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_7708951
_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         'C20 H52 Li2 N6 O2 Si2'
_chemical_formula_sum            'C20 H52 Li2 N6 O2 Si2'
_chemical_formula_weight         478.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-10-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-10-28 deposited with the CCDC.	2021-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.353(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9028(5)
_cell_length_b                   8.8805(3)
_cell_length_c                   19.9387(7)
_cell_measurement_reflns_used    5113
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.4170
_cell_measurement_theta_min      4.6510
_cell_volume                     2840.67(17)
_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)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  70.00   1.00    1.00    --   42.11 -55.00  62.00  100
  2  \w     20.00 120.00   1.00    4.00    --   92.50 -55.00  62.00  100
  3  \w     65.00 165.00   1.00    4.00    --   92.50  55.00-154.00  100
  4  \w    -98.00 -22.00   1.00    1.00    --  -42.11 125.00-180.00   76
  5  \w     14.00 114.00   1.00    1.00    --   42.11  55.00-154.00  100
  6  \w     64.00 169.00   1.00    4.00    --   92.50  30.00 150.00  105
  7  \w     68.00 167.00   1.00    4.00    --   92.50  30.00 -30.00   99
  8  \w    116.00 160.00   1.00    4.00    --   92.50  45.00-180.00   44
  9  \w     78.00 168.00   1.00    4.00    --   92.50  30.00  90.00   90
 10  \w    139.00 165.00   1.00    4.00    --   92.50  77.00 150.00   26
 11  \w    103.00 165.00   1.00    4.00    --   92.50 125.00  90.00   62
 12  \w     15.00  58.00   1.00    4.00    --   92.50 -90.00 -80.29   43
 13  \w     33.00  59.00   1.00    4.00    --   92.50 -86.00 146.94   26
 14  \w     69.00 128.00   1.00    4.00    --   92.50 -86.00 146.94   59
 15  \w     19.00  45.00   1.00    4.00    --   92.50-125.00 -90.00   26
 16  \w     80.00 114.00   1.00    4.00    --   92.50  77.00 150.00   34
 17  \w     46.00  71.00   1.00    4.00    --   92.50-125.00   0.00   25
 18  \w     36.00  75.00   1.00    4.00    --   92.50-125.00 -30.00   39
;
_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      0.0851873000
_diffrn_orient_matrix_UB_12      -0.0799156000
_diffrn_orient_matrix_UB_13      0.0243112000
_diffrn_orient_matrix_UB_21      0.0218634000
_diffrn_orient_matrix_UB_22      0.0824436000
_diffrn_orient_matrix_UB_23      0.0715072000
_diffrn_orient_matrix_UB_31      -0.0385780000
_diffrn_orient_matrix_UB_32      -0.1300055000
_diffrn_orient_matrix_UB_33      0.0303880000
_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  0.0751
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10127
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.661
_diffrn_reflns_theta_max         66.661
_diffrn_reflns_theta_min         4.673
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.328
_exptl_absorpt_correction_T_max  0.77678
_exptl_absorpt_correction_T_min  0.76538
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.111a (Rigaku Oxford Diffraction, 2021)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    1.119
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_crystal_size_rad          0.132
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0746P)^2^+0.6536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2120
_reflns_number_total             2503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03532k2.cif
_cod_data_source_block           elu210008
_cod_original_cell_volume        2840.66(17)
_cod_database_code               7708951
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H20 Si1 O1 Li1 N3'
_reflns_odcompleteness_completeness 98.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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), C5(H5A,H5B), C6(H6A,H6B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              50261
_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 1.233
_oxdiff_exptl_absorpt_empirical_full_min 0.820