# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Saet Byeol Kim' 'Kang Min Ok Dong Woo Lee' _publ_contact_author_name 'Ok, Kang Min' _publ_contact_author_email kmok@cau.ac.kr data_ZnIO3(OH) _database_code_depnum_ccdc_archive 'CCDC 867888' #TrackingRef '- ZnIO3(OH).cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'H I O4 Zn' _chemical_formula_weight 257.28 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc _cell_length_a 4.67670(10) _cell_length_b 11.2392(4) _cell_length_c 6.3308(2) _cell_angle_alpha 90 _cell_angle_beta 90.019(2) _cell_angle_gamma 90 _cell_volume 332.762(17) _cell_formula_units_Z 4 _cell_measurement_temperature 200.0(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 5.135 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.132 _exptl_crystal_size_mid 0.026 _exptl_crystal_size_min 0.024 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 16.493 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_process_details ; SADABS(Blessing, 1995) ; _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 0.67 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'Bruker SMART BREEZE' _diffrn_measurement_method CCD _diffrn_ambient_temperature 200.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_unetI/netI 0.0405 _diffrn_reflns_number 2881 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 4.72 _diffrn_reflns_theta_max 28.27 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 762 _reflns_number_gt 749 _reflns_threshold_expression >2\(I) _cell_measurement_reflns_used omega_scan _cell_measurement_theta_min 4.72 _cell_measurement_theta_max 28.27 #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0598P)^2^+6.6295P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0049(10) _refine_ls_number_reflns 762 _refine_ls_number_parameters 61 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.58(10) _refine_diff_density_max 1.809 _refine_diff_density_min -1.671 _refine_diff_density_rms 0.379 #----------------------------------------------------------------------------# # 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 O O 0.0106 0.006 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.4659 0.30504(4) 0.3551 0.0066(2) Uani 1 1 d . . . Zn1 Zn -0.0347(9) 0.4988(3) 0.1038(5) 0.0097(3) Uani 1 1 d . . . O1 O 0.258(2) 0.4434(8) 0.3545(13) 0.0163(19) Uani 1 1 d . . . O2 O 0.698(2) 0.3436(9) 0.5699(13) 0.019(2) Uani 1 1 d . . . O3 O 0.234(2) 0.3413(8) 0.5715(14) 0.0171(19) Uani 1 1 d . . . O4 O -0.204(2) 0.4121(8) -0.1468(13) 0.0140(17) Uani 1 1 d . . . H1 H -0.30(3) 0.335(13) -0.14(2) 0.00(3) 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 I1 0.0074(4) 0.0055(3) 0.0070(3) 0.0003(4) 0.00006(19) -0.0011(6) Zn1 0.0128(6) 0.0082(5) 0.0082(4) -0.0013(3) -0.0004(4) -0.0005(3) O1 0.012(4) 0.019(5) 0.018(4) -0.002(3) 0.001(3) 0.003(4) O2 0.028(6) 0.018(5) 0.010(3) 0.002(3) -0.009(4) -0.004(4) O3 0.022(5) 0.015(4) 0.015(4) -0.001(3) 0.007(4) 0.001(4) O4 0.016(5) 0.013(4) 0.013(4) 0.002(3) -0.004(3) 0.004(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 I1 O2 1.794(9) . ? I1 O3 1.795(9) . ? I1 O1 1.833(9) . ? Zn1 O4 2.023(10) . ? Zn1 O4 2.031(10) 2_565 ? Zn1 O2 2.178(11) 2_464 ? Zn1 O1 2.186(10) . ? Zn1 O1 2.189(9) 2_564 ? Zn1 O3 2.202(10) 2_564 ? O1 O3 1.793(13) . ? O1 Zn1 2.189(9) 2_565 ? O2 Zn1 2.178(11) 2_665 ? O3 Zn1 2.202(10) 2_565 ? O4 Zn1 2.031(10) 2_564 ? 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 I1 O3 74.5(5) . . ? O2 I1 O1 96.7(4) . . ? O3 I1 O1 59.2(4) . . ? O4 Zn1 O4 134.0(5) . 2_565 ? O4 Zn1 O2 95.2(4) . 2_464 ? O4 Zn1 O2 56.7(3) 2_565 2_464 ? O4 Zn1 O1 132.6(4) . . ? O4 Zn1 O1 79.7(4) 2_565 . ? O2 Zn1 O1 131.5(4) 2_464 . ? O4 Zn1 O1 79.8(4) . 2_564 ? O4 Zn1 O1 131.2(4) 2_565 2_564 ? O2 Zn1 O1 92.6(4) 2_464 2_564 ? O1 Zn1 O1 102.5(5) . 2_564 ? O4 Zn1 O3 122.9(4) . 2_564 ? O4 Zn1 O3 83.8(3) 2_565 2_564 ? O2 Zn1 O3 69.7(4) 2_464 2_564 ? O1 Zn1 O3 86.7(4) . 2_564 ? O1 Zn1 O3 48.2(4) 2_564 2_564 ? O3 O1 I1 59.3(4) . . ? O3 O1 Zn1 134.3(6) . . ? I1 O1 Zn1 125.1(4) . . ? O3 O1 Zn1 66.3(4) . 2_565 ? I1 O1 Zn1 125.6(5) . 2_565 ? Zn1 O1 Zn1 92.7(4) . 2_565 ? I1 O2 Zn1 128.2(5) . 2_665 ? O1 O3 I1 61.5(4) . . ? O1 O3 Zn1 65.5(4) . 2_565 ? I1 O3 Zn1 127.0(5) . 2_565 ? Zn1 O4 Zn1 102.7(4) . 2_564 ? #===END