(Dimethylphosphoryl)methanaminium iodide–(dimethylphosphoryl)methanamine (1/1)
Reiss, Guido J.; Acta Crystallographica Section E 69 (2013) o1253–o1254; doi:10.1107/S1600536813019004

data_2238459
_publ_section_title
;
 (Dimethylphosphoryl)methanaminium iodide--(dimethylphosphoryl)methanamine
 (1/1)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1253
_journal_page_last               o1254
_journal_paper_doi               10.1107/S1600536813019004
_journal_volume                  69
_journal_year                    2013
_chemical_formula_moiety         'C3 H11 N O P +, I -, C3 H10 N O P'
_chemical_formula_sum            'C6 H21 I N2 O2 P2'
_chemical_formula_weight         342.09
_chemical_name_systematic
;
(Dimethylphosphoryl)methanaminium iodide--(dimethylphosphoryl)methanamine (1/1)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7791(3)
_cell_length_b                   11.1766(2)
_cell_length_c                   6.91805(12)
_cell_measurement_reflns_used    8874
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      29.3822
_cell_measurement_theta_min      2.9220
_cell_volume                     1374.68(4)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2011)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 16.2711
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Eos'
_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       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         2.928
_exptl_absorpt_coefficient_mu    2.542
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Oxford Diffraction, 2009), based on expressions derived
by Clark & Reid (1995)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.3551
_exptl_crystal_size_mid          0.1891
_exptl_crystal_size_min          0.1009
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.281
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.173(17)
_refine_ls_extinction_coef       0.00115(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL2013 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         3062
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0163
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0110P)^2^+0.3700P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0321
_refine_ls_wR_factor_ref         0.0325
_reflns_number_gt                2972
_reflns_number_total             3062
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2559.cif
_cod_data_source_block           I
_cod_original_cell_volume        1374.69(4)
_cod_database_code               2238459
_cod_database_fobs_code          2238459
_shelx_hkl_checksum              75343
_shelx_res_checksum              50923
_shelxl_version_number           20.13