# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/2215

data_global

_publ_section_title
;
A new two-strand chain cluster: the synthesis and characterisation of 
[Os3(CO)11{mu3-eta4-(C4H3S)C2C2(C4H3S)]
;

_publ_requested_journal  'J.Chem.Soc.,Dalton Trans.'

loop_
_publ_author_name
'Adams, Christopher J.'
'Clarke, Lionel P.'
'Martin-Castro, Ana M.'
'Raithby, Paul R.'
'Shields, Gregory P.'


data_lpc274b

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C23 H6 O11 Os3 S2'
_chemical_formula_weight          1093.00
_chemical_melting_point           ?
_chemical_compound_source         ?

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'
 'S'  'S'   0.1246   0.1234
 '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'

_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/n

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'

_cell_length_a                    7.071(4)
_cell_length_b                    21.964(12)
_cell_length_c                    16.564(10)
_cell_angle_alpha                 90.00
_cell_angle_beta                  96.15(4)
_cell_angle_gamma                 90.00
_cell_volume                      2557.7(25)
_cell_formula_units_Z             4
_cell_measurement_temperature     195(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        Block
_exptl_crystal_colour             Red
_exptl_crystal_size_max           0.57
_exptl_crystal_size_mid           0.53
_exptl_crystal_size_min           0.46
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.838
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              1968
_exptl_absorpt_coefficient_mu     15.090
_exptl_absorpt_correction_type    psi-scan
_exptl_absorpt_correction_T_min   0.155
_exptl_absorpt_correction_T_max   1.000

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       195(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device        'Stoe-Siemens'
_diffrn_measurement_method        'omega/theta scans'
_diffrn_standards_number          3
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   '60 minutes'
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             6205
_diffrn_reflns_av_R_equivalents   0.0749
_diffrn_reflns_av_sigmaI/netI     0.0429
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        26
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          3.55
_diffrn_reflns_theta_max          25.00
_reflns_number_total              4495
_reflns_number_observed           3972
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        'Stoe DIF4'
_computing_cell_refinement        'Stoe DIF4'
_computing_data_reduction         'Stoe REDU4'
_computing_structure_solution     'SIR92'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     'SHELXTL-PLUS (Siemens, 1991)'
_computing_publication_material   'SHELXL-93 (Sheldrick, 1993)'

