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_7032104
_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_sum            'C175.25 H132.625 F24 Fe4 N41.625 O39.875 S8'
_chemical_formula_weight         4395.53
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-10
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.5873(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.1264(6)
_cell_length_b                   39.5634(6)
_cell_length_c                   29.0472(4)
_cell_measurement_reflns_used    26053
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.5396
_cell_measurement_theta_min      2.6922
_cell_volume                     40936.8(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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      120.01(10)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega -110.00  -41.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9115  -37.0000   90.0000 69
 
  2 omega   -5.00   31.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9115   37.0000   60.0000 36
 
  3 omega  -31.00   34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9115   33.0000 -147.0000 65
 
  4 omega   71.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       39.9115 -125.0000   30.0000 25
 
  5 omega   38.00   97.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       39.9115 -125.0000  150.0000 59
 
  6 omega   33.00   81.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  -30.0000  -90.0000 48
 
  7 omega   80.00  109.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  -94.0000  120.0000 29
 
  8 omega   30.00   87.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  -30.0000 -180.0000 57
 
  9 omega   51.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  -45.0000   90.0000 40
 
 10 omega   50.00   87.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  -94.0000 -150.0000 37
 
 11 omega  103.00  177.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749   30.0000   90.0000 74
 
 12 omega   35.00   96.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  -45.0000  -30.0000 61
 
 13 omega   46.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  -30.0000  120.0000 45
 
 14 omega -114.00  -10.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9115  -57.0000  -90.0000 104
 
 15 omega -119.00   -6.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9115  -77.0000 -180.0000 113
 
 16 omega   10.00  114.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       39.9115   57.0000   60.0000 104
 
