A C60-Templated Tetrameric Porphyrin Barrel Complex via Zinc-Mediated Self-Assembly Utilizing Labile Capping Ligands
Takashi Nakamura; Hitoshi Ube; Ryosuke Miyake; Mitsuhiko Shionoya; Journal of the American Chemical Society 135 (2013) 18790–18793; doi:10.1021/ja4110446

data_4121359
_publ_section_title
;
 A C60-Templated Tetrameric Porphyrin Barrel Complex via Zinc-Mediated
 Self-Assembly Utilizing Labile Capping Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18790
_journal_page_last               18793
_journal_paper_doi               10.1021/ja4110446
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C1648 H1024 N192 O232 S64 Zn48'
_chemical_formula_weight         32416.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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            1
_cell_length_a                   30.152(9)
_cell_length_b                   30.764(9)
_cell_length_c                   44.449(13)
_cell_measurement_reflns_used    9227
_cell_measurement_temperature    93
_cell_measurement_theta_max      21.04
_cell_measurement_theta_min      2.29
_cell_volume                     41231(2)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_sigmaI/netI    0.0955
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            91909
_diffrn_reflns_theta_full        21.14
_diffrn_reflns_theta_max         21.14
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.8635
_exptl_absorpt_correction_T_min  0.7749
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             16576
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         2.517
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.767
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2674
_refine_ls_number_reflns         21496
_refine_ls_number_restraints     7945
_refine_ls_restrained_S_all      1.555
_refine_ls_R_factor_all          0.2513
_refine_ls_R_factor_gt           0.1887
_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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4575
_refine_ls_wR_factor_ref         0.4982
_reflns_number_gt                11201
_reflns_number_total             21496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4110446_si_002.cif
_cod_data_source_block           pccn
_cod_original_cell_volume        41231(21)
_cod_database_code               4121359
_verf_rfacr01_alert_3_a
;
PROBLEM: The Value of the weighted R factor is > 0.45
RESPONSE: Low quality of the crystal might be a reason for the high R factor,
         see _exptl_special_details 
;
_verf_thetm01_alert_3_a
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
         Calculated sin(theta_max)/wavelength =    0.5074
RESPONSE: Low-resolution reflection data was used, see _refine_special_details
;
_verf_rlat084_alert_3_a
;
PROBLEM: High wR2 Value (i.e. > 0.25)  ...........         0.50
RESPONSE: Low quality of the crystal might be a reason for the high R factor,
         see _exptl_special_details 
;
_verf_rlat222_alert_3_a
;
PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min)  ... 10.0 Ratio
RESPONSE: Possible disordered structures were not fully solved
          because of the use of low-resolution reflection data,
          see _refine_special_details and _exptl_special_details 
;
_verf_rlat234_alert_3_a
;
PROBLEM: Large Hirshfeld Difference S6 -- C1P  ....... 0.37 Ang.
RESPONSE: Possible disordered structures were not fully solved
          because of the use of low-resolution reflection data,
          see _refine_special_details and _exptl_special_details 

PROBLEM: Large Hirshfeld Difference C2P -- C3P  ...... 0.33 Ang.
RESPONSE: Possible disordered structures were not fully solved
          because of the use of low-resolution reflection data,
          see _refine_special_details and _exptl_special_details 

PROBLEM: Large Hirshfeld Difference C4N -- C7N  ....... 0.33 Ang.
RESPONSE: Possible disordered structures were not fully solved
          because of the use of low-resolution reflection data,
          see _refine_special_details and _exptl_special_details 
;
_verf_rlatr241_alert_2_a
;
PROBLEM: Check High  Ueq as Compared to Neighbors for  C3P
RESPONSE: Possible disordered structures were not fully solved
          because of the use of low-resolution reflection data,
          see _refine_special_details and _exptl_special_details 

PROBLEM: Check High  Ueq as Compared to Neighbors for  C6P
RESPONSE: Possible disordered structures were not fully solved
          because of the use of low-resolution reflection data,
          see _refine_special_details and _exptl_special_details 

PROBLEM: Check High  Ueq as Compared to Neighbors for  C5N
RESPONSE: Possible disordered structures were not fully solved
          because of the use of low-resolution reflection data,
          see _refine_special_details and _exptl_special_details 
;