Crystal Structure and Solid-State Properties of 3,4-Diaminopyridine Dihydrogen Phosphate and Their Comparison with Other Diaminopyridine Salts
Mahé Nathalie; Nicolaï Béatrice; Allouchi, Hassan; Barrio, Maria; Do, Bernard; Céolin, René; Tamarit, Josep-Lluis; Rietveld, Ivo B.; Crystal Growth & Design 13 (2013) 708–; doi:10.1021/cg3014249

data_4507273
_publ_section_title
;
 Crystal Structure and Solid-State Properties of 3,4-Diaminopyridine
 Dihydrogen Phosphate and Their Comparison with Other Diaminopyridine
 Salts
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              708
_journal_paper_doi               10.1021/cg3014249
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C5 H8 N3, H2 O4 P'
_chemical_formula_sum            'C5 H10 N3 O4 P'
_chemical_formula_weight         207.13
_chemical_name_common            '3,4 DAP phosphate'
_chemical_name_systematic        '3,4 diaminopyridine dihydrogen phosphate'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 128.494(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.3871(13)
_cell_length_b                   7.7263(2)
_cell_length_c                   14.6064(9)
_cell_measurement_reflns_used    4109
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.5407
_cell_measurement_theta_min      2.9231
_cell_volume                     1800.7(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_details
;
  1 omega  -54.00   61.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -79.0000    0.0000 115

  2 omega  -54.00   61.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -79.0000   90.0000 115

  3 omega  -54.00   61.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -79.0000  180.0000 115

  4 omega  -54.00   61.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -79.0000  270.0000 115

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0284969778
_diffrn_orient_matrix_UB_12      0.0235087141
_diffrn_orient_matrix_UB_13      0.0103657544
_diffrn_orient_matrix_UB_21      -0.0239883885
_diffrn_orient_matrix_UB_22      0.0476610648
_diffrn_orient_matrix_UB_23      -0.0529989875
_diffrn_orient_matrix_UB_31      -0.0242119157
_diffrn_orient_matrix_UB_32      -0.0748785870
_diffrn_orient_matrix_UB_33      -0.0304668293
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.1148
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18604
_diffrn_reflns_theta_full        31.54
_diffrn_reflns_theta_max         31.5407
_diffrn_reflns_theta_min         2.9231
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.3350
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0645P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                1992
_reflns_number_total             2837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg3014249_si_002.cif
_cod_data_source_block           3-4-dap-phosphate
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1800.72(30)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4507273
_cell_oxdiff_length_a            20.3856(13)
_cell_oxdiff_length_b            7.7256(3)
_cell_oxdiff_length_c            14.6068(8)
_cell_oxdiff_angle_alpha         89.988(4)
_cell_oxdiff_angle_beta          128.485(7)
_cell_oxdiff_angle_gamma         90.005(4)
_cell_oxdiff_volume              1800.72(16)
_cell_oxdiff_measurement_reflns_used 4109
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_theta     26.32
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'c5 h10 n3 o4 p'