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_1548090
_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 O10 Rb'
_chemical_formula_sum            'C61 H115 N5 O10 Rb Si3 U'
_chemical_formula_weight         1486.34
_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                 104.2695(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8741(3)
_cell_length_b                   18.5622(3)
_cell_length_c                   24.7397(4)
_cell_measurement_reflns_used    18388
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.1360
_cell_measurement_theta_min      2.8880
_cell_volume                     7064.8(2)
_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)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.6296
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega  -40.00    6.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   30.0000   30.0000 46
  2 omega  -45.00   30.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   45.0000  150.0000 75
  3 omega  -42.00   22.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   30.0000   60.0000 64
  4 omega  -32.00   16.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       39.1804  -38.0000 -180.0000 48
  5 omega   19.00   45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       39.1804  -38.0000 -180.0000 26
  6 omega   55.00   91.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000  120.0000 36
  7 omega   34.00   65.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -45.0000  -60.0000 31
  8 omega   31.00   78.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000 -120.0000 47
  9 omega   50.00  120.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -61.0000  -30.0000 70
 10 omega   31.00   68.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000   30.0000 37
 11 omega   90.00  152.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  101.0000  178.0000 62
 12 omega   17.00   89.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295    0.0000 -180.0000 72
 13 omega  109.00  135.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295    0.0000 -180.0000 26
 14 omega   33.00  120.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295 -125.0000  -60.0000 87
 15 omega    9.00   61.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       39.1804   77.0000 -120.0000 52
;
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0145542000
_diffrn_orient_matrix_UB_12      0.0637130000
_diffrn_orient_matrix_UB_13      -0.0365052000
_diffrn_orient_matrix_UB_21      0.0710158000
_diffrn_orient_matrix_UB_22      0.0297494000
_diffrn_orient_matrix_UB_23      0.0490800000
_diffrn_orient_matrix_UB_31      0.0690586000
_diffrn_orient_matrix_UB_32      -0.0439922000
_diffrn_orient_matrix_UB_33      -0.0198237000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33199
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         74.453
_diffrn_reflns_theta_min         2.872
_diffrn_source                   'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.220
_exptl_absorpt_correction_T_max  0.624
_exptl_absorpt_correction_T_min  0.408
_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    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             3068
_exptl_crystal_size_max          0.1726
_exptl_crystal_size_mid          0.1167
_exptl_crystal_size_min          0.0822
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         14071
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+0.7741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0540
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13145
_reflns_number_total             14071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            6.cif
_cod_data_source_block           6
_cod_database_code               1548090
_chemical_oxdiff_formula         'C61 H115 N4 O5 Si3 Rb U'
_chemical_oxdiff_usercomment
'UAWAMH #12653 FOR AW/STL ON MICROMOUNT IN FOMBLIN OIL'
_reflns_odcompleteness_completeness 99.78
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C14-C12A \\sim C14-C12 \\sim C13A-C12A \\sim C13-C12 \\sim C16-C15 \\sim
C17-C15 \\sim C19-C18 \\sim C20-
 C18
 with sigma of 0.02
3. Others
 Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13D)=
 Sof(H13E)=Sof(H13F)=1-FVAR(1)
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=FVAR(1)
4.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), C12A(H12A)
4.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), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
  C48(H48A,H48B), C49(H49A,H49B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,
 H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B)
4.c Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C14(H14D,H14E,H14F)
4.d Aromatic/amide H refined with riding coordinates:
 C35(H35), C36(H36), C37(H37), C38(H38), C51(H51), C52(H52), C53(H53), C54(H54)
4.e 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), 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), C13A(H13D,H13E,H13F)
;
_shelx_res_checksum              6128
_shelx_hkl_checksum              38246
_olex2_submission_special_instructions 'No special instructions were received'