# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1246 data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Cu{H2N(CH2)3N-SO2-Tol}2] _chemical_formula_sum 'C20 H30 Cu N4 O4 S2' _chemical_formula_weight 518.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.019(6) _cell_length_b 24.783(10) _cell_length_c 12.873(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.43(4) _cell_angle_gamma 90.00 _cell_volume 4696(4) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 51 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description lath _exptl_crystal_colour Blue _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 3.260 _exptl_absorpt_correction_type Difabs _exptl_absorpt_correction_T_min 0.085 _exptl_absorpt_correction_T_max 0.540 _exptl_absorpt_process_details ? _exptl_special_details ; Psi-scan data were collected but they were rather noisy. When the data set was corrected for absorption using the psi-data R1 was 7.51% and the max and min were +1.34 and -1.07 e/A^3^. These parameters improved substantially when Difabs was used to correct for absorption (which is quite hefty here). Presumably there is some systematic error in the data which was not corrected using empirical treatments for absorption. Out of 24 reflections located in a random search 3 had non-integral indices with respect to the orientation matrix derived for the other 21 reflections. One might speculate that the systematic error being corrected for by Difabs was related to the presence of a small passenger crystal. ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 8928 _diffrn_reflns_av_R_equivalents 0.2278 _diffrn_reflns_av_sigmaI/netI 0.0972 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 70.17 _reflns_number_total 8543 _reflns_number_gt 3066 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution DIRDIF _computing_structure_refinement SHELXL-97 _computing_molecular_graphics SHELXTL _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^)+(0.0846P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8543 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1678 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1923 _refine_ls_wR_factor_gt 0.1441 _refine_ls_goodness_of_fit_ref 0.857 _refine_ls_restrained_S_all 0.857 _refine_ls_shift/su_max 0.084 _refine_ls_shift/su_mean 0.011 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.62065(12) 0.03460(3) 0.36763(13) 0.0332(3) Uani 1 1 d . . . N1A N 0.5668(6) -0.0236(3) 0.2639(6) 0.042(2) Uani 1 1 d . . . H1A1 H 0.6114 -0.0373 0.2330 0.050 Uiso 1 1 calc R . . H1A2 H 0.5460 -0.0508 0.3002 0.050 Uiso 1 1 calc R . . C2A C 0.4914(7) -0.0045(4) 0.1798(8) 0.052(3) Uani 1 1 d . . . H2A1 H 0.4686 -0.0353 0.1345 0.063 Uiso 1 1 calc R . . H2A2 H 0.4419 0.0077 0.2135 0.063 Uiso 1 1 calc R . . C3A C 0.5125(9) 0.0383(5) 0.1132(8) 0.059(3) Uani 1 1 d . . . H3A1 H 0.4587 0.0441 0.0573 0.071 Uiso 1 1 calc R . . H3A2 H 0.5609 0.0253 0.0786 0.071 Uiso 1 1 calc R . . N5A N 0.6185(5) 0.0866(3) 0.2513(6) 0.0394(19) Uani 1 1 d . . . C4A C 0.5415(7) 0.0925(4) 0.1615(7) 0.050(3) Uani 1 1 d . . . H4A1 H 0.5591 0.1160 0.1077 0.060 Uiso 1 1 calc R . . H4A2 H 0.4904 0.1095 0.1859 0.060 Uiso 1 1 calc R . . S6A S 0.71525(19) 0.10346(10) 0.2366(2) 0.0431(6) Uani 1 1 d . . . O61A O 0.7783(5) 0.0762(3) 0.3196(6) 0.0526(19) Uani 1 1 d . . . O62A O 0.7279(6) 0.0964(3) 0.1287(6) 0.065(2) Uani 1 1 d . . . C7A C 0.7324(7) 0.1740(4) 0.2624(7) 0.040(2) Uani 1 1 d . . . C8A C 0.7652(6) 0.2072(4) 0.1953(7) 0.049(2) Uani 1 1 d . . . H8A H 0.7782 0.1935 0.1318 0.059 Uiso 1 1 calc R . . C9A C 0.7795(6) 0.2605(4) 0.2198(8) 0.061(3) Uani 1 1 d . . . H9A H 0.8018 0.2830 0.1720 0.073 Uiso 1 1 calc R . . C10A C 0.7623(7) 0.2825(4) 0.3124(8) 0.047(3) Uani 1 1 d . . . C11A C 0.7262(6) 0.2478(4) 0.3784(7) 0.050(2) Uani 1 1 d . . . H11A H 0.7118 0.2617 0.4409 0.060 Uiso 1 1 calc R . . C12A C 0.7109(6) 0.1938(3) 0.3556(7) 0.052(2) Uani 1 1 d . . . H12A H 0.6866 0.1711 0.4015 0.062 Uiso 1 1 calc R . . C13A C 0.7780(7) 0.3412(4) 0.3416(8) 0.072(4) Uani 1 1 d . . . H13A H 0.8185 0.3569 0.2998 0.108 Uiso 1 1 calc R . . H13B H 0.8052 0.3441 0.4163 0.108 Uiso 1 1 calc R . . H13C H 0.7205 0.3603 0.3274 0.108 Uiso 1 1 calc R . . N1B N 0.6808(5) -0.0204(3) 0.4737(6) 0.0366(19) Uani 1 1 d . . . H1B1 H 0.6381 -0.0344 0.5074 0.044 Uiso 1 1 calc R . . H1B2 H 0.7015 -0.0479 0.4380 0.044 Uiso 1 1 calc R . . C2B C 0.7573(7) 0.0000(4) 0.5548(7) 0.046(3) Uani 1 1 d . . . H2B1 H 0.8034 0.0157 0.5197 0.055 Uiso 1 1 calc R . . H2B2 H 0.7852 -0.0302 0.5989 0.055 Uiso 1 1 calc R . . C3B C 0.7255(8) 0.0426(4) 0.6254(8) 0.052(3) Uani 1 1 d . . . H3B1 H 0.6744 0.0280 0.6535 0.062 Uiso 1 1 calc R . . H3B2 H 0.7750 0.0501 0.6857 0.062 Uiso 1 1 calc R . . C4B C 0.6968(7) 0.0944(4) 0.5692(7) 0.048(3) Uani 1 1 d . . . H4B1 H 0.6804 0.1204 0.6196 0.057 Uiso 1 1 calc R . . H4B2 H 0.7478 0.1094 0.5415 0.057 Uiso 1 1 calc R . . N5B N 0.6191(5) 0.0866(3) 0.4814(6) 0.0379(19) Uani 1 1 d . . . S6B S 0.52183(19) 0.10564(11) 0.4946(2) 0.0427(6) Uani 1 1 d . . . O61B O 0.4566(5) 0.0775(3) 0.4140(6) 0.0506(18) Uani 1 1 d . . . O62B O 0.5078(6) 0.1026(3) 0.6024(6) 0.060(2) Uani 1 1 d . . . C7B C 0.5113(7) 0.1745(4) 0.4592(8) 0.039(2) Uani 1 1 d . . . C8B C 0.4777(6) 0.1902(3) 0.3566(7) 0.049(2) Uani 1 1 d . . . H8B H 0.4549 0.1642 0.3050 0.058 Uiso 1 1 calc R . . C9B C 0.4774(6) 0.2452(4) 0.3286(7) 0.055(2) Uani 1 1 d . . . H9B H 0.4567 0.2554 0.2575 0.066 Uiso 1 1 calc R . . C10B C 0.5065(8) 0.2841(4) 0.4031(8) 0.053(3) Uani 1 1 d . . . C11B C 0.5385(6) 0.2679(3) 0.5066(7) 0.060(3) Uani 1 1 d . . . H11B H 0.5599 0.2941 0.5583 0.071 Uiso 1 1 calc R . . C12B C 0.5399(6) 0.2138(4) 0.5365(7) 0.053(2) Uani 1 1 d . . . H12B H 0.5598 0.2038 0.6078 0.064 Uiso 1 1 calc R . . C13B C 0.5086(8) 0.3423(4) 0.3718(10) 0.082(4) Uani 1 1 d . . . H13D H 0.5023 0.3449 0.2955 0.123 Uiso 1 1 calc R . . H13E H 0.5658 0.3583 0.4062 0.123 Uiso 1 1 calc R . . H13F H 0.4589 0.3614 0.3935 0.123 Uiso 1 1 calc R . . Cu2 Cu 0.12881(12) 0.03573(3) 0.88160(13) 0.0332(3) Uani 1 1 d . . . N1C N 0.1772(5) -0.0210(3) 0.9876(6) 0.0356(19) Uani 1 1 d . . . H1C1 H 0.1302 -0.0335 1.0158 0.043 Uiso 1 1 calc R . . H1C2 H 0.1971 -0.0490 0.9524 0.043 Uiso 1 1 calc R . . C2C C 0.2509(8) -0.0057(4) 1.0753(8) 0.056(3) Uani 1 1 d . . . H2C1 H 0.3028 0.0072 1.0466 0.067 Uiso 1 1 calc R . . H2C2 H 0.2705 -0.0376 1.1190 0.067 Uiso 1 1 calc R . . C3C C 0.2218(8) 0.0376(4) 1.1431(8) 0.050(3) Uani 1 1 d . . . H3C1 H 0.1667 0.0255 1.1664 0.060 Uiso 1 1 calc R . . H3C2 H 0.2694 0.0423 1.2065 0.060 Uiso 1 1 calc R . . C4C C 0.2033(7) 0.0909(4) 1.0892(7) 0.050(3) Uani 1 1 d . . . H4C1 H 0.1872 0.1171 1.1396 0.060 Uiso 1 1 calc R . . H4C2 H 0.2587 0.1037 1.0678 0.060 Uiso 1 1 calc R . . N5C N 0.1301(5) 0.0884(3) 0.9963(6) 0.0375(19) Uani 1 1 d . . . S6C S 0.0315(2) 0.10583(11) 1.0069(2) 0.0443(6) Uani 1 1 d . . . O61C O 0.0122(6) 0.0990(3) 1.1133(6) 