#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/33/2203316.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_2203316 loop_ _publ_author_name 'G\"obbels, Dirk' 'Wickleder, Mathias S.' _publ_section_title ; Redetermination of mercury(II) hydroxide chlorate(V) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first i40 _journal_page_last i41 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'Hg (OH) Cl O3' _chemical_formula_moiety 'Cl H Hg O4' _chemical_formula_sum 'Cl H Hg O4' _chemical_formula_weight 301.05 _chemical_name_common 'mercuric hydroxide chlorate' _chemical_name_systematic 'mercury(II) hydroxide chlorate(V)' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2c 2b' _symmetry_space_group_name_H-M 'P b c m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 4.6375(6) _cell_length_b 11.4064(19) _cell_length_c 7.1965(11) _cell_measurement_reflns_used 2000 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 29.6 _cell_measurement_theta_min 1.8 _cell_volume 380.67(10) _computing_cell_refinement X-AREA _computing_data_collection 'X-AREA (Stoe & Cie, 2001)' _computing_data_reduction 'X-RED (Stoe & Cie, 2001)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 170(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type IPDS-II _diffrn_measurement_method '\w oscillation scans' _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 0.0999 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 9295 _diffrn_reflns_theta_full 29.98 _diffrn_reflns_theta_max 29.98 _diffrn_reflns_theta_min 3.57 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 40.989 _exptl_absorpt_correction_T_max 0.1164 _exptl_absorpt_correction_T_min 0.0115 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-SHAPE; Stoe & Cie, 1999)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 5.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod-shaped _exptl_crystal_F_000 520 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _refine_diff_density_max 2.029 _refine_diff_density_min -1.207 _refine_ls_extinction_coef 0.0265(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 37 _refine_ls_number_reflns 592 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.967 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0195 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0208P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0427 _reflns_number_gt 457 _reflns_number_total 592 _reflns_threshold_expression I>2\s(I) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-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_type_symbol Hg1 0.56532(4) 0.2500 0.0000 0.01323(12) Uani d S 1 Hg O1 0.5736(8) 0.1638(4) 0.2500 0.0135(10) Uani d S 1 O Cl1 0.9968(4) 0.43891(14) 0.2500 0.0136(3) Uani d S 1 Cl O11 0.6740(10) 0.4461(5) 0.2500 0.0204(9) Uani d S 1 O O12 0.0692(6) 0.3682(4) 0.0831(5) 0.0227(8) Uani d . 1 O H1 0.464(17) 0.097(7) 0.2500 0.010(19) Uiso d S 1 H 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 0.01271(15) 0.01731(16) 0.00967(16) 0.000 0.000 -0.00004(9) O1 0.018(2) 0.014(2) 0.0084(18) -0.0037(16) 0.000 0.000 Cl1 0.0110(5) 0.0151(6) 0.0146(5) -0.0024(7) 0.000 0.000 O11 0.0143(19) 0.020(2) 0.027(2) 0.005(2) 0.000 0.000 O12 0.0163(17) 0.0294(19) 0.0224(18) 0.0029(13) 0.0011(11) -0.0096(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 '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 O1 7_565 . 177.9(2) y Hg1 O1 Hg1 6_556 . 122.6(2) y Hg1 O1 H1 6_556 . 112.8(15) y Hg1 O1 H1 . . 112.8(15) n O12 Cl1 O12 1_655 6_656 107.9(3) y O12 Cl1 O11 1_655 . 104.81(18) y O12 Cl1 O11 6_656 . 104.81(18) y 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 7_565 2.051(2) y Hg1 O1 . 2.051(2) n O1 Hg1 6_556 2.051(2) n O1 H1 . 0.92(8) y Cl1 O12 1_655 1.486(4) y Cl1 O12 6_656 1.486(4) y Cl1 O11 . 1.499(5) y O12 Cl1 1_455 1.486(4) n _cod_database_code 2203316