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_4105520
_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            'C68 H82 Ge2'
_chemical_formula_weight         1044.52
_chemical_name_systematic
; 
 ? 
;
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_cell_angle_gamma                90.00
_cell_formula_units_Z            4
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_cell_length_b                   11.8007(5)
_cell_length_c                   25.3005(16)
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_cell_measurement_temperature    90(2)
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_cell_measurement_theta_min      2.46
_cell_volume                     5690.9(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            24126
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.9523
_exptl_absorpt_correction_T_min  0.9126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       Block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6551
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0367P)^2^+6.2822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                5920
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107380p_si_002.cif
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