#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:49:11 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180156 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/52/7105221.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_7105221
loop_
_publ_author_name
'Komuro, Takashi'
'Tobita, Hiromi'
_publ_section_title
;
 Thermal reaction of a ruthenium bis(silyl) complex having a
 lutidine-based Si,N,Si ligand: formation of a mu-silyl(mu-silylene)
 diruthenium complex involving a 3c-2e Ru-Si-C interaction.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1136
_journal_page_last               1137
_journal_paper_doi               10.1039/b915395k
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C14 H19 N O3 Ru Si2'
_chemical_formula_sum            'C14 H19 N O3 Ru Si2'
_chemical_formula_weight         406.55
_chemical_name_systematic
;
?
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.361(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1593(4)
_cell_length_b                   20.5715(15)
_cell_length_c                   12.3613(13)
_cell_measurement_reflns_used    18995
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.6
_cell_volume                     1763.7(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13609
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  0.9697
_exptl_absorpt_correction_T_min  0.7824
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
HIGASHI, T. (1999). Shape - Program to obtain Crystal Shape using CCD camera.
Rigaku Corporation, Tokyo, Japan.
HIGASHI, T. (1999). Numabs - Numerical Absorption Correction,
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            lemon-yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0268P)²+2.4876P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                3400
_reflns_number_total             3918
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b915395k.txt
_cod_data_source_block           complex1
_cod_database_code               7105221
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.23497(3) 0.132090(10) 0.297547(18) 0.01483(7) Uani 1 1 d . . .
Si1 Si 0.22834(11) 0.24854(4) 0.25610(7) 0.01876(16) Uani 1 1 d . . .
Si2 Si 0.28698(11) 0.01513(4) 0.28681(6) 0.01871(16) Uani 1 1 d . . .
O1 O 0.6672(3) 0.15183(13) 0.4180(2) 0.0382(6) Uani 1 1 d . . .
O2 O 0.1183(3) 0.13555(12) 0.51830(18) 0.0308(5) Uani 1 1 d . . .
O3 O -0.1951(3) 0.11287(14) 0.1736(2) 0.0435(6) Uani 1 1 d . . .
N1 N 0.3070(3) 0.12756(11) 0.13426(19) 0.0185(5) Uani 1 1 d . . .
C1 C 0.3394(5) 0.30866(14) 0.3708(3) 0.0265(6) Uani 1 1 d . . .
H1 H 0.3469 0.3516 0.3379 0.040 Uiso 1 1 calc R . .
H2 H 0.4693 0.2941 0.4092 0.040 Uiso 1 1 calc R . .
H3 H 0.2593 0.3112 0.4244 0.040 Uiso 1 1 calc R . .
C2 C -0.0087(5) 0.28358(15) 0.1713(3) 0.0290(7) Uani 1 1 d . . .
H4 H -0.1046 0.2822 0.2157 0.043 Uiso 1 1 calc R . .
H5 H -0.0548 0.2579 0.1031 0.043 Uiso 1 1 calc R . .
H6 H 0.0110 0.3287 0.1514 0.043 Uiso 1 1 calc R . .
C3 C 0.3991(4) 0.24313(14) 0.1590(3) 0.0257(6) Uani 1 1 d . . .
H7 H 0.3803 0.2817 0.1097 0.031 Uiso 1 1 calc R . .
H8 H 0.5341 0.2435 0.2045 0.031 Uiso 1 1 calc R . .
C4 C 0.3653(4) 0.18272(14) 0.0888(2) 0.0207(6) Uani 1 1 d . . .
C5 C 0.3953(4) 0.18146(16) -0.0193(3) 0.0273(7) Uani 1 1 d . . .
H9 H 0.4309 0.2202 -0.0511 0.033 Uiso 1 1 calc R . .
C6 C 0.3733(5) 0.12386(16) -0.0799(3) 0.0303(7) Uani 1 1 d . . .
H10 H 0.3943 0.1227 -0.1528 0.036 Uiso 1 1 calc R . .
