# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2002

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

loop_
_publ_author_name
'Michael Doran'
'Alexander J. Norquist'
D.O'Hare

_publ_contact_author_name        "Prof Dermot O'Hare"
_publ_contact_author_address     
;
Inorganic Chemistry Laboratory
University of Oxford
South Parks Rd
Oxford
OX1 3QR
UNITED KINGDOM
;

_publ_contact_author_email       DERMOT.OHARE@CHEM.OX.AC.UK

_publ_section_title              
;
[NC4H12]2[(UO2)6(H2O) 2(SO4)7]: the first
organically templated actinide sulfate with a three dimensional
framework structure
;

data_ajn86
_database_code_CSD               195915

_audit_creation_date             2002-08-12T17:12:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C8 H28 N2 O42 S7 U6'
_chemical_formula_structural     'C8 H28 N2 O42 S7 U6'
_chemical_formula_sum            'C8 H28 N2 O42 S7 U6'
_chemical_formula_weight         2476.89
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_Int_Tables_number      20
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, -z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   10.3466(2)
_cell_length_b                   18.5415(3)
_cell_length_c                   22.7001(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4354.82(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    3.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4344
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    22.691
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_absorpt_correction_T_min  0.0194
_exptl_absorpt_correction_T_max  0.0386
_exptl_absorpt_correction_t_ave  0.031

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_number            4863
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         5.16
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_reflns_number_total             4863
_reflns_number_gt                4519
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0450P)²+23.1466P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.00034(2)
_refine_ls_number_reflns         4863
_refine_ls_number_parameters     299
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0783
_refine_ls_wR_factor_gt          0.076
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(9)
_refine_diff_density_max         1.982
_refine_diff_density_min         -1.375
_refine_diff_density_rms         0.282

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.95670(4) 0.74398(2) 0.524522(15) 0.01800(11) Uani 1 1 d . . .
U2 U 0.23963(4) 0.74546(2) 0.746163(15) 0.01780(11) Uani 1 1 d . . .
U3 U 0.61635(4) 0.97027(2) 0.616374(15) 0.01745(11) Uani 1 1 d . . .
S1 S 0.4896(2) 1.14857(13) 0.66300(10) 0.0160(5) Uani 1 1 d . . .
S2 S 0.7405(2) 0.88579(13) 0.47936(11) 0.0170(5) Uani 1 1 d . . .
S3 S 0.6509(2) 0.77115(14) 0.60483(10) 0.0170(5) Uani 1 1 d . . .
S4 S 0.5 0.88699(19) 0.75 0.0176(7) Uani 1 2 d S . .
O1 O 0.8568(8) 0.6862(4) 0.4835(3) 0.0241(17) Uani 1 1 d . . .
O2 O 1.0564(8) 0.8017(4) 0.5662(3) 0.0193(15) Uani 1 1 d . . .
O3 O 0.4373(7) 1.1602(4) 0.6032(3) 0.0213(16) Uani 1 1 d . . .
O4 O 0.6337(9) 0.8332(5) 0.4800(4) 0.035(2) Uani 1 1 d . . .
O5 O 0.5787(8) 0.7267(4) 0.5630(3) 0.0247(18) Uani 1 1 d . . .
O6 O 0.8656(8) 0.8492(5) 0.4770(4) 0.0292(19) Uani 1 1 d . . .
O7 O 0.7829(7) 0.7848(4) 0.5846(3) 0.0231(17) Uani 1 1 d . . .
O8 O 0.6484(8) 0.6801(4) 0.7776(3) 0.0241(17) Uani 1 1 d . . .
O9 O 0.1283(8) 0.8091(4) 0.7724(3) 0.0217(16) Uani 1 1 d . . .
O10 O 0.3854(9) 0.8430(5) 0.7533(3) 0.034(2) Uani 1 1 d . . .
O11 O 0.2725(9) 0.8054(5) 0.6467(3) 0.034(2) Uani 1 1 d . . .
O12 O 0.5871(7) 1.2039(4) 0.6749(3) 0.0207(16) Uani 1 1 d . . .
O13 O 0.3803(8) 1.1543(4) 0.7046(3) 0.0208(16) Uani 1 1 d . . .
O14 O 0.6559(7) 0.7314(4) 0.6611(3) 0.0191(16) Uani 1 1 d . . .
O15 O 0.7527(8) 0.9613(5) 0.6618(3) 0.0259(17) Uani 1 1 d . . .
O16 O 0.4789(7) 0.9791(4) 0.5722(3) 0.0236(17) Uani 1 1 d . . .
O17 O 0.7372(9) 0.9297(4) 0.5332(3) 0.0275(18) Uani 1 1 d . . .
O18 O 0.7327(8) 1.0683(5) 0.5733(4) 0.0262(18) Uani 1 1 d . . .
O19 O 0.5482(8) 1.0761(4) 0.6681(3) 0.0245(17) Uani 1 1 d . . .
O20 O 0.4881(7) 0.9320(4) 0.6971(3) 0.0215(16) Uani 1 1 d . . .
O21 O 0.5840(7) 0.8401(4) 0.6130(3) 0.0216(16) Uani 1 1 d . . .
C1 C 0.0084(13) 0.0687(8) 0.6596(6) 0.037(3) Uani 1 1 d . . .
H1A H -0.0399 0.0931 0.6282 0.056 Uiso 1 1 calc R . .
H1B H 0.0536 0.1047 0.6836 0.056 Uiso 1 1 calc R . .
H1C H -0.0517 0.0415 0.6845 0.056 Uiso 1 1 calc R . .
N1 N 0.1023(10) 0.0194(6) 0.6335(5) 0.039(3) Uani 1 1 d . . .
C3 C 0.1985(17) -0.0080(11) 0.6767(10) 0.074(6) Uani 1 1 d . . .
H3A H 0.1536 -0.0332 0.7087 0.111 Uiso 1 1 calc R . .
H3B H 0.2477 0.0325 0.693 0.111 Uiso 1 1 calc R . .
H3C H 0.2577 -0.0415 0.657 0.111 Uiso 1 1 calc R . .
C4 C 0.0380(17) -0.0374(10) 0.6010(12) 0.088(8) Uani 1 1 d . . .
H4A H -0.0153 -0.0659 0.6281 0.132 Uiso 1 1 calc R . .
H4B H 0.1027 -0.0686 0.5825 0.132 Uiso 1 1 calc R . .
H4C H -0.0171 -0.016 0.5706 0.132 Uiso 1 1 calc R . .
C2 C 0.1789(19) 0.0616(10) 0.5889(10) 0.068(6) Uani 1 1 d . . .
H2A H 0.2355 0.0288 0.5669 0.103 Uiso 1 1 calc R . .
H2B H 0.2315 0.098 0.6091 0.103 Uiso 1 1 calc R . .
H2C H 0.1196 0.0856 0.5615 0.103 Uiso 1 1 calc R . .


