# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004

data_global

_publ_contact_author_email       BERTHET@DRECAM.CEA.FR

_publ_contact_author_name        'Dr Jean Claude Berthet'
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_publ_contact_author_address     
;
DSM/DRECAM/Service de Chimie Moleculaire
Commissariat a l'Energie Atomique
Bat 125, piece 25
Gif sur Yvette
Essonnes
91191 cedex
FRANCE
;

_publ_section_title              
;
Synthesis of the stable UO2I2, the last of the
uranyl dihalides.  X-ray crystal structure of [UO2I2(py)3]
;
loop_
_publ_author_name
J.C.Berthet
'Michel Ephritikhine'
'Martine Nierlich'

data_struc
_database_code_depnum_ccdc_archive 'CCDC 226281'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H15 I2 N3 O2 U'
_chemical_formula_weight         761.13

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 0.0000 0.0000 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   14.968(3)
_cell_length_b                   15.662(3)
_cell_length_c                   17.193(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4030.5(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    25092
_cell_measurement_theta_min      2
_cell_measurement_theta_max      25

_exptl_crystal_description       irregular
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2720
_exptl_absorpt_coefficient_mu    11.128
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_T_max  0.598
_exptl_absorpt_process_details   'MULABS in PLATON;Spek,1998'

_exptl_special_details           
;
Unit cell dimensions were determined from more than a thousand
reflections in all the angular range, taken from ten frames
with \f steps of 2\%.A 180\% range in \f was scanned during
data collection  with 2\%\f steps and 10s exposure by frame.The
crystal to detector distance was 30mm.

;
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\f rotation scans with 2\%steps'
_diffrn_standards_number         none
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25092
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         24.69
_reflns_number_total             3364
_reflns_number_gt                2616
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'DENZO(Otwinowski& Minor,1997)'
_computing_cell_refinement       'DENZO(Otwinowski& Minor,1997)'
_computing_data_reduction        'DENZO(Otwinowski& Minor,1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXTL (Sheldrick,1997)'
_computing_publication_material  'SHELXTL (Sheldrick,1997)'

_refine_special_details          
;
Structure solved by direct method and refined by full matrix
least-squares on F^2^ with anisotropic thermal parameters for all
non hydrogen atoms.Hydrogen atoms  were
introduced at calculated positions as riding atoms, with an
isotropic displacement parameter equal to 1.2 (CH)
times that of the parent atom.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+43.5326P] where P=(Fo^2^+2Fc^2^)/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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3364
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0764
_refine_ls_wR_factor_gt          0.0676
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_restrained_S_all      0.884
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.002
_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        24.69
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.150

