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_1548092
_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         'C41 H91 Li N5 O4 Si3 U'
_chemical_formula_sum            'C41 H91 Li N5 O4 Si3 U'
_chemical_formula_weight         1047.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P -2ac -2n'
_space_group_name_H-M_alt        'P n 21 a'
_symmetry_space_group_name_Hall  'P -2ac -2n'
_symmetry_space_group_name_H-M   'P n 21 a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.55190(20)
_cell_length_b                   13.37345(9)
_cell_length_c                   14.81292(10)
_cell_measurement_reflns_used    13124
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4650
_cell_measurement_theta_min      3.4350
_cell_volume                     5061.83(6)
_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 10.3271
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega  -31.00   12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -120.0000 43
  2 omega    9.00   84.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3823 -125.0000 -180.0000 75
  3 omega   15.00   62.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3823   77.0000    0.0000 47
  4 omega   67.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -94.0000  120.0000 37
  5 omega   30.00   59.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -30.0000  150.0000 29
  6 omega   40.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -45.0000 -180.0000 30
  7 omega   38.00  126.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -77.0000  -30.0000 88
  8 omega   32.00   86.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -30.0000  -90.0000 54
  9 omega   65.00   99.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -45.0000   90.0000 34
 10 omega   10.00  112.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3823   77.0000 -120.0000 102
 11 omega   20.00  111.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3823   38.0000  150.0000 91
 12 omega   82.00  122.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526   30.0000  -60.0000 40
;
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0111271000
_diffrn_orient_matrix_UB_12      -0.0505910000
_diffrn_orient_matrix_UB_13      -0.0914553000
_diffrn_orient_matrix_UB_21      -0.0449890000
_diffrn_orient_matrix_UB_22      -0.0598033000
_diffrn_orient_matrix_UB_23      0.0433378000
_diffrn_orient_matrix_UB_31      -0.0385222000
_diffrn_orient_matrix_UB_32      0.0844719000
_diffrn_orient_matrix_UB_33      -0.0241384000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20152
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.853
_diffrn_reflns_theta_min         3.449
_diffrn_source                   'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.016
_exptl_absorpt_correction_T_max  0.628
_exptl_absorpt_correction_T_min  0.335
_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    1.374
_exptl_crystal_description       block
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.1548
_exptl_crystal_size_mid          0.1186
_exptl_crystal_size_min          0.0912
_refine_diff_density_max         1.683
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.055(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         8470
_refine_ls_number_restraints     1581
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0441P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                8007
_reflns_number_total             8470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            8.cif
_cod_data_source_block           8
_cod_database_code               1548092
_chemical_oxdiff_formula         'C41 H91 N5 Li O4 Si3 U'
_chemical_oxdiff_usercomment
'UDKIOP #12586 IN FOMBLIN FILM ON MICROMOUNT FOR DMK/STL'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.945(7) 0.055(7)
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. Restrained distances
 C6-C4 \\sim C5-C4 \\sim C2-C1 \\sim C3-C1 \\sim C8-C7 \\sim C9-C7 \\sim
C14-C12 \\sim C13-C12 \\sim C20-C18 ~
 C19-C18 \\sim C16-C15 \\sim C17-C15 \\sim C28A-C26A \\sim C27A-C26A \\sim
C24A-C23A \\sim C25A-C23A ~
 C30A-C29A \\sim C31A-C29A \\sim C26-C27
 with sigma of 0.02
 Si3-C23 \\sim Si3-C29 \\sim Si3-C26 \\sim Si1-C7 \\sim Si1-C1 \\sim Si1-C4
\\sim Si2-C12 \\sim Si2-C18 ~
 Si2-C15
 with sigma of 0.02
 C24-C25 \\sim C30-C31 \\sim C5-C6 \\sim C8-C9 \\sim C3-C2 \\sim C14-C13 \\sim
C16-C17 \\sim C19-C20 ~
 C31A-C30A \\sim C24A-C25A \\sim C28A-C27A \\sim C27-C28
 with sigma of 0.02
 C41-C40 \\sim C35-C34 \\sim C37-C36 \\sim C39-C38 \\sim C84-C83 \\sim C90-C89
\\sim C86-C85 \\sim C88-C87
 with sigma of 0.01
 O1-C41 \\sim O4-C40 \\sim O4-C39 \\sim O3-C38 \\sim O3-C37 \\sim O2-C36 \\sim
O2-C35 \\sim O1-C34 \\sim O14-
 C85 \\sim O14-C84 \\sim O13-C83 \\sim O13-C90 \\sim O12-C89 \\sim O12-C88
\\sim O11-C87 \\sim O11-C86
 with sigma of 0.01
 O11-Li1 \\sim O14-Li1 \\sim O13-Li1 \\sim O12-Li1 \\sim O1-Li1 \\sim O2-Li1
\\sim O4-Li1 \\sim O3-Li1
 with sigma of 0.01
 C37-C36 \\sim C39-C38 \\sim C41-C40 \\sim C35-C34 \\sim C90-C89 \\sim C88-C87
\\sim C86-C85 \\sim C84-C83
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Li1 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim C34 \\sim C35 \\sim C36 \\sim C37
\\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim O11 \\sim O12 \\sim O13 \\sim O14
\\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim
C90: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Si3 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim
C30 \\sim C31: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
5. 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
6. Others
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25A)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27D)=
 Sof(H27E)=Sof(H27F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=
 Sof(H29A)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=Sof(H31D)=
 Sof(H31E)=Sof(H31F)=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(O11)=Sof(O12)=Sof(O13)=Sof(O14)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(C84)=
 Sof(H84A)=Sof(H84B)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C86)=Sof(H86A)=Sof(H86B)=
 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(C89)=Sof(H89A)=
 Sof(H89B)=Sof(C90)=Sof(H90A)=Sof(H90B)=1-FVAR(2)
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=
 Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=FVAR(2)
7.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), C23A(H23A), C26A(H26A), C29A(H29A)
7.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),
  C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,
 H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B)
7.c 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), C24A(H24D,H24E,H24F),
 C25A(H25D,H25E,H25F), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F), C30A(H30D,
 H30E,H30F), C31A(H31D,H31E,H31F)
;
_shelx_res_checksum              30041
_shelx_hkl_checksum              51371
_olex2_submission_special_instructions 'No special instructions were received'