# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ubipda_a_sq
_database_code_depnum_ccdc_archive 'CCDC 1422592'
_audit_update_record             
;
2015-09-04 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H20 O14 U2'
_chemical_formula_weight         888.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O 0.0132 0.0074
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
U U -7.3185 4.5872
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c :H'
_space_group_name_Hall           'R 3 -2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   38.410(7)
_cell_length_b                   38.410(7)
_cell_length_c                   8.7096(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11128(4)
_cell_formula_units_Z            18
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6135
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      30.03

_exptl_crystal_description       Block
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.386
_exptl_crystal_F_000             7200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    7.048
_shelx_estimated_absorpt_T_min   0.677
_shelx_estimated_absorpt_T_max   0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.509
_exptl_absorpt_correction_T_max  0.816
_exptl_absorpt_process_details   'SADABS 2014/2 Bruker AXS Madison WI USA'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22040
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.060
_diffrn_reflns_theta_max         30.280
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5634
_reflns_number_gt                4488
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.993
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v8.34A'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_structure_solution    'Bruker SHELXT 2014/3 (beta test)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'

_refine_special_details          
;
 Refined as a 2-component inversion twin.  All non-hydrogen atoms
 were refined anisotropically. Hydrogen atoms on carbon atoms
 were placed geometrically constrained and were refined
 using a riding model. The mu-3 hydroxides hydrogen atoms
 could not be found and were therefore omitted from the
 refinement but not the formula. The structure has a solvent
 channel running through it, water molecules in this channel
 did not appear readily in this channel, thus the residual
 density was treated with the program SQUEEZE [Reference to
 van der Sluis, P. & Spek, A. L., Acta Cryst. 1990, A46, 194-201]
 as implemented in Platon [Reference to Spek, A. L., Acta Cryst.
 2009, D65, 148-155] which allows for the mathematical compensation
 of the electron  contribution of disordered solvent contained in
 the voids to the calculated  diffraction intensities.. According
 to PLATON 672 electron were recovered from a volume of 3808 Ang3.
 This equates to approximately 67 water molecules per cell. This
 was approimated to 4 water per asymmetric unit and this number
 of water molecules were added to the formula.
;
_vrf_CHEMW03_ubipda_a_sq         
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: Formula includes water molecules the number of water
 molecules calculated from the number of electrons determined by
 SQUEEZE in PLATON.
;
_vrf_PLAT342_ubipda_a_sq         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0234 Ang.  
RESPONSE: It wa difficult to get a good crystal with a nice spot shape,
 so data was collected on the best crystal available. The spots were 
 extended as bit in one direction, this could have cause a problem
 getting a pefect integration. However, the low C-C bond precision do not
 change the result of the structure determination.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0133P)²+49.7444P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Intrinsic phasing'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5634
_refine_ls_number_parameters     236
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0739
_refine_ls_wR_factor_gt          0.0689
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.45774(2) 0.55042(2) 0.81604(5) 0.05689(16) Uani 1 1 d . . . . .
O1 O 0.4078(3) 0.5118(3) 0.8531(10) 0.067(3) Uani 1 1 d . . . . .
O2 O 0.5057(4) 0.5870(4) 0.7821(14) 0.097(4) Uani 1 1 d . . . . .
U2 U 0.50573(2) 0.50319(2) 0.57103(6) 0.0686(2) Uani 1 1 d . . . . .
O3 O 0.4674(4) 0.4527(4) 0.5342(11) 0.086(4) Uani 1 1 d . . . . .
O4 O 0.5454(4) 0.5535(3) 0.6106(12) 0.079(3) Uani 1 1 d . . . . .
O5 O 0.4543(4) 0.5215(4) 0.5646(11) 0.089(4) Uani 1 1 d . . . . .
O6 O 0.4751(5) 0.4975(5) 0.8195(11) 0.108(5) Uani 1 1 d . . . . .
O7 O 0.4558(3) 0.6041(3) 0.9536(10) 0.062(2) Uani 1 1 d . . . . .
O8 O 0.4204(3) 0.5701(3) 1.1569(10) 0.056(2) Uani 1 1 d . . . . .
C1 C 0.4347(3) 0.6009(4) 1.0706(13) 0.043(3) Uani 1 1 d . . . . .
C2 C 0.4269(4) 0.6343(4) 1.1074(12) 0.044(3) Uani 1 1 d . . . . .
C3 C 0.4447(4) 0.6690(4) 1.0265(13) 0.049(3) Uani 1 1 d . . . . .
H3A H 0.4622 0.6725 0.9437 0.059 Uiso 1 1 calc R U . . .
C4 C 0.4368(5) 0.6993(5) 1.0660(17) 0.069(4) Uani 1 1 d . . . . .
H4A H 0.4496 0.7240 1.0108 0.083 Uiso 1 1 calc R U . . .
C5 C 0.4115(5) 0.6944(5) 1.181(2) 0.073(5) Uani 1 1 d . . . . .
H5A H 0.4064 0.7156 1.2055 0.087 Uiso 1 1 calc R U . . .
C6 C 0.3926(4) 0.6590(5) 1.2664(16) 0.061(4) Uani 1 1 d . . . . .
H6A H 0.3748 0.6556 1.3483 0.073 Uiso 1 1 calc R U . . .
C7 C 0.4007(4) 0.6292(4) 1.2268(13) 0.047(3) Uani 1 1 d . . . . .
H7A H 0.3882 0.6046 1.2821 0.057 Uiso 1 1 calc R U . . .
O9 O 0.5589(4) 0.4995(4) 0.4300(11) 0.080(3) Uani 1 1 d . . . . .
O10 O 0.5246(3) 0.4648(4) 0.2298(12) 0.078(3) Uani 1 1 d . . . . .
C8 C 0.5553(5) 0.4810(5) 0.3075(15) 0.060(4) Uani 1 1 d . . . . .
C9 C 0.5928(4) 0.4798(5) 0.2593(15) 0.062(4) Uani 1 1 d . . . . .
C10 C 0.6246(5) 0.4906(5) 0.3537(15) 0.070(4) Uani 1 1 d . . . . .
H10A H 0.6232 0.4983 0.4563 0.084 Uiso 1 1 calc R U . . .
C11 C 0.6596(5) 0.4909(4) 0.3044(17) 0.069(4) Uani 1 1 d . . . . .
H11A H 0.6814 0.4981 0.3728 0.083 Uiso 1 1 calc R U . . .
C12 C 0.6614(5) 0.4807(5) 0.1571(16) 0.072(4) Uani 1 1 d . . . . .
H12A H 0.6855 0.4825 0.1201 0.086 Uiso 1 1 calc R U . . .
C13 C 0.6282(5) 0.4676(5) 0.0578(18) 0.078(5) Uani 1 1 d . . . . .
H13A H 0.6291 0.4589 -0.0436 0.093 Uiso 1 1 calc R U . . .
C14 C 0.5944(5) 0.4675(5) 0.1117(16) 0.071(4) Uani 1 1 d . . . . .
H14A H 0.5718 0.4590 0.0460 0.086 Uiso 1 1 calc R U . . .


