# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Sasankasekhar Mohanta' _publ_contact_author_address ; 92 A. P. C. Road Kolkata West Bengal India 700009 ; _publ_contact_author_email 'sm cu chem@yahoo.co.in' loop_ _publ_author_name M.Nayak S.Sarkar S.Hazra H.Sparkes J.Howard S.Mohanta data_1 _database_code_depnum_ccdc_archive 'CCDC 761685' #TrackingRef '- 1-4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H26 Cu N2 O6 Zn, 2(C20 H22 Cu N2 O4), 2(Cl O4)' _chemical_formula_sum 'C60 H70 Cl2 Cu3 N6 O22 Zn' _chemical_formula_weight 1554.11 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' Cl Cl 0.1484 0.1585 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.3706(3) _cell_length_b 22.8263(4) _cell_length_c 21.5225(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.810(3) _cell_angle_gamma 90.00 _cell_volume 6217.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7642 _cell_measurement_theta_min 2.6744 _cell_measurement_theta_max 29.1465 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3196 _exptl_absorpt_coefficient_mu 1.565 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.602 _exptl_absorpt_correction_T_max 0.849 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 16.1511 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23495 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 29.20 _reflns_number_total 7408 _reflns_number_gt 4412 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7408 _refine_ls_number_parameters 445 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.030488(19) 0.2500 0.01868(12) Uani 1 2 d SD . . Cu1 Cu 0.03602(3) -0.042314(14) 0.444266(16) 0.01990(10) Uani 1 1 d . . . Cu2 Cu 0.0000 -0.10298(2) 0.2500 0.02222(14) Uani 1 2 d S . . Cl1 Cl 0.52375(6) 0.17736(3) 0.41738(4) 0.02547(18) Uani 1 1 d D . . O1 O 0.06715(16) 0.15314(8) 0.43187(9) 0.0276(5) Uani 1 1 d . . . O2 O 0.06121(15) 0.04064(8) 0.44779(8) 0.0203(4) Uani 1 1 d . . . O3 O -0.09192(15) -0.03016(8) 0.37451(9) 0.0226(5) Uani 1 1 d . . . O4 O -0.26419(17) 0.01148(10) 0.29703(10) 0.0348(6) Uani 1 1 d . . . O5 O -0.04980(18) 0.06598(9) 0.31759(10) 0.0218(5) Uani 1 1 d D . . O6 O 0.18461(15) 0.05671(8) 0.33118(9) 0.0234(5) Uani 1 1 d . . . O7 O 0.08997(15) -0.04034(8) 0.29001(9) 0.0218(5) Uani 1 1 d . . . O8A O 0.5048(3) 0.1929(3) 0.4766(2) 0.0484(14) Uani 0.77 1 d PD A 1 O9A O 0.4387(3) 0.19812(16) 0.36025(13) 0.0391(10) Uani 0.77 1 d PD A 1 O10A O 0.6214(3) 0.2052(2) 0.41501(17) 0.0382(11) Uani 0.77 1 d PD A 1 O11 O 0.53193(18) 0.11513(9) 0.41256(11) 0.0391(6) Uani 1 1 d . A . N1 N 0.16247(19) -0.05836(10) 0.51572(11) 0.0207(6) Uani 1 1 d . . . N2 N 0.0219(2) -0.12667(10) 0.43783(11) 0.0260(6) Uani 1 1 d . . . N3 N 0.0967(2) -0.16363(10) 0.29128(11) 0.0277(7) Uani 1 1 d . . . C1 C -0.0392(3) 0.23319(13) 0.37616(15) 0.0360(9) Uani 1 1 d . . . H1A H -0.0463 0.2148 0.3338 0.054 Uiso 1 1 calc R . . H1B H -0.0423 0.2759 0.3710 0.054 Uiso 1 1 calc R . . H1C H -0.0968 0.2201 0.3916 0.054 Uiso 1 1 calc R . . C2 C 0.0659(3) 0.21597(12) 0.42578(15) 0.0318(8) Uani 1 1 d . . . H2A H 0.1248 0.2291 0.4107 0.038 Uiso 1 1 calc R . . H2B H 0.0741 0.2345 0.4687 0.038 Uiso 1 1 calc R . . C3 C 0.1566(3) 0.12834(12) 0.47524(14) 0.0239(7) Uani 1 1 d . . . C4 C 0.2469(3) 0.15884(13) 0.50791(15) 0.0296(8) Uani 1 1 d . . . H4 H 0.2498 0.1999 0.5017 0.035 Uiso 1 1 calc R . . C5 C 0.3347(3) 0.12961(13) 0.55036(14) 0.0310(8) Uani 1 1 d . . . H5 H 0.3973 0.1507 0.5725 0.037 Uiso 1 1 calc R . . C6 C 0.3298(2) 0.07095(13) 0.55952(14) 0.0249(7) Uani 1 1 d . . . H6 H 0.3889 0.0514 0.5889 0.030 Uiso 1 1 calc R . . C7 C 0.2383(2) 0.03864(12) 0.52621(13) 0.0192(6) Uani 1 1 d . . . C8 C 0.1503(2) 0.06688(12) 0.48268(13) 0.0187(7) Uani 1 1 d . . . C9 C 0.2386(2) -0.02274(12) 0.54169(14) 0.0213(7) Uani 1 1 d . . . H9 H 0.2999 -0.0380 0.5736 0.026 Uiso 1 1 calc R . . C10 C 0.1653(3) -0.11888(12) 0.53957(14) 0.0283(8) Uani 1 1 d . . . H10A H 0.1265 -0.1216 0.5716 0.034 Uiso 1 1 calc R . . H10B H 0.2393 -0.1312 0.5616 0.034 Uiso 1 1 calc R . . C11 C 0.1142(3) -0.15809(12) 0.48124(15) 0.0316(8) Uani 1 1 d . . . H11A H 0.1649 -0.1669 0.4576 0.038 Uiso 1 1 calc R . . H11B H 0.0919 -0.1955 0.4960 0.038 Uiso 1 1 calc R . . C12 C -0.0588(3) -0.15588(14) 0.40258(15) 0.0339(9) Uani 1 1 d . . . H12 H -0.0564 -0.1973 0.4069 0.041 Uiso 1 1 calc R . . C13 C -0.1521(3) -0.13049(14) 0.35722(15) 0.0328(7) Uani 1 1 d U . . C14 C -0.2365(3) -0.16821(16) 0.32294(16) 0.0432(8) Uani 1 1 d U . . H14 H -0.2298 -0.2092 0.3308 0.052 Uiso 1 1 calc R . . C15 C -0.3260(3) -0.14673(17) 0.27931(16) 0.0469(9) Uani 1 1 d U . . H15 H -0.3805 -0.1728 0.2560 0.056 Uiso 1 1 calc R . . C16 C -0.3388(3) -0.08686(17) 0.26838(15) 0.0429(8) Uani 1 1 d U . . H16 H -0.4022 -0.0722 0.2378 0.051 Uiso 1 1 calc R . . C17 C -0.2604(3) -0.04876(15) 0.30157(14) 0.0345(7) Uani 1 1 d U . . C18 C -0.1639(3) -0.06950(14) 0.34601(14) 0.0290(7) Uani 1 1 d U . . C19 C -0.3643(3) 0.03826(18) 0.26561(16) 0.0457(10) Uani 1 1 d . . . H19A H -0.4190 0.0205 0.2816 0.055 Uiso 1 1 calc R . . H19B H -0.3853 0.0325 0.2175 0.055 Uiso 1 1 calc R . . C20 C -0.3538(3) 0.10264(18) 0.28177(16) 0.0516(11) Uani 1 1 d . . . H20A H -0.3566 0.1087 0.3263 0.077 Uiso 1 1 calc R . . H20B H -0.4118 0.1241 0.2503 0.077 Uiso 1 1 calc R . . H20C H -0.2861 0.1170 0.2793 0.077 Uiso 1 1 calc R . . C21 C 0.1700(3) 0.15766(13) 0.30395(17) 0.0414(9) Uani 1 1 d . . . H21A H 0.1497 0.1468 0.2575 0.062 Uiso 1 1 calc R . . H21B H 0.2070 0.1954 0.3107 0.062 Uiso 1 1 calc R . . H21C H 0.1066 0.1609 0.3172 0.062 Uiso 1 1 calc R . . C22 C 0.2417(3) 0.11157(13) 0.34459(15) 0.0289(8) Uani 1 1 d . . . H22A H 0.3072 0.1088 0.3328 0.035 Uiso 1 1 calc R . . H22B H 0.2611 0.1214 0.3918 0.035 Uiso 1 1 calc R . . C23 C 0.2393(2) 0.00720(13) 0.35923(13) 0.0215(6) Uani 1 1 d U . . C24 C 0.3385(2) 0.00599(15) 0.40602(14) 0.0291(7) Uani 1 1 d U . . H24 H 0.3755 0.0414 0.4215 0.035 Uiso 1 1 calc R . . C25 C 0.3834(3) -0.04768(15) 0.43000(14) 0.0345(7) Uani 1 1 d U . . H25 H 0.4507 -0.0486 0.4630 0.041 Uiso 1 1 calc R . . C26 C 0.3335(3) -0.09875(15) 0.40744(14) 0.0338(7) Uani 1 1 d U . . H26 H 0.3667 -0.1348 0.4245 0.041 Uiso 1 1 calc R . . C27 C 0.2328(3) -0.09946(14) 0.35888(13) 0.0270(7) Uani 1 1 d U . . C28 C 0.1852(2) -0.04504(13) 0.33535(12) 0.0211(6) Uani 1 1 d U . . C29 C 0.1869(3) -0.15548(13) 0.33408(14) 0.0325(9) Uani 1 1 d . . . H29 H 0.2277 -0.1893 0.3513 0.039 Uiso 1 1 calc R . . C30 C 0.0595(3) -0.22159(13) 0.26339(15) 0.0390(10) Uani 1 1 d . . . H30A H 0.0839 -0.2520 0.2978 0.047 Uiso 1 1 calc R . . H30B H 0.0890 -0.2307 0.2278 0.047 Uiso 1 1 calc R . . H5A H -0.0039(19) 0.0721(15) 0.3510(10) 0.061(14) Uiso 1 1 d D . . H5B H -0.090(2) 0.0415(12) 0.3271(15) 0.063(13) Uiso 1 1 d D . . O9B O 0.4223(10) 0.1999(7) 0.3862(5) 0.0391(10) Uani 0.23 1 d PD A 2 O10B O 0.5903(11) 0.2067(8) 0.3922(8) 0.0382(11) Uani 0.23 1 d PD A 2 O8B O 0.5501(14) 0.1933(11) 0.4827(7) 0.0484(14) Uani 0.23 1 d PD 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 Zn1 0.0182(3) 0.0157(3) 0.0206(2) 0.000 0.0041(2) 0.000 Cu1 0.0197(2) 0.01546(19) 0.02483(19) -0.00509(15) 0.00762(17) -0.00465(15) Cu2 0.0313(4) 0.0151(3) 0.0176(3) 0.000 0.0043(3) 0.000 Cl1 0.0248(4) 0.0211(4) 0.0276(4) -0.0001(3) 0.0044(4) 0.0015(3) O1 0.0283(14) 0.0166(11) 0.0309(12) 0.0002(8) -0.0001(11) -0.0046(9) O2 0.0147(11) 0.0160(10) 0.0260(10) -0.0037(9) 0.0007(9) -0.0018(9) O3 0.0165(12) 0.0230(11) 0.0270(11) -0.0064(8) 0.0054(10) -0.0099(9) O4 0.0132(13) 0.0551(16) 0.0310(13) -0.0021(11) 0.0002(11) -0.0038(10) O5 0.0162(13) 0.0228(12) 0.0240(12) -0.0048(9) 0.0031(12) -0.0033(9) O6 0.0178(12) 0.0221(11) 0.0250(11) -0.0030(8) -0.0006(10) -0.0042(9) O7 0.0195(12) 0.0193(11) 0.0222(10) -0.0014(8) 0.0007(9) 0.0021(9) O8A 0.070(4) 0.0491(18) 0.0398(17) 0.0080(14) 0.036(2) 0.022(3) O9A 0.046(2) 0.0332(15) 0.027(2) 0.0104(19) -0.0039(18) -0.0014(13) O10A 0.022(3) 0.0351(15) 0.052(3) -0.001(2) 0.004(2) -0.0009(19) O11 0.0463(17) 0.0192(12) 0.0504(14) 0.0039(10) 0.0137(13) 0.0038(10) N1 0.0230(16) 0.0163(13) 0.0250(14) -0.0007(10) 0.0109(12) -0.0005(10) N2 0.0335(18) 0.0197(14) 0.0277(14) -0.0050(11) 0.0140(14) -0.0068(12) N3 0.047(2) 0.0196(14) 0.0160(13) 0.0025(10) 0.0102(14) 0.0086(12) C1 0.044(2) 0.0222(18) 0.0366(19) 0.0048(14) 