Iron promoted end-on dinitrogen-bridging in heterobimetallic complexes of uranium and lanthanides.
Jori, Nadir; Moreno, Juan J.; Shivaraam, R. A. Keerthi; Rajeshkumar, Thayalan; Scopelliti, Rosario; Maron, Laurent; Campos, Jesús; Mazzanti, Marinella; Chemical science 15 (2024) 6842–6852; doi:10.1039/d4sc01050g

data_1571323
_publ_section_title
;
 Iron promoted end-on dinitrogen-bridging in heterobimetallic complexes of
 uranium and lanthanides.
;
_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              6842
_journal_page_last               6852
_journal_paper_doi               10.1039/d4sc01050g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C38 H102 Fe N5 P4 Si6 Sm'
_chemical_formula_sum            'C38 H102 Fe N5 P4 Si6 Sm'
_chemical_formula_weight         1127.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-01 deposited with the CCDC.	2024-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.235(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8173(5)
_cell_length_b                   18.0593(7)
_cell_length_c                   27.8343(12)
_cell_measurement_reflns_used    34744
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      74.1840
_cell_measurement_theta_min      2.4880
_cell_volume                     5930.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_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     28.00  54.00   0.50    1.50    --   66.21 -95.00-150.00   52
  2  \w     29.00  75.00   0.50    1.50    --   66.21 -95.00-120.00   92
  3  \w     28.00  72.00   0.50    1.50    --   66.21 -95.00-180.00   88
  4  \w     28.00  73.00   0.50    1.50    --   66.21 -95.00  60.00   90
  5  \w   -110.00 -84.00   0.50    1.50    --  -66.84 -15.00-180.00   52
  6  \w    -64.00 -29.00   0.50    1.50    --  -66.84 125.00 -30.00   70
  7  \w   -112.00 -41.00   0.50    1.50    --  -66.84 -15.00  60.00  142
  8  \w   -104.00 -72.00   0.50    1.50    --  -66.84   0.00 -90.00   64
  9  \w    -99.00 -73.00   0.50    1.50    --  -66.84   0.00-180.00   52
 10  \w    -71.00 -37.00   0.50    1.50    --  -66.84 -15.00-180.00   68
 11  \w   -104.00 -73.00   0.50    1.50    --  -66.84   0.00 -60.00   62
 12  \w    -62.00 -36.00   0.50    1.50    --  -66.84 125.00 -90.00   52
 13  \w    -97.00 -48.00   0.50    1.50    --  -69.31 -15.00 120.00   98
 14  \w    -97.00 -33.00   0.50    1.50    --  -69.31   0.00 150.00  128
 15  \w   -106.00 -72.00   0.50    1.50    --  -69.31   0.00  60.00   68
 16  \w     33.00  73.00   0.50    1.50    --   69.48 -95.00 -30.00   80
 17  \w     36.00  96.00   0.50    1.50    --   69.48-125.00 120.00  120
 18  \w     33.00  70.00   0.50    1.50    --   69.48 -95.00 120.00   74
 19  \w   -104.00 -46.00   0.50    1.50    --  -74.00 130.00-168.28  116
 20  \w   -101.00 -44.00   0.50    1.50    --  -74.78 128.00  93.77  114
 21  \w   -109.00 -81.00   0.50    1.50    --  -74.78 135.00 -79.83   56
 22  \w    -68.00 -37.00   0.50    1.50    --  -74.78 143.00 164.37   62
 23  \w   -112.00 -86.00   0.50    1.50    --  -74.78 143.00 164.37   52
 24  \w   -106.00 -33.00   0.50    1.50    --  -74.78 133.00-130.86  146
 25  \w    -81.00 -55.00   0.50    1.50    --  -74.78 149.00  21.75   52
 26  \w   -118.00 -92.00   0.50    1.50    --  -74.78 149.00  21.75   52
 27  \w    -67.00 -32.00   0.50    1.50    --  -74.78 135.00 -79.83   70
 28  \w   -122.00 -49.00   0.50    1.50    --  -74.78 158.00 -69.47  146
 29  \w     80.00 105.00   0.50    1.50    --   78.10-125.00-180.00   50
 30  \w     80.00 105.00   0.50    1.50    --   78.10-125.00 -30.00   50
 31  \w     51.00  76.00   0.50    1.50    --   78.10-125.00 -30.00   50
 32  \w     49.00 105.00   0.50    1.50    --   78.10-125.00  90.00  112
 33  \w     53.00  91.00   0.50    1.50    --   78.10  15.00  90.00   76
 34  \w     48.00 120.00   0.50    1.50    --   78.10  15.00-150.00  144
