#-----------------------------------------------------------------------------80 # Subsequently are contained the CIF's of two structures # 1 = compound (1) # 2 = compound (3) # separated by #===END #-----------------------------------------------------------------------------80 data_global _publ_contact_author ; Dr. Enrique O\~nate Rodr\'iguez Departamento de Qu\'imica Inorg\'anica - I.C.M.A. Facultad de Ciencias Universidad de Zaragoza - C.S.I.C. 50009 Zaragoza, Spain ; _publ_contact_author_email enriqueo@posta.unizar.es #-----------------------------------------------------------------------------80 #Publication details loop_ _publ_author_name 'Castro-Rodrigo, R.' 'Esteruelas, M. A.' 'Fuetes, S.' 'L\'opez, A. M.' 'L\'opez, F.' 'Mascare\~nas, J. L.' 'Mozo, S.' 'O\~nate, E.' 'Saya, L.' 'Villarino, L.' _publ_requested_journal 'JACS' _journal_name_full ; Journal of the american chemical society ; _publ_section_title ; Formation of Osmium- and Ruthenium-Cyclobutylidene Complexes by Ring Expansion of Alkylidenecyclopropanes ; _publ_contact_letter ; May ##, 2009 Please consider this CIF submission as supplementary material of the structures contained in the paper: Formation of Osmium- and Ruthenium-Cyclobutylidene Complexes by Ring Expansion of Alkylidenecyclopropanes that is submitted to JACS for publication. ; _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year 2009 #-----------------------------------------------------------------------------80 # Data for compound 1 (local labelling mae325as) data_mae325as _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H40 B1 N7 Os1 P1, B1 F4, 0.4x(C3H6O1)' _chemical_formula_sum 'C28.20 H42.40 B2 F4 N7 O0.40 Os P' _chemical_formula_weight 804.68 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' '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' 'P' 'P' 0.1023 0.0942 '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 'Pbca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.356(9) _cell_length_b 14.579(9) _cell_length_c 30.450(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6373(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 935 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 24 _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3206 _exptl_absorpt_coefficient_mu 4.108 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details ; Absorption correction performed with SADABS program. This is based on the method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33. SADABS: Area-Detector Absorption Correction. Bruker-AXS within SAINT+ package, v. 6.1 (2000). ; _diffrn_ambient_temperature 100(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 APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 43796 _diffrn_reflns_av_R_equivalents 0.0879 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6229 _reflns_number_gt 5025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.625 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.1 (Bruker AXS, 2000)' _computing_data_reduction 'SAINT+ v. 6.1 (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.1 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.1 (Bruker, 2000)' _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^)+(0.0228P)^2^+67.5269P] 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 6229 _refine_ls_number_parameters 401 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 1.226 _refine_ls_restrained_S_all 1.236 _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 Os Os 0.43592(2) 0.08489(2) 0.386689(10) 0.01659(10) Uani 1 1 d . . . P P 0.48055(16) 0.02662(16) 0.31592(7) 0.0175(5) Uani 1 1 d . . . F1A F 0.9423(5) 0.1129(5) 0.3371(2) 0.047(2) Uiso 0.840(7) 1 d PDU A 1 F2A F 0.8270(5) 0.0903(5) 0.3843(2) 0.058(2) Uiso 0.840(7) 1 d PDU A 1 F3A F 0.8145(5) 0.2027(5) 0.3334(2) 0.047(2) Uiso 0.840(7) 1 d PDU A 1 F4A F 0.9163(6) 0.2166(6) 0.3900(3) 0.073(3) Uiso 0.840(7) 1 d PDU A 1 F1B F 0.8225(19) 