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_7718394
_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         'C72 H84 Lu N5 P2, 1[C7H16]'
_chemical_formula_sum            'C79 H100 Lu N5 P2'
_chemical_formula_weight         1356.54
_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                74.4510(10)
_cell_angle_beta                 89.2780(10)
_cell_angle_gamma                71.2670(10)
_cell_formula_units_Z            2
_cell_length_a                   12.74240(10)
_cell_length_b                   14.66260(10)
_cell_length_c                   20.5619(2)
_cell_measurement_reflns_used    61724
_cell_measurement_temperature    110.9(2)
_cell_measurement_theta_max      80.0090
_cell_measurement_theta_min      3.6470
_cell_volume                     3493.66(6)
_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      110.9
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -62.00  26.00   0.50    0.50    --  -38.50  77.00 -30.00  176
  2  \w    -50.00  25.00   0.50    0.50    --  -38.50  57.00  90.00  150
  3  \w   -105.00 -35.00   0.50    0.50    --  -38.50 -37.00-120.00  140
  4  \w   -105.00 -35.00   0.50    0.50    --  -38.50 -37.00 -30.00  140
  5  \w    -90.00  -2.00   0.50    0.50    --  -38.50 125.00 120.00  176
  6  \w    -42.00  28.00   0.50    0.50    --  -38.50  37.00 -30.00  140
  7  \w    -50.00  25.00   0.50    0.50    --  -38.50  57.00  60.00  150
  8  \w    -44.00  31.00   0.50    0.50    --  -38.50  19.00-120.00  150
  9  \w     23.00  99.00   0.50    0.50    --   47.56-125.00-150.00  152
 10  \w    105.00 175.00   0.50    0.50    --  111.00  50.00-180.00  140
 11  \w     48.00 126.00   0.50    0.50    --  111.00 -63.00   0.00  156
 12  \w     48.00 126.00   0.50    0.50    --  111.00 -63.00-150.00  156
 13  \w     44.00 114.00   0.50    0.50    --  111.00 -37.00 -90.00  140
 14  \w     41.00 121.00   0.50    0.50    --  111.00 -12.00 150.00  160
 15  \w    107.00 178.00   0.50    0.50    --  111.00  25.00 -60.00  142
 16  \w     44.00 114.00   0.50    0.50    --  111.00 -37.00   0.00  140
 17  \w     47.00 117.00   0.50    0.50    --  111.00 -50.00  90.00  140
 18  \w     41.00 115.00   0.50    0.50    --  111.00-109.00-136.00  148
 19  \w     41.00 115.00   0.50    0.50    --  111.00 -25.00   0.00  148
 20  \w    116.00 155.00   0.50    0.50    --  111.00  25.00  90.00   78
 21  \w     41.00 116.00   0.50    0.50    --  111.00-111.00   0.00  150
 22  \w     79.00 105.00   0.50    0.50    --  111.00 -12.00 -90.00   52
 23  \w     88.00 114.00   0.50    0.50    --  111.00-111.00  90.00   52
 24  \w     77.00 116.00   0.50    0.50    --  111.00-111.00 -90.00   78
 25  \w     88.00 113.00   0.50    0.50    --  111.00  77.00  30.00   50
 26  \w    121.00 147.00   0.50    0.50    --  111.00  77.00  30.00   52
 27  \w     49.00 103.00   0.50    0.50    --  111.00 -91.00 -30.00  108
 28  \w     55.00  93.00   0.50    0.50    --  111.00 -77.00  90.00   76
 29  \w    103.00 129.00   0.50    0.50    --  111.00 -77.00  90.00   52
 30  \w     42.00 112.00   0.50    0.50    --  111.00-111.00  60.00  140
 31  \w     90.00 116.00   0.50    0.50    --  111.00-111.00-180.00   52
 32  \w     81.00 107.00   0.50    0.50    --  111.00 -25.00 150.00   52
 33  \w     42.00  72.00   0.50    0.50    --  111.00 -25.00 150.00   60
 34  \w     82.00 117.00   0.50    0.50    --  111.00 -50.00 150.00   70
 35  \w     84.00 110.00   0.50    0.50    --  111.00 -50.00-150.00   52
 36  \w     58.00  92.00   0.50    0.50    --  111.00 178.00-120.00   68
 37  \w     78.00 108.00   0.50    0.50    --  111.00 -37.00  90.00   60
 38  \w     45.00  98.00   0.50    0.50    --  111.00-111.00 -30.00  106
 39  \w     49.00  84.00   0.50    0.50    --  111.00 -63.00  30.00   70
 40  \w     94.00 125.00   0.50    0.50    --  111.00 -63.00  30.00   62
 41  \w     41.00  71.00   0.50    0.50    --  111.00 -12.00   0.00   60
 42  \w     81.00 121.00   0.50    0.50    --  111.00 -12.00   0.00   80
 43  \w    102.00 171.00   0.50    0.50    --  111.00  12.00-180.00  138
 44  \w    115.00 165.00   0.50    0.50    --  111.00  37.00  30.00  100
 45  \w    108.00 165.00   0.50    0.50    --  111.00  37.00 -60.00  114
 46  \w    132.00 161.00   0.50    0.50    --  111.00  25.00 -30.00   58
