#------------------------------------------------------------------------------
#$Date: 2023-03-26 10:09:57 +0200 (Sun 26 de Mar de 2023) $
#$Revision: 282068 $
#$URL: svn://www.crystallography.net/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
'Göbbels, 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_paper_doi               10.1107/S1600536804002648
_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)'
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_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)'
_database_code_amcsd             0010425
_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       'ω 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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0208P)²] where P = (Fo²+2Fc²)/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>2σ(I)
_cod_database_code               2203316
_amcsd_formula_title             Hg(ClO3)(OH)
loop_
_space_group_symop_operation_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
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0010425
