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_7708950
_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         'C16 H40 Li2 N6'
_chemical_formula_sum            'C16 H40 Li2 N6'
_chemical_formula_weight         330.42
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-07 deposited with the CCDC.	2021-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.323(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6022(3)
_cell_length_b                   10.0920(2)
_cell_length_c                   14.6868(3)
_cell_measurement_reflns_used    7077
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.5020
_cell_measurement_theta_min      5.2890
_cell_volume                     2154.24(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     14.00 115.00   1.00    4.00    --   42.24  57.00 -30.00  101
  2  \w      1.00  87.00   1.00    4.00    --   42.24-125.00 120.00   86
  3  \w    -30.00  70.00   1.00    4.00    --   42.24 -57.00-180.00  100
  4  \w      9.00 129.00   1.00   16.00    --   92.50 -88.00 -39.85  120
  5  \w     76.00 166.00   1.00   16.00    --   92.50 125.00 -60.00   90
  6  \w     64.00 169.00   1.00   16.00    --   92.50  30.00 -90.00  105
  7  \w      9.00 129.00   1.00   16.00    --   92.50 -88.00 142.79  120
  8  \w     64.00 169.00   1.00   16.00    --   92.50  30.00 -30.00  105
  9  \w     20.00 122.00   1.00   16.00    --   92.50 -61.00-180.00  102
 10  \w     11.00 145.00   1.00   16.00    --   92.50 -15.00  90.00  134
 11  \w      9.00 129.00   1.00   16.00    --   92.50 -88.00 -24.76  120
 12  \w     20.00 122.00   1.00   16.00    --   92.50 -61.00 -30.00  102
 13  \w     11.00 128.00   1.00   16.00    --   92.50 -86.00-108.01  117
 14  \w     19.00  87.00   1.00   16.00    --   92.50-125.00 -60.00   68
 15  \w     68.00 103.00   1.00   16.00    --   92.50 -88.00  45.47   35
 16  \w     15.00  67.00   1.00   16.00    --   92.50 -94.00  90.00   52
 17  \w    121.00 169.00   1.00   16.00    --   92.50  77.00 150.00   48
 18  \w     28.00  85.00   1.00   16.00    --   92.50 -53.00  69.00   57
 19  \w     91.00 116.00   1.00   16.00    --   92.50 -87.00-171.93   25
 20  \w     30.00  87.00   1.00   16.00    --   92.50-125.00  90.00   57
 21  \w     87.00 116.00   1.00   16.00    --   92.50 -45.00-180.00   29
 22  \w     79.00 105.00   1.00   16.00    --   92.50 -30.00 -60.00   26
 23  \w     85.00 110.00   1.00   16.00    --   92.50  45.00-180.00   25
 24  \w    133.00 159.00   1.00   16.00    --   92.50  45.00-180.00   26
 25  \w     44.00  86.00   1.00   16.00    --   92.50-125.00-180.00   42
 26  \w     17.00  60.00   1.00   16.00    --   92.50 -94.00 -30.00   43
 27  \w    113.00 139.00   1.00   16.00    --   92.50  77.00  90.00   26
 28  \w     84.00 110.00   1.00   16.00    --   92.50 -77.00-180.00   26
 29  \w     22.00  48.00   1.00   16.00    --   92.50 -84.00 110.32   26
 30  \w     94.00 120.00   1.00   16.00    --   92.50 -84.00 110.32   26
;
_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      0.0105032000
_diffrn_orient_matrix_UB_12      -0.0699546000
_diffrn_orient_matrix_UB_13      0.0966941000
_diffrn_orient_matrix_UB_21      0.0555838500
_diffrn_orient_matrix_UB_22      -0.1114937500
_diffrn_orient_matrix_UB_23      -0.0244475000
_diffrn_orient_matrix_UB_31      0.0896307000
_diffrn_orient_matrix_UB_32      0.0773848000
_diffrn_orient_matrix_UB_33      0.0522112000
_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  0.0459
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14540
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.614
_diffrn_reflns_theta_max         66.614
_diffrn_reflns_theta_min         5.336
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.111a (Rigaku Oxford Diffraction, 2021)
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    1.019
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.140
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0599P)^2^+0.9847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1700
_reflns_number_total             1902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03532k2.cif
_cod_data_source_block           elu210016
_cod_database_code               7708950
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C8 H20 Li1 N3'
_reflns_odcompleteness_completeness 98.63
_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), C3(H3A,H3B), C4(H4A,H4B)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              2416
_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 1.148
_oxdiff_exptl_absorpt_empirical_full_min 0.872