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#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/36/2103682.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_2103682
loop_
_publ_author_name
'Olovsson, I.'
'Ptasiewicz-Bak, H.'
'Gustafsson, T.'
'Majerz, I.'
_publ_section_title
;
 Asymmetric hydrogen bonds in centrosymmetric environment: neutron
 study of very short hydrogen bonds in potassium hydrogen
 dichloromaleate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              311
_journal_page_last               316
_journal_paper_doi               10.1107/S0108768101003779
_journal_volume                  57
_journal_year                    2001
_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                80.99(2)
_cell_angle_beta                 85.13(2)
_cell_angle_gamma                88.95(2)
_cell_formula_units_Z            1
_cell_length_a                   5.022(2)
_cell_length_b                   7.827(4)
_cell_length_c                   8.838(4)
_cell_measurement_temperature    30
_cell_volume                     341.9(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  .046
_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            2104
_diffrn_reflns_theta_max         52
_diffrn_standards_decay_%        stable
_diffrn_standards_interval_count 33
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .088
_exptl_absorpt_correction_T_max  .9254
_exptl_absorpt_correction_T_min  .7198
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'gaussian (Coppens, Leiserowitz & Rabinovich, 1965)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.180
_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         .05
_refine_diff_density_min         -.05
_refine_ls_extinction_coef       7245.1
_refine_ls_extinction_method
'Lorentzian type I isotropic (Becker & Coppens, 1974, 1975)'
_refine_ls_goodness_of_fit_ref   1.7718
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1485
_refine_ls_R_factor_gt           .0580
_refine_ls_shift/su_max          .05
_refine_ls_structure_factor_coef Fsqd
_refine_ls_wR_factor_ref         .0805
_reflns_number_gt                1871
_reflns_number_total             2104
_reflns_threshold_expression     Fₒ²>3σ(Fₒ²)
_cod_data_source_file            os0070.cif
_cod_data_source_block           neutron
_cod_original_cell_volume        341.8(2)
_cod_database_code               2103682
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
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
K .0052(7) .0049(7) .0085(6) -.0003(6) .0000(5) -.0011(5)
Cl1 .0055(3) .0052(3) .0084(3) -.0002(2) .0005(2) -.0006(2)
Cl2 .0078(3) .0033(3) .0103(3) .0002(2) .0013(2) -.0018(2)
O1 .0084(5) .0058(4) .0077(4) .0001(4) -.0032(3) -.0019(3)
O2 .0086(5) .0053(4) .0079(4) .0010(4) -.0027(3) -.0009(3)
O3 .0074(5) .0045(5) .0106(4) -.0001(4) .0019(3) -.0018(3)
O4 .0067(5) .0039(5) .0105(4) -.0011(4) .0023(3) -.0008(3)
C1 .0049(4) .0034(4) .0074(4) .0001(3) -.0009(3) -.0010(3)
C2 .0061(4) .0034(4) .0073(4) -.0001(3) -.0006(3) -.0008(3)
C3 .0055(4) .0035(4) .0084(4) -.0004(3) .0000(3) -.0011(3)
C4 .0051(4) .0039(4) .0075(4) .0001(3) .0003(3) -.0011(3)
H2 .009(2) .0135(14) .021(2) -.0046(15) .0061(14) .0041(14)
H4 .023(2) .0137(13) .015(2) -.0024(14) -.0084(15) -.0080(14)
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 .3016(3) -.1559(2) .6242(2) .0062(7) Uequi
Cl1 .47540(10) -.24420(10) .06030(10) .0065(3) Uequi
Cl2 .13810(10) -.57110(10) .20320(10) .0072(3) Uequi
O1 .2346(2) -.00150(10) .33470(10) .0071(4) Uequi
O2 .0246(2) .05080(10) .12150(10) .0072(4) Uequi
O3 -.2508(2) -.22000(10) .40180(10) .0076(5) Uequi
O4 -.2962(2) -.50660(10) .41530(10) .0072(5) Uequi
C1 .1507(2) -.04910(10) .22160(10) .0052(4) Uequi
C2 .2044(2) -.23160(10) .19020(10) .0056(4) Uequi
C3 .0592(2) -.37100(10) .25260(10) .0059(4) Uequi
C4 -.1812(2) -.36050(10) .36560(10) .0055(4) Uequi
H2 .023(2) .0065(17) -.0104(11) .0147(18) Uequi
H4 -.491(3) -.4957(18) .5116(15) .0160(18) Uequi
K1 -.3016(3) .1559(2) -.6242(2) .0062(7) Uequi
Cl11 -.47540(10) .24420(10) -.06030(10) .0065(3) Uequi
Cl21 -.13810(10) .57110(10) -.20320(10) .0072(3) Uequi
O11 -.2346(2) .00150(10) -.33470(10) .0071(4) Uequi
O21 -.0246(2) -.05080(10) -.12150(10) .0072(4) Uequi
O31 .2508(2) .22000(10) -.40180(10) .0076(5) Uequi
O41 .2962(2) .50660(10) -.41530(10) .0072(5) Uequi
C11 -.1507(2) .04910(10) -.22160(10) .0052(4) Uequi
C21 -.2044(2) .23160(10) -.19020(10) .0056(4) Uequi
C31 -.0592(2) .37100(10) -.25260(10) .0059(4) Uequi
C41 .1812(2) .36050(10) -.36560(10) .0055(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
C2 C1 O1 . 120.10(10) yes
C2 C1 O2 . 116.30(10) yes
O1 C1 O2 . 123.50(10) yes
C1 C2 C3 . 125.40(10) no
C1 C2 Cl1 . 112.50(10) no
Cl1 C2 C3 . 122.10(10) no
C2 C3 Cl2 . 120.60(10) no
Cl2 C3 C4 . 117.00(10) no
C2 C3 C4 . 122.30(10) no
C3 C4 O3 . 119.70(10) yes
C3 C4 O4 . 114.20(10) yes
O3 C4 O4 . 126.00(10) yes
C1 O2 H2 . 116.9(6) yes
H2 O21 C11 . 116.7(6) no
C4 O4 H4 . 113.2(6) yes
H4 O41 C41 1_664 117.6(6) no
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 . . 2.699(2) yes
K O41 . 1_546 2.719(2) no
C2 Cl1 . . 1.7160(10) yes
C3 Cl2 . . 1.7210(10) yes
C1 O1 . . 1.2290(10) yes
C1 O2 . . 1.2870(10) yes
C4 O3 . . 1.2290(10) yes
C4 O4 . . 1.2870(10) yes
C1 C2 . . 1.5130(10) yes
C2 C3 . . 1.3410(10) yes
C3 C4 . . 1.5100(10) yes
O2 H2 . . 1.268(12) no
O21 H2 . . 1.185(12) no
O4 H4 . . 1.253(15) no
O41 H4 1_446 . 1.201(15) no
