Entropy-Driven Ball-in-Bowl Assembly of Fullerene and Geodesic Phenylene Bowl
Ikemoto, Koki; Kobayashi, Ryo; Sato, Sota; Isobe, Hiroyuki; Organic Letters  (2017) –; doi:10.1021/acs.orglett.7b00899

data_1545748
_publ_section_title
;
 Entropy-Driven Ball-in-Bowl Assembly of Fullerene and Geodesic Phenylene
 Bowl
;
_journal_name_full               'Organic Letters'
_journal_paper_doi               10.1021/acs.orglett.7b00899
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C160 H150, C60'
_chemical_formula_sum            'C220 H150'
_chemical_formula_weight         2793.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.486(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2965(8)
_cell_length_b                   29.0416(11)
_cell_length_c                   42.143(4)
_cell_measurement_reflns_used    2921
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      26.6260
_cell_measurement_theta_min      2.0350
_cell_volume                     18664(2)
_computing_cell_refinement
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)'
_computing_data_collection       'KEK ugui'
_computing_data_reduction
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'PAD Pilatus3 6M (Dectris)'
_diffrn_measurement_method       'oscillation method, \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.900
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.1252
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            30485
_diffrn_reflns_point_group_measured_fraction_full 0.835
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_theta_full        26.744
_diffrn_reflns_theta_max         26.744
_diffrn_reflns_theta_min         1.776
_diffrn_source                   'KEK PF BL17A beamline'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    0.994
_exptl_crystal_description       rod
_exptl_crystal_F_000             5880
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 2172 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   3.0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2244
_refine_ls_number_reflns         16331
_refine_ls_number_restraints     4150
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.0889
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2313
_refine_ls_wR_factor_ref         0.2666
_reflns_Friedel_coverage         0.637
_reflns_Friedel_fraction_full    0.667
_reflns_Friedel_fraction_max     0.667
_reflns_number_gt                8798
_reflns_number_total             16331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b00899_si_002.cif
_cod_data_source_block           shelxl_sq
_cod_database_code               1545748
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.989
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              71317
_shelx_hkl_checksum              41260
_shelx_fab_checksum              6960