Dinicotinium sulfate
S. Athimoolam; R. K. Rajaram; Acta Crystallographica Section E 61 (2005) o2764–o2767; doi:10.1107/S1600536805023871

data_2206556
_publ_section_title
;
 Dinicotinium sulfate
;
_journal_coeditor_code           SJ6123
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2764
_journal_page_last               o2767
_journal_paper_doi               10.1107/S1600536805023871
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '2C5 H6 N O2 +, S O4 2-'
_chemical_formula_moiety         '2C5 H6 N O2 +, S O4 2-'
_chemical_formula_sum            'C12 H12 N2 O8 S'
_chemical_formula_weight         344.30
_chemical_name_common            'Dinicotinium sulfate'
_chemical_name_systematic
;
Dinicotinium sulfate
;
_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           SHELXTL/PC
_cell_angle_alpha                101.253(11)
_cell_angle_beta                 95.746(8)
_cell_angle_gamma                102.685(11)
_cell_formula_units_Z            2
_cell_length_a                   6.9663(7)
_cell_length_b                   8.3306(14)
_cell_length_c                   12.5098(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.25
_cell_measurement_theta_min      9.97
_cell_volume                     686.85(16)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'SHELXTL/PC and PLATON (Spek, 2003)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  SHELXTL/PC
_computing_structure_solution    'SHELXTL/PC (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius MACH3 four-circle'
_diffrn_measurement_method       \w-2\q
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3062
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_meas      1.654
_exptl_crystal_density_method
'flotation using a mixture of CCl~4~ and CHBr~3~'
_exptl_crystal_description       Block
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.587
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0826P)^2^+2.2093P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.2047
_reflns_number_gt                1650
_reflns_number_total             2414
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj6123.cif
_cod_data_source_block           I
_cod_original_cell_volume        686.85(15)
_cod_database_code               2206556
_cod_database_fobs_code          2206556