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_1529291
_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            'C164 H98 Cl6 O12 P4'
_chemical_formula_weight         2597.0
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.980(5)
_cell_length_b                   17.101(4)
_cell_length_c                   17.472(4)
_cell_measurement_reflns_used    8544
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.61
_cell_volume                     6567(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41016
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.597
_diffrn_reflns_theta_min         1.165
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 3515 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     880
_refine_ls_number_reflns         12313
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0400P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.820
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.995
_reflns_number_gt                9412
_reflns_number_total             12313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02224j2.cif
_cod_data_source_block           tbuc70_0ma_sqd
_cod_depositor_comments
'Adding full bibliography for 1529286--1529292.cif.'
_cod_original_cell_volume        6567(2)
_cod_database_code               1529291
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.993
_shelxl_version_number           2014/6
_shelx_res_checksum              44649