 35  \w     80.00 115.00   0.50    1.50    --   78.10  15.00 -30.00   70
 36  \w     42.00 105.00   0.50    1.50    --   78.10-125.00-120.00  126
 37  \w     59.00 122.00   0.50    1.50    --   78.10  15.00 120.00  126
 38  \w     79.00 104.00   0.50    1.50    --   78.10-125.00 150.00   50
 39  \w     45.00  71.00   0.50    1.50    --   78.10-125.00 150.00   52
 40  \w     80.00 105.00   0.50    1.50    --   78.10-125.00  60.00   50
 41  \w     79.00 104.00   0.50    1.50    --   78.10-125.00 -90.00   50
 42  \w     80.00 105.00   0.50    1.50    --   78.10-125.00   0.00   50
 43  \w     80.00 105.00   0.50    1.50    --   78.10-125.00 120.00   50
 44  \w     80.00 105.00   0.50    1.50    --   78.10-125.00-150.00   50
 45  \w     80.00 105.00   0.50    1.50    --   78.10-125.00 -60.00   50
 46  \w     39.00 105.00   0.50    1.50    --   78.10-125.00  30.00  132
 47  \w     46.00  71.00   0.50    1.50    --   78.10-125.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0100118000
_diffrn_orient_matrix_UB_12      -0.0542392000
_diffrn_orient_matrix_UB_13      -0.0422154000
_diffrn_orient_matrix_UB_21      -0.1202905000
_diffrn_orient_matrix_UB_22      0.0214092000
_diffrn_orient_matrix_UB_23      -0.0195443000
_diffrn_orient_matrix_UB_31      0.0501526000
_diffrn_orient_matrix_UB_32      0.0621903000
_diffrn_orient_matrix_UB_33      -0.0301135000
_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  0.0752
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            94924
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.015
_diffrn_reflns_theta_min         2.918
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.715
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.116
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
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            'clear dark orange'
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.028
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         11946
_refine_ls_number_restraints     569
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0659
_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^)+(0.1280P)^2^+7.7564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.2040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9259
_reflns_number_total             11946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01050g2.cif
_cod_data_source_block           nj1141
_cod_depositor_comments
'Adding full bibliography for 1571317--1571325.cif.'
_cod_database_code               1571323
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C38 H102 N5 P4 Si6 Sm1 Fe1'
_shelx_estimated_absorpt_t_max   0.311
_shelx_estimated_absorpt_t_min   0.122
_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
 C35-C36 = C33-C34 = C30-C29 = C32-C31
 1.54 with sigma of 0.02
 P3-C36
 2.9 with sigma of 0.02
 P3-C32
 2.9 with sigma of 0.02
 P3-C31 \\sim P3-C29 \\sim P3-C35 \\sim P3-C33
 with sigma of 0.02
 C33-C29 \\sim C35-C31
 with sigma of 0.02
 P2-C24 \\sim P1-C23 \\sim P3-C37 \\sim P4-C38
 with sigma of 0.02
3. Rigid bond restraints
 P3, C37
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C39) \\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(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C35)=
 Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=1-FVAR(1)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C33)=
 Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B),
 C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C41(H41A,H41B)
7.b Me refined with riding coordinates:
 C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C)
7.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), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C),
 C28(H28A,H28B,H28C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              3783
_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 3.740
_oxdiff_exptl_absorpt_empirical_full_min 0.380