Proton disorder in a short intramolecular hydrogen bond investigated by single-crystal neutron diffraction at 2.5 and 170K
Truong, Khai-Nghi; Meven, Martin; Englert, Ulli; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618015164

data_2021335
_publ_section_title
;
 Proton disorder in a short intramolecular hydrogen bond investigated by
 single-crystal neutron diffraction at 2.5 and 170K
;
_journal_coeditor_code           LG3228
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618015164
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C12 H15 N O2'
_chemical_formula_moiety         'C12 H15 N O2'
_chemical_formula_sum            'C12 H15 N O2'
_chemical_formula_weight         205.26
_chemical_name_common            '1, neutron data at 170 K, X-ray constrained'
_chemical_name_systematic
;
3-[2-(Pyridin-4-yl)ethyl]pentane-2,4-dione
;
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
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_computing_data_reduction
;
PRON2013 (Meven, 2013)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.168
_diffrn_measured_fraction_theta_max 0.116
_diffrn_measurement_device_type  'closed Eulerian cradle HEiDi'
_diffrn_measurement_method       'rocking scan'
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_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
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_diffrn_reflns_theta_full        28.411
_diffrn_reflns_theta_max         39.264
_diffrn_reflns_theta_min         3.284
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.001
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       prism
_exptl_crystal_F_000             35
_exptl_crystal_size_max          4.2
_exptl_crystal_size_mid          3.3
_exptl_crystal_size_min          3.2
_refine_diff_density_max         0.079
_refine_diff_density_min         -0.082
_refine_ls_extinction_coef       0.65(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2017 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         546
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0010P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1472
_reflns_number_gt                508
_reflns_number_total             546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lg3228sup1.cif
_cod_data_source_block           1b
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_shelx_estimated_absorpt_t_min   0.996
_shelx_estimated_absorpt_t_max   0.997
_shelx_hkl_checksum              16536
_shelx_res_checksum              98502
_cod_database_fobs_code 2021335