Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Paul Kelly' _publ_contact_author_address ; Department of Chemistry Loughborough University Loughborough Leicestershire LE11 3TU UNITED KINGDOM ; _publ_contact_author_email P.F.KELLY@LBORO.AC.UK _publ_section_title ; New Observations of Structural Diversity in Copper(II) Complexes of Diphenylsulfimide. ; loop_ _publ_author_name 'Paul Kelly' 'Sophie Dale' 'Mark R. J. Elsegood' 'Kathryn E. Holmes' data_(2) _database_code_depnum_ccdc_archive 'CCDC 227319' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H58 B2 Cu F8 N6 S5' _chemical_formula_weight 1284.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.1040(4) _cell_length_b 12.3528(5) _cell_length_c 12.8493(5) _cell_angle_alpha 112.138(2) _cell_angle_beta 98.411(2) _cell_angle_gamma 103.464(2) _cell_volume 1533.17(10) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11540 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.94 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.57 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 663 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.865 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13667 _diffrn_reflns_av_R_equivalents 0.0090 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.94 _reflns_number_total 12186 _reflns_number_gt 11744 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0361P)^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 except NH coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.700(5) _refine_ls_number_reflns 12186 _refine_ls_number_parameters 774 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.032 _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 0.270265(16) 0.221077(16) 0.778544(15) 0.01719(5) Uani 1 1 d . . . N1 N 0.18077(14) 0.11574(14) 0.85029(13) 0.0210(3) Uani 1 1 d D . . H1A H 0.157(2) 0.0436(14) 0.8121(18) 0.031 Uiso 1 1 d D . . S1 S 0.22714(4) 0.13901(4) 0.98221(4) 0.01984(9) Uani 1 1 d . . . C1 C 0.33550(18) 0.05434(18) 0.99402(16) 0.0252(4) Uani 1 1 d . . . C2 C 0.2953(2) -0.07256(19) 0.95037(18) 0.0316(4) Uani 1 1 d . . . H2 H 0.2066 -0.1179 0.9189 0.038 Uiso 1 1 calc R . . C3 C 0.3857(2) -0.1332(2) 0.9530(2) 0.0402(5) Uani 1 1 d . . . H3 H 0.3590 -0.2203 0.9247 0.048 Uiso 1 1 calc R . . C4 C 0.5141(2) -0.0666(3) 0.99674(19) 0.0453(6) Uani 1 1 d . . . H4 H 0.5759 -0.1084 0.9969 0.054 Uiso 1 1 calc R . . C5 C 0.5540(2) 0.0600(2) 1.04028(19) 0.0433(6) Uani 1 1 d . . . H5 H 0.6428 0.1050 1.0714 0.052 Uiso 1 1 calc R . . C6 C 0.46445(19) 0.1218(2) 1.03868(18) 0.0343(4) Uani 1 1 d . . . H6 H 0.4913 0.2089 1.0678 0.041 Uiso 1 1 calc R . . C7 C 0.09452(17) 0.05870(17) 1.01768(16) 0.0226(4) Uani 1 1 d . . . C8 C 0.1082(2) 0.0741(2) 1.13199(18) 0.0371(5) Uani 1 1 d . . . H8 H 0.1860 0.1259 1.1897 0.044 Uiso 1 1 calc R . . C9 C 0.0061(2) 0.0126(2) 1.16050(19) 0.0451(6) Uani 1 1 d . . . H9 H 0.0140 0.0224 1.2384 0.054 Uiso 1 1 calc R . . C10 C -0.1062(2) -0.0624(2) 1.0769(2) 0.0360(5) Uani 1 1 d . . . H10 H -0.1754 -0.1041 1.0975 0.043 Uiso 1 1 calc R . . C11 C -0.11916(19) -0.07754(19) 0.96412(19) 0.0322(4) Uani 1 1 d . . . H11 H -0.1970 -0.1299 0.9068 0.039 Uiso 1 1 calc R . . C12 C -0.01810(18) -0.01610(18) 0.93318(17) 0.0275(4) Uani 1 1 d . . . H12 H -0.0268 -0.0257 0.8553 0.033 Uiso 1 1 calc R . . N2 N 0.30947(15) 0.07018(14) 0.67818(14) 0.0239(3) Uani 1 1 d D . . H2A H 0.266(2) 0.0030(15) 0.666(2) 0.036 Uiso 1 1 d D . . S2 S 0.40866(4) 0.05945(4) 0.60061(4) 0.01994(9) Uani 1 1 d . . . C13 C 0.49511(16) -0.03997(16) 0.62227(15) 0.0215(4) Uani 1 1 d . . . C14 C 0.4654(2) -0.10047(19) 0.69112(17) 0.0302(4) Uani 1 1 d . . . H14 H 0.3964 -0.0928 0.7262 0.036 Uiso 1 1 calc R . . C15 C 0.5388(2) -0.17287(19) 0.70784(18) 0.0350(5) Uani 1 1 d . . . H15 H 0.5190 -0.2161 0.7538 0.042 Uiso 1 1 calc R . . C16 C 0.64034(19) -0.18208(19) 0.65777(18) 0.0335(5) Uani 1 1 d . . . H16 H 0.6903 -0.2313 0.6698 0.040 Uiso 1 1 calc R . . C17 C 0.66939(18) -0.12009(19) 0.59041(19) 0.0326(4) Uani 1 1 d . . . H17 H 0.7397 -0.1263 0.5568 0.039 Uiso 1 1 calc R . . C18 C 0.59690(17) -0.04918(18) 0.57156(17) 0.0267(4) Uani 1 1 d . . . H18 H 0.6163 -0.0072 0.5245 0.032 Uiso 1 1 calc R . . C19 C 0.32634(17) -0.03289(17) 0.44956(16) 0.0243(4) Uani 1 1 d . . . C20 C 0.3776(2) 0.0000(2) 0.36959(17) 0.0337(4) Uani 1 1 d . . . H20 H 0.4532 0.0682 0.3953 0.040 Uiso 1 1 calc R . . C21 C 0.3179(3) -0.0673(2) 0.25174(19) 0.0455(6) Uani 1 1 d . . . H21 H 0.3537 -0.0467 0.1964 0.055 Uiso 1 1 calc R . . C22 C 0.2075(2) -0.1633(3) 0.2155(2) 0.0513(7) Uani 1 1 d . . . H22 H 0.1654 -0.2075 0.1349 0.062 Uiso 1 1 calc R . . C23 C 0.1567(2) -0.1967(3) 0.2944(2) 0.0543(7) Uani 1 1 d . . . H23 H 0.0811 -0.2650 0.2679 0.065 Uiso 1 1 calc R . . C24 C 0.2158(2) -0.1306(2) 0.4127(2) 0.0412(5) Uani 1 1 d . . . H24 H 0.1803 -0.1526 0.4676 0.049 Uiso 1 1 calc R . . N3 N 0.37326(14) 0.32656(14) 0.71671(13) 0.0217(3) Uani 1 1 d D . . H3A H 0.397(2) 0.4018(14) 0.7544(18) 0.033 Uiso 1 1 d D . . S3 S 0.33546(4) 0.29172(4) 0.58104(4) 0.01934(9) Uani 1 1 d . . . C25 C 0.23338(17) 0.37315(17) 0.54657(16) 0.0247(4) Uani 1 1 d . . . C26 C 0.13157(19) 0.3066(2) 0.44806(19) 0.0354(5) Uani 1 1 d . . . H26 H 0.1169 0.2215 0.4025 0.042 Uiso 1 1 calc R . . C27 C 0.0511(2) 0.3669(3) 0.4171(2) 0.0518(7) Uani 1 1 d . . . H27 H -0.0184 0.3230 0.3491 0.062 Uiso 1 1 calc R . . C28 C 0.0717(2) 0.4894(3) 0.4844(3) 0.0545(7) Uani 1 1 d . . . H28 H 0.0157 0.5297 0.4634 0.065 Uiso 1 1 calc R . . C29 C 0.1735(3) 0.5545(2) 0.5824(2) 0.0505(6) Uani 1 1 d . . . H29 H 0.1866 0.6391 0.6286 0.061 Uiso 1 1 calc R . . C30 C 0.2570(2) 0.4976(2) 0.6144(2) 0.0357(5) Uani 1 1 d . . . H30 H 0.3282 0.5426 0.6807 0.043 Uiso 1 1 calc R . . C31 C 0.47373(17) 0.36412(17) 0.54555(16) 0.0225(4) Uani 1 1 d . . . C32 C 0.46937(19) 0.3300(2) 0.42857(17) 0.0331(4) Uani 1 1 d . . . H32 H 0.3954 0.2702 0.3703 0.040 Uiso 1 1 calc R . . C33 C 0.5735(2) 0.3837(2) 0.39770(19) 0.0405(5) Uani 1 1 d . . . H33 H 0.5717 0.3598 0.3179 0.049 Uiso 1 1 calc R . . C34 C 0.6803(2) 0.4721(2) 0.4825(2) 0.0354(5) Uani 1 1 d . . . H34 H 0.7508 0.5106 0.4610 0.043 Uiso 1 1 calc R . . C35 C 0.68457(19) 0.50450(19) 0.5987(2) 0.0329(5) Uani 1 1 d . . . H35 H 0.7587 0.5643 0.6569 0.040 Uiso 1 1 calc R . . C36 C 0.58117(18) 0.45026(18) 0.63099(17) 0.0268(4) Uani 1 1 d . . . H36 H 0.5843 0.4722 0.7108 0.032 Uiso 1 1 calc R . . N4 N 0.28311(15) 0.37440(14) 0.91409(14) 0.0248(3) Uani 1 1 d D . . H4A H 0.331(2) 0.4372(16) 0.923(2) 0.037 Uiso 1 1 d D . . S4 S 0.18001(4) 0.39313(4) 0.98765(4) 0.02113(9) Uani 1 1 d . . . C37 C 0.09559(17) 0.48964(16) 0.95571(15) 0.0242(4) Uani 1 1 d . . . C38 C -0.00308(19) 0.5096(2) 1.00809(18) 0.0354(5) Uani 1 1 d . . . H38 H -0.0219 0.4768 1.0620 0.042 Uiso 1 1 calc R . . C39 C -0.0733(2) 0.5783(2) 0.9801(2) 0.0462(6) Uani 1 1 d . . . H39 H -0.1405 0.5936 1.0157 0.055 Uiso 1 1 calc R . . C40 C -0.0467(2) 0.6252(2) 0.9005(2) 0.0436(6) Uani 1 1 d . . . H40 H -0.0949 0.6730 0.8824 0.052 Uiso 1 1 calc R . . C41 C 0.0496(2) 0.6024(2) 0.8478(2) 0.0415(5) Uani 1 1 d . . . H41 H 0.0673 0.6341 0.7929 0.050 Uiso 1 1 calc R . . C42 C 0.1217(2) 0.53323(18) 0.87442(18) 0.0319(4) Uani 1 1 d . . . H42 H 0.1874 0.5164 0.8373 0.038 Uiso 1 1 calc R . . C43 C 0.26478(17) 0.49309(17) 1.13573(15) 0.0225(4) Uani 1 1 d . . . C44 C 0.2410(2) 0.45244(19) 1.21898(18) 0.0344(5) Uani 1 1 d . . . H44 H 0.1777 0.3760 1.1980 0.041 Uiso 1 1 calc R . . C45 C 0.3104(2) 0.5243(2) 1.33381(18) 0.0413(5) Uani 1 1 d . . . H45 H 0.2953 0.4967 1.3918 0.050 Uiso 1 1 calc R . . C46 C 0.4015(2) 0.6359(2) 1.36427(18) 0.0379(5) Uani 1 1 d . . . H46 H 0.4480 0.6855 1.4432 0.045 Uiso 1 1 calc R . . C47 C 0.4249(2) 0.6754(2) 1.27960(18) 0.0374(5) Uani 1 1 d . . . H47 H 0.4880 0.7521 1.3007 0.045 Uiso 1 1 calc R . . C48 C 0.35710(19) 0.60390(19) 1.16401(18) 0.0305(4) Uani 1 1 d . . . H48 H 0.3736 0.6304 1.1056 0.037 Uiso 1 1 calc R . . N5 N 0.07726(14) 0.16970(15) 0.65032(14) 0.0253(3) Uani 1 1 d D . . H5A H 0.042(2) 0.0996(15) 0.642(2) 0.038 Uiso 1 1 d D . . S5 S -0.02420(4) 0.23573(4) 0.63206(4) 0.02189(9) Uani 1 1 d . . . C49 C -0.13316(16) 0.22970(17) 0.72327(15) 0.0225(4) Uani 1 1 d . . . C50 C -0.11837(18) 0.17145(19) 0.79552(18) 0.0289(4) Uani 1 1 d . . . H50 H -0.0535 0.1331 0.7957 0.035 Uiso 1 1 calc R . . C51 C -0.1997(2) 0.1701(2) 0.86733(19) 0.0363(5) Uani 1 1 d . . . H51 H -0.1912 0.1293 0.9164 0.044 Uiso 1 1 calc R . . C52 C -0.2932(2) 0.2274(2) 0.86853(18) 0.0336(5) Uani 1 1 d . . . H52 H -0.3489 0.2254 0.9178 0.040 Uiso 1 1 calc R . . C53 C -0.30532(19) 0.28772(19) 0.79737(17) 0.0322(4) Uani 1 1 d . . . H53 H -0.3688 0.3278 0.7985 0.039 Uiso 1 1 calc R . . C54 C -0.22519(19) 0.28941(18) 0.72530(17) 0.0293(4) Uani 1 1 d . . . H54 H -0.2328 0.3312 0.6771 0.035 Uiso 1 1 calc R . . C55 C -0.13969(16) 0.13710(16) 0.49327(15) 0.0221(3) Uani 1 1 d . . . C56 C -0.21887(18) 0.18655(18) 0.44350(16) 0.0299(4) Uani 1 1 d . . . H56 H -0.2127 0.2709 0.4818 0.036 Uiso 1 1 calc R . . C57 C -0.30732(19) 0.1104(2) 0.33664(17) 0.0356(5) Uani 1 1 d . . . H57 H -0.3615 0.1432 0.3014 0.043 Uiso 1 1 calc R . . C58 C -0.31688(19) -0.0124(2) 0.28142(17) 0.0346(4) Uani 1 1 d . . . H58 H -0.3791 -0.0644 0.2095 0.042 Uiso 1 1 calc R . . C59 C -0.23596(19) -0.05951(19) 0.33076(17) 0.0316(4) Uani 1 1 d . . . H59 H -0.2418 -0.1437 0.2919 0.038 Uiso 1 1 calc R . . C60 C -0.14561(17) 0.01536(17) 0.43714(15) 0.0259(4) Uani 1 1 d . . . H60 H -0.0890 -0.0168 0.4705 0.031 Uiso 1 1 calc R . . B1 B -0.0047(2) -0.2058(2) 0.6123(2) 0.0296(5) Uani 1 1 d . . . F1 F -0.03169(12) -0.09553(11) 0.63668(12) 0.0426(3) Uani 1 1 d . . . F2 F -0.04270(16) -0.27789(15) 0.49520(13) 0.0632(4) Uani 1 1 d . . . F3 F -0.06506(13) -0.26588(14) 0.67009(14) 0.0556(4) Uani 1 1 d . . . F4 F 0.12828(11) -0.17531(12) 0.65413(13) 0.0454(3) Uani 1 1 d . . . B2 B 0.5796(2) 0.6352(2) 0.9554(2) 0.0305(5) Uani 1 1 d . . . F5 F 0.65264(15) 0.68190(15) 0.89495(14) 0.0668(5) Uani 1 1 d . . . F6 F 0.59943(14) 0.52772(13) 0.95105(14) 0.0602(4) Uani 1 1 d . . . F7 F 0.61128(14) 0.72153(13) 1.06916(11) 0.0505(4) Uani 1 1 d . . . F8 F 0.45041(11) 0.60780(12) 0.90358(12) 0.0431(3) Uani 1 1 d . . . C61 C 0.7605(3) 0.4650(4) 0.2118(3) 0.0667(8) Uani 1 1 d . . . C62 C 0.7318(4) 0.5779(4) 0.2356(3) 0.0917(11) Uani 1 1 d . . . H62A H 0.6443 0.5671 0.2446 0.110 Uiso 1 1 calc R . . H62B H 0.7391 0.6006 0.1710 0.110 Uiso 1 1 calc R . . H62C H 0.7924 0.6432 0.3075 0.110 Uiso 1 1 calc R . . N6 N 0.7851(4) 0.3760(3) 0.1958(3) 0.0938(10) Uani 1 1 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 Cu1 0.01865(10) 0.01634(9) 0.01799(9) 0.00747(7) 0.00723(7) 0.00624(7) N1 0.0245(8) 0.0176(7) 0.0206(7) 0.0089(6) 0.0066(6) 0.0045(6) S1 0.0210(2) 0.0200(2) 0.0199(2) 0.00967(17) 0.00689(16) 0.00600(16) C1 0.0270(9) 0.0344(10) 0.0234(9) 0.0175(8) 0.0098(7) 0.0150(8) C2 0.0373(11) 0.0327(11) 0.0341(11) 0.0181(9) 0.0138(9) 0.0179(9) C3 0.0573(15) 0.0470(13) 0.0369(11) 0.0257(10) 0.0205(11) 0.0344(12) C4 0.0536(14) 0.0758(18) 0.0356(11) 0.0354(12) 0.0207(11) 0.0466(13) C5 0.0299(11) 0.0766(18) 0.0365(11) 0.0325(12) 0.0106(9) 0.0244(11) C6 0.0295(10) 0.0458(12) 0.0320(10) 0.0208(9) 0.0075(8) 0.0130(9) C7 0.0238(9) 0.0215(9) 0.0256(9) 0.0115(7) 0.0106(7) 0.0074(7) C8 0.0348(11) 0.0421(12) 0.0250(10) 0.0125(9) 0.0085(8) -0.0018(9) C9 0.0552(14) 0.0481(14) 0.0284(11) 0.0168(10) 0.0205(10) 0.0031(11) C10 0.0344(11) 0.0331(11) 0.0431(12) 0.0180(10) 0.0203(9) 0.0058(9) C11 0.0245(9) 0.0330(11) 0.0404(11) 0.0191(9) 0.0095(8) 0.0049(8) C12 0.0259(9) 0.0316(10) 0.0301(10) 0.0180(9) 0.0086(8) 0.0088(8) N2 0.0271(8) 0.0183(7) 0.0306(8) 0.0104(7) 0.0166(7) 0.0090(6) S2 0.0207(2) 0.0198(2) 0.0215(2) 0.00850(16) 0.00842(16) 0.00900(16) C13 0.0207(8) 0.0176(8) 0.0220(8) 0.0045(7) 0.0018(7) 0.0077(7) C14 0.0352(10) 0.0354(11) 0.0279(9) 0.0151(8) 0.0133(8) 0.0193(9) C15 0.0486(13) 0.0314(11) 0.0308(10) 0.0166(9) 0.0075(9) 0.0187(10) C16 0.0320(10) 0.0320(10) 0.0326(10) 0.0094(9) -0.0010(8) 0.0168(8) C17 0.0229(9) 0.0332(10) 0.0404(11) 0.0119(9) 0.0077(8) 0.0134(8) C18 0.0205(9) 0.0290(10) 0.0319(10) 0.0133(8) 0.0078(8) 0.0091(7) C19 0.0241(9) 0.0266(9) 0.0234(9) 0.0088(8) 0.0047(7) 0.0142(7) C20 0.0402(11) 0.0363(11) 0.0282(10) 0.0150(9) 0.0109(9) 0.0152(9) C21 0.0624(16) 0.0536(14) 0.0268(11) 0.0193(10) 0.0123(11) 0.0257(13) C22 0.0520(15) 0.0628(17) 0.0254(11) 0.0076(11) -0.0029(10) 0.0210(13) C23 0.0362(13) 0.0563(16) 0.0439(14) 0.0055(12) -0.0029(11) 0.0027(11) C24 0.0333(12) 0.0486(14) 0.0330(11) 0.0128(10) 0.0070(9) 0.0066(10) N3 0.0255(8) 0.0185(8) 0.0195(7) 0.0078(6) 0.0064(6) 0.0044(6) S3 0.0207(2) 0.0179(2) 0.0206(2) 0.00890(17) 0.00721(16) 0.00582(16) C25 0.0249(9) 0.0281(9) 0.0304(10) 0.0185(8) 0.0124(8) 0.0114(7) C26 0.0261(10) 0.0428(12) 0.0406(11) 0.0253(10) 0.0074(9) 0.0050(8) C27 0.0284(11) 0.082(2) 0.0632(16) 0.0526(16) 0.0084(11) 0.0154(12) C28 0.0467(14) 0.081(2) 0.0806(19) 0.0618(17) 0.0319(14) 0.0436(14) C29 0.0703(17) 0.0475(14) 0.0648(17) 0.0365(13) 0.0359(14) 0.0412(13) C30 0.0467(12) 0.0374(12) 0.0357(11) 0.0206(10) 0.0181(10) 0.0230(10) C31 0.0236(9) 0.0213(9) 0.0290(9) 0.0139(8) 0.0115(7) 0.0100(7) C32 0.0314(10) 0.0382(11) 0.0273(10) 0.0137(9) 0.0104(8) 0.0054(9) C33 0.0434(12) 0.0555(14) 0.0347(11) 0.0268(11) 0.0226(10) 0.0168(11) C34 0.0309(10) 0.0409(12) 0.0502(13) 0.0314(11) 0.0218(10) 0.0121(9) C35 0.0251(10) 0.0296(11) 0.0448(12) 0.0190(10) 0.0081(9) 0.0054(8) C36 0.0273(9) 0.0267(10) 0.0282(9) 0.0131(8) 0.0094(8) 0.0079(8) N4 0.0271(8) 0.0177(7) 0.0280(8) 0.0070(7) 0.0145(7) 0.0043(6) S4 0.0237(2) 0.0184(2) 0.0207(2) 0.00680(16) 0.00879(16) 0.00635(16) C37 0.0236(9) 0.0194(9) 0.0217(8) 0.0023(7) 0.0017(7) 0.0062(7) C38 0.0286(10) 0.0410(12) 0.0319(11) 0.0101(9) 0.0062(9) 0.0129(9) C39 0.0303(11) 0.0524(15) 0.0442(13) 0.0052(11) 0.0044(10) 0.0217(10) C40 0.0410(12) 0.0316(11) 0.0447(13) 0.0057(10) -0.0088(10) 0.0178(10) C41 0.0491(13) 0.0334(12) 0.0399(12) 0.0175(10) 0.0004(10) 0.0134(10) C42 0.0357(11) 0.0252(10) 0.0324(10) 0.0110(8) 0.0061(8) 0.0091(8) C43 0.0243(9) 0.0236(9) 0.0179(8) 0.0057(7) 0.0067(7) 0.0092(7) C44 0.0406(12) 0.0300(10) 0.0294(10) 0.0128(9) 0.0124(9) 0.0032(9) C45 0.0546(14) 0.0461(13) 0.0239(10) 0.0180(10) 0.0111(10) 0.0111(11) C46 0.0406(12) 0.0396(12) 0.0237(9) 0.0075(9) 0.0020(9) 0.0095(10) C47 0.0357(11) 0.0333(11) 0.0311(10) 0.0083(9) 0.0037(9) 0.0020(9) C48 0.0334(10) 0.0287(10) 0.0266(10) 0.0120(8) 0.0081(8) 0.0043(8) N5 0.0173(7) 0.0266(8) 0.0305(8) 0.0125(7) 0.0019(6) 0.0064(6) S5 0.0177(2) 0.0219(2) 0.0241(2) 0.00968(17) 0.00257(16) 0.00472(16) C49 0.0168(8) 0.0217(9) 0.0203(8) 0.0036(7) 0.0015(7) 0.0022(7) C50 0.0241(9) 0.0308(10) 0.0348(10) 0.0157(9) 0.0079(8) 0.0108(8) C51 0.0390(12) 0.0445(13) 0.0363(11) 0.0238(10) 0.0157(9) 0.0177(10) C52 0.0299(10) 0.0369(11) 0.0324(10) 0.0117(9) 0.0130(8) 0.0097(9) C53 0.0272(10) 0.0334(11) 0.0314(10) 0.0062(9) 0.0071(8) 0.0146(8) C54 0.0297(10) 0.0277(10) 0.0300(10) 0.0123(8) 0.0037(8) 0.0110(8) C55 0.0183(8) 0.0272(9) 0.0208(8) 0.0111(7) 0.0054(7) 0.0054(7) C56 0.0268(9) 0.0330(10) 0.0284(9) 0.0117(8) 0.0032(8) 0.0117(8) C57 0.0298(10) 0.0504(13) 0.0298(10) 0.0191(10) 0.0037(8) 0.0171(9) C58 0.0271(10) 0.0458(12) 0.0221(9) 0.0092(9) 0.0027(8) 0.0071(9) C59 0.0333(10) 0.0313(11) 0.0239(9) 0.0067(8) 0.0079(8) 0.0074(8) C60 0.0257(9) 0.0309(10) 0.0231(9) 0.0130(8) 0.0071(7) 0.0094(7) B1 0.0255(11) 0.0230(11) 0.0381(12) 