Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email PL@ST-AND.AC.UK _publ_contact_author_name 'Dr Philip Lightfoot' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name P.Lightfoot T.A.Bowden H.L.Milton A.M.Z.Slawin data_I _database_code_CSD 197595 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H4 O4 Zn' _chemical_formula_weight 181.44 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 7.585(3) _cell_length_b 5.9843(14) _cell_length_c 6.253(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.51(3) _cell_angle_gamma 90.00 _cell_volume 269.12(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 180 _exptl_absorpt_coefficient_mu 4.488 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max 1.000 _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 'Mercury CCD (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 453 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 4.43 _diffrn_reflns_theta_max 24.71 _reflns_number_total 328 _reflns_number_gt 326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.1800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.20(4) _refine_ls_number_reflns 328 _refine_ls_number_parameters 42 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0240 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0624 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.153 _refine_ls_shift/su_mean 0.021 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 1.0000 0.9956 0.0000 0.0170(3) Uani 1 2 d S . . O2 O 1.0034(5) 0.8027(8) 0.2512(6) 0.0274(9) Uani 1 1 d . . . C1 C 0.9030(6) 0.489(2) 0.4137(8) 0.0197(10) Uani 1 1 d . . . H1A H 0.8845 0.3465 0.3321 0.025 Uiso 1 1 calc R . . H1B H 0.8111 0.4978 0.4897 0.025 Uiso 1 1 calc R . . C2 C 0.8688(8) 0.6747(10) 0.2424(10) 0.0166(12) Uani 1 1 d . . . O1 O 0.7112(5) 0.6984(7) 0.0971(6) 0.0249(9) 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 0.0112(4) 0.0203(4) 0.0165(4) 0.000 -0.0002(3) 0.000 O2 0.015(2) 0.037(2) 0.025(2) 0.009(2) -0.0012(16) -0.013(2) C1 0.019(3) 0.019(3) 0.016(2) 0.001(8) -0.0028(18) -0.003(8) C2 0.015(3) 0.017(3) 0.017(3) 0.004(3) 0.004(2) 0.001(2) O1 0.014(2) 0.027(2) 0.026(2) 0.0079(17) -0.0054(16) -0.0004(17) _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 O2 1.942(4) 2_755 ? Zn1 O2 1.942(4) . ? Zn1 O1 1.947(4) 3 ? Zn1 O1 1.947(4) 4_655 ? O2 C2 1.263(7) . ? C1 C2 1.508(14) . ? C1 C1 1.523(9) 2_756 ? C2 O1 1.259(7) . ? O1 Zn1 1.947(4) 3_445 ? 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 Zn1 O2 107.1(3) 2_755 . ? O2 Zn1 O1 114.90(16) 2_755 3 ? O2 Zn1 O1 108.65(16) . 