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_1573273
_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 O4 Si3 Y'
_chemical_formula_sum            'C20 H51 O4 Si3 Y'
_chemical_formula_weight         528.78
_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
_atom_sites_solution_primary     iterative
_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                 112.542(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9283(3)
_cell_length_b                   32.1189(7)
_cell_length_c                   10.3633(3)
_cell_measurement_reflns_used    11705
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      79.8160
_cell_measurement_theta_min      4.7980
_cell_volume                     3052.23(17)
_computing_cell_refinement       'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.98a 64-bit (release 24-11-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.98a (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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.970
_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     74.00 101.00   0.50    1.00    --  131.00-111.00-150.00   54
  2  \w     53.00 101.00   0.50    1.00    --  131.00-111.00 -90.00   96
  3  \w    -15.00  14.00   0.50    0.50    --   31.09  77.00 -30.00   58
  4  \w    -14.00  11.00   0.50    0.50    --   31.09  77.00 -60.00   50
  5  \w    -17.00  15.00   0.50    0.50    --   31.09  77.00 -90.00   64
  6  \w     42.00  68.00   0.50    1.00    --  131.00-111.00-150.00   52
  7  \w     43.00  75.00   0.50    1.00    --  131.00-111.00 -60.00   64
  8  \w    140.00 173.00   0.50    1.00    --  131.00 -63.00   0.00   66
  9  \w    142.00 173.00   0.50    1.00    --  131.00 -63.00  60.00   62
 10  \w    140.00 171.00   0.50    1.00    --  131.00 -63.00  90.00   62
 11  \w    141.00 172.00   0.50    1.00    --  131.00 -63.00 -90.00   62
 12  \w    140.00 166.00   0.50    1.00    --  131.00 -63.00-120.00   52
 13  \w    140.00 173.00   0.50    1.00    --  131.00 -63.00-180.00   66
 14  \w      2.00  69.00   0.50    1.00    --   81.04 -61.00-120.00  134
 15  \w     -6.00  22.00   0.50    1.00    --   81.04 -30.00-180.00   56
 16  \w     -5.00  22.00   0.50    1.00    --   81.04 -31.00 -13.00   54
 17  \w     25.00 154.00   0.50    1.00    --   81.04  31.00 145.00  258
 18  \w    110.00 173.00   0.50    1.00    --  131.00  77.00  60.00  126
 19  \w    128.00 177.00   0.50    1.00    --  131.00  31.00 145.00   98
 20  \w     86.00 113.00   0.50    1.00    --  131.00  31.00 145.00   54
 21  \w     52.00  81.00   0.50    1.00    --  131.00  31.00 145.00   58
 22  \w     25.00 154.00   0.50    1.00    --   81.04  31.00 145.00  258
 23  \w    104.00 178.00   0.50    1.00    --  131.00 111.00  60.00  148
 24  \w    115.00 146.00   0.50    1.00    --  131.00 111.00  90.00   62
 25  \w    104.00 178.00   0.50    1.00    --  131.00 111.00  30.00  148
 26  \w    151.00 176.00   0.50    1.00    --  131.00 111.00 -30.00   50
 27  \w    107.00 144.00   0.50    1.00    --  131.00 111.00 -30.00   74
 28  \w    103.00 145.00   0.50    1.00    --  131.00 111.00   0.00   84
 29  \w    152.00 178.00   0.50    1.00    --  131.00 111.00  90.00   52
 30  \w    -31.00  -6.00   0.50    1.00    --  -81.04  30.00 120.00   50
 31  \w     -5.00  36.00   0.50    0.50    --  -31.09  31.00 145.00   82
 32  \w    -47.00  -5.00   0.50    1.00    --  -81.04  45.00   0.00   84
 33  \w    -31.00  -3.00   0.50    1.00    --  -81.04  30.00  30.00   56
 34  \w    -32.00  -3.00   0.50    1.00    --  -81.04  30.00 -30.00   58
 35  \w    -32.00   1.00   0.50    1.00    --  -81.04  30.00 -60.00   66
 36  \w    -27.00   1.00   0.50    1.00    --  -81.04  30.00 -90.00   56
 37  \w    -58.00 -23.00   0.50    1.00    -- -106.00  50.00-120.00   70
 38  \w    -58.00 -32.00   0.50    1.00    -- -106.00  50.00-180.00   52
 39  \w    -61.00 -35.00   0.50    1.00    -- -106.00 111.00-150.00   52
 40  \w   -123.00  25.00   0.50    0.50    --  -31.09 -31.00 -13.00  296
 41  \w   -129.00-102.00   0.50    1.00    --  -81.04-111.00  90.00   54
 42  \w   -170.00-136.00   0.50    1.00    --  -81.04-111.00  90.00   68
 43  \w   -124.00 -99.00   0.50    1.00    -- -106.00 -31.00 -13.00   50
 44  \w    -14.00  17.00   0.50    0.50    --  -31.09 -77.00-120.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1179987000
_diffrn_orient_matrix_UB_12      -0.0078745000
_diffrn_orient_matrix_UB_13      -0.1462988000
_diffrn_orient_matrix_UB_21      -0.1022800000
_diffrn_orient_matrix_UB_22      -0.0176186000
_diffrn_orient_matrix_UB_23      0.0669791000
_diffrn_orient_matrix_UB_31      -0.0621180000
_diffrn_orient_matrix_UB_32      0.0439120000
_diffrn_orient_matrix_UB_33      0.0006964000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18955
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.049
_diffrn_reflns_theta_min         2.751
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.98a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_preparation
'crystallization from cooled concentrated hexane solution.'
_exptl_crystal_recrystallization_method hexane
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0873P)^2^+0.9693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5459
_reflns_number_total             6475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05983b2.cif
_cod_data_source_block           pla23171_auto
_cod_depositor_comments
'Adding full bibliography for 1573273--1573282.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1573273
_chemical_oxdiff_formula         'Y C50 H50 Si3 Cl2 O8'
_chemical_oxdiff_usercomment     ELTA189
_shelx_estimated_absorpt_t_max   0.693
_shelx_estimated_absorpt_t_min   0.569
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              73840
_shelx_hkl_checksum              23977
_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 1.956
_oxdiff_exptl_absorpt_empirical_full_min 0.386