Halogen-bonded halide networks from chiral neutral spacers
Lieffrig, Julien; Niassy, Arnode G.; Jeannin, Olivier; Fourmigué, Marc; CrystEngComm 17 (2015) 50–; doi:10.1039/C4CE01935K

data_7218479
_publ_section_title
;
 Halogen-bonded halide networks from chiral neutral spacers
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              50
_journal_paper_doi               10.1039/C4CE01935K
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C20 H44 N, 2(C16 H8 F8 I2 O2), Br'
_chemical_formula_sum            'C52 H60 Br F16 I4 N O4'
_chemical_formula_weight         1654.51
_chemical_name_systematic
; 
6,6'-(((2R,3R)-butane-2,3-diyl)bis(oxy))
bis(1,2,4,5-tetrafluoro-3-iodobenzene),
tetrapentylammonium bromide
;
_space_group_IT_number           16
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2'
_symmetry_space_group_name_H-M   'P 2 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9519(3)
_cell_length_b                   10.6977(3)
_cell_length_c                   30.4347(10)
_cell_measurement_reflns_used    7259
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.68
_cell_volume                     3240.15(17)
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_collection       'Bruker SAINT (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (ALtomare et al., 1999))'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14071
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         0.67
_exptl_absorpt_coefficient_mu    2.625
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.339
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.252
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6357
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+20.4616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1711
_reflns_number_gt                5040
_reflns_number_total             6357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce01935k1.cif
_cod_data_source_block           RR1-Pe4NBr
_cod_depositor_comments
'Adding full bibliography for 7218474--7218479.cif.'
_cod_original_sg_symbol_H-M      P222
_cod_original_formula_sum        'C52 H60 Br F16 I4 N O4 '
_cod_database_code               7218479