3 ? O2 Zn1 O1 108.65(16) 2_755 4_655 ? O2 Zn1 O1 114.90(16) . 4_655 ? O1 Zn1 O1 102.9(2) 3 4_655 ? C2 O2 Zn1 121.5(4) . . ? C2 C1 C1 114.4(4) . 2_756 ? O1 C2 O2 122.1(5) . . ? O1 C2 C1 120.4(5) . . ? O2 C2 C1 117.5(5) . . ? C2 O1 Zn1 130.8(4) . 3_445 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Zn1 O2 C2 -64.4(4) 2_755 . . . ? O1 Zn1 O2 C2 170.9(4) 3 . . . ? O1 Zn1 O2 C2 56.4(5) 4_655 . . . ? Zn1 O2 C2 O1 -16.1(8) . . . . ? Zn1 O2 C2 C1 163.7(6) . . . . ? C1 C1 C2 O1 -176.8(5) 2_756 . . . ? C1 C1 C2 O2 3.3(8) 2_756 . . . ? O2 C2 O1 Zn1 164.4(4) . . . 3_445 ? C1 C2 O1 Zn1 -15.5(8) . . . 3_445 ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.312 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.083 #===END data_II _database_code_CSD 197596 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H4 O4 Zn' _chemical_formula_weight 181.44 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M '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 6.922(4) _cell_length_b 6.787(4) _cell_length_c 11.267(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.285(9) _cell_angle_gamma 90.00 _cell_volume 522.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.31 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 4.627 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.594261 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1211 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 23.37 _reflns_number_total 380 _reflns_number_gt 376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0903P)^2^+0.8475P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 380 _refine_ls_number_parameters 50 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.008 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 0.5000 0.01706(10) 0.7500 0.0109(5) Uani 1 2 d S . . C1 C 0.4013(11) 0.5056(7) 0.9582(7) 0.0131(15) Uani 1 1 d . . . O1 O 0.4853(4) 0.1926(5) 0.8861(3) 0.0147(9) Uani 1 1 d . . . O2 O 0.7134(4) -0.1709(5) 0.7933(3) 0.0151(9) Uani 1 1 d . . . C2 C 0.3634(6) 0.3332(7) 0.8745(4) 0.0109(11) Uani 1 1 d . . . H1 H 0.392(9) 0.634(12) 0.910(6) 0.035(19) Uiso 1 1 d . . . H2 H 0.307(13) 0.520(7) 0.997(7) 0.01(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0091(7) 0.0066(7) 0.0151(8) 0.000 -0.0042(5) 0.000 C1 0.009(4) 0.012(3) 0.016(3) -0.0010(18) -0.004(3) 0.0017(15) O1 0.0143(16) 0.0097(19) 0.0188(17) -0.0014(14) -0.0009(12) 0.0021(14) O2 0.0107(15) 0.011(2) 0.0210(18) -0.0042(14) -0.0066(13) 0.0029(13) C2 0.006(2) 0.011(3) 0.016(2) 0.004(2) 0.0036(17) 0.002(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 O2 1.953(3) 6_657 ? Zn1 O2 1.953(3) . ? Zn1 O1 1.958(3) . ? Zn1 O1 1.958(3) 6_657 ? C1 C2 1.500(8) . ? C1 C1 1.530(15) 5_667 ? O1 C2 1.266(6) . ? O2 C2 1.269(6) 3_545 ? C2 O2 1.269(6) 3_455 ? 