An Unsymmetric Oxo/Imido-Bridged Germanium-Centered Singlet Diradicaloid
Xinping Wang; Yang Peng; Marilyn M. Olmstead; James C. Fettinger; Philip P. Power; Journal of the American Chemical Society 131 (2009) 14164–14165; doi:10.1021/ja906053y

data_4105120
_publ_section_title
;
 An Unsymmetric Oxo/Imido-Bridged Germanium-Centered Singlet Diradicaloid
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14164
_journal_page_last               14165
_journal_paper_doi               10.1021/ja906053y
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C67 H81 Ge2 N O, 0.5(C7 H8)'
_chemical_formula_sum            'C70.5 H85 Ge2 N O'
_chemical_formula_weight         1107.57
_chemical_name_common            D*Ge(O)(NPh)GeD*.0.5toluene
_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           SHELXL-97
_cell_angle_alpha                95.349(6)
_cell_angle_beta                 96.099(6)
_cell_angle_gamma                95.729(6)
_cell_formula_units_Z            2
_cell_length_a                   11.878(5)
_cell_length_b                   12.684(5)
_cell_length_c                   20.133(8)
_cell_measurement_reflns_used    3404
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      21.9
_cell_measurement_theta_min      2.7
_cell_volume                     2984(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_publication_material  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART ApexII'
_diffrn_measurement_method       \w
_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  0.1168
_diffrn_reflns_av_sigmaI/netI    0.1563
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27576
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            purplish-black
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             1174
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.101
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         10757
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1777
_refine_ls_R_factor_gt           0.1091
_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^)+(0.1221P)^2^+25.7798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2718
_refine_ls_wR_factor_ref         0.2956
_reflns_number_gt                6175
_reflns_number_total             10757
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja906053y_si_002_2.cif
_cod_data_source_block           xp229
_cod_original_formula_sum        'C70.50 H85 Ge2 N O'
_cod_database_code               4105120