# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (c) The Royal Society of Chemistry 2009 data_C6-H2TPz _audit_creation_method SHELXL-97 _chemical_name_systematic ; C6-H2TPz ; _chemical_name_common C6-H2TPz _chemical_melting_point ? _chemical_formula_moiety C48H58N8S4 _chemical_formula_sum 'C48 H58 N8 S4' _chemical_formula_weight 875.26 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 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 17.173(8) _cell_length_b 6.043(3) _cell_length_c 22.627(13) _cell_angle_alpha 90.00 _cell_angle_beta 103.433(18) _cell_angle_gamma 90.00 _cell_volume 2284(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9340 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'dark' _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.450 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 0.252 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.261 _exptl_absorpt_correction_T_max 0.988 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number 18759 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17703 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_av_sigmaI/netI 0.0791 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4960 _reflns_number_gt 2231 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.0000 _refine_ls_number_reflns 4960 _refine_ls_number_parameters 277 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1696 _refine_ls_R_factor_gt 0.0912 _refine_ls_wR_factor_ref 0.3330 _refine_ls_wR_factor_gt 0.2590 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.5276(2) 0.1026(6) 0.42370(16) 0.0671(9) Uani 1 1 d . A . H1 H 0.5179 0.0618 0.4665 0.111 Uiso 1 1 d . . . N2 N 0.6263(2) -0.1784(6) 0.41746(16) 0.0697(10) Uani 1 1 d . A . N3 N 0.5718(2) -0.2481(6) 0.50534(15) 0.0651(9) Uani 1 1 d . A . N4 N 0.5520(2) -0.4369(6) 0.59599(16) 0.0695(10) Uani 1 1 d . . . S1 S 0.5466(3) 0.4993(7) 0.28914(16) 0.0850(10) Uani 0.50 1 d PD A 2 S2 S 0.6514(2) 0.1451(8) 0.29770(18) 0.0670(7) Uani 0.50 1 d PD A 1 S3 S 0.7390(3) -0.6407(9) 0.4650(3) 0.0911(12) Uani 0.50 1 d PD A 2 S4 S 0.6934(3) -0.7981(6) 0.56474(17) 0.0655(7) Uani 0.50 1 d PD A 1 C1 C 0.5005(3) 0.2957(8) 0.3930(2) 0.0670(11) Uani 1 1 d . . . C2 C 0.5427(3) 0.3149(7) 0.34513(19) 0.0672(11) Uani 1 1 d D . . C3 C 0.6183(8) 0.3389(19) 0.2667(6) 0.0850(10) Uani 0.50 1 d PD A 2 C4 C 0.6400(11) 0.152(3) 0.3023(8) 0.0850(10) Uani 0.50 1 d PD A 2 H2 H 0.6785 0.0504 0.2975 0.102 Uiso 0.50 1 calc PR A 2 C5 C 0.5932(3) 0.1395(8) 0.34883(19) 0.0688(12) Uani 1 1 d D A . C6 C 0.6089(6) 0.3956(16) 0.2697(5) 0.0670(7) Uani 0.50 1 d PD A 1 C7 C 0.5549(10) 0.466(3) 0.3024(7) 0.0670(7) Uani 0.50 1 d PD A 1 H3 H 0.5292 0.6027 0.2962 0.080 Uiso 0.50 1 calc PR A 1 C8 C 0.5842(3) 0.0024(8) 0.3988(2) 0.0702(12) Uani 1 1 d . . . C9 C 0.6197(3) -0.2920(8) 0.4660(2) 0.0688(11) Uani 1 1 d . . . C10 C 0.6668(3) -0.4880(8) 0.4857(2) 0.0689(12) Uani 1 1 d D A . C11 C 0.7410(8) -0.822(2) 0.5247(5) 0.0911(12) Uani 0.50 1 d PD A 2 C12 C 0.6887(12) -0.767(3) 0.5603(9) 0.0911(12) Uani 0.50 1 d PD A 2 H4 H 0.6821 -0.8444 0.5943 0.109 Uiso 0.50 1 calc PR A 2 C13 C 0.6451(3) -0.5650(8) 0.5359(2) 0.0693(12) Uani 1 1 d D . . C14 C 0.7436(7) -0.8054(18) 0.5063(4) 0.0655(7) Uani 0.50 1 d PD A 1 C15 C 0.7199(10) -0.627(3) 0.4668(8) 0.0655(7) Uani 0.50 1 d PD A 1 H5 H 0.7380 -0.6043 0.4317 0.079 Uiso 0.50 1 calc PR A 1 C16 C 0.5865(3) -0.4127(7) 0.5490(2) 0.0681(11) Uani 1 1 d . A . C17 C 0.6435(4) 0.4811(16) 0.2196(3) 0.138(3) Uani 1 1 d . . . H6 H 0.6016 0.5784 0.1977 0.169 Uiso 1 1 d . . . H7 H 0.6519 0.3702 0.1915 0.169 Uiso 1 1 d . . . C18 C 0.7153(5) 0.6107(10) 0.2385(3) 0.111(2) Uani 1 1 d . A . H8 H 0.7062 0.7163 0.2679 0.139 Uiso 1 1 d . . . H9 H 0.7565 0.5102 0.2596 0.139 Uiso 1 1 d . . . C19 C 0.7510(4) 0.7328(11) 0.1956(3) 0.1022(18) Uani 1 1 d . . . H10 H 0.7100 0.8295 0.1728 0.129 Uiso 1 1 d . . . H11 H 0.7637 0.6278 0.1672 0.129 Uiso 1 1 d . . . C20 C 0.8224(5) 0.8699(11) 0.2195(3) 0.123(2) Uani 1 1 d . A . H12 