Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_name 'C. D. Garner' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 _publ_contact_author 'C. D. Garner' _publ_contact_author_email Dave.Garner@nottingham.ac.uk _publ_section_title ; A Phenol-Imidazole Pro-Ligand that can exist as a Phenoxyl Radical, Alone and when Complexed to Copper(II) and Zinc(II) ; loop_ _publ_author_name 'L. Benisvy' 'A. J. Blake' 'D. Collison' 'E. S. Davies' 'C. D. Garner' ; E.J.L.McInnes ; 'J. McMaster' 'G. Whittaker' 'C. Wilson' data_tbolim _database_code_CSD 199488 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common LH.1Me2CO _chemical_melting_point 283 _chemical_formula_moiety 'C29 H32 N2 O, C3 H6 O' _chemical_formula_sum 'C32 H38 N2 O2' _chemical_formula_weight 482.64 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.059(2) _cell_length_b 8.5608(9) _cell_length_c 19.135(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.566(2) _cell_angle_gamma 90.00 _cell_volume 2835.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3439 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 26.1 _exptl_crystal_description Column _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 16919 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.66 _reflns_number_total 6512 _reflns_number_gt 3621 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.0730P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'OH and CH3 from acetone found from difmap, other geometrically placed' _refine_ls_hydrogen_treatment 'OH and CH3 from acetone as rigid rotating group, others riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6512 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1068 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1478 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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 O1 O 0.46963(7) 0.74600(16) 0.18827(6) 0.0303(3) Uani 1 1 d . . . H1 H 0.5044 0.7416 0.1671 0.046 Uiso 1 1 calc R . . C1 C 0.63242(10) 0.7343(2) 0.24215(9) 0.0222(4) Uani 1 1 d . . . N2 N 0.71083(8) 0.74482(16) 0.26237(7) 0.0234(3) Uani 1 1 d . . . H2A H 0.7406 0.7577 0.3072 0.028 Uiso 1 1 calc R . . C3 C 0.73598(10) 0.7320(2) 0.20091(9) 0.0230(4) Uani 1 1 d . . . C4 C 0.66979(9) 0.7153(2) 0.14344(9) 0.0219(4) Uani 1 1 d . . . N5 N 0.60586(8) 0.71657(17) 0.16975(7) 0.0228(3) Uani 1 1 d . . . C6 C 0.81856(10) 0.7381(2) 0.20503(9) 0.0228(4) Uani 1 1 d . . . C7 C 0.86670(10) 0.8483(2) 0.25013(9) 0.0259(4) Uani 1 1 d . . . H7A H 0.8461 0.9183 0.2783 0.031 Uiso 1 1 calc R . . C8 C 0.94461(10) 0.8551(2) 0.25371(10) 0.0304(4) Uani 1 1 d . . . H8A H 0.9769 0.9312 0.2837 0.036 Uiso 1 1 calc R . . C9 C 0.97532(11) 0.7519(2) 0.21395(10) 0.0336(5) Uani 1 1 d . . . H9A H 1.0287 0.7570 0.2168 0.040 Uiso 1 1 calc R . . C10 C 0.92854(11) 0.6410(2) 0.16991(10) 0.0345(5) Uani 1 1 d . . . H10A H 0.9498 0.5695 0.1429 0.041 Uiso 1 1 calc R . . C11 C 0.85034(10) 0.6346(2) 0.16540(10) 0.0292(4) Uani 1 1 d . . . H11A H 0.8183 0.5588 0.1350 0.035 Uiso 1 1 calc R . . C12 C 0.66016(10) 0.7054(2) 0.06435(9) 0.0230(4) Uani 1 1 d . . . C13 C 0.60087(11) 0.6150(2) 0.01996(9) 0.0312(4) Uani 1 1 d . . . H13A H 0.5678 0.5574 0.0412 0.037 Uiso 1 1 calc R . . C14 C 0.58966(12) 0.6082(3) -0.05457(10) 0.0388(5) Uani 1 1 d . . . H14A H 0.5489 0.5466 -0.0841 0.047 Uiso 1 1 calc R . . C15 C 0.63753(12) 0.6909(3) -0.08634(10) 0.0378(5) Uani 1 1 d . . . H15A H 0.6300 0.6852 -0.1375 0.045 Uiso 1 1 calc R . . C16 C 0.69590(12) 0.7811(2) -0.04359(10) 0.0364(5) Uani 1 1 d . . . H16A H 0.7285 0.8388 -0.0653 0.044 Uiso 1 1 calc R . . C17 C 0.70747(11) 0.7884(2) 0.03149(10) 0.0303(4) Uani 1 1 d . . . H17A H 0.7481 0.8509 0.0606 0.036 Uiso 1 1 calc R . . C18 C 0.58340(10) 0.74057(19) 0.29115(9) 0.0219(4) Uani 1 1 d . . . C19 C 0.50261(10) 0.7475(2) 0.26212(9) 0.0236(4) Uani 1 1 d . . . C20 C 0.45429(10) 0.7557(2) 0.30779(9) 0.0240(4) Uani 1 1 d . . . C21 C 0.48994(10) 0.7558(2) 0.38336(9) 0.0274(4) Uani 1 1 d . . . H21A H 0.4581 0.7615 0.4152 0.033 Uiso 1 1 calc R . . C22 C 0.57030(10) 0.7480(2) 0.41404(9) 0.0262(4) Uani 1 1 d . . . C23 C 0.61571(10) 0.7399(2) 0.36685(9) 0.0238(4) Uani 1 1 d . . . H23A H 0.6702 0.7338 0.3864 0.029 Uiso 1 1 calc R . . C24 C 0.36570(10) 0.7646(2) 0.27581(10) 0.0289(4) Uani 1 1 d . . . C25 C 0.34391(11) 0.9141(3) 0.22984(11) 0.0409(5) Uani 1 1 d . . . H25A H 0.2877 0.9193 0.2093 0.061 Uiso 1 1 calc R . . H25B H 0.3683 0.9127 0.1902 0.061 Uiso 1 1 calc R . . H25C H 0.3619 1.0057 0.2608 0.061 Uiso 1 1 calc R . . C26 C 0.33601(11) 0.6197(3) 0.22853(11) 0.0439(6) Uani 1 1 d . . . H26A H 0.2798 0.6265 0.2082 0.066 Uiso 1 1 calc R . . H26B H 0.3492 0.5254 0.2586 0.066 Uiso 1 1 calc R . . H26C H 0.3601 0.6149 0.1887 0.066 Uiso 1 1 calc R . . C27 C 0.32445(11) 0.7696(3) 0.33578(11) 0.0378(5) Uani 1 1 d . . . H27A H 0.2685 0.7751 0.3134 0.057 Uiso 1 1 calc R . . H27B H 0.3415 0.8619 0.3665 0.057 Uiso 1 1 calc R . . H27C H 0.3370 0.6752 0.3658 0.057 Uiso 1 1 calc R . . C28 C 0.60926(11) 0.7494(2) 0.49702(9) 0.0336(5) Uani 1 1 d . . . C29 C 0.65687(14) 0.6007(3) 0.51860(11) 0.0509(6) Uani 1 1 d . . . H29A H 0.6227 0.5096 0.5074 0.076 Uiso 1 1 calc R . . H29B H 0.6834 0.6030 0.5710 0.076 Uiso 1 1 calc R . . H29C H 0.6952 0.5941 0.4913 0.076 Uiso 1 1 calc R . . C30 C 0.66410(14) 0.8909(3) 0.51588(11) 0.0527(6) Uani 1 1 d . . . H30A H 0.6893 0.8929 0.5685 0.079 Uiso 1 1 calc R . . H30B H 0.6345 0.9873 0.5013 0.079 Uiso 1 1 calc R . . H30C H 0.7034 0.8824 0.4898 0.079 Uiso 1 1 calc R . . C31 C 0.55136(15) 0.7611(4) 0.54116(11) 0.0675(8) Uani 1 1 d . . . H31A H 0.5160 0.6717 0.5299 0.101 Uiso 1 1 calc R . . H31B H 0.5218 0.8582 0.5287 0.101 Uiso 1 1 calc R . . H31C H 0.5790 0.7610 0.5933 0.101 Uiso 1 1 calc R . . O1S O 0.30940(8) 0.75868(19) -0.09165(7) 0.0486(4) Uani 1 1 d . . . C1S C 0.36938(12) 0.8241(3) -0.05910(10) 0.0371(5) Uani 1 1 d . . . C2S C 0.39778(13) 0.8180(3) 0.02258(11) 0.0515(6) Uani 1 1 d . . . H2S1 H 0.3959 0.9230 0.0425 0.077 Uiso 1 1 calc R . . H2S2 H 0.4511 0.7795 0.0376 0.077 Uiso 1 1 calc R . . H2S3 H 0.3649 0.7476 0.0410 0.077 Uiso 1 1 calc R . . C3S C 0.41782(13) 0.9101(3) -0.09813(12) 0.0460(6) Uani 1 1 d . . . H3S1 H 0.4660 0.8528 -0.0931 0.069 Uiso 1 1 calc R . . H3S2 H 0.4297 1.0147 -0.0770 0.069 Uiso 1 1 calc R . . H3S3 H 0.3895 0.9194 -0.1499 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0218(6) 0.0543(9) 0.0158(6) -0.0002(6) 0.0069(5) 0.0013(6) C1 0.0212(9) 0.0278(10) 0.0183(8) 0.0004(7) 0.0066(7) 0.0017(7) N2 0.0209(7) 0.0321(9) 0.0176(7) -0.0026(6) 0.0061(6) -0.0003(6) C3 0.0240(9) 0.0258(10) 0.0210(9) -0.0009(7) 0.0093(7) 0.0005(7) C4 0.0208(9) 0.0262(9) 0.0205(9) -0.0002(7) 0.0090(7) -0.0002(7) N5 0.0213(7) 0.0312(8) 0.0174(7) 0.0010(6) 0.0078(6) 0.0005(6) C6 0.0220(9) 0.0267(10) 0.0204(8) 0.0019(7) 0.0072(7) 0.0004(7) C7 0.0275(10) 0.0288(10) 0.0225(9) -0.0010(8) 0.0090(8) -0.0001(8) C8 0.0241(10) 0.0352(11) 0.0292(10) -0.0004(8) 0.0034(8) -0.0051(8) C9 0.0210(9) 0.0437(12) 0.0377(11) 0.0008(9) 0.0112(8) 0.0003(9) C10 0.0285(11) 0.0396(12) 0.0394(11) -0.0057(9) 0.0159(9) 0.0032(9) C11 0.0259(10) 0.0327(11) 0.0305(10) -0.0060(8) 0.0104(8) -0.0025(8) C12 0.0221(9) 0.0300(10) 0.0184(8) -0.0008(7) 0.0082(7) 0.0045(7) C13 0.0291(10) 0.0411(12) 0.0238(10) 0.0001(8) 0.0085(8) -0.0056(9) C14 0.0396(12) 0.0531(14) 0.0223(10) -0.0068(9) 0.0064(9) -0.0094(10) C15 0.0446(12) 0.0520(13) 0.0186(9) -0.0030(9) 0.0119(9) 0.0013(10) C16 0.0387(12) 0.0495(13) 0.0264(10) -0.0001(9) 0.0178(9) -0.0052(10) C17 0.0291(10) 0.0386(11) 0.0254(9) -0.0023(8) 0.0111(8) -0.0058(8) C18 0.0227(9) 0.0257(9) 0.0191(8) 0.0002(7) 0.0086(7) 0.0022(7) C19 0.0252(9) 0.0290(10) 0.0163(8) -0.0006(7) 0.0053(7) 0.0014(7) C20 0.0217(9) 0.0285(10) 0.0228(9) 0.0000(7) 0.0082(7) 0.0015(7) C21 0.0289(10) 0.0335(11) 0.0241(9) -0.0001(8) 0.0145(8) 0.0033(8) C22 0.0293(10) 0.0310(10) 0.0191(8) 0.0017(7) 0.0080(7) 0.0055(8) C23 0.0217(9) 0.0301(10) 0.0199(8) 0.0009(7) 0.0064(7) 0.0031(7) C24 0.0211(9) 0.0409(12) 0.0265(9) -0.0014(8) 0.0099(8) 0.0016(8) C25 0.0303(11) 0.0571(14) 0.0361(11) 0.0089(10) 0.0109(9) 0.0114(10) C26 0.0299(11) 0.0620(15) 0.0422(12) -0.0143(11) 0.0143(10) -0.0126(10) C27 0.0248(10) 0.0582(14) 0.0348(11) 0.0001(10) 0.0153(8) 0.0037(9) C28 0.0357(11) 0.0496(13) 0.0164(8) 0.0020(8) 0.0089(8) 0.0091(9) C29 0.0596(15) 0.0622(16) 0.0280(11) 0.0119(10) 0.0075(11) 0.0158(12) C30 0.0665(16) 0.0599(16) 0.0257(11) -0.0093(10) 0.0031(11) 0.0024(13) C31 0.0535(15) 0.130(3) 0.0219(11) 0.0053(13) 0.0155(11) 0.0220(15) O1S 0.0321(8) 0.0819(12) 0.0275(8) 0.0000(7) 0.0016(6) -0.0022(8) C1S 0.0351(11) 0.0423(12) 0.0290(10) -0.0006(9) 0.0013(9) 0.0127(10) C2S 0.0497(14) 0.0693(17) 0.0270(11) -0.0007(11) -0.0029(10) 0.0061(12) C3S 0.0520(14) 0.0396(13) 0.0459(13) -0.0022(10) 0.0132(11) -0.0010(10) _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 O1 C19 1.3681(19) . ? O1 H1 0.8400 . ? C1 N5 1.339(2) . ? C1 N2 1.360(2) . ? C1 C18 1.462(2) . ? N2 C3 1.380(2) . ? N2 H2A 0.8800 . ? C3 C4 1.382(2) . ? C3 C6 1.472(2) . ? C4 N5 1.385(2) . ? C4 C12 1.476(2) . ? C6 C11 1.392(2) . ? C6 C7 1.401(2) . ? C7 C8 1.390(3) . ? C7 H7A 0.9500 . ? C8 C9 1.381(3) . ? C8 H8A 0.9500 . ? C9 C10 1.385(3) . ? C9 H9A 0.9500 . ? C10 C11 1.391(3) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C17 1.392(3) . ? C12 C13 1.396(2) . ? C13 C14 1.383(3) . ? C13 H13A 0.9500 . ? C14 C15 1.385(3) . ? C14 H14A 0.9500 . ? C15 C16 1.373(3) . ? C15 H15A 0.9500 . ? C16 C17 1.393(3) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C23 1.399(2) . ? C18 C19 1.407(2) . ? C19 C20 1.402(2) . ? C20 C21 1.405(2) . ? C20 C24 1.543(2) . ? C21 C22 1.403(2) . ? C21 H21A 0.9500 . ? C22 C23 1.384(2) . ? C22 C28 1.543(2) . ? C23 H23A 0.9500 . ? C24 C27 1.537(3) . ? C24 C26 1.539(3) . ? C24 C25 1.539(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C31 1.523(3) . ? C28 C29 1.525(3) . ? C28 C30 1.541(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? O1S C1S 1.221(2) . ? C1S C3S 1.496(3) . ? C1S C2S 1.501(3) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? 