# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 186/1350
data_str382 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 [Mn2(mu-PPh2)(mu-C4H3S)(CO)6]  (COMPOUND 3 IN DALTON PAPER 8/09845J)
; 
_chemical_name_common             ? 
_chemical_formula_moiety          [Mn2(PPh2)(C4H3S)(CO)6]
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C22 H13 Mn2 O6 P S' 
_chemical_formula_weight          546.23 
_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' 
 'P'  'P'   0.1023   0.0942 
 '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' 
 'Mn'  'Mn'   0.3368   0.7283 
 '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                    16.217(3) 
_cell_length_b                    9.1007(12) 
_cell_length_c                    16.280(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  112.084(13) 
_cell_angle_gamma                 90.00 
_cell_volume                      2226.4(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     35
_cell_measurement_theta_min       8
_cell_measurement_theta_max       15
 
_exptl_crystal_description        block
_exptl_crystal_colour             orange
_exptl_crystal_size_max           0.50
_exptl_crystal_size_mid           0.38
_exptl_crystal_size_min           0.25
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.630 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1096 
_exptl_absorpt_coefficient_mu     1.336 
_exptl_absorpt_correction_type    'semi-empirical by psi-scans'
_exptl_absorpt_correction_T_min   0.657
_exptl_absorpt_correction_T_max   1.000 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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        'Nicolet R3v/m'
_diffrn_measurement_method        'omega-2theta scans'
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0
_diffrn_reflns_number             4168 
_diffrn_reflns_av_R_equivalents   0.0238 
_diffrn_reflns_av_sigmaI/netI     0.0216 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -21 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          2.61 
_diffrn_reflns_theta_max          27.57 
_reflns_number_total              3997 
_reflns_number_observed           3375 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'SHELXTL PLUS'
_computing_cell_refinement        'SHELXTL PLUS'   
_computing_data_reduction         'SHELXTL PLUS'   
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'SHELXTL PLUS'   
_computing_publication_material   'SHELXL-93 (Sheldrick, 1993)'      
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 7 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^)+(0.0415P)^2^+1.2884P] 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     ? 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3990 
_refine_ls_number_parameters      289 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0397 
_refine_ls_R_factor_obs           0.0311 
_refine_ls_wR_factor_all          0.0850 
_refine_ls_wR_factor_obs          0.0766 
_refine_ls_goodness_of_fit_all    1.039 
_refine_ls_goodness_of_fit_obs    1.053 
_refine_ls_restrained_S_all       1.068 
_refine_ls_restrained_S_obs       1.053 
_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 
Mn1 Mn 0.35864(3) 0.03687(4) 0.11529(2) 0.03247(12) Uani 1 d . . 
Mn2 Mn 0.33570(3) 0.41519(4) 0.07246(2) 0.03029(12) Uani 1 d . . 
P P 0.25487(5) 0.19390(6) 0.02205(4) 0.0288(2) Uani 1 d . . 
S S 0.37700(5) 0.17970(7) 0.23799(4) 0.0435(2) Uani 1 d . . 
C1 C 0.4134(2) 0.2554(3) 0.15799(15) 0.0347(6) Uani 1 d . . 
C2 C 0.4807(2) 0.1641(3) 0.1511(2) 0.0385(6) Uani 1 d . . 
H2A H 0.5089(2) 0.1830(3) 0.1099(2) 0.080 Uiso 1 d R . 
C3 C 0.4957(2) 0.0325(3) 0.2038(2) 0.0499(8) Uani 1 d . . 
H3A H 0.5365(2) -0.0430(3) 0.2024(2) 0.080 Uiso 1 d R . 
C4 C 0.4419(2) 0.0223(3) 0.2520(2) 0.0489(8) Uani 1 d . . 
H4A H 0.4416(2) -0.0586(3) 0.2898(2) 0.080 Uiso 1 d R . 
C31 C 0.2185(2) 0.1520(3) -0.0968(2) 0.0361(6) Uani 1 d . . 
C32 C 0.2252(2) 0.2497(3) -0.1592(2) 0.0440(7) Uani 1 d . . 
H32A H 0.2510(2) 0.3447(3) -0.1404(2) 0.080 Uiso 1 d R . 
C33 C 0.1955(2) 0.2104(4) -0.2483(2) 0.0613(9) Uani 1 d . . 
H33A H 0.2002(2) 0.2786(4) -0.2913(2) 0.080 Uiso 1 d R . 
C34 C 0.1585(2) 0.0759(5) -0.2746(2) 0.0707(11) Uani 1 d . . 
H34A H 0.1384(2) 0.0482(5) -0.3359(2) 0.080 Uiso 1 d R . 
C35 C 0.1519(2) -0.0211(4) -0.2143(2) 0.0690(11) Uani 1 d . . 
H35A H 0.1248(2) -0.1151(4) -0.2337(2) 0.080 Uiso 1 d R . 
C36 C 0.1821(2) 0.0150(3) -0.1252(2) 0.0541(8) Uani 1 d . . 
H36A H 0.1785(2) -0.0552(3) -0.0827(2) 0.080 Uiso 1 d R . 
C41 C 0.1461(2) 0.1993(3) 0.0327(2) 0.0341(6) Uani 1 d . . 
C42 C 0.0765(2) 0.2801(4) -0.0271(2) 0.0538(9) Uani 1 d . . 
H42A H 0.0857(2) 0.3292(4) -0.0752(2) 0.080 Uiso 1 d R . 
C43 C -0.0038(3) 0.2934(4) -0.0176(2) 0.0647(10) Uani 1 d . . 
H43A H -0.0513(3) 0.3493(4) -0.0595(2) 0.080 Uiso 1 d R . 
C44 C -0.0174(2) 0.2260(4) 0.0515(2) 0.0613(9) Uani 1 d . . 
H44A H -0.0737(2) 0.2329(4) 0.0580(2) 0.080 Uiso 1 d R . 
C45 C 0.0507(3) 0.1460(4) 0.1112(2) 0.0616(10) Uani 1 d . . 
H45A H 0.0421(3) 0.0995(4) 0.1603(2) 0.080 Uiso 1 d R . 
C46 C 0.1315(2) 0.1325(3) 0.1025(2) 0.0462(8) Uani 1 d . . 
H46A H 0.1786(2) 0.0770(3) 0.1451(2) 0.080 Uiso 1 d R . 
C11 C 0.3777(2) -0.0547(3) 0.0276(2) 0.0483(8) Uani 1 d . . 
O11 O 0.3901(2) -0.1164(3) -0.0278(2) 0.0799(8) Uani 1 d . . 
C12 C 0.2862(2) -0.1094(3) 0.1171(2) 0.0438(7) Uani 1 d . . 
O12 O 0.2419(2) -0.2062(2) 0.1193(2) 0.0684(7) Uani 1 d . . 
C21 C 0.2600(2) 0.5333(3) -0.0128(2) 0.0424(7) Uani 1 d . . 
O21 O 0.2132(2) 0.6074(3) -0.0664(2) 0.0697(7) Uani 1 d . . 
C22 C 0.4111(2) 0.5641(3) 0.1301(2) 0.0386(6) Uani 1 d . . 
O22 O 0.45602(15) 0.6581(2) 0.16613(15) 0.0577(6) Uani 1 d . . 
C23 C 0.4007(2) 0.3745(3) 0.0036(2) 0.0392(7) Uani 1 d . . 
O23 O 0.4418(2) 0.3495(3) -0.0376(2) 0.0680(7) Uani 1 d . . 
O24 O 0.2247(2) 0.4690(2) 0.1795(2) 0.0633(7) Uani 1 d . . 
C24 C 0.2682(2) 0.4461(3) 0.1401(2) 0.0404(7) 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 
Mn1 0.0334(3) 0.0296(2) 0.0376(2) 0.00248(14) 0.0170(2) 0.0033(2) 
Mn2 0.0339(3) 0.0269(2) 0.0353(2) 0.00004(13) 0.0189(2) 0.00025(15) 
P 0.0301(5) 0.0293(3) 0.0306(3) 0.0001(2) 0.0155(3) -0.0002(2) 
S 0.0570(6) 0.0421(3) 0.0340(3) 0.0038(3) 0.0202(3) -0.0006(3) 
C1 0.034(2) 0.0365(13) 0.0351(12) 0.0014(10) 0.0143(11) -0.0043(11) 
C2 0.029(2) 0.0388(13) 0.0456(13) 0.0048(11) 0.0121(11) 0.0003(11) 
C3 0.036(2) 0.046(2) 0.060(2) 0.0103(13) 0.0099(14) 0.0071(13) 
C4 0.051(2) 0.0432(15) 0.0471(15) 0.0140(12) 0.0127(14) 0.0039(13) 
C31 0.028(2) 0.0449(14) 0.0364(12) -0.0047(10) 0.0137(10) 0.0033(11) 
C32 0.042(2) 0.056(2) 0.0347(12) -0.0025(12) 0.0151(12) -0.0003(13) 
C33 0.058(2) 0.093(3) 0.0328(13) -0.0022(15) 0.0178(13) 0.003(2) 
C34 0.058(3) 0.099(3) 0.043(2) -0.028(2) 0.005(2) 0.012(2) 
C35 0.055(3) 0.068(2) 0.070(2) -0.032(2) 0.008(2) -0.004(2) 
C36 0.052(2) 0.050(2) 0.055(2) -0.0120(13) 0.0146(15) -0.0083(14) 
C41 0.029(2) 0.0366(13) 0.0394(12) -0.0036(10) 0.0158(11) -0.0029(11) 
C42 0.037(3) 0.075(2) 0.051(2) 0.0134(15) 0.0193(14) 0.009(2) 
C43 0.034(3) 0.095(3) 0.067(2) 0.011(2) 0.021(2) 0.015(2) 
C44 0.038(2) 0.082(2) 0.074(2) -0.007(2) 0.033(2) 0.000(2) 
C45 0.057(3) 0.076(2) 0.070(2) 0.010(2) 0.045(2) 0.001(2) 
C46 0.038(2) 0.057(2) 0.055(2) 0.0117(13) 0.0301(14) 0.0076(14) 
C11 0.043(2) 0.051(2) 0.055(2) 0.0001(13) 0.0241(14) 0.0098(14) 
O11 0.078(2) 0.101(2) 0.0712(15) -0.0232(14) 0.0398(14) 0.024(2) 
C12 0.048(2) 0.0339(14) 0.054(2) 0.0015(11) 0.0239(14) 0.0034(13) 
O12 0.070(2) 0.0412(12) 0.103(2) -0.0012(11) 0.0430(15) -0.0127(11) 
C21 0.044(2) 0.0395(14) 0.0506(15) 0.0011(12) 0.0258(13) 0.0063(13) 
O21 0.076(2) 0.0663(15) 0.0627(14) 0.0165(12) 0.0207(12) 0.0303(13) 
C22 0.038(2) 0.0332(13) 0.0477(14) 0.0000(11) 0.0189(12) 0.0028(11) 
O22 0.051(2) 0.0417(11) 0.0746(14) -0.0109(10) 0.0171(11) -0.0097(10) 
C23 0.042(2) 0.0408(13) 0.0399(13) 0.0087(11) 0.0209(13) 0.0006(12) 
O23 0.071(2) 0.089(2) 0.0661(14) 0.0171(13) 0.0510(14) 0.0189(14) 
O24 0.082(2) 0.0565(13) 0.0767(15) -0.0136(11) 0.0588(15) -0.0010(12) 
C24 0.049(2) 0.0341(13) 0.0439(14) -0.0053(10) 0.0238(13) -0.0022(12) 
 
