Twofold fused concave hosts containing two phosphorus atoms: modules for the sandwich-type encapsulation of fullerenes in variable cavities
Yamamura, Masaki; Hongo, Daigo; Nabeshima, Tatsuya; Chem. Sci. 6 (2015) 6373–; doi:10.1039/C5SC02224J

data_1529288
_publ_section_title
;
 Twofold fused concave hosts containing two phosphorus atoms: modules for
 the sandwich-type encapsulation of fullerenes in variable cavities
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              6373
_journal_paper_doi               10.1039/C5SC02224J
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C152 H96 O12 P4'
_chemical_formula_weight         2238.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-05-18 deposited with the CCDC.
2015-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.759(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.148(8)
_cell_length_b                   23.858(8)
_cell_length_c                   22.983(8)
_cell_measurement_reflns_used    13561
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.75
_cell_volume                     11717(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXD-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0917
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            255517
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.036
_diffrn_reflns_theta_min         0.953
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.992
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.276
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.293
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1581
_refine_ls_number_reflns         28158
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.293
_refine_ls_R_factor_all          0.1705
_refine_ls_R_factor_gt           0.1420
_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^)+(0.0400P)^2^+100.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3361
_refine_ls_wR_factor_ref         0.3457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19655
_reflns_number_total             28158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02224j2.cif
_cod_data_source_block           tbuc60_0ma_sqd
_cod_depositor_comments
'Adding full bibliography for 1529286--1529292.cif.'
_cod_database_code               1529288
_shelx_estimated_absorpt_t_min   0.987
_shelx_estimated_absorpt_t_max   0.996
_shelxl_version_number           2014/6
_shelx_res_checksum              44852