Experimental and theoretical 17O NMR study of the influence of hydrogen-bonding on C=O and O-H oxygens in carboxylic solids.
Wong, Alan; Pike, Kevin J.; Jenkins, Rob; Clarkson, Guy J.; Anupõld, Tiit; Howes, Andrew P.; Crout, David H. G.; Samoson, Ago; Dupree, Ray; Smith, Mark E.; The journal of physical chemistry. A 110 (2006) 1824–1835; doi:10.1021/jp055807y

data_1505723
_publ_section_title
;
 Experimental and theoretical 17O NMR study of the influence of
 hydrogen-bonding on C=O and O-H oxygens in carboxylic solids.
;
_journal_issue                   5
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              1824
_journal_page_last               1835
_journal_paper_doi               10.1021/jp055807y
_journal_volume                  110
_journal_year                    2006
_chemical_formula_sum            'C4 H3 Cl O4'
_chemical_formula_weight         150.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.395(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.558(2)
_cell_length_b                   4.9822(14)
_cell_length_c                   16.015(4)
_cell_measurement_reflns_used    2591
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     602.5(3)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Siemens SMART diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3681
_diffrn_reflns_theta_full        29.01
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                1153
_reflns_number_total             1480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp055807ysi20051220_083820.cif
_cod_data_source_block           choromaleciacid
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1505723