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_1567554
_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         'C18 H36 K N2 O6, 2(C8 H6 N4)'
_chemical_formula_sum            'C34 H48 K N10 O6'
_chemical_formula_weight         731.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-02-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-06-23 deposited with the CCDC.	2022-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.777(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3683(13)
_cell_length_b                   20.5260(10)
_cell_length_c                   14.6910(10)
_cell_measurement_reflns_used    4781
_cell_measurement_temperature    140.01(10)
_cell_measurement_theta_max      71.5460
_cell_measurement_theta_min      3.8180
_cell_volume                     4137.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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      140.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_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    -50.00   1.00   1.00   10.00    --  -43.01  45.00 113.00   51
  2  \w   -115.00 -17.00   1.00   10.00    --  -43.01 -45.00 -36.00   98
  3  \w     -5.00  20.00   1.00   10.00    --   43.01 -45.00 -36.00   25
  4  \w     28.00 101.00   1.00   10.00    --   43.01  45.00 113.00   73
  5  \w     34.00 112.00   1.00   40.00    --  103.80 -45.00 -36.00   78
  6  \w     79.00 150.00   1.00   40.00    --  103.80  45.00 113.00   71
  7  \w    -86.00  -9.00   1.00   10.00    --  -43.01 125.00 120.00   77
  8  \w    -86.00  -7.00   1.00   10.00    --  -43.01 125.00-150.00   79
  9  \w    103.00 177.00   1.00   40.00    --  103.80  77.00   0.00   74
 10  \w     82.00 107.00   1.00   40.00    --  103.80 -94.00 -60.00   25
 11  \w     67.00 126.00   1.00   40.00    --  103.80 178.00-120.00   59
 12  \w    106.00 153.00   1.00   40.00    --  103.80  77.00  30.00   47
 13  \w     28.00  55.00   1.00   40.00    --  103.80-111.00  60.00   27
 14  \w     22.00  86.00   1.00   40.00    --  103.80 -94.00 -30.00   64
 15  \w     68.00 104.00   1.00   40.00    --  103.80-111.00  60.00   36
 16  \w     62.00  92.00   1.00   40.00    --  103.80 178.00   0.00   30
 17  \w     97.00 146.00   1.00   40.00    --  103.80 178.00   0.00   49
 18  \w     57.00 108.00   1.00   40.00    --  103.80-111.00 120.00   51
 19  \w     90.00 166.00   1.00   40.00    --  103.80  61.00 -30.00   76
 20  \w    135.00 174.00   1.00   40.00    --  103.80 111.00 -30.00   39
 21  \w     30.00  65.00   1.00   40.00    --  103.80 -94.00 -60.00   35
 22  \w     82.00 107.00   1.00   40.00    --  103.80 -94.00-180.00   25
 23  \w     42.00  69.00   1.00   40.00    --  103.80 -94.00 150.00   27
 24  \w     71.00 106.00   1.00   40.00    --  103.80 -94.00 150.00   35
 25  \w     40.00  65.00   1.00   40.00    --  103.80 -94.00-180.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0622724000
_diffrn_orient_matrix_UB_12      0.0604758000
_diffrn_orient_matrix_UB_13      -0.0516624000
_diffrn_orient_matrix_UB_21      -0.0927311000
_diffrn_orient_matrix_UB_22      -0.0421458000
_diffrn_orient_matrix_UB_23      -0.0411889000
_diffrn_orient_matrix_UB_31      -0.0113423000
_diffrn_orient_matrix_UB_32      0.0143775000
_diffrn_orient_matrix_UB_33      0.0970292000
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16648
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.755
_diffrn_reflns_theta_min         3.875
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4046
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0703P)^2^+0.4689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3014
_reflns_number_total             4046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03592h2.cif
_cod_data_source_block           mb63
_cod_database_code               1567554
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H56 N10 O7 K1'
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.785
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O3_$1-C9_$1 \\sim O3_$1-C10_$1
 with sigma of 0.02
 C9-C9_$1 \\sim C10-C10_$1
 with sigma of 0.02
3. Others
 Sof(C10)=Sof(H10A)=Sof(H10B)=1-FVAR(1)
 Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 158 electrons were 
found in a volume of 716\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C4H8O] per Asymmetric Unit 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16681
_shelx_hkl_checksum              69325
_shelx_fab_checksum              80843
_olex2_date_sample_data_collection 2021-10-04
_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 1.557
_oxdiff_exptl_absorpt_empirical_full_min 0.641