C7 C 0.3204(4) 0.06843(15) -0.0323(2) 0.0250(6) Uani 1 1 d . . .
H11 H 0.3078 0.0284 -0.0719 0.030 Uiso 1 1 calc R . .
C8 C 0.2850(4) 0.07072(14) 0.0744(2) 0.0194(6) Uani 1 1 d . . .
C9 C 0.2188(4) 0.01123(14) 0.1254(2) 0.0237(6) Uani 1 1 d . . .
H12 H 0.2780 -0.0279 0.1010 0.028 Uiso 1 1 calc R . .
H13 H 0.0771 0.0071 0.0981 0.028 Uiso 1 1 calc R . .
C10 C 0.1255(5) -0.04286(15) 0.3399(3) 0.0303(7) Uani 1 1 d . . .
H14 H 0.1573 -0.0877 0.3243 0.046 Uiso 1 1 calc R . .
H15 H -0.0095 -0.0339 0.3023 0.046 Uiso 1 1 calc R . .
H16 H 0.1448 -0.0371 0.4206 0.046 Uiso 1 1 calc R . .
C11 C 0.5455(4) -0.01422(15) 0.3373(3) 0.0287(7) Uani 1 1 d . . .
H17 H 0.5875 -0.0098 0.4187 0.043 Uiso 1 1 calc R . .
H18 H 0.6292 0.0119 0.3026 0.043 Uiso 1 1 calc R . .
H19 H 0.5533 -0.0600 0.3168 0.043 Uiso 1 1 calc R . .
C12 C 0.5064(4) 0.14430(14) 0.3738(2) 0.0224(6) Uani 1 1 d . . .
C13 C 0.1639(4) 0.13439(14) 0.4353(3) 0.0215(6) Uani 1 1 d . . .
C14 C -0.0363(4) 0.12038(14) 0.2192(3) 0.0233(6) Uani 1 1 d . . .
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
_geom_angle_publ_flag
C13 Ru1 C12 91.14(12) . . ?
C13 Ru1 C14 89.60(12) . . ?
C12 Ru1 C14 179.18(12) . . ?
C13 Ru1 N1 177.79(10) . . ?
C12 Ru1 N1 90.95(10) . . ?
C14 Ru1 N1 88.32(10) . . ?
C13 Ru1 Si2 98.74(9) . . ?
C12 Ru1 Si2 90.35(8) . . ?
C14 Ru1 Si2 89.87(9) . . ?
N1 Ru1 Si2 80.52(6) . . ?
C13 Ru1 Si1 99.67(9) . . ?
C12 Ru1 Si1 86.59(8) . . ?
C14 Ru1 Si1 92.95(9) . . ?
N1 Ru1 Si1 81.18(6) . . ?
Si2 Ru1 Si1 161.39(3) . . ?
C1 Si1 C2 108.39(14) . . ?
C1 Si1 C3 106.91(14) . . ?
C2 Si1 C3 107.32(14) . . ?
C1 Si1 Ru1 119.86(10) . . ?
C2 Si1 Ru1 117.05(11) . . ?
C3 Si1 Ru1 95.27(9) . . ?
C10 Si2 C11 108.40(15) . . ?
C10 Si2 C9 108.20(14) . . ?
C11 Si2 C9 107.58(14) . . ?
C10 Si2 Ru1 119.24(11) . . ?
C11 Si2 Ru1 116.39(10) . . ?
C9 Si2 Ru1 95.40(9) . . ?
C8 N1 C4 119.2(2) . . ?
C8 N1 Ru1 120.54(18) . . ?
C4 N1 Ru1 120.15(19) . . ?
Si1 C1 H1 109.5 . . ?
Si1 C1 H2 109.5 . . ?
H1 C1 H2 109.5 . . ?
Si1 C1 H3 109.5 . . ?
H1 C1 H3 109.5 . . ?
H2 C1 H3 109.5 . . ?
Si1 C2 H4 109.5 . . ?
Si1 C2 H5 109.5 . . ?
H4 C2 H5 109.5 . . ?
Si1 C2 H6 109.5 . . ?
