# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Wen-Yann Yeh' _publ_contact_author_email wenyann@mail.nsysu.edu.tw _publ_section_title ; Synthesis of the phosphino-fullerene PPh2(o-C6H4)(CH2NMeCH)C60 and its function as an e1-P or e3-P,C2 ligand ; loop_ _publ_author_name 'Chia-Hsiang Chen' 'Chi-Shian Chen' 'Huei-Fang Dai' 'Wen-Yann Yeh' # Attachment '- Compound 2.cif' data_a10556 _database_code_depnum_ccdc_archive 'CCDC 843720' #TrackingRef '- Compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C85 H20 N O4 P W), C S2' _chemical_formula_sum 'C171 H40 N2 O8 P2 S2 W2' _chemical_formula_weight 2743.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 10.0412(13) _cell_length_b 16.747(2) _cell_length_c 17.295(2) _cell_angle_alpha 62.545(2) _cell_angle_beta 76.825(2) _cell_angle_gamma 89.449(2) _cell_volume 2497.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 20007 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.04 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1354 _exptl_absorpt_coefficient_mu 2.457 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_process_details 'SADABS, 2003 ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20007 _diffrn_reflns_av_R_equivalents 0.1244 _diffrn_reflns_av_sigmaI/netI 0.1665 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.04 _reflns_number_total 8757 _reflns_number_gt 6042 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8757 _refine_ls_number_parameters 832 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 0.847 _refine_ls_restrained_S_all 0.847 _refine_ls_shift/su_max 0.000 _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 C1 C 0.7529(8) 0.0254(6) 0.4266(5) 0.0240(14) Uani 1 1 d . . . C2 C 0.9919(8) 0.1366(5) 0.3653(5) 0.0240(14) Uani 1 1 d . . . C3 C 0.8596(7) 0.1100(5) 0.2523(5) 0.0190(13) Uani 1 1 d . . . C4 C 0.6099(8) 0.1667(5) 0.3225(5) 0.0190(13) Uani 1 1 d . . . C5 C 1.0525(7) 0.3038(5) 0.1343(5) 0.0225(18) Uani 1 1 d . . . C6 C 1.1640(8) 0.2847(6) 0.1724(5) 0.029(2) Uani 1 1 d . . . H6 H 1.1561 0.2827 0.2291 0.035 Uiso 1 1 calc R . . C7 C 1.2864(8) 0.2688(6) 0.1288(6) 0.041(2) Uani 1 1 d . . . H7 H 1.3621 0.2563 0.1555 0.049 Uiso 1 1 calc R . . C8 C 1.2990(8) 0.2707(6) 0.0476(6) 0.043(3) Uani 1 1 d . . . H8 H 1.3817 0.2566 0.0194 0.052 Uiso 1 1 calc R . . C9 C 1.1921(9) 0.2931(7) 0.0070(6) 0.048(3) Uani 1 1 d . . . H9 H 1.2024 0.2970 -0.0507 0.058 Uiso 1 1 calc R . . C10 C 1.0688(8) 0.3101(6) 0.0497(5) 0.036(2) Uani 1 1 d . . . H10 H 0.9954 0.3260 0.0209 0.043 Uiso 1 1 calc R . . C11 C 0.7770(7) 0.3412(5) 0.1190(5) 0.0185(17) Uani 1 1 d . . . C12 C 0.7230(8) 0.2766(6) 0.1024(5) 0.031(2) Uani 1 1 d . . . H12 H 0.7364 0.2148 0.1354 0.037 Uiso 1 1 calc R . . C13 C 0.6493(8) 0.3024(7) 0.0374(5) 0.035(2) Uani 1 1 d . . . H13 H 0.6141 0.2577 0.0258 0.042 Uiso 1 1 calc R . . C14 C 0.6263(8) 0.3900(7) -0.0101(5) 0.039(2) Uani 1 1 d . . . H14 H 0.5757 0.4067 -0.0545 0.047 Uiso 1 1 calc R . . C15 C 0.6773(8) 0.4525(6) 0.0075(5) 0.032(2) Uani 1 1 d . . . H15 H 0.6586 0.5134 -0.0239 0.039 Uiso 1 1 calc R . . C16 C 0.7556(8) 0.4318(6) 0.0691(5) 0.028(2) Uani 1 1 d . . . H16 H 0.7940 0.4779 0.0775 0.033 Uiso 1 1 calc R . . C17 C 0.9021(8) 0.4120(5) 0.2086(4) 0.0194(17) Uani 1 1 d . . . C18 C 1.0239(8) 0.4710(5) 0.1662(5) 0.026(2) Uani 1 1 d . . . H18 H 1.1034 0.4539 0.1381 0.032 Uiso 1 1 calc R . . C19 C 1.0290(9) 0.5546(6) 0.1648(5) 0.037(2) Uani 1 1 d . . . H19 H 1.1120 0.5945 0.1347 0.044 Uiso 1 1 calc R . . C20 C 0.9161(8) 0.5809(5) 0.2063(5) 0.030(2) Uani 1 1 d . . . H20 H 0.9198 0.6386 0.2041 0.036 Uiso 1 1 calc R . . C21 C 0.7949(8) 0.5196(5) 0.2523(5) 0.0255(19) Uani 1 1 d . . . H21 H 0.7164 0.5356 0.2825 0.031 Uiso 1 1 calc R . . C22 C 0.7901(7) 0.4366(5) 0.2536(5) 0.0214(18) Uani 1 1 d . . . C23 C 0.6621(7) 0.3686(5) 0.3121(4) 0.0199(18) Uani 1 1 d . . . H23 H 0.6576 0.3246 0.2884 0.024 Uiso 1 1 calc R . . C24 C 0.4912(8) 0.4468(6) 0.2308(5) 0.029(2) Uani 1 1 d . . . H24A H 0.4024 0.4708 0.2381 0.043 Uiso 1 1 calc R . . H24B H 0.4840 0.4009 0.2113 0.043 Uiso 1 1 calc R . . H24C H 0.5618 0.4962 0.1854 0.043 Uiso 1 1 calc R . . C25 C 0.4362(7) 0.3257(5) 0.3863(5) 0.0227(19) Uani 1 1 d . . . H25A H 0.4246 0.2823 0.3636 0.027 Uiso 1 1 calc R . . H25B H 0.3449 0.3428 0.4059 0.027 Uiso 1 1 calc R . . C26 C 0.5097(7) 0.2849(5) 0.4647(4) 0.0129(16) Uani 1 1 d . . . C27 C 0.6709(7) 0.3134(5) 0.4138(5) 0.0194(18) Uani 1 1 d . . . C28 C 0.7639(7) 0.2359(5) 0.4306(4) 0.0150(16) Uani 1 1 d . . . C29 C 0.7088(7) 0.1446(5) 0.4874(4) 0.0140(16) Uani 1 1 d . . . C30 C 0.7822(7) 0.0843(5) 0.5528(5) 0.0194(18) Uani 1 1 d . . . C31 C 0.6842(7) 0.0172(5) 0.6318(5) 0.0185(17) Uani 1 1 d . . . C32 C 0.5477(7) 0.0406(5) 0.6237(5) 0.0175(17) Uani 1 1 d . . . C33 C 0.5606(7) 0.1206(5) 0.5383(4) 0.0164(17) Uani 1 1 d . . . C34 C 0.4721(7) 0.1853(5) 0.5297(4) 0.0173(17) Uani 1 1 d . . . C35 C 0.3700(7) 0.1720(5) 0.6104(5) 0.0195(18) Uani 1 1 d . . . C36 C 0.3524(7) 0.0945(5) 0.6915(5) 0.0202(18) Uani 1 1 d . . . C37 C 0.4445(7) 0.0273(5) 0.6986(5) 0.0241(19) Uani 1 1 d . . . C38 C 0.4752(8) -0.0101(5) 0.7867(5) 0.0217(18) Uani 1 1 d . . . C39 C 0.6049(8) -0.0334(5) 0.7957(5) 0.0231(18) Uani 1 1 d . . . C40 C 0.7141(8) -0.0209(5) 0.7168(5) 0.0219(18) Uani 1 1 d . . . C41 C 0.8419(8) 0.0083(5) 0.7243(5) 0.0206(18) Uani 1 1 d . . . C42 C 0.9374(7) 0.0727(6) 0.6472(5) 0.0227(19) Uani 1 1 d . . . C43 C 0.9055(7) 0.1090(5) 0.5601(4) 0.0143(17) Uani 1 1 d . . . C44 C 0.9607(7) 0.2043(5) 0.5077(5) 0.0191(18) Uani 1 1 d . . . C45 C 0.8862(7) 0.2640(5) 0.4524(4) 0.0142(16) Uani 1 1 d . . . C46 C 0.8734(7) 0.3504(5) 0.4508(4) 0.0188(18) Uani 1 1 d . . . C47 C 0.7394(7) 0.3743(5) 0.4411(4) 0.0153(16) Uani 1 1 d . . . C48 C 0.6707(8) 0.4195(5) 0.4848(5) 0.0198(18) Uani 1 1 d . . . C49 C 0.5217(8) 0.3936(5) 0.5296(5) 0.0215(18) Uani 1 1 d . . . C50 C 0.4545(7) 0.3255(5) 0.5270(5) 0.0165(17) Uani 1 1 d . . . C51 C 0.3581(7) 0.2599(5) 0.6065(5) 0.0201(18) Uani 1 1 d . . . C52 C 0.3296(7) 0.2659(5) 0.6878(5) 0.0215(18) Uani 1 1 d . . . C53 C 0.3137(7) 0.1873(6) 0.7705(5) 0.0223(19) Uani 1 1 d . . . C54 C 0.3260(7) 0.1023(5) 0.7745(5) 0.0226(19) Uani 1 1 d . . . C55 C 0.4024(7) 0.0375(5) 0.8321(5) 0.0221(18) Uani 1 1 d . . . C56 C 0.4656(7) 0.0576(5) 0.8870(4) 0.0212(18) Uani 1 1 d . . . C57 C 0.6011(8) 0.0365(5) 0.8948(5) 0.0237(19) Uani 1 1 d . . . C58 C 0.6702(8) -0.0101(5) 0.8516(5) 0.0244(19) Uani 1 1 d . . . C59 C 0.8162(8) 0.0159(5) 0.8073(5) 0.0250(19) Uani 1 1 d . . . C60 C 0.8840(8) 0.0849(6) 0.8096(5) 0.026(2) Uani 1 1 d . . . C61 C 0.9848(7) 0.1522(6) 0.7291(5) 0.027(2) Uani 1 1 d . . . C62 C 1.0101(7) 0.1457(6) 0.6485(5) 0.0222(19) Uani 1 1 d . . . C63 C 1.0247(7) 0.2265(6) 0.5644(5) 0.0216(19) Uani 1 1 d . . . C64 C 1.0148(7) 0.3100(6) 0.5607(5) 0.026(2) Uani 1 1 d . . . C65 C 0.9380(7) 0.3732(5) 0.5038(5) 0.0190(18) Uani 1 1 d . . . C66 C 0.8642(8) 0.4216(5) 0.5488(5) 0.0204(18) Uani 1 1 d . . . C67 C 0.7347(8) 0.4433(5) 0.5395(5) 0.0221(18) Uani 1 1 d . . . C68 C 0.6266(8) 0.4316(5) 0.6180(5) 0.0219(18) Uani 1 1 d . . . C69 C 0.4972(8) 0.4015(5) 0.6118(5) 0.0209(18) Uani 1 1 d . . . C70 C 0.4010(7) 0.3384(5) 0.6886(5) 0.0196(18) Uani 1 1 d . . . C71 C 0.4322(8) 0.3034(6) 0.7763(5) 0.026(2) Uani 1 1 d . . . C72 C 0.3797(8) 0.2091(6) 0.8278(5) 0.0243(19) Uani 1 1 d . . . C73 C 0.4534(8) 0.1470(5) 0.8830(4) 0.0226(19) Uani 1 1 d . . . C74 C 0.5823(8) 0.1769(6) 0.8891(5) 0.028(2) Uani 1 1 d . . . C75 C 0.6722(8) 0.1079(6) 0.8977(5) 0.0246(19) Uani 1 1 d . . . C76 C 0.8132(9) 0.1328(6) 0.8549(5) 0.028(2) Uani 1 1 d . . . C77 C 0.8675(8) 0.2272(6) 0.8036(5) 0.025(2) Uani 1 1 d . . . C78 C 0.9751(7) 0.2401(6) 0.7251(5) 0.0245(19) Uani 1 1 d . . . C79 C 0.9875(7) 0.3173(6) 0.6439(5) 0.028(2) Uani 1 1 d . . . C80 C 0.8972(8) 0.3863(5) 0.6363(5) 0.026(2) Uani 1 1 d . . . C81 C 0.7950(8) 0.3748(5) 0.7107(5) 0.026(2) Uani 1 1 d . . . C82 C 0.7791(8) 0.2932(6) 0.7962(5) 0.0241(19) Uani 1 1 d . . . C83 C 0.6323(8) 0.2681(6) 0.8408(5) 0.027(2) Uani 1 1 d . . . C84 C 0.5561(8) 0.3330(6) 0.7820(5) 0.027(2) Uani 1 1 d . . . C85 C 0.6578(8) 0.3996(5) 0.7010(5) 0.0223(19) Uani 1 1 d . . . C86 C 1.0000 1.0000 0.0000 0.079(6) Uani 1 2 d S . . N1 N 0.5299(6) 0.4052(4) 0.3180(4) 0.0226(16) Uani 1 1 d . . . O1 O 0.7319(6) -0.0535(4) 0.4750(4) 0.0364(15) Uani 1 1 d . . . O2 O 1.0973(6) 0.1222(4) 0.3798(4) 0.0356(15) Uani 1 1 d . . . O3 O 0.8904(5) 0.0809(4) 0.2042(3) 0.0341(14) Uani 1 1 d . . . O4 O 0.5027(5) 0.1686(4) 0.3069(4) 0.0349(15) Uani 1 1 d . . . P1 P 0.8846(2) 0.30749(14) 0.20085(13) 0.0195(5) Uani 1 1 d . . . W1 W 0.80018(3) 0.15539(2) 0.34304(2) 0.01749(10) Uani 1 1 d . . . S1 S 0.9525(4) 0.9083(3) 0.0100(2) 0.1108(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(3) 0.030(4) 0.031(4) -0.026(3) -0.016(3) 0.010(3) C2 0.030(3) 0.030(4) 0.031(4) -0.026(3) -0.016(3) 0.010(3) C3 0.023(3) 0.009(3) 0.023(3) -0.010(3) 0.004(3) -0.008(2) C4 0.023(3) 0.009(3) 0.023(3) -0.010(3) 0.004(3) -0.008(2) C5 0.026(5) 0.014(5) 0.017(4) -0.001(4) -0.001(4) -0.006(4) C6 0.018(4) 0.040(6) 0.026(5) -0.014(5) -0.002(4) 0.001(4) C7 0.023(5) 0.050(7) 0.040(6) -0.011(5) -0.012(4) 0.005(5) C8 0.016(5) 0.063(7) 0.052(6) -0.033(6) 0.003(4) 0.005(5) C9 0.032(6) 0.080(8) 0.026(5) -0.025(6) 0.006(4) 0.004(5) C10 0.026(5) 0.060(7) 0.027(5) -0.025(5) -0.005(4) 0.010(5) C11 0.018(4) 0.022(5) 0.013(4) -0.010(4) 0.005(3) -0.005(4) C12 0.034(5) 0.029(6) 0.027(5) -0.013(5) -0.008(4) 0.005(4) C13 0.032(5) 0.050(7) 0.029(5) -0.024(5) -0.009(4) -0.005(5) C14 0.034(5) 0.057(7) 0.016(5) -0.007(5) -0.009(4) 0.007(5) C15 0.030(5) 0.034(6) 0.020(5) -0.004(5) 0.000(4) 0.008(4) C16 0.036(5) 0.028(5) 0.016(4) -0.007(4) -0.008(4) 0.005(4) C17 0.029(5) 0.013(5) 0.014(4) -0.008(4) 0.002(3) 0.004(4) C18 0.025(5) 0.030(5) 0.030(5) -0.021(5) -0.001(4) -0.003(4) C19 0.039(6) 0.037(6) 0.027(5) -0.012(5) -0.001(4) -0.013(5) C20 0.049(6) 0.017(5) 0.023(5) -0.009(4) -0.009(4) 0.002(4) C21 0.029(5) 0.021(5) 0.029(5) -0.014(4) -0.008(4) 0.004(4) C22 0.026(5) 0.024(5) 0.017(4) -0.010(4) -0.009(4) 0.001(4) C23 0.021(4) 0.028(5) 0.017(4) -0.013(4) -0.010(3) 0.010(4) C24 0.030(5) 0.035(6) 0.020(5) -0.010(4) -0.013(4) 0.017(4) C25 0.019(4) 0.033(5) 0.020(5) -0.014(4) -0.008(4) 0.001(4) C26 0.011(4) 0.011(4) 0.016(4) -0.006(4) -0.001(3) -0.001(3) C27 0.025(4) 0.019(5) 0.015(4) -0.008(4) -0.008(3) 0.006(4) C28 0.021(4) 0.010(4) 0.011(4) -0.005(4) 0.001(3) -0.002(3) C29 0.010(4) 0.025(5) 0.006(4) -0.008(4) -0.001(3) 0.002(3) C30 0.023(4) 0.019(5) 0.023(5) -0.016(4) -0.005(4) 0.008(4) C31 0.029(5) 0.010(4) 0.017(4) -0.007(4) -0.002(4) -0.001(4) C32 0.019(4) 0.013(4) 0.023(5) -0.010(4) -0.008(4) 0.002(3) C33 0.021(4) 0.015(5) 0.012(4) -0.005(4) -0.004(3) -0.005(3) C34 0.017(4) 0.024(5) 0.015(4) -0.011(4) -0.008(3) 0.003(4) C35 0.011(4) 0.031(5) 0.018(4) -0.013(4) -0.002(3) 0.003(4) C36 0.013(4) 0.023(5) 0.020(5) -0.009(4) 0.004(3) -0.003(4) C37 0.020(4) 0.025(5) 0.020(5) -0.008(4) 0.002(4) -0.006(4) C38 0.027(5) 0.013(5) 0.024(5) -0.009(4) -0.003(4) -0.004(4) C39 0.031(5) 0.012(5) 0.015(4) -0.002(4) 0.004(4) -0.001(4) C40 0.029(5) 0.012(5) 0.021(5) -0.004(4) -0.008(4) 0.005(4) C41 0.023(4) 0.020(5) 0.020(5) -0.008(4) -0.011(4) 0.012(4) C42 0.018(4) 0.029(5) 0.026(5) -0.014(4) -0.012(4) 0.019(4) C43 0.011(4) 0.018(5) 0.011(4) -0.005(4) -0.001(3) 0.007(3) C44 0.009(4) 0.032(5) 0.020(4) -0.017(4) 0.002(3) 0.000(4) C45 0.015(4) 0.017(5) 0.007(4) -0.004(4) 0.002(3) -0.005(3) C46 0.019(4) 0.017(5) 0.009(4) -0.003(4) 0.009(3) -0.013(3) C47 0.022(4) 0.007(4) 0.004(4) 0.004(3) 0.003(3) 0.000(3) C48 0.037(5) 0.005(4) 0.013(4) 0.000(4) -0.007(4) 0.005(4) C49 0.026(5) 0.020(5) 0.016(4) -0.007(4) -0.004(4) 0.012(4) C50 0.024(4) 0.016(5) 0.014(4) -0.009(4) -0.012(3) 0.009(4) C51 0.008(4) 0.030(5) 0.021(4) -0.010(4) -0.006(3) 0.003(4) C52 0.013(4) 0.030(5) 0.021(5) -0.013(4) -0.003(3) 0.005(4) C53 0.012(4) 0.032(5) 0.015(4) -0.008(4) 0.005(3) -0.001(4) C54 0.019(4) 0.023(5) 0.012(4) -0.002(4) 0.008(3) -0.006(4) C55 0.020(4) 0.015(5) 0.017(4) 0.000(4) 0.006(4) -0.002(4) C56 0.025(4) 0.019(5) 0.009(4) -0.001(4) 0.003(3) -0.004(4) C57 0.030(5) 0.023(5) 0.009(4) -0.001(4) -0.002(4) 0.003(4) C58 0.034(5) 0.013(5) 0.016(4) 0.001(4) -0.005(4) 0.001(4) C59 0.037(5) 0.022(5) 0.011(4) -0.002(4) -0.010(4) 0.009(4) C60 0.029(5) 0.030(5) 0.015(4) -0.004(4) -0.013(4) 0.005(4) C61 0.017(4) 0.042(6) 0.032(5) -0.018(5) -0.022(4) 0.010(4) C62 0.016(4) 0.033(5) 0.019(4) -0.011(4) -0.009(3) 0.006(4) C63 0.007(4) 0.036(6) 0.024(5) -0.016(4) -0.005(3) 0.002(4) C64 0.018(4) 0.036(6) 0.024(5) -0.017(5) 0.000(4) -0.008(4) C65 0.008(4) 0.019(5) 0.023(5) -0.005(4) -0.001(3) -0.005(3) C66 0.033(5) 0.006(4) 0.018(4) -0.003(4) -0.003(4) -0.007(4) C67 0.031(5) 0.011(5) 0.021(5) -0.005(4) -0.003(4) 0.001(4) C68 0.028(5) 0.018(5) 0.018(4) -0.010(4) 0.001(4) 0.003(4) C69 0.036(5) 0.014(5) 0.022(5) -0.013(4) -0.013(4) 0.014(4) C70 0.021(4) 0.022(5) 0.012(4) -0.005(4) -0.004(3) 0.012(4) C71 0.036(5) 0.029(5) 0.020(5) -0.019(4) -0.004(4) 0.014(4) C72 0.025(5) 0.027(5) 0.014(4) -0.010(4) 0.008(4) -0.002(4) C73 0.026(5) 0.030(5) 0.009(4) -0.007(4) -0.003(4) 0.004(4) C74 0.039(5) 0.037(6) 0.011(4) -0.013(4) -0.008(4) 0.015(4) C75 0.035(5) 0.031(5) 0.014(4) -0.013(4) -0.012(4) 0.009(4) C76 0.042(5) 0.033(6) 0.022(5) -0.019(5) -0.020(4) 0.017(5) C77 0.030(5) 0.032(6) 0.025(5) -0.018(5) -0.017(4) 0.003(4) C78 0.017(4) 0.035(6) 0.024(5) -0.014(5) -0.009(4) 0.003(4) C79 0.013(4) 0.049(6) 0.032(5) -0.024(5) -0.010(4) -0.001(4) C80 0.030(5) 0.023(5) 0.032(5) -0.020(4) -0.006(4) -0.009(4) C81 0.033(5) 0.027(5) 0.022(5) -0.016(4) -0.004(4) -0.007(4) C82 0.029(5) 0.029(5) 0.022(5) -0.016(4) -0.012(4) 0.009(4) C83 0.041(5) 0.026(5) 0.026(5) -0.021(5) -0.009(4) 0.005(4) C84 0.033(5) 0.038(6) 0.032(5) -0.032(5) -0.011(4) 0.014(4) C85 0.031(5) 0.019(5) 0.027(5) -0.018(4) -0.009(4) 0.007(4) C86 0.044(10) 0.121(18) 0.044(10) -0.008(11) -0.027(8) -0.015(10) N1 0.031(4) 0.025(4) 0.011(4) -0.008(3) -0.005(3) 0.007(3) O1 0.051(4) 0.023(4) 0.035(4) -0.010(3) -0.021(3) -0.001(3) O2 0.033(4) 0.046(4) 0.043(4) -0.031(4) -0.015(3) 0.013(3) O3 0.041(4) 0.035(4) 0.035(4) -0.026(3) -0.004(3) 0.003(3) O4 0.029(3) 0.031(4) 0.056(4) -0.028(3) -0.015(3) 0.004(3) P1 0.0211(11) 0.0207(13) 0.0179(11) -0.0109(10) -0.0033(9) 0.0018(9) W1 0.02017(17) 0.01756(19) 0.01693(18) -0.01003(15) -0.00447(13) 0.00258(13) S1 0.111(3) 0.142(4) 0.062(2) -0.022(3) -0.049(2) -0.007(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 C1 O1 1.180(9) . ? C1 W1 1.965(9) . ? C2 O2 1.140(8) . ? C2 W1 2.042(8) . ? C3 O3 1.130(7) . ? C3 W1 2.016(7) . ? C4 O4 1.165(8) . ? C4 W1 2.013(8) . ? C5 C6 1.388(10) . ? C5 C10 1.389(9) . ? C5 P1 1.831(7) . ? C6 C7 1.381(10) . ? C6 H6 0.9500 . ? C7 C8 1.366(10) . ? C7 H7 