# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. #------------------ SUBMISSION DETAILS --------------------------------------# # Name and address of author for correspondence _journal_coden_Cambridge 0182 #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2006-01-02 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? _publ_contact_author_name 'Mark T.Weller' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ UK ; _publ_contact_author_email mtw@soton.ac.uk _publ_contact_author_fax 44(23)80596805 _publ_contact_author_phone 44(23)80593592 _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission ? ; _publ_section_title ; A chiral, 16-ring channel framework and a layered caesium zincoarsenate ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_address S.B.Wiggin ; School of Chemistry University of Southampton Southampton SO17 1BJ UK ; M.T.Weller ; School of Chemistry University of Southampton Southampton SO17 1BJ UK ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_p21_Cs2(ZnAsO3OH)(ZnAsO4)2.H2O _database_code_depnum_ccdc_archive 'CCDC 290224' _audit_creation_date 2006-01-02T15:41:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'As3 H O12 Zn3, H2 O, 2(Cs)' _chemical_formula_sum 'As3 Cs2 H3 O13 Zn3' _chemical_formula_weight 897.71 _chemical_absolute_configuration unk #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.768(2) _cell_length_b 5.2056(12) _cell_length_c 13.747(3) _cell_angle_alpha 90 _cell_angle_beta 110.240(13) _cell_angle_gamma 90 _cell_volume 723.0(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11417 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 120(2) #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 4.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 16.77 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, 2003)' _exptl_absorpt_correction_T_min 0.2848 _exptl_absorpt_correction_T_max 0.8502 _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 11680 reflections reduced R(int) from 0.1212 to 0.0551 Ratio of minimum to maximum apparent transmission: 0.736941 The given Tmin and Tmax were generated using the SHELX SIZE command The partial occupancy water molecules were allowed to freely refine and gave values of 0.48(5) and 0.52(5). It was decided to fix both as half occupied as the values are not significantly different. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD area-detector' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8751 _diffrn_reflns_av_R_equivalents 0.0793 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.61 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.993 _reflns_number_total 3275 _reflns_number_gt 2837 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) &COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_molecular_graphics 'DIAMOND V2.1a (Brandenburg, K., 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0425P)^2^+8.2762P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3275 _refine_ls_number_parameters 202 _refine_ls_number_restraints 2 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1248 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.22(3) _refine_diff_density_max 1.844 _refine_diff_density_min -0.985 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.368 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly As1 As 0.28735(12) 1.2562(3) -0.13867(10) 0.0323(3) Uani 1 d . . . As2 As 0.34014(13) 0.2912(3) 0.52179(9) 0.0338(3) Uani 1 d . . . As3 As 0.20946(11) 0.7992(3) 0.14101(9) 0.0282(3) Uani 1 d . . . Cs1 Cs 0.00822(8) 0.2630(2) 0.27619(7) 0.0448(2) Uani 1 d . . . Cs2 Cs 0.50981(7) 0.26037(19) 0.25690(6) 0.03385(19) Uani 1 d . . . O1 O 0.2827(12) 1.351(2) -0.2541(8) 0.044(3) Uani 1 d . . . O2 O 0.3037(10) 0.9389(19) -0.1222(8) 0.038(2) Uani 1 d . . . O3 O 0.4227(9) 1.3963(18) -0.0465(9) 0.040(2) Uani 1 d . . . O4 O 0.1538(9) 1.363(2) -0.1145(7) 0.036(2) Uani 1 d . . . O5 O 0.3459(9) 0.7052(19) 0.1197(8) 0.037(2) Uani 1 d . . . O6 O 0.1907(10) 1.1148(18) 0.1267(8) 0.035(2) Uani 1 d . . . O7 O 0.0783(8) 0.6584(16) 0.0496(7) 0.0264(18) Uani 1 d . . . O8 O 0.2081(10) 0.706(2) 0.2554(7) 0.037(2) Uani 1 d . . . O9 O 0.3147(11) 0.1527(19) 0.4063(8) 0.041(2) Uani 1 d . . . O10 O 0.3129(10) 0.6059(19) 0.5075(7) 0.037(2) Uani 1 d . . . O11 O 0.4870(9) 0.228(2) 0.6130(7) 0.036(2) Uani 1 d . . . O12 O 0.2242(10) 0.1632(19) 0.5660(8) 0.041(2) Uani 1 d . . . H12 H 0.253 0.1638 0.6311 0.061 Uiso 1 calc RD . . Zn1 Zn 0.10284(13) 1.3071(3) 0.00310(11) 0.0284(3) Uani 1 d . . . Zn2 Zn 0.33689(14) 0.7889(4) 0.39123(11) 0.0338(3) Uani 1 d . . . Zn3 Zn 0.39674(13) 0.7454(4) 0.00014(11) 0.0323(3) Uani 1 d . . . O1W O 0.0506(19) 0.675(4) 0.4809(17) 0.043(5) Uani 0.5 d P 1 . H1B H 0.0107 0.8336 0.4436 0.065 Uiso 0.5 calc PRD 1 . H1A H 0.1472 0.7053 0.5036 0.065 Uiso 0.5 calc PR 1 . O2W O 0.0301(17) 0.751(7) 0.4122(15) 0.047(5) Uani 0.5 d P 2 . H2A H 0.1159 0.75 0.4702 0.071 Uiso 0.5 calc PR 2 . H2B H -0.0416 0.75 0.4419 0.071 Uiso 0.5 calc PR 2 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0312(6) 0.0279(7) 0.0410(7) -0.0024(7) 0.0166(5) -0.0012(7) As2 0.0357(6) 0.0315(8) 0.0297(6) -0.0016(6) 0.0053(5) -0.0031(6) As3 0.0257(5) 0.0277(8) 0.0291(6) 0.0004(6) 0.0070(4) -0.0004(6) Cs1 0.0337(4) 0.0400(5) 0.0573(5) -0.0067(6) 0.0114(4) 0.0002(5) Cs2 0.0319(4) 0.0342(4) 0.0334(4) 0.0007(4) 0.0087(3) 0.0006(4) O1 0.072(7) 0.026(6) 0.047(6) -0.003(4) 0.037(5) -0.009(5) O2 0.042(6) 0.033(6) 0.039(6) 0.003(4) 0.014(5) 0.000(4) O3 0.021(4) 0.027(5) 0.069(7) -0.009(5) 0.014(5) -0.001(4) O4 0.028(4) 0.045(6) 0.035(5) 0.001(4) 0.011(4) 0.004(4) O5 0.025(4) 0.035(6) 0.046(5) 0.003(4) 0.008(4) 0.004(4) O6 0.038(5) 0.022(5) 0.042(6) -0.003(4) 0.009(4) -0.007(4) O7 0.026(4) 0.023(4) 0.030(5) -0.002(3) 0.008(3) 0.001(3) O8 0.045(5) 0.043(7) 0.025(4) 0.005(4) 0.015(4) 0.000(5) O9 0.052(6) 0.031(5) 0.031(5) -0.002(4) 0.002(4) 0.002(5) O10 0.044(6) 0.039(5) 0.029(5) 0.001(4) 0.013(4) 