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_2015733
_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          'C12 H12 N3 +, H3 O4 P -, H2 O4 P'
_chemical_formula_moiety         'C12 H12 N3 +, H3 O4 P -, H2 O4 P'
_chemical_formula_sum            'C12 H17 N3 O8 P2'
_chemical_formula_weight         393.23
_chemical_name_systematic
;
4-[(<i>E</i>)-phenyldiazenyl]anilinium dihydrogenphosphate--phosphoric
acid (1/1)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.5515(4)
_cell_length_b                   10.5973(9)
_cell_length_c                   34.705(3)
_cell_measurement_reflns_used    3527
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.3
_cell_measurement_theta_min      2.85
_cell_volume                     1673.9(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            22198
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         4.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'every 50 frames'
_diffrn_standards_number         '3 frames'
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(Alcock, 1970)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.237
_refine_ls_abs_structure_details 'Flack (1983), 1631 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.11(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4015
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                3323
_reflns_number_total             4015
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3051.cif
_cod_data_source_block           II
_cod_database_code               2015733