Hydrogen phosphate and dihydrogen phosphate salts of 4-aminoazobenzene
Halasz, Ivan; Kaja Lukić; Hrvoj Vančik; Acta Crystallographica Section C 63 (2007) o61–o64; doi:10.1107/S0108270106050979

data_2015732
_publ_section_title
;
 Hydrogen phosphate and dihydrogen phosphate salts of 4-aminoazobenzene
;
_journal_coeditor_code           FA3051
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o61
_journal_page_last               o64
_journal_paper_doi               10.1107/S0108270106050979
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '2C12 H12 N3 +, H O4 P 2-'
_chemical_formula_moiety         '2(C12 H12 N3 +), H O4 P 2-'
_chemical_formula_sum            'C24 H25 N6 O4 P'
_chemical_formula_weight         492.47
_chemical_name_systematic
;
4-[(<i>E</i>)-phenyldiazenyl]anilinium hydrogenphosphate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.709(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.757(4)
_cell_length_b                   11.2998(15)
_cell_length_c                   7.9943(12)
_cell_measurement_reflns_used    2158
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.6
_cell_measurement_theta_min      2.93
_cell_volume                     2400.5(6)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2003)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2003)
;
_computing_data_reduction
;
CrysAlis RED
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and
Schakal99 (Keller, 1999)
;
_computing_publication_material
;
PARST (Nardelli, 1995) and
SHELXL97 (Sheldrick, 1997)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Oxford Xcalibur 3 CCD area-detector diffractometer
;
_diffrn_measurement_method       'omega scans'
_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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            17388
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'every 100 frames'
_diffrn_standards_number         '3 frames'
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.546
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4676
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1400P)^2^+1.0658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2109
_refine_ls_wR_factor_ref         0.2293
_reflns_number_gt                3382
_reflns_number_total             4676
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3051.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2015732