Heterometallic uranium/molybdenum nitride synthesis <i>via</i> partial N-atom transfer.
Barluzzi, Luciano; Jori, Nadir; He, Tianyi; Rajeshkumar, Thayalan; Scopelliti, Rosario; Maron, Laurent; Oyala, Paul; Agapie, Theodor; Mazzanti, Marinella; Chemical communications (Cambridge, England) 58 (2022) 4655–4658; doi:10.1039/d2cc00473a

data_7129807
_publ_section_title
;
 Heterometallic uranium/molybdenum nitride synthesis <i>via</i> partial
 N-atom transfer.
;
_journal_issue                   29
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4655
_journal_page_last               4658
_journal_paper_doi               10.1039/d2cc00473a
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C66 H121 Mo N Na O12 P2 Si3 U, C6 H14'
_chemical_formula_sum            'C72 H135 Mo N Na O12 P2 Si3 U'
_chemical_formula_weight         1709.97
_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             2021-03-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-06 deposited with the CCDC.	2022-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                81.3024(19)
_cell_angle_beta                 79.5672(16)
_cell_angle_gamma                82.5868(18)
_cell_formula_units_Z            2
_cell_length_a                   13.6525(2)
_cell_length_b                   16.4788(4)
_cell_length_c                   19.2469(4)
_cell_measurement_reflns_used    38652
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.9200
_cell_measurement_theta_min      3.8110
_cell_volume                     4186.48(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (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  (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 0.987
_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    -52.00  25.00   1.00    2.00    --  -40.91  89.00 172.00   77
  2  \w     10.00  35.00   1.00    2.00    --   40.91 -89.00  57.00   25
  3  \w     43.00  68.00   1.00    8.00    --  112.00 -89.00  57.00   25
  4  \w    104.00 135.00   1.00    8.00    --  112.00  89.00 172.00   31
  5  \w   -115.00 -31.00   1.00    2.00    --  -40.91 -38.00  90.00   84
  6  \w    -77.00 -27.00   1.00    2.00    --  -40.91 125.00  60.00   50
  7  \w     13.00 113.00   1.00    2.00    --   40.91  57.00 -60.00  100
  8  \w     31.00  97.00   1.00    2.00    --   40.91-125.00   0.00   66
  9  \w     16.00 111.00   1.00    2.00    --   40.91  38.00  60.00   95
 10  \w     55.00 109.00   1.00    8.00    --  112.00-111.00-180.00   54
 11  \w     86.00 172.00   1.00    8.00    --  112.00  45.00-150.00   86
 12  \w     36.00 140.00   1.00    8.00    --  112.00 -30.00  30.00  104
 13  \w     30.00  63.00   1.00    8.00    --  112.00 -94.00   0.00   33
 14  \w     47.00  74.00   1.00    8.00    --  112.00 -77.00 120.00   27
 15  \w     75.00 107.00   1.00    8.00    --  112.00 -94.00   0.00   32
 16  \w    113.00 144.00   1.00    8.00    --  112.00  77.00 -60.00   31
 17  \w     64.00  90.00   1.00    8.00    --  112.00 178.00-150.00   26
 18  \w     89.00 118.00   1.00    8.00    --  112.00 -61.00 -60.00   29
 19  \w     74.00 100.00   1.00    8.00    --  112.00 178.00   0.00   26
 20  \w     88.00 172.00   1.00    8.00    --  112.00  45.00-120.00   84
 21  \w     41.00 101.00   1.00    8.00    --  112.00 -61.00-150.00   60
 22  \w     50.00 109.00   1.00    8.00    --  112.00-111.00 -30.00   59
 23  \w     85.00 117.00   1.00    8.00    --  112.00 -45.00  60.00   32
 24  \w     92.00 119.00   1.00    8.00    --  112.00 -77.00 120.00   27
 25  \w    106.00 158.00   1.00    8.00    --  112.00 111.00 -60.00   52
 26  \w     39.00  97.00   1.00    8.00    --  112.00-111.00 -60.00   58
 27  \w     31.00  63.00   1.00    8.00    --  112.00 -15.00 -30.00   32
 28  \w    140.00 165.00   1.00    8.00    --  112.00 -15.00 -30.00   25
 29  \w     39.00  87.00   1.00    8.00    --  112.00 -45.00   0.00   48
 30  \w     75.00 108.00   1.00    8.00    --  112.00-111.00-150.00   33
 31  \w     68.00 109.00   1.00    8.00    --  112.00-111.00   0.00   41
 32  \w     41.00  67.00   1.00    8.00    --  112.00 -61.00 -60.00   26
 33  \w     55.00 109.00   1.00    8.00    --  112.00-111.00 120.00   54
 34  \w     77.00 109.00   1.00    8.00    --  112.00-111.00 -90.00   32
 35  \w     32.00 102.00   1.00    8.00    --  112.00 -94.00  30.00   70
 36  \w     61.00 115.00   1.00    8.00    --  112.00 178.00  90.00   54
 37  \w     34.00  75.00   1.00    8.00    --  112.00 -94.00-150.00   41
 38  \w     74.00 109.00   1.00    8.00    --  112.00-111.00-120.00   35
 39  \w     42.00  69.00   1.00    8.00    --  112.00-111.00  90.00   27
 40  \w     71.00 108.00   1.00    8.00    --  112.00-111.00  90.00   37
 41  \w     62.00 105.00   1.00    8.00    --  112.00-111.00 150.00   43
 42  \w    106.00 133.00   1.00    8.00    --  112.00 111.00-120.00   27
 43  \w     67.00 138.00   1.00    8.00    --  112.00 -30.00-180.00   71
;
_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      0.0318941000
_diffrn_orient_matrix_UB_12      0.0710943000
_diffrn_orient_matrix_UB_13      0.0315469000
_diffrn_orient_matrix_UB_21      -0.0176515000
_diffrn_orient_matrix_UB_22      0.0593396000
_diffrn_orient_matrix_UB_23      -0.0675625000
_diffrn_orient_matrix_UB_31      -0.1094596000
_diffrn_orient_matrix_UB_32      0.0216254000
_diffrn_orient_matrix_UB_33      0.0343496000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49516
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.009
_diffrn_reflns_theta_min         3.310
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.873
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.194
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
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            'translucent dark black'
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1774
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.188
_refine_diff_density_max         1.724
_refine_diff_density_min         -2.013
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.000193(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         17241
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0433P)^2^+3.4796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17102
_reflns_number_total             17241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00473a2.cif
_cod_data_source_block           lb1231
_cod_depositor_comments          'Adding full bibliography for 7129807.cif.'
_cod_original_cell_volume        4186.49(16)
_cod_database_code               7129807
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C72 H135 N1 O12 Na1 Si3 P2 Mo1 U1'
_shelx_estimated_absorpt_t_max   0.319
_shelx_estimated_absorpt_t_min   0.147
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C92-C91 \\sim C93-C92 \\sim C94-C93 \\sim C95-C94 \\sim C96-C95
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4.a Ternary CH refined with riding coordinates:
 C73(H73), C76(H76), C85(H85), C88(H88)
4.b Secondary CH2 refined with riding coordinates:
 C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B)
4.c Aromatic/amide H refined with riding coordinates:
 C62(H62), C63(H63), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70),
 C71(H71), C80(H80), C81(H81), C82(H82), C83(H83)
4.d 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), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C78(H78A,
 H78B,H78C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C),
 C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C96(H96A,H96B,H96C)
;
_shelx_res_checksum              42601
_olex2_date_sample_data_collection 2021-03-01
_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 2.288
_oxdiff_exptl_absorpt_empirical_full_min 0.629