0.066(2) Uani 1 1 d . . . O62C O -0.0296(5) 0.0796(3) 0.9208(6) 0.0505(18) Uani 1 1 d . . . C7C C 0.0188(7) 0.1754(4) 0.9795(8) 0.040(2) Uani 1 1 d . . . C8C C -0.0159(6) 0.2096(4) 1.0507(7) 0.050(2) Uani 1 1 d . . . H8C H -0.0301 0.1959 1.1135 0.060 Uiso 1 1 calc R . . C9C C -0.0284(6) 0.2645(4) 1.0244(8) 0.058(3) Uani 1 1 d . . . H9C H -0.0484 0.2879 1.0726 0.069 Uiso 1 1 calc R . . C10C C -0.0124(7) 0.2852(4) 0.9307(8) 0.051(3) Uani 1 1 d . . . C11C C 0.0210(6) 0.2499(3) 0.8635(8) 0.050(2) Uani 1 1 d . . . H11C H 0.0340 0.2631 0.7996 0.060 Uiso 1 1 calc R . . C12C C 0.0355(6) 0.1962(3) 0.8883(7) 0.048(2) Uani 1 1 d . . . H12C H 0.0575 0.1734 0.8406 0.058 Uiso 1 1 calc R . . C13C C -0.0276(8) 0.3430(4) 0.9046(9) 0.074(4) Uani 1 1 d . . . H13G H 0.0284 0.3629 0.9286 0.111 Uiso 1 1 calc R . . H13H H -0.0744 0.3570 0.9395 0.111 Uiso 1 1 calc R . . H13I H -0.0468 0.3472 0.8285 0.111 Uiso 1 1 calc R . . N1D N 0.0750(5) -0.0202(3) 0.7737(6) 0.038(2) Uani 1 1 d . . . H1D1 H 0.1201 -0.0340 0.7437 0.046 Uiso 1 1 calc R . . H1D2 H 0.0525 -0.0477 0.8077 0.046 Uiso 1 1 calc R . . C2D C 0.0012(6) 0.0001(4) 0.6876(8) 0.042(2) Uani 1 1 d . . . H2D1 H -0.0472 0.0155 0.7194 0.050 Uiso 1 1 calc R . . H2D2 H -0.0247 -0.0304 0.6431 0.050 Uiso 1 1 calc R . . C3D C 0.0338(9) 0.0424(5) 0.6186(8) 0.054(3) Uani 1 1 d . . . H3D1 H 0.0845 0.0273 0.5905 0.065 Uiso 1 1 calc R . . H3D2 H -0.0155 0.0500 0.5581 0.065 Uiso 1 1 calc R . . C4D C 0.0642(8) 0.0951(4) 0.6735(8) 0.052(3) Uani 1 1 d . . . H4D1 H 0.0863 0.1191 0.6235 0.063 Uiso 1 1 calc R . . H4D2 H 0.0120 0.1126 0.6944 0.063 Uiso 1 1 calc R . . N5D N 0.1363(6) 0.0878(3) 0.7678(6) 0.040(2) Uani 1 1 d . . . S6D S 0.23387(18) 0.10738(10) 0.76423(19) 0.0408(6) Uani 1 1 d . . . O61D O 0.2945(5) 0.0785(3) 0.8480(6) 0.0524(19) Uani 1 1 d . . . O62D O 0.2540(5) 0.1042(3) 0.6591(5) 0.058(2) Uani 1 1 d . . . C7D C 0.2447(7) 0.1770(4) 0.7993(8) 0.044(2) Uani 1 1 d . . . C8D C 0.2154(6) 0.2153(3) 0.7217(7) 0.051(2) Uani 1 1 d . . . H8D H 0.1957 0.2051 0.6505 0.062 Uiso 1 1 calc R . . C9D C 0.2157(7) 0.2686(3) 0.7517(8) 0.061(3) Uani 1 1 d . . . H9D H 0.1960 0.2947 0.6993 0.073 Uiso 1 1 calc R . . C10D C 0.2438(7) 0.2854(4) 0.8552(8) 0.049(3) Uani 1 1 d . . . C11D C 0.2740(6) 0.2466(4) 0.9288(7) 0.053(2) Uani 1 1 d . . . H11D H 0.2964 0.2572 0.9993 0.063 Uiso 1 1 calc R . . C12D C 0.2730(6) 0.1922(3) 0.9035(6) 0.049(2) Uani 1 1 d . . . H12D H 0.2913 0.1662 0.9566 0.059 Uiso 1 1 calc R . . C13D C 0.2439(8) 0.3443(4) 0.8858(8) 0.067(3) Uani 1 1 d . . . H13J H 0.2555 0.3475 0.9624 0.100 Uiso 1 1 calc R . . H13K H 0.1853 0.3601 0.8561 0.100 Uiso 1 1 calc R . . H13L H 0.2911 0.3631 0.8585 0.100 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 0.0325(5) 0.0335(4) 0.0320(6) 0.0001(6) 0.0025(4) 0.0007(7) N1A 0.039(5) 0.040(4) 0.044(5) -0.007(3) -0.001(4) -0.002(4) C2A 0.038(6) 0.048(6) 0.062(6) -0.001(4) -0.013(5) -0.004(4) C3A 0.068(8) 0.067(7) 0.033(5) 0.007(4) -0.013(5) -0.006(6) N5A 0.041(5) 0.042(4) 0.035(4) -0.001(3) 0.006(4) -0.004(3) C4A 0.055(6) 0.048(5) 0.039(5) 0.000(4) -0.009(5) 0.002(5) S6A 0.0498(15) 0.0347(11) 0.0478(13) 0.0019(9) 0.0170(12) 0.0023(10) O61A 0.048(4) 0.039(3) 0.072(5) 0.000(3) 0.014(4) 0.010(3) O62A 0.097(6) 0.052(4) 0.055(4) -0.005(3) 0.038(4) -0.003(4) C7A 0.038(5) 0.039(5) 0.042(5) 0.006(4) 0.006(4) 0.008(4) C8A 0.047(6) 0.058(5) 0.043(5) 0.011(4) 0.010(4) -0.003(4) C9A 0.061(7) 0.052(5) 0.071(7) 0.014(4) 0.016(5) -0.008(5) C10A 