From Tetragermacyclobutene to Tetragermacyclobutadiene Dianion to Tetragermacyclobutadiene Transition Metal Complexes
Vladimir Ya. Lee; Yuki Ito; Hiroyuki Yasuda; Kazunori Takanashi; Akira Sekiguchi; Journal of the American Chemical Society 133 (2011) 5103–5108; doi:10.1021/ja111596g

data_4105876
_publ_section_title
;
 From Tetragermacyclobutene to Tetragermacyclobutadiene Dianion to
 Tetragermacyclobutadiene Transition Metal Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5103
_journal_page_last               5108
_journal_paper_doi               10.1021/ja111596g
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C41 H89 Co Ge4 Si4'
_chemical_formula_weight         1043.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3738(8)
_cell_length_b                   15.9280(6)
_cell_length_c                   17.0381(7)
_cell_measurement_reflns_used    8554
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.44
_cell_measurement_theta_min      2.39
_cell_volume                     5257.7(4)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26509
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    2.685
_exptl_absorpt_correction_T_max  0.5533
_exptl_absorpt_correction_T_min  0.4365
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       prism
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5410
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0223
_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^)+(0.0195P)^2^+2.3831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0548
_reflns_number_gt                4346
_reflns_number_total             5410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja111596g_si_002.cif
_cod_data_source_block           r4ge4cocp_0ma
_cod_database_code               4105876