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_4122725
_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_sum            'C40 H51 Cl Ge N2 O3 W'
_chemical_formula_weight         899.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.2116(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.2024(4)
_cell_length_b                   13.7121(2)
_cell_length_c                   25.3895(4)
_cell_measurement_reflns_used    137335
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      0.90
_cell_volume                     7871.8(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            109593
_diffrn_reflns_theta_full        27.38
_diffrn_reflns_theta_max         27.38
_diffrn_reflns_theta_min         0.90
_exptl_absorpt_coefficient_mu    3.789
_exptl_absorpt_correction_T_max  0.3196
_exptl_absorpt_correction_T_min  0.2804
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.39
_refine_diff_density_max         11.554
_refine_diff_density_min         -2.502
_refine_diff_density_rms         0.356
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         17795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0663P)^2^+63.9103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1404
_reflns_number_gt                15913
_reflns_number_total             17795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja506018f_si_002.cif
_cod_data_source_block           Cp*(CO)3WGeCl(IPr)_1a
_cod_depositor_comments
'Adding full bibliography for 4122725--4122730.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4122725