Halide-Controlled Extending-Shrinking Motion of a Covalent Cage.
Aletti, Anna B.; Miljkovic, Ana; Toma, Lucio; Bruno, Rosaria; Armentano, Donatella; Gunnlaugsson, Thorfinnur; Bergamaschi, Greta; Amendola, Valeria; The Journal of organic chemistry 84 (2019) 4221–4228; doi:10.1021/acs.joc.9b00219

data_4034236
_publ_section_title
;
 Halide-Controlled Extending-Shrinking Motion of a Covalent Cage.
;
_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              4221
_journal_page_last               4228
_journal_paper_doi               10.1021/acs.joc.9b00219
_journal_volume                  84
_journal_year                    2019
_chemical_formula_sum            'C57 H57 F18 N8 P3'
_chemical_formula_weight         1289.01
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.6540(13)
_cell_length_b                   14.6540(13)
_cell_length_c                   17.5993(16)
_cell_measurement_reflns_used    8431
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.2
_cell_measurement_theta_min      2.5
_cell_volume                     3272.9(5)
_computing_cell_refinement       'Bruker APEX'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            64671
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.286
_diffrn_reflns_theta_min         1.157
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       hexagonal-prisms
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4429
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.3357
_refine_ls_R_factor_gt           0.2496
_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^)+(0.6000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.6483
_refine_ls_wR_factor_ref         0.7363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1885
_reflns_number_total             4429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b00219_si_005.cif
_cod_data_source_block           1_PF6_RT
_cod_original_cell_volume        3272.9(7)
_cod_database_code               4034236
_shelxl_version_number           2013-4
_shelx_res_checksum              68313
_shelx_hkl_checksum              21404