H 0.8100 0.9648 0.2498 0.154 Uiso 1 1 d . . . H13 H 0.8638 0.7677 0.2405 0.154 Uiso 1 1 d . . . C21 C 0.8588(4) 1.0021(13) 0.1809(3) 0.116(2) Uani 1 1 d . . . H14 H 0.8188 1.1044 0.1593 0.145 Uiso 1 1 d . . . H15 H 0.8737 0.9086 0.1509 0.145 Uiso 1 1 d . . . C22 C 0.9282(5) 1.1380(12) 0.2073(3) 0.121(2) Uani 1 1 d . A . H16 H 0.9467 1.2173 0.1769 0.146 Uiso 1 1 d . . . H17 H 0.9163 1.2357 0.2361 0.146 Uiso 1 1 d . . . H18 H 0.9713 1.0404 0.2275 0.146 Uiso 1 1 d . . . C23 C 0.8003(4) -0.9962(11) 0.5121(4) 0.129(3) Uani 1 1 d . . . H19 H 0.8101 -0.9980 0.4717 0.162 Uiso 1 1 d . . . H20 H 0.7748 -1.1341 0.5174 0.162 Uiso 1 1 d . . . C24 C 0.8770(3) -0.9838(9) 0.5561(3) 0.0880(15) Uani 1 1 d . A . H21 H 0.9028 -0.8465 0.5516 0.113 Uiso 1 1 d . . . H22 H 0.8683 -0.9887 0.5965 0.113 Uiso 1 1 d . . . C25 C 0.9331(4) -1.1739(11) 0.5495(3) 0.1066(19) Uani 1 1 d . . . H23 H 0.9447 -1.1675 0.5093 0.135 Uiso 1 1 d . . . H24 H 0.9071 -1.3138 0.5517 0.135 Uiso 1 1 d . . . C26 C 1.0094(4) -1.1728(16) 0.5964(3) 0.141(3) Uani 1 1 d . A . H25 H 1.0403 -1.0338 0.5927 0.182 Uiso 1 1 d . . . H26 H 1.0002 -1.1629 0.6370 0.182 Uiso 1 1 d . . . C27 C 1.0629(6) -1.382(2) 0.5890(4) 0.197(6) Uani 1 1 d . . . H27 H 1.0813 -1.3664 0.5525 0.232 Uiso 1 1 d . . . H28 H 1.0259 -1.5087 0.5825 0.232 Uiso 1 1 d . . . C28 C 1.1222(8) -1.436(2) 0.6336(5) 0.226(7) Uani 1 1 d . A . H29 H 1.1609 -1.3145 0.6402 0.248 Uiso 1 1 d . . . H30 H 1.1054 -1.4572 0.6702 0.248 Uiso 1 1 d . . . H31 H 1.1496 -1.5644 0.6249 0.248 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 N1 0.076(2) 0.070(2) 0.058(2) -0.0025(16) 0.0197(17) 0.002(2) N2 0.074(2) 0.074(2) 0.063(2) -0.0022(18) 0.0197(18) 0.004(2) N3 0.068(2) 0.069(2) 0.059(2) -0.0049(16) 0.0174(17) 0.0002(18) N4 0.072(2) 0.074(2) 0.063(2) -0.0026(17) 0.0186(18) 0.007(2) S1 0.103(2) 0.089(2) 0.064(2) 0.0009(14) 0.0217(18) 0.0017(16) S2 0.0673(15) 0.0846(15) 0.0524(13) 0.0010(11) 0.0209(10) 0.0040(13) S3 0.089(3) 0.091(2) 0.096(2) -0.0088(15) 0.028(2) 0.0051(19) S4 0.0774(16) 0.0613(15) 0.0577(13) -0.0017(11) 0.0156(11) 0.0087(12) C1 0.074(3) 0.071(3) 0.056(2) -0.005(2) 0.014(2) -0.005(2) C2 0.074(3) 0.071(3) 0.057(2) -0.003(2) 0.016(2) 0.001(2) C3 0.103(2) 0.089(2) 0.064(2) 0.0009(14) 0.0217(18) 0.0017(16) C4 0.103(2) 0.089(2) 0.064(2) 0.0009(14) 0.0217(18) 0.0017(16) C5 0.072(3) 0.081(3) 0.054(2) -0.004(2) 0.016(2) 0.001(2) C6 0.0673(15) 0.0846(15) 0.0524(13) 0.0010(11) 0.0209(10) 0.0040(13) C7 0.0673(15) 0.0846(15) 0.0524(13) 0.0010(11) 0.0209(10) 0.0040(13) C8 0.079(3) 0.080(3) 0.053(2) -0.010(2) 0.018(2) -0.002(3) C9 0.073(3) 0.073(3) 0.061(3) -0.006(2) 0.018(2) -0.004(2) C10 0.073(3) 0.073(3) 0.062(3) -0.004(2) 0.019(2) 0.003(2) C11 0.089(3) 0.091(2) 0.096(2) -0.0088(15) 0.028(2) 0.0051(19) C12 0.089(3) 0.091(2) 0.096(2) -0.0088(15) 0.028(2) 0.0051(19) C13 0.074(3) 0.069(3) 0.065(3) -0.005(2) 0.016(2) 0.004(2) C14 0.0774(16) 0.0613(15) 0.0577(13) -0.0017(11) 0.0156(11) 0.0087(12) C15 0.0774(16) 0.0613(15) 0.0577(13) -0.0017(11) 0.0156(11) 0.0087(12) C16 0.079(3) 0.068(3) 0.058(3) -0.006(2) 0.016(2) -0.003(2) C17 0.113(5) 0.233(9) 0.071(4) 0.029(5) 0.028(3) -0.051(6) C18 0.152(6) 0.088(4) 0.113(5) -0.007(3) 0.071(4) -0.024(4) C19 0.095(4) 0.123(5) 0.091(4) 0.014(3) 0.027(3) -0.008(4) C20 0.163(6) 0.107(5) 0.114(5) -0.001(4) 0.064(5) -0.028(5) C21 0.111(5) 0.155(6) 0.083(4) 0.026(4) 0.024(3) -0.016(5) C22 0.144(6) 0.116(5) 0.106(5) 0.007(4) 0.036(4) -0.032(5) C23 0.094(4) 0.095(4) 0.180(8) -0.036(4) -0.001(4) 0.022(4) C24 0.084(3) 0.089(4) 0.092(4) 0.000(3) 0.022(3) 0.010(3) C25 0.105(4) 0.109(5) 0.112(5) 0.014(4) 0.038(4) 0.023(4) C26 0.116(5) 0.219(9) 0.095(5) 0.044(5) 0.038(4) 0.067(6) C27 0.162(8) 0.340(15) 0.104(6) 0.061(8) 0.059(6) 0.148(9) C28 0.245(12) 0.323(16) 0.136(8) 0.084(10) 0.098(9) 0.151(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C8 1.371(6) . yes N1 C1 1.382(6) . yes N2 C9 1.322(6) . yes N2 C8 1.324(6) . yes N3 C9 1.371(6) . yes N3 C16 1.383(6) . yes N4 