# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 #TrackingRef 'web_deposit_cif_file_0_MontserratOlivan_1331118408. #XRay_sup_material_polypyridyl.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 ; XX ; _publ_contact_letter ; March ##, 2012 Please consider this CIF submission as supplementary material of the structures contained in the paper: Mono and Dinuclear Osmium N,N'-Di- and Tetraphenylbipyridyls and Extended Bipyridyls. Synthesis, Structure and Electrochemistry that is submitted to Chemical Science for publication. ; _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _publ_contact_author_name 'Dr. Montserrat Olivan' loop_ _publ_author_name M.A.Esteruelas I.Fernandez M.Gomez-Gallego M.Martin-Ortiz ; P.Molina ; M.Olivan F.Oton M.A.Sierra M.Valencia #-----------------------------------------------------------------------------80 # Data for compound 11 (local labelling montse1as) data_montse1as _database_code_depnum_ccdc_archive 'CCDC 870543' #TrackingRef 'web_deposit_cif_file_0_MontserratOlivan_1331118408.XRay_sup_material_polypyridyl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H60 N2 Os P2' _chemical_formula_weight 821.04 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 8.5681(6) _cell_length_b 14.7204(10) _cell_length_c 15.3568(11) _cell_angle_alpha 80.2450(10) _cell_angle_beta 76.4900(10) _cell_angle_gamma 80.7930(10) _cell_volume 1841.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6777 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description needle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 3.580 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.596 _exptl_absorpt_correction_T_max 0.768 _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 20686 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.62 _reflns_number_total 7671 _reflns_number_gt 6571 _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^)+(0.0063P)^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 7671 _refine_ls_number_parameters 428 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0453 _refine_ls_wR_factor_gt 0.0433 _refine_ls_goodness_of_fit_ref 0.897 _refine_ls_restrained_S_all 0.897 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os Os 1.028500(17) 0.271231(10) 0.217378(9) 0.01423(4) Uani 1 1 d D . . H01 H 1.158(3) 0.3373(17) 0.2145(19) 0.030 Uiso 1 1 d D . . H02 H 0.983(3) 0.3724(10) 0.1686(18) 0.030 Uiso 1 1 d D . . H03 H 0.902(3) 0.300(2) 0.1531(16) 0.031(10) Uiso 1 1 d D . . P1 P 1.20835(11) 0.23750(6) 0.08328(6) 0.0171(2) Uani 1 1 d . . . P2 P 0.86750(10) 0.35109(6) 0.33382(6) 0.0150(2) Uani 1 1 d . . . N1 N 0.9089(3) 0.14807(18) 0.25947(17) 0.0145(6) Uani 1 1 d . . . N2 N 0.6080(3) -0.29089(18) 0.36214(18) 0.0201(7) Uani 1 1 d . . . C1 C 1.3878(4) 0.1509(2) 0.0972(2) 0.0229(9) Uani 1 1 d . . . H1 H 1.4190 0.1636 0.1524 0.027 Uiso 1 1 calc R . . C2 C 1.3399(5) 0.0525(2) 0.1209(2) 0.0360(10) Uani 1 1 d . . . H2A H 1.3245 0.0317 0.0665 0.054 Uiso 1 1 calc R . . H2B H 1.2388 0.0524 0.1667 0.054 Uiso 1 1 calc R . . H2C H 1.4257 0.0103 0.1446 0.054 Uiso 1 1 calc R . . C3 C 1.5421(4) 0.1529(3) 0.0235(2) 0.0329(10) Uani 1 1 d . . . H3A H 1.6263 0.1053 0.0420 0.049 Uiso 1 1 calc R . . H3B H 1.5790 0.2142 0.0141 0.049 Uiso 1 1 calc R . . H3C H 1.5200 0.1407 -0.0329 0.049 Uiso 1 1 calc R . . C4 C 1.3107(4) 0.3381(2) 0.0185(2) 0.0269(9) Uani 1 1 d . . . H4 H 1.3881 0.3151 -0.0351 0.032 Uiso 1 1 calc R . . C5 C 1.1949(5) 0.4177(3) -0.0182(3) 0.0486(13) Uani 1 1 d . . . H5A H 1.1161 0.4421 0.0324 0.073 Uiso 1 1 calc R . . H5B H 1.1380 0.3947 -0.0568 0.073 Uiso 1 1 calc R . . H5C H 1.2564 0.4672 -0.0536 0.073 Uiso 1 1 calc R . . C6 C 1.4110(5) 0.3749(3) 0.0721(2) 0.0410(11) Uani 1 1 d . . . H6A H 1.4862 0.4144 0.0308 0.061 Uiso 1 1 calc R . . H6B H 1.4722 0.3225 0.1032 0.061 Uiso 1 1 calc R . . H6C H 1.3388 0.4113 0.1168 0.061 Uiso 1 1 calc R . . C7 C 1.1174(4) 0.2058(3) -0.0044(2) 0.0290(9) Uani 1 1 d . . . H7 H 1.0372 0.2607 -0.0180 0.035 Uiso 1 1 calc R . . C8 C 1.2283(4) 