Reactions of d0 tungsten alkylidyne complexes with O2 or H2O. Formation of an oxo siloxy complex through unusual silyl migrations
Laurel A. Morton; Maozhong Miao; Tabitha M. Callaway; Tianniu Chen; Shu-Jian Chen; Albert A. Tuinman; Xianghua Yu; Zheng Lu; Zi-Ling Xue; Chem.Commun. 49 (2013) 9555–; doi:10.1039/c3cc46014b

data_7109872
_publ_section_title
;
 Reactions of d0 tungsten alkylidyne complexes with O2 or H2O. Formation
 of an oxo siloxy complex through unusual silyl migrations
;
_journal_name_full               Chem.Commun.
_journal_page_first              9555
_journal_paper_doi               10.1039/c3cc46014b
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C31 H84 O2 Si8 W2'
_chemical_formula_weight         1081.40
_chemical_name_systematic
; 
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   16.1077(7)
_cell_length_b                   16.1077(7)
_cell_length_c                   68.397(4)
_cell_measurement_temperature    173(2)
_cell_volume                     15368.6(13)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       91
_diffrn_reflns_limit_l_min       -91
_diffrn_reflns_number            46502
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    4.697
_exptl_absorpt_correction_T_max  0.5393
_exptl_absorpt_correction_T_min  0.3428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             6552
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.421
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         8397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.080
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+126.6670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                5689
_reflns_number_total             8397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc46014b.txt
_cod_data_source_block           wa
_cod_original_cell_volume        15368.5(13)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7109872