H4 C2 H6 109.5 . . ?
H5 C2 H6 109.5 . . ?
C4 C3 Si1 111.9(2) . . ?
C4 C3 H7 109.2 . . ?
Si1 C3 H7 109.2 . . ?
C4 C3 H8 109.2 . . ?
Si1 C3 H8 109.2 . . ?
H7 C3 H8 107.9 . . ?
N1 C4 C5 120.4(3) . . ?
N1 C4 C3 117.9(2) . . ?
C5 C4 C3 121.6(3) . . ?
C6 C5 C4 120.3(3) . . ?
C6 C5 H9 119.9 . . ?
C4 C5 H9 119.9 . . ?
C7 C6 C5 118.8(3) . . ?
C7 C6 H10 120.6 . . ?
C5 C6 H10 120.6 . . ?
C6 C7 C8 120.4(3) . . ?
C6 C7 H11 119.8 . . ?
C8 C7 H11 119.8 . . ?
N1 C8 C7 120.8(3) . . ?
N1 C8 C9 118.2(2) . . ?
C7 C8 C9 121.0(3) . . ?
C8 C9 Si2 111.89(19) . . ?
C8 C9 H12 109.2 . . ?
Si2 C9 H12 109.2 . . ?
C8 C9 H13 109.2 . . ?
Si2 C9 H13 109.2 . . ?
H12 C9 H13 107.9 . . ?
Si2 C10 H14 109.5 . . ?
Si2 C10 H15 109.5 . . ?
H14 C10 H15 109.5 . . ?
Si2 C10 H16 109.5 . . ?
H14 C10 H16 109.5 . . ?
H15 C10 H16 109.5 . . ?
Si2 C11 H17 109.5 . . ?
Si2 C11 H18 109.5 . . ?
H17 C11 H18 109.5 . . ?
Si2 C11 H19 109.5 . . ?
H17 C11 H19 109.5 . . ?
H18 C11 H19 109.5 . . ?
O1 C12 Ru1 179.3(3) . . ?
O2 C13 Ru1 179.1(3) . . ?
O3 C14 Ru1 179.3(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C13 1.895(3) . ?
Ru1 C12 1.954(3) . ?
Ru1 C14 1.958(3) . ?
Ru1 N1 2.206(2) . ?
Ru1 Si2 2.4432(8) . ?
Ru1 Si1 2.4477(8) . ?
Si1 C1 1.901(3) . ?
Si1 C2 1.902(3) . ?
Si1 C3 1.917(3) . ?
Si2 C10 1.888(3) . ?
Si2 C11 1.899(3) . ?
Si2 C9 1.935(3) . ?
O1 C12 1.156(4) . ?
O2 C13 1.152(4) . ?
O3 C14 1.147(4) . ?
N1 C8 1.372(4) . ?
N1 C4 1.376(4) . ?
C1 H1 0.9800 . ?
C1 H2 0.9800 . ?
C1 H3 0.9800 . ?
C2 H4 0.9800 . ?
C2 H5 0.9800 . ?
C2 H6 0.9800 . ?
C3 C4 1.501(4) . ?
C3 H7 0.9900 . ?
C3 H8 0.9900 . ?
C4 C5 1.405(4) . ?
C5 C6 1.390(5) . ?
C5 H9 0.9500 . ?
C6 C7 1.378(4) . ?
C6 H10 0.9500 . ?
C7 C8 1.404(4) . ?
C7 H11 0.9500 . ?
C8 C9 1.506(4) . ?
C9 H12 0.9900 . ?
C9 H13 0.9900 . ?
C10 H14 0.9800 . ?
C10 H15 0.9800 . ?
C10 H16 0.9800 . ?
C11 H17 0.9800 . ?
C11 H18 0.9800 . ?
C11 H19 0.9800 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 Ru1 Si1 C1 44.06(15) . . . . ?
C12 Ru1 Si1 C1 -46.52(14) . . . . ?
C14 Ru1 Si1 C1 134.16(15) . . . . ?
N1 Ru1 Si1 C1 -138.01(13) . . . . ?