0.1911(3) -0.0959(2) 0.0417(12) Uani 1 1 d . . . H8A H 1.3063 0.1355 -0.0884 0.063 Uiso 1 1 calc R . . H8B H 1.2864 0.2453 -0.1198 0.063 Uiso 1 1 calc R . . H8C H 1.1633 0.1833 -0.1382 0.063 Uiso 1 1 calc R . . C9 C 1.0186(5) 0.1248(3) 0.0275(3) 0.0537(14) Uani 1 1 d . . . H9A H 0.9499 0.1241 -0.0152 0.081 Uiso 1 1 calc R . . H9B H 0.9504 0.1316 0.0875 0.081 Uiso 1 1 calc R . . H9C H 1.0916 0.0664 0.0308 0.081 Uiso 1 1 calc R . . C10 C 0.6463(4) 0.3752(2) 0.3354(2) 0.0190(8) Uani 1 1 d . . . H10 H 0.6053 0.3134 0.3531 0.023 Uiso 1 1 calc R . . C11 C 0.6056(4) 0.4127(2) 0.2422(2) 0.0252(9) Uani 1 1 d . . . H11A H 0.4895 0.4136 0.2464 0.038 Uiso 1 1 calc R . . H11B H 0.6669 0.3724 0.1979 0.038 Uiso 1 1 calc R . . H11C H 0.6346 0.4759 0.2231 0.038 Uiso 1 1 calc R . . C12 C 0.5454(4) 0.4357(2) 0.4057(2) 0.0273(9) Uani 1 1 d . . . H12A H 0.5826 0.4971 0.3934 0.041 Uiso 1 1 calc R . . H12B H 0.5580 0.4062 0.4663 0.041 Uiso 1 1 calc R . . H12C H 0.4312 0.4424 0.4024 0.041 Uiso 1 1 calc R . . C13 C 0.9305(4) 0.4655(2) 0.3371(2) 0.0199(8) Uani 1 1 d . . . H13 H 0.8605 0.4904 0.3918 0.024 Uiso 1 1 calc R . . C14 C 0.9102(4) 0.5381(2) 0.2559(2) 0.0257(9) Uani 1 1 d . . . H14A H 0.9531 0.5944 0.2607 0.039 Uiso 1 1 calc R . . H14B H 0.7952 0.5529 0.2543 0.039 Uiso 1 1 calc R . . H14C H 0.9694 0.5136 0.2002 0.039 Uiso 1 1 calc R . . C15 C 1.1061(4) 0.4539(2) 0.3487(2) 0.0265(9) Uani 1 1 d . . . H15A H 1.1797 0.4387 0.2924 0.040 Uiso 1 1 calc R . . H15B H 1.1213 0.4037 0.3979 0.040 Uiso 1 1 calc R . . H15C H 1.1295 0.5120 0.3632 0.040 Uiso 1 1 calc R . . C16 C 0.8743(4) 0.2920(2) 0.4510(2) 0.0186(8) Uani 1 1 d . . . H16 H 0.9868 0.2590 0.4468 0.022 Uiso 1 1 calc R . . C17 C 0.8480(4) 0.3504(2) 0.5282(2) 0.0252(9) Uani 1 1 d . . . H17A H 0.7363 0.3811 0.5393 0.038 Uiso 1 1 calc R . . H17B H 0.9226 0.3975 0.5114 0.038 Uiso 1 1 calc R . . H17C H 0.8682 0.3100 0.5831 0.038 Uiso 1 1 calc R . . C18 C 0.7641(4) 0.2151(2) 0.4799(2) 0.0250(9) Uani 1 1 d . . . H18A H 0.7852 0.1781 0.5363 0.037 Uiso 1 1 calc R . . H18B H 0.7858 0.1750 0.4325 0.037 Uiso 1 1 calc R . . H18C H 0.6507 0.2431 0.4895 0.037 Uiso 1 1 calc R . . C19 C 0.9774(4) 0.0767(2) 0.3139(2) 0.0141(7) Uani 1 1 d . . . C20 C 0.9125(4) -0.0068(2) 0.3393(2) 0.0159(8) Uani 1 1 d . . . H20 H 0.9636 -0.0554 0.3761 0.019 Uiso 1 1 calc R . . C21 C 0.7761(4) -0.0219(2) 0.3129(2) 0.0154(7) Uani 1 1 d . . . C22 C 0.7031(4) 0.0539(2) 0.2624(2) 0.0176(8) Uani 1 1 d . . . H22 H 0.6056 0.0490 0.2451 0.021 Uiso 1 1 calc R . . C23 C 0.7702(4) 0.1356(2) 0.2375(2) 0.0169(8) Uani 1 1 d . . . H23 H 0.7169 0.1857 0.2033 0.020 Uiso 1 1 calc R . . C24 C 1.1176(4) 0.0989(2) 0.3419(2) 0.0139(7) Uani 1 1 d . . . C25 C 1.1927(4) 0.0379(2) 0.4043(2) 0.0178(8) Uani 1 1 d . . . H25 H 1.1542 -0.0202 0.4284 0.021 Uiso 1 1 calc R . . C26 C 1.3221(4) 0.0611(2) 0.4314(2) 0.0218(8) Uani 1 1 d . . . H26 H 1.3726 0.0199 0.4742 0.026 Uiso 1 1 calc R . . C27 C 1.3770(4) 0.1461(2) 0.3947(2) 0.0222(8) Uani 1 1 d . . . H27 H 1.4670 0.1627 0.4120 0.027 Uiso 1 1 calc R . . C28 C 1.3020(4) 0.2066(2) 0.3333(2) 0.0181(8) Uani 1 1 d . . . H28 H 1.3432 0.2640 0.3094 0.022 Uiso 1 1 calc R . . C29 C 1.1667(4) 0.1874(2) 0.3043(2) 0.0148(7) Uani 1 1 d . . . C30 C 0.7134(4) -0.1140(2) 0.3353(2) 0.0151(7) Uani 1 1 d . . . C31 C 0.5854(4) -0.1295(2) 0.3005(2) 0.0159(8) Uani 1 1 d . . . H31 H 0.5301 -0.0794 0.2673 0.019 Uiso 1 1 calc R . . C32 C 0.5376(4) -0.2179(2) 0.3139(2) 0.0174(8) Uani 1 1 d . . . C33 C 0.7273(4) -0.2743(2) 0.3976(2) 0.0237(9) Uani 1 1 d . . . H33 H 0.7764 -0.3246 0.4336 0.028 Uiso 1 1 calc R . . C34 C 0.7846(4) -0.1899(2) 0.3859(2) 0.0227(8) Uani 1 1 d . . . H34 H 0.8716 -0.1835 0.4122 0.027 Uiso 1 1 calc R . . C35 C 0.4099(4) -0.2364(2) 0.2706(2) 0.0169(8) Uani 1 1 d . . . C36 C 0.4180(4) -0.3229(2) 0.2431(2) 0.0217(8) Uani 1 1 d . . . H36 H 0.5017 -0.3707 0.2555 0.026 Uiso 1 1 calc R . . C37 C 0.3061(4) -0.3399(2) 0.1980(2) 0.0270(9) Uani 1 1 d . . . H37 H 0.3139 -0.3988 0.1788 0.032 Uiso 1 1 calc R . . C38 C 