Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Chen, Yao-Lun' 'Chi, Yun' 'Ching, Wei-Li' 'Chou, Tsung-Yi' 'Lee, Gene-Hsiung' 'Liu, Chao-Shiuan' 'Peng, Shie-ming' 'Yu, Huan-Li' _publ_contact_author_name 'Prof Yun Ch' _publ_contact_author_address ; Prof Yun Chi Department of Chemistry National Tsing Hua University 101, Section 2 Kuang Fu Road Hsinchu Taiwan 30013 TAIWAN ; _publ_contact_author_email 'YCHI@MX.NTHU.EDU.TW' _publ_section_title ; Deposition of Osmium Thin Films Using Pyrazolate Complexes as CVD Source Reagents ; data_ic8387_complex_1 _database_code_CSD 172179 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H2 F6 N2 O10 Os3' _chemical_formula_weight 1054.79 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' '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 16.7057(4) _cell_length_b 7.7137(2) _cell_length_c 18.8324(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.524(1) _cell_angle_gamma 90.00 _cell_volume 2207.87(10) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 9587 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 3.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 17.328 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2617 _exptl_absorpt_correction_T_max 0.4915 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART 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_% 0 _diffrn_reflns_number 18414 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5057 _reflns_number_gt 4259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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. ; _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^)+(0.0547P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00153(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5057 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 0.323965(18) 0.20483(4) -0.139498(15) 0.02729(10) Uani 1 1 d . . . Os2 Os 0.231988(18) 0.19652(4) -0.309058(15) 0.02749(10) Uani 1 1 d . . . Os3 Os 0.340462(18) -0.08841(4) -0.226145(16) 0.02801(10) Uani 1 1 d . . . H1 H 0.280(4) 0.337(9) -0.225(4) 0.015(17) Uiso 1 1 d . . . N1 N 0.1877(4) 0.1367(8) -0.1761(3) 0.0305(13) Uani 1 1 d . . . N2 N 0.1454(4) 0.1320(8) -0.2552(3) 0.0282(12) Uani 1 1 d . . . C1 C 0.4391(5) 0.2741(10) -0.1218(5) 0.0364(17) Uani 1 1 d . . . C2 C 0.3693(5) 0.0606(10) -0.0497(5) 0.0378(18) Uani 1 1 d . . . C3 C 0.3075(6) 0.4087(11) -0.0874(5) 0.0417(19) Uani 1 1 d . . . C4 C 0.1609(5) 0.4002(11) -0.3550(5) 0.0392(18) Uani 1 1 d . . . C5 C 0.1793(6) 0.0425(11) -0.3973(4) 0.0389(18) Uani 1 1 d . . . C6 C 0.3180(6) 0.2606(11) -0.3456(5) 0.0389(18) Uani 1 1 d . . . C7 C 0.2363(6) -0.1857(10) -0.2191(5) 0.0380(18) Uani 1 1 d . . . C8 C 0.3232(5) -0.2380(11) -0.3143(5) 0.0396(18) Uani 1 1 d . . . C9 C 0.4395(5) 0.0198(11) -0.2357(5) 0.0359(17) Uani 1 1 d . . . C10 C 0.4186(6) -0.2267(10) -0.1404(5) 0.0376(18) Uani 1 1 d . . . C11 C 0.1533(6) 