Iron, Ruthenium, and Osmium Complexes Supported by the Bis(silyl) Chelate Ligand (9,9-Dimethylxanthene-4,5-diyl)bis(dimethylsilyl): Synthesis, Characterization, and Reactivity
Minglana, Jim Josephus G.; Okazaki, Masaaki; Hasegawa, Kenji; Luh, Lung-Shiang; Yamahira, Nobukazu; Komuro, Takashi; Ogino, Hiroshi; Tobita, Hiromi; Organometallics 26 (2007) 5859–; doi:10.1021/om700720s

data_4073910
_publ_section_title
;
 Iron, Ruthenium, and Osmium Complexes Supported by the Bis(silyl) Chelate
 Ligand (9,9-Dimethylxanthene-4,5-diyl)bis(dimethylsilyl):&#x00A0;
 Synthesis, Characterization, and Reactivity
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5859
_journal_paper_doi               10.1021/om700720s
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C27 H42 O Si2'
_chemical_formula_sum            'C27 H42 O Si2'
_chemical_formula_weight         438.79
_chemical_name_common            1b
_chemical_name_systematic        1b
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 97.83(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.319(4)
_cell_length_b                   10.579(3)
_cell_length_c                   13.042(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.890
_cell_measurement_theta_min      27.750
_cell_volume                     1410.5(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3603
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.58
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.9997
_exptl_absorpt_correction_T_min  0.5746
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            prismatic
_exptl_crystal_density_diffrn    1.033
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colorless
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         3420
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.129
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+0.1239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1597
_reflns_number_gt                2196
_reflns_number_total             3420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700720s-file002.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4073910