0.0054(18) 0.0026(15) C2 0.039(2) 0.0154(16) 0.0353(19) -0.0021(13) 0.0042(17) -0.0091(14) C3 0.029(2) 0.0194(16) 0.0230(16) -0.0033(12) 0.0080(16) -0.0064(13) C4 0.032(2) 0.0204(17) 0.0336(18) -0.0032(13) 0.0075(17) -0.0122(14) C5 0.029(2) 0.0308(19) 0.0301(18) -0.0042(14) 0.0049(17) -0.0153(15) C6 0.0169(19) 0.0320(18) 0.0236(17) -0.0022(13) 0.0035(15) -0.0038(13) C7 0.0189(17) 0.0212(15) 0.0204(14) -0.0053(13) 0.0103(14) -0.0034(13) C8 0.0187(19) 0.0193(15) 0.0199(15) -0.0068(12) 0.0088(15) -0.0075(12) C9 0.0177(18) 0.0250(17) 0.0226(16) -0.0001(12) 0.0084(15) 0.0044(12) C10 0.030(2) 0.0203(16) 0.0351(18) 0.0041(13) 0.0109(16) 0.0017(13) C11 0.045(2) 0.0184(16) 0.0371(19) 0.0006(14) 0.0218(18) 0.0015(15) C12 0.051(3) 0.0233(18) 0.0329(19) -0.0084(14) 0.0217(19) -0.0135(16) C13 0.0377(17) 0.0396(16) 0.0268(14) -0.0159(12) 0.0182(14) -0.0235(13) C14 0.0485(19) 0.0508(17) 0.0336(16) -0.0207(13) 0.0176(15) -0.0336(15) C15 0.0457(19) 0.0652(18) 0.0313(16) -0.0221(15) 0.0144(15) -0.0412(16) C16 0.0369(18) 0.0664(19) 0.0260(15) -0.0140(14) 0.0110(14) -0.0288(15) C17 0.0285(16) 0.0553(18) 0.0224(14) -0.0135(13) 0.0122(13) -0.0204(14) C18 0.0277(16) 0.0409(16) 0.0232(14) -0.0128(12) 0.0147(13) -0.0175(13) C19 0.0139(19) 0.092(3) 0.0297(19) 0.008(2) 0.0049(16) 0.004(2) C20 0.037(3) 0.089(3) 0.0293(19) 0.009(2) 0.0106(19) 0.030(2) C21 0.040(2) 0.0262(19) 0.055(2) -0.0058(16) 0.012(2) -0.0167(16) C22 0.022(2) 0.0324(19) 0.0312(18) -0.0085(14) 0.0067(16) -0.0124(14) C23 0.0161(15) 0.0345(15) 0.0156(13) 0.0006(11) 0.0072(12) 0.0051(12) C24 0.0191(15) 0.0491(17) 0.0175(13) -0.0045(12) 0.0037(12) 0.0003(13) C25 0.0220(15) 0.0570(18) 0.0211(13) -0.0003(13) 0.0022(12) 0.0116(14) C26 0.0312(16) 0.0503(17) 0.0198(13) 0.0044(13) 0.0081(13) 0.0216(13) C27 0.0262(16) 0.0381(15) 0.0145(13) 0.0019(12) 0.0036(12) 0.0148(12) C28 0.0196(14) 0.0308(14) 0.0128(12) 0.0003(11) 0.0052(11) 0.0080(12) C29 0.050(3) 0.0311(19) 0.0169(16) 0.0091(13) 0.0119(18) 0.0234(17) C30 0.075(3) 0.0150(17) 0.029(2) 0.0014(13) 0.020(2) 0.0085(15) O9B 0.046(2) 0.0332(15) 0.027(2) 0.0104(19) -0.0039(18) -0.0014(13) O10B 0.022(3) 0.0351(15) 0.052(3) -0.001(2) 0.004(2) -0.0009(19) O8B 0.070(4) 0.0491(18) 0.0398(17) 0.0080(14) 0.036(2) 0.022(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 Zn1 O5 1.960(2) . ? Zn1 O5 1.960(2) 2 ? Zn1 O7 2.0333(18) 2 ? Zn1 O7 2.0333(18) . ? Zn1 Cu2 3.0467(6) . ? Cu1 O3 1.8977(19) . ? Cu1 N1 1.919(2) . ? Cu1 O2 1.9204(18) . ? Cu1 N2 1.935(2) . ? Cu2 O7 1.8882(18) . ? Cu2 O7 1.8882(18) 2 ? Cu2 N3 1.907(2) 2 ? Cu2 N3 1.907(2) . ? Cl1 O10B 1.359(13) . ? Cl1 O8B 1.384(14) . ? Cl1 O9B 1.402(12) . ? Cl1 O8A 1.423(4) . ? Cl1 O11 1.431(2) . ? Cl1 O9A 1.458(3) . ? Cl1 O10A 1.468(4) . ? O1 C3 1.379(3) . ? O1 C2 1.440(3) . ? O2 C8 1.328(3) . ? O3 C18 1.315(3) . ? O4 C17 1.378(4) . ? O4 C19 1.428(4) . ? O5 H5A 0.793(17) . ? O5 H5B 0.845(17) . ? O6 C23 1.376(3) . ? O6 C22 1.447(3) . ? O7 C28 1.335(3) . ? N1 C9 1.281(3) . ? N1 C10 1.470(3) . ? N2 C12 1.287(4) . ? N2 C11 1.472(4) . ? N3 C29 1.273(4) . ? N3 C30 1.472(4) . ? C1 C2 1.517(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.374(4) . ? C3 C8 1.418(4) . ? C4 C5 1.403(4) . ? C4 H4 0.9500 . ? C5 C6 1.358(4) . ? C5 H5 0.9500 . ? C6 C7 1.410(4) . ? C6 H6 0.9500 . ? C7 C8 1.402(4) . ? C7 C9 1.440(4) . ? C9 H9 0.9500 . ? C10 C11 1.513(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.436(5) . ? C12 H12 0.9500 . ? C13 C18 1.413(4) . ? C13 C14 1.422(4) . ? C14 C15 1.353(5) . ? C14 H14 0.9500 . ? C15 C16 1.388(5) . ? C15 H15 0.9500 . ? C16 C17 1.373(4) . ? C16 H16 0.9500 . ? C17 C18 1.416(5) . ? C19 C20 1.506(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.500(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.383(4) . ? C23 C28 1.403(4) . ? C24 C25 1.389(4) . ? C24 H24 0.9500 . ? C25 C26 1.353(4) . ? C25 H25 0.9500 . ? C26 C27 1.414(4) . ? C26 H26 0.9500 . ? C27 C28 1.413(4) . ? C27 C29 1.444(4) . ? C29 H29 0.9500 . ? C30 C30 1.508(7) 2 ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O5 131.16(12) . 2 ? O5 Zn1 O7 110.29(8) . 2 ? O5 Zn1 O7 108.09(8) 2 2 ? O5 Zn1 O7 108.09(8) . . ? O5 Zn1 O7 110.29(8) 2 . ? O7 Zn1 O7 74.67(10) 2 . ? O5 Zn1 Cu2 114.42(6) . . ? O5 Zn1 Cu2 114.42(6) 2 . ? O7 Zn1 Cu2 37.33(5) 2 . ? O7 Zn1 Cu2 37.33(5) . . ? O3 Cu1 N1 177.05(9) . . ? O3 Cu1 O2 89.37(8) . . ? N1 Cu1 O2 93.36(9) . . ? O3 Cu1 N2 92.68(10) . . ? N1 Cu1 N2 84.71(10) . . ? O2 Cu1 N2 174.62(10) . . ? O7 Cu2 O7 81.55(11) . 2 ? O7 Cu2 N3 177.14(10) . 2 ? O7 Cu2 N3 95.78(10) 2 2 ? O7 Cu2 N3 95.78(10) . . ? O7 Cu2 N3 177.14(10) 2 . ? N3 Cu2 N3 86.91(16) 2 . ? O7 Cu2 Zn1 40.77(6) . . ? O7 Cu2 Zn1 40.77(6) 2 . ? N3 Cu2 Zn1 136.54(8) 2 . ? N3 Cu2 Zn1 136.54(8) . . ? O10B Cl1 O8B 106.9(12) . . ? O10B Cl1 O9B 106.5(9) . . ? O8B Cl1 O9B 106.2(9) . . ? O10B Cl1 O11 112.7(9) . . ? O8B Cl1 O11 109.6(10) . . ? O9B Cl1 O11 114.5(7) . . ? O8A Cl1 O11 110.6(3) . . ? O8A Cl1 O9A 111.0(2) . . ? O11 Cl1 O9A 108.57(18) . . ? O8A Cl1 O10A 110.0(3) . . ? O11 Cl1 O10A 109.7(2) . . ? O9A Cl1 O10A 106.9(2) . . ? C3 O1 C2 116.9(2) . . ? C8 O2 Cu1 125.51(17) . . ? C18 O3 Cu1 127.4(2) . . ? C17 O4 C19 117.9(3) . . ? Zn1 O5 H5A 113(2) . . ? Zn1 O5 H5B 107.4(19) . . ? H5A O5 H5B 105(3) . . ? C23 O6 C22 116.9(2) . . ? C28 O7 Cu2 126.12(17) . . ? C28 O7 Zn1 131.89(17) . . ? Cu2 O7 Zn1 101.89(8) . . ? C9 N1 C10 121.1(2) . . ? C9 N1 Cu1 126.8(2) . . ? C10 N1 Cu1 112.08(18) . . ? C12 N2 C11 119.6(3) . . ? C12 N2 Cu1 127.0(2) . . ? C11 N2 Cu1 113.39(18) . . ? C29 N3 C30 122.9(3) . . ? C29 N3 Cu2 124.9(2) . . ? C30 N3 Cu2 111.9(2) . . ? 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 . . ? O1 C2 C1 107.6(2) . . ? O1 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? O1 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C4 C3 O1 124.4(3) . . ? C4 C3 C8 121.2(3) . . ? O1 C3 C8 114.3(2) . . ? C3 C4 C5 120.3(3) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.6(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 121.1(3) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 120.2(3) . . ? C8 C7 C9 122.8(3) . . ? C6 C7 C9 117.0(3) . . ? O2 C8 C7 125.2(2) . . ? O2 C8 C3 117.2(3) . . ? C7 C8 C3 117.5(3) . . ? N1 C9 C7 125.0(3) . . ? N1 C9 H9 117.5 . . ? C7 C9 H9 117.5 . . ? N1 C10 C11 108.2(2) . . ? N1 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? N1 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? N2 C11 C10 107.5(2) . . ? N2 C11 H11A 110.2 . . ? C10 C11 H11A 110.2 . . ? N2 C11 H11B 110.2 . . ? C10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? N2 C12 C13 124.9(3) . . ? N2 C12 H12 117.6 . . ? C13 C12 H12 117.6 . . ? C18 C13 C14 118.8(3) . . ? C18 C13 C12 122.6(3) . . ? C14 C13 C12 118.6(3) . . ? C15 C14 C13 121.1(4) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 120.5(3) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 120.3(4) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 O4 126.2(3) . . ? C16 C17 C18 121.1(3) . . ? O4 C17 C18 112.7(3) . . ? O3 C18 C13 124.7(3) . . ? O3 C18 C17 117.2(3) . . ? C13 C18 C17 118.2(3) . . ? O4 C19 C20 107.7(3) . . ? O4 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O4 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O6 C22 C21 107.1(2) . . ? O6 C22 H22A 110.3 . . ? C21 C22 H22A 110.3 . . ? O6 C22 H22B 110.3 . . ? C21 C22 H22B 110.3 . . ? H22A C22 H22B 108.6 . . ? O6 C23 C24 125.8(3) . . ? O6 C23 C28 113.5(3) . . ? C24 C23 C28 120.7(3) . . ? C23 C24 C25 119.1(3) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C26 C25 C24 121.5(3) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C25 C26 C27 121.1(3) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 117.8(3) . . ? C28 C27 C29 123.9(3) . . ? C26 C27 C29 118.3(3) . . ? O7 C28 C23 117.2(3) . . ? O7 C28 C27 123.1(3) . . ? C23 C28 C27 119.7(3) . . ? N3 C29 C27 126.0(3) . . ? N3 C29 H29 117.0 . . ? C27 C29 H29 117.0 . . ? N3 C30 C30 109.40(19) . 