C-H Bond Activation by an Isolated Dinuclear U(III)/U(IV) Nitride.
Palumbo, Chad T.; Scopelliti, Rosario; Zivkovic, Ivica; Mazzanti, Marinella; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b12804

data_4134068
_publ_section_title
;
 C-H Bond Activation by an Isolated Dinuclear U(III)/U(IV) Nitride.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12804
_journal_year                    2020
_chemical_formula_moiety         'C32 H88 N5 O2 Si8 U2'
_chemical_formula_sum            'C32 H88 N5 O2 Si8 U2'
_chemical_formula_weight         1277.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                119.636(6)
_cell_angle_beta                 90.690(4)
_cell_angle_gamma                102.546(4)
_cell_formula_units_Z            1
_cell_length_a                   10.9866(5)
_cell_length_b                   12.0174(5)
_cell_length_c                   12.0565(7)
_cell_measurement_reflns_used    4995
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      71.7160
_cell_measurement_theta_min      4.1380
_cell_volume                     1337.10(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_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, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -84.00 -16.00   1.00    5.00    --  -40.41 125.00 -90.00   68
  2  \w    -50.00  34.00   1.00    5.00    --  -40.41  38.00 150.00   84
  3  \w    -84.00 -17.00   1.00    5.00    --  -40.41 -57.00-150.00   67
  4  \w   -114.00 -12.00   1.00    5.00    --  -40.41 -57.00   0.00  102
  5  \w     26.00  72.00   1.00    5.00    --   40.41 -77.00 120.00   46
  6  \w    153.00 178.00   1.00   20.00    --  107.03  61.00  30.00   25
  7  \w     96.00 160.00   1.00   20.00    --  107.03 125.00   0.00   64
  8  \w     85.00 171.00   1.00   20.00    --  107.03  30.00  90.00   86
  9  \w    100.00 170.00   1.00   20.00    --  107.03 125.00  90.00   70
 10  \w     55.00 110.00   1.00   20.00    --  107.03 -94.00   0.00   55
 11  \w     35.00 118.00   1.00   20.00    --  107.03-125.00-120.00   83
 12  \w     81.00 114.00   1.00   20.00    --  107.03  61.00  30.00   33
 13  \w     89.00 130.00   1.00   20.00    --  107.03 -45.00   0.00   41
 14  \w     34.00  81.00   1.00   20.00    --  107.03 -45.00-120.00   47
 15  \w     41.00 139.00   1.00   20.00    --  107.03 -77.00  60.00   98
 16  \w     36.00  63.00   1.00   20.00    --  107.03 -45.00   0.00   27
 17  \w     95.00 129.00   1.00   20.00    --  107.03 -45.00-120.00   34
 18  \w     72.00 118.00   1.00   20.00    --  107.03-125.00 -60.00   46
 19  \w     79.00 177.00   1.00   20.00    --  107.03  30.00-180.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1296946000
_diffrn_orient_matrix_UB_12      0.0735078000
_diffrn_orient_matrix_UB_13      -0.0089398000
_diffrn_orient_matrix_UB_21      0.0228957000
_diffrn_orient_matrix_UB_22      0.0914597000
_diffrn_orient_matrix_UB_23      0.1476165000
_diffrn_orient_matrix_UB_31      0.0608973000
_diffrn_orient_matrix_UB_32      -0.0975700000
_diffrn_orient_matrix_UB_33      0.0133545000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8954
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.477
_diffrn_reflns_theta_min         4.164
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.860
_exptl_absorpt_correction_T_max  0.673
_exptl_absorpt_correction_T_min  0.213
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018).
 Analytical numeric absorption correction using a multifaceted crystal
 model based on expressions derived by R.C. Clark & J.S. Reid.
 (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
 Empirical absorption correction using spherical harmonics as 
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       plate
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.022
_refine_diff_density_max         3.809
_refine_diff_density_min         -2.733
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5181
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0993P)^2^+2.8294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4879
_reflns_number_total             5181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12804_si_005.cif
_cod_data_source_block           ctp447_2
_cod_original_cell_volume        1337.10(13)
_cod_database_code               4134068
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C32 H88.16 N5.08 O2 Si8 U2'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1B-C15B = O1B-C14B
 2.375 with sigma of 0.04
 C15B-C14B
 1.536 with sigma of 0.02
 O1B-C16B = O1B-C13B
 1.436 with sigma of 0.02
 C16B-C15B = C14B-C13B
 1.532 with sigma of 0.02
 C16B-C14B = C15B-C13B
 2.38 with sigma of 0.04
 O1A-C16A = O1A-C13A
 1.436 with sigma of 0.02
 O1A-C15A = O1A-C14A
 2.375 with sigma of 0.04
 C16A-C15A = C14A-C13A
 1.532 with sigma of 0.02
 C16A-C14A = C15A-C13A
 2.38 with sigma of 0.04
 C15A-C14A
 1.536 with sigma of 0.02
 U1-O1B \\sim U1-O1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C2A \\sim C2B \\sim C3A \\sim C3B \\sim C4 \\sim C5 \\sim
C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13A \\sim
C13B \\sim C14A \\sim C14B \\sim C15A \\sim C15B \\sim C16A \\sim C16B \\sim
O1A \\sim O1B \\sim N1 \\sim N2 \\sim N3: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(Si1B)=Sof(O1B)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=
 Sof(H2BC)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=Sof(C13B)=Sof(H13C)=Sof(H13D)=
 Sof(C14B)=Sof(H14C)=Sof(H14D)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(C16B)=
 Sof(H16C)=Sof(H16D)=1-FVAR(1)
 Sof(Si1A)=Sof(O1A)=Sof(N1)=Sof(H1)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=
 Sof(H15A)=Sof(H15B)=Sof(C16A)=Sof(H16A)=Sof(H16B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C13A(H13A,H13B), C13B(H13C,H13D), C14A(H14A,H14B), C14B(H14C,
 H14D), C15A(H15A,H15B), C15B(H15C,H15D), C16A(H16A,H16B), C16B(H16C,H16D)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1)
5.c Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C2B(H2BA,H2BB,H2BC), C3A(H3AA,H3AB,
 H3AC), C3B(H3BA,H3BB,H3BC), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C),
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.363
_oxdiff_exptl_absorpt_empirical_full_min 0.379