#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:48:01 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178628 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/39/4073913.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4073913
loop_
_publ_author_name
'Minglana, Jim Josephus G.'
'Okazaki, Masaaki'
'Hasegawa, Kenji'
'Luh, Lung-Shiang'
'Yamahira, Nobukazu'
'Komuro, Takashi'
'Ogino, Hiroshi'
'Tobita, Hiromi'
_publ_section_title
;
 Iron, Ruthenium, and Osmium Complexes Supported by the Bis(silyl) Chelate
 Ligand (9,9-Dimethylxanthene-4,5-diyl)bis(dimethylsilyl): 
 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            'C23 H24 O5 Os Si2'
_chemical_formula_weight         626.80
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.018(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3110(7)
_cell_length_b                   10.0336(6)
_cell_length_c                   19.1542(19)
_cell_measurement_reflns_used    15472
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.96
_cell_measurement_theta_min      2.13
_cell_volume                     2362.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18006
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.13
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.530
_exptl_absorpt_correction_T_max  0.6078
_exptl_absorpt_correction_T_min  0.2478
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   Higashi
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.152
_refine_diff_density_min         -2.494
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0290
_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/[σ²(Fo²)+(0.0372P)²+26.3198P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                4647
_reflns_number_total             5019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700720s-file002.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4073913
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Os1 Os 0.584957(19) 0.39266(3) 0.163671(11) 0.01833(9) Uani 1 1 d .
Si1 Si 0.50396(14) 0.16190(18) 0.18846(8) 0.0191(3) Uani 1 1 d .
Si2 Si 0.41461(15) 0.52291(18) 0.19502(8) 0.0192(3) Uani 1 1 d .
C1 C 0.5145(5) 0.3667(7) 0.0705(3) 0.0198(12) Uani 1 1 d .
O1 O 0.4768(4) 0.3509(5) 0.0165(2) 0.0267(10) Uani 1 1 d .
C2 C 0.7216(7) 0.2938(8) 0.1485(4) 0.0367(19) Uani 1 1 d .
O2 O 0.8013(4) 0.2407(7) 0.1432(3) 0.0489(17) Uani 1 1 d .
C3 C 0.6079(5) 0.4110(7) 0.2641(4) 0.0260(15) Uani 1 1 d .
O3 O 0.6198(5) 0.4233(6) 0.3221(2) 0.0374(13) Uani 1 1 d .
C4 C 0.6463(6) 0.5668(8) 0.1422(4) 0.0294(15) Uani 1 1 d .
O4 O 0.6845(5) 0.6668(6) 0.1306(3) 0.0477(15) Uani 1 1 d .
O5 O 0.2966(4) 0.2910(4) 0.1391(2) 0.0192(9) Uani 1 1 d .
C5 C 0.4384(6) 0.1421(8) 0.2737(3) 0.0290(15) Uani 1 1 d .
H1 H 0.3700 0.1925 0.2724 0.043 Uiso 1 1 calc R
H2 H 0.4873 0.1760 0.3116 0.043 Uiso 1 1 calc R
H3 H 0.4233 0.0476 0.2817 0.043 Uiso 1 1 calc R
C6 C 0.6159(7) 0.0327(8) 0.1934(4) 0.0338(17) Uani 1 1 d .
H4 H 0.6709 0.0579 0.2299 0.051 Uiso 1 1 calc R
H5 H 0.6496 0.0275 0.1483 0.051 Uiso 1 1 calc R
H6 H 0.5852 -0.0543 0.2047 0.051 Uiso 1 1 calc R
C7 C 0.3455(5) 0.4695(7) 0.2753(3) 0.0219(13) Uani 1 1 d .
H7 H 0.2961 0.5400 0.2893 0.033 Uiso 1 1 calc R
H8 H 0.4003 0.4527 0.3132 0.033 Uiso 1 1 calc R
H9 H 0.3040 0.3877 0.2652 0.033 Uiso 1 1 calc R
C8 C 0.4509(6) 0.7030(7) 0.2105(4) 0.0295(15) Uani 1 1 d .