 17 omega   30.00   89.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  -30.0000   30.0000 59
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0406074000
_diffrn_orient_matrix_UB_12      0.0113557000
_diffrn_orient_matrix_UB_13      0.0181101000
_diffrn_orient_matrix_UB_21      -0.0118058000
_diffrn_orient_matrix_UB_22      0.0118891000
_diffrn_orient_matrix_UB_23      0.0459405000
_diffrn_orient_matrix_UB_31      0.0090699000
_diffrn_orient_matrix_UB_32      -0.0352874000
_diffrn_orient_matrix_UB_33      0.0213424000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0871
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            103300
_diffrn_reflns_theta_full        65.09
_diffrn_reflns_theta_max         65.09
_diffrn_reflns_theta_min         5.55
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.887
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             16848
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         1.709
_refine_diff_density_min         -1.270
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.310
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2274
_refine_ls_number_reflns         34781
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.320
_refine_ls_R_factor_all          0.2118
_refine_ls_R_factor_gt           0.1469
_refine_ls_shift/su_max          0.002
_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          0.3851
_refine_ls_wR_factor_ref         0.4205
_reflns_number_gt                16026
_reflns_number_total             34781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02337d2.cif
_cod_data_source_block           '[2][NTf]'
_cod_depositor_comments
'Adding full bibliography for 7032102--7032104.cif.'
_cod_original_cell_volume        40936.7(11)
_cod_database_code               7032104
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Shared sites
{F11, O1V}
{O17, F1Y}
{O7, F15}
{O5, F1Z}
{O18, F16}
{O2, F17}
{O3, F1X}
3. Restrained distances
 C1K-F1P
 1.35 with sigma of 0.02
 C1K-F1M
 1.35 with sigma of 0.02
 C1K-F3
 1.35 with sigma of 0.02
 F1P-F1M
 2.11 with sigma of 0.02
 F1M-F3
 2.11 with sigma of 0.02
 F1P-F3
 2.11 with sigma of 0.02
 O1Q-O2A
 2.42 with sigma of 0.02
 O1Q-O1T
 2.42 with sigma of 0.02
 O2A-O1T
 2.42 with sigma of 0.02
 O2A-F1P
 2.9 with sigma of 0.02
 O2A-F3
 2.9 with sigma of 0.02
 O1T-F3
 2.9 with sigma of 0.02
 O1T-F1M
 2.9 with sigma of 0.02
 O1Q-F1M
 2.9 with sigma of 0.02
 O1Q-F1P
 2.9 with sigma of 0.02
 S1M-O1T
 1.45 with sigma of 0.02
 S1M-O1Q
 1.45 with sigma of 0.02
 S1M-O2A
 1.45 with sigma of 0.02
 S1M-C1K
 1.7 with sigma of 0.02
 S12-C1E
 1.7 with sigma of 0.02
 S12-O1D
 1.45 with sigma of 0.02
 S12-O1E
 1.45 with sigma of 0.02
 C1E-F1
 1.35 with sigma of 0.02
 C1E-F39
 1.35 with sigma of 0.02
 F19-C1E
 1.35 with sigma of 0.02
 F19-F1
 2.11 with sigma of 0.02
 F1-F39
 2.11 with sigma of 0.02
 F39-F19
 2.11 with sigma of 0.02
 O1E-F1
 2.9 with sigma of 0.02
 O1E-F39
 2.9 with sigma of 0.02
 O1D-F39
 2.9 with sigma of 0.02
 O1D-F19
 2.9 with sigma of 0.02
 S12-O37
 1.45 with sigma of 0.02
 O37-F1
 2.9 with sigma of 0.02
 O37-F19
 2.9 with sigma of 0.02
 O37-O1E
 2.42 with sigma of 0.02
