# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 N10 O18 Zn3' _chemical_formula_weight 1046.83 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.908(4) _cell_length_b 10.0503(18) _cell_length_c 17.068(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4101.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.238 _exptl_crystal_size_mid 0.108 _exptl_crystal_size_min 0.079 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 1.829 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17172 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 23.66 _reflns_number_total 3094 _reflns_number_gt 2106 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+5.4852P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3094 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.87597(3) 0.18852(7) 0.96341(4) 0.0385(2) Uani 1 1 d . . . Zn2 Zn 1.0000 -0.09184(10) 0.7500 0.0390(3) Uani 1 2 d S . . O1 O 0.90232(18) 0.3158(4) 1.0522(2) 0.0535(12) Uani 1 1 d . . . H1E H 0.9144 0.2700 1.0905 0.080 Uiso 1 1 d R . . H1F H 0.9284 0.3654 1.0350 0.080 Uiso 1 1 d R . . O2 O 0.86629(15) 0.0535(4) 0.8682(2) 0.0398(10) Uani 1 1 d . . . O3 O 0.95793(16) 0.1523(5) 0.9335(2) 0.0493(12) Uani 1 1 d . . . O4 O 0.91818(15) -0.0626(4) 0.7835(2) 0.0434(10) Uani 1 1 d . . . O5 O 1.01630(18) -0.2529(4) 0.8253(2) 0.0494(11) Uani 1 1 d . . . O6 O 0.9892(2) -0.4658(5) 0.8332(4) 0.106(2) Uani 1 1 d . . . O7 O 0.98911(15) 0.0428(4) 0.6526(2) 0.0479(11) Uani 1 1 d . . . O1W O 0.9429(3) 0.5634(6) 1.0489(5) 0.162(4) Uani 1 1 d . . . H1WA H 0.9598 0.5007 1.0253 0.243 Uiso 1 1 d R . . H1WB H 0.9107 0.5744 1.0287 0.243 Uiso 1 1 d R . . O2W O 0.0421(3) 0.2165(8) 0.0349(4) 0.129(3) Uani 1 1 d . . . H2WA H 0.0308 0.2408 0.0869 0.194 Uiso 1 1 d R . . H2WB H 0.0282 0.2810 -0.0018 0.194 Uiso 1 1 d R . . N1 N 0.8762(2) -0.0501(5) 1.1001(3) 0.0435(13) Uani 1 1 d . . . H1D H 0.9117 -0.0623 1.1041 0.052 Uiso 1 1 calc R . . N2 N 0.85330(19) 0.0410(5) 1.0527(3) 0.0402(13) Uani 1 1 d . . . N3 N 0.78869(18) 0.2012(5) 0.9719(3) 0.0342(11) Uani 1 1 d . . . N4 N 0.85168(19) 0.3613(5) 0.8879(3) 0.0397(12) Uani 1 1 d . . . N5 N 0.8736(2) 0.4551(5) 0.8405(3) 0.0467(13) Uani 1 1 d . . . H5A H 0.9089 0.4687 0.8347 0.056 Uiso 1 1 calc R . . C1 C 0.8544(3) -0.2295(7) 1.1944(4) 0.064(2) Uani 1 1 d . . . H1A H 0.8917 -0.2141 1.2136 0.096 Uiso 1 1 calc R . . H1B H 0.8533 -0.3127 1.1668 0.096 Uiso 1 1 calc R . . H1C H 0.8288 -0.2323 1.2377 0.096 Uiso 1 1 calc R . . C2 C 0.8383(3) -0.1204(6) 1.1406(4) 0.0450(16) Uani 1 1 d . . . C3 C 0.7874(3) -0.0722(6) 1.1174(4) 0.0474(17) Uani 1 1 d . . . H3 H 0.7524 -0.1006 1.1342 0.057 Uiso 1 1 calc R . . C4 C 0.7986(2) 0.0269(6) 1.0640(3) 0.0359(14) Uani 1 1 d . . . C5 C 0.7614(2) 0.1150(6) 1.0176(3) 0.0379(15) Uani 1 1 d . . . C6 C 0.7036(2) 0.1114(6) 1.0191(4) 0.0422(16) Uani 1 1 d . . . H6 H 0.6847 0.0504 1.0504 0.051 Uiso 1 1 calc R . . C7 C 0.6744(3) 0.2013(6) 0.9726(4) 0.0483(17) Uani 1 1 d . . . H7 H 0.6355 0.2015 0.9730 0.058 Uiso 1 1 calc R . . C8 C 0.7029(2) 0.2896(6) 0.9261(4) 0.0427(16) Uani 1 1 d . . . H8 H 0.6838 0.3506 0.8951 0.051 Uiso 1 1 calc R . . C9 C 0.7602(2) 0.2862(6) 0.9265(4) 0.0379(15) Uani 1 1 d . . . C10 C 0.7964(2) 0.3744(6) 0.8799(3) 0.0372(14) Uani 1 1 d . . . C11 C 0.7834(3) 0.4748(6) 0.8274(4) 0.0432(16) Uani 1 1 d . . . H11 H 0.7479 0.5022 0.8120 0.052 Uiso 1 1 calc R . . C12 C 0.8333(3) 0.5252(6) 0.8029(4) 0.0493(17) Uani 1 1 d . . . C13 C 0.8476(3) 0.6348(7) 0.7479(4) 0.067(2) Uani 1 1 d . . . H13A H 0.8756 0.6907 0.7711 0.101 Uiso 1 1 calc R . . H13B H 0.8147 0.6864 0.7371 0.101 Uiso 1 1 calc R . . H13C H 0.8617 0.5978 0.6999 0.101 Uiso 1 1 calc R . . C14 C 0.9117(2) 0.0159(6) 0.8394(4) 0.0365(14) Uani 1 1 d . . . C15 C 1.0014(3) -0.3634(8) 0.7957(4) 0.066(2) Uani 1 1 d . . . C16 C 1.0353(2) 0.0754(6) 0.6232(4) 0.0398(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0270(4) 0.0530(5) 0.0355(4) -0.0025(4) 0.0036(3) 0.0013(3) Zn2 0.0346(6) 0.0452(6) 0.0373(6) 0.000 0.0044(5) 0.000 O1 0.053(3) 0.069(3) 0.039(3) -0.006(2) -0.003(2) 0.003(2) O2 0.025(2) 0.048(2) 0.047(3) 0.001(2) 0.0065(19) -0.0001(18) O3 0.031(2) 0.075(3) 0.042(3) -0.025(3) 0.002(2) 0.002(2) O4 0.033(2) 0.051(3) 0.046(3) -0.011(2) 0.005(2) -0.005(2) O5 0.055(3) 0.048(3) 0.045(3) 0.002(2) -0.007(2) 0.000(2) O6 0.110(5) 0.076(4) 0.131(6) 0.054(4) -0.056(4) -0.036(3) O7 0.026(2) 0.064(3) 0.054(3) 0.018(2) 0.002(2) -0.001(2) O1W 0.127(6) 0.093(5) 0.265(11) 0.000(6) -0.112(7) -0.011(4) O2W 0.080(5) 0.192(8) 0.115(6) 0.010(5) -0.002(4) -0.018(5) N1 0.038(3) 0.050(3) 0.043(3) 0.008(3) -0.006(3) 0.006(3) N2 0.032(3) 0.051(3) 0.037(3) 0.011(3) 0.002(2) 0.003(2) N3 0.030(3) 0.040(3) 0.033(3) -0.005(2) 0.003(2) -0.001(2) N4 0.038(3) 0.045(3) 0.036(3) -0.003(3) 0.004(2) -0.004(2) N5 0.047(3) 0.050(3) 0.044(3) -0.003(3) 0.004(3) -0.011(3) C1 0.086(6) 0.065(5) 0.040(4) 0.014(4) -0.012(4) -0.009(4) C2 0.048(4) 0.052(4) 0.034(4) 0.009(3) -0.002(3) -0.009(3) C3 0.046(4) 0.051(4) 0.045(4) 0.001(3) 0.014(3) -0.008(3) C4 0.029(3) 0.048(4) 0.030(3) -0.001(3) 0.005(3) 0.001(3) C5 0.034(3) 0.045(4) 0.035(4) -0.006(3) 0.004(3) 0.000(3) C6 0.034(3) 0.047(4) 0.046(4) -0.003(3) 0.006(3) 0.000(3) C7 0.032(3) 0.056(4) 0.057(4) -0.011(4) -0.002(3) 0.004(3) C8 0.033(3) 0.043(4) 0.053(4) -0.002(3) -0.005(3) 0.004(3) C9 0.037(4) 0.035(3) 0.041(4) -0.007(3) -0.003(3) 0.005(3) C10 0.042(4) 0.035(3) 0.035(4) -0.008(3) -0.002(3) 0.001(3) C11 0.048(4) 0.043(4) 0.039(4) -0.003(3) -0.011(3) 0.003(3) C12 0.060(4) 0.045(4) 0.042(4) -0.004(3) -0.004(4) -0.004(4) C13 0.075(5) 0.068(5) 0.059(5) 0.017(4) 0.001(4) -0.018(4) C14 0.029(3) 0.041(4) 0.040(4) 0.003(3) -0.002(3) -0.007(3) C15 0.054(4) 0.062(5) 0.081(6) 0.023(5) -0.023(5) -0.003(4) C16 0.037(4) 0.044(4) 0.038(4) -0.003(3) 0.001(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 2.058(4) . ? Zn1 O1 2.081(4) . ? Zn1 N3 2.096(4) . ? Zn1 O2 2.130(4) . ? Zn1 N2 2.194(5) . ? Zn1 N4 2.239(5) . ? Zn2 O4 2.059(4) . ? Zn2 O4 2.059(4) 3_756 ? Zn2 O5 2.103(4) 3_756 ? Zn2 O5 2.103(4) . ? Zn2 O7 2.159(4) . ? Zn2 O7 2.159(4) 3_756 ? O2 C14 1.250(6) . ? O3 C16 1.249(7) 3_756 ? O4 C14 1.248(7) . ? O5 C15 1.271(8) . ? O6 C15 1.246(8) . ? O7 C16 1.257(6) . ? N1 N2 1.339(6) . ? N1 C2 1.341(7) . ? N2 C4 1.330(7) . ? N3 C5 1.336(7) . ? N3 C9 1.339(7) . ? N4 C10 1.336(7) . ? N4 N5 1.349(6) . ? N5 C12 1.355(8) . ? C1 C2 1.481(8) . ? C2 C3 1.369(8) . ? C3 C4 1.376(8) . ? C4 C5 1.483(8) . ? C5 C6 1.383(8) . ? C6 C7 1.391(8) . ? C7 C8 1.372(8) . ? C8 C9 1.371(8) . ? C9 C10 1.471(8) . ? C10 C11 1.385(8) . ? C11 C12 1.360(8) . ? C12 C13 1.488(9) . ? C14 C16 1.539(8) 3_756 ? C15 C15 1.562(15) 3_756 ? C16 O3 1.249(7) 3_756 ? C16 C14 1.539(8) 3_756 ? 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 O3 Zn1 O1 90.08(17) . . ? O3 Zn1 N3 167.49(17) . . ? O1 Zn1 N3 102.34(17) . . ? O3 Zn1 O2 78.53(15) . . ? O1 Zn1 O2 168.61(15) . . ? N3 Zn1 O2 89.04(15) . . ? O3 Zn1 N2 106.74(18) . . ? O1 Zn1 N2 89.13(18) . . ? N3 Zn1 N2 75.36(18) . . ? O2 Zn1 N2 94.16(17) . . ? O3 Zn1 N4 103.97(18) . . ? O1 Zn1 N4 91.17(17) . . ? N3 Zn1 N4 74.59(18) . . ? O2 Zn1 N4 91.54(16) . . ? N2 Zn1 N4 149.29(17) . . ? O4 Zn2 O4 163.6(2) . 3_756 ? O4 Zn2 O5 95.95(16) . 3_756 ? O4 Zn2 O5 96.68(16) 3_756 3_756 ? O4 Zn2 O5 96.68(16) . . ? O4 Zn2 O5 95.95(16) 3_756 . ? O5 Zn2 O5 79.3(2) 3_756 . ? O4 Zn2 O7 90.56(15) . . ? O4 Zn2 O7 79.12(15) 3_756 . ? O5 Zn2 O7 89.40(17) 3_756 . ? O5 Zn2 O7 167.17(17) . . ? O4 Zn2 O7 79.12(15) . 3_756 ? O4 Zn2 O7 90.56(15) 3_756 3_756 ? O5 Zn2 O7 167.16(17) 3_756 3_756 ? O5 Zn2 O7 89.40(17) . 3_756 ? O7 Zn2 O7 102.4(2) . 3_756 ? C14 O2 Zn1 113.4(4) . . ? C16 O3 Zn1 115.2(4) 3_756 . ? C14 O4 Zn2 114.9(4) . . ? C15 O5 Zn2 112.2(4) . . ? C16 O7 Zn2 111.4(4) . . ? N2 N1 C2 113.3(5) . . ? C4 N2 N1 104.0(5) . . ? C4 N2 Zn1 114.6(4) . . ? N1 N2 Zn1 141.3(4) . . ? C5 N3 C9 120.3(5) . . ? C5 N3 Zn1 119.1(4) . . ? C9 N3 Zn1 120.3(4) . . ? C10 N4 N5 104.7(5) . . ? C10 N4 Zn1 113.1(4) . . ? N5 N4 Zn1 141.9(4) . . ? N4 N5 C12 111.7(5) . . ? N1 C2 C3 105.3(5) . . ? N1 C2 C1 122.3(6) . . ? C3 C2 C1 132.3(6) . . ? C2 C3 C4 106.0(5) . . ? N2 C4 C3 111.3(5) . . ? N2 C4 C5 116.6(5) . . ? C3 C4 C5 132.0(5) . . ? N3 C5 C6 121.0(6) . . ? N3 C5 C4 114.0(5) . . ? C6 C5 C4 125.0(6) . . ? C5 C6 C7 118.3(6) . . ? C8 C7 C6 120.1(6) . . ? C9 C8 C7 118.6(6) . . ? N3 C9 C8 121.7(6) . . ? N3 C9 C10 113.5(5) . . ? C8 C9 C10 124.7(6) . . ? N4 C10 C11 111.0(5) . . ? N4 C10 C9 117.8(5) . . ? C11 C10 C9 131.1(6) . . ? C12 C11 C10 105.9(6) . . ? N5 C12 C11 106.6(6) . . ? N5 C12 C13 121.3(6) . . ? C11 C12 C13 132.1(6) . . ? O4 C14 O2 126.8(5) . . ? O4 C14 C16 117.4(5) . 3_756 ? O2 C14 C16 115.8(5) . 3_756 ? O6 C15 O5 125.7(7) . . ? O6 C15 C15 120.2(5) . 3_756 ? O5 C15 C15 114.1(5) . 3_756 ? O3 C16 O7 125.8(6) 3_756 . ? O3 C16 C14 117.0(5) 3_756 3_756 ? O7 C16 C14 117.2(5) . 3_756 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.66 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.457 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.089 _database_code_depnum_ccdc_archive 'CCDC 854264' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H25 N5 O6 Zn' _chemical_formula_weight 484.83 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 9.718(2) _cell_length_b 9.962(3) _cell_length_c 13.971(3) _cell_angle_alpha 90.00 _cell_angle_beta 128.918(11) _cell_angle_gamma 90.00 _cell_volume 1052.