Room-Temperature Reaction of Carbon Monoxide with a Stable Diarylgermylene
Xinping Wang; Zhongliang Zhu; Yang Peng; Hao Lei; James C. Fettinger; Philip P. Power; Journal of the American Chemical Society 131 (2009) 6912–6913; doi:10.1021/ja9017286

data_4104415
_publ_section_title
;
 Room-Temperature Reaction of Carbon Monoxide with a Stable
 Diarylgermylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6912
_journal_page_last               6913
_journal_paper_doi               10.1021/ja9017286
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         '2(C68 H86 Ge O2), 7(C7 H8)'
_chemical_formula_sum            'C185 H228 Ge2 O4'
_chemical_formula_weight         2660.85
_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                 97.7840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.8193(5)
_cell_length_b                   49.856(2)
_cell_length_c                   14.1848(6)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.57
_cell_volume                     7580.9(6)
_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  0.0808
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       64
_diffrn_reflns_limit_k_min       -64
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            65164
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.9515
_exptl_absorpt_correction_T_min  0.9282
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     925
_refine_ls_number_reflns         17377
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+2.4719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                12679
_reflns_number_total             17377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9017286_si_003.cif
_cod_data_source_block           xp222fmi
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4104415