C1 1.307(6) 3_656 yes N4 C16 1.341(5) . yes S1 C2 1.700(5) . yes S1 C3 1.734(11) . yes S2 C5 1.696(5) . yes S2 C6 1.735(10) . yes S3 C10 1.696(6) . yes S3 C11 1.733(11) . yes S4 C13 1.687(6) . yes S4 C14 1.738(9) . yes C1 N4 1.307(6) 3_656 yes C1 C2 1.441(6) . yes C2 C5 1.360(6) . yes C2 C7 1.383(13) . yes C3 C4 1.385(17) . yes C3 C17 1.508(16) . yes C4 C5 1.466(14) . yes C5 C8 1.438(6) . yes C6 C7 1.380(15) . yes C6 C17 1.491(12) . yes C9 C10 1.446(7) . yes C10 C13 1.357(6) . yes C10 C15 1.377(13) . yes C11 C12 1.379(17) . yes C11 C23 1.537(15) . yes C12 C13 1.469(16) . yes C13 C16 1.445(6) . yes C14 C15 1.399(15) . yes C14 C23 1.496(13) . yes C17 C18 1.440(9) . yes C18 C19 1.462(8) . yes C19 C20 1.474(9) . yes C20 C21 1.431(9) . yes C21 C22 1.456(10) . yes C23 C24 1.458(9) . yes C24 C25 1.529(8) . yes C25 C26 1.483(10) . yes C26 C27 1.592(12) . yes C27 C28 1.297(13) . yes 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 C8 N1 C1 110.7(4) . . yes C9 N2 C8 123.2(4) . . yes C9 N3 C16 106.7(4) . . yes C1 N4 C16 122.1(4) 3_656 . yes C2 S1 C3 90.3(5) . . yes C5 S2 C6 90.0(4) . . yes C10 S3 C11 90.7(5) . . yes C13 S4 C14 90.7(4) . . yes N4 C1 N1 128.5(4) 3_656 . yes N4 C1 C2 125.4(4) 3_656 . yes N1 C1 C2 106.1(4) . . yes C5 C2 C7 111.1(7) . . yes C5 C2 C1 108.4(4) . . yes C7 C2 C1 139.8(8) . . yes C5 C2 S1 115.0(4) . . yes C7 C2 S1 6.4(8) . . yes C1 C2 S1 136.6(4) . . yes C4 C3 C17 142.4(12) . . yes C4 C3 S1 113.4(12) . . yes C17 C3 S1 103.2(7) . . yes C3 C4 C5 110.1(15) . . yes C2 C5 C8 108.2(4) . . yes C2 C5 C4 111.2(9) . . yes C8 C5 C4 140.5(9) . . yes C2 C5 S2 114.3(4) . . yes C8 C5 S2 137.4(4) . . yes C4 C5 S2 3.4(9) . . yes C7 C6 C17 137.4(11) . . yes C7 C6 S2 110.7(10) . . yes C17 C6 S2 111.8(6) . . yes C6 C7 C2 113.5(13) . . yes N2 C8 N1 128.3(4) . . yes N2 C8 C5 125.1(4) . . yes N1 C8 C5 106.6(4) . . yes N2 C9 N3 128.2(4) . . yes N2 C9 C10 122.2(4) . . yes N3 C9 C10 109.6(4) . . yes C13 C10 C15 112.4(7) . . yes C13 C10 C9 107.2(4) . . yes C15 C10 C9 140.1(8) . . yes C13 C10 S3 113.9(4) . . yes C15 C10 S3 5.5(10) . . yes C9 C10 S3 138.9(4) . . yes C12 C11 C23 145.5(13) . . yes C12 C11 S3 113.9(12) . . yes C23 C11 S3 100.5(7) . . yes C11 C12 C13 109.0(16) . . yes C10 C13 C16 107.0(4) . . yes C10 C13 C12 112.6(9) . . yes C16 C13 C12 140.3(9) . . yes C10 C13 S4 113.8(4) . . yes C16 C13 S4 139.1(4) . . yes C12 C13 S4 1.3(10) . . yes C15 C14 C23 137.5(10) . . yes C15 C14 S4 110.1(9) . . yes C23 C14 S4 112.4(7) . . yes C10 C15 C14 112.8(12) . . yes N4 C16 N3 127.2(4) . . yes N4 C16 C13 123.4(4) . . yes N3 C16 C13 109.4(4) . . yes C18 C17 C6 115.3(7) . . yes C18 C17 C3 117.8(7) . . yes C6 C17 C3 15.0(6) . . yes C17 C18 C19 122.6(6) . . yes C18 C19 C20 118.8(6) . . yes C21 C20 C19 122.3(7) . . yes C20 C21 C22 119.7(6) . . yes C24 C23 C14 119.2(6) . . yes C24 C23 C11 111.7(7) . . yes C14 C23 C11 16.7(5) . . yes C23 C24 C25 112.6(5) . . yes C26 C25 C24 113.5(6) . . yes C25 C26 C27 110.9(8) . . yes C28 C27 C26 119.1(11) . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 N1 C1 N4 -178.8(4) . . . 3_656 yes C8 N1 C1 C2 0.8(5) . . . . yes N4 C1 C2 C5 178.8(4) 3_656 . . . yes N1 C1 C2 C5 -0.8(5) . . . . yes N4 C1 C2 C7 9.4(15) 3_656 . . . yes N1 C1 C2 C7 -170.2(13) . . . . yes N4 C1 C2 S1 1.1(8) 3_656 . . . yes N1 C1 C2 S1 -178.5(4) . . . . yes C3 S1 C2 C5 0.9(5) . . . . yes C3 S1 C2 C7 55(8) . . . . yes C3 S1 C2 C1 178.5(7) . . . . yes C2 S1 C3 C4 -1.6(11) . . . . yes C2 S1 C3 C17 -172.8(7) . . . . yes C17 C3 C4 C5 167.7(14) . . . . yes S1 C3 C4 C5 1.8(17) . . . . yes C7 C2 C5 C8 173.2(9) . . . . yes C1 C2 C5 C8 0.5(5) . . . . yes S1 C2 C5 C8 178.8(4) . . . . yes C7 C2 C5 C4 -5.6(13) . . . . yes C1 C2 C5 C4 -178.3(10) . . . . yes S1 C2 C5 C4 0.0(11) . . . . yes C7 C2 C5 S2 -4.0(10) . . . . yes C1 C2 C5 S2 -176.7(4) . . . . yes S1 C2 C5 S2 1.5(5) . . . . yes C3 C4 C5 C2 -1.2(17) . . . . yes C3 C4 C5 C8 -179.3(7) . . . . yes C3 C4 C5 S2 -157(19) . . . . yes C6 S2 C5 C2 0.9(5) . . . . yes C6 S2 