Crystal structure of bis-(4-dimethylaminopyridinium) bis-(2-nitrobenzoate) trihydrate
Sivakumar, N.; Muralidharan, S.; Chakkaravarthi, G.; Velmurugan, D.; Anbalagan, G.; Acta Crystallographica Section E 70 (2014) 221–223; doi:10.1107/S1600536814020583

data_2240007
_publ_section_title
;
 Crystal structure of bis-(4-dimethylaminopyridinium)
 bis-(2-nitrobenzoate) trihydrate
;
_journal_coeditor_code           SU2777
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              221
_journal_page_last               223
_journal_paper_doi               10.1107/S1600536814020583
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '2C7 H11 N2 + , 2C7 H4 N O4 - ,  3H2 O'
_chemical_formula_moiety         '2(C7 H4 N O4) -, 2(C7 H11 N2) +, 3(H2 O)'
_chemical_formula_sum            'C14 H18 N3 O5.5'
_chemical_formula_weight         316.31
_chemical_name_systematic
;
Bis-(4-dimethylaminopyridinium) bis-(2-nitrobenzoate) trihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                108.2380(10)
_cell_angle_beta                 92.247(2)
_cell_angle_gamma                101.5120(10)
_cell_formula_units_Z            4
_cell_length_a                   7.6163(4)
_cell_length_b                   12.7215(7)
_cell_length_c                   17.3478(9)
_cell_measurement_reflns_used    668
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      1.2
_cell_volume                     1554.93(14)
_computing_cell_refinement
;
SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2004)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXS97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24031
_diffrn_reflns_theta_full        26.47
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         1.24
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.9792
_exptl_absorpt_correction_T_min  0.9711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.359
_refine_ls_extinction_coef       0.088(5)
_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   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6426
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0740P)^2^+0.5049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1535
_reflns_number_gt                5126
_reflns_number_total             6426
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            su2777sup1.cif
_cod_data_source_block           I
_cod_database_code               2240007
_cod_database_fobs_code          2240007