# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2002

data_1 

_database_code_CSD	192733


_audit_creation_method            SHELXL-97 

_journal_coden_Cambridge      182

loop_
_publ_author_name
_publ_author_address

'Marciniec, Bogdan'
;  
Department of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Poznan
Poland
; 
'Kubicki, Maciej'
;  
Department of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Poznan
Poland
;
'Kownacki, Ireneusz'
;  
Department of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Poznan
Poland
;

_publ_contact_author_name     	'Dr Bogdan Marciniec'  
_publ_contact_author_address 
;
Faculty of Chemistry
Adam Mickiewicz University
60-780 Poznan
POLAND
;

_publ_contact_author_email       'MARCINB@MAIN.AMU.EDU.PL'

_publ_requested_journal           'Chemical Communications'

_publ_section_title
;
Alkoxy/ siloxy group exchange in the system
vinyltrialkoxysilane - iridium(I)siloxide complex
;

_chemical_name_systematic 
; 
bis-(1,5-cyclooctadiene)-di-\m-(ethoxy)diirydium (I)
; 

_chemical_formula_sum             'C20 H34 Ir2 O2' 
_chemical_formula_weight          690.87 

_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    'P2/n' 

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-x+1/2, y, -z+1/2' 
'-x, -y, -z' 
'x-1/2, -y, z-1/2' 

_cell_length_a                    12.5233(9) 
_cell_length_b                    6.4252(4) 
_cell_length_c                    12.5949(9) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.558(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      1011.49(12) 
_cell_formula_units_Z             2 

_exptl_crystal_density_diffrn     2.268 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_wavelength      0.71073 
_cell_measurement_reflns_used     650
_cell_measurement_theta_min       4
_cell_measurement_theta_max       17
_diffrn_ambient_temperature       293(2) 
_exptl_crystal_F_000              648 
_exptl_absorpt_coefficient_mu     13.152 
_exptl_crystal_description        block
_exptl_crystal_size_max           0.3 
_exptl_crystal_size_mid           0.2 
_exptl_crystal_size_min           0.2 
_exptl_crystal_colour             colourless
_diffrn_measurement_device_type   
;
four-circle diffractometer  with CCD detector
;
_diffrn_measurement_method        \w-scan 
_exptl_absorpt_correction_type    'psi-scan' 
_exptl_absorpt_correction_T_min   0.14 
_exptl_absorpt_correction_T_max   0.20 
_exptl_absorpt_process_details    ? 

_diffrn_radiation_monochromator   graphite 
_diffrn_reflns_number             7276
_reflns_number_total              1758
_diffrn_reflns_theta_max          25.00 
_diffrn_reflns_av_R_equivalents   0.080 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -7 
_diffrn_reflns_limit_k_max        7 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 

_computing_data_collection        'CrysAlisCCD (Oxford Diffraction, 2001)' 
_computing_cell_refinement        'CrysAlisCCD (Oxford Diffraction, 2000)'
_computing_data_reduction         'CrysAlisRed (Oxford Diffraction, 2000)' 
_computing_structure_solution     
;
SHELXS-97 (G.M. Sheldrick, Acta Cryst A46 (1990), 467)
;
_computing_structure_refinement   
;
SHELXL-97 (Program for the Refinement of Crystal Structures. 
University of Göttingen, Germany (1997))
; 

_refine_special_details 
; 
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. 
; 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
'calc w==1/[\s^2^(Fo^2^)+(0.0300P)^2^+30.0000P] where P==(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     riding
_refine_ls_extinction_method      none 
_refine_ls_number_reflns          1758 
_refine_ls_number_parameters      109 
_refine_ls_number_restraints      24 
_refine_ls_R_factor_all           0.0580 
_refine_ls_R_factor_gt            0.0555 
_refine_ls_wR_factor_ref          0.1319 
_refine_ls_wR_factor_gt           0.1303 
_refine_ls_goodness_of_fit_ref    1.132 
_refine_ls_restrained_S_all       1.131 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 