0.1825(4) -0.2710(3) 0.1808(2) 0.0271(9) Uani 1 1 d . . . H38 H 0.1059 -0.2827 0.1495 0.032 Uiso 1 1 calc R . . C39 C 0.1703(4) -0.1855(2) 0.2088(2) 0.0242(9) Uani 1 1 d . . . H39 H 0.0846 -0.1386 0.1977 0.029 Uiso 1 1 calc R . . C40 C 0.2840(4) -0.1683(2) 0.2535(2) 0.0201(8) Uani 1 1 d . . . H40 H 0.2756 -0.1092 0.2725 0.024 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 0.01607(7) 0.01379(7) 0.01258(7) -0.00240(5) -0.00224(5) -0.00171(5) P1 0.0184(5) 0.0175(5) 0.0149(5) -0.0032(4) -0.0024(4) -0.0014(4) P2 0.0157(5) 0.0143(5) 0.0142(5) -0.0021(4) -0.0016(4) -0.0020(4) N1 0.0155(15) 0.0168(16) 0.0115(15) -0.0047(12) -0.0012(12) -0.0030(12) N2 0.0211(17) 0.0166(16) 0.0215(17) -0.0034(13) -0.0015(14) -0.0030(13) C1 0.023(2) 0.025(2) 0.018(2) -0.0060(16) -0.0010(16) 0.0014(17) C2 0.044(3) 0.023(2) 0.034(2) -0.0060(19) 0.000(2) 0.0089(19) C3 0.025(2) 0.039(3) 0.032(2) -0.011(2) -0.0022(19) 0.0053(19) C4 0.032(2) 0.026(2) 0.018(2) -0.0011(17) 0.0038(17) -0.0069(18) C5 0.068(3) 0.032(3) 0.029(3) 0.010(2) 0.005(2) 0.005(2) C6 0.045(3) 0.039(3) 0.038(3) -0.012(2) 0.010(2) -0.026(2) C7 0.020(2) 0.048(3) 0.021(2) -0.0126(19) -0.0030(17) -0.0028(19) C8 0.033(3) 0.073(3) 0.024(2) -0.023(2) -0.0024(19) -0.009(2) C9 0.051(3) 0.089(4) 0.033(3) -0.030(3) 0.001(2) -0.037(3) C10 0.018(2) 0.020(2) 0.0179(19) -0.0026(16) -0.0018(16) -0.0038(16) C11 0.021(2) 0.026(2) 0.028(2) -0.0043(17) -0.0080(17) 0.0027(17) C12 0.019(2) 0.033(2) 0.027(2) -0.0045(18) -0.0022(17) 0.0006(18) C13 0.022(2) 0.0169(19) 0.021(2) -0.0082(16) -0.0002(16) -0.0034(16) C14 0.029(2) 0.0122(19) 0.033(2) -0.0006(17) -0.0007(18) -0.0056(16) C15 0.028(2) 0.029(2) 0.026(2) -0.0107(18) -0.0011(17) -0.0110(18) C16 0.019(2) 0.020(2) 0.0140(19) -0.0049(15) -0.0010(15) 0.0039(16) C17 0.030(2) 0.029(2) 0.017(2) -0.0048(17) -0.0058(17) 0.0009(18) C18 0.040(2) 0.015(2) 0.0132(19) 0.0023(15) 0.0015(17) 0.0001(17) C19 0.0173(18) 0.0132(18) 0.0106(17) -0.0040(14) -0.0003(14) 0.0002(15) C20 0.0192(19) 0.0149(19) 0.0128(18) -0.0010(14) -0.0057(15) 0.0028(15) C21 0.0162(19) 0.0168(19) 0.0121(18) -0.0041(15) -0.0010(15) 0.0004(15) C22 0.0155(19) 0.019(2) 0.021(2) -0.0033(16) -0.0056(15) -0.0042(15) C23 0.0150(19) 0.0164(19) 0.0189(19) -0.0029(15) -0.0062(15) 0.0031(15) C24 0.0107(17) 0.0173(19) 0.0118(17) -0.0049(14) 0.0003(14) 0.0025(14) C25 0.021(2) 0.0142(19) 0.0174(19) -0.0007(15) -0.0032(16) -0.0016(15) C26 0.021(2) 0.026(2) 0.0176(19) -0.0022(16) -0.0077(16) 0.0030(17) C27 0.0163(19) 0.028(2) 0.023(2) -0.0065(17) -0.0053(16) -0.0026(16) C28 0.0172(19) 0.0191(19) 0.0175(19) -0.0057(15) 0.0011(15) -0.0040(15) C29 0.0137(18) 0.0171(19) 0.0127(18) -0.0079(15) 0.0035(14) -0.0024(15) C30 0.0166(19) 0.0159(19) 0.0111(17) -0.0048(14) 0.0023(14) -0.0013(15) C31 0.0188(19) 0.0147(19) 0.0125(18) -0.0033(14) 0.0002(15) -0.0011(15) C32 0.0160(19) 0.019(2) 0.0135(18) -0.0035(15) 0.0038(15) -0.0017(16) C33 0.028(2) 0.018(2) 0.022(2) 0.0050(16) -0.0067(17) -0.0012(17) C34 0.022(2) 0.024(2) 0.023(2) -0.0001(17) -0.0062(17) -0.0061(17) C35 0.0200(19) 0.0165(19) 0.0125(18) -0.0007(15) 0.0029(15) -0.0082(16) C36 0.025(2) 0.017(2) 0.022(2) -0.0009(16) -0.0021(17) -0.0054(17) C37 0.036(2) 0.018(2) 0.029(2) -0.0064(17) -0.0026(19) -0.0115(18) C38 0.027(2) 0.029(2) 0.028(2) -0.0013(18) -0.0054(18) -0.0149(19) C39 0.023(2) 0.024(2) 0.023(2) 0.0002(17) -0.0037(17) -0.0035(17) C40 0.025(2) 0.0161(19) 0.0174(19) 0.0009(15) 0.0006(16) -0.0094(16) _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 C29 2.102(3) . ? Os N1 2.155(3) . ? Os P1 2.3412(9) . ? Os P2 2.3503(9) . ? Os H01 1.579(10) . ? Os H02 1.581(10) . ? Os H03 1.592(10) . ? P1 C7 1.859(3) . ? P1 C4 1.860(3) . ? P1 C1 1.862(3) . ? P2 C13 1.860(3) . ? P2 C10 1.867(3) . ? P2 C16 1.872(3) . ? N1 C23 1.356(4) . ? N1 C19 1.372(4) . ? N2 C33 1.337(4) . ? N2 C32 1.341(4) . ? C1 C3 1.527(4) . ? C1 C2 1.530(4) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.529(5) . ? C4 C6 1.530(5) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C9 1.520(5) . ? C7 C8 1.529(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.532(4) . ? C10 C11 1.542(4) . ? 