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_1571325
_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 U'
_chemical_formula_sum            'C38 H102 Fe N5 P4 Si6 U'
_chemical_formula_weight         1215.54
_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             2022-09-26
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-02-01 deposited with the CCDC.	2024-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                78.7323(15)
_cell_angle_beta                 89.4820(13)
_cell_angle_gamma                89.0470(12)
_cell_formula_units_Z            4
_cell_length_a                   11.55749(16)
_cell_length_b                   19.2532(3)
_cell_length_c                   27.3197(5)
_cell_measurement_reflns_used    24066
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5250
_cell_measurement_theta_min      3.6290
_cell_volume                     5961.04(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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 0.973
_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    -69.00  30.00   1.00    2.00    --  -40.91  57.00   0.00   99
  2  \w    -71.00  29.00   1.00    2.00    --  -40.91  19.00 -60.00  100
  3  \w    -60.00 -16.00   1.00    2.00    --  -40.91  77.00-150.00   44
  4  \w     14.00  83.00   1.00    2.00    --   40.91  57.00 150.00   69
  5  \w     34.00  81.00   1.00    2.00    --   40.91 -99.00  30.00   47
  6  \w     32.00 109.00   1.00    8.00    --  105.15-111.00 150.00   77
  7  \w     29.00 130.00   1.00    8.00    --  105.15 -30.00 150.00  101
  8  \w     43.00  72.00   1.00    8.00    --  105.15 -94.00 -90.00   29
  9  \w    104.00 130.00   1.00    8.00    --  105.15 111.00-150.00   26
 10  \w     27.00  71.00   1.00    8.00    --  105.15 -94.00-180.00   44
 11  \w    144.00 172.00   1.00    8.00    --  105.15 111.00-150.00   28
 12  \w     59.00 120.00   1.00    8.00    --  105.15  15.00-150.00   61
 13  \w    132.00 178.00   1.00    8.00    --  105.15  15.00-150.00   46
 14  \w     34.00 109.00   1.00    8.00    --  105.15-111.00  60.00   75
 15  \w     23.00  75.00   1.00    8.00    --  105.15 -94.00   0.00   52
 16  \w     32.00 106.00   1.00    8.00    --  105.15-111.00 -30.00   74
 17  \w    101.00 133.00   1.00    8.00    --  105.15 -30.00-120.00   32
 18  \w     67.00  93.00   1.00    8.00    --  105.15 -30.00-120.00   26
 19  \w     54.00 109.00   1.00    8.00    --  105.15-111.00-120.00   55
 20  \w    153.00 178.00   1.00    8.00    --  105.15  77.00-180.00   25
 21  \w     78.00 166.00   1.00    8.00    --  105.15  30.00 120.00   88
;
_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      -0.0402608000
_diffrn_orient_matrix_UB_12      -0.0206505000
_diffrn_orient_matrix_UB_13      -0.0487586000
_diffrn_orient_matrix_UB_21      0.0405637000
_diffrn_orient_matrix_UB_22      0.0719407000
_diffrn_orient_matrix_UB_23      -0.0297399000
_diffrn_orient_matrix_UB_31      0.1204445000
_diffrn_orient_matrix_UB_32      -0.0325003000
_diffrn_orient_matrix_UB_33      -0.0066585000
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43530
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.625
_diffrn_reflns_theta_min         3.116
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.923
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.232
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
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    1.354
_exptl_crystal_description       needle
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.116
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1057
_refine_ls_number_reflns         23035
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0315P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20351
_reflns_number_total             23035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01050g2.cif
_cod_data_source_block           jj-007
_cod_depositor_comments
'Adding full bibliography for 1571317--1571325.cif.'
_cod_original_cell_volume        5961.05(17)
_cod_database_code               1571325
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H102 N5 P4 Si6 Fe1 U1'
_shelx_estimated_absorpt_t_max   0.485
_shelx_estimated_absorpt_t_min   0.102
_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
 P8-C77 \\sim P8-C75
 with sigma of 0.02
 C77-C78 \\sim C76-C75
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P8 \\sim C75 \\sim C76 \\sim C77 \\sim C78: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
4. Others
 Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=1-FVAR(1)
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=FVAR(1)
 Fixed X: U1(0.71282) U2(0.30764)
 Fixed Y: U1(0.760241) U2(0.75728)
 Fixed Z: U1(0.088261) U2(0.588409)
5.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,
 H26B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C57(H57A,H57B), C59(H59A,H59B),
  C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C65(H65A,H65B), C67(H67A,
 H67B), C69(H69A,H69B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B),
 C75(H75A,H75B), C77(H77A,H77B)
5.b 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), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C),
 C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C60(H60A,H60B,
 H60C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C70(H70A,
 H70B,H70C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C78(H78A,H78B,H78C)
;
_shelx_res_checksum              45712
_olex2_date_sample_data_collection 2022-09-22
_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 2.874
_oxdiff_exptl_absorpt_empirical_full_min 0.496