# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name "Ol'ga Kizas" _publ_contact_author_email KIZAS@INEOS.AC.RU _publ_section_title ; Reactions of H2Os3(CO)10 with Triallylborane. Formation of novel Triosmium Boron-Containing Olefin Clusters ; loop_ _publ_author_name "Ol'ga Kizas" 'Dmitrii Yu. Antonov' 'Irina G Barakovskaya' 'Yurii N Bubnov' ; F.M.Dolgushin ; 'Sergey Yu. Erdyakov' 'Mariam G. Ezernitskaya' 'Ivan A. Godovikov' 'Evgenii V. Vorontsov' # Attachment 'complex2.CIF' data_osrem _database_code_depnum_ccdc_archive 'CCDC 694582' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H17 B O10 Os3' _chemical_formula_sum 'C19 H17 B O10 Os3' _chemical_formula_weight 986.74 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' B B 0.0013 0.0007 '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' 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 '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 9.5816(7) _cell_length_b 28.057(2) _cell_length_c 9.7448(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.8310(10) _cell_angle_gamma 90.00 _cell_volume 2377.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 115(2) _cell_measurement_reflns_used 6191 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 30.0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 16.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.127 _exptl_absorpt_correction_T_max 0.265 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 115(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18626 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 30.02 _reflns_number_total 6820 _reflns_number_gt 5033 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystals had poor quality (small piece of irregular shape) in addition to their high absorption. Analytical (face indexing procedure) absorption correction was not applicable. Thus, the ADP's of some light atoms in vicinity of Os atoms were poorly determined. To prevent the non-positive values of ADP the ISOR instruction for two atoms (C11 and B1) was applied in refinement. The weighting scheme was chose proceeding from necessity to remove high residual peak (6 e/A3) at the osmium atoms (distances 0.01 A). For this purpose it was necessary to reduce the first parameter in the weight scheme and to keep GOF close to unit increase the second parameter in the weight scheme. Both problems, and uncertainty with anisotropic parameters of some atoms, and the overestimated value of the second parameter in the weighting scheme, are in our opinion caused by considerable absorption effects which could not be completely corrected. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+27.3000P] 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 6820 _refine_ls_number_parameters 301 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.53554(4) 0.094282(11) 0.79937(4) 0.01737(9) Uani 1 1 d . . . Os2 Os 0.70469(4) 0.134971(11) 0.63560(4) 0.01645(9) Uani 1 1 d . . . Os3 Os 0.86280(4) 0.109118(12) 0.94922(4) 0.02125(9) Uani 1 1 d . . . O1 O 0.5698(8) -0.0050(2) 0.6853(8) 0.0288(15) Uani 1 1 d . . . O2 O 0.4905(8) 0.1940(2) 0.9069(8) 0.0289(16) Uani 1 1 d . . . O3 O 0.5199(11) 0.0486(3) 1.0741(9) 0.042(2) Uani 1 1 d . . . O4 O 0.7536(8) 0.0370(2) 0.5205(8) 0.0291(16) Uani 1 1 d . . . O5 O 0.6699(8) 0.2364(2) 0.7369(8) 0.0270(15) Uani 1 1 d . . . O6 O 0.9856(9) 0.1679(3) 0.5978(10) 0.042(2) Uani 1 1 d . . . O7 O 0.9015(9) 0.0091(3) 0.8410(9) 0.0389(19) Uani 1 1 d . . . O8 O 0.8254(9) 0.2098(3) 1.0542(9) 0.0370(18) Uani 1 1 d . . . O9 O 1.1942(10) 0.1305(3) 1.0069(12) 0.052(2) Uani 1 1 d . . . O10 O 0.9206(11) 0.0710(3) 1.2617(10) 0.050(2) Uani 1 1 d . . . C1 C 0.5620(11) 0.0316(3) 0.7275(11) 0.0198(18) Uani 1 1 d . . . C2 C 0.5112(10) 0.1576(3) 0.8654(10) 0.0189(18) Uani 1 1 d . . . C3 C 0.5263(12) 0.0662(3) 0.9726(12) 0.029(2) Uani 1 1 d . . . C4 C 0.7321(10) 0.0726(3) 0.5661(10) 0.0225(19) Uani 1 1 d . . . C5 C 0.6805(11) 0.1979(3) 0.7032(11) 0.024(2) Uani 1 1 d . . . C6 C 0.8822(11) 0.1550(3) 0.6147(11) 0.0219(19) Uani 1 1 d . . . C7 C 0.8817(11) 0.0456(4) 0.8736(11) 0.026(2) Uani 1 1 d . . . C8 C 0.8351(11) 0.1725(3) 1.0120(11) 0.024(2) Uani 1 1 d . . . C9 C 1.0726(14) 0.1235(4) 0.9868(12) 0.032(2) Uani 1 1 d . . . C10 C 0.8981(13) 0.0849(4) 1.1454(12) 0.033(2) Uani 1 1 d . . . C11 C 0.3288(10) 0.0950(3) 0.5776(10) 0.0211(19) Uani 1 1 d U . . H11A H 0.3135 0.0657 0.5144 0.025 Uiso 1 1 calc R . . C12 C 0.2698(11) 0.0927(4) 0.6875(12) 0.027(2) Uani 1 1 d . . . H12A H 0.2226 0.1233 0.6991 0.032 Uiso 1 1 calc R . . C13 C 0.1919(13) 0.0493(4) 0.7158(15) 0.039(3) Uani 1 1 d . . . H13A H 0.0822 0.0499 0.6479 0.059 Uiso 1 1 calc R . . H13B H 0.2046 0.0494 0.8210 0.059 Uiso 1 1 calc R . . H13C H 0.2386 0.0204 0.6970 0.059 Uiso 1 1 calc R . . C14 C 0.4800(11) 0.1310(3) 0.4305(10) 0.0231(19) Uani 1 1 d . . . H14A H 0.4584 0.1003 0.3729 0.028 Uiso 1 1 calc R . . C15 C 0.5671(12) 0.1641(3) 0.3945(11) 0.027(2) Uani 1 1 d . . . H15A H 0.5315 0.1977 0.3921 0.032 Uiso 1 1 calc R . . C16 C 0.6284(15) 0.1538(4) 0.2789(12) 0.037(3) Uani 1 1 d . . . H16A H 0.5538 0.1645 0.1792 0.055 Uiso 1 1 calc R . . H16B H 0.6454 0.1194 0.2760 0.055 Uiso 1 1 calc R . . H16C H 0.7258 0.1707 0.3059 0.055 Uiso 1 1 calc R . . C17 C 0.3185(11) 0.1913(4) 0.5319(12) 0.030(2) Uani 1 1 d . . . H17A H 0.2928 0.1923 0.6203 0.036 Uiso 1 1 calc R . . H17B H 0.3960 0.2163 0.5450 0.036 Uiso 1 1 calc R . . C18 C 0.1738(13) 0.2003(4) 0.3867(13) 0.032(2) Uani 1 1 d . . . H18A H 0.2009 0.1995 0.2992 0.039 Uiso 1 1 calc R . . H18B H 0.0985 0.1746 0.3731 0.039 Uiso 1 1 calc R . . C19 C 0.1007(14) 0.2482(4) 0.3903(14) 0.044(3) Uani 1 1 d . . . H19A H -0.0029 0.2495 0.3080 0.066 Uiso 1 1 calc R . . H19B H 0.1635 0.2739 0.3776 0.066 Uiso 1 1 calc R . . H19C H 0.0943 0.2519 0.4874 0.066 Uiso 1 1 calc R . . B1 B 0.3864(11) 0.1401(4) 0.5210(12) 0.022(2) Uani 1 1 d U . . 