Neutral and Zwitterionic Polymorphs of 2-(p-Tolylamino)nicotinic Acid
Nath, Naba K.; Kumar, S. Sudalai; Nangia, Ashwini; Crystal Growth & Design 11 (2011) 4594–; doi:10.1021/cg200853u

data_4501194
_publ_section_title
;
 Neutral and Zwitterionic Polymorphs of 2-(p-Tolylamino)nicotinic Acid
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4594
_journal_paper_doi               10.1021/cg200853u
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C27 H22 N4 O10'
_chemical_formula_weight         562.49
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.870(11)
_cell_angle_beta                 86.132(9)
_cell_angle_gamma                85.992(9)
_cell_formula_units_Z            2
_cell_length_a                   7.8000(8)
_cell_length_b                   13.0415(16)
_cell_length_c                   14.0098(15)
_cell_measurement_reflns_used    4752
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1092
_cell_measurement_theta_min      2.8065
_cell_volume                     1286.0(3)
_computing_cell_refinement
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
;
_computing_data_collection
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
;
_computing_molecular_graphics
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)/Bruker'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.3291
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 1 omega -49.00 49.00 1.0000 30.0000
 omega____ theta____ kappa____ phi______ frames
 - 18.7785 -77.0000 -120.0000 98
 2 omega -7.00 83.00 1.0000 30.0000
 omega____ theta____ kappa____ phi______ frames
 - 18.7785 77.0000 0.0000 90
 3 omega -51.00 49.00 1.0000 30.0000
 omega____ theta____ kappa____ phi______ frames
 - 18.7785 -77.0000 150.0000 100
 4 omega -47.00 9.00 1.0000 30.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.0128 77.0000 90.0000 56
 5 omega 1.00 52.00 1.0000 30.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.0128 37.0000 120.0000 51
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0016853
_diffrn_orient_matrix_UB_12      0.0377538
_diffrn_orient_matrix_UB_13      -0.0543238
_diffrn_orient_matrix_UB_21      -0.0045241
_diffrn_orient_matrix_UB_22      0.0467954
_diffrn_orient_matrix_UB_23      0.0134618
_diffrn_orient_matrix_UB_31      0.0911108
_diffrn_orient_matrix_UB_32      -0.0011241
_diffrn_orient_matrix_UB_33      -0.0006718
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0153
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9618
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.86559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.0093(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0634P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                3625
_reflns_number_total             5273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200853u_si_006.cif
_cod_data_source_block           TNA-NBA
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4501194