Perfluorinated Ligands Induce Meridional Metal Stereochemistry to Generate M8L12, M10L15, and M12L18 Prisms.
Kieffer, Marion; Pilgrim, Ben S.; Ronson, Tanya K.; Roberts, Derrick A.; Aleksanyan, Mina; Nitschke, Jonathan R.; Journal of the American Chemical Society 138 (2016) 6813–6821; doi:10.1021/jacs.6b02445

data_4130344
_publ_section_title
;
 Perfluorinated Ligands Induce Meridional Metal Stereochemistry to
 Generate M8L12, M10L15, and M12L18 Prisms.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6813
_journal_page_last               6821
_journal_paper_doi               10.1021/jacs.6b02445
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
'C480 H330 F60 Fe10 N60 O30, 10(B12 F12), 0.5(C6 H6), 11(C2 H3 N)'
_chemical_formula_sum            'C505 H366 B120 F180 Fe10 N71 O30'
_chemical_formula_weight         13184.37
_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-2014/6
_cell_angle_alpha                100.828(4)
_cell_angle_beta                 96.645(5)
_cell_angle_gamma                96.070(5)
_cell_formula_units_Z            2
_cell_length_a                   29.007(3)
_cell_length_b                   35.476(4)
_cell_length_c                   44.206(4)
_cell_measurement_reflns_used    9002
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.934
_cell_measurement_theta_min      4.379
_cell_volume                     44000(8)
_computing_cell_refinement
;
'Bruker SAINT' 
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
'Bruker SAINT' 
;
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.889
_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  0.0786
_diffrn_reflns_av_unetI/netI     0.1114
_diffrn_reflns_Laue_measured_fraction_full 0.888
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            124506
_diffrn_reflns_point_group_measured_fraction_full 0.888
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        16.000
_diffrn_reflns_theta_max         15.995
_diffrn_reflns_theta_min         0.656
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.4927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.995
_exptl_crystal_description       block
_exptl_crystal_F_000             13226
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     6872
_refine_ls_number_reflns         41937
_refine_ls_number_restraints     19971
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.2321
_refine_ls_R_factor_gt           0.1794
_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^+275.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4400
_refine_ls_wR_factor_ref         0.4719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22957
_reflns_number_total             41937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b02445_si_003.cif
_cod_data_source_block           mk1034_sqd
_cod_database_code               4130344
_shelx_estimated_absorpt_t_min   0.996
_shelx_estimated_absorpt_t_max   0.998
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              41068
_shelx_hkl_checksum              91093