_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 4 with very negative
F^2^
 or flagged by the user for potential systematic errors.  Weighted
R-factors
 wR and all goodnesses 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 observed
criterion
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1212P)^2^+41.8320P] 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     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          4491
_refine_ls_number_parameters      243
_refine_ls_number_restraints      24
_refine_ls_R_factor_all           0.0693
_refine_ls_R_factor_obs           0.0626
_refine_ls_wR_factor_all          0.1766
_refine_ls_wR_factor_obs          0.1665
_refine_ls_goodness_of_fit_all    1.059
_refine_ls_goodness_of_fit_obs    1.069
_refine_ls_restrained_S_all       1.062
_refine_ls_restrained_S_obs       1.066
_refine_ls_shift/esd_max          0.000
_refine_ls_shift/esd_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_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
Os1 Os 1.00962(8) -0.12381(2) 0.24350(3) 0.0228(2) Uani 1 d . .
C1 C 1.1038(22) -0.0634(6) 0.1563(9) 0.025(3) Uiso 1 d . .
S1 S 1.2498(9) -0.0187(3) 0.0194(3) 0.043(2) Uiso 0.78(2) d PD 1
S1A S 1.2126(23) -0.1466(8) 0.0537(9) 0.043(2) Uiso 0.22(2) d PD 2
Os2 Os 0.96511(8) -0.00264(2) 0.30936(3) 0.0189(2) Uani 1 d . .
C2 C 1.0838(23) -0.0077(7) 0.1840(9) 0.026(3) Uiso 1 d . .
S2 S 1.0422(9) 0.2282(3) 0.1547(4) 0.044(2) Uiso 0.78(2) d PD 3
S2A S 1.2325(24) 0.1327(8) 0.0764(9) 0.044(2) Uiso 0.22(2) d PD 4
Os3 Os 0.95852(8) 0.12897(2) 0.32928(3) 0.0213(2) Uani 1 d . .
C3 C 1.0723(20) 0.0520(6) 0.2033(8) 0.021(3) Uiso 1 d . .
C4 C 1.0660(20) 0.1101(6) 0.2162(8) 0.020(3) Uiso 1 d . .
C5 C 1.1815(18) -0.0741(5) 0.0804(7) 0.027(3) Uiso 1 d D .
C6 C 1.2186(19) -0.1343(8) 0.0459(8) 0.016(4) Uiso 0.78(2) d PD 1
H6A H 1.1927(19) -0.1726(8) 0.0691(8) 0.019 Uiso 0.78(2) calc PR 1
C6A C 1.2466(27) -0.0332(13) 0.0185(9) 0.016(4) Uiso 0.22(2) d PD 2
H6AA H 1.2423(27) 0.0100(13) 0.0201(9) 0.019 Uiso 0.22(2) calc PR 2
C7 C 1.3026(21) -0.1248(8) -0.0306(8) 0.044(4) Uiso 1 d D .
H7A H 1.3397(21) -0.1568(8) -0.0640(8) 0.053 Uiso 1 calc R 1
C8 C 1.3196(22) -0.0694(7) -0.0465(9) 0.046(4) Uiso 1 d D .
H8A H 1.3705(22) -0.0566(7) -0.0945(9) 0.055 Uiso 1 calc R 1
C9 C 1.1136(17) 0.1556(5) 0.1528(7) 0.028(3) Uiso 1 d D .
C10 C 1.2177(21) 0.1450(9) 0.0820(8) 0.025(5) Uiso 0.78(2) d PD 3
H10B H 1.2723(21) 0.1074(9) 0.0682(8) 0.030 Uiso 0.78(2) calc PR 3
C10A C 1.0677(32) 0.2209(8) 0.1433(13) 0.025(5) Uiso 0.22(2) d PD 4
H10A H 1.0011(32) 0.2439(8) 0.1798(13) 0.030 Uiso 0.22(2) calc PR 4
C11 C 1.2237(23) 0.2021(7) 0.0359(11) 0.048(5) Uiso 1 d D .
H11A H 1.2827(23) 0.2063(7) -0.0127(11) 0.058 Uiso 1 calc R 3
C12 C 1.1390(21) 0.2457(9) 0.0698(8) 0.046(4) Uiso 1 d D .
H12A H 1.1319(21) 0.2857(9) 0.0477(8) 0.056 Uiso 1 calc R 3
C101 C 1.0375(26) -0.2031(9) 0.1950(11) 0.040(4) Uiso 1 d . .
O101 O 1.0451(26) -0.2491(6) 0.1685(10) 0.065(5) Uani 1 d . .
C102 C 1.2739(24) -0.1247(7) 0.2901(10) 0.029(3) Uiso 1 d . .
O102 O 1.4319(20) -0.1250(6) 0.3118(10) 0.052(4) Uani 1 d . .
C103 C 0.9067(22) -0.1577(7) 0.3396(9) 0.029(3) Uiso 1 d . .
O103 O 0.8519(23) -0.1755(7) 0.3963(9) 0.060(4) Uani 1 d . .
C104 C 0.7620(25) -0.1096(8) 0.1785(10) 0.034(4) Uiso 1 d . .
O104 O 0.6337(21) -0.1005(7) 0.1332(9) 0.057(4) Uani 1 d . .
C201 C 1.2214(22) -0.0069(6) 0.3602(9) 0.023(3) Uiso 1 d . .
O201 O 1.3743(19) -0.0090(6) 0.3921(8) 0.042(3) Uani 1 d . .
C202 C 0.8711(21) -0.0276(7) 0.4086(8) 0.024(3) Uiso 1 d . .
O202 O 0.8117(17) -0.0403(6) 0.4660(6) 0.041(3) Uani 1 d . .
C203 C 0.7067(23) 0.0020(6) 0.2601(9) 0.026(3) Uiso 1 d . .
O203 O 0.5512(17) 0.0040(5) 0.2323(8) 0.036(3) Uani 1 d . .
C301 C 0.9654(22) 0.2158(7) 0.3355(9) 0.029(3) Uiso 1 d . .
O301 O 0.9680(21) 0.2678(5) 0.3454(10) 0.055(4) Uani 1 d . .
C302 C 0.7082(25) 0.1329(7) 0.2672(10) 0.030(3) Uiso 1 d . .
O302 O 0.5710(19) 0.1371(7) 0.2278(9) 0.054(4) Uani 1 d . .
C303 C 1.2201(24) 0.1242(7) 0.3768(10) 0.028(3) Uiso 1 d . .
O303 O 1.3806(19) 0.1232(6) 0.4033(10) 0.050(4) Uani 1 d . .
C304 C 0.8539(23) 0.1160(7) 0.4338(10) 0.028(3) Uiso 1 d . .
O304 O 0.7973(18) 0.1096(6) 0.4919(7) 0.040(3) Uani 1 d . .

