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_7131730
_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 N4 Na Si'
_chemical_formula_sum            'C22 H45 N4 Na Si'
_chemical_formula_weight         416.70
_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     dual
_audit_creation_date             2023-03-13
_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                 102.389(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   9.6060(4)
_cell_length_c                   20.0799(8)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      78.2940
_cell_measurement_theta_min      3.1950
_cell_volume                     2654.14(19)
_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 0.919
_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     56.00  81.00   0.50    5.04    --   49.01  40.00 -75.00   50
  2  \w    -30.00  10.00   0.50    5.04    --   49.01 -40.00 130.00   80
  3  \w   -123.00 -48.00   0.50    5.04    --  -49.76 -40.00 130.00  150
  4  \w    -22.00  29.00   0.50    5.04    --  -49.76  40.00 -75.00  102
  5  \w   -168.00 -75.00   0.50    5.04    --  -92.01 -40.00 130.00  186
  6  \w    -45.00 -14.00   0.50    5.04    --  -92.01  40.00 -75.00   62
  7  \w    103.00 128.00   0.50    5.04    --   96.11  40.00 -75.00   50
  8  \w     18.00  43.00   0.50    5.04    --   96.11 -40.00 130.00   50
  9  \w    135.00 160.00   0.50    5.04    --  108.00  40.00 -75.00   50
 10  \w    -30.00  21.00   0.50    5.04    --   49.01 -19.00 -30.00  102
 11  \w   -128.00 -68.00   0.50    5.04    --  -92.01 -77.00  30.00  120
 12  \w    -51.00 -21.00   0.50    5.04    --  -92.01  45.00  30.00   60
 13  \w    -51.00 -16.00   0.50    5.04    --  -92.01  45.00  90.00   70
 14  \w    -47.00 -16.00   0.50    5.04    --  -92.01  45.00-120.00   62
 15  \w    -46.00 -14.00   0.50    5.04    --  -92.01  45.00 120.00   64
 16  \w     58.00 105.00   0.50    5.04    --   96.11 -77.00 -60.00   94
 17  \w     28.00  54.00   0.50    5.04    --   96.11 -77.00 -60.00   52
 18  \w     24.00  49.00   0.50    5.04    --   96.11 -45.00 150.00   50
 19  \w     22.00  50.00   0.50    5.04    --   96.11 -45.00-180.00   56
 20  \w     79.00 132.00   0.50    5.04    --   96.11 125.00-180.00  106
 21  \w     25.00  50.00   0.50    5.04    --   96.11 -45.00 -60.00   50
 22  \w     40.00  71.00   0.50    5.04    --  108.00 -61.00 120.00   62
 23  \w     34.00  67.00   0.50    5.04    --  108.00 -61.00 -30.00   66
 24  \w     48.00  96.00   0.50    5.04    --  108.00 -95.00-150.00   96
;
_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      0.0659158000
_diffrn_orient_matrix_UB_12      -0.0709509000
_diffrn_orient_matrix_UB_13      -0.0420078000
_diffrn_orient_matrix_UB_21      0.0736190000
_diffrn_orient_matrix_UB_22      -0.0357049000
_diffrn_orient_matrix_UB_23      0.0663019000
_diffrn_orient_matrix_UB_31      -0.0525700000
_diffrn_orient_matrix_UB_32      -0.1392614000
_diffrn_orient_matrix_UB_33      0.0043527000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18205
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.352
_diffrn_reflns_theta_min         3.212
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_description       irregular
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.00049(11)
_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   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0506P)^2^+0.8497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4605
_reflns_number_total             5237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01376f2.cif
_cod_data_source_block           elu230010
_cod_depositor_comments
'Adding full bibliography for 7131729--7131730.cif.'
_cod_database_code               7131730
_chemical_oxdiff_formula         'C22 H45 Na1 N4 Si1'
_diffrn_oxdiff_digest_frames
;
01a1f7000f6cc42f0641a2d8f29b338dbf01890695d
;
_diffrn_oxdiff_digest_hkl
;
015ec2c21a9756debc92e8f435cd03a77b7298
;
_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:
 C14(H14), 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              9876
_shelx_hkl_checksum              794
_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 1.400
_oxdiff_exptl_absorpt_empirical_full_min 0.577