2 ? N3 C30 H30A 109.8 . . ? C30 C30 H30A 109.8 2 . ? N3 C30 H30B 109.8 . . ? C30 C30 H30B 109.8 2 . ? H30A C30 H30B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.879 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.722 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.074 #END=== data_2 _database_code_depnum_ccdc_archive 'CCDC 761686' #TrackingRef '- 1-4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H29 Cd Cu N3 O6, 2(C20 H22 Cu N2 O4), 2(Cl O4)' _chemical_formula_sum 'C62 H73 Cd Cl2 Cu3 N7 O22' _chemical_formula_weight 1642.19 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' Cl Cl 0.1484 0.1585 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.3303(8) _cell_length_b 14.4792(2) _cell_length_c 20.0508(6) _cell_angle_alpha 90.00 _cell_angle_beta 124.977(4) _cell_angle_gamma 90.00 _cell_volume 6501.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5518 _cell_measurement_theta_min 2.6072 _cell_measurement_theta_max 30.7403 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3356 _exptl_absorpt_coefficient_mu 1.457 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.655 _exptl_absorpt_correction_T_max 0.878 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 16.1511 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14700 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5738 _reflns_number_gt 4807 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0365P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5738 _refine_ls_number_parameters 456 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0600 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.862801(15) 0.7500 0.01244(7) Uani 1 2 d SD . . Cu1 Cu 0.197895(11) 0.695952(18) 0.907448(16) 0.01362(8) Uani 1 1 d . . . Cu2 Cu 0.0000 0.63666(2) 0.7500 0.01313(9) Uani 1 2 d S . . Cl1 Cl 0.33660(3) 0.78726(4) 0.72850(4) 0.02288(14) Uani 1 1 d . . . O1 O 0.06935(7) 0.66968(11) 0.97594(9) 0.0188(4) Uani 1 1 d . . . O2 O 0.13654(6) 0.66940(10) 0.92342(9) 0.0162(3) Uani 1 1 d . . . O3 O 0.19176(6) 0.82619(10) 0.92043(9) 0.0159(3) Uani 1 1 d . . . O4 O 0.16300(6) 0.99624(10) 0.93136(9) 0.0177(3) Uani 1 1 d . . . O5 O 0.07581(7) 0.84745(11) 0.88504(10) 0.0164(3) Uani 1 1 d D . . O6 O 0.07931(6) 0.88778(10) 0.71867(9) 0.0155(3) Uani 1 1 d . . . O7 O 0.03559(6) 0.73361(10) 0.72889(9) 0.0139(3) Uani 1 1 d . . . O8 O 0.35253(9) 0.87228(12) 0.77319(12) 0.0381(5) Uani 1 1 d U . . O9 O 0.27515(8) 0.79228(14) 0.66037(13) 0.0503(6) Uani 1 1 d U . . O10 O 0.37194(9) 0.77634(15) 0.69779(14) 0.0488(6) Uani 1 1 d U . . O11 O 0.34393(10) 0.71210(14) 0.77860(12) 0.0491(6) Uani 1 1 d U . . N1 N 0.20687(7) 0.56592(13) 0.89096(10) 0.0136(4) Uani 1 1 d . . . N2 N 0.25947(8) 0.71425(13) 0.88894(11) 0.0149(4) Uani 1 1 d . . . N3 N 0.03528(7) 0.54101(12) 0.72532(10) 0.0143(4) Uani 1 1 d U . . N4 N 0.0000 1.02063(19) 0.7500 0.0227(6) Uani 1 2 d S A . C1 C 0.02718(11) 0.77324(18) 1.02017(16) 0.0299(6) Uani 1 1 d . . . H1A H 0.0657 0.8046 1.0554 0.045 Uiso 1 1 calc R . . H1B H 0.0042 0.7788 1.0437 0.045 Uiso 1 1 calc R . . H1C H 0.0048 0.8018 0.9661 0.045 Uiso 1 1 calc R . . C2 C 0.03748(10) 0.67337(17) 1.01297(14) 0.0205(5) Uani 1 1 d . . . H2A H 0.0612 0.6441 1.0674 0.025 Uiso 1 1 calc R . . H2B H -0.0011 0.6404 0.9789 0.025 Uiso 1 1 calc R . . C3 C 0.08839(9) 0.58454(15) 0.97000(13) 0.0146(5) Uani 1 1 d . . . C4 C 0.07506(9) 0.50211(16) 0.99046(13) 0.0180(5) Uani 1 1 d . . . H4 H 0.0505 0.5020 1.0099 0.022 Uiso 1 1 calc R . . C5 C 0.09715(9) 0.41881(16) 0.98293(13) 0.0186(5) Uani 1 1 d . . . H5 H 0.0876 0.3623 0.9970 0.022 Uiso 1 1 calc R . . C6 C 0.13280(9) 0.41913(16) 0.95507(13) 0.0171(5) Uani 1 1 d . . . H6 H 0.1478 0.3624 0.9499 0.021 Uiso 1 1 calc R . . C7 C 0.14737(9) 0.50265(15) 0.93408(12) 0.0145(5) Uani 1 1 d . . . C8 C 0.12555(9) 0.58804(16) 0.94092(12) 0.0148(5) Uani 1 1 d . . . C9 C 0.18608(9) 0.49643(16) 0.90728(12) 0.0153(5) Uani 1 1 d . . . H9 H 0.1971 0.4365 0.9012 0.018 Uiso 1 1 calc R . . C10 C 0.24474(9) 0.55050(15) 0.86167(13) 0.0165(5) Uani 1 1 d . . . H10A H 0.2201 0.5507 0.8014 0.020 Uiso 1 1 calc R . . H10B H 0.2652 0.4900 0.8810 0.020 Uiso 1 1 calc R . . C11 C 0.29025(10) 0.62798(15) 0.89484(14) 0.0180(5) Uani 1 1 d . . . H11A H 0.3232 0.6155 0.9523 0.022 Uiso 1 1 calc R . . H11B H 0.3073 0.6331 0.8628 0.022 Uiso 1 1 calc R . . C12 C 0.27377(9) 0.79036(16) 0.87237(13) 0.0157(5) Uani 1 1 d . . . H12 H 0.3023 0.7881 0.8596 0.019 Uiso 1 1 calc R . . C13 C 0.25002(9) 0.87961(15) 0.87150(13) 0.0139(5) Uani 1 1 d . . . C14 C 0.26799(9) 0.95484(16) 0.84559(13) 0.0176(5) Uani 1 1 d . . . H14 H 0.2923 0.9443 0.8266 0.021 Uiso 1 1 calc R . . C15 C 0.25069(9) 1.04266(16) 0.84758(13) 0.0192(5) Uani 1 1 d . . . H15 H 0.2619 1.0927 0.8284 0.023 Uiso 1 1 calc R . . C16 C 0.21650(9) 1.05880(16) 0.87774(13) 0.0172(5) Uani 1 1 d . . . H16 H 0.2060 1.1202 0.8813 0.021 Uiso 1 1 calc R . . C17 C 0.19784(9) 0.98650(16) 0.90233(12) 0.0143(5) Uani 1 1 d . . . C18 C 0.21275(9) 0.89343(16) 0.89826(13) 0.0148(5) Uani 1 1 d . . . C19 C 0.15094(10) 1.08962(16) 0.94310(15) 0.0210(5) Uani 1 1 d . . . H19A H 0.1297 1.1238 0.8909 0.025 Uiso 1 1 calc R . . H19B H 0.1887 1.1222 0.9826 0.025 Uiso 1 1 calc R . . C20 C 0.11268(11) 1.08373(19) 0.97490(16) 0.0305(6) Uani 1 1 d . . . H20A H 0.0751 1.0523 0.9348 0.046 Uiso 1 1 calc R . . H20B H 0.1041 1.1461 0.9845 0.046 Uiso 1 1 calc R . . H20C H 0.1339 1.0489 1.0261 0.046 Uiso 1 1 calc R . . C21 C 0.05671(11) 0.99282(18) 0.60927(15) 0.0306(6) Uani 1 1 d . . . H21A H 0.0644 0.9451 0.5817 0.046 Uiso 1 1 calc R . . H21B H 0.0667 1.0536 0.5986 0.046 Uiso 1 1 calc R . . H21C H 0.0144 0.9916 0.5888 0.046 Uiso 1 1 calc R . . C22 C 0.09453(10) 0.97466(15) 0.69951(14) 0.0186(5) Uani 1 1 d . . . H22A H 0.1372 0.9738 0.7197 0.022 Uiso 1 1 calc R . . H22B H 0.0888 1.0253 0.7276 0.022 Uiso 1 1 calc R . . C23 C 0.09906(9) 0.80845(15) 0.70266(13) 0.0137(5) Uani 1 1 d . . . C24 C 0.13845(9) 0.80587(16) 0.68088(13) 0.0169(5) Uani 1 1 d . . . H24 H 0.1550 0.8616 0.6770 0.020 Uiso 1 1 calc R . . C25 C 0.15423(10) 0.72132(17) 0.66446(14) 0.0197(5) Uani 1 1 d . . . H25 H 0.1807 0.7198 0.6481 0.024 Uiso 1 1 calc R . . C26 C 0.13163(10) 0.64094(16) 0.67199(13) 0.0184(5) Uani 1 1 d . . . H26 H 0.1427 0.5839 0.6608 0.022 Uiso 1 1 calc R . . C27 C 0.09220(9) 0.64091(15) 0.69607(13) 0.0146(5) Uani 1 1 d . . . C28 C 0.07470(9) 0.72616(16) 0.71010(13) 0.0138(5) Uani 1 1 d . . . C29 C 0.07083(9) 0.55287(16) 0.70338(12) 0.0165(5) Uani 1 1 d . . . H29 H 0.0841 0.4992 0.6909 0.020 Uiso 1 1 calc R . . C30 C 0.01310(10) 0.44821(15) 0.72495(13) 0.0193(5) Uani 1 1 d . . . H30A H 0.0463 0.4031 0.7482 0.023 Uiso 1 1 calc R . . H30B H -0.0180 0.4294 0.6683 0.023 Uiso 1 1 calc R . . C31 C 0.0000 1.0990(2) 0.7500 0.0292(8) Uani 1 2 d SDU . . C32A C 0.0000 1.2002(3) 0.7500 0.0239(14) Uani 0.42 2 d SPDU A 1 H32A H 0.0177 1.2228 0.8055 0.036 Uiso 0.21 1 calc PR A 1 H32B H -0.0411 1.2228 0.7142 0.036 Uiso 0.21 1 calc PR A 1 H32C H 0.0234 1.2228 0.7304 0.036 Uiso 0.21 1 calc PR A 1 H5A H 0.0777(11) 0.7921(13) 0.8973(14) 0.042(9) Uiso 1 1 d D . . H5B H 0.1073(8) 0.8644(17) 0.8928(14) 0.036(9) Uiso 1 1 d D . . C32B C 0.0023(4) 1.1954(3) 0.7746(5) 0.0239(14) Uani 0.29 1 d PDU A 2 H32D H 0.0145 1.1972 0.8310 0.036 Uiso 0.29 1 calc PR A 2 H32E H -0.0372 1.2236 0.7389 0.036 Uiso 0.29 1 calc PR A 2 H32F H 0.0313 1.2297 0.7701 0.036 Uiso 0.29 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 Cd1 0.01402(12) 0.00919(12) 0.01739(13) 0.000 0.01092(10) 0.000 Cu1 0.01491(14) 0.01272(15) 0.01695(15) 0.00164(11) 0.01131(12) -0.00030(11) Cu2 0.01490(19) 0.0093(2) 0.0173(2) 0.000 0.01048(16) 0.000 Cl1 0.0282(3) 0.0201(3) 0.0269(3) -0.0048(3) 0.0196(3) -0.0087(3) O1 0.0202(8) 0.0162(8) 0.0273(9) 0.0026(7) 0.0180(7) 0.0018(7) O2 0.0176(8) 0.0115(8) 0.0242(9) 0.0039(7) 0.0148(7) 0.0008(7) O3 0.0201(8) 0.0120(8) 0.0228(9) 0.0017(7) 0.0164(7) -0.0019(7) O4 0.0200(8) 0.0134(8) 0.0248(9) 0.0009(7) 0.0158(7) 0.0001(7) O5 0.0145(8) 0.0145(9) 0.0207(9) -0.0006(7) 0.0104(7) -0.0032(7) O6 0.0185(8) 0.0115(8) 0.0229(8) 0.0028(7) 0.0156(7) 0.0017(7) O7 0.0162(8) 0.0105(8) 0.0205(8) 0.0019(6) 0.0137(7) 0.0027(6) O8 0.0473(11) 0.0264(10) 0.0470(11) -0.0171(8) 0.0308(9) -0.0166(9) O9 0.0323(11) 0.0399(12) 0.0581(13) -0.0070(10) 0.0138(9) -0.0081(10) O10 0.0538(12) 0.0528(13) 0.0683(14) -0.0127(11) 0.0516(11) -0.0092(10) O11 0.0787(14) 0.0314(11) 0.0392(11) 0.0028(9) 0.0349(10) -0.0100(11) N1 0.0115(9) 0.0148(10) 0.0138(9) 0.0012(8) 0.0069(8) 0.0011(8) N2 0.0147(9) 0.0157(10) 0.0158(10) 0.0016(8) 0.0097(8) 0.0017(8) N3 0.0138(7) 0.0115(8) 0.0137(7) -0.0005(6) 0.0055(6) 0.0002(6) N4 0.0235(15) 0.0157(15) 