Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jason Matthews' _publ_contact_author_address ; Department of Chemistry Howard University 525 College Street, NW Washington DC 20059 UNITED STATES OF AMERICA ; _publ_contact_author_email JSMATTHEWS@HOWARD.EDU _publ_section_title ; Synthesis and characterization of zinc AP-MOCVD precursors and their utility in the growth of ZnO ; loop_ _publ_author_name 'Jason Matthews' 'R. Butcher' 'Olamide O. Onakoya' 'Tantiboro S. Ouattara' # Attachment 'B603308C C18H32N2O2Zn revised cif.doc' data_C18H32N2O2Zn _database_code_depnum_ccdc_archive 'CCDC 600122' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H32 N2 O2 Zn' _chemical_formula_weight 373.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0085(6) _cell_length_b 11.0745(9) _cell_length_c 12.4796(10) _cell_angle_alpha 67.725(1) _cell_angle_beta 84.904(1) _cell_angle_gamma 69.131(1) _cell_volume 955.66(13) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_min 0.25 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_max 0.56 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 1.296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.678953 _exptl_absorpt_correction_T_max 0.928069 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7216 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.26 _reflns_number_total 4499 _reflns_number_gt 3800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4499 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.57493(2) 0.746830(19) 0.765802(17) 0.01708(7) Uani 1 1 d . . . O1A O 0.33763(15) 0.87961(12) 0.76477(10) 0.0212(3) Uani 1 1 d . . . O1B O 0.55955(15) 0.60824(12) 0.71098(10) 0.0207(3) Uani 1 1 d . . . N1A N 0.68417(18) 0.87909(14) 0.65650(12) 0.0170(3) Uani 1 1 d . . . N1B N 0.68658(18) 0.61890(14) 0.92240(12) 0.0176(3) Uani 1 1 d . . . C1A C 0.1079(2) 1.09840(18) 0.71130(16) 0.0235(4) Uani 1 1 d . . . H1AA H 0.0274 1.0615 0.6894 0.035 Uiso 1 1 calc R . . H1AB H 0.0852 1.1948 0.6579 0.035 Uiso 1 1 calc R . . H1AC H 0.0867 1.0958 0.7906 0.035 Uiso 1 1 calc R . . C2A C 0.2991(2) 1.01096(17) 0.70514(14) 0.0184(3) Uani 1 1 d . . . C3A C 0.4124(2) 1.07462(17) 0.63859(15) 0.0198(3) Uani 1 1 d . . . H3AA H 0.3630 1.1733 0.6038 0.024 Uiso 1 1 calc R . . C4A C 0.5946(2) 1.01312(17) 0.61424(14) 0.0178(3) Uani 1 1 d . . . C5A C 0.6789(2) 1.11420(18) 0.53476(16) 0.0233(4) Uani 1 1 d . . . H5AA H 0.7895 1.1013 0.5726 0.035 Uiso 1 1 calc R . . H5AB H 0.5955 1.2097 0.5176 0.035 Uiso 1 1 calc R . . H5AC H 0.7063 1.0974 0.4624 0.035 Uiso 1 1 calc R . . C6A C 0.8699(2) 0.82568(17) 0.62458(15) 0.0198(3) Uani 1 1 d . . . H6AA H 0.9504 0.8408 0.6701 0.024 Uiso 1 1 calc R . . H6AB H 0.8798 0.8775 0.5414 0.024 Uiso 1 1 calc R . . C7A C 0.9275(2) 0.67165(17) 0.64744(15) 0.0196(3) Uani 1 1 d . . . H7AA H 0.8409 0.6567 0.6064 0.024 Uiso 1 1 calc R . . H7AB H 0.9238 0.6202 0.7315 0.024 Uiso 1 1 calc R . . C8A C 1.1149(2) 0.61154(18) 0.60883(16) 0.0226(4) Uani 1 1 d . . . H8AA H 1.1204 0.6632 0.5250 0.027 Uiso 1 1 calc R . . H8AB H 1.2031 0.6234 0.6512 