Alkylamido lutetium complexes as prospective lutetium imido precursors: synthesis, characterization and ligand design.
Knott, Jackson P.; Hsiang, Shou-Jen; Hayes, Paul G.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6261–6273; doi:10.1039/d5dt00338e

data_7718395
_publ_section_title
;
 Alkylamido lutetium complexes as prospective lutetium imido precursors:
 synthesis, characterization and ligand design.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6261
_journal_page_last               6273
_journal_paper_doi               10.1039/d5dt00338e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C57 H78 Lu N4 P2 Si, C57 H77 Lu N4 P2 Si, 1[C7H16]'
_chemical_formula_sum            'C121 H171 Lu2 N8 P4 Si2'
_chemical_formula_weight         2267.65
_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   mixed
_audit_creation_date             2025-01-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-16 deposited with the CCDC.	2025-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                110.2276(10)
_cell_angle_beta                 104.4073(10)
_cell_angle_gamma                92.0411(9)
_cell_formula_units_Z            2
_cell_length_a                   12.31417(13)
_cell_length_b                   21.4332(2)
_cell_length_c                   24.4686(2)
_cell_measurement_reflns_used    64606
_cell_measurement_temperature    107.3(3)
_cell_measurement_theta_max      79.8580
_cell_measurement_theta_min      3.5140
_cell_volume                     5816.38(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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_temperature      107.3
_diffrn_detector_type            'Pilatus 200/300K'
_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   -107.00 -36.00   0.50    0.72    --  -38.50 -19.00 -30.00  142
  2  \w    -53.00  18.00   0.50    0.72    --  -38.50  77.00 -60.00  142
  3  \w    -39.00  30.00   0.50    0.72    --  -38.50  19.00  90.00  138
  4  \w    -40.00  19.00   0.50    0.72    --  -38.50  37.00-150.00  118
  5  \w    -54.00  25.00   0.50    0.72    --  -38.50  77.00  90.00  158
  6  \w      3.00  28.00   0.50    0.72    --  -38.50  37.00 -60.00   50
  7  \w     33.00  59.00   0.50    0.72    --   47.56-125.00 -30.00   52
  8  \w     74.00  99.00   0.50    0.72    --   47.56-125.00 -30.00   50
  9  \w     23.00  98.00   0.50    0.72    --   47.56-125.00-150.00  150
 10  \w    -22.00  43.00   0.50    0.72    --   47.56 -19.00-120.00  130
 11  \w      8.00  59.00   0.50    0.72    --   47.56 -57.00-150.00  102
 12  \w     73.00  99.00   0.50    2.87    --  111.00 -12.00-180.00   52
 13  \w     53.00  86.00   0.50    2.87    --  111.00 -63.00-120.00   66
 14  \w     91.00 117.00   0.50    2.87    --  111.00 -63.00-120.00   52
 15  \w    113.00 140.00   0.50    2.87    --  111.00  37.00 150.00   54
 16  \w     90.00 116.00   0.50    2.87    --  111.00-111.00  30.00   52
 17  \w     80.00 107.00   0.50    2.87    --  111.00 -77.00  60.00   54
 18  \w     58.00 114.00   0.50    2.87    --  111.00 -37.00 -60.00  112
 19  \w     46.00  71.00   0.50    2.87    --  111.00-111.00  90.00   50
 20  \w     48.00  83.00   0.50    2.87    --  111.00-111.00  30.00   70
 21  \w     92.00 121.00   0.50    2.87    --  111.00 -12.00   0.00   58
 22  \w     87.00 113.00   0.50    2.87    --  111.00-111.00  90.00   52
 23  \w     43.00  75.00   0.50    2.87    --  111.00-111.00 -90.00   64
 24  \w     79.00 116.00   0.50    2.87    --  111.00-111.00 -90.00   74
 25  \w    131.00 157.00   0.50    2.87    --  111.00  50.00-180.00   52
 26  \w     79.00 111.00   0.50    2.87    --  111.00-111.00-150.00   64
 27  \w     60.00 121.00   0.50    2.87    --  111.00 -63.00 -60.00  122
 28  \w     53.00  94.00   0.50    2.87    --  111.00 -63.00  60.00   82
 29  \w     99.00 125.00   0.50    2.87    --  111.00 -63.00  60.00   52
 30  \w    102.00 142.00   0.50    2.87    --  111.00 -91.00-120.00   80
