Experimental and theoretical charge density study of polymorphic isonicotinamide-oxalic acid molecular complexes with strong O...H...N hydrogen bonds.
Schmidtmann, Marc; Farrugia, Louis J.; Middlemiss, Derek S.; Gutmann, Matthias J.; McIntyre, Garry J.; Wilson, Chick C.; The journal of physical chemistry. A 113 (2009) 13985–13997; doi:10.1021/jp9067813

data_1516360
_publ_section_title
;
 Experimental and theoretical charge density study of polymorphic
 isonicotinamide-oxalic acid molecular complexes with strong O...H...N
 hydrogen bonds.
;
_journal_issue                   50
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              13985
_journal_page_last               13997
_journal_paper_doi               10.1021/jp9067813
_journal_volume                  113
_journal_year                    2009
_chemical_formula_sum            'C14 H14 N4 O6'
_chemical_formula_weight         334.29
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                85.523(4)
_cell_angle_beta                 88.193(4)
_cell_angle_gamma                84.252(5)
_cell_formula_units_Z            1
_cell_length_a                   3.6706(4)
_cell_length_b                   7.6027(8)
_cell_length_c                   12.4780(12)
_cell_volume                     345.31(6)
_computing_molecular_graphics    'Volkov et al, (2006)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            64585
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        58.05
_diffrn_reflns_theta_max         58.049
_diffrn_reflns_theta_min         1.637
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2004/1 (Sheldrick, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             174
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.139
_refine_diff_density_min         -0.126
_refine_diff_density_rms         0.027
_refine_ls_extinction_coef       0.12(2)
_refine_ls_extinction_expression
;
Becker, P.J. & Coppens, P. (1974) Acta Cryst., A30, 129-153.
;
_refine_ls_extinction_method     'Becker-Coppens type 2 isotropic'
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         7501
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.027
_refine_ls_R_factor_gt           0.015
_refine_ls_R_Fsqd_factor         0.016
_refine_ls_shift/su_max          0.00299
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
calc w1 = 1/[s^2^(Fo)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.017
_reflns_number_gt                7501
_reflns_number_total             8857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1-II_CD.cif
_cod_data_source_block           XD
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1516360