# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 _journal_name_full CrystEngComm _journal_coden_Cambridge ? _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jiang-Gao Mao' _publ_contact_author_email mjg@fjirsm.ac.cn _publ_section_title ; Towards Rational Design of Zinc(II) and Cadmium(II) Sulfonate-Arsonates with Low Dimensional Aggregations ; loop_ _publ_author_name Fei-Yan Yi Hai-Bing Xu Tian-Hua Zhou data_1 _database_code_depnum_ccdc_archive 'CCDC 763188' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H9 As O9 S Zn2' _chemical_formula_weight 462.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7702(16) _cell_length_b 8.2854(10) _cell_length_c 11.1489(14) _cell_angle_alpha 90.00 _cell_angle_beta 95.420(10) _cell_angle_gamma 90.00 _cell_volume 1174.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2819 _cell_measurement_theta_min 3.0675 _cell_measurement_theta_max 27.4680 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 7.098 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7390 _exptl_absorpt_correction_T_max 1 _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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8697 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2688 _reflns_number_gt 2343 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0548P)^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 shelxtl _refine_ls_extinction_coef ? _refine_ls_number_reflns 2688 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.03824(3) 0.09534(4) 0.39175(3) 0.01446(13) Uani 1 1 d . . . Zn2 Zn -0.05466(3) 0.20912(5) 0.13113(3) 0.01263(12) Uani 1 1 d . . . As1 As -0.13112(3) 0.41846(4) 0.35127(3) 0.00980(11) Uani 1 1 d . . . S1 S -0.28455(7) 0.36419(13) 0.08019(8) 0.0220(2) Uani 1 1 d . . . C1 C -0.2764(3) 0.4823(4) 0.3131(3) 0.0151(7) Uani 1 1 d . . . C2 C -0.3311(3) 0.4796(4) 0.1972(3) 0.0178(7) Uani 1 1 d . . . C3 C -0.4298(3) 0.5495(5) 0.1768(4) 0.0292(9) Uani 1 1 d . . . H3A H -0.4648 0.5485 0.0998 0.035 Uiso 1 1 calc R . . C4 C -0.4767(3) 0.6210(6) 0.2709(4) 0.0340(10) Uani 1 1 d . . . H4A H -0.5424 0.6697 0.2568 0.041 Uiso 1 1 calc R . . C5 C -0.4252(3) 0.6194(6) 0.3856(4) 0.0320(10) Uani 1 1 d . . . H5A H -0.4574 0.6645 0.4491 0.038 Uiso 1 1 calc R . . C6 C -0.3252(3) 0.5506(5) 0.4074(3) 0.0213(8) Uani 1 1 d . . . H6A H -0.2913 0.5506 0.4849 0.026 Uiso 1 1 calc R . . O1 O -0.1099(2) 0.4365(3) 0.5012(2) 0.0157(5) Uani 1 1 d . . . O2 O -0.09406(19) 0.2323(3) 0.30711(19) 0.0140(5) Uani 1 1 d . . . O3 O -0.05503(19) 0.5562(3) 0.2884(2) 0.0144(5) Uani 1 1 d . . . O4 O -0.1703(2) 0.3994(3) 0.0858(2) 0.0174(5) Uani 1 1 d . . . O5 O -0.3009(3) 0.1973(4) 0.1139(3) 0.0438(9) Uani 1 1 d . . . O6 O -0.3395(3) 0.4145(5) -0.0310(3) 0.0494(10) Uani 1 1 d . . . O7 O 0.03723(19) 0.1177(3) 0.57621(19) 0.0129(5) Uani 1 1 d . . . H7A H 0.1084 0.1219 0.6175 0.015 Uiso 1 1 calc R . . O1W O 0.1462(2) 0.2766(3) 0.3960(2) 0.0247(6) Uani 1 1 d . . . H1WA H 0.1527 0.3088 0.3247 0.037 Uiso 1 1 d R . . H1WB H 0.1255 0.3545 0.4375 0.037 Uiso 1 1 d R . . O2W O 0.2378(3) 0.0795(4) 0.7109(3) 0.0448(9) Uani 1 1 d . . . H2WA H 0.2522 -0.0188 0.7267 0.067 Uiso 1 1 d R . . H2WB H 0.2902 0.1322 0.6900 0.067 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0231(3) 0.0100(2) 0.0107(2) -0.00078(13) 0.00350(17) -0.00090(15) Zn2 0.0184(2) 0.0087(2) 0.0108(2) -0.00008(13) 0.00206(16) 0.00022(14) As1 0.01322(19) 0.00715(18) 0.00924(18) 0.00034(11) 0.00215(13) 0.00039(12) S1 0.0157(5) 0.0337(5) 0.0166(4) -0.0087(4) 0.0021(3) -0.0032(4) C1 0.0127(16) 0.0110(17) 0.0221(17) 0.0006(13) 0.0038(13) 0.0017(13) C2 0.0168(17) 0.0191(19) 0.0175(16) -0.0030(13) 0.0021(14) -0.0026(14) C3 0.024(2) 0.034(2) 0.029(2) -0.0054(17) -0.0043(17) 0.0098(18) C4 0.022(2) 0.042(3) 0.037(2) -0.0069(19) 0.0009(18) 0.0144(19) C5 0.024(2) 0.039(3) 0.034(2) -0.0121(19) 0.0081(18) 0.0125(19) C6 0.0198(19) 0.026(2) 0.0184(17) -0.0039(14) 0.0053(15) 0.0011(16) O1 0.0221(13) 0.0143(12) 0.0107(11) 0.0011(9) 0.0015(10) -0.0003(10) O2 0.0225(13) 0.0088(11) 0.0112(11) 0.0011(8) 0.0037(9) 0.0043(10) O3 0.0198(13) 0.0117(12) 0.0115(11) 0.0004(9) 0.0006(10) -0.0036(10) O4 0.0148(13) 0.0174(14) 0.0201(12) 0.0001(9) 0.0023(10) 0.0003(10) O5 0.047(2) 0.0291(18) 0.060(2) -0.0217(15) 0.0277(16) -0.0197(15) O6 0.0262(18) 0.102(3) 0.0188(15) -0.0065(15) -0.0035(13) 0.0115(17) O7 0.0154(12) 0.0113(11) 0.0122(11) -0.0001(8) 0.0024(9) 0.0010(9) O1W 0.0340(16) 0.0200(14) 0.0214(13) -0.0077(10) 0.0093(12) -0.0066(12) O2W 0.040(2) 0.037(2) 0.059(2) -0.0061(15) 0.0159(18) 0.0040(15) _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 O1W 2.036(3) . ? Zn1 O7 2.058(2) 3_556 ? Zn1 O3 2.065(2) 2_545 ? Zn1 O7 2.066(2) . ? Zn1 O2 2.175(2) . ? Zn1 O4 2.338(2) 2_545 ? Zn1 Zn1 3.1179(8) 3_556 ? Zn2 O1 1.964(2) 4_565 ? Zn2 O7 1.987(2) 4_565 ? Zn2 O3 2.034(2) 2_545 ? Zn2 O2 2.080(2) . ? Zn2 O4 2.187(2) . ? As1 O1 1.675(2) . ? As1 O3 1.693(2) . ? As1 O2 1.700(2) . ? As1 C1 1.937(3) . ? S1 O6 1.427(3) . ? S1 O5 1.453(3) . ? S1 O4 1.483(3) . ? S1 C2 1.766(4) . ? C1 C6 1.392(5) . ? C1 C2 1.410(5) . ? C2 C3 1.386(5) . ? C3 C4 1.389(6) . ? C3 H3A 0.9300 . ? C4 C5 1.382(6) . ? C4 H4A 0.9300 . ? C5 C6 1.398(5) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? O1 Zn2 1.964(2) 4_566 ? O3 Zn2 2.034(2) 2 ? O3 Zn1 2.065(2) 2 ? O4 Zn1 2.338(2) 2 ? O7 Zn2 1.987(2) 4_566 ? O7 Zn1 2.058(2) 3_556 ? O7 H7A 0.9800 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8501 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? 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 O1W Zn1 O7 162.83(10) . 3_556 ? O1W Zn1 O3 90.37(10) . 2_545 ? O7 Zn1 O3 97.31(9) 3_556 2_545 ? O1W Zn1 O7 88.76(10) . . ? O7 Zn1 O7 81.78(9) 3_556 . ? O3 Zn1 O7 173.17(9) 2_545 . ? O1W Zn1 O2 97.00(10) . . ? O7 Zn1 O2 99.53(9) 3_556 . ? O3 Zn1 O2 78.93(9) 2_545 . ? O7 Zn1 O2 107.90(9) . . ? O1W Zn1 O4 91.69(10) . 2_545 ? O7 Zn1 O4 74.38(9) 3_556 2_545 ? O3 Zn1 O4 81.64(9) 2_545 2_545 ? O7 Zn1 O4 91.61(9) . 2_545 ? O2 Zn1 O4 158.72(9) . 2_545 ? O1W Zn1 Zn1 128.06(7) . 3_556 ? O7 Zn1 Zn1 40.98(6) 3_556 3_556 ? O3 Zn1 Zn1 137.90(7) 2_545 3_556 ? O7 Zn1 Zn1 40.80(7) . 3_556 ? O2 Zn1 Zn1 108.24(6) . 3_556 ? O4 Zn1 Zn1 80.85(6) 2_545 3_556 ? O1 Zn2 O7 113.44(10) 4_565 4_565 ? O1 Zn2 O3 97.30(10) 4_565 2_545 ? O7 Zn2 O3 100.59(9) 4_565 2_545 ? O1 Zn2 O2 130.58(10) 4_565 . ? O7 Zn2 O2 115.25(9) 4_565 . ? O3 Zn2 O2 81.90(9) 2_545 . ? O1 Zn2 O4 94.87(10) 4_565 . ? O7 Zn2 O4 79.28(10) 4_565 . ? O3 Zn2 O4 166.72(9) 2_545 . ? O2 Zn2 O4 86.15(9) . . ? O1 As1 O3 107.95(11) . . ? O1 As1 O2 110.30(11) . . ? O3 As1 O2 107.76(11) . . ? O1 As1 C1 104.84(13) . . ? O3 As1 C1 107.46(13) . . ? O2 As1 C1 118.13(13) . . ? O6 S1 O5 115.6(2) . . ? O6 S1 O4 112.32(18) . . ? O5 S1 O4 109.92(18) . . ? O6 S1 C2 108.13(19) . . ? O5 S1 C2 104.93(17) . . ? O4 S1 C2 105.13(15) . . ? C6 C1 C2 118.6(3) . . ? C6 C1 As1 115.7(3) . . ? C2 C1 As1 125.3(3) . . ? C3 C2 C1 120.5(3) . . ? C3 C2 S1 118.0(3) . . ? C1 C2 S1 120.9(3) . . ? C2 C3 C4 120.3(4) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 119.5(4) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 120.8(4) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C1 C6 C5 120.1(3) . . ? C1 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? As1 O1 Zn2 133.97(14) . 4_566 ? As1 O2 Zn2 117.13(11) . . ? As1 O2 Zn1 125.02(12) . . ? Zn2 O2 Zn1 96.53(9) . . ? As1 O3 Zn2 129.44(12) . 2 ? As1 O3 Zn1 128.69(13) . 2 ? Zn2 O3 Zn1 101.58(10) 2 2 ? S1 O4 Zn2 120.56(14) . . ? S1 O4 Zn1 146.93(15) . 2 ? Zn2 O4 Zn1 90.63(9) . 2 ? Zn2 O7 Zn1 105.43(11) 4_566 3_556 ? Zn2 O7 Zn1 115.53(11) 4_566 . ? Zn1 O7 Zn1 98.22(9) 3_556 . ? Zn2 O7 H7A 112.2 4_566 . ? Zn1 O7 H7A 112.2 3_556 . ? Zn1 O7 H7A 112.2 . . ? Zn1 O1W H1WA 109.6 . . ? Zn1 O1W H1WB 109.1 . . ? H1WA O1W H1WB 109.5 . . ? H2WA O2W H2WB 112.8 . . ? 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 O7 H7A O2W 0.98 1.90 2.861(4) 166.0 . O1W H1WA O2W 0.85 1.98 2.740(4) 148.8 4_565 O1W H1WB O1 0.85 1.88 2.698(3) 161.1 3_566 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.370 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.165 #===end data_2 _database_code_depnum_ccdc_archive 'CCDC 763189' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H16 As2 Cd3 O16 S2' _chemical_formula_weight 967.41 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.5726(8) _cell_length_b 13.0537(7) _cell_length_c 14.0286(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.830(5) _cell_angle_gamma 90.00 _cell_volume 2286.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4757 _cell_measurement_theta_min 2.1384 _cell_measurement_theta_max 27.4526 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 5.899 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.8018 _exptl_absorpt_correction_T_max 1 _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17764 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5217 _reflns_number_gt 3971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0477P)^2^+2.4259P] 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 shelxtl _refine_ls_extinction_coef ? _refine_ls_number_reflns 5217 _refine_ls_number_parameters 326 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 Cd1 Cd -0.02325(4) 0.25495(4) 0.73587(4) 0.02225(14) Uani 1 1 d . . . Cd2 Cd 0.07638(5) 0.39480(4) 0.96340(4) 0.02683(15) Uani 1 1 d . . . Cd3 Cd 0.05317(5) 0.46768(4) 1.39654(4) 0.02548(15) Uani 1 1 d . . . As1 As -0.09134(6) 0.21214(6) 0.98931(5) 0.01911(17) Uani 1 1 d . . . As2 As 0.12047(6) 0.48590(6) 1.20147(5) 0.01968(17) Uani 1 1 d . . . S1 S -0.22564(15) 0.08232(16) 0.79123(14) 0.0263(4) Uani 1 1 d . . . S2 S 0.2890(8) 0.2992(7) 1.1277(6) 0.0447(11) Uani 0.386(6) 1 d P . . S2' S 0.3042(4) 0.3224(4) 1.0901(4) 0.0447(11) Uani 0.61 1 d PD . . C1 C -0.2432(6) 0.1824(6) 0.9632(6) 0.0241(16) Uani 1 1 d . . . C2 C -0.2936(6) 0.1221(6) 0.8881(5) 0.0248(17) Uani 1 1 d . . . C3 C -0.4014(8) 0.0965(8) 0.8850(7) 0.045(2) Uani 1 1 d . . . H3A H -0.4351 0.0582 0.8343 0.054 Uiso 1 1 calc R . . C4 C -0.4573(7) 0.1285(9) 0.9576(7) 0.053(3) Uani 1 1 d . . . H4A H -0.5284 0.1088 0.9572 0.063 Uiso 1 1 calc R . . C5 C -0.4106(8) 0.1892(8) 1.0312(7) 0.049(3) Uani 1 1 d . . . H5A H -0.4510 0.2123 1.0782 0.059 Uiso 1 1 calc R . . C6 C -0.3037(6) 0.2160(7) 1.0352(6) 0.035(2) Uani 1 1 d . . . H6A H -0.2720 0.2561 1.0855 0.042 Uiso 1 1 calc R . . C7 C 0.2704(6) 0.5046(7) 1.1868(6) 0.0311(19) Uani 1 1 d . . . C8 C 0.3358(7) 0.4382(7) 1.1422(7) 0.039(2) Uani 1 1 d . . . C9 C 0.4384(8) 0.4698(10) 1.1270(8) 0.060(3) Uani 1 1 d . . . H9A H 0.4817 0.4267 1.0956 0.072 Uiso 1 1 calc R . . C10 C 0.4752(8) 0.5635(11) 1.1580(10) 0.074(4) Uani 1 1 d . . . H10A H 0.5446 0.5828 1.1493 0.089 Uiso 1 1 calc R . . C11 C 0.4135(8) 0.6284(9) 1.2009(9) 0.067(4) Uani 1 1 d . . . H11A H 0.4398 0.6928 1.2199 0.081 Uiso 1 1 calc R . . C12 C 0.3096(7) 0.6004(7) 1.2174(7) 0.044(2) Uani 1 1 d . . . H12A H 0.2675 0.6451 1.2483 0.053 Uiso 1 1 calc R . . O1 O -0.0321(4) 0.2682(4) 0.9009(4) 0.0246(12) Uani 1 1 d . . . O2 O -0.0752(4) 0.2905(4) 1.0847(3) 0.0248(11) Uani 1 1 d . . . O3 O -0.0254(4) 0.1015(4) 1.0146(4) 0.0250(11) Uani 1 1 d . . . O4 O -0.1371(5) 0.0181(5) 0.8319(5) 0.0490(17) Uani 1 1 d . . . O5 O -0.3005(5) 0.0295(5) 0.7232(4) 0.0438(16) Uani 1 1 d . . . O6 O -0.1865(5) 0.1768(5) 0.7507(5) 0.0470(17) Uani 1 1 d . . . O7 O 0.0480(4) 0.4921(4) 1.0950(4) 0.0252(12) Uani 1 1 d . . . O8 O 0.0886(4) 0.5807(4) 1.2759(3) 0.0225(11) Uani 1 1 d . . . O9 O 0.0911(4) 0.3814(3) 1.2644(3) 0.0206(11) Uani 1 1 d . . . O10 O 0.1829(5) 0.3116(5) 1.0824(5) 0.0451(16) Uani 1 1 d . . . O11 O 0.357(2) 0.256(2) 1.056(2) 0.097(5) Uani 0.386(6) 1 d P . . O11' O 0.3467(14) 0.3175(13) 1.0010(11) 0.097(5) Uani 0.61 1 d PD . . O12 O 0.3048(17) 0.2498(17) 1.2116(19) 0.069(4) Uani 0.386(6) 1 d P . . O12' O 0.3516(11) 0.2483(10) 1.1570(11) 0.069(4) Uani 0.61 1 d PD . . O1W O 0.1316(5) 0.3436(5) 0.7959(5) 0.0467(17) Uani 1 1 d . . . H1WA H 0.1423 0.3956 0.7619 0.070 Uiso 1 1 d R . . H1WB H 0.1867 0.3052 0.8010 0.070 Uiso 1 1 d R . . O2W O 0.1941(5) 0.5255(4) 0.9433(4) 0.0339(13) Uani 1 1 d . . . H2WA H 0.1721 0.5588 0.8927 0.051 Uiso 1 1 d R . . H2WB H 0.2556 0.5004 0.9381 0.051 Uiso 1 1 d R . . O3W O 0.2228(6) 0.4205(6) 1.4637(5) 0.063(2) Uani 1 1 d . . . H3WA H 0.2221 0.4105 1.5235 0.095 Uiso 1 1 d R . . H3WB H 0.2409 0.3655 1.4374 0.095 Uiso 1 1 d R . . O4W O 0.3076(11) 0.2707(11) 1.3481(13) 0.196(8) Uani 1 1 d . . . H4WA H 0.2984 0.3235 1.3125 0.295 Uiso 1 1 d R . . H4WB H 0.3738 0.2560 1.3572 0.295 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0318(3) 0.0180(3) 0.0171(3) 0.0003(2) 0.0032(2) 0.0003(2) Cd2 0.0317(3) 0.0202(3) 0.0286(3) -0.0039(2) 0.0036(2) 0.0023(2) Cd3 0.0354(3) 0.0221(3) 0.0208(3) -0.0018(2) 0.0111(2) -0.0025(2) As1 0.0257(4) 0.0163(4) 0.0157(4) -0.0010(3) 0.0039(3) 0.0005(3) As2 0.0235(4) 0.0180(4) 0.0182(4) 0.0010(3) 0.0053(3) 0.0007(3) S1 0.0260(9) 0.0309(11) 0.0228(10) -0.0063(8) 0.0063(8) -0.0037(8) S2 0.049(2) 0.044(3) 0.043(3) -0.003(2) 0.017(2) 0.023(2) S2' 0.049(2) 0.044(3) 0.043(3) -0.003(2) 0.017(2) 0.023(2) C1 0.024(4) 0.021(4) 0.029(4) 0.006(3) 0.012(3) 0.003(3) C2 0.027(4) 0.024(4) 0.026(4) -0.001(3) 0.016(3) 0.002(3) C3 0.040(5) 0.057(6) 0.038(6) -0.005(5) 0.012(4) -0.003(5) C4 0.028(5) 0.083(8) 0.050(6) -0.003(6) 0.016(4) -0.007(5) C5 0.045(6) 0.073(7) 0.032(5) -0.001(5) 0.019(4) 0.006(5) C6 0.029(4) 0.050(5) 0.026(5) -0.010(4) 0.004(3) 0.006(4) C7 0.024(4) 0.042(5) 0.028(4) 0.007(4) 0.006(3) 0.003(4) C8 0.027(4) 0.051(6) 0.039(5) -0.002(4) 0.007(4) 0.012(4) C9 0.037(6) 0.086(9) 0.060(7) 0.014(6) 0.021(5) 0.017(6) C10 0.023(5) 0.090(10) 0.110(11) 0.050(9) 0.010(6) 0.000(6) C11 0.031(5) 0.063(8) 0.105(10) 0.025(7) -0.003(6) -0.026(5) C12 0.028(5) 0.046(6) 0.058(6) 0.005(5) 0.001(4) -0.007(4) O1 0.031(3) 0.026(3) 0.017(3) 0.002(2) 0.007(2) -0.004(2) O2 0.038(3) 0.018(3) 0.018(3) -0.002(2) 0.002(2) 0.003(2) O3 0.035(3) 0.015(3) 0.028(3) 0.002(2) 0.010(2) 0.003(2) O4 0.042(4) 0.059(4) 0.047(4) -0.011(3) 0.008(3) 0.019(3) O5 0.036(3) 0.064(4) 0.032(3) -0.021(3) 0.003(3) -0.012(3) O6 0.058(4) 0.046(4) 0.040(4) -0.008(3) 0.019(3) -0.024(3) O7 0.033(3) 0.023(3) 0.019(3) 0.000(2) 0.000(2) 0.002(2) O8 0.029(3) 0.018(3) 0.021(3) -0.001(2) 0.006(2) 0.000(2) O9 0.027(3) 0.013(2) 0.023(3) 0.002(2) 0.007(2) -0.003(2) O10 0.047(4) 0.032(3) 0.053(4) -0.002(3) -0.007(3) 0.006(3) O11 0.123(11) 0.105(13) 0.070(11) -0.014(8) 0.041(10) 0.048(10) O11' 0.123(11) 0.105(13) 0.070(11) -0.014(8) 0.041(10) 0.048(10) O12 0.052(8) 0.058(6) 0.095(12) 0.023(7) 0.004(6) 0.032(6) O12' 0.052(8) 0.058(6) 0.095(12) 0.023(7) 0.004(6) 0.032(6) O1W 0.039(4) 0.035(4) 0.066(5) -0.001(3) 0.010(3) -0.007(3) O2W 0.040(3) 0.033(3) 0.031(3) 0.004(3) 0.011(3) 0.001(3) O3W 0.058(5) 0.065(5) 0.062(5) -0.007(4) -0.016(4) 0.008(4) O4W 0.103(11) 0.162(14) 0.32(2) -0.001(15) 0.000(13) 0.015(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.224(5) 4_565 ? Cd1 O9 2.293(5) 4_565 ? Cd1 O8 2.296(5) 3_567 ? Cd1 O6 2.323(6) . ? Cd1 O1W 2.334(6) . ? Cd1 O1 2.338(5) . ? Cd2 O7 2.235(5) 3_567 ? Cd2 O1 2.252(5) . ? Cd2 O10 2.286(6) . ? Cd2 O2W 2.298(6) . ? Cd2 O7 2.302(5) . ? Cd2 O1W 2.616(7) . ? Cd3 O3 2.198(5) 2_557 ? Cd3 O3 2.218(5) 4_566 ? Cd3 O9 2.268(5) . ? Cd3 O3W 2.310(7) . ? Cd3 O8 2.328(5) . ? Cd3 O4 2.462(7) 4_566 ? Cd3 As2 2.9685(9) . ? Cd3 Cd3 3.4423(11) 3_568 ? As1 O2 1.678(5) . ? As1 O3 1.682(5) . ? As1 O1 1.688(5) . ? As1 C1 1.940(8) . ? As2 O7 1.657(5) . ? As2 O9 1.690(5) . ? As2 O8 1.697(5) . ? As2 C7 1.935(8) . ? S1 O5 1.435(6) . ? S1 O4 1.455(7) . ? S1 O6 1.468(6) . ? S1 C2 1.767(7) . ? S2 S2' 0.656(7) . ? S2 O12' 1.073(14) . ? S2 O12 1.34(2) . ? S2 O10 1.417(12) . ? S2 O11 1.50(2) . ? S2 C8 1.911(14) . ? S2 O11' 2.013(15) . ? S2' O11 1.22(2) . ? S2' O11' 1.419(14) . ? S2' O12' 1.427(12) . ? S2' O10 1.522(8) . ? S2' C8 1.705(11) . ? S2' O12 1.95(2) . ? C1 C2 1.404(11) . ? C1 C6 1.406(10) . ? C2 C3 1.392(11) . ? C3 C4 1.370(12) . ? C3 H3A 0.9300 . ? C4 C5 1.376(14) . ? C4 H4A 0.9300 . ? C5 C6 1.383(12) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.393(12) . ? C7 C8 1.394(11) . ? C8 C9 1.394(13) . ? C9 C10 1.361(17) . ? C9 H9A 0.9300 . ? C10 C11 1.339(18) . ? C10 H10A 0.9300 . ? C11 C12 1.402(13) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? O2 Cd1 2.224(5) 4_566 ? O3 Cd3 2.198(5) 2_547 ? O3 Cd3 2.218(5) 4_565 ? O4 Cd3 2.462(7) 4_565 ? O7 Cd2 2.235(5) 3_567 ? O8 Cd1 2.296(5) 3_567 ? O9 Cd1 2.293(5) 4_566 ? O11 O11' 1.11(3) . ? O11 O12' 1.43(3) . ? O12 O12' 1.02(2) . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8501 . ? O2W H2WA 0.8501 . ? O2W H2WB 0.8501 . ? O3W H3WA 0.8498 . ? O3W H3WB 0.8498 . ? O4W H4WA 0.8501 . ? O4W H4WB 0.8499 . ? 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 Cd1 O9 93.81(18) 4_565 4_565 ? O2 Cd1 O8 96.82(18) 4_565 3_567 ? O9 Cd1 O8 161.68(18) 4_565 3_567 ? O2 Cd1 O6 78.8(2) 4_565 . ? O9 Cd1 O6 100.7(2) 4_565 . ? O8 Cd1 O6 96.0(2) 3_567 . ? O2 Cd1 O1W 127.9(2) 4_565 . ? O9 Cd1 O1W 80.9(2) 4_565 . ? O8 Cd1 O1W 80.7(2) 3_567 . ? O6 Cd1 O1W 153.3(2) . . ? O2 Cd1 O1 157.08(18) 4_565 . ? O9 Cd1 O1 89.27(18) 4_565 . ? O8 Cd1 O1 86.74(18) 3_567 . ? O6 Cd1 O1 78.3(2) . . ? O1W Cd1 O1 75.0(2) . . ? O7 Cd2 O1 88.70(19) 3_567 . ? O7 Cd2 O10 154.8(2) 3_567 . ? O1 Cd2 O10 102.2(2) . . ? O7 Cd2 O2W 84.1(2) 3_567 . ? O1 Cd2 O2W 150.00(19) . . ? O10 Cd2 O2W 96.4(2) . . ? O7 Cd2 O7 76.2(2) 3_567 . ? O1 Cd2 O7 124.90(18) . . ? O10 Cd2 O7 79.0(2) . . ? O2W Cd2 O7 81.50(19) . . ? O7 Cd2 O1W 95.11(19) 3_567 . ? O1 Cd2 O1W 71.10(18) . . ? O10 Cd2 O1W 109.8(2) . . ? O2W Cd2 O1W 80.56(19) . . ? O7 Cd2 O1W 160.76(19) . . ? O3 Cd3 O3 77.58(19) 2_557 4_566 ? O3 Cd3 O9 157.14(18) 2_557 . ? O3 Cd3 O9 124.31(17) 4_566 . ? O3 Cd3 O3W 100.5(2) 2_557 . ? O3 Cd3 O3W 93.3(2) 4_566 . ? O9 Cd3 O3W 85.8(2) . . ? O3 Cd3 O8 88.04(18) 2_557 . ? O3 Cd3 O8 160.28(18) 4_566 . ? O9 Cd3 O8 69.12(17) . . ? O3W Cd3 O8 102.6(2) . . ? O3 Cd3 O4 86.3(2) 2_557 4_566 ? O3 Cd3 O4 78.9(2) 4_566 4_566 ? O9 Cd3 O4 91.5(2) . 4_566 ? O3W Cd3 O4 168.4(2) . 4_566 ? O8 Cd3 O4 86.91(19) . 4_566 ? O3 Cd3 As2 122.77(13) 2_557 . ? O3 Cd3 As2 157.18(13) 4_566 . ? O9 Cd3 As2 34.47(12) . . ? O3W Cd3 As2 92.7(2) . . ? O8 Cd3 As2 34.79(12) . . ? O4 Cd3 As2 91.44(16) 4_566 . ? O3 Cd3 Cd3 39.01(13) 2_557 3_568 ? O3 Cd3 Cd3 38.58(12) 4_566 3_568 ? O9 Cd3 Cd3 162.11(12) . 3_568 ? O3W Cd3 Cd3 98.8(2) . 3_568 ? O8 Cd3 Cd3 125.79(12) . 3_568 ? O4 Cd3 Cd3 80.48(16) 4_566 3_568 ? As2 Cd3 Cd3 159.99(3) . 3_568 ? O2 As1 O3 110.2(3) . . ? O2 As1 O1 107.4(3) . . ? O3 As1 O1 106.1(2) . . ? O2 As1 C1 107.2(3) . . ? O3 As1 C1 108.5(3) . . ? O1 As1 C1 117.3(3) . . ? O7 As2 O9 112.3(3) . . ? O7 As2 O8 112.0(2) . . ? O9 As2 O8 100.7(2) . . ? O7 As2 C7 109.6(3) . . ? O9 As2 C7 115.7(3) . . ? O8 As2 C7 106.1(3) . . ? O7 As2 Cd3 130.46(19) . . ? O9 As2 Cd3 49.42(16) . . ? O8 As2 Cd3 51.51(16) . . ? C7 As2 Cd3 119.7(2) . . ? O5 S1 O4 113.2(4) . . ? O5 S1 O6 111.8(4) . . ? O4 S1 O6 111.1(4) . . ? O5 S1 C2 108.3(4) . . ? O4 S1 C2 106.6(4) . . ? O6 S1 C2 105.4(4) . . ? S2' S2 O12' 108.8(14) . . ? S2' S2 O12 154.7(18) . . ? O12' S2 O12 48.6(11) . . ? S2' S2 O10 86.2(13) . . ? O12' S2 O10 148.3(13) . . ? O12 S2 O10 119.0(12) . . ? S2' S2 O11 52.4(14) . . ? O12' S2 O11 64.9(13) . . ? O12 S2 O11 111.9(15) . . ? O10 S2 O11 108.8(14) . . ? S2' S2 C8 62.1(12) . . ? O12' S2 C8 110.2(11) . . ? O12 S2 C8 110.7(13) . . ? O10 S2 C8 101.5(6) . . ? O11 S2 C8 103.3(13) . . ? S2' S2 O11' 20.7(10) . . ? O12' S2 O11' 94.9(10) . . ? O12 S2 O11' 143.5(12) . . ? O10 S2 O11' 90.5(7) . . ? O11 S2 O11' 32.8(11) . . ? C8 S2 O11' 80.9(7) . . ? S2 S2' O11 102.3(18) . . ? S2 S2' O11' 149.8(15) . . ? O11 S2' O11' 49.0(13) . . ? S2 S2' O12' 45.4(11) . . ? O11 S2' O12' 64.8(14) . . ? O11' S2' O12' 112.1(9) . . ? S2 S2' O10 68.3(12) . . ? O11 S2' O10 119.7(16) . . ? O11' S2' O10 114.3(9) . . ? O12' S2' O10 108.7(7) . . ? S2 S2' C8 98.0(14) . . ? O11 S2' C8 133.1(16) . . ? O11' S2' C8 108.9(9) . . ? O12' S2' C8 105.2(8) . . ? O10 S2' C8 107.0(4) . . ? S2 S2' O12 17.0(13) . . ? O11 S2' O12 93.0(15) . . ? O11' S2' O12 141.8(10) . . ? O12' S2' O12 30.5(7) . . ? O10 S2' O12 85.3(7) . . ? C8 S2' O12 94.6(8) . . ? C2 C1 C6 118.6(7) . . ? C2 C1 As1 126.9(5) . . ? C6 C1 As1 114.0(6) . . ? C3 C2 C1 120.6(7) . . ? C3 C2 S1 117.6(6) . . ? C1 C2 S1 121.7(5) . . ? C4 C3 C2 119.2(9) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C3 C4 C5 121.5(9) . . ? C3 C4 H4A 119.2 . . ? C5 C4 H4A 119.2 . . ? C4 C5 C6 120.1(8) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C1 119.9(8) . . ? C5 C6 H6A 120.1 . . ? C1 C6 H6A 120.1 . . ? C12 C7 C8 119.3(8) . . ? C12 C7 As2 113.2(6) . . ? C8 C7 As2 127.2(7) . . ? C9 C8 C7 119.4(10) . . ? C9 C8 S2' 111.7(8) . . ? C7 C8 S2' 128.6(7) . . ? C9 C8 S2 122.9(8) . . ? C7 C8 S2 116.6(7) . . ? S2' C8 S2 19.9(3) . . ? C10 C9 C8 120.2(10) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C11 C10 C9 121.3(10) . . ? C11 C10 H10A 119.4 . . ? C9 C10 H10A 119.4 . . ? C10 C11 C12 120.6(11) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C7 C12 C11 119.1(10) . . ? C7 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? As1 O1 Cd2 109.4(2) . . ? As1 O1 Cd1 140.6(3) . . ? Cd2 O1 Cd1 110.0(2) . . ? As1 O2 Cd1 126.3(3) . 