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_1573278
_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         'C18 H47 O3 Sc Si3'
_chemical_formula_sum            'C18 H47 O3 Sc Si3'
_chemical_formula_weight         440.78
_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     dual
_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                 101.9560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.48680(10)
_cell_length_b                   15.77720(10)
_cell_length_c                   18.69720(10)
_cell_measurement_reflns_used    39959
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      79.6700
_cell_measurement_theta_min      3.6600
_cell_volume                     2737.80(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.107a 64-bit (release 07-02-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_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     54.00  91.00   0.50    0.33    --  113.25-125.00  90.00   74
  2  \w      3.00  79.00   0.50    0.08    --   47.94 -99.00  60.00  152
  3  \w     67.00  92.00   0.50    0.08    --   47.94-125.00  30.00   50
  4  \w     69.00  94.00   0.50    0.08    --   47.94-125.00   0.00   50
  5  \w     56.00  82.00   0.50    0.33    --  113.25-125.00 -90.00   52
  6  \w     65.00 111.00   0.50    0.33    --  113.25-125.00-150.00   92
  7  \w     58.00  84.00   0.50    0.33    --  113.25-125.00 -60.00   52
  8  \w     44.00  69.00   0.50    0.33    --  113.25-125.00 -30.00   50
  9  \w     63.00  89.00   0.50    0.33    --  113.25-125.00   0.00   52
 10  \w     51.00  77.00   0.50    0.33    --  113.25-125.00  60.00   52
 11  \w     44.00 110.00   0.50    0.33    --  113.25-125.00  30.00  132
 12  \w     63.00 104.00   0.50    0.33    --  113.25 -94.00  90.00   82
 13  \w     57.00 106.00   0.50    0.33    --  113.25 -98.00 -37.97   98
 14  \w     81.00 107.00   0.50    0.33    --  113.25-125.00-120.00   52
 15  \w     72.00  99.00   0.50    0.33    --  113.25-125.00-180.00   54
 16  \w     69.00 105.00   0.50    0.33    --  113.25 -94.00-180.00   72
 17  \w     75.00 106.00   0.50    0.33    --  113.25 -94.00-150.00   62
 18  \w     51.00  82.00   0.50    0.33    --  113.25 -94.00 -60.00   62
 19  \w     43.00  69.00   0.50    0.33    --  113.25 -94.00   0.00   52
 20  \w     76.00 106.00   0.50    0.33    --  113.25 -94.00-120.00   60
 21  \w     73.00 106.00   0.50    0.33    --  113.25 -94.00   0.00   66
 22  \w     52.00  77.00   0.50    0.33    --  113.25 -94.00  30.00   50
 23  \w     72.00  99.00   0.50    0.33    --  113.25 -94.00 150.00   54
 24  \w     52.00 106.00   0.50    0.33    --  113.25 -94.00 120.00  108
 25  \w    104.00 130.00   0.50    0.33    --  113.25 -88.00  27.42   52
 26  \w    100.00 141.00   0.50    0.33    --  113.25 -87.00  -9.17   82
 27  \w     44.00  70.00   0.50    0.33    --  113.25 -88.00-171.89   52
 28  \w     42.00  71.00   0.50    0.33    --  113.25 -82.00-165.79   58
 29  \w     45.00  71.00   0.50    0.33    --  113.25 -94.00-120.00   52
 30  \w     68.00  94.00   0.50    0.33    --  113.25 -87.00-141.04   52
 31  \w    102.00 130.00   0.50    0.33    --  113.25 -87.00-141.04   56
 32  \w    108.00 137.00   0.50    0.33    --  113.25 -88.00-171.89   58
 33  \w     83.00 109.00   0.50    0.33    --  113.25 -82.00-165.79   52
 34  \w    -25.00   2.00   0.50    0.08    --   47.94 -19.00-180.00   54
 35  \w    109.00 135.00   0.50    0.33    --  113.25 -77.00-120.00   52
 36  \w     64.00 114.00   0.50    0.33    --  113.25 -77.00   0.00  100
 37  \w     96.00 137.00   0.50    0.33    --  113.25 -79.00 146.74   82
 38  \w     43.00  69.00   0.50    0.33    --  113.25 -79.00 146.74   52
 39  \w     60.00 109.00   0.50    0.33    --  113.25 -79.00 121.58   98
 40  \w     94.00 134.00   0.50    0.33    --  113.25 -77.00 -30.90   80
 41  \w     47.00  77.00   0.50    0.33    --  113.25 -77.00 -90.00   60
 42  \w     46.00  72.00   0.50    0.33    --  113.25 -77.00-150.00   52
 43  \w     42.00  67.00   0.50    0.33    --  113.25 -61.00-120.00   50
 44  \w     49.00  78.00   0.50    0.33    --  113.25 -77.00-120.00   58
 45  \w     60.00  86.00   0.50    0.33    --  113.25 -77.00 -30.90   52
 46  \w     42.00  67.00   0.50    0.33    --  113.25 -61.00   0.00   50
 47  \w     44.00  71.00   0.50    0.33    --  113.25 -61.00 120.00   54
 48  \w     42.00  68.00   0.50    0.33    --  113.25 -61.00 150.00   52
 49  \w     45.00  70.00   0.50    0.33    --  113.25 -61.00  90.00   50
 50  \w     42.00  67.00   0.50    0.33    --  113.25 -61.00  60.00   50
 51  \w     45.00  70.00   0.50    0.33    --  113.25 -61.00 -60.00   50
 52  \w    148.00 174.00   0.50    0.33    --  113.25 125.00-150.00   52
 53  \w    139.00 165.00   0.50    0.33    --  113.25 125.00-180.00   52
 54  \w     97.00 133.00   0.50    0.33    --  113.25 125.00-150.00   72
