# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 182/1207

# The synthesis and crystal structure of the first metal-bound stannatrane 
# complex Os(Sn[OCH2CH2]3N)(S2CNMe2)(CO)(PPh3)2:structural comparisons with 
# the analogous silatrane complex Os(Si[OCH2CH2]3N)(S2CNMe2)(CO)(PPh3)2 

data_compound5

_audit_creation_method            SHELXL-97
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'C48 H50 Cl4 N2 O4 Os P2 S2 Sn' 
_chemical_formula_weight          1295.65 
 
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' 
 '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' 
 'Sn'  'Sn'  -0.6537   1.4246 
 '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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    'P 21/c' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    12.45670(10) 
_cell_length_b                    19.2826(2) 
_cell_length_c                    21.7933(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  100.76(1) 
_cell_angle_gamma                 90.00 
_cell_volume                      5142.61(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     203(2) 
_cell_measurement_reflns_used     8192 
_cell_measurement_theta_min       2 
_cell_measurement_theta_max       27 
 
_exptl_crystal_description        Tablet 
_exptl_crystal_colour             Colourless 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.45 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.673 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2560 
_exptl_absorpt_coefficient_mu     3.349 
_exptl_absorpt_correction_type    'Multi-scan' 
_exptl_absorpt_correction_T_min   0.2852 
_exptl_absorpt_correction_T_max   0.6335 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       203(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_type   'Siemens SMART' 
_diffrn_measurement_method        'Area detector w scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             30688 
_diffrn_reflns_av_R_equivalents   0.0400 
_diffrn_reflns_av_sigmaI/netI     0.0438 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          1.42 
_diffrn_reflns_theta_max          27.51 
_reflns_number_total              11288 
_reflns_number_gt                 10019 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Siemens SMART (Siemens, 1995)'
_computing_cell_refinement        'Siemens SMART' 
_computing_data_reduction         'Siemens SAINT  (Siemens, 1995)' 
_computing_structure_solution     'SHELXS Sheldrick, (1990)' 
_computing_structure_refinement   'SHELXL-97 Sheldrick, (1997)' 
_computing_molecular_graphics     'Siemens SHELXTL (Siemens, 1994)' 
_computing_publication_material   'SHELXL-97' 
 
