#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/26/2012621.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2012621 loop_ _publ_author_name 'Weil, Matthias' 'Kolitsch, Uwe' _publ_section_title ; Hg~3~Se~3~O~10~, a mercury(II) compound with mixed-valence oxoselenium(IV/VI) anions ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i47 _journal_page_last i49 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac 'Hg3 Se3 O10' _chemical_formula_structural 'Hg3 (Se O3)2 Se O4' _chemical_formula_sum 'Hg3 O10 Se3' _chemical_formula_weight 998.65 _chemical_name_systematic ; Trimercury(II) {bis[selenite(IV)] selenate(VI)}] ; _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens none _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELX97 _cell_angle_alpha 90 _cell_angle_beta 108.422(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.3979(9) _cell_length_b 5.3327(6) _cell_length_c 11.1482(12) _cell_measurement_reflns_used 981 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 59.65 _cell_measurement_theta_min 5.34 _cell_volume 473.67(9) _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction SAINT _computing_molecular_graphics 'ATOMS (Dowty, 1998)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measurement_device_type 'Siemens SMART CCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 6813 _diffrn_reflns_theta_full 30.26 _diffrn_reflns_theta_max 30.26 _diffrn_reflns_theta_min 1.93 _exptl_absorpt_coefficient_mu 60.065 _exptl_absorpt_correction_T_max 0.446 _exptl_absorpt_correction_T_min 0.064 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(HABITUS; Herrendorf, 1993-97)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 7.002 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description fragment _exptl_crystal_F_000 844 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.98 _refine_diff_density_min -1.51 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -0.015(11) _refine_ls_extinction_coef 0.0090(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 146 _refine_ls_number_reflns 2684 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.032 _refine_ls_R_factor_gt 0.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.025P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.058 _refine_ls_wR_factor_ref 0.060 _reflns_number_gt 2435 _reflns_number_total 2684 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file br1358.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21' _cod_database_code 2012621 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Hg1 0.00338(3) 0.24647(10) 0.12945(3) 0.01513(9) Uani d . 1 . . Hg Hg2 0.00612(4) 0.25889(11) 0.62586(3) 0.01722(9) Uani d . 1 . . Hg Hg3 0.37438(4) 0.74340(19) 0.20835(3) 0.02385(10) Uani d . 1 . . Hg Se1 0.26005(9) 0.2248(3) 0.96051(7) 0.01227(17) Uani d . 1 . . Se Se2 0.26538(10) 0.2866(2) 0.42224(8) 0.0120(2) Uani d . 1 . . Se Se3 0.64667(9) 0.2506(4) 0.28524(7) 0.01271(15) Uani d . 