Molecular and electronic structure of terminal and alkali metal-capped uranium(V) nitride complexes
David M. King; Peter A. Cleaves; Ashley J. Wooles; Benedict M. Gardner; Nicholas F. Chilton; Floriana Tuna; William Lewis; Eric J. L. McInnes; Stephen T. Liddle; Nature Communications 7 (2016) 13773–; doi:10.1038/ncomms13773

data_1548091
_publ_section_title
;
 Molecular and electronic structure of terminal and alkali metal-capped
 uranium(V) nitride complexes
;
_journal_name_full               'Nature Communications'
_journal_page_first              13773
_journal_paper_doi               10.1038/ncomms13773
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C33 H75 N5 Si3 U, C28 H40 Cs O10'
_chemical_formula_sum            'C61 H115 Cs N5 O10 Si3 U'
_chemical_formula_weight         1533.78
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.2246(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.09798(19)
_cell_length_b                   18.4937(2)
_cell_length_c                   24.5732(3)
_cell_measurement_reflns_used    24086
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      68.5700
_cell_measurement_theta_min      3.8280
_cell_volume                     7121.71(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_area_resol_mean 8.0750
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -53.00  -26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  150.0000 27
  2 omega  -81.00  -40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  150.0000 41
  3 omega  -45.00   33.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   38.0000  150.0000 78
  4 omega    8.00   33.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   38.0000 -180.0000 25
  5 omega   19.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   82.0000  -44.9794 25
  6 omega   20.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -78.0927 25
  7 omega   19.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   82.0000   82.7798 26
  8 omega   31.00  124.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000    0.0000 93
  9 omega   23.00  104.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000   60.0000 81
 10 omega  -16.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  150.0000 85
 11 omega   50.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000 -150.0000 38
 12 omega   33.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  120.0000 50
 13 omega  126.00  174.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  -90.0000 48
 14 omega   50.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -150.0000 57
 15 omega   37.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 49
 16 omega   78.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 27
 17 omega  120.00  147.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000   90.0000 27
 18 omega   61.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000   90.0000 27
 19 omega   92.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000  -30.0000 48
 20 omega  116.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000    0.0000 62
 21 omega   84.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 94
 22 omega  141.00  167.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 26
 23 omega   88.00  165.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   60.0000 77
 24 omega  109.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000    0.0000 67
 25 omega  -82.00  -34.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -120.0000 48
 26 omega  -51.00   42.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   25.0000  -30.0000 93
 27 omega  -25.00    1.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -79.0000 -150.4036 26
 28 omega   30.00  125.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -120.0000 95
 29 omega   20.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  132.2200 29
 30 omega   20.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   39.5109 29
 31 omega   30.00  125.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -180.0000 95
 32 omega   64.00  173.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000   30.0000 109
 33 omega   75.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 103
 34 omega   35.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   12.0000 -120.0000 143
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0087654000
_diffrn_orient_matrix_UB_12      0.0424051000
_diffrn_orient_matrix_UB_13      -0.0523616000
_diffrn_orient_matrix_UB_21      -0.0650673000
_diffrn_orient_matrix_UB_22      0.0560043000
_diffrn_orient_matrix_UB_23      0.0110095000
_diffrn_orient_matrix_UB_31      0.0731532000
_diffrn_orient_matrix_UB_32      0.0447710000
_diffrn_orient_matrix_UB_33      0.0358478000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            52126
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.407
_diffrn_reflns_theta_min         3.020
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.254
_exptl_absorpt_correction_T_max  1.001
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3140
_exptl_crystal_size_max          0.2261
_exptl_crystal_size_mid          0.0724
_exptl_crystal_size_min          0.0632
_refine_diff_density_max         8.172
_refine_diff_density_min         -4.030
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         13224
_refine_ls_number_restraints     1661
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0635P)^2^+68.4954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11481
_reflns_number_total             13224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            7.cif
_cod_data_source_block           7
_cod_original_cell_volume        7121.73(15)
_cod_database_code               1548091
_chemical_oxdiff_formula         C61H115N5O10Si3CsU
_chemical_oxdiff_usercomment
'UPACLH #12744 in fomblin film on micromount for PAC/STL'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C55-C54 \\sim C49-C48 \\sim C51-C50 \\sim C53-C52 \\sim C35-C34 \\sim C37-C36
\\sim C39-C38 \\sim C41-C40
 with sigma of 0.02
 C3-C1 \\sim C2-C1 \\sim C5A-C4A \\sim C5-C4 \\sim C6-C4 \\sim C6-C4A \\sim
C8-C7 \\sim C9-C7 \\sim C20-C18 ~
 C19-C18 \\sim C13-C12 \\sim C14-C12 \\sim C17-C15 \\sim C17A-C15A \\sim
C16-C15 \\sim C16A-C15A \\sim C31A-
 C29A \\sim C30A-C29A \\sim C31-C29 \\sim C30-C29 \\sim C28-C26 \\sim C27-C26
\\sim C24A-C23A \\sim C25A-
 C23A \\sim C25-C23 \\sim C24-C23 \\sim C28A-C26A \\sim C27A-C26A
 with sigma of 0.02
 Si2-C15 \\sim Si2-C15A \\sim Si2-C18 \\sim Si2-C12 \\sim Si1-C4 \\sim Si1-C7
\\sim Si1-C1 \\sim Si3-C23A
 \\sim Si3-C23 \\sim Si3-C26A \\sim Si3-C26 \\sim Si3-C29A \\sim Si3-C29
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si3 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim
C30 \\sim C31 \\sim C24A \\sim C29A \\sim C30A \\sim C31A \\sim C26A \\sim C27A
\\sim C28A \\sim C23A \\sim C25A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C29A)=Sof(H29A)=Sof(C30A)=
 Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=
 Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=
 Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C23A)=Sof(H23A)=Sof(C25A)=Sof(H25D)=
 Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Sof(H6BD)=Sof(H6BE)=Sof(H6BF)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=
 Sof(H5AC)=1-FVAR(2)
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(H6AA)=Sof(H6AB)=
 Sof(H6AC)=FVAR(2)
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C15A)=Sof(H15A)=Sof(C16A)=
 Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(3)
 Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=
 Sof(H17B)=Sof(H17C)=FVAR(3)
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), C29A(H29A), C26A(H26A), C23A(H23A), C4A(H4A), C15A(H15A)
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), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
  C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,
 H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B)
6.c Me refined with riding coordinates:
 C6(H6AA,H6AB,H6AC), C6(H6BD,H6BE,H6BF)
6.d Aromatic/amide H refined with riding coordinates:
 C43(H43), C44(H44), C45(H45), C46(H46), C57(H57), C58(H58), C59(H59), C60(H60)
6.e Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), 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), C24A(H24D,H24E,H24F), C30A(H30D,H30E,H30F),
 C31A(H31D,H31E,H31F), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F), C25A(H25D,
 H25E,H25F), C5A(H5AA,H5AB,H5AC), C17A(H17D,H17E,H17F), C16A(H16D,H16E,H16F)
;
_shelx_res_checksum              15404
_shelx_hkl_checksum              97441
_olex2_submission_special_instructions 'No special instructions were received'