4_566 ? As1 O3 Cd3 134.0(3) . 2_547 ? As1 O3 Cd3 116.4(3) . 4_565 ? Cd3 O3 Cd3 102.42(19) 2_547 4_565 ? S1 O4 Cd3 140.0(4) . 4_565 ? S1 O6 Cd1 138.1(4) . . ? As2 O7 Cd2 130.4(3) . 3_567 ? As2 O7 Cd2 125.1(3) . . ? Cd2 O7 Cd2 103.8(2) 3_567 . ? As2 O8 Cd1 138.2(3) . 3_567 ? As2 O8 Cd3 93.7(2) . . ? Cd1 O8 Cd3 123.1(2) 3_567 . ? As2 O9 Cd3 96.1(2) . . ? As2 O9 Cd1 135.0(3) . 4_566 ? Cd3 O9 Cd1 109.85(19) . 4_566 ? S2 O10 S2' 25.5(3) . . ? S2 O10 Cd2 145.2(5) . . ? S2' O10 Cd2 120.2(4) . . ? O11' O11 S2' 75.0(18) . . ? O11' O11 O12' 137(2) . . ? S2' O11 O12' 64.7(12) . . ? O11' O11 S2 100(2) . . ? S2' O11 S2 25.3(6) . . ? O12' O11 S2 42.9(9) . . ? O11 O11' S2' 56.0(14) . . ? O11 O11' S2 47.3(14) . . ? S2' O11' S2 9.4(5) . . ? O12' O12 S2 52.2(14) . . ? O12' O12 S2' 45.2(12) . . ? S2 O12 S2' 8.3(6) . . ? O12 O12' S2 79.2(15) . . ? O12 O12' S2' 104.3(16) . . ? S2 O12' S2' 25.8(5) . . ? O12 O12' O11 147(2) . . ? S2 O12' O11 72.2(13) . . ? S2' O12' O11 50.5(11) . . ? Cd1 O1W Cd2 98.7(2) . . ? Cd1 O1W H1WA 112.0 . . ? Cd2 O1W H1WA 112.1 . . ? Cd1 O1W H1WB 112.0 . . ? Cd2 O1W H1WB 112.0 . . ? H1WA O1W H1WB 109.7 . . ? Cd2 O2W H2WA 109.3 . . ? Cd2 O2W H2WB 109.3 . . ? H2WA O2W H2WB 109.5 . . ? Cd3 O3W H3WA 109.0 . . ? Cd3 O3W H3WB 109.3 . . ? H3WA O3W H3WB 109.5 . . ? H4WA O4W H4WB 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2W H2WA O2 0.85 2.36 2.832(7) 115.9 3_567 O1W H1WA O4 0.85 2.07 2.905(9) 168.6 2_556 O1W H1WB O4W 0.85 1.87 2.696(15) 164.2 4_565 O3W H3WB O4W 0.85 2.01 2.828(17) 160.3 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.406 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.217 #===end data_3 _database_code_depnum_ccdc_archive 'CCDC 763190' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H54 As2 N8 O18 S2 Zn2' _chemical_formula_weight 1423.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'S' 'S' 0.1246 0.1234 '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 'triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.320(3) _cell_length_b 14.576(4) _cell_length_c 20.283(6) _cell_angle_alpha 79.202(7) _cell_angle_beta 83.149(6) _cell_angle_gamma 88.874(8) _cell_volume 2975.6(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5685 _cell_measurement_theta_min 2.0585 _cell_measurement_theta_max 27.4565 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 2.057 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7266 _exptl_absorpt_correction_T_max 1 _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23346 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0794 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13391 _reflns_number_gt 8604 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.1052P)^2^+0.2544P] 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 SHELXL _refine_ls_extinction_coef 0.0028(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 13391 _refine_ls_number_parameters 776 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.2012 _refine_ls_wR_factor_gt 0.1746 _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 0.74511(6) 0.79457(4) 0.99371(3) 0.03930(18) Uani 1 1 d . . . Zn2 Zn 0.80523(6) 1.22785(5) 0.52257(3) 0.04230(19) Uani 1 1 d . . . As1 As 0.72609(5) 0.86403(4) 0.83264(3) 0.03889(17) Uani 1 1 d . . . As2 As 0.67285(6) 1.08803(4) 0.65951(3) 0.04264(18) Uani 1 1 d . . . S1 S 1.02773(14) 0.78062(10) 0.88502(7) 0.0442(3) Uani 1 1 d . . . S2 S 0.71243(14) 1.33206(10) 0.65965(7) 0.0441(3) Uani 1 1 d . . . N1 N 0.5698(4) 0.7947(3) 1.0631(2) 0.0411(10) Uani 1 1 d . . . N2 N 0.7420(4) 0.9329(3) 1.0156(2) 0.0420(11) Uani 1 1 d . . . N3 N 0.8650(5) 0.7303(3) 1.0705(2) 0.0466(12) Uani 1 1 d . . . N4 N 0.7441(5) 0.6482(3) 0.9891(3) 0.0528(13) Uani 1 1 d . . . N5 N 0.8704(5) 1.3670(3) 0.4669(2) 0.0455(11) Uani 1 1 d . . . N6 N 0.6308(5) 1.2958(3) 0.4925(2) 0.0442(11) Uani 1 1 d . . . N7 N 0.8684(5) 1.1688(4) 0.4351(2) 0.0515(12) Uani 1 1 d . . . N8 N 0.9960(4) 1.1761(3) 0.5404(3) 0.0482(12) Uani 1 1 d . . . C1 C 0.8342(6) 0.7673(4) 0.7999(3) 0.0479(14) Uani 1 1 d . . . C2 C 0.9533(6) 0.7375(4) 0.8214(3) 0.0472(14) Uani 1 1 d . . . C3 C 1.0260(8) 0.6711(5) 0.7925(4) 0.071(2) Uani 1 1 d . . . H3A H 1.1059 0.6513 0.8070 0.085 Uiso 1 1 calc R . . C4 C 0.9784(11) 0.6346(6) 0.7417(5) 0.098(3) Uani 1 1 d . . . H4A H 1.0253 0.5888 0.7228 0.118 Uiso 1 1 calc R . . C5 C 0.8626(10) 0.6656(7) 0.7193(5) 0.097(3) Uani 1 1 d . . . H5A H 0.8329 0.6431 0.6839 0.116 Uiso 1 1 calc R . . C6 C 0.7897(8) 0.7305(6) 0.7494(4) 0.077(2) Uani 1 1 d . . . H6A H 0.7094 0.7494 0.7352 0.092 Uiso 1 1 calc R . . C7 C 0.5473(5) 1.1736(4) 0.6941(3) 0.0441(13) Uani 1 1 d . . . C8 C 0.5655(5) 1.2687(4) 0.6928(3) 0.0448(13) Uani 1 1 d . . . C9 C 0.4651(6) 1.3197(5) 0.7207(4) 0.0617(17) Uani 1 1 d . . . H9B H 0.4757 1.3834 0.7188 0.074 Uiso 1 1 calc R . . C10 C 0.3498(7) 1.2763(7) 0.7514(4) 0.075(2) Uani 1 1 d . . . H10A H 0.2843 1.3103 0.7715 0.090 Uiso 1 1 calc R . . C11 C 0.3319(7) 1.1836(7) 0.7522(4) 0.072(2) Uani 1 1 d . . . H11A H 0.2533 1.1550 0.7719 0.086 Uiso 1 1 calc R . . C12 C 0.4294(6) 1.1319(5) 0.7242(3) 0.0573(17) Uani 1 1 d . . . H12A H 0.4163 1.0686 0.7253 0.069 Uiso 1 1 calc R . . C13 C 0.4906(6) 0.7216(5) 1.0873(3) 0.0566(16) Uani 1 1 d . . . H13A H 0.5131 0.6646 1.0748 0.068 Uiso 1 1 calc R . . C14 C 0.3775(7) 0.7265(6) 1.1298(4) 0.068(2) Uani 1 1 d . . . H14A H 0.3245 0.6744 1.1460 0.082 Uiso 1 1 calc R . . C15 C 0.3458(7) 0.8105(7) 1.1474(3) 0.071(2) Uani 1 1 d . . . H15A H 0.2697 0.8164 1.1758 0.086 Uiso 1 1 calc R . . C16 C 0.4267(6) 0.8873(5) 1.1231(3) 0.0545(16) Uani 1 1 d . . . H16A H 0.4056 0.9448 1.1350 0.065 Uiso 1 1 calc R . . C17 C 0.5398(5) 0.8766(4) 1.0806(3) 0.0415(12) Uani 1 1 d . . . C18 C 0.6332(5) 0.9551(4) 1.0532(3) 0.0419(12) Uani 1 1 d . . . C19 C 0.6117(6) 1.0446(5) 1.0645(3) 0.0526(15) Uani 1 1 d . . . H19A H 0.5362 1.0589 1.0904 0.063 Uiso 1 1 calc R . . C20 C 0.7029(7) 1.1122(4) 1.0371(3) 0.0550(15) Uani 1 1 d . . . H20A H 0.6904 1.1730 1.0445 0.066 Uiso 1 1 calc R . . C21 C 0.8124(7) 1.0894(5) 0.9990(3) 0.0579(16) Uani 1 1 d . . . H21A H 0.8757 1.1344 0.9803 0.069 Uiso 1 1 calc R . . C22 C 0.8284(6) 0.9993(5) 0.9883(3) 0.0538(15) Uani 1 1 d . . . H22A H 0.9019 0.9845 0.9611 0.065 Uiso 1 1 calc R . . C23 C 0.9190(6) 0.7762(5) 1.1124(3) 0.0548(16) Uani 1 1 d . . . H23A H 0.9064 0.8404 1.1079 0.066 Uiso 1 1 calc R . . C24 C 0.9924(7) 0.7319(7) 1.1618(4) 0.072(2) Uani 1 1 d . . . H24A H 1.0278 0.7650 1.1903 0.086 Uiso 1 1 calc R . . C25 C 1.0113(8) 0.6381(8) 1.1673(4) 0.089(3) Uani 1 1 d . . . H25A H 1.0603 0.6067 1.2001 0.106 Uiso 1 1 calc R . . C26 C 0.9594(8) 0.5896(6) 1.1256(4) 0.077(2) Uani 1 1 d . . . H26A H 0.9734 0.5258 1.1290 0.093 Uiso 1 1 calc R . . C27 C 0.8831(6) 0.6391(5) 1.0766(3) 0.0550(16) Uani 1 1 d . . . C28 C 0.8190(7) 0.5923(4) 1.0309(4) 0.0609(18) Uani 1 1 d . . . C29 C 0.8288(10) 0.4995(5) 1.0292(5) 0.089(3) Uani 1 1 d . . . H29A H 0.8799 0.4614 1.0579 0.107 Uiso 1 1 calc R . . C30 C 0.7645(11) 0.4623(6) 0.9859(6) 0.098(3) Uani 1 1 d . . . H30A H 0.7734 0.3992 0.9842 0.118 Uiso 1 1 calc R . . C31 C 0.6846(11) 0.5186(6) 0.9438(5) 0.097(3) Uani 1 1 d . . . H31A H 0.6364 0.4942 0.9151 0.117 Uiso 1 1 calc R . . C32 C 0.6814(8) 0.6122(5) 0.9472(4) 0.0645(18) Uani 1 1 d . . . H32A H 0.6325 0.6519 0.9184 0.077 Uiso 1 1 calc R . . C33 C 0.9935(6) 1.3951(5) 0.4535(3) 0.0552(16) Uani 1 1 d . . . H33A H 1.0578 1.3560 0.4715 0.066 Uiso 1 1 calc R . . C34 C 1.0296(7) 1.4799(5) 0.4138(4) 0.0638(18) Uani 1 1 d . . . H34A H 1.1168 1.4980 0.4051 0.077 Uiso 1 1 calc R . . C35 C 0.9361(8) 1.5364(5) 0.3877(4) 0.074(2) Uani 1 1 d . . . H35A H 0.9590 1.5945 0.3616 0.089 Uiso 1 1 calc R . . C36 C 0.8031(7) 1.5082(5) 0.3996(4) 0.0668(19) Uani 1 1 d . . . H36A H 0.7378 1.5462 0.3814 0.080 Uiso 1 1 calc R . . C37 C 0.7751(6) 1.4202(4) 0.4402(3) 0.0478(14) Uani 1 1 d . . . C38 C 0.6424(6) 1.3843(4) 0.4578(3) 0.0459(13) Uani 1 1 d . . . C39 C 0.5314(7) 1.4334(5) 0.4402(4) 0.0657(19) Uani 1 1 d . . . H39A H 0.5394 1.4937 0.4151 0.079 Uiso 1 1 calc R . . C40 C 0.4122(7) 1.3949(6) 0.4590(5) 0.080(2) Uani 1 1 d . . . H40A H 0.3384 1.4292 0.4480 0.097 Uiso 1 1 calc R . . C41 C 0.3992(7) 1.3033(5) 0.4950(4) 0.070(2) Uani 1 1 d . . . H41A H 0.3180 1.2747 0.5076 0.084 Uiso 1 1 calc R . . C42 C 0.5125(6) 1.2577(5) 0.5108(3) 0.0546(16) Uani 1 1 d . . . H42A H 0.5063 1.1971 0.5356 0.065 Uiso 1 1 calc R . . C43 C 0.7994(7) 1.1715(5) 0.3830(3) 0.0605(17) Uani 1 1 d . . . H43A H 0.7175 1.1994 0.3842 0.073 Uiso 1 1 calc R . . C44 C 0.8482(9) 1.1331(5) 0.3268(3) 0.073(2) Uani 1 1 d . . . H44A H 0.8002 1.1362 0.2904 0.087 Uiso 1 1 calc R . . C45 C 0.9670(9) 1.0913(6) 0.3263(4) 0.079(2) Uani 1 1 d . . . H45A H 0.9993 1.0639 0.2898 0.094 Uiso 1 1 calc R . . C46 C 1.0400(8) 1.0889(5) 0.3790(4) 0.070(2) Uani 1 1 d . . . H46A H 1.1224 1.0618 0.3781 0.084 Uiso 1 1 calc R . . C47 C 0.9868(6) 1.1286(4) 0.4342(3) 0.0554(16) Uani 1 1 d . . . C48 C 1.0546(6) 1.1277(4) 0.4937(3) 0.0488(14) Uani 1 1 d . . . C49 C 1.1709(6) 1.0795(5) 0.5048(4) 0.067(2) Uani 1 1 d . . . H49A H 1.2113 1.0463 0.4731 0.080 Uiso 1 1 calc R . . C50 C 1.2244(7) 1.0820(6) 0.5632(5) 0.078(2) Uani 1 1 d . . . H50A H 1.3024 1.0509 0.5707 0.093 Uiso 1 1 calc R . . C51 C 1.1648(7) 1.1295(6) 0.6106(4) 0.075(2) Uani 1 1 d . . . H51A H 1.2003 1.1305 0.6505 0.089 Uiso 1 1 calc R . . C52 C 1.0503(6) 1.1758(5) 0.5971(4) 0.0622(18) Uani 1 1 d . . . H52A H 1.0089 1.2083 0.6289 0.075 Uiso 1 1 calc R . . O1 O 0.6552(4) 0.8301(3) 0.91111(18) 0.0463(10) Uani 1 1 d . . . O2 O 0.5931(4) 0.8693(3) 0.7876(2) 0.0586(12) Uani 1 1 d . . . H2A H 0.6061 0.9092 0.7532 0.088 Uiso 1 1 calc R . . O3 O 0.7995(4) 0.9677(3) 0.81310(19) 0.0443(9) Uani 1 1 d . . . O4 O 1.0735(5) 0.7008(4) 0.9287(3) 0.0751(15) Uani 1 1 d . . . O5 O 1.1301(4) 0.8425(3) 0.8477(2) 0.0611(12) Uani 1 1 d . . . O6 O 0.9264(3) 0.8307(3) 0.91982(18) 0.0437(9) Uani 1 1 d . . . O7 O 0.6015(5) 0.9833(3) 0.6791(2) 0.0650(13) Uani 1 1 d . . . O8 O 0.7125(4) 1.1119(3) 0.57625(19) 0.0500(10) Uani 1 1 d . . . O9 O 0.8071(4) 1.0852(3) 0.7012(2) 0.0515(10) Uani 1 1 d . . . H9A H 0.7965 1.0459 0.7361 0.077 Uiso 1 1 calc R . . O10 O 0.6693(5) 1.4159(3) 0.6187(3) 0.0855(18) Uani 1 1 d . . . O11 O 0.7742(5) 1.3450(4) 0.7166(2) 0.0773(16) Uani 1 1 d . . . O12 O 0.7900(4) 1.2745(3) 0.61819(19) 0.0472(9) Uani 1 1 d . . . O1W O 1.0485(6) 1.0370(4) 0.8303(3) 0.0957(19) Uani 1 1 d . . . H1WA H 1.1078 1.0086 0.8092 0.144 Uiso 1 1 d R . . H1WB H 0.9741 1.0167 0.8256 0.144 Uiso 1 1 d R . . O2W O 0.3792(6) 0.7501(6) 0.8186(5) 0.146(3) Uani 1 1 d . . . H2WA H 0.4447 0.7866 0.8088 0.219 Uiso 1 1 d R . . H2WB H 0.3418 0.7540 0.8577 0.219 Uiso 1 1 d R . . O3W O 0.5474(10) 0.8560(7) 0.6073(4) 0.160(4) Uani 1 1 d . . . H3WA H 0.5661 0.8960 0.6302 0.240 Uiso 1 1 d R . . H3WB H 0.4960 0.8803 0.5791 0.240 Uiso 1 1 d R . . O4W O 0.4550(11) 0.6959(7) 0.6924(5) 0.172(4) Uani 1 1 d . . . H4WA H 0.3876 0.7070 0.7181 0.259 Uiso 1 1 d R . . H4WB H 0.4811 0.7462 0.6660 0.259 Uiso 1 1 d R . . O5W O 0.5362(11) 1.0220(11) 0.5114(9) 0.112(5) Uani 0.50 1 d P . . O6W O 0.6134(17) 0.5251(10) 0.7483(11) 0.176(9) Uani 0.50 1 d P . . H6WB H 0.5696 0.5726 0.7328 0.264 Uiso 0.50 1 d PR . . H6WA H 0.5625 0.4846 0.7737 0.264 Uiso 0.50 1 d PR . . O7W O 0.4238(16) 0.5295(12) 0.8482(7) 0.131(6) Uani 0.50 1 d P . . O8W O 0.2818(16) 0.5191(13) 0.7456(10) 0.162(8) Uani 0.50 1 d P . . H8WA H 0.3255 0.5220 0.7782 0.243 Uiso 0.50 1 d PR . . H8WB H 0.3195 0.5515 0.7094 0.243 Uiso 0.50 1 d PR . . 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 0.0447(3) 0.0364(3) 0.0345(3) -0.0038(3) -0.0007(2) 0.0064(3) Zn2 0.0436(4) 0.0423(4) 0.0375(3) -0.0024(3) 0.0003(3) 0.0085(3) As1 0.0413(3) 0.0397(3) 0.0329(3) -0.0011(2) -0.0026(2) 0.0039(2) As2 0.0521(3) 0.0364(3) 0.0365(3) 0.0018(2) -0.0067(2) 0.0006(3) S1 0.0428(7) 0.0457(8) 0.0419(8) -0.0057(6) -0.0012(6) 0.0112(6) S2 0.0433(7) 0.0384(7) 0.0473(8) -0.0061(6) 0.0051(6) 0.0016(6) N1 0.040(2) 0.048(3) 0.034(2) -0.009(2) 0.0047(18) 0.000(2) N2 0.044(2) 0.042(3) 0.038(2) -0.005(2) -0.0009(19) 0.003(2) N3 0.044(3) 0.048(3) 0.041(3) 0.004(2) 0.001(2) 0.002(2) N4 0.064(3) 0.034(3) 0.057(3) -0.008(2) 0.003(2) 0.006(2) N5 0.051(3) 0.041(3) 0.042(3) -0.007(2) 0.004(2) 0.001(2) N6 0.051(3) 0.039(3) 0.037(2) 0.001(2) 0.001(2) 0.002(2) N7 0.062(3) 0.051(3) 0.036(3) -0.004(2) 0.005(2) 0.004(3) N8 0.039(2) 0.047(3) 0.056(3) -0.006(2) -0.003(2) 0.010(2) C1 0.057(3) 0.050(3) 0.035(3) -0.013(2) 0.009(2) -0.004(3) C2 0.057(3) 0.037(3) 0.045(3) -0.012(2) 0.011(3) 0.003(3) C3 0.072(5) 0.059(4) 0.084(5) -0.029(4) 0.001(4) 0.014(4) C4 0.118(8) 0.077(6) 0.112(8) -0.059(5) -0.001(6) 0.023(6) C5 0.095(6) 0.116(8) 0.102(7) -0.080(6) -0.007(5) -0.001(6) C6 0.067(4) 0.101(6) 0.073(5) -0.042(5) -0.008(4) -0.008(4) C7 0.043(3) 0.054(3) 0.034(3) -0.006(2) -0.002(2) -0.002(3) C8 0.043(3) 0.052(3) 0.037(3) -0.005(2) -0.001(2) 0.011(3) C9 0.049(4) 0.067(4) 0.071(4) -0.028(4) 0.004(3) 0.011(3) C10 0.043(4) 0.102(7) 0.080(5) -0.031(5) 0.011(3) 0.003(4) C11 0.046(4) 0.109(7) 0.060(4) -0.021(4) 0.011(3) -0.014(4) C12 0.053(3) 0.075(5) 0.043(3) -0.011(3) 0.000(3) -0.018(3) C13 0.056(4) 0.054(4) 0.056(4) -0.005(3) 0.006(3) -0.012(3) C14 0.058(4) 0.083(5) 0.058(4) -0.008(4) 0.012(3) -0.015(4) C15 0.046(3) 0.117(7) 0.046(4) -0.013(4) 0.010(3) -0.002(4) C16 0.045(3) 0.071(4) 0.052(4) -0.028(3) 0.001(3) 0.008(3) C17 0.039(3) 0.052(3) 0.032(3) -0.007(2) -0.002(2) 0.003(3) C18 0.038(3) 0.054(3) 0.037(3) -0.012(2) -0.010(2) 0.006(3) C19 0.054(3) 0.057(4) 0.052(4) -0.024(3) -0.006(3) 0.012(3) C20 0.071(4) 0.043(3) 0.054(4) -0.016(3) -0.013(3) 0.008(3) C21 0.061(4) 0.051(4) 0.062(4) -0.015(3) -0.001(3) -0.007(3) C22 0.047(3) 0.060(4) 0.050(4) -0.006(3) 0.006(3) -0.004(3) C23 0.043(3) 0.072(4) 0.043(3) -0.001(3) 0.003(2) -0.005(3) C24 0.051(4) 0.102(7) 0.056(4) 0.003(4) -0.014(3) -0.006(4) C25 0.065(5) 0.124(8) 0.069(5) 0.017(5) -0.027(4) 0.003(5) C26 0.072(5) 0.062(5) 0.085(6) 0.021(4) -0.014(4) 0.015(4) C27 0.051(3) 0.049(4) 0.057(4) 0.006(3) 0.002(3) 0.010(3) C28 0.063(4) 0.036(3) 0.073(5) 0.008(3) 0.005(3) 0.013(3) C29 0.116(7) 0.047(4) 0.105(7) -0.009(4) -0.029(6) 0.030(5) C30 0.129(8) 0.047(4) 0.120(8) -0.018(5) -0.020(7) 0.020(5) C31 0.131(8) 0.069(5) 0.099(7) -0.035(5) -0.012(6) -0.016(6) C32 0.091(5) 0.046(4) 0.057(4) -0.011(3) -0.010(4) 0.003(4) C33 0.047(3) 0.057(4) 0.060(4) -0.010(3) 0.001(3) -0.003(3) C34 0.062(4) 0.061(4) 0.067(4) -0.016(3) 0.006(3) -0.017(4) C35 0.080(5) 0.057(4) 0.075(5) 0.002(4) 0.012(4) -0.026(4) C36 0.075(5) 0.051(4) 0.066(5) 0.008(3) -0.002(4) 0.003(4) C37 0.061(4) 0.041(3) 0.037(3) -0.003(2) 0.004(2) -0.001(3) C38 0.056(3) 0.043(3) 0.039(3) -0.006(2) -0.008(2) 0.003(3) C39 0.062(4) 0.048(4) 0.082(5) 0.004(3) -0.014(4) 0.007(3) C40 0.051(4) 0.075(5) 0.112(7) -0.006(5) -0.018(4) 0.019(4) C41 0.045(3) 0.067(5) 0.093(6) 0.002(4) -0.007(3) 0.004(3) C42 0.046(3) 0.048(4) 0.065(4) 0.001(3) -0.008(3) 0.001(3) C43 0.079(5) 0.051(4) 0.045(4) -0.001(3) -0.001(3) 0.015(3) C44 0.107(6) 0.066(5) 0.041(4) -0.004(3) -0.003(4) -0.001(5) C45 0.110(7) 0.067(5) 0.050(4) -0.012(4) 0.026(4) 0.009(5) C46 0.075(5) 0.065(5) 0.062(5) -0.012(4) 0.025(4) 0.010(4) C47 0.059(4) 0.044(3) 0.053(4) -0.003(3) 0.024(3) 0.003(3) C48 0.045(3) 0.039(3) 0.056(4) -0.001(3) 0.008(3) 0.001(3) C49 0.045(4) 0.057(4) 0.090(6) -0.005(4) 0.013(4) 0.001(3) C50 0.037(3) 0.069(5) 0.118(7) 0.004(5) -0.007(4) 0.006(3) C51 0.053(4) 0.083(5) 0.089(6) -0.011(5) -0.025(4) -0.002(4) C52 0.047(3) 0.074(5) 0.065(4) -0.013(4) -0.007(3) 0.004(3) O1 0.042(2) 0.056(2) 0.035(2) 0.0013(18) 0.0005(15) 0.0125(18) O2 0.051(2) 0.065(3) 0.053(3) 0.013(2) -0.0136(19) -0.008(2) O3 0.054(2) 0.035(2) 0.043(2) -0.0029(16) -0.0115(17) 0.0014(18) O4 0.086(3) 0.066(3) 0.070(3) -0.001(3) -0.020(3) 0.038(3) O5 0.044(2) 0.078(3) 0.061(3) -0.021(2) 0.0103(19) -0.014(2) O6 0.0400(19) 0.048(2) 0.041(2) -0.0071(17) 0.0028(15) 0.0095(17) O7 0.102(4) 0.039(2) 0.053(3) 0.005(2) -0.022(2) -0.013(2) O8 0.066(3) 0.044(2) 0.037(2) -0.0041(17) 0.0011(18) 0.007(2) O9 0.055(2) 0.048(2) 0.048(2) 0.0040(19) -0.0153(18) 0.005(2) O10 0.074(3) 0.050(3) 0.113(5) 0.018(3) 0.014(3) 0.013(3) O11 0.075(3) 0.110(4) 0.053(3) -0.032(3) 0.005(2) -0.038(3) O12 0.049(2) 0.053(2) 0.038(2) -0.0117(18) 0.0060(16) 0.0022(19) O1W 0.084(4) 0.075(4) 0.132(5) -0.023(4) -0.018(4) -0.016(3) O2W 0.067(4) 0.172(8) 0.218(9) -0.116(7) 0.040(5) -0.033(5) O3W 0.220(10) 0.165(8) 0.109(6) -0.050(6) -0.026(6) -0.051(8) O4W 0.206(10) 0.170(9) 0.150(8) -0.057(7) -0.012(7) 0.015(8) O5W 0.068(9) 0.136(13) 0.148(12) -0.068(9) -0.020(8) 0.024(8) O6W 0.159(15) 0.096(11) 0.28(2) -0.114(13) 0.093(15) -0.035(10) O7W 0.138(13) 0.168(15) 0.082(9) -0.021(9) 0.003(8) 0.012(11) O8W 0.126(14) 0.175(18) 0.21(2) -0.099(16) -0.031(13) 0.009(13) _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 1.991(4) . ? Zn1 N2 2.143(5) . ? Zn1 N4 2.153(5) . ? Zn1 N1 2.156(4) . ? Zn1 N3 2.168(5) . ? Zn1 O6 2.257(4) . ? Zn2 O8 2.021(4) . ? Zn2 N6 2.135(5) . ? Zn2 N8 2.141(5) . ? Zn2 N7 2.142(5) . ? Zn2 O12 2.160(4) . ? Zn2 N5 2.203(5) . ? As1 O1 1.660(4) . ? As1 O3 1.662(4) . ? As1 O2 1.729(4) . ? As1 C1 1.945(6) . ? As2 O8 1.662(4) . ? As2 O7 1.667(4) . ? As2 O9 1.703(4) . ? As2 C7 1.942(6) . ? S1 O4 1.433(5) . ? S1 O5 1.447(4) . ? S1 O6 1.453(4) . ? S1 C2 1.791(7) . ? S2 O11 1.428(5) . ? S2 O10 1.437(5) . ? S2 O12 1.459(4) . ? S2 C8 1.784(6) . ? N1 C17 1.329(7) . ? N1 C13 1.337(7) . ? N2 C22 1.324(7) . ? N2 C18 1.350(7) . ? N3 C27 1.323(8) . ? N3 C23 1.349(8) . ? N4 C32 1.315(9) . ? N4 C28 1.361(8) . ? N5 C33 1.323(7) . ? N5 C37 1.342(8) . ? N6 C42 1.333(7) . ? N6 C38 1.348(7) . ? N7 C43 1.337(9) . ? N7 C47 1.345(8) . ? N8 C52 1.337(8) . ? N8 C48 1.362(8) . ? C1 C6 1.370(9) . ? C1 C2 1.388(9) . ? C2 C3 1.387(9) . ? C3 C4 1.386(12) . ? C3 H3A 0.9300 . ? C4 C5 1.367(13) . ? C4 H4A 0.9300 . ? C5 C6 1.383(12) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.391(8) . ? C7 C8 1.398(8) . ? C8 C9 1.391(8) . ? C9 C10 1.382(9) . ? C9 H9B 0.9300 . ? C10 C11 1.365(11) . ? C10 H10A 0.9300 . ? C11 C12 1.378(10) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.376(9) . ? C13 H13A 0.9300 . ? C14 C15 1.361(11) . ? C14 H14A 0.9300 . ? C15 C16 1.387(10) . ? C15 H15A 0.9300 . ? C16 C17 1.389(7) . ? C16 H16A 0.9300 . ? C17 C18 1.492(8) . ? C18 C19 1.374(8) . ? C19 C20 1.369(9) . ? C19 H19A 0.9300 . ? C20 C21 1.364(9) . ? C20 H20A 0.9300 . ? C21 C22 1.375(9) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.384(9) . ? C23 H23A 0.9300 . ? C24 C25 1.363(13) . ? C24 H24A 0.9300 . ? C25 C26 1.358(13) . ? C25 H25A 0.9300 . ? C26 C27 1.422(9) . ? C26 H26A 0.9300 . ? C27 C28 1.472(11) . ? C28 C29 1.361(10) . ? C29 C30 1.355(13) . ? C29 H29A 0.9300 . ? C30 C31 1.401(13) . ? C30 H30A 0.9300 . ? C31 C32 1.379(10) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.375(9) . ? C33 H33A 0.9300 . ? C34 C35 1.347(11) . ? C34 H34A 0.9300 . ? C35 C36 1.421(10) . ? C35 H35A 0.9300 . ? C36 C37 1.404(8) . ? C36 H36A 0.9300 . ? C37 C38 1.455(8) . ? C38 C39 1.387(9) . ? C39 C40 1.345(10) . ? C39 H39A 0.9300 . ? C40 C41 1.396(10) . ? C40 H40A 0.9300 . ? C41 C42 1.375(9) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 C44 1.400(10) . ? C43 H43A 0.9300 . ? C44 C45 1.358(11) . ? C44 H44A 0.9300 . ? C45 C46 1.375(12) . ? C45 H45A 0.9300 . ? C46 C47 1.405(9) . ? C46 H46A 0.9300 . ? C47 C48 1.463(10) . ? C48 C49 1.399(9) . ? C49 C50 1.372(11) . ? C49 H49A 0.9300 . ? C50 C51 1.368(12) . ? C50 H50A 0.9300 . ? C51 C52 1.380(10) . ? C51 H51A 0.9300 . ? C52 H52A 0.9300 . ? O2 H2A 0.8200 . ? O9 H9A 0.8200 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8499 . ? O3W H3WB 0.8499 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8501 . ? O5W O5W 1.18(2) 2_676 ? O6W H6WB 0.8500 . ? O6W H6WA 0.8500 . ? O8W H8WA 0.8500 . ? O8W H8WB 0.8500 . ? 