# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Prof M Almeida' _publ_contact_author_address ; Quimica ITN E. N. 10 Sacav\'em P-2686-953 PORTUGAL ; _publ_contact_author_email MALMEIDA@ITN.PT _publ_section_title ; Multistability in a family of DT-TTF organic radical based compounds (DT-TTF)4[M(L)2]3 (M = Au, Cu; L = pds, pdt, bdt) ; loop_ _publ_author_name 'M. Almeida' 'Enric Canadell' 'Joao Dias' 'Pascale Foury-Leylekian' 'Rui T. Henriques' ; E.B.Lopes ; 'Jorge Morgado' 'Xavi Ribas' 'C. Rovira' 'Isabel Santos' 'Joao Seica' 'Jaume Veciana' ; J.Vidal-Gancedo ; 'Klaus Wurst' data_3cor _database_code_depnum_ccdc_archive 'CCDC 259175' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H28 Cu3 N12 S24 Se12' _chemical_formula_weight 2872.56 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' 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 32.8784(2) _cell_length_b 9.6280(4) _cell_length_c 26.7125(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.853(2) _cell_angle_gamma 90.00 _cell_volume 8355.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 93377 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 24.0 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5500 _exptl_absorpt_coefficient_mu 6.636 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19605 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 22.50 _reflns_number_total 10768 _reflns_number_gt 8500 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; racemic twin with small crystal size and low diffraction, carbon atoms were refined isotropically because of low ratio of reflection to parameter and negativ displacement parameter for several carbon atoms. ; _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^)+(0.0240P)^2^+79.3052P] 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 riding _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 0.382(11) _refine_ls_number_reflns 10768 _refine_ls_number_parameters 717 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.003 _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 0.73032(5) 0.29292(15) 0.46507(6) 0.0266(4) Uani 1 1 d . . . Cu2 Cu 0.65615(5) 0.11435(15) 0.69857(6) 0.0279(4) Uani 1 1 d . . . Cu3 Cu 0.44339(6) 0.67276(16) 0.83947(8) 0.0399(5) Uani 1 1 d . . . Se1 Se 0.67646(4) 0.34076(14) 0.40222(5) 0.0334(4) Uani 1 1 d . . . Se2 Se 0.68708(4) 0.24591(13) 0.52268(5) 0.0338(4) Uani 1 1 d . . . Se3 Se 0.77203(4) 0.35120(15) 0.40682(6) 0.0370(4) Uani 1 1 d . . . Se4 Se 0.78488(4) 0.23822(14) 0.52716(5) 0.0349(4) Uani 1 1 d . . . Se5 Se 0.60132(4) 0.04401(14) 0.63959(5) 0.0348(4) Uani 1 1 d . . . Se6 Se 0.61438(4) 0.18645(14) 0.75523(5) 0.0367(4) Uani 1 1 d . . . Se7 Se 0.69955(4) 0.04637(13) 0.64347(5) 0.0318(3) Uani 1 1 d . . . Se8 Se 0.70987(4) 0.18277(14) 0.75873(5) 0.0340(4) Uani 1 1 d . . . Se9 Se 0.44104(5) 0.87207(15) 0.88655(6) 0.0465(4) Uani 1 1 d . . . Se10 Se 0.45145(5) 0.53191(15) 0.91027(7) 0.0552(5) Uani 1 1 d . . . Se11 Se 0.43675(5) 0.81779(15) 0.77060(6) 0.0477(4) Uani 1 1 d . . . Se12 Se 0.44385(5) 0.47585(15) 0.79139(7) 0.0589(5) Uani 1 1 d . . . S1 S 0.62749(11) 0.6667(3) 0.38162(14) 0.0282(9) Uani 1 1 d . . . S2 S 0.50512(11) 0.8190(4) 0.36841(16) 0.0447(10) Uani 1 1 d . . . S3 S 0.62728(10) 0.9732(3) 0.39004(14) 0.0313(9) Uani 1 1 d . . . S4 S 0.72556(11) 0.6730(3) 0.38740(14) 0.0281(9) Uani 1 1 d . . . S5 S 0.84497(11) 0.8376(4) 0.38490(17) 0.0445(10) Uani 1 1 d . . . S6 S 0.72412(10) 0.9795(3) 0.39372(14) 0.0338(9) Uani 1 1 d . . . S7 S 0.63837(11) 0.6132(3) 0.50796(14) 0.0345(9) Uani 1 1 d . . . S8 S 0.51727(12) 0.7625(4) 0.51070(17) 0.0524(11) Uani 1 1 d . . . S9 S 0.63914(10) 0.9182(3) 0.52057(13) 0.0298(9) Uani 1 1 d . . . S10 S 0.73490(11) 0.6103(3) 0.51339(14) 0.0348(9) Uani 1 1 d . . . S11 S 0.85792(11) 0.7527(4) 0.52633(17) 0.0477(11) Uani 1 1 d . . . S12 S 0.73754(11) 0.9166(3) 0.52489(14) 0.0337(9) Uani 1 1 d . . . S13 S 0.65109(11) 0.4122(3) 0.63105(15) 0.0377(9) Uani 1 1 d . . . S14 S 0.52899(11) 0.5507(4) 0.63630(17) 0.0477(11) Uani 1 1 d . . . S15 S 0.64957(11) 0.7183(3) 0.64433(14) 0.0298(8) Uani 1 1 d . . . S16 S 0.74763(10) 0.4172(3) 0.63751(15) 0.0378(9) Uani 1 1 d . . . S17 S 0.87078(12) 0.5673(4) 0.65588(16) 0.0474(11) Uani 1 1 d . . . S18 S 0.74892(10) 0.7242(3) 0.64910(14) 0.0329(9) Uani 1 1 d . . . S19 S 0.65972(10) 0.5164(3) 0.76762(14) 0.0312(9) Uani 1 1 d . . . S20 S 0.54013(11) 0.6739(3) 0.77651(17) 0.0429(10) Uani 1 1 d . . . S21 S 0.66130(11) 0.8250(3) 0.77487(15) 0.0305(9) Uani 1 1 d . . . S22 S 0.75754(10) 0.5132(3) 0.77406(14) 0.0318(9) Uani 1 1 d . . . S23 S 0.88073(11) 0.6636(4) 0.79453(16) 0.0422(10) Uani 1 1 d . . . S24 S 0.75851(12) 0.8217(3) 0.77979(15) 0.0345(10) Uani 1 1 d . . . N1 N 0.5925(4) 0.3406(12) 0.4066(5) 0.048(3) Uani 1 1 d . . . N2 N 0.6016(4) 0.2363(12) 0.5065(5) 0.047(3) Uani 1 1 d . . . N3 N 0.8560(4) 0.3379(12) 0.4176(5) 0.048(4) Uani 1 1 d . . . N4 N 0.8672(3) 0.2192(13) 0.5153(5) 0.051(4) Uani 1 1 d . . . N5 N 0.5193(4) 0.0287(12) 0.6516(5) 0.046(3) Uani 1 1 d . . . N6 N 0.5293(4) 0.1759(12) 0.7457(5) 0.045(3) Uani 1 1 d . . . N7 N 0.7842(3) 0.0456(11) 0.6582(5) 0.037(3) Uani 1 1 d . . . N8 N 0.7930(4) 0.1761(11) 0.7540(5) 0.047(4) Uani 1 1 d . . . N9 N 0.4577(4) 0.8987(14) 0.9896(6) 0.060(4) Uani 1 1 d . . . N10 N 0.4649(4) 0.6138(16) 1.0126(6) 0.070(5) Uani 1 1 d . . . N11 N 0.4248(4) 0.7417(17) 0.6694(6) 0.074(5) Uani 1 1 d . . . N12 N 0.4279(3) 0.4525(15) 0.6880(6) 0.071(5) Uani 1 1 d . . . C1 C 0.6296(4) 0.3134(13) 0.4360(5) 0.033(3) Uiso 1 1 d . . . C2 C 0.6344(4) 0.2669(13) 0.4833(5) 0.033(3) Uiso 1 1 d . . . C3 C 0.5656(5) 0.2618(16) 0.4762(6) 0.057(4) Uiso 1 1 d . . . H3 H 0.5414 0.2437 0.4898 0.069 Uiso 1 1 calc . . . C4 C 0.5608(5) 0.3100(14) 0.4290(6) 0.043(4) Uiso 1 1 d . . . H4 H 0.5341 0.3225 0.4113 0.051 Uiso 1 1 calc . . . C5 C 0.8253(4) 0.3120(12) 0.4428(5) 0.029(3) Uiso 1 1 d . . . C6 C 0.8299(4) 0.2592(13) 0.4915(5) 0.034(3) Uiso 1 1 d . . . C7 C 0.8985(5) 0.2409(16) 0.4894(7) 0.058(5) Uiso 1 1 d . . . H7 H 0.9251 0.2134 0.5042 0.070 Uiso 1 1 calc . . . C8 C 0.8935(5) 0.3014(15) 0.4424(6) 0.052(4) Uiso 1 1 d . . . H8 H 0.9168 0.3181 0.4269 0.063 Uiso 1 1 calc . . . C9 C 0.5561(4) 0.0764(12) 0.6753(5) 0.028(3) Uiso 1 1 d . . . C10 C 0.5615(4) 0.1420(12) 0.7198(5) 0.033(3) Uiso 1 1 d . . . C11 C 0.4918(6) 0.1333(17) 0.7205(7) 0.063(5) Uiso 1 1 d . . . H11 H 0.4679 0.1553 0.7342 0.076 Uiso 1 1 calc . . . C12 C 0.4883(5) 0.0605(16) 0.6767(7) 0.061(5) Uiso 1 1 d . . . H12 H 0.4618 0.0298 0.6627 0.073 Uiso 1 1 calc . . . C13 C 0.7521(4) 0.0831(13) 0.6801(5) 0.032(3) Uiso 1 1 d . . . C14 C 0.7562(4) 0.1451(12) 0.7279(5) 0.026(3) Uiso 1 1 d . . . C15 C 0.8251(5) 0.1389(15) 0.7283(6) 0.050(4) Uiso 1 1 d . . . H15 H 0.8518 0.1591 0.7447 0.060 Uiso 1 1 calc . . . C16 C 0.8224(5) 0.0797(14) 0.6845(6) 0.046(4) Uiso 1 1 d . . . H16 H 0.8463 0.0599 0.6706 0.056 Uiso 1 1 calc . . . C17 C 0.4534(4) 0.8008(16) 0.9532(6) 0.047(4) Uiso 1 1 d . . . C18 C 0.4570(4) 0.6654(14) 0.9645(6) 0.046(4) Uiso 1 1 d . . . C19 C 0.4687(6) 0.715(2) 1.0481(7) 0.073(5) Uiso 1 1 d . . . H19 H 0.4737 0.6888 1.0824 0.087 Uiso 1 1 