#------------------------------------------------------------------------------
#$Date: 2019-10-28 09:27:44 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219813 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/46/4514629.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_4514629
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            'C32 H24 F12 O20 S4 U2'
_chemical_formula_weight         1560.81
_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                102.634(4)
_cell_angle_beta                 94.632(5)
_cell_angle_gamma                96.374(5)
_cell_formula_units_Z            1
_cell_length_a                   5.6883(4)
_cell_length_b                   12.7612(11)
_cell_length_c                   16.5764(15)
_cell_measurement_reflns_used    63633
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.30
_cell_volume                     1160.02(17)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'2 φ and 12 ω scans with 2° steps (768 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  0.0622
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            63633
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.300
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.274
_exptl_absorpt_correction_T_max  0.559
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.234
_exptl_crystal_description       platelet
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.465
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0193P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4109
_reflns_number_total             4388
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cs9b01408_si_002.cif
_cod_data_source_block           27
_cod_database_code               4514629
_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 0.93849(2) 0.88179(2) 0.81547(2) 0.02587(6) Uani 1 1 d . .
S1 S 0.81393(16) 0.85396(7) 1.02963(7) 0.0259(2) Uani 1 1 d . .
S2 S 0.78729(17) 0.76002(7) 0.59899(7) 0.0279(2) Uani 1 1 d . .
O1 O 1.1999(4) 0.8290(2) 0.8416(2) 0.0308(7) Uani 1 1 d . .
O2 O 0.6746(4) 0.9316(2) 0.78656(19) 0.0284(7) Uani 1 1 d . .
O3 O 0.7054(4) 0.7102(2) 0.81430(18) 0.0321(7) Uani 1 1 d . .
O4 O 1.1360(4) 0.99157(19) 0.73411(18) 0.0296(6) Uani 1 1 d . .
O5 O 0.8086(4) 0.88505(19) 0.95002(17) 0.0306(6) Uani 1 1 d . .
O6 O 0.8987(5) 0.9451(2) 1.0978(2) 0.0374(7) Uani 1 1 d . .
O7 O 0.9104(4) 0.7570(2) 1.0328(2) 0.0395(8) Uani 1 1 d . .
O8 O 0.9294(4) 0.7706(2) 0.68064(18) 0.0306(6) Uani 1 1 d . .
O9 O 0.5380(4) 0.7551(2) 0.60545(19) 0.0338(7) Uani 1 1 d . .
O10 O 0.8895(5) 0.8291(2) 0.5507(2) 0.0350(7) Uani 1 1 d . .
F1 F 0.3862(4) 0.90933(16) 1.03367(17) 0.0365(6) Uani 1 1 d . .
F2 F 0.4744(4) 0.80807(18) 1.11730(16) 0.0379(6) Uani 1 1 d . .
F3 F 0.4004(4) 0.73919(17) 0.98573(17) 0.0376(6) Uani 1 1 d . .
F4 F 0.7472(4) 0.55249(17) 0.59062(17) 0.0411(6) Uani 1 1 d . .
F5 F 0.7167(5) 0.59432(19) 0.47135(17) 0.0446(6) Uani 1 1 d . .
F6 F 1.0612(4) 0.61582(18) 0.54315(17) 0.0429(6) Uani 1 1 d . .
C1 C 0.5086(7) 0.6664(3) 0.7779(3) 0.0312(10) Uani 1 1 d . .
H1 H 0.4429 0.6945 0.7339 0.037 Uiso 1 1 calc R U
C2 C 0.3729(7) 0.5749(3) 0.7985(3) 0.0310(10) Uani 1 1 d . .
C3 C 0.4624(7) 0.5283(3) 0.8615(3) 0.0326(10) Uani 1 1 d . .
H3 H 0.6163 0.5547 0.8901 0.039 Uiso 1 1 calc R U
C4 C 0.3248(8) 0.4438(3) 0.8815(3) 0.0395(11) Uani 1 1 d . .