0.0130(9) 0.0061(9) 0.0053(8) F1 0.0346(6) 0.0311(7) 0.0604(8) 0.0185(6) 0.0048(6) 0.0137(5) F2 0.0742(11) 0.0508(9) 0.0393(8) 0.0013(7) 0.0046(7) 0.0118(8) F3 0.0456(8) 0.0509(9) 0.0759(10) 0.0407(8) 0.0180(7) 0.0006(6) F4 0.0244(6) 0.0377(7) 0.0764(10) 0.0278(7) 0.0089(6) 0.0108(5) B2 0.0260(11) 0.0231(11) 0.0335(12) 0.0051(9) 0.0084(9) 0.0034(8) F5 0.0560(9) 0.0624(10) 0.0527(9) 0.0100(7) 0.0265(7) -0.0164(8) F6 0.0511(8) 0.0351(7) 0.0790(11) 0.0110(7) -0.0004(8) 0.0197(7) F7 0.0614(9) 0.0359(7) 0.0318(7) 0.0006(6) 0.0060(6) 0.0030(6) F8 0.0273(6) 0.0328(7) 0.0595(8) 0.0151(6) 0.0007(6) 0.0064(5) C61 0.078(2) 0.085(2) 0.0543(18) 0.0403(18) 0.0300(16) 0.0292(19) C62 0.112(3) 0.109(3) 0.079(2) 0.057(2) 0.024(2) 0.051(2) N6 0.123(3) 0.093(2) 0.073(2) 0.0320(18) 0.0454(19) 0.041(2) _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 N4 1.9891(15) . ? Cu1 N3 1.9972(15) . ? Cu1 N2 2.0144(15) . ? Cu1 N1 2.0249(16) . ? Cu1 N5 2.2926(15) . ? N1 S1 1.5905(16) . ? S1 C1 1.7936(18) . ? S1 C7 1.7936(19) . ? C1 C2 1.382(3) . ? C1 C6 1.385(3) . ? C2 C3 1.389(3) . ? C3 C4 1.377(4) . ? C4 C5 1.378(4) . ? C5 C6 1.390(3) . ? C7 C12 1.380(3) . ? C7 C8 1.388(3) . ? C8 C9 1.388(3) . ? C9 C10 1.374(3) . ? C10 C11 1.371(3) . ? C11 C12 1.398(3) . ? N2 S2 1.5854(15) . ? S2 C19 1.7974(19) . ? S2 C13 1.7989(17) . ? C13 C14 1.385(3) . ? C13 C18 1.391(3) . ? C14 C15 1.394(3) . ? C15 C16 1.384(3) . ? C16 C17 1.380(3) . ? C17 C18 1.380(3) . ? C19 C24 1.378(3) . ? C19 C20 1.387(3) . ? C20 C21 1.387(3) . ? C21 C22 1.366(4) . ? C22 C23 1.375(4) . ? C23 C24 1.391(3) . ? N3 S3 1.5928(16) . ? S3 C25 1.7923(18) . ? S3 C31 1.7994(19) . ? C25 C26 1.386(3) . ? C25 C30 1.388(3) . ? C26 C27 1.393(3) . ? C27 C28 1.373(4) . ? C28 C29 1.381(4) . ? C29 C30 1.389(3) . ? C31 C36 1.381(3) . ? C31 C32 1.390(3) . ? C32 C33 1.382(3) . ? C33 C34 1.381(3) . ? C34 C35 1.383(3) . ? C35 C36 1.389(3) . ? N4 S4 1.5914(15) . ? S4 C43 1.7874(18) . ? S4 C37 1.8015(18) . ? C37 C42 1.380(3) . ? C37 C38 1.389(3) . ? C38 C39 1.383(3) . ? C39 C40 1.387(4) . ? C40 C41 1.374(3) . ? C41 C42 1.395(3) . ? C43 C44 1.376(3) . ? C43 C48 1.385(3) . ? C44 C45 1.386(3) . ? C45 C46 1.380(3) . ? C46 C47 1.383(3) . ? C47 C48 1.388(3) . ? N5 S5 1.5762(15) . ? S5 C55 1.8097(18) . ? S5 C49 1.8115(19) . ? C49 C50 1.386(3) . ? C49 C54 1.390(3) . ? C50 C51 1.384(3) . ? C51 C52 1.386(3) . ? C52 C53 1.391(3) . ? C53 C54 1.377(3) . ? C55 C60 1.382(3) . ? C55 C56 1.391(3) . ? C56 C57 1.391(3) . ? C57 C58 1.381(3) . ? C58 C59 1.379(3) . ? C59 C60 1.394(3) . ? B1 F2 1.366(3) . ? B1 F3 1.371(3) . ? B1 F1 1.392(3) . ? B1 F4 1.403(2) . ? B2 F7 1.377(3) . ? B2 F6 1.377(3) . ? B2 F5 1.378(3) . ? B2 F8 1.394(3) . ? C61 N6 1.145(4) . ? C61 C62 1.433(5) . ? 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 N4 Cu1 N3 88.03(6) . . ? N4 Cu1 N2 160.84(7) . . ? N3 Cu1 N2 92.86(6) . . ? N4 Cu1 N1 91.27(6) . . ? N3 Cu1 N1 174.90(7) . . ? N2 Cu1 N1 86.16(6) . . ? N4 Cu1 N5 105.76(6) . . ? N3 Cu1 N5 96.32(6) . . ? N2 Cu1 N5 93.18(6) . . ? N1 Cu1 N5 88.73(6) . . ? S1 N1 Cu1 124.15(9) . . ? N1 S1 C1 109.73(8) . . ? N1 S1 C7 107.58(9) . . ? C1 S1 C7 99.97(9) . . ? C2 C1 C6 121.09(18) . . ? C2 C1 S1 122.30(15) . . ? C6 C1 S1 116.29(15) . . ? C1 C2 C3 119.4(2) . . ? C4 C3 C2 119.8(2) . . ? C3 C4 C5 120.8(2) . . ? C4 C5 C6 120.0(2) . . ? C1 C6 C5 119.0(2) . . ? C12 C7 C8 121.12(17) . . ? C12 C7 S1 120.59(14) . . ? C8 C7 S1 118.28(15) . . ? C9 C8 C7 118.80(19) . . ? C10 C9 C8 120.5(2) . . ? C11 C10 C9 120.46(19) . . ? C10 C11 C12 120.18(19) . . ? C7 C12 C11 118.91(18) . . ? S2 N2 Cu1 129.00(9) . . ? N2 S2 C19 110.48(9) . . ? N2 S2 C13 109.14(8) . . ? C19 S2 C13 98.75(8) . . ? C14 C13 C18 121.27(17) . . ? C14 C13 S2 121.36(14) . . ? C18 C13 S2 117.31(14) . . ? C13 C14 C15 118.66(18) . . ? C16 C15 C14 120.3(2) . . ? C17 C16 C15 120.25(18) . . ? C18 C17 C16 120.39(18) . . ? C17 C18 C13 119.15(18) . . ? C24 C19 C20 120.42(19) . . ? C24 C19 S2 122.66(16) . . ? C20 C19 S2 116.91(15) . . ? C19 C20 C21 119.6(2) . . ? C22 C21 C20 119.9(2) . . ? C21 C22 C23 120.7(2) . . ? C22 C23 C24 120.1(2) . . ? C19 C24 C23 119.3(2) . . ? S3 N3 Cu1 119.29(9) . . ? N3 S3 C25 112.07(9) . . ? N3 S3 C31 107.96(8) . . ? C25 S3 C31 97.42(8) . . ? C26 C25 C30 121.75(19) . . ? C26 C25 S3 116.86(15) . . ? C30 C25 S3 121.38(15) . . ? C25 C26 C27 118.7(2) . . ? C28 C27 C26 120.3(2) . . ? C27 C28 C29 120.3(2) . . ? C28 C29 C30 120.8(2) . . ? C25 C30 C29 118.1(2) . . ? C36 C31 C32 120.73(18) . . ? C36 C31 S3 121.55(15) . . ? C32 C31 S3 117.72(15) . . ? C33 C32 C31 119.50(19) . . ? C34 C33 C32 120.2(2) . . ? C33 C34 C35 119.91(19) . . ? C34 C35 C36 120.45(19) . . ? C31 C36 C35 119.15(19) . . ? S4 N4 Cu1 126.08(9) . . ? N4 S4 C43 107.76(9) . . ? N4 S4 C37 110.44(9) . . ? C43 S4 C37 99.46(8) . . ? C42 C37 C38 121.49(19) . . ? C42 C37 S4 120.53(15) . . ? C38 C37 S4 117.76(16) . . ? C39 C38 C37 118.6(2) . . ? C38 C39 C40 120.8(2) . . ? C41 C40 C39 119.8(2) . . ? C40 C41 C42 120.5(2) . . ? C37 C42 C41 118.8(2) . . ? C44 C43 C48 121.47(18) . . ? C44 C43 S4 117.65(15) . . ? C48 C43 S4 120.75(15) . . ? C43 C44 C45 119.2(2) . . ? C46 C45 C44 120.3(2) . . ? C45 C46 C47 119.87(19) . . ? C46 C47 C48 120.5(2) . . ? C43 C48 C47 118.58(19) . . ? S5 N5 Cu1 136.68(9) . . ? N5 S5 C55 108.30(8) . . ? N5 S5 C49 110.98(9) . . ? C55 S5 C49 97.38(8) . . ? C50 C49 C54 120.80(17) . . ? C50 C49 S5 119.16(14) . . ? C54 C49 S5 119.93(14) . . ? C51 C50 C49 118.90(18) . . ? C50 C51 C52 120.8(2) . . ? C51 C52 C53 119.8(2) . . ? C54 C53 C52 119.99(18) . . ? C53 C54 C49 119.76(18) . . ? C60 C55 C56 121.12(17) . . ? C60 C55 S5 119.76(13) . . ? C56 C55 S5 119.10(14) . . ? C55 C56 C57 118.90(18) . . ? C58 C57 C56 120.48(19) . . ? C59 C58 C57 119.93(18) . . ? C58 C59 C60 120.58(19) . . ? C55 C60 C59 118.94(17) . . ? F2 B1 F3 110.61(18) . . ? F2 B1 F1 110.15(18) . . ? F3 B1 F1 109.85(19) . . ? F2 B1 F4 110.49(19) . . ? F3 B1 F4 108.77(18) . . ? F1 B1 F4 106.89(16) . . ? F7 B2 F6 110.3(2) . . ? F7 B2 F5 109.16(17) . . ? F6 B2 F5 110.60(19) . . ? F7 B2 F8 110.11(18) . . ? F6 B2 F8 107.77(17) . . ? F5 B2 F8 108.9(2) . . ? N6 C61 C62 178.2(4) . . ? 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 N1 H1A F1 0.792(14) 2.541(19) 3.123(2) 131(2) . N1 H1A F4 0.792(14) 2.608(16) 3.374(2) 163(2) . N2 H2A F4 0.799(15) 2.309(15) 3.100(2) 171(2) . N3 H3A F8 0.823(14) 2.406(15) 3.208(2) 165(2) . N4 H4A F8 0.787(15) 2.335(16) 3.107(2) 167(2) . N5 H5A F1 0.819(15) 2.331(16) 3.145(2) 172(2) . _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.324 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.041 # END of data for (2) data_(3) _database_code_depnum_ccdc_archive 'CCDC 227320' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H52 B2 Cu F8 N5 O0.50 S4' _chemical_formula_weight 1120.39 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.7430(6) _cell_length_b 20.5911(7) _cell_length_c 30.9059(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10655.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12119 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.60 _exptl_crystal_description lath _exptl_crystal_colour blue _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4624 _exptl_absorpt_coefficient_mu 0.637 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 74826 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9392 _reflns_number_gt 5920 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0875P)^2^+5.6162P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except NH coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9392 _refine_ls_number_parameters 693 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1774 _refine_ls_wR_factor_gt 0.1596 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _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 Cu1 Cu 0.73952(3) 0.35125(3) 0.164204(14) 0.04161(18) Uani 1 1 d . . . N1 N 0.7732(2) 0.3634(3) 0.22509(12) 0.0864(18) Uani 1 1 d D . . H1A H 0.823(2) 0.362(3) 0.232(2) 0.130 Uiso 1 1 d D . . S1 S 0.71195(7) 0.34969(10) 0.26386(4) 0.0801(6) Uani 1 1 d . . . C1 C 0.7308(3) 0.2727(4) 0.28698(18) 0.089(2) Uani 1 1 d . . . C2 C 0.6893(4) 0.2551(4) 0.3249(2) 0.094(2) Uani 1 1 d . . . H2 H 0.6526 0.2848 0.3375 0.113 Uiso 1 1 calc R . . C3 C 0.7008(5) 0.1970(5) 0.3437(3) 0.127(3) Uani 1 1 d . . . H3 H 0.6728 0.1850 0.3692 0.153 Uiso 1 1 calc R . . C4 C 0.7552(7) 0.1550(4) 0.3244(4) 0.144(4) Uani 1 1 d . . . H4 H 0.7655 0.1140 0.3373 0.172 Uiso 1 1 calc R . . C5 C 0.7943(5) 0.1719(5) 0.2867(3) 0.133(4) Uani 1 1 d . . . H5 H 0.8299 0.1419 0.2736 0.160 Uiso 1 1 calc R . . C6 C 0.7828(4) 0.2304(5) 0.2684(2) 0.103(3) Uani 1 1 d . . . H6 H 0.8107 0.2420 0.2428 0.123 Uiso 1 1 calc R . . C7 C 0.7410(2) 0.3974(3) 0.30906(13) 0.0559(13) Uani 1 1 d . . . C8 C 0.8165(3) 0.3921(3) 0.32682(15) 0.0609(14) Uani 1 1 d . . . H8 H 0.8545 0.3630 0.3148 0.073 Uiso 1 1 calc R . . C9 C 0.8360(3) 0.4297(3) 0.36237(17) 0.0703(15) Uani 1 1 d . . . H9 H 0.8877 0.4265 0.3748 0.084 Uiso 1 1 calc R . . C10 C 0.7808(4) 0.4716(3) 0.37972(18) 0.0759(16) Uani 1 1 d . . . H10 H 0.7942 0.4967 0.4045 0.091 Uiso 1 1 calc R . . C11 C 0.7067(4) 0.4772(3) 0.3615(2) 0.0807(18) Uani 1 1 d . . . H11 H 0.6688 0.5064 0.3735 0.097 Uiso 1 1 calc R . . C12 C 0.6867(3) 0.4402(3) 0.32564(17) 0.0743(17) Uani 1 1 d . . . H12 H 0.6356 0.4446 0.3126 0.089 Uiso 1 1 calc R . . N2 N 0.85125(19) 0.35119(17) 0.14633(10) 0.0394(8) Uani 1 1 d D . . H2A H 0.885(2) 0.354(2) 0.1673(12) 0.059 Uiso 1 1 d D . . S2 S 0.88580(6) 0.36093(5) 0.09880(3) 0.0366(3) Uani 1 1 d . . . C13 C 0.9393(2) 0.4372(2) 0.09723(12) 0.0386(9) Uani 1 1 d . . . C14 C 0.9837(2) 0.4532(2) 0.06083(13) 0.0453(10) Uani 1 1 d . . . H14 H 0.9859 0.4245 0.0368 0.054 Uiso 1 1 calc R . . C15 C 1.0247(3) 0.5114(2) 0.05996(16) 0.0561(13) Uani 1 1 d . . . H15 H 1.0550 0.5228 0.0351 0.067 Uiso 1 1 calc R . . C16 C 1.0220(3) 0.5528(2) 0.0948(2) 0.0676(15) Uani 1 1 d . . . H16 H 1.0506 0.5926 0.0941 0.081 Uiso 1 1 calc R . . C17 C 0.9777(4) 0.5365(3) 0.1310(2) 0.0808(17) Uani 1 1 d . . . H17 H 0.9762 0.5653 0.1550 0.097 Uiso 1 1 calc R . . C18 C 0.9353(3) 0.4783(2) 0.13245(16) 0.0572(12) Uani 1 1 d . . . H18 H 0.9043 0.4672 0.1571 0.069 Uiso 1 1 calc R . . C19 C 0.9699(2) 0.30796(19) 0.09205(12) 0.0390(9) Uani 1 1 d . . . C20 C 1.0215(3) 0.2956(2) 0.12591(15) 0.0592(13) Uani 1 1 d . . . H20 H 1.0120 0.3148 0.1534 0.071 Uiso 1 1 calc R . . C21 C 1.0864(3) 0.2559(3) 0.12014(18) 0.0678(14) Uani 1 1 d . . . H21 H 1.1215 0.2477 0.1437 0.081 Uiso 1 1 calc R . . C22 C 1.1007(3) 0.2281(2) 0.08093(17) 0.0614(13) Uani 1 1 d . . . H22 H 1.1456 0.2005 0.0770 0.074 Uiso 1 1 calc R . . C23 C 1.0507(4) 0.2401(3) 0.04769(17) 0.0751(16) Uani 1 1 d . . . H23 H 1.0613 0.2212 0.0202 0.090 Uiso 1 1 calc R . . C24 C 0.9836(3) 0.2796(2) 0.05266(14) 0.0596(13) Uani 1 1 d . . . H24 H 0.9481 0.2867 0.0292 0.071 Uiso 1 1 calc R . . N3 N 0.69717(19) 0.39156(18) 0.11028(11) 0.0423(8) Uani 1 1 d D . . H3A H 0.716(3) 0.381(2) 0.0854(11) 0.064 Uiso 1 1 d D . . S3 S 0.60695(6) 0.41594(6) 0.11266(3) 0.0445(3) Uani 1 1 d . . . C25 C 0.5393(3) 0.3562(3) 0.09117(12) 0.0501(12) Uani 1 1 d . . . C26 C 0.4590(3) 0.3680(3) 0.09536(16) 0.0779(18) Uani 1 1 d . . . H26 H 0.4404 0.4078 0.1071 0.094 Uiso 1 1 calc R . . C27 C 0.4065(5) 0.3215(6) 0.0823(2) 0.125(4) Uani 1 1 d . . . H27 H 0.3508 0.3299 0.0841 0.149 Uiso 1 1 calc R . . C28 C 0.4320(6) 0.2639(5) 0.0670(2) 0.120(4) Uani 1 1 d . . . H28 H 0.3941 0.2318 0.0589 0.144 Uiso 1 1 calc R . . C29 C 0.5135(5) 0.2510(3) 0.06275(17) 0.100(2) Uani 1 1 d . . . H29 H 0.5316 0.2106 0.0517 0.120 Uiso 1 1 calc R . . C30 C 0.5680(3) 0.2993(3) 0.07518(14) 0.0628(14) Uani 1 1 d . . . H30 H 0.6239 0.2923 0.0725 0.075 Uiso 1 1 calc R . . C31 C 0.5933(3) 0.4801(2) 0.07429(15) 0.0545(12) Uani 1 1 d . . . C32 C 0.6119(3) 0.4741(3) 0.03223(18) 0.0737(16) Uani 1 1 d . . . H32 H 0.6314 0.4342 0.0211 0.088 Uiso 1 1 calc R . . C33 C 0.6017(3) 0.5289(3) 0.0047(2) 0.0856(19) Uani 1 1 d . . . H33 H 0.6163 0.5267 -0.0250 0.103 Uiso 1 1 calc R . . C34 C 0.5709(4) 0.5841(3) 0.0215(3) 0.0899(19) Uani 1 1 d . . . H34 H 0.5622 0.6198 0.0026 0.108 Uiso 1 1 calc R . . C35 C 0.5523(6) 0.5909(4) 0.0630(3) 0.131(3) Uani 1 1 d . . . H35 H 0.5312 0.6307 0.0736 0.158 Uiso 1 1 calc R . . C36 C 0.5644(5) 0.5384(3) 0.0904(2) 0.101(2) Uani 1 1 d . . . H36 H 0.5529 0.5424 0.1203 0.121 Uiso 1 1 calc R . . N5 N 0.6374(2) 0.3110(3) 0.17972(11) 0.0536(10) Uani 1 1 d D A . H5A H 0.600(3) 0.331(2) 0.1944(16) 0.080 Uiso 1 1 d D . . C49 C 0.6276(3) 0.2507(3) 0.17198(13) 0.0584(14) Uani 1 1 d . . . C50 C 0.5512(4) 0.2162(3) 0.18405(18) 0.0715(15) Uani 1 1 d . A . H50A H 0.5165 0.2461 0.2000 0.086 Uiso 1 1 calc R . . H50B H 0.5637 0.1786 0.2022 0.086 Uiso 1 1 calc R . . H50C H 0.5239 0.2017 0.1577 0.086 Uiso 1 1 calc R . . N4 N 0.6958(3) 0.2297(2) 0.15124(17) 0.0466(13) Uani 0.732(4) 1 d PU A 1 S4 S 0.69518(12) 0.15221(9) 0.14121(6) 0.0549(7) Uani 0.732(4) 1 d PU A 1 N4X N 0.6525(8) 0.1823(7) 0.1533(4) 0.039(3) Uani 0.268(4) 1 d PU A 2 S4X S 0.7401(2) 0.20117(18) 0.13348(12) 0.0336(14) Uani 0.268(4) 1 d PU A 2 C37 C 0.7159(4) 0.1505(3) 0.08300(17) 0.0711(16) Uani 1 1 d . . . C38 C 0.6954(4) 0.0922(3) 0.0666(2) 0.087(2) Uani 1 1 d . A . H38 H 0.6796 0.0576 0.0850 0.104 Uiso 1 1 calc R . . C39 C 0.6979(3) 0.0842(3) 0.0227(2) 0.089(2) Uani 1 1 d . . . H39 H 0.6835 0.0436 0.0104 0.107 Uiso 1 1 calc R A . C40 C 0.7211(4) 0.1340(4) -0.0035(2) 0.0827(19) Uani 1 1 d . A . H40 H 0.7213 0.1283 -0.0340 0.099 Uiso 1 1 calc R . . C41 C 0.7439(4) 0.1923(3) 0.0139(2) 0.0803(17) Uani 1 1 d . . . H41 H 0.7611 0.2266 -0.0044 0.096 Uiso 1 1 calc R A . C42 C 0.7420(3) 0.2008(3) 0.0577(2) 0.0749(17) Uani 1 1 d . A . H42 H 0.7583 0.2408 0.0703 0.090 Uiso 1 1 calc R . . C43 C 0.7939(5) 0.1321(4) 0.16199(19) 0.086(2) Uani 1 1 d . . . C44 C 0.7901(4) 0.0705(5) 0.1779(2) 0.101(2) Uani 1 1 d . A . H44 H 0.7429 0.0453 0.1748 0.122 Uiso 1 1 calc R . . C45 C 0.8547(6) 0.0460(4) 0.1981(2) 0.106(2) Uani 1 1 d . . . H45 H 0.8521 0.0033 0.2096 0.127 Uiso 1 1 calc R A . C46 C 0.9217(5) 0.0795(4) 0.2023(2) 0.098(2) Uani 1 1 d . A . H46 H 0.9664 0.0604 0.2163 0.117 Uiso 1 1 calc R . . C47 C 0.9270(4) 0.1422(4) 0.1864(2) 0.094(2) Uani 1 1 d . . . H47 H 0.9751 0.1664 0.1893 0.113 Uiso 1 1 calc R A . C48 C 0.8600(5) 0.1697(3) 0.1659(2) 0.089(2) Uani 1 1 d . A . H48 H 0.8611 0.2129 0.1553 0.107 Uiso 1 1 calc R . . B1 B 1.0000 0.3307(6) 0.2500 0.074(3) Uani 1 2 d S . . F1 F 1.0547(2) 0.2920(2) 0.22948(12) 0.1261(16) Uani 1 1 d . . . F2 F 0.9613(2) 0.36839(19) 0.21993(10) 0.1001(12) Uani 1 1 d . . . B2 B 0.2880(3) 0.1191(3) 0.01871(16) 0.0496(12) Uani 1 1 d DU . . F3 F 0.23936(19) 0.14559(14) -0.01311(9) 0.0722(8) Uani 1 1 d DU B . F4 F 0.2704(5) 0.0576(3) 0.0294(3) 0.128(4) Uani 0.663(8) 1 d PDU B 1 F5 F 0.3670(3) 0.1236(4) 0.0089(2) 0.101(3) Uani 0.663(8) 1 d PDU B 1 F6 F 0.2792(3) 0.1588(3) 0.05446(16) 0.087(2) Uani 0.663(8) 1 d PDU B 1 F4X F 0.3131(6) 0.0662(5) -0.0067(4) 0.091(4) Uani 0.337(8) 1 d PDU B 2 F5X F 0.3553(10) 0.1516(7) 0.0252(7) 0.156(9) Uani 0.337(8) 1 d PDU B 2 F6X F 0.2435(8) 0.0953(7) 0.0507(3) 0.109(5) Uani 0.337(8) 1 d PDU B 2 O1 O 1.0000 0.5557(4) 0.2500 0.121(2) Uani 1 2 d S . . C51 C 1.0676(6) 0.5250(5) 0.2403(3) 0.130(3) Uani 1 1 d . . . H51A H 1.0782 0.4945 0.2644 0.156 Uiso 1 1 calc R . . H51B H 1.0563 0.4980 0.2145 0.156 Uiso 1 1 calc R . . C52 C 1.1354(6) 0.5553(5) 0.2325(3) 0.176(5) Uani 