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_1546268
_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         'C6 Cl5 O, C6 H8 N'
_chemical_formula_sum            'C12 H8 Cl5 N O'
_chemical_formula_weight         359.44
_chemical_melting_point          77(2)
_chemical_name_common            '4-Methylpyridinium Pentachlorophenolate'
_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                69.82(3)
_cell_angle_beta                 85.61(4)
_cell_angle_gamma                76.26(4)
_cell_formula_units_Z            2
_cell_length_a                   7.389(8)
_cell_length_b                   8.922(8)
_cell_length_c                   12.014(12)
_cell_measurement_reflns_used    1777
_cell_measurement_temperature    298
_cell_measurement_theta_max      32.9
_cell_measurement_theta_min      2.5
_cell_volume                     722.1(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6793
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1071P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1613
_refine_ls_wR_factor_ref         0.1943
_reflns_number_gt                2152
_reflns_number_total             2815
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            lq5005.cif
_cod_data_source_block           CNT-1-RT
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '75-79' was changed to '77(2)' - 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        722.1(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1546268