1 . . Se O1 0.1017(8) 0.1229(12) 0.8322(6) 0.0187(14) Uani d . 1 . . O O2 0.1144(9) 0.4039(12) 0.4812(7) 0.0191(14) Uani d . 1 . . O O3 0.1562(8) 0.0649(12) 0.3169(6) 0.0176(14) Uani d . 1 . . O O4 0.1604(9) 0.4619(11) 0.0134(7) 0.0159(14) Uani d . 1 . . O O5 0.2287(9) 0.0004(13) 0.0601(7) 0.0242(17) Uani d . 1 . . O O6 0.2451(10) 0.5265(14) 0.3179(8) 0.0293(18) Uani d . 1 . . O O7 0.5236(8) 0.0632(12) 0.3330(6) 0.0197(14) Uani d . 1 . . O O8 0.5272(9) 0.4256(13) 0.1660(6) 0.0214(14) Uani d . 1 . . O O9 0.7470(9) 0.4314(13) 0.4004(7) 0.0238(15) Uani d . 1 . . O O10 0.7704(9) 0.0820(12) 0.2280(6) 0.0227(15) Uani d . 1 . . O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Hg1 0.01823(15) 0.01396(19) 0.01333(14) 0.0008(2) 0.00517(11) 0.0000(2) Hg2 0.02466(17) 0.01580(19) 0.01375(14) -0.0026(2) 0.00971(12) -0.00090(18) Hg3 0.02511(18) 0.01728(17) 0.02787(18) 0.0001(3) 0.00653(13) 0.0091(2) Se1 0.0129(3) 0.0120(4) 0.0121(3) -0.0011(4) 0.0044(3) -0.0010(4) Se2 0.0118(4) 0.0130(5) 0.0108(3) -0.0005(3) 0.0032(3) 0.0002(3) Se3 0.0115(3) 0.0140(4) 0.0127(3) -0.0004(6) 0.0039(3) -0.0023(4) O1 0.023(3) 0.020(3) 0.010(3) -0.009(3) 0.003(3) -0.001(2) O2 0.021(4) 0.022(3) 0.019(3) 0.009(3) 0.015(3) 0.007(3) O3 0.019(3) 0.017(3) 0.014(3) -0.004(3) 0.002(3) -0.004(3) O4 0.023(4) 0.011(3) 0.019(4) 0.008(3) 0.014(3) 0.002(2) O5 0.021(4) 0.022(4) 0.024(4) 0.004(3) -0.001(3) 0.007(3) O6 0.030(4) 0.024(3) 0.041(5) 0.004(3) 0.022(4) 0.019(3) O7 0.021(3) 0.021(3) 0.022(4) -0.004(3) 0.012(3) 0.002(3) O8 0.019(4) 0.028(4) 0.016(3) 0.004(3) 0.004(3) 0.007(3) O9 0.026(4) 0.021(3) 0.023(4) -0.007(3) 0.005(3) -0.011(3) O10 0.027(4) 0.022(3) 0.023(4) 0.001(3) 0.014(3) -0.010(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hg1 O1 2_556 2.287(6) y Hg1 O3 . 2.293(7) y Hg1 O4 2_545 2.312(7) y Hg1 O4 . 2.411(7) y Hg1 O5 . 2.612(8) y Hg1 O10 1_455 2.677(7) y Hg1 O5 2 2.738(8) y Hg1 O6 . 2.840(9) y Hg1 Se1 1_554 3.2821(8) ? Hg1 Se2 . 3.3169(9) ? Hg2 O2 . 2.226(6) y Hg2 O2 2_546 2.295(7) y Hg2 O1 . 2.301(6) y Hg2 O3 2_556 2.340(6) y Hg2 O10 2_656 2.686(7) y Hg2 O6 2_546 2.686(8) y Hg2 O9 2_646 2.796(7) y Hg2 O9 1_455 2.906(8) y Hg2 Se2 2_546 3.3252(15) ? Hg2 Se2 2_556 3.5542(15) ? Hg3 O5 1_565 2.197(7) y Hg3 O6 . 2.201(7) y Hg3 O8 . 2.263(7) y Hg3 O7 1_565 2.304(7) y Hg3 O4 . 2.782(7) y Hg3 O3 1_565 3.027(6) y Hg3 Se3 . 3.4103(15) ? Hg3 Se3 1_565 3.4700(14) ? Hg3 Se1 1_564 3.6702(12) ? Se1 O1 . 1.705(6) y Se1 O5 1_556 1.709(7) y Se1 O4 1_556 1.720(6) y Se2 O6 . 1.702(7) y Se2 O3 . 1.714(6) y Se2 O2 . 1.719(6) y Se3 O9 . 1.613(7) y Se3 O7 . 1.643(6) y Se3 O10 . 1.647(6) y Se3 O8 . 1.674(7) y O1 Hg1 2_546 2.287(6) ? O1 Hg1 2_556 3.501(6) ? O1 Hg1 1_556 3.718(6) ? O1 Hg3 2_546 3.931(7) ? O2 Hg2 2_556 2.295(7) ? O2 Hg2 2_546 3.676(7) ? O3 Hg2 2_546 2.340(6) ? O3 Hg3 1_545 3.027(6) ? O3 Hg2 2_556 4.063(7) ? O4 Se1 1_554 1.720(6) ? O4 Hg1 2 2.312(7) ? O5 Se1 1_554 1.709(7) ? O5 Hg3 1_545 2.197(7) ? O5 Hg1 2_545 2.738(8) ? O6 Hg2 2_556 2.686(7) ? O7 Hg3 1_545 2.304(7) ? O7 Hg2 2_646 4.159(7) ? O8 Hg3 1_545 3.935(7) ? O9 Hg2 2_656 2.796(7) ? O9 Hg2 1_655 2.906(8) ? O10 Hg1 1_655 2.677(7) ? O10 Hg2 2_646 2.686(7) ? O10 Hg3 1_545 3.729(7) ? O10 Hg2 2_656 4.156(7) ? 