0.037(5) 0.042(5) 0.055(6) -0.004(4) -0.009(5) -0.006(4) C11A 0.051(6) 0.055(5) 0.042(5) -0.004(4) 0.006(4) -0.002(5) C12A 0.045(5) 0.052(5) 0.061(6) 0.001(4) 0.016(5) -0.008(4) C13A 0.078(8) 0.047(6) 0.076(8) 0.013(5) -0.025(6) -0.011(5) N1B 0.036(5) 0.032(4) 0.043(4) 0.002(3) 0.011(4) 0.004(3) C2B 0.048(6) 0.050(6) 0.035(5) 0.005(4) -0.005(5) 0.010(5) C3B 0.055(6) 0.054(6) 0.038(5) 0.004(4) -0.011(5) 0.008(5) C4B 0.053(6) 0.044(5) 0.038(5) -0.010(4) -0.010(4) 0.004(4) N5B 0.043(4) 0.030(4) 0.039(4) -0.003(3) 0.003(4) 0.007(3) S6B 0.0472(15) 0.0372(12) 0.0479(13) 0.0003(9) 0.0196(11) -0.0003(10) O61B 0.042(4) 0.049(4) 0.062(4) -0.012(3) 0.014(3) -0.003(3) O62B 0.091(6) 0.051(4) 0.049(4) 0.001(3) 0.040(4) -0.007(4) C7B 0.035(5) 0.033(4) 0.052(5) -0.002(3) 0.013(4) 0.014(4) C8B 0.046(5) 0.042(4) 0.058(6) -0.006(4) 0.013(4) 0.003(4) C9B 0.056(6) 0.060(6) 0.051(6) 0.010(4) 0.013(5) 0.013(5) C10B 0.056(7) 0.037(5) 0.067(7) 0.002(4) 0.016(5) 0.001(4) C11B 0.069(7) 0.045(5) 0.062(6) -0.013(4) 0.007(6) -0.008(5) C12B 0.064(7) 0.055(5) 0.040(5) -0.005(4) 0.008(5) 0.009(5) C13B 0.083(9) 0.042(5) 0.123(10) 0.020(6) 0.022(7) 0.015(5) Cu2 0.0317(5) 0.0341(4) 0.0327(6) 0.0009(6) 0.0034(4) 0.0001(7) N1C 0.031(4) 0.040(4) 0.036(4) -0.002(3) 0.008(4) 0.006(3) C2C 0.066(7) 0.043(5) 0.044(5) 0.006(4) -0.023(5) 0.001(5) C3C 0.060(6) 0.045(5) 0.038(5) 0.001(4) -0.005(5) 0.004(5) C4C 0.063(6) 0.043(5) 0.040(5) -0.004(4) 0.002(5) -0.005(5) N5C 0.043(4) 0.035(4) 0.033(4) -0.003(3) 0.001(3) 0.006(3) S6C 0.0482(15) 0.0382(12) 0.0506(13) -0.0007(9) 0.0201(12) -0.0038(10) O61C 0.101(6) 0.054(4) 0.056(4) 0.001(3) 0.047(4) -0.009(4) O62C 0.037(4) 0.048(4) 0.067(4) -0.014(3) 0.012(3) -0.002(3) C7C 0.029(5) 0.041(5) 0.049(5) 0.005(4) 0.002(4) 0.005(4) C8C 0.061(6) 0.052(5) 0.041(5) -0.008(4) 0.017(5) -0.003(5) C9C 0.049(6) 0.053(5) 0.067(6) -0.014(4) 0.004(5) 0.015(4) C10C 0.041(6) 0.043(5) 0.061(6) -0.010(4) -0.010(5) 0.010(4) C11C 0.041(5) 0.038(4) 0.067(6) 0.002(4) 0.002(5) 0.003(4) C12C 0.050(6) 0.036(4) 0.055(5) -0.002(4) 0.004(5) 0.004(4) C13C 0.071(8) 0.043(5) 0.096(9) 0.005(5) -0.011(7) 0.012(5) N1D 0.033(5) 0.037(4) 0.043(4) 0.000(3) 0.004(4) 0.001(4) C2D 0.020(4) 0.046(5) 0.056(6) -0.003(4) 0.000(4) 0.000(4) C3D 0.066(7) 0.062(7) 0.030(5) 0.002(4) 0.000(5) -0.002(5) C4D 0.070(7) 0.036(5) 0.045(5) 0.001(4) -0.003(5) -0.004(5) N5D 0.046(5) 0.036(4) 0.036(4) -0.001(3) 0.000(4) -0.003(3) S6D 0.0472(15) 0.0356(11) 0.0427(13) 0.0013(9) 0.0166(11) 0.0007(10) O61D 0.042(4) 0.040(3) 0.075(5) 0.005(3) 0.010(3) 0.007(3) O62D 0.092(6) 0.046(4) 0.045(4) -0.003(3) 0.036(4) 0.002(4) C7D 0.037(5) 0.037(5) 0.058(6) -0.014(4) 0.008(5) -0.002(4) C8D 0.074(7) 0.031(4) 0.052(5) -0.001(3) 0.020(5) -0.007(4) C9D 0.071(7) 0.039(5) 0.070(7) 0.005(4) 0.007(6) -0.008(5) C10D 0.039(6) 0.043(5) 0.066(7) -0.001(4) 0.012(5) -0.005(4) C11D 0.059(6) 0.052(5) 0.048(5) -0.016(4) 0.013(5) -0.010(5) C12D 0.054(6) 0.056(5) 0.037(5) 0.000(4) 0.009(4) -0.010(4) C13D 0.081(8) 0.045(5) 0.074(7) -0.019(5) 0.015(6) 0.002(5) _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 N5B 1.954(8) . ? Cu1 N5A 1.970(8) . ? Cu1 N1B 2.013(7) . ? Cu1 N1A 2.023(7) . ? N1A C2A 1.480(11) . ? C2A C3A 1.438(15) . ? C3A C4A 1.508(14) . ? N5A C4A 1.472(10) . ? N5A S6A 1.560(9) . ? S6A O61A 1.448(7) . ? S6A O62A 1.449(7) . ? S6A C7A 1.789(10) . ? C7A C8A 1.355(12) . ? C7A C12A 1.392(12) . ? C8A C9A 1.364(12) . ? C9A C10A 1.381(13) . ? C10A C11A 