Reactivity of a triamidoamine terminal uranium(VI)-nitride with 3d-transition metal metallocenes.
Seed, John A.; Cleaves, Peter A.; Hatton, Georgina R.; King, David M.; Tuna, Floriana; Wooles, Ashley J.; Chilton, Nicholas F.; Liddle, Stephen T.; Chemical communications (Cambridge, England) 60 (2024) 9990–9993; doi:10.1039/d4cc03846k

data_7133539
_publ_section_title
;
 Reactivity of a triamidoamine terminal uranium(VI)-nitride with
 3d-transition metal metallocenes.
;
_journal_issue                   73
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9990
_journal_page_last               9993
_journal_paper_doi               10.1039/d4cc03846k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C43 H85 Co N5 Si3 U'
_chemical_formula_sum            'C43 H85 Co N5 Si3 U'
_chemical_formula_weight         1053.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-07-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-07-26 deposited with the CCDC.	2024-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.576(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.6210(8)
_cell_length_b                   14.0125(4)
_cell_length_c                   27.1921(7)
_cell_measurement_reflns_used    16997
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.5810
_cell_measurement_theta_min      3.0061
_cell_volume                     9731.2(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_details
;
  1 omega   -7.00   32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        6.6846   38.0000 -120.0000 39

  2 omega   47.00   74.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        6.6846   38.0000  -90.0000 27

  3 omega    5.00   32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -6.7627  -99.0000 -120.0000 27

  4 omega  -76.00  -36.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -6.7627  -57.0000  -90.0000 40

  5 omega  -14.00   62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -6.7627   38.0000    0.0000 76

  6 omega  -77.00  -32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -6.7627  -38.0000 -150.0000 45

  7 omega  -15.00   19.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -6.7627   57.0000   90.0000 34

  8 omega  -20.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -6.7627  -99.0000   60.0000 53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0056520000
_diffrn_orient_matrix_UB_12      -0.0404519000
_diffrn_orient_matrix_UB_13      -0.0143496000
_diffrn_orient_matrix_UB_21      -0.0241218000
_diffrn_orient_matrix_UB_22      0.0060403000
_diffrn_orient_matrix_UB_23      -0.0143421000
_diffrn_orient_matrix_UB_31      0.0125340000
_diffrn_orient_matrix_UB_32      0.0298410000
_diffrn_orient_matrix_UB_33      -0.0165298000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            83460
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.693
_diffrn_reflns_theta_min         3.006
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.772
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             4312
_exptl_crystal_size_max          0.4052
_exptl_crystal_size_mid          0.3249
_exptl_crystal_size_min          0.2476
_refine_diff_density_max         1.937
_refine_diff_density_min         -1.885
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         21733
_refine_ls_number_restraints     345
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0286P)^2^+9.0765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17434
_reflns_number_total             21733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03846k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7133539--7133540.cif.'
_cod_database_code               7133539
_nottingham_internal_coll_name   UDKIPW
_nottingham_internal_coll_number 13365
_nottingham_internal_coll_client DMK/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time 15.0000
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxdmk
_nottingham_internal_coll_date   13/03/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 13/03/2014
_nottingham_internal_process_user pczdk
_nottingham_internal_solution_date 14/03/2014
_nottingham_internal_solution_user DMK/STL
_manchester_internal_refinement_date 26/07/2024
_manchester_internal_refinement_user AW
_manchester_internal_validation_date 26/07/2024
_manchester_internal_validation_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C43 H85 N4 Co Si3 U'
_shelx_estimated_absorpt_t_max   0.455
_shelx_estimated_absorpt_t_min   0.310
_reflns_odcompleteness_completeness 97.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 C42-C41 \\sim C43A-C42A \\sim C43-C42 \\sim C43A-C39A \\sim C43-C39 \\sim
C40A-C39A \\sim C40-C39 ~
 C41A-C40A \\sim C41-C40 \\sim C42A-C41A \\sim C85-C82 \\sim C84-C83 \\sim
C83-C82 \\sim C86-C84 \\sim C86-
 C85
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C39A \\sim C40A \\sim C41A
\\sim C42A \\sim C43A \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C39, C40, C41, C42, C43, C39A, C40A, C41A, C42A, C43A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=
 Sof(H42A)=Sof(C43A)=Sof(H43A)=1-FVAR(1)
 Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=
 Sof(C43)=Sof(H43)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C12(H12), C15(H15), C18(H18), C23(H23), C26(H26),
 C29(H29), C34(H34), C44(H44), C47(H47), C50(H50), C55(H55), C58(H58), C61(H61),
  C66(H66), C69(H69), C72(H72), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B), C22(H22A,H22B), C32(H32A,
 H32B), C33(H33A,H33B), C53(H53A,H53B), C54(H54A,H54B), C64(H64A,H64B),
 C65(H65A,H65B), C75(H75A,H75B), C76(H76A,H76B)
6.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
 C42(H42), C43(H43), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86),
 C39A(H39A), C40A(H40A), C41A(H41A), C42A(H42A), C43A(H43A)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,
 H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C67(H67A,
 H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C),
 C73(H73A,H73B,H73C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              84499
_shelx_hkl_checksum              83862
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'