Directed Lithiation of Pentadienylsilanes
Day, Benjamin M.; McDouall, Joseph J. W.; Clayden, Jonathan; Layfield, Richard A.; Organometallics 34 (2015) 2348–; doi:10.1021/om501144f

data_4085185
_publ_section_title
;
 Directed Lithiation of Pentadienylsilanes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2348
_journal_paper_doi               10.1021/om501144f
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C14 H28 Li N O2 Si'
_chemical_formula_sum            'C14 H28 Li N O2 Si'
_chemical_formula_weight         277.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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Olex2 1.2
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_cell_length_c                   14.0204(7)
_cell_measurement_reflns_used    3305
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_cell_volume                     874.42(7)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_diffrn_measured_fraction_theta_full 0.998
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;
  1 omega    1.00   68.00   1.0000    8.0750
omega____ theta____ kappa____ phi______ frames
    -       19.4509   57.0000   30.0000 67

  2 omega   -5.00   87.00   1.0000    8.0750
omega____ theta____ kappa____ phi______ frames
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  3 omega   -6.00   83.00   1.0000    8.0750
omega____ theta____ kappa____ phi______ frames
    -       19.4509   77.0000  -90.0000 89

  4 omega   19.00   88.00   1.0000    8.0750
omega____ theta____ kappa____ phi______ frames
    -       19.4509   57.0000 -180.0000 69

  5 omega   39.00   75.00   1.0000    8.0750
omega____ theta____ kappa____ phi______ frames
    -       19.4509 -122.0000  -89.0000 36

  6 omega  -36.00   50.00   1.0000    8.0750
omega____ theta____ kappa____ phi______ frames
    -       19.4509  -77.0000  120.0000 86

  7 omega  -49.00   19.00   1.0000    8.0750
omega____ theta____ kappa____ phi______ frames
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  8 omega  -46.00   33.00   1.0000    8.0750
omega____ theta____ kappa____ phi______ frames
    -       19.4509  -57.0000  -60.0000 79

  9 omega  -49.00   27.00   1.0000    8.0750
omega____ theta____ kappa____ phi______ frames
    -       19.4509  -57.0000 -150.0000 76

 10 omega  -73.00  -44.00   1.0000    8.0750
omega____ theta____ kappa____ phi______ frames
    -      -18.3571  122.0000   -8.0000 29
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_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
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_diffrn_orient_matrix_UB_33      -0.0051544000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_min       -9
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_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11481
_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.361
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.132
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_exptl_absorpt_correction_T_min  0.79049
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
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_exptl_crystal_size_min          0.05
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         3579
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+0.5823P] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501144f_si_002.cif
_cod_data_source_block           aral202
_cod_depositor_comments
'Adding full bibliography for 4085184--4085185.cif.'
_cod_database_code               4085185
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C14H28N1Li1N1O2Si1
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_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
2.c X=CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              27216
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_olex2_submission_special_instructions 'No special instructions were received'