# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Karsten Gloe' _publ_contact_author_email KARSTEN.GLOE@CHEMIE.TU-DRESDEN.DE _publ_section_title ; Self-assembly of neutral hexanuclear circular copper(II) meso-helicates: topological control by sulfate ions ; loop_ _publ_author_name 'Karsten Gloe' 'Bernd Buchner' 'Thomas Doert' 'Gerhard Geipel' 'Kerstin Gloe' 'Anne Jager' 'Olga Kataeva' ; H.B.T.Jeazet ; # Attachment 'gloe__CCDC_732800-732802_2.cif' data_62_v2 _database_code_depnum_ccdc_archive 'CCDC 732800' #TrackingRef 'gloe__CCDC_732800-732802_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C144 H108 Cu6 N24 O24 S12 + 24 H2 O' _chemical_formula_sum 'C144 H156 Cu6 N24 O48 S12' _chemical_formula_weight 3756.89 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 trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 23.7647(6) _cell_length_b 23.7647(6) _cell_length_c 25.3824(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12414.5(6) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9904 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.09 _exptl_crystal_description needle _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.51 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5814 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.907 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details 'SADABS version 2.10 (Sheldrick,Bruker AXS Inc.,2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_device 'Bruker Kappa APEX II CCD' _diffrn_measurement_method '0.5 deg, \f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45135 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6315 _reflns_number_gt 4533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2, 1-4 (Bruker AXS, 2005-2007)' _computing_cell_refinement 'APEX2 v2, 1-4 (Bruker AXS, 2005-2007)' _computing_data_reduction 'SAINT NT v6.0 (Bruker AXS, 2003)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997), WinGX (Farrugia 1999), PLATON (Spek 2005)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia 1999), enCIFer (Allen et al. 2004)' _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^)+(0.0736P)^2^+50.5259P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6315 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1578 _refine_ls_wR_factor_gt 0.1382 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.036 _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 Cu1 Cu 0.58682(2) 0.565974(19) 0.148466(16) 0.03039(14) Uani 1 1 d . . . N1 N 0.60943(14) 0.65458(13) 0.12038(12) 0.0331(6) Uani 1 1 d . . . C2 C 0.57683(19) 0.68544(18) 0.13127(15) 0.0389(8) Uani 1 1 d . . . H2 H 0.5435 0.6676 0.1572 0.047 Uiso 1 1 calc R . . C3 C 0.5896(2) 0.74195(19) 0.10641(17) 0.0450(9) Uani 1 1 d . . . H3 H 0.5655 0.7626 0.1152 0.054 Uiso 1 1 calc R . . C4 C 0.6379(2) 0.76862(19) 0.06850(17) 0.0466(10) Uani 1 1 d . . . H4 H 0.6473 0.8077 0.0510 0.056 Uiso 1 1 calc R . . C5 C 0.6721(2) 0.73731(18) 0.05655(16) 0.0427(9) Uani 1 1 d . . . H5 H 0.7053 0.7542 0.0305 0.051 Uiso 1 1 calc R . . C6 C 0.65687(17) 0.68041(16) 0.08362(14) 0.0335(8) Uani 1 1 d . . . C7 C 0.69126(18) 0.64468(17) 0.07302(14) 0.0361(8) Uani 1 1 d . . . H7 H 0.7273 0.6618 0.0496 0.043 Uiso 1 1 calc R . . N8 N 0.67189(14) 0.59031(14) 0.09580(11) 0.0334(6) Uani 1 1 d . . . C9 C 0.70373(16) 0.55428(17) 0.08643(14) 0.0348(8) Uani 1 1 d . . . C10 C 0.73056(18) 0.55314(19) 0.03805(15) 0.0399(8) Uani 1 1 d . . . H10 H 0.7302 0.5792 0.0098 0.048 Uiso 1 1 calc R . . C11 C 0.75768(19) 0.51415(19) 0.03119(16) 0.0421(9) Uani 1 1 d . . . H11 H 0.7763 0.5136 -0.0018 0.051 Uiso 1 1 calc R . . C12 C 0.75780(18) 0.47547(18) 0.07267(16) 0.0397(8) Uani 1 1 d . . . C13 C 0.73216(18) 0.47773(19) 0.12099(16) 0.0420(9) Uani 1 1 d . . . H13 H 0.7333 0.4525 0.1495 0.050 Uiso 1 1 calc R . . C14 C 0.70493(17) 0.51655(18) 0.12776(15) 0.0388(8) Uani 1 1 d . . . H14 H 0.6869 0.5175 0.1609 0.047 Uiso 1 1 calc R . . S15 S 0.78236(6) 0.41698(5) 0.06648(5) 0.0575(3) Uani 1 1 d . . . C16 C 0.44723(18) 0.60633(18) -0.01564(17) 0.0418(9) Uani 1 1 d . . . C17 C 0.50977(17) 0.61619(17) -0.01598(15) 0.0358(8) Uani 1 1 d . . . H17 H 0.5395 0.6431 -0.0423 0.043 Uiso 1 1 calc R . . C18 C 0.52935(16) 0.58773(16) 0.02107(13) 0.0305(7) Uani 1 1 d . . . H18 H 0.5723 0.5946 0.0201 0.037 Uiso 1 1 calc R . . C19 C 0.48632(16) 0.54873(16) 0.06015(14) 0.0322(7) Uani 1 1 d . . . C20 C 0.42365(19) 0.5388(2) 0.06135(18) 0.0488(10) Uani 1 1 d . . . H20 H 0.3942 0.5123 0.0880 0.059 Uiso 1 1 calc R . . C21 C 0.40435(19) 0.5675(2) 0.0237(2) 0.0523(11) Uani 1 1 d . . . H21 H 0.3614 0.5607 0.0245 0.063 Uiso 1 1 calc R . . N22 N 0.50767(14) 0.52047(14) 0.09888(11) 0.0316(6) Uani 1 1 d . . . C23 C 0.47096(18) 0.46004(17) 0.10960(15) 0.0367(8) Uani 1 1 d . . . H23 H 0.4309 0.4348 0.0916 0.044 Uiso 1 1 calc R . . C24 C 0.49186(19) 0.43092(17) 0.14970(14) 0.0372(8) Uani 1 1 d . . . N25 N 0.54756(15) 0.47323(14) 0.17430(11) 0.0345(7) Uani 1 1 d . . . C26 C 0.5700(2) 0.45075(19) 0.21206(15) 0.0401(9) Uani 1 1 d . . . H26 H 0.6090 0.4800 0.2299 0.048 Uiso 1 1 calc R . . C27 C 0.5376(2) 0.3850(2) 0.22609(17) 0.0494(10) Uani 1 1 d . . . H27 H 0.5548 0.3700 0.2528 0.059 Uiso 1 1 calc R . . C28 C 0.4809(2) 0.3424(2) 0.20122(18) 0.0522(11) Uani 1 1 d . . . H28 H 0.4581 0.2977 0.2107 0.063 Uiso 1 1 calc R . . C29 C 0.4575(2) 0.36568(19) 0.16187(17) 0.0466(10) Uani 1 1 d . . . H29 H 0.4185 0.3373 0.1437 0.056 Uiso 1 1 calc R . . S1 S 0.61338(5) 0.61403(4) 0.25714(4) 0.0423(3) Uani 1 1 d . . . O1 O 0.64513(13) 0.60183(13) 0.20981(10) 0.0426(6) Uani 1 1 d . . . O2 O 0.59851(18) 0.56259(14) 0.29587(12) 0.0624(9) Uani 1 1 d . . . O3 O 0.55359(15) 0.61078(15) 0.23824(13) 0.0587(8) Uani 1 1 d . . . O4 O 0.65755(18) 0.67673(13) 0.27901(12) 0.0615(9) Uani 1 1 d . . . O1W O 0.3284(3) 0.2053(3) 0.1224(3) 0.147(2) Uiso 1 1 d . . . O2W O 0.5312(4) 0.0772(4) 0.3736(3) 0.112(2) Uiso 0.70 1 d P . . O3W O 0.5435(8) 0.2531(8) 0.2888(7) 0.138(5) Uiso 0.45 1 d P . . O4W O 0.6667 0.3333 0.2360(9) 0.134(7) Uiso 0.51 3 d SP . . O5W O 0.4957(7) 0.1751(7) 0.3072(6) 0.126(4) Uiso 0.40 1 d P . . O6W O 0.3333 0.6667 0.0710(11) 0.128(9) Uiso 0.38 3 d SP . . O7W O 0.5212(8) 0.1399(8) 0.3374(6) 0.102(5) Uiso 0.30 1 d P . . O8W O 0.3333 0.6667 0.1667 0.12(2) Uiso 0.21 6 d SP . . O9W O 0.4415(13) 0.7371(13) 0.1334(10) 0.141(8) Uiso 0.25 1 d P . . O10W O 0.4437(13) 0.1708(13) 0.2758(10) 0.138(8) Uiso 0.25 1 d P . . O12W O 0.5687(10) 0.2779(10) 0.3124(8) 0.121(6) Uiso 0.32 1 d P . . 