Lemniscular [16]Cycloparaphenylene: A Radially Conjugated Figure-Eight Aromatic Molecule.
Senthilkumar, Kabali; Kondratowicz, Mateusz; Lis, Tadeusz; Chmielewski, Piotr J.; Cybińska, Joanna; Zafra, José L; Casado, Juan; Vives, Thomas; Crassous, Jeanne; Favereau, Ludovic; Stępień, Marcin; Journal of the American Chemical Society 141 (2019) 7421–7427; doi:10.1021/jacs.9b01797

data_4128689
_publ_section_title
;
 Lemniscular [16]Cycloparaphenylene: A Radially Conjugated Figure-Eight
 Aromatic Molecule.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7421
_journal_page_last               7427
_journal_paper_doi               10.1021/jacs.9b01797
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C104 H84 N2 O8, 7.5(C6 H5 Cl)'
_chemical_formula_sum            'C149 H121.5 Cl7.5 N2 O8'
_chemical_formula_weight         2333.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                115.86(3)
_cell_angle_beta                 91.04(2)
_cell_angle_gamma                101.68(2)
_cell_formula_units_Z            2
_cell_length_a                   14.638(3)
_cell_length_b                   21.545(5)
_cell_length_c                   21.633(5)
_cell_measurement_reflns_used    14377
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.5
_cell_volume                     5968(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Xcalibur R kappa-geometry diffractometer with a Ruby CCD detector
;
_diffrn_measurement_method       w/
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42278
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.579
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5
Analytical numeric absorption correction using a
multifaceted crystal model based on expressions
derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             2442
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.470
_exptl_crystal_size_min          0.430
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1495
_refine_ls_number_reflns         23363
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0708
_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^)+(0.0961P)^2^+7.8825P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1797
_refine_ls_wR_factor_ref         0.2063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16596
_reflns_number_total             23363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01797_si_004.cif
_cod_data_source_block           ksk307a
_cod_original_formula_sum        'C149 H121.50 Cl7.50 N2 O8'
_cod_database_code               4128689
_shelx_estimated_absorpt_t_min   0.879
_shelx_estimated_absorpt_t_max   0.904
_shelxl_version_number           2013-2
_shelx_res_checksum              33091
_shelx_hkl_checksum              70495