Halogen Bonding inside a Molecular Container
Hamdy S. El-Sheshtawy; Bassem S. Bassil; Khaleel I. Assaf; Ulrich Kortz; Werner M. Nau; Journal of the American Chemical Society 134 (2012) 19935–19941; doi:10.1021/ja3102902

data_4118960
_publ_contact_author_address
;
School of Engineering and Science, Jacobs University Bremen, 
Campus Ring 1, D-28759 Bremen, Germany
;
_publ_contact_author_email       w.nau@jacobs-university.de
_publ_contact_author_name        'Werner Nau'
_publ_section_title
;
 Halogen Bonding inside a Molecular Container
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19935
_journal_page_last               19941
_journal_paper_doi               10.1021/ja3102902
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C36 H56 I2 N24 O22'
_chemical_formula_weight         1430.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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            4
_cell_length_a                   19.3748(10)
_cell_length_b                   16.0589(10)
_cell_length_c                   16.0249(11)
_cell_measurement_reflns_used    3705
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.92
_cell_measurement_theta_min      2.54
_cell_volume                     4986.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25924
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    1.371
_exptl_absorpt_correction_T_max  0.8982
_exptl_absorpt_correction_T_min  0.8023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_description       block
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.787
_refine_diff_density_min         -2.226
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3153
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1400P)^2^+70.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2034
_refine_ls_wR_factor_ref         0.2163
_reflns_number_gt                2716
_reflns_number_total             3153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3102902_si_002.cif
_cod_data_source_block           wn4
_cod_database_code               4118960