2-Amino-5-chloropyridinium 6-oxo-1,6-dihydropyridine-2-carboxylate 0.85-hydrate
Hemamalini, Madhukar; Fun, Hoong-Kun; Acta Crystallographica Section E 66 (2010) o2338–; doi:10.1107/S1600536810032307

data_2227315
_publ_section_title
;
 2-Amino-5-chloropyridinium 6-oxo-1,6-dihydropyridine-2-carboxylate
 0.85-hydrate
;
_journal_coeditor_code           CI5153
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2338
_journal_paper_doi               10.1107/S1600536810032307
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C5 H6 Cl N2 + , C6 H4 N O3 - , 0.85H2 O'
_chemical_formula_moiety         'C5 H6 N2 Cl + , C6 H4 O3 N - , 0.85H2 O'
_chemical_formula_sum            'C11 H11.7 Cl N3 O3.85'
_chemical_formula_weight         282.98
_chemical_name_systematic
;
2-Amino-5-chloropyridinium 6-oxo-1,6-dihydropyridine-2-carboxylate 0.85-hydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   3.80960(10)
_cell_length_b                   15.6046(3)
_cell_length_c                   20.9370(3)
_cell_measurement_reflns_used    6806
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.03
_cell_measurement_theta_min      2.34
_cell_volume                     1244.65(4)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (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 SMART APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            15196
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.9660
_exptl_absorpt_correction_T_min  0.8513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.169
_refine_ls_abs_structure_details 'Flack (1983), with 1458 Fridel pairs'
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0653P)^2^+0.0443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                3129
_reflns_number_total             3632
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci5153.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C11 H11.70 Cl N3 O3.85'
_cod_database_code               2227315
_cod_database_fobs_code          2227315