 47  \w     83.00 109.00   0.50    0.50    --  111.00 -91.00 -60.00   52
 48  \w     43.00  68.00   0.50    0.50    --  111.00 -91.00 150.00   50
 49  \w    111.00 141.00   0.50    0.50    --  111.00 -91.00 150.00   60
 50  \w     57.00  82.00   0.50    0.50    --  111.00 -77.00   0.00   50
 51  \w    102.00 128.00   0.50    0.50    --  111.00 -77.00   0.00   52
 52  \w     83.00 111.00   0.50    0.50    --  111.00-111.00  30.00   56
 53  \w     91.00 116.00   0.50    0.50    --  111.00-111.00 120.00   50
 54  \w    101.00 132.00   0.50    0.50    --  111.00 111.00-180.00   62
 55  \w    152.00 177.00   0.50    0.50    --  111.00 111.00-180.00   50
 56  \w     71.00 107.00   0.50    0.50    --  111.00 -25.00  60.00   72
 57  \w    100.00 164.00   0.50    0.50    --  111.00 111.00  30.00  128
 58  \w     84.00 126.00   0.50    0.50    --  111.00 -63.00  90.00   84
 59  \w     66.00 102.00   0.50    0.50    --  111.00 -50.00 -60.00   72
 60  \w     80.00 106.00   0.50    0.50    --  111.00 -50.00   0.00   52
 61  \w     48.00  74.00   0.50    0.50    --  111.00 -50.00 120.00   52
 62  \w     58.00  84.00   0.50    0.50    --  111.00 -91.00 120.00   52
 63  \w     93.00 150.00   0.50    0.50    --  111.00 178.00 -30.00  114
 64  \w     52.00 115.00   0.50    0.50    --  111.00-111.00 -60.00  126
 65  \w     80.00 125.00   0.50    0.50    --  111.00 -77.00 -60.00   90
 66  \w     94.00 120.00   0.50    0.50    --  111.00 -91.00 120.00   52
 67  \w    106.00 132.00   0.50    0.50    --  111.00  50.00 120.00   52
 68  \w    111.00 137.00   0.50    0.50    --  111.00  37.00 -30.00   52
 69  \w     55.00  81.00   0.50    0.50    --  111.00 -50.00-150.00   52
 70  \w     91.00 117.00   0.50    0.50    --  111.00 -50.00 120.00   52
 71  \w     54.00  80.00   0.50    0.50    --  111.00 -50.00 -90.00   52
 72  \w     73.00 115.00   0.50    0.50    --  111.00-111.00-120.00   84
 73  \w    146.00 171.00   0.50    0.50    --  111.00  12.00 -90.00   50
 74  \w     51.00  85.00   0.50    0.50    --  111.00 -37.00 150.00   68
 75  \w    126.00 151.00   0.50    0.50    --  111.00 178.00-120.00   50
 76  \w    118.00 144.00   0.50    0.50    --  111.00 178.00 -90.00   52
 77  \w    123.00 167.00   0.50    0.50    --  111.00 111.00 120.00   88
;
_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  0.0448
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            79766
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.430
_diffrn_reflns_theta_min         3.314
_exptl_absorpt_coefficient_mu    3.480
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77129
_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    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.380
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00047(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         15242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+1.6699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14588
_reflns_number_total             15242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00338e2.cif
_cod_data_source_block           ph18067
_cod_depositor_comments
'Adding full bibliography for 7718388--7718395.cif.'
_cod_database_code               7718394
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.722
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C32(H32), C11(H11), C6(H6), C5(H5A), C23(H23)
2.b Aromatic/amide H refined with riding coordinates:
 C60(H60), C28(H28), C69(H69), C72(H72), C30(H30), C41(H41), C31(H31),
 C68(H68), C65(H65), C66(H66), C27(H27), C57(H57), C3(H3), C2(H2), C56(H56),
 C70(H70), C62(H62), C22(H22), C64(H64), C63(H63), C39(H39), C18(H18), C71(H71),
  C19(H19), C40(H40), C37(H37), C58(H58), C51(H51), C49(H49), C59(H59),
 C43(H43), C21(H21), C50(H50), C38(H38), C47(H47), C53(H53), C46(H46), C52(H52),
  C44(H44), C45(H45)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C10(H10A,H10B,
 H10C), C15(H15A,H15B,H15C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C34(H34A,H34B,
 H34C), C33(H33A,H33B,H33C), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              98503
_shelx_hkl_checksum              42050
_shelx_fab_checksum              17160
_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
;