Non-Planar Oligoarylene Macrocycles from Biphenyl
Robert, Antoine; Dechambenoit, Pierre; Hillard, Elizabeth A.; Bock, Harald; Durola, Fabien; Chem. Commun.  (2017) –; doi:10.1039/C7CC06798D

data_7120696
_publ_section_title
;
 Non-Planar Oligoarylene Macrocycles from Biphenyl
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06798D
_journal_year                    2017
_chemical_formula_moiety         'C68 H64 O16, 2(C H Cl3)'
_chemical_formula_sum            'C70 H66 Cl6 O16'
_chemical_formula_weight         1375.92
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-19 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                84.693(4)
_cell_angle_beta                 87.138(4)
_cell_angle_gamma                66.145(4)
_cell_formula_units_Z            2
_cell_length_a                   13.6192(12)
_cell_length_b                   13.9816(12)
_cell_length_c                   19.4394(16)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.60
_cell_measurement_theta_min      2.63
_cell_volume                     3370.6(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    'Intrinsic Phasing SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II Quasar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            221832
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.142
_diffrn_reflns_theta_max         25.142
_diffrn_reflns_theta_min         1.768
_diffrn_source                   'Incoatec microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.405
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         11960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+7.6302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8765
_reflns_number_total             11960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06798d2.cif
_cod_data_source_block           compound_10
_cod_database_code               7120696
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.866
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              77243