0.9500 . ? C8 C9 1.371(11) . ? C8 H8 0.9500 . ? C9 C10 1.389(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.384(9) . ? C11 C16 1.401(10) . ? C11 P1 1.854(7) . ? C12 C13 1.386(10) . ? C12 H12 0.9500 . ? C13 C14 1.360(12) . ? C13 H13 0.9500 . ? C14 C15 1.352(11) . ? C14 H14 0.9500 . ? C15 C16 1.382(10) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.389(9) . ? C17 C18 1.398(10) . ? C17 P1 1.829(7) . ? C18 C19 1.391(10) . ? C18 H18 0.9500 . ? C19 C20 1.381(10) . ? C19 H19 0.9500 . ? C20 C21 1.413(10) . ? C20 H20 0.9500 . ? C21 C22 1.381(9) . ? C21 H21 0.9500 . ? C22 C23 1.531(10) . ? C23 N1 1.459(9) . ? C23 C27 1.590(9) . ? C23 H23 1.0000 . ? C24 N1 1.485(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N1 1.456(9) . ? C25 C26 1.563(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C34 1.509(10) . ? C26 C50 1.526(8) . ? C26 C27 1.613(9) . ? C27 C47 1.528(9) . ? C27 C28 1.548(10) . ? C28 C29 1.412(9) . ? C28 C45 1.501(9) . ? C28 W1 2.422(6) . ? C29 C30 1.468(9) . ? C29 C33 1.496(9) . ? C29 W1 2.376(6) . ? C30 C43 1.361(9) . ? C30 C31 1.446(10) . ? C31 C40 1.411(9) . ? C31 C32 1.442(10) . ? C32 C37 1.388(9) . ? C32 C33 1.444(9) . ? C33 C34 1.371(9) . ? C34 C35 1.453(9) . ? C35 C36 1.377(10) . ? C35 C51 1.448(10) . ? C36 C37 1.429(10) . ? C36 C54 1.465(9) . ? C37 C38 1.462(9) . ? C38 C39 1.379(10) . ? C38 C55 1.446(9) . ? C39 C58 1.469(9) . ? C39 C40 1.471(9) . ? C40 C41 1.431(9) . ? C41 C42 1.404(10) . ? C41 C59 1.465(9) . ? C42 C62 1.442(10) . ? C42 C43 1.453(9) . ? C43 C44 1.458(10) . ? C44 C45 1.380(10) . ? C44 C63 1.464(9) . ? C45 C46 1.441(9) . ? C46 C65 1.415(9) . ? C46 C47 1.425(9) . ? C47 C48 1.380(9) . ? C48 C67 1.447(9) . ? C48 C49 1.484(10) . ? C49 C50 1.353(9) . ? C49 C69 1.454(9) . ? C50 C51 1.433(10) . ? C51 C52 1.419(9) . ? C52 C53 1.403(10) . ? C52 C70 1.423(10) . ? C53 C54 1.400(10) . ? C53 C72 1.480(9) . ? C54 C55 1.447(10) . ? C55 C56 1.412(9) . ? C56 C57 1.422(10) . ? C56 C73 1.472(10) . ? C57 C58 1.394(10) . ? C57 C75 1.425(10) . ? C58 C59 1.456(10) . ? C59 C60 1.366(10) . ? C60 C76 1.443(10) . ? C60 C61 1.471(10) . ? C61 C62 1.413(9) . ? C61 C78 1.446(10) . ? C62 C63 1.435(10) . ? C63 C64 1.373(10) . ? C64 C65 1.433(10) . ? C64 C79 1.464(9) . ? C65 C66 1.456(9) . ? C66 C67 1.372(10) . ? C66 C80 1.467(10) . ? C67 C68 1.465(9) . ? C68 C85 1.392(9) . ? C68 C69 1.442(10) . ? C69 C70 1.398(10) . ? C70 C71 1.461(9) . ? C71 C84 1.384(10) . ? C71 C72 1.438(11) . ? C72 C73 1.390(10) . ? C73 C74 1.436(10) . ? C74 C83 1.389(11) . ? C74 C75 1.434(10) . ? C75 C76 1.405(10) . ? C76 C77 1.443(11) . ? C77 C82 1.389(10) . ? C77 C78 1.456(10) . ? C78 C79 1.382(10) . ? C79 C80 1.438(11) . ? C80 C81 1.385(10) . ? C81 C82 1.453(10) . ? C81 C85 1.458(10) . ? C82 C83 1.462(10) . ? C83 C84 1.456(11) . ? C84 C85 1.476(10) . ? C86 S1 1.532(5) . ? C86 S1 1.532(5) 2_775 ? P1 W1 2.563(2) . ? 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 O1 C1 W1 176.2(7) . . ? O2 C2 W1 177.1(7) . . ? O3 C3 W1 177.0(6) . . ? O4 C4 W1 174.1(6) . . ? C6 C5 C10 118.4(7) . . ? C6 C5 P1 119.6(5) . . ? C10 C5 P1 121.7(6) . . ? C7 C6 C5 120.7(7) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C6 120.3(8) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 119.9(8) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C10 120.3(8) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C5 120.2(8) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? C12 C11 C16 118.8(7) . . ? C12 C11 P1 119.6(6) . . ? C16 C11 P1 121.5(5) . . ? C11 C12 C13 119.7(8) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 121.8(8) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C15 C14 C13 118.2(8) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? C14 C15 C16 122.9(9) . . ? C14 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C15 C16 C11 118.6(7) . . ? C15 C16 H16 120.7 . . ? C11 C16 H16 120.7 . . ? C22 C17 C18 118.4(7) . . ? C22 C17 P1 119.8(6) . . ? C18 C17 P1 121.7(5) . . ? C19 C18 C17 120.3(7) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 121.4(8) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 118.2(8) . . ? C19 C20 H20 120.9 . . ? C21 C20 H20 120.9 . . ? C22 C21 C20 120.3(7) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C17 121.3(7) . . ? C21 C22 C23 118.5(7) . . ? C17 C22 C23 120.1(7) . . ? N1 C23 C22 117.0(6) . . ? N1 C23 C27 104.1(5) . . ? C22 C23 C27 111.1(5) . . ? N1 C23 H23 108.1 . . ? C22 C23 H23 108.1 . . ? C27 C23 H23 108.1 . . ? N1 C24 H24A 109.5 . . ? N1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C26 103.1(5) . . ? N1 C25 H25A 111.1 . . ? C26 C25 H25A 111.1 . . ? N1 C25 H25B 111.1 . . ? C26 C25 H25B 111.1 . . ? H25A C25 H25B 109.1 . . ? C34 C26 C50 100.4(5) . . ? C34 C26 C25 116.5(6) . . ? C50 C26 C25 106.9(6) . . ? C34 C26 C27 114.5(6) . . ? C50 C26 C27 115.1(5) . . ? C25 C26 C27 103.7(5) . . ? C47 C27 C28 103.3(5) . . ? C47 C27 C23 110.6(6) . . ? C28 C27 C23 113.6(5) . . ? C47 C27 C26 112.2(5) . . ? C28 C27 C26 117.0(6) . . ? C23 C27 C26 100.5(5) . . ? C29 C28 C45 114.4(6) . . ? C29 C28 C27 121.0(6) . . ? C45 C28 C27 105.8(5) . . ? C29 C28 W1 71.1(4) . . ? C45 C28 W1 118.3(4) . . ? C27 C28 W1 123.4(4) . . ? C28 C29 C30 119.1(6) . . ? C28 C29 C33 120.7(6) . . ? C30 C29 C33 104.2(6) . . ? C28 C29 W1 74.7(4) . . ? C30 C29 W1 111.2(4) . . ? C33 C29 W1 125.7(4) . . ? C43 C30 C31 119.7(6) . . ? C43 C30 C29 124.3(7) . . ? C31 C30 C29 109.6(6) . . ? C40 C31 C32 120.1(6) . . ? C40 C31 C30 120.5(7) . . ? C32 C31 C30 108.2(6) . . ? C37 C32 C31 120.9(6) . . ? C37 C32 C33 120.6(7) . . ? C31 C32 C33 107.9(6) . . ? C34 C33 C32 120.7(6) . . ? C34 C33 C29 121.9(7) . . ? C32 C33 C29 109.1(6) . . ? C33 C34 C35 117.4(7) . . ? C33 C34 C26 124.3(6) . . ? C35 C34 C26 110.7(6) . . ? C36 C35 C51 121.0(6) . . ? C36 C35 C34 122.6(7) . . ? C51 C35 C34 107.1(7) . . ? C35 C36 C37 118.8(6) . . ? C35 C36 C54 119.0(7) . . ? C37 C36 C54 108.2(7) . . ? C32 C37 C36 119.6(7) . . ? C32 C37 C38 119.5(7) . . ? C36 C37 C38 108.7(6) . . ? C39 C38 C55 120.3(6) . . ? C39 C38 C37 120.3(7) . . ? C55 C38 C37 106.9(7) . . ? C38 C39 C58 120.2(6) . . ? C38 C39 C40 120.5(6) . . ? C58 C39 C40 106.8(6) . . ? C31 C40 C41 119.3(7) . . ? C31 C40 C39 118.7(7) . . ? C41 C40 C39 108.9(6) . . ? C42 C41 C40 120.0(6) . . ? C42 C41 C59 119.0(7) . . ? C40 C41 C59 108.4(6) . . ? C41 C42 C62 121.3(6) . . ? C41 C42 C43 119.5(7) . . ? C62 C42 C43 107.1(7) . . ? C30 C43 C42 120.9(7) . . ? C30 C43 C44 118.0(6) . . ? C42 C43 C44 108.5(6) . . ? C45 C44 C43 118.3(6) . . ? C45 C44 C63 121.7(7) . . ? C43 C44 C63 107.1(6) . . ? C44 C45 C46 118.2(6) . . ? C44 C45 C28 124.2(7) . . ? C46 C45 C28 110.5(6) . . ? C65 C46 C47 121.2(6) . . ? C65 C46 C45 120.3(7) . . ? C47 C46 C45 107.9(6) . . ? C48 C47 C46 119.4(6) . . ? C48 C47 C27 125.3(7) . . ? C46 C47 C27 110.8(6) . . ? C47 C48 C67 120.4(7) . . ? C47 C48 C49 119.9(6) . . ? C67 C48 C49 108.0(6) . . ? C50 C49 C69 121.0(7) . . ? C50 C49 C48 119.4(6) . . ? C69 C49 C48 107.4(6) . . ? C49 C50 C51 119.7(6) . . ? C49 C50 C26 125.1(6) . . ? C51 C50 C26 109.9(6) . . ? C52 C51 C50 121.2(7) . . ? C52 C51 C35 119.2(7) . . ? C50 C51 C35 108.6(6) . . ? C53 C52 C51 120.1(7) . . ? C53 C52 C70 109.8(6) . . ? C51 C52 C70 118.1(7) . . ? C54 C53 C52 120.9(6) . . ? C54 C53 C72 118.2(7) . . ? C52 C53 C72 108.0(6) . . ? C53 C54 C55 121.2(7) . . ? C53 C54 C36 119.8(7) . . ? C55 C54 C36 107.1(7) . . ? C56 C55 C38 118.7(7) . . ? C56 C55 C54 121.0(7) . . ? C38 C55 C54 109.1(6) . . ? C55 C56 C57 121.7(7) . . ? C55 C56 C73 118.0(7) . . ? C57 C56 C73 106.8(6) . . ? C58 C57 C56 119.3(6) . . ? C58 C57 C75 120.8(7) . . ? C56 C57 C75 109.4(7) . . ? C57 C58 C59 119.4(7) . . ? C57 C58 C39 119.7(7) . . ? C59 C58 C39 108.1(6) . . ? C60 C59 C58 119.7(7) . . ? C60 C59 C41 120.4(7) . . ? C58 C59 C41 107.8(6) . . ? C59 C60 C76 121.1(7) . . ? C59 C60 C61 120.7(6) . . ? C76 C60 C61 106.6(7) . . ? C62 C61 C78 119.3(7) . . ? C62 C61 C60 119.4(7) . . ? C78 C61 C60 109.3(7) . . ? C61 C62 C63 119.4(7) . . ? C61 C62 C42 119.2(7) . . ? C63 C62 C42 109.6(6) . . ? C64 C63 C62 121.3(6) . . ? C64 C63 C44 119.6(7) . . ? C62 C63 C44 107.7(6) . . ? C63 C64 C65 119.7(6) . . ? C63 C64 C79 119.8(7) . . ? C65 C64 C79 107.3(7) . . ? C46 C65 C64 120.4(7) . . ? C46 C65 C66 118.5(7) . . ? C64 C65 C66 109.3(6) . . ? C67 C66 C65 119.7(6) . . ? C67 C66 C80 121.3(7) . . ? C65 C66 C80 106.8(7) . . ? C66 C67 C48 120.9(6) . . ? C66 C67 C68 119.8(6) . . ? C48 C67 C68 107.4(6) . . ? C85 C68 C69 120.7(7) . . ? C85 C68 C67 119.2(7) . . ? C69 C68 C67 109.1(6) . . ? C70 C69 C68 121.0(6) . . ? C70 C69 C49 119.1(7) . . ? C68 C69 C49 108.1(6) . . ? C69 C70 C52 121.0(6) . . ? C69 C70 C71 119.2(7) . . ? C52 C70 C71 107.6(7) . . ? C84 C71 C72 120.1(7) . . ? C84 C71 C70 119.6(7) . . ? C72 C71 C70 107.9(7) . . ? C73 C72 C71 120.4(7) . . ? C73 C72 C53 120.6(7) . . ? C71 C72 C53 106.7(7) . . ? C72 C73 C74 120.0(7) . . ? C72 C73 C56 120.9(6) . . ? C74 C73 C56 107.5(7) . . ? C83 C74 C75 121.3(8) . . ? C83 C74 C73 120.0(7) . . ? C75 C74 C73 108.1(7) . . ? C76 C75 C57 119.6(7) . . ? C76 C75 C74 119.5(8) . . ? C57 C75 C74 108.2(7) . . ? C75 C76 C60 119.4(7) . . ? C75 C76 C77 120.3(7) . . ? C60 C76 C77 108.5(7) . . ? C82 C77 C76 119.5(7) . . ? C82 C77 C78 119.5(8) . . ? C76 C77 C78 109.2(7) . . ? C79 C78 C61 120.8(7) . . ? C79 C78 C77 119.9(7) . . ? C61 C78 C77 106.3(7) . . ? C78 C79 C80 120.7(7) . . ? C78 C79 C64 119.4(8) . . ? C80 C79 C64 108.5(7) . . ? C81 C80 C79 119.9(8) . . ? C81 C80 C66 119.0(7) . . ? C79 C80 C66 108.0(6) . . ? C80 C81 C82 120.0(8) . . ? C80 C81 C85 120.1(7) . . ? C82 C81 C85 107.8(6) . . ? C77 C82 C81 120.0(7) . . ? C77 C82 C83 120.7(8) . . ? C81 C82 C83 108.5(7) . . ? C74 C83 C84 120.0(7) . . ? C74 C83 C82 118.7(7) . . ? C84 C83 C82 108.2(7) . . ? C71 C84 C83 119.5(8) . . ? C71 C84 C85 121.3(7) . . ? C83 C84 C85 107.3(7) . . ? C68 C85 C81 120.6(7) . . ? C68 C85 C84 118.2(7) . . ? C81 C85 C84 108.2(7) . . ? S1 C86 S1 180.000(1) . 2_775 ? C25 N1 C23 102.4(6) . . ? C25 N1 C24 112.3(6) . . ? C23 N1 C24 112.5(5) . . ? C17 P1 C5 105.0(3) . . ? C17 P1 C11 100.3(3) . . ? C5 P1 C11 102.5(3) . . ? C17 P1 W1 120.7(2) . . ? C5 P1 W1 111.2(3) . . ? C11 P1 W1 115.0(2) . . ? C1 W1 C4 91.3(3) . . ? C1 W1 C3 82.3(3) . . ? C4 W1 C3 91.2(3) . . ? C1 W1 C2 85.9(3) . . ? C4 W1 C2 176.8(3) . . ? C3 W1 C2 86.9(3) . . ? C1 W1 C29 74.4(3) . . ? C4 W1 C29 89.2(2) . . ? C3 W1 C29 156.7(3) . . ? C2 W1 C29 91.5(2) . . ? C1 W1 C28 108.1(3) . . ? C4 W1 C28 93.9(2) . . ? C3 W1 C28 168.3(2) . . ? C2 W1 C28 88.4(2) . . ? C29 W1 C28 34.2(2) . . ? C1 W1 P1 163.20(19) . . ? C4 W1 P1 89.3(2) . . ? C3 W1 P1 80.9(2) . . ? C2 W1 P1 92.9(2) . . ? C29 W1 P1 122.44(19) . . ? C28 W1 P1 88.61(17) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.605 _refine_diff_density_min -1.992 _refine_diff_density_rms 0.154 # Attachment '- Compound 3.cif' data_a11325a _database_code_depnum_ccdc_archive 'CCDC 843721' #TrackingRef '- Compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H20 N O11 Os3 P' _chemical_formula_sum 'C92 H20 N O11 Os3 P' _chemical_formula_weight 1916.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 17.4180(16) _cell_length_b 19.6754(19) _cell_length_c 23.140(2) _cell_angle_alpha 106.174(6) _cell_angle_beta 95.677(6) _cell_angle_gamma 90.006(7) _cell_volume 7575.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 53527 _cell_measurement_theta_min 1.57 _cell_measurement_theta_max 25.03 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.74 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3640 _exptl_absorpt_coefficient_mu 5.103 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1163 _exptl_absorpt_correction_T_max 0.9048 _exptl_absorpt_process_details 'SADABS, 2003 ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53527 _diffrn_reflns_av_R_equivalents 0.1499 _diffrn_reflns_av_sigmaI/netI 0.2396 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.03 _reflns_number_total 25085 _reflns_number_gt 12131 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1803P)^2^+476.5912P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25085 _refine_ls_number_parameters 1033 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2716 _refine_ls_R_factor_gt 0.1668 _refine_ls_wR_factor_ref 0.4249 _refine_ls_wR_factor_gt 0.3611 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 C1 C 0.131(3) 0.621(2) 0.261(2) 0.069(13) Uiso 1 1 d . . . C2 C 0.048(2) 0.5099(18) 0.2686(17) 0.043(9) Uiso 1 1 d . . . C3 C 0.163(2) 0.5597(19) 0.1461(17) 0.048(9) Uiso 1 1 d . . . C4 C -0.054(2) 0.417(2) 0.1795(19) 0.055(10) Uiso 1 1 d . . . C5 C 0.031(2) 0.3511(19) 0.0931(16) 0.042(9) Uiso 1 1 d . . . C6 C 0.053(2) 0.4605(18) 0.0579(17) 0.044(9) Uiso 1 1 d . . . C7 C -0.102(3) 0.427(2) 0.064(2) 0.073(13) Uiso 1 1 d . . . C8 C 0.008(2) 0.6089(19) 0.1044(17) 0.046(9) Uiso 1 1 d . . . C9 C -0.139(3) 0.597(3) 0.124(2) 0.082(15) Uiso 1 1 d . . . C10 C -0.025(3) 0.682(3) 0.213(2) 0.087(15) Uiso 1 1 d . . . C11 C -0.095(3) 0.561(2) 0.227(2) 0.062(11) Uiso 1 1 d . . . C12 C 0.746(2) 0.9364(17) 0.8541(16) 0.037(8) Uiso 1 1 d . . . C13 C 0.698(2) 0.8780(18) 0.7393(16) 0.041(9) Uiso 1 1 d . . . C14 C 0.6110(19) 0.9892(16) 0.7291(15) 0.033(8) Uiso 1 1 d . . . C15 C 0.553(3) 0.819(3) 0.788(3) 0.092(16) Uiso 1 1 d . . . C16 C 0.4802(17) 0.9398(15) 0.7719(16) 0.061(11) Uiso 1 1 d . . . C17 C 0.460(4) 0.907(3) 0.877(3) 0.105(19) Uiso 1 1 d . . . C18 C 0.616(2) 0.895(2) 0.9031(19) 0.054(10) Uiso 1 1 d . . . C19 C 0.518(3) 1.073(3) 0.941(3) 0.091(16) Uiso 1 1 d . . . C20 C 0.668(3) 1.038(2) 0.951(2) 0.063(12) Uiso 1 1 d . . . C21 C 0.640(3) 1.152(2) 0.911(2) 0.066(12) Uiso 1 1 d . . . C22 C 0.532(2) 1.0834(17) 0.8224(16) 0.038(8) Uiso 1 1 d . . . C23 C 0.215(2) 0.3849(19) 0.1540(17) 0.047(9) Uiso 1 1 d . . . C24 C 0.2310(12) 0.4020(14) 0.1000(13) 0.086(15) Uiso 1 1 d . . . H24 H 0.2293 0.4485 0.0980 0.103 Uiso 1 1 calc R . . C25 C 0.249(3) 0.348(3) 0.051(3) 0.094(17) Uiso 1 1 d . . . H25 H 0.2541 0.3577 0.0143 0.113 Uiso 1 1 calc R . . C26 C 0.261(3) 0.279(3) 0.055(2) 0.077 Uiso 1 1 d . . . H26 H 0.2787 0.2454 0.0227 0.092 Uiso 1 1 calc R . . C27 C 0.247(3) 0.263(3) 0.105(2) 0.083(15) Uiso 1 1 d . . . H27 H 0.2474 0.2153 0.1047 0.100 Uiso 1 1 calc R . . C28 C 0.232(3) 0.314(2) 0.157(2) 0.067(12) Uiso 1 1 d . . . H28 H 0.2334 0.3024 0.1931 0.080 Uiso 1 1 calc R . . C29 C 0.300(2) 0.497(2) 0.243(2) 0.060(11) Uani 1 1 d . . . C30 C 0.361(3) 0.450(3) 0.231(2) 0.111(18) Uani 1 1 d . . . H30 H 0.3492 0.4026 0.2114 0.133 Uiso 1 1 calc R . . C31 C 0.441(2) 0.473(3) 0.249(2) 0.081(15) Uani 1 1 d . . . H31 H 0.4820 0.4425 0.2421 0.097 Uiso 1 1 calc R . . C32 C 0.448(4) 0.547(3) 0.277(2) 0.100(19) Uani 1 1 d . . . H32 H 0.4977 0.5644 0.2913 0.120 Uiso 1 1 calc R . . C33 C 0.393(3) 0.594(3) 0.286(3) 0.11(2) Uani 1 1 d . . . H33 