Halogen bonds in the crystal structure of 5-bromo-3,4′-bipyridine – 1,4-diiodotetrafluorobenzene (2/1), C26H14Br2F4I2N4
Wang, Weizhou; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 1187–1188; doi:10.1515/ncrs-2019-0316

data_8105973
_publ_section_title
;
 Halogen bonds in the crystal structure of 5-bromo-3,4&#x2032;-bipyridine
 -- 1,4-diiodotetrafluorobenzene (2/1), C26H14Br2F4I2N4
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1187
_journal_page_last               1188
_journal_paper_doi               10.1515/ncrs-2019-0316
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C6 F4 I2, 2(C10 H7 Br N2)'
_chemical_formula_sum            'C26 H14 Br2 F4 I2 N4'
_chemical_formula_weight         872.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                102.745(4)
_cell_angle_beta                 105.489(4)
_cell_angle_gamma                91.949(4)
_cell_formula_units_Z            1
_cell_length_a                   8.7472(4)
_cell_length_b                   8.7822(4)
_cell_length_c                   9.4065(4)
_cell_measurement_reflns_used    4493
_cell_measurement_temperature    290
_cell_measurement_theta_max      26.4130
_cell_measurement_theta_min      3.7010
_cell_volume                     675.88(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      290.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -13.00  45.00   1.00    5.55    --  -15.84  38.00-120.00   58
  2  \w    -85.00   1.00   1.00    5.55    --  -15.84 -38.00 120.00   86
  3  \w      8.00  80.00   1.00    5.55    --   16.93  57.00   0.00   72
  4  \w    -41.00  17.00   1.00    5.55    --   16.93 -57.00  90.00   58
  5  \w    -20.00  56.00   1.00    5.55    --   16.93 -99.00 -60.00   76
  6  \w    -13.00  56.00   1.00    5.55    --   16.93 -99.00-180.00   69
  7  \w     -7.00  81.00   1.00    5.55    --   16.93  77.00-120.00   88
  8  \w    -20.00  56.00   1.00    5.55    --   16.93 -99.00  60.00   76
  9  \w     -7.00  84.00   1.00    5.55    --   16.93  77.00  90.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0683136000
_diffrn_orient_matrix_UB_12      0.0388967000
_diffrn_orient_matrix_UB_13      -0.0083763000
_diffrn_orient_matrix_UB_21      -0.0338045000
_diffrn_orient_matrix_UB_22      0.0723625000
_diffrn_orient_matrix_UB_23      0.0121123000
_diffrn_orient_matrix_UB_31      0.0366164000
_diffrn_orient_matrix_UB_32      0.0132338000
_diffrn_orient_matrix_UB_33      0.0792148000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10224
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.350
_diffrn_reflns_theta_min         3.509
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.334
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.142
_exptl_crystal_description       block
_exptl_crystal_F_000             410
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.0555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2689
_reflns_number_total             3228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0316_suppl.cif
_cod_data_source_block           wwz180521-4
_cod_original_cell_volume        675.88(5)
_cod_database_code               8105973
_shelx_estimated_absorpt_t_max   0.400
_shelx_estimated_absorpt_t_min   0.327
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11), C13(H13)
;
_shelx_res_checksum              39751
_shelx_hkl_checksum              94483
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.606
_oxdiff_exptl_absorpt_empirical_full_min 0.752