Synthesis, Structure, and Reactivity of Uranium(VI) Nitrides
Barluzzi, Luciano; Hsueh, Fang-Che; Scopelliti, Rosario; Atkinson, Benjamin E.; Kaltsoyannis, Nikolas; Mazzanti, Marinella; Chemical Science  (2021) –; doi:10.1039/D1SC01796A

data_1562345
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Uranium(VI) Nitrides
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01796A
_journal_year                    2021
_chemical_formula_moiety         'C44 H97 Cl O14 Si3 U'
_chemical_formula_sum            'C44 H97 Cl O14 Si3 U'
_chemical_formula_weight         1207.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-01-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-03-22 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.2905(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.6881(3)
_cell_length_b                   14.15493(12)
_cell_length_c                   38.5283(4)
_cell_measurement_reflns_used    58783
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      31.3720
_cell_measurement_theta_min      2.9580
_cell_volume                     12855.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (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 10.5633
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.931
_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    -51.00  52.00   1.00   18.00    --   19.91 -19.00 -83.00  103
  2  \w     16.00 100.00   1.00   18.00    --   19.91  19.00  84.00   84
  3  \w    -22.00  60.00   1.00   18.00    --  -20.06  19.00  84.00   82
  4  \w    -93.00 -65.00   1.00   18.00    --  -20.06 -19.00 -83.00   28
  5  \w    -38.00  20.00   1.00   18.00    --   19.91 -77.00 -90.00   58
  6  \w     23.00  49.00   1.00   18.00    --   19.91 -77.00 -90.00   26
  7  \w      1.00  93.00   1.00   18.00    --   19.91  57.00   0.00   92
  8  \w    -92.00 -59.00   1.00   18.00    --  -20.06 150.00-110.76   33
  9  \w    -28.00  49.00   1.00   18.00    --  -20.06  38.00 150.00   77
 10  \w    -42.00  10.00   1.00   18.00    --  -20.06 -77.00 150.00   52
 11  \w    -38.00  13.00   1.00   18.00    --  -20.06 -77.00  30.00   51
 12  \w    -39.00  12.00   1.00   18.00    --  -20.06 -77.00  90.00   51
 13  \w   -109.00 -61.00   1.00   18.00    --  -20.06-178.00  90.00   48
 14  \w    -77.00 -40.00   1.00   18.00    --  -20.06 126.00  38.06   37
 15  \w    -39.00  11.00   1.00   18.00    --  -20.06 -77.00-150.00   50
;
_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      0.0220675000
_diffrn_orient_matrix_UB_12      -0.0235053000
_diffrn_orient_matrix_UB_13      -0.0048591000
_diffrn_orient_matrix_UB_21      0.0138619000
_diffrn_orient_matrix_UB_22      0.0438587000
_diffrn_orient_matrix_UB_23      -0.0000677000
_diffrn_orient_matrix_UB_31      0.0150514000
_diffrn_orient_matrix_UB_32      -0.0059768000
_diffrn_orient_matrix_UB_33      0.0186551000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            166080
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.024
_diffrn_reflns_theta_min         2.871
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.671
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.198
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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            green
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       prism
_exptl_crystal_F_000             4992
_exptl_crystal_size_max          0.662
_exptl_crystal_size_mid          0.479
_exptl_crystal_size_min          0.365
_refine_diff_density_max         1.462
_refine_diff_density_min         -2.753
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.244(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1381
_refine_ls_number_reflns         43877
_refine_ls_number_restraints     1525
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0477P)^2^+22.6682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.877
_reflns_number_gt                40134
_reflns_number_total             43877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01796a2.cif
_cod_data_source_block           lb1156b
_cod_database_code               1562345
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 H105 O15 Si3 Cl1 U1'
_shelx_estimated_absorpt_t_max   0.442
_shelx_estimated_absorpt_t_min   0.271
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.756(4)
 0.244(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C50-C45 \\sim C46-C45 \\sim C49-C45 \\sim C48-C45 \\sim C51-C45 \\sim C47-C45
 with sigma of 0.02
 C46-C47 \\sim C46-C48 \\sim C47-C48 \\sim C49-C50 \\sim C49-C51 \\sim C50-C51
 with sigma of 0.02
 C154-C153 \\sim C155-C153
 with sigma of 0.02
 C112-C111 \\sim C113-C110 \\sim C114-C109
 with sigma of 0.02
 C160-C156 \\sim C157-C156 \\sim C158-C157 \\sim C161-C160 \\sim C159-C158
\\sim C161-C159
 with sigma of 0.02
 C146-C145 \\sim C149-C145 \\sim C150-C149 \\sim C147-C146 \\sim C150-C148
