#Supplementary Material (ESI) for Journal of Materials Chemistry #This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'D Sherrington' _publ_contact_author_name 'D Sherrington' _publ_contact_author_email D.SHERRINGTON@STRATH.AC.UK _publ_section_title ; Synthesis of main chain chiral (meth)acrylates via chirality transfer from polymerizable chiral metal complexes ; # Attachment '6xsherrstruct.cif' data_sherr2 _database_code_depnum_ccdc_archive 'CCDC 715351' #------------------------------------------- #------- COMPOUND CMS --------------------- #-------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H36 Cu N2 O4' _chemical_formula_weight 468.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.0626(2) _cell_length_b 12.0807(3) _cell_length_c 16.4661(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2200.59(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5236 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'plate - fragment of large crystal' _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 1.024 _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 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10090 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0679 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5070 _reflns_number_gt 3972 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect & Denzo' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution Shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Unmodeled disorder in =CH2 and -CH3 positions 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^)+(0.0357P)^2^+0.0538P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(11) _refine_ls_number_reflns 5070 _refine_ls_number_parameters 288 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0684 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.69406(3) 0.97634(3) 0.843438(18) 0.01720(9) Uani 1 1 d . . . O1 O 0.79514(18) 0.87956(15) 0.91121(10) 0.0231(4) Uani 1 1 d . . . O2 O 0.64118(18) 0.76856(17) 0.88190(12) 0.0289(5) Uani 1 1 d . . . O3 O 0.61273(15) 1.02898(17) 0.94293(10) 0.0225(4) Uani 1 1 d . . . O4 O 0.7235(2) 1.17108(17) 0.90286(12) 0.0321(5) Uani 1 1 d . . . N1 N 0.8008(2) 0.95507(16) 0.74256(12) 0.0178(5) Uani 1 1 d . . . N2 N 0.55312(18) 1.01869(19) 0.76599(12) 0.0172(5) Uani 1 1 d . . . C1 C 0.9267(2) 0.9239(2) 0.76571(16) 0.0205(6) Uani 1 1 d . . . H1A H 0.9737 0.9067 0.7161 0.025 Uiso 1 1 calc R . . H1B H 0.9248 0.8566 0.8000 0.025 Uiso 1 1 calc R . . C2 C 0.9884(2) 1.0173(2) 0.81200(16) 0.0236(6) Uani 1 1 d . . . H2A H 0.9425 1.0334 0.8622 0.028 Uiso 1 1 calc R . . H2B H 1.0710 0.9940 0.8278 0.028 Uiso 1 1 calc R . . C3 C 0.9956(3) 1.1211(2) 0.76007(18) 0.0254(7) Uani 1 1 d . . . H3A H 1.0502 1.1082 0.7134 0.030 Uiso 1 1 calc R . . H3B H 1.0288 1.1830 0.7926 0.030 Uiso 1 1 calc R . . C4 C 0.8689(3) 1.1512(2) 0.72931(18) 0.0237(7) Uani 1 1 d . . . H4A H 0.8183 1.1751 0.7757 0.028 Uiso 1 1 calc R . . H4B H 0.8750 1.2141 0.6910 0.028 Uiso 1 1 calc R . . C5 C 0.8085(3) 1.0543(2) 0.68709(15) 0.0202(6) Uani 1 1 d . . . H5 H 0.8623 1.0328 0.6409 0.024 Uiso 1 1 calc R . . C6 C 0.6851(2) 1.0810(2) 0.65057(16) 0.0211(6) Uani 1 1 d . . . H6 H 0.6958 1.1452 0.6130 0.025 Uiso 1 1 calc R . . C7 C 0.6423(2) 0.9829(2) 0.59979(15) 0.0239(6) Uani 1 1 d . . . H7A H 0.7032 0.9638 0.5581 0.029 Uiso 1 1 calc R . . H7B H 0.5651 1.0006 0.5723 0.029 Uiso 1 1 calc R . . C8 C 0.6252(2) 0.8866(2) 0.65912(18) 0.0230(6) Uani 1 1 d . . . H8 H 0.5998 0.8204 0.6270 0.028 Uiso 1 1 calc R . . C9 C 0.7473(2) 0.8604(2) 0.69820(17) 0.0217(6) Uani 1 1 d . . . H9A H 0.7370 0.7978 0.7364 0.026 Uiso 1 1 calc R . . H9B H 0.8044 0.8365 0.6553 0.026 Uiso 1 1 calc R . . C10 C 0.5868(2) 1.1118(2) 0.71133(16) 0.0200(6) Uani 1 1 d . . . H10A H 0.6153 1.1748 0.7447 0.024 Uiso 1 1 calc R . . H10B H 0.5141 1.1364 0.6813 0.024 Uiso 1 1 calc R . . C11 C 0.5240(2) 0.9122(2) 0.72085(16) 0.0189(6) Uani 1 1 d . . . H11 H 0.5237 0.8510 0.7617 0.023 Uiso 1 1 calc R . . C12 C 0.4002(2) 0.9122(2) 0.67926(16) 0.0229(7) Uani 1 1 d . . . H12A H 0.4018 0.9649 0.6333 0.027 Uiso 1 1 calc R . . H12B H 0.3842 0.8375 0.6569 0.027 Uiso 1 1 calc R . . C13 C 0.2987(3) 0.9435(2) 0.73621(17) 0.0271(7) Uani 1 1 d . . . H13A H 0.2920 0.8881 0.7803 0.033 Uiso 1 1 calc R . . H13B H 0.2211 0.9453 0.7063 0.033 Uiso 1 1 calc R . . C14 C 0.3251(2) 1.0566(2) 0.77175(17) 0.0247(7) Uani 1 1 d . . . H14A H 0.2598 1.0782 0.8096 0.030 Uiso 1 1 calc R . . H14B H 0.3293 1.1124 0.7278 0.030 Uiso 1 1 calc R . . C15 C 0.4457(2) 1.0515(2) 0.81689(15) 0.0203(6) Uani 1 1 d . . . H15A H 0.4619 1.1251 0.8409 0.024 Uiso 1 1 calc R . . H15B H 0.4379 0.9981 0.8622 0.024 Uiso 1 1 calc R . . C16 C 0.7387(3) 0.7874(2) 0.91705(17) 0.0211(7) Uani 1 1 d . . . C17 C 0.7967(3) 0.6994(2) 0.96838(16) 0.0280(7) Uani 1 1 d . . . C18 C 0.9227(3) 0.7042(3) 0.9826(3) 0.0407(10) Uani 1 1 d . . . C19 C 0.7229(3) 0.6136(3) 0.9998(2) 0.0449(9) Uani 1 1 d . . . H19A H 0.6979 0.5645 0.9556 0.067 Uiso 1 1 calc R . . H19B H 0.6512 0.6459 1.0255 0.067 Uiso 1 1 calc R . . H19C H 0.7686 0.5712 1.0402 0.067 Uiso 1 1 calc R . . C20 C 0.6451(3) 1.1306(3) 0.94764(17) 0.0230(7) Uani 1 1 d . . . C21 C 0.5810(3) 1.2030(2) 1.00791(17) 0.0281(7) Uani 1 1 d . . . C22 C 0.6371(4) 1.3102(3) 1.0265(2) 0.0527(11) Uani 1 1 d . . . H22A H 0.5809 1.3552 1.0585 0.079 Uiso 1 1 calc R . . H22B H 0.6565 1.3487 0.9758 0.079 Uiso 1 1 calc R . . H22C H 0.7114 1.2982 1.0577 0.079 Uiso 1 1 calc R . . C23 C 0.4740(4) 1.1687(4) 1.0382(2) 0.0492(11) Uani 1 1 d . . . H23A H 0.438(3) 1.101(3) 1.0275(19) 0.039(11) Uiso 1 1 d . . . H23B H 0.443(3) 1.215(3) 1.072(2) 0.062(12) Uiso 1 1 d . . . H18B H 0.948(3) 0.653(2) 1.010(2) 0.036(10) Uiso 1 1 d . . . H18A H 0.960(3) 0.743(3) 0.951(2) 0.040(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01775(15) 0.01595(15) 0.01791(15) -0.00028(15) 0.00029(15) 0.00016(15) O1 0.0219(10) 0.0234(10) 0.0239(10) 0.0057(8) -0.0030(9) 0.0018(10) O2 0.0283(12) 0.0319(13) 0.0266(11) 0.0031(10) -0.0027(10) -0.0023(10) O3 0.0239(10) 0.0231(10) 0.0206(10) -0.0034(10) -0.0007(8) 0.0020(10) O4 0.0419(14) 0.0282(12) 0.0262(12) -0.0013(10) 0.0018(11) 0.0002(11) N1 0.0160(11) 0.0162(12) 0.0212(11) 0.0006(9) 0.0006(10) -0.0011(11) N2 0.0157(11) 0.0163(11) 0.0195(11) -0.0014(11) 0.0014(9) 0.0005(11) C1 0.0187(15) 0.0201(15) 0.0228(15) 0.0014(13) 0.0032(13) 0.0055(13) C2 0.0156(13) 0.0250(14) 0.0302(14) 0.0019(14) 0.0023(11) -0.0012(14) C3 0.0226(16) 0.0222(16) 0.0315(17) 0.0013(14) 0.0022(13) -0.0034(13) C4 0.0236(16) 0.0173(15) 0.0301(17) 0.0051(13) 0.0028(13) -0.0013(13) C5 0.0186(13) 0.0208(14) 0.0211(13) 0.0034(11) 0.0052(13) -0.0019(13) C6 0.0205(13) 0.0213(13) 0.0214(13) 0.0072(13) -0.0017(15) 0.0025(13) C7 0.0222(13) 0.0324(16) 0.0170(14) 0.0010(14) -0.0015(11) 0.0022(14) C8 0.0250(15) 0.0234(15) 0.0206(14) -0.0069(15) -0.0008(14) -0.0010(12) C9 0.0234(15) 0.0188(15) 0.0229(15) -0.0076(13) 0.0012(13) 0.0024(12) C10 0.0196(15) 0.0159(14) 0.0245(16) 0.0022(13) 0.0005(13) 0.0000(12) C11 0.0223(16) 0.0142(15) 0.0203(14) -0.0028(12) -0.0031(12) -0.0014(12) C12 0.0222(15) 0.0222(15) 0.0243(16) -0.0012(13) -0.0040(12) -0.0021(13) C13 0.0192(15) 0.0304(16) 0.0317(15) 0.0032(13) -0.0029(14) -0.0032(14) C14 0.0177(16) 0.0292(16) 0.0271(15) 0.0014(13) 0.0033(12) 0.0043(13) C15 0.0173(14) 0.0218(16) 0.0218(14) -0.0013(11) 0.0041(11) -0.0011(11) C16 0.0240(16) 0.0236(17) 0.0157(15) -0.0005(13) 0.0025(13) 0.0056(13) C17 0.0412(19) 0.0232(15) 0.0194(15) -0.0018(12) -0.0010(15) 0.0058(16) C18 0.030(2) 0.042(2) 0.050(2) 0.024(2) -0.0084(19) 0.0050(18) C19 0.060(2) 0.0310(19) 0.043(2) 0.0097(16) -0.0140(18) -0.0063(18) C20 0.0259(16) 0.0262(18) 0.0169(15) -0.0014(13) -0.0069(13) 0.0077(14) C21 0.0386(19) 0.0289(18) 0.0167(15) 0.0008(14) -0.0047(14) 0.0103(15) C22 0.109(3) 0.0259(19) 0.0236(18) -0.0031(16) 0.001(2) 0.018(2) C23 0.046(3) 0.064(3) 0.037(2) -0.026(2) -0.0059(19) 0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.9654(18) . ? Cu1 O3 1.9743(17) . ? Cu1 N1 2.054(2) . ? Cu1 N2 2.078(2) . ? O1 C16 1.280(3) . ? O2 C16 1.245(3) . ? O3 C20 1.281(3) . ? O4 C20 1.239(3) . ? N1 C9 1.480(3) . ? N1 C1 1.493(3) . ? N1 C5 1.509(3) . ? N2 C10 1.488(3) . ? N2 C15 1.507(3) . ? N2 C11 1.520(3) . ? C1 C2 1.523(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.520(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.534(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.517(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.526(4) . ? C5 H5 1.0000 . ? C6 C10 1.524(4) . ? C6 C7 1.526(4) . ? C6 H6 1.0000 . ? C7 C8 1.530(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.530(4) . ? C8 C11 1.543(4) . ? C8 H8 1.0000 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.531(4) . ? C11 H11 1.0000 . ? C12 C13 1.512(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.514(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.528(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.502(4) . ? C17 C18 1.414(5) . ? C17 C19 1.417(4) . ? C18 H18B 0.81(3) . ? C18 H18A 0.81(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.501(4) . ? C21 C23 1.350(5) . ? C21 C22 1.468(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.92(3) . ? C23 H23B 0.86(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O3 88.84(8) . . ? O1 Cu1 N1 93.31(8) . . ? O3 Cu1 N1 166.73(8) . . ? O1 Cu1 N2 157.18(8) . . ? O3 Cu1 N2 95.05(8) . . ? N1 Cu1 N2 88.03(8) . . ? C16 O1 Cu1 106.40(17) . . ? C20 O3 Cu1 103.38(17) . . ? C9 N1 C1 107.68(19) . . ? C9 N1 C5 109.74(19) . . ? C1 N1 C5 107.6(2) . . ? C9 N1 Cu1 105.44(16) . . ? C1 N1 Cu1 111.19(15) . . ? C5 N1 Cu1 114.99(15) . . ? C10 N2 C15 109.6(2) . . ? C10 N2 C11 113.41(19) . . ? C15 N2 C11 109.10(19) . . ? C10 N2 Cu1 111.67(16) . . ? C15 N2 Cu1 108.36(14) . . ? C11 N2 Cu1 104.51(15) . . ? N1 C1 C2 111.1(2) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C3 C2 C1 110.7(2) . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 109.5(2) . . ? C2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? C2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C3 111.7(2) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? N1 C5 C4 111.1(2) . . ? N1 C5 C6 110.8(2) . . ? C4 C5 C6 114.3(2) . . ? N1 C5 H5 106.7 . . ? C4 C5 H5 106.7 . . ? C6 C5 H5 106.7 . . ? C10 C6 C7 109.2(2) . . ? C10 C6 C5 115.5(2) . . ? C7 C6 C5 109.2(2) . . ? C10 C6 H6 107.5 . . ? C7 C6 H6 107.5 . . ? C5 C6 H6 107.5 . . ? C6 C7 C8 106.2(2) . . ? C6 C7 H7A 110.5 . . ? C8 C7 H7A 110.5 . . ? C6 C7 H7B 110.5 . . ? C8 C7 H7B 110.5 . . ? H7A C7 H7B 108.7 . . ? C9 C8 C7 108.5(2) . . ? C9 C8 C11 113.9(2) . . ? C7 C8 C11 111.0(2) . . ? C9 C8 H8 107.8 . . ? C7 C8 H8 107.8 . . ? C11 C8 H8 107.8 . . ? N1 C9 C8 113.6(2) . . ? N1 C9 H9A 108.8 . . ? C8 C9 H9A 108.8 . . ? N1 C9 H9B 108.8 . . ? C8 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? N2 C10 C6 113.0(2) . . ? N2 C10 H10A 109.0 . . ? C6 C10 H10A 109.0 . . ? N2 C10 H10B 109.0 . . ? C6 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? N2 C11 C12 114.1(2) . . ? N2 C11 C8 109.7(2) . . ? C12 C11 C8 110.7(2) . . ? N2 C11 H11 107.3 . . ? C12 C11 H11 107.3 . . ? C8 C11 H11 107.3 . . ? C13 C12 C11 112.8(2) . . ? C13 C12 H12A 109.0 . . ? C11 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? C11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C12 C13 C14 108.8(2) . . ? C12 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? C12 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C13 C14 C15 108.7(2) . . ? C13 C14 H14A 109.9 . . ? C15 C14 H14A 109.9 . . ? C13 C14 H14B 109.9 . . ? C15 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? N2 C15 C14 115.4(2) . . ? N2 C15 H15A 108.4 . . ? C14 C15 H15A 108.4 . . ? N2 C15 H15B 108.4 . . ? C14 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? O2 C16 O1 123.1(3) . . ? O2 C16 C17 120.2(3) . . ? O1 C16 C17 116.7(3) . . ? C18 C17 C19 122.5(3) . . ? C18 C17 C16 119.0(3) . . ? C19 C17 C16 118.5(3) . . ? C17 C18 H18B 114(2) . . ? C17 C18 H18A 115(2) . . ? H18B C18 H18A 128(3) . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O4 C20 O3 122.6(3) . . ? O4 C20 C21 119.6(3) . . ? O3 C20 C21 117.8(3) . . ? C23 C21 C22 124.4(3) . . ? C23 C21 C20 118.6(3) . . ? C22 C21 C20 116.9(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 126(2) . . ? C21 C23 H23B 113(2) . . ? H23A C23 H23B 122(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cu1 O1 C16 90.07(17) . . . . ? N1 Cu1 O1 C16 -103.04(17) . . . . ? N2 Cu1 O1 C16 -10.2(3) . . . . ? O1 Cu1 O3 C20 113.08(17) . . . . ? N1 Cu1 O3 C20 13.5(4) . . . . ? N2 Cu1 O3 C20 -89.45(17) . . . . ? O1 Cu1 N1 C9 91.92(16) . . . . ? O3 Cu1 N1 C9 -169.1(3) . . . . ? N2 Cu1 N1 C9 -65.27(16) . . . . ? O1 Cu1 N1 C1 -24.49(16) . . . . ? O3 Cu1 N1 C1 74.5(4) . . . . ? N2 Cu1 N1 C1 178.31(16) . . . . ? O1 Cu1 N1 C5 -147.06(18) . . . . ? O3 Cu1 N1 C5 -48.0(5) . . . . ? N2 Cu1 N1 C5 55.75(18) . . . . ? O1 Cu1 N2 C10 -149.4(2) . . . . ? O3 Cu1 N2 C10 111.54(16) . . . . ? N1 Cu1 N2 C10 -55.53(17) . . . . ? O1 Cu1 N2 C15 89.8(3) . . . . ? O3 Cu1 N2 C15 -9.24(17) . . . . ? N1 Cu1 N2 C15 -176.30(16) . . . . ? O1 Cu1 N2 C11 -26.4(3) . . . . ? O3 Cu1 N2 C11 -125.47(15) . . . . ? N1 Cu1 N2 C11 67.46(15) . . . . ? C9 N1 C1 C2 -179.9(2) . . . . ? C5 N1 C1 C2 61.9(2) . . . . ? Cu1 N1 C1 C2 -64.9(2) . . . . ? N1 C1 C2 C3 -60.5(3) . . . . ? C1 C2 C3 C4 54.1(3) . . . . ? C2 C3 C4 C5 -53.1(3) . . . . ? C9 N1 C5 C4 -177.1(2) . . . . ? C1 N1 C5 C4 -60.2(3) . . . . ? Cu1 N1 C5 C4 64.3(3) . . . . ? C9 N1 C5 C6 54.7(3) . . . . ? C1 N1 C5 C6 171.6(2) . . . . ? Cu1 N1 C5 C6 -63.9(2) . . . . ? C3 C4 C5 N1 57.1(3) . . . . ? C3 C4 C5 C6 -176.5(2) . . . . ? N1 C5 C6 C10 62.0(3) . . . . ? C4 C5 C6 C10 -64.6(3) . . . . ? N1 C5 C6 C7 -61.6(3) . . . . ? C4 C5 C6 C7 171.9(2) . . . . ? C10 C6 C7 C8 -62.9(3) . . . . ? C5 C6 C7 C8 64.3(3) . . . . ? C6 C7 C8 C9 -61.7(3) . . . . ? C6 C7 C8 C11 64.1(3) . . . . ? C1 N1 C9 C8 -171.1(2) . . . . ? C5 N1 C9 C8 -54.2(3) . . . . ? Cu1 N1 C9 C8 70.2(2) . . . . ? C7 C8 C9 N1 58.9(3) . . . . ? C11 C8 C9 N1 -65.1(3) . . . . ? C15 N2 C10 C6 -173.1(2) . . . . ? C11 N2 C10 C6 -50.9(3) . . . . ? Cu1 N2 C10 C6 66.8(2) . . . . ? C7 C6 C10 N2 57.9(3) . . . . ? C5 C6 C10 N2 -65.7(3) . . . . ? C10 N2 C11 C12 -75.6(3) . . . . ? C15 N2 C11 C12 46.8(3) . . . . ? Cu1 N2 C11 C12 162.55(18) . . . . ? C10 N2 C11 C8 49.3(3) . . . . ? C15 N2 C11 C8 171.8(2) . . . . ? Cu1 N2 C11 C8 -72.5(2) . . . . ? C9 C8 C11 N2 65.7(3) . . . . ? C7 C8 C11 N2 -57.0(3) . . . . ? C9 C8 C11 C12 -167.5(2) . . . . ? C7 C8 C11 C12 69.8(3) . . . . ? N2 C11 C12 C13 -52.2(3) . . . . ? C8 C11 C12 C13 -176.6(2) . . . . ? C11 C12 C13 C14 57.3(3) . . . . ? C12 C13 C14 C15 -59.1(3) . . . . ? C10 N2 C15 C14 73.0(3) . . . . ? C11 N2 C15 C14 -51.7(3) . . . . ? Cu1 N2 C15 C14 -164.95(18) . . . . ? C13 C14 C15 N2 59.3(3) . . . . ? Cu1 O1 C16 O2 2.5(3) . . . . ? Cu1 O1 C16 C17 -178.43(18) . . . . ? O2 C16 C17 C18 156.7(3) . . . . ? O1 C16 C17 C18 -22.4(4) . . . . ? O2 C16 C17 C19 -22.5(4) . . . . ? O1 C16 C17 C19 158.4(3) . . . . ? Cu1 O3 C20 O4 -8.9(3) . . . . ? Cu1 O3 C20 C21 168.6(2) . . . . ? O4 C20 C21 C23 160.2(3) . . . . ? O3 C20 C21 C23 -17.4(4) . . . . ? O4 C20 C21 C22 -16.6(4) . . . . ? O3 C20 C21 C22 165.