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_4105877
_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            'C36 H84 Cl2 Ge4 Si4'
_chemical_formula_weight         990.65
_chemical_name_systematic
; 
 dichlorotetragermetene
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 112.773(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   41.2970(9)
_cell_length_b                   15.6660(7)
_cell_length_c                   17.2710(7)
_cell_measurement_reflns_used    51989
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.06
_cell_volume                     10302.6(7)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51989
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    2.530
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       cube
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.006
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.00133(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         11764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                8979
_reflns_number_total             11764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja111596g_si_004.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               4105877