calc . . . C20 C 0.4658(6) 0.8497(19) 1.0375(7) 0.075(5) Uiso 1 1 d . . . H20 H 0.4696 0.9136 1.0644 0.090 Uiso 1 1 calc . . . C21 C 0.4310(4) 0.6895(14) 0.7163(6) 0.041(4) Uiso 1 1 d . . . C22 C 0.4335(5) 0.5460(16) 0.7275(6) 0.057(4) Uiso 1 1 d . . . C23 C 0.4209(6) 0.513(2) 0.6406(8) 0.079(6) Uiso 1 1 d . . . H23 H 0.4172 0.4533 0.6125 0.095 Uiso 1 1 calc . . . C24 C 0.4190(6) 0.646(2) 0.6311(8) 0.081(6) Uiso 1 1 d . . . H24 H 0.4135 0.6762 0.5973 0.097 Uiso 1 1 calc . . . C25 C 0.6555(4) 0.8206(12) 0.3878(5) 0.028(3) Uiso 1 1 d . . . C26 C 0.5797(4) 0.7460(12) 0.3777(4) 0.024(3) Uiso 1 1 d . . . C27 C 0.5415(4) 0.6926(14) 0.3694(5) 0.036(3) Uiso 1 1 d . . . H27 H 0.5355 0.5976 0.3647 0.044 Uiso 1 1 calc . . . C28 C 0.5413(4) 0.9493(14) 0.3778(5) 0.039(4) Uiso 1 1 d . . . H28 H 0.5356 1.0446 0.3801 0.047 Uiso 1 1 calc . . . C29 C 0.5790(4) 0.8931(12) 0.3816(5) 0.028(3) Uiso 1 1 d . . . C30 C 0.6975(4) 0.8235(12) 0.3900(5) 0.030(3) Uiso 1 1 d . . . C31 C 0.7727(4) 0.7566(12) 0.3880(5) 0.026(3) Uiso 1 1 d . . . C32 C 0.8090(4) 0.7046(13) 0.3845(5) 0.034(3) Uiso 1 1 d . . . H32 H 0.8148 0.6095 0.3820 0.041 Uiso 1 1 calc . . . C33 C 0.8097(5) 0.9647(14) 0.3876(6) 0.043(4) Uiso 1 1 d . . . H33 H 0.8152 1.0606 0.3884 0.051 Uiso 1 1 calc . . . C34 C 0.7710(4) 0.9033(12) 0.3883(5) 0.023(3) Uiso 1 1 d . . . C35 C 0.6670(4) 0.7653(12) 0.5155(5) 0.026(3) Uiso 1 1 d . . . C36 C 0.5909(4) 0.6914(13) 0.5100(5) 0.037(3) Uiso 1 1 d . . . C37 C 0.5520(4) 0.6343(14) 0.5064(5) 0.040(3) Uiso 1 1 d . . . H37 H 0.5457 0.5393 0.5021 0.048 Uiso 1 1 calc . . . C38 C 0.5545(4) 0.8953(14) 0.5180(5) 0.041(4) Uiso 1 1 d . . . H38 H 0.5495 0.9905 0.5220 0.049 Uiso 1 1 calc . . . C39 C 0.5907(4) 0.8365(13) 0.5169(5) 0.033(3) Uiso 1 1 d . . . C40 C 0.7085(4) 0.7678(12) 0.5172(5) 0.027(3) Uiso 1 1 d . . . C41 C 0.7838(4) 0.6845(13) 0.5190(5) 0.035(3) Uiso 1 1 d . . . C42 C 0.8210(4) 0.6266(13) 0.5202(5) 0.036(3) Uiso 1 1 d . . . H42 H 0.8261 0.5309 0.5180 0.043 Uiso 1 1 calc . . . C43 C 0.8229(5) 0.8837(14) 0.5278(6) 0.042(4) Uiso 1 1 d . . . H43 H 0.8299 0.9784 0.5301 0.050 Uiso 1 1 calc . . . C44 C 0.7851(4) 0.8373(12) 0.5254(5) 0.026(3) Uiso 1 1 d . . . C45 C 0.6788(4) 0.5687(11) 0.6391(4) 0.023(3) Uiso 1 1 d . . . C46 C 0.6035(4) 0.4903(12) 0.6336(5) 0.030(3) Uiso 1 1 d . . . C47 C 0.5657(4) 0.4277(13) 0.6297(5) 0.038(3) Uiso 1 1 d . . . H47 H 0.5606 0.3324 0.6242 0.045 Uiso 1 1 calc . . . C48 C 0.5639(4) 0.6844(13) 0.6419(5) 0.038(4) Uiso 1 1 d . . . H48 H 0.5576 0.7786 0.6458 0.046 Uiso 1 1 calc . . . C49 C 0.6023(4) 0.6333(12) 0.6397(5) 0.027(3) Uiso 1 1 d . . . C50 C 0.7200(3) 0.5697(10) 0.6416(4) 0.018(3) Uiso 1 1 d . . . C51 C 0.7961(4) 0.4950(12) 0.6453(5) 0.025(3) Uiso 1 1 d . . . C52 C 0.8335(4) 0.4383(14) 0.6470(5) 0.042(4) Uiso 1 1 d . . . H52 H 0.8388 0.3430 0.6438 0.050 Uiso 1 1 calc . . . C53 C 0.8350(4) 0.6947(13) 0.6579(5) 0.033(3) Uiso 1 1 d . . . H53 H 0.8413 0.7896 0.6624 0.040 Uiso 1 1 calc . . . C54 C 0.7961(4) 0.6418(13) 0.6522(5) 0.033(3) Uiso 1 1 d . . . C55 C 0.6887(4) 0.6689(11) 0.7742(5) 0.027(3) Uiso 1 1 d . . . C56 C 0.6131(4) 0.6003(13) 0.7715(5) 0.031(3) Uiso 1 1 d . . . C57 C 0.5752(4) 0.5446(13) 0.7726(5) 0.032(3) Uiso 1 1 d . . . H57 H 0.5692 0.4491 0.7714 0.038 Uiso 1 1 calc . . . C58 C 0.5760(4) 0.8005(13) 0.7782(5) 0.032(3) Uiso 1 1 d . . . H58 H 0.5707 0.8959 0.7810 0.038 Uiso 1 1 calc . . . C59 C 0.6133(4) 0.7459(12) 0.7750(5) 0.029(3) Uiso 1 1 d . . . C60 C 0.7294(4) 0.6693(11) 0.7770(5) 0.024(3) Uiso 1 1 d . . . C61 C 0.8052(4) 0.5936(13) 0.7837(5) 0.035(3) Uiso 1 1 d . . . C62 C 0.8440(4) 0.5352(14) 0.7869(5) 0.041(4) Uiso 1 1 d . . . H62 H 0.8495 0.4396 0.7852 0.049 Uiso 1 1 calc . . . C63 C 0.8454(4) 0.7946(13) 0.7933(5) 0.028(3) Uiso 1 1 d . . . H63 H 0.8520 0.8895 0.7966 0.034 Uiso 1 1 calc . . . C64 C 0.8057(4) 0.7417(12) 0.7870(5) 0.030(3) Uiso 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 0.0243(8) 0.0245(7) 0.0311(9) -0.0010(7) 0.0042(7) 0.0020(6) Cu2 0.0238(8) 0.0288(8) 0.0311(9) -0.0027(7) 0.0051(7) -0.0006(7) Cu3 0.0225(7) 0.0337(8) 0.0627(13) 0.0059(8) 0.0037(8) -0.0010(6) Se1 0.0276(8) 0.0389(8) 0.0330(9) 0.0028(6) 0.0019(7) 0.0028(6) Se2 0.0277(8) 0.0372(7) 0.0373(9) 0.0074(7) 0.0068(7) 0.0004(6) Se3 0.0304(9) 0.0474(9) 0.0343(9) 0.0085(7) 0.0085(7) 0.0040(6) Se4 0.0276(8) 0.0427(8) 0.0343(9) 0.0057(7) 0.0045(7) 0.0013(6) Se5 0.0252(8) 0.0433(8) 0.0353(9) -0.0090(7) 0.0028(7) 0.0004(6) Se6 0.0286(9) 0.0448(8) 0.0374(9) -0.0125(7) 0.0078(7) -0.0018(6) Se7 0.0265(7) 0.0349(7) 0.0343(8) -0.0044(6) 0.0056(6) 0.0012(6) Se8 0.0283(8) 0.0376(7) 0.0354(9) -0.0074(7) 0.0031(7) -0.0021(6) Se9 0.0497(10) 0.0358(8) 0.0524(11) 0.0074(7) 0.0030(8) -0.0049(7) Se10 0.0393(9) 0.0431(9) 0.0837(13) 0.0251(9) 0.0106(8) 0.0052(7) Se11 0.0439(10) 0.0434(8) 0.0562(11) 0.0069(8) 0.0087(8) 0.0127(7) Se12 0.0392(9) 0.0363(8) 0.0986(14) -0.0076(9) 0.0021(9) -0.0042(7) S1 0.025(2) 0.0215(17) 0.038(2) 0.0012(15) 0.0032(17) -0.0013(14) S2 0.025(2) 0.050(2) 0.059(3) -0.0035(19) 0.0051(19) 0.0025(16) S3 0.0228(19) 0.0262(17) 0.045(2) -0.0045(16) 0.0056(16) 0.0023(14) S4 0.022(2) 0.0261(17) 0.037(2) -0.0006(15) 0.0072(17) 0.0022(14) S5 0.023(2) 0.043(2) 0.067(3) 0.0003(19) 0.008(2) -0.0025(16) S6 0.028(2) 0.0277(17) 0.046(2) -0.0032(16) 0.0062(17) -0.0027(15) S7 0.035(2) 0.0298(18) 0.039(2) -0.0053(17) 0.0055(17) -0.0066(16) S8 0.025(2) 0.067(3) 0.067(3) -0.001(2) 0.011(2) -0.0080(18) S9 0.024(2) 0.0253(17) 0.039(2) -0.0043(15) 0.0033(16) -0.0028(14) S10 0.032(2) 0.0259(17) 0.046(2) -0.0075(17) 0.0053(17) -0.0033(16) S11 0.026(2) 0.046(2) 0.071(3) 0.003(2) 0.008(2) 0.0074(17) S12 0.0274(19) 0.0286(17) 0.044(2) -0.0019(17) 0.0010(17) -0.0001(15) S13 0.031(2) 0.0240(17) 0.059(3) 0.0017(16) 0.0095(18) 0.0007(14) S14 0.027(2) 0.043(2) 0.074(3) 0.009(2) 0.009(2) -0.0034(16) S15 0.0241(19) 0.0286(17) 0.036(2) -0.0007(16) 0.0036(16) -0.0012(15) S16 0.028(2) 0.0288(18) 0.057(3) 0.0014(17) 0.0061(18) 0.0057(14) S17 0.028(2) 0.053(2) 0.061(3) 0.000(2) 0.006(2) 0.0037(17) S18 0.028(2) 0.0275(18) 0.044(2) 0.0010(16) 0.0079(18) 0.0036(15) S19 0.0229(18) 0.0275(17) 0.043(2) -0.0025(16) 0.0047(16) -0.0004(15) S20 0.025(2) 0.041(2) 0.064(3) 0.0041(19) 0.013(2) 0.0011(16) S21 0.029(2) 0.0199(16) 0.041(2) 0.0032(16) 0.0012(18) -0.0016(15) S22 0.0258(18) 0.0241(17) 0.046(2) 0.0031(16) 0.0054(17) -0.0001(14) S23 0.024(2) 0.045(2) 0.058(3) -0.0031(19) 0.0087(19) 0.0002(16) S24 0.029(2) 0.0242(17) 0.050(3) 0.0007(17) 0.0072(19) 0.0022(15) N1 0.038(8) 0.064(8) 0.044(8) 0.005(6) 0.016(7) -0.005(6) N2 0.035(8) 0.057(8) 0.051(9) 0.012(7) 0.011(7) 0.001(6) N3 0.030(8) 0.059(8) 0.059(9) 0.016(7) 0.020(7) 0.004(6) N4 0.021(7) 0.078(9) 0.054(9) 0.016(7) 0.004(6) 0.003(6) N5 0.036(8) 0.060(8) 0.042(8) -0.019(7) 0.006(6) 0.000(6) N6 0.038(8) 0.058(8) 0.038(8) -0.019(6) 0.001(6) 0.007(6) N7 0.028(7) 0.040(7) 0.049(8) -0.016(6) 0.020(6) -0.004(5) N8 0.022(7) 0.051(7) 0.067(10) -0.013(7) 0.002(7) -0.009(5) N9 0.048(9) 0.078(9) 0.059(10) 0.025(8) 0.020(7) -0.003(7) N10 0.025(8) 0.090(10) 0.093(12) 0.056(10) 0.008(7) 0.017(7) N11 0.020(8) 0.117(12) 0.083(12) 0.005(10) 