H 0.4034 0.6421 0.3024 0.126 Uiso 1 1 calc R . . C34 C 0.316(2) 0.566(2) 0.2671(17) 0.053(10) Uani 1 1 d . . . H34 H 0.2752 0.5966 0.2724 0.064 Uiso 1 1 calc R . . C35 C 0.1817(16) 0.4098(12) 0.2778(15) 0.025(7) Uani 1 1 d . . . C36 C 0.117(2) 0.3622(17) 0.2563(19) 0.050(10) Uani 1 1 d . . . H36 H 0.0898 0.3628 0.2198 0.060 Uiso 1 1 calc R . . C37 C 0.093(2) 0.3165(17) 0.285(2) 0.052(11) Uani 1 1 d . . . H37 H 0.0503 0.2865 0.2680 0.062 Uiso 1 1 calc R . . C38 C 0.131(2) 0.3144(17) 0.3377(18) 0.043(9) Uani 1 1 d . . . H38 H 0.1174 0.2805 0.3563 0.051 Uiso 1 1 calc R . . C39 C 0.189(2) 0.3635(17) 0.3641(16) 0.041(9) Uani 1 1 d . . . H39 H 0.2123 0.3646 0.4024 0.049 Uiso 1 1 calc R . . C40 C 0.2154(18) 0.4106(15) 0.3363(13) 0.028(7) Uani 1 1 d . . . C41 C 0.2843(19) 0.4566(16) 0.3679(15) 0.039(9) Uani 1 1 d . . . H41 H 0.3083 0.4757 0.3389 0.047 Uiso 1 1 calc R . . C42 C 0.377(2) 0.3569(19) 0.3489(17) 0.050(10) Uani 1 1 d . . . H42A H 0.3378 0.3223 0.3282 0.075 Uiso 1 1 calc R . . H42B H 0.4173 0.3347 0.3683 0.075 Uiso 1 1 calc R . . H42C H 0.3989 0.3766 0.3202 0.075 Uiso 1 1 calc R . . C43 C 0.4008(19) 0.4726(16) 0.4299(15) 0.041(9) Uani 1 1 d . . . H43A H 0.4280 0.4908 0.4025 0.049 Uiso 1 1 calc R . . H43B H 0.4378 0.4561 0.4568 0.049 Uiso 1 1 calc R . . C44 C 0.3471(17) 0.5284(15) 0.4655(14) 0.028(7) Uiso 1 1 d . . . C45 C 0.2690(16) 0.5193(14) 0.4256(13) 0.022(6) Uiso 1 1 d . . . C46 C 0.2390(18) 0.5866(16) 0.4107(14) 0.031(7) Uiso 1 1 d . . . C47 C 0.1623(19) 0.5932(16) 0.4138(15) 0.033(8) Uiso 1 1 d . . . C48 C 0.1355(18) 0.5411(16) 0.4432(14) 0.031(7) Uiso 1 1 d . . . C49 C 0.2047(18) 0.5027(15) 0.4560(14) 0.028(7) Uiso 1 1 d . . . C50 C 0.2104(19) 0.4822(16) 0.5098(15) 0.033(8) Uiso 1 1 d . . . C51 C 0.2841(19) 0.4960(16) 0.5500(15) 0.034(8) Uiso 1 1 d . . . C52 C 0.343(2) 0.5212(17) 0.5316(16) 0.040(8) Uiso 1 1 d . . . C53 C 0.3962(19) 0.5724(17) 0.5737(15) 0.035(8) Uiso 1 1 d . . . C54 C 0.4190(19) 0.6227(16) 0.5432(15) 0.034(8) Uiso 1 1 d . . . C55 C 0.3857(18) 0.6037(16) 0.4847(14) 0.030(7) Uiso 1 1 d . . . C56 C 0.3622(19) 0.6548(16) 0.4607(15) 0.033(8) Uiso 1 1 d . . . C57 C 0.2891(19) 0.6450(16) 0.4196(15) 0.034(8) Uiso 1 1 d . . . C58 C 0.252(2) 0.7166(17) 0.4328(16) 0.039(8) Uiso 1 1 d . . . C59 C 0.1726(18) 0.7207(16) 0.4340(14) 0.030(7) Uiso 1 1 d . . . C60 C 0.1228(19) 0.6581(16) 0.4242(15) 0.034(8) Uiso 1 1 d . . . C61 C 0.064(2) 0.6756(18) 0.4643(16) 0.040(8) Uiso 1 1 d . . . C62 C 0.0403(19) 0.6277(17) 0.4906(15) 0.036(8) Uiso 1 1 d . . . C63 C 0.079(2) 0.5557(19) 0.4833(17) 0.048(10) Uiso 1 1 d . . . C64 C 0.086(2) 0.5320(17) 0.5360(16) 0.039(8) Uiso 1 1 d . . . C65 C 0.1502(19) 0.5036(16) 0.5493(15) 0.034(8) Uiso 1 1 d . . . C66 C 0.1891(17) 0.5204(15) 0.6123(14) 0.026(7) Uiso 1 1 d . . . C67 C 0.2682(19) 0.5169(16) 0.6112(15) 0.033(8) Uiso 1 1 d . . . C68 C 0.322(2) 0.5674(18) 0.6539(16) 0.044(9) Uiso 1 1 d . . . C69 C 0.384(2) 0.5921(18) 0.6326(16) 0.041(9) Uiso 1 1 d . . . C70 C 0.395(2) 0.668(2) 0.6674(18) 0.054(10) Uiso 1 1 d . . . C71 C 0.419(2) 0.717(2) 0.6411(18) 0.055(10) Uiso 1 1 d . . . C72 C 0.434(2) 0.6934(18) 0.5769(16) 0.042(9) Uiso 1 1 d . . . C73 C 0.410(2) 0.7481(19) 0.5493(17) 0.046(9) Uiso 1 1 d . . . C74 C 0.3697(17) 0.7302(15) 0.4938(14) 0.027(7) Uiso 1 1 d . . . C75 C 0.306(2) 0.7647(18) 0.4770(16) 0.041(9) Uiso 1 1 d . . . C76 C 0.277(2) 0.8218(18) 0.5215(16) 0.044(9) Uiso 1 1 d . . . C77 C 0.1919(18) 0.8267(16) 0.5202(14) 0.031(7) Uiso 1 1 d . . . C78 C 0.142(2) 0.7773(19) 0.4799(17) 0.048(9) Uiso 1 1 d . . . C79 C 0.077(2) 0.7507(18) 0.4982(16) 0.042(9) Uiso 1 1 d . . . C80 C 0.062(2) 0.7707(18) 0.5570(16) 0.040(9) Uiso 1 1 d . . . C81 C 0.039(2) 0.721(2) 0.5894(19) 0.057(11) Uiso 1 1 d . . . C82 C 0.0271(19) 0.6490(16) 0.5568(15) 0.033(8) Uiso 1 1 d . . . C83 C 0.050(2) 0.5938(17) 0.5812(16) 0.039(8) Uiso 1 1 d . . . C84 C 0.087(2) 0.6134(18) 0.6433(17) 0.044(9) Uiso 1 1 d . . . C85 C 0.155(2) 0.5769(18) 0.6584(16) 0.043(9) Uiso 1 1 d . . . C86 C 0.208(2) 0.6271(18) 0.7016(16) 0.044(9) Uiso 1 1 d . . . C87 C 0.285(2) 0.6210(19) 0.6994(17) 0.046(9) Uiso 1 1 d . . . C88 C 0.332(2) 0.6818(18) 0.7073(16) 0.040(8) Uiso 1 1 d . . . C89 C 0.3005(19) 0.7496(16) 0.7219(15) 0.034(8) Uiso 1 1 d . . . C90 C 0.3269(18) 0.8025(16) 0.6906(14) 0.030(7) Uiso 1 1 d . . . C91 C 0.385(2) 0.7853(18) 0.6517(17) 0.044(9) Uiso 1 1 d . . . C92 C 0.378(2) 0.8044(17) 0.5988(15) 0.038(8) Uiso 1 1 d . . . C93 C 0.3130(19) 0.8414(16) 0.5818(15) 0.035(8) Uiso 1 1 d . . . C94 C 0.2518(18) 0.8580(16) 0.6236(14) 0.030(7) Uiso 1 1 d . . . C95 C 0.2574(19) 0.8387(16) 0.6759(15) 0.035(8) Uiso 1 1 d . . . C96 C 0.192(2) 0.8102(17) 0.6960(15) 0.038(8) Uiso 1 1 d . . . C97 C 0.218(2) 0.7556(17) 0.7260(15) 0.037(8) Uiso 1 1 d . . . C98 C 0.171(2) 0.6957(18) 0.7129(16) 0.043(9) Uiso 1 1 d . . . C99 C 0.1000(19) 0.6866(17) 0.6776(15) 0.036(8) Uiso 1 1 d . . . C100 C 0.071(2) 0.739(2) 0.6503(18) 0.054(10) Uiso 1 1 d . . . C101 C 0.124(2) 0.8026(18) 0.6595(17) 0.044(9) Uiso 1 1 d . . . C102 C 0.1156(19) 0.8204(16) 0.6049(15) 0.034(8) Uiso 1 1 d . . . C103 C 0.180(2) 0.851(2) 0.5847(18) 0.053(10) Uiso 1 1 d . . . C104 C 0.811(2) 1.1141(17) 0.8439(16) 0.039(8) Uiso 1 1 d . . . C105 C 0.839(2) 1.101(2) 0.8978(17) 0.052(10) Uiso 1 1 d . . . H105 H 0.8374 1.0548 0.9005 0.062 Uiso 1 1 calc R . . C106 C 0.869(3) 1.156(3) 0.949(3) 0.096(17) Uiso 1 1 d . . . H106 H 0.8843 1.1449 0.9852 0.115 Uiso 1 1 calc R . . C107 C 0.878(3) 1.223(3) 0.948(3) 0.100(18) Uiso 1 1 d . . . H107 H 0.9012 1.2579 0.9813 0.120 Uiso 1 1 calc R . . C108 C 0.851(3) 1.240(3) 0.896(2) 0.091(16) Uiso 1 1 d . . . H108 H 0.8525 1.2869 0.8960 0.109 Uiso 1 1 calc R . . C109 C 0.818(2) 1.186(2) 0.840(2) 0.060(11) Uiso 1 1 d . . . H109 H 0.8030 1.1982 0.8043 0.071 Uiso 1 1 calc R . . C110 C 0.872(2) 1.0062(17) 0.7572(19) 0.053(11) Uani 1 1 d . . . C111 C 0.933(2) 1.048(2) 0.7661(18) 0.056(11) Uiso 1 1 d . . . H111 H 0.9278 1.0960 0.7838 0.067 Uiso 1 1 calc R . . C112 C 1.005(3) 1.025(2) 0.751(2) 0.072(13) Uiso 1 1 d . . . H112 H 1.0473 1.0556 0.7597 0.086 Uiso 1 1 calc R . . C113 C 1.011(4) 0.953(3) 0.721(2) 0.097(19) Uani 1 1 d . . . H113 H 1.0562 0.9362 0.7042 0.117 Uiso 1 1 calc R . . C114 C 0.954(3) 0.910(3) 0.717(2) 0.071(13) Uani 1 1 d . . . H114 H 0.9620 0.8620 0.7038 0.085 Uiso 1 1 calc R . . C115 C 0.878(2) 0.934(2) 0.7323(17) 0.052(11) Uani 1 1 d . . . H115 H 0.8356 0.9023 0.7259 0.063 Uiso 1 1 calc R . . C116 C 0.7392(17) 1.0903(15) 0.7230(14) 0.025(7) Uiso 1 1 d . . . C117 C 0.6822(18) 1.1374(14) 0.7479(14) 0.030(8) Uani 1 1 d . . . H117 H 0.6676 1.1380 0.7856 0.036 Uiso 1 1 calc R . . C118 C 0.6471(19) 1.1832(16) 0.7173(14) 0.033(8) Uani 1 1 d . . . H118 H 0.6086 1.2129 0.7340 0.039 Uiso 1 1 calc R . . C119 C 0.670(2) 1.1838(15) 0.6629(17) 0.040(9) Uani 1 1 d . . . H119 H 0.6487 1.2152 0.6427 0.048 Uiso 1 1 calc R . . C120 C 0.726(2) 1.1371(16) 0.6378(16) 0.043(9) Uani 1 1 d . . . H120 H 0.7394 1.1371 0.5999 0.052 Uiso 1 1 calc R . . C121 C 0.7620(16) 1.0903(16) 0.6665(15) 0.031(7) Uani 1 1 d . . . C122 C 0.821(2) 1.0434(15) 0.6321(15) 0.035(7) Uani 1 1 d . . . H122 H 0.8528 1.0233 0.6602 0.042 Uiso 1 1 calc R . . C123 C 0.916(2) 1.1421(19) 0.6481(18) 0.054(11) Uani 1 1 d . . . H12A H 0.8811 1.1760 0.6692 0.081 Uiso 1 1 calc R . . H12B H 0.9475 1.1644 0.6267 0.081 Uiso 1 1 calc R . . H12C H 0.9477 1.1245 0.6767 0.081 Uiso 1 1 calc R . . C124 C 0.9191(17) 1.0301(16) 0.5703(15) 0.036(9) Uani 1 1 d . . . H12D H 0.9544 1.0110 0.5965 0.044 Uiso 1 1 calc R . . H12E H 0.9483 1.0495 0.5447 0.044 Uiso 1 1 calc R . . C125 C 0.8577(19) 0.9722(16) 0.5314(15) 0.034(8) Uiso 1 1 d . . . C126 C 0.7878(17) 0.9810(15) 0.5754(14) 0.027(7) Uiso 1 1 d . . . C127 C 0.7664(18) 0.9154(16) 0.5900(14) 0.031(7) Uiso 1 1 d . . . C128 C 0.6806(18) 0.9060(15) 0.5884(14) 0.029(7) Uiso 1 1 d . . . C129 C 0.6524(19) 0.9589(16) 0.5575(15) 0.035(8) Uiso 1 1 d . . . C130 C 0.7088(18) 0.9962(16) 0.5417(14) 0.030(7) Uiso 1 1 d . . . C131 C 0.703(2) 1.0137(18) 0.4899(16) 0.042(9) Uiso 1 1 d . . . C132 C 0.7699(18) 1.0055(16) 0.4521(14) 0.031(7) Uiso 1 1 d . . . C133 C 0.838(2) 0.9793(18) 0.4698(16) 0.040(9) Uiso 1 1 d . . . C134 C 0.876(2) 0.9283(18) 0.4260(16) 0.041(9) Uiso 1 1 d . . . C135 C 0.913(2) 0.8807(19) 0.4557(17) 0.047(9) Uiso 1 1 d . . . C136 C 0.8907(18) 0.8950(16) 0.5144(14) 0.031(7) Uiso 1 1 d . . . C137 C 0.8727(19) 0.8463(17) 0.5429(15) 0.036(8) Uiso 1 1 d . . . C138 C 0.806(2) 0.8536(17) 0.5823(15) 0.038(8) Uiso 1 1 d . . . C139 C 0.7716(18) 0.7840(16) 0.5661(14) 0.031(7) Uiso 1 1 d . . . C140 C 0.687(2) 0.780(2) 0.5656(17) 0.049(10) Uiso 1 1 d . . . C141 C 0.6479(19) 0.8439(17) 0.5767(15) 0.036(8) Uiso 1 1 d . . . C142 C 0.578(2) 0.8257(19) 0.5369(17) 0.047(9) Uiso 1 1 d . . . C143 C 0.544(2) 0.8734(18) 0.5089(17) 0.045(9) Uiso 1 1 d . . . C144 C 0.5807(19) 0.9412(16) 0.5179(15) 0.033(8) Uiso 1 1 d . . . C145 C 0.569(2) 0.9608(18) 0.4629(16) 0.042(9) Uiso 1 1 d . . . C146 C 0.533(2) 0.9032(18) 0.4138(16) 0.041(9) Uiso 1 1 d . . . C147 C 0.5490(19) 0.8859(16) 0.3583(15) 0.035(8) Uiso 1 1 d . . . C148 C 0.613(2) 0.9214(19) 0.3417(17) 0.046(9) Uiso 1 1 d . . . C149 C 0.646(2) 0.9754(18) 0.3868(16) 0.040(8) Uiso 1 1 d . . . C150 C 0.6322(18) 0.9949(16) 0.4484(14) 0.030(7) Uiso 1 1 d . . . C151 C 0.7370(18) 0.9830(15) 0.3919(14) 0.028(7) Uiso 1 1 d . . . C152 C 0.774(3) 0.938(2) 0.347(2) 0.064(12) Uiso 1 1 d . . . C153 C 0.848(2) 0.9084(18) 0.3674(16) 0.042(9) Uiso 1 1 d . . . C154 C 0.850(2) 0.832(2) 0.3302(18) 0.051(10) Uiso 1 1 d . . . C155 C 0.879(2) 0.7837(18) 0.3589(16) 0.040(9) Uiso 1 1 d . . . C156 C 0.9114(19) 0.8062(16) 0.4215(15) 0.034(8) Uiso 1 1 d . . . C157 C 0.8945(19) 0.7519(17) 0.4503(15) 0.036(8) Uiso 1 1 d . . . C158 C 0.876(2) 0.7716(19) 0.5068(17) 0.048(10) Uiso 1 1 d . . . C159 C 0.813(2) 0.7355(18) 0.5271(17) 0.045(9) Uiso 1 1 d . . . C160 C 0.770(2) 0.6803(17) 0.4809(16) 0.039(8) Uiso 1 1 d . . . C161 C 0.647(2) 0.7199(19) 0.5206(17) 0.046(9) Uiso 1 1 d . . . C162 C 0.852(2) 0.6962(18) 0.4028(16) 0.041(9) Uiso 1 1 d . . . C163 C 0.793(2) 0.6622(17) 0.4198(16) 0.039(8) Uiso 1 1 d . . . C164 C 0.689(2) 0.6738(17) 0.4777(15) 0.037(8) Uiso 1 1 d . . . C165 C 0.8442(19) 0.7146(17) 0.3460(15) 0.037(8) Uiso 1 1 d . . . C166 C 0.774(2) 0.6985(19) 0.3081(17) 0.045(9) Uiso 1 1 d . . . C167 C 0.741(2) 0.748(2) 0.2795(18) 0.055(10) Uiso 1 1 d . . . C168 C 0.776(2) 0.8140(19) 0.2878(17) 0.046(9) Uiso 1 1 d . . . C169 C 0.729(2) 0.8804(19) 0.2993(17) 0.047(9) Uiso 1 1 d . . . C170 C 0.648(2) 0.8724(18) 0.2988(16) 0.044(9) Uiso 1 1 d . . . C171 C 0.614(2) 0.8049(18) 0.2867(16) 0.040(8) Uiso 1 1 d . . . C172 C 0.551(2) 0.8147(19) 0.3239(17) 0.046(9) Uiso 1 1 d . . . C173 C 0.532(2) 0.7613(18) 0.3501(16) 0.041(9) Uiso 1 1 d . . . C174 C 0.579(2) 0.6976(18) 0.3409(16) 0.041(9) Uiso 1 1 d . . . C175 C 0.6399(19) 0.6913(17) 0.3059(15) 0.036(8) Uiso 1 1 d . . . C176 C 0.6587(19) 0.7419(16) 0.2762(15) 0.035(8) Uiso 1 1 d . . . C177 C 0.709(2) 0.6602(17) 0.3222(16) 0.039(8) Uiso 1 1 d . . . C178 C 0.722(2) 0.6440(17) 0.3782(16) 0.040(8) Uiso 1 1 d . . . C179 C 0.657(2) 0.6518(18) 0.4159(16) 0.043(9) Uiso 1 1 d . . . C180 C 0.5866(19) 0.6772(17) 0.3979(15) 0.035(8) Uiso 1 1 d . . . C181 C 0.549(2) 0.7284(18) 0.4421(17) 0.043(9) Uiso 1 1 d . . . C182 C 0.5759(19) 0.7494(16) 0.5015(15) 0.033(8) Uiso 1 1 d . . . C183 C 0.513(2) 0.7808(17) 0.4106(16) 0.038(8) Uiso 1 1 d . . . C184 C 0.511(2) 0.8497(18) 0.4450(16) 0.042(9) Uiso 1 1 d . . . N1 N 0.3428(15) 0.4160(13) 0.3965(13) 0.037(7) Uani 1 1 d . . . N2 N 0.8709(14) 1.0830(13) 0.6050(12) 0.030(6) Uani 1 1 d . . . O1 O 0.1550(19) 0.6782(17) 0.2918(15) 0.082(9) Uiso 1 1 d . . . O2 O 0.0244(18) 0.5045(16) 0.3101(14) 0.073(9) Uiso 1 1 d . . . O3 O 0.1847(17) 0.5838(15) 0.1093(14) 0.075(9) Uiso 1 1 d . . . O4 O -0.0788(18) 0.3969(16) 0.2160(15) 0.078(9) Uiso 1 1 d . . . O5 O 0.0487(17) 0.2921(15) 0.0758(13) 0.068(8) Uiso 1 1 d . . . O6 O 0.0867(16) 0.4708(14) 0.0206(13) 0.063(8) Uiso 1 1 d . . . O7 O -0.158(2) 0.4190(17) 0.0365(15) 0.081(9) Uiso 1 1 d . . . O8 O 0.0339(17) 0.6238(15) 0.0645(13) 0.066(8) Uiso 1 1 d . . . O9 O -0.196(3) 0.596(2) 0.0990(19) 0.112(13) Uiso 1 1 d . . . O10 O -0.011(2) 0.741(2) 0.2426(18) 0.106(12) Uiso 1 1 d . . . O11 O -0.1257(18) 0.5494(16) 0.2648(15) 0.076(9) Uiso 1 1 d . . . O12 O 0.7913(19) 0.9211(16) 0.8864(14) 0.076(9) Uiso 1 1 d . . . O13 O 0.7089(18) 0.8216(17) 0.7126(14) 0.078(9) Uiso 1 1 d . . . O14 O 0.5717(17) 0.9958(15) 0.6904(14) 0.066(8) Uiso 1 1 d . . . O15 O 0.563(2) 0.757(2) 0.7650(17) 0.103(12) Uiso 1 1 d . . . O16 O 0.4402(16) 0.9485(18) 0.7372(15) 0.117(13) Uiso 1 1 d . . . O17 O 0.414(3) 0.907(3) 0.911(2) 0.145(17) Uiso 1 1 d . . . O18 O 0.6536(18) 0.8817(16) 0.9404(15) 0.076(9) Uiso 1 1 d . . . O19 O 0.470(3) 1.083(2) 0.973(2) 0.121(14) Uiso 1 1 d . . . O20 O 0.716(3) 1.032(2) 0.985(2) 0.124(14) Uiso 1 1 d . . . O21 O 0.663(2) 1.210(2) 0.9254(18) 0.106(12) Uiso 1 1 d . . . O22 O 0.4961(18) 1.0983(16) 0.7873(14) 0.072(8) Uiso 1 1 d . . . P1 P 0.2020(5) 0.4562(4) 0.2219(4) 0.033(2) Uani 1 1 d . . . P2 P 0.7771(5) 1.0433(4) 0.7781(4) 0.031(2) Uani 1 1 d . . . Os1 Os 0.10201(9) 0.53495(7) 0.20830(6) 0.0390(4) Uani 1 1 d . . . Os2 Os -0.00685(9) 0.44111(7) 0.11644(7) 0.0422(4) Uani 1 1 d . . . Os3 Os -0.04231(9) 0.58771(8) 0.16757(7) 0.0495(4) Uani 1 1 d . . . Os4 Os 0.68055(9) 0.96564(7) 0.79414(7) 0.0402(4) Uani 1 1 d . . . Os5 Os 0.54908(10) 0.91284(9) 0.83766(9) 0.0600(5) Uani 1 1 d . . . Os6 Os 0.59745(9) 1.05955(8) 0.88719(7) 0.0487(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C29 0.045 0.06(3) 0.07(3) 0.01(2) 0.02(2) 0.00(2) C30 0.111 0.12(4) 0.09(4) 0.00(3) 0.05(3) -0.09(3) C31 0.04(3) 0.09(4) 0.10(4) 0.02(3) -0.04(3) -0.02(2) C32 0.13(5) 0.06(3) 0.08(4) -0.02(3) -0.03(3) -0.02(3) C33 0.08(4) 0.06(3) 0.17(6) 0.00(3) 0.03(4) -0.03(3) C34 0.05(2) 0.07(3) 0.04(2) 0.01(2) 0.016(19) -0.01(2) C35 0.020(16) 0.001(12) 0.06(2) 0.006(12) 0.008(15) 0.001(11) C36 0.04(2) 0.034(19) 0.08(3) 0.033(19) -0.01(2) -0.012(17) C37 0.03(2) 0.027(18) 0.10(4) 0.01(2) 0.02(2) -0.017(16) C38 0.05(2) 0.024(17) 0.05(3) 0.004(16) 0.00(2) -0.004(16) C39 0.05(2) 0.04(2) 0.02(2) -0.004(15) 0.020(17) 0.014(18) C40 0.04(2) 0.023(15) 0.016(18) -0.004(13) 0.003(15) 0.006(14) C41 0.04(2) 0.027(17) 0.04(2) -0.008(14) -0.003(16) 0.020(15) C42 0.04(2) 0.05(2) 0.05(3) 0.003(18) -0.003(18) 0.032(18) C43 0.03(2) 0.034(18) 0.04(2) -0.006(15) -0.017(16) 0.012(15) C110 0.04(2) 0.022(17) 0.08(3) 0.000(18) 0.00(2) 0.014(16) C113 0.09(4) 0.06(3) 0.10(4) -0.03(3) 0.00(3) 0.02(3) C114 0.06(3) 0.06(3) 0.09(4) 0.01(3) 0.01(3) 0.03(2) C115 0.05(3) 0.08(3) 0.05(3) 0.05(2) 0.02(2) 0.03(2) C117 0.04(2) 0.014(14) 0.03(2) 0.002(13) 0.009(15) -0.001(13) C118 0.04(2) 0.030(17) 