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 0.0348(2) 0.0294(2) 0.0252(2) 0.00043(16) 0.00270(17) 0.01474(18) N1 0.0381(16) 0.0288(14) 0.0287(15) -0.0044(12) -0.0037(13) 0.0140(13) C2 0.042(2) 0.040(2) 0.035(2) -0.0088(16) -0.0037(16) 0.0212(17) C3 0.053(2) 0.039(2) 0.046(2) -0.0106(18) -0.0123(19) 0.0252(19) C4 0.061(3) 0.0329(19) 0.042(2) -0.0037(17) -0.014(2) 0.0206(19) C5 0.048(2) 0.0344(19) 0.036(2) 0.0022(16) -0.0040(17) 0.0126(17) C6 0.0367(18) 0.0297(17) 0.0293(18) -0.0024(14) -0.0042(15) 0.0130(15) C7 0.0353(18) 0.0385(19) 0.0283(18) 0.0024(15) 0.0039(15) 0.0138(16) N8 0.0344(15) 0.0377(16) 0.0269(15) 0.0009(13) 0.0008(12) 0.0173(13) C9 0.0278(17) 0.0376(19) 0.0344(19) 0.0015(15) 0.0022(14) 0.0129(15) C10 0.044(2) 0.045(2) 0.0324(19) 0.0087(16) 0.0059(16) 0.0235(18) C11 0.043(2) 0.048(2) 0.038(2) 0.0033(17) 0.0095(17) 0.0243(18) C12 0.0316(18) 0.0377(19) 0.048(2) 0.0088(17) 0.0051(16) 0.0160(16) C13 0.0340(19) 0.045(2) 0.042(2) 0.0150(17) 0.0062(16) 0.0158(17) C14 0.0333(18) 0.044(2) 0.034(2) 0.0073(16) 0.0040(15) 0.0164(16) S15 0.0571(7) 0.0432(6) 0.0774(8) 0.0246(6) 0.0289(6) 0.0290(5) C16 0.0368(19) 0.0318(18) 0.053(2) -0.0031(17) -0.0114(18) 0.0141(16) C17 0.0357(18) 0.0295(17) 0.036(2) -0.0016(15) -0.0013(15) 0.0114(15) C18 0.0304(16) 0.0294(17) 0.0272(17) -0.0041(14) -0.0004(14) 0.0116(14) C19 0.0311(17) 0.0313(17) 0.0307(18) -0.0043(14) -0.0014(14) 0.0129(14) C20 0.035(2) 0.049(2) 0.055(3) 0.011(2) 0.0127(18) 0.0150(18) C21 0.0292(19) 0.051(2) 0.074(3) 0.009(2) 0.000(2) 0.0182(18) N22 0.0326(15) 0.0317(15) 0.0269(15) -0.0002(12) 0.0040(12) 0.0134(12) C23 0.0354(18) 0.0349(18) 0.0334(19) -0.0033(15) 0.0050(15) 0.0127(15) C24 0.046(2) 0.0345(18) 0.0290(18) 0.0020(15) 0.0112(16) 0.0182(16) N25 0.0414(16) 0.0362(16) 0.0280(15) 0.0025(13) 0.0086(13) 0.0210(14) C26 0.050(2) 0.043(2) 0.034(2) 0.0045(16) 0.0093(17) 0.0285(18) C27 0.065(3) 0.052(2) 0.042(2) 0.015(2) 0.015(2) 0.038(2) C28 0.070(3) 0.040(2) 0.048(3) 0.0129(19) 0.021(2) 0.029(2) C29 0.053(2) 0.036(2) 0.042(2) 0.0036(17) 0.0131(19) 0.0155(18) S1 0.0593(6) 0.0304(4) 0.0252(5) -0.0023(3) 0.0016(4) 0.0134(4) O1 0.0455(15) 0.0458(15) 0.0304(14) 0.0018(12) 0.0004(11) 0.0182(12) O2 0.106(3) 0.0387(15) 0.0315(15) 0.0037(12) 0.0118(16) 0.0277(17) O3 0.0577(19) 0.0604(19) 0.0518(19) -0.0028(15) 0.0124(15) 0.0248(16) O4 0.092(2) 0.0331(15) 0.0409(17) -0.0068(13) -0.0127(16) 0.0178(16) _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 O1 1.972(3) . ? Cu1 N25 2.025(3) . ? Cu1 N1 2.025(3) . ? Cu1 N22 2.063(3) . ? Cu1 N8 2.245(3) . ? N1 C2 1.335(5) . ? N1 C6 1.351(5) . ? C2 C3 1.373(6) . ? C2 H2 0.9500 . ? C3 C4 1.384(6) . ? C3 H3 0.9500 . ? C4 C5 1.383(6) . ? C4 H4 0.9500 . ? C5 C6 1.394(5) . ? C5 H5 0.9500 . ? C6 C7 1.468(5) . ? C7 N8 1.273(5) . ? C7 H7 0.9500 . ? N8 C9 1.418(5) . ? C9 C10 1.390(5) . ? C9 C14 1.390(5) . ? C10 C11 1.379(5) . ? C10 H10 0.9500 . ? C11 C12 1.398(5) . ? C11 H11 0.9500 . ? C12 C13 1.382(6) . ? C12 S15 1.763(4) . ? C13 C14 1.377(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? S15 C16 1.766(4) 12_655 ? C16 C17 1.384(5) . ? C16 C21 1.395(6) . ? C16 S15 1.766(4) 11_565 ? C17 C18 1.369(5) . ? C17 H17 0.9500 . ? C18 C19 1.393(5) . ? C18 H18 0.9500 . ? C19 C20 1.387(5) . ? C19 N22 1.420(5) . ? C20 C21 1.379(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? N22 C23 1.283(4) . ? C23 C24 1.451(5) . ? C23 H23 0.9500 . ? C24 N25 1.350(5) . ? C24 C29 1.378(5) . ? N25 C26 1.332(5) . ? C26 C27 1.399(6) . ? C26 H26 0.9500 . ? C27 C28 1.370(7) . ? C27 H27 0.9500 . ? C28 C29 1.387(6) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? S1 O4 1.437(3) . ? S1 O3 1.465(4) . ? S1 O2 1.468(3) . ? S1 O1 1.522(3) . ? O2W O10W 1.61(3) 18_545 ? O3W O12W 0.84(2) . ? O3W O5W 1.69(2) . ? O5W O10W 1.43(3) . ? O5W O7W 1.47(2) . ? O10W O2W 1.61(3) 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 O1 Cu1 N25 93.23(12) . . ? O1 Cu1 N1 93.72(11) . . ? N25 Cu1 N1 169.77(12) . . ? O1 Cu1 N22 165.34(11) . . ? N25 Cu1 N22 79.86(12) . . ? N1 Cu1 N22 91.64(11) . . ? O1 Cu1 N8 90.63(11) . . ? N25 Cu1 N8 109.79(11) . . ? N1 Cu1 N8 77.63(12) . . ? N22 Cu1 N8 103.85(11) . . ? C2 N1 C6 118.3(3) . . ? C2 N1 Cu1 125.0(3) . . ? C6 N1 Cu1 116.3(2) . . ? N1 C2 C3 122.4(4) . . ? N1 C2 H2 118.8 . . ? C3 C2 H2 118.8 . . ? C2 C3 C4 119.7(4) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 118.8(4) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 118.4(4) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? N1 C6 C5 122.3(3) . . ? N1 C6 C7 116.3(3) . . ? C5 C6 C7 121.4(3) . . ? N8 C7 C6 118.7(3) . . ? N8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 N8 C9 120.3(3) . . ? C7 N8 Cu1 110.7(2) . . ? C9 N8 Cu1 128.9(2) . . ? C10 C9 C14 119.8(3) . . ? C10 C9 N8 123.3(3) . . ? C14 C9 N8 116.9(3) . . ? C11 C10 C9 119.8(4) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 120.1(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 119.8(4) . . ? C13 C12 S15 115.8(3) . . ? C11 C12 S15 124.1(3) . . ? C14 C13 C12 120.0(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C9 120.4(4) . . ? C13 C14 H14 119.8 . . ? C9 C14 H14 119.8 . . ? C12 S15 C16 104.37(18) . 12_655 ? C17 C16 C21 118.9(4) . . ? C17 C16 S15 122.6(3) . 11_565 ? C21 C16 S15 118.3(3) . 11_565 ? C18 C17 C16 120.9(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 120.0(3) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 119.9(3) . . ? C20 C19 N22 120.8(3) . . ? C18 C19 N22 119.4(3) . . ? C21 C20 C19 119.7(4) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C16 120.7(4) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C23 N22 C19 118.2(3) . . ? C23 N22 Cu1 112.9(3) . . ? C19 N22 Cu1 128.5(2) . . ? N22 C23 C24 118.6(3) . . ? N22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? N25 C24 C29 122.9(4) . . ? N25 C24 C23 114.3(3) . . ? C29 C24 C23 122.8(4) . . ? C26 N25 C24 118.3(3) . . ? C26 N25 Cu1 127.6(3) . . ? C24 N25 Cu1 114.0(2) . . ? N25 C26 C27 121.5(4) . . ? N25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C28 C27 C26 119.9(4) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 118.6(4) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? C24 C29 C28 118.7(4) . . ? C24 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? O4 S1 O3 111.6(2) . . ? O4 S1 O2 110.58(18) . . ? O3 S1 O2 110.6(2) . . ? O4 S1 O1 109.13(19) . . ? O3 S1 O1 106.98(16) . . ? O2 S1 O1 107.80(17) . . ? S1 O1 Cu1 113.40(16) . . ? O12W O3W O5W 115(2) . . ? O10W O5W O7W 146.9(18) . . ? O10W O5W O3W 90.4(15) . . ? O7W O5W O3W 121.8(13) . . ? O5W O10W O2W 118.5(19) . 