_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 
Mn1 C11 1.777(3) . yes 
Mn1 C12 1.783(3) . yes
Mn1 C4 2.130(3) . yes
Mn1 C3 2.148(3) . yes
Mn1 C2 2.174(3) . yes 
Mn1 C1 2.182(2) . yes 
Mn1 P 2.2929(8) . yes
Mn1 S 2.3069(8) . yes
Mn2 C21 1.819(3) . yes 
Mn2 C22 1.830(3) . yes 
Mn2 C24 1.842(3) . yes 
Mn2 C23 1.842(3) . yes
Mn2 C1 2.079(2) . yes 
Mn2 P 2.3746(8) . yes 
P C41 1.837(3) . ? 
P C31 1.838(2) . ? 
S C4 1.741(3) . yes 
S C1 1.760(3) . yes 
C1 C2 1.409(4) . yes 
C2 C3 1.439(4) . yes 
C3 C4 1.380(5) . yes 
C31 C36 1.382(4) . ? 
C31 C32 1.385(4) . ? 
C32 C33 1.392(4) . ? 
C33 C34 1.359(5) . ? 
C34 C35 1.354(6) . ? 
C35 C36 1.383(4) . ? 
C41 C46 1.385(4) . ? 
C41 C42 1.391(4) . ? 
C42 C43 1.374(5) . ? 
C43 C44 1.371(5) . ? 
C44 C45 1.374(5) . ? 
C45 C46 1.376(5) . ? 
C11 O11 1.143(4) . ? 
C12 O12 1.146(3) . ? 
C21 O21 1.138(3) . ? 
C22 O22 1.134(3) . ? 
C23 O23 1.133(3) . ? 
O24 C24 1.138(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 
C11 Mn1 C12 88.74(14) . . ? 
C11 Mn1 C4 125.24(13) . . ? 
C12 Mn1 C4 95.67(12) . . ? 
C11 Mn1 C3 94.69(14) . . ? 
C12 Mn1 C3 119.83(12) . . ? 
C4 Mn1 C3 37.62(12) . . ? 
C11 Mn1 C2 92.85(13) . . ? 
C12 Mn1 C2 158.73(11) . . ? 
C4 Mn1 C2 66.26(11) . . ? 
C3 Mn1 C2 38.90(10) . . ? 
C11 Mn1 C1 120.70(13) . . ? 
C12 Mn1 C1 150.06(12) . . ? 
C4 Mn1 C1 72.65(10) . . ? 
C3 Mn1 C1 66.97(11) . . ? 
C2 Mn1 C1 37.75(10) . . ? 
C11 Mn1 P 93.81(10) . . ? 
C12 Mn1 P 98.74(10) . . ? 
C4 Mn1 P 138.57(9) . . ? 
C3 Mn1 P 140.61(8) . . ? 
C2 Mn1 P 102.31(7) . . ? 
C1 Mn1 P 75.65(7) . . yes 
C11 Mn1 S 162.72(11) . . ? 
C12 Mn1 S 106.11(9) . . ? 
C4 Mn1 S 45.99(9) . . ? 
C3 Mn1 S 70.45(9) . . ? 
C2 Mn1 S 70.09(8) . . ? 
C1 Mn1 S 46.05(7) . . ? 
P Mn1 S 92.62(3) . . ? 
C21 Mn2 C22 94.75(12) . . ? 
C21 Mn2 C24 89.09(13) . . ? 
C22 Mn2 C24 90.76(12) . . ? 
C21 Mn2 C23 91.74(12) . . ? 
C22 Mn2 C23 92.05(13) . . ? 
C24 Mn2 C23 177.00(12) . . ? 
C21 Mn2 C1 171.79(11) . . ? 
C22 Mn2 C1 93.15(11) . . ? 
C24 Mn2 C1 93.03(11) . . ? 
C23 Mn2 C1 85.76(11) . . ? 
C21 Mn2 P 96.36(9) . . ? 
C22 Mn2 P 168.77(8) . . ? 
C24 Mn2 P 87.78(8) . . ? 
C23 Mn2 P 89.26(9) . . ? 
C1 Mn2 P 75.81(7) . . yes 
C41 P C31 99.51(12) . . ? 
C41 P Mn1 116.49(8) . . ? 
C31 P Mn1 115.65(9) . . ? 
C41 P Mn2 111.68(8) . . ? 
C31 P Mn2 117.20(9) . . ? 
Mn1 P Mn2 97.32(3) . . yes 
C4 S C1 93.74(14) . . ? 
C4 S Mn1 61.64(10) . . ? 
C1 S Mn1 63.24(8) . . ? 
C2 C1 S 108.2(2) . . ? 
C2 C1 Mn2 130.7(2) . . ? 
S C1 Mn2 118.85(15) . . ? 
C2 C1 Mn1 70.8(2) . . ? 
S C1 Mn1 70.71(9) . . ? 
Mn2 C1 Mn1 110.66(11) . . yes
C1 C2 C3 114.0(3) . . ? 
C1 C2 Mn1 71.4(2) . . ? 
C3 C2 Mn1 69.6(2) . . ? 
C4 C3 C2 113.1(3) . . ? 
C4 C3 Mn1 70.5(2) . . ? 
C2 C3 Mn1 71.5(2) . . ? 
C3 C4 S 110.5(2) . . ? 
C3 C4 Mn1 71.9(2) . . ? 
S C4 Mn1 72.37(10) . . ? 
C36 C31 C32 118.3(2) . . ? 
C36 C31 P 117.9(2) . . ? 
C32 C31 P 123.8(2) . . ? 
C31 C32 C33 120.5(3) . . ? 
C34 C33 C32 119.9(3) . . ? 
C35 C34 C33 120.3(3) . . ? 
C34 C35 C36 120.8(3) . . ? 
C31 C36 C35 120.2(3) . . ? 
C46 C41 C42 117.6(3) . . ? 
C46 C41 P 122.2(2) . . ? 
C42 C41 P 120.1(2) . . ? 
C43 C42 C41 121.4(3) . . ? 
C44 C43 C42 120.4(3) . . ? 
C43 C44 C45 118.9(3) . . ? 
C44 C45 C46 121.2(3) . . ? 
C45 C46 C41 120.6(3) . . ? 
O11 C11 Mn1 178.5(3) . . ? 
O12 C12 Mn1 177.8(3) . . ? 
O21 C21 Mn2 179.4(3) . . ? 
O22 C22 Mn2 178.2(3) . . ? 
O23 C23 Mn2 178.9(3) . . ? 
O24 C24 Mn2 177.4(3) . . ? 
 