1.391(13) . ? C10A C13A 1.509(12) . ? C11A C12A 1.380(11) . ? N1B C2B 1.480(11) . ? C2B C3B 1.530(14) . ? C3B C4B 1.494(13) . ? C4B N5B 1.468(10) . ? N5B S6B 1.576(9) . ? S6B O62B 1.446(7) . ? S6B O61B 1.456(7) . ? S6B C7B 1.766(10) . ? C7B C8B 1.373(12) . ? C7B C12B 1.397(12) . ? C8B C9B 1.410(11) . ? C9B C10B 1.369(13) . ? C10B C11B 1.384(13) . ? C10B C13B 1.499(13) . ? C11B C12B 1.394(12) . ? Cu2 N5C 1.969(7) . ? Cu2 N5D 1.972(8) . ? Cu2 N1C 1.994(7) . ? Cu2 N1D 2.015(7) . ? N1C C2C 1.465(11) . ? C2C C3C 1.502(15) . ? C3C C4C 1.492(13) . ? C4C N5C 1.456(11) . ? N5C S6C 1.575(9) . ? S6C O62C 1.446(7) . ? S6C O61C 1.465(8) . ? S6C C7C 1.762(10) . ? C7C C12C 1.351(13) . ? C7C C8C 1.421(13) . ? C8C C9C 1.406(12) . ? C9C C10C 1.376(14) . ? C10C C11C 1.393(13) . ? C10C C13C 1.479(13) . ? C11C C12C 1.377(11) . ? N1D C2D 1.490(10) . ? C2D C3D 1.518(15) . ? C3D C4D 1.512(14) . ? C4D N5D 1.469(11) . ? N5D S6D 1.553(9) . ? S6D O62D 1.446(7) . ? S6D O61D 1.454(7) . ? S6D C7D 1.783(10) . ? C7D C12D 1.377(11) . ? C7D C8D 1.384(12) . ? C8D C9D 1.376(11) . ? C9D C10D 1.380(13) . ? C10D C11D 1.362(12) . ? C10D C13D 1.513(13) . ? C11D C12D 1.387(11) . ? 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 N5B Cu1 N5A 97.9(2) . . ? N5B Cu1 N1B 90.5(3) . . ? N5A Cu1 N1B 153.7(4) . . ? N5B Cu1 N1A 154.5(4) . . ? N5A Cu1 N1A 91.2(3) . . ? N1B Cu1 N1A 91.8(2) . . ? C2A N1A Cu1 113.7(6) . . ? C3A C2A N1A 116.5(9) . . ? C2A C3A C4A 119.4(10) . . ? C4A N5A S6A 118.9(7) . . ? C4A N5A Cu1 123.7(7) . . ? S6A N5A Cu1 113.1(4) . . ? N5A C4A C3A 110.6(8) . . ? O61A S6A O62A 117.4(5) . . ? O61A S6A N5A 105.9(5) . . ? O62A S6A N5A 112.7(5) . . ? O61A S6A C7A 105.7(4) . . ? O62A S6A C7A 104.7(5) . . ? N5A S6A C7A 110.1(5) . . ? C8A C7A C12A 120.8(9) . . ? C8A C7A S6A 122.2(8) . . ? C12A C7A S6A 117.0(7) . . ? C7A C8A C9A 120.0(10) . . ? C8A C9A C10A 122.4(9) . . ? C9A C10A C11A 116.4(9) . . ? C9A C10A C13A 123.3(10) . . ? C11A C10A C13A 120.3(10) . . ? C12A C11A C10A 122.6(9) . . ? C11A C12A C7A 117.8(9) . . ? C2B N1B Cu1 115.4(6) . . ? N1B C2B C3B 111.4(8) . . ? C4B C3B C2B 113.6(9) . . ? N5B C4B C3B 111.7(8) . . ? C4B N5B S6B 119.3(7) . . ? C4B N5B Cu1 122.5(6) . . ? S6B N5B Cu1 115.3(4) . . ? O62B S6B O61B 116.9(5) . . ? O62B S6B N5B 113.8(5) . . ? O61B S6B N5B 106.7(4) . . ? O62B S6B C7B 106.0(5) . . ? O61B S6B C7B 105.5(5) . . ? N5B S6B C7B 107.4(5) . . ? C8B C7B C12B 119.4(9) . . ? C8B C7B S6B 121.3(7) . . ? C12B C7B S6B 119.3(7) . . ? C7B C8B C9B 120.2(8) . . ? C10B C9B C8B 121.1(9) . . ? C9B C10B C11B 118.1(9) . . ? C9B C10B C13B 120.7(10) . . ? C11B C10B C13B 121.1(10) . . ? C10B C11B C12B 122.0(8) . . ? C11B C12B C7B 119.1(8) . . ? N5C Cu2 N5D 97.4(2) . . ? N5C Cu2 N1C 90.4(3) . . ? N5D Cu2 N1C 154.6(4) . . ? N5C Cu2 N1D 156.4(4) . . ? N5D Cu2 N1D 90.7(3) . . ? N1C Cu2 N1D 91.7(2) . . ? C2C N1C Cu2 117.5(6) . . ? N1C C2C C3C 111.7(9) . . ? C4C C3C C2C 114.3(9) . . ? N5C C4C C3C 112.7(8) . . ? C4C N5C S6C 119.1(7) . . ? C4C N5C Cu2 122.5(6) . . ? S6C N5C Cu2 112.1(4) . . ? O62C S6C O61C 116.8(5) . . ? O62C S6C N5C 105.9(4) . . ? O61C S6C N5C 114.5(5) . . ? O62C S6C C7C 105.0(5) . . ? O61C S6C C7C 105.5(5) . . ? N5C S6C C7C 108.5(5) . . ? C12C C7C C8C 119.2(9) . . ? C12C C7C S6C 121.1(8) . . ? C8C C7C S6C 119.6(8) . . ? C9C C8C C7C 118.1(9) . . ? C10C C9C C8C 122.3(9) . . ? C9C C10C C11C 117.2(9) . . ? C9C C10C C13C 121.0(10) . . ? C11C C10C C13C 121.7(11) . . ? C12C C11C C10C 121.6(10) . . ? C7C