0.02(2) 0.011(14) -0.019(16) -0.001(15) C119 0.05(2) 0.015(15) 0.06(3) 0.016(15) 0.007(19) 0.014(15) C120 0.06(3) 0.030(18) 0.04(2) 0.013(16) 0.013(19) 0.014(17) C121 0.012(15) 0.040 0.04(2) 0.006(14) -0.012(14) -0.012(13) C122 0.045 0.018(15) 0.04(2) 0.005(14) 0.021(17) 0.018(14) C123 0.04(2) 0.05(2) 0.07(3) 0.00(2) 0.02(2) -0.004(18) C124 0.018(17) 0.040(19) 0.04(2) -0.002(16) 0.006(15) -0.022(15) N1 0.020(15) 0.032(15) 0.06(2) 0.004(13) 0.022(14) 0.011(12) N2 0.016(14) 0.030(14) 0.044(18) 0.004(12) 0.018(12) -0.002(11) P1 0.027(5) 0.030(4) 0.040(6) 0.008(4) -0.004(4) -0.005(4) P2 0.026(5) 0.030(4) 0.033(5) 0.006(4) 0.002(4) 0.010(4) Os1 0.0449(9) 0.0337(7) 0.0359(9) 0.0068(6) 0.0001(7) -0.0009(6) Os2 0.0450(9) 0.0411(8) 0.0374(9) 0.0071(6) 0.0005(7) -0.0029(7) Os3 0.0499(10) 0.0456(9) 0.0496(11) 0.0091(7) 0.0014(8) 0.0071(7) Os4 0.0443(9) 0.0343(7) 0.0405(9) 0.0077(6) 0.0051(7) 0.0052(6) Os5 0.0576(11) 0.0537(10) 0.0693(13) 0.0153(8) 0.0155(9) -0.0040(8) Os6 0.0487(10) 0.0523(9) 0.0424(10) 0.0075(7) 0.0079(7) 0.0115(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.20(5) . ? C1 Os1 1.83(5) . ? C2 O2 1.12(4) . ? C2 Os1 1.93(4) . ? C3 O3 1.17(4) . ? C3 Os1 2.04(4) . ? C4 O4 1.15(4) . ? C4 Os2 1.91(4) . ? C5 O5 1.17(4) . ? C5 Os2 1.85(4) . ? C6 O6 1.15(4) . ? C6 Os2 1.91(4) . ? C7 O7 1.11(5) . ? C7 Os2 1.92(5) . ? C8 O8 1.17(4) . ? C8 Os3 1.92(4) . ? C9 O9 1.10(6) . ? C9 Os3 1.91(6) . ? C10 O10 1.18(6) . ? C10 Os3 1.87(6) . ? C11 O11 1.13(5) . ? C11 Os3 1.93(5) . ? C12 O12 1.13(4) . ? C12 Os4 1.92(4) . ? C13 O13 1.13(4) . ? C13 Os4 1.88(4) . ? C14 O14 1.11(4) . ? C14 Os4 1.99(3) . ? C15 O15 1.21(6) . ? C15 Os5 1.89(6) . ? C16 O16 1.0609 . ? C16 Os5 2.0309(19) . ? C17 O17 1.19(7) . ? C17 Os5 1.89(7) . ? C18 O18 1.12(4) . ? C18 Os5 1.93(4) . ? C19 O19 1.16(6) . ? C19 Os6 1.91(6) . ? C20 O20 1.13(5) . ? C20 Os6 1.96(5) . ? C21 O21 1.16(5) . ? C21 Os6 1.88(5) . ? C22 O22 1.08(4) . ? C22 Os6 1.96(4) . ? C23 C24 1.44(4) . ? C23 C28 1.45(5) . ? C23 P1 1.82(4) . ? C24 C25 1.39(5) . ? C24 H24 0.9300 . ? C25 C26 1.39(7) . ? C25 H25 0.9300 . ? C26 C27 1.33(6) . ? C26 H26 0.9300 . ? C27 C28 1.38(6) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C34 1.32(5) . ? C29 C30 1.40(7) . ? C29 P1 1.86(4) . ? C30 C31 1.44(6) . ? C30 H30 0.9300 . ? C31 C32 1.42(6) . ? C31 H31 0.9300 . ? C32 C33 1.33(7) . ? C32 H32 0.9300 . ? C33 C34 1.43(6) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C40 1.42(4) . ? C35 C36 1.42(4) . ? C35 P1 1.84(3) . ? C36 C37 1.35(5) . ? C36 H36 0.9300 . ? C37 C38 1.34(5) . ? C37 H37 0.9300 . ? C38 C39 1.38(5) . ? C38 H38 0.9300 . ? C39 C40 1.37(5) . ? C39 H39 0.9300 . ? C40 C41 1.50(4) . ? C41 N1 1.51(4) . ? C41 C45 1.59(4) . ? C41 H41 0.9800 . ? C42 N1 1.53(4) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 N1 1.49(4) . ? C43 C44 1.55(4) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.55(4) . ? C44 C55 1.55(4) . ? C44 C52 1.59(5) . ? C45 C49 1.46(4) . ? C45 C46 1.54(4) . ? C46 C47 1.35(4) . ? C46 C57 1.40(4) . ? C47 C60 1.42(4) . ? C47 C48 1.48(4) . ? C48 C63 1.39(5) . ? C48 C49 1.47(4) . ? C49 C50 1.40(4) . ? C50 C65 1.45(5) . ? C50 C51 1.49(4) . ? C51 C52 1.29(4) . ? C51 C67 1.42(4) . ? C52 C53 1.45(5) . ? C53 C69 1.35(5) . ? C53 C54 1.44(4) . ? C54 C55 1.37(4) . ? C54 C72 1.40(5) . ? C55 C56 1.32(4) . ? C56 C74 1.47(4) . ? C56 C57 1.49(5) . ? C57 C58 1.52(4) . ? C58 C59 1.38(5) . ? C58 C75 1.45(5) . ? C59 C78 1.45(5) . ? C59 C60 1.46(4) . ? C60 C61 1.42(5) . ? C61 C62 1.34(5) . ? C61 C79 1.47(5) . ? C62 C82 1.51(5) . ? C62 C63 1.54(5) . ? C63 C64 1.42(5) . ? C64 C65 1.29(4) . ? C64 C83 1.54(5) . ? C65 C66 1.49(4) . ? C66 C67 1.38(4) . ? C66 C85 1.48(4) . ? C67 C68 1.46(5) . ? C68 C69 1.37(5) . ? C68 C87 1.46(5) . ? C69 C70 1.48(5) . ? C70 C71 1.35(5) . ? C70 C88 1.48(5) . ? C71 C91 1.44(5) . ? C71 C72 1.48(5) . ? C72 C73 1.44(5) . ? C73 C74 1.36(5) . ? C73 C92 1.51(5) . ? C74 C75 1.39(4) . ? C75 C76 1.42(5) . ? C76 C93 1.42(5) . ? C76 C77 1.49(5) . ? C77 C78 1.38(5) . ? C77 C103 1.47(5) . ? C78 C79 1.40(5) . ? C79 C80 1.36(5) . ? C80 C81 1.47(5) . ? C80 C102 1.50(5) . ? C81 C82 1.41(5) . ? C81 C100 1.41(5) . ? C82 C83 1.40(5) . ? C83 C84 1.46(5) . ? C84 C99 1.44(5) . ? C84 C85 1.44(5) . ? C85 C86 1.45(5) . ? C86 C87 1.35(5) . ? C86 C98 1.46(5) . ? C87 C88 1.41(5) . ? C88 C89 1.41(4) . ? C89 C97 1.46(5) . ? C89 C90 1.52(4) . ? C90 C91 1.40(5) . ? C90 C95 1.46(4) . ? C91 C92 1.37(5) . ? C92 C93 1.43(5) . ? C93 C94 1.48(5) . ? C94 C95 1.36(4) . ? C94 C103 1.45(5) . ? C95 C96 1.44(5) . ? C96 C101 1.37(5) . ? C96 C97 1.48(5) . ? C97 C98 1.37(5) . ? C98 C99 1.40(5) . ? C99 C100 1.43(5) . ? C100 C101 1.50(5) . ? C101 C102 1.40(5) . ? C102 C103 1.45(5) . ? C104 C105 1.38(5) . ? C104 C109 1.46(5) . ? C104 P2 1.80(3) . ? C105 C106 1.43(6) . ? C105 H105 0.9300 . ? C106 C107 1.34(7) . ? C106 H106 0.9300 . ? C107 C108 1.37(7) . ? C107 H107 0.9300 . ? C108 C109 1.49(6) . ? C108 H108 0.9300 . ? C109 H109 0.9300 . ? C110 C111 1.31(5) . ? C110 C115 1.39(5) . ? C110 P2 1.86(4) . ? C111 C112 1.37(6) . ? C111 H111 0.9300 . ? C112 C113 1.40(6) . ? C112 H112 0.9300 . ? C113 C114 1.28(7) . ? C113 H113 0.9300 . ? C114 C115 1.45(5) . ? C114 H114 0.9300 . ? C115 H115 0.9300 . ? C116 C121 1.40(4) . ? C116 C117 1.41(4) . ? C116 P2 1.85(3) . ? C117 C118 1.40(4) . ? C117 H117 0.9300 . ? C118 C119 1.36(5) . ? C118 H118 0.9300 . ? C119 C120 1.39(5) . ? C119 H119 0.9300 . ? C120 C121 1.40(4) . ? C120 H120 0.9300 . ? C121 C122 1.51(4) . ? C122 N2 1.46(4) . ? C122 C126 1.58(4) . ? C122 H122 0.9800 . ? C123 N2 1.47(4) . ? C123 H12A 0.9600 . ? C123 H12B 0.9600 . ? C123 H12C 0.9600 . ? C124 N2 1.45(4) . ? C124 C125 1.58(4) . ? C124 H12D 0.9700 . ? C124 H12E 0.9700 . ? C125 C133 1.48(5) . ? C125 C136 1.58(4) . ? C125 C126 1.64(4) . ? C126 C127 1.48(4) . ? C126 C130 1.58(4) . ? C127 C138 1.38(4) . ? C127 C128 1.50(4) . ? C128 C141 1.29(4) . ? C128 C129 1.48(4) . ? C129 C130 1.36(4) . ? C129 C144 1.45(4) . ? C130 C131 1.33(4) . ? C131 C150 1.46(5) . ? C131 C132 1.51(5) . ? C132 C133 1.36(5) . ? C132 C151 1.40(4) . ? C133 C134 1.43(5) . ? C134 C153 1.34(5) . ? C134 C135 1.43(5) . ? C135 C136 1.40(5) . ? C135 C156 1.46(5) . ? C136 C137 1.36(4) . ? C137 C158 1.48(5) . ? C137 C138 1.53(5) . ? C138 C139 1.43(4) . ? C139 C159 1.38(5) . ? C139 C140 1.47(5) . ? C140 C141 1.41(5) . ? C140 C161 1.46(5) . ? C141 C142 1.44(5) . ? C142 C143 1.38(5) . ? C142 C182 1.49(5) . ? C143 C144 1.43(5) . ? C143 C184 1.48(5) . ? C144 C145 1.42(5) . ? C145 C150 1.41(5) . ? C145 C146 1.45(5) . ? C146 C147 1.29(4) . ? C146 C184 1.50(5) . ? C147 C172 1.41(5) . ? C147 C148 1.45(5) . ? C148 C149 1.35(5) . ? C148 C170 1.37(5) . ? C149 C150 1.41(5) . ? C149 C151 1.59(4) . ? C151 C152 1.38(5) . ? C152 C169 1.49(5) . ? C152 C153 1.50(5) . ? C153 C154 1.52(5) . ? C154 C155 1.37(5) . ? C154 C168 1.51(5) . ? C155 C165 1.43(5) . ? C155 C156 1.45(5) . ? C156 C157 1.45(4) . ? C157 C158 1.33(5) . ? C157 C162 1.46(5) . ? C158 C159 1.49(5) . ? C159 C160 1.44(5) . ? C160 C164 1.42(5) . ? C160 C163 1.45(5) . ? C161 C164 1.40(5) . ? C161 C182 1.46(5) . ? C162 C163 1.38(5) . ? C162 C165 1.45(5) . ? C163 C178 1.46(5) . ? C164 C179 1.43(5) . ? C165 C166 1.41(5) . ? C166 C167 1.42(5) . ? C166 C177 1.47(5) . ? C167 C168 1.39(5) . ? C167 C176 1.43(5) . ? C168 C169 1.52(5) . ? C169 C170 1.42(5) . ? C170 C171 1.40(5) . ? C171 C172 1.44(5) . ? C171 C176 1.44(5) . ? C172 C173 1.41(5) . ? C173 C183 1.42(5) . ? C173 C174 1.48(5) . ? C174 C175 1.38(5) . ? C174 C180 1.48(5) . ? C175 C176 1.41(4) . ? C175 C177 1.42(5) . ? C177 C178 1.42(5) . ? C178 C179 1.48(5) . ? C179 C180 1.39(5) . ? C180 C181 1.43(5) . ? C181 C182 1.36(5) . ? C181 C183 1.52(5) . ? C183 C184 1.37(5) . ? P1 Os1 2.387(9) . ? P2 Os4 2.395(9) . ? Os1 Os3 2.892(2) . ? Os1 Os2 2.922(2) . ? Os2 Os3 2.889(2) . ? Os4 Os5 2.894(2) . ? Os4 Os6 2.923(2) . ? Os5 Os6 2.884(2) . ? 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 O1 C1 Os1 174(4) . . ? O2 C2 Os1 168(3) . . ? O3 C3 Os1 164(3) . . ? O4 C4 Os2 174(4) . . ? O5 C5 Os2 174(3) . . ? O6 C6 Os2 177(3) . . ? O7 C7 Os2 176(5) . . ? O8 C8 Os3 175(3) . . ? O9 C9 Os3 174(5) . . ? O10 C10 Os3 177(5) . . ? O11 C11 Os3 175(4) . . ? O12 C12 Os4 173(3) . . ? O13 C13 Os4 171(3) . . ? O14 C14 Os4 174(3) . . ? O15 C15 Os5 168(5) . . ? O16 C16 Os5 173.27(5) . . ? O17 C17 Os5 168(6) . . ? O18 C18 Os5 177(4) . . ? O19 C19 Os6 178(5) . . ? O20 C20 Os6 169(4) . . ? O21 C21 Os6 177(4) . . ? O22 C22 Os6 178(3) . . ? C24 C23 C28 116(3) . . ? C24 C23 P1 119(2) . . ? C28 C23 P1 122(3) . . ? C25 C24 C23 119(3) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C24 C25 C26 122(5) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C27 C26 C25 120(5) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 122(5) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C27 C28 C23 120(4) . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? C34 C29 C30 120(4) . . ? C34 C29 P1 125(3) . . ? C30 C29 P1 115(3) . . ? C29 C30 C31 122(5) . . ? C29 C30 H30 118.9 . . ? C31 C30 H30 118.9 . . ? C32 C31 C30 111(5) . . ? C32 C31 H31 124.3 . . ? C30 C31 H31 124.3 . . ? C33 C32 C31 128(5) . . ? C33 C32 H32 115.8 . . ? C31 C32 H32 115.8 . . ? C32 C33 C34 115(5) . . ? C32 C33 H33 122.3 . . ? C34 C33 H33 122.3 . . ? C29 C34 C33 123(4) . . ? C29 C34 H34 118.7 . . ? C33 C34 H34 118.7 . . ? C40 C35 C36 114(3) . . ? C40 C35 P1 135(2) . . ? C36 C35 P1 111(3) . . ? C37 C36 C35 125(4) . . ? C37 C36 H36 117.7 . . ? C35 C36 H36 117.7 . . ? C38 C37 C36 119(3) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C39 119(3) . . ? C37 C38 H38 120.5 . . ? C39 C38 H38 120.5 . . ? C40 C39 C38 123(3) . . ? C40 C39 H39 118.7 . . ? C38 C39 H39 118.7 . . ? C39 C40 C35 120(3) . . ? C39 C40 C41 117(3) . . ? C35 C40 C41 123(3) . . ? C40 C41 N1 111(3) . . ? C40 C41 C45 116(3) . . ? N1 C41 C45 100(2) . . ? C40 C41 H41 109.6 . . ? N1 C41 H41 109.6 . . ? C45 C41 H41 109.6 . . ? N1 C42 H42A 109.5 . . ? N1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N1 C43 C44 100(2) . . ? N1 C43 H43A 111.7 . . ? C44 C43 H43A 111.7 . . ? N1 C43 H43B 111.7 . . ? C44 C43 H43B 111.7 . . ? H43A C43 H43B 109.5 . . ? C45 C44 C43 106(2) . . ? C45 C44 C55 116(2) . . ? C43 C44 C55 111(3) . . ? C45 C44 C52 115(2) . . ? C43 C44 C52 111(3) . . ? C55 C44 C52 97(2) . . ? C49 C45 C46 100(2) . . ? C49 C45 C44 113(2) . . ? C46 C45 C44 115(2) . . ? C49 C45 C41 112(2) . . ? C46 C45 C41 114(2) . . ? C44 C45 C41 103(2) . . ? C47 C46 C57 122(3) . . ? C47 C46 C45 112(3) . . ? C57 C46 C45 120(3) . . ? C46 C47 C60 125(3) . . ? C46 C47 C48 108(3) . . ? C60 C47 C48 116(3) . . ? C63 C48 C49 120(3) . . ? C63 C48 C47 123(3) . . ? C49 C48 C47 105(3) . . ? C50 C49 C45 126(3) . . ? C50 C49 C48 117(3) . . ? C45 C49 C48 111(3) . . ? C49 C50 C65 118(3) . . ? C49 C50 C51 119(3) . . ? C65 C50 C51 106(3) . . ? C52 C51 C67 122(3) . . ? C52 C51 C50 118(3) . . ? C67 C51 C50 110(3) . . ? C51 C52 C53 121(3) . . ? C51 C52 C44 125(3) . . ? C53 C52 C44 109(3) . . ? C69 C53 C54 122(3) . . ? C69 C53 C52 118(3) . . ? C54 C53 C52 108(3) . . ? C55 C54 C72 123(3) . . ? C55 C54 C53 110(3) . . ? C72 C54 C53 119(3) . . ? C56 C55 C54 118(3) . . ? C56 C55 C44 123(3) . . ? C54 C55 C44 113(3) . . ? C55 C56 C74 123(3) . . ? C55 C56 C57 120(3) . . ? C74 C56 C57 107(3) . . ? C46 C57 C56 122(3) . . ? C46 C57 C58 116(3) . . ? C56 C57 C58 106(3) . . ? C59 C58 C75 123(3) . . ? C59 C58 C57 120(3) . . ? C75 C58 C57 106(3) . . ? C58 C59 C78 119(3) . . ? C58 C59 C60 122(3) . . ? C78 C59 C60 107(3) . . ? C47 C60 C61 123(3) . . ? C47 C60 C59 115(3) . . ? C61 C60 C59 108(3) . . ? C62 C61 C60 120(3) . . ? C62 C61 C79 121(3) . . ? C60 C61 C79 107(3) . . ? C61 C62 C82 121(3) . . ? C61 C62 C63 122(3) . . ? C82 C62 C63 102(3) . . ? C48 C63 C64 121(3) . . ? C48 C63 C62 116(3) . . ? C64 C63 C62 115(3) . . ? C65 C64 C63 118(3) . . ? C65 C64 C83 123(3) . . ? C63 C64 C83 101(3) . . ? C64 C65 C50 125(3) . . ? C64 C65 C66 122(3) . . ? C50 C65 C66 106(3) . . ? C67 C66 C85 120(3) . . ? C67 C66 C65 110(3) . . ? C85 C66 C65 117(3) . . ? C66 C67 C51 108(3) . . ? C66 C67 C68 123(3) . . ? C51 C67 C68 117(3) . . ? C69 C68 C67 119(3) . . ? C69 C68 C87 115(3) . . ? C67 C68 C87 114(3) . . ? C53 C69 C68 123(3) . . ? C53 C69 C70 119(3) . . ? C68 C69 C70 106(3) . . ? C71 C70 C88 121(4) . . ? C71 C70 C69 121(4) . . ? C88 C70 C69 105(3) . . ? C70 C71 C91 122(4) . . ? C70 C71 C72 119(4) . . ? C91 C71 C72 107(3) . . ? C54 C72 C73 118(3) . . ? C54 C72 C71 120(3) . . ? C73 C72 C71 108(3) . . ? C74 C73 C72 119(3) . . ? C74 C73 C92 118(3) . . ? C72 C73 C92 105(3) . . ? C73 C74 C75 125(3) . . ? C73 C74 C56 118(3) . . ? C75 C74 C56 109(3) . . ? C74 C75 C76 118(3) . . ? C74 C75 C58 112(3) . . ? C76 C75 C58 120(3) . . ? C93 C76 C75 120(3) . . ? C93 C76 C77 111(3) . . ? C75 C76 C77 117(3) . . ? C78 C77 C103 121(3) . . ? C78 C77 C76 122(3) . . ? C103 C77 C76 103(3) . . ? C77 C78 C79 122(3) . . ? C77 C78 C59 120(3) . . ? C79 C78 C59 108(3) . . ? C80 C79 C78 121(3) . . ? C80 C79 C61 118(3) . . ? C78 C79 C61 109(3) . . ? C79 C80 C81 124(3) . . ? C79 C80 C102 122(3) . . ? C81 C80 C102 101(3) . . ? C82 C81 C100 120(4) . . ? C82 C81 C80 118(3) . . ? C100 C81 C80 112(3) . . ? C83 C82 C81 123(3) . . ? C83 C82 C62 108(3) . . ? C81 C82 C62 118(3) . . ? C82 C83 C84 117(3) . . ? C82 C83 C64 114(3) . . ? C84 C83 C64 116(3) . . ? C99 C84 C85 106(3) . . ? C99 C84 C83 121(3) . . ? C85 C84 C83 120(3) . . ? C84 C85 C86 109(3) . . ? C84 C85 C66 122(3) . . ? C86 C85 C66 117(3) . . ? C87 C86 C85 120(3) . . ? C87 C86 C98 122(3) . . ? C85 C86 C98 106(3) . . ? C86 C87 C88 120(3) . . ? C86 C87 C68 125(3) . . ? C88 C87 C68 103(3) . . ? C87 C88 C89 120(3) . . ? C87 C88 C70 112(3) . . ? C89 C88 C70 119(3) . . ? C88 C89 C97 119(3) . . ? C88 C89 C90 118(3) . . ? C97 C89 C90 109(3) . . ? C91 C90 C95 122(3) . . ? C91 C90 C89 120(3) . . ? C95 C90 C89 106(3) . . ? C92 C91 C90 119(3) . . ? C92 C91 C71 109(3) . . ? C90 C91 C71 119(3) . . ? C91 C92 C93 122(3) . . ? C91 C92 C73 110(3) . . ? C93 C92 C73 117(3) . . ? C76 C93 C92 121(3) . . ? C76 C93 C94 109(3) . . ? C92 C93 C94 117(3) . . ? C95 C94 C103 122(3) . . ? C95 C94 C93 121(3) . . ? C103 C94 C93 105(3) . . ? C94 C95 C96 122(3) . . ? C94 C95 C90 118(3) . . ? C96 C95 C90 109(3) . . ? C101 C96 C95 117(3) . . ? C101 C96 C97 121(3) . . ? C95 C96 C97 110(3) . . ? C98 C97 C89 120(3) . . ? C98 C97 C96 116(3) . . ? C89 C97 C96 106(3) . . ? C97 C98 C99 124(3) . . ? C97 C98 C86 118(3) . . ? C99 C98 C86 108(3) . . ? C98 C99 C100 121(3) . . ? C98 C99 C84 110(3) . . ? C100 C99 C84 118(3) . . ? C81 C100 C99 121(4) . . ? C81 C100 C101 107(3) . . ? C99 C100 C101 116(3) . . ? C96 C101 C102 123(3) . . ? C96 C101 C100 121(3) . . ? C102 C101 C100 106(3) . . ? C101 C102 C103 120(3) . . ? C101 C102 C80 113(3) . . ? C103 C102 C80 117(3) . . ? C94 