0.002(4) O11 0.036(5) 0.039(6) 0.029(4) 0.005(5) 0.007(4) -0.005(5) O12 0.039(6) 0.037(5) 0.043(6) 0.006(4) 0.010(4) -0.005(4) Zn1 0.0248(6) 0.0287(9) 0.0309(7) -0.0011(6) 0.0087(5) -0.0011(7) Zn2 0.0362(7) 0.0322(9) 0.0297(7) 0.0009(7) 0.0072(5) -0.0004(7) Zn3 0.0296(7) 0.0250(8) 0.0453(8) -0.0008(8) 0.0169(6) 0.0001(8) O1W 0.027(10) 0.054(14) 0.039(12) -0.001(10) -0.001(9) -0.017(9) O2W 0.024(9) 0.081(17) 0.033(10) -0.018(15) 0.005(7) -0.006(13) #------------------ MOLECULAR GEOMETRY --------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 O1 1.646(10) . ? As1 O2 1.668(10) . ? As1 O4 1.679(9) . ? As1 O3 1.728(10) . ? As1 Cs1 4.0164(18) 2 ? As1 Cs1 4.0620(18) 2_565 ? As2 O10 1.664(10) . ? As2 O11 1.676(9) . ? As2 O9 1.678(10) . ? As2 O12 1.702(10) . ? As2 Cs1 3.9807(17) . ? As3 O8 1.651(9) . ? As3 O6 1.659(10) . ? As3 O5 1.667(9) . ? As3 O7 1.698(9) . ? As3 Cs1 4.0945(17) 1_565 ? As3 Cs1 4.3275(18) . ? Cs1 O4 3.105(10) 2_535 ? Cs1 O2W 3.12(3) . ? Cs1 O9 3.215(10) . ? Cs1 O2W 3.22(3) 1_545 ? Cs1 O8 3.234(10) . ? Cs1 O6 3.387(11) 1_545 ? Cs1 O2 3.418(10) 2_545 ? Cs1 O1W 3.44(2) . ? Cs1 O1W 3.64(2) 2_546 ? Cs1 O8 3.680(11) 1_545 ? Cs1 O1 3.722(12) 2_535 ? O1 Cs1 3.722(12) 2_565 ? O2 Zn3 1.919(10) . ? O2 Cs1 3.418(10) 2 ? O3 Zn3 1.979(10) 1_565 ? O3 Zn3 1.986(9) 2_655 ? O4 Zn1 1.900(10) . ? O4 Cs1 3.105(10) 2_565 ? O5 Zn3 1.916(10) . ? O6 Zn1 1.917(10) . ? O6 Cs1 3.387(11) 1_565 ? O7 Zn1 1.985(8) 1_545 ? O7 Zn1 1.988(9) 2_545 ? O8 Zn2 1.950(9) . ? O8 Cs1 3.680(11) 1_565 ? O9 Zn2 1.929(10) 1_545 ? O10 Zn2 1.953(10) . ? O11 Zn2 1.942(9) 2_646 ? O12 H12 0.84 . ? Zn1 O7 1.985(8) 1_565 ? Zn1 O7 1.988(9) 2 ? Zn1 Cs1 4.2229(18) 1_565 ? Zn1 Cs1 4.3157(19) 2_565 ? Zn2 O9 1.929(10) 1_565 ? Zn2 O11 1.942(9) 2_656 ? Zn2 Cs1 4.153(2) 1_565 ? Zn3 O3 1.979(10) 1_545 ? Zn3 O3 1.986(9) 2_645 ? O1W Cs1 3.64(2) 2_556 ? O1W H1B 0.99 . ? O1W H1A 0.99 . ? O2W Cs1 3.22(3) 1_565 ? O2W H2A 0.99 . ? O2W H2B 0.99 . ? 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 As1 O2 113.2(5) . . ? O1 As1 O4 110.5(5) . . ? O2 As1 O4 111.0(5) . . ? O1 As1 O3 108.5(5) . . ? O2 As1 O3 107.2(5) . . ? O4 As1 O3 106.2(5) . . ? O1 As1 Cs1 89.0(4) . 2 ? O2 As1 Cs1 57.3(4) . 2 ? O4 As1 Cs1 73.2(3) . 2 ? O3 As1 Cs1 161.0(4) . 2 ? O1 As1 Cs1 66.4(4) . 2_565 ? O2 As1 Cs1 137.3(4) . 2_565 ? O3 As1 Cs1 113.2(3) . 2_565 ? Cs1 As1 Cs1 80.24(3) 2 2_565 ? O10 As2 O11 111.3(5) . . ? O10 As2 O9 110.3(5) . . ? O11 As2 O9 115.3(5) . . ? O10 As2 O12 107.8(5) . . ? O11 As2 O12 106.0(5) . . ? O9 As2 O12 105.7(5) . . ? O10 As2 Cs1 82.3(3) . . ? O11 As2 Cs1 164.9(4) . . ? O9 As2 Cs1 51.4(4) . . ? O12 As2 Cs1 74.6(4) . . ? O8 As3 O6 111.3(5) . . ? O8 As3 O5 112.3(5) . . ? O6 As3 O5 110.4(5) . . ? O8 As3 O7 107.4(5) . . ? O6 As3 O7 107.7(4) . . ? O5 As3 O7 107.5(5) . . ? O8 As3 Cs1 63.9(4) . 1_565 ? O6 As3 Cs1 53.7(4) . 1_565 ? O5 As3 Cs1 152.8(4) . 1_565 ? O7 As3 Cs1 98.9(3) . 