C12C C11C 121.5(9) . . ? C2D N1D Cu2 114.7(6) . . ? N1D C2D C3D 112.9(8) . . ? C4D C3D C2D 115.2(9) . . ? N5D C4D C3D 112.6(8) . . ? C4D N5D S6D 118.8(7) . . ? C4D N5D Cu2 123.6(7) . . ? S6D N5D Cu2 114.8(4) . . ? O62D S6D O61D 116.8(5) . . ? O62D S6D N5D 112.6(4) . . ? O61D S6D N5D 106.3(4) . . ? O62D S6D C7D 105.3(5) . . ? O61D S6D C7D 106.0(4) . . ? N5D S6D C7D 109.6(5) . . ? C12D C7D C8D 120.5(9) . . ? C12D C7D S6D 120.5(8) . . ? C8D C7D S6D 118.7(7) . . ? C9D C8D C7D 118.2(8) . . ? C8D C9D C10D 122.9(9) . . ? C11D C10D C9D 117.1(9) . . ? C11D C10D C13D 121.1(9) . . ? C9D C10D C13D 121.8(9) . . ? C10D C11D C12D 122.4(8) . . ? C7D C12D C11D 118.8(8) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 70.17 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.558 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.089 #===END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Cu(C10H15N2O2S)2] _chemical_formula_sum 'C20 H30 Cu N4 O4 S2' _chemical_formula_weight 518.14 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 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 32.427(7) _cell_length_b 6.1076(15) _cell_length_c 23.254(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.30(3) _cell_angle_gamma 90.00 _cell_volume 4577.6(19) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 15 _cell_measurement_theta_max 15.5 _exptl_crystal_description needle _exptl_crystal_colour Green _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.907 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_process_details ; The crystal size and morphology were refined against a set of psi-scan data (Stoe X-Shape), and the results used to perform an numerical absorption correction by Gaussian integration. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -5 _diffrn_reflns_number 6336 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.1093 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4050 _reflns_number_gt 1955 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution DIRDIF _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _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^)+(0.0435P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4050 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1426 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.12439(2) 0.58243(11) 0.87575(4) 0.02047(19) Uani 1 1 d . . . N1A N 0.16967(14) 0.3610(8) 0.8735(2) 0.0249(12) Uani 1 1 d . . . H1A1 H 0.1697 0.2723 0.9050 0.030 Uiso 1 1 calc R . . H1A2 H 0.1637 0.2761 0.8415 0.030 Uiso 1 1 calc R . . C2A C 0.21211(16) 0.4520(10) 0.8726(3) 0.0265(15) Uani 1 1 d . . . H2A1 H 0.2127 0.5455 0.8385 0.032 Uiso 1 1 calc R . . H2A2 H 0.2317 0.3315 0.8695 0.032 Uiso 1 1 calc R . . C3A C 0.22586(17) 0.5849(12) 0.9266(3) 0.0288(15) Uani 1 1 d . . . H3A1 H 0.2212 0.4984 0.9608 0.035 Uiso 1 1 calc R . . H3A2 H 0.2557 0.6131 0.9282 0.035 Uiso 1 1 calc R . . C4A C 0.2035(2) 0.7994(12) 0.9288(3) 0.0254(17) Uani 1 1 d . . . H4A1 H 0.2148 0.8802 0.9634 0.030 Uiso 1 1 calc R . . H4A2 H 0.2083 0.8870 0.8949 0.030 Uiso 1 1 calc R . . N5A N 0.15784(19) 0.7701(8) 0.9301(3) 0.0224(17) Uani 1 1 d . . . S6A S 0.13528(5) 0.9002(3) 0.97482(6) 0.0221(4) Uani 1 1 d . . . C7A C 0.15646(18) 0.8194(13) 1.0457(3) 0.0195(15) Uani 1 1 d . . . C8A C 0.17027(18) 0.6029(11) 1.0554(3) 0.0250(16) Uani 1 1 d . . . H8A H 0.1675 0.4977 1.0257 0.030 Uiso 1 1 calc R . . C9A C 0.18813(18) 0.5511(11) 1.1107(3) 