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_4120365
_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 N72 Pd12) 6(B F4) 12(B F) O267.20 '
_chemical_formula_sum            'C456 H264 B18 F36 N72 O267.2 Pd12'
_chemical_formula_weight         13181.97
_chemical_name_common            'M12L24 sphere 2b from ligand 1b and Pd2+'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           69
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2 2'
_symmetry_space_group_name_H-M   'F m m m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   61.994(12)
_cell_length_b                   61.977(12)
_cell_length_c                   61.977(12)
_cell_measurement_reflns_used    6608
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.12
_cell_measurement_theta_min      0.80
_cell_volume                     238128(8)
_computing_cell_refinement       HKL2000
_computing_data_collection       BSS
_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      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
' 1.00 degrees, 0.5 sec, detector distance 125.60 mm, Al 1300um attn.'
_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  0.1646
_diffrn_reflns_av_sigmaI/netI    0.1008
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            31401
_diffrn_reflns_theta_full        17.12
_diffrn_reflns_theta_max         17.12
_diffrn_reflns_theta_min         0.80
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.9866
_exptl_absorpt_correction_T_min  0.9605
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.368
_exptl_crystal_description       cubic
_exptl_crystal_F_000             26430
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         6742
_refine_ls_number_restraints     569
_refine_ls_restrained_S_all      2.029
_refine_ls_R_factor_all          0.3084
_refine_ls_R_factor_gt           0.2432
_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          0.5430
_refine_ls_wR_factor_ref         0.5713
_reflns_number_gt                3393
_reflns_number_total             6742
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja4043609_si_003.cif
_cod_data_source_block           fmmm
_cod_original_cell_volume        238128(83)
_cod_original_formula_sum        'C456 H264 B18 F36 N72 O267.20 Pd12'
_cod_database_code               4120365