Catalytic one-electron reduction of uranyl(VI) to Group 1 uranyl(V) complexes via Al(III) coordination
Markus Zegke; Gary S. Nichol; Polly L. Arnold; Jason B. Love; Chem.Commun. 51 (2015) 5876–; doi:10.1039/C5cc00867K

data_7116859
_publ_section_title
;
 Catalytic one-electron reduction of uranyl(VI) to Group 1 uranyl(V)
 complexes via Al(III) coordination
;
_journal_name_full               Chem.Commun.
_journal_page_first              5876
_journal_paper_doi               10.1039/C5cc00867K
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety
'C59.39 H59.39 Li0.87 N11.48 O2 U, 5(C5 H5 N)'
_chemical_formula_sum            'C84.47 H84.47 Li0.87 N16.49 O2 U'
_chemical_formula_weight         1606.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2015-01-29 deposited with the CCDC.
2015-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.634(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2782(5)
_cell_length_b                   24.4176(6)
_cell_length_c                   22.8717(7)
_cell_measurement_reflns_used    18855
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      29.0870
_cell_measurement_theta_min      3.7290
_cell_volume                     7973.5(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean 8.0521
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -90.00   21.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9205  -19.0000   60.0000 222

  2 omega  -25.00   22.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9205  -99.0000    0.0000 94

  3 omega  -89.00    1.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9205  -57.0000    0.0000 180

  4 omega   34.00   98.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6393  179.0000  150.0000 128

  5 omega   32.00   98.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6393 -179.0000    0.0000 132

  6 omega    0.00   90.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6393   57.0000  -90.0000 180

  7 omega  -51.00   -1.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6393  -38.0000  120.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0488903000
_diffrn_orient_matrix_UB_12      -0.0050372000
_diffrn_orient_matrix_UB_13      0.0012450000
_diffrn_orient_matrix_UB_21      -0.0044907000
_diffrn_orient_matrix_UB_22      -0.0105102000
_diffrn_orient_matrix_UB_23      0.0287681000
_diffrn_orient_matrix_UB_31      -0.0074406000
_diffrn_orient_matrix_UB_32      -0.0265973000
_diffrn_orient_matrix_UB_33      -0.0115919000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0922
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41408
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.020
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       prism
_exptl_crystal_F_000             3269
_exptl_crystal_size_max          0.9171
_exptl_crystal_size_mid          0.5792
_exptl_crystal_size_min          0.3542
_refine_diff_density_max         1.254
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.369(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     960
_refine_ls_number_reflns         18020
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0431P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                14162
_reflns_number_total             18020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc00867k2.cif
_cod_data_source_block           p14024
_cod_database_code               7116859
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C64 H64 Li1 N12 O2 U1'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C85-C86
 1.4 with sigma of 0.01
 U1B-O2B \\sim U1A-O2A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C78, C79, C80, C81, C82, N16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N12, C58, C59, C60, C61, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H1)=Sof(H8)=Sof(U1B)=Sof(O2B)=1-FVAR(1)
 Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=
 Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50)=
 Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=
 Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=
 Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=
 Sof(H4)=Sof(H5A)=Sof(N9)=Sof(N11)=Sof(N10)=Sof(N12)=Sof(O2A)=Sof(U1A)=Sof(Li1)=
 FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C12(H12), C14(H14), C16(H16), C17(H17),
 C23(H23), C24(H24), C26(H26), C28(H28), C33(H33), C35(H35), C37(H37), C38(H38),
  C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49),
 C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C68(H68), C69(H69),
 C70(H70), C71(H71), C72(H72), C83(H83), C1B(H1B), C1A(H1A), C86(H86), C85(H85),
  C82(H82), C81(H81), C80(H80), C79(H79), C78(H78), C77(H77), C76(H76),
 C75(H75), C74(H74), C73(H73), N1(H1), N4(H4), N5(H5A), N8(H8), C63(H63),
 C64(H64), C65(H65), C66(H66), C67(H67)
5.b Fitted hexagon refined as free rotating group:
 C83(C1B,C1A,C86,C85,N84), C82(C81,C80,C79,C78,N16), N13(C63,C64,C65,C66,C67)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C)
;
_shelx_res_checksum              51269
_shelx_hkl_checksum              65830
_olex2_submission_special_instructions 'No special instructions were received'