Leveraging a reduced polyoxomolybdate-alkoxide cluster for the formation of a stable U(v) sandwich complex.
Shiels, Dominic; Brennessel, William W.; Crawley, Matthew R.; Matson, Ellen M.; Chemical science 15 (2024) 11072–11083; doi:10.1039/d4sc02644f

data_1571930
_publ_section_title
;
 Leveraging a reduced polyoxomolybdate-alkoxide cluster for the formation
 of a stable U(v) sandwich complex.
;
_journal_issue                   28
_journal_name_full               'Chemical science'
_journal_page_first              11072
_journal_page_last               11083
_journal_paper_doi               10.1039/d4sc02644f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety
'C8 H24 Mo10 N2 O36 U, C16 H36 N, 2.609(C H2 Cl2)'
_chemical_formula_sum            'C26.61 H65.22 Cl5.22 Mo10 N3 O36 U'
_chemical_formula_weight         2385.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-04-14
_audit_creation_method
;
Olex2 1.5-ac6-015
(compiled 2023.12.04 svn.r209d9fb2 for Rigaku Oxford Diffraction, GUI svn.r6873)
;
_audit_update_record
;
2024-04-19 deposited with the CCDC.	2024-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.3130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.31000(10)
_cell_length_b                   21.22060(10)
_cell_length_c                   18.90170(10)
_cell_measurement_reflns_used    66863
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      80.2190
_cell_measurement_theta_min      3.1690
_cell_volume                     6366.22(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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    -35.00  25.00   0.50    0.34    --  -47.28  41.00-167.00  120
  2  \w   -120.00 -35.00   0.50    0.34    --  -47.28 -41.00  39.00  170
  3  \w     35.00 120.00   0.50    0.34    --   47.28  41.00-167.00  170
  4  \w    -25.00  55.00   0.50    0.34    --   47.28 -41.00  39.00  160
  5  \w    101.00 178.00   0.50    1.34    --  113.25  41.00-167.00  154
  6  \w    101.00 178.00   0.50    1.34    --  113.25  41.00-167.00  154
  7  \w    -10.00  28.00   0.50    0.34    --  -47.28  19.00   0.00   76
  8  \w    -10.00  28.00   0.50    0.34    --  -47.28  19.00-120.00   76
  9  \w    -86.00 -13.00   0.50    0.34    --  -47.28 125.00 -60.00  146
 10  \w    -10.00  28.00   0.50    0.34    --  -47.28  19.00 -30.00   76
 11  \w   -164.00 -79.00   0.50    1.34    --  -91.75 -41.00  39.00  170
 12  \w    -63.00 -19.00   0.50    1.34    --  -91.75  61.00  30.00   88
 13  \w    -63.00 -19.00   0.50    1.34    --  -91.75  61.00   0.00   88
 14  \w     42.00  83.00   0.50    1.34    --  113.25 -61.00-180.00   82
 15  \w     42.00  83.00   0.50    1.34    --  113.25 -61.00 -90.00   82
 16  \w     42.00 106.00   0.50    1.34    --  113.25 -94.00  90.00  128
 17  \w     42.00  83.00   0.50    1.34    --  113.25 -61.00  90.00   82
 18  \w     42.00  83.00   0.50    1.34    --  113.25 -61.00-120.00   82
 19  \w     42.00  83.00   0.50    1.34    --  113.25 -61.00  30.00   82
 20  \w     95.00 178.00   0.50    1.34    --  113.25 125.00  90.00  166
 21  \w     42.00  83.00   0.50    1.34    --  113.25 -61.00 120.00   82
 22  \w     44.00 111.00   0.50    1.34    --  113.25-125.00   0.00  134
 23  \w     42.00  83.00   0.50    1.34    --  113.25 -61.00  60.00   82
 24  \w     95.00 178.00   0.50    1.34    --  113.25 125.00  90.00  166
 25  \w     97.00 178.00   0.50    1.34    --  113.25  61.00 150.00  162
 26  \w     42.00 106.00   0.50    1.34    --  113.25 -94.00  30.00  128
 27  \w    101.00 178.00   0.50    1.34    --  113.25  30.00 -30.00  154
 28  \w    101.00 178.00   0.50    1.34    --  113.25  45.00 -90.00  154
 29  \w    101.00 178.00   0.50    1.34    --  113.25  45.00-150.00  154
 30  \w     97.00 178.00   0.50    1.34    --  113.25  61.00 120.00  162
 31  \w     42.00 106.00   0.50    1.34    --  113.25 -94.00-120.00  128
 32  \w     42.00  83.00   0.50    1.34    --  113.25 -61.00-150.00   82
 33  \w     25.00 119.00   0.50    0.34    --   47.28  77.00   0.00  188
 34  \w     25.00 119.00   0.50    0.34    --   47.28  77.00 -90.00  188
 35  \w     32.00 119.00   0.50    0.34    --   47.28  57.00-120.00  174
 36  \w     34.00  93.00   0.50    0.34    --   47.28-125.00-120.00  118
 37  \w     25.00 119.00   0.50    0.34    --   47.28  77.00 -30.00  188
 38  \w     25.00 119.00   0.50    0.34    --   47.28  77.00  90.00  188
 39  \w     41.00 115.00   0.50    1.34    --  113.25   0.00 150.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0876517000
_diffrn_orient_matrix_UB_12      0.0163560000
_diffrn_orient_matrix_UB_13      0.0472164000
_diffrn_orient_matrix_UB_21      0.0416835000
_diffrn_orient_matrix_UB_22      -0.0333771000
_diffrn_orient_matrix_UB_23      -0.0550962000
_diffrn_orient_matrix_UB_31      -0.0006636000
_diffrn_orient_matrix_UB_32      0.0623601000
_diffrn_orient_matrix_UB_33      -0.0418266000
_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  0.0566
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            109066
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.409
_diffrn_reflns_theta_min         3.180
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.413
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.118a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark yellow-green'
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.489
_exptl_crystal_description       block
_exptl_crystal_F_000             4538
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.663
_refine_diff_density_min         -1.692
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         13749
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0389
_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/[\s^2^(Fo^2^)+(0.0480P)^2^+51.8368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13207
_reflns_number_total             13749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02644f2.cif
_cod_data_source_block           matds08
_cod_depositor_comments
'Adding full bibliography for 1571928--1571932.cif.'
_cod_original_cell_volume        6366.22(6)
_cod_database_code               1571930
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.302
_shelx_estimated_absorpt_t_min   0.181
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O24-C6 \\sim O24-C6A \\sim O25-C7 \\sim O25-C7A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.2A
Uanis(C7) \\sim Ueq, Uanis(C7A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O24, C6, C6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O25, C7, C7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(Cl3')=Sof(Cl4')=Sof(C26')=
 Sof(H26C)=Sof(H26D)=1-FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(Cl3)=Sof(Cl4)=Sof(Cl5)=Sof(Cl6)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=FVAR(1)
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=1-FVAR(2)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,
 H27B), C26'(H26C,H26D)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C6A(H6AA,H6AB,
 H6AC), C7A(H7AA,H7AB,H7AC), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C20(H20A,
 H20B,H20C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              96630
_shelx_hkl_checksum              22736
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id matds08
_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 1.569
_oxdiff_exptl_absorpt_empirical_full_min 0.712