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 C19 O1 H1 109.5 . . ? N5 C1 N2 109.79(15) . . ? N5 C1 C18 124.30(15) . . ? N2 C1 C18 125.91(14) . . ? C1 N2 C3 108.73(13) . . ? C1 N2 H2A 125.6 . . ? C3 N2 H2A 125.6 . . ? N2 C3 C4 105.43(15) . . ? N2 C3 C6 121.74(15) . . ? C4 C3 C6 132.83(16) . . ? C3 C4 N5 109.36(15) . . ? C3 C4 C12 130.12(16) . . ? N5 C4 C12 120.44(14) . . ? C1 N5 C4 106.68(14) . . ? C11 C6 C7 118.97(16) . . ? C11 C6 C3 121.13(16) . . ? C7 C6 C3 119.90(16) . . ? C8 C7 C6 120.04(17) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C9 C8 C7 120.36(17) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 120.17(17) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C9 C10 C11 119.80(18) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C10 C11 C6 120.65(17) . . ? C10 C11 H11A 119.7 . . ? C6 C11 H11A 119.7 . . ? C17 C12 C13 118.14(16) . . ? C17 C12 C4 121.72(16) . . ? C13 C12 C4 120.11(16) . . ? C14 C13 C12 120.79(18) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C15 120.34(18) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C16 C15 C14 119.69(17) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? C15 C16 C17 120.24(18) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C12 C17 C16 120.81(17) . . ? C12 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? C23 C18 C19 119.23(16) . . ? C23 C18 C1 120.92(15) . . ? C19 C18 C1 119.85(14) . . ? O1 C19 C20 118.64(15) . . ? O1 C19 C18 120.30(15) . . ? C20 C19 C18 121.06(15) . . ? C19 C20 C21 117.23(16) . . ? C19 C20 C24 120.96(14) . . ? C21 C20 C24 121.81(16) . . ? C22 C21 C20 123.11(17) . . ? C22 C21 H21A 118.4 . . ? C20 C21 H21A 118.4 . . ? C23 C22 C21 117.64(15) . . ? C23 C22 C28 119.40(16) . . ? C21 C22 C28 122.96(16) . . ? C22 C23 C18 121.72(16) . . ? C22 C23 H23A 119.1 . . ? C18 C23 H23A 119.1 . . ? C27 C24 C26 107.44(16) . . ? C27 C24 C25 107.69(16) . . ? C26 C24 C25 110.18(16) . . ? C27 C24 C20 111.95(14) . . ? C26 C24 C20 109.96(15) . . ? C25 C24 C20 109.56(15) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C31 C28 C29 109.16(18) . . ? C31 C28 C30 108.38(19) . . ? C29 C28 C30 108.50(18) . . ? C31 C28 C22 112.80(17) . . ? C29 C28 C22 109.19(16) . . ? C30 C28 C22 108.73(16) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O1S C1S C3S 122.09(18) . . ? O1S C1S C2S 120.4(2) . . ? C3S C1S C2S 117.54(19) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C1S C3S H3S1 109.5 . . ? C1S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C1S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N5 0.84 1.83 2.5960(18) 150.7 . N2 H2A O1S 0.88 1.98 2.8525(19) 168.8 4_676 _diffrn_measured_fraction_theta_max 0.892 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.309 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.077 #end===== data_cupzbu _database_code_CSD 199489 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (CuL2).3MeOH _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H74 Cu N4 O5' _chemical_formula_weight 1006.78 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.207(1) _cell_length_b 13.790(1) _cell_length_c 18.805(2) _cell_angle_alpha 70.972(2) _cell_angle_beta 74.630(2) _cell_angle_gamma 68.125(2) _cell_volume 2739.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7140 _cell_measurement_theta_min 2.315 _cell_measurement_theta_max 28.485 _exptl_crystal_description column _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1074 _exptl_absorpt_coefficient_mu 0.450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.615 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details 'Bruker SADABS v2.03 (2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19728 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.87 _reflns_number_total 12281 _reflns_number_gt 9231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0783P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed, MeOH delta-F' _refine_ls_hydrogen_treatment 'riding model, MeOH rigid rotating group' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12280 _refine_ls_number_parameters 646 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.1306 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Cu Cu 0.55407(2) 0.94469(2) 0.269330(15) 0.01831(9) Uani 1 1 d . . . O1 O 0.42376(13) 1.04860(12) 0.31448(9) 0.0208(3) Uani 1 1 d . . . C1 C 0.61991(19) 0.97532(18) 0.39585(12) 0.0189(4) Uani 1 1 d . . . N2 N 0.70183(16) 0.93146(15) 0.44335(10) 0.0198(4) Uani 1 1 d . . . H2A H 0.7073 0.9615 0.4765 0.024 Uiso 1 1 calc R . . C3 C 0.7753(2) 0.83225(18) 0.43157(13) 0.0200(5) Uani 1 1 d . . . C4 C 0.73470(19) 0.81716(17) 0.37593(12) 0.0190(4) Uani 1 1 d . . . N5 N 0.63816(16) 0.90681(15) 0.35439(10) 0.0182(4) Uani 1 1 d . . . C6 C 0.8763(2) 0.76446(19) 0.47336(13) 0.0223(5) Uani 1 1 d . . . C7 C 0.9622(2) 0.8061(2) 0.47539(15) 0.0315(6) Uani 1 1 d . . . H7A H 0.9555 0.8796 0.4506 0.038 Uiso 1 1 calc R . . C8 C 1.0582(2) 0.7410(2) 0.51341(16) 0.0399(7) Uani 1 1 d . . . H8A H 1.1170 0.7702 0.5142 0.048 Uiso 1 1 calc R . . C9 C 1.0688(2) 0.6342(2) 0.55009(16) 0.0389(7) Uani 1 1 d . . . H9A H 1.1342 0.5900 0.5763 0.047 Uiso 1 1 calc R . . C10 C 0.9832(3) 0.5920(2) 0.54839(16) 0.0409(7) Uani 1 1 d . . . H10A H 0.9900 0.5185 0.5734 0.049 Uiso 1 1 calc R . . C11 C 0.8874(2) 0.6565(2) 0.51043(15) 0.0334(6) Uani 1 1 d . . . H11A H 0.8289 0.6269 0.5097 0.040 Uiso 1 1 calc R . . C12 C 0.7839(2) 0.72849(18) 0.33766(13) 0.0217(5) Uani 1 1 d . . . C13 C 0.9067(2) 0.69247(19) 0.31130(14) 0.0284(5) Uani 1 1 d . . . H13A H 0.9582 0.7226 0.3208 0.034 Uiso 1 1 calc R . . C14 C 0.9541(3) 0.6134(2) 0.27152(16) 0.0377(7) Uani 1 1 d . . . H14A H 1.0376 0.5907 0.2531 0.045 Uiso 1 1 calc R . . C15 C 0.8806(3) 0.5674(2) 0.25839(16) 0.0407(7) Uani 1 1 d . . . H15A H 0.9135 0.5124 0.2317 0.049 Uiso 1 1 calc R . . C16 C 0.7581(3) 0.6022(2) 0.28459(15) 0.0369(7) Uani 1 1 d . . . H16A H 0.7072 0.5711 0.2756 0.044 Uiso 1 1 calc R . . C17 C 0.7099(2) 0.68255(19) 0.32400(14) 0.0268(5) Uani 1 1 d . . . H17A H 0.6262 0.7061 0.3416 0.032 Uiso 1 1 calc R . . C18 C 0.53559(19) 1.08458(18) 0.38542(12) 0.0195(5) Uani 1 1 d . . . C19 C 0.44633(19) 1.11890(18) 0.33954(12) 0.0199(5) Uani 1 1 d . . . C20 C 0.3791(2) 1.23089(19) 0.32065(13) 0.0220(5) Uani 1 1 d . . . C21 C 0.4017(2) 1.29951(19) 0.35100(13) 0.0256(5) Uani 1 1 d . . . H21A H 0.3566 1.3740 0.3386 0.031 Uiso 1 1 calc R . . C22 C 0.4865(2) 1.26631(18) 0.39855(13) 0.0233(5) Uani 1 1 d . . . C23 C 0.5532(2) 1.15785(18) 0.41480(13) 0.0220(5) Uani 1 1 d . . . H23A H 0.6121 1.1326 0.4466 0.026 Uiso 1 1 calc R . . C24 C 0.2887(2) 1.2746(2) 0.26516(14) 0.0268(5) Uani 1 1 d . . . C25 C 0.3548(2) 1.2496(2) 0.18816(14) 0.0344(6) Uani 1 1 d . . . H25A H 0.3920 1.1714 0.1956 0.052 Uiso 1 1 calc R . . H25B H 0.4167 1.2852 0.1671 0.052 Uiso 1 1 calc R . . H25C H 0.2977 1.2764 0.1527 0.052 Uiso 1 1 calc R . . C26 C 0.1881(2) 1.2232(2) 0.29672(16) 0.0353(6) Uani 1 1 d . . . H26A H 0.2226 1.1444 0.3065 0.053 Uiso 1 1 calc R . . H26B H 0.1340 1.2496 0.2594 0.053 Uiso 1 1 calc R . . H26C H 0.1434 1.2426 0.3444 0.053 Uiso 1 1 calc R . . C27 C 0.2315(3) 1.3981(2) 0.25000(16) 0.0393(7) Uani 1 1 d . . . H27A H 0.2944 1.4326 0.2299 0.059 Uiso 1 1 calc R . . H27B H 0.1861 1.4169 0.2977 0.059 Uiso 1 1 calc R . . H27C H 0.1775 1.4235 0.2127 0.059 Uiso 1 1 calc R . . C28 C 0.5093(2) 1.34941(19) 0.42589(14) 0.0282(5) Uani 1 1 d . . . C29 C 0.5596(3) 1.4262(3) 0.35668(19) 0.0516(8) Uani 1 1 d . . . H29A H 0.6346 1.3846 0.3306 0.077 Uiso 1 1 calc R . . H29B H 0.5749 1.4793 0.3737 0.077 Uiso 1 1 calc R . . H29C H 0.5016 1.4637 0.3215 0.077 Uiso 1 1 calc R . . C30 C 0.3932(3) 1.4169(2) 0.46538(17) 0.0456(8) Uani 1 1 d . . . H30A H 0.3593 1.3693 0.5098 0.068 Uiso 1 1 calc R . . H30B H 0.3359 1.4550 0.4297 0.068 Uiso 1 1 calc R . . H30C H 0.4099 1.4696 0.4820 0.068 Uiso 1 1 calc R . . C31 C 0.5992(4) 1.2963(3) 0.4805(2) 0.0722(12) Uani 1 1 d . . . H31A H 0.6742 1.2529 0.4557 0.108 Uiso 1 1 calc R . . H31B H 0.5672 1.2495 0.5264 0.108 Uiso 1 1 calc R . . H31C H 0.6143 1.3521 0.4946 0.108 Uiso 1 1 calc R . . O1A O 0.45755(13) 0.91169(13) 0.22101(9) 0.0224(3) Uani 1 1 d . . . C1A C 0.70081(19) 0.84734(18) 0.14627(12) 0.0195(5) Uani 1 1 d . . . N2A N 0.81263(16) 0.82610(16) 0.10496(11) 0.0238(4) Uani 1 1 d . . . H2AA H 0.8410 0.7848 0.0729 0.029 Uiso 1 1 calc R . . C3A C 0.8748(2) 0.87966(19) 0.12122(13) 0.0224(5) Uani 1 1 d . . . C4A C 0.79701(19) 0.93509(18) 0.17238(13) 0.0200(5) Uani 1 1 d . . . N5A N 0.68862(16) 0.91367(15) 0.18816(10) 0.0184(4) Uani 1 1 d . . . C6A C 1.0020(2) 0.8630(2) 0.08814(13) 0.0257(5) Uani 1 1 d . . . C7A C 1.0568(2) 0.9406(2) 0.07641(14) 0.0278(5) Uani 1 1 d . . . H7AA H 1.0113 1.0071 0.0894 0.033 Uiso 1 1 calc R . . C8A C 1.1774(2) 0.9215(2) 0.04586(15) 0.0357(6) Uani 1 1 d . . . H8AA H 1.2137 0.9752 0.0378 0.043 Uiso 1 1 calc R . . C9A C 1.2448(2) 0.8251(3) 0.02711(18) 0.0460(8) Uani 1 1 d . . . H9AA H 1.3274 0.8124 0.0066 0.055 Uiso 1 1 calc R . . C10A C 1.1923(3) 0.7472(3) 0.0381(2) 0.0507(8) Uani 1 1 d . . . H10B H 1.2384 0.6810 0.0249 0.061 Uiso 1 1 calc R . . C11A C 1.0715(2) 0.7660(2) 0.06866(17) 0.0377(7) Uani 1 1 d . . . H11B H 1.0357 0.7121 0.0764 0.045 Uiso 1 1 calc R . . C12A C 0.8072(2) 1.01208(18) 0.20754(13) 0.0215(5) Uani 1 1 d . . . C13A C 0.9005(2) 0.9883(2) 0.24533(14) 0.0269(5) Uani 1 1 d . . . H13B H 0.9613 0.9202 0.2491 0.032 Uiso 1 1 calc R . . C14A C 0.9060(2) 1.0636(2) 0.27794(16) 0.0347(6) Uani 1 1 d . . . H14B H 0.9713 1.0470 0.3030 0.042 Uiso 1 1 calc R . . C15A C 0.8173(2) 1.1617(2) 0.27402(16) 0.0368(6) Uani 1 1 d . . . H15B H 0.8211 1.2124 0.2967 0.044 Uiso 1 1 calc R . . C16A C 0.7225(2) 1.1865(2) 0.23696(15) 0.0336(6) Uani 1 1 d . . . H16B H 0.6611 1.2541 0.2344 0.040 Uiso 1 1 calc R . . C17A C 0.7173(2) 1.11268(19) 0.20364(14) 0.0268(5) Uani 1 1 d . . . H17B H 0.6525 1.1302 0.1779 0.032 Uiso 1 1 calc R . . C18A C 0.6149(2) 0.79514(18) 0.14996(12) 0.0198(5) Uani 1 1 d . . . C19A C 0.49772(19) 0.82575(18) 0.19228(13) 0.0198(5) Uani 1 1 d . . . C20A C 0.4235(2) 0.7615(2) 0.20374(13) 0.0233(5) Uani 1 1 d . . . C21A C 0.4663(2) 0.67593(19) 0.16943(14) 0.0263(5) Uani 1 1 d . . . H21B H 0.4147 0.6354 0.1758 0.032 Uiso 1 1 calc R . . C22A C 0.5800(2) 0.64585(19) 0.12634(13) 0.0238(5) Uani 1 1 d . . . C23A C 0.6532(2) 0.70667(19) 0.11818(13) 0.0225(5) Uani 1 1 d . . . H23B H 0.7318 0.6878 0.0901 0.027 Uiso 1 1 calc R . . C24A C 0.3056(2) 0.7782(2) 0.26030(15) 0.0298(6) Uani 1 1 d . . . C25A C 0.2359(3) 0.7041(3) 0.26202(19) 0.0486(8) Uani 1 1 d . . . H25D H 0.1614 0.7176 0.2986 0.073 Uiso 1 1 calc R . . H25E H 0.2848 0.6284 0.2775 0.073 Uiso 1 1 calc R . . H25F H 0.2173 0.7192 0.2111 0.073 Uiso 1 1 calc R . . C26A C 0.3374(2) 0.7479(2) 0.34041(15) 0.0359(6) Uani 1 1 d . . . H26D H 0.3814 0.7941 