#-----------------------------------------------------------------------------80 # Subsequently are contained the CIF's of two structures # 1 = compound (2) # 2 = compound (4) # separated by #===END #-----------------------------------------------------------------------------80 data_global _publ_contact_author ; Dr. Enrique O\~nate Rodr\'iguez Departamento de Qu\'imica Inorg\'anica - I.S.Q.C.H. 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 'Esteruelas, M. A.' 'Larramona, C.' 'O\~nate, E.' _publ_requested_journal 'Organometallics' _journal_name_full ; Organometallics ; _publ_section_title ; Osmium_mediated Direct C-H Bond Activation at 8-position of Quinolines ; _publ_contact_letter ; march ##, 2016 Please consider this CIF submission as supplementary material of the structures contained in the paper: Osmium_mediated Direct C-H Bond Activation at 8-position of Quinolines that is submitted to Organometallics for publication. ; _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? # --------------------------------------------------------------------- # Data for compound 2 (local labelling as enrique194) data_enrique194 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H51 N Os P2' _chemical_formula_weight 641.83 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 'monoclinic' _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0424(4) _cell_length_b 16.1531(7) _cell_length_c 19.6745(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.3040(10) _cell_angle_gamma 90.00 _cell_volume 2818.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9998 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 29 _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 4.653 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.727 _exptl_absorpt_correction_T_max 0.862 _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. 7.56a (2008). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_reflns_number 33494 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.61 _reflns_number_total 6778 _reflns_number_gt 6056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'apex2 v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+ v. 7.56a (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ v. 7.56a (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.14 (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^)+(0.0292P)^2^+5.1615P] 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 6778 _refine_ls_number_parameters 320 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0608 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os Os 0.850929(13) 0.290269(7) 0.059187(6) 0.01339(4) Uani 1 1 d D A . H01 H 0.689(2) 0.274(2) 0.0757(18) 0.016 Uiso 1 1 d D . . H02 H 0.713(3) 0.3428(18) 0.0197(16) 0.016 Uiso 1 1 d D . . H03 H 0.891(4) 0.3568(16) 0.0059(14) 0.016 Uiso 1 1 d D . . P1 P 0.78923(9) 0.19707(5) -0.03276(4) 0.01518(16) Uani 1 1 d . . . P2 P 0.86508(9) 0.39408(5) 0.14308(4) 0.01548(16) Uani 1 1 d . . . N1 N 1.0989(7) 0.2651(7) 0.0762(5) 0.0114(17) Uani 0.70 1 d PDU . . C8B C 1.0863(15) 0.260(2) 0.0868(14) 0.011(5) Uani 0.30 1 d PDU . . C1 C 1.2317(4) 0.2818(2) 0.06655(17) 0.0202(7) Uani 1 1 d . A . H1 H 1.2418 0.3242 0.0343 0.024 Uiso 1 1 d R . . C2 C 1.3618(4) 0.2395(2) 0.10107(18) 0.0228(7) Uani 1 1 d . . . H2 H 1.4575 0.2537 0.0913 0.027 Uiso 1 1 calc R A . C3 C 1.3525(4) 0.1785(2) 0.14825(18) 0.0226(7) Uani 1 1 d . A . H3 H 1.4408 0.1507 0.1714 0.027 Uiso 1 1 calc R . . C4 C 1.2092(4) 0.1572(2) 0.16218(17) 0.0189(6) Uani 1 1 d . . . C5 C 1.1765(4) 0.0953(2) 0.20826(18) 0.0227(7) Uani 1 1 d . A . H5 H 1.2551 0.0624 0.2340 0.027 Uiso 1 1 calc R . . C6 C 1.0305(4) 0.0837(2) 0.21514(17) 0.0221(7) Uani 1 1 d . . . H6 H 1.0088 0.0413 0.2452 0.027 Uiso 1 1 calc R A . C7 C 0.9097(4) 0.1329(2) 0.17903(16) 0.0193(6) Uani 1 1 d . A . H7 H 0.8105 0.1236 0.1867 0.023 Uiso 1 1 d R . . C8 C 0.9275(16) 0.1950(9) 0.1337(8) 0.013(2) Uani 0.70 1 d PDU . . N1B N 0.949(3) 0.1906(17) 0.1335(16) 0.015(6) Uani 0.30 1 d PDU . . C9 C 1.0854(4) 0.20237(18) 0.12656(16) 0.0156(6) Uani 1 1 d . A . C10 C 0.9257(4) 0.1838(2) -0.09222(18) 0.0214(7) Uani 1 1 d . . . H10 H 0.8695 0.1598 -0.1367 0.026 Uiso 1 1 calc R . . C11 C 0.9936(4) 0.2667(2) -0.10899(19) 0.0274(8) Uani 1 1 d . . . H11A H 1.0574 0.2890 -0.0669 0.041 Uiso 1 1 calc R . . H11B H 0.9123 0.3059 -0.1263 0.041 Uiso 1 1 calc R . . H11C H 1.0546 0.2581 -0.1444 0.041 Uiso 1 1 calc R . . C12 C 1.0556(4) 0.1245(2) -0.0628(2) 0.0299(8) Uani 1 1 d . . . H12A H 1.1260 0.1215 -0.0948 0.045 Uiso 1 1 calc R . . H12B H 1.0148 0.0692 -0.0572 0.045 Uiso 1 1 calc R . . H12C H 1.1087 0.1449 -0.0177 0.045 Uiso 1 1 calc R . . C13 C 0.7626(4) 0.0875(2) -0.00712(18) 0.0213(7) Uani 1 1 d . . . H13 H 0.8626 0.0693 0.0200 0.026 Uiso 1 1 calc R . . C14 C 0.6513(4) 0.0781(2) 0.04185(19) 0.0257(7) Uani 1 1 d . . . H14A H 0.5482 0.0758 0.0147 0.039 Uiso 1 1 calc R . . H14B H 0.6610 0.1255 