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.349 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.067 #===END #--------------------------------------------- #--------COMPOUND CMN ----------------------- #---------------------------------------------- data_gsherr3 _database_code_depnum_ccdc_archive 'CCDC 715352' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 Cu2 N4 O8' _chemical_formula_weight 791.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.5553(2) _cell_length_b 9.6147(2) _cell_length_c 11.1816(3) _cell_angle_alpha 104.235(1) _cell_angle_beta 107.076(1) _cell_angle_gamma 96.800(1) _cell_volume 931.47(4) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4070 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.10 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 414 _exptl_absorpt_coefficient_mu 1.196 _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 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27636 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.02 _reflns_number_total 8130 _reflns_number_gt 6865 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; H atoms on O2CC(Me)(=CH2) ligands placed w.r.t. bond length and observed e density. However, C-C lengths suggest disorder/scrambling of CH3 with CH2. This was not modeled. 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^)+(0.0237P)^2^+0.5141P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(11) _refine_ls_number_reflns 8130 _refine_ls_number_parameters 458 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.027 _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 Cu1 Cu 0.37547(3) 0.86231(3) 0.86287(3) 0.02656(14) Uani 1 1 d . . . Cu2 Cu 0.29338(3) 0.92449(3) 0.63956(3) 0.02648(14) Uani 1 1 d . . . O1 O 0.5745(4) 0.9570(4) 0.8767(4) 0.0344(9) Uani 1 1 d . . . O2 O 0.5082(4) 1.0011(4) 0.6819(4) 0.0353(9) Uani 1 1 d . . . O3 O 0.3967(4) 0.6799(4) 0.7444(3) 0.0330(8) Uani 1 1 d . . . O4 O 0.3222(4) 0.7305(4) 0.5526(3) 0.0326(8) Uani 1 1 d . . . O5 O 0.1640(4) 0.7767(4) 0.8222(4) 0.0345(9) Uani 1 1 d . . . O6 O 0.0919(4) 0.8342(4) 0.6337(3) 0.0320(8) Uani 1 1 d . . . O7 O 0.3359(4) 1.0556(4) 0.9432(3) 0.0322(8) Uani 1 1 d . . . O8 O 0.2756(4) 1.1098(4) 0.7533(3) 0.0327(8) Uani 1 1 d . . . N1 N 0.4579(4) 0.7852(4) 1.0327(4) 0.0269(10) Uani 1 1 d . . . N2 N 0.7732(3) 0.5088(3) 1.0374(3) 0.0347(6) Uani 1 1 d . . . N3 N 0.2024(4) 1.0043(4) 0.4738(4) 0.0251(9) Uani 1 1 d . . . N4 N -0.1447(3) 1.3144(3) 0.3675(3) 0.0329(6) Uani 1 1 d . . . C1 C 0.3875(5) 0.7893(5) 1.1208(5) 0.0263(10) Uani 1 1 d . . . H1 H 0.3015 0.8317 1.1111 0.032 Uiso 1 1 calc R . . C2 C 0.4360(5) 0.7343(5) 1.2243(4) 0.0326(10) Uani 1 1 d . . . H2 H 0.3849 0.7390 1.2859 0.039 Uiso 1 1 calc R . . C3 C 0.5603(5) 0.6719(5) 1.2375(5) 0.0324(10) Uani 1 1 d . . . H3 H 0.5956 0.6338 1.3090 0.039 Uiso 1 1 calc R . . C4 C 0.6337(4) 0.6644(4) 1.1475(4) 0.0283(10) Uani 1 1 d . . . C5 C 0.5783(5) 0.7229(5) 1.0444(5) 0.0293(11) Uani 1 1 d . . . H5 H 0.6269 0.7185 0.9811 0.035 Uiso 1 1 calc R . . C6 C 0.7705(4) 0.5975(4) 1.1608(4) 0.0339(8) Uani 1 1 d . . . H6 H 0.7734 0.5351 1.2208 0.041 Uiso 1 1 calc R . . C7 C 0.9188(6) 0.7097(6) 1.2130(7) 0.0553(16) Uani 1 1 d . . . H7A H 0.9068 0.7957 1.1801 0.066 Uiso 1 1 calc R . . H7B H 0.9563 0.7435 1.3099 0.066 Uiso 1 1 calc R . . C8 C 1.0247(5) 0.6255(5) 1.1601(5) 0.0587(13) Uani 1 1 d . . . H8A H 1.1049 0.6105 1.2324 0.070 Uiso 1 1 calc R . . H8B H 1.0709 0.6789 1.1115 0.070 Uiso 1 1 calc R . . C9 C 0.9250(4) 0.4785(4) 1.0689(4) 0.0460(10) Uani 1 1 d . . . H9A H 0.9518 0.4473 0.9887 0.055 Uiso 1 1 calc R . . H9B H 0.9337 0.4012 1.1134 0.055 Uiso 1 1 calc R . . C10 C 0.6590(5) 0.3772(5) 0.9807(4) 0.0454(11) Uani 1 1 d . . . H10A H 0.6713 0.3178 1.0413 0.068 Uiso 1 1 calc R . . H10B H 0.6674 0.3211 0.8980 0.068 Uiso 1 1 calc R . . H10C H 0.5603 0.4030 0.9640 0.068 Uiso 1 1 calc R . . C11 C 0.2555(5) 1.0110(5) 0.3779(5) 0.0320(11) Uani 1 1 d . . . H11 H 0.3428 0.9735 0.3765 0.038 Uiso 1 1 calc R . . C12 C 0.1887(5) 1.0709(5) 0.2790(4) 0.0332(11) Uani 1 1 d . . . H12 H 0.2292 1.0730 0.2112 0.040 Uiso 1 1 calc R . . C13 C 0.0631(5) 1.1267(5) 0.2814(4) 0.0332(10) Uani 1 1 d . . . H13 H 0.0163 1.1685 0.2153 0.040 Uiso 1 1 calc R . . C14 C 0.0053(5) 1.1216(5) 0.3805(4) 0.0287(10) Uani 1 1 d . . . C15 C 0.0801(5) 1.0589(5) 0.4730(5) 0.0282(11) Uani 1 1 d . . . H15 H 0.0413 1.0543 0.5413 0.034 Uiso 1 1 calc R . . C16 C -0.1356(4) 1.1730(4) 0.3902(4) 0.0288(8) Uani 1 1 d . . . H16 H -0.1408 1.1791 0.4793 0.035 Uiso 1 1 calc R . . C17 C -0.2800(5) 1.0740(6) 0.2870(6) 0.0505(14) Uani 1 1 d . . . H17A H -0.3127 0.9887 0.3142 0.061 Uiso 1 1 calc R . . H17B H -0.2665 1.0383 0.2010 0.061 Uiso 1 1 calc R . . C18 C -0.3930(5) 1.1759(5) 0.2813(5) 0.0543(12) Uani 1 1 d . . . H18A H -0.4455 1.1727 0.1897 0.065 Uiso 1 1 calc R . . H18B H -0.4679 1.1477 0.3208 0.065 Uiso 1 1 calc R . . C19 C -0.2976(4) 1.3274(4) 0.3601(4) 0.0389(8) Uani 1 1 d . . . H19A H -0.3295 1.4014 0.3157 0.047 Uiso 1 1 calc R . . H19B H -0.3056 1.3564 0.4488 0.047 Uiso 1 1 calc R . . C20 C -0.0312(5) 1.4335(5) 0.4683(5) 0.0526(12) Uani 1 1 d . . . H20A H -0.0366 1.4333 0.5545 0.079 Uiso 1 1 calc R . . H20B H -0.0485 1.5272 0.4532 0.079 Uiso 1 1 calc R . . H20C H 0.0680 1.4204 0.4653 0.079 Uiso 1 1 calc R . . C21 C 0.6031(5) 1.0023(5) 0.7881(5) 0.0310(12) Uani 1 1 d . . . C22 C 0.7659(6) 1.0621(6) 0.8096(6) 0.0374(13) Uani 1 1 d . . . C23 C 0.8712(6) 1.0514(7) 0.9166(6) 0.0494(16) Uani 1 1 d . . . H23A H 0.9739 1.0884 0.9333 0.059 Uiso 1 1 calc R . . H23B H 0.8423 1.0069 0.9751 0.059 Uiso 1 1 calc R . . C24 C 0.7952(6) 1.1267(6) 0.7142(6) 0.0508(16) Uani 1 1 d . . . H24A H 0.9012 1.1740 0.7447 0.076 Uiso 1 1 calc R . . H24B H 0.7335 1.2000 0.7021 0.076 Uiso 1 1 calc R . . H24C H 0.7710 1.0503 0.6307 0.076 Uiso 1 1 calc R . . C25 C 0.3689(5) 0.6492(5) 0.6226(5) 0.0272(11) Uani 1 1 d . . . C26 C 0.3972(5) 0.5048(5) 0.5553(5) 0.0276(11) Uani 1 1 d . . . C27 C 0.4482(6) 0.4092(6) 0.6300(5) 0.0382(13) Uani 1 1 d . . . H27A H 0.3690 0.3725 0.6605 0.057 Uiso 1 1 calc R . . H27B H 0.5369 0.4628 0.7057 0.057 Uiso 1 1 calc R . . H27C H 0.4738 0.3265 0.5754 0.057 Uiso 1 1 calc R . . C28 C 0.3688(6) 0.4697(5) 0.4199(5) 0.0327(12) Uani 1 1 d . . . H28A H 0.3834 0.3786 0.3739 0.039 Uiso 1 1 calc R . . H28B H 0.3349 0.5372 0.3741 0.039 Uiso 1 1 calc R . . C29 C 0.0661(5) 0.7826(5) 0.7202(5) 0.0274(11) Uani 1 1 d . . . C30 C -0.0934(5) 0.7248(6) 0.7017(5) 0.0353(12) Uani 1 1 d . . . C31 C -0.1251(7) 0.6560(7) 0.7961(6) 0.0576(18) Uani 1 1 d . . . H31A H -0.2304 0.6510 0.7890 0.086 Uiso 1 1 calc R . . H31B H -0.0613 0.7141 0.8849 0.086 Uiso 1 1 calc R . . H31C H -0.1050 0.5567 0.7780 0.086 Uiso 1 1 calc R . . C32 C -0.2056(6) 0.7400(6) 0.5985(6) 0.0436(14) Uani 1 1 d . . . H32A H -0.3073 0.7051 0.5872 0.052 Uiso 1 1 calc R . . H32B H -0.1813 0.7853 0.5386 0.052 Uiso 1 1 calc R . . C33 C 0.2934(5) 1.1379(5) 0.8733(5) 0.0251(11) Uani 1 1 d . . . C34 C 0.2633(5) 1.2841(5) 0.9382(5) 0.0283(11) Uani 1 1 d . . . C35 C 0.2822(6) 1.3210(6) 1.0731(5) 0.0370(13) Uani 1 1 d . . . H35A H 0.2515 1.4143 1.0996 0.056 Uiso 1 1 calc R . . H35B H 0.3876 1.3305 1.1236 0.056 Uiso 1 1 calc R . . H35C H 0.2205 1.2439 1.0897 0.056 Uiso 1 1 calc R . . C36 C 0.2166(6) 1.3762(6) 0.8605(5) 0.0357(12) Uani 1 1 d . . . H36A H 0.1961 1.4679 0.8985 0.043 Uiso 1 1 calc R . . H36B H 0.2055 1.3465 0.7701 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0250(3) 0.0248(3) 0.0287(3) 0.0071(3) 0.0076(3) 0.0061(2) Cu2 0.0273(3) 0.0241(3) 0.0281(3) 0.0068(3) 0.0091(3) 0.0077(2) O1 0.0272(19) 0.034(2) 0.041(2) 0.0126(17) 0.0105(18) 0.0031(16) O2 0.031(2) 0.035(2) 0.041(2) 0.0085(18) 0.0168(18) 0.0028(17) O3 0.041(2) 0.031(2) 0.027(2) 0.0073(16) 0.0116(17) 0.0122(17) O4 0.0362(19) 0.029(2) 0.0314(19) 0.0062(16) 0.0088(15) 0.0140(16) O5 0.0250(19) 0.042(2) 0.037(2) 0.0154(18) 0.0074(17) 0.0049(17) O6 0.0218(17) 0.035(2) 0.041(2) 0.0139(17) 0.0100(17) 0.0079(16) O7 0.041(2) 0.029(2) 0.0262(18) 0.0041(15) 0.0116(15) 0.0112(16) O8 0.044(2) 0.0225(19) 0.030(2) 0.0031(16) 0.0125(17) 0.0093(16) N1 0.022(2) 0.021(2) 0.036(2) 0.0086(19) 0.0058(19) 0.0068(17) N2 0.0296(15) 0.0372(17) 0.0424(17) 0.0139(14) 0.0159(13) 0.0118(13) N3 0.024(2) 0.025(2) 0.027(2) 0.0066(18) 0.0104(18) 0.0065(18) N4 0.0283(15) 0.0267(14) 0.0469(17) 0.0121(13) 0.0161(13) 0.0055(11) C1 0.024(2) 0.025(2) 0.034(2) 0.0105(17) 0.0152(17) 0.0047(16) C2 0.040(2) 0.026(2) 0.036(2) 0.0102(16) 0.0181(19) 0.0069(17) C3 0.034(2) 0.029(2) 0.034(2) 0.0121(17) 0.0093(19) 0.0035(18) C4 0.023(2) 0.0211(18) 0.034(2) 0.0053(17) 0.0017(17) 0.0071(15) C5 0.027(2) 0.029(2) 0.032(2) 0.005(2) 0.0129(19) 0.0074(19) C6 0.030(2) 0.0280(18) 0.043(2) 0.0099(16) 0.0123(17) 0.0061(15) C7 0.035(3) 0.033(3) 0.085(4) 0.013(3) 0.006(3) 0.007(2) C8 0.026(2) 0.056(3) 0.092(4) 0.025(3) 0.015(2) 0.008(2) C9 0.034(2) 0.050(2) 0.071(3) 0.028(2) 0.029(2) 0.0226(18) C10 0.041(2) 0.036(2) 0.057(3) 0.007(2) 0.018(2) 0.0126(18) C11 0.028(2) 0.026(2) 0.041(3) 0.0025(18) 0.0141(19) 0.0109(18) C12 0.039(3) 0.035(2) 0.031(2) 0.0096(17) 0.021(2) 0.0051(19) C13 0.040(3) 0.0257(19) 0.035(2) 0.0134(17) 0.009(2) 0.0078(17) C14 0.028(2) 0.0232(18) 0.032(2) 0.0046(16) 0.0093(17) 0.0030(15) C15 0.029(2) 0.024(2) 0.027(2) 0.0055(19) 0.0055(19) 0.0051(19) C16 0.0256(18) 0.0295(18) 0.039(2) 0.0167(17) 0.0142(15) 0.0104(14) C17 0.030(2) 0.033(3) 0.080(4) 0.015(3) 0.010(2) 0.003(2) C18 0.028(2) 0.053(3) 0.079(3) 0.022(2) 0.011(2) 0.0111(19) C19 0.0281(19) 0.039(2) 0.060(2) 0.0275(19) 0.0168(18) 0.0139(16) C20 0.040(2) 0.032(2) 0.075(3) -0.007(2) 0.022(2) 0.0051(18) C21 0.030(3) 0.020(3) 0.039(3) 0.002(2) 0.010(3) 0.008(2) C22 0.031(3) 0.031(3) 0.046(3) -0.002(2) 0.020(3) 0.003(2) C23 0.019(2) 0.076(4) 0.044(3) 0.013(3) 0.005(2) -0.004(3) C24 0.034(3) 0.055(4) 0.059(4) 0.007(3) 0.025(3) -0.008(3) C25 0.016(2) 0.030(3) 0.030(3) 0.002(2) 0.007(2) -0.001(2) C26 0.024(2) 0.025(3) 0.035(3) 0.006(2) 0.013(2) 0.006(2) C27 0.043(3) 0.034(3) 0.037(3) 0.004(2) 0.018(2) 0.006(2) C28 0.044(3) 0.021(2) 0.028(2) -0.0039(19) 0.013(2) 0.008(2) C29 0.027(3) 0.020(3) 0.034(3) 0.001(2) 0.015(2) 0.005(2) C30 0.027(3) 0.034(3) 0.036(3) -0.004(2) 0.012(2) -0.001(2) C31 0.045(4) 0.076(5) 0.057(4) 0.025(4) 0.024(3) 0.005(3) C32 0.034(3) 0.045(3) 0.050(3) 0.002(3) 0.019(3) 0.010(2) C33 0.017(2) 0.024(3) 0.034(3) 0.008(2) 0.008(2) 0.0022(19) C34 0.018(2) 0.024(3) 0.036(3) 0.000(2) 0.009(2) -0.001(2) C35 0.034(3) 0.040(3) 0.040(3) 0.013(2) 0.016(2) 0.010(2) C36 0.044(3) 0.029(3) 0.040(3) 0.011(2) 0.016(2) 0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.954(3) . ? Cu1 O5 1.962(4) . ? Cu1 O7 1.987(3) . ? Cu1 O3 1.993(3) . ? Cu1 N1 2.174(4) . ? Cu1 Cu2 2.6273(4) . ? Cu2 O2 1.970(4) . ? Cu2 O4 1.971(3) . ? Cu2 O8 1.976(3) . ? Cu2 O6 1.992(3) . ? Cu2 N3 2.166(4) . ? O1 C21 1.261(6) . ? O2 C21 1.262(6) . ? O3 C25 1.258(6) . ? O4 C25 1.266(6) . ? O5 C29 1.263(6) . ? O6 C29 1.261(6) . ? O7 C33 1.263(5) . ? O8 C33 1.257(6) . ? N1 C1 1.342(6) . ? N1 C5 1.347(6) . ? N2 C10 1.437(5) . ? N2 C6 1.442(4) . ? N2 C9 1.471(4) . ? N3 C11 1.325(6) . ? N3 C15 1.335(6) . ? N4 C16 1.450(4) . ? N4 C20 1.453(5) . ? N4 C19 1.461(4) . ? C1 C2 1.371(6) . ? C1 H1 0.9500 . ? C2 C3 1.379(5) . ? C2 H2 0.9500 . ? C3 C4 1.379(6) . ? C3 H3 0.9500 . ? C4 C5 1.399(6) . ? C4 C6 1.509(5) . ? C5 H5 0.9500 . ? C6 C7 1.534(6) . ? C6 H6 1.0000 . ? C7 C8 1.530(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.532(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.396(6) . ? C11 H11 0.9500 . ? C12 C13 1.376(6) . ? C12 H12 0.9500 . ? C13 C14 1.384(6) . ? C13 H13 0.9500 . ? C14 C15 1.385(6) . ? C14 C16 1.512(5) . ? C15 H15 0.9500 . ? C16 C17 1.535(6) . ? C16 H16 1.0000 . ? C17 C18 1.540(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.520(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.519(7) . ? C22 C23 1.354(8) . ? C22 C24 1.436(8) . ? C23 H23A 0.9500 . ? C23 H23B 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.504(6) . ? C26 C28 1.402(7) . ? C26 C27 1.423(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9500 . ? C28 H28B 0.9500 . ? C29 C30 1.494(7) . ? C30 C32 1.376(8) . ? C30 C31 1.459(8) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9500 . ? C32 H32B 0.9500 . ? C33 C34 1.517(6) . ? C34 C36 1.408(7) . ? C34 C35 1.413(7) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9500 . ? C36 H36B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O5 170.44(15) . . ? O1 Cu1 O7 90.32(15) . . ? O5 Cu1 O7 88.44(15) . . ? O1 Cu1 O3 89.25(15) . . ? O5 Cu1 O3 89.82(16) . . ? O7 Cu1 O3 166.92(13) . . ? O1 Cu1 N1 93.97(14) . . ? O5 Cu1 N1 95.56(14) . . ? O7 Cu1 N1 101.71(14) . . ? O3 Cu1 N1 91.36(13) . . ? O1 Cu1 Cu2 83.49(10) . . ? O5 Cu1 Cu2 86.98(10) . . ? O7 Cu1 Cu2 86.68(10) . . ? O3 Cu1 Cu2 80.28(9) . . ? N1 Cu1 Cu2 171.28(11) . . ? O2 Cu2 O4 88.51(15) . . ? O2 Cu2 O8 90.50(15) . . ? O4 Cu2 O8 170.64(14) . . ? O2 Cu2 O6 167.07(15) . . ? O4 Cu2 O6 90.37(14) . . ? O8 Cu2 O6 88.50(15) . . ? O2 Cu2 N3 99.73(15) . . ? O4 Cu2 N3 101.49(14) . . ? O8 Cu2 N3 87.86(14) . . ? O6 Cu2 N3 93.11(14) . . ? O2 Cu2 Cu1 85.23(11) . . ? O4 Cu2 Cu1 88.66(10) . . ? O8 Cu2 Cu1 81.98(9) . . ? O6 Cu2 Cu1 81.87(10) . . ? N3 Cu2 Cu1 168.75(10) . . ? C21 O1 Cu1 124.1(3) . . ? C21 O2 Cu2 121.3(3) . . ? C25 O3 Cu1 127.1(3) . . ? C25 O4 Cu2 118.2(3) . . ? C29 O5 Cu1 120.5(3) . . ? C29 O6 Cu2 125.1(3) . . ? C33 O7 Cu1 119.9(3) . . ? C33 O8 Cu2 126.0(3) . . ? C1 N1 C5 119.3(4) . . ? C1 N1 Cu1 122.3(3) . . ? C5 N1 Cu1 118.3(3) . . ? C10 N2 C6 113.3(3) . . ? C10 N2 C9 112.6(3) . . ? C6 N2 C9 103.8(3) . . ? C11 N3 C15 116.9(4) . . ? C11 N3 Cu2 128.6(3) . . ? C15 N3 Cu2 114.5(3) . . ? C16 N4 C20 112.8(3) . . ? C16 N4 C19 103.1(2) . . ? C20 N4 C19 113.7(3) . . ? N1 C1 C2 122.0(4) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C1 C2 C3 118.8(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 117.7(4) . . ? C3 C4 C6 121.2(4) . . ? C5 C4 C6 121.1(4) . . ? N1 C5 C4 121.7(4) . . ? N1 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? N2 C6 C4 113.0(3) . . ? N2 C6 C7 102.8(4) . . ? C4 C6 C7 114.3(3) . . ? N2 C6 H6 108.8 . . ? C4 C6 H6 108.8 . . ? C7 C6 H6 108.8 . . ? C8 C7 C6 104.0(4) . . ? C8 C7 H7A 111.0 . . ? C6 C7 H7A 111.0 . . ? C8 C7 H7B 111.0 . . ? C6 C7 H7B 111.0 . . ? H7A C7 H7B 109.0 . . ? C7 C8 C9 104.6(4) . . ? C7 C8 H8A 110.8 . . ? C9 C8 H8A 110.8 . . ? C7 C8 H8B 110.8 . . ? C9 C8 H8B 110.8 . . ? H8A C8 H8B 108.9 . . ? N2 C9 C8 103.8(3) . . ? N2 C9 H9A 111.0 . . ? C8 C9 H9A 111.0 . . ? N2 C9 H9B 111.0 . . ? C8 C9 H9B 111.0 . . ? H9A C9 H9B 109.0 