1 1 d . . . H52A H 1.1335 0.5747 0.2036 0.264 Uiso 1 1 calc R . . H52B H 1.1796 0.5242 0.2340 0.264 Uiso 1 1 calc R . . H52C H 1.1433 0.5895 0.2542 0.264 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 0.0272(3) 0.0745(4) 0.0232(2) -0.0007(2) -0.00305(18) 0.0022(2) N1 0.034(2) 0.204(6) 0.0214(18) -0.004(3) 0.0000(16) -0.002(3) S1 0.0272(6) 0.1884(18) 0.0249(6) -0.0148(8) -0.0011(4) -0.0073(8) C1 0.048(3) 0.158(6) 0.061(3) -0.067(4) 0.018(3) -0.046(4) C2 0.089(5) 0.116(6) 0.078(4) -0.039(4) 0.024(3) -0.057(4) C3 0.135(7) 0.116(7) 0.130(7) -0.054(6) 0.059(6) -0.057(6) C4 0.181(11) 0.081(6) 0.168(10) -0.021(6) 0.013(8) -0.061(6) C5 0.120(7) 0.129(8) 0.150(9) -0.073(7) 0.050(6) -0.049(6) C6 0.088(5) 0.132(7) 0.088(5) -0.061(5) 0.021(4) -0.049(5) C7 0.037(2) 0.104(4) 0.027(2) 0.008(2) 0.0008(18) 0.006(3) C8 0.047(3) 0.087(4) 0.049(3) -0.015(3) -0.012(2) 0.013(3) C9 0.064(3) 0.085(4) 0.062(3) -0.018(3) -0.020(3) 0.003(3) C10 0.098(5) 0.068(4) 0.061(3) -0.008(3) 0.013(3) -0.014(3) C11 0.087(4) 0.079(4) 0.076(4) 0.004(3) 0.034(4) 0.019(3) C12 0.052(3) 0.111(5) 0.059(3) 0.024(3) 0.017(3) 0.022(3) N2 0.0255(17) 0.068(2) 0.0249(16) 0.0041(16) -0.0027(13) -0.0025(16) S2 0.0300(5) 0.0543(6) 0.0253(5) 0.0014(4) -0.0009(4) -0.0022(5) C13 0.032(2) 0.044(2) 0.040(2) 0.0062(19) -0.0096(17) 0.0046(18) C14 0.047(2) 0.055(3) 0.034(2) 0.0098(19) -0.0082(18) -0.006(2) C15 0.051(3) 0.059(3) 0.059(3) 0.025(3) -0.014(2) -0.006(2) C16 0.070(4) 0.041(3) 0.092(4) 0.011(3) -0.014(3) -0.008(3) C17 0.095(4) 0.052(3) 0.096(5) -0.022(3) 0.000(4) -0.002(3) C18 0.062(3) 0.052(3) 0.058(3) -0.007(2) 0.013(2) 0.004(2) C19 0.040(2) 0.038(2) 0.039(2) 0.0033(18) 0.0046(17) -0.0028(18) C20 0.047(3) 0.082(4) 0.048(3) -0.015(2) -0.007(2) 0.015(3) C21 0.050(3) 0.082(4) 0.072(3) -0.011(3) -0.004(3) 0.022(3) C22 0.059(3) 0.053(3) 0.073(3) 0.013(3) 0.017(3) 0.013(2) C23 0.104(4) 0.068(4) 0.053(3) -0.006(3) 0.025(3) 0.024(3) C24 0.080(4) 0.063(3) 0.036(2) -0.004(2) 0.003(2) 0.010(3) N3 0.0288(18) 0.066(2) 0.0326(18) -0.0019(17) -0.0081(14) 0.0059(17) S3 0.0354(5) 0.0632(7) 0.0351(5) -0.0024(5) -0.0103(4) 0.0075(5) C25 0.043(3) 0.084(4) 0.023(2) 0.008(2) -0.0093(17) -0.013(2) C26 0.041(3) 0.144(5) 0.049(3) 0.017(3) -0.005(2) -0.016(3) C27 0.070(5) 0.237(11) 0.067(5) 0.046(6) -0.025(4) -0.070(7) C28 0.130(8) 0.182(9) 0.047(4) 0.044(5) -0.038(4) -0.119(7) C29 0.152(7) 0.100(5) 0.049(3) 0.017(3) -0.031(4) -0.068(5) C30 0.076(4) 0.076(4) 0.037(2) 0.003(2) -0.009(2) -0.024(3) C31 0.041(3) 0.071(3) 0.052(3) 0.003(2) -0.021(2) 0.007(2) C32 0.054(3) 0.094(4) 0.072(4) 0.028(3) 0.008(3) 0.014(3) C33 0.061(4) 0.110(5) 0.086(4) 0.030(4) 0.006(3) 0.009(3) C34 0.101(5) 0.062(4) 0.107(6) 0.013(4) -0.021(4) -0.010(4) C35 0.216(10) 0.089(5) 0.089(6) 0.002(4) -0.052(6) 0.052(6) C36 0.145(6) 0.078(4) 0.080(4) -0.008(3) -0.044(4) 0.041(4) N5 0.037(2) 0.097(4) 0.0262(18) 0.006(2) -0.0015(15) 0.005(2) C49 0.048(3) 0.099(4) 0.028(2) 0.004(3) -0.0014(19) 0.025(3) C50 0.093(4) 0.057(3) 0.064(3) 0.004(3) -0.006(3) -0.003(3) N4 0.043(3) 0.042(3) 0.055(3) -0.005(2) 0.010(3) -0.009(3) S4 0.0587(12) 0.0479(12) 0.0581(11) -0.0027(8) 0.0114(8) -0.0098(9) N4X 0.029(6) 0.041(8) 0.048(7) -0.007(6) 0.010(6) 0.018(6) S4X 0.032(2) 0.032(2) 0.037(2) -0.0031(16) 0.0048(16) -0.0011(17) C37 0.085(4) 0.074(4) 0.054(3) -0.006(3) 0.005(3) 0.025(3) C38 0.105(5) 0.065(4) 0.090(5) -0.003(3) 0.053(4) 0.006(3) C39 0.075(4) 0.066(4) 0.125(6) -0.039(4) 0.025(4) -0.024(3) C40 0.073(4) 0.114(6) 0.061(3) -0.029(4) 0.017(3) 0.005(4) C41 0.078(4) 0.068(4) 0.094(5) 0.009(3) 0.029(3) 0.003(3) C42 0.062(3) 0.060(4) 0.103(5) -0.032(3) -0.007(3) -0.001(3) C43 0.096(5) 0.106(6) 0.056(4) -0.014(4) -0.006(3) 0.051(4) C44 0.088(5) 0.150(8) 0.066(4) 0.008(4) -0.008(4) -0.003(5) C45 0.160(8) 0.080(5) 0.077(4) 0.000(4) -0.013(5) 0.004(5) C46 0.110(6) 0.087(5) 0.097(5) -0.012(4) -0.024(4) 0.044(5) C47 0.085(5) 0.103(6) 0.095(5) -0.039(4) 0.006(4) -0.006(4) C48 0.134(7) 0.062(4) 0.072(4) -0.004(3) 0.011(4) 0.033(4) B1 0.021(4) 0.161(10) 0.040(4) 0.000 -0.003(3) 0.000 F1 0.096(3) 0.198(4) 0.085(2) 0.034(3) 0.015(2) 0.075(3) F2 0.084(2) 0.153(3) 0.0631(19) -0.034(2) -0.0468(17) 0.041(2) B2 0.065(3) 0.043(3) 0.040(3) 0.003(2) -0.008(2) 0.004(2) F3 0.082(2) 0.073(2) 0.0621(18) 0.0205(14) -0.0147(15) 0.0072(16) F4 0.182(8) 0.059(4) 0.142(8) 0.049(4) -0.091(7) -0.039(4) F5 0.065(3) 0.160(8) 0.077(4) 0.022(4) 0.027(3) 0.051(4) F6 0.053(3) 0.134(5) 0.074(3) -0.062(3) -0.003(2) 0.007(3) F4X 0.087(7) 0.055(6) 0.131(10) -0.007(6) 0.039(6) 0.017(5) F5X 0.185(15) 0.082(10) 0.200(19) 0.049(9) -0.107(13) -0.087(12) F6X 0.178(12) 0.095(11) 0.055(6) 0.034(6) 0.044(7) 0.042(9) O1 0.085(5) 0.179(8) 0.099(5) 0.000 0.018(4) 0.000 C51 0.118(7) 0.158(8) 0.113(7) 0.010(6) -0.003(6) 0.013(7) C52 0.118(7) 0.221(11) 0.189(10) -0.069(9) 0.031(7) -0.067(8) _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 1.951(3) . ? Cu1 N5 1.960(4) . ? Cu1 N1 1.980(4) . ? Cu1 N3 1.992(3) . ? N1 S1 1.602(4) . ? S1 C1 1.767(8) . ? S1 C7 1.775(5) . ? C1 C6 1.359(9) . ? C1 C2 1.410(8) . ? C2 C3 1.343(11) . ? C3 C4 1.389(12) . ? C4 C5 1.381(12) . ? C5 C6 1.344(12) . ? C7 C12 1.367(7) . ? C7 C8 1.381(6) . ? C8 C9 1.383(7) . ? C9 C10 1.373(7) . ? C10 C11 1.367(8) . ? C11 C12 1.386(8) . ? N2 S2 1.591(3) . ? S2 C19 1.793(4) . ? S2 C13 1.809(4) . ? C13 C18 1.380(6) . ? C13 C14 1.388(5) . ? C14 C15 1.381(6) . ? C15 C16 1.375(7) . ? C16 C17 1.383(8) . ? C17 C18 1.395(7) . ? C19 C24 1.370(6) . ? C19 C20 1.380(6) . ? C20 C21 1.372(6) . ? C21 C22 1.361(7) . ? C22 C23 1.349(7) . ? C23 C24 1.394(7) . ? N3 S3 1.594(3) . ? S3 C31 1.790(5) . ? S3 C25 1.798(5) . ? C25 C30 1.361(7) . ? C25 C26 1.372(7) . ? C26 C27 1.359(10) . ? C27 C28 1.346(12) . ? C28 C29 1.397(12) . ? C29 C30 1.403(7) . ? C31 C32 1.342(7) . ? C31 C36 1.387(7) . ? C32 C33 1.424(8) . ? C33 C34 1.351(9) . ? C34 C35 1.327(10) . ? C35 C36 1.388(9) . ? N5 C49 1.277(7) . ? C49 N4 1.379(7) . ? C49 C50 1.509(7) . ? C49 N4X 1.576(15) . ? N4 S4 1.625(6) . ? S4 C43 1.822(7) . ? S4 C37 1.832(6) . ? N4X S4X 1.637(14) . ? S4X C43 1.900(8) . ? S4X C37 1.920(7) . ? C37 C38 1.348(8) . ? C37 C42 1.370(8) . ? C38 C39 1.365(9) . ? C39 C40 1.364(9) . ? C40 C41 1.370(9) . ? C41 C42 1.364(8) . ? C43 C48 1.356(10) . ? C43 C44 1.362(10) . ? C44 C45 1.346(10) . ? C45 C46 1.323(10) . ? C46 C47 1.384(10) . ? C47 C48 1.406(10) . ? B1 F1 1.370(8) 3_755 ? B1 F1 1.370(8) . ? B1 F2 1.373(7) 3_755 ? B1 F2 1.373(7) . ? B2 F5X 1.325(12) . ? B2 F6X 1.332(10) . ? B2 F4 1.340(7) . ? B2 F5 1.360(8) . ? B2 F6 1.383(7) . ? B2 F3 1.389(6) . ? B2 F4X 1.407(10) . ? O1 C51 1.331(9) . ? O1 C51 1.331(9) 3_755 ? C51 C52 1.317(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 N2 Cu1 N5 154.96(18) . . ? N2 Cu1 N1 89.79(15) . . ? N5 Cu1 N1 93.95(16) . . ? N2 Cu1 N3 96.01(13) . . ? N5 Cu1 N3 94.02(14) . . ? N1 Cu1 N3 147.5(2) . . ? S1 N1 Cu1 120.4(2) . . ? N1 S1 C1 110.3(3) . . ? N1 S1 C7 108.4(2) . . ? C1 S1 C7 97.4(2) . . ? C6 C1 C2 120.1(8) . . ? C6 C1 S1 121.2(6) . . ? C2 C1 S1 118.7(6) . . ? C3 C2 C1 121.2(8) . . ? C2 C3 C4 117.5(8) . . ? C5 C4 C3 121.1(10) . . ? C6 C5 C4 120.8(9) . . ? C5 C6 C1 119.3(8) . . ? C12 C7 C8 120.7(5) . . ? C12 C7 S1 118.0(4) . . ? C8 C7 S1 121.3(4) . . ? C7 C8 C9 119.2(5) . . ? C10 C9 C8 120.2(5) . . ? C11 C10 C9 120.2(5) . . ? C10 C11 C12 120.1(5) . . ? C7 C12 C11 119.6(5) . . ? S2 N2 Cu1 127.59(19) . . ? N2 S2 C19 108.42(18) . . ? N2 S2 C13 108.31(18) . . ? C19 S2 C13 97.82(18) . . ? C18 C13 C14 121.4(4) . . ? C18 C13 S2 119.1(3) . . ? C14 C13 S2 119.5(3) . . ? C15 C14 C13 119.2(4) . . ? C16 C15 C14 120.4(5) . . ? C15 C16 C17 120.1(5) . . ? C16 C17 C18 120.5(5) . . ? C13 C18 C17 118.4(5) . . ? C24 C19 C20 119.3(4) . . ? C24 C19 S2 119.7(3) . . ? C20 C19 S2 121.0(3) . . ? C21 C20 C19 120.5(4) . . ? C22 C21 C20 120.4(5) . . ? C23 C22 C21 119.4(5) . . ? C22 C23 C24 121.5(5) . . ? C19 C24 C23 118.8(5) . . ? S3 N3 Cu1 115.46(19) . . ? N3 S3 C31 108.8(2) . . ? N3 S3 C25 111.4(2) . . ? C31 S3 C25 100.3(2) . . ? C30 C25 C26 122.1(5) . . ? C30 C25 S3 120.1(4) . . ? C26 C25 S3 117.5(4) . . ? C27 C26 C25 118.8(7) . . ? C28 C27 C26 121.3(8) . . ? C27 C28 C29 120.7(7) . . ? C28 C29 C30 118.4(7) . . ? C25 C30 C29 118.7(6) . . ? C32 C31 C36 120.5(5) . . ? C32 C31 S3 123.0(4) . . ? C36 C31 S3 116.5(4) . . ? C31 C32 C33 118.6(6) . . ? C34 C33 C32 118.8(6) . . ? C35 C34 C33 123.4(7) . . ? C34 C35 C36 118.1(7) . . ? C31 C36 C35 120.5(7) . . ? C49 N5 Cu1 118.5(4) . . ? N5 C49 N4 106.6(5) . . ? N5 C49 C50 121.3(4) . . ? N4 C49 C50 132.1(6) . . ? N5 C49 N4X 154.7(7) . . ? N4 C49 N4X 48.1(5) . . ? C50 C49 N4X 84.0(6) . . ? C49 N4 S4 113.0(4) . . ? N4 S4 C43 98.6(3) . . ? N4 S4 C37 101.8(3) . . ? C43 S4 C37 99.8(3) . . ? C49 N4X S4X 99.3(8) . . ? N4X S4X C43 94.3(5) . . ? N4X S4X C37 89.2(5) . . ? C43 S4X C37 94.0(3) . . ? C38 C37 C42 122.6(5) . . ? C38 C37 S4 109.8(5) . . ? C42 C37 S4 127.4(5) . . ? C38 C37 S4X 147.6(5) . . ? C42 C37 S4X 89.2(4) . . ? S4 C37 S4X 39.81(16) . . ? C37 C38 C39 118.2(6) . . ? C40 C39 C38 120.6(6) . . ? C39 C40 C41 120.2(6) . . ? C42 C41 C40 119.8(6) . . ? C41 C42 C37 118.5(5) . . ? C48 C43 C44 122.5(6) . . ? C48 C43 S4 130.0(6) . . ? C44 C43 S4 107.3(7) . . ? C48 C43 S4X 90.1(6) . . ? C44 C43 S4X 147.4(7) . . ? S4 C43 S4X 40.16(18) . . ? C45 C44 C43 118.6(8) . . ? C46 C45 C44 122.1(7) . . ? C45 C46 C47 120.3(7) . . ? C46 C47 C48 118.9(7) . . ? C43 C48 C47 117.5(6) . . ? F1 B1 F1 108.8(9) 3_755 . ? F1 B1 F2 109.3(2) 3_755 3_755 ? F1 B1 F2 109.0(3) . 3_755 ? F1 B1 F2 109.0(3) 3_755 . ? F1 B1 F2 109.3(2) . . ? F2 B1 F2 111.3(9) 3_755 . ? F5X B2 F6X 123.2(12) . . ? F5X B2 F4 128.7(9) . . ? F6X B2 F4 49.3(6) . . ? F5X B2 F5 34.2(9) . . ? F6X B2 F5 137.2(8) . . ? F4 B2 F5 109.4(7) . . ? F5X B2 F6 70.7(10) . . ? F6X B2 F6 64.2(7) . . ? F4 B2 F6 109.8(6) . . ? F5 B2 F6 104.0(5) . . ? F5X B2 F3 114.1(8) . . ? F6X B2 F3 110.0(7) . . ? F4 B2 F3 114.6(5) . . ? F5 B2 F3 112.7(5) . . ? F6 B2 F3 105.7(5) . . ? F5X B2 F4X 102.8(11) . . ? F6X B2 F4X 107.3(8) . . ? F4 B2 F4X 58.1(6) . . ? F5 B2 F4X 68.8(6) . . ? F6 B2 F4X 159.4(7) . . ? F3 B2 F4X 94.9(6) . . ? C51 O1 C51 123.2(11) . 3_755 ? C52 C51 O1 123.2(10) . . ? 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 N1 H1A F2 0.86(3) 2.35(4) 3.155(5) 155(6) . N2 H2A F2 0.86(3) 2.09(3) 2.948(4) 175(4) . N3 H3A F3 0.86(3) 2.34(3) 3.178(4) 169(5) 4 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.510 _refine_diff_density_min -1.026 _refine_diff_density_rms 0.070 # END of data for (3) data_(4) _database_code_depnum_ccdc_archive 'CCDC 227321' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H44 Cl2 Cu N4 O8 S4' _chemical_formula_weight 1067.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 17.1827(7) _cell_length_b 20.0047(9) _cell_length_c 14.4205(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.157(2) _cell_angle_gamma 90.00 _cell_volume 4826.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10767 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.77 _exptl_crystal_description block _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2204 _exptl_absorpt_coefficient_mu 0.794 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_T_max 0.785 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21218 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 29.01 _reflns_number_total 5864 _reflns_number_gt 4862 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0367P)^2^+5.3645P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except NH coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5864 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Cu1 Cu 0.5000 0.684562(12) 0.2500 0.01834(7) Uani 1 2 d S . . N1 N 0.43572(9) 0.61956(7) 0.16343(10) 0.0273(3) Uani 1 1 d . . . H1A H 0.4121(13) 0.6297(11) 0.1125(16) 0.041 Uiso 1 1 d . . . S1 S 0.40384(2) 0.551153(19) 0.19748(3) 0.02078(9) Uani 1 1 d . . . C1 C 0.29798(10) 0.55801(8) 0.19033(11) 0.0236(3) Uani 1 1 d . . . C2 C 0.26097(11) 0.61959(9) 0.17535(14) 0.0351(4) Uani 1 1 d . . . H2 H 0.2897 0.6581 0.1638 0.042 Uiso 1 1 calc R . . C3 C 0.18058(13) 0.62407(11) 0.17759(17) 0.0459(5) Uani 1 1 d . . . H3 H 0.1540 0.6659 0.1664 0.055 Uiso 1 1 calc R . . C4 C 0.13921(12) 0.56842(11) 0.19583(15) 0.0406(5) Uani 1 1 d . . . H4 H 0.0843 0.5720 0.1970 0.049 Uiso 1 1 calc R . . C5 C 0.17749(11) 0.50755(10) 0.21235(14) 0.0356(4) Uani 1 1 d . . . H5 H 0.1490 0.4694 0.2257 0.043 Uiso 1 1 calc R . . C6 C 0.25717(10) 0.50164(9) 0.20967(12) 0.0294(4) Uani 1 1 d . . . H6 H 0.2836 0.4597 0.2209 0.035 Uiso 1 1 calc R . . C7 C 0.40537(9) 0.48788(8) 0.11047(11) 0.0223(3) Uani 1 1 d . . . C8 C 0.42118(11) 0.42306(9) 0.14342(15) 0.0331(4) Uani 1 1 d . . . H8 H 0.4288 0.4131 0.2093 0.040 Uiso 1 1 calc R . . C9 C 0.42557(12) 0.37297(10) 0.07799(19) 0.0468(6) Uani 1 1 d . . . H9 H 0.4363 0.3282 0.0990 0.056 Uiso 1 1 calc R . . C10 C 0.41447(13) 0.38804(12) -0.01683(19) 0.0535(7) Uani 1 1 d . . . H10 H 0.4173 0.3536 -0.0613 0.064 Uiso 1 1 calc R . . C11 C 0.39919(14) 0.45292(14) -0.04807(16) 0.0533(6) Uani 1 1 d . . . H11 H 0.3915 0.4627 -0.1140 0.064 Uiso 1 1 calc R . . C12 C 0.39491(11) 0.50398(11) 0.01557(13) 0.0348(4) Uani 1 1 d . . . H12 H 0.3851 0.5488 -0.0057 0.042 Uiso 1 1 calc R . . N2 N 0.51765(9) 0.74866(7) 0.35484(10) 0.0271(3) Uani 1 1 d . . . H2A H 0.5431(13) 0.7398(11) 0.4066(16) 0.041 Uiso 1 1 d . . . S2 S 0.47688(2) 0.820611(19) 0.35107(3) 0.02267(9) Uani 1 1 d . . . C13 C 0.42023(10) 0.82468(8) 0.44048(12) 0.0248(3) Uani 1 1 d . . . C14 C 0.45549(12) 0.81440(8) 0.53570(13) 0.0301(4) Uani 1 1 d . . . H14 H 0.5116 0.8080 0.5559 0.036 Uiso 1 1 calc R . . C15 C 0.40744(14) 0.81361(9) 0.60121(15) 0.0401(5) Uani 1 1 d . . . H15 H 0.4304 0.8059 0.6667 0.048 Uiso 1 1 calc R . . C16 C 0.32609(15) 0.82407(11) 0.57089(19) 0.0521(6) Uani 1 1 d . . . H16 H 0.2935 0.8240 0.6160 0.063 Uiso 1 1 calc R . . C17 C 0.29207(13) 0.83446(13) 0.4769(2) 0.0551(6) Uani 1 1 d . . . H17 H 0.2361 0.8418 0.4575 0.066 Uiso 1 1 calc R . . C18 C 0.33837(11) 0.83450(10) 0.40898(16) 0.0395(5) Uani 1 1 d . . . H18 H 0.3147 0.8410 0.3434 0.047 Uiso 1 1 calc R . . C19 C 0.55358(10) 0.88105(8) 0.39547(11) 0.0235(3) Uani 1 1 d . . . C20 C 0.63295(11) 0.86344(9) 0.40860(13) 0.0311(4) Uani 1 1 d . . . H20 H 0.6477 0.8187 0.3987 0.037 Uiso 1 1 calc R . . C21 C 0.69121(11) 0.91243(10) 0.43667(14) 0.0368(4) Uani 1 1 d . . . H21 H 0.7461 0.9008 0.4471 0.044 Uiso 1 1 calc R . . C22 C 0.66981(12) 0.97764(10) 0.44940(13) 0.0342(4) Uani 1 1 d . . . H22 H 0.7099 1.0107 0.4683 0.041 Uiso 1 1 calc R . . C23 C 0.59005(12) 0.99489(9) 0.43468(14) 0.0351(4) Uani 1 1 d . . . H23 H 0.5755 1.0399 0.4432 0.042 Uiso 1 1 calc R . . C24 C 0.53126(11) 0.94671(8) 0.40757(14) 0.0310(4) Uani 1 1 d . . . H24 H 0.4764 0.9584 0.3974 0.037 Uiso 1 1 calc R . . Cl1 Cl 0.64416(3) 0.68553(2) 0.64093(3) 0.02856(10) Uani 1 1 d . . . O1 O 0.63838(11) 0.61549(7) 0.65826(12) 0.0539(4) Uani 1 1 d . . . O2 O 0.62617(10) 0.69575(8) 0.53946(10) 0.0486(4) Uani 1 1 d . . . O3 O 0.72356(9) 0.70819(9) 0.68096(12) 0.0582(5) Uani 1 1 d . . . O4 O 0.58820(8) 0.72167(7) 0.68198(11) 0.0420(3) Uani 1 1 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 Cu1 0.02127(14) 0.01494(13) 0.01813(13) 0.000 0.00308(10) 0.000 N1 0.0356(8) 0.0211(7) 0.0212(7) 0.0036(5) -0.0021(6) -0.0084(6) S1 0.02459(19) 0.01822(18) 0.01801(18) 0.00042(14) 0.00166(14) -0.00239(14) C1 0.0250(8) 0.0255(8) 0.0188(7) -0.0032(6) 