0.0354(17) 0.000 0.0208(13) 0.000 C1 0.0309(14) 0.0286(15) 0.0368(16) -0.0041(12) 0.0233(13) 0.0022(12) C2 0.0198(12) 0.0262(13) 0.0210(13) -0.0020(10) 0.0150(10) -0.0014(11) C3 0.0130(11) 0.0152(12) 0.0124(11) 0.0011(9) 0.0054(9) -0.0001(9) C4 0.0149(11) 0.0227(13) 0.0164(11) 0.0008(10) 0.0091(9) -0.0031(10) C5 0.0191(12) 0.0147(12) 0.0188(12) 0.0018(10) 0.0091(10) -0.0051(10) C6 0.0139(11) 0.0157(12) 0.0155(11) -0.0007(9) 0.0047(9) -0.0004(9) C7 0.0117(10) 0.0148(12) 0.0120(11) -0.0004(9) 0.0040(9) -0.0016(9) C8 0.0097(11) 0.0193(13) 0.0092(11) 0.0016(9) 0.0018(9) -0.0014(9) C9 0.0138(11) 0.0153(12) 0.0104(11) 0.0002(9) 0.0032(9) 0.0012(9) C10 0.0180(11) 0.0172(12) 0.0166(11) 0.0020(9) 0.0113(10) 0.0047(10) C11 0.0168(12) 0.0200(13) 0.0216(12) 0.0051(10) 0.0135(10) 0.0049(10) C12 0.0132(11) 0.0210(13) 0.0149(11) 0.0015(10) 0.0092(9) -0.0013(10) C13 0.0109(11) 0.0161(12) 0.0127(11) 0.0011(9) 0.0056(9) -0.0013(9) C14 0.0135(11) 0.0225(13) 0.0171(12) 0.0021(10) 0.0090(9) -0.0040(10) C15 0.0154(11) 0.0207(13) 0.0206(12) 0.0031(10) 0.0098(10) -0.0058(10) C16 0.0139(11) 0.0147(12) 0.0189(12) 0.0001(10) 0.0069(9) -0.0008(9) C17 0.0108(10) 0.0199(12) 0.0111(11) 0.0000(9) 0.0056(9) -0.0008(9) C18 0.0118(11) 0.0176(12) 0.0116(11) 0.0020(9) 0.0047(9) -0.0035(9) C19 0.0212(12) 0.0148(12) 0.0287(14) 0.0021(10) 0.0153(11) 0.0025(10) C20 0.0297(14) 0.0295(15) 0.0394(16) 0.0019(12) 0.0240(13) 0.0074(12) C21 0.0351(14) 0.0274(15) 0.0329(14) 0.0140(12) 0.0216(12) 0.0099(12) C22 0.0214(12) 0.0121(12) 0.0291(13) -0.0005(10) 0.0184(11) -0.0024(10) C23 0.0135(11) 0.0142(12) 0.0131(11) 0.0024(9) 0.0074(9) 0.0040(9) C24 0.0143(11) 0.0197(13) 0.0173(12) 0.0031(10) 0.0094(10) 0.0015(10) C25 0.0169(12) 0.0266(13) 0.0212(12) 0.0023(11) 0.0142(10) 0.0050(10) C26 0.0169(12) 0.0213(13) 0.0160(12) -0.0015(10) 0.0089(10) 0.0077(10) C27 0.0126(11) 0.0155(12) 0.0117(11) 0.0007(9) 0.0047(9) 0.0025(9) C28 0.0112(11) 0.0188(12) 0.0112(11) 0.0015(9) 0.0064(9) 0.0028(9) C29 0.0158(11) 0.0156(12) 0.0130(11) -0.0015(9) 0.0053(9) 0.0066(10) C30 0.0193(12) 0.0100(11) 0.0245(13) -0.0031(9) 0.0101(10) 0.0003(10) C31 0.0247(11) 0.0272(12) 0.0341(12) 0.000 0.0160(9) 0.000 C32A 0.0241(15) 0.0230(15) 0.0241(17) 0.000 0.0135(10) 0.000 C32B 0.0241(15) 0.0230(15) 0.0241(17) 0.000 0.0135(10) 0.000 _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 Cd1 O7 2.2576(14) 2_556 ? Cd1 O7 2.2576(14) . ? Cd1 N4 2.285(3) . ? Cd1 O5 2.2895(16) 2_556 ? Cd1 O5 2.2895(16) . ? Cd1 O6 2.6049(14) 2_556 ? Cd1 O6 2.6049(14) . ? Cu1 O2 1.9176(15) . ? Cu1 O3 1.9240(16) . ? Cu1 N2 1.9379(18) . ? Cu1 N1 1.9512(19) . ? Cu2 O7 1.8888(15) 2_556 ? Cu2 O7 1.8888(15) . ? Cu2 N3 1.9079(18) . ? Cu2 N3 1.9079(18) 2_556 ? Cl1 O11 1.415(2) . ? Cl1 O10 1.4210(19) . ? Cl1 O8 1.4354(18) . ? Cl1 O9 1.436(2) . ? O1 C3 1.370(3) . ? O1 C2 1.433(3) . ? O2 C8 1.312(3) . ? O3 C18 1.329(3) . ? O4 C17 1.379(2) . ? O4 C19 1.443(3) . ? O5 H5A 0.831(17) . ? O5 H5B 0.818(16) . ? O6 C23 1.383(3) . ? O6 C22 1.444(3) . ? O7 C28 1.326(3) . ? N1 C9 1.287(3) . ? N1 C10 1.470(3) . ? N2 C12 1.276(3) . ? N2 C11 1.472(3) . ? N3 C29 1.287(3) . ? N3 C30 1.472(3) . ? N4 C31 1.135(4) . ? C1 C2 1.496(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.377(3) . ? C3 C8 1.433(3) . ? C4 C5 1.395(3) . ? C4 H4 0.9500 . ? C5 C6 1.373(3) . ? C5 H5 0.9500 . ? C6 C7 1.411(3) . ? C6 H6 0.9500 . ? C7 C8 1.413(3) . ? C7 C9 1.438(3) . ? C9 H9 0.9500 . ? C10 C11 1.517(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.442(3) . ? C12 H12 0.9500 . ? C13 C14 1.411(3) . ? C13 C18 1.411(3) . ? C14 C15 1.365(3) . ? C14 H14 0.9500 . ? C15 C16 1.393(3) . ? C15 H15 0.9500 . ? C16 C17 1.374(3) . ? C16 H16 0.9500 . ? C17 C18 1.424(3) . ? C19 C20 1.507(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.506(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.375(3) . ? C23 C28 1.414(3) . ? C24 C25 1.399(3) . ? C24 H24 0.9500 . ? C25 C26 1.366(3) . ? C25 H25 0.9500 . ? C26 C27 1.411(3) . ? C26 H26 0.9500 . ? C27 C28 1.409(3) . ? C27 C29 1.444(3) . ? C29 H29 0.9500 . ? C30 C30 1.532(5) 2_556 ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32A 1.465(3) . ? C31 C32B 1.469(3) . ? C31 C32B 1.469(3) 2_556 ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 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 O7 Cd1 O7 68.09(7) 2_556 . ? O7 Cd1 N4 145.95(4) 2_556 . ? O7 Cd1 N4 145.95(4) . . ? O7 Cd1 O5 86.92(6) 2_556 2_556 ? O7 Cd1 O5 83.85(6) . 2_556 ? N4 Cd1 O5 95.57(4) . 2_556 ? O7 Cd1 O5 83.85(6) 2_556 . ? O7 Cd1 O5 86.92(6) . . ? N4 Cd1 O5 95.57(4) . . ? O5 Cd1 O5 168.86(8) 2_556 . ? O7 Cd1 O6 64.04(5) 2_556 2_556 ? O7 Cd1 O6 131.90(5) . 2_556 ? N4 Cd1 O6 82.02(3) . 2_556 ? O5 Cd1 O6 89.13(5) 2_556 2_556 ? O5 Cd1 O6 92.42(5) . 2_556 ? O7 Cd1 O6 131.90(5) 2_556 . ? O7 Cd1 O6 64.04(5) . . ? N4 Cd1 O6 82.02(3) . . ? O5 Cd1 O6 92.42(5) 2_556 . ? O5 Cd1 O6 89.13(5) . . ? O6 Cd1 O6 164.04(7) 2_556 . ? O2 Cu1 O3 91.24(6) . . ? O2 Cu1 N2 176.14(7) . . ? O3 Cu1 N2 92.55(7) . . ? O2 Cu1 N1 92.39(7) . . ? O3 Cu1 N1 176.19(7) . . ? N2 Cu1 N1 83.80(8) . . ? O7 Cu2 O7 84.00(9) 2_556 . ? O7 Cu2 N3 177.98(7) 2_556 . ? O7 Cu2 N3 94.56(7) . . ? O7 Cu2 N3 94.57(7) 2_556 2_556 ? O7 Cu2 N3 177.98(7) . 2_556 ? N3 Cu2 N3 86.90(11) . 2_556 ? O11 Cl1 O10 111.54(14) . . ? O11 Cl1 O8 110.34(12) . . ? O10 Cl1 O8 109.13(12) . . ? O11 Cl1 O9 109.07(13) . . ? O10 Cl1 O9 107.95(14) . . ? O8 Cl1 O9 108.75(12) . . ? C3 O1 C2 116.91(18) . . ? C8 O2 Cu1 125.50(14) . . ? C18 O3 Cu1 125.80(14) . . ? C17 O4 C19 116.26(17) . . ? Cd1 O5 H5A 107.7(16) . . ? Cd1 O5 H5B 109.6(16) . . ? H5A O5 H5B 111(2) . . ? C23 O6 C22 116.84(16) . . ? C23 O6 Cd1 115.48(12) . . ? C22 O6 Cd1 126.26(12) . . ? C28 O7 Cu2 127.29(14) . . ? C28 O7 Cd1 128.67(14) . . ? Cu2 O7 Cd1 103.95(6) . . ? C9 N1 C10 119.83(19) . . ? C9 N1 Cu1 126.49(16) . . ? C10 N1 Cu1 113.57(14) . . ? C12 N2 C11 120.50(19) . . ? C12 N2 Cu1 126.69(16) . . ? C11 N2 Cu1 112.81(14) . . ? C29 N3 C30 120.63(19) . . ? C29 N3 Cu2 125.77(16) . . ? C30 N3 Cu2 113.32(14) . . ? C31 N4 Cd1 180.000(2) . . ? 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 . . ? O1 C2 C1 106.86(19) . . ? O1 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O1 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.6 . . ? O1 C3 C4 125.1(2) . . ? O1 C3 C8 113.38(19) . . ? C4 C3 C8 121.5(2) . . ? C3 C4 C5 120.8(2) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 119.5(2) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 120.8(2) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C8 120.9(2) . . ? C6 C7 C9 116.9(2) . . ? C8 C7 C9 122.2(2) . . ? O2 C8 C7 125.8(2) . . ? O2 C8 C3 117.7(2) . . ? C7 C8 C3 116.5(2) . . ? N1 C9 C7 125.0(2) . . ? N1 C9 H9 117.5 . . ? C7 C9 H9 117.5 . . ? N1 C10 C11 107.50(18) . . ? N1 C10 H10A 110.2 . . ? C11 C10 H10A 110.2 . . ? N1 C10 H10B 110.2 . . ? C11 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? N2 C11 C10 107.76(17) . . ? N2 C11 H11A 110.2 . . ? C10 C11 H11A 110.2 . . ? N2 C11 H11B 110.2 . . ? C10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? N2 C12 C13 125.1(2) . . ? N2 C12 H12 117.5 . . ? C13 C12 H12 117.5 . . ? C14 C13 C18 120.7(2) . . ? C14 C13 C12 116.6(2) . . ? C18 C13 C12 122.7(2) . . ? C15 C14 C13 120.6(2) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.9(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.5(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 O4 124.2(2) . . ? C16 C17 C18 121.6(2) . . ? O4 C17 C18 114.24(19) . . ? O3 C18 C13 124.5(2) . . ? O3 C18 C17 118.8(2) . . ? C13 C18 C17 116.7(2) . . ? O4 C19 C20 107.15(19) . . ? O4 C19 H19A 110.3 . . ? C20 C19 H19A 110.3 . . ? O4 C19 H19B 110.3 . . ? C20 C19 H19B 110.3 . . ? H19A C19 H19B 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O6 C22 C21 111.57(19) . . ? O6 C22 H22A 109.3 . . ? C21 C22 H22A 109.3 . . ? O6 C22 H22B 109.3 . . ? C21 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C24 C23 O6 125.3(2) . . ? C24 C23 C28 120.8(2) . . ? O6 C23 C28 113.92(19) . . ? C23 C24 C25 120.1(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.0(2) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 121.4(2) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C28 C27 C26 118.8(2) . . ? C28 C27 C29 123.4(2) . . ? C26 C27 C29 117.9(2) . . ? O7 C28 C27 123.3(2) . . ? O7 C28 C23 117.8(2) . . ? C27 C28 C23 118.9(2) . . ? N3 C29 C27 125.5(2) . . ? N3 C29 H29 117.2 . . ? C27 C29 H29 117.2 . . ? N3 C30 C30 110.04(12) . 