#------------------------------------------------------------------------------
#$Date: 2019-10-28 09:27:44 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219813 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/46/4514628.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_4514628
loop_
_publ_author_name
'Monsigny, Louis'
'Thuéry, Pierre'
'Berthet, Jean-Claude'
'Cantat, Thibault'
_publ_section_title
;
 Breaking C--O Bonds with Uranium: Uranyl Complexes as Selective Catalysts
 in the Hydrosilylation of Aldehydes
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              9025
_journal_paper_doi               10.1021/acscatal.9b01408
_journal_volume                  9
_journal_year                    2019
_chemical_formula_sum            'C9 H6 F6 O9 S2 U'
_chemical_formula_weight         674.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                75.998(5)
_cell_angle_beta                 71.713(4)
_cell_angle_gamma                79.448(5)
_cell_formula_units_Z            2
_cell_length_a                   8.7768(7)
_cell_length_b                   9.4553(6)
_cell_length_c                   11.5011(10)
_cell_measurement_reflns_used    38780
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.46
_cell_volume                     873.34(12)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'1 φ and 12 ω scans with 2° steps (637 frames)'
_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  0.0408
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            38780
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.461
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.635
_exptl_absorpt_correction_T_max  0.286
_exptl_absorpt_correction_T_min  0.211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.564
_exptl_crystal_description       irregular
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.933
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0231P)²+0.4087P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3034
_reflns_number_total             3310
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cs9b01408_si_002.cif
_cod_data_source_block           26
_cod_database_code               4514628
_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.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
U1 U 0.70206(2) 0.20717(3) 0.04133(2) 0.02669(9) Uani 1 1 d . .
S1 S 1.12066(17) 0.1517(2) -0.16903(14) 0.0302(4) Uani 1 1 d . .
S2 S 0.69020(18) 0.5798(2) -0.17166(14) 0.0314(4) Uani 1 1 d . .
O1 O 0.8104(5) 0.2443(6) 0.1317(4) 0.0351(11) Uani 1 1 d . .
O2 O 0.5909(5) 0.1669(6) -0.0463(4) 0.0324(11) Uani 1 1 d . .
O3 O 0.5249(5) 0.0727(6) 0.2201(4) 0.0333(11) Uani 1 1 d . .
O4 O 0.9458(5) 0.1822(5) -0.1267(4) 0.0327(11) Uani 1 1 d . .
O5 O 1.1830(5) 0.0459(5) -0.0732(4) 0.0319(11) Uani 1 1 d . .
O6 O 1.1817(5) 0.1244(6) -0.2916(4) 0.0444(14) Uani 1 1 d . .
O7 O 0.7398(5) 0.4423(6) -0.0975(4) 0.0391(11) Uani 1 1 d . .
O8 O 0.5152(5) 0.6208(5) -0.1317(4) 0.0367(11) Uani 1 1 d . .
O9 O 0.7869(5) 0.6938(6) -0.1938(5) 0.0420(13) Uani 1 1 d . .
F1 F 1.3508(5) 0.3034(7) -0.1974(6) 0.0799(17) Uani 1 1 d . .
F2 F 1.1486(6) 0.4273(6) -0.2559(5) 0.0756(16) Uani 1 1 d . .
F3 F 1.1310(6) 0.3599(6) -0.0616(5) 0.0733(16) Uani 1 1 d . .
F4 F 0.8752(4) 0.4931(6) -0.3719(4) 0.0545(13) Uani 1 1 d . .
F5 F 0.6789(6) 0.6536(7) -0.4003(4) 0.0646(14) Uani 1 1 d . .
F6 F 0.6365(6) 0.4306(6) -0.3144(4) 0.0672(16) Uani 1 1 d . .
C1 C 0.3950(7) 0.0240(8) 0.2374(6) 0.0316(15) Uani 1 1 d . .
H1 H 0.3471 0.0468 0.1706 0.038 Uiso 1 1 calc R U
C2 C 0.3142(7) -0.0643(8) 0.3529(6) 0.0297(15) Uani 1 1 d . .
C3 C 0.3872(8) -0.1189(9) 0.4501(6) 0.0399(18) Uani 1 1 d . .
H3 H 0.4938 -0.1004 0.4401 0.048 Uiso 1 1 calc R U
C4 C 0.3020(8) -0.1987(10) 0.5589(6) 0.0452(19) Uani 1 1 d . .
H4 H 0.3500 -0.2351 0.6253 0.054 Uiso 1 1 calc R U
C5 C 0.1459(8) -0.2283(9) 0.5748(7) 0.0447(19) Uani 1 1 d . .
H5 H 0.0882 -0.2834 0.6517 0.054 Uiso 1 1 calc R U
C6 C 0.0758(8) -0.1771(9) 0.4786(7) 0.0413(18) Uani 1 1 d . .
H6 H -0.0305 -0.1969 0.4890 0.050 Uiso 1 1 calc R U
C7 C 0.1605(8) -0.0967(8) 0.3667(6) 0.0353(16) Uani 1 1 d . .
