Exploring the salt–cocrystal continuum with solid-state NMR using natural-abundance samples: implications for crystal engineering
Rajput, Lalit; Banik, Manas; Yarava, Jayasubba Reddy; Joseph, Sumy; Pandey, Manoj Kumar; Nishiyama, Yusuke; Desiraju, Gautam R.; IUCrJ 4 (2017) –; doi:10.1107/S205225251700687X

data_1546263
_publ_section_title
;
 Exploring the salt--cocrystal continuum with solid-state NMR using
 natural-abundance samples: implications for crystal engineering
;
_journal_issue                   4
_journal_name_full               IUCrJ
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205225251700687X
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C7 H3 N2 O6, C7 H10 N'
_chemical_formula_sum            'C14 H13 N3 O6'
_chemical_formula_weight         319.27
_chemical_melting_point          120.5(15)
_chemical_name_common            '4-Ethylpyridinium 3,5-Dinitrobenzoate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.500(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.439(6)
_cell_length_b                   14.091(9)
_cell_length_c                   12.167(8)
_cell_measurement_reflns_used    5652
_cell_measurement_temperature    110
_cell_measurement_theta_max      33.8
_cell_measurement_theta_min      2.4
_cell_volume                     1440.2(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  Rigaku
_diffrn_measurement_method       'profile data from \w-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  0.0968
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13152
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         2815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0640P)^2^+0.3170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                2683
_reflns_number_total             2815
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            lq5005.cif
_cod_data_source_block           SA-2-LT
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '119-122' was changed to '120.5(15)'
- the average value was taken and precision was estimated.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        1440.0(17)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1546263