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 122.9(4) . . ? N3 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C13 C12 C11 118.8(4) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 119.7(4) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C15 116.6(4) . . ? C13 C14 C16 124.5(4) . . ? C15 C14 C16 118.8(4) . . ? N3 C15 C14 125.2(5) . . ? N3 C15 H15 117.4 . . ? C14 C15 H15 117.4 . . ? N4 C16 C14 113.7(3) . . ? N4 C16 C17 102.3(3) . . ? C14 C16 C17 114.0(4) . . ? N4 C16 H16 108.8 . . ? C14 C16 H16 108.8 . . ? C17 C16 H16 108.8 . . ? C16 C17 C18 103.2(4) . . ? C16 C17 H17A 111.1 . . ? C18 C17 H17A 111.1 . . ? C16 C17 H17B 111.1 . . ? C18 C17 H17B 111.1 . . ? H17A C17 H17B 109.1 . . ? C19 C18 C17 104.2(3) . . ? C19 C18 H18A 110.9 . . ? C17 C18 H18A 110.9 . . ? C19 C18 H18B 110.9 . . ? C17 C18 H18B 110.9 . . ? H18A C18 H18B 108.9 . . ? N4 C19 C18 105.1(3) . . ? N4 C19 H19A 110.7 . . ? C18 C19 H19A 110.7 . . ? N4 C19 H19B 110.7 . . ? C18 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O1 C21 O2 125.7(5) . . ? O1 C21 C22 117.6(5) . . ? O2 C21 C22 116.8(5) . . ? C23 C22 C24 125.2(5) . . ? C23 C22 C21 117.9(5) . . ? C24 C22 C21 116.8(5) . . ? C22 C23 H23A 120.0 . . ? C22 C23 H23B 120.0 . . ? H23A C23 H23B 120.0 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 C25 O4 125.6(5) . . ? O3 C25 C26 117.0(4) . . ? O4 C25 C26 117.3(4) . . ? C28 C26 C27 123.0(5) . . ? C28 C26 C25 117.8(4) . . ? C27 C26 C25 119.2(5) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 120.0 . . ? C26 C28 H28B 120.0 . . ? H28A C28 H28B 120.0 . . ? O6 C29 O5 125.4(5) . . ? O6 C29 C30 117.5(4) . . ? O5 C29 C30 117.1(4) . . ? C32 C30 C31 122.0(5) . . ? C32 C30 C29 119.6(5) . . ? C31 C30 C29 118.4(5) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 120.0 . . ? C30 C32 H32B 120.0 . . ? H32A C32 H32B 120.0 . . ? O8 C33 O7 125.3(4) . . ? O8 C33 C34 116.5(4) . . ? O7 C33 C34 118.2(4) . . ? C36 C34 C35 123.1(5) . . ? C36 C34 C33 118.3(4) . . ? C35 C34 C33 118.7(4) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 120.0 . . ? C34 C36 H36B 120.0 . . ? H36A C36 H36B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cu1 Cu2 O2 2.97(13) . . . . ? O5 Cu1 Cu2 O2 -177.7(2) . . . . ? O7 Cu1 Cu2 O2 93.67(15) . . . . ? O3 Cu1 Cu2 O2 -87.38(15) . . . . ? N1 Cu1 Cu2 O2 -70.5(7) . . . . ? O1 Cu1 Cu2 O4 91.59(14) . . . . ? O5 Cu1 Cu2 O4 -89.10(15) . . . . ? O7 Cu1 Cu2 O4 -177.71(19) . . . . ? O3 Cu1 Cu2 O4 1.23(13) . . . . ? N1 Cu1 Cu2 O4 18.1(7) . . . . ? O1 Cu1 Cu2 O8 -88.22(15) . . . . ? O5 Cu1 Cu2 O8 91.10(15) . . . . ? O7 Cu1 Cu2 O8 2.49(13) . . . . ? O3 Cu1 Cu2 O8 -178.6(2) . . . . ? N1 Cu1 Cu2 O8 -161.7(7) . . . . ? O1 Cu1 Cu2 O6 -177.84(19) . . . . ? O5 Cu1 Cu2 O6 1.47(12) . . . . ? O7 Cu1 Cu2 O6 -87.14(14) . . . . ? O3 Cu1 Cu2 O6 91.80(14) . . . . ? N1 Cu1 Cu2 O6 108.6(7) . . . . ? O1 Cu1 Cu2 N3 -113.8(6) . . . . ? O5 Cu1 Cu2 N3 65.6(6) . . . . ? O7 Cu1 Cu2 N3 -23.1(6) . . . . ? O3 Cu1 Cu2 N3 155.9(6) . . . . ? N1 Cu1 Cu2 N3 172.7(12) . . . . ? O5 Cu1 O1 C21 -8.6(12) . . . . ? O7 Cu1 O1 C21 -91.2(4) . . . . ? O3 Cu1 O1 C21 75.8(4) . . . . ? N1 Cu1 O1 C21 167.1(4) . . . . ? Cu2 Cu1 O1 C21 -4.5(4) . . . . ? O4 Cu2 O2 C21 -91.4(4) . . . . ? O8 Cu2 O2 C21 79.3(4) . . . . ? O6 Cu2 O2 C21 -6.2(10) . . . . ? N3 Cu2 O2 C21 167.2(4) . . . . ? Cu1 Cu2 O2 C21 -2.6(4) . . . . ? O1 Cu1 O3 C25 -84.7(4) . . . . ? O5 Cu1 O3 C25 85.7(4) . . . . ? O7 Cu1 O3 C25 3.4(10) . . . . ? N1 Cu1 O3 C25 -178.7(4) . . . . ? Cu2 Cu1 O3 C25 -1.2(4) . . . . ? O2 Cu2 O4 C25 83.5(3) . . . . ? O8 Cu2 O4 C25 -0.5(12) . . . . ? O6 Cu2 O4 C25 -83.6(3) . . . . ? N3 Cu2 O4 C25 -176.8(3) . . . . ? Cu1 Cu2 O4 C25 -1.7(3) . . . . ? O1 Cu1 O5 C29 1.0(13) . . . . ? O7 Cu1 O5 C29 83.7(4) . . . . ? O3 Cu1 O5 C29 -83.3(4) . . . . ? N1 Cu1 O5 C29 -174.7(4) . . . . ? Cu2 Cu1 O5 C29 -3.1(4) . . . . ? O2 Cu2 O6 C29 3.2(9) . . . . ? O4 Cu2 O6 C29 88.2(4) . . . . ? O8 Cu2 O6 C29 -82.5(4) . . . . ? N3 Cu2 O6 C29 -170.3(4) . . . . ? Cu1 Cu2 O6 C29 -0.4(4) . . . . ? O1 Cu1 O7 C33 82.0(3) . . . . ? O5 Cu1 O7 C33 -88.6(3) . . . . ? O3 Cu1 O7 C33 -6.1(9) . . . . ? N1 Cu1 O7 C33 176.1(3) . . . . ? Cu2 Cu1 O7 C33 -1.5(3) . . . . ? O2 Cu2 O8 C33 -89.7(4) . . . . ? O4 Cu2 O8 C33 -5.8(12) . . . . ? O6 Cu2 O8 C33 77.4(4) . . . . ? N3 Cu2 O8 C33 170.5(4) . . . . ? Cu1 Cu2 O8 C33 -4.6(4) . . . . ? O1 Cu1 N1 C1 139.1(4) . . . . ? O5 Cu1 N1 C1 -41.6(4) . . . . ? O7 Cu1 N1 C1 47.9(4) . . . . ? O3 Cu1 N1 C1 -131.6(4) . . . . ? Cu2 Cu1 N1 C1 -148.2(5) . . . . ? O1 Cu1 N1 C5 -45.2(4) . . . . ? O5 Cu1 N1 C5 134.1(4) . . . . ? O7 Cu1 N1 C5 -136.4(4) . . . . ? O3 Cu1 N1 C5 44.1(4) . . . . ? Cu2 Cu1 N1 C5 27.5(10) . . . . ? O2 Cu2 N3 C11 39.1(4) . . . . ? O4 Cu2 N3 C11 -51.3(5) . . . . ? O8 Cu2 N3 C11 129.3(4) . . . . ? O6 Cu2 N3 C11 -142.3(4) . . . . ? Cu1 Cu2 N3 C11 154.6(4) . . . . ? O2 Cu2 N3 C15 -137.9(4) . . . . ? O4 Cu2 N3 C15 131.7(3) . . . . ? O8 Cu2 N3 C15 -47.7(4) . . . . ? O6 Cu2 N3 C15 40.7(4) . . . . ? Cu1 Cu2 N3 C15 -22.4(8) . . . . ? C5 N1 C1 C2 1.2(7) . . . . ? Cu1 N1 C1 C2 176.9(3) . . . . ? N1 C1 C2 C3 -0.5(7) . . . . ? C1 C2 C3 C4 -0.4(7) . . . . ? C2 C3 C4 C5 0.5(7) . . . . ? C2 C3 C4 C6 179.6(4) . . . . ? C1 N1 C5 C4 -1.1(7) . . . . ? Cu1 N1 C5 C4 -177.0(3) . . . . ? C3 C4 C5 N1 0.3(7) . . . . ? C6 C4 C5 N1 -178.8(4) . . . . ? C10 N2 C6 C4 -67.8(4) . . . . ? C9 N2 C6 C4 169.8(3) . . . . ? C10 N2 C6 C7 168.5(3) . . . . ? C9 N2 C6 C7 46.1(4) . . . . ? C3 C4 C6 N2 139.6(4) . . . . ? C5 C4 C6 N2 -41.3(5) . . . . ? C3 C4 C6 C7 -103.2(5) . . . . ? C5 C4 C6 C7 75.9(6) . . . . ? N2 C6 C7 C8 -32.0(5) . . . . ? C4 C6 C7 C8 -154.9(4) . . . . ? C6 C7 C8 C9 6.6(5) . . . . ? C10 N2 C9 C8 -164.8(3) . . . . ? C6 N2 C9 C8 -41.9(4) . . . . ? C7 C8 C9 N2 20.5(5) . . . . ? C15 N3 C11 C12 -0.4(7) . . . . ? Cu2 N3 C11 C12 -177.3(3) . . . . ? N3 C11 C12 C13 0.6(7) . . . . ? C11 C12 C13 C14 -0.4(7) . . . . ? C12 C13 C14 C15 0.0(7) . . . . ? C12 C13 C14 C16 -177.1(4) . . . . ? C11 N3 C15 C14 -0.1(7) . . . . ? Cu2 N3 C15 C14 177.3(4) . . . . ? C13 C14 C15 N3 0.3(7) . . . . ? C16 C14 C15 N3 177.6(4) . . . . ? C20 N4 C16 C14 -66.1(4) . . . . ? C19 N4 C16 C14 170.8(3) . . . . ? C20 N4 C16 C17 170.5(4) . . . . ? C19 N4 C16 C17 47.4(4) . . . . ? C13 C14 C16 N4 -45.9(6) . . . . ? C15 C14 C16 N4 137.1(4) . . . . ? C13 C14 C16 C17 70.9(6) . . . . ? C15 C14 C16 C17 -106.1(5) . . . . ? N4 C16 C17 C18 -35.2(5) . . . . ? C14 C16 C17 C18 -158.4(4) . . . . ? C16 C17 C18 C19 10.4(5) . . . . ? C16 N4 C19 C18 -41.1(4) . . . . ? C20 N4 C19 C18 -163.6(3) . . . . ? C17 C18 C19 N4 17.9(5) . . . . ? Cu1 O1 C21 O2 4.2(7) . . . . ? Cu1 O1 C21 C22 -175.0(3) . . . . ? Cu2 O2 C21 O1 0.0(7) . . . . ? Cu2 O2 C21 C22 179.2(3) . . . . ? O1 C21 C22 C23 5.6(7) . . . . ? O2 C21 C22 C23 -173.7(5) . . . . ? O1 C21 C22 C24 -173.9(5) . . . . ? O2 C21 C22 C24 6.8(7) . . . . ? Cu1 O3 C25 O4 0.3(7) . . . . ? Cu1 O3 C25 C26 178.8(3) . . . . ? Cu2 O4 C25 O3 1.4(6) . . . . ? Cu2 O4 C25 C26 -177.1(3) . . . . ? O3 C25 C26 C28 -179.1(5) . . . . ? O4 C25 C26 C28 -0.5(6) . . . . ? O3 C25 C26 C27 2.1(6) . . . . ? O4 C25 C26 C27 -179.3(4) . . . . ? Cu2 O6 C29 O5 -1.9(7) . . . . ? Cu2 O6 C29 C30 177.5(3) . . . . ? Cu1 O5 C29 O6 3.8(7) . . . . ? Cu1 O5 C29 C30 -175.6(3) . . . . ? O6 C29 C30 C32 -5.1(7) . . . . ? O5 C29 C30 C32 174.4(5) . . . . ? O6 C29 C30 C31 176.1(5) . . . . ? O5 C29 C30 C31 -4.4(7) . . . . ? Cu2 O8 C33 O7 5.2(7) . . . . ? Cu2 O8 C33 C34 -175.9(3) . . . . ? Cu1 O7 C33 O8 -1.5(6) . . . . ? Cu1 O7 C33 C34 179.6(3) . . . . ? O8 C33 C34 C36 0.7(6) . . . . ? O7 C33 C34 C36 179.7(4) . . . . ? O8 C33 C34 C35 -179.9(5) . . . . ? O7 C33 C34 C35 -0.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.302 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.054 #===END #------------------------------------------- #-------COMPOUND Z3VBS --------------------- #------------------------------------------- data_shersot1 _database_code_depnum_ccdc_archive 'CCDC 715353' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H40 N2 O4 Zn' _chemical_formula_weight 594.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.6170(2) _cell_length_b 12.0528(3) _cell_length_c 13.7930(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.446(1) _cell_angle_gamma 90.00 _cell_volume 1432.48(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3384 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Collected at Soton June 2004. ; _diffrn_ambient_temperature 120(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 16884 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.53 _reflns_number_total 6407 _reflns_number_gt 6010 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0092P)^2^+0.4008P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.026(8) _refine_ls_number_reflns 6407 _refine_ls_number_parameters 355 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.004 _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 0.12358(2) 0.17441(2) 0.735657(14) 0.02445(6) Uani 1 1 d . . . O1 O 0.2613(2) 0.11395(14) 0.63013(16) 0.0522(5) Uani 1 1 d . . . O2 O 0.3143(3) 0.01889(17) 0.76121(14) 0.0554(6) Uani 1 1 d . . . O3 O 0.14968(18) 0.33413(13) 0.73694(10) 0.0312(3) Uani 1 1 d . . . O4 O 0.3808(2) 0.32601(13) 0.81125(13) 0.0374(4) Uani 1 1 d . . . N1 N -0.0911(2) 0.12537(16) 0.67616(13) 0.0303(4) Uani 1 1 d . . . N2 N 0.0320(2) 0.13586(13) 0.87236(12) 0.0222(3) Uani 1 1 d . . . C1 C -0.0872(3) 0.1342(2) 0.56730(17) 0.0423(7) Uani 1 1 d . . . H1A H -0.1840 0.1028 0.5395 0.051 Uiso 1 1 calc R . . H1B H 0.0012 0.0906 0.5422 0.051 Uiso 1 1 calc R . . C2 C -0.0709(3) 0.2541(3) 0.53616(17) 0.0469(7) Uani 1 1 d . . . H2A H -0.0683 0.2581 0.4645 0.056 Uiso 1 1 calc R . . H2B H 0.0282 0.2843 0.5615 0.056 Uiso 1 1 calc R . . C3 C -0.2048(3) 0.3241(3) 0.57327(19) 0.0504(7) Uani 1 1 d . . . H3A H -0.3028 0.3002 0.5417 0.061 Uiso 1 1 calc R . . H3B H -0.1871 0.4030 0.5569 0.061 Uiso 1 1 calc R . . C4 C -0.2180(3) 0.3112(2) 0.68342(18) 0.0408(6) Uani 1 1 d . . . H4A H -0.1267 0.3458 0.7152 0.049 Uiso 1 1 calc R . . H4B H -0.3120 0.3504 0.7060 0.049 Uiso 1 1 calc R . . C5 C -0.2273(2) 0.1896(2) 0.71293(15) 0.0346(6) Uani 1 1 d . . . H5 H -0.3219 0.1581 0.6808 0.042 Uiso 1 1 calc R . . C6 C -0.2464(2) 0.1726(3) 0.82212(13) 0.0314(4) Uani 1 1 d . . . H6 H -0.3383 0.2168 0.8433 0.038 Uiso 1 1 calc R . . C7 C -0.2825(3) 0.0498(2) 0.83955(18) 0.0380(6) Uani 1 1 d . . . H7A H -0.3059 0.0366 0.9088 0.046 Uiso 1 1 calc R . . H7B H -0.3731 0.0264 0.8000 0.046 Uiso 1 1 calc R . . C8 C -0.1377(3) -0.01467(19) 0.80990(18) 0.0372(6) Uani 1 1 d . . . H8 H -0.1605 -0.0955 0.8181 0.045 Uiso 1 1 calc R . . C9 C -0.1075(3) 0.0059(2) 0.70260(18) 0.0371(6) Uani 1 1 d . . . H9A H -0.0114 -0.0336 0.6842 0.044 Uiso 1 1 calc R . . H9B H -0.1941 -0.0263 0.6643 0.044 Uiso 1 1 calc R . . C10 C -0.1081(2) 0.20610(16) 0.88589(14) 0.0249(4) Uani 1 1 d . . . H10A H -0.0808 0.2842 0.8716 0.030 Uiso 1 1 calc R . . H10B H -0.1395 0.2022 0.9547 0.030 Uiso 1 1 calc R . . C11 C -0.0010(3) 0.01425(17) 0.87748(16) 0.0295(5) Uani 1 1 d . . . H11 H 0.0924 -0.0250 0.8519 0.035 Uiso 1 1 calc R . . C12 C -0.0263(3) -0.02788(18) 0.98107(17) 0.0364(6) Uani 1 1 d . . . H12A H -0.1246 0.0031 1.0061 0.044 Uiso 1 1 calc R . . H12B H -0.0362 -0.1097 0.9800 0.044 Uiso 1 1 calc R . . C13 C 0.1063(3) 0.0045(2) 1.04916(18) 0.0398(6) Uani 1 1 d . . . H13A H 0.2029 -0.0332 1.0291 0.048 Uiso 1 1 calc R . . H13B H 0.0820 -0.0193 1.1161 0.048 Uiso 1 1 calc R . . C14 C 0.1295(3) 0.13028(19) 1.04643(15) 0.0326(5) Uani 1 1 d . . . H14A H 0.0361 0.1680 1.0718 0.039 Uiso 1 1 calc R . . H14B H 0.2193 0.1511 1.0878 0.039 Uiso 1 1 calc R . . C15 C 0.1579(2) 0.1664(2) 0.94256(12) 0.0249(4) Uani 1 1 d . . . H15A H 0.1712 0.2480 0.9415 0.030 Uiso 1 1 calc R . . H15B H 0.2563 0.1329 0.9204 0.030 Uiso 1 1 calc R . . C16 C 0.3350(3) 0.03851(18) 0.67444(19) 0.0344(5) Uani 1 1 d . A . C17 C 0.4468(2) -0.03018(16) 0.61702(15) 0.0224(4) Uani 1 1 d . . . C18 C 0.5145(7) -0.1244(5) 0.6467(4) 0.0254(17) Uiso 0.50 1 d P A 1 H18 H 0.4946 -0.1515 0.7101 0.030 Uiso 0.50 1 calc PR A 1 C19 C 0.6158(5) -0.1848(3) 0.5847(4) 0.0197(8) Uiso 0.50 1 d P A 1 C20 C 0.6376(5) -0.1421(4) 0.4926(3) 0.0217(8) Uiso 0.50 1 d P A 1 H20 H 0.7011 -0.1817 0.4485 0.026 Uiso 0.50 1 calc PR A 1 C21 C 0.5698(5) -0.0439(4) 0.4627(3) 0.0263(10) Uiso 0.50 1 d P A 1 H21 H 0.5872 -0.0168 0.3990 0.032 Uiso 0.50 1 calc PR A 1 C22 C 0.4771(7) 0.0148(5) 0.5252(4) 0.0255(14) Uiso 0.50 1 d P A 1 H22 H 0.4344 0.0843 0.5066 0.031 Uiso 0.50 1 calc PR A 1 C23 C 0.6973(5) -0.2848(4) 0.6153(3) 0.0289(9) Uiso 0.50 1 d P A 1 H23 H 0.7575 -0.3214 0.5675 0.035 Uiso 0.50 1 calc PR A 1 C24 C 0.6962(6) -0.3301(6) 0.7030(3) 0.0390(11) Uiso 0.50 1 d P A 1 H24A H 0.6378 -0.2968 0.7534 0.047 Uiso 0.50 1 calc PR A 1 H24B H 0.7537 -0.3959 0.7154 0.047 Uiso 0.50 1 calc PR A 1 C25 C 0.2700(3) 0.37737(18) 0.77905(14) 0.0263(5) Uani 1 1 d . . . C26 C 0.2618(2) 0.50244(17) 0.78753(14) 0.0244(4) Uani 1 1 d . . . C27 C 0.3597(2) 0.55648(17) 0.85329(14) 0.0240(4) Uani 1 1 d . . . H27 H 0.4343 0.5145 0.8886 0.029 Uiso 1 1 calc R . . C28 C 0.3504(2) 0.6707(2) 0.86837(12) 0.0251(4) Uani 1 1 d . . . C29 C 0.2423(3) 0.73110(17) 0.81399(15) 0.0302(5) Uani 1 1 d . . . H29 H 0.2345 0.8091 0.8224 0.036 Uiso 1 1 calc R . . C30 C 0.1464(2) 0.6777(3) 0.74780(13) 0.0322(4) Uani 1 1 d . . . H30 H 0.0739 0.7196 0.7106 0.039 Uiso 1 1 calc R . . C31 C 0.1549(3) 0.56401(19) 0.73521(15) 0.0296(5) Uani 1 1 d . . . H31 H 0.0871 0.5282 0.6905 0.036 Uiso 1 1 calc R . . C32 C 0.4520(3) 0.72343(18) 0.94120(15) 0.0305(5) Uani 1 1 d . . . H32 H 0.5030 0.6753 0.9857 0.037 Uiso 1 1 calc R . . C33 C 0.4798(3) 0.8307(2) 0.95126(18) 0.0389(6) Uani 1 1 d . . . H33A H 0.4318 0.8825 0.9087 0.047 Uiso 1 1 calc R . . H33B H 0.5478 0.8560 1.0011 0.047 Uiso 1 1 calc R . . C21A C 0.6006(5) -0.0880(5) 0.4793(3) 0.0238(9) Uiso 0.50 1 d P A 2 H21A H 0.6372 -0.0746 0.4156 0.029 Uiso 0.50 1 calc PR A 2 C20A C 0.6475(5) -0.1816(4) 0.5296(4) 0.0210(8) Uiso 0.50 1 d P A 2 H20A H 0.7145 -0.2330 0.4988 0.025 Uiso 0.50 1 calc PR A 2 C24A C 0.7595(6) -0.3704(4) 0.6584(4) 0.0376(11) Uiso 0.50 1 d P A 2 H24C H 0.8140 -0.3632 0.5991 0.045 Uiso 0.50 1 calc PR A 2 H24D H 0.7833 -0.4297 0.7014 0.045 Uiso 0.50 1 calc PR A 2 C19A C 0.5994(5) -0.2027(3) 0.6240(3) 0.0212(9) Uiso 0.50 1 d P A 2 C23A C 0.6522(6) -0.2992(4) 0.6807(4) 0.0317(11) Uiso 0.50 1 d P A 2 H23A H 0.6019 -0.3108 0.7409 0.038 Uiso 0.50 1 calc PR A 2 C18A C 0.5000(7) -0.1282(5) 0.6660(4) 0.0217(15) Uiso 0.50 1 d P A 2 H18A H 0.4650 -0.1421 0.7300 0.026 Uiso 0.50 1 calc PR A 2 C22A C 0.4985(7) -0.0130(5) 0.5234(4) 0.0256(14) Uiso 0.50 1 d P A 2 H22A H 0.4642 0.0505 0.4885 0.031 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02294(11) 0.02561(11) 0.02488(10) -0.00221(12) 0.00430(8) -0.00739(12) O1 0.0298(10) 0.0275(9) 0.0991(16) -0.0129(10) -0.0069(10) 0.0079(8) O2 0.0645(14) 0.0516(12) 0.0507(12) -0.0258(10) 