Reactivity of Ar'GeGeAr' (Ar' = C6H3-2,6-Dipp2, Dipp = C6H3-2,6-iPr2) toward Alkynes: Isolation of a Stable Digermacyclobutadiene
Chunming Cui; Marilyn M. Olmstead; Philip P. Power; Journal of the American Chemical Society 126 (2004) 5062–5063; doi:10.1021/ja0318481

data_4112474
_publ_section_title
;
 Reactivity of Ar'GeGeAr' (Ar' = C6H3-2,6-Dipp2, Dipp = C6H3-2,6-iPr2)
 toward Alkynes: Isolation of a Stable Digermacyclobutadiene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5062
_journal_page_last               5063
_journal_paper_doi               10.1021/ja0318481
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C84 H107.38 Ge2'
_chemical_formula_weight         1262.26
_chemical_name_common
'[Dipp*Ge(PhC=CPh)GeDipp*].1.5n-hexane.0.17methylcyclopentane'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   43.910(7)
_cell_length_b                   43.910(7)
_cell_length_c                   19.208(7)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      40.0
_cell_measurement_theta_min      3.8
_cell_volume                     32073(14)
_computing_cell_refinement       'P3-PC (Siemens, 1994)'
_computing_data_collection       'P3-PC (Siemens, 1994)'
_computing_data_reduction        'XDISK (Siemens, 1994)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'Siemens rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            17298
_diffrn_reflns_theta_full        56.04
_diffrn_reflns_theta_max         56.04
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  0.5524
_exptl_absorpt_correction_T_min  0.5192
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   XABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             12157
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         9237
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+328.5847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1705
_reflns_number_gt                7378
_reflns_number_total             9237
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0318481si20031219_053744.cif
_cod_data_source_block           mn1554
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4112474