0.001(7) 0.005(8) N12 0.015(7) 0.095(10) 0.102(12) -0.035(9) 0.008(7) 0.023(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Se1 2.292(2) . ? Cu1 Se2 2.295(2) . ? Cu1 Se3 2.296(2) . ? Cu1 Se4 2.309(2) . ? Cu2 Se8 2.294(2) . ? Cu2 Se7 2.297(2) . ? Cu2 Se6 2.302(2) . ? Cu2 Se5 2.306(2) . ? Cu3 Se12 2.291(2) . ? Cu3 Se11 2.293(2) . ? Cu3 Se9 2.302(2) . ? Cu3 Se10 2.309(3) . ? Se1 C1 1.920(15) . ? Se2 C2 1.894(13) . ? Se3 C5 1.900(13) . ? Se4 C6 1.889(14) . ? Se5 C9 1.912(14) . ? Se6 C10 1.898(13) . ? Se7 C13 1.884(13) . ? Se8 C14 1.877(14) . ? Se9 C17 1.892(15) . ? Se10 C18 1.924(15) . ? Se11 C21 1.892(14) . ? Se12 C22 1.817(16) . ? S1 C26 1.736(12) . ? S1 C25 1.740(12) . ? S2 C27 1.703(14) . ? S2 C28 1.721(14) . ? S3 C25 1.745(12) . ? S3 C29 1.747(13) . ? S4 C30 1.725(12) . ? S4 C31 1.745(13) . ? S5 C33 1.695(15) . ? S5 C32 1.741(14) . ? S6 C34 1.732(13) . ? S6 C30 1.733(12) . ? S7 C35 1.737(12) . ? S7 C36 1.740(14) . ? S8 C37 1.698(14) . ? S8 C38 1.759(14) . ? S9 C35 1.751(12) . ? S9 C39 1.764(14) . ? S10 C41 1.743(13) . ? S10 C40 1.757(12) . ? S11 C42 1.705(13) . ? S11 C43 1.714(15) . ? S12 C40 1.716(12) . ? S12 C44 1.737(13) . ? S13 C46 1.746(13) . ? S13 C45 1.757(11) . ? S14 C48 1.717(14) . ? S14 C47 1.718(14) . ? S15 C49 1.745(13) . ? S15 C45 1.749(12) . ? S16 C50 1.739(11) . ? S16 C51 1.743(12) . ? S17 C53 1.708(13) . ? S17 C52 1.735(14) . ? S18 C54 1.731(14) . ? S18 C50 1.761(11) . ? S19 C55 1.745(12) . ? S19 C56 1.751(14) . ? S20 C58 1.692(14) . ? S20 C57 1.712(13) . ? S21 C59 1.752(13) . ? S21 C55 1.754(12) . ? S22 C61 1.733(14) . ? S22 C60 1.773(12) . ? S23 C63 1.711(13) . ? S23 C62 1.718(14) . ? S24 C64 1.717(13) . ? S24 C60 1.748(12) . ? N1 C4 1.31(2) . ? N1 C1 1.371(18) . ? N2 C3 1.350(19) . ? N2 C2 1.355(18) . ? N3 C5 1.322(18) . ? N3 C8 1.352(19) . ? N4 C7 1.34(2) . ? N4 C6 1.349(16) . ? N5 C12 1.34(2) . ? N5 C9 1.356(16) . ? N6 C11 1.37(2) . ? N6 C10 1.388(19) . ? N7 C13 1.331(17) . ? N7 C16 1.380(18) . ? N8 C14 1.332(16) . ? N8 C15 1.39(2) . ? N9 C17 1.346(19) . ? N9 C20 1.35(2) . ? N10 C19 1.35(2) . ? N10 C18 1.366(19) . ? N11 C21 1.335(19) . ? N11 C24 1.37(2) . ? N12 C22 1.379(19) . ? N12 C23 1.38(2) . ? C1 C2 1.329(18) . ? C3 C4 1.33(2) . ? C5 C6 1.384(18) . ? C7 C8 1.37(2) . ? C9 C10 1.332(17) . ? C11 C12 1.35(2) . ? C13 C14 1.398(18) . ? C15 C16 1.29(2) . ? C17 C18 1.339(18) . ? C19 C20 1.33(2) . ? C21 C22 1.413(19) . ? C23 C24 1.30(2) . ? C25 C30 1.372(17) . ? C26 C27 1.345(17) . ? C26 C29 1.420(16) . ? C28 C29 1.342(18) . ? C31 C32 1.312(17) . ? C31 C34 1.414(16) . ? C33 C34 1.407(18) . ? C35 C40 1.358(16) . ? C36 C37 1.383(18) . ? C36 C39 1.410(17) . ? C38 C39 1.324(18) . ? C41 C42 1.342(17) . ? C41 C44 1.481(16) . ? C43 C44 1.313(19) . ? C45 C50 1.345(14) . ? C46 C47 1.373(18) . ? C46 C49 1.388(16) . ? C48 C49 1.362(19) . ? C51 C52 1.341(17) . ? C51 C54 1.426(17) . ? C53 C54 1.363(18) . ? C55 C60 1.328(16) . ? C56 C57 1.359(18) . ? C56 C59 1.404(17) . ? C58 C59 1.349(18) . ? C61 C62 1.384(18) . ? C61 C64 1.428(17) . ? C63 C64 1.386(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 Se1 Cu1 Se2 92.43(8) . . ? Se1 Cu1 Se3 85.94(8) . . ? Se2 Cu1 Se3 177.01(9) . . ? Se1 Cu1 Se4 178.21(9) . . ? Se2 Cu1 Se4 88.07(8) . . ? Se3 Cu1 Se4 93.64(7) . . ? Se8 Cu2 Se7 92.49(8) . . ? Se8 Cu2 Se6 85.73(7) . . ? Se7 Cu2 Se6 178.15(9) . . ? Se8 Cu2 Se5 178.66(10) . . ? Se7 Cu2 Se5 88.63(7) . . ? Se6 Cu2 Se5 93.16(7) . . ? Se12 Cu3 Se11 93.56(10) . . ? Se12 Cu3 Se9 178.32(11) . . ? Se11 Cu3 Se9 85.62(8) . . ? Se12 Cu3 Se10 87.90(9) . . ? Se11 Cu3 Se10 178.16(11) . . ? Se9 Cu3 Se10 92.95(9) . . ? C1 Se1 Cu1 102.4(4) . . ? C2 Se2 Cu1 102.4(5) . . ? C5 Se3 Cu1 102.0(4) . . ? C6 Se4 Cu1 101.3(4) . . ? C9 Se5 Cu2 101.4(4) . . ? C10 Se6 Cu2 101.4(5) . . ? C13 Se7 Cu2 103.0(5) . . ? C14 Se8 Cu2 103.1(4) . . ? C17 Se9 Cu3 101.0(5) . . ? C18 Se10 Cu3 102.1(4) . . ? C21 Se11 Cu3 101.7(4) . . ? C22 Se12 Cu3 101.7(5) . . ? C26 S1 C25 95.3(6) . . ? C27 S2 C28 92.9(7) . . ? C25 S3 C29 95.8(6) . . ? C30 S4 C31 95.3(6) . . ? C33 S5 C32 93.7(7) . . ? C34 S6 C30 94.4(6) . . ? C35 S7 C36 96.0(6) . . ? C37 S8 C38 94.2(7) . . ? C35 S9 C39 95.8(6) . . ? C41 S10 C40 95.6(6) . . ? C42 S11 C43 93.2(7) . . ? C40 S12 C44 96.7(6) . . ? C46 S13 C45 94.4(6) . . ? C48 S14 C47 93.1(7) . . ? C49 S15 C45 95.9(6) . . ? C50 S16 C51 96.1(5) . . ? C53 S17 C52 92.5(7) . . ? C54 S18 C50 94.7(6) . . ? C55 S19 C56 94.3(6) . . ? C58 S20 C57 93.0(7) . . ? C59 S21 C55 95.3(6) . . ? C61 S22 C60 94.6(6) . . ? C63 S23 C62 93.8(7) . . ? C64 S24 C60 96.2(6) . . ? C4 N1 C1 113.2(13) . . ? C3 N2 C2 111.9(13) . . ? C5 N3 C8 114.4(13) . . ? C7 N4 C6 115.2(13) . . ? C12 N5 C9 112.4(12) . . ? C11 N6 C10 112.4(13) . . ? C13 N7 C16 115.6(12) . . ? C14 N8 C15 112.3(13) . . ? C17 N9 C20 115.0(14) . . ? C19 N10 C18 112.3(14) . . ? C21 N11 C24 115.5(16) . . ? C22 N12 C23 114.1(15) . . ? C2 C1 N1 125.0(14) . . ? C2 C1 Se1 120.5(10) . . ? N1 C1 Se1 114.4(11) . . ? C1 C2 N2 121.4(12) . . ? C1 C2 Se2 121.9(11) . . ? N2 C2 Se2 116.6(10) . . ? C4 C3 N2 126.5(16) . . ? N1 C4 C3 121.8(14) . . ? N3 C5 C6 124.5(13) . . ? N3 C5 Se3 115.0(10) . . ? C6 C5 Se3 120.5(11) . . ? N4 C6 C5 120.6(13) . . ? N4 C6 Se4 117.2(10) . . ? C5 C6 Se4 122.2(10) . . ? N4 C7 C8 123.0(15) . . ? N3 C8 C7 122.1(16) . . ? C10 C9 N5 124.3(13) . . ? C10 C9 Se5 121.1(10) . . ? N5 C9 Se5 114.6(9) . . ? C9 C10 N6 123.3(12) . . ? C9 C10 Se6 122.5(11) . . ? N6 C10 Se6 114.1(10) . . ? C12 C11 N6 121.9(17) . . ? N5 C12 C11 125.4(16) . . ? N7 C13 C14 123.1(12) . . ? N7 C13 Se7 116.5(10) . . ? C14 C13 Se7 120.4(10) . . ? N8 C14 C13 121.8(13) . . ? N8 C14 Se8 117.3(10) . . ? C13 C14 Se8 120.9(10) . . ? C16 C15 N8 127.5(14) . . ? C15 C16 N7 119.7(15) . . ? C18 C17 N9 121.5(15) . . ? C18 C17 Se9 124.3(12) . . ? N9 C17 Se9 114.2(11) . . ? C17 C18 N10 124.3(15) . . ? C17 C18 Se10 119.0(12) . . ? N10 C18 Se10 116.6(11) . . ? C20 C19 N10 124.0(18) . . ? C19 C20 N9 122.8(17) . . ? N11 C21 C22 124.2(15) . . ? N11 C21 Se11 117.1(11) . . ? C22 C21 Se11 118.7(11) . . ? N12 C22 C21 118.7(15) . . ? N12 C22 Se12 117.4(12) . . ? C21 C22 Se12 124.0(12) . . ? C24 C23 N12 126.2(19) . . ? C23 C24 N11 121(2) . . ? C30 C25 S1 122.5(9) . . ? C30 C25 S3 121.2(9) . . ? S1 C25 S3 116.3(7) . . ? C27 C26 C29 111.6(11) . . ? C27 C26 S1 131.0(10) . . ? C29 C26 S1 117.3(9) . . ? C26 C27 S2 111.4(10) . . ? C29 C28 S2 109.1(10) . . ? C28 C29 C26 114.9(11) . . ? C28 C29 S3 129.9(10) . . ? C26 C29 S3 115.2(9) . . ? C25 C30 S4 121.4(9) . . ? C25 C30 S6 121.1(9) . . ? S4 C30 S6 117.5(8) . . ? C32 C31 C34 114.8(11) . . ? C32 C31 S4 129.9(10) . . ? C34 C31 S4 115.1(9) . . ? C31 C32 S5 110.1(10) . . ? C34 C33 S5 108.9(10) . . ? C33 C34 C31 112.5(11) . . ? C33 C34 S6 129.9(10) . . ? C31 C34 S6 117.4(9) . . ? C40 C35 S7 122.9(9) . . ? C40 C35 S9 121.2(9) . . ? S7 C35 S9 115.9(7) . . ? C37 C36 C39 112.4(12) . . ? C37 C36 S7 130.6(10) . . ? C39 C36 S7 117.1(10) . . ? C36 C37 S8 109.3(10) . . ? C39 C38 S8 107.4(10) . . ? C38 C39 C36 116.7(13) . . ? C38 C39 S9 128.0(10) . . ? C36 C39 S9 115.2(10) . . ? C35 C40 S12 123.7(9) . . ? C35 C40 S10 119.0(9) . . ? S12 C40 S10 117.2(7) . . ? C42 