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Hg1 O3 2_556 . 109.8(2) ? O1 Hg1 O4 2_556 2_545 121.6(2) ? O3 Hg1 O4 . 2_545 113.0(2) ? O1 Hg1 O4 2_556 . 89.5(2) ? O3 Hg1 O4 . . 116.6(2) ? O4 Hg1 O4 2_545 . 104.50(16) ? O1 Hg1 O5 2_556 . 148.7(2) ? O3 Hg1 O5 . . 79.0(2) ? O4 Hg1 O5 2_545 . 78.2(3) ? O4 Hg1 O5 . . 60.69(19) ? O1 Hg1 O10 2_556 1_455 80.5(2) ? O3 Hg1 O10 . 1_455 76.0(2) ? O4 Hg1 O10 2_545 1_455 73.4(2) ? O4 Hg1 O10 . 1_455 166.2(2) ? O5 Hg1 O10 . 1_455 130.4(2) ? O1 Hg1 O5 2_556 2 59.2(2) ? O3 Hg1 O5 . 2 165.8(2) ? O4 Hg1 O5 2_545 2 70.7(2) ? O4 Hg1 O5 . 2 74.1(3) ? O5 Hg1 O5 . 2 115.18(14) ? O10 Hg1 O5 1_455 2 92.6(2) ? O1 Hg1 O6 2_556 . 68.2(2) ? O3 Hg1 O6 . . 59.0(2) ? O4 Hg1 O6 2_545 . 170.0(2) ? O4 Hg1 O6 . . 76.2(2) ? O5 Hg1 O6 . . 93.9(2) ? O10 Hg1 O6 1_455 . 108.2(2) ? O5 Hg1 O6 2 . 118.6(2) ? O2 Hg2 O2 . 2_546 97.12(17) ? O2 Hg2 O1 . . 137.8(2) ? O2 Hg2 O1 2_546 . 102.5(2) ? O2 Hg2 O3 . 2_556 111.2(2) ? O2 Hg2 O3 2_546 2_556 121.2(2) ? O1 Hg2 O3 . 2_556 89.8(2) ? O2 Hg2 O10 . 2_656 81.3(2) ? O2 Hg2 O10 2_546 2_656 162.4(2) ? O1 Hg2 O10 . 2_656 68.9(2) ? O3 Hg2 O10 2_556 2_656 75.1(2) ? O2 Hg2 O6 . 2_546 149.4(3) ? O2 Hg2 O6 2_546 2_546 59.4(2) ? O1 Hg2 O6 . 2_546 70.9(2) ? O3 Hg2 O6 2_556 2_546 71.9(2) ? O10 Hg2 O6 2_656 2_546 127.2(2) ? O2 Hg2 O9 . 2_646 69.8(2) ? O2 Hg2 O9 2_546 2_646 69.5(2) ? O1 Hg2 O9 . 2_646 82.6(2) ? O3 Hg2 O9 2_556 2_646 168.3(2) ? O10 Hg2 O9 2_656 2_646 93.7(2) ? O6 Hg2 O9 2_546 2_646 113.5(2) ? O2 Hg2 O9 . 1_455 68.2(2) ? O2 Hg2 O9 2_546 1_455 74.0(2) ? O1 Hg2 O9 . 1_455 153.4(2) ? O3 Hg2 O9 2_556 1_455 70.9(2) ? O10 Hg2 O9 2_656 1_455 120.7(2) ? O6 Hg2 O9 2_546 1_455 85.4(2) ? O9 Hg2 O9 2_646 1_455 118.99(15) ? O5 Hg3 O6 1_565 . 119.3(3) ? O5 Hg3 O8 1_565 . 121.9(3) ? O6 Hg3 O8 . . 97.7(3) ? O5 Hg3 O7 1_565 1_565 93.4(3) ? O6 Hg3 O7 . 1_565 108.9(3) ? O8 Hg3 O7 . 1_565 116.4(2) ? O5 Hg3 O4 1_565 . 71.3(2) ? O6 Hg3 O4 . . 80.8(3) ? O8 Hg3 O4 . . 72.7(2) ? O7 Hg3 O4 1_565 . 164.7(2) ? O5 Hg3 O3 1_565 1_565 71.6(2) ? O6 Hg3 O3 . 1_565 67.0(2) ? O8 Hg3 O3 . 1_565 164.1(2) ? O7 Hg3 O3 1_565 1_565 67.8(2) ? O4 Hg3 O3 . 1_565 107.15(18) ? O5 Hg3 O9 1_565 . 155.5(2) ? O6 Hg3 O9 . . 85.2(2) ? O8 Hg3 O9 . . 48.2(2) ? O7 Hg3 O9 1_565 . 77.2(2) ? O4 Hg3 O9 . . 116.21(17) ? O3 Hg3 O9 1_565 . 123.18(16) ? O1 Se1 O5 . 1_556 94.7(3) y O1 Se1 O4 . 1_556 100.8(3) y O5 Se1 O4 1_556 1_556 95.8(3) y O6 Se2 O3 . . 97.7(4) y O6 Se2 O2 . . 93.5(3) y O3 Se2 O2 . . 102.3(3) y O9 Se3 O7 . . 109.2(3) y O9 Se3 O10 . . 113.6(4) y O7 Se3 O10 . . 109.4(4) y O9 Se3 O8 . . 109.3(4) y O7 Se3 O8 . . 108.4(3) y O10 Se3 O8 . . 106.9(3) y _cod_database_fobs_code 2012621 _journal_paper_doi 10.1107/S0108270102001920