_refine_diff_density_max    0.246 
_refine_diff_density_min   -0.265 
_refine_diff_density_rms    0.056 


#=END

data_str405 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 [Re2(mu-Ph2PC4H3S)(CO)8] (COMPOUND 4 IN DALTON PAPER 8/09845J)
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      [Re2(Ph2PC4H3S)(CO)8] 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C24 H13 O8 P Re2 S' 
_chemical_formula_weight          864.77 
_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' 
 'P'  'P'   0.1023   0.0942 
 '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' 
 'Re'  'Re'  -1.0185   7.2310 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            orthorhombic 
_symmetry_space_group_name_H-M    Pcab 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y, z+1/2' 
 'x+1/2, -y+1/2, z' 
 '-x, -y+1/2, z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y, -z-1/2' 
 '-x-1/2, y-1/2, -z' 
 'x, y-1/2, -z-1/2' 
 
_cell_length_a                    14.781(5) 
_cell_length_b                    16.863(5) 
_cell_length_c                    20.407(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      5086.5(29) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     33 
_cell_measurement_theta_min       6.5
_cell_measurement_theta_max       13.3
 
_exptl_crystal_description        block 
_exptl_crystal_colour             'pale yellow'
_exptl_crystal_size_max           0.35
_exptl_crystal_size_mid           0.28 
_exptl_crystal_size_min           0.22 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.259 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              3216 
_exptl_absorpt_coefficient_mu     9.702 
_exptl_absorpt_correction_type    'semi-empirical, psi-scans' 
_exptl_absorpt_correction_T_min   0.690 
_exptl_absorpt_correction_T_max   1.000
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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        'Nicolet R3v/m' 
_diffrn_measurement_method        'omega scans' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0
_diffrn_reflns_number             4392 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0418 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          2.71 
_diffrn_reflns_theta_max          24.98 
_reflns_number_total              4392 
_reflns_number_observed           3387 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'SHELXTL PLUS' 
_computing_cell_refinement        'SHELXTL PLUS'      
_computing_data_reduction         'SHELXTL PLUS'     
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'SHELXTL PLUS'     
_computing_publication_material   'SHELXL-93 (Sheldrick, 1993)'      
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 8 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^)+(0.0668P)^2^+9.9952P] 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     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00120(8) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          4384 
_refine_ls_number_parameters      326 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0568 
_refine_ls_R_factor_obs           0.0407 
_refine_ls_wR_factor_all          0.1146 
_refine_ls_wR_factor_obs          0.0995 
_refine_ls_goodness_of_fit_all    1.034 
_refine_ls_goodness_of_fit_obs    1.047 
_refine_ls_restrained_S_all       1.051 
_refine_ls_restrained_S_obs       1.047 
_refine_ls_shift/esd_max          0.001 
_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 
Re1 Re 0.16545(3) 0.29782(2) 0.37676(2) 0.0327(2) Uani 1 d . . 
Re2 Re 0.19086(3) 0.42155(2) 0.48372(2) 0.0313(2) Uani 1 d . . 
S1 S 0.1669(2) 0.5165(2) 0.39306(12) 0.0338(6) Uani 1 d . . 
P1 P 0.2237(2) 0.39149(15) 0.29634(11) 0.0287(5) Uani 1 d . . 
C1 C 0.2420(7) 0.4897(6) 0.3309(4) 0.033(2) Uani 1 d . . 
C2 C 0.3015(8) 0.5476(7) 0.3201(5) 0.046(3) Uani 1 d . . 
H2A H 0.3463(8) 0.5465(7) 0.2861(5) 0.080 Uiso 1 d R . 
C3 C 0.2909(9) 0.6145(7) 0.3625(6) 0.052(3) Uani 1 d . . 
H3A H 0.3307(9) 0.6594(7) 0.3606(6) 0.080 Uiso 1 d R . 
C4 C 0.2213(8) 0.6072(6) 0.4054(5) 0.043(3) Uani 1 d . . 
H4A H 0.2049(8) 0.6465(6) 0.4374(5) 0.080 Uiso 1 d R . 
C31 C 0.3282(6) 0.3712(6) 0.2527(5) 0.032(2) Uani 1 d . . 
C32 C 0.3586(7) 0.4255(7) 0.2048(5) 0.040(2) Uani 1 d . . 
H32A H 0.3256(7) 0.4736(7) 0.1970(5) 0.080 Uiso 1 d R . 