C41 C44 113.6(12) . . ? C42 C41 S10 131.2(10) . . ? C44 C41 S10 115.2(9) . . ? C41 C42 S11 109.9(10) . . ? C44 C43 S11 112.6(10) . . ? C43 C44 C41 110.7(12) . . ? C43 C44 S12 134.0(10) . . ? C41 C44 S12 115.2(9) . . ? C50 C45 S15 123.5(8) . . ? C50 C45 S13 120.7(8) . . ? S15 C45 S13 115.8(7) . . ? C47 C46 C49 113.7(12) . . ? C47 C46 S13 128.0(10) . . ? C49 C46 S13 118.3(10) . . ? C46 C47 S14 109.4(9) . . ? C49 C48 S14 109.7(10) . . ? C48 C49 C46 114.0(12) . . ? C48 C49 S15 130.4(10) . . ? C46 C49 S15 115.6(10) . . ? C45 C50 S16 121.5(8) . . ? C45 C50 S18 122.3(8) . . ? S16 C50 S18 116.2(7) . . ? C52 C51 C54 114.7(11) . . ? C52 C51 S16 130.2(10) . . ? C54 C51 S16 115.1(9) . . ? C51 C52 S17 109.8(10) . . ? C54 C53 S17 111.6(10) . . ? C53 C54 C51 111.5(12) . . ? C53 C54 S18 130.7(10) . . ? C51 C54 S18 117.7(9) . . ? C60 C55 S19 122.5(9) . . ? C60 C55 S21 120.8(9) . . ? S19 C55 S21 116.6(7) . . ? C57 C56 C59 112.9(12) . . ? C57 C56 S19 129.2(10) . . ? C59 C56 S19 117.9(10) . . ? C56 C57 S20 110.0(9) . . ? C59 C58 S20 110.8(10) . . ? C58 C59 C56 113.4(12) . . ? C58 C59 S21 131.2(10) . . ? C56 C59 S21 115.5(9) . . ? C55 C60 S24 123.0(9) . . ? C55 C60 S22 121.5(9) . . ? S24 C60 S22 115.3(7) . . ? C62 C61 C64 113.6(12) . . ? C62 C61 S22 129.2(10) . . ? C64 C61 S22 117.2(10) . . ? C61 C62 S23 109.8(10) . . ? C64 C63 S23 110.8(9) . . ? C63 C64 C61 112.0(11) . . ? C63 C64 S24 131.8(10) . . ? C61 C64 S24 116.1(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.598 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.116 data_4cor _database_code_depnum_ccdc_archive 'CCDC 259176' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H28 Cu3 N12 S36' _chemical_formula_weight 2309.76 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' 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 Cc 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' _cell_length_a 32.5313(2) _cell_length_b 9.4923(4) _cell_length_c 26.3669(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.166(2) _cell_angle_gamma 90.00 _cell_volume 8038.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 34056 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 24.0 _exptl_crystal_description prism _exptl_crystal_colour plack _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.909 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4636 _exptl_absorpt_coefficient_mu 1.776 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20764 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 24.17 _reflns_number_total 11754 _reflns_number_gt 9411 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0265P)^2^+11.8460P] 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 riding _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 0.006(12) _refine_ls_number_reflns 11754 _refine_ls_number_parameters 1036 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.022 _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 0.72973(3) 0.29581(8) 0.46453(3) 0.0251(2) Uani 1 1 d . . . Cu2 Cu 0.65725(3) 0.11137(8) 0.69941(3) 0.0251(2) Uani 1 1 d . . . Cu3 Cu 0.44375(3) 0.66899(9) 0.83867(4) 0.0372(2) Uani 1 1 d . . . S1 S 0.62718(6) 0.66805(17) 0.37969(7) 0.0252(4) Uani 1 1 d . . . S2 S 0.50340(6) 0.8225(2) 0.36727(9) 0.0399(5) Uani 1 1 d . . . S3 S 0.62722(5) 0.97909(17) 0.38945(7) 0.0297(4) Uani 1 1 d . . . S4 S 0.72570(6) 0.67241(17) 0.38601(7) 0.0258(4) Uani 1 1 d . . . S5 S 0.84713(6) 0.83614(19) 0.38656(9) 0.0382(5) Uani 1 1 d . . . S6 S 0.72496(6) 0.98361(17) 0.39332(7) 0.0299(5) Uani 1 1 d . . . S7 S 0.63658(6) 0.61817(18) 0.50682(7) 0.0312(5) Uani 1 1 d . . . S8 S 0.51506(7) 0.7747(2) 0.51104(9) 0.0497(6) Uani 1 1 d . . . S9 S 0.63882(6) 0.92617(17) 0.52264(8) 0.0295(5) Uani 1 1 d . . . S10 S 0.73471(6) 0.61398(18) 0.51315(7) 0.0314(4) Uani 1 1 d . . . S11 S 0.85921(6) 0.7598(2) 0.52901(9) 0.0435(5) Uani 1 1 d . . . S12 S 0.73741(6) 0.92342(17) 0.52703(7) 0.0304(5) Uani 1 1 d . . . S13 S 0.65172(5) 0.40787(17) 0.62815(7) 0.0331(5) Uani 1 1 d . . . S14 S 0.52818(6) 0.5469(2) 0.63422(9) 0.0444(5) Uani 1 1 d . . . S15 S 0.65032(6) 0.71873(18) 0.64490(7) 0.0268(4) Uani 1 1 d . . . S16 S 0.74945(6) 0.41393(18) 0.63523(8) 0.0358(5) Uani 1 1 d . . . S17 S 0.87383(6) 0.5673(2) 0.65731(9) 0.0461(6) Uani 1 1 d . . . S18 S 0.75039(6) 0.72476(18) 0.65036(7) 0.0291(5) Uani 1 1 d . . . S19 S 0.66001(5) 0.50770(17) 0.76838(7) 0.0265(4) Uani 1 1 d . . . S20 S 0.53865(6) 0.66477(19) 0.77594(9) 0.0390(5) Uani 1 1 d . . . S21 S 0.66142(6) 0.82051(18) 0.77732(7) 0.0278(4) Uani 1 1 d . . . S22 S 0.75890(6) 0.50611(17) 0.77519(7) 0.0276(4) Uani 1 1 d . . . S23 S 0.88338(7) 0.65969(19) 0.79652(9) 0.0408(5) Uani 1 1 d . . . S24 S 0.75963(6) 0.81849(18) 0.78265(8) 0.0306(5) Uani 1 1 d . . . S25 S 0.67764(6) 0.34546(19) 0.40439(7) 0.0312(5) Uani 1 1 d . . . S26 S 0.68819(6) 0.24816(17) 0.51950(7) 0.0306(4) Uani 1 1 d . . . S27 S 0.77004(6) 0.3536(2) 0.40921(8) 0.0339(5) Uani 1 1 d . . . S28 S 0.78259(6) 0.24177(19) 0.52355(8) 0.0332(5) Uani 1 1 d . . . S29 S 0.60433(6) 0.0423(2) 0.64246(7) 0.0329(5) Uani 1 1 d . . . S30 S 0.61674(6) 0.1782(2) 0.75345(8) 0.0335(5) Uani 1 1 d . . . S31 S 0.69902(6) 0.04731(18) 0.64629(7) 0.0314(4) Uani 1 1 d . . . S32 S 0.70931(6) 0.17555(18) 0.75730(7) 0.0305(5) Uani 1 1 d . . . S33 S 0.44408(7) 0.8612(2) 0.88400(9) 0.0436(6) Uani 1 1 d . . . S34 S 0.45293(7) 0.5345(2) 0.90708(9) 0.0498(6) Uani 1 1 d . . . S35 S 0.43585(7) 0.8049(2) 0.77116(8) 0.0428(5) Uani 1 1 d . . . S36 S 0.44204(7) 0.4775(2) 0.79306(10) 0.0519(6) Uani 1 1 d . . . N1 N 0.5970(2) 0.3478(6) 0.4064(3) 0.0352(16) Uani 1 1 d . . . N2 N 0.6059(2) 0.2406(6) 0.5068(3) 0.0405(17) Uani 1 1 d . . . N3 N 0.8523(2) 0.3489(7) 0.4177(3) 0.0413(18) Uani 1 1 d . . . N4 N 0.8630(2) 0.2230(7) 0.5158(3) 0.0500(19) Uani 1 1 d . . . N5 N 0.5246(2) 0.0311(7) 0.6505(3) 0.0447(17) Uani 1 1 d . . . N6 N 0.5353(2) 0.1703(6) 0.7451(3) 0.0420(18) Uani 1 1 d . . . N7 N 0.7814(2) 0.0475(6) 0.6574(3) 0.0378(17) Uani 1 1 d . . . N8 N 0.7897(2) 0.1762(6) 0.7550(3) 0.0423(17) Uani 1 1 d . . . N9 N 0.4586(2) 0.8972(8) 0.9846(3) 0.057(2) Uani 1 1 d . . . N10 N 0.4649(2) 0.6068(8) 1.0061(3) 0.057(2) Uani 1 1 d . . . N11 N 0.4243(2) 0.7370(9) 0.6729(3) 0.062(2) Uani 1 1 d . . . N12 N 0.4279(2) 0.4436(8) 0.6928(4) 0.067(2) Uani 1 1 d . . . C1 C 0.6341(2) 0.3202(7) 0.4340(3) 0.0248(17) Uani 1 1 d . . . C2 C 0.6384(2) 0.2697(6) 0.4839(3) 0.0279(18) Uani 1 1 d . . . C3 C 0.5685(2) 0.2675(7) 0.4787(4) 0.045(2) Uani 1 1 d . . . H3 H 0.5445 0.2489 0.4933 0.054 Uiso 1 1 calc . . . C4 C 0.5638(3) 0.3205(8) 0.4300(4) 0.047(2) Uani 1 1 d . . . H4 H 0.5368 0.3384 0.4124 0.057 Uiso 1 1 calc . . . C5 C 0.8198(2) 0.3208(6) 0.4416(3) 0.0257(18) Uani 1 1 d . . . C6 C 0.8256(2) 0.2622(6) 0.4916(3) 0.0303(18) Uani 1 1 d . . . C7 C 0.8940(3) 0.2495(10) 0.4903(4) 0.060(3) Uani 1 1 d . . . H7 H 0.9209 0.2224 0.5055 0.072 Uiso 1 1 calc . . . C8 C 0.8895(3) 0.3135(9) 0.4435(4) 0.053(2) Uani 1 1 d . . . H8 H 0.9134 0.3332 0.4289 0.064 Uiso 1 1 calc . . . C9 C 0.5616(2) 0.0724(7) 0.6741(3) 0.0265(17) Uani 1 1 d . . . C10 C 0.5674(2) 0.1384(6) 0.7214(3) 0.0234(17) Uani 