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 1.523(4) . ? C13 C15 1.536(4) . ? 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 C18 1.532(4) . ? C16 C17 1.534(4) . ? 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 . ? C19 C20 1.388(4) . ? C19 C24 1.466(4) . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 C22 1.395(4) . ? C21 C30 1.494(4) . ? C22 C23 1.373(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.397(4) . ? C24 C29 1.419(4) . ? C25 C26 1.380(4) . ? C25 H25 0.9500 . ? C26 C27 1.388(4) . ? C26 H26 0.9500 . ? C27 C28 1.383(4) . ? C27 H27 0.9500 . ? C28 C29 1.419(4) . ? C28 H28 0.9500 . ? C30 C31 1.391(4) . ? C30 C34 1.391(4) . ? C31 C32 1.394(4) . ? C31 H31 0.9500 . ? C32 C35 1.487(4) . ? C33 C34 1.377(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.391(4) . ? C35 C36 1.394(4) . ? C36 C37 1.382(4) . ? C36 H36 0.9500 . ? C37 C38 1.384(5) . ? C37 H37 0.9500 . ? C38 C39 1.379(4) . ? C38 H38 0.9500 . ? C39 C40 1.391(4) . ? C39 H39 0.9500 . ? C40 H40 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 C29 Os N1 76.48(11) . . ? C29 Os P1 95.59(8) . . ? N1 Os P1 102.26(7) . . ? C29 Os P2 92.86(8) . . ? N1 Os P2 94.66(7) . . ? P1 Os P2 162.44(3) . . ? C29 Os H01 79.8(11) . . ? N1 Os H01 156.3(11) . . ? P1 Os H01 80.9(10) . . ? P2 Os H01 85.5(10) . . ? C29 Os H02 146.5(11) . . ? N1 Os H02 134.9(11) . . ? P1 Os H02 89.0(10) . . ? P2 Os H02 75.6(10) . . ? H01 Os H02 68.1(14) . . ? C29 Os H03 159.7(11) . . ? N1 Os H03 84.0(11) . . ? P1 Os H03 83.2(10) . . ? P2 Os H03 94.1(11) . . ? H01 Os H03 119.7(15) . . ? H02 Os H03 53.8(13) . . ? C7 P1 C4 100.65(16) . . ? C7 P1 C1 108.47(16) . . ? C4 P1 C1 100.19(16) . . ? C7 P1 Os 116.11(11) . . ? C4 P1 Os 113.65(12) . . ? C1 P1 Os 115.66(11) . . ? C13 P2 C10 105.24(15) . . ? C13 P2 C16 101.07(15) . . ? C10 P2 C16 103.27(15) . . ? C13 P2 Os 114.08(11) . . ? C10 P2 Os 116.43(10) . . ? C16 P2 Os 114.98(11) . . ? C23 N1 C19 117.1(3) . . ? C23 N1 Os 125.4(2) . . ? C19 N1 Os 117.5(2) . . ? C33 N2 C32 116.2(3) . . ? C3 C1 C2 110.2(3) . . ? C3 C1 P1 119.4(3) . . ? C2 C1 P1 110.5(2) . . ? C3 C1 H1 105.2 . . ? C2 C1 H1 105.2 . . ? P1 C1 H1 105.2 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C6 110.0(3) . . ? C5 C4 P1 113.4(3) . . ? C6 C4 P1 112.7(2) . . ? C5 C4 H4 106.8 . . ? C6 C4 H4 106.8 . . ? P1 C4 H4 106.8 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9 C7 C8 108.4(3) . . ? C9 C7 P1 114.7(3) . . ? C8 C7 P1 117.8(2) . . ? C9 C7 H7 104.9 . . ? C8 C7 H7 104.9 . . ? P1 C7 H7 104.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 109.6(3) . . ? C12 C10 P2 115.8(2) . . ? C11 C10 P2 114.3(2) . . ? C12 C10 H10 105.4 . . ? C11 C10 H10 105.4 . . ? P2 C10 H10 105.4 . . ? 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 109.5(3) . . ? C14 C13 P2 114.7(2) . . ? C15 C13 P2 110.8(2) . . ? C14 C13 H13 107.2 . . ? C15 C13 H13 107.2 . . ? P2 C13 H13 107.2 . . ? 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 . . ? C18 C16 C17 109.1(3) . . ? C18 C16 P2 111.4(2) . . ? C17 C16 P2 119.6(2) . . ? C18 C16 H16 105.1 . . ? C17 C16 H16 105.1 . . ? P2 C16 H16 105.1 . . ? 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 . . ? N1 C19 C20 120.6(3) . . ? N1 C19 C24 113.8(3) . . ? C20 C19 C24 125.6(3) . . ? C21 C20 C19 122.5(3) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C22 115.6(3) . . ? C20 C21 C30 122.1(3) . . ? C22 C21 C30 122.3(3) . . ? C23 C22 C21 120.9(3) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? N1 C23 C22 123.1(3) . . ? N1 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? C25 C24 C29 122.8(3) . . ? C25 C24 C19 121.6(3) . . ? C29 C24 C19 115.6(3) . . ? C26 C25 C24 120.6(3) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 118.7(3) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 123.3(3) . . ? C27 C28 H28 118.3 . . ? C29 C28 H28 118.3 . . ? C28 C29 C24 113.9(3) . . ? C28 C29 Os 129.6(2) . . ? C24 C29 Os 116.4(2) . . ? C31 