C5 C8 -175.2(6) . . . . yes C6 S2 C5 C4 26(17) . . . . yes C5 S2 C6 C7 2.4(9) . . . . yes C5 S2 C6 C17 179.3(7) . . . . yes C17 C6 C7 C2 179.0(11) . . . . yes S2 C6 C7 C2 -5.2(15) . . . . yes C5 C2 C7 C6 5.9(15) . . . . yes C1 C2 C7 C6 175.1(7) . . . . yes S1 C2 C7 C6 -122(8) . . . . yes C9 N2 C8 N1 -0.9(8) . . . . yes C9 N2 C8 C5 175.6(4) . . . . yes C1 N1 C8 N2 176.5(4) . . . . yes C1 N1 C8 C5 -0.5(5) . . . . yes C2 C5 C8 N2 -177.1(4) . . . . yes C4 C5 C8 N2 1.1(16) . . . . yes S2 C5 C8 N2 -0.8(8) . . . . yes C2 C5 C8 N1 0.0(5) . . . . yes C4 C5 C8 N1 178.1(14) . . . . yes S2 C5 C8 N1 176.2(5) . . . . yes C8 N2 C9 N3 -0.9(8) . . . . yes C8 N2 C9 C10 -179.5(4) . . . . yes C16 N3 C9 N2 -179.5(5) . . . . yes C16 N3 C9 C10 -0.8(5) . . . . yes N2 C9 C10 C13 -179.4(4) . . . . yes N3 C9 C10 C13 1.8(5) . . . . yes N2 C9 C10 C15 -6.9(16) . . . . yes N3 C9 C10 C15 174.3(14) . . . . yes N2 C9 C10 S3 1.4(9) . . . . yes N3 C9 C10 S3 -177.5(5) . . . . yes C11 S3 C10 C13 1.0(5) . . . . yes C11 S3 C10 C15 -74(9) . . . . yes C11 S3 C10 C9 -179.8(7) . . . . yes C10 S3 C11 C12 -0.8(9) . . . . yes C10 S3 C11 C23 175.4(7) . . . . yes C23 C11 C12 C13 -172.9(14) . . . . yes S3 C11 C12 C13 0.4(15) . . . . yes C15 C10 C13 C16 -176.8(10) . . . . yes C9 C10 C13 C16 -2.0(5) . . . . yes S3 C10 C13 C16 177.4(4) . . . . yes C15 C10 C13 C12 4.8(13) . . . . yes C9 C10 C13 C12 179.6(10) . . . . yes S3 C10 C13 C12 -0.9(11) . . . . yes C15 C10 C13 S4 4.2(11) . . . . yes C9 C10 C13 S4 179.0(4) . . . . yes S3 C10 C13 S4 -1.5(5) . . . . yes C11 C12 C13 C10 0.3(15) . . . . yes C11 C12 C13 C16 -177.3(7) . . . . yes C14 S4 C13 C10 -2.2(5) . . . . yes C14 S4 C13 C16 179.4(7) . . . . yes C13 S4 C14 C15 -0.4(10) . . . . yes C13 S4 C14 C23 178.8(7) . . . . yes C13 C10 C15 C14 -4.5(18) . . . . yes C9 C10 C15 C14 -176.7(7) . . . . yes S3 C10 C15 C14 102(9) . . . . yes C23 C14 C15 C10 -176.1(11) . . . . yes S4 C14 C15 C10 2.8(17) . . . . yes C1 N4 C16 N3 -2.1(7) 3_656 . . . yes C1 N4 C16 C13 179.5(4) 3_656 . . . yes C9 N3 C16 N4 -179.1(4) . . . . yes C9 N3 C16 C13 -0.5(5) . . . . yes C10 C13 C16 N4 -179.7(4) . . . . yes C12 C13 C16 N4 -2.1(16) . . . . yes S4 C13 C16 N4 -1.2(8) . . . . yes C10 C13 C16 N3 1.7(5) . . . . yes C12 C13 C16 N3 179.3(14) . . . . yes S4 C13 C16 N3 -179.8(5) . . . . yes C7 C6 C17 C18 89.3(16) . . . . yes S2 C6 C17 C18 -86.5(9) . . . . yes C7 C6 C17 C3 -168(4) . . . . yes S2 C6 C17 C3 17(3) . . . . yes C4 C3 C17 C18 -69(2) . . . . yes S1 C3 C17 C18 98.0(9) . . . . yes C4 C3 C17 C6 -153(4) . . . . yes S1 C3 C17 C6 14(3) . . . . yes C6 C17 C18 C19 -171.2(7) . . . . yes C3 C17 C18 C19 172.2(7) . . . . yes C17 C18 C19 C20 177.0(7) . . . . yes C18 C19 C20 C21 -177.2(7) . . . . yes C19 C20 C21 C22 178.6(7) . . . . yes C15 C14 C23 C24 101.7(18) . . . . yes S4 C14 C23 C24 -77.2(9) . . . . yes C15 C14 C23 C11 169(4) . . . . yes S4 C14 C23 C11 -10(2) . . . . yes C12 C11 C23 C24 -78.1(19) . . . . yes S3 C11 C23 C24 108.1(8) . . . . yes C12 C11 C23 C14 162(4) . . . . yes S3 C11 C23 C14 -12(2) . . . . yes C14 C23 C24 C25 -170.8(7) . . . . yes C11 C23 C24 C25 172.6(7) . . . . yes C23 C24 C25 C26 -176.2(6) . . . . yes C24 C25 C26 C27 176.9(6) . . . . yes C25 C26 C27 C28 -164.3(11) . . . . yes _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.610 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.084 data_C6-CuTPz _audit_creation_method SHELXL-97 _chemical_name_systematic ; C6-CuTPz ; _chemical_name_common C6-CuTPz _chemical_melting_point ? _chemical_formula_moiety 'C48 H56 Cu N8 S4 ' _chemical_formula_sum 'C48 H56 Cu N8 S4' _chemical_formula_weight 936.79 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 'P 1 21/c 1' _symmetry_Int_Tables_number 14 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 17.173(8) _cell_length_b 6.043(3) _cell_length_c 22.627(13) _cell_angle_alpha 90.00 _cell_angle_beta 103.433(18) _cell_angle_gamma 90.00 _cell_volume 2284(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5326 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 100.2 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'violet' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 986 _exptl_absorpt_coefficient_mu 0.