0.3413 0.054 Uiso 1 1 calc R . . H26E H 0.3873 0.6721 0.3529 0.054 Uiso 1 1 calc R . . H26F H 0.2638 0.7583 0.3779 0.054 Uiso 1 1 calc R . . C27A C 0.2211(2) 0.8944(2) 0.24298(17) 0.0371(7) Uani 1 1 d . . . H27D H 0.2623 0.9440 0.2416 0.056 Uiso 1 1 calc R . . H27E H 0.1501 0.9014 0.2828 0.056 Uiso 1 1 calc R . . H27F H 0.1966 0.9123 0.1934 0.056 Uiso 1 1 calc R . . C28A C 0.6259(2) 0.5490(2) 0.09098(15) 0.0303(6) Uani 1 1 d . . . C29A C 0.6523(3) 0.5876(3) 0.00569(17) 0.0576(9) Uani 1 1 d . . . H29D H 0.5786 0.6373 -0.0136 0.086 Uiso 1 1 calc R . . H29E H 0.6833 0.5256 -0.0167 0.086 Uiso 1 1 calc R . . H29F H 0.7120 0.6252 -0.0083 0.086 Uiso 1 1 calc R . . C30A C 0.7415(3) 0.4694(2) 0.1215(2) 0.0513(8) Uani 1 1 d . . . H30D H 0.8016 0.5063 0.1083 0.077 Uiso 1 1 calc R . . H30E H 0.7723 0.4080 0.0984 0.077 Uiso 1 1 calc R . . H30F H 0.7238 0.4433 0.1770 0.077 Uiso 1 1 calc R . . C31A C 0.5359(3) 0.4866(3) 0.1130(2) 0.0513(8) Uani 1 1 d . . . H31D H 0.4614 0.5344 0.0940 0.077 Uiso 1 1 calc R . . H31E H 0.5194 0.4610 0.1686 0.077 Uiso 1 1 calc R . . H31F H 0.5694 0.4247 0.0904 0.077 Uiso 1 1 calc R . . O1S O 0.83850(17) 0.79170(18) -0.04083(11) 0.0445(5) Uani 1 1 d . . . H1S H 0.7738 0.8314 -0.0564 0.067 Uiso 1 1 calc R . . C1S C 0.9321(3) 0.7826(3) -0.1038(2) 0.0622(10) Uani 1 1 d . . . H1S1 H 0.9169 0.8507 -0.1435 0.093 Uiso 1 1 calc R . . H1S2 H 0.9362 0.7241 -0.1242 0.093 Uiso 1 1 calc R . . H1S3 H 1.0082 0.7666 -0.0874 0.093 Uiso 1 1 calc R . . O2S O 0.37239(16) 1.06803(16) 0.08865(11) 0.0360(4) Uani 1 1 d . . . H2S H 0.3847 1.0210 0.1299 0.054 Uiso 1 1 calc R . . C2S C 0.4796(2) 1.0930(2) 0.05078(15) 0.0346(6) Uani 1 1 d . . . H2S1 H 0.4991 1.1300 0.0799 0.052 Uiso 1 1 calc R . . H2S2 H 0.4686 1.1400 -0.0003 0.052 Uiso 1 1 calc R . . H2S3 H 0.5451 1.0261 0.0466 0.052 Uiso 1 1 calc R . . O3S O 0.27642(15) 0.98600(15) 0.44427(10) 0.0302(4) Uani 1 1 d . . . H3S H 0.3167 0.9999 0.4006 0.045 Uiso 1 1 calc R . . C3S C 0.1667(3) 0.9793(3) 0.43780(17) 0.0417(7) Uani 1 1 d . . . H3S1 H 0.1270 0.9491 0.4884 0.063 Uiso 1 1 calc R . . H3S2 H 0.1821 0.9326 0.4043 0.063 Uiso 1 1 calc R . . H3S3 H 0.1151 1.0517 0.4163 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.01721(15) 0.02006(15) 0.01928(15) -0.00804(11) -0.00583(10) -0.00306(11) O1 0.0173(8) 0.0228(8) 0.0249(8) -0.0121(7) -0.0073(6) -0.0012(7) C1 0.0173(11) 0.0213(11) 0.0194(11) -0.0050(9) -0.0044(9) -0.0067(9) N2 0.0206(10) 0.0200(10) 0.0198(10) -0.0055(8) -0.0076(8) -0.0042(8) C3 0.0202(11) 0.0190(11) 0.0199(11) -0.0032(9) -0.0059(9) -0.0048(9) C4 0.0173(11) 0.0171(11) 0.0213(11) -0.0028(9) -0.0069(9) -0.0032(9) N5 0.0167(9) 0.0185(9) 0.0198(9) -0.0043(8) -0.0065(7) -0.0040(8) C6 0.0197(11) 0.0225(12) 0.0208(12) -0.0054(10) -0.0068(9) -0.0001(9) C7 0.0300(14) 0.0329(14) 0.0300(14) -0.0030(11) -0.0122(11) -0.0072(11) C8 0.0263(14) 0.0526(19) 0.0409(16) -0.0074(14) -0.0153(12) -0.0096(13) C9 0.0318(15) 0.0393(16) 0.0336(15) -0.0062(13) -0.0181(12) 0.0080(12) C10 0.0532(18) 0.0240(14) 0.0381(16) -0.0005(12) -0.0245(14) 0.0013(13) C11 0.0377(15) 0.0266(13) 0.0368(15) -0.0041(11) -0.0178(12) -0.0065(12) C12 0.0278(12) 0.0143(11) 0.0195(11) -0.0013(9) -0.0113(9) -0.0004(9) C13 0.0271(13) 0.0235(13) 0.0302(13) -0.0066(11) -0.0102(10) 0.0005(10) C14 0.0364(15) 0.0270(14) 0.0353(15) -0.0100(12) -0.0083(12) 0.0094(12) C15 0.064(2) 0.0208(13) 0.0294(14) -0.0095(11) -0.0100(14) 0.0002(13) C16 0.064(2) 0.0225(13) 0.0299(14) -0.0025(11) -0.0200(13) -0.0149(13) C17 0.0332(14) 0.0204(12) 0.0266(13) -0.0043(10) -0.0110(10) -0.0053(10) C18 0.0198(11) 0.0195(11) 0.0184(11) -0.0049(9) -0.0040(9) -0.0046(9) C19 0.0183(11) 0.0227(12) 0.0183(11) -0.0085(9) -0.0043(9) -0.0023(9) C20 0.0218(12) 0.0224(12) 0.0179(11) -0.0057(9) -0.0060(9) -0.0001(10) C21 0.0295(13) 0.0194(12) 0.0253(12) -0.0073(10) -0.0087(10) -0.0005(10) C22 0.0289(13) 0.0191(12) 0.0233(12) -0.0085(10) -0.0066(10) -0.0048(10) C23 0.0243(12) 0.0232(12) 0.0198(11) -0.0063(10) -0.0079(9) -0.0054(10) C24 0.0261(13) 0.0245(12) 0.0267(13) -0.0096(10) -0.0128(10) 0.0038(10) C25 0.0424(16) 0.0350(15) 0.0217(13) -0.0085(11) -0.0132(11) -0.0011(12) C26 0.0260(13) 0.0410(16) 0.0359(15) -0.0104(13) -0.0144(11) -0.0001(12) C27 0.0417(16) 0.0305(15) 0.0396(16) -0.0122(13) -0.0244(13) 0.0104(12) C28 0.0356(14) 0.0213(12) 0.0318(14) -0.0096(11) -0.0118(11) -0.0067(11) C29 0.063(2) 0.0457(19) 0.057(2) -0.0215(16) 0.0010(16) -0.0289(17) C30 0.061(2) 0.0420(17) 0.0423(17) -0.0216(14) -0.0002(15) -0.0217(16) C31 0.111(3) 0.0360(18) 0.098(3) -0.0229(19) -0.072(3) -0.011(2) O1A 0.0188(8) 0.0246(9) 0.0275(9) -0.0134(7) -0.0064(7) -0.0034(7) C1A 0.0187(11) 0.0212(11) 0.0184(11) -0.0058(9) -0.0051(9) -0.0040(9) N2A 0.0211(10) 0.0272(11) 0.0255(11) -0.0134(9) -0.0022(8) -0.0055(9) C3A 0.0206(12) 0.0240(12) 0.0228(12) -0.0057(10) -0.0029(9) -0.0078(10) C4A 0.0182(11) 0.0182(11) 0.0227(12) -0.0033(9) -0.0061(9) -0.0044(9) N5A 0.0170(9) 0.0179(9) 0.0205(10) -0.0052(8) -0.0055(7) -0.0038(8) C6A 0.0230(12) 0.0326(14) 0.0226(12) -0.0092(11) -0.0032(9) -0.0086(11) C7A 0.0281(13) 0.0345(14) 0.0236(12) -0.0076(11) -0.0037(10) -0.0129(11) C8A 0.0308(14) 0.0507(17) 0.0303(14) -0.0066(13) -0.0032(11) -0.0223(13) C9A 0.0221(14) 0.070(2) 0.0489(18) -0.0268(17) 0.0089(12) -0.0175(15) C10A 0.0298(15) 0.055(2) 0.070(2) -0.0385(18) 0.0050(15) -0.0056(14) C11A 0.0244(13) 0.0406(16) 0.0510(18) -0.0225(14) 0.0021(12) -0.0099(12) C12A 0.0213(11) 0.0229(12) 0.0214(12) -0.0067(10) -0.0009(9) -0.0090(10) C13A 0.0241(12) 0.0259(13) 0.0315(13) -0.0102(11) -0.0068(10) -0.0046(10) C14A 0.0314(14) 0.0425(16) 0.0398(16) -0.0185(13) -0.0078(12) -0.0138(13) C15A 0.0423(16) 0.0326(15) 0.0441(16) -0.0206(13) 0.0001(13) -0.0168(13) C16A 0.0346(15) 0.0229(13) 0.0421(16) -0.0111(12) -0.0024(12) -0.0078(11) C17A 0.0257(13) 0.0238(12) 0.0304(13) -0.0064(10) -0.0067(10) -0.0061(10) C18A 0.0229(12) 0.0189(11) 0.0185(11) -0.0035(9) -0.0088(9) -0.0048(9) C19A 0.0204(11) 0.0199(11) 0.0204(11) -0.0073(9) -0.0089(9) -0.0021(9) C20A 0.0204(12) 0.0293(13) 0.0230(12) -0.0099(10) -0.0070(9) -0.0057(10) C21A 0.0312(13) 0.0269(13) 0.0285(13) -0.0072(10) -0.0104(10) -0.0137(11) C22A 0.0296(13) 0.0222(12) 0.0233(12) -0.0092(10) -0.0087(10) -0.0060(10) C23A 0.0227(12) 0.0227(12) 0.0223(12) -0.0076(10) -0.0055(9) -0.0044(10) C24A 0.0226(12) 0.0403(15) 0.0326(14) -0.0159(12) -0.0024(10) -0.0121(11) C25A 0.0345(16) 0.067(2) 0.062(2) -0.0361(18) 0.0091(14) -0.0304(16) C26A 0.0361(15) 0.0425(16) 0.0291(14) -0.0098(12) -0.0001(11) -0.0151(13) C27A 0.0198(13) 0.0507(18) 0.0444(16) -0.0222(14) -0.0083(11) -0.0040(12) C28A 0.0378(15) 0.0264(13) 0.0327(14) -0.0136(11) -0.0075(11) -0.0104(11) C29A 0.101(3) 0.0429(18) 0.0366(18) -0.0197(15) -0.0037(18) -0.0287(19) C30A 0.058(2) 0.0323(16) 0.065(2) -0.0205(16) -0.0184(17) -0.0030(15) C31A 0.058(2) 0.0459(18) 0.065(2) -0.0319(17) -0.0025(17) -0.0228(16) O1S 0.0347(11) 0.0609(14) 0.0326(11) -0.0145(10) -0.0058(9) -0.0065(10) C1S 0.050(2) 0.089(3) 0.050(2) -0.036(2) 0.0035(16) -0.017(2) O2S 0.0336(10) 0.0367(11) 0.0358(11) -0.0041(9) -0.0122(8) -0.0089(9) C2S 0.0382(15) 0.0344(15) 0.0285(14) -0.0091(12) -0.0071(11) -0.0063(12) O3S 0.0327(10) 0.0389(10) 0.0242(9) -0.0101(8) -0.0055(7) -0.0145(8) C3S 0.0405(16) 0.0500(18) 0.0436(17) -0.0182(15) -0.0037(13) -0.0208(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 Cu O1A 1.9126(15) . y Cu O1 1.9192(15) . y Cu N5A 1.9452(18) . y Cu N5 1.9523(18) . y O1 C19 1.343(2) . ? C1 N5 1.335(3) . ? C1 N2 1.354(3) . ? C1 C18 1.458(3) . ? N2 C3 1.380(3) . ? C3 C4 1.371(3) . ? C3 C6 1.479(3) . ? C4 N5 1.386(3) . ? C4 C12 1.473(3) . ? C6 C7 1.383(3) . ? C6 C11 1.394(3) . ? C7 C8 1.390(4) . ? C8 C9 1.380(4) . ? C9 C10 1.383(4) . ? C10 C11 1.386(4) . ? C12 C17 1.392(3) . ? C12 C13 1.397(3) . ? C13 C14 1.384(3) . ? C14 C15 1.383(4) . ? C15 C16 1.393(4) . ? C16 C17 1.393(3) . ? C18 C23 1.400(3) . ? C18 C19 1.415(3) . ? C19 C20 1.427(3) . ? C20 C21 1.389(3) . ? C20 C24 1.541(3) . ? C21 C22 1.397(3) . ? C22 C23 1.385(3) . ? C22 C28 1.534(3) . ? C24 C26 1.533(4) . ? C24 C25 1.538(3) . ? C24 C27 1.541(3) . ? C28 C31 1.517(4) . ? C28 C30 1.528(4) . ? C28 C29 1.534(4) . ? O1A C19A 1.334(3) . ? C1A N5A 1.336(3) . ? C1A N2A 1.357(3) . ? C1A C18A 1.454(3) . ? N2A C3A 1.380(3) . ? C3A C4A 1.366(3) . ? C3A C6A 1.471(3) . ? C4A N5A 1.397(3) . ? C4A C12A 1.476(3) . ? C6A C7A 1.394(3) . ? C6A C11A 1.397(3) . ? C7A C8A 1.388(3) . ? C8A C9A 1.380(4) . ? C9A C10A 1.381(4) . ? C10A C11A 1.391(4) . ? C12A C13A 1.381(3) . ? C12A C17A 1.406(3) . ? C13A C14A 1.396(3) . ? C14A C15A 1.376(4) . ? C15A C16A 1.386(4) . ? C16A C17A 1.385(3) . ? C18A C23A 1.402(3) . ? C18A C19A 1.422(3) . ? C19A C20A 1.422(3) . ? C20A C21A 1.392(3) . ? C20A C24A 1.535(3) . ? C21A C22A 1.396(3) . ? C22A C23A 1.387(3) . ? C22A C28A 1.538(3) . ? C24A C27A 1.532(4) . ? C24A C26A 1.541(4) . ? C24A C25A 1.543(3) . ? C28A C29A 1.502(4) . ? C28A C31A 1.532(4) . ? C28A C30A 1.545(4) . ? O1S C1S 1.413(3) . ? O2S C2S 1.421(3) . ? O3S C3S 1.415(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Cu O1 95.33(6) . . y O1A Cu N5A 90.15(7) . . y O1 Cu N5A 149.28(7) . . y O1A Cu N5 148.97(7) . . y O1 Cu N5 90.10(7) . . y N5A Cu N5 100.58(7) . . y C19 O1 Cu 119.66(13) . . y N5 C1 N2 108.70(19) . . ? N5 C1 C18 125.6(2) . . ? N2 C1 C18 125.28(19) . . ? C1 N2 C3 109.19(18) . . ? C4 C3 N2 105.85(19) . . ? C4 C3 C6 131.4(2) . . ? N2 C3 C6 122.69(19) . . ? C3 C4 N5 108.40(19) . . ? C3 C4 C12 129.4(2) . . ? N5 C4 C12 122.00(19) . . ? C1 N5 C4 107.85(17) . . ? C1 N5 Cu 122.68(15) . . ? C4 N5 Cu 128.84(14) . . ? C7 C6 C11 118.9(2) . . ? C7 C6 C3 120.9(2) . . ? C11 C6 C3 120.2(2) . . ? C6 C7 C8 120.4(2) . . ? C9 C8 C7 120.5(3) . . ? C8 C9 C10 119.4(3) . . ? C9 C10 C11 120.3(3) . . ? C10 C11 C6 120.5(2) . . ? C17 C12 C13 118.8(2) . . ? C17 C12 C4 121.4(2) . . ? C13 C12 C4 119.7(2) . . ? C14 C13 C12 120.8(2) . . ? C15 C14 C13 120.4(3) . . ? C14 C15 C16 119.5(2) . . ? C15 C16 C17 120.2(3) . . ? C12 C17 C16 120.3(2) . . ? C23 C18 C19 120.7(2) . . ? C23 C18 C1 118.4(2) . . ? C19 C18 C1 120.53(19) . . ? O1 C19 C18 121.5(2) . . ? O1 C19 C20 120.11(19) . . ? C18 C19 C20 118.4(2) . . ? C21 C20 C19 117.9(2) . . ? C21 C20 C24 121.3(2) . . ? C19 C20 C24 120.7(2) . . ? C20 C21 C22 124.3(2) . . ? C23 C22 C21 117.0(2) . . ? C23 C22 C28 122.5(2) . . ? C21 C22 C28 120.3(2) . . ? C22 C23 C18 121.5(2) . . ? C26 C24 C25 109.7(2) . . ? C26 C24 C27 108.2(2) . . ? C25 