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 947 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 21.55 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.422 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.081 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 1.214 _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 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4287 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 23.11 _reflns_number_total 1478 _reflns_number_gt 1235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0554P)^2^+0.9812P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1478 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.5000 0.16088(7) 0.7500 0.0337(3) Uani 1 2 d S . . O1 O 0.7218(4) 0.2364(3) 0.8906(3) 0.0465(8) Uani 1 1 d . . . O2 O 0.6299(4) 0.4042(4) 0.9402(3) 0.0655(11) Uani 1 1 d . . . O1W O 0.2984(5) 0.5671(4) 0.3717(3) 0.0677(11) Uani 1 1 d . . . H1WA H 0.2318 0.6256 0.3683 0.102 Uiso 1 1 d R . . H1WB H 0.3910 0.6049 0.3907 0.102 Uiso 1 1 d R . . N1 N 0.7164(4) 0.1529(4) 0.6324(3) 0.0397(9) Uani 1 1 d . . . H1D H 0.7248 0.2378 0.6257 0.048 Uiso 1 1 calc R . . N2 N 0.6314(4) 0.0994(4) 0.6711(3) 0.0343(9) Uani 1 1 d . . . N3 N 0.5000 -0.0512(5) 0.7500 0.0304(11) Uani 1 2 d S . . C1 C 0.8862(6) 0.0942(6) 0.5598(5) 0.0564(14) Uani 1 1 d . . . H1A H 0.8898 0.1900 0.5544 0.085 Uiso 1 1 calc R . . H1B H 0.8281 0.0554 0.4799 0.085 Uiso 1 1 calc R . . H1C H 1.0046 0.0599 0.6159 0.085 Uiso 1 1 calc R . . C2 C 0.7864(5) 0.0586(5) 0.6053(4) 0.0404(11) Uani 1 1 d . . . C3 C 0.7460(6) -0.0623(5) 0.6284(4) 0.0421(11) Uani 1 1 d . . . H3B H 0.7761 -0.1470 0.6188 0.051 Uiso 1 1 calc R . . C4 C 0.6507(5) -0.0326(4) 0.6691(4) 0.0324(10) Uani 1 1 d . . . C5 C 0.5742(5) -0.1189(4) 0.7093(4) 0.0345(10) Uani 1 1 d . . . C6 C 0.5742(6) -0.2574(5) 0.7078(4) 0.0449(12) Uani 1 1 d . . . H6A H 0.6243 -0.3029 0.6783 0.054 Uiso 1 1 calc R . . C7 C 0.5000 -0.3284(7) 0.7500 0.0558(19) Uani 1 2 d S . . H7A H 0.5000 -0.4217 0.7500 0.084 Uiso 1 2 calc SR . . C8 C 0.7475(6) 0.3333(5) 0.9580(4) 0.0386(11) Uani 1 1 d . . . C9 C 0.9367(6) 0.3640(5) 1.0657(4) 0.0468(12) Uani 1 1 d . . . H9A H 1.0116 0.2918 1.0753 0.056 Uiso 1 1 calc R . . H9B H 0.9487 0.3679 1.1400 0.056 Uiso 1 1 calc R . . C10 C 0.9997(8) 0.4961(7) 1.0504(5) 0.083(2) Uani 1 1 d . . . H10A H 0.9251 0.5674 1.0422 0.124 Uiso 1 1 calc R . . H10B H 1.1190 0.5130 1.1251 0.124 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 Zn 0.0337(4) 0.0285(4) 0.0390(5) 0.000 0.0229(4) 0.000 O1 0.0408(18) 0.050(2) 0.051(2) -0.0160(17) 0.0299(17) -0.0116(16) O2 0.053(2) 0.056(2) 0.091(3) -0.023(2) 0.047(2) -0.0079(19) O1W 0.062(2) 0.057(2) 0.088(3) 0.007(2) 0.049(2) 0.0065(19) N1 0.039(2) 0.045(2) 0.039(2) 0.0017(18) 0.0266(19) -0.0019(19) N2 0.0338(19) 0.037(2) 0.037(2) -0.0005(17) 0.0243(18) -0.0004(17) N3 0.032(3) 0.029(3) 0.031(3) 0.000 0.020(2) 0.000 C1 0.053(3) 0.073(4) 0.055(3) 0.004(3) 0.040(3) 0.006(3) C2 0.031(2) 0.059(3) 0.033(3) -0.003(2) 0.021(2) 0.003(2) C3 0.039(3) 0.047(3) 0.040(3) -0.007(2) 0.025(2) 0.007(2) C4 0.028(2) 0.037(3) 0.029(2) -0.004(2) 0.017(2) 0.003(2) C5 0.031(2) 0.032(2) 0.030(2) -0.0038(19) 0.014(2) 0.000(2) C6 0.049(3) 0.036(3) 0.048(3) -0.004(2) 0.030(3) 0.005(2) C7 0.058(5) 0.039(4) 0.053(4) 0.000 0.026(4) 0.000 C8 0.043(3) 0.035(3) 0.045(3) 0.000(2) 0.031(2) -0.009(2) C9 0.047(3) 0.046(3) 0.039(3) -0.007(2) 0.023(2) -0.016(2) C10 0.060(3) 0.109(5) 0.059(4) -0.013(4) 0.028(3) -0.046(4) _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 Zn O1 1.936(3) . ? Zn O1 1.936(3) 2_656 ? Zn N3 2.113(5) . ? Zn N2 2.234(3) . ? Zn N2 2.234(3) 2_656 ? O1 C8 1.260(5) . ? O2 C8 1.229(5) . ? N1 C2 1.347(5) . ? N1 N2 1.349(5) . ? N2 C4 1.331(5) . ? N3 C5 1.347(5) 2_656 ? N3 C5 1.347(5) . ? C1 C2 1.498(6) . ? C2 C3 1.366(6) . ? C3 C4 1.389(6) . ? C4 C5 1.461(6) . ? C5 C6 1.379(6) . ? C6 C7 1.380(6) . ? C7 C6 1.379(6) 2_656 ? C8 C9 1.504(6) . ? C9 C10 1.522(7) . ? C10 C10 1.413(10) 3_767 ? 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 Zn O1 134.3(2) . 2_656 ? O1 Zn N3 112.85(10) . . ? O1 Zn N3 112.85(10) 2_656 . ? O1 Zn N2 89.43(12) . . ? O1 Zn N2 102.88(12) 2_656 . ? N3 Zn N2 74.09(9) . . ? O1 Zn N2 102.88(12) . 2_656 ? O1 Zn N2 89.43(12) 2_656 2_656 ? N3 Zn N2 74.09(9) . 2_656 ? N2 Zn N2 148.17(19) . 2_656 ? C8 O1 Zn 128.9(3) . . ? C2 N1 N2 112.4(4) . . ? C4 N2 N1 104.6(3) . . ? C4 N2 Zn 114.4(3) . . ? N1 N2 Zn 140.6(3) . . ? C5 N3 C5 119.9(5) 2_656 . ? C5 N3 Zn 120.1(3) 2_656 . ? C5 N3 Zn 120.1(3) . . ? N1 C2 C3 106.1(4) . . ? N1 C2 C1 122.0(4) . . ? C3 C2 C1 131.9(4) . . ? C2 C3 C4 105.9(4) . . ? N2 C4 C3 111.0(4) . . ? N2 C4 C5 117.5(4) . . ? C3 C4 C5 131.6(4) . . ? N3 C5 C6 120.8(4) . . ? N3 C5 C4 113.9(4) . . ? C6 C5 C4 125.3(4) . . ? C5 C6 C7 120.0(5) . . ? C6 C7 C6 118.3(7) 2_656 . ? O2 C8 O1 124.5(4) . . ? O2 C8 C9 118.9(4) . . ? O1 C8 C9 116.6(4) . . ? C8 C9 C10 112.5(4) . . ? C10 C10 C9 116.2(7) 3_767 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.11 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.744 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.070 _database_code_depnum_ccdc_archive 'CCDC 854265' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H37 N10 O5 Zn2' _chemical_formula_weight 976.63 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' _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 11.044(2) _cell_length_b 11.997(2) _cell_length_c 17.106(3) _cell_angle_alpha 87.79(3) _cell_angle_beta 74.90(3) _cell_angle_gamma 79.42(3) _cell_volume 2150.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.245 _exptl_crystal_size_mid 0.178 _exptl_crystal_size_min 0.089 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1002 _exptl_absorpt_coefficient_mu 1.178 _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 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20923 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9695 _reflns_number_gt 6615 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0806P)^2^+0.0262P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9695 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1459 _refine_ls_wR_factor_gt 0.1224 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.80360(4) 0.33150(3) 0.15873(2) 0.03046(12) Uani 1 1 d . . . Zn2 Zn 0.62131(4) 0.23117(3) 0.04280(2) 0.02968(12) Uani 1 1 d . . . O1 O 0.7722(2) 0.11349(19) 0.04568(15) 0.0399(6) Uani 1 1 d . . . O2 O 0.8996(2) 0.18282(19) 0.10807(15) 0.0390(6) Uani 1 1 d . . . O3 O 0.9399(4) 0.0570(3) 0.3021(2) 0.0770(11) Uani 1 1 d . . . O4 O 0.8775(5) -0.0696(3) 0.2417(2) 0.0951(13) Uani 1 1 d . . . O1W O 0.1275(4) 0.8373(4) 0.2135(3) 0.1006(14) Uani 1 1 d . . . H1WA H 0.0925 0.8297 0.1757 0.151 Uiso 1 1 d R . . H1WB H 0.0759 0.8293 0.2590 0.151 Uiso 1 1 d R . . N1 N 0.9371(3) 0.2733(2) 0.31429(17) 0.0357(7) Uani 1 1 d . . . H1A H 0.9239 0.2051 0.3240 0.043 Uiso 1 1 calc R . . N2 N 0.9125(3) 0.3343(2) 0.25083(17) 0.0354(7) Uani 1 1 d . . . N3 N 0.8755(3) 0.4846(2) 0.14102(17) 0.0343(6) Uani 1 1 d . . . N4 N 0.7521(3) 0.4043(2) 0.05300(16) 0.0348(7) Uani 1 1 d . . . N5 N 0.6891(3) 0.3726(2) 0.00066(16) 0.0326(6) Uani 1 1 d . . . N6 N 0.6275(3) 0.1251(2) -0.14044(17) 0.0377(7) Uani 1 1 d . . . H6A H 0.7045 0.1297 -0.1662 0.045 Uiso 1 1 calc R . . N7 N 0.5783(3) 0.1503(2) -0.06133(17) 0.0351(7) Uani 1 1 d . . . N8 N 0.4369(3) 0.1939(2) 0.08702(17) 0.0321(6) Uani 1 1 d . . . N9 N 0.5684(3) 0.2754(2) 0.16846(16) 0.0328(6) Uani 1 1 d . . . N10 N 0.6302(3) 0.3075(2) 0.22119(16) 0.0332(6) Uani 1 1 d . . . C1 C 1.1137(5) 0.3264(4) 0.4611(3) 0.0659(14) Uani 1 1 d . . . H1 H 1.1529 0.3833 0.4326 0.079 Uiso 1 1 calc R . . C2 C 1.1475(6) 0.2823(5) 0.5303(3) 0.0822(18) Uani 1 1 d . . . H2 H 1.2094 0.3098 0.5480 0.099 Uiso 1 1 calc R . . C3 C 1.0905(6) 0.1990(4) 0.5725(3) 0.0733(16) Uani 1 1 d . . . H3 H 1.1129 0.1711 0.6193 0.088 Uiso 1 1 calc R . . C4 C 1.0024(5) 0.1565(5) 0.5476(3) 0.0728(15) Uani 1 1 d . . . H4 H 0.9664 0.0979 0.5760 0.087 Uiso 1 1 calc R . . C5 C 0.9643(5) 0.2005(4) 0.4785(3) 0.0611(13) Uani 1 1 d . . . H5 H 0.9013 0.1725 0.4625 0.073 Uiso 1 1 calc R . . C6 C 1.0205(4) 0.2854(3) 0.4342(2) 0.0440(9) Uani 1 1 d . . . C7 C 0.9850(4) 0.3326(3) 0.3608(2) 0.0378(8) Uani 1 1 d . . . C8 C 0.9915(4) 0.4379(3) 0.3256(2) 0.0428(9) Uani 1 1 d . . . H8 H 1.0205 0.4976 0.3438 0.051 Uiso 1 1 calc R . . C9 C 0.9460(4) 0.4356(3) 0.2582(2) 0.0357(8) Uani 1 1 d . . . C10 C 0.9276(4) 0.5199(3) 0.1955(2) 0.0406(9) Uani 1 1 d . . . C11 C 0.9618(6) 0.6253(3) 0.1908(3) 0.0676(15) Uani 1 1 d . . . H11 H 0.9935 0.6513 0.2307 0.081 Uiso 1 1 calc R . . C12 C 0.9468(6) 0.6917(4) 0.1236(3) 0.082(2) Uani 1 1 d . . . H12 H 0.9713 0.7624 0.1177 0.099 Uiso 1 1 calc R . . C13 C 0.8965(5) 0.6542(3) 0.0664(3) 0.0608(13) Uani 1 1 d . . . H13 H 0.8883 0.6979 0.0214 0.073 Uiso 1 1 calc R . . C14 C 0.8579(4) 0.5489(3) 0.0771(2) 0.0380(8) Uani 1 1 d . . . C15 C 0.7941(4) 0.4993(3) 0.0261(2) 0.0349(8) Uani 1 1 d . . . C16 C 0.7616(4) 0.5312(3) -0.0464(2) 0.0415(9) Uani 1 1 d . . . H16 H 0.7797 0.5938 -0.0781 0.050 Uiso 1 1 calc R . . C17 C 0.6960(4) 0.4487(3) -0.0605(2) 0.0347(8) Uani 1 1 d . . . C18 C 0.6416(4) 0.4359(3) -0.1292(2) 0.0383(8) Uani 1 1 d . . . C19 C 0.7114(5) 0.4561(4) -0.2071(2) 0.0646(13) Uani 1 1 d . . . H19 H 0.7870 0.4837 -0.2147 0.078 Uiso 1 1 calc R . . C20 C 0.6691(6) 0.4355(5) -0.2726(3) 0.0767(16) Uani 1 1 d . . . H20 H 0.7167 0.4492 -0.3243 0.092 Uiso 1 1 calc R . . C21 C 0.5578(5) 0.3950(4) -0.2634(3) 0.0619(13) Uani 1 1 d . . . H21 H 0.5320 0.3783 -0.3085 0.074 Uiso 1 1 calc R . . C22 C 0.4847(4) 0.3795(3) -0.1863(3) 0.0536(11) Uani 1 1 d . . . H22 H 0.4070 0.3556 -0.1789 0.064 Uiso 1 1 calc R . . C23 C 0.5282(4) 0.4000(3) -0.1198(2) 0.0440(9) Uani 1 1 d . . . H23 H 0.4791 0.3890 -0.0680 0.053 Uiso 1 1 calc R . . C24 C 0.6909(5) 0.0334(4) -0.3101(3) 0.0589(12) Uani 1 1 d . . . H24 H 0.7604 0.0353 -0.2894 0.071 Uiso 1 1 calc R . . C25 C 0.7111(6) 0.0015(4) -0.3898(3) 0.0745(15) Uani 1 1 d . . . H25 H 0.7937 -0.0204 -0.4219 0.089 Uiso 1 1 calc R . . C26 C 0.6076(7) 0.0024(5) -0.4219(3) 0.087(2) Uani 1 1 d . . . H26 H 0.6209 -0.0171 -0.4760 0.105 Uiso 1 1 calc R . . C27 C 0.4870(7) 0.0319(5) -0.3742(3) 0.0883(19) Uani 1 1 d . . . H27 H 0.4179 0.0313 -0.3957 0.106 Uiso 1 1 calc R . . C28 C 0.4660(6) 0.0626(4) -0.2943(3) 0.0695(14) Uani 1 1 d . . . H28 H 0.3831 0.0835 -0.2625 0.083 Uiso 1 1 calc R . . C29 C 0.5693(4) 0.0623(3) -0.2608(2) 0.0471(10) Uani 1 1 d . . . C30 C 0.5425(4) 0.0916(3) -0.1752(2) 0.0410(9) Uani 1 1 d . . . C31 C 0.4320(4) 0.0939(3) -0.1141(2) 0.0415(9) Uani 1 1 d . . . H31 H 0.3560 0.0748 -0.1182 0.050 Uiso 1 1 calc R . . C32 C 0.4584(4) 0.1308(3) -0.0453(2) 0.0353(8) Uani 1 1 d . . . C33 C 0.3785(3) 0.1514(3) 0.0379(2) 0.0336(7) Uani 1 1 d . . . C34 C 0.2568(4) 0.1288(3) 0.0657(2) 0.0429(9) Uani 1 1 d . . . H34 H 0.2184 0.0980 0.0314 0.051 Uiso 1 1 calc R . . C35 C 0.1930(4) 0.1532(3) 0.1458(2) 0.0451(9) Uani 1 1 d . . . H35 H 0.1099 0.1409 0.1657 0.054 Uiso 1 1 calc R . . C36 C 0.2533(4) 0.1959(3) 0.1962(2) 0.0452(9) Uani 1 1 d . . . H36 H 0.2114 0.2126 0.2502 0.054 Uiso 1 1 calc R . . C37 C 0.3771(3) 0.2135(3) 0.1650(2) 0.0354(8) Uani 1 1 d . . . C38 C 0.4571(3) 0.2514(3) 0.2120(2) 0.0340(7) Uani 1 1 d . . . C39 C 0.4433(4) 0.2671(3) 0.2932(2) 0.0436(9) Uani 1 1 d . . . H39 H 0.3749 0.2563 0.3360 0.052 Uiso 1 1 calc R . . C40 C 0.5545(4) 0.3028(3) 0.2971(2) 0.0365(8) Uani 1 1 d . . . C41 C 0.5912(4) 0.3356(3) 0.3689(2) 0.0397(8) Uani 1 1 d . . . C42 C 0.6450(4) 0.4307(3) 0.3685(2) 0.0477(10) Uani 1 1 d . . . H42 H 0.6599 0.4748 0.3222 0.057 Uiso 1 1 calc R . . C43 C 0.6770(5) 0.4605(4) 0.4374(3) 0.0648(13) Uani 1 1 d . . . H43 H 0.7145 0.5240 0.4367 0.078 Uiso 1 1 calc R . . C44 C 0.6540(6) 0.3980(5) 0.5054(3) 0.0768(16) Uani 1 1 d . . . H44 H 0.6755 0.4188 0.5511 0.092 Uiso 1 1 calc R . . C45 C 0.5991(6) 0.3041(5) 0.5071(3) 0.0766(16) Uani 1 1 d . . . H45 H 0.5829 0.2615 0.5541 0.092 Uiso 1 1 calc R . . C46 C 0.5677(5) 0.2726(4) 0.4391(2) 0.0626(13) Uani 1 1 d . . . H46 H 0.5307 0.2087 0.4404 0.075 Uiso 1 1 calc R . . C47 C 0.8714(3) 0.1086(3) 0.0690(2) 0.0322(7) Uani 1 1 d . . . C48 C 0.9697(3) 0.0014(3) 0.0458(2) 0.0334(7) Uani 1 1 d . . . H48A H 0.9294 -0.0644 0.0610 0.040 Uiso 1 1 calc R . . H48B H 1.0352 -0.0013 0.0745 0.040 Uiso 1 1 calc R . . C49 C 0.8638(6) 0.0240(4) 0.2749(3) 0.0677(14) Uani 1 1 d . . . H49 H 0.7867 0.0729 0.2789 0.081 