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_4073914
_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_sum            'C52 H48 O16 Ru4 Si4'
_chemical_formula_weight         1445.54
_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                90.3239(19)
_cell_angle_beta                 111.541(2)
_cell_angle_gamma                103.163(3)
_cell_formula_units_Z            2
_cell_length_a                   15.2588(9)
_cell_length_b                   17.1038(11)
_cell_length_c                   12.2358(6)
_cell_measurement_reflns_used    11662
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      54.94
_cell_measurement_theta_min      4.22
_cell_volume                     2878.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25453
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  0.8913
_exptl_absorpt_correction_T_min  0.7189
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   Coppens_numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         12542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+3.9074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                11174
_reflns_number_total             12542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700720s-file002.cif
_cod_data_source_block           3/5
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073914