Photochemical Synthesis of a Stable Terminal Uranium(VI) Nitride
Barluzzi, Luciano; Scopelliti, Rosario; Mazzanti, Marinella; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c09814

data_4135320
_publ_section_title
;
 Photochemical Synthesis of a Stable Terminal Uranium(VI) Nitride
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c09814
_journal_year                    2020
_chemical_formula_moiety         'C66 H144 K N5 O22 Si4 U, 0.5[C6H14]'
_chemical_formula_sum            'C66 H144 K N5 O22 Si4 U'
_chemical_formula_weight         1749.34
_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             2020-08-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                90.6362(19)
_cell_angle_beta                 93.3686(18)
_cell_angle_gamma                91.8783(17)
_cell_formula_units_Z            4
_cell_length_a                   14.2473(3)
_cell_length_b                   24.0781(5)
_cell_length_c                   27.7546(7)
_cell_measurement_reflns_used    27645
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      28.3320
_cell_measurement_theta_min      3.1080
_cell_volume                     9498.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.76a (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 2018/2 (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 0.997
_diffrn_measured_fraction_theta_max 0.998
_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   -107.00 -70.00   1.00   30.00    --  -17.94-178.00 -90.00   37
  2  \w    -33.00   8.00   1.00   30.00    --  -17.94 -77.00  60.00   41
  3  \w    -35.00  12.00   1.00   30.00    --  -17.94 -77.00-120.00   47
  4  \w    -15.00  25.00   1.00   30.00    --   18.87 -99.00 120.00   40
  5  \w     17.00  58.00   1.00   30.00    --   18.87 -99.00-150.00   41
  6  \w     13.00  44.00   1.00   30.00    --   18.87 -99.00  60.00   31
  7  \w     -5.00  22.00   1.00   30.00    --   18.87 -77.00 -90.00   27
  8  \w    -66.00 107.00   1.00   30.00    --   18.87   0.00 120.00  173
;
_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      0.0069139000
_diffrn_orient_matrix_UB_12      0.0211531000
_diffrn_orient_matrix_UB_13      0.0179679000
_diffrn_orient_matrix_UB_21      0.0002442000
_diffrn_orient_matrix_UB_22      -0.0204440000
_diffrn_orient_matrix_UB_23      0.0182069000
_diffrn_orient_matrix_UB_31      0.0494173000
_diffrn_orient_matrix_UB_32      -0.0018617000
_diffrn_orient_matrix_UB_33      -0.0010744000
_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  0.0462
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            94947
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.916
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.863
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.41.76a (Rigaku Oxford Diffraction, 2020)
 Numerical absorption correction based on Gaussian integration over
 a multifaceted crystal model.
 Empirical absorption correction using spherical harmonics
 as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       prism
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.431
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.798
_refine_diff_density_min         -1.404
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1934
_refine_ls_number_reflns         38753
_refine_ls_number_restraints     2912
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0424P)^2^+30.1188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28182
_reflns_number_total             38753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c09814_si_003.cif
_cod_data_source_block           lb1010
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        9498.7(4)
_cod_database_code               4135320
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C67.50 H147 K N5 O22 Si4 U'
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.501
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si4-O63A \\sim Si4-O63B \\sim Si4-O62A \\sim Si4-O62B
 with sigma of 0.02
 C63A-C61 \\sim C63B-C61 \\sim C62A-C61 \\sim C62B-C61 \\sim C64A-C61 \\sim
C64B-C61
 with sigma of 0.02
 C51A-C50A \\sim C50A-C52A \\sim C52A-C51A \\sim C52B-C51B \\sim C51B-C50B
\\sim C50B-C52B
 with sigma of 0.02
 C51A-C49 \\sim C50A-C49 \\sim C52A-C49 \\sim C52B-C49 \\sim C51B-C49 \\sim
C50B-C49
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O41