0.0330(17) Uani 1 1 d . . . H9A H 0.1986 0.4090 1.1178 0.040 Uiso 1 1 calc R . . C10A C 0.1912(2) 0.7014(14) 1.1565(3) 0.0295(19) Uani 1 1 d . . . C11A C 0.17685(17) 0.9064(13) 1.1447(3) 0.0292(16) Uani 1 1 d . . . H11A H 0.1784 1.0099 1.1748 0.035 Uiso 1 1 calc R . . C12A C 0.15981(17) 0.9695(10) 1.0898(3) 0.0256(15) Uani 1 1 d . . . H12A H 0.1506 1.1141 1.0830 0.031 Uiso 1 1 calc R . . C13A C 0.2112(2) 0.6353(13) 1.2160(3) 0.050(2) Uani 1 1 d . . . H13A H 0.2407 0.6119 1.2146 0.075 Uiso 1 1 calc R . . H13B H 0.1985 0.5012 1.2279 0.075 Uiso 1 1 calc R . . H13C H 0.2072 0.7506 1.2435 0.075 Uiso 1 1 calc R . . O61A O 0.09221(12) 0.8344(8) 0.96684(18) 0.0322(11) Uani 1 1 d . . . O62A O 0.14238(14) 1.1366(7) 0.97393(17) 0.0353(12) Uani 1 1 d . . . N1B N 0.07897(13) 0.3603(8) 0.8788(2) 0.0250(13) Uani 1 1 d . . . H1B1 H 0.0796 0.2672 0.8484 0.030 Uiso 1 1 calc R . . H1B2 H 0.0845 0.2802 0.9118 0.030 Uiso 1 1 calc R . . C2B C 0.03624(17) 0.4509(11) 0.8775(3) 0.0313(16) Uani 1 1 d . . . H2B1 H 0.0347 0.5457 0.9112 0.038 Uiso 1 1 calc R . . H2B2 H 0.0165 0.3305 0.8797 0.038 Uiso 1 1 calc R . . C3B C 0.02442(17) 0.5807(11) 0.8229(3) 0.0295(15) Uani 1 1 d . . . H3B1 H -0.0056 0.6047 0.8186 0.035 Uiso 1 1 calc R . . H3B2 H 0.0310 0.4938 0.7897 0.035 Uiso 1 1 calc R . . C4B C 0.0462(2) 0.8023(13) 0.8215(3) 0.0302(18) Uani 1 1 d . . . H4B1 H 0.0352 0.8825 0.7866 0.036 Uiso 1 1 calc R . . H4B2 H 0.0405 0.8889 0.8552 0.036 Uiso 1 1 calc R . . N5B N 0.0906(2) 0.7736(8) 0.8218(3) 0.0241(17) Uani 1 1 d . . . S6B S 0.11390(5) 0.9071(3) 0.77746(7) 0.0230(4) Uani 1 1 d . . . C7B C 0.09232(18) 0.8342(12) 0.7064(3) 0.0219(16) Uani 1 1 d . . . C8B C 0.07033(19) 0.9848(10) 0.6707(3) 0.0298(16) Uani 1 1 d . . . H8B H 0.0654 1.1257 0.6847 0.036 Uiso 1 1 calc R . . C9B C 0.05563(18) 0.9301(13) 0.6148(3) 0.0333(17) Uani 1 1 d . . . H9B H 0.0406 1.0336 0.5911 0.040 Uiso 1 1 calc R . . C10B C 0.0628(3) 0.7241(13) 0.5932(4) 0.033(2) Uani 1 1 d . . . C11B C 0.08454(19) 0.5718(12) 0.6299(3) 0.0334(16) Uani 1 1 d . . . H11B H 0.0894 0.4306 0.6161 0.040 Uiso 1 1 calc R . . C12B C 0.09867(19) 0.6257(11) 0.6853(3) 0.0267(16) Uani 1 1 d . . . H12B H 0.1129 0.5208 0.7095 0.032 Uiso 1 1 calc R . . C13B C 0.0487(2) 0.6691(15) 0.5311(3) 0.059(2) Uani 1 1 d . . . H13D H 0.0187 0.6749 0.5247 0.088 Uiso 1 1 calc R . . H13E H 0.0581 0.5231 0.5226 0.088 Uiso 1 1 calc R . . H13F H 0.0603 0.7740 0.5060 0.088 Uiso 1 1 calc R . . O61B O 0.15688(12) 0.8397(8) 0.78417(18) 0.0329(11) Uani 1 1 d . . . O62B O 0.10726(14) 1.1426(7) 0.77988(18) 0.0349(12) 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 0.0183(3) 0.0199(4) 0.0219(4) -0.0010(5) -0.0034(3) -0.0005(4) N1A 0.029(3) 0.018(3) 0.026(3) -0.002(2) -0.003(2) 0.003(2) C2A 0.020(3) 0.028(4) 0.033(4) -0.002(3) 0.009(3) 0.000(3) C3A 0.018(3) 0.042(4) 0.027(4) 0.001(4) 0.001(3) -0.004(3) C4A 0.022(4) 0.039(4) 0.015(4) -0.009(4) 0.002(3) -0.011(4) N5A 0.017(3) 0.033(4) 0.018(4) -0.007(2) 0.002(3) -0.001(2) S6A 0.0267(8) 0.0225(9) 0.0165(8) -0.0012(8) -0.0008(7) 0.0028(8) C7A 0.021(3) 0.026(4) 0.011(3) -0.007(3) 0.001(3) 0.001(3) C8A 0.036(4) 0.019(4) 0.022(4) -0.006(3) 0.010(3) -0.001(3) C9A 0.030(3) 0.028(4) 0.039(4) 0.015(4) -0.005(3) -0.002(3) C10A 0.028(4) 0.034(4) 0.026(5) 0.015(4) 0.002(3) -0.005(4) C11A 0.027(3) 0.037(4) 0.023(4) -0.012(4) 0.001(3) -0.008(4) C12A 0.030(3) 0.023(4) 0.023(4) -0.006(3) 0.002(3) -0.001(3) C13A 0.064(5) 0.054(6) 0.029(4) 0.016(4) -0.009(4) -0.004(4) O61A 