# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email thzhou@fjirsm.ac.cn _publ_contact_author_name 'Tian-Hua Zhou' _publ_author_name 'Jiang-Gao Mao' data_1P _database_code_depnum_ccdc_archive 'CCDC 825906' #TrackingRef '1P AND 1M.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 As N3 O5 Zn' _chemical_formula_weight 494.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.806(2) _cell_length_b 9.5007(15) _cell_length_c 11.490(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.951(14) _cell_angle_gamma 90.00 _cell_volume 891.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2868 _cell_measurement_theta_min 2.1416 _cell_measurement_theta_max 27.4797 _exptl_crystal_description needles _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.081 _exptl_crystal_size_min 0.023 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 3.257 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6109 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Mercury2 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number 2168 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7042 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _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 2.87 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3804 _reflns_number_gt 3581 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.021(12) _refine_ls_number_reflns 3804 _refine_ls_number_parameters 253 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.12986(4) 0.78061(4) -0.60432(3) 0.02467(10) Uani 1 1 d . . . Zn1 Zn 0.00680(5) 0.60344(4) -0.41757(4) 0.02564(11) Uani 1 1 d . . . O1 O 0.1726(3) 0.6681(3) -0.4854(2) 0.0291(6) Uani 1 1 d . . . O2 O -0.0110(3) 0.8994(3) -0.6111(3) 0.0314(7) Uani 1 1 d . . . O3 O 0.3136(4) 0.8609(3) -0.5868(3) 0.0384(7) Uani 1 1 d . . . H3B H 0.2956 0.9382 -0.6209 0.058 Uiso 1 1 calc R . . O4 O 0.1173(3) 0.2502(3) -0.6335(2) 0.0339(7) Uani 1 1 d . . . O5 O 0.2851(4) 0.1147(4) -0.6925(3) 0.0480(8) Uani 1 1 d . . . N1 N 0.2609(4) 0.4945(4) -0.6707(3) 0.0330(8) Uani 1 1 d . . . H1A H 0.3016 0.5437 -0.6032 0.040 Uiso 1 1 calc R . . N2 N 0.2018(4) 0.6169(4) -0.2245(3) 0.0279(7) Uani 1 1 d . . . C1 C 0.0580(5) 0.6781(4) -0.7578(4) 0.0280(9) Uani 1 1 d . . . C6 C -0.0725(5) 0.7347(5) -0.8579(4) 0.0338(10) Uani 1 1 d . . . H6A H -0.1178 0.8204 -0.8489 0.041 Uiso 1 1 calc R . . C5 C -0.1350(6) 0.6621(5) -0.9720(4) 0.0395(11) Uani 1 1 d . . . H5A H -0.2200 0.7001 -1.0401 0.047 Uiso 1 1 calc R . . C4 C -0.0684(6) 0.5332(5) -0.9815(4) 0.0407(11) Uani 1 1 d . . . H4A H -0.1110 0.4838 -1.0567 0.049 Uiso 1 1 calc R . . C3 C 0.0592(6) 0.4758(5) -0.8830(4) 0.0361(10) Uani 1 1 d . . . H3A H 0.1004 0.3885 -0.8929 0.043 Uiso 1 1 calc R . . C2 C 0.1284(5) 