_refine_special_details 
; 
 All non-hydrogen atoms refined anisotropically except the half-weighted
chlorine atoms of a disordered dichloromethane molecule.  Hydrogen atoms
in calculated positions refined by a riding model.
;
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+10.5539P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          11288 
_refine_ls_number_parameters      576 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0409 
_refine_ls_R_factor_gt            0.0354 
_refine_ls_wR_factor_ref          0.1022 
_refine_ls_wR_factor_gt           0.0982 
_refine_ls_goodness_of_fit_ref    1.022 
_refine_ls_restrained_S_all       1.022 
_refine_ls_shift/su_max           0.008 
_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_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Os Os 0.272455(12) 0.270945(7) 0.147078(7) 0.02089(6) Uani 1 d . . . 
Sn Sn 0.13081(2) 0.176759(14) 0.165019(13) 0.02422(8) Uani 1 d . . . 
P1 P 0.15765(8) 0.36144(5) 0.17262(5) 0.0234(2) Uani 1 d . . . 
P2 P 0.40052(8) 0.19151(5) 0.11901(5) 0.0237(2) Uani 1 d . . . 
S1 S 0.36362(9) 0.26099(5) 0.25691(5) 0.0268(2) Uani 1 d . . . 
S2 S 0.42241(8) 0.35725(5) 0.16891(5) 0.0277(2) Uani 1 d . . . 
N1 N 0.5252(3) 0.35307(19) 0.28869(18) 0.0330(8) Uani 1 d . . . 
N2 N -0.0122(3) 0.0966(2) 0.1795(2) 0.0362(9) Uani 1 d . . . 
O1 O 0.1620(3) 0.28380(19) 0.01244(16) 0.0418(8) Uani 1 d . . . 
O2 O 0.0252(3) 0.17233(17) 0.08033(15) 0.0355(7) Uani 1 d . . . 
O3 O 0.2108(3) 0.08646(16) 0.19188(17) 0.0381(7) Uani 1 d . . . 
O4 O 0.0790(3) 0.21100(17) 0.24301(16) 0.0368(7) Uani 1 d . . . 
C1 C 0.2050(3) 0.2793(2) 0.0643(2) 0.0270(9) Uani 1 d . . . 
C2 C 0.4476(3) 0.3272(2) 0.2445(2) 0.0278(8) Uani 1 d . . . 
C3 C 0.5457(5) 0.3227(3) 0.3514(2) 0.0450(12) Uani 1 d . . . 
H3A H 0.5434 0.2726 0.3481 0.068 Uiso 1 calc R . . 
H3B H 0.4901 0.3384 0.3740 0.068 Uiso 1 calc R . . 
H3C H 0.6171 0.3371 0.3735 0.068 Uiso 1 calc R . . 
C4 C 0.5870(4) 0.4144(3) 0.2774(3) 0.0482(13) Uani 1 d . . . 
H4A H 0.5871 0.4184 0.2330 0.072 Uiso 1 calc R . . 
H4B H 0.6615 0.4103 0.3000 0.072 Uiso 1 calc R . . 
H4C H 0.5534 0.4553 0.2916 0.072 Uiso 1 calc R . . 
C5 C -0.0763(4) 0.1399(3) 0.0750(3) 0.0508(14) Uani 1 d . . . 
H5A H -0.0998 0.1235 0.0320 0.061 Uiso 1 calc R . . 
H5B H -0.1302 0.1738 0.0836 0.061 Uiso 1 calc R . . 
C6 C -0.0737(6) 0.0813(4) 0.1178(3) 0.080(2) Uani 1 d . . . 
H6A H -0.1487 0.0689 0.1211 0.096 Uiso 1 calc R . . 
H6B H -0.0409 0.0412 0.1007 0.096 Uiso 1 calc R . . 
C7 C 0.1517(5) 0.0253(3) 0.1916(3) 0.0572(16) Uani 1 d . . . 
H7A H 0.1935 -0.0072 0.2215 0.069 Uiso 1 calc R . . 
H7B H 0.1427 0.0042 0.1501 0.069 Uiso 1 calc R . . 
C8 C 0.0453(5) 0.0352(3) 0.2074(5) 0.080(3) Uani 1 d . . . 
H8A H 0.0537 0.0385 0.2529 0.096 Uiso 1 calc R . . 
H8B H 0.0003 -0.0057 0.1940 0.096 Uiso 1 calc R . . 
C9 C -0.0039(5) 0.1779(3) 0.2664(3) 0.0492(13) Uani 1 d . . . 
H9A H -0.0504 0.2131 0.2807 0.059 Uiso 1 calc R . . 
H9B H 0.0288 0.1500 0.3027 0.059 Uiso 1 calc R . . 
C10 C -0.0733(5) 0.1320(3) 0.2197(3) 0.0641(18) Uani 1 d . . . 
H10A H -0.1095 0.0975 0.2419 0.077 Uiso 1 calc R . . 
H10B H -0.1303 0.1601 0.1941 0.077 Uiso 1 calc R . . 
C11 C 0.1491(4) 0.4382(2) 0.1213(2) 0.0321(9) Uani 1 d . . . 
C12 C 0.0723(4) 0.4898(2) 0.1272(3) 0.0408(11) Uani 1 d . . . 
H12A H 0.0291 0.4855 0.1581 0.049 Uiso 1 calc R . . 
C13 C 0.0592(5) 0.5467(3) 0.0884(3) 0.0543(14) Uani 1 d . . . 
H13A H 0.0084 0.5813 0.0934 0.065 Uiso 1 calc R . . 
C14 C 0.1206(6) 0.5530(3) 0.0421(3) 0.0589(16) Uani 1 d . . . 
H14A H 0.1101 0.5911 0.0146 0.071 Uiso 1 calc R . . 
C15 C 0.1975(6) 0.5033(3) 0.0365(3) 0.0566(15) Uani 1 d . . . 
H15A H 0.2411 0.5082 0.0059 0.068 Uiso 1 calc R . . 
C16 C 0.2109(4) 0.4457(3) 0.0756(2) 0.0418(11) Uani 1 d . . . 
H16A H 0.2627 0.4117 0.0708 0.050 Uiso 1 calc R . . 
C21 C 0.2029(3) 0.3980(2) 0.2504(2) 0.0272(8) Uani 1 d . . . 
C22 C 0.2591(3) 0.4608(2) 0.2579(2) 0.0339(10) Uani 1 d . . . 
H22A H 0.2660 0.4873 0.2227 0.041 Uiso 1 calc R . . 
C23 C 0.3052(4) 0.4844(3) 0.3175(2) 0.0415(12) Uani 1 d . . . 
H23A H 0.3433 0.5267 0.3222 0.050 Uiso 1 calc R . . 
C24 C 0.2954(4) 0.4464(3) 0.3688(2) 0.0451(12) Uani 1 d . . . 
H24A H 0.3271 0.4626 0.4088 0.054 Uiso 1 calc R . . 
C25 C 0.2388(4) 0.3837(3) 0.3626(2) 0.0436(12) Uani 1 d . . . 
H25A H 0.2310 0.3582 0.3982 0.052 Uiso 1 calc R . . 
C26 C 0.1935(4) 0.3590(2) 0.3031(2) 0.0348(10) Uani 1 d . . . 
H26A H 0.1568 0.3162 0.2986 0.042 Uiso 1 calc R . . 
C31 C 0.0100(3) 0.3461(2) 0.1653(2) 0.0300(9) Uani 1 d . . . 
C32 C -0.0483(4) 0.3577(3) 0.2122(3) 0.0427(11) Uani 1 d . . . 
H32A H -0.0112 0.3698 0.2524 0.051 Uiso 1 calc R . . 
C33 C -0.1618(4) 0.3515(3) 0.2005(3) 0.0548(15) Uani 1 d . . . 
H33A H -0.2007 0.3583 0.2331 0.066 Uiso 1 calc R . . 
C34 C -0.2163(4) 0.3357(3) 0.1420(3) 0.0515(15) Uani 1 d . . . 
H34A H -0.2930 0.3332 0.1339 0.062 Uiso 1 calc R . . 
C35 C -0.1592(4) 0.3234(3) 0.0948(3) 0.0471(13) Uani 1 d . . . 
H35A H -0.1970 0.3116 0.0547 0.056 Uiso 1 calc R . . 
C36 C -0.0466(4) 0.3284(2) 0.1062(2) 0.0365(10) Uani 1 d . . . 
H36A H -0.0081 0.3198 0.0738 0.044 Uiso 1 calc R . . 
C41 C 0.4815(3) 0.2262(2) 0.0630(2) 0.0276(9) Uani 1 d . . . 
C42 C 0.4534(4) 0.2886(3) 0.0323(2) 0.0351(10) Uani 1 d . . . 
H42A H 0.3933 0.3138 0.0409 0.042 Uiso 1 calc R . . 
C43 C 0.5130(4) 0.3146(3) -0.0110(2) 0.0423(11) Uani 1 d . . . 
H43A H 0.4924 0.3566 -0.0316 0.051 Uiso 1 calc R . . 
C44 C 0.6020(4) 0.2784(3) -0.0234(2) 0.0393(11) Uani 1 d . . . 
H44A H 0.6427 0.2959 -0.0522 0.047 Uiso 1 calc R . . 
C45 C 0.6311(4) 0.2162(3) 0.0066(2) 0.0401(11) Uani 1 d . . . 
H45A H 0.6916 0.1914 -0.0019 0.048 Uiso 1 calc R . . 
C46 C 0.5715(4) 0.1902(2) 0.0493(2) 0.0347(10) Uani 1 d . . . 
H46A H 0.5919 0.1477 0.0693 0.042 Uiso 1 calc R . . 
C51 C 0.5045(3) 0.1639(2) 0.1850(2) 0.0277(8) Uani 1 d . . . 
C52 C 0.4798(4) 0.1111(2) 0.2247(2) 0.0347(10) Uani 1 d . . . 
H52A H 0.4137 0.0865 0.2142 0.042 Uiso 1 calc R . . 
C53 C 0.5522(4) 0.0951(3) 0.2789(2) 0.0417(11) Uani 1 d . . . 
H53A H 0.5359 0.0591 0.3048 0.050 Uiso 1 calc R . . 
C54 C 0.6487(4) 0.1320(3) 0.2955(2) 0.0444(12) Uani 1 d . . . 
H54A H 0.6977 0.1212 0.3325 0.053 Uiso 1 calc R . . 
C55 C 0.6727(4) 0.1848(3) 0.2573(2) 0.0405(11) Uani 1 d . . . 
H55A H 0.7375 0.2104 0.2689 0.049 Uiso 1 calc R . . 
C56 C 0.6018(4) 0.2001(2) 0.2021(2) 0.0335(9) Uani 1 d . . . 
H56A H 0.6197 0.2354 0.1760 0.040 Uiso 1 calc R . . 
C61 C 0.3543(3) 0.1095(2) 0.0801(2) 0.0267(8) Uani 1 d . . . 
C62 C 0.2474(4) 0.1029(2) 0.0465(2) 0.0324(9) Uani 1 d . . . 
H62A H 0.1995 0.1409 0.0434 0.039 Uiso 1 calc R . . 
C63 C 0.2115(4) 0.0405(3) 0.0176(2) 0.0406(11) Uani 1 d . . . 
H63A H 0.1396 0.0365 -0.0048 0.049 Uiso 1 calc R . . 
C64 C 0.2815(4) -0.0155(2) 0.0219(2) 0.0406(11) Uani 1 d . . . 
H64A H 0.2566 -0.0579 0.0033 0.049 Uiso 1 calc R . . 
C65 C 0.3872(4) -0.0095(2) 0.0532(2) 0.0383(11) Uani 1 d . . . 
H65A H 0.4354 -0.0472 0.0546 0.046 Uiso 1 calc R . . 
C66 C 0.4232(4) 0.0523(2) 0.0830(2) 0.0336(9) Uani 1 d . . . 
H66A H 0.4952 0.0556 0.1053 0.040 Uiso 1 calc R . . 
C70 C 0.0212(5) 0.7959(3) 0.0715(3) 0.0489(13) Uani 1 d . . . 
H70A H -0.0371 0.7781 0.0919 0.059 Uiso 1 calc R . . 
H70B H -0.0089 0.8016 0.0270 0.059 Uiso 1 calc R . . 
Cl1 Cl 0.0651(2) 0.87626(10) 0.10373(10) 0.0914(6) Uani 1 d . . . 
Cl2 Cl 0.12783(19) 0.73623(10) 0.08076(11) 0.0840(6) Uani 1 d . . . 
C71 C 0.2969(8) 0.1125(4) 0.3446(3) 0.081(2) Uani 1 d . . . 
Cl3 Cl 0.23663(17) 0.15160(14) 0.40144(9) 0.0902(6) Uani 1 d . . . 
Cl4 Cl 0.2665(5) 0.0227(3) 0.3486(2) 0.1017(14) Uiso 0.50 d P . . 
Cl4' Cl 0.3481(5) 0.0240(3) 0.3659(3) 0.1044(14) Uiso 0.50 d P . . 
 
