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_7716706
_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 N O6 U2, 2(O), 8[C4H8O], 1[Cs]'
_chemical_formula_sum            'C116 H190 Cs N O14 U2'
_chemical_formula_weight         2431.763
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-20 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.0671(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8121(2)
_cell_length_b                   19.1272(4)
_cell_length_c                   21.0703(4)
_cell_measurement_reflns_used    11130
_cell_measurement_temperature    173.04(14)
_cell_measurement_theta_max      72.6160
_cell_measurement_theta_min      3.0220
_cell_volume                     5858.50(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.04(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9939
_diffrn_measured_fraction_theta_max 0.9702
_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    -86.00 -33.00   1.00    5.00    --  -40.66 125.00-120.00   53
  2  \w   -119.00  -2.00   1.00    5.00    --  -40.66 -19.00 120.00  117
  3  \w    -58.00 -16.00   1.00    5.00    --  -40.66 125.00 -60.00   42
  4  \w     25.00  54.00   1.00    5.00    --   40.66  57.00 -30.00   29
  5  \w    106.00 175.00   1.00   20.00    --  105.15  77.00-120.00   69
  6  \w     23.00  83.00   1.00   20.00    --  105.15 -94.00   0.00   60
  7  \w    103.00 167.00   1.00   20.00    --  105.15  77.00 -60.00   64
  8  \w    130.00 170.00   1.00   20.00    --  105.15 111.00 -90.00   40
  9  \w     25.00 104.00   1.00   20.00    --  105.15 -94.00-120.00   79
 10  \w    121.00 158.00   1.00   20.00    --  105.15  77.00 -30.00   37
 11  \w     45.00 108.00   1.00   20.00    --  105.15-108.00 -25.00   63
 12  \w     87.00 112.00   1.00   20.00    --  105.15-125.00-107.00   25
 13  \w    104.00 174.00   1.00   20.00    --  105.15  77.00-180.00   70
 14  \w     32.00  57.00   1.00   20.00    --  105.15 -94.00  60.00   25
;
_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      -0.0071546000
_diffrn_orient_matrix_UB_12      -0.0294636000
_diffrn_orient_matrix_UB_13      0.0669009000
_diffrn_orient_matrix_UB_21      0.0051972000
_diffrn_orient_matrix_UB_22      0.0747405000
_diffrn_orient_matrix_UB_23      0.0277135000
_diffrn_orient_matrix_UB_31      -0.1056143000
_diffrn_orient_matrix_UB_32      0.0055957000
_diffrn_orient_matrix_UB_33      -0.0175736000
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.9939
_diffrn_reflns_Laue_measured_fraction_max 0.9702
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25396
_diffrn_reflns_point_group_measured_fraction_full 0.9939
_diffrn_reflns_point_group_measured_fraction_max 0.9702
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         72.76
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       prism
_exptl_crystal_F_000             2477.520
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.7075
_refine_diff_density_min         -1.9778
_refine_diff_density_rms         0.1630
_refine_ls_d_res_high            0.8072
_refine_ls_d_res_low             14.5366
_refine_ls_goodness_of_fit_ref   1.0868
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    189
_refine_ls_number_parameters     768
_refine_ls_number_reflns         11310
_refine_ls_number_restraints     828
_refine_ls_restrained_S_all      1.0465
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+26.4475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -18
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                9492
_reflns_number_total             11310
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt01819b2.cif
_cod_data_source_block           lb857
_cod_depositor_comments
'Adding full bibliography for 7716706--7716710.cif.'