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_symetry_multiplicity 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
Ir1 Ir 0.25515(4) 0.88456(8) 0.13547(4) 0.0324(2) Uani 1 1 d . . . 
O1 O 0.1491(7) 0.7615(15) 0.2390(8) 0.036(2) Uani 1 1 d . . . 
C11 C 0.0338(12) 0.761(3) 0.2250(16) 0.054(4) Uani 1 1 d . . . 
H11A H 0.0117 0.8071 0.1537 0.064 Uiso 1 1 d R . . 
H11B H 0.0042 0.8559 0.2752 0.064 Uiso 1 1 d R . . 
C12 C -0.008(2) 0.550(4) 0.244(2) 0.086(7) Uani 1 1 d U . . 
H12A H -0.0846 0.5506 0.2337 0.104 Uiso 1 1 d R . . 
H12B H 0.0121 0.5060 0.3156 0.104 Uiso 1 1 d R . . 
H12C H 0.0215 0.4559 0.1947 0.104 Uiso 1 1 d R . . 
C1 C 0.3659(13) 1.091(2) 0.0783(15) 0.051(4) Uani 1 1 d . . . 
H1 H 0.3921 1.0967 0.1490 0.061 Uiso 1 1 d R . . 
C2 C 0.3721(13) 0.906(3) 0.0234(13) 0.046(4) Uani 1 1 d . . . 
H2 H 0.4074 0.7961 0.0582 0.055 Uiso 1 1 d R . . 
C3 C 0.3266(19) 0.871(4) -0.0874(19) 0.081(6) Uani 1 1 d U . . 
H3A H 0.3584 0.9711 -0.1337 0.098 Uiso 1 1 d R . . 
H3B H 0.3478 0.7335 -0.1099 0.098 Uiso 1 1 d R . . 
C4 C 0.2144(17) 0.885(4) -0.1040(13) 0.068(6) Uani 1 1 d . . . 
H4A H 0.1886 0.7635 -0.1434 0.081 Uiso 1 1 d R . . 
H4B H 0.1978 1.0059 -0.1481 0.081 Uiso 1 1 d R . . 
C5 C 0.1507(11) 0.906(3) 0.0000(12) 0.046(4) Uani 1 1 d . . . 
H5 H 0.1147 0.7900 0.0240 0.055 Uiso 1 1 d R . . 
C6 C 0.1477(14) 1.091(3) 0.0553(16) 0.056(4) Uani 1 1 d . . . 
H6 H 0.1081 1.0924 0.1153 0.067 Uiso 1 1 d R . . 
C7 C 0.2011(17) 1.291(4) 0.028(2) 0.077(6) Uani 1 1 d U . . 
H7A H 0.1721 1.3331 -0.0414 0.093 Uiso 1 1 d R . . 
H7B H 0.1816 1.3969 0.0784 0.093 Uiso 1 1 d R . . 
C8 C 0.3174(16) 1.289(3) 0.0263(19) 0.069(5) Uani 1 1 d U . . 
H8A H 0.3461 1.4106 0.0639 0.083 Uiso 1 1 d R . . 
H8B H 0.3373 1.2978 -0.0468 0.083 Uiso 1 1 d R . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Ir1 0.0282(3) 0.0321(3) 0.0363(4) -0.0011(2) -0.0019(2) -0.0007(2) 
O1 0.031(5) 0.041(5) 0.035(5) 0.003(4) -0.007(4) 0.002(4) 
C11 0.028(7) 0.062(10) 0.070(12) -0.003(9) -0.005(8) -0.005(7) 
C12 0.078(10) 0.081(9) 0.099(10) 0.004(8) 0.000(8) -0.015(8) 
C1 0.039(8) 0.046(9) 0.066(11) 0.012(8) -0.004(8) -0.002(7) 
C2 0.042(8) 0.054(9) 0.044(9) 0.009(7) 0.011(7) 0.005(7) 
C3 0.077(9) 0.091(10) 0.077(9) 0.004(8) 0.008(8) 0.007(8) 
C4 0.084(14) 0.096(15) 0.024(8) -0.016(9) 0.005(8) -0.009(12) 
C5 0.021(6) 0.078(11) 0.039(8) 0.006(8) 0.002(6) 0.002(7) 
C6 0.049(10) 0.052(10) 0.065(12) 0.011(9) -0.008(8) 0.009(8) 
C7 0.072(9) 0.069(9) 0.092(10) 0.029(8) 0.007(8) -0.001(7) 
C8 0.064(8) 0.062(8) 0.082(9) 0.013(7) 0.004(7) 0.005(7) 

_geom_special_details 
; 
All esds (except the esd in the dihedral angle between two l.s. planes) 
are estimated using the full covariance matrix.  The cell esds are taken 
into account individually in the estimation of esds in distances, angles 
and torsion angles; correlations between esds in cell parameters are only 
used when they are defined by crystal symmetry.  An approximate (isotropic) 
treatment of cell esds is used for estimating esds involving l.s. planes. 
; 

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 
Ir1 O1 2.075(10) . ? 
Ir1 O1 2.080(9) 2 ? 
Ir1 Ir1 2.8958(11) 2 ? 
O1 C11 1.444(17) . ? 
O1 Ir1 2.080(9) 2 ? 
C11 C12 1.48(3) . ? 
C1 C2 1.37(2) . ? 
C1 C8 1.54(2) . ? 
C2 C3 1.49(3) . ? 
C3 C4 1.41(3) . ? 
C4 C5 1.58(2) . ? 
C5 C6 1.38(2) . ? 
C6 C7 1.50(3) . ? 
C7 C8 1.46(3) . ? 

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 
O1 Ir1 O1 74.9(4) . 2 ? 
O1 Ir1 Ir1 45.9(3) . 2 ? 
O1 Ir1 Ir1 45.7(3) 2 2 ? 
C11 O1 Ir1 126.8(10) . . ? 
C11 O1 Ir1 128.3(10) . 2 ? 
Ir1 O1 Ir1 88.4(4) . 2 ? 
O1 C11 C12 110.2(16) . . ? 
C2 C1 C8 122.1(17) . . ? 
C1 C2 C3 124.8(17) . . ? 
C4 C3 C2 116.6(18) . . ? 
C3 C4 C5 115.6(15) . . ? 
C6 C5 C4 121.5(16) . . ? 
C5 C6 C7 126.8(19) . . ? 
C8 C7 C6 117.4(17) . . ? 
C7 C8 C1 111.4(16) . . ? 

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 
O1 Ir1 O1 C11 -179.3(11) 2 . . . ? 
Ir1 Ir1 O1 C11 138.8(13) 2 . . . ? 
O1 Ir1 O1 Ir1 41.9(4) 2 . . 2 ? 
Ir1 O1 C11 C12 131.0(15) . . . . ? 
Ir1 O1 C11 C12 -106.0(17) 2 . . . ? 
C8 C1 C2 C3 -5(3) . . . . ? 
C1 C2 C3 C4 -64(3) . . . . ? 
C2 C3 C4 C5 -8(3) . . . . ? 
C3 C4 C5 C6 76(2) . . . . ? 
C4 C5 C6 C7 0(3) . . . . ? 
C5 C6 C7 C8 -61(3) . . . . ? 
C6 C7 C8 C1 -13(3) . . . . ? 
C2 C1 C8 C7 83(2) . . . . ? 

_diffrn_measured_fraction_theta_max    0.985 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.985 
_refine_diff_density_max    3.716 
_refine_diff_density_min   -2.199 
_refine_diff_density_rms    0.299