1_565 ? O6 As3 Cs1 129.1(4) . . ? O5 As3 Cs1 119.2(4) . . ? O7 As3 Cs1 68.1(3) . . ? Cs1 As3 Cs1 76.30(3) 1_565 . ? O4 Cs1 O2W 152.1(4) 2_535 . ? O4 Cs1 O9 119.5(3) 2_535 . ? O2W Cs1 O9 87.8(4) . . ? O4 Cs1 O2W 76.7(4) 2_535 1_545 ? O2W Cs1 O2W 110.6(6) . 1_545 ? O9 Cs1 O2W 71.0(4) . 1_545 ? O4 Cs1 O8 129.9(2) 2_535 . ? O2W Cs1 O8 63.7(4) . . ? O9 Cs1 O8 65.8(3) . . ? O2W Cs1 O8 136.5(4) 1_545 . ? O4 Cs1 O6 73.3(2) 2_535 1_545 ? O2W Cs1 O6 127.6(4) . 1_545 ? O9 Cs1 O6 66.3(3) . 1_545 ? O2W Cs1 O6 102.9(4) 1_545 1_545 ? O8 Cs1 O6 64.2(2) . 1_545 ? O4 Cs1 O2 63.1(2) 2_535 2_545 ? O2W Cs1 O2 90.4(4) . 2_545 ? O9 Cs1 O2 172.8(3) . 2_545 ? O2W Cs1 O2 116.1(3) 1_545 2_545 ? O8 Cs1 O2 107.2(2) . 2_545 ? O6 Cs1 O2 109.7(2) 1_545 2_545 ? O4 Cs1 O1W 152.4(4) 2_535 . ? O2W Cs1 O1W 16.2(6) . . ? O9 Cs1 O1W 80.6(4) . . ? O2W Cs1 O1W 94.5(6) 1_545 . ? O8 Cs1 O1W 74.0(4) . . ? O6 Cs1 O1W 134.2(4) 1_545 . ? O2 Cs1 O1W 99.4(4) 2_545 . ? O4 Cs1 O1W 109.8(4) 2_535 2_546 ? O2W Cs1 O1W 63.5(6) . 2_546 ? O9 Cs1 O1W 86.4(4) . 2_546 ? O2W Cs1 O1W 50.4(6) 1_545 2_546 ? O8 Cs1 O1W 120.3(4) . 2_546 ? O6 Cs1 O1W 148.2(3) 1_545 2_546 ? O2 Cs1 O1W 99.0(3) 2_545 2_546 ? O1W Cs1 O1W 49.0(3) . 2_546 ? O4 Cs1 O8 67.3(2) 2_535 1_545 ? O2W Cs1 O8 139.9(4) . 1_545 ? O9 Cs1 O8 52.2(2) . 1_545 ? O2W Cs1 O8 57.7(4) 1_545 1_545 ? O8 Cs1 O8 97.5(2) . 1_545 ? O6 Cs1 O8 45.2(2) 1_545 1_545 ? O2 Cs1 O8 129.7(2) 2_545 1_545 ? O1W Cs1 O8 129.7(4) . 1_545 ? O1W Cs1 O8 105.3(3) 2_546 1_545 ? O4 Cs1 O1 46.1(2) 2_535 2_535 ? O2W Cs1 O1 114.0(4) . 2_535 ? O9 Cs1 O1 128.0(3) . 2_535 ? O2W Cs1 O1 57.3(3) 1_545 2_535 ? O8 Cs1 O1 166.2(2) . 2_535 ? O6 Cs1 O1 117.9(2) 1_545 2_535 ? O2 Cs1 O1 59.0(2) 2_545 2_535 ? O1W Cs1 O1 107.2(4) . 2_535 ? O1W Cs1 O1 66.0(4) 2_546 2_535 ? O8 Cs1 O1 92.2(2) 1_545 2_535 ? O4 Cs1 As2 138.52(19) 2_535 . ? O2W Cs1 As2 66.5(4) . . ? O9 Cs1 As2 24.10(19) . . ? O2W Cs1 As2 71.0(3) 1_545 . ? O8 Cs1 As2 67.59(16) . . ? O6 Cs1 As2 89.08(16) 1_545 . ? O2 Cs1 As2 156.49(17) 2_545 . ? O1W Cs1 As2 57.1(3) . . ? O1W Cs1 As2 67.4(3) 2_546 . ? O8 Cs1 As2 73.58(15) 1_545 . ? O1 Cs1 As2 125.02(17) 2_535 . ? As1 O1 Cs1 89.7(4) . 2_565 ? As1 O2 Zn3 129.6(6) . . ? As1 O2 Cs1 98.4(4) . 2 ? Zn3 O2 Cs1 120.4(4) . 2 ? As1 O3 Zn3 116.6(5) . 1_565 ? As1 O3 Zn3 123.5(5) . 2_655 ? Zn3 O3 Zn3 119.5(5) 1_565 2_655 ? As1 O4 Zn1 129.6(6) . . ? As1 O4 Cs1 112.8(4) . 2_565 ? Zn1 O4 Cs1 117.1(4) . 2_565 ? As3 O5 Zn3 130.5(5) . . ? As3 O6 Zn1 128.7(5) . . ? As3 O6 Cs1 103.1(4) . 1_565 ? Zn1 O6 Cs1 102.0(4) . 1_565 ? As3 O7 Zn1 117.8(5) . 1_545 ? As3 O7 Zn1 124.2(5) . 2_545 ? Zn1 O7 Zn1 117.7(4) 1_545 2_545 ? As3 O8 Zn2 127.6(6) . . ? As3 O8 Cs1 121.3(5) . . ? Zn2 O8 Cs1 110.3(4) . . ? As3 O8 Cs1 92.3(4) . 1_565 ? Zn2 O8 Cs1 89.6(3) . 1_565 ? Cs1 O8 Cs1 97.5(2) . 1_565 ? As2 O9 Zn2 122.5(6) . 1_545 ? As2 O9 Cs1 104.5(5) . . ? Zn2 O9 Cs1 104.9(4) 1_545 . ? As2 O10 Zn2 120.6(6) . . ? As2 O11 Zn2 128.6(5) . 2_646 ? As2 O12 H12 109.5 . . ? O4 Zn1 O6 129.4(4) . . ? O4 Zn1 O7 104.1(4) . 1_565 ? O6 Zn1 O7 106.0(4) . 1_565 ? O4 Zn1 O7 106.5(4) . 