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 
Os 0.02147(9) 0.01939(9) 0.02201(10) -0.00045(5) 0.00461(6) -0.00264(5) 
Sn 0.02409(14) 0.02006(14) 0.02927(15) -0.00100(10) 0.00696(11) -0.00381(10) 
P1 0.0257(5) 0.0191(5) 0.0258(5) -0.0020(4) 0.0059(4) -0.0023(4) 
P2 0.0222(5) 0.0231(5) 0.0256(5) -0.0018(4) 0.0042(4) -0.0014(4) 
S1 0.0314(5) 0.0241(5) 0.0249(5) 0.0003(4) 0.0051(4) -0.0031(4) 
S2 0.0274(5) 0.0262(5) 0.0295(5) 0.0016(4) 0.0047(4) -0.0064(4) 
N1 0.0332(19) 0.0290(19) 0.034(2) -0.0046(15) -0.0020(15) -0.0052(15) 
N2 0.037(2) 0.032(2) 0.043(2) -0.0015(17) 0.0159(17) -0.0102(16) 
O1 0.0397(18) 0.054(2) 0.0295(18) 0.0034(15) 0.0008(14) -0.0054(16) 
O2 0.0316(16) 0.0388(18) 0.0349(17) -0.0011(14) 0.0026(13) -0.0095(13) 
O3 0.0379(17) 0.0260(16) 0.053(2) 0.0076(14) 0.0160(15) 0.0056(13) 
O4 0.0441(18) 0.0326(16) 0.0384(18) -0.0067(14) 0.0200(15) -0.0081(14) 
C1 0.0231(19) 0.027(2) 0.030(2) 0.0019(16) 0.0038(17) -0.0007(15) 
C2 0.028(2) 0.0229(19) 0.033(2) -0.0036(16) 0.0063(17) -0.0005(16) 
C3 0.051(3) 0.048(3) 0.031(3) -0.007(2) -0.004(2) 0.001(2) 
C4 0.042(3) 0.043(3) 0.059(3) -0.013(2) 0.006(2) -0.018(2) 
C5 0.035(3) 0.060(3) 0.053(3) 0.001(3) -0.002(2) -0.018(2) 
C6 0.078(5) 0.099(6) 0.060(4) -0.001(4) 0.008(3) -0.058(4) 
C7 0.056(3) 0.021(2) 0.097(5) 0.007(3) 0.022(3) 0.002(2) 
C8 0.063(4) 0.028(3) 0.162(8) 0.017(4) 0.051(5) -0.003(3) 
C9 0.050(3) 0.054(3) 0.051(3) -0.007(2) 0.027(3) -0.011(2) 
C10 0.052(3) 0.062(4) 0.089(5) -0.022(3) 0.040(3) -0.023(3) 
C11 0.033(2) 0.024(2) 0.037(2) -0.0009(17) 0.0021(18) -0.0036(17) 
C12 0.049(3) 0.025(2) 0.049(3) 0.003(2) 0.010(2) 0.004(2) 
C13 0.065(4) 0.035(3) 0.060(4) 0.005(2) 0.002(3) 0.014(3) 
C14 0.088(4) 0.037(3) 0.052(3) 0.018(2) 0.010(3) 0.012(3) 
C15 0.085(4) 0.043(3) 0.047(3) 0.015(2) 0.025(3) 0.003(3) 
C16 0.054(3) 0.031(2) 0.043(3) 0.007(2) 0.016(2) 0.005(2) 
C21 0.028(2) 0.024(2) 0.030(2) -0.0063(16) 0.0062(16) 0.0006(16) 
C22 0.029(2) 0.030(2) 0.043(3) -0.0064(19) 0.0068(19) -0.0020(17) 
C23 0.034(2) 0.040(3) 0.049(3) -0.021(2) 0.004(2) -0.004(2) 
C24 0.039(3) 0.059(3) 0.036(3) -0.021(2) 0.004(2) -0.001(2) 
C25 0.047(3) 0.056(3) 0.030(2) -0.006(2) 0.013(2) 0.003(2) 
C26 0.040(2) 0.034(2) 0.032(2) -0.0065(18) 0.0119(19) -0.0030(19) 
C31 0.028(2) 0.022(2) 0.040(2) 0.0000(17) 0.0070(18) 0.0008(16) 
C32 0.037(2) 0.043(3) 0.051(3) -0.009(2) 0.015(2) -0.004(2) 
C33 0.035(3) 0.053(3) 0.083(4) -0.008(3) 0.027(3) -0.002(2) 
C34 0.026(2) 0.042(3) 0.087(5) 0.004(3) 0.013(3) -0.005(2) 
C35 0.034(2) 0.042(3) 0.060(4) 0.002(2) -0.005(2) -0.006(2) 
C36 0.031(2) 0.037(2) 0.039(3) 0.000(2) 0.0030(19) -0.0013(19) 
C41 0.0250(19) 0.032(2) 0.025(2) -0.0041(16) 0.0041(16) -0.0048(16) 
C42 0.033(2) 0.040(2) 0.033(2) 0.0040(19) 0.0097(19) 0.0028(19) 
C43 0.040(3) 0.051(3) 0.036(3) 0.010(2) 0.010(2) 0.002(2) 
C44 0.035(2) 0.057(3) 0.028(2) -0.003(2) 0.0119(19) -0.009(2) 
C45 0.033(2) 0.050(3) 0.040(3) -0.009(2) 0.013(2) -0.003(2) 
C46 0.033(2) 0.034(2) 0.038(2) -0.0043(19) 0.0091(19) 0.0012(18) 
C51 0.0268(19) 0.029(2) 0.027(2) -0.0031(16) 0.0046(16) 0.0049(16) 
C52 0.036(2) 0.033(2) 0.035(2) -0.0005(18) 0.0042(19) 0.0068(18) 
C53 0.050(3) 0.039(3) 0.035(3) 0.004(2) 0.007(2) 0.010(2) 
C54 0.044(3) 0.053(3) 0.032(3) -0.004(2) -0.004(2) 0.020(2) 
C55 0.027(2) 0.051(3) 0.040(3) -0.015(2) -0.0020(19) 0.003(2) 
C56 0.029(2) 0.038(2) 0.033(2) -0.0034(19) 0.0042(18) 0.0009(18) 
C61 0.031(2) 0.0223(19) 0.027(2) -0.0008(15) 0.0079(16) -0.0026(16) 
C62 0.033(2) 0.035(2) 0.030(2) -0.0068(18) 0.0054(18) -0.0032(18) 
C63 0.036(2) 0.046(3) 0.039(3) -0.012(2) 0.004(2) -0.008(2) 
C64 0.053(3) 0.030(2) 0.039(3) -0.0094(19) 0.007(2) -0.012(2) 
C65 0.050(3) 0.022(2) 0.041(3) -0.0010(18) 0.003(2) 0.0042(19) 
C66 0.033(2) 0.030(2) 0.036(2) -0.0036(18) 0.0022(18) 0.0016(18) 
C70 0.049(3) 0.047(3) 0.050(3) -0.005(3) 0.007(2) -0.006(2) 
Cl1 0.1339(18) 0.0558(10) 0.0831(14) -0.0275(9) 0.0163(13) -0.0134(11) 
Cl2 0.0958(14) 0.0717(12) 0.0929(15) 0.0156(10) 0.0394(12) 0.0339(10) 
C71 0.131(7) 0.067(4) 0.050(4) -0.012(3) 0.033(4) -0.020(5) 
Cl3 0.0717(11) 0.1396(19) 0.0587(11) -0.0241(12) 0.0105(9) -0.0016(12) 
 
_geom_special_details 
; 
 ?
;
 
