Feeding a Molecular Squid: A Pliable Nanocarbon Receptor for Electron-Poor Aromatics.
Frydrych, Rafał; Lis, Tadeusz; Bury, Wojciech; Cybińska, Joanna; Stępień, Marcin; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c07956

data_4135220
_publ_section_title
;
 Feeding a Molecular Squid: A Pliable Nanocarbon Receptor for
 Electron-Poor Aromatics.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c07956
_journal_year                    2020
_chemical_formula_moiety         'C80 H78 O4, 3(C6 H6)'
_chemical_formula_sum            'C98 H96 O4'
_chemical_formula_weight         1337.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.979(5)
_cell_length_b                   18.110(3)
_cell_length_c                   25.513(5)
_cell_measurement_reflns_used    13890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      3.6
_cell_volume                     15238(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            63836
_diffrn_reflns_point_group_measured_fraction_full 0.742
_diffrn_reflns_point_group_measured_fraction_max 0.740
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         67.158
_diffrn_reflns_theta_min         3.625
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted cry
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       block
_exptl_crystal_F_000             5728
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 4669 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.19(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1750
_refine_ls_number_reflns         20179
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0827
_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^)+(0.1238P)^2^+9.3954P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2146
_refine_ls_wR_factor_ref         0.2355
_reflns_Friedel_coverage         0.489
_reflns_Friedel_fraction_full    0.500
_reflns_Friedel_fraction_max     0.498
_reflns_number_gt                15625
_reflns_number_total             20179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c07956_si_006.cif
_cod_data_source_block           rf05a
_cod_database_code               4135220
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.959
_shelxl_version_number           2013-2
_shelx_res_checksum              78326
_shelx_hkl_checksum              17734