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_1571319
_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         'C36 H93.2 Fe N4 O P4 Si4 Yb'
_chemical_formula_sum            'C36 H93.2 Fe N4 O P4 Si4 Yb'
_chemical_formula_weight         1063.47
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-07-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-02-07 deposited with the CCDC.	2024-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.5143(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.35562(15)
_cell_length_b                   36.8715(3)
_cell_length_c                   14.64313(18)
_cell_measurement_reflns_used    36339
_cell_measurement_temperature    200.07(16)
_cell_measurement_theta_max      76.5290
_cell_measurement_theta_min      3.2250
_cell_volume                     5514.24(12)
_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      200.07(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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    -89.00  36.00   1.00    1.00    --  -43.01  17.00  -9.00  125
  2  \w   -123.00 -75.00   1.00    1.00    --  -43.01 -17.00-178.00   48
  3  \w     67.00 124.00   1.00    1.00    --   43.01  17.00  -9.00   57
  4  \w      2.00  27.00   1.00    1.00    --   43.01 -17.00-178.00   25
  5  \w    134.00 160.00   1.00    4.00    --  112.00  17.00  -9.00   26
  6  \w     71.00  96.00   1.00    4.00    --  112.00 -17.00-178.00   25
  7  \w    -45.00 -18.00   1.00    1.00    --  -43.01 125.00   0.00   27
  8  \w     28.00  89.00   1.00    1.00    --   43.01-125.00  30.00   61
  9  \w     28.00  92.00   1.00    1.00    --   43.01-125.00-150.00   64
 10  \w     -4.00  60.00   1.00    1.00    --   43.01 -77.00  90.00   64
 11  \w     39.00  66.00   1.00    4.00    --  112.00 -30.00  90.00   27
 12  \w     71.00 130.00   1.00    4.00    --  112.00 -30.00  90.00   59
 13  \w     46.00  73.00   1.00    4.00    --  112.00 -61.00 -90.00   27
 14  \w     53.00 109.00   1.00    4.00    --  112.00-111.00-180.00   56
 15  \w    123.00 176.00   1.00    4.00    --  112.00 111.00-120.00   53
 16  \w     53.00 109.00   1.00    4.00    --  112.00-111.00-150.00   56
 17  \w     62.00 128.00   1.00    4.00    --  112.00 178.00 120.00   66
 18  \w     84.00 176.00   1.00    4.00    --  112.00  61.00 -60.00   92
 19  \w     68.00 109.00   1.00    4.00    --  112.00-111.00 120.00   41
 20  \w    104.00 171.00   1.00    4.00    --  112.00  77.00 -90.00   67
 21  \w     40.00 109.00   1.00    4.00    --  112.00-111.00 -90.00   69
 22  \w    103.00 175.00   1.00    4.00    --  112.00  77.00-150.00   72
 23  \w     81.00 109.00   1.00    4.00    --  112.00-111.00   0.00   28
 24  \w     40.00  65.00   1.00    4.00    --  112.00-111.00   0.00   25
 25  \w    105.00 170.00   1.00    4.00    --  112.00 111.00 -30.00   65
 26  \w     62.00 102.00   1.00    4.00    --  112.00 178.00   0.00   40
 27  \w     59.00  86.00   1.00    4.00    --  112.00 -94.00 -90.00   27
 28  \w     55.00 104.00   1.00    4.00    --  112.00 -30.00 -90.00   49
 29  \w     61.00  88.00   1.00    4.00    --  112.00-111.00  60.00   27
 30  \w     84.00 177.00   1.00    4.00    --  112.00  61.00-120.00   93
 31  \w     80.00 106.00   1.00    4.00    --  112.00 -61.00 -90.00   26
 32  \w     63.00  88.00   1.00    4.00    --  112.00 -94.00-150.00   25
 33  \w     43.00  80.00   1.00    4.00    --  112.00 -61.00-120.00   37
 34  \w     86.00 140.00   1.00    4.00    --  112.00 -61.00-120.00   54
 35  \w     70.00  97.00   1.00    4.00    --  112.00-111.00 150.00   27
 36  \w    124.00 164.00   1.00    4.00    --  112.00 111.00-150.00   40
