Crystallization of a salt of a weak organic acid and base: solubility relations, supersaturation control and polymorphic behavior.
Jones, H. P.; Davey, R. J.; Cox, B. G.; The journal of physical chemistry. B 109 (2005) 5273–5278; doi:10.1021/jp045000q

data_1506365
_publ_section_title
;
 Crystallization of a salt of a weak organic acid and base: solubility
 relations, supersaturation control and polymorphic behavior.
;
_journal_issue                   11
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              5273
_journal_page_last               5278
_journal_paper_doi               10.1021/jp045000q
_journal_volume                  109
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C7 H3 N2 O6, 0.5(C2 H10 N2)'
_chemical_formula_structural     'C7 H3 N2 O6, 0.5(C2 H10 N2)'
_chemical_formula_sum            'C8 H8 N3 O6'
_chemical_formula_weight         242.17
_chemical_name_systematic
;
 ethylenediammonium 3,5-dinitrobenzoate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-05-14T13:15:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                94.764(2)
_cell_angle_beta                 108.278(2)
_cell_angle_gamma                97.433(2)
_cell_formula_units_Z            2
_cell_length_a                   6.7331(3)
_cell_length_b                   7.8045(3)
_cell_length_c                   10.4466(5)
_cell_measurement_reflns_used    3386
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     512.40(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.137034
_diffrn_orient_matrix_UB_12      0.227907E-1
_diffrn_orient_matrix_UB_13      0.771685E-1
_diffrn_orient_matrix_UB_21      -0.797234E-1
_diffrn_orient_matrix_UB_22      0.12786E-2
_diffrn_orient_matrix_UB_23      0.66223E-1
_diffrn_orient_matrix_UB_31      -0.29092E-2
_diffrn_orient_matrix_UB_32      -0.128331
_diffrn_orient_matrix_UB_33      0.8035E-3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3046
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.83
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.57
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             250
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.18
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.09(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+0.1318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1363
_reflns_number_gt                1463
_reflns_number_total             1784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp045000qsi20041102_072345.cif
_cod_data_source_block           eac_01d
_cod_database_code               1506365