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_4120681
_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         'C27 H50 Ge O3 Si3 W'
_chemical_formula_sum            'C27 H50 Ge O3 Si3 W'
_chemical_formula_weight         763.38
_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                81.533(6)
_cell_angle_beta                 78.365(6)
_cell_angle_gamma                76.447(5)
_cell_formula_units_Z            2
_cell_length_a                   8.9578(7)
_cell_length_b                   9.0925(7)
_cell_length_c                   21.2200(17)
_cell_measurement_reflns_used    17575
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      3.200
_cell_volume                     1636.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.827
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18252
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.16
_diffrn_standards_number         18252
_exptl_absorpt_coefficient_mu    4.564
_exptl_absorpt_correction_T_max  0.9143
_exptl_absorpt_correction_T_min  0.6582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.804
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         7518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0279P)^2^+1.2022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                6866
_reflns_number_total             7518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4109853_si_002.cif
_cod_data_source_block           tf_ex05
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4120681