Synthesis of a 1-Hydrosilene Stable in Solution and Its Unique Properties#
Ozaki, Shuhei; Sasamori, Takahiro; Tokitoh, Norihiro; Organometallics 27 (2008) 2163–; doi:10.1021/om8001334

data_4071369
_publ_section_title
;
 Synthesis of a 1-Hydrosilene Stable in Solution and Its Unique
 Properties#
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2163
_journal_paper_doi               10.1021/om8001334
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C41 H72 O2 Si7'
_chemical_formula_sum            'C41 H72 O2 Si7'
_chemical_formula_weight         793.62
_chemical_name_common            compound5
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                84.6454(16)
_cell_angle_beta                 92.711(2)
_cell_angle_gamma                73.972(6)
_cell_formula_units_Z            2
_cell_length_a                   10.1725(6)
_cell_length_b                   11.8167(5)
_cell_length_c                   20.9701(10)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.80
_cell_volume                     2405.1(2)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_sigmaI/netI    0.1020
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21194
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.9775
_exptl_absorpt_correction_T_min  0.9557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          15.000
_refine_ls_shift/su_mean         0.032
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1632
_reflns_number_gt                5162
_reflns_number_total             8848
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8001334-file001.cif
_cod_data_source_block           comp5
_cod_original_sg_symbol_Hall     '    -P 1'
_cod_database_code               4071369