_cod_database_code               7716706
_chemical_oxdiff_formula         'C116 H190 N1 O14 Cs1 U2'
_reflns_odcompleteness_completeness 99.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 O3-C29 \\sim O3-C35
 with sigma of 0.02
 C41-C36 \\sim C41-C30 \\sim C45-C34 \\sim C45-C40
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
O3 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C45: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
Cs1 \\sim O4 \\sim O7 \\sim O5 \\sim C53 \\sim C49 \\sim O9 \\sim C61 \\sim C52
\\sim C64 \\sim C56 \\sim C54 \\sim C50 \\sim C69 \\sim C72 \\sim C62 \\sim C51
\\sim C63 \\sim C55 \\sim C70 \\sim C71 \\sim O6 \\sim C57 \\sim C60 \\sim C58
\\sim C59 \\sim O8 \\sim C65 \\sim C68 \\sim C66 \\sim C67 \\sim C76 \\sim O10
\\sim C73 \\sim C74 \\sim C75: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(O9) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(O10)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C70) \\sim Ueq,
Uanis(C72) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 Cs1, O4, O7, O5, C53, C49, O9, C61, C52, C64, C56, C54, C50, C69, C72, C62,
 C51, C63, C55, C70, C71, O6, C57, C60, C58, C59, O8, C65, C68, C66, C67, C76,
 O10, C73, C74, C75
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C35)=Sof(C36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=
 Sof(C40)=1-FVAR(1)
 Sof(C29)=Sof(C30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=
 Sof(C34)=FVAR(1)
 Fixed Sof: Cs1(0.5) O5(0.5) C53(0.5) H53a(0.5) H53b(0.5) C54(0.5) H54a(0.5)
 H54b(0.5) C55(0.5) H55a(0.5) H55b(0.5) C56(0.5) H56a(0.5) H56b(0.5) O7(0.5)
 C61(0.5) H61a(0.5) H61b(0.5) C62(0.5) H62a(0.5) H62b(0.5) C63(0.5) H63a(0.5)
 H63b(0.5) C64(0.5) H64a(0.5) H64b(0.5) O9(0.5) C69(0.5) H69a(0.5) H69b(0.5)
 C70(0.5) H70a(0.5) H70b(0.5) C71(0.5) H71a(0.5) H71b(0.5) C72(0.5) H72a(0.5)
 H72b(0.5) O6(0.5) C57(0.5) H57a(0.5) H57b(0.5) C58(0.5) H58a(0.5) H58b(0.5)
 C59(0.5) H59a(0.5) H59b(0.5) C60(0.5) H60a(0.5) H60b(0.5) O8(0.5) C65(0.5)
 H65a(0.5) H65b(0.5) C66(0.5) H66a(0.5) H66b(0.5) C67(0.5) H67a(0.5) H67b(0.5)
 C68(0.5) H68a(0.5) H68b(0.5) O10(0.5) C73(0.5) H73a(0.5) H73b(0.5) C74(0.5)
 H74a(0.5) H74b(0.5) C75(0.5) H75a(0.5) H75b(0.5) C76(0.5) H76a(0.5) H76b(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C49(H49a,H49b), C50(H50a,H50b), C51(H51a,H51b), C52(H52a,H52b), C53(H53a,
 H53b), C54(H54a,H54b), C55(H55a,H55b), C56(H56a,H56b), C61(H61a,H61b),
 C62(H62a,H62b), C63(H63a,H63b), C64(H64a,H64b), C69(H69a,H69b), C70(H70a,H70b),
  C71(H71a,H71b), C72(H72a,H72b), C57(H57a,H57b), C58(H58a,H58b), C59(H59a,
 H59b), C60(H60a,H60b), C65(H65a,H65b), C66(H66a,H66b), C67(H67a,H67b),
 C68(H68a,H68b), C73(H73a,H73b), C74(H74a,H74b), C75(H75a,H75b), C76(H76a,H76b)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C14(H14), C17(H17), C18(H18), C19(H19), C31(H31), C32(H32),
 C33(H33), C37(H37), C38(H38), C39(H39)
5.c Fitted pentagon refined as free rotating group:
 O4(C49,C50,C51,C52), O5(C53,C54,C55,C56), O7(C61,C62,C63,C64), O9(C69,C70,C71,
 C72), O6(C57,C58,C59,C60), O8(C65,C66,C67,C68), O10(C73,C74,C75,C76)
5.d Fitted hexagon refined as free rotating group:
 C35(C36,C37,C38,C39,C40)
5.e Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c),
 C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C22(H22a,H22b,H22c), C23(H23a,H23b,
 H23c), C24(H24a,H24b,H24c), C26(H26a,H26b,H26c), C27(H27a,H27b,H27c), C28(H28a,
 H28b,H28c), C42(H42a,H42b,H42c), C43(H43a,H43b,H43c), C44(H44a,H44b,H44c),
 C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.290
_oxdiff_exptl_absorpt_empirical_full_min 0.836