0.2297(16) 0.3787(10) 0.060(6) Uiso 0.160(7) 1 d PDU A 2 F2B F 0.8234(19) 0.1031(19) 0.3357(9) 0.071(7) Uiso 0.160(7) 1 d PDU A 2 F3B F 0.9505(15) 0.194(2) 0.3401(9) 0.058(6) Uiso 0.160(7) 1 d PDU A 2 F4B F 0.908(2) 0.108(2) 0.3979(8) 0.080(7) Uiso 0.160(7) 1 d PDU A 2 N1 N 0.4811(5) 0.2202(5) 0.3763(2) 0.0207(17) Uani 1 1 d . . . N2 N 0.3806(5) 0.1345(5) 0.4470(2) 0.0181(16) Uani 1 1 d . . . N3 N 0.2979(5) 0.1014(5) 0.4622(2) 0.0207(16) Uani 1 1 d . . . N4 N 0.3936(5) -0.0439(5) 0.4094(2) 0.0187(16) Uani 1 1 d . . . N5 N 0.3065(5) -0.0536(5) 0.4270(2) 0.0208(16) Uani 1 1 d . . . N6 N 0.2916(5) 0.1090(4) 0.3643(2) 0.0163(15) Uani 1 1 d . . . N7 N 0.2199(5) 0.0762(5) 0.3903(2) 0.0228(16) Uani 1 1 d . . . B1 B 0.2439(8) 0.0304(7) 0.4343(3) 0.021(2) Uani 1 1 d . . . H1 H 0.182(6) 0.014(6) 0.453(3) 0.026 Uiso 1 1 d . . . B2 B 0.8750(6) 0.1576(6) 0.3618(3) 0.039(3) Uani 1 1 d D . . C1 C 0.5709(7) 0.2392(7) 0.3868(3) 0.034(2) Uani 1 1 d . . . C2 C 0.6075(8) 0.3282(7) 0.3838(3) 0.040(3) Uani 1 1 d . . . H2 H 0.6707 0.3399 0.3912 0.048 Uiso 1 1 calc R . . C3 C 0.5503(10) 0.3980(7) 0.3700(3) 0.046(3) Uani 1 1 d . . . H3 H 0.5745 0.4583 0.3668 0.056 Uiso 1 1 calc R . . C4 C 0.4578(9) 0.3809(7) 0.3609(3) 0.038(3) Uani 1 1 d . . . H4 H 0.4172 0.4291 0.3522 0.046 Uiso 1 1 calc R . . C5 C 0.4251(8) 0.2911(6) 0.3647(3) 0.031(2) Uani 1 1 d . . . H5 H 0.3612 0.2792 0.3590 0.037 Uiso 1 1 calc R . . C6 C 0.6246(7) 0.1575(7) 0.4027(3) 0.024(2) Uani 1 1 d . . . H6 H 0.6748 0.1391 0.3817 0.029 Uiso 1 1 calc R . . C7 C 0.5541(6) 0.0800(6) 0.4106(3) 0.0226(18) Uani 1 1 d . . . C8 C 0.6053(7) 0.0534(7) 0.4531(3) 0.028(2) Uani 1 1 d . . . H8A H 0.6477 0.0002 0.4498 0.034 Uiso 1 1 calc R . . H8B H 0.5638 0.0456 0.4788 0.034 Uiso 1 1 calc R . . C9 C 0.6559(7) 0.1489(7) 0.4513(3) 0.029(2) Uani 1 1 d . . . H9A H 0.6284 0.1957 0.4710 0.035 Uiso 1 1 calc R . . H9B H 0.7243 0.1452 0.4552 0.035 Uiso 1 1 calc R . . C10 C 0.4111(7) 0.1929(6) 0.4773(3) 0.026(2) Uani 1 1 d . . . H10 H 0.4675 0.2266 0.4753 0.031 Uiso 1 1 calc R . . C11 C 0.3492(7) 0.1980(7) 0.5123(3) 0.027(2) Uani 1 1 d . . . H11 H 0.3550 0.2340 0.5381 0.033 Uiso 1 1 calc R . . C12 C 0.2778(6) 0.1399(6) 0.5014(3) 0.022(2) Uani 1 1 d . . . H12 H 0.2236 0.1286 0.5184 0.027 Uiso 1 1 calc R . . C13 C 0.4342(7) -0.1258(6) 0.4121(3) 0.026(2) Uani 1 1 d . . . H13 H 0.4956 -0.1392 0.4024 0.031 Uiso 1 1 calc R . . C14 C 0.3738(8) -0.1887(6) 0.4311(3) 0.031(2) Uani 1 1 d . . . H14 H 0.3851 -0.2517 0.4369 0.037 Uiso 1 1 calc R . . C15 C 0.2948(8) -0.1403(6) 0.4396(3) 0.029(2) Uani 1 1 d . . . H15 H 0.2399 -0.1646 0.4526 0.035 Uiso 1 1 calc R . . C16 C 0.2488(7) 0.1506(6) 0.3309(3) 0.0216(19) Uani 1 1 d . . . H16 H 0.2804 0.1792 0.3071 0.026 Uiso 1 1 calc R . . C17 C 0.1528(6) 0.1469(6) 0.3351(3) 0.024(2) Uani 1 1 d . . . H17 H 0.1072 0.1713 0.3158 0.029 Uiso 1 1 calc R . . C18 C 0.1384(6) 0.1001(6) 0.3735(3) 0.023(2) Uani 1 1 d . . . H18 H 0.0794 0.0870 0.3861 0.027 Uiso 1 1 calc R . . C19 C 0.3770(6) -0.0220(6) 0.2867(3) 0.0183(18) Uani 1 1 d . . . H19 H 0.3312 0.0294 0.2843 0.022 Uiso 1 1 calc R . . C20 C 0.3280(6) -0.0971(6) 0.3123(3) 0.025(2) Uani 1 1 d . . . H20A H 0.2755 -0.1205 0.2951 0.038 Uiso 1 1 calc R . . H20B H 0.3051 -0.0721 0.3402 0.038 Uiso 1 1 calc R . . H20C H 0.3719 -0.1471 0.3182 0.038 Uiso 1 1 calc R . . C21 C 0.3929(7) -0.0563(7) 0.2393(3) 0.031(2) Uani 1 1 d . . . H21A H 0.4300 -0.1127 0.2400 0.047 Uiso 1 1 calc R . . H21B H 0.4263 -0.0093 0.2225 0.047 Uiso 1 1 calc R . . H21C H 0.3327 -0.0687 0.2254 0.047 Uiso 1 1 calc R . . C22 C 0.5673(7) -0.0689(6) 0.3151(3) 0.026(2) Uani 1 1 d . . . H22 H 0.5310 -0.1259 0.3215 0.031 Uiso 1 1 calc R . . C23 C 0.6153(7) -0.0860(8) 0.2704(3) 0.036(2) Uani 1 1 d . . . H23A H 0.6562 -0.0342 0.2634 0.054 Uiso 1 1 calc R . . H23B H 0.5678 -0.0921 0.2474 0.054 Uiso 1 1 calc R . . H23C H 0.6521 -0.1425 0.2719 0.054 Uiso 1 1 calc R . . C24 C 0.6433(7) -0.0648(7) 0.3500(3) 