H4 H 0.3841 0.4117 0.9242 0.047 Uiso 1 1 calc R U
C5 C 0.0996(8) 0.4050(3) 0.8394(3) 0.0456(13) Uani 1 1 d . .
H5 H 0.0060 0.3466 0.8535 0.055 Uiso 1 1 calc R U
C6 C 0.0118(8) 0.4510(3) 0.7775(3) 0.0442(12) Uani 1 1 d . .
H6 H -0.1427 0.4250 0.7492 0.053 Uiso 1 1 calc R U
C7 C 0.1505(7) 0.5354(3) 0.7565(3) 0.0358(10) Uani 1 1 d . .
H7 H 0.0918 0.5663 0.7130 0.043 Uiso 1 1 calc R U
C8 C 1.2832(6) 0.9834(3) 0.6829(3) 0.0281(9) Uani 1 1 d . .
H8 H 1.3226 0.9136 0.6594 0.034 Uiso 1 1 calc R U
C9 C 1.3977(6) 1.0759(3) 0.6573(3) 0.0299(9) Uani 1 1 d . .
C10 C 1.3334(6) 1.1786(3) 0.6843(3) 0.0311(9) Uani 1 1 d . .
H10 H 1.2118 1.1894 0.7201 0.037 Uiso 1 1 calc R U
C11 C 1.4471(7) 1.2647(3) 0.6587(3) 0.0398(11) Uani 1 1 d . .
H11 H 1.4027 1.3350 0.6764 0.048 Uiso 1 1 calc R U
C12 C 1.6270(7) 1.2488(3) 0.6069(3) 0.0391(11) Uani 1 1 d . .
H12 H 1.7049 1.3087 0.5897 0.047 Uiso 1 1 calc R U
C13 C 1.6943(7) 1.1466(3) 0.5800(3) 0.0404(11) Uani 1 1 d . .
H13 H 1.8179 1.1366 0.5449 0.048 Uiso 1 1 calc R U
C14 C 1.5787(6) 1.0594(3) 0.6050(3) 0.0321(10) Uani 1 1 d . .
H14 H 1.6218 0.9890 0.5867 0.038 Uiso 1 1 calc R U
C15 C 0.4982(7) 0.8261(3) 1.0429(3) 0.0302(9) Uani 1 1 d . .
C16 C 0.8323(7) 0.6221(3) 0.5477(3) 0.0355(10) 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 178.32(11) . .
O1 U1 O8 87.04(12) . .
O2 U1 O8 91.33(12) . .
O1 U1 O6 89.79(12) . 2_777
O2 U1 O6 91.77(12) . 2_777
O8 U1 O6 143.18(9) . 2_777
O1 U1 O5 91.87(11) . .
O2 U1 O5 89.17(11) . .
O8 U1 O5 143.08(9) . .
O6 U1 O5 73.66(9) 2_777 .
O1 U1 O4 92.90(10) . .
O2 U1 O4 87.05(10) . .
O8 U1 O4 73.44(9) . .
O6 U1 O4 70.10(9) 2_777 .
O5 U1 O4 143.40(9) . .
O1 U1 O3 89.86(10) . .
O2 U1 O3 89.25(10) . .
O8 U1 O3 72.95(9) . .
O6 U1 O3 143.76(9) 2_777 .
O5 U1 O3 70.14(9) . .
O4 U1 O3 146.08(10) . .
O7 S1 O6 115.5(2) . .
O7 S1 O5 116.09(17) . .
O6 S1 O5 111.53(16) . .
O7 S1 C15 105.57(16) . .
O6 S1 C15 102.98(17) . .
O5 S1 C15 103.23(18) . .
O10 S2 O9 117.94(16) . .
O10 S2 O8 113.04(18) . .
O9 S2 O8 112.67(16) . .
O10 S2 C16 106.05(18) . .
O9 S2 C16 105.25(18) . .
O8 S2 C16 99.54(19) . .
C1 O3 U1 131.9(3) . .
C8 O4 U1 138.4(2) . .
S1 O5 U1 153.40(15) . .