C33 C 0.4380(7) 0.4098(7) 0.1690(5) 0.045(3) Uani 1 d . . 
H33A H 0.4600(7) 0.4471(7) 0.1372(5) 0.080 Uiso 1 d R . 
C34 C 0.4838(8) 0.3400(9) 0.1809(6) 0.059(3) Uani 1 d . . 
H34A H 0.5377(8) 0.3276(9) 0.1567(6) 0.080 Uiso 1 d R . 
C35 C 0.4527(8) 0.2857(8) 0.2265(6) 0.057(3) Uani 1 d . . 
H35A H 0.4828(8) 0.2357(8) 0.2321(6) 0.080 Uiso 1 d R . 
C36 C 0.3764(8) 0.3022(7) 0.2626(5) 0.044(3) Uani 1 d . . 
H36A H 0.3582(8) 0.2665(7) 0.2968(5) 0.080 Uiso 1 d R . 
C41 C 0.1468(6) 0.4107(6) 0.2273(5) 0.033(2) Uani 1 d . . 
C42 C 0.1348(7) 0.3519(7) 0.1820(5) 0.042(2) Uani 1 d . . 
H42A H 0.1657(7) 0.3021(7) 0.1867(5) 0.080 Uiso 1 d R . 
C43 C 0.0773(8) 0.3629(7) 0.1281(5) 0.044(3) Uani 1 d . . 
H43A H 0.0672(8) 0.3201(7) 0.0979(5) 0.080 Uiso 1 d R . 
C44 C 0.0365(9) 0.4330(9) 0.1196(6) 0.062(4) Uani 1 d . . 
H44A H -0.0011(9) 0.4411(9) 0.0818(6) 0.080 Uiso 1 d R . 
C45 C 0.0463(9) 0.4923(9) 0.1643(6) 0.065(4) Uani 1 d . . 
H45A H 0.0176(9) 0.5428(9) 0.1579(6) 0.080 Uiso 1 d R . 
C46 C 0.1015(8) 0.4814(7) 0.2190(6) 0.051(3) Uani 1 d . . 
H46A H 0.1084(8) 0.5226(7) 0.2511(6) 0.080 Uiso 1 d R . 
C11 C 0.1658(8) 0.2163(7) 0.3123(6) 0.050(3) Uani 1 d . . 
O11 O 0.1679(7) 0.1658(6) 0.2737(5) 0.074(3) Uani 1 d . . 
C12 C 0.0471(8) 0.3434(7) 0.3559(5) 0.044(3) Uani 1 d . . 
O12 O -0.0230(6) 0.3709(6) 0.3446(4) 0.061(2) Uani 1 d . . 
C13 C 0.2835(9) 0.2652(7) 0.4126(6) 0.050(3) Uani 1 d . . 
O13 O 0.3495(6) 0.2416(6) 0.4345(5) 0.073(3) Uani 1 d . . 
C14 C 0.1089(9) 0.2300(7) 0.4423(6) 0.056(3) Uani 1 d . . 
O14 O 0.0754(8) 0.1904(7) 0.4816(5) 0.089(4) Uani 1 d . . 
C21 C 0.3225(8) 0.4245(7) 0.4633(6) 0.045(3) Uani 1 d . . 
O21 O 0.3973(6) 0.4263(6) 0.4520(5) 0.073(3) Uani 1 d . . 
C22 C 0.2089(8) 0.3380(7) 0.5443(5) 0.046(3) Uani 1 d . . 
O22 O 0.2173(7) 0.2856(5) 0.5812(4) 0.066(3) Uani 1 d . . 
C23 C 0.2042(7) 0.5033(7) 0.5474(5) 0.043(3) Uani 1 d . . 
O23 O 0.2127(7) 0.5529(5) 0.5873(4) 0.071(3) Uani 1 d . . 
C24 C 0.0589(7) 0.4074(6) 0.4952(5) 0.037(2) Uani 1 d . . 
O24 O -0.0169(6) 0.3979(6) 0.5042(4) 0.060(2) 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 
Re1 0.0390(3) 0.0225(2) 0.0366(2) 0.0004(2) 0.0036(2) -0.0033(2) 
Re2 0.0360(3) 0.0265(2) 0.0315(2) 0.0015(2) 0.0016(2) 0.0013(2) 
S1 0.0406(13) 0.0252(13) 0.0356(12) 0.0002(10) 0.0007(10) 0.0043(11) 
P1 0.0305(12) 0.0219(12) 0.0337(12) 0.0010(10) 0.0020(10) -0.0013(10) 
C1 0.041(5) 0.028(5) 0.031(5) -0.003(4) 0.001(4) -0.005(5) 
C2 0.053(7) 0.043(7) 0.043(6) -0.003(5) -0.001(5) -0.009(6) 
C3 0.063(8) 0.028(6) 0.065(7) 0.001(5) -0.003(6) -0.015(6) 
C4 0.068(8) 0.022(5) 0.038(5) -0.002(4) -0.003(5) 0.008(5) 
C31 0.033(5) 0.034(6) 0.031(5) -0.003(4) -0.006(4) -0.005(4) 
C32 0.037(6) 0.047(7) 0.036(5) -0.001(5) -0.002(4) -0.003(5) 
C33 0.041(6) 0.050(7) 0.043(6) 0.003(5) 0.003(5) -0.004(5) 
C34 0.043(6) 0.086(10) 0.048(6) -0.010(7) 0.017(5) 0.014(7) 
C35 0.052(7) 0.057(8) 0.062(8) 0.005(6) 0.010(6) 0.025(6) 
C36 0.045(6) 0.040(7) 0.046(6) 0.007(5) 0.005(5) 0.009(5) 
C41 0.025(5) 0.042(6) 0.033(5) -0.003(4) 0.003(4) 0.003(4) 
C42 0.044(6) 0.032(6) 0.049(6) 0.001(5) -0.001(5) 0.001(5) 
C43 0.054(7) 0.048(7) 0.031(5) -0.004(5) -0.010(5) -0.011(6) 
C44 0.049(7) 0.084(11) 0.052(7) 0.008(7) -0.015(6) 0.009(7) 
C45 0.075(9) 0.066(9) 0.054(7) 0.014(7) -0.018(7) 0.033(7) 
C46 0.045(6) 0.047(7) 0.059(7) -0.010(6) -0.008(5) 0.013(6) 
C11 0.060(8) 0.027(6) 0.062(7) 0.001(5) 0.007(6) 0.002(5) 
O11 0.099(8) 0.042(5) 0.082(6) -0.033(5) 0.002(6) -0.007(5) 
C12 0.048(7) 0.040(7) 0.043(6) -0.004(5) 0.005(5) -0.012(6) 
O12 0.040(5) 0.069(6) 0.075(6) 0.000(5) -0.005(4) 0.008(4) 
C13 0.074(9) 0.028(6) 0.047(6) -0.006(5) 0.021(6) 0.007(6) 
O13 0.062(6) 0.070(7) 0.087(7) 0.003(6) -0.014(5) 0.029(5) 
C14 0.067(8) 0.042(7) 0.058(7) 0.002(6) -0.007(6) -0.015(7) 
O14 0.113(9) 0.086(8) 0.068(6) 0.033(6) 0.018(6) -0.037(7) 
C21 0.049(7) 0.043(7) 0.042(6) 0.018(5) 0.006(5) 0.001(5) 
O21 0.040(5) 0.100(9) 0.078(6) 0.016(5) 0.006(5) -0.001(5) 
C22 0.057(7) 0.034(6) 0.047(6) -0.009(5) -0.003(5) -0.003(5) 
O22 0.091(7) 0.046(5) 0.060(5) 0.030(4) -0.003(5) 0.005(5) 
C23 0.045(6) 0.041(7) 0.042(6) 0.009(5) 0.007(5) 0.005(5) 
O23 0.115(8) 0.047(5) 0.052(5) -0.025(4) -0.016(5) -0.004(5) 
C24 0.033(6) 0.032(6) 0.046(6) -0.005(4) 0.007(5) 0.005(5) 
O24 0.049(5) 0.065(6) 0.065(5) 0.000(4) 0.009(4) -0.001(5) 
 