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.014 _exptl_absorpt_correction_T_max 0.986 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number 21633 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5199 _diffrn_reflns_av_R_equivalents 0.124 _diffrn_reflns_av_sigmaI/netI 0.3198 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 27.64 _reflns_number_total 5199 _reflns_number_gt 956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.11' _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^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5199 _refine_ls_number_parameters 283 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.2808 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.2012 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 0.658 _refine_ls_restrained_S_all 0.658 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.5287(4) 0.0996(11) 0.4268(2) 0.0851(17) Uani 1 1 d . A . Cu1 Cu 0.5000 0.0000 0.5000 0.0889(5) Uani 1 2 d S . . N2 N 0.6266(4) -0.1836(12) 0.4179(3) 0.0894(18) Uani 1 1 d . A . N3 N 0.5727(3) -0.2451(9) 0.5053(3) 0.0828(17) Uani 1 1 d . A . N4 N 0.5517(4) -0.4343(10) 0.5958(3) 0.0916(19) Uani 1 1 d . . . S1 S 0.5460(6) 0.4944(14) 0.2901(4) 0.1119(18) Uani 0.50 1 d PD A 2 S2 S 0.6517(4) 0.1388(12) 0.2981(3) 0.0857(13) Uani 0.50 1 d PD A 1 S3 S 0.7362(5) -0.6562(10) 0.4649(3) 0.120(2) Uani 0.50 1 d PD A 2 S4 S 0.6934(4) -0.7970(9) 0.5664(2) 0.0779(12) Uani 0.50 1 d PD A 1 C1 C 0.5022(5) 0.2876(15) 0.3950(3) 0.090(2) Uani 1 1 d . . . C2 C 0.5430(5) 0.3092(13) 0.3454(3) 0.088(2) Uani 1 1 d D . . C3 C 0.6193(12) 0.322(3) 0.2739(10) 0.1119(18) Uani 0.50 1 d PD A 2 C4 C 0.6417(16) 0.136(5) 0.3071(12) 0.1119(18) Uani 0.50 1 d PD A 2 H2 H 0.6803 0.0332 0.3027 0.134 Uiso 0.50 1 calc PR A 2 C5 C 0.5925(4) 0.1335(13) 0.3504(3) 0.085(2) Uani 1 1 d D A . C6 C 0.6110(11) 0.385(2) 0.2685(9) 0.0857(13) Uani 0.50 1 d PD A 1 C7 C 0.5535(17) 0.460(4) 0.3002(12) 0.0857(13) Uani 0.50 1 d PD A 1 H3 H 0.5259 0.5927 0.2920 0.103 Uiso 0.50 1 calc PR A 1 C8 C 0.5849(5) -0.0054(16) 0.4011(3) 0.090(2) Uani 1 1 d . . . C9 C 0.6205(5) -0.2974(14) 0.4664(4) 0.088(2) Uani 1 1 d . . . C10 C 0.6668(4) -0.4904(13) 0.4865(3) 0.0846(19) Uani 1 1 d D A . C11 C 0.7329(12) -0.814(3) 0.5284(7) 0.120(2) Uani 0.50 1 d PD A 2 C12 C 0.6865(16) -0.758(4) 0.5653(12) 0.120(2) Uani 0.50 1 d PD A 2 H4 H 0.6813 -0.8289 0.6006 0.144 Uiso 0.50 1 calc PR A 2 C13 C 0.6466(4) -0.5641(13) 0.5385(3) 0.088(2) Uani 1 1 d D . . C14 C 0.7464(9) -0.820(3) 0.5099(6) 0.0779(12) Uani 0.50 1 d PD A 1 C15 C 0.7299(15) -0.616(3) 0.4779(11) 0.0779(12) Uani 0.50 1 d PD A 1 H5 H 0.7612 -0.5687 0.4518 0.094 Uiso 0.50 1 calc PR A 1 C16 C 0.5858(5) -0.4086(13) 0.5484(4) 0.086(2) Uani 1 1 d . A . C17 C 0.6436(6) 0.459(2) 0.2203(4) 0.149(4) Uani 1 1 d . . . H6 H 0.6016 0.5784 0.1977 0.169 Uiso 1 1 d . . . H7 H 0.6519 0.3702 0.1915 0.169 Uiso 1 1 d . . . C18 C 0.7099(7) 0.6069(14) 0.2376(4) 0.133(3) Uani 1 1 d . A . H8 H 0.7062 0.7163 0.2679 0.139 Uiso 1 1 d . . . H9 H 0.7565 0.5102 0.2596 0.139 Uiso 1 1 d . . . C19 C 0.7522(6) 0.7281(17) 0.1973(4) 0.128(3) Uani 1 1 d . . . H10 H 0.7100 0.8295 0.1728 0.129 Uiso 1 1 d . . . H11 H 0.7637 0.6278 0.1672 0.129 Uiso 1 1 d . . . C20 C 0.8235(7) 0.8714(16) 0.2196(4) 0.148(4) Uani 1 1 d . A . H12 H 0.8100 0.9648 0.2498 0.154 Uiso 1 1 d . . . H13 H 0.8638 0.7677 0.2405 0.154 Uiso 1 1 d . . . C21 C 0.8602(6) 0.992(2) 0.1823(4) 0.143(3) Uani 1 1 d . . . H14 H 0.8188 1.1044 0.1593 0.145 Uiso 1 1 d . . . H15 H 0.8737 0.9086 0.1509 0.145 Uiso 1 1 d . . . C22 C 0.9278(7) 1.1376(17) 0.2067(4) 0.153(4) Uani 1 1 d . A . H16 H 0.9467 1.2173 0.1769 0.146 Uiso 1 1 d . . . H17 H 0.9163 1.2357 0.2361 0.146 Uiso 1 1 d . . . H18 H 0.9713 1.0404 0.2275 0.146 Uiso 1 1 d . . . C23 C 