2_556 ? N3 C30 H30A 109.7 . . ? C30 C30 H30A 109.7 2_556 . ? N3 C30 H30B 109.7 . . ? C30 C30 H30B 109.7 2_556 . ? H30A C30 H30B 108.2 . . ? N4 C31 C32A 180.000(3) . . ? N4 C31 C32B 161.8(3) . . ? N4 C31 C32B 161.8(3) . 2_556 ? C31 C32A H32A 109.5 . . ? C31 C32A H32B 109.5 . . ? C31 C32A H32C 109.5 . . ? C31 C32B H32D 109.5 . . ? C31 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 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 O5 H5A O1 0.831(17) 2.468(19) 3.217(2) 150(3) . O5 H5A O2 0.831(17) 2.25(2) 2.921(2) 138(2) . O5 H5B O3 0.818(16) 2.12(2) 2.840(2) 147(2) . O5 H5B O4 0.818(16) 2.28(2) 2.940(2) 138(2) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.520 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.059 #END=== data_3 _database_code_depnum_ccdc_archive 'CCDC 761687' #TrackingRef '- 1-4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H54 Cl2 Cu2 Hg2 N4 O18' _chemical_formula_sum 'C46 H54 Cl2 Cu2 Hg2 N4 O18' _chemical_formula_weight 1550.10 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' Cl Cl 0.1484 0.1585 '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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8064(5) _cell_length_b 19.7143(8) _cell_length_c 20.4235(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5156.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8102 _cell_measurement_theta_min 2.294 _cell_measurement_theta_max 30.492 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.997 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3016 _exptl_absorpt_coefficient_mu 6.931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6985 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (G. Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 6K CCD Detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57844 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5269 _reflns_number_gt 4592 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1999)' _computing_cell_refinement 'SAINT version 6.45A (Bruker, 2003)' _computing_data_reduction 'SAINT version 6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0201P)^2^+7.3096P] 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 5269 _refine_ls_number_parameters 346 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0493 _refine_ls_wR_factor_gt 0.0466 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.245703(7) -0.083614(5) 0.461707(5) 0.01643(4) Uani 1 1 d . . . Cu1 Cu 0.06442(3) 0.029470(16) 0.436095(15) 0.01551(7) Uani 1 1 d . . . Cl1 Cl 0.32882(5) 0.05521(3) 0.36155(3) 0.01938(13) Uani 1 1 d D . . O1 O 0.14835(16) -0.18960(10) 0.40207(9) 0.0231(4) Uani 1 1 d . . . O2 O 0.10804(14) -0.06039(9) 0.40885(9) 0.0161(4) Uani 1 1 d . . . O3 O 0.11713(14) 0.00856(9) 0.52190(9) 0.0166(4) Uani 1 1 d . . . O4 O 0.23024(15) -0.03279(11) 0.62258(9) 0.0223(4) Uani 1 1 d . . . O5 O 0.46384(18) -0.19145(11) 0.43749(12) 0.0359(5) Uani 1 1 d . . . O6A O 0.2911(6) 0.0508(5) 0.4287(4) 0.0269(12) Uani 0.52 1 d PDU A 1 O7A O 0.2909(5) 0.1062(4) 0.3176(4) 0.0314(11) Uani 0.52 1 d PDU A 1 O8A O 0.4379(6) 0.0677(5) 0.3746(4) 0.0347(12) Uani 0.52 1 d PDU A 1 O9 O 0.31736(18) -0.01156(10) 0.33344(10) 0.0307(5) Uani 1 1 d . A . N1 N 0.02237(18) 0.05279(12) 0.34724(11) 0.0184(5) Uani 1 1 d . . . N2 N 0.02617(18) 0.12085(12) 0.45733(10) 0.0173(5) Uani 1 1 d . . . C1 C 0.2079(3) -0.27822(16) 0.47023(17) 0.0322(7) Uani 1 1 d . . . H1A H 0.2726 -0.2531 0.4782 0.048 Uiso 1 1 calc R . . H1B H 0.2217 -0.3270 0.4732 0.048 Uiso 1 1 calc R . . H1C H 0.1557 -0.2655 0.5031 0.048 Uiso 1 1 calc R . . C2 C 0.1672(3) -0.26150(14) 0.40307(16) 0.0296(7) Uani 1 1 d . . . H2A H 0.2192 -0.2740 0.3693 0.036 Uiso 1 1 calc R . . H2B H 0.1018 -0.2866 0.3943 0.036 Uiso 1 1 calc R . . C3 C 0.1060(2) -0.16197(14) 0.34685(14) 0.0201(6) Uani 1 1 d . . . C4 C 0.0834(2) -0.19731(15) 0.29003(14) 0.0240(6) Uani 1 1 d . . . H4 H 0.1003 -0.2441 0.2867 0.029 Uiso 1 1 calc R . . C5 C 0.0357(2) -0.16416(15) 0.23758(14) 0.0247(6) Uani 1 1 d . . . H5 H 0.0196 -0.1884 0.1987 0.030 Uiso 1 1 calc R . . C6 C 0.0121(2) -0.09652(16) 0.24232(13) 0.0225(6) Uani 1 1 d . . . H6 H -0.0217 -0.0744 0.2068 0.027 Uiso 1 1 calc R . . C7 C 0.0371(2) -0.05923(15) 0.29918(13) 0.0182(5) Uani 1 1 d . . . C8 C 0.0848(2) -0.09181(14) 0.35203(13) 0.0169(5) Uani 1 1 d . . . C9 C 0.0116(2) 0.01252(14) 0.29876(13) 0.0178(6) Uani 1 1 d . . . H9 H -0.0153 0.0310 0.2592 0.021 Uiso 1 1 calc R . . C10 C 0.0012(2) 0.12577(14) 0.34068(14) 0.0233(6) Uani 1 1 d . . . H10A H -0.0517 0.1336 0.3061 0.028 Uiso 1 1 calc R . . H10B H 0.0659 0.1501 0.3284 0.028 Uiso 1 1 calc R . . C11 C -0.0390(2) 0.15164(14) 0.40631(14) 0.0206(6) Uani 1 1 d . . . H11A H -0.0339 0.2017 0.4083 0.025 Uiso 1 1 calc R . . H11B H -0.1130 0.1385 0.4124 0.025 Uiso 1 1 calc R . . C12 C 0.0554(2) 0.15318(14) 0.50816(13) 0.0180(5) Uani 1 1 d . . . H12 H 0.0349 0.1993 0.5118 0.022 Uiso 1 1 calc R . . C13 C 0.1176(2) 0.12494(14) 0.56085(13) 0.0181(5) Uani 1 1 d . . . C14 C 0.1476(2) 0.17052(14) 0.61064(14) 0.0223(6) Uani 1 1 d . . . H14 H 0.1282 0.2169 0.6073 0.027 Uiso 1 1 calc R . . C15 C 0.2040(2) 0.14928(16) 0.66353(14) 0.0250(6) Uani 1 1 d . . . H15 H 0.2234 0.1806 0.6967 0.030 Uiso 1 1 calc R . . C16 C 0.2330(2) 0.08108(15) 0.66847(15) 0.0219(6) Uani 1 1 d . . . H16 H 0.2723 0.0663 0.7052 0.026 Uiso 1 1 calc R . . C17 C 0.2052(2) 0.03511(14) 0.62080(13) 0.0181(6) Uani 1 1 d . . . C18 C 0.1460(2) 0.05577(14) 0.56497(12) 0.0153(5) Uani 1 1 d . . . C19 C 0.2923(3) -0.05406(17) 0.67748(14) 0.0275(7) Uani 1 1 d . . . H19A H 0.2579 -0.0401 0.7187 0.033 Uiso 1 1 calc R . . H19B H 0.3617 -0.0320 0.6755 0.033 Uiso 1 1 calc R . . C20 C 0.3054(3) -0.12984(18) 0.67663(15) 0.0331(8) Uani 1 1 d . . . H20A H 0.2366 -0.1515 0.6750 0.050 Uiso 1 1 calc R . . H20B H 0.3423 -0.1443 0.7163 0.050 Uiso 1 1 calc R . . H20C H 0.3460 -0.1431 0.6380 0.050 Uiso 1 1 calc R . . C21 C 0.3813(2) -0.11389(15) 0.50854(14) 0.0205(6) Uani 1 1 d . . . H21A H 0.4083 -0.0761 0.5356 0.025 Uiso 1 1 calc R . . H21B H 0.3658 -0.1525 0.5379 0.025 Uiso 1 1 calc R . . C22 C 0.4619(2) -0.13439(15) 0.46001(13) 0.0207(6) Uani 1 1 d . . . C23 C 0.5408(2) -0.08229(16) 0.44062(16) 0.0275(7) Uani 1 1 d . . . H23A H 0.5850 -0.1004 0.4056 0.041 Uiso 1 1 calc R . . H23B H 0.5842 -0.0708 0.4785 0.041 Uiso 1 1 calc R . . H23C H 0.5049 -0.0415 0.4250 0.041 Uiso 1 1 calc R . . O7B O 0.2611(5) 0.1022(5) 0.3270(4) 0.0314(11) Uani 0.48 1 d PDU A 2 O6B O 0.2701(7) 0.0597(6) 0.4224(4) 0.0269(12) Uani 0.48 1 d PDU A 2 O8B O 0.4347(7) 0.0762(6) 0.3601(5) 0.0347(12) Uani 0.48 1 d PDU 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 Hg1 0.01429(7) 0.01743(7) 0.01758(6) -0.00026(4) -0.00136(4) 0.00141(4) Cu1 0.01815(16) 0.01521(15) 0.01316(15) -0.00050(13) -0.00092(13) 0.00145(13) Cl1 0.0207(3) 0.0202(3) 0.0172(3) -0.0007(3) 0.0005(3) 0.0001(3) O1 0.0288(11) 0.0170(10) 0.0234(10) -0.0019(8) -0.0058(9) 0.0025(8) O2 0.0154(9) 0.0186(9) 0.0142(9) -0.0025(7) -0.0024(7) 0.0021(7) O3 0.0161(9) 0.0191(10) 0.0145(9) -0.0032(7) -0.0020(7) 0.0004(7) O4 0.0233(10) 0.0282(12) 0.0155(9) -0.0014(9) -0.0072(8) 0.0059(8) O5 0.0345(13) 0.0219(11) 0.0514(14) -0.0070(11) 0.0104(11) 0.0043(10) O6A 0.029(2) 0.0279(19) 0.0235(14) -0.0030(13) 0.0026(15) 0.0004(17) O7A 0.035(2) 0.0288(13) 0.0302(17) 0.0017(12) -0.0060(18) 0.0020(18) O8A 0.0262(12) 0.040(2) 0.038(3) 0.0062(18) 0.0024(15) -0.0058(12) O9 0.0406(13) 0.0222(11) 0.0294(11) -0.0063(9) 0.0068(10) 0.0002(10) N1 0.0179(12) 0.0195(12) 0.0179(11) 0.0025(9) 0.0026(9) 0.0015(9) N2 0.0171(12) 0.0170(11) 0.0179(11) 0.0020(9) 0.0020(9) -0.0005(9) C1 0.0309(18) 0.0190(16) 0.047(2) 0.0003(14) -0.0086(15) 0.0053(13) C2 0.0338(17) 0.0153(14) 0.0397(18) -0.0066(13) -0.0062(14) 0.0047(13) C3 0.0156(14) 0.0239(15) 0.0209(14) -0.0034(11) -0.0001(11) -0.0007(11) C4 0.0240(15) 0.0231(15) 0.0248(15) -0.0083(12) 0.0029(12) -0.0001(12) C5 0.0253(15) 0.0325(17) 0.0163(13) -0.0110(12) 0.0010(12) -0.0036(12) C6 0.0167(14) 0.0362(17) 0.0145(13) -0.0034(12) -0.0007(11) 0.0012(12) C7 0.0128(13) 0.0257(14) 0.0160(13) -0.0029(11) 0.0045(10) -0.0013(11) C8 0.0130(12) 0.0220(14) 