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
U U 0.12013(2) 0.39314(2) 0.599930(17) 0.02819(11) Uani 1 1 d . . .
I1 I -0.03102(5) 0.32217(5) 0.70577(4) 0.0561(2) Uani 1 1 d . . .
I2 I 0.27445(4) 0.52694(4) 0.58810(3) 0.03836(16) Uani 1 1 d . . .
O1 O 0.0469(4) 0.4744(4) 0.5700(3) 0.0322(14) Uani 1 1 d . . .
O2 O 0.1933(4) 0.3107(4) 0.6266(3) 0.0387(15) Uani 1 1 d . . .
N1 N 0.1738(5) 0.3777(5) 0.4590(4) 0.0315(17) Uani 1 1 d . . .
N2 N 0.0277(5) 0.2893(5) 0.5190(4) 0.0322(17) Uani 1 1 d . . .
N3 N 0.1332(5) 0.4634(5) 0.7311(4) 0.0279(16) Uani 1 1 d . . .
C1 C 0.2241(6) 0.3115(7) 0.4386(6) 0.041(2) Uani 1 1 d . . .
H1B H 0.2483 0.2769 0.4772 0.050 Uiso 1 1 calc R . .
C2 C 0.2416(7) 0.2926(7) 0.3610(6) 0.050(3) Uani 1 1 d . . .
H2B H 0.2782 0.2467 0.3485 0.060 Uiso 1 1 calc R . .
C3 C 0.2055(7) 0.3410(7) 0.3031(6) 0.051(3) Uani 1 1 d . . .
H3A H 0.2143 0.3270 0.2511 0.062 Uiso 1 1 calc R . .
C4 C 0.1557(7) 0.4112(8) 0.3238(5) 0.051(3) Uani 1 1 d . . .
H4A H 0.1322 0.4467 0.2856 0.061 Uiso 1 1 calc R . .
C5 C 0.1407(6) 0.4289(7) 0.4012(5) 0.039(2) Uani 1 1 d . . .
H5A H 0.1072 0.4767 0.4146 0.047 Uiso 1 1 calc R . .
C6 C 0.0459(7) 0.2047(6) 0.5174(5) 0.040(2) Uani 1 1 d . . .
H6A H 0.0925 0.1837 0.5476 0.048 Uiso 1 1 calc R . .
C7 C -0.0032(7) 0.1480(6) 0.4715(6) 0.047(3) Uani 1 1 d . . .
H7A H 0.0093 0.0899 0.4722 0.057 Uiso 1 1 calc R . .
C8 C -0.0698(8) 0.1796(7) 0.4256(6) 0.053(3) Uani 1 1 d . . .
H8A H -0.1012 0.1432 0.3928 0.064 Uiso 1 1 calc R . .
C9 C -0.0908(7) 0.2653(6) 0.4277(5) 0.043(2) Uani 1 1 d . . .
H9A H -0.1375 0.2872 0.3981 0.052 Uiso 1 1 calc R . .
C10 C -0.0403(6) 0.3177(6) 0.4752(5) 0.038(2) Uani 1 1 d . . .
H10A H -0.0542 0.3756 0.4769 0.046 Uiso 1 1 calc R . .
C11 C 0.0856(6) 0.5337(6) 0.7500(5) 0.035(2) Uani 1 1 d . . .
H11A H 0.0542 0.5616 0.7108 0.042 Uiso 1 1 calc R . .
C12 C 0.0812(6) 0.5661(6) 0.8244(5) 0.038(2) Uani 1 1 d . . .
H12A H 0.0482 0.6150 0.8353 0.046 Uiso 1 1 calc R . .
C13 C 0.1270(6) 0.5240(6) 0.8820(5) 0.038(2) Uani 1 1 d . . .
H13A H 0.1239 0.5435 0.9331 0.046 Uiso 1 1 calc R . .
C14 C 0.1766(6) 0.4542(6) 0.8650(5) 0.040(2) Uani 1 1 d . . .
H14A H 0.2087 0.4261 0.9036 0.048 Uiso 1 1 calc R . .
C15 C 0.1788(6) 0.4253(6) 0.7891(5) 0.037(2) Uani 1 1 d . . .
H15A H 0.2133 0.3776 0.7775 0.045 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U 0.03412(18) 0.02561(17) 0.02484(17) -0.00191(14) -0.00168(14) 0.00330(15)
I1 0.0693(5) 0.0624(5) 0.0365(3) -0.0101(3) 0.0143(3) -0.0326(4)
I2 0.0426(4) 0.0401(4) 0.0325(3) -0.0053(3) 0.0053(3) -0.0080(3)
O1 0.033(4) 0.035(4) 0.028(3) -0.002(3) -0.003(2) 0.003(3)
O2 0.048(4) 0.032(4) 0.036(3) 0.001(3) -0.005(3) 0.005(3)
N1 0.029(4) 0.033(4) 0.033(4) -0.012(3) 0.003(3) 0.002(3)
N2 0.036(4) 0.032(4) 0.028(4) -0.001(3) -0.001(3) 0.003(4)
N3 0.029(4) 0.029(4) 0.026(4) -0.003(3) 0.002(3) -0.010(3)
C1 0.027(5) 0.046(6) 0.051(6) -0.015(5) 0.006(4) -0.013(5)
C2 0.050(7) 0.032(6) 0.067(7) -0.023(5) 0.019(6) -0.015(5)
C3 0.047(7) 0.069(8) 0.039(6) -0.024(6) 0.011(5) -0.015(6)
C4 0.032(5) 0.089(9) 0.032(5) 0.005(5) 0.001(4) -0.008(6)
C5 0.031(5) 0.051(6) 0.035(5) 0.002(5) -0.003(4) 0.002(4)
C6 0.045(6) 0.032(6) 0.044(6) -0.004(4) 0.013(4) -0.002(5)
C7 0.058(7) 0.030(5) 0.054(6) -0.007(5) 0.035(5) -0.009(5)
C8 0.067(8) 0.055(7) 0.039(6) -0.009(5) 0.006(5) -0.024(6)
C9 0.054(6) 0.039(6) 0.036(5) 0.009(4) -0.006(4) -0.013(5)
C10 0.051(6) 0.030(5) 0.034(5) 0.002(4) 0.001(4) -0.005(5)
C11 0.037(5) 0.034(5) 0.034(5) 0.002(4) -0.002(4) 0.003(5)
C12 0.041(6) 0.042(6) 0.032(5) -0.010(4) 0.011(4) 0.000(5)
C13 0.042(6) 0.043(6) 0.030(5) -0.007(4) 0.004(4) -0.013(5)
C14 0.046(6) 0.047(6) 0.027(5) 0.003(4) -0.005(4) -0.005(5)
C15 0.044(6) 0.034(5) 0.034(5) 0.002(4) -0.007(4) -0.004(4)