0.0735 0.039 Uiso 1 1 calc R . . H14C H 0.6734 0.0269 0.0687 0.039 Uiso 1 1 calc R . . C15 C 0.7223(5) 0.0257(2) -0.06737(19) 0.0288(8) Uani 1 1 d . . . H15A H 0.7278 -0.0309 -0.0490 0.043 Uiso 1 1 calc R . . H15B H 0.7937 0.0317 -0.0986 0.043 Uiso 1 1 calc R . . H15C H 0.6198 0.0368 -0.0929 0.043 Uiso 1 1 calc R . . C16 C 0.6105(4) 0.2183(2) -0.09666(17) 0.0192(6) Uani 1 1 d . . . H16 H 0.5882 0.1678 -0.1264 0.023 Uiso 1 1 calc R . . C17 C 0.4749(4) 0.2325(2) -0.06249(19) 0.0266(8) Uani 1 1 d . . . H17A H 0.4907 0.2829 -0.0343 0.040 Uiso 1 1 calc R . . H17B H 0.4633 0.1851 -0.0329 0.040 Uiso 1 1 calc R . . H17C H 0.3837 0.2386 -0.0984 0.040 Uiso 1 1 calc R . . C18 C 0.6226(4) 0.2909(2) -0.14512(19) 0.0293(8) Uani 1 1 d . . . H18A H 0.5236 0.3018 -0.1742 0.044 Uiso 1 1 calc R . . H18B H 0.6949 0.2772 -0.1746 0.044 Uiso 1 1 calc R . . H18C H 0.6572 0.3402 -0.1176 0.044 Uiso 1 1 calc R . . C19A C 0.7343(8) 0.4823(5) 0.1094(5) 0.0209(19) Uiso 0.50 1 d PD A 1 H19A H 0.7489 0.4916 0.0609 0.025 Uiso 0.50 1 calc PR A 1 C20A C 0.5691(10) 0.4554(7) 0.1018(6) 0.032(3) Uiso 0.50 1 d PD A 1 H20A H 0.5450 0.4479 0.1479 0.048 Uiso 0.50 1 calc PR A 1 H20B H 0.5534 0.4031 0.0762 0.048 Uiso 0.50 1 calc PR A 1 H20C H 0.5033 0.4981 0.0766 0.048 Uiso 0.50 1 calc PR A 1 C21A C 0.7622(10) 0.5660(5) 0.1444(4) 0.0389(19) Uiso 0.50 1 d PD A 1 H21A H 0.6926 0.6068 0.1188 0.058 Uiso 0.50 1 calc PR A 1 H21B H 0.8663 0.5833 0.1449 0.058 Uiso 0.50 1 calc PR A 1 H21C H 0.7459 0.5620 0.1921 0.058 Uiso 0.50 1 calc PR A 1 C19B C 0.7216(8) 0.4788(4) 0.1265(4) 0.0171(18) Uiso 0.50 1 d PD A 2 H19B H 0.7393 0.5154 0.1683 0.021 Uiso 0.50 1 calc PR A 2 C20B C 0.5588(8) 0.4485(6) 0.1161(5) 0.020(2) Uiso 0.50 1 d PD A 2 H20D H 0.4903 0.4960 0.1085 0.030 Uiso 0.50 1 calc PR A 2 H20E H 0.5441 0.4182 0.1574 0.030 Uiso 0.50 1 calc PR A 2 H20F H 0.5376 0.4117 0.0757 0.030 Uiso 0.50 1 calc PR A 2 C21B C 0.7407(8) 0.5331(4) 0.0640(3) 0.0228(14) Uiso 0.50 1 d PD A 2 H21D H 0.7476 0.4975 0.0245 0.034 Uiso 0.50 1 calc PR A 2 H21E H 0.8329 0.5662 0.0764 0.034 Uiso 0.50 1 calc PR A 2 H21F H 0.6535 0.5700 0.0517 0.034 Uiso 0.50 1 calc PR A 2 C22 C 0.8379(4) 0.3588(2) 0.23045(17) 0.0202(7) Uani 1 1 d . A . H22 H 0.9288 0.3246 0.2492 0.024 Uiso 1 1 calc R . . C23 C 0.7033(4) 0.3010(2) 0.2293(2) 0.0295(8) Uani 1 1 d . . . H23A H 0.7194 0.2682 0.2720 0.044 Uiso 1 1 calc R A . H23B H 0.6934 0.2639 0.1892 0.044 Uiso 1 1 calc R . . H23C H 0.6111 0.3339 0.2258 0.044 Uiso 1 1 calc R . . C24 C 0.8366(4) 0.4274(2) 0.28424(18) 0.0260(7) Uani 1 1 d . . . H24A H 0.7427 0.4591 0.2722 0.039 Uiso 1 1 calc R A . H24B H 0.9227 0.4644 0.2847 0.039 Uiso 1 1 calc R . . H24C H 0.8436 0.4025 0.3302 0.039 Uiso 1 1 calc R . . C25 C 1.0467(4) 0.4522(2) 0.16818(17) 0.0201(6) Uani 1 1 d . A . H25 H 1.0267 0.5020 0.1953 0.024 Uiso 1 1 calc R . . C26 C 1.1693(4) 0.4002(2) 0.21496(19) 0.0243(7) Uani 1 1 d . . . H26A H 1.1728 0.3449 0.1949 0.037 Uiso 1 1 calc R A . H26B H 1.1453 0.3954 0.2613 0.037 Uiso 1 1 calc R . . H26C H 1.2675 0.4272 0.2184 0.037 Uiso 1 1 calc R . . C27 C 1.1051(4) 0.4829(2) 0.10435(19) 0.0264(8) Uani 1 1 d . . . H27A H 1.2004 0.5125 0.1194 0.040 Uiso 1 1 calc R A . H27B H 1.0306 0.5202 0.0772 0.040 Uiso 1 1 calc R . . H27C H 1.1214 0.4354 0.0757 0.040 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 0.01389(6) 0.01209(6) 0.01401(7) 0.00032(4) 0.00233(4) -0.00068(4) P1 0.0166(4) 0.0140(4) 0.0146(4) -0.0007(3) 0.0021(3) -0.0005(3) P2 0.0165(4) 0.0125(4) 0.0168(4) -0.0012(3) 0.0020(3) -0.0003(3) N1 0.014(2) 0.013(3) 0.009(3) 0.004(2) 0.007(2) 0.000(2) C8B 0.013(6) 0.012(6) 0.010(6) -0.005(4) 0.010(4) -0.007(4) C1 0.0209(16) 0.0192(16) 0.0210(16) -0.0011(12) 0.0056(13) -0.0022(13) C2 0.0156(15) 0.0257(17) 0.0278(18) -0.0062(14) 0.0060(13) -0.0022(13) C3 0.0152(15) 0.0259(17) 0.0249(17) -0.0029(14) -0.0005(13) 0.0047(13) C4 0.0175(15) 0.0175(15) 0.0209(16) -0.0056(12) 0.0022(12) 0.0015(12) C5 0.0277(18) 0.0171(16) 0.0208(17) 0.0020(13) -0.0012(14) 0.0053(13) C6 0.0315(18) 0.0160(15) 0.0187(16) 0.0012(12) 0.0048(14) -0.0012(13) C7 0.0207(16) 0.0174(15) 0.0200(16) 0.0023(12) 0.0045(13) -0.0008(12) C8 0.008(3) 0.014(3) 0.016(4) -0.001(2) 0.000(2) 0.000(2) N1B 0.016(8) 0.013(7) 0.014(7) -0.006(4) -0.001(4) 0.003(4) C9 0.0166(15) 0.0129(14) 0.0172(15) -0.0016(11) 0.0026(12) -0.0002(11) C10 0.0228(16) 0.0230(17) 0.0201(16) -0.0042(13) 0.0085(13) -0.0005(13) C11 0.0305(19) 0.032(2) 0.0228(18) -0.0014(15) 0.0138(15) -0.0039(15) C12 0.0255(18) 0.031(2) 0.033(2) -0.0063(16) 0.0066(15) 0.0049(15) C13 0.0280(17) 0.0135(15) 0.0215(16) 0.0022(12) 0.0028(14) 0.0005(13) C14 0.0286(18) 0.0206(17) 0.0259(18) 0.0032(14) 0.0006(15) -0.0098(14) C15 0.042(2) 0.0166(17) 0.0263(18) -0.0003(14) 0.0036(16) -0.0012(15) C16 0.0188(15) 0.0205(16) 0.0162(15) -0.0045(12) -0.0015(12) -0.0007(12) C17 0.0180(16) 0.0306(19) 0.0282(19) 0.0005(15) -0.0024(14) 0.0012(14) C18 0.032(2) 0.030(2) 0.0239(18) 