#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:50:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179992 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/86/7028616.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7028616
loop_
_publ_author_name
'Hashem, Emtithal'
'McCabe, Thomas'
'Schulzke, Carola'
'Baker, Robert J.'
_publ_section_title
;
 Synthesis, structure and photophysical properties of [UO2X2(O=PPh3)2] (X
 = Cl, Br, I).
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1125
_journal_page_last               1131
_journal_paper_doi               10.1039/c3dt52480a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C48 H48 Cl4 Li2 N6 O4 P2 U'
_chemical_formula_weight         1228.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.91(3)
_cell_angle_beta                 93.92(3)
_cell_angle_gamma                108.10(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5374(19)
_cell_length_b                   12.329(3)
_cell_length_c                   13.578(3)
_cell_measurement_reflns_used    4118
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      31.2338
_cell_measurement_theta_min      3.1415
_cell_volume                     1339.1(8)
_computing_data_collection       'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Mercury 2.3'
_computing_publication_material  'Mercury 2.3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      108(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.786
_diffrn_measurement_details
;
scan:
    Number of images: 250
               Slice: -55.0000 - 70.0000
         Image width: 0.5000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 50.0000
                 Phi: 0.0000
                 XTD: 45.1786
              2theta: -20.0542
scan:
    Number of images: 218
               Slice: -55.0000 - 54.0000
         Image width: 0.5000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 50.0000
                 Phi: 90.0000
                 XTD: 45.1786
              2theta: -20.0542
scan:
    Number of images: 180
               Slice: -110.0000 - -20.0000
         Image width: 0.5000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 0.0000
                 XTD: 45.1786
              2theta: -20.0542
scan:
    Number of images: 150
               Slice: -91.2500 - -16.2500
         Image width: 0.5000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 90.0000
                 XTD: 45.1786
              2theta: -20.0542

;
_diffrn_measurement_device
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12900
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.18
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    3.335
_exptl_absorpt_correction_T_max  0.6610
_exptl_absorpt_correction_T_min  0.1900
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.682
_refine_diff_density_min         -1.651
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0359P)²+0.7418P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0560
_reflns_number_gt                6804
_reflns_number_total             6805
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3dt52480a.txt
_cod_data_source_block           compound_2
_cod_original_cell_volume        1339.2(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7028616
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
U1 U 0.0000 0.5000 0.5000 0.01439(4) Uani 1 2 d S
Cl1 Cl -0.04109(6) 0.25171(5) 0.38062(5) 0.02753(11) Uani 1 1 d .
Cl2 Cl -0.29438(5) 0.44769(6) 0.43265(5) 0.02452(10) Uani 1 1 d .
P1 P 1.05674(5) 0.24164(5) -0.00894(4) 0.01358(9) Uani 1 1 d .
O1 O 0.03649(17) 0.52617(16) 0.38391(13) 0.0226(3) Uani 1 1 d .
O2 O 1.03857(15) 0.12059(14) 0.00072(12) 0.0162(3) Uani 1 1 d .
N1 N 0.7095(2) 0.0073(2) 0.04648(18) 0.0253(4) Uani 1 1 d .
N2 N 0.7735(2) -0.1076(2) -0.21280(17) 0.0248(4) Uani 1 1 d .
C6 C 0.3041(3) 0.7914(3) 0.4346(3) 0.0445(7) Uani 1 1 d .
H6A H 0.3821 0.8107 0.4969 0.067 Uiso 1 1 calc R
H6B H 0.2780 0.7027 0.3762 0.067 Uiso 1 1 calc R
H6C H 0.2135 0.8010 0.4611 0.067 Uiso 1 1 calc R
Li1 Li 0.8574(4) -0.0337(4) -0.0479(3) 0.0185(7) Uani 1 1 d .
C1 C 0.6549(2) 0.0546(2) 0.11639(19) 0.0218(4) Uani 1 1 d .
C2 C 0.5835(3) 0.1146(3) 0.2047(2) 0.0281(5) Uani 1 1 d .
H2A H 0.5015 0.1313 0.1737 0.042 Uiso 1 1 calc R
H2B H 0.6591 0.1961 0.2632 0.042 Uiso 1 1 calc R
H2C H 0.5421 0.0566 0.2364 0.042 Uiso 1 1 calc R
C3 C 0.7290(2) -0.1617(2) -0.30728(18) 0.0209(4) Uani 1 1 d .
