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_1529287
_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            'C50 H52 Cl12 O6 P2'
_chemical_formula_weight         1236.26
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-05-18 deposited with the CCDC.
2015-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.2630(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0579(14)
_cell_length_b                   17.329(2)
_cell_length_c                   27.445(3)
_cell_measurement_reflns_used    8994
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      2.91
_cell_volume                     5733.3(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            32282
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.9350
_exptl_absorpt_correction_T_min  0.6855
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         13151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+3.8990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                10317
_reflns_number_total             13151
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc02224j2.cif
_cod_data_source_block           166syn_0m
_cod_depositor_comments
'Adding full bibliography for 1529286--1529292.cif.'
_cod_original_cell_volume        5733.4(12)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1529287