# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef 'web_deposit_cif_file_0_MontserratOlivan_1324462838.CC-helicenes.cif' _publ_contact_author ; Dr. Montserrat Oliv\'an Departamento de Qu\'imica Inorg\'anica - ISQCH Universidad de Zaragoza - CSIC 50009 Zaragoza, Spain ; _publ_contact_author_email molivan@unizar.es _publ_section_title ; Preparation and Characterisation of [6]-Azaosmahelicenes: The First d4-Heterometallahelicenes ; _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _publ_contact_author_name 'Dr. Montserrat Olivan' loop_ _publ_author_name O.Crespo B.Eguillor M.A.Esteruelas I.Fernandez ; J.Garcia-Raboso ; M.Gomez-Gallego M.Martin-Ortiz M.Olivan M.A.Sierra #-----------------------------------------------------------------------------80 # Data for compound 1a (local labelling montse11s) data_montse11s _database_code_depnum_ccdc_archive 'CCDC 859551' #TrackingRef 'web_deposit_cif_file_0_MontserratOlivan_1324462838.CC-helicenes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H17 N' _chemical_formula_weight 319.39 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' _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 6.1897(6) _cell_length_b 11.9527(11) _cell_length_c 21.870(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.2010(10) _cell_angle_gamma 90.00 _cell_volume 1615.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3589 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.689 _exptl_absorpt_correction_T_max 0.957 _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). ; _exptl_special_details ; ? ; _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 14407 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.64 _reflns_number_total 3802 _reflns_number_gt 2418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2008.4-0, Bruker AXS' _computing_cell_refinement 'APEX2 v2008.4-0, Bruker AXS' _computing_data_reduction ; SAINT-Bruker integration program embedded in APEX2 v2008.4-0, Bruker AXS ; _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^)+(0.0467P)^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 3802 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _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 N1 N 0.51118(19) -0.02756(10) 0.40066(5) 0.0269(3) Uani 1 1 d . . . C1 C 0.5909(2) -0.08252(12) 0.45032(6) 0.0298(3) Uani 1 1 d . . . H1 H 0.4909 -0.1115 0.4777 0.036 Uiso 1 1 calc R . . C2 C 0.8085(2) -0.09989(12) 0.46451(7) 0.0314(4) Uani 1 1 d . . . H2 H 0.8562 -0.1397 0.5004 0.038 Uiso 1 1 calc R . . C3 C 0.9547(2) -0.05755(12) 0.42496(7) 0.0291(3) Uani 1 1 d . . . H3 H 1.1058 -0.0674 0.4332 0.035 Uiso 1 1 calc R . . C4 C 0.8780(2) -0.00092(11) 0.37340(6) 0.0250(3) Uani 1 1 d . . . H4 H 0.9760 0.0284 0.3456 0.030 Uiso 1 1 calc R . . C5 C 0.6552(2) 0.01316(11) 0.36215(6) 0.0226(3) Uani 1 1 d . . . C6 C 0.5635(2) 0.06136(11) 0.30345(6) 0.0221(3) Uani 1 1 d . . . C7 C 0.3832(2) 0.00802(11) 0.27701(6) 0.0250(3) Uani 1 1 d . . . H7 H 0.3056 -0.0430 0.3008 0.030 Uiso 1 1 calc R . . C8 C 0.3123(2) 0.02740(12) 0.21606(7) 0.0281(3) Uani 1 1 d . . . H8 H 0.1796 -0.0042 0.2004 0.034 Uiso 1 1 calc R . . C9 C 0.4327(2) 0.09160(12) 0.17874(6) 0.0280(3) Uani 1 1 d . . . C10 C 0.3694(3) 0.09927(14) 0.11086(7) 0.0378(4) Uani 1 1 d . . . H10A H 0.2298 0.0620 0.1024 0.057 Uiso 1 1 calc R . . H10B H 0.4800 0.0626 0.0875 0.057 Uiso 1 1 calc R . . H10C H 0.3574 0.1781 0.0988 0.057 Uiso 1 1 calc R . . C11 C 0.6200(2) 0.14740(11) 0.20431(6) 0.0259(3) Uani 1 1 d . . . C12 C 0.6726(2) 0.14337(11) 0.26884(6) 0.0228(3) Uani 1 1 d . . . C13 C 0.7663(2) 0.20226(12) 0.16589(7) 0.0311(4) Uani 1 1 d . . . H13 H 0.7321 0.2066 0.1231 0.037 Uiso 1 1 calc R . . C14 C 0.9522(2) 0.24792(12) 0.18938(7) 0.0325(4) Uani 1 1 d . . . H14 H 1.0591 0.2714 0.1626 0.039 Uiso 1 1 calc R . . C15 C 0.9904(2) 0.26147(12) 0.25389(7) 0.0282(3) Uani 1 1 d . . . C16 C 0.8398(2) 0.21902(11) 0.29400(6) 0.0241(3) Uani 1 1 d . . . C17 C 0.8545(2) 0.25948(11) 0.35683(6) 0.0250(3) Uani 1 1 d . . . C18 C 1.0395(2) 0.32272(12) 0.37791(7) 0.0290(4) Uani 1 1 d . . . C19 C 1.2021(2) 0.34975(12) 0.33668(8) 0.0351(4) Uani 