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 Zn1 0.0332(2) 0.0282(2) 0.0312(2) -0.00302(15) -0.00831(17) -0.00779(17) Zn2 0.0278(2) 0.0316(2) 0.0303(2) -0.00246(15) -0.00820(16) -0.00523(16) O1 0.0323(14) 0.0369(13) 0.0539(16) -0.0118(11) -0.0209(12) 0.0016(11) O2 0.0376(15) 0.0350(12) 0.0468(15) -0.0144(11) -0.0168(12) -0.0008(11) O3 0.107(3) 0.0437(17) 0.093(3) 0.0074(17) -0.043(2) -0.020(2) O4 0.138(4) 0.061(2) 0.088(3) -0.0200(19) -0.022(3) -0.027(2) O1W 0.070(3) 0.142(4) 0.097(3) -0.013(3) -0.012(2) -0.047(3) N1 0.0423(18) 0.0304(14) 0.0365(16) 0.0033(12) -0.0117(14) -0.0105(13) N2 0.0393(17) 0.0305(14) 0.0383(16) -0.0013(12) -0.0116(14) -0.0086(13) N3 0.0403(18) 0.0313(14) 0.0343(15) 0.0003(12) -0.0123(13) -0.0098(13) N4 0.0456(18) 0.0332(15) 0.0300(15) 0.0008(12) -0.0133(13) -0.0133(14) N5 0.0375(17) 0.0352(15) 0.0262(14) 0.0008(11) -0.0099(13) -0.0073(13) N6 0.0380(18) 0.0438(17) 0.0320(15) -0.0056(13) -0.0106(13) -0.0060(14) N7 0.0358(17) 0.0375(15) 0.0322(15) -0.0053(12) -0.0093(13) -0.0052(13) N8 0.0294(16) 0.0351(15) 0.0331(15) 0.0005(12) -0.0097(12) -0.0071(12) N9 0.0307(16) 0.0396(15) 0.0287(14) -0.0053(12) -0.0074(12) -0.0071(13) N10 0.0340(17) 0.0386(15) 0.0279(14) -0.0048(12) -0.0077(12) -0.0077(13) C1 0.089(4) 0.064(3) 0.066(3) 0.017(2) -0.043(3) -0.038(3) C2 0.118(5) 0.082(4) 0.077(4) 0.012(3) -0.066(4) -0.041(4) C3 0.110(5) 0.073(3) 0.047(3) 0.013(2) -0.035(3) -0.022(3) C4 0.078(4) 0.091(4) 0.059(3) 0.023(3) -0.023(3) -0.033(3) C5 0.071(3) 0.075(3) 0.050(3) 0.015(2) -0.026(2) -0.031(3) C6 0.050(2) 0.049(2) 0.037(2) -0.0020(17) -0.0142(18) -0.0116(19) C7 0.043(2) 0.0416(19) 0.0312(18) -0.0019(15) -0.0110(16) -0.0112(17) C8 0.056(3) 0.0382(19) 0.043(2) -0.0006(16) -0.0222(19) -0.0191(19) C9 0.043(2) 0.0321(17) 0.0350(18) -0.0027(14) -0.0129(16) -0.0100(16) C10 0.049(2) 0.0353(18) 0.043(2) -0.0015(16) -0.0201(18) -0.0110(17) C11 0.116(4) 0.041(2) 0.074(3) 0.010(2) -0.062(3) -0.034(3) C12 0.144(6) 0.044(2) 0.102(4) 0.023(3) -0.089(4) -0.047(3) C13 0.096(4) 0.034(2) 0.068(3) 0.020(2) -0.040(3) -0.028(2) C14 0.043(2) 0.0308(17) 0.043(2) 0.0008(15) -0.0153(17) -0.0086(16) C15 0.041(2) 0.0308(17) 0.0338(18) 0.0035(14) -0.0090(16) -0.0104(16) C16 0.052(2) 0.0355(18) 0.038(2) 0.0086(16) -0.0119(18) -0.0134(18) C17 0.039(2) 0.0352(17) 0.0302(17) 0.0026(14) -0.0129(15) -0.0022(16) C18 0.045(2) 0.0373(18) 0.0326(18) 0.0038(15) -0.0119(16) -0.0050(17) C19 0.070(3) 0.099(4) 0.033(2) 0.016(2) -0.019(2) -0.032(3) C20 0.091(4) 0.112(4) 0.033(2) 0.012(3) -0.020(3) -0.031(4) C21 0.077(4) 0.071(3) 0.047(3) 0.000(2) -0.038(3) -0.006(3) C22 0.052(3) 0.052(2) 0.062(3) -0.007(2) -0.028(2) -0.001(2) C23 0.044(2) 0.047(2) 0.041(2) 0.0001(17) -0.0154(18) -0.0010(18) C24 0.075(3) 0.065(3) 0.042(2) -0.006(2) -0.013(2) -0.027(3) C25 0.097(4) 0.088(4) 0.041(2) -0.012(2) -0.009(3) -0.032(3) C26 0.144(6) 0.093(4) 0.034(3) -0.006(3) -0.022(3) -0.045(4) C27 0.115(5) 0.116(5) 0.053(3) -0.011(3) -0.049(4) -0.028(4) C28 0.079(4) 0.091(4) 0.052(3) -0.011(2) -0.031(3) -0.025(3) C29 0.066(3) 0.045(2) 0.038(2) -0.0019(17) -0.021(2) -0.017(2) C30 0.049(2) 0.0394(19) 0.040(2) -0.0026(16) -0.0157(18) -0.0131(18) C31 0.048(2) 0.047(2) 0.038(2) -0.0030(16) -0.0204(18) -0.0170(19) C32 0.037(2) 0.0347(18) 0.0380(19) 0.0003(15) -0.0133(16) -0.0096(16) C33 0.0335(19) 0.0319(17) 0.0381(18) -0.0016(14) -0.0130(15) -0.0063(15) C34 0.040(2) 0.047(2) 0.049(2) 0.0011(18) -0.0172(18) -0.0176(18) C35 0.035(2) 0.054(2) 0.050(2) 0.0011(18) -0.0098(18) -0.0158(18) C36 0.036(2) 0.057(2) 0.041(2) -0.0053(18) -0.0021(17) -0.0134(19) C37 0.0315(19) 0.0393(19) 0.0353(18) -0.0026(15) -0.0076(15) -0.0066(15) C38 0.0303(19) 0.0398(18) 0.0295(17) -0.0025(14) -0.0020(14) -0.0079(15) C39 0.041(2) 0.056(2) 0.0315(19) -0.0050(17) 0.0000(16) -0.0150(19) C40 0.038(2) 0.0414(19) 0.0284(17) -0.0062(14) -0.0032(15) -0.0083(16) C41 0.041(2) 0.047(2) 0.0293(18) -0.0061(15) -0.0071(16) -0.0038(17) C42 0.047(2) 0.050(2) 0.045(2) -0.0130(18) -0.0098(19) -0.0065(19) C43 0.060(3) 0.075(3) 0.065(3) -0.035(3) -0.021(3) -0.012(3) C44 0.082(4) 0.110(4) 0.042(3) -0.025(3) -0.023(3) -0.011(3) C45 0.098(4) 0.102(4) 0.037(2) 0.000(3) -0.028(3) -0.019(4) C46 0.084(4) 0.070(3) 0.035(2) -0.005(2) -0.010(2) -0.024(3) C47 0.0333(19) 0.0301(16) 0.0325(17) -0.0018(14) -0.0080(15) -0.0038(14) C48 0.036(2) 0.0300(16) 0.0359(18) -0.0051(14) -0.0147(16) -0.0010(14) C49 0.089(4) 0.053(3) 0.061(3) 0.001(2) -0.015(3) -0.022(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 O2 2.001(2) . ? Zn1 N10 2.001(3) . ? Zn1 N3 2.113(3) . ? Zn1 N4 2.142(3) . ? Zn1 N2 2.221(3) . ? Zn2 O1 1.987(3) . ? Zn2 N5 2.013(3) . ? Zn2 N8 2.104(3) . ? Zn2 N9 2.136(3) . ? Zn2 N7 2.255(3) . ? O1 C47 1.251(4) . ? O2 C47 1.262(4) . ? O3 C49 1.192(6) . ? O4 C49 1.244(6) . ? N1 N2 1.344(4) . ? N1 C7 1.349(4) . ? N2 C9 1.354(4) . ? N3 C10 1.333(4) . ? N3 C14 1.348(4) . ? N4 C15 1.330(4) . ? N4 N5 1.370(4) . ? N5 C17 1.358(4) . ? N6 N7 1.344(4) . ? N6 C30 1.359(4) . ? N7 C32 1.343(4) . ? N8 C37 1.333(4) . ? N8 C33 1.349(4) . ? N9 C38 1.336(4) . ? N9 N10 1.368(4) . ? N10 C40 1.355(4) . ? C1 C2 1.390(6) . ? C1 C6 1.401(6) . ? C2 C3 1.362(7) . ? C3 C4 1.343(7) . ? C4 C5 1.407(6) . ? C5 C6 1.387(5) . ? C6 C7 1.474(5) . ? C7 C8 1.384(5) . ? C8 C9 1.376(5) . ? C9 C10 1.473(5) . ? C10 C11 1.378(5) . ? C11 C12 1.403(6) . ? C12 C13 1.369(6) . ? C13 C14 1.397(5) . ? C14 C15 1.459(5) . ? C15 C16 1.399(5) . ? C16 C17 1.391(5) . ? C17 C18 1.477(5) . ? C18 C23 1.368(5) . ? C18 C19 1.391(5) . ? C19 C20 1.367(6) . ? C20 C21 1.373(7) . ? C21 C22 1.381(6) . ? C22 C23 1.390(5) . ? C24 C29 1.377(7) . ? C24 C25 1.380(6) . ? C25 C26 1.389(8) . ? C26 C27 1.360(9) . ? C27 C28 1.379(7) . ? C28 C29 1.403(6) . ? C29 C30 1.459(5) . ? C30 C31 1.381(5) . ? C31 C32 1.390(5) . ? C32 C33 1.469(5) . ? C33 C34 1.377(5) . ? C34 C35 1.383(5) . ? C35 C36 1.381(5) . ? C36 C37 1.384(5) . ? C37 C38 1.477(5) . ? C38 C39 1.374(5) . ? C39 C40 1.390(5) . ? C40 C41 1.477(5) . ? C41 C42 1.379(5) . ? C41 C46 1.385(5) . ? C42 C43 1.393(5) . ? C43 C44 1.352(7) . ? C44 C45 1.370(7) . ? C45 C46 1.382(6) . ? C47 C48 1.514(5) . ? C48 C48 1.534(7) 2_755 ? 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 O2 Zn1 N10 107.54(11) . . ? O2 Zn1 N3 124.23(11) . . ? N10 Zn1 N3 128.14(12) . . ? O2 Zn1 N4 96.86(11) . . ? N10 Zn1 N4 97.66(12) . . ? N3 Zn1 N4 75.05(11) . . ? O2 Zn1 N2 96.24(11) . . ? N10 Zn1 N2 105.28(11) . . ? N3 Zn1 N2 74.04(10) . . ? N4 Zn1 N2 148.67(10) . . ? O1 Zn2 N5 106.25(11) . . ? O1 Zn2 N8 119.77(11) . . ? N5 Zn2 N8 133.84(12) . . ? O1 Zn2 N9 96.67(11) . . ? N5 Zn2 N9 97.23(11) . . ? N8 Zn2 N9 75.15(11) . . ? O1 Zn2 N7 94.72(11) . . ? N5 Zn2 N7 107.27(11) . . ? N8 Zn2 N7 73.97(11) . . ? N9 Zn2 N7 148.80(11) . . ? C47 O1 Zn2 136.2(2) . . ? C47 O2 Zn1 133.2(2) . . ? N2 N1 C7 111.5(3) . . ? N1 N2 C9 105.3(3) . . ? N1 N2 Zn1 139.3(2) . . ? C9 N2 Zn1 113.9(2) . . ? C10 N3 C14 121.4(3) . . ? C10 N3 Zn1 120.2(2) . . ? C14 N3 Zn1 118.2(2) . . ? C15 N4 N5 108.5(3) . . ? C15 N4 Zn1 116.5(2) . . ? N5 N4 Zn1 134.8(2) . . ? C17 N5 N4 107.9(3) . . ? C17 N5 Zn2 143.5(2) . . ? N4 N5 Zn2 108.62(19) . . ? N7 N6 C30 112.6(3) . . ? C32 N7 N6 104.6(3) . . ? C32 N7 Zn2 113.6(2) . . ? N6 N7 Zn2 141.2(2) . . ? C37 N8 C33 119.8(3) . . ? C37 N8 Zn2 119.0(2) . . ? C33 N8 Zn2 121.2(2) . . ? C38 N9 N10 107.7(3) . . ? C38 N9 Zn2 116.4(2) . . ? N10 N9 Zn2 135.0(2) . . ? C40 N10 N9 107.7(3) . . ? C40 N10 Zn1 143.2(2) . . ? N9 N10 Zn1 108.8(2) . . ? C2 C1 C6 120.1(4) . . ? C3 C2 C1 120.4(5) . . ? C4 C3 C2 120.9(5) . . ? C3 C4 C5 120.2(5) . . ? C6 C5 C4 120.2(4) . . ? C5 C6 C1 118.1(4) . . ? C5 C6 C7 122.0(4) . . ? C1 C6 C7 119.9(4) . . ? N1 C7 C8 106.9(3) . . ? N1 C7 C6 122.6(3) . . ? C8 C7 C6 130.5(3) . . ? C9 C8 C7 105.5(3) . . ? N2 C9 C8 110.7(3) . . ? N2 C9 C10 116.4(3) . . ? C8 C9 C10 132.8(3) . . ? N3 C10 C11 121.7(3) . . ? N3 C10 C9 113.7(3) . . ? C11 C10 C9 124.6(3) . . ? C10 C11 C12 117.3(4) . . ? C13 C12 C11 121.0(4) . . ? C12 C13 C14 118.6(4) . . ? N3 C14 C13 119.9(3) . . ? N3 C14 C15 113.9(3) . . ? C13 C14 C15 126.2(3) . . ? N4 C15 C16 109.8(3) . . ? N4 C15 C14 116.0(3) . . ? C16 C15 C14 134.2(3) . . ? C17 C16 C15 104.7(3) . . ? N5 C17 C16 109.1(3) . . ? N5 C17 C18 121.5(3) . . ? C16 C17 C18 129.4(3) . . ? C23 C18 C19 118.5(4) . . ? C23 C18 C17 122.6(3) . . ? C19 C18 C17 118.8(4) . . ? C20 C19 C18 120.2(4) . . ? C19 C20 C21 121.3(4) . . ? C20 C21 C22 119.1(4) . . ? C21 C22 C23 119.4(4) . . ? C18 C23 C22 121.3(4) . . ? C29 C24 C25 121.1(5) . . ? C24 C25 C26 119.7(6) . . ? C27 C26 C25 119.9(5) . . ? C26 C27 C28 120.6(6) . . ? C27 C28 C29 120.3(6) . . ? C24 C29 C28 118.3(4) . . ? C24 C29 C30 123.4(4) . . ? C28 C29 C30 118.3(4) . . ? N6 C30 C31 105.9(3) . . ? N6 C30 C29 124.2(4) . . ? C31 C30 C29 129.9(3) . . ? C30 C31 C32 105.5(3) . . ? N7 C32 C31 111.3(3) . . ? N7 C32 C33 117.6(3) . . ? C31 C32 C33 131.1(3) . . ? N8 C33 C34 121.7(3) . . ? N8 C33 C32 113.2(3) . . ? C34 C33 C32 125.1(3) . . ? C33 C34 C35 118.4(3) . . ? C36 C35 C34 119.8(4) . . ? C35 C36 C37 118.9(4) . . ? N8 C37 C36 121.3(3) . . ? N8 C37 C38 113.3(3) . . ? C36 C37 C38 125.4(3) . . ? N9 C38 C39 110.7(3) . . ? N9 C38 C37 115.5(3) . . ? C39 C38 C37 133.8(3) . . ? C38 C39 C40 104.6(3) . . ? N10 C40 C39 109.2(3) . . ? N10 C40 C41 121.8(3) . . ? C39 C40 C41 128.9(3) . . ? C42 C41 C46 118.9(4) . . ? C42 C41 C40 121.1(3) . . ? C46 C41 C40 120.0(3) . . ? C41 C42 C43 119.9(4) . . ? C44 C43 C42 120.6(4) . . ? C43 C44 C45 120.2(4) . . ? C44 C45 C46 120.0(5) . . ? C45 C46 C41 120.4(4) . . ? O1 C47 O2 127.7(3) . . ? O1 C47 C48 115.5(3) . . ? O2 C47 C48 116.7(3) . . ? C47 C48 C48 110.0(3) . 2_755 ? O3 C49 O4 126.4(6) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.469 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.086 _database_code_depnum_ccdc_archive 'CCDC 854266' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H42 N10 O6 Zn2' _chemical_formula_weight 1021.73 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' 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' 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' _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 10.9728(19) _cell_length_b 12.610(2) _cell_length_c 16.807(3) _cell_angle_alpha 77.404(2) _cell_angle_beta 79.051(2) _cell_angle_gamma 89.147(2) _cell_volume 2227.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3788 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 24.79 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.679 _exptl_crystal_size_mid 0.392 _exptl_crystal_size_min 0.193 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 1.