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_1548088
_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         'C66 H150 Cs2 N10 Si6 U2'
_chemical_formula_sum            'C66 H150 Cs2 N10 Si6 U2'
_chemical_formula_weight         1994.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 100.7821(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.76348(12)
_cell_length_b                   17.09580(9)
_cell_length_c                   22.50605(12)
_cell_measurement_reflns_used    47691
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.3170
_cell_measurement_theta_min      2.5230
_cell_volume                     8603.83(8)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.6296
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -43.00   30.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -150.0000 73
  2 omega  -50.00   33.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -60.0000 83
  3 omega  -90.00  -54.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  120.0000 36
  4 omega  -65.00  -24.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   61.0000 -180.0000 41
  5 omega  -12.00   64.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9304  -57.0000  -90.0000 76
  6 omega   15.00  104.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9304   57.0000   60.0000 89
  7 omega   35.00   97.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -45.0000  120.0000 62
  8 omega   34.00   93.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -45.0000  -90.0000 59
  9 omega   49.00  132.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -77.0000   30.0000 83
 10 omega   48.00   75.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000  150.0000 27
 11 omega   41.00   67.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295 -125.0000 -180.0000 26
 12 omega   92.00  122.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295 -125.0000 -180.0000 30
 13 omega  131.00  169.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   45.0000 -180.0000 38
 14 omega   51.00   81.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000 -180.0000 30
 15 omega   26.00   58.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -94.0000  120.0000 32
 16 omega   57.00  100.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -94.0000 -180.0000 43
 17 omega   25.00   98.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -94.0000  -60.0000 73
 18 omega   30.00   84.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000    0.0000 54
 19 omega   41.00  122.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295 -125.0000   60.0000 81
 20 omega   32.00  101.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -94.0000 -120.0000 69
 21 omega   17.00  171.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295    0.0000    0.0000 154
 22 omega   14.00  107.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9304   57.0000  -60.0000 93
 23 omega  -29.00   64.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9304  -57.0000    0.0000 93
 24 omega   14.00  107.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9304   57.0000 -150.0000 93
 25 omega    9.00  110.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9304   77.0000    0.0000 101
 26 omega  -38.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9304  -19.0000 -120.0000 110
 27 omega   14.00  107.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9304   57.0000  120.0000 93
 28 omega   63.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   15.0000  150.0000 115
 29 omega   80.00  172.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   45.0000  -60.0000 92
 30 omega   77.00  171.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   61.0000 -150.0000 94
 31 omega   73.00  165.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   77.0000  150.0000 92
 32 omega   77.00  171.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   61.0000   30.0000 94
;
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0541585000
_diffrn_orient_matrix_UB_12      -0.0404534000
_diffrn_orient_matrix_UB_13      -0.0393110000
_diffrn_orient_matrix_UB_21      0.0093416000
_diffrn_orient_matrix_UB_22      -0.0717106000
_diffrn_orient_matrix_UB_23      0.0421717000
_diffrn_orient_matrix_UB_31      -0.0415113000
_diffrn_orient_matrix_UB_32      0.0366783000
_diffrn_orient_matrix_UB_33      0.0391437000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60370
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         74.661
_diffrn_reflns_theta_min         3.254
_diffrn_source                   'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.112
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_correction_T_min  0.141
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             3976
_exptl_crystal_size_max          0.2937
_exptl_crystal_size_mid          0.2295
_exptl_crystal_size_min          0.1036
_refine_diff_density_max         2.179
_refine_diff_density_min         -1.894
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8740
_refine_ls_number_restraints     1176
_refine_ls_restrained_S_all      2.187
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0500P)^2^+120.2020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8719
_reflns_number_total             8740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4.cif
_cod_data_source_block           4
_cod_database_code               1548088
_chemical_oxdiff_formula         'C66 H150 N8 Si6 U Cs'
_chemical_oxdiff_usercomment
'UAWAMI #12660 FOR AW/STL ON MICROMOUNT IN FOMBLIN OIL'
_reflns_odcompleteness_completeness 100.00
_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. Restrained distances
 C1A-C2A = C23-C24
 1.55 with sigma of 0.001
 Si3-C26A = Si3-C26
 1.86 with sigma of 0.01
 C25-C23 = C24A-C23A = C25A-C23A = C28-C26 = C28A-C26A = C27A-C26A = C27-C26
 1.55 with sigma of 0.01
 Si1-C5 = Si1-C2 = C2A-C1A = Si1-C3A = Si1-C6 = Si1-C3 = Si3-C25A = Si3-C24A =
 C24-C23 = Si3-C25 = Si3-C27 = C27A-Si3 = C28-Si3 = C28A-Si3 = C28A-C27A = C28-
 C27
 2.8 with sigma of 0.01
 Si1-C4 \\sim Si1-C1 \\sim Si1-C7 \\sim Si2-C15 \\sim Si2-C12 \\sim Si2-C18
\\sim Si3-C23 \\sim Si3-C29 ~
 Si3-C26 \\sim Si1-C1 \\sim Si1-C1A \\sim Si3-C23 \\sim Si3-C23A
 with sigma of 0.01
 C5A-C6A \\sim C17-C16 \\sim C3A-C2A \\sim C8-C9 \\sim C30-C31 \\sim C20-C19
\\sim C5-C6
 with sigma of 0.01
 C6-C4 \\sim C5-C4 \\sim C6A-C4A \\sim C5A-C4A \\sim C20-C18 \\sim C19-C18
\\sim C17-C15 \\sim C16-C15 ~
 C13-C12 \\sim C14-C12 \\sim C28-C26 \\sim C27-C26 \\sim C31-C29 \\sim C30-C29
\\sim C24-C23 \\sim C25-C23
 \\sim C1-C2 \\sim C1-C3 \\sim C1A-C2A \\sim C1A-C3A \\sim C23-C24 \\sim
C23-C25 \\sim C23A-C24A \\sim C23A-C25A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
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(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(H6AC)=1-FVAR(1)
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=FVAR(1)
 Sof(Cs1A)=1-FVAR(2)
 Sof(Cs1)=FVAR(2)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=1-FVAR(3)
 Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H3C)=FVAR(3)
 Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=1-FVAR(4)
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25A)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=FVAR(4)
 Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=
 Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(5)
 Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28A)=
 Sof(H28B)=Sof(H28C)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C1A(H1A), C4(H4), C4A(H4A), C7(H7), C12(H12), C15(H15), C18(H18),
 C23(H23), C23A(H23A), C26(H26), C26A(H26A), C29(H29)
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)
6.c Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC), C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC),
 C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC), C6(H6A,H6B,H6C), C6A(H6AA,H6AB,H6AC),
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C), C24A(H24D,H24E,H24F),
 C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F), C27(H27A,H27B,H27C), C27A(H27D,H27E,
 H27F), C28(H28A,H28B,H28C), C28A(H28D,H28E,H28F), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              93749
_shelx_hkl_checksum              27543
_olex2_submission_special_instructions 'No special instructions were received'