1 1 d . . . H19 H 1.3305 0.3866 0.3515 0.042 Uiso 1 1 calc R . . C20 C 1.1751(2) 0.32350(12) 0.27677(8) 0.0338(4) Uani 1 1 d . . . H20 H 1.2804 0.3466 0.2494 0.041 Uiso 1 1 calc R . . C21 C 0.6834(2) 0.25045(12) 0.39711(6) 0.0259(3) Uani 1 1 d . . . H21 H 0.5544 0.2127 0.3836 0.031 Uiso 1 1 calc R . . C22 C 0.6994(2) 0.29478(12) 0.45494(7) 0.0307(4) Uani 1 1 d . . . H22 H 0.5810 0.2884 0.4805 0.037 Uiso 1 1 calc R . . C23 C 0.8889(3) 0.34950(12) 0.47679(7) 0.0360(4) Uani 1 1 d . . . H23 H 0.9020 0.3766 0.5177 0.043 Uiso 1 1 calc R . . C24 C 1.0541(3) 0.36342(12) 0.43873(8) 0.0357(4) Uani 1 1 d . . . H24 H 1.1816 0.4013 0.4534 0.043 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 N1 0.0299(6) 0.0262(7) 0.0248(7) 0.0009(5) 0.0045(5) -0.0033(5) C1 0.0382(9) 0.0264(8) 0.0253(8) 0.0001(7) 0.0052(7) -0.0034(7) C2 0.0443(9) 0.0258(8) 0.0236(8) 0.0004(6) -0.0037(7) 0.0028(7) C3 0.0303(8) 0.0262(8) 0.0301(8) -0.0045(7) -0.0040(7) 0.0027(6) C4 0.0267(7) 0.0209(7) 0.0274(8) -0.0021(6) 0.0019(6) -0.0005(6) C5 0.0259(7) 0.0185(7) 0.0235(7) -0.0032(6) 0.0024(6) -0.0017(6) C6 0.0218(7) 0.0209(7) 0.0237(7) -0.0021(6) 0.0035(6) 0.0031(6) C7 0.0233(7) 0.0226(8) 0.0293(8) -0.0018(6) 0.0038(6) 0.0006(6) C8 0.0263(7) 0.0250(8) 0.0323(8) -0.0050(7) -0.0042(6) 0.0022(6) C9 0.0329(8) 0.0252(8) 0.0256(8) -0.0032(6) -0.0016(6) 0.0082(6) C10 0.0489(10) 0.0365(9) 0.0273(9) -0.0014(7) -0.0044(7) 0.0075(8) C11 0.0303(8) 0.0213(7) 0.0263(8) 0.0009(6) 0.0046(6) 0.0055(6) C12 0.0222(7) 0.0211(7) 0.0254(8) -0.0004(6) 0.0032(6) 0.0046(6) C13 0.0405(9) 0.0280(8) 0.0254(8) 0.0047(7) 0.0070(7) 0.0070(7) C14 0.0354(8) 0.0265(8) 0.0371(9) 0.0083(7) 0.0155(7) 0.0054(7) C15 0.0249(7) 0.0219(8) 0.0382(9) 0.0071(7) 0.0067(6) 0.0040(6) C16 0.0216(7) 0.0208(7) 0.0301(8) 0.0047(6) 0.0029(6) 0.0028(6) C17 0.0252(7) 0.0180(7) 0.0313(8) 0.0029(6) -0.0025(6) 0.0013(6) C18 0.0273(8) 0.0203(7) 0.0383(9) 0.0050(7) -0.0067(7) 0.0006(6) C19 0.0236(7) 0.0243(8) 0.0565(11) 0.0081(8) -0.0063(8) -0.0030(6) C20 0.0248(8) 0.0251(8) 0.0522(11) 0.0124(7) 0.0082(7) 0.0004(6) C21 0.0274(7) 0.0208(7) 0.0291(8) 0.0020(6) -0.0016(6) -0.0002(6) C22 0.0386(9) 0.0239(8) 0.0291(8) 0.0015(7) -0.0007(7) 0.0029(7) C23 0.0485(10) 0.0271(9) 0.0309(9) -0.0015(7) -0.0103(8) 0.0011(7) C24 0.0356(9) 0.0239(8) 0.0457(10) 0.0018(7) -0.0163(8) -0.0020(7) _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 N1 C1 1.3397(17) . ? N1 C5 1.3509(17) . ? C1 C2 1.380(2) . ? C1 H1 0.9500 . ? C2 C3 1.383(2) . ? C2 H2 0.9500 . ? C3 C4 1.3767(19) . ? C3 H3 0.9500 . ? C4 C5 1.3970(18) . ? C4 H4 0.9500 . ? C5 C6 1.4903(18) . ? C6 C7 1.3836(18) . ? C6 C12 1.4309(19) . ? C7 C8 1.3991(18) . ? C7 H7 0.9500 . ? C8 C9 1.371(2) . ? C8 H8 0.9500 . ? C9 C11 1.4245(19) . ? C9 C10 1.5168(19) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.429(2) . ? C11 C12 1.4313(18) . ? C12 C16 1.4587(18) . ? C13 C14 1.349(2) . ? C13 H13 0.9500 . ? C14 C15 1.427(2) . ? C14 H14 0.9500 . ? C15 C16 1.4098(19) . ? C15 C20 1.430(2) . ? C16 C17 1.4546(19) . ? C17 C21 1.4191(19) . ? C17 C18 1.4268(19) . ? C18 C24 1.415(2) . ? C18 C19 1.425(2) . ? C19 C20 1.349(2) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.3698(19) . ? C21 H21 0.9500 . ? C22 C23 1.403(2) . ? C22 H22 0.9500 . ? C23 C24 1.364(2) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? 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 N1 C5 117.13(12) . . ? N1 C1 C2 124.51(14) . . ? N1 C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C1 C2 C3 117.96(13) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C4 C3 C2 118.97(13) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.70(14) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 121.74(12) . . ? N1 C5 C6 116.31(12) . . ? C4 C5 C6 121.54(12) . . ? C7 C6 C12 119.22(12) . . ? C7 C6 C5 116.20(12) . . ? C12 C6 C5 123.52(12) . . ? C6 C7 C8 121.64(13) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C9 C8 C7 120.53(13) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C11 119.08(13) . . ? C8 C9 C10 119.82(13) . . ? C11 C9 C10 121.06(14) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C13 