17 ? 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 O1 Cu1 N1 C2 -92.6(3) . . . . ? N25 Cu1 N1 C2 40.1(8) . . . . ? N22 Cu1 N1 C2 73.7(3) . . . . ? N8 Cu1 N1 C2 177.5(3) . . . . ? O1 Cu1 N1 C6 94.7(3) . . . . ? N25 Cu1 N1 C6 -132.6(6) . . . . ? N22 Cu1 N1 C6 -98.9(3) . . . . ? N8 Cu1 N1 C6 4.9(2) . . . . ? C6 N1 C2 C3 0.3(5) . . . . ? Cu1 N1 C2 C3 -172.3(3) . . . . ? N1 C2 C3 C4 0.1(6) . . . . ? C2 C3 C4 C5 0.1(6) . . . . ? C3 C4 C5 C6 -0.6(6) . . . . ? C2 N1 C6 C5 -0.8(5) . . . . ? Cu1 N1 C6 C5 172.4(3) . . . . ? C2 N1 C6 C7 -180.0(3) . . . . ? Cu1 N1 C6 C7 -6.8(4) . . . . ? C4 C5 C6 N1 0.9(5) . . . . ? C4 C5 C6 C7 -179.9(3) . . . . ? N1 C6 C7 N8 4.8(5) . . . . ? C5 C6 C7 N8 -174.4(3) . . . . ? C6 C7 N8 C9 179.8(3) . . . . ? C6 C7 N8 Cu1 -0.5(4) . . . . ? O1 Cu1 N8 C7 -95.9(3) . . . . ? N25 Cu1 N8 C7 170.4(2) . . . . ? N1 Cu1 N8 C7 -2.3(2) . . . . ? N22 Cu1 N8 C7 86.4(3) . . . . ? O1 Cu1 N8 C9 83.7(3) . . . . ? N25 Cu1 N8 C9 -10.0(3) . . . . ? N1 Cu1 N8 C9 177.4(3) . . . . ? N22 Cu1 N8 C9 -94.0(3) . . . . ? C7 N8 C9 C10 -34.4(5) . . . . ? Cu1 N8 C9 C10 146.0(3) . . . . ? C7 N8 C9 C14 148.4(4) . . . . ? Cu1 N8 C9 C14 -31.2(4) . . . . ? C14 C9 C10 C11 0.6(6) . . . . ? N8 C9 C10 C11 -176.5(3) . . . . ? C9 C10 C11 C12 0.5(6) . . . . ? C10 C11 C12 C13 -1.7(6) . . . . ? C10 C11 C12 S15 172.4(3) . . . . ? C11 C12 C13 C14 1.8(6) . . . . ? S15 C12 C13 C14 -172.7(3) . . . . ? C12 C13 C14 C9 -0.8(6) . . . . ? C10 C9 C14 C13 -0.4(6) . . . . ? N8 C9 C14 C13 176.9(3) . . . . ? C13 C12 S15 C16 -156.1(3) . . . 12_655 ? C11 C12 S15 C16 29.6(4) . . . 12_655 ? C21 C16 C17 C18 0.9(6) . . . . ? S15 C16 C17 C18 -173.0(3) 11_565 . . . ? C16 C17 C18 C19 -0.6(5) . . . . ? C17 C18 C19 C20 0.1(5) . . . . ? C17 C18 C19 N22 -178.9(3) . . . . ? C18 C19 C20 C21 0.2(6) . . . . ? N22 C19 C20 C21 179.1(4) . . . . ? C19 C20 C21 C16 0.1(7) . . . . ? C17 C16 C21 C20 -0.6(7) . . . . ? S15 C16 C21 C20 173.5(4) 11_565 . . . ? C20 C19 N22 C23 47.8(5) . . . . ? C18 C19 N22 C23 -133.2(3) . . . . ? C20 C19 N22 Cu1 -124.1(3) . . . . ? C18 C19 N22 Cu1 54.8(4) . . . . ? O1 Cu1 N22 C23 -58.3(6) . . . . ? N25 Cu1 N22 C23 4.4(2) . . . . ? N1 Cu1 N22 C23 -169.8(3) . . . . ? N8 Cu1 N22 C23 112.5(2) . . . . ? O1 Cu1 N22 C19 114.0(5) . . . . ? N25 Cu1 N22 C19 176.7(3) . . . . ? N1 Cu1 N22 C19 2.5(3) . . . . ? N8 Cu1 N22 C19 -75.2(3) . . . . ? C19 N22 C23 C24 -179.1(3) . . . . ? Cu1 N22 C23 C24 -5.9(4) . . . . ? N22 C23 C24 N25 4.1(5) . . . . ? N22 C23 C24 C29 -176.4(3) . . . . ? C29 C24 N25 C26 -0.1(5) . . . . ? C23 C24 N25 C26 179.4(3) . . . . ? C29 C24 N25 Cu1 -179.5(3) . . . . ? C23 C24 N25 Cu1 0.0(4) . . . . ? O1 Cu1 N25 C26 -14.6(3) . . . . ? N1 Cu1 N25 C26 -147.4(6) . . . . ? N22 Cu1 N25 C26 178.4(3) . . . . ? N8 Cu1 N25 C26 77.2(3) . . . . ? O1 Cu1 N25 C24 164.7(2) . . . . ? N1 Cu1 N25 C24 32.0(8) . . . . ? N22 Cu1 N25 C24 -2.3(2) . . . . ? N8 Cu1 N25 C24 -103.5(2) . . . . ? C24 N25 C26 C27 0.4(5) . . . . ? Cu1 N25 C26 C27 179.8(3) . . . . ? N25 C26 C27 C28 -0.8(6) . . . . ? C26 C27 C28 C29 0.9(6) . . . . ? N25 C24 C29 C28 0.2(6) . . . . ? C23 C24 C29 C28 -179.3(4) . . . . ? C27 C28 C29 C24 -0.6(6) . . . . ? O4 S1 O1 Cu1 -135.07(18) . . . . ? O3 S1 O1 Cu1 -14.2(2) . . . . ? O2 S1 O1 Cu1 104.8(2) . . . . ? N25 Cu1 O1 S1 -85.43(17) . . . . ? N1 Cu1 O1 S1 87.05(17) . . . . ? N22 Cu1 O1 S1 -24.2(5) . . . . ? N8 Cu1 O1 S1 164.70(17) . . . . ? O12W O3W O5W O10W 144(3) . . . . ? O12W O3W O5W O7W -45(3) . . . . ? O7W O5W O10W O2W 126(3) . . . 17 ? O3W O5W O10W O2W -67.3(19) . . . 17 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.089 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.103 #=======================================================================END # 6. CRYSTALLOGRAPHIC DATA data_shelxl_3 _database_code_depnum_ccdc_archive 'CCDC 732801' #TrackingRef 'gloe__CCDC_732800-732802_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C144 H108 Cu6 N24 O30 S6 + 24 H2 O' _chemical_formula_sum 'C144 H156 Cu6 N24 O54 S6' _chemical_formula_weight 3660.53 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 trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 23.4688(3) _cell_length_b 23.4688(3) _cell_length_c 25.3619(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12097.5(3) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9840 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 31.18 _exptl_crystal_description needle _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.49 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5670 _exptl_absorpt_coefficient_mu 0.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6735 _exptl_absorpt_correction_T_max 0.8330 _exptl_absorpt_process_details 'SADABS version 2.10 (Sheldrick,Bruker AXS Inc.,2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_device 'Bruker Kappa APEX II CCD' _diffrn_measurement_method '0.5 deg frames in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55153 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 31.55 _reflns_number_total 8975 _reflns_number_gt 6296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2, 1-4 (Bruker AXS, 2005-2007)' _computing_cell_refinement 'APEX2 v2, 1-4 (Bruker AXS, 2005-2007)' _computing_data_reduction 'SAINT NT v6.0 (Bruker AXS, 2003)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997), WinGX (Farrugia 1999), PLATON (Spek 2005)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia 1999), enCIFer (Allen et al. 2004)' _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^)+(0.0887P)^2^+2.4209P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8975 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1528 _refine_ls_wR_factor_gt 0.1428 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 0.586817(13) 0.560581(12) 0.146056(10) 0.02143(9) Uani 1 1 d . . . S1 S 0.61416(3) 0.60905(3) 0.25492(2) 0.02520(13) Uani 1 1 d . . . O1 O 