0.0159(13) -0.0038(11) 0.0001(10) -0.0012(10) C9 0.0133(13) 0.0260(15) 0.0141(12) 0.0018(11) 0.0011(10) -0.0007(11) C10 0.0284(15) 0.0205(15) 0.0210(14) 0.0067(12) -0.0002(12) 0.0031(12) C11 0.0225(15) 0.0165(13) 0.0229(14) 0.0009(11) -0.0012(12) 0.0023(11) C12 0.0153(13) 0.0156(13) 0.0231(14) 0.0005(11) 0.0046(11) -0.0014(10) C13 0.0138(13) 0.0215(14) 0.0192(13) -0.0016(11) 0.0042(11) -0.0036(11) C14 0.0219(15) 0.0199(14) 0.0250(15) -0.0047(11) 0.0051(12) -0.0044(11) C15 0.0227(15) 0.0308(16) 0.0216(14) -0.0083(13) 0.0025(12) -0.0075(13) C16 0.0170(14) 0.0330(17) 0.0158(13) -0.0042(12) 0.0005(11) -0.0027(12) C17 0.0105(13) 0.0264(15) 0.0173(13) -0.0020(11) 0.0026(10) -0.0011(11) C18 0.0111(12) 0.0203(13) 0.0145(12) -0.0022(11) 0.0026(10) -0.0030(10) C19 0.0273(16) 0.0396(18) 0.0155(14) 0.0046(13) -0.0067(12) 0.0019(14) C20 0.0372(19) 0.043(2) 0.0189(15) 0.0021(14) -0.0044(13) 0.0150(15) C21 0.0167(14) 0.0246(15) 0.0203(13) 0.0012(12) -0.0026(11) 0.0033(11) C22 0.0169(14) 0.0241(15) 0.0210(14) 0.0015(12) -0.0019(11) 0.0045(11) C23 0.0238(16) 0.0327(17) 0.0261(15) 0.0023(13) -0.0002(13) -0.0029(13) O7B 0.035(2) 0.0288(13) 0.0302(17) 0.0017(12) -0.0060(18) 0.0020(18) O6B 0.029(2) 0.0279(19) 0.0235(14) -0.0030(13) 0.0026(15) 0.0004(17) O8B 0.0262(12) 0.040(2) 0.038(3) 0.0062(18) 0.0024(15) -0.0058(12) _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 Hg1 C21 2.070(3) . ? Hg1 O2 2.1173(18) . ? Hg1 Cu1 3.2609(3) . ? Cu1 N2 1.917(2) . ? Cu1 O3 1.9226(18) . ? Cu1 O2 1.9390(18) . ? Cu1 N1 1.948(2) . ? Cl1 O8B 1.417(9) . ? Cl1 O7A 1.432(7) . ? Cl1 O8A 1.443(8) . ? Cl1 O9 1.444(2) . ? Cl1 O7B 1.452(7) . ? Cl1 O6B 1.455(8) . ? Cl1 O6A 1.456(8) . ? O1 C3 1.365(3) . ? O1 C2 1.438(3) . ? O2 C8 1.349(3) . ? O3 C18 1.333(3) . ? O4 C17 1.377(4) . ? O4 C19 1.437(3) . ? O5 C22 1.215(4) . ? N1 C9 1.276(4) . ? N1 C10 1.470(4) . ? N2 C12 1.274(4) . ? N2 C11 1.466(3) . ? C1 C2 1.504(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.384(4) . ? C3 C8 1.414(4) . ? C4 C5 1.396(4) . ? C4 H4 0.9500 . ? C5 C6 1.371(4) . ? C5 H5 0.9500 . ? C6 C7 1.411(4) . ? C6 H6 0.9500 . ? C7 C8 1.396(4) . ? C7 C9 1.452(4) . ? C9 H9 0.9500 . ? C10 C11 1.524(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.450(4) . ? C12 H12 0.9500 . ? C13 C14 1.410(4) . ? C13 C18 1.414(4) . ? C14 C15 1.365(4) . ? C14 H14 0.9500 . ? C15 C16 1.398(4) . ? C15 H15 0.9500 . ? C16 C17 1.377(4) . ? C16 H16 0.9500 . ? C17 C18 1.429(4) . ? C19 C20 1.503(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.487(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.494(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 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 C21 Hg1 O2 175.03(9) . . ? C21 Hg1 Cu1 150.27(8) . . ? O2 Hg1 Cu1 34.67(5) . . ? N2 Cu1 O3 94.88(9) . . ? N2 Cu1 O2 175.77(9) . . ? O3 Cu1 O2 87.97(8) . . ? N2 Cu1 N1 85.32(10) . . ? O3 Cu1 N1 175.40(9) . . ? O2 Cu1 N1 91.60(9) . . ? N2 Cu1 Hg1 142.02(7) . . ? O3 Cu1 Hg1 57.13(5) . . ? O2 Cu1 Hg1 38.40(5) . . ? N1 Cu1 Hg1 120.50(7) . . ? O7A Cl1 O8A 108.9(4) . . ? O8B Cl1 O9 110.8(5) . . ? O7A Cl1 O9 110.9(4) . . ? O8A Cl1 O9 109.1(4) . . ? O8B Cl1 O7B 112.0(5) . . ? O9 Cl1 O7B 109.1(4) . . ? O8B Cl1 O6B 119.6(6) . . ? O9 Cl1 O6B 110.1(4) . . ? O7B Cl1 O6B 93.9(5) . . ? O7A Cl1 O6A 121.3(4) . . ? O8A Cl1 O6A 99.1(5) . . ? O9 Cl1 O6A 106.6(4) . . ? C3 O1 C2 118.1(2) . . ? C8 O2 Cu1 127.07(17) . . ? C8 O2 Hg1 121.55(16) . . ? Cu1 O2 Hg1 106.93(8) . . ? C18 O3 Cu1 123.32(17) . . ? C17 O4 C19 115.7(2) . . ? C9 N1 C10 121.2(2) . . ? C9 N1 Cu1 127.3(2) . . ? C10 N1 Cu1 111.52(17) . . ? C12 N2 C11 122.6(2) . . ? C12 N2 Cu1 125.4(2) . . ? C11 N2 Cu1 111.95(17) . . ? 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 . . ? O1 C2 C1 106.7(2) . . ? O1 C2 H2A 110.4 . . ? C1 C2 H2A 110.4 . . ? O1 C2 H2B 110.4 . . ? C1 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? O1 C3 C4 125.1(3) . . ? O1 C3 C8 113.9(2) . . ? C4 C3 C8 121.0(3) . . ? C3 C4 C5 120.0(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 119.9(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 121.0(3) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C6 119.7(3) . . ? C8 C7 C9 123.4(2) . . ? C6 C7 C9 116.8(3) . . ? O2 C8 C7 123.4(2) . . ? O2 C8 C3 118.1(2) . . ? C7 C8 C3 118.4(2) . . ? N1 C9 C7 125.2(3) . . ? N1 C9 H9 117.4 . . ? C7 C9 H9 117.4 . . ? N1 C10 C11 108.0(2) . . ? N1 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? N1 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? N2 C11 C10 107.1(2) . . ? N2 C11 H11A 110.3 . . ? C10 C11 H11A 110.3 . . ? N2 C11 H11B 110.3 . . ? C10 C11 H11B 110.3 . . ? H11A C11 H11B 108.5 . . ? N2 C12 C13 125.0(3) . . ? N2 C12 H12 117.5 . . ? C13 C12 H12 117.5 . . ? C14 C13 C18 120.1(3) . . ? C14 C13 C12 116.1(3) . . ? C18 C13 C12 123.8(2) . . ? C15 C14 C13 121.3(3) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 119.5(3) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 120.9(3) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 O4 124.1(3) . . ? C16 C17 C18 120.9(3) . . ? O4 C17 C18 114.9(2) . . ? O3 C18 C13 124.2(2) . . ? O3 C18 C17 118.4(2) . . ? C13 C18 C17 117.3(2) . . ? O4 C19 C20 110.0(2) . . ? O4 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? O4 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 Hg1 110.66(19) . . ? C22 C21 H21A 109.5 . . ? Hg1 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? Hg1 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? O5 C22 C21 121.2(3) . . ? O5 C22 C23 121.5(3) . . ? C21 C22 C23 117.3(3) . . ? 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 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.740 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.092 #END=== data_4 _database_code_depnum_ccdc_archive 'CCDC 761688' #TrackingRef '- 1-4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H48 Ag2 Cu2 N4 O10, 2(C20 H22 Cu N2 O4), 2(Cl O4)' _chemical_formula_sum 'C80 H92 Ag2 Cl2 Cu4 N8 O26' _chemical_formula_weight 2122.42 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' Cl Cl 0.1484 0.1585 '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' Ag Ag -0.8971 1.1015 '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 14.3298(6) _cell_length_b 13.3337(6) _cell_length_c 22.3930(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.0450(10) _cell_angle_gamma 90.00 _cell_volume 4150.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9520 _cell_measurement_theta_min 2.166 _cell_measurement_theta_max 27.949 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 1.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (G. Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31297 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8483 _reflns_number_gt 6278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0314P)^2^+1.1805P] 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 8483 _refine_ls_number_parameters 560 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.213727(19) 0.85317(2) 0.042436(11) 0.02315(8) Uani 1 1 d D . . Cu1 Cu 0.38470(3) 1.01331(3) 0.004284(18) 0.02006(10) Uani 1 1 d . . . Cu2 Cu 0.05580(3) 0.99055(3) -0.055861(17) 0.01653(10) Uani 1 1 d . . . Cl1 Cl 0.85560(6) 0.62548(6) 0.15752(4) 0.02437(19) Uani 1 1 d . . . O1 O 0.31092(17) 0.70800(17) -0.06752(10) 0.0270(6) Uani 1 1 d . . . O2 O 0.33331(16) 0.89183(17) -0.03279(9) 0.0216(5) Uani 1 1 d . . . O3 O 0.45106(16) 0.93787(17) 0.07396(10) 0.0234(5) Uani 1 1 d . . . O4 O 0.52759(18) 0.8065(2) 0.15445(11) 0.0324(6) Uani 1 1 d . . . O5 O 0.34679(18) 0.7497(2) 0.06454(11) 0.0280(6) Uani 1 1 d D . . H5A H 0.350(2) 0.739(3) 0.0277(9) 0.042 Uiso 1 1 d D . . H5B H 0.3893(17) 0.793(2) 0.0782(15) 0.042 Uiso 1 1 d D . . O6 O 0.11402(16) 0.67281(16) 0.00399(10) 0.0221(5) Uani 1 1 d . . . O7 O 0.07480(15) 0.85223(16) -0.03986(9) 0.0179(5) Uani 1 1 d . . . O8 O 0.12874(16) 1.00920(16) 0.02684(9) 0.0196(5) Uani 1 1 d . . . O9 O 0.24766(16) 0.99594(17) 0.13381(10) 0.0232(5) Uani 1 1 d . . . O10 O 0.81868(18) 0.61264(18) 0.09229(10) 0.0298(6) Uani 1 1 d U . . O11 O 0.8256(2) 0.7209(2) 0.17658(12) 0.0500(8) Uani 1 1 d U . . O12 O 0.95849(18) 0.62254(19) 0.17233(12) 0.0348(6) Uani 1 1 d U . . O13 O 0.82042(19) 0.5467(2) 0.19008(11) 0.0408(7) Uani 1 1 d U . . N1 N 0.3160(2) 1.0929(2) -0.06450(13) 