Nitride Protonation and NH3 Binding versus N‒H Bond Cleavage in Uranium Nitrides
Keener, Megan; Scopelliti, Rosario; Mazzanti, Marinella; Chemical Science  (2021) –; doi:10.1039/D1SC03957A

data_1564372
_publ_section_title
;
 Nitride Protonation and NH3 Binding versus N--H Bond Cleavage in Uranium
 Nitrides
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03957A
_journal_year                    2021
_chemical_formula_moiety         'C72 H162 N4 O24 Si6 U2, 2[C4H8O]'
_chemical_formula_sum            'C72 H172 N4 O24 Si6 U2'
_chemical_formula_weight         2122.73
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-05-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-16 deposited with the CCDC.	2021-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                106.7988(13)
_cell_angle_beta                 114.1561(17)
_cell_angle_gamma                91.4673(12)
_cell_formula_units_Z            1
_cell_length_a                   14.2581(2)
_cell_length_b                   14.80263(18)
_cell_length_c                   15.5045(3)
_cell_measurement_reflns_used    36457
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.6060
_cell_measurement_theta_min      3.7170
_cell_volume                     2819.33(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_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 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_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    -78.00   4.00   1.00    1.00    --  -40.91 112.00 135.00   82
  2  \w     18.00  84.00   1.00    1.00    --   40.91-112.00  42.00   66
  3  \w    108.00 142.00   1.00    4.00    --  105.15 112.00 135.00   34
  4  \w     46.00 105.00   1.00    4.00    --  105.15-112.00  42.00   59
  5  \w      1.00  29.00   1.00    1.00    --   38.00  90.00 -89.10   28
  6  \w   -115.00 -16.00   1.00    1.00    --  -40.91 -38.00 150.00   99
  7  \w   -114.00 -16.00   1.00    1.00    --  -40.91 -38.00 -60.00   98
  8  \w   -112.00 -13.00   1.00    1.00    --  -40.91 -57.00  60.00   99
  9  \w      9.00  34.00   1.00    1.00    --   40.91  75.00 104.57   25
 10  \w      6.00  82.00   1.00    1.00    --   40.91 -99.00 -30.00   76
 11  \w     16.00  41.00   1.00    1.00    --   50.00  81.00 -38.42   25
 12  \w     16.00  42.00   1.00    1.00    --   50.00  81.00-154.98   26
 13  \w     16.00  41.00   1.00    1.00    --   50.00  82.00  73.24   25
 14  \w     16.00  41.00   1.00    1.00    --   50.00  82.00-117.79   25
 15  \w     16.00  41.00   1.00    1.00    --   50.00  82.00  10.24   25
 16  \w     16.00  41.00   1.00    1.00    --   50.00  82.00 -79.87   25
 17  \w     16.00  41.00   1.00    1.00    --   50.00  82.00 126.29   25
 18  \w     31.00  57.00   1.00    1.00    --   62.00  69.00   6.81   26
 19  \w     78.00 105.00   1.00    1.00    --   62.00  69.00   6.81   27
 20  \w     36.00  61.00   1.00    1.00    --   66.00  71.00 162.34   25
 21  \w    102.00 131.00   1.00    1.00    --   66.00  71.00 162.34   29
 22  \w     37.00  64.00   1.00    1.00    --   66.00  70.00 -96.71   27
 23  \w    111.00 142.00   1.00    1.00    --   70.00  71.00  56.95   31
 24  \w     99.00 126.00   1.00    1.00    --   70.00  71.00 -76.46   27
 25  \w     40.00  67.00   1.00    1.00    --   70.00  71.00  56.95   27
 26  \w     39.00  65.00   1.00    1.00    --   70.00  69.00 131.48   26
 27  \w     40.00  65.00   1.00    1.00    --   70.00  71.00 -76.46   25
 28  \w     85.00 143.00   1.00    1.00    --   70.00  69.00-131.95   58
 29  \w     40.00  65.00   1.00    1.00    --   70.00  69.00-131.95   25
 30  \w     43.00  71.00   1.00    4.00    --   74.00  71.00  83.95   28
 31  \w     44.00  70.00   1.00    4.00    --   74.00  66.00  -2.65   26
 32  \w     43.00  70.00   1.00    4.00    --   74.00  69.00-176.41   27
 33  \w     47.00  73.00   1.00    4.00    --   78.00  69.00 -48.13   26
 34  \w     47.00  73.00   1.00    4.00    --   78.00  69.00  20.87   26
 35  \w     53.00  80.00   1.00    4.00    --   82.00  59.00-103.64   27
 36  \w     52.00  77.00   1.00    4.00    --   82.00  70.00 -82.57   25
 37  \w    125.00 152.00   1.00    4.00    --   82.00  68.00  55.06   27
 38  \w     53.00  83.00   1.00    4.00    --   82.00  68.00  55.06   30
 39  \w     56.00  99.00   1.00    4.00    --   86.00  68.00 176.08   43
 40  \w     56.00 104.00   1.00    4.00    --   86.00  66.00  16.84   48
 41  \w    109.00 159.00   1.00    4.00    --   86.00  66.00  16.84   50
 42  \w     56.00 100.00   1.00    4.00    --   86.00  65.00 137.89   44