120.85(13) . . ? C9 C11 C12 120.43(13) . . ? C13 C11 C12 118.60(13) . . ? C6 C12 C11 117.17(12) . . ? C6 C12 C16 124.82(12) . . ? C11 C12 C16 117.95(12) . . ? C14 C13 C11 121.12(14) . . ? C14 C13 H13 119.4 . . ? C11 C13 H13 119.4 . . ? C13 C14 C15 120.89(14) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 119.71(13) . . ? C16 C15 C20 120.84(14) . . ? C14 C15 C20 119.36(14) . . ? C15 C16 C17 117.34(13) . . ? C15 C16 C12 117.91(13) . . ? C17 C16 C12 124.63(12) . . ? C21 C17 C18 116.94(13) . . ? C21 C17 C16 123.46(12) . . ? C18 C17 C16 119.23(13) . . ? C24 C18 C19 120.45(14) . . ? C24 C18 C17 119.60(14) . . ? C19 C18 C17 119.86(14) . . ? C20 C19 C18 120.56(14) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C15 120.93(14) . . ? C19 C20 H20 119.5 . . ? C15 C20 H20 119.5 . . ? C22 C21 C17 121.70(13) . . ? C22 C21 H21 119.1 . . ? C17 C21 H21 119.1 . . ? C21 C22 C23 120.73(15) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 119.32(15) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C18 121.41(14) . . ? C23 C24 H24 119.3 . . ? C18 C24 H24 119.3 . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.176 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.043 #===END #-----------------------------------------------------------------------------80 # Data for compound 3a (local labelling montse17bbs) data_montse17bbs _database_code_depnum_ccdc_archive 'CCDC 859552' #TrackingRef 'web_deposit_cif_file_0_MontserratOlivan_1324462838.CC-helicenes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H61 N Os P2' _chemical_formula_weight 832.06 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' 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 tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 39.3354(14) _cell_length_b 39.3354(14) _cell_length_c 11.0574(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17108.8(13) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7449 _cell_measurement_theta_min 2 _cell_measurement_theta_max 21 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6816 _exptl_absorpt_coefficient_mu 3.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.597 _exptl_absorpt_correction_T_max 0.785 _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). ; _exptl_special_details ; ? ; _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 76515 _diffrn_reflns_av_R_equivalents 0.1003 _diffrn_reflns_av_sigmaI/netI 0.1148 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -52 _diffrn_reflns_limit_k_max 52 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28.67 _reflns_number_total 10436 _reflns_number_gt 4986 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2008.4-0, Bruker AXS' _computing_cell_refinement 'APEX2 v2008.4-0, Bruker AXS' _computing_data_reduction ; SAINT-Bruker integration program embedded in APEX2 v2008.4-0, Bruker AXS ; _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^)+(0.0549P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10436 _refine_ls_number_parameters 435 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 0.857 _refine_ls_restrained_S_all 0.869 _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 Os Os 0.156822(6) 0.148039(6) 0.01033(2) 0.04965(10) Uani 1 1 d D A . H01 H 0.1286(10) 0.1358(13) -0.084(4) 0.068(18) Uiso 1 1 d D . . H02 H 0.1703(12) 0.1193(9) -0.078(4) 0.050(16) Uiso 1 1 d D . . H03 H 0.1956(5) 0.1378(15) 0.027(6) 0.08(2) Uiso 1 1 d D . . P1 P 0.17829(5) 0.18385(5) -0.14088(19) 0.0673(6) Uani 1 1 d D . . P2 P 0.14016(5) 0.10057(4) 0.12313(19) 0.0621(5) Uani 1 1 d D . . N N 0.11514(11) 0.18216(10) 0.0509(4) 0.0345(11) Uani 1 1 d . . . C1 C 0.08661(15) 0.18451(14) -0.0146(5) 0.0424(14) Uani 1 1 d . A . H1 H 0.0819 0.1668 -0.0705 0.051 Uiso 1 1 calc R . . C2 C 0.06375(15) 0.21073(15) -0.0066(5) 0.0471(15) Uani 1 1 d . . . H2 H 0.0434 0.2107 -0.0530 0.056 Uiso 1 1 calc R A . C3 C 0.07141(14) 0.23779(15) 0.0730(5) 0.0409(14) Uani 1 1 d . A . H3 H 0.0572 0.2573 0.0771 0.049 Uiso 1 1 calc R . . C4 C 0.09979(13) 0.23517(14) 0.1438(5) 0.0352(13) Uani 1 1 d . . . H4 H 0.1054 0.2531 0.1979 0.042 Uiso 1 1 calc R A . C5 C 0.12072(13) 