0.0224(6) Uani 1 1 d . . . N2 N 0.4396(2) 1.1386(2) 0.03887(13) 0.0268(7) Uani 1 1 d . . . N3 N -0.00964(19) 0.9731(2) -0.14075(12) 0.0185(6) Uani 1 1 d . . . N4 N 0.03641(19) 1.1321(2) -0.07119(11) 0.0176(6) Uani 1 1 d . . . C1 C 0.3655(3) 0.5459(3) -0.0339(2) 0.0493(12) Uani 1 1 d . . . H1A H 0.4329 0.5656 -0.0286 0.074 Uiso 1 1 calc R . . H1B H 0.3586 0.4741 -0.0431 0.074 Uiso 1 1 calc R . . H1C H 0.3454 0.5600 0.0041 0.074 Uiso 1 1 calc R . . C2 C 0.3036(3) 0.6044(3) -0.08605(18) 0.0353(10) Uani 1 1 d . . . H2A H 0.3265 0.5954 -0.1240 0.042 Uiso 1 1 calc R . . H2B H 0.2360 0.5815 -0.0941 0.042 Uiso 1 1 calc R . . C3 C 0.2676(2) 0.7777(3) -0.11086(15) 0.0242(8) Uani 1 1 d . . . C4 C 0.2133(3) 0.7559(3) -0.16945(16) 0.0328(9) Uani 1 1 d . . . H4 H 0.2015 0.6882 -0.1823 0.039 Uiso 1 1 calc R . . C5 C 0.1760(3) 0.8345(3) -0.20959(16) 0.0349(10) Uani 1 1 d . . . H5 H 0.1382 0.8199 -0.2497 0.042 Uiso 1 1 calc R . . C6 C 0.1931(2) 0.9314(3) -0.19183(16) 0.0318(9) Uani 1 1 d . . . H6 H 0.1683 0.9836 -0.2201 0.038 Uiso 1 1 calc R . . C7 C 0.2472(2) 0.9559(3) -0.13200(15) 0.0234(8) Uani 1 1 d . . . C8 C 0.2841(2) 0.8787(3) -0.09011(14) 0.0218(8) Uani 1 1 d . . . C9 C 0.2657(2) 1.0603(3) -0.11610(16) 0.0258(8) Uani 1 1 d . . . H9 H 0.2382 1.1087 -0.1464 0.031 Uiso 1 1 calc R . . C10 C 0.3285(3) 1.2013(3) -0.05260(18) 0.0320(9) Uani 1 1 d . . . H10A H 0.2754 1.2271 -0.0357 0.038 Uiso 1 1 calc R . . H10B H 0.3269 1.2372 -0.0915 0.038 Uiso 1 1 calc R . . C11 C 0.4238(3) 1.2193(3) -0.00716(17) 0.0324(9) Uani 1 1 d . . . H11A H 0.4764 1.2198 -0.0288 0.039 Uiso 1 1 calc R . . H11B H 0.4230 1.2851 0.0132 0.039 Uiso 1 1 calc R . . C12 C 0.4876(3) 1.1538(3) 0.09421(17) 0.0314(9) Uani 1 1 d . . . H12 H 0.5059 1.2209 0.1058 0.038 Uiso 1 1 calc R . . C13 C 0.5160(2) 1.0774(3) 0.14003(16) 0.0308(9) Uani 1 1 d . . . C14 C 0.5686(3) 1.1068(4) 0.19979(18) 0.0406(11) Uani 1 1 d . . . H14 H 0.5789 1.1761 0.2089 0.049 Uiso 1 1 calc R . . C15 C 0.6045(3) 1.0375(4) 0.24436(19) 0.0473(12) Uani 1 1 d . . . H15 H 0.6380 1.0588 0.2843 0.057 Uiso 1 1 calc R . . C16 C 0.5919(3) 0.9356(4) 0.23111(16) 0.0407(11) Uani 1 1 d . . . H16 H 0.6177 0.8874 0.2619 0.049 Uiso 1 1 calc R . . C17 C 0.5420(3) 0.9044(3) 0.17337(15) 0.0318(9) Uani 1 1 d . . . C18 C 0.5001(2) 0.9744(3) 0.12684(15) 0.0263(8) Uani 1 1 d . . . C19 C 0.5741(3) 0.7282(3) 0.19497(17) 0.0422(11) Uani 1 1 d . . . H19A H 0.5493 0.7265 0.2325 0.051 Uiso 1 1 calc R . . H19B H 0.6444 0.7400 0.2073 0.051 Uiso 1 1 calc R . . C20 C 0.5530(3) 0.6314(3) 0.16069(19) 0.0483(12) Uani 1 1 d . . . H20A H 0.4835 0.6193 0.1500 0.072 Uiso 1 1 calc R . . H20B H 0.5857 0.5764 0.1866 0.072 Uiso 1 1 calc R . . H20C H 0.5761 0.6348 0.1230 0.072 Uiso 1 1 calc R . . C21 C 0.1790(3) 0.5885(3) 0.09798(16) 0.0336(9) Uani 1 1 d . . . H21A H 0.2385 0.6274 0.1033 0.050 Uiso 1 1 calc R . . H21B H 0.1938 0.5225 0.1172 0.050 Uiso 1 1 calc R . . H21C H 0.1343 0.6239 0.1174 0.050 Uiso 1 1 calc R . . C22 C 0.1336(3) 0.5755(2) 0.03027(15) 0.0270(8) Uani 1 1 d . . . H22A H 0.1779 0.5389 0.0102 0.032 Uiso 1 1 calc R . . H22B H 0.0732 0.5365 0.0244 0.032 Uiso 1 1 calc R . . C23 C 0.0641(2) 0.6782(2) -0.05715(14) 0.0186(7) Uani 1 1 d . . . C24 C 0.0351(2) 0.5971(3) -0.09511(15) 0.0221(8) Uani 1 1 d . . . H24 H 0.0508 0.5310 -0.0801 0.027 Uiso 1 1 calc R . . C25 C -0.0174(3) 0.6119(3) -0.15575(15) 0.0260(8) Uani 1 1 d . . . H25 H -0.0377 0.5559 -0.1819 0.031 Uiso 1 1 calc R . . C26 C -0.0397(2) 0.7073(3) -0.17760(15) 0.0252(8) Uani 1 1 d . . . H26 H -0.0755 0.7165 -0.2189 0.030 Uiso 1 1 calc R . . C27 C -0.0105(2) 0.7916(2) -0.14005(14) 0.0188(7) Uani 1 1 d . . . C28 C 0.0435(2) 0.7780(2) -0.07852(14) 0.0182(7) Uani 1 1 d . . . C29 C -0.0320(2) 0.8892(3) -0.16773(14) 0.0197(7) Uani 1 1 d . . . H29 H -0.0657 0.8911 -0.2098 0.024 Uiso 1 1 calc R . . C30 C -0.0264(2) 1.0685(2) -0.17425(14) 0.0212(8) Uani 1 1 d . . . H30A H -0.0860 1.0644 -0.2076 0.025 Uiso 1 1 calc R . . H30B H 0.0280 1.0835 -0.1929 0.025 Uiso 1 1 calc R . . C31 C -0.0360(2) 1.1510(3) -0.12900(14) 0.0220(7) Uani 1 1 d . . . H31A H -0.0251 1.2175 -0.1458 0.026 Uiso 1 1 calc R . . H31B H -0.1014 1.1502 -0.1216 0.026 Uiso 1 1 calc R . . C32 C 0.0747(2) 1.2035(2) -0.03537(14) 0.0195(7) Uani 1 1 d . . . H32 H 0.0581 1.2703 -0.0486 0.023 Uiso 1 1 calc R . . C33 C 0.1417(2) 1.1898(3) 0.02402(14) 0.0189(7) Uani 1 1 d . . . C34 C 0.1830(2) 1.2774(3) 0.05565(15) 0.0247(8) Uani 1 1 d . . . H34 H 0.1669 1.3413 0.0372 0.030 Uiso 1 1 calc R . . C35 C 0.2456(3) 1.2712(3) 0.11232(16) 0.0288(9) Uani 1 1 d . . . H35 H 0.2732 1.3305 0.1328 0.035 Uiso 1 1 calc R . . C36 C 0.2690(2) 1.1779(3) 0.14008(15) 0.0258(8) Uani 1 1 d . . . H36 H 0.3119 1.1740 0.1797 0.031 Uiso 1 1 calc R . . C37 C 0.2306(2) 1.0918(3) 0.11079(14) 0.0194(7) Uani 1 1 d . . . C38 C 0.1656(2) 1.0954(2) 0.05173(14) 0.0174(7) Uani 1 1 d . . . C39 C 0.3051(2) 0.9866(3) 0.19599(14) 0.0268(8) Uani 1 1 d . . . H39A H 0.2734 1.0212 0.2249 0.032 Uiso 1 1 calc R . . H39B H 0.3692 1.0171 0.1997 0.032 Uiso 1 1 calc R . . C40 C 0.3151(3) 0.8763(3) 0.21078(16) 0.0314(9) Uani 1 1 d . . . H40A H 0.2513 0.8473 0.2079 0.047 Uiso 1 1 calc R . . H40B H 0.3551 0.8672 0.2526 0.047 Uiso 1 1 calc R . . H40C H 0.3454 0.8427 0.1814 0.047 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 Ag1 0.02167(15) 0.02496(15) 0.02179(13) 0.00233(12) 0.00326(10) 0.00444(12) Cu1 0.0188(2) 0.0195(2) 0.0224(2) -0.00068(18) 0.00596(17) 0.00160(18) Cu2 0.0191(2) 0.0157(2) 0.01479(19) 0.00086(16) 0.00398(16) 0.00054(17) Cl1 0.0297(5) 0.0198(5) 0.0212(4) -0.0022(3) 0.0015(4) 0.0027(4) O1 0.0311(15) 0.0223(14) 0.0274(13) -0.0079(11) 0.0063(11) -0.0037(11) O2 0.0221(13) 0.0235(13) 0.0173(11) 0.0000(10) 0.0015(10) 0.0005(11) O3 0.0232(13) 0.0256(13) 0.0182(12) -0.0013(10) -0.0012(10) 0.0018(11) O4 0.0292(15) 0.0442(17) 0.0217(12) 0.0099(12) 0.0021(11) 0.0080(13) O5 0.0258(14) 0.0299(15) 0.0278(13) 0.0008(12) 0.0057(11) 0.0039(11) O6 0.0268(14) 0.0153(12) 0.0223(12) 0.0024(10) 0.0018(10) -0.0001(10) O7 0.0212(13) 0.0138(11) 0.0169(11) -0.0011(9) 0.0011(9) -0.0007(10) O8 0.0229(13) 0.0159(12) 0.0184(11) -0.0010(10) 0.0022(10) -0.0001(10) O9 0.0243(13) 0.0249(14) 0.0175(11) 0.0007(10) -0.0006(10) 0.0005(11) O10 0.0413(15) 0.0239(12) 0.0215(11) -0.0001(10) 0.0022(10) 0.0018(11) O11 0.0595(17) 0.0390(15) 0.0419(14) -0.0182(13) -0.0065(13) 0.0213(13) O12 0.0283(14) 0.0316(14) 0.0425(14) -0.0004(12) 0.0046(11) -0.0033(11) O13 0.0424(15) 0.0516(16) 0.0283(13) 0.0054(12) 0.0084(11) -0.0154(13) N1 0.0208(16) 0.0210(16) 0.0300(16) 0.0068(13) 0.0148(13) 0.0046(13) N2 0.0231(17) 0.0249(17) 0.0369(18) -0.0050(14) 0.0161(14) -0.0013(14) N3 0.0182(15) 0.0201(15) 0.0182(14) 0.0040(12) 0.0062(12) 0.0028(12) N4 0.0182(15) 0.0186(15) 0.0175(13) 0.0001(12) 0.0075(11) 0.0003(12) C1 0.039(3) 0.024(2) 0.081(3) -0.011(2) 0.006(2) 0.000(2) C2 0.034(2) 0.024(2) 0.050(2) -0.0188(19) 0.0127(19) -0.0066(18) C3 0.0169(18) 0.031(2) 0.0261(18) -0.0044(16) 0.0076(15) -0.0018(16) C4 0.025(2) 0.046(3) 0.029(2) -0.0148(19) 0.0115(17) -0.0083(19) C5 0.022(2) 0.062(3) 0.0203(18) -0.0084(19) 0.0041(16) -0.003(2) C6 0.0173(19) 0.056(3) 0.0221(18) 0.0041(18) 0.0045(15) 0.0100(19) C7 0.0129(18) 0.038(2) 0.0212(17) 0.0045(16) 0.0073(14) 0.0054(16) C8 0.0126(17) 0.035(2) 0.0183(16) 0.0003(15) 0.0050(14) 0.0007(15) C9 0.0163(19) 0.038(2) 0.0252(19) 0.0142(17) 0.0093(15) 0.0086(17) C10 0.032(2) 0.022(2) 0.049(2) 0.0091(18) 0.0247(19) 0.0051(17) C11 0.038(2) 0.021(2) 0.047(2) -0.0011(18) 0.0253(19) 0.0011(17) C12 0.026(2) 0.033(2) 0.042(2) -0.0175(19) 0.0216(18) -0.0082(18) C13 0.0173(19) 0.049(3) 0.029(2) -0.0149(18) 0.0118(16) -0.0048(18) C14 0.025(2) 0.066(3) 0.035(2) -0.024(2) 0.0174(18) -0.013(2) C15 0.026(2) 0.090(4) 0.028(2) -0.024(2) 0.0093(18) -0.014(2) C16 0.027(2) 0.076(3) 0.0196(19) -0.004(2) 0.0058(16) 0.002(2) C17 0.018(2) 0.058(3) 0.0200(18) 0.0007(19) 0.0062(15) 0.0027(19) C18 0.0139(18) 0.043(2) 0.0250(18) -0.0080(17) 0.0111(15) -0.0032(17) C19 0.030(2) 0.070(3) 0.028(2) 0.027(2) 0.0072(18) 0.009(2) C20 0.047(3) 0.051(3) 0.047(3) 0.030(2) 0.012(2) 0.012(2) C21 0.040(2) 0.024(2) 0.032(2) 0.0077(17) -0.0019(18) -0.0021(18) C22 0.029(2) 0.0173(19) 0.032(2) 0.0068(16) 0.0039(16) 0.0032(16) C23 0.0192(18) 0.0194(18) 