0.031(2) Uani 1 1 d . . . H24A H 0.6822 -0.1198 0.3480 0.046 Uiso 1 1 calc R . . H24B H 0.6145 -0.0616 0.3792 0.046 Uiso 1 1 calc R . . H24C H 0.6818 -0.0102 0.3452 0.046 Uiso 1 1 calc R . . C25 C 0.5272(6) 0.1079(6) 0.2743(3) 0.023(2) Uani 1 1 d . . . H25 H 0.5390 0.0710 0.2472 0.028 Uiso 1 1 calc R . . C26 C 0.4572(7) 0.1814(7) 0.2616(3) 0.028(2) Uani 1 1 d . . . H26A H 0.4411 0.2178 0.2876 0.042 Uiso 1 1 calc R . . H26B H 0.4009 0.1524 0.2499 0.042 Uiso 1 1 calc R . . H26C H 0.4845 0.2214 0.2392 0.042 Uiso 1 1 calc R . . C27 C 0.6203(7) 0.1508(7) 0.2871(3) 0.030(2) Uani 1 1 d . . . H27A H 0.6481 0.1804 0.2613 0.045 Uiso 1 1 calc R . . H27B H 0.6624 0.1029 0.2979 0.045 Uiso 1 1 calc R . . H27C H 0.6103 0.1966 0.3102 0.045 Uiso 1 1 calc R . . O1 O 0.0527(11) 0.1113(8) 0.5156(5) 0.034(3) Uiso 0.40 1 d PD B -1 C28 C 0.0224(14) 0.0458(12) 0.5042(7) 0.034(3) Uiso 0.40 1 d PD B -1 C29 C -0.056(2) 0.0432(9) 0.4708(10) 0.034(3) Uiso 0.40 1 d PD B -1 H29A H -0.0637 0.1041 0.4576 0.052 Uiso 0.40 1 calc PR B -1 H29B H -0.1142 0.0254 0.4854 0.052 Uiso 0.40 1 calc PR B -1 H29C H -0.0413 -0.0015 0.4478 0.052 Uiso 0.40 1 calc PR B -1 C30 C 0.036(2) -0.0472(10) 0.5225(11) 0.034(3) Uiso 0.40 1 d PD B -1 H30A H 0.0877 -0.0463 0.5435 0.052 Uiso 0.40 1 calc PR B -1 H30B H 0.0500 -0.0901 0.4987 0.052 Uiso 0.40 1 calc PR B -1 H30C H -0.0211 -0.0667 0.5376 0.052 Uiso 0.40 1 calc PR B -1 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 0.02100(17) 0.01297(16) 0.01579(16) -0.00044(14) -0.00012(15) -0.00081(15) P 0.0190(11) 0.0169(12) 0.0165(11) -0.0021(9) 0.0014(9) -0.0018(9) N1 0.033(4) 0.013(4) 0.016(4) 0.000(3) 0.000(3) -0.002(3) N2 0.021(4) 0.019(4) 0.015(4) -0.001(3) 0.004(3) 0.001(3) N3 0.027(4) 0.014(4) 0.021(4) 0.001(3) 0.000(3) 0.004(3) N4 0.023(4) 0.011(4) 0.022(4) -0.001(3) -0.003(3) -0.003(3) N5 0.030(4) 0.015(4) 0.018(4) 0.001(3) 0.001(3) -0.004(3) N6 0.019(4) 0.012(4) 0.019(4) 0.000(3) 0.003(3) 0.002(3) N7 0.035(4) 0.014(4) 0.019(4) 0.002(3) 0.009(3) -0.005(3) B1 0.027(6) 0.018(5) 0.020(5) 0.001(4) -0.001(4) -0.002(5) B2 0.037(7) 0.056(9) 0.023(6) -0.008(6) 0.004(5) -0.006(6) C1 0.043(6) 0.036(6) 0.022(4) -0.004(5) 0.007(5) -0.014(5) C2 0.057(7) 0.039(7) 0.023(5) -0.007(5) 0.008(5) -0.032(6) C3 0.094(10) 0.021(6) 0.025(5) -0.006(4) 0.009(6) -0.025(6) C4 0.079(9) 0.013(5) 0.022(5) 0.011(4) 0.002(5) -0.005(5) C5 0.054(7) 0.022(5) 0.017(4) -0.002(4) 0.000(5) 0.004(5) C6 0.027(5) 0.030(6) 0.015(4) -0.007(4) 0.001(4) -0.011(4) C7 0.023(5) 0.022(5) 0.024(4) -0.003(4) 0.005(4) -0.002(4) C8 0.032(5) 0.030(6) 0.023(5) -0.001(4) 0.000(4) -0.002(4) C9 0.025(5) 0.037(6) 0.026(5) -0.006(4) -0.001(4) -0.008(4) C10 0.033(6) 0.019(5) 0.025(5) -0.004(4) -0.010(4) 0.004(4) C11 0.035(6) 0.026(5) 0.021(5) -0.002(4) -0.001(4) 0.012(4) C12 0.028(5) 0.023(5) 0.016(4) 0.001(4) 0.006(4) 0.005(4) C13 0.035(5) 0.021(5) 0.020(5) 0.005(4) -0.005(4) 0.000(5) C14 0.060(7) 0.010(5) 0.021(5) 0.003(4) -0.004(5) 0.002(5) C15 0.047(6) 0.015(5) 0.025(5) 0.003(4) -0.001(4) -0.013(5) C16 0.026(5) 0.012(5) 0.026(5) -0.001(4) -0.003(4) 0.005(4) C17 0.030(5) 0.023(5) 0.021(5) -0.008(4) -0.010(4) 0.012(4) C18 0.021(5) 0.023(5) 0.024(5) -0.006(4) -0.002(4) 0.000(4) C19 0.018(4) 0.021(5) 0.017(4) 0.001(4) 0.000(3) 0.001(4) C20 0.028(5) 0.020(5) 0.028(5) 0.001(4) -0.003(4) -0.006(4) C21 0.026(5) 0.044(7) 0.024(5) -0.006(4) 0.004(4) -0.004(5) C22 0.025(5) 0.019(5) 0.033(5) -0.004(4) -0.007(4) 0.002(4) C23 0.028(5) 0.046(7) 0.034(5) -0.019(5) 0.004(4) 0.010(5) C24 0.030(5) 0.025(6) 0.037(6) -0.004(4) -0.001(4) 0.013(4) C25 0.031(5) 0.023(5) 0.015(4) -0.005(4) 0.004(4) -0.008(4) C26 0.034(6) 0.026(5) 0.024(5) 0.005(4) 0.004(4) -0.005(4) C27 0.035(6) 0.037(6) 0.018(5) -0.003(4) 0.005(4) -0.012(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 Os C7 1.847(9) . ? Os N4 2.092(7) . ? Os N1 2.100(7) . ? Os N2 2.127(7) . ? Os N6 2.210(7) . ? Os P 2.403(2) . ? P C25 1.858(9) . ? P C22 1.869(9) . ? P