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 N2 94.55(18) . . ? O1 Zn1 N4 93.1(2) . . ? N2 Zn1 N4 170.74(18) . . ? O1 Zn1 N1 94.76(16) . . ? N2 Zn1 N1 76.91(18) . . ? N4 Zn1 N1 97.22(19) . . ? O1 Zn1 N3 165.97(19) . . ? N2 Zn1 N3 97.63(19) . . ? N4 Zn1 N3 75.5(2) . . ? N1 Zn1 N3 94.77(17) . . ? O1 Zn1 O6 83.11(14) . . ? N2 Zn1 O6 90.10(16) . . ? N4 Zn1 O6 96.05(17) . . ? N1 Zn1 O6 166.66(17) . . ? N3 Zn1 O6 89.90(15) . . ? O8 Zn2 N6 94.56(17) . . ? O8 Zn2 N8 94.25(18) . . ? N6 Zn2 N8 170.88(17) . . ? O8 Zn2 N7 95.73(18) . . ? N6 Zn2 N7 100.0(2) . . ? N8 Zn2 N7 76.7(2) . . ? O8 Zn2 O12 84.92(16) . . ? N6 Zn2 O12 94.67(17) . . ? N8 Zn2 O12 88.43(18) . . ? N7 Zn2 O12 165.16(18) . . ? O8 Zn2 N5 169.23(18) . . ? N6 Zn2 N5 75.48(18) . . ? N8 Zn2 N5 95.88(18) . . ? N7 Zn2 N5 90.13(18) . . ? O12 Zn2 N5 91.73(17) . . ? O1 As1 O3 118.0(2) . . ? O1 As1 O2 101.0(2) . . ? O3 As1 O2 107.89(19) . . ? O1 As1 C1 112.9(2) . . ? O3 As1 C1 111.9(2) . . ? O2 As1 C1 103.3(3) . . ? O8 As2 O7 107.7(2) . . ? O8 As2 O9 111.5(2) . . ? O7 As2 O9 108.8(2) . . ? O8 As2 C7 114.4(2) . . ? O7 As2 C7 105.8(3) . . ? O9 As2 C7 108.4(2) . . ? O4 S1 O5 114.3(3) . . ? O4 S1 O6 112.3(3) . . ? O5 S1 O6 111.9(3) . . ? O4 S1 C2 106.7(3) . . ? O5 S1 C2 104.5(3) . . ? O6 S1 C2 106.2(3) . . ? O11 S2 O10 115.6(4) . . ? O11 S2 O12 112.4(3) . . ? O10 S2 O12 111.0(3) . . ? O11 S2 C8 106.3(3) . . ? O10 S2 C8 104.2(3) . . ? O12 S2 C8 106.5(3) . . ? C17 N1 C13 119.4(5) . . ? C17 N1 Zn1 114.9(3) . . ? C13 N1 Zn1 125.7(4) . . ? C22 N2 C18 119.0(5) . . ? C22 N2 Zn1 125.1(4) . . ? C18 N2 Zn1 115.3(4) . . ? C27 N3 C23 118.8(6) . . ? C27 N3 Zn1 116.4(5) . . ? C23 N3 Zn1 124.8(4) . . ? C32 N4 C28 119.7(6) . . ? C32 N4 Zn1 124.2(4) . . ? C28 N4 Zn1 116.0(5) . . ? C33 N5 C37 120.6(5) . . ? C33 N5 Zn2 124.8(4) . . ? C37 N5 Zn2 114.2(4) . . ? C42 N6 C38 119.5(5) . . ? C42 N6 Zn2 123.2(4) . . ? C38 N6 Zn2 117.1(4) . . ? C43 N7 C47 120.1(6) . . ? C43 N7 Zn2 124.3(5) . . ? C47 N7 Zn2 115.6(4) . . ? C52 N8 C48 119.1(6) . . ? C52 N8 Zn2 125.0(4) . . ? C48 N8 Zn2 115.0(4) . . ? C6 C1 C2 119.0(6) . . ? C6 C1 As1 115.8(6) . . ? C2 C1 As1 125.1(5) . . ? C3 C2 C1 120.6(6) . . ? C3 C2 S1 114.7(5) . . ? C1 C2 S1 124.7(4) . . ? C4 C3 C2 119.2(8) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C5 C4 C3 120.2(8) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 120.0(8) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C1 C6 C5 120.9(8) . . ? C1 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C12 C7 C8 119.0(6) . . ? C12 C7 As2 114.0(5) . . ? C8 C7 As2 127.0(4) . . ? C9 C8 C7 119.4(6) . . ? C9 C8 S2 115.6(5) . . ? C7 C8 S2 125.0(4) . . ? C10 C9 C8 120.5(7) . . ? C10 C9 H9B 119.8 . . ? C8 C9 H9B 119.8 . . ? C11 C10 C9 120.0(7) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.5(6) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C11 C12 C7 120.5(7) . . ? C11 C12 H12A 119.7 . . ? C7 C12 H12A 119.7 . . ? N1 C13 C14 123.1(7) . . ? N1 C13 H13A 118.4 . . ? C14 C13 H13A 118.4 . . ? C15 C14 C13 117.6(7) . . ? C15 C14 H14A 121.2 . . ? C13 C14 H14A 121.2 . . ? C14 C15 C16 120.3(6) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C15 C16 C17 118.7(6) . . ? C15 C16 H16A 120.6 . . ? C17 C16 H16A 120.6 . . ? N1 C17 C16 120.9(5) . . ? N1 C17 C18 117.0(5) . . ? C16 C17 C18 122.2(6) . . ? N2 C18 C19 121.4(5) . . ? N2 C18 C17 115.3(5) . . ? C19 C18 C17 123.3(5) . . ? C20 C19 C18 119.2(6) . . ? C20 C19 H19A 120.4 . . ? C18 C19 H19A 120.4 . . ? C21 C20 C19 119.2(6) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C20 C21 C22 119.4(6) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? N2 C22 C21 121.8(6) . . ? N2 C22 H22A 119.1 . . ? C21 C22 H22A 119.1 . . ? N3 C23 C24 122.7(7) . . ? N3 C23 H23A 118.6 . . ? C24 C23 H23A 118.6 . . ? C25 C24 C23 117.9(8) . . ? C25 C24 H24A 121.0 . . ? C23 C24 H24A 121.0 . . ? C26 C25 C24 121.0(7) . . ? C26 C25 H25A 119.5 . . ? C24 C25 H25A 119.5 . . ? C25 C26 C27 118.3(8) . . ? C25 C26 H26A 120.9 . . ? C27 C26 H26A 120.9 . . ? N3 C27 C26 121.3(7) . . ? N3 C27 C28 116.5(5) . . ? C26 C27 C28 122.3(7) . . ? C29 C28 N4 120.0(8) . . ? C29 C28 C27 124.6(7) . . ? N4 C28 C27 115.4(6) . . ? C30 C29 C28 120.3(8) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 120.3(8) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C32 C31 C30 116.2(9) . . ? C32 C31 H31A 121.9 . . ? C30 C31 H31A 121.9 . . ? N4 C32 C31 123.4(7) . . ? N4 C32 H32A 118.3 . . ? C31 C32 H32A 118.3 . . ? N5 C33 C34 122.4(6) . . ? N5 C33 H33A 118.8 . . ? C34 C33 H33A 118.8 . . ? C35 C34 C33 118.7(6) . . ? C35 C34 H34A 120.7 . . ? C33 C34 H34A 120.7 . . ? C34 C35 C36 120.9(6) . . ? C34 C35 H35A 119.6 . . ? C36 C35 H35A 119.6 . . ? C37 C36 C35 116.6(7) . . ? C37 C36 H36A 121.7 . . ? C35 C36 H36A 121.7 . . ? N5 C37 C36 120.8(6) . . ? N5 C37 C38 117.1(5) . . ? C36 C37 C38 122.1(6) . . ? N6 C38 C39 119.5(6) . . ? N6 C38 C37 115.7(5) . . ? C39 C38 C37 124.8(5) . . ? C40 C39 C38 120.8(6) . . ? C40 C39 H39A 119.6 . . ? C38 C39 H39A 119.6 . . ? C39 C40 C41 120.1(7) . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C42 C41 C40 116.7(6) . . ? C42 C41 H41A 121.7 . . ? C40 C41 H41A 121.7 . . ? N6 C42 C41 123.4(6) . . ? N6 C42 H42A 118.3 . . ? C41 C42 H42A 118.3 . . ? N7 C43 C44 121.2(7) . . ? N7 C43 H43A 119.4 . . ? C44 C43 H43A 119.4 . . ? C45 C44 C43 118.8(8) . . ? C45 C44 H44A 120.6 . . ? C43 C44 H44A 120.6 . . ? C44 C45 C46 120.9(7) . . ? C44 C45 H45A 119.6 . . ? C46 C45 H45A 119.6 . . ? C45 C46 C47 118.1(7) . . ? C45 C46 H46A 120.9 . . ? C47 C46 H46A 120.9 . . ? N7 C47 C46 120.9(7) . . ? N7 C47 C48 116.4(6) . . ? C46 C47 C48 122.7(7) . . ? N8 C48 C49 120.2(7) . . ? N8 C48 C47 115.9(5) . . ? C49 C48 C47 123.9(6) . . ? C50 C49 C48 118.9(7) . . ? C50 C49 H49A 120.6 . . ? C48 C49 H49A 120.6 . . ? C51 C50 C49 121.0(7) . . ? C51 C50 H50A 119.5 . . ? C49 C50 H50A 119.5 . . ? C50 C51 C52 117.7(8) . . ? C50 C51 H51A 121.2 . . ? C52 C51 H51A 121.2 . . ? N8 C52 C51 123.0(7) . . ? N8 C52 H52A 118.5 . . ? C51 C52 H52A 118.5 . . ? As1 O1 Zn1 126.5(2) . . ? As1 O2 H2A 109.5 . . ? S1 O6 Zn1 137.1(2) . . ? As2 O8 Zn2 126.3(2) . . ? As2 O9 H9A 109.5 . . ? S2 O12 Zn2 143.2(3) . . ? H1WA O1W H1WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? H3WA O3W H3WB 109.5 . . ? H4WA O4W H4WB 109.5 . . ? H6WB O6W H6WA 109.5 . . ? H8WA O8W H8WB 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2A O7 0.82 1.68 2.492(6) 167.6 . O9 H9A O3 0.82 1.76 2.569(5) 170.5 . O1W H1WA O5 0.85 2.42 2.911(8) 117.8 . O1W H1WB O3 0.85 2.01 2.863(7) 178.9 . O2W H2WA O2 0.85 1.93 2.775(8) 179.4 . O2W H2WB O5 0.85 2.53 2.928(8) 110.1 1_455 O3W H3WA O7 0.85 1.82 2.668(9) 178.3 . O3W H3WB O5W 0.85 2.27 2.82(2) 122.1 . O4W H4WA O2W 0.85 2.23 2.836(12) 127.8 . O4W H4WB O3W 0.85 1.89 2.742(13) 177.3 . O6W H6WA O7W 0.85 2.14 2.65(2) 118.5 . O8W H8WA O7W 0.85 1.86 2.71(2) 178.9 . _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.467 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.108 #===end data_4 _database_code_depnum_ccdc_archive 'CCDC 763193' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 As2 Cd2 N4 O12 S2' _chemical_formula_weight 1097.33 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' 'S' 'S' 0.1246 0.1234 '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' 'Cd' 'Cd' -0.8075 1.2024 '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 8.191(5) _cell_length_b 20.656(12) _cell_length_c 21.283(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.942(13) _cell_angle_gamma 90.00 _cell_volume 3588(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7157 _cell_measurement_theta_min 3.0459 _cell_measurement_theta_max 27.4797 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.032 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 3.202 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.5957 _exptl_absorpt_correction_T_max 1 _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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27333 _diffrn_reflns_av_R_equivalents 0.0870 _diffrn_reflns_av_sigmaI/netI 0.0854 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7828 _reflns_number_gt 5678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0460P)^2^+22.2040P] 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 SHELXL _refine_ls_extinction_coef 0.000357 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7828 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1569 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.59260(8) 0.26337(3) 0.21497(3) 0.0314(2) Uani 1 1 d . . . Cd2 Cd 0.43752(9) 0.43708(3) 0.29302(3) 0.0329(2) Uani 1 1 d . . . As1 As 0.81840(11) 0.36360(4) 0.32060(4) 0.0294(2) Uani 1 1 d . . . As2 As 0.21424(12) 0.33914(4) 0.18407(4) 0.0297(2) Uani 1 1 d . . . S1 S 0.4768(3) 0.30967(12) 0.38258(12) 0.0343(6) Uani 1 1 d . . . S2 S 0.5647(3) 0.39163(11) 0.12751(12) 0.0345(6) Uani 1 1 d . . . N1 N 0.5585(10) 0.1593(3) 0.2560(4) 0.0357(19) Uani 1 1 d . . . N2 N 0.7108(10) 0.1860(4) 0.1526(4) 0.0346(19) Uani 1 1 d . . . N3 N 0.3119(10) 0.5109(4) 0.3568(4) 0.040(2) Uani 1 1 d . . . N4 N 0.4456(11) 0.5420(4) 0.2491(4) 0.040(2) Uani 1 1 d . . . C1 C 0.8131(12) 0.3136(4) 0.3967(5) 0.035(2) Uani 1 1 d . . . C2 C 0.6714(12) 0.2923(4) 0.4214(5) 0.034(2) Uani 1 1 d . . . C3 C 0.6814(15) 0.2559(5) 0.4752(5) 0.048(3) Uani 1 1 d . . . H3B H 0.5858 0.2422 0.4917 0.057 Uiso 1 1 calc R . . C4 C 0.8299(16) 0.2393(5) 0.5051(6) 0.057(3) Uani 1 1 d . . . H4A H 0.8348 0.2148 0.5419 0.068 Uiso 1 1 calc R . . C5 C 0.9720(15) 0.2588(6) 0.4808(6) 0.056(3) Uani 1 1 d . . . H5A H 1.0731 0.2479 0.5013 0.067 Uiso 1 1 calc R . . C6 C 0.9648(13) 0.2947(5) 0.4256(5) 0.046(3) Uani 1 1 d . . . H6A H 1.0606 0.3062 0.4080 0.055 Uiso 1 1 calc R . . C7 C 0.2276(12) 0.3864(4) 0.1063(5) 0.033(2) Uani 1 1 d . . . C8 C 0.3735(12) 0.4056(4) 0.0838(5) 0.035(2) Uani 1 1 d . . . C9 C 0.3754(15) 0.4322(5) 0.0249(5) 0.047(3) Uani 1 1 d . . . H9B H 0.4741 0.4437 0.0094 0.056 Uiso 1 1 calc R . . C10 C 0.2288(17) 0.4418(6) -0.0113(6) 0.066(4) Uani 1 1 d . . . H10A H 0.2291 0.4596 -0.0514 0.080 Uiso 1 1 calc R . . C11 C 0.0840(17) 0.4254(7) 0.0114(7) 0.070(4) Uani 1 1 d . . . H11A H -0.0143 0.4336 -0.0125 0.085 Uiso 1 1 calc R . . C12 C 0.0828(15) 0.3962(5) 0.0703(5) 0.051(3) Uani 1 1 d . . . H12A H -0.0157 0.3834 0.0852 0.061 Uiso 1 1 calc R . . C13 C 0.4832(14) 0.1471(5) 0.3081(5) 0.050(3) Uani 1 1 d . . . H13A H 0.4461 0.1818 0.3308 0.060 Uiso 1 1 calc R . . C14 C 0.4586(15) 0.0857(6) 0.3295(6) 0.057(3) Uani 1 1 d . . . H14A H 0.4101 0.0795 0.3669 0.068 Uiso 1 1 calc R . . C15 C 0.5048(17) 0.0335(5) 0.2960(5) 0.059(3) Uani 1 1 d . . . H15A H 0.4829 -0.0085 0.3085 0.071 Uiso 1 1 calc R . . C16 C 0.5835(15) 0.0451(5) 0.2441(6) 0.052(3) Uani 1 1 d . . . H16A H 0.6205 0.0106 0.2211 0.062 Uiso 1 1 calc R . . C17 C 0.6097(12) 0.1078(4) 0.2248(5) 0.038(2) Uani 1 1 d . . . C18 C 0.6941(12) 0.1238(4) 0.1674(5) 0.032(2) Uani 1 1 d . . . C19 C 0.7454(12) 0.0744(5) 0.1282(5) 0.041(2) Uani 1 1 d . . . H19A H 0.7266 0.0312 0.1375 0.049 Uiso 1 1 calc R . . C20 C 0.8234(15) 0.0908(5) 0.0763(5) 0.050(3) Uani 1 1 d . . . H20A H 0.8619 0.0587 0.0506 0.060 Uiso 1 1 calc R . . C21 C 0.8444(14) 0.1548(5) 0.0623(5) 0.048(3) Uani 1 1 d . . . H21A H 0.8957 0.1668 0.0268 0.057 Uiso 1 1 calc R . . C22 C 0.7891(13) 0.2006(5) 0.1012(5) 0.043(3) Uani 1 1 d . . . H22A H 0.8062 0.2440 0.0920 0.052 Uiso 1 1 calc R . . C23 C 0.2454(14) 0.4949(5) 0.4084(6) 0.051(3) Uani 1 1 d . . . H23A H 0.2431 0.4512 0.4188 0.061 Uiso 1 1 calc R . . C24 C 0.1786(15) 0.5381(6) 0.4486(6) 0.060(3) Uani 1 1 d . . . H24A H 0.1368 0.5247 0.4857 0.072 Uiso 1 1 calc R . . C25 C 0.1773(15) 0.6026(6) 0.4305(6) 0.058(3) Uani 1 1 d . . . H25A H 0.1320 0.6335 0.4556 0.070 Uiso 1 1 calc R . . C26 C 0.2412(14) 0.6207(5) 0.3771(6) 0.051(3) Uani 1 1 d . . . H26A H 0.2386 0.6639 0.3647 0.062 Uiso 1 1 calc R . . C27 C 0.3114(12) 0.5740(5) 0.3402(5) 0.040(2) Uani 1 1 d . . . C28 C 0.3874(13) 0.5912(5) 0.2824(5) 0.041(2) Uani 1 1 d . . . C29 C 0.3952(15) 0.6541(5) 0.2610(6) 0.054(3) Uani 1 1 d . . . H29A H 0.3530 0.6876 0.2839 0.065 Uiso 1 1 calc R . . C30 C 0.4646(16) 0.6671(5) 0.2064(7) 0.063(4) Uani 1 1 d . . . H30A H 0.4693 0.7095 0.1919 0.076 Uiso 1 1 calc R . . C31 C 0.5263(17) 0.6187(5) 0.1735(6) 0.061(4) Uani 1 1 d . . . H31A H 0.5750 0.6268 0.1364 0.073 Uiso 1 1 calc R . . C32 C 0.5148(15) 0.5555(5) 0.1969(5) 0.051(3) Uani 1 1 d . . . H32A H 0.5579 0.5217 0.1747 0.061 Uiso 1 1 calc R . . O1 O 0.8115(7) 0.3155(3) 0.2578(3) 0.0315(14) Uani 1 1 d . . . O2 O 0.6982(8) 0.4279(3) 0.3186(3) 0.0364(16) Uani 1 1 d . . . O3 O 1.0125(8) 0.3943(4) 0.3302(3) 0.0484(19) Uani 1 1 d . . . H3A H 1.0595 0.3872 0.2985 0.073 Uiso 1 1 calc R . . O4 O 0.5020(9) 0.3048(3) 0.3150(3) 0.0430(17) Uani 1 1 d . . . O5 O 0.4368(9) 0.3758(3) 0.3968(4) 0.0449(18) Uani 1 1 d . . . O6 O 0.3654(9) 0.2619(3) 0.4038(4) 0.0488(19) Uani 1 1 d . . . O7 O 0.2180(7) 0.3871(3) 0.2469(3) 0.0333(15) Uani 1 1 d . . . O8 O 0.3315(8) 0.2743(3) 0.1866(3) 0.0344(15) Uani 1 1 d . . . O9 O 0.0177(8) 0.3097(3) 0.1722(3) 0.0426(18) Uani 1 1 d . . . H9A H -0.0303 0.3159 0.2039 0.064 Uiso 1 1 calc R . . O10 O 0.5248(8) 0.3981(3) 0.1924(3) 0.0368(16) Uani 1 1 d . . . O11 O 0.6130(8) 0.3261(3) 0.1150(3) 0.0427(18) Uani 1 1 d . . . O12 O 0.6765(9) 0.4393(4) 0.1082(4) 0.053(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0281(4) 0.0275(3) 0.0390(4) -0.0033(3) 0.0057(3) -0.0011(3) Cd2 0.0298(4) 0.0269(3) 0.0426(4) -0.0045(3) 0.0057(3) 0.0001(3) As1 0.0240(5) 0.0308(5) 0.0343(5) -0.0039(4) 0.0078(4) -0.0039(4) As2 0.0241(5) 0.0310(5) 0.0350(5) -0.0019(4) 0.0076(4) -0.0022(4) S1 0.0283(13) 0.0355(12) 0.0406(13) 0.0043(10) 0.0123(11) 0.0008(10) S2 0.0342(14) 0.0301(11) 0.0413(13) 0.0008(10) 0.0147(11) -0.0023(10) N1 0.032(5) 0.025(4) 0.051(5) 0.003(4) 0.009(4) -0.004(3) N2 0.031(5) 0.030(4) 0.042(5) -0.004(4) 0.002(4) 0.009(3) N3 0.040(5) 0.026(4) 0.055(6) -0.009(4) 0.005(4) 0.001(4) N4 0.044(5) 0.027(4) 0.050(5) 0.000(4) 0.003(4) 0.004(4) C1 0.041(6) 0.028(5) 0.038(5) -0.005(4) 0.012(5) -0.003(4) C2 0.031(5) 0.031(5) 0.040(5) -0.002(4) 0.005(4) -0.002(4) C3 0.058(8) 0.039(6) 0.048(6) 0.017(5) 0.017(6) -0.003(5) C4 0.063(9) 0.043(6) 0.063(8) 0.020(6) 0.003(7) 0.003(6) C5 0.046(8) 0.061(7) 0.057(7) 0.015(6) -0.017(6) 0.005(6) C6 0.024(6) 0.057(7) 0.057(7) -0.005(6) -0.003(5) 0.005(5) C7 0.033(6) 0.030(5) 0.038(5) 0.003(4) 0.010(5) 0.003(4) C8 0.042(6) 0.027(4) 0.037(5) 0.003(4) 0.000(5) -0.004(4) C9 0.056(7) 0.046(6) 0.040(6) 0.014(5) 0.008(6) -0.009(5) C10 0.071(10) 0.073(9) 0.055(8) 0.024(7) 0.009(7) 0.002(8) C11 0.055(9) 0.074(9) 0.080(10) 0.027(8) -0.008(8) 0.020(7) C12 0.051(7) 0.049(6) 0.054(7) 0.007(6) 0.005(6) 0.007(6) C13 0.056(8) 0.043(6) 0.053(7) -0.009(5) 0.017(6) -0.009(5) C14 0.058(8) 0.060(7) 0.055(7) 0.008(6) 0.018(6) -0.010(6) C15 0.094(10) 0.035(6) 0.049(7) 0.011(5) 0.010(7) 0.011(6) C16 0.062(8) 0.021(5) 0.074(8) -0.004(5) 0.012(7) 0.001(5) C17 0.036(6) 0.027(5) 0.051(6) 0.003(4) 0.005(5) 0.000(4) C18 0.032(5) 0.021(4) 0.043(5) -0.005(4) -0.002(5) 0.001(4) C19 0.035(6) 0.032(5) 0.056(7) 0.000(5) 0.002(5) 0.009(4) C20 0.061(8) 0.042(6) 0.047(6) -0.015(5) 0.001(6) 0.008(6) C21 0.052(7) 0.049(6) 0.043(6) -0.004(5) 0.015(6) 0.010(5) C22 0.042(6) 0.041(6) 0.048(6) -0.005(5) 0.009(5) 0.004(5) C23 0.058(8) 0.034(5) 0.063(7) 0.007(5) 0.021(6) 0.007(5) C24 0.059(8) 0.050(7) 0.074(8) -0.018(6) 0.025(7) 0.008(6) C25 0.050(7) 0.065(8) 0.061(8) -0.024(6) 0.013(6) 0.018(6) C26 0.055(8) 0.041(6) 0.058(7) -0.014(5) 0.002(6) 0.014(5) C27 0.019(5) 0.047(6) 0.052(6) -0.007(5) -0.008(5) 0.003(4) C28 0.036(6) 0.034(5) 0.052(6) -0.005(5) -0.007(5) 0.007(5) C29 0.065(8) 0.025(5) 0.071(8) -0.006(5) -0.003(7) 0.008(5) C30 0.074(9) 0.029(6) 0.087(10) 0.008(6) 0.009(8) -0.006(6) C31 0.086(10) 0.032(6) 0.066(8) 0.007(6) 0.009(7) -0.013(6) C32 0.070(8) 0.030(5) 0.055(7) 0.005(5) 0.018(6) 0.003(5) O1 0.024(3) 0.037(3) 0.035(3) -0.004(3) 0.011(3) -0.003(3) O2 0.031(4) 0.028(3) 0.050(4) -0.001(3) 0.005(3) -0.005(3) O3 0.022(4) 0.072(5) 0.053(5) -0.013(4) 0.013(3) -0.017(4) O4 0.039(4) 0.053(4) 0.038(4) -0.002(3) 0.009(3) -0.003(3) O5 0.043(4) 0.031(3) 0.063(5) -0.004(3) 0.015(4) 0.012(3) O6 0.037(4) 0.047(4) 0.065(5) 0.008(4) 0.025(4) -0.007(3) O7 0.026(4) 0.040(4) 0.035(3) -0.014(3) 0.009(3) -0.007(3) O8 0.029(4) 0.026(3) 0.051(4) -0.005(3) 0.012(3) -0.001(3) O9 0.024(4) 0.064(5) 0.041(4) -0.020(3) 0.010(3) -0.014(3) O10 0.039(4) 0.037(4) 0.037(4) -0.002(3) 0.015(3) 0.000(3) O11 0.041(4) 0.035(4) 0.055(4) -0.003(3) 0.018(4) 0.009(3) O12 0.046(5) 0.049(4) 0.067(5) 0.015(4) 0.023(4) -0.014(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 Cd1 O8 2.183(7) . ? Cd1 O1 2.218(6) . ? Cd1 N2 2.340(7) . ? Cd1 N1 2.346(7) . ? Cd1 O4 2.468(7) . ? Cd1 O11 2.509(7) . ? Cd2 O2 2.166(7) . ? Cd2 O7 2.227(6) . ? Cd2 N3 2.339(8) . ? Cd2 N4 2.363(8) . ? Cd2 O10 2.451(6) . ? Cd2 O5 2.546(7) . ? As1 O2 1.652(6) . ? As1 O1 1.663(6) . ? As1 O3 1.707(6) . ? As1 C1 1.925(10) . ? As2 O8 1.646(6) . ? As2 O7 1.662(6) . ? As2 O9 1.718(6) . ? As2 C7 1.933(9) . ? S1 O5 1.442(7) . ? S1 O6 1.443(7) . ? S1 O4 1.474(7) . ? S1 C2 1.767(10) . ? S2 O12 1.429(7) . ? S2 O11 1.441(7) . ? S2 O10 1.453(6) . ? S2 C8 1.775(10) . ? N1 C13 1.339(13) . ? N1 C17 1.340(12) . ? N2 C18 1.334(11) . ? N2 C22 1.348(13) . ? N3 C23 1.309(13) . ? N3 C27 1.350(13) . ? N4 C32 1.319(13) . ? N4 C28 1.350(12) . ? C1 C2 1.386(13) . ? C1 C6 1.393(14) . ? C2 C3 1.368(13) . ? C3 C4 1.367(16) . ? C3 H3B 0.9300 . ? C4 C5 1.375(17) . ? C4 H4A 0.9300 . ? C5 C6 1.385(15) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.370(15) . ? C7 C8 1.383(13) . ? C8 C9 1.370(13) . ? C9 C10 1.384(17) . ? C9 H9B 0.9300 . ? C10 C11 1.362(18) . ? C10 H10A 0.9300 . ? C11 C12 1.393(17) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.369(15) . ? C13 H13A 0.9300 . ? C14 C15 1.362(16) . ? C14 H14A 0.9300 . ? C15 C16 1.348(16) . ? C15 H15A 0.9300 . ? C16 C17 1.382(13) . ? C16 H16A 0.9300 . ? C17 C18 1.492(13) . ? C18 C19 1.405(13) . ? C19 C20 1.365(15) . ? C19 H19A 0.9300 . ? C20 C21 1.370(15) . ? C20 H20A 0.9300 . ? C21 C22 1.361(13) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.380(15) . ? C23 H23A 0.9300 . ? C24 C25 1.386(17) . ? C24 H24A 0.9300 . ? C25 C26 1.346(16) . ? C25 H25A 0.9300 . ? C26 C27 1.398(14) . ? C26 H26A 0.9300 . ? C27 C28 1.470(15) . ? C28 C29 1.380(14) . ? C29 C30 1.365(17) . ? C29 H29A 0.9300 . ? C30 C31 1.345(17) . ? C30 H30A 0.9300 . ? C31 C32 1.403(14) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? O3 H3A 0.8200 . ? O9 H9A 0.8200 . ? 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 O8 Cd1 O1 143.2(2) . . ? O8 Cd1 N2 110.9(3) . . ? O1 Cd1 N2 101.8(3) . . ? O8 Cd1 N1 93.0(3) . . ? O1 Cd1 N1 114.2(3) . . ? N2 Cd1 N1 69.8(3) . . ? O8 Cd1 O4 80.9(2) . . ? O1 Cd1 O4 76.7(2) . . ? N2 Cd1 O4 153.7(3) . . ? N1 Cd1 O4 86.7(3) . . ? O8 Cd1 O11 81.2(2) . . ? O1 Cd1 O11 89.2(2) . . ? N2 Cd1 O11 79.1(2) . . ? N1 Cd1 O11 143.9(3) . . ? O4 Cd1 O11 126.8(2) . . ? O2 Cd2 O7 144.2(2) . . ? O2 Cd2 N3 112.6(3) . . ? O7 Cd2 N3 100.4(3) . . ? O2 Cd2 N4 96.8(3) . . ? O7 Cd2 N4 107.5(3) . . ? N3 Cd2 N4 70.1(3) . . ? O2 Cd2 O10 80.5(2) . . ? O7 Cd2 O10 75.4(2) . . ? N3 Cd2 O10 153.8(3) . . ? N4 Cd2 O10 86.3(3) . . ? O2 Cd2 O5 79.3(2) . . ? O7 Cd2 O5 95.1(2) . . ? N3 Cd2 O5 77.7(3) . . ? N4 Cd2 O5 143.3(3) . . ? O10 Cd2 O5 128.1(2) . . ? O2 As1 O1 118.8(3) . . ? O2 As1 O3 104.6(3) . . ? O1 As1 O3 106.6(3) . . ? O2 As1 C1 113.3(4) . . ? O1 As1 C1 110.8(3) . . ? O3 As1 C1 100.7(4) . . ? O8 As2 O7 119.2(3) . . ? O8 As2 O9 104.7(3) . . ? O7 As2 O9 106.3(3) . . ? O8 As2 C7 111.3(4) . . ? O7 As2 C7 112.9(4) . . ? O9 As2 C7 100.0(4) . . ? O5 S1 O6 114.9(4) . . ? O5 S1 O4 108.8(4) . . ? O6 S1 O4 113.8(4) . . ? O5 S1 C2 107.8(4) . . ? O6 S1 C2 106.5(5) . . ? O4 S1 C2 104.2(4) . . ? O12 S2 O11 113.7(4) . . ? O12 S2 O10 114.3(4) . . ? O11 S2 O10 110.5(4) . . ? O12 S2 C8 107.2(5) . . ? O11 S2 C8 107.5(4) . . ? O10 S2 C8 102.8(4) . . ? C13 N1 C17 116.6(8) . . ? C13 N1 Cd1 124.0(7) . . ? C17 N1 Cd1 119.4(6) . . ? C18 N2 C22 118.3(8) . . ? C18 N2 Cd1 117.9(6) . . ? C22 N2 Cd1 123.8(6) . . ? C23 N3 C27 118.1(9) . . ? C23 N3 Cd2 123.9(7) . . ? C27 N3 Cd2 118.0(7) . . ? C32 N4 C28 118.7(9) . . ? C32 N4 Cd2 123.7(7) . . ? C28 N4 Cd2 117.4(7) . . ? C2 C1 C6 119.2(9) . . ? C2 C1 As1 124.7(8) . . ? C6 C1 As1 116.0(7) . . ? C3 C2 C1 120.0(10) . . ? C3 C2 S1 119.3(8) . . ? C1 C2 S1 120.6(8) . . ? C4 C3 C2 121.0(11) . . ? C4 C3 H3B 119.5 . . ? C2 C3 H3B 119.5 . . ? C3 C4 C5 120.0(11) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 120.0(11) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C1 119.7(10) . . ? C5 C6 H6A 120.1 . . ? C1 C6 H6A 120.1 . . ? C12 C7 C8 119.8(9) . . ? C12 C7 As2 116.3(7) . . ? C8 C7 As2 123.8(8) . . ? C9 C8 C7 120.6(10) . . ? C9 C8 S2 117.8(8) . . ? C7 C8 S2 121.4(7) . . ? C8 C9 C10 119.3(11) . . ? C8 C9 H9B 120.3 . . ? C10 C9 H9B 120.3 . . ? C11 C10 C9 120.5(12) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 120.1(13) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C7 C12 C11 119.6(11) . . ? C7 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? N1 C13 C14 122.8(10) . . ? N1 C13 H13A 118.6 . . ? C14 C13 H13A 118.6 . . ? C15 C14 C13 120.3(11) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C16 C15 C14 117.6(11) . . ? C16 C15 H15A 121.2 . . ? C14 C15 H15A 121.2 . . ? C15 C16 C17 120.4(10) . . ? C15 C16 H16A 119.8 . . ? C17 C16 H16A 119.8 . . ? N1 C17 C16 122.3(9) . . ? N1 C17 C18 114.7(8) . . ? C16 C17 C18 123.0(9) . . ? N2 C18 C19 121.2(9) . . ? N2 C18 C17 118.1(8) . . ? C19 C18 C17 120.6(8) . . ? C20 C19 C18 119.0(9) . . ? C20 C19 H19A 120.5 . . ? C18 C19 H19A 120.5 . . ? C19 C20 C21 119.4(10) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C22 C21 C20 119.0(10) . . ? C22 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? N2 C22 C21 122.9(10) . . ? N2 C22 H22A 118.5 . . ? C21 C22 H22A 118.5 . . ? N3 C23 C24 124.9(10) . . ? N3 C23 H23A 117.5 . . ? C24 C23 H23A 117.5 . . ? C23 C24 C25 116.3(11) . . ? C23 C24 H24A 121.9 . . ? C25 C24 H24A 121.9 . . ? C26 C25 C24 120.5(10) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C27 119.3(11) . . ? C25 C26 H26A 120.3 . . ? C27 C26 H26A 120.3 . . ? N3 C27 C26 120.8(10) . . ? N3 C27 C28 117.4(9) . . ? C26 C27 C28 121.8(10) . . ? N4 C28 C29 120.5(10) . . ? N4 C28 C27 116.8(9) . . ? C29 C28 C27 122.6(10) . . ? C30 C29 C28 120.1(11) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C31 C30 C29 119.9(11) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 117.9(12) . . ? C30 C31 H31A 121.0 . . ? C32 C31 H31A 121.0 . . ? N4 C32 C31 122.8(11) . . ? N4 C32 H32A 118.6 . . ? C31 C32 H32A 118.6 . . ? As1 O1 Cd1 126.2(3) . . ? As1 O2 Cd2 130.5(3) . . ? As1 O3 H3A 109.5 . . ? S1 O4 Cd1 160.6(5) . . ? S1 O5 Cd2 105.8(4) . . ? As2 O7 Cd2 126.1(3) . . ? As2 O8 Cd1 130.4(3) . . ? As2 O9 H9A 109.5 . . ? S2 O10 Cd2 165.3(4) . . ? S2 O11 Cd1 106.8(4) . . ? 