# 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 #TrackingRef '- Complex11_ligando_CCDC806039.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2010-10-12 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? _publ_contact_author_name 'Fernando Lopez Ortiz' _publ_contact_author_address ;\'Area de Qu\'imica Org\'anica Universidad de Almer\'ia Crta. Sacramento s/n, 04230 Almer\'ia, Spain ; _publ_contact_author_email flortiz@ulal.es _publ_contact_author_phone 0034950015481 _publ_contact_author_fax 0034950015478 loop_ _publ_author_name _publ_author_address C.Popovici ;\'Area de Qu\'imica Org\'anica Universidad de Almer\'ia Crta. Sacramento s/n, 04230 Almer\'ia, Spain ; I.Fernandez ;\'Area de Qu\'imica Org\'anica Universidad de Almer\'ia Crta. Sacramento s/n, 04230 Almer\'ia, Spain ; P.Ona-Burgos ;\'Area de Qu\'imica Org\'anica Universidad de Almer\'ia Crta. Sacramento s/n, 04230 Almer\'ia, Spain ; L.Roces ;Departamento de Qu\'imica F\'isica y Anal\'itica Universidad de Oviedo Juli\'an Claver\'ia 8, 33006 Oviedo, Spain ; S.Garcia-Granda ;Departamento de Qu\'imica F\'isica y Anal\'itica Universidad de Oviedo Juli\'an Claver\'ia 8, 33006 Oviedo, Spain ; F.Lopez-Ortiz ;\'Area de Qu\'imica Org\'anica Universidad de Almer\'ia Crta. Sacramento s/n, 04230 Almer\'ia, Spain ; _publ_section_title ; Synthesis and structure of tridentate bis(phosphinic amide)-phosphine oxide complexes of yttrium nitrate. Applications of 31P,89Y NMR methods in structural elucidation in solution ; _publ_section_references ; Blessing, R. H. (1995) Acta Cryst., A51, 33-38. Blessing, R. H. (1987) Cryst. Rev. 1, 3-58. Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397. Bruker (2007) APEX2 (Version 2.1-4), SAINT (version 7.34A), SADABS (version 2007/4), BrukerAXS Inc, Madison, Wisconsin, USA. Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358. Flack H. D. & Bernardinelli, G. (71999). Acta Cryst. A55, 908-915. Flack H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148. Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580 LePage, Y. (1987). J. Appl. Cryst. 20, 264-269. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst, A24, 351-359 Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr. 34, 824-828 Streltsov, V. A. & Zavodnik, V. E. (1990) Sov. Phys. Crystallogr. 35, 281. ABSCOR: Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. APEX, APEX2, SMART, SAINT, SAINT-Plus: Bruker (2007). Program name(s). Bruker AXS Inc., Madison, Wisconsin, USA. [Older versions (pre-1997) should refer to Siemens Analytical X-ray Instruments Inc. instead of Bruker AXS.] CAD-4 Software: Enraf-Nonius (1989). CAD-4 Software (or CAD-4 EXPRESS). Enraf-Nonius, Delft, The Netherlands. Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. CAMERON: Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. Chemical Crystallography Laboratory, Oxford, England. CrysAlis CCD, CrysAlis RED and associated programs: Oxford Diffraction (2006). Program name(s). Oxford Diffraction Ltd, Abingdon, England. CRYSTALS: Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487. COLLECT: Nonius [or Hooft, R. W. W.] (1998). COLLECT. Nonius BV, Delft, The Netherlands. DENZO/SCALEPACK: Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press. DIAMOND: Brandenburg, K. [or Brandenburg, K. & Putz, H., or Brandenburg, K. & Berndt, M.] (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. DIF4 and REDU4: Stoe & Cie (1991). Program name(s). Stoe & Cie, Darmstadt, Germany. DIFABS: Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158 - 166. DIRAX: Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96. DIRDIF99: Beurskens, P.T., Beurskens, G., de Gelder, R., Garci\'ia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M. (1999) The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338. EVALCCD: Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220-229. JANA2000: Petricek, V. & Dusek, M. (2000). JANA2000. Institute of Physics, Czech Academy of Sciences, Prague, Czech Republic. Mercury: Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457. Mogul: Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell, W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris, S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144. ORTEPII: Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ORTEPIII: Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. PROCESS: Rigaku (1996). PROCESS. Rigaku Corporation, Tokyo, Japan. PROCESS-AUTO: Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. publCIF: Westrip, S. P. (2008). publCIF. In preparation. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of G ttingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. SIR2002: Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103. SUPERFLIP Palatinus, L. & Chapuis, G. (2007) J. Appl. Cryst. 