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 
Os C1 1.849(4) . ? 
Os P2 2.3727(10) . ? 
Os P1 2.3868(10) . ? 
Os S1 2.4577(11) . ? 
Os S2 2.4805(10) . ? 
Os Sn 2.6119(3) . ? 
Sn O3 2.037(3) . ? 
Sn O4 2.037(3) . ? 
Sn O2 2.058(3) . ? 
Sn N2 2.422(4) . ? 
P1 C21 1.824(4) . ? 
P1 C31 1.840(4) . ? 
P1 C11 1.846(5) . ? 
P2 C51 1.827(4) . ? 
P2 C61 1.836(4) . ? 
P2 C41 1.848(4) . ? 
S1 C2 1.704(4) . ? 
S2 C2 1.719(5) . ? 
N1 C2 1.327(5) . ? 
N1 C4 1.456(6) . ? 
N1 C3 1.464(6) . ? 
N2 C10 1.435(7) . ? 
N2 C6 1.449(8) . ? 
N2 C8 1.457(8) . ? 
O1 C1 1.160(5) . ? 
O2 C5 1.396(6) . ? 
O3 C7 1.390(6) . ? 
O4 C9 1.389(6) . ? 
C5 C6 1.462(9) . ? 
C7 C8 1.443(8) . ? 
C9 C10 1.497(8) . ? 
C11 C16 1.375(7) . ? 
C11 C12 1.403(6) . ? 
C12 C13 1.376(7) . ? 
C13 C14 1.380(9) . ? 
C14 C15 1.377(9) . ? 
C15 C16 1.391(7) . ? 
C21 C22 1.393(6) . ? 
C21 C26 1.396(6) . ? 
C22 C23 1.394(7) . ? 
C23 C24 1.361(8) . ? 
C24 C25 1.394(8) . ? 
C25 C26 1.397(7) . ? 
C31 C32 1.377(7) . ? 
C31 C36 1.391(6) . ? 
C32 C33 1.394(7) . ? 
C33 C34 1.362(9) . ? 
C34 C35 1.377(8) . ? 
C35 C36 1.381(7) . ? 
C41 C42 1.388(6) . ? 
C41 C46 1.397(6) . ? 
C42 C43 1.398(7) . ? 
C43 C44 1.380(7) . ? 
C44 C45 1.381(7) . ? 
C45 C46 1.388(7) . ? 
C51 C56 1.389(6) . ? 
C51 C52 1.406(6) . ? 
C52 C53 1.381(7) . ? 
C53 C54 1.386(8) . ? 
C54 C55 1.382(8) . ? 
C55 C56 1.385(7) . ? 
C61 C66 1.391(6) . ? 
C61 C62 1.400(6) . ? 
C62 C63 1.392(6) . ? 
C63 C64 1.380(7) . ? 
C64 C65 1.370(7) . ? 
C65 C66 1.390(6) . ? 
C70 Cl2 1.740(6) . ? 
C70 Cl1 1.747(6) . ? 
C71 Cl3 1.737(8) . ? 
C71 Cl4 1.776(9) . ? 
C71 Cl4' 1.850(10) . ? 
 
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 
C1 Os P2 90.56(13) . . ? 
C1 Os P1 88.90(13) . . ? 
P2 Os P1 173.23(3) . . ? 
C1 Os S1 179.31(13) . . ? 
P2 Os S1 89.43(4) . . ? 
P1 Os S1 91.03(4) . . ? 
C1 Os S2 108.51(13) . . ? 
P2 Os S2 87.94(3) . . ? 
P1 Os S2 85.83(3) . . ? 
S1 Os S2 70.80(3) . . ? 
C1 Os Sn 90.57(13) . . ? 
P2 Os Sn 95.47(3) . . ? 
P1 Os Sn 91.29(3) . . ? 
S1 Os Sn 90.12(3) . . ? 
S2 Os Sn 160.62(3) . . ? 
O3 Sn O4 104.56(14) . . ? 
O3 Sn O2 114.75(14) . . ? 
O4 Sn O2 120.83(14) . . ? 
O3 Sn N2 75.50(13) . . ? 
O4 Sn N2 75.08(13) . . ? 
O2 Sn N2 74.24(13) . . ? 
O3 Sn Os 109.23(9) . . ? 
O4 Sn Os 103.16(9) . . ? 
O2 Sn Os 103.37(9) . . ? 
N2 Sn Os 175.27(10) . . ? 
C21 P1 C31 105.8(2) . . ? 
C21 P1 C11 103.0(2) . . ? 
C31 P1 C11 97.6(2) . . ? 
C21 P1 Os 113.85(14) . . ? 
C31 P1 Os 119.70(14) . . ? 
C11 P1 Os 114.48(15) . . ? 
C51 P2 C61 103.14(19) . . ? 
C51 P2 C41 103.4(2) . . ? 
C61 P2 C41 99.82(18) . . ? 
C51 P2 Os 113.40(14) . . ? 
C61 P2 Os 120.47(14) . . ? 
C41 P2 Os 114.37(14) . . ? 
C2 S1 Os 88.44(15) . . ? 
C2 S2 Os 87.37(14) . . ? 
C2 N1 C4 121.2(4) . . ? 
C2 N1 C3 120.2(4) . . ? 
C4 N1 C3 118.5(4) . . ? 
C10 N2 C6 114.4(5) . . ? 
C10 N2 C8 114.0(5) . . ? 
C6 N2 C8 110.8(6) . . ? 
C10 N2 Sn 105.3(3) . . ? 
C6 N2 Sn 106.5(3) . . ? 
C8 N2 Sn 104.9(3) . . ? 
C5 O2 Sn 120.7(3) . . ? 
C7 O3 Sn 119.6(3) . . ? 
C9 O4 Sn 122.0(3) . . ? 
O1 C1 Os 179.2(4) . . ? 
N1 C2 S1 123.5(3) . . ? 
N1 C2 S2 123.1(3) . . ? 
S1 C2 S2 113.4(2) . . ? 
O2 C5 C6 112.4(5) . . ? 
N2 C6 C5 112.3(5) . . ? 
O3 C7 C8 113.3(5) . . ? 
C7 C8 N2 114.2(5) . . ? 
O4 C9 C10 113.4(5) . . ? 
N2 C10 C9 113.0(5) . . ? 
C16 C11 C12 118.3(4) . . ? 
C16 C11 P1 123.1(4) . . ? 
C12 C11 P1 118.5(4) . . ? 
C13 C12 C11 120.9(5) . . ? 
C12 C13 C14 120.1(5) . . ? 
C15 C14 C13 119.5(5) . . ? 
C14 C15 C16 120.5(5) . . ? 
C11 C16 C15 120.6(5) . . ? 
C22 C21 C26 119.2(4) . . ? 
C22 C21 P1 120.4(3) . . ? 
C26 C21 P1 119.9(3) . . ? 
C21 C22 C23 120.3(5) . . ? 
C24 C23 C22 120.3(5) . . ? 
C23 C24 C25 120.5(5) . . ? 
C24 C25 C26 119.7(5) . . ? 
C21 C26 C25 119.9(4) . . ? 
C32 C31 C36 118.7(4) . . ? 
C32 C31 P1 124.5(4) . . ? 
C36 C31 P1 116.4(3) . . ? 
C31 C32 C33 120.6(5) . . ? 
C34 C33 C32 120.0(5) . . ? 
C33 C34 C35 120.1(5) . . ? 
C34 C35 C36 120.1(5) . . ? 
C35 C36 C31 120.4(5) . . ? 
C42 C41 C46 118.0(4) . . ? 
C42 C41 P2 120.8(3) . . ? 
C46 C41 P2 121.3(3) . . ? 
C41 C42 C43 121.1(4) . . ? 
C44 C43 C42 120.0(5) . . ? 
C43 C44 C45 119.7(5) . . ? 
C44 C45 C46 120.4(5) . . ? 
C45 C46 C41 120.9(5) . . ? 
C56 C51 C52 118.7(4) . . ? 
C56 C51 P2 121.3(3) . . ? 
C52 C51 P2 119.4(3) . . ? 
C53 C52 C51 120.3(5) . . ? 
C52 C53 C54 120.3(5) . . ? 
C55 C54 C53 119.8(5) . . ? 
C54 C55 C56 120.3(5) . . ? 
C55 C56 C51 120.6(5) . . ? 
C66 C61 C62 118.1(4) . . ? 
C66 C61 P2 121.6(3) . . ? 
C62 C61 P2 120.3(3) . . ? 
C63 C62 C61 120.5(4) . . ? 
C64 C63 C62 120.0(4) . . ? 
C65 C64 C63 120.2(4) . . ? 
C64 C65 C66 120.1(4) . . ? 
C65 C66 C61 121.0(4) . . ? 
Cl2 C70 Cl1 111.4(3) . . ? 
Cl3 C71 Cl4 105.3(4) . . ? 
Cl3 C71 Cl4' 113.4(4) . . ? 
Cl4 C71 Cl4' 32.5(2) . . ? 
 
