Synthesis of Silylium and Germylium Ions by a Substituent Exchange Reaction
Schäfer, André; Reißmann, Matti; Jung, Sebastian; Schäfer, Annemarie; Saak, Wolfgang; Brendler, Erica; Müller, Thomas; Organometallics 32 (2013) 4713–; doi:10.1021/om400366z

data_4081243
_publ_section_title
;
 Synthesis of Silylium and Germylium Ions by a Substituent Exchange
 Reaction
;
_journal_name_full               Organometallics
_journal_page_first              4713
_journal_paper_doi               10.1021/om400366z
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C42 H36 B12 Cl12 N2'
_chemical_formula_weight         1123.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.9460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5998(3)
_cell_length_b                   12.5409(2)
_cell_length_c                   17.0420(3)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      34.96
_cell_measurement_theta_min      3.40
_cell_volume                     2561.84(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond Crystal Impact, 2010)'
_computing_publication_material  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46344
_diffrn_reflns_theta_full        35.01
_diffrn_reflns_theta_max         35.01
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.7739
_exptl_absorpt_correction_T_min  0.7279
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         11245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.5396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0752
_reflns_number_gt                9590
_reflns_number_total             11245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400366z_si_003.cif
_cod_data_source_block           ANS201
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4081243