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.590 _exptl_absorpt_correction_T_max 0.802 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11203 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7713 _reflns_number_gt 5858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0602P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7713 _refine_ls_number_parameters 631 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.180 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.08292(4) 0.18394(3) 0.79940(2) 0.03489(13) Uani 1 1 d . . . Zn2 Zn 0.17457(4) 0.45867(3) 0.66873(2) 0.03574(13) Uani 1 1 d . . . O1 O -0.1789(3) 0.2664(2) 0.8071(2) 0.0727(9) Uani 1 1 d . . . O2 O -0.0179(2) 0.27288(19) 0.86827(14) 0.0445(6) Uani 1 1 d . . . O3 O 0.1515(3) 0.5425(3) 0.8167(2) 0.0892(11) Uani 1 1 d . . . O4 O 0.0250(2) 0.49472(19) 0.74230(14) 0.0443(6) Uani 1 1 d . . . O1W O 0.2758(5) 0.6952(4) 0.8485(3) 0.1460(18) Uani 1 1 d . . . H1WA H 0.3187 0.7295 0.8027 0.219 Uiso 1 1 d RD . . H1WB H 0.2123 0.7315 0.8622 0.219 Uiso 1 1 d R . . O2W O 0.7143(3) 0.1039(3) 0.7706(2) 0.0902(11) Uani 1 1 d . . . H2WA H 0.7361 0.1324 0.8074 0.135 Uiso 1 1 d R . . H2WB H 0.7575 0.0484 0.7655 0.135 Uiso 1 1 d R . . N1 N 0.0736(3) 0.2083(2) 0.67877(16) 0.0347(6) Uani 1 1 d . . . N2 N 0.1079(3) 0.3120(2) 0.63874(16) 0.0351(6) Uani 1 1 d . . . N3 N 0.1765(2) 0.5015(2) 0.53969(16) 0.0349(6) Uani 1 1 d . . . N4 N 0.2465(3) 0.6308(2) 0.62505(17) 0.0418(7) Uani 1 1 d . . . N5 N 0.2872(3) 0.7101(2) 0.65443(17) 0.0434(7) Uani 1 1 d . . . H5A H 0.2917 0.7032 0.7058 0.052 Uiso 1 1 calc RD . . N6 N 0.3031(2) 0.3732(2) 0.72343(16) 0.0352(6) Uani 1 1 d . . . N7 N 0.2579(3) 0.2753(2) 0.77069(16) 0.0359(7) Uani 1 1 d . . . N8 N 0.2031(3) 0.0834(2) 0.86644(16) 0.0341(6) Uani 1 1 d . . . N9 N -0.0254(3) 0.0234(2) 0.86395(17) 0.0392(7) Uani 1 1 d . . . N10 N -0.1340(3) -0.0279(2) 0.86966(17) 0.0419(7) Uani 1 1 d . . . H10A H -0.1924 0.0005 0.8450 0.050 Uiso 1 1 calc R . . C1 C -0.0983(4) 0.0061(3) 0.6160(3) 0.0629(12) Uani 1 1 d . . . H1A H -0.1374 0.0569 0.5809 0.075 Uiso 1 1 calc R . . C2 C -0.1402(5) -0.0996(4) 0.6372(3) 0.0822(15) Uani 1 1 d . . . H2A H -0.2088 -0.1197 0.6182 0.099 Uiso 1 1 calc R . . C3 C -0.0812(5) -0.1757(4) 0.6864(3) 0.0752(15) Uani 1 1 d . . . H3A H -0.1087 -0.2480 0.7000 0.090 Uiso 1 1 calc R . . C4 C 0.0188(4) -0.1461(3) 0.7158(3) 0.0603(12) Uani 1 1 d . . . H4A H 0.0586 -0.1984 0.7493 0.072 Uiso 1 1 calc R . . C5 C 0.0607(4) -0.0387(3) 0.6960(2) 0.0442(9) Uani 1 1 d . . . H5B H 0.1283 -0.0191 0.7162 0.053 Uiso 1 1 calc R . . C6 C 0.0015(3) 0.0399(3) 0.6457(2) 0.0405(8) Uani 1 1 d . . . C7 C 0.0416(3) 0.1549(3) 0.6232(2) 0.0360(8) Uani 1 1 d . . . C8 C 0.0546(3) 0.2256(3) 0.5465(2) 0.0387(8) Uani 1 1 d . . . H8A H 0.0379 0.2113 0.4976 0.046 Uiso 1 1 calc R . . C9 C 0.0981(3) 0.3230(3) 0.55850(19) 0.0343(8) Uani 1 1 d . . . C10 C 0.1342(3) 0.4287(3) 0.5031(2) 0.0341(8) Uani 1 1 d . . . C11 C 0.1259(3) 0.4556(3) 0.4196(2) 0.0417(9) Uani 1 1 d . . . H11A H 0.0931 0.4059 0.3952 0.050 Uiso 1 1 calc R . . C12 C 0.1675(3) 0.5576(3) 0.3735(2) 0.0465(9) Uani 1 1 d . . . H12A H 0.1643 0.5766 0.3173 0.056 Uiso 1 1 calc R . . C13 C 0.2136(3) 0.6308(3) 0.4110(2) 0.0462(9) Uani 1 1 d . . . H13A H 0.2433 0.6991 0.3802 0.055 Uiso 1 1 calc R . . C14 C 0.2150(3) 0.6015(3) 0.4949(2) 0.0361(8) Uani 1 1 d . . . C15 C 0.2543(3) 0.6726(3) 0.5445(2) 0.0375(8) Uani 1 1 d . . . C16 C 0.2999(3) 0.7789(3) 0.5239(2) 0.0421(9) Uani 1 1 d . . . H16A H 0.3136 0.8252 0.4716 0.051 Uiso 1 1 calc R . . C17 C 0.3206(3) 0.8021(3) 0.5969(2) 0.0413(8) Uani 1 1 d . . . C18 C 0.3655(3) 0.9019(3) 0.6157(2) 0.0458(9) Uani 1 1 d . . . C19 C 0.3451(4) 1.0014(3) 0.5682(3) 0.0656(12) Uani 1 1 d . . . H19A H 0.3063 1.0049 0.5231 0.079 Uiso 1 1 calc R . . C20 C 0.3812(5) 1.0962(4) 0.5862(3) 0.0825(16) Uani 1 1 d . . . H20A H 0.3647 1.1630 0.5543 0.099 Uiso 1 1 calc R . . C21 C 0.4414(5) 1.0922(4) 0.6510(3) 0.0783(16) Uani 1 1 d . . . H21A H 0.4670 1.1560 0.6629 0.094 Uiso 1 1 calc R . . C22 C 0.4635(5) 0.9929(4) 0.6984(3) 0.0826(15) Uani 1 1 d . . . H22A H 0.5044 0.9893 0.7426 0.099 Uiso 1 1 calc R . . C23 C 0.4256(4) 0.8995(4) 0.6806(3) 0.0672(12) Uani 1 1 d . . . H23A H 0.4409 0.8328 0.7132 0.081 Uiso 1 1 calc R . . C24 C 0.5048(3) 0.5283(3) 0.6086(2) 0.0402(8) Uani 1 1 d . . . H24A H 0.4691 0.4891 0.5776 0.048 Uiso 1 1 calc R . . C25 C 0.5689(3) 0.6247(3) 0.5693(2) 0.0466(9) Uani 1 1 d . . . H25A H 0.5757 0.6504 0.5123 0.056 Uiso 1 1 calc R . . C26 C 0.6227(4) 0.6826(3) 0.6152(3) 0.0535(10) Uani 1 1 d . . . H26A H 0.6654 0.7480 0.5893 0.064 Uiso 1 1 calc R . . C27 C 0.6131(4) 0.6433(3) 0.6991(3) 0.0572(11) Uani 1 1 d . . . H27A H 0.6499 0.6822 0.7298 0.069 Uiso 1 1 calc R . . C28 C 0.5496(3) 0.5474(3) 0.7383(2) 0.0510(10) Uani 1 1 d . . . H28A H 0.5445 0.5215 0.7950 0.061 Uiso 1 1 calc R . . C29 C 0.4929(3) 0.4888(3) 0.6933(2) 0.0357(8) Uani 1 1 d . . . C30 C 0.4198(3) 0.3874(3) 0.7352(2) 0.0366(8) Uani 1 1 d . . . C31 C 0.4519(3) 0.2972(3) 0.7898(2) 0.0413(9) Uani 1 1 d . . . H31A H 0.5266 0.2849 0.8084 0.050 Uiso 1 1 calc R . . C32 C 0.3474(3) 0.2294(3) 0.8105(2) 0.0365(8) Uani 1 1 d . . . C33 C 0.3175(3) 0.1209(3) 0.8633(2) 0.0366(8) Uani 1 1 d . . . C34 C 0.3993(4) 0.0591(3) 0.9068(2) 0.0481(9) Uani 1 1 d . . . H34A H 0.4794 0.0851 0.9035 0.058 Uiso 1 1 calc R . . C35 C 0.3589(4) -0.0418(3) 0.9553(2) 0.0551(11) Uani 1 1 d . . . H35A H 0.4119 -0.0842 0.9854 0.066 Uiso 1 1 calc R . . C36 C 0.2414(4) -0.0797(3) 0.9591(2) 0.0497(10) Uani 1 1 d . . . H36A H 0.2138 -0.1476 0.9917 0.060 Uiso 1 1 calc R . . C37 C 0.1644(3) -0.0156(3) 0.9140(2) 0.0376(8) Uani 1 1 d . . . C38 C 0.0380(3) -0.0474(3) 0.91036(19) 0.0375(8) Uani 1 1 d . . . C39 C -0.0308(4) -0.1431(3) 0.9459(2) 0.0431(9) Uani 1 1 d . . . H39A H -0.0070 -0.2042 0.9811 0.052 Uiso 1 1 calc R . . C40 C -0.1418(4) -0.1290(3) 0.9182(2) 0.0419(9) Uani 1 1 d . . . C41 C -0.2505(4) -0.2031(3) 0.9344(2) 0.0480(10) Uani 1 1 d . . . C42 C -0.2642(4) -0.2928(3) 0.9998(2) 0.0601(12) Uani 1 1 d . . . H42A H -0.2051 -0.3062 1.0335 0.072 Uiso 1 1 calc R . . C43 C -0.3661(6) -0.3627(4) 1.0150(3) 0.0807(16) Uani 1 1 d . . . H43A H -0.3746 -0.4234 1.0588 0.097 Uiso 1 1 calc R . . C44 C -0.4546(5) -0.3435(5) 0.9664(4) 0.0881(18) Uani 1 1 d . . . H44A H -0.5231 -0.3906 0.9774 0.106 Uiso 1 1 calc R . . C45 C -0.4416(5) -0.2547(4) 0.9016(4) 0.0832(15) Uani 1 1 d . . . H45A H -0.5017 -0.2418 0.8686 0.100 Uiso 1 1 calc R . . C46 C -0.3404(4) -0.1842(4) 0.8845(3) 0.0666(12) Uani 1 1 d . . . H46A H -0.3320 -0.1245 0.8400 0.080 Uiso 1 1 calc R . . C47 C -0.1260(4) 0.2992(3) 0.8559(2) 0.0478(9) Uani 1 1 d . . . C48 C -0.1953(4) 0.3755(4) 0.9072(3) 0.0700(14) Uani 1 1 d . . . C49A C -0.1882(9) 0.4908(8) 0.8658(6) 0.072(3) Uani 0.50 1 d P . . C49B C -0.1120(9) 0.4561(6) 0.9346(4) 0.058(2) Uani 0.50 1 d P . . C50 C -0.0649(5) 0.5543(4) 0.8661(3) 0.0683(13) Uani 1 1 d . . . C51 C 0.0448(4) 0.5289(3) 0.8045(2) 0.0526(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0397(3) 0.0344(2) 0.0306(2) -0.00446(17) -0.01003(17) 0.00214(17) Zn2 0.0380(2) 0.0373(2) 0.0306(2) -0.00276(17) -0.00859(17) 0.00079(18) O1 0.079(2) 0.066(2) 0.077(2) -0.0087(16) -0.0342(18) -0.0035(17) O2 0.0527(17) 0.0417(14) 0.0379(14) -0.0071(11) -0.0082(12) 0.0101(12) O3 0.074(2) 0.132(3) 0.082(2) -0.061(2) -0.0209(19) 0.003(2) O4 0.0454(15) 0.0494(15) 0.0380(14) -0.0132(12) -0.0035(11) -0.0010(12) O1W 0.147(4) 0.167(4) 0.116(4) -0.009(3) -0.026(3) -0.070(3) O2W 0.090(3) 0.068(2) 0.126(3) -0.019(2) -0.054(2) 0.0128(19) N1 0.0407(17) 0.0315(15) 0.0328(15) -0.0059(12) -0.0104(12) -0.0024(13) N2 0.0412(17) 0.0350(16) 0.0286(15) -0.0051(12) -0.0074(12) 0.0000(13) N3 0.0324(16) 0.0375(16) 0.0321(15) -0.0013(12) -0.0068(12) 0.0034(13) N4 0.0466(19) 0.0382(17) 0.0378(17) -0.0017(13) -0.0087(14) 0.0004(14) N5 0.0484(19) 0.0447(18) 0.0338(16) -0.0027(14) -0.0067(14) 0.0020(15) N6 0.0349(16) 0.0321(16) 0.0370(16) -0.0015(12) -0.0098(12) -0.0038(12) N7 0.0372(17) 0.0355(16) 0.0348(15) -0.0018(12) -0.0127(13) -0.0011(13) N8 0.0415(17) 0.0316(15) 0.0298(15) -0.0059(12) -0.0092(12) 0.0007(13) N9 0.0431(18) 0.0358(16) 0.0366(16) -0.0029(13) -0.0080(13) -0.0007(14) N10 0.0440(19) 0.0393(17) 0.0412(17) -0.0047(13) -0.0098(14) 0.0004(14) C1 0.072(3) 0.056(3) 0.068(3) -0.016(2) -0.029(2) -0.011(2) C2 0.095(4) 0.069(3) 0.094(4) -0.026(3) -0.037(3) -0.024(3) C3 0.095(4) 0.055(3) 0.075(3) -0.029(3) 0.003(3) -0.027(3) C4 0.074(3) 0.041(2) 0.060(3) -0.009(2) 0.000(2) 0.005(2) C5 0.048(2) 0.042(2) 0.042(2) -0.0117(17) -0.0039(17) 0.0016(18) C6 0.044(2) 0.040(2) 0.040(2) -0.0163(16) -0.0052(16) -0.0003(17) C7 0.0348(19) 0.040(2) 0.0363(19) -0.0130(16) -0.0081(15) 0.0004(15) C8 0.042(2) 0.045(2) 0.0338(19) -0.0133(16) -0.0134(15) 0.0024(16) C9 0.0328(19) 0.041(2) 0.0289(18) -0.0062(15) -0.0071(14) 0.0044(15) C10 0.0277(18) 0.042(2) 0.0320(18) -0.0068(15) -0.0065(14) 0.0077(15) C11 0.041(2) 0.051(2) 0.0332(19) -0.0075(17) -0.0101(16) 0.0077(17) C12 0.047(2) 0.062(3) 0.0294(19) -0.0036(18) -0.0110(16) 0.010(2) C13 0.045(2) 0.047(2) 0.038(2) 0.0070(17) -0.0063(17) 0.0034(18) C14 0.0308(19) 0.039(2) 0.0346(19) -0.0010(15) -0.0059(14) 0.0041(15) C15 0.0316(19) 0.040(2) 0.0358(19) 0.0005(15) -0.0047(15) 0.0025(15) C16 0.041(2) 0.038(2) 0.041(2) 0.0030(16) -0.0072(16) 0.0012(16) C17 0.035(2) 0.040(2) 0.044(2) -0.0034(16) -0.0025(16) 0.0020(16) C18 0.043(2) 0.043(2) 0.047(2) -0.0062(18) -0.0010(17) -0.0020(17) C19 0.086(3) 0.048(3) 0.058(3) 0.000(2) -0.016(2) -0.018(2) C20 0.117(5) 0.046(3) 0.075(3) -0.001(2) -0.007(3) -0.023(3) C21 0.091(4) 0.068(3) 0.074(3) -0.035(3) 0.014(3) -0.027(3) C22 0.103(4) 0.083(4) 0.079(4) -0.043(3) -0.032(3) 0.007(3) C23 0.087(4) 0.055(3) 0.067(3) -0.021(2) -0.025(3) 0.010(2) C24 0.038(2) 0.041(2) 0.043(2) -0.0127(16) -0.0076(16) -0.0011(16) C25 0.043(2) 0.046(2) 0.047(2) -0.0071(18) -0.0014(17) -0.0054(18) C26 0.045(2) 0.045(2) 0.067(3) -0.013(2) -0.001(2) -0.0100(18) C27 0.052(3) 0.060(3) 0.068(3) -0.031(2) -0.012(2) -0.013(2) C28 0.047(2) 0.061(3) 0.047(2) -0.0174(19) -0.0063(18) -0.012(2) C29 0.0281(18) 0.039(2) 0.040(2) -0.0094(16) -0.0068(15) 0.0010(15) C30 0.037(2) 0.040(2) 0.0346(19) -0.0104(16) -0.0094(15) -0.0004(16) C31 0.041(2) 0.046(2) 0.041(2) -0.0100(17) -0.0160(16) -0.0006(17) C32 0.041(2) 0.036(2) 0.0357(19) -0.0103(15) -0.0136(16) 0.0048(16) C33 0.049(2) 0.0337(19) 0.0301(18) -0.0086(14) -0.0124(16) 0.0046(16) C34 0.053(2) 0.047(2) 0.049(2) -0.0048(18) -0.0259(19) 0.0059(19) C35 0.067(3) 0.050(3) 0.054(2) -0.0047(19) -0.035(2) 0.011(2) C36 0.071(3) 0.036(2) 0.042(2) 0.0017(17) -0.023(2) 0.0020(19) C37 0.049(2) 0.0338(19) 0.0310(18) -0.0063(15) -0.0102(16) 0.0045(16) C38 0.056(2) 0.0322(19) 0.0248(17) -0.0058(14) -0.0092(16) 0.0025(17) C39 0.059(3) 0.037(2) 0.0325(19) -0.0042(15) -0.0100(17) 0.0005(18) C40 0.055(2) 0.037(2) 0.0314(19) -0.0088(16) 0.0002(17) -0.0014(17) C41 0.052(2) 0.043(2) 0.046(2) -0.0178(18) 0.0096(18) -0.0081(18) C42 0.075(3) 0.048(2) 0.050(2) -0.013(2) 0.009(2) -0.013(2) C43 0.099(4) 0.056(3) 0.075(3) -0.025(3) 0.029(3) -0.029(3) C44 0.066(4) 0.076(4) 0.119(5) -0.049(4) 0.024(3) -0.025(3) C45 0.061(3) 0.084(4) 0.111(4) -0.040(3) -0.009(3) -0.010(3) C46 0.064(3) 0.061(3) 