Single metal four-electron reduction by U(ii) and masked "U(ii)" compounds.
Modder, Dieuwertje K.; Palumbo, Chad T.; Douair, Iskander; Scopelliti, Rosario; Maron, Laurent; Mazzanti, Marinella; Chemical science 12 (2021) 6153–6158; doi:10.1039/d1sc00668a

data_1563143
_publ_section_title
;
 Single metal four-electron reduction by U(ii) and masked
 &quot;U(ii)&quot; compounds.
;
_journal_issue                   17
_journal_name_full               'Chemical science'
_journal_page_first              6153
_journal_page_last               6158
_journal_paper_doi               10.1039/d1sc00668a
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C30 H64 N5 Si6 U, C18 H36 K N2 O6'
_chemical_formula_sum            'C48 H100 K N7 O6 Si6 U'
_chemical_formula_weight         1317.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-10-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-03-26 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                103.478(4)
_cell_angle_beta                 101.463(3)
_cell_angle_gamma                90.908(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4770(3)
_cell_length_b                   16.6790(8)
_cell_length_c                   19.0067(8)
_cell_measurement_reflns_used    12607
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.6540
_cell_measurement_theta_min      3.9160
_cell_volume                     3460.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 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 0.972
_diffrn_measured_fraction_theta_max 0.947
_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   -113.00 -13.00   1.00    4.00    --  -40.91 -57.00 -65.00  100
  2  \w    -55.00  31.00   1.00    4.00    --  -40.91  57.00  76.00   86
  3  \w     -5.00  20.00   1.00    4.00    --   40.91 -57.00 -65.00   25
  4  \w     73.00 100.00   1.00    4.00    --   40.91  57.00  76.00   27
  5  \w     32.00 129.00   1.00   16.00    --  105.15 -57.00 -65.00   97
  6  \w     87.00 177.00   1.00   16.00    --  105.15  57.00  76.00   90
  7  \w    -65.00  33.00   1.00    4.00    --  -40.91  38.00-120.00   98
  8  \w    -80.00  -9.00   1.00    4.00    --  -40.91 125.00  90.00   71
  9  \w     59.00  90.00   1.00    4.00    --   40.91-125.00-120.00   31
 10  \w     34.00 107.00   1.00   16.00    --  105.15-111.00 -90.00   73
 11  \w    109.00 136.00   1.00   16.00    --  105.15 -15.00  60.00   27
 12  \w     31.00 108.00   1.00   16.00    --  105.15-111.00 120.00   77
 13  \w     60.00  90.00   1.00   16.00    --  105.15 -15.00  60.00   30
 14  \w    104.00 132.00   1.00   16.00    --  105.15 111.00 120.00   28
 15  \w     79.00 178.00   1.00   16.00    --  105.15  45.00  30.00   99
 16  \w     79.00 106.00   1.00   16.00    --  105.15 -94.00   0.00   27
 17  \w    104.00 171.00   1.00   16.00    --  105.15  77.00 -60.00   67
 18  \w    104.00 132.00   1.00   16.00    --  105.15 -77.00  90.00   28
 19  \w    105.00 147.00   1.00   16.00    --  105.15  45.00 -90.00   42
 20  \w     24.00  75.00   1.00   16.00    --  105.15 -94.00 -60.00   51
 21  \w     24.00  58.00   1.00   16.00    --  105.15 -15.00  60.00   34
 22  \w     70.00 109.00   1.00   16.00    --  105.15-111.00   0.00   39
 23  \w    117.00 178.00   1.00   16.00    --  105.15  77.00 -30.00   61
 24  \w     29.00 106.00   1.00   16.00    --  105.15 -94.00 150.00   77
;
_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      0.0505621000
_diffrn_orient_matrix_UB_12      -0.0624842000
_diffrn_orient_matrix_UB_13      -0.0579272000
_diffrn_orient_matrix_UB_21      0.0864268000
_diffrn_orient_matrix_UB_22      0.0687856000
_diffrn_orient_matrix_UB_23      -0.0055550000
_diffrn_orient_matrix_UB_31      0.0938757000
_diffrn_orient_matrix_UB_32      -0.0205962000
_diffrn_orient_matrix_UB_33      0.0622523000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14136
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.725
_diffrn_reflns_theta_min         3.938
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.476
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.158
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.112
_refine_diff_density_max         5.937
_refine_diff_density_min         -5.122
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         14136
_refine_ls_number_restraints     934
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.1069
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1197P)^2^+86.4352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2799
_refine_ls_wR_factor_ref         0.2818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13270
_reflns_number_total             14136
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -175.1076\% 
around [0.95 -0.02 -0.31] (reciprocal) or [1.00 0.00 0.00] (direct)
;
_cod_data_source_file            d1sc00668a2.cif
_cod_data_source_block           dkm297_sq
_cod_original_cell_volume        3460.2(3)
_cod_database_code               1563143
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C52 H108 N7 O7 Si6 K1 U1'
_shelx_estimated_absorpt_t_max   0.450
_shelx_estimated_absorpt_t_min   0.202
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.658(3)
 0.342(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C31-C32 \\sim C34-C33 \\sim C36-C35 \\sim C48-C47 \\sim C46-C45 \\sim C44-C43
\\sim C37-C38 \\sim C40-C39
 \\sim C42-C41
 with sigma of 0.02
 Si6-C28 \\sim Si6-C29 \\sim Si6-C30 \\sim Si5-C26 \\sim Si5-C25 \\sim Si5-C27
\\sim Si3-C20 \\sim Si3-C21
 \\sim Si3-C19 \\sim Si4-C24 \\sim Si4-C22 \\sim Si4-C23 \\sim Si2-C16 \\sim
Si2-C18 \\sim Si2-C17 \\sim Si1-
 C14 \\sim Si1-C15 \\sim Si1-C13
 with sigma of 0.02
 O3-C39 \\sim O3-C38 \\sim O4-C40 \\sim O4-C41 \\sim O2-C34 \\sim O2-C35 \\sim
O6-C47 \\sim O6-C46 \\sim O5-
 C45 \\sim O5-C44 \\sim O1-C32 \\sim O1-C33
 with sigma of 0.02
 N1-C1 \\sim N2-C7
 with sigma of 0.02
 N7-C42 \\sim N7-C36 \\sim N7-C48 \\sim N6-C31 \\sim N6-C37 \\sim N6-C43
 with sigma of 0.02
 Si4-N4 \\sim Si3-N4 \\sim Si1-N3 \\sim Si2-N3 \\sim Si5-N5 \\sim Si6-N5
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C12(H12), C11(H11), C10(H10), C9(H9),
 C8(H8)
5.c Fitted hexagon refined as free rotating group:
 C1(C6,C5,C4,C3,C2), C7(C12,C11,C10,C9,C8)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              53121
_shelx_fab_checksum              35120
_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 4.403
_oxdiff_exptl_absorpt_empirical_full_min 0.486
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2