C24 C27 107.2(2) . . ? C26 C24 C20 111.0(2) . . ? C25 C24 C20 108.94(19) . . ? C27 C24 C20 111.7(2) . . ? C31 C28 C30 108.7(2) . . ? C31 C28 C22 112.0(2) . . ? C30 C28 C22 111.0(2) . . ? C31 C28 C29 108.0(3) . . ? C30 C28 C29 108.1(2) . . ? C22 C28 C29 109.0(2) . . ? C19A O1A Cu 122.50(14) . . ? N5A C1A N2A 109.08(19) . . ? N5A C1A C18A 126.3(2) . . ? N2A C1A C18A 124.23(19) . . ? C1A N2A C3A 109.12(18) . . ? C4A C3A N2A 105.92(19) . . ? C4A C3A C6A 134.1(2) . . ? N2A C3A C6A 119.8(2) . . ? C3A C4A N5A 108.75(19) . . ? C3A C4A C12A 132.1(2) . . ? N5A C4A C12A 119.07(19) . . ? C1A N5A C4A 107.11(18) . . ? C1A N5A Cu 123.02(15) . . ? C4A N5A Cu 128.71(14) . . ? C7A C6A C11A 118.3(2) . . ? C7A C6A C3A 122.1(2) . . ? C11A C6A C3A 119.6(2) . . ? C8A C7A C6A 120.5(2) . . ? C9A C8A C7A 120.4(3) . . ? C8A C9A C10A 120.1(2) . . ? C9A C10A C11A 119.7(3) . . ? C10A C11A C6A 121.0(3) . . ? C13A C12A C17A 118.7(2) . . ? C13A C12A C4A 122.5(2) . . ? C17A C12A C4A 118.7(2) . . ? C12A C13A C14A 120.5(2) . . ? C15A C14A C13A 120.4(2) . . ? C14A C15A C16A 120.0(2) . . ? C17A C16A C15A 120.0(2) . . ? C16A C17A C12A 120.5(2) . . ? C23A C18A C19A 120.4(2) . . ? C23A C18A C1A 118.9(2) . . ? C19A C18A C1A 120.37(19) . . ? O1A C19A C20A 120.3(2) . . ? O1A C19A C18A 121.67(19) . . ? C20A C19A C18A 118.00(19) . . ? C21A C20A C19A 118.6(2) . . ? C21A C20A C24A 120.9(2) . . ? C19A C20A C24A 120.2(2) . . ? C20A C21A C22A 124.3(2) . . ? C23A C22A C21A 116.4(2) . . ? C23A C22A C28A 120.5(2) . . ? C21A C22A C28A 123.0(2) . . ? C22A C23A C18A 122.2(2) . . ? C27A C24A C20A 113.2(2) . . ? C27A C24A C26A 109.3(2) . . ? C20A C24A C26A 107.4(2) . . ? C27A C24A C25A 107.1(2) . . ? C20A C24A C25A 112.2(2) . . ? C26A C24A C25A 107.5(2) . . ? C29A C28A C31A 109.6(2) . . ? C29A C28A C22A 109.6(2) . . ? C31A C28A C22A 112.1(2) . . ? C29A C28A C30A 109.6(3) . . ? C31A C28A C30A 107.0(2) . . ? C22A C28A C30A 108.9(2) . . ? 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 O1A Cu O1 C19 -162.45(16) . . . . ? N5A Cu O1 C19 -63.1(2) . . . . ? N5 Cu O1 C19 48.15(16) . . . . ? N5 C1 N2 C3 0.5(2) . . . . y C18 C1 N2 C3 -172.7(2) . . . . y C1 N2 C3 C4 -0.5(2) . . . . y C1 N2 C3 C6 178.5(2) . . . . ? N2 C3 C4 N5 0.3(2) . . . . y C6 C3 C4 N5 -178.5(2) . . . . ? N2 C3 C4 C12 175.9(2) . . . . ? C6 C3 C4 C12 -3.0(4) . . . . ? N2 C1 N5 C4 -0.3(2) . . . . y C18 C1 N5 C4 172.9(2) . . . . y N2 C1 N5 Cu -171.92(13) . . . . ? C18 C1 N5 Cu 1.2(3) . . . . ? C3 C4 N5 C1 0.0(2) . . . . y C12 C4 N5 C1 -176.0(2) . . . . ? C3 C4 N5 Cu 170.95(15) . . . . ? C12 C4 N5 Cu -5.0(3) . . . . ? O1A Cu N5 C1 -126.39(17) . . . . ? O1 Cu N5 C1 -25.83(17) . . . . ? N5A Cu N5 C1 125.21(17) . . . . ? O1A Cu N5 C4 63.8(2) . . . . ? O1 Cu N5 C4 164.38(18) . . . . ? N5A Cu N5 C4 -44.58(19) . . . . ? C4 C3 C6 C7 126.0(3) . . . . y N2 C3 C6 C7 -52.7(3) . . . . y C4 C3 C6 C11 -52.9(4) . . . . y N2 C3 C6 C11 128.4(2) . . . . y C11 C6 C7 C8 0.4(4) . . . . ? C3 C6 C7 C8 -178.6(2) . . . . ? C6 C7 C8 C9 -0.4(4) . . . . ? C7 C8 C9 C10 0.3(4) . . . . ? C8 C9 C10 C11 -0.2(4) . . . . ? C9 C10 C11 C6 0.1(4) . . . . ? C7 C6 C11 C10 -0.2(4) . . . . ? C3 C6 C11 C10 178.7(2) . . . . ? C3 C4 C12 C17 137.1(3) . . . . y N5 C4 C12 C17 -47.8(3) . . . . y C3 C4 C12 C13 -45.8(4) . . . . y N5 C4 C12 C13 129.3(2) . . . . y C17 C12 C13 C14 0.7(4) . . . . ? C4 C12 C13 C14 -176.4(2) . . . . ? C12 C13 C14 C15 -1.1(4) . . . . ? C13 C14 C15 C16 0.9(4) . . . . ? C14 C15 C16 C17 -0.2(4) . . . . ? C13 C12 C17 C16 -0.1(4) . . . . ? C4 C12 C17 C16 177.0(2) . . . . ? C15 C16 C17 C12 -0.2(4) . . . . ? N5 C1 C18 C23 -159.3(2) . . . . y N2 C1 C18 C23 12.7(3) . . . . y N5 C1 C18 C19 13.8(3) . . . . y N2 C1 C18 C19 -174.1(2) . . . . y Cu O1 C19 C18 -47.3(3) . . . . ? Cu O1 C19 C20 133.22(18) . . . . ? C23 C18 C19 O1 -176.2(2) . . . . y C1 C18 C19 O1 10.8(3) . . . . y C23 C18 C19 C20 3.3(3) . . . . y C1 C18 C19 C20 -169.7(2) . . . . y O1 C19 C20 C21 176.9(2) . . . . y C18 C19 C20 C21 -2.6(3) . . . . y O1 C19 C20 C24 -6.0(3) . . . . ? C18 C19 C20 C24 174.5(2) . . . . ? C19 C20 C21 C22 0.3(4) . . . . y C24 C20 C21 C22 -176.7(2) . . . . ? C20 C21 C22 C23 1.2(4) . . . . y C20 C21 C22 C28 176.9(2) . . . . ? C21 C22 C23 C18 -0.6(3) . . . . y C28 C22 C23 C18 -176.1(2) . . . . ? C19 C18 C23 C22 -1.7(3) . . . . y C1 C18 C23 C22 171.4(2) . . . . y C21 C20 C24 C26 -120.9(2) . . . . ? C19 C20 C24 C26 62.1(3) . . . . ? C21 C20 C24 C25 118.2(2) . . . . ? C19 C20 C24 C25 -58.8(3) . . . . ? C21 C20 C24 C27 -0.1(3) . . . . ? C19 C20 C24 C27 -177.0(2) . . . . ? C23 C22 C28 C31 -7.9(4) . . . . ? C21 C22 C28 C31 176.7(3) . . . . ? C23 C22 C28 C30 -129.6(3) . . . . ? C21 C22 C28 C30 55.0(3) . . . . ? C23 C22 C28 C29 111.5(3) . . . . ? C21 C22 C28 C29 -63.9(3) . . . . ? O1 Cu O1A C19A -166.04(17) . . . . ? N5A Cu O1A C19A 44.23(17) . . . . ? N5 Cu O1A C19A -66.9(2) . . . . ? N5A C1A N2A C3A 0.5(3) . . . . y C18A C1A N2A C3A -172.9(2) . . . . y C1A N2A C3A C4A -1.0(3) . . . . y C1A N2A C3A C6A 175.2(2) . . . . ? N2A C3A C4A N5A 1.1(3) . . . . y C6A C3A C4A N5A -174.3(3) . . . . ? N2A C3A C4A C12A -175.6(2) . . . . ? C6A C3A C4A C12A 9.0(5) . . . . y N2A C1A N5A C4A 0.1(3) . . . . y C18A C1A N5A C4A 173.4(2) . . . . y N2A C1A N5A Cu -168.55(15) . . . . ? C18A C1A N5A Cu 4.7(3) . . . . ? C3A C4A N5A C1A -0.8(3) . . . . y C12A C4A N5A C1A 176.4(2) . . . . ? C3A C4A N5A Cu 167.07(16) . . . . ? C12A C4A N5A Cu -15.8(3) . . . . ? O1A Cu N5A C1A -25.46(18) . . . . ? O1 Cu N5A C1A -126.21(18) . . . . ? N5 Cu N5A C1A 125.25(18) . . . . ? O1A Cu N5A C4A 168.45(19) . . . . ? O1 Cu N5A C4A 67.7(2) . . . . ? N5 Cu N5A C4A -40.8(2) . . . . ? C4A C3A C6A C7A -30.9(4) . . . . y N2A C3A C6A C7A 154.2(2) . . . . y C4A C3A C6A C11A 148.2(3) . . . . y N2A C3A C6A C11A -26.7(4) . . . . y C11A C6A C7A C8A 0.2(4) . . . . ? C3A C6A C7A C8A 179.3(2) . . . . ? C6A C7A C8A C9A -0.4(4) . . . . ? C7A C8A C9A C10A 0.5(5) . . . . ? C8A C9A C10A C11A -0.5(5) . . . . ? C9A C10A C11A C6A 0.3(5) . . . . ? C7A C6A C11A C10A -0.2(4) . . . . ? C3A C6A C11A C10A -179.2(3) . . . . ? C3A C4A C12A C13A -53.4(4) . . . . y N5A C4A C12A C13A 130.2(2) . . . . y C3A C4A C12A C17A 127.8(3) . . . . y N5A C4A C12A C17A -48.6(3) . . . . y C17A C12A C13A C14A -1.0(4) . . . . ? C4A C12A C13A C14A -179.7(2) . . . . ? C12A C13A C14A C15A 1.2(4) . . . . ? C13A C14A C15A C16A -0.6(4) . . . . ? C14A C15A C16A C17A -0.3(4) . . . . ? C15A C16A C17A C12A 0.5(4) . . . . ? C13A C12A C17A C16A 0.1(4) . . . . ? C4A C12A C17A C16A 179.0(2) . . . . ? N5A C1A C18A C23A -162.9(2) . . . . y N2A C1A C18A C23A 9.4(3) . . . . y N5A C1A C18A C19A 10.3(4) . . . . y N2A C1A C18A C19A -177.4(2) . . . . y Cu O1A C19A C20A 137.54(18) . . . . ? Cu O1A C19A C18A -42.2(3) . . . . ? C23A C18A C19A O1A -177.7(2) . . . . y C1A C18A C19A O1A 9.1(3) . . . . y C23A C18A C19A C20A 2.5(3) . . . . y C1A C18A C19A C20A -170.6(2) . . . . y O1A C19A C20A C21A 176.6(2) . . . . y C18A C19A C20A C21A -3.7(3) . . . . y O1A C19A C20A C24A -10.5(3) . . . . ? C18A C19A C20A C24A 169.2(2) . . . . ? C19A C20A C21A C22A 2.5(4) . . . . y C24A C20A C21A C22A -170.3(2) . . . . ? C20A C21A C22A C23A 0.0(4) . . . . y C20A C21A C22A C28A 178.3(2) . . . . ? C21A C22A C23A C18A -1.3(3) . . . . y C28A C22A C23A C18A -179.6(2) . . . . ? C19A C18A C23A C22A 0.0(4) . . . . y C1A C18A C23A C22A 173.2(2) . . . . ? C21A C20A C24A C27A -131.0(2) . . . . ? C19A C20A C24A C27A 56.3(3) . . . . ? C21A C20A C24A C26A 108.2(3) . . . . ? C19A C20A C24A C26A -64.5(3) . . . . ? C21A C20A C24A C25A -9.7(3) . . . . ? C19A C20A C24A C25A 177.6(2) . . . . ? C23A C22A C28A C29A -63.5(3) . . . . ? C21A C22A C28A C29A 118.3(3) . . . . ? C23A C22A C28A C31A 174.6(2) . . . . ? C21A C22A C28A C31A -3.7(4) . . . . ? C23A C22A C28A C30A 56.4(3) . . . . ? C21A C22A C28A C30A -121.8(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2A H2AA O1S 0.88 2.12 2.849(3) 140.1 . O3S H3S O1 0.84 1.90 2.719(2) 165.0 . O2S H2S O1A 0.84 2.03 2.851(2) 165.0 . N2 H2A O3S 0.88 1.94 2.815(2) 174.6 2_676 O1S H1S O2S 0.84 1.91 2.749(3) 174.7 2_675 _diffrn_measured_fraction_theta_max 0.852 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.695 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.078 #end===== data_ZNIMTB _database_code_CSD 199490 _refine_special_details ; Disorder on solvent has been modelled with MeCN/CH2Cl2 with respective occupancies of 0.5 and 0.3; partially occupied atoms refined with isotropic adps and H-atoms were not located. Restraints were applied on CH2Cl2 geometry. Two MeCN molecules are also present, for which the H-atoms could not be found. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (ZnL2).2.5MeCN.0.3CH2Cl2 _chemical_melting_point ? _chemical_formula_moiety 'Zn C58 H62 O2 N4, 2.5(C2 H3 N), 0.3(C H2 Cl2)' _chemical_formula_sum 'C63.30 H70.10 Cl0.60 N6.50 O2 Zn' _chemical_formula_weight 1040.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.9519(9) _cell_length_b 17.8270(9) _cell_length_c 19.2760(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.088(1) _cell_angle_gamma 90.00 _cell_volume 5696.