Isolable Photoreactive Polysilyl Radicals
Gregory Molev; Boris Tumanskii; Dennis Sheberla; Mark Botoshansky; Dmitry Bravo-Zhivotovskii; Yitzhak Apeloig; Journal of the American Chemical Society 131 (2009) 11698–11700; doi:10.1021/ja905097b

data_4104912
_publ_section_title
;
 Isolable Photoreactive Polysilyl Radicals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11698
_journal_page_last               11700
_journal_paper_doi               10.1021/ja905097b
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C36 H85 Si6'
_chemical_formula_weight         686.58
_chemical_name_common            Dimitry-71
_chemical_name_systematic
; 
 ? 
;
_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                75.86(2)
_cell_angle_beta                 86.89(2)
_cell_angle_gamma                73.76(2)
_cell_formula_units_Z            2
_cell_length_a                   11.116(2)
_cell_length_b                   12.684(3)
_cell_length_c                   17.491(3)
_cell_measurement_reflns_used    18217
_cell_measurement_temperature    240(1)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      1.72
_cell_volume                     2295.7(8)
_computing_cell_refinement       'DENZO SMN (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 2001)'
_computing_data_reduction        'DENZO SMN (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'TEXSAN  (MSC, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      240(1)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1911
_diffrn_reflns_av_sigmaI/netI    0.3150
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18108
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.203
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.993
_exptl_crystal_description       plate
_exptl_crystal_F_000             770
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.525
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.026(5)
_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   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.3028
_refine_ls_R_factor_gt           0.1523
_refine_ls_shift/su_max          0.354
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1960P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3579
_refine_ls_wR_factor_ref         0.4056
_reflns_number_gt                2448
_reflns_number_total             7817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905097b_si_002.cif
_cod_data_source_block           dimitry71
_cod_database_code               4104912