Reactions of a Tungsten-Germylyne Complex with α,β-Unsaturated Ketones: Complete Cleavage of the W≡Ge Bond and Formation of Two Types of η(3)-Germoxyallyl Tungsten Complexes.
Fukuda, Tetsuya; Hashimoto, Hisako; Tobita, Hiromi; Journal of the American Chemical Society 136 (2014) 80–83; doi:10.1021/ja4109853

data_4120680
_publ_section_title
;
 Reactions of a Tungsten-Germylyne Complex with \a,\b-Unsaturated Ketones:
 Complete Cleavage of the W\\tb Ge Bond and Formation of Two Types of
 \h(3)-Germoxyallyl Tungsten Complexes.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              80
_journal_page_last               83
_journal_paper_doi               10.1021/ja4109853
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C32 H58 Ge O4 Si3 W'
_chemical_formula_sum            'C32 H58 Ge O4 Si3 W'
_chemical_formula_weight         847.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 101.0203(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9057(6)
_cell_length_b                   10.5686(4)
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_cell_measurement_reflns_used    54361
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.41
_cell_volume                     3777.9(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
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_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotation-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0871
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_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47086
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    3.965
_exptl_absorpt_correction_T_max  0.6068
_exptl_absorpt_correction_T_min  0.4758
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'NUMABS (Higashi, 1999)''ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.941
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         8609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+7.1132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1110
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4109853_si_002.cif
_cod_data_source_block           tf072
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               4120680