_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 
Re1 C11 1.903(12) . yes 
Re1 C14 1.949(13) . yes 
Re1 C12 1.958(12) . yes 
Re1 C13 1.969(14) . yes 
Re1 P1 2.435(2) . yes 
Re1 Re2 3.0428(9) . yes
Re2 C22 1.894(12) . yes 
Re2 C23 1.905(12) . yes 
Re2 C24 1.979(11) . yes 
Re2 C21 1.991(12) . yes
Re2 S1 2.473(3) . yes 
S1 C1 1.744(10) . yes 
S1 C4 1.746(11) . yes 
P1 C31 1.816(10) . ? 
P1 C1 1.821(10) . ? 
P1 C41 1.839(10) . ? 
C1 C2 1.333(15) . yes
C2 C3 1.43(2) . yes 
C3 C4 1.36(2) . yes
C31 C36 1.379(15) . ? 
C31 C32 1.413(15) . ? 
C32 C33 1.41(2) . ? 
C33 C34 1.38(2) . ? 
C34 C35 1.38(2) . ? 
C35 C36 1.37(2) . ? 
C41 C42 1.368(15) . ? 
C41 C46 1.378(15) . ? 
C42 C43 1.402(14) . ? 
C43 C44 1.34(2) . ? 
C44 C45 1.36(2) . ? 
C45 C46 1.40(2) . ? 
C11 O11 1.160(14) . ? 
C12 O12 1.158(14) . ? 
C13 O13 1.146(15) . ? 
C14 O14 1.154(14) . ? 
C21 O21 1.130(14) . ? 
C22 O22 1.167(14) . ? 
C23 O23 1.174(14) . ? 
C24 O24 1.148(13) . ? 
 