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 O3 H3A O7 0.82 1.77 2.553(9) 158.9 1_655 O9 H9A O1 0.82 1.80 2.591(8) 160.8 1_455 _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.773 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.183 #===end data_5 _database_code_depnum_ccdc_archive 'CCDC 763194' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 As2 N4 O14 S2 Zn2' _chemical_formula_weight 1087.34 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' 'S' 'S' 0.1246 0.1234 '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 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.161(6) _cell_length_b 14.429(4) _cell_length_c 14.001(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.449(4) _cell_angle_gamma 90.00 _cell_volume 3870.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5423 _cell_measurement_theta_min 3.1762 _cell_measurement_theta_max 27.4758 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 3.120 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.6307 _exptl_absorpt_correction_T_max 1 _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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14284 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4425 _reflns_number_gt 4101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0350P)^2^+2.1946P] 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 shelxtl _refine_ls_extinction_coef ? _refine_ls_number_reflns 4425 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0642 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.346889(12) 0.215201(17) -0.062657(16) 0.02174(7) Uani 1 1 d . . . As1 As 0.290049(10) 0.197203(13) 0.160187(13) 0.01792(7) Uani 1 1 d . . . S1 S 0.29623(3) 0.43232(3) 0.13748(3) 0.02119(11) Uani 1 1 d . . . N1 N 0.41448(9) 0.10386(13) -0.09598(12) 0.0249(4) Uani 1 1 d . . . N2 N 0.44047(9) 0.28663(12) -0.09407(12) 0.0241(4) Uani 1 1 d . . . C1 C 0.30562(10) 0.28373(14) 0.26306(14) 0.0214(4) Uani 1 1 d . . . C2 C 0.30748(10) 0.37972(15) 0.25130(14) 0.0232(4) Uani 1 1 d . . . C3 C 0.31912(13) 0.43688(17) 0.32973(16) 0.0357(5) Uani 1 1 d . . . H3A H 0.3214 0.5008 0.3218 0.043 Uiso 1 1 calc R . . C4 C 0.32723(15) 0.39851(19) 0.41962(17) 0.0453(6) Uani 1 1 d . . . H4A H 0.3351 0.4367 0.4721 0.054 Uiso 1 1 calc R . . C5 C 0.32370(16) 0.30502(19) 0.43164(17) 0.0449(7) Uani 1 1 d . . . H5A H 0.3283 0.2800 0.4926 0.054 Uiso 1 1 calc R . . C6 C 0.31334(12) 0.24651(17) 0.35404(15) 0.0315(5) Uani 1 1 d . . . H6A H 0.3116 0.1827 0.3629 0.038 Uiso 1 1 calc R . . C8 C 0.51549(13) 0.41590(19) -0.11882(18) 0.0416(6) Uani 1 1 d . . . H8A H 0.5213 0.4799 -0.1186 0.050 Uiso 1 1 calc R . . C9 C 0.56935(12) 0.35916(19) -0.14313(18) 0.0406(6) Uani 1 1 d . . . H9A H 0.6122 0.3843 -0.1601 0.049 Uiso 1 1 calc R . . C10 C 0.56017(11) 0.26298(18) -0.14247(15) 0.0303(5) Uani 1 1 d . . . C11 C 0.61388(12) 0.1971(2) -0.16306(18) 0.0406(6) Uani 1 1 d . . . H11A H 0.6579 0.2182 -0.1799 0.049 Uiso 1 1 calc R . . C12 C 0.60217(12) 0.1057(2) -0.15858(18) 0.0411(6) Uani 1 1 d . . . H12A H 0.6385 0.0649 -0.1710 0.049 Uiso 1 1 calc R . . C13 C 0.53461(11) 0.06927(17) -0.13498(16) 0.0323(5) Uani 1 1 d . . . C14 C 0.51926(13) -0.02540(19) -0.13082(18) 0.0403(6) Uani 1 1 d . . . H14A H 0.5540 -0.0691 -0.1418 0.048 Uiso 1 1 calc R . . C15 C 0.45276(14) -0.05306(18) -0.11051(18) 0.0406(6) Uani 1 1 d . . . H15A H 0.4417 -0.1158 -0.1079 0.049 Uiso 1 1 calc R . . C16 C 0.40147(12) 0.01390(16) -0.09376(16) 0.0336(5) Uani 1 1 d . . . H16A H 0.3563 -0.0057 -0.0805 0.040 Uiso 1 1 calc R . . C17 C 0.48042(10) 0.13168(16) -0.11598(14) 0.0238(4) Uani 1 1 d . . . C18 C 0.49363(10) 0.22961(16) -0.11743(14) 0.0246(4) Uani 1 1 d . . . C7 C 0.45132(12) 0.37667(17) -0.09425(16) 0.0330(5) Uani 1 1 d . . . H7A H 0.4149 0.4158 -0.0774 0.040 Uiso 1 1 calc R . . O1 O 0.31370(8) 0.09203(10) 0.20931(11) 0.0295(3) Uani 1 1 d . . . H1A H 0.2850 0.0768 0.2495 0.044 Uiso 1 1 calc R . . O2 O 0.20626(7) 0.18987(9) 0.13109(11) 0.0247(3) Uani 1 1 d . . . O3 O 0.34862(8) 0.21094(10) 0.07525(10) 0.0244(3) Uani 1 1 d . . . O4 O 0.27131(9) 0.52585(10) 0.15592(11) 0.0334(4) Uani 1 1 d . . . O5 O 0.24403(8) 0.37580(11) 0.08907(10) 0.0292(3) Uani 1 1 d . . . O6 O 0.36275(8) 0.43125(11) 0.09124(11) 0.0330(4) Uani 1 1 d . . . O1W O 0.48787(18) 0.2805(3) 0.1446(3) 0.1237(13) Uani 1 1 d . . . H1WA H 0.4554 0.3188 0.1315 0.186 Uiso 1 1 d R . . H1WB H 0.5228 0.2915 0.1093 0.186 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01753(12) 0.02758(14) 0.02014(12) 0.00221(9) 0.00250(9) 0.00231(9) As1 0.01775(11) 0.01855(12) 0.01746(11) -0.00018(7) 0.00088(8) 0.00134(7) S1 0.0234(2) 0.0190(2) 0.0212(2) -0.00071(19) 0.00103(18) -0.00255(18) N1 0.0219(8) 0.0305(10) 0.0224(8) -0.0007(7) 0.0002(7) 0.0021(7) N2 0.0197(9) 0.0303(10) 0.0222(8) 0.0020(7) 0.0029(7) 0.0009(7) C1 0.0196(9) 0.0270(11) 0.0175(9) -0.0023(8) -0.0007(7) 0.0017(8) C2 0.0233(10) 0.0258(11) 0.0204(9) -0.0031(8) -0.0008(8) -0.0011(8) C3 0.0474(14) 0.0296(13) 0.0299(12) -0.0075(10) -0.0064(10) 0.0010(10) C4 0.0657(18) 0.0456(16) 0.0243(11) -0.0122(11) -0.0117(11) 0.0019(13) C5 0.0643(19) 0.0531(17) 0.0171(11) 0.0015(10) -0.0087(11) 0.0017(13) C6 0.0388(13) 0.0322(13) 0.0236(10) 0.0027(9) -0.0035(9) 0.0014(10) C8 0.0406(14) 0.0386(15) 0.0455(14) 0.0027(12) 0.0019(11) -0.0118(11) C9 0.0276(12) 0.0555(17) 0.0388(13) -0.0001(12) 0.0034(10) -0.0172(11) C10 0.0188(10) 0.0492(15) 0.0231(10) -0.0036(10) 0.0010(8) -0.0050(9) C11 0.0177(11) 0.0665(19) 0.0378(13) -0.0112(12) 0.0055(10) -0.0030(10) C12 0.0214(11) 0.0601(18) 0.0417(13) -0.0138(13) 0.0024(10) 0.0113(11) C13 0.0264(11) 0.0436(14) 0.0268(11) -0.0080(10) -0.0023(9) 0.0087(10) C14 0.0384(13) 0.0442(15) 0.0384(13) -0.0102(11) -0.0050(11) 0.0158(11) C15 0.0446(14) 0.0323(14) 0.0447(14) -0.0063(11) -0.0040(12) 0.0062(11) C16 0.0302(11) 0.0343(13) 0.0363(12) -0.0018(10) -0.0015(10) 0.0008(9) C17 0.0192(9) 0.0348(12) 0.0176(9) -0.0025(8) -0.0003(7) 0.0038(8) C18 0.0197(10) 0.0385(13) 0.0157(9) -0.0007(8) 0.0005(8) -0.0004(9) C7 0.0311(12) 0.0333(13) 0.0347(12) 0.0009(10) 0.0023(9) 0.0002(9) O1 0.0293(8) 0.0235(8) 0.0356(8) 0.0068(7) 0.0043(6) 0.0061(6) O2 0.0191(7) 0.0233(8) 0.0315(8) 0.0026(6) -0.0033(6) -0.0012(5) O3 0.0211(7) 0.0338(8) 0.0183(7) -0.0011(6) 0.0028(6) 0.0000(6) O4 0.0472(10) 0.0202(8) 0.0328(8) 0.0004(6) 0.0043(7) 0.0048(7) O5 0.0308(8) 0.0290(8) 0.0277(8) 0.0016(6) -0.0058(6) -0.0085(6) O6 0.0292(8) 0.0355(9) 0.0343(8) 0.0025(7) 0.0084(7) -0.0050(7) O1W 0.086(2) 0.172(4) 0.113(3) 0.002(2) -0.022(2) 0.000(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 1.9317(15) . ? Zn1 O2 1.9534(15) 7 ? Zn1 N2 2.1174(18) . ? Zn1 N1 2.1179(18) . ? Zn1 O5 2.2104(15) 7 ? As1 O3 1.6535(14) . ? As1 O2 1.6568(15) . ? As1 O1 1.7252(15) . ? As1 C1 1.927(2) . ? S1 O6 1.4343(16) . ? S1 O5 1.4540(15) . ? S1 O4 1.4553(16) . ? S1 C2 1.777(2) . ? N1 C16 1.322(3) . ? N1 C17 1.357(3) . ? N2 C7 1.316(3) . ? N2 C18 1.352(3) . ? C1 C6 1.389(3) . ? C1 C2 1.395(3) . ? C2 C3 1.390(3) . ? C3 C4 1.383(3) . ? C3 H3A 0.9300 . ? C4 C5 1.361(4) . ? C4 H4A 0.9300 . ? C5 C6 1.389(3) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C8 C9 1.363(4) . ? C8 C7 1.399(3) . ? C8 H8A 0.9300 . ? C9 C10 1.399(4) . ? C9 H9A 0.9300 . ? C10 C18 1.410(3) . ? C10 C11 1.432(3) . ? C11 C12 1.339(4) . ? C11 H11A 0.9300 . ? C12 C13 1.438(3) . ? C12 H12A 0.9300 . ? C13 C14 1.399(4) . ? C13 C17 1.402(3) . ? C14 C15 1.367(4) . ? C14 H14A 0.9300 . ? C15 C16 1.399(3) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 C18 1.436(3) . ? C7 H7A 0.9300 . ? O1 H1A 0.8200 . ? O2 Zn1 1.9534(15) 7 ? O5 Zn1 2.2104(15) 7 ? O1W H1WA 0.8499 . ? O1W H1WB 0.8501 . ? 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 O2 121.15(6) . 7 ? O3 Zn1 N2 102.42(6) . . ? O2 Zn1 N2 89.77(7) 7 . ? O3 Zn1 N1 100.97(6) . . ? O2 Zn1 N1 137.83(6) 7 . ? N2 Zn1 N1 78.64(7) . . ? O3 Zn1 O5 98.95(6) . 7 ? O2 Zn1 O5 85.83(6) 7 7 ? N2 Zn1 O5 157.23(6) . 7 ? N1 Zn1 O5 89.72(7) . 7 ? O3 As1 O2 119.52(8) . . ? O3 As1 O1 102.39(7) . . ? O2 As1 O1 107.03(7) . . ? O3 As1 C1 110.97(8) . . ? O2 As1 C1 111.66(8) . . ? O1 As1 C1 103.48(8) . . ? O6 S1 O5 113.21(10) . . ? O6 S1 O4 112.59(10) . . ? O5 S1 O4 112.18(10) . . ? O6 S1 C2 107.35(10) . . ? O5 S1 C2 104.87(9) . . ? O4 S1 C2 105.94(9) . . ? C16 N1 C17 118.12(19) . . ? C16 N1 Zn1 128.59(15) . . ? C17 N1 Zn1 113.15(14) . . ? C7 N2 C18 118.76(19) . . ? C7 N2 Zn1 127.96(15) . . ? C18 N2 Zn1 113.27(14) . . ? C6 C1 C2 119.30(19) . . ? C6 C1 As1 116.71(16) . . ? C2 C1 As1 123.97(15) . . ? C3 C2 C1 120.0(2) . . ? C3 C2 S1 118.21(17) . . ? C1 C2 S1 121.80(15) . . ? C4 C3 C2 119.8(2) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C5 C4 C3 120.3(2) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 120.8(2) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C1 C6 C5 119.7(2) . . ? C1 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C9 C8 C7 119.2(2) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C8 C9 C10 119.9(2) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C9 C10 C18 117.0(2) . . ? C9 C10 C11 124.5(2) . . ? C18 C10 C11 118.4(2) . . ? C12 C11 C10 121.6(2) . . ? C12 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C11 C12 C13 121.5(2) . . ? C11 C12 H12A 119.3 . . ? C13 C12 H12A 119.3 . . ? C14 C13 C17 117.6(2) . . ? C14 C13 C12 123.8(2) . . ? C17 C13 C12 118.6(2) . . ? C15 C14 C13 119.4(2) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C14 C15 C16 119.4(2) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? N1 C16 C15 122.8(2) . . ? N1 C16 H16A 118.6 . . ? C15 C16 H16A 118.6 . . ? N1 C17 C13 122.8(2) . . ? N1 C17 C18 117.30(18) . . ? C13 C17 C18 119.91(19) . . ? N2 C18 C10 122.5(2) . . ? N2 C18 C17 117.54(18) . . ? C10 C18 C17 120.0(2) . . ? N2 C7 C8 122.6(2) . . ? N2 C7 H7A 118.7 . . ? C8 C7 H7A 118.7 . . ? As1 O1 H1A 109.5 . . ? As1 O2 Zn1 125.19(8) . 7 ? As1 O3 Zn1 135.74(9) . . ? S1 O5 Zn1 161.72(10) . 7 ? H1WA O1W H1WB 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O4 0.82 1.87 2.678(2) 170.9 4_545 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.418 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.074 #===end data_6 _database_code_depnum_ccdc_archive 'CCDC 763196' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H56 As4 Cd4 N8 O26 S4' _chemical_formula_weight 2326.77 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' 'S' 'S' 0.1246 0.1234 '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' 'Cd' 'Cd' -0.8075 1.2024 '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 8.003(3) _cell_length_b 11.771(4) _cell_length_c 21.224(9) _cell_angle_alpha 81.526(9) _cell_angle_beta 81.531(9) _cell_angle_gamma 75.679(10) _cell_volume 1903.2(12) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4075 _cell_measurement_theta_min 3.1011 _cell_measurement_theta_max 27.4835 _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.030 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 3.026 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.1775 _exptl_absorpt_correction_T_max 1 _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15071 _diffrn_reflns_av_R_equivalents 0.0887 _diffrn_reflns_av_sigmaI/netI 0.1550 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8603 _reflns_number_gt 4553 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0583P)^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 shelxtl _refine_ls_extinction_coef ? _refine_ls_number_reflns 8603 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1334 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.59790(8) 0.35958(5) -0.02943(3) 0.02799(16) Uani 1 1 d . . . Cd2 Cd 0.37593(8) 0.16523(5) 0.46826(3) 0.03110(17) Uani 1 1 d . . . As1 As 0.19780(11) 0.52505(7) -0.07473(4) 0.0257(2) Uani 1 1 d . . . As2 As 0.80991(11) 0.03981(7) 0.42755(4) 0.0253(2) Uani 1 1 d . . . S1 S 0.5032(3) 0.38500(19) -0.19170(10) 0.0344(5) Uani 1 1 d . . . S2 S 0.4819(3) -0.02960(19) 0.36581(10) 0.0315(5) Uani 1 1 d . . . N1 N 0.5033(9) 0.2469(6) 0.0646(3) 0.0346(17) Uani 1 1 d . . . N2 N 0.7282(9) 0.1636(6) -0.0362(3) 0.0332(16) Uani 1 1 d . . . N3 N 0.3390(10) 0.3387(7) 0.5171(4) 0.046(2) Uani 1 1 d . . . N4 N 0.2105(10) 0.3251(6) 0.4071(4) 0.0426(19) Uani 1 1 d . . . C1 C 0.2620(12) 0.5939(7) -0.1609(4) 0.034(2) Uani 1 1 d . . . C2 C 0.3937(11) 0.5352(7) -0.2049(4) 0.0276(18) Uani 1 1 d . . . C3 C 0.4359(14) 0.5978(8) -0.2626(4) 0.044(2) Uani 1 1 d . . . H3A H 0.5249 0.5608 -0.2913 0.053 Uiso 1 1 calc R . . C4 C 0.3530(17) 0.7115(10) -0.2794(5) 0.066(3) Uani 1 1 d . . . H4A H 0.3839 0.7509 -0.3191 0.079 Uiso 1 1 calc R . . C5 C 0.2210(18) 0.7682(9) -0.2364(6) 0.071(4) Uani 1 1 d . . . H5A H 0.1640 0.8463 -0.2468 0.085 Uiso 1 1 calc R . . C6 C 0.1753(14) 0.7074(8) -0.1780(5) 0.050(3) Uani 1 1 d . . . H6A H 0.0843 0.7443 -0.1500 0.060 Uiso 1 1 calc R . . C7 C 0.8338(10) -0.0314(6) 0.3498(3) 0.0225(16) Uani 1 1 d . . . C8 C 0.6974(10) -0.0648(7) 0.3272(4) 0.0263(17) Uani 1 1 d . . . C9 C 0.7324(12) -0.1295(8) 0.2757(4) 0.037(2) Uani 1 1 d . . . H9A H 0.6434 -0.1529 0.2613 0.044 Uiso 1 1 calc R . . C10 C 0.9010(14) -0.1596(9) 0.2454(4) 0.050(3) Uani 1 1 d . . . H10A H 0.9240 -0.2031 0.2107 0.059 Uiso 1 1 calc R . . C11 C 1.0332(13) -0.1259(8) 0.2662(5) 0.047(2) Uani 1 1 d . . . H11A H 1.1450 -0.1456 0.2450 0.056 Uiso 1 1 calc R . . C12 C 1.0020(11) -0.0634(7) 0.3178(4) 0.0326(19) Uani 1 1 d . . . H12A H 1.0933 -0.0419 0.3318 0.039 Uiso 1 1 calc R . . C13 C 0.3977(14) 0.2901(9) 0.1136(5) 0.052(3) Uani 1 1 d . . . H13A H 0.3503 0.3709 0.1117 0.062 Uiso 1 1 calc R . . C14 C 0.3556(15) 0.2154(11) 0.1691(5) 0.063(3) Uani 1 1 d . . . H14A H 0.2862 0.2478 0.2042 0.076 Uiso 1 1 calc R . . C15 C 0.4148(15) 0.0986(10) 0.1715(5) 0.058(3) Uani 1 1 d . . . H15A H 0.3829 0.0496 0.2074 0.070 Uiso 1 1 calc R . . C16 C 0.5253(13) 0.0496(8) 0.1197(5) 0.039(2) Uani 1 1 d . . . C17 C 0.5914(14) -0.0752(8) 0.1167(5) 0.050(3) Uani 1 1 d . . . H17A H 0.5597 -0.1280 0.1508 0.060 Uiso 1 1 calc R . . C18 C 0.6991(15) -0.1179(8) 0.0653(5) 0.053(3) Uani 1 1 d . . . H18A H 0.7407 -0.1989 0.0648 0.064 Uiso 1 1 calc R . . C19 C 0.7485(13) -0.0378(8) 0.0119(5) 0.042(2) Uani 1 1 d . . . C20 C 0.8587(14) -0.0762(8) -0.0419(5) 0.055(3) Uani 1 1 d . . . H20A H 0.9020 -0.1566 -0.0443 0.066 Uiso 1 1 calc R . . C21 C 0.9038(13) 0.0038(8) -0.0914(5) 0.052(3) Uani 1 1 d . . . H21A H 0.9785 -0.0210 -0.1272 0.062 Uiso 1 1 calc R . . C22 C 0.8352(12) 0.1212(8) -0.0863(4) 0.042(2) Uani 1 1 d . . . H22A H 0.8650 0.1753 -0.1200 0.051 Uiso 1 1 calc R . . C23 C 0.6840(12) 0.0839(7) 0.0123(4) 0.033(2) Uani 1 1 d . . . C24 C 0.5696(11) 0.1292(7) 0.0667(4) 0.033(2) Uani 1 1 d . . . C25 C 0.3997(14) 0.3449(9) 0.5710(5) 0.054(3) Uani 1 1 d . . . H25A H 0.4561 0.2755 0.5935 0.064 Uiso 1 1 calc R . . C26 C 0.3818(15) 0.4524(10) 0.5953(6) 0.061(3) Uani 1 1 d . . . H26A H 0.4231 0.4531 0.6340 0.074 Uiso 1 1 calc R . . C27 C 0.3060(16) 0.5536(10) 0.5633(6) 0.070(4) Uani 1 1 d . . . H27A H 0.2967 0.6248 0.5790 0.084 Uiso 1 1 calc R . . C28 C 0.2390(14) 0.5524(8) 0.5047(6) 0.055(3) Uani 1 1 d . . . C29 C 0.1534(16) 0.6562(9) 0.4692(7) 0.069(4) Uani 1 1 d . . . H29A H 0.1389 0.7293 0.4836 0.083 Uiso 1 1 calc R . . C30 C 0.0932(17) 0.6486(9) 0.4145(7) 0.076(4) Uani 1 1 d . . . H30A H 0.0396 0.7180 0.3912 0.092 Uiso 1 1 calc R . . C31 C 0.1076(14) 0.5391(8) 0.3903(6) 0.053(3) Uani 1 1 d . . . C32 C 0.0451(15) 0.5275(10) 0.3338(6) 0.065(3) Uani 1 1 d . . . H32A H -0.0057 0.5942 0.3079 0.078 Uiso 1 1 calc R . . C33 C 0.0592(14) 0.4188(10) 0.3171(5) 0.058(3) Uani 1 1 d . . . H33A H 0.0141 0.4099 0.2807 0.069 Uiso 1 1 calc R . . C34 C 0.1423(13) 0.3199(9) 0.3553(5) 0.050(3) Uani 1 1 d . . . H34A H 0.1496 0.2458 0.3433 0.060 Uiso 1 1 calc R . . C35 C 0.1925(12) 0.4324(8) 0.4260(5) 0.039(2) Uani 1 1 d . . . C36 C 0.2610(11) 0.4399(7) 0.4839(5) 0.037(2) Uani 1 1 d . . . O1 O 0.3563(7) 0.5060(5) -0.0287(3) 0.0297(13) Uani 1 1 d . . . O2 O 0.0468(8) 0.6457(5) -0.0490(3) 0.0417(16) Uani 1 1 d . . . H2A H 0.0003 0.6274 -0.0131 0.063 Uiso 1 1 calc R . . O3 O 0.1020(7) 0.4135(5) -0.0660(3) 0.0330(13) Uani 1 1 d . . . O4 O 0.4271(11) 0.3228(6) -0.2286(3) 0.064(2) Uani 1 1 d . . . O5 O 0.6861(9) 0.3814(6) -0.2125(3) 0.0543(18) Uani 1 1 d . . . O6 O 0.4684(8) 0.3531(5) -0.1224(3) 0.0354(14) Uani 1 1 d . . . O7 O 0.8266(7) -0.0686(5) 0.4895(2) 0.0285(13) Uani 1 1 d . . . O8 O 0.9976(8) 0.0905(5) 0.4163(3) 0.0383(15) Uani 1 1 d . . . H8B H 1.0405 0.0782 0.4502 0.057 Uiso 1 1 calc R . . O9 O 0.6498(7) 0.1581(5) 0.4348(3) 0.0313(13) Uani 1 1 d . . . O10 O 0.3926(8) -0.1059(6) 0.3450(3) 0.0489(18) Uani 1 1 d . . . O11 O 0.5043(8) -0.0518(6) 0.4345(3) 0.0398(15) Uani 1 1 d . . . O12 O 0.4137(8) 0.0951(5) 0.3486(3) 0.0465(17) Uani 1 1 d . . . O1W O 0.8020(8) 0.4192(6) -0.1064(3) 0.0449(16) Uani 1 1 d . . . H1WA H 0.8827 0.4317 -0.0883 0.067 Uiso 1 1 d R . . H1WB H 0.8440 0.3652 -0.1307 0.067 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0307(4) 0.0266(3) 0.0250(3) -0.0023(2) 0.0007(3) -0.0063(3) Cd2 0.0307(4) 0.0277(3) 0.0337(4) -0.0007(2) 0.0047(3) -0.0110(3) As1 0.0259(5) 0.0265(4) 0.0231(4) 0.0015(3) 0.0004(3) -0.0076(3) As2 0.0260(5) 0.0329(4) 0.0192(4) 0.0003(3) -0.0008(3) -0.0139(4) S1 0.0443(15) 0.0359(12) 0.0239(11) -0.0080(9) -0.0025(10) -0.0091(10) S2 0.0218(12) 0.0425(12) 0.0322(12) -0.0108(9) 0.0000(9) -0.0091(9) N1 0.037(5) 0.034(4) 0.031(4) -0.007(3) 0.010(3) -0.013(3) N2 0.027(4) 0.035(4) 0.034(4) -0.004(3) 0.001(3) -0.004(3) N3 0.046(5) 0.041(5) 0.051(5) -0.010(4) 0.017(4) -0.023(4) N4 0.046(5) 0.031(4) 0.047(5) -0.003(3) 0.006(4) -0.009(4) C1 0.036(5) 0.025(4) 0.039(5) 0.008(4) 0.001(4) -0.014(4) C2 0.028(5) 0.036(5) 0.023(4) -0.004(3) -0.003(3) -0.014(4) C3 0.061(7) 0.047(6) 0.026(5) 0.003(4) -0.001(5) -0.020(5) C4 0.090(10) 0.067(8) 0.036(6) 0.018(5) -0.001(6) -0.028(7) C5 0.094(11) 0.043(6) 0.060(8) 0.024(5) -0.002(7) -0.007(6) C6 0.053(7) 0.044(6) 0.037(6) 0.011(4) 0.012(5) -0.001(5) C7 0.016(4) 0.029(4) 0.020(4) 0.003(3) 0.000(3) -0.005(3) C8 0.022(5) 0.036(4) 0.020(4) -0.005(3) 0.001(3) -0.005(3) C9 0.043(6) 0.044(5) 0.026(5) -0.002(4) -0.002(4) -0.018(4) C10 0.054(7) 0.065(7) 0.031(5) -0.020(5) 0.010(5) -0.016(5) C11 0.039(6) 0.054(6) 0.035(6) -0.004(4) 0.012(4) 0.001(5) C12 0.022(5) 0.040(5) 0.033(5) 0.001(4) 0.000(4) -0.007(4) C13 0.058(7) 0.046(6) 0.046(6) -0.008(5) 0.007(5) -0.010(5) C14 0.064(8) 0.078(8) 0.041(7) -0.009(6) 0.024(5) -0.020(7) C15 0.075(9) 0.061(7) 0.041(6) 0.008(5) 0.010(6) -0.036(6) C16 0.047(6) 0.036(5) 0.038(5) 0.005(4) -0.008(5) -0.017(4) C17 0.060(8) 0.039(5) 0.050(7) 0.021(4) -0.019(6) -0.017(5) C18 0.080(9) 0.032(5) 0.053(7) 0.009(4) -0.025(6) -0.021(5) C19 0.053(7) 0.032(5) 0.042(6) -0.005(4) -0.014(5) -0.006(4) C20 0.069(8) 0.027(5) 0.064(7) -0.016(5) -0.007(6) 0.003(5) C21 0.053(7) 0.036(5) 0.060(7) -0.015(5) 0.002(6) 0.003(5) C22 0.045(6) 0.036(5) 0.039(6) -0.005(4) 0.012(5) -0.006(4) C23 0.040(6) 0.031(4) 0.032(5) -0.005(4) -0.012(4) -0.010(4) C24 0.036(5) 0.027(4) 0.034(5) 0.002(3) -0.008(4) -0.007(4) C25 0.054(7) 0.054(6) 0.060(7) -0.009(5) 0.010(6) -0.034(5) C26 0.062(8) 0.054(7) 0.072(9) -0.022(6) 0.011(6) -0.023(6) C27 0.076(9) 0.058(8) 0.086(10) -0.032(7) 0.032(7) -0.043(7) C28 0.046(7) 0.032(5) 0.083(9) -0.020(5) 0.026(6) -0.014(5) C29 0.063(9) 0.038(6) 0.093(10) -0.009(6) 0.036(7) -0.014(6) C30 0.073(9) 0.030(6) 0.098(11) 0.012(6) 0.039(8) 0.002(5) C31 0.040(6) 0.032(5) 0.067(8) 0.011(5) 0.019(5) 0.003(4) C32 0.051(8) 0.057(7) 0.067(9) 0.016(6) 0.010(6) 0.001(6) C33 0.052(7) 0.060(7) 0.049(7) 0.020(5) 0.000(6) -0.010(6) C34 0.049(7) 0.051(6) 0.043(6) -0.001(5) 0.007(5) -0.010(5) C35 0.033(6) 0.035(5) 0.041(6) 0.001(4) 0.012(4) -0.004(4) C36 0.030(5) 0.022(4) 0.054(6) -0.005(4) 0.023(4) -0.010(4) O1 0.022(3) 0.036(3) 0.032(3) -0.006(2) -0.001(3) -0.007(2) O2 0.050(4) 0.027(3) 0.038(4) 0.007(3) -0.004(3) 0.003(3) O3 0.027(3) 0.042(3) 0.032(3) -0.005(3) 0.005(3) -0.019(3) O4 0.105(7) 0.047(4) 0.052(5) -0.019(3) -0.017(4) -0.032(4) O5 0.034(4) 0.083(5) 0.035(4) -0.009(3) 0.018(3) -0.004(4) O6 0.042(4) 0.039(3) 0.023(3) 0.002(2) -0.001(3) -0.010(3) O7 0.028(3) 0.036(3) 0.026(3) 0.001(2) -0.006(2) -0.015(3) O8 0.036(4) 0.058(4) 0.030(3) 0.009(3) -0.007(3) -0.034(3) O9 0.025(3) 0.036(3) 0.031(3) 0.000(2) 0.002(3) -0.009(3) O10 0.033(4) 0.063(4) 0.060(5) -0.033(4) 0.002(3) -0.019(3) O11 0.028(4) 0.073(4) 0.022(3) -0.005(3) 0.011(3) -0.026(3) O12 0.035(4) 0.044(4) 0.057(5) -0.008(3) -0.011(3) 0.001(3) O1W 0.034(4) 0.067(4) 0.039(4) -0.007(3) 0.008(3) -0.027(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.250(5) . ? Cd1 O1 2.270(5) 2_665 ? Cd1 O1W 2.296(6) . ? Cd1 N2 2.301(7) . ? Cd1 N1 2.364(7) . ? Cd1 O6 2.379(5) . ? Cd2 O9 2.187(6) . ? Cd2 O7 2.216(5) 2_656 ? Cd2 N4 2.353(8) . ? Cd2 N3 2.359(7) . ? Cd2 O11 2.469(6) 2_656 ? Cd2 O11 2.668(6) . ? Cd2 O12 2.737(6) . ? As1 O3 1.653(5) . ? As1 O1 1.665(5) . ? As1 O2 1.721(6) . ? As1 C1 1.939(9) . ? As2 O9 1.651(6) . ? As2 O7 1.687(5) . ? As2 O8 1.722(5) . ? As2 C7 1.923(7) . ? S1 O4 1.432(6) . ? S1 O5 1.457(7) . ? S1 O6 1.467(6) . ? S1 C2 1.769(8) . ? S2 O10 1.429(6) . ? S2 O12 1.446(6) . ? S2 O11 1.473(6) . ? S2 C8 1.774(8) . ? N1 C13 1.319(12) . ? N1 C24 1.352(10) . ? N2 C22 1.337(11) . ? N2 C23 1.356(11) . ? N3 C25 1.325(12) . ? N3 C36 1.349(12) . ? N4 C34 1.313(11) . ? N4 C35 1.349(10) . ? C1 C6 1.367(12) . ? C1 C2 1.414(11) . ? C2 C3 1.376(12) . ? C3 C4 1.360(14) . ? C3 H3A 0.9300 . ? C4 C5 1.394(16) . ? C4 H4A 0.9300 . ? C5 C6 1.384(14) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.404(11) . ? C7 C8 1.414(10) . ? C8 C9 1.378(10) . ? C9 C10 1.391(13) . ? C9 H9A 0.9300 . ? C10 C11 1.366(13) . ? C10 H10A 0.9300 . ? C11 C12 1.368(11) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.414(15) . ? C13 H13A 0.9300 . ? C14 C15 1.335(14) . ? C14 H14A 0.9300 . ? C15 C16 1.403(14) . ? C15 H15A 0.9300 . ? C16 C24 1.415(12) . ? C16 C17 1.440(12) . ? C17 C18 1.363(15) . ? C17 H17A 0.9300 . ? C18 C19 1.438(14) . ? C18 H18A 0.9300 . ? C19 C20 1.393(14) . ? C19 C23 1.398(11) . ? C20 C21 1.373(15) . ? C20 H20A 0.9300 . ? C21 C22 1.369(11) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.444(12) . ? C25 C26 1.404(13) . ? C25 H25A 0.9300 . ? C26 C27 1.332(17) . ? C26 H26A 0.9300 . ? C27 C28 1.427(16) . ? C27 H27A 0.9300 . ? C28 C29 1.413(16) . ? C28 C36 1.419(11) . ? C29 C30 1.344(17) . ? C29 H29A 0.9300 . ? C30 C31 1.429(15) . ? C30 H30A 0.9300 . ? C31 C32 1.402(15) . ? C31 C35 1.436(13) . ? C32 C33 1.351(14) . ? C32 H32A 0.9300 . ? C33 C34 1.397(14) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.440(13) . ? O1 Cd1 2.270(5) 2_665 ? O2 H2A 0.8200 . ? O7 Cd2 2.216(5) 2_656 ? O8 H8B 0.8200 . ? O11 Cd2 2.469(6) 2_656 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8501 . ? 