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 0.01900(17) 0.01634(15) 0.01777(18) 0.00024(13) 0.00872(14) -0.00067(12) Os2 0.01693(17) 0.01625(15) 0.01652(18) 0.00030(12) 0.00736(14) 0.00005(12) Os3 0.01917(18) 0.02284(17) 0.01759(19) 0.00039(14) 0.00364(15) 0.00270(13) O1 0.037(4) 0.021(3) 0.031(4) -0.005(3) 0.016(3) 0.000(3) O2 0.037(4) 0.021(3) 0.032(4) 0.000(3) 0.018(3) 0.002(3) O3 0.074(6) 0.032(4) 0.033(5) 0.001(3) 0.034(5) -0.007(4) O4 0.039(4) 0.021(3) 0.029(4) -0.005(3) 0.016(3) 0.004(3) O5 0.033(4) 0.022(3) 0.028(4) -0.008(3) 0.016(3) -0.002(3) O6 0.039(5) 0.040(4) 0.057(6) 0.002(4) 0.031(4) -0.002(4) O7 0.044(5) 0.027(4) 0.030(4) -0.003(3) 0.000(4) 0.015(3) O8 0.039(5) 0.034(4) 0.035(4) -0.012(3) 0.012(4) 0.000(3) O9 0.026(5) 0.047(5) 0.079(7) -0.009(5) 0.017(5) -0.010(4) O10 0.073(7) 0.045(5) 0.029(5) 0.014(4) 0.019(5) 0.011(4) C1 0.023(5) 0.019(4) 0.021(5) 0.001(3) 0.014(4) -0.001(3) C2 0.016(4) 0.026(4) 0.010(4) -0.001(3) 0.001(3) 0.001(3) C3 0.034(6) 0.026(5) 0.026(6) 0.002(4) 0.012(5) 0.000(4) C4 0.017(4) 0.026(5) 0.017(5) 0.006(4) 0.000(4) 0.002(4) C5 0.027(5) 0.030(5) 0.019(5) 0.007(4) 0.011(4) 0.002(4) C6 0.020(5) 0.026(4) 0.022(5) 0.000(4) 0.010(4) 0.001(4) C7 0.021(5) 0.036(5) 0.012(5) -0.002(4) -0.003(4) 0.005(4) C8 0.021(5) 0.027(5) 0.018(5) 0.004(4) 0.002(4) 0.003(4) C9 0.038(6) 0.034(5) 0.017(5) 0.003(4) 0.005(5) 0.007(5) C10 0.037(6) 0.042(6) 0.015(5) -0.003(4) 0.006(5) 0.008(5) C11 0.011(4) 0.023(4) 0.017(4) -0.001(3) -0.006(3) 0.005(3) C12 0.022(5) 0.035(5) 0.031(6) -0.004(4) 0.018(4) -0.010(4) C13 0.032(6) 0.026(5) 0.071(9) -0.007(5) 0.033(6) -0.008(4) C14 0.027(5) 0.020(4) 0.016(5) 0.001(3) 0.003(4) 0.003(4) C15 0.032(6) 0.023(4) 0.025(5) 0.005(4) 0.011(4) 0.004(4) C16 0.066(8) 0.027(5) 0.021(5) 0.004(4) 0.022(6) 0.008(5) C17 0.021(5) 0.031(5) 0.030(6) 0.005(4) 0.005(4) 0.001(4) C18 0.033(6) 0.030(5) 0.033(6) -0.001(4) 0.014(5) 0.005(4) C19 0.032(6) 0.040(6) 0.042(7) -0.001(5) -0.003(5) 0.013(5) B1 0.009(4) 0.031(5) 0.021(5) 0.002(4) 0.001(4) 0.002(4) _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 C3 1.898(10) . ? Os1 C2 1.937(9) . ? Os1 C1 1.948(9) . ? Os1 C11 2.236(9) . ? Os1 C12 2.311(10) . ? Os1 Os3 2.8797(5) . ? Os1 Os2 2.9410(5) . ? Os2 C6 1.881(9) . ? Os2 C5 1.933(10) . ? Os2 C4 1.934(10) . ? Os2 C14 2.242(9) . ? Os2 C15 2.308(10) . ? Os2 Os3 2.8763(5) . ? Os3 C10 1.921(11) . ? Os3 C9 1.929(12) . ? Os3 C8 1.935(10) . ? Os3 C7 1.965(10) . ? O1 C1 1.120(10) . ? O2 C2 1.145(11) . ? O3 C3 1.131(12) . ? O4 C4 1.146(11) . ? O5 C5 1.145(11) . ? O6 C6 1.131(11) . ? O7 C7 1.113(11) . ? O8 C8 1.142(11) . ? O9 C9 1.115(13) . ? O10 C10 1.130(13) . ? C11 C12 1.407(14) . ? C11 B1 1.571(14) . ? C11 H11A 1.0000 . ? C12 C13 1.513(13) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.390(13) . ? C14 B1 1.520(14) . ? C14 H14A 1.0000 . ? C15 C16 1.500(14) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.530(14) . ? C17 B1 1.598(14) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.522(14) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 C3 Os1 C2 91.6(4) . . ? C3 Os1 C1 90.4(4) . . ? C2 Os1 C1 177.9(4) . . ? C3 Os1 C11 120.7(4) . . ? C2 Os1 C11 97.5(3) . . ? C1 Os1 C11 81.8(4) . . ? C3 Os1 C12 87.6(4) . . ? C2 Os1 C12 85.0(4) . . ? C1 Os1 C12 95.6(4) . . ? C11 Os1 C12 36.0(3) . . ? C3 Os1 Os3 93.2(3) . . ? C2 Os1 Os3 87.5(3) . . ? C1 Os1 Os3 92.0(3) . . ? C11 Os1 Os3 145.4(3) . . ? C12 Os1 Os3 172.4(3) . . ? C3 Os1 Os2 152.3(3) . . ? C2 Os1 Os2 89.7(3) . . ? C1 Os1 Os2 88.3(3) . . ? C11 Os1 Os2 86.5(3) . . ? C12 Os1 Os2 120.0(2) . . ? Os3 Os1 Os2 59.216(13) . . ? C6 Os2 C5 90.4(4) . . ? C6 Os2 C4 88.3(4) . . ? C5 Os2 C4 178.7(4) . . ? C6 Os2 C14 119.5(4) . . ? C5 Os2 C14 98.1(4) . . ? C4 Os2 C14 82.2(4) . . ? C6 Os2 C15 86.6(4) . . ? C5 Os2 C15 85.7(4) . . ? C4 Os2 C15 93.9(4) . . ? C14 Os2 C15 35.5(3) . . ? C6 Os2 Os3 95.4(3) . . ? C5 Os2 Os3 87.3(3) . . ? C4 Os2 Os3 93.2(3) . . ? C14 Os2 Os3 144.5(2) . . ? C15 Os2 Os3 172.8(2) . . ? C6 Os2 Os1 154.6(3) . . ? C5 Os2 Os1 89.9(3) . . ? C4 Os2 Os1 91.5(3) . . ? C14 Os2 Os1 85.6(3) . . ? C15 Os2 Os1 118.7(3) . . ? Os3 Os2 Os1 59.329(13) . . ? C10 Os3 C9 98.7(5) . . ? C10 Os3 C8 90.1(4) . . ? C9 Os3 C8 91.0(4) . . ? C10 Os3 C7 92.7(4) . . ? C9 Os3 C7 90.5(4) . . ? C8 Os3 C7 176.7(4) . . ? C10 Os3 Os2 160.2(4) . . ? C9 Os3 Os2 101.0(3) . . ? C8 Os3 Os2 91.3(3) . . ? C7 Os3 Os2 85.5(3) . . ? C10 Os3 Os1 98.8(4) . . ? C9 Os3 Os1 162.3(3) . . ? C8 Os3 Os1 91.6(3) . . ? C7 Os3 Os1 86.0(3) . . ? Os2 Os3 Os1 61.455(12) . . ? O1 C1 Os1 176.4(8) . . ? O2 C2 Os1 176.0(8) . . ? O3 C3 Os1 178.5(9) . . ? O4 C4 Os2 175.6(8) . . ? O5 C5 Os2 175.5(8) . . ? O6 C6 Os2 177.5(9) . . ? O7 C7 Os3 174.7(9) . . ? O8 C8 Os3 176.8(9) . . ? O9 C9 Os3 177.9(10) . . ? O10 C10 Os3 179.0(12) . . ? C12 C11 B1 128.2(9) . . ? C12 C11 Os1 74.9(6) . . ? B1 C11 Os1 92.7(5) . . ? C12 C11 H11A 115.4 . . ? B1 C11 H11A 115.4 . . ? Os1 C11 H11A 115.4 . . ? C11 C12 C13 124.3(9) . . ? C11 C12 Os1 69.1(5) . . ? C13 C12 Os1 117.4(8) . . ? C11 C12 H12A 113.0 . . ? C13 C12 H12A 113.0 . . ? Os1 C12 H12A 113.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 B1 126.7(9) . . ? C15 C14 Os2 74.8(6) . . ? B1 C14 Os2 93.1(6) . . ? C15 C14 H14A 115.9 . . ? B1 C14 H14A 115.9 . . ? Os2 C14 H14A 115.9 . . ? C14 C15 C16 121.8(9) . . ? C14 C15 Os2 69.7(5) . . ? C16 C15 Os2 117.4(7) . . ? C14 C15 H15A 113.7 . . ? C16 C15 H15A 113.7 . . ? Os2 C15 H15A 113.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 B1 108.9(8) . . ? C18 C17 H17A 109.9 . . ? B1 C17 H17A 109.9 . . ? C18 C17 H17B 109.9 . . ? B1 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C19 C18 C17 111.9(9) . . ? C19 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? C19 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 B1 C11 116.6(8) . . ? C14 B1 C17 123.1(9) . . ? C11 B1 C17 119.2(8) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 3.195 _refine_diff_density_min -3.315 _refine_diff_density_rms 0.360 # Attachment 'complex3.CIF' data_osbx4 _database_code_depnum_ccdc_archive 'CCDC 694583' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H21 B O10 Os3' _chemical_formula_sum 'C21 H21 B O10 Os3' _chemical_formula_weight 1014.79 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' B B 0.0013 0.0007 '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' 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 'P 21/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 9.707(3) _cell_length_b 16.418(5) _cell_length_c 16.152(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.054(7) _cell_angle_gamma 90.00 _cell_volume 2554.