0.0407(10) -0.0252(11) O3 0.0322(9) 0.0281(8) 0.0332(8) -0.0025(6) 0.0012(7) -0.0119(7) O4 0.0405(10) 0.0258(8) 0.0457(10) 0.0027(8) -0.0043(8) -0.0017(7) N1 0.0245(9) 0.0388(10) 0.0277(9) -0.0086(8) 0.0045(7) -0.0084(8) N2 0.0241(9) 0.0173(7) 0.0253(8) -0.0023(6) 0.0044(7) -0.0026(6) C1 0.0286(12) 0.0708(18) 0.0276(11) -0.0130(11) -0.0005(9) -0.0105(12) C2 0.0347(14) 0.080(2) 0.0258(12) 0.0072(13) -0.0001(10) -0.0060(15) C3 0.0336(14) 0.0755(19) 0.0422(14) 0.0134(14) -0.0054(11) -0.0021(14) C4 0.0303(13) 0.0537(16) 0.0384(13) 0.0035(11) 0.0028(10) 0.0020(12) C5 0.0206(9) 0.0500(17) 0.0333(10) -0.0080(11) 0.0013(8) -0.0072(11) C6 0.0202(9) 0.0393(10) 0.0349(9) -0.0062(14) 0.0066(7) -0.0001(13) C7 0.0301(13) 0.0424(14) 0.0416(13) -0.0073(11) 0.0111(10) -0.0176(11) C8 0.0381(14) 0.0267(12) 0.0470(14) -0.0093(10) 0.0134(11) -0.0143(10) C9 0.0348(13) 0.0360(13) 0.0406(13) -0.0177(11) 0.0106(11) -0.0181(11) C10 0.0265(10) 0.0212(10) 0.0271(9) -0.0049(7) 0.0059(8) -0.0001(8) C11 0.0336(12) 0.0177(10) 0.0374(12) -0.0026(9) 0.0135(10) -0.0029(9) C12 0.0413(14) 0.0219(11) 0.0461(14) 0.0061(10) 0.0149(11) -0.0009(10) C13 0.0472(15) 0.0353(13) 0.0371(12) 0.0116(10) 0.0140(11) 0.0079(12) C14 0.0361(12) 0.0341(11) 0.0276(10) 0.0016(9) 0.0054(9) 0.0031(10) C15 0.0255(9) 0.0245(10) 0.0247(8) 0.0002(10) 0.0014(7) -0.0015(11) C16 0.0224(11) 0.0233(11) 0.0575(15) -0.0133(10) 0.0085(11) -0.0082(9) C17 0.0180(10) 0.0225(10) 0.0266(10) -0.0037(8) 0.0028(8) -0.0036(8) C25 0.0303(12) 0.0251(11) 0.0235(10) -0.0004(9) 0.0051(9) -0.0075(9) C26 0.0242(11) 0.0253(10) 0.0237(9) 0.0032(8) 0.0031(8) -0.0062(9) C27 0.0237(10) 0.0247(10) 0.0236(9) 0.0045(8) 0.0017(8) -0.0029(8) C28 0.0269(9) 0.0241(9) 0.0243(8) 0.0009(11) 0.0060(7) -0.0113(12) C29 0.0363(12) 0.0229(11) 0.0314(11) 0.0017(8) 0.0036(9) -0.0023(9) C30 0.0319(10) 0.0326(10) 0.0319(9) 0.0052(13) -0.0029(8) 0.0026(14) C31 0.0332(12) 0.0299(11) 0.0257(10) -0.0005(9) -0.0007(9) -0.0048(9) C32 0.0301(12) 0.0311(11) 0.0303(11) -0.0009(9) 0.0017(9) -0.0074(9) C33 0.0444(14) 0.0365(12) 0.0357(12) -0.0077(10) 0.0014(11) -0.0101(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 1.9382(15) . ? Zn1 O1 2.021(2) . ? Zn1 N2 2.1016(16) . ? Zn1 N1 2.1026(18) . ? Zn1 C16 2.596(2) . ? O1 C16 1.264(3) . ? O2 C16 1.234(3) . ? O3 C25 1.294(3) . ? O4 C25 1.219(3) . ? N1 C9 1.492(3) . ? N1 C5 1.498(3) . ? N1 C1 1.506(3) . ? N2 C10 1.488(3) . ? N2 C15 1.494(2) . ? N2 C11 1.495(2) . ? C1 C2 1.515(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.521(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.532(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.522(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.530(3) . ? C5 H5 1.0000 . ? C6 C10 1.530(3) . ? C6 C7 1.532(4) . ? C6 H6 1.0000 . ? C7 C8 1.528(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.525(3) . ? C8 C11 1.537(3) . ? C8 H8 1.0000 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.534(3) . ? C11 H11 1.0000 . ? C12 C13 1.524(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.530(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.519(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.501(3) . ? C17 C18 1.339(7) . ? C17 C22A 1.385(6) . ? C17 C22 1.404(6) . ? C17 C18A 1.434(6) . ? C18 C19 1.426(7) . ? C18 H18 0.9500 . ? C19 C20 1.385(6) . ? C19 C23 1.455(6) . ? C20 C21 1.382(6) . ? C20 H20 0.9500 . ? C21 C22 1.375(7) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.328(6) . ? C23 H23 0.9500 . ? C24 H24A 0.9500 . ? C24 H24B 0.9500 . ? C25 C26 1.514(3) . ? C26 C31 1.382(3) . ? C26 C27 1.395(3) . ? C27 C28 1.395(3) . ? C27 H27 0.9500 . ? C28 C29 1.396(3) . ? C28 C32 1.471(3) . ? C29 C30 1.385(3) . ? C29 H29 0.9500 . ? C30 C31 1.383(4) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.322(3) . ? C32 H32 0.9500 . ? C33 H33A 0.9500 . ? C33 H33B 0.9500 . ? C21A C20A 1.382(7) . ? C21A C22A 1.403(8) . ? C21A H21A 0.9500 . ? C20A C19A 1.393(6) . ? C20A H20A 0.9500 . ? C24A C23A 1.300(7) . ? C24A H24C 0.9500 . ? C24A H24D 0.9500 . ? C19A C18A 1.372(7) . ? C19A C23A 1.471(7) . ? C23A H23A 0.9500 . ? C18A H18A 0.9500 . ? C22A H22A 0.9500 . ? 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 107.21(7) . . ? O3 Zn1 N2 104.82(6) . . ? O1 Zn1 N2 142.47(7) . . ? O3 Zn1 N1 112.61(7) . . ? O1 Zn1 N1 97.89(7) . . ? N2 Zn1 N1 87.29(7) . . ? O3 Zn1 C16 123.23(7) . . ? O1 Zn1 C16 28.45(8) . . ? N2 Zn1 C16 114.94(7) . . ? N1 Zn1 C16 108.25(7) . . ? C16 O1 Zn1 101.93(17) . . ? C25 O3 Zn1 119.77(15) . . ? C9 N1 C5 109.90(18) . . ? C9 N1 C1 108.33(18) . . ? C5 N1 C1 108.94(18) . . ? C9 N1 Zn1 105.11(15) . . ? C5 N1 Zn1 114.31(13) . . ? C1 N1 Zn1 110.07(13) . . ? C10 N2 C15 111.36(15) . . ? C10 N2 C11 113.40(16) . . ? C15 N2 C11 110.39(18) . . ? C10 N2 Zn1 107.31(12) . . ? C15 N2 Zn1 104.54(11) . . ? C11 N2 Zn1 109.39(11) . . ? N1 C1 C2 110.66(19) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? C1 C2 C3 111.2(2) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 109.9(2) . . ? C2 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? C2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C3 111.5(2) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? N1 C5 C4 111.37(18) . . ? N1 C5 C6 110.8(2) . . ? C4 C5 C6 113.5(2) . . ? N1 C5 H5 106.9 . . ? C4 C5 H5 106.9 . . ? C6 C5 H5 106.9 . . ? C5 C6 C10 116.17(17) . . ? C5 C6 C7 107.9(2) . . ? C10 C6 C7 108.8(2) . . ? C5 C6 H6 107.9 . . ? C10 C6 H6 107.9 . . ? C7 C6 H6 107.9 . . ? C8 C7 C6 106.40(17) . . ? C8 C7 H7A 110.4 . . ? C6 C7 H7A 110.4 . . ? C8 C7 H7B 110.4 . . ? C6 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? C9 C8 C7 108.8(2) . . ? C9 C8 C11 114.57(19) . . ? C7 C8 C11 110.25(18) . . ? C9 C8 H8 107.6 . . ? C7 C8 H8 107.6 . . ? C11 C8 H8 107.6 . . ? N1 C9 C8 114.27(17) . . ? N1 C9 H9A 108.7 . . ? C8 C9 H9A 108.7 . . ? N1 C9 H9B 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? N2 C10 C6 114.03(17) . . ? N2 C10 H10A 108.7 . . ? C6 C10 H10A 108.7 . . ? N2 C10 H10B 108.7 . . ? C6 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N2 C11 C12 113.40(17) . . ? N2 C11 C8 109.81(18) . . ? C12 C11 C8 112.09(18) . . ? N2 C11 H11 107.1 . . ? C12 C11 H11 107.1 . . ? C8 C11 H11 107.1 . . ? C13 C12 C11 112.21(18) . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 C14 109.6(2) . . ? C12 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? C12 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C15 C14 C13 109.23(19) . . ? C15 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? C15 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? N2 C15 C14 114.76(17) . . ? N2 C15 H15A 108.6 . . ? C14 C15 H15A 108.6 . . ? N2 C15 H15B 108.6 . . ? C14 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? O2 C16 O1 122.1(2) . . ? O2 C16 C17 120.3(2) . . ? O1 C16 C17 117.6(2) . . ? O2 C16 Zn1 72.45(15) . . ? O1 C16 Zn1 49.62(12) . . ? C17 C16 Zn1 167.08(18) . . ? C18 C17 C22A 105.6(4) . . ? C18 C17 C22 121.3(4) . . ? C22A C17 C22 15.8(3) . . ? C18 C17 C18A 11.7(4) . . ? C22A C17 C18A 117.3(4) . . ? C22 C17 C18A 133.0(4) . . ? C18 C17 C16 125.9(3) . . ? C22A C17 C16 128.5(3) . . ? C22 C17 C16 112.8(3) . . ? C18A C17 C16 114.2(3) . . ? C17 C18 C19 121.1(5) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C20 C19 C18 116.6(4) . . ? C20 C19 C23 120.3(5) . . ? C18 C19 C23 123.0(5) . . ? C21 C20 C19 122.2(4) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C22 C21 C20 120.0(5) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C17 118.7(5) . . ? C21 C22 H22 120.7 . . ? C17 C22 H22 120.7 . . ? C24 C23 C19 126.7(5) . . ? C24 C23 H23 116.6 . . ? C19 C23 H23 116.6 . . ? C23 C24 H24A 120.0 . . ? C23 C24 H24B 120.0 . . ? H24A C24 H24B 120.0 . . ? O4 C25 O3 125.6(2) . . ? O4 C25 C26 121.0(2) . . ? O3 C25 C26 113.4(2) . . ? C31 C26 C27 119.07(19) . . ? C31 C26 C25 121.73(19) . . ? C27 C26 C25 119.13(19) . . ? C28 C27 C26 121.52(19) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C27 C28 C29 118.23(19) . . ? C27 C28 C32 119.6(2) . . ? C29 C28 C32 122.2(2) . . ? C30 C29 C28 120.3(2) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 120.7(2) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C26 C31 C30 120.2(2) . . ? C26 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C33 C32 C28 126.9(2) . . ? C33 C32 H32 116.6 . . ? C28 C32 H32 116.6 . . ? C32 C33 H33A 120.0 . . ? C32 C33 H33B 120.0 . . ? H33A C33 H33B 120.0 . . ? C20A C21A C22A 119.3(4) . . ? C20A C21A H21A 120.3 . . ? C22A C21A H21A 120.3 . . ? C21A C20A C19A 122.0(4) . . ? C21A C20A H20A 119.0 . . ? C19A C20A H20A 119.0 . . ? C23A C24A H24C 120.0 . . ? C23A C24A H24D 120.0 . . ? H24C C24A H24D 120.0 . . ? C18A C19A C20A 117.8(4) . . ? C18A C19A C23A 119.0(4) . . ? C20A C19A C23A 123.3(4) . . ? C24A C23A C19A 127.9(5) . . ? C24A C23A H23A 116.1 . . ? C19A C23A H23A 116.1 . . ? C19A C18A C17 122.6(5) . . ? C19A C18A H18A 118.7 . . ? C17 C18A H18A 118.7 . . ? C17 C22A C21A 121.0(5) . . ? C17 C22A H22A 119.5 . . ? C21A C22A H22A 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 O1 C16 129.24(14) . . . . ? N2 Zn1 O1 C16 -18.2(2) . . . . ? N1 Zn1 O1 C16 -114.06(14) . . . . ? O1 Zn1 O3 C25 -79.47(15) . . . . ? N2 Zn1 O3 C25 80.70(15) . . . . ? N1 Zn1 O3 C25 173.98(13) . . . . ? C16 Zn1 O3 C25 -53.30(17) . . . . ? O3 Zn1 N1 C9 -166.64(12) . . . . ? O1 Zn1 N1 C9 80.95(13) . . . . ? N2 Zn1 N1 C9 -61.71(13) . . . . ? C16 Zn1 N1 C9 53.69(14) . . . . ? O3 Zn1 N1 C5 -46.06(16) . . . . ? O1 Zn1 N1 C5 -158.47(15) . . . . ? N2 Zn1 N1 C5 58.87(15) . . . . ? C16 Zn1 N1 C5 174.27(15) . . . . ? O3 Zn1 N1 C1 76.92(16) . . . . ? O1 Zn1 N1 C1 -35.50(17) . . . . ? N2 Zn1 N1 C1 -178.15(16) . . . . ? C16 Zn1 N1 C1 -62.76(17) . . . . ? O3 Zn1 N2 C10 53.57(13) . . . . ? O1 Zn1 N2 C10 -158.56(12) . . . . ? N1 Zn1 N2 C10 -59.12(12) . . . . ? C16 Zn1 N2 C10 -168.00(11) . . . . ? O3 Zn1 N2 C15 -64.80(14) . . . . ? O1 Zn1 N2 C15 83.08(17) . . . . ? N1 Zn1 N2 C15 -177.48(14) . . . . ? C16 Zn1 N2 C15 73.63(14) . . . . ? O3 Zn1 N2 C11 176.98(14) . . . . ? O1 Zn1 N2 C11 -35.14(19) . . . . ? N1 Zn1 N2 C11 64.30(14) . . . . ? C16 Zn1 N2 C11 -44.59(15) . . . . ? C9 N1 C1 C2 179.9(2) . . . . ? C5 N1 C1 C2 60.4(3) . . . . ? Zn1 N1 C1 C2 -65.7(2) . . . . ? N1 C1 C2 C3 -59.2(3) . . . . ? C1 C2 C3 C4 54.5(3) . . . . ? C2 C3 C4 C5 -53.0(3) . . . . ? C9 N1 C5 C4 -177.50(19) . . . . ? C1 N1 C5 C4 -59.0(2) . . . . ? Zn1 N1 C5 C4 64.6(2) . . . . ? C9 N1 C5 C6 55.2(3) . . . . ? C1 N1 C5 C6 173.8(2) . . . . ? Zn1 N1 C5 C6 -62.7(2) . . . . ? C3 C4 C5 N1 56.2(3) . . . . ? C3 C4 C5 C6 -177.96(18) . . . . ? N1 C5 C6 C10 58.8(3) . . . . ? C4 C5 C6 C10 -67.3(3) . . . . ? N1 C5 C6 C7 -63.6(2) . . . . ? C4 C5 C6 C7 170.25(19) . . . . ? C5 C6 C7 C8 65.6(2) . . . . ? C10 C6 C7 C8 -61.2(2) . . . . ? C6 C7 C8 C9 -61.2(2) . . . . ? C6 C7 C8 C11 65.2(2) . . . . ? C5 N1 C9 C8 -52.3(3) . . . . ? C1 N1 C9 C8 -171.2(2) . . . . ? Zn1 N1 C9 C8 71.2(2) . . . . ? C7 C8 C9 N1 56.3(3) . . . . ? C11 C8 C9 N1 -67.7(3) . . . . ? C15 N2 C10 C6 -175.05(17) . . . . ? C11 N2 C10 C6 -49.8(2) . . . . ? Zn1 N2 C10 C6 71.10(18) . . . . ? C5 C6 C10 N2 -67.0(3) . . . . ? C7 C6 C10 N2 55.0(2) . . . . ? C10 N2 C11 C12 -75.7(2) . . . . ? C15 N2 C11 C12 50.0(2) . . . . ? Zn1 N2 C11 C12 164.54(15) . . . . ? C10 N2 C11 C8 50.5(2) . . . . ? C15 N2 C11 C8 176.29(15) . . . . ? Zn1 N2 C11 C8 -69.20(17) . . . . ? C9 C8 C11 N2 63.6(2) . . . . ? C7 C8 C11 N2 -59.6(2) . . . . ? C9 C8 C11 C12 -169.37(19) . . . . ? C7 C8 C11 C12 67.4(2) . . . . ? N2 C11 C12 C13 -52.8(3) . . . . ? C8 C11 C12 C13 -177.83(18) . . . . ? C11 C12 C13 C14 55.2(2) . . . . ? C12 C13 C14 C15 -56.3(2) . . . . ? C10 N2 C15 C14 73.2(2) . . . . ? C11 N2 C15 C14 -53.7(2) . . . . ? Zn1 N2 C15 C14 -171.25(16) . . . . ? C13 C14 C15 N2 57.5(3) . . . . ? Zn1 O1 C16 O2 -0.7(3) . . . . ? Zn1 O1 C16 C17 177.43(15) . . . . ? O3 Zn1 C16 O2 117.17(14) . . . . ? O1 Zn1 C16 O2 179.4(2) . . . . ? N2 Zn1 C16 O2 -12.76(16) . . . . ? N1 Zn1 C16 O2 -108.41(14) . . . . ? O3 Zn1 C16 O1 -62.18(16) . . . . ? N2 Zn1 C16 O1 167.89(14) . . . . ? N1 Zn1 C16 O1 72.24(15) . . . . ? O3 Zn1 C16 C17 -72.4(7) . . . . ? O1 Zn1 C16 C17 -10.2(6) . . . . ? N2 Zn1 C16 C17 157.6(6) . . . . ? N1 Zn1 C16 C17 62.0(7) . . . . ? O2 C16 C17 C18 10.3(5) . . . . ? O1 C16 C17 C18 -167.9(4) . . . . ? Zn1 C16 C17 C18 -159.1(6) . . . . ? O2 C16 C17 C22A -171.8(3) . . . . ? O1 C16 C17 C22A 10.1(4) . . . . ? Zn1 C16 C17 C22A 18.9(8) . . . . ? O2 C16 C17 C22 -169.4(3) . . . . ? O1 C16 C17 C22 12.4(4) . . . . ? Zn1 C16 C17 C22 21.2(8) . . . . ? O2 C16 C17 C18A 11.1(4) . . . . ? O1 C16 C17 C18A -167.1(3) . . . . ? Zn1 C16 C17 C18A -158.3(6) . . . . ? C22A C17 C18 C19 -0.2(6) . . . . ? C22 C17 C18 C19 -2.2(7) . . . . ? C18A C17 C18 C19 174(3) . . . . ? C16 C17 C18 C19 178.1(4) . . . . ? C17 C18 C19 C20 -1.2(7) . . . . ? C17 C18 C19 C23 177.1(4) . . . . ? C18 C19 C20 C21 2.4(6) . . . . ? C23 C19 C20 C21 -176.0(4) . . . . ? C19 C20 C21 C22 -0.1(7) . . . . ? C20 C21 C22 C17 -3.3(7) . . . . ? C18 C17 C22 C21 4.5(7) . . . . ? C22A C17 C22 C21 -2.5(12) . . . . ? C18A C17 C22 C21 3.6(7) . . . . ? C16 C17 C22 C21 -175.8(4) . . . . ? C20 C19 C23 C24 174.8(5) . . . . ? C18 C19 C23 C24 -3.5(7) . . . . ? Zn1 O3 C25 O4 7.8(3) . . . . ? Zn1 O3 C25 C26 -171.10(12) . . . . ? O4 C25 C26 C31 166.6(2) . . . . ? O3 C25 C26 C31 -14.4(3) . . . . ? O4 C25 C26 C27 -16.5(3) . . . . ? O3 C25 C26 C27 162.50(17) . . . . ? C31 C26 C27 C28 1.0(3) . . . . ? C25 C26 C27 C28 -176.01(17) . . . . ? C26 C27 C28 C29 -1.5(3) . . . . ? C26 C27 C28 C32 177.66(17) . . . . ? C27 C28 C29 C30 0.7(3) . . . . ? C32 C28 C29 C30 -178.45(18) . . . . ? C28 C29 C30 C31 0.7(3) . . . . ? C27 C26 C31 C30 0.4(3) . . . . ? C25 C26 C31 C30 177.29(18) . . . . ? C29 C30 C31 C26 -1.2(3) . . . . ? C27 C28 C32 C33 165.8(2) . . . . ? C29 C28 C32 C33 -15.1(3) . . . . ? C22A C21A C20A C19A -1.6(6) . . . . ? C21A C20A C19A C18A 1.3(6) . . . . ? C21A C20A C19A C23A -177.4(4) . . . . ? C18A C19A C23A C24A -170.8(5) . . . . ? C20A C19A C23A C24A 7.9(7) . . . . ? C20A C19A C18A C17 -0.9(7) . . . . ? C23A C19A C18A C17 177.9(4) . . . . ? C18 C17 C18A C19A -5.1(19) . . . . ? C22A C17 C18A C19A 0.8(7) . . . . ? C22 C17 C18A C19A -1.1(8) . . . . ? C16 C17 C18A C19A 178.2(4) . . . . ? C18 C17 C22A C21A 0.2(6) . . . . ? C22 C17 C22A C21A 174.0(18) . . . . ? C18A C17 C22A C21A -1.0(6) . . . . ? C16 C17 C22A C21A -178.1(3) . . . . ? C20A C21A C22A C17 1.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.513 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.045 #===END #----------------------------------------------- #-------------COMPOUND ZADAC ----------------- #------------------------------------------------ data_shersot2 _database_code_depnum_ccdc_archive 'CCDC 715354' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H24 N2 O5 Zn' _chemical_formula_weight 353.