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_1563142
_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, 2(C9 H18 K0.5 N O3)'
_chemical_formula_sum            'C48 H100 K N7 O6 Si6 U'
_chemical_formula_weight         1317.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-05-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-03-26 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.9909(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.6297(5)
_cell_length_b                   23.9733(5)
_cell_length_c                   23.9063(5)
_cell_measurement_reflns_used    8692
_cell_measurement_temperature    139.9(6)
_cell_measurement_theta_max      72.5570
_cell_measurement_theta_min      6.5910
_cell_volume                     12951.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (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    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_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   -114.00 -15.00   1.00   13.50    --  -40.91 -46.00  27.00   99
  2  \w    -48.00  30.00   1.00   13.50    --  -40.91  46.00 177.00   78
  3  \w      9.00  48.00   1.00   13.50    --   40.91 -46.00  27.00   39
  4  \w     61.00 108.00   1.00   13.50    --   40.91  46.00 177.00   47
  5  \w     92.00 178.00   1.00   55.00    --  105.15  46.00 177.00   86
  6  \w     34.00 119.00   1.00   55.00    --  105.15 -46.00  27.00   85
  7  \w     28.00  95.00   1.00   13.50    --   40.91-125.00-120.00   67
  8  \w     55.00  97.00   1.00   13.50    --   40.91-125.00 -30.00   42
  9  \w     23.00 106.00   1.00   55.00    --  105.15 -94.00  30.00   83
 10  \w    151.00 177.00   1.00   55.00    --  105.15  77.00-180.00   26
 11  \w    124.00 173.00   1.00   55.00    --  105.15 111.00  60.00   49
 12  \w    104.00 165.00   1.00   55.00    --  105.15  77.00 120.00   61
 13  \w    104.00 164.00   1.00   55.00    --  105.15  77.00  90.00   60
 14  \w     47.00  99.00   1.00   55.00    --  105.15-111.00   0.00   52
;
_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      0.0593439000
_diffrn_orient_matrix_UB_12      -0.0075441000
_diffrn_orient_matrix_UB_13      -0.0278904000
_diffrn_orient_matrix_UB_21      0.0312782000
_diffrn_orient_matrix_UB_22      0.0349815000
_diffrn_orient_matrix_UB_23      0.0468162000
_diffrn_orient_matrix_UB_31      0.0120368000
_diffrn_orient_matrix_UB_32      -0.0534391000
_diffrn_orient_matrix_UB_33      0.0344833000
_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     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14444
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.788
_diffrn_reflns_theta_min         3.688
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.057
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (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            'lustrous intense black'
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       needle
_exptl_crystal_F_000             5440
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.044
_refine_diff_density_max         4.553
_refine_diff_density_min         -1.422
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         14444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.841
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0859P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1328
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7639
_reflns_number_total             14444
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 2.1669\% 
 around [0.50 -0.10 -0.86] (reciprocal) or [0.52 -0.11 -0.84] (direct)
;
_cod_data_source_file            d1sc00668a2.cif
_cod_data_source_block           dkm134
_cod_database_code               1563142
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 H100 N7 O6 Si6 K1 U1'
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.357
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.808(2)
 0.192(2)
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.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)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12)
3.c 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              76533
_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 2.530
_oxdiff_exptl_absorpt_empirical_full_min 0.618
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2