C30 C34 116.4(3) . . ? C31 C30 C21 120.7(3) . . ? C34 C30 C21 122.8(3) . . ? C30 C31 C32 120.7(3) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? N2 C32 C31 122.5(3) . . ? N2 C32 C35 116.7(3) . . ? C31 C32 C35 120.7(3) . . ? N2 C33 C34 125.1(3) . . ? N2 C33 H33 117.5 . . ? C34 C33 H33 117.5 . . ? C33 C34 C30 119.1(3) . . ? C33 C34 H34 120.4 . . ? C30 C34 H34 120.4 . . ? C40 C35 C36 118.4(3) . . ? C40 C35 C32 121.7(3) . . ? C36 C35 C32 119.8(3) . . ? C37 C36 C35 120.8(3) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C38 119.9(3) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 120.2(3) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 119.7(3) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C39 C40 C35 120.8(3) . . ? C39 C40 H40 119.6 . . ? C35 C40 H40 119.6 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.62 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.111 _refine_diff_density_min -1.342 _refine_diff_density_rms 0.112 #===END #-----------------------------------------------------------------------------80 # Data for compound 12 (local labelling mae389as) data_mae389as _database_code_depnum_ccdc_archive 'CCDC 870544' #TrackingRef 'web_deposit_cif_file_0_MontserratOlivan_1331118408.XRay_sup_material_polypyridyl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H104 N2 Os2 P4, 2(C7 H8)' _chemical_formula_sum 'C72 H120 N2 Os2 P4' _chemical_formula_weight 1517.98 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 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 17.258(4) _cell_length_b 8.775(2) _cell_length_c 23.919(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.864(5) _cell_angle_gamma 90.00 _cell_volume 3516.5(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3750 _cell_measurement_theta_min 2 _cell_measurement_theta_max 20 _exptl_crystal_description prism _exptl_crystal_colour 'dark violet' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 3.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.655 _exptl_absorpt_correction_T_max 0.825 _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 43143 _diffrn_reflns_av_R_equivalents 0.0867 _diffrn_reflns_av_sigmaI/netI 0.1129 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 28.98 _reflns_number_total 8774 _reflns_number_gt 5956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.625 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.1 (Bruker AXS, 2000)' _computing_data_reduction 'SAINT+ v. 6.1 (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.1 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.1 (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0143P)^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 8774 _refine_ls_number_parameters 384 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 0.852 _refine_ls_restrained_S_all 0.852 _refine_ls_shift/su_max 0.012 _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 0.202870(12) 0.68115(2) 0.447369(9) 0.02012(6) Uani 1 1 d D . . H01 H 0.160(3) 0.829(3) 0.463(2) 0.062(17) Uiso 1 1 d D . . H02 H 0.1128(10) 0.683(6) 0.4505(19) 0.050 Uiso 1 1 d D . . H03 H 0.135(2) 0.560(4) 0.4259(18) 0.050 Uiso 1 1 d D . . P1 P 0.16340(8) 0.77187(15) 0.35325(6) 0.0259(3) Uani 1 1 d . . . P2 P 0.20703(8) 0.61025(15) 0.54216(6) 0.0238(3) Uani 1 1 d . . . N N 0.3127(2) 0.8044(4) 0.46872(15) 0.0182(9) Uani 1 1 d . . . C1 C 0.3801(3) 0.7348(5) 0.46219(19) 0.0191(11) Uani 1 1 d . . . C2 C 0.4526(3) 0.8108(6) 0.47469(18) 0.0211(11) Uani 1 1 d . . . H2 H 0.4987 0.7580 0.4699 0.025 Uiso 1 1 calc R . . C3 C 0.4609(3) 0.9601(5) 0.49379(19) 0.0183(11) Uani 1 1 d . . . C4 C 0.3908(3) 1.0305(5) 0.50003(19) 0.0206(11) Uani 1 1 d . . . H4 H 0.3920 1.1331 0.5130 0.025 Uiso 1 1 calc R . . C5 C 0.3207(3) 0.9516(5) 0.4875(2) 0.0242(12) Uani 1 1 d . . . H5 H 0.2742 1.0028 0.4921 0.029 Uiso 1 1 calc R . . C6 C 0.2871(3) 0.5296(5) 0.42844(19) 0.0212(11) Uani 1 1 d . . . C7 C 0.3671(3) 0.5788(5) 0.44063(19) 0.0197(11) Uani 1 1 d . . . C8 C 0.4300(3) 0.4923(5) 0.43059(19) 0.0217(12) Uani 