40, 786-790. TEXSAN: Molecular Structure Corporation & Rigaku (2000). TEXSAN. MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. X-AREA, X-RED, X-RED32, X-SHAPE: Stoe & Cie (2002). Program name(s). Stoe & Cie GmbH, Darmstadt, Germany. XCAD4: Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany. XSCANS: Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _publ_requested_category FO #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_lil2m _database_code_depnum_ccdc_archive 'CCDC 806039' #TrackingRef '- Complex11_ligando_CCDC806039.cif' _audit_creation_date 2010-10-12T20:51:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C42 H51 N2 O3 P3' _chemical_formula_moiety 'C42 H51 N2 O3 P3' _chemical_formula_weight 724.76 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.567(2) _cell_length_b 19.623(3) _cell_length_c 14.296(2) _cell_angle_alpha 90 _cell_angle_beta 90.334(4) _cell_angle_gamma 90 _cell_volume 3806.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_hall '-P 2ybc ' #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_crystal_colour colourless _exptl_crystal_description prism _exptl_crystal_size_max 0.204 _exptl_crystal_size_mid 0.174 _exptl_crystal_size_min 0.064 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.198 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Linear fit to sin(theta)/lambda - 12 parameters ; _exptl_absorpt_correction_T_min 0.7051 _exptl_absorpt_correction_T_max 1.1197 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_unetI/netI 0.1377 _diffrn_reflns_number 19397 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 25.71 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.926 _diffrn_measured_fraction_theta_max 0.865 _reflns_number_total 6271 _reflns_number_gt 3686 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0005P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6271 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.0623 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_restrained_S_all 0.877 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.349 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.053 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 P1 P -0.30654(5) 0.07161(4) -0.11345(6) 0.0173(2) Uani 1 1 d . . . P2 P -0.28845(5) 0.02657(4) -0.37893(6) 0.0146(2) Uani 1 1 d . . . P3 P -0.19232(5) -0.13891(4) -0.39780(6) 0.0176(2) Uani 1 1 d . . . O1 O -0.36716(12) 0.09003(9) -0.02919(14) 0.0222(5) Uani 1 1 d . . . O2 O -0.19343(11) 0.04760(8) -0.34765(13) 0.0146(5) Uani 1 1 d . . . O3 O -0.20301(12) -0.10270(9) -0.30309(13) 0.0190(5) Uani 1 1 d . . . N1 N -0.20270(14) 0.04414(11) -0.07814(17) 0.0150(6) Uani 1 1 d . . . N2 N -0.08734(14) -0.16625(11) -0.43047(17) 0.0174(6) Uani 1 1 d . . . C1 C -0.36563(18) 0.00400(13) -0.1854(2) 0.0144(8) Uani 1 1 d . . . C2 C -0.36319(17) -0.01340(13) -0.2867(2) 0.0140(8) Uani 1 1 d . . . C3 C -0.42536(18) -0.06214(13) -0.3234(2) 0.0174(8) Uani 1 1 d . . . H3 H -0.4243 -0.0732 -0.388 0.021 Uiso 1 1 calc R . . C4 C -0.48920(18) -0.09437(14) -0.2631(2) 0.0202(8) Uani 1 1 d . . . H4 H -0.5332 -0.1277 -0.2874 0.024 Uiso 1 1 calc R . . C5 C -0.49134(18) -0.07901(13) -0.1635(2) 0.0200(8) Uani 1 1 d . . . H5 H -0.5353 -0.1029 -0.1238 0.024 Uiso 1 1 calc R . . C6 C -0.43041(17) -0.03035(13) -0.1271(2) 0.0189(8) Uani 1 1 d . . . H6 H -0.4323 -0.02 -0.0622 0.023 Uiso 1 1 calc R . . C7 C -0.29688(19) 0.14748(13) -0.1890(2) 0.0152(7) Uani 1 1 d . . . C8 C -0.38058(19) 0.17982(14) -0.2130(2) 0.0196(8) Uani 1 1 d . . . H8 H -0.4418 0.1588 -0.1991 0.024 Uiso 1 1 calc R . . C9 C -0.3810(2) 0.24314(14) -0.2574(2) 0.0208(8) Uani 1 1 d . . . H9 H -0.442 0.2633 -0.2749 0.025 Uiso 1 1 calc R . . C10 C -0.2976(2) 0.27567(14) -0.2756(2) 0.0237(8) Uani 1 1 d . . . H10 H -0.2976 0.3196 -0.3035 0.028 Uiso 1 1 calc R . . C11 C -0.2137(2) 0.24406(14) -0.2531(2) 0.0252(9) Uani 1 1 d . . . H11 H -0.1527 0.2657 -0.2663 0.03 Uiso 1 1 calc R . . C12 C -0.21328(18) 0.17986(14) -0.2106(2) 0.0186(8) Uani 1 1 d . . . H12 H -0.152 0.1587 -0.1966 0.022 Uiso 1 1 calc R . . C13 C -0.1646(2) 0.06347(14) 0.0204(2) 0.0232(8) Uani 1 1 d . . . H13 H -0.0949 0.0468 0.0226 0.028 Uiso 1 1 calc R . . C14 C -0.21590(19) 0.02927(14) 0.1057(2) 0.0335(9) Uani 1 1 d . . . H14A H -0.219 -0.0201 0.0959 0.05 Uiso 1 1 calc R . . H14B H -0.2828 0.0474 0.1119 0.05 Uiso 1 1 calc R . . H14C H -0.1781 0.039 0.1628 0.05 Uiso 1 1 calc R . . C15 C -0.15764(19) 0.14005(14) 0.0350(2) 0.0296(9) Uani 1 1 d . . . H15A H -0.1246 0.1609 -0.0187 0.044 Uiso 1 1 calc R . . H15B H -0.1198 0.1495 0.0921 0.044 Uiso 1 1 calc R . . H15C H -0.2241 0.1591 0.0409 0.044 Uiso 1 1 calc R . . C16 C -0.14773(18) -0.00567(13) -0.1357(2) 0.0181(8) Uani 1 1 d . . . H16 H -0.188 -0.0157 -0.1929 0.022 Uiso 1 1 calc R . . C17 C -0.13618(19) -0.07289(13) -0.0793(2) 