0.027 Uiso 1 1 calc R . . C9A C 1.1634(2) 0.45744(19) 0.63171(18) 0.0306(4) Uani 1 1 d . . . H9AA H 1.2790 0.4237 0.5994 0.046 Uiso 1 1 calc R . . H9AB H 1.0710 0.4448 0.5950 0.046 Uiso 1 1 calc R . . H9AC H 1.1715 0.4047 0.7155 0.046 Uiso 1 1 calc R . . C1B C 0.6447(3) 0.38436(19) 0.70527(17) 0.0286(4) Uani 1 1 d . . . H1BA H 0.6982 0.4150 0.6306 0.043 Uiso 1 1 calc R . . H1BB H 0.5230 0.3897 0.6920 0.043 Uiso 1 1 calc R . . H1BC H 0.7172 0.2880 0.7516 0.043 Uiso 1 1 calc R . . C2B C 0.6380(2) 0.47721(18) 0.76922(15) 0.0200(3) Uani 1 1 d . . . C3B C 0.7125(2) 0.41753(17) 0.88053(15) 0.0203(3) Uani 1 1 d . . . H3BA H 0.7608 0.3186 0.9116 0.024 Uiso 1 1 calc R . . C4B C 0.7271(2) 0.48387(17) 0.95555(15) 0.0187(3) Uani 1 1 d . . . C5B C 0.7970(2) 0.38889(18) 1.07812(15) 0.0234(4) Uani 1 1 d . . . H5BA H 0.7126 0.4193 1.1325 0.035 Uiso 1 1 calc R . . H5BB H 0.9135 0.3923 1.0919 0.035 Uiso 1 1 calc R . . H5BC H 0.8103 0.2933 1.0896 0.035 Uiso 1 1 calc R . . C6B C 0.7137(2) 0.67539(17) 1.00631(14) 0.0199(3) Uani 1 1 d . . . H6BA H 0.8302 0.6160 1.0499 0.024 Uiso 1 1 calc R . . H6BB H 0.6184 0.6735 1.0625 0.024 Uiso 1 1 calc R . . C7B C 0.7106(2) 0.82356(17) 0.94611(15) 0.0198(3) Uani 1 1 d . . . H7BA H 0.5899 0.8845 0.9093 0.024 Uiso 1 1 calc R . . H7BB H 0.7969 0.8269 0.8841 0.024 Uiso 1 1 calc R . . C8B C 0.7576(2) 0.87885(18) 1.02948(15) 0.0214(4) Uani 1 1 d . . . H8BA H 0.6706 0.8763 1.0911 0.026 Uiso 1 1 calc R . . H8BB H 0.8778 0.8174 1.0668 0.026 Uiso 1 1 calc R . . C9B C 0.7563(2) 1.02699(19) 0.96905(16) 0.0261(4) Uani 1 1 d . . . H9BA H 0.7765 1.0611 1.0269 0.039 Uiso 1 1 calc R . . H9BB H 0.6402 1.0871 0.9274 0.039 Uiso 1 1 calc R . . H9BC H 0.8514 1.0283 0.9139 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.01953(10) 0.01371(10) 0.01419(11) -0.00224(7) -0.00033(7) -0.00440(7) O1A 0.0208(6) 0.0172(6) 0.0198(6) -0.0033(5) 0.0010(5) -0.0040(5) O1B 0.0233(6) 0.0164(6) 0.0202(6) -0.0049(5) -0.0030(5) -0.0056(5) N1A 0.0197(7) 0.0171(7) 0.0130(7) -0.0045(6) 0.0008(5) -0.0061(6) N1B 0.0200(6) 0.0172(7) 0.0136(7) -0.0037(6) 0.0014(5) -0.0064(6) C1A 0.0218(8) 0.0231(9) 0.0224(10) -0.0086(8) -0.0035(7) -0.0029(7) C2A 0.0213(8) 0.0179(8) 0.0140(8) -0.0072(7) -0.0043(6) -0.0019(7) C3A 0.0256(8) 0.0116(8) 0.0178(9) -0.0033(7) -0.0039(7) -0.0028(7) C4A 0.0250(8) 0.0170(8) 0.0117(8) -0.0036(6) -0.0033(6) -0.0085(7) C5A 0.0285(9) 0.0195(9) 0.0198(9) -0.0025(7) -0.0020(7) -0.0104(7) C6A 0.0191(8) 0.0196(9) 0.0183(9) -0.0052(7) 0.0019(6) -0.0062(7) C7A 0.0189(8) 0.0198(9) 0.0174(9) -0.0049(7) 0.0006(6) -0.0059(7) C8A 0.0210(8) 0.0223(9) 0.0217(9) -0.0071(7) 0.0015(7) -0.0057(7) C9A 0.0268(9) 0.0242(10) 0.0359(12) -0.0113(9) -0.0013(8) -0.0026(8) C1B 0.0318(10) 0.0235(10) 0.0306(11) -0.0128(8) -0.0020(8) -0.0061(8) C2B 0.0158(7) 0.0201(9) 0.0240(9) -0.0083(7) 0.0043(7) -0.0070(7) C3B 0.0213(8) 0.0120(8) 0.0225(9) -0.0033(7) 0.0015(7) -0.0036(6) C4B 0.0160(7) 0.0172(8) 0.0169(9) -0.0018(7) 0.0014(6) -0.0041(6) C5B 0.0263(9) 0.0174(9) 0.0187(9) -0.0004(7) -0.0005(7) -0.0051(7) C6B 0.0235(8) 