Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guo-Cong Guo' _publ_contact_author_address ; Fujian Institute of Research on the Structure of Matter Chinese Academy of Science Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email GCGUO@MS.FJIRSM.AC.CN _publ_section_title ; Synthesis, crystal and band structures, and optical properties of a new mixed-framework mercury selenide diselenite, (Hg3Se2)(Se2O5) ; loop_ _publ_author_name 'Guo-Cong Guo' 'Sheng-Ping Guo' 'Jin-Shun Huang' 'Ying-Bing Lu' ; Ming-Sheng Wan ; 'Ke-Jun Wu' 'Jian-Ping Zou' data_2 _database_code_depnum_ccdc_archive 'CCDC 646333' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'Hg3 O5 Se4' _chemical_formula_sum 'Hg3 O5 Se4' _chemical_formula_weight 997.61 _symmetry_space_group_name_Hall '-P 1' 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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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 7.487(2) _cell_length_b 7.7626(12) _cell_length_c 9.0689(18) _cell_angle_alpha 95.528(16) _cell_angle_beta 108.55(2) _cell_angle_gamma 107.759(16) _cell_volume 464.87(18) _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 light-green _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 7.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 65.052 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.6353 _exptl_absorpt_correction_T_max 0.9903 _exptl_absorpt_process_details 'Psi (Rigaku WinAFC)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1815 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.04 _reflns_number_total 1650 _reflns_number_gt 1363 _reflns_threshold_expression >2sigma(I) _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction 'CrystalStructure Version 3.10' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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. The instruction "isor 0.01 0.02 o1 o3" is used for giving reasonable displacement parameter for O1 and O3 atoms ; _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^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00207(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1650 _refine_ls_number_parameters 110 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.003 _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 Hg1 Hg 0.01806(5) 0.98760(5) 0.75872(5) 0.02318(10) Uani 1 1 d . . . Hg2 Hg 0.00756(6) 0.47625(5) 0.71666(5) 0.02471(11) Uani 1 1 d . . . Hg3 Hg -0.27368(6) 1.18436(5) 0.91213(4) 0.02845(11) Uani 1 1 d . . . Se1 Se 0.24915(13) 0.80678(12) 0.80504(11) 0.0175(2) Uani 1 1 d . . . Se2 Se -0.22861(13) 1.14516(12) 0.64966(11) 0.0181(2) Uani 1 1 d . . . Se3 Se -0.34846(13) 1.63705(12) 0.90941(10) 0.0145(2) Uani 1 1 d . . . Se4 Se -0.62267(13) 1.33064(12) 0.60511(10) 0.0174(2) Uani 1 1 d . . . O1 O -0.2045(9) 1.8549(8) 0.9266(8) 0.0185(17) Uani 1 1 d U . . O2 O -0.1798(10) 1.5366(9) 0.9715(9) 0.033(2) Uani 1 1 d . . . O3 O -0.4265(10) 1.5571(9) 0.6928(7) 0.0228(18) Uani 1 1 d U . . O4 O -0.6350(10) 1.2614(10) 0.7708(8) 0.030(2) Uani 1 1 d . . . O5 O -0.8252(10) 1.3855(11) 0.5313(8) 0.032(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 Hg1 0.02179(16) 0.02119(17) 0.02664(17) 0.00501(14) 0.00575(14) 0.01109(13) Hg2 0.02475(18) 0.01661(17) 0.02979(18) 0.00512(14) 0.00864(15) 0.00469(14) Hg3 0.04149(19) 0.02653(18) 0.02429(17) 0.00861(14) 0.01643(15) 0.01595(16) Se1 0.0156(4) 0.0161(4) 0.0234(4) 0.0058(3) 0.0092(3) 0.0066(3) Se2 0.0164(4) 0.0170(4) 0.0186(4) 0.0031(3) 0.0035(3) 0.0060(3) Se3 0.0127(4) 0.0129(4) 0.0157(4) 0.0021(3) 0.0051(3) 0.0022(3) Se4 0.0166(4) 0.0182(4) 0.0151(4) 0.0006(3) 0.0055(3) 0.0045(3) O1 0.015(3) 0.008(2) 0.030(3) 0.004(2) 0.003(2) 0.006(2) O2 0.023(3) 0.025(3) 0.045(4) 0.014(3) -0.003(3) 0.013(3) O3 0.033(3) 0.017(3) 0.012(2) 0.008(2) 0.008(2) -0.001(2) O4 0.021(3) 0.033(4) 0.029(3) 0.006(3) 0.009(3) -0.001(3) O5 0.017(3) 0.067(5) 0.018(3) 0.017(3) 0.007(2) 0.020(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 Hg1 Se1 2.5046(12) . ? Hg1 Se2 2.5168(12) . ? Hg1 O1 2.650(7) 1_545 ? Hg2 Se2 2.5189(11) 1_545 ? Hg2 Se1 2.5195(11) . ? Hg2 O5 2.557(8) 1_645 ? Hg3 Se1 2.5051(12) 2_577 ? Hg3 Se2 2.5113(12) . ? Hg3 O2 2.562(7) . ? Se1 Hg3 2.5051(12) 2_577 ? Se2 Hg2 2.5189(11) 1_565 ? Se3 O2 1.659(8) . ? Se3 O1 1.666(6) . ? Se3 O3 1.844(6) . ? Se4 O5 1.653(8) . ? Se4 O4 1.664(8) . ? Se4 O3 1.815(6) . ? O1 Hg1 2.650(7) 1_565 ? O5 Hg2 2.557(8) 1_465 ? 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 Se1 Hg1 Se2 167.58(4) . . ? Se1 Hg1 O1 101.60(15) . 1_545 ? Se2 Hg1 O1 86.17(15) . 1_545 ? Se2 Hg2 Se1 175.77(4) 1_545 . ? Se2 Hg2 O5 89.48(17) 1_545 1_645 ? Se1 Hg2 O5 93.23(17) . 1_645 ? Se1 Hg3 Se2 165.82(4) 2_577 . ? Se1 Hg3 O2 87.80(19) 2_577 . ? Se2 Hg3 O2 98.7(2) . . ? Hg1 Se1 Hg3 92.27(4) . 2_577 ? Hg1 Se1 Hg2 102.75(4) . . ? Hg3 Se1 Hg2 92.01(4) 2_577 . ? Hg3 Se2 Hg1 89.81(4) . . ? Hg3 Se2 Hg2 91.35(4) . 1_565 ? Hg1 Se2 Hg2 100.46(4) . 1_565 ? O2 Se3 O1 102.5(3) . . ? O2 Se3 O3 99.1(4) . . ? O1 Se3 O3 98.4(3) . . ? O5 Se4 O4 105.2(4) . . ? O5 Se4 O3 101.8(4) . . ? O4 Se4 O3 99.3(3) . . ? Se3 O1 Hg1 128.9(3) . 1_565 ? Se3 O2 Hg3 122.4(3) . . ? Se4 O3 Se3 116.1(4) . . ? Se4 O5 Hg2 119.5(3) . 1_465 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.838 _refine_diff_density_min -2.315 _refine_diff_density_rms 0.435