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#$Date: 2016-03-21 08:10:55 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178598 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/09/4070996.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_4070996
loop_
_publ_author_name
'Okazaki, Masaaki'
'Yamahira, Nobukazu'
'Minglana, Jim Josephus Gabrillo'
'Komuro, Takashi'
'Ogino, Hiroshi'
'Tobita, Hiromi'
_publ_section_title
;
 [Ru(xantsil)(CO)(η6-toluene)]: Synthon for a Highly Unsaturated
 Ruthenium(II) Complex through Facile Dissociation of the Toluene Ligand
 [xantsil = (9,9-dimethylxanthene-4,5-diyl)bis(dimethylsilyl)]
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              918
_journal_paper_doi               10.1021/om701194e
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C28 H36 N4 O2 Ru Si2'
_chemical_formula_sum            'C28 H36 N4 O2 Ru Si2'
_chemical_formula_weight         617.86
_chemical_name_common            'complex 2'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.3683(7)
_cell_length_b                   14.0012(3)
_cell_length_c                   9.5533(2)
_cell_measurement_reflns_used    27150
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.94
_cell_measurement_theta_min      3.43
_cell_volume                     2991.93(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21810
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.82
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.9392
_exptl_absorpt_correction_T_min  0.7853
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   Higashi
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.442
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0260P)²+2.3928P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                3241
_reflns_number_total             3355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701194e-file003.cif
_cod_data_source_block           2/CH3CN
_cod_database_code               4070996
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
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
Ru1 Ru 0.910916(8) 0.2500 0.097287(18) 0.01744(7) Uani 1 2 d S
Si1 Si 0.919136(19) 0.12265(3) 0.26372(5) 0.01858(10) Uani 1 1 d .
N1 N 0.89675(6) 0.14384(12) -0.06936(15) 0.0243(3) Uani 1 1 d .
N2 N 0.81658(9) 0.2500 0.1172(2) 0.0211(4) Uani 1 2 d S
O1 O 0.85239(7) 0.2500 0.44419(17) 0.0178(3) Uani 1 2 d S
C1 C 0.99176(12) 0.2500 0.1109(3) 0.0274(6) Uani 1 2 d S
O2 O 1.04341(8) 0.2500 0.1252(2) 0.0444(6) Uani 1 2 d S
C2 C 0.89007(8) 0.08942(14) -0.15602(18) 0.0252(4) Uani 1 1 d .
C3 C 0.88173(10) 0.01854(17) -0.2662(2) 0.0384(5) Uani 1 1 d .
H1 H 0.8928 -0.0447 -0.2307 0.058 Uiso 1 1 calc R
H2 H 0.9070 0.0347 -0.3465 0.058 Uiso 1 1 calc R
H3 H 0.8397 0.0180 -0.2953 0.058 Uiso 1 1 calc R
C4 C 0.76659(11) 0.2500 0.1377(3) 0.0264(5) Uani 1 2 d S
C5 C 0.70283(13) 0.2500 0.1681(4) 0.0542(10) Uani 1 2 d S
H4 H 0.6808 0.2734 0.0862 0.081 Uiso 0.50 1 calc PR
H5 H 0.6949 0.2918 0.2482 0.081 Uiso 0.50 1 calc PR
H6 H 0.6898 0.1849 0.1901 0.081 Uiso 0.50 1 calc PR
C6 C 0.97596(8) 0.12914(15) 0.41006(18) 0.0282(4) Uani 1 1 d .
H7 H 0.9821 0.0652 0.4492 0.042 Uiso 1 1 calc R
H8 H 0.9613 0.1720 0.4835 0.042 Uiso 1 1 calc R
H9 H 1.0139 0.1536 0.3733 0.042 Uiso 1 1 calc R
C7 C 0.93940(9) 0.00535(14) 0.1767(2) 0.0294(4) Uani 1 1 d .
H10 H 0.9775 0.0124 0.1269 0.044 Uiso 1 1 calc R
H11 H 0.9080 -0.0124 0.1100 0.044 Uiso 1 1 calc R
H12 H 0.9432 -0.0446 0.2480 0.044 Uiso 1 1 calc R
C8 C 0.84669(7) 0.09308(13) 0.36186(16) 0.0190(3) Uani 1 1 d .
C9 C 0.81636(8) 0.00607(13) 0.36327(18) 0.0238(4) Uani 1 1 d .
H13 H 0.8331 -0.0472 0.3157 0.029 Uiso 1 1 calc R
C10 C 0.76199(8) -0.00430(14) 0.43303(19) 0.0279(4) Uani 1 1 d .
H14 H 0.7427 -0.0648 0.4346 0.033 Uiso 1 1 calc R
C11 C 0.73580(8) 0.07293(13) 0.50006(18) 0.0246(4) Uani 1 1 d .
H15 H 0.6981 0.0654 0.5443 0.029 Uiso 1 1 calc R
C12 C 0.76421(7) 0.16156(12) 0.50327(16) 0.0183(3) Uani 1 1 d .
C13 C 0.81964(7) 0.16633(12) 0.43756(16) 0.0168(3) Uani 1 1 d .
