Uranium–nitride chemistry: uranium–uranium electronic communication mediated by nitride bridges
King, David M.; Atkinson, Benjamin E.; Chatelain, Lucile; Gregson, Matthew; Seed, John A.; Wooles, Ashley J.; Kaltsoyannis, Nikolas; Liddle, Stephen T.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00998F

data_7710360
_publ_section_title
;
 Uranium--nitride chemistry: uranium--uranium electronic communication
 mediated by nitride bridges
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00998F
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C66 H151 Li3 N10 Si6 U2'
_chemical_formula_sum            'C66 H151 Li3 N10 Si6 U2'
_chemical_formula_weight         1750.38
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-15 deposited with the CCDC.	2022-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9119(2)
_cell_length_b                   16.9119(2)
_cell_length_c                   28.5448(6)
_cell_measurement_reflns_used    16278
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.3420
_cell_measurement_theta_min      4.0480
_cell_volume                     8164.2(2)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -64.00  -18.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  127.0000  148.0000 46

  2 omega -109.00  -12.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000    0.0000 97

  3 omega  -50.00   34.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  150.0000 84

  4 omega   41.00   68.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       43.3152 -125.0000  -30.0000 27

  5 omega  130.00  157.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   61.0000 -120.0000 27

  6 omega   45.00  109.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -95.0000 -150.0000 64

  7 omega   43.00   93.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -45.0000   60.0000 50

  8 omega   54.00   88.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000  120.0000 34

  9 omega   61.00  172.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   15.0000   60.0000 111

 10 omega   58.00   85.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000 -150.0000 27

 11 omega   37.00   78.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -45.0000 -180.0000 41

 12 omega   39.00   91.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000 -120.0000 52

 13 omega   46.00   88.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000   90.0000 42
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      -0.0354180000
_diffrn_orient_matrix_UB_12      0.0776197000
_diffrn_orient_matrix_UB_13      -0.0188059000
_diffrn_orient_matrix_UB_21      -0.0076854000
_diffrn_orient_matrix_UB_22      0.0312171000
_diffrn_orient_matrix_UB_23      0.0504730000
_diffrn_orient_matrix_UB_31      0.0836187000
_diffrn_orient_matrix_UB_32      0.0359605000
_diffrn_orient_matrix_UB_33      -0.0033005000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            36472
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.482
_diffrn_reflns_theta_min         4.008
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    12.229
_exptl_absorpt_correction_T_max  0.633
_exptl_absorpt_correction_T_min  0.336
_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            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             3576
_exptl_crystal_size_max          0.1303
_exptl_crystal_size_mid          0.0493
_exptl_crystal_size_min          0.0449
_refine_diff_density_max         1.175
_refine_diff_density_min         -1.276
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.031(6)
_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     413
_refine_ls_number_reflns         8252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0254P)^2^+8.1785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                7828
_reflns_number_total             8252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00998f2.cif
_cod_data_source_block           5
_cod_original_cell_volume        8164.2(3)
_cod_database_code               7710360
_nottingham_internal_coll_name   UMGALE
_nottingham_internal_coll_number 15053
_nottingham_internal_coll_client MG/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '17.5000, 70.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxmjg
_nottingham_internal_coll_date   08/08/2015
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_process_date 09/08/2015
_nottingham_internal_process_user pczmjg1
_nottingham_internal_solution_date 10/08/2015
_nottingham_internal_solution_user pczmjg1
_nottingham_internal_refinement_date 10/08/2015
_nottingham_internal_refinement_user pczmjg1
_nottingham_internal_self_archive_date 10/08/2015
_nottingham_internal_self_validation_date 10/08/2015
_nottingham_internal_self_validation_user pczmjg1
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C53 H99 Li2 N5 O6 Si3 U'
_chemical_oxdiff_usercomment
'UMGALE #15053 SN-659 FOR MG/STL IN FOMBLIN FILM ON MICROMOUNT'
_shelx_estimated_absorpt_t_max   0.610
_shelx_estimated_absorpt_t_min   0.299
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.031(6)
 -0.031(6)
2. 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
3.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)
3.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)
3.c Aromatic/amide H refined with riding coordinates:
 N6(H6)
3.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)
;
_shelx_res_checksum              65992
_olex2_submission_special_instructions 'No special instructions were received'