1 1 d . . . C11 C 0.4976(3) 0.1311(9) 0.7209(4) 0.052(2) Uani 1 1 d . . . H11 H 0.4741 0.1540 0.7358 0.063 Uiso 1 1 calc . . . C12 C 0.4922(2) 0.0597(10) 0.6758(4) 0.058(3) Uani 1 1 d . . . H12 H 0.4653 0.0290 0.6617 0.070 Uiso 1 1 calc . . . C13 C 0.7483(2) 0.0813(7) 0.6798(3) 0.0293(18) Uani 1 1 d . . . C14 C 0.7527(2) 0.1427(6) 0.7287(3) 0.0257(18) Uani 1 1 d . . . C15 C 0.8229(3) 0.1437(8) 0.7321(4) 0.044(2) Uani 1 1 d . . . H15 H 0.8498 0.1643 0.7495 0.053 Uiso 1 1 calc . . . C16 C 0.8188(2) 0.0826(7) 0.6852(4) 0.042(2) Uani 1 1 d . . . H16 H 0.8430 0.0634 0.6711 0.050 Uiso 1 1 calc . . . C17 C 0.4545(2) 0.8008(9) 0.9474(3) 0.041(2) Uani 1 1 d . . . C18 C 0.4575(2) 0.6543(8) 0.9578(4) 0.046(2) Uani 1 1 d . . . C19 C 0.4693(3) 0.7088(13) 1.0433(4) 0.063(3) Uani 1 1 d . . . H19 H 0.4745 0.6812 1.0780 0.075 Uiso 1 1 calc . . . C20 C 0.4665(3) 0.8493(11) 1.0318(4) 0.063(3) Uani 1 1 d . . . H20 H 0.4703 0.9145 1.0590 0.076 Uiso 1 1 calc . . . C21 C 0.4308(2) 0.6861(9) 0.7196(4) 0.044(2) Uani 1 1 d . . . C22 C 0.4334(2) 0.5379(9) 0.7304(4) 0.054(3) Uani 1 1 d . . . C23 C 0.4213(3) 0.4960(14) 0.6444(5) 0.076(3) Uani 1 1 d . . . H23 H 0.4176 0.4336 0.6163 0.092 Uiso 1 1 calc . . . C24 C 0.4198(3) 0.6398(14) 0.6354(4) 0.073(3) Uani 1 1 d . . . H24 H 0.4153 0.6711 0.6011 0.087 Uiso 1 1 calc . . . C25 C 0.6546(2) 0.8254(6) 0.3865(3) 0.0211(16) Uani 1 1 d . . . C26 C 0.5787(2) 0.7494(7) 0.3758(3) 0.0278(17) Uani 1 1 d . . . C27 C 0.5397(2) 0.6916(8) 0.3685(3) 0.0356(19) Uani 1 1 d . . . H27 H 0.5337 0.5949 0.3647 0.043 Uiso 1 1 calc . . . C28 C 0.5395(2) 0.9521(7) 0.3752(3) 0.036(2) Uani 1 1 d . . . H28 H 0.5334 1.0487 0.3762 0.043 Uiso 1 1 calc . . . C29 C 0.5785(2) 0.8980(7) 0.3801(3) 0.0285(17) Uani 1 1 d . . . C30 C 0.6977(2) 0.8266(6) 0.3883(2) 0.0219(16) Uani 1 1 d . . . C31 C 0.7735(2) 0.7561(7) 0.3869(3) 0.0245(17) Uani 1 1 d . . . C32 C 0.8113(2) 0.7021(7) 0.3850(3) 0.0302(18) Uani 1 1 d . . . H32 H 0.8174 0.6056 0.3830 0.036 Uiso 1 1 calc . . . C33 C 0.8110(2) 0.9652(8) 0.3897(3) 0.0346(19) Uani 1 1 d . . . H33 H 0.8166 1.0624 0.3911 0.042 Uiso 1 1 calc . . . C34 C 0.7731(2) 0.9070(6) 0.3900(3) 0.0249(17) Uani 1 1 d . . . C35 C 0.6654(2) 0.7711(6) 0.5157(3) 0.0263(17) Uani 1 1 d . . . C36 C 0.5895(2) 0.6982(7) 0.5096(3) 0.0296(17) Uani 1 1 d . . . C37 C 0.5496(2) 0.6444(8) 0.5052(3) 0.0388(19) Uani 1 1 d . . . H37 H 0.5426 0.5489 0.4998 0.047 Uiso 1 1 calc . . . C38 C 0.5522(3) 0.9025(8) 0.5190(3) 0.042(2) Uani 1 1 d . . . H38 H 0.5470 0.9986 0.5238 0.050 Uiso 1 1 calc . . . C39 C 0.5899(2) 0.8469(7) 0.5173(3) 0.0285(18) Uani 1 1 d . . . C40 C 0.7080(2) 0.7705(6) 0.5184(3) 0.0250(16) Uani 1 1 d . . . C41 C 0.7838(2) 0.6890(7) 0.5210(3) 0.0306(17) Uani 1 1 d . . . C42 C 0.8219(2) 0.6315(7) 0.5213(3) 0.039(2) Uani 1 1 d . . . H42 H 0.8271 0.5349 0.5178 0.046 Uiso 1 1 calc . . . C43 C 0.8240(2) 0.8918(7) 0.5328(3) 0.0345(19) Uani 1 1 d . . . H43 H 0.8309 0.9875 0.5379 0.041 Uiso 1 1 calc . . . C44 C 0.7847(2) 0.8388(7) 0.5273(3) 0.0295(19) Uani 1 1 d . . . C45 C 0.6792(2) 0.5658(6) 0.6387(3) 0.0263(17) Uani 1 1 d . . . C46 C 0.6033(2) 0.4849(7) 0.6309(3) 0.0278(17) Uani 1 1 d . . . C47 C 0.5648(2) 0.4232(7) 0.6272(3) 0.039(2) Uani 1 1 d . . . H47 H 0.5594 0.3267 0.6216 0.046 Uiso 1 1 calc . . . C48 C 0.5637(2) 0.6798(7) 0.6426(3) 0.0334(19) Uani 1 1 d . . . H48 H 0.5573 0.7745 0.6482 0.040 Uiso 1 1 calc . . . C49 C 0.6025(2) 0.6315(7) 0.6403(3) 0.0244(17) Uani 1 1 d . . . C50 C 0.7214(2) 0.5700(6) 0.6418(3) 0.0251(17) Uani 1 1 d . . . C51 C 0.7980(2) 0.4946(7) 0.6443(3) 0.0306(18) Uani 1 1 d . . . C52 C 0.8369(2) 0.4392(8) 0.6450(3) 0.0373(19) Uani 1 1 d . . . H52 H 0.8424 0.3437 0.6395 0.045 Uiso 1 1 calc . . . C53 C 0.8379(2) 0.6974(7) 0.6594(3) 0.0367(19) Uani 1 1 d . . . H53 H 0.8443 0.7934 0.6648 0.044 Uiso 1 1 calc . . . C54 C 0.7983(2) 0.6426(7) 0.6523(3) 0.0291(18) Uani 1 1 d . . . C55 C 0.6890(2) 0.6635(6) 0.7754(3) 0.0230(17) Uani 1 1 d . . . C56 C 0.6129(2) 0.5889(6) 0.7725(3) 0.0231(17) Uani 1 1 d . . . C57 C 0.5745(2) 0.5338(7) 0.7716(3) 0.0294(18) Uani 1 1 d . . . H57 H 0.5682 0.4372 0.7690 0.035 Uiso 1 1 calc . . . C58 C 0.5753(2) 0.7943(7) 0.7791(3) 0.0328(18) Uani 1 1 d . . . H58 H 0.5698 0.8909 0.7820 0.039 Uiso 1 1 calc . . . C59 C 0.6134(2) 0.7390(7) 0.7770(3) 0.0289(18) Uani 1 1 d . . . C60 C 0.7310(2) 0.6631(6) 0.7782(3) 0.0251(17) Uani 1 1 d . . . C61 C 0.8077(2) 0.5865(7) 0.7845(3) 0.0271(18) Uani 1 1 d . . . C62 C 0.8462(2) 0.5299(7) 0.7878(3) 0.0328(19) Uani 1 1 d . . . H62 H 0.8518 0.4331 0.7857 0.039 Uiso 1 1 calc . . . C63 C 0.8473(2) 0.7911(7) 0.7948(3) 0.0338(19) Uani 1 1 d . . . H63 H 0.8535 0.8878 0.7976 0.041 Uiso 1 1 calc . . . C64 C 0.8079(2) 0.7353(7) 0.7887(3) 0.0284(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 0.0231(5) 0.0226(4) 0.0298(5) -0.0006(4) 0.0049(4) -0.0003(4) Cu2 0.0232(5) 0.0243(4) 0.0278(5) -0.0021(4) 0.0045(4) 0.0001(4) Cu3 0.0216(4) 0.0319(4) 0.0570(7) 0.0056(4) 0.0032(4) -0.0005(4) S1 0.0220(11) 0.0235(9) 0.0299(11) -0.0005(8) 0.0034(9) -0.0011(7) S2 0.0195(12) 0.0474(12) 0.0543(15) 0.0011(10) 0.0104(10) 0.0004(8) S3 0.0235(11) 0.0241(9) 0.0411(12) -0.0039(8) 0.0038(9) 0.0014(8) S4 0.0229(11) 0.0225(9) 0.0322(11) -0.0005(8) 0.0049(9) 0.0015(7) S5 0.0236(12) 0.0410(11) 0.0506(14) -0.0001(9) 0.0075(10) -0.0014(8) S6 0.0263(11) 0.0212(9) 0.0426(13) -0.0039(8) 0.0070(9) -0.0003(8) S7 0.0302(11) 0.0255(9) 0.0384(12) -0.0022(8) 0.0070(9) -0.0047(8) S8 0.0253(12) 0.0588(13) 0.0655(16) 0.0006(11) 0.0090(11) -0.0063(9) S9 0.0252(11) 0.0242(9) 0.0399(12) -0.0014(8) 0.0078(9) -0.0013(8) S10 0.0334(11) 0.0231(9) 0.0382(12) -0.0041(8) 0.0078(9) 0.0008(8) S11 0.0273(12) 0.0456(12) 0.0567(15) -0.0009(10) 0.0044(10) 0.0042(9) S12 0.0253(11) 0.0235(9) 0.0416(12) -0.0024(8) 0.0030(9) -0.0007(8) S13 0.0265(11) 0.0242(9) 0.0495(13) 0.0019(8) 0.0088(9) 0.0018(7) S14 0.0246(12) 0.0437(11) 0.0640(16) 0.0018(10) 0.0045(10) -0.0038(9) S15 0.0230(11) 0.0258(9) 0.0318(11) -0.0018(8) 0.0054(8) -0.0001(8) S16 0.0303(11) 0.0250(10) 0.0525(13) 0.0001(9) 0.0079(10) 0.0040(8) S17 0.0268(12) 0.0540(13) 0.0578(15) 0.0031(10) 0.0076(10) 0.0047(9) S18 0.0268(11) 0.0265(10) 0.0344(11) -0.0002(8) 0.0057(9) 0.0023(8) S19 0.0216(10) 0.0232(9) 0.0353(11) 0.0004(8) 0.0065(8) 0.0006(7) S20 0.0224(12) 0.0405(11) 0.0554(15) 0.0020(9) 0.0100(10) 0.0034(8) S21 0.0243(11) 0.0237(9) 0.0361(12) 0.0016(8) 0.0066(9) 0.0024(8) S22 0.0243(11) 0.0220(9) 0.0368(12) -0.0015(8) 0.0061(9) -0.0014(7) S23 0.0244(12) 0.0439(12) 0.0543(15) 0.0005(10) 0.0066(10) -0.0019(9) S24 0.0259(12) 0.0233(9) 0.0428(12) 0.0030(8) 0.0064(9) -0.0014(8) S25 0.0261(12) 0.0391(11) 0.0278(11) 0.0022(8) 0.0028(9) 0.0008(8) S26 0.0239(11) 0.0378(10) 0.0299(11) 0.0059(8) 0.0038(8) 0.0017(8) S27 0.0273(12) 0.0453(12) 0.0305(12) 0.0067(9) 0.0086(9) 0.0023(9) S28 0.0273(11) 0.0401(11) 0.0323(12) 0.0078(9) 0.0054(9) -0.0014(8) S29 0.0243(11) 0.0429(11) 0.0316(12) -0.0102(9) 0.0044(9) 0.0004(9) S30 0.0251(12) 0.0434(11) 0.0322(12) -0.0112(9) 0.0048(9) -0.0028(9) S31 0.0277(11) 0.0346(9) 0.0326(11) -0.0069(8) 0.0072(9) -0.0005(8) S32 0.0236(11) 0.0374(10) 