Separation and Selective Formation of Fullerene Adducts within an M(II)8L6 Cage.
Brenner, Wolfgang; Ronson, Tanya K.; Nitschke, Jonathan R.; Journal of the American Chemical Society 139 (2017) 75–78; doi:10.1021/jacs.6b11523

data_4125636
_publ_section_title
;
 Separation and Selective Formation of Fullerene Adducts within an
 M(II)8L6 Cage.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              75
_journal_page_last               78
_journal_paper_doi               10.1021/jacs.6b11523
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety
'C432 H168 F96 Fe8 N120 Ni6, 16(C2 F6 N O4 S2)'
_chemical_formula_sum            'C464 H168 F192 Fe8 N136 Ni6 O64 S32'
_chemical_formula_weight         14144.31
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n'
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   39.8773(3)
_cell_length_b                   39.8773(3)
_cell_length_c                   27.4426(4)
_cell_measurement_reflns_used    36200
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.7080
_cell_measurement_theta_min      1.5190
_cell_volume                     43639.2(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
Diamond GDA
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1149
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            300370
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        16.680
_diffrn_reflns_theta_max         16.680
_diffrn_reflns_theta_min         1.521
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.3440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark pink'
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       needle
_exptl_crystal_F_000             14064
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1563
_refine_ls_number_reflns         13220
_refine_ls_number_restraints     3985
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1451
_refine_ls_R_factor_gt           0.1276
_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^+120.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3709
_refine_ls_wR_factor_ref         0.3888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10354
_reflns_number_total             13220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b11523_si_001.cif
_cod_data_source_block           wb3_sq
_cod_original_cell_volume        43639.2(9)
_cod_database_code               4125636
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              42118
_shelx_hkl_checksum              78712
_shelx_fab_checksum              24802