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
Os1 0.0245(4) 0.0149(3) 0.0286(3) 0.0019(2) 0.0008(3) -0.0013(2)
Os2 0.0204(3) 0.0180(3) 0.0179(3) 0.0019(2) 0.0010(2) 0.0004(2)
Os3 0.0214(4) 0.0181(3) 0.0235(3) -0.0022(2) -0.0012(2) 0.0016(2)
O101 0.103(14) 0.023(7) 0.073(10) -0.005(6) 0.021(10) -0.006(7)
O102 0.030(7) 0.049(9) 0.074(10) 0.003(6) -0.007(7) 0.007(6)
O103 0.064(10) 0.068(10) 0.049(8) 0.012(7) 0.010(7) -0.016(8)
O104 0.052(9) 0.047(8) 0.064(9) -0.007(7) -0.035(7) 0.002(7)
O201 0.038(7) 0.048(8) 0.037(7) -0.002(5) -0.002(6) 0.002(6)
O202 0.035(7) 0.065(8) 0.022(5) 0.013(5) 0.003(5) -0.006(6)
O203 0.024(6) 0.040(7) 0.042(7) 0.002(5) -0.003(5) 0.002(5)
O301 0.059(9) 0.018(6) 0.089(10) -0.016(6) 0.012(8) 0.004(6)
O302 0.026(7) 0.071(10) 0.061(9) -0.020(7) -0.020(6) 0.015(6)
O303 0.030(7) 0.051(9) 0.066(9) 0.016(6) -0.005(7) -0.007(6)
O304 0.036(7) 0.051(7) 0.034(6) 0.004(5) 0.006(5) 0.010(6)

_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
Os1 C101 1.94(2) . ?
Os1 C102 1.94(2) . ?
Os1 C103 1.97(2) . ?
Os1 C104 1.98(2) . ?
Os1 C1 2.121(14) . ?
Os1 Os2 2.906(2) . ?
C1 C2 1.32(2) . ?
C1 C5 1.44(2) . ?
S1 C8 1.671(11) . ?
S1 C5 1.685(10) . ?
S1A C7 1.666(13) . ?
S1A C5 1.674(13) . ?
Os2 C201 1.92(2) . ?
Os2 C202 1.918(14) . ?
Os2 C203 1.92(2) . ?
Os2 C3 2.321(13) . ?
Os2 C2 2.32(2) . ?
Os2 Os3 2.911(2) . ?
C2 C3 1.35(2) . ?
S2 C12 1.674(12) . ?
S2 C9 1.676(11) . ?
S2A C11 1.664(13) . ?
S2A C9 1.670(13) . ?
Os3 C301 1.91(2) . ?
Os3 C303 1.93(2) . ?
Os3 C302 1.95(2) . ?
Os3 C304 1.97(2) . ?
Os3 C4 2.136(13) . ?
C3 C4 1.30(2) . ?
C4 C9 1.51(2) . ?
C5 C6A 1.47(2) . ?
C5 C6 1.475(14) . ?
C6 C7 1.471(15) . ?
C6A C8 1.47(2) . ?
C7 C8 1.25(2) . ?
C9 C10 1.468(14) . ?
C9 C10A 1.48(2) . ?
C10 C11 1.471(15) . ?
C10A C12 1.47(2) . ?
C11 C12 1.29(3) . ?
C101 O101 1.11(2) . ?
C102 O102 1.14(2) . ?
C103 O103 1.12(2) . ?
C104 O104 1.13(2) . ?
C201 O201 1.15(2) . ?
C202 O202 1.12(2) . ?
C203 O203 1.15(2) . ?
C301 O301 1.15(2) . ?
C302 O302 1.11(2) . ?
C303 O303 1.17(2) . ?
C304 O304 1.09(2) . ?

