Monomeric lithium and sodium silylbenzyl complexes: syntheses, structures, and CO bond olefination.
Barker, Jordan; Davison, Nathan; Waddell, Paul G.; Lu, Erli; Chemical communications (Cambridge, England) 59 (2023) 8083–8086; doi:10.1039/d3cc01376f

data_7131729
_publ_section_title
;
 Monomeric lithium and sodium silylbenzyl complexes: syntheses,
 structures, and C&#xe001;O bond olefination.
;
_journal_issue                   52
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8083
_journal_page_last               8086
_journal_paper_doi               10.1039/d3cc01376f
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C22 H45 Li N4 Si'
_chemical_formula_sum            'C22 H45 Li N4 Si'
_chemical_formula_weight         400.65
_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             2023-03-03
_audit_creation_method
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-03-20 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.668(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8325(3)
_cell_length_b                   15.3730(5)
_cell_length_c                   17.1794(5)
_cell_measurement_reflns_used    7735
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      76.8940
_cell_measurement_theta_min      3.8510
_cell_volume                     2591.43(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.921
_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    -30.00  -1.00   0.50    2.21    --   48.76 -41.00-128.00   58
  2  \w     49.00 125.00   0.50    2.21    --   48.76  41.00  23.00  152
  3  \w    -24.00  25.00   0.50    2.21    --  -49.76  41.00  23.00   98
  4  \w    -81.00 -50.00   0.50    2.21    --  -49.76 -41.00-128.00   62
  5  \w   -131.00 -79.00   0.50    2.21    --  -92.01 -41.00-128.00  104
  6  \w    -38.00 -13.00   0.50    2.21    --  -92.01  41.00  23.00   50
  7  \w   -169.00-137.00   0.50    2.21    --  -92.01 -41.00-128.00   64
  8  \w    103.00 128.00   0.50    2.21    --   96.11  41.00  23.00   50
  9  \w     19.00  46.00   0.50    2.21    --   96.11 -41.00-128.00   54
 10  \w    -30.00  26.00   0.50    2.21    --   48.76 -19.00  60.00  112
 11  \w    -47.00 -14.00   0.50    2.21    --  -92.01  45.00-180.00   66
 12  \w   -105.00 -38.00   0.50    2.21    --  -92.01  77.00   0.00  134
 13  \w    -42.00 -16.00   0.50    2.21    --  -92.01  45.00 150.00   52
 14  \w    -48.00 -17.00   0.50    2.21    --  -92.01  45.00-120.00   62
 15  \w    -44.00 -14.00   0.50    2.21    --  -92.01  45.00-150.00   60
 16  \w    -50.00 -15.00   0.50    2.21    --  -92.01  45.00 120.00   70
 17  \w     25.00  57.00   0.50    2.21    --   96.11 -61.00 150.00   64
 18  \w     18.00  43.00   0.50    2.21    --   96.11 -45.00 -90.00   50
 19  \w     37.00  68.00   0.50    2.21    --   96.11 -61.00  90.00   62
 20  \w     18.00  43.00   0.50    2.21    --   96.11 -45.00-180.00   50
 21  \w     18.00  43.00   0.50    2.21    --   96.11 -45.00 -60.00   50
 22  \w     38.00 105.00   0.50    2.21    --  108.00-125.00 120.00  134
 23  \w     41.00  67.00   0.50    2.21    --  108.00 -61.00 -30.00   52
 24  \w     42.00  87.00   0.50    2.21    --  108.00 -95.00 -90.00   90
 25  \w     71.00  96.00   0.50    2.21    --  108.00 -77.00  60.00   50
 26  \w    111.00 136.00   0.50    2.21    --  108.00  41.00  23.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0744795000
_diffrn_orient_matrix_UB_12      0.0321777000
_diffrn_orient_matrix_UB_13      -0.0708201000
_diffrn_orient_matrix_UB_21      0.1335194000
_diffrn_orient_matrix_UB_22      -0.0410288000
_diffrn_orient_matrix_UB_23      0.0346282000
_diffrn_orient_matrix_UB_31      -0.0359684000
_diffrn_orient_matrix_UB_32      -0.0854405000
_diffrn_orient_matrix_UB_33      -0.0432801000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17608
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.453
_diffrn_reflns_theta_min         3.862
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.00041(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0550P)^2^+0.7164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4337
_reflns_number_total             5136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01376f2.cif
_cod_data_source_block           elu230007_fa
_cod_depositor_comments
'Adding full bibliography for 7131729--7131730.cif.'
_cod_database_code               7131729
_chemical_oxdiff_formula         'C22 H45 Li1 N4 Si1'
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.858
_diffrn_oxdiff_digest_frames
;
013eac779ebb8cef311c23ecbd64b9fbd7019002b4b
;
_diffrn_oxdiff_digest_hkl
;
012a17e329026f08c289040b9743f9f3a64c36
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              88055
_shelx_hkl_checksum              46512
_shelx_shelxl_version_number     2019/1
_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 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.643