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_4514130
_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         '2(C4 H3 O4), H12 Mg O6'
_chemical_formula_sum            'C8 H18 Mg O14'
_chemical_formula_weight         362.53
_chemical_name_common            'Magnesium hydrogen maleate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 103.66(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.192(2)
_cell_length_b                   11.756(2)
_cell_length_c                   6.6189(13)
_cell_measurement_radiation      Synchrotron
_cell_measurement_reflns_used    239172
_cell_measurement_temperature    25
_cell_measurement_theta_max      36.06
_cell_measurement_theta_min      0.86
_cell_measurement_wavelength     0.3531
_cell_volume                     770.6(3)
_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 0.818
_diffrn_measured_fraction_theta_max 0.818
_diffrn_measurement_details      '24 images, exposure time  75 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  0.0645
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            30530
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)'
_diffrn_reflns_resolution_max    1.67
_diffrn_reflns_theta_full        70.90
_diffrn_reflns_theta_max         71.00
_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    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             146
_exptl_crystal_size_max          1.5
_exptl_crystal_size_mid          1.5
_exptl_crystal_size_min          0.9
_refine_diff_density_max         0.83
_refine_diff_density_min         -0.98
_refine_ls_extinction_coef       4.4(4)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9999
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.0003579
_refine_ls_shift/su_mean         0.0000336
_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: 
 172. 56.7 24.3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0565
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0434
_reflns_number_gt                2467
_reflns_number_total             3046
_reflns_threshold_expression     >2sigma(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0343
_oxford_refine_ls_scale          1.751(11)
_oxford_reflns_number_all        2937
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            MgHmal_F2.cif
_cod_data_source_block           MgHmal_neutron_F2
_cod_depositor_comments
'Adding full bibliography for 4514126--4514133.cif.'
_cod_original_cell_volume        770.63(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C8 H18 Mg1 O14'
_cod_database_code               4514130