0.0068(15) 0.0002(15) 0.0001(16) C22 0.0214(16) 0.0228(17) 0.0165(15) -0.0017(13) 0.0040(12) -0.0010(13) C23 0.0259(18) 0.035(2) 0.0293(19) -0.0008(16) 0.0107(15) -0.0062(15) C24 0.0308(19) 0.0282(19) 0.0201(17) -0.0046(14) 0.0073(14) 0.0040(15) C25 0.0209(16) 0.0156(15) 0.0234(16) -0.0036(13) 0.0032(13) -0.0047(12) C26 0.0239(17) 0.0206(17) 0.0261(18) -0.0040(13) -0.0010(14) -0.0026(13) C27 0.0239(17) 0.0215(17) 0.035(2) -0.0002(15) 0.0087(15) -0.0059(14) _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 C8 2.145(8) . ? Os N1B 2.237(10) . ? Os N1 2.238(6) . ? Os C8B 2.146(11) . ? Os P1 2.3355(8) . ? Os P2 2.3387(8) . ? Os H01 1.585(10) . ? Os H02 1.580(10) . ? Os H03 1.591(10) . ? P1 C13 1.869(3) . ? P1 C10 1.871(3) . ? P1 C16 1.874(3) . ? P2 C19B 1.870(7) . ? P2 C25 1.872(3) . ? P2 C22 1.872(3) . ? P2 C19A 1.887(8) . ? N1 C1 1.281(9) . ? N1 C9 1.439(10) . ? C8B C9 1.22(3) . ? C8B C1 1.49(2) . ? C1 C2 1.414(5) . ? C1 H1 0.9500 . ? C2 C3 1.368(5) . ? C2 H2 0.9500 . ? C3 C4 1.418(5) . ? C3 H3 0.9500 . ? C4 C9 1.404(4) . ? C4 C5 1.419(5) . ? C5 C6 1.367(5) . ? C5 H5 0.9500 . ? C6 C7 1.423(5) . ? C6 H6 0.9500 . ? C7 C8 1.373(10) . ? C7 N1B 1.39(2) . ? C7 H7 0.9500 . ? C8 C9 1.467(15) . ? N1B C9 1.28(3) . ? C10 C11 1.535(5) . ? C10 C12 1.539(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.531(5) . ? C13 C15 1.538(5) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.527(5) . ? C16 C18 1.529(5) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19A C21A 1.516(8) . ? C19A C20A 1.535(8) . ? C19A H19A 1.0000 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C19B C20B 1.527(7) . ? C19B C21B 1.546(7) . ? C19B H19B 1.0000 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22 C23 1.530(5) . ? C22 C24 1.533(5) . ? 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 C27 1.536(5) . ? C25 C26 1.544(5) . ? 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 . ? 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 C8 Os N1B 4.9(12) . . ? C8 Os N1 65.7(5) . . ? N1B Os N1 61.0(8) . . ? C8 Os C8B 59.6(9) . . ? N1B Os C8B 55.0(11) . . ? N1 Os C8B 6.6(10) . . ? C8 Os P1 93.6(5) . . ? N1B Os P1 92.6(10) . . ? N1 Os P1 94.6(3) . . ? C8B Os P1 97.2(8) . . ? C8 Os P2 93.8(5) . . ? N1B Os P2 95.5(10) . . ? N1 Os P2 96.3(3) . . ? C8B Os P2 94.0(8) . . ? P1 Os P2 168.68(3) . . ? C8 Os H01 86.0(13) . . ? N1B Os H01 90.7(15) . . ? N1 Os H01 151.7(13) . . ? C8B Os H01 145.4(15) . . ? P1 Os H01 87.9(13) . . ? P2 Os H01 84.1(13) . . ? C8 Os H02 147.1(13) . . ? N1B Os H02 151.7(15) . . ? N1 Os H02 147.3(13) . . ? C8B Os H02 153.3(15) . . ? P1 Os H02 85.4(13) . . ? P2 Os H02 83.7(13) . . ? H01 Os H02 61.0(17) . . ? C8 Os H03 148.3(13) . . ? N1B Os H03 143.6(15) . . ? N1 Os H03 82.6(13) . . ? C8B Os H03 88.7(15) . . ? P1 Os H03 88.6(12) . . ? P2 Os H03 89.6(12) . . ? H01 Os H03 125.7(18) . . ? H02 Os H03 64.6(17) . . ? C13 P1 C10 101.32(16) . . ? C13 P1 C16 102.38(15) . . ? C10 P1 C16 100.89(15) . . ? C13 P1 Os 115.16(11) . . ? C10 P1 Os 118.11(11) . . ? C16 P1 Os 116.45(11) . . ? C19B P2 C25 102.8(2) . . ? C19B P2 C22 99.9(3) . . ? C25 P2 C22 100.18(15) . . ? C19B P2 C19A 11.6(3) . . ? C25 P2 C19A 99.8(2) . . ? C22 P2 C19A 111.5(3) . . ? C19B P2 Os 117.5(2) . . ? C25 P2 Os 118.02(11) . . ? C22 P2 Os 115.53(11) . . ? C19A P2 Os 110.5(2) . . ? C1 N1 C9 117.3(5) . . ? C1 N1 Os 151.7(7) . . ? C9 N1 Os 90.8(4) . . ? C9 C8B C1 118.0(11) . . ? C9 C8B Os 101.8(13) . . ? C1 C8B Os 139.8(17) . . ? N1 C1 C8B 7.0(12) . . ? N1 C1 C2 122.9(5) . . ? C8B C1 C2 117.0(10) . . ? N1 C1 H1 117.8 . . ? C8B C1 H1 123.6 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 121.2(3) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C9 C4 C3 116.6(3) . . ? C9 C4 C5 116.1(3) . . ? C3 C4 C5 127.4(3) . . ? C6 C5 C4 119.1(3) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 122.5(3) . . ? C5 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C8 C7 C6 123.8(7) . . ? C8 C7 N1B 8.6(16) . . ? C6 C7 N1B 115.4(10) . . ? C8 C7 H7 116.9 . . ? C6 C7 H7 119.3 . . ? N1B C7 H7 125.3 . . ? C7 C8 C9 111.2(8) . . ? C7 C8 Os 154.9(10) . . ? C9 C8 Os 93.8(5) . . ? C9 N1B C7 122.8(11) . . ? C9 N1B Os 95.2(10) . . ? C7 N1B Os 141.9(17) . . ? C8B C9 N1B 108.0(6) . . ? C8B C9 C4 127.8(7) . . ? N1B C9 C4 124.1(5) . . ? C8B C9 N1 6.7(13) . . ? N1B C9 N1 113.0(7) . . ? C4 C9 N1 122.9(4) . . ? C8B C9 C8 104.6(9) . . ? N1B C9 C8 3.9(14) . . ? C4 C9 C8 127.3(4) . . ? N1 C9 C8 109.8(3) . . ? C11 C10 C12 108.4(3) . . ? C11 C10 P1 112.0(2) . . ? C12 C10 P1 112.6(2) . . ? C11 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? P1 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 109.6(3) . . ? C14 C13 P1 113.5(2) . . ? C15 C13 P1 115.5(2) . . ? C14 C13 H13 105.8 . . ? C15 C13 H13 105.8 . . ? P1 C13 H13 105.