Synthesis and crystal structures of 2-bromo-1,3-dimethylimidazolium iodides
Lampl, Martin; Laus, Gerhard; Kahlenberg, Volker; Wurst, Klaus; Huppertz, Hubert; Schottenberger, Herwig; Acta Crystallographica Section E 74 (2018) 497–501; doi:10.1107/S2056989018003390

data_2242413
_publ_section_title
;
 Synthesis and crystal structures of 2-bromo-1,3-dimethylimidazolium
 iodides
;
_journal_coeditor_code           HB7718
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              497
_journal_page_last               501
_journal_paper_doi               10.1107/S2056989018003390
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C5 H8 Br N2 +, I -, 1/3 C H Cl3'
_chemical_formula_moiety         'C5 H8 Br N2 +, I -, 0.33333(C H Cl3)'
_chemical_formula_sum            'C5.33333 H8.33333 Br Cl I N2'
_chemical_formula_weight         342.73
_chemical_name_systematic
;
2-Bromo-1,3-dimethylimidazolium iodide chloroform 0.33-solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 128.314(16)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   13.9135(14)
_cell_length_b                   21.9492(10)
_cell_length_c                   6.4529(6)
_cell_measurement_reflns_used    3263
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      3.343
_cell_volume                     1546.2(4)
_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2014)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2002 (Burla <i>et al.</i>,  2003)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Gemini-R Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.343
_diffrn_reflns_theta_min         3.350
_diffrn_standards_decay_%        0.0(2)
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.184
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.42704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.435
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 961 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.038(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2522
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0183
_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^)+(0.0049P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0341
_refine_ls_wR_factor_ref         0.0349
_reflns_number_gt                2426
_reflns_number_total             2522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7718sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2019-09-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1546.2(3)
_cod_original_formula_moiety     '3(C5 H8 Br N2 +), 3(I -), C H Cl3'
_cod_original_formula_iupac      '3C5 H8 Br N2 +, 3I -, C H Cl3'
_cod_original_formula_sum        'C16 H25 Br3 Cl3 I3 N6'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1028.20
_cod_database_code               2242413
_cod_database_fobs_code          2242413
_shelx_estimated_absorpt_t_min   0.257
_shelx_estimated_absorpt_t_max   0.672
_shelx_hkl_checksum              64572
_shelx_res_checksum              76088