1 1 d . . . H8 H 0.4827 0.5325 0.4399 0.026 Uiso 1 1 calc R . . C9 C 0.4160(3) 0.3486(5) 0.4072(2) 0.0254(12) Uani 1 1 d . . . H9 H 0.4587 0.2877 0.4010 0.030 Uiso 1 1 calc R . . C10 C 0.3383(3) 0.2947(5) 0.3928(2) 0.0282(13) Uani 1 1 d . . . H10 H 0.3275 0.1972 0.3753 0.034 Uiso 1 1 calc R . . C11 C 0.2765(3) 0.3801(5) 0.4033(2) 0.0249(12) Uani 1 1 d . . . H11 H 0.2242 0.3382 0.3936 0.030 Uiso 1 1 calc R . . C12 C 0.2364(4) 0.9034(6) 0.3322(2) 0.0415(16) Uani 1 1 d . . . H12 H 0.2605 0.9621 0.3680 0.050 Uiso 1 1 calc R . . C13 C 0.3057(3) 0.8164(8) 0.3183(2) 0.0541(18) Uani 1 1 d . . . H13A H 0.2887 0.7711 0.2799 0.081 Uiso 1 1 calc R . . H13B H 0.3230 0.7356 0.3469 0.081 Uiso 1 1 calc R . . H13C H 0.3502 0.8865 0.3192 0.081 Uiso 1 1 calc R . . C14 C 0.2054(4) 1.0263(7) 0.2856(2) 0.0537(19) Uani 1 1 d . . . H14A H 0.2501 1.0895 0.2807 0.081 Uiso 1 1 calc R . . H14B H 0.1659 1.0906 0.2976 0.081 Uiso 1 1 calc R . . H14C H 0.1806 0.9765 0.2490 0.081 Uiso 1 1 calc R . . C15 C 0.0729(3) 0.8927(6) 0.3380(2) 0.0397(16) Uani 1 1 d . . . H15 H 0.0644 0.9304 0.2975 0.048 Uiso 1 1 calc R . . C16 C -0.0022(3) 0.8046(8) 0.3423(3) 0.071(2) Uani 1 1 d . . . H16A H 0.0066 0.7568 0.3803 0.106 Uiso 1 1 calc R . . H16B H -0.0137 0.7257 0.3124 0.106 Uiso 1 1 calc R . . H16C H -0.0475 0.8750 0.3369 0.106 Uiso 1 1 calc R . . C17 C 0.0831(4) 1.0333(7) 0.3778(2) 0.065(2) Uani 1 1 d . . . H17A H 0.0418 1.1086 0.3618 0.097 Uiso 1 1 calc R . . H17B H 0.1359 1.0782 0.3807 0.097 Uiso 1 1 calc R . . H17C H 0.0781 1.0023 0.4161 0.097 Uiso 1 1 calc R . . C18 C 0.1451(4) 0.6256(6) 0.2966(2) 0.0406(16) Uani 1 1 d . . . H18 H 0.1982 0.5775 0.2985 0.049 Uiso 1 1 calc R . . C19 C 0.1165(4) 0.6843(7) 0.2347(2) 0.0572(19) Uani 1 1 d . . . H19A H 0.1131 0.5990 0.2077 0.086 Uiso 1 1 calc R . . H19B H 0.1544 0.7600 0.2270 0.086 Uiso 1 1 calc R . . H19C H 0.0638 0.7313 0.2297 0.086 Uiso 1 1 calc R . . C20 C 0.0901(4) 0.4940(7) 0.3058(2) 0.059(2) Uani 1 1 d . . . H20A H 0.0342 0.5256 0.2925 0.089 Uiso 1 1 calc R . . H20B H 0.1014 0.4683 0.3468 0.089 Uiso 1 1 calc R . . H20C H 0.0998 0.4046 0.2838 0.089 Uiso 1 1 calc R . . C21 C 0.1388(4) 0.7226(6) 0.5761(3) 0.0435(16) Uani 1 1 d . . . H21 H 0.1463 0.6843 0.6165 0.052 Uiso 1 1 calc R . . C22 C 0.0500(4) 0.7018(8) 0.5461(3) 0.072(2) Uani 1 1 d . . . H22A H 0.0174 0.7638 0.5658 0.108 Uiso 1 1 calc R . . H22B H 0.0354 0.5943 0.5477 0.108 Uiso 1 1 calc R . . H22C H 0.0408 0.7342 0.5059 0.108 Uiso 1 1 calc R . . C23 C 0.1620(5) 0.8922(7) 0.5802(3) 0.076(3) Uani 1 1 d . . . H23A H 0.1462 0.9385 0.5418 0.114 Uiso 1 1 calc R . . H23B H 0.2198 0.9019 0.5951 0.114 Uiso 1 1 calc R . . H23C H 0.1346 0.9442 0.6062 0.114 Uiso 1 1 calc R . . C24 C 0.1680(4) 0.4168(6) 0.5501(2) 0.0416(16) Uani 1 1 d . . . H24 H 0.1118 0.4197 0.5265 0.050 Uiso 1 1 calc R . . C25 C 0.1604(4) 0.3709(7) 0.6101(3) 0.066(2) Uani 1 1 d . . . H25A H 0.1277 0.2786 0.6073 0.098 Uiso 1 1 calc R . . H25B H 0.1350 0.4536 0.6267 0.098 Uiso 1 1 calc R . . H25C H 0.2136 0.3510 0.6347 0.098 Uiso 1 1 calc R . . C26 C 0.2053(5) 0.2923(6) 0.5247(3) 0.076(2) Uani 1 1 d . . . H26A H 0.2530 0.2568 0.5527 0.114 Uiso 1 1 calc R . . H26B H 0.2203 0.3291 0.4901 0.114 Uiso 1 1 calc R . . H26C H 0.1673 0.2079 0.5145 0.114 Uiso 1 1 calc R . . C27 C 0.3034(3) 0.6349(7) 0.5947(2) 0.0421(16) Uani 1 1 d . . . H27 H 0.3253 0.7333 0.5840 0.050 Uiso 1 1 calc R . . C28 C 0.3057(4) 0.6495(7) 0.6589(2) 0.0516(19) Uani 1 1 d . . . H28A H 0.2859 0.5552 0.6724 0.077 Uiso 1 1 calc R . . H28B H 0.2720 0.7350 0.6647 0.077 Uiso 1 1 calc R . . H28C H 0.3607 0.6677 0.6806 0.077 Uiso 1 1 calc R . . C29 C 0.3638(4) 0.5140(8) 0.5878(2) 0.063(2) Uani 1 1 d . . . H29A H 0.4172 0.5445 0.6094 0.095 Uiso 1 1 calc R . . H29B H 0.3635 0.5034 0.5469 0.095 Uiso 1 1 calc R . . H29C H 0.3496 0.4163 0.6025 0.095 Uiso 1 1 calc R . . C30 C 0.3972(4) 1.0362(7) 0.6655(3) 0.0497(18) Uani 1 1 d . . . H30 H 0.3629 1.0855 0.6336 0.060 Uiso 1 1 calc R . . C31 C 0.4652(4) 0.9643(7) 0.6585(3) 0.0536(19) Uani 1 1 d . . . H31 H 0.4784 0.9671 0.6222 0.064 Uiso 1 1 calc R . . C32 C 0.5146(4) 0.8878(7) 0.7042(3) 0.0556(19) Uani 1 1 d . . . H32 H 0.5610 0.8367 0.6992 0.067 Uiso 1 1 calc R . . C33 C 0.4956(4) 0.8870(7) 0.7567(3) 0.061(2) Uani 1 1 d . . . H33 H 0.5284 0.8333 0.7881 0.073 Uiso 1 1 calc R . . C34 C 0.4293(4) 0.9635(7) 0.7642(3) 0.0493(18) Uani 1 1 d . . . H34 H 0.4184 0.9657 0.8013 0.059 Uiso 1 1 calc R . . C35 C 0.3782(4) 1.0369(7) 0.7192(3) 0.0492(17) Uani 1 1 d . . . C36 C 0.3042(4) 1.1146(8) 0.7264(3) 0.077(2) Uani 1 1 d . . . H36A H 0.3013 1.1079 0.7667 0.116 Uiso 1 1 calc R . . H36B H 0.2574 1.0649 0.7018 0.116 Uiso 1 1 calc R . . H36C H 0.3054 1.2219 0.7153 0.116 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 0.01761(10) 0.01891(9) 0.02216(10) 0.00038(11) 0.00147(7) -0.00348(11) P1 0.0254(8) 0.0244(7) 0.0246(8) -0.0007(6) -0.0003(6) -0.0051(6) P2 0.0235(8) 0.0229(7) 0.0247(8) -0.0009(6) 0.0052(6) -0.0046(6) N 0.017(2) 0.017(2) 0.019(2) -0.0013(18) 0.0024(17) -0.0010(19) C1 0.022(3) 0.021(3) 0.012(3) 0.003(2) 0.000(2) 0.002(2) C2 0.017(3) 0.026(3) 0.019(3) 0.001(2) 0.001(2) 0.006(2) C3 0.018(3) 0.022(3) 0.014(3) 0.002(2) 0.001(2) -0.003(2) C4 0.022(3) 0.015(2) 0.023(3) -0.005(2) 0.001(2) -0.002(2) C5 0.023(3) 0.022(3) 0.027(3) 0.002(2) 0.005(2) 0.003(2) C6 0.022(3) 0.022(3) 0.019(3) 0.001(2) 0.002(2) -0.005(2) C7 0.025(3) 0.016(3) 0.015(3) -0.001(2) 0.000(2) -0.003(2) C8 0.022(3) 0.022(3) 0.020(3) 0.000(2) 0.002(2) -0.003(2) C9 0.030(3) 0.018(3) 0.027(3) 0.000(2) 0.005(2) 0.007(2) C10 0.043(4) 0.015(3) 0.024(3) -0.003(2) 0.003(3) -0.007(2) C11 0.026(3) 0.024(3) 0.022(3) 0.002(2) 0.000(2) -0.003(2) C12 0.049(4) 0.044(4) 0.025(3) 0.003(3) -0.004(3) -0.023(3) C13 0.033(4) 0.096(5) 0.033(4) 0.021(4) 0.008(3) -0.004(4) C14 0.072(5) 0.053(4) 0.027(4) 0.014(3) -0.006(3) -0.025(4) C15 0.039(4) 0.044(4) 0.031(4) 0.008(3) -0.001(3) 0.012(3) C16 0.032(4) 0.103(6) 0.072(5) 0.043(5) 0.002(4) 0.020(4) C17 0.087(6) 0.060(5) 0.041(4) 0.010(4) 0.003(4) 0.040(4) C18 0.051(4) 0.034(3) 0.029(3) -0.002(3) -0.007(3) -0.007(3) C19 0.087(5) 0.044(4) 0.032(4) -0.008(3) -0.003(4) -0.021(4) C20 0.079(5) 0.041(4) 0.041(4) -0.006(3) -0.017(4) -0.018(4) C21 0.056(5) 0.038(4) 0.043(4) 0.006(3) 0.024(3) 0.009(3) C22 0.046(5) 0.105(6) 0.072(5) 0.005(5) 0.028(4) 0.022(5) C23 0.146(8) 0.042(4) 0.049(5) 0.003(4) 0.043(5) 0.024(5) C24 0.057(4) 0.032(3) 0.038(4) 0.003(3) 0.017(3) -0.016(3) C25 0.108(6) 0.044(4) 0.053(5) 0.006(3) 0.034(4) -0.025(4) C26 0.152(8) 0.028(4) 0.071(5) 0.012(3) 0.074(5) 0.007(4) C27 0.038(4) 0.053(4) 0.033(4) 0.006(3) 0.004(3) -0.018(3) C28 0.059(5) 0.058(5) 0.032(4) 0.001(3) -0.001(3) -0.022(3) C29 0.038(4) 0.122(7) 0.028(4) 0.018(4) 0.005(3) 0.012(4) C30 0.073(5) 0.038(4) 0.035(4) -0.004(3) 0.007(4) 0.005(4) C31 0.077(6) 0.049(4) 0.036(4) -0.006(3) 0.016(4) -0.006(4) C32 0.066(5) 0.049(4) 0.047(5) -0.011(4) 0.003(4) 0.005(4) C33 0.079(6) 0.055(5) 0.041(5) -0.009(4) -0.001(4) 0.006(4) C34 0.072(5) 0.046(4) 0.027(4) -0.005(3) 0.007(4) -0.009(4) C35 0.059(5) 0.038(4) 0.050(4) -0.015(3) 0.011(4) -0.003(3) C36 0.085(6) 0.066(5) 0.081(6) -0.012(4) 0.022(5) 0.017(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 C6 2.098(5) . ? Os N 2.135(4) . ? Os P1 2.3304(15) . ? Os P2 2.3355(15) . ? Os H01 1.584(10) . ? Os H02 1.573(10) . ? Os H03 1.578(10) . ? P1 C18 1.839(5) . ? P1 C15 1.850(5) . ? P1 C12 1.864(6) . ? P2 C27 1.841(5) . ? P2 C24 1.852(5) . ? P2 C21 1.865(6) . ? N C1 1.356(6) . ? N C5 1.363(6) . ? C1 C2 1.386(6) . ? C1 C7 1.461(6) . ? C2 C3 1.384(6) . ? C2 H2 0.9500 . ? C3 C4 1.398(6) . ? C3 C3 1.487(9) 3_676 ? C4 C5 1.363(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.408(6) . ? C6 C11 1.436(6) . ? C7 C8 1.392(6) . ? C8 C9 1.378(6) . ? C8 H8 0.9500 . ? C9 C10 1.385(6) . ? C9 H9 0.9500 . ? C10 C11 1.376(6) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.522(8) . ? C12 C14 1.552(7) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.535(8) . ? C15 C17 1.542(7) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.533(7) . ? C18 