0.64524(8) 0.59468(8) 0.20754(6) 0.0286(3) Uani 1 1 d . . . O2 O 0.55446(9) 0.60745(9) 0.23575(7) 0.0359(4) Uani 1 1 d . . . O3 O 0.59750(9) 0.55725(8) 0.29434(7) 0.0350(4) Uani 1 1 d . . . O4 O 0.66172(10) 0.67296(8) 0.27589(7) 0.0376(4) Uani 1 1 d . . . N1 N 0.61280(9) 0.65165(9) 0.11961(7) 0.0236(4) Uani 1 1 d . . . C2 C 0.58178(12) 0.68464(11) 0.13213(10) 0.0281(5) Uani 1 1 d . . . H2 H 0.5479 0.6668 0.1579 0.034 Uiso 1 1 calc R . . C3 C 0.59779(13) 0.74414(12) 0.10844(10) 0.0321(5) Uani 1 1 d . . . H3 H 0.5751 0.7666 0.1180 0.039 Uiso 1 1 calc R . . C4 C 0.64701(13) 0.77052(12) 0.07078(10) 0.0328(5) Uani 1 1 d . . . H4 H 0.6585 0.8111 0.0541 0.039 Uiso 1 1 calc R . . C5 C 0.67912(12) 0.73668(11) 0.05797(10) 0.0297(5) Uani 1 1 d . . . H5 H 0.7132 0.7537 0.0323 0.036 Uiso 1 1 calc R . . C6 C 0.66098(11) 0.67738(11) 0.08306(9) 0.0251(4) Uani 1 1 d . . . C7 C 0.69219(11) 0.63878(11) 0.06978(9) 0.0265(4) Uani 1 1 d . . . H7 H 0.7285 0.6559 0.0462 0.032 Uiso 1 1 calc R . . N8 N 0.67016(9) 0.58157(9) 0.09020(8) 0.0243(4) Uani 1 1 d . . . C9 C 0.69962(11) 0.54363(11) 0.07605(9) 0.0254(4) Uani 1 1 d . . . C10 C 0.69759(12) 0.49849(12) 0.11232(10) 0.0306(5) Uani 1 1 d . . . H10 H 0.6765 0.4937 0.1453 0.037 Uiso 1 1 calc R . . C11 C 0.72584(12) 0.46034(13) 0.10126(11) 0.0337(5) Uani 1 1 d . . . H11 H 0.7242 0.4294 0.1263 0.040 Uiso 1 1 calc R . . C12 C 0.75631(13) 0.46805(12) 0.05337(11) 0.0349(6) Uani 1 1 d . . . C13 C 0.75800(13) 0.51186(13) 0.01636(11) 0.0359(6) Uani 1 1 d . . . H13 H 0.7790 0.5162 -0.0166 0.043 Uiso 1 1 calc R . . C14 C 0.72915(13) 0.54954(13) 0.02714(10) 0.0326(5) Uani 1 1 d . . . H14 H 0.7295 0.5792 0.0015 0.039 Uiso 1 1 calc R . . O15 O 0.78180(11) 0.42706(10) 0.04343(9) 0.0499(6) Uani 1 1 d . . . N16 N 0.54630(10) 0.46658(9) 0.17086(8) 0.0246(4) Uani 1 1 d . . . C17 C 0.56895(12) 0.44274(12) 0.20792(10) 0.0309(5) Uani 1 1 d . . . H17 H 0.6079 0.4721 0.2265 0.037 Uiso 1 1 calc R . . C18 C 0.53684(14) 0.37584(13) 0.22020(11) 0.0372(6) Uani 1 1 d . . . H18 H 0.5546 0.3598 0.2461 0.045 Uiso 1 1 calc R . . C19 C 0.47957(15) 0.33326(13) 0.19463(11) 0.0390(6) Uani 1 1 d . . . H19 H 0.4573 0.2876 0.2028 0.047 Uiso 1 1 calc R . . C20 C 0.45437(13) 0.35766(12) 0.15657(10) 0.0336(5) Uani 1 1 d . . . H20 H 0.4146 0.3295 0.1385 0.040 Uiso 1 1 calc R . . C21 C 0.48963(12) 0.42477(11) 0.14617(9) 0.0266(4) Uani 1 1 d . . . C22 C 0.46799(11) 0.45537(11) 0.10710(9) 0.0265(4) Uani 1 1 d . . . H22 H 0.4271 0.4308 0.0893 0.032 Uiso 1 1 calc R . . N23 N 0.50615(9) 0.51674(9) 0.09757(8) 0.0236(4) Uani 1 1 d . . . C24 C 0.48509(11) 0.54789(11) 0.06049(10) 0.0261(4) Uani 1 1 d . . . C25 C 0.52858(11) 0.58742(11) 0.02158(9) 0.0256(4) Uani 1 1 d . . . H25 H 0.5708 0.5913 0.0187 0.031 Uiso 1 1 calc R . . C26 C 0.51029(12) 0.62119(11) -0.01305(10) 0.0306(5) Uani 1 1 d . . . H26 H 0.5400 0.6486 -0.0396 0.037 Uiso 1 1 calc R . . C27 C 0.44901(13) 0.61476(12) -0.00875(11) 0.0368(6) Uani 1 1 d . . . C28 C 0.40493(13) 0.57444(14) 0.02882(14) 0.0481(8) Uani 1 1 d . . . H28 H 0.3624 0.5698 0.0308 0.058 Uiso 1 1 calc R . . C29 C 0.42277(12) 0.54056(14) 0.06377(12) 0.0411(7) Uani 1 1 d . . . H29 H 0.3925 0.5126 0.0897 0.049 Uiso 1 1 calc R . . O1W O 0.6667 0.3333 0.2366(4) 0.075(2) Uiso 0.67 3 d SP . . O2W O 0.6611(3) 0.4878(3) 0.3191(3) 0.0792(16) Uiso 0.50 1 d P . . O3W O 0.6112(3) 0.4593(3) 0.3400(3) 0.0893(19) Uiso 0.50 1 d P . . O4W O 0.8676(4) 0.6815(4) 0.0859(3) 0.095(2) Uiso 0.50 1 d P . . O5W O 0.7112(3) 0.4637(3) 0.2825(3) 0.0828(17) Uiso 0.50 1 d P . . O6W O 0.9113(4) 0.7442(4) 0.1070(3) 0.102(2) Uiso 0.50 1 d P . . O7W O 0.3333 0.6667 0.1667 0.132(9) Uiso 0.42 6 d SP . . O8W O 0.8815(4) 0.6875(4) 0.1330(4) 0.109(2) Uiso 0.50 1 d P . . O9W O 0.6667 0.3333 0.2978(10) 0.129(8) Uiso 0.33 3 d SP . . O10W O 0.5509(8) 0.4579(8) 0.3636(6) 0.129(5) Uiso 0.30 1 d P . . O11W O 0.6667 0.3333 0.2004(8) 0.080(4) Uiso 0.33 3 d SP . . O12W O 0.2734(13) 0.7098(13) 0.1465(10) 0.134(8) Uiso 0.19 1 d P . . 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 0.02456(14) 0.02176(14) 0.01644(14) 0.00092(9) 0.00118(9) 0.01042(10) S1 0.0318(3) 0.0236(2) 0.0167(3) -0.00069(19) 0.0005(2) 0.0113(2) O1 0.0303(8) 0.0382(9) 0.0177(8) -0.0014(7) 0.0000(6) 0.0173(7) O2 0.0325(9) 0.0466(10) 0.0297(10) 0.0043(8) 0.0043(7) 0.0206(8) O3 0.0509(11) 0.0269(8) 0.0233(9) 0.0040(7) 0.0053(8) 0.0166(8) O4 0.0499(11) 0.0239(8) 0.0307(10) -0.0051(7) -0.0083(8) 0.0121(8) N1 0.0283(9) 0.0218(8) 0.0184(9) -0.0020(7) -0.0011(7) 0.0107(7) C2 0.0341(12) 0.0288(11) 0.0225(12) -0.0043(9) -0.0015(9) 0.0166(9) C3 0.0430(13) 0.0293(11) 0.0287(13) -0.0065(9) -0.0069(10) 0.0215(11) C4 0.0463(14) 0.0234(10) 0.0259(13) -0.0019(9) -0.0084(10) 0.0152(10) C5 0.0324(11) 0.0241(10) 0.0240(12) 0.0020(9) -0.0010(9) 0.0077(9) C6 0.0274(10) 0.0233(10) 0.0201(11) -0.0001(8) -0.0016(8) 0.0093(8) C7 0.0240(10) 0.0308(11) 0.0212(11) 0.0027(9) 0.0032(8) 0.0111(9) N8 0.0259(9) 0.0293(9) 0.0181(9) -0.0003(7) 0.0005(7) 0.0142(8) C9 0.0230(10) 0.0309(11) 0.0224(11) 0.0024(8) 0.0036(8) 0.0135(9) C10 0.0295(11) 0.0353(12) 0.0279(13) 0.0091(10) 0.0094(9) 0.0168(10) C11 0.0333(12) 0.0347(12) 0.0357(14) 0.0139(10) 0.0114(10) 0.0188(10) C12 0.0348(12) 0.0329(12) 0.0411(15) 0.0100(11) 0.0136(11) 0.0202(10) C13 0.0441(14) 0.0466(14) 0.0263(13) 0.0094(11) 0.0146(11) 0.0296(12) C14 0.0417(13) 0.0416(13) 0.0215(12) 0.0084(10) 0.0069(10) 0.0261(11) O15 0.0556(12) 0.0411(10) 0.0666(15) 0.0263(10) 0.0378(11) 0.0345(10) N16 0.0295(9) 0.0268(9) 0.0185(9) 0.0030(7) 0.0049(7) 0.0148(8) C17 0.0360(12) 0.0381(13) 0.0243(12) 0.0060(10) 0.0062(9) 0.0227(11) C18 0.0512(15) 0.0386(13) 0.0317(14) 0.0107(11) 0.0070(11) 0.0300(12) C19 0.0519(16) 0.0293(12) 0.0381(15) 0.0094(10) 0.0121(12) 0.0221(12) C20 0.0409(13) 0.0246(11) 0.0295(13) 0.0039(9) 0.0085(10) 0.0119(10) C21 0.0332(11) 0.0263(10) 0.0197(11) 0.0031(8) 0.0057(9) 0.0144(9) C22 0.0293(11) 0.0240(10) 0.0213(11) -0.0003(8) 0.0014(8) 0.0096(9) N23 0.0269(9) 0.0242(8) 0.0174(9) 0.0024(7) 0.0012(7) 0.0110(7) C24 0.0270(10) 0.0228(10) 0.0238(12) 0.0016(8) -0.0031(8) 0.0088(8) C25 0.0286(11) 0.0237(10) 0.0205(11) -0.0013(8) -0.0020(8) 0.0102(8) C26 0.0383(13) 0.0235(10) 0.0232(12) 0.0019(8) -0.0047(9) 0.0103(9) C27 0.0368(13) 0.0243(11) 0.0409(16) 0.0024(10) -0.0156(11) 0.0089(10) C28 0.0271(12) 