Structural Influences in Lithium Pentadienylsilane Complexes
Day, Benjamin M.; Clayden, Jonathan; Layfield, Richard A.; Organometallics 32 (2013) 4448–; doi:10.1021/om400596y

data_4081183
_publ_section_title
;
 Structural Influences in Lithium Pentadienylsilane Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4448
_journal_paper_doi               10.1021/om400596y
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C22 H52 Li N5 Si2'
_chemical_formula_sum            'C22 H52 Li N5 Si2'
_chemical_formula_weight         449.80
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-06-17
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                100.332(3)
_cell_angle_beta                 101.726(2)
_cell_angle_gamma                94.214(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0142(3)
_cell_length_b                   12.4095(4)
_cell_length_c                   15.2613(4)
_cell_measurement_reflns_used    8750
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.0780
_cell_measurement_theta_min      3.0000
_cell_volume                     1452.45(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9738
_diffrn_measured_fraction_theta_max 0.9386
_diffrn_measurement_details
;
  1 omega   88.70  267.70   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   73.8686  -15.7900 179

  2 omega   91.88  227.88   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   73.8686 -175.7905 136

  3 omega   85.19  258.19   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   73.8686  -65.7906 173

  4 phi    -12.95  245.25   1.0008    5.0000
omega____ theta____ kappa____ phi______ frames
-130.7909  111.0000   73.8686     -     258

  5 omega  -83.31   58.69   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000   73.8686  -25.7908 142

  6 phi    153.17  331.31   1.0008    5.0000
omega____ theta____ kappa____ phi______ frames
 143.2791   90.0000   73.8686     -     178

  7 omega   94.21  268.21   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   73.8686   24.2094 174

  8 omega  -73.74   42.26   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -65.0000   73.8686 -140.7912 116

  9 phi     19.27  164.40   1.0009    5.0000
omega____ theta____ kappa____ phi______ frames
 154.2091  110.0000   73.8686     -     145

 10 omega  -53.54   50.46   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.0000   73.8686   54.2081 104

 11 phi     28.35  152.45   1.0008    5.0000
omega____ theta____ kappa____ phi______ frames
 124.9791  100.5000   73.8686     -     124

 12 phi    212.72  332.83   1.0009    5.0000
omega____ theta____ kappa____ phi______ frames
 174.2091  112.0000   73.8686     -     120

 13 omega  128.31  227.31   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   73.8686  114.2094 99

 14 omega   95.39  174.39   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.8686   74.2097 79

 15 omega  166.21  268.21   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.8686 -125.7919 102

 16 omega  -28.45   42.55   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.0000   73.8686  -85.7905 71

 17 omega  -75.77   25.23   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -50.0000   73.8686  174.2088 101

 18 omega  146.28  221.27   0.9998    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   73.8686  149.2084 75

 19 omega   79.21  153.21   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   73.8686   89.2091 74

 20 phi    -25.79   48.26   1.0006    5.0000
omega____ theta____ kappa____ phi______ frames
 -60.9809  -60.0000   73.8686     -     74
;
_diffrn_measurement_device_type  'Bruker SMART APEX 2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      0.0524009000
_diffrn_orient_matrix_UB_12      0.0335247000
_diffrn_orient_matrix_UB_13      0.1048733000
_diffrn_orient_matrix_UB_21      -0.0928112000
_diffrn_orient_matrix_UB_22      0.1040469000
_diffrn_orient_matrix_UB_23      -0.0035938000
_diffrn_orient_matrix_UB_31      -0.1664105000
_diffrn_orient_matrix_UB_32      -0.0646865000
_diffrn_orient_matrix_UB_33      0.0074714000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15097
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         5.675
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.215
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.02186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_description       needle
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0930P)^2^+0.5499P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4364
_reflns_number_total             5183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400596y_si_002.cif
_cod_data_source_block           xral6
_cod_original_cell_volume        1452.46(8)
_cod_database_code               4081183
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 97.38
_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:
 C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C)
;
_shelx_hkl_checksum              641
_shelx_res_checksum              89773
_shelxl_version_number           2013-2