0.5463(4) -0.7677(4) 0.0294(9) Uani 1 1 d . . . C7 C 0.3357(5) 0.3600(4) -0.6769(4) 0.0332(10) Uani 1 1 d . . . H7A H 0.4425 0.3562 -0.6095 0.040 Uiso 1 1 calc R . . H7B H 0.3529 0.3556 -0.7555 0.040 Uiso 1 1 calc R . . C8 C 0.2375(5) 0.2290(4) -0.6677(4) 0.0289(9) Uani 1 1 d . . . C9 C 0.1694(5) 0.6642(5) -0.1276(4) 0.0329(10) Uani 1 1 d . . . H9A H 0.0671 0.7039 -0.1433 0.039 Uiso 1 1 calc R . . C10 C 0.2790(5) 0.6579(5) -0.0048(3) 0.0314(9) Uani 1 1 d . . . H10A H 0.2508 0.6948 0.0594 0.038 Uiso 1 1 calc R . . C11 C 0.4314(4) 0.5963(5) 0.0226(3) 0.0268(8) Uani 1 1 d . . . C12 C 0.4656(6) 0.5461(5) -0.0787(4) 0.0417(12) Uani 1 1 d . . . H12A H 0.5657 0.5035 -0.0654 0.050 Uiso 1 1 calc R . . C13 C 0.3505(6) 0.5597(5) -0.1994(4) 0.0394(12) Uani 1 1 d . . . H13A H 0.3771 0.5280 -0.2660 0.047 Uiso 1 1 calc R . . C14 C 0.5546(5) 0.5914(5) 0.1540(3) 0.0295(9) Uani 1 1 d . . . C15 C 0.5587(5) 0.6937(5) 0.2399(4) 0.0352(10) Uani 1 1 d . . . H15A H 0.4789 0.7634 0.2190 0.042 Uiso 1 1 calc R . . C18 C 0.6716(5) 0.4847(5) 0.1935(4) 0.0319(10) Uani 1 1 d . . . H18A H 0.6707 0.4111 0.1399 0.038 Uiso 1 1 calc R . . C16 C 0.6833(5) 0.6920(5) 0.3583(4) 0.0359(10) Uani 1 1 d . . . H16A H 0.6867 0.7640 0.4140 0.043 Uiso 1 1 calc R . . N3 N 0.7979(4) 0.5922(4) 0.3959(3) 0.0296(7) Uani 1 1 d . . . C17 C 0.7895(5) 0.4903(5) 0.3141(4) 0.0326(9) Uani 1 1 d . . . H17B H 0.8671 0.4187 0.3392 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 As1 0.0290(2) 0.0200(2) 0.02200(17) 0.00003(18) 0.00601(15) -0.00050(17) Zn1 0.0288(2) 0.0228(2) 0.0215(2) 0.00097(19) 0.00496(17) 0.00003(19) O1 0.0340(15) 0.0294(16) 0.0226(12) 0.0045(12) 0.0090(12) 0.0005(12) O2 0.0287(15) 0.0233(16) 0.0362(15) -0.0024(13) 0.0052(13) 0.0027(12) O3 0.0326(16) 0.0296(17) 0.0470(18) 0.0067(14) 0.0081(14) -0.0025(13) O4 0.0284(15) 0.038(2) 0.0318(14) 0.0039(13) 0.0073(12) -0.0046(13) O5 0.067(2) 0.0240(18) 0.059(2) -0.0008(17) 0.0304(18) -0.0016(17) N1 0.0364(19) 0.024(2) 0.0343(19) -0.0025(16) 0.0083(16) -0.0008(16) N2 0.0285(16) 0.029(2) 0.0194(14) -0.0031(15) 0.0010(13) -0.0024(15) C1 0.035(2) 0.024(2) 0.0245(18) 0.0027(16) 0.0103(17) -0.0029(17) C6 0.042(2) 0.029(2) 0.0268(19) 0.0047(17) 0.0084(19) 0.0003(18) C5 0.050(3) 0.041(3) 0.0213(18) 0.0080(19) 0.0070(19) -0.005(2) C4 0.054(3) 0.042(3) 0.025(2) -0.004(2) 0.014(2) -0.014(2) C3 0.045(3) 0.031(3) 0.035(2) -0.008(2) 0.018(2) -0.0067(19) C2 0.036(2) 0.025(2) 0.027(2) -0.0026(16) 0.0113(18) -0.0077(17) C7 0.033(2) 0.021(2) 0.046(3) 0.0008(19) 0.015(2) -0.0009(17) C8 0.032(2) 0.027(2) 0.0221(17) 0.0020(16) 0.0037(17) -0.0033(16) C9 0.025(2) 0.043(3) 0.0242(18) 0.0037(19) 0.0025(17) 0.0052(18) C10 0.034(2) 0.041(3) 0.0195(17) 0.0013(18) 0.0097(17) 0.0003(18) C11 0.0278(19) 0.026(2) 