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 18.5904(6) _cell_length_b 8.5393(3) _cell_length_c 22.3795(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.848(2) _cell_angle_gamma 90.00 _cell_volume 3400.23(19) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4113 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description sheet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 1.465 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details sadabs # SADABS gives ratio of Tmin to Tmax of 0.7540 _exptl_special_details ; Southampton NCS data collection 2004src0485 ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator 'confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD' _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 22356 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 29.15 _reflns_number_total 7574 _reflns_number_gt 5674 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0300P)^2^+4.3150P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.042(17) _refine_ls_number_reflns 7574 _refine_ls_number_parameters 380 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.041 _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 0.68115(3) 0.51653(5) 0.54249(2) 0.02710(18) Uani 1 1 d . . . Zn2 Zn 0.81604(3) 0.75289(5) 0.95440(2) 0.02631(17) Uani 1 1 d . . . O1 O 0.76623(18) 0.3822(5) 0.58466(16) 0.0385(9) Uani 1 1 d . A . O2 O 0.7880(2) 0.5427(7) 0.66500(18) 0.0640(14) Uani 1 1 d . A . O3 O 0.64394(18) 0.3930(5) 0.46633(15) 0.0326(9) Uani 1 1 d . . . O4 O 0.54921(19) 0.5625(5) 0.44801(16) 0.0388(10) Uani 1 1 d . . . O5 O 0.72968(17) 0.8809(5) 0.90865(15) 0.0347(9) Uani 1 1 d . B . O6 O 0.7017(2) 0.6862(6) 0.84022(18) 0.0487(12) Uani 1 1 d . B . O7 O 0.84854(16) 0.8841(4) 1.02914(14) 0.0294(8) Uani 1 1 d . . . O8 O 0.94979(19) 0.7346(5) 1.05973(16) 0.0407(9) Uani 1 1 d . . . O1S O 0.8461(2) 0.7091(5) 0.77144(16) 0.0528(12) Uani 1 1 d . . . H1S H 0.8196 0.6422 0.7474 0.079 Uiso 1 1 calc R . . O2S O 0.6431(2) 0.5183(6) 0.73191(15) 0.0491(10) Uani 1 1 d . . . H2S H 0.6551 0.5800 0.7624 0.074 Uiso 1 1 calc R . . N1 N 0.70459(19) 0.7443(7) 0.52725(17) 0.0294(10) Uani 1 1 d . . . H1N H 0.7524 0.7705 0.5509 0.035 Uiso 1 1 calc R . . H2N H 0.7008 0.7604 0.4858 0.035 Uiso 1 1 calc R . . N2 N 0.6177(2) 0.5979(5) 0.59559(18) 0.0241(10) Uani 1 1 d . . . H3N H 0.5673 0.5853 0.5754 0.029 Uiso 1 1 calc R . . H4N H 0.6290 0.5462 0.6332 0.029 Uiso 1 1 calc R . . N3 N 0.8883(2) 0.6692(6) 0.90973(18) 0.0280(10) Uani 1 1 d . . . H5N H 0.8682 0.6787 0.8672 0.034 Uiso 1 1 calc R . . H6N H 0.9331 0.7229 0.9218 0.034 Uiso 1 1 calc R . . N4 N 0.79480(19) 0.5264(6) 0.97274(16) 0.0271(10) Uani 1 1 d . . . H7N H 0.8183 0.5018 1.0138 0.032 Uiso 1 1 calc R . . H8N H 0.7440 0.5099 0.9647 0.032 Uiso 1 1 calc R . . C1 C 0.6481(2) 0.8379(6) 0.5460(2) 0.0285(10) Uani 1 1 d . . . H1 H 0.5994 0.8287 0.5123 0.034 Uiso 1 1 calc R . . C2 C 0.6682(3) 1.0103(10) 0.5544(3) 0.0397(14) Uani 1 1 d . . . H2A H 0.6692 1.0546 0.5138 0.048 Uiso 1 1 calc R . . H2B H 0.7192 1.0212 0.5839 0.048 Uiso 1 1 calc R . . C3 C 0.6127(3) 1.1039(8) 0.5790(3) 0.0502(16) Uani 1 1 d . . . H3A H 0.6316 1.2122 0.5884 0.060 Uiso 1 1 calc R . . H3B H 0.5637 1.1092 0.5463 0.060 Uiso 1 1 calc R . . C4 C 0.6017(3) 1.0305(6) 0.6376(3) 0.0492(13) Uani 1 1 d . . . H4A H 0.6490 1.0379 0.6720 0.059 Uiso 1 1 calc R . . H4B H 0.5623 1.0887 0.6501 0.059 Uiso 1 1 calc R . . C5 C 0.5789(3) 0.8606(7) 0.6264(3) 0.0422(15) Uani 1 1 d . . . H5A H 0.5296 0.8540 0.5941 0.051 Uiso 1 1 calc R . . H5B H 0.5733 0.8145 0.6654 0.051 Uiso 1 1 calc R . . C6 C 0.6372(2) 0.7673(5) 0.60502(19) 0.0286(9) Uani 1 1 d . . . H6 H 0.6861 0.7752 0.6385 0.034 Uiso 1 1 calc R . . C7 C 0.8031(3) 0.4226(9) 0.6399(3) 0.0431(16) Uani 1 1 d D . . C10 C 0.5809(3) 0.4479(8) 0.4327(2) 0.0329(14) Uani 1 1 d . . . C11 C 0.5438(3) 0.3725(8) 0.3706(2) 0.0498(15) Uani 1 1 d . . . H11 H 0.4981 0.4161 0.3452 0.060 Uiso 1 1 calc R . . C12 C 0.5704(3) 0.2539(9) 0.3505(3) 0.0678(17) Uani 1 1 d . . . H12A H 0.6160 0.2081 0.3750 0.081 Uiso 1 1 calc R . . H12B H 0.5448 0.2107 0.3109 0.081 Uiso 1 1 calc R . . C13 C 0.8997(2) 0.5032(6) 0.92783(19) 0.0294(9) Uani 1 1 d . . . H13 H 0.9358 0.4980 0.9707 0.035 Uiso 1 1 calc R . . C14 C 0.9330(3) 0.4110(7) 0.8841(3) 0.0461(16) Uani 1 1 d . . . H14A H 0.9823 0.4563 0.8850 0.055 Uiso 1 1 calc R . . H14B H 0.8994 0.4198 0.8409 0.055 Uiso 1 1 calc R . . C15 C 0.9431(3) 0.2383(7) 0.9026(3) 0.0557(14) Uani 1 1 d . . . H15A H 0.9625 0.1806 0.8721 0.067 Uiso 1 1 calc R . . H15B H 0.9803 0.2284 0.9442 0.067 Uiso 1 1 calc R . . C16 C 0.8687(3) 0.1669(9) 0.9044(3) 0.0538(17) Uani 1 1 d . . . H16A H 0.8768 0.0569 0.9187 0.065 Uiso 1 1 calc R . . H16B H 0.8330 0.1671 0.8618 0.065 Uiso 1 1 calc R . . C17 C 0.8351(3) 0.2592(9) 0.9484(2) 0.0399(14) Uani 1 1 d . . . H17A H 0.7856 0.2142 0.9471 0.048 Uiso 1 1 calc R . . H17B H 0.8684 0.2498 0.9916 0.048 Uiso 1 1 calc R . . C18 C 0.8256(2) 0.4310(6) 0.9302(2) 0.0299(11) Uani 1 1 d . . . H18 H 0.7894 0.4377 0.8874 0.036 Uiso 1 1 calc R . . C19 C 0.6899(3) 0.8185(8) 0.8586(3) 0.0396(16) Uani 1 1 d D . . C22 C 0.9093(3) 0.8397(7) 1.0693(2) 0.0269(11) Uani 1 1 d . . . C1S C 0.8137(4) 0.8606(10) 0.7559(3) 0.066(2) Uani 1 1 d . . . H1S1 H 0.8376 0.9346 0.7893 0.099 Uiso 1 1 calc R . . H1S2 H 0.7597 0.8556 0.7513 0.099 Uiso 1 1 calc R . . H1S3 H 0.8216 0.8958 0.7166 0.099 Uiso 1 1 calc R . . C23 C 0.9266(3) 0.9251(7) 1.1299(2) 0.0386(12) Uani 1 1 d . . . H23 H 0.8960 1.0116 1.1334 0.046 Uiso 1 1 calc R . . C24 C 0.9828(3) 0.8854(7) 1.1788(2) 0.0522(14) Uani 1 1 d . . . H24A H 1.0141 0.7993 1.1762 0.063 Uiso 1 1 calc R . . H24B H 0.9919 0.9430 1.2166 0.063 Uiso 1 1 calc R . . C2S C 0.6827(4) 0.3770(9) 0.7481(3) 0.0651(19) Uani 1 1 d . . . H2S1 H 0.7368 0.3977 0.7594 0.098 Uiso 1 1 calc R . . H2S2 H 0.6687 0.3051 0.7125 0.098 Uiso 1 1 calc R . . H2S3 H 0.6701 0.3297 0.7837 0.098 Uiso 1 1 calc R . . C8 C 0.8606(7) 0.3387(17) 0.6865(7) 0.059(4) Uiso 0.50 1 d P A 1 H8 H 0.8835 0.3810 0.7268 0.070 Uiso 0.50 1 calc PR A 1 C9 C 0.8786(8) 0.2053(17) 0.6703(6) 0.064(4) Uiso 0.50 1 d P A 1 H9A H 0.8546 0.1661 0.6297 0.077 Uiso 0.50 1 calc PR A 1 H9B H 0.9160 0.1446 0.6988 0.077 Uiso 0.50 1 calc PR A 1 C20 C 0.6223(5) 0.8855(14) 0.8162(5) 0.036(3) Uiso 0.50 1 d PD B 1 H20 H 0.5917 0.8280 0.7818 0.043 Uiso 0.50 1 calc PR B 1 C21 C 0.6057(6) 1.0291(14) 0.8278(5) 0.040(2) Uiso 0.50 1 d P B 1 H21A H 0.6372 1.0839 0.8625 0.048 Uiso 0.50 1 calc PR B 1 H21B H 0.5621 1.0784 0.8016 0.048 Uiso 0.50 1 calc PR B 1 C8A C 0.8673(7) 0.3034(16) 0.6631(7) 0.059(4) Uiso 0.50 1 d PD A 2 H8A H 0.8718 0.2206 0.6361 0.071 Uiso 0.50 1 calc PR A 2 C9A C 0.9160(8) 0.3118(18) 0.7189(6) 0.079(4) Uiso 0.50 1 d P A 2 H9A1 H 0.9124 0.3938 0.7466 0.095 Uiso 0.50 1 calc PR A 2 H9A2 H 0.9549 0.2360 0.7316 0.095 Uiso 0.50 1 calc PR A 2 C20A C 0.6244(6) 0.9334(16) 0.8296(6) 0.042(3) Uiso 0.50 1 d PD B 2 H20A H 0.6267 1.0392 0.8432 0.050 Uiso 0.50 1 calc PR B 2 C21A C 0.5635(6) 0.8796(16) 0.7845(5) 0.060(3) Uiso 0.50 1 d P B 2 H21C H 0.5617 0.7736 0.7713 0.072 Uiso 0.50 1 calc PR B 2 H21D H 0.5228 0.9481 0.7662 0.072 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0254(3) 0.0253(4) 0.0311(4) -0.0021(3) 0.0090(3) -0.0007(3) Zn2 0.0227(3) 0.0287(4) 0.0283(3) -0.0020(3) 0.0086(2) -0.0006(3) O1 0.0337(19) 0.036(2) 0.043(2) -0.0061(19) 0.0065(16) 0.0100(19) O2 0.047(2) 0.100(4) 0.037(2) -0.022(3) -0.0012(17) -0.004(3) O3 0.0284(17) 0.037(2) 0.0313(18) -0.0056(18) 0.0071(14) 0.0017(18) O4 0.0326(18) 0.047(2) 0.0336(19) -0.0034(17) 0.0037(14) 0.0066(17) O5 0.0305(18) 0.037(2) 0.0327(18) 0.0000(18) 0.0027(14) 0.0023(18) O6 0.048(2) 0.058(3) 0.034(2) -0.005(2) 0.0020(17) -0.010(2) O7 0.0225(16) 0.031(2) 0.0317(17) -0.0085(17) 0.0031(13) 0.0054(16) O8 0.0318(17) 0.052(3) 0.0343(17) -0.0094(19) 0.0042(13) 0.0188(19) O1S 0.049(2) 0.072(3) 0.032(2) -0.009(2) 0.0046(16) -0.007(2) O2S 0.065(2) 0.055(2) 0.0232(16) -0.0024(19) 0.0067(16) -0.002(2) N1 0.026(2) 0.029(3) 0.033(2) 0.001(2) 0.0098(17) -0.001(2) N2 0.0210(19) 0.026(2) 0.027(2) -0.0035(19) 0.0094(16) -0.0003(19) N3 0.030(2) 0.030(3) 0.024(2) -0.007(2) 0.0075(17) -0.011(2) N4 0.0217(19) 0.031(3) 0.032(2) -0.004(2) 0.0136(16) -0.001(2) C1 0.027(2) 0.024(2) 0.032(3) 0.001(2) 0.0055(18) 0.002(2) C2 0.040(3) 0.030(4) 0.049(3) 0.006(3) 0.013(3) -0.013(3) C3 0.053(3) 0.024(3) 0.072(4) -0.005(3) 0.016(3) 0.006(3) C4 0.055(3) 0.032(3) 0.064(3) -0.019(3) 0.022(3) 0.001(3) C5 0.049(3) 0.036(4) 0.048(3) -0.004(3) 0.024(3) 0.004(3) C6 0.025(2) 0.029(2) 0.031(2) -0.004(2) 0.0065(16) -0.001(2) C7 0.033(3) 0.055(4) 0.039(3) 0.013(3) 0.007(2) 0.000(3) C10 0.030(3) 0.045(4) 0.024(2) -0.001(2) 0.008(2) -0.003(2) C11 0.047(3) 0.063(4) 0.040(3) -0.010(3) 0.013(3) 0.000(3) C12 0.060(3) 0.086(5) 0.055(3) -0.027(4) 0.013(3) -0.012(4) C13 0.027(2) 0.030(2) 0.034(2) -0.003(2) 0.0139(18) -0.002(2) C14 0.046(3) 0.044(4) 0.064(4) -0.017(3) 0.040(3) -0.011(3) C15 0.060(3) 0.043(3) 0.079(4) -0.017(3) 0.043(3) 0.002(3) C16 0.067(4) 0.036(3) 0.073(4) -0.010(3) 0.043(3) -0.003(3) C17 0.046(3) 0.025(3) 0.053(3) -0.007(3) 0.021(3) 0.001(4) C18 0.025(2) 0.036(3) 0.030(2) -0.004(2) 0.0100(18) -0.005(2) C19 0.023(3) 0.060(4) 0.034(3) 0.012(3) 0.005(2) -0.005(3) C22 0.026(2) 0.028(3) 0.029(2) -0.005(2) 0.011(2) -0.006(2) C1S 0.065(4) 0.086(6) 0.044(3) -0.013(4) 0.010(3) -0.002(4) C23 0.033(3) 0.044(3) 0.036(3) -0.015(2) 0.005(2) 0.000(2) C24 0.043(3) 0.077(4) 0.033(3) -0.014(3) 0.006(2) 0.013(3) C2S 0.092(5) 0.047(4) 0.057(4) -0.007(3) 0.024(4) 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 O3 1.953(3) . ? Zn1 O1 1.960(3) . ? Zn1 N2 2.025(4) . ? Zn1 N1 2.043(6) . ? Zn2 O7 1.957(3) . ? Zn2 O5 1.967(3) . ? Zn2 N3 2.023(4) . ? Zn2 N4 2.039(5) . ? O1 C7 1.275(6) . ? O2 C7 1.240(8) . ? O3 C10 1.284(6) . ? O4 C10 1.241(6) . ? O5 C19 1.268(7) . ? O6 C19 1.243(7) . ? O7 C22 1.281(5) . ? O8 C22 1.229(6) . ? O1S C1S 1.427(8) . ? O1S H1S 0.8400 . ? O2S C2S 1.404(8) . ? O2S H2S 0.8400 . ? N1 C1 1.474(6) . ? N1 H1N 0.9200 . ? N1 H2N 0.9200 . ? N2 C6 1.491(6) . ? N2 H3N 0.9200 . ? N2 H4N 0.9200 . ? N3 C13 1.473(7) . ? N3 H5N 0.9200 . ? N3 H6N 0.9200 . ? N4 C18 1.488(6) . ? N4 H7N 0.9200 . ? N4 H8N 0.9200 . ? C1 C2 1.517(9) . ? C1 C6 1.518(6) . ? C1 H1 1.0000 . ? C2 C3 1.527(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.520(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.512(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.530(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6 1.0000 . ? C7 C8 1.448(14) . ? C7 C8A 1.540(9) . ? C10 C11 1.505(7) . ? C11 C12 1.265(8) . ? C11 H11 0.9500 . ? C12 H12A 0.9500 . ? C12 H12B 0.9500 . ? C13 C14 1.521(6) . ? C13 C18 1.525(6) . ? C13 H13 1.0000 . ? C14 C15 1.529(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.523(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.529(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.519(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18 1.0000 . ? C19 C20 1.454(8) . ? C19 C20A 1.552(8) . ? C22 C23 1.491(7) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C23 C24 1.320(6) . ? C23 H23 0.9500 . ? C24 H24A 0.9500 . ? C24 H24B 0.9500 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C8 C9 1.27(2) . ? C8 H8 0.9500 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? C20 C21 1.309(16) . ? C20 H20 0.9500 . ? C21 H21A 0.9500 . ? C21 H21B 0.9500 . ? C8A C9A 1.316(18) . ? C8A H8A 0.9500 . ? C9A H9A1 0.9500 . ? C9A H9A2 0.9500 . ? C20A C21A 1.359(16) . ? C20A H20A 0.9500 . ? C21A H21C 0.9500 . ? C21A H21D 0.9500 . ? 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 97.83(16) . . ? O3 Zn1 N2 125.33(14) . . ? O1 Zn1 N2 116.40(15) . . ? O3 Zn1 N1 114.03(15) . . ? O1 Zn1 N1 117.14(15) . . ? N2 Zn1 N1 87.71(17) . . ? O7 Zn2 O5 97.48(15) . . ? O7 Zn2 N3 122.67(15) . . ? O5 Zn2 N3 119.84(16) . . ? O7 Zn2 N4 113.61(15) . . ? O5 Zn2 N4 117.08(15) . . ? N3 Zn2 N4 87.68(17) . . ? C7 O1 Zn1 116.1(4) . . ? C10 O3 Zn1 110.3(4) . . ? C19 O5 Zn2 114.0(4) . . ? C22 O7 Zn2 114.9(3) . . ? C1S O1S H1S 109.5 . . ? C2S O2S H2S 109.5 . . ? C1 N1 Zn1 105.3(3) . . ? C1 N1 H1N 110.7 . . ? Zn1 N1 H1N 110.7 . . ? C1 N1 H2N 110.7 . . ? Zn1 N1 H2N 110.7 . . ? H1N N1 H2N 108.8 . . ? C6 N2 Zn1 104.9(3) . . ? C6 N2 H3N 110.8 . . ? Zn1 N2 H3N 110.8 . . ? C6 N2 H4N 110.8 . . ? Zn1 N2 H4N 110.8 . . ? H3N N2 H4N 108.8 . . ? C13 N3 Zn2 105.5(3) . . ? C13 N3 H5N 110.6 . . ? Zn2 N3 H5N 110.6 . . ? C13 N3 H6N 110.6 . . ? Zn2 N3 H6N 110.6 . . ? H5N N3 H6N 108.8 . . ? C18 N4 Zn2 105.0(3) . . ? C18 N4 H7N 110.8 . . ? Zn2 N4 H7N 110.8 . . ? C18 N4 H8N 110.8 . . ? Zn2 N4 H8N 110.8 . . ? H7N N4 H8N 108.8 . . ? N1 C1 C2 113.1(5) . . ? N1 C1 C6 108.6(4) . . ? C2 C1 C6 111.6(4) . . ? N1 C1 H1 107.8 . . ? C2 C1 H1 107.8 . . ? C6 C1 H1 107.8 . . ? C1 C2 C3 112.7(5) . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C4 C3 C2 111.7(5) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 110.7(5) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 111.2(4) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N2 C6 C1 110.5(3) . . ? N2 C6 C5 112.6(4) . . ? C1 C6 C5 110.5(4) . . ? N2 C6 H6 107.7 . . ? C1 C6 H6 107.7 . . ? C5 C6 H6 107.7 . . ? O2 C7 O1 122.3(6) . . ? O2 C7 C8 107.4(8) . . ? O1 C7 C8 129.9(9) . . ? O2 C7 C8A 130.5(8) . . ? O1 C7 C8A 107.1(8) . . ? C8 C7 C8A 24.7(7) . . ? O4 C10 O3 123.5(5) . . ? O4 C10 C11 117.7(5) . . ? O3 C10 C11 118.8(5) . . ? C12 C11 C10 123.2(6) . . ? C12 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? C11 C12 H12A 120.0 . . ? C11 C12 H12B 120.0 . . ? H12A C12 H12B 120.0 . . ? N3 C13 C14 112.0(4) . . ? N3 C13 C18 109.8(4) . . ? C14 C13 C18 110.7(4) . . ? N3 C13 H13 108.1 . . ? C14 C13 H13 108.1 . . ? C18 C13 H13 108.1 . . ? C13 C14 C15 111.5(4) . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 110.6(5) . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C15 C16 C17 110.8(5) . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C18 C17 C16 111.3(5) . . ? C18 C17 H17A 109.4 . . ? C16 C17 H17A 109.4 . . ? C18 C17 H17B 109.4 . . ? C16 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N4 C18 C17 113.2(4) . . ? N4 C18 C13 108.6(4) . . ? C17 C18 C13 111.3(4) . . ? N4 C18 H18 107.8 . . ? C17 C18 H18 107.8 . . ? C13 C18 H18 107.8 . . ? O6 C19 O5 124.0(5) . . ? O6 C19 C20 110.1(7) . . ? O5 C19 C20 125.7(8) . . ? O6 C19 C20A 129.0(8) . . ? O5 C19 C20A 106.8(7) . . ? C20 C19 C20A 18.9(7) . . ? O8 C22 O7 123.6(5) . . ? O8 C22 C23 122.3(4) . . ? O7 C22 C23 114.0(5) . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C24 C23 C22 122.6(5) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C23 C24 H24A 120.0 . . ? C23 C24 H24B 120.0 . . ? H24A C24 H24B 120.0 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C9 C8 C7 116.0(13) . . ? C9 C8 H8 122.0 . . ? C7 C8 H8 122.0 . . ? C8 C9 H9A 120.0 . . ? C8 C9 H9B 120.0 . . ? H9A C9 H9B 120.0 . . ? C21 C20 C19 116.6(10) . . ? C21 C20 H20 121.7 . . ? C19 C20 H20 121.7 . . ? C20 C21 H21A 120.0 . . ? C20 C21 H21B 120.0 . . ? H21A C21 H21B 120.0 . . ? C9A C8A C7 122.5(13) . . ? C9A C8A H8A 118.7 . . ? C7 C8A H8A 118.7 . . ? C8A C9A H9A1 120.0 . . ? C8A C9A H9A2 120.0 . . ? H9A1 C9A H9A2 120.0 . . ? C21A C20A C19 118.6(12) . . ? C21A C20A H20A 120.7 . . ? C19 C20A H20A 120.7 . . ? C20A C21A H21C 120.0 . . ? C20A C21A H21D 120.0 . . ? H21C C21A H21D 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 O1 C7 -176.0(4) . . . . ? N2 Zn1 O1 C7 -39.9(5) . . . . ? N1 Zn1 O1 C7 61.8(4) . . . . ? O1 Zn1 O3 C10 172.2(3) . . . . ? N2 Zn1 O3 C10 41.9(4) . . . . ? N1 Zn1 O3 C10 -63.3(4) . . . . ? O7 Zn2 O5 C19 -173.2(4) . . . . ? N3 Zn2 O5 C19 52.1(4) . . . . ? N4 Zn2 O5 C19 -51.8(4) . . . . ? O5 Zn2 O7 C22 -175.4(3) . . . . ? N3 Zn2 O7 C22 -42.5(4) . . . . ? N4 Zn2 O7 C22 60.6(4) . . . . ? O3 Zn1 N1 C1 112.2(3) . . . . ? O1 Zn1 N1 C1 -134.5(3) . . . . ? N2 Zn1 N1 C1 -15.8(3) . . . . ? O3 Zn1 N2 C6 -130.2(3) . . . . ? O1 Zn1 N2 C6 107.2(3) . . . . ? N1 Zn1 N2 C6 -12.1(3) . . . . ? O7 Zn2 N3 C13 103.3(3) . . . . ? O5 Zn2 N3 C13 -133.6(3) . . . . ? N4 Zn2 N3 C13 -13.4(3) . . . . ? O7 Zn2 N4 C18 -139.8(2) . . . . ? O5 Zn2 N4 C18 107.7(3) . . . . ? N3 Zn2 N4 C18 -14.9(3) . . . . ? Zn1 N1 C1 C2 164.8(3) . . . . ? Zn1 N1 C1 C6 40.4(4) . . . . ? N1 C1 C2 C3 -175.3(4) . . . . ? C6 C1 C2 C3 -52.5(5) . . . . ? C1 C2 C3 C4 52.2(6) . . . . ? C2 C3 C4 C5 -54.4(6) . . . . ? C3 C4 C5 C6 57.5(6) . . . . ? Zn1 N2 C6 C1 38.2(4) . . . . ? Zn1 N2 C6 C5 162.3(3) . . . . ? N1 C1 C6 N2 -54.7(4) . . . . ? C2 C1 C6 N2 -179.9(4) . . . . ? N1 C1 C6 C5 -180.0(4) . . . . ? C2 C1 C6 C5 54.8(5) . . . . ? C4 C5 C6 N2 178.1(4) . . . . ? C4 C5 C6 C1 -57.8(5) . . . . ? Zn1 O1 C7 O2 -2.5(8) . . . . ? Zn1 O1 C7 C8 169.8(8) . . . . ? Zn1 O1 C7 C8A -179.0(6) . . . . ? Zn1 O3 C10 O4 -0.7(6) . . . . ? Zn1 O3 C10 C11 177.9(4) . . . . ? O4 C10 C11 C12 -179.0(6) . . . . ? O3 C10 C11 C12 2.3(9) . . . . ? Zn2 N3 C13 C14 162.7(3) . . . . ? Zn2 N3 C13 C18 39.3(4) . . . . ? N3 C13 C14 C15 -178.9(4) . . . . ? C18 C13 C14 C15 -55.9(6) . . . . ? C13 C14 C15 C16 56.5(6) . . . . ? C14 C15 C16 C17 -56.0(7) . . . . ? C15 C16 C17 C18 56.1(7) . . . . ? Zn2 N4 C18 C17 164.1(3) . . . . ? Zn2 N4 C18 C13 39.8(4) . . . . ? C16 C17 C18 N4 -178.5(4) . . . . ? C16 C17 C18 C13 -55.8(6) . . . . ? N3 C13 C18 N4 -55.0(5) . . . . ? C14 C13 C18 N4 -179.2(4) . . . . ? N3 C13 C18 C17 179.7(4) . . . . ? C14 C13 C18 C17 55.5(5) . . . . ? Zn2 O5 C19 O6 2.4(7) . . . . ? Zn2 O5 C19 C20 179.0(6) . . . . ? Zn2 O5 C19 C20A 179.1(6) . . . . ? Zn2 O7 C22 O8 8.1(6) . . . . ? Zn2 O7 C22 C23 -170.8(3) . . . . ? O8 C22 C23 C24 -5.7(8) . . . . ? O7 C22 C23 C24 173.3(5) . . . . ? O2 C7 C8 C9 174.4(10) . . . . ? O1 C7 C8 C9 1.2(16) . . . . ? C8A C7 C8 C9 -25.0(18) . . . . ? O6 C19 C20 C21 -175.9(8) . . . . ? O5 C19 C20 C21 7.1(13) . . . . ? C20A C19 C20 C21 7(2) . . . . ? O2 C7 C8A C9A 3.8(18) . . . . ? O1 C7 C8A C9A -180.0(12) . . . . ? C8 C7 C8A C9A -20.7(16) . . . . ? O6 C19 C20A C21A 12.6(15) . . . . ? O5 C19 C20A C21A -163.9(9) . . . . ? C20 C19 C20A C21A 15.8(18) . . . . ? _diffrn_measured_fraction_theta_max 0.854 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.493 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.089 #===END #-------------------------------------------------------------------- #-----------------------compound ZMS-------------------------------- #--------------------------------------------------------------- data_ds1 _database_code_depnum_ccdc_archive 'CCDC 282828' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H36 N2 O4 Zn' _chemical_formula_weight 469.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.1674(2) _cell_length_b 11.4910(2) _cell_length_c 14.8774(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.205(1) _cell_angle_gamma 90.00 _cell_volume 2226.07(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5374 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description cuboid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 1.135 _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 123(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 'Nonius Kappa CCD' _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_% 0 _diffrn_reflns_number 41630 _diffrn_reflns_av_R_equivalents 0.099 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.51 _reflns_number_total 10225 _reflns_number_gt 8384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect & Denzo' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SHELXS-97 _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^)+(0.0363P)^2^+2.4353P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.026(11) _refine_ls_number_reflns 10225 _refine_ls_number_parameters 546 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.28445(3) 0.11087(3) 0.06497(3) 0.02149(11) Uani 1 1 d . . . Zn2 Zn 0.23022(3) 0.66191(3) 0.44582(3) 0.02162(11) Uani 1 1 d . . . O1 O 0.2542(2) 0.2126(3) -0.0470(2) 0.0310(6) Uani 1 1 d . . . O2 O 0.3566(2) 0.1174(3) -0.1030(2) 0.0413(8) Uani 1 1 d . . . O3 O 0.1620(2) 0.0123(3) 0.0457(2) 0.0320(7) Uani 1 1 d . . . O4 O 0.1261(2) 0.1794(3) 0.0944(2) 0.0423(8) Uani 1 1 d . . . O5 O 0.3530(2) 0.5828(2) 0.4432(2) 0.0306(7) Uani 1 1 d . . . O6 O 0.3974(3) 0.7664(3) 0.4501(3) 0.0442(8) Uani 1 1 d . . . O7 O 0.2532(2) 0.7345(3) 0.56839(19) 0.0315(7) Uani 1 1 d . . . O8 O 0.1517(3) 0.6211(3) 0.6117(2) 0.0499(9) Uani 1 1 d . . . N1 N 0.3861(2) -0.0326(3) 0.1026(2) 0.0219(7) Uani 1 1 d . . . N2 N 0.3767(2) 0.1865(3) 0.1999(2) 0.0240(7) Uani 1 1 d . . . N3 N 0.1285(2) 0.5223(3) 0.3872(2) 0.0209(7) Uani 1 1 d . . . N4 N 0.1439(2) 0.7611(3) 0.3229(2) 0.0233(7) Uani 1 1 d . . . C1 C 0.3457(3) -0.1129(3) 0.0164(3) 0.0256(8) Uani 1 1 d . . . H1A H 0.3604 -0.0786 -0.0378 0.031 Uiso 1 1 calc R . . H1B H 0.2702 -0.1184 -0.0056 0.031 Uiso 1 1 calc R . . C2 C 0.3907(3) -0.2352(4) 0.0363(3) 0.0319(9) Uani 1 1 d . . . H2A H 0.4655 -0.2320 0.0526 0.038 Uiso 1 1 calc R . . H2B H 0.3584 -0.2840 -0.0228 0.038 Uiso 1 1 calc R . . C3 C 0.3712(3) -0.2886(4) 0.1215(3) 0.0358(10) Uani 1 1 d . . . H3A H 0.2964 -0.2958 0.1038 0.043 Uiso 1 1 calc R . . H3B H 0.4018 -0.3673 0.1358 0.043 Uiso 1 1 calc R . . C4 C 0.4183(3) -0.2122(4) 0.2106(3) 0.0316(10) Uani 1 1 d . . . H4A H 0.4938 -0.2104 0.2309 0.038 Uiso 1 1 calc R . . H4B H 0.4037 -0.2458 0.2651 0.038 Uiso 1 1 calc R . . C5 C 0.3762(3) -0.0868(3) 0.1909(3) 0.0251(9) Uani 1 1 d . . . H5 H 0.3012 -0.0909 0.1770 0.030 Uiso 1 1 calc R . . C6 C 0.4262(3) -0.0108(4) 0.2815(3) 0.0263(9) Uani 1 1 d . . . H6 H 0.4247 -0.0550 0.3388 0.032 Uiso 1 1 calc R . . C7 C 0.3714(3) 0.1057(4) 0.2765(3) 0.0275(8) Uani 1 1 d . . . H7A H 0.2983 0.0902 0.2632 0.033 Uiso 1 1 calc R . . H7B H 0.4024 0.1444 0.3410 0.033 Uiso 1 1 calc R . . C8 C 0.4868(3) 0.2002(3) 0.2111(3) 0.0254(9) Uani 1 1 d . . . H8 H 0.5249 0.2380 0.2759 0.030 Uiso 1 1 calc R . . C9 C 0.5380(3) 0.0823(4) 0.2131(3) 0.0265(10) Uani 1 1 d . . . H9 H 0.6112 0.0979 0.2243 0.032 Uiso 1 1 calc R . . C10 C 0.4925(3) 0.0068(4) 0.1214(3) 0.0245(9) Uani 1 1 d . . . H10A H 0.4916 0.0517 0.0644 0.029 Uiso 1 1 calc R . . H10B H 0.5368 -0.0622 0.1289 0.029 Uiso 1 1 calc R . . C11 C 0.5385(3) 0.0144(4) 0.3010(3) 0.0311(10) Uani 1 1 d . . . H11A H 0.5709 0.0607 0.3616 0.037 Uiso 1 1 calc R . . H11B H 0.5772 -0.0592 0.3085 0.037 Uiso 1 1 calc R . . C12 C 0.3370(3) 0.3017(4) 0.2149(3) 0.0294(10) Uani 1 1 d . . . H12A H 0.3791 0.3303 0.2815 0.035 Uiso 1 1 calc R . . H12B H 0.2655 0.2927 0.2096 0.035 Uiso 1 1 calc R . . C13 C 0.3395(3) 0.3904(4) 0.1403(3) 0.0315(9) Uani 1 1 d . . . H13A H 0.3167 0.4669 0.1550 0.038 Uiso 1 1 calc R . . H13B H 0.2912 0.3664 0.0743 0.038 Uiso 1 1 calc R . . C14 C 0.4466(3) 0.4020(4) 0.1413(4) 0.0359(10) Uani 1 1 d . . . H14A H 0.4921 0.4403 0.2027 0.043 Uiso 1 1 calc R . . H14B H 0.4440 0.4516 0.0859 0.043 Uiso 1 1 calc R . . C15 C 0.4907(3) 0.2832(4) 0.1333(3) 0.0289(9) Uani 1 1 d . . . H15A H 0.4511 0.2500 0.0677 0.035 Uiso 1 1 calc R . . H15B H 0.5628 0.2925 0.1405 0.035 Uiso 1 1 calc R . . C16 C 0.2971(3) 0.1972(4) -0.1079(3) 0.0282(9) Uani 1 1 d . . . C17 C 0.2710(3) 0.2860(4) -0.1888(3) 0.0294(9) Uani 1 1 d . . . C18 C 0.2323(3) 0.3979(4) -0.1754(4) 0.0416(12) Uani 1 1 d . . . H18A H 0.2169 0.4452 -0.2343 0.062 Uiso 1 1 calc R . . H18B H 0.2841 0.4374 -0.1192 0.062 Uiso 1 1 calc R . . H18C H 0.1695 0.3870 -0.1635 0.062 Uiso 1 1 calc R . . C19 C 0.2873(3) 0.2567(4) -0.2719(3) 0.0407(11) Uani 1 1 d . . . H19A H 0.2728 0.3116 -0.3234 0.049 Uiso 1 1 calc R . . H19B H 0.3129 0.1819 -0.2773 0.049 Uiso 1 1 calc R . . C20 C 0.1011(3) 0.0785(4) 0.0648(3) 0.0254(9) Uani 1 1 d . . . C21 C -0.0021(3) 0.0315(4) 0.0532(3) 0.0279(9) Uani 1 1 d . . . C22 C -0.0740(3) 0.1148(5) 0.0692(4) 0.0455(11) Uani 1 1 d . . . H22A H -0.1398 0.0760 0.0561 0.068 Uiso 1 1 calc R . . H22B H -0.0851 0.1813 0.0250 0.068 Uiso 1 1 calc R . . H22C H -0.0448 0.1420 0.1371 0.068 Uiso 1 1 calc R . . C23 C -0.0252(3) -0.0793(4) 0.0286(3) 0.0345(10) Uani 1 1 d . . . H23A H -0.0907 -0.1089 0.0204 0.041 Uiso 1 1 calc R . . H23B H 0.0238 -0.1289 0.0192 0.041 Uiso 1 1 calc R . . C24 C 0.1631(3) 0.4260(3) 0.4606(3) 0.0264(9) Uani 1 1 d . . . H24A H 0.1490 0.4489 0.5183 0.032 Uiso 1 1 calc R . . H24B H 0.2383 0.4171 0.4825 0.032 Uiso 1 1 calc R . . C25 C 0.1132(3) 0.3088(3) 0.4248(3) 0.0287(9) Uani 1 1 d . . . H25A H 0.0389 0.3134 0.4103 0.034 Uiso 1 1 calc R . . H25B H 0.1440 0.2495 0.4764 0.034 Uiso 1 1 calc R . . C26 C 0.1290(3) 0.2736(4) 0.3327(3) 0.0306(9) Uani 1 1 d . . . H26A H 0.2031 0.2608 0.3490 0.037 Uiso 1 1 calc R . . H26B H 0.0923 0.1998 0.3069 0.037 Uiso 1 1 calc R . . C27 C 0.0891(3) 0.3675(3) 0.2558(3) 0.0276(9) Uani 1 1 d . . . H27A H 0.0138 0.3747 0.2352 0.033 Uiso 1 1 calc R . . H27B H 0.1027 0.3450 0.1978 0.033 Uiso 1 1 calc R . . C28 C 0.1394(3) 0.4852(4) 0.2937(3) 0.0240(9) Uani 1 1 d . . . H28 H 0.2144 0.4770 0.3090 0.029 Uiso 1 1 calc R . . C29 C 0.0970(3) 0.5804(3) 0.2148(3) 0.0269(9) Uani 1 1 d . . . H29 H 0.1016 0.5502 0.1536 0.032 Uiso 1 1 calc R . . C30 C 0.1537(3) 0.6963(4) 0.2391(3) 0.0289(10) Uani 1 1 d . . . H30A H 0.2275 0.6819 0.2549 0.035 Uiso 1 1 calc R . . H30B H 0.1274 0.7464 0.1802 0.035 Uiso 1 1 calc R . . C31 C 0.0329(3) 0.7708(4) 0.3075(3) 0.0273(9) Uani 1 1 d . . . H31 H -0.0017 0.8189 0.2474 0.033 Uiso 1 1 calc R . . C32 C -0.0200(3) 0.6501(4) 0.2875(3) 0.0278(9) Uani 1 1 d . . . H32 H -0.0939 0.6630 0.2751 0.033 Uiso 1 1 calc R . . C33 C 0.0213(3) 0.5601(4) 0.3685(3) 0.0249(8) Uani 1 1 d . . . H33A H 0.0200 0.5932 0.4295 0.030 Uiso 1 1 calc R . . H33B H -0.0243 0.4912 0.3508 0.030 Uiso 1 1 calc R . . C34 C -0.0165(3) 0.6031(4) 0.1923(3) 0.0296(9) Uani 1 1 d . . . H34A H -0.0567 0.5302 0.1723 0.035 Uiso 1 1 calc R . . H34B H -0.0450 0.6609 0.1390 0.035 Uiso 1 1 calc R . . C35 C 0.1847(3) 0.8812(4) 0.3252(3) 0.0290(9) Uani 1 1 d . . . H35A H 0.1452 0.9205 0.2623 0.035 Uiso 1 1 calc R . . H35B H 0.2573 0.8767 0.3329 0.035 Uiso 1 1 calc R . . C36 C 0.1780(3) 0.9519(4) 0.4079(3) 0.0334(10) Uani 1 1 d . . . H36A H 0.2033 1.0317 0.4058 0.040 Uiso 1 1 calc R . . H36B H 0.2224 0.9164 0.4711 0.040 Uiso 1 1 calc R . . C37 C 0.0678(3) 0.9577(4) 0.4013(4) 0.0377(11) Uani 1 1 d . . . H37A H 0.0669 0.9958 0.4606 0.045 Uiso 1 1 calc R . . H37B H 0.0257 1.0051 0.3439 0.045 Uiso 1 1 calc R . . C38 C 0.0222(3) 0.8360(4) 0.3917(3) 0.0309(9) Uani 1 1 d . . . H38A H 0.0578 0.7924 0.4533 0.037 Uiso 1 1 calc R . . H38B H -0.0514 0.8417 0.3804 0.037 Uiso 1 1 calc R . . C39 C 0.4174(3) 0.6629(5) 0.4477(3) 0.0276(9) Uani 1 1 d . . . C40 C 0.5204(3) 0.6258(4) 0.4491(3) 0.0323(10) Uani 1 1 d . . . C41 C 0.5958(3) 0.7162(5) 0.4647(3) 0.0426(12) Uani 1 1 d . . . H41A H 0.6605 0.6816 0.4686 0.064 Uiso 1 1 calc R . . H41B H 0.6071 0.7571 0.5259 0.064 Uiso 1 1 calc R . . H41C H 0.5711 0.7714 0.4101 0.064 Uiso 1 1 calc R . . C42 C 0.5356(4) 0.5120(5) 0.4360(4) 0.0549(15) Uani 1 1 d . . . H42A H 0.5997 0.4868 0.4366 0.066 Uiso 1 1 calc R . . H42B H 0.4822 0.4573 0.4261 0.066 Uiso 1 1 calc R . . C43 C 0.2050(3) 0.7072(4) 0.6231(3) 0.0269(9) Uani 1 1 d . . . C44 C 0.2152(3) 0.7924(4) 0.7032(3) 0.0289(9) Uani 1 1 d . . . C45 C 0.1783(3) 0.7556(4) 0.7745(3) 0.0396(11) Uani 1 1 d . . . H45A H 0.1831 0.8202 0.8191 0.059 Uiso 1 1 calc R . . H45B H 0.2198 0.6902 0.8117 0.059 Uiso 1 1 calc R . . H45C H 0.1065 0.7311 0.7420 0.059 Uiso 1 1 calc R . . C46 C 0.2583(4) 0.9028(4) 0.7038(4) 0.0439(12) Uani 1 1 d . . . H46A H 0.2639 0.9571 0.7538 0.053 Uiso 1 1 calc R . . H46B H 0.2819 0.9230 0.6543 0.053 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 0.0229(2) 0.0215(2) 0.0198(2) 0.0002(2) 0.00809(17) -0.00007(19) Zn2 0.0219(2) 0.0237(2) 0.0190(2) 0.0012(2) 0.00773(17) 0.00078(19) O1 0.0318(15) 0.0364(16) 0.0253(15) 0.0060(13) 0.0116(12) -0.0017(13) O2 0.0517(18) 0.0400(18) 0.0358(17) 0.0075(16) 0.0209(14) 0.0119(18) O3 0.0218(14) 0.0335(17) 0.0397(18) 0.0050(14) 0.0110(13) 0.0038(13) O4 0.0423(17) 0.036(2) 0.049(2) -0.0119(16) 0.0179(14) -0.0109(15) O5 0.0223(13) 0.0344(18) 0.0329(16) -0.0047(13) 0.0086(12) 0.0003(12) O6 0.045(2) 0.035(2) 0.052(2) 0.0109(17) 0.0189(17) 0.0047(16) O7 0.0343(15) 0.0417(18) 0.0205(15) -0.0036(13) 0.0129(12) -0.0013(13) O8 0.067(2) 0.049(2) 0.0447(19) -0.0204(18) 0.0338(17) -0.026(2) N1 0.0251(16) 0.0216(17) 0.0195(17) -0.0010(13) 0.0094(13) 0.0018(13) N2 0.0224(15) 0.027(2) 0.0239(17) -0.0008(14) 0.0104(13) -0.0002(13) N3 0.0208(15) 0.0216(17) 0.0179(16) -0.0012(13) 0.0050(13) 0.0011(13) N4 0.0222(16) 0.0246(18) 0.0236(17) 0.0030(14) 0.0095(13) 0.0054(13) C1 0.029(2) 0.026(2) 0.022(2) -0.0038(17) 0.0109(16) 0.0006(17) C2 0.040(2) 0.026(2) 0.033(2) -0.0071(19) 0.0176(19) 0.0012(19) C3 0.041(2) 0.021(2) 0.051(3) 0.003(2) 0.024(2) 0.0038(19) C4 0.034(2) 0.031(2) 0.032(2) 0.0094(19) 0.0153(19) 0.0017(18) C5 0.023(2) 0.029(2) 0.025(2) 0.0051(17) 0.0109(17) 0.0050(17) C6 0.029(2) 0.031(2) 0.017(2) 0.0029(16) 0.0075(16) 0.0019(17) C7 0.0318(19) 0.034(2) 0.0177(18) -0.001(2) 0.0110(15) -0.001(2) C8 0.0228(19) 0.027(2) 0.028(2) -0.0041(17) 0.0128(16) -0.0044(16) C9 0.0197(18) 0.032(3) 0.029(2) -0.0003(17) 0.0110(16) -0.0009(16) C10 0.0223(19) 0.025(2) 0.024(2) 0.0021(17) 0.0078(16) 0.0030(16) C11 0.028(2) 0.037(2) 0.023(2) 0.0032(18) 0.0035(17) 0.0028(18) C12 0.028(2) 0.026(2) 0.038(3) -0.0097(18) 0.0169(19) -0.0025(17) C13 0.034(2) 0.022(2) 0.041(3) -0.0003(19) 0.017(2) 0.0017(18) C14 0.041(2) 0.029(2) 0.041(3) -0.002(2) 0.019(2) -0.008(2) C15 0.024(2) 0.032(2) 0.034(2) -0.0002(19) 0.0149(18) 0.0006(17) C16 0.027(2) 0.032(2) 0.021(2) 0.0009(16) 0.0042(16) -0.0040(17) C17 0.028(2) 0.033(2) 0.025(2) 0.0046(18) 0.0072(17) -0.0070(18) C18 0.035(2) 0.038(3) 0.044(3) 0.012(2) 0.008(2) -0.004(2) C19 0.040(3) 0.047(3) 0.035(3) 0.018(2) 0.015(2) -0.001(2) C20 0.0242(19) 0.030(2) 0.020(2) 0.0033(17) 0.0066(16) -0.0012(17) C21 0.0225(19) 0.037(2) 0.022(2) 0.0043(18) 0.0059(16) 0.0007(17) C22 0.035(2) 0.049(3) 0.059(3) -0.012(3) 0.024(2) -0.004(2) C23 