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_7120695
_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         'C80 H64 O16, C H Cl3, C H4 O'
_chemical_formula_sum            'C82 H69 Cl3 O17'
_chemical_formula_weight         1432.72
_chemical_name_common            tetra-3,6-phenanthrylene-octacarboxylate
_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
;
2017-06-16 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                111.079(8)
_cell_angle_beta                 92.542(6)
_cell_angle_gamma                114.545(5)
_cell_formula_units_Z            2
_cell_length_a                   14.0409(16)
_cell_length_b                   15.132(2)
_cell_length_c                   19.481(2)
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.30
_cell_measurement_theta_min      2.20
_cell_volume                     3420.3(8)
_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 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_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  0.0977
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            223838
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        23.779
_diffrn_reflns_theta_max         23.779
_diffrn_reflns_theta_min         1.151
_diffrn_source                   'Incoatec microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_meas      ?
_exptl_crystal_description       shunk
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.773
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         9984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.1237
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1063P)^2^+55.2437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3599
_refine_ls_wR_factor_ref         0.3713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8100
_reflns_number_total             9984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06798d2.cif
_cod_data_source_block           compound_11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7120695
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.912
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              55707