Location of the H atoms in ammonium persulphate by deuteron NMR. Verification by X-ray diffraction
Schmidt, Thorsten; Schmitt, Heike; Zimmermann, Herbert; Haeberlen, Ulrich; Lalowicz, Zdzisław T.; Olejniczak, Zbigniew; Oeser, Thomas; Acta Crystallographica Section B 58 (2002) 760–769; doi:10.1107/S0108768102011199

data_2103460
_publ_section_title
;
 Location of the H atoms in ammonium persulphate by deuteron NMR.
 Verification by X-ray diffraction
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              760
_journal_page_last               769
_journal_paper_doi               10.1107/S0108768102011199
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         '(SO4)2 (NH4)2'
_chemical_formula_sum            'H8 N2 O8 S2'
_chemical_formula_weight         228.20
_chemical_name_systematic
;
 ammonium persulphate-d8
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.9660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.1340(2)
_cell_length_b                   7.9324(3)
_cell_length_c                   7.7541(3)
_cell_measurement_reflns_used    786
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.0
_cell_volume                     375.88(2)
_computing_cell_refinement       'Collect Package, BRUKER NONIUS B.V. 1999'
_computing_data_collection       'Collect Package, BRUKER NONIUS B.V. 1999'
_computing_data_reduction        'Collect Package, BRUKER NONIUS B.V. 1999'
_computing_molecular_graphics    'SCHAKAL 99, Keller 1999'
_computing_structure_refinement  'SHELXL97, Sheldrick 1997'
_computing_structure_solution    'SHELXS97, Sheldrick 1990'
_diffrn_ambient_temperature      118(2)
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'NONIUS KappaCCD diffraktometer'
_diffrn_measurement_method       'phi- and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_sigmaI/netI    0.036
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1393
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         5.14
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.8681
_exptl_absorpt_correction_T_min  0.8004
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             236
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.303
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    'refined isotropic'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.028
_refine_ls_R_factor_gt           0.028
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0151P)^2^+0.2285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.068
_refine_ls_wR_factor_ref         0.069
_reflns_number_gt                768
_reflns_number_total             791
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sn0024.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2103460
_cod_database_fobs_code          2103460