0.8020(6) -1.0065(17) 0.5166(5) 0.172(4) Uani 1 1 d . . . H19 H 0.8101 -0.9980 0.4717 0.162 Uiso 1 1 d . . . H20 H 0.7748 -1.1341 0.5174 0.162 Uiso 1 1 d . . . C24 C 0.8785(6) -0.9850(16) 0.5567(3) 0.124(3) Uani 1 1 d . A . H21 H 0.9028 -0.8465 0.5516 0.113 Uiso 1 1 d . . . H22 H 0.8683 -0.9887 0.5965 0.113 Uiso 1 1 d . . . C25 C 0.9369(7) -1.1796(16) 0.5507(5) 0.143(4) Uani 1 1 d . . . H23 H 0.9447 -1.1675 0.5093 0.135 Uiso 1 1 d . . . H24 H 0.9071 -1.3138 0.5517 0.135 Uiso 1 1 d . . . C26 C 1.0138(8) -1.170(2) 0.5965(5) 0.188(5) Uani 1 1 d . A . H25 H 1.0403 -1.0338 0.5927 0.182 Uiso 1 1 d . . . H26 H 1.0002 -1.1629 0.6370 0.182 Uiso 1 1 d . . . C27 C 1.0685(9) -1.368(3) 0.5917(5) 0.285(11) Uani 1 1 d . . . H27 H 1.0813 -1.3664 0.5525 0.232 Uiso 1 1 d . . . H28 H 1.0259 -1.5087 0.5825 0.232 Uiso 1 1 d . . . C28 C 1.1182(11) -1.448(3) 0.6307(7) 0.292(10) Uani 1 1 d . A . H29 H 1.1609 -1.3145 0.6402 0.248 Uiso 1 1 d . . . H30 H 1.1054 -1.4572 0.6702 0.248 Uiso 1 1 d . . . H31 H 1.1496 -1.5644 0.6249 0.248 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 N1 0.089(5) 0.077(5) 0.086(4) 0.006(4) 0.012(4) 0.006(4) Cu1 0.0969(10) 0.0763(9) 0.0951(8) -0.0042(8) 0.0256(7) -0.0013(9) N2 0.090(5) 0.077(5) 0.101(5) -0.012(4) 0.021(4) 0.002(4) N3 0.089(5) 0.069(4) 0.088(4) -0.004(4) 0.016(4) -0.006(4) N4 0.094(5) 0.080(5) 0.101(4) -0.003(4) 0.024(4) 0.003(4) S1 0.130(4) 0.096(4) 0.109(4) 0.001(3) 0.027(3) -0.002(4) S2 0.086(3) 0.087(3) 0.086(3) 0.001(3) 0.025(2) 0.004(3) S3 0.136(4) 0.090(4) 0.139(5) -0.029(4) 0.043(4) 0.004(3) S4 0.085(3) 0.062(3) 0.086(2) -0.010(2) 0.018(2) 0.010(2) C1 0.095(7) 0.093(7) 0.079(5) -0.018(5) 0.015(5) -0.013(6) C2 0.106(6) 0.078(6) 0.085(5) 0.005(4) 0.034(5) 0.006(5) C3 0.130(4) 0.096(4) 0.109(4) 0.001(3) 0.027(3) -0.002(4) C4 0.130(4) 0.096(4) 0.109(4) 0.001(3) 0.027(3) -0.002(4) C5 0.087(6) 0.081(6) 0.091(5) -0.005(5) 0.027(4) 0.001(5) C6 0.086(3) 0.087(3) 0.086(3) 0.001(3) 0.025(2) 0.004(3) C7 0.086(3) 0.087(3) 0.086(3) 0.001(3) 0.025(2) 0.004(3) C8 0.093(6) 0.081(6) 0.097(5) -0.004(6) 0.026(5) -0.011(6) C9 0.091(6) 0.087(7) 0.084(5) -0.011(5) 0.017(5) -0.004(5) C10 0.077(5) 0.062(5) 0.111(5) -0.011(5) 0.015(4) 0.005(5) C11 0.136(4) 0.090(4) 0.139(5) -0.029(4) 0.043(4) 0.004(3) C12 0.136(4) 0.090(4) 0.139(5) -0.029(4) 0.043(4) 0.004(3) C13 0.091(6) 0.087(7) 0.086(5) -0.007(4) 0.017(4) -0.003(5) C14 0.085(3) 0.062(3) 0.086(2) -0.010(2) 0.018(2) 0.010(2) C15 0.085(3) 0.062(3) 0.086(2) -0.010(2) 0.018(2) 0.010(2) C16 0.087(6) 0.067(6) 0.099(6) -0.012(5) 0.009(5) -0.002(5) C17 0.126(8) 0.208(12) 0.113(6) 0.024(7) 0.028(6) -0.047(8) C18 0.197(11) 0.082(6) 0.141(7) -0.006(6) 0.083(8) -0.030(7) C19 0.126(8) 0.128(8) 0.134(7) 0.033(6) 0.037(6) 0.021(7) C20 0.192(11) 0.117(8) 0.156(8) -0.019(7) 0.081(8) -0.064(8) C21 0.116(8) 0.181(10) 0.131(7) 0.041(8) 0.024(6) -0.028(8) C22 0.170(10) 0.144(9) 0.154(8) 0.009(7) 0.058(7) -0.028(8) C23 0.095(7) 0.099(7) 0.287(12) -0.058(9) -0.030(8) 0.011(7) C24 0.137(8) 0.109(7) 0.123(6) 0.007(6) 0.024(6) 0.005(8) C25 0.139(9) 0.116(8) 0.187(9) 0.041(7) 0.068(8) 0.049(8) C26 0.167(11) 0.258(15) 0.149(8) 0.077(9) 0.055(8) 0.091(11) C27 0.232(16) 0.49(3) 0.157(11) 0.140(13) 0.101(11) 0.256(17) C28 0.30(2) 0.39(2) 0.216(14) 0.142(16) 0.123(14) 0.180(19) _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 N1 C1 1.365(9) . yes N1 C8 1.390(9) . yes N1 Cu1 1.932(5) . yes Cu1 N3 1.923(6) 3_656 yes Cu1 N3 1.923(6) . yes Cu1 N1 1.932(5) 3_656 yes N2 C8 1.300(9) . yes N2 C9 1.320(8) . yes N3 C16 1.370(8) . yes N3 C9 1.373(8) . yes N4 C1 1.333(9) 3_656 yes N4 C16 1.345(8) . yes S1 C2 1.687(9) . yes S1 C3 1.738(15) . yes S2 C6 1.714(12) . yes S2 C5 1.731(9) . yes S3 C10 1.714(9) . yes S3 C11 1.736(15) . yes S4 C13 1.669(10) . yes S4 C14 1.738(11) . yes C1 N4 1.333(8) 3_656 yes C1 C2 1.461(9) . yes C2 C5 1.348(9) . yes C2 C7 1.411(18) . yes C3 C4 1.358(18) . yes C3 C17 1.60(3) . yes C4 C5 1.437(17) . yes C5 C8 1.451(9) . yes C6 C17 1.41(2) . yes C6 C7 