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 
C11 Re1 C14 93.0(5) . . ? 
C11 Re1 C12 97.8(5) . . ? 
C14 Re1 C12 89.8(5) . . ? 
C11 Re1 C13 93.0(5) . . ? 
C14 Re1 C13 87.8(5) . . ? 
C12 Re1 C13 169.0(4) . . ? 
C11 Re1 P1 90.1(4) . . ? 
C14 Re1 P1 174.4(4) . . ? 
C12 Re1 P1 85.1(3) . . ? 
C13 Re1 P1 96.8(3) . . ? 
C11 Re1 Re2 172.3(4) . . ? 
C14 Re1 Re2 87.9(4) . . ? 
C12 Re1 Re2 89.8(3) . . ? 
C13 Re1 Re2 79.4(3) . . ? 
P1 Re1 Re2 89.72(6) . . yes 
C22 Re2 C23 94.5(5) . . ? 
C22 Re2 C24 88.4(5) . . ? 
C23 Re2 C24 96.2(4) . . ? 
C22 Re2 C21 91.0(5) . . ? 
C23 Re2 C21 91.3(5) . . ? 
C24 Re2 C21 172.5(5) . . ? 
C22 Re2 S1 172.2(3) . . ? 
C23 Re2 S1 93.3(3) . . ? 
C24 Re2 S1 91.5(3) . . ? 
C21 Re2 S1 88.2(3) . . ? 
C22 Re2 Re1 88.6(3) . . ? 
C23 Re2 Re1 176.8(3) . . ? 
C24 Re2 Re1 83.2(3) . . ? 
C21 Re2 Re1 89.3(4) . . ? 
S1 Re2 Re1 83.67(7) . . yes
C1 S1 C4 92.2(5) . . ? 
C1 S1 Re2 106.5(3) . . yes
C4 S1 Re2 113.2(4) . . yes 
C31 P1 C1 103.6(5) . . yes 
C31 P1 C41 100.5(4) . . yes 
C1 P1 C41 103.2(5) . . yes
C31 P1 Re1 120.6(4) . . yes
C1 P1 Re1 112.4(3) . . yes
C41 P1 Re1 114.4(3) . . yes
C2 C1 S1 110.5(8) . . ? 
C2 C1 P1 134.4(8) . . ? 
S1 C1 P1 115.0(5) . . ? 
C1 C2 C3 113.9(11) . . ? 
C4 C3 C2 113.7(10) . . ? 
C3 C4 S1 109.6(8) . . ? 
C36 C31 C32 118.9(9) . . ? 
C36 C31 P1 121.8(8) . . ? 
C32 C31 P1 119.2(8) . . ? 
C33 C32 C31 120.2(10) . . ? 
C34 C33 C32 118.5(11) . . ? 
C35 C34 C33 121.3(10) . . ? 
C36 C35 C34 120.0(11) . . ? 
C31 C36 C35 121.0(11) . . ? 
C42 C41 C46 118.8(9) . . ? 
C42 C41 P1 118.0(8) . . ? 
C46 C41 P1 123.1(8) . . ? 
C41 C42 C43 120.8(10) . . ? 
C44 C43 C42 119.5(11) . . ? 
C43 C44 C45 121.0(11) . . ? 
C44 C45 C46 120.1(12) . . ? 
C41 C46 C45 119.8(11) . . ? 
O11 C11 Re1 178.3(11) . . ? 
O12 C12 Re1 178.8(9) . . ? 
O13 C13 Re1 175.5(11) . . ? 
O14 C14 Re1 179.4(12) . . ? 
O21 C21 Re2 179.7(7) . . ? 
O22 C22 Re2 177.9(11) . . ? 
O23 C23 Re2 179.1(10) . . ? 
O24 C24 Re2 177.3(10) . . ? 
 
_refine_diff_density_max    1.684 
_refine_diff_density_min   -1.939 
_refine_diff_density_rms    0.207 

#=END

data_str469 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 [Re2(mu-PPh2)(mu-C4H3S)(CO)8] (COMPOUND 5 IN DALTON PAPER 8/09845J)
; 
_chemical_name_common             ? 
_chemical_formula_moiety          [Re2(PPh2)(C4H3S)(CO)8]
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C24 H13 O8 P Re2 S' 
_chemical_formula_weight          864.77 
_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' 
 'P'  'P'   0.1023   0.0942 
 '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' 
 'Re'  'Re'  -1.0185   7.2310 
 '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)/a
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z' 
 