0.0196(9) 0.0143(8) -0.0052(7) 0.0008(6) -0.0061(7) C7B 0.0205(8) 0.0202(9) 0.0169(9) -0.0057(7) 0.0007(6) -0.0062(7) C8B 0.0244(8) 0.0216(9) 0.0181(9) -0.0066(7) -0.0006(7) -0.0084(7) C9B 0.0282(9) 0.0243(9) 0.0253(10) -0.0070(8) -0.0019(7) -0.0103(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O1A 1.9424(12) . ? Zn O1B 1.9455(11) . ? Zn N1B 1.9836(14) . ? Zn N1A 1.9893(14) . ? O1A C2A 1.291(2) . ? O1B C2B 1.289(2) . ? N1A C4A 1.308(2) . ? N1A C6A 1.472(2) . ? N1B C4B 1.312(2) . ? N1B C6B 1.473(2) . ? C1A C2A 1.506(2) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C2A C3A 1.374(2) . ? C3A C4A 1.434(2) . ? C3A H3AA 0.9500 . ? C4A C5A 1.506(2) . ? C5A H5AA 0.9800 . ? C5A H5AB 0.9800 . ? C5A H5AC 0.9800 . ? C6A C7A 1.516(2) . ? C6A H6AA 0.9900 . ? C6A H6AB 0.9900 . ? C7A C8A 1.527(2) . ? C7A H7AA 0.9900 . ? C7A H7AB 0.9900 . ? C8A C9A 1.524(2) . ? C8A H8AA 0.9900 . ? C8A H8AB 0.9900 . ? C9A H9AA 0.9800 . ? C9A H9AB 0.9800 . ? C9A H9AC 0.9800 . ? C1B C2B 1.507(2) . ? C1B H1BA 0.9800 . ? C1B H1BB 0.9800 . ? C1B H1BC 0.9800 . ? C2B C3B 1.376(2) . ? C3B C4B 1.426(2) . ? C3B H3BA 0.9500 . ? C4B C5B 1.507(2) . ? C5B H5BA 0.9800 . ? C5B H5BB 0.9800 . ? C5B H5BC 0.9800 . ? C6B C7B 1.516(2) . ? C6B H6BA 0.9900 . ? C6B H6BB 0.9900 . ? C7B C8B 1.522(2) . ? C7B H7BA 0.9900 . ? C7B H7BB 0.9900 . ? C8B C9B 1.520(2) . ? C8B H8BA 0.9900 . ? C8B H8BB 0.9900 . ? C9B H9BA 0.9800 . ? C9B H9BB 0.9800 . ? C9B H9BC 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Zn O1B 110.08(5) . . ? O1A Zn N1B 114.78(5) . . ? O1B Zn N1B 98.11(5) . . ? O1A Zn N1A 98.37(5) . . ? O1B Zn N1A 114.25(5) . . ? N1B Zn N1A 121.68(6) . . ? C2A O1A Zn 121.04(11) . . ? C2B O1B Zn 120.70(11) . . ? C4A N1A C6A 119.45(14) . . ? C4A N1A Zn 121.01(11) . . ? C6A N1A Zn 119.53(10) . . ? C4B N1B C6B 118.85(14) . . ? C4B N1B Zn 120.90(11) . . ? C6B N1B Zn 120.12(10) . . ? C2A C1A H1AA 109.5 . . ? C2A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? C2A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? O1A C2A C3A 126.81(15) . . ? O1A C2A C1A 114.05(15) . . ? C3A C2A C1A 119.13(15) . . ? C2A C3A C4A 129.14(15) . . ? C2A C3A H3AA 115.4 . . ? C4A C3A H3AA 115.4 . . ? N1A C4A C3A 123.50(15) . . ? N1A C4A C5A 121.23(15) . . ? C3A C4A C5A 115.27(14) . . ? C4A C5A H5AA 109.5 . . ? C4A C5A H5AB 109.5 . . ? H5AA C5A H5AB 109.5 . . ? C4A C5A H5AC 109.5 . . ? H5AA C5A H5AC 109.5 . . ? H5AB C5A H5AC 109.5 . . ? N1A C6A C7A 110.89(13) . . ? N1A C6A H6AA 109.5 . . ? C7A C6A H6AA 109.5 . . ? N1A C6A H6AB 109.5 . . ? C7A C6A H6AB 109.5 . . ? H6AA C6A H6AB 108.1 . . ? C6A C7A C8A 113.62(13) . . ? C6A C7A H7AA 108.8 . . ? C8A C7A H7AA 108.8 . . ? C6A C7A H7AB 108.8 . . ? C8A C7A H7AB 108.8 . . ? H7AA C7A H7AB 107.7 . . ? C9A C8A C7A 111.10(14) . . ? C9A C8A H8AA 109.4 . . ? C7A C8A H8AA 109.4 . . ? C9A C8A H8AB 109.4 . . ? C7A C8A H8AB 109.4 . . ? H8AA C8A H8AB 108.0 . . ? C8A C9A H9AA 109.5 . . ? C8A C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C8A C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C2B C1B H1BA 109.5 . . ? C2B C1B H1BB 109.5 . . ? H1BA C1B H1BB 109.5 . . ? C2B C1B H1BC 109.5 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? O1B C2B C3B 126.61(16) . . ? O1B C2B C1B 114.39(15) . . ? C3B C2B C1B 119.00(16) . . ? C2B C3B C4B 128.83(16) . . ? C2B C3B H3BA 115.6 . . ? C4B C3B H3BA 115.6 . . ? N1B C4B C3B 123.59(15) . . ? N1B C4B C5B 120.39(15) . . ? C3B C4B C5B 116.01(15) . . ? C4B C5B H5BA 109.5 . . ? C4B C5B H5BB 109.5 . . ? H5BA C5B H5BB 109.5 . . ? C4B C5B H5BC 109.5 . . ? H5BA C5B H5BC 109.5 . . ? H5BB C5B H5BC 109.5 . . ? N1B C6B C7B 111.34(13) . . ? N1B C6B H6BA 109.4 . . ? C7B C6B H6BA 109.4 . . ? N1B C6B H6BB 109.4 . . ? C7B C6B H6BB 109.4 . . ? H6BA C6B H6BB 108.0 . . ? C6B C7B C8B 112.25(14) . . ? C6B C7B H7BA 109.2 . . ? C8B C7B H7BA 109.2 . . ? C6B C7B H7BB 109.2 . . ? C8B C7B H7BB 109.2 . . ? H7BA C7B H7BB 107.9 . . ? C9B C8B C7B 112.34(14) . . ? C9B C8B H8BA 109.1 . . ? C7B C8B H8BA 109.1 . . ? C9B C8B H8BB 109.1 . . ? C7B C8B H8BB 109.1 . . ? H8BA C8B H8BB 107.9 . . ? C8B C9B H9BA 109.5 . . ? C8B C9B H9BB 109.5 . . ? H9BA C9B H9BB 109.5 . . ? C8B C9B H9BC 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? 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 O1B Zn O1A C2A -121.44(12) . . . . ? N1B Zn O1A C2A 129.03(12) . . . . ? N1A Zn O1A C2A -1.71(13) . . . . ? O1A Zn O1B C2B -129.95(12) . . . . ? N1B Zn O1B C2B -9.76(13) . . . . ? N1A Zn O1B C2B 120.49(12) . . . . ? O1A Zn N1A C4A 3.39(13) . . . . ? O1B Zn N1A C4A 119.94(12) . . . . ? N1B Zn N1A C4A -122.67(12) . . . . ? O1A Zn N1A C6A -177.92(11) . . . . ? O1B Zn N1A C6A -61.37(12) . . . . ? N1B Zn N1A C6A 56.01(13) . . . . ? O1A Zn N1B C4B 117.68(12) . . . . ? O1B Zn N1B C4B 1.08(13) . . . . ? N1A Zn N1B C4B -124.06(12) . . . . ? O1A Zn N1B C6B -58.06(13) . . . . ? O1B Zn N1B C6B -174.66(11) . . . . ? N1A Zn N1B C6B 60.20(13) . . . . ? Zn O1A C2A C3A -1.1(2) . . . . ? Zn O1A C2A C1A 178.26(10) . . . . ? O1A C2A C3A C4A 3.3(3) . . . . ? C1A C2A C3A C4A -176.03(15) . . . . ? C6A N1A C4A C3A 178.83(14) . . . . ? Zn N1A C4A C3A -2.5(2) . . . . ? C6A N1A C4A C5A -0.9(2) . . . . ? Zn N1A C4A C5A 177.83(11) . . . . ? C2A C3A C4A N1A -1.1(3) . . . . ? C2A C3A C4A C5A 178.59(16) . . . . ? C4A N1A C6A C7A -160.91(14) . . . . ? Zn N1A C6A C7A 20.38(17) . . . . ? N1A C6A C7A C8A 176.22(13) . . . . ? C6A C7A C8A C9A -178.78(15) . . . . ? Zn O1B C2B C3B 11.6(2) . . . . ? Zn O1B C2B C1B -168.64(11) . . . . ? O1B C2B C3B C4B -2.5(3) . . . . ? C1B C2B C3B C4B 177.74(16) . . . . ? C6B N1B C4B C3B -177.60(14) . . . . ? Zn N1B C4B C3B 6.6(2) . . . . ? C6B N1B C4B C5B 1.1(2) . . . . ? Zn N1B C4B C5B -174.67(11) . . . . ? C2B C3B C4B N1B -8.1(3) . . . . ? C2B C3B C4B C5B 173.10(16) . . . . ? C4B N1B C6B C7B 164.03(14) . . . . ? Zn N1B C6B C7B -20.15(18) . . . . ? N1B C6B C7B C8B -174.05(13) . . . . ? C6B C7B C8B C9B 179.45(14) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.367 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.058 data_C18H32N2O4Zn _database_code_depnum_ccdc_archive 'CCDC 600123' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H32 N2 O4 Zn' _chemical_formula_weight 405.