Synthesis, structure and redox properties of single-atom bridged diuranium complexes supported by aryloxides.
Hsueh, Fang-Che; Barluzzi, Luciano; Rajeshkumar, Thayalan; Scopelliti, Rosario; Zivkovic, Ivica; Maron, Laurent; Mazzanti, Marinella; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13416–13426; doi:10.1039/d4dt01819b

data_7716710
_publ_section_title
;
 Synthesis, structure and redox properties of single-atom bridged
 diuranium complexes supported by aryloxides.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13416
_journal_page_last               13426
_journal_paper_doi               10.1039/d4dt01819b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C84 H126 O7 U2, 2(C22 H44 K N2 O7), 1(C12 H10 N2), 4[C4H8O]'
_chemical_formula_sum            'C156 H256 K2 N6 O25 U2'
_chemical_formula_weight         3170.052
_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_Int_Tables_number      2
_audit_creation_date             2024-02-29
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-12 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                77.156(5)
_cell_angle_beta                 66.138(5)
_cell_angle_gamma                82.519(5)
_cell_formula_units_Z            1
_cell_length_a                   15.1585(8)
_cell_length_b                   16.4391(10)
_cell_length_c                   18.5969(10)
_cell_measurement_reflns_used    9267
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.4850
_cell_measurement_theta_min      3.1690
_cell_volume                     4127.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.105a 64-bit (release 11-01-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9499
_diffrn_measured_fraction_theta_max 0.9179
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -57.00  25.00   1.00    7.50    --  -40.91  72.00-101.00   82
  2  \w     33.00 136.00   1.00   30.00    --  105.78 -72.00 128.00  103
  3  \w    138.00 165.00   1.00   30.00    --  105.78  72.00-101.00   27
  4  \w    109.00 136.00   1.00   30.00    --  105.78  72.00-101.00   27
  5  \w    -69.00  31.00   1.00    7.50    --  -40.91  57.00  30.00  100
  6  \w    -63.00  31.00   1.00    7.50    --  -40.91  38.00-150.00   94
  7  \w    -64.00  17.00   1.00    7.50    --  -40.91  38.00 150.00   81
  8  \w     33.00  63.00   1.00    7.50    --   40.91 -77.00  30.00   30
  9  \w    -21.00  17.00   1.00    7.50    --   40.91 -77.00  30.00   38
 10  \w     34.00  61.00   1.00    7.50    --   40.91 -72.00 128.00   27
 11  \w     44.00  69.00   1.00    7.50    --   40.91 -77.00-120.00   25
 12  \w    -21.00   5.00   1.00    7.50    --   40.91 -77.00-120.00   26
 13  \w    150.00 177.00   1.00   30.00    --  105.78  77.00  30.00   27
 14  \w     57.00 109.00   1.00   30.00    --  105.78-108.00  16.76   52
 15  \w     79.00 107.00   1.00   30.00    --  105.78-111.00  90.00   28
 16  \w    106.00 133.00   1.00   30.00    --  105.78  77.00  30.00   27
 17  \w     33.00 108.00   1.00   30.00    --  105.78-111.00 150.00   75
 18  \w     38.00 134.00   1.00   30.00    --  105.78 -30.00 -90.00   96
 19  \w     80.00 105.00   1.00   30.00    --  105.78-111.00-120.00   25
 20  \w     24.00 104.00   1.00   30.00    --  105.78 -94.00 -60.00   80
 21  \w    105.00 175.00   1.00   30.00    --  105.78  77.00 -60.00   70
 22  \w     45.00  71.00   1.00   30.00    --  105.78-111.00-120.00   26
 23  \w     65.00 125.00   1.00   30.00    --  105.78 -61.00 -30.00   60
 24  \w     83.00 108.00   1.00   30.00    --  105.78-111.00 -90.00   25
 25  \w     89.00 169.00   1.00   30.00    --  105.78  61.00  90.00   80
 26  \w     58.00 158.00   1.00   30.00    --  105.78 -15.00  90.00  100
 27  \w     57.00  85.00   1.00   30.00    --  105.78 -45.00 -90.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0085645000
_diffrn_orient_matrix_UB_12      -0.0243685000
_diffrn_orient_matrix_UB_13      -0.0721116000
_diffrn_orient_matrix_UB_21      -0.0492123000
_diffrn_orient_matrix_UB_22      0.0859122000
_diffrn_orient_matrix_UB_23      -0.0170686000
_diffrn_orient_matrix_UB_31      0.0996112000
_diffrn_orient_matrix_UB_32      0.0356428000
_diffrn_orient_matrix_UB_33      -0.0550327000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.9499
_diffrn_reflns_Laue_measured_fraction_max 0.9179
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31475
_diffrn_reflns_point_group_measured_fraction_full 0.9499
_diffrn_reflns_point_group_measured_fraction_max 0.9179
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         73.36
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.436
_exptl_absorpt_correction_T_max  0.576
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1653.214
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.123
_refine_diff_density_max         2.6949
_refine_diff_density_min         -2.5288
_refine_diff_density_rms         0.2108
_refine_ls_d_res_high            0.8046
_refine_ls_d_res_low             13.8486
_refine_ls_goodness_of_fit_ref   1.0220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    192
_refine_ls_number_parameters     874
_refine_ls_number_reflns         15234
_refine_ls_number_restraints     295
_refine_ls_restrained_S_all      1.0117
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+22.8903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1962
_refine_ls_wR_factor_ref         0.2059
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -16
_reflns_limit_k_max              20
_reflns_limit_k_min              -19
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                12550
_reflns_number_total             15234
_reflns_threshold_expression     I>=2u(I)
_twin_special_details
;
Component 2 rotated by 9.2479\% 
around [-0.74 -0.53 -0.42] (reciprocal) or [-0.88 -0.47 0.03] (direct)
;
_cod_data_source_file            d4dt01819b2.cif
_cod_data_source_block           ah719
_cod_depositor_comments
'Adding full bibliography for 7716706--7716710.cif.'