2 ? O6 Zn1 O7 103.9(4) . 2 ? O7 Zn1 O7 104.7(2) 1_565 2 ? O4 Zn1 Cs1 173.7(3) . 1_565 ? O6 Zn1 Cs1 51.7(3) . 1_565 ? O7 Zn1 Cs1 70.3(3) 1_565 1_565 ? O7 Zn1 Cs1 78.2(3) 2 1_565 ? O4 Zn1 Cs1 39.8(3) . 2_565 ? O6 Zn1 Cs1 167.4(3) . 2_565 ? O7 Zn1 Cs1 75.7(3) 1_565 2_565 ? O7 Zn1 Cs1 87.4(2) 2 2_565 ? Cs1 Zn1 Cs1 137.99(5) 1_565 2_565 ? O9 Zn2 O11 108.7(5) 1_565 2_656 ? O9 Zn2 O8 104.2(4) 1_565 . ? O11 Zn2 O8 108.3(4) 2_656 . ? O9 Zn2 O10 109.6(4) 1_565 . ? O11 Zn2 O10 110.6(4) 2_656 . ? O8 Zn2 O10 115.1(4) . . ? O9 Zn2 Cs1 48.4(3) 1_565 1_565 ? O11 Zn2 Cs1 142.9(3) 2_656 1_565 ? O8 Zn2 Cs1 62.4(3) . 1_565 ? O10 Zn2 Cs1 105.3(3) . 1_565 ? O9 Zn2 Cs1 123.1(3) 1_565 . ? O11 Zn2 Cs1 124.8(3) 2_656 . ? O8 Zn2 Cs1 44.6(3) . . ? O10 Zn2 Cs1 70.5(3) . . ? Cs1 Zn2 Cs1 75.81(3) 1_565 . ? O5 Zn3 O2 126.3(4) . . ? O5 Zn3 O3 107.0(4) . 1_545 ? O2 Zn3 O3 106.7(4) . 1_545 ? O5 Zn3 O3 107.9(4) . 2_645 ? O2 Zn3 O3 103.3(4) . 2_645 ? O3 Zn3 O3 103.6(3) 1_545 2_645 ? Cs1 O1W Cs1 144.5(6) . 2_556 ? Cs1 O1W H1B 100.8 . . ? Cs1 O1W H1B 100.8 2_556 . ? Cs1 O1W H1A 100.8 . . ? Cs1 O1W H1A 100.8 2_556 . ? H1B O1W H1A 104.4 . . ? Cs1 O2W Cs1 110.6(6) . 1_565 ? Cs1 O2W H2A 109.5 . . ? Cs1 O2W H2A 109.5 1_565 . ? Cs1 O2W H2B 109.5 . . ? Cs1 O2W H2B 109.5 1_565 . ? H2A O2W H2B 108.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O12 H12 O1 1_546 0.84 1.79 2.527(15) 146.2 O1W H1B O1W 2_556 0.99 2.27 2.94(2) 124.1 O1W H1A O10 . 0.99 1.84 2.74(2) 149.9 O1W H1A O12 1_565 0.99 2.57 3.13(2) 115.9 O2W H2A O10 . 0.99 2.14 2.97(2) 140.1 O2W H2B O12 2_556 0.99 1.98 2.89(2) 151.4 #===END #\#CIF_1.1 # As3 Cs H8 O15 Zn3 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-10-20 at 15:18:48 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\cifdoc.dat # CIF files read : mono #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_mono_CsAs3Zn3O13H4.2H2O _database_code_depnum_ccdc_archive 'CCDC 290225' _audit_creation_date 2006-01-03T09:24:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'As3 H4 O13 Zn3, 2(H2 O), Cs' _chemical_formula_sum 'As3 Cs H8 O15 Zn3' _chemical_formula_weight 801.84 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 16.1047(9) _cell_length_b 6.5829(4) _cell_length_c 12.9291(7) _cell_angle_alpha 90 _cell_angle_beta 99.263(4) _cell_angle_gamma 90 _cell_volume 1352.81(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4927 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 120(2) #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 3.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 15.29 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, 2003)' _exptl_absorpt_correction_T_min 0.2915 _exptl_absorpt_correction_T_max 0.5451 _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 21055 reflections reduced R(int) from 0.1421 to 0.0636 Ratio of minimum to maximum apparent transmission: 0.544066 The given Tmin and Tmax were generated using the SHELX SIZE command ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_reflns_number 