Ammonium <i>O</i>,<i>O</i>'-diethyl dithiophosphate
Okuniewski, Andrzej; Becker, Barbara; Acta Crystallographica Section E 67 (2011) o1749–o1750; doi:10.1107/S1600536811022811

data_2230908
_publ_section_title
;
 Ammonium <i>O</i>,<i>O</i>'-diethyl dithiophosphate
;
_journal_coeditor_code           WM2499
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1749
_journal_page_last               o1750
_journal_paper_doi               10.1107/S1600536811022811
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'N H4 +, C4 H10 O2 P S2 -'
_chemical_formula_moiety         'H4 N +, C4 H10 O2 P S2 -'
_chemical_formula_sum            'C4 H14 N O2 P S2'
_chemical_formula_weight         203.25
_chemical_melting_point          438.0(10)
_chemical_name_systematic
;
Ammonium <i>O</i>,<i>O</i>'-diethyl dithiophosphate
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 110.305(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0274(7)
_cell_length_b                   7.2006(3)
_cell_length_c                   12.5690(7)
_cell_measurement_reflns_used    2402
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.395
_cell_measurement_theta_min      2.823
_cell_volume                     1020.89(10)
_computing_cell_refinement
;
<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)
;
_computing_data_collection
;
<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)
;
_computing_data_reduction
;
<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009) and <i>Mercury</i>
(Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
<i>WinGX</i> (Farrugia, 1999) and <i>PLATON</i> (Spek, 2009)
;
_computing_structure_refinement
;
<i>SHELXL97</i> (Sheldrick, 2008)
;
_computing_structure_solution
;
<i>SHELXS97</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3955
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.3
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Oxford Diffraction, 2010) using a multi-faceted crystal
model
based on expressions derived by Clark & Reid (1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.3004
_exptl_crystal_size_mid          0.1627
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2004
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                1579
_reflns_number_total             2004
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2499.cif
_cod_data_source_block           I
_cod_original_cell_volume        1020.89(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2230908
_cod_database_fobs_code          2230908