0.0204(17) -0.0017(18) 0.0019(15) -0.0024(18) C12 0.035(2) 0.055(3) 0.027(2) -0.009(2) 0.0024(19) 0.012(2) C13 0.037(2) 0.051(3) 0.025(2) -0.006(2) 0.0054(19) 0.011(2) C14 0.0271(19) 0.031(2) 0.0250(18) 0.0002(19) 0.0037(15) -0.0015(18) C15 0.035(2) 0.035(2) 0.0253(19) -0.0026(18) -0.0011(18) 0.0065(19) C18 0.039(2) 0.026(2) 0.0211(19) -0.0027(17) -0.0002(18) -0.0005(18) C16 0.042(2) 0.032(2) 0.0233(18) -0.0048(18) 0.0010(18) 0.006(2) N3 0.0296(16) 0.0305(19) 0.0203(14) 0.0006(16) -0.0002(13) 0.0003(16) C17 0.031(2) 0.035(3) 0.0257(19) 0.0003(18) 0.0034(17) 0.0015(18) _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 As1 O2 1.657(3) . ? As1 O1 1.663(3) . ? As1 O3 1.732(3) . ? As1 C1 1.904(4) . ? Zn1 O2 1.964(3) 2_544 ? Zn1 O4 1.991(3) 2_554 ? Zn1 O1 1.991(3) . ? Zn1 N2 2.245(3) . ? Zn1 N3 2.245(3) 1_454 ? O2 Zn1 1.964(3) 2_554 ? O3 H3B 0.8200 . ? O4 C8 1.276(5) . ? O4 Zn1 1.991(3) 2_544 ? O5 C8 1.236(5) . ? N1 C2 1.369(5) . ? N1 C7 1.452(5) . ? N1 H1A 0.8600 . ? N2 C9 1.327(5) . ? N2 C13 1.346(5) . ? C1 C6 1.394(5) . ? C1 C2 1.421(6) . ? C6 C5 1.398(6) . ? C6 H6A 0.9300 . ? C5 C4 1.380(7) . ? C5 H5A 0.9300 . ? C4 C3 1.375(6) . ? C4 H4A 0.9300 . ? C3 C2 1.404(6) . ? C3 H3A 0.9300 . ? C7 C8 1.542(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C10 1.382(5) . ? C9 H9A 0.9300 . ? C10 C11 1.389(6) . ? C10 H10A 0.9300 . ? C11 C12 1.391(6) . ? C11 C14 1.494(5) . ? C12 C13 1.384(6) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.376(6) . ? C14 C18 1.395(6) . ? C15 C16 1.392(5) . ? C15 H15A 0.9300 . ? C18 C17 1.388(5) . ? C18 H18A 0.9300 . ? C16 N3 1.333(5) . ? C16 H16A 0.9300 . ? N3 C17 1.332(5) . ? N3 Zn1 2.245(3) 1_656 ? C17 H17B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 As1 O1 114.30(15) . . ? O2 As1 O3 110.85(15) . . ? O1 As1 O3 105.85(14) . . ? O2 As1 C1 108.73(16) . . ? O1 As1 C1 109.12(16) . . ? O3 As1 C1 107.78(16) . . ? O2 Zn1 O4 128.32(13) 2_544 2_554 ? O2 Zn1 O1 113.56(12) 2_544 . ? O4 Zn1 O1 117.54(12) 2_554 . ? O2 Zn1 N2 86.06(12) 2_544 . ? O4 Zn1 N2 88.29(12) 2_554 . ? O1 Zn1 N2 88.12(11) . . ? O2 Zn1 N3 94.04(13) 2_544 1_454 ? O4 Zn1 N3 88.31(12) 2_554 1_454 ? O1 Zn1 N3 95.73(11) . 1_454 ? N2 Zn1 N3 175.74(13) . 1_454 ? As1 O1 Zn1 123.11(15) . . ? As1 O2 Zn1 134.23(17) . 2_554 ? As1 O3 H3B 109.5 . . ? C8 O4 Zn1 126.2(3) . 2_544 ? C2 N1 C7 122.7(4) . . ? C2 N1 H1A 118.6 . . ? C7 N1 H1A 118.6 . . ? C9 N2 C13 117.0(3) . . ? C9 N2 Zn1 121.6(3) . . ? C13 N2 Zn1 120.8(3) . . ? C6 C1 C2 121.6(4) . . ? C6 C1 As1 116.9(3) . . ? C2 C1 As1 121.4(3) . . ? C1 C6 C5 119.8(4) . . ? C1 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C4 C5 C6 118.8(4) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? C3 C4 C5 121.8(4) . . ? C3 C4 H4A 119.1 . . ? C5 C4 H4A 119.1 . . ? C4 C3 C2 121.4(4) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? N1 C2 C3 122.3(4) . . ? N1 C2 C1 121.1(4) . . ? C3 C2 C1 116.5(4) . . ? N1 C7 C8 115.5(3) . . ? N1 C7 H7A 108.4 . . ? C8 C7 H7A 108.4 . . ? N1 C7 H7B 108.4 . . ? C8 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? O5 C8 O4 127.0(4) . . ? O5 C8 C7 116.5(4) . . ? O4 C8 C7 116.4(4) . . ? N2 C9 C10 123.7(4) . . ? N2 C9 H9A 118.1 . . ? C10 C9 H9A 118.1 . . ? C9 C10 C11 119.8(4) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C10 C11 C12 116.6(3) . . ? C10 C11 C14 121.1(3) . . ? C12 C11 C14 122.2(4) . . ? C13 C12 C11 120.0(4) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? N2 C13 C12 122.8(4) . . ? N2 C13 H13A 118.6 . . ? C12 C13 H13A 118.6 . . ? C15 C14 C18 117.5(4) . . ? C15 C14 C11 121.1(4) . . ? C18 C14 C11 121.4(4) . . ? C14 C15 C16 119.5(4) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C17 C18 C14 118.9(4) . . ? C17 C18 H18A 120.6 . . ? C14 C18 H18A 120.6 . . ? N3 C16 C15 123.3(4) . . ? N3 C16 H16A 118.3 . . ? C15 C16 H16A 118.3 . . ? C17 N3 C16 116.9(3) . . ? C17 N3 Zn1 121.2(3) . 1_656 ? C16 N3 Zn1 121.8(3) . 1_656 ? N3 C17 C18 123.8(4) . . ? N3 C17 H17B 118.1 . . ? C18 C17 H17B 118.1 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.424 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.082 #===END data_1M _database_code_depnum_ccdc_archive 'CCDC 825907' #TrackingRef '1P AND 1M.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 As N3 O5 Zn' _chemical_formula_weight 494.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.806(2) _cell_length_b 9.5007(15) _cell_length_c 11.490(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.951(14) _cell_angle_gamma 90.00 _cell_volume 891.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2935 _cell_measurement_theta_min 2.1443 _cell_measurement_theta_max 27.4680 _exptl_crystal_description needles _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.432 _exptl_crystal_size_mid 0.067 _exptl_crystal_size_min 0.061 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 3.257 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5351 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Mercury2 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number 2158 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7003 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _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 2.49 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3787 _reflns_number_gt 3581 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+1.7735P] 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 0.002(14) _refine_ls_number_reflns 3787 _refine_ls_number_parameters 257 