Tetramethylammonium dihydrogen phosphate hemihydrate
Fujita, Kyoko; MacFarlane, Douglas R.; Noguchi, Keiichi; Ohno, Hiroyuki; Acta Crystallographica Section E 65 (2009) o797–; doi:10.1107/S1600536809009179

data_2221409
_publ_section_title
;
 Tetramethylammonium dihydrogen phosphate hemihydrate
;
_journal_coeditor_code           IS2395
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o797
_journal_paper_doi               10.1107/S1600536809009179
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C4 H12 N +, H2 O4 P -, 0.5H2 O'
_chemical_formula_moiety         'C4 H12 N +, H2 O4 P -, 0.5(H2 O)'
_chemical_formula_sum            'C4 H15 N O4.5 P'
_chemical_formula_weight         180.14
_chemical_name_common            'tetramethylammonium dihydrogen phosphate'
_chemical_name_systematic
;
Tetramethylammonium dihydrogen phosphate hemihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 103.6140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.3213(3)
_cell_length_b                   9.2607(2)
_cell_length_c                   13.1990(2)
_cell_measurement_reflns_used    13463
_cell_measurement_temperature    193.0(10)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.4
_cell_volume                     1701.34(6)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku/MSC, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku/MSC, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      193.0(10)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14805
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_diffrn_reflns_theta_min         5.74
_exptl_absorpt_coefficient_mu    2.723
_exptl_absorpt_correction_T_max  0.580
_exptl_absorpt_correction_T_min  0.390
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(<i>NUMABS</i>; Higashi, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.307
_refine_ls_extinction_coef       0.0039(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+2.3234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                1505
_reflns_number_total             1565
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is2395.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2221409
_cod_database_fobs_code          2221409