_diffrn_measured_fraction_theta_max    0.928 
_diffrn_reflns_theta_full              27.51 
_diffrn_measured_fraction_theta_full   0.928 
_refine_diff_density_max    2.251 
_refine_diff_density_min   -2.086 
_refine_diff_density_rms    0.134 
 
#==END 

data_compound6 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'C46 H48 N2 O4 Os P2 S2 Si' 
_chemical_formula_weight          1037.21 
 
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' 
 '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' 
 'Os'  'Os'  -1.2165   7.6030 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    'P c a 21'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z+1/2' 
 'x+1/2, -y, z' 
 '-x+1/2, y, z+1/2' 
 
_cell_length_a                    19.9139(2) 
_cell_length_b                    9.94490(10) 
_cell_length_c                    22.2254(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      4401.56(7) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     203(2) 
_cell_measurement_reflns_used     8192 
_cell_measurement_theta_min       2
_cell_measurement_theta_max       27 
 
_exptl_crystal_description        Prism 
_exptl_crystal_colour             Colourless 
_exptl_crystal_size_max           0.24 
_exptl_crystal_size_mid           0.22 
_exptl_crystal_size_min           0.18 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.565 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2088 
_exptl_absorpt_coefficient_mu     3.137 
_exptl_absorpt_correction_type    'Multi-scan' 
_exptl_absorpt_correction_T_min   0.5198 
_exptl_absorpt_correction_T_max   0.6021 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       203(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_type   'Siemens SMART' 
_diffrn_measurement_method        'Area detector w scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             27335 
_diffrn_reflns_av_R_equivalents   0.0281 
_diffrn_reflns_av_sigmaI/netI     0.0313 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        25 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -27 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          1.83 
_diffrn_reflns_theta_max          27.49 
_reflns_number_total              9007 
_reflns_number_gt                 8353 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Siemens SMART (Siemens, 1995)'
_computing_cell_refinement        'Siemens SMART' 
_computing_data_reduction         'Siemens SAINT  (Siemens, 1995)' 
_computing_structure_solution     'SHELXS Sheldrick, (1990)' 
_computing_structure_refinement   'SHELXL-97 Sheldrick, (1997)' 
_computing_molecular_graphics     'Siemens SHELXTL (Siemens, 1994)' 
_computing_publication_material   'SHELXL-97' 
 