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5579 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 22.85 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2206 _exptl_absorpt_coefficient_mu 0.51 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 46084 _diffrn_reflns_av_R_equivalents 0.078 _diffrn_reflns_av_sigmaI/netI 0.118 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.88 _reflns_number_total 13891 _reflns_number_gt 7197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.052P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson method' _atom_sites_solution_secondary Difmap _atom_sites_solution_hydrogens 'geometrically placed, none for solvent' _refine_ls_hydrogen_treatment 'riding model, none for solvent' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13450 _refine_ls_number_parameters 664 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.116 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.109 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.889 _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 Zn1 Zn 0.724067(18) 0.759449(17) 0.823707(16) 0.02138(9) Uani 1 1 d . . . O1 O 0.69216(11) 0.70315(10) 0.89781(9) 0.0237(4) Uani 1 1 d . . . C1 C 0.82062(16) 0.80596(15) 0.95916(14) 0.0216(6) Uani 1 1 d . . . N2 N 0.89352(13) 0.83311(12) 0.99134(11) 0.0224(5) Uani 1 1 d . . . H2A H 0.9131 0.8324 1.0374 0.027 Uiso 1 1 calc R . . C3 C 0.93267(16) 0.86210(15) 0.94135(14) 0.0216(6) Uani 1 1 d . . . C4 C 0.88114(15) 0.84986(15) 0.87709(14) 0.0216(6) Uani 1 1 d . . . N5 N 0.81175(13) 0.81492(12) 0.88894(11) 0.0214(5) Uani 1 1 d . . . C6 C 1.01101(16) 0.89981(15) 0.96119(15) 0.0250(6) Uani 1 1 d . . . C7 C 1.03312(16) 0.95701(16) 0.92014(15) 0.0286(7) Uani 1 1 d . . . H7A H 0.9971 0.9721 0.8778 0.034 Uiso 1 1 calc R . . C8 C 1.10670(18) 0.99207(17) 0.94017(17) 0.0357(8) Uani 1 1 d . . . H8A H 1.1215 1.0301 0.9108 0.043 Uiso 1 1 calc R . . C9 C 1.15930(18) 0.97264(18) 1.00256(17) 0.0385(8) Uani 1 1 d . . . H9A H 1.2096 0.9977 1.0165 0.046 Uiso 1 1 calc R . . C10 C 1.13787(18) 0.91637(18) 1.04433(17) 0.0380(8) Uani 1 1 d . . . H10B H 1.1734 0.9028 1.0875 0.046 Uiso 1 1 calc R . . C11 C 1.06511(16) 0.87987(16) 1.02353(15) 0.0292(7) Uani 1 1 d . . . H11A H 1.0515 0.8405 1.0521 0.035 Uiso 1 1 calc R . . C12 C 0.88736(16) 0.86871(15) 0.80378(14) 0.0241(6) Uani 1 1 d . . . C13 C 0.95764(17) 0.85361(16) 0.77941(15) 0.0300(7) Uani 1 1 d . . . H13B H 1.0031 0.8324 0.8106 0.036 Uiso 1 1 calc R . . C14 C 0.9611(2) 0.86953(17) 0.70971(16) 0.0382(8) Uani 1 1 d . . . H14B H 1.0094 0.8598 0.6936 0.046 Uiso 1 1 calc R . . C15 C 0.8956(2) 0.89926(17) 0.66369(16) 0.0383(8) Uani 1 1 d . . . H15A H 0.8982 0.9092 0.6158 0.046 Uiso 1 1 calc R . . C16 C 0.82592(19) 0.91461(17) 0.68754(16) 0.0367(8) Uani 1 1 d . . . H16A H 0.7806 0.9356 0.6561 0.044 Uiso 1 1 calc R . . C17 C 0.82212(17) 0.89930(16) 0.75772(15) 0.0293(7) Uani 1 1 d . . . H17A H 0.7741 0.9101 0.7739 0.035 Uiso 1 1 calc R . . C18 C 0.75962(15) 0.77769(15) 0.99633(14) 0.0214(6) Uani 1 1 d . . . C19 C 0.69665(15) 0.72872(15) 0.96299(14) 0.0213(6) Uani 1 1 d . . . C20 C 0.63821(16) 0.70654(15) 1.00255(14) 0.0229(6) Uani 1 1 d . . . C21 C 0.64321(16) 0.73627(16) 1.06992(14) 0.0267(6) Uani 1 1 d . . . H21A H 0.6031 0.7221 1.0952 0.032 Uiso 1 1 calc R . . C22 C 0.70330(17) 0.78548(16) 1.10285(14) 0.0271(7) Uani 1 1 d . . . C23 C 0.76172(16) 0.80450(15) 1.06522(14) 0.0260(7) Uani 1 1 d . . . H23A H 0.8046 0.8367 1.0867 0.031 Uiso 1 1 calc R . . C24 C 0.56983(16) 0.65232(16) 0.96967(15) 0.0275(7) Uani 1 1 d . . . C25 C 0.60536(17) 0.57731(16) 0.95027(16) 0.0323(7) Uani 1 1 d . . . H25A H 0.6408 0.5867 0.9171 0.048 Uiso 1 1 calc R . . H25B H 0.5614 0.5439 0.9281 0.048 Uiso 1 1 calc R . . H25C H 0.6364 0.5537 0.9934 0.048 Uiso 1 1 calc R . . C26 C 0.51651(17) 0.68839(17) 0.90432(15) 0.0339(7) Uani 1 1 d . . . H26D H 0.4946 0.7358 0.9179 0.051 Uiso 1 1 calc R . . H26E H 0.4720 0.6544 0.8846 0.051 Uiso 1 1 calc R . . H26F H 0.5487 0.6981 0.8686 0.051 Uiso 1 1 calc R . . C27 C 0.51518(18) 0.63270(18) 1.02137(16) 0.0398(8) Uani 1 1 d . . . H27A H 0.4909 0.6787 1.0354 0.060 Uiso 1 1 calc R . . H27B H 0.5473 0.6084 1.0636 0.060 Uiso 1 1 calc R . . H27C H 0.4725 0.5985 0.9981 0.060 Uiso 1 1 calc R . . C28 C 0.7047(2) 0.82094(19) 1.17577(15) 0.0382(8) Uani 1 1 d . . . C29 C 0.6374(2) 0.7920(2) 1.20972(16) 0.0464(9) Uani 1 1 d . . . H29D H 0.6431 0.7376 1.2166 0.070 Uiso 1 1 calc R . . H29E H 0.5851 0.8031 1.1787 0.070 Uiso 1 1 calc R . . H29F H 0.6406 0.8165 1.2557 0.070 Uiso 1 1 calc R . . C30 C 0.6934(3) 0.9065(2) 1.1669(2) 0.0737(14) Uani 1 1 d . . . H30D H 0.6417 0.9170 1.1348 0.111 Uiso 1 1 calc R . . H30E H 0.7374 0.9275 1.1471 0.111 Uiso 1 1 calc R . . H30F H 0.6940 0.9294 1.2133 0.111 Uiso 1 1 calc R . . C31 C 0.7853(2) 0.8039(3) 1.22562(18) 0.0673(12) Uani 1 1 d . . . H31D H 0.7921 0.7495 1.2311 0.101 Uiso 1 1 calc R . . H31E H 0.7863 0.8268 1.2720 0.101 Uiso 1 1 calc R . . H31F H 0.8293 0.8246 1.2057 0.101 Uiso 1 1 calc R . . O1A O 0.75846(11) 0.69493(10) 0.75693(9) 0.0237(4) Uani 1 1 d . . . C1A C 0.63604(16) 0.79822(15) 0.68400(14) 0.0231(6) Uani 1 1 d . . . N2A N 0.56762(13) 0.82898(12) 0.64573(12) 0.0260(5) Uani 1 1 d . . . H2AA H 0.5527 0.8279 0.5992 0.031 Uiso 1 1 calc R . . C3A C 0.52495(16) 0.86228(15) 0.69083(15) 0.0248(6) Uani 1 1 d . . . C4A C 0.56866(16) 0.85074(15) 0.75771(15) 0.0235(6) Uani 1 1 d . . . N5A N 0.63830(13) 0.81054(12) 0.75298(11) 0.0216(5) Uani 1 1 d . . . C6A C 0.44818(16) 0.90101(16) 0.66293(15) 0.0286(7) Uani 1 1 d . . . C7A C 0.4415(2) 0.97766(18) 0.6716(2) 0.0540(10) Uani 1 1 d . . . H7AA H 0.4867 1.0056 0.6957 0.065 Uiso 1 1 calc R . . C8A C 0.3691(2) 1.0138(2) 0.6452(2) 0.0649(12) Uani 1 1 d . . . H8AA H 0.3653 1.0665 0.6511 0.078 Uiso 1 1 calc R . . C9A C 0.3035(2) 0.97479(19) 0.6109(2) 0.0561(11) Uani 1 1 d . . . H9AA H 0.2542 1.0001 0.5928 0.067 Uiso 1 1 calc R . . C10A C 0.30914(19) 0.89811(19) 0.60253(19) 0.0520(10) Uani 1 1 d . . . H10A H 0.2634 0.8704 0.5792 0.062 Uiso 1 1 calc R . . C11A C 0.38150(18) 0.86179(18) 0.62824(17) 0.0416(8) Uani 1 1 d . . . H11B H 0.3852 0.8092 0.6219 0.050 Uiso 1 1 calc R . . C12A C 0.55120(17) 0.87349(15) 0.82628(15) 0.0262(7) Uani 1 1 d . . . C13A C 0.61283(18) 0.88556(15) 0.88537(15) 0.0286(7) Uani 1 1 d . . . H13A H 0.6675 0.8808 0.8812 0.034 Uiso 1 1 calc R . . C14A C 0.5952(2) 0.90445(16) 0.95027(16) 0.0383(8) Uani 1 1 d . . . H14A H 0.6377 0.9110 0.9906 0.046 Uiso 1 1 calc R . . C15A C 0.5165(2) 0.91368(18) 0.95624(19) 0.0468(9) Uani 1 1 d . . . H15B H 0.5046 0.9266 1.0008 0.056 Uiso 1 1 calc R . . C16A C 0.4551(2) 0.90441(17) 0.8983(2) 0.0460(9) Uani 1 1 d . . . H16B H 0.4009 0.9127 0.9025 0.055 Uiso 1 1 calc R . . C17A C 0.47143(19) 0.88305(16) 0.83357(18) 0.0378(8) Uani 1 1 d . . . H17B H 0.4283 0.8749 0.7941 0.045 Uiso 1 1 calc R . . C18A C 0.69636(15) 0.76147(15) 0.65103(14) 0.0223(6) Uani 1 1 d . . . C19A C 0.75504(16) 0.71201(15) 0.68953(14) 0.0227(6) Uani 1 1 d . . . C20A C 0.81112(16) 0.67785(15) 0.65247(14) 0.0219(6) Uani 1 1 d . . . C21A C 0.80558(17) 0.69636(15) 0.58167(14) 0.0262(7) Uani 1 1 d . . . H21B H 0.8435 0.6744 0.5578 0.031 Uiso 1 1 calc R . . C22A C 0.74851(16) 0.74475(16) 0.54337(14) 0.0269(6) Uani 1 1 d . . . C23A C 0.69450(17) 0.77669(15) 0.57936(14) 0.0263(7) Uani 1 1 d . . . H23B H 0.6547 0.8101 0.5547 0.032 Uiso 1 1 calc R . . C24A C 0.87370(16) 0.62141(15) 0.69061(14) 0.0236(6) Uani 1 1 d . . . C25A C 0.92920(16) 0.65874(16) 0.75444(15) 0.0310(7) Uani 1 1 d . . . H25D H 0.9565 0.7017 0.7382 0.047 Uiso 1 1 calc R . . H25E H 0.9695 0.6224 0.7778 0.047 Uiso 1 1 calc R . . H25F H 0.8970 0.6759 0.7881 0.047 Uiso 1 1 calc R . . C26A C 0.82981(17) 0.55336(15) 0.71418(15) 0.0300(7) Uani 1 1 d . . . H26A H 0.8696 0.5172 0.7386 0.045 Uiso 1 1 calc R . . H26B H 0.7961 0.5296 0.6725 0.045 Uiso 1 1 calc R . . H26C H 0.7958 0.5701 0.7465 0.045 Uiso 1 1 calc R . . C27A C 0.92709(17) 0.59151(17) 0.64193(15) 0.0341(7) Uani 1 1 d . . . H27D H 0.9566 0.6332 0.6260 0.051 Uiso 1 1 calc R . . H27E H 0.8933 0.5670 0.6007 0.051 Uiso 1 1 calc R . . H27F H 0.9656 0.5551 0.6679 0.051 Uiso 1 1 calc R . . C28A C 0.74389(18) 0.76314(17) 0.46494(15) 0.0327(7) Uani 1 1 d . . . C29A C 0.6587(2) 0.7531(2) 0.42220(16) 0.0634(12) Uani 1 1 d . . . H29A H 0.6217 0.7847 0.4423 0.095 Uiso 1 1 calc R . . H29B H 0.6428 0.7004 0.4239 0.095 Uiso 1 1 calc R . . H29C H 0.6566 0.7678 0.3729 0.095 Uiso 1 1 calc R . . C30A C 0.8012(2) 0.7137(2) 0.43277(18) 0.0611(11) Uani 1 1 d . . . H30A H 0.7967 0.7269 0.3827 0.092 Uiso 1 1 calc R . . H30B H 0.7868 0.6608 0.4365 0.092 Uiso 1 1 calc R . . H30C H 0.8569 0.7218 0.4585 0.092 Uiso 1 1 calc R . . C31A C 0.7712(2) 0.84437(19) 0.45868(17) 0.0517(10) Uani 1 1 d . . . H31A H 0.7365 0.8782 0.4789 0.078 Uiso 1 1 calc R . . H31B H 0.7675 0.8568 0.4086 0.078 Uiso 1 1 calc R . . H31C H 0.8272 0.8500 0.4845 0.078 Uiso 1 1 calc R . . N1AS N 0.4890(2) 0.8492(2) 0.49261(16) 0.0774(12) Uani 1 1 d . . . C1AS C 0.4318(2) 0.8765(2) 0.46136(19) 0.0582(11) Uani 1 1 d . . . C2AS C 0.3581(2) 0.9127(2) 0.4224(2) 0.0667(12) Uani 1 1 d . . . N1SA N 0.96770(16) 0.83904(16) 0.15301(14) 0.0422(7) Uani 1 1 d . . . C1SA C 1.0168(2) 0.86706(18) 0.19419(17) 0.0345(8) Uani 1 1 d . . . C2SA C 1.0810(2) 0.90529(19) 0.24619(18) 0.0489(9) Uani 1 1 d . . . Cl2S Cl 0.1229(3) 1.0100(2) 0.6720(2) 0.0786(12) Uiso 0.30 1 d PD A 1 Cl1S Cl 0.1795(3) 0.9166(2) 0.7950(2) 0.0778(11) Uiso 0.30 1 d PD A 1 C3S C 0.1947(8) 0.9414(7) 0.7108(6) 0.086(5) Uiso 0.30 1 d PD A 1 N1S N 0.1026(6) 1.0166(6) 0.7040(5) 0.110(3) Uiso 0.50 1 d P B 2 C1S C 0.1484(6) 0.9717(5) 0.7332(5) 0.076(3) Uiso 0.50 1 d P B 2 C2S C 0.2126(7) 0.9162(7) 0.7688(6) 0.105(4) Uiso 0.50 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02320(15) 0.02154(18) 0.01859(16) -0.00032(15) 0.00250(12) 0.00044(15) O1 0.0303(11) 0.0211(11) 0.0200(10) -0.0009(8) 0.0060(8) -0.0033(8) C1 0.0256(15) 0.0180(15) 0.0196(15) -0.0008(12) 0.0013(12) 0.0019(12) N2 0.0256(12) 0.0214(13) 0.0185(12) 0.0006(10) 0.0007(10) 0.0001(10) C3 0.0246(14) 0.0160(15) 0.0241(15) 0.0003(12) 0.0046(12) 0.0011(12) C4 0.0220(14) 0.0174(15) 0.0255(16) -0.0005(12) 0.0049(12) 0.0000(11) N5 0.0245(12) 0.0192(13) 0.0205(13) 0.0012(10) 0.0048(10) 0.0005(10) C6 0.0244(15) 0.0216(16) 0.0291(17) -0.0054(13) 0.0058(13) 0.0020(12) C7 0.0279(16) 0.0242(17) 0.0320(18) -0.0010(13) 0.0027(13) -0.0008(13) C8 0.0357(18) 0.0254(18) 0.047(2) -0.0007(15) 0.0098(16) -0.0048(14) C9 0.0269(17) 0.0311(19) 0.055(2) -0.0135(17) 0.0035(16) -0.0067(14) C10 0.0281(17) 0.040(2) 0.042(2) -0.0027(16) -0.0032(15) 0.0026(15) C11 0.0276(16) 0.0283(18) 0.0300(17) 0.0006(14) 0.0025(13) 0.0000(13) C12 0.0287(15) 0.0189(16) 0.0249(16) -0.0036(12) 0.0063(13) -0.0083(12) C13 0.0339(17) 0.0245(17) 0.0332(18) -0.0004(14) 0.0105(14) -0.0024(13) C14 0.051(2) 0.033(2) 0.038(2) -0.0052(16) 0.0263(17) -0.0043(16) C15 0.064(2) 0.032(2) 0.0214(17) -0.0001(14) 0.0154(17) -0.0136(17) C16 0.046(2) 0.0290(19) 0.0314(19) 0.0047(15) 0.0001(15) -0.0063(15) C17 0.0323(16) 0.0287(18) 0.0266(17) -0.0004(14) 0.0057(13) -0.0059(13) C18 0.0243(14) 0.0205(16) 0.0194(15) 0.0018(12) 0.0045(12) 0.0011(11) C19 0.0230(14) 0.0196(16) 0.0198(15) 0.0014(12) 0.0011(11) 0.0025(11) C20 0.0262(15) 0.0170(15) 0.0251(16) 0.0037(12) 0.0042(12) 0.0028(12) C21 0.0273(14) 0.0277(17) 0.0268(16) 0.0072(14) 0.0097(12) 0.0011(13) C22 0.0339(16) 0.0289(17) 0.0185(15) 0.0016(13) 0.0056(13) 0.0015(13) C23 0.0281(15) 0.0245(17) 0.0240(16) -0.0015(13) 0.0020(12) -0.0032(13) C24 0.0287(16) 0.0255(17) 0.0286(17) 0.0020(13) 0.0064(13) -0.0002(13) C25 0.0336(17) 0.0244(17) 0.0376(19) 0.0025(14) 0.0049(14) -0.0036(14) C26 0.0292(16) 0.0319(19) 0.0384(19) 0.0031(15) 0.0021(14) -0.0001(14) C27 