0.023(2) 0.043(3) 0.029(3) -0.010(2) -0.002(2) 0.005(2) O62A 0.061(3) 0.018(3) 0.026(3) -0.003(2) 0.000(2) 0.003(2) N1B 0.022(3) 0.029(3) 0.023(3) 0.002(3) -0.002(2) -0.001(2) C2B 0.024(3) 0.036(4) 0.034(4) 0.003(3) 0.002(3) -0.003(3) C3B 0.018(3) 0.043(4) 0.026(4) 0.003(4) -0.005(3) 0.005(3) C4B 0.024(4) 0.036(4) 0.030(5) 0.012(4) -0.002(3) 0.000(4) N5B 0.025(4) 0.026(4) 0.021(4) 0.009(2) -0.002(3) 0.000(2) S6B 0.0253(8) 0.0245(9) 0.0181(9) 0.0008(8) -0.0023(7) -0.0043(8) C7B 0.020(3) 0.023(4) 0.022(4) -0.006(4) 0.005(3) -0.002(3) C8B 0.036(4) 0.024(4) 0.028(4) -0.002(3) -0.001(3) 0.001(3) C9B 0.029(3) 0.042(5) 0.028(4) 0.015(4) -0.002(3) -0.001(4) C10B 0.037(5) 0.051(6) 0.013(4) -0.009(4) 0.010(4) -0.019(4) C11B 0.037(4) 0.030(4) 0.037(4) -0.014(4) 0.018(3) -0.009(4) C12B 0.035(4) 0.018(4) 0.026(4) 0.002(3) 0.003(3) -0.003(3) C13B 0.072(6) 0.082(6) 0.021(4) -0.009(4) 0.001(4) -0.039(5) O61B 0.023(2) 0.052(3) 0.023(3) 0.004(3) 0.0018(19) -0.005(2) O62B 0.060(3) 0.016(3) 0.027(3) -0.005(2) -0.002(2) -0.004(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 N5A 1.946(6) . ? Cu1 N5B 1.959(6) . ? Cu1 N1A 2.001(5) . ? Cu1 N1B 2.009(5) . ? N1A C2A 1.487(7) . ? C2A C3A 1.520(8) . ? C3A C4A 1.501(9) . ? C4A N5A 1.494(8) . ? N5A S6A 1.554(6) . ? S6A O61A 1.445(4) . ? S6A O62A 1.463(5) . ? S6A C7A 1.784(7) . ? C7A C12A 1.372(8) . ? C7A C8A 1.406(9) . ? C8A C9A 1.388(8) . ? C9A C10A 1.401(10) . ? C10A C11A 1.354(10) . ? C10A C13A 1.515(9) . ? C11A C12A 1.388(8) . ? N1B C2B 1.489(7) . ? C2B C3B 1.510(8) . ? C3B C4B 1.528(9) . ? C4B N5B 1.449(9) . ? N5B S6B 1.572(6) . ? S6B O61B 1.445(4) . ? S6B O62B 1.456(5) . ? S6B C7B 1.779(7) . ? C7B C8B 1.384(8) . ? C7B C12B 1.388(10) . ? C8B C9B 1.375(8) . ? C9B C10B 1.384(10) . ? C10B C11B 1.400(10) . ? C10B C13B 1.503(10) . ? C11B C12B 1.359(8) . ? 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 N5A Cu1 N5B 107.33(18) . . ? N5A Cu1 N1A 93.3(2) . . ? N5B Cu1 N1A 138.3(2) . . ? N5A Cu1 N1B 137.1(2) . . ? N5B Cu1 N1B 93.7(2) . . ? N1A Cu1 N1B 95.01(16) . . ? C2A N1A Cu1 115.5(4) . . ? N1A C2A C3A 112.1(5) . . ? C4A C3A C2A 113.3(5) . . ? N5A C4A C3A 112.3(6) . . ? C4A N5A S6A 119.5(5) . . ? C4A N5A Cu1 122.7(4) . . ? S6A N5A Cu1 117.8(4) . . ? O61A S6A O62A 115.1(3) . . ? O61A S6A N5A 106.9(3) . . ? O62A S6A N5A 114.1(3) . . ? O61A S6A C7A 108.1(3) . . ? O62A S6A C7A 103.9(3) . . ? N5A S6A C7A 108.3(3) . . ? C12A C7A C8A 120.7(6) . . ? C12A C7A S6A 119.8(6) . . ? C8A C7A S6A 119.5(5) . . ? C9A C8A C7A 117.2(6) . . ? C8A C9A C10A 122.9(6) . . ? C11A C10A C9A 117.2(7) . . ? C11A C10A C13A 122.4(8) . . ? C9A C10A C13A 120.5(7) . . ? C10A C11A C12A 122.5(7) . . ? C7A C12A C11A 119.6(6) . . ? C2B N1B Cu1 115.6(4) . . ? N1B C2B C3B 111.3(5) . . ? C2B C3B C4B 114.0(5) . . ? N5B C4B C3B 110.7(6) . . ? C4B N5B S6B 118.9(5) . . ? C4B N5B Cu1 124.1(5) . . ? S6B N5B Cu1 116.9(4) . . ? O61B S6B O62B 115.0(3) . . ? O61B S6B N5B 108.0(3) . . ? O62B S6B N5B 113.8(3) . . ? O61B S6B C7B 107.8(3) . . ? O62B S6B C7B 103.8(3) . . ? N5B S6B C7B 108.1(3) . . ? C8B C7B C12B 118.9(6) . . ? C8B C7B S6B 121.0(5) . . ? C12B C7B S6B 120.0(5) . . ? C9B C8B C7B 120.5(6) . . ? C8B C9B C10B 120.7(7) . . ? C9B C10B C11B 118.4(7) . . ? C9B C10B C13B 120.5(8) . . ? C11B C10B C13B 121.1(7) . . ? C12B C11B C10B 120.8(7) . . ? C11B C12B C7B 120.7(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.908 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.087