0.0289(9) Uani 1 1 d . . . H17A H -0.2014 -0.0896 -0.0612 0.043 Uiso 1 1 calc R . . H17B H -0.0964 -0.0643 -0.0231 0.043 Uiso 1 1 calc R . . H17C H -0.1034 -0.1071 -0.1182 0.043 Uiso 1 1 calc R . . C18 C -0.05340(16) 0.02316(13) -0.1658(2) 0.0232(8) Uani 1 1 d . . . H18A H -0.0654 0.0654 -0.2007 0.035 Uiso 1 1 calc R . . H18B H -0.0194 -0.0096 -0.206 0.035 Uiso 1 1 calc R . . H18C H -0.0124 0.033 -0.1108 0.035 Uiso 1 1 calc R . . C19 C -0.28527(18) -0.02786(14) -0.4911(2) 0.0145(7) Uani 1 1 d . . . C20 C -0.23211(18) -0.08842(13) -0.5019(2) 0.0140(7) Uani 1 1 d . . . C21 C -0.21786(19) -0.11381(14) -0.5964(2) 0.0193(8) Uani 1 1 d . . . H21 H -0.1797 -0.1541 -0.603 0.023 Uiso 1 1 calc R . . C22 C -0.25542(18) -0.08423(14) -0.6794(2) 0.0214(8) Uani 1 1 d . . . H22 H -0.2415 -0.1029 -0.7392 0.026 Uiso 1 1 calc R . . C23 C -0.31224(18) -0.02801(14) -0.6696(2) 0.0219(8) Uani 1 1 d . . . H23 H -0.343 -0.0075 -0.7224 0.026 Uiso 1 1 calc R . . C24 C -0.32512(18) 0.00000(14) -0.5773(2) 0.0179(8) Uani 1 1 d . . . H24 H -0.3632 0.0404 -0.5725 0.021 Uiso 1 1 calc R . . C25 C -0.35715(18) 0.09883(13) -0.4202(2) 0.0130(7) Uani 1 1 d . . . C26 C -0.45427(18) 0.10120(14) -0.4163(2) 0.0180(8) Uani 1 1 d . . . H26 H -0.4904 0.0656 -0.3873 0.022 Uiso 1 1 calc R . . C27 C -0.5021(2) 0.15640(14) -0.4553(2) 0.0219(8) Uani 1 1 d . . . H27 H -0.572 0.158 -0.4518 0.026 Uiso 1 1 calc R . . C28 C -0.4543(2) 0.20925(14) -0.4991(2) 0.0236(8) Uani 1 1 d . . . H28 H -0.4902 0.2461 -0.5258 0.028 Uiso 1 1 calc R . . C29 C -0.3579(2) 0.20735(14) -0.5030(2) 0.0242(8) Uani 1 1 d . . . H29 H -0.3222 0.2429 -0.5326 0.029 Uiso 1 1 calc R . . C30 C -0.30917(19) 0.15286(13) -0.4635(2) 0.0174(8) Uani 1 1 d . . . H30 H -0.2392 0.1521 -0.4659 0.021 Uiso 1 1 calc R . . C31 C -0.26697(18) -0.21424(14) -0.3997(2) 0.0187(8) Uani 1 1 d . . . C32 C -0.28028(19) -0.25613(14) -0.4806(2) 0.0243(8) Uani 1 1 d . . . H32 H -0.2503 -0.244 -0.5381 0.029 Uiso 1 1 calc R . . C33 C -0.33622(18) -0.31358(14) -0.4748(3) 0.0303(9) Uani 1 1 d . . . H33 H -0.3462 -0.3418 -0.528 0.036 Uiso 1 1 calc R . . C34 C -0.3792(2) -0.33021(15) -0.3877(3) 0.0323(10) Uani 1 1 d . . . H34 H -0.4169 -0.3708 -0.3833 0.039 Uiso 1 1 calc R . . C35 C -0.36831(19) -0.28885(15) -0.3065(3) 0.0296(9) Uani 1 1 d . . . H35 H -0.3988 -0.3015 -0.2494 0.035 Uiso 1 1 calc R . . C36 C -0.31271(18) -0.23003(14) -0.3121(2) 0.0224(8) Uani 1 1 d . . . H36 H -0.305 -0.2009 -0.2595 0.027 Uiso 1 1 calc R . . C37 C -0.0409(2) -0.22387(14) -0.3769(2) 0.0270(9) Uani 1 1 d . . . H37 H 0.0314 -0.2191 -0.3885 0.032 Uiso 1 1 calc R . . C38 C -0.06753(19) -0.29372(13) -0.4168(3) 0.0505(12) Uani 1 1 d . . . H38A H -0.059 -0.2933 -0.4848 0.076 Uiso 1 1 calc R . . H38B H -0.1363 -0.3043 -0.402 0.076 Uiso 1 1 calc R . . H38C H -0.0243 -0.3284 -0.3891 0.076 Uiso 1 1 calc R . . C39 C -0.0513(2) -0.22047(16) -0.2657(2) 0.0469(11) Uani 1 1 d . . . H39A H -0.0332 -0.1748 -0.2438 0.07 Uiso 1 1 calc R . . H39B H -0.0075 -0.2543 -0.2369 0.07 Uiso 1 1 calc R . . H39C H -0.1196 -0.2302 -0.2484 0.07 Uiso 1 1 calc R . . C40 C -0.02001(19) -0.11619(14) -0.4747(2) 0.0236(8) Uani 1 1 d . . . H40 H -0.0627 -0.0789 -0.5001 0.028 Uiso 1 1 calc R . . C41 C 0.03129(19) -0.14905(15) -0.5598(2) 0.0373(10) Uani 1 1 d . . . H41A H -0.0186 -0.1674 -0.6027 0.056 Uiso 1 1 calc R . . H41B H 0.0744 -0.186 -0.5383 0.056 Uiso 1 1 calc R . . H41C H 0.0707 -0.1146 -0.5922 0.056 Uiso 1 1 calc R . . C42 C 0.04658(18) -0.08336(14) -0.4006(2) 0.0336(9) Uani 1 1 d . . . H42A H 0.0059 -0.0636 -0.3511 0.05 Uiso 1 1 calc R . . H42B H 0.0862 -0.0474 -0.4296 0.05 Uiso 1 1 calc R . . H42C H 0.0903 -0.118 -0.3737 0.05 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0193(4) 0.0200(5) 0.0127(6) -0.0007(4) 0.0012(4) 0.0001(4) P2 0.0178(4) 0.0154(5) 0.0106(5) 0.0016(4) 0.0010(4) 0.0002(4) P3 0.0184(4) 0.0162(5) 0.0182(6) 0.0013(4) 0.0003(4) 0.0011(4) O1 0.0223(10) 0.0281(13) 0.0162(14) -0.0027(11) 0.0072(10) 0.0004(9) O2 0.0104(9) 0.0174(12) 0.0160(14) 0.0014(10) -0.0004(10) -0.0004(8) O3 0.0221(10) 0.0189(12) 0.0159(14) -0.0028(10) 0.0005(10) 0.0027(9) N1 0.0164(12) 0.0190(15) 0.0097(17) 0.0001(12) -0.0037(12) 0.0007(11) N2 0.0140(12) 0.0113(14) 0.0268(19) 0.0059(13) 0.0006(13) 0.0002(11) C1 0.0116(14) 0.0125(17) 0.019(2) 0.0041(16) -0.0029(15) 0.0002(12) C2 0.0106(14) 0.0104(17) 0.021(2) 0.0053(15) -0.0020(15) 0.0003(13) C3 0.0223(16) 0.0120(18) 0.018(2) 0.0000(16) -0.0011(16) 0.0009(13) C4 0.0162(15) 0.0180(18) 0.026(2) -0.0002(17) -0.0005(16) -0.0026(13) C5 0.0176(16) 0.0157(18) 0.027(2) 0.0067(17) 0.0041(16) -0.0037(14) C6 0.0203(15) 0.0210(18) 0.015(2) -0.0010(16) 0.0015(16) 0.0037(14) C7 0.0215(16) 0.0147(17) 0.009(2) -0.0059(15) -0.0006(15) 0.0025(14) C8 0.0169(16) 0.0242(19) 0.018(2) -0.0059(17) 0.0008(16) 0.0002(14) C9 