C103 C102 115(3) . . ? C94 C103 C77 112(3) . . ? C102 C103 C77 118(3) . . ? C105 C104 C109 118(3) . . ? C105 C104 P2 122(3) . . ? C109 C104 P2 120(3) . . ? C104 C105 C106 122(4) . . ? C104 C105 H105 118.8 . . ? C106 C105 H105 118.8 . . ? C107 C106 C105 123(6) . . ? C107 C106 H106 118.7 . . ? C105 C106 H106 118.7 . . ? C106 C107 C108 118(6) . . ? C106 C107 H107 121.2 . . ? C108 C107 H107 121.2 . . ? C107 C108 C109 124(5) . . ? C107 C108 H108 118.1 . . ? C109 C108 H108 118.1 . . ? C104 C109 C108 116(4) . . ? C104 C109 H109 122.1 . . ? C108 C109 H109 122.1 . . ? C111 C110 C115 120(4) . . ? C111 C110 P2 120(3) . . ? C115 C110 P2 120(3) . . ? C110 C111 C112 124(4) . . ? C110 C111 H111 118.1 . . ? C112 C111 H111 118.1 . . ? C111 C112 C113 118(5) . . ? C111 C112 H112 121.2 . . ? C113 C112 H112 121.2 . . ? C114 C113 C112 119(5) . . ? C114 C113 H113 120.4 . . ? C112 C113 H113 120.4 . . ? C113 C114 C115 123(5) . . ? C113 C114 H114 118.3 . . ? C115 C114 H114 118.3 . . ? C110 C115 C114 115(4) . . ? C110 C115 H115 122.4 . . ? C114 C115 H115 122.4 . . ? C121 C116 C117 119(3) . . ? C121 C116 P2 131(2) . . ? C117 C116 P2 110(2) . . ? C118 C117 C116 122(3) . . ? C118 C117 H117 119.1 . . ? C116 C117 H117 119.1 . . ? C119 C118 C117 119(3) . . ? C119 C118 H118 120.4 . . ? C117 C118 H118 120.4 . . ? C118 C119 C120 119(3) . . ? C118 C119 H119 120.3 . . ? C120 C119 H119 120.3 . . ? C119 C120 C121 123(3) . . ? C119 C120 H120 118.3 . . ? C121 C120 H120 118.3 . . ? C120 C121 C116 117(3) . . ? C120 C121 C122 116(3) . . ? C116 C121 C122 127(3) . . ? N2 C122 C121 112(2) . . ? N2 C122 C126 102(2) . . ? C121 C122 C126 116(3) . . ? N2 C122 H122 108.8 . . ? C121 C122 H122 108.8 . . ? C126 C122 H122 108.8 . . ? N2 C123 H12A 109.5 . . ? N2 C123 H12B 109.5 . . ? H12A C123 H12B 109.5 . . ? N2 C123 H12C 109.5 . . ? H12A C123 H12C 109.5 . . ? H12B C123 H12C 109.5 . . ? N2 C124 C125 102(2) . . ? N2 C124 H12D 111.3 . . ? C125 C124 H12D 111.3 . . ? N2 C124 H12E 111.3 . . ? C125 C124 H12E 111.3 . . ? H12D C124 H12E 109.2 . . ? C133 C125 C124 113(3) . . ? C133 C125 C136 99(3) . . ? C124 C125 C136 113(3) . . ? C133 C125 C126 117(3) . . ? C124 C125 C126 102(2) . . ? C136 C125 C126 113(2) . . ? C127 C126 C122 114(3) . . ? C127 C126 C130 101(2) . . ? C122 C126 C130 115(2) . . ? C127 C126 C125 114(2) . . ? C122 C126 C125 102(2) . . ? C130 C126 C125 111(2) . . ? C138 C127 C126 129(3) . . ? C138 C127 C128 114(3) . . ? C126 C127 C128 112(3) . . ? C141 C128 C129 122(3) . . ? C141 C128 C127 122(3) . . ? C129 C128 C127 101(3) . . ? C130 C129 C144 119(3) . . ? C130 C129 C128 115(3) . . ? C144 C129 C128 117(3) . . ? C131 C130 C129 123(3) . . ? C131 C130 C126 124(3) . . ? C129 C130 C126 107(3) . . ? C130 C131 C150 120(3) . . ? C130 C131 C132 121(3) . . ? C150 C131 C132 107(3) . . ? C133 C132 C151 121(3) . . ? C133 C132 C131 121(3) . . ? C151 C132 C131 105(3) . . ? C132 C133 C134 119(3) . . ? C132 C133 C125 123(3) . . ? C134 C133 C125 112(3) . . ? C153 C134 C135 123(3) . . ? C153 C134 C133 121(3) . . ? C135 C134 C133 108(3) . . ? C136 C135 C134 109(3) . . ? C136 C135 C156 116(3) . . ? C134 C135 C156 117(3) . . ? C137 C136 C135 126(3) . . ? C137 C136 C125 122(3) . . ? C135 C136 C125 108(3) . . ? C136 C137 C158 115(3) . . ? C136 C137 C138 124(3) . . ? C158 C137 C138 109(3) . . ? C127 C138 C139 125(3) . . ? C127 C138 C137 116(3) . . ? C139 C138 C137 104(3) . . ? C159 C139 C138 112(3) . . ? C159 C139 C140 124(3) . . ? C138 C139 C140 116(3) . . ? C141 C140 C161 115(3) . . ? C141 C140 C139 117(3) . . ? C161 C140 C139 117(3) . . ? C128 C141 C140 125(3) . . ? C128 C141 C142 121(3) . . ? C140 C141 C142 103(3) . . ? C143 C142 C141 121(3) . . ? C143 C142 C182 118(3) . . ? C141 C142 C182 111(3) . . ? C142 C143 C144 120(3) . . ? C142 C143 C184 121(3) . . ? C144 C143 C184 107(3) . . ? C145 C144 C143 109(3) . . ? C145 C144 C129 122(3) . . ? C143 C144 C129 119(3) . . ? C150 C145 C144 116(3) . . ? C150 C145 C146 115(3) . . ? C144 C145 C146 111(3) . . ? C147 C146 C145 126(3) . . ? C147 C146 C184 123(3) . . ? C145 C146 C184 103(3) . . ? C146 C147 C172 122(3) . . ? C146 C147 C148 120(3) . . ? C172 C147 C148 105(3) . . ? C149 C148 C170 129(4) . . ? C149 C148 C147 114(3) . . ? C170 C148 C147 108(3) . . ? C148 C149 C150 128(3) . . ? C148 C149 C151 116(3) . . ? C150 C149 C151 101(3) . . ? C145 C150 C149 116(3) . . ? C145 C150 C131 121(3) . . ? C149 C150 C131 113(3) . . ? C152 C151 C132 122(3) . . ? C152 C151 C149 117(3) . . ? C132 C151 C149 112(3) . . ? C151 C152 C169 120(4) . . ? C151 C152 C153 116(4) . . ? C169 C152 C153 109(3) . . ? C134 C153 C152 121(3) . . ? C134 C153 C154 121(3) . . ? C152 C153 C154 107(3) . . ? C155 C154 C168 120(3) . . ? C155 C154 C153 118(3) . . ? C168 C154 C153 109(3) . . ? C154 C155 C165 121(3) . . ? C154 C155 C156 121(3) . . ? C165 C155 C156 109(3) . . ? C155 C156 C157 109(3) . . ? C155 C156 C135 121(3) . . ? C157 C156 C135 120(3) . . ? C158 C157 C156 119(3) . . ? C158 C157 C162 122(3) . . ? C156 C157 C162 105(3) . . ? C157 C158 C137 124(3) . . ? C157 C158 C159 122(3) . . ? C137 C158 C159 104(3) . . ? C139 C159 C160 117(3) . . ? C139 C159 C158 111(3) . . ? C160 C159 C158 116(3) . . ? C164 C160 C159 121(3) . . ? C164 C160 C163 108(3) . . ? C159 C160 C163 119(3) . . ? C164 C161 C140 120(3) . . ? C164 C161 C182 120(3) . . ? C140 C161 C182 104(3) . . ? C163 C162 C165 121(3) . . ? C163 C162 C157 117(3) . . ? C165 C162 C157 111(3) . . ? C162 C163 C160 123(3) . . ? C162 C163 C178 118(3) . . ? C160 C163 C178 108(3) . . ? C161 C164 C160 121(3) . . ? C161 C164 C179 120(3) . . ? C160 C164 C179 109(3) . . ? C166 C165 C155 119(3) . . ? C166 C165 C162 119(3) . . ? C155 C165 C162 106(3) . . ? C165 C166 C167 121(3) . . ? C165 C166 C177 123(3) . . ? C167 C166 C177 106(3) . . ? C168 C167 C166 121(4) . . ? C168 C167 C176 120(3) . . ? C166 C167 C176 109(3) . . ? C167 C168 C154 118(3) . . ? C167 C168 C169 120(3) . . ? C154 C168 C169 107(3) . . ? C170 C169 C152 121(3) . . ? C170 C169 C168 118(3) . . ? C152 C169 C168 108(3) . . ? C148 C170 C171 112(3) . . ? C148 C170 C169 117(3) . . ? C171 C170 C169 120(3) . . ? C170 C171 C172 104(3) . . ? C170 C171 C176 122(3) . . ? C172 C171 C176 121(3) . . ? C173 C172 C147 119(3) . . ? C173 C172 C171 120(3) . . ? C147 C172 C171 111(3) . . ? C172 C173 C183 119(3) . . ? C172 C173 C174 119(3) . . ? C183 C173 C174 108(3) . . ? C175 C174 C173 119(3) . . ? C175 C174 C180 121(3) . . ? C173 C174 C180 108(3) . . ? C174 C175 C176 124(3) . . ? C174 C175 C177 120(3) . . ? C176 C175 C177 108(3) . . ? C175 C176 C167 108(3) . . ? C175 C176 C171 117(3) . . ? C167 C176 C171 119(3) . . ? C178 C177 C175 121(3) . . ? C178 C177 C166 114(3) . . ? C175 C177 C166 108(3) . . ? C177 C178 C163 125(3) . . ? C177 C178 C179 118(3) . . ? C163 C178 C179 107(3) . . ? C180 C179 C164 120(3) . . ? C180 C179 C178 121(3) . . ? C164 C179 C178 108(3) . . ? C179 C180 C181 119(3) . . ? C179 C180 C174 118(3) . . ? C181 C180 C174 109(3) . . ? C182 C181 C180 123(3) . . ? C182 C181 C183 121(3) . . ? C180 C181 C183 107(3) . . ? C181 C182 C161 118(3) . . ? C181 C182 C142 121(3) . . ? C161 C182 C142 107(3) . . ? C184 C183 C173 123(3) . . ? C184 C183 C181 117(3) . . ? C173 C183 C181 109(3) . . ? C183 C184 C143 122(3) . . ? C183 C184 C146 114(3) . . ? C143 C184 C146 109(3) . . ? C43 N1 C41 102(2) . . ? C43 N1 C42 113(2) . . ? C41 N1 C42 112(3) . . ? C124 N2 C122 105(2) . . ? C124 N2 C123 113(2) . . ? C122 N2 C123 115(3) . . ? C23 P1 C35 103.9(15) . . ? C23 P1 C29 102.3(18) . . ? C35 P1 C29 108.6(18) . . ? C23 P1 Os1 114.0(12) . . ? C35 P1 Os1 111.8(9) . . ? C29 P1 Os1 115.2(15) . . ? C104 P2 C116 103.3(14) . . ? C104 P2 C110 98.8(17) . . ? C116 P2 C110 108.8(17) . . ? C104 P2 Os4 114.8(12) . . ? C116 P2 Os4 111.2(10) . . ? C110 P2 Os4 118.3(12) . . ? C1 Os1 C2 91.0(18) . . ? C1 Os1 C3 88.8(18) . . ? C2 Os1 C3 177.4(15) . . ? C1 Os1 P1 106.0(15) . . ? C2 Os1 P1 89.9(11) . . ? C3 Os1 P1 87.5(11) . . ? C1 Os1 Os3 92.5(14) . . ? C2 Os1 Os3 87.4(11) . . ? C3 Os1 Os3 95.3(11) . . ? P1 Os1 Os3 161.4(2) . . ? C1 Os1 Os2 152.0(14) . . ? C2 Os1 Os2 87.9(11) . . ? C3 Os1 Os2 93.5(11) . . ? P1 Os1 Os2 101.9(2) . . ? Os3 Os1 Os2 59.59(5) . . ? C5 Os2 C4 89.7(16) . . ? C5 Os2 C6 85.4(15) . . ? C4 Os2 C6 172.0(16) . . ? C5 Os2 C7 99.7(18) . . ? C4 Os2 C7 93.0(19) . . ? C6 Os2 C7 94.1(18) . . ? C5 Os2 Os3 170.0(11) . . ? C4 Os2 Os3 89.6(12) . . ? C6 Os2 Os3 94.1(10) . . ? C7 Os2 Os3 90.3(14) . . ? C5 Os2 Os1 110.3(11) . . ? C4 Os2 Os1 88.9(12) . . ? C6 Os2 Os1 86.8(11) . . ? C7 Os2 Os1 150.0(14) . . ? Os3 Os2 Os1 59.69(5) . . ? C10 Os3 C9 99(2) . . ? C10 Os3 C8 89(2) . . ? C9 Os3 C8 88.1(19) . . ? C10 Os3 C11 95(2) . . ? C9 Os3 C11 90(2) . . ? C8 Os3 C11 176.3(17) . . ? C10 Os3 Os2 157.3(17) . . ? C9 Os3 Os2 103.0(15) . . ? C8 Os3 Os2 87.7(11) . . ? C11 Os3 Os2 89.3(13) . . ? C10 Os3 Os1 96.7(16) . . ? C9 Os3 Os1 163.5(15) . . ? C8 Os3 Os1 88.6(11) . . ? C11 Os3 Os1 91.9(13) . . ? Os2 Os3 Os1 60.73(5) . . ? C13 Os4 C12 87.6(15) . . ? C13 Os4 C14 88.9(14) . . ? C12 Os4 C14 176.2(13) . . ? C13 Os4 P2 103.6(11) . . ? C12 Os4 P2 93.8(10) . . ? C14 Os4 P2 88.5(9) . . ? C13 Os4 Os5 94.2(11) . . ? C12 Os4 Os5 88.6(10) . . ? C14 Os4 Os5 90.1(9) . . ? P2 Os4 Os5 162.1(2) . . ? C13 Os4 Os6 153.6(11) . . ? C12 Os4 Os6 91.5(10) . . ? C14 Os4 Os6 90.9(9) . . ? P2 Os4 Os6 102.8(2) . . ? Os5 Os4 Os6 59.45(6) . . ? C15 Os5 C17 101(3) . . ? C15 Os5 C18 94(2) . . ? C17 Os5 C18 92(2) . . ? C15 Os5 C16 90.5(17) . . ? C17 Os5 C16 88.5(19) . . ? C18 Os5 C16 175.7(12) . . ? C15 Os5 Os6 155.9(17) . . ? C17 Os5 Os6 102.7(19) . . ? C18 Os5 Os6 86.6(12) . . ? C16 Os5 Os6 89.09(7) . . ? C15 Os5 Os4 95.1(17) . . ? C17 Os5 Os4 163.2(19) . . ? C18 Os5 Os4 90.0(12) . . ? C16 Os5 Os4 88.54(7) . . ? Os6 Os5 Os4 60.78(5) . . ? C21 Os6 C19 99(2) . . ? C21 Os6 C22 89.3(17) . . ? C19 Os6 C22 94(2) . . ? C21 Os6 C20 88.6(19) . . ? C19 Os6 C20 88(2) . . ? C22 Os6 C20 177.0(17) . . ? C21 Os6 Os5 171.5(14) . . ? C19 Os6 Os5 90.0(17) . . ? C22 Os6 Os5 89.8(10) . . ? C20 Os6 Os5 91.9(13) . . ? C21 Os6 Os4 111.7(14) . . ? C19 Os6 Os4 149.7(17) . . ? C22 Os6 Os4 88.1(10) . . ? C20 Os6 Os4 90.6(13) . . ? Os5 Os6 Os4 59.77(5) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 10.569 _refine_diff_density_min -2.260 _refine_diff_density_rms 0.368 # Attachment '- Compound 1.cif' data_a11647 _database_code_depnum_ccdc_archive 'CCDC 843722' #TrackingRef '- Compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C81 H20 N P' _chemical_formula_sum 'C81 H20 N P' _chemical_formula_weight 1037.95 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.620(3) _cell_length_b 14.2383(18) _cell_length_c 30.475(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.428(8) _cell_angle_gamma 90.00 _cell_volume 9665(2) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 25609 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4224 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9538 _exptl_absorpt_correction_T_max 0.9667 _exptl_absorpt_process_details 'SADABS, 2003 ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25609 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0905 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8395 _reflns_number_gt 5009 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1752P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8395 _refine_ls_number_parameters 751 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1356 _refine_ls_R_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.2906 _refine_ls_wR_factor_gt 0.2671 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.119 _refine_ls_shift/su_mean 0.022 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 C1 C 0.3870(2) 0.5823(3) 1.03965(14) 0.0334(11) Uani 1 1 d . A 1 C2 C 0.3826(3) 0.6698(4) 1.05930(18) 0.0582(15) Uani 1 1 d . A 1 H2 H 0.3444 0.6939 1.0576 0.070 Uiso 1 1 calc R A 1 C3 C 0.4360(3) 0.7230(4) 1.08203(19) 0.0614(16) Uani 1 1 d . A 1 H3 H 0.4337 0.7820 1.0959 0.074 Uiso 1 1 calc R A 1 C4 C 0.4892(3) 0.6876(4) 1.0832(2) 0.0639(16) Uani 1 1 d . A 1 H4 H 0.5246 0.7229 1.0980 0.077 Uiso 1 1 calc R A 1 C5 C 0.4945(3) 0.6008(4) 1.0636(2) 0.0667(16) Uani 1 1 d . A 1 H5 H 0.5326 0.5773 1.0647 0.080 Uiso 1 1 calc R A 1 C6 C 0.4435(3) 0.5512(4) 1.04276(19) 0.0565(14) Uani 1 1 d . A 1 H6 H 0.4469 0.4918 1.0297 0.068 Uiso 1 1 calc R A 1 C7 C 0.3248(2) 0.4259(3) 1.05939(16) 0.0423(12) Uani 1 1 d . A 1 C8 C 0.3649(2) 0.4322(3) 1.10438(16) 0.0431(12) Uani 1 1 d . A 1 H8 H 0.3934 0.4818 1.1125 0.052 Uiso 1 1 calc R A 1 C9 C 0.3635(2) 0.3656(4) 1.13801(18) 0.0530(14) Uani 1 1 d . A 1 H9 H 0.3902 0.3714 1.1691 0.064 Uiso 1 1 calc R A 1 C10 C 0.3238(3) 0.2924(4) 1.1261(2) 0.0524(14) Uani 1 1 d . A 1 H10 H 0.3237 0.2467 1.1488 0.063 Uiso 1 1 calc R A 1 C11 C 0.2834(3) 0.2842(4) 1.0810(2) 0.0654(17) Uani 1 1 d . A 1 H11 H 0.2562 0.2328 1.0725 0.078 Uiso 1 1 calc R A 1 C12 C 0.2837(3) 0.3526(4) 1.04876(19) 0.0553(15) Uani 1 1 d . A 1 H12 H 0.2549 0.3493 1.0184 0.066 Uiso 1 1 calc R A 1 C13 C 0.3271(2) 0.4463(3) 0.96733(16) 0.0393(11) Uani 1 1 d . A 1 C14 C 0.3635(2) 0.3645(3) 0.97788(18) 0.0453(12) Uani 1 1 d . A 1 H14 H 0.3837 0.3480 1.0094 0.054 Uiso 1 1 calc R A 1 C15 C 0.3700(2) 0.3085(4) 0.94262(19) 0.0511(13) Uani 1 1 d . A 1 H15 H 0.3943 0.2537 0.9503 0.061 Uiso 1 1 calc R A 1 C16 C 0.3407(2) 0.3321(3) 0.89526(19) 0.0476(13) Uani 1 1 d . A 1 H16 H 0.3450 0.2938 0.8710 0.057 Uiso 1 1 calc R A 1 C17 C 0.3060(2) 0.4113(3) 0.88531(17) 0.0452(13) Uani 1 1 d . A 1 H17 H 0.2867 0.4276 0.8536 0.054 Uiso 1 1 calc R A 1 C18 C 0.29733(19) 0.4711(3) 0.92035(14) 0.0300(10) Uani 1 1 d . A 1 C19 C 0.2597(2) 0.5578(3) 0.90559(15) 0.0373(11) Uani 1 1 d . A 1 H19 H 0.2462 0.5794 0.9317 0.045 Uiso 1 1 calc R A 1 C20 C 0.1624(2) 0.4794(4) 0.8748(2) 0.0636(16) Uani 1 1 d . A 1 H20A H 0.1278 0.4696 0.8466 0.095 Uiso 1 1 calc R A 1 H20B H 0.1490 0.5091 0.8987 0.095 Uiso 1 1 calc R A 1 H20C H 0.1811 0.4187 0.8863 0.095 Uiso 1 1 calc R A 1 C21 C 0.1819(2) 0.6343(3) 0.85049(17) 0.0423(12) Uani 1 1 d . A 1 H21A H 0.1629 0.6585 0.8727 0.051 Uiso 1 1 calc R A 1 H21B H 0.1516 0.6332 0.8189 0.051 Uiso 1 1 calc R A 1 C22 C 0.23730(19) 0.6963(3) 0.85148(16) 0.0376(11) Uani 1 1 d . A 1 C23 C 0.29196(18) 0.6441(3) 0.88883(16) 0.0318(10) Uani 1 1 d . A 1 C24 C 0.3263(2) 0.7052(3) 0.93135(14) 0.0332(11) Uani 1 1 d . A 1 C25 C 0.3070(2) 0.7913(3) 0.94035(15) 0.0386(11) Uani 1 1 d . A 1 C26 C 0.2572(2) 0.8385(3) 0.90435(16) 0.0380(11) Uani 1 1 d . A 1 C27 C 0.22870(19) 0.7995(3) 0.86213(16) 0.0356(11) Uani 1 1 d . A 1 C28 C 0.2146(2) 0.8544(3) 0.82104(17) 0.0412(12) Uani 1 1 d . A 1 C29 C 0.22507(19) 0.7983(3) 0.78437(16) 0.0369(11) Uani 1 1 d . A 1 C30 C 0.24544(19) 0.7061(3) 0.80423(15) 0.0372(11) Uani 1 1 d . A 1 C31 C 0.28869(19) 0.6611(3) 0.79103(14) 0.0310(10) Uani 1 