0.0018(6) 0.0005(6) C2 0.0361(10) 0.0238(9) 0.0444(11) -0.0037(8) 0.0071(8) 0.0032(7) C3 0.0398(11) 0.0355(11) 0.0608(14) -0.0093(10) 0.0083(10) 0.0139(9) C4 0.0303(10) 0.0488(12) 0.0432(11) -0.0099(9) 0.0093(8) 0.0043(9) C5 0.0295(9) 0.0430(11) 0.0342(10) -0.0005(8) 0.0073(8) -0.0046(8) C6 0.0286(9) 0.0284(9) 0.0301(9) 0.0031(7) 0.0046(7) 0.0010(7) C7 0.0190(7) 0.0228(8) 0.0246(8) -0.0044(6) 0.0040(6) -0.0019(6) C8 0.0315(9) 0.0228(8) 0.0442(11) -0.0015(7) 0.0067(8) -0.0012(7) C9 0.0328(10) 0.0276(10) 0.0801(17) -0.0178(10) 0.0132(10) 0.0004(8) C10 0.0374(11) 0.0567(15) 0.0711(17) -0.0400(13) 0.0224(11) -0.0053(10) C11 0.0543(14) 0.0767(18) 0.0328(11) -0.0213(11) 0.0181(10) -0.0035(12) C12 0.0365(10) 0.0430(11) 0.0254(9) -0.0026(8) 0.0083(8) 0.0017(8) N2 0.0389(8) 0.0194(7) 0.0200(7) -0.0022(5) 0.0002(6) 0.0080(6) S2 0.0275(2) 0.01802(19) 0.02048(19) -0.00101(14) 0.00130(15) 0.00345(15) C13 0.0266(8) 0.0171(7) 0.0311(9) -0.0028(6) 0.0072(7) 0.0002(6) C14 0.0358(9) 0.0238(8) 0.0314(9) -0.0006(7) 0.0094(8) 0.0026(7) C15 0.0590(13) 0.0285(10) 0.0378(11) -0.0025(8) 0.0216(10) -0.0033(9) C16 0.0544(14) 0.0450(13) 0.0695(17) -0.0115(11) 0.0406(13) -0.0110(10) C17 0.0289(10) 0.0599(15) 0.0806(18) -0.0138(13) 0.0213(11) -0.0048(10) C18 0.0280(9) 0.0383(11) 0.0499(12) -0.0050(9) 0.0041(8) 0.0002(8) C19 0.0286(8) 0.0214(8) 0.0207(8) -0.0010(6) 0.0057(6) 0.0002(6) C20 0.0321(9) 0.0273(9) 0.0344(9) -0.0057(7) 0.0085(7) 0.0042(7) C21 0.0281(9) 0.0413(11) 0.0424(11) -0.0072(9) 0.0107(8) -0.0009(8) C22 0.0368(10) 0.0349(10) 0.0329(10) -0.0057(8) 0.0123(8) -0.0095(8) C23 0.0425(11) 0.0214(9) 0.0425(11) -0.0046(7) 0.0122(9) -0.0023(8) C24 0.0315(9) 0.0216(8) 0.0395(10) -0.0020(7) 0.0072(8) 0.0033(7) Cl1 0.0317(2) 0.0277(2) 0.0239(2) 0.00058(15) 0.00154(16) 0.00719(16) O1 0.0849(12) 0.0295(8) 0.0536(10) 0.0113(7) 0.0289(9) 0.0160(8) O2 0.0603(10) 0.0549(9) 0.0269(7) 0.0116(6) 0.0020(7) 0.0095(8) O3 0.0297(8) 0.0768(12) 0.0614(11) -0.0272(9) -0.0032(7) 0.0056(8) O4 0.0387(8) 0.0373(8) 0.0522(9) -0.0087(6) 0.0148(7) 0.0064(6) _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 1.9527(14) . ? Cu1 N2 1.9527(14) 2_655 ? Cu1 N1 1.9600(14) . ? Cu1 N1 1.9600(14) 2_655 ? N1 S1 1.5926(14) . ? S1 C7 1.7866(16) . ? S1 C1 1.8034(17) . ? C1 C2 1.381(2) . ? C1 C6 1.389(2) . ? C2 C3 1.392(3) . ? C3 C4 1.378(3) . ? C4 C5 1.379(3) . ? C5 C6 1.384(2) . ? C7 C12 1.377(2) . ? C7 C8 1.387(2) . ? C8 C9 1.390(3) . ? C9 C10 1.370(4) . ? C10 C11 1.379(4) . ? C11 C12 1.386(3) . ? N2 S2 1.5963(14) . ? S2 C13 1.7855(18) . ? S2 C19 1.7957(17) . ? C13 C14 1.384(3) . ? C13 C18 1.390(2) . ? C14 C15 1.389(3) . ? C15 C16 1.382(3) . ? C16 C17 1.364(4) . ? C17 C18 1.396(3) . ? C19 C20 1.379(2) . ? C19 C24 1.390(2) . ? C20 C21 1.393(3) . ? C21 C22 1.379(3) . ? C22 C23 1.382(3) . ? C23 C24 1.387(3) . ? Cl1 O3 1.4288(15) . ? Cl1 O1 1.4308(15) . ? Cl1 O4 1.4342(14) . ? Cl1 O2 1.4396(14) . ? 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 N2 97.91(9) . 2_655 ? N2 Cu1 N1 153.44(7) . . ? N2 Cu1 N1 88.68(6) 2_655 . ? N2 Cu1 N1 88.68(6) . 2_655 ? N2 Cu1 N1 153.44(7) 2_655 2_655 ? N1 Cu1 N1 96.87(9) . 2_655 ? S1 N1 Cu1 123.87(9) . . ? N1 S1 C7 109.34(8) . . ? N1 S1 C1 109.29(8) . . ? C7 S1 C1 100.93(7) . . ? C2 C1 C6 121.34(16) . . ? C2 C1 S1 119.97(13) . . ? C6 C1 S1 118.38(13) . . ? C1 C2 C3 118.55(18) . . ? C4 C3 C2 120.69(19) . . ? C3 C4 C5 119.99(18) . . ? C4 C5 C6 120.46(18) . . ? C5 C6 C1 118.96(17) . . ? C12 C7 C8 122.02(17) . . ? C12 C7 S1 120.84(14) . . ? C8 C7 S1 117.06(13) . . ? C7 C8 C9 118.6(2) . . ? C10 C9 C8 120.1(2) . . ? C9 C10 C11 120.38(19) . . ? C10 C11 C12 120.8(2) . . ? C7 C12 C11 118.1(2) . . ? S2 N2 Cu1 125.18(9) . . ? N2 S2 C13 108.89(8) . . ? N2 S2 C19 108.32(8) . . ? C13 S2 C19 100.86(8) . . ? C14 C13 C18 121.81(18) . . ? C14 C13 S2 121.47(14) . . ? C18 C13 S2 116.61(15) . . ? C13 C14 C15 118.85(19) . . ? C16 C15 C14 119.9(2) . . ? C17 C16 C15 120.7(2) . . ? C16 C17 C18 120.9(2) . . ? C13 C18 C17 117.8(2) . . ? C20 C19 C24 121.09(16) . . ? C20 C19 S2 119.97(13) . . ? C24 C19 S2 118.67(13) . . ? C19 C20 C21 118.87(17) . . ? C22 C21 C20 120.55(18) . . ? C21 C22 C23 120.06(17) . . ? C22 C23 C24 120.22(17) . . ? C23 C24 C19 119.20(17) . . ? O3 Cl1 O1 109.76(11) . . ? O3 Cl1 O4 109.97(9) . . ? O1 Cl1 O4 109.99(9) . . ? O3 Cl1 O2 109.26(11) . . ? O1 Cl1 O2 108.01(10) . . ? O4 Cl1 O2 109.81(9) . . ? 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 N1 H1A O2 0.78(2) 2.51(2) 3.255(2) 159(2) 2_655 N2 H2A O2 0.79(2) 2.29(2) 3.070(2) 168(2) . _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.352 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.055 # END of data for (4) data_(5) _database_code_depnum_ccdc_archive 'CCDC 227322' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H51 Cl2 Cu N4 O9.50 S4' _chemical_formula_weight 1122.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.7535(8) _cell_length_b 10.3848(6) _cell_length_c 35.2904(19) _cell_angle_alpha 90.00 _cell_angle_beta 99.713(2) _cell_angle_gamma 90.00 _cell_volume 5329.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11689 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.35 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.736 _exptl_absorpt_correction_T_max 0.869 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 37365 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9390 _reflns_number_gt 7217 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0640P)^2^+18.8264P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except NH coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9390 _refine_ls_number_parameters 675 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1736 _refine_ls_wR_factor_gt 0.1611 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 -0.23245(7) 0.2500 0.0307(2) Uani 1 2 d S . . N1 N -0.0086(4) -0.0990(4) 0.21039(12) 0.0540(13) Uani 1 1 d D . . H1A H -0.016(5) -0.024(4) 0.215(2) 0.081 Uiso 1 1 d D . . S1 S -0.04528(11) -0.13063(12) 0.16622(3) 0.0453(3) Uani 1 1 d . . . C1 C 0.0000(4) -0.0137(5) 0.13747(13) 0.0412(12) Uani 1 1 d . . . C2 C -0.0049(4) 0.1155(5) 0.14481(15) 0.0515(14) Uani 1 1 d . . . H2 H -0.0357 0.1451 0.1647 0.062 Uiso 1 1 calc R . . C3 C 0.0351(5) 0.2018(6) 0.12310(16) 0.0599(16) Uani 1 1 d . . . H3 H 0.0334 0.2911 0.1287 0.072 Uiso 1 1 calc R . . C4 C 0.0770(4) 0.1614(7) 0.09363(16) 0.0572(16) Uani 1 1 d . . . H4 H 0.1032 0.2224 0.0786 0.069 Uiso 1 1 calc R . . C5 C 0.0814(4) 0.0327(7) 0.08575(16) 0.0611(17) Uani 1 1 d . . . H5 H 0.1106 0.0047 0.0652 0.073 Uiso 1 1 calc R . . C6 C 0.0430(4) -0.0580(6) 0.10783(15) 0.0550(15) Uani 1 1 d . . . H6 H 0.0463 -0.1475 0.1027 0.066 Uiso 1 1 calc R . . C7 C -0.1664(4) -0.0969(5) 0.15468(16) 0.0516(14) Uani 1 1 d . . . C8 C -0.2141(5) -0.0616(7) 0.1834(2) 0.0702(19) Uani 1 1 d . . . H8 H -0.1827 -0.0457 0.2088 0.084 Uiso 1 1 calc R . . C9 C -0.3086(6) -0.0497(9) 0.1745(3) 0.093(3) Uani 1 1 d . . . H9 H -0.3424 -0.0243 0.1939 0.112 Uiso 1 1 calc R . . C10 C -0.3540(6) -0.0739(9) 0.1382(3) 0.094(3) Uani 1 1 d . . . H10 H -0.4191 -0.0666 0.1326 0.113 Uiso 1 1 calc R . . C11 C -0.3050(5) -0.1094(8) 0.1095(2) 0.082(2) Uani 1 1 d . . . H11 H -0.3366 -0.1249 0.0841 0.099 Uiso 1 1 calc R . . C12 C -0.2109(5) -0.1221(6) 0.11758(17) 0.0634(17) Uani 1 1 d . . . H12 H -0.1771 -0.1476 0.0982 0.076 Uiso 1 1 calc R . . N2 N 0.0493(3) -0.3664(4) 0.22047(12) 0.0384(10) Uani 1 1 d D . . H2A H 0.039(4) -0.442(4) 0.2207(17) 0.058 Uiso 1 1 d D . . S2 S 0.12921(9) -0.34170(12) 0.19582(3) 0.0382(3) Uani 1 1 d . . . C13 C 0.0944(3) -0.4116(4) 0.14921(13) 0.0325(10) Uani 1 1 d . . . C14 C 0.0021(3) -0.4369(5) 0.13717(15) 0.0416(12) Uani 1 1 d . . . H14 H -0.0399 -0.4317 0.1548 0.050 Uiso 1 1 calc R . . C15 C -0.0282(4) -0.4699(6) 0.09927(17) 0.0529(14) Uani 1 1 d . . . H15 H -0.0916 -0.4864 0.0905 0.063 Uiso 1 1 calc R . . C16 C 0.0336(4) -0.4789(6) 0.07405(16) 0.0539(15) Uani 1 1 d . . . H16 H 0.0121 -0.5003 0.0479 0.065 Uiso 1 1 calc R . . C17 C 0.1249(4) -0.4573(6) 0.08624(15) 0.0494(14) Uani 1 1 d . . . H17 H 0.1672 -0.4668 0.0689 0.059 Uiso 1 1 calc R . . C18 C 0.1563(4) -0.4214(5) 0.12415(14) 0.0417(12) Uani 1 1 d . . . H18 H 0.2196 -0.4037 0.1327 0.050 Uiso 1 1 calc R . . C19 C 0.2258(4) -0.4369(7) 0.21499(15) 0.0513(14) Uani 1 1 d . . . C20 C 0.2237(5) -0.5685(7) 0.21373(17) 0.0623(17) Uani 1 1 d . . . H20 H 0.1717 -0.6125 0.2001 0.075 Uiso 1 1 calc R . . C21 C 0.2994(6) -0.6371(10) 0.2328(2) 0.093(3) Uani 1 1 d . . . H21 H 0.2993 -0.7286 0.2326 0.111 Uiso 1 1 calc R . . C22 C 0.3745(7) -0.5704(15) 0.2520(3) 0.121(5) Uani 1 1 d . . . H22 H 0.4262 -0.6171 0.2647 0.145 Uiso 1 1 calc R . . C23 C 0.3760(6) -0.4397(15) 0.2532(2) 0.120(4) Uani 1 1 d . . . H23 H 0.4283 -0.3959 0.2666 0.144 Uiso 1 1 calc R . . C24 C 0.3012(4) -0.3704(9) 0.23470(18) 0.080(2) Uani 1 1 d . . . H24 H 0.3013 -0.2789 0.2355 0.096 Uiso 1 1 calc R . . Cu2 Cu 0.5000 0.5000 0.0000 0.0466(3) Uani 1 2 d S . . N3 N 0.4403(3) 0.4501(5) 0.04366(12) 0.0506(12) Uani 1 1 d D . . H3A H 0.387(3) 0.433(7) 0.0409(19) 0.076 Uiso 1 1 d D . . S3 S 0.47363(9) 0.49837(16) 0.08697(3) 0.0490(4) Uani 1 1 d . . . C25 C 0.4397(3) 0.3791(6) 0.11827(13) 0.0448(13) Uani 1 1 d . . . C26 C 0.5086(4) 0.3266(7) 0.14548(15) 0.0552(16) Uani 1 1 d . . . H26 H 0.5696 0.3589 0.1487 0.066 Uiso 1 1 calc R . . C27 C 0.4860(4) 0.2253(7) 0.16806(16) 0.0616(17) Uani 1 1 d . . . H27 H 0.5323 0.1879 0.1868 0.074 Uiso 1 1 calc R . . C28 C 0.3975(5) 0.1788(7) 0.16342(17) 0.0635(17) Uani 1 1 d . . . H28 H 0.3830 0.1085 0.1785 0.076 Uiso 1 1 calc R . . C29 C 0.3299(4) 0.2349(7) 0.13664(18) 0.0649(17) Uani 1 1 d . . . H29 H 0.2685 0.2042 0.1340 0.078 Uiso 1 1 calc R . . C30 C 0.3501(4) 0.3346(6) 0.11373(16) 0.0547(15) Uani 1 1 d . . . H30 H 0.3034 0.3721 0.0952 0.066 Uiso 1 1 calc R . . C31 C 0.4040(3) 0.6319(6) 0.09747(14) 0.0456(13) Uani 1 1 d . . . C32 C 0.4185(4) 0.6853(7) 0.13445(16) 0.0605(17) Uani 1 1 d . . . H32 H 0.4610 0.6472 0.1546 0.073 Uiso 1 1 calc R . . C33 C 0.3700(5) 0.7946(8) 0.14122(19) 0.072(2) Uani 1 1 d . . . H33 H 0.3798 0.8324 0.1661 0.086 Uiso 1 1 calc R . . C34 C 0.3072(5) 0.8493(7) 0.11213(19) 0.0663(17) Uani 1 1 d . . . H34 H 0.2729 0.9229 0.1172 0.080 Uiso 1 1 calc R . . C35 C 0.2943(4) 0.7968(7) 0.07568(18) 0.0617(16) Uani 1 1 d . . . H35 H 0.2517 0.8352 0.0557 0.074 Uiso 1 1 calc R . . C36 C 0.3432(4) 0.6881(6) 0.06800(15) 0.0519(14) Uani 1 1 d . . . H36 H 0.3350 0.6528 0.0428 0.062 Uiso 1 1 calc R . . N4 N 0.6251(3) 0.4736(5) 0.03096(12) 0.0431(11) Uani 1 1 d D . . H4A H 0.666(3) 0.512(6) 0.0240(18) 0.065 Uiso 1 1 d D . . S4 S 0.65519(8) 0.34845(13) 0.05585(3) 0.0410(3) Uani 1 1 d . . . C37 C 0.7138(3) 0.3964(5) 0.10288(13) 0.0349(11) Uani 1 1 d . . . C38 C 0.7484(4) 0.2996(6) 0.12870(14) 0.0454(13) Uani 1 1 d . . . H38 H 0.7469 0.2120 0.1208 0.055 Uiso 1 1 calc R . . C39 C 0.7850(4) 0.3343(7) 0.16628(15) 0.0554(16) Uani 1 1 d . . . H39 H 0.8092 0.2700 0.1843 0.066 Uiso 1 1 calc R . . C40 C 0.7864(3) 0.4596(7) 0.17716(15) 0.0498(15) Uani 1 1 d . . . H40 H 0.8116 0.4819 0.2029 0.060 Uiso 1 1 calc R . . C41 C 0.7518(4) 0.5561(6) 0.15149(15) 0.0486(13) Uani 1 1 d . . . H41 H 0.7531 0.6434 0.1596 0.058 Uiso 1 1 calc R . . C42 C 0.7147(3) 0.5233(5) 0.11339(15) 0.0423(12) Uani 1 1 d . . . H42 H 0.6907 0.5877 0.0953 0.051 Uiso 1 1 calc R . . C43 C 0.7493(4) 0.2691(5) 0.03902(14) 0.0457(13) Uani 1 1 d . . . C44 C 0.8183(4) 0.3369(6) 0.02608(16) 0.0515(14) Uani 1 1 d . . . H44 H 0.8169 0.4283 0.0257 0.062 Uiso 1 1 calc R . . C45 C 0.8900(4) 0.2718(7) 0.01367(18) 0.0673(19) Uani 1 1 d . . . H45 H 0.9368 0.3180 0.0040 0.081 Uiso 1 1 calc R . . C46 C 0.8925(7) 0.1408(9) 0.0155(2) 0.094(3) Uani 1 1 d . . . H46 H 0.9415 0.0957 0.0071 0.112 Uiso 1 1 calc R . . C47 C 0.8280(10) 0.0760(8) 0.0288(3) 0.119(4) Uani 1 1 d . . . H47 H 0.8328 -0.0150 0.0309 0.142 Uiso 1 1 calc R . . C48 C 0.7531(7) 0.1370(7) 0.0398(2) 0.093(3) Uani 1 1 d . . . H48 H 0.7052 0.0883 0.0477 0.112 Uiso 1 1 calc R . . Cl1 Cl 0.0000 -0.73990(15) 0.2500 0.0369(4) Uani 1 2 d SDU . . O1 O 0.0047(3) -0.6595(4) 0.21735(12) 0.0627(11) Uani 1 1 d DU . . O2 O -0.0789(3) -0.8213(4) 0.24157(13) 0.0683(12) Uani 1 1 d DU . . Cl2 Cl 0.5000 -0.0684(4) 0.2500 0.0992(10) Uani 1 2 d SDU . . O3 O 0.5110(5) -0.1344(10) 0.21867(19) 0.162(4) Uani 1 1 d DU A . O4 O 0.3907(7) -0.0279(16) 0.2379(3) 0.142(7) Uani 0.568(18) 1 d PDU A 1 O4X O 0.4580(11) 0.0485(11) 0.2497(4) 0.094(6) Uiso 0.432(18) 1 d PDU . 2 Cl3 Cl 0.80580(13) 0.71918(18) -0.00090(4) 0.0684(5) Uani 1 1 d U . . O5 O 0.7680(5) 0.6110(6) -0.02141(17) 0.109(2) Uani 1 1 d U . . O6 O 0.7608(6) 0.7263(8) 0.03047(17) 0.148(3) Uani 1 1 d U . . O7 O 0.7810(6) 0.8211(7) -0.02795(17) 0.134(3) Uani 1 1 d U . . O8 O 0.8918(4) 0.7292(14) 0.0096(3) 0.229(6) Uani 1 1 d U . . O9 O 0.5000 1.0000 0.0000 0.149(5) Uani 1 2 d S . . C49 C 0.5498(9) 0.9289(13) -0.0586(4) 0.146(5) Uani 1 1 d . . . C50 C 0.5321(14) 1.0220(19) -0.0375(6) 0.095(5) Uani 0.50 1 d P B 1 C50X C 0.5388(17) 0.908(2) -0.0183(8) 0.142(10) Uani 0.50 1 d P B 2 O10 O 0.5392(7) 0.7428(9) 0.0261(3) 0.076(3) Uani 0.50 1 d P C 1 O10X O 0.2326(16) -0.003(2) 0.2134(7) 0.247(14) Uani 0.50 1 d P D 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 0.0445(5) 0.0244(4) 0.0248(4) 0.000 0.0106(3) 0.000 N1 0.108(4) 0.029(2) 0.026(2) 0.0008(18) 0.013(2) 0.006(3) S1 0.0809(10) 0.0290(6) 0.0281(6) 0.0019(5) 0.0153(6) 0.0109(6) C1 0.054(3) 0.041(3) 0.029(2) 0.007(2) 0.008(2) 0.011(2) C2 0.077(4) 0.040(3) 0.040(3) 0.006(2) 0.019(3) 0.002(3) C3 0.087(5) 0.048(3) 0.046(3) 0.007(3) 0.014(3) -0.005(3) C4 0.053(4) 0.075(4) 0.043(3) 0.017(3) 0.007(3) 0.001(3) C5 0.060(4) 0.089(5) 0.038(3) 0.013(3) 0.021(3) 0.025(3) C6 0.077(4) 0.052(3) 0.038(3) 0.008(3) 0.017(3) 0.020(3) C7 0.073(4) 0.040(3) 0.046(3) 0.008(2) 0.020(3) -0.001(3) C8 0.092(5) 0.062(4) 0.065(4) 0.010(3) 0.036(4) 0.008(4) C9 0.090(6) 0.097(6) 0.106(7) 0.027(5) 0.054(5) 0.011(5) C10 0.072(5) 0.095(6) 0.119(7) 0.046(6) 0.028(5) 0.003(5) C11 0.073(5) 0.091(6) 0.078(5) 0.032(4) 0.000(4) -0.009(4) C12 0.085(5) 0.060(4) 0.045(3) 0.010(3) 0.012(3) -0.004(3) N2 0.050(3) 0.029(2) 0.042(2) 0.0005(19) 0.0239(19) 0.002(2) S2 0.0443(7) 0.0373(7) 0.0367(6) -0.0019(5) 0.0172(5) -0.0055(5) C13 0.035(3) 0.031(2) 0.033(2) 0.0014(19) 0.011(2) 0.003(2) C14 0.038(3) 0.037(3) 0.054(3) -0.005(2) 0.021(2) -0.002(2) C15 0.041(3) 0.059(4) 0.058(3) -0.006(3) 0.008(3) -0.006(3) C16 0.059(4) 0.065(4) 0.037(3) -0.003(3) 0.006(3) -0.005(3) C17 0.050(3) 0.067(4) 0.035(3) 0.004(3) 0.017(2) 0.000(3) C18 0.034(3) 0.056(3) 0.037(3) 0.001(2) 0.011(2) -0.001(2) C19 0.041(3) 0.081(4) 0.035(3) 0.007(3) 0.016(2) 0.005(3) C20 0.065(4) 0.075(5) 0.048(3) 0.009(3) 0.014(3) 0.029(3) C21 0.086(6) 0.134(8) 0.064(5) 0.032(5) 0.028(4) 0.061(6) C22 0.067(6) 0.237(14) 0.063(5) 0.055(8) 0.024(5) 0.065(9) C23 0.056(5) 0.245(15) 0.058(5) 0.032(8) 0.003(4) -0.012(8) C24 0.050(4) 0.141(7) 0.049(4) 0.012(4) 0.009(3) -0.014(4) Cu2 0.0312(5) 0.0844(7) 0.0247(4) 0.0163(4) 0.0064(3) 0.0186(5) N3 0.040(2) 0.084(4) 0.029(2) 0.007(2) 0.008(2) 0.002(3) S3 0.0312(6) 0.0891(11) 0.0264(6) 0.0114(6) 0.0039(5) 0.0023(7) C25 0.038(3) 0.072(4) 0.026(2) 0.009(2) 0.011(2) 0.005(3) C26 0.038(3) 0.094(5) 0.033(3) 0.009(3) 0.005(2) 0.005(3) C27 0.057(4) 0.088(5) 0.039(3) 0.013(3) 0.006(3) 0.018(3) C28 0.080(5) 0.067(4) 0.046(3) 0.009(3) 0.016(3) -0.002(4) C29 0.050(4) 0.084(5) 0.061(4) 0.011(4) 0.009(3) -0.008(3) C30 