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_4514129
_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_absolute_configuration syn
_chemical_formula_moiety         '4(C4 O4 H3), Ba2, 8(O1 H2)'
_chemical_formula_sum            'C16 H28 Ba2 O24'
_chemical_formula_weight         879.06
_chemical_name_common            'Barium hydrogen maleate'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     isomor
_audit_creation_date             2017-03-14
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                90
_cell_angle_beta                 92.90(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.4162(13)
_cell_length_b                   19.016(4)
_cell_length_c                   11.412(2)
_cell_measurement_radiation      Synchrotron
_cell_measurement_reflns_used    58696
_cell_measurement_temperature    25
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      0.53
_cell_measurement_wavelength     0.353226
_cell_volume                     1390.6(5)
_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 0.851
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_details      '21 images, exposure time 125 to 250 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  0.1089
_diffrn_reflns_av_unetI/netI     0.1011
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17394
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)'
_diffrn_reflns_resolution_max    1.11
_diffrn_reflns_theta_full        68.83
_diffrn_reflns_theta_max         68.92
_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    2.099
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         1516
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.0002685
_refine_ls_shift/su_mean         0.0000427
_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: 
 1.07 -0.942 0.208 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0270
_refine_ls_wR_factor_gt          0.0229
_refine_ls_wR_factor_ref         0.0223
_reflns_number_gt                1575
_reflns_number_total             1702
_reflns_threshold_expression     >2sigma(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0335
_oxford_refine_ls_scale          0.4320(8)
_oxford_reflns_number_all        1693
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            BaHmal_F_iso_butH1.cif
_cod_data_source_block           BaHmal_neutron_F_iso_butH1s
_cod_depositor_comments
'Adding full bibliography for 4514126--4514133.cif.'
_cod_original_cell_volume        1390.6(3)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4514129