_cell_length_a                    9.367(2) 
_cell_length_b                    30.236(13) 
_cell_length_c                    9.481(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  105.37(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2589.2(16) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     25
_cell_measurement_theta_min       7 
_cell_measurement_theta_max       14 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.45 
_exptl_crystal_size_mid           0.32 
_exptl_crystal_size_min           0.25 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.218 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1608 
_exptl_absorpt_coefficient_mu     9.530 
_exptl_absorpt_correction_type    'empirical, psi-scans'
_exptl_absorpt_correction_T_min   0.455
_exptl_absorpt_correction_T_max   1.000 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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        'Nicolet R3v/m'
_diffrn_measurement_method        'omega scans'
_diffrn_standards_number          3
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             4763 
_diffrn_reflns_av_R_equivalents   0.0621 
_diffrn_reflns_av_sigmaI/netI     0.0341 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        35 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        10 
_diffrn_reflns_theta_min          2.60 
_diffrn_reflns_theta_max          25.01 
_reflns_number_total              4483 
_reflns_number_observed           3738 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'SHELXTL PLUS' 
_computing_cell_refinement        'SHELXTL PLUS'   
_computing_data_reduction         'SHELXTL PLUS'   
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'SHELXTL PLUS'   
_computing_publication_material   'SHELXL-93 (Sheldrick, 1993)'   
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 3 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^)+(0.0866P)^2^+18.3878P] 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     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0006(2) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          4480 
_refine_ls_number_parameters      326 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0594 
_refine_ls_R_factor_obs           0.0491 
_refine_ls_wR_factor_all          0.1352 
_refine_ls_wR_factor_obs          0.1257 
_refine_ls_goodness_of_fit_all    1.030 
_refine_ls_goodness_of_fit_obs    1.060 
_refine_ls_restrained_S_all       1.036 
_refine_ls_restrained_S_obs       1.060 
_refine_ls_shift/esd_max          -0.002 
_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 
Re1 Re 0.54418(4) 0.668624(13) 0.02556(5) 0.0301(2) Uani 1 d . . 
Re2 Re 0.90833(4) 0.590247(14) -0.00708(5) 0.0348(2) Uani 1 d . . 
S S 0.6553(3) 0.66557(9) -0.1844(3) 0.0368(6) Uani 1 d . . 
C1 C 0.7258(12) 0.6109(4) -0.1865(12) 0.035(2) Uani 1 d . . 
C2 C 0.6453(12) 0.5930(4) -0.3114(12) 0.037(2) Uani 1 d . . 
H2A H 0.6656(12) 0.5636(4) -0.3392(12) 0.080 Uiso 1 d R . 
C3 C 0.5276(15) 0.6192(4) -0.4011(14) 0.049(3) Uani 1 d . . 
H3A H 0.4635(15) 0.6092(4) -0.4920(14) 0.080 Uiso 1 d R . 
C4 C 0.5160(15) 0.6590(4) -0.3459(14) 0.049(3) Uani 1 d . . 
H4A H 0.4432(15) 0.6811(4) -0.3874(14) 0.080 Uiso 1 d R . 
P P 0.7644(3) 0.62209(8) 0.1592(3) 0.0280(5) Uani 1 d . . 
C31 C 0.8745(12) 0.6558(4) 0.3127(13) 0.036(2) Uani 1 d . . 
C32 C 1.0128(14) 0.6728(4) 0.3128(15) 0.050(3) Uani 1 d . . 
H32A H 1.0567(14) 0.6648(4) 0.2357(15) 0.080 Uiso 1 d R . 
C33 C 1.0850(15) 0.7011(5) 0.4261(17) 0.064(4) Uani 1 d . . 
H33A H 1.1801(15) 0.7129(5) 0.4264(17) 0.080 Uiso 1 d R . 
C34 C 1.0231(17) 0.7117(5) 0.5395(16) 0.068(4) Uani 1 d . . 
H34A H 1.0731(17) 0.7314(5) 0.6161(16) 0.080 Uiso 1 d R . 
C35 C 0.8867(17) 0.6942(5) 0.5393(16) 0.062(4) Uani 1 d . . 
H35A H 0.8443(17) 0.7007(5) 0.6188(16) 0.080 Uiso 1 d R . 
C36 C 0.8126(15) 0.6666(4) 0.4279(15) 0.050(3) Uani 1 d . . 
H36A H 0.7165(15) 0.6553(4) 0.4265(15) 0.080 Uiso 1 d R . 
C41 C 0.7146(11) 0.5759(3) 0.2650(11) 0.031(2) Uani 1 d . . 
C42 C 0.5726(12) 0.5592(4) 0.2386(12) 0.040(3) Uani 1 d . . 
H42A H 0.4929(12) 0.5738(4) 0.1695(12) 0.080 Uiso 1 d R . 
C43 C 0.5453(15) 0.5212(4) 0.3079(16) 0.057(4) Uani 1 d . . 
H43A H 0.4469(15) 0.5092(4) 0.2850(16) 0.080 Uiso 1 d R . 
C44 C 0.6569(16) 0.5005(4) 0.4079(15) 0.054(3) Uani 1 d . . 
H44A H 0.6369(16) 0.4744(4) 0.4568(15) 0.080 Uiso 1 d R . 
C45 C 0.7987(13) 0.5179(4) 0.4426(14) 0.044(3) Uani 1 d . . 
H45A H 0.8774(13) 0.5039(4) 0.5146(14) 0.080 Uiso 1 d R . 
C46 C 0.8262(12) 0.5549(4) 0.3712(13) 0.042(3) Uani 1 d . . 
H46A H 0.9247(12) 0.5667(4) 0.3944(13) 0.080 Uiso 1 d R . 
C11 C 0.3931(13) 0.7082(4) -0.0874(12) 0.040(3) Uani 1 d . . 
O11 O 0.3061(11) 0.7323(3) -0.1507(12) 0.066(3) Uani 1 d . . 
C12 C 0.4543(15) 0.6666(4) 0.1827(15) 0.051(3) Uani 1 d . . 
O12 O 0.3974(13) 0.6658(4) 0.2795(13) 0.079(4) Uani 1 d . . 
C13 C 0.6644(13) 0.7208(4) 0.1122(12) 0.038(2) Uani 1 d . . 
O13 O 0.7309(12) 0.7501(3) 0.1589(11) 0.065(3) Uani 1 d . . 
C14 C 0.4268(13) 0.6166(4) -0.0678(13) 0.045(3) Uani 1 d . . 
O14 O 0.3570(13) 0.5873(4) -0.1241(13) 0.078(4) Uani 1 d . . 
C21 C 0.9932(13) 0.5644(5) -0.1564(16) 0.055(3) Uani 1 d . . 
O21 O 1.0400(11) 0.5496(5) -0.2424(14) 0.088(4) Uani 1 d . . 
C22 C 1.0080(14) 0.6458(5) -0.0317(14) 0.052(3) Uani 1 d . . 
O22 O 1.0590(13) 0.6787(4) -0.0533(14) 0.086(4) Uani 1 d . . 
C23 C 1.0721(14) 0.5712(5) 0.1591(15) 0.054(3) Uani 1 d . . 
O23 O 1.1672(12) 0.5609(5) 0.2525(13) 0.088(4) Uani 1 d . . 
C24 C 0.7915(15) 0.5344(4) -0.0006(13) 0.048(3) Uani 1 d . . 
O24 O 0.7290(12) 0.5030(3) -0.0069(13) 0.069(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 
Re1 0.0260(3) 0.0314(3) 0.0322(3) 0.0047(2) 0.0064(2) 0.0041(2) 
Re2 0.0249(3) 0.0418(3) 0.0366(3) -0.0060(2) 0.0064(2) 0.0035(2) 
S 0.041(2) 0.0352(14) 0.0362(15) 0.0014(11) 0.0132(12) -0.0002(11) 
C1 0.034(6) 0.038(6) 0.034(6) 0.006(4) 0.014(5) -0.005(4) 
C2 0.037(6) 0.041(6) 0.030(6) 0.008(5) 0.004(5) -0.008(5) 
C3 0.058(8) 0.055(8) 0.031(6) 0.003(5) 0.009(6) -0.012(6) 
C4 0.051(7) 0.051(7) 0.042(7) 0.019(6) 0.009(6) 0.000(6) 
P 0.0207(12) 0.0310(13) 0.0308(14) 0.0004(10) 0.0040(10) 0.0003(9) 
C31 0.032(6) 0.034(5) 0.041(6) -0.003(5) 0.005(5) -0.002(4) 
C32 0.046(7) 0.065(8) 0.046(7) -0.017(6) 0.022(6) -0.014(6) 
C33 0.036(7) 0.081(10) 0.070(10) -0.016(8) 0.007(7) -0.025(7) 
C34 0.067(10) 0.074(10) 0.053(9) -0.030(7) -0.003(7) -0.018(8) 
C35 0.071(10) 0.067(9) 0.049(8) -0.018(7) 0.020(7) 0.002(7) 
C36 0.047(7) 0.057(7) 0.052(8) -0.003(6) 0.022(6) -0.009(6) 
C41 0.027(5) 0.034(5) 0.032(5) -0.003(4) 0.006(4) 0.001(4) 
C42 0.027(5) 0.062(7) 0.031(6) 0.016(5) 0.009(5) -0.004(5) 
C43 0.046(7) 0.053(8) 0.064(9) 0.008(6) -0.001(7) -0.012(6) 
C44 0.071(9) 0.038(6) 0.053(8) 0.014(6) 0.017(7) -0.013(6) 
C45 0.043(7) 0.042(6) 0.045(7) 0.004(5) 0.009(6) 0.009(5) 
C46 0.029(6) 0.051(7) 0.039(6) 0.005(5) -0.002(5) 0.006(5) 
C11 0.047(7) 0.041(6) 0.033(6) -0.006(5) 0.013(5) 0.006(5) 
O11 0.063(6) 0.054(5) 0.073(7) 0.026(5) 0.001(5) 0.023(5) 
C12 0.054(8) 0.046(7) 0.049(8) 0.019(6) 0.010(7) 0.024(6) 
O12 0.070(7) 0.109(9) 0.073(7) 0.038(6) 0.043(6) 0.040(6) 
C13 0.045(7) 0.040(6) 0.025(5) -0.004(4) 0.004(5) 0.003(5) 
O13 0.082(7) 0.041(5) 0.064(7) 0.002(5) 0.007(6) -0.005(5) 
C14 0.032(6) 0.065(8) 0.032(6) 0.015(5) -0.002(5) -0.006(6) 
O14 0.076(8) 0.070(7) 0.072(7) 0.001(5) -0.011(6) -0.037(6) 
C21 0.030(6) 0.071(9) 0.064(9) -0.022(7) 0.013(6) 0.006(6) 
O21 0.049(6) 0.134(10) 0.087(8) -0.048(8) 0.025(6) 0.021(6) 
C22 0.042(7) 0.083(10) 0.036(7) -0.011(6) 0.022(6) -0.013(7) 
O22 0.071(7) 0.106(9) 0.085(8) -0.020(7) 0.026(6) -0.056(7) 
C23 0.036(7) 0.071(9) 0.051(8) -0.015(7) 0.006(6) 0.015(6) 
O23 0.052(6) 0.135(11) 0.065(7) 0.001(7) -0.006(6) 0.029(7) 
C24 0.063(8) 0.034(6) 0.038(7) -0.006(5) 0.000(6) 0.003(6) 
O24 0.071(7) 0.049(6) 0.080(8) -0.002(5) 0.009(6) -0.001(5) 
 