S1 O6 U1 165.98(18) . 2_777
S2 O8 U1 135.02(14) . .
O3 C1 C2 123.9(4) . .
O3 C1 H1 118.1 . .
C2 C1 H1 118.1 . .
C7 C2 C3 120.1(4) . .
C7 C2 C1 119.1(4) . .
C3 C2 C1 120.8(4) . .
C4 C3 C2 119.2(4) . .
C4 C3 H3 120.4 . .
C2 C3 H3 120.4 . .
C3 C4 C5 120.4(5) . .
C3 C4 H4 119.8 . .
C5 C4 H4 119.8 . .
C6 C5 C4 120.3(4) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
C5 C6 C7 119.5(5) . .
C5 C6 H6 120.2 . .
C7 C6 H6 120.2 . .
C2 C7 C6 120.4(4) . .
C2 C7 H7 119.8 . .
C6 C7 H7 119.8 . .
O4 C8 C9 122.6(3) . .
O4 C8 H8 118.7 . .
C9 C8 H8 118.7 . .
C10 C9 C14 120.6(3) . .
C10 C9 C8 121.3(3) . .
C14 C9 C8 118.1(3) . .
C11 C10 C9 119.6(3) . .
C11 C10 H10 120.2 . .
C9 C10 H10 120.2 . .
C10 C11 C12 120.1(4) . .
C10 C11 H11 120.0 . .
C12 C11 H11 120.0 . .
C13 C12 C11 120.9(3) . .
C13 C12 H12 119.5 . .
C11 C12 H12 119.5 . .
C14 C13 C12 119.2(3) . .
C14 C13 H13 120.4 . .
C12 C13 H13 120.4 . .
C13 C14 C9 119.6(3) . .
C13 C14 H14 120.2 . .
C9 C14 H14 120.2 . .
F2 C15 F3 109.1(3) . .
F2 C15 F1 109.3(3) . .
F3 C15 F1 108.7(4) . .
F2 C15 S1 110.2(3) . .
F3 C15 S1 109.1(2) . .
F1 C15 S1 110.3(2) . .
F6 C16 F4 108.9(3) . .
F6 C16 F5 109.4(3) . .
F4 C16 F5 108.2(4) . .
F6 C16 S2 110.4(3) . .
F4 C16 S2 109.8(3) . .
F5 C16 S2 110.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.760(3) .
U1 O2 1.765(3) .
U1 O8 2.364(3) .
U1 O6 2.397(3) 2_777
U1 O5 2.399(2) .
U1 O4 2.401(2) .
U1 O3 2.426(2) .
S1 O7 1.418(2) .
S1 O6 1.440(3) .
S1 O5 1.458(3) .
S1 C15 1.832(4) .
S2 O10 1.424(3) .
S2 O9 1.426(2) .
S2 O8 1.491(3) .
S2 C16 1.834(4) .
O3 C1 1.239(5) .
O4 C8 1.236(4) .
O6 U1 2.397(3) 2_777
F1 C15 1.328(4) .
F2 C15 1.318(4) .
F3 C15 1.325(5) .
F4 C16 1.329(4) .
F5 C16 1.334(5) .
F6 C16 1.321(4) .
C1 C2 1.447(5) .
C1 H1 0.9500 .
C2 C7 1.379(6) .
C2 C3 1.398(6) .
C3 C4 1.377(5) .
C3 H3 0.9500 .
C4 C5 1.392(7) .
C4 H4 0.9500 .
C5 C6 1.376(7) .
C5 H5 0.9500 .
C6 C7 1.387(5) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 C9 1.446(5) .
C8 H8 0.9500 .
C9 C10 1.388(5) .
C9 C14 1.404(5) .
C10 C11 1.377(5) .
C10 H10 0.9500 .
C11 C12 1.392(5) .
C11 H11 0.9500 .
C12 C13 1.389(5) .
C12 H12 0.9500 .
C13 C14 1.387(5) .
C13 H13 0.9500 .
C14 H14 0.9500 .
