Assembling Diuranium Complexes in Different States of Charge with a Bridging Redox-Active Ligand
Modder, dieuwertje; Batov, Mikhail; Rajeshkumar, Thayalan; Scopelliti, Rosario; Zivkovic, Ivica; Sienkiewicz, Andrzej; Maron, Laurent; Mazzanti, Marinella; Chemical Science  (2022) –; doi:10.1039/D2SC03592H

data_1567553
_publ_section_title
;
 Assembling Diuranium Complexes in Different States of Charge with a
 Bridging Redox-Active Ligand
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC03592H
_journal_year                    2022
_chemical_formula_moiety         'C44 H114 N10 Si12 U2'
_chemical_formula_sum            'C44 H114 N10 Si12 U2'
_chemical_formula_weight         1596.59
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-06-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-06-23 deposited with the CCDC.	2022-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.683(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.4164(5)
_cell_length_b                   11.4199(2)
_cell_length_c                   29.7959(6)
_cell_measurement_reflns_used    9762
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5760
_cell_measurement_theta_min      3.7770
_cell_volume                     7958.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (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 0.970
_diffrn_measured_fraction_theta_max 0.944
_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    -63.00 -38.00   1.00    4.00    --  -40.91 112.00   6.00   25
  2  \w     62.00  87.00   1.00    4.00    --   40.91-112.00 -86.00   25
  3  \w    104.00 167.00   1.00   16.00    --  105.15 112.00   6.00   63
  4  \w     69.00  96.00   1.00   16.00    --  105.15-112.00 -86.00   27
  5  \w   -115.00 -25.00   1.00    4.00    --  -40.91 -38.00 150.00   90
  6  \w     39.00  95.00   1.00    4.00    --   40.91-125.00-180.00   56
  7  \w    -32.00  59.00   1.00    4.00    --   40.91 -38.00 -30.00   91
  8  \w     35.00 109.00   1.00   16.00    --  105.15-111.00 120.00   74
  9  \w     44.00 109.00   1.00   16.00    --  105.15-111.00   0.00   65
 10  \w    109.00 168.00   1.00   16.00    --  105.15 111.00 -90.00   59
 11  \w     36.00  63.00   1.00   16.00    --  105.15-111.00 -30.00   27
 12  \w    104.00 164.00   1.00   16.00    --  105.15  77.00  90.00   60
 13  \w    105.00 170.00   1.00   16.00    --  105.15 111.00  30.00   65
 14  \w    121.00 147.00   1.00   16.00    --  105.15 111.00-150.00   26
 15  \w    127.00 170.00   1.00   16.00    --  105.15  30.00-180.00   43
 16  \w    107.00 169.00   1.00   16.00    --  105.15  77.00-120.00   62
;
_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      -0.0241706000
_diffrn_orient_matrix_UB_12      -0.0889642000
_diffrn_orient_matrix_UB_13      -0.0396281000
_diffrn_orient_matrix_UB_21      0.0182147000
_diffrn_orient_matrix_UB_22      -0.1012525000
_diffrn_orient_matrix_UB_23      0.0352872000
_diffrn_orient_matrix_UB_31      -0.0585035000
_diffrn_orient_matrix_UB_32      0.0052741000
_diffrn_orient_matrix_UB_33      0.0099141000
_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     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            9407
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.828
_diffrn_reflns_theta_min         4.143
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.339
_exptl_absorpt_correction_T_max  0.520
_exptl_absorpt_correction_T_min  0.118
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (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 green'
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       prism
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.104
_refine_diff_density_max         1.408
_refine_diff_density_min         -1.839
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         9407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0672P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8306
_reflns_number_total             9407
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 7.6525\% 
around [-0.90 -0.02 0.44] (reciprocal) or [-0.99 -0.10 0.10] (direct)
Component 3 rotated by 2.1621\% 
around [-0.78 -0.09 0.62] (reciprocal) or [-0.83 -0.47 0.31] (direct)
;
_cod_data_source_file            d2sc03592h2.cif
_cod_data_source_block           dkm206_sq
_cod_database_code               1567553
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C52 H130 N10 O2 Si12 U2'
_shelx_estimated_absorpt_t_max   0.338
_shelx_estimated_absorpt_t_min   0.131
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4791(19)
 0.1442(11) 0.3767(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 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)
;
_shelx_res_checksum              96422
_shelx_hkl_checksum              94772
_shelx_fab_checksum              68087
_platon_squeeze_void_probe_radius 1.20
_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 9.626
_oxdiff_exptl_absorpt_empirical_full_min 0.391
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3