_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 
Re1 C12 1.896(15) . yes 
Re1 C11 1.944(12) . yes 
Re1 C13 1.984(12) . yes
Re1 C14 1.987(13) . yes 
Re1 S 2.481(3) . yes 
Re1 P 2.541(3) . yes 
Re2 C21 1.961(13) . yes 
Re2 C22 1.965(15) . yes 
Re2 C23 1.972(13) . yes 
Re2 C24 2.021(13) . yes
Re2 C1 2.160(11) . yes 
Re2 P 2.522(3) . yes 
S C4 1.739(13) . yes 
S C1 1.781(11) . yes 
C1 C2 1.34(2) . yes 
C2 C3 1.44(2) . yes 
C3 C4 1.33(2) . yes 
P C41 1.849(11) . ? 
P C31 1.850(11) . ? 
C31 C32 1.39(2) . ? 
C31 C36 1.40(2) . ? 
C32 C33 1.40(2) . ? 
C33 C34 1.39(2) . ? 
C34 C35 1.38(2) . ? 
C35 C36 1.38(2) . ? 
C41 C42 1.383(15) . ? 
C41 C46 1.398(15) . ? 
C42 C43 1.38(2) . ? 
C43 C44 1.36(2) . ? 
C44 C45 1.38(2) . ? 
C45 C46 1.37(2) . ? 
C11 O11 1.138(14) . ? 
C12 O12 1.18(2) . ? 
C13 O13 1.107(14) . ? 
C14 O14 1.15(2) . ? 
C21 O21 1.12(2) . ? 
C22 O22 1.15(2) . ? 
C23 O23 1.12(2) . ? 
C24 O24 1.109(15) . ? 
 
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 
C12 Re1 C11 92.4(5) . . ? 
C12 Re1 C13 91.2(5) . . ? 
C11 Re1 C13 89.4(5) . . ? 
C12 Re1 C14 90.9(6) . . ? 
C11 Re1 C14 90.3(5) . . ? 
C13 Re1 C14 177.8(5) . . ? 
C12 Re1 S 175.8(4) . . ? 
C11 Re1 S 88.8(3) . . ? 
C13 Re1 S 92.8(3) . . ? 
C14 Re1 S 85.0(4) . . ? 
C12 Re1 P 93.5(3) . . ? 
C11 Re1 P 172.8(4) . . ? 
C13 Re1 P 86.4(3) . . ? 
C14 Re1 P 93.7(3) . . ? 
S Re1 P 85.52(9) . . yes 
C21 Re2 C22 87.6(6) . . ? 
C21 Re2 C23 94.7(5) . . ? 
C22 Re2 C23 93.0(6) . . ? 
C21 Re2 C24 90.9(6) . . ? 
C22 Re2 C24 174.4(5) . . ? 
C23 Re2 C24 92.5(6) . . ? 
C21 Re2 C1 86.3(5) . . ? 
C22 Re2 C1 87.7(5) . . ? 
C23 Re2 C1 178.9(5) . . ? 
C24 Re2 C1 86.8(4) . . ? 
C21 Re2 P 172.0(4) . . ? 
C22 Re2 P 95.6(4) . . ? 
C23 Re2 P 92.5(4) . . ? 
C24 Re2 P 85.2(4) . . ? 
C1 Re2 P 86.5(3) . . yes 
C4 S C1 94.5(6) . . yes
C4 S Re1 109.5(5) . . yes 
C1 S Re1 106.2(4) . . yes 
C2 C1 S 105.2(8) . . ? 
C2 C1 Re2 136.2(9) . . ? 
S C1 Re2 118.6(6) . . yes
C1 C2 C3 117.6(11) . . ? 
C4 C3 C2 113.3(11) . . ? 
C3 C4 S 109.2(10) . . ? 
C41 P C31 99.0(5) . . ? 
C41 P Re2 107.7(3) . . ? 
C31 P Re2 115.0(4) . . ? 
C41 P Re1 113.6(3) . . ? 
C31 P Re1 107.3(4) . . ? 
Re2 P Re1 113.43(10) . . yes
C32 C31 C36 119.3(11) . . ? 
C32 C31 P 121.9(9) . . ? 
C36 C31 P 118.7(9) . . ? 
C31 C32 C33 119.1(12) . . ? 
C34 C33 C32 121.3(12) . . ? 
C35 C34 C33 119.1(12) . . ? 
C36 C35 C34 120.6(13) . . ? 
C35 C36 C31 120.6(12) . . ? 
C42 C41 C46 117.6(10) . . ? 
C42 C41 P 123.2(8) . . ? 
C46 C41 P 119.1(8) . . ? 
C43 C42 C41 120.6(11) . . ? 
C44 C43 C42 120.5(12) . . ? 
C43 C44 C45 120.1(11) . . ? 
C46 C45 C44 119.2(11) . . ? 
C45 C46 C41 121.8(11) . . ? 
O11 C11 Re1 178.0(10) . . ? 
O12 C12 Re1 179.2(9) . . ? 
O13 C13 Re1 179.1(10) . . ? 
O14 C14 Re1 178.4(11) . . ? 
O21 C21 Re2 179.2(12) . . ? 
O22 C22 Re2 175.8(13) . . ? 
O23 C23 Re2 178.4(14) . . ? 
O24 C24 Re2 174.8(12) . . ? 
 
_refine_diff_density_max    2.005 
_refine_diff_density_min   -1.934 
_refine_diff_density_rms    0.238 

#=END