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_7120697
_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         '3(C68 H56 O16), 1.65 (C H Cl3)'
_chemical_formula_sum            'C205.65 H169.65 Cl4.95 O48'
_chemical_formula_weight         3584.33
_chemical_name_common            propellicene-octacarboxylate
_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
;
2017-06-16 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.784(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3857(9)
_cell_length_b                   34.8893(17)
_cell_length_c                   29.1718(14)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      17.22
_cell_measurement_theta_min      2.24
_cell_volume                     19314.6(16)
_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-2013 (Sheldrick, 2013)'
_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  0.2183
_diffrn_reflns_av_unetI/netI     0.0978
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            462513
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        20.909
_diffrn_reflns_theta_max         20.909
_diffrn_reflns_theta_min         1.426
_diffrn_source                   'Incoatec microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.7122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_meas      ?
_exptl_crystal_description       shunk
_exptl_crystal_F_000             7487
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0027(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.430
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2492
_refine_ls_number_reflns         20335
_refine_ls_number_restraints     465
_refine_ls_restrained_S_all      1.461
_refine_ls_R_factor_all          0.2395
_refine_ls_R_factor_gt           0.1416
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3721
_refine_ls_wR_factor_ref         0.4291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9914
_reflns_number_total             20335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06798d2.cif
_cod_data_source_block           compound_12
_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               7120697
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              21117