Investigating Hydrogen-Bonded Phosphonic Acids with Proton Ultrafast MAS NMR and DFT Calculations
Blanchard, John W.; Groy, Thomas L.; Yarger, Jeffery L.; Holland, Gregory P.; The Journal of Physical Chemistry C 116 (2012) 18824–; doi:10.1021/jp305229s

data_1508526
_publ_section_title
;
 Investigating Hydrogen-Bonded Phosphonic Acids with Proton Ultrafast MAS
 NMR and DFT Calculations
;
_journal_issue                   35
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              18824
_journal_paper_doi               10.1021/jp305229s
_journal_volume                  116
_journal_year                    2012
_chemical_formula_moiety         'C3 H7 O5 P'
_chemical_formula_sum            'C3 H7 O5 P'
_chemical_formula_weight         154.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.9560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.7700(5)
_cell_length_b                   5.3158(5)
_cell_length_c                   20.0297(17)
_cell_measurement_reflns_used    103
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      30.4806
_cell_measurement_theta_min      5.3490
_cell_volume                     612.06(9)
_computing_cell_refinement       'SAINT V7.60A (Bruker AXS, 2008)'
_computing_data_collection
'Bruker Instrument Service v2009, 3, 0, 0 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT V7.60A (Bruker AXS, 2008)'
_computing_molecular_graphics    'XShell ver. 6.3.1 (Bruker AXS, 2004)'
_computing_publication_material  'Bruker APEX2 (Bruker AXS, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            5698
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         2.04
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.333
_refine_ls_extinction_coef       0.105(8)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0519P)^2^+0.1898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                1347
_reflns_number_total             1416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp305229s_si_001.cif
_cod_data_source_block           I
_cod_database_code               1508526