0.0229(17) 0.0213(19) 0.018(2) -0.0034(17) -0.0034(16) 0.0059(15) C10 0.0335(18) 0.0144(19) 0.023(2) -0.0003(17) -0.0020(18) 0.0008(15) C11 0.0216(17) 0.025(2) 0.029(2) 0.0052(18) 0.0001(17) -0.0032(15) C12 0.0144(15) 0.0232(19) 0.018(2) 0.0003(17) -0.0018(15) 0.0026(14) C13 0.0221(16) 0.029(2) 0.019(2) -0.0033(18) -0.0024(17) 0.0013(15) C14 0.0360(19) 0.044(2) 0.021(2) 0.0051(19) -0.0031(18) 0.0003(17) C15 0.0250(17) 0.039(2) 0.024(2) -0.0115(19) -0.0004(17) -0.0040(16) C16 0.0190(16) 0.0175(18) 0.018(2) 0.0001(16) -0.0050(16) 0.0022(14) C17 0.0316(18) 0.021(2) 0.034(2) -0.0016(18) -0.0102(18) 0.0036(15) C18 0.0202(15) 0.0261(19) 0.023(2) -0.0044(17) -0.0032(16) 0.0072(15) C19 0.0152(15) 0.0168(18) 0.011(2) 0.0022(16) 0.0000(15) -0.0076(14) C20 0.0159(15) 0.0102(17) 0.016(2) -0.0006(15) 0.0001(15) -0.0023(13) C21 0.0204(16) 0.0146(18) 0.023(2) -0.0007(16) 0.0000(17) -0.0005(13) C22 0.0231(17) 0.024(2) 0.017(2) -0.0050(17) 0.0054(16) -0.0040(15) C23 0.0215(16) 0.028(2) 0.016(2) 0.0024(17) -0.0048(16) -0.0053(15) C24 0.0177(16) 0.0162(18) 0.020(2) 0.0021(16) 0.0017(16) -0.0009(13) C25 0.0159(15) 0.0119(17) 0.011(2) -0.0034(15) -0.0026(15) -0.0006(13) C26 0.0209(16) 0.0187(18) 0.014(2) -0.0024(16) -0.0006(16) -0.0007(14) C27 0.0202(16) 0.026(2) 0.020(2) -0.0051(17) -0.0023(16) 0.0042(15) C28 0.0269(18) 0.0208(19) 0.023(2) -0.0018(17) -0.0067(17) 0.0109(15) C29 0.0333(19) 0.0187(19) 0.021(2) 0.0058(17) -0.0043(18) -0.0052(15) C30 0.0186(15) 0.0191(18) 0.014(2) -0.0006(16) -0.0040(15) 0.0007(14) C31 0.0146(15) 0.0170(18) 0.024(2) 0.0013(17) -0.0012(16) 0.0049(13) C32 0.0200(16) 0.0199(19) 0.033(3) 0.0015(18) 0.0024(17) 0.0012(15) C33 0.0170(16) 0.020(2) 0.054(3) -0.007(2) -0.0012(19) 0.0009(15) C34 0.0159(17) 0.019(2) 0.062(3) 0.007(2) 0.002(2) -0.0015(14) C35 0.0183(17) 0.027(2) 0.044(3) 0.018(2) 0.0069(18) 0.0004(15) C36 0.0176(16) 0.0203(19) 0.029(2) 0.0051(17) -0.0017(17) 0.0062(14) C37 0.0179(16) 0.022(2) 0.041(3) 0.0074(19) -0.0017(18) 0.0030(14) C38 0.0252(18) 0.019(2) 0.107(4) 0.002(2) -0.003(2) 0.0017(16) C39 0.0264(18) 0.058(3) 0.056(3) 0.031(2) -0.001(2) 0.0124(18) C40 0.0223(16) 0.0167(18) 0.032(2) -0.0023(17) 0.0002(17) -0.0006(14) C41 0.0210(17) 0.051(2) 0.041(3) -0.003(2) 0.0106(18) -0.0126(16) C42 0.0247(17) 0.029(2) 0.047(3) -0.0083(19) -0.0011(18) -0.0111(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 P1 O1 1.507(2) . ? P1 N1 1.588(2) . ? P1 C7 1.844(3) . ? P1 C1 1.858(3) . ? P2 O2 1.4232(16) . ? P2 C25 1.795(3) . ? P2 C2 1.843(3) . ? P2 C19 1.927(3) . ? P3 O3 1.537(2) . ? P3 N2 1.594(2) . ? P3 C31 1.792(3) . ? P3 C20 1.865(3) . ? N1 C16 1.482(3) . ? N1 C13 1.545(3) . ? N2 C40 1.485(3) . ? N2 C37 1.502(3) . ? C1 C6 1.389(4) . ? C1 C2 1.489(4) . ? C2 C3 1.377(3) . ? C3 C4 1.378(4) . ? C3 H3 0.95 . ? C4 C5 1.456(4) . ? C4 H4 0.95 . ? C5 C6 1.364(3) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C12 1.338(3) . ? C7 C8 1.344(3) . ? C8 C9 1.395(3) . ? C8 H8 0.95 . ? C9 C10 1.326(3) . ? C9 H9 0.95 . ? C10 C11 1.333(3) . ? C10 H10 0.95 . ? C11 C12 1.399(3) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C15 1.520(3) . ? C13 C14 1.559(4) . ? C13 H13 1 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C18 1.466(3) . ? C16 C17 1.553(3) . ? C16 H16 1 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 C20 1.399(3) . ? C19 C24 1.450(4) . ? C20 C21 1.454(4) . ? C21 C22 1.413(4) . ? C21 H21 0.95 . ? C22 C23 1.354(3) . ? C22 H22 0.95 . ? C23 C24 1.441(4) . ? C23 H23 0.95 . ? C24 H24 0.95 . ? C25 C26 1.320(3) . ? C25 C30 1.391(3) . ? C26 C27 1.379(3) . ? C26 H26 0.95 . ? C27 C28 1.376(4) . ? C27 H27 0.95 . ? C28 C29 1.310(3) . ? C28 H28 0.95 . ? C29 C30 1.377(3) . ? C29 H29 0.95 . ? C30 H30 0.95 . ? C31 C32 1.430(4) . ? C31 C36 1.435(4) . ? C32 C33 1.362(3) . ? C32 H32 0.95 . ? C33 C34 1.415(4) . ? C33 H33 0.95 . ? C34 C35 1.424(4) . ? C34 H34 0.95 . ? C35 C36 1.382(3) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C37 C38 1.527(4) . ? C37 C39 1.597(4) . ? C37 H37 1 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 C42 1.531(3) . ? C40 C41 1.545(4) . ? C40 H40 1 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? 