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
C101 Os1 C102 91.1(7) . . ?
C101 Os1 C103 93.3(7) . . ?
C102 Os1 C103 95.7(7) . . ?
C101 Os1 C104 92.3(7) . . ?
C102 Os1 C104 166.9(7) . . ?
C103 Os1 C104 96.8(7) . . ?
C101 Os1 C1 103.1(6) . . ?
C102 Os1 C1 85.3(6) . . ?
C103 Os1 C1 163.5(6) . . ?
C104 Os1 C1 81.6(6) . . ?
C101 Os1 Os2 177.6(5) . . ?
C102 Os1 Os2 89.9(4) . . ?
C103 Os1 Os2 88.8(5) . . ?
C104 Os1 Os2 86.3(5) . . ?
C1 Os1 Os2 74.8(4) . . ?
C2 C1 C5 121.2(13) . . ?
C2 C1 Os1 106.8(10) . . ?
C5 C1 Os1 132.0(10) . . ?
C8 S1 C5 91.9(8) . . ?
C7 S1A C5 91.1(12) . . ?
C201 Os2 C202 90.4(6) . . ?
C201 Os2 C203 179.0(6) . . ?
C202 Os2 C203 88.7(6) . . ?
C201 Os2 C3 89.3(6) . . ?
C202 Os2 C3 165.4(6) . . ?
C203 Os2 C3 91.4(6) . . ?
C201 Os2 C2 88.6(6) . . ?
C202 Os2 C2 160.7(6) . . ?
C203 Os2 C2 92.4(6) . . ?
C3 Os2 C2 33.9(5) . . ?
C201 Os2 Os1 89.2(4) . . ?
C202 Os2 Os1 97.0(4) . . ?
C203 Os2 Os1 91.5(4) . . ?
C3 Os2 Os1 97.6(3) . . ?
C2 Os2 Os1 63.7(4) . . ?
C201 Os2 Os3 91.4(4) . . ?
C202 Os2 Os3 100.1(4) . . ?
C203 Os2 Os3 88.2(4) . . ?
C3 Os2 Os3 65.4(3) . . ?
C2 Os2 Os3 99.2(4) . . ?
Os1 Os2 Os3 162.91(3) . . ?
C1 C2 C3 172.4(15) . . ?
C1 C2 Os2 114.7(11) . . ?
C3 C2 Os2 72.9(8) . . ?
C12 S2 C9 92.9(9) . . ?
C11 S2A C9 91.7(12) . . ?
C301 Os3 C303 90.8(6) . . ?
C301 Os3 C302 90.1(7) . . ?
C303 Os3 C302 172.3(6) . . ?
C301 Os3 C304 96.1(6) . . ?
C303 Os3 C304 93.9(7) . . ?
C302 Os3 C304 93.7(7) . . ?
C301 Os3 C4 103.4(6) . . ?
C303 Os3 C4 86.1(6) . . ?
C302 Os3 C4 86.2(6) . . ?
C304 Os3 C4 160.5(6) . . ?
C301 Os3 Os2 175.6(4) . . ?
C303 Os3 Os2 88.0(4) . . ?
C302 Os3 Os2 90.5(5) . . ?
C304 Os3 Os2 88.2(4) . . ?
C4 Os3 Os2 72.3(4) . . ?
C4 C3 C2 175.5(14) . . ?
C4 C3 Os2 111.3(10) . . ?
C2 C3 Os2 73.2(9) . . ?
C3 C4 C9 121.4(12) . . ?
C3 C4 Os3 111.0(10) . . ?
C9 C4 Os3 127.4(9) . . ?
C1 C5 C6A 133.1(12) . . ?
C1 C5 C6 125.6(11) . . ?
C1 C5 S1A 117.2(9) . . ?
C6A C5 S1A 109.7(12) . . ?
C1 C5 S1 124.4(9) . . ?
C6 C5 S1 110.0(10) . . ?
C7 C6 C5 108.1(15) . . ?
C5 C6A C8 109.8(19) . . ?
C8 C7 C6 112.1(16) . . ?
C8 C7 S1A 120.7(15) . . ?
C7 C8 C6A 108.7(18) . . ?
C7 C8 S1 117.9(14) . . ?
C10 C9 C4 128.2(11) . . ?
C10A C9 C4 130.8(12) . . ?
C10A C9 S2A 109.5(13) . . ?
C4 C9 S2A 119.7(9) . . ?
C10 C9 S2 110.0(11) . . ?
C4 C9 S2 121.7(9) . . ?
C9 C10 C11 109.0(16) . . ?
C12 C10A C9 110.9(21) . . ?
C12 C11 C10 111.5(16) . . ?
C12 C11 S2A 120.3(16) . . ?
C11 C12 C10A 107.6(19) . . ?
C11 C12 S2 116.5(14) . . ?
O101 C101 Os1 176.6(17) . . ?
O102 C102 Os1 175.1(15) . . ?
O103 C103 Os1 177.4(14) . . ?
O104 C104 Os1 171.3(16) . . ?
O201 C201 Os2 178.7(13) . . ?
O202 C202 Os2 177.4(14) . . ?
O203 C203 Os2 178.4(14) . . ?
O301 C301 Os3 174.9(14) . . ?
O302 C302 Os3 175.3(16) . . ?
O303 C303 Os3 177.1(13) . . ?
O304 C304 Os3 178.9(14) . . ?

_refine_diff_density_max    4.927
_refine_diff_density_min   -3.548
_refine_diff_density_rms    0.488