C4 C 0.6693(3) -0.2338(3) -0.4281(2) 0.0293(5) Uani 1 1 d .
H4A H 0.7297 -0.2850 -0.4621 0.044 Uiso 1 1 calc R
H4B H 0.6747 -0.1734 -0.4582 0.044 Uiso 1 1 calc R
H4C H 0.5636 -0.2913 -0.4448 0.044 Uiso 1 1 calc R
C5 C 0.3608(4) 0.8793(3) 0.3898(2) 0.0451(7) Uani 1 1 d .
N3 N 0.4043(5) 0.9496(4) 0.3556(3) 0.0796(13) Uani 1 1 d .
C11 C 0.8910(2) 0.2804(2) 0.01164(17) 0.0160(3) Uani 1 1 d .
C12 C 0.8776(2) 0.3546(2) 0.11873(18) 0.0197(4) Uani 1 1 d .
H12 H 0.9625 0.3967 0.1801 0.024 Uiso 1 1 calc R
C13 C 0.7402(2) 0.3671(2) 0.1356(2) 0.0231(4) Uani 1 1 d .
H13 H 0.7315 0.4180 0.2086 0.028 Uiso 1 1 calc R
C14 C 0.6155(2) 0.3056(2) 0.0462(2) 0.0253(4) Uani 1 1 d .
H14 H 0.5214 0.3136 0.0582 0.030 Uiso 1 1 calc R
C15 C 0.6285(2) 0.2325(2) -0.0606(2) 0.0242(4) Uani 1 1 d .
H15 H 0.5436 0.1919 -0.1218 0.029 Uiso 1 1 calc R
C16 C 0.7649(2) 0.2184(2) -0.07863(18) 0.0197(4) Uani 1 1 d .
H16 H 0.7728 0.1670 -0.1517 0.024 Uiso 1 1 calc R
C21 C 1.2198(2) 0.3735(2) 0.09408(16) 0.0161(3) Uani 1 1 d .
C22 C 1.2481(2) 0.3789(2) 0.19894(18) 0.0210(4) Uani 1 1 d .
H22 H 1.1778 0.3183 0.2151 0.025 Uiso 1 1 calc R
C23 C 1.3782(3) 0.4725(2) 0.27954(19) 0.0264(4) Uani 1 1 d .
H23 H 1.3973 0.4754 0.3504 0.032 Uiso 1 1 calc R
C24 C 1.4806(3) 0.5619(3) 0.2561(2) 0.0279(5) Uani 1 1 d .
H24 H 1.5707 0.6248 0.3105 0.033 Uiso 1 1 calc R
C25 C 1.4514(2) 0.5594(2) 0.1537(2) 0.0255(4) Uani 1 1 d .
H25 H 1.5203 0.6221 0.1389 0.031 Uiso 1 1 calc R
C26 C 1.3212(2) 0.4653(2) 0.07208(18) 0.0215(4) Uani 1 1 d .
H26 H 1.3017 0.4637 0.0018 0.026 Uiso 1 1 calc R
C31 C 1.0794(2) 0.2194(2) -0.14586(16) 0.0169(4) Uani 1 1 d .
C32 C 1.0645(2) 0.3055(2) -0.18404(19) 0.0220(4) Uani 1 1 d .
H32 H 1.0460 0.3796 -0.1364 0.026 Uiso 1 1 calc R
C33 C 1.0769(3) 0.2819(2) -0.2917(2) 0.0275(5) Uani 1 1 d .
H33 H 1.0673 0.3403 -0.3177 0.033 Uiso 1 1 calc R
C34 C 1.1029(3) 0.1744(3) -0.36103(19) 0.0308(5) Uani 1 1 d .
H34 H 1.1099 0.1585 -0.4350 0.037 Uiso 1 1 calc R
C35 C 1.1191(3) 0.0889(3) -0.3238(2) 0.0316(5) Uani 1 1 d .
H35 H 1.1381 0.0153 -0.3720 0.038 Uiso 1 1 calc R
C36 C 1.1073(3) 0.1112(2) -0.21567(18) 0.0231(4) Uani 1 1 d .
H36 H 1.1182 0.0530 -0.1898 0.028 Uiso 1 1 calc R
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'
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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O1 U1 O1 180.000(1) . 2_566
O1 U1 Cl1 89.82(6) . 2_566
O1 U1 Cl1 90.18(6) 2_566 2_566
O1 U1 Cl1 90.18(6) . .
