Observation of strong halogen bonds in the solid state structures of bis-haloimidazolium macrocycles
White, Nicholas G.; Caballero, Antonio; Beer, Paul D.; CrystEngComm 16 (2014) 3722–; doi:10.1039/c3ce41944d

data_7214323
_publ_section_title
;
 Observation of strong halogen bonds in the solid state structures of
 bis-haloimidazolium macrocycles
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              3722
_journal_paper_doi               10.1039/c3ce41944d
_journal_volume                  16
_journal_year                    2014
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C26 H28 I2 N4, 3(C2 H6 O S), 2(Br)'
_chemical_formula_sum            'C32 H46 Br2 I2 N4 O3 S3'
_chemical_formula_weight         1044.54
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           'CRYSTALS (Betteridge et al., 2003)'
_cell_angle_alpha                89.5146(4)
_cell_angle_beta                 84.8630(4)
_cell_angle_gamma                85.5213(5)
_cell_formula_units_Z            2
_cell_length_a                   8.70900(10)
_cell_length_b                   8.97990(10)
_cell_length_c                   26.0376(3)
_cell_measurement_reflns_used    8237
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2021.92(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Crystal Maker (Crystal Maker Software Ltd.)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            32968
_diffrn_reflns_theta_full        26.670
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         5.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.722
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.17
_refine_diff_density_min         -1.28
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9631
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.0010653
_refine_ls_shift/su_mean         0.0000257
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 21.5 31.3 15.3 4.01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1121
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1121
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                6909
_reflns_number_total             9210
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.95
_oxford_diffrn_Wilson_scale      26.78
_oxford_refine_ls_r_factor_ref   0.0529
_oxford_refine_ls_scale          0.23832(15)
_oxford_reflns_number_all        8317
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c3ce41944d.txt
_cod_data_source_block           6Br
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7214323