0.075(3) -0.021(2) -0.007(2) -0.012(2) C47 0.057(3) 0.037(2) 0.040(2) 0.0060(17) -0.0019(19) 0.0027(19) C48 0.070(3) 0.051(3) 0.071(3) -0.005(2) 0.019(2) 0.019(2) C49A 0.077(7) 0.070(6) 0.057(6) -0.007(5) 0.004(5) 0.031(5) C49B 0.092(7) 0.040(4) 0.029(4) -0.005(3) 0.012(4) 0.014(4) C50 0.082(3) 0.064(3) 0.052(3) -0.022(2) 0.014(2) 0.001(3) C51 0.064(3) 0.045(2) 0.049(2) -0.0120(19) -0.009(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.966(2) . ? Zn1 N1 2.005(3) . ? Zn1 N8 2.123(3) . ? Zn1 N7 2.172(3) . ? Zn1 N9 2.305(3) . ? Zn2 O4 1.970(2) . ? Zn2 N6 2.003(3) . ? Zn2 N3 2.114(3) . ? Zn2 N2 2.191(3) . ? Zn2 N4 2.238(3) . ? O1 C47 1.232(5) . ? O2 C47 1.270(5) . ? O3 C51 1.247(5) . ? O4 C51 1.269(4) . ? N1 N2 1.356(3) . ? N1 C7 1.362(4) . ? N2 C9 1.350(4) . ? N3 C10 1.343(4) . ? N3 C14 1.347(4) . ? N4 N5 1.325(4) . ? N4 C15 1.328(4) . ? N5 C17 1.343(4) . ? N6 C30 1.354(4) . ? N6 N7 1.357(3) . ? N7 C32 1.346(4) . ? N8 C33 1.336(4) . ? N8 C37 1.353(4) . ? N9 C38 1.332(4) . ? N9 N10 1.341(4) . ? N10 C40 1.349(4) . ? C1 C2 1.365(6) . ? C1 C6 1.394(5) . ? C2 C3 1.365(7) . ? C3 C4 1.374(6) . ? C4 C5 1.385(5) . ? C5 C6 1.395(5) . ? C6 C7 1.469(5) . ? C7 C8 1.381(5) . ? C8 C9 1.393(5) . ? C9 C10 1.461(4) . ? C10 C11 1.390(4) . ? C11 C12 1.382(5) . ? C12 C13 1.376(5) . ? C13 C14 1.382(5) . ? C14 C15 1.469(5) . ? C15 C16 1.385(5) . ? C16 C17 1.382(5) . ? C17 C18 1.474(5) . ? C18 C23 1.373(5) . ? C18 C19 1.374(5) . ? C19 C20 1.376(6) . ? C20 C21 1.369(7) . ? C21 C22 1.375(7) . ? C22 C23 1.365(6) . ? C24 C25 1.381(5) . ? C24 C29 1.384(5) . ? C25 C26 1.382(5) . ? C26 C27 1.374(5) . ? C27 C28 1.372(5) . ? C28 C29 1.392(5) . ? C29 C30 1.482(4) . ? C30 C31 1.385(5) . ? C31 C32 1.383(5) . ? C32 C33 1.463(5) . ? C33 C34 1.388(5) . ? C34 C35 1.380(5) . ? C35 C36 1.367(5) . ? C36 C37 1.377(5) . ? C37 C38 1.465(5) . ? C38 C39 1.387(5) . ? C39 C40 1.380(5) . ? C40 C41 1.473(5) . ? C41 C42 1.383(5) . ? C41 C46 1.397(6) . ? C42 C43 1.384(6) . ? C43 C44 1.370(8) . ? C44 C45 1.370(7) . ? C45 C46 1.379(6) . ? C47 C48 1.529(6) . ? C48 C49A 1.464(10) . ? C48 C49B 1.572(10) . ? C49A C49B 1.537(13) . ? C49A C50 1.583(11) . ? C49B C50 1.515(8) . ? C50 C51 1.512(6) . ? 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 O2 Zn1 N1 118.99(10) . . ? O2 Zn1 N8 111.43(10) . . ? N1 Zn1 N8 129.26(10) . . ? O2 Zn1 N7 99.18(10) . . ? N1 Zn1 N7 91.69(10) . . ? N8 Zn1 N7 74.66(10) . . ? O2 Zn1 N9 95.33(10) . . ? N1 Zn1 N9 106.30(10) . . ? N8 Zn1 N9 73.09(10) . . ? N7 Zn1 N9 147.60(10) . . ? O4 Zn2 N6 116.93(11) . . ? O4 Zn2 N3 116.72(10) . . ? N6 Zn2 N3 126.10(11) . . ? O4 Zn2 N2 100.49(10) . . ? N6 Zn2 N2 90.56(10) . . ? N3 Zn2 N2 75.14(10) . . ? O4 Zn2 N4 94.40(10) . . ? N6 Zn2 N4 107.13(11) . . ? N3 Zn2 N4 73.45(10) . . ? N2 Zn2 N4 148.58(10) . . ? C47 O2 Zn1 119.7(3) . . ? C51 O4 Zn2 115.3(3) . . ? N2 N1 C7 108.4(3) . . ? N2 N1 Zn1 110.95(18) . . ? C7 N1 Zn1 140.6(2) . . ? C9 N2 N1 107.8(2) . . ? C9 N2 Zn2 114.5(2) . . ? N1 N2 Zn2 137.6(2) . . ? C10 N3 C14 120.1(3) . . ? C10 N3 Zn2 119.0(2) . . ? C14 N3 Zn2 120.9(2) . . ? N5 N4 C15 104.6(3) . . ? N5 N4 Zn2 140.0(2) . . ? C15 N4 Zn2 115.4(2) . . ? N4 N5 C17 114.1(3) . . ? C30 N6 N7 108.2(3) . . ? C30 N6 Zn2 138.9(2) . . ? N7 N6 Zn2 112.4(2) . . ? C32 N7 N6 107.5(3) . . ? C32 N7 Zn1 115.9(2) . . ? N6 N7 Zn1 136.5(2) . . ? C33 N8 C37 119.9(3) . . ? C33 N8 Zn1 118.9(2) . . ? C37 N8 Zn1 121.2(2) . . ? C38 N9 N10 104.9(3) . . ? C38 N9 Zn1 113.7(2) . . ? N10 N9 Zn1 141.4(2) . . ? N9 N10 C40 112.7(3) . . ? C2 C1 C6 121.7(4) . . ? C3 C2 C1 119.8(5) . . ? C2 C3 C4 120.3(4) . . ? C3 C4 C5 120.4(4) . . ? C4 C5 C6 119.9(4) . . ? C1 C6 C5 117.9(3) . . ? C1 C6 C7 120.0(3) . . ? C5 C6 C7 122.1(3) . . ? N1 C7 C8 109.1(3) . . ? N1 C7 C6 122.8(3) . . ? C8 C7 C6 128.1(3) . . ? C7 C8 C9 104.9(3) . . ? N2 C9 C8 109.7(3) . . ? N2 C9 C10 117.0(3) . . ? C8 C9 C10 133.3(3) . . ? N3 C10 C11 121.0(3) . . ? N3 C10 C9 114.2(3) . . ? C11 C10 C9 124.7(3) . . ? C12 C11 C10 118.7(3) . . ? C13 C12 C11 119.8(3) . . ? C12 C13 C14 119.1(3) . . ? N3 C14 C13 121.2(3) . . ? N3 C14 C15 113.4(3) . . ? C13 C14 C15 125.4(3) . . ? N4 C15 C16 110.8(3) . . ? N4 C15 C14 116.8(3) . . ? C16 C15 C14 132.4(3) . . ? C17 C16 C15 106.0(3) . . ? N5 C17 C16 104.5(3) . . ? N5 C17 C18 123.7(3) . . ? C16 C17 C18 131.8(3) . . ? C23 C18 C19 118.0(4) . . ? C23 C18 C17 122.3(4) . . ? C19 C18 C17 119.7(4) . . ? C18 C19 C20 121.1(5) . . ? C21 C20 C19 120.0(5) . . ? C20 C21 C22 119.3(4) . . ? C23 C22 C21 120.0(5) . . ? C22 C23 C18 121.5(5) . . ? C25 C24 C29 121.2(3) . . ? C24 C25 C26 119.5(4) . . ? C27 C26 C25 119.8(4) . . ? C28 C27 C26 120.8(4) . . ? C27 C28 C29 120.3(4) . . ? C24 C29 C28 118.5(3) . . ? C24 C29 C30 120.6(3) . . ? C28 C29 C30 121.0(3) . . ? N6 C30 C31 109.6(3) . . ? N6 C30 C29 121.0(3) . . ? C31 C30 C29 129.4(3) . . ? C32 C31 C30 104.2(3) . . ? N7 C32 C31 110.4(3) . . ? N7 C32 C33 115.9(3) . . ? C31 C32 C33 133.7(3) . . ? N8 C33 C34 121.2(3) . . ? N8 C33 C32 114.5(3) . . ? C34 C33 C32 124.3(3) . . ? C35 C34 C33 118.4(4) . . ? C36 C35 C34 120.3(4) . . ? C35 C36 C37 118.9(3) . . ? N8 C37 C36 121.2(3) . . ? N8 C37 C38 114.1(3) . . ? C36 C37 C38 124.7(3) . . ? N9 C38 C39 110.9(3) . . ? N9 C38 C37 117.8(3) . . ? C39 C38 C37 131.2(3) . . ? C40 C39 C38 105.8(3) . . ? N10 C40 C39 105.6(3) . . ? N10 C40 C41 123.9(4) . . ? C39 C40 C41 130.6(4) . . ? C42 C41 C46 119.3(4) . . ? C42 C41 C40 119.7(4) . . ? C46 C41 C40 121.0(4) . . ? C41 C42 C43 119.8(5) . . ? C44 C43 C42 120.7(5) . . ? C45 C44 C43 119.7(5) . . ? C44 C45 C46 120.8(5) . . ? C45 C46 C41 119.6(5) . . ? O1 C47 O2 124.8(4) . . ? O1 C47 C48 118.3(4) . . ? O2 C47 C48 116.8(4) . . ? C49A C48 C47 115.5(5) . . ? C49A C48 C49B 60.7(5) . . ? C47 C48 C49B 115.9(4) . . ? C48 C49A C49B 63.1(5) . . ? C48 C49A C50 115.5(7) . . ? C49B C49A C50 58.1(5) . . ? C50 C49B C49A 62.5(5) . . ? C50 C49B C48 113.2(6) . . ? C49A C49B C48 56.2(5) . . ? C51 C50 C49B 112.4(4) . . ? C51 C50 C49A 112.8(4) . . ? C49B C50 C49A 59.4(5) . . ? O3 C51 O4 122.5(4) . . ? O3 C51 C50 118.6(4) . . ? O4 C51 C50 118.8(4) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.503 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.063 _database_code_depnum_ccdc_archive 'CCDC 854267' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H38 N10 O3.50 Zn2' _chemical_formula_weight 953.67 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.358(4) _cell_length_b 15.040(6) _cell_length_c 15.209(6) _cell_angle_alpha 72.965(5) _cell_angle_beta 84.833(6) _cell_angle_gamma 81.685(5) _cell_volume 2454.8(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.121 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10266 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 23.08 _reflns_number_total 6738 _reflns_number_gt 4479 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1634P)^2^+6.1467P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6738 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1154 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2774 _refine_ls_wR_factor_gt 0.2475 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.08859(9) 0.72556(7) 0.04450(7) 0.0417(4) Uani 1 1 d . . . Zn2 Zn 0.27811(9) 0.85640(6) 0.11300(7) 0.0424(4) Uani 1 1 d . . . O1 O 0.2523(5) 0.6566(4) 0.0450(4) 0.0506(16) Uani 1 1 d . . . O2 O 0.3725(6) 0.7460(4) 0.0801(5) 0.0564(17) Uani 1 1 d . . . O1W O 0.4502(18) 0.6475(10) 0.3200(12) 0.110(7) Uani 0.50 1 d P . . H1WA H 0.4509 0.6960 0.3378 0.165 Uiso 0.50 1 d PR . . H1WB H 0.4333 0.6022 0.3658 0.165 Uiso 0.50 1 d PR . . O2W O 0.7485(9) 0.3223(8) 0.2177(7) 0.128(4) Uani 1 1 d . . . H2WA H 0.7193 0.2850 0.1956 0.192 Uiso 1 1 d R . . N1 N 0.0957(6) 0.8563(5) -0.0376(5) 0.0449(18) Uani 1 1 d . . . N2 N 0.1684(7) 0.8992(5) -0.0017(5) 0.0443(18) Uani 1 1 d . . . N3 N 0.3104(7) 0.9956(5) 0.0430(5) 0.0429(18) Uani 1 1 d . . . N4 N 0.4178(7) 0.8837(5) 0.1851(5) 0.051(2) Uani 1 1 d . . . N5 N 0.4811(8) 0.8390(6) 0.2576(5) 0.060(2) Uani 1 1 d . . . H5A H 0.4783 0.7813 0.2881 0.072 Uiso 1 1 calc R . . N6 N 0.1556(7) 0.8038(5) 0.2096(5) 0.0491(19) Uani 1 1 d . . . N7 N 0.0849(6) 0.7603(5) 0.1721(5) 0.0434(18) Uani 1 1 d . . . N8 N -0.0560(6) 0.6642(5) 0.1228(5) 0.0430(17) Uani 1 1 d . . . N9 N 0.0183(7) 0.6498(5) -0.0419(5) 0.0477(19) Uani 1 1 d . . . N10 N 0.0347(7) 0.6368(5) -0.1250(5) 0.0480(19) Uani 1 1 d . . . H10A H 0.0935 0.6544 -0.1628 0.058 Uiso 1 1 calc R . . C1 C 0.0162(10) 0.8954(8) -0.2693(7) 0.067(3) Uani 1 1 d . . . H1A H 0.0834 0.9238 -0.2956 0.081 Uiso 1 1 calc R . . C2 C -0.0518(13) 0.8630(10) -0.3222(8) 0.087(4) Uani 1 1 d . . . H2A H -0.0285 0.8658 -0.3830 0.105 Uiso 1 1 calc R . . C3 C -0.1576(12) 0.8258(9) -0.2809(9) 0.080(3) Uani 1 1 d . . . H3A H -0.2067 0.8067 -0.3158 0.096 Uiso 1 1 calc R . . C4 C -0.1877(9) 0.8176(7) -0.1909(8) 0.065(3) Uani 1 1 d . . . H4A H -0.2561 0.7911 -0.1644 0.078 Uiso 1 1 calc R . . C5 C -0.1209(8) 0.8470(6) -0.1390(7) 0.051(2) Uani 1 1 d . . . H5B H -0.1446 0.8417 -0.0777 0.061 Uiso 1 1 calc R . . C6 C -0.0172(9) 0.8851(6) -0.1756(6) 0.050(2) Uani 1 1 d . . . C7 C 0.0602(8) 0.9157(6) -0.1195(6) 0.045(2) Uani 1 1 d . . . C8 C 0.1078(9) 0.9982(6) -0.1365(6) 0.051(2) Uani 1 1 d . . . H8A H 0.0977 1.0508 -0.1871 0.061 Uiso 1 1 calc R . . C9 C 0.1752(8) 0.9845(6) -0.0596(6) 0.044(2) Uani 1 1 d . . . C10 C 0.2566(8) 1.0413(6) -0.0349(6) 0.041(2) Uani 1 1 d . . . C11 C 0.2811(9) 1.1312(6) -0.0856(7) 0.052(2) Uani 1 1 d . . . H11A H 0.2434 1.1624 -0.1399 0.063 Uiso 1 1 calc R . . C12 C 0.3622(9) 1.1726(7) -0.0534(7) 0.057(3) Uani 1 1 d . . . H12A H 0.3794 1.2326 -0.0855 0.068 Uiso 1 1 calc R . . C13 C 0.4178(9) 1.1238(6) 0.0274(7) 0.055(2) Uani 1 1 d . . . H13A H 0.4726 1.1506 0.0501 0.066 Uiso 1 1 calc R . . C14 C 0.3907(8) 1.0347(6) 0.0737(7) 0.050(2) Uani 1 1 d . . . C15 C 0.4471(8) 0.9721(6) 0.1581(6) 0.046(2) Uani 1 1 d . . . C16 C 0.5288(10) 0.9820(7) 0.2134(7) 0.063(3) Uani 1 1 d . . . H16A H 0.5627 1.0360 0.2085 0.075 Uiso 1 1 calc R . . C17 C 0.5517(10) 0.8962(8) 0.2782(7) 0.064(3) Uani 1 1 d . . . C18 C 0.6342(11) 0.8648(9) 0.3531(8) 0.074(3) Uani 1 1 d . . . C19 C 0.7144(11) 0.9195(11) 0.3611(9) 0.091(4) Uani 1 1 d . . . H19A H 0.7168 0.9796 0.3215 0.109 Uiso 1 1 calc R . . C20 C 0.7941(15) 0.8817(17) 0.4318(15) 0.133(7) Uani 1 1 d . . . H20A H 0.8499 0.9190 0.4374 0.160 Uiso 1 1 calc R . . C21 C 0.7965(16) 0.7965(15) 0.4920(11) 0.114(6) Uani 1 1 d . . . H21A H 0.8523 0.7754 0.5371 0.136 Uiso 1 1 calc R . . C22 C 0.7146(16) 0.7417(12) 0.4849(11) 0.119(6) Uani 1 1 d . . . H22A H 0.7123 0.6826 0.5264 0.143 Uiso 1 1 calc R . . C23 C 0.6341(14) 0.7745(12) 0.4151(9) 0.108(5) Uani 1 1 d . . . H23A H 0.5795 0.7363 0.4094 0.129 Uiso 1 1 calc R . . C24 C 0.2162(11) 0.9139(8) 0.3370(8) 0.074(3) Uani 1 1 d . . . H24A H 0.2063 0.9536 0.2777 0.089 Uiso 1 1 calc R . . C25 C 0.2749(14) 0.9417(10) 0.4005(11) 0.100(5) Uani 1 1 d . . . H25A H 0.3038 0.9995 0.3817 0.121 Uiso 1 1 calc R . . C26 C 0.2903(16) 0.8887(13) 