0.0306(12) -0.0068(8) 0.0047(9) -0.0021(8) S33 0.0473(14) 0.0331(11) 0.0490(14) 0.0075(10) 0.0031(11) -0.0070(9) S34 0.0370(12) 0.0388(11) 0.0739(17) 0.0197(11) 0.0094(11) 0.0064(9) S35 0.0394(13) 0.0396(11) 0.0497(14) 0.0023(10) 0.0077(10) 0.0089(10) S36 0.0408(13) 0.0361(11) 0.0773(17) -0.0045(11) 0.0049(11) -0.0050(9) N1 0.024(4) 0.038(4) 0.044(4) -0.006(3) 0.006(4) -0.001(3) N2 0.027(4) 0.032(4) 0.064(5) 0.009(3) 0.012(4) 0.002(3) N3 0.023(4) 0.062(5) 0.041(4) 0.001(3) 0.013(4) -0.006(3) N4 0.019(4) 0.076(5) 0.055(5) 0.023(4) 0.008(4) 0.005(3) N5 0.031(4) 0.059(4) 0.045(4) -0.011(3) 0.008(4) 0.000(3) N6 0.036(5) 0.048(4) 0.041(4) -0.012(3) 0.006(4) -0.005(3) N7 0.026(4) 0.036(4) 0.054(5) -0.006(3) 0.014(4) 0.003(3) N8 0.029(4) 0.045(4) 0.052(5) -0.007(3) 0.006(4) 0.002(3) N9 0.048(5) 0.079(5) 0.041(5) 0.005(4) -0.002(4) -0.005(4) N10 0.023(4) 0.086(5) 0.061(6) 0.030(5) 0.009(4) 0.014(4) N11 0.038(5) 0.097(6) 0.050(6) -0.008(5) 0.003(4) 0.013(4) N12 0.033(4) 0.082(6) 0.087(7) -0.048(5) 0.017(4) -0.006(4) C1 0.017(4) 0.024(4) 0.033(5) 0.000(3) 0.000(3) 0.002(3) C2 0.025(5) 0.016(3) 0.041(5) -0.004(3) -0.001(4) -0.001(3) C3 0.023(5) 0.035(4) 0.080(7) 0.016(4) 0.022(5) 0.004(3) C4 0.028(5) 0.041(5) 0.069(7) 0.000(4) -0.005(5) 0.004(4) C5 0.030(5) 0.018(3) 0.029(5) -0.003(3) 0.004(4) -0.001(3) C6 0.029(5) 0.020(4) 0.043(5) -0.004(3) 0.008(4) -0.004(3) C7 0.030(6) 0.084(7) 0.065(7) 0.024(5) 0.002(5) 0.013(5) C8 0.025(6) 0.067(6) 0.067(7) 0.015(5) 0.009(5) -0.007(4) C9 0.012(4) 0.030(4) 0.037(5) 0.002(3) 0.004(3) 0.000(3) C10 0.018(4) 0.022(4) 0.031(5) -0.002(3) 0.007(4) 0.005(3) C11 0.038(6) 0.073(6) 0.051(6) -0.003(5) 0.023(5) 0.006(5) C12 0.019(5) 0.084(7) 0.071(7) -0.014(5) 0.007(5) -0.006(4) C13 0.024(5) 0.024(4) 0.041(5) 0.001(3) 0.005(4) -0.004(3) C14 0.016(4) 0.015(3) 0.046(5) 0.007(3) 0.004(4) -0.001(3) C15 0.023(5) 0.043(5) 0.063(7) -0.004(4) -0.002(5) -0.001(4) C16 0.023(5) 0.033(4) 0.071(7) -0.004(4) 0.014(5) -0.001(3) C17 0.026(4) 0.058(5) 0.036(5) 0.014(4) -0.002(4) -0.013(4) C18 0.017(5) 0.063(6) 0.056(6) 0.019(4) 0.004(4) 0.003(4) C19 0.028(5) 0.123(9) 0.037(6) 0.015(6) 0.004(4) 0.000(5) C20 0.042(6) 0.073(7) 0.071(8) 0.002(5) 0.000(5) -0.004(5) C21 0.015(4) 0.057(6) 0.059(6) -0.004(5) 0.001(4) 0.004(4) C22 0.009(4) 0.066(6) 0.083(7) -0.018(5) -0.002(4) 0.003(4) C23 0.028(6) 0.124(10) 0.078(9) -0.047(8) 0.010(5) 0.010(6) C24 0.039(6) 0.135(11) 0.046(7) -0.015(7) 0.009(5) 0.011(6) C25 0.023(5) 0.022(3) 0.019(4) 0.002(3) 0.007(3) 0.002(3) C26 0.023(4) 0.034(4) 0.027(4) 0.003(3) 0.005(3) -0.002(3) C27 0.033(5) 0.033(4) 0.040(5) 0.002(4) 0.003(4) 0.002(4) C28 0.038(5) 0.023(4) 0.048(5) -0.003(3) 0.012(4) 0.004(3) C29 0.025(5) 0.032(4) 0.029(4) 0.000(3) 0.004(3) -0.001(3) C30 0.027(5) 0.026(4) 0.012(4) -0.001(3) 0.002(3) -0.002(3) C31 0.017(4) 0.032(4) 0.025(4) -0.002(3) 0.006(3) -0.004(3) C32 0.026(5) 0.027(4) 0.038(5) 0.007(3) 0.008(4) -0.004(3) C33 0.028(5) 0.037(4) 0.040(5) -0.002(4) 0.009(4) 0.000(4) C34 0.021(4) 0.024(4) 0.031(5) -0.006(3) 0.009(3) -0.003(3) C35 0.031(5) 0.024(4) 0.024(4) -0.003(3) 0.004(3) 0.000(3) C36 0.027(4) 0.034(4) 0.027(4) 0.002(3) 0.004(3) -0.003(3) C37 0.037(5) 0.042(5) 0.039(5) -0.002(4) 0.011(4) -0.009(4) C38 0.035(5) 0.038(4) 0.052(6) 0.012(4) 0.006(4) -0.004(4) C39 0.026(5) 0.033(4) 0.026(4) -0.004(3) 0.002(3) -0.007(3) C40 0.032(5) 0.024(4) 0.019(4) 0.001(3) 0.003(3) 0.003(3) C41 0.033(5) 0.029(4) 0.029(4) -0.007(3) 0.004(3) 0.000(3) C42 0.039(5) 0.028(4) 0.049(5) 0.002(4) 0.006(4) 0.005(4) C43 0.031(5) 0.021(4) 0.049(5) 0.004(4) 0.001(4) 0.003(3) C44 0.027(5) 0.028(4) 0.032(5) -0.001(3) 0.000(4) 0.002(3) C45 0.031(5) 0.025(4) 0.022(4) 0.001(3) 0.000(3) -0.005(3) C46 0.017(4) 0.036(4) 0.028(4) 0.011(3) -0.003(3) 0.005(3) C47 0.039(5) 0.024(4) 0.054(5) 0.007(3) 0.012(4) 0.001(3) C48 0.030(5) 0.030(4) 0.040(5) -0.003(3) 0.004(4) -0.005(3) C49 0.023(5) 0.024(4) 0.027(4) 0.003(3) 0.005(3) 0.001(3) C50 0.024(5) 0.021(3) 0.030(4) -0.001(3) 0.005(3) -0.002(3) C51 0.034(5) 0.033(4) 0.027(4) 0.011(3) 0.009(3) 0.007(3) C52 0.029(5) 0.040(4) 0.042(5) 0.004(4) 0.003(4) 0.008(3) C53 0.027(5) 0.029(4) 0.052(5) -0.005(4) 0.003(4) 0.003(3) C54 0.030(5) 0.030(4) 0.030(5) 0.000(3) 0.013(4) 0.006(3) C55 0.023(5) 0.014(3) 0.032(4) 0.000(3) 0.003(3) -0.001(3) C56 0.026(5) 0.023(4) 0.021(4) -0.001(3) 0.008(3) 0.001(3) C57 0.028(5) 0.026(4) 0.034(5) 0.006(3) 0.003(4) 0.007(3) C58 0.032(5) 0.026(4) 0.039(5) 0.000(3) 0.003(4) 0.002(4) C59 0.021(5) 0.036(4) 0.029(5) 0.004(3) 0.004(3) -0.003(3) C60 0.031(5) 0.019(4) 0.023(4) -0.001(3) 0.000(3) -0.003(3) C61 0.032(5) 0.025(4) 0.024(4) -0.002(3) 0.004(3) -0.005(3) C62 0.021(4) 0.026(4) 0.052(5) 0.007(3) 0.009(4) 0.003(3) C63 0.024(5) 0.033(4) 0.044(5) -0.005(4) 0.004(4) -0.007(3) C64 0.025(5) 0.033(4) 0.028(4) 0.005(3) 0.005(4) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S25 2.180(2) . ? Cu1 S26 2.181(2) . ? Cu1 S27 2.181(2) . ? Cu1 S28 2.188(2) . ? Cu2 S32 2.179(2) . ? Cu2 S30 2.183(2) . ? Cu2 S31 2.187(2) . ? Cu2 S29 2.197(2) . ? Cu3 S36 2.175(2) . ? Cu3 S35 2.180(2) . ? Cu3 S33 2.180(2) . ? Cu3 S34 2.191(2) . ? S1 C25 1.734(6) . ? S1 C26 1.745(7) . ? S2 C28 1.691(8) . ? S2 C27 1.710(8) . ? S3 C25 1.717(6) . ? S3 C29 1.744(7) . ? S4 C30 1.730(7) . ? S4 C31 1.741(7) . ? S5 C33 1.709(8) . ? S5 C32 1.721(7) . ? S6 C30 1.729(6) . ? S6 C34 1.743(7) . ? S7 C36 1.722(7) . ? S7 C35 1.725(7) . ? S8 C37 1.694(8) . ? S8 C38 1.701(8) . ? S9 C35 1.732(7) . ? S9 C39 1.746(7) . ? S10 C41 1.730(7) . ? S10 C40 1.739(6) . ? S11 C42 1.709(7) . ? S11 C43 1.711(7) . ? S12 C44 1.734(8) . ? S12 C40 1.734(7) . ? S13 C45 1.746(6) . ? S13 C46 1.749(7) . ? S14 C48 1.702(7) . ? S14 C47 1.704(7) . ? S15 C49 1.749(7) . ? S15 C45 1.752(7) . ? S16 C51 1.738(7) . ? S16 C50 1.763(6) . ? S17 C52 1.704(8) . ? S17 C53 1.708(7) . ? S18 C54 1.737(7) . ? S18 C50 1.741(6) . ? S19 C56 1.735(7) . ? S19 C55 1.749(6) . ? S20 C58 1.705(8) . ? S20 C57 1.720(7) . ? S21 C59 1.741(7) . ? S21 C55 1.746(6) . ? S22 C61 1.744(7) . ? S22 C60 1.753(7) . ? S23 C63 1.708(7) . ? S23 C62 1.716(7) . ? S24 C60 1.739(6) . ? S24 C64 1.742(7) . ? S25 C1 1.738(8) . ? S26 C2 1.751(7) . ? S27 C5 1.734(8) . ? S28 C6 1.756(8) . ? S29 C9 1.754(7) . ? S30 C10 1.732(7) . ? S31 C13 1.734(8) . ? S32 C14 1.731(7) . ? S33 C17 1.749(8) . ? S34 C18 1.742(9) . ? S35 C21 1.753(9) . ? S36 C22 1.729(10) . ? N1 C1 1.334(9) . ? N1 C4 1.356(11) . ? N2 C2 1.326(9) . ? N2 C3 1.345(11) . ? N3 C8 1.332(11) . ? N3 C5 1.341(9) . ? N4 C7 1.321(11) . ? N4 C6 1.333(9) . ? N5 C9 1.326(9) . ? N5 C12 1.362(10) . ? N6 C10 1.337(9) . ? N6 C11 1.339(11) . ? N7 C13 1.346(9) . ? N7 C16 1.358(10) . ? N8 C14 1.330(9) . ? N8 C15 1.353(10) . ? N9 C20 1.310(12) . ? N9 C17 1.333(10) . ? N10 C18 1.337(11) . ? N10 C19 1.369(12) . ? N11 C21 1.310(11) . ? N11 C24 1.343(13) . ? N12 C22 1.328(10) . ? N12 C23 1.355(14) . ? C1 C2 1.385(10) . ? C3 C4 1.365(12) . ? C5 C6 1.415(10) . ? C7 C8 1.364(12) . ? C9 C10 1.380(10) . ? C11 C12 1.356(12) . ? C13 C14 1.403(10) . ? C15 C16 1.355(11) . ? C17 C18 1.418(11) . ? C19 C20 1.368(14) . ? C21 C22 1.435(12) . ? C23 C24 1.385(15) . ? C25 C30 