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1010 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 29.0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 14.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.021 _exptl_absorpt_correction_T_max 0.099 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28722 _diffrn_reflns_av_R_equivalents 0.0742 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 30.01 _reflns_number_total 7365 _reflns_number_gt 5013 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The weighting scheme was chose proceeding from necessity to remove high residual peak (8 e/A3) at the osmium atoms (distances 0.01 A). For this purpose it was necessary to reduce the first parameter in the weight scheme and to keep GOF close to unit increase the second parameter in the weight scheme. The overestimated value of the second parameter in the weighting scheme, are in our opinion caused by considerable absorption effects which could not be completely corrected. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+46.7000P] 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 7365 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.003 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.76627(4) 0.29036(2) 0.41413(2) 0.02102(10) Uani 1 1 d . . . Os2 Os 0.55627(4) 0.22938(3) 0.51625(2) 0.02298(11) Uani 1 1 d . . . Os3 Os 0.76029(4) 0.12191(3) 0.46168(3) 0.02546(11) Uani 1 1 d . . . O1 O 0.9381(8) 0.3460(6) 0.5791(5) 0.040(2) Uani 1 1 d . . . O2 O 0.5944(9) 0.2365(5) 0.2500(5) 0.0315(18) Uani 1 1 d . . . O3 O 1.0288(10) 0.2725(7) 0.3303(6) 0.055(3) Uani 1 1 d . . . O4 O 0.7433(10) 0.2657(7) 0.6790(5) 0.050(3) Uani 1 1 d . . . O5 O 0.3623(8) 0.1824(5) 0.3587(4) 0.0296(17) Uani 1 1 d . . . O6 O 0.4103(11) 0.1067(6) 0.6144(6) 0.049(3) Uani 1 1 d . . . O7 O 0.9744(10) 0.1654(5) 0.6113(5) 0.041(2) Uani 1 1 d . . . O8 O 0.5680(9) 0.0697(5) 0.3040(5) 0.037(2) Uani 1 1 d . . . O9 O 0.6540(11) -0.0241(6) 0.5559(6) 0.054(3) Uani 1 1 d . . . O10 O 0.9990(12) 0.0494(8) 0.3813(8) 0.076(4) Uani 1 1 d . . . C1 C 0.8740(11) 0.3215(6) 0.5183(7) 0.024(2) Uani 1 1 d . . . C2 C 0.6528(10) 0.2560(6) 0.3122(6) 0.0197(19) Uani 1 1 d . . . C3 C 0.9279(12) 0.2784(8) 0.3635(8) 0.036(3) Uani 1 1 d . . . C4 C 0.6799(12) 0.2503(7) 0.6180(7) 0.030(2) Uani 1 1 d . . . C5 C 0.4367(11) 0.2025(7) 0.4150(6) 0.026(2) Uani 1 1 d . . . C6 C 0.4661(14) 0.1518(8) 0.5779(7) 0.037(3) Uani 1 1 d . . . C7 C 0.8926(13) 0.1505(7) 0.5573(7) 0.033(3) Uani 1 1 d . . . C8 C 0.6348(11) 0.0924(6) 0.3613(7) 0.026(2) Uani 1 1 d . . . C9 C 0.6949(13) 0.0316(7) 0.5209(7) 0.032(3) Uani 1 1 d . . . C10 C 0.9112(14) 0.0783(8) 0.4117(8) 0.040(3) Uani 1 1 d . . . C11 C 0.6713(10) 0.4149(6) 0.4261(6) 0.022(2) Uani 1 1 d . . . H11A H 0.7073 0.4434 0.4791 0.026 Uiso 1 1 calc R . . C12 C 0.7561(12) 0.4251(8) 0.3630(7) 0.032(3) Uani 1 1 d . . . C13 C 0.8907(12) 0.4729(8) 0.3831(8) 0.040(3) Uani 1 1 d . . . H13A H 0.8755 0.5297 0.3656 0.059 Uiso 1 1 calc R . . H13B H 0.9628 0.4489 0.3533 0.059 Uiso 1 1 calc R . . H13C H 0.9204 0.4709 0.4433 0.059 Uiso 1 1 calc R . . C131 C 0.7012(14) 0.4296(8) 0.2718(7) 0.038(3) Uani 1 1 d . . . H13D H 0.6807 0.4864 0.2563 0.058 Uiso 1 1 calc R . . H13E H 0.6162 0.3971 0.2612 0.058 Uiso 1 1 calc R . . H13F H 0.7710 0.4082 0.2385 0.058 Uiso 1 1 calc R . . C14 C 0.4919(13) 0.3607(7) 0.5184(7) 0.030(2) Uani 1 1 d . . . H14A H 0.5538 0.3936 0.5597 0.036 Uiso 1 1 calc R . . C15 C 0.3865(13) 0.3222(8) 0.5539(8) 0.036(3) Uani 1 1 d . . . C16 C 0.3854(15) 0.3277(9) 0.6490(8) 0.047(3) Uani 1 1 d . . . H16A H 0.3178 0.3689 0.6616 0.070 Uiso 1 1 calc R . . H16B H 0.4780 0.3431 0.6756 0.070 Uiso 1 1 calc R . . H16C H 0.3597 0.2747 0.6705 0.070 Uiso 1 1 calc R . . C161 C 0.2431(12) 0.3038(9) 0.5128(10) 0.048(4) Uani 1 1 d . . . H16D H 0.1854 0.3527 0.5130 0.073 Uiso 1 1 calc R . . H16E H 0.2026 0.2601 0.5433 0.073 Uiso 1 1 calc R . . H16F H 0.2476 0.2865 0.4551 0.073 Uiso 1 1 calc R . . C17 C 0.4089(11) 0.3776(7) 0.3494(7) 0.026(2) Uani 1 1 d . . . H17A H 0.4517 0.3593 0.3000 0.032 Uiso 1 1 calc R . . H17B H 0.3322 0.3398 0.3575 0.032 Uiso 1 1 calc R . . C18 C 0.3512(13) 0.4649(8) 0.3345(7) 0.034(3) Uani 1 1 d . . . H18A H 0.3034 0.4808 0.3828 0.041 Uiso 1 1 calc R . . H18B H 0.4302 0.5026 0.3325 0.041 Uiso 1 1 calc R . . C19 C 0.2521(15) 0.4756(9) 0.2563(9) 0.050(4) Uani 1 1 d . . . H19A H 0.2219 0.5325 0.2515 0.074 Uiso 1 1 calc R . . H19B H 0.1712 0.4403 0.2585 0.074 Uiso 1 1 calc R . . H19C H 0.2986 0.4609 0.2078 0.074 Uiso 1 1 calc R . . B1 B 0.5191(14) 0.3765(8) 0.4280(8) 0.028(3) Uani 1 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 0.01871(19) 0.0215(2) 0.02236(19) -0.00075(15) 0.00069(13) -0.00192(15) Os2 0.0227(2) 0.0238(2) 0.0221(2) 0.00076(16) 0.00136(14) -0.00412(16) Os3 0.0277(2) 0.0192(2) 0.0275(2) -0.00164(16) -0.00441(15) 0.00074(16) O1 0.029(4) 0.044(5) 0.041(5) 0.012(4) -0.017(4) -0.017(4) O2 0.042(5) 0.027(4) 0.024(4) 0.002(3) -0.004(3) 0.003(4) O3 0.033(5) 0.091(9) 0.043(5) -0.008(5) 0.011(4) 0.014(5) O4 0.040(5) 0.088(8) 0.021(4) -0.020(5) 0.005(4) -0.031(5) O5 0.032(4) 0.034(4) 0.021(4) -0.004(3) -0.004(3) -0.005(3) O6 0.070(7) 0.038(6) 0.044(5) 0.000(4) 0.024(5) -0.024(5) O7 0.056(6) 0.026(5) 0.036(5) 0.003(4) -0.017(4) -0.017(4) O8 0.038(5) 0.029(5) 0.040(5) -0.003(4) -0.011(4) 0.006(4) O9 0.073(7) 0.037(6) 0.047(5) 0.003(5) -0.017(5) -0.015(5) O10 0.056(7) 0.088(9) 0.083(8) -0.061(7) 0.005(6) 0.027(6) C1 0.023(5) 0.020(5) 0.029(5) -0.001(4) 0.004(4) 0.001(4) C2 0.021(5) 0.017(5) 0.022(5) 0.003(4) 0.008(4) 0.002(4) C3 0.019(5) 0.044(8) 0.044(7) -0.020(6) 0.002(5) 0.006(5) C4 0.035(6) 0.033(6) 0.021(5) 0.003(5) 0.005(4) -0.002(5) C5 0.023(5) 0.032(6) 0.023(5) 0.002(4) 0.003(4) 0.001(4) C6 0.049(8) 0.031(7) 0.030(6) 0.002(5) -0.004(5) 0.006(6) C7 0.042(7) 0.024(6) 0.030(6) -0.004(5) -0.012(5) 0.000(5) C8 0.027(5) 0.016(5) 0.031(5) 0.000(4) -0.005(4) 0.004(4) C9 0.046(7) 0.019(6) 0.027(5) 0.001(4) -0.013(5) -0.003(5) C10 0.042(7) 0.040(8) 