0.4856(11) 0.121(6) Uani 1 1 d . . . H26A H 0.3300 0.9079 0.5263 0.145 Uiso 1 1 calc R . . C27 C 0.247(2) 0.8064(17) 0.5114(16) 0.159(8) Uiso 1 1 d . . . H27A H 0.2574 0.7681 0.5712 0.191 Uiso 1 1 calc R . . C28 C 0.1847(16) 0.7745(13) 0.4493(12) 0.129(6) Uiso 1 1 d . . . H28A H 0.1531 0.7179 0.4693 0.154 Uiso 1 1 calc R . . C29 C 0.1737(10) 0.8292(8) 0.3619(7) 0.062(3) Uani 1 1 d . . . C30 C 0.1173(10) 0.7935(7) 0.2982(6) 0.058(3) Uani 1 1 d . . . C31 C 0.0182(10) 0.7423(8) 0.3165(7) 0.065(3) Uani 1 1 d . . . H31A H -0.0274 0.7256 0.3714 0.078 Uiso 1 1 calc R . . C32 C 0.0042(8) 0.7231(6) 0.2371(6) 0.047(2) Uani 1 1 d . . . C33 C -0.0801(9) 0.6717(6) 0.2085(7) 0.051(2) Uani 1 1 d . . . C34 C -0.1760(10) 0.6340(7) 0.2626(7) 0.065(3) Uani 1 1 d . . . H34A H -0.1934 0.6414 0.3211 0.078 Uiso 1 1 calc R . . C35 C -0.2445(10) 0.5854(8) 0.2276(8) 0.068(3) Uani 1 1 d . . . H35A H -0.3088 0.5591 0.2628 0.082 Uiso 1 1 calc R . . C36 C -0.2179(9) 0.5755(7) 0.1393(8) 0.064(3) Uani 1 1 d . . . H36A H -0.2625 0.5419 0.1151 0.077 Uiso 1 1 calc R . . C37 C -0.1232(8) 0.6173(6) 0.0892(7) 0.051(2) Uani 1 1 d . . . C38 C -0.0815(8) 0.6119(6) -0.0059(6) 0.048(2) Uani 1 1 d . . . C39 C -0.1279(8) 0.5760(6) -0.0671(7) 0.050(2) Uani 1 1 d . . . H39A H -0.1965 0.5467 -0.0582 0.060 Uiso 1 1 calc R . . C40 C -0.0526(9) 0.5925(6) -0.1434(7) 0.051(2) Uani 1 1 d . . . C41 C -0.0597(9) 0.5724(6) -0.2325(7) 0.058(3) Uani 1 1 d . . . C42 C 0.0198(11) 0.6011(8) -0.3068(8) 0.075(3) Uani 1 1 d . . . H42A H 0.0805 0.6349 -0.3026 0.089 Uiso 1 1 calc R . . C43 C 0.0076(13) 0.5787(9) -0.3873(9) 0.089(4) Uani 1 1 d . . . H43A H 0.0618 0.5965 -0.4369 0.107 Uiso 1 1 calc R . . C44 C -0.0834(14) 0.5306(10) -0.3954(10) 0.092(4) Uani 1 1 d . . . H44A H -0.0923 0.5175 -0.4504 0.110 Uiso 1 1 calc R . . C45 C -0.1601(12) 0.5025(9) -0.3215(10) 0.084(4) Uani 1 1 d . . . H45A H -0.2204 0.4687 -0.3263 0.101 Uiso 1 1 calc R . . C46 C -0.1509(10) 0.5224(8) -0.2408(8) 0.066(3) Uani 1 1 d . . . H46A H -0.2049 0.5030 -0.1915 0.079 Uiso 1 1 calc R . . C47 C 0.3524(8) 0.6760(6) 0.0576(6) 0.046(2) Uani 1 1 d . . . C48 C 0.4618(9) 0.6114(7) 0.0419(9) 0.069(3) Uani 1 1 d . . . H48A H 0.5031 0.5879 0.0989 0.083 Uiso 1 1 calc R . . H48B H 0.5145 0.6481 -0.0037 0.083 Uiso 1 1 calc R . . C49 C 0.4415(8) 0.5285(6) 0.0107(8) 0.059(3) Uani 1 1 d . . . H49A H 0.3956 0.5507 -0.0440 0.089 Uiso 1 1 calc R . . H49B H 0.3952 0.4880 0.0584 0.089 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 Zn1 0.0400(7) 0.0369(6) 0.0487(7) -0.0142(5) -0.0008(5) -0.0033(5) Zn2 0.0504(7) 0.0343(6) 0.0449(6) -0.0158(5) -0.0028(5) -0.0030(5) O1 0.046(4) 0.040(3) 0.071(4) -0.025(3) -0.003(3) -0.002(3) O2 0.050(4) 0.043(4) 0.088(5) -0.036(3) -0.008(3) -0.004(3) O1W 0.147(18) 0.035(8) 0.113(14) 0.019(9) 0.010(12) 0.010(10) O2W 0.104(8) 0.166(10) 0.119(8) -0.038(7) 0.012(6) -0.053(7) N1 0.048(5) 0.038(4) 0.051(5) -0.014(4) -0.008(4) -0.007(3) N2 0.054(5) 0.033(4) 0.047(4) -0.013(4) -0.005(4) -0.005(3) N3 0.053(5) 0.036(4) 0.043(4) -0.017(3) -0.001(4) -0.003(4) N4 0.058(5) 0.052(5) 0.047(5) -0.018(4) -0.011(4) 0.000(4) N5 0.075(6) 0.051(5) 0.058(5) -0.022(4) -0.015(5) -0.001(4) N6 0.055(5) 0.047(4) 0.049(5) -0.019(4) 0.000(4) -0.006(4) N7 0.048(5) 0.039(4) 0.046(4) -0.015(3) 0.000(4) -0.006(4) N8 0.045(4) 0.033(4) 0.049(5) -0.008(3) -0.004(3) -0.005(3) N9 0.043(5) 0.048(4) 0.053(5) -0.017(4) 0.001(4) -0.003(4) N10 0.050(5) 0.044(4) 0.053(5) -0.017(4) 0.003(4) -0.010(4) C1 0.077(8) 0.079(7) 0.050(6) -0.015(5) -0.008(5) -0.026(6) C2 0.110(11) 0.112(10) 0.050(7) -0.032(7) -0.020(7) -0.012(9) C3 0.086(9) 0.082(8) 0.083(9) -0.028(7) -0.019(7) -0.024(7) C4 0.048(6) 0.069(7) 0.088(8) -0.037(6) -0.013(6) -0.001(5) C5 0.049(6) 0.047(5) 0.057(6) -0.021(5) -0.009(5) 0.012(5) C6 0.050(6) 0.047(5) 0.055(6) -0.020(5) -0.009(5) 0.005(5) C7 0.050(6) 0.039(5) 0.045(5) -0.013(4) -0.011(4) 0.006(4) C8 0.062(6) 0.040(5) 0.046(5) -0.007(4) -0.008(5) -0.001(5) C9 0.049(6) 0.042(5) 0.040(5) -0.017(4) -0.003(4) 0.004(4) C10 0.049(6) 0.033(5) 0.044(5) -0.018(4) 0.000(4) -0.004(4) C11 0.060(6) 0.030(5) 0.064(6) -0.014(4) -0.001(5) 0.003(4) C12 0.066(7) 0.039(5) 0.068(7) -0.019(5) 0.005(5) -0.010(5) C13 0.064(7) 0.037(5) 0.068(7) -0.022(5) -0.003(5) -0.008(5) C14 0.054(6) 0.044(5) 0.063(6) -0.035(5) 0.009(5) -0.004(5) C15 0.053(6) 0.037(5) 0.050(5) -0.017(4) -0.006(4) -0.003(4) C16 0.074(8) 0.055(7) 0.068(7) -0.029(6) -0.009(6) -0.013(6) C17 0.062(7) 0.069(7) 0.071(7) -0.039(6) -0.003(5) -0.006(6) C18 0.078(8) 0.088(9) 0.062(7) -0.039(7) -0.029(6) 0.021(7) C19 0.076(9) 0.127(11) 0.084(9) -0.047(8) -0.038(7) -0.001(8) C20 0.093(12) 0.19(2) 0.161(18) -0.114(16) -0.023(12) -0.004(13) C21 0.114(14) 0.150(16) 0.085(11) -0.065(11) -0.037(10) 0.044(13) C22 0.138(15) 0.115(13) 0.097(11) -0.025(9) -0.056(11) 0.029(11) C23 0.116(12) 0.130(13) 0.085(10) -0.035(9) -0.047(9) -0.005(10) C24 0.089(9) 0.063(7) 0.081(8) -0.042(6) -0.014(7) 0.002(6) C25 0.118(12) 0.096(10) 0.110(12) -0.063(9) -0.031(9) 0.000(9) C26 0.148(16) 0.144(15) 0.094(11) -0.057(11) -0.034(10) -0.026(12) C29 0.078(8) 0.070(7) 0.040(6) -0.018(5) 0.000(5) -0.011(6) C30 0.087(8) 0.048(6) 0.036(5) -0.010(4) 0.001(5) -0.005(6) C31 0.072(8) 0.077(7) 0.050(6) -0.026(5) 0.017(5) -0.014(6) C32 0.049(6) 0.043(5) 0.045(5) -0.011(4) 0.006(4) 0.000(4) C33 0.049(6) 0.042(5) 0.060(6) -0.019(5) 0.007(5) 0.001(5) C34 0.065(7) 0.066(7) 0.062(7) -0.017(5) 0.018(5) -0.017(6) C35 0.055(7) 0.075(7) 0.070(8) -0.012(6) 0.013(6) -0.018(6) C36 0.043(6) 0.068(7) 0.083(8) -0.017(6) -0.002(5) -0.017(5) C37 0.040(6) 0.047(5) 0.063(6) -0.013(5) -0.005(5) 0.005(4) C38 0.034(5) 0.042(5) 0.061(6) -0.009(5) -0.003(4) 0.004(4) C39 0.042(6) 0.041(5) 0.070(7) -0.015(5) -0.007(5) -0.011(4) C40 0.052(6) 0.045(5) 0.061(6) -0.019(5) -0.015(5) -0.004(5) C41 0.058(7) 0.043(5) 0.071(7) -0.018(5) -0.013(5) 0.006(5) C42 0.091(9) 0.078(8) 0.062(7) -0.023(6) -0.001(6) -0.027(7) C43 0.101(11) 0.096(10) 0.073(8) -0.030(7) 0.007(7) -0.017(8) C44 0.107(11) 0.098(10) 0.085(10) -0.046(8) -0.034(9) 0.000(9) C45 0.079(9) 0.087(9) 0.102(10) -0.044(8) -0.023(8) -0.016(7) C46 0.061(7) 0.078(7) 0.071(7) -0.035(6) -0.004(5) -0.019(6) C47 0.044(6) 0.039(5) 0.060(6) -0.020(4) -0.003(4) -0.005(4) C48 0.042(6) 0.065(7) 0.122(10) -0.061(7) -0.003(6) -0.004(5) C49 0.038(5) 0.045(5) 0.105(8) -0.043(6) 0.000(5) 0.001(4) _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 1.994(6) . ? Zn1 N1 2.005(7) . ? Zn1 N8 2.099(7) . ? Zn1 N7 2.149(7) . ? Zn1 N9 2.234(7) . ? Zn2 N6 1.997(8) . ? Zn2 O2 2.009(6) . ? Zn2 N3 2.120(7) . ? Zn2 N2 2.125(7) . ? Zn2 N4 2.157(7) . ? O1 C47 1.259(10) . ? O2 C47 1.253(10) . ? N1 N2 1.355(9) . ? N1 C7 1.359(10) . ? N2 C9 1.336(11) . ? N3 C10 1.335(10) . ? N3 C14 1.338(11) . ? N4 N5 1.325(10) . ? N4 C15 1.353(11) . ? N5 C17 1.372(12) . ? N6 C30 1.349(12) . ? N6 N7 1.361(10) . ? N7 C32 1.338(11) . ? N8 C37 1.334(11) . ? N8 C33 1.342(11) . ? N9 N10 1.327(10) . ? N9 C38 1.342(11) . ? N10 C40 1.362(11) . ? C1 C2 1.390(15) . ? C1 C6 1.410(14) . ? C2 C3 1.416(17) . ? C3 C4 1.355(16) . ? C4 C5 1.342(13) . ? C5 C6 1.384(13) . ? C6 C7 1.482(12) . ? C7 C8 1.370(12) . ? C8 C9 1.405(12) . ? C9 C10 1.483(12) . ? C10 C11 1.400(12) . ? C11 C12 1.380(13) . ? C12 C13 1.387(14) . ? C13 C14 1.382(13) . ? C14 C15 1.486(13) . ? C15 C16 1.358(13) . ? C16 C17 1.381(14) . ? C17 C18 1.466(15) . ? C18 C19 1.349(17) . ? C18 C23 1.408(18) . ? C19 C20 1.40(2) . ? C20 C21 1.34(2) . ? C21 C22 1.36(2) . ? C22 C23 1.394(18) . ? C24 C29 1.365(15) . ? C24 C25 1.410(16) . ? C25 C26 1.318(19) . ? C26 C27 1.34(2) . ? C27 C28 1.45(2) . ? C28 C29 1.349(19) . ? C29 C30 1.468(14) . ? C30 C31 1.416(14) . ? C31 C32 1.349(13) . ? C32 C33 1.481(13) . ? C33 C34 1.389(13) . ? C34 C35 1.375(15) . ? C35 C36 1.395(15) . ? C36 C37 1.378(13) . ? C37 C38 1.502(13) . ? C38 C39 1.378(13) . ? C39 C40 1.361(13) . ? C40 C41 1.484(13) . ? C41 C42 1.386(15) . ? C41 C46 1.399(14) . ? C42 C43 1.386(15) . ? C43 C44 1.378(17) . ? C44 C45 1.361(18) . ? C45 C46 1.363(15) . ? C47 C48 1.509(13) . ? C48 C49 1.511(12) . ? C49 C49 1.536(17) 2_665 ? 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 N1 107.6(3) . . ? O1 Zn1 N8 122.6(3) . . ? N1 Zn1 N8 129.8(3) . . ? O1 Zn1 N7 99.7(3) . . ? N1 Zn1 N7 96.1(3) . . ? N8 Zn1 N7 75.3(3) . . ? O1 Zn1 N9 94.2(3) . . ? N1 Zn1 N9 105.1(3) . . ? N8 Zn1 N9 74.6(3) . . ? N7 Zn1 N9 149.8(3) . . ? N6 Zn2 O2 105.9(3) . . ? N6 Zn2 N3 132.5(3) . . ? O2 Zn2 N3 121.5(3) . . ? N6 Zn2 N2 98.0(3) . . ? O2 Zn2 N2 96.6(3) . . ? N3 Zn2 N2 74.6(3) . . ? N6 Zn2 N4 106.0(3) . . ? O2 Zn2 N4 95.4(3) . . ? N3 Zn2 N4 74.7(3) . . ? N2 Zn2 N4 149.0(3) . . ? C47 O1 Zn1 132.5(6) . . ? C47 O2 Zn2 137.8(6) . . ? N2 N1 C7 108.0(7) . . ? N2 N1 Zn1 109.0(5) . . ? C7 N1 Zn1 142.7(6) . . ? C9 N2 N1 107.7(7) . . ? C9 N2 Zn2 117.4(6) . . ? N1 N2 Zn2 134.7(5) . . ? C10 N3 C14 120.3(7) . . ? C10 N3 Zn2 119.8(5) . . ? C14 N3 Zn2 119.8(6) . . ? N5 N4 C15 105.7(7) . . ? N5 N4 Zn2 137.5(6) . . ? C15 N4 Zn2 116.5(6) . . ? N4 N5 C17 111.7(8) . . ? C30 N6 N7 107.9(8) . . ? C30 N6 Zn2 144.2(7) . . ? N7 N6 Zn2 107.9(5) . . ? C32 N7 N6 108.2(7) . . ? C32 N7 Zn1 116.2(6) . . ? N6 N7 Zn1 135.1(6) . . ? C37 N8 C33 119.6(8) . . ? C37 N8 Zn1 121.2(6) . . ? C33 N8 Zn1 119.2(6) . . ? N10 N9 C38 104.9(7) . . ? N10 N9 Zn1 140.6(6) . . ? C38 N9 Zn1 114.0(6) . . ? N9 N10 C40 112.1(8) . . ? C2 C1 C6 119.7(11) . . ? C1 C2 C3 118.1(11) . . ? C4 C3 C2 120.5(11) . . ? C5 C4 C3 121.5(11) . . ? C4 C5 C6 120.8(10) . . ? C5 C6 C1 119.2(9) . . ? C5 C6 C7 122.2(9) . . ? C1 C6 C7 118.6(9) . . ? N1 C7 C8 110.1(8) . . ? N1 C7 C6 119.5(8) . . ? C8 C7 C6 130.4(8) . . ? C7 C8 C9 103.8(8) . . ? N2 C9 C8 110.4(8) . . ? N2 C9 C10 116.0(7) . . ? C8 C9 C10 133.4(8) . . ? N3 C10 C11 121.2(8) . . ? N3 C10 C9 112.1(7) . . ? C11 C10 C9 126.6(8) . . ? C12 C11 C10 118.8(9) . . ? C11 C12 C13 119.1(9) . . ? C14 C13 C12 119.3(9) . . ? N3 C14 C13 121.3(9) . . ? N3 C14 C15 113.2(8) . . ? C13 C14 C15 125.5(9) . . ? N4 C15 C16 110.6(8) . . ? N4 C15 C14 115.3(7) . . ? C16 C15 C14 134.0(9) . . ? C15 C16 C17 106.7(9) . . ? N5 C17 C16 105.3(9) . . ? N5 C17 C18 123.7(10) . . ? C16 C17 C18 130.9(10) . . ? C19 C18 C23 119.2(11) . . ? C19 C18 C17 120.9(12) . . ? C23 C18 C17 119.8(12) . . ? C18 C19 C20 116.9(15) . . ? C21 C20 C19 125.5(18) . . ? C20 C21 C22 117.6(16) . . ? C21 C22 C23 119.7(16) . . ? C22 C23 C18 120.9(15) . . ? C29 C24 C25 120.4(12) . . ? C26 C25 C24 122.3(15) . . ? C25 C26 C27 117.9(17) . . ? C26 C27 C28 122(2) . . ? C29 C28 C27 118.3(17) . . ? C28 C29 C24 118.7(12) . . ? C28 C29 C30 117.8(12) . . ? C24 C29 C30 123.5(9) . . ? N6 C30 C31 108.2(8) . . ? N6 C30 C29 123.8(10) . . ? C31 C30 C29 128.0(9) . . ? C32 C31 C30 105.1(9) . . ? N7 C32 C31 110.6(9) . . ? N7 C32 C33 115.6(8) . . ? C31 C32 C33 133.7(9) . . ? N8 C33 C34 121.5(9) . . ? N8 C33 C32 113.4(8) . . ? C34 C33 C32 125.1(9) . . ? C35 C34 C33 118.5(10) . . ? C34 C35 C36 120.1(10) . . ? C37 C36 C35 117.8(10) . . ? N8 C37 C36 122.5(9) . . ? N8 C37 C38 113.0(8) . . ? C36 C37 C38 124.4(9) . . ? N9 C38 C39 111.1(8) . . ? N9 C38 C37 116.7(8) . . ? C39 C38 C37 132.2(9) . . ? C40 C39 C38 105.8(8) . . ? C39 C40 N10 106.2(8) . . ? C39 C40 C41 129.9(9) . . ? N10 C40 C41 123.8(9) . . ? C42 C41 C46 119.4(10) . . ? C42 C41 C40 122.7(9) . . ? C46 C41 C40 117.9(10) . . ? C43 C42 C41 119.0(11) . . ? C44 C43 C42 121.3(12) . . ? C45 C44 C43 118.8(12) . . ? C44 C45 C46 121.9(12) . . ? C45 C46 C41 119.6(11) . . ? O2 C47 O1 126.7(8) . . ? O2 C47 C48 115.1(8) . . ? O1 C47 C48 118.2(8) . . ? C47 C48 C49 116.6(8) . . ? C48 C49 C49 112.7(10) . 