#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/34/2103460.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2103460
loop_
_publ_author_name
'Schmidt, Thorsten'
'Schmitt, Heike'
'Zimmermann, Herbert'
'Haeberlen, Ulrich'
'Lalowicz, Zdzisław T.'
'Olejniczak, Zbigniew'
'Oeser, Thomas'
_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/[σ²(Fo²)+(0.0151P)²+0.2285P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_type_symbol
S1 0.21386(5) 0.85461(4) 0.63745(4) 0.01348(16) Uani d 1 S
O3 0.11829(13) 1.01867(13) 0.52348(13) 0.0213(3) Uani d 1 O
O1 0.18431(17) 0.71093(13) 0.52550(13) 0.0242(3) Uani d 1 O
O4 0.08329(16) 0.84816(12) 0.78417(12) 0.0191(2) Uani d 1 O
O2 0.43508(14) 0.91084(13) 0.67523(13) 0.0198(2) Uani d 1 O
N1 0.2287(2) 0.88530(17) 0.14819(16) 0.0172(3) Uani d 1 N
D1 0.217(4) 0.862(2) 0.042(3) 0.036(6) Uiso d 1 H
D2 0.352(4) 0.908(3) 0.182(3) 0.036(5) Uiso d 1 H
D3 0.191(4) 0.798(3) 0.196(3) 0.048(7) Uiso d 1 H
D4 0.143(3) 0.963(3) 0.169(2) 0.022(4) Uiso d 1 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
S1 0.0126(2) 0.0144(2) 0.0133(2) 0.00095(10) 0.00006(13) -0.00041(10)
O3 0.0098(5) 0.0242(5) 0.0285(6) -0.0041(4) -0.0056(4) 0.0105(4)
O1 0.0247(5) 0.0233(6) 0.0247(5) -0.0002(4) 0.0030(4) -0.0107(4)
O4 0.0188(5) 0.0248(5) 0.0141(5) 0.0022(4) 0.0028(4) 0.0008(3)
O2 0.0130(4) 0.0217(5) 0.0239(5) 0.0003(4) -0.0028(4) 0.0016(4)
N1 0.0161(6) 0.0173(6) 0.0181(6) 0.0005(4) 0.0002(5) -0.0002(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle
O2 S1 O1 . 116.00(6)
O2 S1 O4 . 115.36(6)
O1 S1 O4 . 113.45(6)
O2 S1 O3 . 98.62(5)
O1 S1 O3 . 106.37(6)
O4 S1 O3 . 104.68(5)
O3 O3 S1 3_576 105.44(9)
D1 N1 D2 . 112(2)
D1 N1 D3 . 104(2)
D2 N1 D3 . 110(2)
D1 N1 D4 . 110.0(19)
D2 N1 D4 . 111.2(19)
D3 N1 D4 . 109(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
S1 O2 . 1.4344(9)
S1 O1 . 1.4346(10)
S1 O4 . 1.4478(10)
S1 O3 . 1.6518(10)
O3 O3 3_576 1.4949(17)
N1 D1 . 0.84(2)
N1 D2 . 0.80(2)
N1 D3 . 0.83(3)
N1 D4 . 0.84(2)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_4
_geom_torsion
O2 S1 O3 O3 3_576 -178.60(10)
O1 S1 O3 O3 3_576 60.96(11)
O4 S1 O3 O3 3_576 -59.42(11)
