Predicting the Position of the Hydrogen Atom in the Short Intramolecular Hydrogen Bond of the Hydrogen Maleate Anion from Geometric Correlations
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; Crystal Growth & Design 17 (2017) 3812–; doi:10.1021/acs.cgd.7b00390

data_4514128
_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 &amp; 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/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ 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)
_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