The reaction of 3-nitropyridine with sulfite ions; a pathway to 2,5-disubstituted pyridines
Bakke, Jan M.; Ranes, Eli; Rømming, Christian; Sletvold, Ingrid; Journal of the Chemical Society, Perkin Transactions 1  (2000) 1241–; doi:10.1039/a909875e

data_7213249
_publ_section_title
;
 The reaction of 3-nitropyridine with sulfite ions; a pathway to
 2,5-disubstituted pyridines
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1241
_journal_paper_doi               10.1039/a909875e
_journal_year                    2000
_chemical_formula_moiety         C5H4N2O7S2.Na2.4H2O
_chemical_formula_sum            'C5 H11.5 N2 Na2 O11 S2'
_chemical_formula_weight         385.76
_chemical_name_systematic
; 
Disodium salt of5-N-sulfinohydroxylamino-2-pyridinesulfonic acid
 ? 
;
_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                66.5210(10)
_cell_angle_beta                 79.9700(10)
_cell_angle_gamma                88.0550(10)
_cell_formula_units_Z            2
_cell_length_a                   5.40230(10)
_cell_length_b                   11.5582(3)
_cell_length_c                   12.6662(3)
_cell_measurement_temperature    150(2)
_cell_volume                     713.77(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10834
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         6.81
_exptl_absorpt_coefficient_mu    0.492
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             395
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         5016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.224
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                4086
_reflns_number_total             5016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909875esup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C5 H11.50 N2 Na2 O11 S2'
_cod_database_code               7213249