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_7710359
_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_formula_moiety         'C66 H150 Li4 N10 Si6 U2'
_chemical_formula_sum            'C66 H150 Li4 N10 Si6 U2'
_chemical_formula_weight         1756.31
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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     heavy
_audit_creation_date             2021-07-05
_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                100.569(2)
_cell_angle_beta                 105.912(2)
_cell_angle_gamma                110.139(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7485(3)
_cell_length_b                   13.3689(3)
_cell_length_c                   15.0115(4)
_cell_measurement_reflns_used    10181
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.1620
_cell_measurement_theta_min      3.2020
_cell_volume                     2025.52(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.6296
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
  1 omega  -46.00  -18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -90.0000 28

  2 omega -110.00  -19.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000  120.0000 91

  3 omega  -39.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   30.0000  -60.0000 74

  4 omega    7.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   60.0000 26

  5 omega   63.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       39.0554 -147.0000 -149.0000 44

  6 omega    6.00   93.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       39.0554 -125.0000   60.0000 87

  7 omega   33.00   86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000  -90.0000 53

  8 omega   25.00  143.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -15.0000  -60.0000 118

  9 omega   30.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000  150.0000 61

 10 omega   48.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295 -125.0000  120.0000 67

 11 omega   32.00   57.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000 -150.0000 25

 12 omega   40.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000   90.0000 51

 13 omega   44.00  123.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -77.0000  150.0000 79

 14 omega   82.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -94.0000 -120.0000 27

 15 omega   91.00  166.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   45.0000  -60.0000 75

 16 omega   93.00  118.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295 -125.0000   60.0000 25

 17 omega   96.00  122.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295 -125.0000 -120.0000 26

 18 omega  103.00  161.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  125.0000 -120.0000 58

 19 omega   47.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -45.0000  -30.0000 42

 20 omega   32.00  132.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -77.0000  -90.0000 100
;
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0710683000
_diffrn_orient_matrix_UB_12      -0.0341159000
_diffrn_orient_matrix_UB_13      -0.0641157000
_diffrn_orient_matrix_UB_21      -0.1099790000
_diffrn_orient_matrix_UB_22      -0.0130849000
_diffrn_orient_matrix_UB_23      -0.0916175000
_diffrn_orient_matrix_UB_31      0.0732681000
_diffrn_orient_matrix_UB_32      0.1237138000
_diffrn_orient_matrix_UB_33      0.0086109000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15012
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.518
_diffrn_reflns_theta_min         3.217
_diffrn_source                   'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.323
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_correction_T_min  0.330
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.1466
_exptl_crystal_size_mid          0.0978
_exptl_crystal_size_min          0.0508
_refine_diff_density_max         1.305
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         8018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0453
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7784
_reflns_number_total             8018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00998f2.cif
_cod_data_source_block           2
_cod_original_cell_volume        2025.53(10)
_cod_database_code               7710359
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C66 H150 N10 Li4 Si6 U2'
_chemical_oxdiff_usercomment
'UDKIOU #12699 IN FOMBLIN FILM ON MICROMOUNT FOR DMK/STL'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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.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)
2.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)
2.c Me refined with riding coordinates:
 C16(H16A,H16B,H16C)
2.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), 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              20144
_olex2_submission_special_instructions 'No special instructions were received'