C1 C3 C4 2.0(15) . . . . ? C2 C1 C3 C4 179.1(14) . . . . ? N2 C1 C3 N3 179.2(11) . . . . ? C2 C1 C3 N3 -4(2) . . . . ? O2 N3 C3 C1 3(2) . . . . ? O1 N3 C3 C1 -175.9(13) . . . . ? O2 N3 C3 C4 -179.8(14) . . . . ? O1 N3 C3 C4 1(2) . . . . ? N2 N1 C4 C3 1.2(15) . . . . ? Cu1 N1 C4 C3 -167.5(9) . . . . ? N2 N1 C4 C5 -178.7(11) . . . . ? Cu1 N1 C4 C5 13(2) . . . . ? C1 C3 C4 N1 -2.0(15) . . . . ? N3 C3 C4 N1 -179.2(12) . . . . ? C1 C3 C4 C5 178.0(14) . . . . ? N3 C3 C4 C5 1(2) . . . . ? N4 N5 C6 C8 2.1(13) . . . . ? Cu3 N5 C6 C8 -179.1(8) . . . . ? N4 N5 C6 C7 -178.1(12) . . . . ? Cu3 N5 C6 C7 1(2) . . . . ? N5 C6 C8 C9 -0.9(15) . . . . ? C7 C6 C8 C9 179.3(14) . . . . ? N5 C6 C8 N6 -178.6(11) . . . . ? C7 C6 C8 N6 2(2) . . . . ? O6 N6 C8 C9 -174.3(16) . . . . ? O5 N6 C8 C9 3(2) . . . . ? O6 N6 C8 C6 3(2) . . . . ? O5 N6 C8 C6 -179.7(13) . . . . ? N5 N4 C9 C8 2.1(14) . . . . ? Cu2 N4 C9 C8 -173.2(9) . . . . ? N5 N4 C9 C10 -179.8(11) . . . . ? Cu2 N4 C9 C10 5.0(19) . . . . ? C6 C8 C9 N4 -0.8(16) . . . . ? N6 C8 C9 N4 176.9(12) . . . . ? C6 C8 C9 C10 -178.6(13) . . . . ? N6 C8 C9 C10 -1(2) . . . . ? N7 N8 C11 C13 0.3(12) . . . . ? Cu1 N8 C11 C13 -173.0(8) . . . . ? N7 N8 C11 C12 179.9(10) . . . . ? Cu1 N8 C11 C12 6.6(17) . . . . ? N8 C11 C13 N9 -173.7(11) . . . . ? C12 C11 C13 N9 7(2) . . . . ? N8 C11 C13 C14 1.8(13) . . . . ? C12 C11 C13 C14 -177.8(12) . . . . ? O3 N9 C13 C11 15.2(19) . . . . ? O4 N9 C13 C11 -171.0(12) . . . . ? O3 N9 C13 C14 -159.5(12) . . . . ? O4 N9 C13 C14 14.3(19) . . . . ? N8 N7 C14 C13 3.5(12) . . . . ? Cu3 N7 C14 C13 -172.3(8) . . . . ? N8 N7 C14 C15 -178.6(11) . . . . ? Cu3 N7 C14 C15 5.5(17) . . . . ? C11 C13 C14 N7 -3.2(12) . . . . ? N9 C13 C14 N7 172.3(11) . . . . ? C11 C13 C14 C15 179.1(12) . . . . ? N9 C13 C14 C15 -5(2) . . . . ? Cu1 O8 C16 O9 -0.8(13) . . . . ? Cu1 O8 C16 C17 -174.6(9) . . . . ? Cu4 O9 C16 O8 162.9(8) . . . . ? Cu4 O9 C16 C17 -24(2) . . . . ? Cu2 O10 C18 O11 2.5(14) . . . . ? Cu2 O10 C18 C19 -174.4(10) . . . . ? Cu4 O11 C18 O10 154.8(11) . . . . ? Cu2 O11 C18 O10 -2.2(12) . . . . ? Cu4 O11 C18 C19 -28(2) . . . . ? Cu2 O11 C18 C19 174.8(11) . . . . ? Cu4 O11 C18 Cu2 156.9(14) . . . . ? N2 Cu2 C18 O10 -92.4(8) . . . . ? N4 Cu2 C18 O10 77.6(8) . . . . ? O7 Cu2 C18 O10 177.8(6) . . . . ? O11 Cu2 C18 O10 177.8(12) . . . . ? N2 Cu2 C18 O11 89.8(7) . . . . ? N4 Cu2 C18 O11 -100.2(7) . . . . ? O10 Cu2 C18 O11 -177.8(12) . . . . ? O7 Cu2 C18 O11 0.0(10) . . . . ? N2 Cu2 C18 C19 -60(6) . . . . ? N4 Cu2 C18 C19 110(6) . . . . ? O10 Cu2 C18 C19 32(6) . . . . ? O7 Cu2 C18 C19 -150(6) . . . . ? O11 Cu2 C18 C19 -150(7) . . . . ? Cu4 O13 C20 O12 167.3(8) . . . . ? Cu3 O13 C20 O12 1.1(9) . . . . ? Cu4 O13 C20 C21 -10.8(19) . . . . ? Cu3 O13 C20 C21 -177.0(10) . . . . ? Cu3 O12 C20 O13 -1.3(11) . . . . ? Cu3 O12 C20 C21 176.8(9) . . . . ? Cu1 O14 C22 N10 170.1(10) . . . . ? C24 N10 C22 O14 -175.7(13) . . . . ? C23 N10 C22 O14 4(2) . . . . ? C30 C29 O15 C28A 153(4) . . . . ? C30 C29 O15 C28 -179(6) . . . . ? C27 C28 O15 C29 -173(4) . . . . ? C27 C28 O15 C28A -129(8) . . . . ? C29 O15 C28A C27A 161(14) . . . . ? C28 O15 C28A C27A 6(13) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.36 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.913 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.147 #===END