0.0171(16) -0.0010(14) 0.0041(14) 0.0012(14) C24 0.0239(19) 0.0182(18) 0.0256(18) 0.0033(15) 0.0086(15) 0.0023(15) C25 0.031(2) 0.0222(19) 0.0238(18) -0.0080(15) 0.0040(16) 0.0002(16) C26 0.025(2) 0.030(2) 0.0202(17) -0.0038(16) 0.0033(15) 0.0013(16) C27 0.0192(18) 0.0183(18) 0.0199(16) -0.0004(14) 0.0066(14) 0.0021(15) C28 0.0153(18) 0.0205(18) 0.0203(16) -0.0016(14) 0.0074(14) -0.0005(14) C29 0.0191(18) 0.0257(19) 0.0132(15) -0.0017(14) 0.0015(13) 0.0020(15) C30 0.0244(19) 0.0227(19) 0.0159(16) 0.0020(14) 0.0042(14) 0.0020(15) C31 0.0186(18) 0.0237(19) 0.0232(17) 0.0079(15) 0.0039(14) 0.0025(15) C32 0.0205(19) 0.0150(17) 0.0263(17) 0.0014(15) 0.0123(15) 0.0025(14) C33 0.0150(18) 0.0214(18) 0.0227(17) -0.0019(15) 0.0095(14) 0.0003(14) C34 0.029(2) 0.0178(19) 0.0298(19) -0.0041(15) 0.0124(16) -0.0045(16) C35 0.031(2) 0.025(2) 0.032(2) -0.0137(17) 0.0086(17) -0.0030(17) C36 0.022(2) 0.032(2) 0.0220(17) -0.0097(16) 0.0024(15) -0.0018(16) C37 0.0197(18) 0.0227(19) 0.0166(16) -0.0027(14) 0.0059(14) 0.0007(15) C38 0.0158(17) 0.0194(18) 0.0188(16) -0.0043(14) 0.0079(14) -0.0028(14) C39 0.0214(19) 0.044(2) 0.0147(16) -0.0032(16) 0.0041(14) -0.0012(17) C40 0.024(2) 0.047(3) 0.0206(18) 0.0075(17) -0.0001(15) 0.0030(18) _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 Ag1 O5 2.308(3) . ? Ag1 O7 2.362(2) . ? Ag1 O8 2.393(2) . ? Cu1 O2 1.886(2) . ? Cu1 O3 1.905(2) . ? Cu1 N2 1.928(3) . ? Cu1 N1 1.932(3) . ? Cu2 O7 1.886(2) . ? Cu2 O8 1.909(2) . ? Cu2 N3 1.919(3) . ? Cu2 N4 1.927(3) . ? Cl1 O12 1.431(3) . ? Cl1 O10 1.438(2) . ? Cl1 O13 1.438(3) . ? Cl1 O11 1.440(3) . ? O1 C3 1.378(4) . ? O1 C2 1.439(4) . ? O2 C8 1.318(4) . ? O3 C18 1.315(4) . ? O4 C17 1.372(5) . ? O4 C19 1.436(4) . ? O5 H5A 0.852(18) . ? O5 H5B 0.841(18) . ? O6 C23 1.384(4) . ? O6 C22 1.425(4) . ? O7 C28 1.320(4) . ? O8 C38 1.329(4) . ? O9 C37 1.377(4) . ? O9 C39 1.441(4) . ? N1 C9 1.280(4) . ? N1 C10 1.473(4) . ? N2 C12 1.279(4) . ? N2 C11 1.469(4) . ? N3 C29 1.275(4) . ? N3 C30 1.467(4) . ? N4 C32 1.280(4) . ? N4 C31 1.471(4) . ? C1 C2 1.501(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.384(5) . ? C3 C8 1.425(5) . ? C4 C5 1.400(5) . ? C4 H4 0.9500 . ? C5 C6 1.356(5) . ? C5 H5 0.9500 . ? C6 C7 1.414(5) . ? C6 H6 0.9500 . ? C7 C8 1.407(5) . ? C7 C9 1.445(5) . ? C9 H9 0.9500 . ? C10 C11 1.512(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.433(5) . ? C12 H12 0.9500 . ? C13 C18 1.412(5) . ? C13 C14 1.422(5) . ? C14 C15 1.366(6) . ? C14 H14 0.9500 . ? C15 C16 1.393(6) . ? C15 H15 0.9500 . ? C16 C17 1.381(5) . ? C16 H16 0.9500 . ? C17 C18 1.420(5) . ? C19 C20 1.496(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.508(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.376(4) . ? C23 C28 1.420(4) . ? C24 C25 1.398(5) . ? C24 H24 0.9500 . ? C25 C26 1.372(5) . ? C25 H25 0.9500 . ? C26 C27 1.406(4) . ? C26 H26 0.9500 . ? C27 C28 1.419(4) . ? C27 C29 1.441(4) . ? C29 H29 0.9500 . ? C30 C31 1.524(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.451(4) . ? C32 H32 0.9500 . ? C33 C38 1.408(5) . ? C33 C34 1.420(5) . ? C34 C35 1.367(5) . ? C34 H34 0.9500 . ? C35 C36 1.395(5) . ? C35 H35 0.9500 . ? C36 C37 1.370(5) . ? C36 H36 0.9500 . ? C37 C38 1.422(4) . ? C39 C40 1.506(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 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 O5 Ag1 O7 131.32(8) . . ? O5 Ag1 O8 156.31(8) . . ? O7 Ag1 O8 65.67(7) . . ? O2 Cu1 O3 88.34(9) . . ? O2 Cu1 N2 177.31(11) . . ? O3 Cu1 N2 93.13(11) . . ? O2 Cu1 N1 92.96(11) . . ? O3 Cu1 N1 178.05(11) . . ? N2 Cu1 N1 85.62(13) . . ? O7 Cu2 O8 85.60(9) . . ? O7 Cu2 N3 94.76(10) . . ? O8 Cu2 N3 176.14(10) . . ? O7 Cu2 N4 179.31(10) . . ? O8 Cu2 N4 93.81(10) . . ? N3 Cu2 N4 85.85(11) . . ? O12 Cl1 O10 109.67(15) . . ? O12 Cl1 O13 109.31(16) . . ? O10 Cl1 O13 109.88(15) . . ? O12 Cl1 O11 108.70(17) . . ? O10 Cl1 O11 110.09(15) . . ? O13 Cl1 O11 109.17(18) . . ? C3 O1 C2 117.1(3) . . ? C8 O2 Cu1 127.0(2) . . ? C18 O3 Cu1 126.4(2) . . ? C17 O4 C19 118.9(3) . . ? Ag1 O5 H5A 98(2) . . ? Ag1 O5 H5B 99(2) . . ? H5A O5 H5B 105(3) . . ? C23 O6 C22 117.3(3) . . ? C28 O7 Cu2 126.77(19) . . ? C28 O7 Ag1 127.12(19) . . ? Cu2 O7 Ag1 101.45(9) . . ? C38 O8 Cu2 126.0(2) . . ? C38 O8 Ag1 123.64(19) . . ? Cu2 O8 Ag1 99.65(9) . . ? C37 O9 C39 116.7(3) . . ? C9 N1 C10 120.9(3) . . ? C9 N1 Cu1 126.8(3) . . ? C10 N1 Cu1 112.3(2) . . ? C12 N2 C11 121.3(3) . . ? C12 N2 Cu1 126.7(3) . . ? C11 N2 Cu1 112.0(2) . . ? C29 N3 C30 121.9(3) . . ? C29 N3 Cu2 125.6(2) . . ? C30 N3 Cu2 112.4(2) . . ? C32 N4 C31 121.9(3) . . ? C32 N4 Cu2 126.6(2) . . ? C31 N4 Cu2 111.4(2) . . ? 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 . . ? O1 C2 C1 106.6(3) . . ? O1 C2 H2A 110.4 . . ? C1 C2 H2A 110.4 . . ? O1 C2 H2B 110.4 . . ? C1 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? O1 C3 C4 125.4(3) . . ? O1 C3 C8 113.4(3) . . ? C4 C3 C8 121.2(3) . . ? C3 C4 C5 119.4(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 120.7(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 121.1(4) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 119.6(3) . . ? C8 C7 C9 121.6(3) . . ? C6 C7 C9 118.8(3) . . ? O2 C8 C7 125.3(3) . . ? O2 C8 C3 116.7(3) . . ? C7 C8 C3 117.9(3) . . ? N1 C9 C7 125.3(3) . . ? N1 C9 H9 117.3 . . ? C7 C9 H9 117.3 . . ? N1 C10 C11 109.2(3) . . ? N1 C10 H10A 109.8 . . ? C11 C10 H10A 109.8 . . ? N1 C10 H10B 109.8 . . ? C11 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? N2 C11 C10 108.4(3) . . ? N2 C11 H11A 110.0 . . ? C10 C11 H11A 110.0 . . ? N2 C11 H11B 110.0 . . ? C10 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? N2 C12 C13 125.0(4) . . ? N2 C12 H12 117.5 . . ? C13 C12 H12 117.5 . . ? C18 C13 C14 119.1(4) . . ? C18 C13 C12 122.6(3) . . ? C14 C13 C12 118.1(4) . . ? C15 C14 C13 121.4(4) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 119.8(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.3(4) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? O4 C17 C16 125.5(4) . . ? O4 C17 C18 113.2(3) . . ? C16 C17 C18 121.3(4) . . ? O3 C18 C13 125.0(3) . . ? O3 C18 C17 117.1(3) . . ? C13 C18 C17 117.9(3) . . ? O4 C19 C20 107.3(3) . . ? O4 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O4 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O6 C22 C21 107.7(3) . . ? O6 C22 H22A 110.2 . . ? C21 C22 H22A 110.2 . . ? O6 C22 H22B 110.2 . . ? C21 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? C24 C23 O6 125.2(3) . . ? C24 C23 C28 121.4(3) . . ? O6 C23 C28 113.4(3) . . ? C23 C24 C25 120.0(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.1(3) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 121.2(3) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C26 C27 C28 119.4(3) . . ? C26 C27 C29 117.6(3) . . ? C28 C27 C29 122.9(3) . . ? O7 C28 C27 124.0(3) . . ? O7 C28 C23 118.2(3) . . ? C27 C28 C23 117.9(3) . . ? N3 C29 C27 125.8(3) . . ? N3 C29 H29 117.1 . . ? C27 C29 H29 117.1 . . ? N3 C30 C31 108.4(2) . . ? N3 C30 H30A 110.0 . . ? C31 C30 H30A 110.0 . . ? N3 C30 H30B 110.0 . . ? C31 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? N4 C31 C30 107.7(3) . . ? N4 C31 H31A 110.2 . . ? C30 C31 H31A 110.2 . . ? N4 C31 H31B 110.2 . . ? C30 C31 H31B 110.2 . . ? H31A C31 H31B 108.5 . . ? N4 C32 C33 124.6(3) . . ? N4 C32 H32 117.7 . . ? C33 C32 H32 117.7 . . ? C38 C33 C34 119.3(3) . . ? C38 C33 C32 123.6(3) . . ? C34 C33 C32 117.1(3) . . ? C35 C34 C33 120.9(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 120.0(3) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 120.6(3) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 O9 125.8(3) . . ? C36 C37 C38 120.9(3) . . ? O9 C37 C38 113.4(3) . . ? O8 C38 C33 124.0(3) . . ? O8 C38 C37 117.7(3) . . ? C33 C38 C37 118.3(3) . . ? O9 C39 C40 107.4(3) . . ? O9 C39 H39A 110.2 . . ? C40 C39 H39A 110.2 . . ? O9 C39 H39B 110.2 . . ? C40 C39 H39B 110.2 . . ? H39A C39 H39B 108.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 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 O5 H5A O1 0.852(18) 2.11(2) 2.929(3) 161(3) . O5 H5A O2 0.852(18) 2.43(3) 2.859(3) 112(3) . O5 H5B O3 0.841(18) 2.14(2) 2.902(3) 151(3) . O5 H5B O4 0.841(18) 2.29(2) 2.968(3) 138(3) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.476 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.091