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_7718393
_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 H44 Cl2 Lu N7 P2, C7 H8'
_chemical_formula_sum            'C35 H52 Cl2 Lu N7 P2'
_chemical_formula_weight         878.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-03-06
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-03-07 deposited with the CCDC.	2025-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.413(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.5525(5)
_cell_length_b                   13.3420(3)
_cell_length_c                   30.8950(7)
_cell_measurement_reflns_used    29951
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      30.9830
_cell_measurement_theta_min      3.6250
_cell_volume                     7951.0(3)
_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      100.0(3)
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.808
_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   8.00   0.50   66.80    --    3.76 -41.00-105.00  140
  2  \w    -66.00  73.00   0.50   66.80    --    3.76   0.00 120.00  278
  3  \w     -8.00  62.00   0.50   66.80    --   -4.54  38.00-150.00  140
  4  \w      0.00  50.00   0.50   66.80    --    3.76  38.00 -90.00  100
  5  \w    -20.00  32.00   0.50   66.80    --   -4.54 -99.00  60.00  104
;
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.808
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            48568
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.808
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.751
_diffrn_reflns_theta_min         3.394
_exptl_absorpt_coefficient_mu    2.732
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87557
_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    1.468
_exptl_crystal_description       plate
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         10026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+15.3420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8804
_reflns_number_total             10026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00338e2.cif
_cod_data_source_block           ph17066
_cod_depositor_comments
'Adding full bibliography for 7718388--7718395.cif.'
_cod_database_code               7718393
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.342
_shelx_estimated_absorpt_t_min   0.251
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8), C14(H14), C5(H5), C11(H11)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C19(H19), C2(H2), C25(H25), C33(H33), C31(H31), C35(H35), C32(H32),
 C34(H34)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C27(H27A,H27B,H27C), C16(H16A,H16B,H16C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C6(H6A,H6B,H6C), C21(H21A,H21B,H21C), C15(H15A,
 H15B,H15C), C7(H7A,H7B,H7C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C),
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              35462
_shelx_hkl_checksum              16645
_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
;