#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.757(8) . ?
U1 O2 1.761(7) . ?
U1 O3 2.377(7) 5_545 ?
U1 O4 2.327(9) 7_566 ?
U1 O5 2.416(7) 7_566 ?
U1 O6 2.420(8) . ?
U1 O7 2.380(7) . ?
U2 O8 1.761(8) 4_656 ?
U2 O9 1.753(8) . ?
U2 O10 2.360(9) . ?
U2 O11 2.540(8) . ?
U2 O12 2.387(7) 5_445 ?
U2 O13 2.376(8) 8_546 ?
U2 O14 2.381(7) 4_656 ?
U3 O15 1.755(8) . ?
U3 O16 1.748(7) . ?
U3 O17 2.386(8) . ?
U3 O18 2.389(8) . ?
U3 O19 2.394(8) . ?
U3 O20 2.372(7) . ?
U3 O21 2.438(7) . ?
S1 O3 1.476(7) . ?
S1 O12 1.464(8) . ?
S1 O13 1.477(8) . ?
S1 O19 1.478(8) . ?
S2 O4 1.474(9) . ?
S2 O6 1.462(8) . ?
S2 O17 1.469(8) . ?
S2 O18 1.471(8) 3_576 ?
S3 O5 1.463(8) . ?
S3 O7 1.464(8) . ?
S3 O14 1.475(7) . ?
S3 O21 1.466(8) . ?
S4 O10 1.442(9) 4_656 ?
S4 O20 1.467(7) . ?
N1 C1 1.460(17) . ?
N1 C2 1.51(2) . ?
N1 C3 1.486(19) . ?
N1 C4 1.447(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 179.6(4) . . ?
O1 U1 O4 93.7(4) . 7_566 ?
O2 U1 O4 86.4(4) . 7_566 ?
O1 U1 O3 87.1(3) . 5_545 ?
O2 U1 O3 92.5(3) . 5_545 ?
O4 U1 O3 72.4(3) 7_566 5_545 ?
O1 U1 O7 93.1(3) . . ?
O2 U1 O7 86.7(3) . . ?
O4 U1 O7 144.7(3) 7_566 . ?
O3 U1 O7 73.4(3) 5_545 . ?
O1 U1 O5 90.5(3) . 7_566 ?
O2 U1 O5 89.9(3) . 7_566 ?
O4 U1 O5 72.0(3) 7_566 7_566 ?
O3 U1 O5 144.1(3) 5_545 7_566 ?
O7 U1 O5 142.6(3) . 7_566 ?
O1 U1 O6 91.5(3) . . ?
O2 U1 O6 88.7(3) . . ?
O4 U1 O6 141.5(3) 7_566 . ?
O3 U1 O6 146.0(3) 5_545 . ?
O7 U1 O6 72.8(3) . . ?
O5 U1 O6 69.8(3) 7_566 . ?
O9 U2 O8 177.9(3) . 4_656 ?
O9 U2 O10 83.1(4) . . ?
O8 U2 O10 97.4(4) 4_656 . ?
O9 U2 O13 88.6(3) . 8_546 ?
O8 U2 O13 89.9(3) 4_656 8_546 ?
O10 U2 O13 147.8(3) . 8_546 ?
O9 U2 O14 94.1(3) . 4_656 ?
O8 U2 O14 84.1(3) 4_656 4_656 ?
O10 U2 O14 74.5(3) . 4_656 ?
O13 U2 O14 75.1(2) 8_546 4_656 ?
O9 U2 O12 90.8(3) . 5_445 ?
O8 U2 O12 90.3(3) 4_656 5_445 ?
O10 U2 O12 135.8(3) . 5_445 ?
O13 U2 O12 75.1(2) 8_546 5_445 ?
O14 U2 O12 149.7(2) 4_656 5_445 ?