0.028(2) 0.036(3) 0.035(2) -0.001(2) 0.0073(18) -0.0076(18) C24 0.028(2) 0.028(2) 0.021(2) 0.0012(17) 0.0083(16) 0.0035(17) C25 0.031(2) 0.025(2) 0.029(2) 0.0034(17) 0.0109(18) -0.0001(17) C26 0.027(2) 0.027(2) 0.033(2) -0.0031(18) 0.0063(18) 0.0028(18) C27 0.028(2) 0.030(2) 0.023(2) -0.0037(17) 0.0075(17) 0.0049(17) C28 0.022(2) 0.029(2) 0.019(2) -0.0019(17) 0.0064(16) 0.0047(17) C29 0.029(2) 0.033(2) 0.0187(19) -0.0014(16) 0.0095(16) 0.0045(17) C30 0.028(2) 0.039(3) 0.020(2) 0.0054(17) 0.0096(16) 0.0016(18) C31 0.0221(19) 0.033(2) 0.025(2) 0.0017(18) 0.0073(16) 0.0058(17) C32 0.0183(16) 0.033(3) 0.028(2) -0.0011(19) 0.0054(15) 0.0043(17) C33 0.0201(18) 0.023(2) 0.033(2) -0.0007(18) 0.0122(17) -0.0010(16) C34 0.0270(19) 0.030(2) 0.025(2) 0.000(2) 0.0031(15) 0.004(2) C35 0.028(2) 0.027(2) 0.031(2) 0.0094(18) 0.0113(18) 0.0038(18) C36 0.034(2) 0.021(2) 0.041(3) 0.0046(19) 0.011(2) 0.0008(18) C37 0.036(2) 0.033(3) 0.045(3) -0.002(2) 0.017(2) 0.006(2) C38 0.027(2) 0.031(2) 0.036(2) 0.000(2) 0.0141(19) 0.0044(18) C39 0.0247(18) 0.042(3) 0.0174(18) 0.004(2) 0.0098(14) 0.002(2) C40 0.0227(18) 0.056(3) 0.0169(18) 0.0028(19) 0.0061(14) 0.0055(19) C41 0.028(2) 0.066(3) 0.030(2) 0.010(2) 0.0075(19) -0.011(2) C42 0.028(2) 0.064(4) 0.069(4) -0.019(3) 0.016(2) 0.007(2) C43 0.026(2) 0.029(2) 0.022(2) -0.0030(17) 0.0052(16) -0.0004(18) C44 0.025(2) 0.035(2) 0.023(2) -0.0034(18) 0.0062(17) 0.0029(18) C45 0.035(2) 0.054(3) 0.026(2) -0.009(2) 0.0071(19) 0.006(2) C46 0.049(3) 0.042(3) 0.039(3) -0.017(2) 0.015(2) -0.003(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 O1 1.939(3) . ? Zn1 O3 1.996(3) . ? Zn1 N2 2.104(3) . ? Zn1 N1 2.114(3) . ? Zn2 O7 1.913(3) . ? Zn2 O5 1.977(3) . ? Zn2 N4 2.092(3) . ? Zn2 N3 2.102(3) . ? O1 C16 1.288(5) . ? O2 C16 1.228(5) . ? O3 C20 1.264(5) . ? O4 C20 1.241(5) . ? O5 C39 1.280(5) . ? O6 C39 1.226(6) . ? O7 C43 1.291(5) . ? O8 C43 1.216(5) . ? N1 C10 1.491(5) . ? N1 C1 1.498(5) . ? N1 C5 1.509(5) . ? N2 C12 1.489(5) . ? N2 C7 1.495(5) . ? N2 C8 1.509(5) . ? N3 C24 1.496(5) . ? N3 C33 1.497(4) . ? N3 C28 1.519(5) . ? N4 C35 1.491(5) . ? N4 C31 1.502(5) . ? N4 C30 1.506(5) . ? C1 C2 1.524(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.527(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.509(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.543(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.526(6) . ? C5 H5 1.0000 . ? C6 C11 1.528(5) . ? C6 C7 1.534(6) . ? C6 H6 1.0000 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C15 1.518(6) . ? C8 C9 1.532(5) . ? C8 H8 1.0000 . ? C9 C11 1.521(6) . ? C9 C10 1.528(5) . ? C9 H9 1.0000 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.517(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.518(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.525(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.508(6) . ? C17 C19 1.385(6) . ? C17 C18 1.442(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9500 . ? C19 H19B 0.9500 . ? C20 C21 1.503(5) . ? C21 C23 1.330(6) . ? C21 C22 1.485(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9500 . ? C23 H23B 0.9500 . ? C24 C25 1.516(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.527(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.511(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.529(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.543(6) . ? C28 H28 1.0000 . ? C29 C30 1.524(6) . ? C29 C34 1.529(5) . ? C29 H29 1.0000 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C38 1.517(6) . ? C31 C32 1.549(6) . ? C31 H31 1.0000 . ? C32 C33 1.520(6) . ? C32 C34 1.535(6) . ? C32 H32 1.0000 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.509(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.526(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.524(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.513(5) . ? C40 C42 1.351(7) . ? C40 C41 1.442(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9500 . ? C42 H42B 0.9500 . ? C43 C44 1.504(5) . ? C44 C46 1.406(6) . ? C44 C45 1.421(6) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9500 . ? C46 H46B 0.9500 . ? 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 O3 109.47(12) . . ? O1 Zn1 N2 114.48(12) . . ? O3 Zn1 N2 123.36(12) . . ? O1 Zn1 N1 126.47(12) . . ? O3 Zn1 N1 93.32(12) . . ? N2 Zn1 N1 88.11(12) . . ? O7 Zn2 O5 113.51(12) . . ? O7 Zn2 N4 114.63(13) . . ? O5 Zn2 N4 116.69(12) . . ? O7 Zn2 N3 124.06(12) . . ? O5 Zn2 N3 96.03(12) . . ? N4 Zn2 N3 89.09(12) . . ? C16 O1 Zn1 121.1(3) . . ? C20 O3 Zn1 104.9(3) . . ? C39 O5 Zn2 106.4(3) . . ? C43 O7 Zn2 124.2(3) . . ? C10 N1 C1 111.4(3) . . ? C10 N1 C5 113.3(3) . . ? C1 N1 C5 110.9(3) . . ? C10 N1 Zn1 110.2(2) . . ? C1 N1 Zn1 105.3(2) . . ? C5 N1 Zn1 105.4(2) . . ? C12 N2 C7 107.6(3) . . ? C12 N2 C8 109.0(3) . . ? C7 N2 C8 109.9(3) . . ? C12 N2 Zn1 112.4(2) . . ? C7 N2 Zn1 105.7(2) . . ? C8 N2 Zn1 112.0(2) . . ? C24 N3 C33 111.5(3) . . ? C24 N3 C28 109.8(3) . . ? C33 N3 C28 111.9(3) . . ? C24 N3 Zn2 106.8(2) . . ? C33 N3 Zn2 109.6(2) . . ? C28 N3 Zn2 107.1(2) . . ? C35 N4 C31 108.0(3) . . ? C35 N4 C30 108.4(3) . . ? C31 N4 C30 110.1(3) . . ? C35 N4 Zn2 113.4(2) . . ? C31 N4 Zn2 113.0(2) . . ? C30 N4 Zn2 104.0(2) . . ? N1 C1 C2 114.4(3) . . ? N1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C1 C2 C3 109.5(3) . . ? C1 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 . . ? C1 C2 H2B 109.8 . . ? C3 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 109.5(4) . . ? C4 C3 H3A 109.8 . . ? C2 C3 H3A 109.8 . . ? C4 C3 H3B 109.8 . . ? C2 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C3 C4 C5 111.8(3) . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N1 C5 C6 111.3(3) . . ? N1 C5 C4 112.9(3) . . ? C6 C5 C4 110.9(3) . . ? N1 C5 H5 107.2 . . ? C6 C5 H5 107.2 . . ? C4 C5 H5 107.2 . . ? C5 C6 C11 111.3(3) . . ? C5 C6 C7 114.0(3) . . ? C11 C6 C7 108.3(3) . . ? C5 C6 H6 107.7 . . ? C11 C6 H6 107.7 . . ? C7 C6 H6 107.7 . . ? N2 C7 C6 113.7(3) . . ? N2 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? N2 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N2 C8 C15 109.1(3) . . ? N2 C8 C9 111.8(3) . . ? C15 C8 C9 114.3(3) . . ? N2 C8 H8 107.1 . . ? C15 C8 H8 107.1 . . ? C9 C8 H8 107.1 . . ? C11 C9 C10 109.5(3) . . ? C11 C9 C8 108.2(3) . . ? C10 C9 C8 117.0(3) . . ? C11 C9 H9 107.2 . . ? C10 C9 H9 107.2 . . ? C8 C9 H9 107.2 . . ? N1 C10 C9 112.3(3) . . ? N1 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? N1 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? C9 C11 C6 106.3(3) . . ? C9 C11 H11A 110.5 . . ? C6 C11 H11A 110.5 . . ? C9 C11 H11B 110.5 . . ? C6 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? N2 C12 C13 111.6(3) . . ? N2 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? N2 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C12 C13 C14 111.3(4) . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C13 C14 C15 111.1(4) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C8 C15 C14 111.3(3) . . ? C8 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? C8 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? O2 C16 O1 124.4(4) . . ? O2 C16 C17 119.9(4) . . ? O1 C16 C17 115.7(4) . . ? C19 C17 C18 123.1(4) . . ? C19 C17 C16 118.2(4) . . ? C18 C17 C16 118.7(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 120.0 . . ? C17 C19 H19B 120.0 . . ? H19A C19 H19B 120.0 . . ? O4 C20 O3 121.2(4) . . ? O4 C20 C21 120.4(4) . . ? O3 C20 C21 118.5(4) . . ? C23 C21 C22 123.4(4) . . ? C23 C21 C20 119.9(4) . . ? C22 C21 C20 116.6(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 120.0 . . ? C21 C23 H23B 120.0 . . ? H23A C23 H23B 120.0 . . ? N3 C24 C25 115.3(3) . . ? N3 C24 H24A 108.4 . . ? C25 C24 H24A 108.4 . . ? N3 C24 H24B 108.4 . . ? C25 C24 H24B 108.4 . . ? H24A C24 H24B 107.5 . . ? C24 C25 C26 109.7(3) . . ? C24 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? C24 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C27 C26 C25 110.3(3) . . ? C27 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? C27 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C26 C27 C28 111.8(3) . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? N3 C28 C27 112.6(3) . . ? N3 C28 C29 110.3(3) . . ? C27 C28 C29 111.2(3) . . ? N3 C28 H28 107.5 . . ? C27 C28 H28 107.5 . . ? C29 C28 H28 107.5 . . ? C30 C29 C34 108.3(3) . . ? C30 C29 C28 115.4(3) . . ? C34 C29 C28 110.4(3) . . ? C30 C29 H29 107.5 . . ? C34 C29 H29 107.5 . . ? C28 C29 H29 107.5 . . ? N4 C30 C29 114.6(3) . . ? N4 C30 H30A 108.6 . . ? C29 C30 H30A 108.6 . . ? N4 C30 H30B 108.6 . . ? C29 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? N4 C31 C38 110.5(3) . . ? N4 C31 C32 111.2(3) . . ? C38 C31 C32 113.7(3) . . ? N4 C31 H31 107.0 . . ? C38 C31 H31 107.0 . . ? C32 C31 H31 107.0 . . ? C33 C32 C34 110.5(4) . . ? C33 C32 C31 116.8(3) . . ? C34 C32 C31 107.7(3) . . ? C33 C32 H32 107.1 . . ? C34 C32 H32 107.1 . . ? C31 C32 H32 107.1 . . ? N3 C33 C32 112.9(3) . . ? N3 C33 H33A 109.0 . . ? C32 C33 H33A 109.0 . . ? N3 C33 H33B 109.0 . . ? C32 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C29 C34 C32 105.7(3) . . ? C29 C34 H34A 110.6 . . ? C32 C34 H34A 110.6 . . ? C29 C34 H34B 110.6 . . ? C32 C34 H34B 110.6 . . ? H34A C34 H34B 108.7 . . ? N4 C35 C36 111.6(3) . . ? N4 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? N4 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C37 111.3(4) . . ? C35 C36 H36A 109.4 . . ? C37 C36 H36A 109.4 . . ? C35 C36 H36B 109.4 . . ? C37 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C38 C37 C36 110.5(4) . . ? C38 C37 H37A 109.5 . . ? C36 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C31 C38 C37 110.7(4) . . ? C31 C38 H38A 109.5 . . ? C37 C38 H38A 109.5 . . ? C31 C38 H38B 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? O6 C39 O5 122.0(4) . . ? O6 C39 C40 120.4(4) . . ? O5 C39 C40 117.5(4) . . ? C42 C40 C41 124.8(4) . . ? C42 C40 C39 118.6(4) . . ? C41 C40 C39 116.7(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 120.0 . . ? C40 C42 H42B 120.0 . . ? H42A C42 H42B 120.0 . . ? O8 C43 O7 124.3(4) . . ? O8 C43 C44 120.1(4) . . ? O7 C43 C44 115.5(4) . . ? C46 C44 C45 123.4(4) . . ? C46 C44 C43 119.9(4) . . ? C45 C44 C43 116.7(4) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 120.0 . . ? C44 C46 H46B 120.0 . . ? H46A C46 H46B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 O1 C16 -109.8(3) . . . . ? N2 Zn1 O1 C16 106.9(3) . . . . ? N1 Zn1 O1 C16 0.0(3) . . . . ? O1 Zn1 O3 C20 -77.6(3) . . . . ? N2 Zn1 O3 C20 61.7(3) . . . . ? N1 Zn1 O3 C20 151.7(3) . . . . ? O7 Zn2 O5 C39 -68.2(3) . . . . ? N4 Zn2 O5 C39 68.5(3) . . . . ? N3 Zn2 O5 C39 160.5(2) . . . . ? O5 Zn2 O7 C43 -118.8(3) . . . . ? N4 Zn2 O7 C43 103.6(3) . . . . ? N3 Zn2 O7 C43 -3.1(4) . . . . ? O1 Zn1 N1 C10 61.3(3) . . . . ? O3 Zn1 N1 C10 178.6(2) . . . . ? N2 Zn1 N1 C10 -58.1(2) . . . . ? O1 Zn1 N1 C1 -58.9(3) . . . . ? O3 Zn1 N1 C1 58.4(2) . . . . ? N2 Zn1 N1 C1 -178.3(2) . . . . ? O1 Zn1 N1 C5 -176.1(2) . . . . ? O3 Zn1 N1 C5 -58.9(2) . . . . ? N2 Zn1 N1 C5 64.5(2) . . . . ? O1 Zn1 N2 C12 50.7(3) . . . . ? O3 Zn1 N2 C12 -86.9(3) . . . . ? N1 Zn1 N2 C12 -179.7(3) . . . . ? O1 Zn1 N2 C7 167.8(2) . . . . ? O3 Zn1 N2 C7 30.2(3) . . . . ? N1 Zn1 N2 C7 -62.5(2) . . . . ? O1 Zn1 N2 C8 -72.5(3) . . . . ? O3 Zn1 N2 C8 149.9(2) . . . . ? N1 Zn1 N2 C8 57.2(2) . . . . ? O7 Zn2 N3 C24 -58.2(3) . . . . ? O5 Zn2 N3 C24 65.6(2) . . . . ? N4 Zn2 N3 C24 -177.7(2) . . . . ? O7 Zn2 N3 C33 62.7(3) . . . . ? O5 Zn2 N3 C33 -173.6(2) . . . . ? N4 Zn2 N3 C33 -56.8(2) . . . . ? O7 Zn2 N3 C28 -175.7(2) . . . . ? O5 Zn2 N3 C28 -52.0(2) . . . . ? N4 Zn2 N3 C28 64.8(2) . . . . ? O7 Zn2 N4 C35 52.4(3) . . . . ? O5 Zn2 N4 C35 -83.8(3) . . . . ? N3 Zn2 N4 C35 179.9(3) . . . . ? O7 Zn2 N4 C31 -70.8(3) . . . . ? O5 Zn2 N4 C31 153.0(2) . . . . ? N3 Zn2 N4 C31 56.7(3) . . . . ? O7 Zn2 N4 C30 169.8(2) . . . . ? O5 Zn2 N4 C30 33.7(3) . . . . ? N3 Zn2 N4 C30 -62.6(2) . . . . ? C10 N1 C1 C2 74.9(4) . . . . ? C5 N1 C1 C2 -52.2(4) . . . . ? Zn1 N1 C1 C2 -165.7(3) . . . . ? N1 C1 C2 C3 57.0(5) . . . . ? C1 C2 C3 C4 -58.0(5) . . . . ? C2 C3 C4 C5 57.2(5) . . . . ? C10 N1 C5 C6 48.6(4) . . . . ? C1 N1 C5 C6 174.6(3) . . . . ? Zn1 N1 C5 C6 -72.0(3) . . . . ? C10 N1 C5 C4 -76.8(4) . . . . ? C1 N1 C5 C4 49.2(4) . . . . ? Zn1 N1 C5 C4 162.6(3) . . . . ? C3 C4 C5 N1 -53.4(4) . . . . ? C3 C4 C5 C6 -179.1(3) . . . . ? N1 C5 C6 C11 -55.6(4) . . . . ? C4 C5 C6 C11 70.9(4) . . . . ? N1 C5 C6 C7 67.2(4) . . . . ? C4 C5 C6 C7 -166.3(3) . . . . ? C12 N2 C7 C6 -170.4(3) . . . . ? C8 N2 C7 C6 -51.7(4) . . . . ? Zn1 N2 C7 C6 69.4(3) . . . . ? C5 C6 C7 N2 -66.4(4) . . . . ? C11 C6 C7 N2 58.0(4) . . . . ? C12 N2 C8 C15 -61.8(4) . . . . ? C7 N2 C8 C15 -179.6(3) . . . . ? Zn1 N2 C8 C15 63.2(3) . . . . ? C12 N2 C8 C9 170.8(3) . . . . ? C7 N2 C8 C9 53.0(4) . . . . ? Zn1 N2 C8 C9 -64.2(3) . . . . ? N2 C8 C9 C11 -61.6(4) . . . . ? C15 C8 C9 C11 173.8(3) . . . . ? N2 C8 C9 C10 62.6(4) . . . . ? C15 C8 C9 C10 -62.0(4) . . . . ? C1 N1 C10 C9 -176.2(3) . . . . ? C5 N1 C10 C9 -50.4(4) . . . . ? Zn1 N1 C10 C9 67.4(3) . . . . ? C11 C9 C10 N1 58.2(4) . . . . ? C8 C9 C10 N1 -65.3(4) . . . . ? C10 C9 C11 C6 -62.9(4) . . . . ? C8 C9 C11 C6 65.8(4) . . . . ? C5 C6 C11 C9 62.6(4) . . . . ? C7 C6 C11 C9 -63.4(4) . . . . ? C7 N2 C12 C13 179.9(3) . . . . ? C8 N2 C12 C13 60.7(4) . . . . ? Zn1 N2 C12 C13 -64.1(4) . . . . ? N2 C12 C13 C14 -55.5(5) . . . . ? C12 C13 C14 C15 51.0(5) . . . . ? N2 C8 C15 C14 58.9(4) . . . . ? C9 C8 C15 C14 -175.1(3) . . . . ? C13 C14 C15 C8 -53.6(5) . . . . ? Zn1 O1 C16 O2 2.3(5) . . . . ? Zn1 O1 C16 C17 -177.0(2) . . . . ? O2 C16 C17 C19 20.3(6) . . . . ? O1 C16 C17 C19 -160.4(4) . . . . ? O2 C16 C17 C18 -158.5(4) . . . . ? O1 C16 C17 C18 20.9(5) . . . . ? Zn1 O3 C20 O4 -3.9(5) . . . . ? Zn1 O3 C20 C21 177.6(3) . . . . ? O4 C20 C21 C23 -174.9(4) . . . . ? O3 C20 C21 C23 3.7(6) . . . . ? O4 C20 C21 C22 5.9(6) . . . . ? O3 C20 C21 C22 -175.6(4) . . . . ? C33 N3 C24 C25 71.9(4) . . . . ? C28 N3 C24 C25 -52.8(4) . . . . ? Zn2 N3 C24 C25 -168.5(3) . . . . ? N3 C24 C25 C26 55.5(4) . . . . ? C24 C25 C26 C27 -55.4(4) . . . . ? C25 C26 C27 C28 56.4(4) . . . . ? C24 N3 C28 C27 51.1(4) . . . . ? C33 N3 C28 C27 -73.2(4) . . . . ? Zn2 N3 C28 C27 166.7(2) . . . . ? C24 N3 C28 C29 176.0(3) . . . . ? C33 N3 C28 C29 51.7(4) . . . . ? Zn2 N3 C28 C29 -68.4(3) . . . . ? C26 C27 C28 N3 -54.9(4) . . . . ? C26 C27 C28 C29 -179.3(3) . . . . ? N3 C28 C29 C30 63.6(4) . . . . ? C27 C28 C29 C30 -170.7(3) . . . . ? N3 C28 C29 C34 -59.6(4) . . . . ? C27 C28 C29 C34 66.2(4) . . . . ? C35 N4 C30 C29 -168.8(3) . . . . ? C31 N4 C30 C29 -51.0(4) . . . . ? Zn2 N4 C30 C29 70.3(3) . . . . ? C34 C29 C30 N4 57.3(4) . . . . ? C28 C29 C30 N4 -66.9(4) . . . . ? C35 N4 C31 C38 -61.9(4) . . . . ? C30 N4 C31 C38 179.9(3) . . . . ? Zn2 N4 C31 C38 64.2(4) . . . . ? C35 N4 C31 C32 170.8(3) . . . . ? C30 N4 C31 C32 52.7(4) . . . . ? Zn2 N4 C31 C32 -63.1(4) . . . . ? N4 C31 C32 C33 62.3(4) . . . . ? C38 C31 C32 C33 -63.2(4) . . . . ? N4 C31 C32 C34 -62.7(4) . . . . ? C38 C31 C32 C34 171.8(3) . . . . ? C24 N3 C33 C32 -174.7(3) . . . . ? C28 N3 C33 C32 -51.3(4) . . . . ? Zn2 N3 C33 C32 67.4(4) . . . . ? C34 C32 C33 N3 57.2(4) . . . . ? C31 C32 C33 N3 -66.3(5) . . . . ? C30 C29 C34 C32 -63.6(4) . . . . ? C28 C29 C34 C32 63.5(4) . . . . ? C33 C32 C34 C29 -61.7(4) . . . . ? C31 C32 C34 C29 67.0(4) . . . . ? C31 N4 C35 C36 61.0(4) . . . . ? C30 N4 C35 C36 -179.8(3) . . . . ? Zn2 N4 C35 C36 -64.9(4) . . . . ? N4 C35 C36 C37 -57.0(4) . . . . ? C35 C36 C37 C38 52.0(5) . . . . ? N4 C31 C38 C37 59.1(4) . . . . ? C32 C31 C38 C37 -175.1(3) . . . . ? C36 C37 C38 C31 -53.2(5) . . . . ? Zn2 O5 C39 O6 -1.8(5) . . . . ? Zn2 O5 C39 C40 178.7(3) . . . . ? O6 C39 C40 C42 -173.1(4) . . . . ? O5 C39 C40 C42 6.4(6) . . . . ? O6 C39 C40 C41 6.9(6) . . . . ? O5 C39 C40 C41 -173.6(3) . . . . ? Zn2 O7 C43 O8 12.2(6) . . . . ? Zn2 O7 C43 C44 -165.8(2) . . . . ? O8 C43 C44 C46 -166.6(4) . . . . ? O7 C43 C44 C46 11.4(6) . . . . ? O8 C43 C44 C45 12.5(6) . . . . ? O7 C43 C44 C45 -169.