0.036(7) -0.005(6) -0.005(5) 0.009(6) C11 0.020(5) 0.023(5) 0.020(5) 0.004(4) -0.004(4) -0.005(4) C12 0.030(6) 0.037(7) 0.030(6) -0.002(5) 0.006(4) -0.002(5) C13 0.022(6) 0.046(8) 0.050(7) 0.000(6) 0.001(5) -0.009(5) C131 0.047(7) 0.039(7) 0.028(6) 0.007(5) 0.002(5) 0.000(6) C14 0.042(7) 0.017(5) 0.028(5) 0.006(4) -0.006(5) -0.006(5) C15 0.034(7) 0.028(6) 0.045(7) 0.002(5) 0.005(5) -0.006(5) C16 0.047(8) 0.049(9) 0.049(8) 0.006(7) 0.028(6) 0.003(7) C161 0.017(6) 0.055(9) 0.073(10) -0.006(8) 0.005(6) -0.001(6) C17 0.026(5) 0.022(5) 0.029(5) 0.003(4) -0.001(4) 0.001(4) C18 0.035(6) 0.035(7) 0.032(6) -0.002(5) -0.002(5) 0.011(5) C19 0.048(8) 0.049(9) 0.048(8) 0.007(7) -0.009(6) 0.011(7) B1 0.032(7) 0.018(6) 0.034(7) -0.002(5) 0.002(5) 0.006(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 Os1 C3 1.867(12) . ? Os1 C1 1.938(10) . ? Os1 C2 1.948(10) . ? Os1 C11 2.261(11) . ? Os1 C12 2.359(13) . ? Os1 Os3 2.8727(10) . ? Os1 Os2 2.9503(8) . ? Os2 C6 1.895(14) . ? Os2 C5 1.937(10) . ? Os2 C4 1.943(11) . ? Os2 C14 2.247(11) . ? Os2 C15 2.379(13) . ? Os2 Os3 2.8706(8) . ? Os3 C10 1.898(14) . ? Os3 C9 1.915(12) . ? Os3 C7 1.941(10) . ? Os3 C8 1.965(10) . ? O1 C1 1.167(12) . ? O2 C2 1.138(12) . ? O3 C3 1.177(14) . ? O4 C4 1.124(13) . ? O5 C5 1.138(12) . ? O6 C6 1.126(15) . ? O7 C7 1.132(13) . ? O8 C8 1.127(12) . ? O9 C9 1.170(14) . ? O10 C10 1.137(16) . ? C11 C12 1.397(15) . ? C11 B1 1.609(17) . ? C11 H11A 1.0000 . ? C12 C131 1.506(16) . ? C12 C13 1.525(16) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C131 H13D 0.9800 . ? C131 H13E 0.9800 . ? C131 H13F 0.9800 . ? C14 C15 1.386(16) . ? C14 B1 1.537(17) . ? C14 H14A 1.0000 . ? C15 C161 1.497(17) . ? C15 C16 1.540(18) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C161 H16D 0.9800 . ? C161 H16E 0.9800 . ? C161 H16F 0.9800 . ? C17 C18 1.546(16) . ? C17 B1 1.557(16) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.501(16) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 C3 Os1 C1 90.9(5) . . ? C3 Os1 C2 91.0(5) . . ? C1 Os1 C2 177.4(4) . . ? C3 Os1 C11 120.4(5) . . ? C1 Os1 C11 82.5(4) . . ? C2 Os1 C11 98.0(4) . . ? C3 Os1 C12 86.9(5) . . ? C1 Os1 C12 92.9(4) . . ? C2 Os1 C12 88.9(4) . . ? C11 Os1 C12 35.1(4) . . ? C3 Os1 Os3 93.5(4) . . ? C1 Os1 Os3 92.8(3) . . ? C2 Os1 Os3 85.4(3) . . ? C11 Os1 Os3 145.7(3) . . ? C12 Os1 Os3 174.3(3) . . ? C3 Os1 Os2 152.2(4) . . ? C1 Os1 Os2 86.6(3) . . ? C2 Os1 Os2 90.9(3) . . ? C11 Os1 Os2 86.7(3) . . ? C12 Os1 Os2 120.8(3) . . ? Os3 Os1 Os2 59.055(16) . . ? C6 Os2 C5 91.3(5) . . ? C6 Os2 C4 87.2(5) . . ? C5 Os2 C4 176.9(5) . . ? C6 Os2 C14 119.3(5) . . ? C5 Os2 C14 95.3(4) . . ? C4 Os2 C14 87.8(5) . . ? C6 Os2 C15 85.2(5) . . ? C5 Os2 C15 90.0(4) . . ? C4 Os2 C15 92.6(5) . . ? C14 Os2 C15 34.7(4) . . ? C6 Os2 Os3 97.4(4) . . ? C5 Os2 Os3 88.0(3) . . ? C4 Os2 Os3 89.5(4) . . ? C14 Os2 Os3 143.0(3) . . ? C15 Os2 Os3 176.7(3) . . ? C6 Os2 Os1 156.5(4) . . ? C5 Os2 Os1 89.4(3) . . ? C4 Os2 Os1 90.9(3) . . ? C14 Os2 Os1 84.0(3) . . ? C15 Os2 Os1 118.3(3) . . ? Os3 Os2 Os1 59.13(2) . . ? C10 Os3 C9 103.9(6) . . ? C10 Os3 C7 87.7(5) . . ? C9 Os3 C7 91.0(5) . . ? C10 Os3 C8 89.3(5) . . ? C9 Os3 C8 90.6(4) . . ? C7 Os3 C8 176.9(5) . . ? C10 Os3 Os2 163.8(4) . . ? C9 Os3 Os2 92.3(4) . . ? C7 Os3 Os2 91.2(4) . . ? C8 Os3 Os2 91.4(3) . . ? C10 Os3 Os1 102.0(4) . . ? C9 Os3 Os1 153.9(4) . . ? C7 Os3 Os1 86.9(4) . . ? C8 Os3 Os1 92.8(3) . . ? Os2 Os3 Os1 61.82(2) . . ? O1 C1 Os1 175.1(10) . . ? O2 C2 Os1 175.3(9) . . ? O3 C3 Os1 178.3(13) . . ? O4 C4 Os2 174.7(11) . . ? O5 C5 Os2 175.0(10) . . ? O6 C6 Os2 178.7(12) . . ? O7 C7 Os3 176.8(12) . . ? O8 C8 Os3 174.6(9) . . ? O9 C9 Os3 178.9(10) . . ? O10 C10 Os3 177.4(13) . . ? C12 C11 B1 133.2(9) . . ? C12 C11 Os1 76.3(7) . . ? B1 C11 Os1 91.8(6) . . ? C12 C11 H11A 113.1 . . ? B1 C11 H11A 113.1 . . ? Os1 C11 H11A 113.1 . . ? C11 C12 C131 123.4(10) . . ? C11 C12 C13 118.2(10) . . ? C131 C12 C13 111.9(10) . . ? C11 C12 Os1 68.6(7) . . ? C131 C12 Os1 112.5(8) . . ? C13 C12 Os1 114.3(8) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C131 H13D 109.5 . . ? C12 C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? C12 C131 H13F 109.5 . . ? H13D C131 H13F 109.5 . . ? H13E C131 H13F 109.5 . . ? C15 C14 B1 133.8(11) . . ? C15 C14 Os2 77.9(7) . . ? B1 C14 Os2 93.8(7) . . ? C15 C14 H14A 112.6 . . ? B1 C14 H14A 112.6 . . ? Os2 C14 H14A 112.6 . . ? C14 C15 C161 127.0(12) . . ? C14 C15 C16 118.8(11) . . ? C161 C15 C16 109.6(11) . . ? C14 C15 Os2 67.4(7) . . ? C161 C15 Os2 113.1(9) . . ? C16 C15 Os2 112.5(9) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C161 H16D 109.5 . . ? C15 C161 H16E 109.5 . . ? H16D C161 H16E 109.5 . . ? C15 C161 H16F 109.5 . . ? H16D C161 H16F 109.5 . . ? H16E C161 H16F 109.5 . . ? C18 C17 B1 109.7(9) . . ? C18 C17 H17A 109.7 . . ? B1 C17 H17A 109.7 . . ? C18 C17 H17B 109.7 . . ? B1 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C19 C18 C17 114.9(10) . . ? C19 C18 H18A 108.5 . . ? C17 C18 H18A 108.5 . . ? C19 C18 H18B 108.5 . . ? C17 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 B1 C17 126.5(11) . . ? C14 B1 C11 110.4(10) . . ? C17 B1 C11 121.4(10) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 4.828 _refine_diff_density_min -2.901 _refine_diff_density_rms 0.387 # Attachment 'complex4.CIF' data_sad1 _database_code_depnum_ccdc_archive 'CCDC 694584' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H19 B O10 Os3, 0.25(C5 H12)' _chemical_formula_sum 'C21.25 H22 B O10 Os3' _chemical_formula_weight 1018.80 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' B B 0.0013 0.0007 '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' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6191(5) _cell_length_b 14.8240(7) _cell_length_c 19.2700(10) _cell_angle_alpha 93.9240(10) _cell_angle_beta 98.0350(10) _cell_angle_gamma 102.9230(10) _cell_volume 2637.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8281 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.9 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1850 _exptl_absorpt_coefficient_mu 14.