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_1573281
_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 Si3 Y'
_chemical_formula_sum            'C18 H47 O3 Si3 Y'
_chemical_formula_weight         484.73
_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   geom
_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                 92.304(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1358(2)
_cell_length_b                   18.3119(3)
_cell_length_c                   13.4974(2)
_cell_measurement_reflns_used    32523
_cell_measurement_temperature    99.99(11)
_cell_measurement_theta_max      32.3080
_cell_measurement_theta_min      2.1660
_cell_volume                     2750.13(8)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(11)
_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 0.888
_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    -38.00  24.00   0.50   32.62    --    8.78 -57.00 120.00  124
  2  \w     -4.00  84.00   0.50   32.62    --    8.78  19.00-180.00  176
  3  \w    -67.00 -13.00   0.50   32.62    --    8.78 -19.00-180.00  108
  4  \w    -67.00 -13.00   0.50   32.62    --    8.78 -19.00  30.00  108
  5  \w    -14.00  16.00   0.50   32.62    --    8.78  77.00   0.00   60
  6  \w    -67.00 -13.00   0.50   32.62    --    8.78 -19.00-120.00  108
  7  \w     -6.00  38.00   0.50   32.62    --    8.78  57.00-120.00   88
  8  \w    -38.00   6.00   0.50   32.62    --   -9.17 -57.00 -90.00   88
  9  \w    -32.00  16.00   0.50   32.62    --   -9.17  77.00-150.00   96
 10  \w    -16.00  14.00   0.50   32.62    --   -9.17 -77.00-150.00   60
 11  \w    -38.00   6.00   0.50   32.62    --   -9.17 -57.00  30.00   88
 12  \w    -38.00   6.00   0.50   32.62    --   -9.17  90.00 -89.96   88
 13  \w    -38.00   6.00   0.50   32.62    --   -9.17 -57.00 -30.00   88
 14  \w     -4.00  82.00   0.50   32.62    --    8.78  37.00 -90.00  172
 15  \w    -16.00  32.00   0.50   32.62    --    8.78 -77.00  60.00   96
;
_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      -0.0099556000
_diffrn_orient_matrix_UB_12      -0.0053464000
_diffrn_orient_matrix_UB_13      -0.0517318000
_diffrn_orient_matrix_UB_21      -0.0074684000
_diffrn_orient_matrix_UB_22      -0.0379954000
_diffrn_orient_matrix_UB_23      0.0079958000
_diffrn_orient_matrix_UB_31      -0.0624955000
_diffrn_orient_matrix_UB_32      0.0053906000
_diffrn_orient_matrix_UB_33      0.0051283000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            74421
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.371
_diffrn_reflns_theta_min         1.875
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.264
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       prism
_exptl_crystal_F_000             1040
_exptl_crystal_preparation       'crystallization in freezer.'
_exptl_crystal_recrystallization_method hexane
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         8757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+0.9981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7768
_reflns_number_total             8757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05983b2.cif
_cod_data_source_block           pla23043_refinalized
_cod_depositor_comments
'Adding full bibliography for 1573273--1573282.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1573281
_chemical_oxdiff_formula         'Y Si3 O3 C18 H47'
_chemical_oxdiff_usercomment     'Diglyme solvate'
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.444
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C15(H15A,H15B), C1(H1A,H1B), C2(H2A,H2B), C17(H17A,H17B),
 C16(H16A,H16B), C14(H14A,H14B)
1.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C),
 C13(H13A,H13B,H13C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              35434
_shelx_hkl_checksum              32865
_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 1.398
_oxdiff_exptl_absorpt_empirical_full_min 0.823