\\sim O42 \\sim O43 \\sim O44 \\sim O61 \\sim O62A \\sim O62B \\sim O63A \\sim
O63B \\sim O64 \\sim O161 \\sim O162 \\sim O163 \\sim O164 \\sim O165 \\sim
O166 \\sim O81 \\sim O82 \\sim O83 \\sim O84 \\sim O101 \\sim O102 \\sim O103
\\sim O104 \\sim O121 \\sim O122 \\sim O123 \\sim O124 \\sim O141 \\sim O142
\\sim O143 \\sim O144 \\sim O181 \\sim O182 \\sim O183 \\sim O184 \\sim O185
\\sim O186 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim
C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C21 \\sim C22 \\sim C23 \\sim
C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim
C32 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim
C48 \\sim C49 \\sim C50A \\sim C50B \\sim C51A \\sim C51B \\sim C52A \\sim C52B
\\sim C61 \\sim C62A \\sim C62B \\sim C63A \\sim C63B \\sim C64A \\sim C64B
\\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72
\\sim C161 \\sim C162 \\sim C163 \\sim C164 \\sim C165 \\sim C166 \\sim C167
\\sim C168 \\sim C169 \\sim C170 \\sim C171 \\sim C172 \\sim C173 \\sim C174
\\sim C175 \\sim C176 \\sim C177 \\sim C178 \\sim C81 \\sim C82 \\sim C83 \\sim
C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim C91 \\sim
C92 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim
C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111 \\sim C112 \\sim C121 \\sim
C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim C127 \\sim C128 \\sim
C129 \\sim C130 \\sim C131 \\sim C132 \\sim C141 \\sim C142 \\sim C143 \\sim
C144 \\sim C145 \\sim C146 \\sim C147 \\sim C148 \\sim C149 \\sim C150 \\sim
C151 \\sim C152 \\sim C181 \\sim C182 \\sim C183 \\sim C184 \\sim C185 \\sim
C186 \\sim C187 \\sim C188 \\sim C189 \\sim C190 \\sim C191 \\sim C192 \\sim
C193 \\sim C194 \\sim C195 \\sim C196 \\sim C197 \\sim C198: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O62B)=Sof(O63B)=Sof(C50B)=Sof(H50D)=Sof(H50E)=Sof(H50F)=Sof(C51B)=
 Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52B)=Sof(H52D)=Sof(H52E)=Sof(H52F)=
 Sof(C62B)=Sof(H62D)=Sof(H62E)=Sof(H62F)=Sof(C63B)=Sof(H63D)=Sof(H63E)=
 Sof(H63F)=Sof(C64B)=Sof(H64D)=Sof(H64E)=Sof(H64F)=1-FVAR(1)
 Sof(O62A)=Sof(O63A)=Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51A)=
 Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=
 Sof(C62A)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C63A)=Sof(H63A)=Sof(H63B)=
 Sof(H63C)=Sof(C64A)=Sof(H64A)=Sof(H64B)=Sof(H64C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C161(H16A,H16B), C162(H16C,H16D), C163(H16E,H16F), C164(H16G,H16H), C165(H16I,
 H16J), C166(H16K,H16L), C167(H16M,H16N), C168(H16O,H16P), C169(H16Q,H16R),
 C170(H17A,H17B), C171(H17C,H17D), C172(H17E,H17F), C173(H17G,H17H), C174(H17I,
 H17J), C175(H17K,H17L), C176(H17M,H17N), C177(H17O,H17P), C178(H17Q,H17R),
 C181(H18A,H18B), C182(H18C,H18D), C183(H18E,H18F), C184(H18G,H18H), C185(H18I,
 H18J), C186(H18K,H18L), C187(H18M,H18N), C188(H18O,H18P), C189(H18Q,H18R),
 C190(H19A,H19B), C191(H19C,H19D), C192(H19E,H19F), C193(H19G,H19H), C194(H19I,
 H19J), C195(H19K,H19L), C196(H19M,H19N), C197(H19O,H19P), C198(H19Q,H19R)
6.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(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), 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), C50A(H50A,H50B,H50C), C50B(H50D,H50E,H50F), C51A(H51A,
 H51B,H51C), C51B(H51D,H51E,H51F), C52A(H52A,H52B,H52C), C52B(H52D,H52E,H52F),
 C62A(H62A,H62B,H62C), C62B(H62D,H62E,H62F), C63A(H63A,H63B,H63C), C63B(H63D,
 H63E,H63F), C64A(H64A,H64B,H64C), C64B(H64D,H64E,H64F), 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(H10D,H10E,
 H10F), C103(H10G,H10H,H10I), C104(H10J,H10K,H10L), C106(H10M,H10N,H10O),
 C107(H10P,H10Q,H10R), C108(H10S,H10T,H10U), C110(H11D,H11E,H11F), C111(H11G,
 H11H,H11I), C112(H11J,H11K,H11L), C122(H12D,H12E,H12F), C123(H12G,H12H,H12I),
 C124(H12J,H12K,H12L), C126(H12M,H12N,H12O), C127(H12P,H12Q,H12R), C128(H12S,
 H12T,H12U), C130(H13A,H13B,H13C), C131(H13D,H13E,H13F), C132(H13G,H13H,H13I),
 C142(H14A,H14B,H14C), C143(H14D,H14E,H14F), C144(H14G,H14H,H14I), C146(H14J,
 H14K,H14L), C147(H14M,H14N,H14O), C148(H14P,H14Q,H14R), C150(H15A,H15B,H15C),
 C151(H15D,H15E,H15F), C152(H15G,H15H,H15I)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37624
_shelx_hkl_checksum              91297
_shelx_fab_checksum              52239
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.165
_oxdiff_exptl_absorpt_empirical_full_min 0.891