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C18 108.7(3) . . ? C17 C16 P1 113.2(2) . . ? C18 C16 P1 113.6(2) . . ? C17 C16 H16 107.0 . . ? C18 C16 H16 107.0 . . ? P1 C16 H16 107.0 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21A C19A C20A 111.6(7) . . ? C21A C19A P2 118.5(6) . . ? C20A C19A P2 110.6(6) . . ? C21A C19A H19A 104.9 . . ? C20A C19A H19A 104.9 . . ? P2 C19A H19A 104.9 . . ? C20B C19B C21B 109.3(6) . . ? C20B C19B P2 114.0(5) . . ? C21B C19B P2 111.9(5) . . ? C20B C19B H19B 107.1 . . ? C21B C19B H19B 107.1 . . ? P2 C19B H19B 107.1 . . ? C19B C20B H20D 109.5 . . ? C19B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C19B C21B H21D 109.5 . . ? C19B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C19B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C23 C22 C24 109.7(3) . . ? C23 C22 P2 114.8(2) . . ? C24 C22 P2 115.7(2) . . ? C23 C22 H22 105.2 . . ? C24 C22 H22 105.2 . . ? P2 C22 H22 105.2 . . ? 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 . . ? C27 C25 C26 109.9(3) . . ? C27 C25 P2 111.7(2) . . ? C26 C25 P2 112.0(2) . . ? C27 C25 H25 107.7 . . ? C26 C25 H25 107.7 . . ? P2 C25 H25 107.7 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.918 _refine_diff_density_min -1.124 _refine_diff_density_rms 0.108 #===END # --------------------------------------------------------------------- # Data for compound 4 (local labelling as enriquen61) data_enriquen61 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H53 N Os P2' _chemical_formula_weight 655.85 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 'triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9257(14) _cell_length_b 16.717(3) _cell_length_c 20.972(3) _cell_angle_alpha 107.975(2) _cell_angle_beta 91.234(3) _cell_angle_gamma 95.736(2) _cell_volume 2957.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6014 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27 _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 4.436 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.862 _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. 7.56a (2008). ; _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 APEX DUO CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_reflns_number 32602 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0839 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 29.58 _reflns_number_total 14963 _reflns_number_gt 10334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'apex2 v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+ v. 7.56a (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ v. 7.56a (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.14 (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^)+(0.0102P)^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 14963 _refine_ls_number_parameters 623 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 0.77204(2) 0.707837(12) 0.028896(10) 0.01820(5) Uani 1 1 d D . . H01 H 0.921(2) 0.663(2) 0.018(2) 0.022 Uiso 1 1 d D . . H02 H 0.774(4) 0.6112(9) -0.0110(18) 0.022 Uiso 1 1 d D . . H03 H 0.617(2) 0.658(2) -0.0078(18) 0.022 Uiso 1 1 d D . . Os2 Os 0.66832(2) 0.275408(12) 0.466187(9) 0.01718(5) Uani 1 1 d D . . H04 H 0.542(3) 0.3367(19) 0.4910(19) 0.021 Uiso 1 1 d D . . H05 H 0.700(4) 0.3667(12) 0.5196(16) 0.021 Uiso 1 1 d D . . H06 H 0.8332(19) 0.301(2) 0.5003(18) 0.021 Uiso 1 1 d D . . P1 P 0.71191(14) 0.65675(9) 0.11841(7) 0.0212(3) Uani 1 1 d . . . P2 P 0.83614(13) 0.72609(8) -0.07354(6) 0.0191(3) Uani 1 1 d . . . P3 P 0.60256(14) 0.23001(8) 0.55719(7) 0.0204(3) Uani 1 1 d . . . P4 P 0.73731(13) 0.34691(8) 0.38946(6) 0.0177(3) Uani 1 1 d . . . N1 N 0.6581(4) 0.8251(2) 0.06001(19) 0.0210(9) Uani 1 1 d . . . N2 N 0.7288(4) 0.1491(2) 0.40472(19) 0.0201(9) Uani 1 1 d . . . C1 C 0.5385(6) 0.8651(3) 0.0565(3) 0.0305(13) Uani 1 1 d . . . H1 H 0.4517 0.8332 0.0304 0.037 Uiso 1 1 calc R . . C2 C 0.5325(6) 0.9510(4) 0.0887(3) 0.0341(14) Uani 1 1 d . . . C3 C 0.3923(6) 0.9908(4) 0.0797(3) 0.0470(17) Uani 1 1 d . . . H3A H 0.3915 1.0445 0.1158 0.071 Uiso 1 1 calc R . . H3B H 0.3029 0.9524 0.0812 0.071 Uiso 1 1 calc R . . H3C H 0.3915 1.0013 0.0362 0.071 Uiso 1 1 calc R . . C4 C 0.6571(6) 0.9976(4) 0.1262(3) 0.0377(14) Uani 1 1 d . . . H4 H 0.6548 1.0562 0.1488 0.045 Uiso 1 1 calc R . . C5 C 0.7895(6) 0.9595(3) 0.1317(3) 0.0279(12) Uani 1 1 d . . . C6 C 0.7815(6) 0.8719(3) 0.0969(2) 0.0243(11) Uani 1 1 d . . . C7 C 0.8980(6) 0.8207(3) 0.0925(2) 0.0260(12) Uani 1 1 d . . . C8 C 1.0330(6) 0.8623(4) 0.1279(3) 0.0335(13) Uani 1 1 d . . . H8 H 1.1174 0.8317 0.1274 0.040 Uiso 1 1 calc R . . C9 C 1.0443(6) 0.9491(4) 0.1642(3) 0.0399(15) Uani 1 1 d . . . H9 H 1.1367 0.9756 0.1882 0.048 Uiso 1 1 calc R . . C10 C 0.9263(6) 0.9973(4) 0.1662(3) 0.0350(14) Uani 1 1 d . . . H10 H 0.9384 1.0559 0.1910 0.042 Uiso 1 1 calc R . . C11 C 0.7094(6) 0.5391(3) 0.0956(3) 0.0281(12) Uani 1 1 d . . . H11 H 0.6219 0.5150 0.0624 0.034 Uiso 1 1 calc R . . C12 C 0.6806(7) 0.5007(4) 0.1523(3) 0.0447(16) Uani 1 1 d . . . H12A H 0.6599 0.4390 0.1334 0.067 Uiso 1 1 calc R . . H12B H 0.5938 0.5235 