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_7718389
_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         'C28 H45 N7 P2'
_chemical_formula_sum            'C28 H45 N7 P2'
_chemical_formula_weight         541.65
_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
_audit_creation_date             2025-02-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-11 deposited with the CCDC.	2025-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.5340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.09120(10)
_cell_length_b                   24.3906(2)
_cell_length_c                   11.85320(10)
_cell_measurement_reflns_used    19539
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      79.5850
_cell_measurement_theta_min      3.6030
_cell_volume                     3040.23(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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 0.988
_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   -102.00 -27.00   0.50    0.51    --  -38.50 -57.00-180.00  150
  2  \w    -50.00  25.00   0.50    0.51    --  -38.50  57.00 -90.00  150
  3  \w   -103.00 -15.00   0.50    0.51    --  -38.50 -77.00-150.00  176
  4  \w   -102.00 -27.00   0.50    0.51    --  -38.50 -57.00 120.00  150
  5  \w    -14.00  61.00   0.50    0.51    --   49.06 -57.00-120.00  150
  6  \w    107.00 177.00   0.50    2.04    --  111.00  38.00-180.00  140
  7  \w     41.00 116.00   0.50    2.04    --  111.00-111.00 150.00  150
  8  \w     47.00 117.00   0.50    2.04    --  111.00 -50.00  90.00  140
  9  \w     45.00 115.00   0.50    2.04    --  111.00 -38.00 -60.00  140
 10  \w    105.00 175.00   0.50    2.04    --  111.00  50.00-150.00  140
 11  \w    105.00 175.00   0.50    2.04    --  111.00  50.00 150.00  140
 12  \w     41.00 143.00   0.50    2.04    --  111.00 -91.00  90.00  204
 13  \w     41.00 115.00   0.50    2.04    --  111.00 -25.00  30.00  148
 14  \w    105.00 175.00   0.50    2.04    --  111.00  50.00  60.00  140
 15  \w     41.00 143.00   0.50    2.04    --  111.00 -91.00 120.00  204
 16  \w     47.00 117.00   0.50    2.04    --  111.00 -50.00 150.00  140
 17  \w     41.00 143.00   0.50    2.04    --  111.00 -91.00 120.00  204
 18  \w    107.00 178.00   0.50    2.04    --  111.00  25.00 -90.00  142
 19  \w     41.00 116.00   0.50    2.04    --  111.00-111.00 -60.00  150
 20  \w     48.00 126.00   0.50    2.04    --  111.00 -63.00   0.00  156
 21  \w    101.00 178.00   0.50    2.04    --  111.00  12.00-120.00  154
 22  \w     42.00  99.00   0.50    2.04    --  111.00 -25.00-120.00  114
;
_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     0.0321
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33645
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.995
_diffrn_reflns_theta_min         3.624
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.183
_exptl_crystal_description       prism
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         6555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0446P)^2^+1.8591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5868
_reflns_number_total             6555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00338e2.cif
_cod_data_source_block           ph17028
_cod_depositor_comments
'Adding full bibliography for 7718388--7718395.cif.'
_cod_database_code               7718389
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.518
_shelx_estimated_absorpt_t_min   0.313
_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:
 C11(H11), C6(H6), C12(H12), C5(H5)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C2(H2), C25(H25), C19(H19)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C22(H22A,H22B,H22C), C7(H7A,H7B,
 H7C), C21(H21A,H21B,H21C), C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C16(H16A,
 H16B,H16C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C)
;
_shelx_res_checksum              21764
_shelx_hkl_checksum              32145
_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
;