C14 C 0.74007(10) 0.2500 0.5781(2) 0.0191(5) Uani 1 2 d S
C15 C 0.76350(13) 0.2500 0.7297(2) 0.0270(5) Uani 1 2 d S
H16 H 0.7538 0.3111 0.7744 0.041 Uiso 0.50 1 calc PR
H17 H 0.8070 0.2411 0.7293 0.041 Uiso 0.50 1 calc PR
H18 H 0.7447 0.1978 0.7820 0.041 Uiso 0.50 1 calc PR
C16 C 0.67154(11) 0.2500 0.5803(3) 0.0303(6) Uani 1 2 d S
H19 H 0.6574 0.2138 0.6616 0.045 Uiso 0.50 1 calc PR
H20 H 0.6564 0.2203 0.4944 0.045 Uiso 0.50 1 calc PR
H21 H 0.6570 0.3159 0.5862 0.045 Uiso 0.50 1 calc PR
N3 N 0.89342(14) -0.2500 0.4134(3) 0.0664(11) Uani 1 2 d S
C17 C 0.93239(13) -0.2500 0.3391(3) 0.0350(7) Uani 1 2 d S
C18 C 0.98110(13) -0.2500 0.2401(3) 0.0329(6) Uani 1 2 d S
H22 H 0.9896 -0.3157 0.2107 0.049 Uiso 0.50 1 calc PR
H23 H 1.0168 -0.2226 0.2841 0.049 Uiso 0.50 1 calc PR
H24 H 0.9701 -0.2117 0.1581 0.049 Uiso 0.50 1 calc PR
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'
N N 0.0061 0.0033 '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'
Ru Ru -1.2594 0.8363 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 Ru1 N2 170.73(9) . .
C1 Ru1 N1 101.28(7) . .
N2 Ru1 N1 85.50(5) . .
C1 Ru1 N1 101.28(7) . 8_565
N2 Ru1 N1 85.50(5) . 8_565
N1 Ru1 N1 84.96(8) . 8_565
C1 Ru1 Si1 82.87(5) . 8_565
N2 Ru1 Si1 90.97(4) . 8_565
N1 Ru1 Si1 173.51(4) . 8_565
N1 Ru1 Si1 89.34(4) 8_565 8_565
C1 Ru1 Si1 82.87(5) . .
N2 Ru1 Si1 90.97(4) . .
N1 Ru1 Si1 89.34(4) . .
N1 Ru1 Si1 173.51(4) 8_565 .
Si1 Ru1 Si1 96.17(2) 8_565 .
C6 Si1 C7 101.84(9) . .
C6 Si1 C8 102.52(8) . .
C7 Si1 C8 103.27(8) . .
C6 Si1 Ru1 120.41(7) . .
C7 Si1 Ru1 111.83(6) . .
C8 Si1 Ru1 114.85(5) . .
C2 N1 Ru1 179.18(15) . .
C4 N2 Ru1 175.2(2) . .
C13 O1 C13 115.77(17) . 8_565
O2 C1 Ru1 177.4(2) . .
N1 C2 C3 179.3(2) . .
N2 C4 C5 178.4(3) . .
C13 C8 C9 115.26(14) . .
C13 C8 Si1 117.51(13) . .
C9 C8 Si1 127.20(13) . .
C10 C9 C8 121.33(16) . .
C11 C10 C9 120.53(17) . .
C10 C11 C12 120.77(15) . .
C13 C12 C11 116.03(15) . .
C13 C12 C14 119.15(15) . .
C11 C12 C14 124.77(15) . .
O1 C13 C12 119.47(15) . .
O1 C13 C8 114.66(14) . .
C12 C13 C8 125.87(15) . .
C12 C14 C12 108.23(18) . 8_565
C12 C14 C16 111.08(13) . .
C12 C14 C16 111.08(13) 8_565 .
C12 C14 C15 108.64(13) . .
C12 C14 C15 108.64(13) 8_565 .
C16 C14 C15 109.1(2) . .
N3 C17 C18 178.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 C1 1.813(3) .
Ru1 N2 2.119(2) .
Ru1 N1 2.2010(16) .
Ru1 N1 2.2010(16) 8_565
Ru1 Si1 2.3960(5) 8_565
Ru1 Si1 2.3960(5) .
Si1 C6 1.8916(18) .
Si1 C7 1.8958(19) .
Si1 C8 1.9175(17) .
N1 C2 1.135(2) .
N2 C4 1.135(3) .
O1 C13 1.3832(18) .
O1 C13 1.3832(18) 8_565
C1 O2 1.163(3) .
C2 C3 1.458(3) .
C4 C5 1.455(4) .
C8 C13 1.393(2) .
C8 C9 1.394(2) .
C9 C10 1.394(2) .
C10 C11 1.387(3) .
C11 C12 1.395(2) .
C12 C13 1.391(2) .
C12 C14 1.528(2) .
C14 C12 1.528(2) 8_565
C14 C16 1.533(3) .
C14 C15 1.541(3) .
N3 C17 1.124(4) .
C17 C18 1.443(4) .