0.1765 0.067 Uiso 1 1 calc R . . H12C H 0.7699 0.5149 0.1834 0.067 Uiso 1 1 calc R . . C13 C 0.8477(6) 0.5028(4) 0.0595(3) 0.0464(17) Uani 1 1 d . . . H13A H 0.9379 0.5232 0.0899 0.070 Uiso 1 1 calc R . . H13B H 0.8612 0.5212 0.0197 0.070 Uiso 1 1 calc R . . H13C H 0.8321 0.4408 0.0457 0.070 Uiso 1 1 calc R . . C14 C 0.5194(5) 0.6700(4) 0.1511(3) 0.0320(13) Uani 1 1 d . . . H14 H 0.5062 0.6383 0.1844 0.038 Uiso 1 1 calc R . . C15 C 0.3958(6) 0.6327(4) 0.0954(3) 0.0463(17) Uani 1 1 d . . . H15A H 0.2971 0.6431 0.1139 0.069 Uiso 1 1 calc R . . H15B H 0.3999 0.5716 0.0763 0.069 Uiso 1 1 calc R . . H15C H 0.4108 0.6594 0.0601 0.069 Uiso 1 1 calc R . . C16 C 0.5022(6) 0.7634(3) 0.1878(3) 0.0434(16) Uani 1 1 d . . . H16A H 0.5155 0.7962 0.1564 0.065 Uiso 1 1 calc R . . H16B H 0.5786 0.7857 0.2251 0.065 Uiso 1 1 calc R . . H16C H 0.4014 0.7680 0.2053 0.065 Uiso 1 1 calc R . . C17 C 0.8376(5) 0.7060(4) 0.1957(2) 0.0297(12) Uani 1 1 d . . . H17 H 0.8396 0.7684 0.2041 0.036 Uiso 1 1 calc R . . C18 C 0.7905(6) 0.6923(4) 0.2617(3) 0.0447(16) Uani 1 1 d . . . H18A H 0.8103 0.6356 0.2615 0.067 Uiso 1 1 calc R . . H18B H 0.6827 0.6977 0.2665 0.067 Uiso 1 1 calc R . . H18C H 0.8485 0.7348 0.2994 0.067 Uiso 1 1 calc R . . C19 C 1.0005(6) 0.6881(4) 0.1832(3) 0.0418(15) Uani 1 1 d . . . H19A H 1.0679 0.7292 0.2182 0.063 Uiso 1 1 calc R . . H19B H 1.0262 0.6927 0.1392 0.063 Uiso 1 1 calc R . . H19C H 1.0120 0.6308 0.1842 0.063 Uiso 1 1 calc R . . C20 C 1.0115(5) 0.7947(3) -0.0765(3) 0.0273(12) Uani 1 1 d . . . H20 H 1.0296 0.7871 -0.1248 0.033 Uiso 1 1 calc R . . C21 C 1.1471(5) 0.7658(4) -0.0463(3) 0.0349(14) Uani 1 1 d . . . H21A H 1.2396 0.8005 -0.0502 0.052 Uiso 1 1 calc R . . H21B H 1.1554 0.7063 -0.0706 0.052 Uiso 1 1 calc R . . H21C H 1.1325 0.7724 0.0012 0.052 Uiso 1 1 calc R . . C22 C 1.0019(6) 0.8887(3) -0.0419(3) 0.0325(13) Uani 1 1 d . . . H22A H 0.9803 0.8980 0.0053 0.049 Uiso 1 1 calc R . . H22B H 0.9210 0.9075 -0.0643 0.049 Uiso 1 1 calc R . . H22C H 1.0980 0.9211 -0.0446 0.049 Uiso 1 1 calc R . . C23 C 0.6968(5) 0.7733(3) -0.1139(2) 0.0241(11) Uani 1 1 d . . . H23 H 0.6988 0.8328 -0.0834 0.029 Uiso 1 1 calc R . . C24 C 0.5336(5) 0.7351(4) -0.1156(3) 0.0332(13) Uani 1 1 d . . . H24A H 0.4657 0.7725 -0.1261 0.050 Uiso 1 1 calc R . . H24B H 0.5119 0.7287 -0.0717 0.050 Uiso 1 1 calc R . . H24C H 0.5183 0.6795 -0.1501 0.050 Uiso 1 1 calc R . . C25 C 0.7324(6) 0.7829(4) -0.1825(3) 0.0362(14) Uani 1 1 d . . . H25A H 0.7202 0.7270 -0.2166 0.054 Uiso 1 1 calc R . . H25B H 0.8365 0.8088 -0.1806 0.054 Uiso 1 1 calc R . . H25C H 0.6633 0.8190 -0.1940 0.054 Uiso 1 1 calc R . . C26 C 0.8739(5) 0.6229(3) -0.1339(2) 0.0228(11) Uani 1 1 d . . . H26 H 0.9368 0.5971 -0.1071 0.027 Uiso 1 1 calc R . . C27 C 0.7322(6) 0.5605(3) -0.1569(3) 0.0346(14) Uani 1 1 d . . . H27A H 0.6774 0.5733 -0.1929 0.052 Uiso 1 1 calc R . . H27B H 0.6675 0.5652 -0.1190 0.052 Uiso 1 1 calc R . . H27C H 0.7604 0.5028 -0.1735 0.052 Uiso 1 1 calc R . . C28 C 0.9658(6) 0.6231(4) -0.1950(3) 0.0359(14) Uani 1 1 d . . . H28A H 0.9833 0.5650 -0.2198 0.054 Uiso 1 1 calc R . . H28B H 1.0628 0.6577 -0.1798 0.054 Uiso 1 1 calc R . . H28C H 0.9098 0.6467 -0.2243 0.054 Uiso 1 1 calc R . . C29 C 0.8291(6) 0.0941(3) 0.3896(3) 0.0247(11) Uani 1 1 d . . . H29 H 0.9247 0.1086 0.4135 0.030 Uiso 1 1 calc R . . C30 C 0.8003(6) 0.0149(3) 0.3395(3) 0.0327(13) Uani 1 1 d . . . C31 C 0.9183(7) -0.0467(4) 0.3275(3) 0.0444(16) Uani 1 1 d . . . H31A H 0.9068 -0.0799 0.3587 0.067 Uiso 1 1 calc R . . H31B H 1.0192 -0.0152 0.3349 0.067 Uiso 1 1 calc R . . H31C H 0.9052 -0.0848 0.2812 0.067 Uiso 1 1 calc R . . C32 C 0.6652(6) -0.0057(3) 0.3043(3) 0.0333(13) Uani 1 1 d . . . H32 H 0.6455 -0.0583 0.2696 0.040 Uiso 1 1 calc R . . C33 C 0.5529(6) 0.0511(3) 0.3190(2) 0.0241(11) Uani 1 1 d . . . C34 C 0.5901(5) 0.1274(3) 0.3712(2) 0.0207(11) Uani 1 1 d . . . C35 C 0.4993(5) 0.1935(3) 0.3956(2) 0.0195(10) Uani 1 1 d . . . C36 C 0.3577(5) 0.1798(3) 0.3636(3) 0.0288(12) Uani 1 1 d . . . H36 H 0.2891 0.2211 0.3770 0.035 Uiso 1 1 calc R . . C37 C 0.3153(6) 0.1032(3) 0.3102(3) 0.0305(13) Uani 1 1 d . . . H37 H 0.2174 0.0953 0.2890 0.037 Uiso 1 1 calc R . . C38 C 0.4061(6) 0.0407(3) 0.2877(3) 0.0310(13) Uani 1 1 d . . . H38 H 0.3722 -0.0090 0.2518 0.037 Uiso 1 1 calc R . . C39 C 0.6425(6) 0.3085(3) 0.6423(3) 0.0279(12) Uani 1 1 d . . . H39 H 0.6070 0.2801 0.6756 0.033 Uiso 1 1 calc R . . C40 C 0.8100(6) 0.3371(4) 0.6583(3) 0.0413(15) Uani 1 1 d . . . H40A H 0.8547 0.3500 0.6199 0.062 Uiso 1 1 calc R . . H40B H 0.8594 0.2918 0.6676 0.062 Uiso 1 1 calc R . . H40C H 0.8238 0.3878 0.6978 0.062 Uiso 1 1 calc R . . C41 C 0.5596(7) 0.3868(3) 0.6535(3) 0.0436(16) Uani 1 1 d . . . H41A H 0.5913 0.4273 0.6977 0.065 Uiso 1 1 calc R . . H41B H 0.4507 0.3704 0.6514 0.065 Uiso 1 1 calc R . . H41C H 0.5836 0.4130 0.6185 0.065 Uiso 1 1 calc R . . C42 C 0.6948(6) 0.1374(3) 0.5637(3) 0.0289(12) Uani 1 1 d . . . H42 H 0.6524 0.0887 0.5242 0.035 Uiso 1 1 calc R . . C43 C 0.8653(6) 0.1455(4) 0.5564(3) 0.0346(14) Uani 1 1 d . . . H43A H 0.9170 0.1724 0.6007 0.052 Uiso 1 1 calc R . . H43B H 0.8907 0.1801 0.5272 0.052 Uiso 1 1 calc R . . H43C H 0.8975 0.0891 0.5366 0.052 Uiso 1 1 calc R . . C44 C 0.6587(7) 0.1101(4) 0.6256(3) 0.0459(16) Uani 1 1 d . . . H44A H 0.6948 0.0551 0.6204 0.069 Uiso 1 1 calc R . . H44B H 0.5494 0.1055 0.6303 0.069 Uiso 1 1 calc R . . H44C H 0.7088 0.1522 0.6658 0.069 Uiso 1 1 calc R . . C45 C 0.3980(5) 0.1926(3) 0.5626(3) 0.0306(13) Uani 1 1 d . . . H45 H 0.3825 0.1945 0.6101 0.037 Uiso 1 1 calc R . . C46 C 0.3540(6) 0.1014(3) 0.5179(3) 0.0415(15) Uani 1 1 d . . . H46A H 0.2448 0.0872 0.5177 0.062 Uiso 1 1 calc R . . H46B H 0.4061 0.0629 0.5354 0.062 Uiso 1 1 calc R . . H46C H 0.3831 0.0956 0.4720 0.062 Uiso 1 1 calc R . . C47 C 0.2922(5) 0.2506(4) 0.5449(3) 0.0401(15) Uani 1 1 d . . . H47A H 0.2967 0.2451 0.4971 0.060 Uiso 1 1 calc R . . H47B H 0.3238 0.3095 0.5718 0.060 Uiso 1 1 calc R . . H47C H 0.1887 0.2343 0.5545 0.060 Uiso 1 1 calc R . . C48 C 0.8681(5) 0.3006(3) 0.3233(2) 0.0232(11) Uani 1 1 d . . . H48 H 0.8984 0.3446 0.3013 0.028 Uiso 1 1 calc R . . C49 C 1.0130(5) 0.2823(3) 0.3547(3) 0.0305(13) Uani 1 1 d . . . H49A H 0.9878 0.2393 0.3769 0.046 Uiso 1 1 calc R . . H49B H 1.0605 0.3343 0.3878 0.046 Uiso 1 1 calc R . . H49C H 1.0829 0.2614 0.3195 0.046 Uiso 1 1 calc R . . C50 C 0.7961(6) 0.2215(3) 0.2677(3) 0.0309(13) Uani 1 1 d . . . H50A H 0.8685 0.2030 0.2332 0.046 Uiso 1 1 calc R . . H50B H 0.7058 0.2350 0.2476 0.046 Uiso 1 1 calc R . . H50C H 0.7682 0.1761 0.2871 0.046 Uiso 1 1 calc R . . C51 C 0.5785(5) 0.3630(3) 0.3370(2) 0.0213(11) Uani 1 1 d . . . H51 H 0.5403 0.3053 0.3066 0.026 Uiso 1 1 calc R . . C52 C 0.4437(5) 0.3962(3) 0.3762(3) 0.0262(12) Uani 1 1 d . . . H52A H 0.4674 0.4567 0.4003 0.039 Uiso 1 1 calc R . . H52B H 0.4212 0.3654 0.4084 0.039 Uiso 1 1 calc R . . H52C H 0.3559 0.3877 0.3450 0.039 Uiso 1 1 calc R . . C53 C 0.6213(5) 0.4149(3) 0.2908(3) 0.0301(12) Uani 1 1 d . . . H53A H 0.5324 0.4159 0.2630 0.045 Uiso 1 1 calc R . . H53B H 0.6999 0.3893 0.2619 0.045 Uiso 1 1 calc R . . H53C H 0.6593 0.4728 0.3177 0.045 Uiso 1 1 calc R . . C54 C 0.8449(5) 0.4521(3) 0.4323(2) 0.0255(12) Uani 1 1 d . . . H54 H 0.9151 0.4417 0.4660 0.031 Uiso 1 1 calc R . . C55 C 0.7444(6) 0.5156(3) 0.4744(3) 0.0355(14) Uani 1 1 d . . . H55A H 0.8075 0.5621 0.5072 0.053 Uiso 1 1 calc R . . H55B H 0.6746 0.4870 0.4980 0.053 Uiso 1 1 calc R . . H55C H 0.6867 0.5382 0.4448 0.053 Uiso 1 1 calc R . . C56 C 0.9477(6) 0.4950(3) 0.3913(3) 0.0348(14) Uani 1 1 d . . . H56A H 0.8864 0.5072 0.3569 0.052 Uiso 1 1 calc R . . H56B H 1.0216 0.4571 0.3698 0.052 Uiso 1 1 calc R . . H56C H 1.0006 0.5479 0.4213 0.052 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 Os1 0.01894(11) 0.02061(11) 0.01630(11) 0.00706(9) 0.00314(8) 0.00348(8) Os2 0.01819(10) 0.01815(11) 0.01591(11) 0.00636(9) 0.00175(8) 0.00191(8) P1 0.0208(7) 0.0272(7) 0.0186(7) 0.0103(6) 0.0052(5) 0.0054(6) P2 0.0203(6) 0.0219(7) 0.0169(7) 0.0080(6) 0.0041(5) 0.0048(5) P3 0.0251(7) 0.0179(7) 0.0190(7) 0.0067(6) 0.0050(5) 0.0021(5) P4 0.0191(6) 0.0191(7) 0.0154(6) 0.0060(5) 0.0022(5) 0.0023(5) N1 0.024(2) 0.023(2) 0.017(2) 0.0095(19) 0.0040(17) 0.0013(18) N2 0.021(2) 0.021(2) 0.018(2) 0.0062(18) -0.0004(17) 0.0005(17) C1 0.025(3) 0.039(3) 0.032(3) 0.017(3) 0.007(2) 0.003(2) C2 0.044(4) 0.035(3) 0.029(3) 0.013(3) 0.014(3) 0.018(3) C3 0.047(4) 0.052(4) 0.053(4) 0.024(4) 0.019(3) 0.024(3) C4 0.050(4) 0.033(3) 0.029(3) 0.008(3) 0.017(3) 0.004(3) C5 0.039(3) 0.018(3) 0.024(3) 0.001(2) 0.011(2) 0.001(2) C6 0.030(3) 0.026(3) 0.016(3) 0.007(2) 0.005(2) 0.000(2) C7 0.031(3) 0.029(3) 0.018(3) 0.009(2) 0.004(2) 0.000(2) C8 0.027(3) 0.042(4) 0.031(3) 0.011(3) 0.002(2) 0.003(3) C9 0.032(3) 0.051(4) 0.027(3) 0.003(3) 0.000(3) -0.010(3) C10 0.045(4) 0.027(3) 0.026(3) 0.001(3) 0.007(3) -0.006(3) C11 0.030(3) 0.029(3) 0.027(3) 0.011(3) 0.005(2) 0.005(2) C12 0.058(4) 0.038(4) 0.045(4) 0.020(3) 0.017(3) 0.013(3) C13 0.060(4) 0.039(4) 0.054(4) 0.027(3) 0.026(3) 0.029(3) C14 0.029(3) 0.040(3) 0.031(3) 0.015(3) 0.016(2) 0.008(3) C15 0.027(3) 0.067(5) 0.049(4) 0.025(4) 0.009(3) 0.002(3) C16 0.054(4) 0.040(4) 0.045(4) 0.021(3) 0.029(3) 0.019(3) C17 0.032(3) 0.037(3) 0.021(3) 0.012(3) 0.001(2) -0.003(3) C18 0.053(4) 0.060(4) 0.019(3) 0.012(3) -0.001(3) -0.002(3) C19 0.036(3) 0.062(4) 0.036(4) 0.028(3) -0.002(3) 0.001(3) C20 0.026(3) 0.030(3) 0.027(3) 0.010(3) 0.006(2) 0.002(2) C21 0.018(3) 0.048(4) 0.039(4) 0.014(3) 0.007(2) 0.000(3) C22 0.042(3) 0.025(3) 0.031(3) 0.010(3) 0.009(3) -0.003(3) C23 0.028(3) 0.026(3) 0.021(3) 0.009(2) 0.000(2) 0.009(2) C24 0.029(3) 0.045(4) 0.028(3) 0.013(3) -0.001(2) 0.011(3) C25 0.038(3) 0.048(4) 0.033(3) 0.026(3) 0.001(3) 0.008(3) C26 0.028(3) 0.022(3) 0.020(3) 0.007(2) 0.002(2) 0.007(2) C27 0.042(3) 0.025(3) 0.030(3) -0.002(3) 