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_7718391
_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         '2(C58 H88 Lu N5 P2)'
_chemical_formula_sum            'C116 H176 Lu2 N10 P4'
_chemical_formula_weight         2184.48
_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   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                90
_cell_angle_beta                 95.2220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.96740(10)
_cell_length_b                   17.02750(10)
_cell_length_c                   21.66410(10)
_cell_measurement_reflns_used    39142
_cell_measurement_temperature    110.3(4)
_cell_measurement_theta_max      79.9420
_cell_measurement_theta_min      3.3010
_cell_volume                     5498.34(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      110.3
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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    -42.00  28.00   0.50    0.50    --  -38.50  37.00-150.00  140
  2  \w   -108.00 -49.00   0.50    0.50    --  -38.50 -19.00 120.00  118
  3  \w    -38.00  27.00   0.50    0.50    --  -38.50  37.00 -60.00  130
  4  \w    -45.00  -4.00   0.50    0.50    --  -38.50 125.00   0.00   82
  5  \w     -6.00  26.00   0.50    0.50    --  -38.50  37.00  60.00   64
  6  \w     44.00 114.00   0.50    0.50    --   47.56  37.00-120.00  140
  7  \w     47.00 114.00   0.50    0.50    --   47.56  37.00 -60.00  134
  8  \w     41.00 101.00   0.50    1.83    --  111.00-111.00 -60.00  120
  9  \w     62.00  95.00   0.50    1.83    --  111.00 -50.00 150.00   66
 10  \w     48.00 114.00   0.50    1.83    --  111.00 -37.00-180.00  132
 11  \w     53.00  79.00   0.50    1.83    --  111.00 -50.00-150.00   52
 12  \w     78.00 104.00   0.50    1.83    --  111.00 -50.00 -30.00   52
 13  \w    140.00 167.00   0.50    1.83    --  111.00  37.00 120.00   54
 14  \w    102.00 133.00   0.50    1.83    --  111.00 178.00 -60.00   62
 15  \w    121.00 147.00   0.50    1.83    --  111.00 111.00 -30.00   52
 16  \w     73.00 106.00   0.50    1.83    --  111.00 -50.00  60.00   66
 17  \w    153.00 178.00   0.50    1.83    --  111.00  25.00  60.00   50
 18  \w     48.00 109.00   0.50    1.83    --  111.00 -63.00-150.00  122
 19  \w    130.00 178.00   0.50    1.83    --  111.00  25.00-180.00   96
 20  \w    110.00 136.00   0.50    1.83    --  111.00  37.00  60.00   52
 21  \w    152.00 178.00   0.50    1.83    --  111.00 111.00  30.00   52
 22  \w    133.00 168.00   0.50    1.83    --  111.00  63.00  60.00   70
 23  \w     87.00 113.00   0.50    1.83    --  111.00 -25.00-120.00   52
 24  \w     88.00 117.00   0.50    1.83    --  111.00 -50.00-150.00   58
 25  \w     43.00  76.00   0.50    1.83    --  111.00 -25.00-180.00   66
 26  \w     78.00 117.00   0.50    1.83    --  111.00 -50.00   0.00   78
 27  \w    112.00 145.00   0.50    1.83    --  111.00  12.00-180.00   66
 28  \w     66.00  99.00   0.50    1.83    --  111.00 178.00 -60.00   66
 29  \w    113.00 143.00   0.50    1.83    --  111.00  25.00  60.00   60
 30  \w     49.00 111.00   0.50    1.83    --  111.00 -55.00 -28.00  124
 31  \w     46.00  71.00   0.50    1.83    --  111.00 -37.00  60.00   50
 32  \w     90.00 115.00   0.50    1.83    --  111.00 -25.00 -30.00   50
 33  \w    149.00 174.00   0.50    1.83    --  111.00  12.00-120.00   50
 34  \w     43.00  70.00   0.50    1.83    --  111.00 -25.00 -30.00   54
 35  \w     86.00 113.00   0.50    1.83    --  111.00 -37.00  60.00   54
 36  \w    129.00 167.00   0.50    1.83    --  111.00  50.00-120.00   76
 37  \w     44.00 109.00   0.50    1.83    --  111.00 -37.00 -30.00  130
 38  \w     46.00  83.00   0.50    1.83    --  111.00 -37.00 150.00   74
 39  \w    108.00 146.00   0.50    1.83    --  111.00  12.00-120.00   76
 40  \w    135.00 171.00   0.50    1.83    --  111.00  63.00-150.00   72
 41  \w     53.00 107.00   0.50    1.83    --  111.00 -50.00 -90.00  108
 42  \w    108.00 134.00   0.50    1.83    --  111.00  25.00 150.00   52
 43  \w    107.00 173.00   0.50    1.83    --  111.00  50.00  90.00  132
 44  \w    115.00 142.00   0.50    1.83    --  111.00 -91.00 -30.00   54
 45  \w    109.00 134.00   0.50    1.83    --  111.00  37.00 -30.00   50
 46  \w     50.00  95.00   0.50    1.83    --  111.00 -91.00 -30.00   90
;
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            64880
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.334
_diffrn_reflns_theta_min         3.307
_exptl_absorpt_coefficient_mu    4.285
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69932
_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            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         11972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+7.2766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11106
_reflns_number_total             11972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00338e2.cif
_cod_data_source_block           ph18062
_cod_depositor_comments
'Adding full bibliography for 7718388--7718395.cif.'
_cod_database_code               7718391
_shelx_shelxl_version_number     2019/3
_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:
 C41(H41), C56(H56), C6(H6), C44(H44), C11(H11), C12(H12), C23(H23), C5(H5A),
 C53(H53), C32(H32)
2.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C39(H39), C30(H30), C19(H19), C2(H2), C27(H27), C3(H3), C22(H22),
 C49(H49), C28(H28), C37(H37), C21(H21), C51(H51), C18(H18), C38(H38), C50(H50)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C7(H7A,H7B,
 H7C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C57(H57A,H57B,H57C), C15(H15A,
 H15B,H15C), C58(H58A,H58B,H58C), C55(H55A,H55B,H55C), C24(H24A,H24B,H24C),
 C10(H10A,H10B,H10C), C43(H43A,H43B,H43C), C25(H25A,H25B,H25C), C8(H8A,H8B,H8C),
  C9(H9A,H9B,H9C), C42(H42A,H42B,H42C), C34(H34A,H34B,H34C), C33(H33A,H33B,
 H33C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              79544
_shelx_hkl_checksum              4994
_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
;