Facile synthesis of dichlorosilane by metathesis reaction and dehydrogenation of dihydrogermane by a frustrated Lewis pair.
Jana, Anukul; Tavcar, Gasper; Roesky, Herbert W.; Schulzke, Carola; Dalton transactions (Cambridge, England : 2003) 39 (2010) 6217–6220; doi:10.1039/c002395g

data_7025631
_publ_section_title
;
 Facile synthesis of dichlorosilane by metathesis reaction and
 dehydrogenation of dihydrogermane by a frustrated Lewis pair.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6217
_journal_page_last               6220
_journal_paper_doi               10.1039/c002395g
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C20 H24 Cl2 Ge N2'
_chemical_formula_weight         435.90
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.174(3)
_cell_length_b                   7.3558(15)
_cell_length_c                   15.804(3)
_cell_measurement_reflns_used    19271
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      54.0
_cell_measurement_theta_min      4.7
_cell_volume                     1996.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0980
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17399
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.807
_exptl_absorpt_correction_T_max  0.7076
_exptl_absorpt_correction_T_min  0.4529
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                1574
_reflns_number_total             2102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002395g.txt
_cod_data_source_block           ja2
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7025631