2_665 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 23.08 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.614 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.140 _database_code_depnum_ccdc_archive 'CCDC 854268' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_7 #TrackingRef '7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H56 N10 O8 Zn2' _chemical_formula_weight 1127.85 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' _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 12.411(3) _cell_length_b 14.631(3) _cell_length_c 16.969(3) _cell_angle_alpha 66.11(3) _cell_angle_beta 78.09(3) _cell_angle_gamma 72.06(3) _cell_volume 2668.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.165 _exptl_crystal_size_min 0.207 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26029 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12045 _reflns_number_gt 8201 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+0.6866P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12045 _refine_ls_number_parameters 692 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1458 _refine_ls_wR_factor_gt 0.1269 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.027 _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 0.90202(3) 0.76770(3) 0.56316(2) 0.03847(11) Uani 1 1 d . . . Zn2 Zn 0.71592(3) 0.69075(2) 0.46577(2) 0.03740(11) Uani 1 1 d . . . N1 N 0.9600(2) 0.7793(2) 0.74120(18) 0.0449(6) Uani 1 1 d . . . H1B H 0.9081 0.7527 0.7771 0.054 Uiso 1 1 calc R . . N2 N 0.9728(2) 0.79584(19) 0.65669(17) 0.0417(6) Uani 1 1 d . . . N3 N 1.0221(2) 0.85138(18) 0.48976(17) 0.0391(6) Uani 1 1 d . . . N4 N 0.8784(2) 0.80430(18) 0.42840(16) 0.0392(6) Uani 1 1 d . . . N5 N 0.8116(2) 0.78686(19) 0.38494(16) 0.0404(6) Uani 1 1 d . . . N6 N 0.5145(2) 0.7766(2) 0.33370(17) 0.0423(6) Uani 1 1 d . . . H6A H 0.5018 0.8417 0.3222 0.051 Uiso 1 1 calc R . . N7 N 0.5891(2) 0.70372(19) 0.38834(16) 0.0399(6) Uani 1 1 d . . . N8 N 0.7293(2) 0.53919(18) 0.48100(17) 0.0398(6) Uani 1 1 d . . . N9 N 0.8484(2) 0.60004(18) 0.55136(17) 0.0418(6) Uani 1 1 d . . . N10 N 0.9067(2) 0.61901(19) 0.60066(17) 0.0411(6) Uani 1 1 d . . . O1 O 0.74377(17) 0.84475(16) 0.58927(14) 0.0433(5) Uani 1 1 d . . . H1C H 0.7240 0.8460 0.6397 0.065 Uiso 1 1 d R . . H1D H 0.6980 0.8206 0.5765 0.065 Uiso 1 1 d R . . O2 O 0.61764(19) 0.75154(17) 0.55131(15) 0.0475(5) Uani 1 1 d . . . O3 O 0.5610(3) 0.6058(2) 0.6083(2) 0.0792(9) Uani 1 1 d . . . O4 O 0.2319(2) 0.2725(2) 1.16417(19) 0.0733(8) Uani 1 1 d . A . O5 O 0.3302(2) 0.13500(19) 1.26107(16) 0.0601(7) Uani 1 1 d . A . C1 C 1.1188(5) 0.8416(5) 0.8683(3) 0.0946(18) Uani 1 1 d . . . H1A H 1.1756 0.8629 0.8254 0.114 Uiso 1 1 calc R . . C2 C 1.1159(6) 0.8454(6) 0.9488(4) 0.125(3) Uani 1 1 d . . . H2A H 1.1714 0.8684 0.9595 0.151 Uiso 1 1 calc R . . C3 C 1.0322(5) 0.8157(5) 1.0130(3) 0.1030(19) Uani 1 1 d . . . H3A H 1.0299 0.8198 1.0666 0.124 Uiso 1 1 calc R . . C4 C 0.9542(4) 0.7809(5) 0.9975(3) 0.0936(17) Uani 1 1 d . . . H4A H 0.8979 0.7596 1.0410 0.112 Uiso 1 1 calc R . . C5 C 0.9564(4) 0.7761(4) 0.9166(3) 0.0767(13) Uani 1 1 d . . . H5A H 0.9011 0.7519 0.9071 0.092 Uiso 1 1 calc R . . C6 C 1.0383(3) 0.8065(3) 0.8507(2) 0.0533(9) Uani 1 1 d . . . C7 C 1.0380(3) 0.8093(2) 0.7638(2) 0.0467(8) Uani 1 1 d . . . C8 C 1.1061(3) 0.8461(3) 0.6885(2) 0.0489(8) Uani 1 1 d . . . H8A H 1.1685 0.8717 0.6825 0.059 Uiso 1 1 calc R . . C9 C 1.0629(3) 0.8370(2) 0.6244(2) 0.0420(7) Uani 1 1 d . . . C10 C 1.0893(3) 0.8718(2) 0.5300(2) 0.0412(7) Uani 1 1 d . . . C11 C 1.1714(3) 0.9244(3) 0.4836(2) 0.0496(8) Uani 1 1 d . . . H11A H 1.2176 0.9384 0.5118 0.059 Uiso 1 1 calc R . . C12 C 1.1832(3) 0.9556(3) 0.3945(2) 0.0524(9) Uani 1 1 d . . . H12A H 1.2388 0.9900 0.3620 0.063 Uiso 1 1 calc R . . C13 C 1.1124(3) 0.9358(2) 0.3538(2) 0.0473(8) Uani 1 1 d . . . H13A H 1.1195 0.9570 0.2937 0.057 Uiso 1 1 calc R . . C14 C 1.0308(3) 0.8840(2) 0.4031(2) 0.0397(7) Uani 1 1 d . . . C15 C 0.9483(3) 0.8595(2) 0.3695(2) 0.0400(7) Uani 1 1 d . . . C16 C 0.9260(3) 0.8793(2) 0.2865(2) 0.0472(8) Uani 1 1 d . . . H16A H 0.9616 0.9158 0.2343 0.057 Uiso 1 1 calc R . . C17 C 0.8387(3) 0.8324(2) 0.2986(2) 0.0436(7) Uani 1 1 d . . . C18 C 0.7789(3) 0.8315(3) 0.2324(2) 0.0460(8) Uani 1 1 d . . . C19 C 0.7285(4) 0.9247(3) 0.1702(2) 0.0612(10) Uani 1 1 d . . . H19A H 0.7340 0.9865 0.1706 0.073 Uiso 1 1 calc R . . C20 C 0.6707(4) 0.9268(4) 0.1084(3) 0.0787(13) Uani 1 1 d . . . H20A H 0.6382 0.9894 0.0669 0.094 Uiso 1 1 calc R . . C21 C 0.6612(4) 0.8361(5) 0.1079(3) 0.0815(14) Uani 1 1 d . . . H21A H 0.6203 0.8376 0.0670 0.098 Uiso 1 1 calc R . . C22 C 0.7120(4) 0.7423(4) 0.1680(3) 0.0714(12) Uani 1 1 d . . . H22A H 0.7065 0.6809 0.1668 0.086 Uiso 1 1 calc R . . C23 C 0.7705(3) 0.7402(3) 0.2294(2) 0.0581(9) Uani 1 1 d . . . H23A H 0.8048 0.6771 0.2695 0.070 Uiso 1 1 calc R . . C24 C 0.3635(3) 0.9051(3) 0.1948(2) 0.0593(10) Uani 1 1 d . . . H24A H 0.4130 0.9362 0.2032 0.071 Uiso 1 1 calc R . . C25 C 0.2793(4) 0.9644(4) 0.1384(3) 0.0711(12) Uani 1 1 d . . . H25A H 0.2721 1.0350 0.1098 0.085 Uiso 1 1 calc R . . C26 C 0.2068(4) 0.9184(4) 0.1252(3) 0.0783(13) Uani 1 1 d . . . H26A H 0.1517 0.9577 0.0866 0.094 Uiso 1 1 calc R . . C27 C 0.2154(4) 0.8161(4) 0.1684(3) 0.0782(13) Uani 1 1 d . . . H27A H 0.1648 0.7859 0.1602 0.094 Uiso 1 1 calc R . . C28 C 0.2997(3) 0.7552(3) 0.2251(3) 0.0631(10) Uani 1 1 d . . . H28A H 0.3057 0.6848 0.2537 0.076 Uiso 1 1 calc R . . C29 C 0.3741(3) 0.8001(3) 0.2386(2) 0.0482(8) Uani 1 1 d . . . C30 C 0.4613(3) 0.7356(3) 0.2986(2) 0.0431(7) Uani 1 1 d . . . C31 C 0.5052(3) 0.6294(3) 0.3331(2) 0.0462(8) Uani 1 1 d . . . H31A H 0.4859 0.5795 0.3220 0.055 Uiso 1 1 calc R . . C32 C 0.5841(3) 0.6134(2) 0.38771(19) 0.0386(7) Uani 1 1 d . . . C33 C 0.6573(3) 0.5198(2) 0.4447(2) 0.0391(7) Uani 1 1 d . . . C34 C 0.6528(3) 0.4197(2) 0.4628(2) 0.0466(8) Uani 1 1 d . . . H34A H 0.6032 0.4065 0.4368 0.056 Uiso 1 1 calc R . . C35 C 0.7243(3) 0.3402(2) 0.5208(2) 0.0515(9) Uani 1 1 d . . . H35A H 0.7238 0.2722 0.5335 0.062 Uiso 1 1 calc R . . C36 C 0.7965(3) 0.3605(2) 0.5601(2) 0.0482(8) Uani 1 1 d . . . H36A H 0.8445 0.3069 0.5993 0.058 Uiso 1 1 calc R . . C37 C 0.7961(3) 0.4626(2) 0.5399(2) 0.0412(7) Uani 1 1 d . . . C38 C 0.8596(3) 0.4973(2) 0.5818(2) 0.0406(7) Uani 1 1 d . . . C39 C 0.9241(3) 0.4485(2) 0.6520(2) 0.0482(8) Uani 1 1 d . . . H39A H 0.9439 0.3783 0.6850 0.058 Uiso 1 1 calc R . . C40 C 0.9526(3) 0.5273(2) 0.6621(2) 0.0430(7) Uani 1 1 d . . . C41 C 1.0163(3) 0.5233(2) 0.7283(2) 0.0484(8) Uani 1 1 d . . . C42 C 1.1143(3) 0.5583(3) 0.7043(3) 0.0655(11) Uani 1 1 d . . . H42A H 1.1409 0.5832 0.6461 0.079 Uiso 1 1 calc R . . C43 C 1.1721(4) 0.5566(4) 0.7655(5) 0.0936(17) Uani 1 1 d . . . H43A H 1.2385 0.5793 0.7486 0.112 Uiso 1 1 calc R . . C44 C 1.1338(6) 0.5219(4) 0.8509(5) 0.113(2) Uani 1 1 d . . . H44A H 1.1731 0.5220 0.8919 0.136 Uiso 1 1 calc R . . C45 C 1.0378(7) 0.4871(5) 0.8760(3) 0.117(2) Uani 1 1 d . . . H45A H 1.0117 0.4631 0.9343 0.141 Uiso 1 1 calc R . . C46 C 0.9787(5) 0.4872(4) 0.8148(3) 0.0842(15) Uani 1 1 d . . . H46A H 0.9134 0.4628 0.8324 0.101 Uiso 1 1 calc R . . C47 C 0.5661(3) 0.6855(3) 0.6129(2) 0.0561(9) Uani 1 1 d . . . C48 C 0.5115(5) 0.7144(4) 0.6897(3) 0.0897(16) Uani 1 1 d . A . H48A H 0.4455 0.7721 0.6726 0.108 Uiso 1 1 calc R . . H48B H 0.5648 0.7376 0.7072 0.108 Uiso 1 1 calc R . . C49 C 0.4745(6) 0.6279(5) 0.7672(4) 0.106(2) Uani 1 1 d . . . H49A H 0.4294 0.6564 0.8096 0.128 Uiso 1 1 d R A . H49B H 0.4257 0.6009 0.7490 0.128 Uiso 1 1 d R . . C50A C 0.5639(7) 0.5413(5) 0.8118(4) 0.132(3) Uani 0.686(7) 1 d PDU A 1 H50A H 0.6046 0.5625 0.8417 0.158 Uiso 0.686(7) 1 calc PR A 1 H50B H 0.6176 0.5152 0.7708 0.158 Uiso 0.686(7) 1 calc PR A 1 C51A C 0.5029(8) 0.4538(7) 0.8798(5) 0.116(3) Uani 0.686(7) 1 d PDU A 1 H51A H 0.4393 0.4835 0.9134 0.139 Uiso 0.686(7) 1 calc PR A 1 H51B H 0.4746 0.4233 0.8495 0.139 Uiso 0.686(7) 1 calc PR A 1 C52A C 0.5923(7) 0.3712(6) 0.9395(6) 0.110(3) Uani 0.686(7) 1 d PDU A 1 H52A H 0.6620 0.3506 0.9058 0.132 Uiso 0.686(7) 1 calc PR A 1 H52B H 0.6095 0.3972 0.9785 0.132 Uiso 0.686(7) 1 calc PR A 1 C53A C 0.5393(6) 0.2814(6) 0.9894(4) 0.138(3) Uani 0.686(7) 1 d PDU A 1 H53A H 0.5263 0.2574 0.9474 0.166 Uiso 0.686(7) 1 calc PR A 1 H53B H 0.5963 0.2262 1.0247 0.166 Uiso 0.686(7) 1 calc PR A 1 C50B C 0.5639(7) 0.5413(5) 0.8118(4) 0.132(3) Uani 0.314(7) 1 d PD A 2 H50C H 0.6265 0.5742 0.7930 0.158 Uiso 0.314(7) 1 calc PR A 2 H50D H 0.5778 0.5005 0.7760 0.158 Uiso 0.314(7) 1 calc PR A 2 C51B C 0.6059(16) 0.4552(11) 0.8963(9) 0.116(3) Uani 0.314(7) 1 d PD A 2 H51C H 0.5933 0.4802 0.9433 0.139 Uiso 0.314(7) 1 calc PR A 2 H51D H 0.6853 0.4199 0.8893 0.139 Uiso 0.314(7) 1 calc PR A 2 C52B C 0.5247(17) 0.3871(12) 0.9083(12) 0.110(3) Uani 0.314(7) 1 d PD A 2 H52C H 0.5354 0.3715 0.8564 0.132 Uiso 0.314(7) 1 calc PR A 2 H52D H 0.4470 0.4276 0.9129 0.132 Uiso 0.314(7) 1 calc PR A 2 C53B C 0.5393(6) 0.2814(6) 0.9894(4) 0.138(3) Uani 0.314(7) 1 d PD A 2 H53C H 0.5508 0.2239 0.9713 0.166 Uiso 0.314(7) 1 calc PR A 2 H53D H 0.6040 0.2700 1.0190 0.166 Uiso 0.314(7) 1 calc PR A 2 C54 C 0.4316(5) 0.2919(4) 1.0473(3) 0.104(2) Uani 1 1 d . . . H54A H 0.4259 0.3454 1.0689 0.125 Uiso 1 1 d R A . H54B H 0.3677 0.3141 1.0135 0.125 Uiso 1 1 d R . . C55 C 0.4219(4) 0.1963(4) 1.1217(3) 0.0841(14) Uani 1 1 d . A . H55A H 0.4894 0.1715 1.1523 0.101 Uiso 1 1 calc R . . H55B H 0.4225 0.1446 1.0995 0.101 Uiso 1 1 calc R . . C56 C 0.3192(3) 0.2031(3) 1.1865(2) 0.0539(9) Uani 1 1 d . . . O1W O 0.6750(4) 1.0227(3) 0.3680(4) 0.155(2) Uani 1 1 d . . . H1W H 0.7325 0.9701 0.3773 0.232 Uiso 1 1 d R . . H2W H 0.6300 1.0149 0.4149 0.232 Uiso 1 1 d R . . O2W O 0.4373(6) 0.9213(5) 0.5038(4) 0.253(4) Uani 1 1 d . . . H3W H 0.4915 0.8592 0.5229 0.379 Uiso 1 1 d R . . H4W H 0.4641 0.9504 0.4518 0.379 Uiso 1 1 d R . . O3W O 0.4983(2) 0.9719(2) 0.3257(2) 0.0766(9) Uani 1 1 d . . . H6W H 0.4568 1.0323 0.3034 0.115 Uiso 1 1 d R . . H5W H 0.5652 0.9736 0.3260 0.115 Uiso 1 1 d 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 Zn1 0.0389(2) 0.03506(19) 0.0415(2) -0.01048(15) -0.00145(15) -0.01570(15) Zn2 0.0436(2) 0.03183(18) 0.0376(2) -0.00957(14) -0.00544(15) -0.01386(15) N1 0.0428(15) 0.0496(15) 