1.395(9) . ? C26 C27 1.368(10) . ? C26 C29 1.415(9) . ? C28 C29 1.355(10) . ? C31 C32 1.343(9) . ? C31 C34 1.435(9) . ? C33 C34 1.351(10) . ? C35 C40 1.374(10) . ? C36 C37 1.383(10) . ? C36 C39 1.426(9) . ? C38 C39 1.343(11) . ? C41 C42 1.353(10) . ? C41 C44 1.431(9) . ? C43 C44 1.362(10) . ? C45 C50 1.361(9) . ? C46 C47 1.372(10) . ? C46 C49 1.414(10) . ? C48 C49 1.353(10) . ? C51 C52 1.366(9) . ? C51 C54 1.421(9) . ? C53 C54 1.372(10) . ? C55 C60 1.355(9) . ? C56 C57 1.350(10) . ? C56 C59 1.430(9) . ? C58 C59 1.357(10) . ? C61 C62 1.352(10) . ? C61 C64 1.416(9) . ? C63 C64 1.373(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 S25 Cu1 S26 92.08(8) . . ? S25 Cu1 S27 86.54(8) . . ? S26 Cu1 S27 177.27(8) . . ? S25 Cu1 S28 178.47(9) . . ? S26 Cu1 S28 88.77(8) . . ? S27 Cu1 S28 92.66(8) . . ? S32 Cu2 S30 86.79(8) . . ? S32 Cu2 S31 91.92(8) . . ? S30 Cu2 S31 178.65(9) . . ? S32 Cu2 S29 178.46(9) . . ? S30 Cu2 S29 92.53(8) . . ? S31 Cu2 S29 88.77(8) . . ? S36 Cu3 S35 93.07(9) . . ? S36 Cu3 S33 178.83(11) . . ? S35 Cu3 S33 86.67(9) . . ? S36 Cu3 S34 87.51(10) . . ? S35 Cu3 S34 178.81(11) . . ? S33 Cu3 S34 92.76(9) . . ? C25 S1 C26 94.0(3) . . ? C28 S2 C27 93.6(4) . . ? C25 S3 C29 94.9(3) . . ? C30 S4 C31 95.0(3) . . ? C33 S5 C32 93.6(4) . . ? C30 S6 C34 95.2(3) . . ? C36 S7 C35 95.2(3) . . ? C37 S8 C38 93.7(4) . . ? C35 S9 C39 95.1(3) . . ? C41 S10 C40 95.9(3) . . ? C42 S11 C43 93.4(4) . . ? C44 S12 C40 94.8(3) . . ? C45 S13 C46 94.4(3) . . ? C48 S14 C47 93.0(4) . . ? C49 S15 C45 94.9(3) . . ? C51 S16 C50 95.2(3) . . ? C52 S17 C53 93.2(4) . . ? C54 S18 C50 95.2(3) . . ? C56 S19 C55 94.9(3) . . ? C58 S20 C57 92.8(4) . . ? C59 S21 C55 94.9(3) . . ? C61 S22 C60 95.0(3) . . ? C63 S23 C62 93.1(4) . . ? C60 S24 C64 95.0(3) . . ? C1 S25 Cu1 103.7(3) . . ? C2 S26 Cu1 103.8(3) . . ? C5 S27 Cu1 103.9(3) . . ? C6 S28 Cu1 103.2(3) . . ? C9 S29 Cu2 102.7(3) . . ? C10 S30 Cu2 103.1(3) . . ? C13 S31 Cu2 104.0(3) . . ? C14 S32 Cu2 104.0(3) . . ? C17 S33 Cu3 103.5(3) . . ? C18 S34 Cu3 103.6(3) . . ? C21 S35 Cu3 103.7(3) . . ? C22 S36 Cu3 103.7(3) . . ? C1 N1 C4 115.6(7) . . ? C2 N2 C3 115.2(7) . . ? C8 N3 C5 115.5(7) . . ? C7 N4 C6 114.5(7) . . ? C9 N5 C12 115.3(7) . . ? C10 N6 C11 116.0(7) . . ? C13 N7 C16 114.5(7) . . ? C14 N8 C15 115.8(7) . . ? C20 N9 C17 116.3(8) . . ? C18 N10 C19 115.3(8) . . ? C21 N11 C24 114.9(9) . . ? C22 N12 C23 116.1(9) . . ? N1 C1 C2 122.0(7) . . ? N1 C1 S25 117.3(6) . . ? C2 C1 S25 120.6(6) . . ? N2 C2 C1 122.6(7) . . ? N2 C2 S26 117.8(6) . . ? C1 C2 S26 119.5(6) . . ? N2 C3 C4 123.0(7) . . ? N1 C4 C3 121.6(7) . . ? N3 C5 C6 121.2(7) . . ? N3 C5 S27 118.5(6) . . ? C6 C5 S27 120.3(6) . . ? N4 C6 C5 122.1(7) . . ? N4 C6 S28 118.4(6) . . ? C5 C6 S28 119.5(6) . . ? N4 C7 C8 124.4(8) . . ? N3 C8 C7 122.1(8) . . ? N5 C9 C10 122.8(6) . . ? N5 C9 S29 117.3(6) . . ? C10 C9 S29 120.0(5) . . ? N6 C10 C9 121.4(7) . . ? N6 C10 S30 117.1(6) . . ? C9 C10 S30 121.5(5) . . ? N6 C11 C12 122.5(8) . . ? C11 C12 N5 121.8(8) . . ? N7 C13 C14 122.2(7) . . ? N7 C13 S31 118.2(6) . . ? C14 C13 S31 119.7(6) . . ? N8 C14 C13 121.9(7) . . ? N8 C14 S32 117.7(6) . . ? C13 C14 S32 120.4(6) . . ? N8 C15 C16 122.3(7) . . ? C15 C16 N7 123.2(7) . . ? N9 C17 C18 122.4(7) . . ? N9 C17 S33 117.4(6) . . ? C18 C17 S33 120.2(7) . . ? N10 C18 C17 120.7(8) . . ? N10 C18 S34 119.4(7) . . ? C17 C18 S34 119.8(7) . . ? C20 C19 N10 122.3(9) . . ? N9 C20 C19 123.0(9) . . ? N11 C21 C22 122.9(8) . . ? N11 C21 S35 118.2(7) . . ? C22 C21 S35 118.8(7) . . ? N12 C22 C21 121.1(9) . . ? N12 C22 S36 118.2(8) . . ? C21 C22 S36 120.6(7) . . ? N12 C23 C24 121.2(9) . . ? N11 C24 C23 123.7(10) . . ? C30 C25 S3 121.2(5) . . ? C30 C25 S1 120.5(5) . . ? S3 C25 S1 118.3(4) . . ? C27 C26 C29 113.3(6) . . ? C27 C26 S1 129.8(5) . . ? C29 C26 S1 116.8(5) . . ? C26 C27 S2 109.5(5) . . ? C29 C28 S2 111.0(5) . . ? C28 C29 C26 112.7(6) . . ? C28 C29 S3 131.5(6) . . ? C26 C29 S3 115.9(5) . . ? C25 C30 S6 120.7(5) . . ? C25 C30 S4 121.6(5) . . ? S6 C30 S4 117.7(4) . . ? C32 C31 C34 113.4(6) . . ? C32 C31 S4 130.4(5) . . ? C34 C31 S4 116.2(5) . . ? C31 C32 S5 109.8(5) . . ? C34 C33 S5 110.0(5) . . ? C33 C34 C31 113.2(6) . . ? C33 C34 S6 131.1(5) . . ? C31 C34 S6 115.7(5) . . ? C40 C35 S7 121.7(5) . . ? C40 C35 S9 121.0(5) . . ? S7 C35 S9 117.4(4) . . ? C37 C36 C39 111.4(6) . . ? C37 C36 S7 131.6(5) . . ? C39 C36 S7 117.0(5) . . ? C36 C37 S8 110.5(5) . . ? C39 C38 S8 110.4(6) . . ? C38 C39 C36 114.0(6) . . ? C38 C39 S9 130.8(6) . . ? C36 C39 S9 115.2(5) . . ? C35 C40 S12 122.3(5) . . ? C35 C40 S10 120.8(5) . . ? S12 C40 S10 116.9(4) . . ? C42 C41 C44 113.5(6) . . ? C42 C41 S10 131.4(5) . . ? C44 C41 S10 115.1(5) . . ? C41 C42 S11 110.3(5) . . ? C44 C43 S11 110.5(5) . . ? C43 C44 C41 112.4(6) . . ? C43 C44 S12 130.3(5) . . ? C41 C44 S12 117.3(5) . . ? C50 C45 S13 121.4(5) . . ? C50 C45 S15 121.4(5) . . ? S13 C45 S15 117.2(4) . . ? C47 C46 C49 113.0(6) . . ? C47 C46 S13 129.5(6) . . ? C49 C46 S13 117.4(5) . . ? C46 C47 S14 110.1(5) . . ? C49 C48 S14 111.2(5) . . ? C48 C49 C46 112.6(6) . . ? C48 C49 S15 131.4(5) . . ? C46 C49 S15 115.9(5) . . ? C45 C50 S18 123.5(5) . . ? C45 C50 S16 120.1(5) . . ? S18 C50 S16 116.3(4) . . ? C52 C51 C54 113.2(6) . . ? C52 C51 S16 130.7(6) . . ? C54 C51 S16 116.1(5) . . ? C51 C52 S17 110.6(5) . . ? C54 C53 S17 110.7(5) . . ? C53 C54 C51 112.3(6) . . ? C53 C54 S18 130.6(5) . . ? C51 C54 S18 117.1(5) . . ? C60 C55 S21 121.3(5) . . ? C60 C55 S19 121.7(5) . . ? S21 C55 S19 117.0(4) . . ? C57 C56 C59 112.7(6) . . ? C57 C56 S19 130.7(5) . . ? C59 C56 S19 116.6(5) . . ? C56 C57 S20 110.7(5) . . ? C59 C58 S20 110.9(5) . . ? C58 C59 C56 112.9(6) . . ? C58 C59 S21 130.8(5) . . ? C56 C59 S21 116.3(5) . . ? C55 C60 S24 121.7(5) . . ? C55 C60 S22 121.6(5) . . ? S24 C60 S22 116.7(4) . . ? C62 C61 C64 113.5(6) . . ? C62 C61 S22 130.4(5) . . ? C64 C61 S22 116.1(5) . . ? C61 C62 S23 110.4(5) . . ? C64 C63 S23 110.2(5) . . ? C63 C64 C61 112.7(6) . . ? C63 C64 S24 130.3(5) . . ? C61 C64 S24 116.9(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.17 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.334 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.081 data_x57 _database_code_depnum_ccdc_archive 'CCDC 259177' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H8 Cu N4 S10' _chemical_formula_weight 664.