Isomerization of an N-Heterocyclic Germylene to an Azagermabenzen-1-ylidene and Its Coupling to a Unique Bis(germylene)§
Yao, Shenglai; Zhang, Xinhao; Xiong, Yun; Schwarz, Helmut; Driess, Matthias; Organometallics 29 (2010) 5353–; doi:10.1021/om100383y

data_4066289
_publ_section_title
;
 Isomerization of an N-Heterocyclic Germylene to an
 Azagermabenzen-1-ylidene and Its Coupling to a Unique
 Bis(germylene)&#x00A7;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5353
_journal_paper_doi               10.1021/om100383y
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C64 H94 Ge2 N4'
_chemical_formula_weight         1064.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_cell_angle_alpha                78.926(12)
_cell_angle_beta                 82.882(17)
_cell_angle_gamma                78.326(16)
_cell_formula_units_Z            2
_cell_length_a                   11.403(3)
_cell_length_b                   14.520(2)
_cell_length_c                   18.793(3)
_cell_measurement_reflns_used    6968
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6572
_cell_measurement_theta_min      2.9263
_cell_volume                     2978.8(10)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       \w
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.1652
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23925
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  0.9301
_exptl_absorpt_correction_T_min  0.8670
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
Analytical numeric absorption correction using a multifaceted crystal
  model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         10182
_refine_ls_number_restraints     381
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                5230
_reflns_number_total             10182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100383y_si_002.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        2978.7(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4066289