0.0914(14) -0.0617(5) 0.052(2) Uani 1 1 d . . . C12 C 0.1286(5) 0.1059(11) -0.1471(4) 0.0354(17) Uani 1 1 d . . . C13 C 0.0474(6) 0.0805(12) -0.2063(5) 0.045(2) Uani 1 1 d . . . H13A H -0.0051 0.0563 -0.2022 0.054 Uiso 1 1 calc R . . C14 C 0.0608(5) 0.0988(11) -0.2733(4) 0.0367(18) Uani 1 1 d . . . C15 C -0.0035(6) 0.0728(12) -0.3557(5) 0.046(2) Uani 1 1 d . . . O1 O 0.5072(4) 0.3223(9) -0.1130(4) 0.0567(17) Uani 1 1 d . . . O2 O 0.3990(5) -0.0239(10) 0.0056(4) 0.0601(18) Uani 1 1 d . . . O3 O 0.3024(5) 0.5272(9) -0.0545(5) 0.069(2) Uani 1 1 d . . . O4 O 0.1231(5) 0.5214(9) -0.3799(4) 0.0597(18) Uani 1 1 d . . . O5 O 0.1523(5) -0.0473(10) -0.4485(4) 0.0598(18) Uani 1 1 d . . . O6 O 0.3687(5) 0.2958(9) -0.3683(4) 0.0602(19) Uani 1 1 d . . . O7 O 0.1776(4) -0.2497(9) -0.2161(5) 0.0584(18) Uani 1 1 d . . . O8 O 0.3118(5) -0.3202(9) -0.3653(4) 0.0622(19) Uani 1 1 d . . . O9 O 0.4986(4) 0.0751(10) -0.2432(5) 0.064(2) Uani 1 1 d . . . O10 O 0.4631(5) -0.3059(9) -0.0895(5) 0.0615(19) Uani 1 1 d . . . F1 F 0.0815(4) 0.0811(10) -0.0483(3) 0.080(2) Uani 1 1 d . . . F2 F 0.1976(5) 0.2258(11) -0.0235(3) 0.089(2) Uani 1 1 d . . . F3 F 0.2015(5) -0.0470(10) -0.0315(4) 0.092(2) Uani 1 1 d . . . F4 F -0.0841(4) 0.0510(10) -0.3589(4) 0.081(2) Uani 1 1 d . . . F5 F -0.0070(4) 0.2070(9) -0.4003(4) 0.084(2) Uani 1 1 d . . . F6 F 0.0135(4) -0.0633(8) -0.3888(3) 0.0694(18) 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 0.02424(16) 0.03306(16) 0.02126(15) -0.00214(10) 0.00613(12) -0.00002(10) Os2 0.02576(16) 0.03667(17) 0.02001(15) 0.00169(10) 0.00945(12) 0.00084(11) Os3 0.02397(16) 0.03021(16) 0.03158(16) -0.00169(11) 0.01325(12) -0.00034(11) N1 0.029(3) 0.044(3) 0.018(3) 0.000(3) 0.010(2) 0.002(3) N2 0.024(3) 0.038(3) 0.020(3) -0.003(2) 0.008(2) 0.000(2) C1 0.034(4) 0.033(4) 0.039(4) 0.000(3) 0.012(4) -0.001(3) C2 0.036(4) 0.043(4) 0.031(4) -0.008(3) 0.011(3) -0.002(3) C3 0.040(5) 0.047(5) 0.036(4) -0.005(4) 0.014(4) -0.001(4) C4 0.035(4) 0.053(5) 0.032(4) 0.004(4) 0.017(3) 0.001(4) C5 0.042(5) 0.051(5) 0.024(4) 0.000(3) 0.014(3) 0.000(4) C6 0.039(5) 0.047(4) 0.033(4) 0.013(3) 0.018(4) 0.002(4) C7 0.040(5) 0.038(4) 0.038(4) 0.002(3) 0.019(4) 0.000(3) C8 0.034(4) 0.043(4) 0.042(5) -0.008(4) 0.016(4) -0.001(4) C9 0.028(4) 0.041(4) 0.035(4) 0.003(3) 0.010(3) 0.002(3) C10 0.037(5) 0.033(4) 0.043(5) 0.000(3) 0.018(4) 0.001(3) C11 0.039(5) 0.092(8) 0.029(4) 0.003(5) 0.018(4) 0.005(5) C12 0.032(4) 0.048(4) 0.029(4) -0.002(3) 0.014(3) 0.001(3) C13 0.032(4) 0.066(6) 0.041(5) -0.005(4) 0.019(4) -0.005(4) C14 0.019(4) 0.059(5) 0.030(4) -0.005(4) 0.009(3) -0.002(3) C15 0.028(4) 0.065(6) 0.038(5) -0.010(4) 0.008(4) -0.004(4) O1 0.035(4) 0.059(4) 0.071(5) -0.002(3) 0.017(3) -0.004(3) O2 0.067(5) 0.070(4) 0.037(3) 0.017(3) 0.016(3) 0.012(4) O3 0.082(5) 0.057(4) 0.072(5) -0.028(4) 0.037(4) 0.000(4) O4 0.058(4) 0.056(4) 0.060(4) 0.019(3) 0.019(3) 0.026(3) O5 