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_4514126
_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, Na O3 H6'
_chemical_formula_sum            'C4 H9 Na O7'
_chemical_formula_weight         192.10
_chemical_name_common            'Sodium hydrogen maleate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     isomor
_audit_creation_date             2016-07-07
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                103.95(3)
_cell_angle_beta                 91.49(3)
_cell_angle_gamma                99.82(3)
_cell_formula_units_Z            2
_cell_length_a                   5.9390(12)
_cell_length_b                   6.2687(13)
_cell_length_c                   11.247(2)
_cell_measurement_radiation      Synchrotron
_cell_measurement_reflns_used    23021
_cell_measurement_temperature    25
_cell_measurement_theta_max      36.165
_cell_measurement_theta_min      0.93
_cell_measurement_wavelength     0.3542
_cell_volume                     399.43(15)
_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 0.743
_diffrn_measured_fraction_theta_max 0.743
_diffrn_measurement_details      '35 images, exposure time  67 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  0.0487
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26890
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)'
_diffrn_reflns_resolution_max    1.82
_diffrn_reflns_theta_full        70.96
_diffrn_reflns_theta_max         71.06
_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    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             76
_exptl_crystal_size_max          1.2
_exptl_crystal_size_mid          0.9
_exptl_crystal_size_min          0.8
_refine_diff_density_max         0.82
_refine_diff_density_min         -0.87
_refine_ls_extinction_coef       19.9(7)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9998
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2981
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.0006363
_refine_ls_shift/su_mean         0.0000494
_refine_ls_structure_factor_coef F
_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: 
 1.65 -1.05 0.856 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0536
_refine_ls_wR_factor_gt          0.0304
_refine_ls_wR_factor_ref         0.0287
_reflns_number_gt                3144
_reflns_number_total             3713
_reflns_threshold_expression     >2sigma(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0309
_oxford_refine_ls_scale          1.058(2)
_oxford_reflns_number_all        3710
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            NaHmal_F.cif
_cod_data_source_block           NaHmal_neutron
_cod_depositor_comments
'Adding full bibliography for 4514126--4514133.cif.'
_cod_database_code               4514126