#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:20:45 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179056 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/18/4301828.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_4301828
loop_
_publ_author_name
'Skye Fortier'
'Guang Wu'
'Trevor W. Hayton'
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W. Hayton'
_publ_section_title
;
Synthesis and Redox Chemistry of High-Valent Uranium Aryloxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3000
_journal_page_last               3011
_journal_paper_doi               10.1021/ic802266y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C32 H18 F20 O6 U'
_chemical_formula_weight         1116.49
_chemical_name_systematic
; 
 Uranium(VI) bis(tert-butoxide) tetrakis(pentafluorophenoxide)
;
_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                68.547(7)
_cell_angle_beta                 63.240(7)
_cell_angle_gamma                62.611(6)
_cell_formula_units_Z            1
_cell_length_a                   10.147(5)
_cell_length_b                   10.565(5)
_cell_length_c                   10.637(5)
_cell_measurement_temperature    150(2)
_cell_volume                     885.8(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0989
_diffrn_reflns_av_sigmaI/netI    0.1108
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5948
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    4.731
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.466
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Psi Scan'
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       kite
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.218
_refine_diff_density_min         -1.690
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0757P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1475
_reflns_number_gt                2775
_reflns_number_total             3319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802266y_si_002_3.cif
_cod_data_source_block           Complex_6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        885.8(8)
_cod_database_code               4301828
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
_atom_site_disorder_assembly
_atom_site_disorder_group
F8 F 1.0282(8) 0.8450(8) 0.4374(8) 0.079(2) Uani 1 1 d . . .
F7 F 0.9576(9) 0.8582(8) 0.2121(8) 0.079(2) Uani 1 1 d . . .
C10 C 0.9468(13) 0.7652(12) 0.4551(13) 0.055(3) Uani 1 1 d . . .
C9 C 0.9076(13) 0.7757(12) 0.3405(12) 0.056(3) Uani 1 1 d . . .
U1 U 0.5000 0.5000 0.5000 0.0428(2) Uani 1 2 d S . .
F1 F 0.6943(7) 0.2610(6) 0.8090(7) 0.0587(16) Uani 1 1 d . . .
F5 F 0.5112(8) 0.0522(7) 0.6277(7) 0.0595(16) Uani 1 1 d . . .
F2 F 0.7757(8) 0.0081(7) 0.9948(7) 0.0644(17) Uani 1 1 d . . .
O2 O 0.6812(9) 0.5340(7) 0.5117(8) 0.0508(17) Uani 1 1 d . . .
O1 O 0.5677(9) 0.2865(7) 0.6187(8) 0.0548(18) Uani 1 1 d . . .
O3 O 0.3411(11) 0.5781(9) 0.6954(8) 0.073(3) Uani 1 1 d . . .
C2 C 0.6715(12) 0.1451(11) 0.8086(11) 0.046(2) Uani 1 1 d . . .
C1 C 0.6023(11) 0.1649(11) 0.7106(10) 0.042(2) Uani 1 1 d . . .
C6 C 0.5777(13) 0.0409(11) 0.7183(11) 0.050(3) Uani 1 1 d . . .
C3 C 0.7106(11) 0.0189(11) 0.9034(11) 0.046(2) Uani 1 1 d . . .
C13 C 0.2685(14) 0.6609(13) 0.8071(12) 0.058(3) Uani 1 1 d . . .
F10 F 0.7683(7) 0.5150(7) 0.7300(6) 0.0531(14) Uani 1 1 d . . .
F4 F 0.5860(8) -0.1990(6) 0.8196(7) 0.0607(16) Uani 1 1 d . . .
F9 F 0.9387(7) 0.6665(8) 0.6935(7) 0.0657(18) Uani 1 1 d . . .
F3 F 0.7235(8) -0.2245(7) 0.9980(7) 0.0667(17) Uani 1 1 d . . .
F6 F 0.7904(8) 0.7022(8) 0.2477(7) 0.0678(18) Uani 1 1 d . . .
C7 C 0.7708(11) 0.6099(10) 0.4887(10) 0.039(2) Uani 1 1 d . . .
C12 C 0.8118(11) 0.6003(10) 0.6015(10) 0.042(2) Uani 1 1 d . . .
C8 C 0.8230(12) 0.6953(11) 0.3599(11) 0.046(2) Uani 1 1 d . . .
C4 C 0.6845(12) -0.0986(11) 0.9049(11) 0.048(2) Uani 1 1 d . . .
C11 C 0.8995(12) 0.6792(12) 0.5827(12) 0.049(3) Uani 1 1 d . . .
C5 C 0.6169(12) -0.0852(10) 0.8125(11) 0.047(2) Uani 1 1 d . . .
C15 C 0.365(2) 0.586(2) 0.9029(18) 0.111(6) Uani 1 1 d . . .
H15A H 0.4712 0.5846 0.8483 0.167 Uiso 1 1 calc R . .
H15B H 0.3666 0.4884 0.9430 0.167 Uiso 1 1 calc R . .