0.20649(14) 0.1376(5) 0.0356(13) Uani 1 1 d . A . C6 C 0.15187(13) 0.20142(13) 0.2082(5) 0.0359(13) Uani 1 1 d . . . C7 C 0.17455(14) 0.17791(14) 0.1565(6) 0.0443(15) Uani 1 1 d . A . C8 C 0.20823(14) 0.17868(15) 0.2051(5) 0.0447(15) Uani 1 1 d . . . H8 H 0.2239 0.1620 0.1775 0.054 Uiso 1 1 calc R A . C9 C 0.21942(14) 0.20155(15) 0.2880(5) 0.0407(14) Uani 1 1 d . A . C10 C 0.25588(13) 0.20237(15) 0.3253(6) 0.0500(16) Uani 1 1 d . . . H10A H 0.2683 0.1842 0.2836 0.075 Uiso 1 1 calc R A . H10B H 0.2575 0.1990 0.4129 0.075 Uiso 1 1 calc R . . H10C H 0.2658 0.2244 0.3038 0.075 Uiso 1 1 calc R . . C11 C 0.19563(13) 0.22407(13) 0.3420(5) 0.0365(13) Uani 1 1 d . . . C12 C 0.16034(13) 0.22105(13) 0.3129(5) 0.0353(13) Uani 1 1 d . A . C13 C 0.13674(13) 0.23847(14) 0.3920(5) 0.0360(13) Uani 1 1 d . . . C14 C 0.14804(14) 0.26660(14) 0.4615(5) 0.0385(14) Uani 1 1 d . A . C15 C 0.18365(14) 0.27256(15) 0.4722(5) 0.0465(16) Uani 1 1 d . . . H15 H 0.1917 0.2920 0.5144 0.056 Uiso 1 1 calc R A . C16 C 0.20609(14) 0.25045(15) 0.4219(5) 0.0441(15) Uani 1 1 d . A . H16 H 0.2296 0.2527 0.4408 0.053 Uiso 1 1 calc R . . C17 C 0.12430(15) 0.28774(16) 0.5209(5) 0.0464(15) Uani 1 1 d . . . H17 H 0.1322 0.3078 0.5598 0.056 Uiso 1 1 calc R A . C18 C 0.09082(15) 0.28044(17) 0.5242(5) 0.0477(16) Uani 1 1 d . A . H18 H 0.0753 0.2960 0.5595 0.057 Uiso 1 1 calc R . . C19 C 0.07891(14) 0.24954(17) 0.4748(5) 0.0447(15) Uani 1 1 d . . . C20 C 0.10179(14) 0.22736(15) 0.4125(5) 0.0410(14) Uani 1 1 d . A . C21 C 0.09032(14) 0.19448(16) 0.3791(5) 0.0447(15) Uani 1 1 d . . . H21 H 0.1056 0.1790 0.3418 0.054 Uiso 1 1 calc R A . C22 C 0.05693(15) 0.18468(18) 0.4004(5) 0.0546(18) Uani 1 1 d . A . H22 H 0.0496 0.1625 0.3787 0.065 Uiso 1 1 calc R . . C23 C 0.03396(16) 0.2074(2) 0.4539(6) 0.064(2) Uani 1 1 d . . . H23 H 0.0108 0.2012 0.4640 0.076 Uiso 1 1 calc R A . C24 C 0.04513(15) 0.2384(2) 0.4910(5) 0.0550(18) Uani 1 1 d . A . H24 H 0.0295 0.2532 0.5296 0.066 Uiso 1 1 calc R . . C25 C 0.1689(2) 0.23000(17) -0.1209(7) 0.073(2) Uani 1 1 d . A . H25 H 0.1459 0.2297 -0.0821 0.087 Uiso 1 1 calc R . . C26 C 0.1640(3) 0.2537(2) -0.2243(8) 0.110(3) Uani 1 1 d . . . H26A H 0.1578 0.2762 -0.1936 0.165 Uiso 1 1 calc R A . H26B H 0.1457 0.2452 -0.2765 0.165 Uiso 1 1 calc R . . H26C H 0.1851 0.2553 -0.2708 0.165 Uiso 1 1 calc R . . C27 C 0.19081(17) 0.24658(17) -0.0248(6) 0.0629(19) Uani 1 1 d . . . H27A H 0.2134 0.2513 -0.0582 0.094 Uiso 1 1 calc R A . H27B H 0.1929 0.2313 0.0447 0.094 Uiso 1 1 calc R . . H27C H 0.1803 0.2679 0.0012 0.094 Uiso 1 1 calc R . . C28A C 0.1686(3) 0.1726(3) -0.2947(8) 0.076(4) Uiso 0.60 1 d PD A 1 H28A H 0.1779 0.1908 -0.3486 0.091 Uiso 0.60 1 calc PR A 1 C29A C 0.1297(2) 0.1723(3) -0.3083(11) 0.066(3) Uiso 0.60 1 d PD A 1 H29A H 0.1238 0.1699 -0.3939 0.098 Uiso 0.60 1 calc PR A 1 H29B H 0.1204 0.1936 -0.2769 0.098 Uiso 0.60 1 calc PR A 1 H29C H 0.1203 0.1531 -0.2627 0.098 Uiso 0.60 1 calc PR A 1 C30A C 0.1839(3) 0.1389(4) -0.3338(16) 0.110(5) Uiso 0.60 1 d PD A 1 H30A H 0.1831 0.1228 -0.2663 0.165 Uiso 0.60 1 calc PR A 1 H30B H 0.2076 0.1424 -0.3584 0.165 Uiso 0.60 1 calc PR A 1 H30C H 0.1709 0.1298 -0.4021 0.165 Uiso 0.60 1 calc PR A 1 C28B C 0.1534(4) 0.1812(5) -0.2870(12) 0.085(7) Uiso 0.40 1 d PD A 2 H28B H 0.1629 0.2002 -0.3368 0.101 Uiso 0.40 1 calc PR A 2 C29B C 0.1143(4) 0.1876(5) -0.2908(18) 0.068(5) Uiso 0.40 1 d PD A 2 H29D H 0.1076 0.1940 -0.3730 0.102 Uiso 0.40 1 calc PR A 2 H29E H 0.1085 0.2060 -0.2348 0.102 Uiso 0.40 1 calc PR A 2 H29F H 0.1023 0.1668 -0.2669 0.102 Uiso 0.40 1 calc PR A 2 C30B C 0.1601(5) 0.1489(5) -0.366(2) 0.106(8) Uiso 0.40 1 d PD A 2 H30D H 0.1407 0.1451 -0.4199 0.159 Uiso 0.40 1 calc PR A 2 H30E H 0.1630 0.1291 -0.3130 0.159 Uiso 0.40 1 calc PR A 2 H30F H 0.1808 0.1522 -0.4139 0.159 Uiso 0.40 1 calc PR A 2 C31A C 0.2259(2) 0.1847(3) -0.1423(13) 0.077(4) Uiso 0.60 1 d PD A 1 H31A H 0.2314 0.1986 -0.0691 0.093 Uiso 0.60 1 calc PR A 1 C32A C 0.2432(4) 0.2047(3) -0.2454(13) 0.099(5) Uiso 0.60 1 d PD A 1 H32A H 0.2666 0.2103 -0.2220 0.148 Uiso 0.60 1 calc PR A 1 H32B H 0.2306 0.2258 -0.2608 0.148 Uiso 