2-Amino-4,6-dimethylpyrimidin-1-ium 1-oxo-2,6,7-trioxa-1λ^5^-phosphabicyclo[2.2.2]octane-4-carboxylate
Hou, Xu-Feng; Li, Gong-Chun; Lai, Peng-Yang; Acta Crystallographica Section E 66 (2010) o1528–; doi:10.1107/S1600536810019896

data_2226434
_publ_section_title
;
 2-Amino-4,6-dimethylpyrimidin-1-ium
 1-oxo-2,6,7-trioxa-1\l^5^-phosphabicyclo[2.2.2]octane-4-carboxylate
;
_journal_coeditor_code           FJ2308
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1528
_journal_paper_doi               10.1107/S1600536810019896
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C6 H10 N3 +, C5 H6 O6 P -'
_chemical_formula_moiety         'C6 H10 N3 +, C5 H6 O6 P -'
_chemical_formula_sum            'C11 H16 N3 O6 P'
_chemical_formula_weight         317.24
_chemical_name_systematic
;
2-Amino-4,6-dimethylpyrimidin-1-ium
1-oxo-2,6,7-trioxa-1\l^5^-phosphabicyclo[2.2.2]octane-4-carboxylate
;
_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                90.00
_cell_angle_beta                 99.611(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5080(13)
_cell_length_b                   6.1870(8)
_cell_length_c                   23.974(2)
_cell_measurement_reflns_used    5985
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      36.30
_cell_measurement_theta_min      2.20
_cell_volume                     1390.5(3)
_computing_cell_refinement       'CrystalClear-SM Expert (Rigaku/MSC, 2009)'
_computing_data_collection       'CrystalClear-SM Expert (Rigaku/MSC, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert (Rigaku/MSC, 2009)'
_computing_molecular_graphics    'CrystalStructure (Rigaku/MSC, 2009)'
_computing_publication_material  'CrystalStructure (Rigaku/MSC, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            23989
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         36.48
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.9685
_exptl_absorpt_correction_T_min  0.9468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku/MSC, 2009)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.383
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         6532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1073
_reflns_number_gt                4883
_reflns_number_total             6532
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fj2308.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2226434
_cod_database_fobs_code          2226434