25027 _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD area-detector' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.66 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.989 _reflns_number_total 3130 _reflns_number_gt 2706 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) &COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_molecular_graphics 'DIAMOND V2.1a (Brandenburg, K., 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0304P)^2^+19.5208P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3130 _refine_ls_number_parameters 213 _refine_ls_number_restraints 8 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0902 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.023 _refine_diff_density_max 1.014 _refine_diff_density_min -1.29 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.368 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly As1 As 0.50789(4) 0.85129(10) 0.65291(5) 0.01276(15) Uani 1 d . . . As2 As 0.81926(4) -0.04013(10) 0.65996(5) 0.01435(16) Uani 1 d . . . As3 As 0.67936(4) 0.41660(10) 0.49897(5) 0.01337(15) Uani 1 d . . . Cs1 Cs 0.90956(3) 0.25325(7) 0.42902(4) 0.02056(13) Uani 1 d . . . O1 O 0.4544(3) 1.0413(7) 0.5840(4) 0.0146(9) Uani 1 d . . . O2 O 0.4618(3) 0.8038(8) 0.7583(4) 0.0166(10) Uani 1 d . . . O1W O 0.9058(3) -0.2444(9) 0.4306(4) 0.0236(12) Uani 1 d D . . O3 O 0.6100(3) 0.9084(7) 0.6924(4) 0.0158(10) Uani 1 d . . . O2W O 0.9627(3) 0.0284(8) 0.1916(4) 0.0240(11) Uani 1 d D . . O4 O 0.4996(3) 0.6468(7) 0.5748(4) 0.0133(9) Uani 1 d . . . O5 O 0.7781(3) -0.0517(8) 0.5336(4) 0.0188(10) Uani 1 d . . . O6 O 0.7774(3) 0.1144(8) 0.7388(4) 0.0179(10) Uani 1 d . . . O7 O 0.9194(3) 0.0574(8) 0.6533(4) 0.0181(10) Uani 1 d . . . H7 H 0.9482 0.0593 0.7136 0.027 Uiso 1 calc R . . O8 O 0.8358(3) -0.2742(7) 0.7111(4) 0.0183(10) Uani 1 d . . . H8 H 0.7898 -0.3243 0.7212 0.027 Uiso 1 calc RD . . O9 O 0.6845(3) 0.2514(7) 0.4005(4) 0.0155(10) Uani 1 d . . . O10 O 0.6381(3) 0.6376(7) 0.4526(4) 0.0164(10) Uani 1 d . . . O11 O 0.6323(3) 0.3126(7) 0.5927(4) 0.0157(10) Uani 1 d . . . O12 O 0.7844(3) 0.4566(7) 0.5505(4) 0.0177(10) Uani 1 d . . . H12 H 0.8024 0.3584 0.5892 0.026 Uiso 1 calc RD . . O13 O 0.6978(3) -0.1032(7) 0.2890(4) 0.0174(10) Uani 1 d . . . H13 H 0.6606 -0.177 0.2547 0.026 Uiso 1 calc R . . Zn1 Zn 0.65644(5) 0.31367(12) 0.24094(6) 0.01456(17) Uani 1 d . . . Zn2 Zn 0.49710(5) 0.33603(11) 0.58498(6) 0.01383(17) Uani 1 d . . . Zn3 Zn 0.67059(5) -0.05943(12) 0.43653(6) 0.01448(17) Uani 1 d . . . H1A H 0.894(4) -0.241(13) 0.3648(16) 0.022 Uiso 1 d D . . H1B H 0.864(3) -0.238(13) 0.463(4) 0.022 Uiso 1 d D . . H2A H 0.922(3) -0.048(9) 0.200(6) 0.022 Uiso 1 d D . . H2B H 0.952(4) 0.130(3) 0.153(2) 0.022 Uiso 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0140(3) 0.0106(3) 0.0137(3) -0.0001(2) 0.0022(2) -0.0004(2) As2 0.0137(3) 0.0135(3) 0.0159(3) -0.0003(3) 0.0023(2) -0.0003(2) As3 0.0140(3) 0.0110(3) 0.0151(3) -0.0001(2) 