H10 H 0.4757 0.7421 0.1672 0.044 Uiso 1 1 calc R
H11 H 0.5092 0.7093 0.2472 0.044 Uiso 1 1 calc R
H12 H 0.3868 0.7515 0.2251 0.044 Uiso 1 1 calc R
C9 C 0.4024(5) 0.1037(6) 0.1163(3) 0.0179(12) Uani 1 1 d .
C10 C 0.4184(6) -0.0088(7) 0.0744(3) 0.0240(13) Uani 1 1 d .
H13 H 0.4802 -0.0639 0.0836 0.029 Uiso 1 1 calc R
C11 C 0.3442(6) -0.0401(7) 0.0194(3) 0.0282(15) Uani 1 1 d .
H14 H 0.3558 -0.1172 -0.0080 0.034 Uiso 1 1 calc R
C12 C 0.2547(6) 0.0383(7) 0.0040(3) 0.0254(14) Uani 1 1 d .
H15 H 0.2059 0.0158 -0.0342 0.030 Uiso 1 1 calc R
C13 C 0.2352(5) 0.1502(6) 0.0440(3) 0.0168(12) Uani 1 1 d .
C14 C 0.3096(5) 0.1786(6) 0.0988(3) 0.0169(11) Uani 1 1 d .
C15 C 0.3081(5) 0.5229(6) 0.1208(3) 0.0178(12) Uani 1 1 d .
C16 C 0.2741(5) 0.6347(7) 0.0827(3) 0.0216(13) Uani 1 1 d .
H16 H 0.3021 0.7200 0.0954 0.026 Uiso 1 1 calc R
C17 C 0.1988(6) 0.6222(7) 0.0256(4) 0.0251(14) Uani 1 1 d .
H17 H 0.1785 0.6990 -0.0010 0.030 Uiso 1 1 calc R
C18 C 0.1534(5) 0.5004(7) 0.0073(3) 0.0206(13) Uani 1 1 d .
H18 H 0.1012 0.4946 -0.0309 0.025 Uiso 1 1 calc R
C19 C 0.1841(5) 0.3853(6) 0.0448(3) 0.0188(12) Uani 1 1 d .
C20 C 0.2578(6) 0.4025(6) 0.1010(3) 0.0212(13) Uani 1 1 d .
C21 C 0.1382(5) 0.2467(6) 0.0326(3) 0.0178(12) Uani 1 1 d .
C22 C 0.0563(5) 0.2167(7) 0.0873(3) 0.0243(14) Uani 1 1 d .
H19 H 0.0929 0.2196 0.1340 0.036 Uiso 1 1 calc R
H20 H 0.0253 0.1278 0.0789 0.036 Uiso 1 1 calc R
H21 H -0.0019 0.2833 0.0843 0.036 Uiso 1 1 calc R
C23 C 0.0815(6) 0.2313(8) -0.0405(3) 0.0264(14) Uani 1 1 d .
H22 H 0.0524 0.1407 -0.0458 0.040 Uiso 1 1 calc R
H23 H 0.1342 0.2475 -0.0762 0.040 Uiso 1 1 calc R
H24 H 0.0219 0.2958 -0.0460 0.040 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C3 Os1 C4 95.0(3)
C3 Os1 C1 161.9(3)
C4 Os1 C1 94.8(3)
C3 Os1 C2 96.5(3)
C4 Os1 C2 94.4(3)
C1 Os1 C2 97.9(3)
C3 Os1 Si2 78.3(2)
C4 Os1 Si2 85.6(2)
C1 Os1 Si2 87.28(18)
C2 Os1 Si2 174.8(2)
C3 Os1 Si1 86.6(2)
C4 Os1 Si1 178.5(2)
C1 Os1 Si1 83.76(19)
C2 Os1 Si1 85.2(2)
Si2 Os1 Si1 94.90(6)
C5 Si1 C6 103.3(3)
C5 Si1 C9 107.7(3)
C6 Si1 C9 106.0(3)
