Reversible reduction drives anion ejection and C60 binding within an FeII4L6 cage
Lu, Zhenpin; Ronson, Tanya K.; Nitschke, Jonathan R.; Chemical Science 11 (2020) 1097–1101; doi:10.1039/C9SC05728E

data_1556875
_publ_section_title
;
 Reversible reduction drives anion ejection and C60 binding within an
 FeII4L6 cage
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1097
_journal_page_last               1101
_journal_paper_doi               10.1039/C9SC05728E
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety
"'C288 H276 Fe4 N48 O24, 3(C2 F6 N1 O4 S2), 8.2(C H12 B11), 4.5(C2 H3 N) [+ 8.8 anions + solvent]'"
_chemical_formula_sum            'C311.2 H387.9 B90.2 F18 Fe4 N55.5 O36 S6'
_chemical_formula_weight         7214.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-06-20 deposited with the CCDC.	2019-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.3200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.3570(2)
_cell_length_b                   32.3478(3)
_cell_length_c                   45.8124(3)
_cell_measurement_reflns_used    51451
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.4331340098
_cell_measurement_theta_min      0.584060727671
_cell_volume                     48294.4(6)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.9.3-gb491019a-release'
_computing_data_collection       'Diamond GDA'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.9.3-gb491019a-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.5.546-gdf2e0b53-dials-1.9 (Winter, G., 2010)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I19-1'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            89539
_diffrn_reflns_point_group_measured_fraction_full 0.870
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        21.258
_diffrn_reflns_theta_max         21.258
_diffrn_reflns_theta_min         1.211
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.97710440761
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.052: AIMLESS, version 0.6.2 : 15/01/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.992
_exptl_crystal_description       block
_exptl_crystal_F_000             14978
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.26(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4647
_refine_ls_number_reflns         51296
_refine_ls_number_restraints     11859
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.1030
_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^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2631
_refine_ls_wR_factor_ref         0.2822
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.750
_reflns_Friedel_fraction_max     0.750
_reflns_number_gt                34171
_reflns_number_total             51296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05728e2.cif
_cod_data_source_block           zl194_sq
_cod_depositor_comments
;Adding full bibliography for 1556875.cif.

 Adding full bibliography for 1556875.cif.
;
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum
'C311.20 H387.90 B90.20 F18 Fe4 N55.50 O36 S6'
_cod_database_code               1556875
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.993
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              95475
_shelx_fab_checksum              36224