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.8136(4) _cell_length_b 10.5663(3) _cell_length_c 18.58310(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.834(2) _cell_angle_gamma 90.00 _cell_volume 2270.35(10) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 14388 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 24.0 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 1.901 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD' _diffrn_measurement_method 'phi and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10317 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 23.00 _reflns_number_total 3143 _reflns_number_gt 2568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0492P)^2^+11.7582P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3143 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 0.54753(6) 0.13050(7) 0.57475(4) 0.0256(3) Uani 1 1 d . . . S1 S 0.49362(14) 0.04641(16) 0.66999(10) 0.0290(4) Uani 1 1 d . . . S2 S 0.69581(15) 0.00469(17) 0.58546(10) 0.0338(5) Uani 1 1 d . . . S3 S 0.40305(15) 0.26193(16) 0.56546(10) 0.0307(4) Uani 1 1 d . . . S4 S 0.60492(15) 0.21349(18) 0.48096(10) 0.0363(5) Uani 1 1 d . . . S5 S 0.21578(14) -0.00115(16) 0.58405(9) 0.0271(4) Uani 1 1 d . . . S6 S 0.23461(16) -0.26314(17) 0.75931(10) 0.0359(5) Uani 1 1 d . . . S7 S 0.00637(15) 0.01544(17) 0.64736(10) 0.0341(5) Uani 1 1 d . . . S8 S 0.11756(14) 0.21800(17) 0.47035(10) 0.0304(4) Uani 1 1 d . . . S9 S -0.10141(17) 0.51234(18) 0.36784(11) 0.0405(5) Uani 1 1 d . . . S10 S -0.09252(14) 0.23356(16) 0.53305(10) 0.0296(4) Uani 1 1 d . . . N1 N 0.5878(5) -0.1395(5) 0.7573(3) 0.0330(14) Uani 1 1 d . . . N2 N 0.7693(5) -0.1762(6) 0.6818(3) 0.0390(15) Uani 1 1 d . . . N3 N 0.3278(5) 0.4325(6) 0.4621(3) 0.0385(15) Uani 1 1 d . . . N4 N 0.5025(5) 0.3806(6) 0.3843(3) 0.0369(15) Uani 1 1 d . . . C1 C 0.5970(5) -0.0709(6) 0.6994(3) 0.0257(15) Uani 1 1 d . . . C2 C 0.6879(5) -0.0892(6) 0.6613(4) 0.0262(15) Uani 1 1 d . . . C3 C 0.7590(7) -0.2457(6) 0.7407(4) 0.0381(19) Uani 1 1 d . . . H3 H 0.8148 -0.3081 0.7577 0.046 Uiso 1 1 calc . . . C4 C 0.6681(7) -0.2283(7) 0.7775(4) 0.0363(18) Uani 1 1 d . . . H4 H 0.6635 -0.2807 0.8177 0.044 Uiso 1 1 calc . . . C5 C 0.4102(6) 0.3469(6) 0.4851(4) 0.0275(16) Uani 1 1 d . . . C6 C 0.4972(6) 0.3208(6) 0.4468(4) 0.0270(16) Uani 1 1 d . . . C7 C 0.4185(7) 0.4678(7) 0.3617(4) 0.0394(19) Uani 1 1 d . . . H7 H 0.4185 0.5126 0.3180 0.047 Uiso 1 1 calc . . . C8 C 0.3334(6) 0.4932(7) 0.4003(4) 0.0380(19) Uani 1 1 d . . . H8 H 0.2777 0.5552 0.3825 0.046 Uiso 1 1 calc . . . C9 C 0.0832(5) 0.0692(6) 0.5835(3) 0.0235(15) Uani 1 1 d . . . C10 C 0.2098(5) -0.1016(6) 0.6576(3) 0.0238(15) Uani 1 1 d . . . C11 C 0.2871(6) -0.1920(7) 0.6904(4) 0.0332(17) Uani 1 1 d . . . H11 H 0.3576 -0.2116 0.6771 0.040 Uiso 1 1 calc . . . C12 C 0.1115(6) -0.1743(7) 0.7446(4) 0.0360(18) Uani 1 1 d . . . H12 H 0.0526 -0.1810 0.7715 0.043 Uiso 1 1 calc . . . C13 C 0.1110(6) -0.0924(6) 0.6883(4) 0.0304(17) Uani 1 1 d . . . C14 C 0.0412(5) 0.1654(6) 0.5345(4) 0.0260(15) Uani 1 1 d . . . C15 C 0.0185(5) 0.3335(6) 0.4336(4) 0.0267(16) Uani 1 1 d . . . C16 C 0.0186(6) 0.4209(7) 0.3800(4) 0.0362(18) Uani 1 1 d . . . H16 H 0.0776 0.4295 0.3532 0.043 Uiso 1 1 calc . . . C17 C -0.1555(6) 0.4358(7) 0.4346(4) 0.0373(18) Uani 1 1 d . . . H17 H -0.2254 0.4562 0.4487 0.045 Uiso 1 1 calc . . . C18 C -0.0829(6) 0.3417(6) 0.4643(4) 0.0285(16) 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 0.0236(4) 0.0261(5) 0.0277(5) -0.0008(4) 0.0067(3) 0.0017(3) S1 0.0251(9) 0.0315(9) 0.0324(10) 0.0012(8) 0.0104(7) 0.0029(7) S2 0.0319(9) 0.0360(10) 0.0375(11) 0.0094(9) 0.0168(8) 0.0118(8) S3 0.0301(9) 0.0314(10) 0.0338(10) 0.0031(8) 0.0137(8) 0.0081(8) S4 0.0352(10) 0.0395(11) 0.0386(11) 0.0075(9) 0.0177(9) 0.0104(8) S5 0.0241(9) 0.0311(9) 0.0275(9) 0.0078(8) 0.0089(7) 0.0032(7) S6 0.0398(11) 0.0338(10) 0.0339(11) 0.0106(8) 0.0069(8) 0.0012(8) S7 0.0320(10) 0.0389(11) 0.0363(11) 0.0113(9) 0.0180(8) 0.0069(8) S8 0.0247(9) 0.0364(10) 0.0326(10) 0.0112(8) 0.0116(8) 0.0052(8) S9 0.0488(12) 0.0304(10) 0.0387(11) 0.0082(9) 0.0005(9) 0.0070(9) S10 0.0264(9) 0.0312(10) 0.0340(10) 0.0040(8) 0.0130(8) 0.0060(7) N1 0.040(3) 0.032(3) 0.027(3) 0.000(3) 0.006(3) -0.002(3) N2 0.036(3) 0.042(4) 0.042(4) 0.011(3) 0.015(3) 0.009(3) N3 0.035(3) 0.036(3) 0.044(4) 0.003(3) 0.007(3) 0.013(3) N4 0.038(3) 0.036(4) 0.039(4) 0.004(3) 0.013(3) 0.001(3) C1 0.029(4) 0.026(4) 0.020(4) -0.006(3) 0.000(3) -0.009(3) C2 0.024(4) 0.027(4) 0.028(4) -0.001(3) 0.007(3) 0.003(3) C3 0.044(5) 0.027(4) 0.040(5) 0.006(4) 0.004(4) 0.011(3) C4 0.045(5) 0.035(4) 0.028(4) 0.005(3) 0.007(4) 0.001(4) C5 0.032(4) 0.021(4) 0.029(4) -0.004(3) 0.005(3) -0.005(3) C6 0.030(4) 0.024(4) 0.028(4) -0.001(3) 0.007(3) -0.005(3) C7 0.045(5) 0.034(4) 0.038(4) 0.007(4) 0.005(4) -0.008(4) C8 0.039(4) 0.024(4) 0.047(5) 0.008(4) -0.002(4) 0.000(3) C9 0.020(3) 0.027(4) 0.026(4) -0.003(3) 0.010(3) -0.002(3) C10 0.022(3) 0.025(4) 0.025(4) 0.000(3) 0.006(3) 0.001(3) C11 0.035(4) 0.033(4) 0.031(4) 0.007(3) 0.005(3) -0.008(3) C12 0.039(4) 0.046(5) 0.026(4) 0.009(4) 0.014(3) 0.002(4) C13 0.038(4) 0.027(4) 0.024(4) 0.000(3) 0.003(3) -0.003(3) C14 0.029(4) 0.021(3) 0.027(4) -0.001(3) 0.003(3) -0.001(3) C15 0.026(4) 0.028(4) 0.027(4) -0.001(3) 0.007(3) 0.001(3) C16 0.037(4) 0.041(4) 0.032(4) 0.006(4) 0.008(3) 0.002(3) C17 0.035(4) 0.038(4) 0.038(4) 0.000(4) 0.006(3) 0.005(3) C18 0.031(4) 0.028(4) 0.026(4) -0.003(3) 0.004(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S2 2.1754(19) . ? Cu1 S3 2.1796(18) . ? Cu1 S4 2.180(2) . ? Cu1 S1 2.1885(19) . ? S1 C1 1.747(7) . ? S2 C2 1.742(7) . ? S3 C5 1.760(7) . ? S4 C6 1.726(7) . ? S5 C9 1.731(6) . ? S5 C10 1.743(7) . ? S6 C12 1.705(7) . ? S6 C11 1.706(7) . ? S7 C9 1.731(7) . ? S7 C13 1.737(7) . ? S8 C14 1.729(7) . ? S8 C15 1.731(7) . ? S9 C16 1.692(7) . ? S9 C17 1.711(8) . ? S10 C14 1.731(7) . ? S10 C18 1.735(7) . ? N1 C1 1.320(9) . ? N1 C4 1.333(9) . ? N2 C2 1.328(8) . ? N2 C3 1.345(9) . ? N3 C8 1.328(9) . ? N3 C5 1.334(8) . ? N4 C6 1.334(9) . ? N4 C7 1.356(9) . ? C1 C2 1.416(9) . ? C3 C4 1.399(11) . ? C5 C6 1.392(9) . ? C7 C8 1.376(11) . ? C9 C14 1.387(9) . ? C10 C11 1.375(9) . ? C10 C13 1.404(10) . ? C12 C13 1.357(10) . ? C15 C16 1.360(10) . ? C15 C18 1.431(9) . ? C17 C18 1.355(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 S2 Cu1 S3 178.01(8) . . ? S2 Cu1 S4 86.69(7) . . ? S3 Cu1 S4 92.71(7) . . ? S2 Cu1 S1 92.31(7) . . ? S3 Cu1 S1 88.27(7) . . ? S4 Cu1 S1 178.82(7) . . ? C1 S1 Cu1 103.9(2) . . ? C2 S2 Cu1 104.3(2) . . ? C5 S3 Cu1 102.7(2) . . ? C6 S4 Cu1 103.4(2) . . ? C9 S5 C10 94.8(3) . . ? C12 S6 C11 93.8(3) . . ? C9 S7 C13 95.1(3) . . ? C14 S8 C15 95.3(3) . . ? C16 S9 C17 93.5(3) . . ? C14 S10 C18 95.1(3) . . ? C1 N1 C4 116.4(6) . . ? C2 N2 C3 115.5(6) . . ? C8 N3 C5 116.2(6) . . ? C6 N4 C7 115.4(6) . . ? N1 C1 C2 122.0(6) . . ? N1 C1 S1 118.4(5) . . ? C2 C1 S1 119.6(5) . . ? N2 C2 C1 122.0(6) . . ? N2 C2 S2 118.1(5) . . ? C1 C2 S2 119.9(5) . . ? N2 C3 C4 122.2(6) . . ? N1 C4 C3 121.9(7) . . ? N3 C5 C6 122.5(6) . . ? N3 C5 S3 117.3(5) . . ? C6 C5 S3 120.1(5) . . ? N4 C6 C5 121.5(6) . . ? N4 C6 S4 117.9(5) . . ? C5 C6 S4 120.5(5) . . ? N4 C7 C8 122.5(7) . . ? N3 C8 C7 121.9(6) . . ? C14 C9 S7 121.5(5) . . ? C14 C9 S5 121.4(5) . . ? S7 C9 S5 117.1(4) . . ? C11 C10 C13 113.5(6) . . ? C11 C10 S5 129.9(5) . . ? C13 C10 S5 116.6(5) . . ? C10 C11 S6 109.2(5) . . ? C13 C12 S6 110.1(5) . . ? C12 C13 C10 113.3(6) . . ? C12 C13 S7 130.3(6) . . ? C10 C13 S7 116.4(5) . . ? C9 C14 S8 121.4(5) . . ? C9 C14 S10 121.2(5) . . ? S8 C14 S10 117.3(4) . . ? C16 C15 C18 112.2(6) . . ? C16 C15 S8 131.7(5) . . ? C18 C15 S8 116.1(5) . . ? C15 C16 S9 111.0(5) . . ? C18 C17 S9 110.0(5) . . ? C17 C18 C15 113.3(6) . . ? C17 C18 S10 130.7(6) . . ? C15 C18 S10 116.1(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.822 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.107