0.006(3) 0.002(3) C28 0.045(3) 0.039(3) 0.025(3) 0.006(3) 0.018(3) 0.015(3) C29 0.029(3) 0.024(3) 0.024(3) 0.010(2) 0.006(2) 0.009(2) C30 0.046(4) 0.031(3) 0.026(3) 0.013(3) 0.011(3) 0.015(3) C31 0.066(4) 0.042(4) 0.033(4) 0.015(3) 0.014(3) 0.030(3) C32 0.055(4) 0.028(3) 0.020(3) 0.011(2) 0.008(3) 0.005(3) C33 0.036(3) 0.022(3) 0.013(3) 0.007(2) 0.002(2) -0.004(2) C34 0.022(3) 0.024(3) 0.019(3) 0.011(2) 0.003(2) 0.001(2) C35 0.021(2) 0.020(3) 0.018(3) 0.009(2) 0.003(2) -0.004(2) C36 0.021(3) 0.032(3) 0.035(3) 0.014(3) -0.005(2) 0.003(2) C37 0.026(3) 0.032(3) 0.034(3) 0.016(3) -0.010(2) -0.010(2) C38 0.046(3) 0.026(3) 0.018(3) 0.006(2) -0.006(2) -0.006(3) C39 0.040(3) 0.021(3) 0.024(3) 0.010(2) 0.007(2) 0.001(2) C40 0.049(4) 0.038(4) 0.030(3) 0.003(3) -0.004(3) -0.002(3) C41 0.064(4) 0.028(3) 0.032(4) 0.000(3) 0.007(3) 0.008(3) C42 0.041(3) 0.022(3) 0.027(3) 0.010(2) 0.011(2) 0.009(2) C43 0.043(3) 0.039(3) 0.031(3) 0.019(3) 0.007(3) 0.017(3) C44 0.068(4) 0.036(4) 0.045(4) 0.025(3) 0.017(3) 0.016(3) C45 0.026(3) 0.035(3) 0.031(3) 0.013(3) 0.010(2) -0.006(2) C46 0.034(3) 0.040(4) 0.047(4) 0.014(3) 0.005(3) -0.010(3) C47 0.024(3) 0.050(4) 0.047(4) 0.016(3) 0.011(3) 0.002(3) C48 0.027(3) 0.030(3) 0.013(3) 0.006(2) 0.009(2) 0.006(2) C49 0.022(3) 0.039(3) 0.034(3) 0.013(3) 0.010(2) 0.009(2) C50 0.037(3) 0.036(3) 0.023(3) 0.010(3) 0.008(2) 0.012(3) C51 0.026(3) 0.021(3) 0.017(3) 0.005(2) 0.001(2) 0.003(2) C52 0.024(3) 0.030(3) 0.030(3) 0.016(3) 0.002(2) 0.010(2) C53 0.032(3) 0.037(3) 0.025(3) 0.014(3) 0.001(2) 0.008(3) C54 0.030(3) 0.028(3) 0.018(3) 0.009(2) -0.007(2) -0.007(2) C55 0.043(3) 0.020(3) 0.037(3) 0.001(3) 0.001(3) -0.001(3) C56 0.045(3) 0.033(3) 0.026(3) 0.013(3) 0.002(3) -0.010(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 C7 2.135(5) . ? Os1 N1 2.223(4) . ? Os1 P2 2.3362(13) . ? Os1 P1 2.3416(13) . ? Os1 H01 1.582(10) . ? Os1 H02 1.576(10) . ? Os1 H03 1.586(10) . ? Os2 C35 2.141(5) . ? Os2 N2 2.234(4) . ? Os2 P3 2.3272(13) . ? Os2 P4 2.3409(13) . ? Os2 H04 1.585(10) . ? Os2 H05 1.584(10) . ? Os2 H06 1.581(10) . ? P1 C17 1.865(5) . ? P1 C14 1.872(5) . ? P1 C11 1.873(5) . ? P2 C23 1.858(5) . ? P2 C20 1.860(5) . ? P2 C26 1.865(5) . ? P3 C39 1.862(5) . ? P3 C42 1.864(5) . ? P3 C45 1.887(5) . ? P4 C54 1.864(5) . ? P4 C48 1.865(4) . ? P4 C51 1.867(5) . ? N1 C1 1.327(6) . ? N1 C6 1.357(6) . ? N2 C29 1.320(5) . ? N2 C34 1.369(6) . ? C1 C2 1.392(7) . ? C1 H1 0.9500 . ? C2 C4 1.369(8) . ? C2 C3 1.509(7) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.416(7) . ? C4 H4 0.9500 . ? C5 C10 1.393(7) . ? C5 C6 1.413(7) . ? C6 C7 1.399(7) . ? C7 C8 1.401(7) . ? C8 C9 1.408(8) . ? C8 H8 0.9500 . ? C9 C10 1.382(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.531(7) . ? C11 C13 1.541(6) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.527(8) . ? C14 C16 1.539(7) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.526(7) . ? C17 C18 1.532(7) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.526(7) . ? C20 C21 1.540(7) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.526(6) . ? C23 C25 1.532(7) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.524(7) . ? C26 C28 1.536(6) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.409(7) . ? C29 H29 0.9500 . ? C30 C32 1.358(7) . ? C30 C31 1.517(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.422(7) . ? C32 H32 0.9500 . ? C33 C34 1.406(7) . ? C33 C38 1.423(7) . ? C34 C35 1.409(6) . ? C35 C36 1.382(6) . ? C36 C37 1.427(7) . ? C36 H36 0.9500 . ? C37 C38 1.361(7) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.521(7) . ? C39 C41 1.525(7) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.530(7) . ? C42 C44 1.534(7) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.530(7) . ? C45 C47 1.536(7) . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C50 1.538(7) . ? C48 C49 1.539(6) . ? C48 H48 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C53 1.518(6) . ? C51 C52 1.524(6) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.535(7) . ? C54 C56 1.542(6) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 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 Os1 N1 62.09(17) . . ? C7 Os1 P2 97.22(13) . . ? N1 Os1 P2 93.12(10) . . ? C7 Os1 P1 93.28(13) . . ? N1 Os1 P1 98.85(10) . . ? P2 Os1 P1 166.81(5) . . ? C7 Os1 H01 89.6(14) . . ? N1 Os1 H01 150.2(13) . . ? P2 Os1 H01 80.6(15) . . ? P1 Os1 H01 91.5(15) . . ? C7 Os1 H02 146.1(13) . . ? N1 Os1 H02 151.7(13) . . ? P2 Os1 H02 83.4(15) . . ? P1 Os1 H02 83.5(15) . . ? H01 Os1 H02 56.9(14) . . ? C7 Os1 H03 150.2(13) . . ? N1 Os1 H03 88.3(13) . . ? P2 Os1 H03 87.4(15) . . ? P1 Os1 H03 87.5(15) . . ? H01 Os1 H03 120.2(17) . . ? H02 Os1 H03 63.6(15) . . ? C35 Os2 N2 62.52(16) . . ? C35 Os2 P3 96.84(12) . . ? N2 Os2 P3 93.91(10) . . ? C35 Os2 P4 90.97(12) . . ? N2 Os2 P4 96.47(10) . . ? P3 Os2 P4 169.08(5) . . ? C35 Os2 H04 86.7(13) . . ? N2 Os2 H04 148.7(13) . . ? P3 Os2 H04 83.4(15) . . ? P4 