Nitrogen activation and cleavage by a multimetallic uranium complex.
Keener, Megan; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Zivkovic, Ivica; Mazzanti, Marinella; Chemical science 13 (2022) 8025–8035; doi:10.1039/d2sc02997a

data_1567209
_publ_section_title
;
 Nitrogen activation and cleavage by a multimetallic uranium complex.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              8025
_journal_page_last               8035
_journal_paper_doi               10.1039/d2sc02997a
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C60 H144 K N3 O16 Si8 U2'
_chemical_formula_sum            'C60 H144 K N3 O16 Si8 U2'
_chemical_formula_weight         1903.65
_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             2022-04-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-25 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                108.265(2)
_cell_angle_beta                 92.266(2)
_cell_angle_gamma                107.449(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1046(3)
_cell_length_b                   16.1530(4)
_cell_length_c                   22.2432(5)
_cell_measurement_reflns_used    24048
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.9650
_cell_measurement_theta_min      3.3040
_cell_volume                     4540.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.976
_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   -113.00 -88.00   1.00    5.00    --  -40.91-141.00 -86.00   25
  2  \w    -58.00 -10.00   1.00    5.00    --  -40.91 129.00 158.00   48
  3  \w    -68.00 -43.00   1.00    5.00    --  -40.91 141.00 -28.00   25
  4  \w     49.00  74.00   1.00    5.00    --   40.91-141.00 -86.00   25
  5  \w     40.00  65.00   1.00    5.00    --   40.91-129.00  85.00   25
  6  \w     70.00 125.00   1.00   20.00    --  112.00-141.00 -86.00   55
  7  \w     77.00 116.00   1.00   20.00    --  112.00-129.00  85.00   39
  8  \w    122.00 149.00   1.00   20.00    --  112.00 129.00 158.00   27
  9  \w    106.00 131.00   1.00   20.00    --  112.00 141.00 -28.00   25
 10  \w   -113.00 -40.00   1.00    5.00    --  -40.91 -57.00  30.00   73
 11  \w   -121.00   0.00   1.00    5.00    --  -40.91 -19.00-120.00  121
 12  \w     40.00  97.00   1.00    5.00    --   40.91-125.00 -30.00   57
 13  \w     -8.00  40.00   1.00    5.00    --   40.91 -38.00 120.00   48
 14  \w      8.00  74.00   1.00    5.00    --   40.91 -99.00 120.00   66
 15  \w    108.00 135.00   1.00   20.00    --  112.00 111.00 -90.00   27
 16  \w    144.00 172.00   1.00   20.00    --  112.00 111.00 120.00   28
 17  \w     66.00 138.00   1.00   20.00    --  112.00 -45.00  30.00   72
 18  \w     41.00  68.00   1.00   20.00    --  112.00-111.00 150.00   27
 19  \w     75.00 107.00   1.00   20.00    --  112.00-111.00 -30.00   32
 20  \w     69.00 109.00   1.00   20.00    --  112.00-111.00 150.00   40
 21  \w    106.00 166.00   1.00   20.00    --  112.00  77.00 120.00   60
 22  \w     62.00  89.00   1.00   20.00    --  112.00 178.00  30.00   27
 23  \w     37.00 109.00   1.00   20.00    --  112.00-111.00 -90.00   72
 24  \w    105.00 131.00   1.00   20.00    --  112.00 111.00 120.00   26
 25  \w     53.00 109.00   1.00   20.00    --  112.00-111.00  60.00   56
 26  \w    128.00 177.00   1.00   20.00    --  112.00  77.00 150.00   49
 27  \w    123.00 178.00   1.00   20.00    --  112.00  30.00-150.00   55