C19 1.872(9) . ? F1A B2 1.387(8) . ? F2A B2 1.381(8) . ? F3A B2 1.391(8) . ? F4A B2 1.352(8) . ? F1B B2 1.393(10) . ? F2B B2 1.345(10) . ? F3B B2 1.378(10) . ? F4B B2 1.395(10) . ? N1 C1 1.357(12) . ? N1 C5 1.357(12) . ? N2 C10 1.331(11) . ? N2 N3 1.362(10) . ? N3 C12 1.350(10) . ? N3 B1 1.547(12) . ? N4 C13 1.330(11) . ? N4 N5 1.368(10) . ? N5 C15 1.332(11) . ? N5 B1 1.535(13) . ? N6 C16 1.333(11) . ? N6 N7 1.384(9) . ? N7 C18 1.324(11) . ? N7 B1 1.538(12) . ? B1 H1 1.08(9) . ? C1 C2 1.402(13) . ? C1 C6 1.498(14) . ? C2 C3 1.375(16) . ? C2 H2 0.9500 . ? C3 C4 1.380(17) . ? C3 H3 0.9500 . ? C4 C5 1.396(13) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.536(12) . ? C6 C9 1.553(12) . ? C6 H6 1.0000 . ? C7 C8 1.538(12) . ? C8 C9 1.572(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.388(13) . ? C10 H10 0.9500 . ? C11 C12 1.370(13) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.389(13) . ? C13 H13 0.9500 . ? C14 C15 1.359(14) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.386(13) . ? C16 H16 0.9500 . ? C17 C18 1.368(13) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.517(12) . ? C19 C21 1.543(12) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.524(12) . ? C22 C23 1.545(12) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.519(13) . ? C25 C27 1.527(12) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O1 C28 1.105(17) . ? C28 C30 1.479(10) . ? C28 C29 1.519(9) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 C7 Os N4 95.9(3) . . ? C7 Os N1 79.1(4) . . ? N4 Os N1 169.3(3) . . ? C7 Os N2 90.9(3) . . ? N4 Os N2 84.9(3) . . ? N1 Os N2 85.8(3) . . ? C7 Os N6 171.4(3) . . ? N4 Os N6 88.4(3) . . ? N1 Os N6 95.4(3) . . ? N2 Os N6 82.1(3) . . ? C7 Os P 95.5(3) . . ? N4 Os P 93.3(2) . . ? N1 Os P 96.59(19) . . ? N2 Os P 173.5(2) . . ? N6 Os P 91.67(18) . . ? C25 P C22 103.0(4) . . ? C25 P C19 101.7(4) . . ? C22 P C19 103.9(4) . . ? C25 P Os 118.8(3) . . ? C22 P Os 117.0(3) . . ? C19 P Os 110.4(3) . . ? C1 N1 C5 117.9(8) . . ? C1 N1 Os 116.8(6) . . ? C5 N1 Os 124.9(7) . . ? C10 N2 N3 106.1(7) . . ? C10 N2 Os 134.0(6) . . ? N3 N2 Os 119.9(5) . . ? C12 N3 N2 109.8(7) . . ? C12 N3 B1 131.0(8) . . ? N2 N3 B1 119.2(7) . . ? C13 N4 N5 106.5(7) . . ? C13 N4 Os 134.3(6) . . ? N5 N4 Os 119.2(5) . . ? C15 N5 N4 109.0(8) . . ? C15 N5 B1 129.9(8) . . ? N4 N5 B1 120.6(7) . . ? C16 N6 N7 104.6(7) . . ? C16 N6 Os 137.7(6) . . ? N7 N6 Os 117.7(5) . . ? C18 N7 N6 110.2(7) . . ? C18 N7 B1 130.5(8) . . ? N6 N7 B1 118.9(7) . . ? N5 B1 N7 110.5(7) . . ? N5 B1 N3 108.7(8) . . ? N7 B1 N3 107.5(7) . . ? N5 B1 H1 112(5) . . ? N7 B1 H1 112(5) . . ? N3 B1 H1 105(5) . . ? F2B B2 F4A 172.5(14) . . ? F2B B2 F3B 112.3(9) . . ? F4A B2 F3B 73.3(13) . . ? F2B B2 F2A 66.3(14) . . ? F4A B2 F2A 110.8(7) . . ? F3B B2 F2A 155.1(14) . . ? F2B B2 F1A 77.7(14) . . ? F4A B2 F1A 109.8(7) . . ? F3B B2 F1A 51.3(13) . . ? F2A B2 F1A 106.5(6) . . ? F2B B2 F3A 64.5(14) . . ? F4A B2 F3A 111.5(7) . . ? F3B B2 F3A 90.5(14) . . ? F2A B2 F3A 109.4(6) . . ? F1A B2 F3A 108.7(6) . . ? F2B B2 F1B 111.4(9) . . ? F4A B2 F1B 61.4(13) . . ? F3B B2 F1B 108.0(8) . . ? F2A B2 F1B 94.7(14) . . ? F1A B2 F1B 158.8(13) . . ? F3A B2 F1B 62.2(13) . . ? F2B B2 F4B 110.4(9) . . ? F4A B2 F4B 71.2(14) . . ? F3B B2 F4B 108.0(9) . . ? F2A B2 F4B 54.2(14) . . ? F1A B2 F4B 87.0(14) . . ? F3A B2 F4B 161.0(14) . . ? F1B B2 F4B 106.4(8) . . ? N1 C1 C2 122.0(10) . . ? N1 C1 C6 113.7(8) . . ? C2 C1 C6 124.3(10) . . ? C3 C2 C1 118.7(11) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 120.2(10) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 118.4(10) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 122.5(10) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C1 C6 C7 107.3(8) . . ? C1 C6 C9 121.4(8) . . ? C7 C6 C9 88.9(7) . . ? C1 C6 H6 112.2 . . ? C7 C6 H6 112.2 . . ? C9 C6 H6 112.2 . . ? C6 C7 C8 90.2(7) . . ? C6 C7 Os 121.0(7) . . ? C8 C7 Os 141.3(7) . . ? C7 C8 C9 88.1(7) . . ? C7 