Unsymmetrically Substituted Disilyne Dsi2iPrSi-Si\τbSi-SiNpDsi2 (Np = CH2tBu): Synthesis and Characterization
Yoshitaka Murata; Masaaki Ichinohe; Akira Sekiguchi; Journal of the American Chemical Society 132 (2010) 16768–16770; doi:10.1021/ja1091744

data_4103591
_publ_section_title
;
 Unsymmetrically Substituted Disilyne Dsi2iPrSi-Si\\tbSi-SiNpDsi2 (Np =
 CH2tBu): Synthesis and Characterization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16768
_journal_page_last               16770
_journal_paper_doi               10.1021/ja1091744
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C36 H94 Si12'
_chemical_formula_weight         864.19
_chemical_name_systematic
; 
 1,1,4,4-Tetrakis[bis(trimethylsilyl)methyl]- 
 1-(2,2-dimethylpropyl)-4-isopropyl-2-tetrasilyne 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.255(2)
_cell_angle_beta                 104.710(2)
_cell_angle_gamma                109.116(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9153(18)
_cell_length_b                   16.404(3)
_cell_length_c                   18.292(3)
_cell_measurement_reflns_used    8952
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.21
_cell_volume                     2770.0(8)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30275
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_correction_T_min  0.9663
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         12267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+0.4736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                7982
_reflns_number_total             12267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1091744_si_002.cif
_cod_data_source_block           Dsi2iPrSiSiSiSiNpDsi2
_cod_depositor_comments
;
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_cell_volume        2770.1(8)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4103591