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_1571321
_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 Tm'
_chemical_formula_sum            'C38 H102 Fe N5 P4 Si6 Tm'
_chemical_formula_weight         1146.44
_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             2023-12-21
_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                 94.1162(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.60150(16)
_cell_length_b                   18.3958(2)
_cell_length_c                   27.5562(4)
_cell_measurement_reflns_used    27606
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      75.2220
_cell_measurement_theta_min      3.2130
_cell_volume                     5865.84(13)
_computing_cell_refinement       'CrysAlisPro 1.171.43.103a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.103a 64-bit (release 20-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.103a (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      139.99(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 0.999
_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     41.00  91.00   0.50    0.20    --   79.75-128.00 -88.63  100
  2  \w     60.00 106.00   0.50    0.20    --   79.75-125.00 -67.43   92
  3  \w     53.00 104.00   0.50    0.20    --   79.75-123.00  11.39  102
  4  \w     38.00 105.00   0.50    0.20    --   79.75-125.00  35.74  134
  5  \w     66.00  92.00   0.50    0.20    --   76.50-125.00   0.00   52
  6  \w   -101.00 -75.00   0.50    0.20    --  -72.00 -77.00 -67.86   52
  7  \w   -112.00 -85.00   0.50    0.20    --  -76.25 -75.00 -71.50   54
  8  \w    -76.00 -44.00   0.50    0.20    --  -40.00 -75.00 -68.43   64
  9  \w   -115.00 -82.00   0.50    0.20    --  -72.00 -55.00 -53.60   66
 10  \w   -118.00 -93.00   0.50    0.20    --  -76.25 -51.00  78.22   50
 11  \w   -114.00 -88.00   0.50    0.20    --  -76.25 -67.00 114.57   52
 12  \w   -118.00 -85.00   0.50    0.20    --  -72.00 -41.00 134.66   66
 13  \w   -120.00 -90.00   0.50    0.20    --  -76.00 -44.00 117.98   60
 14  \w   -121.00 -90.00   0.50    0.20    --  -76.00 -41.00  10.79   62
 15  \w     52.00 113.00   0.50    0.20    --   79.75   4.00 -23.66  122
 16  \w     72.00 104.00   0.50    0.20    --   68.00  76.00-175.33   64
 17  \w     63.00  94.00   0.50    0.20    --   56.00  71.00 -21.25   62
 18  \w     56.00  87.00   0.50    0.20    --   48.00  67.00-108.73   62
 19  \w     72.00 104.00   0.50    0.20    --   68.00  76.00  56.27   64
 20  \w     66.00  97.00   0.50    0.20    --   60.00  73.00 109.58   62
 21  \w     47.00  78.00   0.50    0.20    --   40.00  70.00 178.89   62
 22  \w     95.00 121.00   0.50    0.20    --   79.75  36.00 171.60   52
 23  \w     91.00 116.00   0.50    0.20    --   79.75  44.00 138.75   50
 24  \w     94.00 125.00   0.50    0.20    --   79.75  37.00 104.31   62
 25  \w     61.00  93.00   0.50    0.20    --   52.00  64.00  41.17   64
 26  \w     90.00 115.00   0.50    0.20    --   79.75  36.00 139.27   50
 27  \w     95.00 121.00   0.50    0.20    --   79.75  44.00 -44.05   52
 28  \w    101.00 126.00   0.50    0.20    --   79.75  24.00-133.35   50
 29  \w     93.00 118.00   0.50    0.20    --   79.75  36.00-148.76   50
 30  \w     94.00 120.00   0.50    0.20    --   79.75  36.00 -92.94   52
 31  \w     79.00 126.00   0.50    0.20    --   79.75  26.00 -40.03   94
 32  \w     99.00 125.00   0.50    0.20    --   79.75  16.00  46.39   52
 33  \w     51.00  81.00   0.50    0.20    --   79.75  16.00  46.39   60
 34  \w     63.00 106.00   0.50    0.20    --   79.75  13.00 106.96   86
 35  \w     91.00 124.00   0.50    0.20    --   79.75  14.00 157.21   66
 36  \w     52.00  78.00   0.50    0.20    --   79.75  14.00 157.21   52
 37  \w     45.00  99.00   0.50    0.20    --   79.75   4.00-122.74  108
;
_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      0.0025124000
_diffrn_orient_matrix_UB_12      -0.0177046000
_diffrn_orient_matrix_UB_13      -0.0545363000
_diffrn_orient_matrix_UB_21      0.1129384000
_diffrn_orient_matrix_UB_22      0.0436043000
_diffrn_orient_matrix_UB_23      -0.0019891000
_diffrn_orient_matrix_UB_31      0.0705731000
_diffrn_orient_matrix_UB_32      -0.0692355000
_diffrn_orient_matrix_UB_33      0.0127605000
_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  0.0452
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            62660
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.563
_diffrn_reflns_theta_min         3.216
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.159
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.188
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.103a (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 intense red'
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.192
_refine_diff_density_max         1.581
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         12041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+6.0585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10262
_reflns_number_total             12041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01050g2.cif
_cod_data_source_block           ks803
_cod_depositor_comments
'Adding full bibliography for 1571317--1571325.cif.'
_cod_original_cell_volume        5865.83(14)
_cod_database_code               1571321
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C38 H102 N5 P4 Si6 Fe1 Tm1'
_shelx_estimated_absorpt_t_max   0.340
_shelx_estimated_absorpt_t_min   0.237
_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:
 C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C27(H27A,H27B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B)
2.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), C21(H21A,H21B,H21C),
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C32(H32A,H32B,
 H32C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              1568
_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 2.119
_oxdiff_exptl_absorpt_empirical_full_min 0.387