0.0023(2) -0.0003(2) Cs1 0.0222(2) 0.0193(2) 0.0205(2) 0.00225(16) 0.00457(17) 0.00206(16) O1 0.016(2) 0.012(2) 0.016(2) -0.0015(18) 0.0028(18) -0.0031(18) O2 0.017(2) 0.018(2) 0.016(2) 0.0016(19) 0.0052(18) 0.0012(19) O1W 0.019(3) 0.034(3) 0.019(3) -0.001(2) 0.005(2) 0.000(2) O3 0.014(2) 0.017(2) 0.016(2) 0.0009(19) 0.0010(18) 0.0005(18) O2W 0.022(3) 0.022(3) 0.028(3) 0.005(2) 0.003(2) -0.005(2) O4 0.015(2) 0.011(2) 0.014(2) -0.0048(17) 0.0029(17) -0.0034(17) O5 0.018(2) 0.019(3) 0.019(3) 0.002(2) 0.0013(19) 0.000(2) O6 0.015(2) 0.020(2) 0.020(3) -0.005(2) 0.0054(19) 0.0016(19) O7 0.015(2) 0.021(3) 0.017(2) 0.003(2) 0.0011(19) -0.0022(19) O8 0.018(2) 0.016(2) 0.022(3) 0.004(2) 0.0051(19) -0.0012(19) O9 0.016(2) 0.012(2) 0.018(3) -0.0023(18) 0.0009(18) -0.0021(18) O10 0.019(2) 0.011(2) 0.019(2) 0.0020(19) 0.0026(19) -0.0002(18) O11 0.019(2) 0.016(2) 0.013(2) 0.0005(19) 0.0047(18) -0.0022(19) O12 0.012(2) 0.013(2) 0.027(3) 0.001(2) 0.0019(19) 0.0017(18) O13 0.020(2) 0.018(2) 0.013(2) -0.0028(19) -0.0002(18) -0.0022(19) Zn1 0.0142(4) 0.0140(4) 0.0155(4) 0.0001(3) 0.0022(3) -0.0009(3) Zn2 0.0161(4) 0.0109(4) 0.0146(4) 0.0002(3) 0.0026(3) -0.0002(3) Zn3 0.0149(4) 0.0118(4) 0.0165(4) 0.0006(3) 0.0020(3) -0.0002(3) #------------------ MOLECULAR GEOMETRY --------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 O4 1.675(4) . ? As1 O2 1.683(5) . ? As1 O3 1.684(5) . ? As1 O1 1.689(5) . ? As2 O6 1.658(5) . ? As2 O5 1.663(5) . ? As2 O8 1.681(5) . ? As2 O7 1.752(5) . ? As3 O10 1.671(5) . ? As3 O11 1.675(5) . ? As3 O9 1.687(5) . ? As3 O12 1.736(5) . ? Cs1 H1A 3.36(8) . ? Cs1 H1B 3.36(8) . ? O1 Zn3 1.991(5) 3_666 ? O1 Zn2 2.058(5) 1_565 ? O2 Zn2 2.038(5) 2_656 ? O2 Zn1 2.056(5) 3_666 ? O1W H1A 0.84(2) . ? O1W H1B 0.85(2) . ? O3 Zn1 2.037(5) 4_576 ? O2W H2A 0.844(19) . ? O2W H2B 0.834(19) . ? O4 Zn2 2.051(5) . ? O4 Zn2 2.079(5) 3_666 ? O5 Zn3 1.969(5) . ? O6 Zn1 2.009(5) 4_566 ? O7 H7 0.84 . ? O8 H8 0.84 . ? O9 Zn1 2.080(5) . ? O9 Zn3 2.119(5) . ? O10 Zn3 2.081(5) 1_565 ? O10 Zn2 2.160(5) 3_666 ? O11 Zn1 2.068(5) 4_566 ? O11 Zn2 2.170(5) . ? O12 H12 0.84 . ? O13 Zn3 2.045(5) . ? O13 H13 0.84 . ? Zn1 O6 2.009(5) 4_565 ? Zn1 O3 2.037(5) 4_575 ? Zn1 O2 2.056(5) 3_666 ? Zn1 O11 2.068(5) 4_565 ? Zn1 Zn2 3.1553(11) 4_565 ? Zn2 O2 2.038(5) 2_646 ? Zn2 O1 2.058(5) 1_545 ? Zn2 O4 2.079(5) 3_666 ? Zn2 O10 2.160(5) 3_666 ? Zn2 Zn2 3.0925(15) 3_666 ? Zn2 Zn1 3.1553(11) 4_566 ? Zn3 O1 1.991(5) 3_666 ? Zn3 O10 2.081(5) 1_545 ? 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 O4 As1 O2 109.6(2) . . ? O4 As1 O3 110.0(2) . . ? O2 As1 O3 109.4(2) . . ? O4 As1 O1 107.0(2) . . ? O2 As1 O1 108.1(2) . . ? O3 As1 O1 112.6(2) . . ? O6 As2 O5 119.7(2) . . ? O6 As2 O8 112.0(2) . . ? O5 As2 O8 110.9(2) . . ? O6 As2 O7 105.9(2) . . ? O5 As2 O7 101.1(2) . . ? O8 As2 O7 105.5(2) . . ? O10 As3 O11 114.5(2) . . ? O10 As3 O9 110.8(2) . . ? O11 As3 O9 111.5(2) . . ? O10 As3 O12 108.2(2) . . ? O11 As3 O12 108.1(2) . . ? O9 As3 O12 102.9(2) . . ? H1A Cs1 H1B 24.6(6) . . ? As1 O1 Zn3 122.3(3) . 