0.60 1 calc PR A 1 H32C H 0.2435 0.1908 -0.3190 0.148 Uiso 0.60 1 calc PR A 1 C33A C 0.2463(3) 0.1516(3) -0.1208(12) 0.087(4) Uiso 0.60 1 d PD A 1 H33A H 0.2389 0.1342 -0.1785 0.130 Uiso 0.60 1 calc PR A 1 H33B H 0.2423 0.1436 -0.0382 0.130 Uiso 0.60 1 calc PR A 1 H33C H 0.2706 0.1562 -0.1321 0.130 Uiso 0.60 1 calc PR A 1 C31B C 0.2186(3) 0.1753(5) -0.2154(14) 0.096(7) Uiso 0.40 1 d PD A 2 H31B H 0.2190 0.1509 -0.2407 0.115 Uiso 0.40 1 calc PR A 2 C32B C 0.2305(5) 0.1974(6) -0.3236(15) 0.105(8) Uiso 0.40 1 d PD A 2 H32D H 0.2273 0.2214 -0.3041 0.157 Uiso 0.40 1 calc PR A 2 H32E H 0.2170 0.1916 -0.3953 0.157 Uiso 0.40 1 calc PR A 2 H32F H 0.2546 0.1930 -0.3399 0.157 Uiso 0.40 1 calc PR A 2 C33B C 0.2431(5) 0.1798(5) -0.1099(13) 0.070(5) Uiso 0.40 1 d PD A 2 H33D H 0.2627 0.1647 -0.1206 0.105 Uiso 0.40 1 calc PR A 2 H33E H 0.2315 0.1742 -0.0342 0.105 Uiso 0.40 1 calc PR A 2 H33F H 0.2509 0.2034 -0.1071 0.105 Uiso 0.40 1 calc PR A 2 C34A C 0.1204(3) 0.1079(3) 0.2651(7) 0.071(3) Uiso 0.60 1 d PDU A 1 H34A H 0.1058 0.1286 0.2576 0.085 Uiso 0.60 1 calc PR A 1 C35A C 0.1501(2) 0.1163(3) 0.3536(11) 0.068(3) Uiso 0.60 1 d PDU A 1 H35A H 0.1408 0.1250 0.4297 0.103 Uiso 0.60 1 calc PR A 1 H35B H 0.1649 0.1335 0.3171 0.103 Uiso 0.60 1 calc PR A 1 H35C H 0.1633 0.0956 0.3695 0.103 Uiso 0.60 1 calc PR A 1 C36A C 0.0985(3) 0.0789(3) 0.3152(11) 0.069(3) Uiso 0.60 1 d PDU A 1 H36A H 0.1131 0.0598 0.3383 0.104 Uiso 0.60 1 calc PR A 1 H36B H 0.0824 0.0714 0.2530 0.104 Uiso 0.60 1 calc PR A 1 H36C H 0.0859 0.0869 0.3862 0.104 Uiso 0.60 1 calc PR A 1 C34B C 0.1482(4) 0.0997(5) 0.2905(8) 0.080(4) Uiso 0.40 1 d PDU A 2 H34B H 0.1429 0.1239 0.3104 0.097 Uiso 0.40 1 calc PR A 2 C35B C 0.1293(4) 0.0816(5) 0.3991(15) 0.082(4) Uiso 0.40 1 d PDU A 2 H35D H 0.1369 0.0915 0.4757 0.123 Uiso 0.40 1 calc PR A 2 H35E H 0.1345 0.0572 0.3981 0.123 Uiso 0.40 1 calc PR A 2 H35F H 0.1047 0.0848 0.3906 0.123 Uiso 0.40 1 calc PR A 2 C36B C 0.1863(3) 0.0993(4) 0.3223(16) 0.071(4) Uiso 0.40 1 d PDU A 2 H36D H 0.1892 0.1035 0.4091 0.106 Uiso 0.40 1 calc PR A 2 H36E H 0.1981 0.1170 0.2762 0.106 Uiso 0.40 1 calc PR A 2 H36F H 0.1960 0.0771 0.3019 0.106 Uiso 0.40 1 calc PR A 2 C37A C 0.1070(2) 0.0750(3) 0.0416(9) 0.065(3) Uiso 0.60 1 d PDU A 1 H37A H 0.1026 0.0546 0.0934 0.077 Uiso 0.60 1 calc PR A 1 C38A C 0.1140(3) 0.0611(3) -0.0870(10) 0.078(4) Uiso 0.60 1 d PDU A 1 H38A H 0.0931 0.0514 -0.1204 0.116 Uiso 0.60 1 calc PR A 1 H38B H 0.1316 0.0435 -0.0829 0.116 Uiso 0.60 1 calc PR A 1 H38C H 0.1219 0.0797 -0.1390 0.116 Uiso 0.60 1 calc PR A 1 C39A C 0.0726(4) 0.0950(6) 0.0363(14) 0.067(4) Uiso 0.60 1 d PDU A 1 H39A H 0.0740 0.1125 -0.0264 0.101 Uiso 0.60 1 calc PR A 1 H39B H 0.0683 0.1057 0.1148 0.101 Uiso 0.60 1 calc PR A 1 H39C H 0.0541 0.0793 0.0173 0.101 Uiso 0.60 1 calc PR A 1 C37B C 0.0933(2) 0.0961(4) 0.1536(13) 0.063(3) Uiso 0.40 1 d PDU A 2 H37B H 0.0904 0.0735 0.1939 0.076 Uiso 0.40 1 calc PR A 2 C38B C 0.0721(4) 0.1216(4) 0.2281(12) 0.057(4) Uiso 0.40 1 d PDU A 2 H38D H 0.0730 0.1440 0.1894 0.086 Uiso 0.40 1 calc PR A 2 H38E H 0.0814 0.1232 0.3101 0.086 Uiso 0.40 1 calc PR A 2 H38F H 0.0485 0.1139 0.2320 0.086 Uiso 0.40 1 calc PR A 2 C39B C 0.0766(6) 0.0926(9) 0.0254(17) 0.066(4) Uiso 0.40 1 d PDU A 2 H39D H 0.0518 0.0927 0.0335 0.100 Uiso 0.40 1 calc PR A 2 H39E H 0.0839 0.0712 -0.0119 0.100 Uiso 0.40 1 calc PR A 2 H39F H 0.0837 0.1117 -0.0256 0.100 Uiso 0.40 1 calc PR A 2 C40A C 0.1754(2) 0.0676(2) 0.1209(12) 0.088(3) Uiso 0.60 1 d PDU A 1 H40A H 0.1807 0.0628 0.0341 0.106 Uiso 0.60 1 calc PR A 1 C41A C 0.2088(3) 0.0800(3) 0.1800(11) 0.075(3) Uiso 0.60 1 d PDU A 1 H41A H 0.2056 0.0819 0.2677 0.112 Uiso 0.60 1 calc PR A 1 H41B H 0.2149 0.1023 0.1468 0.112 Uiso 0.60 1 calc PR A 1 H41C H 0.2270 0.0637 0.1631 0.112 Uiso 0.60 1 calc PR A 1 C42A C 0.1657(3) 0.0331(3) 0.1793(13) 0.095(4) Uiso 0.60 1 d PDU A 1 H42A H 0.1840 0.0166 0.1657 0.142 Uiso 0.60 1 calc PR A 1 H42B H 0.1446 0.0247 0.1428 0.142 Uiso 0.60 1 calc PR A 1 H42C H 0.1623 0.0362 0.2664 0.142 Uiso 0.60 1 calc PR A 1 C40B C 0.1508(5) 0.0577(3) 0.0753(16) 0.092(4) Uiso 0.40 1 d PDU A 2 