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_1571317
_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         'C52 H132 Fe2 N6 P8 Si4 Sm, 0.5(C6 H14)'
_chemical_formula_sum            'C55 H139 Fe2 N6 P8 Si4 Sm'
_chemical_formula_weight         1506.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-11-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 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                 97.369(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4532(5)
_cell_length_b                   29.5233(9)
_cell_length_c                   23.5755(8)
_cell_measurement_reflns_used    3549
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.4330
_cell_measurement_theta_min      3.5030
_cell_volume                     7905.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.94a 64-bit (release 20-10-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.94a (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    'olex2.solve 1.5 (Bourhis et al., 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 0.999
_diffrn_measured_fraction_theta_max 0.972
_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    -71.00  -4.00   1.00   10.00    --  -41.04 100.00-151.00   67
  2  \w     38.00  81.00   1.00   10.00    --   41.04-100.00 103.00   43
  3  \w    105.00 148.00   1.00   40.00    --  105.15 100.00-151.00   43
  4  \w     41.00  67.00   1.00   40.00    --  105.15-100.00 103.00   26
  5  \w   -113.00 -17.00   1.00   10.00    --  -41.04 -38.00 -90.00   96
  6  \w    -66.00  33.00   1.00   10.00    --  -41.04  38.00  90.00   99
  7  \w      9.00  35.00   1.00   10.00    --   41.04 -99.00-120.00   26
  8  \w     34.00 123.00   1.00   40.00    --  105.15 -61.00 120.00   89
  9  \w     33.00  88.00   1.00   40.00    --  105.15-111.00 150.00   55
 10  \w     91.00 163.00   1.00   40.00    --  105.15  45.00   0.00   72
 11  \w     78.00 103.00   1.00   40.00    --  105.15-111.00-180.00   25
 12  \w     79.00 172.00   1.00   40.00    --  105.15  45.00 -90.00   93
 13  \w     49.00 128.00   1.00   40.00    --  105.15 -61.00-120.00   79
;
_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      0.0079433000
_diffrn_orient_matrix_UB_12      -0.0453103000
_diffrn_orient_matrix_UB_13      0.0326885000
_diffrn_orient_matrix_UB_21      -0.0742114000
_diffrn_orient_matrix_UB_22      0.0200802000
_diffrn_orient_matrix_UB_23      0.0439671000
_diffrn_orient_matrix_UB_31      -0.1132724000
_diffrn_orient_matrix_UB_32      -0.0163485000
_diffrn_orient_matrix_UB_33      -0.0365576000
_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  0.1009
_diffrn_reflns_av_unetI/netI     0.1287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37561
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.923
_diffrn_reflns_theta_min         2.994
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.776
_exptl_absorpt_correction_T_max  0.638
_exptl_absorpt_correction_T_min  0.295
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.94a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3204
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         15331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0252P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9347
_reflns_number_total             15331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01050g2.cif
_cod_data_source_block           nj1144
_cod_depositor_comments
'Adding full bibliography for 1571317--1571325.cif.'
_cod_database_code               1571317
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C55 H139 N6 P8 Si4 Fe2 Sm1'
_shelx_estimated_absorpt_t_max   0.589
_shelx_estimated_absorpt_t_min   0.205
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B),
 C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
  C19(H19A,H19B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,
 H38B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B),
 C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C51(H51A,H51B), C54(H54A,H54B),
  C55(H55A,H55B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C39(H39A,
 H39B,H39C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C),
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              39945
_olex2_date_sample_data_collection 2023-10-31
_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 1.920
_oxdiff_exptl_absorpt_empirical_full_min 0.549