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_1571324
_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 Dy Fe N5 P4 Si6'
_chemical_formula_sum            'C38 H102 Dy Fe N5 P4 Si6'
_chemical_formula_weight         1140.01
_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             2023-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-02-01 deposited with the CCDC.	2024-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.323(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6319(5)
_cell_length_b                   18.3899(9)
_cell_length_c                   27.7329(15)
_cell_measurement_reflns_used    6482
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      71.6660
_cell_measurement_theta_min      3.9590
_cell_volume                     5915.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.99(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 0.981
_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   -111.00 -80.00   1.00    7.50    --  -40.85-151.00  72.00   31
  2  \w    -85.00  -3.00   1.00    7.50    --  -40.85 122.00 -44.00   82
  3  \w    -86.00 -61.00   1.00    7.50    --  -40.85 151.00 116.00   25
  4  \w     58.00  83.00   1.00    7.50    --   40.85-122.00-125.00   25
  5  \w     53.00  78.00   1.00    7.50    --   40.85-151.00  72.00   25
  6  \w     61.00  86.00   1.00   30.00    --  105.46-151.00  72.00   25
  7  \w     84.00 111.00   1.00   30.00    --  105.46-122.00-125.00   27
  8  \w    122.00 170.00   1.00   30.00    --  105.46 122.00 -44.00   48
  9  \w     97.00 123.00   1.00   30.00    --  105.46 151.00 116.00   26
 10  \w    -65.00  31.00   1.00    7.50    --  -40.85  38.00-120.00   96
 11  \w   -110.00 -16.00   1.00    7.50    --  -40.85 -38.00  60.00   94
 12  \w    -32.00  52.00   1.00    7.50    --   40.85 -38.00 -90.00   84
 13  \w     84.00 177.00   1.00   30.00    --  105.46  30.00-180.00   93
 14  \w    152.00 177.00   1.00   30.00    --  105.46  77.00 -60.00   25
 15  \w    104.00 172.00   1.00   30.00    --  105.46 111.00   0.00   68
 16  \w     31.00 134.00   1.00   30.00    --  105.46 -77.00  30.00  103
 17  \w     71.00 130.00   1.00   30.00    --  105.46 -45.00-180.00   59
 18  \w     31.00 126.00   1.00   30.00    --  105.46 -30.00   0.00   95
 19  \w    104.00 132.00   1.00   30.00    --  105.46  77.00 -60.00   28
 20  \w     33.00  58.00   1.00   30.00    --  105.46 -45.00-180.00   25
 21  \w     84.00 109.00   1.00   30.00    --  105.46-111.00 120.00   25
 22  \w     81.00 128.00   1.00   30.00    --  105.46 178.00  60.00   47
 23  \w     33.00 109.00   1.00   30.00    --  105.46-111.00  30.00   76
 24  \w     84.00 109.00   1.00   30.00    --  105.46-111.00  60.00   25
 25  \w     63.00 109.00   1.00   30.00    --  105.46-111.00 -60.00   46
 26  \w    101.00 131.00   1.00   30.00    --  105.46 -45.00-150.00   30
 27  \w     94.00 173.00   1.00   30.00    --  105.46  30.00 -90.00   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      0.0954132000
_diffrn_orient_matrix_UB_12      -0.0574265000
_diffrn_orient_matrix_UB_13      -0.0035054000
_diffrn_orient_matrix_UB_21      0.0335525000
_diffrn_orient_matrix_UB_22      0.0081049000
_diffrn_orient_matrix_UB_23      0.0545673000
_diffrn_orient_matrix_UB_31      -0.0861240000
_diffrn_orient_matrix_UB_32      -0.0603930000
_diffrn_orient_matrix_UB_33      0.0107929000
_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  0.1327
_diffrn_reflns_av_unetI/netI     0.1235
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            47358
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.254
_diffrn_reflns_theta_min         4.000
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.048
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_correction_T_min  0.123
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (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 orange'
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.123
_refine_diff_density_max         1.734
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         11642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.867
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0594P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6285
_reflns_number_total             11642
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -177.1416\% 
around [-0.01 1.00 -0.06] (reciprocal) or [-0.02 1.00 -0.03] (direct)
;
_cod_data_source_file            d4sc01050g2.cif
_cod_data_source_block           nj1187
_cod_depositor_comments
'Adding full bibliography for 1571317--1571325.cif.'
_cod_database_code               1571324
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C38 H102 N5 P4 Si6 Fe1 Dy1'
_shelx_estimated_absorpt_t_max   0.344
_shelx_estimated_absorpt_t_min   0.164
_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), C32(H32A,H32B), 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), C31(H31A,H31B,
 H31C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              28948
_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 6.527
_oxdiff_exptl_absorpt_empirical_full_min 0.197
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2