C8 H8A 114.0 . . ? C9 C8 H8A 114.0 . . ? C7 C8 H8B 114.0 . . ? C9 C8 H8B 114.0 . . ? H8A C8 H8B 111.2 . . ? C6 C9 C8 88.3(7) . . ? C6 C9 H9A 113.9 . . ? C8 C9 H9A 113.9 . . ? C6 C9 H9B 113.9 . . ? C8 C9 H9B 113.9 . . ? H9A C9 H9B 111.1 . . ? N2 C10 C11 110.9(9) . . ? N2 C10 H10 124.6 . . ? C11 C10 H10 124.6 . . ? C12 C11 C10 105.0(8) . . ? C12 C11 H11 127.5 . . ? C10 C11 H11 127.5 . . ? N3 C12 C11 108.2(8) . . ? N3 C12 H12 125.9 . . ? C11 C12 H12 125.9 . . ? N4 C13 C14 110.2(9) . . ? N4 C13 H13 124.9 . . ? C14 C13 H13 124.9 . . ? C15 C14 C13 104.9(8) . . ? C15 C14 H14 127.5 . . ? C13 C14 H14 127.5 . . ? N5 C15 C14 109.4(9) . . ? N5 C15 H15 125.3 . . ? C14 C15 H15 125.3 . . ? N6 C16 C17 111.7(8) . . ? N6 C16 H16 124.2 . . ? C17 C16 H16 124.2 . . ? C18 C17 C16 104.4(8) . . ? C18 C17 H17 127.8 . . ? C16 C17 H17 127.8 . . ? N7 C18 C17 109.1(8) . . ? N7 C18 H18 125.4 . . ? C17 C18 H18 125.4 . . ? C20 C19 C21 108.4(7) . . ? C20 C19 P 113.3(6) . . ? C21 C19 P 116.7(6) . . ? C20 C19 H19 105.9 . . ? C21 C19 H19 105.9 . . ? P C19 H19 105.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C23 107.6(8) . . ? C24 C22 P 115.9(6) . . ? C23 C22 P 115.4(7) . . ? C24 C22 H22 105.6 . . ? C23 C22 H22 105.6 . . ? P C22 H22 105.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 110.8(8) . . ? C26 C25 P 112.6(6) . . ? C27 C25 P 113.8(6) . . ? C26 C25 H25 106.3 . . ? C27 C25 H25 106.3 . . ? P C25 H25 106.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O1 C28 C30 128.3(13) . . ? O1 C28 C29 121.7(10) . . ? C30 C28 C29 109.1(17) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.516 _refine_diff_density_min -2.681 _refine_diff_density_rms 0.167 #===END #-----------------------------------------------------------------------------80 # Data for compound 3 (local labelling mae372as) data_mae372as _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H35 N1 Os1 P1, P1 F6, C3 H4 O1' _chemical_formula_sum 'C26 H41 F6 N O Os P2' _chemical_formula_weight 749.74 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' 'N' 'N' 0.0061 0.0033 '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' 'P' 'P' 0.1023 0.0942 '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' 'O' 'O' 0.0106 0.0060 '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 9.1653(11) _cell_length_b 11.1937(13) _cell_length_c 14.2705(17) _cell_angle_alpha 78.851(2) _cell_angle_beta 89.570(2) _cell_angle_gamma 89.340(2) _cell_volume 1436.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3930 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 24 _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 4.610 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.678 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details ; Absorption correction performed with SADABS program. This is based on the method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33. SADABS: Area-Detector Absorption Correction. Bruker-AXS within SAINT+ package, v. 6.1 (2000). ; _diffrn_ambient_temperature 150(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 APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 18125 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 28.81 _reflns_number_total 6887 _reflns_number_gt 6173 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.625 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.1 (Bruker AXS, 2000)' _computing_data_reduction 'SAINT+ v. 6.1 (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.1 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.1 (Bruker, 2000)' _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^)+(0.0249P)^2^+2.0238P] 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 6887 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 Os Os 0.81214(2) 0.740156(17) 0.677800(13) 0.01849(6) Uani 1 1 d . . . P1 P 0.72006(14) 0.54710(11) 0.74198(9) 0.0198(3) Uani 1 1 d . . . P2 P 0.18891(15) 0.16526(13) 0.75332(10) 0.0297(3) Uani 1 