Hirshfeld atom refinement for modelling strong hydrogen bonds
Woińska, Magdalena; Jayatilaka, Dylan; Spackman, Mark A.; Edwards, Alison J.; Dominiak, Paulina M.; Woźniak, Krzysztof; Nishibori, Eiji; Sugimoto, Kunihisa; Grabowsky, Simon; Acta Crystallographica Section A 70 (2014) 483–498; doi:10.1107/S2053273314012443

data_2310144
_publ_section_title
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 Hirshfeld atom refinement for modelling strong hydrogen bonds
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_journal_coeditor_code           KX5029
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section A'
_journal_page_first              483
_journal_page_last               498
_journal_paper_doi               10.1107/S2053273314012443
_journal_volume                  70
_journal_year                    2014
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C9 H12 N O2, C4 H3 O4'
_chemical_formula_sum            'C13 H15 N O6'
_chemical_formula_weight         281.27
_chemical_name_common            'L-phenylalaninium 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
_cell_angle_alpha                90
_cell_angle_beta                 101.36(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.905(2)
_cell_length_b                   5.2338(10)
_cell_length_c                   11.439(2)
_cell_measurement_reflns_used    124185
_cell_measurement_temperature    25
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      0.9
_cell_volume                     640.1(2)
_computing_data_collection       'MAATEL/ANSTO control program'
_computing_data_reduction
'argonne_boxes (Wilkinson et al., 1988) & LaueG (Piltz, 2011)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_diffrn_ambient_temperature      12
_diffrn_measured_fraction_theta_full 0.804
_diffrn_measured_fraction_theta_max 0.804
_diffrn_measurement_details      '30 images, exposure time  67 to  83 minutes'
_diffrn_measurement_device       'Laue image-plate diffractometer'
_diffrn_measurement_device_type  KOALA
_diffrn_measurement_method       Laue
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.85
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31922
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)'
_diffrn_reflns_resolution_max    1.67
_diffrn_reflns_theta_full        70.85
_diffrn_reflns_theta_max         70.95
_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            colorless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             152
_exptl_crystal_size_max          1.8
_exptl_crystal_size_mid          1.6
_exptl_crystal_size_min          0.7
_refine_diff_density_max         0.96
_refine_diff_density_min         -1.00
_refine_ls_extinction_coef       5.6(10)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9996
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         2231
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.0002806
_refine_ls_shift/su_mean         0.0000283
_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: 
 4.39 -0.947 1.73 1.80 
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0290
_reflns_number_gt                2231
_reflns_number_total             2487
_reflns_threshold_expression     >3sigma(F)
_oxford_refine_ls_scale          1.367(3)
_cod_data_source_file            kx5029sup1.cif
_cod_data_source_block           neutron
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C13 H15 N1 O6'
_cod_database_code               2310144
_cod_database_fobs_code          2310144
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT FIRST    (X'S,U'S)  UNTIL LAST 
CONT EXTPARAM 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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