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_2021334
_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 2.5 K'
_chemical_name_systematic
;
3-[2-(Pyridin-4-yl)ethyl]pentane-2,4-dione
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_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
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 91.59(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.768(7)
_cell_length_b                   11.115(2)
_cell_length_c                   22.30(4)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    2.5(5)
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      6.0
_cell_volume                     2172(4)
_computing_data_reduction
;
PRON2013 (Meven, 2013)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_diffrn_ambient_temperature      2.5(5)
_diffrn_measured_fraction_theta_full 0.754
_diffrn_measured_fraction_theta_max 0.474
_diffrn_measurement_device_type  'closed Eulerian cradle HEiDi'
_diffrn_measurement_method       'rocking scan'
_diffrn_radiation_source         'FRM II'
_diffrn_radiation_type           neutrons
_diffrn_radiation_wavelength     0.795
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            4136
_diffrn_reflns_theta_full        28.411
_diffrn_reflns_theta_max         39.362
_diffrn_reflns_theta_min         2.039
_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    1.255
_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         0.102
_refine_diff_density_min         -0.097
_refine_ls_extinction_coef       0.41(3)
_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   1.145
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         2207
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0650P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                1978
_reflns_number_total             2207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lg3228sup1.cif
_cod_data_source_block           1a
_cod_original_cell_volume        2172(5)
_cod_database_code               2021334
_shelx_estimated_absorpt_t_min   0.996
_shelx_estimated_absorpt_t_max   0.997
_shelx_hkl_checksum              72217
_shelx_res_checksum              84211
_cod_database_fobs_code 2021334