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_1563141
_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         'C32 H64 N3 Si6 U, C18 H36 K N2 O6'
_chemical_formula_sum            'C50 H100 K N5 O6 Si6 U'
_chemical_formula_weight         1313.01
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-08-11
_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                90
_cell_angle_beta                 93.6596(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.66789(14)
_cell_length_b                   17.47136(16)
_cell_length_c                   24.16489(19)
_cell_measurement_reflns_used    20811
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5720
_cell_measurement_theta_min      3.1120
_cell_volume                     6601.39(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.78a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.78a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.78a (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 2018/2 (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 0.997
_diffrn_measured_fraction_theta_max 0.975
_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   -112.00 -78.00   1.00    4.00    --  -40.91 -55.00 -59.00   34
  2  \w    -69.00  30.00   1.00    4.00    --  -40.91  55.00  83.00   99
  3  \w     50.00  96.00   1.00    4.00    --   40.91  55.00  83.00   46
  4  \w     -6.00  35.00   1.00    4.00    --   40.91 -55.00 -59.00   41
  5  \w     97.00 175.00   1.00   16.00    --  105.15  55.00  83.00   78
  6  \w     39.00 130.00   1.00   16.00    --  105.15 -55.00 -59.00   91
  7  \w    -20.00  73.00   1.00    4.00    --   40.91 -77.00-120.00   93
  8  \w     49.00  97.00   1.00    4.00    --   40.91-125.00-150.00   48
  9  \w    133.00 160.00   1.00   16.00    --  105.15  30.00-180.00   27
 10  \w     32.00 131.00   1.00   16.00    --  105.15 -45.00 150.00   99
 11  \w     25.00 154.00   1.00   16.00    --  105.15 -15.00 -90.00  129
 12  \w    135.00 162.00   1.00   16.00    --  105.15 111.00-120.00   27
 13  \w     98.00 129.00   1.00   16.00    --  105.15  30.00-180.00   31
 14  \w    119.00 172.00   1.00   16.00    --  105.15 111.00   0.00   53
;
_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      0.0191395000
_diffrn_orient_matrix_UB_12      -0.0569694000
_diffrn_orient_matrix_UB_13      0.0478599000
_diffrn_orient_matrix_UB_21      0.0905869000
_diffrn_orient_matrix_UB_22      -0.0125961000
_diffrn_orient_matrix_UB_23      -0.0196688000
_diffrn_orient_matrix_UB_31      0.0338716000
_diffrn_orient_matrix_UB_32      0.0660628000
_diffrn_orient_matrix_UB_33      0.0374433000
_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  0.0210
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33861
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.677
_diffrn_reflns_theta_min         3.123
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.875
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.291
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.41.78a (Rigaku Oxford Diffraction, 2020)
 Numerical absorption correction based on Gaussian integration over
 a multifaceted crystal model.
 Empirical absorption correction using spherical harmonics
 as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       plate
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.943
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         12806
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+12.4631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11775
_reflns_number_total             12806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00668a2.cif
_cod_data_source_block           dkm246
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               1563141
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C50 H100 K N5 O6 Si6 U'
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.270
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. 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
2. Uiso/Uaniso restraints and constraints
K1 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim N4 \\sim N5
\\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40
\\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48
\\sim C49 \\sim C50: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
3.a Secondary CH2 refined with riding coordinates:
 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), C49(H49A,H49B), C50(H50A,H50B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14)
3.c Idealised Me refined as rotating group:
 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), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              37236
_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 1.439
_oxdiff_exptl_absorpt_empirical_full_min 0.738