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_7214324
_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 Br2 N4, 2(N O3), 1.5(H2 O)'
_chemical_formula_sum            'C26 H31 Br2 N6 O7.5'
_chemical_formula_weight         707.38
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_method           'CRYSTALS (Betteridge et al., 2003)'
_cell_angle_alpha                100.8354(10)
_cell_angle_beta                 95.9931(10)
_cell_angle_gamma                95.4914(11)
_cell_formula_units_Z            2
_cell_length_a                   8.7552(2)
_cell_length_b                   9.1778(2)
_cell_length_c                   19.3962(5)
_cell_measurement_reflns_used    6324
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     1511.75(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.040
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23830
_diffrn_reflns_theta_full        26.977
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         2.155
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.736
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.93
_refine_diff_density_min         -1.08
_refine_ls_extinction_coef       280(20)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9691
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6907
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.0002020
_refine_ls_shift/su_mean         0.0000113
_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: 
 16.0 23.7 11.0 2.77 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2173
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.2173
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                4657
_reflns_number_total             6931
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.73
_oxford_diffrn_Wilson_scale      25.96
_oxford_refine_ls_r_factor_ref   0.0994
_oxford_refine_ls_scale          0.2098(3)
_oxford_reflns_number_all        6907
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c3ce41944d.txt
_cod_data_source_block           1NO3
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7214324