#------------------------------------------------------------------------------
#$Date: 2017-08-05 20:34:20 +0200 (Sat 05 de Aug de 2017) $
#$Revision: 199568 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/41/4514128.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4514128
loop_
_publ_author_name
'Malaspina, Lorraine A.'
'Edwards, Alison J.'
'Woińska, Magdalena'
'Jayatilaka, Dylan'
'Turner, Michael J.'
'Price, Jason R.'
'Herbst-Irmer, Regine'
'Sugimoto, Kunihisa'
'Nishibori, Eiji'
'Grabowsky, Simon'
_publ_contact_author
;
  Dr. Simon Grabowsky
  University of Bremen
  Institute for Inorganic Chemistry and Crystallography
  Leobener Str. NW2
  28359 Bremen
  Germany
;
_publ_section_title
;
 Predicting the Position of the Hydrogen Atom in the Short Intramolecular
 Hydrogen Bond of the Hydrogen Maleate Anion from Geometric Correlations
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3812
_journal_paper_doi               10.1021/acs.cgd.7b00390
_journal_volume                  17
_journal_year                    2017
_chemical_formula_moiety         'C4 H3 O4, K'
_chemical_formula_sum            'C4 H3 K O4'
_chemical_formula_weight         154.16
_chemical_name_common            'Potassium hydrogen maleate'
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      57
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     isomor
_audit_creation_date             2017-03-09
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.5071(9)
_cell_length_b                   7.7017(15)
_cell_length_c                   15.921(3)
_cell_measurement_radiation      Synchrotron
_cell_measurement_reflns_used    133388
_cell_measurement_temperature    25
_cell_measurement_theta_max      36.075
_cell_measurement_theta_min      0.635
_cell_measurement_wavelength     0.3531
_cell_volume                     552.66(19)
_computing_cell_refinement       'LaueG (Piltz, 2011)'
_computing_data_collection       'MAATEL/ANSTO control program'
_computing_data_reduction
'argonne_boxes (Wilkinson et al., 1988) & LaueG (Piltz, 2011)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      12
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_details      '20 images, exposure time 100 to 100 minutes'
_diffrn_measurement_device       'Laue image-plate diffractometer'
_diffrn_measurement_device_type  KOALA
_diffrn_measurement_method       Laue
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.85
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16079
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)'
_diffrn_reflns_resolution_max    1.54
_diffrn_reflns_theta_full        70.68
_diffrn_reflns_theta_max         70.78
_diffrn_source                   'nuclear reactor'
_diffrn_source_details           'thermal neutrons, supermirror guides'
_diffrn_source_type
'OPAL reactor, ANSTO, Lucas Heights, Australia'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             176
_exptl_crystal_size_max          1.6
_exptl_crystal_size_mid          1.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         695
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.0005269
_refine_ls_shift/su_mean         0.0000804
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 80.9 36.7 55.0 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0644
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                774
_reflns_number_total             946
_reflns_threshold_expression     >2sigma(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0237
_oxford_refine_ls_scale          1.299(6)
_oxford_reflns_number_all        811
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_iucr_refine_instructions_details
;
#
# Punched on 09/03/17 at 15:38: 6
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT K    (    1 ,X'S,U'S)  UNTIL LAST 
END                                                                             
#
# Punched on 09/03/17 at 15:38: 6
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_cod_data_source_file            KHmal_F2.cif
_cod_data_source_block           KHmal_neutron_F2
_cod_depositor_comments
'Adding full bibliography for 4514126--4514133.cif.'
_cod_original_cell_volume        552.66(11)
_cod_original_sg_symbol_H-M      'P b c m '
_cod_database_code               4514128
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,z
x,-y+1/2,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
-x,-y,z+1/2
x,y,-z+1/2
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
K1 K 0.7613(3) 0.2500 0.5000 0.0048 1.0000 Uani S T
O3 O 1.26408(14) 0.08071(8) 0.42891(4) 0.0067 1.0000 Uani . .
C1 C 1.21688(13) 0.10372(6) 0.35308(3) 0.0047 1.0000 Uani . .
O1 O 1.01024(15) 0.20572(8) 0.32615(3) 0.0066 1.0000 Uani . .
C2 C 1.41275(15) 0.01030(6) 0.29216(3) 0.0057 1.0000 Uani . .
H2 H 1.5813(3) -0.06738(17) 0.32338(8) 0.0207 1.0000 Uani . .
H1 H 1.0012(4) 0.2081(3) 0.2500 0.0186 1.0000 Uani S T
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
K1 0.0051(9) 0.0046(6) 0.0048(6) 0.0007(3) 0.0000 0.0000
O3 0.0080(3) 0.0077(2) 0.0044(2) 0.00015(16) -0.00005(17) 0.00057(17)
C1 0.0051(2) 0.00502(19) 0.00396(19) -0.00015(13) -0.00017(15) 0.00009(15)
O1 0.0073(3) 0.0076(2) 0.0050(2) -0.00011(18) -0.00044(17) 0.00251(18)
C2 0.0064(3) 0.00627(19) 0.00451(17) 0.00011(12) -0.00023(18) 0.00146(15)
H2 0.0208(7) 0.0243(6) 0.0170(4) 0.0021(4) -0.0032(5) 0.0110(5)
H1 0.0170(10) 0.0176(7) 0.0211(7) 0.0000 0.0000 0.0050(6)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 6.6484
'Neutron Data Booklet 2nd Ed July 2003, ILL Table 1.1'
H 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 -3.7409
'Neutron Data Booklet 2nd Ed July 2003, ILL Table 1.1'
O 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 5.8050
'Neutron Data Booklet 2nd Ed July 2003, ILL Table 1.1'
K 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 3.6700
'Neutron Data Booklet 2nd Ed July 2003, ILL Table 1.1'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 . C1 O1 . 122.30(5) yes
O3 . C1 C2 . 117.50(5) yes
O1 . C1 C2 . 120.19(5) yes
C1 . O1 H1 . 111.40(10) no
C1 . C2 C2 8_555 130.42(3) yes
C1 . C2 H2 . 112.37(8) no
C2 8_555 C2 H2 . 117.21(7) no
O1 . H1 O1 8_555 175.80(18) no
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
O3 C1 . 1.2387(8) yes
C1 O1 . 1.2916(8) yes
C1 C2 . 1.4959(8) yes
O1 H1 . 1.2131(6) no
C2 C2 8_555 1.3424(11) yes
C2 H2 . 1.0871(14) no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C2 H2 O1 3_845 153.30(10) 1.0872(15) 2.5387(16) 3.5439(11) yes