0.041(3) 0.082(4) 0.040(3) 0.009(3) 0.004(2) 0.003(3) C31 0.032(3) 0.072(4) 0.032(3) 0.002(3) 0.003(2) -0.010(3) C32 0.054(4) 0.087(5) 0.037(3) -0.004(3) -0.001(3) -0.011(3) C33 0.074(5) 0.091(5) 0.049(4) -0.017(4) 0.001(3) -0.021(4) C34 0.063(4) 0.065(4) 0.069(4) -0.011(3) 0.006(3) -0.005(3) C35 0.058(4) 0.073(4) 0.051(4) 0.002(3) 0.002(3) 0.000(3) C36 0.044(3) 0.074(4) 0.036(3) 0.007(3) 0.001(2) 0.000(3) N4 0.034(2) 0.060(3) 0.034(2) 0.020(2) 0.0002(18) -0.001(2) S4 0.0342(7) 0.0532(8) 0.0325(6) 0.0129(6) -0.0035(5) -0.0050(6) C37 0.023(2) 0.049(3) 0.032(2) 0.007(2) 0.0040(19) 0.001(2) C38 0.044(3) 0.054(3) 0.037(3) 0.009(2) 0.002(2) 0.012(3) C39 0.048(3) 0.078(5) 0.037(3) 0.015(3) -0.001(2) 0.016(3) C40 0.032(3) 0.088(5) 0.028(3) 0.003(3) 0.001(2) -0.002(3) C41 0.041(3) 0.062(4) 0.043(3) -0.001(3) 0.008(2) -0.007(3) C42 0.034(3) 0.052(3) 0.040(3) 0.011(2) 0.005(2) -0.007(2) C43 0.059(3) 0.045(3) 0.028(2) 0.006(2) -0.006(2) 0.005(3) C44 0.040(3) 0.050(3) 0.059(3) -0.006(3) -0.005(3) 0.007(3) C45 0.048(4) 0.090(5) 0.060(4) -0.021(4) -0.003(3) 0.025(3) C46 0.126(8) 0.101(7) 0.046(4) -0.016(4) -0.010(4) 0.074(6) C47 0.228(13) 0.051(5) 0.081(6) -0.004(4) 0.041(7) 0.046(7) C48 0.163(9) 0.037(4) 0.087(5) -0.002(4) 0.044(6) -0.004(5) Cl1 0.0475(10) 0.0236(8) 0.0360(8) 0.000 -0.0037(7) 0.000 O1 0.088(3) 0.043(2) 0.055(2) 0.0094(19) 0.005(2) -0.010(2) O2 0.067(3) 0.052(2) 0.079(3) 0.012(2) -0.009(2) -0.019(2) Cl2 0.117(2) 0.140(3) 0.0375(12) 0.000 0.0031(13) 0.000 O3 0.103(5) 0.285(11) 0.102(5) -0.100(6) 0.031(4) -0.057(6) O4 0.079(9) 0.245(17) 0.102(9) 0.084(10) 0.015(7) 0.028(10) Cl3 0.0827(12) 0.0824(11) 0.0448(8) -0.0046(8) 0.0245(8) -0.0356(9) O5 0.129(5) 0.101(4) 0.094(4) -0.022(4) 0.012(4) -0.004(4) O6 0.197(7) 0.192(7) 0.076(4) -0.045(4) 0.088(4) -0.095(6) O7 0.208(8) 0.126(5) 0.075(4) 0.015(4) 0.042(4) -0.024(5) O8 0.053(4) 0.473(19) 0.154(7) 0.113(10) -0.004(4) -0.021(7) O9 0.154(9) 0.099(7) 0.225(13) 0.056(8) 0.121(9) 0.039(7) C49 0.176(12) 0.125(10) 0.164(11) 0.022(9) 0.109(10) 0.026(9) C50 0.102(13) 0.090(13) 0.100(13) -0.005(11) 0.033(11) -0.026(11) C50X 0.14(2) 0.109(18) 0.19(3) -0.072(19) 0.055(18) -0.004(15) O10 0.092(7) 0.067(6) 0.077(6) 0.003(5) 0.038(5) 0.007(5) O10X 0.28(3) 0.25(2) 0.26(2) -0.117(19) 0.21(2) -0.18(2) _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 1.951(4) 2 ? Cu1 N2 1.951(4) . ? Cu1 N1 1.957(4) 2 ? Cu1 N1 1.957(4) . ? N1 S1 1.596(4) . ? S1 C1 1.783(5) . ? S1 C7 1.798(6) . ? C1 C2 1.371(7) . ? C1 C6 1.390(7) . ? C2 C3 1.375(8) . ? C3 C4 1.363(8) . ? C4 C5 1.369(9) . ? C5 C6 1.401(8) . ? C7 C8 1.378(8) . ? C7 C12 1.387(8) . ? C8 C9 1.382(11) . ? C9 C10 1.363(12) . ? C10 C11 1.392(11) . ? C11 C12 1.375(10) . ? N2 S2 1.599(4) . ? S2 C19 1.773(6) . ? S2 C13 1.792(5) . ? C13 C18 1.378(6) . ? C13 C14 1.381(7) . ? C14 C15 1.380(8) . ? C15 C16 1.380(8) . ? C16 C17 1.363(8) . ? C17 C18 1.391(7) . ? C19 C20 1.367(9) . ? C19 C24 1.392(9) . ? C20 C21 1.398(9) . ? C21 C22 1.382(15) . ? C22 C23 1.358(16) . ? C23 C24 1.385(13) . ? Cu2 N3 1.969(4) 3_665 ? Cu2 N3 1.969(4) . ? Cu2 N4 1.999(4) 3_665 ? Cu2 N4 1.999(4) . ? N3 S3 1.605(5) . ? S3 C25 1.786(5) . ? S3 C31 1.801(6) . ? C25 C30 1.385(8) . ? C25 C26 1.386(7) . ? C26 C27 1.394(9) . ? C27 C28 1.376(9) . ? C28 C29 1.382(9) . ? C29 C30 1.377(8) . ? C31 C36 1.382(7) . ? C31 C32 1.401(8) . ? C32 C33 1.384(10) . ? C33 C34 1.384(9) . ? C34 C35 1.381(9) . ? C35 C36 1.391(9) . ? N4 S4 1.589(4) . ? S4 C43 1.800(6) . ? S4 C37 1.807(5) . ? C37 C42 1.369(7) . ? C37 C38 1.394(7) . ? C38 C39 1.393(8) . ? C39 C40 1.356(9) . ? C40 C41 1.389(8) . ? C41 C42 1.405(7) . ? C43 C48 1.373(8) . ? C43 C44 1.378(8) . ? C44 C45 1.387(8) . ? C45 C46 1.362(11) . ? C46 C47 1.315(14) . ? C47 C48 1.384(13) . ? Cl1 O2 1.428(4) . ? Cl1 O2 1.428(4) 2 ? Cl1 O1 1.434(4) 2 ? Cl1 O1 1.434(4) . ? Cl2 O3 1.334(6) . ? Cl2 O3 1.334(6) 2_655 ? Cl2 O4X 1.362(10) 2_655 ? Cl2 O4X 1.362(10) . ? Cl2 O4 1.652(9) . ? Cl2 O4 1.652(9) 2_655 ? O4X O4X 1.23(3) 2_655 ? Cl3 O8 1.265(7) . ? Cl3 O6 1.386(5) . ? Cl3 O5 1.400(6) . ? Cl3 O7 1.431(7) . ? O9 C50X 1.34(2) 3_675 ? O9 C50X 1.34(2) . ? O9 C50 1.497(19) . ? O9 C50 1.497(19) 3_675 ? C49 C50 1.27(2) . ? C49 C50X 1.48(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N2 89.1(2) 2 . ? N2 Cu1 N1 96.22(18) 2 2 ? N2 Cu1 N1 154.3(2) . 2 ? N2 Cu1 N1 154.3(2) 2 . ? N2 Cu1 N1 96.22(18) . . ? N1 Cu1 N1 89.8(3) 2 . ? S1 N1 Cu1 121.5(3) . . ? N1 S1 C1 108.5(3) . . ? N1 S1 C7 110.0(3) . . ? C1 S1 C7 101.1(2) . . ? C2 C1 C6 120.7(5) . . ? C2 C1 S1 121.5(4) . . ? C6 C1 S1 117.8(4) . . ? C1 C2 C3 119.4(5) . . ? C4 C3 C2 121.1(6) . . ? C3 C4 C5 119.9(6) . . ? C4 C5 C6 120.4(5) . . ? C1 C6 C5 118.4(6) . . ? C8 C7 C12 121.7(7) . . ? C8 C7 S1 119.8(5) . . ? C12 C7 S1 118.1(5) . . ? C7 C8 C9 118.5(7) . . ? C10 C9 C8 121.0(8) . . ? C9 C10 C11 120.0(8) . . ? C12 C11 C10 120.3(8) . . ? C11 C12 C7 118.6(7) . . ? S2 N2 Cu1 123.5(2) . . ? N2 S2 C19 108.8(2) . . ? N2 S2 C13 108.1(2) . . ? C19 S2 C13 102.2(2) . . ? C18 C13 C14 120.9(4) . . ? C18 C13 S2 120.1(4) . . ? C14 C13 S2 118.3(4) . . ? C15 C14 C13 119.1(5) . . ? C16 C15 C14 120.0(5) . . ? C17 C16 C15 120.7(5) . . ? C16 C17 C18 119.9(5) . . ? C13 C18 C17 119.2(5) . . ? C20 C19 C24 121.6(7) . . ? C20 C19 S2 122.2(5) . . ? C24 C19 S2 115.9(6) . . ? C19 C20 C21 118.8(8) . . ? C22 C21 C20 119.3(10) . . ? C23 C22 C21 121.6(9) . . ? C22 C23 C24 119.8(10) . . ? C23 C24 C19 118.9(10) . . ? N3 Cu2 N3 180.0(2) 3_665 . ? N3 Cu2 N4 91.71(18) 3_665 3_665 ? N3 Cu2 N4 88.29(18) . 3_665 ? N3 Cu2 N4 88.29(18) 3_665 . ? N3 Cu2 N4 91.71(18) . . ? N4 Cu2 N4 180.0(3) 3_665 . ? S3 N3 Cu2 123.9(3) . . ? N3 S3 C25 107.4(3) . . ? N3 S3 C31 110.0(2) . . ? C25 S3 C31 100.3(2) . . ? C30 C25 C26 121.5(5) . . ? C30 C25 S3 121.4(4) . . ? C26 C25 S3 116.9(4) . . ? C25 C26 C27 118.4(5) . . ? C28 C27 C26 120.7(6) . . ? C27 C28 C29 119.6(6) . . ? C30 C29 C28 121.1(6) . . ? C29 C30 C25 118.7(5) . . ? C36 C31 C32 120.8(6) . . ? C36 C31 S3 119.3(4) . . ? C32 C31 S3 119.6(4) . . ? C33 C32 C31 118.9(6) . . ? C34 C33 C32 120.7(6) . . ? C35 C34 C33 119.9(7) . . ? C34 C35 C36 120.5(6) . . ? C31 C36 C35 119.2(5) . . ? S4 N4 Cu2 124.1(3) . . ? N4 S4 C43 110.6(2) . . ? N4 S4 C37 109.2(2) . . ? C43 S4 C37 98.8(2) . . ? C42 C37 C38 122.1(5) . . ? C42 C37 S4 119.7(4) . . ? C38 C37 S4 117.9(4) . . ? C39 C38 C37 118.4(5) . . ? C40 C39 C38 120.2(5) . . ? C39 C40 C41 121.4(5) . . ? C40 C41 C42 119.4(6) . . ? C37 C42 C41 118.5(5) . . ? C48 C43 C44 119.1(7) . . ? C48 C43 S4 118.9(6) . . ? C44 C43 S4 122.0(4) . . ? C43 C44 C45 120.1(6) . . ? C46 C45 C44 119.1(8) . . ? C47 C46 C45 120.9(8) . . ? C46 C47 C48 121.7(8) . . ? C43 C48 C47 119.0(8) . . ? O2 Cl1 O2 107.4(4) . 2 ? O2 Cl1 O1 111.3(3) . 2 ? O2 Cl1 O1 109.0(2) 2 2 ? O2 Cl1 O1 109.0(2) . . ? O2 Cl1 O1 111.3(3) 2 . ? O1 Cl1 O1 108.8(4) 2 . ? O3 Cl2 O3 118.1(9) . 2_655 ? O3 Cl2 O4X 110.3(7) . 2_655 ? O3 Cl2 O4X 124.7(7) 2_655 2_655 ? O3 Cl2 O4X 124.7(7) . . ? O3 Cl2 O4X 110.3(7) 2_655 . ? O4X Cl2 O4X 53.9(13) 2_655 . ? O3 Cl2 O4 99.6(6) . . ? O3 Cl2 O4 95.5(5) 2_655 . ? O4X Cl2 O4 101.4(11) 2_655 . ? O4X Cl2 O4 49.3(7) . . ? O3 Cl2 O4 95.5(5) . 2_655 ? O3 Cl2 O4 99.6(6) 2_655 2_655 ? O4X Cl2 O4 49.3(7) 2_655 2_655 ? O4X Cl2 O4 101.4(11) . 2_655 ? O4 Cl2 O4 150.5(12) . 2_655 ? O4X O4X Cl2 63.0(7) 2_655 . ? O8 Cl3 O6 110.7(6) . . ? O8 Cl3 O5 120.6(7) . . ? O6 Cl3 O5 104.7(4) . . ? O8 Cl3 O7 105.4(6) . . ? O6 Cl3 O7 113.0(5) . . ? O5 Cl3 O7 102.3(4) . . ? C50X O9 C50X 180(2) 3_675 . ? C50X O9 C50 122.8(14) 3_675 . ? C50X O9 C50 57.2(14) . . ? C50X O9 C50 57.2(14) 3_675 3_675 ? C50X O9 C50 122.8(14) . 3_675 ? C50 O9 C50 180.0(5) . 3_675 ? C50 C49 C50X 58.9(13) . . ? C49 C50 O9 121.9(16) . . ? O9 C50X C49 119(2) . . ? 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 N1 H1A O2 0.80(4) 2.54(4) 3.315(6) 161(7) 1_565 N2 H2A O1 0.80(4) 2.32(4) 3.113(6) 176(6) . N3 H3A O5 0.80(4) 2.32(4) 3.106(8) 170(7) 3_665 N4 H4A O5 0.80(4) 2.59(4) 3.349(8) 160(6) . N4 H4A O6 0.80(4) 2.62(5) 3.303(8) 145(6) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.121 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.088 #END of data for (5) data_(6) _database_code_depnum_ccdc_archive 'CCDC 227323' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H44 Cu N6 O6 S4' _chemical_formula_weight 992.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4903(4) _cell_length_b 23.5948(8) _cell_length_c 19.4528(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.126(2) _cell_angle_gamma 90.00 _cell_volume 4739.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 22985 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.84 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 0.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 41399 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 29.10 _reflns_number_total 11453 _reflns_number_gt 9656 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0435P)^2^+2.2185P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except NH coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11453 _refine_ls_number_parameters 598 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.520153(17) 0.086047(8) 0.205110(9) 0.01966(5) Uani 1 1 d . . . N1 N 0.49156(13) 0.10244(6) 0.10549(7) 0.0271(3) Uani 1 1 d D . . H1A H 0.530(2) 0.1288(8) 0.0903(11) 0.041 Uiso 1 1 d D . . S1 S 0.35601(4) 0.091948(17) 0.05471(2) 0.02471(8) Uani 1 1 d . . . C1 C 0.39140(17) 0.09182(7) -0.03230(8) 0.0264(3) Uani 1 1 d . . . C2 C 0.5064(2) 0.06771(8) -0.04277(10) 0.0382(4) Uani 1 1 d . . . H2 H 0.5685 0.0554 -0.0041 0.046 Uiso 1 1 calc R . . C3 C 0.5303(2) 0.06156(9) -0.11041(11) 0.0453(5) Uani 1 1 d . . . H3 H 0.6095 0.0453 -0.1181 0.054 Uiso 1 1 calc R . . C4 C 0.4390(2) 0.07908(9) -0.16652(10) 0.0413(4) Uani 1 1 d . . . H4 H 0.4549 0.0742 -0.2127 0.050 Uiso 1 1 calc R . . C5 C 0.32513(19) 0.10352(9) -0.15556(9) 0.0389(4) Uani 1 1 d . . . H5 H 0.2634 0.1160 -0.1943 0.047 Uiso 1 1 calc R . . C6 C 0.29967(17) 0.11013(8) -0.08841(9) 0.0319(4) Uani 1 1 d . . . H6 H 0.2209 0.1269 -0.0809 0.038 Uiso 1 1 calc R . . C7 C 0.25474(17) 0.15340(7) 0.05173(8) 0.0294(3) Uani 1 1 d . . . C8 C 0.3081(2) 0.20725(8) 0.05821(10) 0.0381(4) Uani 1 1 d . . . H8 H 0.3984 0.2128 0.0604 0.046 Uiso 1 1 calc R . . C9 C 0.2256(3) 0.25303(9) 0.06150(11) 0.0505(5) Uani 1 1 d . . . H9 H 0.2600 0.2904 0.0659 0.061 Uiso 1 1 calc R . . C10 C 0.0935(2) 0.24469(11) 0.05840(11) 0.0537(6) Uani 1 1 d . . . H10 H 0.0386 0.2763 0.0614 0.064 Uiso 1 1 calc R . . C11 C 0.0419(2) 0.19099(10) 0.05104(11) 0.0478(5) Uani 1 1 d . . . H11 H -0.0487 0.1856 0.0479 0.057 Uiso 1 1 calc R . . C12 C 0.12259(18) 0.14462(9) 0.04817(9) 0.0368(4) Uani 1 1 d . . . H12 H 0.0879 0.1073 0.0438 0.044 Uiso 1 1 calc R . . N2 N 0.34835(13) 0.05194(6) 0.20807(7) 0.0250(3) Uani 1 1 d D . . H2A H 0.341(2) 0.0224(7) 0.2286(10) 0.037 Uiso 1 1 d D . . S2 S 0.24136(4) 0.096611(16) 0.22226(2) 0.02419(8) Uani 1 1 d . . . C13 C 0.23895(16) 0.10266(7) 0.31382(8) 0.0263(3) Uani 1 1 d . . . C14 C 0.23718(18) 0.05550(7) 0.35628(9) 0.0330(4) Uani 1 1 d . . . H14 H 0.2273 0.0185 0.3367 0.040 Uiso 1 1 calc R . . C15 C 0.2500(2) 0.06333(8) 0.42785(10) 0.0408(4) Uani 1 1 d . . . H15 H 0.2487 0.0315 0.4577 0.049 Uiso 1 1 calc R . . C16 C 0.2649(2) 0.11762(9) 0.45601(10) 0.0416(4) Uani 1 1 d . . . H16 H 0.2747 0.1227 0.5051 0.050 Uiso 1 1 calc R . . C17 C 0.2656(2) 0.16409(9) 0.41323(10) 0.0441(5) Uani 1 1 d . . . H17 H 0.2751 0.2011 0.4328 0.053 Uiso 1 1 calc R . . C18 C 0.2524(2) 0.15688(8) 0.34161(10) 0.0369(4) Uani 1 1 d . . . H18 H 0.2526 0.1888 0.3118 0.044 Uiso 1 1 calc R . . C19 C 0.08640(15) 0.06602(7) 0.18876(8) 0.0268(3) Uani 1 1 d . . . C20 C -0.02399(17) 0.09825(8) 0.19098(10) 0.0334(4) Uani 1 1 d . . . H20 H -0.0182 0.1333 0.2154 0.040 Uiso 1 1 calc R . . C21 C -0.14298(18) 0.07807(9) 0.15676(11) 0.0415(5) Uani 1 1 d . . . H21 H -0.2191 0.0997 0.1572 0.050 Uiso 1 1 calc R . . C22 C -0.15115(18) 0.02679(10) 0.12214(11) 0.0445(5) Uani 1 1 d . . . H22 H -0.2329 0.0132 0.0992 0.053 Uiso 1 1 calc R . . C23 C -0.04082(19) -0.00491(9) 0.12067(10) 0.0416(4) Uani 1 1 d . . . H23 H -0.0471 -0.0403 0.0971 0.050 Uiso 1 1 calc R . . C24 C 0.07943(17) 0.01492(8) 0.15357(9) 0.0334(4) Uani 1 1 d . . . H24 H 0.1557 -0.0064 0.1519 0.040 Uiso 1 1 calc R . . N3 N 0.59939(13) 0.04128(6) 0.28461(7) 0.0247(3) Uani 1 1 d D . . H3A H 0.5563(19) 0.0191(8) 0.3027(10) 0.037 Uiso 1 1 d D . . S3 S 0.74839(4) 0.043837(16) 0.319835(19) 0.02216(8) Uani 1 1 d . . . C25 C 0.75919(15) 0.05817(6) 0.41131(8) 0.0237(3) Uani 1 1 d . . . C26 C 0.64971(16) 0.07028(7) 0.43887(9) 0.0288(3) Uani 1 1 d . . . H26 H 0.5664 0.0680 0.4105 0.035 Uiso 1 1 calc R . . C27 C 0.66291(18) 0.08592(8) 0.50881(9) 0.0334(4) Uani 1 1 d . . . H27 H 0.5884 0.0942 0.5285 0.040 Uiso 1 1 calc R . . C28 C 0.78520(19) 0.08936(8) 0.54952(9) 0.0345(4) Uani 1 1 d . . . H28 H 0.7941 0.1001 0.5972 0.041 Uiso 1 1 calc R . . C29 C 0.89466(18) 0.07722(8) 0.52133(9) 0.0367(4) Uani 1 1 d . . . H29 H 0.9780 0.0798 0.5496 0.044 Uiso 1 1 calc R . . C30 C 0.88246(17) 0.06138(8) 0.45183(9) 0.0323(4) Uani 1 1 d . . . H30 H 0.9570 0.0529 0.4322 0.039 Uiso 1 1 calc R . . C31 C 0.81460(15) -0.02633(7) 0.32423(7) 0.0230(3) Uani 1 1 d . . . C32 C 0.75363(16) -0.07102(7) 0.35219(8) 0.0261(3) Uani 1 1 d . . . H32 H 0.6778 -0.0647 0.3716 0.031 Uiso 1 1 calc R . . C33 C 0.80608(17) -0.12488(7) 0.35109(9) 0.0295(3) Uani 1 1 d . . . H33 H 0.7658 -0.1561 0.3696 0.035 Uiso 1 1 calc R . . C34 C 0.91763(17) -0.13329(7) 0.32286(9) 0.0318(4) Uani 1 1 d . . . H34 H 0.9532 -0.1703 0.3224 0.038 Uiso 1 1 calc R . . C35 C 0.97744(17) -0.08854(8) 0.29539(9) 0.0311(4) Uani 1 1 d . . . H35 H 1.0535 -0.0948 0.2762 0.037 Uiso 1 1 calc R . . C36 C 0.92558(16) -0.03417(7) 0.29592(8) 0.0278(3) Uani 1 1 d . . . H36 H 0.9657 -0.0031 0.2772 0.033 Uiso 1 1 calc R . . N4 N 0.62989(14) 0.15369(6) 0.22641(7) 0.0274(3) Uani 1 1 d D . . H4A H 0.631(2) 0.1782(8) 0.1985(10) 0.041 Uiso 1 1 d D . . S4 S 0.64623(4) 0.180166(16) 0.30297(2) 0.02512(8) Uani 1 1 d . . . C37 C 0.79510(16) 0.21844(7) 0.32167(9) 0.0304(3) Uani 1 1 d . . . C38 C 0.86075(19) 0.21514(9) 0.39014(11) 0.0441(5) Uani 1 1 d . . . H38 H 0.8266 0.1938 0.4241 0.053 Uiso 1 1 calc R . . C39 C 0.9778(2) 0.24392(12) 0.40779(14) 0.0599(7) Uani 1 1 d . . . H39 H 1.0236 0.2430 0.4545 0.072 Uiso 1 1 calc R . . C40 C 1.0269(2) 0.27357(11) 0.35783(16) 0.0605(7) Uani 1 1 d . . . H40 H 1.1068 0.2931 0.3704 0.073 Uiso 1 1 calc R . . C41 C 0.9625(2) 0.27552(9) 0.28959(14) 0.0523(6) Uani 1 1 d . . . H41 H 0.9990 0.2957 0.2555 0.063 Uiso 1 1 calc R . . C42 C 0.84443(19) 0.24803(8) 0.27067(11) 0.0389(4) Uani 1 1 d . . . H42 H 0.7987 0.2495 0.2240 0.047 Uiso 1 1 calc R . . C43 C 0.53111(16) 0.23679(7) 0.30289(9) 0.0270(3) Uani 1 1 d . . . C44 C 0.5329(2) 0.26814(8) 0.36340(10) 0.0391(4) Uani 1 1 d . . . H44 H 0.5979 0.2617 0.4032 0.047 Uiso 1 1 calc R . . C45 C 0.4380(2) 0.30904(9) 0.36478(11) 0.0469(5) Uani 1 1 d . . . H45 H 0.4380 0.3308 0.4059 0.056 Uiso 1 1 calc R . . C46 C 0.34339(19) 0.31820(8) 0.30649(11) 0.0407(4) Uani 1 1 d . . . H46 H 0.2793 0.3465 0.3076 0.049 Uiso 1 1 calc R . . C47 C 0.34196(18) 0.28638(8) 0.24695(10) 0.0359(4) Uani 1 1 d . . . H47 H 0.2766 0.2926 0.2072 0.043 Uiso 1 1 calc R . . C48 C 0.43616(16) 0.24502(7) 0.24477(9) 0.0300(3) Uani 1 1 d . . . H48 H 0.4351 0.2228 0.2039 0.036 Uiso 1 1 calc R . . N5 N 0.38748(14) -0.08071(6) 0.31508(8) 