 28  \w    112.00 139.00   1.00   20.00    --  112.00  77.00  60.00   27
 29  \w    143.00 172.00   1.00   20.00    --  112.00  77.00  60.00   29
 30  \w     80.00 109.00   1.00   20.00    --  112.00-111.00-150.00   29
 31  \w     41.00 109.00   1.00   20.00    --  112.00-111.00   0.00   68
 32  \w     75.00 109.00   1.00   20.00    --  112.00-111.00  90.00   34
 33  \w    115.00 141.00   1.00   20.00    --  112.00 -61.00 150.00   26
 34  \w     64.00  91.00   1.00   20.00    --  112.00 -77.00  60.00   27
 35  \w     85.00 157.00   1.00   20.00    --  112.00  30.00-120.00   72
 36  \w     87.00 121.00   1.00   20.00    --  112.00  30.00-150.00   34
 37  \w     95.00 138.00   1.00   20.00    --  112.00 178.00  30.00   43
 38  \w     38.00  90.00   1.00   20.00    --  112.00-111.00  30.00   52
 39  \w     45.00 102.00   1.00   20.00    --  112.00 -61.00 150.00   57
 40  \w    116.00 175.00   1.00   20.00    --  112.00 111.00  30.00   59
 41  \w    121.00 162.00   1.00   20.00    --  112.00 111.00 150.00   41
 42  \w     57.00 108.00   1.00   20.00    --  112.00-111.00-180.00   51
 43  \w     48.00  75.00   1.00   20.00    --  112.00 -45.00-150.00   27
 44  \w    106.00 133.00   1.00   20.00    --  112.00 -45.00-150.00   27
 45  \w     29.00 100.00   1.00   20.00    --  112.00 -94.00  90.00   71
 46  \w    151.00 176.00   1.00   20.00    --  112.00  61.00  90.00   25
 47  \w    133.00 170.00   1.00   20.00    --  112.00 111.00-180.00   37
 48  \w     88.00 143.00   1.00   20.00    --  112.00  61.00  90.00   55
;
_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      -0.0573031000
_diffrn_orient_matrix_UB_12      -0.0581725000
_diffrn_orient_matrix_UB_13      0.0385017000
_diffrn_orient_matrix_UB_21      -0.0495647000
_diffrn_orient_matrix_UB_22      -0.0807436000
_diffrn_orient_matrix_UB_23      -0.0627602000
_diffrn_orient_matrix_UB_31      0.0875173000
_diffrn_orient_matrix_UB_32      -0.0375262000
_diffrn_orient_matrix_UB_33      0.0040400000
_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     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22028
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.105
_diffrn_reflns_theta_min         3.051
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.805
_exptl_absorpt_correction_T_max  0.512
_exptl_absorpt_correction_T_min  0.199
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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            'clear light brown'
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       prism
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.786
_refine_diff_density_min         -1.730
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         22028
_refine_ls_number_restraints     381
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0511
_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^)+(0.1023P)^2^+1.6506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17681
_reflns_number_total             22028
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 13.7402\% 
around [-0.11 0.81 -0.57] (reciprocal) or [0.15 0.98 -0.15] (direct)
Component 3 rotated by 3.2575\% 
around [-0.58 -0.70 0.42] (reciprocal) or [-0.74 -0.67 -0.02] (direct)
;
_cod_data_source_file            d2sc02997a2.cif
_cod_data_source_block           mk426
_cod_depositor_comments
'Adding full bibliography for 1567201--1567212.cif.'
