Synthesis, Structure, and Bonding Nature of Ethynediyl-Bridged Bis(silylene) Dinuclear Complexes of Tungsten and Molybdenum
Sakaba, Hiroyuki; Oike, Hiroyuki; Kawai, Masaaki; Takami, Masato; Kabuto, Chizuko; Ray, Mausumi; Nakao, Yoshihide; Sato, Hirofumi; Sakaki, Shigeyoshi; Organometallics 30 (2011) 4515–; doi:10.1021/om200096z

data_4064427
_publ_section_title
;
 Synthesis, Structure, and Bonding Nature of Ethynediyl-Bridged
 Bis(silylene) Dinuclear Complexes of Tungsten and Molybdenum
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4515
_journal_paper_doi               10.1021/om200096z
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C57 H58 O4 Si2 W2 '
_chemical_formula_sum            'C57 H58 O4 Si2 W2'
_chemical_formula_weight         1230.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.8710(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.754(4)
_cell_length_b                   17.657(5)
_cell_length_c                   18.402(4)
_cell_measurement_reflns_used    16934
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     5116(2)
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            71469
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    4.590
_exptl_absorpt_correction_T_max  0.632
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2432.00
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.120
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.822
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         11510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.822
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                8131
_reflns_number_total             11510
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om200096z_si_001.cif
_cod_data_source_block           complex5
_cod_original_formula_sum        'C57 H58 O4 Si2 W2 '
_cod_database_code               4064427