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_4121637
_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         'C33 H76 N5 Si3 U, C20 H40 K O10'
_chemical_formula_sum            'C53 H116 K N5 O10 Si3 U'
_chemical_formula_weight         1344.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.1694(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.1227(4)
_cell_length_b                   20.4398(3)
_cell_length_c                   24.3891(4)
_cell_measurement_reflns_used    24940
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.2040
_cell_measurement_theta_min      2.7120
_cell_volume                     13264.8(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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-2013 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0120620000
_diffrn_orient_matrix_UB_12      -0.0477497000
_diffrn_orient_matrix_UB_13      0.0444812000
_diffrn_orient_matrix_UB_21      -0.0356744000
_diffrn_orient_matrix_UB_22      0.0510081000
_diffrn_orient_matrix_UB_23      0.0177907000
_diffrn_orient_matrix_UB_31      -0.0439614000
_diffrn_orient_matrix_UB_32      -0.0283110000
_diffrn_orient_matrix_UB_33      -0.0429978000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            56550
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.626
_diffrn_reflns_theta_min         2.726
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.386
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             5616
_exptl_crystal_size_max          0.1295
_exptl_crystal_size_mid          0.0725
_exptl_crystal_size_min          0.0596
_refine_diff_density_max         1.367
_refine_diff_density_min         -1.603
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         13414
_refine_ls_number_restraints     572
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+22.4848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11125
_reflns_number_total             13414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja502405e_si_002.cif
_cod_data_source_block           3c
_cod_depositor_comments
'Adding full bibliography for 4121632--4121637.cif.'
_cod_original_cell_volume        13264.8(3)
_cod_database_code               4121637
_nottingham_internal_coll_name   UDKIPR
_nottingham_internal_coll_number 13210
_nottingham_internal_coll_client DMK/STL
_nottingham_internal_coll_type   sphere
_nottingham_internal_coll_frame_time '10.0000 and 40.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   DMK/WL
_nottingham_internal_coll_date   6/02/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user DMK/WL
_nottingham_internal_process_date 07/02/2014
_nottingham_internal_solution_user DMK/WL
_nottingham_internal_solution_date 07/02/2014
_nottingham_internal_refinement_user DMK/WL
_nottingham_internal_refinement_date 07/02/2014
_nottingham_internal_self_validation_user DMK
_nottingham_internal_self_validation_date 07/02/2014
_nottingham_internal_self_archive_date 07/02/2014
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C53 H116 N5 K O10 Si3 U'
_chemical_oxdiff_usercomment
'UDKIPR #13210 IN FOMBLIN FILM ON MICROMOUNT FOR DMK/STL GVB-7'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 H5-N5
 0.94 with sigma of 0.01
 H5-U1
 3.06 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O6 \\sim C45 \\sim O7 \\sim O8 \\sim C53 \\sim C46 \\sim C44 \\sim C47 \\sim
C52 \\sim C51 \\sim C48 \\sim C50 \\sim C49 \\sim O10 \\sim O9 \\sim O6A \\sim
C45A \\sim O7A \\sim O8A \\sim C53A \\sim C46A \\sim C44A \\sim C47A \\sim C52A
\\sim C51A \\sim C50 \\sim C49 \\sim C49A \\sim O10A \\sim O9A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O6, C45, O7, O8, C53, C46, C44, C47, C52, C51, C48, C50, C49, O10, O9, O6A,
 C45A, O7A, O8A, C53A, C46A, C44A, C47A, C52A, C51A, C50, C49, C49A, O10A, O9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O6A)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=Sof(C44A)=Sof(H44C)=Sof(H44D)=
 Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C47A)=
 Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(C49A)=Sof(H49C)=
 Sof(H49D)=Sof(C50A)=Sof(H50C)=Sof(H50D)=Sof(C51A)=Sof(H51C)=Sof(H51D)=
 Sof(C52A)=Sof(H52C)=Sof(H52D)=Sof(C53A)=Sof(H53C)=Sof(H53D)=1-FVAR(1)
 Sof(O6)=Sof(O7)=Sof(O8)=Sof(O9)=Sof(O10)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=
 Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=
 Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=
 Sof(C53)=Sof(H53A)=Sof(H53B)=FVAR(1)
6.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)
6.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),
  C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C44A(H44C,H44D), C45(H45A,
 H45B), C45A(H45C,H45D), C46(H46A,H46B), C46A(H46C,H46D), C47(H47A,H47B),
 C47A(H47C,H47D), C48(H48A,H48B), C48A(H48C,H48D), C49(H49A,H49B), C49A(H49C,
 H49D), C50(H50A,H50B), C50A(H50C,H50D), C51(H51A,H51B), C51A(H51C,H51D),
 C52(H52A,H52B), C52A(H52C,H52D), C53(H53A,H53B), C53A(H53C,H53D)
6.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)
;