Lewis Base Mediated Autoionization of GeCl2 and SnCl2
Amit Pratap Singh; Herbert W. Roesky; Elena Carl; Dietmar Stalke; Jean-Philippe Demers; Adam Lange; Journal of the American Chemical Society 134 (2012) 4998–5003; doi:10.1021/ja300563g

data_4117689
_publ_section_title
;
 Lewis Base Mediated Autoionization of GeCl2 and SnCl2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4998
_journal_page_last               5003
_journal_paper_doi               10.1021/ja300563g
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         '2(C33 H43 Cl Ge N3), 3(C7 H8), 2(Cl3 Ge)'
_chemical_formula_sum            'C43.5 H55 Cl4 Ge2 N3'
_chemical_formula_weight         906.89
_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                93.66(2)
_cell_angle_beta                 97.33(2)
_cell_angle_gamma                103.26(2)
_cell_formula_units_Z            2
_cell_length_a                   10.330(3)
_cell_length_b                   13.013(3)
_cell_length_c                   16.873(7)
_cell_measurement_reflns_used    9725
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.743
_cell_measurement_theta_min      2.240
_cell_volume                     2179.4(12)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'shelXle v0.477'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker Smart Apex II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9181
_diffrn_reflns_theta_full        26.83
_diffrn_reflns_theta_max         26.83
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  0.745432
_exptl_absorpt_correction_T_min  0.654535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS-2008/4
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       needle
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         9181
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0247P)^2^+0.9303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                7897
_reflns_number_total             9181
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja300563g_si_002.cif
_cod_data_source_block           twin4_a
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_formula_sum        'C43.50 H55 Cl4 Ge2 N3'
_cod_database_code               4117689