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.616 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.076 #===END #---------------------------------------------------------------- #--------------compound ZAS------------------------------------ #---------------------------------------------------------------- data_0703 _database_code_depnum_ccdc_archive 'CCDC 282829' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H32 N2 O4 Zn' _chemical_formula_weight 441.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.7634(6) _cell_length_b 10.9958(9) _cell_length_c 24.578(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2098.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 140298 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22025 _diffrn_reflns_av_R_equivalents 0.0863 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.36 _reflns_number_total 4682 _reflns_number_gt 3796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect & Denzo' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR _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^)+(0.0183P)^2^+1.6114P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(14) _refine_ls_number_reflns 4682 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 0.67925(5) 0.09164(3) 0.641920(15) 0.02548(10) Uani 1 1 d . . . O1 O 0.8320(3) 0.1736(2) 0.69488(9) 0.0315(5) Uani 1 1 d . . . O2 O 0.7637(3) 0.0144(2) 0.74578(11) 0.0422(7) Uani 1 1 d . . . O3 O 0.8092(3) -0.0346(2) 0.60526(10) 0.0345(6) Uani 1 1 d . . . O4 O 0.7832(4) 0.0482(2) 0.52269(12) 0.0538(9) Uani 1 1 d . . . N1 N 0.5907(4) 0.2527(3) 0.60527(11) 0.0242(6) Uani 1 1 d . . . N2 N 0.4255(4) 0.0525(2) 0.66465(11) 0.0254(7) Uani 1 1 d . . . C1 C 0.7477(4) 0.3099(3) 0.58132(15) 0.0301(8) Uani 1 1 d . . . H1A H 0.7845 0.2611 0.5495 0.036 Uiso 1 1 calc R . . H1B H 0.8415 0.3066 0.6086 0.036 Uiso 1 1 calc R . . C2 C 0.7244(5) 0.4422(3) 0.56315(14) 0.0337(9) Uani 1 1 d . . . H2A H 0.8355 0.4747 0.5498 0.040 Uiso 1 1 calc R . . H2B H 0.6401 0.4460 0.5330 0.040 Uiso 1 1 calc R . . C3 C 0.6610(5) 0.5185(3) 0.61059(15) 0.0360(9) Uani 1 1 d . . . H3A H 0.6403 0.6030 0.5984 0.043 Uiso 1 1 calc R . . H3B H 0.7494 0.5202 0.6396 0.043 Uiso 1 1 calc R . . C4 C 0.4939(5) 0.4641(3) 0.63286(16) 0.0350(9) Uani 1 1 d . . . H4A H 0.4549 0.5124 0.6645 0.042 Uiso 1 1 calc R . . H4B H 0.4033 0.4686 0.6046 0.042 Uiso 1 1 calc R . . C5 C 0.5185(4) 0.3318(3) 0.65008(14) 0.0274(8) Uani 1 1 d . . . H5 H 0.6042 0.3314 0.6805 0.033 Uiso 1 1 calc R . . C6 C 0.3505(4) 0.2768(3) 0.67252(14) 0.0307(8) Uani 1 1 d . . . H6 H 0.3019 0.3355 0.6996 0.037 Uiso 1 1 calc R . . C7 C 0.2181(4) 0.2609(3) 0.62738(14) 0.0340(9) Uani 1 1 d . . . H7A H 0.1958 0.3396 0.6091 0.041 Uiso 1 1 calc R . . H7B H 0.1082 0.2300 0.6425 0.041 Uiso 1 1 calc R . . C8 C 0.2936(4) 0.1695(3) 0.58713(14) 0.0292(8) Uani 1 1 d . . . H8 H 0.2086 0.1600 0.5569 0.035 Uiso 1 1 calc R . . C9 C 0.4591(4) 0.2227(3) 0.56242(13) 0.0277(8) Uani 1 1 d . . . H9A H 0.5089 0.1633 0.5366 0.033 Uiso 1 1 calc R . . H9B H 0.4304 0.2974 0.5418 0.033 Uiso 1 1 calc R . . C10 C 0.3733(4) 0.1544(3) 0.70133(14) 0.0298(8) Uani 1 1 d . . . H10A H 0.4615 0.1637 0.7301 0.036 Uiso 1 1 calc R . . H10B H 0.2634 0.1325 0.7193 0.036 Uiso 1 1 calc R . . C11 C 0.3090(5) 0.0459(3) 0.61561(13) 0.0281(7) Uani 1 1 d . . . H11 H 0.1915 0.0251 0.6294 0.034 Uiso 1 1 calc R . . C12 C 0.3651(5) -0.0589(3) 0.57934(14) 0.0305(9) Uani 1 1 d . . . H12A H 0.4831 -0.0432 0.5658 0.037 Uiso 1 1 calc R . . H12B H 0.2873 -0.0638 0.5475 0.037 Uiso 1 1 calc R . . C13 C 0.3622(5) -0.1796(3) 0.60972(15) 0.0354(9) Uani 1 1 d . . . H13A H 0.2415 -0.2021 0.6179 0.042 Uiso 1 1 calc R . . H13B H 0.4118 -0.2439 0.5863 0.042 Uiso 1 1 calc R . . C14 C 0.4639(5) -0.1720(3) 0.66238(15) 0.0343(9) Uani 1 1 d . . . H14A H 0.4456 -0.2472 0.6838 0.041 Uiso 1 1 calc R . . H14B H 0.5883 -0.1659 0.6539 0.041 Uiso 1 1 calc R . . C15 C 0.4100(5) -0.0635(3) 0.69584(14) 0.0306(9) Uani 1 1 d . . . H15A H 0.2890 -0.0742 0.7077 0.037 Uiso 1 1 calc R . . H15B H 0.4828 -0.0588 0.7288 0.037 Uiso 1 1 calc R . . C16 C 0.8386(4) 0.1129(3) 0.73927(13) 0.0271(7) Uani 1 1 d . . . C17 C 0.9404(5) 0.1653(4) 0.78527(15) 0.0347(9) Uani 1 1 d . . . C18 C 1.0143(5) 0.2740(4) 0.78243(18) 0.0406(10) Uani 1 1 d . . . C19 C 0.8298(6) -0.0342(3) 0.55300(15) 0.0355(8) Uani 1 1 d . . . C20 C 0.9181(5) -0.1429(4) 0.52887(19) 0.0415(10) Uani 1 1 d . . . C21 C 0.9469(6) -0.2448(4) 0.5540(2) 0.0439(11) Uani 1 1 d . . . H17 H 0.940(4) 0.107(3) 0.8219(13) 0.022(8) Uiso 1 1 d . . . H18B H 1.069(5) 0.307(3) 0.8155(16) 0.039(11) Uiso 1 1 d . . . H18A H 1.013(4) 0.320(3) 0.7475(15) 0.021(9) Uiso 1 1 d . . . H21A H 0.997(6) -0.313(4) 0.5370(18) 0.058(14) Uiso 1 1 d . . . H21B H 0.914(4) -0.249(3) 0.5922(15) 0.028(10) Uiso 1 1 d . . . H20 H 0.943(5) -0.140(3) 0.4888(17) 0.049(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02233(17) 0.02927(18) 0.02482(17) 0.00203(19) 0.00065(19) -0.00036(19) O1 0.0268(12) 0.0390(13) 0.0286(12) 0.0055(10) -0.0048(12) -0.0031(13) O2 0.0418(16) 0.0327(15) 0.0521(18) 0.0054(13) -0.0011(14) -0.0069(12) O3 0.0289(13) 0.0398(13) 0.0347(14) -0.0049(11) 0.0025(13) 0.0037(13) O4 0.078(2) 0.0406(16) 0.0428(16) 0.0064(13) 0.0175(16) 0.0089(15) N1 0.0238(15) 0.0287(16) 0.0200(14) 0.0016(13) 0.0000(12) -0.0019(13) N2 0.0262(15) 0.0274(16) 0.0226(15) 0.0017(12) 0.0011(12) -0.0033(12) C1 0.0252(17) 0.037(2) 0.0278(19) 0.0030(16) 0.0045(15) -0.0056(15) C2 0.034(2) 0.034(2) 0.033(2) 0.0055(16) 0.0007(15) -0.0053(15) C3 0.040(2) 0.0285(18) 0.039(2) 0.0026(16) -0.004(2) -0.0053(19) C4 0.036(2) 0.0309(19) 0.038(2) -0.0002(17) 0.0024(18) 0.0016(16) C5 0.0288(18) 0.0276(18) 0.026(2) -0.0038(15) 0.0006(16) 0.0010(15) C6 0.024(2) 0.0302(18) 0.038(2) -0.0035(16) 0.0054(16) 0.0023(15) C7 0.0219(19) 0.034(2) 0.046(2) 0.0037(16) -0.0001(15) 0.0024(15) C8 0.024(2) 0.0318(19) 0.0315(19) 0.0033(15) -0.0077(16) 0.0002(16) C9 0.0319(19) 0.0280(18) 0.0231(18) 0.0030(15) -0.0059(15) 0.0008(16) C10 0.0259(19) 0.037(2) 0.0265(19) -0.0051(16) 0.0045(15) -0.0055(16) C11 0.0207(17) 0.0348(18) 0.0287(17) -0.0004(14) -0.0068(16) -0.0018(16) C12 0.033(2) 0.035(2) 0.0232(17) -0.0009(15) -0.0073(15) -0.0045(15) C13 0.042(2) 0.0310(19) 0.033(2) -0.0013(16) -0.0009(18) -0.0052(17) C14 0.035(2) 0.030(2) 0.037(2) 0.0079(16) -0.0034(18) -0.0036(17) C15 0.0283(19) 0.034(2) 0.0295(19) 0.0053(16) 0.0006(15) -0.0046(16) C16 0.0198(16) 0.034(2) 0.0279(17) 0.0004(14) -0.0005(15) 0.0037(16) C17 0.031(2) 0.047(2) 0.027(2) 0.0014(18) 0.0000(16) 0.0032(18) C18 0.033(2) 0.056(3) 0.032(2) -0.010(2) 0.0012(19) -0.002(2) C19 0.033(2) 0.0328(19) 0.041(2) -0.0064(17) 0.007(2) -0.007(2) C20 0.040(2) 0.039(2) 0.046(3) -0.010(2) 0.012(2) -0.0091(19) C21 0.040(2) 0.038(3) 0.054(3) -0.011(2) 0.004(2) -0.005(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 O3 1.938(2) . ? Zn1 O1 1.978(2) . ? Zn1 N2 2.092(3) . ? Zn1 N1 2.102(3) . ? O1 C16 1.280(4) . ? O2 C16 1.239(4) . ? O3 C19 1.294(4) . ? O4 C19 1.228(5) . ? N1 C1 1.492(4) . ? N1 C9 1.504(4) . ? N1 C5 1.512(4) . ? N2 C15 1.493(4) . ? N2 C10 1.494(4) . ? N2 C11 1.509(4) . ? C1 C2 1.533(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.519(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.530(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.527(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.540(5) . ? C5 H5 1.0000 . ? C6 C7 1.522(5) . ? C6 C10 1.531(5) . ? C6 H6 1.0000 . ? C7 C8 1.527(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C11 1.534(4) . ? C8 C9 1.536(5) . ? C8 H8 1.0000 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.520(5) . ? C11 H11 1.0000 . ? C12 C13 1.524(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.519(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.509(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.495(5) . ? C17 C18 1.328(6) . ? C17 H17 1.11(3) . ? C18 H18B 0.99(4) . ? C18 H18A 1.00(4) . ? C19 C20 1.500(5) . ? C20 C21 1.299(6) . ? C20 H20 1.00(4) . ? C21 H21A 0.94(4) . ? C21 H21B 0.97(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 108.67(11) . . ? O3 Zn1 N2 117.82(11) . . ? O1 Zn1 N2 118.85(11) . . ? O3 Zn1 N1 125.06(11) . . ? O1 Zn1 N1 95.42(10) . . ? N2 Zn1 N1 88.84(11) . . ? C16 O1 Zn1 110.3(2) . . ? C19 O3 Zn1 121.5(2) . . ? C1 N1 C9 111.8(3) . . ? C1 N1 C5 110.3(3) . . ? C9 N1 C5 112.6(2) . . ? C1 N1 Zn1 104.9(2) . . ? C9 N1 Zn1 109.7(2) . . ? C5 N1 Zn1 107.10(19) . . ? C15 N2 C10 108.0(3) . . ? C15 N2 C11 108.7(3) . . ? C10 N2 C11 110.8(3) . . ? C15 N2 Zn1 112.9(2) . . ? C10 N2 Zn1 105.2(2) . . ? C11 N2 Zn1 111.2(2) . . ? N1 C1 C2 114.7(3) . . ? N1 C1 H1A 108.6 . . ? C2 C1 H1A 108.6 . . ? N1 C1 H1B 108.6 . . ? C2 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C3 C2 C1 109.8(3) . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 C3 C4 109.5(3) . . ? C2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? C2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C3 111.4(3) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? N1 C5 C4 113.1(3) . . ? N1 C5 C6 110.4(3) . . ? C4 C5 C6 111.5(3) . . ? N1 C5 H5 107.1 . . ? C4 C5 H5 107.1 . . ? C6 C5 H5 107.1 . . ? C7 C6 C10 108.3(3) . . ? C7 C6 C5 110.9(3) . . ? C10 C6 C5 114.4(3) . . ? C7 C6 H6 107.7 . . ? C10 C6 H6 107.7 . . ? C5 C6 H6 107.7 . . ? C6 C7 C8 106.8(3) . . ? C6 C7 H7A 110.4 . . ? C8 C7 H7A 110.4 . . ? C6 C7 H7B 110.4 . . ? C8 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? C7 C8 C11 108.5(3) . . ? C7 C8 C9 109.1(3) . . ? C11 C8 C9 116.9(3) . . ? C7 C8 H8 107.3 . . ? C11 C8 H8 107.3 . . ? C9 C8 H8 107.3 . . ? N1 C9 C8 112.0(3) . . ? N1 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? N1 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? N2 C10 C6 114.3(3) . . ? N2 C10 H10A 108.7 . . ? C6 C10 H10A 108.7 . . ? N2 C10 H10B 108.7 . . ? C6 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N2 C11 C12 109.5(3) . . ? N2 C11 C8 111.6(3) . . ? C12 C11 C8 115.2(3) . . ? N2 C11 H11 106.7 . . ? C12 C11 H11 106.7 . . ? C8 C11 H11 106.7 . . ? C11 C12 C13 111.6(3) . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 111.2(3) . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 111.3(3) . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? N2 C15 C14 111.9(3) . . ? N2 C15 H15A 109.2 . . ? C14 C15 H15A 109.2 . . ? N2 C15 H15B 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? O2 C16 O1 123.2(3) . . ? O2 C16 C17 119.2(3) . . ? O1 C16 C17 117.7(3) . . ? C18 C17 C16 122.4(4) . . ? C18 C17 H17 124.5(17) . . ? C16 C17 H17 113.0(17) . . ? C17 C18 H18B 119(2) . . ? C17 C18 H18A 120(2) . . ? H18B C18 H18A 122(3) . . ? O4 C19 O3 124.6(3) . . ? O4 C19 C20 118.9(4) . . ? O3 C19 C20 116.5(4) . . ? C21 C20 C19 125.3(4) . . ? C21 C20 H20 118(2) . . ? C19 C20 H20 117(2) . . ? C20 C21 H21A 123(3) . . ? C20 C21 H21B 117(2) . . ? H21A C21 H21B 120(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 O1 C16 -82.9(2) . . . . ? N2 Zn1 O1 C16 55.5(2) . . . . ? N1 Zn1 O1 C16 147.2(2) . . . . ? O1 Zn1 O3 C19 -120.5(3) . . . . ? N2 Zn1 O3 C19 100.6(3) . . . . ? N1 Zn1 O3 C19 -9.5(3) . . . . ? O3 Zn1 N1 C1 -55.0(2) . . . . ? O1 Zn1 N1 C1 62.4(2) . . . . ? N2 Zn1 N1 C1 -178.8(2) . . . . ? O3 Zn1 N1 C9 65.2(2) . . . . ? O1 Zn1 N1 C9 -177.4(2) . . . . ? N2 Zn1 N1 C9 -58.6(2) . . . . ? O3 Zn1 N1 C5 -172.24(18) . . . . ? O1 Zn1 N1 C5 -54.9(2) . . . . ? N2 Zn1 N1 C5 64.0(2) . . . . ? O3 Zn1 N2 C15 51.0(2) . . . . ? O1 Zn1 N2 C15 -83.7(2) . . . . ? N1 Zn1 N2 C15 -179.3(2) . . . . ? O3 Zn1 N2 C10 168.53(19) . . . . ? O1 Zn1 N2 C10 33.8(2) . . . . ? N1 Zn1 N2 C10 -61.8(2) . . . . ? O3 Zn1 N2 C11 -71.4(2) . . . . ? O1 Zn1 N2 C11 153.81(18) . . . . ? N1 Zn1 N2 C11 58.3(2) . . . . ? C9 N1 C1 C2 74.1(4) . . . . ? C5 N1 C1 C2 -52.1(4) . . . . ? Zn1 N1 C1 C2 -167.1(2) . . . . ? N1 C1 C2 C3 56.1(4) . . . . ? C1 C2 C3 C4 -56.6(4) . . . . ? C2 C3 C4 C5 57.1(4) . . . . ? C1 N1 C5 C4 50.8(4) . . . . ? C9 N1 C5 C4 -74.9(3) . . . . ? Zn1 N1 C5 C4 164.4(2) . . . . ? C1 N1 C5 C6 176.6(3) . . . . ? C9 N1 C5 C6 51.0(4) . . . . ? Zn1 N1 C5 C6 -69.8(3) . . . . ? C3 C4 C5 N1 -54.8(4) . . . . ? C3 C4 C5 C6 -180.0(3) . . . . ? N1 C5 C6 C7 -57.5(4) . . . . ? C4 C5 C6 C7 69.3(4) . . . . ? N1 C5 C6 C10 65.3(4) . . . . ? C4 C5 C6 C10 -167.9(3) . . . . ? C10 C6 C7 C8 -62.9(3) . . . . ? C5 C6 C7 C8 63.3(3) . . . . ? C6 C7 C8 C11 65.6(3) . . . . ? C6 C7 C8 C9 -62.7(3) . . . . ? C1 N1 C9 C8 -177.2(3) . . . . ? C5 N1 C9 C8 -52.3(4) . . . . ? Zn1 N1 C9 C8 66.9(3) . . . . ? C7 C8 C9 N1 58.4(4) . . . . ? C11 C8 C9 N1 -65.1(4) . . . . ? C15 N2 C10 C6 -169.4(3) . . . . ? C11 N2 C10 C6 -50.4(4) . . . . ? Zn1 N2 C10 C6 69.8(3) . . . . ? C7 C6 C10 N2 57.0(4) . . . . ? C5 C6 C10 N2 -67.2(4) . . . . ? C15 N2 C11 C12 -61.2(3) . . . . ? C10 N2 C11 C12 -179.8(3) . . . . ? Zn1 N2 C11 C12 63.6(3) . . . . ? C15 N2 C11 C8 170.0(3) . . . . ? C10 N2 C11 C8 51.5(4) . . . . ? Zn1 N2 C11 C8 -65.2(3) . . . . ? C7 C8 C11 N2 -60.4(4) . . . . ? C9 C8 C11 N2 63.4(4) . . . . ? C7 C8 C11 C12 174.0(3) . . . . ? C9 C8 C11 C12 -62.2(4) . . . . ? N2 C11 C12 C13 58.1(4) . . . . ? C8 C11 C12 C13 -175.1(3) . . . . ? C11 C12 C13 C14 -52.6(4) . . . . ? C12 C13 C14 C15 50.7(4) . . . . ? C10 N2 C15 C14 -178.8(3) . . . . ? C11 N2 C15 C14 61.0(4) . . . . ? Zn1 N2 C15 C14 -62.9(3) . . . . ? C13 C14 C15 N2 -55.9(4) . . . . ? Zn1 O1 C16 O2 2.8(4) . . . . ? Zn1 O1 C16 C17 -176.5(2) . . . . ? O2 C16 C17 C18 -175.4(4) . . . . ? O1 C16 C17 C18 3.9(5) . . . . ? Zn1 O3 C19 O4 6.0(6) . . . . ? Zn1 O3 C19 C20 -174.3(3) . . . . ? O4 C19 C20 C21 -167.3(4) . . . . ? O3 C19 C20 C21 13.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.36 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.613 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.069 #===END