0.0384(18) 0.042(2) 0.042(2) -0.0013(16) 0.0154(16) -0.0128(16) C28 0.050(2) 0.046(2) 0.0213(16) -0.0056(15) 0.0126(15) -0.0103(17) C29 0.054(2) 0.060(2) 0.0284(18) -0.0086(17) 0.0166(16) -0.0045(18) C30 0.138(4) 0.041(2) 0.056(3) -0.017(2) 0.053(3) -0.013(3) C31 0.054(2) 0.120(4) 0.029(2) -0.017(2) 0.0082(18) -0.012(2) O1A 0.0306(11) 0.0222(11) 0.0178(10) 0.0013(8) 0.0040(8) 0.0057(8) C1A 0.0270(15) 0.0160(15) 0.0238(16) 0.0023(12) -0.0002(12) -0.0005(12) N2A 0.0301(13) 0.0216(14) 0.0222(13) -0.0018(10) -0.0034(11) 0.0043(10) C3A 0.0216(14) 0.0177(15) 0.0330(17) -0.0019(13) 0.0009(13) 0.0004(12) C4A 0.0231(14) 0.0175(15) 0.0296(17) -0.0018(13) 0.0051(13) -0.0016(12) N5A 0.0220(12) 0.0188(13) 0.0229(13) 0.0012(10) 0.0019(10) -0.0007(10) C6A 0.0261(15) 0.0189(16) 0.0365(18) -0.0036(13) -0.0033(13) 0.0023(12) C7A 0.0380(19) 0.0224(19) 0.085(3) -0.0117(18) -0.0240(18) -0.0003(15) C8A 0.049(2) 0.022(2) 0.106(3) -0.014(2) -0.025(2) 0.0109(17) C9A 0.037(2) 0.033(2) 0.085(3) -0.008(2) -0.0192(19) 0.0155(16) C10A 0.0306(18) 0.035(2) 0.079(3) -0.0124(19) -0.0145(18) -0.0010(15) C11A 0.0313(17) 0.0236(18) 0.063(2) -0.0102(16) -0.0047(16) 0.0040(14) C12A 0.0305(16) 0.0143(15) 0.0361(18) 0.0037(13) 0.0121(14) 0.0039(12) C13A 0.0394(17) 0.0184(16) 0.0299(17) 0.0020(13) 0.0115(14) 0.0078(13) C14A 0.063(2) 0.0252(18) 0.0276(18) 0.0044(14) 0.0120(16) 0.0125(16) C15A 0.078(3) 0.0262(19) 0.047(2) 0.0063(17) 0.039(2) 0.0122(18) C16A 0.050(2) 0.029(2) 0.071(3) 0.0076(19) 0.039(2) 0.0098(17) C17A 0.0370(18) 0.0253(18) 0.055(2) 0.0034(16) 0.0192(16) 0.0023(14) C18A 0.0246(13) 0.0196(15) 0.0213(14) -0.0020(12) 0.0017(11) 0.0023(12) C19A 0.0283(15) 0.0195(15) 0.0193(15) 0.0007(12) 0.0024(12) -0.0029(12) C20A 0.0255(14) 0.0176(15) 0.0218(15) -0.0020(12) 0.0033(12) -0.0032(12) C21A 0.0304(16) 0.0236(17) 0.0249(16) -0.0049(13) 0.0065(13) -0.0004(13) C22A 0.0345(15) 0.0239(17) 0.0223(15) 0.0004(13) 0.0060(12) -0.0027(13) C23A 0.0318(16) 0.0235(17) 0.0209(15) 0.0036(12) -0.0006(12) 0.0030(13) C24A 0.0263(15) 0.0196(16) 0.0247(16) -0.0016(12) 0.0048(12) 0.0026(12) C25A 0.0281(16) 0.0260(17) 0.0360(18) -0.0014(14) -0.0003(13) 0.0037(13) C26A 0.0299(16) 0.0224(17) 0.0353(18) 0.0003(14) 0.0013(13) 0.0032(13) C27A 0.0337(17) 0.0302(18) 0.0390(19) -0.0011(15) 0.0090(15) 0.0078(14) C28A 0.0451(18) 0.0324(18) 0.0217(15) 0.0058(14) 0.0092(13) 0.0038(15) C29A 0.054(2) 0.109(4) 0.0228(18) 0.010(2) -0.0017(16) -0.010(2) C30A 0.090(3) 0.061(3) 0.036(2) 0.0055(19) 0.022(2) 0.024(2) C31A 0.069(3) 0.048(2) 0.040(2) 0.0152(18) 0.0149(19) -0.001(2) N1AS 0.067(2) 0.112(3) 0.045(2) 0.002(2) -0.0074(18) 0.032(2) C1AS 0.063(3) 0.073(3) 0.034(2) -0.001(2) 0.0002(19) 0.003(2) C2AS 0.049(2) 0.083(3) 0.058(3) 0.012(2) -0.0109(19) 0.019(2) N1SA 0.0460(17) 0.0434(18) 0.0339(16) -0.0009(14) 0.0012(14) -0.0066(14) C1SA 0.042(2) 0.0304(19) 0.0315(19) 0.0079(15) 0.0082(16) 0.0033(15) C2SA 0.051(2) 0.043(2) 0.043(2) -0.0056(17) -0.0118(17) -0.0081(17) _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 Zn1 O1 1.9143(18) . y Zn1 O1A 1.9065(17) . y Zn1 N5 1.996(2) . y Zn1 N5A 1.993(2) . y O1 C19 1.324(3) . ? C1 N5 1.340(3) . ? C1 N2 1.351(3) . ? C1 C18 1.465(4) . ? N2 C3 1.380(3) . ? C3 C4 1.375(4) . ? C3 C6 1.466(4) . ? C4 N5 1.392(3) . ? C4 C12 1.478(4) . ? C6 C7 1.389(4) . ? C6 C11 1.397(4) . ? C7 C8 1.376(4) . ? C8 C9 1.383(4) . ? C9 C10 1.382(4) . ? C10 C11 1.378(4) . ? C12 C17 1.378(4) . ? C12 C13 1.395(4) . ? C13 C14 1.387(4) . ? C14 C15 1.374(4) . ? C15 C16 1.381(4) . ? C16 C17 1.395(4) . ? C18 C23 1.405(3) . ? C18 C19 1.424(4) . ? C19 C20 1.427(3) . ? C20 C21 1.389(4) . ? C20 C24 1.540(4) . ? C21 C22 1.393(4) . ? C22 C23 1.387(4) . ? C22 C28 1.537(4) . ? C24 C26 1.530(4) . ? C24 C27 1.536(4) . ? C24 C25 1.544(4) . ? C28 C29 1.520(4) . ? C28 C31 1.527(5) . ? C28 C30 1.542(5) . ? O1A C19A 1.324(3) . ? C1A N5A 1.340(3) . ? C1A N2A 1.353(3) . ? C1A C18A 1.467(4) . ? N2A C3A 1.377(3) . ? C3A C4A 1.361(4) . ? C3A C6A 1.472(4) . ? C4A N5A 1.400(3) . ? C4A C12A 1.471(4) . ? C6A C11A 1.377(4) . ? C6A C7A 1.384(4) . ? C7A C8A 1.385(4) . ? C8A C9A 1.361(4) . ? C9A C10A 1.382(4) . ? C10A C11A 1.384(4) . ? C12A C13A 1.392(4) . ? C12A C17A 1.399(4) . ? C13A C14A 1.387(4) . ? C14A C15A 1.374(4) . ? C15A C16A 1.367(5) . ? C16A C17A 1.388(4) . ? C18A C23A 1.402(3) . ? C18A C19A 1.417(4) . ? C19A C20A 1.439(4) . ? C20A C21A 1.388(4) . ? C20A C24A 1.534(4) . ? C21A C22A 1.388(4) . ? C22A C23A 1.382(4) . ? C22A C28A 1.533(4) . ? C24A C27A 1.530(4) . ? C24A C25A 1.535(4) . ? C24A C26A 1.540(4) . ? C28A C29A 1.516(4) . ? C28A C31A 1.533(4) . ? C28A C30A 1.536(4) . ? N1AS C1AS 1.138(4) . ? C1AS C2AS 1.466(5) . ? N1SA C1SA 1.139(4) . ? C1SA C2SA 1.482(4) . ? Cl2S C3S 1.777(9) . ? Cl1S C3S 1.753(9) . ? N1S C1S 1.173(11) . ? C1S C2S 1.524(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Zn1 O1 111.21(8) . . y O1A Zn1 N5A 95.52(8) . . y O1 Zn1 N5A 118.07(8) . . y O1A Zn1 N5 115.57(8) . . y O1 Zn1 N5 94.53(8) . . y N5A Zn1 N5 123.02(9) . . y C19 O1 Zn1 123.97(17) . . ? N5 C1 N2 108.6(2) . . ? N5 C1 C18 126.4(2) . . ? N2 C1 C18 124.8(2) . . ? C1 N2 C3 109.9(2) . . ? C4 C3 N2 105.2(2) . . ? C4 C3 C6 132.7(2) . . ? N2 C3 C6 122.1(2) . . ? C3 C4 N5 108.8(2) . . ? C3 C4 C12 131.8(2) . . ? N5 C4 C12 119.4(2) . . ? C1 N5 C4 107.4(2) . . ? C1 N5 Zn1 119.26(17) . . ? C4 N5 Zn1 131.43(18) . . ? C7 C6 C11 118.0(3) . . ? C7 C6 C3 121.7(3) . . ? C11 C6 C3 120.2(3) . . ? C8 C7 C6 120.7(3) . . ? C7 C8 C9 120.8(3) . . ? C10 C9 C8 119.2(3) . . ? C11 C10 C9 120.1(3) . . ? C10 C11 C6 121.1(3) . . ? C17 C12 C13 119.1(3) . . ? C17 C12 C4 119.9(2) . . ? C13 C12 C4 121.0(3) . . ? C14 C13 C12 119.9(3) . . ? C15 C14 C13 120.8(3) . . ? C14 C15 C16 119.6(3) . . ? C15 C16 C17 120.0(3) . . ? C12 C17 C16 120.6(3) . . ? C23 C18 C19 120.2(2) . . ? C23 C18 C1 117.7(2) . . ? C19 C18 C1 122.0(2) . . ? O1 C19 C18 121.9(2) . . ? O1 C19 C20 120.2(2) . . ? C18 C19 C20 117.9(2) . . ? C21 C20 C19 118.8(3) . . ? C21 C20 C24 121.2(2) . . ? C19 C20 C24 120.1(2) . . ? C20 C21 C22 124.2(2) . . ? C23 C22 C21 116.7(2) . . ? C23 C22 C28 120.1(3) . . ? C21 C22 C28 123.1(2) . . ? C22 C23 C18 122.1(3) . . ? C26 C24 C27 107.3(2) . . ? C26 C24 C20 109.8(2) . . ? C27 C24 C20 112.3(2) . . ? C26 C24 C25 111.0(2) . . ? C27 C24 C25 106.2(2) . . ? C20 C24 C25 110.2(2) . . ? C29 C28 C31 108.4(3) . . ? C29 C28 C22 112.6(3) . . ? C31 C28 C22 109.5(3) . . ? C29 C28 C30 107.3(3) . . ? C31 C28 C30 109.9(3) . . ? C22 C28 C30 109.1(3) . . ? C19A O1A Zn1 124.55(17) . . ? N5A C1A N2A 108.5(2) . . ? N5A C1A C18A 128.7(2) . . ? N2A C1A C18A 122.7(2) . . ? C1A N2A C3A 109.5(2) . . ? C4A C3A N2A 106.2(2) . . ? C4A C3A C6A 132.9(3) . . ? N2A C3A C6A 120.9(2) . . ? C3A C4A N5A 108.3(2) . . ? C3A C4A C12A 129.6(3) . . ? N5A C4A C12A 122.1(2) . . ? C1A N5A C4A 107.4(2) . . ? C1A N5A Zn1 117.98(17) . . ? C4A N5A Zn1 133.90(18) . . ? C11A C6A C7A 118.7(3) . . ? C11A C6A C3A 120.8(3) . . ? C7A C6A C3A 120.5(3) . . ? C6A C7A C8A 120.3(3) . . ? C9A C8A C7A 120.7(3) . . ? C8A C9A C10A 119.6(3) . . ? C9A C10A C11A 119.9(3) . . ? C6A C11A C10A 120.8(3) . . ? C13A C12A C17A 118.3(3) . . ? C13A C12A C4A 121.4(2) . . ? C17A C12A C4A 120.3(3) . . ? C14A C13A C12A 120.6(3) . . ? C15A C14A C13A 120.1(3) . . ? C16A C15A C14A 120.2(3) . . ? C15A C16A C17A 120.5(3) . . ? C16A C17A C12A 120.2(3) . . ? C23A C18A C19A 120.3(2) . . ? C23A C18A C1A 117.8(2) . . ? C19A C18A C1A 121.8(2) . . ? O1A C19A C18A 122.6(2) . . ? O1A C19A C20A 119.5(2) . . ? C18A C19A C20A 117.9(2) . . ? C21A C20A C19A 118.2(3) . . ? C21A C20A C24A 121.7(2) . . ? C19A C20A C24A 120.2(2) . . ? C22A C21A C20A 124.5(3) . . ? C23A C22A C21A 116.8(2) . . ? C23A C22A C28A 120.3(3) . . ? C21A C22A C28A 122.9(2) . . ? C22A C23A C18A 122.3(3) . . ? C27A C24A C20A 111.9(2) . . ? C27A C24A C25A 107.5(2) . . ? C20A C24A C25A 110.3(2) . . ? C27A C24A C26A 106.9(2) . . ? C20A C24A C26A 109.3(2) . . ? C25A C24A C26A 111.0(2) . . ? C29A C28A C31A 109.8(3) . . ? C29A C28A C22A 110.9(2) . . ? C31A C28A C22A 109.0(2) . . ? C29A C28A C30A 108.9(3) . . ? C31A C28A C30A 106.4(3) . . ? C22A C28A C30A 111.7(3) . . ? N1AS C1AS C2AS 178.9(5) . . ? N1SA C1SA C2SA 178.3(3) . . ? Cl1S C3S Cl2S 110.0(6) . . ? N1S C1S C2S 175.9(11) . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.74 _refine_diff_density_min -0.69 _refine_diff_density_rms 0.07 #end===== data_imphzn _database_code_CSD 199491 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (ZnL2)(BF4).2CH2Cl2.0.75pentane _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62.50 H70.25 B Cl4 F4 N4 O2 Zn' _chemical_formula_weight 1203.46 _refine_special_details ; Disorder was identified in the included solvent. One pentane molecule is modelled as half occupied, a second region containing pentane was modelled as two pentane sites. Each site was modelled as 0.25 occupied with all sites overlapping except one terminal Me group. Both sites lie across an inversion centre, giving 0.25 pentane in this region and 0.75 pentane in total per asymmetric unit. Suitable restraints were applied to geometry of the pentane. The R-factor reflects the generally weak nature of the diffraction data at higher scattering angles. Despite repeated efforts we have been unable so far to collect a higher quality data set for this compound. These data were collected using a relatively large crystal and long scan times. Reducing the temperature from 150K to 85K similarly had little impact on the intensity of the reflections at higher scattering angles and may reflect the degree of disordered solvent included in the crystals. ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.964(4) _cell_length_b 17.079(5) _cell_length_c 28.310(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.729(6) _cell_angle_gamma 90.00 _cell_volume 6749(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 25.6 _exptl_crystal_description column _exptl_crystal_colour green-black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2513 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details 'Bruker SADABS v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 33249 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_av_sigmaI/netI 0.0889 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.94 _reflns_number_total 15494 _reflns_number_gt 9548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1999)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.1577P)^2^+59.9605P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed, one pentane omitted' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0015(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15494 _refine_ls_number_parameters 715 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1712 _refine_ls_R_factor_gt 0.1178 _refine_ls_wR_factor_ref 0.3686 _refine_ls_wR_factor_gt 0.3306 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Zn1 Zn -0.02154(5) 0.01439(5) 0.69632(3) 0.0259(2) Uani 1 1 d . . . O1 O 0.0437(4) -0.0267(3) 0.64499(17) 0.0295(11) Uani 1 1 d . . . C1 C 0.1398(4) 0.1158(4) 0.6800(2) 0.0226(13) Uani 1 1 d . . . N2 N 0.1933(4) 0.1727(3) 0.70140(19) 0.0242(11) Uani 1 1 d . . . H2A H 0.2479 0.1908 0.6912 0.029 Uiso 1 1 calc R . . C3 C 0.1491(5) 0.1979(4) 0.7416(2) 0.0275(14) Uani 1 1 d . . . C4 C 0.0683(5) 0.1546(4) 0.7450(2) 0.0274(14) Uani 1 1 d . . . N5 N 0.0620(4) 0.1048(3) 0.70619(19) 0.0241(11) Uani 1 1 d . . . C6 C 0.1915(5) 0.2573(4) 0.7742(2) 0.0277(14) Uani 1 1 d . . . C7 C 0.1353(6) 0.2936(4) 0.8076(3) 0.0328(15) Uani 1 1 d . . . H7A H 0.0688 0.2823 0.8086 0.039 Uiso 1 1 calc R . . C8 C 0.1775(7) 0.3469(5) 0.8398(3) 0.0405(18) Uani 1 1 d . . . H8A H 0.1396 0.3709 0.8630 0.049 Uiso 1 1 calc R . . C9 C 0.2732(6) 0.3647(5) 0.8378(3) 0.0410(19) Uani 1 1 d . . . H9A H 0.3009 0.4008 0.8597 0.049 Uiso 1 1 calc R . . C10 C 0.3296(6) 0.3304(5) 0.8043(3) 0.0415(19) Uani 1 1 d . . . H10A H 0.3955 0.3435 0.8028 0.050 Uiso 1 1 calc R . . C11 C 0.2885(5) 0.2763(4) 0.7727(3) 0.0328(15) Uani 1 1 d . . . H11A H 0.3272 0.2521 0.7498 0.039 Uiso 1 1 calc R . . C12 C -0.0095(5) 0.1519(4) 0.7794(3) 0.0317(15) Uani 1 1 d . . . C13 C 0.0065(7) 0.1142(6) 0.8232(3) 0.048(2) Uani 1 1 d . . . H13A H 0.0677 0.0931 0.8314 0.058 Uiso 1 1 calc R . . C14 C -0.0676(9) 0.1084(7) 0.8541(3) 0.068(3) Uani 1 1 d . . . H14A H -0.0577 0.0820 0.8834 0.081 Uiso 1 1 calc R . . C15 C -0.1583(8) 0.1414(7) 0.8424(4) 0.062(3) Uani 1 1 d . . . H15A H -0.2089 0.1383 0.8641 0.074 Uiso 1 1 calc R . . C16 C -0.1724(7) 0.1772(6) 0.8005(4) 0.057(3) Uani 1 1 d . . . H16A H -0.2332 0.1994 0.7927 0.069 Uiso 1 1 calc R . . C17 C -0.0992(6) 0.1820(5) 0.7684(3) 0.0402(18) Uani 1 1 d . . . H17A H -0.1110 0.2064 0.7386 0.048 Uiso 1 1 calc R . . C18 C 0.1602(5) 0.0777(4) 0.6356(2) 0.0242(13) Uani 1 1 d . . . C19 C 0.1114(5) 0.0080(4) 0.6207(2) 0.0246(13) Uani 1 1 d . . . C20 C 0.1368(5) -0.0266(4) 0.5764(2) 0.0268(14) Uani 1 1 d . . . C21 C 0.2064(5) 0.0105(4) 0.5503(2) 0.0276(14) Uani 1 1 d . . . H21A H 0.2239 -0.0131 0.5214 0.033 Uiso 1 1 calc R . . C22 C 0.2521(5) 0.0800(4) 0.5636(2) 0.0252(13) Uani 1 1 d . . . C23 C 0.2295(5) 0.1118(4) 0.6069(2) 0.0254(13) Uani 1 1 d . . . H23A H 0.2616 0.1578 0.6175 0.030 Uiso 1 1 calc R . . C24 C 0.0883(5) -0.1028(4) 0.5599(3) 0.0323(15) Uani 1 1 d . . . C25 C 0.1048(6) -0.1682(4) 0.5967(3) 0.0390(18) Uani 1 1 d . . . H25A H 0.1737 -0.1763 0.6021 0.059 Uiso 1 1 calc R . . H25B H 0.0754 -0.2169 0.5850 0.059 Uiso 1 1 calc R . . H25C H 0.0757 -0.1532 0.6265 0.059 Uiso 1 1 calc R . . C26 C 0.1276(6) -0.1321(5) 0.5131(3) 0.0415(19) Uani 1 1 d . . . H26A H 0.1965 -0.1421 0.5171 0.062 Uiso 1 1 calc R . . H26B H 0.1167 -0.0923 0.4886 0.062 Uiso 1 1 calc R . . H26C H 0.0947 -0.1806 0.5037 0.062 Uiso 1 1 calc R . . C27 C -0.0201(6) -0.0881(5) 0.5506(3) 0.0369(17) Uani 1 1 d . . . H27A H -0.0288 -0.0463 0.5271 0.055 Uiso 1 1 calc R . . H27B H -0.0496 -0.0726 0.5801 0.055 Uiso 1 1 calc R . . H27C H -0.0504 -0.1362 0.5386 0.055 Uiso 1 1 calc R . . C28 C 0.3252(5) 0.1173(5) 0.5307(3) 0.0328(15) Uani 1 1 d . . . C29 C 0.3644(6) 0.1944(5) 0.5500(3) 0.0429(19) Uani 1 1 d . . . H29A H 0.3949 0.1856 0.5812 0.064 Uiso 1 1 calc R . . H29B H 0.3118 0.2319 0.5529 0.064 Uiso 1 1 calc R . . H29C H 0.4116 0.2153 0.5285 0.064 Uiso 1 1 calc R . . C30 C 0.4083(6) 0.0602(5) 0.5239(3) 0.0424(19) Uani 1 1 d . . . H30A H 0.4396 0.0490 0.5546 0.064 Uiso 1 1 calc R . . H30B H 0.4547 0.0837 0.5029 0.064 Uiso 1 1 calc R . . H30C H 0.3836 0.0114 0.5100 0.064 Uiso 1 1 calc R . . C31 C 0.2775(6) 0.1333(5) 0.4818(3) 0.0420(19) Uani 1 1 d . . . H31A H 0.3243 0.1571 0.4611 0.063 Uiso 1 1 calc R . . H31B H 0.2233 0.1691 0.4854 0.063 Uiso 1 1 calc R . . H31C H 0.2545 0.0839 0.4680 0.063 Uiso 1 1 calc R . . O1A O -0.1539(3) 0.0431(3) 0.67390(17) 0.0291(10) Uani 1 1 d . . . C1A C -0.1631(5) -0.0362(4) 0.7641(2) 0.0249(13) Uani 1 1 d . . . N2A N -0.1749(4) -0.0792(3) 0.80388(19) 0.0251(11) Uani 1 1 d . . . H2AA H -0.2294 -0.0863 0.8181 0.030 Uiso 1 1 calc R . . C3A C -0.0883(5) -0.1094(4) 0.8182(2) 0.0264(14) Uani 1 1 d . . . C4A C -0.0231(5) -0.0861(4) 0.7854(2) 0.0239(13) Uani 1 1 d . . . N5A N -0.0712(4) -0.0410(3) 0.75174(19) 0.0225(11) Uani 1 1 d . . . C6A C -0.0804(5) -0.1574(4) 0.8613(2) 0.0271(14) Uani 1 1 d . . . C7A C -0.0232(6) -0.2239(4) 0.8647(3) 0.0342(16) Uani 1 1 d . . . H7AA H 0.0139 -0.2393 0.8387 0.041 Uiso 1 1 calc R . . C8A C -0.0201(6) -0.2680(5) 0.9060(3) 0.044(2) Uani 1 1 d . . . H8AA H 0.0189 -0.3135 0.9083 0.053 Uiso 1 1 calc R . . C9A C -0.0742(6) -0.2453(6) 0.9439(3) 0.050(2) Uani 1 1 d . . . H9AA H -0.0716 -0.2755 0.9721 0.060 Uiso 1 1 calc R . . C10A C -0.1315(6) -0.1800(6) 0.9414(3) 0.051(2) Uani 1 1 d . . . H10B H -0.1687 -0.1651 0.9675 0.061 Uiso 1 1 calc R . . C11A C -0.1342(6) -0.1355(6) 0.8997(3) 0.044(2) Uani 1 1 d . . . H11B H -0.1731 -0.0900 0.8977 0.053 Uiso 1 1 calc R . . C12A C 0.0813(5) -0.0984(4) 0.7842(3) 0.0329(16) Uani 1 1 d . . . C13A C 0.1379(6) -0.0930(5) 0.8256(3) 0.0405(19) Uani 1 1 d . . . H13B H 0.1089 -0.0819 0.8548 0.049 Uiso 1 1 calc R . . C14A C 0.2360(6) -0.1037(6) 0.8242(4) 0.056(3) Uani 1 1 d . . . H14B H 0.2741 -0.1008 0.8526 0.067 Uiso 1 1 calc R . . C15A C 0.2780(7) -0.1184(6) 0.7823(5) 0.067(3) Uani 1 1 d . . . H15B H 0.3455 -0.1250 0.7816 0.080 Uiso 1 1 calc R . . C16A C 0.2233(7) -0.1240(6) 0.7405(4) 0.057(3) Uani 1 1 d . . . H16B H 0.2526 -0.1347 0.7113 0.069 Uiso 1 1 calc R . . C17A C 0.1258(6) -0.1137(5) 0.7424(3) 0.0419(19) Uani 1 1 d . . . H17B H 0.0880 -0.1172 0.7140 0.050 Uiso 1 1 calc R . . C18A C -0.2407(5) 0.0093(4) 0.7425(2) 0.0256(13) Uani 1 1 d . . . C19A C -0.2303(5) 0.0470(4) 0.6970(2) 0.0245(13) Uani 1 1 d . . . C20A C -0.3105(5) 0.0917(4) 0.6767(2) 0.0271(14) Uani 1 1 d . . . C21A C -0.3904(5) 0.0990(4) 0.7036(3) 0.0344(16) Uani 1 1 d . . . H21B H -0.4426 0.1290 0.6912 0.041 Uiso 1 1 calc R . . C22A C -0.3995(5) 0.0647(5) 0.7484(3) 0.0337(16) Uani 1 1 d . . . C23A C -0.3250(5) 0.0190(4) 0.7662(2) 0.0295(14) Uani 1 1 d . . . H23B H -0.3321 -0.0065 0.7957 0.035 Uiso 1 1 calc R . . C24A C -0.3033(6) 0.1282(5) 0.6276(3) 0.0367(17) Uani 1 1 d . . . C25A C -0.3974(7) 0.1699(8) 0.6127(4) 0.067(3) Uani 1 1 d . . . H25D H -0.4502 0.1321 0.6123 0.101 Uiso 1 1 calc R . . H25E H -0.3913 0.1923 0.5810 0.101 Uiso 1 1 calc R . . H25F H -0.4105 0.2118 0.6352 0.101 Uiso 1 1 calc R . . C26A C -0.2868(7) 0.0643(6) 0.5905(3) 0.048(2) Uani 1 1 d . . . H26D H -0.3399 0.0268 0.5906 0.072 Uiso 1 1 calc R . . H26E H -0.2265 0.0371 0.5980 0.072 Uiso 1 1 calc R . . H26F H -0.2836 0.0884 0.5591 0.072 Uiso 1 1 calc R . . C27A C -0.2204(7) 0.1885(5) 0.6280(3) 0.052(2) Uani 1 1 d . . . H27D H -0.1602 0.1624 0.6373 0.077 Uiso 1 1 calc R . . H27E H -0.2336 0.2304 0.6505 0.077 Uiso 1 1 calc R . . H27F H -0.2148 0.2109 0.5963 0.077 Uiso 1 1 calc R . . C28A C -0.4882(6) 0.0825(5) 0.7766(3) 0.044(2) Uani 1 1 d . . . C29A C -0.5798(6) 0.0697(7) 0.7467(4) 0.064(3) Uani 1 1 d . . . H29D H -0.5845 0.0145 0.7374 0.096 Uiso 1 1 calc R . . H29E H -0.5784 0.1025 0.7184 0.096 Uiso 1 1 calc R . . H29F H -0.6355 0.0838 0.7652 0.096 Uiso 1 1 calc R . . C30A C -0.4934(8) 0.0330(8) 0.8216(4) 0.080(4) Uani 1 1 d . . . H30D H -0.4975 -0.0225 0.8131 0.121 Uiso 1 1 calc R . . H30E H -0.5502 0.0480 0.8390 0.121 Uiso 1 1 calc R . . H30F H -0.4358 0.0420 0.8415 0.121 Uiso 1 1 calc R . . C31A C -0.4821(7) 0.1705(6) 0.7912(4) 0.057(3) Uani 1 1 d . . . H31D H -0.4792 0.2031 0.7627 0.085 Uiso 1 1 calc R . . H31E H -0.4244 0.1791 0.8111 0.085 Uiso 1 1 calc R . . H31F H -0.5389 0.1846 0.8088 0.085 Uiso 1 1 calc R . . C1P C 0.374(4) -0.265(3) 0.5210(16) 0.082(14) Uiso 0.25 1 d PD . . H1PA H 0.4025 -0.3145 0.5113 0.124 Uiso 0.25 1 calc PR . . H1PB H 0.3852 -0.2248 0.4970 0.124 Uiso 0.25 1 calc PR . . H1PC H 0.3050 -0.2717 0.5246 0.124 Uiso 0.25 1 calc PR . . C2P C 0.414(3) -0.242(2) 0.5622(14) 0.082(14) Uiso 0.25 1 d PD . . H2PA H 0.4829 -0.2372 0.5548 0.099 Uiso 0.25 1 calc PR . . H2PB H 0.4102 -0.2897 0.5820 0.099 Uiso 0.25 1 calc PR . . C3P C 0.401(3) -0.184(2) 0.5930(14) 0.085(15) Uiso 0.25 1 d PD . . H3PA H 0.3876 -0.2127 0.6225 0.102 Uiso 0.25 1 calc PR . . H3PB H 0.3390 -0.1618 0.5823 0.102 Uiso 0.25 1 calc PR . . C4P C 0.450(2) -0.1216(16) 0.6087(11) 0.043(7) Uiso 0.25 1 d PD . . H4PA H 0.4598 -0.0905 0.5797 0.052 Uiso 0.25 1 calc PR . . H4PB H 0.5136 -0.1427 0.6179 0.052 Uiso 0.25 1 calc PR . . C5P C 0.433(2) -0.0673(16) 0.6418(9) 0.030(6) Uiso 0.25 1 d PD . . H5PA H 0.4870 -0.0304 0.6436 0.045 Uiso 0.25 1 calc PR . . H5PB H 0.4268 -0.0930 0.6725 0.045 Uiso 0.25 1 calc PR . . H5PC H 0.3741 -0.0390 0.6335 0.045 Uiso 0.25 1 calc PR . . Cl1S Cl 0.1374(2) 0.18775(18) 0.92786(10) 0.0695(8) Uani 1 1 d . . . Cl2S Cl 0.2651(3) 0.0890(2) 0.87591(15) 0.1012(12) Uani 1 1 d . . . C1S C 0.2483(9) 0.1782(6) 0.9038(5) 0.071(3) Uani 1 1 d . . . H1SA H 0.2981 0.1844 0.9292 0.085 Uiso 1 1 calc R . . H1SB H 0.2571 0.2209 0.8807 0.085 Uiso 1 1 calc R . . C2S C 0.6013(15) -0.0526(13) 0.9454(7) 0.075(5) Uiso 0.60 1 d P A 1 H2SA H 0.5339 -0.0348 0.9425 0.090 Uiso 0.60 1 calc PR A 1 H2SB H 0.6077 -0.1023 0.9278 0.090 Uiso 0.60 1 calc PR A 1 Cl3S Cl 0.6850(5) 0.0245(4) 0.9217(3) 0.0933(18) Uiso 0.60 1 d P A 1 Cl4S Cl 0.6348(10) -0.0647(7) 1.0028(4) 0.156(4) Uiso 0.60 1 d P A 1 C2S' C 0.698(4) -0.054(4) 0.980(2) 0.15(2) Uiso 0.40 1 d P B 2 H2SC H 0.7379 -0.0322 1.0065 0.185 Uiso 0.40 1 calc PR B 2 H2SD H 0.7323 -0.0980 0.9662 0.185 Uiso 0.40 1 calc PR B 2 Cl3' Cl 0.6821(12) 0.0029(10) 0.9468(6) 0.142(5) Uiso 0.40 1 d P B 2 Cl4' Cl 0.5690(12) -0.0922(10) 1.0055(6) 0.145(5) Uiso 0.40 1 d P B 2 B1 B 0.4172(6) 0.1852(6) 1.1660(4) 0.040(2) Uani 1 1 d . . . F1 F 0.3784(4) 0.2609(3) 1.16870(19) 0.0553(14) Uani 1 1 d . . . F2 F 0.3426(4) 0.1318(3) 1.16040(19) 0.0544(14) Uani 1 1 d . . . F3 F 0.4656(4) 0.1690(4) 1.2079(2) 0.079(2) Uani 1 1 d . . . F4 F 0.4758(4) 0.1778(3) 1.1288(2) 0.0647(17) Uani 1 1 d . . . C6P