 O1E-O1D
 2.42 with sigma of 0.02
 O1D-O37
 2.42 with sigma of 0.02
 S6-C1G
 1.7 with sigma of 0.02
 S6-O1I
 1.45 with sigma of 0.02
 S6-O1G
 1.45 with sigma of 0.02
 S6-O1J
 1.45 with sigma of 0.02
 O1J-O1I
 2.42 with sigma of 0.02
 O1I-O1G
 2.42 with sigma of 0.02
 O1G-O1J
 2.42 with sigma of 0.02
 S10-C1W
 1.7 with sigma of 0.02
 S10-O1F
 1.45 with sigma of 0.02
 S10-O32
 1.45 with sigma of 0.02
 S10-O27
 1.45 with sigma of 0.02
 O32-O27
 2.42 with sigma of 0.02
 O27-O1F
 2.42 with sigma of 0.02
 O1F-O32
 2.42 with sigma of 0.02
 O1F-F13
 2.9 with sigma of 0.02
 F7-O1F
 2.9 with sigma of 0.02
 O32-F7
 2.9 with sigma of 0.02
 O32-F9
 2.9 with sigma of 0.02
 F9-O27
 2.9 with sigma of 0.02
 O27-F13
 2.9 with sigma of 0.02
 C1W-F9
 1.35 with sigma of 0.02
 C1W-F7
 1.35 with sigma of 0.02
 C1W-F13
 1.35 with sigma of 0.02
 F7-F13
 2.11 with sigma of 0.02
 F9-F13
 2.11 with sigma of 0.02
 F9-F7
 2.11 with sigma of 0.02
 F2-F28
 2.11 with sigma of 0.02
 F2-F24
 2.11 with sigma of 0.02
 F24-F28
 2.11 with sigma of 0.02
 C1-F2
 1.35 with sigma of 0.02
 C1-F28
 1.35 with sigma of 0.02
 C1-F24
 1.35 with sigma of 0.02
 C1-S9
 1.7 with sigma of 0.02
 F2-O15
 2.9 with sigma of 0.02
 O30-F2
 2.9 with sigma of 0.02
 O1J-F1B
 2.9 with sigma of 0.02
 F10-O1J
 2.9 with sigma of 0.02
 O1I-F1B
 2.9 with sigma of 0.02
 O1G-F10
 2.9 with sigma of 0.02
 C1G-F1B
 1.35 with sigma of 0.02
 C1G-F10
 1.35 with sigma of 0.02
 F1B-F10
 2.11 with sigma of 0.02
 O1I-F35
 2.9 with sigma of 0.02
 O1G-F35
 2.9 with sigma of 0.02
 C1G-F35
 1.35 with sigma of 0.02
 F1B-F35
 2.11 with sigma of 0.02
 F10-F35
 2.11 with sigma of 0.02
 S5-C1F
 1.7 with sigma of 0.02
 S5-O1C
 1.45 with sigma of 0.02
 S5-O1B
 1.45 with sigma of 0.02
 S5-O20
 1.45 with sigma of 0.02
 O1B-O20
 2.42 with sigma of 0.02
 O1B-O1C
 2.42 with sigma of 0.02
 O1C-O20
 2.42 with sigma of 0.02
 O1B-F32
 2.9 with sigma of 0.02
 O1B-F31
 2.9 with sigma of 0.02
 O20-F31
 2.9 with sigma of 0.02
 O20-F36
 2.9 with sigma of 0.02
 O1C-F36
 2.9 with sigma of 0.02
 O1C-F32
 2.9 with sigma of 0.02
 C1F-F32
 1.35 with sigma of 0.02
 C1F-F36
 1.35 with sigma of 0.02
 C1F-F31
 1.35 with sigma of 0.02
 F32-F31
 2.11 with sigma of 0.02
 F31-F36
 2.11 with sigma of 0.02
 F36-F32
 2.11 with sigma of 0.02
 C1P-F1U
 1.35 with sigma of 0.02
 C1P-F4
 1.35 with sigma of 0.02
 C1P-F1Q
 1.35 with sigma of 0.02
 S1L-C1P
 1.7 with sigma of 0.02
 F1Q-F4
 2.11 with sigma of 0.02
 F4-F1U
 2.11 with sigma of 0.02
 F1U-F1Q
 2.11 with sigma of 0.02
 S1L-O1U
 1.45 with sigma of 0.02
 S1L-O1L
 1.45 with sigma of 0.02
 O1U-O1L
 2.42 with sigma of 0.02
 O1L_$1-O1U
 2.42 with sigma of 0.02
 O1U_$1-O1L
 2.42 with sigma of 0.02
 O1U-F1U
 2.9 with sigma of 0.02
 O1U-F1Q
 2.9 with sigma of 0.02
 O1L-F1U
 2.9 with sigma of 0.02
 O1L-F4
 2.9 with sigma of 0.02
 N1-C11
 1.15 with sigma of 0.02
 N1P-C1O
 1.15 with sigma of 0.02
 N23-C12
 1.15 with sigma of 0.02
 N1H-C1Y
 1.15 with sigma of 0.02
 N1M-C1L
 1.15 with sigma of 0.02
 N1J-C1S
 1.15 with sigma of 0.02
 N7-C1N
 1.15 with sigma of 0.02
 C1N-C1D
 1.45 with sigma of 0.02
 C1L-C1H
 1.45 with sigma of 0.02
 C11-C14
 1.45 with sigma of 0.02
 C22-C1O