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 Cd1 O1 74.1(2) . 2_665 ? O1 Cd1 O1W 107.6(2) . . ? O1 Cd1 O1W 86.1(2) 2_665 . ? O1 Cd1 N2 149.2(2) . . ? O1 Cd1 N2 132.3(2) 2_665 . ? O1W Cd1 N2 91.9(2) . . ? O1 Cd1 N1 95.9(2) . . ? O1 Cd1 N1 91.5(2) 2_665 . ? O1W Cd1 N1 154.7(2) . . ? N2 Cd1 N1 71.3(2) . . ? O1 Cd1 O6 73.79(19) . . ? O1 Cd1 O6 139.66(19) 2_665 . ? O1W Cd1 O6 81.0(2) . . ? N2 Cd1 O6 86.4(2) . . ? N1 Cd1 O6 115.5(2) . . ? O9 Cd2 O7 148.0(2) . 2_656 ? O9 Cd2 N4 107.6(2) . . ? O7 Cd2 N4 100.4(2) 2_656 . ? O9 Cd2 N3 93.3(2) . . ? O7 Cd2 N3 110.6(2) 2_656 . ? N4 Cd2 N3 70.7(3) . . ? O9 Cd2 O11 82.7(2) . 2_656 ? O7 Cd2 O11 77.39(18) 2_656 2_656 ? N4 Cd2 O11 156.7(2) . 2_656 ? N3 Cd2 O11 88.2(3) . 2_656 ? O9 Cd2 O11 75.05(18) . . ? O7 Cd2 O11 76.08(19) 2_656 . ? N4 Cd2 O11 126.0(2) . . ? N3 Cd2 O11 161.6(2) . . ? O11 Cd2 O11 76.39(19) 2_656 . ? O9 Cd2 O12 77.00(19) . . ? O7 Cd2 O12 95.89(19) 2_656 . ? N4 Cd2 O12 75.2(2) . . ? N3 Cd2 O12 139.7(2) . . ? O11 Cd2 O12 128.01(19) 2_656 . ? O11 Cd2 O12 52.33(18) . . ? O3 As1 O1 114.4(3) . . ? O3 As1 O2 107.9(3) . . ? O1 As1 O2 103.9(3) . . ? O3 As1 C1 118.3(3) . . ? O1 As1 C1 111.5(3) . . ? O2 As1 C1 98.3(3) . . ? O9 As2 O7 117.8(3) . . ? O9 As2 O8 105.5(3) . . ? O7 As2 O8 107.7(3) . . ? O9 As2 C7 115.7(3) . . ? O7 As2 C7 108.1(3) . . ? O8 As2 C7 100.3(3) . . ? O4 S1 O5 114.1(4) . . ? O4 S1 O6 112.8(4) . . ? O5 S1 O6 112.7(4) . . ? O4 S1 C2 106.0(4) . . ? O5 S1 C2 105.8(4) . . ? O6 S1 C2 104.5(4) . . ? O10 S2 O12 115.2(4) . . ? O10 S2 O11 114.5(4) . . ? O12 S2 O11 109.5(4) . . ? O10 S2 C8 106.0(4) . . ? O12 S2 C8 107.0(4) . . ? O11 S2 C8 103.7(3) . . ? C13 N1 C24 119.7(8) . . ? C13 N1 Cd1 125.3(6) . . ? C24 N1 Cd1 114.9(5) . . ? C22 N2 C23 117.2(7) . . ? C22 N2 Cd1 125.1(6) . . ? C23 N2 Cd1 117.5(6) . . ? C25 N3 C36 118.5(8) . . ? C25 N3 Cd2 125.4(7) . . ? C36 N3 Cd2 115.9(6) . . ? C34 N4 C35 117.8(8) . . ? C34 N4 Cd2 126.2(6) . . ? C35 N4 Cd2 115.9(6) . . ? C6 C1 C2 119.7(8) . . ? C6 C1 As1 116.4(7) . . ? C2 C1 As1 123.9(6) . . ? C3 C2 C1 117.9(8) . . ? C3 C2 S1 117.7(7) . . ? C1 C2 S1 124.4(6) . . ? C4 C3 C2 122.8(10) . . ? C4 C3 H3A 118.6 . . ? C2 C3 H3A 118.6 . . ? C3 C4 C5 119.0(10) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? C6 C5 C4 119.5(10) . . ? C6 C5 H5A 120.2 . . ? C4 C5 H5A 120.2 . . ? C1 C6 C5 121.0(10) . . ? C1 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? C12 C7 C8 118.4(7) . . ? C12 C7 As2 117.0(5) . . ? C8 C7 As2 124.2(6) . . ? C9 C8 C7 119.8(8) . . ? C9 C8 S2 119.1(6) . . ? C7 C8 S2 121.1(6) . . ? C8 C9 C10 120.0(8) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 120.7(8) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C12 120.4(9) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C7 120.7(8) . . ? C11 C12 H12A 119.6 . . ? C7 C12 H12A 119.6 . . ? N1 C13 C14 120.9(10) . . ? N1 C13 H13A 119.5 . . ? C14 C13 H13A 119.5 . . ? C15 C14 C13 120.4(10) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 120.0(9) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C15 C16 C24 117.1(8) . . ? C15 C16 C17 124.2(9) . . ? C24 C16 C17 118.7(9) . . ? C18 C17 C16 121.7(9) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C17 C18 C19 120.1(9) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C20 C19 C23 117.4(9) . . ? C20 C19 C18 122.7(9) . . ? C23 C19 C18 119.9(9) . . ? C21 C20 C19 120.5(9) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C22 C21 C20 117.8(10) . . ? C22 C21 H21A 121.1 . . ? C20 C21 H21A 121.1 . . ? N2 C22 C21 124.5(9) . . ? N2 C22 H22A 117.7 . . ? C21 C22 H22A 117.7 . . ? N2 C23 C19 122.5(8) . . ? N2 C23 C24 117.4(7) . . ? C19 C23 C24 120.1(8) . . ? N1 C24 C16 121.8(8) . . ? N1 C24 C23 118.7(8) . . ? C16 C24 C23 119.5(8) . . ? N3 C25 C26 122.3(11) . . ? N3 C25 H25A 118.8 . . ? C26 C25 H25A 118.8 . . ? C27 C26 C25 120.3(12) . . ? C27 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C26 C27 C28 119.9(10) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C29 C28 C36 121.1(11) . . ? C29 C28 C27 122.7(10) . . ? C36 C28 C27 116.2(10) . . ? C30 C29 C28 119.6(11) . . ? C30 C29 H29A 120.2 . . ? C28 C29 H29A 120.2 . . ? C29 C30 C31 123.2(12) . . ? C29 C30 H30A 118.4 . . ? C31 C30 H30A 118.4 . . ? C32 C31 C30 124.8(11) . . ? C32 C31 C35 117.0(9) . . ? C30 C31 C35 118.2(11) . . ? C33 C32 C31 119.6(10) . . ? C33 C32 H32A 120.2 . . ? C31 C32 H32A 120.2 . . ? C32 C33 C34 119.3(11) . . ? C32 C33 H33A 120.4 . . ? C34 C33 H33A 120.4 . . ? N4 C34 C33 124.0(10) . . ? N4 C34 H34A 118.0 . . ? C33 C34 H34A 118.0 . . ? N4 C35 C31 122.2(9) . . ? N4 C35 C36 118.8(8) . . ? C31 C35 C36 119.1(9) . . ? N3 C36 C28 122.8(10) . . ? N3 C36 C35 118.2(8) . . ? C28 C36 C35 118.9(9) . . ? As1 O1 Cd1 126.0(3) . . ? As1 O1 Cd1 126.8(3) . 2_665 ? Cd1 O1 Cd1 105.9(2) . 2_665 ? As1 O2 H2A 109.5 . . ? S1 O6 Cd1 136.6(4) . . ? As2 O7 Cd2 126.1(3) . 2_656 ? As2 O8 H8B 109.5 . . ? As2 O9 Cd2 127.9(3) . . ? S2 O11 Cd2 155.2(4) . 2_656 ? S2 O11 Cd2 100.2(3) . . ? Cd2 O11 Cd2 103.61(19) 2_656 . ? S2 O12 Cd2 97.9(3) . . ? Cd1 O1W H1WA 109.3 . . ? Cd1 O1W H1WB 109.2 . . ? H1WA O1W H1WB 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2A O3 0.82 1.81 2.630(9) 179.8 2_565 O8 H8B O7 0.82 1.76 2.557(7) 165.2 2_756 O1W H1WA O3 0.85 1.84 2.648(8) 158.6 1_655 O1W H1WB O5 0.85 2.25 2.691(9) 112.1 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.726 _refine_diff_density_min -2.262 _refine_diff_density_rms 0.208 #===end data_7 _database_code_depnum_ccdc_archive 'CCDC 763197' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H34 As2 Cd2 N4 O14 S2' _chemical_formula_weight 1185.43 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' 'S' 'S' 0.1246 0.1234 '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' 'Cd' 'Cd' -0.8075 1.2024 '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 8.631(7) _cell_length_b 11.609(7) _cell_length_c 11.754(7) _cell_angle_alpha 60.83(3) _cell_angle_beta 73.29(4) _cell_angle_gamma 75.08(4) _cell_volume 975.3(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2534 _cell_measurement_theta_min 3.4252 _cell_measurement_theta_max 27.4680 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 2.956 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.1759 _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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7555 _diffrn_reflns_av_R_equivalents 0.1117 _diffrn_reflns_av_sigmaI/netI 0.1706 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4159 _reflns_number_gt 2652 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0506P)^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 SHELXL _refine_ls_extinction_coef 0.0050(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4159 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.1742 _refine_ls_wR_factor_gt 0.1591 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.66021(7) 0.88367(6) 0.41873(6) 0.0288(2) Uani 1 1 d . . . As1 As 0.25671(9) 1.00583(8) 0.38063(8) 0.0277(3) Uani 1 1 d . . . S1 S 0.5668(2) 1.1943(2) 0.2190(2) 0.0322(5) Uani 1 1 d . . . N1 N 0.8823(8) 0.8067(7) 0.2924(7) 0.0317(16) Uani 1 1 d . . . N2 N 0.6729(8) 0.6521(7) 0.5055(7) 0.0325(17) Uani 1 1 d . . . C1 C 0.2568(10) 1.1665(8) 0.2156(9) 0.0316(19) Uani 1 1 d . . . C2 C 0.3881(10) 1.2415(8) 0.1475(8) 0.032(2) Uani 1 1 d . . . C3 C 0.3795(12) 1.3542(9) 0.0303(9) 0.044(2) Uani 1 1 d . . . H3A H 0.4668 1.4028 -0.0145 0.052 Uiso 1 1 calc R . . C4 C 0.2381(13) 1.3944(10) -0.0202(11) 0.053(3) Uani 1 1 d . . . H4A H 0.2338 1.4695 -0.1014 0.064 Uiso 1 1 calc R . . C5 C 0.1041(14) 1.3290(11) 0.0437(12) 0.057(3) Uani 1 1 d . . . H5A H 0.0087 1.3607 0.0095 0.069 Uiso 1 1 calc R . . C6 C 0.1162(12) 1.2116(10) 0.1634(10) 0.048(3) Uani 1 1 d . . . H6A H 0.0282 1.1638 0.2079 0.057 Uiso 1 1 calc R . . C7 C 0.9887(11) 0.8817(10) 0.1899(9) 0.042(2) Uani 1 1 d . . . H7A H 0.9778 0.9713 0.1689 0.051 Uiso 1 1 calc R . . C8 C 1.1139(11) 0.8321(10) 0.1139(9) 0.045(2) Uani 1 1 d . . . H8A H 1.1851 0.8872 0.0437 0.054 Uiso 1 1 calc R . . C9 C 1.1304(11) 0.7003(10) 0.1446(9) 0.044(2) Uani 1 1 d . . . H9A H 1.2127 0.6655 0.0940 0.052 Uiso 1 1 calc R . . C10 C 1.0225(10) 0.6160(9) 0.2534(8) 0.035(2) Uani 1 1 d . . . C11 C 1.0337(11) 0.4799(10) 0.2884(10) 0.046(2) Uani 1 1 d . . . H11A H 1.1150 0.4420 0.2400 0.055 Uiso 1 1 calc R . . C12 C 0.9263(13) 0.4033(10) 0.3923(10) 0.050(3) Uani 1 1 d . . . H12A H 0.9330 0.3143 0.4127 0.060 Uiso 1 1 calc R . . C13 C 0.8047(11) 0.4582(9) 0.4695(9) 0.038(2) Uani 1 1 d . . . C14 C 0.6904(12) 0.3829(9) 0.5797(10) 0.048(3) Uani 1 1 d . . . H14A H 0.6956 0.2929 0.6045 0.057 Uiso 1 1 calc R . . C15 C 0.5754(12) 0.4398(9) 0.6482(9) 0.046(3) Uani 1 1 d . . . H15A H 0.5005 0.3904 0.7200 0.055 Uiso 1 1 calc R . . C16 C 0.5700(11) 0.5776(9) 0.6090(9) 0.038(2) Uani 1 1 d . . . H16A H 0.4915 0.6169 0.6576 0.046 Uiso 1 1 calc R . . C17 C 0.7884(10) 0.5949(8) 0.4358(9) 0.0311(19) Uani 1 1 d . . . C18 C 0.8992(10) 0.6757(8) 0.3243(8) 0.0301(19) Uani 1 1 d . . . O1 O 0.1098(6) 0.9288(6) 0.3826(6) 0.0397(15) Uani 1 1 d . . . H1A H 0.0220 0.9488 0.4240 0.060 Uiso 1 1 calc R . . O2 O 0.4226(6) 0.8970(5) 0.3772(6) 0.0313(13) Uani 1 1 d . . . O3 O 0.1941(6) 1.0383(5) 0.5112(5) 0.0297(13) Uani 1 1 d . . . O4 O 0.6414(8) 1.3131(6) 0.1625(6) 0.0474(18) Uani 1 1 d . . . O5 O 0.6709(7) 1.0882(6) 0.1899(6) 0.0378(15) Uani 1 1 d . . . O6 O 0.5006(7) 1.1439(6) 0.3615(5) 0.0377(15) Uani 1 1 d . . . O1W O 0.5396(19) 0.8716(15) 0.1258(14) 0.201(7) Uani 1 1 d . . . H1WA H 0.5098 0.8754 0.1996 0.301 Uiso 1 1 d R . . H1WB H 0.5916 0.9362 0.0692 0.301 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0182(4) 0.0343(4) 0.0350(4) -0.0190(3) 0.0017(3) -0.0057(3) As1 0.0159(5) 0.0327(5) 0.0356(5) -0.0182(4) 0.0011(3) -0.0057(4) S1 0.0229(11) 0.0356(12) 0.0332(12) -0.0153(10) 0.0058(9) -0.0089(9) N1 0.029(4) 0.038(4) 0.030(4) -0.018(3) 0.001(3) -0.009(3) N2 0.023(4) 0.036(4) 0.042(4) -0.023(4) 0.002(3) -0.007(3) C1 0.025(5) 0.031(5) 0.044(5) -0.023(4) -0.008(4) 0.001(3) C2 0.027(5) 0.036(5) 0.033(5) -0.018(4) -0.006(4) 0.003(4) C3 0.043(6) 0.039(5) 0.042(6) -0.015(5) -0.008(4) 0.002(4) C4 0.068(8) 0.042(6) 0.048(6) -0.013(5) -0.028(6) 0.002(5) C5 0.055(7) 0.055(7) 0.071(8) -0.032(6) -0.027(6) 0.005(5) C6 0.039(6) 0.050(6) 0.066(7) -0.028(6) -0.021(5) -0.006(5) C7 0.035(6) 0.050(6) 0.038(5) -0.020(5) 0.001(4) -0.008(4) C8 0.031(5) 0.060(7) 0.036(5) -0.020(5) 0.001(4) -0.008(5) C9 0.027(5) 0.067(7) 0.036(5) -0.029(5) -0.001(4) 0.002(4) C10 0.029(5) 0.045(6) 0.029(5) -0.019(4) -0.006(4) 0.003(4) C11 0.041(6) 0.051(6) 0.048(6) -0.034(5) -0.013(5) 0.020(5) C12 0.060(7) 0.044(6) 0.050(7) -0.029(5) -0.014(5) 0.006(5) C13 0.031(5) 0.041(5) 0.044(6) -0.019(5) -0.009(4) -0.003(4) C14 0.064(7) 0.030(5) 0.050(6) -0.016(5) -0.010(5) -0.013(5) C15 0.053(7) 0.040(6) 0.040(6) -0.014(5) 0.004(5) -0.020(5) C16 0.033(5) 0.041(5) 0.041(5) -0.021(5) 0.002(4) -0.007(4) C17 0.027(5) 0.035(5) 0.036(5) -0.023(4) -0.003(4) -0.001(4) C18 0.022(4) 0.039(5) 0.031(5) -0.020(4) -0.004(3) 0.000(3) O1 0.014(3) 0.058(4) 0.055(4) -0.035(3) 0.006(3) -0.013(3) O2 0.019(3) 0.030(3) 0.038(3) -0.012(3) -0.002(2) -0.003(2) O3 0.017(3) 0.042(3) 0.038(3) -0.023(3) 0.000(2) -0.011(2) O4 0.040(4) 0.041(4) 0.050(4) -0.008(3) -0.003(3) -0.019(3) O5 0.022(3) 0.043(4) 0.044(4) -0.022(3) 0.002(3) -0.001(3) O6 0.028(3) 0.057(4) 0.027(3) -0.018(3) -0.003(2) -0.007(3) O1W 0.248(19) 0.233(18) 0.168(15) -0.134(14) 0.015(13) -0.078(15) _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 Cd1 O2 2.192(6) . ? Cd1 O3 2.233(5) 2_676 ? Cd1 N1 2.335(7) . ? Cd1 N2 2.349(7) . ? Cd1 O6 2.462(6) 2_676 ? Cd1 O5 2.574(6) . ? As1 O2 1.653(6) . ? As1 O3 1.665(6) . ? As1 O1 1.719(5) . ? As1 C1 1.927(9) . ? S1 O4 1.441(6) . ? S1 O5 1.451(6) . ? S1 O6 1.463(6) . ? S1 C2 1.802(9) . ? N1 C7 1.343(10) . ? N1 C18 1.355(10) . ? N2 C16 1.329(10) . ? N2 C17 1.351(10) . ? C1 C6 1.383(12) . ? C1 C2 1.410(11) . ? C2 C3 1.366(12) . ? C3 C4 1.383(13) . ? C3 H3A 0.9300 . ? C4 C5 1.370(14) . ? C4 H4A 0.9300 . ? C5 C6 1.410(14) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.387(13) . ? C7 H7A 0.9300 . ? C8 C9 1.368(14) . ? C8 H8A 0.9300 . ? C9 C10 1.423(12) . ? C9 H9A 0.9300 . ? C10 C18 1.406(11) . ? C10 C11 1.410(13) . ? C11 C12 1.362(13) . ? C11 H11A 0.9300 . ? C12 C13 1.415(13) . ? C12 H12A 0.9300 . ? C13 C17 1.414(11) . ? C13 C14 1.421(12) . ? C14 C15 1.339(13) . ? C14 H14A 0.9300 . ? C15 C16 1.424(12) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 C18 1.434(10) . ? O1 H1A 0.8200 . ? O3 Cd1 2.233(5) 2_676 ? O6 Cd1 2.462(6) 2_676 ? O1W H1WA 0.8501 . ? O1W H1WB 0.8499 . ? 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 Cd1 O3 146.5(2) . 2_676 ? O2 Cd1 N1 114.1(2) . . ? O3 Cd1 N1 96.2(2) 2_676 . ? O2 Cd1 N2 85.7(2) . . ? O3 Cd1 N2 118.9(2) 2_676 . ? N1 Cd1 N2 71.2(2) . . ? O2 Cd1 O6 83.7(2) . 2_676 ? O3 Cd1 O6 76.52(19) 2_676 2_676 ? N1 Cd1 O6 149.0(2) . 2_676 ? N2 Cd1 O6 85.8(2) . 2_676 ? O2 Cd1 O5 79.31(19) . . ? O3 Cd1 O5 93.4(2) 2_676 . ? N1 Cd1 O5 79.2(2) . . ? N2 Cd1 O5 137.6(2) . . ? O6 Cd1 O5 130.8(2) 2_676 . ? O2 As1 O3 118.4(3) . . ? O2 As1 O1 101.7(3) . . ? O3 As1 O1 107.2(3) . . ? O2 As1 C1 112.7(3) . . ? O3 As1 C1 111.8(3) . . ? O1 As1 C1 103.1(3) . . ? O4 S1 O5 113.8(4) . . ? O4 S1 O6 113.8(4) . . ? O5 S1 O6 110.4(4) . . ? O4 S1 C2 106.6(4) . . ? O5 S1 C2 108.0(4) . . ? O6 S1 C2 103.5(4) . . ? C7 N1 C18 118.5(7) . . ? C7 N1 Cd1 125.6(6) . . ? C18 N1 Cd1 115.9(5) . . ? C16 N2 C17 119.0(7) . . ? C16 N2 Cd1 125.5(6) . . ? C17 N2 Cd1 115.4(5) . . ? C6 C1 C2 118.5(8) . . ? C6 C1 As1 116.9(7) . . ? C2 C1 As1 124.5(6) . . ? C3 C2 C1 121.1(8) . . ? C3 C2 S1 118.7(7) . . ? C1 C2 S1 120.0(7) . . ? C2 C3 C4 118.6(9) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C5 C4 C3 123.1(10) . . ? C5 C4 H4A 118.4 . . ? C3 C4 H4A 118.4 . . ? C4 C5 C6 117.5(10) . . ? C4 C5 H5A 121.3 . . ? C6 C5 H5A 121.3 . . ? C1 C6 C5 121.1(9) . . ? C1 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? N1 C7 C8 123.3(9) . . ? N1 C7 H7A 118.4 . . ? C8 C7 H7A 118.4 . . ? C9 C8 C7 118.5(8) . . ? C9 C8 H8A 120.7 . . ? C7 C8 H8A 120.7 . . ? C8 C9 C10 120.5(8) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C18 C10 C11 120.6(8) . . ? C18 C10 C9 116.7(8) . . ? C11 C10 C9 122.6(8) . . ? C12 C11 C10 120.6(8) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C13 120.5(9) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C17 C13 C12 120.3(8) . . ? C17 C13 C14 116.7(8) . . ? C12 C13 C14 123.0(9) . . ? C15 C14 C13 120.8(8) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C14 C15 C16 118.7(8) . . ? C14 C15 H15A 120.6 . . ? C16 C15 H15A 120.6 . . ? N2 C16 C15 122.3(8) . . ? N2 C16 H16A 118.8 . . ? C15 C16 H16A 118.8 . . ? N2 C17 C13 122.4(7) . . ? N2 C17 C18 118.7(7) . . ? C13 C17 C18 118.9(7) . . ? N1 C18 C10 122.5(7) . . ? N1 C18 C17 118.5(7) . . ? C10 C18 C17 119.0(8) . . ? As1 O1 H1A 109.5 . . ? As1 O2 Cd1 128.7(3) . . ? As1 O3 Cd1 125.9(3) . 2_676 ? S1 O5 Cd1 103.7(3) . . ? S1 O6 Cd1 164.6(4) . 2_676 ? H1WA O1W H1WB 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O3 0.82 1.80 2.579(8) 158.6 2_576 O1W H1WA O2 0.85 2.12 2.969(15) 175.8 . _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 3.118 _refine_diff_density_min -2.917 _refine_diff_density_rms 0.231 #===end data_8 _database_code_depnum_ccdc_archive 'CCDC 763198' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H32 As2 N6 O12 S2 Zn2' _chemical_formula_weight 1157.44 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' 'S' 'S' 0.1246 0.1234 '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 'triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.393(2) _cell_length_b 9.906(3) _cell_length_c 13.577(4) _cell_angle_alpha 88.783(9) _cell_angle_beta 74.243(6) _cell_angle_gamma 75.784(8) _cell_volume 1051.