Unusual Electrocyclic Rearrangements with Group 14 Element Compounds: Reversible Isomerization of a π-Aromatic Digermyl Complex with Carbon-Carbon and Germanium-Germanium Multiple Bond Cleavage
Owen T. Summerscales; J. Oscar C. Jiménez-Halla; Gabriel Merino; Philip P. Power; Journal of the American Chemical Society 133 (2011) 180–183; doi:10.1021/ja107380p

data_4105521
_publ_section_title
;
 Unusual Electrocyclic Rearrangements with Group 14 Element Compounds:
 Reversible Isomerization of a \p-Aromatic Digermyl Complex with
 Carbon-Carbon and Germanium-Germanium Multiple Bond Cleavage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              180
_journal_page_last               183
_journal_paper_doi               10.1021/ja107380p
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C72 H92 Ge2 O'
_chemical_formula_weight         1118.64
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.156(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0753(7)
_cell_length_b                   34.0196(17)
_cell_length_c                   13.3778(7)
_cell_measurement_reflns_used    9706
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      68.13
_cell_measurement_theta_min      3.55
_cell_volume                     5941.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            46784
_diffrn_reflns_theta_full        68.61
_diffrn_reflns_theta_max         68.61
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    1.563
_exptl_absorpt_correction_T_max  0.9259
_exptl_absorpt_correction_T_min  0.8918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         10509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.059
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                10469
_reflns_number_total             10509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107380p_si_003.cif
_cod_data_source_block           ots10f1
_cod_database_code               4105521