3_666 ? As1 O1 Zn2 123.6(2) . 1_565 ? Zn3 O1 Zn2 105.9(2) 3_666 1_565 ? As1 O2 Zn2 132.1(3) . 2_656 ? As1 O2 Zn1 127.1(3) . 3_666 ? Zn2 O2 Zn1 100.8(2) 2_656 3_666 ? H1A O1W H1B 116(4) . . ? As1 O3 Zn1 125.9(3) . 4_576 ? H2A O2W H2B 117(4) . . ? As1 O4 Zn2 139.8(3) . . ? As1 O4 Zn2 122.9(3) . 3_666 ? Zn2 O4 Zn2 96.99(18) . 3_666 ? As2 O5 Zn3 142.9(3) . . ? As2 O6 Zn1 130.1(3) . 4_566 ? As2 O7 H7 109.5 . . ? As2 O8 H8 109.5 . . ? As3 O9 Zn1 126.3(3) . . ? As3 O9 Zn3 115.9(3) . . ? Zn1 O9 Zn3 113.2(2) . . ? As3 O10 Zn3 141.1(3) . 1_565 ? As3 O10 Zn2 118.6(2) . 3_666 ? Zn3 O10 Zn2 99.30(19) 1_565 3_666 ? As3 O11 Zn1 142.7(3) . 4_566 ? As3 O11 Zn2 120.3(2) . . ? Zn1 O11 Zn2 96.21(19) 4_566 . ? As3 O12 H12 109.5 . . ? Zn3 O13 H13 109.5 . . ? O6 Zn1 O3 95.34(19) 4_565 4_575 ? O6 Zn1 O2 171.5(2) 4_565 3_666 ? O3 Zn1 O2 92.56(19) 4_575 3_666 ? O6 Zn1 O11 96.88(19) 4_565 4_565 ? O3 Zn1 O11 94.06(19) 4_575 4_565 ? O2 Zn1 O11 79.47(19) 3_666 4_565 ? O6 Zn1 O9 90.19(19) 4_565 . ? O3 Zn1 O9 119.53(19) 4_575 . ? O2 Zn1 O9 88.58(18) 3_666 . ? O11 Zn1 O9 144.92(19) 4_565 . ? O6 Zn1 Zn2 139.06(14) 4_565 4_565 ? O3 Zn1 Zn2 82.13(13) 4_575 4_565 ? O2 Zn1 Zn2 39.39(13) 3_666 4_565 ? O11 Zn1 Zn2 43.13(13) 4_565 4_565 ? O9 Zn1 Zn2 126.65(13) . 4_565 ? O2 Zn2 O4 99.25(19) 2_646 . ? O2 Zn2 O1 87.86(19) 2_646 1_545 ? O4 Zn2 O1 161.80(19) . 1_545 ? O2 Zn2 O4 159.61(18) 2_646 3_666 ? O4 Zn2 O4 83.01(19) . 3_666 ? O1 Zn2 O4 96.17(18) 1_545 3_666 ? O2 Zn2 O10 112.72(18) 2_646 3_666 ? O4 Zn2 O10 86.26(18) . 3_666 ? O1 Zn2 O10 75.54(18) 1_545 3_666 ? O4 Zn2 O10 87.61(18) 3_666 3_666 ? O2 Zn2 O11 77.52(18) 2_646 . ? O4 Zn2 O11 92.53(18) . . ? O1 Zn2 O11 105.41(18) 1_545 . ? O4 Zn2 O11 82.14(17) 3_666 . ? O10 Zn2 O11 169.75(18) 3_666 . ? O2 Zn2 Zn2 137.45(15) 2_646 3_666 ? O4 Zn2 Zn2 41.85(13) . 3_666 ? O1 Zn2 Zn2 134.61(14) 1_545 3_666 ? O4 Zn2 Zn2 41.16(12) 3_666 3_666 ? O10 Zn2 Zn2 85.91(13) 3_666 3_666 ? O11 Zn2 Zn2 86.41(13) . 3_666 ? O2 Zn2 Zn1 39.81(13) 2_646 4_566 ? O4 Zn2 Zn1 109.29(13) . 4_566 ? O1 Zn2 Zn1 86.91(13) 1_545 4_566 ? O4 Zn2 Zn1 120.26(13) 3_666 4_566 ? O10 Zn2 Zn1 148.80(13) 3_666 4_566 ? O11 Zn2 Zn1 40.66(12) . 4_566 ? Zn2 Zn2 Zn1 123.90(4) 3_666 4_566 ? O5 Zn3 O1 148.2(2) . 3_666 ? O5 Zn3 O13 107.4(2) . . ? O1 Zn3 O13 104.33(19) 3_666 . ? O5 Zn3 O10 99.84(19) . 1_545 ? O1 Zn3 O10 78.77(19) 3_666 1_545 ? O13 Zn3 O10 93.05(19) . 1_545 ? O5 Zn3 O9 90.11(19) . . ? O1 Zn3 O9 93.06(19) 3_666 . ? O13 Zn3 O9 83.38(19) . . ? O10 Zn3 O9 170.04(18) 1_545 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O7 H7 O2W 3_756 0.84 1.82 2.592(7) 151 O8 H8 O13 4_556 0.84 1.9 2.706(7) 160.5 O12 H12 O6 . 0.84 2.6 3.333(7) 147.2 O13 H13 O3 4_565 0.84 1.85 2.651(7) 158.9 O1W H1A O8 4 0.84(2) 2.06(3) 2.882(7) 166(6) O1W H1B O5 . 0.85(2) 2.16(5) 2.914(7) 148(8) O2W H2A O8 4 0.844(19) 1.84(2) 2.685(7) 176(9) O2W H2B O7 4_565 0.834(19) 2.12(2) 2.838(7) 144(3) #===END