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2463 _cell_measurement_theta_min 3.0098 _cell_measurement_theta_max 27.4758 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 2.874 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7737 _exptl_absorpt_correction_T_max 1 _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8301 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4742 _reflns_number_gt 3634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0390P)^2^+0.4826P] 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 shelxtl _refine_ls_extinction_coef ? _refine_ls_number_reflns 4742 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.43538(5) 0.88398(4) 0.65414(3) 0.03067(11) Uani 1 1 d . . . As1 As 0.69532(4) 0.79166(3) 0.42559(2) 0.02942(10) Uani 1 1 d . . . S1 S 0.81796(11) 0.75793(10) 0.15514(7) 0.0374(2) Uani 1 1 d . . . N1 N 0.2276(3) 0.7753(3) 0.6747(2) 0.0326(6) Uani 1 1 d . . . N2 N 0.4065(3) 0.8063(3) 0.79949(19) 0.0272(6) Uani 1 1 d . . . N3 N 0.6213(3) 0.9524(3) 0.7101(2) 0.0328(6) Uani 1 1 d . . . C1 C 0.6020(4) 0.6976(3) 0.3398(2) 0.0301(7) Uani 1 1 d . . . C2 C 0.6485(4) 0.6899(3) 0.2325(2) 0.0290(7) Uani 1 1 d . . . C3 C 0.5653(4) 0.6205(4) 0.1832(3) 0.0373(8) Uani 1 1 d . . . H3A H 0.5946 0.6152 0.1120 0.045 Uiso 1 1 calc R . . C4 C 0.4394(5) 0.5588(4) 0.2380(3) 0.0441(9) Uani 1 1 d . . . H4A H 0.3827 0.5151 0.2035 0.053 Uiso 1 1 calc R . . C5 C 0.3978(5) 0.5619(4) 0.3434(3) 0.0463(9) Uani 1 1 d . . . H5A H 0.3156 0.5180 0.3803 0.056 Uiso 1 1 calc R . . C6 C 0.4795(4) 0.6309(4) 0.3938(3) 0.0383(8) Uani 1 1 d . . . H6A H 0.4522 0.6327 0.4649 0.046 Uiso 1 1 calc R . . C7 C 0.1441(5) 0.7590(4) 0.6069(3) 0.0413(8) Uani 1 1 d . . . H7A H 0.1688 0.8015 0.5447 0.050 Uiso 1 1 calc R . . C8 C 0.0232(5) 0.6827(4) 0.6238(3) 0.0458(9) Uani 1 1 d . . . H8A H -0.0308 0.6725 0.5740 0.055 Uiso 1 1 calc R . . C9 C -0.0154(5) 0.6218(4) 0.7167(3) 0.0451(9) Uani 1 1 d . . . H9A H -0.0963 0.5695 0.7306 0.054 Uiso 1 1 calc R . . C10 C 0.0668(4) 0.6392(4) 0.7889(3) 0.0389(8) Uani 1 1 d . . . H10A H 0.0418 0.5992 0.8521 0.047 Uiso 1 1 calc R . . C11 C 0.1872(4) 0.7171(3) 0.7659(2) 0.0283(7) Uani 1 1 d . . . C12 C 0.2811(4) 0.7434(3) 0.8391(2) 0.0282(7) Uani 1 1 d . . . C13 C 0.2419(5) 0.7098(4) 0.9404(3) 0.0400(8) Uani 1 1 d . . . H13A H 0.1532 0.6673 0.9675 0.048 Uiso 1 1 calc R . . C14 C 0.3380(5) 0.7411(4) 1.0004(3) 0.0450(9) Uani 1 1 d . . . H14A H 0.3141 0.7201 1.0691 0.054 Uiso 1 1 calc R . . C15 C 0.4690(5) 0.8031(4) 0.9589(3) 0.0433(9) Uani 1 1 d . . . H15A H 0.5366 0.8216 0.9985 0.052 Uiso 1 1 calc R . . C16 C 0.4990(4) 0.8375(3) 0.8578(2) 0.0312(7) Uani 1 1 d . . . C17 C 0.6289(4) 0.9139(3) 0.8047(3) 0.0323(7) Uani 1 1 d . . . C18 C 0.7489(5) 0.9439(4) 0.8475(3) 0.0429(9) Uani 1 1 d . . . H18A H 0.7525 0.9166 0.9130 0.052 Uiso 1 1 calc R . . C19 C 0.8622(5) 1.0140(4) 0.7923(3) 0.0517(11) Uani 1 1 d . . . H19A H 0.9437 1.0350 0.8200 0.062 Uiso 1 1 calc R . . C20 C 0.8553(5) 1.0539(4) 0.6949(4) 0.0533(11) Uani 1 1 d . . . H20A H 0.9312 1.1020 0.6564 0.064 Uiso 1 1 calc R . . C21 C 0.7335(5) 1.0204(4) 0.6567(3) 0.0431(9) Uani 1 1 d . . . H21A H 0.7289 1.0461 0.5910 0.052 Uiso 1 1 calc R . . O1 O 0.6118(3) 0.7552(2) 0.54534(17) 0.0403(6) Uani 1 1 d . . . O2 O 0.9103(3) 0.7086(3) 0.39827(19) 0.0417(6) Uani 1 1 d . . . H2A H 0.9507 0.6958 0.3361 0.063 Uiso 1 1 calc R . . O3 O 0.6797(3) 0.9599(2) 0.4112(2) 0.0435(6) Uani 1 1 d . . . O4 O 0.9654(3) 0.6976(3) 0.19138(19) 0.0476(7) Uani 1 1 d . . . O5 O 0.8405(4) 0.7114(5) 0.0529(2) 0.0984(15) Uani 1 1 d . . . O6 O 0.7660(4) 0.9049(3) 0.1751(4) 0.1048(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0332(2) 0.0350(2) 0.0279(2) 0.00838(16) -0.01146(16) -0.01326(18) As1 0.03107(18) 0.03059(19) 0.02807(18) 0.00542(13) -0.00950(14) -0.00920(15) S1 0.0304(4) 0.0447(5) 0.0345(5) 0.0109(4) -0.0045(3) -0.0102(4) N1 0.0328(15) 0.0366(16) 0.0323(15) 0.0062(12) -0.0130(12) -0.0114(13) N2 0.0283(13) 0.0277(14) 0.0261(13) 0.0027(10) -0.0078(11) -0.0073(12) N3 0.0273(14) 0.0311(15) 0.0401(16) 0.0009(12) -0.0093(12) -0.0073(12) C1 0.0260(16) 0.0286(17) 0.0357(18) 0.0082(14) -0.0096(14) -0.0064(14) C2 0.0257(16) 0.0265(17) 0.0329(17) 0.0047(13) -0.0071(13) -0.0041(14) C3 0.043(2) 0.038(2) 0.0338(18) 0.0005(15) -0.0168(16) -0.0084(17) C4 0.045(2) 0.040(2) 0.057(2) 0.0046(18) -0.0219(19) -0.0198(18) C5 0.041(2) 0.045(2) 0.058(2) 0.0132(18) -0.0115(19) -0.0226(19) C6 0.041(2) 0.038(2) 0.0369(19) 0.0063(15) -0.0076(16) -0.0150(17) C7 0.042(2) 0.050(2) 0.0366(19) 0.0075(16) -0.0169(16) -0.0127(18) C8 0.043(2) 0.051(2) 0.050(2) -0.0008(18) -0.0252(18) -0.0104(19) C9 0.042(2) 0.041(2) 0.061(2) 0.0058(18) -0.0221(19) -0.0185(18) C10 0.0383(19) 0.036(2) 0.045(2) 0.0095(16) -0.0110(16) -0.0145(17) C11 0.0262(16) 0.0255(16) 0.0321(17) 0.0043(13) -0.0084(13) -0.0045(13) C12 0.0268(16) 0.0281(17) 0.0270(16) 0.0016(13) -0.0061(13) -0.0034(14) C13 0.040(2) 0.045(2) 0.0338(18) 0.0053(15) -0.0059(16) -0.0133(18) C14 0.050(2) 0.058(3) 0.0283(18) 0.0082(16) -0.0121(17) -0.015(2) C15 0.047(2) 0.053(2) 0.0350(19) 0.0001(17) -0.0202(17) -0.0112(19) C16 0.0325(17) 0.0290(17) 0.0323(17) -0.0014(13) -0.0127(14) -0.0036(14) C17 0.0302(17) 0.0295(18) 0.0364(18) -0.0040(14) -0.0102(14) -0.0041(14) C18 0.042(2) 0.041(2) 0.050(2) -0.0096(17) -0.0202(18) -0.0083(18) C19 0.038(2) 0.051(3) 0.073(3) -0.012(2) -0.021(2) -0.016(2) C20 0.038(2) 0.048(2) 0.077(3) -0.002(2) -0.008(2) -0.025(2) C21 0.038(2) 0.040(2) 0.051(2) 0.0085(17) -0.0081(17) -0.0143(17) O1 0.0526(15) 0.0378(14) 0.0264(12) 0.0054(10) -0.0057(11) -0.0098(12) O2 0.0341(13) 0.0500(16) 0.0414(14) 0.0000(11) -0.0150(11) -0.0059(12) O3 0.0538(16) 0.0300(13) 0.0583(16) 0.0132(11) -0.0314(13) -0.0151(12) O4 0.0358(14) 0.0676(19) 0.0444(15) 0.0139(13) -0.0122(12) -0.0217(14) O5 0.068(2) 0.213(5) 0.0324(16) 0.004(2) -0.0054(15) -0.077(3) O6 0.053(2) 0.0392(19) 0.179(4) 0.036(2) 0.027(2) -0.0028(16) _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 1.945(2) 2_676 ? Zn1 O1 1.992(2) . ? Zn1 N2 2.077(3) . ? Zn1 N3 2.158(3) . ? Zn1 N1 2.218(3) . ? As1 O3 1.652(2) . ? As1 O1 1.657(2) . ? As1 O2 1.729(2) . ? As1 C1 1.933(3) . ? S1 O5 1.420(3) . ? S1 O6 1.423(3) . ? S1 O4 1.444(3) . ? S1 C2 1.791(3) . ? N1 C7 1.333(4) . ? N1 C11 1.349(4) . ? N2 C12 1.336(4) . ? N2 C16 1.337(4) . ? N3 C21 1.337(4) . ? N3 C17 1.346(4) . ? C1 C6 1.391(4) . ? C1 C2 1.401(4) . ? C2 C3 1.385(4) . ? C3 C4 1.383(5) . ? C3 H3A 0.9300 . ? C4 C5 1.377(5) . ? C4 H4A 0.9300 . ? C5 C6 1.383(5) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.377(5) . ? C7 H7A 0.9300 . ? C8 C9 1.379(5) . ? C8 H8A 0.9300 . ? C9 C10 1.378(5) . ? C9 H9A 0.9300 . ? C10 C11 1.384(4) . ? C10 H10A 0.9300 . ? C11 C12 1.488(4) . ? C12 C13 1.379(4) . ? C13 C14 1.379(5) . ? C13 H13A 0.9300 . ? C14 C15 1.373(5) . ? C14 H14A 0.9300 . ? C15 C16 1.378(5) . ? C15 H15A 0.9300 . ? C16 C17 1.495(5) . ? C17 C18 1.383(4) . ? C18 C19 1.365(5) . ? C18 H18A 0.9300 . ? C19 C20 1.384(6) . ? C19 H19A 0.9300 . ? C20 C21 1.373(5) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? O2 H2A 0.8200 . ? O3 Zn1 1.945(2) 2_676 ? 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 108.38(11) 2_676 . ? O3 Zn1 N2 137.85(11) 2_676 . ? O1 Zn1 N2 113.29(10) . . ? O3 Zn1 N3 107.54(10) 2_676 . ? O1 Zn1 N3 93.74(11) . . ? N2 Zn1 N3 76.23(10) . . ? O3 Zn1 N1 93.43(10) 2_676 . ? O1 Zn1 N1 98.17(10) . . ? N2 Zn1 N1 75.01(10) . . ? N3 Zn1 N1 151.23(10) . . ? O3 As1 O1 112.91(12) . . ? O3 As1 O2 107.59(12) . . ? O1 As1 O2 105.11(12) . . ? O3 As1 C1 117.36(13) . . ? O1 As1 C1 106.80(13) . . ? O2 As1 C1 106.21(12) . . ? O5 S1 O6 115.8(3) . . ? O5 S1 O4 112.0(2) . . ? O6 S1 O4 110.7(2) . . ? O5 S1 C2 105.68(17) . . ? O6 S1 C2 106.24(17) . . ? O4 S1 C2 105.55(15) . . ? C7 N1 C11 117.8(3) . . ? C7 N1 Zn1 127.4(2) . . ? C11 N1 Zn1 114.7(2) . . ? C12 N2 C16 120.4(3) . . ? C12 N2 Zn1 120.2(2) . . ? C16 N2 Zn1 118.7(2) . . ? C21 N3 C17 118.8(3) . . ? C21 N3 Zn1 125.6(2) . . ? C17 N3 Zn1 115.5(2) . . ? C6 C1 C2 119.5(3) . . ? C6 C1 As1 114.2(2) . . ? C2 C1 As1 126.4(2) . . ? C3 C2 C1 118.7(3) . . ? C3 C2 S1 118.0(2) . . ? C1 C2 S1 123.3(2) . . ? C4 C3 C2 121.2(3) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C5 C4 C3 120.3(3) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 119.2(3) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C5 C6 C1 121.1(3) . . ? C5 C6 H6A 119.4 . . ? C1 C6 H6A 119.4 . . ? N1 C7 C8 123.6(3) . . ? N1 C7 H7A 118.2 . . ? C8 C7 H7A 118.2 . . ? C7 C8 C9 118.0(3) . . ? C7 C8 H8A 121.0 . . ? C9 C8 H8A 121.0 . . ? C10 C9 C8 119.5(3) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C9 C10 C11 118.9(3) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? N1 C11 C10 122.1(3) . . ? N1 C11 C12 115.0(3) . . ? C10 C11 C12 123.0(3) . . ? N2 C12 C13 121.7(3) . . ? N2 C12 C11 114.5(3) . . ? C13 C12 C11 123.8(3) . . ? C12 C13 C14 118.0(3) . . ? C12 C13 H13A 121.0 . . ? C14 C13 H13A 121.0 . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 119.1(3) . . ? C14 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? N2 C16 C15 120.7(3) . . ? N2 C16 C17 114.5(3) . . ? C15 C16 C17 124.8(3) . . ? N3 C17 C18 121.5(3) . . ? N3 C17 C16 114.7(3) . . ? C18 C17 C16 123.8(3) . . ? C19 C18 C17 119.1(4) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? C18 C19 C20 119.7(3) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C21 C20 C19 118.3(4) . . ? C21 C20 H20A 120.9 . . ? C19 C20 H20A 120.9 . . ? N3 C21 C20 122.6(4) . . ? N3 C21 H21A 118.7 . . ? C20 C21 H21A 118.7 . . ? As1 O1 Zn1 127.04(14) . . ? As1 O2 H2A 109.5 . . ? As1 O3 Zn1 140.47(14) . 2_676 ? 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 O2 H2A O4 0.82 1.93 2.720(4) 160.2 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.589 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.082 #===end data_9 _database_code_depnum_ccdc_archive 'CCDC 763199' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H36 As2 Cd2 N6 O14 S2' _chemical_formula_weight 1287.53 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' 'S' 'S' 0.1246 0.1234 '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' 'Cd' 'Cd' -0.8075 1.2024 '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 8.430(3) _cell_length_b 11.210(4) _cell_length_c 13.470(5) _cell_angle_alpha 91.350(2) _cell_angle_beta 107.890(5) _cell_angle_gamma 111.450(4) _cell_volume 1114.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3105 _cell_measurement_theta_min 2.6911 _cell_measurement_theta_max 27.4835 _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.919 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 2.598 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.8709 _exptl_absorpt_correction_T_max 1 _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8199 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0255 _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 -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4825 _reflns_number_gt 4207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0371P)^2^+0.0806P] 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 shelxtl _refine_ls_extinction_coef ? _refine_ls_number_reflns 4825 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0584 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Cd1 Cd 0.336947(19) 0.935935(13) 0.287905(10) 0.02456(6) Uani 1 1 d . . . As1 As 0.45725(3) 1.182659(19) 0.487627(14) 0.02401(6) Uani 1 1 d . . . S1 S 0.39700(7) 1.26548(5) 0.22984(4) 0.02657(11) Uani 1 1 d . . . N1 N 0.5753(2) 0.97423(16) 0.22007(13) 0.0271(3) Uani 1 1 d . . . N2 N 0.2281(2) 0.81297(15) 0.12266(12) 0.0232(3) Uani 1 1 d . . . N3 N 0.0220(2) 0.80799(16) 0.24094(13) 0.0270(3) Uani 1 1 d . . . C1 C 0.6426(3) 1.26743(18) 0.42690(15) 0.0245(4) Uani 1 1 d . . . C2 C 0.6159(3) 1.30321(18) 0.32543(15) 0.0255(4) Uani 1 1 d . . . C3 C 0.7654(3) 1.3672(2) 0.29577(17) 0.0333(5) Uani 1 1 d . . . H3A H 0.7489 1.3948 0.2302 0.040 Uiso 1 1 calc R . . C4 C 0.9395(3) 1.3905(2) 0.36289(19) 0.0388(5) Uani 1 1 d . . . H4A H 1.0385 1.4320 0.3415 0.047 Uiso 1 1 calc R . . C5 C 0.9652(3) 1.3523(2) 0.46075(19) 0.0381(5) Uani 1 1 d . . . H5A H 1.0813 1.3657 0.5050 0.046 Uiso 1 1 calc R . . C6 C 0.8180(3) 1.2937(2) 0.49344(17) 0.0317(4) Uani 1 1 d . . . H6A H 0.8368 1.2716 0.5610 0.038 Uiso 1 1 calc R . . C7 C 0.7474(3) 1.0546(2) 0.27111(18) 0.0349(5) Uani 1 1 d . . . H7A H 0.7764 1.0969 0.3384 0.042 Uiso 1 1 calc R . . C8 C 0.8841(3) 1.0779(2) 0.2291(2) 0.0423(6) Uani 1 1 d . . . H8A H 1.0022 1.1341 0.2674 0.051 Uiso 1 1 calc R . . C9 C 0.8414(3) 1.0160(2) 0.1292(2) 0.0391(5) Uani 1 1 d . . . H9A H 0.9298 1.0315 0.0980 0.047 Uiso 1 1 calc R . . C10 C 0.6656(3) 0.9308(2) 0.07621(18) 0.0333(5) Uani 1 1 d . . . H10A H 0.6347 0.8868 0.0093 0.040 Uiso 1 1 calc R . . C11 C 0.5348(3) 0.91123(18) 0.12373(15) 0.0245(4) Uani 1 1 d . . . C12 C 0.3432(3) 0.81700(18) 0.07174(15) 0.0252(4) Uani 1 1 d . . . C13 C 0.2868(3) 0.7370(2) -0.02279(17) 0.0374(5) Uani 1 1 d . . . H13A H 0.3685 0.7388 -0.0566 0.045 Uiso 1 1 calc R . . C14 C 0.1058(3) 0.6540(3) -0.06599(18) 0.0431(6) Uani 1 1 d . . . H14A H 0.0647 0.6001 -0.1299 0.052 Uiso 1 1 calc R . . C15 C -0.0133(3) 0.6513(2) -0.01420(17) 0.0353(5) Uani 1 1 d . . . H15A H -0.1354 0.5974 -0.0432 0.042 Uiso 1 1 calc R . . C16 C 0.0537(3) 0.73089(18) 0.08218(15) 0.0246(4) Uani 1 1 d . . . C17 C -0.0608(3) 0.72781(18) 0.14882(15) 0.0251(4) Uani 1 1 d . . . C18 C -0.2427(3) 0.6467(2) 0.11668(18) 0.0347(5) Uani 1 1 d . . . H18A H -0.2984 0.5924 0.0520 0.042 Uiso 1 1 calc R . . C19 C -0.3402(3) 0.6477(2) 0.18252(19) 0.0392(5) Uani 1 1 d . . . H19A H -0.4620 0.5930 0.1628 0.047 Uiso 1 1 calc R . . C20 C -0.2562(3) 0.7298(2) 0.27720(19) 0.0380(5) Uani 1 1 d . . . H20A H -0.3194 0.7321 0.3225 0.046 Uiso 1 1 calc R . . C21 C -0.0745(3) 0.8092(2) 0.30315(17) 0.0337(5) Uani 1 1 d . . . H21A H -0.0171 0.8659 0.3667 0.040 Uiso 1 1 calc R . . O1 O 0.3272(2) 1.03209(15) 0.42835(12) 0.0395(4) Uani 1 1 d . . . O2 O 0.3259(2) 1.27307(17) 0.47596(13) 0.0432(4) Uani 1 1 d . . . H2A H 0.3068 1.2962 0.4177 0.065 Uiso 1 1 calc R . . O3 O 0.5560(2) 1.19879(13) 0.61691(10) 0.0307(3) Uani 1 1 d . . . O4 O 0.3050(2) 1.32487(16) 0.27783(12) 0.0376(4) Uani 1 1 d . . . O5 O 0.3084(2) 1.12454(15) 0.21215(14) 0.0446(4) Uani 1 1 d . . . O6 O 0.4254(2) 1.31803(17) 0.13704(12) 0.0423(4) Uani 1 1 d . . . O1W O 0.7448(3) 1.43442(17) 0.76031(15) 0.0529(5) Uani 1 1 d . . . H1WB H 0.6884 1.3637 0.7173 0.079 Uiso 1 1 d R . . H1WA H 0.6735 1.4726 0.7580 0.079 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02625(9) 0.02518(8) 0.02125(8) -0.00067(5) 0.00811(6) 0.00920(6) As1 0.02721(11) 0.02707(11) 0.01976(10) 0.00106(7) 0.00999(8) 0.01135(9) S1 0.0298(3) 0.0275(2) 0.0243(2) 0.00559(18) 0.0083(2) 0.0140(2) N1 0.0249(8) 0.0251(8) 0.0315(9) 0.0013(7) 0.0088(7) 0.0109(7) N2 0.0247(8) 0.0235(8) 0.0214(8) 0.0022(6) 0.0080(6) 0.0095(7) N3 0.0262(8) 0.0308(9) 0.0254(8) 0.0022(7) 0.0094(7) 0.0122(7) C1 0.0259(9) 0.0257(9) 0.0242(9) 0.0010(7) 0.0100(8) 0.0114(8) C2 0.0282(10) 0.0248(9) 0.0259(9) 0.0018(7) 0.0112(8) 0.0114(8) C3 0.0366(12) 0.0334(11) 0.0305(11) 0.0044(8) 0.0179(9) 0.0092(9) C4 0.0304(11) 0.0381(12) 0.0434(13) -0.0021(10) 0.0196(10) 0.0032(10) C5 0.0236(10) 0.0404(12) 0.0419(13) -0.0037(10) 0.0068(10) 0.0074(9) C6 0.0293(11) 0.0370(11) 0.0259(10) 0.0022(8) 0.0061(8) 0.0126(9) C7 0.0274(10) 0.0306(10) 0.0402(12) -0.0058(9) 0.0066(9) 0.0091(9) C8 0.0263(11) 0.0359(12) 0.0571(15) -0.0022(11) 0.0106(11) 0.0074(10) C9 0.0315(11) 0.0416(12) 0.0517(14) 0.0122(10) 0.0232(11) 0.0149(10) C10 0.0338(11) 0.0364(11) 0.0331(11) 0.0071(9) 0.0151(9) 0.0144(10) C11 0.0267(10) 0.0235(9) 0.0262(9) 0.0057(7) 0.0096(8) 0.0126(8) C12 0.0292(10) 0.0259(9) 0.0226(9) 0.0045(7) 0.0100(8) 0.0123(8) C13 0.0354(12) 0.0443(13) 0.0311(11) -0.0040(9) 0.0169(10) 0.0099(10) C14 0.0393(13) 0.0496(14) 0.0295(11) -0.0138(10) 0.0123(10) 0.0060(11) C15 0.0298(11) 0.0383(11) 0.0277(11) -0.0042(9) 0.0064(9) 0.0055(9) C16 0.0256(9) 0.0242(9) 0.0228(9) 0.0028(7) 0.0070(8) 0.0097(8) C17 0.0258(10) 0.0241(9) 0.0261(10) 0.0041(7) 0.0084(8) 0.0108(8) C18 0.0277(11) 0.0334(11) 0.0369(12) -0.0018(9) 0.0110(9) 0.0058(9) C19 0.0273(11) 0.0388(12) 0.0495(14) 0.0070(10) 0.0170(10) 0.0073(10) C20 0.0382(12) 0.0463(13) 0.0414(13) 0.0116(10) 0.0238(11) 0.0208(11) C21 0.0356(12) 0.0415(12) 0.0283(11) 0.0025(9) 0.0127(9) 0.0185(10) O1 0.0410(9) 0.0364(8) 0.0330(8) -0.0099(6) 0.0200(7) 0.0011(7) O2 0.0517(10) 0.0619(11) 0.0402(9) 0.0160(8) 0.0250(8) 0.0406(9) O3 0.0447(9) 0.0281(7) 0.0208(7) 0.0015(5) 0.0106(6) 0.0167(7) O4 0.0427(9) 0.0479(9) 0.0337(8) 0.0085(7) 0.0141(7) 0.0293(8) O5 0.0375(9) 0.0298(8) 0.0518(10) 0.0027(7) -0.0039(8) 0.0129(7) O6 0.0465(10) 0.0591(11) 0.0257(8) 0.0154(7) 0.0128(7) 0.0244(9) O1W 0.0513(11) 0.0345(9) 0.0591(12) -0.0030(8) 0.0024(9) 0.0155(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 Cd1 O1 2.1937(15) . ? Cd1 O3 2.2620(15) 2_676 ? Cd1 N2 2.3177(17) . ? Cd1 N1 2.3607(18) . ? Cd1 N3 2.3764(18) . ? Cd1 O5 2.4274(17) . ? As1 O1 1.6534(16) . ? As1 O3 1.6561(15) . ? As1 O2 1.7321(16) . ? As1 C1 1.936(2) . ? S1 O6 1.4429(16) . ? S1 O5 1.4563(17) . ? S1 O4 1.4588(16) . ? S1 C2 1.785(2) . ? N1 C7 1.338(3) . ? N1 C11 1.345(3) . ? N2 C12 1.339(2) . ? N2 C16 1.341(3) . ? N3 C17 1.338(3) . ? N3 C21 1.338(3) . ? C1 C6 1.390(3) . ? C1 C2 1.408(3) . ? C2 C3 1.386(3) . ? C3 C4 1.390(3) . ? C3 H3A 0.9300 . ? C4 C5 1.374(4) . ? C4 H4A 0.9300 . ? C5 C6 1.385(3) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.379(3) . ? C7 H7A 0.9300 . ? C8 C9 1.377(4) . ? C8 H8A 0.9300 . ? C9 C10 1.378(3) . ? C9 H9A 0.9300 . ? C10 C11 1.391(3) . ? C10 H10A 0.9300 . ? C11 C12 1.496(3) . ? C12 C13 1.384(3) . ? C13 C14 1.386(3) . ? C13 H13A 0.9300 . ? C14 C15 1.380(3) . ? C14 H14A 0.9300 . ? C15 C16 1.388(3) . ? C15 H15A 0.9300 . ? C16 C17 1.500(3) . ? C17 C18 1.385(3) . ? C18 C19 1.384(3) . ? C18 H18A 0.9300 . ? C19 C20 1.374(3) . ? C19 H19A 0.9300 . ? C20 C21 1.385(3) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? O2 H2A 0.8200 . ? O3 Cd1 2.2620(15) 2_676 ? O1W H1WB 0.8501 . ? O1W H1WA 0.8500 . ? 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 Cd1 O3 91.56(6) . 2_676 ? O1 Cd1 N2 157.75(6) . . ? O3 Cd1 N2 97.80(6) 2_676 . ? O1 Cd1 N1 131.00(6) . . ? O3 Cd1 N1 85.94(6) 2_676 . ? N2 Cd1 N1 70.09(6) . . ? O1 Cd1 N3 89.05(6) . . ? O3 Cd1 N3 98.48(6) 2_676 . ? N2 Cd1 N3 69.68(6) . . ? N1 Cd1 N3 139.75(6) . . ? O1 Cd1 O5 83.83(7) . . ? O3 Cd1 O5 163.76(6) 2_676 . ? N2 Cd1 O5 92.12(6) . . ? N1 Cd1 O5 85.41(6) . . ? N3 Cd1 O5 97.00(6) . . ? O1 As1 O3 115.03(8) . . ? O1 As1 O2 109.58(9) . . ? O3 As1 O2 103.21(7) . . ? O1 As1 C1 112.51(8) . . ? O3 As1 C1 108.30(8) . . ? O2 As1 C1 107.58(8) . . ? O6 S1 O5 113.11(11) . . ? O6 S1 O4 113.14(10) . . ? O5 S1 O4 111.35(11) . . ? O6 S1 C2 106.81(10) . . ? O5 S1 C2 105.41(9) . . ? O4 S1 C2 106.36(10) . . ? C7 N1 C11 118.07(18) . . ? C7 N1 Cd1 124.29(14) . . ? C11 N1 Cd1 117.64(13) . . ? C12 N2 C16 120.24(17) . . ? C12 N2 Cd1 119.50(13) . . ? C16 N2 Cd1 120.05(12) . . ? C17 N3 C21 118.70(18) . . ? C17 N3 Cd1 117.85(13) . . ? C21 N3 Cd1 123.41(14) . . ? C6 C1 C2 118.99(18) . . ? C6 C1 As1 114.17(15) . . ? C2 C1 As1 126.84(15) . . ? C3 C2 C1 119.21(19) . . ? C3 C2 S1 117.57(16) . . ? C1 C2 S1 123.19(15) . . ? C2 C3 C4 120.8(2) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C5 C4 C3 119.9(2) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 119.9(2) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C5 C6 C1 121.0(2) . . ? C5 C6 H6A 119.5 . . ? C1 C6 H6A 119.5 . . ? N1 C7 C8 123.4(2) . . ? N1 C7 H7A 118.3 . . ? C8 C7 H7A 118.3 . . ? C9 C8 C7 118.4(2) . . ? C9 C8 H8A 120.8 . . ? C7 C8 H8A 120.8 . . ? C8 C9 C10 119.1(2) . . ? C8 C9 H9A 120.5 . . ? C10 C9 H9A 120.5 . . ? C9 C10 C11 119.4(2) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? N1 C11 C10 121.58(19) . . ? N1 C11 C12 116.44(17) . . ? C10 C11 C12 121.97(18) . . ? N2 C12 C13 121.36(19) . . ? N2 C12 C11 116.12(17) . . ? C13 C12 C11 122.52(18) . . ? C12 C13 C14 118.5(2) . . ? C12 C13 H13A 120.7 . . ? C14 C13 H13A 120.7 . . ? C15 C14 C13 120.0(2) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C16 118.4(2) . . ? C14 C15 H15A 120.8 . . ? C16 C15 H15A 120.8 . . ? N2 C16 C15 121.35(18) . . ? N2 C16 C17 115.96(17) . . ? C15 C16 C17 122.66(18) . . ? N3 C17 C18 121.76(18) . . ? N3 C17 C16 116.40(17) . . ? C18 C17 C16 121.84(18) . . ? C19 C18 C17 118.9(2) . . ? C19 C18 H18A 120.6 . . ? C17 C18 H18A 120.6 . . ? C20 C19 C18 119.7(2) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C19 C20 C21 118.0(2) . . ? C19 C20 H20A 121.0 . . ? C21 C20 H20A 121.0 . . ? N3 C21 C20 123.0(2) . . ? N3 C21 H21A 118.5 . . ? C20 C21 H21A 118.5 . . ? As1 O1 Cd1 126.27(8) . . ? As1 O2 H2A 109.5 . . ? As1 O3 Cd1 128.98(7) . 2_676 ? S1 O5 Cd1 141.25(10) . . ? H1WB O1W H1WA 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2A O4 0.82 1.91 2.711(2) 163.6 . O1W H1WB O3 0.85 1.98 2.835(2) 179.8 . O1W H1WA O4 0.85 2.29 2.913(2) 130.7 2_686 _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.510 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.061 #===end data_10 _database_code_depnum_ccdc_archive 'CCDC 763191' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H13 As N2 O6 S Zn' _chemical_formula_weight 501.63 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' 'S' 'S' 0.1246 0.1234 '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)/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 14.0169(11) _cell_length_b 8.0918(5) _cell_length_c 15.4783(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.599(6) _cell_angle_gamma 90.00 _cell_volume 1752.