_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
U O1 1.757(6) . ?
U O2 1.754(6) . ?
U N3 2.517(6) . ?
U N2 2.548(7) . ?
U N1 2.564(7) . ?
U I1 3.1089(8) . ?
U I2 3.1254(8) . ?
N1 C1 1.329(12) . ?
N1 C5 1.370(11) . ?
N2 C10 1.342(11) . ?
N2 C6 1.353(11) . ?
N3 C15 1.348(11) . ?
N3 C11 1.351(11) . ?
C1 C2 1.392(14) . ?
C2 C3 1.364(15) . ?
C3 C4 1.374(15) . ?
C4 C5 1.378(13) . ?
C6 C7 1.396(14) . ?
C7 C8 1.365(15) . ?
C8 C9 1.378(15) . ?
C9 C10 1.383(13) . ?
C11 C12 1.377(12) . ?
C12 C13 1.374(13) . ?
C13 C14 1.354(13) . ?
C14 C15 1.381(12) . ?

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 U O2 178.1(3) . . ?
O1 U N3 89.6(2) . . ?
O2 U N3 92.2(3) . . ?
O1 U N2 87.9(3) . . ?
O2 U N2 90.7(3) . . ?
N3 U N2 144.1(2) . . ?
O1 U N1 89.3(2) . . ?
O2 U N1 89.0(3) . . ?
N3 U N1 149.7(2) . . ?
N2 U N1 66.1(2) . . ?
O1 U I1 88.63(19) . . ?
O2 U I1 92.2(2) . . ?
N3 U I1 71.85(15) . . ?
N2 U I1 72.30(16) . . ?
N1 U I1 138.37(16) . . ?
O1 U I2 87.50(19) . . ?
O2 U I2 92.8(2) . . ?
N3 U I2 73.00(15) . . ?
N2 U I2 142.54(16) . . ?
N1 U I2 76.70(16) . . ?
I1 U I2 144.649(19) . . ?
C1 N1 C5 118.1(8) . . ?
C1 N1 U 120.0(6) . . ?
C5 N1 U 121.1(6) . . ?
C10 N2 C6 117.8(8) . . ?
C10 N2 U 120.4(6) . . ?
C6 N2 U 121.8(6) . . ?
C15 N3 C11 116.8(7) . . ?
C15 N3 U 120.6(6) . . ?
C11 N3 U 122.1(5) . . ?
N1 C1 C2 121.7(10) . . ?
C3 C2 C1 120.5(10) . . ?
C2 C3 C4 118.0(9) . . ?
C3 C4 C5 120.0(10) . . ?
N1 C5 C4 121.6(9) . . ?
N2 C6 C7 121.9(10) . . ?
C8 C7 C6 118.7(10) . . ?
C9 C8 C7 120.3(10) . . ?
C8 C9 C10 117.9(10) . . ?
N2 C10 C9 123.3(9) . . ?
N3 C11 C12 123.3(8) . . ?
C11 C12 C13 118.0(9) . . ?
C14 C13 C12 120.3(8) . . ?
C13 C14 C15 118.8(9) . . ?
N3 C15 C14 122.8(9) . . ?