O9 U2 O11 95.5(3) . . ?
O8 U2 O11 86.6(3) 4_656 . ?
O10 U2 O11 68.9(3) . . ?
O13 U2 O11 143.1(3) 8_546 . ?
O14 U2 O11 140.7(3) 4_656 . ?
O12 U2 O11 68.1(3) 5_445 . ?
O16 U3 O15 179.1(3) . . ?
O16 U3 O20 90.9(3) . . ?
O15 U3 O20 88.2(3) . . ?
O16 U3 O17 90.1(3) . . ?
O15 U3 O17 90.8(3) . . ?
O20 U3 O17 144.1(3) . . ?
O16 U3 O18 96.0(3) . . ?
O15 U3 O18 84.7(3) . . ?
O20 U3 O18 145.7(3) . . ?
O17 U3 O18 69.7(3) . . ?
O16 U3 O19 88.0(3) . . ?
O15 U3 O19 91.5(3) . . ?
O20 U3 O19 72.6(3) . . ?
O17 U3 O19 143.2(3) . . ?
O18 U3 O19 74.0(3) . . ?
O16 U3 O21 87.9(3) . . ?
O15 U3 O21 92.0(3) . . ?
O20 U3 O21 69.6(3) . . ?
O17 U3 O21 74.6(3) . . ?
O18 U3 O21 144.1(3) . . ?
O19 U3 O21 141.9(3) . . ?
O12 S1 O3 108.7(4) . . ?
O12 S1 O13 111.0(4) . . ?
O3 S1 O13 107.2(5) . . ?
O12 S1 O19 109.8(5) . . ?
O3 S1 O19 110.8(5) . . ?
O13 S1 O19 109.3(4) . . ?
O6 S2 O17 108.0(5) . . ?
O6 S2 O18 106.7(5) . 3_576 ?
O17 S2 O18 110.8(5) . 3_576 ?
O6 S2 O4 110.9(6) . . ?
O17 S2 O4 109.9(5) . . ?
O18 S2 O4 110.5(5) 3_576 . ?
O5 S3 O7 111.7(5) . . ?
O5 S3 O21 109.4(5) . . ?
O7 S3 O21 109.2(5) . . ?
O5 S3 O14 107.4(4) . . ?
O7 S3 O14 109.0(4) . . ?
O21 S3 O14 110.0(4) . . ?
O10 S4 O10 111.0(8) 4_656 . ?
O10 S4 O20 107.2(5) 4_656 4_656 ?
O10 S4 O20 110.4(5) . 4_656 ?
O10 S4 O20 110.4(5) 4_656 . ?
O10 S4 O20 107.2(4) . . ?
O20 S4 O20 110.7(6) 4_656 . ?
S2 O17 U3 147.7(5) . . ?
S2 O6 U1 134.6(5) . . ?
S4 O10 U2 162.9(6) . . ?
S1 O19 U3 145.9(5) . . ?
S2 O18 U3 143.2(5) 3_576 . ?
S2 O4 U1 175.4(5) . 7_466 ?
S1 O3 U1 139.0(5) . 5_455 ?
S1 O13 U2 138.8(5) . 8_556 ?
S4 O20 U3 139.1(5) . . ?
S3 O14 U2 136.6(4) . 4_656 ?
S1 O12 U2 143.8(4) . 5 ?
S3 O21 U3 143.4(5) . . ?
S3 O5 U1 132.3(5) . 7_466 ?
S3 O7 U1 146.1(5) . . ?
C4 N1 C1 110.8(11) . . ?
C4 N1 C3 113.3(16) . . ?
C1 N1 C3 113.1(13) . . ?
C4 N1 C2 106.1(16) . . ?
C1 N1 C2 107.3(13) . . ?
C3 N1 C2 105.6(13) . . ?