H40B H 0.1761 0.0567 0.0654 0.110 Uiso 0.40 1 calc PR A 2 C41B C 0.1351(7) 0.0546(6) -0.0506(16) 0.129(6) Uiso 0.40 1 d PDU A 2 H41D H 0.1497 0.0406 -0.1019 0.194 Uiso 0.40 1 calc PR A 2 H41E H 0.1328 0.0773 -0.0865 0.194 Uiso 0.40 1 calc PR A 2 H41F H 0.1126 0.0440 -0.0441 0.194 Uiso 0.40 1 calc PR A 2 C42B C 0.1403(6) 0.0275(5) 0.1550(17) 0.096(5) Uiso 0.40 1 d PDU A 2 H42D H 0.1157 0.0281 0.1679 0.144 Uiso 0.40 1 calc PR A 2 H42E H 0.1520 0.0290 0.2331 0.144 Uiso 0.40 1 calc PR A 2 H42F H 0.1466 0.0062 0.1147 0.144 Uiso 0.40 1 calc PR A 2 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 0.04576(16) 0.04154(15) 0.06164(18) -0.01242(13) -0.00485(14) -0.00348(11) P1 0.0623(12) 0.0725(13) 0.0672(13) -0.0160(11) 0.0173(10) -0.0173(10) P2 0.0612(12) 0.0364(9) 0.0887(15) -0.0002(10) -0.0281(11) -0.0041(8) N 0.036(3) 0.030(2) 0.037(3) 0.006(2) -0.006(2) -0.005(2) C1 0.052(4) 0.040(3) 0.035(3) 0.005(3) -0.007(3) -0.012(3) C2 0.047(4) 0.048(4) 0.046(4) 0.012(3) -0.016(3) -0.006(3) C3 0.040(3) 0.046(4) 0.037(3) 0.010(3) 0.002(3) 0.001(3) C4 0.037(3) 0.040(3) 0.029(3) 0.005(3) -0.003(3) -0.005(3) C5 0.035(3) 0.041(3) 0.031(3) 0.004(3) 0.001(3) -0.010(3) C6 0.031(3) 0.034(3) 0.043(4) 0.001(3) 0.000(3) -0.004(2) C7 0.037(3) 0.039(3) 0.057(4) 0.004(3) -0.006(3) -0.006(3) C8 0.038(3) 0.047(4) 0.050(4) 0.001(3) 0.000(3) 0.006(3) C9 0.032(3) 0.046(3) 0.044(4) 0.001(3) -0.006(3) -0.004(3) C10 0.033(3) 0.058(4) 0.060(4) -0.001(3) -0.006(3) 0.004(3) C11 0.032(3) 0.038(3) 0.040(3) 0.005(3) -0.003(3) -0.003(3) C12 0.032(3) 0.033(3) 0.040(3) 0.003(3) -0.002(3) -0.002(2) C13 0.032(3) 0.049(3) 0.028(3) 0.011(3) -0.003(3) 0.002(3) C14 0.036(3) 0.048(4) 0.032(3) 0.002(3) -0.002(3) 0.002(3) C15 0.043(4) 0.048(4) 0.048(4) -0.008(3) -0.012(3) -0.007(3) C16 0.030(3) 0.059(4) 0.043(4) -0.002(3) -0.007(3) -0.002(3) C17 0.050(4) 0.056(4) 0.032(3) -0.001(3) -0.004(3) 0.001(3) C18 0.041(4) 0.068(4) 0.035(4) 0.005(3) 0.001(3) 0.014(3) C19 0.033(3) 0.077(5) 0.024(3) 0.014(3) -0.001(3) 0.005(3) C20 0.034(3) 0.059(4) 0.030(3) 0.016(3) -0.007(3) -0.007(3) C21 0.038(3) 0.061(4) 0.035(3) 0.011(3) -0.007(3) -0.006(3) C22 0.042(4) 0.083(5) 0.039(4) 0.023(4) -0.006(3) -0.023(4) C23 0.032(4) 0.120(7) 0.038(4) 0.027(4) 0.001(3) -0.017(4) C24 0.034(3) 0.099(6) 0.032(4) 0.008(4) -0.001(3) -0.002(3) C25 0.082(5) 0.067(5) 0.069(5) 0.014(4) -0.024(4) -0.022(4) C26 0.139(9) 0.121(8) 0.069(6) -0.002(6) -0.030(6) 0.005(7) C27 0.063(4) 0.059(4) 0.067(5) 0.007(4) -0.011(4) -0.012(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 Os C7 2.116(6) . ? Os N 2.166(4) . ? Os P2 2.3393(19) . ? Os P1 2.344(2) . ? Os H01 1.598(10) . ? Os H02 1.586(10) . ? Os H03 1.588(10) . ? P1 C28A 1.799(8) . ? P1 C31B 1.820(9) . ? P1 C25 1.866(7) . ? P1 C31A 1.871(8) . ? P1 C28B 1.892(9) . ? P2 C34A 1.775(8) . ? P2 C40B 1.815(9) . ? P2 C34B 1.878(9) . ? P2 C37A 1.878(7) . ? P2 C37B 1.881(8) . ? P2 C40A 1.900(8) . ? N C1 1.339(7) . ? N C5 1.372(6) . ? C1 C2 1.371(8) . ? C1 H1 0.9500 . ? C2 C3 1.413(8) . ? C2 H2 0.9500 . ? C3 C4 1.367(7) . ? C3 H3 0.9500 . ? C4 C5 1.398(7) . ? C4 H4 0.9500 . ? C5 C6 1.467(7) . ? C6 C7 1.407(7) . ? C6 C12 1.431(7) . ? C7 C8 1.430(7) . ? C8 C9 1.358(8) . ? C8 H8 0.9500 . ? C9 C11 1.420(7) . ? C9 C10 1.492(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.424(7) . ? C11 C12 1.430(7) . ? C12 C13 1.448(7) . ? C13 C14 1.419(7) . ? C13 C20 1.460(7) . ? C14 C17 1.412(8) . ? C14 C15 1.425(7) . ? C15 C16 1.358(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.348(8) . ? C17 H17 0.9500 . ? C18 C19 1.413(8) . ? C18 H18 0.9500 . ? C19 C24 1.411(8) . ? C19 C20 1.430(8) . ? C20 C21 1.419(8) . ? C21 C22 1.389(7) . ? C21 H21 0.9500 . ? C22 C23 1.402(9) . ? C22 H22 0.9500 . ? C23 C24 1.359(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.487(10) . ? C25 C27 1.516(8) . ? 