# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2017

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1544486'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[PPh4][UCl6]'
_chemical_name_common            'Uranium(IV) hexachloride'
_chemical_melting_point          'not measured'
_chemical_formula_moiety         UCl6(P(C6H5)4)
_chemical_formula_sum            'C24 H20 Cl6 P U'
_chemical_formula_weight         790.10

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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'

_cell_length_a                   22.6559(16)
_cell_length_b                   6.7274(5)
_cell_length_c                   17.4505(12)
_cell_angle_alpha                90
_cell_angle_beta                 97.2180(7)
_cell_angle_gamma                90
_cell_volume                     2638.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    14783
_cell_measurement_theta_min      1.812
_cell_measurement_theta_max      28.628

_exptl_crystal_description       blocks
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_F_000             1492
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    6.832
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_T_max  0.504
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14783
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.812
_diffrn_reflns_theta_max         28.628
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3229
_reflns_number_gt                2956
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXP-2014 (Sheldrick, 2014)'
_computing_publication_material  'SHELXCIF-2014 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0115P)²+3.1408P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3229
_refine_ls_number_parameters     147
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0148
_refine_ls_R_factor_gt           0.0123
_refine_ls_wR_factor_ref         0.0288
_refine_ls_wR_factor_gt          0.0280
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_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 0.2500 0.7500 0.0000 0.01138(3) Uani 1 2 d S . P . .
Cl1 Cl 0.34736(2) 0.93228(7) 0.00444(2) 0.02093(9) Uani 1 1 d . . . . .
Cl2 Cl 0.28946(2) 0.56089(7) 0.11998(3) 0.02297(9) Uani 1 1 d . . . . .
Cl3 Cl 0.21122(2) 1.01081(8) 0.08330(3) 0.03022(11) Uani 1 1 d . . . . .
P1 P 0.0000 0.16732(9) 0.2500 0.01092(11) Uani 1 2 d S T P . .
C1 C -0.00944(7) 0.0097(2) 0.16628(9) 0.0123(3) Uani 1 1 d . . . . .
C2 C 0.03431(7) -0.1332(2) 0.15818(9) 0.0147(3) Uani 1 1 d . . . . .
H2A H 0.0668 -0.1466 0.1961 0.018 Uiso 1 1 calc R U . . .
C3 C 0.02911(8) -0.2545(2) 0.09364(10) 0.0172(3) Uani 1 1 d . . . . .
H3A H 0.0587 -0.3466 0.0872 0.021 Uiso 1 1 calc R U . . .
C4 C -0.02063(8) -0.2383(2) 0.03838(10) 0.0179(3) Uani 1 1 d . . . . .
H4A H -0.0244 -0.3212 -0.0046 0.021 Uiso 1 1 calc R U . . .
C5 C -0.06443(7) -0.1000(3) 0.04683(10) 0.0167(3) Uani 1 1 d . . . . .
H5A H -0.0977 -0.0913 0.0099 0.020 Uiso 1 1 calc R U . . .
C6 C -0.05877(7) 0.0262(2) 0.11045(9) 0.0140(3) Uani 1 1 d . . . . .
H6A H -0.0878 0.1212 0.1157 0.017 Uiso 1 1 calc R U . . .
C7 C 0.06470(7) 0.3212(2) 0.24735(9) 0.0123(3) Uani 1 1 d . . . . .
C8 C 0.07680(7) 0.4680(2) 0.30358(10) 0.0150(3) Uani 1 1 d . . . . .
H8A H 0.0507 0.4889 0.3399 0.018 Uiso 1 1 calc R U . . .
C9 C 0.12774(7) 0.5827(2) 0.30533(10) 0.0166(3) Uani 1 1 d . . . . .
H9A H 0.1361 0.6793 0.3433 0.020 Uiso 1 1 calc R U . . .
C10 C 0.16630(7) 0.5537(3) 0.25053(10) 0.0171(3) Uani 1 1 d . . . . .
H10A H 0.2003 0.6315 0.2516 0.021 Uiso 1 1 calc R U . . .
C11 C 0.15417(7) 0.4090(3) 0.19427(10) 0.0178(3) Uani 1 1 d . . . . .
H11A H 0.1801 0.3902 0.1576 0.021 Uiso 1 1 calc R U . . .
C12 C 0.10357(8) 0.2919(2) 0.19219(10) 0.0153(3) Uani 1 1 d . . . . .
H12A H 0.0956 0.1947 0.1544 0.018 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 Cl3 2.5068(5) 7_565 ?
U1 Cl3 2.5068(5) . ?
U1 Cl2 2.5162(4) . ?
U1 Cl2 2.5162(4) 7_565 ?
U1 Cl1 2.5163(4) . ?
U1 Cl1 2.5164(4) 7_565 ?
P1 C1 1.7960(16) . ?
P1 C1 1.7961(16) 2 ?
P1 C7 1.7999(16) 2 ?
P1 C7 1.7999(16) . ?
C1 C6 1.392(2) . ?
C1 C2 1.401(2) . ?
C2 C3 1.384(2) . ?
C3 C4 1.392(3) . ?
C4 C5 1.382(2) . ?
C5 C6 1.391(2) . ?
C7 C8 1.395(2) . ?
C7 C12 1.398(2) . ?
C8 C9 1.385(2) . ?
C9 C10 1.388(2) . ?
C10 C11 1.385(2) . ?
C11 C12 1.388(2) . ?

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
Cl3 U1 Cl3 179.999(18) 7_565 . ?
Cl3 U1 Cl2 90.850(17) 7_565 . ?
Cl3 U1 Cl2 89.150(17) . . ?
Cl3 U1 Cl2 89.150(17) 7_565 7_565 ?
Cl3 U1 Cl2 90.850(17) . 7_565 ?
Cl2 U1 Cl2 180.0 . 7_565 ?
Cl3 U1 Cl1 89.386(16) 7_565 . ?
Cl3 U1 Cl1 90.615(16) . . ?
Cl2 U1 Cl1 90.133(14) . . ?
Cl2 U1 Cl1 89.865(14) 7_565 . ?
Cl3 U1 Cl1 90.615(16) 7_565 7_565 ?
Cl3 U1 Cl1 89.384(16) . 7_565 ?
Cl2 U1 Cl1 89.866(14) . 7_565 ?
Cl2 U1 Cl1 90.136(14) 7_565 7_565 ?
Cl1 U1 Cl1 180.0 . 7_565 ?
C1 P1 C1 107.65(11) . 2 ?
C1 P1 C7 110.25(7) . 2 ?
C1 P1 C7 109.44(7) 2 2 ?
C1 P1 C7 109.44(7) . . ?
C1 P1 C7 110.25(7) 2 . ?
C7 P1 C7 109.79(11) 2 . ?
C6 C1 C2 120.02(15) . . ?
C6 C1 P1 121.70(12) . . ?
C2 C1 P1 118.28(12) . . ?
C3 C2 C1 119.87(15) . . ?
C2 C3 C4 119.74(16) . . ?
C5 C4 C3 120.57(16) . . ?
C4 C5 C6 120.06(16) . . ?
C5 C6 C1 119.70(15) . . ?
C8 C7 C12 119.96(15) . . ?
C8 C7 P1 118.54(12) . . ?
C12 C7 P1 121.47(13) . . ?
C9 C8 C7 119.96(15) . . ?
C8 C9 C10 120.08(16) . . ?
C11 C10 C9 120.08(16) . . ?
C10 C11 C12 120.48(16) . . ?
C11 C12 C7 119.44(16) . . ?

_refine_diff_density_max         0.405
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.069

