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_4131485
_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, C60, 8(B F4), 6.5(C7 H5 N O2)'
_chemical_formula_sum            'C435 H344.5 B8 F32 Fe4 N54.5 Ni6 O13'
_chemical_formula_weight         7813.27
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
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_cell_angle_gamma                120
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_cell_length_b                   38.8188(8)
_cell_length_c                   111.372(3)
_cell_measurement_reflns_used    45351
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      1.4650
_cell_volume                     145342(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'GDA 8.44; generic data acquisition software'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean 0
_diffrn_detector_type            'Dectris Pilatus 2M'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       '\f rotation with 0.2 degree frames'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I19'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       92
_diffrn_reflns_limit_l_min       -92
_diffrn_reflns_number            316681
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        16.681
_diffrn_reflns_theta_max         16.681
_diffrn_reflns_theta_min         1.471
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.5653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_description       block
_exptl_crystal_F_000             48480
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1302
_refine_ls_number_reflns         9789
_refine_ls_number_restraints     2795
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1546
_refine_ls_R_factor_gt           0.1424
_refine_ls_shift/su_max          0.001
_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^+1500.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3763
_refine_ls_wR_factor_ref         0.3879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8028
_reflns_number_total             9789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b05788_si_003.cif
_cod_data_source_block           dwc60_sq
_cod_original_cell_volume        145342(7)
_cod_original_formula_sum        'C435 H344.50 B8 F32 Fe4 N54.50 Ni6 O13'
_cod_database_code               4131485
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.994
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              36240
_shelx_hkl_checksum              70379
_shelx_fab_checksum              22876