1 d . . . F1 F 0.1373(4) 0.3025(3) 0.7175(3) 0.0680(12) Uani 1 1 d . . . F2 F 0.1546(4) 0.1363(3) 0.6505(2) 0.0540(10) Uani 1 1 d . . . F3 F 0.2402(4) 0.0274(3) 0.7870(2) 0.0488(9) Uani 1 1 d . . . F4 F 0.2250(5) 0.1921(4) 0.8552(3) 0.0719(13) Uani 1 1 d . . . F5 F 0.3499(4) 0.2022(3) 0.7181(3) 0.0487(9) Uani 1 1 d . . . F6 F 0.0274(4) 0.1268(4) 0.7877(3) 0.0610(11) Uani 1 1 d . . . O O 0.2760(5) 0.7259(4) 0.9103(3) 0.0462(11) Uani 1 1 d . . . N N 0.6151(4) 0.7938(3) 0.6086(3) 0.0208(8) Uani 1 1 d . . . C1 C 0.7133(5) 0.8118(4) 0.7697(3) 0.0229(10) Uani 1 1 d . . . C2 C 0.7400(6) 0.9026(5) 0.8345(4) 0.0291(12) Uani 1 1 d . . . H2A H 0.828(6) 0.936(5) 0.832(4) 0.035 Uiso 1 1 d . . . H2B H 0.715(6) 0.875(5) 0.896(4) 0.035 Uiso 1 1 d . . . C3 C 0.6139(6) 0.9782(5) 0.7785(4) 0.0329(13) Uani 1 1 d . . . H3A H 0.541(6) 1.029(5) 0.822(4) 0.039 Uiso 1 1 d . . . H3B H 0.653(6) 1.028(5) 0.721(4) 0.039 Uiso 1 1 d . . . C4 C 0.5564(5) 0.8578(5) 0.7536(4) 0.0230(10) Uani 1 1 d . . . H4 H 0.490(6) 0.825(5) 0.794(4) 0.028 Uiso 1 1 d . . . C5 C 0.5109(5) 0.8488(4) 0.6557(3) 0.0224(10) Uani 1 1 d . . . C6 C 0.5898(5) 0.7878(4) 0.5166(3) 0.0241(10) Uani 1 1 d . . . H6 H 0.6630 0.7538 0.4819 0.029 Uiso 1 1 calc R . . C7 C 0.4611(6) 0.8295(4) 0.4709(4) 0.0273(11) Uani 1 1 d . . . H7 H 0.4467 0.8241 0.4061 0.033 Uiso 1 1 calc R . . C8 C 0.3543(6) 0.8789(5) 0.5205(4) 0.0283(11) Uani 1 1 d . . . H8 H 0.2642 0.9060 0.4909 0.034 Uiso 1 1 calc R . . C9 C 0.3800(5) 0.8883(4) 0.6135(4) 0.0261(11) Uani 1 1 d . . . H9 H 0.3073 0.9221 0.6487 0.031 Uiso 1 1 calc R . . C10 C 1.0519(5) 0.7542(6) 0.7075(4) 0.0382(14) Uani 1 1 d . . . H10 H 1.0893 0.7396 0.7706 0.046 Uiso 1 1 calc R . . C11 C 1.0345(5) 0.6668(5) 0.6469(4) 0.0338(13) Uani 1 1 d . . . H11 H 1.0582 0.5826 0.6639 0.041 Uiso 1 1 calc R . . C12 C 0.9772(5) 0.7248(5) 0.5590(4) 0.0322(12) Uani 1 1 d . . . H12 H 0.9581 0.6878 0.5058 0.039 Uiso 1 1 calc R . . C13 C 0.9532(6) 0.8473(5) 0.5635(4) 0.0329(13) Uani 1 1 d . . . H13 H 0.9115 0.9074 0.5146 0.040 Uiso 1 1 calc R . . C14 C 1.0017(6) 0.8662(5) 0.6537(4) 0.0385(14) Uani 1 1 d . . . H14 H 1.0005 0.9418 0.6744 0.046 Uiso 1 1 calc R . . C15 C 0.7817(5) 0.4280(5) 0.6753(4) 0.0263(11) Uani 1 1 d . . . H15 H 0.8907 0.4283 0.6777 0.032 Uiso 1 1 calc R . . C16 C 0.7433(6) 0.4562(5) 0.5679(4) 0.0335(13) Uani 1 1 d . . . H16A H 0.8016 0.4034 0.5344 0.050 Uiso 1 1 calc R . . H16B H 0.7647 0.5416 0.5413 0.050 Uiso 1 1 calc R . . H16C H 0.6394 0.4413 0.5601 0.050 Uiso 1 1 calc R . . C17 C 0.7378(6) 0.2990(5) 0.7202(4) 0.0329(12) Uani 1 1 d . . . H17A H 0.6315 0.2921 0.7183 0.049 Uiso 1 1 calc R . . H17B H 0.7706 0.2802 0.7867 0.049 Uiso 1 1 calc R . . H17C H 0.7832 0.2416 0.6846 0.049 Uiso 1 1 calc R . . C18 C 0.7880(6) 0.4880(5) 0.8636(3) 0.0269(11) Uani 1 1 d . . . H18 H 0.7391 0.4083 0.8866 0.032 Uiso 1 1 calc R . . C19 C 0.7447(6) 0.5710(5) 0.9333(4) 0.0348(13) Uani 1 1 d . . . H19A H 0.7643 0.5289 0.9988 0.052 Uiso 1 1 calc R . . H19B H 0.6405 0.5912 0.9265 0.052 Uiso 1 1 calc R . . H19C H 0.8015 0.6460 0.9190 0.052 Uiso 1 1 calc R . . C20 C 0.9508(6) 0.4631(5) 0.8690(4) 0.0340(13) Uani 1 1 d . . . H20A H 1.0032 0.5400 0.8505 0.051 Uiso 1 1 calc R . . H20B H 0.9776 0.4085 0.8256 0.051 Uiso 1 1 calc R . . H20C H 0.9769 0.4249 0.9345 0.051 Uiso 1 1 calc R . . C21 C 0.5183(5) 0.5385(5) 0.7581(4) 0.0273(11) Uani 1 1 d . . . H21 H 0.4886 0.6173 0.7762 0.033 Uiso 1 1 calc R . . C22 C 0.4340(6) 0.5342(5) 0.6661(4) 0.0324(12) Uani 1 1 d . . . H22A H 0.4405 0.4519 0.6523 0.049 Uiso 1 1 calc R . . H22B H 0.4763 0.5923 0.6129 0.049 Uiso 1 1 calc R . . H22C H 0.3314 0.5556 0.6745 0.049 Uiso 1 1 calc R . . C23 C 0.4592(6) 0.4390(5) 0.8386(4) 0.0377(14) Uani 1 1 d . . . H23A H 0.3534 0.4496 0.8446 0.057 Uiso 1 1 calc R . . H23B H 0.5060 0.4453 0.8989 0.057 Uiso 1 1 calc R . . H23C H 0.4804 0.3588 0.8236 0.057 Uiso 1 1 calc R . . C24 C 0.2466(6) 0.8034(5) 0.9560(4) 0.0333(13) Uani 1 1 d . . . C25 C 0.3630(8) 0.8685(6) 0.9987(4) 0.0531(18) Uani 1 1 d . . . H25A H 0.4527 0.8191 1.0058 0.080 Uiso 1 1 calc R . . H25B H 0.3307 0.8819 1.0615 0.080 Uiso 1 1 calc R . . H25C H 0.3818 0.9471 0.9568 0.080 Uiso 1 1 calc R . . C26 C 0.0915(7) 0.8409(6) 0.9711(5) 0.0525(18) Uani 1 1 d . . . H26A H 0.0250 0.7868 0.9461 0.079 Uiso 1 1 calc R . . H26B H 0.0754 0.9250 0.9375 0.079 Uiso 1 1 calc R . . H26C H 0.0730 0.8354 1.0395 0.079 Uiso 1 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 0.01567(10) 0.01847(10) 0.02103(10) -0.00317(7) 0.00086(7) 0.00026(7) P1 0.0201(6) 0.0187(6) 0.0208(6) -0.0042(5) -0.0013(5) 0.0017(5) P2 0.0279(7) 0.0285(7) 0.0333(8) -0.0078(6) 0.0054(6) -0.0005(6) F1 0.061(3) 0.030(2) 0.106(3) 0.004(2) 0.025(2) 0.0168(18) F2 0.072(3) 0.056(2) 0.0330(19) -0.0056(17) -0.0069(18) -0.017(2) F3 0.063(2) 0.0341(19) 0.046(2) 0.0015(16) 0.0063(18) 0.0081(17) F4 0.091(3) 0.087(3) 0.049(2) -0.039(2) 0.011(2) -0.028(3) F5 0.0299(18) 0.054(2) 0.062(2) -0.0127(19) 0.0129(17) -0.0080(16) F6 0.029(2) 0.068(3) 0.081(3) -0.002(2) 0.0141(19) -0.0059(18) O 0.061(3) 0.042(3) 0.037(2) -0.011(2) 0.001(2) -0.003(2) N 0.016(2) 0.021(2) 0.025(2) -0.0047(17) 0.0027(16) -0.0033(16) C1 0.024(3) 0.018(2) 0.026(3) -0.0025(19) -0.001(2) -0.004(2) C2 0.030(3) 0.029(3) 0.032(3) -0.015(2) -0.009(2) 0.003(2) C3 0.037(3) 0.025(3) 0.040(3) -0.014(2) -0.006(3) 0.007(2) C4 0.020(3) 0.024(3) 0.026(3) -0.007(2) 0.002(2) 0.000(2) C5 0.022(2) 0.017(2) 0.028(3) -0.0015(19) 0.003(2) -0.0012(19) C6 0.025(3) 0.021(2) 0.026(3) -0.003(2) 0.004(2) 0.000(2) C7 0.029(3) 0.024(3) 0.028(3) -0.003(2) -0.005(2) -0.002(2) C8 0.021(3) 0.024(3) 0.040(3) -0.006(2) -0.007(2) -0.001(2) C9 0.019(2) 0.021(3) 0.039(3) -0.007(2) 0.001(2) -0.002(2) C10 0.015(3) 0.071(4) 0.027(3) -0.006(3) 0.000(2) -0.011(3) C11 0.015(3) 0.035(3) 0.050(4) -0.006(3) 0.008(2) 0.001(2) C12 0.017(3) 0.048(3) 0.034(3) -0.013(3) 0.006(2) -0.004(2) C13 0.022(3) 0.035(3) 0.035(3) 0.008(2) 0.009(2) -0.005(2) C14 0.030(3) 0.033(3) 0.057(4) -0.020(3) 0.012(3) -0.017(3) C15 0.022(3) 0.026(3) 0.033(3) -0.011(2) -0.003(2) 0.005(2) C16 0.041(3) 0.033(3) 0.030(3) -0.013(2) 0.001(2) 0.001(3) C17 0.041(3) 0.023(3) 0.035(3) -0.005(2) -0.009(3) 0.007(2) C18 0.034(3) 0.023(3) 0.023(3) -0.004(2) -0.004(2) -0.001(2) C19 0.043(3) 0.039(3) 0.022(3) -0.004(2) -0.001(2) -0.001(3) C20 0.036(3) 0.031(3) 0.035(3) -0.006(2) -0.015(2) 0.006(2) C21 0.020(3) 0.027(3) 0.035(3) -0.006(2) 0.004(2) -0.003(2) C22 0.022(3) 0.035(3) 0.038(3) -0.002(2) -0.006(2) -0.003(2) C23 0.035(3) 0.044(3) 0.034(3) -0.007(3) 0.007(3) -0.006(3) C24 0.045(3) 0.031(3) 0.020(3) 0.004(2) 0.000(2) -0.004(3) C25 0.062(5) 0.061(5) 0.036(4) -0.008(3) -0.006(3) -0.016(4) C26 0.041(4) 0.058(4) 0.051(4) 0.009(3) 0.008(3) 0.005(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 Os C1 1.886(5) . ? Os N 2.090(4) . ? Os C14 2.233(5) . ? Os C13 2.240(5) . ? Os C10 2.254(5) . ? Os C11 2.260(5) . ? Os C12 2.294(5) . ? Os P1 2.3422(13) . ? P1 C18 1.844(5) . ? P1 C15 1.862(5) . ? P1 C21 1.863(5) . ? P2 F4 1.579(4) . ? P2 F5 1.589(3) . ? P2 F1 1.591(4) . ? P2 F3 1.592(4) . ? P2 F6 1.594(4) . ? P2 F2 1.596(4) . ? O C24 1.209(6) . ? N C6 1.350(6) . ? N C5 1.370(6) . ? C1 C2 1.524(7) . ? C1 C4 1.525(7) . ? C2 C3 1.556(8) . ? C2 H2A 0.89(6) . ? C2 H2B 0.90(6) . ? C3 C4 1.557(7) . ? C3 H3A 1.13(6) . ? C3 H3B 0.97(6) . ? C4 C5 1.483(7) . ? C4 H4 0.87(5) . ? C5 C9 1.376(7) . ? C6 C7 1.383(7) . ? C6 H6 0.9500 . ? C7 C8 1.376(7) . ? C7 H7 0.9500 . ? C8 C9 1.374(7) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C14 1.412(8) . ? C10 C11 1.436(8) . ? C10 H10 0.9500 . ? C11 C12 1.400(8) . ? C11 H11 0.9500 . ? C12 C13 1.399(8) . ? C12 H12 0.9500 . ? C13 C14 1.419(8) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C17 1.520(7) . ? C15 C16 1.545(7) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.515(7) . ? C18 C19 1.534(7) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.537(7) . ? C21 