H7 H 0.1135 -0.0637 0.2995 0.042 Uiso 1 1 calc R U
C8 C 1.1921(9) 0.3230(9) -0.1709(8) 0.049(2) Uani 1 1 d . .
C9 C 0.7215(8) 0.5356(10) -0.3245(7) 0.0426(19) Uani 1 1 d . .
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'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 '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
O1 U1 O2 178.6(2) . .
O1 U1 O3 92.03(18) . .
O2 U1 O3 86.62(18) . .
O1 U1 O8 87.48(18) . 2_665
O2 U1 O8 92.36(17) . 2_665
O3 U1 O8 72.13(16) . 2_665
O1 U1 O5 89.8(2) . 2_755
O2 U1 O5 89.54(19) . 2_755
O3 U1 O5 71.33(15) . 2_755
O8 U1 O5 143.22(15) 2_665 2_755
O1 U1 O4 90.86(16) . .
O2 U1 O4 90.06(16) . .
O3 U1 O4 143.49(16) . .
O8 U1 O4 144.37(16) 2_665 .
O5 U1 O4 72.30(15) 2_755 .
O1 U1 O7 91.4(2) . .
O2 U1 O7 89.9(2) . .
O3 U1 O7 145.36(15) . .
O8 U1 O7 73.60(15) 2_665 .
O5 U1 O7 143.16(14) 2_755 .
O4 U1 O7 70.87(15) . .
O6 S1 O4 114.5(3) . .
O6 S1 O5 116.1(3) . .
O4 S1 O5 111.2(3) . .
O6 S1 C8 106.9(4) . .
O4 S1 C8 103.7(3) . .
O5 S1 C8 102.9(3) . .
O9 S2 O7 115.1(3) . .
O9 S2 O8 115.8(3) . .
O7 S2 O8 112.1(3) . .
O9 S2 C9 105.7(3) . .
O7 S2 C9 103.8(3) . .
O8 S2 C9 102.5(3) . .
C1 O3 U1 133.2(4) . .
S1 O4 U1 149.5(3) . .
S1 O5 U1 137.5(3) . 2_755
S2 O7 U1 155.5(3) . .
S2 O8 U1 146.6(3) . 2_665
O3 C1 C2 123.4(6) . .
O3 C1 H1 118.3 . .
C2 C1 H1 118.3 . .
C7 C2 C3 120.2(7) . .
C7 C2 C1 118.2(6) . .
C3 C2 C1 121.7(6) . .
C4 C3 C2 118.7(6) . .
C4 C3 H3 120.6 . .
C2 C3 H3 120.6 . .
C3 C4 C5 121.5(7) . .
C3 C4 H4 119.3 . .
C5 C4 H4 119.3 . .
C6 C5 C4 119.7(7) . .
C6 C5 H5 120.2 . .
C4 C5 H5 120.2 . .
C5 C6 C7 119.9(6) . .
C5 C6 H6 120.1 . .
C7 C6 H6 120.1 . .
C6 C7 C2 120.0(6) . .
C6 C7 H7 120.0 . .
C2 C7 H7 120.0 . .
F2 C8 F3 109.5(7) . .
F2 C8 F1 109.5(7) . .
F3 C8 F1 109.3(7) . .
F2 C8 S1 109.5(6) . .
F3 C8 S1 110.1(6) . .
F1 C8 S1 108.9(6) . .
F6 C9 F4 109.2(6) . .
F6 C9 F5 109.8(6) . .
F4 C9 F5 108.3(6) . .
F6 C9 S2 110.6(5) . .
F4 C9 S2 109.7(5) . .
F5 C9 S2 109.2(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.739(4) .
U1 O2 1.747(4) .
U1 O3 2.391(4) .
U1 O8 2.408(4) 2_665
U1 O5 2.409(5) 2_755
U1 O4 2.410(4) .
U1 O7 2.413(5) .
S1 O6 1.412(4) .
S1 O4 1.453(4) .
S1 O5 1.469(5) .
S1 C8 1.835(9) .
S2 O9 1.419(5) .
S2 O7 1.448(5) .
S2 O8 1.465(4) .
S2 C9 1.831(7) .
O3 C1 1.248(8) .
O5 U1 2.409(5) 2_755
O8 U1 2.408(4) 2_665
F1 C8 1.316(8) .
F2 C8 1.305(9) .
F3 C8 1.308(9) .
F4 C9 1.313(7) .
F5 C9 1.314(10) .
F6 C9 1.310(9) .
C1 C2 1.433(9) .
C1 H1 0.9500 .
C2 C7 1.390(9) .
C2 C3 1.405(9) .
C3 C4 1.363(10) .
C3 H3 0.9500 .
C4 C5 1.396(10) .
C4 H4 0.9500 .
C5 C6 1.376(10) .
C5 H5 0.9500 .
C6 C7 1.386(10) .
C6 H6 0.9500 .
C7 H7 0.9500 .