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 0.669 _refine_ls_restrained_S_all 0.669 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.002 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 As1 As 0.86993(5) 0.21927(4) 1.60433(4) 0.02577(11) Uani 1 1 d . . . Zn1 Zn 0.99306(6) 0.39648(5) 1.41758(4) 0.02682(12) Uani 1 1 d . . . O1 O 0.8258(4) 0.3327(4) 1.4849(3) 0.0323(7) Uani 1 1 d . . . O2 O 1.0110(4) 0.1001(3) 1.6112(3) 0.0344(7) Uani 1 1 d . . . O3 O 0.6855(4) 0.1397(4) 1.5871(4) 0.0392(8) Uani 1 1 d . . . H3B H 0.7032 0.0623 1.6212 0.059 Uiso 1 1 calc R . . O4 O 0.8821(4) 0.7504(4) 1.6335(3) 0.0353(8) Uani 1 1 d . . . O5 O 0.7150(5) 0.8863(4) 1.6918(4) 0.0497(9) Uani 1 1 d . . . N1 N 0.7379(5) 0.5051(4) 1.6703(4) 0.0343(9) Uani 1 1 d . . . N2 N 0.7978(4) 0.3842(4) 1.2249(3) 0.0289(8) Uani 1 1 d . . . C1 C 0.9434(6) 0.3224(5) 1.7581(4) 0.0275(9) Uani 1 1 d . . . C6 C 1.0731(6) 0.2663(5) 1.8584(4) 0.0351(10) Uani 1 1 d . . . H6A H 1.1183 0.1803 1.8498 0.042 Uiso 1 1 calc R . . C5 C 1.1348(7) 0.3384(6) 1.9712(4) 0.0410(12) Uani 1 1 d . . . H5A H 1.2200 0.3001 2.0390 0.049 Uiso 1 1 calc R . . C4 C 1.0690(7) 0.4677(6) 1.9825(5) 0.0431(12) Uani 1 1 d . . . H4A H 1.1118 0.5169 2.0577 0.052 Uiso 1 1 calc R . . C3 C 0.9404(7) 0.5243(5) 1.8829(5) 0.0377(11) Uani 1 1 d . . . H3A H 0.8982 0.6113 1.8926 0.045 Uiso 1 1 calc R . . C2 C 0.8720(6) 0.4538(5) 1.7677(4) 0.0294(9) Uani 1 1 d . . . C7 C 0.6653(6) 0.6394(5) 1.6769(5) 0.0344(10) Uani 1 1 d . . . H7A H 0.6485 0.6438 1.7556 0.041 Uiso 1 1 calc R . . H7B H 0.5583 0.6436 1.6097 0.041 Uiso 1 1 calc R . . C8 C 0.7621(5) 0.7699(5) 1.6676(4) 0.0304(9) Uani 1 1 d . . . C9 C 0.8304(6) 0.3368(6) 1.1277(4) 0.0347(10) Uani 1 1 d . . . H9A H 0.9332 0.2981 1.1433 0.042 Uiso 1 1 calc R . . C10 C 0.7203(5) 0.3417(5) 1.0046(4) 0.0308(9) Uani 1 1 d . . . H10A H 0.7482 0.3037 0.9407 0.037 Uiso 1 1 calc R . . C11 C 0.5681(5) 0.4035(5) 0.9772(4) 0.0296(8) Uani 1 1 d . . . C12 C 0.5343(6) 0.4537(6) 1.0785(4) 0.0403(12) Uani 1 1 d . . . H12A H 0.4341 0.4962 1.0652 0.048 Uiso 1 1 calc R . . C13 C 0.6504(6) 0.4404(6) 1.1999(5) 0.0398(12) Uani 1 1 d . . . H13A H 0.6238 0.4722 1.2665 0.048 Uiso 1 1 calc R . . C14 C 0.4451(5) 0.4096(5) 0.8460(4) 0.0309(9) Uani 1 1 d . . . C15 C 0.4408(6) 0.3057(6) 0.7597(4) 0.0369(11) Uani 1 1 d . . . H15A H 0.5201 0.2355 0.7810 0.044 Uiso 1 1 calc R . . C18 C 0.3286(6) 0.5155(5) 0.8069(4) 0.0352(11) Uani 1 1 d . . . H18A H 0.3296 0.5888 0.8608 0.042 Uiso 1 1 calc R . . C16 C 0.3170(6) 0.3077(6) 0.6415(4) 0.0384(11) Uani 1 1 d . . . H16A H 0.3135 0.2358 0.5857 0.046 Uiso 1 1 calc R . . N3 N 0.2019(4) 0.4088(5) 0.6040(3) 0.0313(8) Uani 1 1 d . . . C17 C 0.2095(6) 0.5107(5) 0.6857(4) 0.0334(10) Uani 1 1 d . . . H17B H 0.1317 