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_7708948
_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 H41 Li N4 Si'
_chemical_formula_sum            'C16 H41 Li N4 Si'
_chemical_formula_weight         324.56
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-05
_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                 94.108(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8910(3)
_cell_length_b                   18.7942(5)
_cell_length_c                   10.9483(3)
_cell_measurement_reflns_used    4359
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.4230
_cell_measurement_theta_min      4.6400
_cell_volume                     2235.22(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -85.00 -60.00   1.00   15.00    --  -42.11 126.00-177.00   25
  2  \w     86.00 125.00   1.00   60.00    --   92.50  48.00 -46.00   39
  3  \w     55.00  81.00   1.00   60.00    --   92.50-144.00 -62.00   26
  4  \w     37.00  64.00   1.00   60.00    --   92.50-126.00 106.00   27
  5  \w     44.00  71.00   1.00   60.00    --   92.50 -72.00 -13.00   27
  6  \w    -67.00  13.00   1.00   15.00    --  -42.11  77.00   0.00   80
  7  \w      2.00  63.00   1.00   15.00    --   42.11-125.00 -30.00   61
  8  \w     20.00  87.00   1.00   60.00    --   92.50-125.00-180.00   67
  9  \w     64.00 156.00   1.00   60.00    --   92.50  61.00  60.00   92
 10  \w     27.00 116.00   1.00   60.00    --   92.50 -45.00 120.00   89
 11  \w    103.00 129.00   1.00   60.00    --   92.50  30.00  30.00   26
 12  \w     33.00  71.00   1.00   60.00    --   92.50 -94.00  60.00   38
 13  \w    142.00 168.00   1.00   60.00    --   92.50  30.00  30.00   26
 14  \w     93.00 120.00   1.00   60.00    --   92.50  77.00  30.00   27
 15  \w     17.00  90.00   1.00   15.00    --   42.24  72.00 116.00   73
 16  \w     47.00  87.00   1.00   60.00    --   92.50-125.00 -30.00   40
 17  \w     28.00  78.00   1.00   60.00    --   92.50-125.00 120.00   50
 18  \w    118.00 164.00   1.00   60.00    --   92.50  61.00  30.00   46
 19  \w    111.00 137.00   1.00   60.00    --   92.50  77.00  90.00   26
 20  \w     11.00  37.00   1.00   60.00    --   92.50 -94.00  60.00   26
 21  \w     56.00  81.00   1.00   60.00    --   92.50 -94.00  60.00   25
 22  \w     30.00  74.00   1.00   60.00    --   92.50 -94.00-120.00   44
 23  \w     69.00  95.00   1.00   60.00    --   92.50  72.00 116.00   26
 24  \w    142.00 167.00   1.00   60.00    --   92.50  72.00 116.00   25
 25  \w     85.00 134.00   1.00   60.00    --   92.50  77.00 -30.00   49
 26  \w    118.00 144.00   1.00   60.00    --   92.50  45.00  90.00   26
 27  \w     74.00 122.00   1.00   60.00    --   92.50 -77.00  60.00   48
 28  \w     29.00  87.00   1.00   60.00    --   92.50-125.00  30.00   58
;
_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      -0.1134078000
_diffrn_orient_matrix_UB_12      -0.0411680000
_diffrn_orient_matrix_UB_13      -0.0545238000
_diffrn_orient_matrix_UB_21      0.0109885000
_diffrn_orient_matrix_UB_22      -0.0516688000
_diffrn_orient_matrix_UB_23      0.1095022000
_diffrn_orient_matrix_UB_31      -0.0843938000
_diffrn_orient_matrix_UB_32      0.0485067000
_diffrn_orient_matrix_UB_33      0.0703779000
_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  0.0870
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17538
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.623
_diffrn_reflns_theta_max         66.623
_diffrn_reflns_theta_min         4.683
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92216
_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    0.964
_exptl_crystal_description       irregular
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3923
_refine_ls_number_restraints     345
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0794P)^2^+0.4445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2893
_reflns_number_total             3923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03532k2.cif
_cod_data_source_block           elu210009_auto
_cod_database_code               7708948
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H41 Li1 N4 Si1'
_reflns_odcompleteness_completeness 98.62
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6A-C5 \\sim C6B-C5
 with sigma of 0.02
 N2-C2A \\sim N2-C2B
 with sigma of 0.02
 N3-C6B \\sim N3-C6A
 with sigma of 0.02
 C2A-C1 \\sim C2B-C1
 with sigma of 0.02
 N3-C7A \\sim N3-C7B \\sim N3-C8B \\sim N3-C8A
 with sigma of 0.02
 N2-C4A \\sim N2-C4B \\sim N2-C3A \\sim N2-C3B
 with sigma of 0.02
 C2B-C3B \\sim C2A-C3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2A \\sim C2B \\sim C3B \\sim C3A \\sim C4B \\sim C4A \\sim C6A \\sim C6B \\sim
C8A \\sim C8B \\sim C7A \\sim C7B: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
4. 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
5. Others
 Fixed Sof: H1AA(0.8072) H1AB(0.8072) H1BC(0.1928) H1BD(0.1928) H5AA(0.8072)
 H5AB(0.8072) H5BC(0.1928) H5BD(0.1928) C2A(0.8072) H2AA(0.8072) H2AB(0.8072)
 C3A(0.8072) H3AA(0.8072) H3AB(0.8072) H3AC(0.8072) C4A(0.8072) H4AA(0.8072)
 H4AB(0.8072) H4AC(0.8072) C6A(0.8072) H6AA(0.8072) H6AB(0.8072) C7A(0.8072)
 H7AA(0.8072) H7AB(0.8072) H7AC(0.8072) C8A(0.8072) H8AA(0.8072) H8AB(0.8072)
 H8AC(0.8072) C2B(0.1928) H2BA(0.1928) H2BB(0.1928) C3B(0.1928) H3BA(0.1928)
 H3BB(0.1928) H3BC(0.1928) C4B(0.1928) H4BA(0.1928) H4BB(0.1928) H4BC(0.1928)
 C6B(0.1928) H6BA(0.1928) H6BB(0.1928) C7B(0.1928) H7BA(0.1928) H7BB(0.1928)
 H7BC(0.1928) C8B(0.1928) H8BA(0.1928) H8BB(0.1928) H8BC(0.1928)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C5(H5AA,H5AB), C5(H5BC,H5BD), C9(H9A,H9B),
 C10(H10A,H10B), C13(H13A,H13B), C2A(H2AA,H2AB), C6A(H6AA,H6AB), C2B(H2BA,H2BB),
  C6B(H6BA,H6BB)
6.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C7A(H7AA,
 H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C3B(H3BA,H3BB,H3BC), C4B(H4BA,H4BB,H4BC),
 C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,H8BC)
;
_shelx_res_checksum              56215
_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 1.171
_oxdiff_exptl_absorpt_empirical_full_min 0.842