 55  \w     95.00 120.00   0.50    0.33    --  113.25 125.00-120.00   50
 56  \w    110.00 139.00   0.50    0.33    --  113.25 125.00   0.00   58
 57  \w    118.00 162.00   0.50    0.33    --  113.25 125.00 120.00   88
 58  \w    136.00 166.00   0.50    0.33    --  113.25  15.00  30.00   60
 59  \w    122.00 148.00   0.50    0.33    --  113.25  77.00  90.00   52
 60  \w    120.00 161.00   0.50    0.33    --  113.25  77.00 120.00   82
 61  \w    111.00 148.00   0.50    0.33    --  113.25  77.00 150.00   74
 62  \w    108.00 177.00   0.50    0.33    --  113.25  61.00  90.00  138
 63  \w    106.00 152.00   0.50    0.33    --  113.25  61.00 120.00   92
 64  \w    107.00 154.00   0.50    0.33    --  113.25  61.00  60.00   94
 65  \w    111.00 146.00   0.50    0.33    --  113.25  61.00 150.00   70
 66  \w    115.00 141.00   0.50    0.33    --  113.25  61.00   0.00   52
 67  \w    150.00 177.00   0.50    0.33    --  113.25  61.00   0.00   54
 68  \w    135.00 178.00   0.50    0.33    --  113.25  77.00 -30.00   86
 69  \w    107.00 137.00   0.50    0.33    --  113.25  61.00  30.00   60
 70  \w    107.00 141.00   0.50    0.33    --  113.25  61.00 -60.00   68
 71  \w    108.00 162.00   0.50    0.33    --  113.25  61.00-120.00  108
 72  \w    115.00 159.00   0.50    0.33    --  113.25  77.00-180.00   88
 73  \w    139.00 170.00   0.50    0.33    --  113.25  61.00-150.00   62
 74  \w    110.00 143.00   0.50    0.33    --  113.25  45.00 -90.00   66
 75  \w    150.00 176.00   0.50    0.33    --  113.25  45.00 -90.00   52
 76  \w    136.00 167.00   0.50    0.33    --  113.25  45.00  30.00   62
 77  \w    115.00 157.00   0.50    0.33    --  113.25  30.00 -60.00   84
 78  \w    105.00 156.00   0.50    0.33    --  113.25  30.00  60.00  102
 79  \w    106.00 151.00   0.50    0.33    --  113.25  45.00  90.00   90
 80  \w    131.00 157.00   0.50    0.33    --  113.25  45.00 120.00   52
 81  \w    122.00 170.00   0.50    0.33    --  113.25  15.00  60.00   96
 82  \w    110.00 136.00   0.50    0.33    --  113.25  30.00-120.00   52
 83  \w    115.00 142.00   0.50    0.33    --  113.25  30.00 -30.00   54
 84  \w    118.00 144.00   0.50    0.33    --  113.25  30.00  30.00   52
 85  \w     38.00 116.00   0.50    0.08    --   47.94  47.00 153.73  156
 86  \w    -59.00  21.00   0.50    0.08    --  -47.94  57.00 -60.00  160
 87  \w    -53.00 -20.00   0.50    0.33    --  -91.75  45.00-150.00   66
 88  \w    -16.00  28.00   0.50    0.08    --  -47.94  19.00-120.00   88
 89  \w      1.00  28.00   0.50    0.08    --  -47.94  19.00 -60.00   54
 90  \w    -14.00  19.00   0.50    0.08    --  -47.94  19.00  90.00   66
 91  \w   -120.00 -36.00   0.50    0.08    --  -47.94 -45.00 155.76  168
 92  \w   -162.00-133.00   0.50    0.33    --  -91.75 -77.00  90.00   58
;
_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      -0.0407594000
_diffrn_orient_matrix_UB_12      0.0439128000
_diffrn_orient_matrix_UB_13      -0.0750762000
_diffrn_orient_matrix_UB_21      -0.0477926000
_diffrn_orient_matrix_UB_22      0.0792961000
_diffrn_orient_matrix_UB_23      0.0367877000
_diffrn_orient_matrix_UB_31      0.1535274000
_diffrn_orient_matrix_UB_32      0.0364098000
_diffrn_orient_matrix_UB_33      0.0103806000
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61454
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.043
_diffrn_reflns_theta_min         3.700
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.648
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.467
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.107a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale colourless'
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_description       prism
_exptl_crystal_F_000             968
_exptl_crystal_recrystallization_method hexane
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0495P)^2^+0.6268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5703
_reflns_number_total             5972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05983b2.cif
_cod_data_source_block           pla24006_refinalized
_cod_depositor_comments
'Adding full bibliography for 1573273--1573282.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1573278
_chemical_oxdiff_formula         'Sc Si3 C50 O3 H30'
_chemical_oxdiff_usercomment     ELTA-224
_shelx_estimated_absorpt_t_max   0.735
_shelx_estimated_absorpt_t_min   0.529
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C3(H3A,H3B), C16(H16A,H16B), C15(H15A,H15B), C14(H14A,H14B)
1.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C7(H7A,
 H7B,H7C), C18(H18A,H18B,H18C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              32794
_shelx_hkl_checksum              68598
_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 1.586
_oxdiff_exptl_absorpt_empirical_full_min 0.728