0.5821 0.6607 0.040 Uiso 1 1 calc R . . H1A H 0.727(7) 0.467(7) 1.595(5) 0.038(15) 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 As1 0.0275(2) 0.0240(2) 0.02326(19) 0.00038(18) 0.00651(15) -0.00049(16) Zn1 0.0272(2) 0.0269(2) 0.0233(2) 0.00103(19) 0.00597(18) -0.00025(18) O1 0.0333(16) 0.0357(18) 0.0284(15) 0.0046(13) 0.0121(13) -0.0002(13) O2 0.0308(17) 0.0258(17) 0.0411(17) -0.0007(15) 0.0071(14) -0.0003(12) O3 0.0279(16) 0.0367(19) 0.048(2) 0.0061(16) 0.0080(15) -0.0009(13) O4 0.0311(16) 0.040(2) 0.0300(15) 0.0046(14) 0.0062(12) -0.0039(13) O5 0.065(2) 0.030(2) 0.063(2) -0.0013(19) 0.034(2) 0.0003(18) N1 0.033(2) 0.029(2) 0.039(2) -0.0023(18) 0.0112(17) 0.0008(16) N2 0.0257(17) 0.036(2) 0.0187(15) -0.0008(15) 0.0013(13) -0.0029(16) C1 0.034(2) 0.026(2) 0.0226(19) 0.0007(16) 0.0107(17) -0.0035(17) C6 0.041(3) 0.033(2) 0.029(2) 0.0049(18) 0.011(2) -0.0004(19) C5 0.053(3) 0.042(3) 0.021(2) 0.007(2) 0.006(2) -0.007(2) C4 0.051(3) 0.051(3) 0.025(2) -0.006(2) 0.012(2) -0.015(3) C3 0.048(3) 0.033(3) 0.036(2) -0.010(2) 0.021(2) -0.005(2) C2 0.037(2) 0.026(2) 0.027(2) 0.0007(16) 0.0143(18) -0.0031(17) C7 0.031(2) 0.029(2) 0.046(3) 0.002(2) 0.017(2) 0.0026(18) C8 0.030(2) 0.031(2) 0.028(2) 0.0027(17) 0.0078(17) -0.0005(17) C9 0.025(2) 0.049(3) 0.027(2) 0.003(2) 0.0070(17) 0.0032(19) C10 0.027(2) 0.042(3) 0.0215(19) 0.0000(18) 0.0065(16) 0.0002(18) C11 0.0260(19) 0.032(2) 0.0253(19) -0.0027(19) 0.0030(16) -0.0025(18) C12 0.032(2) 0.055(3) 0.026(2) -0.010(2) 0.0010(19) 0.012(2) C13 0.032(2) 0.056(3) 0.025(2) -0.007(2) 0.0031(18) 0.013(2) C14 0.0252(19) 0.037(2) 0.026(2) -0.001(2) 0.0043(16) -0.0007(18) C15 0.035(2) 0.040(3) 0.028(2) -0.004(2) 0.0030(19) 0.007(2) C18 0.039(3) 0.033(3) 0.027(2) -0.0056(19) 0.0038(19) -0.0018(19) C16 0.040(3) 0.039(3) 0.026(2) -0.0005(19) -0.0004(19) 0.007(2) N3 0.0290(17) 0.036(2) 0.0217(16) 0.0008(17) 0.0016(13) -0.0004(16) C17 0.032(2) 0.035(3) 0.026(2) 0.0024(18) 0.0025(17) 0.0023(18) _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 As1 O2 1.661(3) . ? As1 O1 1.672(3) . ? As1 O3 1.735(3) . ? As1 C1 1.909(4) . ? Zn1 O2 1.960(3) 2_758 ? Zn1 O4 1.990(3) 2_748 ? Zn1 O1 1.997(3) . ? Zn1 N2 2.242(3) . ? Zn1 N3 2.245(3) 1_656 ? O2 Zn1 1.960(3) 2_748 ? O3 H3B 0.8200 . ? O4 C8 1.271(5) . ? O4 Zn1 1.990(3) 2_758 ? O5 C8 1.249(6) . ? N1 C2 1.378(6) . ? N1 C7 1.442(6) . ? N1 H1A 0.91(6) . ? N2 C9 1.332(6) . ? N2 C13 1.332(6) . ? C1 C6 1.390(6) . ? C1 C2 1.420(6) . ? C6 C5 1.385(7) . ? C6 H6A 0.9300 . ? C5 C4 1.385(8) . ? C5 H5A 0.9300 . ? C4 C3 1.383(8) . ? C4 H4A 0.9300 . ? C3 C2 1.403(6) . ? C3 H3A 0.9300 . ? C7 C8 1.531(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C10 1.384(6) . ? C9 H9A 0.9300 . ? C10 C11 1.387(6) . ? C10 H10A 