 31  \w     86.00 115.00   0.50    2.87    --  111.00-109.00  41.00   58
 32  \w     52.00  77.00   0.50    2.87    --  111.00 -12.00   0.00   50
 33  \w     51.00  77.00   0.50    2.87    --  111.00 -77.00  60.00   52
 34  \w    142.00 172.00   0.50    2.87    --  111.00  50.00-120.00   60
 35  \w     57.00  96.00   0.50    2.87    --  111.00 -37.00  90.00   78
 36  \w     91.00 116.00   0.50    2.87    --  111.00-111.00   0.00   50
 37  \w     44.00  72.00   0.50    2.87    --  111.00 -37.00  30.00   56
 38  \w    151.00 177.00   0.50    2.87    --  111.00  37.00  90.00   52
 39  \w     89.00 115.00   0.50    2.87    --  111.00-111.00-180.00   52
 40  \w     42.00  74.00   0.50    2.87    --  111.00-111.00 120.00   64
 41  \w     83.00 115.00   0.50    2.87    --  111.00-111.00 120.00   64
 42  \w    104.00 167.00   0.50    2.87    --  111.00  12.00-180.00  126
 43  \w     49.00  75.00   0.50    2.87    --  111.00 -91.00  60.00   52
 44  \w     94.00 143.00   0.50    2.87    --  111.00 -91.00  60.00   98
 45  \w     42.00  69.00   0.50    2.87    --  111.00 -25.00-150.00   54
 46  \w     89.00 114.00   0.50    2.87    --  111.00 -25.00-150.00   50
 47  \w     90.00 116.00   0.50    2.87    --  111.00-111.00-120.00   52
 48  \w     84.00 113.00   0.50    2.87    --  111.00-111.00 -30.00   58
 49  \w     49.00  80.00   0.50    2.87    --  111.00 -77.00-120.00   62
 50  \w    101.00 133.00   0.50    2.87    --  111.00 -77.00-120.00   64
 51  \w     69.00 114.00   0.50    2.87    --  111.00 -25.00 120.00   90
 52  \w     62.00  88.00   0.50    2.87    --  111.00 -50.00-120.00   52
 53  \w     85.00 111.00   0.50    2.87    --  111.00 -37.00-150.00   52
 54  \w     93.00 120.00   0.50    2.87    --  111.00 -77.00-150.00   54
 55  \w     46.00  80.00   0.50    2.87    --  111.00 -77.00-150.00   68
 56  \w     57.00 116.00   0.50    2.87    --  111.00 -63.00  90.00  118
 57  \w    120.00 146.00   0.50    2.87    --  111.00  50.00  30.00   52
 58  \w    118.00 175.00   0.50    2.87    --  111.00  37.00  60.00  114
 59  \w     50.00 117.00   0.50    2.87    --  111.00 -50.00  90.00  134
 60  \w     42.00  74.00   0.50    2.87    --  111.00 -91.00-120.00   64
 61  \w     63.00 116.00   0.50    2.87    --  111.00-111.00 150.00  106
 62  \w     55.00  81.00   0.50    2.87    --  111.00 -77.00 -30.00   52
 63  \w    109.00 177.00   0.50    2.87    --  111.00  37.00   0.00  136
 64  \w    113.00 139.00   0.50    2.87    --  111.00 178.00 -60.00   52
 65  \w     52.00 113.00   0.50    2.87    --  111.00 -50.00 -60.00  122
 66  \w     80.00 106.00   0.50    2.87    --  111.00 178.00 -60.00   52
 67  \w     44.00  69.00   0.50    2.87    --  111.00 -25.00  60.00   50
 68  \w     43.00  72.00   0.50    2.87    --  111.00 -91.00 -30.00   58
 69  \w     94.00 127.00   0.50    2.87    --  111.00 -91.00 -30.00   66
 70  \w     88.00 122.00   0.50    2.87    --  111.00  77.00  90.00   68
 71  \w    150.00 176.00   0.50    2.87    --  111.00  77.00  90.00   52
 72  \w     55.00  85.00   0.50    2.87    --  111.00 -77.00-180.00   60
 73  \w     60.00  86.00   0.50    2.87    --  111.00 -91.00  30.00   52
 74  \w    114.00 139.00   0.50    2.87    --  111.00  50.00-120.00   50
 75  \w    102.00 132.00   0.50    2.87    --  111.00 -77.00 -30.00   60
 76  \w    128.00 172.00   0.50    2.87    --  111.00  37.00-150.00   88
 77  \w    127.00 176.00   0.50    2.87    --  111.00  25.00  30.00   98
 78  \w     45.00  85.00   0.50    2.87    --  111.00 -37.00-180.00   80
 79  \w     45.00  78.00   0.50    2.87    --  111.00 -37.00-150.00   66
 80  \w    101.00 127.00   0.50    2.87    --  111.00 -77.00   0.00   52
 81  \w    100.00 132.00   0.50    2.87    --  111.00 -77.00 150.00   64
 82  \w    116.00 154.00   0.50    2.87    --  111.00  50.00 -30.00   76
 83  \w    118.00 144.00   0.50    2.87    --  111.00  37.00-180.00   52
 84  \w    111.00 136.00   0.50    2.87    --  111.00  37.00 -60.00   50