0.0315(3) Uani 1 1 d . . . O1 O 0.40014(16) -0.13149(6) 0.33095(8) 0.0512(4) Uani 1 1 d . . . O2 O 0.30852(14) -0.06521(6) 0.26244(8) 0.0441(3) Uani 1 1 d . . . O3 O 0.45362(12) -0.04390(5) 0.35230(7) 0.0367(3) Uani 1 1 d . . . N6 N 0.69534(14) 0.22469(6) 0.07042(8) 0.0309(3) Uani 1 1 d . . . O4 O 0.68462(17) 0.17642(7) 0.04489(9) 0.0568(4) Uani 1 1 d . . . O5 O 0.77171(16) 0.25931(6) 0.05368(10) 0.0557(4) Uani 1 1 d . . . O6 O 0.62410(14) 0.23836(6) 0.11366(7) 0.0426(3) Uani 1 1 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 Cu1 0.01895(9) 0.02200(9) 0.01760(9) 0.00097(6) 0.00203(7) 0.00022(7) N1 0.0252(7) 0.0344(7) 0.0201(6) 0.0045(5) -0.0003(5) -0.0049(6) S1 0.02510(19) 0.02886(19) 0.01898(17) 0.00178(14) 0.00062(14) -0.00172(15) C1 0.0328(8) 0.0263(7) 0.0189(7) -0.0016(6) 0.0019(6) -0.0030(6) C2 0.0429(10) 0.0420(10) 0.0288(9) 0.0008(8) 0.0040(8) 0.0131(8) C3 0.0524(12) 0.0484(12) 0.0373(10) -0.0058(9) 0.0137(9) 0.0121(10) C4 0.0562(12) 0.0439(10) 0.0252(8) -0.0080(8) 0.0113(8) -0.0082(9) C5 0.0417(10) 0.0516(11) 0.0209(8) 0.0002(8) -0.0018(7) -0.0092(9) C6 0.0307(8) 0.0403(9) 0.0231(8) 0.0010(7) 0.0004(6) -0.0032(7) C7 0.0334(9) 0.0344(9) 0.0199(7) 0.0014(6) 0.0033(6) 0.0055(7) C8 0.0451(11) 0.0361(9) 0.0315(9) -0.0012(7) 0.0023(8) 0.0018(8) C9 0.0753(16) 0.0366(10) 0.0380(11) -0.0015(8) 0.0052(10) 0.0091(10) C10 0.0634(15) 0.0613(14) 0.0373(11) 0.0035(10) 0.0114(10) 0.0317(12) C11 0.0421(11) 0.0671(14) 0.0359(10) 0.0089(10) 0.0116(9) 0.0195(10) C12 0.0344(9) 0.0490(11) 0.0270(8) 0.0057(8) 0.0055(7) 0.0058(8) N2 0.0205(6) 0.0283(7) 0.0267(7) 0.0018(5) 0.0059(5) 0.0002(5) S2 0.02226(18) 0.02750(18) 0.02379(18) 0.00267(14) 0.00680(14) 0.00082(14) C13 0.0259(8) 0.0295(8) 0.0252(8) 0.0006(6) 0.0093(6) 0.0016(6) C14 0.0415(10) 0.0273(8) 0.0318(9) 0.0009(7) 0.0106(7) 0.0016(7) C15 0.0566(12) 0.0361(10) 0.0319(9) 0.0080(8) 0.0139(9) 0.0057(9) C16 0.0541(12) 0.0451(11) 0.0278(9) -0.0039(8) 0.0134(8) 0.0022(9) C17 0.0635(13) 0.0347(10) 0.0375(10) -0.0084(8) 0.0185(9) -0.0055(9) C18 0.0503(11) 0.0283(8) 0.0356(9) 0.0014(7) 0.0177(8) -0.0024(8) C19 0.0206(7) 0.0351(8) 0.0252(8) 0.0057(6) 0.0055(6) 0.0005(6) C20 0.0257(8) 0.0404(9) 0.0359(9) 0.0085(7) 0.0106(7) 0.0065(7) C21 0.0233(8) 0.0573(12) 0.0446(11) 0.0157(9) 0.0082(8) 0.0085(8) C22 0.0246(9) 0.0634(13) 0.0432(11) 0.0070(10) -0.0006(8) -0.0054(9) C23 0.0330(9) 0.0493(11) 0.0410(10) -0.0051(9) 0.0025(8) -0.0070(8) C24 0.0246(8) 0.0408(10) 0.0345(9) -0.0004(7) 0.0043(7) 0.0005(7) N3 0.0223(6) 0.0265(7) 0.0238(6) 0.0062(5) -0.0005(5) -0.0039(5) S3 0.02249(18) 0.02308(17) 0.02001(17) 0.00244(13) 0.00127(13) -0.00069(14) C25 0.0277(8) 0.0216(7) 0.0201(7) 0.0002(6) -0.0001(6) 0.0006(6) C26 0.0277(8) 0.0314(8) 0.0261(8) 0.0022(6) 0.0017(6) 0.0015(6) C27 0.0363(9) 0.0363(9) 0.0284(8) 0.0000(7) 0.0079(7) 0.0043(7) C28 0.0441(10) 0.0337(9) 0.0239(8) -0.0040(7) 0.0011(7) 0.0037(7) C29 0.0342(9) 0.0425(10) 0.0291(9) -0.0065(7) -0.0060(7) 0.0019(8) C30 0.0269(8) 0.0385(9) 0.0299(8) -0.0051(7) 0.0008(7) 0.0021(7) C31 0.0241(7) 0.0260(7) 0.0176(7) -0.0001(6) 0.0003(6) 0.0025(6) C32 0.0270(8) 0.0280(8) 0.0232(7) -0.0003(6) 0.0041(6) 0.0005(6) C33 0.0335(9) 0.0257(8) 0.0277(8) -0.0007(6) 0.0016(7) -0.0002(6) C34 0.0368(9) 0.0300(8) 0.0266(8) -0.0055(7) 0.0001(7) 0.0074(7) C35 0.0284(8) 0.0400(10) 0.0246(8) -0.0042(7) 0.0039(7) 0.0072(7) C36 0.0268(8) 0.0342(8) 0.0221(7) 0.0011(6) 0.0032(6) 0.0001(7) N4 0.0359(8) 0.0235(6) 0.0220(6) 0.0008(5) 0.0029(6) -0.0056(6) S4 0.0294(2) 0.02257(17) 0.02198(18) 0.00031(14) 0.00068(15) -0.00251(15) C37 0.0252(8) 0.0267(8) 0.0372(9) -0.0062(7) -0.0005(7) -0.0008(6) C38 0.0365(10) 0.0513(12) 0.0408(11) -0.0091(9) -0.0032(8) -0.0005(9) C39 0.0363(11) 0.0716(16) 0.0637(15) -0.0224(13) -0.0138(11) -0.0029(11) C40 0.0277(10) 0.0554(14) 0.094(2) -0.0199(13) -0.0003(11) -0.0079(9) C41 0.0351(11) 0.0391(11) 0.0848(17) -0.0032(11) 0.0165(11) -0.0067(8) C42 0.0343(9) 0.0311(9) 0.0503(11) -0.0003(8) 0.0044(8) -0.0026(7) C43 0.0278(8) 0.0259(7) 0.0276(8) 0.0017(6) 0.0057(6) -0.0032(6) C44 0.0410(10) 0.0414(10) 0.0327(9) -0.0060(8) 0.0004(8) 0.0050(8) C45 0.0512(12) 0.0458(11) 0.0445(11) -0.0111(9) 0.0105(9) 0.0087(9) C46 0.0385(10) 0.0357(10) 0.0508(11) 0.0084(8) 0.0154(9) 0.0062(8) C47 0.0315(9) 0.0395(10) 0.0373(9) 0.0119(8) 0.0074(7) 0.0008(7) C48 0.0293(8) 0.0327(8) 0.0281(8) 0.0034(7) 0.0054(7) -0.0037(7) N5 0.0303(7) 0.0287(7) 0.0389(8) 0.0001(6) 0.0154(6) -0.0013(6) O1 0.0680(10) 0.0259(7) 0.0603(9) 0.0030(6) 0.0132(8) 0.0023(6) O2 0.0454(8) 0.0382(7) 0.0451(8) 0.0005(6) -0.0019(6) -0.0036(6) O3 0.0333(7) 0.0359(7) 0.0414(7) 0.0009(5) 0.0081(5) -0.0090(5) N6 0.0301(7) 0.0314(7) 0.0300(7) 0.0099(6) 0.0019(6) 0.0011(6) O4 0.0639(10) 0.0435(8) 0.0654(10) -0.0137(7) 0.0179(8) -0.0063(7) O5 0.0516(9) 0.0409(8) 0.0845(12) 0.0128(8) 0.0389(9) -0.0037(7) O6 0.0433(8) 0.0438(8) 0.0453(8) 0.0107(6) 0.0204(6) 0.0010(6) _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 N3 1.9355(13) . ? Cu1 N1 1.9470(13) . ? Cu1 N4 1.9689(14) . ? Cu1 N2 1.9838(13) . ? N1 S1 1.6016(14) . ? S1 C7 1.7924(17) . ? S1 C1 1.7955(16) . ? C1 C2 1.381(3) . ? C1 C6 1.391(2) . ? C2 C3 1.390(3) . ? C3 C4 1.383(3) . ? C4 C5 1.376(3) . ? C5 C6 1.387(2) . ? C7 C8 1.385(3) . ? C7 C12 1.391(3) . ? C8 C9 1.392(3) . ? C9 C10 1.390(4) . ? C10 C11 1.375(4) . ? C11 C12 1.390(3) . ? N2 S2 1.5987(14) . ? S2 C13 1.7915(16) . ? S2 C19 1.7932(17) . ? C13 C18 1.386(2) . ? C13 C14 1.388(2) . ? C14 C15 1.387(2) . ? C15 C16 1.391(3) . ? C16 C17 1.377(3) . ? C17 C18 1.386(3) . ? C19 C24 1.382(3) . ? C19 C20 1.392(2) . ? C20 C21 1.391(3) . ? C21 C22 1.380(3) . ? C22 C23 1.383(3) . ? C23 C24 1.391(2) . ? N3 S3 1.5937(13) . ? S3 C31 1.7916(16) . ? S3 C25 1.7952(15) . ? C25 C26 1.380(2) . ? C25 C30 1.393(2) . ? C26 C27 1.393(2) . ? C27 C28 1.386(3) . ? C28 C29 1.387(3) . ? C29 C30 1.387(2) . ? C31 C36 1.385(2) . ? C31 C32 1.392(2) . ? C32 C33 1.387(2) . ? C33 C34 1.392(2) . ? C34 C35 1.383(3) . ? C35 C36 1.394(2) . ? N4 S4 1.5963(14) . ? S4 C37 1.7852(17) . ? S4 C43 1.8007(17) . ? C37 C42 1.386(3) . ? C37 C38 1.390(3) . ? C38 C39 1.392(3) . ? C39 C40 1.370(4) . ? C40 C41 1.380(4) . ? C41 C42 1.389(3) . ? C43 C48 1.383(2) . ? C43 C44 1.388(2) . ? C44 C45 1.390(3) . ? C45 C46 1.386(3) . ? C46 C47 1.378(3) . ? C47 C48 1.395(3) . ? N5 O1 1.2384(19) . ? N5 O2 1.253(2) . ? N5 O3 1.2584(19) . ? N6 O5 1.228(2) . ? N6 O4 1.240(2) . ? N6 O6 1.261(2) . ? 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 N3 Cu1 N1 150.82(6) . . ? N3 Cu1 N4 96.96(6) . . ? N1 Cu1 N4 91.75(6) . . ? N3 Cu1 N2 91.16(6) . . ? N1 Cu1 N2 97.34(6) . . ? N4 Cu1 N2 145.41(6) . . ? S1 N1 Cu1 123.22(8) . . ? N1 S1 C7 110.60(8) . . ? N1 S1 C1 105.86(8) . . ? C7 S1 C1 100.98(8) . . ? C2 C1 C6 120.93(16) . . ? C2 C1 S1 118.07(13) . . ? C6 C1 S1 120.67(13) . . ? C1 C2 C3 119.38(17) . . ? C4 C3 C2 120.03(19) . . ? C5 C4 C3 120.19(18) . . ? C4 C5 C6 120.59(17) . . ? C5 C6 C1 118.87(17) . . ? C8 C7 C12 121.62(17) . . ? C8 C7 S1 120.75(14) . . ? C12 C7 S1 117.44(14) . . ? C7 C8 C9 118.1(2) . . ? C10 C9 C8 120.7(2) . . ? C11 C10 C9 120.4(2) . . ? C10 C11 C12 119.8(2) . . ? C11 C12 C7 119.3(2) . . ? S2 N2 Cu1 113.99(8) . . ? N2 S2 C13 110.93(7) . . ? N2 S2 C19 106.92(8) . . ? C13 S2 C19 102.89(7) . . ? C18 C13 C14 121.26(16) . . ? C18 C13 S2 116.29(13) . . ? C14 C13 S2 122.13(13) . . ? C15 C14 C13 118.77(17) . . ? C14 C15 C16 120.15(17) . . ? C17 C16 C15 120.48(18) . . ? C16 C17 C18 119.96(18) . . ? C17 C18 C13 119.37(17) . . ? C24 C19 C20 121.33(16) . . ? C24 C19 S2 119.78(13) . . ? C20 C19 S2 118.34(14) . . ? C21 C20 C19 118.64(18) . . ? C22 C21 C20 120.46(18) . . ? C21 C22 C23 120.27(18) . . ? C22 C23 C24 120.2(2) . . ? C19 C24 C23 119.07(17) . . ? S3 N3 Cu1 125.02(8) . . ? N3 S3 C31 109.17(7) . . ? N3 S3 C25 108.63(7) . . ? C31 S3 C25 99.81(7) . . ? C26 C25 C30 121.47(15) . . ? C26 C25 S3 120.82(12) . . ? C30 C25 S3 117.49(13) . . ? C25 C26 C27 119.19(16) . . ? C28 C27 C26 119.77(17) . . ? C27 C28 C29 120.63(16) . . ? C28 C29 C30 120.02(17) . . ? C29 C30 C25 118.92(16) . . ? C36 C31 C32 122.01(15) . . ? C36 C31 S3 116.77(12) . . ? C32 C31 S3 121.17(12) . . ? C33 C32 C31 118.51(15) . . ? C32 C33 C34 120.02(16) . . ? C35 C34 C33 120.92(16) . . ? C34 C35 C36 119.71(16) . . ? C31 C36 C35 118.83(16) . . ? S4 N4 Cu1 118.45(8) . . ? N4 S4 C37 109.55(8) . . ? N4 S4 C43 109.12(8) . . ? C37 S4 C43 100.80(8) . . ? C42 C37 C38 121.99(17) . . ? C42 C37 S4 122.17(14) . . ? C38 C37 S4 115.80(15) . . ? C37 C38 C39 118.4(2) . . ? C40 C39 C38 120.0(2) . . ? C39 C40 C41 121.2(2) . . ? C40 C41 C42 120.2(2) . . ? C37 C42 C41 118.3(2) . . ? C48 C43 C44 121.26(16) . . ? C48 C43 S4 119.44(13) . . ? C44 C43 S4 119.07(13) . . ? C43 C44 C45 118.93(18) . . ? C46 C45 C44 120.31(19) . . ? C47 C46 C45 120.18(18) . . ? C46 C47 C48 120.24(17) . . ? C43 C48 C47 119.07(17) . . ? O1 N5 O2 120.84(16) . . ? O1 N5 O3 120.01(16) . . ? O2 N5 O3 119.15(15) . . ? O5 N6 O4 121.51(17) . . ? O5 N6 O6 119.84(16) . . ? O4 N6 O6 118.64(15) . . ? 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 N1 H1A O4 0.823(16) 2.277(17) 3.062(2) 160(2) . N2 H2A O2 0.814(15) 2.214(16) 3.015(2) 168(2) . N3 H3A O3 0.812(15) 2.159(16) 2.9698(18) 176(2) . N4 H4A O6 0.796(15) 2.167(16) 2.9593(19) 174(2) . _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.959 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.055 # END of data for (6) data_(7) _database_code_depnum_ccdc_archive 'CCDC 227324' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H103 Cu2 N13 O14 S9' _chemical_formula_weight 2222.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 10.4434(5) _cell_length_b 16.9500(8) _cell_length_c 30.3408(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.810(2) _cell_angle_gamma 90.00 _cell_volume 5364.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11983 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 26.68 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 0.933 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 46430 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.95 _reflns_number_total 24224 _reflns_number_gt 15853 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0497P)^2^+5.5213P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.549(10) _refine_ls_number_reflns 24224 _refine_ls_number_parameters 1391 _refine_ls_number_restraints 1672 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.126 _refine_ls_shift/su_mean 0.004 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 0.83896(5) 0.97665(3) 0.646516(19) 0.02936(14) Uani 1 1 d . . . N1 N 0.6938(4) 1.0493(2) 0.64127(14) 0.0363(10) Uani 1 1 d U . . H1A H 0.6888 1.0853 0.6621 0.054 Uiso 1 1 calc R . . S1 S 0.58457(13) 1.05004(9) 0.60345(5) 0.0442(3) Uani 1 1 d U . . C1 C 0.5299(5) 1.1513(4) 0.59558(19) 0.0521(17) Uani 1 1 d D . . C2 C 0.5261(6) 1.2002(4) 0.6309(2) 0.0598(17) Uani 1 1 d D . . H2 H 0.5490 1.1814 0.6597 0.072 Uiso 1 1 calc R . . C3 C 0.4878(6) 1.2792(4) 0.6243(3) 0.078(2) Uani 1 1 d D . . H3 H 0.4855 1.3147 0.6485 0.093 Uiso 1 1 calc R . . C4 C 0.4542(7) 1.3039(5) 0.5827(3) 0.086(3) Uani 1 1 d D . . H4 H 0.4258 1.3567 0.5783 0.103 Uiso 1 1 calc R . . C5 C 0.4602(6) 1.2547(4) 0.5470(3) 0.070(2) Uani 1 1 d D . . H5 H 0.4379 1.2738 0.5182 0.085 Uiso 1 1 calc R . . C6 C 0.4997(6) 1.1756(5) 0.5531(2) 0.072(2) Uani 1 1 d D . . H6 H 0.5052 1.1406 0.5288 0.086 Uiso 1 1 calc R . . C7 C 0.4422(5) 1.0069(3) 0.6236(2) 0.0454(14) Uani 1 1 d . . . C8 C 0.3312(7) 1.0065(4) 0.5973(3) 0.066(2) Uani 1 1 d . . . H8 H 0.3289 1.0316 0.5693 0.079 Uiso 1 1 calc R . . C9 C 0.2217(7) 0.9694(5) 0.6119(4) 0.081(3) Uani 1 1 d . . . H9 H 0.1440 0.9706 0.5943 0.097 Uiso 1 1 calc R . . C10 C 0.2270(7) 0.9312(5) 0.6517(3) 0.084(3) Uani 1 1 d . . . H10 H 0.1540 0.9033 0.6608 0.101 Uiso 1 1 calc R . . C11 C 0.3362(7) 0.9329(4) 0.6783(3) 0.073(2) Uani 1 1 d . . . H11 H 0.3376 0.9082 0.7064 0.088 Uiso 1 1 calc R . . C12 C 0.4449(6) 0.9705(4) 0.6645(2) 0.0597(17) Uani 1 1 d . . . H12 H 0.5209 0.9713 0.6830 0.072 Uiso 1 1 calc R . . N2 N 0.8490(5) 0.9528(3) 0.58347(14) 0.0439(11) Uani 1 1 d U . . H2A H 0.8605 0.9033 0.5760 0.066 Uiso 1 1 calc R . . S2 S 0.83779(12) 1.01628(7) 0.54496(4) 0.0336(3) Uani 1 1 d U . . C13 C 0.7192(5) 0.9858(3) 0.50346(17) 0.0379(12) Uani 1 1 d . . . C14 C 0.6997(5) 1.0342(3) 0.46728(18) 0.0429(13) Uani 1 1 d . . . H14 H 0.7513 1.0798 0.4639 0.051 Uiso 1 1 calc R . . C15 C 0.6036(6) 1.0152(4) 0.43593(19) 0.0519(15) Uani 1 1 d . . . H15 H 0.5889 1.0481 0.4108 0.062 Uiso 1 1 calc R . . C16 C 0.5298(6) 0.9493(4) 0.4409(2) 0.0511(15) Uani 1 1 d . . . H16 H 0.4654 0.9360 0.4190 0.061 Uiso 1 1 calc R . . C17 C 0.5487(6) 0.9027(4) 0.4774(2) 0.0616(18) Uani 1 1 d . . . H17 H 0.4946 0.8585 0.4813 0.074 Uiso 1 1 calc R . . C18 C 0.6459(6) 0.9191(3) 0.5092(2) 0.0520(16) Uani 1 1 d . . . H18 H 0.6614 0.8855 0.5339 0.062 Uiso 1 1 calc R . . C19 C 0.9792(5) 1.0139(3) 0.51386(16) 0.0364(12) Uani 1 1 d . . . C20 C 1.0269(6) 0.9442(4) 0.4974(2) 0.0595(17) Uani 1 1 d . . . H20 H 0.9840 0.8955 0.5013 0.071 Uiso 1 1 calc R . . C21 C 1.1400(7) 0.9477(5) 0.4748(2) 0.068(2) Uani 1 1 d . . . H21 H 1.1742 0.9010 0.4626 0.082 Uiso 1 1 calc R . . C22 C 1.2030(6) 1.0194(5) 0.4700(2) 0.0650(19) Uani 1 1 d . . . H22 H 1.2814 1.0210 0.4554 0.078 Uiso 1 1 calc R . . C23 C 1.1534(6) 1.0867(4) 0.4858(2) 0.0594(17) Uani 1 1 d . . . H23 H 1.1958 1.1356 0.4817 0.071 Uiso 1 1 calc R . . C24 C 1.0404(5) 1.0844(3) 0.50813(18) 0.0436(13) Uani 1 1 d . . . H24 H 1.0056 1.1317 0.5194 0.052 Uiso 1 1 calc R . . N3 N 0.9177(4) 0.8737(2) 0.66117(13) 0.0366(10) Uani 1 1 d U . . H3A H 0.9524 0.8443 0.6410 0.055 Uiso 1 1 calc R . . S3 S 0.91531(13) 0.84622(7) 0.71176(4) 0.0341(3) Uani 1 1 d U . . C25 C 1.0086(6) 0.7587(3) 0.71871(17) 0.0424(13) Uani 1 1 d . . . C26 C 0.9913(9) 0.6946(4) 0.6920(2) 0.080(2) Uani 1 1 d . . . H26 H 0.9278 0.6949 0.6685 0.096 Uiso 1 1 calc R . . C27 C 1.0686(10) 0.6286(5) 0.6998(3) 0.109(4) Uani 1 1 d . . . H27 H 1.0608 0.5841 0.6808 0.131 Uiso 1 1 calc R . . C28 C 1.1552(8) 0.6281(4) 0.7347(3) 0.076(2) Uani 1 1 d . . . H28 H 1.2066 0.5826 0.7402 0.091 Uiso 1 1 calc R . . C29 C 1.1698(6) 0.6916(4) 0.7620(3) 0.0653(19) Uani 1 1 d . . . H29 H 1.2312 0.6904 0.7861 0.078 Uiso 1 1 calc R . . C30 C 1.0941(6) 0.7582(3) 0.75422(19) 0.0490(15) Uani 1 1 d . . . H30 H 1.1018 0.8025 0.7733 0.059 Uiso 1 1 calc R . . C31 C 0.7583(6) 0.8127(3) 0.7239(2) 0.0473(14) Uani 1 1 d . . . C32 C 0.7251(8) 0.8205(5) 0.7660(3) 0.080(2) Uani 1 1 d . . . H32 H 0.7855 0.8400 0.7878 0.096 Uiso 1 1 calc R . . C33 C 0.6026(9) 0.8001(7) 0.7774(3) 0.109(4) Uani 1 1 d . . . H33 H 0.5789 0.8048 0.8071 0.130 Uiso 1 1 calc R . . C34 C 0.5199(9) 0.7745(6) 0.7471(4) 0.106(3) Uani 1 1 d . . . H34 H 0.4355 0.7619 0.7550 0.127 Uiso 1 1 calc R . . C35 C 0.5517(10) 0.7654(7) 0.7045(4) 0.125(4) Uani 1 1 d . . . H35 H 0.4904 0.7458 0.6831 0.150 Uiso 1 1 calc R . . C36 C 0.6745(7) 0.7849(5) 0.6926(3) 0.085(3) Uani 1 1 d . . . H36 H 0.6986 0.7788 0.6630 0.102 Uiso 1 1 calc R . . N4 N 0.8870(4) 1.0281(2) 0.70316(13) 0.0364(10) Uani 1 1 d U . . H4A H 0.8274 1.0568 0.7149 0.055 Uiso 1 1 calc R . . S4 S 1.02045(12) 1.02350(7) 0.72977(4) 0.0328(3) Uani 1 1 d U . . C37 C 0.9968(5) 1.0055(3) 0.78677(17) 0.0363(12) Uani 1 1 d . . . C38 C 1.0977(6) 0.9728(3) 0.8118(2) 0.0521(15) Uani 1 1 d . . . H38 H 1.1769 0.9613 0.7991 0.063 Uiso 1 1 calc R . . C39 C 1.0801(7) 