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_4134067
_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
'C55 H154 N10 Si16 U4, C32 H88 N5 O2 Si8 U2,0.8[C7H8],0.6[C6H14]'
_chemical_formula_sum            'C87 H242 N15 O2 Si24 U6'
_chemical_formula_weight         3633.28
_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             2019-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                85.1695(17)
_cell_angle_beta                 76.7807(18)
_cell_angle_gamma                68.9745(19)
_cell_formula_units_Z            2
_cell_length_a                   20.4459(4)
_cell_length_b                   20.6717(4)
_cell_length_c                   20.7789(4)
_cell_measurement_reflns_used    22062
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.3830
_cell_measurement_theta_min      3.7810
_cell_volume                     7980.3(3)
_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, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.968
_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   -115.00 -23.00   1.00    7.50    --  -43.01 -57.00-120.00   92
  2  \w    -71.00  21.00   1.00    7.50    --  -43.01  57.00  30.00   92
  3  \w   -119.00 -88.00   1.00    7.50    --  -43.01 -99.00  30.00   31
  4  \w    -89.00 -17.00   1.00    7.50    --  -43.01 125.00  90.00   72
  5  \w   -112.00 -83.00   1.00    7.50    --  -43.01 -99.00 -30.00   29
  6  \w   -120.00 -95.00   1.00    7.50    --  -43.01 -99.00 -90.00   25
  7  \w    104.00 172.00   1.00   30.00    --  105.68  77.00 150.00   68
  8  \w     37.00 118.00   1.00   30.00    --  105.68-125.00  30.00   81
  9  \w     53.00 121.00   1.00   30.00    --  105.68 -77.00   0.00   68
 10  \w     41.00 118.00   1.00   30.00    --  105.68 -45.00   0.00   77
 11  \w     37.00 127.00   1.00   30.00    --  105.68 -45.00  90.00   90
 12  \w     30.00  56.00   1.00   30.00    --  105.68 -94.00-120.00   26
 13  \w     72.00 117.00   1.00   30.00    --  105.68-125.00-180.00   45
 14  \w     34.00 115.00   1.00   30.00    --  105.68 -45.00-150.00   81
 15  \w     52.00  77.00   1.00   30.00    --  105.68 -94.00 -60.00   25
 16  \w     57.00 102.00   1.00   30.00    --  105.68 -94.00-150.00   45
 17  \w     84.00 109.00   1.00   30.00    --  105.68 -94.00-120.00   25
 18  \w     19.00 164.00   1.00   30.00    --  105.68   0.00 -30.00  145
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0755178000
_diffrn_orient_matrix_UB_12      -0.0516345000
_diffrn_orient_matrix_UB_13      -0.0280277000
_diffrn_orient_matrix_UB_21      0.0147822000
_diffrn_orient_matrix_UB_22      0.0551910000
_diffrn_orient_matrix_UB_23      -0.0499105000
_diffrn_orient_matrix_UB_31      0.0300917000
_diffrn_orient_matrix_UB_32      0.0257378000
_diffrn_orient_matrix_UB_33      0.0502350000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57518
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.676
_diffrn_reflns_theta_min         3.550
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.908
_exptl_absorpt_correction_T_max  0.588
_exptl_absorpt_correction_T_min  0.107
_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,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       plate
_exptl_crystal_F_000             3546
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.580
_refine_diff_density_min         -1.863
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1379
_refine_ls_number_reflns         31207
_refine_ls_number_restraints     325
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+10.0662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26270
_reflns_number_total             31207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12804_si_008.cif
_cod_data_source_block           ctp420_2
_cod_database_code               4134067
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C96.20 H256.80 N15 O2 Si24 U6'
_reflns_odcompleteness_completeness 99.87
_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, All N(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
 Si3A-C21 \\sim Si3A-C22A \\sim Si3A-C23A \\sim Si3B-C21 \\sim Si3B-C23B \\sim
Si3B-C22B
 with sigma of 0.02
 C22A-C23A \\sim C23A-C21 \\sim C21-C22A
 with sigma of 0.02
 Si16-C95 \\sim Si16-C96 \\sim Si16-C94 \\sim Si3-C111 \\sim Si3-C96 \\sim
Si3-C6AA
 with sigma of 0.02
 Si17-N10 \\sim Si18-N10
 with sigma of 0.02
 Si17-C101 \\sim Si17-C103 \\sim Si17-C102 \\sim Si18-C109 \\sim Si18-C108
\\sim Si18-C110
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si3A \\sim Si3B \\sim C21 \\sim C22A \\sim C22B \\sim C23A \\sim C23B: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01
Si3 \\sim Si16 \\sim Si17 \\sim Si18 \\sim C6AA \\sim C94 \\sim C95 \\sim C96
\\sim C101 \\sim C102 \\sim C103 \\sim C108 \\sim C109 \\sim C110 \\sim C111:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O1 \\sim O2 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim
C57 \\sim C58: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
4. Others
 Sof(Si3)=Sof(Si18)=Sof(C6AA)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(H96D)=
 Sof(H96E)=Sof(H96F)=Sof(C108)=Sof(H10S)=Sof(H10T)=Sof(H10U)=Sof(C109)=
 Sof(H10V)=Sof(H10W)=Sof(H10X)=Sof(C110)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C111)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(Si16)=Sof(Si17)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=Sof(C95)=Sof(H95A)=
 Sof(H95B)=Sof(H95C)=Sof(H96A)=Sof(H96B)=Sof(H96C)=Sof(C101)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=Sof(C102)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C103)=
 Sof(H10G)=Sof(H10H)=Sof(H10I)=FVAR(1)
 Sof(Si3B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22B)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(2)
 Sof(Si3A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22A)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B)
5.b Aromatic/amide H refined with riding coordinates:
 N11(H11), N111(H111), C151(H151), C152(H152), C153(H153), C154(H154),
 C155(H155)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C21(H21A,H21B,H21C), C21(H21D,H21E,H21F), C22A(H22A,
 H22B,H22C), C22B(H22D,H22E,H22F), C23A(H23A,H23B,H23C), C23B(H23D,H23E,H23F),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C6AA(H6AA,H6AB,H6AC), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,
 H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C81(H81A,H81B,H81C),
 C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,
 H85C), C86(H86A,H86B,H86C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C93(H93A,
 H93B,H93C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C),
 C96(H96D,H96E,H96F), C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C103(H10G,
 H10H,H10I), C104(H10J,H10K,H10L), C105(H10M,H10N,H10O), C106(H10P,H10Q,H10R),
 C108(H10S,H10T,H10U), C109(H10V,H10W,H10X), C110(H11A,H11B,H11C), C111(H11D,
 H11E,H11F), C120(H12A,H12B,H12C), C121(H12D,H12E,H12F), C122(H12G,H12H,H12I),
 C123(H12J,H12K,H12L), C124(H12M,H12N,H12O), C125(H12P,H12Q,H12R), C130(H13A,
 H13B,H13C), C131(H13D,H13E,H13F), C132(H13G,H13H,H13I), C133(H13J,H13K,H13L),
 C134(H13M,H13N,H13O), C135(H13P,H13Q,H13R), C140(H14A,H14B,H14C), C141(H14D,
 H14E,H14F), C142(H14G,H14H,H14I), C143(H14J,H14K,H14L), C144(H14M,H14N,H14O),
 C145(H14P,H14Q,H14R), C156(H15A,H15B,H15C)
;
_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 1.614
_oxdiff_exptl_absorpt_empirical_full_min 0.656