3-[(Diphenylphosphinothioyl)oxy]-<i>N</i>-methylpropan-1-aminium diphenylphosphanylthioate
Karaman, Merve; İrişli, Sevil; Büyükgüngör, Orhan; Acta Crystallographica Section C 70 (2014) 320–322; doi:10.1107/S2053229614002757

data_2019493
_publ_section_title
;
 3-[(Diphenylphosphinothioyl)oxy]-<i>N</i>-methylpropan-1-aminium
 diphenylphosphanylthioate
;
_journal_coeditor_code           QS3034
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              320
_journal_page_last               322
_journal_paper_doi               10.1107/S2053229614002757
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C16 H21 N O P S +, C12 H10 O P S -'
_chemical_formula_moiety         'C16 H21 N O P S +, C12 H10 O P S -'
_chemical_formula_sum            'C28 H31 N O2 P2 S2'
_chemical_formula_weight         539.60
_chemical_name_systematic
;
3-[(Diphenylphosphinothioyl)oxy]-<i>N</i>-methylpropan-1-aminium
diphenylphosphanylthioate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.201(3)
_cell_angle_beta                 72.482(3)
_cell_angle_gamma                74.886(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6999(4)
_cell_length_b                   13.1458(6)
_cell_length_c                   13.6405(5)
_cell_measurement_reflns_used    26612
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.54
_cell_volume                     1436.09(11)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material
'WinGX (Farrugia, 2012) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26612
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  0.8895
_exptl_absorpt_correction_T_min  0.8124
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.43
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+0.2299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                5051
_reflns_number_total             5944
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            qs3034sup1.cf
_cod_data_source_block           I
_cod_database_code               2019493
_cod_database_fobs_code          2019493