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 Zn1 O2 98.4(2) 6_657 . ? O2 Zn1 O1 117.40(13) 6_657 . ? O2 Zn1 O1 109.56(12) . . ? O2 Zn1 O1 109.56(12) 6_657 6_657 ? O2 Zn1 O1 117.40(13) . 6_657 ? O1 Zn1 O1 105.04(19) . 6_657 ? C2 C1 C1 113.3(6) . 5_667 ? C2 O1 Zn1 119.7(3) . . ? C2 O2 Zn1 131.6(3) 3_545 . ? O1 C2 O2 120.8(5) . 3_455 ? O1 C2 C1 118.5(4) . . ? O2 C2 C1 120.7(4) 3_455 . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 23.37 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.937 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.188 #===END data_III _database_code_CSD 197597 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H8 K2 O8 Zn' _chemical_formula_weight 375.71 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'I2/a ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 7.402(3) _cell_length_b 21.346(7) _cell_length_c 8.013(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.26(3) _cell_angle_gamma 90.00 _cell_volume 1215.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Platelet _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 2.737 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.6741 _exptl_absorpt_correction_T_max 1.00000 _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 'Mercury CCD (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2406 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0849 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 24.69 _reflns_number_total 982 _reflns_number_gt 655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 982 _refine_ls_number_parameters 104 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.2500 0.13831(4) 0.5000 0.0211(3) Uani 1 2 d S . . K1 K 0.2500 0.05052(7) 0.0000 0.0268(4) Uani 1 2 d S . . K2 K 0.7500 -0.03426(7) 0.5000 0.0316(5) Uani 1 2 d S . . O1 O -0.4537(5) 0.19815(15) 0.4068(5) 0.0315(10) Uani 1 1 d . . . O2 O -0.6259(5) 0.11615(18) 0.2924(5) 0.0342(11) Uani 1 1 d . . . O3 O -0.1601(5) 0.07873(15) 0.3536(4) 0.0283(10) Uani 1 1 d . . . O4 O -0.0437(5) 0.05197(16) 0.1403(4) 0.0268(9) Uani 1 1 d . . . C1 C -0.6070(8) 0.1735(3) 0.3197(7) 0.0246(13) Uani 1 1 d . . . C2 C -0.7715(9) 0.2155(3) 0.2505(9) 0.0317(16) Uani 1 1 d . . . C3 C -0.1426(7) 0.0870(2) 