A Digermyne with a Ge-Ge Single Bond That Activates Dihydrogen in the Solid State
Jiaye Li; Christian Schenk; Catharina Goedecke; Gernot Frenking; Cameron Jones; Journal of the American Chemical Society 133 (2011) 18622–18625; doi:10.1021/ja209215a

data_4107158
_publ_section_title
;
 A Digermyne with a Ge-Ge Single Bond That Activates Dihydrogen in the
 Solid State
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18622
_journal_page_last               18625
_journal_paper_doi               10.1021/ja209215a
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C80 H95 Ge2 K N2 O2 Si2'
_chemical_formula_weight         1357.04
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 107.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.375(3)
_cell_length_b                   21.468(4)
_cell_length_c                   14.592(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3695.6(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13869
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.037
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         13869
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0103P)^2^+4.0910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0912
_reflns_number_gt                11353
_reflns_number_total             13869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja209215a_si_006.cif
_cod_data_source_block           compound2S
_cod_original_cell_volume        3695.6(13)
_cod_database_code               4107158