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_1575980
_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 H118 N2 U2, C5 H12'
_chemical_formula_sum            'C73 H130 N2 U2'
_chemical_formula_weight         1511.84
_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
_audit_creation_date             2025-06-10
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.22 svn.r631f81ec for OlexSys, GUI svn.r7248)
;
_audit_update_record
;
2025-06-13 deposited with the CCDC.	2025-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.8290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   44.3908(7)
_cell_length_b                   11.6107(2)
_cell_length_c                   56.6934(11)
_cell_measurement_reflns_used    4046
_cell_measurement_temperature    150
_cell_measurement_theta_max      18.59
_cell_measurement_theta_min      1.86
_cell_volume                     28599.7(9)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
 786 frames, detector distance = 100 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  0.0475
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            81690
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.231
_exptl_absorpt_coefficient_mu    4.563
_exptl_absorpt_correction_T_max  0.9984
_exptl_absorpt_correction_T_min  0.9920
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             12256
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.033
_refine_diff_density_max         2.150
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1463
_refine_ls_number_reflns         25119
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+227.7990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17262
_reflns_number_total             25119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc07194a3.cif
_cod_data_source_block           A
_cod_depositor_comments
'Adding full bibliography for 1575976--1575980.cif.'
_cod_database_code               1575980
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.529
_diffrn_oxdiff_ac3_digest_hkl    411b9eae574a06265ac7f2ad8f17459946f237
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C146-C145 \\sim C144-C145 \\sim C144-C142 \\sim C142-C143 \\sim C140-C141
\\sim C140-C137 \\sim C137-
 C138 \\sim C138-C139
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C142 \\sim C143 \\sim C144 \\sim C145 \\sim C146: within 2A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 2A
C137 \\sim C138 \\sim C139 \\sim C140 \\sim C141: within 2A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 2A
4.a Secondary CH2 refined with riding coordinates:
 C137(H13V,H13W), C138(H13X,H13Y), C140(H14A,H14B), C142(H14F,H14G), C144(H14K,
 H14L), C145(H14M,H14N)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C1(H1A), C4(H4), C18(H18), C21(H21), C37(H37), C39(H39),
 C53(H53), C56(H56), N3(H3), N4(H4A), C70(H70), C73(H73), C88(H88), C90(H90),
 C105(H105), C107(H107), C122(H122), C124(H124)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C51(H51A,H51B,H51C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,
 H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C75(H75A,H75B,H75C),
 C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C80(H80A,H80B,
 H80C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,
 H85B,H85C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C),
 C96(H96A,H96B,H96C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C), C100(H10A,H10B,
 H10C), C101(H10D,H10E,H10F), C102(H10G,H10H,H10I), C109(H10J,H10K,H10L),
 C110(H11D,H11E,H11F), C111(H11G,H11H,H11I), C113(H11J,H11K,H11L), C114(H11M,
 H11N,H11O), C115(H11P,H11Q,H11R), C117(H11S,H11T,H11U), C118(H11V,H11W,H11X),
 C119(H11Y,H,HA), C126(H12D,H12E,H12F), C127(H12G,H12H,H12I), C128(H12J,H12K,
 H12L), C130(H13D,H13E,H13F), C131(H13G,H13H,H13I), C132(H13J,H13K,H13L),
 C134(H13M,H13N,H13O), C135(H13P,H13Q,H13R), C136(H13S,H13T,H13U), C139(H13Z,HB,
 HC), C141(H14C,H14D,H14E), C143(H14H,H14I,H14J), C146(H14O,H14P,H14Q)
;
_shelx_res_checksum              84348
_olex2_submission_special_instructions 'No special instructions were received'