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 P1 N1 108.34(12) . . ? O1 P1 C7 108.39(12) . . ? N1 P1 C7 113.22(12) . . ? O1 P1 C1 112.21(12) . . ? N1 P1 C1 108.23(12) . . ? C7 P1 C1 106.52(13) . . ? O2 P2 C25 110.00(11) . . ? O2 P2 C2 113.57(12) . . ? C25 P2 C2 106.53(12) . . ? O2 P2 C19 113.42(11) . . ? C25 P2 C19 100.29(13) . . ? C2 P2 C19 111.98(12) . . ? O3 P3 N2 120.18(12) . . ? O3 P3 C31 109.77(13) . . ? N2 P3 C31 102.94(12) . . ? O3 P3 C20 115.40(12) . . ? N2 P3 C20 101.54(13) . . ? C31 P3 C20 105.39(13) . . ? C16 N1 C13 120.1(2) . . ? C16 N1 P1 119.73(19) . . ? C13 N1 P1 119.89(19) . . ? C40 N2 C37 117.2(2) . . ? C40 N2 P3 117.05(17) . . ? C37 N2 P3 118.47(19) . . ? C6 C1 C2 119.3(2) . . ? C6 C1 P1 106.7(2) . . ? C2 C1 P1 133.7(2) . . ? C3 C2 C1 120.8(3) . . ? C3 C2 P2 111.2(2) . . ? C1 C2 P2 127.9(2) . . ? C2 C3 C4 117.8(3) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? C3 C4 C5 122.1(3) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 120.2(3) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 119.7(3) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C12 C7 C8 115.7(3) . . ? C12 C7 P1 125.6(2) . . ? C8 C7 P1 117.9(2) . . ? C7 C8 C9 122.5(3) . . ? C7 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? C10 C9 C8 121.1(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 117.2(3) . . ? C9 C10 H10 121.4 . . ? C11 C10 H10 121.4 . . ? C10 C11 C12 121.7(3) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C7 C12 C11 121.8(3) . . ? C7 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C15 C13 N1 112.8(2) . . ? C15 C13 C14 110.2(3) . . ? N1 C13 C14 117.3(2) . . ? C15 C13 H13 105.1 . . ? N1 C13 H13 105.1 . . ? C14 C13 H13 105.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 N1 110.6(2) . . ? C18 C16 C17 113.2(2) . . ? N1 C16 C17 108.8(2) . . ? C18 C16 H16 108 . . ? N1 C16 H16 108 . . ? C17 C16 H16 108 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 114.6(3) . . ? C20 C19 P2 125.2(2) . . ? C24 C19 P2 119.2(2) . . ? C19 C20 C21 117.7(3) . . ? C19 C20 P3 120.7(2) . . ? C21 C20 P3 121.3(2) . . ? C22 C21 C20 126.2(3) . . ? C22 C21 H21 116.9 . . ? C20 C21 H21 116.9 . . ? C23 C22 C21 116.7(3) . . ? C23 C22 H22 121.6 . . ? C21 C22 H22 121.6 . . ? C22 C23 C24 118.6(3) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C23 C24 C19 126.0(3) . . ? C23 C24 H24 117 . . ? C19 C24 H24 117 . . ? C26 C25 C30 117.5(3) . . ? C26 C25 P2 122.1(2) . . ? C30 C25 P2 120.32(19) . . ? C25 C26 C27 118.6(3) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? C28 C27 C26 123.6(3) . . ? C28 C27 H27 118.2 . . ? C26 C27 H27 118.2 . . ? C29 C28 C27 118.1(3) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? C28 C29 C30 118.8(3) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? C29 C30 C25 123.3(2) . . ? C29 C30 H30 118.3 . . ? C25 C30 H30 118.3 . . ? C32 C31 C36 121.9(3) . . ? C32 C31 P3 123.7(2) . . ? C36 C31 P3 114.4(2) . . ? C33 C32 C31 119.6(3) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 118.5(3) . . ? C32 C33 H33 120.8 . . ? C34 C33 H33 120.8 . . ? C33 C34 C35 123.0(3) . . ? C33 C34 H34 118.5 . . ? C35 C34 H34 118.5 . . ? C36 C35 C34 118.9(3) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C35 C36 C31 118.0(3) . . ? C35 C36 H36 121 . . ? C31 C36 H36 121 . . ? N2 C37 C38 112.8(2) . . ? N2 C37 C39 115.9(2) . . ? C38 C37 C39 112.8(3) . . ? N2 C37 H37 104.7 . . ? C38 C37 H37 104.7 . . ? C39 C37 H37 104.7 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N2 C40 C42 110.2(3) . . ? N2 C40 C41 109.9(2) . . ? C42 C40 C41 117.0(2) . . ? N2 C40 H40 106.4 . . ? C42 C40 H40 106.4 . . ? C41 C40 H40 106.4 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? # END of CIF # Attachment '- complex13_CCDC806040.cif' data_478_2m_nitrato _database_code_depnum_ccdc_archive 'CCDC 806040' #TrackingRef '- complex13_CCDC806040.cif' _audit_creation_date 2010-12-28T22:01:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C84 H102 N5 O9 P6 Y, C2 H3 N, 2(N O3)' _chemical_formula_sum 'C86 H105 N8 O15 P6 Y' _chemical_formula_weight 1765.51 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.831(2) _cell_length_b 15.879(2) _cell_length_c 23.473(3) _cell_angle_alpha 74.596(2) _cell_angle_beta 73.845(3) _cell_angle_gamma 62.892(3) _cell_volume 4663.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 988 _cell_measurement_theta_min 2.318 _cell_measurement_theta_max 15.53 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.422 _exptl_crystal_size_mid 0.216 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Linear fit to sin(theta)/lambda - 12 parameters ; _exptl_absorpt_correction_T_min 0.6352 _exptl_absorpt_correction_T_max 0.9964 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_unetI/netI 0.1739 _diffrn_reflns_number 24286 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.92 _diffrn_reflns_theta_max 24.45 _diffrn_reflns_theta_full 24.45 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 15189 _reflns_number_gt 7436 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-86 ' _computing_structure_refinement 'SHELXL-97 ' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. Aditional disordered solvent molecules were not modelled and the disordered density was taken into account using SQUEEZE/PLATON ; _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^)+(0.0469P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 15189 _refine_ls_number_parameters 1016 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 0.804 _refine_ls_restrained_S_all 0.804 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.178 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.066 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 -0.037 0.500 587 165 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y1 Y 1.04371(4) 0.27348(3) 0.21585(2) 0.02835(14) Uani 1 1 d . . . P1 P 0.81725(10) 0.31276(10) 0.33883(6) 0.0388(4) Uani 1 1 d . . . P2 P 1.01162(10) 0.39607(10) 0.33363(6) 0.0362(4) Uani 1 1 d . . . P3 P 0.99176(10) 0.53717(9) 0.19076(6) 0.0368(4) Uani 1 1 d . . . P4 P 1.03683(10) 0.05705(9) 0.17885(6) 0.0333(3) Uani 1 1 d . . . P5 P 1.21199(10) 0.02968(9) 0.26358(6) 0.0319(3) Uani 1 1 d . . . P6 P 1.32073(10) 0.18038(9) 0.15058(6) 0.0321(3) Uani 1 1 d . . . O1 O 0.9018(2) 0.2764(2) 0.28687(14) 0.0376(9) Uani 1 1 d . . . O2 O 1.0580(2) 0.3125(2) 0.30114(13) 0.0310(8) Uani 1 1 d . . . O3 O 1.0050(2) 0.4356(2) 0.19889(13) 0.0321(8) Uani 1 1 d . . . O4 O 1.0453(2) 0.1457(2) 0.18393(13) 0.0327(8) Uani 1 1 d . . . O5 O 1.1444(2) 0.1318(2) 0.26988(13) 0.0314(8) Uani 1 1 d . . . O6 O 1.2091(2) 0.2416(2) 0.17027(14) 0.0351(9) Uani 1 1 d . . . O8 O 1.0413(3) 0.3172(2) 0.10630(14) 0.0355(9) Uani 1 1 d . . . O7 O 0.8951(2) 0.3495(2) 0.16659(15) 0.0379(9) Uani 1 1 d . . . O9 O 0.8999(3) 0.3700(3) 0.07062(17) 0.0636(12) Uani 1 1 d . . . N1 N 0.8356(3) 0.2377(3) 0.40192(19) 0.0477(12) Uani 1 1 d . . . N2 N 1.0440(3) 0.5819(3) 0.12652(17) 0.0371(11) Uani 1 1 d . . . N3 N 0.9226(3) 0.0750(3) 0.17119(19) 0.0389(11) Uani 1 1 d . . . N5 N 0.9434(4) 0.3466(3) 0.1133(2) 0.0404(12) Uani 1 1 d . . . N4 N 1.3969(3) 0.1778(3) 0.19011(18) 0.0369(11) Uani 1 1 d . . . C1 C 0.7970(4) 0.4300(3) 0.3503(2) 0.0396(14) Uani 1 1 d . . . C2 C 0.8726(4) 0.4639(3) 0.3437(2) 0.0355(13) Uani 1 1 d . . . C3 C 0.8403(4) 0.5581(4) 0.3514(2) 0.0461(15) Uani 1 1 d . . . H3 H 0.891 0.5819 0.3457 0.055 Uiso 1 1 calc R . . C4 C 0.7385(5) 0.6181(4) 0.3668(3) 0.0598(17) Uani 1 1 d . . . H4 H 0.7192 0.6818 0.3718 0.072 Uiso 1 1 calc R . . C5 C 0.6663(5) 0.5841(5) 0.3746(3) 0.0675(19) Uani 1 1 d . . . H5 H 0.5955 0.6242 0.3857 0.081 Uiso 1 1 calc R . . C6 C 0.6950(4) 0.4912(4) 0.3665(2) 0.0580(17) Uani 1 1 d . . . H6 H 0.643 0.4689 0.3723 0.07 Uiso 1 1 calc R . . C7 C 0.6975(4) 0.3333(4) 0.3214(2) 0.0403(14) Uani 1 1 d . . . C8 C 0.6628(4) 0.4030(4) 0.2729(3) 0.0615(18) Uani 1 1 d . . . H8 H 0.7035 0.4364 0.2492 0.074 Uiso 1 1 calc R . . C9 C 0.5679(5) 0.4246(5) 0.2583(3) 0.0684(19) Uani 1 1 d . . . H9 H 0.5453 0.4717 0.2246 0.082 Uiso 1 1 calc R . . C10 C 0.5097(5) 0.3789(5) 0.2920(3) 0.073(2) Uani 1 1 d . . . H10 H 0.4435 0.3967 0.284 0.087 Uiso 1 1 calc R . . C11 C 0.5456(5) 0.3054(6) 0.3387(3) 0.091(2) Uani 1 1 d . . . H11 H 0.5074 0.2685 0.3599 0.109 Uiso 1 1 calc R . . C12 C 0.6385(5) 0.2860(5) 0.3544(3) 0.0678(19) Uani 1 1 d . . . H12 H 0.6604 0.2393 0.3884 0.081 Uiso 1 1 calc R . . C13 C 1.0379(4) 0.3543(4) 0.4094(2) 0.0448(15) Uani 1 1 d . . . C14 C 1.1232(5) 0.2714(4) 0.4188(3) 0.0618(18) Uani 1 1 d . . . H14 H 1.1643 0.2363 0.3868 0.074 Uiso 1 1 calc R . . C15 C 1.1492(6) 0.2385(5) 0.4763(3) 0.102(3) Uani 1 1 d . . . H15 H 1.209 0.1815 0.4833 0.122 Uiso 1 1 calc R . . C16 C 1.0875(7) 0.2895(6) 0.5226(3) 0.094(3) Uani 1 1 d . . . H16 H 1.104 0.2666 0.5618 0.112 Uiso 1 1 calc R . . C17 C 1.0047(6) 0.3706(5) 0.5125(3) 0.078(2) Uani 1 1 d . . . H17 H 0.9634 0.4054 0.5446 0.094 Uiso 1 1 calc R . . C18 C 0.9782(5) 0.4047(4) 0.4569(3) 0.0650(18) Uani 1 1 d . . . H18 H 0.9191 0.4627 0.4506 0.078 Uiso 1 1 calc R . . C19 C 1.0645(4) 0.4848(3) 0.3014(2) 0.0387(13) Uani 1 1 d . . . C20 C 1.0506(4) 0.5468(3) 0.2458(2) 0.0362(13) Uani 1 1 d . . . C21 C 1.0856(4) 0.6190(4) 0.2309(2) 0.0548(16) Uani 1 1 d . . . H21 H 1.072 0.6638 0.195 0.066 Uiso 1 1 calc R . . C22 C 1.1397(5) 0.6277(4) 0.2670(3) 0.0610(18) Uani 1 1 d . . . H22 H 1.1643 0.6767 0.2556 0.073 Uiso 1 1 calc R . . C23 C 1.1570(5) 0.5644(4) 0.3193(3) 0.0667(19) Uani 1 1 d . . . H23 H 1.1964 0.568 0.3436 0.08 Uiso 1 1 calc R . . C24 C 1.1186(4) 0.4961(4) 0.3371(3) 0.0492(15) Uani 1 1 d . . . H24 H 1.1289 0.4553 0.3747 0.059 Uiso 1 1 calc R . . C25 C 0.8568(4) 0.6150(4) 0.2030(2) 0.0453(15) Uani 1 1 d . . . C26 C 0.7846(4) 0.5857(4) 0.1996(2) 0.0539(16) Uani 1 1 d . . . H26 H 0.8066 0.5222 0.1931 0.065 Uiso 1 1 calc R . . C27 C 0.6809(5) 0.6463(5) 0.2053(3) 0.078(2) Uani 1 1 d . . . H27 H 0.6326 0.6251 0.2018 0.093 Uiso 1 1 calc R . . C28 C 0.6487(6) 0.7371(6) 0.2161(3) 0.096(3) Uani 1 1 d . . . H28 H 0.578 0.7798 0.2188 0.115 Uiso 1 1 calc R . . C29 C 0.7185(6) 0.7671(5) 0.2232(3) 0.086(3) Uani 1 1 d . . . H29 H 0.6949 0.8291 0.2329 0.103 Uiso 1 1 calc R . . C30 C 0.8218(5) 0.7077(4) 0.2164(2) 0.0661(19) Uani 1 1 d . . . H30 H 0.8696 0.729 0.2206 0.079 Uiso 1 1 calc R . . C31 C 0.7707(6) 0.2696(5) 0.4581(3) 0.073(2) Uani 1 1 d . . . H31 H 0.7096 0.3274 0.4454 0.088 Uiso 1 1 calc R . . C32 C 0.8075(6) 0.3022(6) 0.4941(3) 0.128(3) Uani 1 1 d . . . H32A H 0.8353 0.348 0.4687 0.192 Uiso 1 1 calc R . . H32B H 0.8619 0.2475 0.5132 0.192 Uiso 1 1 calc R . . H32C H 0.7507 0.3337 0.5252 0.192 Uiso 1 1 calc R . . C33 C 0.7253(6) 0.2009(6) 0.4993(3) 0.125(3) Uani 1 1 d . . . H33A H 0.6973 0.1791 0.4757 0.187 Uiso 1 1 calc R . . H33B H 0.6701 0.2339 0.5305 0.187 Uiso 1 1 calc R . . H33C H 0.7793 0.1455 0.5182 0.187 Uiso 1 1 calc R . . C34 C 0.9243(6) 0.1403(5) 0.4008(3) 0.099(3) Uani 1 1 d . . . H34 H 0.9718 0.1465 0.3618 0.119 Uiso 1 1 calc R . . C35 C 0.9861(6) 0.1153(5) 0.4489(4) 0.152(4) Uani 1 1 d . . . H35A H 1.0037 0.1685 0.4472 0.228 Uiso 1 1 calc R . . H35B H 1.0495 0.0573 0.4423 0.228 Uiso 1 1 calc R . . H35C H 0.9453 0.1038 0.4885 0.228 Uiso 1 1 calc R . . C36 C 0.8870(6) 0.0715(5) 0.3959(4) 0.126(3) Uani 1 1 d . . . H36A H 0.8477 0.0981 0.3632 0.189 Uiso 1 1 calc R . . H36B H 0.8426 0.0594 0.4338 0.189 Uiso 1 1 calc R . . H36C H 0.9459 0.0112 0.3875 0.189 Uiso 1 1 calc R . . C37 C 0.9931(4) 0.6274(3) 0.0728(2) 0.0441(14) Uani 1 1 d . . . H37 H 1.051 0.6249 0.038 0.053 Uiso 1 1 calc R . . C38 C 0.9445(4) 0.5707(4) 0.0598(2) 0.0532(16) Uani 1 1 d . . . H38A H 0.9941 0.5036 0.0603 0.08 Uiso 1 1 calc R . . H38B H 0.9247 0.5974 0.0201 0.08 Uiso 1 1 calc R . . H38C H 0.8832 0.5743 0.0905 0.08 Uiso 1 1 calc R . . C39 C 0.9238(4) 0.7327(3) 0.0708(2) 0.0610(17) Uani 1 1 d . . . H39A H 0.9603 0.7657 0.0784 0.092 Uiso 1 1 calc R . . H39B H 0.8617 0.7408 0.1017 0.092 Uiso 1 1 calc R . . H39C H 0.9043 0.7599 0.0311 0.092 Uiso 1 1 calc R . . C40 C 1.1587(4) 0.5389(4) 0.1104(2) 0.0468(15) Uani 1 1 d . . . H40 H 1.1858 0.5071 0.1487 0.056 Uiso 1 1 calc R . . C41 C 1.1998(4) 0.6176(4) 0.0805(3) 0.0676(18) Uani 1 1 d . . . H41A H 1.1725 0.6659 0.1068 0.101 Uiso 1 1 calc R . . H41B H 1.1774 0.6482 0.0418 0.101 Uiso 1 1 calc R . . H41C H 1.2752 0.5884 0.0743 0.101 Uiso 1 1 calc R . . C42 C 1.2007(4) 0.4630(3) 0.0711(2) 0.0473(15) Uani 1 1 d . . . H42A H 1.1756 0.413 0.091 0.071 Uiso 1 1 calc R . . H42B H 1.2761 0.4345 0.0643 0.071 Uiso 1 1 calc R . . H42C H 1.1775 0.4922 0.0324 0.071 Uiso 1 1 calc R . . C43 C 1.0670(3) -0.0309(3) 0.2466(2) 0.0320(12) Uani 1 1 d . . . C44 C 1.1384(3) -0.0432(3) 0.2809(2) 0.0338(13) Uani 1 1 d . . . C45 C 1.1543(4) -0.1145(3) 0.3314(2) 0.0431(14) Uani 1 1 d . . . H45 H 1.2032 -0.1238 0.3539 0.052 Uiso 1 1 calc R . . C46 C 1.1004(4) -0.1724(4) 0.3497(2) 0.0483(15) Uani 1 1 d . . . H46 H 1.1109 -0.2194 0.3849 0.058 Uiso 1 1 calc R . . C47 C 1.0320(4) -0.1603(4) 0.3160(3) 0.0477(15) Uani 1 1 d . . . H47 H 0.9953 -0.1998 0.3275 0.057 Uiso 1 1 calc R . . C48 C 1.0165(4) -0.0912(4) 0.2656(2) 0.0414(14) Uani 1 1 d . . . H48 H 0.9692 -0.0846 0.2428 0.05 Uiso 1 1 calc R . . C49 C 1.1296(4) 0.0027(3) 0.1167(2) 0.0334(13) Uani 1 1 d . . . C50 C 1.1666(4) -0.0940(4) 0.1141(2) 0.0404(14) Uani 1 1 d . . . H50 H 1.1458 -0.135 0.1472 0.049 Uiso 1 1 calc R . . C51 C 1.2335(4) -0.1309(4) 0.0639(2) 0.0418(14) Uani 1 1 d . . . H51 H 1.2576 -0.1969 0.062 0.05 Uiso 1 1 calc R . . C52 C 1.2652(4) -0.0715(4) 0.0164(2) 0.0463(15) Uani 1 1 d . . . H52 H 1.3107 -0.0967 -0.0183 0.056 Uiso 1 1 calc R . . C53 C 1.2312(4) 0.0238(4) 0.0192(2) 0.0469(15) Uani 1 1 d . . . H53 H 1.2537 0.0642 -0.0135 0.056 Uiso 1 1 calc R . . C54 C 1.1638(4) 0.0612(4) 0.0700(2) 0.0362(13) Uani 1 1 d . . . H54 H 1.1416 0.1267 0.0724 0.043 Uiso 1 1 calc R . . C55 C 1.2976(4) -0.0191(3) 0.3174(2) 0.0329(13) Uani 1 1 d . . . C56 C 1.3915(4) -0.0971(4) 0.3115(2) 0.0479(15) Uani 1 1 d . . . H56 H 1.4141 -0.1291 0.2779 0.058 Uiso 1 1 calc R . . C57 C 1.4527(4) -0.1286(4) 0.3541(3) 0.0574(17) Uani 1 1 d . . . H57 H 1.5167 -0.183 0.3502 0.069 Uiso 1 1 calc R . . C58 C 1.4213(5) -0.0818(5) 0.4019(3) 0.0621(19) Uani 1 1 d . . . H58 H 1.4646 -0.103 0.4306 0.074 Uiso 1 1 calc R . . C59 C 1.3286(5) -0.0052(4) 0.4087(3) 0.0557(17) Uani 1 1 d . . . H59 H 1.3066 0.0261 0.4426 0.067 Uiso 1 1 calc R . . C60 C 1.2667(4) 0.0269(4) 0.3661(2) 0.0444(15) Uani 1 1 d . . . H60 H 1.2024 0.081 0.3705 0.053 Uiso 1 1 calc R . . C61 C 1.2990(3) 0.0009(3) 0.1930(2) 0.0295(12) Uani 1 1 d . . . C62 C 1.3466(3) 0.0574(3) 0.1516(2) 0.0290(12) Uani 1 1 d . . . C63 C 1.4235(4) 0.0141(3) 0.1039(2) 0.0372(13) Uani 1 1 d . . . H63 H 1.4566 0.0509 0.0754 0.045 Uiso 1 1 calc R . . C64 C 1.4524(3) -0.0781(3) 0.0971(2) 0.0372(13) Uani 1 1 d . . . H64 H 1.5049 -0.1042 0.0647 0.045 Uiso 1 1 calc R . . C65 C 1.4055(4) -0.1325(3) 0.1369(2) 0.0397(14) Uani 1 1 d . . . H65 H 1.4248 -0.1966 0.1327 0.048 Uiso 1 1 calc R . . C66 C 1.3287(4) -0.0920(3) 0.1841(2) 0.0355(13) Uani 1 1 d . . . H66 H 1.2953 -0.1296 0.2114 0.043 Uiso 1 1 calc R . . C67 C 1.3551(4) 0.2267(3) 0.0732(2) 0.0333(13) Uani 1 1 d . . . C68 