_refine_special_details 
; 
 All non-hydrogen atoms allowed to refine anisotropically.  Hydrogen
atoms in calculated positions and allowed to ride on the carrier atom.
A racemic twin, both enantiomers refined with equal weighting.
;
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+11.3270P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.00 
_refine_ls_number_reflns          9007 
_refine_ls_number_parameters      525 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0395 
_refine_ls_R_factor_gt            0.0346 
_refine_ls_wR_factor_ref          0.0762 
_refine_ls_wR_factor_gt           0.0737 
_refine_ls_goodness_of_fit_ref    1.173 
_refine_ls_restrained_S_all       1.173 
_refine_ls_shift/su_max           0.024 
_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_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Os Os 0.312097(9) 0.085634(18) 0.000429(15) 0.02608(5) Uani 1 d . . . 
Si Si 0.37166(8) 0.25141(18) -0.05525(7) 0.0305(3) Uani 1 d . . . 
S1 S 0.22210(7) 0.25440(15) 0.00671(10) 0.0329(3) Uani 1 d . . . 
S2 S 0.21480(7) -0.00384(16) 0.06280(7) 0.0309(3) Uani 1 d . . . 
P1 P 0.26113(7) -0.00711(16) -0.08667(7) 0.0280(3) Uani 1 d . . . 
P2 P 0.35683(7) 0.15778(16) 0.09394(7) 0.0288(3) Uani 1 d . . . 
O1 O 0.4257(2) -0.1139(4) -0.0071(3) 0.0445(13) Uani 1 d . . . 
O2 O 0.3317(2) 0.2923(5) -0.1190(2) 0.0353(10) Uani 1 d . . . 
O3 O 0.4499(2) 0.2149(5) -0.0758(2) 0.0378(12) Uani 1 d . . . 
O4 O 0.3748(2) 0.3919(4) -0.01460(17) 0.0361(11) Uani 1 d . . . 
N1 N 0.1153(3) 0.1809(6) 0.0712(3) 0.0414(13) Uani 1 d . . . 
N2 N 0.4387(3) 0.4965(7) -0.1245(3) 0.0469(14) Uani 1 d . . . 
C1 C 0.3811(3) -0.0372(6) -0.0053(4) 0.0307(12) Uani 1 d . . . 
C2 C 0.1757(3) 0.1472(6) 0.0500(3) 0.0299(12) Uani 1 d . . . 
C3 C 0.0855(4) 0.3079(9) 0.0584(4) 0.061(2) Uani 1 d . . . 
H3A H 0.0918 0.3292 0.0162 0.092 Uiso 1 calc R . . 
H3B H 0.1067 0.3766 0.0829 0.092 Uiso 1 calc R . . 
H3C H 0.0379 0.3042 0.0675 0.092 Uiso 1 calc R . . 
C4 C 0.0816(5) 0.0976(11) 0.1151(5) 0.069(3) Uani 1 d . . . 
H4A H 0.0877 0.0036 0.1047 0.103 Uiso 1 calc R . . 
H4B H 0.0341 0.1188 0.1154 0.103 Uiso 1 calc R . . 
H4C H 0.1005 0.1143 0.1546 0.103 Uiso 1 calc R . . 
C5 C 0.3212(4) 0.4283(8) -0.1379(4) 0.0421(18) Uani 1 d . . . 
H5A H 0.3071 0.4821 -0.1032 0.051 Uiso 1 calc R . . 
H5B H 0.2847 0.4303 -0.1676 0.051 Uiso 1 calc R . . 
C6 C 0.3835(4) 0.4912(8) -0.1655(3) 0.0494(18) Uani 1 d . . . 
H6A H 0.3968 0.4392 -0.2010 0.059 Uiso 1 calc R . . 
H6B H 0.3728 0.5827 -0.1788 0.059 Uiso 1 calc R . . 
C7 C 0.4796(4) 0.2566(9) -0.1300(4) 0.055(2) Uani 1 d . . . 
H7A H 0.4492 0.2348 -0.1632 0.066 Uiso 1 calc R . . 
H7B H 0.5212 0.2059 -0.1361 0.066 Uiso 1 calc R . . 
C8 C 0.4956(4) 0.4065(8) -0.1320(4) 0.049(2) Uani 1 d . . . 
H8A H 0.5285 0.4263 -0.1004 0.059 Uiso 1 calc R . . 
H8B H 0.5169 0.4265 -0.1707 0.059 Uiso 1 calc R . . 
C9 C 0.4279(3) 0.4880(7) -0.0130(3) 0.0463(19) Uani 1 d . . . 
H9A H 0.4705 0.4406 -0.0071 0.056 Uiso 1 calc R . . 
H9B H 0.4211 0.5476 0.0216 0.056 Uiso 1 calc R . . 
C10 C 0.4328(4) 0.5717(7) -0.0688(3) 0.0461(17) Uani 1 d . . . 
H10A H 0.3928 0.6289 -0.0713 0.055 Uiso 1 calc R . . 
H10B H 0.4719 0.6309 -0.0651 0.055 Uiso 1 calc R . . 
C11 C 0.3108(3) -0.0344(6) -0.1557(3) 0.0308(12) Uani 1 d . . . 
C12 C 0.2791(4) -0.0569(8) -0.2108(3) 0.0452(17) Uani 1 d . . . 
H12A H 0.2325 -0.0440 -0.2143 0.054 Uiso 1 calc R . . 
C13 C 0.3163(4) -0.0988(9) -0.2610(3) 0.055(2) Uani 1 d . . . 
H13A H 0.2945 -0.1169 -0.2977 0.066 Uiso 1 calc R . . 
C14 C 0.3844(5) -0.1131(9) -0.2563(4) 0.055(2) Uani 1 d . . . 
H14A H 0.4095 -0.1406 -0.2899 0.066 Uiso 1 calc R . . 
C15 C 0.4158(4) -0.0879(9) -0.2034(4) 0.053(2) Uani 1 d . . . 
H15A H 0.4626 -0.0979 -0.2007 0.063 Uiso 1 calc R . . 
C16 C 0.3792(3) -0.0470(8) -0.1526(3) 0.0379(16) Uani 1 d . . . 
H16A H 0.4017 -0.0283 -0.1163 0.045 Uiso 1 calc R . . 
C21 C 0.1856(3) 0.0810(7) -0.1126(3) 0.0340(13) Uani 1 d . . . 
C22 C 0.1907(3) 0.1857(7) -0.1538(3) 0.0395(15) Uani 1 d . . . 
H22A H 0.2324 0.2043 -0.1717 0.047 Uiso 1 calc R . . 
C23 C 0.1354(4) 0.2632(8) -0.1689(4) 0.0499(19) Uani 1 d . . . 
H23A H 0.1396 0.3334 -0.1969 0.060 Uiso 1 calc R . . 
C24 C 0.0742(4) 0.2366(9) -0.1425(4) 0.056(2) Uani 1 d . . . 
H24A H 0.0369 0.2908 -0.1515 0.067 Uiso 1 calc R . . 
C25 C 0.0672(4) 0.1274(12) -0.1015(4) 0.056(3) Uani 1 d . . . 
H25A H 0.0251 0.1055 -0.0850 0.067 Uiso 1 calc R . . 
C26 C 0.1241(4) 0.0541(8) -0.0865(3) 0.0501(19) Uani 1 d . . . 
H26A H 0.1207 -0.0154 -0.0580 0.060 Uiso 1 calc R . . 
C31 C 0.2303(3) -0.1805(7) -0.0767(3) 0.0381(15) Uani 1 d . . . 
C32 C 0.1875(4) -0.2368(8) -0.1202(4) 0.058(2) Uani 1 d . . . 
H32A H 0.1737 -0.1847 -0.1533 0.070 Uiso 1 calc R . . 
C33 C 0.1656(4) -0.3670(8) -0.1148(4) 0.056(2) Uani 1 d . . . 
H33A H 0.1398 -0.4055 -0.1457 0.067 Uiso 1 calc R . . 
C34 C 0.1809(4) -0.4417(7) -0.0648(4) 0.0487(18) Uani 1 d . . . 
H34A H 0.1625 -0.5280 -0.0598 0.058 Uiso 1 calc R . . 
C35 C 0.2234(4) -0.3892(7) -0.0219(3) 0.0451(17) Uani 1 d . . . 
H35A H 0.2360 -0.4414 0.0115 0.054 Uiso 1 calc R . . 
C36 C 0.2479(3) -0.2587(6) -0.0280(3) 0.0358(13) Uani 1 d . . . 
H36A H 0.2768 -0.2235 0.0015 0.043 Uiso 1 calc R . . 
C41 C 0.3024(3) 0.2713(7) 0.1364(3) 0.0311(14) Uani 1 d . . . 
C42 C 0.2981(4) 0.4082(8) 0.1198(3) 0.0394(18) Uani 1 d . . . 
H42A H 0.3261 0.4417 0.0892 0.047 Uiso 1 calc R . . 