_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 O2 1.694(14) . ?
U1 O1 1.771(11) . ?
U1 O5 2.345(10) 4_665 ?
U1 O8 2.351(8) 4_664 ?
U1 O7 2.417(8) . ?
U1 O5 2.428(10) . ?
U1 O6 2.435(11) . ?
U1 U2 3.8190(8) . ?
U1 U2 3.8822(8) 4_665 ?
U2 O3 1.782(13) . ?
U2 O4 1.797(11) . ?
U2 O10 2.356(10) 4_665 ?
U2 O6 2.370(10) 4_664 ?
U2 O5 2.408(10) . ?
U2 O6 2.421(10) . ?
U2 O9 2.449(9) . ?
U2 U1 3.8821(8) 4_664 ?
O5 U1 2.345(10) 4_664 ?
O6 U2 2.370(10) 4_665 ?
O7 C1 1.270(13) . ?
O8 C1 1.270(15) . ?
O8 U1 2.351(8) 4_665 ?
C1 C2 1.491(17) . ?
C2 C3 1.354(17) . ?
C2 C7 1.391(16) . ?
C3 C4 1.383(18) . ?
C4 C5 1.35(2) . ?
C5 C6 1.39(2) . ?
C6 C7 1.373(17) . ?
O9 C8 1.251(16) . ?
O10 C8 1.225(18) . ?
O10 U2 2.356(10) 4_664 ?
C8 C9 1.523(18) . ?
C9 C10 1.35(2) . ?
C9 C14 1.380(18) . ?
C10 C11 1.403(19) . ?
C11 C12 1.354(18) . ?
C12 C13 1.41(2) . ?
C13 C14 1.383(19) . ?

