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_1548093
_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         'C45 H99 N5 O6 Rb1 Si3 U1'
_chemical_formula_sum            'C52.5 H116.5 N5 O6 Rb Si3 U'
_chemical_formula_weight         1321.77
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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            8
_cell_length_a                   23.7586(3)
_cell_length_b                   23.7586(3)
_cell_length_c                   23.7586(3)
_cell_measurement_reflns_used    4588
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4020
_cell_measurement_theta_min      4.5640
_cell_volume                     13411.0(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega  -37.00   15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -150.0000 52
  2 omega   35.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000 -150.0000 52
  3 omega   44.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000    0.0000 54
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0622477000
_diffrn_orient_matrix_UB_12      -0.0052103000
_diffrn_orient_matrix_UB_13      -0.0174467000
_diffrn_orient_matrix_UB_21      0.0088995000
_diffrn_orient_matrix_UB_22      -0.0628997000
_diffrn_orient_matrix_UB_23      -0.0130148000
_diffrn_orient_matrix_UB_31      -0.0158557000
_diffrn_orient_matrix_UB_32      -0.0148862000
_diffrn_orient_matrix_UB_33      0.0610695000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13287
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.506
_diffrn_reflns_theta_min         4.161
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.542
_exptl_absorpt_correction_T_max  0.570
_exptl_absorpt_correction_T_min  0.299
_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    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             5484
_exptl_crystal_size_max          0.4122
_exptl_crystal_size_mid          0.1745
_exptl_crystal_size_min          0.1419
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.538
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4474
_refine_ls_number_restraints     697
_refine_ls_restrained_S_all      2.398
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0699
_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^)+(0.1191P)^2^+36.7738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2120
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3530
_reflns_number_total             4474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            10.cif
_cod_data_source_block           10
_cod_original_cell_volume        13411.0(4)
_cod_original_formula_sum        'C52.50 H116.50 N5 O6 Rb Si3 U'
_cod_database_code               1548093
_chemical_oxdiff_formula         'C78H174 N9 Si6 O6 U Rb'
_chemical_oxdiff_usercomment
'UAWAME #12579 FOR AW/STL ON MICROMOUNT IN FOMBLIN OIL'
_reflns_odcompleteness_completeness 99.61
_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
 C14-C13 = C10-C11 = C15_$1-C12
 1.55 with sigma of 0.01
 N2-C11 = N1-C10 = O1-C12 = O2-C14 = O2-C15 = O1-C13
 1.45 with sigma of 0.01
 N2-C11
 1.45 with sigma of 0.001
 H8AA-H5AC
 -2 with sigma of 0.02
 Si1A-C4A \\sim Si1-C4 \\sim Si1A-C1A \\sim Si1-C1 \\sim Si1A-C7A \\sim Si1-C7
 with sigma of 0.01
 Si1A-N1 \\sim Si1-N1
 with sigma of 0.01
 C2A-C1A \\sim C4A-C5A \\sim C4A-C6A \\sim C7A-C8A \\sim C9A-C7A \\sim C1-C3
\\sim C1-C2 \\sim C6-C4 \\sim C5-
 C4 \\sim C8-C7 \\sim C7-C9
 with sigma of 0.01
 C8A-C9A \\sim C6A-C5A \\sim C2A-C3A \\sim C2-C3 \\sim C9-C8 \\sim C6-C5
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: 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(Si1A)=Sof(C7A)=Sof(H7A)=Sof(C1A)=Sof(H1A)=Sof(C4A)=Sof(H4A)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C6A)=
 Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(Si1)=Sof(C4)=Sof(H4)=Sof(C1)=Sof(H1)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C4(H4), C1(H1), C7(H7), C7A(H7A), C1A(H1A), C4A(H4A)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C14(H14A,H14B), C13(H13A,H13B), C12(H12A,
 H12B), C15(H15A,H15B)
6.c Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C2A(H2AA,H2AB,H2AC), C5A(H5AA,H5AB,H5AC), C8A(H8AA,
 H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C6A(H6AA,H6AB,H6AC), C3A(H3AA,H3AB,H3AC)
;
_shelx_res_checksum              35614
_shelx_hkl_checksum              95250
_shelx_fab_checksum              77031
_olex2_submission_special_instructions 'No special instructions were received'