C43 C 0.2538(4) 0.4921(7) 0.1475(3) 0.0437(16) Uani 1 d . . . 
H43A H 0.2521 0.5833 0.1365 0.052 Uiso 1 calc R . . 
C44 C 0.2119(4) 0.4450(8) 0.1912(3) 0.0530(19) Uani 1 d . . . 
H44A H 0.1814 0.5037 0.2099 0.064 Uiso 1 calc R . . 
C45 C 0.2141(4) 0.3109(9) 0.2081(3) 0.0500(18) Uani 1 d . . . 
H45A H 0.1850 0.2788 0.2382 0.060 Uiso 1 calc R . . 
C46 C 0.2590(3) 0.2246(7) 0.1807(3) 0.0375(14) Uani 1 d . . . 
H46A H 0.2603 0.1336 0.1921 0.045 Uiso 1 calc R . . 
C51 C 0.4399(4) 0.2376(7) 0.0980(3) 0.0360(16) Uani 1 d . . . 
C52 C 0.4894(3) 0.1941(7) 0.0592(3) 0.0395(15) Uani 1 d . . . 
H52A H 0.4791 0.1291 0.0299 0.047 Uiso 1 calc R . . 
C53 C 0.5554(3) 0.2462(8) 0.0629(4) 0.055(2) Uani 1 d . . . 
H53A H 0.5888 0.2161 0.0362 0.066 Uiso 1 calc R . . 
C54 C 0.5701(4) 0.3403(8) 0.1054(4) 0.057(2) Uani 1 d . . . 
H54A H 0.6143 0.3730 0.1086 0.068 Uiso 1 calc R . . 
C55 C 0.5221(5) 0.3876(9) 0.1432(5) 0.063(3) Uani 1 d . . . 
H55A H 0.5332 0.4537 0.1717 0.075 Uiso 1 calc R . . 
C56 C 0.4555(4) 0.3383(8) 0.1401(3) 0.0450(16) Uani 1 d . . . 
H56A H 0.4222 0.3725 0.1658 0.054 Uiso 1 calc R . . 
C61 C 0.3725(3) 0.0202(7) 0.1480(3) 0.0325(14) Uani 1 d . . . 
C62 C 0.3610(4) -0.1143(7) 0.1332(3) 0.0403(16) Uani 1 d . . . 
H62A H 0.3420 -0.1358 0.0957 0.048 Uiso 1 calc R . . 
C63 C 0.3770(4) -0.2158(8) 0.1728(4) 0.0520(19) Uani 1 d . . . 
H63A H 0.3692 -0.3057 0.1617 0.062 Uiso 1 calc R . . 
C64 C 0.4043(4) -0.1881(8) 0.2282(3) 0.0497(19) Uani 1 d . . . 
H64A H 0.4154 -0.2579 0.2549 0.060 Uiso 1 calc R . . 
C65 C 0.4151(4) -0.0557(9) 0.2439(4) 0.0492(19) Uani 1 d . . . 
H65A H 0.4326 -0.0349 0.2820 0.059 Uiso 1 calc R . . 
C66 C 0.4004(4) 0.0470(7) 0.2038(3) 0.0429(16) Uani 1 d . . . 
H66A H 0.4096 0.1364 0.2147 0.051 Uiso 1 calc 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 
Os 0.02226(8) 0.03202(9) 0.02396(8) -0.00070(15) 0.00045(15) -0.00229(8) 
Si 0.0255(8) 0.0397(9) 0.0265(8) 0.0004(7) 0.0003(6) -0.0042(7) 
S1 0.0312(6) 0.0348(6) 0.0327(9) 0.0008(8) -0.0012(8) 0.0010(5) 
S2 0.0284(7) 0.0325(7) 0.0317(7) 0.0005(6) 0.0040(6) -0.0028(6) 
P1 0.0217(7) 0.0374(8) 0.0250(7) -0.0009(6) 0.0003(6) -0.0022(6) 
P2 0.0245(7) 0.0343(8) 0.0277(7) -0.0007(6) -0.0030(6) -0.0040(6) 
O1 0.043(2) 0.048(2) 0.043(4) -0.008(3) 0.001(3) 0.0097(18) 
O2 0.033(2) 0.042(3) 0.032(2) 0.0024(19) -0.004(2) -0.007(2) 
O3 0.026(2) 0.050(3) 0.037(3) 0.005(2) 0.005(2) -0.002(2) 
O4 0.038(2) 0.039(2) 0.031(3) -0.0012(16) 0.0031(17) -0.0097(18) 
N1 0.032(3) 0.048(3) 0.045(3) -0.005(3) 0.006(3) 0.002(2) 
N2 0.043(3) 0.054(4) 0.044(3) -0.004(3) 0.008(3) -0.001(3) 
C1 0.028(2) 0.041(3) 0.024(3) -0.003(3) -0.003(3) -0.004(2) 
C2 0.024(3) 0.036(3) 0.030(3) -0.008(2) 0.003(2) 0.000(2) 
C3 0.045(4) 0.063(5) 0.075(6) -0.007(5) 0.007(4) 0.015(4) 
C4 0.034(5) 0.086(7) 0.086(8) -0.015(6) 0.019(5) -0.002(4) 
C5 0.035(4) 0.047(4) 0.044(5) -0.001(3) -0.001(3) 0.004(3) 
C6 0.061(5) 0.053(4) 0.034(4) 0.005(3) -0.005(3) 0.000(4) 
C7 0.041(4) 0.072(6) 0.052(4) -0.008(4) 0.024(4) 0.005(4) 
C8 0.039(5) 0.058(5) 0.052(5) 0.004(4) 0.010(4) -0.004(4) 
C9 0.047(4) 0.048(4) 0.044(5) -0.005(3) 0.003(3) -0.019(3) 
C10 0.051(4) 0.045(4) 0.042(4) -0.007(3) 0.006(3) -0.018(3) 
C11 0.032(3) 0.033(3) 0.027(3) -0.001(2) 0.003(3) -0.001(3) 
C12 0.041(4) 0.061(5) 0.034(3) -0.004(3) -0.001(3) 0.010(3) 
C13 0.058(5) 0.075(6) 0.033(4) -0.012(4) 0.000(3) 0.011(4) 
C14 0.054(5) 0.066(6) 0.043(4) -0.003(4) 0.012(4) 0.015(4) 
C15 0.036(4) 0.084(6) 0.038(4) -0.001(4) 0.007(3) 0.012(4) 
C16 0.029(3) 0.051(4) 0.034(4) -0.001(3) -0.001(3) -0.002(3) 
C21 0.023(3) 0.046(3) 0.033(3) -0.014(3) 0.000(2) -0.002(3) 
C22 0.032(3) 0.042(4) 0.044(4) -0.005(3) -0.004(3) 0.001(3) 
C23 0.050(4) 0.044(4) 0.056(5) -0.015(4) -0.018(4) 0.010(3) 
C24 0.037(4) 0.069(5) 0.062(5) -0.021(4) -0.012(4) 0.018(4) 
C25 0.017(4) 0.106(7) 0.044(4) -0.018(5) 0.001(3) 0.004(4) 
C26 0.037(4) 0.074(5) 0.040(4) -0.009(4) 0.000(3) -0.014(3) 
C31 0.034(3) 0.042(4) 0.038(3) -0.007(3) 0.003(3) -0.005(3) 
C32 0.073(6) 0.049(4) 0.052(4) 0.007(4) -0.021(4) -0.017(4) 
C33 0.051(4) 0.051(4) 0.066(5) -0.001(4) -0.016(4) -0.010(4) 
C34 0.040(4) 0.038(4) 0.067(5) -0.001(3) -0.002(4) -0.007(3) 
C35 0.055(4) 0.040(4) 0.041(4) 0.007(3) 0.003(3) 0.008(3) 
C36 0.034(3) 0.036(3) 0.038(3) -0.005(3) -0.001(3) 0.001(3) 
C41 0.028(3) 0.040(4) 0.025(3) -0.004(3) -0.002(3) -0.001(3) 
C42 0.034(4) 0.046(4) 0.038(4) -0.005(3) -0.006(3) -0.004(3) 
C43 0.054(4) 0.037(4) 0.040(4) -0.006(3) -0.007(3) 0.007(3) 
C44 0.058(5) 0.061(5) 0.039(4) -0.008(4) -0.004(4) 0.014(4) 
C45 0.043(4) 0.071(5) 0.036(4) -0.005(3) 0.004(3) 0.003(4) 
C46 0.035(3) 0.044(4) 0.033(3) -0.002(3) -0.003(3) -0.003(3) 
C51 0.035(4) 0.041(4) 0.032(4) 0.005(3) -0.006(3) -0.004(3) 
C52 0.030(3) 0.041(4) 0.047(4) 0.009(3) 0.003(3) -0.003(3) 
C53 0.024(3) 0.061(5) 0.081(6) 0.012(4) -0.004(4) -0.005(3) 
C54 0.029(4) 0.052(5) 0.089(6) 0.011(4) -0.026(4) -0.012(3) 
C55 0.053(6) 0.051(5) 0.083(7) 0.008(5) -0.021(5) -0.018(4) 
C56 0.044(4) 0.046(4) 0.045(4) -0.002(3) -0.011(3) -0.009(3) 
C61 0.031(3) 0.039(4) 0.027(3) 0.004(3) -0.002(3) -0.001(3) 
C62 0.041(4) 0.044(4) 0.036(4) 0.001(3) -0.008(3) -0.004(3) 
C63 0.058(5) 0.043(4) 0.055(5) 0.012(3) -0.009(4) -0.002(3) 
C64 0.051(4) 0.054(4) 0.044(4) 0.020(4) -0.011(3) 0.001(4) 
C65 0.043(4) 0.064(5) 0.040(4) 0.006(4) -0.016(3) -0.007(4) 
C66 0.050(4) 0.047(4) 0.032(3) 0.004(3) -0.011(3) -0.006(3) 
 
