Variation of guest selectivity within [Fe4L4](8+) tetrahedral cages through subtle modification of the face-capping ligand.
Ferguson, Alan; Staniland, Robert W.; Fitchett, Christopher M.; Squire, Marie A.; Williamson, Bryce E.; Kruger, Paul E.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14550–14553; doi:10.1039/c4dt02337d

data_7032103
_publ_section_title
;
 Variation of guest selectivity within [Fe4L4](8+) tetrahedral cages
 through subtle modification of the face-capping ligand.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14550
_journal_page_last               14553
_journal_paper_doi               10.1039/c4dt02337d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'C156 H108 Fe4 N36 O12, 12.5(C2 H3 N), (H2 O), 8(B F4)'
_chemical_formula_sum            'C181 H147.5 B8 F32 Fe4 N48.5 O13'
_chemical_formula_weight         4127.84
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-02
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                103.56(3)
_cell_angle_beta                 95.35(3)
_cell_angle_gamma                115.89(3)
_cell_formula_units_Z            2
_cell_length_a                   21.800(4)
_cell_length_b                   22.237(4)
_cell_length_c                   22.317(5)
_cell_measurement_reflns_used    1038
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      11.05
_cell_measurement_theta_min      2.76
_cell_volume                     9222(5)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            92634
_diffrn_reflns_theta_full        23.14
_diffrn_reflns_theta_max         23.14
_diffrn_reflns_theta_min         1.07
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         1.487
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.619
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2145
_refine_ls_number_reflns         24491
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.620
_refine_ls_R_factor_all          0.1579
_refine_ls_R_factor_gt           0.1325
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3831
_refine_ls_wR_factor_ref         0.4020
_reflns_number_gt                16988
_reflns_number_total             24491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02337d2.cif
_cod_data_source_block           '[OTf@1]'
_cod_depositor_comments
'Adding full bibliography for 7032102--7032104.cif.'
_cod_original_cell_volume        9222(3)
_cod_database_code               7032103
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-F1 = B1-F2 = B1-F3 = B1-F4
 1.32301 with sigma of 0.02
 F1-F2 = F1-F3 = F1-F4 = F2-F3 = F2-F4 = F3-F4
 2.160475 with sigma of 0.02
 B2-F5 = B2-F6 = B2-F7 = B2-F8
 1.32301 with sigma of 0.02
 F5-F6 = F5-F7 = F5-F8 = F6-F7 = F6-F8 = F7-F8
 2.160475 with sigma of 0.02
 B3-F21 = B3-F22 = B3-F23 = B3-F24
 1.32301 with sigma of 0.02
 F21-F22 = F21-F23 = F21-F24 = F22-F23 = F22-F24 = F23-F24
 2.160475 with sigma of 0.02
 B4-F9 = B4-F10 = B4-F11 = B4-F12
 1.32301 with sigma of 0.02
 F9-F10 = F9-F11 = F9-F12 = F10-F11 = F10-F12 = F11-F12
 2.160475 with sigma of 0.02
 B5-F29 = B5-F30 = B5-F31 = B5-F32
 1.32301 with sigma of 0.02
 F29-F30 = F29-F31 = F29-F32 = F30-F31 = F30-F32 = F31-F32
 2.160475 with sigma of 0.02
 B6-F17 = B6-F18 = B6-F19 = B6-F20
 1.32301 with sigma of 0.02
 F17-F18 = F17-F19 = F17-F20 = F18-F19 = F18-F20 = F19-F20
 2.160475 with sigma of 0.02
 B7-F13 = B7-F14 = B7-F15 = B7-F16
 1.32301 with sigma of 0.02
 F13-F14 = F13-F15 = F13-F16 = F14-F15 = F14-F16 = F15-F16
 2.160475 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(B1) = Uiso(F4) = Uiso(F2) = Uiso(F1) = Uiso(F3)
Uiso(B7) = Uiso(F14) = Uiso(F13) = Uiso(F15) = Uiso(F16)
Uiso(B3) = Uiso(F23) = Uiso(F24) = Uiso(F21) = Uiso(F22)
Uiso(F17) = Uiso(F18) = Uiso(B6) = Uiso(F19) = Uiso(F20)
Uiso(N39) = Uiso(C169) = Uiso(C170)
4. Same fragment restrains
{N40, C161, C162}
{N43, C167, C168}
{N46, C157, C158}
{N45, C165, C166}
{N41, C173, C174}
{N37, C159, C160}
{N39, C169, C170}
as
{N42, C175, C176}
5. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
6.a Me refined with riding coordinates:
 C162(H16A,H16B,H16C), C172(H17A,H17B,H17C), C176(H17D,H17E,H17F), C164(H16D,
 H16E,H16F), C158(H15A,H15B,H15C), C160(H16G,H16H,H16I), C166(H16J,H16K,H16L),
 C174(H17G,H17H,H17I), C168(H16M,H16N,H16O), C170(H17J,H17K,H17L)
6.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C60(H60), C116(H116), C9(H9), C72(H72), C120(H120), C33(H33),
 C12(H12), C42(H42), C107(H107), C45(H45), C69(H69), C95(H95), C57(H57),
 C117(H117), C8(H8), C71(H71), C141(H141), C143(H143), C4(H4), C48(H48),
 C24(H24), C11(H11), C6(H6), C68(H68), C131(H131), C108(H108), C119(H119),
 C47(H47), C54(H54), C59(H59), C13(H13), C96(H96), C21(H21), C36(H36), C23(H23),
  C144(H144), C56(H56), C14(H14), C16(H16), C15(H15), C114(H114), C18(H18),
 C20(H20), C105(H105), C93(H93), C61(H61), C35(H35), C1A(H1A), C49(H49),
 C132(H132), C140(H140), C83(H83), C44(H44), C52(H52), C50(H50), C51(H51),
 C104(H104), C90(H90), C109(H109), C1C(H1C), C80(H80), C66(H66), C1D(H1D),
 C81(H81), C112(H112), C92(H92), C1E(H1E), C63(H63), C126(H126), C111(H111),
 C128(H128), C64(H64), C84(H84), C123(H123), C129(H129), C62(H62), C25(H25),
 C102(H102), C124(H124), C78(H78), C40(H40), C136(H136), C138(H138), C37(H37),
 C121(H121), C85(H85), C122(H122), C110(H110), C1F(H1F), C39(H39), C26(H26),
 C97(H97), C76(H76), C86(H86), C133(H133), C73(H73), C27(H27), C38(H38),
 C75(H75), C134(H134), C87(H87), C98(H98), C88(H88), C135(H135), C100(H100),
 C99(H99), C74(H74)
;