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_4105119
_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         '(C60 H74 Ge2 O4), 3.5(C7 H8)'
_chemical_formula_sum            'C84.5 H102 Ge2 O4'
_chemical_formula_weight         1326.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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                 105.873(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.330(3)
_cell_length_b                   16.550(3)
_cell_length_c                   27.623(5)
_cell_measurement_reflns_used    4278
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      2.62
_cell_volume                     7181(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0828
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12967
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  0.9381
_exptl_absorpt_correction_T_min  0.8047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS V2008/3 (Sheldrick, 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2820
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.928
_refine_diff_density_min         -2.157
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         13160
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0924
_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^)+(0.1065P)^2^+31.7496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2316
_refine_ls_wR_factor_ref         0.2420
_reflns_number_gt                10368
_reflns_number_total             13160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906053y_si_002_1.cif
_cod_data_source_block           tw51
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C84.50 H102 Ge2 O4'
_cod_database_code               4105119