0.0434(15) 0.069(2) 0.0175(14) -0.0046(13) 0.0136(11) C29 0.0275(12) 0.0421(14) 0.0490(18) 0.0191(13) 0.0065(11) 0.0139(11) _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. Hydrogen atoms at disordered water molecules were not revealed. ; 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 O1 1.9634(17) . ? Cu1 N16 2.0171(19) . ? Cu1 N1 2.0214(18) . ? Cu1 N23 2.0511(19) . ? Cu1 N8 2.2610(19) . ? S1 O4 1.4506(17) . ? S1 O2 1.4655(19) . ? S1 O3 1.4681(18) . ? S1 O1 1.5282(17) . ? N1 C2 1.340(3) . ? N1 C6 1.349(3) . ? C2 C3 1.388(3) . ? C2 H2 0.9500 . ? C3 C4 1.384(4) . ? C3 H3 0.9500 . ? C4 C5 1.380(4) . ? C4 H4 0.9500 . ? C5 C6 1.389(3) . ? C5 H5 0.9500 . ? C6 C7 1.461(3) . ? C7 N8 1.282(3) . ? C7 H7 0.9500 . ? N8 C9 1.419(3) . ? C9 C10 1.386(3) . ? C9 C14 1.393(3) . ? C10 C11 1.383(3) . ? C10 H10 0.9500 . ? C11 C12 1.375(4) . ? C11 H11 0.9500 . ? C12 C13 1.378(4) . ? C12 O15 1.387(3) . ? C13 C14 1.383(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? O15 C27 1.386(3) 12_655 ? N16 C17 1.333(3) . ? N16 C21 1.349(3) . ? C17 C18 1.395(3) . ? C17 H17 0.9500 . ? C18 C19 1.372(4) . ? C18 H18 0.9500 . ? C19 C20 1.396(4) . ? C19 H19 0.9500 . ? C20 C21 1.390(3) . ? C20 H20 0.9500 . ? C21 C22 1.456(3) . ? C22 N23 1.282(3) . ? C22 H22 0.9500 . ? N23 C24 1.423(3) . ? C24 C29 1.387(3) . ? C24 C25 1.389(3) . ? C25 C26 1.387(3) . ? C25 H25 0.9500 . ? C26 C27 1.373(4) . ? C26 H26 0.9500 . ? C27 C28 1.376(4) . ? C27 O15 1.386(3) 11_565 ? C28 C29 1.388(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? O1W O11W 0.918(17) . ? O1W O9W 1.55(3) . ? O2W O3W 1.148(8) . ? O2W O5W 1.796(9) . ? O3W O10W 1.523(17) . ? O4W O8W 1.227(10) . ? O4W O6W 1.413(10) . ? O6W O8W 1.328(10) . ? O9W O9W 1.80(5) 16_655 ? 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 O1 Cu1 N16 92.83(8) . . ? O1 Cu1 N1 93.02(7) . . ? N16 Cu1 N1 171.05(8) . . ? O1 Cu1 N23 164.14(7) . . ? N16 Cu1 N23 79.99(8) . . ? N1 Cu1 N23 92.65(7) . . ? O1 Cu1 N8 93.27(7) . . ? N16 Cu1 N8 108.48(7) . . ? N1 Cu1 N8 77.93(7) . . ? N23 Cu1 N8 102.39(7) . . ? O4 S1 O2 112.31(12) . . ? O4 S1 O3 110.80(11) . . ? O2 S1 O3 110.45(11) . . ? O4 S1 O1 108.12(11) . . ? O2 S1 O1 106.81(10) . . ? O3 S1 O1 108.16(10) . . ? S1 O1 Cu1 113.66(9) . . ? C2 N1 C6 118.7(2) . . ? C2 N1 Cu1 124.66(16) . . ? C6 N1 Cu1 116.33(15) . . ? N1 C2 C3 121.8(2) . . ? N1 C2 H2 119.1 . . ? C3 C2 H2 119.1 . . ? C4 C3 C2 119.6(2) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 118.6(2) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 119.1(2) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? N1 C6 C5 122.1(2) . . ? N1 C6 C7 116.67(19) . . ? C5 C6 C7 121.2(2) . . ? N8 C7 C6 119.4(2) . . ? N8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 N8 C9 119.1(2) . . ? C7 N8 Cu1 109.45(15) . . ? C9 N8 Cu1 131.40(15) . . ? C10 C9 C14 119.5(2) . . ? C10 C9 N8 118.1(2) . . ? C14 C9 N8 122.4(2) . . ? C11 C10 C9 121.1(2) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 118.7(2) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C13 121.3(2) . . ? C11 C12 O15 116.5(2) . . ? C13 C12 O15 122.2(2) . . ? C12 C13 C14 120.1(2) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C9 119.4(2) . . ? C13 C14 H14 120.3 . . ? C9 C14 H14 120.3 . . ? C12 O15 C27 117.9(2) . 12_655 ? C17 N16 C21 118.5(2) . . ? C17 N16 Cu1 127.60(17) . . ? C21 N16 Cu1 113.90(15) . . ? N16 C17 C18 121.7(2) . . ? N16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C19 C18 C17 119.7(2) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 119.3(2) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C21 C20 C19 117.5(3) . . ? C21 C20 H20 121.2 . . ? C19 C20 H20 121.2 . . ? N16 C21 C20 123.2(2) . . ? N16 C21 C22 114.67(19) . . ? C20 C21 C22 122.1(2) . . ? N23 C22 C21 117.5(2) . . ? N23 C22 H22 121.2 . . ? C21 C22 H22 121.2 . . ? C22 N23 C24 118.3(2) . . ? C22 N23 Cu1 113.67(16) . . ? C24 N23 Cu1 127.53(14) . . ? C29 C24 C25 120.2(2) . . ? C29 C24 N23 120.8(2) . . ? C25 C24 N23 119.0(2) . . ? C26 C25 C24 119.8(2) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C27 C26 C25 119.5(2) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 121.1(2) . . ? C26 C27 O15 122.2(3) . 11_565 ? C28 C27 O15 116.7(3) . 11_565 ? C27 C28 C29 119.8(3) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C24 C29 C28 119.5(2) . . ? C24 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? O11W O1W O9W 180.000(7) . . ? O3W O2W O5W 133.9(6) . . ? O2W O3W O10W 149.4(9) . . ? O8W O4W O6W 59.9(6) . . ? O8W O6W O4W 53.1(5) . . ? O4W O8W O6W 67.0(7) . . ? O1W O9W O9W 179.997(2) . 16_655 ? 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 O4 S1 O1 Cu1 -134.24(11) . . . . ? O2 S1 O1 Cu1 -13.16(13) . . . . ? O3 S1 O1 Cu1 105.73(11) . . . . ? N16 Cu1 O1 S1 -87.52(11) . . . . ? N1 Cu1 O1 S1 85.70(11) . . . . ? N23 Cu1 O1 S1 -25.1(3) . . . . ? N8 Cu1 O1 S1 163.77(11) . . . . ? O1 Cu1 N1 C2 -91.17(19) . . . . ? N16 Cu1 N1 C2 39.5(6) . . . . ? N23 Cu1 N1 C2 74.01(19) . . . . ? N8 Cu1 N1 C2 176.1(2) . . . . ? O1 Cu1 N1 C6 95.24(16) . . . . ? N16 Cu1 N1 C6 -134.1(5) . . . . ? N23 Cu1 N1 C6 -99.58(16) . . . . ? N8 Cu1 N1 C6 2.53(16) . . . . ? C6 N1 C2 C3 0.2(3) . . . . ? Cu1 N1 C2 C3 -173.26(18) . . . . ? N1 C2 C3 C4 0.1(4) . . . . ? C2 C3 C4 C5 -0.3(4) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? C2 N1 C6 C5 -0.3(3) . . . . ? Cu1 N1 C6 C5 173.72(17) . . . . ? C2 N1 C6 C7 -178.5(2) . . . . ? Cu1 N1 C6 C7 -4.5(3) . . . . ? C4 C5 C6 N1 0.1(3) . . . . ? C4 C5 C6 C7 178.2(2) . . . . ? N1 C6 C7 N8 4.5(3) . . . . ? C5 C6 C7 N8 -173.7(2) . . . . ? C6 C7 N8 C9 178.4(2) . . . . ? C6 C7 N8 Cu1 -2.2(3) . . . . ? O1 Cu1 N8 C7 -92.51(16) . . . . ? N16 Cu1 N8 C7 173.40(15) . . . . ? N1 Cu1 N8 C7 -0.12(16) . . . . ? N23 Cu1 N8 C7 89.96(16) . . . . ? O1 Cu1 N8 C9 86.9(2) . . . . ? N16 Cu1 N8 C9 -7.2(2) . . . . ? N1 Cu1 N8 C9 179.2(2) . . . . ? N23 Cu1 N8 C9 -90.7(2) . . . . ? C7 N8 C9 C10 152.1(2) . . . . ? Cu1 N8 C9 C10 -27.2(3) . . . . ? C7 N8 C9 C14 -28.9(3) . . . . ? Cu1 N8 C9 C14 151.75(19) . . . . ? C14 C9 C10 C11 1.6(4) . . . . ? N8 C9 C10 C11 -179.4(2) . . . . ? C9 C10 C11 C12 0.1(4) . . . . ? C10 C11 C12 C13 -1.2(4) . . . . ? C10 C11 C12 O15 -177.8(2) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? O15 C12 C13 C14 176.9(3) . . . . ? C12 C13 C14 C9 1.2(4) . . . . ? C10 C9 C14 C13 -2.3(4) . . . . ? N8 C9 C14 C13 178.8(2) . . . . ? C11 C12 O15 C27 -153.5(3) . . . 