Synthesis and Characterization of an f-Block Terminal Parent Imido [U═NH] Complex: A Masked Uranium(IV) Nitride.
King, David M.; McMaster, Jonathan; Tuna, Floriana; McInnes, Eric J. L.; Lewis, William; Blake, Alexander J.; Liddle, Stephen T.; Journal of the American Chemical Society 136 (2014) 5619–; doi:10.1021/ja502405e

data_4121635
_publ_section_title
;
 Synthesis and Characterization of an f-Block Terminal Parent Imido
 [U&#x2550;NH] Complex: A Masked Uranium(IV) Nitride.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5619
_journal_paper_doi               10.1021/ja502405e
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C66 H152 N10 Rb2 Si6 U2'
_chemical_formula_sum            'C66 H152 N10 Rb2 Si6 U2'
_chemical_formula_weight         1901.51
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-13
_audit_creation_method
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Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7768(2)
_cell_length_b                   23.1164(4)
_cell_length_c                   26.8905(5)
_cell_measurement_reflns_used    5320
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.3720
_cell_measurement_theta_min      3.2660
_cell_volume                     8563.8(3)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_reduction
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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, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
  1 omega  -48.00  -15.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   19.0000  -30.0000 33

  2 omega  -31.00   60.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       39.1804  -38.0000   60.0000 91

  3 omega   82.00  173.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   30.0000    0.0000 91

  4 omega   50.00  122.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295 -125.0000 -180.0000 72

  5 omega   31.00   59.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000 -180.0000 28

  6 omega   42.00  102.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -94.0000  -90.0000 60
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0140542000
_diffrn_orient_matrix_UB_12      0.0579295000
_diffrn_orient_matrix_UB_13      0.0273589000
_diffrn_orient_matrix_UB_21      0.0265343000
_diffrn_orient_matrix_UB_22      -0.0328373000
_diffrn_orient_matrix_UB_23      0.0479887000
_diffrn_orient_matrix_UB_31      0.1077629000
_diffrn_orient_matrix_UB_32      0.0006604000
_diffrn_orient_matrix_UB_33      -0.0152689000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            19617
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.597
_diffrn_reflns_theta_min         3.287
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    13.040
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_correction_T_min  0.468
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.0907
_exptl_crystal_size_mid          0.0684
_exptl_crystal_size_min          0.058
_refine_diff_density_max         1.702
_refine_diff_density_min         -2.325
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8413
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0397P)^2^+28.3056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5777
_reflns_number_total             8413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja502405e_si_002.cif
_cod_data_source_block           2d
_cod_depositor_comments
'Adding full bibliography for 4121632--4121637.cif.'
_cod_original_cell_volume        8563.9(3)
_cod_database_code               4121635
_nottingham_internal_coll_name   UDKIOV
_nottingham_internal_coll_number 12729
_nottingham_internal_coll_client DK/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time 8+24
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   DMK
_nottingham_internal_coll_date   16/08/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user DMK
_nottingham_internal_process_date 28/08/2013
_nottingham_internal_solution_user DMK
_nottingham_internal_solution_date 28/08/2013
_nottingham_internal_refinement_user DMK
_nottingham_internal_refinement_date 28/08/2013
_nottingham_internal_self_validation_user DMK
_nottingham_internal_self_validation_date 14/02/2014
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C66 H152 N10 Si6 Rb2 U2'
_chemical_oxdiff_usercomment
'UDKIOV #12729 IN FOMBLIN FILM ON MICROMOUNT FOR DMK/STL'
_reflns_odcompleteness_completeness 98.59
_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 N(H) groups
2. Restrained distances
 N5-H5
 0.98 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C17 \\sim C15 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
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)
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)
4.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)
;