\\sim C148-C147
 with sigma of 0.02
 C102-C105 \\sim C104-C106 \\sim C103-C107
 with sigma of 0.02
 Si6-O107 \\sim Si6-O104 \\sim Si6-O103 \\sim Si6-O106 \\sim Si6-O102 \\sim
Si6-O105
 with sigma of 0.02
 O123-C154 \\sim O123-C155
 with sigma of 0.02
 O107-C115 \\sim O104-C115 \\sim O103-C108 \\sim O106-C108 \\sim O102-C101
\\sim O105-C101
 with sigma of 0.02
 C112-C113 \\sim C113-C114 \\sim C112-C114
 with sigma of 0.02
 C111-C110 \\sim C110-C109 \\sim C109-C111
 with sigma of 0.02
 C105-C106 \\sim C106-C107 \\sim C105-C107
 with sigma of 0.02
 C102-C104 \\sim C104-C103 \\sim C102-C103
 with sigma of 0.02
 C121-C119 \\sim C119-C120 \\sim C121-C120
 with sigma of 0.02
 C102-C101 \\sim C104-C101 \\sim C105-C101 \\sim C103-C101 \\sim C107-C101
\\sim C106-C101 \\sim C112-
 C108 \\sim C111-C108 \\sim C113-C108 \\sim C110-C108 \\sim C109-C108 \\sim
C114-C108 \\sim C119-C115 ~
 C116-C115 \\sim C118-C115 \\sim C121-C115 \\sim C117-C115 \\sim C120-C115
 with sigma of 0.02
 C118-C117 \\sim C117-C116 \\sim C116-C118
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C156 \\sim C157 \\sim C160 \\sim C158 \\sim C161: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
Uanis(C118) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(O105)=Sof(O106)=Sof(O107)=Sof(C105)=Sof(H10J)=Sof(H10K)=Sof(H10L)=
 Sof(C106)=Sof(H10M)=Sof(H10N)=Sof(H10O)=Sof(C107)=Sof(H10P)=Sof(H10Q)=
 Sof(H10R)=Sof(C112)=Sof(H11G)=Sof(H11H)=Sof(H11I)=Sof(C113)=Sof(H11J)=
 Sof(H11K)=Sof(H11L)=Sof(C114)=Sof(H11M)=Sof(H11N)=Sof(H11O)=Sof(C119)=
 Sof(H11Y)=Sof(HC)=Sof(HD)=Sof(C120)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C121)=
 Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(O102)=Sof(O103)=Sof(O104)=Sof(C102)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C103)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C104)=Sof(H10G)=Sof(H10H)=
 Sof(H10I)=Sof(C109)=Sof(H10S)=Sof(H10T)=Sof(H10U)=Sof(C110)=Sof(H11A)=
 Sof(H11B)=Sof(H11C)=Sof(C111)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C116)=
 Sof(H11P)=Sof(H11Q)=Sof(H11R)=Sof(C117)=Sof(H11S)=Sof(H11T)=Sof(H11U)=
 Sof(C118)=Sof(H11V)=Sof(H11W)=Sof(H11X)=FVAR(1)
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=1-FVAR(2)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(2)
 Sof(H15G)=Sof(H15H)=Sof(C155)=Sof(H15K)=Sof(H15L)=1-FVAR(3)
 Sof(H15E)=Sof(H15F)=Sof(C154)=Sof(H15I)=Sof(H15J)=FVAR(3)
 Sof(H14K)=Sof(H14L)=Sof(H14S)=Sof(H14T)=Sof(C149)=Sof(H14U)=Sof(H14V)=
 Sof(C150)=Sof(H15Y)=Sof(HB)=1-FVAR(4)
 Sof(H14I)=Sof(H14J)=Sof(C146)=Sof(H14M)=Sof(H14N)=Sof(C147)=Sof(H14O)=
 Sof(H14P)=Sof(H14Q)=Sof(H14R)=FVAR(4)
 Sof(H15O)=Sof(H15P)=Sof(H15W)=Sof(H15X)=Sof(C160)=Sof(H16A)=Sof(H16B)=
 Sof(C161)=Sof(H16C)=Sof(H16D)=1-FVAR(5)
 Sof(H15M)=Sof(H15N)=Sof(C157)=Sof(H15Q)=Sof(H15R)=Sof(C158)=Sof(H15S)=
 Sof(H15T)=Sof(H15U)=Sof(H15V)=FVAR(5)
 Fixed X: U1(0.382529) U2(0.64505)
 Fixed Y: U1(0.77998) U2(0.60742)
 Fixed Z: U1(0.596459) U2(0.40214)
7.a Secondary CH2 refined with riding coordinates:
 C141(H14A,H14B), C142(H14C,H14D), C143(H14E,H14F), C144(H14G,H14H), C145(H14I,
 H14J), C145(H14K,H14L), C146(H14M,H14N), C147(H14O,H14P), C148(H14Q,H14R),
 C148(H14S,H14T), C149(H14U,H14V), C150(H15Y,HB), C151(H15A,H15B), C152(H15C,
 H15D), C153(H15E,H15F), C153(H15G,H15H), C154(H15I,H15J), C155(H15K,H15L),
 C156(H15M,H15N), C156(H15O,H15P), C157(H15Q,H15R), C158(H15S,H15T), C159(H15U,
 H15V), C159(H15W,H15X), C160(H16A,H16B), C161(H16C,H16D)
7.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10V,H10W,H10X), C11(H11Z,H,HA), C12(H12G,H12H,
 H12I), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C62(H62A,H62B,
 H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C67(H67A,
 H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C),
 C72(H72A,H72B,H72C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,
 H84C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C90(H90A,
 H90B,H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C102(H10A,H10B,H10C),
 C103(H10D,H10E,H10F), C104(H10G,H10H,H10I), C105(H10J,H10K,H10L), C106(H10M,
 H10N,H10O), C107(H10P,H10Q,H10R), C109(H10S,H10T,H10U), C110(H11A,H11B,H11C),
 C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C113(H11J,H11K,H11L), C114(H11M,
 H11N,H11O), C116(H11P,H11Q,H11R), C117(H11S,H11T,H11U), C118(H11V,H11W,H11X),
 C119(H11Y,HC,HD), C120(H12A,H12B,H12C), C121(H12D,H12E,H12F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 312 electrons were 
found in a volume of 1456\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
0.5[C4H8O], 0.5[C4H8O] per Asymmetric Unit 
which account for 320 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              45901
_shelx_hkl_checksum              6188
_shelx_fab_checksum              92015
_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 1.442
_oxdiff_exptl_absorpt_empirical_full_min 0.707