1 d . A 1 C32 C 0.3393(2) 0.6131(3) 0.82587(17) 0.0409(12) Uani 1 1 d . A 1 C33 C 0.34286(19) 0.6108(3) 0.87313(16) 0.0336(11) Uani 1 1 d . A 1 C34 C 0.3999(2) 0.6297(3) 0.90858(17) 0.0369(11) Uani 1 1 d . A 1 C35 C 0.3894(2) 0.6850(3) 0.94388(16) 0.0397(12) Uani 1 1 d . A 1 C36 C 0.4317(2) 0.7537(3) 0.96802(16) 0.0423(12) Uani 1 1 d . A 1 C37 C 0.4116(2) 0.8427(3) 0.97775(15) 0.0437(12) Uani 1 1 d . A 1 C38 C 0.3505(2) 0.8636(3) 0.96399(15) 0.0407(12) Uani 1 1 d . A 1 C39 C 0.3282(2) 0.9526(4) 0.94428(17) 0.0464(13) Uani 1 1 d . A 1 C40 C 0.2714(2) 0.9401(3) 0.90736(18) 0.0432(12) Uani 1 1 d . A 1 C41 C 0.2553(2) 0.9929(4) 0.86730(18) 0.0457(13) Uani 1 1 d . A 1 C42 C 0.2267(2) 0.9504(3) 0.82303(18) 0.0436(12) Uani 1 1 d . A 1 C43 C 0.2499(2) 0.9947(4) 0.78962(18) 0.0495(13) Uani 1 1 d . A 1 C44 C 0.2595(2) 0.9389(3) 0.75440(16) 0.0448(13) Uani 1 1 d . A 1 C45 C 0.2455(2) 0.8395(4) 0.75159(16) 0.0452(13) Uani 1 1 d . A 1 C46 C 0.2918(2) 0.7902(3) 0.73765(15) 0.0426(12) Uani 1 1 d . A 1 C47 C 0.3127(2) 0.7046(3) 0.75792(16) 0.0446(13) Uani 1 1 d . A 1 C48 C 0.3766(2) 0.6824(3) 0.77152(16) 0.0421(12) Uani 1 1 d . A 1 C49 C 0.3922(2) 0.6269(3) 0.81356(19) 0.0473(13) Uani 1 1 d . A 1 C50 C 0.4479(2) 0.6383(3) 0.84881(19) 0.0454(13) Uani 1 1 d . A 1 C51 C 0.4533(2) 0.6416(3) 0.89681(18) 0.0424(12) Uani 1 1 d . A 1 C52 C 0.4969(2) 0.7134(4) 0.9214(2) 0.0519(14) Uani 1 1 d . A 1 C53 C 0.4862(2) 0.7659(3) 0.95623(16) 0.0388(11) Uani 1 1 d . A 1 C54 C 0.4991(2) 0.8671(4) 0.95864(18) 0.0502(14) Uani 1 1 d . A 1 C55 C 0.4530(2) 0.9143(3) 0.97128(15) 0.0403(12) Uani 1 1 d . A 1 C56 C 0.4307(3) 1.0014(3) 0.95249(17) 0.0505(14) Uani 1 1 d . A 1 C57 C 0.3676(2) 1.0209(3) 0.93812(17) 0.0444(12) Uani 1 1 d . A 1 C58 C 0.3507(3) 1.0782(3) 0.89628(18) 0.0502(14) Uani 1 1 d . A 1 C59 C 0.2972(3) 1.0657(3) 0.8608(2) 0.0547(14) Uani 1 1 d . A 1 C60 C 0.2922(2) 1.0627(3) 0.81304(19) 0.0458(13) Uani 1 1 d . A 1 C61 C 0.3449(3) 1.0781(3) 0.80107(19) 0.0525(14) Uani 1 1 d . A 1 C62 C 0.3556(3) 1.0231(3) 0.76559(17) 0.0506(14) Uani 1 1 d . A 1 C63 C 0.3118(2) 0.9532(4) 0.74171(15) 0.0479(13) Uani 1 1 d . A 1 C64 C 0.3315(2) 0.8628(3) 0.73123(15) 0.0456(13) Uani 1 1 d . A 1 C65 C 0.3943(2) 0.8414(4) 0.74498(17) 0.0498(14) Uani 1 1 d . A 1 C66 C 0.4160(3) 0.7512(4) 0.76485(19) 0.0560(15) Uani 1 1 d . A 1 C67 C 0.4745(2) 0.7643(4) 0.80109(19) 0.0489(14) Uani 1 1 d . A 1 C68 C 0.4878(2) 0.8667(4) 0.80416(19) 0.0470(13) Uani 1 1 d . A 1 C69 C 0.4377(3) 0.9126(4) 0.76928(18) 0.0559(15) Uani 1 1 d . A 1 C70 C 0.4182(2) 0.9995(4) 0.77826(18) 0.0487(13) Uani 1 1 d . A 1 C71 C 0.4487(2) 1.0444(3) 0.82460(17) 0.0485(13) Uani 1 1 d . A 1 C72 C 0.4024(2) 1.0919(3) 0.8378(2) 0.0509(14) Uani 1 1 d . A 1 C73 C 0.4054(2) 1.0921(3) 0.88402(19) 0.0464(13) Uani 1 1 d . A 1 C74 C 0.4543(2) 1.0463(3) 0.91867(16) 0.0409(12) Uani 1 1 d . A 1 C75 C 0.4976(2) 1.0007(3) 0.90629(18) 0.0476(13) Uani 1 1 d . A 1 C76 C 0.4950(2) 0.9988(4) 0.8587(2) 0.0516(14) Uani 1 1 d . A 1 C77 C 0.5161(2) 0.9062(4) 0.8479(2) 0.0536(15) Uani 1 1 d . A 1 C78 C 0.5325(2) 0.8531(4) 0.8902(2) 0.0524(14) Uani 1 1 d . A 1 C79 C 0.5195(2) 0.7526(4) 0.88720(19) 0.0465(13) Uani 1 1 d . A 1 C80 C 0.4900(2) 0.7121(4) 0.8420(2) 0.0522(14) Uani 1 1 d . A 1 C81 C 0.5220(2) 0.9075(4) 0.92612(18) 0.0485(13) Uani 1 1 d . A 1 N1 N 0.20678(17) 0.5413(3) 0.86407(14) 0.0459(10) Uani 1 1 d . A 1 P1 P 0.31613(6) 0.51742(9) 1.01487(4) 0.0324(4) Uani 0.90 1 d P A 1 P1' P 0.3698(5) 0.4659(8) 1.0113(4) 0.0324(4) Uani 0.10 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.046(3) 0.028(3) 0.025(2) 0.004(2) 0.011(2) -0.008(2) C2 0.081(4) 0.054(4) 0.051(3) 0.006(3) 0.038(3) 0.004(3) C3 0.085(5) 0.050(4) 0.047(3) -0.017(3) 0.019(3) -0.030(3) C4 0.057(4) 0.066(4) 0.061(4) 0.003(3) 0.010(3) -0.015(3) C5 0.059(4) 0.048(4) 0.084(4) 0.003(3) 0.011(3) -0.010(3) C6 0.059(4) 0.046(3) 0.062(4) 0.008(3) 0.017(3) 0.003(3) C7 0.059(3) 0.037(3) 0.036(3) 0.000(2) 0.021(3) -0.005(2) C8 0.051(3) 0.046(3) 0.035(3) 0.008(2) 0.018(2) -0.004(2) C9 0.058(4) 0.067(4) 0.036(3) 0.014(3) 0.020(3) 0.013(3) C10 0.068(4) 0.043(3) 0.057(3) 0.022(3) 0.035(3) 0.010(3) C11 0.093(5) 0.047(4) 0.068(4) 0.010(3) 0.042(4) -0.017(3) C12 0.075(4) 0.052(4) 0.043(3) 0.001(3) 0.024(3) -0.018(3) C13 0.046(3) 0.033(3) 0.038(3) 0.006(2) 0.012(2) -0.008(2) C14 0.056(3) 0.039(3) 0.042(3) -0.002(2) 0.017(3) 0.003(2) C15 0.057(3) 0.043(3) 0.055(3) -0.001(3) 0.020(3) 0.003(3) C16 0.063(4) 0.027(3) 0.061(3) -0.006(2) 0.032(3) -0.003(2) C17 0.059(3) 0.039(3) 0.037(3) -0.002(2) 0.014(3) -0.008(2) C18 0.036(3) 0.024(2) 0.027(2) -0.0030(19) 0.007(2) -0.0162(19) C19 0.036(3) 0.041(3) 0.034(3) -0.002(2) 0.011(2) -0.006(2) C20 0.040(3) 0.055(4) 0.098(5) 0.004(3) 0.025(3) -0.017(3) C21 0.030(3) 0.048(3) 0.047(3) 0.004(2) 0.009(2) 0.003(2) C22 0.037(3) 0.032(3) 0.037(3) 0.000(2) 0.003(2) -0.002(2) C23 0.023(2) 0.022(2) 0.046(3) -0.004(2) 0.005(2) -0.0003(17) C24 0.048(3) 0.027(3) 0.030(2) 0.0009(19) 0.020(2) -0.003(2) C25 0.044(3) 0.041(3) 0.033(3) -0.005(2) 0.015(2) -0.005(2) C26 0.039(3) 0.035(3) 0.046(3) 0.004(2) 0.022(2) 0.003(2) C27 0.025(2) 0.036(3) 0.045(3) 0.002(2) 0.012(2) 0.0035(19) C28 0.033(3) 0.039(3) 0.047(3) -0.001(2) 0.007(2) 0.004(2) C29 0.026(3) 0.036(3) 0.038(3) 0.001(2) -0.004(2) -0.005(2) C30 0.026(3) 0.044(3) 0.037(3) -0.009(2) 0.004(2) -0.014(2) C31 0.036(3) 0.024(2) 0.026(2) -0.0081(19) 0.002(2) -0.0100(19) C32 0.048(3) 0.022(3) 0.056(3) -0.009(2) 0.021(3) -0.005(2) C33 0.036(3) 0.022(2) 0.043(3) -0.005(2) 0.013(2) -0.0042(19) C34 0.034(3) 0.021(2) 0.047(3) 0.007(2) 0.001(2) 0.0039(19) C35 0.041(3) 0.036(3) 0.035(3) 0.017(2) 0.002(2) -0.005(2) C36 0.047(3) 0.041(3) 0.029(2) 0.015(2) 0.000(2) -0.003(2) C37 0.061(4) 0.043(3) 0.023(2) 0.001(2) 0.008(2) -0.004(2) C38 0.055(3) 0.040(3) 0.031(2) -0.008(2) 0.019(2) -0.003(2) C39 0.063(4) 0.039(3) 0.039(3) -0.010(2) 0.019(3) 0.005(3) C40 0.038(3) 0.041(3) 0.052(3) -0.013(2) 0.017(3) 0.008(2) C41 0.037(3) 0.043(3) 0.059(3) -0.003(3) 0.018(3) 0.010(2) C42 0.034(3) 0.033(3) 0.061(3) 0.003(3) 0.011(3) 0.011(2) C43 0.043(3) 0.041(3) 0.052(3) 0.011(3) 0.000(3) 0.013(2) C44 0.048(3) 0.034(3) 0.035(3) 0.011(2) -0.009(2) 0.007(2) C45 0.037(3) 0.052(3) 0.032(3) 0.001(2) -0.008(2) -0.003(2) C46 0.055(3) 0.041(3) 0.022(2) -0.003(2) -0.001(2) -0.018(2) C47 0.060(4) 0.044(3) 0.030(2) -0.016(2) 0.016(2) -0.014(2) C48 0.052(3) 0.041(3) 0.040(3) -0.018(2) 0.025(3) -0.008(2) C49 0.063(4) 0.025(3) 0.057(3) -0.011(2) 0.024(3) 0.000(2) C50 0.034(3) 0.041(3) 0.062(3) -0.006(3) 0.017(3) 0.016(2) C51 0.039(3) 0.020(3) 0.061(3) 0.010(2) 0.007(3) 0.009(2) C52 0.033(3) 0.045(3) 0.062(4) 0.024(3) -0.005(3) 0.014(2) C53 0.031(3) 0.037(3) 0.033(3) 0.006(2) -0.009(2) 0.000(2) C54 0.036(3) 0.056(4) 0.043(3) 0.007(3) -0.006(2) -0.013(2) C55 0.048(3) 0.035(3) 0.030(2) -0.003(2) 0.002(2) -0.011(2) C56 0.068(4) 0.034(3) 0.038(3) -0.016(2) 0.003(3) -0.012(3) C57 0.059(4) 0.026(3) 0.045(3) -0.017(2) 0.013(3) -0.006(2) C58 0.065(4) 0.026(3) 0.046(3) -0.011(2) 0.001(3) 0.007(2) C59 0.069(4) 0.022(3) 0.064(4) -0.003(3) 0.010(3) 0.011(2) C60 0.050(3) 0.028(3) 0.057(3) 0.014(2) 0.014(3) 0.006(2) C61 0.068(4) 0.026(3) 0.052(3) 0.013(2) 0.005(3) 0.005(2) C62 0.080(4) 0.027(3) 0.040(3) 0.018(2) 0.014(3) -0.006(3) C63 0.062(4) 0.044(3) 0.028(3) 0.011(2) 0.003(2) -0.006(3) C64 0.067(4) 0.042(3) 0.024(2) 0.000(2) 0.011(2) -0.014(3) C65 0.057(4) 0.064(4) 0.035(3) -0.006(3) 0.022(3) -0.020(3) C66 0.073(4) 0.060(4) 0.049(3) -0.012(3) 0.038(3) 0.001(3) C67 0.037(3) 0.065(4) 0.056(3) -0.015(3) 0.030(3) -0.004(3) C68 0.048(3) 0.047(3) 0.058(3) 0.004(3) 0.035(3) -0.002(2) C69 0.068(4) 0.062(4) 0.046(3) 0.006(3) 0.030(3) -0.012(3) C70 0.054(4) 0.046(3) 0.049(3) 0.016(3) 0.020(3) -0.012(3) C71 0.064(4) 0.034(3) 0.044(3) 0.004(2) 0.012(3) -0.025(3) C72 0.053(3) 0.017(3) 0.068(4) 0.004(2) 0.001(3) -0.014(2) C73 0.064(4) 0.017(3) 0.060(3) -0.011(2) 0.023(3) -0.011(2) C74 0.050(3) 0.027(3) 0.041(3) -0.006(2) 0.008(2) -0.020(2) C75 0.040(3) 0.037(3) 0.050(3) 0.007(2) -0.005(2) -0.022(2) C76 0.046(3) 0.045(3) 0.064(4) 0.002(3) 0.017(3) -0.023(3) C77 0.039(3) 0.061(4) 0.066(4) 0.008(3) 0.025(3) -0.020(3) C78 0.022(3) 0.065(4) 0.064(4) 0.002(3) 0.006(3) -0.005(2) C79 0.021(3) 0.052(3) 0.062(3) 0.007(3) 0.008(2) 0.003(2) C80 0.045(3) 0.048(3) 0.070(4) 0.000(3) 0.028(3) 0.013(3) C81 0.029(3) 0.057(4) 0.047(3) 0.000(3) -0.004(2) -0.019(2) N1 0.036(2) 0.053(3) 0.047(2) 0.002(2) 0.011(2) -0.011(2) P1 0.0381(8) 0.0298(8) 0.0324(7) 0.0036(6) 0.0158(6) 0.0001(6) P1' 0.0381(8) 0.0298(8) 0.0324(7) 0.0036(6) 0.0158(6) 0.0001(6) _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 C1 C6 1.378(7) . ? C1 C2 1.402(7) . ? C1 P1 1.839(5) . ? C2 C3 1.436(8) . ? C2 H2 0.9500 . ? C3 C4 1.345(8) . ? C3 H3 0.9500 . ? C4 C5 1.396(8) . ? C4 H4 0.9500 . ? C5 C6 1.359(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.388(7) . ? C7 C8 1.386(7) . ? C7 P1 1.843(5) . ? C8 C9 1.404(6) . ? C8 H8 0.9500 . ? C9 C10 1.369(7) . ? C9 H9 0.9500 . ? C10 C11 1.394(8) . ? C10 H10 0.9500 . ? C11 C12 1.385(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.414(6) . ? C13 C14 1.419(7) . ? C13 P1 1.855(5) . ? C14 C15 1.387(7) . ? C14 H14 0.9500 . ? C15 C16 1.418(7) . ? C15 H15 0.9500 . ? C16 C17 1.368(7) . ? C16 H16 0.9500 . ? C17 C18 1.433(6) . ? C17 H17 0.9500 . ? C18 C19 1.500(6) . ? C19 N1 1.473(6) . ? C19 C23 1.614(6) . ? C19 H19 1.0000 . ? C20 N1 1.488(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N1 1.452(6) . ? C21 C22 1.571(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C30 1.521(6) . ? C22 C27 1.533(6) . ? C22 C23 1.593(6) . ? C23 C33 1.510(6) . ? C23 C24 1.547(6) . ? C24 C25 1.367(6) . ? C24 C35 1.440(6) . ? C25 C38 1.464(6) . ? C25 C26 1.477(6) . ? C26 C27 1.357(6) . ? C26 C40 1.481(7) . ? C27 C28 1.418(6) . ? C28 C42 1.395(6) . ? C28 C29 1.459(6) . ? C29 C45 1.376(6) . ? C29 C30 1.458(6) . ? C30 C31 1.375(6) . ? C31 C47 1.450(6) . ? C31 C32 1.476(6) . ? C32 C33 1.415(6) . ? C32 C49 1.432(7) . ? C33 C34 1.444(6) . ? C34 C35 1.420(6) . ? C34 C51 1.432(6) . ? C35 C36 1.416(7) . ? C36 C37 1.419(7) . ? C36 C53 1.457(7) . ? C37 C38 1.393(7) . ? C37 C55 1.471(6) . ? C38 C39 1.425(7) . ? C39 C57 1.401(7) . ? C39 C40 1.447(7) . ? C40 C41 1.375(7) . ? C41 C42 1.427(7) . ? C41 C59 1.491(7) . ? C42 C43 1.451(7) . ? C43 C60 1.404(7) . ? C43 C44 1.414(7) . ? C44 C63 1.428(7) . ? C44 C45 1.449(7) . ? C45 C46 1.477(7) . ? C46 C47 1.382(7) . ? C46 C64 1.453(6) . ? C47 C48 1.460(7) . ? C48 C66 1.412(7) . ? C48 C49 1.445(7) . ? C49 C50 1.404(7) . ? C50 C51 1.426(7) . ? C50 C80 1.508(7) . ? C51 C52 1.467(7) . ? C52 C53 1.391(7) . ? C52 C79 1.432(7) . ? C53 C54 1.469(7) . ? C54 C81 1.401(7) . ? C54 C55 1.436(7) . ? C55 C56 1.394(7) . ? C56 C57 1.435(7) . ? C56 C74 1.471(7) . ? C57 C58 1.453(7) . ? C58 C59 1.374(7) . ? C58 C73 1.472(7) . ? C59 C60 1.423(7) . ? C60 C61 1.426(7) . ? C61 C62 1.424(7) . ? C61 C72 1.457(7) . ? C62 C70 1.439(7) . ? C62 C63 1.444(7) . ? C63 C64 1.440(7) . ? C64 C65 1.433(8) . ? C65 C66 1.439(7) . ? C65 C69 1.457(7) . ? C66 C67 1.465(7) . ? C67 C80 1.392(7) . ? C67 C68 1.488(7) . ? C68 C77 1.394(7) . ? C68 C69 1.457(8) . ? C69 C70 1.379(7) . ? C70 C71 1.498(7) . ? C71 C76 1.394(7) . ? C71 C72 1.453(7) . ? C72 C73 1.386(7) . ? C73 C74 1.436(7) . ? C74 C75 1.366(7) . ? C75 C76 1.432(7) . ? C75 C81 1.491(7) . ? C76 C77 1.485(7) . ? C77 C78 1.431(7) . ? C78 C81 1.430(7) . ? C78 C79 1.460(7) . ? C79 C80 1.441(7) . ? 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 C1 C2 117.6(5) . . ? C6 C1 P1 126.5(4) . . ? C2 C1 P1 115.8(4) . . ? C1 C2 C3 119.8(5) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 118.6(5) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 122.5(6) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C6 C5 C4 117.9(6) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.1 . . ? C5 C6 C1 123.6(6) . . ? C5 C6 H6 118.2 . . ? C1 C6 H6 118.2 . . ? C12 C7 C8 118.3(4) . . ? C12 C7 P1 117.5(4) . . ? C8 C7 P1 123.7(4) . . ? C7 C8 C9 120.3(5) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 120.0(5) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.7(5) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 118.4(5) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? C7 C12 C11 122.2(6) . . ? C7 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C18 C13 C14 119.6(4) . . ? C18 C13 P1 120.2(4) . . ? C14 C13 P1 120.2(4) . . ? C15 C14 C13 120.7(5) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 120.7(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 118.3(5) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? C16 C17 C18 123.3(5) . . ? C16 C17 H17 118.4 . . ? C18 C17 H17 118.4 . . ? C13 C18 C17 117.4(4) . . ? C13 C18 C19 123.7(4) . . ? C17 C18 C19 118.9(4) . . ? N1 C19 C18 112.0(4) . . ? N1 C19 C23 101.8(3) . . ? C18 C19 C23 115.3(3) . . ? N1 C19 H19 109.1 . . ? C18 C19 H19 109.1 . . ? C23 C19 H19 109.1 . . ? N1 C20 H20A 109.5 . . ? N1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 C22 104.6(4) . . ? N1 C21 H21A 110.8 . . ? C22 C21 H21A 110.8 . . ? N1 C21 H21B 110.8 . . ? C22 C21 H21B 110.8 . . ? H21A C21 H21B 108.9 . . ? C30 C22 C27 100.3(4) . . ? C30 C22 C21 113.6(4) . . ? C27 C22 C21 112.0(4) . . ? C30 C22 C23 113.1(4) . . ? C27 C22 C23 115.4(4) . . ? C21 C22 C23 102.9(3) . . ? C33 C23 C24 101.0(3) . . ? C33 C23 C22 117.5(4) . . ? C24 C23 C22 114.2(3) . . ? C33 C23 C19 111.7(3) . . ? C24 C23 C19 109.5(3) . . ? C22 C23 C19 103.1(3) . . ? C25 C24 C35 120.7(4) . . ? C25 C24 C23 123.8(4) . . ? C35 C24 C23 108.5(4) . . ? C24 C25 C38 120.3(4) . . ? C24 C25 C26 119.7(4) . . ? C38 C25 C26 107.5(4) . . ? C27 C26 C25 122.7(4) . . ? C27 C26 C40 119.3(4) . . ? C25 C26 C40 106.9(4) . . ? C26 C27 C28 120.6(4) . . ? C26 C27 C22 122.3(4) . . ? C28 C27 C22 110.5(4) . . ? C42 C28 C27 121.1(4) . . ? C42 C28 C29 119.0(4) . . ? C27 C28 C29 109.0(4) . . ? C45 C29 C28 120.8(4) . . ? C45 C29 C30 122.5(4) . . ? C28 C29 C30 106.9(4) . . ? C31 C30 C29 118.2(4) . . ? C31 C30 C22 125.0(4) . . ? C29 C30 C22 110.3(4) . . ? C30 C31 C47 120.3(4) . . ? C30 C31 C32 120.5(4) . . ? C47 C31 C32 106.7(4) . . ? C33 C32 C49 120.5(4) . . ? C33 C32 C31 120.2(4) . . ? C49 C32 C31 108.5(4) . . ? C32 C33 C34 118.8(4) . . ? C32 C33 C23 122.1(4) . . ? C34 C33 C23 110.3(4) . . ? C35 C34 C51 121.0(4) . . ? C35 C34 C33 108.4(4) . . ? C51 C34 C33 121.0(4) . . ? C36 C35 C34 120.4(4) . . ? C36 C35 C24 119.3(4) . . ? C34 C35 C24 109.6(4) . . ? C35 C36 C37 119.8(4) . . ? C35 C36 C53 118.9(4) . . ? C37 C36 C53 109.3(4) . . ? C38 C37 C36 120.9(4) . . ? C38 C37 C55 118.7(4) . . ? C36 C37 C55 107.8(4) . . ? C37 C38 C39 121.1(4) . . ? C37 C38 C25 119.0(4) . . ? C39 C38 C25 108.5(5) . . ? C57 C39 C38 120.3(5) . . ? C57 C39 C40 117.8(5) . . ? C38 C39 C40 