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_7203746
_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 H10 Cl2 N2 O4'
_chemical_formula_weight         317.12
_chemical_name_common            'binicotinic acid dihydrochloride'
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 96.160(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9485(18)
_cell_length_b                   5.9793(8)
_cell_length_c                   8.6189(12)
_cell_measurement_temperature    173(2)
_cell_volume                     663.45(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2231
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.8164
_exptl_absorpt_correction_T_min  0.7978
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1537
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0378P)^2^+0.3413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                1532
_reflns_number_total             1537
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b501901j.txt
_cod_data_source_block           c:\frames\102\work\102s
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7203746