Pathway-Dependent Post-assembly Modification of an Anthracene-Edged M(II)4L6 Tetrahedron.
Ronson, Tanya K.; Pilgrim, Ben S.; Nitschke, Jonathan R.; Journal of the American Chemical Society 138 (2016) 10417–10420; doi:10.1021/jacs.6b06710

data_4130786
_publ_section_title
;
 Pathway-Dependent Post-assembly Modification of an Anthracene-Edged
 M(II)4L6 Tetrahedron.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10417
_journal_page_last               10420
_journal_paper_doi               10.1021/jacs.6b06710
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
'C264 H156 Fe4 N48, C60, 8(Cl O4), 3(C2 H3 N)'
_chemical_formula_sum            'C330 H165 Cl8 Fe4 N51 O32'
_chemical_formula_weight         5863.12
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   26.1142(13)
_cell_length_b                   26.1142(13)
_cell_length_c                   110.422(6)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      80.054
_cell_measurement_theta_min      5.051
_cell_volume                     65214(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       87
_diffrn_reflns_limit_l_min       -91
_diffrn_reflns_number            46512
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        39.968
_diffrn_reflns_theta_max         39.968
_diffrn_reflns_theta_min         2.526
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.934
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.4396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.896
_exptl_crystal_description       block
_exptl_crystal_F_000             17988
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         8542
_refine_ls_number_restraints     2463
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1701
_refine_ls_R_factor_gt           0.1274
_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^+350.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3501
_refine_ls_wR_factor_ref         0.3749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5419
_reflns_number_total             8542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b06710_si_004.cif
_cod_data_source_block           jnb117_sqd
_cod_original_cell_volume        65214(7)
_cod_database_code               4130786
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.576
_shelx_estimated_absorpt_t_max   0.722
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              207
_shelx_hkl_checksum              12035