109.6(5) . . ? C41 C40 C39 122.3(5) . . ? C41 C40 C26 119.3(4) . . ? C39 C40 C26 107.5(4) . . ? C40 C41 C42 120.8(5) . . ? C40 C41 C59 119.8(5) . . ? C42 C41 C59 107.2(4) . . ? C28 C42 C41 118.8(4) . . ? C28 C42 C43 121.0(5) . . ? C41 C42 C43 108.0(4) . . ? C60 C43 C44 120.4(5) . . ? C60 C43 C42 108.3(5) . . ? C44 C43 C42 118.8(5) . . ? C43 C44 C63 119.8(5) . . ? C43 C44 C45 120.2(5) . . ? C63 C44 C45 109.0(4) . . ? C29 C45 C44 120.1(5) . . ? C29 C45 C46 118.6(4) . . ? C44 C45 C46 107.7(4) . . ? C47 C46 C64 122.5(5) . . ? C47 C46 C45 118.6(4) . . ? C64 C46 C45 105.9(4) . . ? C46 C47 C31 121.6(4) . . ? C46 C47 C48 120.0(4) . . ? C31 C47 C48 108.4(4) . . ? C66 C48 C49 121.4(5) . . ? C66 C48 C47 118.5(5) . . ? C49 C48 C47 107.7(4) . . ? C50 C49 C32 119.5(5) . . ? C50 C49 C48 120.8(5) . . ? C32 C49 C48 108.6(4) . . ? C49 C50 C51 122.1(4) . . ? C49 C50 C80 118.0(5) . . ? C51 C50 C80 106.2(4) . . ? C50 C51 C34 117.8(4) . . ? C50 C51 C52 110.8(4) . . ? C34 C51 C52 118.8(4) . . ? C53 C52 C79 123.5(5) . . ? C53 C52 C51 119.3(5) . . ? C79 C52 C51 105.6(5) . . ? C52 C53 C36 121.7(4) . . ? C52 C53 C54 118.6(4) . . ? C36 C53 C54 106.9(4) . . ? C81 C54 C55 120.2(5) . . ? C81 C54 C53 119.4(5) . . ? C55 C54 C53 108.0(4) . . ? C56 C55 C54 121.5(4) . . ? C56 C55 C37 119.6(5) . . ? C54 C55 C37 108.0(4) . . ? C55 C56 C57 120.7(5) . . ? C55 C56 C74 119.7(5) . . ? C57 C56 C74 107.4(5) . . ? C39 C57 C56 119.5(5) . . ? C39 C57 C58 120.5(5) . . ? C56 C57 C58 109.3(4) . . ? C59 C58 C57 121.9(5) . . ? C59 C58 C73 118.2(5) . . ? C57 C58 C73 106.9(4) . . ? C58 C59 C60 123.4(5) . . ? C58 C59 C41 117.7(5) . . ? C60 C59 C41 106.4(5) . . ? C43 C60 C61 120.7(5) . . ? C43 C60 C59 110.1(5) . . ? C61 C60 C59 118.4(5) . . ? C60 C61 C62 120.0(5) . . ? C60 C61 C72 119.6(5) . . ? C62 C61 C72 107.6(5) . . ? C61 C62 C70 110.5(5) . . ? C61 C62 C63 118.9(5) . . ? C70 C62 C63 118.3(5) . . ? C44 C63 C62 120.1(5) . . ? C44 C63 C64 107.7(4) . . ? C62 C63 C64 119.8(5) . . ? C65 C64 C63 120.3(4) . . ? C65 C64 C46 117.5(5) . . ? C63 C64 C46 109.6(4) . . ? C64 C65 C66 120.1(4) . . ? C64 C65 C69 119.0(5) . . ? C66 C65 C69 108.4(5) . . ? C48 C66 C65 121.4(5) . . ? C48 C66 C67 118.8(5) . . ? C65 C66 C67 108.5(5) . . ? C80 C67 C66 120.6(5) . . ? C80 C67 C68 118.7(5) . . ? C66 C67 C68 107.4(5) . . ? C77 C68 C69 122.0(5) . . ? C77 C68 C67 118.6(5) . . ? C69 C68 C67 106.9(5) . . ? C70 C69 C65 120.0(5) . . ? C70 C69 C68 120.1(5) . . ? C65 C69 C68 108.8(5) . . ? C69 C70 C62 122.5(5) . . ? C69 C70 C71 118.8(5) . . ? C62 C70 C71 106.4(5) . . ? C76 C71 C72 119.2(5) . . ? C76 C71 C70 121.0(5) . . ? C72 C71 C70 106.8(5) . . ? C73 C72 C71 119.5(5) . . ? C73 C72 C61 120.1(5) . . ? C71 C72 C61 108.6(5) . . ? C72 C73 C74 120.2(5) . . ? C72 C73 C58 120.3(5) . . ? C74 C73 C58 108.2(4) . . ? C75 C74 C73 120.4(4) . . ? C75 C74 C56 118.6(4) . . ? C73 C74 C56 108.2(4) . . ? C74 C75 C76 120.3(5) . . ? C74 C75 C81 122.3(5) . . ? C76 C75 C81 105.9(5) . . ? C71 C76 C75 120.3(5) . . ? C71 C76 C77 119.1(5) . . ? C75 C76 C77 109.7(5) . . ? C68 C77 C78 123.2(5) . . ? C68 C77 C76 118.8(5) . . ? C78 C77 C76 106.2(5) . . ? C81 C78 C77 109.9(5) . . ? C81 C78 C79 119.4(5) . . ? C77 C78 C79 118.2(5) . . ? C52 C79 C80 111.1(5) . . ? C52 C79 C78 117.4(5) . . ? C80 C79 C78 118.5(5) . . ? C67 C80 C79 122.8(5) . . ? C67 C80 C50 120.4(5) . . ? C79 C80 C50 106.2(4) . . ? C54 C81 C78 121.7(5) . . ? C54 C81 C75 117.7(5) . . ? C78 C81 C75 108.3(5) . . ? C21 N1 C19 104.3(4) . . ? C21 N1 C20 110.8(4) . . ? C19 N1 C20 111.4(4) . . ? C1 P1 C7 100.9(2) . . ? C1 P1 C13 104.5(2) . . ? C7 P1 C13 100.3(2) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.805 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.132 # Attachment '- Compound 5.cif' data_a12561 _database_code_depnum_ccdc_archive 'CCDC 843723' #TrackingRef '- Compound 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C84 H20 N O3 P Ru), 3(C S2), H2O' _chemical_formula_sum 'C171 H42 N2 O7 P2 Ru2 S6' _chemical_formula_weight 2692.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 10.0828(13) _cell_length_b 16.351(2) _cell_length_c 16.5332(19) _cell_angle_alpha 84.296(7) _cell_angle_beta 77.770(7) _cell_angle_gamma 77.840(9) _cell_volume 2599.8(6) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 23286 _cell_measurement_theta_min 1.26 _cell_measurement_theta_max 25.04 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8509 _exptl_absorpt_correction_T_max 0.9897 _exptl_absorpt_process_details 'SADABS, 2003 ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23286 _diffrn_reflns_av_R_equivalents 0.1175 _diffrn_reflns_av_sigmaI/netI 0.2617 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.04 _reflns_number_total 8638 _reflns_number_gt 3971 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1445P)^2^+43.5657P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8638 _refine_ls_number_parameters 839 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2496 _refine_ls_R_factor_gt 0.1196 _refine_ls_wR_factor_ref 0.3715 _refine_ls_wR_factor_gt 0.3090 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 C1 C 0.674(2) 0.8971(17) 0.5222(12) 0.058(6) Uani 1 1 d . A 1 C2 C 0.476(2) 0.8262(15) 0.5973(12) 0.061(6) Uani 1 1 d . A 1 C3 C 0.578(2) 0.6834(13) 0.5282(11) 0.052(5) Uani 1 1 d . A 1 C4 C 0.9884(16) 0.6716(10) 0.5455(10) 0.031(4) Uani 1 1 d . A 1 C5 C 1.0551(14) 0.7138(10) 0.4742(9) 0.025(4) Uani 1 1 d . A 1 C6 C 1.1920(17) 0.6782(11) 0.4396(9) 0.034(4) Uani 1 1 d . A 1 H6 H 1.2405 0.7064 0.3934 0.041 Uiso 1 1 calc R A 1 C7 C 1.2572(16) 0.6036(11) 0.4710(9) 0.035(4) Uani 1 1 d . A 1 H7 H 1.3486 0.5791 0.4455 0.041 Uiso 1 1 calc R A 1 C8 C 1.1890(18) 0.5646(12) 0.5399(9) 0.042(5) Uani 1 1 d . A 1 H8 H 1.2362 0.5140 0.5628 0.050 Uiso 1 1 calc R A 1 C9 C 1.0569(19) 0.5956(12) 0.5761(10) 0.045(5) Uani 1 1 d . A 1 H9 H 1.0112 0.5658 0.6222 0.054 Uiso 1 1 calc R A 1 C10 C 0.8632(16) 0.7925(10) 0.6652(8) 0.026(4) Uani 1 1 d . A 1 C11 C 0.9981(17) 0.7855(11) 0.6772(10) 0.040(4) Uani 1 1 d . A 1 H11 H 1.0696 0.7448 0.6487 0.048 Uiso 1 1 calc R A 1 C12 C 1.0307(18) 0.8351(12) 0.7287(10) 0.043(5) Uani 1 1 d . A 1 H12 H 1.1229 0.8269 0.7372 0.052 Uiso 1 1 calc R A 1 C13 C 0.9335(17) 0.8952(11) 0.7672(9) 0.035(4) Uani 1 1 d . A 1 H13 H 0.9569 0.9293 0.8033 0.042 Uiso 1 1 calc R A 1 C14 C 0.800(2) 0.9081(12) 0.7547(10) 0.048(5) Uani 1 1 d . A 1 H14 H 0.7317 0.9520 0.7811 0.057 Uiso 1 1 calc R A 1 C15 C 0.7632(18) 0.8567(12) 0.7032(10) 0.043(5) Uani 1 1 d . A 1 H15 H 0.6710 0.8657 0.6945 0.052 Uiso 1 1 calc R A 1 C16 C 0.7647(16) 0.6397(10) 0.6782(9) 0.031(4) Uani 1 1 d . A 1 C17 C 0.7351(18) 0.6519(11) 0.7632(11) 0.041(5) Uani 1 1 d . A 1 H17 H 0.7494 0.7012 0.7832 0.050 Uiso 1 1 calc R A 1 C18 C 0.686(2) 0.5920(13) 0.8163(10) 0.055(6) Uani 1 1 d . A 1 H18 H 0.6664 0.5999 0.8741 0.066 Uiso 1 1 calc R A 1 C19 C 0.6626(16) 0.5199(11) 0.7898(9) 0.036(4) Uani 1 1 d . A 1 H19 H 0.6244 0.4799 0.8284 0.043 Uiso 1 1 calc R A 1 C20 C 0.6957(17) 0.5071(12) 0.7069(11) 0.043(5) Uani 1 1 d . A 1 H20 H 0.6870 0.4557 0.6883 0.051 Uiso 1 1 calc R A 1 C21 C 0.7413(18) 0.5670(11) 0.6503(10) 0.041(5) Uani 1 1 d . A 1 H21 H 0.7568 0.5594 0.5926 0.050 Uiso 1 1 calc R A 1 C22 C 0.9907(15) 0.7961(9) 0.4375(8) 0.021(3) Uani 1 1 d . A 1 H22 H 0.9188 0.8241 0.4831 0.026 Uiso 1 1 calc R A 1 C23 C 1.1372(17) 0.8827(11) 0.4668(10) 0.039(4) Uani 1 1 d . A 1 H23A H 1.1799 0.9318 0.4453 0.047 Uiso 1 1 d R A 1 H23B H 1.0665 0.8982 0.5172 0.047 Uiso 1 1 d R A 1 H23C H 1.1971 0.8421 0.4778 0.047 Uiso 1 1 d R A 1 C24 C 0.9766(16) 0.9252(10) 0.3744(9) 0.035(4) Uani 1 1 d . A 1 H24A H 1.0241 0.9683 0.3413 0.041 Uiso 1 1 calc R A 1 H24B H 0.9076 0.9515 0.4212 0.041 Uiso 1 1 calc R A 1 C25 C 0.9086(15) 0.8801(11) 0.3199(8) 0.030(4) Uani 1 1 d . A 1 C26 C 0.9125(15) 0.7863(10) 0.3663(9) 0.028(3) Uani 1 1 d . A 1 C27 C 0.7707(17) 0.7592(11) 0.3956(9) 0.035(4) Uani 1 1 d . A 1 C28 C 0.6427(15) 0.8127(10) 0.3901(9) 0.027(4) Uani 1 1 d . A 1 C29 C 0.6468(17) 0.8959(10) 0.3406(9) 0.030(4) Uani 1 1 d . A 1 C30 C 0.7646(17) 0.9237(10) 0.3070(10) 0.032(4) Uani 1 1 d . A 1 C31 C 0.7784(19) 0.9700(10) 0.2271(10) 0.037(4) Uani 1 1 d . A 1 C32 C 0.9160(19) 0.9441(10) 0.1808(11) 0.039(5) Uani 1 1 d . A 1 C33 C 0.9885(17) 0.8839(11) 0.2326(9) 0.032(4) Uani 1 1 d . A 1 C34 C 1.0813(17) 0.8183(12) 0.1958(10) 0.036(4) Uani 1 1 d . A 1 C35 C 1.0895(16) 0.7322(10) 0.2349(10) 0.031(3) Uani 1 1 d . A 1 C36 C 0.9999(16) 0.7180(10) 0.3089(9) 0.032(4) Uani 1 1 d . A 1 C37 C 0.9285(15) 0.6482(10) 0.3185(8) 0.025(4) Uani 1 1 d . A 1 C38 C 0.7903(15) 0.6733(9) 0.3648(8) 0.024(4) Uani 1 1 d . A 1 C39 C 0.6889(17) 0.6401(11) 0.3459(9) 0.039(5) Uani 1 1 d . A 1 C40 C 0.5562(17) 0.6955(12) 0.3419(10) 0.042(4) Uani 1 1 d . A 1 C41 C 0.5339(15) 0.7807(12) 0.3571(9) 0.034(4) Uani 1 1 d . A 1 C42 C 0.4663(16) 0.8437(13) 0.3074(10) 0.042(5) Uani 1 1 d . A 1 C43 C 0.5314(17) 0.9140(12) 0.2962(10) 0.041(5) Uani 1 1 d . A 1 C44 C 0.5401(16) 0.9632(10) 0.2214(10) 0.033(4) Uani 1 1 d . A 1 C45 C 0.665(2) 0.9906(11) 0.1865(11) 0.046(5) Uani 1 1 d . A 1 C46 C 0.6931(19) 0.9840(12) 0.0936(11) 0.047(4) Uani 1 1 d . A 1 C47 C 0.825(2) 0.9613(12) 0.0549(11) 0.056(5) Uani 1 1 d . A 1 C48 C 0.9388(19) 0.9424(11) 0.0947(9) 0.039(5) Uani 1 1 d . A 1 C49 C 1.0421(17) 0.8733(12) 0.0565(9) 0.036(3) Uani 1 1 d . A 1 C50 C 1.1096(15) 0.8109(11) 0.1070(9) 0.033(4) Uani 1 1 d . A 1 C51 C 1.1290(14) 0.7240(11) 0.0910(9) 0.030(4) Uani 1 1 d . A 1 C52 C 1.1154(18) 0.6773(12) 0.1696(10) 0.043(4) Uani 1 1 d . A 1 C53 C 1.0556(16) 0.6049(12) 0.1775(10) 0.039(4) Uani 1 1 d . A 1 C54 C 0.9611(16) 0.5920(10) 0.2557(10) 0.029(4) Uani 1 1 d . A 1 C55 C 0.8492(16) 0.5599(10) 0.2379(10) 0.031(4) Uani 1 1 d . A 1 C56 C 0.7139(17) 0.5861(11) 0.2777(10) 0.036(4) Uani 1 1 d . A 1 C57 C 0.6011(18) 0.6039(12) 0.2380(10) 0.040(5) Uani 1 1 d . A 1 C58 C 0.5010(16) 0.6734(12) 0.2761(10) 0.038(5) Uani 1 1 d . A 1 C59 C 0.4303(14) 0.7333(13) 0.2273(9) 0.034(4) Uani 1 1 d . A 1 C60 C 0.4106(15) 0.8195(14) 0.2442(10) 0.046(5) Uani 1 1 d . A 1 C61 C 0.4230(17) 0.8691(13) 0.1639(12) 0.049(5) Uani 1 1 d . A 1 C62 C 0.4873(19) 0.9366(13) 0.1543(12) 0.051(5) Uani 1 1 d . A 1 C63 C 0.5802(19) 0.9518(11) 0.0785(10) 0.038(5) Uani 1 1 d . A 1 C64 C 0.6081(17) 0.8974(11) 0.0143(10) 0.038(5) Uani 1 1 d . A 1 C65 C 0.747(2) 0.8738(12) -0.0291(10) 0.043(5) Uani 1 1 d . A 1 C66 C 0.856(2) 0.9031(12) -0.0140(9) 0.045(5) Uani 1 1 d . A 1 C67 C 0.9872(18) 0.8495(13) -0.0092(11) 0.049(5) Uani 1 1 d . A 1 C68 C 1.0061(16) 0.7638(12) -0.0251(8) 0.035(4) Uani 1 1 d . A 1 C69 C 0.8959(17) 0.7335(13) -0.0458(9) 0.042(5) Uani 1 1 d . A 1 C70 C 0.7701(18) 0.7835(13) -0.0486(9) 0.045(5) Uani 1 1 d . A 1 C71 C 0.6441(17) 0.7547(12) -0.0137(9) 0.033(4) Uani 1 1 d . A 1 C72 C 0.5424(18) 0.8259(12) 0.0248(11) 0.045(5) Uani 1 1 d . A 1 C73 C 0.4512(18) 0.8105(13) 0.0995(10) 0.043(5) Uani 1 1 d . A 1 C74 C 0.4575(16) 0.7273(13) 0.1368(10) 0.040(5) Uani 1 1 d . A 1 C75 C 0.5518(17) 0.6605(12) 0.1007(10) 0.041(5) Uani 1 1 d . A 1 C76 C 0.6476(18) 0.6750(13) 0.0236(11) 0.045(4) Uani 1 1 d . A 1 C77 C 0.7753(19) 0.6218(11) 0.0263(9) 0.039(4) Uani 1 1 d . A 1 C78 C 0.9010(17) 0.6485(11) -0.0075(9) 0.036(3) Uani 1 1 d . A 1 C79 C 1.0143(17) 0.6293(12) 0.0349(9) 0.039(4) Uani 1 1 d . A 1 C80 C 1.0781(16) 0.7005(12) 0.0238(9) 0.037(4) Uani 1 1 d . A 1 C81 C 1.0045(17) 0.5826(11) 0.1118(11) 0.040(4) Uani 1 1 d . A 1 C82 C 0.8755(17) 0.5522(10) 0.1457(10) 0.037(4) Uani 1 1 d . A 1 C83 C 0.7651(18) 0.5717(11) 0.1081(10) 0.039(5) Uani 1 1 d . A 1 C84 C 0.6256(17) 0.5971(11) 0.1519(11) 0.039(5) Uani 1 1 d . A 1 C85 C 0.341(2) 0.7126(16) 0.8137(14) 0.078(7) Uani 1 1 d . B 1 C86 C 0.5000 0.5000 1.0000 0.055(8) Uani 1 2 d S . 1 N1 N 1.0763(13) 0.8547(9) 0.4037(8) 0.035(4) Uani 1 1 d . A 1 O1 O 0.6702(15) 0.9688(10) 0.5268(8) 0.064(4) Uani 1 1 d . A 1 O2 O 0.3752(17) 0.8507(11) 0.6406(11) 0.094(6) Uani 1 1 d . A 1 O3 O 0.5276(14) 0.6243(9) 0.5356(7) 0.062(4) Uani 1 1 d . A 1 P1 P 0.8163(4) 0.7225(3) 0.6018(2) 0.0266(10) Uani 1 1 d . A 1 Ru1 Ru 0.64346(14) 0.78671(10) 0.52151(8) 0.0336(5) Uani 1 1 d . A 1 S3 S 0.3732(5) 0.5652(4) 0.9844(3) 0.0589(15) Uani 1 1 d . C 1 S2 S 0.3698(7) 0.7826(4) 0.8591(4) 0.0825(19) Uani 1 1 d . B 1 S1 S 0.3057(11) 0.6437(5) 0.7693(6) 0.136(4) Uani 1 1 d . B 1 O4 O 1.330(2) 0.7867(15) 0.5191(14) 0.047(6) Uiso 0.50 1 d P D 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(12) 0.09(2) 0.052(13) -0.021(13) -0.015(9) -0.026(13) C2 0.052(13) 0.086(18) 0.037(12) 0.000(12) -0.003(10) -0.002(13) C3 0.063(13) 0.061(15) 0.042(12) -0.011(10) -0.018(9) -0.025(12) C4 0.039(10) 0.019(10) 0.038(10) -0.002(8) -0.011(8) -0.006(8) C5 0.014(8) 0.030(10) 0.030(9) -0.016(8) -0.007(6) 0.004(7) C6 0.042(10) 0.042(12) 0.021(9) -0.005(8) -0.015(7) -0.005(9) C7 0.029(9) 0.043(12) 0.033(10) -0.009(9) -0.016(7) 0.003(8) C8 0.053(12) 0.046(13) 0.021(9) 0.002(9) -0.006(8) 0.000(10) C9 0.049(12) 0.051(14) 0.033(10) 0.004(9) -0.008(9) -0.009(10) C10 0.033(9) 0.031(11) 0.019(8) -0.001(7) -0.007(7) -0.015(8) C11 0.034(10) 0.052(13) 0.034(10) -0.021(9) -0.008(8) 0.000(9) C12 0.031(10) 0.059(14) 0.043(11) -0.027(10) -0.007(8) -0.004(10) C13 0.044(11) 0.052(13) 0.022(9) 0.004(8) -0.010(8) -0.035(10) C14 0.061(13) 0.051(14) 0.030(10) -0.024(9) -0.016(9) 0.008(11) C15 0.036(10) 0.048(13) 0.049(11) -0.020(10) -0.017(9) 0.002(10) C16 0.036(9) 0.034(11) 0.025(9) -0.005(8) -0.008(7) -0.003(8) C17 0.050(11) 0.024(11) 0.044(12) -0.005(9) 0.009(9) -0.010(9) C18 0.070(14) 0.077(16) 0.018(10) -0.028(10) 0.002(9) -0.016(13) C19 0.035(10) 0.049(13) 0.021(9) 0.007(8) -0.008(7) -0.004(9) C20 0.039(10) 0.049(13) 0.047(12) -0.001(9) -0.013(8) -0.021(9) C21 0.056(11) 0.054(13) 0.018(9) 0.002(9) -0.004(8) -0.023(10) C22 0.036(9) 0.021(9) 0.006(7) 0.000(6) -0.011(6) 0.002(7) C23 0.046(11) 0.037(12) 0.042(10) 0.003(9) -0.024(8) -0.013(9) C24 0.031(9) 0.042(12) 0.033(9) 0.010(8) -0.010(7) -0.017(8) C25 0.029(9) 0.050(12) 0.015(8) 0.001(8) -0.006(6) -0.013(8) C26 0.031(9) 0.023(10) 0.033 -0.005(8) -0.005(7) -0.010(8) C27 0.050(11) 0.041(12) 0.024(9) 0.007(8) -0.022(8) -0.020(9) C28 0.023(8) 0.035(11) 0.026 -0.010(8) -0.006(6) -0.007(8) C29 0.042(10) 0.033(11) 0.018(8) -0.014(7) -0.012(7) -0.001(8) C30 0.036(10) 0.023(10) 0.040(10) -0.014(8) -0.011(8) -0.005(8) C31 0.059(12) 0.014(10) 0.040(11) 0.006(8) -0.021(9) -0.004(9) C32 0.057(12) 0.022(11) 0.050(12) 0.018(9) -0.026(9) -0.027(9) C33 0.039(10) 0.034(11) 0.029(9) -0.002(8) -0.008(8) -0.022(9) C34 0.032 0.057(14) 0.032(10) -0.003(9) -0.015(7) -0.030(8) C35 0.038 0.029(10) 0.036 0.002(8) -0.029(5) -0.011(8) C36 0.035 0.035(11) 0.032(9) 0.003(8) -0.026(7) -0.005(8) C37 0.033(9) 0.033(10) 0.016(8) 0.014(7) -0.015(7) -0.020(8) C38 0.033(9) 0.025(10) 0.020(8) 0.005(7) -0.014(7) -0.011(8) C39 