_cod_original_cell_volume        4540.79(19)
_cod_database_code               1567209
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C60 H60 N3 O16 K1 U2'
_shelx_estimated_absorpt_t_max   0.420
_shelx_estimated_absorpt_t_min   0.140
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6245(18)
 0.1905(14) 0.1850(12)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O105-C115 \\sim O103-C107 \\sim O106-C111 \\sim O104-C111
 with sigma of 0.02
 C113-C114 \\sim C114-C112 \\sim C112-C113
 with sigma of 0.02
 C117-C116 \\sim C116-C118 \\sim C117-C118
 with sigma of 0.02
 Si8-O102 \\sim Si8-O105 \\sim Si8-O103 \\sim Si8-O106 \\sim Si8-O104
 with sigma of 0.02
 C108-C110 \\sim C110-C109 \\sim C108-C109
 with sigma of 0.02
 C102-C101 \\sim C105-C101 \\sim C103-C101 \\sim C106-C101 \\sim C104-C101
 with sigma of 0.02
 C113-C111 \\sim C120-C111 \\sim C119-C111 \\sim C112-C111 \\sim C114-C111
\\sim C121-C111
 with sigma of 0.02
 C104-C103 \\sim C106-C105
 with sigma of 0.02
 C120-C119 \\sim C119-C121 \\sim C120-C121
 with sigma of 0.02
 C108-C107 \\sim C110-C107 \\sim C109-C107 \\sim C117-C115 \\sim C116-C115
\\sim C118-C115
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C115 \\sim C108 \\sim C116 \\sim C107 \\sim C117 \\sim C110 \\sim C118 \\sim
C109 \\sim Si8 \\sim O105 \\sim O103 \\sim O106 \\sim O104 \\sim O102 \\sim
C111 \\sim C120 \\sim C113 \\sim C119 \\sim C112 \\sim C121 \\sim C114 \\sim
C105 \\sim C101 \\sim C102 \\sim C104 \\sim C106 \\sim C103: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C88) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C86) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(O105)=Sof(O106)=Sof(C105)=Sof(H10M)=Sof(H10N)=Sof(H10O)=Sof(C106)=
 Sof(H10P)=Sof(H10Q)=Sof(H10R)=Sof(C115)=Sof(C116)=Sof(H11P)=Sof(H11Q)=
 Sof(H11R)=Sof(C117)=Sof(H11S)=Sof(H11T)=Sof(H11U)=Sof(C118)=Sof(H11V)=
 Sof(H11W)=Sof(H11X)=Sof(C119)=Sof(H11Y)=Sof(H)=Sof(HA)=Sof(C120)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(C121)=Sof(H12G)=Sof(H12H)=Sof(H12I)=1-FVAR(1)
 Sof(O103)=Sof(O104)=Sof(C103)=Sof(H10G)=Sof(H10H)=Sof(H10I)=Sof(C104)=
 Sof(H10J)=Sof(H10K)=Sof(H10L)=Sof(C107)=Sof(C108)=Sof(H10S)=Sof(H10T)=
 Sof(H10U)=Sof(C109)=Sof(H10V)=Sof(H10W)=Sof(H10X)=Sof(C110)=Sof(H11D)=
 Sof(H11E)=Sof(H11F)=Sof(C112)=Sof(H11G)=Sof(H11H)=Sof(H11I)=Sof(C113)=
 Sof(H11J)=Sof(H11K)=Sof(H11L)=Sof(C114)=Sof(H11M)=Sof(H11N)=Sof(H11O)=FVAR(1)
6.a Me refined with riding coordinates:
 C102(H10D,H10E,H10F), C103(H10G,H10H,H10I), C104(H10J,H10K,H10L), C105(H10M,
 H10N,H10O), C106(H10P,H10Q,H10R), C108(H10S,H10T,H10U), C109(H10V,H10W,H10X),
 C110(H11D,H11E,H11F), C112(H11G,H11H,H11I), C113(H11J,H11K,H11L), C114(H11M,
 H11N,H11O), C116(H11P,H11Q,H11R), C117(H11S,H11T,H11U), C118(H11V,H11W,H11X),
 C119(H11Y,H,HA), C120(H12D,H12E,H12F), C121(H12G,H12H,H12I)
6.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C82(H82A,
 H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C),
 C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C90(H90A,H90B,H90C), C91(H91A,H91B,
 H91C), C92(H92A,H92B,H92C)
;
_shelx_res_checksum              74817
_shelx_hkl_checksum              11737
_olex2_date_sample_data_collection 2021-08-31
_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 3.251
_oxdiff_exptl_absorpt_empirical_full_min 0.173
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3