C20 1.543(7) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.537(7) . ? C21 C22 1.540(8) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.471(7) . ? C24 C25 1.525(7) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.524(8) . ? C27 C28 1.532(7) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.376(8) . ? C30 C35 1.399(8) . ? C30 H30 0.9500 . ? C31 C32 1.387(8) . ? C31 H31 0.9500 . ? C32 C33 1.372(8) . ? C32 H32 0.9500 . ? C33 C34 1.375(8) . ? C33 H33 0.9500 . ? C34 C35 1.377(8) . ? C34 H34 0.9500 . ? C35 C36 1.493(8) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 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 C6 Os N 75.60(17) . . ? C6 Os P1 93.74(13) . . ? N Os P1 95.47(10) . . ? C6 Os P2 100.31(13) . . ? N Os P2 94.80(10) . . ? P1 Os P2 164.29(5) . . ? C6 Os H01 163.4(19) . . ? N Os H01 88.2(19) . . ? P1 Os H01 84.0(17) . . ? P2 Os H01 84.5(17) . . ? C6 Os H02 139.5(19) . . ? N Os H02 144.4(19) . . ? P1 Os H02 88.8(17) . . ? P2 Os H02 76.0(16) . . ? H01 Os H02 57(2) . . ? C6 Os H03 90.2(18) . . ? N Os H03 165.7(18) . . ? P1 Os H03 83.9(16) . . ? P2 Os H03 89.1(16) . . ? H01 Os H03 106(2) . . ? H02 Os H03 50(2) . . ? C18 P1 C15 105.5(3) . . ? C18 P1 C12 103.9(3) . . ? C15 P1 C12 100.6(3) . . ? C18 P1 Os 115.64(18) . . ? C15 P1 Os 115.11(19) . . ? C12 P1 Os 114.34(18) . . ? C27 P2 C24 109.2(3) . . ? C27 P2 C21 101.6(3) . . ? C24 P2 C21 99.0(3) . . ? C27 P2 Os 116.36(19) . . ? C24 P2 Os 114.59(19) . . ? C21 P2 Os 113.99(19) . . ? C1 N C5 116.2(4) . . ? C1 N Os 118.8(3) . . ? C5 N Os 125.0(3) . . ? N C1 C2 120.9(4) . . ? N C1 C7 113.5(4) . . ? C2 C1 C7 125.6(5) . . ? C3 C2 C1 122.9(4) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? C2 C3 C4 115.5(4) . . ? C2 C3 C3 121.9(5) . 3_676 ? C4 C3 C3 122.5(5) . 3_676 ? C5 C4 C3 119.8(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N C5 C4 124.7(5) . . ? N C5 H5 117.7 . . ? C4 C5 H5 117.7 . . ? C7 C6 C11 112.8(4) . . ? C7 C6 Os 117.2(3) . . ? C11 C6 Os 130.0(4) . . ? C8 C7 C6 124.3(4) . . ? C8 C7 C1 120.7(4) . . ? C6 C7 C1 114.9(4) . . ? C9 C8 C7 120.0(5) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 118.6(5) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 121.0(5) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C6 123.2(5) . . ? C10 C11 H11 118.4 . . ? C6 C11 H11 118.4 . . ? C13 C12 C14 110.2(5) . . ? C13 C12 P1 111.5(4) . . ? C14 C12 P1 119.0(4) . . ? C13 C12 H12 104.9 . . ? C14 C12 H12 104.9 . . ? P1 C12 H12 104.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C17 109.6(5) . . ? C16 C15 P1 112.6(4) . . ? C17 C15 P1 111.7(4) . . ? C16 C15 H15 107.6 . . ? C17 C15 H15 107.6 . . ? P1 C15 H15 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C20 108.8(5) . . ? C19 C18 P1 115.9(4) . . ? C20 C18 P1 114.8(4) . . ? C19 C18 H18 105.4 . . ? C20 C18 H18 105.4 . . ? P1 C18 H18 105.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C22 111.0(5) . . ? C23 C21 P2 111.0(4) . . ? C22 C21 P2 113.3(4) . . ? C23 C21 H21 107.1 . . ? C22 C21 H21 107.1 . . ? P2 C21 H21 107.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C25 109.6(5) . . ? C26 C24 P2 115.7(4) . . ? C25 C24 P2 117.0(4) . . ? C26 C24 H24 104.3 . . ? C25 C24 H24 104.3 . . ? P2 C24 H24 104.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 108.2(5) . . ? C29 C27 P2 111.9(4) . . ? C28 C27 P2 119.8(4) . . ? C29 C27 H27 105.2 . . ? C28 C27 H27 105.2 . . ? P2 C27 H27 105.2 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 120.4(6) . . ? C31 C30 H30 119.8 . . ? C35 C30 H30 119.8 . . ? C30 C31 C32 120.5(6) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C33 C32 C31 119.1(7) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 120.3(7) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C35 121.6(6) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C34 C35 C30 118.0(6) . . ? C34 C35 C36 121.8(6) . . ? C30 C35 C36 120.2(6) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.909 _refine_diff_density_min -1.260 _refine_diff_density_rms 0.134 #===END