Room temperature dinitrogen cleavage and hydrogenation with organometallic complexes of uranium.
Shephard, Angus C. G.; Pedussaut, Lucie; De Marchi, Linda; Demonti, Luca; Rajeshkumar, Thayalan; Casaretto, Nicolas; Maron, Laurent; Danoun, Grégory; Simler, Thomas; Nocton, Grégory; Chemical science 16 (2025) 21334–21345; doi:10.1039/d5sc07194a

data_1575979
_publ_section_title
;
 Room temperature dinitrogen cleavage and hydrogenation with
 organometallic complexes of uranium.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              21334
_journal_page_last               21345
_journal_paper_doi               10.1039/d5sc07194a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C68 H116 I N2 U3, 3(C7 H8)'
_chemical_formula_sum            'C89 H140 I N2 U3'
_chemical_formula_weight         2079.01
_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
_audit_creation_date             2025-05-19
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-06-13 deposited with the CCDC.	2025-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                77.506(2)
_cell_angle_beta                 82.208(2)
_cell_angle_gamma                65.737(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0922(3)
_cell_length_b                   14.3701(3)
_cell_length_c                   23.5776(5)
_cell_measurement_reflns_used    77184
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      2.11
_cell_volume                     4243.94(17)
_computing_cell_refinement
;
X-Area Recipe 2.0.2 (STOE, 2024)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.194.0 (STOE, 2023)
;
_computing_data_reduction
;
X-Area Integrate 2.5.18.0 (STOE, 2024)
X-Area LANA 2.8.4 (STOE, 2024)
;
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 1122 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            72299
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.210
_exptl_absorpt_coefficient_mu    6.116
_exptl_absorpt_correction_T_max  0.6129
_exptl_absorpt_correction_T_min  0.2165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2034
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.055
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     943
_refine_ls_number_reflns         18716
_refine_ls_number_restraints     384
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15421
_reflns_number_total             18716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc07194a3.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1575976--1575980.cif.'
_cod_database_code               1575979
_shelx_shelxl_version_number     2019/2
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim
C87 \\sim C88 \\sim C89 \\sim C90 \\sim C91 \\sim C92: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
2. Rigid body (RIGU) restrains
 C79, C80, C81, C82, C83, C84, C85, C86, C87, C88, C89, C90, C91, C92
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C6, C7, C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Sof(C79)=Sof(C80)=Sof(H80)=Sof(C81)=Sof(H81)=Sof(C82)=Sof(H82)=Sof(C83)=
 Sof(H83)=Sof(C84)=Sof(H84)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=1-FVAR(2)
 Sof(C86)=Sof(C87)=Sof(H87)=Sof(C88)=Sof(H88)=Sof(C89)=Sof(H89)=Sof(C90)=
 Sof(H90)=Sof(C91)=Sof(H91)=Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(H92C)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C22(H22), C25(H25), C39(H39), C42(H42), C56(H56), C59(H59),
 C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C87(H87), C88(H88), C89(H89),
  C90(H90), C91(H91), C94(H94), C95(H95), C96(H96), C97(H97), C98(H98),
 C105(H105), C104(H104), C103(H103), C102(H102), C101(H101)
4.b Fitted hexagon refined as free rotating group:
 C79(C80,C81,C82,C83,C84), C86(C87,C88,C89,C90,C91), C93(C94,C95,C96,C97,C98),
 C100(C105,C104,C103,C102,C101)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,
 H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C),
 C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C85(H85A,H85B,H85C), C92(H92A,H92B,
 H92C), C99(H99A,H99B,H99C), C106(H10D,H10E,H10F)
;
_shelx_res_checksum              25213
_olex2_submission_special_instructions 'No special instructions were received'