0.040(10) 0.054(13) 0.024(9) 0.014(9) -0.004(7) -0.023(10) C40 0.037 0.052(13) 0.039 0.001(9) 0.009(8) -0.030(9) C41 0.022(8) 0.052(12) 0.031 -0.004(9) 0.001(7) -0.021(9) C42 0.024(9) 0.069(15) 0.026(10) -0.010(9) -0.002(7) 0.002(10) C43 0.032(10) 0.048(13) 0.027(10) -0.020(9) 0.005(7) 0.026(9) C44 0.029(9) 0.026(11) 0.038(10) -0.011(8) -0.009(8) 0.015(8) C45 0.072(14) 0.023(11) 0.037(11) -0.008(9) -0.021(10) 0.016(10) C46 0.040(11) 0.044 0.046(12) 0.014(9) -0.015(9) 0.014(10) C47 0.094(17) 0.041 0.048(12) 0.028(10) -0.036(12) -0.039(10) C48 0.066(12) 0.040(12) 0.019(9) 0.013(8) -0.008(8) -0.038(10) C49 0.038(7) 0.052(9) 0.024(6) -0.003(6) -0.002(5) -0.024(7) C50 0.020(8) 0.048(13) 0.031(9) 0.012(9) 0.001(7) -0.018(8) C51 0.014(8) 0.044(12) 0.032(9) -0.007(8) -0.008(7) 0.001(8) C52 0.043 0.047(13) 0.040(11) -0.005(10) -0.018(8) 0.003(10) C53 0.023(9) 0.051(13) 0.039(11) -0.011(9) -0.013(8) 0.009(9) C54 0.039(10) 0.020(10) 0.033(10) 0.006(8) -0.022(8) -0.003(8) C55 0.037(10) 0.018(10) 0.037(10) 0.004(8) -0.009(8) -0.006(8) C56 0.046(11) 0.032(11) 0.035(10) 0.014(8) -0.005(8) -0.028(9) C57 0.046(11) 0.050(13) 0.037(10) -0.002(9) -0.008(8) -0.039(10) C58 0.023(9) 0.062(14) 0.031(10) -0.005(10) 0.008(8) -0.028(10) C59 0.011(8) 0.067(15) 0.027(9) 0.001(9) -0.006(7) -0.011(9) C60 0.012(8) 0.087(17) 0.035(11) -0.001(11) 0.006(7) -0.012(10) C61 0.023(10) 0.067(15) 0.060(13) -0.015(11) -0.020(9) 0.004(10) C62 0.035(11) 0.044(14) 0.067(14) -0.008(11) -0.030(10) 0.029(10) C63 0.053(12) 0.031(11) 0.027(10) 0.002(9) -0.028(9) 0.017(9) C64 0.040(10) 0.044(13) 0.023(9) 0.020(9) -0.014(8) 0.004(9) C65 0.064(13) 0.044(13) 0.027(10) 0.008(9) -0.029(9) -0.009(11) C66 0.066(13) 0.058(14) 0.016(9) 0.018(9) 0.000(8) -0.040(11) C67 0.040(11) 0.057(15) 0.042 0.019(10) 0.012(8) -0.025(11) C68 0.028(9) 0.062(14) 0.012(8) 0.000(8) 0.005(7) -0.016(9) C69 0.032(10) 0.074(15) 0.019(9) -0.001(9) -0.001(7) -0.011(10) C70 0.044(12) 0.072(16) 0.021(9) -0.008(9) -0.019(8) -0.002(11) C71 0.037(10) 0.042(12) 0.025(9) -0.012(9) -0.022(8) -0.004(9) C72 0.041(11) 0.061(14) 0.045(11) 0.009(10) -0.040(9) -0.012(11) C73 0.042 0.063(14) 0.025(10) -0.009(10) -0.027(7) 0.013(10) C74 0.013(8) 0.071(15) 0.041(11) -0.017(11) -0.008(7) -0.010(9) C75 0.025(9) 0.066(14) 0.040(11) -0.003(10) -0.016(8) -0.020(10) C76 0.040 0.063(14) 0.046 -0.024(10) -0.036(6) -0.003(10) C77 0.061(12) 0.038(12) 0.025(9) -0.016(8) -0.012(8) -0.016(10) C78 0.038(7) 0.052(9) 0.024(6) -0.003(6) -0.002(5) -0.024(7) C79 0.033(10) 0.054(13) 0.025(9) -0.014(9) -0.008(7) 0.008(9) C80 0.020(8) 0.062(14) 0.025(9) -0.009(9) 0.007(7) -0.006(9) C81 0.033(10) 0.026(11) 0.049(12) -0.002(9) 0.003(8) 0.013(8) C82 0.042(11) 0.022(11) 0.049(11) -0.008(8) -0.016(9) 0.000(8) C83 0.054(12) 0.042(12) 0.036(10) -0.006(9) -0.011(9) -0.036(10) C84 0.036(10) 0.044(12) 0.050(11) 0.007(9) -0.023(9) -0.024(9) C85 0.075(16) 0.076(19) 0.071(16) -0.002(14) -0.020(13) 0.018(14) C86 0.042(16) 0.09(2) 0.032(15) -0.005(15) -0.002(12) -0.019(16) N1 0.030(7) 0.045(10) 0.040(8) 0.007(7) -0.019(6) -0.023(7) O1 0.074(10) 0.056(11) 0.062(9) -0.020(8) -0.005(7) -0.015(9) O2 0.058(10) 0.100(15) 0.098(13) -0.013(11) 0.014(9) 0.015(10) O3 0.077(10) 0.079(11) 0.042(8) 0.011(7) -0.012(7) -0.050(9) P1 0.030(2) 0.032(3) 0.022(2) -0.0004(19) -0.0071(17) -0.012(2) Ru1 0.0275(8) 0.0488(11) 0.0280(8) -0.0025(7) -0.0060(6) -0.0141(7) S3 0.054(3) 0.059(4) 0.065(4) -0.010(3) -0.016(3) -0.005(3) S2 0.084(5) 0.071(5) 0.095(5) -0.004(4) -0.024(4) -0.016(4) S1 0.186(10) 0.073(6) 0.172(9) 0.000(6) -0.111(8) -0.002(6) _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 C1 O1 1.17(2) . ? C1 Ru1 1.89(2) . ? C2 O2 1.13(2) . ? C2 Ru1 1.91(2) . ? C3 O3 1.17(2) . ? C3 Ru1 1.93(2) . ? C4 C9 1.39(2) . ? C4 C5 1.42(2) . ? C4 P1 1.852(17) . ? C5 C6 1.40(2) . ? C5 C22 1.49(2) . ? C6 C7 1.37(2) . ? C6 H6 0.9500 . ? C7 C8 1.37(2) . ? C7 H7 0.9500 . ? C8 C9 1.35(2) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.39(2) . ? C10 C11 1.40(2) . ? C10 P1 1.820(15) . ? C11 C12 1.36(2) . ? C11 H11 0.9500 . ? C12 C13 1.34(2) . ? C12 H12 0.9500 . ? C13 C14 1.38(2) . ? C13 H13 0.9500 . ? C14 C15 1.40(2) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.40(2) . ? C16 C17 1.40(2) . ? C16 P1 1.838(16) . ? C17 C18 1.35(2) . ? C17 H17 0.9500 . ? C18 C19 1.38(2) . ? C18 H18 0.9500 . ? C19 C20 1.37(2) . ? C19 H19 0.9500 . ? C20 C21 1.37(2) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 N1 1.418(18) . ? C22 C26 1.586(19) . ? C22 H22 1.0000 . ? C23 N1 1.471(18) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 H23C 0.8326 . ? C24 N1 1.477(19) . ? C24 C25 1.56(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C33 1.50(2) . ? C25 C30 1.53(2) . ? C25 C26 1.64(2) . ? C26 C36 1.54(2) . ? C26 C27 1.55(2) . ? C27 C28 1.41(2) . ? C27 C38 1.50(2) . ? C27 Ru1 2.235(16) . ? C28 C29 1.52(2) . ? C28 C41 1.53(2) . ? C28 Ru1 2.173(14) . ? C29 C30 1.35(2) . ? C29 C43 1.47(2) . ? C30 C31 1.45(2) . ? C31 C45 1.41(2) . ? C31 C32 1.43(2) . ? C32 C48 1.39(2) . ? C32 C33 1.43(2) . ? C33 C34 1.36(2) . ? C34 C50 1.45(2) . ? C34 C35 1.48(2) . ? C35 C36 1.39(2) . ? C35 C52 1.42(2) . ? C36 C37 1.45(2) . ? C37 C54 1.40(2) . ? C37 C38 1.44(2) . ? C38 C39 1.36(2) . ? C39 C56 1.45(2) . ? C39 C40 1.46(2) . ? C40 C41 1.40(2) . ? C40 C58 1.43(2) . ? C41 C42 1.41(2) . ? C42 C60 1.41(2) . ? C42 C43 1.42(3) . ? C43 C44 1.40(2) . ? C44 C45 1.41(2) . ? C44 C62 1.46(2) . ? C45 C46 1.51(2) . ? C46 C47 1.34(3) . ? C46 C63 1.43(3) . ? C47 C48 1.40(2) . ? C47 C66 1.50(3) . ? C48 C49 1.46(2) . ? C49 C50 1.41(2) . ? C49 C67 1.44(2) . ? C50 C51 1.44(2) . ? C51 C80 1.43(2) . ? C51 C52 1.44(2) . ? C52 C53 1.42(2) . ? C53 C81 1.40(2) . ? C53 C54 1.46(2) . ? C54 C55 1.43(2) . ? C55 C56 1.38(2) . ? C55 C82 1.50(2) . ? C56 C57 1.40(2) . ? C57 C84 1.40(2) . ? C57 C58 1.45(2) . ? C58 C59 1.38(2) . ? C59 C60 1.43(2) . ? C59 C74 1.47(2) . ? C60 C61 1.48(2) . ? C61 C62 1.37(3) . ? C61 C73 1.45(2) . ? C62 C63 1.43(3) . ? C63 C64 1.40(2) . ? C64 C65 1.43(2) . ? C64 C72 1.44(2) . ? C65 C66 1.36(2) . ? C65 C70 1.50(2) . ? C66 C67 1.44(3) . ? C67 C68 1.42(2) . ? C68 C69 1.42(2) . ? C68 C80 1.42(2) . ? C69 C70 1.36(2) . ? C69 C78 1.46(2) . ? C70 C71 1.43(2) . ? C71 C76 1.38(2) . ? C71 C72 1.48(2) . ? C72 C73 1.41(2) . ? C73 C74 1.43(3) . ? C74 C75 1.38(2) . ? C75 C84 1.45(2) . ? C75 C76 1.46(2) . ? C76 C77 1.40(2) . ? C77 C78 1.41(2) . ? C77 C83 1.51(2) . ? C78 C79 1.43(2) . ? C79 C81 1.41(2) . ? C79 C80 1.42(2) . ? C81 C82 1.47(2) . ? C82 C83 1.35(2) . ? C83 C84 1.43(2) . ? C85 S2 1.53(3) . ? C85 S1 1.54(3) . ? C86 S3 1.533(5) . ? C86 S3 1.533(5) 2_667 ? P1 Ru1 2.415(4) . ? 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 O1 C1 Ru1 169.5(18) . . ? O2 C2 Ru1 178(2) . . ? O3 C3 Ru1 174.5(18) . . ? C9 C4 C5 119.9(15) . . ? C9 C4 P1 120.5(12) . . ? C5 C4 P1 119.4(12) . . ? C6 C5 C4 117.6(14) . . ? C6 C5 C22 118.6(14) . . ? C4 C5 C22 123.8(13) . . ? C7 C6 C5 121.3(15) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 119.3(16) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C9 C8 C7 122.3(17) . . ? C9 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C8 C9 C4 119.5(16) . . ? C8 C9 H9 120.2 . . ? C4 C9 H9 120.2 . . ? C15 C10 C11 117.3(14) . . ? C15 C10 P1 120.0(11) . . ? C11 C10 P1 122.6(13) . . ? C12 C11 C10 122.1(17) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C13 C12 C11 120.3(16) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.4(15) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 120.2(17) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C10 C15 C14 119.4(16) . . ? C10 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C21 C16 C17 119.7(15) . . ? C21 C16 P1 119.0(11) . . ? C17 C16 P1 121.1(12) . . ? C18 C17 C16 118.6(16) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C17 C18 C19 122.4(16) . . ? C17 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C20 C19 C18 118.7(16) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? C19 C20 C21 121.1(17) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C16 119.3(15) . . ? C20 C21 H21 120.4 . . ? C16 C21 H21 120.4 . . ? N1 C22 C5 118.6(12) . . ? N1 C22 C26 105.1(10) . . ? C5 C22 C26 112.9(12) . . ? N1 C22 H22 106.5 . . ? C5 C22 H22 106.5 . . ? C26 C22 H22 106.5 . . ? N1 C23 H23A 111.0 . . ? N1 C23 H23B 111.2 . . ? H23A C23 H23B 108.6 . . ? N1 C23 H23C 105.4 . . ? H23A C23 H23C 110.3 . . ? H23B C23 H23C 110.3 . . ? N1 C24 C25 101.5(13) . . ? N1 C24 H24A 111.5 . . ? C25 C24 H24A 111.5 . . ? N1 C24 H24B 111.5 . . ? C25 C24 H24B 111.5 . . ? H24A C24 H24B 109.3 . . ? C33 C25 C30 100.4(12) . . ? C33 C25 C24 108.1(12) . . ? C30 C25 C24 116.1(14) . . ? C33 C25 C26 116.2(14) . . ? C30 C25 C26 113.3(12) . . ? C24 C25 C26 103.3(11) . . ? C36 C26 C27 104.6(12) . . ? C36 C26 C22 110.1(12) . . ? C27 C26 C22 115.8(12) . . ? C36 C26 C25 111.4(12) . . ? C27 C26 C25 116.0(12) . . ? C22 C26 C25 99.0(11) . . ? C28 C27 C38 115.5(13) . . ? C28 C27 C26 123.6(14) . . ? C38 C27 C26 105.7(14) . . ? C28 C27 Ru1 68.9(9) . . ? C38 C27 Ru1 119.2(10) . . ? C26 C27 Ru1 121.2(10) . . ? C27 C28 C29 117.4(13) . . ? C27 C28 C41 119.9(14) . . ? C29 C28 C41 101.8(12) . . ? C27 C28 Ru1 73.7(9) . . ? C29 C28 Ru1 127.5(10) . . ? C41 C28 Ru1 116.3(10) . . ? C30 C29 C43 119.5(15) . . ? C30 C29 C28 123.8(14) . . ? C43 C29 C28 108.2(14) . . ? C29 C30 C31 120.5(14) . . ? C29 C30 C25 124.8(15) . . ? C31 C30 C25 108.4(14) . . ? C45 C31 C32 120.4(15) . . ? C45 C31 C30 119.8(16) . . ? C32 C31 C30 109.1(14) . . ? C48 C32 C33 124.2(18) . . ? C48 C32 C31 119.9(15) . . ? C33 C32 C31 106.8(14) . . ? C34 C33 C32 117.6(15) . . ? C34 C33 C25 124.5(15) . . ? C32 C33 C25 111.9(16) . . ? C33 C34 C50 121.7(15) . . ? C33 C34 C35 120.6(15) . . ? C50 C34 C35 107.1(15) . . ? C36 C35 C52 120.5(15) . . ? C36 C35 C34 119.6(16) . . ? C52 C35 C34 106.7(14) . . ? C35 C36 C37 119.8(14) . . ? C35 C36 C26 125.2(14) . . ? C37 C36 C26 108.6(13) . . ? C54 C37 C38 122.7(13) . . ? C54 C37 C36 118.9(13) . . ? C38 C37 C36 109.2(14) . . ? C39 C38 C37 117.7(14) . . ? C39 C38 C27 125.0(15) . . ? C37 C38 C27 110.6(13) . . ? C38 C39 C56 122.3(15) . . ? C38 C39 C40 118.2(16) . . ? C56 C39 C40 104.9(14) . . ? C41 C40 C58 117.8(17) . . ? C41 C40 C39 121.0(15) . . ? C58 C40 C39 109.8(16) . . ? C40 C41 C42 122.1(15) . . ? C40 C41 C28 119.0(15) . . ? C42 C41 C28 110.5(15) . . ? C41 C42 C60 118.4(18) . . ? C41 C42 C43 109.5(14) . . ? C60 C42 C43 121.9(16) . . ? C44 C43 C42 120.5(16) . . ? C44 C43 C29 120.6(16) . . ? C42 C43 C29 108.9(15) . . ? C43 C44 C45 119.1(15) . . ? C43 C44 C62 117.9(17) . . ? C45 C44 C62 108.1(15) . . ? C31 C45 C44 120.3(16) . . ? C31 C45 C46 118.1(17) . . ? C44 C45 C46 108.8(15) . . ? C47 C46 C63 125.0(19) . . ? C47 C46 C45 117.6(16) . . ? C63 C46 C45 104.8(15) . . ? C46 C47 C48 124.5(18) . . ? C46 C47 C66 117.7(17) . . ? C48 C47 C66 107.1(19) . . ? C32 C48 C47 119.4(17) . . ? C32 C48 C49 117.1(15) . . ? C47 C48 C49 110.7(15) . . ? C50 C49 C67 119.6(17) . . ? C50 C49 C48 119.5(14) . . ? C67 C49 C48 106.0(15) . . ? C49 C50 C51 120.4(14) . . ? C49 C50 C34 119.7(16) . . ? C51 C50 C34 108.4(13) . . ? C50 C51 C80 119.9(14) . . ? C50 C51 C52 107.6(14) . . ? C80 C51 C52 121.0(15) . . ? C53 C52 C35 122.1(16) . . ? C53 C52 C51 117.9(15) . . ? C35 C52 C51 110.1(16) . . ? C81 C53 C52 120.9(16) . . ? C81 C53 C54 109.5(15) . . ? C52 C53 C54 116.1(15) . . ? C37 C54 C55 117.0(14) . . ? C37 C54 C53 122.2(14) . . ? C55 C54 C53 108.1(13) . . ? C56 C55 C54 122.0(15) . . ? C56 C55 C82 117.4(14) . . ? C54 C55 C82 107.4(13) . . ? C55 C56 C57 124.1(16) . . ? C55 C56 C39 117.8(15) . . ? C57 C56 C39 109.8(16) . . ? C56 C57 C84 118.6(16) . . ? C56 C57 C58 109.2(15) . . ? C84 C57 C58 120.1(16) . . ? C59 C58 C40 121.8(18) . . ? C59 C58 C57 119.8(15) . . ? C40 C58 C57 106.2(15) . . ? C58 C59 C60 118.8(15) . . ? C58 C59 C74 120.3(17) . . ? C60 C59 C74 108.2(15) . . ? C42 C60 C59 120.9(17) . . ? C42 C60 C61 118.1(18) . . ? C59 C60 C61 108.0(16) . . ? C62 C61 C73 121.1(18) . . ? C62 C61 C60 118.9(17) . . ? C73 C61 C60 107.0(18) . . ? C61 C62 C63 120.1(18) . . ? C61 C62 C44 122.5(18) . . ? C63 C62 C44 107.2(17) . . ? C64 C63 C46 117.3(17) . . ? C64 C63 C62 120.3(17) . . ? C46 C63 C62 111.1(15) . . ? C63 C64 C65 118.8(17) . . ? C63 C64 C72 119.5(16) . . ? C65 C64 C72 108.9(17) . . ? C66 C65 C64 124.2(18) . . ? C66 C65 C70 118.2(17) . . ? C64 C65 C70 107.8(16) . . ? C65 C66 C67 122.6(18) . . ? C65 C66 C47 116.9(17) . . ? C67 C66 C47 106.2(16) . . ? C68 C67 C49 120.1(17) . . ? C68 C67 C66 118.5(17) . . ? C49 C67 C66 110.0(18) . . ? C67 C68 C69 119.4(16) . . ? C67 C68 C80 120.6(15) . . ? C69 C68 C80 108.8(16) . . ? C70 C69 C68 122.3(18) . . ? C70 C69 C78 118.9(16) . . ? C68 C69 C78 106.7(14) . . ? C69 C70 C71 121.1(18) . . ? C69 C70 C65 118.8(16) . . ? C71 C70 C65 107.2(16) . . ? C76 C71 C70 120.5(16) . . ? C76 C71 C72 119.7(16) . . ? C70 C71 C72 107.9(16) . . ? C73 C72 C64 120.3(17) . . ? C73 C72 C71 118.7(17) . . ? C64 C72 C71 108.2(16) . . ? C72 C73 C74 120.3(17) . . ? C72 C73 C61 118.5(19) . . ? C74 C73 C61 109.2(15) . . ? C75 C74 C73 121.2(16) . . ? C75 C74 C59 119.8(16) . . ? C73 C74 C59 107.6(16) . . ? C74 C75 C84 120.0(16) . . ? C74 C75 C76 119.4(17) . . ? C84 C75 C76 108.0(15) . . ? C71 C76 C77 119.6(17) . . ? C71 C76 C75 120.7(17) . . ? C77 C76 C75 108.3(16) . . ? C76 C77 C78 121.1(17) . . ? C76 C77 C83 108.9(16) . . ? C78 C77 C83 117.9(14) . . ? C77 C78 C79 121.0(15) . . ? C77 C78 C69 118.7(16) . . ? C79 C78 C69 108.0(14) . . ? C81 C79 C80 119.0(15) . . ? C81 C79 C78 121.1(16) . . ? C80 C79 C78 107.6(15) . . ? C68 C80 C79 108.9(14) . . ? C68 C80 C51 119.3(16) . . ? C79 C80 C51 119.5(15) . . ? C53 C81 C79 121.6(17) . . ? C53 C81 C82 108.9(15) . . ? C79 C81 C82 117.9(15) . . ? C83 C82 C81 122.2(15) . . ? C83 C82 C55 117.6(15) . . ? C81 C82 C55 106.0(13) . . ? C82 C83 C84 123.4(15) . . ? C82 C83 C77 119.8(15) . . ? C84 C83 C77 106.0(15) . . ? C57 C84 C83 118.9(14) . . ? C57 C84 C75 120.0(17) . . ? C83 C84 C75 108.8(15) . . ? S2 C85 S1 177.4(18) . . ? S3 C86 S3 180.0(4) . 2_667 ? C22 N1 C23 112.1(12) . . ? C22 N1 C24 102.0(11) . . ? C23 N1 C24 109.6(13) . . ? C10 P1 C16 102.4(7) . . ? C10 P1 C4 101.5(7) . . ? C16 P1 C4 103.0(7) . . ? C10 P1 Ru1 115.5(5) . . ? C16 P1 Ru1 114.2(5) . . ? C4 P1 Ru1 118.1(5) . . ? C1 Ru1 C2 84.2(9) . . ? C1 Ru1 C3 169.4(9) . . ? C2 Ru1 C3 85.9(9) . . ? C1 Ru1 C28 86.7(7) . . ? C2 Ru1 C28 117.2(7) . . ? C3 Ru1 C28 94.6(6) . . ? C1 Ru1 C27 96.7(7) . . ? C2 Ru1 C27 154.0(7) . . ? C3 Ru1 C27 90.6(7) . . ? C28 Ru1 C27 37.4(5) . . ? C1 Ru1 P1 95.4(6) . . ? C2 Ru1 P1 107.8(6) . . ? C3 Ru1 P1 91.1(6) . . ? C28 Ru1 P1 134.9(4) . . ? C27 Ru1 P1 98.0(4) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.267 _refine_diff_density_min -1.209 _refine_diff_density_rms 0.171