[2+2] Halogen-bonded boxes employing azobenzenes
Nieland, Esther; Topornicki, Thomas; Kunde, Tom; Schmidt, Bernd M.; Chemical Communications  (2019) –; doi:10.1039/C9CC03061A

data_7123400
_publ_section_title
;
 [2+2] Halogen-bonded boxes employing azobenzenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03061A
_journal_year                    2019
_chemical_formula_moiety         'C28 H24 N2, C12 F8 I2 N2'
_chemical_formula_sum            'C40 H24 F8 I2 N4'
_chemical_formula_weight         966.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-04-12 deposited with the CCDC.    2019-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.538(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7877(13)
_cell_length_b                   7.9384(6)
_cell_length_c                   24.9913(18)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.1545
_cell_measurement_theta_min      2.698
_cell_volume                     3652.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            137004
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.157
_diffrn_reflns_theta_min         2.213
_diffrn_source                   'Incoatec Microfocus Source'
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1880
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         8092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+3.4247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.0462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7354
_reflns_number_total             8092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03061a2.cif
_cod_data_source_block           mo_h18_037_0m_a
_cod_database_code               7123400
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.724
_shelx_estimated_absorpt_t_max   0.770
_shelx_res_checksum              7277