Phase transition and proton ordering at 50K in 3-(pyridin-4-yl)pentane-2,4-dione
Truong, Khai-Nghi; Merkens, Carina; Meven, Martin; Faßbänder, Björn; Dronskowski, Richard; Englert, Ulli; Acta Crystallographica Section B 73 (2017) 1172–1178; doi:10.1107/S2052520617015591

data_2108188
_publ_section_title
;
 Phase transition and proton ordering at 50K in
 3-(pyridin-4-yl)pentane-2,4-dione
;
_journal_coeditor_code           HW5050SUP1
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              1172
_journal_page_last               1178
_journal_paper_doi               10.1107/S2052520617015591
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C10 H11 N O2'
_chemical_formula_sum            'C10 H11 N O2'
_chemical_formula_weight         177.20
_chemical_name_common            'compound 1beta'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                101.482(3)
_cell_angle_beta                 96.2307(13)
_cell_angle_gamma                96.0785(13)
_cell_formula_units_Z            2
_cell_length_a                   6.2755(2)
_cell_length_b                   8.6368(2)
_cell_length_c                   8.6570(2)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    2.5(5)
_cell_volume                     453.17(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      2.5(5)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.638
_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     0.793
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.638
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2315
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.638
_diffrn_reflns_theta_full        28.411
_diffrn_reflns_theta_max         36.069
_diffrn_reflns_theta_min         2.703
_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    1.299
_exptl_crystal_description       prism
_exptl_crystal_F_000             18
_exptl_crystal_size_max          4.4
_exptl_crystal_size_mid          4.3
_exptl_crystal_size_min          3.3
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       1.9(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1555
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.1069
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2514
_refine_ls_wR_factor_ref         0.2844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1121
_reflns_number_total             1555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hw5050sup1.cif
_cod_data_source_block           2k5
_cod_database_code               2108188
_cod_database_fobs_code          2108188
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              8137
_shelx_hkl_checksum              82974