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_4033652
_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            'C91 H84 Cl8 F8'
_chemical_formula_weight         1613.18
_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
_cell_angle_alpha                119.204(2)
_cell_angle_beta                 97.369(2)
_cell_angle_gamma                102.306(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3910(4)
_cell_length_b                   20.0066(6)
_cell_length_c                   20.2292(6)
_cell_measurement_reflns_used    8473
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.62
_cell_measurement_theta_min      2.55
_cell_volume                     4447.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            61640
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.696
_diffrn_reflns_theta_max         66.696
_diffrn_reflns_theta_min         2.550
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    2.795
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
Solvent molecules (four CH2Cl2 and six C5H12 
molecules (42 electrons both) in the full unit cell 
are disordered in the hoop and were treated 
by SQUEEZE.         
;
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         15617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0574P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1313
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10585
_reflns_number_total             15617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02340_si_004.cif
_cod_data_source_block           cu_jasti109_0m_a_sqd
_cod_original_cell_volume        4447.3(2)
_cod_database_code               4033652
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.679
_shelx_estimated_absorpt_t_max   0.921
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              63919
_shelx_hkl_checksum              18185