0.9575(4) 0.8556(2) 0.0599(18) Uani 1 1 d . . . H39 H 1.1481 0.9346 0.8732 0.072 Uiso 1 1 calc R . . C40 C 0.9665(8) 0.9746(4) 0.8747(2) 0.0627(18) Uani 1 1 d . . . H40 H 0.9573 0.9646 0.9052 0.075 Uiso 1 1 calc R . . C41 C 0.8676(7) 1.0056(4) 0.8498(2) 0.0586(18) Uani 1 1 d . . . H41 H 0.7890 1.0168 0.8630 0.070 Uiso 1 1 calc R . . C42 C 0.8799(6) 1.0213(4) 0.80499(19) 0.0483(14) Uani 1 1 d . . . H42 H 0.8102 1.0423 0.7874 0.058 Uiso 1 1 calc R . . C43 C 1.0866(5) 1.1207(3) 0.73333(17) 0.0367(12) Uani 1 1 d . . . C44 C 1.2177(6) 1.1279(4) 0.7294(2) 0.0535(15) Uani 1 1 d . . . H44 H 1.2687 1.0820 0.7265 0.064 Uiso 1 1 calc R . . C45 C 1.2745(8) 1.2014(5) 0.7296(2) 0.074(2) Uani 1 1 d . . . H45 H 1.3641 1.2068 0.7264 0.089 Uiso 1 1 calc R . . C46 C 1.1977(9) 1.2673(5) 0.7347(2) 0.080(3) Uani 1 1 d . . . H46 H 1.2357 1.3182 0.7354 0.097 Uiso 1 1 calc R . . C47 C 1.0682(8) 1.2602(4) 0.7386(2) 0.0640(19) Uani 1 1 d . . . H47 H 1.0172 1.3060 0.7419 0.077 Uiso 1 1 calc R . . C48 C 1.0107(7) 1.1853(3) 0.73785(18) 0.0496(14) Uani 1 1 d . . . H48 H 0.9209 1.1797 0.7404 0.060 Uiso 1 1 calc R . . Cu2 Cu 0.09548(6) 0.49642(4) 0.97603(2) 0.03670(15) Uani 1 1 d . . . N5 N 0.0660(4) 0.6095(3) 0.99158(14) 0.0407(10) Uani 1 1 d U A . H5A H 0.1274 0.6440 0.9877 0.061 Uiso 1 1 calc R . . S5 S -0.06395(13) 0.63890(8) 1.01055(5) 0.0381(3) Uani 1 1 d U . . C49 C -0.1533(5) 0.6966(3) 0.96986(17) 0.0363(12) Uani 1 1 d D A . C50 C -0.0931(6) 0.7384(3) 0.9387(2) 0.0539(16) Uani 1 1 d D . . H50 H -0.0021 0.7394 0.9385 0.065 Uiso 1 1 calc R A . C51 C -0.1670(8) 0.7796(4) 0.9071(2) 0.074(2) Uani 1 1 d D A . H51 H -0.1265 0.8090 0.8850 0.089 Uiso 1 1 calc R . . C52 C -0.2976(8) 0.7781(4) 0.9076(2) 0.075(2) Uani 1 1 d D . . H52 H -0.3480 0.8063 0.8859 0.090 Uiso 1 1 calc R A . C53 C -0.3562(7) 0.7353(5) 0.9397(3) 0.082(2) Uani 1 1 d D A . H53 H -0.4471 0.7351 0.9404 0.099 Uiso 1 1 calc R . . C54 C -0.2849(5) 0.6932(4) 0.9704(2) 0.0575(16) Uani 1 1 d D . . H54 H -0.3254 0.6622 0.9918 0.069 Uiso 1 1 calc R A . C55 C -0.0237(5) 0.7157(3) 1.05062(17) 0.0396(13) Uani 1 1 d D A . C56 C -0.1218(5) 0.7484(3) 1.07401(18) 0.0475(14) Uani 1 1 d D . . H56 H -0.2089 0.7348 1.0674 0.057 Uiso 1 1 calc R A . C57 C -0.0883(6) 0.8018(3) 1.10748(19) 0.0587(18) Uani 1 1 d D A . H57 H -0.1536 0.8254 1.1238 0.070 Uiso 1 1 calc R . . C58 C 0.0361(6) 0.8208(3) 1.11726(18) 0.0506(15) Uani 1 1 d D . . H58 H 0.0575 0.8570 1.1404 0.061 Uiso 1 1 calc R A . C59 C 0.1307(6) 0.7874(3) 1.09369(18) 0.0497(15) Uani 1 1 d D A . H59 H 0.2176 0.8009 1.1007 0.060 Uiso 1 1 calc R . . C60 C 0.1023(5) 0.7346(3) 1.05993(17) 0.0366(12) Uani 1 1 d D . . H60 H 0.1684 0.7120 1.0436 0.044 Uiso 1 1 calc R A . N6 N 0.1457(8) 0.4667(3) 1.03933(17) 0.094(2) Uani 1 1 d U A . H6A H 0.1646 0.4172 1.0453 0.141 Uiso 1 1 calc R . . S6 S 0.1523(2) 0.52875(10) 1.07850(5) 0.0749(6) Uani 1 1 d U . . C61 C 0.2638(8) 0.4947(4) 1.1200(2) 0.075(2) Uani 1 1 d D A . C62 C 0.2998(8) 0.5423(4) 1.1555(2) 0.075(2) Uani 1 1 d D . . H62 H 0.2595 0.5921 1.1586 0.090 Uiso 1 1 calc R A . C63 C 0.3916(8) 0.5191(5) 1.1859(3) 0.085(3) Uani 1 1 d D A . H63 H 0.4119 0.5513 1.2108 0.102 Uiso 1 1 calc R . . C64 C 0.4546(12) 0.4499(6) 1.1807(3) 0.117(4) Uani 1 1 d D . . H64 H 0.5181 0.4340 1.2024 0.141 Uiso 1 1 calc R A . C65 C 0.4283(14) 0.4028(6) 1.1449(3) 0.165(6) Uani 1 1 d D A . H65 H 0.4721 0.3543 1.1414 0.198 Uiso 1 1 calc R . . C66 C 0.3382(10) 0.4273(5) 1.1145(3) 0.106(3) Uani 1 1 d D . . H66 H 0.3248 0.3973 1.0882 0.127 Uiso 1 1 calc R A . C67 C 0.0083(7) 0.5262(4) 1.1079(2) 0.068(2) Uani 1 1 d D A . C68 C -0.0186(9) 0.5874(4) 1.1355(2) 0.080(2) Uani 1 1 d D . . H68 H 0.0418 0.6286 1.1407 0.096 Uiso 1 1 calc R A . C69 C -0.1335(9) 0.5884(5) 1.1555(3) 0.088(3) Uani 1 1 d D A . H69 H -0.1536 0.6313 1.1740 0.105 Uiso 1 1 calc R . . C70 C -0.2214(8) 0.5269(6) 1.1488(3) 0.098(3) Uani 1 1 d D . . H70 H -0.3009 0.5273 1.1628 0.118 Uiso 1 1 calc R A . C71 C -0.1890(10) 0.4645(5) 1.1210(3) 0.101(3) Uani 1 1 d D A . H71 H -0.2470 0.4218 1.1162 0.121 Uiso 1 1 calc R . . C72 C -0.0746(9) 0.4646(5) 1.1008(3) 0.090(3) Uani 1 1 d D . . H72 H -0.0530 0.4223 1.0820 0.108 Uiso 1 1 calc R A . N7 N 0.1336(6) 0.3831(3) 0.96263(18) 0.0457(14) Uani 0.865(5) 1 d PU A 1 H7A H 0.0699 0.3490 0.9619 0.069 Uiso 0.865(5) 1 calc PR A 1 S7 S 0.27186(18) 0.35215(9) 0.95333(5) 0.0416(6) Uani 0.865(5) 1 d PU A 1 N7X N 0.213(4) 0.4030(19) 0.9556(11) 0.035(5) Uani 0.135(5) 1 d PU A 2 H7X H 0.2762 0.4136 0.9383 0.052 Uiso 0.135(5) 1 calc PR A 2 S7X S 0.1926(10) 0.3195(6) 0.9694(3) 0.038(3) Uani 0.135(5) 1 d PU A 2 C73 C 0.3342(6) 0.2967(4) 1.0016(2) 0.0576(18) Uani 1 1 d DU . . C74 C 0.4620(7) 0.3084(5) 1.0104(3) 0.091(3) Uani 1 1 d DU A . H74 H 0.5098 0.3413 0.9919 0.109 Uiso 1 1 calc R . . C75 C 0.5218(10) 0.2713(7) 1.0470(4) 0.152(6) Uani 1 1 d DU . . H75 H 0.6103 0.2789 1.0545 0.183 Uiso 1 1 calc R A . C76 C 0.4489(14) 0.2243(7) 1.0712(4) 0.175(8) Uani 1 1 d DU A . H76 H 0.4891 0.1960 1.0950 0.210 Uiso 1 1 calc R . . C77 C 0.3186(13) 0.2151(5) 1.0631(3) 0.139(5) Uani 1 1 d DU . . H77 H 0.2703 0.1841 1.0824 0.167 Uiso 1 1 calc R A . C78 C 0.2581(9) 0.2517(4) 1.0264(2) 0.086(3) Uani 1 1 d DU A . H78 H 0.1691 0.2455 1.0193 0.103 Uiso 1 1 calc R B 2 C79 C 0.2526(7) 0.2710(4) 0.9144(2) 0.0633(19) Uani 1 1 d DU . . C80 C 0.3648(8) 0.2442(4) 0.8979(2) 0.076(2) Uani 1 1 d DU A . H80 H 0.4455 0.2637 0.9087 0.091 Uiso 1 1 calc R . . C81 C 0.3560(9) 0.1877(4) 0.8650(2) 0.085(3) Uani 1 1 d DU . . H81 H 0.4323 0.1676 0.8534 0.102 Uiso 1 1 calc R A . C82 C 0.2423(10) 0.1607(4) 0.8491(2) 0.090(3) Uani 1 1 d DU A . H82 H 0.2391 0.1218 0.8265 0.108 Uiso 1 1 calc R . . C83 C 0.1305(10) 0.1887(5) 0.8651(2) 0.095(3) Uani 1 1 d DU . . H83 H 0.0504 0.1695 0.8534 0.114 Uiso 1 1 calc R A . C84 C 0.1338(8) 0.2458(4) 0.8991(2) 0.079(2) Uani 1 1 d DU A . H84 H 0.0575 0.2659 0.9107 0.094 Uiso 1 1 calc R . . N8 N 0.1275(5) 0.5313(3) 0.91575(15) 0.0528(13) Uani 1 1 d U A . H8A H 0.1526 0.5804 0.9123 0.079 Uiso 1 1 calc R . . S8 S 0.11210(17) 0.47870(8) 0.87336(4) 0.0495(4) Uani 1 1 d U . . C85 C -0.0007(7) 0.5249(3) 0.83545(19) 0.0548(17) Uani 1 1 d D A . C86 C -0.0446(10) 0.4847(5) 0.7985(2) 0.101(3) Uani 1 1 d D . . H86 H -0.0129 0.4335 0.7927 0.121 Uiso 1 1 calc R A . C87 C -0.1349(10) 0.5188(7) 0.7698(3) 0.115(4) Uani 1 1 d D A . H87 H -0.1613 0.4909 0.7438 0.138 Uiso 1 1 calc R . . C88 C -0.1881(8) 0.5910(6) 0.7772(3) 0.093(3) Uani 1 1 d D . . H88 H -0.2515 0.6133 0.7575 0.111 Uiso 1 1 calc R A . C89 C -0.1447(8) 0.6289(5) 0.8145(3) 0.089(3) Uani 1 1 d D A . H89 H -0.1795 0.6791 0.8209 0.107 Uiso 1 1 calc R . . C90 C -0.0511(7) 0.5970(4) 0.8439(2) 0.069(2) Uani 1 1 d D . . H90 H -0.0229 0.6255 0.8695 0.083 Uiso 1 1 calc R A . C91 C 0.2542(6) 0.4851(3) 0.84312(18) 0.0538(16) Uani 1 1 d D A . C92 C 0.3024(7) 0.4158(4) 0.8265(2) 0.0621(18) Uani 1 1 d D . . H92 H 0.2579 0.3674 0.8296 0.075 Uiso 1 1 calc R A . C93 C 0.4154(8) 0.4183(5) 0.8055(2) 0.083(2) Uani 1 1 d D A . H93 H 0.4493 0.3709 0.7940 0.099 Uiso 1 1 calc R . . C94 C 0.4803(8) 0.4876(5) 0.8007(2) 0.079(2) Uani 1 1 d D . . H94 H 0.5585 0.4882 0.7860 0.095 Uiso 1 1 calc R A . C95 C 0.4323(7) 0.5560(4) 0.8172(2) 0.0677(19) Uani 1 1 d D A . H95 H 0.4773 0.6042 0.8138 0.081 Uiso 1 1 calc R . . C96 C 0.3186(6) 0.5555(4) 0.8389(2) 0.0595(18) Uani 1 1 d D . . H96 H 0.2855 0.6029 0.8506 0.071 Uiso 1 1 calc R A . N9 N -0.0985(6) 0.4508(4) 0.9774(2) 0.0586(18) Uani 0.763(5) 1 d PU A 1 H9A H -0.1233 0.4258 1.0009 0.088 Uiso 0.763(5) 1 calc PR A 1 S9 S -0.1940(2) 0.46233(13) 0.93680(7) 0.0544(8) Uani 0.763(5) 1 d PU A 1 N9X N -0.110(2) 0.4886(13) 0.9451(7) 0.055(4) Uani 0.237(5) 1 d PU A 2 H9X H -0.1403 0.5215 0.9247 0.082 Uiso 0.237(5) 1 calc PR A 2 S9X S -0.1930(7) 0.4179(4) 0.9642(2) 0.050(2) Uani 0.237(5) 1 d PU A 2 C97 C -0.2357(5) 0.3659(4) 0.9126(2) 0.0621(19) Uani 1 1 d D . . C98 C -0.2305(8) 0.2965(5) 0.9349(3) 0.088(3) Uani 1 1 d D A . H98 H -0.2120 0.2961 0.9659 0.105 Uiso 1 1 calc R C 2 C99 C -0.2521(10) 0.2266(5) 0.9126(4) 0.122(4) Uani 1 1 d D . . H99 H -0.2491 0.1778 0.9279 0.147 Uiso 1 1 calc R A . C100 C -0.2779(11) 0.2285(7) 0.8681(5) 0.157(7) Uani 1 1 d D A . H100 H -0.2970 0.1809 0.8526 0.188 Uiso 1 1 calc R . . C101 C -0.2763(14) 0.2981(9) 0.8457(3) 0.168(7) Uani 1 1 d D . . H101 H -0.2891 0.2991 0.8145 0.202 Uiso 1 1 calc R A . C102 C -0.2558(10) 0.3671(6) 0.8690(3) 0.105(3) Uani 1 1 d D A . H102 H -0.2560 0.4160 0.8537 0.127 Uiso 1 1 calc R . . C103 C -0.3464(7) 0.4854(5) 0.9611(3) 0.081(2) Uani 1 1 d D . . C104 C -0.4413(7) 0.5120(5) 0.9333(3) 0.094(3) Uani 1 1 d D A . H104 H -0.4323 0.5118 0.9023 0.113 Uiso 1 1 calc R . . C105 C -0.5512(7) 0.5395(5) 0.9510(3) 0.093(3) Uani 1 1 d D . . H105 H -0.6198 0.5571 0.9317 0.111 Uiso 1 1 calc R A . C106 C -0.5651(9) 0.5423(5) 0.9957(3) 0.090(3) Uani 1 1 d D A . H106 H -0.6401 0.5645 1.0071 0.107 Uiso 1 1 calc R . . C107 C -0.4712(10) 0.5134(5) 1.0232(3) 0.105(3) Uani 1 1 d D . . H107 H -0.4825 0.5118 1.0541 0.126 Uiso 1 1 calc R A . C108 C -0.3574(9) 0.4856(5) 1.0064(3) 0.095(3) Uani 1 1 d D A . H108 H -0.2891 0.4674 1.0255 0.114 Uiso 1 1 calc R . . N10 N 0.2667(5) 0.7429(3) 0.92328(18) 0.0531(13) Uani 1 1 d DU . . O1 O 0.2593(5) 0.7181(3) 0.96135(17) 0.0795(15) Uani 1 1 d DU . . O2 O 0.2025(5) 0.7106(3) 0.89270(15) 0.0655(12) Uani 1 1 d DU . . O3 O 0.3354(5) 0.8004(3) 0.91670(17) 0.0772(14) Uani 1 1 d DU . . N11 N 0.4874(7) 0.0090(4) 0.8093(2) 0.0693(16) Uani 1 1 d U . . O4 O 0.4430(8) -0.0028(4) 0.7730(2) 0.129(3) Uani 1 1 d U . . O5 O 0.5633(6) 0.0636(4) 0.8143(2) 0.113(2) Uani 1 1 d U . . O6 O 0.4458(7) -0.0281(5) 0.8398(2) 0.124(3) Uani 1 1 d U . . N12 N 0.6476(6) 0.3184(3) 0.73193(18) 0.0573(13) Uani 1 1 d U . . O7 O 0.7455(6) 0.2797(4) 0.7286(3) 0.117(2) Uani 1 1 d U . . O8 O 0.6485(7) 0.3897(3) 0.7324(3) 0.128(3) Uani 1 1 d U . . O9 O 0.5503(6) 0.2865(4) 0.7348(3) 0.136(3) Uani 1 1 d U . . N13 N 0.8861(16) 0.7427(7) 0.5610(4) 0.096(4) Uani 0.704(11) 1 d PDU D 1 O10 O 0.8222(10) 0.7438(6) 0.5941(3) 0.094(3) Uani 0.704(11) 1 d PDU D 1 O11 O 0.9572(11) 0.7986(5) 0.5567(4) 0.151(5) Uani 0.704(11) 1 d PDU D 1 O12 O 0.8986(19) 0.6851(5) 0.5402(3) 0.236(9) Uani 0.704(11) 1 d PDU D 1 N13X N 0.930(2) 0.7382(14) 0.5597(8) 0.073(6) Uani 0.296(11) 1 d PDU D 2 O10X O 1.020(3) 0.709(2) 0.5814(10) 0.202(14) Uani 0.296(11) 1 d PDU D 2 O11X O 0.843(3) 0.7691(16) 0.5781(10) 0.115(10) Uani 0.296(11) 1 d PDU D 2 O12X O 0.9462(17) 0.7329(17) 0.5218(6) 0.108(8) Uani 0.296(11) 1 d PDU D 2 O1W O 0.6519(4) 0.1147(2) 0.73052(14) 0.0586(11) Uani 1 1 d . . . O2W O 0.3227(6) 0.8255(4) 0.82149(17) 0.0971(18) Uani 1 1 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 Cu1 0.0305(3) 0.0290(3) 0.0283(3) 0.0029(3) -0.0019(2) -0.0005(3) N1 0.036(2) 0.035(2) 0.037(2) -0.0017(19) 0.0007(18) 0.0031(19) S1 0.0351(7) 0.0634(9) 0.0336(7) 0.0018(6) -0.0032(6) 0.0104(6) C1 0.021(3) 0.081(5) 0.054(4) 0.033(3) -0.004(2) 0.003(3) C2 0.050(4) 0.057(4) 0.071(5) 0.019(4) -0.010(3) 0.007(3) C3 0.056(4) 0.061(4) 0.114(7) 0.025(4) -0.015(4) 0.020(3) C4 0.064(5) 0.074(6) 0.119(8) 0.043(5) -0.007(5) 0.005(4) C5 0.045(4) 0.088(6) 0.078(5) 0.050(5) -0.001(4) 0.012(4) C6 0.041(4) 0.118(6) 0.057(4) 0.037(4) 0.009(3) 0.018(4) C7 0.031(3) 0.052(3) 0.053(4) -0.010(3) -0.002(3) 0.003(2) C8 0.054(4) 0.058(4) 0.082(5) -0.013(3) -0.027(4) -0.007(3) C9 0.040(4) 0.070(5) 0.132(8) -0.039(5) -0.011(5) -0.003(4) C10 0.052(5) 0.084(6) 0.117(7) -0.052(6) 0.023(5) -0.026(4) C11 0.055(4) 0.086(5) 0.081(5) -0.028(4) 0.029(4) -0.017(4) C12 0.043(4) 0.078(5) 0.058(4) -0.009(3) 0.001(3) -0.016(3) N2 0.064(3) 0.033(2) 0.035(2) 0.0011(19) 0.001(2) 0.005(2) S2 0.0418(7) 0.0316(7) 0.0275(6) 0.0018(5) 0.0017(5) 0.0011(5) C13 0.043(3) 0.039(3) 0.031(3) -0.001(2) 0.000(2) 0.001(2) C14 0.038(3) 0.049(3) 0.041(3) 0.009(3) -0.006(2) -0.010(3) C15 0.053(4) 0.062(4) 0.039(3) 0.011(3) -0.010(3) 0.003(3) C16 0.046(3) 0.055(4) 0.051(4) -0.010(3) -0.004(3) -0.008(3) C17 0.072(5) 0.045(4) 0.068(4) 0.002(3) -0.001(4) -0.024(3) C18 0.073(4) 0.040(3) 0.041(3) 0.013(3) -0.012(3) -0.008(3) C19 0.036(3) 0.046(3) 0.027(3) -0.001(2) -0.005(2) 0.006(2) C20 0.067(4) 0.049(4) 0.063(4) -0.004(3) 0.015(3) 0.014(3) C21 0.065(5) 0.078(5) 0.063(4) -0.002(4) 0.020(4) 0.028(4) C22 0.039(4) 0.095(6) 0.060(4) 0.004(4) -0.003(3) 0.005(4) C23 0.049(4) 0.070(5) 0.059(4) 0.014(3) 0.001(3) -0.017(3) C24 0.045(3) 0.045(3) 0.041(3) 0.005(3) 0.002(3) -0.001(3) N3 0.050(3) 0.030(2) 0.030(2) -0.0008(17) 0.0025(19) 0.0014(19) S3 0.0438(7) 0.0269(6) 0.0309(6) 0.0017(5) -0.0041(5) 0.0004(5) C25 0.060(4) 0.034(3) 0.033(3) 0.004(2) -0.003(3) 0.000(3) C26 0.134(7) 0.054(4) 0.050(4) -0.014(3) -0.029(4) 0.039(4) C27 0.199(11) 0.068(5) 0.058(5) -0.016(4) -0.016(6) 0.070(6) C28 0.098(6) 0.056(4) 0.076(5) 0.011(4) 0.019(4) 0.037(4) C29 0.054(4) 0.052(4) 0.089(5) 0.020(4) -0.012(4) 0.006(3) C30 0.056(4) 0.039(3) 0.051(4) 0.008(3) -0.007(3) 0.000(3) C31 0.049(3) 0.038(3) 0.055(4) 0.014(3) 0.001(3) -0.004(3) C32 0.067(5) 0.116(7) 0.059(5) 0.025(4) 0.012(4) 0.018(5) C33 0.061(5) 0.168(10) 0.097(7) 0.064(7) 0.018(5) 0.020(6) C34 0.075(6) 0.130(8) 0.114(8) 0.059(7) 0.013(6) -0.033(6) C35 0.099(8) 0.154(10) 0.121(10) 0.000(8) -0.007(7) -0.048(7) C36 0.065(5) 0.119(7) 0.071(5) -0.013(5) -0.002(4) -0.045(5) N4 0.039(2) 0.036(2) 0.033(2) -0.0091(18) -0.0071(18) 0.0007(19) S4 0.0341(7) 0.0320(6) 0.0319(7) -0.0019(5) -0.0030(5) 0.0000(5) C37 0.044(3) 0.028(3) 0.036(3) -0.003(2) -0.003(2) -0.006(2) C38 0.059(4) 0.050(4) 0.045(3) -0.003(3) -0.013(3) 0.006(3) C39 0.079(5) 0.063(4) 0.035(3) 0.005(3) -0.011(3) 0.014(4) C40 0.103(6) 0.046(4) 0.040(3) 0.005(3) 0.010(4) -0.010(4) C41 0.071(5) 0.054(4) 0.052(4) 0.010(3) 0.024(4) -0.007(3) C42 0.052(4) 0.054(4) 0.039(3) 0.001(3) 0.000(3) -0.002(3) C43 0.038(3) 0.042(3) 0.030(3) -0.001(2) -0.001(2) -0.009(2) C44 0.055(4) 0.057(4) 0.048(4) 0.000(3) 0.000(3) -0.016(3) C45 0.075(5) 0.077(5) 0.070(5) 0.001(4) 0.004(4) -0.037(4) C46 0.123(8) 0.065(5) 0.053(4) 0.001(4) 0.005(5) -0.056(5) C47 0.103(6) 0.036(3) 0.053(4) 0.001(3) 0.002(4) -0.018(4) C48 0.071(4) 0.037(3) 0.041(3) -0.003(2) 0.006(3) -0.007(3) Cu2 0.0480(4) 0.0332(3) 0.0286(3) -0.0048(3) -0.0009(3) 0.0054(3) N5 0.040(2) 0.041(3) 0.041(3) -0.016(2) 0.0031(19) 0.004(2) S5 0.0414(7) 0.0327(7) 0.0408(7) -0.0093(6) 0.0067(6) 0.0016(6) C49 0.041(3) 0.028(3) 0.040(3) -0.009(2) 0.000(2) -0.004(2) C50 0.060(4) 0.046(3) 0.056(4) -0.003(3) -0.001(3) 0.001(3) C51 0.120(7) 0.050(4) 0.051(4) 0.002(3) -0.004(4) -0.003(4) C52 0.099(6) 0.057(4) 0.066(5) -0.011(4) -0.030(5) 0.034(4) C53 0.068(5) 0.070(5) 0.107(7) -0.003(5) -0.018(5) 0.017(4) C54 0.046(4) 0.052(4) 0.075(5) -0.003(3) 0.000(3) 0.006(3) C55 0.048(3) 0.036(3) 0.035(3) -0.010(2) 0.005(2) 0.010(2) C56 0.044(3) 0.053(4) 0.045(3) -0.010(3) 0.006(3) 0.010(3) C57 0.083(5) 0.048(4) 0.046(4) -0.011(3) 0.016(3) 0.025(3) C58 0.070(4) 0.044(3) 0.038(3) -0.013(3) -0.002(3) 0.004(3) C59 0.056(4) 0.049(3) 0.044(3) -0.009(3) -0.006(3) 0.004(3) C60 0.042(3) 0.032(3) 0.036(3) -0.002(2) 0.001(2) 0.004(2) N6 0.211(8) 0.040(3) 0.032(3) -0.002(2) 0.002(4) -0.004(4) S6 0.156(2) 0.0382(8) 0.0302(8) -0.0008(7) -0.0011(10) -0.0138(11) C61 0.144(8) 0.045(4) 0.036(3) -0.002(3) 0.015(4) -0.022(4) C62 0.117(7) 0.040(4) 0.069(5) -0.016(3) 0.015(5) -0.011(4) C63 0.101(7) 0.098(7) 0.055(5) 0.006(5) -0.003(5) -0.001(5) C64 0.187(11) 0.091(7) 0.072(6) -0.009(5) -0.003(7) 0.015(7) C65 