Noncovalent Tailoring of the Binding Pocket of Self-Assembled Cages by Remote Bulky Ancillary Groups
Yu Fang; Takashi Murase; Sota Sato; Makoto Fujita; Journal of the American Chemical Society 135 (2013) 613–615; doi:10.1021/ja311373f

data_4119196
_publ_contact_author             'Makoto Fujita'
_publ_contact_author_email       mfujita@appchem.t.u-tokyo.ac.jp
_publ_section_title
;
 Noncovalent Tailoring of the Binding Pocket of Self-Assembled Cages by
 Remote Bulky Ancillary Groups
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              613
_journal_page_last               615
_journal_paper_doi               10.1021/ja311373f
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety
; 
'C2016 H1728 F11.18 N288 O19 P1.86 Pd48, 
74.14(F6 P), F3 P, 4(F5 P), 2(F2 P), 38(O)' 
;
_chemical_formula_sum            'C2016 H1728 F483 N288 O57 P83 Pd48'
_chemical_formula_weight         47755.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'charge flipping'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.05(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   44.419(9)
_cell_length_b                   75.649(15)
_cell_length_c                   46.041(9)
_cell_measurement_reflns_used    146867
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      0.57
_cell_volume                     142358(6)
_computing_cell_refinement       HKL2000
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'Yadokari-XG 2009'
_computing_publication_material  'Yadokari-XG 2009'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    superflip
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details
;
' data sets were measured with 0.50 degrees, 0.5 sec, detector distance 90 mm 
and with 0.50 degrees, 0.5 sec, detector distance 316 mm'
;
_diffrn_measurement_device_type  'CCD MX225HE (Rayonix)'
_diffrn_measurement_method       'oscillation method, \w scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_source         'SPring-8 BL41XU beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.85000
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       77
_diffrn_reflns_limit_k_min       -77
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            557706
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         0.57
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.9756
_exptl_absorpt_correction_T_min  0.9405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       plate
_exptl_crystal_F_000             48192
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.423
_refine_diff_density_min         -1.943
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     13399
_refine_ls_number_reflns         152706
_refine_ls_number_restraints     8282
_refine_ls_restrained_S_all      1.859
_refine_ls_R_factor_all          0.1880
_refine_ls_R_factor_gt           0.1638
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4344
_refine_ls_wR_factor_ref         0.4531
_reflns_number_gt                111095
_reflns_number_total             152706
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja311373f_si_002.cif
_cod_data_source_block           M6L4
_cod_original_cell_volume        142362(49)
_cod_database_code               4119196