Halogen and Hydrogen Bond Architectures in Switchable Chains of Di- and Trihaloimidazoles
Andrzejewski, Michał; Marciniak, Jędrzej; Rajewski, Kacper W.; Katrusiak, Andrzej; Crystal Growth & Design 15 (2015) 1658–; doi:10.1021/cg501561w

data_4512829
_publ_section_title
;
 Halogen and Hydrogen Bond Architectures in Switchable Chains of Di- and
 Trihaloimidazoles
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1658
_journal_paper_doi               10.1021/cg501561w
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C3 H2 I2 N2'
_chemical_formula_sum            'C3 H2 I2 N2'
_chemical_formula_weight         319.87
_chemical_name_common            diiodoimidazole
_chemical_name_systematic
;
 4,5-diiodo-1H-imidazole
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.8867(4)
_cell_length_b                   6.8867(4)
_cell_length_c                   28.275(3)
_cell_measurement_reflns_used    612
_cell_measurement_temperature    296
_cell_measurement_theta_max      16.5890
_cell_measurement_theta_min      3.2770
_cell_volume                     1340.99(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.1(7)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details
;
  1 omega  -14.00   16.60   0.8500  150.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7462   77.0000  -90.0000 36

  2 omega  -38.00   49.55   0.8500  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.6056   77.0000  150.0000 103

  3 omega    3.00   77.80   0.8500  150.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7462 -135.0000   64.0000 88

  4 omega  -85.00    3.40   0.8500  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.6056  -57.0000  150.0000 104

  5 omega  -85.00    3.40   0.8500  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.6056  -57.0000   30.0000 104
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1018697000
_diffrn_orient_matrix_UB_12      0.0126433000
_diffrn_orient_matrix_UB_13      -0.0020837000
_diffrn_orient_matrix_UB_21      0.0126301000
_diffrn_orient_matrix_UB_22      -0.1022085000
_diffrn_orient_matrix_UB_23      -0.0001558000
_diffrn_orient_matrix_UB_31      -0.0085544000
_diffrn_orient_matrix_UB_32      -0.0004391000
_diffrn_orient_matrix_UB_33      -0.0249982000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2087
_diffrn_reflns_av_unetI/netI     0.2449
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            9628
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.188
_diffrn_reflns_theta_min         2.882
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.268
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.169
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.179
_refine_ls_abs_structure_details
;
 Flack x determined using 99 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1517
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.2999
_refine_ls_R_factor_gt           0.0803
_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^)+(0.0620P)^2^+0.0230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1923
_reflns_Friedel_coverage         0.534
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.893
_reflns_number_gt                474
_reflns_number_total             1517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501561w_si_002.cif
_cod_data_source_block           diiodoimidazole
_cod_depositor_comments
'Adding full bibliography for 4512828--4512833.cif.'
_cod_original_cell_volume        1341.0(2)
_cod_database_code               4512829
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid body (RIGU) restrains
 C2, N3, C4, C5, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'