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.6208(6) _cell_length_b 14.0222(11) _cell_length_c 19.2162(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.473(1) _cell_angle_gamma 90.00 _cell_volume 2052.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_min 0.55 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_max 0.95 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.784310 _exptl_absorpt_correction_T_max 0.894385 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15417 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.40 _reflns_number_total 5066 _reflns_number_gt 4236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+1.2643P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5066 _refine_ls_number_parameters 234 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0723 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Zn Zn 0.87897(2) 0.526252(13) 0.205072(9) 0.01487(6) Uani 1 1 d . . . O1A O 0.77340(15) 0.55403(8) 0.29461(6) 0.0174(2) Uani 1 1 d . . . O2A O 0.66789(16) 0.50340(8) 0.39493(6) 0.0186(2) Uani 1 1 d . . . O1B O 0.82315(14) 0.62555(8) 0.13736(6) 0.0179(2) Uani 1 1 d . . . O2B O 0.89833(15) 0.73258(8) 0.05827(6) 0.0185(2) Uani 1 1 d . . . N1A N 0.74804(18) 0.40957(10) 0.18564(7) 0.0168(3) Uani 1 1 d . . . N1B N 1.13201(17) 0.54620(10) 0.21120(7) 0.0167(3) Uani 1 1 d . . . C1A C 0.7038(3) 0.59316(15) 0.49868(10) 0.0308(4) Uani 1 1 d . . . H1AA H 0.7221 0.6573 0.5177 0.046 Uiso 1 1 calc R . . H1AB H 0.7987 0.5512 0.5154 0.046 Uiso 1 1 calc R . . H1AC H 0.5910 0.5682 0.5139 0.046 Uiso 1 1 calc R . . C2A C 0.7036(2) 0.59739(12) 0.42086(9) 0.0221(3) Uani 1 1 d . . . H2AA H 0.6124 0.6424 0.4035 0.027 Uiso 1 1 calc R . . H2AB H 0.8190 0.6196 0.4049 0.027 Uiso 1 1 calc R . . C3A C 0.7013(2) 0.48776(11) 0.32749(8) 0.0151(3) Uani 1 1 d . . . C4A C 0.6484(2) 0.39955(11) 0.30282(8) 0.0163(3) Uani 1 1 d . . . H4AA H 0.5985 0.3573 0.3355 0.020 Uiso 1 1 calc R . . C5A C 0.6610(2) 0.36597(11) 0.23432(9) 0.0167(3) Uani 1 1 d . . . C6A C 0.5665(2) 0.27421(12) 0.21931(9) 0.0235(4) Uani 1 1 d . . . H6AA H 0.4857 0.2829 0.1793 0.035 Uiso 1 1 calc R . . H6AB H 0.5001 0.2554 0.2601 0.035 Uiso 1 1 calc R . . H6AC H 0.6520 0.2244 0.2087 0.035 Uiso 1 1 calc R . . C7A C 0.7513(2) 0.37079(13) 0.11487(9) 0.0232(4) Uani 1 1 d . . . H7AA H 0.7240 0.3011 0.1168 0.028 Uiso 1 1 calc R . . C8A C 0.9327(3) 0.38333(17) 0.08619(10) 0.0346(5) Uani 1 1 d . . . H8AA H 1.0191 0.3519 0.1171 0.052 Uiso 1 1 calc R . . H8AB H 0.9601 0.4515 0.0831 0.052 Uiso 1 1 calc R . . H8AC H 0.9365 0.3547 0.0397 0.052 Uiso 1 1 calc R . . C9A C 0.6146(3) 0.41930(15) 0.06868(10) 0.0319(4) Uani 1 1 d . . . H9AA H 0.4977 0.4075 0.0869 0.048 Uiso 1 1 calc R . . H9AB H 0.6205 0.3937 0.0213 0.048 Uiso 1 1 calc R . . H9AC H 0.6373 0.4881 0.0679 0.048 Uiso 1 1 calc R . . C1B C 0.6972(3) 0.80686(16) -0.01850(11) 0.0345(5) Uani 1 1 d . . . H1BA H 0.5727 0.8151 -0.0311 0.052 Uiso 1 1 calc R . . H1BB H 0.7577 0.7772 -0.0574 0.052 Uiso 1 1 calc R . . H1BC H 0.7500 0.8692 -0.0083 0.052 Uiso 1 1 calc R . . C2B C 0.7144(2) 0.74480(14) 0.04392(9) 0.0239(4) Uani 1 1 d . . . H2BA H 0.6575 0.7750 0.0841 0.029 Uiso 1 1 calc R . . H2BB H 0.6579 0.6823 0.0348 0.029 Uiso 1 1 calc R . . C3B C 0.9442(2) 0.66954(11) 0.10808(8) 0.0158(3) Uani 1 1 d . . . C4B C 1.1231(2) 0.66292(12) 0.12036(8) 0.0187(3) Uani 1 1 d . . . H4BA H 1.1951 0.7002 0.0913 0.022 Uiso 1 1 calc R . . C5B C 1.2102(2) 0.60705(12) 0.17112(8) 0.0177(3) Uani 1 1 d . . . C6B C 1.4051(2) 0.62261(15) 0.17689(10) 0.0270(4) Uani 1 1 d . . . H6BA H 1.4375 0.6418 0.2245 0.040 Uiso 1 1 calc R . . H6BB H 1.4390 0.6728 0.1444 0.040 Uiso 1 1 calc R . . H6BC H 1.4660 0.5633 0.1655 0.040 Uiso 1 1 calc R . . C7B C 1.2327(2) 0.49691(13) 0.26632(9) 0.0220(4) Uani 1 1 d . . . H7BA H 1.3561 0.4887 0.2509 0.026 Uiso 1 1 calc R . . C8B C 1.1559(3) 0.39970(14) 0.27964(11) 0.0316(4) Uani 1 1 d . . . H8BA H 1.1553 0.3623 0.2365 0.047 Uiso 1 1 calc R . . H8BB H 1.0354 0.4067 0.2956 0.047 Uiso 1 1 calc R . . H8BC H 1.2270 0.3669 0.3155 0.047 Uiso 1 1 calc R . . C9B C 1.2352(3) 0.55639(16) 0.33217(10) 0.0305(4) Uani 1 1 d . . . H9BA H 1.2816 0.6200 0.3221 0.046 Uiso 1 1 calc R . . H9BB H 1.3100 0.5255 0.3677 0.046 Uiso 1 1 calc R . . H9BC H 1.1156 0.5622 0.3492 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.01493(9) 0.01528(10) 0.01440(10) 0.00140(7) 0.00035(6) -0.00060(7) O1A 0.0217(5) 0.0141(5) 0.0164(6) 0.0006(4) 0.0025(4) -0.0029(4) O2A 0.0261(6) 0.0153(5) 0.0144(5) -0.0010(4) 0.0027(5) -0.0048(4) O1B 0.0161(5) 0.0197(6) 0.0178(6) 0.0043(5) -0.0003(4) -0.0016(4) O2B 0.0187(5) 0.0202(6) 0.0166(6) 0.0054(5) 0.0002(4) 0.0002(4) N1A 0.0205(6) 0.0153(6) 0.0147(6) -0.0016(5) 0.0003(5) 0.0009(5) N1B 0.0157(6) 0.0187(7) 0.0155(6) 0.0008(5) -0.0011(5) 0.0029(5) C1A 0.0442(11) 0.0272(10) 0.0213(9) -0.0064(8) 0.0057(8) -0.0074(8) C2A 0.0286(9) 0.0174(8) 0.0204(8) -0.0041(7) 0.0017(7) -0.0034(7) C3A 0.0142(7) 0.0156(7) 0.0154(7) 0.0014(6) -0.0001(6) 0.0013(6) C4A 0.0178(7) 0.0138(7) 0.0174(8) 0.0033(6) 0.0006(6) -0.0012(6) C5A 0.0168(7) 0.0127(7) 0.0204(8) 0.0009(6) -0.0018(6) 0.0027(6) C6A 0.0329(9) 0.0158(8) 0.0217(9) -0.0016(7) 0.0004(7) -0.0034(7) C7A 0.0340(9) 0.0192(8) 0.0165(8) -0.0050(7) 0.0026(7) -0.0025(7) C8A 0.0351(10) 0.0448(12) 0.0242(10) -0.0106(9) 0.0087(8) -0.0004(9) C9A 0.0413(11) 0.0335(11) 0.0204(9) -0.0040(8) -0.0076(8) -0.0022(9) C1B 0.0322(10) 0.0372(11) 0.0337(11) 0.0158(9) -0.0061(8) 0.0048(8) C2B 0.0206(8) 0.0277(9) 0.0232(9) 0.0065(7) -0.0045(7) 0.0004(7) C3B 0.0216(7) 0.0137(7) 0.0121(7) -0.0010(6) 0.0015(6) 0.0001(6) C4B 0.0184(7) 0.0215(8) 0.0163(8) 0.0029(6) 0.0040(6) -0.0016(6) C5B 0.0153(7) 0.0207(8) 0.0173(8) -0.0025(6) 0.0019(6) 0.0010(6) C6B 0.0158(8) 0.0344(10) 0.0308(10) 0.0058(8) 0.0025(7) -0.0004(7) C7B 0.0175(7) 0.0264(9) 0.0218(9) 0.0045(7) -0.0027(6) 0.0045(6) C8B 0.0278(9) 0.0287(10) 0.0380(11) 0.0129(8) -0.0041(8) 0.0041(8) C9B 0.0304(9) 0.0408(11) 0.0201(9) 0.0026(8) -0.0053(7) 0.0043(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O1B 