1.421(19) . yes C9 C10 1.425(9) . yes C10 C15 1.374(16) . yes C10 C13 1.375(8) . yes C11 C12 1.323(18) . yes C11 C23 1.73(2) . yes C12 C13 1.419(18) . yes C13 C16 1.459(9) . yes C14 C15 1.426(18) . yes C14 C23 1.461(17) . yes C17 C18 1.428(11) . yes C18 C19 1.484(11) . yes C19 C20 1.489(11) . yes C20 C21 1.373(10) . yes C21 C22 1.460(12) . yes C23 C24 1.419(11) . yes C24 C25 1.572(11) . yes C25 C26 1.478(14) . yes C26 C27 1.543(17) . yes C27 C28 1.179(14) . yes 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 C1 N1 C8 109.8(7) . . yes C1 N1 Cu1 126.2(5) . . yes C8 N1 Cu1 123.8(5) . . yes N3 Cu1 N3 180.0(2) 3_656 . yes N3 Cu1 N1 90.1(3) 3_656 3_656 yes N3 Cu1 N1 89.9(3) . 3_656 yes N3 Cu1 N1 89.9(3) 3_656 . yes N3 Cu1 N1 90.1(3) . . yes N1 Cu1 N1 179.999(1) 3_656 . yes C8 N2 C9 121.9(7) . . yes C16 N3 C9 105.5(7) . . yes C16 N3 Cu1 126.7(5) . . yes C9 N3 Cu1 127.8(6) . . yes C1 N4 C16 119.7(6) 3_656 . yes C2 S1 C3 84.7(10) . . yes C6 S2 C5 91.9(8) . . yes C10 S3 C11 85.7(9) . . yes C13 S4 C14 94.5(7) . . yes N4 C1 N1 129.0(7) 3_656 . yes N4 C1 C2 122.4(8) 3_656 . yes N1 C1 C2 108.6(7) . . yes C5 C2 C7 112.6(12) . . yes C5 C2 C1 105.6(7) . . yes C7 C2 C1 141.2(13) . . yes C5 C2 S1 117.3(6) . . yes C7 C2 S1 5.6(14) . . yes C1 C2 S1 137.0(7) . . yes C4 C3 C17 139.3(17) . . yes C4 C3 S1 120.4(19) . . yes C17 C3 S1 100.3(11) . . yes C3 C4 C5 104(2) . . yes C2 C5 C4 113.2(13) . . yes C2 C5 C8 110.7(7) . . yes C4 C5 C8 136.1(14) . . yes C2 C5 S2 112.7(6) . . yes C4 C5 S2 0.5(13) . . yes C8 C5 S2 136.5(7) . . yes C17 C6 C7 137.4(15) . . yes C17 C6 S2 112.3(11) . . yes C7 C6 S2 110.2(16) . . yes C2 C7 C6 112(2) . . yes N2 C8 N1 130.2(7) . . yes N2 C8 C5 124.4(8) . . yes N1 C8 C5 105.3(7) . . yes N2 C9 N3 126.1(8) . . yes N2 C9 C10 123.1(8) . . yes N3 C9 C10 110.8(7) . . yes C15 C10 C13 107.9(11) . . yes C15 C10 C9 143.7(11) . . yes C13 C10 C9 107.9(6) . . yes C15 C10 S3 8.9(14) . . yes C13 C10 S3 112.6(7) . . yes C9 C10 S3 139.5(7) . . yes C12 C11 C23 143.7(16) . . yes C12 C11 S3 121.5(18) . . yes C23 C11 S3 94.9(11) . . yes C11 C12 C13 104(2) . . yes C10 C13 C12 116.1(13) . . yes C10 C13 C16 104.7(7) . . yes C12 C13 C16 139.2(14) . . yes C10 C13 S4 113.6(6) . . yes C12 C13 S4 3.0(13) . . yes C16 C13 S4 141.6(7) . . yes C15 C14 C23 140.1(14) . . yes C15 C14 S4 103.1(13) . . yes C23 C14 S4 115.3(11) . . yes C10 C15 C14 118.4(18) . . yes N4 C16 N3 128.4(7) . . yes N4 C16 C13 120.5(8) . . yes N3 C16 C13 111.1(7) . . yes C6 C17 C18 114.9(10) . . yes C6 C17 C3 14.1(9) . . yes C18 C17 C3 116.6(10) . . yes C17 C18 C19 127.8(8) . . yes C18 C19 C20 124.1(8) . . yes C21 C20 C19 123.9(9) . . yes C20 C21 C22 121.6(8) . . yes C24 C23 C14 118.8(10) . . yes C24 C23 C11 114.0(9) . . yes C14 C23 C11 16.4(7) . . yes C23 C24 C25 113.0(9) . . yes C26 C25 C24 113.1(10) . . yes C25 C26 C27 112.2(13) . . yes C28 C27 C26 127.8(16) . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N1 Cu1 N3 3.6(6) . . . 3_656 yes C8 N1 Cu1 N3 178.9(6) . . . 3_656 yes C1 N1 Cu1 N3 -176.4(6) . . . . yes C8 N1 Cu1 N3 -1.1(6) . . . . yes C1 N1 Cu1 N1 -73(15) . . . 3_656 yes C8 N1 Cu1 N1 103(15) . . . 3_656 yes N3 Cu1 N3 C16 -131(7) 3_656 . . . yes N1 Cu1 N3 C16 1.7(5) 3_656 . . . yes N1 Cu1 N3 C16 -178.3(5) . . . . yes N3 Cu1 N3 C9 47(7) 3_656 . . . yes N1 Cu1 N3 C9 179.6(6) 3_656 . . . yes N1 Cu1 N3 C9 -0.4(6) . . . . yes C8 N1 C1 N4 179.6(7) . . . 3_656 yes Cu1 N1 C1 N4 -4.6(11) . . . 