12_655 ? C13 C12 O15 C27 29.9(4) . . . 12_655 ? O1 Cu1 N16 C17 -15.4(2) . . . . ? N1 Cu1 N16 C17 -146.1(4) . . . . ? N23 Cu1 N16 C17 178.8(2) . . . . ? N8 Cu1 N16 C17 79.0(2) . . . . ? O1 Cu1 N16 C21 164.28(16) . . . . ? N1 Cu1 N16 C21 33.6(6) . . . . ? N23 Cu1 N16 C21 -1.49(15) . . . . ? N8 Cu1 N16 C21 -101.32(16) . . . . ? C21 N16 C17 C18 2.3(3) . . . . ? Cu1 N16 C17 C18 -178.03(18) . . . . ? N16 C17 C18 C19 -1.6(4) . . . . ? C17 C18 C19 C20 0.1(4) . . . . ? C18 C19 C20 C21 0.6(4) . . . . ? C17 N16 C21 C20 -1.6(3) . . . . ? Cu1 N16 C21 C20 178.74(19) . . . . ? C17 N16 C21 C22 178.8(2) . . . . ? Cu1 N16 C21 C22 -0.9(2) . . . . ? C19 C20 C21 N16 0.1(4) . . . . ? C19 C20 C21 C22 179.7(2) . . . . ? N16 C21 C22 N23 4.5(3) . . . . ? C20 C21 C22 N23 -175.1(2) . . . . ? C21 C22 N23 C24 -178.4(2) . . . . ? C21 C22 N23 Cu1 -5.7(3) . . . . ? O1 Cu1 N23 C22 -60.1(3) . . . . ? N16 Cu1 N23 C22 3.98(17) . . . . ? N1 Cu1 N23 C22 -170.89(17) . . . . ? N8 Cu1 N23 C22 110.88(17) . . . . ? O1 Cu1 N23 C24 111.9(3) . . . . ? N16 Cu1 N23 C24 175.9(2) . . . . ? N1 Cu1 N23 C24 1.05(19) . . . . ? N8 Cu1 N23 C24 -77.18(19) . . . . ? C22 N23 C24 C29 49.1(3) . . . . ? Cu1 N23 C24 C29 -122.5(2) . . . . ? C22 N23 C24 C25 -132.6(2) . . . . ? Cu1 N23 C24 C25 55.8(3) . . . . ? C29 C24 C25 C26 1.9(4) . . . . ? N23 C24 C25 C26 -176.3(2) . . . . ? C24 C25 C26 C27 -0.5(4) . . . . ? C25 C26 C27 C28 -1.1(4) . . . . ? C25 C26 C27 O15 -177.5(2) . . . 11_565 ? C26 C27 C28 C29 1.3(5) . . . . ? O15 C27 C28 C29 177.9(3) 11_565 . . . ? C25 C24 C29 C28 -1.8(4) . . . . ? N23 C24 C29 C28 176.5(3) . . . . ? C27 C28 C29 C24 0.2(5) . . . . ? O5W O2W O3W O10W -161.6(15) . . . . ? O11W O1W O9W O9W 0(100) . . . 16_655 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 31.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.890 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.108 #=======================================================================END # 5. CRYSTALLOGRAPHIC DATA data_shelxl_2 _database_code_depnum_ccdc_archive 'CCDC 732802' #TrackingRef 'gloe__CCDC_732800-732802_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C150 H120 Cu6 N24 O24 S6 + 24 H2 O' _chemical_formula_sum 'C150 H168 Cu6 N24 O48 S6' _chemical_formula_weight 3648.68 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 trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 23.6595(2) _cell_length_b 23.6595(2) _cell_length_c 25.3773(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12302.3(2) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9885 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 25.67 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.43 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5670 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7480 _exptl_absorpt_correction_T_max 0.8731 _exptl_absorpt_process_details 'SADABS version 2.10 (Sheldrick,Bruker AXS Inc.,2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_device 'Bruker Kappa APEX II CCD' _diffrn_measurement_method '0.5 deg frames in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71838 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 30.99 _reflns_number_total 8702 _reflns_number_gt 4845 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2, 1-4 (Bruker AXS, 2005-2007)' _computing_cell_refinement 'APEX2 v2, 1-4 (Bruker AXS, 2005-2007)' _computing_data_reduction 'SAINT NT v6.0 (Bruker AXS, 2003)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997), WinGX (Farrugia 1999), PLATON (Spek 2005)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia 1999), enCIFer (Allen et al. 2004)' _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^)+(0.0934P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8702 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1637 _refine_ls_wR_factor_gt 0.1382 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _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 0.898981(16) 0.253718(16) 0.019960(12) 0.02657(11) Uani 1 1 d . . . S1 S 0.94621(4) 0.27860(4) -0.08830(3) 0.03504(19) Uani 1 1 d . . . O1 O 0.93370(11) 0.31095(10) -0.04160(8) 0.0383(5) Uani 1 1 d . . . O2 O 0.94393(12) 0.21918(11) -0.06821(9) 0.0475(6) Uani 1 1 d . . . O3 O 1.00898(11) 0.32390(13) -0.11036(9) 0.0507(6) Uani 1 1 d . . . O4 O 0.89403(11) 0.26187(13) -0.12704(9) 0.0482(6) Uani 1 1 d . . . N1 N 0.80612(11) 0.21405(12) -0.00576(9) 0.0305(5) Uani 1 1 d . . . C2 C 0.78296(16) 0.23707(16) -0.04286(12) 0.0374(7) Uani 1 1 d . . . H2B H 0.8122 0.2765 -0.0604 0.045 Uiso 1 1 calc R . . C3 C 0.71779(17) 0.20535(18) -0.05644(13) 0.0442(8) Uani 1 1 d . . . H3B H 0.7025 0.2234 -0.0824 0.053 Uiso 1 1 calc R . . C4 C 0.67446(17) 0.14672(19) -0.03194(13) 0.0460(8) Uani 1 1 d . . . H4B H 0.6295 0.1242 -0.0410 0.055 Uiso 1 1 calc R . . C5 C 0.69836(15) 0.12176(17) 0.00607(12) 0.0404(7) Uani 1 1 d . . . H5A H 0.6703 0.0817 0.0234 0.049 Uiso 1 1 calc R . . C6 C 0.76427(14) 0.15715(15) 0.01793(11) 0.0324(6) Uani 1 1 d . . . C7 C 0.79414(14) 0.13606(14) 0.05772(11) 0.0312(6) Uani 1 1 d . . . H7A H 0.7694 0.0957 0.0756 0.037 Uiso 1 1 calc R . . N8 N 0.85454(11) 0.17354(11) 0.06780(9) 0.0283(5) Uani 1 1 d . . . C9 C 0.88461(13) 0.15234(14) 0.10594(11) 0.0296(6) Uani 1 1 d . . . C10 C 0.88007(17) 0.09265(16) 0.10114(14) 0.0450(8) Uani 1 1 d . . . H10A H 0.8560 0.0643 0.0730 0.054 Uiso 1 1 calc R . . C11 C 0.91120(18) 0.07372(17) 0.13815(16) 0.0530(9) Uani 1 1 d . . . H11A H 0.9085 0.0325 0.1347 0.064 Uiso 1 1 calc R . . C12 C 0.94568(15) 0.11394(16) 0.17949(13) 0.0393(7) Uani 1 1 d . . . C13 C 0.95019(14) 0.17436(15) 0.18299(12) 0.0346(7) Uani 1 1 d . . . H13A H 0.9748 0.2030 0.2108 0.042 Uiso 1 1 calc R . . C14 C 0.91969(14) 0.19390(14) 0.14702(11) 0.0300(6) Uani 1 1 d . . . H14A H 0.9227 0.2353 0.1503 0.036 Uiso 1 1 calc R . . C15 C 0.97615(16) 0.09177(17) 0.22097(16) 0.0500(9) Uani 1 1 d . . . H15A H 0.9528 0.0862 0.2547 0.060 Uiso 1 1 calc R . . H15B H 0.9694 0.0485 0.2106 0.060 Uiso 1 1 calc R . . N16 N 0.98816(11) 0.27828(12) 0.04828(9) 0.0294(5) Uani 1 1 d . . . C17 C 1.02013(14) 0.24673(15) 0.03690(11) 0.0344(6) Uani 1 1 d . . . H17A H 1.0029 0.2134 0.0109 0.041 Uiso 1 1 calc R . . C18 C 1.07806(16) 0.26147(17) 0.06220(13) 0.0413(7) Uani 