Neutron diffraction study of a very short O–H‥N hydrogen bond: crystalline adduct of 2-methylpyridine and pentachlorophenol
Steiner, Thomas; Wilson, Chick C.; Majerz, Irena; Chemical Communications  (2000) 1231–; doi:10.1039/b001179g

data_7110891
_publ_section_title
;
 Neutron diffraction study of a very short O--H&#x2025;N hydrogen bond:
 crystalline adduct of 2-methylpyridine and pentachlorophenol
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1231
_journal_paper_doi               10.1039/b001179g
_journal_year                    2000
_chemical_formula_sum            'C12 H8 Cl5 N O'
_chemical_formula_weight         359.47
_chemical_name_systematic
; 
 2-methylpyridine pentachlorophenol 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.61(3)
_cell_angle_beta                 105.06(3)
_cell_angle_gamma                99.87(3)
_cell_formula_units_Z            2
_cell_length_a                   9.276(5)
_cell_length_b                   11.668(6)
_cell_length_c                   6.849(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    30(1)
_cell_volume                     670.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      30(1)
_diffrn_measured_fraction_theta_full 0.085
_diffrn_measured_fraction_theta_max 0.085
_diffrn_measurement_device_type  SXD
_diffrn_measurement_method       'time-of-flight LAUE diffraction'
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ISIS spallation source'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.5-5.0
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_av_sigmaI/netI    0.043
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12790
_diffrn_reflns_theta_full        66.67
_exptl_absorpt_coefficient_mu    '1.450, at 1 Angstrom'
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
The linear absorption coefficient is wavelength dependent
 and it is calculated as: 
          mu = 0.49 + 0.96 * lambda  [cm^-1]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flat plate'
_exptl_crystal_F_000             22.58
_exptl_crystal_size_max          2.5
_exptl_crystal_size_mid          2.0
_exptl_crystal_size_min          1.0
_refine_diff_density_max         3.472
_refine_diff_density_min         -3.094
_refine_diff_density_rms         0.638
_refine_ls_extinction_coef       0.160
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'Becker-Coppens Lorentzian model'
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1277P)^2^+30.3892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.1830
_reflns_number_gt                4303
_reflns_number_total             4303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001179gsup1.cif
_cod_data_source_block           sxd1
_cod_original_cell_volume        670.0(6)
_cod_database_code               7110891