Precision Nanotube Mimics via Self-Assembly of Programmed Carbon Nanohoops.
Van Raden, Jeff M.; Leonhardt, Erik J.; Zakharov, Lev N.; Pérez-Guardiola, A; Pérez-Jiménez, A J; Marshall, Checkers R.; Brozek, Carl K.; Sancho-García, J C; Jasti, Ramesh; The Journal of organic chemistry  (2019) –; doi:10.1021/acs.joc.9b02340

data_4033656
_publ_section_title
;
 Precision Nanotube Mimics via Self-Assembly of Programmed Carbon
 Nanohoops.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b02340
_journal_year                    2019
_chemical_formula_sum            'C65 H48 F4'
_chemical_formula_weight         905.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.018(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.539(2)
_cell_length_b                   8.1703(7)
_cell_length_c                   21.1171(16)
_cell_measurement_reflns_used    1456
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      40.67
_cell_measurement_theta_min      4.43
_cell_volume                     5269.0(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHEXLTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.1084
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19529
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        49.820
_diffrn_reflns_theta_max         49.820
_diffrn_reflns_theta_min         2.894
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.7498
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
One or two solvent pentane molecules, C5H12, 40 electron,
are highly disordered inside inside the hoop molecule and 
were treated by SQUEEZE.
;
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         5331
_refine_ls_number_restraints     1086
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.2033
_refine_ls_R_factor_gt           0.1338
_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^)+(0.2200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3765
_refine_ls_wR_factor_ref         0.4214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2474
_reflns_number_total             5331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02340_si_003.cif
_cod_data_source_block           jastir87_a_sqd
_cod_database_code               4033656
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   0.982
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              93348
_shelx_hkl_checksum              11675