Stabilization of reactive rare earth alkyl complexes through mechanistic studies.
Tanuhadi, Elias; Bair, Anna S.; Johnson, Mary; Fontaine, Philip; Klosin, Jerzy; Pal, Sudipta; Arnold, Polly L.; Chemical science 16 (2024) 280–287; doi:10.1039/d4sc05983b

data_1573274
_publ_section_title
;
 Stabilization of reactive rare earth alkyl complexes through mechanistic
 studies.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              280
_journal_page_last               287
_journal_paper_doi               10.1039/d4sc05983b
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C20 H51 Lu O4 Si3'
_chemical_formula_sum            'C20 H51 Lu O4 Si3'
_chemical_formula_weight         614.84
_chemical_name_systematic        Lur3G3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-04-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-04-25 deposited with the CCDC.	2024-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.415(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6318(3)
_cell_length_b                   9.5844(3)
_cell_length_c                   29.2885(7)
_cell_measurement_reflns_used    22543
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6410
_cell_measurement_theta_min      3.1930
_cell_volume                     2984.40(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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     33.00  58.00   0.50    0.50    --    3.98  50.00 -73.00   50
  2  \w     -9.00  39.00   0.50    0.50    --    3.98 -99.00 -90.00   96
  3  \w    -12.00  39.00   0.50    0.50    --    3.98 -99.00 150.00  102
  4  \w    -45.00  28.00   0.50    0.50    --    3.98 -77.00  90.00  146
  5  \w    -49.00 -24.00   0.50    0.50    --    3.98 -50.00 139.00   50
  6  \w    -14.00  11.00   0.50    0.50    --   -3.67 -50.00 139.00   50
  7  \w    -72.00 -32.00   0.50    0.50    --   -3.67 -50.00 139.00   80
  8  \w    -45.00  21.00   0.50    0.50    --   -3.67 -77.00 -60.00  132
  9  \w      1.00  26.00   0.50    0.50    --   -3.67  50.00 -73.00   50
 10  \w     28.00  69.00   0.50    0.50    --   -3.67  57.00 -60.00   82
 11  \w     -2.00  45.00   0.50    0.50    --   -3.67  77.00 150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            44266
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.941
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Rigaku XtaLab P200'
_exptl_absorpt_coefficient_mu    3.448
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_preparation       'Recrystallization from cold hexane.'
_exptl_crystal_recrystallization_method 'Recrystallization from cold hexane.'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.867
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         6086
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0161P)^2^+9.2682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5867
_reflns_number_total             6086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05983b2.cif
_cod_data_source_block           lug3_abair_arnold
_cod_depositor_comments
'Adding full bibliography for 1573273--1573282.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1573274
_shelx_estimated_absorpt_t_max   0.531
_shelx_estimated_absorpt_t_min   0.405
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8927(5)
 0.1073(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C54(H54A,H54B), C5(H5A,H5B), C1(H1A,H1B), C10(H10A,H10B),
 C13(H13A,H13B), C16(H16A,H16B), C18(H18A,H18B), C17(H17A,H17B)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C2(H2A,H2B,H2C), C8(H8A,H8B,H8C),
 C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C14(H14A,H14B,H14C), C4(H4A,H4B,H4C),
 C15(H15A,H15B,H15C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              23837
_shelx_hkl_checksum              46264
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;