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4543 _cell_measurement_theta_min 3.1544 _cell_measurement_theta_max 27.4797 _exptl_crystal_description 'brick' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.902 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 3.433 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.6052 _exptl_absorpt_correction_T_max 1 _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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13039 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3998 _reflns_number_gt 3483 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0365P)^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 shelxtl _refine_ls_extinction_coef ? _refine_ls_number_reflns 3998 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.71655(2) 0.69373(4) 0.612737(19) 0.02365(10) Uani 1 1 d . . . As1 As 0.814018(18) 1.05030(3) 0.690664(17) 0.02244(9) Uani 1 1 d . . . S1 S 0.93775(5) 0.68806(8) 0.66774(5) 0.02555(16) Uani 1 1 d . . . N1 N 0.68882(15) 0.5966(3) 0.48761(14) 0.0275(5) Uani 1 1 d . . . N2 N 0.57005(16) 0.7619(3) 0.58142(15) 0.0297(5) Uani 1 1 d . . . C1 C 0.94124(18) 1.0315(3) 0.65029(16) 0.0237(6) Uani 1 1 d . . . C2 C 0.98658(17) 0.8812(3) 0.63641(16) 0.0240(6) Uani 1 1 d . . . C3 C 1.07327(19) 0.8813(4) 0.59705(19) 0.0350(7) Uani 1 1 d . . . H3A H 1.1034 0.7817 0.5861 0.042 Uiso 1 1 calc R . . C4 C 1.1147(2) 1.0281(4) 0.5742(2) 0.0418(8) Uani 1 1 d . . . H4A H 1.1721 1.0269 0.5473 0.050 Uiso 1 1 calc R . . C5 C 1.0719(2) 1.1752(4) 0.5909(2) 0.0413(8) Uani 1 1 d . . . H5A H 1.1012 1.2739 0.5769 0.050 Uiso 1 1 calc R . . C6 C 0.9850(2) 1.1779(4) 0.62870(18) 0.0323(7) Uani 1 1 d . . . H6A H 0.9558 1.2784 0.6396 0.039 Uiso 1 1 calc R . . C7 C 0.7523(2) 0.5134(4) 0.44380(19) 0.0329(7) Uani 1 1 d . . . H7A H 0.8120 0.4909 0.4710 0.040 Uiso 1 1 calc R . . C8 C 0.7334(2) 0.4595(4) 0.3601(2) 0.0449(8) Uani 1 1 d . . . H8A H 0.7794 0.4027 0.3311 0.054 Uiso 1 1 calc R . . C9 C 0.6442(3) 0.4919(5) 0.3202(2) 0.0537(10) Uani 1 1 d . . . H9A H 0.6294 0.4578 0.2636 0.064 Uiso 1 1 calc R . . C10 C 0.5775(2) 0.5755(4) 0.3657(2) 0.0442(8) Uani 1 1 d . . . H10A H 0.5168 0.5964 0.3403 0.053 Uiso 1 1 calc R . . C11 C 0.60174(19) 0.6277(4) 0.44914(18) 0.0298(6) Uani 1 1 d . . . C12 C 0.53514(19) 0.7212(4) 0.50197(19) 0.0301(6) Uani 1 1 d . . . C13 C 0.4440(2) 0.7677(5) 0.4715(2) 0.0437(8) Uani 1 1 d . . . H13A H 0.4205 0.7377 0.4162 0.052 Uiso 1 1 calc R . . C14 C 0.3889(2) 0.8589(5) 0.5244(2) 0.0494(9) Uani 1 1 d . . . H14A H 0.3276 0.8914 0.5052 0.059 Uiso 1 1 calc R . . C15 C 0.4251(2) 0.9015(5) 0.6059(2) 0.0478(8) Uani 1 1 d . . . H15A H 0.3888 0.9631 0.6426 0.057 Uiso 1 1 calc R . . C16 C 0.5168(2) 0.8510(4) 0.6324(2) 0.0385(7) Uani 1 1 d . . . H16A H 0.5419 0.8801 0.6873 0.046 Uiso 1 1 calc R . . O1 O 0.73846(13) 0.9282(2) 0.63511(13) 0.0345(5) Uani 1 1 d . . . O2 O 0.80952(14) 1.0343(2) 0.79724(12) 0.0318(5) Uani 1 1 d . . . O3 O 0.78992(15) 1.2490(2) 0.65611(15) 0.0411(5) Uani 1 1 d . . . H3B H 0.7386 1.2790 0.6735 0.062 Uiso 1 1 calc R . . O4 O 0.86411(13) 0.6451(2) 0.59938(12) 0.0298(4) Uani 1 1 d . . . O5 O 1.01619(14) 0.5731(3) 0.67277(16) 0.0448(6) Uani 1 1 d . . . O6 O 0.89596(14) 0.7220(2) 0.74945(12) 0.0323(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02355(17) 0.02549(18) 0.02131(17) 0.00017(12) -0.00328(12) -0.00425(12) As1 0.02141(15) 0.02109(16) 0.02473(15) -0.00380(11) 0.00082(10) -0.00208(10) S1 0.0218(3) 0.0225(3) 0.0317(4) -0.0013(3) -0.0037(3) 0.0004(3) N1 0.0271(12) 0.0297(13) 0.0243(12) 0.0004(10) -0.0079(9) -0.0043(10) N2 0.0268(12) 0.0282(13) 0.0333(13) 0.0024(11) -0.0051(10) -0.0028(10) C1 0.0259(13) 0.0249(14) 0.0202(13) -0.0030(11) 0.0002(10) -0.0049(11) C2 0.0211(12) 0.0281(15) 0.0222(13) -0.0002(11) -0.0028(10) -0.0025(11) C3 0.0248(14) 0.0440(18) 0.0363(17) -0.0048(15) 0.0019(12) 0.0041(14) C4 0.0248(15) 0.064(2) 0.0377(18) 0.0044(16) 0.0089(12) -0.0088(15) C5 0.0376(17) 0.048(2) 0.0391(18) 0.0108(15) 0.0080(14) -0.0160(15) C6 0.0348(16) 0.0319(16) 0.0301(16) -0.0001(13) 0.0018(12) -0.0076(13) C7 0.0305(15) 0.0349(16) 0.0328(16) -0.0052(13) -0.0037(12) -0.0024(13) C8 0.047(2) 0.052(2) 0.0358(19) -0.0100(16) -0.0002(14) 0.0055(16) C9 0.065(2) 0.065(2) 0.0292(18) -0.0122(17) -0.0174(15) 0.011(2) C10 0.0451(19) 0.052(2) 0.0325(17) -0.0030(15) -0.0183(14) 0.0025(16) C11 0.0285(14) 0.0290(15) 0.0307(15) 0.0039(12) -0.0077(11) -0.0080(12) C12 0.0253(14) 0.0308(16) 0.0327(16) 0.0097(13) -0.0089(11) -0.0065(12) C13 0.0336(17) 0.058(2) 0.0379(19) 0.0083(16) -0.0112(13) -0.0001(16) C14 0.0273(16) 0.061(2) 0.059(2) 0.0147(19) -0.0033(15) 0.0084(16) C15 0.0352(18) 0.049(2) 0.060(2) 0.0030(18) 0.0064(15) 0.0075(16) C16 0.0353(17) 0.0403(19) 0.0394(18) -0.0039(15) -0.0014(13) -0.0014(14) O1 0.0271(10) 0.0298(11) 0.0450(13) -0.0101(9) -0.0112(9) -0.0030(9) O2 0.0383(11) 0.0344(12) 0.0231(10) -0.0044(9) 0.0046(8) 0.0050(9) O3 0.0443(13) 0.0271(11) 0.0536(14) 0.0051(11) 0.0161(10) 0.0083(10) O4 0.0241(10) 0.0343(11) 0.0305(11) -0.0069(9) -0.0026(8) -0.0043(8) O5 0.0284(11) 0.0312(12) 0.0738(17) -0.0017(11) -0.0046(10) 0.0089(9) O6 0.0368(11) 0.0321(11) 0.0278(11) 0.0005(9) 0.0009(8) -0.0079(9) _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 1.950(2) . ? Zn1 O2 1.9502(19) 2_646 ? Zn1 N1 2.104(2) . ? Zn1 O4 2.1281(18) . ? Zn1 N2 2.152(2) . ? As1 O1 1.6500(18) . ? As1 O2 1.6597(19) . ? As1 O3 1.721(2) . ? As1 C1 1.932(3) . ? S1 O5 1.438(2) . ? S1 O6 1.453(2) . ? S1 O4 1.4725(19) . ? S1 C2 1.786(3) . ? N1 C7 1.334(4) . ? N1 C11 1.348(3) . ? N2 C16 1.332(4) . ? N2 C12 1.336(4) . ? C1 C6 1.384(4) . ? C1 C2 1.395(4) . ? C2 C3 1.393(4) . ? C3 C4 1.378(4) . ? C3 H3A 0.9300 . ? C4 C5 1.365(4) . ? C4 H4A 0.9300 . ? C5 C6 1.384(4) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.377(4) . ? C7 H7A 0.9300 . ? C8 C9 1.384(5) . ? C8 H8A 0.9300 . ? C9 C10 1.382(5) . ? C9 H9A 0.9300 . ? C10 C11 1.381(4) . ? C10 H10A 0.9300 . ? C11 C12 1.486(4) . ? C12 C13 1.386(4) . ? C13 C14 1.375(5) . ? C13 H13A 0.9300 . ? C14 C15 1.374(5) . ? C14 H14A 0.9300 . ? C15 C16 1.386(4) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? O2 Zn1 1.9502(19) 2_656 ? O3 H3B 0.8200 . ? 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 O2 123.46(9) . 2_646 ? O1 Zn1 N1 123.03(9) . . ? O2 Zn1 N1 112.25(9) 2_646 . ? O1 Zn1 O4 93.09(8) . . ? O2 Zn1 O4 100.03(8) 2_646 . ? N1 Zn1 O4 88.05(8) . . ? O1 Zn1 N2 85.87(9) . . ? O2 Zn1 N2 96.40(9) 2_646 . ? N1 Zn1 N2 76.69(9) . . ? O4 Zn1 N2 160.90(8) . . ? O1 As1 O2 114.09(10) . . ? O1 As1 O3 106.88(10) . . ? O2 As1 O3 111.26(10) . . ? O1 As1 C1 111.07(10) . . ? O2 As1 C1 114.12(10) . . ? O3 As1 C1 98.06(11) . . ? O5 S1 O6 115.05(14) . . ? O5 S1 O4 112.66(13) . . ? O6 S1 O4 111.55(11) . . ? O5 S1 C2 106.02(13) . . ? O6 S1 C2 104.68(12) . . ? O4 S1 C2 105.95(12) . . ? C7 N1 C11 119.0(2) . . ? C7 N1 Zn1 124.45(18) . . ? C11 N1 Zn1 116.53(19) . . ? C16 N2 C12 119.5(3) . . ? C16 N2 Zn1 124.6(2) . . ? C12 N2 Zn1 115.69(19) . . ? C6 C1 C2 119.7(3) . . ? C6 C1 As1 116.2(2) . . ? C2 C1 As1 123.86(19) . . ? C3 C2 C1 119.1(3) . . ? C3 C2 S1 118.6(2) . . ? C1 C2 S1 122.35(19) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C1 120.2(3) . . ? C5 C6 H6A 119.9 . . ? C1 C6 H6A 119.9 . . ? N1 C7 C8 122.9(3) . . ? N1 C7 H7A 118.6 . . ? C8 C7 H7A 118.6 . . ? C7 C8 C9 118.3(3) . . ? C7 C8 H8A 120.8 . . ? C9 C8 H8A 120.8 . . ? C10 C9 C8 119.1(3) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? C11 C10 C9 119.4(3) . . ? C11 C10 H10A 120.3 . . ? C9 C10 H10A 120.3 . . ? N1 C11 C10 121.3(3) . . ? N1 C11 C12 115.8(2) . . ? C10 C11 C12 123.0(3) . . ? N2 C12 C13 121.5(3) . . ? N2 C12 C11 115.2(2) . . ? C13 C12 C11 123.3(3) . . ? C14 C13 C12 118.9(3) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C15 C14 C13 119.6(3) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C16 118.6(3) . . ? C14 C15 H15A 120.7 . . ? C16 C15 H15A 120.7 . . ? N2 C16 C15 121.9(3) . . ? N2 C16 H16A 119.0 . . ? C15 C16 H16A 119.0 . . ? As1 O1 Zn1 139.81(12) . . ? As1 O2 Zn1 132.78(12) . 2_656 ? As1 O3 H3B 109.5 . . ? S1 O4 Zn1 121.89(11) . . ? 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 O3 H3B O2 0.82 2.23 2.814(3) 128.6 2_656 O3 H3B O6 0.82 2.34 3.074(3) 149.4 2_656 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.491 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.083 #===end data_11 _database_code_depnum_ccdc_archive 'CCDC 763192' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H17 As N2 O8 S Zn' _chemical_formula_weight 537.70 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' 'As' 'As' 0.0499 2.0058 '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' 'S' 'S' 0.1246 0.1234 '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 'orthorhombic' _symmetry_space_group_name_H-M 'Pna2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 17.880(3) _cell_length_b 10.4331(17) _cell_length_c 21.170(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3949.1(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9829 _cell_measurement_theta_min 2.1756 _cell_measurement_theta_max 27.4835 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 3.060 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.8453 _exptl_absorpt_correction_T_max 1 _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 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29938 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8966 _reflns_number_gt 8236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0260P)^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 shelxtl _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(6) _refine_ls_number_reflns 8966 _refine_ls_number_parameters 523 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 -0.47638(2) 0.31638(4) -0.453995(19) 0.02818(9) Uani 1 1 d . . . Zn2 Zn -0.63992(2) 0.79166(3) -0.477407(18) 0.02640(9) Uani 1 1 d . . . As1 As -0.632692(17) 0.48327(3) -0.490512(15) 0.02485(8) Uani 1 1 d . . . As2 As -0.532622(18) 0.03903(3) -0.509628(15) 0.02517(8) Uani 1 1 d . . . S1 S -0.56089(5) 0.42950(9) -0.34227(4) 0.0336(2) Uani 1 1 d . . . S2 S -0.61287(5) -0.12607(10) -0.63675(4) 0.0351(2) Uani 1 1 d . . . N1 N -0.40823(17) 0.3751(3) -0.52992(14) 0.0326(7) Uani 1 1 d . . . N2 N -0.37440(17) 0.3499(3) -0.40880(14) 0.0303(6) Uani 1 1 d . . . N3 N -0.66605(16) 0.7833(3) -0.37887(13) 0.0304(6) Uani 1 1 d . . . N4 N -0.75726(15) 0.7929(3) -0.47676(15) 0.0322(6) Uani 1 1 d . . . C1 C -0.68987(19) 0.4642(3) -0.41399(16) 0.0274(7) Uani 1 1 d . . . C2 C -0.6589(2) 0.4465(3) -0.35389(16) 0.0300(8) Uani 1 1 d . . . C3 C -0.7058(2) 0.4397(4) -0.30144(19) 0.0422(9) Uani 1 1 d . . . H3A H -0.6856 0.4273 -0.2614 0.051 Uiso 1 1 calc R . . C4 C -0.7828(2) 0.4512(4) -0.3090(2) 0.0512(11) Uani 1 1 d . . . H4A H -0.8139 0.4482 -0.2739 0.061 Uiso 1 1 calc R . . C5 C -0.8128(2) 0.4671(4) -0.3679(2) 0.0451(10) Uani 1 1 d . . . H5A H -0.8644 0.4736 -0.3726 0.054 Uiso 1 1 calc R . . C6 C -0.7669(2) 0.4735(3) -0.4208(2) 0.0363(8) Uani 1 1 d . . . H6A H -0.7878 0.4840 -0.4607 0.044 Uiso 1 1 calc R . . C7 C -0.48202(19) -0.0290(3) -0.58262(16) 0.0306(8) Uani 1 1 d . . . C8 C -0.5145(2) -0.1044(4) -0.62986(17) 0.0331(8) Uani 1 1 d . . . C9 C -0.4706(2) -0.1532(4) -0.67877(19) 0.0479(11) Uani 1 1 d . . . H9A H -0.4920 -0.2034 -0.7103 0.057 Uiso 1 1 calc R . . C10 C -0.3940(3) -0.1257(5) -0.6799(2) 0.0609(14) Uani 1 1 d . . . H10A H -0.3641 -0.1613 -0.7112 0.073 Uiso 1 1 calc R . . C11 C -0.3626(2) -0.0470(5) -0.6354(2) 0.0529(12) Uani 1 1 d . . . H11A H -0.3123 -0.0251 -0.6383 0.064 Uiso 1 1 calc R . . C12 C -0.4055(2) -0.0001(4) -0.58633(19) 0.0390(9) Uani 1 1 d . . . H12A H -0.3834 0.0511 -0.5555 0.047 Uiso 1 1 calc R . . C13 C -0.4313(2) 0.3942(4) -0.58934(18) 0.0454(10) Uani 1 1 d . . . H13A H -0.4822 0.3922 -0.5982 0.055 Uiso 1 1 calc R . . C14 C -0.3812(3) 0.4168(5) -0.6381(2) 0.0531(11) Uani 1 1 d . . . H14A H -0.3980 0.4320 -0.6790 0.064 Uiso 1 1 calc R . . C15 C -0.3057(2) 0.4162(5) -0.62437(19) 0.0491(11) Uani 1 1 d . . . H15A H -0.2709 0.4294 -0.6564 0.059 Uiso 1 1 calc R . . C16 C -0.2821(2) 0.3961(4) -0.56387(19) 0.0418(9) Uani 1 1 d . . . H16A H -0.2313 0.3941 -0.5545 0.050 Uiso 1 1 calc R . . C17 C -0.33505(19) 0.3786(3) -0.51604(17) 0.0299(8) Uani 1 1 d . . . C18 C -0.3158(2) 0.3686(3) -0.44762(18) 0.0302(7) Uani 1 1 d . . . C19 C -0.2444(2) 0.3820(4) -0.4246(2) 0.0409(9) Uani 1 1 d . . . H19A H -0.2044 0.3916 -0.4523 0.049 Uiso 1 1 calc R . . C20 C -0.2321(2) 0.3813(4) -0.3606(2) 0.0464(10) Uani 1 1 d . . . H20A H -0.1840 0.3912 -0.3446 0.056 Uiso 1 1 calc R . . C21 C -0.2922(2) 0.3658(4) -0.3201(2) 0.0497(11) Uani 1 1 d . . . H21A H -0.2854 0.3667 -0.2766 0.060 Uiso 1 1 calc R . . C22 C -0.3624(2) 0.3489(4) -0.34572(18) 0.0391(9) Uani 1 1 d . . . H22A H -0.4028 0.3365 -0.3187 0.047 Uiso 1 1 calc R . . C23 C -0.6162(2) 0.7831(4) -0.33188(19) 0.0399(9) Uani 1 1 d . . . H23A H -0.5658 0.7745 -0.3419 0.048 Uiso 1 1 calc R . . C24 C -0.6360(3) 0.7950(4) -0.26908(19) 0.0497(11) Uani 1 1 d . . . H24A H -0.5998 0.7956 -0.2375 0.060 Uiso 1 1 calc R . . C25 C -0.7105(3) 0.8059(4) -0.2544(2) 0.0560(12) Uani 1 1 d . . . H25A H -0.7256 0.8152 -0.2126 0.067 Uiso 1 1 calc R . . C26 C -0.7634(3) 0.8027(4) -0.3030(2) 0.0502(11) Uani 1 1 d . . . H26A H -0.8142 0.8069 -0.2938 0.060 Uiso 1 1 calc R . . C27 C -0.7392(2) 0.7931(3) -0.36458(17) 0.0320(8) Uani 1 1 d . . . C28 C -0.7903(2) 0.7957(3) -0.42012(18) 0.0313(8) Uani 1 1 d . . . C29 C -0.8675(2) 0.8019(4) -0.4137(2) 0.0457(10) Uani 1 1 d . . . H29A H -0.8894 0.8042 -0.3738 0.055 Uiso 1 1 calc R . . C30 C -0.9112(2) 0.8046(4) -0.4674(2) 0.0494(11) Uani 1 1 d . . . H30A H -0.9629 0.8110 -0.4642 0.059 Uiso 1 1 calc R . . C31 C -0.8774(2) 0.7979(4) -0.5257(2) 0.0470(11) Uani 1 1 d . . . H31A H -0.9061 0.7969 -0.5624 0.056 Uiso 1 1 calc R . . C32 C -0.8005(2) 0.7925(4) -0.5292(2) 0.0397(9) Uani 1 1 d . . . H32A H -0.7777 0.7884 -0.5686 0.048 Uiso 1 1 calc R . . O1 O -0.56886(12) 0.3678(2) -0.50059(10) 0.0294(5) Uani 1 1 d . . . O2 O -0.70132(15) 0.4540(3) -0.54506(13) 0.0431(7) Uani 1 1 d . . . H2A H -0.6860 0.4726 -0.5804 0.065 Uiso 1 1 d R . . O3 O -0.59679(13) 0.6281(2) -0.50173(12) 0.0341(6) Uani 1 1 d . . . O4 O -0.52604(15) 0.5272(3) -0.38109(14) 0.0489(7) Uani 1 1 d . . . O5 O -0.54028(15) 0.3025(2) -0.36662(13) 0.0437(7) Uani 1 1 d . . . O6 O -0.54784(17) 0.4418(3) -0.27541(12) 0.0523(7) Uani 1 1 d . . . O7 O -0.47181(12) 0.1298(2) -0.47062(12) 0.0320(6) Uani 1 1 d . . . O8 O -0.56582(14) -0.0718(2) -0.46071(11) 0.0341(6) Uani 1 1 d . . . O9 O -0.60464(13) 0.1344(2) -0.53600(13) 0.0386(6) Uani 1 1 d . . . H9B H -0.5964 0.2091 -0.5262 0.058 Uiso 1 1 d R . . O10 O -0.62468(19) -0.2417(3) -0.67205(16) 0.0644(9) Uani 1 1 d . . . O11 O -0.63903(15) -0.0135(3) -0.66926(12) 0.0470(7) Uani 1 1 d . . . O12 O -0.64217(14) -0.1309(2) -0.57231(11) 0.0359(6) Uani 1 1 d . . . O1W O -0.6652(2) 0.5054(3) -0.66044(15) 0.0657(9) Uani 1 1 d . . . H1WA H -0.6277 0.4602 -0.6710 0.099 Uiso 1 1 d R . . H1WB H -0.6542 0.5844 -0.6635 0.099 Uiso 1 1 d R . . O2W O -0.5245(2) 0.0322(3) -0.33501(15) 0.0758(12) Uani 1 1 d . . . H2WA H -0.5066 0.0431 -0.3718 0.114 Uiso 1 1 d R . . H2WB H -0.5529 0.0948 -0.3258 0.114 Uiso 1 1 d R . . O3W O -0.5524(3) 0.1325(3) -0.7552(2) 0.0989(15) Uani 1 1 d . . . H3WA H -0.5387 0.0852 -0.7858 0.148 Uiso 1 1 d R . . H3WB H -0.5786 0.0888 -0.7296 0.148 Uiso 1 1 d R . . O4W O -0.5590(2) 0.3826(4) -0.7283(2) 0.1134(18) Uani 1 1 d . . . H4WA H -0.5700 0.3036 -0.7313 0.170 Uiso 1 1 d R . . H4WB H -0.5568 0.4154 -0.7650 0.170 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02603(19) 0.02622(19) 0.03229(19) -0.00203(17) -0.00011(17) -0.00331(16) Zn2 0.02513(18) 0.02238(18) 0.03169(19) -0.00059(16) 0.00199(16) -0.00092(15) As1 0.02373(16) 0.02271(16) 0.02810(16) -0.00012(14) 0.00104(14) 0.00160(13) As2 0.02342(16) 0.02153(16) 0.03055(17) -0.00144(14) -0.00024(14) -0.00137(13) S1 0.0341(5) 0.0380(5) 0.0289(4) -0.0032(4) -0.0003(4) 0.0020(4) S2 0.0344(5) 0.0414(5) 0.0294(4) -0.0014(4) -0.0028(4) -0.0043(4) N1 0.0301(16) 0.0342(17) 0.0336(16) 0.0036(13) 0.0000(13) -0.0034(13) N2 0.0328(17) 0.0265(15) 0.0315(15) 0.0006(12) -0.0028(13) -0.0031(13) N3 0.0348(16) 0.0256(15) 0.0307(15) -0.0014(12) 0.0048(13) -0.0017(13) N4 0.0277(14) 0.0280(14) 0.0409(16) -0.0006(13) -0.0006(14) -0.0038(12) C1 0.0263(17) 0.0212(16) 0.0348(18) -0.0006(15) 0.0046(14) -0.0032(14) C2 0.0345(19) 0.0247(17) 0.0308(17) -0.0018(14) 0.0070(15) -0.0023(15) C3 0.047(2) 0.045(2) 0.0349(19) -0.0019(18) 0.0119(18) -0.0022(19) C4 0.048(3) 0.051(3) 0.054(3) -0.001(2) 0.025(2) -0.002(2) C5 0.030(2) 0.049(2) 0.056(3) -0.002(2) 0.0124(18) -0.0019(18) C6 0.033(2) 0.0290(19) 0.047(2) 0.0011(16) 0.0026(17) -0.0018(16) C7 0.0290(19) 0.035(2) 0.0276(17) 0.0026(15) 0.0001(14) 0.0066(15) C8 0.0330(19) 0.037(2) 0.0299(17) 0.0027(16) 0.0014(15) 0.0057(16) C9 0.049(3) 0.063(3) 0.031(2) -0.0059(19) 0.0027(18) 0.006(2) C10 0.048(3) 0.088(4) 0.047(3) -0.006(3) 0.018(2) 0.017(3) C11 0.030(2) 0.074(3) 0.055(3) 0.008(3) 0.013(2) 0.007(2) C12 0.030(2) 0.047(2) 0.040(2) 0.0084(18) 0.0043(17) 0.0010(17) C13 0.033(2) 0.062(3) 0.041(2) 0.007(2) 0.0002(17) -0.005(2) C14 0.052(3) 0.074(3) 0.033(2) 0.005(2) 0.0010(19) -0.011(2) C15 0.041(2) 0.069(3) 0.038(2) 0.001(2) 0.0113(18) -0.012(2) C16 0.028(2) 0.051(2) 0.047(2) -0.0036(19) 0.0059(17) -0.0024(18) C17 0.0261(17) 0.0280(17) 0.0356(19) 0.0010(15) -0.0004(16) -0.0051(14) C18 0.0302(18) 0.0207(16) 0.0398(18) -0.0017(16) -0.0017(16) 0.0000(14) C19 0.028(2) 0.043(2) 0.052(2) -0.0009(19) -0.0023(18) 0.0035(17) C20 0.033(2) 0.049(2) 0.057(3) -0.005(2) -0.0130(19) 0.0004(19) C21 0.047(3) 0.054(3) 0.048(2) -0.001(2) -0.012(2) 0.000(2) C22 0.043(2) 0.041(2) 0.0339(19) -0.0016(17) -0.0032(17) 0.0018(18) C23 0.039(2) 0.037(2) 0.043(2) -0.0039(18) -0.0004(17) -0.0018(17) C24 0.060(3) 0.057(3) 0.0314(19) -0.0004(19) -0.0032(19) -0.006(2) C25 0.077(3) 0.057(3) 0.034(2) 0.000(2) 0.011(2) 0.001(2) C26 0.051(3) 0.055(3) 0.045(2) 0.003(2) 0.016(2) 0.000(2) C27 0.0326(19) 0.0250(18) 0.0383(19) -0.0001(15) 0.0088(16) 0.0017(15) C28 0.0278(19) 0.0225(18) 0.043(2) -0.0007(16) 0.0047(15) 0.0008(15) C29 0.033(2) 0.047(2) 0.057(3) -0.001(2) 0.0110(19) 0.0003(19) C30 0.0286(19) 0.041(2) 0.078(3) 0.000(2) -0.001(2) -0.0001(17) C31 0.033(2) 0.046(3) 0.062(3) -0.002(2) -0.013(2) -0.0023(18) C32 0.035(2) 0.035(2) 0.049(2) -0.0007(17) -0.0033(18) -0.0017(17) O1 0.0294(12) 0.0261(11) 0.0327(13) -0.0030(11) -0.0021(10) 0.0054(9) O2 0.0336(14) 0.0559(18) 0.0397(14) -0.0056(13) -0.0063(12) 0.0022(13) O3 0.0359(13) 0.0225(11) 0.0440(15) 0.0025(11) 0.0103(11) 0.0009(10) O4 0.0344(15) 0.0515(17) 0.0609(18) 0.0133(14) 0.0073(14) -0.0067(13) O5 0.0479(16) 0.0372(15) 0.0460(15) -0.0020(13) 0.0028(13) 0.0086(13) O6 0.0539(18) 0.074(2) 0.0290(13) -0.0121(14) -0.0045(12) -0.0010(16) O7 0.0267(12) 0.0243(11) 0.0452(15) -0.0027(11) -0.0075(11) -0.0017(9) O8 0.0414(14) 0.0328(13) 0.0281(12) -0.0024(11) -0.0018(11) -0.0120(11) O9 0.0254(13) 0.0258(13) 0.0647(18) -0.0068(12) -0.0099(12) 0.0020(10) O10 0.066(2) 0.066(2) 0.061(2) -0.0279(18) -0.0036(17) -0.0187(18) O11 0.0381(16) 0.0675(19) 0.0356(14) 0.0182(14) -0.0050(12) 0.0026(14) O12 0.0339(13) 0.0453(15) 0.0285(12) 0.0104(12) -0.0008(10) -0.0024(12) O1W 0.075(2) 0.071(2) 0.0509(19) -0.0055(17) 0.0128(17) -0.0114(18) O2W 0.128(4) 0.056(2) 0.0437(18) 0.0089(16) -0.006(2) -0.011(2) O3W 0.116(3) 0.054(2) 0.127(4) 0.002(2) 0.070(3) -0.010(2) O4W 0.106(4) 0.065(3) 0.170(5) 0.002(3) 0.075(4) -0.011(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 O7 1.980(2) . ? Zn1 O1 1.999(2) . ? Zn1 N2 2.089(3) . ? Zn1 N1 2.108(3) . ? Zn1 O5 2.179(3) . ? Zn2 O3 1.943(2) . ? Zn2 O8 1.977(2) 1_565 ? Zn2 N4 2.098(3) . ? Zn2 N3 2.139(3) . ? Zn2 O12 2.166(2) 1_565 ? As1 O3 1.658(2) . ? As1 O1 1.673(2) . ? As1 O2 1.712(3) . ? As1 C1 1.926(3) . ? As2 O7 1.661(2) . ? As2 O8 1.662(2) . ? As2 O9 1.720(2) . ? As2 C7 1.926(3) . ? S1 O6 1.440(3) . ? S1 O4 1.450(3) . ? S1 O5 1.468(3) . ? S1 C2 1.779(4) . ? S2 O10 1.435(3) . ? S2 O11 1.439(3) . ? S2 O12 1.462(3) . ? S2 C8 1.780(4) . ? N1 C13 1.338(5) . ? N1 C17 1.341(4) . ? N2 C18 1.345(5) . ? N2 C22 1.353(5) . ? N3 C23 1.336(5) . ? N3 C27 1.347(4) . ? N4 C28 1.337(5) . ? N4 C32 1.352(5) . ? C1 C6 1.389(5) . ? C1 C2 1.400(5) . ? C2 C3 1.393(5) . ? C3 C4 1.391(6) . ? C3 H3A 0.9300 . ? C4 C5 1.367(6) . ? C4 H4A 0.9300 . ? C5 C6 1.389(5) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.398(5) . ? C7 C12 1.404(5) . ? C8 C9 1.396(5) . ? C9 C10 1.398(6) . ? C9 H9A 0.9300 . ? C10 C11 1.370(7) . ? C10 H10A 0.9300 . ? C11 C12 1.380(6) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.387(6) . ? C13 H13A 0.9300 . ? C14 C15 1.381(6) . ? C14 H14A 0.9300 . ? C15 C16 1.365(6) . ? C15 H15A 0.9300 . ? C16 C17 1.399(5) . ? C16 H16A 0.9300 . ? C17 C18 1.492(5) . ? C18 C19 1.375(5) . ? C19 C20 1.373(6) . ? C19 H19A 0.9300 . ? C20 C21 1.383(6) . ? C20 H20A 0.9300 . ? C21 C22 1.378(6) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.382(5) . ? C23 H23A 0.9300 . ? C24 C25 1.371(6) . ? C24 H24A 0.9300 . ? C25 C26 1.397(7) . ? C25 H25A 0.9300 . ? C26 C27 1.378(5) . ? C26 H26A 0.9300 . ? C27 C28 1.488(5) . ? C28 C29 1.389(5) . ? C29 C30 1.379(6) . ? C29 H29A 0.9300 . ? C30 C31 1.377(6) . ? C30 H30A 0.9300 . ? C31 C32 1.378(6) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? O2 H2A 0.8199 . ? O8 Zn2 1.977(2) 1_545 ? O9 H9B 0.8201 . ? O12 Zn2 2.166(2) 1_545 ? O1W H1WA 0.8499 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8499 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8501 . ? 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 O7 Zn1 O1 102.15(9) . . ? O7 Zn1 N2 102.11(10) . . ? O1 Zn1 N2 154.61(10) . . ? O7 Zn1 N1 97.26(11) . . ? O1 Zn1 N1 91.37(11) . . ? N2 Zn1 N1 78.23(11) . . ? O7 Zn1 O5 96.16(10) . . ? O1 Zn1 O5 90.17(10) . . ? N2 Zn1 O5 94.59(11) . . ? N1 Zn1 O5 165.85(11) . . ? O3 Zn2 O8 114.48(10) . 1_565 ? O3 Zn2 N4 113.85(10) . . ? O8 Zn2 N4 131.63(11) 1_565 . ? O3 Zn2 N3 108.02(11) . . ? O8 Zn2 N3 90.08(10) 1_565 . ? N4 Zn2 N3 77.03(12) . . ? O3 Zn2 O12 95.12(10) . 1_565 ? O8 Zn2 O12 84.81(9) 1_565 1_565 ? N4 Zn2 O12 89.15(11) . 1_565 ? N3 Zn2 O12 156.30(10) . 