0.0444(15) -0.0128(12) -0.0049(12) -0.0200(12) N2 0.0404(14) 0.0413(14) 0.0459(15) -0.0140(12) -0.0024(12) -0.0173(12) N3 0.0370(13) 0.0351(13) 0.0434(15) -0.0121(11) 0.0016(11) -0.0134(11) N4 0.0437(14) 0.0355(13) 0.0359(13) -0.0063(10) -0.0025(11) -0.0168(11) N5 0.0458(15) 0.0404(13) 0.0350(13) -0.0097(11) -0.0045(11) -0.0162(12) N6 0.0455(15) 0.0395(14) 0.0409(15) -0.0122(11) -0.0095(12) -0.0092(12) N7 0.0430(14) 0.0383(13) 0.0394(14) -0.0125(11) -0.0083(11) -0.0111(11) N8 0.0454(15) 0.0321(12) 0.0422(14) -0.0126(11) -0.0044(12) -0.0115(11) N9 0.0503(16) 0.0310(12) 0.0445(15) -0.0092(11) -0.0110(12) -0.0127(11) N10 0.0434(15) 0.0377(13) 0.0419(14) -0.0077(11) -0.0118(12) -0.0140(11) O1 0.0390(12) 0.0488(12) 0.0491(13) -0.0230(10) -0.0012(10) -0.0158(10) O2 0.0457(13) 0.0562(13) 0.0469(13) -0.0229(11) 0.0049(10) -0.0217(11) O3 0.103(2) 0.092(2) 0.075(2) -0.0463(17) 0.0210(17) -0.0650(19) O4 0.0564(17) 0.0794(19) 0.0649(18) -0.0013(15) -0.0031(14) -0.0270(15) O5 0.0669(17) 0.0602(15) 0.0464(14) -0.0175(12) 0.0011(12) -0.0137(13) C1 0.100(4) 0.154(5) 0.056(3) -0.032(3) -0.008(3) -0.076(4) C2 0.141(6) 0.212(7) 0.072(4) -0.053(4) -0.006(4) -0.112(6) C3 0.112(4) 0.160(5) 0.056(3) -0.041(3) -0.016(3) -0.054(4) C4 0.083(3) 0.149(5) 0.053(3) -0.029(3) -0.005(2) -0.046(3) C5 0.071(3) 0.110(4) 0.060(3) -0.029(2) -0.009(2) -0.040(3) C6 0.054(2) 0.054(2) 0.050(2) -0.0108(16) -0.0155(17) -0.0159(17) C7 0.0461(18) 0.0414(17) 0.055(2) -0.0151(15) -0.0100(16) -0.0145(14) C8 0.0427(18) 0.0496(19) 0.061(2) -0.0199(16) -0.0074(16) -0.0188(15) C9 0.0366(16) 0.0397(16) 0.0541(19) -0.0188(14) 0.0005(14) -0.0167(13) C10 0.0405(17) 0.0350(15) 0.0506(19) -0.0170(14) 0.0010(14) -0.0146(13) C11 0.0478(19) 0.0462(18) 0.063(2) -0.0238(16) 0.0007(16) -0.0224(15) C12 0.0492(19) 0.0475(19) 0.066(2) -0.0227(17) 0.0105(17) -0.0266(16) C13 0.0502(19) 0.0390(17) 0.0480(19) -0.0118(14) 0.0058(15) -0.0174(15) C14 0.0376(16) 0.0303(14) 0.0453(18) -0.0100(13) 0.0012(13) -0.0092(12) C15 0.0406(17) 0.0344(15) 0.0398(17) -0.0074(13) 0.0010(13) -0.0138(13) C16 0.0490(19) 0.0445(18) 0.0391(17) -0.0044(14) 0.0005(15) -0.0173(15) C17 0.0485(19) 0.0418(17) 0.0363(16) -0.0087(13) -0.0013(14) -0.0148(14) C18 0.0477(19) 0.0522(19) 0.0354(16) -0.0144(14) 0.0033(14) -0.0159(15) C19 0.074(3) 0.062(2) 0.043(2) -0.0096(17) -0.0090(18) -0.021(2) C20 0.085(3) 0.095(3) 0.048(2) -0.015(2) -0.015(2) -0.020(3) C21 0.081(3) 0.128(4) 0.051(2) -0.041(3) -0.001(2) -0.040(3) C22 0.082(3) 0.096(3) 0.061(3) -0.049(3) 0.015(2) -0.040(3) C23 0.066(2) 0.062(2) 0.049(2) -0.0251(17) 0.0073(18) -0.0212(19) C24 0.057(2) 0.072(2) 0.046(2) -0.0154(18) -0.0080(17) -0.0191(19) C25 0.068(3) 0.081(3) 0.051(2) -0.009(2) -0.016(2) -0.013(2) C26 0.059(3) 0.117(4) 0.051(2) -0.027(3) -0.021(2) -0.006(3) C27 0.065(3) 0.113(4) 0.067(3) -0.034(3) -0.024(2) -0.024(3) C28 0.065(2) 0.079(3) 0.057(2) -0.029(2) -0.013(2) -0.024(2) C29 0.0459(19) 0.066(2) 0.0359(17) -0.0221(16) -0.0030(14) -0.0152(16) C30 0.0410(17) 0.0568(19) 0.0358(16) -0.0188(14) -0.0027(13) -0.0162(15) C31 0.052(2) 0.0510(19) 0.0454(18) -0.0229(15) 0.0005(15) -0.0221(16) C32 0.0431(17) 0.0406(16) 0.0360(16) -0.0165(13) 0.0004(13) -0.0153(13) C33 0.0446(17) 0.0371(15) 0.0375(16) -0.0159(13) 0.0023(13) -0.0140(13) C34 0.056(2) 0.0441(18) 0.0485(19) -0.0235(15) 0.0036(16) -0.0205(16) C35 0.064(2) 0.0350(16) 0.057(2) -0.0182(15) 0.0016(18) -0.0176(16) C36 0.055(2) 0.0318(15) 0.054(2) -0.0152(14) -0.0031(16) -0.0090(14) C37 0.0442(17) 0.0331(15) 0.0430(17) -0.0128(13) -0.0029(14) -0.0077(13) C38 0.0469(18) 0.0302(14) 0.0412(17) -0.0088(12) -0.0074(14) -0.0087(13) C39 0.055(2) 0.0312(15) 0.052(2) -0.0037(14) -0.0157(16) -0.0109(14) C40 0.0421(17) 0.0414(17) 0.0399(17) -0.0063(13) -0.0079(14) -0.0117(14) C41 0.054(2) 0.0358(16) 0.050(2) -0.0058(14) -0.0162(16) -0.0094(14) C42 0.047(2) 0.067(2) 0.082(3) -0.026(2) -0.015(2) -0.0096(18) C43 0.066(3) 0.090(3) 0.139(5) -0.050(4) -0.048(3) -0.003(3) C44 0.145(6) 0.084(4) 0.128(6) -0.040(4) -0.089(5) -0.002(4) C45 0.177(7) 0.122(5) 0.055(3) -0.012(3) -0.044(4) -0.046(5) C46 0.105(4) 0.096(3) 0.055(3) -0.011(2) -0.014(2) -0.050(3) C47 0.059(2) 0.070(2) 0.056(2) -0.0300(19) 0.0066(17) -0.0366(19) C48 0.118(4) 0.092(3) 0.074(3) -0.047(3) 0.038(3) -0.054(3) C49 0.151(6) 0.101(4) 0.078(4) -0.045(3) 0.051(4) -0.068(4) C50A 0.220(9) 0.110(5) 0.084(4) -0.033(4) 0.001(5) -0.082(5) C51A 0.140(7) 0.129(7) 0.079(5) -0.035(4) 0.017(4) -0.056(5) C52A 0.097(6) 0.132(6) 0.109(7) -0.046(4) 0.024(4) -0.060(5) C53A 0.150(6) 0.156(6) 0.094(4) -0.030(4) 0.058(4) -0.087(5) C50B 0.220(9) 0.110(5) 0.084(4) -0.033(4) 0.001(5) -0.082(5) C51B 0.140(7) 0.129(7) 0.079(5) -0.035(4) 0.017(4) -0.056(5) C52B 0.097(6) 0.132(6) 0.109(7) -0.046(4) 0.024(4) -0.060(5) C53B 0.150(6) 0.156(6) 0.094(4) -0.030(4) 0.058(4) -0.087(5) C54 0.136(5) 0.096(4) 0.086(4) -0.045(3) 0.059(3) -0.063(4) C55 0.081(3) 0.100(4) 0.058(3) -0.020(2) 0.013(2) -0.031(3) C56 0.057(2) 0.061(2) 0.047(2) -0.0157(17) 0.0011(17) -0.0294(19) O1W 0.094(3) 0.116(3) 0.287(7) -0.107(4) -0.036(4) -0.013(3) O2W 0.187(6) 0.276(8) 0.142(5) -0.019(5) -0.034(5) 0.083(5) O3W 0.0681(18) 0.0548(16) 0.109(3) -0.0322(16) -0.0202(17) -0.0085(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 Zn1 N10 1.989(2) . ? Zn1 O1 2.002(2) . ? Zn1 N3 2.096(2) . ? Zn1 N2 2.188(3) . ? Zn1 N4 2.188(3) . ? Zn2 O2 2.008(2) . ? Zn2 N5 2.016(2) . ? Zn2 N8 2.083(2) . ? Zn2 N9 2.157(3) . ? Zn2 N7 2.169(3) . ? N1 N2 1.338(4) . ? N1 C7 1.351(4) . ? N2 C9 1.345(4) . ? N3 C14 1.341(4) . ? N3 C10 1.343(4) . ? N4 C15 1.350(4) . ? N4 N5 1.353(4) . ? N5 C17 1.359(4) . ? N6 N7 1.341(4) . ? N6 C30 1.358(4) . ? N7 C32 1.346(4) . ? N8 C33 1.336(4) . ? N8 C37 1.343(4) . ? N9 C38 1.349(4) . ? N9 N10 1.365(4) . ? N10 C40 1.361(4) . ? O2 C47 1.312(4) . ? O3 C47 1.222(4) . ? O4 C56 1.237(5) . ? O5 C56 1.257(4) . ? C1 C2 1.381(7) . ? C1 C6 1.383(5) . ? C2 C3 1.372(7) . ? C3 C4 1.336(7) . ? C4 C5 1.397(6) . ? C5 C6 1.375(5) . ? C6 C7 1.460(5) . ? C7 C8 1.383(5) . ? C8 C9 1.374(5) . ? C9 C10 1.470(5) . ? C10 C11 1.382(4) . ? C11 C12 1.381(5) . ? C12 C13 1.380(5) . ? C13 C14 1.382(4) . ? C14 C15 1.462(4) . ? C15 C16 1.388(5) . ? C16 C17 1.393(4) . ? C17 C18 1.474(5) . ? C18 C23 1.394(5) . ? C18 C19 1.395(5) . ? C19 C20 1.374(6) . ? C20 C21 1.371(7) . ? C21 C22 1.386(7) . ? C22 C23 1.373(6) . ? C24 C29 1.385(5) . ? C24 C25 1.394(5) . ? C25 C26 1.375(6) . ? C26 C27 1.355(6) . ? C27 C28 1.400(6) . ? C28 C29 1.386(5) . ? C29 C30 1.465(5) . ? C30 C31 1.388(5) . ? C31 C32 1.389(4) . ? C32 C33 1.469(4) . ? C33 C34 1.386(4) . ? C34 C35 1.380(5) . ? C35 C36 1.382(5) . ? C36 C37 1.389(4) . ? C37 C38 1.467(4) . ? C38 C39 1.386(4) . ? C39 C40 1.386(5) . ? C40 C41 1.474(5) . ? C41 C46 1.377(5) . ? C41 C42 1.384(5) . ? C42 C43 1.368(7) . ? C43 C44 1.361(8) . ? C44 C45 1.359(9) . ? C45 C46 1.388(7) . ? C47 C48 1.498(6) . ? C48 C49 1.518(6) . ? C49 C50A 1.454(9) . ? C50A C51A 1.608(7) . ? C51A C52A 1.537(8) . ? C52A C53A 1.510(7) . ? C53A C54 1.493(7) . ? C51B C52B 1.555(9) . ? C54 C55 1.476(6) . ? C55 C56 1.509(6) . ? 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 N10 Zn1 O1 109.07(10) . . ? N10 Zn1 N3 131.31(11) . . ? O1 Zn1 N3 118.93(9) . . ? N10 Zn1 N2 111.19(10) . . ? O1 Zn1 N2 93.48(10) . . ? N3 Zn1 N2 74.86(10) . . ? N10 Zn1 N4 94.54(10) . . ? O1 Zn1 N4 94.03(10) . . ? N3 Zn1 N4 75.22(10) . . ? N2 Zn1 N4 149.04(9) . . ? O2 Zn2 N5 109.61(10) . . ? O2 Zn2 N8 120.88(10) . . ? N5 Zn2 N8 128.60(11) . . ? O2 Zn2 N9 93.42(10) . . ? N5 Zn2 N9 92.94(10) . . ? N8 Zn2 N9 75.90(10) . . ? O2 Zn2 N7 100.90(10) . . ? N5 Zn2 N7 105.16(10) . . ? N8 Zn2 N7 75.47(10) . . ? N9 Zn2 N7 151.36(9) . . ? N2 N1 C7 112.4(3) . . ? N1 N2 C9 105.1(3) . . ? N1 N2 Zn1 140.07(19) . . ? C9 N2 Zn1 114.7(2) . . ? C14 N3 C10 120.7(3) . . ? C14 N3 Zn1 119.6(2) . . ? C10 N3 Zn1 119.7(2) . . ? C15 N4 N5 107.9(2) . . ? C15 N4 Zn1 114.4(2) . . ? N5 N4 Zn1 137.73(18) . . ? N4 N5 C17 108.6(2) . . ? N4 N5 Zn2 111.70(18) . . ? C17 N5 Zn2 139.2(2) . . ? N7 N6 C30 112.1(3) . . ? N6 N7 C32 105.4(2) . . ? N6 N7 Zn2 139.72(19) . . ? C32 N7 Zn2 114.7(2) . . ? C33 N8 C37 121.1(3) . . ? C33 N8 Zn2 119.6(2) . . ? C37 N8 Zn2 118.2(2) . . ? C38 N9 N10 107.7(2) . . ? C38 N9 Zn2 114.6(2) . . ? N10 N9 Zn2 135.39(19) . . ? C40 N10 N9 108.1(2) . . ? C40 N10 Zn1 138.7(2) . . ? N9 N10 Zn1 113.20(18) . . ? C47 O2 Zn2 111.8(2) . . ? C2 C1 C6 121.0(5) . . ? C3 C2 C1 120.8(5) . . ? C4 C3 C2 119.2(5) . . ? C3 C4 C5 120.6(5) . . ? C6 C5 C4 121.5(4) . . ? C5 C6 C1 116.9(4) . . ? C5 C6 C7 122.7(3) . . ? C1 C6 C7 120.3(3) . . ? N1 C7 C8 105.8(3) . . ? N1 C7 C6 123.5(3) . . ? C8 C7 C6 130.6(3) . . ? C9 C8 C7 106.0(3) . . ? N2 C9 C8 110.8(3) . . ? N2 C9 C10 116.3(3) . . ? C8 C9 C10 132.7(3) . . ? N3 C10 C11 121.1(3) . . ? N3 C10 C9 113.6(3) . . ? C11 C10 C9 125.2(3) . . ? C12 C11 C10 118.5(3) . . ? C13 C12 C11 119.9(3) . . ? C12 C13 C14 119.3(3) . . ? N3 C14 C13 120.5(3) . . ? N3 C14 C15 113.9(3) . . ? C13 C14 C15 125.6(3) . . ? N4 C15 C16 109.9(3) . . ? N4 C15 C14 116.9(3) . . ? C16 C15 C14 133.3(3) . . ? C15 C16 C17 104.8(3) . . ? N5 C17 C16 108.8(3) . . ? N5 C17 C18 122.8(3) . . ? C16 C17 C18 128.4(3) . . ? C23 C18 C19 118.1(4) . . ? C23 C18 C17 122.3(3) . . ? C19 C18 C17 119.6(3) . . ? C20 C19 C18 121.1(4) . . ? C21 C20 C19 119.8(4) . . ? C20 C21 C22 120.4(4) . . ? C23 C22 C21 119.8(4) . . ? C22 C23 C18 120.7(4) . . ? C29 C24 C25 120.5(4) . . ? C26 C25 C24 119.9(4) . . ? C27 C26 C25 120.1(4) . . ? C26 C27 C28 120.8(4) . . ? C29 C28 C27 119.8(4) . . ? C24 C29 C28 118.8(4) . . ? C24 C29 C30 122.0(3) . . ? C28 C29 C30 119.2(3) . . ? N6 C30 C31 106.2(3) . . ? N6 C30 C29 122.0(3) . . ? C31 C30 C29 131.8(3) . . ? C30 C31 C32 105.5(3) . . ? N7 C32 C31 110.8(3) . . ? N7 C32 C33 116.2(3) . . ? C31 C32 C33 132.9(3) . . ? N8 C33 C34 121.4(3) . . ? N8 C33 C32 113.5(3) . . ? C34 C33 C32 125.0(3) . . ? C35 C34 C33 117.8(3) . . ? C34 C35 C36 120.7(3) . . ? C35 C36 C37 118.7(3) . . ? N8 C37 C36 120.1(3) . . ? N8 C37 C38 114.6(3) . . ? C36 C37 C38 125.2(3) . . ? N9 C38 C39 110.1(3) . . ? N9 C38 C37 115.5(3) . . ? C39 C38 C37 134.2(3) . . ? C40 C39 C38 104.9(3) . . ? N10 C40 C39 109.2(3) . . ? N10 C40 C41 120.8(3) . . ? C39 C40 C41 129.9(3) . . ? C46 C41 C42 118.5(4) . . ? C46 C41 C40 121.0(3) . . ? C42 C41 C40 120.5(3) . . ? C43 C42 C41 120.5(5) . . ? C44 C43 C42 120.8(5) . . ? C45 C44 C43 119.8(5) . . ? C44 C45 C46 120.3(6) . . ? C41 C46 C45 120.2(5) . . ? O3 C47 O2 122.8(3) . . ? O3 C47 C48 121.3(3) . . ? O2 C47 C48 115.8(3) . . ? C47 C48 C49 114.5(4) . . ? C50A C49 C48 117.0(5) . . ? C49 C50A C51A 106.8(6) . . ? C52A C51A C50A 107.3(6) . . ? C53A C52A C51A 105.3(6) . . ? C54 C53A C52A 121.6(7) . . ? C55 C54 C53A 114.3(5) . . ? C54 C55 C56 117.2(4) . . ? O4 C56 O5 124.7(4) . . ? O4 C56 C55 119.8(4) . . ? O5 C56 C55 115.6(4) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.649 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 854269'