Hollow and Solid Spheres Assembled from Functionalized Macrocycles Containing Adamantane.
Tominaga, Masahide; Kunitomi, Nobuto; Ohara, Kazuaki; Kawahata, Masatoshi; Itoh, Tsutomu; Katagiri, Kosuke; Yamaguchi, Kentaro; The Journal of organic chemistry 84 (2019) 5109–5117; doi:10.1021/acs.joc.9b00069

data_4034307
_publ_section_title
;
 Hollow and Solid Spheres Assembled from Functionalized Macrocycles
 Containing Adamantane.
;
_journal_issue                   9
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5109
_journal_page_last               5117
_journal_paper_doi               10.1021/acs.joc.9b00069
_journal_volume                  84
_journal_year                    2019
_chemical_formula_sum            'C98 H95 N3 O34'
_chemical_formula_weight         1858.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                113.198(2)
_cell_angle_beta                 97.551(2)
_cell_angle_gamma                90.007(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8426(4)
_cell_length_b                   20.6842(7)
_cell_length_c                   24.5207(9)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.54
_cell_measurement_theta_min      3.61
_cell_volume                     4541.3(3)
_computing_cell_refinement       'SAINT (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXLE (H\"ubschle et al., 2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            61337
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.025
_diffrn_reflns_theta_min         1.980
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.9396
_exptl_absorpt_correction_T_min  0.8643
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1344
_refine_ls_number_reflns         18543
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0847
_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^)+(0.1654P)^2^+3.0280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2389
_refine_ls_wR_factor_ref         0.2690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12665
_reflns_number_total             18543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b00069_si_005.cif
_cod_data_source_block           3b
_cod_database_code               4034307
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.910
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              47113
_shelx_hkl_checksum              33524
_shelx_fab_checksum              35926