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_7718392
_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         'C50 H81 Lu N4 P2 Si'
_chemical_formula_sum            'C50 H81 Lu N4 P2 Si'
_chemical_formula_weight         1003.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2025-01-16 deposited with the CCDC.	2025-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.2891(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.59705(9)
_cell_length_b                   20.55239(15)
_cell_length_c                   11.79321(10)
_cell_measurement_reflns_used    22617
_cell_measurement_temperature    107.75(15)
_cell_measurement_theta_max      79.8870
_cell_measurement_theta_min      4.0630
_cell_volume                     2581.85(4)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      107.75(15)
_diffrn_detector                 'CCD plate'
_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    -44.00  31.00   0.50    0.50    --  -38.50  19.00 150.00  150
  2  \w    -50.00  25.00   0.50    0.50    --  -38.50  57.00  30.00  150
  3  \w   -105.00 -35.00   0.50    0.50    --  -38.50 -37.00-150.00  140
  4  \w     42.00 117.00   0.50    0.50    --   47.56  19.00 -30.00  150
  5  \w    -16.00  59.00   0.50    0.50    --   47.56 -57.00 -30.00  150
  6  \w    -22.00  54.00   0.50    0.50    --   47.56 -19.00 -30.00  152
  7  \w     41.00 143.00   0.50    1.31    --  111.00 -91.00 -90.00  204
  8  \w    105.00 175.00   0.50    1.31    --  111.00  50.00  90.00  140
  9  \w     47.00 117.00   0.50    1.31    --  111.00 -50.00 120.00  140
 10  \w     47.00 117.00   0.50    1.31    --  111.00 -50.00-150.00  140
 11  \w     46.00 134.00   0.50    1.31    --  111.00 -77.00-180.00  176
 12  \w     57.00  90.00   0.50    1.31    --  111.00 -50.00 -30.00   66
 13  \w     43.00 100.00   0.50    1.31    --  111.00 -25.00 120.00  114
 14  \w     96.00 173.00   0.50    1.31    --  111.00  63.00 120.00  154
 15  \w    118.00 154.00   0.50    1.31    --  111.00 111.00  90.00   72
 16  \w    140.00 174.00   0.50    1.31    --  111.00  50.00  60.00   68
 17  \w     52.00 116.00   0.50    1.31    --  111.00-111.00  60.00  128
 18  \w     43.00 105.00   0.50    1.31    --  111.00-111.00 -60.00  124
 19  \w     55.00 100.00   0.50    1.31    --  111.00 -12.00 120.00   90
 20  \w     61.00 114.00   0.50    1.31    --  111.00 -50.00   0.00  106
 21  \w     55.00  81.00   0.50    1.31    --  111.00 -37.00   0.00   52
 22  \w     71.00 101.00   0.50    1.31    --  111.00 -63.00 -60.00   60
 23  \w     47.00  90.00   0.50    1.31    --  111.00 -50.00  90.00   86
 24  \w     91.00 117.00   0.50    1.31    --  111.00 -91.00 -30.00   52
 25  \w     71.00 133.00   0.50    1.31    --  111.00 -77.00   0.00  124
 26  \w     73.00 125.00   0.50    1.31    --  111.00 -63.00 -90.00  104
 27  \w     44.00 115.00   0.50    1.31    --  111.00 -25.00 -60.00  142
 28  \w    140.00 166.00   0.50    1.31    --  111.00  50.00 150.00   52
 29  \w    108.00 135.00   0.50    1.31    --  111.00  50.00   0.00   54
 30  \w    119.00 149.00   0.50    1.31    --  111.00 178.00-150.00   60
 31  \w     80.00 105.00   0.50    1.31    --  111.00-111.00   0.00   50
 32  \w     62.00 113.00   0.50    1.31    --  111.00 178.00-150.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Pilatus 200/300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0399646000
_diffrn_orient_matrix_UB_12      0.0720435000
_diffrn_orient_matrix_UB_13      0.0169823000
_diffrn_orient_matrix_UB_21      -0.0359834000
_diffrn_orient_matrix_UB_22      0.0045039000
_diffrn_orient_matrix_UB_23      0.1123242000
_diffrn_orient_matrix_UB_31      0.1341829000
_diffrn_orient_matrix_UB_32      -0.0202349000
_diffrn_orient_matrix_UB_33      0.0856189000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30369
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.149
_diffrn_reflns_theta_min         4.081
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.723
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87929
_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 white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 4338 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.022(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         10423
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+3.2072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    0.898
_reflns_Friedel_fraction_max     0.846
_reflns_number_gt                10128
_reflns_number_total             10423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00338e2.cif
_cod_data_source_block           ph18052
_cod_depositor_comments
'Adding full bibliography for 7718388--7718395.cif.'
_cod_database_code               7718392
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C50 H79 Lu N4 P2 Si'
_shelx_estimated_absorpt_t_max   0.650
_shelx_estimated_absorpt_t_min   0.332
_reflns_odcompleteness_completeness 98.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95
_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:
 C5(H5), C23(H23), C14(H14), C45(H45), C8(H8), C32(H32), C11(H11), C48(H48)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C3(H3), C30(H30), C21(H21), C28(H28), C29(H29), C19(H19), C18(H18),
 C44(H44), C43(H43), C42(H42), C20(H20), C2(H2)
2.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C25(H25A,H25B,H25C), C6(H6A,H6B,H6C), C13(H13A,H13B,
 H13C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C7(H7A,H7B,H7C), C46(H46A,
 H46B,H46C), C33(H33A,H33B,H33C), C50(H50A,H50B,H50C), C24(H24A,H24B,H24C),
 C38(H38A,H38B,H38C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C),
  C49(H49A,H49B,H49C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C), C37(H37A,H37B,
 H37C)
;
_shelx_res_checksum              65859
_shelx_hkl_checksum              55303
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.226
_oxdiff_exptl_absorpt_empirical_full_min 0.845