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_1567556
_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, 2(C18 H36 K N2 O6), 4(C4 H10 O)'
_chemical_formula_sum            'C96 H226 K2 N14 O16 Si12 U2'
_chemical_formula_weight         2724.23
_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             2020-05-13
_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                63.8536(11)
_cell_angle_beta                 84.3138(8)
_cell_angle_gamma                74.6504(9)
_cell_formula_units_Z            1
_cell_length_a                   13.78160(13)
_cell_length_b                   16.73893(18)
_cell_length_c                   17.00630(17)
_cell_measurement_reflns_used    29165
_cell_measurement_temperature    139.9(9)
_cell_measurement_theta_max      75.8420
_cell_measurement_theta_min      4.3420
_cell_volume                     3395.39(7)
_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    'ShelXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.9(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_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    -19.00  12.00   1.00    2.00    --  -40.91  21.00 110.00   31
  2  \w   -119.00  -3.00   1.00    2.00    --  -40.91 -21.00 -55.00  116
  3  \w     40.00 120.00   1.00    2.00    --   40.91  21.00 110.00   80
  4  \w    122.00 177.00   1.00    8.00    --  112.00  21.00 110.00   55
  5  \w     74.00 128.00   1.00    8.00    --  112.00 -21.00 -55.00   54
  6  \w     41.00  70.00   1.00    8.00    --  112.00 -21.00 -55.00   29
  7  \w    -85.00  -9.00   1.00    2.00    --  -40.91 125.00  90.00   76
  8  \w     43.00  78.00   1.00    2.00    --   40.91-125.00  90.00   35
  9  \w     -4.00  21.00   1.00    2.00    --   40.91 -21.00 -55.00   25
 10  \w    -17.00  64.00   1.00    2.00    --   40.91 -77.00-150.00   81
 11  \w      8.00  82.00   1.00    2.00    --   40.91 -99.00 -60.00   74
 12  \w     87.00 177.00   1.00    8.00    --  112.00  30.00   0.00   90
 13  \w     40.00 137.00   1.00    8.00    --  112.00 -45.00-180.00   97
 14  \w     30.00 100.00   1.00    8.00    --  112.00 -94.00   0.00   70
 15  \w     60.00  87.00   1.00    8.00    --  112.00-111.00 -90.00   27
 16  \w     84.00 171.00   1.00    8.00    --  112.00  61.00  30.00   87
 17  \w     30.00  92.00   1.00    8.00    --  112.00 -94.00 150.00   62
 18  \w     44.00  69.00   1.00    8.00    --  112.00-111.00  30.00   25
 19  \w     74.00 109.00   1.00    8.00    --  112.00-111.00 -60.00   35
 20  \w     37.00  84.00   1.00    8.00    --  112.00 -30.00  30.00   47
 21  \w    113.00 140.00   1.00    8.00    --  112.00 -61.00  60.00   27
 22  \w     35.00  62.00   1.00    8.00    --  112.00 -15.00 120.00   27
 23  \w     63.00 109.00   1.00    8.00    --  112.00-111.00  60.00   46
 24  \w     53.00 109.00   1.00    8.00    --  112.00-111.00 -30.00   56
 25  \w     71.00 155.00   1.00    8.00    --  112.00 -15.00 120.00   84
 26  \w     36.00 109.00   1.00    8.00    --  112.00-111.00-150.00   73
 27  \w     55.00 109.00   1.00    8.00    --  112.00-111.00   0.00   54
 28  \w     37.00  79.00   1.00    8.00    --  112.00-111.00 150.00   42
 29  \w     83.00 109.00   1.00    8.00    --  112.00-111.00 150.00   26
 30  \w     96.00 123.00   1.00    8.00    --  112.00 -61.00-180.00   27
 31  \w    107.00 138.00   1.00    8.00    --  112.00 -30.00  30.00   31
 32  \w     36.00 109.00   1.00    8.00    --  112.00-111.00  90.00   73
 33  \w     91.00 134.00   1.00    8.00    --  112.00  45.00 -60.00   43
 34  \w    138.00 166.00   1.00    8.00    --  112.00  45.00 -60.00   28
 35  \w     64.00 101.00   1.00    8.00    --  112.00 -94.00  90.00   37
 36  \w     55.00  84.00   1.00    8.00    --  112.00 -61.00-180.00   29
 37  \w     46.00  80.00   1.00    8.00    --  112.00 -61.00  60.00   34
 38  \w     41.00  66.00   1.00    8.00    --  112.00-111.00-180.00   25
 39  \w     74.00 109.00   1.00    8.00    --  112.00-111.00-120.00   35
 40  \w     43.00  70.00   1.00    8.00    --  112.00 -94.00 -30.00   27
 41  \w     37.00  70.00   1.00    8.00    --  112.00 -94.00-150.00   33
;
_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      -0.0757657000
_diffrn_orient_matrix_UB_12      -0.0601444000
_diffrn_orient_matrix_UB_13      0.0256578000
_diffrn_orient_matrix_UB_21      -0.0811711000
_diffrn_orient_matrix_UB_22      0.0763161000
_diffrn_orient_matrix_UB_23      0.0129046000
_diffrn_orient_matrix_UB_31      -0.0333700000
_diffrn_orient_matrix_UB_32      0.0419023000
_diffrn_orient_matrix_UB_33      -0.0967626000
_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  0.0276
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40729
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.054
_diffrn_reflns_theta_min         2.895
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.674
_exptl_absorpt_correction_T_max  0.554
_exptl_absorpt_correction_T_min  0.251
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
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 as
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1418
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         14025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0221
_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^)+(0.0245P)^2^+2.5506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0536
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13728
_reflns_number_total             14025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03592h2.cif
_cod_data_source_block           dkm132
_cod_database_code               1567556
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C96 H226 K2 N14 O16 Si12 U2'
_shelx_estimated_absorpt_t_max   0.454
_shelx_estimated_absorpt_t_min   0.203
_reflns_odcompleteness_completeness 99.90
_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.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), 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), C43(H43A,H43B), C45(H45A,H45B), C47(H47A,H47B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
2.c 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), C42(H42A,H42B,H42C),
 C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              96709
_shelx_hkl_checksum              38004
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.459
_oxdiff_exptl_absorpt_empirical_full_min 0.665