_geom_special_details 
; 
 ?
;
 
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 
Os C1 1.843(6) . ? 
Os P2 2.3723(15) . ? 
Os P1 2.3725(15) . ? 
Os Si 2.3783(17) . ? 
Os S1 2.4593(14) . ? 
Os S2 2.5431(15) . ? 
Si O3 1.664(5) . ? 
Si O4 1.665(4) . ? 
Si O2 1.674(5) . ? 
S1 C2 1.708(6) . ? 
S2 C2 1.716(6) . ? 
P1 C21 1.833(6) . ? 
P1 C31 1.844(7) . ? 
P1 C11 1.845(6) . ? 
P2 C41 1.828(7) . ? 
P2 C51 1.837(7) . ? 
P2 C61 1.848(6) . ? 
O1 C1 1.171(7) . ? 
O2 C5 1.432(9) . ? 
O3 C7 1.404(8) . ? 
O4 C9 1.426(7) . ? 
N1 C2 1.333(7) . ? 
N1 C3 1.424(10) . ? 
N1 C4 1.445(12) . ? 
N2 C6 1.428(9) . ? 
N2 C10 1.451(9) . ? 
N2 C8 1.453(10) . ? 
C5 C6 1.519(11) . ? 
C7 C8 1.525(11) . ? 
C9 C10 1.495(10) . ? 
C11 C16 1.369(9) . ? 
C11 C12 1.397(9) . ? 
C12 C13 1.403(10) . ? 
C13 C14 1.367(11) . ? 
C14 C15 1.355(11) . ? 
C15 C16 1.406(10) . ? 
C21 C26 1.382(9) . ? 
C21 C22 1.390(10) . ? 
C22 C23 1.386(9) . ? 
C23 C24 1.378(11) . ? 
C24 C25 1.424(14) . ? 
C25 C26 1.387(12) . ? 
C31 C36 1.379(9) . ? 
C31 C32 1.405(9) . ? 
C32 C33 1.372(11) . ? 
C33 C34 1.370(11) . ? 
C34 C35 1.379(10) . ? 
C35 C36 1.392(9) . ? 
C41 C46 1.389(9) . ? 
C41 C42 1.413(10) . ? 
C42 C43 1.361(10) . ? 
C43 C44 1.363(11) . ? 
C44 C45 1.386(11) . ? 
C45 C46 1.381(10) . ? 
C51 C52 1.379(10) . ? 
C51 C56 1.405(10) . ? 
C52 C53 1.415(9) . ? 
C53 C54 1.362(12) . ? 
C54 C55 1.356(14) . ? 
C55 C56 1.416(11) . ? 
C61 C66 1.385(9) . ? 
C61 C62 1.396(9) . ? 
C62 C63 1.376(10) . ? 
C63 C64 1.375(10) . ? 
C64 C65 1.378(11) . ? 
C65 C66 1.386(10) . ? 
 
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 
C1 Os P2 88.9(2) . . ? 
C1 Os P1 90.3(2) . . ? 
P2 Os P1 173.26(5) . . ? 
C1 Os Si 92.9(2) . . ? 
P2 Os Si 93.38(5) . . ? 
P1 Os Si 93.34(5) . . ? 
C1 Os S1 178.34(18) . . ? 
P2 Os S1 91.00(6) . . ? 
P1 Os S1 89.99(6) . . ? 
Si Os S1 85.40(6) . . ? 
C1 Os S2 112.0(2) . . ? 
P2 Os S2 85.09(5) . . ? 
P1 Os S2 89.01(5) . . ? 
Si Os S2 154.98(6) . . ? 
S1 Os S2 69.67(5) . . ? 
O3 Si O4 107.3(2) . . ? 
O3 Si O2 105.5(2) . . ? 
O4 Si O2 105.8(2) . . ? 
O3 Si Os 117.3(2) . . ? 
O4 Si Os 108.53(15) . . ? 
O2 Si Os 111.80(18) . . ? 
C2 S1 Os 90.0(2) . . ? 
C2 S2 Os 87.1(2) . . ? 
C21 P1 C31 102.2(3) . . ? 
C21 P1 C11 104.4(3) . . ? 
C31 P1 C11 98.1(3) . . ? 
C21 P1 Os 114.9(2) . . ? 
C31 P1 Os 114.1(2) . . ? 
C11 P1 Os 120.4(2) . . ? 
C41 P2 C51 104.0(3) . . ? 
C41 P2 C61 102.8(3) . . ? 
C51 P2 C61 97.8(3) . . ? 
C41 P2 Os 114.6(2) . . ? 
C51 P2 Os 120.8(2) . . ? 
C61 P2 Os 114.2(2) . . ? 
C5 O2 Si 123.2(4) . . ? 
C7 O3 Si 124.4(5) . . ? 
C9 O4 Si 127.1(4) . . ? 
C2 N1 C3 121.9(6) . . ? 
C2 N1 C4 120.9(6) . . ? 
C3 N1 C4 116.7(6) . . ? 
C6 N2 C10 120.0(6) . . ? 
C6 N2 C8 120.3(6) . . ? 
C10 N2 C8 118.6(7) . . ? 
O1 C1 Os 177.7(7) . . ? 
N1 C2 S1 122.0(5) . . ? 
N1 C2 S2 124.8(5) . . ? 
S1 C2 S2 113.2(3) . . ? 
O2 C5 C6 112.8(6) . . ? 
N2 C6 C5 112.8(6) . . ? 
O3 C7 C8 113.7(7) . . ? 
N2 C8 C7 115.8(7) . . ? 
O4 C9 C10 113.7(5) . . ? 
N2 C10 C9 115.2(6) . . ? 
C16 C11 C12 118.7(6) . . ? 
C16 C11 P1 120.3(5) . . ? 
C12 C11 P1 120.6(5) . . ? 
C11 C12 C13 120.4(7) . . ? 
C14 C13 C12 119.6(7) . . ? 
C15 C14 C13 120.3(7) . . ? 
C14 C15 C16 120.8(7) . . ? 
C11 C16 C15 120.1(7) . . ? 
C26 C21 C22 119.0(7) . . ? 
C26 C21 P1 120.2(6) . . ? 
C22 C21 P1 120.4(5) . . ? 
C23 C22 C21 121.2(7) . . ? 
C24 C23 C22 119.5(8) . . ? 
C23 C24 C25 120.3(7) . . ? 
C26 C25 C24 118.3(8) . . ? 
C21 C26 C25 121.4(8) . . ? 
C36 C31 C32 118.0(6) . . ? 
C36 C31 P1 122.5(5) . . ? 
C32 C31 P1 119.5(5) . . ? 
C33 C32 C31 120.6(7) . . ? 
C34 C33 C32 120.8(7) . . ? 
C33 C34 C35 119.5(7) . . ? 
C34 C35 C36 120.0(6) . . ? 
C31 C36 C35 120.9(6) . . ? 
C46 C41 C42 118.0(6) . . ? 
C46 C41 P2 121.9(5) . . ? 
C42 C41 P2 119.8(5) . . ? 
C43 C42 C41 120.8(7) . . ? 
C42 C43 C44 120.5(7) . . ? 
C43 C44 C45 120.3(7) . . ? 
C46 C45 C44 119.9(7) . . ? 
C45 C46 C41 120.5(7) . . ? 
C52 C51 C56 118.8(7) . . ? 
C52 C51 P2 118.5(5) . . ? 
C56 C51 P2 122.7(6) . . ? 
C51 C52 C53 120.8(7) . . ? 
C54 C53 C52 119.5(8) . . ? 
C55 C54 C53 121.1(7) . . ? 
C54 C55 C56 120.6(8) . . ? 
C51 C56 C55 119.1(8) . . ? 
C66 C61 C62 117.5(6) . . ? 
C66 C61 P2 120.5(5) . . ? 
C62 C61 P2 121.9(5) . . ? 
C63 C62 C61 121.0(7) . . ? 
C64 C63 C62 121.1(7) . . ? 
C63 C64 C65 118.7(7) . . ? 
C64 C65 C66 120.6(7) . . ? 
C61 C66 C65 121.2(7) . . ? 
 
_diffrn_measured_fraction_theta_max    0.982 
_diffrn_reflns_theta_full              27.49 
_diffrn_measured_fraction_theta_full   0.982 
_refine_diff_density_max    1.648 
_refine_diff_density_min   -1.455 
_refine_diff_density_rms    0.104 

#==END