^13^C and ^19^F solid-state NMR and X-ray crystallographic study of halogen-bonded frameworks featuring nitrogen-containing heterocycles
Szell, Patrick M. J.; Gabriel, Shaina A.; Gill, Russell D. D.; Wan, Shirley Y. H.; Gabidullin, Bulat; Bryce, David L.; Acta Crystallographica Section C 73 (2017) 157–167; doi:10.1107/S2053229616015023

data_2020824
_publ_section_title
;
 ^13^C and ^19^F solid-state NMR and X-ray crystallographic study of
 halogen-bonded frameworks featuring nitrogen-containing heterocycles
;
_journal_coeditor_code           YP3130
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              157
_journal_page_last               167
_journal_paper_doi               10.1107/S2053229616015023
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C6 F3 I3, C8 H12 N2'
_chemical_formula_moiety         'C6 F3 I3, C8 H12 N2'
_chemical_formula_sum            'C14 H12 F3 I3 N2'
_chemical_formula_weight         645.96
_chemical_melting_point          398
_chemical_name_systematic
;
2,3,5,6-Tetramethylpyrazine--1,3,5-trifluoro-2,4,6-triiodobenzene (1/1)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 115.398(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9818(3)
_cell_length_b                   26.7046(9)
_cell_length_c                   9.2220(3)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.77
_cell_measurement_theta_min      2.56
_cell_volume                     1775.69(11)
_computing_cell_refinement
;
APEX2 (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT and XPREP (Bruker, 2009)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
CIFTAB (Sheldrick, 1997)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b) and <i>WinGX</i> (Farrugia, 2012)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      200(2)
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
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_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.901
_diffrn_reflns_theta_min         1.525
_exptl_absorpt_coefficient_mu    5.305
_exptl_absorpt_correction_T_max  0.7456
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2003)
;
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_exptl_crystal_description       rod
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_exptl_crystal_size_max          0.518
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.586
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         4238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+1.8982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0674
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_database_fobs_code          2020824
_shelx_estimated_absorpt_t_min   0.170
_shelx_estimated_absorpt_t_max   0.606
_shelx_hkl_checksum              9036
_shelx_res_checksum              4286