 43  \w     64.00 133.00   1.00    4.00    --   94.00  66.00 140.43   69
 44  \w     77.00 126.00   1.00    4.00    --  105.15  61.00 -90.00   49
 45  \w     79.00 118.00   1.00    4.00    --  105.15  45.00  90.00   39
 46  \w     76.00 174.00   1.00    4.00    --  105.15  61.00 -60.00   98
 47  \w     96.00 137.00   1.00    4.00    --  105.15 -77.00 -30.00   41
 48  \w     75.00 106.00   1.00    4.00    --  105.15  66.00  45.76   31
 49  \w     36.00  68.00   1.00    4.00    --  105.15 -77.00 -30.00   32
 50  \w     78.00 176.00   1.00    4.00    --  105.15  61.00-180.00   98
 51  \w     63.00 106.00   1.00    4.00    --  105.15-111.00 -30.00   43
 52  \w     79.00 106.00   1.00    4.00    --  105.15  61.00 150.00   27
 53  \w     82.00 109.00   1.00    4.00    --  105.15-111.00  90.00   27
 54  \w     32.00  59.00   1.00    4.00    --  105.15-111.00  90.00   27
 55  \w    104.00 162.00   1.00    4.00    --  105.15 111.00-120.00   58
 56  \w    110.00 147.00   1.00    4.00    --  105.15  61.00-120.00   37
 57  \w     77.00 107.00   1.00    4.00    --  105.15  61.00-120.00   30
 58  \w     30.00 109.00   1.00    4.00    --  105.15-111.00-150.00   79
 59  \w    121.00 169.00   1.00    4.00    --  105.15  61.00  30.00   48
 60  \w     76.00 103.00   1.00    4.00    --  105.15  61.00  30.00   27
 61  \w    140.00 172.00   1.00    4.00    --  105.15  66.00  45.76   32
 62  \w    116.00 143.00   1.00    4.00    --  105.15  61.00 -30.00   27
 63  \w     34.00 132.00   1.00    4.00    --  105.15 -61.00-180.00   98
 64  \w     80.00 174.00   1.00    4.00    --  105.15  61.00   0.00   94
 65  \w     77.00 167.00   1.00    4.00    --  105.15  61.00 120.00   90
 66  \w     76.00 106.00   1.00    4.00    --  105.15  61.00 -30.00   30
 67  \w     76.00 177.00   1.00    4.00    --  105.15  61.00-150.00  101
 68  \w     76.00 175.00   1.00    4.00    --  105.15  61.00  90.00   99
 69  \w    131.00 156.00   1.00    4.00    --  105.15  61.00 -90.00   25
 70  \w     88.00 143.00   1.00    4.00    --  105.15 178.00-120.00   55
;
_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      0.0359821000
_diffrn_orient_matrix_UB_12      0.0010234000
_diffrn_orient_matrix_UB_13      -0.0808853000
_diffrn_orient_matrix_UB_21      0.0411746000
_diffrn_orient_matrix_UB_22      0.1080786000
_diffrn_orient_matrix_UB_23      0.0520634000
_diffrn_orient_matrix_UB_31      0.1068820000
_diffrn_orient_matrix_UB_32      -0.0215877000
_diffrn_orient_matrix_UB_33      0.0635509000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12820
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.719
_diffrn_reflns_theta_min         3.162
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.094
_exptl_absorpt_correction_T_max  0.618
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
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            'clear light blue'
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.107
_refine_diff_density_max         1.643
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         12820
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0529P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12030
_reflns_number_total             12820
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 3.5714\% 
around [-0.15 0.99 -0.04] (reciprocal) or [-0.01 0.97 0.23] (direct)
;
_cod_data_source_file            d1sc03957a2.cif
_cod_data_source_block           mk-207_twin1_hklf5_sq
_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/RSC/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        2819.32(9)
_cod_database_code               1564372
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C72 H162 N4 O24 Si6 U2'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5851(9)
 0.4149(9)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-H1B \\sim N1-H1A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
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 C50 \\sim C51 \\sim C52: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
5.a Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), C2(H2D,H2E,H2F), 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), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C)
;
_shelx_res_checksum              89138
_shelx_hkl_checksum              87089
_shelx_fab_checksum              87464
_platon_squeeze_void_probe_radius 1.20
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.755
_oxdiff_exptl_absorpt_empirical_full_min 0.490
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2