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_4033655
_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            'C77 H41 Cl15 F12'
_chemical_formula_weight         1725.85
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   19.8149(6)
_cell_length_b                   19.8149(6)
_cell_length_c                   13.6041(6)
_cell_measurement_reflns_used    2506
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      65.05
_cell_measurement_theta_min      2.57
_cell_volume                     4625.8(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1426
_diffrn_reflns_av_unetI/netI     0.1122
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33778
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.593
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         2.575
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    4.606
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       needle
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
The molecule form a columns in the packing. 
In the structure there are five CHCl3 solvent molecules
located inside and outside the columns. These CHCl3 
solvent molecules have been located and refined.
Another CHCl3 solvent molecules are highly diosrdered 
and occipied positions in the center line of 
the columns. Those CHCl3 solvent molecules were treated
by SQUEEZE. It is hard to evaluate how many molecules 
could located in area treated by SQUEEZE; these 
positions could be not full occupied.     
;
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1125P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2261
_refine_ls_wR_factor_ref         0.2475
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2437
_reflns_number_total             5443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02340_si_001.cif
_cod_data_source_block           cu_jastir117_0m_a_sqd
_cod_database_code               4033655
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.586
_shelx_estimated_absorpt_t_max   0.914
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              63223
_shelx_hkl_checksum              86378