C5 Si1 Os1 116.5(2)
C6 Si1 Os1 109.7(3)
C9 Si1 Os1 112.80(19)
C7 Si2 C8 105.1(3)
C7 Si2 C15 106.9(3)
C8 Si2 C15 105.6(3)
C7 Si2 Os1 117.2(2)
C8 Si2 Os1 109.6(2)
C15 Si2 Os1 111.60(19)
O1 C1 Os1 178.1(5)
O2 C2 Os1 176.3(7)
O3 C3 Os1 178.8(7)
O4 C4 Os1 178.1(7)
C14 O5 C20 114.0(4)
C14 C9 C10 115.6(6)
C14 C9 Si1 120.5(5)
C10 C9 Si1 123.7(5)
C11 C10 C9 120.5(6)
C12 C11 C10 121.3(6)
C11 C12 C13 120.3(6)
C14 C13 C12 117.3(6)
C14 C13 C21 117.0(5)
C12 C13 C21 125.8(5)
O5 C14 C13 120.0(5)
O5 C14 C9 115.1(5)
C13 C14 C9 124.9(6)
C16 C15 C20 115.9(5)
C16 C15 Si2 125.1(5)
C20 C15 Si2 119.0(5)
C15 C16 C17 120.4(6)
C18 C17 C16 121.3(6)
C17 C18 C19 120.3(5)
C20 C19 C18 116.3(6)
C20 C19 C21 117.3(5)
C18 C19 C21 126.2(5)
C19 C20 C15 125.6(6)
C19 C20 O5 119.7(6)
C15 C20 O5 114.4(5)
C19 C21 C22 109.4(5)
C19 C21 C23 112.3(5)
C22 C21 C23 108.8(5)
C19 C21 C13 106.0(5)
C22 C21 C13 108.3(5)
C23 C21 C13 112.1(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Os1 C3 1.938(7)
Os1 C4 1.955(8)
Os1 C1 1.960(6)
Os1 C2 1.987(9)
Os1 Si2 2.5689(18)
Os1 Si1 2.5750(18)
Si1 C5 1.869(7)
Si1 C6 1.891(8)
Si1 C9 1.905(6)
Si2 C7 1.874(6)
Si2 C8 1.881(7)
Si2 C15 1.883(6)
C1 O1 1.123(8)
C2 O2 1.125(10)
C3 O3 1.121(9)
C4 O4 1.136(9)
O5 C14 1.381(7)
O5 C20 1.405(7)
C9 C14 1.394(8)
C9 C10 1.405(9)
C10 C11 1.392(10)
C11 C12 1.373(10)
C12 C13 1.387(9)
C13 C14 1.385(8)
C13 C21 1.544(8)
C15 C16 1.391(9)
C15 C20 1.400(9)
C16 C17 1.401(9)
C17 C18 1.382(10)
C18 C19 1.401(8)
C19 C20 1.383(9)
C19 C21 1.514(9)
C21 C22 1.521(8)
C21 C23 1.539(8)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C3 Os1 Si1 C5 28.8(3)
C4 Os1 Si1 C5 -159(8)
C1 Os1 Si1 C5 -135.8(3)
C2 Os1 Si1 C5 125.6(3)
Si2 Os1 Si1 C5 -49.1(3)
C3 Os1 Si1 C6 -88.0(3)
C4 Os1 Si1 C6 84(8)
C1 Os1 Si1 C6 107.3(3)
C2 Os1 Si1 C6 8.7(3)
Si2 Os1 Si1 C6 -166.0(3)
C3 Os1 Si1 C9 154.1(3)
C4 Os1 Si1 C9 -34(8)
C1 Os1 Si1 C9 -10.6(3)
C2 Os1 Si1 C9 -109.1(3)
Si2 Os1 Si1 C9 76.1(2)
C3 Os1 Si2 C7 -42.1(3)
C4 Os1 Si2 C7 -138.1(3)
C1 Os1 Si2 C7 126.8(3)
C2 Os1 Si2 C7 -48(2)
Si1 Os1 Si2 C7 43.3(2)
