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_7133540
_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 N5 Si3 U V'
_chemical_formula_sum            'C43 H85 N5 Si3 U V'
_chemical_formula_weight         1045.39
_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                 90.1352(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.8279(4)
_cell_length_b                   23.7780(3)
_cell_length_c                   20.6637(3)
_cell_measurement_reflns_used    18273
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.5430
_cell_measurement_theta_min      4.3330
_cell_volume                     9742.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
  1 omega  -23.00   31.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  150.0000 54

  2 omega  -51.00   34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   19.0000  -60.0000 85

  3 omega  -49.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   30.0000 82

  4 omega   33.00   97.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  -30.0000 64

  5 omega   30.00   81.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   60.0000 51

  6 omega  139.00  178.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000   30.0000 39

  7 omega   62.00   96.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000   90.0000 34

  8 omega   35.00   98.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  -90.0000 63

  9 omega   30.00   72.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  150.0000 42

 10 omega  109.00  178.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000  -30.0000 69

 11 omega   28.00   78.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  -90.0000 50

 12 omega   16.00   44.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
    -       43.0792   57.0000 -120.0000 28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      0.0085780000
_diffrn_orient_matrix_UB_12      -0.0498871000
_diffrn_orient_matrix_UB_13      0.0468218000
_diffrn_orient_matrix_UB_21      -0.0653161000
_diffrn_orient_matrix_UB_22      -0.0265455000
_diffrn_orient_matrix_UB_23      -0.0266339000
_diffrn_orient_matrix_UB_31      0.0412589000
_diffrn_orient_matrix_UB_32      -0.0315865000
_diffrn_orient_matrix_UB_33      -0.0515790000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
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_diffrn_reflns_number            18009
_diffrn_reflns_point_group_measured_fraction_full 0.946
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_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.673
_diffrn_reflns_theta_min         3.602
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.841
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             4280
_exptl_crystal_size_max          0.1085
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.071
_refine_diff_density_max         4.215
_refine_diff_density_min         -3.827
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         18009
_refine_ls_number_restraints     278
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0404P)^2^+184.7892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16421
_reflns_number_total             18009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03846k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7133539--7133540.cif.'
_cod_original_cell_volume        9742.3(3)
_cod_database_code               7133540
_nottingham_internal_coll_name   UPACMV
_nottingham_internal_coll_number 15107
_nottingham_internal_coll_client PAC/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '15.0000, 60.0000, 42.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxpacl
_nottingham_internal_coll_date   04/09/2015
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 07/09/2015
_nottingham_internal_process_user pcxpacl
_nottingham_internal_solution_date 07/09/2015
_nottingham_internal_solution_user pcxpacl
_manchester_internal_refinement_date 26/07/2024
_manchester_internal_refinement_user AW
_manchester_internal_validation_date 26/07/2024
_manchester_internal_validation_user AW
_manchester_internal_archive_date 26/07/2024
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C43 H85 N5 Si3 U V'
_chemical_oxdiff_usercomment
'UPACMV 15107 GVB-726 IN FOMBLIN FILM ON MICROMOUNT FOR PAC/STL'
_shelx_estimated_absorpt_t_max   0.487
_shelx_estimated_absorpt_t_min   0.360
_reflns_odcompleteness_completeness 94.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8113(14)
 0.1887(14)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(N5) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(N6) \\sim
Ueq, Uanis(N9) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma
of 0.004 and sigma for terminal atoms of 0.008
4. Rigid body (RIGU) restrains
 C77, C78, C79, C80, C81, V2, C82, C83, C84, C85, C86, N10, N6, N8, N9, N7, N5,
  U1, N3, N4, N2, N1, C47, C48, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.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), C44(H44), C47(H47), C50(H50), C55(H55), C58(H58), C61(H61), C66(H66),
  C69(H69), C72(H72)
5.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)
5.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
 C41(H41), C42(H42), C43(H43), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81),
  C82(H82), C83(H83), C84(H84), C85(H85), C86(H86)
5.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              37941
_shelx_hkl_checksum              45829
_olex2_submission_special_instructions 'No special instructions were received'