Tuning the Redox Properties of Fullerene Clusters within a Metal-Organic Capsule.
Rizzuto, Felix J.; Wood, Daniel M.; Ronson, Tanya K.; Nitschke, Jonathan R.; Journal of the American Chemical Society 139 (2017) 11008–11011; doi:10.1021/jacs.7b05788

data_4131484
_publ_section_title
;
 Tuning the Redox Properties of Fullerene Clusters within a Metal-Organic
 Capsule.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11008
_journal_page_last               11011
_journal_paper_doi               10.1021/jacs.7b05788
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety
'C336 H312 Fe4 N48 Ni6, 3(C60), 8(S O3 C F3), 0.5(C4 H10 O)'
_chemical_formula_sum            'C526 H317 F24 Fe4 N48 Ni6 O24.5 S8'
_chemical_formula_weight         8989.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                65.910(2)
_cell_angle_beta                 67.466(2)
_cell_angle_gamma                62.464(3)
_cell_formula_units_Z            2
_cell_length_a                   31.3706(16)
_cell_length_b                   31.5616(16)
_cell_length_c                   33.5735(15)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.404
_cell_measurement_theta_min      4.319
_cell_volume                     26120(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Rigaku Saturn 724+ detector on Crystal Logic diffractometer'
_diffrn_measurement_method       '\w  scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1065
_diffrn_reflns_av_unetI/netI     0.1448
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            91331
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        16.680
_diffrn_reflns_theta_max         16.681
_diffrn_reflns_theta_min         0.731
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.7442
_exptl_absorpt_correction_T_min  0.5082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             9242
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3802
_refine_ls_number_reflns         31517
_refine_ls_number_restraints     10269
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.2004
_refine_ls_R_factor_gt           0.1310
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 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          0.3251
_refine_ls_wR_factor_ref         0.3751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14141
_reflns_number_total             31517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b05788_si_002.cif
_cod_data_source_block           dwa_sq_d
_cod_original_formula_sum        'C526 H317 F24 Fe4 N48 Ni6 O24.50 S8'
_cod_database_code               4131484
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.996
_shelxl_version_number           2013-2
_shelx_res_checksum              54719
_shelx_hkl_checksum              41544