Os2 H04 89.4(15) . . ? C35 Os2 H05 142.4(13) . . ? N2 Os2 H05 155.0(13) . . ? P3 Os2 H05 85.4(15) . . ? P4 Os2 H05 83.7(15) . . ? H04 Os2 H05 56.2(14) . . ? C35 Os2 H06 153.5(13) . . ? N2 Os2 H06 91.1(13) . . ? P3 Os2 H06 87.1(15) . . ? P4 Os2 H06 89.3(15) . . ? H04 Os2 H06 119.8(17) . . ? H05 Os2 H06 63.9(15) . . ? C17 P1 C14 102.5(2) . . ? C17 P1 C11 108.0(2) . . ? C14 P1 C11 100.4(2) . . ? C17 P1 Os1 114.36(17) . . ? C14 P1 Os1 117.38(18) . . ? C11 P1 Os1 112.76(17) . . ? C23 P2 C20 100.5(2) . . ? C23 P2 C26 108.9(2) . . ? C20 P2 C26 101.4(2) . . ? C23 P2 Os1 115.90(15) . . ? C20 P2 Os1 118.99(17) . . ? C26 P2 Os1 109.87(16) . . ? C39 P3 C42 103.1(2) . . ? C39 P3 C45 100.5(2) . . ? C42 P3 C45 100.9(2) . . ? C39 P3 Os2 116.85(16) . . ? C42 P3 Os2 115.03(16) . . ? C45 P3 Os2 117.95(18) . . ? C54 P4 C48 100.7(2) . . ? C54 P4 C51 108.1(2) . . ? C48 P4 C51 100.6(2) . . ? C54 P4 Os2 111.35(16) . . ? C48 P4 Os2 119.11(17) . . ? C51 P4 Os2 115.44(15) . . ? C1 N1 C6 117.2(4) . . ? C1 N1 Os1 149.7(4) . . ? C6 N1 Os1 93.0(3) . . ? C29 N2 C34 118.6(4) . . ? C29 N2 Os2 149.0(4) . . ? C34 N2 Os2 92.5(3) . . ? N1 C1 C2 123.9(5) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C4 C2 C1 118.5(5) . . ? C4 C2 C3 121.8(5) . . ? C1 C2 C3 119.7(6) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C5 120.7(5) . . ? C2 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C10 C5 C6 116.2(5) . . ? C10 C5 C4 128.4(5) . . ? C6 C5 C4 115.5(5) . . ? N1 C6 C7 109.3(4) . . ? N1 C6 C5 124.1(5) . . ? C7 C6 C5 126.5(5) . . ? C6 C7 C8 114.8(5) . . ? C6 C7 Os1 95.6(3) . . ? C8 C7 Os1 149.6(4) . . ? C7 C8 C9 120.4(5) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 122.7(5) . . ? C10 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? C9 C10 C5 119.6(5) . . ? C9 C10 H10 120.2 . . ? C5 C10 H10 120.2 . . ? C12 C11 C13 108.0(4) . . ? C12 C11 P1 116.4(4) . . ? C13 C11 P1 115.3(4) . . ? C12 C11 H11 105.4 . . ? C13 C11 H11 105.4 . . ? P1 C11 H11 105.4 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C16 110.3(5) . . ? C15 C14 P1 111.8(4) . . ? C16 C14 P1 111.5(4) . . ? C15 C14 H14 107.7 . . ? C16 C14 H14 107.7 . . ? P1 C14 H14 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 110.5(4) . . ? C19 C17 P1 111.6(4) . . ? C18 C17 P1 119.1(4) . . ? C19 C17 H17 104.8 . . ? C18 C17 H17 104.8 . . ? P1 C17 H17 104.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C21 110.3(4) . . ? C22 C20 P2 113.6(3) . . ? C21 C20 P2 110.1(3) . . ? C22 C20 H20 107.5 . . ? C21 C20 H20 107.5 . . ? P2 C20 H20 107.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C25 109.9(4) . . ? C24 C23 P2 114.7(3) . . ? C25 C23 P2 117.2(3) . . ? C24 C23 H23 104.5 . . ? C25 C23 H23 104.5 . . ? P2 C23 H23 104.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C28 109.4(4) . . ? C27 C26 P2 112.9(3) . . ? C28 C26 P2 118.9(4) . . ? C27 C26 H26 104.8 . . ? C28 C26 H26 104.8 . . ? P2 C26 H26 104.8 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C29 C30 122.7(5) . . ? N2 C29 H29 118.6 . . ? C30 C29 H29 118.6 . . ? C32 C30 C29 119.1(5) . . ? C32 C30 C31 121.3(5) . . ? C29 C30 C31 119.6(5) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 C33 120.3(5) . . ? C30 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 C38 115.1(5) . . ? C34 C33 C32 116.5(5) . . ? C38 C33 C32 128.4(5) . . ? N2 C34 C33 122.7(4) . . ? N2 C34 C35 109.7(4) . . ? C33 C34 C35 127.6(5) . . ? C36 C35 C34 114.8(5) . . ? C36 C35 Os2 149.8(4) . . ? C34 C35 Os2 95.3(3) . . ? C35 C36 C37 119.6(5) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 124.2(5) . . ? C38 C37 H37 117.9 . . ? C36 C37 H37 117.9 . . ? C37 C38 C33 118.8(5) . . ? C37 C38 H38 120.6 . . ? C33 C38 H38 120.6 . . ? C40 C39 C41 108.5(4) . . ? C40 C39 P3 112.6(3) . . ? C41 C39 P3 113.5(4) . . ? C40 C39 H39 107.3 . . ? C41 C39 H39 107.3 . . ? P3 C39 H39 107.3 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C44 109.8(4) . . ? C43 C42 P3 114.1(4) . . ? C44 C42 P3 115.3(3) . . ? C43 C42 H42 105.5 . . ? C44 C42 H42 105.5 . . ? P3 C42 H42 105.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C47 109.5(5) . . ? C46 C45 P3 112.4(4) . . ? C47 C45 P3 111.8(3) . . ? C46 C45 H45 107.7 . . ? C47 C45 H45 107.7 . . ? P3 C45 H45 107.7 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C50 C48 C49 110.8(4) . . ? C50 C48 P4 113.8(3) . . ? C49 C48 P4 110.7(3) . . ? C50 C48 H48 107.0 . . ? C49 C48 H48 107.0 . . ? P4 C48 H48 107.0 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C53 C51 C52 109.7(4) . . ? C53 C51 P4 115.6(3) . . ? C52 C51 P4 114.4(3) . . ? C53 C51 H51 105.3 . . ? C52 C51 H51 105.3 . . ? P4 C51 H51 105.3 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C56 109.8(4) . . ? C55 C54 P4 112.1(3) . . ? C56 C54 P4 119.3(4) . . ? C55 C54 H54 104.7 . . ? C56 C54 H54 104.7 . . ? P4 C54 H54 104.7 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.934 _refine_diff_density_min -1.926 _refine_diff_density_rms 0.172 #===END