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 . ? C28A C30A 1.517(9) . ? C28A C29A 1.536(9) . ? C28A H28A 1.0000 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C30A H30A 0.9800 . ? C30A H30B 0.9800 . ? C30A H30C 0.9800 . ? C28B C29B 1.559(9) . ? C28B C30B 1.563(9) . ? C28B H28B 1.0000 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? C31A C32A 1.545(9) . ? C31A C33A 1.548(9) . ? C31A H31A 1.0000 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C33A H33A 0.9800 . ? C33A H33B 0.9800 . ? C33A H33C 0.9800 . ? C31B C33B 1.522(10) . ? C31B C32B 1.550(9) . ? C31B H31B 1.0000 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C33B H33D 0.9800 . ? C33B H33E 0.9800 . ? C33B H33F 0.9800 . ? C34A C36A 1.535(8) . ? C34A C35A 1.559(8) . ? C34A H34A 1.0000 . ? C35A H35A 0.9800 . ? C35A H35B 0.9800 . ? C35A H35C 0.9800 . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C34B C36B 1.542(9) . ? C34B C35B 1.582(9) . ? C34B H34B 1.0000 . ? C35B H35D 0.9800 . ? C35B H35E 0.9800 . ? C35B H35F 0.9800 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 0.9800 . ? C37A C38A 1.547(8) . ? C37A C39A 1.565(9) . ? C37A H37A 1.0000 . ? C38A H38A 0.9800 . ? C38A H38B 0.9800 . ? C38A H38C 0.9800 . ? C39A H39A 0.9800 . ? C39A H39B 0.9800 . ? C39A H39C 0.9800 . ? C37B C38B 1.544(9) . ? C37B C39B 1.569(10) . ? C37B H37B 1.0000 . ? C38B H38D 0.9800 . ? C38B H38E 0.9800 . ? C38B H38F 0.9800 . ? C39B H39D 0.9800 . ? C39B H39E 0.9800 . ? C39B H39F 0.9800 . ? C40A C41A 1.547(9) . ? C40A C42A 1.548(9) . ? C40A H40A 1.0000 . ? C41A H41A 0.9800 . ? C41A H41B 0.9800 . ? C41A H41C 0.9800 . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C40B C41B 1.529(10) . ? C40B C42B 1.536(9) . ? C40B H40B 1.0000 . ? C41B H41D 0.9800 . ? C41B H41E 0.9800 . ? C41B H41F 0.9800 . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 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 N 75.36(19) . . ? C7 Os P2 97.37(16) . . ? N Os P2 99.91(12) . . ? C7 Os P1 95.30(16) . . ? N Os P1 92.75(12) . . ? P2 Os P1 163.97(7) . . ? C7 Os H01 153(2) . . ? N Os H01 78(2) . . ? P2 Os H01 85(2) . . ? P1 Os H01 88(2) . . ? C7 Os H02 139.1(18) . . ? N Os H02 145.4(18) . . ? P2 Os H02 81.5(18) . . ? P1 Os H02 82.5(18) . . ? H01 Os H02 67(2) . . ? C7 Os H03 75(2) . . ? N Os H03 149(2) . . ? P2 Os H03 90(2) . . ? P1 Os H03 84(2) . . ? H01 Os H03 132(3) . . ? H02 Os H03 64(3) . . ? C28A P1 C31B 73.2(6) . . ? C28A P1 C25 108.1(5) . . ? C31B P1 C25 114.0(7) . . ? C28A P1 C31A 102.1(6) . . ? C31B P1 C31A 29.3(6) . . ? C25 P1 C31A 100.5(5) . . ? C28A P1 C28B 21.5(5) . . ? C31B P1 C28B 93.1(8) . . ? C25 P1 C28B 93.0(6) . . ? C31A P1 C28B 120.8(7) . . ? C28A P1 Os 116.7(4) . . ? C31B P1 Os 121.7(6) . . ? C25 P1 Os 115.4(3) . . ? C31A P1 Os 112.2(4) . . ? C28B P1 Os 112.9(6) . . ? C34A P2 C40B 120.7(7) . . ? C34A P2 C34B 37.4(5) . . ? C40B P2 C34B 103.4(8) . . ? C34A P2 C37A 102.0(5) . . ? C40B P2 C37A 61.6(7) . . ? C34B P2 C37A 125.4(6) . . ? C34A P2 C37B 55.1(5) . . ? C40B P2 C37B 101.1(8) . . ? C34B P2 C37B 89.2(6) . . ? C37A P2 C37B 49.9(5) . . ? C34A P2 C40A 116.2(5) . . ? C40B P2 C40A 36.2(6) . . ? C34B P2 C40A 82.9(7) . . ? C37A P2 C40A 97.7(5) . . ? C37B P2 C40A 130.8(6) . . ? C34A P2 Os 117.6(4) . . ? C40B P2 Os 121.4(6) . . ? C34B P2 Os 119.5(6) . . ? C37A P2 Os 111.5(4) . . ? C37B P2 Os 116.4(5) . . ? C40A P2 Os 109.5(4) . . ? C1 N C5 117.7(5) . . ? C1 N Os 124.4(4) . . ? C5 N Os 117.1(3) . . ? N C1 C2 124.5(5) . . ? N C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C1 C2 C3 117.8(5) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C4 C3 C2 118.3(5) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 120.9(5) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? N C5 C4 120.2(5) . . ? N C5 C6 114.3(5) . . ? C4 C5 C6 125.1(5) . . ? C7 C6 C12 122.4(5) . . ? C7 C6 C5 113.7(5) . . ? C12 C6 C5 123.5(5) . . ? C6 C7 C8 114.9(5) . . ? C6 C7 Os 117.8(4) . . ? C8 C7 Os 127.2(4) . . ? C9 C8 C7 124.6(5) . . ? C9 C8 H8 117.7 . . ? C7 C8 H8 117.7 . . ? C8 C9 C11 118.9(5) . . ? C8 C9 C10 120.8(5) . . ? C11 C9 C10 120.2(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C16 121.7(5) . . ? C9 C11 C12 119.6(5) . . ? C16 C11 C12 118.7(5) . . ? C11 C12 C6 116.9(5) . . ? C11 C12 C13 116.6(5) . . ? C6 C12 C13 126.5(5) . . ? C14 C13 C12 119.7(5) . . ? C14 C13 C20 116.3(5) . . ? C12 C13 C20 123.8(5) . . ? C17 C14 C13 120.3(5) . . ? C17 C14 C15 