3_656 yes C8 N1 C1 C2 0.0(8) . . . . yes Cu1 N1 C1 C2 175.8(4) . . . . yes N4 C1 C2 C5 179.8(7) 3_656 . . . yes N1 C1 C2 C5 -0.5(8) . . . . yes N4 C1 C2 C7 9(3) 3_656 . . . yes N1 C1 C2 C7 -171(2) . . . . yes N4 C1 C2 S1 3.6(13) 3_656 . . . yes N1 C1 C2 S1 -176.7(8) . . . . yes C3 S1 C2 C5 -0.4(8) . . . . yes C3 S1 C2 C7 34(16) . . . . yes C3 S1 C2 C1 175.5(11) . . . . yes C2 S1 C3 C4 -0.2(14) . . . . yes C2 S1 C3 C17 -177.2(12) . . . . yes C17 C3 C4 C5 176(2) . . . . yes S1 C3 C4 C5 1(2) . . . . yes C7 C2 C5 C4 -2(2) . . . . yes C1 C2 C5 C4 -176.2(14) . . . . yes S1 C2 C5 C4 0.9(17) . . . . yes C7 C2 C5 C8 174.6(15) . . . . yes C1 C2 C5 C8 0.9(8) . . . . yes S1 C2 C5 C8 177.9(6) . . . . yes C7 C2 C5 S2 -2.3(17) . . . . yes C1 C2 C5 S2 -176.0(5) . . . . yes S1 C2 C5 S2 1.1(9) . . . . yes C3 C4 C5 C2 -1(2) . . . . yes C3 C4 C5 C8 -177.0(10) . . . . yes C6 S2 C5 C2 0.8(7) . . . . yes C6 S2 C5 C8 -174.9(10) . . . . yes C5 S2 C6 C17 -179.6(12) . . . . yes C5 S2 C6 C7 0.8(13) . . . . yes C5 C2 C7 C6 3(2) . . . . yes C1 C2 C7 C6 173.2(10) . . . . yes S1 C2 C7 C6 -145(18) . . . . yes C17 C6 C7 C2 178(2) . . . . yes S2 C6 C7 C2 -2(2) . . . . yes C9 N2 C8 N1 -0.5(12) . . . . yes C9 N2 C8 C5 176.2(6) . . . . yes C1 N1 C8 N2 177.7(8) . . . . yes Cu1 N1 C8 N2 1.8(11) . . . . yes C1 N1 C8 C5 0.6(8) . . . . yes Cu1 N1 C8 C5 -175.4(4) . . . . yes C2 C5 C8 N2 -178.3(7) . . . . yes C4 C5 C8 N2 -2(2) . . . . yes S2 C5 C8 N2 -2.5(13) . . . . yes C2 C5 C8 N1 -0.9(8) . . . . yes C4 C5 C8 N1 175.2(19) . . . . yes S2 C5 C8 N1 174.9(7) . . . . yes C8 N2 C9 N3 -1.4(11) . . . . yes C8 N2 C9 C10 -178.5(7) . . . . yes C16 N3 C9 N2 180.0(7) . . . . yes Cu1 N3 C9 N2 1.7(10) . . . . yes C16 N3 C9 C10 -2.6(7) . . . . yes Cu1 N3 C9 C10 179.1(4) . . . . yes N2 C9 C10 C15 10(3) . . . . yes N3 C9 C10 C15 -168(2) . . . . yes N2 C9 C10 C13 178.8(6) . . . . yes N3 C9 C10 C13 1.3(8) . . . . yes N2 C9 C10 S3 -3.1(13) . . . . yes N3 C9 C10 S3 179.4(7) . . . . yes C11 S3 C10 C15 59(7) . . . . yes C11 S3 C10 C13 -0.1(7) . . . . yes C11 S3 C10 C9 -178.1(10) . . . . yes C10 S3 C11 C12 -0.8(11) . . . . yes C10 S3 C11 C23 179.8(8) . . . . yes C23 C11 C12 C13 -179.6(17) . . . . yes S3 C11 C12 C13 1.4(18) . . . . yes C15 C10 C13 C12 -7.1(18) . . . . yes C9 C10 C13 C12 179.5(14) . . . . yes S3 C10 C13 C12 0.9(15) . . . . yes C15 C10 C13 C16 173.9(13) . . . . yes C9 C10 C13 C16 0.5(7) . . . . yes S3 C10 C13 C16 -178.1(5) . . . . yes C15 C10 C13 S4 -9.0(15) . . . . yes C9 C10 C13 S4 177.6(5) . . . . yes S3 C10 C13 S4 -1.0(7) . . . . yes C11 C12 C13 C10 -1.4(19) . . . . yes C11 C12 C13 C16 177.2(10) . . . . yes C11 C12 C13 S4 35(25) . . . . yes C14 S4 C13 C10 0.1(7) . . . . yes C14 S4 C13 C12 -144(26) . . . . yes C14 S4 C13 C16 175.6(10) . . . . yes C13 S4 C14 C15 8.3(14) . . . . yes C13 S4 C14 C23 177.4(11) . . . . yes C13 C10 C15 C14 17(3) . . . . yes C9 C10 C15 C14 -173.8(11) . . . . yes S3 C10 C15 C14 -107(8) . . . . yes C23 C14 C15 C10 179.3(15) . . . . yes S4 C14 C15 C10 -16(2) . . . . yes C1 N4 C16 N3 -0.3(11) 3_656 . . . yes C1 N4 C16 C13 178.2(6) 3_656 . . . yes C9 N3 C16 N4 -178.4(7) . . . . yes Cu1 N3 C16 N4 -0.2(10) . . . . yes C9 N3 C16 C13 2.9(7) . . . . yes Cu1 N3 C16 C13 -178.8(4) . . . . yes C10 C13 C16 N4 179.1(6) . . . . yes C12 C13 C16 N4 0(2) . . . . yes S4 C13 C16 N4 3.4(13) . . . . yes C10 C13 C16 N3 -2.2(8) . . . . yes C12 C13 C16 N3 179.1(18) . . . . yes S4 C13 C16 N3 -177.9(7) . . . . yes C7 C6 C17 C18 86(2) . . . . yes S2 C6 C17 C18 -93.3(13) . . . . yes C7 C6 C17 C3 -174(7) . . . . yes S2 C6 C17 C3 7(5) . . . . yes C4 C3 C17 C6 -169(7) . . . . yes S1 C3 C17 C6 7(5) . . . . yes C4 C3 C17 C18 -82(3) . . . . yes S1 C3 C17 C18 93.9(12) . . . . yes C6 C17 C18 C19 -174.1(10) . . . . yes C3 C17 C18 C19 170.4(10) . . . . yes C17 C18 C19 C20 -177.2(10) . . . . yes C18 C19 C20 C21 -176.8(9) . . . . yes C19 C20 C21 C22 177.1(10) . . . . yes C15 C14 C23 C24 82(3) . . . . yes S4 C14 C23 C24 -81.4(14) . . . . yes C15 C14 C23 C11 159(5) . . . . yes S4 C14 C23 C11 -4(3) . . . . yes C12 C11 C23 C24 -74(2) . . . . yes S3 C11 C23 C24 105.3(11) . . . . yes C12 C11 C23 C14 175(5) . . . . yes S3 C11 C23 C14 -6(3) . . . . yes C14 C23 C24 C25 -169.8(9) . . . . yes C11 C23 C24 C25 172.6(8) . . . . yes C23 C24 C25 C26 -174.3(9) . . . . yes C24 C25 C26 C27 177.3(8) . . . . yes C25 C26 C27 C28 -153(2) . . . . yes _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.64 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.254 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.055 # END