0.1996(7) 0.0186(12) Uani 1 1 d . . . C4 C -0.2503(9) 0.1398(3) 0.0935(6) 0.0219(13) Uani 1 1 d . . . H1 H -0.859(8) 0.207(2) 0.320(7) 0.036(17) Uiso 1 1 d . . . H2 H -0.825(7) 0.199(2) 0.129(7) 0.037(16) Uiso 1 1 d . . . H3 H -0.210(6) 0.174(2) 0.154(6) 0.016(14) Uiso 1 1 d . . . H4 H -0.385(7) 0.1412(19) 0.109(6) 0.019(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0231(6) 0.0219(5) 0.0192(6) 0.000 0.0072(4) 0.000 K1 0.0284(11) 0.0282(9) 0.0258(10) 0.000 0.0107(8) 0.000 K2 0.0370(12) 0.0276(10) 0.0340(11) 0.000 0.0160(9) 0.000 O1 0.021(2) 0.029(2) 0.039(3) -0.0027(18) 0.001(2) 0.0039(17) O2 0.037(3) 0.026(2) 0.037(3) -0.0017(17) 0.005(2) -0.0002(18) O3 0.041(3) 0.027(2) 0.022(2) 0.0023(17) 0.017(2) 0.0077(18) O4 0.026(2) 0.033(2) 0.025(2) -0.0016(18) 0.0129(18) 0.0080(19) C1 0.018(3) 0.033(4) 0.024(4) 0.004(3) 0.009(3) 0.000(3) C2 0.022(4) 0.034(3) 0.037(4) -0.003(3) 0.004(3) 0.001(3) C3 0.017(3) 0.020(3) 0.015(3) -0.001(2) -0.001(3) -0.006(2) C4 0.028(4) 0.023(3) 0.015(3) -0.004(2) 0.007(3) 0.001(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 Zn1 O1 1.957(3) 2_456 ? Zn1 O1 1.957(3) . ? Zn1 O3 1.968(3) 2_456 ? Zn1 O3 1.968(3) . ? Zn1 K2 3.684(2) 1_455 ? K1 O2 2.663(4) 1_655 ? K1 O2 2.663(4) 2_455 ? K1 O4 2.713(4) 2 ? K1 O4 2.713(4) . ? K1 O4 2.724(4) 5 ? K1 O4 2.724(4) 6_655 ? K1 C3 3.331(5) 5 ? K1 C3 3.331(5) 6_655 ? K1 K2 4.0213(13) 5_655 ? K1 K2 4.0213(13) 5_656 ? K1 K1 4.283(2) 5 ? K1 K1 4.283(2) 5_655 ? K2 O2 2.743(4) 6_755 ? K2 O2 2.743(4) 5_556 ? K2 O3 2.841(4) 2_556 ? K2 O3 2.841(4) 1_655 ? K2 O3 3.081(4) 6_655 ? K2 O3 3.081(4) 5_656 ? K2 O4 3.109(4) 6_655 ? K2 O4 3.109(4) 5_656 ? K2 C3 3.404(5) 6_655 ? K2 C3 3.404(5) 5_656 ? K2 Zn1 3.684(2) 1_655 ? K2 K2 3.9793(16) 5_756 ? O1 C1 1.268(6) . ? O2 C1 1.245(6) . ? O2 K1 2.663(4) 1_455 ? O2 K2 2.743(4) 5_556 ? O3 C3 1.289(6) . ? O3 K2 2.841(4) 1_455 ? O3 K2 3.081(4) 5_656 ? O4 C3 1.231(6) . ? O4 K1 2.724(4) 5 ? O4 K2 3.109(4) 5_656 ? C1 C2 1.488(7) . ? C2 C2 1.509(12) 7_355 ? C3 C4 1.499(7) . ? C3 K1 3.331(5) 5 ? C3 K2 3.404(5) 5_656 ? C4 C4 1.500(10) 2_455 ? 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 O1 98.5(2) 2_456 . ? O1 Zn1 O3 123.18(15) 2_456 2_456 ? O1 Zn1 O3 107.23(16) . 2_456 ? O1 Zn1 O3 107.23(16) 2_456 . ? O1 Zn1 O3 123.18(15) . . ? O3 Zn1 O3 99.5(2) 2_456 . ? O1 Zn1 K2 130.74(11) 2_456 1_455 ? O1 Zn1 K2 130.74(11) . 1_455 ? O3 Zn1 K2 49.75(10) 2_456 1_455 ? O3 Zn1 K2 49.75(10) . 