M12L24 Spheres with Endo and Exo Coordination Sites: Scaffolds for Non-Covalent Functionalization
Kate Harris; Qing-Fu Sun; Sota Sato; Makoto Fujita; Journal of the American Chemical Society 135 (2013) 12497–12499; doi:10.1021/ja4043609

data_4120364
_publ_section_title
;
 M12L24 Spheres with Endo and Exo Coordination Sites: Scaffolds for
 Non-Covalent Functionalization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12497
_journal_page_last               12499
_journal_paper_doi               10.1021/ja4043609
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C456 H264 B20 F54 N72 O12.4 Pd12'
_chemical_formula_sum            'C456 H264 B20 F54 N72 O12.4 Pd12'
_chemical_formula_weight         9468.79
_chemical_name_common            'M12L24 sphere 2a from ligand 1a and Pd2+'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 127.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   47.453(10)
_cell_length_b                   48.537(10)
_cell_length_c                   38.130(8)
_cell_measurement_reflns_used    9068
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.23
_cell_measurement_theta_min      1.65
_cell_volume                     69506(4)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
' 2.00 degrees, 0.5 sec, detector distance 152.40 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     1.00000
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33981
_diffrn_reflns_theta_full        18.23
_diffrn_reflns_theta_max         18.23
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  0.9794
_exptl_absorpt_correction_T_min  0.9674
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.452
_exptl_crystal_description       cubic
_exptl_crystal_F_000             9482
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.561
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         9108
_refine_ls_number_restraints     965
_refine_ls_restrained_S_all      2.499
_refine_ls_R_factor_all          0.2366
_refine_ls_R_factor_gt           0.2149
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5329
_refine_ls_wR_factor_ref         0.5562
_reflns_number_gt                6529
_reflns_number_total             9108
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja4043609_si_002.cif
_cod_data_source_block           c2m
_cod_original_cell_volume        69501(24)
_cod_original_formula_sum        'C456 H264 B20 F54 N72 O12.40 Pd12'
_cod_database_code               4120364