Addition of methyllithium to disilyne RSiSiR (R = SiiPr[CH(SiMe3)2]), giving a disilenyllithium, and its unexpected isomerization to a disilacyclopropylsilyllithium
Yamaguchi, Torahiko; Ichinohe, Masaaki; Sekiguchi, Akira; New Journal of Chemistry 34 (2010) 1544–; doi:10.1039/c0nj00027b

data_7053443
_publ_section_title
;
 Addition of methyllithium to disilyne RSi&#xE002;SiR (R =
 SiiPr[CH(SiMe3)2]), giving a disilenyllithium, and its unexpected
 isomerization to a disilacyclopropylsilyllithium
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1544
_journal_paper_doi               10.1039/c0nj00027b
_journal_volume                  34
_journal_year                    2010
_chemical_formula_sum            'C61 H127 Li O2 Si12'
_chemical_formula_weight         1236.65
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 100.564(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   53.017(2)
_cell_length_b                   14.9830(5)
_cell_length_c                   19.9430(9)
_cell_measurement_reflns_used    76584
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.18
_cell_volume                     15573.3(11)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.112
_diffrn_reflns_av_sigmaI/netI    0.1390
_diffrn_reflns_limit_h_max       69
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            76584
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.235
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             5440
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.00176(9)
_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   0.907
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         17550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1738
_reflns_number_gt                8949
_reflns_number_total             17550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00027b.txt
_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 1891 2012-01-12 08:04:46Z andrius 

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      'C 2/c '
_cod_database_code               7053443