On the Synthesis, Structure, and Reactivity of Tetramesityldigermene
Hurni, Krysten L.; Rupar, Paul A.; Payne, Nicholas C.; Baines, Kim M.; Organometallics 26 (2007) 5569–; doi:10.1021/om7005358

data_4073685
_publ_section_title
;
 On the Synthesis, Structure, and Reactivity of Tetramesityldigermene
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5569
_journal_paper_doi               10.1021/om7005358
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C41 H54 Ge2 O2'
_chemical_formula_sum            'C41 H54 Ge2 O2'
_chemical_formula_weight         724.02
_chemical_melting_point          463
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.320(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8332(4)
_cell_length_b                   14.0900(3)
_cell_length_c                   20.2794(6)
_cell_measurement_temperature    150(2)
_cell_volume                     3656.50(19)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2001)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_av_sigmaI/netI    0.063
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15532
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.04
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.677
_exptl_absorpt_correction_T_max  0.8845
_exptl_absorpt_correction_T_min  0.5030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1520
_exptl_crystal_recrystallization_method 'slow evaporation from C6H6'
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         8310
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+1.2471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1414
_reflns_number_gt                5465
_reflns_number_total             8310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7005358-file003.cif
_cod_data_source_block           Compound8a
_cod_original_cell_volume        3656.50(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4073685