Protonation-assisted spontaneous resolution: formation of a homochiral 2D interpenetrated hydrogen-bonded network from 4,4?-binicotinic acid under highly acidic conditions
Custelcean, Radu; Gorbunova, Maryna G.; CrystEngComm 7 (2005) 297–; doi:10.1039/b501901j

data_7203745
_publ_section_title
;
 Protonation-assisted spontaneous resolution: formation of a homochiral
 2D interpenetrated hydrogen-bonded network from 4,4?-binicotinic acid
 under highly acidic conditions
;
_journal_issue                   49
_journal_name_full               CrystEngComm
_journal_page_first              297
_journal_paper_doi               10.1039/b501901j
_journal_volume                  7
_journal_year                    2005
_chemical_formula_sum            'C12 H13 Cl N2 O6'
_chemical_formula_weight         316.69
_chemical_name_common            'binicotinic acid hydrochloride dihydrate'
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.740(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.665(6)
_cell_length_b                   6.222(3)
_cell_length_c                   11.579(6)
_cell_measurement_temperature    173(2)
_cell_volume                     686.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5003
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_T_max  0.9939
_exptl_absorpt_correction_T_min  0.9352
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0529P)^2^+0.4543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                1088
_reflns_number_total             1217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b501901j.txt
_cod_data_source_block           022s
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               7203745