An (η3-Disilaallyl)lithium Derivative: Interconversion of π-Allyl-Type Bonding and η1Coordination to a Silyllithium Fragment
Tanaka, Hiroaki; Inoue, Shigeyoshi; Ichinohe, Masaaki; Sekiguchi, Akira; Organometallics 28 (2009) 6625–; doi:10.1021/om900861z

data_4070488
_publ_section_title
;
 An (\h3-Disilaallyl)lithium Derivative: Interconversion of \p-Allyl-Type
 Bonding and \h1Coordination to a Silyllithium Fragment
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6625
_journal_paper_doi               10.1021/om900861z
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C75 H135 Li O2 Si5'
_chemical_formula_weight         1216.22
_chemical_name_systematic
; 
 E-1-{(di-tert-butylmethylsilyloxy)-1-{2,2-di-tert-butyl-
 1-(di-tert-butylmethylsilyl)-2-methyl-1-[(tetrahydrofuran)lithio]disilanyl}- 
 2-[tris(3,5-di-tert-butylphenyl)methyl]silene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.4010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.1160(3)
_cell_length_b                   23.2540(3)
_cell_length_c                   17.1640(4)
_cell_measurement_reflns_used    84163
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.00
_cell_volume                     8014.8(2)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            84163
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.008
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Cube
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.371
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0076(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         19242
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1212P)^2^+5.6717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2035
_refine_ls_wR_factor_ref         0.2182
_reflns_number_gt                15515
_reflns_number_total             19242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900861z_si_001.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c        '
_cod_database_code               4070488