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_7718388
_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         'C42 H72.699 N3 P2 Sc Si2'
_chemical_formula_sum            'C42 H72.7 N3 P2 Sc Si2'
_chemical_formula_weight         782.81
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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                 105.8330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3033(2)
_cell_length_b                   17.2331(2)
_cell_length_c                   17.6226(2)
_cell_measurement_reflns_used    29788
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.1830
_cell_measurement_theta_min      3.6690
_cell_volume                     4763.34(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (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      100
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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  38.00 -60.00  140
  2  \w   -108.00  31.00   0.50    0.50    --  -38.50   0.00 -30.00  278
  3  \w   -105.00 -35.00   0.50    0.50    --  -38.50 -38.00 -30.00  140
  4  \w     46.00 115.00   0.50    0.50    --   49.06  38.00 150.00  138
  5  \w     46.00 115.00   0.50    0.50    --   49.06  38.00  60.00  138
  6  \w     38.00 110.00   0.50    0.62    --  106.38 -30.00 -90.00  144
  7  \w     42.00 130.00   0.50    0.62    --  106.38 -77.00 150.00  176
  8  \w     38.00 109.00   0.50    0.62    --  106.38 -94.00 150.00  142
  9  \w     38.00 115.00   0.50    0.62    --  106.38 -15.00-150.00  154
 10  \w     38.00 115.00   0.50    0.62    --  106.38 -15.00 -60.00  154
 11  \w     38.00 110.00   0.50    0.62    --  106.38 -30.00 -30.00  144
 12  \w     93.00 169.00   0.50    0.62    --  106.38  61.00 -60.00  152
 13  \w     38.00 109.00   0.50    0.62    --  106.38 -94.00-180.00  142
 14  \w     42.00 111.00   0.50    0.62    --  106.38 -45.00 -90.00  138
 15  \w     38.00 110.00   0.50    0.62    --  106.38 -30.00-180.00  144
 16  \w     38.00 115.00   0.50    0.62    --  106.38 -15.00   0.00  154
 17  \w     26.00 114.00   0.50    0.50    --   49.06  77.00-180.00  176
 18  \w     23.00 100.00   0.50    0.50    --   49.06-125.00 120.00  154
 19  \w     26.00 114.00   0.50    0.50    --   49.06  77.00 -30.00  176
 20  \w     26.00 114.00   0.50    0.50    --   49.06  77.00-120.00  176
;
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47561
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.631
_diffrn_reflns_theta_min         3.657
_exptl_absorpt_coefficient_mu    2.649
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       plate
_exptl_crystal_F_000             1699
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Heptane'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.00026(4)
_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   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         9883
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0505P)^2^+3.0147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8927
_reflns_number_total             9883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00338e2.cif
_cod_data_source_block           ph16006
_cod_depositor_comments
'Adding full bibliography for 7718388--7718395.cif.'
_cod_original_formula_sum        'C42 H72.70 N3 P2 Sc Si2'
_cod_database_code               7718388
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.879
_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. Restrained distances
 C23-C24A \\sim C23-C24B
 with sigma of 0.02
 C20-C24A \\sim C20-C24B
 with sigma of 0.02
 C25A-C24A \\sim C25A-C24B
 with sigma of 0.02
 C25A-C24A \\sim C25B-C24A
 with sigma of 0.02
 C25A-C24B \\sim C25B-C24B
 with sigma of 0.02
3. Others
 Sof(C24B)=Sof(H24B)=1-FVAR(1)
 Sof(C24A)=Sof(H24A)=FVAR(1)
 Sof(C25B)=Sof(H25A)=Sof(H25B)=Sof(H25C)=1-FVAR(2)
 Sof(C25A)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C11(H11), C12(H12), C24A(H24A), C32(H32)
4.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C18(H18), C19(H19), C21(H21), C22(H22), C27(H27), C28(H28),
 C30(H30), C31(H31)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C25B(H25A,H25B,H25C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              10655
_shelx_hkl_checksum              57754
_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
;