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_4117690
_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 N3 Sn), 3(C7 H8), 2(Cl3 Sn)'
_chemical_formula_sum            'C43.5 H55 Cl4 N3 Sn2'
_chemical_formula_weight         999.09
_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                92.68(2)
_cell_angle_beta                 99.08(2)
_cell_angle_gamma                103.21(2)
_cell_formula_units_Z            2
_cell_length_a                   10.438(2)
_cell_length_b                   13.174(2)
_cell_length_c                   16.908(4)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.535
_cell_measurement_theta_min      2.213
_cell_volume                     2226.8(8)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Smart APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56085
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       13
_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       -21
_diffrn_reflns_number            53144
_diffrn_reflns_theta_full        20.60
_diffrn_reflns_theta_max         20.60
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.5907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       needle
_exptl_crystal_F_000             1010
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.941
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.092
_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     517
_refine_ls_number_reflns         9044
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0313P)^2^+0.6545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                7376
_reflns_number_total             9044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja300563g_si_003.cif
_cod_data_source_block           sad
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_formula_sum        'C43.50 H55 Cl4 N3 Sn2'
_cod_database_code               4117690