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

data_7123397
_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         'C16 F8 I2 N2, C28 H24 N2, C H Cl3'
_chemical_formula_sum            'C45 H25 Cl3 F8 I2 N4'
_chemical_formula_weight         1133.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     shelxt
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-04-12 deposited with the CCDC.    2019-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                104.955(2)
_cell_angle_beta                 101.248(2)
_cell_angle_gamma                102.538(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2396(7)
_cell_length_b                   12.5466(7)
_cell_length_c                   15.6010(9)
_cell_measurement_reflns_used    9710
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.8
_cell_volume                     2177.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            70409
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.197
_diffrn_reflns_theta_min         3.801
_diffrn_source                   'Incoatec Microfocus Source'
_exptl_absorpt_coefficient_mu    13.670
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.2552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1104
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.519
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         7933
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+4.1609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7459
_reflns_number_total             7933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03061a2.cif
_cod_data_source_block           BMS004_0m_a
_cod_database_code               7123397
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              50716