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.081 _exptl_absorpt_correction_T_max 0.199 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29025 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 29.01 _reflns_number_total 13834 _reflns_number_gt 9729 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystals had poor quality (small piece of irregular shape) in addition to their high absorption. Analytical (face indexing procedure) absorption correction was not applicable. Thus, the ADP's of some light atoms in vicinity of Os atoms were poorly determined. To prevent the non-positive values of ADP the ISOR instruction for two atoms (B1A and B1B) was applied in refinement. Besides, the several DFIX instructions were used for restriction on geometry of disordered solvate molecule of pentane. The weighting scheme was chose proceeding from necessity to remove high residual peak (6 e/A3) at the osmium atoms (distances 0.01 A). For this purpose it was necessary to reduce the first parameter in the weight scheme and to keep GOF close to unit increase the second parameter in the weight scheme. Both problems, and uncertainty with anisotropic parameters of some atoms, and the overestimated value of the second parameter in the weighting scheme, are in our opinion caused by considerable absorption effects which could not be completely corrected. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13834 _refine_ls_number_parameters 654 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _refine_ls_shift/su_max 0.002 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1A Os 0.36627(3) 0.810314(17) 0.144202(14) 0.01950(6) Uani 1 1 d . . . Os2A Os 0.59040(3) 0.769852(17) 0.065275(13) 0.01742(6) Uani 1 1 d . . . Os3A Os 0.30989(3) 0.646228(17) 0.046799(14) 0.01871(6) Uani 1 1 d . . . O1A O 0.2631(6) 0.9191(3) 0.0238(3) 0.0377(13) Uani 1 1 d . . . O2A O 0.4624(5) 0.6981(3) 0.2628(3) 0.0298(12) Uani 1 1 d . . . O3A O 0.0719(7) 0.7701(4) 0.1908(4) 0.0578(18) Uani 1 1 d . . . O4A O 0.5040(6) 0.8833(4) -0.0538(3) 0.0390(14) Uani 1 1 d . . . O5A O 0.6989(5) 0.6558(3) 0.1804(2) 0.0271(11) Uani 1 1 d . . . O6A O 0.6967(6) 0.6546(4) -0.0434(3) 0.0445(15) Uani 1 1 d . . . O7A O 0.2140(6) 0.7519(3) -0.0767(3) 0.0346(13) Uani 1 1 d . . . O8A O 0.4032(5) 0.5275(3) 0.1624(2) 0.0269(11) Uani 1 1 d . . . O9A O 0.3574(6) 0.5002(3) -0.0604(3) 0.0361(13) Uani 1 1 d . . . O10A O -0.0090(6) 0.5807(3) 0.0608(3) 0.0360(13) Uani 1 1 d . . . B1A B 0.6531(8) 0.9061(5) 0.1802(4) 0.0166(15) Uani 1 1 d U . . C1A C 0.2996(7) 0.8759(4) 0.0666(4) 0.0245(16) Uani 1 1 d . . . C2A C 0.4317(7) 0.7403(5) 0.2173(4) 0.0233(15) Uani 1 1 d . . . C3A C 0.1840(9) 0.7848(5) 0.1729(4) 0.0359(19) Uani 1 1 d . . . C4A C 0.5309(7) 0.8409(5) -0.0088(4) 0.0246(15) Uani 1 1 d . . . C5A C 0.6554(7) 0.6985(4) 0.1396(3) 0.0208(14) Uani 1 1 d . . . C6A C 0.6555(8) 0.6979(5) -0.0019(4) 0.0296(17) Uani 1 1 d . . . C7A C 0.2537(7) 0.7165(5) -0.0297(4) 0.0264(16) Uani 1 1 d . . . C8A C 0.3721(7) 0.5755(4) 0.1214(3) 0.0198(14) Uani 1 1 d . . . C9A C 0.3394(7) 0.5541(5) -0.0205(4) 0.0243(15) Uani 1 1 d . . . C10A C 0.1122(8) 0.6033(5) 0.0563(4) 0.0257(16) Uani 1 1 d . . . C11A C 0.5239(7) 0.9467(4) 0.1802(4) 0.0229(15) Uani 1 1 d . . . H11A H 0.5199 0.9928 0.1449 0.027 Uiso 1 1 calc R . . C12A C 0.4197(9) 0.9459(5) 0.2246(4) 0.0363(19) Uani 1 1 d . . . C13A C 0.3123(9) 1.0084(5) 0.2125(5) 0.046(2) Uani 1 1 d . . . H13A H 0.3536 1.0694 0.2394 0.069 Uiso 1 1 calc R . . H13B H 0.2217 0.9794 0.2282 0.069 Uiso 1 1 calc R . . H13C H 0.2935 1.0163 0.1622 0.069 Uiso 1 1 calc R . . C131 C 0.4380(11) 0.9245(7) 0.2991(4) 0.058(3) Uani 1 1 d . . . H13D H 0.4955 0.9800 0.3293 0.087 Uiso 1 1 calc R . . H13E H 0.4877 0.8737 0.3036 0.087 Uiso 1 1 calc R . . H13F H 0.3429 0.9058 0.3137 0.087 Uiso 1 1 calc R . . C14A C 0.7237(7) 0.9120(4) 0.1115(4) 0.0230(15) Uani 1 1 d . . . H14A H 0.7100 0.9646 0.0836 0.028 Uiso 1 1 calc R . . C15A C 0.8215(8) 0.8626(5) 0.0906(4) 0.0309(17) Uani 1 1 d . . . H15A H 0.8828 0.8441 0.1309 0.037 Uiso 1 1 calc R . . C16A C 0.8985(9) 0.8870(6) 0.0302(5) 0.050(2) Uani 1 1 d . . . H16A H 0.9891 0.9333 0.0471 0.075 Uiso 1 1 calc R . . H16B H 0.8376 0.9127 -0.0044 0.075 Uiso 1 1 calc R . . H16C H 0.9195 0.8310 0.0082 0.075 Uiso 1 1 calc R . . C17A C 0.7505(8) 0.8790(5) 0.2489(4) 0.0289(17) Uani 1 1 d . . . H17A H 0.6868 0.8498 0.2814 0.035 Uiso 1 1 calc R . . H17B H 0.8052 0.8341 0.2337 0.035 Uiso 1 1 calc R . . C18A C 0.8557(9) 0.9684(5) 0.2867(4) 0.039(2) Uani 1 1 d . . . H18A H 0.9060 1.0026 0.2515 0.046 Uiso 1 1 calc R . . H18B H 0.7996 1.0086 0.3075 0.046 Uiso 1 1 calc R . . C19A C 0.9664(10) 0.9506(6) 0.3436(5) 0.055(3) Uani 1 1 d . . . H19A H 1.0345 1.0095 0.3629 0.083 Uiso 1 1 calc R . . H19B H 1.0189 0.9080 0.3240 0.083 Uiso 1 1 calc R . . H19C H 0.9183 0.9227 0.3813 0.083 Uiso 1 1 calc R . . Os1B Os 0.20199(3) 0.435968(17) 0.336086(13) 0.01771(6) Uani 1 1 d . . . Os2B Os -0.08406(3) 0.309195(17) 0.295762(13) 0.01835(6) Uani 1 1 d . . . Os3B Os 0.15409(3) 0.284038(18) 0.227556(14) 0.01986(6) Uani 1 1 d . . . O1B O 0.2842(6) 0.3151(3) 0.4513(3) 0.0333(12) Uani 1 1 d . . . O2B O 0.1335(5) 0.5628(3) 0.2230(2) 0.0275(11) Uani 1 1 d . . . O3B O 0.5208(6) 0.5014(4) 0.3286(3) 0.0415(14) Uani 1 1 d . . . O4B O -0.0172(6) 0.1831(4) 0.4096(3) 0.0371(13) Uani 1 1 d . . . O5B O -0.1716(5) 0.4323(3) 0.1831(2) 0.0270(11) Uani 1 1 d . . . O6B O -0.2957(6) 0.1452(3) 0.2075(3) 0.0408(14) Uani 1 1 d . . . O7B O 0.2373(6) 0.1591(3) 0.3400(3) 0.0353(13) Uani 1 1 d . . . O8B O 0.0725(5) 0.4043(3) 0.1114(3) 0.0283(11) Uani 1 1 d . . . O9B O -0.0014(6) 0.1092(4) 0.1296(3) 0.0436(15) Uani 1 1 d . . . O10B O 0.4573(6) 0.3113(4) 0.1909(3) 0.0431(14) Uani 1 1 d . . . B1B B -0.0434(8) 0.4757(5) 0.3789(4) 0.0144(14) Uani 1 1 d U . . C1B C 0.2491(7) 0.3566(5) 0.4072(3) 0.0216(15) Uani 1 1 d . . . C2B C 0.1531(7) 0.5143(5) 0.2638(4) 0.0214(15) Uani 1 1 d . . . C3B C 0.4013(8) 0.4761(5) 0.3301(4) 0.0269(16) Uani 1 1 d . . . C4B C -0.0375(7) 0.2295(5) 0.3663(4) 0.0240(15) Uani 1 1 d . . . C5B C -0.1335(7) 0.3899(4) 0.2252(4) 0.0216(15) Uani 1 1 d . . . C6B C -0.2157(8) 0.2060(5) 0.2404(4) 0.0264(16) Uani 1 1 d . . . C7B C 0.2048(8) 0.2073(5) 0.3013(4) 0.0229(15) Uani 1 1 d . . . C8B