0.058(4) 0.077(5) 0.037(3) -0.017(3) 0.012(3) -0.008(4) O6 0.050(4) 0.075(5) 0.070(5) 0.020(4) 0.039(4) 0.002(3) O7 0.049(4) 0.055(4) 0.087(5) 0.002(4) 0.043(4) -0.010(3) O8 0.060(4) 0.063(4) 0.064(4) -0.033(4) 0.027(4) -0.004(3) O9 0.035(4) 0.081(5) 0.082(5) 0.015(4) 0.031(4) -0.006(3) O10 0.051(4) 0.056(4) 0.069(5) 0.022(4) 0.017(4) 0.013(3) F1 0.060(4) 0.148(7) 0.047(3) 0.011(4) 0.038(3) 0.000(4) F2 0.102(5) 0.134(6) 0.036(3) -0.031(4) 0.035(3) -0.047(5) F3 0.103(6) 0.121(6) 0.050(4) 0.038(4) 0.031(4) 0.041(5) F4 0.025(3) 0.149(7) 0.061(4) -0.024(4) 0.009(3) -0.009(3) F5 0.069(4) 0.100(5) 0.048(4) 0.022(3) -0.011(3) -0.021(4) F6 0.058(4) 0.093(5) 0.050(3) -0.032(3) 0.016(3) 0.000(3) _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 H1 1.79(6) . ? Os1 C1 1.888(8) . ? Os1 C2 1.899(8) . ? Os1 C3 1.932(8) . ? Os1 N1 2.153(6) . ? Os1 Os3 2.8685(4) . ? Os1 Os2 2.9135(4) . ? Os2 H1 1.80(6) . ? Os2 C6 1.899(8) . ? Os2 C5 1.932(8) . ? Os2 C4 1.943(9) . ? Os2 N2 2.141(6) . ? Os2 Os3 2.8642(4) . ? Os3 C10 1.924(9) . ? Os3 C9 1.926(8) . ? Os3 C8 1.942(8) . ? Os3 C7 1.949(8) . ? N1 C12 1.332(10) . ? N1 N2 1.360(8) . ? N2 C14 1.334(9) . ? C1 O1 1.142(10) . ? C2 O2 1.152(10) . ? C3 O3 1.127(10) . ? C4 O4 1.116(10) . ? C5 O5 1.119(10) . ? C6 O6 1.128(10) . ? C7 O7 1.120(10) . ? C8 O8 1.100(10) . ? C9 O9 1.138(9) . ? C10 O10 1.119(10) . ? C11 F2 1.303(12) . ? C11 F3 1.315(11) . ? C11 F1 1.328(10) . ? C11 C12 1.489(11) . ? C12 C13 1.366(11) . ? C13 C14 1.377(11) . ? C14 C15 1.490(11) . ? C15 F6 1.311(10) . ? C15 F5 1.319(11) . ? C15 F4 1.333(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 H1 Os1 C1 90.1(19) . . ? H1 Os1 C2 179(2) . . ? C1 Os1 C2 90.5(3) . . ? H1 Os1 C3 85(2) . . ? C1 Os1 C3 91.7(4) . . ? C2 Os1 C3 96.5(3) . . ? H1 Os1 N1 83(2) . . ? C1 Os1 N1 172.1(3) . . ? C2 Os1 N1 96.9(3) . . ? C3 Os1 N1 90.4(3) . . ? H1 Os1 Os3 92(2) . . ? C1 Os1 Os3 89.6(2) . . ? C2 Os1 Os3 87.0(2) . . ? C3 Os1 Os3 176.3(3) . . ? N1 Os1 Os3 87.94(16) . . ? H1 Os1 Os2 36(2) . . ? C1 Os1 Os2 103.6(2) . . ? C2 Os1 Os2 142.8(2) . . ? C3 Os1 Os2 116.9(3) . . ? N1 Os1 Os2 68.73(15) . . ? Os3 Os1 Os2 59.381(9) . . ? H1 Os2 C6 92(2) . . ? H1 Os2 C5 179(2) . . ? C6 Os2 C5 89.5(4) . . ? H1 Os2 C4 83(2) . . ? C6 Os2 C4 92.5(4) . . ? C5 Os2 C4 97.9(3) . . ? H1 Os2 N2 83(2) . . ? C6 Os2 N2 173.7(3) . . ? C5 Os2 N2 96.2(3) . . ? C4 Os2 N2 89.5(3) . . ? H1 Os2 Os3 92(2) . . ? C6 Os2 Os3 89.7(2) . . ? C5 Os2 Os3 87.5(2) . . ? C4 Os2 Os3 174.2(2) . . ? N2 Os2 Os3 87.85(16) . . ? H1 Os2 Os1 36(2) . . ? C6 Os2 Os1 104.9(3) . . ? C5 Os2 Os1 143.2(2) . . ? C4 Os2 Os1 114.7(2) . . ? N2 Os2 Os1 68.83(15) . . ? Os3 Os2 Os1 59.526(9) . . ? C10 Os3 C9 90.5(3) . . ? C10 Os3 C8 101.3(4) . . ? C9 Os3 C8 90.4(3) . . ? C10 Os3 C7 92.5(3) . . ? C9 Os3 C7 176.7(3) . . ? C8 Os3 C7 90.5(4) . . ? C10 Os3 Os2 159.8(2) . . ? C9 Os3 Os2 89.4(2) . . ? C8 Os3 Os2 98.9(3) . . ? C7 Os3 Os2 