1_565 ? O3 As1 O1 111.93(11) . . ? O3 As1 O2 110.06(13) . . ? O1 As1 O2 105.94(12) . . ? O3 As1 C1 114.83(13) . . ? O1 As1 C1 113.28(13) . . ? O2 As1 C1 99.70(14) . . ? O7 As2 O8 108.69(12) . . ? O7 As2 O9 108.76(11) . . ? O8 As2 O9 109.71(13) . . ? O7 As2 C7 107.53(14) . . ? O8 As2 C7 114.30(14) . . ? O9 As2 C7 107.71(14) . . ? O6 S1 O4 115.13(19) . . ? O6 S1 O5 112.64(18) . . ? O4 S1 O5 109.10(17) . . ? O6 S1 C2 106.65(17) . . ? O4 S1 C2 105.95(16) . . ? O5 S1 C2 106.78(16) . . ? O10 S2 O11 112.9(2) . . ? O10 S2 O12 113.84(19) . . ? O11 S2 O12 110.97(16) . . ? O10 S2 C8 107.17(19) . . ? O11 S2 C8 104.87(17) . . ? O12 S2 C8 106.38(16) . . ? C13 N1 C17 120.1(3) . . ? C13 N1 Zn1 125.6(3) . . ? C17 N1 Zn1 113.9(2) . . ? C18 N2 C22 118.7(3) . . ? C18 N2 Zn1 115.1(2) . . ? C22 N2 Zn1 126.2(3) . . ? C23 N3 C27 118.8(3) . . ? C23 N3 Zn2 125.5(3) . . ? C27 N3 Zn2 115.3(2) . . ? C28 N4 C32 118.9(3) . . ? C28 N4 Zn2 116.6(2) . . ? C32 N4 Zn2 124.5(3) . . ? C6 C1 C2 119.7(3) . . ? C6 C1 As1 115.6(3) . . ? C2 C1 As1 124.6(3) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 S1 118.5(3) . . ? C1 C2 S1 121.9(3) . . ? C4 C3 C2 119.9(4) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C5 C4 C3 120.3(4) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 120.6(4) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C1 C6 C5 119.9(4) . . ? C1 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C8 C7 C12 119.0(3) . . ? C8 C7 As2 125.9(3) . . ? C12 C7 As2 115.1(3) . . ? C9 C8 C7 120.2(4) . . ? C9 C8 S2 116.7(3) . . ? C7 C8 S2 122.7(3) . . ? C8 C9 C10 119.2(4) . . ? C8 C9 H9A 120.4 . . ? C10 C9 H9A 120.4 . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C12 120.2(4) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C11 C12 C7 120.5(4) . . ? C11 C12 H12A 119.8 . . ? C7 C12 H12A 119.8 . . ? N1 C13 C14 121.7(4) . . ? N1 C13 H13A 119.1 . . ? C14 C13 H13A 119.1 . . ? C15 C14 C13 118.3(4) . . ? C15 C14 H14A 120.8 . . ? C13 C14 H14A 120.8 . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 119.4(4) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? N1 C17 C16 120.4(3) . . ? N1 C17 C18 115.8(3) . . ? C16 C17 C18 123.8(3) . . ? N2 C18 C19 121.4(4) . . ? N2 C18 C17 115.1(3) . . ? C19 C18 C17 123.4(4) . . ? C20 C19 C18 119.8(4) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C19 C20 C21 119.2(4) . . ? C19 C20 H20A 120.4 . . ? C21 C20 H20A 120.4 . . ? C22 C21 C20 118.6(4) . . ? C22 C21 H21A 120.7 . . ? C20 C21 H21A 120.7 . . ? N2 C22 C21 122.2(4) . . ? N2 C22 H22A 118.9 . . ? C21 C22 H22A 118.9 . . ? N3 C23 C24 123.0(4) . . ? N3 C23 H23A 118.5 . . ? C24 C23 H23A 118.5 . . ? C25 C24 C23 118.3(4) . . ? C25 C24 H24A 120.8 . . ? C23 C24 H24A 120.8 . . ? C24 C25 C26 119.3(4) . . ? C24 C25 H25A 120.4 . . ? C26 C25 H25A 120.4 . . ? C27 C26 C25 119.1(4) . . ? C27 C26 H26A 120.5 . . ? C25 C26 H26A 120.5 . . ? N3 C27 C26 121.5(4) . . ? N3 C27 C28 114.8(3) . . ? C26 C27 C28 123.7(3) . . ? N4 C28 C29 121.9(4) . . ? N4 C28 C27 116.0(3) . . ? C29 C28 C27 122.2(3) . . ? C30 C29 C28 118.9(4) . . ? C30 C29 H29A 120.6 . . ? C28 C29 H29A 120.6 . . ? C31 C30 C29 119.3(3) . . ? C31 C30 H30A 120.3 . . ? C29 C30 H30A 120.3 . . ? C30 C31 C32 119.2(4) . . ? C30 C31 H31A 120.4 . . ? C32 C31 H31A 120.4 . . ? N4 C32 C31 121.8(4) . . ? N4 C32 H32A 119.1 . . ? C31 C32 H32A 119.1 . . ? As1 O1 Zn1 134.01(13) . . ? As1 O2 H2A 109.5 . . ? As1 O3 Zn2 127.50(13) . . ? S1 O5 Zn1 111.70(15) . . ? As2 O7 Zn1 128.43(13) . . ? As2 O8 Zn2 128.99(13) . 1_545 ? As2 O9 H9B 109.5 . . ? S2 O12 Zn2 150.66(17) . 1_545 ? H1WA O1W H1WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? H3WA O3W H3WB 109.5 . . ? H4WA O4W H4WB 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2A O1W 0.82 1.77 2.583(4) 172.0 . O9 H9B O1 0.82 1.81 2.627(3) 173.7 . O1W H1WA O4W 0.85 1.91 2.704(5) 155.7 . O1W H1WB O10 0.85 1.90 2.747(5) 177.1 1_565 O3W H3WA O2W 0.85 1.97 2.774(5) 158.5 2_454 O3W H3WB O11 0.85 1.98 2.835(4) 179.5 . O4W H4WB O6 0.85 2.40 2.829(5) 111.7 2_464 O4W H4WA O3W 0.85 1.88 2.673(5) 154.3 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.471 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.076 #===end data_12 _database_code_depnum_ccdc_archive 'CCDC 763195' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H15 As N2 O7 S Zn' _chemical_formula_weight 543.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 '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' '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.648(6) _cell_length_b 8.181(4) _cell_length_c 37.325(17) _cell_angle_alpha 90.00 _cell_angle_beta 94.225(7) _cell_angle_gamma 90.00 _cell_volume 3852(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7261 _cell_measurement_theta_min 3.0356 _cell_measurement_theta_max 27.4410 _exptl_crystal_description 'prism' _exptl_crystal_colour 'white' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 3.135 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.0274 _exptl_absorpt_correction_T_max 1 _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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27305 _diffrn_reflns_av_R_equivalents 0.1387 _diffrn_reflns_av_sigmaI/netI 0.1628 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8644 _reflns_number_gt 5148 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0277P)^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 shelxtl _refine_ls_extinction_coef ? _refine_ls_number_reflns 8644 _refine_ls_number_parameters 531 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.903 _refine_ls_shift/su_max 0.005 _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 0.87784(5) 0.63335(9) 0.04466(2) 0.0297(2) Uani 1 1 d . . . Zn2 Zn 0.48479(5) 0.11629(9) 0.19275(2) 0.02737(19) Uani 1 1 d . . . As1 As 1.00604(5) 0.71420(8) -0.030801(18) 0.02716(17) Uani 1 1 d . . . As2 As 0.41372(4) 0.47691(7) 0.227880(18) 0.02445(17) Uani 1 1 d . . . S2 S 0.26623(11) 0.11835(19) 0.22943(5) 0.0291(4) Uani 1 1 d . . . S1 S 0.74139(13) 0.8196(2) -0.01939(5) 0.0392(4) Uani 1 1 d . . . N1 N 0.9554(4) 0.7683(6) 0.08724(14) 0.0317(13) Uani 1 1 d . . . N2 N 0.7623(4) 0.6255(6) 0.08438(15) 0.0327(13) Uani 1 1 d . . . N3 N 0.4638(4) -0.0117(6) 0.14438(14) 0.0309(13) Uani 1 1 d . . . N4 N 0.6315(4) 0.1762(6) 0.16774(15) 0.0318(13) Uani 1 1 d . . . C14 C 1.0916(6) 0.9304(9) 0.1176(2) 0.047(2) Uani 1 1 d . . . H14A H 1.1578 0.9793 0.1170 0.057 Uiso 1 1 calc R . . C15 C 1.0377(6) 0.9465(9) 0.1470(2) 0.050(2) Uani 1 1 d . . . H15A H 1.0659 1.0064 0.1666 0.060 Uiso 1 1 calc R . . C16 C 0.9367(6) 0.8706(8) 0.1479(2) 0.0396(17) Uani 1 1 d . . . C17 C 0.8714(7) 0.8813(9) 0.1777(2) 0.053(2) Uani 1 1 d . . . H17A H 0.8952 0.9390 0.1982 0.063 Uiso 1 1 calc R . . C18 C 0.7758(6) 0.8078(9) 0.1761(2) 0.048(2) Uani 1 1 d . . . H18A H 0.7350 0.8172 0.1957 0.058 Uiso 1 1 calc R . . C19 C 0.7335(6) 0.7154(8) 0.1454(2) 0.0390(17) Uani 1 1 d . . . C20 C 0.6353(6) 0.6329(9) 0.1426(2) 0.048(2) Uani 1 1 d . . . H20A H 0.5923 0.6341 0.1618 0.058 Uiso 1 1 calc R . . C21 C 0.6035(5) 0.5518(8) 0.1120(2) 0.047(2) Uani 1 1 d . . . H21A H 0.5394 0.4957 0.1102 0.056 Uiso 1 1 calc R . . C22 C 0.6679(5) 0.5530(9) 0.0830(2) 0.0436(19) Uani 1 1 d . . . H22A H 0.6435 0.5008 0.0619 0.052 Uiso 1 1 calc R . . C23 C 0.7941(5) 0.7048(7) 0.11513(18) 0.0288(14) Uani 1 1 d . . . C24 C 0.8981(5) 0.7825(8) 0.11680(17) 0.0319(15) Uani 1 1 d . . . C13 C 1.0494(5) 0.8407(8) 0.08750(19) 0.0379(17) Uani 1 1 d . . . H13A H 1.0885 0.8320 0.0674 0.046 Uiso 1 1 calc R . . C6 C 0.9047(5) 0.6109(8) -0.09721(19) 0.0403(17) Uani 1 1 d . . . H6A H 0.9739 0.5811 -0.1010 0.048 Uiso 1 1 calc R . . C1 C 0.8823(5) 0.6806(8) -0.06439(17) 0.0307(15) Uani 1 1 d . . . C5 C 0.8250(6) 0.5859(9) -0.1240(2) 0.049(2) Uani 1 1 d . . . H5A H 0.8408 0.5348 -0.1453 0.059 Uiso 1 1 calc R . . C4 C 0.7233(6) 0.6351(9) -0.1199(2) 0.050(2) Uani 1 1 d . . . H4A H 0.6708 0.6213 -0.1384 0.060 Uiso 1 1 calc R . . C3 C 0.6995(5) 0.7060(9) -0.0876(2) 0.047(2) Uani 1 1 d . . . H3A H 0.6303 0.7385 -0.0845 0.056 Uiso 1 1 calc R . . C2 C 0.7782(5) 0.7291(8) -0.05971(17) 0.0308(15) Uani 1 1 d . . . C7 C 0.2603(4) 0.4623(7) 0.22355(16) 0.0259(14) Uani 1 1 d . . . C12 C 0.2066(5) 0.6109(8) 0.22119(18) 0.0346(16) Uani 1 1 d . . . H12A H 0.2442 0.7083 0.2202 0.042 Uiso 1 1 calc R . . C11 C 0.0961(5) 0.6130(9) 0.2203(2) 0.0419(18) Uani 1 1 d . . . H11A H 0.0609 0.7129 0.2193 0.050 Uiso 1 1 calc R . . C10 C 0.0384(5) 0.4716(9) 0.22085(18) 0.0423(19) Uani 1 1 d . . . H10A H -0.0353 0.4753 0.2202 0.051 Uiso 1 1 calc R . . C9 C 0.0918(4) 0.3209(8) 0.22244(19) 0.0374(17) Uani 1 1 d . . . H9A H 0.0529 0.2244 0.2226 0.045 Uiso 1 1 calc R . . C8 C 0.2023(4) 0.3134(7) 0.22385(16) 0.0237(13) Uani 1 1 d . . . C26 C 0.8001(5) 0.2966(8) 0.1595(2) 0.048(2) Uani 1 1 d . . . H26A H 0.8579 0.3556 0.1693 0.057 Uiso 1 1 calc R . . C27 C 0.7996(5) 0.2409(9) 0.1250(2) 0.047(2) Uani 1 1 d . . . H27A H 0.8560 0.2638 0.1111 0.057 Uiso 1 1 calc R . . C28 C 0.7124(5) 0.1479(8) 0.1106(2) 0.0372(17) Uani 1 1 d . . . C29 C 0.7016(6) 0.0821(10) 0.0750(2) 0.052(2) Uani 1 1 d . . . H29A H 0.7553 0.1007 0.0598 0.063 Uiso 1 1 calc R . . C30 C 0.6166(6) -0.0057(10) 0.0628(2) 0.055(2) Uani 1 1 d . . . H30A H 0.6110 -0.0415 0.0391 0.066 Uiso 1 1 calc R . . C31 C 0.5339(5) -0.0452(8) 0.08609(19) 0.0382(17) Uani 1 1 d . . . C32 C 0.4460(6) -0.1474(9) 0.0752(2) 0.0450(19) Uani 1 1 d . . . H32A H 0.4388 -0.1916 0.0522 0.054 Uiso 1 1 calc R . . C33 C 0.3729(6) -0.1785(9) 0.0994(2) 0.047(2) Uani 1 1 d . . . H33A H 0.3152 -0.2453 0.0927 0.057 Uiso 1 1 calc R . . C34 C 0.3829(5) -0.1120(8) 0.13392(19) 0.0386(17) Uani 1 1 d . . . H34A H 0.3326 -0.1374 0.1500 0.046 Uiso 1 1 calc R . . C35 C 0.5403(5) 0.0157(8) 0.12095(18) 0.0308(15) Uani 1 1 d . . . C36 C 0.6299(5) 0.1168(7) 0.13339(18) 0.0282(15) Uani 1 1 d . . . C25 C 0.7136(5) 0.2653(8) 0.1803(2) 0.0403(17) Uani 1 1 d . . . H25A H 0.7142 0.3083 0.2034 0.048 Uiso 1 1 calc R . . O1 O 1.1053(3) 0.6066(5) -0.04619(12) 0.0334(11) Uani 1 1 d . . . O2 O 1.0393(3) 0.9157(5) -0.03911(12) 0.0386(12) Uani 1 1 d . . . H2A H 1.0824 0.9480 -0.0232 0.058 Uiso 1 1 calc R . . O3 O 0.9929(3) 0.6899(5) 0.01255(12) 0.0363(11) Uani 1 1 d . . . O4 O 0.7555(3) 0.6893(6) 0.00771(13) 0.0487(14) Uani 1 1 d . . . O5 O 0.6309(3) 0.8665(6) -0.02517(14) 0.0548(15) Uani 1 1 d . . . O6 O 0.8131(4) 0.9554(6) -0.01222(14) 0.0571(15) Uani 1 1 d . . . O7 O 0.3476(3) 0.1410(5) 0.25881(12) 0.0370(11) Uani 1 1 d . . . O8 O 0.3125(3) 0.0863(5) 0.19513(12) 0.0367(11) Uani 1 1 d . . . O9 O 0.1831(3) 0.0031(5) 0.23591(14) 0.0466(14) Uani 1 1 d . . . O10 O 0.4579(3) 0.4610(5) 0.27115(11) 0.0307(10) Uani 1 1 d . . . O11 O 0.4726(3) 0.3516(5) 0.20013(13) 0.0373(12) Uani 1 1 d . . . O12 O 0.4267(3) 0.6738(5) 0.21142(13) 0.0378(12) Uani 1 1 d . . . H12 H 0.4879 0.7053 0.2158 0.057 Uiso 1 1 calc R . . O1W O 0.2720(8) 0.6898(11) 0.0210(3) 0.183(4) Uiso 1 1 d . . . H1WA H 0.2186 0.7431 0.0122 0.275 Uiso 1 1 d R . . H1WB H 0.2541 0.5911 0.0244 0.275 Uiso 1 1 d R . . O2W O 0.4617(7) 0.6387(10) -0.0122(2) 0.160(4) Uiso 1 1 d . . . H2WA H 0.5122 0.7036 -0.0160 0.240 Uiso 1 1 d R . . H2WB H 0.4028 0.6866 -0.0172 0.240 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0235(4) 0.0366(5) 0.0298(5) 0.0002(3) 0.0058(3) 0.0029(3) Zn2 0.0202(4) 0.0342(4) 0.0282(5) 0.0001(3) 0.0045(3) 0.0039(3) As1 0.0197(3) 0.0319(4) 0.0306(4) 0.0003(3) 0.0063(2) 0.0000(3) As2 0.0136(3) 0.0281(4) 0.0316(4) -0.0031(3) 0.0017(2) 0.0003(2) S2 0.0172(8) 0.0328(9) 0.0384(11) -0.0029(7) 0.0089(6) -0.0013(6) S1 0.0233(9) 0.0623(13) 0.0320(11) -0.0013(9) 0.0017(7) 0.0099(8) N1 0.026(3) 0.034(3) 0.035(4) 0.000(3) 0.001(2) 0.002(2) N2 0.034(3) 0.027(3) 0.038(4) 0.002(2) 0.009(2) 0.009(2) N3 0.023(3) 0.041(3) 0.029(3) 0.001(2) 0.006(2) 0.005(2) N4 0.019(3) 0.035(3) 0.042(4) -0.003(3) 0.006(2) 0.003(2) C14 0.033(4) 0.053(5) 0.055(6) -0.006(4) -0.006(3) -0.005(3) C15 0.051(5) 0.058(5) 0.039(5) -0.005(4) -0.008(4) 0.004(4) C16 0.043(4) 0.043(4) 0.031(4) 0.001(3) -0.002(3) 0.009(3) C17 0.071(6) 0.059(5) 0.027(5) -0.004(4) 0.000(4) 0.017(4) C18 0.061(5) 0.055(5) 0.031(5) 0.006(4) 0.016(4) 0.017(4) C19 0.047(4) 0.033(4) 0.039(5) 0.012(3) 0.012(3) 0.018(3) C20 0.042(5) 0.048(5) 0.058(6) 0.014(4) 0.030(4) 0.012(4) C21 0.032(4) 0.037(4) 0.074(7) 0.015(4) 0.016(4) 0.004(3) C22 0.025(4) 0.055(5) 0.052(5) 0.005(4) 0.008(3) -0.004(3) C23 0.033(4) 0.025(3) 0.029(4) 0.006(3) 0.007(3) 0.007(3) C24 0.038(4) 0.035(4) 0.024(4) 0.001(3) 0.006(3) 0.010(3) C13 0.023(3) 0.049(4) 0.041(5) 0.008(3) -0.001(3) 0.005(3) C6 0.033(4) 0.052(5) 0.037(5) 0.001(3) 0.007(3) -0.001(3) C1 0.028(4) 0.036(4) 0.028(4) 0.001(3) 0.006(3) 0.001(3) C5 0.058(5) 0.060(5) 0.030(5) -0.011(4) -0.004(3) -0.001(4) C4 0.050(5) 0.053(5) 0.044(5) -0.006(4) -0.010(4) -0.011(4) C3 0.028(4) 0.070(6) 0.042(5) 0.002(4) -0.005(3) 0.000(3) C2 0.025(3) 0.040(4) 0.027(4) 0.004(3) 0.000(3) -0.004(3) C7 0.012(3) 0.037(4) 0.029(4) -0.005(3) 0.002(2) 0.002(2) C12 0.026(4) 0.033(4) 0.046(5) -0.002(3) 0.004(3) 0.005(3) C11 0.024(4) 0.045(5) 0.055(5) -0.001(4) -0.006(3) 0.016(3) C10 0.015(3) 0.066(5) 0.045(5) -0.010(4) -0.001(3) 0.015(3) C9 0.012(3) 0.055(5) 0.046(5) -0.003(3) 0.003(3) 0.000(3) C8 0.014(3) 0.029(3) 0.029(4) -0.002(3) 0.006(2) 0.002(2) C26 0.024(4) 0.041(5) 0.079(7) 0.008(4) 0.004(4) -0.007(3) C27 0.026(4) 0.059(5) 0.059(6) 0.004(4) 0.019(3) -0.002(3) C28 0.036(4) 0.036(4) 0.041(5) 0.011(3) 0.015(3) 0.012(3) C29 0.050(5) 0.069(6) 0.042(5) 0.005(4) 0.031(4) 0.012(4) C30 0.057(5) 0.075(6) 0.034(5) 0.002(4) 0.016(4) 0.022(4) C31 0.032(4) 0.049(5) 0.034(4) 0.006(3) 0.011(3) 0.015(3) C32 0.050(5) 0.052(5) 0.032(5) -0.015(4) -0.001(3) 0.012(4) C33 0.034(4) 0.059(5) 0.049(5) -0.013(4) 0.001(3) 0.000(4) C34 0.028(4) 0.045(4) 0.043(5) -0.008(3) 0.003(3) 0.002(3) C35 0.024(3) 0.034(4) 0.035(4) -0.002(3) 0.007(3) 0.011(3) C36 0.020(3) 0.021(3) 0.044(5) 0.008(3) 0.011(3) 0.011(2) C25 0.028(4) 0.047(5) 0.046(5) 0.002(4) 0.003(3) -0.002(3) O1 0.021(2) 0.035(3) 0.046(3) 0.001(2) 0.0099(19) 0.0060(18) O2 0.034(3) 0.032(3) 0.049(3) 0.000(2) 0.001(2) -0.005(2) O3 0.020(2) 0.053(3) 0.037(3) -0.004(2) 0.0098(18) -0.006(2) O4 0.026(3) 0.088(4) 0.033(3) 0.013(3) 0.002(2) 0.009(2) O5 0.027(3) 0.090(4) 0.048(4) -0.004(3) -0.002(2) 0.024(3) O6 0.045(3) 0.063(4) 0.062(4) -0.026(3) -0.002(3) 0.001(3) O7 0.027(3) 0.039(3) 0.044(3) -0.004(2) 0.002(2) 0.006(2) O8 0.027(2) 0.042(3) 0.042(3) -0.010(2) 0.0095(19) 0.000(2) O9 0.031(3) 0.030(3) 0.081(4) -0.001(3) 0.019(2) -0.010(2) O10 0.031(3) 0.031(3) 0.029(3) -0.002(2) -0.0042(18) -0.0042(19) O11 0.025(2) 0.036(3) 0.053(3) -0.014(2) 0.016(2) -0.0019(19) O12 0.028(2) 0.023(2) 0.061(4) 0.012(2) -0.007(2) -0.0052(19) _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 1.974(4) 3_765 ? Zn1 O3 2.006(4) . ? Zn1 O4 2.048(4) . ? Zn1 N1 2.116(5) . ? Zn1 N2 2.158(6) . ? Zn2 O10 1.953(4) 2_645 ? Zn2 O11 1.952(4) . ? Zn2 N3 2.087(5) . ? Zn2 N4 2.193(5) . ? Zn2 O8 2.201(4) . ? As1 O3 1.651(5) . ? As1 O1 1.670(4) . ? As1 O2 1.735(4) . ? As1 C1 1.952(6) . ? As2 O11 1.671(4) . ? As2 O10 1.675(4) . ? As2 O12 1.736(4) . ? As2 C7 1.939(5) . ? S2 O9 1.446(4) . ? S2 O7 1.459(4) . ? S2 O8 1.470(5) . ? S2 C8 1.794(6) . ? S1 O5 1.450(4) . ? S1 O6 1.447(5) . ? S1 O4 1.471(5) . ? S1 C2 1.770(7) . ? N1 C13 1.328(7) . ? N1 C24 1.368(8) . ? N2 C22 1.331(8) . ? N2 C23 1.354(8) . ? N3 C34 1.347(8) . ? N3 C35 1.370(8) . ? N4 C25 1.326(8) . ? N4 C36 1.370(8) . ? C14 C15 1.343(10) . ? C14 C13 1.413(9) . ? C14 H14A 0.9300 . ? C15 C16 1.422(10) . ? C15 H15A 0.9300 . ? C16 C24 1.421(9) . ? C16 C17 1.436(10) . ? C17 C18 1.348(10) . ? C17 H17A 0.9300 . ? C18 C19 1.441(10) . ? C18 H18A 0.9300 . ? C19 C20 1.411(9) . ? C19 C23 1.413(9) . ? C20 C21 1.357(10) . ? C20 H20A 0.9300 . ? C21 C22 1.400(10) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.459(9) . ? C13 H13A 0.9300 . ? C6 C5 1.383(8) . ? C6 C1 1.399(9) . ? C6 H6A 0.9300 . ? C1 C2 1.398(8) . ? C5 C4 1.367(10) . ? C5 H5A 0.9300 . ? C4 C3 1.389(10) . ? C4 H4A 0.9300 . ? C3 C2 1.399(8) . ? C3 H3A 0.9300 . ? C7 C12 1.392(8) . ? C7 C8 1.423(8) . ? C12 C11 1.395(8) . ? C12 H12A 0.9300 . ? C11 C10 1.370(9) . ? C11 H11A 0.9300 . ? C10 C9 1.405(8) . ? C10 H10A 0.9300 . ? C9 C8 1.396(7) . ? C9 H9A 0.9300 . ? C26 C27 1.365(10) . ? C26 C25 1.411(9) . ? C26 H26A 0.9300 . ? C27 C28 1.413(9) . ? C27 H27A 0.9300 . ? C28 C36 1.417(9) . ? C28 C29 1.431(10) . ? C29 C30 1.344(10) . ? C29 H29A 0.9300 . ? C30 C31 1.446(10) . ? C30 H30A 0.9300 . ? C31 C35 1.390(9) . ? C31 C32 1.425(9) . ? C32 C33 1.363(10) . ? C32 H32A 0.9300 . ? C33 C34 1.397(9) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.451(8) . ? C25 H25A 0.9300 . ? O1 Zn1 1.974(4) 3_765 ? O2 H2A 0.8200 . ? O10 Zn2 1.953(4) 2_655 ? O12 H12 0.8200 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? 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 99.52(17) 3_765 . ? O1 Zn1 O4 108.43(19) 3_765 . ? O3 Zn1 O4 95.25(19) . . ? O1 Zn1 N1 117.00(19) 3_765 . ? O3 Zn1 N1 90.69(19) . . ? O4 Zn1 N1 132.4(2) . . ? O1 Zn1 N2 91.58(18) 3_765 . ? O3 Zn1 N2 167.15(19) . . ? O4 Zn1 N2 87.3(2) . . ? N1 Zn1 N2 78.4(2) . . ? O10 Zn2 O11 124.99(19) 2_645 . ? O10 Zn2 N3 106.70(19) 2_645 . ? O11 Zn2 N3 127.6(2) . . ? O10 Zn2 N4 98.99(19) 2_645 . ? O11 Zn2 N4 85.28(18) . . ? N3 Zn2 N4 78.5(2) . . ? O10 Zn2 O8 102.60(17) 2_645 . ? O11 Zn2 O8 90.89(16) . . ? N3 Zn2 O8 85.18(18) . . ? N4 Zn2 O8 155.95(19) . . ? O3 As1 O1 114.0(2) . . ? O3 As1 O2 109.4(2) . . ? O1 As1 O2 104.0(2) . . ? O3 As1 C1 118.6(2) . . ? O1 As1 C1 107.0(2) . . ? O2 As1 C1 102.3(2) . . ? O11 As2 O10 114.7(2) . . ? O11 As2 O12 107.0(2) . . ? O10 As2 O12 112.3(2) . . ? O11 As2 C7 113.6(2) . . ? O10 As2 C7 109.6(2) . . ? O12 As2 C7 98.5(2) . . ? O9 S2 O7 116.0(3) . . ? O9 S2 O8 111.8(3) . . ? O7 S2 O8 111.9(3) . . ? O9 S2 C8 105.8(3) . . ? O7 S2 C8 105.1(3) . . ? O8 S2 C8 105.2(3) . . ? O5 S1 O6 114.1(3) . . ? O5 S1 O4 111.1(3) . . ? O6 S1 O4 112.8(3) . . ? O5 S1 C2 107.2(3) . . ? O6 S1 C2 106.1(3) . . ? O4 S1 C2 104.8(3) . . ? C13 N1 C24 118.9(6) . . ? C13 N1 Zn1 127.1(5) . . ? C24 N1 Zn1 114.0(4) . . ? C22 N2 C23 117.1(6) . . ? C22 N2 Zn1 129.7(5) . . ? C23 N2 Zn1 113.2(4) . . ? C34 N3 C35 118.2(6) . . ? C34 N3 Zn2 127.0(5) . . ? C35 N3 Zn2 114.8(4) . . ? C25 N4 C36 118.9(6) . . ? C25 N4 Zn2 129.6(5) . . ? C36 N4 Zn2 111.4(4) . . ? C15 C14 C13 121.1(7) . . ? C15 C14 H14A 119.4 . . ? C13 C14 H14A 119.4 . . ? C14 C15 C16 119.1(7) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? C15 C16 C24 117.3(7) . . ? C15 C16 C17 124.0(7) . . ? C24 C16 C17 118.8(7) . . ? C18 C17 C16 120.2(7) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C19 123.3(7) . . ? C17 C18 H18A 118.4 . . ? C19 C18 H18A 118.4 . . ? C20 C19 C23 116.0(7) . . ? C20 C19 C18 125.6(7) . . ? C23 C19 C18 118.4(7) . . ? C21 C20 C19 120.0(7) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C22 119.6(7) . . ? C20 C21 H21A 120.2 . . ? C22 C21 H21A 120.2 . . ? N2 C22 C21 123.0(7) . . ? N2 C22 H22A 118.5 . . ? C21 C22 H22A 118.5 . . ? N2 C23 C19 124.2(6) . . ? N2 C23 C24 117.1(6) . . ? C19 C23 C24 118.7(6) . . ? N1 C24 C16 122.1(6) . . ? N1 C24 C23 117.2(6) . . ? C16 C24 C23 120.7(6) . . ? N1 C13 C14 121.5(7) . . ? N1 C13 H13A 119.2 . . ? C14 C13 H13A 119.2 . . ? C5 C6 C1 120.7(7) . . ? C5 C6 H6A 119.6 . . ? C1 C6 H6A 119.6 . . ? C2 C1 C6 118.6(6) . . ? C2 C1 As1 126.7(5) . . ? C6 C1 As1 114.6(5) . . ? C4 C5 C6 121.0(7) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C4 C3 119.2(7) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C3 C2 120.9(7) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C1 C2 C3 119.5(7) . . ? C1 C2 S1 122.3(5) . . ? C3 C2 S1 118.2(5) . . ? C12 C7 C8 120.0(5) . . ? C12 C7 As2 115.6(4) . . ? C8 C7 As2 124.4(4) . . ? C7 C12 C11 119.7(6) . . ? C7 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C10 C11 C12 121.6(6) . . ? C10 C11 H11A 119.2 . . ? C12 C11 H11A 119.2 . . ? C11 C10 C9 119.1(6) . . ? C11 C10 H10A 120.4 . . ? C9 C10 H10A 120.4 . . ? C8 C9 C10 121.1(6) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C9 C8 C7 118.5(5) . . ? C9 C8 S2 119.0(5) . . ? C7 C8 S2 122.3(4) . . ? C27 C26 C25 120.6(7) . . ? C27 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C26 C27 C28 119.1(7) . . ? C26 C27 H27A 120.5 . . ? C28 C27 H27A 120.5 . . ? C27 C28 C36 117.3(7) . . ? C27 C28 C29 125.0(7) . . ? C36 C28 C29 117.7(7) . . ? C30 C29 C28 122.4(7) . . ? C30 C29 H29A 118.8 . . ? C28 C29 H29A 118.8 . . ? C29 C30 C31 120.8(8) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C35 C31 C32 117.9(6) . . ? C35 C31 C30 119.2(7) . . ? C32 C31 C30 122.9(7) . . ? C33 C32 C31 118.3(7) . . ? C33 C32 H32A 120.9 . . ? C31 C32 H32A 120.9 . . ? C32 C33 C34 121.2(7) . . ? C32 C33 H33A 119.4 . . ? C34 C33 H33A 119.4 . . ? N3 C34 C33 121.4(7) . . ? N3 C34 H34A 119.3 . . ? C33 C34 H34A 119.3 . . ? N3 C35 C31 122.9(6) . . ? N3 C35 C36 117.4(6) . . ? C31 C35 C36 119.7(6) . . ? N4 C36 C28 122.5(6) . . ? N4 C36 C35 117.3(6) . . ? C28 C36 C35 120.1(7) . . ? N4 C25 C26 121.6(7) . . ? N4 C25 H25A 119.2 . . ? C26 C25 H25A 119.2 . . ? As1 O1 Zn1 126.6(2) . 3_765 ? As1 O2 H2A 109.5 . . ? As1 O3 Zn1 138.0(2) . . ? S1 O4 Zn1 132.2(3) . . ? S2 O8 Zn2 118.3(2) . . ? As2 O10 Zn2 134.1(2) . 2_655 ? As2 O11 Zn2 137.4(3) . . ? As2 O12 H12 109.5 . . ? H1WA O1W H1WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2A O6 0.82 1.96 2.782(6) 174.5 3_775 O12 H12 O10 0.82 2.24 2.816(6) 127.2 2_655 O12 H12 O7 0.82 2.28 2.998(6) 145.9 2_655 O2W H2WA O5 0.85 2.06 2.905(10) 178.1 . O2W H2WB O1W 0.85 2.26 2.813(14) 122.4 . _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.777 _refine_diff_density_min -1.448 _refine_diff_density_rms 0.171 #===end