1 1 d . . . H18A H 1.1001 0.2385 0.0533 0.050 Uiso 1 1 calc R . . C19 C 1.10346(15) 0.30950(17) 0.10021(13) 0.0403(7) Uani 1 1 d . . . H19A H 1.1430 0.3200 0.1178 0.048 Uiso 1 1 calc R . . C20 C 1.07000(15) 0.34216(16) 0.11229(12) 0.0381(7) Uani 1 1 d . . . H20A H 1.0862 0.3754 0.1384 0.046 Uiso 1 1 calc R . . C21 C 1.01267(14) 0.32548(14) 0.08565(11) 0.0318(6) Uani 1 1 d . . . C22 C 0.97439(15) 0.35697(14) 0.09724(11) 0.0334(6) Uani 1 1 d . . . H22A H 0.9904 0.3924 0.1213 0.040 Uiso 1 1 calc R . . N23 N 0.91938(12) 0.33635(11) 0.07474(9) 0.0300(5) Uani 1 1 d . . . C24 C 0.88179(14) 0.36626(14) 0.08581(11) 0.0307(6) Uani 1 1 d . . . C25 C 0.87948(16) 0.38965(16) 0.13557(12) 0.0388(7) Uani 1 1 d . . . H25A H 0.9040 0.3863 0.1639 0.047 Uiso 1 1 calc R . . C26 C 0.84112(16) 0.41777(16) 0.14334(13) 0.0404(7) Uani 1 1 d . . . H26A H 0.8403 0.4345 0.1772 0.049 Uiso 1 1 calc R . . C27 C 0.80382(15) 0.42233(15) 0.10322(13) 0.0372(7) Uani 1 1 d . . . C28 C 0.80652(15) 0.39850(15) 0.05411(12) 0.0375(7) Uani 1 1 d . . . H28A H 0.7816 0.4014 0.0260 0.045 Uiso 1 1 calc R . . C29 C 0.84480(15) 0.37067(14) 0.04524(12) 0.0361(7) Uani 1 1 d . . . H29A H 0.8459 0.3544 0.0112 0.043 Uiso 1 1 calc R . . O1W O 0.6667 0.3333 -0.0721(4) 0.163(4) Uiso 1 3 d S . . O2W O 0.8017(5) 0.2800(5) -0.1744(4) 0.117(3) Uiso 0.50 1 d P . . O3W O 0.8283(5) 0.3229(5) -0.1561(4) 0.115(3) Uiso 0.50 1 d P . . O4W O 0.5795(5) 0.1983(5) -0.1138(4) 0.118(3) Uiso 0.50 1 d P . . O5W O 0.9911(5) 0.4569(5) -0.0903(4) 0.136(3) Uiso 0.50 1 d P . . O6W O 1.0000 0.0000 0.0000 0.150(9) Uiso 0.50 6 d SP . . O7W O 0.9908(5) 0.4606(5) -0.0427(4) 0.133(3) Uiso 0.50 1 d P . . O8W O 0.7971(8) 0.2237(9) -0.1990(7) 0.157(6) Uiso 0.35 1 d P . . O9W O 1.0000 0.5000 0.0000 0.152(7) Uiso 0.38 2 d SP . . O10W O 0.9315(9) 0.4237(9) -0.0717(7) 0.146(5) Uiso 0.33 1 d P . . O11W O 1.0647(12) 0.1050(11) 0.0209(9) 0.136(8) Uiso 0.22 1 d P . . 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 0.02749(19) 0.02941(19) 0.02167(17) -0.00224(13) -0.00073(13) 0.01336(15) S1 0.0291(4) 0.0454(4) 0.0224(3) 0.0002(3) 0.0018(3) 0.0125(3) O1 0.0434(12) 0.0390(12) 0.0276(11) -0.0001(9) 0.0002(9) 0.0169(10) O2 0.0590(15) 0.0460(13) 0.0373(13) -0.0070(10) -0.0039(11) 0.0260(12) O3 0.0309(12) 0.0734(17) 0.0365(13) 0.0135(12) 0.0049(9) 0.0176(12) O4 0.0330(12) 0.0740(17) 0.0297(12) -0.0059(11) -0.0030(9) 0.0209(12) N1 0.0321(13) 0.0379(13) 0.0239(12) -0.0042(10) -0.0028(9) 0.0194(11) C2 0.0470(18) 0.0425(17) 0.0292(15) -0.0050(13) -0.0042(13) 0.0271(15) C3 0.052(2) 0.057(2) 0.0355(18) -0.0071(15) -0.0114(15) 0.0359(18) C4 0.0359(17) 0.061(2) 0.0416(19) -0.0107(16) -0.0107(14) 0.0242(17) C5 0.0337(16) 0.0459(18) 0.0347(16) -0.0070(14) -0.0034(13) 0.0147(15) C6 0.0291(14) 0.0384(16) 0.0277(14) -0.0062(12) -0.0029(11) 0.0154(13) C7 0.0300(15) 0.0311(15) 0.0280(14) -0.0024(11) 0.0011(11) 0.0120(12) N8 0.0294(12) 0.0301(12) 0.0239(11) -0.0034(9) -0.0030(9) 0.0138(10) C9 0.0247(13) 0.0305(14) 0.0299(14) 0.0020(11) 0.0004(11) 0.0110(12) C10 0.047(2) 0.0317(16) 0.052(2) -0.0104(15) -0.0186(16) 0.0172(15) C11 0.050(2) 0.0318(17) 0.076(3) -0.0017(17) -0.0167(19) 0.0191(16) C12 0.0290(15) 0.0381(17) 0.0470(19) 0.0130(14) -0.0010(13) 0.0138(13) C13 0.0313(15) 0.0395(17) 0.0302(15) 0.0029(12) -0.0010(12) 0.0155(13) C14 0.0304(14) 0.0321(15) 0.0272(14) -0.0017(11) 0.0007(11) 0.0154(12) C15 0.0366(18) 0.044(2) 0.063(2) 0.0200(17) -0.0046(16) 0.0161(16) N16 0.0260(12) 0.0336(13) 0.0246(11) 0.0023(10) 0.0043(9) 0.0120(10) C17 0.0325(15) 0.0405(17) 0.0310(15) 0.0019(13) 0.0071(12) 0.0188(14) C18 0.0374(17) 0.050(2) 0.0414(18) 0.0098(15) 0.0084(14) 0.0258(16) C19 0.0291(15) 0.054(2) 0.0355(16) 0.0088(14) 0.0017(13) 0.0194(15) C20 0.0326(16) 0.0408(17) 0.0304(15) -0.0008(13) -0.0012(12) 0.0105(14) C21 0.0311(15) 0.0324(15) 0.0271(14) 0.0005(11) 0.0010(11) 0.0124(12) C22 0.0376(16) 0.0309(15) 0.0283(14) -0.0022(11) -0.0013(12) 0.0146(13) N23 0.0343(13) 0.0302(12) 0.0247(11) -0.0019(9) -0.0023(10) 0.0154(11) C24 0.0347(15) 0.0294(14) 0.0274(14) -0.0028(11) -0.0017(11) 0.0155(12) C25 0.0488(19) 0.0444(18) 0.0292(15) -0.0093(13) -0.0085(13) 0.0278(16) C26 0.0495(19) 0.0447(18) 0.0331(16) -0.0118(14) -0.0059(14) 0.0281(16) C27 0.0361(16) 0.0327(16) 0.0434(17) -0.0113(13) -0.0106(14) 0.0176(14) C28 0.0415(17) 0.0330(16) 0.0381(17) -0.0072(13) -0.0125(14) 0.0187(14) C29 0.0434(18) 0.0340(16) 0.0282(15) -0.0063(12) -0.0066(13) 0.0174(14) _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 O1 1.959(2) . ? Cu1 N1 2.018(2) . ? Cu1 N16 2.020(2) . ? Cu1 N8 2.045(2) . ? Cu1 N23 2.246(2) . ? S1 O3 1.441(2) . ? S1 O4 1.469(2) . ? S1 O2 1.471(3) . ? S1 O1 1.518(2) . ? N1 C2 1.335(4) . ? N1 C6 1.350(4) . ? C2 C3 1.379(5) . ? C2 H2B 0.9500 . ? C3 C4 1.393(5) . ? C3 H3B 0.9500 . ? C4 C5 1.390(5) . ? C4 H4B 0.9500 . ? C5 C6 1.385(4) . ? C5 H5A 0.9500 . ? C6 C7 1.456(4) . ? C7 N8 1.275(4) . ? C7 H7A 0.9500 . ? N8 C9 1.432(4) . ? C9 C10 1.367(4) . ? C9 C14 1.388(4) . ? C10 C11 1.398(5) . ? C10 H10A 0.9500 . ? C11 C12 1.377(5) . ? C11 H11A 0.9500 . ? C12 C13 1.382(5) . ? C12 C15 1.510(4) . ? C13 C14 1.379(4) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C27 1.510(4) 15_545 ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? N16 C17 1.333(4) . ? N16 C21 1.355(4) . ? C17 C18 1.391(4) . ? C17 H17A 0.9500 . ? C18 C19 1.378(5) . ? C18 H18A 0.9500 . ? C19 C20 1.389(5) . ? C19 H19A 0.9500 . ? C20 C21 1.385(4) . ? C20 H20A 0.9500 . ? C21 C22 1.462(4) . ? C22 N23 1.274(4) . ? C22 H22A 0.9500 . ? N23 C24 1.414(4) . ? C24 C29 1.388(4) . ? C24 C25 1.391(4) . ? C25 C26 1.382(4) . ? C25 H25A 0.9500 . ? C26 C27 1.387(4) . ? C26 H26A 0.9500 . ? C27 C28 1.382(4) . ? C27 C15 1.510(4) 14_565 ? C28 C29 1.379(4) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? O2W O3W 1.002(11) . ? O2W O8W 1.424(18) . ? O5W O7W 1.211(12) . ? O5W O10W 1.312(18) . ? O7W O9W 1.375(11) . ? O7W O10W 1.432(18) . ? O9W O7W 1.375(11) 10_765 ? 