C3 Os1 Si2 C8 77.4(3)
C4 Os1 Si2 C8 -18.5(3)
C1 Os1 Si2 C8 -113.6(3)
C2 Os1 Si2 C8 71(2)
Si1 Os1 Si2 C8 162.9(2)
C3 Os1 Si2 C15 -165.9(3)
C4 Os1 Si2 C15 98.1(3)
C1 Os1 Si2 C15 3.0(3)
C2 Os1 Si2 C15 -172(2)
Si1 Os1 Si2 C15 -80.5(2)
C3 Os1 C1 O1 -159(17)
C4 Os1 C1 O1 78(18)
C2 Os1 C1 O1 -17(18)
Si2 Os1 C1 O1 164(18)
Si1 Os1 C1 O1 -101(18)
C3 Os1 C2 O2 -24(10)
C4 Os1 C2 O2 72(10)
C1 Os1 C2 O2 167(10)
Si2 Os1 C2 O2 -18(12)
Si1 Os1 C2 O2 -110(10)
C4 Os1 C3 O3 70(32)
C1 Os1 C3 O3 -52(33)
C2 Os1 C3 O3 165(32)
Si2 Os1 C3 O3 -14(32)
Si1 Os1 C3 O3 -110(32)
C3 Os1 C4 O4 61(22)
C1 Os1 C4 O4 -135(22)
C2 Os1 C4 O4 -36(22)
Si2 Os1 C4 O4 138(22)
Si1 Os1 C4 O4 -111(21)
C5 Si1 C9 C14 70.6(6)
C6 Si1 C9 C14 -179.4(5)
Os1 Si1 C9 C14 -59.3(5)
C5 Si1 C9 C10 -114.2(6)
C6 Si1 C9 C10 -4.2(6)
Os1 Si1 C9 C10 115.9(5)
C14 C9 C10 C11 -0.1(9)
Si1 C9 C10 C11 -175.5(5)
C9 C10 C11 C12 0.9(10)
C10 C11 C12 C13 -1.0(11)
C11 C12 C13 C14 0.5(10)
C11 C12 C13 C21 180.0(6)
C20 O5 C14 C13 -37.9(8)
C20 O5 C14 C9 140.0(6)
C12 C13 C14 O5 177.9(6)
C21 C13 C14 O5 -1.7(8)
C12 C13 C14 C9 0.3(9)
C21 C13 C14 C9 -179.3(6)
C10 C9 C14 O5 -178.2(5)
Si1 C9 C14 O5 -2.6(7)
C10 C9 C14 C13 -0.5(9)
Si1 C9 C14 C13 175.1(5)
C7 Si2 C15 C16 117.1(6)
C8 Si2 C15 C16 5.5(6)
Os1 Si2 C15 C16 -113.5(5)
C7 Si2 C15 C20 -63.0(6)
C8 Si2 C15 C20 -174.6(5)
Os1 Si2 C15 C20 66.4(5)
C20 C15 C16 C17 -3.7(9)
Si2 C15 C16 C17 176.2(5)
C15 C16 C17 C18 2.4(10)
C16 C17 C18 C19 -1.5(10)
C17 C18 C19 C20 2.0(9)
C17 C18 C19 C21 177.3(6)
C18 C19 C20 C15 -3.8(10)
C21 C19 C20 C15 -179.5(6)
C18 C19 C20 O5 -176.9(5)
C21 C19 C20 O5 7.4(9)
C16 C15 C20 C19 4.6(9)
Si2 C15 C20 C19 -175.3(5)
C16 C15 C20 O5 178.1(5)
Si2 C15 C20 O5 -1.8(7)
C14 O5 C20 C19 35.2(8)
C14 O5 C20 C15 -138.7(5)
C20 C19 C21 C22 73.9(7)
C18 C19 C21 C22 -101.3(7)
C20 C19 C21 C23 -165.2(6)
C18 C19 C21 C23 19.5(9)
C20 C19 C21 C13 -42.6(7)
C18 C19 C21 C13 142.1(6)
C14 C13 C21 C19 40.0(7)
C12 C13 C21 C19 -139.5(6)
C14 C13 C21 C22 -77.2(7)
C12 C13 C21 C22 103.2(7)
C14 C13 C21 C23 162.8(6)
C12 C13 C21 C23 -16.7(9)