H15C H 0.3202 0.6378 0.9790 0.167 Uiso 1 1 calc R . .
C14 C 0.277(5) 0.800(2) 0.727(2) 0.225(18) Uani 1 1 d . . .
H14A H 0.3827 0.7882 0.6613 0.338 Uiso 1 1 calc R . .
H14B H 0.2495 0.8587 0.7921 0.338 Uiso 1 1 calc R . .
H14C H 0.2050 0.8457 0.6752 0.338 Uiso 1 1 calc R . .
C16 C 0.115(2) 0.649(5) 0.897(3) 0.26(2) Uani 1 1 d . . .
H16A H 0.0894 0.6614 0.9919 0.388 Uiso 1 1 calc R . .
H16B H 0.1181 0.5552 0.9033 0.388 Uiso 1 1 calc R . .
H16C H 0.0368 0.7233 0.8568 0.388 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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_
_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
C11 C10 F8 120.6(10) . . ?
C11 C10 C9 120.1(9) . . ?
F8 C10 C9 119.3(11) . . ?
F7 C9 C8 120.6(10) . . ?
F7 C9 C10 120.4(10) . . ?
C8 C9 C10 118.9(10) . . ?
O2 U1 O2 180.0 . 2_666 ?
O2 U1 O1 89.5(3) . 2_666 ?
O2 U1 O1 90.5(3) 2_666 2_666 ?
O2 U1 O1 90.5(3) . . ?
O2 U1 O1 89.5(3) 2_666 . ?
O1 U1 O1 180.000(1) 2_666 . ?
O2 U1 O3 89.6(3) . 2_666 ?
O2 U1 O3 90.4(3) 2_666 2_666 ?
O1 U1 O3 90.2(3) 2_666 2_666 ?
O1 U1 O3 89.8(3) . 2_666 ?
O2 U1 O3 90.4(3) . . ?
O2 U1 O3 89.6(3) 2_666 . ?
O1 U1 O3 89.8(3) 2_666 . ?
O1 U1 O3 90.2(3) . . ?
O3 U1 O3 180.000(1) 2_666 . ?
C7 O2 U1 156.4(6) . . ?
C1 O1 U1 170.1(6) . . ?
C13 O3 U1 159.9(8) . . ?
F1 C2 C3 119.4(8) . . ?
F1 C2 C1 116.9(9) . . ?
C3 C2 C1 123.6(9) . . ?
O1 C1 C6 123.3(8) . . ?
O1 C1 C2 122.6(8) . . ?
C6 C1 C2 114.1(9) . . ?
F5 C6 C5 120.3(9) . . ?
F5 C6 C1 117.3(9) . . ?
C5 C6 C1 122.5(9) . . ?
F2 C3 C2 120.4(9) . . ?
F2 C3 C4 120.2(9) . . ?
C2 C3 C4 119.4(9) . . ?
C14 C13 O3 102.5(11) . . ?
C14 C13 C16 119(3) . . ?
O3 C13 C16 109.5(15) . . ?
C14 C13 C15 113.5(19) . . ?
O3 C13 C15 106.9(10) . . ?
C16 C13 C15 104.9(15) . . ?
C8 C7 O2 123.0(8) . . ?
C8 C7 C12 118.0(9) . . ?
O2 C7 C12 119.0(9) . . ?
F10 C12 C11 118.4(8) . . ?
F10 C12 C7 121.1(8) . . ?
C11 C12 C7 120.4(10) . . ?
F6 C8 C7 119.3(9) . . ?
F6 C8 C9 118.6(10) . . ?
C7 C8 C9 122.1(9) . . ?
F3 C4 C5 120.6(9) . . ?
F3 C4 C3 120.0(9) . . ?
C5 C4 C3 119.4(9) . . ?
C10 C11 F9 120.6(9) . . ?
C10 C11 C12 120.4(9) . . ?
F9 C11 C12 119.0(10) . . ?
F4 C5 C6 120.3(9) . . ?
F4 C5 C4 118.7(9) . . ?
C6 C5 C4 121.0(9) . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
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
F8 C10 1.346(12) . ?
F7 C9 1.339(13) . ?
C10 C11 1.345(16) . ?
C10 C9 1.398(16) . ?
C9 C8 1.373(15) . ?
U1 O2 2.091(6) . ?
U1 O2 2.091(6) 2_666 ?
U1 O1 2.104(7) 2_666 ?
U1 O1 2.104(7) . ?
U1 O3 2.148(7) 2_666 ?
U1 O3 2.148(7) . ?
F1 C2 1.348(11) . ?
F5 C6 1.352(11) . ?
F2 C3 1.350(10) . ?
O2 C7 1.363(11) . ?
O1 C1 1.306(12) . ?
O3 C13 1.448(11) . ?
C2 C3 1.357(15) . ?
C2 C1 1.410(13) . ?
C1 C6 1.410(14) . ?
C6 C5 1.354(15) . ?
C3 C4 1.376(15) . ?
