#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/33/2103332.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_2103332
loop_
_publ_author_name
'Olovsson, I.'
'Ptasiewicz-Bak, H.'
'Gustafsson, T.'
'Majerz, I.'
_publ_section_title
;
 Asymmetric hydrogen bonds in centrosymmetric environment. II. Neutron
 study of very short hydrogen bonds in potassium hydrogen
 dichloromaleate at 90K and 170K
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              627
_journal_page_last               631
_journal_paper_doi               10.1107/S0108768102004858
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'K2 Cl4 O8 C8 H2'
_chemical_formula_sum            'C8 H2 Cl4 K2 O8'
_chemical_formula_weight         446.1
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_type_scat_source           Sears(1992)
_cell_angle_alpha                81.46(5)
_cell_angle_beta                 85.05(5)
_cell_angle_gamma                89.35(5)
_cell_formula_units_Z            1
_cell_length_a                   5.048(3)
_cell_length_b                   7.840(4)
_cell_length_c                   8.839(4)
_cell_measurement_temperature    170
_cell_volume                     344.6(3)
_computing_cell_refinement
'STOE 4-circle X-ray Diffractometer Control Program'
_computing_data_collection       'Aracor Diffractometer Control Program'
_computing_data_reduction        'ARACOR-DATRED vers. 950320'
_computing_structure_refinement  'UPALS Lundgren (1982)'
_diffrn_measurement_device       'Huber-Aracor 400 mm diameter four-circle'
_diffrn_measurement_method       θ-2θ
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.207
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1614
_diffrn_reflns_theta_max         52
_diffrn_standards_decay_%        stable
_diffrn_standards_interval_count 33
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9173
_exptl_absorpt_correction_T_min  0.7004
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'gaussian (Coppens, Leiserowitz & Rabinovich, 1965)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.150
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'plate with 6 faces'
_exptl_crystal_size_max          4.2
_exptl_crystal_size_mid          3.5
_exptl_crystal_size_min          1.0
_refine_diff_density_max         0.04
_refine_diff_density_min         -0.04
_refine_ls_extinction_coef       6580.1
_refine_ls_extinction_method
'Lorentzian type I isotropic (Becker & Coppens, 1974, 1975)'
_refine_ls_goodness_of_fit_ref   1.0116
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1236
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.05
_refine_ls_structure_factor_coef Fsqd
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                1236
_reflns_number_total             1370
_reflns_threshold_expression     Fₒ²>3σ(Fₒ²)
_cod_data_source_file            os0089.cif
_cod_data_source_block           1
_cod_database_code               2103332
loop_
_symmetry_equiv_pos_as_xyz
x,y,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_thermal_displace_type
K .3011(3) -.1556(2) .6239(2) .0159(8) Uequi
Cl1 .47000(10) -.24610(10) .05850(10) .0152(3) Uequi
Cl2 .13240(10) -.57110(10) .20160(10) .0188(4) Uequi
O1 .2357(2) -.00330(10) .33370(10) .0173(5) Uequi
O2 .0261(2) .04900(10) .12260(10) .0148(5) Uequi
O3 -.2501(2) -.22090(10) .40200(10) .0159(5) Uequi
O4 -.2980(2) -.50610(10) .41440(10) .0157(5) Uequi
C1 .1506(2) -.05070(10) .22130(10) .0103(4) Uequi
C2 .2011(2) -.23300(10) .18860(10) .0096(4) Uequi
C3 .0552(2) -.37170(10) .25140(10) .0105(4) Uequi
C4 -.1824(2) -.36100(10) .36520(10) .0106(4) Uequi
H2 .0250(19) .0074(15) -.0042(12) .022(2) Uequi
H4 -.494(2) -.5036(14) .5163(8) .0201(19) Uequi
K1 -.3011(3) .1556(2) -.6239(2) .0159(8) Uequi
Cl11 -.47000(10) .24610(10) -.05850(10) .0152(3) Uequi
Cl21 -.13240(10) .57110(10) -.20160(10) .0188(4) Uequi
O11 -.2357(2) .00330(10) -.33370(10) .0173(5) Uequi
O21 -.0261(2) -.04900(10) -.12260(10) .0148(5) Uequi
O31 .2501(2) .22090(10) -.40200(10) .0159(5) Uequi
O41 .2980(2) .50610(10) -.41440(10) .0157(5) Uequi
C11 -.1506(2) .05070(10) -.22130(10) .0103(4) Uequi
C21 -.2011(2) .23300(10) -.18860(10) .0096(4) Uequi
C31 -.0552(2) .37170(10) -.25140(10) .0105(4) Uequi
C41 .1824(2) .36100(10) -.36520(10) .0106(4) Uequi
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
_geom_angle_publ_flag
O1 C1 O2 . 123.40(10) yes
O1 C1 C2 . 120.10(10) yes
O2 C1 C2 . 116.40(10) yes
C1 C2 C3 . 125.30(10) yes
C1 C2 Cl1 . 112.50(10) yes
Cl1 C2 C3 . 122.30(10) yes
C2 C3 Cl2 . 120.40(10) yes
Cl2 C3 C4 . 117.10(10) yes
C2 C3 C4 . 122.50(10) yes
C3 C4 O3 . 119.70(10) yes
C3 C4 O4 . 114.30(10) yes
O3 C4 O4 . 125.90(10) yes
H2 O2 C1 . 116.8(5) yes
H2 O21 C11 . 117.7(5) yes
H4 O4 C4 . 116.2(5) yes
H4 O41 C41 1_664 114.9(6) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
K O1 . . 2.710(2) yes
K O41 . 1_546 2.723(2) yes
Cl1 C2 . . 1.7140(10) yes
Cl2 C3 . . 1.7180(10) yes
O1 C1 . . 1.2240(10) yes
O2 C1 . . 1.2830(10) yes
O3 C4 . . 1.2280(10) yes
O4 C4 . . 1.2830(10) yes
C1 C2 . . 1.5150(10) yes
C2 C3 . . 1.3420(10) yes
C3 C4 . . 1.5080(10) yes
O2 H2 . . 1.214(11) yes
O21 H2 . . 1.243(11) yes
O4 H4 . . 1.282(10) yes
O41 H4 1_446 . 1.175(11) yes