C -0.0358(19) 0.0286(17) 0.9967(10) 0.082(7) Uiso 0.50 1 d P . . C7P C -0.095(3) 0.059(2) 1.0341(14) 0.120(12) Uiso 0.50 1 d P . . C8P C -0.149(3) 0.112(2) 1.0312(13) 0.048(8) Uiso 0.25 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 Zn1 0.0252(4) 0.0244(4) 0.0284(4) 0.0026(3) 0.0062(3) -0.0024(3) O1 0.036(3) 0.023(3) 0.030(2) 0.0043(19) 0.007(2) -0.003(2) C1 0.023(3) 0.018(3) 0.027(3) 0.000(2) 0.002(3) -0.001(2) N2 0.020(3) 0.025(3) 0.028(3) -0.001(2) 0.000(2) -0.002(2) C3 0.031(3) 0.022(3) 0.029(3) -0.002(3) 0.000(3) 0.005(3) C4 0.038(4) 0.021(3) 0.023(3) 0.001(3) -0.002(3) 0.001(3) N5 0.025(3) 0.023(3) 0.025(3) 0.002(2) 0.004(2) 0.001(2) C6 0.033(4) 0.022(3) 0.028(3) 0.002(3) -0.003(3) -0.001(3) C7 0.039(4) 0.028(4) 0.032(4) -0.002(3) 0.004(3) 0.003(3) C8 0.060(5) 0.030(4) 0.032(4) -0.006(3) 0.003(4) 0.002(4) C9 0.056(5) 0.028(4) 0.038(4) -0.005(3) -0.007(4) -0.004(4) C10 0.040(4) 0.037(4) 0.047(5) 0.002(4) -0.008(4) -0.006(3) C11 0.033(4) 0.029(4) 0.036(4) -0.002(3) -0.002(3) 0.000(3) C12 0.040(4) 0.023(3) 0.033(4) -0.005(3) 0.007(3) -0.004(3) C13 0.058(5) 0.054(5) 0.032(4) -0.006(4) 0.008(4) -0.015(4) C14 0.099(9) 0.075(7) 0.031(5) -0.007(4) 0.022(5) -0.038(7) C15 0.065(7) 0.062(7) 0.061(6) -0.024(5) 0.034(5) -0.025(5) C16 0.046(5) 0.050(6) 0.078(7) -0.024(5) 0.022(5) -0.003(4) C17 0.041(4) 0.036(4) 0.044(4) -0.011(3) 0.012(4) -0.004(3) C18 0.027(3) 0.022(3) 0.023(3) 0.003(2) -0.001(3) -0.001(3) C19 0.023(3) 0.027(3) 0.024(3) 0.002(3) -0.001(2) -0.003(3) C20 0.030(3) 0.023(3) 0.027(3) 0.002(3) 0.000(3) 0.003(3) C21 0.027(3) 0.029(3) 0.027(3) -0.005(3) 0.005(3) 0.000(3) C22 0.021(3) 0.027(3) 0.028(3) -0.001(3) 0.002(3) -0.002(3) C23 0.022(3) 0.026(3) 0.029(3) -0.004(3) 0.002(3) -0.003(3) C24 0.033(4) 0.032(4) 0.033(4) -0.006(3) 0.003(3) -0.005(3) C25 0.051(5) 0.026(4) 0.040(4) -0.002(3) 0.005(4) -0.003(3) C26 0.047(5) 0.043(5) 0.036(4) -0.016(3) 0.007(3) -0.013(4) C27 0.039(4) 0.040(4) 0.033(4) -0.002(3) 0.004(3) -0.012(3) C28 0.028(4) 0.038(4) 0.033(4) -0.001(3) 0.008(3) -0.004(3) C29 0.038(4) 0.039(5) 0.052(5) 0.001(4) 0.014(4) -0.010(3) C30 0.038(4) 0.043(5) 0.047(5) -0.001(4) 0.015(4) 0.001(4) C31 0.041(4) 0.049(5) 0.036(4) 0.003(4) 0.011(3) -0.008(4) O1A 0.027(2) 0.033(3) 0.028(2) 0.005(2) 0.0034(19) 0.001(2) C1A 0.027(3) 0.021(3) 0.027(3) -0.003(2) 0.006(3) 0.000(2) N2A 0.026(3) 0.024(3) 0.026(3) 0.001(2) 0.001(2) 0.000(2) C3A 0.032(3) 0.022(3) 0.026(3) 0.001(3) 0.000(3) -0.004(3) C4A 0.027(3) 0.023(3) 0.021(3) 0.001(2) -0.002(3) -0.003(3) N5A 0.021(3) 0.020(3) 0.026(3) 0.001(2) 0.000(2) 0.001(2) C6A 0.029(3) 0.030(4) 0.022(3) 0.004(3) 0.003(3) -0.004(3) C7A 0.040(4) 0.030(4) 0.032(4) 0.004(3) -0.006(3) -0.004(3) C8A 0.039(4) 0.039(5) 0.052(5) 0.022(4) -0.015(4) -0.005(3) C9A 0.047(5) 0.061(6) 0.041(5) 0.026(4) -0.013(4) -0.004(4) C10A 0.042(5) 0.077(7) 0.033(4) 0.015(4) 0.007(4) 0.006(4) C11A 0.041(4) 0.056(5) 0.035(4) 0.011(4) 0.003(3) 0.008(4) C12A 0.024(3) 0.028(4) 0.046(4) 0.009(3) 0.000(3) -0.001(3) C13A 0.034(4) 0.034(4) 0.053(5) 0.011(4) -0.009(4) -0.011(3) C14A 0.032(4) 0.049(5) 0.087(7) 0.019(5) -0.011(5) -0.003(4) C15A 0.027(4) 0.055(6) 0.117(10) 0.020(6) 0.000(5) -0.004(4) C16A 0.043(5) 0.048(6) 0.082(7) 0.013(5) 0.022(5) 0.006(4) C17A 0.036(4) 0.042(5) 0.048(5) 0.015(4) 0.006(4) 0.006(3) C18A 0.028(3) 0.022(3) 0.026(3) -0.001(3) 0.000(3) -0.001(3) C19A 0.025(3) 0.023(3) 0.026(3) -0.005(3) -0.001(3) 0.001(3) C20A 0.025(3) 0.030(4) 0.026(3) 0.002(3) 0.003(3) 0.002(3) C21A 0.027(4) 0.033(4) 0.044(4) 0.006(3) -0.001(3) 0.011(3) C22A 0.026(3) 0.034(4) 0.041(4) 0.005(3) 0.007(3) 0.005(3) C23A 0.032(3) 0.026(3) 0.030(3) 0.003(3) 0.005(3) 0.002(3) C24A 0.041(4) 0.035(4) 0.034(4) 0.012(3) 0.003(3) 0.007(3) C25A 0.050(6) 0.096(9) 0.057(6) 0.035(6) 0.012(5) 0.031(6) C26A 0.057(5) 0.055(6) 0.032(4) 0.004(4) 0.002(4) 0.007(4) C27A 0.064(6) 0.035(5) 0.056(5) 0.015(4) 0.002(4) -0.006(4) C28A 0.041(4) 0.046(5) 0.046(5) 0.010(4) 0.018(4) 0.016(4) C29A 0.033(5) 0.075(7) 0.084(7) 0.010(6) 0.020(5) 0.005(5) C30A 0.068(7) 0.090(9) 0.087(8) 0.050(7) 0.053(6) 0.042(6) C31A 0.055(6) 0.056(6) 0.060(6) -0.011(5) 0.014(5) 0.019(5) Cl1S 0.0814(19) 0.0736(18) 0.0542(14) -0.0119(13) 0.0130(13) 0.0024(15) Cl2S 0.086(2) 0.100(3) 0.119(3) -0.025(2) 0.022(2) 0.029(2) C1S 0.080(8) 0.040(6) 0.095(9) 0.008(6) 0.010(7) -0.002(5) B1 0.030(4) 0.037(5) 0.054(6) 0.003(4) 0.006(4) 0.001(4) F1 0.064(3) 0.043(3) 0.060(3) 0.009(2) 0.021(3) 0.017(2) F2 0.040(3) 0.062(3) 0.062(3) 0.013(3) 0.009(2) -0.015(2) F3 0.067(4) 0.089(5) 0.079(4) -0.028(4) -0.036(3) 0.040(3) F4 0.058(3) 0.042(3) 0.096(4) -0.011(3) 0.043(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.875(5) . ? Zn1 N5 1.950(6) . ? Zn1 N5A 1.976(5) . ? Zn1 O1A 1.997(5) . ? O1 C19 1.325(8) . ? C1 N5 1.347(8) . ? C1 N2 1.356(8) . ? C1 C18 1.453(9) . ? N2 C3 1.379(9) . ? C3 C4 1.355(10) . ? C3 C6 1.484(9) . ? C4 N5 1.390(8) . ? C4 C12 1.481(10) . ? C6 C7 1.391(10) . ? C6 C11 1.395(10) . ? C7 C8 1.406(11) . ? C8 C9 1.373(12) . ? C9 C10 1.380(12) . ? C10 C11 1.398(11) . ? C12 C17 1.381(11) . ? C12 C13 1.408(12) . ? C13 C14 1.378(13) . ? C14 C15 1.417(17) . ? C15 C16 1.344(16) . ? C16 C17 1.390(12) . ? C18 C23 1.408(9) . ? C18 C19 1.429(9) . ? C19 C20 1.440(9) . ? C20 C21 1.392(10) . ? C20 C24 1.533(10) . ? C21 C22 1.395(9) . ? C22 C23 1.385(9) . ? C22 C28 1.540(9) . ? C24 C26 1.533(10) . ? C24 C25 1.542(11) . ? C24 C27 1.548(11) . ? C28 C29 1.522(11) . ? C28 C30 1.532(11) . ? C28 C31 1.541(11) . ? O1A C19A 1.269(8) . ? C1A N5A 1.342(8) . ? C1A N2A 1.358(9) . ? C1A C18A 1.453(9) . ? N2A C3A 1.366(9) . ? C3A C4A 1.379(9) . ? C3A C6A 1.471(9) . ? C4A N5A 1.383(8) . ? C4A C12A 1.474(9) . ? C6A C7A 1.391(10) . ? C6A C11A 1.391(11) . ? C7A C8A 1.391(10) . ? C8A C9A 1.385(13) . ? C9A C10A 1.374(14) . ? C10A C11A 1.403(11) . ? C12A C17A 1.377(11) . ? C12A C13A 1.396(11) . ? C13A C14A 1.384(12) . ? C14A C15A 1.363(16) . ? C15A C16A 1.394(16) . ? C16A C17A 1.375(12) . ? C18A C23A 1.383(9) . ? C18A C19A 1.452(9) . ? C19A C20A 1.459(9) . ? C20A C21A 1.377(10) . ? C20A C24A 1.530(10) . ? C21A C22A 1.405(11) . ? C22A C23A 1.383(10) . ? C22A C28A 1.524(10) . ? C24A C26A 1.537(12) . ? C24A C25A 1.543(11) . ? C24A C27A 1.549(12) . ? C28A C29A 1.528(14) . ? C28A C30A 1.532(13) . ? C28A C31A 1.560(14) . ? C1P C2P 1.33(2) . ? C2P C3P 1.33(2) . ? C3P C4P 1.34(2) . ? C4P C5P 1.34(2) . ? Cl1S C1S 1.719(12) . ? Cl2S C1S 1.736(12) . ? C2S Cl4S 1.69(2) . ? C2S Cl3S 1.90(2) . ? C2S' Cl3' 1.36(6) . ? C2S' Cl4' 2.06(6) . ? B1 F4 1.359(11) . ? B1 F3 1.375(12) . ? B1 F2 1.391(11) . ? B1 F1 1.404(11) . ? C6P C6P 1.41(5) 3_557 ? C6P C7P 1.46(4) . ? C7P C8P 1.18(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N5 96.0(2) . . ? O1 Zn1 N5A 128.8(2) . . ? N5 Zn1 N5A 119.2(2) . . ? O1 Zn1 O1A 108.2(2) . . ? N5 Zn1 O1A 113.3(2) . . ? N5A Zn1 O1A 91.5(2) . . ? C19 O1 Zn1 127.3(4) . . ? N5 C1 N2 107.3(6) . . ? N5 C1 C18 126.6(6) . . ? N2 C1 C18 126.0(6) . . ? C1 N2 C3 109.7(6) . . ? C4 C3 N2 106.5(6) . . ? C4 C3 C6 130.3(6) . . ? N2 C3 C6 123.1(6) . . ? C3 C4 N5 108.1(6) . . ? C3 C4 C12 133.9(6) . . ? N5 C4 C12 118.0(6) . . ? C1 N5 C4 108.4(6) . . ? C1 N5 Zn1 121.4(4) . . ? C4 N5 Zn1 128.4(5) . . ? C7 C6 C11 119.1(7) . . ? C7 C6 C3 120.3(6) . . ? C11 C6 C3 120.6(6) . . ? C6 C7 C8 119.6(7) . . ? C9 C8 C7 120.4(8) . . ? C8 C9 C10 120.7(7) . . ? C9 C10 C11 119.3(8) . . ? C6 C11 C10 120.9(7) . . ? C17 C12 C13 119.2(8) . . ? C17 C12 C4 121.2(7) . . ? C13 C12 C4 119.5(7) . . ? C14 C13 C12 119.3(10) . . ? C13 C14 C15 120.4(10) . . ? C16 C15 C14 119.5(9) . . ? C15 C16 C17 120.9(10) . . ? C12 C17 C16 120.7(9) . . ? C23 C18 C19 120.3(6) . . ? C23 C18 C1 118.1(6) . . ? C19 C18 C1 121.6(6) . . ? O1 C19 C18 124.1(6) . . ? O1 C19 C20 117.8(6) . . ? C18 C19 C20 118.1(6) . . ? C21 C20 C19 118.1(6) . . ? C21 C20 C24 122.2(6) . . ? C19 C20 C24 119.8(6) . . ? C20 C21 C22 124.4(6) . . ? C23 C22 C21 117.3(6) . . ? C23 C22 C28 123.1(6) . . ? C21 C22 C28 119.6(6) . . ? C22 C23 C18 121.8(6) . . ? C26 C24 C20 112.0(6) . . ? C26 C24 C25 107.3(6) . . ? C20 C24 C25 110.7(6) . . ? C26 C24 C27 106.2(6) . . ? C20 C24 C27 109.6(6) . . ? C25 C24 C27 110.9(6) . . ? C29 C28 C30 109.3(6) . . ? C29 C28 C22 112.2(6) . . ? C30 C28 C22 109.3(6) . . ? C29 C28 C31 108.1(7) . . ? C30 C28 C31 108.0(7) . . ? C22 C28 C31 109.9(6) . . ? C19A O1A Zn1 129.3(4) . . ? N5A C1A N2A 108.9(6) . . ? N5A C1A C18A 129.0(6) . . ? N2A C1A C18A 122.0(6) . . ? C1A N2A C3A 108.7(6) . . ? N2A C3A C4A 106.7(6) . . ? N2A C3A C6A 120.0(6) . . ? C4A C3A C6A 133.3(6) . . ? C3A C4A N5A 107.9(6) . . ? C3A C4A C12A 130.4(6) . . ? N5A C4A C12A 121.6(6) . . ? C1A N5A C4A 107.6(5) . . ? C1A N5A Zn1 122.6(4) . . ? C4A N5A Zn1 129.7(4) . . ? C7A C6A C11A 119.2(7) . . ? C7A C6A C3A 122.8(6) . . ? C11A C6A C3A 118.0(7) . . ? C6A C7A C8A 120.2(8) . . ? C9A C8A C7A 119.7(8) . . ? C10A C9A C8A 121.2(7) . . ? C9A C10A C11A 118.9(8) . . ? C6A C11A C10A 120.7(8) . . ? C17A C12A C13A 118.4(7) . . ? C17A C12A C4A 121.2(7) . . ? C13A C12A C4A 120.4(7) . . ? C14A C13A C12A 120.2(9) . . ? C15A C14A C13A 120.1(10) . . ? C14A C15A C16A 120.8(9) . . ? C17A C16A C15A 118.4(10) . . ? C16A C17A C12A 122.1(9) . . ? C23A C18A C19A 119.1(6) . . ? C23A C18A C1A 119.7(6) . . ? C19A C18A C1A 121.1(6) . . ? O1A C19A C18A 122.8(6) . . ? O1A C19A C20A 118.2(6) . . ? C18A C19A C20A 119.0(6) . . ? C21A C20A C19A 117.0(6) . . ? C21A C20A C24A 122.9(6) . . ? C19A C20A C24A 120.0(6) . . ? C20A C21A C22A 124.0(6) . . ? C23A C22A C21A 118.5(6) . . ? C23A C22A C28A 122.4(7) . . ? C21A C22A C28A 119.1(6) . . ? C22A C23A C18A 122.2(7) . . ? C20A C24A C26A 110.3(6) . . ? C20A C24A C25A 111.0(7) . . ? C26A C24A C25A 106.5(8) . . ? C20A C24A C27A 109.5(7) . . ? C26A C24A C27A 110.5(7) . . ? C25A C24A C27A 109.0(8) . . ? C22A C28A C29A 111.2(7) . . ? C22A C28A C30A 112.7(7) . . ? C29A C28A C30A 108.7(9) . . ? C22A C28A C31A 107.0(7) . . ? C29A C28A C31A 108.8(8) . . ? C30A C28A C31A 108.3(9) . . ? C1P C2P C3P 136(4) . . ? C2P C3P C4P 137(4) . . ? C3P C4P C5P 134(3) . . ? Cl1S C1S Cl2S 113.5(7) . . ? Cl4S C2S Cl3S 105.7(13) . . ? Cl3' C2S' Cl4' 110(4) . . ? F4 B1 F3 111.0(8) . . ? F4 B1 F2 108.4(8) . . ? F3 B1 F2 108.2(8) . . ? F4 B1 F1 111.7(7) . . ? F3 B1 F1 108.6(8) . . ? F2 B1 F1 108.7(7) . . ? C6P C6P C7P 124(3) 3_557 . ? C8P C7P C6P 127(4) . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.691 _refine_diff_density_min -1.017 _refine_diff_density_rms 0.171