C 0.1007(7) 0.3618(4) 0.1560(4) 0.0217(15) Uani 1 1 d . . . C9B C 0.0543(8) 0.1743(5) 0.1665(4) 0.0281(17) Uani 1 1 d . . . C10B C 0.3448(8) 0.3022(5) 0.2038(4) 0.0280(17) Uani 1 1 d . . . C11B C 0.1085(7) 0.4984(4) 0.4230(3) 0.0204(14) Uani 1 1 d . . . H11B H 0.1132 0.4646 0.4661 0.024 Uiso 1 1 calc R . . C12B C 0.2360(7) 0.5663(5) 0.4214(4) 0.0250(15) Uani 1 1 d . . . C13B C 0.3629(8) 0.5740(6) 0.4779(4) 0.038(2) Uani 1 1 d . . . H13G H 0.3573 0.6175 0.5175 0.056 Uiso 1 1 calc R . . H13H H 0.4524 0.5969 0.4591 0.056 Uiso 1 1 calc R . . H13I H 0.3621 0.5127 0.4941 0.056 Uiso 1 1 calc R . . C132 C 0.2399(9) 0.6562(5) 0.3905(4) 0.038(2) Uani 1 1 d . . . H13J H 0.2438 0.7053 0.4280 0.057 Uiso 1 1 calc R . . H13K H 0.1528 0.6500 0.3557 0.057 Uiso 1 1 calc R . . H13L H 0.3256 0.6725 0.3676 0.057 Uiso 1 1 calc R . . C14B C -0.1487(7) 0.3832(4) 0.3868(3) 0.0221(15) Uani 1 1 d . . . H14B H -0.1306 0.3576 0.4330 0.027 Uiso 1 1 calc R . . C15B C -0.2780(7) 0.3379(5) 0.3430(4) 0.0258(16) Uani 1 1 d . . . H15B H -0.3267 0.3814 0.3170 0.031 Uiso 1 1 calc R . . C16B C -0.3833(8) 0.2546(6) 0.3626(4) 0.041(2) Uani 1 1 d . . . H16D H -0.4531 0.2762 0.3881 0.061 Uiso 1 1 calc R . . H16E H -0.3301 0.2188 0.3927 0.061 Uiso 1 1 calc R . . H16F H -0.4346 0.2151 0.3197 0.061 Uiso 1 1 calc R . . C17B C -0.1121(7) 0.5538(4) 0.3382(3) 0.0211(14) Uani 1 1 d . . . H17C H -0.0421 0.5891 0.3110 0.025 Uiso 1 1 calc R . . H17D H -0.2017 0.5234 0.3054 0.025 Uiso 1 1 calc R . . C18B C -0.1444(8) 0.6188(5) 0.3964(4) 0.0269(16) Uani 1 1 d . . . H18C H -0.2175 0.5822 0.4214 0.032 Uiso 1 1 calc R . . H18D H -0.0552 0.6433 0.4309 0.032 Uiso 1 1 calc R . . C19B C -0.1987(9) 0.6990(5) 0.3692(5) 0.042(2) Uani 1 1 d . . . H19D H -0.2157 0.7381 0.4088 0.063 Uiso 1 1 calc R . . H19E H -0.2893 0.6754 0.3365 0.063 Uiso 1 1 calc R . . H19F H -0.1267 0.7359 0.3447 0.063 Uiso 1 1 calc R . . C1S C 0.5000 1.0000 0.5000 0.138(10) Uani 1 2 d SD . . H1SA H 0.5159 1.0326 0.4594 0.165 Uiso 0.50 1 d PR A . H1SB H 0.5506 1.0423 0.5402 0.165 Uiso 0.50 1 d PR . . C2S C 0.559(3) 0.9156(17) 0.4923(18) 0.24(3) Uani 0.50 1 d PD A 1 H2SA H 0.5054 0.8722 0.4533 0.291 Uiso 0.50 1 d PR A 1 H2SB H 0.5456 0.8847 0.5339 0.291 Uiso 0.50 1 d PR A 1 C2S' C 0.661(2) 1.0228(18) 0.4961(16) 0.18(2) Uani 0.50 1 d PD A 2 H2SC H 0.6873 1.0512 0.4550 0.213 Uiso 0.50 1 d PR A 2 H2SD H 0.7222 1.0567 0.5377 0.213 Uiso 0.50 1 d PR A 2 C3S C 0.719(2) 0.9372(15) 0.4902(7) 0.199(11) Uani 1 1 d D . . H3SA H 0.7411 0.8757 0.4880 0.299 Uiso 0.50 1 d PR A . H3SB H 0.7780 0.9760 0.5319 0.299 Uiso 0.50 1 d PR . . H3SC H 0.7414 0.9666 0.4477 0.299 Uiso 0.50 1 d PR . . H3SD H 0.8211 0.9472 0.4894 0.299 Uiso 0.50 1 d PR . . H3SE H 0.6949 0.9020 0.5286 0.299 Uiso 0.50 1 d PR . . H3SF H 0.6668 0.9034 0.4466 0.299 Uiso 0.50 1 d PR . . 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 Os1A 0.01817(14) 0.01871(13) 0.02188(14) -0.00047(11) 0.00623(11) 0.00380(10) Os2A 0.01740(14) 0.01889(13) 0.01700(13) 0.00436(10) 0.00553(10) 0.00398(10) Os3A 0.01915(14) 0.01738(12) 0.01781(13) 0.00063(10) 0.00230(11) 0.00134(10) O1A 0.037(3) 0.035(3) 0.044(3) 0.009(3) 0.000(3) 0.017(3) O2A 0.037(3) 0.028(3) 0.023(3) 0.005(2) 0.007(2) 0.003(2) O3A 0.038(4) 0.057(4) 0.088(5) 0.015(4) 0.035(4) 0.014(3) O4A 0.036(3) 0.043(3) 0.038(3) 0.024(3) 0.002(3) 0.005(3) O5A 0.037(3) 0.024(2) 0.022(3) 0.006(2) 0.005(2) 0.009(2) O6A 0.061(4) 0.049(4) 0.033(3) 0.007(3) 0.024(3) 0.021(3) O7A 0.041(3) 0.030(3) 0.027(3) 0.011(2) -0.010(2) 0.002(2) O8A 0.031(3) 0.027(3) 0.024(3) 0.006(2) 0.006(2) 0.007(2) O9A 0.051(4) 0.034(3) 0.022(3) -0.008(2) 0.000(3) 0.014(3) O10A 0.027(3) 0.041(3) 0.040(3) 0.006(3) 0.011(3) 0.003(3) B1A 0.015(2) 0.018(2) 0.014(2) -0.0018(17) 0.0009(17) -0.0009(16) C1A 0.024(4) 0.017(3) 0.030(4) -0.006(3) 0.000(3) 0.006(3) C2A 0.021(4) 0.023(3) 0.024(4) -0.005(3) 0.008(3) 0.003(3) C3A 0.036(5) 0.033(4) 0.040(5) -0.001(4) 0.013(4) 0.008(4) C4A 0.019(4) 0.032(4) 0.024(4) 0.007(3) 0.008(3) 0.004(3) C5A 0.017(4) 0.024(3) 0.019(3) -0.003(3) 0.003(3) 0.000(3) C6A 0.027(4) 0.028(4) 0.036(4) 0.012(3) 0.012(3) 0.003(3) C7A 0.020(4) 0.025(4) 0.029(4) -0.006(3) 0.001(3) -0.002(3) C8A 0.019(4) 0.016(3) 0.022(4) -0.003(3) 0.008(3) -0.002(3) C9A 0.023(4) 0.024(4) 0.024(4) 0.010(3) 0.000(3) 0.000(3) C10A 0.036(5) 0.022(3) 0.018(4) 0.000(3) 0.002(3) 0.008(3) C11A 0.026(4) 0.012(3) 0.028(4) -0.003(3) 0.000(3) 0.004(3) C12A 0.030(5) 0.034(4) 0.044(5) 0.005(4) 0.003(4) 0.007(3) C13A 0.038(5) 0.034(4) 0.066(6) -0.008(4) 0.021(5) 0.004(4) C131 0.071(7) 0.064(6) 0.039(5) -0.009(5) 0.016(5) 0.013(5) C14A 0.022(4) 0.017(3) 0.024(4) 0.006(3) 0.000(3) -0.006(3) C15A 0.024(4) 0.035(4) 0.038(4) 0.012(4) 0.012(3) 0.008(3) C16A 0.044(6) 0.043(5) 0.063(6) 0.003(5) 0.029(5) -0.004(4) C17A 0.038(5) 0.021(3) 0.024(4) 0.001(3) -0.001(3) 0.003(3) C18A 0.048(5) 0.023(4) 0.036(5) 0.001(3) -0.018(4) 0.006(4) C19A 0.062(7) 0.036(5) 0.050(6) 0.007(4) -0.023(5) -0.005(4) Os1B 0.01373(13) 0.02164(13) 0.01633(13) -0.00161(10) 0.00240(10) 0.00227(10) Os2B 0.01567(14) 0.02068(13) 0.01708(13) -0.00067(10) 0.00346(10) 0.00120(10) Os3B 0.02039(15) 0.02331(13) 0.01606(13) -0.00141(11) 0.00504(11) 0.00527(11) O1B 0.036(3) 0.039(3) 0.023(3) 0.002(2) -0.002(2) 0.009(2) O2B 0.032(3) 0.025(3) 0.024(3) 0.003(2) 0.009(2) 0.002(2) O3B 0.018(3) 0.046(3) 0.058(4) 0.000(3) 0.011(3) 0.002(3) O4B 0.045(4) 0.037(3) 0.030(3) 0.017(3) 0.007(3) 0.007(3) O5B 0.027(3) 0.035(3) 0.019(3) 0.002(2) -0.001(2) 0.010(2) O6B 0.043(4) 0.029(3) 0.037(3) -0.001(3) -0.010(3) -0.006(3) O7B 0.047(4) 0.036(3) 0.030(3) 0.007(2) 0.007(3) 0.023(3) O8B 0.028(3) 0.033(3) 0.023(3) 0.003(2) 0.007(2) 0.004(2) O9B 0.064(4) 0.036(3) 0.023(3) -0.003(3) 0.005(3) -0.001(3) O10B 0.027(3) 0.062(4) 0.043(3) 0.008(3) 0.012(3) 0.013(3) B1B 0.012(2) 0.014(2) 0.019(2) -0.0049(16) 0.0065(17) 0.0055(16) C1B 0.017(4) 0.028(4) 0.019(3) -0.005(3) 0.000(3) 0.006(3) C2B 0.015(3) 0.025(3) 0.021(4) -0.006(3) 0.003(3) -0.001(3) C3B 0.026(4) 0.022(4) 0.031(4) 0.000(3) 0.003(3) 0.004(3) C4B 0.018(4) 0.023(3) 0.028(4) -0.003(3) 0.008(3) -0.003(3) C5B 0.018(4) 0.020(3) 0.022(4) -0.006(3) 0.003(3) -0.002(3) C6B 0.023(4) 0.025(4) 0.028(4) 