_cod_database_code               7716710
_chemical_oxdiff_formula         'C160 H264 N6 O26 K2 U2'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C65-C64
 2.4 with sigma of 0.02
 C62-C61 \\sim C62-C63 \\sim C63-C64 \\sim C65-C61 \\sim C66-C65 \\sim C66-C64
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O10 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C73 \\sim N4 \\sim C78 \\sim C74 \\sim C77 \\sim C75 \\sim C76 \\sim C67 \\sim
N3 \\sim C72 \\sim C68 \\sim C71 \\sim C69 \\sim C70: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
4. Others
 Sof(N4)=Sof(C73)=Sof(C78)=Sof(H78)=Sof(C77)=Sof(H77)=Sof(C76)=Sof(H76)=
 Sof(C75)=Sof(H75)=Sof(C74)=Sof(H74)=1-FVAR(1)
 Sof(N3)=Sof(C67)=Sof(C72)=Sof(H72)=Sof(C71)=Sof(H71)=Sof(C70)=Sof(H70)=
 Sof(C69)=Sof(H69)=Sof(C68)=Sof(H68)=FVAR(1)
 Sof(H61c)=Sof(H61d)=Sof(H64c)=Sof(H64d)=Sof(C65)=Sof(H65a)=Sof(H65b)=Sof(C66)=
 Sof(H66a)=Sof(H66b)=1-FVAR(2)
 Sof(H61a)=Sof(H61b)=Sof(C62)=Sof(H62a)=Sof(H62b)=Sof(C63)=Sof(H63a)=Sof(H63b)=
 Sof(H64a)=Sof(H64b)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C43(H43a,H43b), C44(H44a,H44b), C45(H45a,H45b), C46(H46a,H46b), C47(H47a,
 H47b), C48(H48a,H48b), C49(H49a,H49b), C50(H50a,H50b), C51(H51a,H51b),
 C52(H52a,H52b), C53(H53a,H53b), C54(H54a,H54b), C55(H55a,H55b), C56(H56a,H56b),
  C57(H57a,H57b), C58(H58a,H58b), C59(H59a,H59b), C60(H60a,H60b), C61(H61a,
 H61b), C61(H61c,H61d), C62(H62a,H62b), C63(H63a,H63b), C64(H64a,H64b),
 C64(H64c,H64d), C65(H65a,H65b), C66(H66a,H66b)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C17(H17), C18(H18), C19(H19), C31(H31), C32(H32),
 C33(H33), C72(H72), C71(H71), C70(H70), C69(H69), C68(H68), C78(H78), C77(H77),
  C76(H76), C75(H75), C74(H74)
5.c Fitted hexagon refined as free rotating group:
 C67(C72,C71,C70,C69,C68), C73(C78,C77,C76,C75,C74)
5.d Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c), C12(H12a,H12b,H12c),
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C22(H22a,H22b,H22c), C23(H23a,H23b,
 H23c), C24(H24a,H24b,H24c), C26(H26a,H26b,H26c), C27(H27a,H27b,H27c), C28(H28a,
 H28b,H28c), C36(H36a,H36b,H36c), C37(H37a,H37b,H37c), C38(H38a,H38b,H38c),
 C40(H40a,H40b,H40c), C41(H41a,H41b,H41c), C42(H42a,H42b,H42c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 166 electrons were 
found in a volume of 939\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
4[C4H8O] per Asymmetric Unit 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 5.394
_oxdiff_exptl_absorpt_empirical_full_min 0.162
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2