87.3(2) . . ? C10 Os3 Os1 98.7(2) . . ? C9 Os3 Os1 90.0(2) . . ? C8 Os3 Os1 159.9(3) . . ? C7 Os3 Os1 88.0(2) . . ? Os2 Os3 Os1 61.092(10) . . ? C12 N1 N2 108.0(6) . . ? C12 N1 Os1 141.0(5) . . ? N2 N1 Os1 110.9(4) . . ? C14 N2 N1 107.3(6) . . ? C14 N2 Os2 141.0(5) . . ? N1 N2 Os2 111.6(4) . . ? O1 C1 Os1 177.0(8) . . ? O2 C2 Os1 178.0(8) . . ? O3 C3 Os1 176.4(8) . . ? O4 C4 Os2 177.1(8) . . ? O5 C5 Os2 176.9(8) . . ? O6 C6 Os2 178.6(9) . . ? O7 C7 Os3 176.4(8) . . ? O8 C8 Os3 178.3(9) . . ? O9 C9 Os3 176.1(8) . . ? O10 C10 Os3 178.4(8) . . ? F2 C11 F3 107.6(9) . . ? F2 C11 F1 107.0(8) . . ? F3 C11 F1 107.9(9) . . ? F2 C11 C12 112.1(8) . . ? F3 C11 C12 112.0(8) . . ? F1 C11 C12 110.1(7) . . ? N1 C12 C13 110.2(7) . . ? N1 C12 C11 122.3(7) . . ? C13 C12 C11 127.3(8) . . ? C12 C13 C14 104.4(7) . . ? N2 C14 C13 110.2(7) . . ? N2 C14 C15 121.4(7) . . ? C13 C14 C15 128.3(8) . . ? F6 C15 F5 106.7(8) . . ? F6 C15 F4 106.9(8) . . ? F5 C15 F4 107.0(8) . . ? F6 C15 C14 113.5(7) . . ? F5 C15 C14 112.4(7) . . ? F4 C15 C14 110.0(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.908 _refine_diff_density_min -1.856 _refine_diff_density_rms 0.226 #===END data_ic8388_complex_2 _database_code_CSD 172180 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H2 F12 N4 O6 Os2' _chemical_formula_weight 954.62 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' 'F' 'F' 0.0171 0.0103 '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 Tetragonal _symmetry_space_group_name_H-M P-42(1)m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 11.9181(2) _cell_length_b 11.9181(2) _cell_length_c 8.2009(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1164.86(4) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 9399 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 2.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 11.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2737 _exptl_absorpt_correction_T_max 0.4915 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART 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_% 0 _diffrn_reflns_number 12364 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1437 _reflns_number_gt 1377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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. ; _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^)+(0.0212P)^2^+0.5493P] 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 SHELXL _refine_ls_extinction_coef 0.0462(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(12) _refine_ls_number_reflns 1437 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0157 _refine_ls_R_factor_gt 0.0146 _refine_ls_wR_factor_ref 0.0365 _refine_ls_wR_factor_gt 0.0363 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 Os1 Os 0.918550(11) 0.418550(11) 0.46933(2) 0.02426(9) Uani 1 2 d S . . N1 N 0.8772(3) 0.5436(2) 0.6442(4) 0.0255(6) Uani 1 1 d . . . C1 C 0.9866(4) 