0.001(3) 0.003(3) 0.001(3) C7B 0.027(4) 0.027(4) 0.018(3) -0.004(3) 0.009(3) 0.011(3) C8B 0.024(4) 0.023(3) 0.019(3) -0.003(3) 0.009(3) 0.005(3) C9B 0.038(5) 0.027(4) 0.018(4) 0.000(3) 0.007(3) 0.005(3) C10B 0.034(5) 0.034(4) 0.019(4) 0.001(3) 0.004(3) 0.014(3) C11B 0.023(4) 0.026(3) 0.012(3) 0.003(3) 0.004(3) 0.005(3) C12B 0.020(4) 0.034(4) 0.025(4) 0.003(3) 0.009(3) 0.011(3) C13B 0.031(5) 0.049(5) 0.029(4) -0.016(4) -0.003(4) 0.011(4) C132 0.045(5) 0.036(4) 0.034(4) -0.006(4) 0.010(4) 0.012(4) C14B 0.025(4) 0.029(4) 0.015(3) -0.001(3) 0.009(3) 0.009(3) C15B 0.018(4) 0.032(4) 0.024(4) 0.001(3) 0.000(3) 0.001(3) C16B 0.024(4) 0.055(5) 0.037(5) -0.008(4) 0.012(4) -0.005(4) C17B 0.017(3) 0.027(4) 0.019(3) -0.002(3) 0.007(3) 0.003(3) C18B 0.031(4) 0.024(4) 0.029(4) 0.000(3) 0.006(3) 0.013(3) C19B 0.055(6) 0.021(4) 0.055(6) 0.014(4) 0.011(5) 0.017(4) C1S 0.13(2) 0.24(3) 0.032(9) 0.027(15) 0.027(12) 0.01(2) C2S 0.21(5) 0.46(9) 0.21(4) 0.27(5) 0.18(4) 0.26(6) C2S' 0.19(4) 0.33(6) 0.13(3) 0.14(3) 0.12(3) 0.20(4) C3S 0.22(2) 0.40(3) 0.055(9) 0.052(15) 0.028(12) 0.22(2) _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 Os1A C3A 1.878(8) . ? Os1A C2A 1.924(7) . ? Os1A C1A 1.950(7) . ? Os1A C11A 2.239(6) . ? Os1A C12A 2.365(8) . ? Os1A Os3A 2.8695(4) . ? Os1A Os2A 2.9481(4) . ? Os2A C6A 1.882(8) . ? Os2A C4A 1.929(7) . ? Os2A C5A 1.952(7) . ? Os2A C14A 2.257(6) . ? Os2A C15A 2.304(7) . ? Os2A Os3A 2.8629(4) . ? Os3A C10A 1.904(8) . ? Os3A C9A 1.913(7) . ? Os3A C8A 1.942(7) . ? Os3A C7A 1.947(8) . ? O1A C1A 1.142(8) . ? O2A C2A 1.154(8) . ? O3A C3A 1.157(9) . ? O4A C4A 1.141(8) . ? O5A C5A 1.136(7) . ? O6A C6A 1.157(8) . ? O7A C7A 1.139(8) . ? O8A C8A 1.152(7) . ? O9A C9A 1.130(8) . ? O10A C10A 1.156(8) . ? B1A C11A 1.497(10) . ? B1A C14A 1.568(10) . ? B1A C17A 1.639(10) . ? C11A C12A 1.404(10) . ? C11A H11A 1.0000 . ? C12A C131 1.487(11) . ? C12A C13A 1.540(11) . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C131 H13D 0.9800 . ? C131 H13E 0.9800 . ? C131 H13F 0.9800 . ? C14A C15A 1.398(10) . ? C14A H14A 1.0000 . ? C15A C16A 1.486(10) . ? C15A H15A 1.0000 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C17A C18A 1.540(9) . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? C18A C19A 1.499(10) . ? C18A H18A 0.9900 . ? C18A H18B 0.9900 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? Os1B C3B 1.899(8) . ? Os1B C1B 1.938(7) . ? Os1B C2B 1.946(7) . ? Os1B C11B 2.247(6) . ? Os1B C12B 2.382(7) . ? Os1B Os3B 2.8776(4) . ? Os1B Os2B 2.9319(4) . ? Os2B C6B 1.900(7) . ? Os2B C4B 1.932(8) . ? Os2B C5B 1.950(7) . ? Os2B C14B 2.239(6) . ? Os2B C15B 2.296(7) . ? Os2B Os3B 2.8759(4) . ? Os3B C9B 1.917(7) . ? Os3B C10B 1.918(8) . ? Os3B C8B 1.943(7) . ? Os3B C7B 1.956(7) . ? O1B C1B 1.139(8) . ? O2B C2B 1.128(8) . ? O3B C3B 1.131(8) . ? O4B C4B 1.141(8) . ? O5B C5B 1.130(8) . ? O6B C6B 1.133(8) . ? O7B C7B 1.129(8) . ? O8B C8B 1.139(8) . ? O9B C9B 1.137(8) . ? O10B C10B 1.125(8) . ? B1B C11B 1.537(9) . ? B1B C14B 1.542(9) . ? B1B C17B 1.648(10) . ? C11B C12B 1.408(9) . ? C11B H11B 1.0000 . ? C12B C132 1.491(10) . ? C12B C13B 1.497(10) . ? C13B H13G 0.9800 . ? C13B H13H 0.9800 . ? C13B H13I 0.9800 . ? C132 H13J 0.9800 . ? C132 H13K 0.9800 . ? C132 H13L 0.9800 . ? C14B C15B 1.402(9) . ? C14B H14B 1.0000 . ? C15B C16B 1.518(9) . ? C15B H15B 1.0000 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17B C18B 1.538(9) . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? C18B C19B 1.499(9) . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C1S C2S 1.494(18) 2_676 ? C1S C2S 1.494(18) . ? C1S C2S' 1.524(18) 2_676 ? C1S C2S' 1.524(18) . ? C1S H1SA 0.9600 . ? C1S H1SB 0.9600 . ? C2S C3S 1.508(18) . ? C2S H2SA 0.9600 . ? C2S H2SB 0.9601 . ? C2S' C3S 1.501(18) . ? C2S' H2SC 0.9599 . ? C2S' H2SD 0.9600 . ? C3S H3SA 0.9799 . ? C3S H3SB 0.9801 . ? C3S H3SC 0.9801 . ? C3S H3SD 0.9600 . ? C3S H3SE 0.9599 . ? C3S H3SF 0.9598 . ? 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 C3A Os1A C2A 88.6(3) . . ? C3A Os1A C1A 92.1(3) . . ? C2A Os1A C1A 177.0(3) . . ? C3A Os1A C11A 120.4(3) . . ? C2A Os1A C11A 98.1(3) . . ? C1A Os1A C11A 84.0(3) . . ? C3A Os1A C12A 85.7(3) . . ? C2A Os1A C12A 90.8(3) . . ? C1A Os1A C12A 92.1(3) . . ? C11A Os1A C12A 35.4(2) . . ? C3A Os1A Os3A 95.8(2) . . ? C2A Os1A Os3A 88.66(19) . . ? C1A Os1A Os3A 88.41(18) . . ? C11A Os1A Os3A 143.24(18) . . ? C12A Os1A Os3A 178.40(19) . . ? C3A Os1A Os2A 154.7(2) . . ? C2A Os1A Os2A 89.2(2) . . ? C1A Os1A Os2A 88.9(2) . . ? C11A Os1A Os2A 84.94(18) . . ? C12A Os1A Os2A 119.5(2) . . ? Os3A Os1A Os2A 58.939(9) . . ? C6A Os2A C4A 88.5(3) . . ? C6A Os2A C5A 90.6(3) . . ? C4A Os2A C5A 178.6(3) . . ? C6A Os2A C14A 120.9(3) . . ? C4A Os2A C14A 81.4(3) . . ? C5A Os2A C14A 98.0(2) . . ? C6A Os2A C15A 88.1(3) . . ? C4A Os2A C15A 93.7(3) . . ? C5A Os2A C15A 85.1(3) . . ? C14A Os2A C15A 35.7(2) . . ? C6A Os2A Os3A 93.2(2) . . ? C4A Os2A Os3A 92.0(2) . . ? C5A Os2A Os3A 89.15(19) . . ? C14A Os2A Os3A 144.79(18) . . ? C15A Os2A Os3A 174.16(19) . . ? C6A Os2A Os1A 152.4(2) . . ? C4A Os2A Os1A 90.8(2) . . ? C5A Os2A Os1A 90.48(19) . . ? C14A Os2A Os1A 86.22(18) . . ? C15A Os2A Os1A 119.54(18) . . ? Os3A Os2A Os1A 59.161(9) . . ? C10A Os3A C9A 103.3(3) . . ? C10A Os3A C8A 92.0(3) . . ? C9A Os3A C8A 88.8(3) . . ? C10A Os3A C7A 89.9(3) . . ? C9A Os3A C7A 89.7(3) . . ? C8A Os3A C7A 177.8(3) . . ? C10A Os3A Os2A 157.9(2) . . ? C9A Os3A Os2A 98.6(2) . . ? C8A Os3A Os2A 91.40(18) . . ? C7A Os3A Os2A 87.3(2) . . ? C10A Os3A Os1A 96.2(2) . . ? C9A Os3A Os1A 160.5(2) . . ? C8A Os3A Os1A 90.99(18) . . ? C7A Os3A Os1A 89.94(19) . . ? Os2A Os3A Os1A 61.900(9) . . ? C11A B1A C14A 116.1(6) . . ? C11A B1A C17A 126.7(6) . . ? C14A B1A C17A 115.5(6) . . ? O1A C1A Os1A 175.8(6) . . ? O2A C2A Os1A 175.4(6) . . ? O3A C3A Os1A 179.2(7) . . ? O4A C4A Os2A 175.7(6) . . ? O5A C5A Os2A 175.9(6) . . ? O6A C6A Os2A 179.1(7) . . ? O7A C7A Os3A 175.1(6) . . ? O8A C8A Os3A 174.8(5) . . ? O9A C9A Os3A 179.6(7) . . ? O10A C10A Os3A 177.1(6) . . ? C12A C11A B1A 134.9(7) . . ? C12A C11A Os1A 77.2(4) . . ? B1A C11A Os1A 93.7(4) . . ? C12A C11A H11A 112.2 . . ? B1A C11A H11A 112.2 . . ? Os1A C11A H11A 112.2 . . ? C11A C12A C131 124.6(8) . . ? C11A C12A C13A 119.6(7) . . ? C131 C12A C13A 110.5(8) . . ? C11A C12A Os1A 67.4(4) . . ? C131 C12A Os1A 112.2(6) . . ? C13A C12A Os1A 114.4(5) . . ? C12A C13A H13A 109.5 . . ? C12A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? C12A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? C12A C131 H13D 109.5 . . ? C12A C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? C12A C131 H13F 109.5 . . ? H13D C131 H13F 109.5 . . ? H13E C131 H13F 109.5 . . ? C15A C14A B1A 128.0(6) . . ? C15A C14A Os2A 74.0(4) . . ? B1A C14A Os2A 92.1(4) . . ? C15A C14A H14A 115.6 . . ? B1A C14A H14A 115.6 . . ? Os2A C14A H14A 115.6 . . ? C14A C15A C16A 121.7(7) . . ? C14A C15A Os2A 70.3(4) . . ? C16A C15A Os2A 117.4(6) . . ? C14A C15A H15A 113.5 . . ? C16A C15A H15A 113.5 . . ? Os2A C15A H15A 113.5 . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C18A C17A B1A 108.8(5) . . ? C18A C17A H17A 109.9 . . ? B1A C17A H17A 109.9 . . ? C18A C17A H17B 109.9 . . ? B1A C17A H17B 109.9 . . ? H17A C17A H17B 108.3 . . ? C19A C18A C17A 113.5(6) . . ? C19A C18A H18A 108.9 . . ? C17A C18A H18A 108.9 . . ? C19A C18A H18B 108.9 . . ? C17A C18A H18B 108.9 . . ? H18A C18A H18B 107.7 . . ? C18A C19A H19A 109.5 . . ? C18A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C18A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C3B Os1B C1B 89.5(3) . . ? C3B Os1B C2B 90.8(3) . . ? C1B Os1B C2B 179.3(3) . . ? C3B Os1B C11B 120.5(3) . . ? C1B Os1B C11B 82.3(3) . . ? C2B Os1B C11B 98.1(3) . . ? C3B Os1B C12B 87.1(3) . . ? C1B Os1B C12B 92.4(3) . . ? C2B Os1B C12B 88.2(2) . . ? C11B Os1B C12B 35.3(2) . . ? C3B Os1B Os3B 93.5(2) . . ? C1B Os1B Os3B 90.58(18) . . ? C2B Os1B Os3B 88.75(18) . . ? C11B Os1B Os3B 144.95(16) . . ? C12B Os1B Os3B 176.92(17) . . ? C3B Os1B Os2B 152.8(2) . . ? C1B Os1B Os2B 89.44(19) . . ? C2B Os1B Os2B 89.93(19) . . ? C11B Os1B Os2B 86.20(16) . . ? C12B Os1B Os2B 120.08(16) . . ? Os3B Os1B Os2B 59.336(9) . . ? C6B Os2B C4B 90.4(3) . . ? C6B Os2B C5B 89.5(3) . . ? C4B Os2B C5B 179.1(3) . . ? C6B Os2B C14B 120.8(3) . . ? C4B Os2B C14B 82.2(3) . . ? C5B Os2B C14B 97.1(3) . . ? C6B Os2B C15B 87.0(3) . . ? C4B Os2B C15B 93.9(3) . . ? C5B Os2B C15B 85.2(3) . . ? C14B Os2B C15B 36.0(2) . . ? C6B Os2B Os3B 93.2(2) . . ? C4B Os2B Os3B 91.1(2) . . ? C5B Os2B Os3B 89.8(2) . . ? C14B Os2B Os3B 145.15(17) . . ? C15B Os2B Os3B 175.00(18) . . ? C6B Os2B Os1B 152.6(2) . . ? C4B Os2B Os1B 90.77(19) . . ? C5B Os2B Os1B 89.67(19) . . ? C14B Os2B Os1B 86.42(17) . . ? C15B Os2B Os1B 120.25(16) . . ? Os3B Os2B Os1B 59.391(9) . . ? C9B Os3B C10B 101.3(3) . . ? C9B Os3B C8B 90.4(3) . . ? C10B Os3B C8B 90.9(3) . . ? C9B Os3B C7B 90.3(3) . . ? C10B Os3B C7B 90.3(3) . . ? C8B Os3B C7B 178.4(3) . . ? C9B Os3B Os2B 97.6(2) . . ? C10B Os3B Os2B 161.0(2) . . ? C8B Os3B Os2B 89.89(19) . . ? C7B Os3B Os2B 88.62(19) . . ? C9B Os3B Os1B 158.9(2) . . ? C10B Os3B Os1B 99.7(2) . . ? C8B Os3B Os1B 91.01(18) . . ? C7B Os3B Os1B 87.78(18) . . ? Os2B Os3B Os1B 61.272(9) . . ? C11B B1B C14B 118.3(6) . . ? C11B B1B C17B 123.0(6) . . ? C14B B1B C17B 117.2(6) . . ? O1B C1B Os1B 175.2(6) . . ? O2B C2B Os1B 175.7(6) . . ? O3B C3B Os1B 177.9(7) . . ? O4B C4B Os2B 175.9(6) . . ? O5B C5B Os2B 175.1(6) . . ? O6B C6B Os2B 179.0(7) . . ? O7B C7B Os3B 174.7(6) . . ? O8B C8B Os3B 176.0(6) . . ? O9B C9B Os3B 178.1(7) . . ? O10B C10B Os3B 178.3(7) . . ? C12B C11B B1B 133.4(6) . . ? C12B C11B Os1B 77.6(4) . . ? B1B C11B Os1B 92.4(4) . . ? C12B C11B H11B 112.9 . . ? B1B C11B H11B 112.9 . . ? Os1B C11B H11B 112.9 . . ? C11B C12B C132 124.1(6) . . ? C11B C12B C13B 118.9(6) . . ? C132 C12B C13B 111.4(6) . . ? C11B C12B Os1B 67.1(4) . . ? C132 C12B Os1B 114.0(5) . . ? C13B C12B Os1B 112.9(5) . . ? C12B C13B H13G 109.5 . . ? C12B C13B H13H 109.5 . . ? H13G C13B H13H 109.5 . . ? C12B C13B H13I 109.5 . . ? H13G C13B H13I 109.5 . . ? H13H C13B H13I 109.5 . . ? C12B C132 H13J 109.5 . . ? C12B C132 H13K 109.5 . . ? H13J C132 H13K 109.5 . . ? C12B C132 H13L 109.5 . . ? H13J C132 H13L 109.5 . . ? H13K C132 H13L 109.5 . . ? C15B C14B B1B 128.7(6) . . ? C15B C14B Os2B 74.2(4) . . ? B1B C14B Os2B 92.2(4) . . ? C15B C14B H14B 115.2 . . ? B1B C14B H14B 115.2 . . ? Os2B C14B H14B 115.2 . . ? C14B C15B C16B 123.2(7) . . ? C14B C15B Os2B 69.8(4) . . ? C16B C15B Os2B 117.0(5) . . ? C14B C15B H15B 113.3 . . ? C16B C15B H15B 113.3 . . ? Os2B C15B H15B 113.3 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C18B C17B B1B 105.9(5) . . ? C18B C17B H17C 110.5 . . ? B1B C17B H17C 110.5 . . ? C18B C17B H17D 110.5 . . ? B1B C17B H17D 110.5 . . ? H17C C17B H17D 108.7 . . ? C19B C18B C17B 113.5(6) . . ? C19B C18B H18C 108.9 . . ? C17B C18B H18C 108.9 . . ? C19B C18B H18D 108.9 . . ? C17B C18B H18D 108.9 . . ? H18C C18B H18D 107.7 . . ? C18B C19B H19D 109.5 . . ? C18B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C2S C1S C2S' 113.2(15) . 2_676 ? C2S C1S C2S' 113.2(15) 2_676 . ? C2S C1S H1SA 106.9 . . ? C2S' C1S H1SA 108.8 2_676 . ? C2S C1S H1SB 112.3 . . ? C2S' C1S H1SB 109.0 2_676 . ? H1SA C1S H1SB 106.3 . . ? C1S C2S C3S 113.7(18) . . ? C1S C2S H2SA 112.0 . . ? C3S C2S H2SA 111.9 . . ? C1S C2S H2SB 106.2 . . ? C3S C2S H2SB 106.3 . . ? H2SA C2S H2SB 106.1 . . ? C1S C2S H3SE 127.1 . . ? H2SA C2S H3SE 120.0 . . ? C1S C2S H3SF 125.1 . . ? H2SB C2S H3SF 124.6 . . ? C3S C2S' C1S 112.4(17) . . ? C3S C2S' H1SA 125.6 . . ? C3S C2S' H1SB 128.2 . . ? C3S C2S' H2SC 101.3 . . ? C1S C2S' H2SC 115.1 . . ? H1SB C2S' H2SC 127.9 . . ? C3S C2S' H2SD 101.1 . . ? C1S C2S' H2SD 115.0 . . ? H1SA C2S' H2SD 130.5 . . ? H2SC C2S' H2SD 110.2 . . ? C1S C2S' H3SB 127.8 . . ? H1SB C2S' H3SB 116.5 . . ? H2SC C2S' H3SB 112.8 . . ? C2S C3S H3SA 103.3 . . ? C2S C3S H3SB 113.8 . . ? H3SA C3S H3SB 109.5 . . ? C2S C3S H3SC 111.1 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? C2S' C3S H3SD 116.2 . . ? C2S' C3S H3SE 107.9 . . ? H3SD C3S H3SE 109.5 . . ? C2S' C3S H3SF 104.0 . . ? H3SD C3S H3SF 109.5 . . ? H3SE C3S H3SF 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 29.01 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.832 _refine_diff_density_min -1.960 _refine_diff_density_rms 0.242