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
O2 U1 O1 179.2(6) . . ?
O2 U1 O5 87.4(5) . 4_665 ?
O1 U1 O5 92.0(5) . 4_665 ?
O2 U1 O8 93.8(5) . 4_664 ?
O1 U1 O8 87.0(4) . 4_664 ?
O5 U1 O8 146.5(3) 4_665 4_664 ?
O2 U1 O7 82.1(4) . . ?
O1 U1 O7 98.2(4) . . ?
O5 U1 O7 76.4(3) 4_665 . ?
O8 U1 O7 70.7(3) 4_664 . ?
O2 U1 O5 90.6(5) . . ?
O1 U1 O5 89.5(4) . . ?
O5 U1 O5 137.8(4) 4_665 . ?
O8 U1 O5 75.7(3) 4_664 . ?
O7 U1 O5 145.0(3) . . ?
O2 U1 O6 93.3(5) . . ?
O1 U1 O6 86.0(5) . . ?
O5 U1 O6 71.3(3) 4_665 . ?
O8 U1 O6 141.8(3) 4_664 . ?
O7 U1 O6 147.5(3) . . ?
O5 U1 O6 66.7(3) . . ?
O2 U1 U2 73.4(3) . . ?
O1 U1 U2 106.3(3) . . ?
O5 U1 U2 102.5(2) 4_665 . ?
O8 U1 U2 109.9(2) 4_664 . ?
O7 U1 U2 155.5(2) . . ?
O5 U1 U2 37.7(2) . . ?
O6 U1 U2 38.0(3) . . ?
O2 U1 U2 89.9(4) . 4_665 ?
O1 U1 U2 89.3(3) . 4_665 ?
O5 U1 U2 35.8(3) 4_665 4_665 ?
O8 U1 U2 175.7(2) 4_664 4_665 ?
O7 U1 U2 112.0(2) . 4_665 ?
O5 U1 U2 102.1(2) . 4_665 ?
O6 U1 U2 35.5(2) . 4_665 ?
U2 U1 U2 69.107(16) . 4_665 ?
O3 U2 O4 178.1(5) . . ?
O3 U2 O10 86.2(4) . 4_665 ?
O4 U2 O10 91.9(5) . 4_665 ?
O3 U2 O6 93.3(5) . 4_664 ?
O4 U2 O6 87.9(5) . 4_664 ?
O10 U2 O6 145.5(4) 4_665 4_664 ?
O3 U2 O5 87.8(4) . . ?
O4 U2 O5 93.9(5) . . ?
O10 U2 O5 142.9(4) 4_665 . ?
O6 U2 O5 71.4(3) 4_664 . ?
O3 U2 O6 87.9(5) . . ?
O4 U2 O6 92.2(5) . . ?
O10 U2 O6 75.9(4) 4_665 . ?
O6 U2 O6 138.5(5) 4_664 . ?
O5 U2 O6 67.3(3) . . ?
O3 U2 O9 96.0(4) . . ?
O4 U2 O9 82.8(4) . . ?
O10 U2 O9 70.3(3) 4_665 . ?
O6 U2 O9 75.5(4) 4_664 . ?
O5 U2 O9 146.8(3) . . ?
O6 U2 O9 145.7(3) . . ?
O3 U2 U1 106.6(3) . . ?
O4 U2 U1 74.5(3) . . ?
O10 U2 U1 110.1(3) 4_665 . ?
O6 U2 U1 103.1(2) 4_664 . ?
O5 U2 U1 38.0(2) . . ?
O6 U2 U1 38.3(3) . . ?
O9 U2 U1 157.4(3) . . ?
O3 U2 U1 90.1(3) . 4_664 ?
O4 U2 U1 91.7(4) . 4_664 ?
O10 U2 U1 175.8(3) 4_665 4_664 ?
O6 U2 U1 36.7(3) 4_664 4_664 ?
O5 U2 U1 34.7(2) . 4_664 ?
O6 U2 U1 101.9(2) . 4_664 ?
O9 U2 U1 112.1(2) . 4_664 ?
U1 U2 U1 69.069(16) . 4_664 ?
U1 O5 U2 109.5(4) 4_664 . ?
U1 O5 U1 132.3(4) 4_664 . ?
U2 O5 U1 104.3(4) . . ?
U2 O6 U2 131.5(5) 4_665 . ?
U2 O6 U1 107.8(4) 4_665 . ?
U2 O6 U1 103.7(4) . . ?
C1 O7 U1 127.2(8) . . ?
C1 O8 U1 133.5(8) . 4_665 ?
O7 C1 O8 121.6(11) . . ?
O7 C1 C2 118.8(11) . . ?
O8 C1 C2 119.5(10) . . ?
C3 C2 C7 120.0(12) . . ?
C3 C2 C1 121.2(11) . . ?
C7 C2 C1 118.8(11) . . ?
C2 C3 C4 119.1(13) . . ?
C5 C4 C3 121.0(15) . . ?
C4 C5 C6 121.4(13) . . ?
C7 C6 C5 117.1(13) . . ?
C6 C7 C2 121.4(13) . . ?
C8 O9 U2 127.0(10) . . ?
C8 O10 U2 129.2(10) . 4_664 ?
O10 C8 O9 124.5(13) . . ?
O10 C8 C9 121.1(13) . . ?
O9 C8 C9 114.5(14) . . ?
C10 C9 C14 119.0(12) . . ?
C10 C9 C8 123.0(13) . . ?
C14 C9 C8 118.0(13) . . ?
C9 C10 C11 121.9(13) . . ?
C12 C11 C10 118.4(15) . . ?
C11 C12 C13 121.2(14) . . ?
C14 C13 C12 118.3(13) . . ?
C9 C14 C13 121.1(13) . . ?

_refine_diff_density_max         0.928
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.107

_shelxl_version_number           2014-3