1.9454(11) . ? Zn N1A 1.9475(14) . ? Zn N1B 1.9491(13) . ? Zn O1A 1.9572(11) . ? O1A C3A 1.2578(19) . ? O2A C3A 1.3453(19) . ? O2A C2A 1.432(2) . ? O1B C3B 1.2550(19) . ? O2B C3B 1.3426(19) . ? O2B C2B 1.432(2) . ? N1A C5A 1.312(2) . ? N1A C7A 1.465(2) . ? N1B C5B 1.304(2) . ? N1B C7B 1.465(2) . ? C1A C2A 1.497(2) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C4A 1.381(2) . ? C4A C5A 1.404(2) . ? C4A H4AA 0.9500 . ? C5A C6A 1.499(2) . ? C6A H6AA 0.9800 . ? C6A H6AB 0.9800 . ? C6A H6AC 0.9800 . ? C7A C8A 1.512(3) . ? C7A C9A 1.512(3) . ? C7A H7AA 1.0000 . ? C8A H8AA 0.9800 . ? C8A H8AB 0.9800 . ? C8A H8AC 0.9800 . ? C9A H9AA 0.9800 . ? C9A H9AB 0.9800 . ? C9A H9AC 0.9800 . ? C1B C2B 1.485(2) . ? C1B H1BA 0.9800 . ? C1B H1BB 0.9800 . ? C1B H1BC 0.9800 . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B C4B 1.380(2) . ? C4B C5B 1.405(2) . ? C4B H4BA 0.9500 . ? C5B C6B 1.503(2) . ? C6B H6BA 0.9800 . ? C6B H6BB 0.9800 . ? C6B H6BC 0.9800 . ? C7B C8B 1.508(3) . ? C7B C9B 1.515(3) . ? C7B H7BA 1.0000 . ? C8B H8BA 0.9800 . ? C8B H8BB 0.9800 . ? C8B H8BC 0.9800 . ? C9B H9BA 0.9800 . ? C9B H9BB 0.9800 . ? C9B H9BC 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1B Zn N1A 111.77(5) . . ? O1B Zn N1B 97.85(5) . . ? N1A Zn N1B 129.30(6) . . ? O1B Zn O1A 110.97(5) . . ? N1A Zn O1A 96.64(5) . . ? N1B Zn O1A 110.29(5) . . ? C3A O1A Zn 119.29(10) . . ? C3A O2A C2A 116.49(13) . . ? C3B O1B Zn 120.07(10) . . ? C3B O2B C2B 116.87(13) . . ? C5A N1A C7A 120.64(14) . . ? C5A N1A Zn 121.39(11) . . ? C7A N1A Zn 117.97(11) . . ? C5B N1B C7B 119.79(14) . . ? C5B N1B Zn 121.65(11) . . ? C7B N1B Zn 118.36(11) . . ? C2A C1A H1AA 109.5 . . ? C2A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? C2A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? O2A C2A C1A 107.85(14) . . ? O2A C2A H2AA 110.1 . . ? C1A C2A H2AA 110.1 . . ? O2A C2A H2AB 110.1 . . ? C1A C2A H2AB 110.1 . . ? H2AA C2A H2AB 108.5 . . ? O1A C3A O2A 117.35(14) . . ? O1A C3A C4A 128.08(15) . . ? O2A C3A C4A 114.56(14) . . ? C3A C4A C5A 126.58(15) . . ? C3A C4A H4AA 116.7 . . ? C5A C4A H4AA 116.7 . . ? N1A C5A C4A 124.07(15) . . ? N1A C5A C6A 120.80(15) . . ? C4A C5A C6A 115.12(14) . . ? C5A C6A H6AA 109.5 . . ? C5A C6A H6AB 109.5 . . ? H6AA C6A H6AB 109.5 . . ? C5A C6A H6AC 109.5 . . ? H6AA C6A H6AC 109.5 . . ? H6AB C6A H6AC 109.5 . . ? N1A C7A C8A 109.42(15) . . ? N1A C7A C9A 110.49(15) . . ? C8A C7A C9A 110.85(16) . . ? N1A C7A H7AA 108.7 . . ? C8A C7A H7AA 108.7 . . ? C9A C7A H7AA 108.7 . . ? C7A C8A H8AA 109.5 . . ? C7A C8A H8AB 109.5 . . ? H8AA C8A H8AB 109.5 . . ? C7A C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? C7A C9A H9AA 109.5 . . ? C7A C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C7A C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C2B C1B H1BA 109.5 . . ? C2B C1B H1BB 109.5 . . ? H1BA C1B H1BB 109.5 . . ? C2B C1B H1BC 109.5 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? O2B C2B C1B 106.94(15) . . ? O2B C2B H2BA 110.3 . . ? C1B C2B H2BA 110.3 . . ? O2B C2B H2BB 110.3 . . ? C1B C2B H2BB 110.3 . . ? H2BA C2B H2BB 108.6 . . ? O1B C3B O2B 117.52(14) . . ? O1B C3B C4B 128.64(15) . . ? O2B C3B C4B 113.84(14) . . ? C3B C4B C5B 127.11(15) . . ? C3B C4B H4BA 116.4 . . ? C5B C4B H4BA 116.4 . . ? N1B C5B C4B 124.07(15) . . ? N1B C5B C6B 121.16(15) . . ? C4B C5B C6B 114.77(15) . . ? C5B C6B H6BA 109.5 . . ? C5B C6B H6BB 109.5 . . ? H6BA C6B H6BB 109.5 . . ? C5B C6B H6BC 109.5 . . ? H6BA C6B H6BC 109.5 . . ? H6BB C6B H6BC 109.5 . . ? N1B C7B C8B 110.53(14) . . ? N1B C7B C9B 109.82(14) . . ? C8B C7B C9B 110.63(16) . . ? N1B C7B H7BA 108.6 . . ? C8B C7B H7BA 108.6 . . ? C9B C7B H7BA 108.6 . . ? C7B C8B H8BA 109.5 . . ? C7B C8B H8BB 109.5 . . ? H8BA C8B H8BB 109.5 . . ? C7B C8B H8BC 109.5 . . ? H8BA C8B H8BC 109.5 . . ? H8BB C8B H8BC 109.5 . . ? C7B C9B H9BA 109.5 . . ? C7B C9B H9BB 109.5 . . ? H9BA C9B H9BB 109.5 . . ? C7B C9B H9BC 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? 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 O1B Zn O1A C3A 137.33(11) . . . . ? N1A Zn O1A C3A 20.94(12) . . . . ? N1B Zn O1A C3A -115.35(12) . . . . ? N1A Zn O1B C3B -130.32(12) . . . . ? N1B Zn O1B C3B 7.72(13) . . . . ? O1A Zn O1B C3B 123.04(12) . . . . ? O1B Zn N1A C5A -130.18(12) . . . . ? N1B Zn N1A C5A 108.69(13) . . . . ? O1A Zn N1A C5A -14.43(13) . . . . ? O1B Zn N1A C7A 50.62(13) . . . . ? N1B Zn N1A C7A -70.52(14) . . . . ? O1A Zn N1A C7A 166.36(12) . . . . ? O1B Zn N1B C5B -5.17(14) . . . . ? N1A Zn N1B C5B 121.47(13) . . . . ? O1A Zn N1B C5B -121.02(13) . . . . ? O1B Zn N1B C7B 169.71(12) . . . . ? N1A Zn N1B C7B -63.65(14) . . . . ? O1A Zn N1B C7B 53.86(13) . . . . ? C3A O2A C2A C1A -165.32(14) . . . . ? Zn O1A C3A O2A 164.62(10) . . . . ? Zn O1A C3A C4A -16.4(2) . . . . ? C2A O2A C3A O1A 5.5(2) . . . . ? C2A O2A C3A C4A -173.67(14) . . . . ? O1A C3A C4A C5A -1.6(3) . . . . ? O2A C3A C4A C5A 177.45(14) . . . . ? C7A N1A C5A C4A -178.59(15) . . . . ? Zn N1A C5A C4A 2.2(2) . . . . ? C7A N1A C5A C6A 1.6(2) . . . . ? Zn N1A C5A C6A -177.62(11) . . . . ? C3A C4A C5A N1A 9.9(3) . . . . ? C3A C4A C5A C6A -170.21(16) . . . . ? C5A N1A C7A C8A -140.80(17) . . . . ? Zn N1A C7A C8A 38.42(18) . . . . ? C5A N1A C7A C9A 96.88(19) . . . . ? Zn N1A C7A C9A -83.90(16) . . . . ? C3B O2B C2B C1B -172.44(15) . . . . ? Zn O1B C3B O2B 175.42(10) . . . . ? Zn O1B C3B C4B -5.2(2) . . . . ? C2B O2B C3B O1B 0.9(2) . . . . ? C2B O2B C3B C4B -178.57(14) . . . . ? O1B C3B C4B C5B -2.6(3) . . . . ? O2B C3B C4B C5B 176.78(16) . . . . ? C7B N1B C5B C4B -175.13(16) . . . . ? Zn N1B C5B C4B -0.3(2) . . . . ? C7B N1B C5B C6B 4.5(2) . . . . ? Zn N1B C5B C6B 179.30(13) . . . . ? C3B C4B C5B N1B 5.8(3) . . . . ? C3B C4B C5B C6B -173.83(17) . . . . ? C5B N1B C7B C8B -149.88(16) . . . . ? Zn N1B C7B C8B 35.15(18) . . . . ? C5B N1B C7B C9B 87.78(19) . . . . ? Zn N1B C7B C9B -87.19(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C6A H6AC O1A 0.98 2.46 3.333(2) 148.6 2_645 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.402 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.061