0.9300 . ? C11 C12 1.389(6) . ? C11 C14 1.493(6) . ? C12 C13 1.393(6) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.389(7) . ? C14 C18 1.387(7) . ? C15 C16 1.388(6) . ? C15 H15A 0.9300 . ? C18 C17 1.396(6) . ? C18 H18A 0.9300 . ? C16 N3 1.345(6) . ? C16 H16A 0.9300 . ? N3 C17 1.333(6) . ? N3 Zn1 2.245(3) 1_454 ? C17 H17B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 As1 O1 114.73(17) . . ? O2 As1 O3 111.11(17) . . ? O1 As1 O3 105.48(17) . . ? O2 As1 C1 108.50(18) . . ? O1 As1 C1 108.84(18) . . ? O3 As1 C1 107.96(18) . . ? O2 Zn1 O4 128.01(15) 2_758 2_748 ? O2 Zn1 O1 113.28(14) 2_758 . ? O4 Zn1 O1 118.10(14) 2_748 . ? O2 Zn1 N2 85.76(15) 2_758 . ? O4 Zn1 N2 88.67(14) 2_748 . ? O1 Zn1 N2 87.84(13) . . ? O2 Zn1 N3 93.79(15) 2_758 1_656 ? O4 Zn1 N3 88.39(14) 2_748 1_656 ? O1 Zn1 N3 96.09(13) . 1_656 ? N2 Zn1 N3 175.88(14) . 1_656 ? As1 O1 Zn1 122.35(18) . . ? As1 O2 Zn1 134.30(19) . 2_748 ? As1 O3 H3B 109.5 . . ? C8 O4 Zn1 127.1(3) . 2_758 ? C2 N1 C7 122.2(4) . . ? C2 N1 H1A 113(4) . . ? C7 N1 H1A 121(4) . . ? C9 N2 C13 116.9(4) . . ? C9 N2 Zn1 121.3(3) . . ? C13 N2 Zn1 121.2(3) . . ? C6 C1 C2 121.5(4) . . ? C6 C1 As1 117.4(3) . . ? C2 C1 As1 121.1(3) . . ? C5 C6 C1 120.0(5) . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? C6 C5 C4 119.7(5) . . ? C6 C5 H5A 120.2 . . ? C4 C5 H5A 120.2 . . ? C3 C4 C5 120.6(5) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C4 C3 C2 121.7(5) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? N1 C2 C3 122.2(4) . . ? N1 C2 C1 121.2(4) . . ? C3 C2 C1 116.6(4) . . ? N1 C7 C8 116.3(4) . . ? N1 C7 H7A 108.2 . . ? C8 C7 H7A 108.2 . . ? N1 C7 H7B 108.2 . . ? C8 C7 H7B 108.2 . . ? H7A C7 H7B 107.4 . . ? O5 C8 O4 125.6(4) . . ? O5 C8 C7 117.5(4) . . ? O4 C8 C7 116.9(4) . . ? N2 C9 C10 123.9(4) . . ? N2 C9 H9A 118.1 . . ? C10 C9 H9A 118.1 . . ? C9 C10 C11 119.6(4) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C10 C11 C12 116.5(4) . . ? C10 C11 C14 121.4(4) . . ? C12 C11 C14 122.1(4) . . ? C11 C12 C13 120.1(4) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? N2 C13 C12 122.9(5) . . ? N2 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? C15 C14 C18 117.7(4) . . ? C15 C14 C11 120.6(4) . . ? C18 C14 C11 121.7(4) . . ? C16 C15 C14 119.4(5) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C14 C18 C17 119.2(4) . . ? C14 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? N3 C16 C15 123.1(5) . . ? N3 C16 H16A 118.5 . . ? C15 C16 H16A 118.5 . . ? C17 N3 C16 117.3(4) . . ? C17 N3 Zn1 121.2(3) . 1_454 ? C16 N3 Zn1 121.3(3) . 1_454 ? N3 C17 C18 123.2(4) . . ? N3 C17 H17B 118.4 . . ? C18 C17 H17B 118.4 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.435 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.083 #===END