 37  \w     74.00 109.00   1.00    4.00    --  112.00-111.00 -30.00   35
 38  \w    122.00 148.00   1.00    4.00    --  112.00 111.00-180.00   26
 39  \w     70.00 108.00   1.00    4.00    --  112.00-105.00  29.51   38
 40  \w     52.00  97.00   1.00    4.00    --  112.00-111.00  90.00   45
;
_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      -0.1370282000
_diffrn_orient_matrix_UB_12      0.0007583000
_diffrn_orient_matrix_UB_13      -0.0599956000
_diffrn_orient_matrix_UB_21      -0.0608732000
_diffrn_orient_matrix_UB_22      0.0093250000
_diffrn_orient_matrix_UB_23      0.0862416000
_diffrn_orient_matrix_UB_31      0.0163803000
_diffrn_orient_matrix_UB_32      0.0407145000
_diffrn_orient_matrix_UB_33      -0.0186584000
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            65865
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.775
_diffrn_reflns_theta_min         3.287
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.304
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.062
_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    1.281
_exptl_crystal_description       prism
_exptl_crystal_F_000             2229
_exptl_crystal_size_max          0.522
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.229
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         11541
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0452P)^2^+1.8910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10704
_reflns_number_total             11541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01050g2.cif
_cod_data_source_block           nj1161
_cod_depositor_comments
'Adding full bibliography for 1571317--1571325.cif.'
_cod_original_cell_volume        5514.23(12)
_cod_database_code               1571319
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C36 H93.2 N4 O1 P4 Si4 Fe1 Yb1'
_shelx_estimated_absorpt_t_max   0.286
_shelx_estimated_absorpt_t_min   0.115
_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-C13 \\sim Si4-C16 \\sim Si4-C15 \\sim Si4-C18 \\sim Si4-C14 \\sim Si4-C17
 with sigma of 0.02
 C13-C15 \\sim C15-C14 \\sim C13-C14 \\sim C16-C18 \\sim C18-C17 \\sim C16-C17
 with sigma of 0.02
 Si1-C6 \\sim Si1-C3 \\sim Si1-C5 \\sim Si1-C2 \\sim Si1-C1 \\sim Si1-C4
 with sigma of 0.02
 C1-C3 \\sim C3-C2 \\sim C2-C1 \\sim C4-C6 \\sim C6-C5 \\sim C4-C5
 with sigma of 0.02
 O1-C39 \\sim O1-C46 \\sim O1-C43 \\sim O1-C41
 with sigma of 0.02
 C40-C39 \\sim C44-C43 \\sim C45-C44 \\sim C46-C45 \\sim C42-C41
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si1 \\sim Si4 \\sim O1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6
\\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C39 \\sim C40
\\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=
 Sof(H6A)=Sof(H6B)=Sof(H6C)=1-FVAR(2)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(2)
 Fixed Sof: C39(0.6) H39A(0.6) H39B(0.6) C40(0.6) H40A(0.6) H40B(0.6)
 H40C(0.6) C41(0.6) H41A(0.6) H41B(0.6) C42(0.6) H42A(0.6) H42B(0.6) H42C(0.6)
 C43(0.4) H43A(0.4) H43B(0.4) C44(0.4) H44A(0.4) H44B(0.4) C45(0.4) H45A(0.4)
 H45B(0.4) C46(0.4) H46A(0.4) H46B(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C25(H25A,
 H25B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B),
  C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B)
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), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,
 H42B,H42C)
;
_shelx_res_checksum              59006
_olex2_date_sample_data_collection 2023-05-12
_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 1.706
_oxdiff_exptl_absorpt_empirical_full_min 0.705