C13 C14 1.42(2) . ?
C13 C16 1.45(2) . ?
C13 C15 1.492(18) . ?
F10 C12 1.340(12) . ?
F4 C5 1.345(11) . ?
F9 C11 1.350(11) . ?
F3 C4 1.346(12) . ?
F6 C8 1.344(11) . ?
C7 C8 1.362(14) . ?
C7 C12 1.394(12) . ?
C12 C11 1.388(14) . ?
C4 C5 1.368(14) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 C10 C9 F7 -178.3(10) . . . . ?
F8 C10 C9 F7 3.6(16) . . . . ?
C11 C10 C9 C8 -1.1(16) . . . . ?
F8 C10 C9 C8 -179.3(9) . . . . ?
O2 U1 O2 C7 -48(100) 2_666 . . . ?
O1 U1 O2 C7 0.9(15) 2_666 . . . ?
O1 U1 O2 C7 -179.1(15) . . . . ?
O3 U1 O2 C7 91.1(15) 2_666 . . . ?
O3 U1 O2 C7 -88.9(15) . . . . ?
O2 U1 O1 C1 65(4) . . . . ?
O2 U1 O1 C1 -115(4) 2_666 . . . ?
O1 U1 O1 C1 -16(100) 2_666 . . . ?
O3 U1 O1 C1 155(4) 2_666 . . . ?
O3 U1 O1 C1 -25(4) . . . . ?
O2 U1 O3 C13 32(2) . . . . ?
O2 U1 O3 C13 -148(2) 2_666 . . . ?
O1 U1 O3 C13 -58(2) 2_666 . . . ?
O1 U1 O3 C13 122(2) . . . . ?
O3 U1 O3 C13 -46(100) 2_666 . . . ?
U1 O1 C1 C6 143(4) . . . . ?
U1 O1 C1 C2 -39(5) . . . . ?
F1 C2 C1 O1 3.2(14) . . . . ?
C3 C2 C1 O1 -178.9(10) . . . . ?
F1 C2 C1 C6 -178.3(9) . . . . ?
C3 C2 C1 C6 -0.5(14) . . . . ?
O1 C1 C6 F5 -1.7(15) . . . . ?
C2 C1 C6 F5 179.8(9) . . . . ?
O1 C1 C6 C5 178.7(10) . . . . ?
C2 C1 C6 C5 0.3(15) . . . . ?
F1 C2 C3 F2 -1.8(14) . . . . ?
C1 C2 C3 F2 -179.6(9) . . . . ?
F1 C2 C3 C4 178.8(9) . . . . ?
C1 C2 C3 C4 0.9(15) . . . . ?
U1 O3 C13 C14 38(3) . . . . ?
U1 O3 C13 C16 165(2) . . . . ?
U1 O3 C13 C15 -82(2) . . . . ?
U1 O2 C7 C8 -44.0(19) . . . . ?
U1 O2 C7 C12 136.1(12) . . . . ?
C8 C7 C12 F10 -178.0(8) . . . . ?
O2 C7 C12 F10 1.9(13) . . . . ?
C8 C7 C12 C11 1.7(14) . . . . ?
O2 C7 C12 C11 -178.3(8) . . . . ?
O2 C7 C8 F6 -2.5(14) . . . . ?
C12 C7 C8 F6 177.5(8) . . . . ?
O2 C7 C8 C9 177.2(9) . . . . ?
C12 C7 C8 C9 -2.9(15) . . . . ?
F7 C9 C8 F6 -0.6(15) . . . . ?
C10 C9 C8 F6 -177.7(9) . . . . ?
F7 C9 C8 C7 179.7(9) . . . . ?
C10 C9 C8 C7 2.6(16) . . . . ?
F2 C3 C4 F3 0.2(15) . . . . ?
C2 C3 C4 F3 179.7(9) . . . . ?
F2 C3 C4 C5 179.3(9) . . . . ?
C2 C3 C4 C5 -1.2(15) . . . . ?
F8 C10 C11 F9 -2.9(15) . . . . ?
C9 C10 C11 F9 179.0(9) . . . . ?
F8 C10 C11 C12 178.2(9) . . . . ?
C9 C10 C11 C12 0.1(16) . . . . ?
F10 C12 C11 C10 179.4(9) . . . . ?
C7 C12 C11 C10 -0.4(15) . . . . ?
F10 C12 C11 F9 0.5(13) . . . . ?
C7 C12 C11 F9 -179.3(8) . . . . ?
F5 C6 C5 F4 -1.9(15) . . . . ?
C1 C6 C5 F4 177.6(9) . . . . ?
F5 C6 C5 C4 179.9(9) . . . . ?
C1 C6 C5 C4 -0.6(16) . . . . ?
F3 C4 C5 F4 1.9(14) . . . . ?
C3 C4 C5 F4 -177.1(8) . . . . ?
F3 C4 C5 C6 -179.9(9) . . . . ?
C3 C4 C5 C6 1.0(15) . . . . ?