O1 U1 Cl1 89.82(6) 2_566 .
Cl1 U1 Cl1 180.0 2_566 .
O1 U1 Cl2 90.27(6) . 2_566
O1 U1 Cl2 89.73(6) 2_566 2_566
Cl1 U1 Cl2 91.17(5) 2_566 2_566
Cl1 U1 Cl2 88.83(5) . 2_566
O1 U1 Cl2 89.73(6) . .
O1 U1 Cl2 90.27(6) 2_566 .
Cl1 U1 Cl2 88.83(5) 2_566 .
Cl1 U1 Cl2 91.17(5) . .
Cl2 U1 Cl2 180.0 2_566 .
O2 P1 C11 110.34(8) . .
O2 P1 C21 109.61(9) . .
C11 P1 C21 109.45(10) . .
O2 P1 C31 110.77(10) . .
C11 P1 C31 107.24(9) . .
C21 P1 C31 109.39(9) . .
P1 O2 Li1 144.84(14) . 2_755
P1 O2 Li1 128.93(13) . .
Li1 O2 Li1 86.19(15) 2_755 .
C1 N1 Li1 164.0(2) . .
C3 N2 Li1 172.1(2) . .
O2 Li1 O2 93.81(15) 2_755 .
O2 Li1 N1 110.13(17) 2_755 .
O2 Li1 N1 109.8(2) . .
O2 Li1 N2 117.9(2) 2_755 .
O2 Li1 N2 109.13(18) . .
N1 Li1 N2 114.05(17) . .
O2 Li1 Li1 47.28(11) 2_755 2_755
O2 Li1 Li1 46.53(12) . 2_755
N1 Li1 Li1 120.0(2) . 2_755
N2 Li1 Li1 125.6(2) . 2_755
N1 C1 C2 179.3(2) . .
N2 C3 C4 178.5(3) . .
N3 C5 C6 178.9(5) . .
C12 C11 C16 119.58(18) . .
C12 C11 P1 120.58(15) . .
C16 C11 P1 119.07(16) . .
C13 C12 C11 120.1(2) . .
C14 C13 C12 120.3(2) . .
C15 C14 C13 119.9(2) . .
C14 C15 C16 120.4(2) . .
C15 C16 C11 119.7(2) . .
C26 C21 C22 119.50(19) . .
C26 C21 P1 123.02(15) . .
C22 C21 P1 117.41(15) . .
C23 C22 C21 120.38(19) . .
C22 C23 C24 119.8(2) . .
C25 C24 C23 120.2(2) . .
C24 C25 C26 120.4(2) . .
C25 C26 C21 119.75(19) . .
C36 C31 C32 120.05(18) . .
C36 C31 P1 118.36(14) . .
C32 C31 P1 121.55(17) . .
C33 C32 C31 119.6(2) . .
C34 C33 C32 120.3(2) . .
C33 C34 C35 120.5(2) . .
C34 C35 C36 119.9(2) . .
C31 C36 C35 119.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.7730(14) .
U1 O1 1.7730(14) 2_566
U1 Cl1 2.6721(12) 2_566
U1 Cl1 2.6721(12) .
U1 Cl2 2.6762(9) 2_566
U1 Cl2 2.6762(9) .
P1 O2 1.5106(14) .
P1 C11 1.795(2) .
P1 C21 1.799(2) .
P1 C31 1.8002(19) .
O2 Li1 1.922(4) 2_755
O2 Li1 1.945(4) .
N1 C1 1.141(3) .
N1 Li1 2.009(4) .
N2 C3 1.140(3) .
N2 Li1 2.016(4) .
C6 C5 1.439(4) .
Li1 O2 1.922(4) 2_755
Li1 Li1 2.642(7) 2_755
C1 C2 1.457(3) .
C3 C4 1.461(3) .
C5 N3 1.132(4) .
C11 C12 1.395(3) .
C11 C16 1.404(3) .
C12 C13 1.390(3) .
C13 C14 1.389(3) .
C14 C15 1.387(4) .
C15 C16 1.389(3) .
C21 C26 1.396(3) .
C21 C22 1.400(3) .
C22 C23 1.389(3) .
C23 C24 1.393(3) .
C24 C25 1.384(3) .
C25 C26 1.396(3) .
C31 C36 1.393(3) .
C31 C32 1.401(3) .
C32 C33 1.386(3) .
C33 C34 1.375(4) .
C34 C35 1.388(4) .
C35 C36 1.396(3) .