Si2 Ru1 Si1 C1 -127.43(14) . . . . ?
C13 Ru1 Si1 C2 -90.49(14) . . . . ?
C12 Ru1 Si1 C2 178.93(14) . . . . ?
C14 Ru1 Si1 C2 -0.39(14) . . . . ?
N1 Ru1 Si1 C2 87.44(13) . . . . ?
Si2 Ru1 Si1 C2 98.01(14) . . . . ?
C13 Ru1 Si1 C3 157.00(13) . . . . ?
C12 Ru1 Si1 C3 66.42(13) . . . . ?
C14 Ru1 Si1 C3 -112.90(13) . . . . ?
N1 Ru1 Si1 C3 -25.06(12) . . . . ?
Si2 Ru1 Si1 C3 -14.49(14) . . . . ?
C13 Ru1 Si2 C10 36.35(15) . . . . ?
C12 Ru1 Si2 C10 127.56(15) . . . . ?
C14 Ru1 Si2 C10 -53.23(15) . . . . ?
N1 Ru1 Si2 C10 -141.54(14) . . . . ?
Si1 Ru1 Si2 C10 -152.13(14) . . . . ?
C13 Ru1 Si2 C11 -96.62(14) . . . . ?
C12 Ru1 Si2 C11 -5.41(14) . . . . ?
C14 Ru1 Si2 C11 173.80(14) . . . . ?
N1 Ru1 Si2 C11 85.49(13) . . . . ?
Si1 Ru1 Si2 C11 74.90(15) . . . . ?
C13 Ru1 Si2 C9 150.71(13) . . . . ?
C12 Ru1 Si2 C9 -118.08(13) . . . . ?
C14 Ru1 Si2 C9 61.13(13) . . . . ?
N1 Ru1 Si2 C9 -27.18(11) . . . . ?
Si1 Ru1 Si2 C9 -37.77(14) . . . . ?
C12 Ru1 N1 C8 112.4(2) . . . . ?
C14 Ru1 N1 C8 -67.9(2) . . . . ?
Si2 Ru1 N1 C8 22.25(19) . . . . ?
Si1 Ru1 N1 C8 -161.2(2) . . . . ?
C12 Ru1 N1 C4 -70.9(2) . . . . ?
C14 Ru1 N1 C4 108.8(2) . . . . ?
Si2 Ru1 N1 C4 -161.1(2) . . . . ?
Si1 Ru1 N1 C4 15.52(19) . . . . ?
C1 Si1 C3 C4 161.0(2) . . . . ?
C2 Si1 C3 C4 -82.9(2) . . . . ?
Ru1 Si1 C3 C4 37.6(2) . . . . ?
C8 N1 C4 C5 2.2(4) . . . . ?
Ru1 N1 C4 C5 -174.5(2) . . . . ?
C8 N1 C4 C3 -176.5(2) . . . . ?
Ru1 N1 C4 C3 6.8(3) . . . . ?
Si1 C3 C4 N1 -32.9(3) . . . . ?
Si1 C3 C4 C5 148.3(2) . . . . ?
N1 C4 C5 C6 -2.4(4) . . . . ?
C3 C4 C5 C6 176.4(3) . . . . ?
C4 C5 C6 C7 0.4(5) . . . . ?
C5 C6 C7 C8 1.5(5) . . . . ?
C4 N1 C8 C7 -0.3(4) . . . . ?
Ru1 N1 C8 C7 176.4(2) . . . . ?
C4 N1 C8 C9 -179.3(2) . . . . ?
Ru1 N1 C8 C9 -2.6(3) . . . . ?
C6 C7 C8 N1 -1.7(4) . . . . ?
C6 C7 C8 C9 177.3(3) . . . . ?
N1 C8 C9 Si2 -26.2(3) . . . . ?
C7 C8 C9 Si2 154.8(2) . . . . ?
C10 Si2 C9 C8 159.5(2) . . . . ?
C11 Si2 C9 C8 -83.6(2) . . . . ?
Ru1 Si2 C9 C8 36.3(2) . . . . ?