 85  \w    150.00 177.00   0.50    2.87    --  111.00  37.00 -60.00   54
 86  \w    121.00 147.00   0.50    2.87    --  111.00  37.00  30.00   52
 87  \w    108.00 156.00   0.50    2.87    --  111.00  37.00 120.00   96
 88  \w    117.00 142.00   0.50    2.87    --  111.00  25.00-180.00   50
 89  \w    126.00 154.00   0.50    2.87    --  111.00  25.00-120.00   56
 90  \w    113.00 159.00   0.50    2.87    --  111.00  25.00 -30.00   92
 91  \w     78.00 109.00   0.50    2.87    --  111.00-111.00 -60.00   62
 92  \w    102.00 148.00   0.50    2.87    --  111.00 109.00 137.00   92
 93  \w    153.00 178.00   0.50    2.87    --  111.00 111.00  60.00   50
 94  \w     91.00 117.00   0.50    2.87    --  111.00 -63.00 -30.00   52
 95  \w     59.00  85.00   0.50    2.87    --  111.00 -63.00  30.00   52
 96  \w    138.00 175.00   0.50    2.87    --  111.00  77.00-150.00   74
 97  \w     77.00 103.00   0.50    2.87    --  111.00 -91.00   0.00   52
 98  \w     42.00 100.00   0.50    2.87    --  111.00 -91.00-150.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Pilatus 200/300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            131024
_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         80.409
_diffrn_reflns_theta_min         3.492
_exptl_absorpt_coefficient_mu    4.258
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull light colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             2366
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.392
_refine_diff_density_min         -3.251
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1209
_refine_ls_number_reflns         25332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0584
_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^)+(0.1026P)^2^+12.9419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22477
_reflns_number_total             25332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00338e2.cif
_cod_data_source_block           ph18030
_cod_depositor_comments
'Adding full bibliography for 7718388--7718395.cif.'
_cod_original_cell_volume        5816.40(11)
_cod_database_code               7718395
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.815
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C8A(H8A), C11A(H11A), C23(H23), C8(H8), C14A(H14A), C14(H14), C5(H5),
 C32A(H32A), C11(H11), C32(H32), C5A(H5A), C58(H58)
2.b Secondary CH2 refined with riding coordinates:
 C35A(H35B,H35A), C35(H35C,H35D)
2.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C28A(H28A), C30A(H30A), C29A(H29A), C27A(H27A), C42(H42), C21(H21),
 C29(H29), C51A(H51A), C53A(H53A), C45A(H45A), C57(H57), C49A(H49A), C41A(H41A),
  C30(H30), C21A(H21A), C48A(H48A), C50A(H50A), C19(H19), C27(H27), C41(H41),
 C57A(H57A), C20(H20), C55(H55), C47A(H47A), C54A(H54A), C54(H54), C55A(H55A),
 C18A(H18A), C42A(H42A), C44A(H44A), C3A(H3A), C53(H53), C28(H28), C43(H43),
 C3(H3), C19A(H19A), C2A(H2A), C50(H50), C56(H56), C51(H51), C47(H47), C2(H2),
 C48(H48), C43A(H43A), C44(H44), C56A(H56A), C49(H49), C45(H45), C20A(H20A)
2.d Idealised Me refined as rotating group:
 C13A(H13A,H13B,H13C), C12A(H12A,H12B,H12C), C16A(H16A,H16B,H16C), C6(H6A,H6B,
 H6C), C6A(H6AA,H6AB,H6AC), C9A(H9AA,H9AB,H9AC), C15(H15D,H15E,H15F), C7(H7A,
 H7B,H7C), C15A(H15A,H15B,H15C), C13(H13D,H13E,H13F), C16(H16D,H16E,H16F),
 C10(H10D,H10E,H10F), C9(H9A,H9B,H9C), C36(H36D,H36E,H36F), C33(H33D,H33E,H33F),
  C38A(H38A,H38B,H38C), C36A(H36A,H36B,H36C), C34(H34D,H34E,H34F), C25(H25A,
 H25B,H25C), C10A(H10A,H10B,H10C), C33A(H33A,H33B,H33C), C37A(H37A,H37B,H37C),
 C34A(H34A,H34B,H34C), C37(H37D,H37E,H37F), C12(H12D,H12E,H12F), C38(H38D,H38E,
 H38F), C24(H24A,H24B,H24C), C7A(H7AA,H7AB,H7AC), C60(H60A,H60B,H60C), C59(H59A,
 H59B,H59C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76715
_shelx_hkl_checksum              96448
_shelx_fab_checksum              89147
_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
;