121.0(5) . . ? C13 C14 C15 118.8(5) . . ? C16 C15 C14 120.0(5) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C11 122.2(5) . . ? C15 C16 H16 118.9 . . ? C11 C16 H16 118.9 . . ? C18 C17 C14 122.2(6) . . ? C18 C17 H17 118.9 . . ? C14 C17 H17 118.9 . . ? C17 C18 C19 119.8(6) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C24 C19 C18 122.1(6) . . ? C24 C19 C20 117.7(6) . . ? C18 C19 C20 120.1(5) . . ? C21 C20 C19 118.8(5) . . ? C21 C20 C13 122.1(6) . . ? C19 C20 C13 119.0(5) . . ? C22 C21 C20 120.6(6) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.3(6) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.4(6) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C19 123.0(7) . . ? C23 C24 H24 118.5 . . ? C19 C24 H24 118.5 . . ? C26 C25 C27 110.1(6) . . ? C26 C25 P1 123.0(6) . . ? C27 C25 P1 112.9(5) . . ? C26 C25 H25 102.7 . . ? C27 C25 H25 102.7 . . ? P1 C25 H25 102.7 . . ? 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 . . ? C30A C28A C29A 111.1(7) . . ? C30A C28A P1 113.6(9) . . ? C29A C28A P1 107.8(7) . . ? C30A C28A H28A 108.0 . . ? C29A C28A H28A 108.0 . . ? P1 C28A H28A 108.0 . . ? C29B C28B C30B 106.4(8) . . ? C29B C28B P1 121.7(12) . . ? C30B C28B P1 115.7(12) . . ? C29B C28B H28B 103.6 . . ? C30B C28B H28B 103.6 . . ? P1 C28B H28B 103.6 . . ? C28B C29B H29D 109.5 . . ? C28B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C28B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C28B C30B H30D 109.5 . . ? C28B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C28B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C32A C31A C33A 108.2(7) . . ? C32A C31A P1 117.2(9) . . ? C33A C31A P1 120.1(8) . . ? C32A C31A H31A 102.8 . . ? C33A C31A H31A 102.8 . . ? P1 C31A H31A 102.8 . . ? C33B C31B C32B 109.7(9) . . ? C33B C31B P1 100.5(11) . . ? C32B C31B P1 120.5(13) . . ? C33B C31B H31B 108.5 . . ? C32B C31B H31B 108.5 . . ? P1 C31B H31B 108.5 . . ? C31B C32B H32D 109.5 . . ? C31B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C31B C33B H33D 109.5 . . ? C31B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C31B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C36A C34A C35A 110.7(7) . . ? C36A C34A P2 116.4(7) . . ? C35A C34A P2 105.2(7) . . ? C36A C34A H34A 108.1 . . ? C35A C34A H34A 108.1 . . ? P2 C34A H34A 108.1 . . ? C36B C34B C35B 106.3(8) . . ? C36B C34B P2 112.9(10) . . ? C35B C34B P2 132.6(12) . . ? C36B C34B H34B 99.4 . . ? C35B C34B H34B 99.4 . . ? P2 C34B H34B 99.4 . . ? C34B C35B H35D 109.5 . . ? C34B C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C34B C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? C34B C36B H36D 109.5 . . ? C34B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C34B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C38A C37A C39A 107.3(7) . . ? C38A C37A P2 120.3(8) . . ? C39A C37A P2 110.4(9) . . ? C38A C37A H37A 106.0 . . ? C39A C37A H37A 106.0 . . ? P2 C37A H37A 106.0 . . ? C38B C37B C39B 108.2(8) . . ? C38B C37B P2 124.3(10) . . ? C39B C37B P2 104.9(12) . . ? C38B C37B H37B 106.1 . . ? C39B C37B H37B 106.1 . . ? P2 C37B H37B 106.1 . . ? C37B C38B H38D 109.5 . . ? C37B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C37B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? C37B C39B H39D 109.5 . . ? C37B C39B H39E 109.5 . . ? H39D C39B H39E 109.5 . . ? C37B C39B H39F 109.5 . . ? H39D C39B H39F 109.5 . . ? H39E C39B H39F 109.5 . . ? C41A C40A C42A 108.1(7) . . ? C41A C40A P2 113.4(8) . . ? C42A C40A P2 114.4(8) . . ? C41A C40A H40A 106.8 . . ? C42A C40A H40A 106.8 . . ? P2 C40A H40A 106.8 . . ? C41B C40B C42B 110.6(9) . . ? C41B C40B P2 104.2(13) . . ? C42B C40B P2 119.3(13) . . ? C41B C40B H40B 107.4 . . ? C42B C40B H40B 107.4 . . ? P2 C40B H40B 107.4 . . ? C40B C41B H41D 109.5 . . ? C40B C41B H41E 109.5 . . ? H41D C41B H41E 109.5 . . ? C40B C41B H41F 109.5 . . ? H41D C41B H41F 109.5 . . ? H41E C41B H41F 109.5 . . ? C40B C42B H42D 109.5 . . ? C40B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C40B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.852 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.117 #===END