(Dimethylphosphoryl)methanaminium hydrogen oxalate‒oxalic acid (2/1)
Bialek, Sebastian; Clemens, Rebecca; Reiss, Guido J.; Acta Crystallographica Section E 70 (2014) o312–; doi:10.1107/S1600536814002931

data_2239482
_publ_section_title
;
 (Dimethylphosphoryl)methanaminium hydrogen oxalate--oxalic acid (2/1)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o312
_journal_paper_doi               10.1107/S1600536814002931
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C3 H11 N O P +, C2 H O4 -, 0.5C2 H2 O4'
_chemical_formula_moiety         'C3 H11 N O P +, C2 H O4 -, 0.5(C2 H2 O4)'
_chemical_formula_sum            'C6 H13 N O7 P'
_chemical_formula_weight         242.14
_chemical_name_systematic
;
(Dimethylphosphoryl)methanaminium hydrogen oxalate; oxalic acid
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                   11.1482(6)
_cell_length_b                   13.0903(7)
_cell_length_c                   7.0432(4)
_cell_measurement_reflns_used    9422
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      35.88
_cell_measurement_theta_min      2.89
_cell_volume                     1027.84(10)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            92924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.400
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       lath
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.519
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.155
_refine_ls_abs_structure_details
;
refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.54(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0194
_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^)+(0.0300P)^2^+0.1500P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0521
_reflns_number_gt                2990
_reflns_number_total             3002
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm5001sup1.cif
_cod_data_source_block           I
_cod_database_code               2239482
_cod_database_fobs_code          2239482
_shelx_estimated_absorpt_t_min   0.866
_shelx_estimated_absorpt_t_max   0.962