Cationic Metallogermylene and Dicationic Dimetallodigermenes: Synthesis by Chloride Abstraction from N-Heterocyclic Carbene-Stabilized Chlorometallogermylenes.
Inomata, Koya; Watanabe, Takahito; Tobita, Hiromi; Journal of the American Chemical Society 136 (2014) 14341–; doi:10.1021/ja506018f

data_4122729
_publ_section_title
;
 Cationic Metallogermylene and Dicationic Dimetallodigermenes: Synthesis
 by Chloride Abstraction from N-Heterocyclic Carbene-Stabilized
 Chlorometallogermylenes.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14341
_journal_paper_doi               10.1021/ja506018f
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'(C48 H70 Ge2 N4 O6 W2), 2(C32 H12 B F24), 3(C6 H5 F)'
_chemical_formula_sum            'C130 H109 B2 F51 Ge2 N4 O6 W2'
_chemical_formula_weight         3326.71
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.4360(11)
_cell_angle_beta                 94.1879(10)
_cell_angle_gamma                98.6647(9)
_cell_formula_units_Z            2
_cell_length_a                   12.8703(4)
_cell_length_b                   19.4136(5)
_cell_length_c                   27.6906(10)
_cell_measurement_reflns_used    55016
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.34
_cell_volume                     6794.1(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_molecular_graphics    'Yadokari-XG 2009'
_computing_publication_material  'Yadokari-XG 2009'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            76190
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         0.74
_exptl_absorpt_coefficient_mu    2.250
_exptl_absorpt_correction_T_max  0.7147
_exptl_absorpt_correction_T_min  0.6031
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            orange/green
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3292
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.126
_refine_diff_density_min         -1.464
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1563
_refine_ls_number_reflns         30094
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0776
_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^)+(0.0892P)^2^+53.1520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.1982
_reflns_number_gt                22689
_reflns_number_total             30094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja506018f_si_002.cif
_cod_data_source_block           '[{Cp*(CO)3WGe(MeIiPr)}2](BAr4)2_3'
_cod_depositor_comments
'Adding full bibliography for 4122725--4122730.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4122729