0.3267(4) 0.3071(7) 0.0391(10) Uani 1 1 d . . . C2 C 0.8057(3) 0.3057(3) 0.5269(8) 0.0335(11) Uani 1 2 d S . . C3 C 0.8287(4) 0.6713(4) 0.8291(8) 0.0358(13) Uani 1 2 d S . . H3A H 0.7905 0.7095 0.9109 0.043 Uiso 1 2 calc SR . . C4 C 0.7985(3) 0.5717(4) 0.7548(5) 0.0297(8) Uani 1 1 d . . . C5 C 0.6972(4) 0.5019(5) 0.7811(6) 0.0455(11) Uani 1 1 d . . . O1 O 1.0257(4) 0.2728(4) 0.2085(6) 0.0684(12) Uani 1 1 d . . . O2 O 0.7394(3) 0.2394(3) 0.5516(6) 0.0541(12) Uani 1 2 d S . . F1 F 0.6275(2) 0.5543(3) 0.8850(5) 0.0680(10) Uani 1 1 d . . . F2 F 0.6427(3) 0.4825(4) 0.6448(4) 0.0694(10) Uani 1 1 d . . . F3 F 0.7212(3) 0.4032(3) 0.8469(5) 0.0642(9) 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 0.02499(9) 0.02499(9) 0.02280(11) -0.00255(6) -0.00255(6) -0.00074(8) N1 0.0275(15) 0.0247(14) 0.0243(15) -0.0001(12) -0.0018(12) -0.0014(10) C1 0.038(2) 0.045(2) 0.035(3) -0.0109(19) -0.0048(19) 0.0017(19) C2 0.0344(16) 0.0344(16) 0.032(3) -0.0064(18) -0.0064(18) -0.004(2) C3 0.0396(19) 0.0396(19) 0.028(3) -0.0097(17) 0.0097(17) 0.004(2) C4 0.0284(17) 0.0325(19) 0.0280(19) 0.0024(18) 0.0055(15) 0.0014(16) C5 0.033(2) 0.055(3) 0.048(3) -0.009(2) 0.014(2) -0.0031(19) O1 0.074(3) 0.071(3) 0.060(3) -0.034(2) 0.007(2) 0.012(2) O2 0.0509(16) 0.0509(16) 0.061(3) -0.0043(16) -0.0043(16) -0.018(2) F1 0.0438(15) 0.076(2) 0.084(2) -0.0222(19) 0.0367(17) -0.0053(14) F2 0.0400(16) 0.107(3) 0.0609(19) -0.017(2) 0.0008(16) -0.0239(17) F3 0.0631(19) 0.0473(17) 0.082(2) 0.0078(17) 0.0227(17) -0.0131(15) _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 C1 1.904(5) . ? Os1 C1 1.904(5) 8_545 ? Os1 C2 1.960(6) . ? Os1 N1 2.126(3) 8_545 ? Os1 N1 2.126(3) . ? Os1 Os1 2.7457(4) 2_765 ? N1 N1 1.334(6) 7_665 ? N1 C4 1.347(5) . ? C1 O1 1.133(6) . ? C2 O2 1.136(8) . ? C3 C4 1.382(6) . ? C3 C4 1.382(6) 7_665 ? C4 C5 1.482(6) . ? C5 F2 1.314(6) . ? C5 F3 1.326(6) . ? C5 F1 1.344(5) . ? 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 Os1 C1 90.1(3) . 8_545 ? C1 Os1 C2 93.8(2) . . ? C1 Os1 C2 93.8(2) 8_545 . ? C1 Os1 N1 92.27(17) . 8_545 ? C1 Os1 N1 166.63(17) 8_545 8_545 ? C2 Os1 N1 99.19(17) . 8_545 ? C1 Os1 N1 166.63(17) . . ? C1 Os1 N1 92.27(17) 8_545 . ? C2 Os1 N1 99.19(17) . . ? N1 Os1 N1 82.50(17) 8_545 . ? C1 Os1 Os1 96.06(15) . 2_765 ? C1 Os1 Os1 96.06(15) 8_545 2_765 ? C2 Os1 Os1 166.07(19) . 2_765 ? N1 Os1 Os1 70.61(9) 8_545 2_765 ? N1 Os1 Os1 70.61(9) . 2_765 ? N1 N1 C4 108.4(2) 7_665 . ? N1 N1 Os1 109.39(9) 7_665 . ? C4 N1 Os1 142.2(3) . . ? O1 C1 Os1 178.7(5) . . ? O2 C2 Os1 176.4(6) . . ? C4 C3 C4 104.7(5) . 7_665 ? N1 C4 C3 109.2(4) . . ? N1 C4 C5 121.7(4) . . ? C3 C4 C5 129.1(4) . . ? F2 C5 F3 107.3(5) . . ? F2 C5 F1 108.4(4) . . ? F3 C5 F1 106.7(4) . . ? F2 C5 C4 112.2(4) . . ? F3 C5 C4 112.4(4) . . ? F1 C5 C4 109.6(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.625 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.085 #===END