0.288(17) 0.113(9) 0.085(7) -0.033(7) -0.071(10) 0.079(10) C66 0.181(10) 0.063(5) 0.072(6) -0.030(4) -0.009(6) 0.031(6) C67 0.109(6) 0.043(4) 0.048(4) -0.002(3) -0.034(4) -0.003(4) C68 0.134(8) 0.056(4) 0.052(4) 0.006(3) 0.019(5) -0.015(5) C69 0.123(8) 0.075(5) 0.063(5) 0.013(4) -0.014(5) -0.011(5) C70 0.093(6) 0.140(9) 0.059(5) 0.029(6) -0.009(5) -0.009(6) C71 0.144(10) 0.085(6) 0.069(6) -0.006(5) -0.048(6) -0.012(6) C72 0.096(7) 0.097(7) 0.074(6) -0.010(5) -0.014(5) -0.011(5) N7 0.052(3) 0.033(3) 0.052(3) 0.000(2) 0.001(3) 0.002(3) S7 0.0599(12) 0.0259(9) 0.0394(9) -0.0033(7) 0.0048(8) 0.0004(8) N7X 0.038(10) 0.025(8) 0.042(10) -0.012(8) 0.015(10) 0.013(9) S7X 0.043(6) 0.038(5) 0.032(5) 0.005(4) -0.001(4) 0.012(4) C73 0.076(5) 0.041(3) 0.053(4) -0.025(3) -0.020(3) 0.022(3) C74 0.073(5) 0.092(6) 0.104(6) -0.055(5) -0.031(5) 0.020(4) C75 0.140(9) 0.147(11) 0.158(11) -0.106(9) -0.109(9) 0.106(8) C76 0.34(2) 0.095(9) 0.077(8) -0.038(6) -0.100(11) 0.122(12) C77 0.295(17) 0.047(5) 0.077(7) 0.000(5) 0.010(9) 0.013(8) C78 0.150(8) 0.051(4) 0.055(5) -0.006(4) -0.008(5) 0.002(5) C79 0.110(6) 0.037(3) 0.040(4) -0.007(3) -0.013(4) 0.013(4) C80 0.118(7) 0.052(4) 0.054(4) -0.013(3) -0.020(4) 0.029(4) C81 0.149(8) 0.051(4) 0.053(4) -0.011(4) -0.018(5) 0.039(5) C82 0.181(10) 0.046(4) 0.041(4) -0.012(3) -0.001(5) -0.008(5) C83 0.166(9) 0.072(5) 0.047(4) -0.011(4) -0.004(5) -0.054(6) C84 0.116(7) 0.067(5) 0.052(4) -0.006(4) -0.009(4) -0.020(4) N8 0.087(4) 0.039(3) 0.033(2) -0.0065(19) 0.007(2) -0.002(3) S8 0.0867(12) 0.0343(7) 0.0283(7) -0.0028(6) 0.0103(7) 0.0013(7) C85 0.080(5) 0.049(4) 0.036(3) -0.001(3) 0.011(3) -0.015(3) C86 0.166(10) 0.080(6) 0.054(5) -0.019(4) -0.014(6) -0.004(6) C87 0.131(9) 0.146(10) 0.065(6) -0.015(6) -0.035(6) -0.010(8) C88 0.070(5) 0.130(9) 0.076(6) 0.014(6) -0.014(5) -0.013(6) C89 0.081(6) 0.094(6) 0.090(6) 0.014(5) -0.025(5) 0.003(5) C90 0.091(5) 0.064(5) 0.051(4) -0.003(3) -0.004(4) 0.017(4) C91 0.079(5) 0.055(4) 0.028(3) 0.000(3) 0.006(3) 0.020(3) C92 0.081(5) 0.059(4) 0.046(4) -0.010(3) 0.005(3) 0.019(4) C93 0.102(6) 0.078(6) 0.069(5) -0.021(4) 0.016(5) 0.040(5) C94 0.095(6) 0.092(6) 0.053(5) -0.001(4) 0.018(4) 0.018(5) C95 0.077(5) 0.072(5) 0.056(4) 0.007(4) 0.014(4) 0.008(4) C96 0.086(5) 0.049(4) 0.045(4) 0.003(3) 0.021(3) 0.010(4) N9 0.047(4) 0.068(4) 0.059(4) 0.006(3) -0.017(3) -0.023(3) S9 0.0513(13) 0.0611(15) 0.0500(13) 0.0137(11) -0.0075(10) -0.0153(10) N9X 0.043(8) 0.059(9) 0.059(9) 0.003(7) -0.034(7) -0.028(7) S9X 0.054(4) 0.048(4) 0.047(4) 0.004(3) -0.004(3) -0.003(3) C97 0.029(3) 0.097(6) 0.060(4) -0.014(4) -0.004(3) -0.010(3) C98 0.096(7) 0.107(7) 0.062(5) 0.003(5) 0.019(4) 0.016(5) C99 0.101(8) 0.074(6) 0.196(14) -0.024(8) 0.048(9) -0.012(6) C100 0.072(7) 0.171(13) 0.224(19) -0.138(13) -0.028(9) -0.015(8) C101 0.159(12) 0.27(2) 0.071(8) -0.073(11) -0.035(8) 0.052(15) C102 0.138(9) 0.113(8) 0.067(6) 0.004(5) 0.015(6) 0.025(6) C103 0.069(5) 0.084(6) 0.090(6) -0.037(5) -0.005(5) -0.007(4) C104 0.051(5) 0.131(8) 0.100(7) -0.061(6) -0.007(5) -0.015(5) C105 0.055(5) 0.111(7) 0.112(7) -0.066(6) -0.005(4) -0.017(4) C106 0.084(6) 0.054(5) 0.133(9) -0.036(5) 0.037(6) -0.023(4) C107 0.142(10) 0.046(5) 0.130(9) -0.014(5) 0.051(8) -0.007(5) C108 0.099(7) 0.065(5) 0.121(8) -0.002(5) 0.000(6) 0.007(5) N10 0.043(3) 0.061(3) 0.056(3) 0.004(3) 0.005(3) -0.002(2) O1 0.069(3) 0.102(4) 0.067(3) 0.014(3) -0.005(3) -0.023(3) O2 0.077(3) 0.065(3) 0.054(3) -0.008(2) 0.003(2) -0.008(2) O3 0.069(3) 0.076(3) 0.087(4) 0.008(3) 0.009(3) -0.027(3) N11 0.086(5) 0.073(4) 0.047(3) -0.001(3) -0.008(3) 0.002(3) O4 0.177(7) 0.147(6) 0.060(3) 0.012(4) -0.036(4) 0.008(5) O5 0.075(4) 0.125(5) 0.141(6) -0.025(4) 0.034(4) -0.029(4) O6 0.150(6) 0.165(7) 0.059(3) -0.018(4) 0.006(4) -0.082(5) N12 0.059(3) 0.053(3) 0.061(3) -0.009(3) 0.008(3) 0.000(3) O7 0.100(4) 0.094(4) 0.159(6) 0.015(4) 0.031(4) 0.047(4) O8 0.153(6) 0.049(3) 0.190(7) 0.000(4) 0.092(5) 0.015(3) O9 0.081(4) 0.154(6) 0.179(7) -0.109(5) 0.062(4) -0.063(4) N13 0.204(13) 0.038(5) 0.046(6) -0.002(5) -0.012(6) 0.017(7) O10 0.111(7) 0.110(8) 0.056(5) 0.011(5) -0.039(4) -0.037(5) O11 0.217(12) 0.049(5) 0.201(12) 0.013(6) 0.132(10) 0.036(5) O12 0.58(3) 0.055(6) 0.069(7) -0.024(5) -0.037(11) 0.052(10) N13X 0.128(15) 0.037(11) 0.054(9) 0.002(10) -0.008(9) 0.000(10) O10X 0.18(2) 0.25(3) 0.18(2) 0.13(2) 0.002(17) 0.06(2) O11X 0.17(2) 0.073(17) 0.103(19) -0.034(15) 0.044(15) 0.007(15) O12X 0.060(11) 0.18(2) 0.083(10) -0.078(13) 0.009(9) -0.035(12) O1W 0.066(3) 0.058(3) 0.052(2) -0.007(2) 0.002(2) 0.021(2) O2W 0.116(5) 0.108(5) 0.068(4) -0.012(3) 0.008(3) -0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.954(4) . ? Cu1 N2 1.963(4) . ? Cu1 N4 1.970(4) . ? Cu1 N3 1.971(4) . ? N1 S1 1.578(4) . ? S1 C7 1.791(6) . ? S1 C1 1.821(6) . ? C1 C2 1.357(8) . ? C1 C6 1.375(7) . ? C2 C3 1.410(7) . ? C3 C4 1.359(8) . ? C4 C5 1.371(9) . ? C5 C6 1.413(8) . ? C7 C8 1.374(8) . ? C7 C12 1.386(9) . ? C8 C9 1.396(11) . ? C9 C10 1.367(12) . ? C10 C11 1.365(11) . ? C11 C12 1.383(9) . ? N2 S2 1.588(4) . ? S2 C19 1.791(5) . ? S2 C13 1.799(5) . ? C13 C14 1.378(7) . ? C13 C18 1.380(8) . ? C14 C15 1.387(8) . ? C15 C16 1.369(8) . ? C16 C17 1.368(9) . ? C17 C18 1.392(9) . ? C19 C24 1.371(8) . ? C19 C20 1.384(8) . ? C20 C21 1.396(9) . ? C21 C22 1.393(10) . ? C22 C23 1.351(10) . ? C23 C24 1.390(8) . ? N3 S3 1.605(4) . ? S3 C25 1.781(5) . ? S3 C31 1.791(6) . ? C25 C26 1.363(8) . ? C25 C30 1.366(8) . ? C26 C27 1.392(10) . ? C27 C28 1.359(11) . ? C28 C29 1.361(10) . ? C29 C30 1.391(8) . ? C31 C32 1.346(9) . ? C31 C36 1.345(9) . ? C32 C33 1.386(11) . ? C33 C34 1.304(13) . ? C34 C35 1.357(14) . ? C35 C36 1.389(12) . ? N4 S4 1.578(4) . ? S4 C37 1.785(5) . ? S4 C43 1.788(5) . ? C37 C38 1.383(8) . ? C37 C42 1.391(8) . ? C38 C39 1.376(9) . ? C39 C40 1.376(10) . ? C40 C41 1.355(10) . ? C41 C42 1.398(8) . ? C43 C48 1.363(8) . ? C43 C44 1.385(8) . ? C44 C45 1.380(9) . ? C45 C46 1.386(11) . ? C46 C47 1.369(11) . ? C47 C48 1.404(8) . ? Cu2 N8 1.966(5) . ? Cu2 N5 2.001(4) . ? Cu2 N7 2.007(5) . ? Cu2 N6 2.029(5) . ? Cu2 N7X 2.12(3) . ? Cu2 N9 2.171(7) . ? Cu2 N9X 2.303(19) . ? N5 S5 1.580(4) . ? S5 C49 1.799(5) . ? S5 C55 1.816(5) . ? C49 C50 1.361(7) . ? C49 C54 1.377(7) . ? C50 C51 1.389(8) . ? C51 C52 1.365(9) . ? C52 C53 1.382(9) . ? C53 C54 1.366(8) . ? C55 C60 1.371(7) . ? C55 C56 1.390(6) . ? C56 C57 1.393(7) . ? C57 C58 1.357(7) . ? C58 C59 1.370(7) . ? C59 C60 1.382(7) . ? N6 S6 1.586(5) . ? S6 C61 1.769(8) . ? S6 C67 1.786(8) . ? C61 C62 1.384(8) . ? C61 C66 1.395(9) . ? C62 C63 1.355(9) . ? C63 C64 1.358(9) . ? C64 C65 1.366(10) . ? C65 C66 1.350(9) . ? C67 C72 1.366(9) . ? C67 C68 1.370(8) . ? C68 C69 1.371(9) . ? C69 C70 1.397(9) . ? C70 C71 1.405(9) . ? C71 C72 1.370(10) . ? N7 S7 1.575(6) . ? S7 C79 1.818(6) . ? S7 C73 1.832(6) . ? N7X S7X 1.49(4) . ? S7X C73 1.773(11) . ? S7X C79 1.990(12) . ? S7X C78 2.159(12) . ? C73 C78 1.356(8) . ? C73 C74 1.363(8) . ? C74 C75 1.398(10) . ? C75 C76 1.344(11) . ? C76 C77 1.379(11) . ? C77 C78 1.398(10) . ? C79 C84 1.371(8) . ? C79 C80 1.373(8) . ? C80 C81 1.383(8) . ? C81 C82 1.340(9) . ? C82 C83 1.372(9) . ? C83 C84 1.413(8) . ? N8 S8 1.566(5) . ? S8 C85 1.786(7) . ? S8 C91 1.786(6) . ? C85 C90 1.360(8) . ? C85 C86 1.371(8) . ? C86 C87 1.378(9) . ? C87 C88 1.367(10) . ? C88 C89 1.359(9) . ? C89 C90 1.399(8) . ? C91 C96 1.379(8) . ? C91 C92 1.382(7) . ? C92 C93 1.368(8) . ? C93 C94 1.367(9) . ? C94 C95 1.369(8) . ? C95 C96 1.385(8) . ? N9 S9 1.558(7) . ? S9 C103 1.828(8) . ? S9 C97 1.836(7) . ? N9X S9X 1.60(2) . ? S9X C97 1.834(9) . ? S9X C103 1.967(10) . ? S9X C98 2.268(11) . ? C97 C102 1.331(8) . ? C97 C98 1.357(9) . ? C98 C99 1.379(9) . ? C99 C100 1.364(11) . ? C100 C101 1.362(11) . ? C101 C102 1.377(11) . ? C103 C104 1.347(9) . ? C103 C108 1.385(9) . ? C104 C105 1.373(9) . ? C105 C106 1.372(9) . ? C106 C107 1.349(10) . ? C107 C108 1.398(9) . ? N10 O3 1.233(6) . ? N10 O1 1.235(6) . ? N10 O2 1.245(6) . ? N11 O4 1.191(8) . ? N11 O6 1.218(8) . ? N11 O5 1.223(8) . ? N12 O9 1.157(7) . ? N12 O8 1.210(7) . ? N12 O7 1.223(7) . ? N13 O12 1.172(11) . ? N13 O11 1.215(14) . ? N13 O10 1.232(13) . ? N13X O12X 1.174(16) . ? N13X O11X 1.215(17) . ? N13X O10X 1.225(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N2 97.38(18) . . ? N1 Cu1 N4 87.44(17) . . ? N2 Cu1 N4 156.61(19) . . ? N1 Cu1 N3 152.90(18) . . ? N2 Cu1 N3 89.78(17) . . ? N4 Cu1 N3 96.29(17) . . ? S1 N1 Cu1 126.5(3) . . ? N1 S1 C7 109.4(3) . . ? N1 S1 C1 108.3(3) . . ? C7 S1 C1 99.8(3) . . ? C2 C1 C6 122.9(6) . . ? C2 C1 S1 119.6(4) . . ? C6 C1 S1 117.5(5) . . ? C1 C2 C3 119.2(6) . . ? C4 C3 C2 118.9(7) . . ? C3 C4 C5 121.8(7) . . ? C4 C5 C6 119.9(6) . . ? C1 C6 C5 117.4(7) . . ? C8 C7 C12 119.8(6) . . ? C8 C7 S1 119.7(6) . . ? C12 C7 S1 120.4(4) . . ? C7 C8 C9 120.0(8) . . ? C10 C9 C8 119.7(8) . . ? C11 C10 C9 120.5(8) . . ? C10 C11 C12 120.3(8) . . ? C11 C12 C7 119.7(6) . . ? S2 N2 Cu1 124.9(3) . . ? N2 S2 C19 109.8(2) . . ? N2 S2 C13 110.1(3) . . ? C19 S2 C13 100.5(2) . . ? C14 C13 C18 121.8(5) . . ? C14 C13 S2 117.1(4) . . ? C18 C13 S2 121.0(4) . . ? C13 C14 C15 118.8(5) . . ? C16 C15 C14 120.4(5) . . ? C17 C16 C15 120.0(6) . . ? C16 C17 C18 121.1(6) . . ? C13 C18 C17 117.8(5) . . ? C24 C19 C20 121.3(5) . . ? C24 C19 S2 116.7(4) . . ? C20 C19 S2 122.0(5) . . ? C19 C20 C21 118.0(7) . . ? C22 C21 C20 120.2(7) . . ? C23 C22 C21 120.6(6) . . ? C22 C23 C24 119.9(6) . . ? C19 C24 C23 119.9(6) . . ? S3 N3 Cu1 116.5(2) . . ? N3 S3 C25 108.7(2) . . ? N3 S3 C31 110.2(3) . . ? C25 S3 C31 102.2(3) . . ? C26 C25 C30 121.8(6) . . ? C26 C25 S3 122.6(5) . . ? C30 C25 S3 115.6(4) . . ? C25 C26 C27 118.7(7) . . ? C28 C27 C26 119.7(7) . . ? C27 C28 C29 121.3(7) . . ? C28 C29 C30 119.5(7) . . ? C25 C30 C29 118.9(6) . . ? C32 C31 C36 121.1(7) . . ? C32 C31 S3 116.3(6) . . ? C36 C31 S3 122.4(5) . . ? C31 C32 C33 119.7(9) . . ? C34 C33 C32 119.7(9) . . ? C33 C34 C35 121.6(9) . . ? C34 C35 C36 119.6(9) . . ? C31 C36 C35 118.4(8) . . ? S4 N4 Cu1 127.2(3) . . ? N4 S4 C37 110.1(2) . . ? N4 S4 C43 108.3(2) . . ? C37 S4 C43 99.8(2) . . ? C38 C37 C42 121.2(5) . . ? C38 C37 S4 117.6(4) . . ? C42 C37 S4 121.2(4) . . ? C39 C38 C37 118.2(6) . . ? C38 C39 C40 121.7(6) . . ? C41 C40 C39 119.7(6) . . ? C40 C41 C42 120.9(6) . . ? C37 C42 C41 118.3(6) . . ? C48 C43 C44 121.3(5) . . ? C48 C43 S4 121.4(4) . . ? C44 C43 S4 117.2(4) . . ? C45 C44 C43 120.4(7) . . ? C44 C45 C46 118.4(7) . . ? C47 C46 C45 121.2(7) . . ? C46 C47 C48 120.1(7) . . ? C43 C48 C47 118.5(6) . . ? N8 Cu2 N5 88.10(19) . . ? N8 Cu2 N7 93.1(2) . . ? N5 Cu2 N7 176.9(2) . . ? N8 Cu2 N6 155.1(3) . . ? N5 Cu2 N6 92.9(2) . . ? N7 Cu2 N6 84.8(2) . . ? N8 Cu2 N7X 79.9(10) . . ? N5 Cu2 N7X 152.2(11) . . ? N7 Cu2 N7X 25.9(10) . . ? N6 Cu2 N7X 88.0(9) . . ? N8 Cu2 N9 109.0(3) . . ? N5 Cu2 N9 100.5(2) . . ? N7 Cu2 N9 81.8(3) . . ? N6 Cu2 N9 95.3(3) . . ? N7X Cu2 N9 107.1(11) . . ? N8 Cu2 N9X 80.6(6) . . ? N5 Cu2 N9X 90.0(6) . . ? N7 Cu2 N9X 93.0(6) . . ? N6 Cu2 N9X 124.3(7) . . ? N7X Cu2 N9X 112.3(11) . . ? N9 Cu2 N9X 30.2(6) . . ? S5 N5 Cu2 122.2(3) . . ? N5 S5 C49 110.3(2) . . ? N5 S5 C55 107.2(2) . . ? C49 S5 C55 99.5(2) . . ? C50 C49 C54 121.7(5) . . ? C50 C49 S5 121.2(4) . . ? C54 C49 S5 117.0(4) . . ? C49 C50 C51 118.8(6) . . ? C52 C51 C50 120.3(7) . . ? C51 C52 C53 119.7(6) . . ? C54 C53 C52 120.7(7) . . ? C53 C54 C49 118.7(6) . . ? C60 C55 C56 121.7(5) . . ? C60 C55 S5 119.6(4) . . ? C56 C55 S5 118.4(4) . . ? C55 C56 C57 117.8(5) . . ? C58 C57 C56 121.2(5) . . ? C57 C58 C59 119.7(5) . . ? C58 C59 C60 121.4(5) . . ? C55 C60 C59 118.3(5) . . ? S6 N6 Cu2 123.0(3) . . ? N6 S6 C61 108.6(3) . . ? N6 S6 C67 110.6(4) . . ? C61 S6 C67 100.3(3) . . ? C62 C61 C66 116.0(7) . . ? C62 C61 S6 120.5(6) . . ? C66 C61 S6 122.2(5) . . ? C63 C62 C61 121.1(7) . . ? C62 C63 C64 120.2(8) . . ? C63 C64 C65 121.1(9) . . ? C66 C65 C64 118.1(9) . . ? C65 C66 C61 122.9(7) . . ? C72 C67 C68 121.8(8) . . ? C72 C67 S6 118.8(6) . . ? C68 C67 S6 119.3(6) . . ? C67 C68 C69 119.3(7) . . ? C68 C69 C70 120.7(8) . . ? C69 C70 C71 118.2(8) . . ? C72 C71 C70 120.6(8) . . ? C67 C72 C71 119.3(8) . . ? S7 N7 Cu2 123.2(4) . . ? N7 S7 C79 107.2(3) . . ? N7 S7 C73 108.7(3) . . ? C79 S7 C73 98.9(3) . . ? S7X N7X Cu2 122(2) . . ? N7X S7X C73 103.6(16) . . ? N7X S7X C79 95.7(13) . . ? C73 S7X C79 94.8(5) . . ? N7X S7X C78 133.3(15) . . ? C79 S7X C78 110.6(5) . . ? C78 C73 C74 124.6(7) . . ? C78 C73 S7X 86.1(6) . . ? C74 C73 S7X 149.1(8) . . ? C78 C73 S7 122.5(5) . . ? C74 C73 S7 112.9(6) . . ? C73 C74 C75 119.1(9) . . ? C76 C75 C74 117.2(9) . . ? C75 C76 C77 123.4(9) . . ? C76 C77 C78 119.6(9) . . ? C73 C78 C77 115.9(8) . . ? C73 C78 S7X 55.0(5) . . ? C77 C78 S7X 170.7(8) . . ? C84 C79 C80 123.2(6) . . ? C84 C79 S7 121.7(5) . . ? C80 C79 S7 114.7(5) . . ? C84 C79 S7X 95.5(6) . . ? C80 C79 S7X 138.7(6) . . ? C79 C80 C81 117.7(7) . . ? C82 C81 C80 121.5(8) . . ? C81 C82 C83 120.5(7) . . ? C82 C83 C84 120.3(7) . . ? C79 C84 C83 116.7(7) . . ? S8 N8 Cu2 125.3(3) . . ? N8 S8 C85 108.5(3) . . ? N8 S8 C91 109.4(3) . . ? C85 S8 C91 100.4(3) . . ? C90 C85 C86 118.9(7) . . ? C90 C85 S8 121.5(5) . . ? C86 C85 S8 119.5(6) . . ? C85 C86 C87 120.0(8) . . ? C88 C87 C86 122.8(8) . . ? C89 C88 C87 116.0(8) . . ? C88 C89 C90 122.8(8) . . ? C85 C90 C89 119.5(7) . . ? C96 C91 C92 120.9(6) . . ? C96 C91 S8 121.5(4) . . ? C92 C91 S8 117.6(5) . . ? C93 C92 C91 118.8(6) . . ? C94 C93 C92 121.2(6) . . ? C93 C94 C95 119.9(7) . . ? C94 C95 C96 120.3(7) . . ? C91 C96 C95 118.9(6) . . ? S9 N9 Cu2 120.2(4) . . ? N9 S9 C103 104.2(4) . . ? N9 S9 C97 109.5(4) . . ? C103 S9 C97 99.1(3) . . ? S9X N9X Cu2 113.8(12) . . ? N9X S9X C97 99.4(9) . . ? N9X S9X C103 90.0(9) . . ? C97 S9X C103 94.3(4) . . ? N9X S9X C98 128.5(9) . . ? C97 S9X C98 36.7(3) . . ? C103 S9X C98 112.6(4) . . ? C102 C97 C98 120.7(7) . . ? C102 C97 S9X 149.6(7) . . ? C98 C97 S9X 89.3(6) . . ? C102 C97 S9 114.0(7) . . ? C98 C97 S9 124.7(6) . . ? C97 C98 C99 119.8(8) . . ? C97 C98 S9X 53.9(4) . . ? C99 C98 S9X 173.6(7) . . ? C100 C99 C98 119.1(9) . . ? C101 C100 C99 120.5(10) . . ? C100 C101 C102 119.0(10) . . ? C97 C102 C101 120.7(9) . . ? C104 C103 C108 121.7(8) . . ? C104 C103 S9 116.6(6) . . ? C108 C103 S9 121.1(6) . . ? C104 C103 S9X 143.0(6) . . ? C108 C103 S9X 93.4(6) . . ? C103 C104 C105 118.2(8) . . ? C106 C105 C104 122.0(8) . . ? C107 C106 C105 119.4(8) . . ? C106 C107 C108 120.1(9) . . ? C103 C108 C107 118.5(8) . . ? O3 N10 O1 118.9(6) . . ? O3 N10 O2 121.6(6) . . ? O1 N10 O2 119.5(5) . . ? O4 N11 O6 118.7(8) . . ? O4 N11 O5 117.7(8) . . ? O6 N11 O5 123.2(7) . . ? O9 N12 O8 118.1(7) . . ? O9 N12 O7 119.8(7) . . ? O8 N12 O7 122.1(7) . . ? O12 N13 O11 120.4(14) . . ? O12 N13 O10 122.0(13) . . ? O11 N13 O10 115.7(10) . . ? O12X N13X O11X 129(2) . . ? O12X N13X O10X 111(2) . . ? O11X N13X O10X 120(2) . . ? 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 N1 H1A O1W 0.88 2.19 2.978(6) 149.0 1_565 N2 H2A O11 0.88 2.14 2.977(9) 159.3 . N2 H2A O11X 0.88 2.28 3.12(3) 158.6 . N3 H3A O11X 0.88 2.52 3.15(3) 128.6 . N3 H3A O10 0.88 2.57 3.129(11) 122.5 . N4 H4A O1W 0.88 2.15 3.012(6) 165.6 1_565 N5 H5A O1 0.88 2.06 2.914(7) 164.7 . N8 H8A O2 0.88 2.35 3.224(7) 171.3 . N9 H9A O12 0.88 2.23 2.993(11) 144.4 2_465 _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.567 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.078 # END of data for (7) ## END of data for 6 compounds