C22 1.538(7) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.496(8) . ? C24 C26 1.504(8) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 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 C1 Os N 78.47(18) . . ? C1 Os C14 97.8(2) . . ? N Os C14 119.3(2) . . ? C1 Os C13 122.6(2) . . ? N Os C13 95.23(18) . . ? C14 Os C13 37.0(2) . . ? C1 Os C10 105.9(2) . . ? N Os C10 155.40(19) . . ? C14 Os C10 36.7(2) . . ? C13 Os C10 61.7(2) . . ? C1 Os C11 140.9(2) . . ? N Os C11 139.84(19) . . ? C14 Os C11 60.7(2) . . ? C13 Os C11 60.3(2) . . ? C10 Os C11 37.1(2) . . ? C1 Os C12 157.5(2) . . ? N Os C12 105.73(17) . . ? C14 Os C12 60.6(2) . . ? C13 Os C12 35.93(19) . . ? C10 Os C12 61.22(19) . . ? C11 Os C12 35.8(2) . . ? C1 Os P1 92.24(15) . . ? N Os P1 91.46(11) . . ? C14 Os P1 148.92(17) . . ? C13 Os P1 145.17(15) . . ? C10 Os P1 112.24(17) . . ? C11 Os P1 93.64(15) . . ? C12 Os P1 109.53(15) . . ? C18 P1 C15 102.7(2) . . ? C18 P1 C21 102.8(2) . . ? C15 P1 C21 109.1(2) . . ? C18 P1 Os 112.25(17) . . ? C15 P1 Os 112.97(17) . . ? C21 P1 Os 115.80(17) . . ? F4 P2 F5 90.2(2) . . ? F4 P2 F1 90.9(3) . . ? F5 P2 F1 89.4(2) . . ? F4 P2 F3 90.3(2) . . ? F5 P2 F3 90.4(2) . . ? F1 P2 F3 178.8(2) . . ? F4 P2 F6 90.4(2) . . ? F5 P2 F6 179.2(2) . . ? F1 P2 F6 91.0(2) . . ? F3 P2 F6 89.1(2) . . ? F4 P2 F2 179.0(3) . . ? F5 P2 F2 89.3(2) . . ? F1 P2 F2 90.0(2) . . ? F3 P2 F2 88.8(2) . . ? F6 P2 F2 90.0(2) . . ? C6 N C5 117.7(4) . . ? C6 N Os 123.5(3) . . ? C5 N Os 118.6(3) . . ? C2 C1 C4 90.5(4) . . ? C2 C1 Os 139.8(4) . . ? C4 C1 Os 120.9(3) . . ? C1 C2 C3 85.4(4) . . ? C1 C2 H2A 118(4) . . ? C3 C2 H2A 118(4) . . ? C1 C2 H2B 114(4) . . ? C3 C2 H2B 112(4) . . ? H2A C2 H2B 109(5) . . ? C2 C3 C4 88.2(4) . . ? C2 C3 H3A 115(3) . . ? C4 C3 H3A 118(3) . . ? C2 C3 H3B 109(4) . . ? C4 C3 H3B 109(3) . . ? H3A C3 H3B 114(4) . . ? C5 C4 C1 109.4(4) . . ? C5 C4 C3 122.4(4) . . ? C1 C4 C3 85.3(4) . . ? C5 C4 H4 109(3) . . ? C1 C4 H4 118(4) . . ? C3 C4 H4 111(3) . . ? N C5 C9 121.5(4) . . ? N C5 C4 112.4(4) . . ? C9 C5 C4 126.1(4) . . ? N C6 C7 122.4(5) . . ? N C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C8 C7 C6 119.3(5) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C9 C8 C7 118.9(5) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C5 120.1(5) . . ? C8 C9 H9 120.0 . . ? C5 C9 H9 120.0 . . ? C14 C10 C11 105.6(5) . . ? C14 C10 Os 70.9(3) . . ? C11 C10 Os 71.7(3) . . ? C14 C10 H10 127.2 . . ? C11 C10 H10 127.2 . . ? Os C10 H10 122.1 . . ? C12 C11 C10 109.5(5) . . ? C12 C11 Os 73.4(3) . . ? C10 C11 Os 71.2(3) . . ? C12 C11 H11 125.2 . . ? C10 C11 H11 125.2 . . ? Os C11 H11 121.8 . . ? C13 C12 C11 107.6(5) . . ? C13 C12 Os 69.9(3) . . ? C11 C12 Os 70.8(3) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? Os C12 H12 124.7 . . ? C12 C13 C14 108.3(5) . . ? C12 C13 Os 74.2(3) . . ? C14 C13 Os 71.2(3) . . ? C12 C13 H13 125.9 . . ? C14 C13 H13 125.9 . . ? Os C13 H13 120.5 . . ? C10 C14 C13 108.9(5) . . ? C10 C14 Os 72.5(3) . . ? C13 C14 Os 71.8(3) . . ? C10 C14 H14 125.6 . . ? C13 C14 H14 125.6 . . ? Os C14 H14 121.9 . . ? C17 C15 C16 110.5(4) . . ? C17 C15 P1 114.9(4) . . ? C16 C15 P1 114.2(3) . . ? C17 C15 H15 105.4 . . ? C16 C15 H15 105.4 . . ? P1 C15 H15 105.4 . . ? 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 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C19 109.8(4) . . ? C20 C18 P1 114.4(4) . . ? C19 C18 P1 112.0(4) . . ? C20 C18 H18 106.8 . . ? C19 C18 H18 106.8 . . ? P1 C18 H18 106.8 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C22 108.6(4) . . ? C23 C21 P1 117.2(4) . . ? C22 C21 P1 114.1(4) . . ? C23 C21 H21 105.2 . . ? C22 C21 H21 105.2 . . ? P1 C21 H21 105.2 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O C24 C25 121.6(6) . . ? O C24 C26 121.7(6) . . ? C25 C24 C26 116.7(6) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.663 _refine_diff_density_min -1.832 _refine_diff_density_rms 0.146 #===END