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_1548087
_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 N10 Rb2 Si6 U2'
_chemical_formula_sum            'C66 H150 N10 Rb2 Si6 U2'
_chemical_formula_weight         1899.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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                   13.7527(3)
_cell_length_b                   23.1023(5)
_cell_length_c                   26.7606(4)
_cell_measurement_reflns_used    19383
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4840
_cell_measurement_theta_min      4.1050
_cell_volume                     8502.4(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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -49.00   33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  120.0000 82
  2 omega  -92.00   -2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000 -120.0000 90
  3 omega   55.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -77.0000  -30.0000 26
  4 omega   52.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000 -120.0000 37
  5 omega  105.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  125.0000 -150.0000 71
  6 omega   35.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  150.0000 51
  7 omega   33.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000 -150.0000 50
  8 omega   33.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   90.0000 58
  9 omega   21.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.6627   48.0000   15.0000 92
 10 omega   19.00  112.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.6627   57.0000  120.0000 93
 11 omega   83.00  175.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000 -180.0000 92
 12 omega   85.00  161.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   30.0000  -90.0000 76
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            40718
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         74.622
_diffrn_reflns_theta_min         3.303
_exptl_absorpt_coefficient_mu    13.134
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.165
_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_density_diffrn    1.484
_exptl_crystal_description       COLUMN
_exptl_crystal_F_000             3832
_exptl_crystal_size_max          0.2246
_exptl_crystal_size_mid          0.1073
_exptl_crystal_size_min          0.0664
_refine_diff_density_max         2.654
_refine_diff_density_min         -2.380
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7300
_reflns_number_total             8544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3.cif
_cod_data_source_block           3
_cod_original_cell_volume        8502.3(3)
_cod_database_code               1548087
_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.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)
2.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)
2.c Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C19(H19A,H19B,H19C), C25(H25A,H25B,H25C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C)
2.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), 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), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              28537
_shelx_hkl_checksum              16588
_olex2_submission_special_instructions 'No special instructions were received'