 1.45 with sigma of 0.02
 C1Z-C1Y
 1.45 with sigma of 0.02
 C12-C10
 1.45 with sigma of 0.02
 C1B-C1S
 1.45 with sigma of 0.02
 N23-C10
 2.6 with sigma of 0.04
 N1M-C1H
 2.6 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uiso(F16) = Uiso(O18)
Uiso(F1Z) = Uiso(O5)
Uiso(F3) = Uiso(O2A) = Uiso(S1M) = Uiso(O1Q) = Uiso(O1T) = Uiso(C1K) = Uiso(F1M)
Uiso(F1U) = Uiso(C1P) = Uiso(S1L) = Uiso(O1U) = Uiso(O1L) = Uiso(F1Q) = Uiso(F4)
Uiso(S9) = Uiso(O30) = Uiso(O36) = Uiso(O15) = Uiso(C1) = Uiso(F28) = Uiso(F2) =
Uiso(S6) = Uiso(O1G) = Uiso(O1J) = Uiso(O1I) = Uiso(F1B) = Uiso(C1G) = Uiso(F10)
Uiso(S5) = Uiso(O1B) = Uiso(O20) = Uiso(O1C) = Uiso(C1F) = Uiso(F31) = Uiso(F32)
5. Others
 Fixed Sof: S2(0.4) S3(0.3) O7(0.3) O2(0.7) O3(0.4) O5(0.3) O17(0.7) O18(0.3)
 C9(0.3) S1(0.75) S10(0.5) F11(0.75) O1A(0.75) C13(0.75) S12(0.5) S1A(0.3)
 F27(0.3) O1D(0.5) O1E(0.5) O1F(0.5) N1(0.5) C10(0.5) H10A(0.5) H10B(0.5)
 H10C(0.5) F19(0.5) C11(0.5) N23(0.5) F1(0.5) C12(0.5) O37(0.5) F39(0.5)
 C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) S1G(0.25) N1H(0.5) N1J(0.5) O1K(0.5)
 S1M(0.5) C1N(0.5) C1O(0.5) N1P(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5)
 C1S(0.5) O1H(0.25) F4(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) H1DC(0.5) N7(0.5)
 O27(0.5) F1M(0.5) O1N(0.5) F1U(0.5) C1A(0.4) F6(0.3) F5(0.25) C29(0.3)
 O1L(0.5) C1P(0.5) C1Y(0.5) C1Z(0.5) H1ZA(0.5) H1ZB(0.5) H1ZC(0.5) C22(0.5)
 H22A(0.5) H22B(0.5) H22C(0.5) N1M(0.5) O1O(0.5) F1P(0.5) C1W(0.5) F9(0.5)
 F13(0.5) F7(0.5) C24(0.25) O1Q(0.5) O2A(0.5) O32(0.5) O1R(0.5) O1S(0.3)
 F12(0.3) O1M(0.5) O1T(0.5) C1K(0.5) F3(0.5) C1H(0.5) H1HA(0.5) H1HB(0.5)
 H1HC(0.5) C1L(0.5) C1E(0.5) O1V(0.25) F1Y(0.3) F15(0.4) F1Z(0.4) F16(0.4)
 F17(0.3) F1X(0.3)
6.a Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C1B(H1BA,H1BB,H1BC), C1D(H1DA,H1DB,
 H1DC), C1Z(H1ZA,H1ZB,H1ZC), C22(H22A,H22B,H22C), C1H(H1HA,H1HB,H1HC)
6.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C36(H36), C38(H38), C39(H39), C41(H41), C43(H43), C46(H46),
 C58(H58), C59(H59), C61(H61), C65(H65), C68(H68), C70(H70), C71(H71), C72(H72),
  C73(H73), C78(H78), C80(H80), C84(H84), C86(H86), C87(H87), C88(H88),
 C89(H89), C90(H90), C92(H92), C97(H97), C100(H100), C108(H108), C111(H111),
 C113(H113), C116(H116), C117(H117), C120(H120), C121(H121), C123(H123),
 C124(H124), C126(H126), C133(H133), C136(H136), C138(H138), C140(H140),
 C141(H141), C142(H142), C143(H143), C147(H147), C148(H148), C151(H151),
 C152(H152), C153(H153), C154(H154), C155(H155), C157(H157), C160(H160),
 C162(H162), C163(H163), C164(H164), C165(H165), C166(H166), C167(H167),
 C169(H169), C170(H170), C171(H171), C172(H172), C173(H173), C174(H174),
 C175(H175), C177(H177), C178(H178), C179(H179), C181(H181), C184(H184),
 C188(H188), C189(H189), C190(H190), C192(H192), C194(H194), C195(H195),
 C197(H197), C198(H198), C199(H199), C201(H201), C202(H202), C203(H203),
 C204(H204), C205(H205), C206(H206), C207(H207), C209(H209), C213(H213),
 C219(H219), C227(H227), C228(H228), C229(H229), C231(H231), C232(H232),
 C238(H238), C252(H252), C259(H259), C276(H276), C26(H26), C2(H2), C3(H3),
 C4(H4), C6(H6), C34(H34), C7(H7), C8(H8), C23(H23)
;