Proton location in acid⋯pyridine hydrogen bonds of multi-component crystals
Seaton, Colin C.; CrystEngComm 16 (2014) 5878–; doi:10.1039/c4ce00043a

data_7215668
_publ_section_title
;
 Proton location in acid&#x22EF;pyridine hydrogen bonds of multi-component
 crystals
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              5878
_journal_paper_doi               10.1039/c4ce00043a
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C7 H4 N2 O6; C6 H7 N2 O; C7 H6 N O2'
_chemical_formula_sum            'C20 H17 N5 O9'
_chemical_formula_weight         471.39
_chemical_name_systematic
;
 3,5-dinitrobenzoic acid isonicotinamide 3-aminobenzoic acid
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                93.761(5)
_cell_angle_beta                 90.458(5)
_cell_angle_gamma                95.498(5)
_cell_formula_units_Z            2
_cell_length_a                   7.0678(4)
_cell_length_b                   8.8189(5)
_cell_length_c                   16.2172(9)
_cell_measurement_reflns_used    2186
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1815
_cell_measurement_theta_min      2.8884
_cell_volume                     1003.90(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXL97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details
;
  1 omega   -5.00   21.00   1.0000   38.2900
omega____ theta____ kappa____ phi______ frames
    -      -21.0746   77.0000   90.0000 26

  2 omega  -17.00  106.00   1.0000   38.2900
omega____ theta____ kappa____ phi______ frames
    -       22.4808   77.0000  -60.0000 123

  3 omega  -16.00  104.00   1.0000   38.2900
omega____ theta____ kappa____ phi______ frames
    -       22.4808   77.0000   60.0000 120

  4 omega  -10.00  102.00   1.0000   38.2900
omega____ theta____ kappa____ phi______ frames
    -       22.4808   77.0000 -180.0000 112

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.1030
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7010
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.253
_diffrn_reflns_theta_min         3.141
_diffrn_source
;
'Enhance (Mo) X-ray Source'   
;
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.781
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.781
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2430
_reflns_number_total             4447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce00043a2.cif
_cod_data_source_block           35dnba_ina_3aba
_cod_depositor_comments
'Adding full bibliography for 7215667--7215669.cif.'
_cod_database_code               7215668
_shelxl_version_number           2013-4
_shelx_res_checksum              54647
_shelx_hkl_checksum              45270