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_4033653
_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            'C150 H88 F8 O4'
_chemical_formula_weight         2106.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.436(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.1372(10)
_cell_length_b                   20.9252(9)
_cell_length_c                   19.7816(8)
_cell_measurement_reflns_used    6204
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      65.78
_cell_measurement_theta_min      2.81
_cell_volume                     9871.1(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39936
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.655
_diffrn_reflns_theta_max         66.655
_diffrn_reflns_theta_min         2.809
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       cut-strip
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
In the crystal structure there are one toluene molecule, C7H8,
disordered in a general position and four O2Et2 solvent 
molecules, O1C4H10, disordred over an inversion center. 
These molecules were treated by QUEEZE. 
;
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8726
_refine_ls_number_restraints     564
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0994
_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^)+(0.1764P)^2^+23.0531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2924
_refine_ls_wR_factor_ref         0.3079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6396
_reflns_number_total             8726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02340_si_005.cif
_cod_data_source_block           cu_jastif85_0m_a_sqd
_cod_database_code               4033653
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.914
_shelx_estimated_absorpt_t_max   0.985
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              94377
_shelx_hkl_checksum              25183