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 O1 Cu1 N1 92.65(9) . . ? O1 Cu1 N16 93.91(9) . . ? N1 Cu1 N16 170.64(10) . . ? O1 Cu1 N8 163.33(9) . . ? N1 Cu1 N8 79.94(9) . . ? N16 Cu1 N8 91.96(9) . . ? O1 Cu1 N23 93.36(9) . . ? N1 Cu1 N23 108.37(9) . . ? N16 Cu1 N23 77.90(9) . . ? N8 Cu1 N23 103.12(9) . . ? O3 S1 O4 110.79(14) . . ? O3 S1 O2 112.17(15) . . ? O4 S1 O2 110.50(15) . . ? O3 S1 O1 108.45(14) . . ? O4 S1 O1 107.99(13) . . ? O2 S1 O1 106.75(13) . . ? S1 O1 Cu1 113.21(12) . . ? C2 N1 C6 118.4(3) . . ? C2 N1 Cu1 127.7(2) . . ? C6 N1 Cu1 113.89(19) . . ? N1 C2 C3 122.0(3) . . ? N1 C2 H2B 119.0 . . ? C3 C2 H2B 119.0 . . ? C2 C3 C4 119.8(3) . . ? C2 C3 H3B 120.1 . . ? C4 C3 H3B 120.1 . . ? C5 C4 C3 118.7(3) . . ? C5 C4 H4B 120.7 . . ? C3 C4 H4B 120.7 . . ? C6 C5 C4 117.9(3) . . ? C6 C5 H5A 121.0 . . ? C4 C5 H5A 121.0 . . ? N1 C6 C5 123.3(3) . . ? N1 C6 C7 114.3(2) . . ? C5 C6 C7 122.4(3) . . ? N8 C7 C6 117.9(3) . . ? N8 C7 H7A 121.0 . . ? C6 C7 H7A 121.0 . . ? C7 N8 C9 118.2(2) . . ? C7 N8 Cu1 113.79(19) . . ? C9 N8 Cu1 127.65(18) . . ? C10 C9 C14 120.6(3) . . ? C10 C9 N8 120.4(3) . . ? C14 C9 N8 119.0(3) . . ? C9 C10 C11 119.3(3) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? C12 C11 C10 121.0(3) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 118.5(3) . . ? C11 C12 C15 120.8(3) . . ? C13 C12 C15 120.7(3) . . ? C14 C13 C12 121.4(3) . . ? C14 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C13 C14 C9 119.2(3) . . ? C13 C14 H14A 120.4 . . ? C9 C14 H14A 120.4 . . ? C27 C15 C12 115.1(3) 15_545 . ? C27 C15 H15A 108.5 15_545 . ? C12 C15 H15A 108.5 . . ? C27 C15 H15B 108.5 15_545 . ? C12 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C17 N16 C21 119.0(3) . . ? C17 N16 Cu1 124.4(2) . . ? C21 N16 Cu1 116.18(19) . . ? N16 C17 C18 121.6(3) . . ? N16 C17 H17A 119.2 . . ? C18 C17 H17A 119.2 . . ? C19 C18 C17 119.9(3) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C18 C19 C20 118.6(3) . . ? C18 C19 H19A 120.7 . . ? C20 C19 H19A 120.7 . . ? C21 C20 C19 118.9(3) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? N16 C21 C20 122.1(3) . . ? N16 C21 C22 116.2(3) . . ? C20 C21 C22 121.7(3) . . ? N23 C22 C21 119.3(3) . . ? N23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? C22 N23 C24 119.8(2) . . ? C22 N23 Cu1 110.2(2) . . ? C24 N23 Cu1 130.04(18) . . ? C29 C24 C25 119.4(3) . . ? C29 C24 N23 117.9(3) . . ? C25 C24 N23 122.6(3) . . ? C26 C25 C24 119.2(3) . . ? C26 C25 H25A 120.4 . . ? C24 C25 H25A 120.4 . . ? C25 C26 C27 122.0(3) . . ? C25 C26 H26A 119.0 . . ? C27 C26 H26A 119.0 . . ? C28 C27 C26 118.0(3) . . ? C28 C27 C15 119.8(3) . 14_565 ? C26 C27 C15 122.2(3) . 14_565 ? C29 C28 C27 121.2(3) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? C28 C29 C24 120.3(3) . . ? C28 C29 H29A 119.9 . . ? C24 C29 H29A 119.9 . . ? O3W O2W O8W 150.1(13) . . ? O7W O5W O10W 69.0(10) . . ? O5W O7W O9W 146.3(11) . . ? O5W O7W O10W 58.8(9) . . ? O9W O7W O10W 126.4(11) . . ? O7W O9W O7W 180.0(10) . 10_765 ? O5W O10W O7W 52.2(9) . . ? 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 O3 S1 O1 Cu1 -135.28(14) . . . . ? O4 S1 O1 Cu1 104.60(15) . . . . ? O2 S1 O1 Cu1 -14.23(17) . . . . ? N1 Cu1 O1 S1 -86.01(14) . . . . ? N16 Cu1 O1 S1 87.31(14) . . . . ? N8 Cu1 O1 S1 -23.1(4) . . . . ? N23 Cu1 O1 S1 165.40(13) . . . . ? O1 Cu1 N1 C2 -16.6(3) . . . . ? N16 Cu1 N1 C2 -151.1(5) . . . . ? N8 Cu1 N1 C2 178.4(3) . . . . ? N23 Cu1 N1 C2 77.8(3) . . . . ? O1 Cu1 N1 C6 162.5(2) . . . . ? N16 Cu1 N1 C6 28.0(7) . . . . ? N8 Cu1 N1 C6 -2.5(2) . . . . ? N23 Cu1 N1 C6 -103.1(2) . . . . ? C6 N1 C2 C3 1.7(4) . . . . ? Cu1 N1 C2 C3 -179.3(2) . . . . ? N1 C2 C3 C4 -1.5(5) . . . . ? C2 C3 C4 C5 0.3(5) . . . . ? C3 C4 C5 C6 0.6(5) . . . . ? C2 N1 C6 C5 -0.7(4) . . . . ? Cu1 N1 C6 C5 -179.9(2) . . . . ? C2 N1 C6 C7 179.9(3) . . . . ? Cu1 N1 C6 C7 0.7(3) . . . . ? C4 C5 C6 N1 -0.5(5) . . . . ? C4 C5 C6 C7 178.9(3) . . . . ? N1 C6 C7 N8 2.9(4) . . . . ? C5 C6 C7 N8 -176.5(3) . . . . ? C6 C7 N8 C9 -178.5(2) . . . . ? C6 C7 N8 Cu1 -5.0(3) . . . . ? O1 Cu1 N8 C7 -60.5(4) . . . . ? N1 Cu1 N8 C7 4.1(2) . . . . ? N16 Cu1 N8 C7 -171.2(2) . . . . ? N23 Cu1 N8 C7 110.8(2) . . . . ? O1 Cu1 N8 C9 112.2(3) . . . . ? N1 Cu1 N8 C9 176.8(2) . . . . ? N16 Cu1 N8 C9 1.6(2) . . . . ? N23 Cu1 N8 C9 -76.5(2) . . . . ? C7 N8 C9 C10 53.1(4) . . . . ? Cu1 N8 C9 C10 -119.4(3) . . . . ? C7 N8 C9 C14 -128.4(3) . . . . ? Cu1 N8 C9 C14 59.1(3) . . . . ? C14 C9 C10 C11 0.0(5) . . . . ? N8 C9 C10 C11 178.4(3) . . . . ? C9 C10 C11 C12 0.7(6) . . . . ? C10 C11 C12 C13 -1.5(6) . . . . ? C10 C11 C12 C15 176.7(3) . . . . ? C11 C12 C13 C14 1.7(5) . . . . ? C15 C12 C13 C14 -176.5(3) . . . . ? C12 C13 C14 C9 -1.1(4) . . . . ? C10 C9 C14 C13 0.2(4) . . . . ? N8 C9 C14 C13 -178.3(2) . . . . ? C11 C12 C15 C27 126.2(4) . . . 15_545 ? C13 C12 C15 C27 -55.7(5) . . . 15_545 ? O1 Cu1 N16 C17 -91.1(2) . . . . ? N1 Cu1 N16 C17 43.3(7) . . . . ? N8 Cu1 N16 C17 73.3(2) . . . . ? N23 Cu1 N16 C17 176.3(2) . . . . ? O1 Cu1 N16 C21 96.4(2) . . . . ? N1 Cu1 N16 C21 -129.2(5) . . . . ? N8 Cu1 N16 C21 -99.2(2) . . . . ? N23 Cu1 N16 C21 3.78(19) . . . . ? C21 N16 C17 C18 -0.4(4) . . . . ? Cu1 N16 C17 C18 -172.7(2) . . . . ? N16 C17 C18 C19 0.3(5) . . . . ? C17 C18 C19 C20 0.0(5) . . . . ? C18 C19 C20 C21 -0.2(5) . . . . ? C17 N16 C21 C20 0.2(4) . . . . ? Cu1 N16 C21 C20 173.1(2) . . . . ? C17 N16 C21 C22 -178.4(3) . . . . ? Cu1 N16 C21 C22 -5.5(3) . . . . ? C19 C20 C21 N16 0.1(4) . . . . ? C19 C20 C21 C22 178.7(3) . . . . ? N16 C21 C22 N23 4.3(4) . . . . ? C20 C21 C22 N23 -174.4(3) . . . . ? C21 C22 N23 C24 179.7(2) . . . . ? C21 C22 N23 Cu1 -1.0(3) . . . . ? O1 Cu1 N23 C22 -94.7(2) . . . . ? N1 Cu1 N23 C22 171.3(2) . . . . ? N16 Cu1 N23 C22 -1.5(2) . . . . ? N8 Cu1 N23 C22 87.7(2) . . . . ? O1 Cu1 N23 C24 84.5(2) . . . . ? N1 Cu1 N23 C24 -9.5(3) . . . . ? N16 Cu1 N23 C24 177.7(2) . . . . ? N8 Cu1 N23 C24 -93.1(2) . . . . ? C22 N23 C24 C29 145.6(3) . . . . ? Cu1 N23 C24 C29 -33.6(4) . . . . ? C22 N23 C24 C25 -36.0(4) . . . . ? Cu1 N23 C24 C25 144.9(2) . . . . ? C29 C24 C25 C26 -1.0(5) . . . . ? N23 C24 C25 C26 -179.4(3) . . . . ? C24 C25 C26 C27 1.2(5) . . . . ? C25 C26 C27 C28 -0.9(5) . . . . ? C25 C26 C27 C15 175.9(3) . . . 14_565 ? C26 C27 C28 C29 0.4(5) . . . . ? C15 C27 C28 C29 -176.5(3) 14_565 . . . ? C27 C28 C29 C24 -0.2(5) . . . . ? C25 C24 C29 C28 0.5(5) . . . . ? N23 C24 C29 C28 179.0(3) . . . . ? O10W O5W O7W O9W -110(2) . . . . ? O5W O7W O9W O7W -146(100) . . . 10_765 ? O10W O7W O9W O7W 127(100) . . . 10_765 ? O9W O7W O10W O5W 139.6(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.908 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.096