1_455 ? O2 K1 O2 116.50(18) 1_655 2_455 ? O2 K1 O4 103.85(11) 1_655 2 ? O2 K1 O4 75.44(12) 2_455 2 ? O2 K1 O4 75.44(12) 1_655 . ? O2 K1 O4 103.85(11) 2_455 . ? O4 K1 O4 178.70(15) 2 . ? O2 K1 O4 143.24(12) 1_655 5 ? O2 K1 O4 92.53(11) 2_455 5 ? O4 K1 O4 105.06(10) 2 5 ? O4 K1 O4 76.02(11) . 5 ? O2 K1 O4 92.53(11) 1_655 6_655 ? O2 K1 O4 143.24(12) 2_455 6_655 ? O4 K1 O4 76.02(11) 2 6_655 ? O4 K1 O4 105.06(10) . 6_655 ? O4 K1 O4 73.13(15) 5 6_655 ? O2 K1 C3 149.68(12) 1_655 5 ? O2 K1 C3 93.68(12) 2_455 5 ? O4 K1 C3 85.55(11) 2 5 ? O4 K1 C3 95.60(14) . 5 ? O4 K1 C3 20.47(11) 5 5 ? O4 K1 C3 61.39(12) 6_655 5 ? O2 K1 C3 93.68(12) 1_655 6_655 ? O2 K1 C3 149.68(12) 2_455 6_655 ? O4 K1 C3 95.60(14) 2 6_655 ? O4 K1 C3 85.55(11) . 6_655 ? O4 K1 C3 61.39(12) 5 6_655 ? O4 K1 C3 20.47(11) 6_655 6_655 ? C3 K1 C3 56.39(17) 5 6_655 ? O2 K1 K2 145.66(10) 1_655 5_655 ? O2 K1 K2 42.71(9) 2_455 5_655 ? O4 K1 K2 50.55(7) 2 5_655 ? O4 K1 K2 129.60(8) . 5_655 ? O4 K1 K2 71.09(8) 5 5_655 ? O4 K1 K2 100.68(8) 6_655 5_655 ? C3 K1 K2 60.81(9) 5 5_655 ? C3 K1 K2 109.60(10) 6_655 5_655 ? O2 K1 K2 42.71(9) 1_655 5_656 ? O2 K1 K2 145.66(10) 2_455 5_656 ? O4 K1 K2 129.60(8) 2 5_656 ? O4 K1 K2 50.55(7) . 5_656 ? O4 K1 K2 100.68(8) 5 5_656 ? O4 K1 K2 71.09(8) 6_655 5_656 ? C3 K1 K2 109.60(10) 5 5_656 ? C3 K1 K2 60.81(9) 6_655 5_656 ? K2 K1 K2 170.09(6) 5_655 5_656 ? O2 K1 K1 110.50(9) 1_655 5 ? O2 K1 K1 100.35(8) 2_455 5 ? O4 K1 K1 142.97(9) 2 5 ? O4 K1 K1 38.10(7) . 5 ? O4 K1 K1 37.92(8) 5 5 ? O4 K1 K1 88.85(9) 6_655 5 ? C3 K1 K1 57.73(10) 5 5 ? C3 K1 K1 69.29(10) 6_655 5 ? K2 K1 K1 101.40(3) 5_655 5 ? K2 K1 K1 73.47(3) 5_656 5 ? O2 K1 K1 100.35(8) 1_655 5_655 ? O2 K1 K1 110.50(9) 2_455 5_655 ? O4 K1 K1 38.10(7) 2 5_655 ? O4 K1 K1 142.97(9) . 5_655 ? O4 K1 K1 88.85(9) 5 5_655 ? O4 K1 K1 37.92(8) 6_655 5_655 ? C3 K1 K1 69.29(10) 5 5_655 ? C3 K1 K1 57.73(10) 6_655 5_655 ? K2 K1 K1 73.47(3) 5_655 5_655 ? K2 K1 K1 101.40(3) 5_656 5_655 ? K1 K1 K1 119.53(8) 5 5_655 ? O2 K2 O2 100.82(17) 6_755 5_556 ? O2 K2 O3 161.50(12) 6_755 2_556 ? O2 K2 O3 97.68(11) 5_556 2_556 ? O2 K2 O3 97.68(11) 6_755 1_655 ? O2 K2 O3 161.50(12) 5_556 1_655 ? O3 K2 O3 63.83(15) 2_556 1_655 ? O2 K2 O3 91.97(11) 6_755 6_655 ? O2 K2 O3 64.72(10) 5_556 6_655 ? O3 K2 O3 95.68(9) 2_556 6_655 ? O3 K2 O3 115.09(11) 1_655 6_655 ? O2 K2 O3 64.72(10) 6_755 5_656 ? O2 K2 O3 91.97(11) 5_556 5_656 ? O3 K2 O3 115.09(11) 2_556 5_656 ? O3 K2 O3 95.68(9) 1_655 5_656 ? O3 K2 O3 144.11(14) 6_655 5_656 ? O2 K2 O4 68.05(10) 6_755 6_655 ? O2 K2 O4 102.63(10) 5_556 6_655 ? O3 K2 O4 107.58(10) 2_556 6_655 ? O3 K2 O4 84.51(10) 1_655 6_655 ? O3 K2 O4 41.51(9) 6_655 6_655 ? O3 K2 O4 132.37(10) 5_656 6_655 ? O2 K2 O4 102.63(10) 6_755 5_656 ? O2 K2 O4 68.05(10) 5_556 5_656 ? O3 K2 O4 84.51(10) 2_556 5_656 ? O3 K2 O4 107.58(10) 1_655 5_656 ? O3 K2 O4 132.37(10) 6_655 5_656 ? O3 K2 O4 41.51(9) 5_656 5_656 ? O4 K2 O4 166.03(13) 6_655 5_656 ? O2 K2 C3 74.03(12) 6_755 6_655 ? O2 K2 C3 81.58(12) 5_556 6_655 ? O3 K2 C3 108.69(11) 2_556 6_655 ? O3 K2 C3 103.95(12) 1_655 6_655 ? O3 K2 C3 22.21(10) 6_655 6_655 ? O3 K2 C3 136.21(11) 5_656 6_655 ? O4 K2 C3 21.17(10) 6_655 6_655 ? O4 K2 C3 148.44(12) 5_656 6_655 ? O2 K2 C3 81.58(12) 6_755 5_656 ? O2 K2 C3 74.03(12) 5_556 5_656 ? O3 K2 C3 103.95(12) 2_556 5_656 ? O3 K2 C3 108.69(11) 1_655 5_656 ? O3 K2 C3 136.21(11) 6_655 5_656 ? O3 K2 C3 22.21(10) 5_656 5_656 ? O4 K2 C3 148.44(12) 6_655 5_656 ? O4 K2 C3 21.17(10) 5_656 5_656 ? C3 K2 C3 141.36(17) 6_655 5_656 ? O2 K2 Zn1 129.59(9) 6_755 1_655 ? O2 K2 Zn1 129.59(9) 5_556 1_655 ? O3 K2 Zn1 31.92(7) 2_556 1_655 ? O3 K2 Zn1 31.92(7) 1_655 1_655 ? O3 K2 Zn1 107.94(7) 6_655 1_655 ? O3 K2 Zn1 107.94(7) 5_656 1_655 ? O4 K2 Zn1 96.98(7) 6_655 1_655 ? O4 K2 Zn1 96.98(7) 5_656 1_655 ? C3 K2 Zn1 109.32(8) 6_655 1_655 ? C3 K2 Zn1 109.32(8) 5_656 1_655 ? O2 K2 K2 76.39(8) 6_755 5_756 ? O2 K2 K2 134.72(8) 5_556 5_756 ? O3 K2 K2 90.77(9) 2_556 5_756 ? O3 K2 K2 50.40(8) 1_655 5_756 ? O3 K2 K2 158.46(7) 6_655 5_756 ? O3 K2 K2 45.28(7) 5_656 5_756 ? O4 K2 K2 116.97(7) 6_655 5_756 ? O4 K2 K2 68.64(7) 5_656 5_756 ? C3 K2 K2 136.99(10) 6_655 5_756 ? C3 K2 K2 60.79(9) 5_656 5_756 ? Zn1 K2 K2 68.44(4) 1_655 5_756 ? C1 O1 Zn1 114.5(3) . . ? C1 O2 K1 131.8(3) . 1_455 ? C1 O2 K2 124.1(4) . 5_556 ? K1 O2 K2 96.12(13) 1_455 5_556 ? C3 O3 Zn1 128.6(3) . . ? C3 O3 K2 127.6(3) . 1_455 ? Zn1 O3 K2 98.34(14) . 1_455 ? C3 O3 K2 93.1(3) . 5_656 ? Zn1 O3 K2 115.71(14) . 5_656 ? K2 O3 K2 84.32(9) 1_455 5_656 ? C3 O4 K1 143.0(3) . . ? C3 O4 K1 108.8(3) . 5 ? K1 O4 K1 103.98(11) . 5 ? C3 O4 K2 93.0(3) . 5_656 ? K1 O4 K2 87.09(10) . 5_656 ? K1 O4 K2 116.77(12) 5 5_656 ? O2 C1 O1 122.9(5) . . ? O2 C1 C2 119.1(5) . . ? O1 C1 C2 117.9(5) . . ? C1 C2 C2 116.0(6) . 7_355 ? O4 C3 O3 121.1(5) . . ? O4 C3 C4 121.1(5) . . ? O3 C3 C4 117.8(5) . . ? O4 C3 K1 50.7(2) . 5 ? O3 C3 K1 105.3(3) . 5 ? C4 C3 K1 111.9(3) . 5 ? O4 C3 K2 65.8(3) . 5_656 ? O3 C3 K2 64.7(3) . 5_656 ? C4 C3 K2 149.6(3) . 5_656 ? K1 C3 K2 95.14(13) 5 5_656 ? C3 C4 C4 114.6(4) . 2_455 ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.414 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.127