A Monomeric (Trimethylsilyl)methyl Lithium Complex: Synthesis, Structure, Decomposition and Preliminary Reactivity Studies New Talent: Europe themed issue of Dalton Transactions
Davison, Nathan; Waddell, Paul G.; Dixon, Casey; Wills, Corinne; Penfold, Thomas; Lu, Erli; Dalton Transactions  (2021) –; doi:10.1039/D1DT03532K

data_7708949
_publ_section_title
;
 A Monomeric (Trimethylsilyl)methyl Lithium Complex: Synthesis, Structure,
 Decomposition and Preliminary Reactivity Studies New Talent: Europe
 themed issue of Dalton Transactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03532K
_journal_year                    2021
_chemical_formula_moiety         'C68 H84 Li4 O4 Si4'
_chemical_formula_sum            'C68 H84 Li4 O4 Si4'
_chemical_formula_weight         1105.47
_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             2021-10-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-11-05 deposited with the CCDC.	2021-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.5910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7436(2)
_cell_length_b                   22.0133(3)
_cell_length_c                   23.1214(4)
_cell_measurement_reflns_used    15564
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.4260
_cell_measurement_theta_min      3.7770
_cell_volume                     6465.40(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.111a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.111a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.111a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -87.00 -62.00   1.00   25.00    --  -42.24 -44.00 -40.00   25
  2  \w    -43.00 -18.00   1.00   25.00    --  -42.24  44.00 110.00   25
  3  \w    -30.00  50.00   1.00   25.00    --   42.24 -44.00 -40.00   80
  4  \w     21.00 115.00   1.00   25.00    --   42.24  44.00 110.00   94
  5  \w     69.00 117.00   1.00  100.00    --   92.50 -44.00 -40.00   48
  6  \w    116.00 142.00   1.00  100.00    --   92.50  44.00 110.00   26
  7  \w    -91.00 -22.00   1.00   25.00    --  -42.24 125.00-150.00   69
  8  \w    125.00 151.00   1.00  100.00    --   92.50  30.00-150.00   26
  9  \w     74.00 100.00   1.00  100.00    --   92.50  45.00-120.00   26
 10  \w     88.00 121.00   1.00  100.00    --   92.50 -61.00 120.00   33
 11  \w     33.00  59.00   1.00  100.00    --   92.50-125.00  30.00   26
 12  \w     23.00  87.00   1.00  100.00    --   92.50 -86.00 -41.53   64
 13  \w     20.00  67.00   1.00  100.00    --   92.50 -61.00 120.00   47
 14  \w    124.00 150.00   1.00  100.00    --   92.50  45.00-120.00   26
 15  \w     42.00  88.00   1.00  100.00    --   92.50 -30.00 -90.00   46
 16  \w     11.00  77.00   1.00  100.00    --   92.50 -85.00 127.94   66
 17  \w    103.00 128.00   1.00  100.00    --   92.50 -85.00 127.94   25
 18  \w     68.00 118.00   1.00  100.00    --   92.50  44.00-140.95   50
 19  \w     64.00 122.00   1.00  100.00    --   92.50  30.00-150.00   58
 20  \w     91.00 116.00   1.00  100.00    --   92.50 -86.00 -41.53   25
 21  \w     69.00 169.00   1.00  100.00    --   92.50  30.00  90.00  100
 22  \w     67.00 114.00   1.00  100.00    --   92.50  43.00  11.42   47
 23  \w    128.00 166.00   1.00  100.00    --   92.50  43.00  11.42   38
 24  \w     94.00 120.00   1.00  100.00    --   92.50 125.00 -60.00   26
 25  \w    140.00 165.00   1.00  100.00    --   92.50 125.00 -60.00   25
 26  \w     77.00 152.00   1.00  100.00    --   92.50 125.00   0.00   75
 27  \w     74.00 100.00   1.00  100.00    --   92.50  45.00 120.00   26
 28  \w    121.00 158.00   1.00  100.00    --   92.50  45.00 120.00   37
 29  \w     25.00  52.00   1.00  100.00    --   92.50 -80.00-148.93   27
 30  \w     66.00  92.00   1.00  100.00    --   92.50 -80.00-148.93   26
 31  \w     28.00  87.00   1.00  100.00    --   92.50-125.00  60.00   59
 32  \w     30.00  61.00   1.00  100.00    --   92.50 -94.00 -90.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0735833000
_diffrn_orient_matrix_UB_12      0.0312637000
_diffrn_orient_matrix_UB_13      -0.0405691000
_diffrn_orient_matrix_UB_21      0.0704672000
_diffrn_orient_matrix_UB_22      0.0220750000
_diffrn_orient_matrix_UB_23      0.0531033000
_diffrn_orient_matrix_UB_31      0.0657571000
_diffrn_orient_matrix_UB_32      -0.0585993000
_diffrn_orient_matrix_UB_33      -0.0016484000
_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  0.0810
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            59102
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.634
_diffrn_reflns_theta_max         66.634
_diffrn_reflns_theta_min         3.836
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.193
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.111a (Rigaku Oxford Diffraction, 2021)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         11344
_refine_ls_number_restraints     784
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+2.8691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8856
_reflns_number_total             11344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03532k2.cif
_cod_data_source_block           elu210013_fa
_cod_database_code               7708949
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H21 Li1 O1 Si1'
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.779
_reflns_odcompleteness_completeness 98.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C31(H31A,H31B), C48(H48A,H48B), C65(H65A,H65B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C37(H37), C38(H38), C39(H39), C40(H40),
 C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C54(H54), C55(H55),
  C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C68(H68A,H68B,H68C)
;
_shelx_res_checksum              93115
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.134
_oxdiff_exptl_absorpt_empirical_full_min 0.866