C 1.2875(4) 0.2471(3) 0.0337(2) 0.0403(14) Uani 1 1 d . . . H68 H 1.2267 0.236 0.0485 0.048 Uiso 1 1 calc R . . C69 C 1.3107(4) 0.2830(4) -0.0257(2) 0.0441(14) Uani 1 1 d . . . H69 H 1.2657 0.2963 -0.052 0.053 Uiso 1 1 calc R . . C70 C 1.3985(4) 0.3003(3) -0.0480(2) 0.0425(14) Uani 1 1 d . . . H70 H 1.4127 0.3261 -0.0892 0.051 Uiso 1 1 calc R . . C71 C 1.4651(4) 0.2802(3) -0.0109(2) 0.0405(14) Uani 1 1 d . . . H71 H 1.5251 0.2925 -0.0261 0.049 Uiso 1 1 calc R . . C72 C 1.4440(4) 0.2415(3) 0.0493(2) 0.0363(13) Uani 1 1 d . . . H72 H 1.4918 0.2249 0.0744 0.044 Uiso 1 1 calc R . . C73 C 0.8923(4) 0.0571(4) 0.1221(3) 0.0561(16) Uani 1 1 d . . . H73 H 0.8155 0.091 0.1304 0.067 Uiso 1 1 calc R . . C74 C 0.9099(5) -0.0425(4) 0.1239(3) 0.094(2) Uani 1 1 d . . . H74A H 0.8874 -0.0696 0.1651 0.141 Uiso 1 1 calc R . . H74B H 0.9835 -0.0805 0.1109 0.141 Uiso 1 1 calc R . . H74C H 0.8706 -0.0437 0.097 0.141 Uiso 1 1 calc R . . C75 C 0.9217(4) 0.1073(5) 0.0595(3) 0.074(2) Uani 1 1 d . . . H75A H 0.9052 0.1738 0.0613 0.112 Uiso 1 1 calc R . . H75B H 0.8831 0.1063 0.0321 0.112 Uiso 1 1 calc R . . H75C H 0.9957 0.074 0.0449 0.112 Uiso 1 1 calc R . . C76 C 0.8341(5) 0.1347(5) 0.2129(3) 0.0672(19) Uani 1 1 d . . . H76 H 0.8644 0.1511 0.2393 0.081 Uiso 1 1 calc R . . C77 C 0.7657(4) 0.2271(4) 0.1819(3) 0.094(3) Uani 1 1 d . . . H77A H 0.8067 0.2618 0.1563 0.141 Uiso 1 1 calc R . . H77B H 0.7139 0.2659 0.2118 0.141 Uiso 1 1 calc R . . H77C H 0.7312 0.2147 0.157 0.141 Uiso 1 1 calc R . . C78 C 0.7728(4) 0.0801(5) 0.2543(3) 0.085(2) Uani 1 1 d . . . H78A H 0.8193 0.0205 0.2753 0.128 Uiso 1 1 calc R . . H78B H 0.7388 0.0649 0.2306 0.128 Uiso 1 1 calc R . . H78C H 0.7207 0.1195 0.2838 0.128 Uiso 1 1 calc R . . C79 C 1.4832(4) 0.0891(4) 0.2114(2) 0.0478(15) Uani 1 1 d . . . H79 H 1.4658 0.0345 0.2131 0.057 Uiso 1 1 calc R . . C80 C 1.5854(4) 0.0723(4) 0.1664(3) 0.0615(18) Uani 1 1 d . . . H80A H 1.575 0.0756 0.1263 0.092 Uiso 1 1 calc R . . H80B H 1.6377 0.0089 0.1789 0.092 Uiso 1 1 calc R . . H80C H 1.6084 0.1216 0.1654 0.092 Uiso 1 1 calc R . . C81 C 1.4969(5) 0.0835(5) 0.2737(3) 0.087(2) Uani 1 1 d . . . H81A H 1.4316 0.0929 0.3018 0.13 Uiso 1 1 calc R . . H81B H 1.5183 0.1334 0.2737 0.13 Uiso 1 1 calc R . . H81C H 1.5498 0.0204 0.2862 0.13 Uiso 1 1 calc R . . C82 C 1.3727(4) 0.2809(5) 0.1988(3) 0.087(3) Uani 1 1 d . . . H82 H 1.3248 0.326 0.1707 0.104 Uiso 1 1 calc R . . C83 C 1.4640(5) 0.3039(5) 0.1801(3) 0.100(2) Uani 1 1 d . . . H83A H 1.4966 0.2923 0.1388 0.151 Uiso 1 1 calc R . . H83B H 1.5133 0.2631 0.207 0.151 Uiso 1 1 calc R . . H83C H 1.4425 0.3714 0.1821 0.151 Uiso 1 1 calc R . . C84 C 1.3115(4) 0.2975(6) 0.2615(4) 0.124(4) Uani 1 1 d . . . H84A H 1.2519 0.2821 0.2688 0.186 Uiso 1 1 calc R . . H84B H 1.2876 0.3649 0.2649 0.186 Uiso 1 1 calc R . . H84C H 1.3553 0.2564 0.2912 0.186 Uiso 1 1 calc R . . N1S N 0.6455(4) 0.2949(5) 0.0454(3) 0.093(2) Uani 1 1 d . . . C2S C 0.6361(5) 0.3627(6) 0.0582(3) 0.078(2) Uani 1 1 d . . . C1S C 0.6240(5) 0.4494(4) 0.0750(3) 0.097(2) Uani 1 1 d . . . H1S H 0.6693 0.4326 0.1034 0.146 Uiso 1 1 calc R . . H2S H 0.5522 0.4833 0.0938 0.146 Uiso 1 1 calc R . . H3S H 0.6422 0.4909 0.039 0.146 Uiso 1 1 calc R . . N1NI N 0.3808(5) 0.6313(4) 0.1732(3) 0.0724(17) Uani 1 1 d D . . O1NI O 0.4676(4) 0.6270(3) 0.1650(2) 0.1031(18) Uani 1 1 d D . . O2NI O 0.3041(4) 0.7053(3) 0.1844(3) 0.115(2) Uani 1 1 d D . . O3NI O 0.3707(4) 0.5573(4) 0.1784(3) 0.132(2) Uani 1 1 d D . . N2NI N 0.7779 0.833 0.3324 0.170(3) Uiso 1 1 d GU . . O6NI O 0.8493(2) 0.75826(19) 0.3469(2) 0.144(2) Uiso 1 1 d GU . . O5NI O 0.68990(16) 0.8539(4) 0.3622(2) 0.227(3) Uiso 1 1 d GU . . O4NI O 0.7915(4) 0.8807(4) 0.28328(16) 0.367(6) Uiso 1 1 d GU . . 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 Y1 0.0280(3) 0.0286(3) 0.0278(3) -0.0048(2) -0.0046(2) -0.0114(2) P1 0.0364(9) 0.0466(9) 0.0304(9) -0.0051(7) -0.0018(7) -0.0175(8) P2 0.0436(10) 0.0356(8) 0.0299(8) -0.0065(7) -0.0065(7) -0.0163(7) P3 0.0409(9) 0.0282(8) 0.0332(9) -0.0045(7) -0.0038(7) -0.0095(7) P4 0.0332(9) 0.0335(8) 0.0378(9) -0.0061(7) -0.0094(7) -0.0157(7) P5 0.0322(9) 0.0302(8) 0.0367(9) -0.0022(7) -0.0102(7) -0.0152(7) P6 0.0292(9) 0.0266(8) 0.0409(9) -0.0056(7) -0.0043(7) -0.0130(7) O1 0.042(2) 0.050(2) 0.028(2) -0.0070(17) -0.0049(17) -0.0258(18) O2 0.035(2) 0.036(2) 0.0266(19) -0.0106(16) -0.0050(15) -0.0161(17) O3 0.027(2) 0.0257(19) 0.034(2) -0.0033(16) -0.0055(15) -0.0044(16) O4 0.034(2) 0.032(2) 0.037(2) -0.0070(16) -0.0118(16) -0.0140(16) O5 0.030(2) 0.0305(19) 0.037(2) -0.0044(16) -0.0098(16) -0.0136(16) O6 0.028(2) 0.0286(19) 0.043(2) -0.0056(16) -0.0032(16) -0.0089(16) O8 0.031(2) 0.041(2) 0.033(2) -0.0054(17) -0.0047(17) -0.0134(18) O7 0.037(2) 0.048(2) 0.025(2) -0.0051(18) -0.0036(17) -0.0157(18) O9 0.062(3) 0.097(3) 0.039(3) 0.007(2) -0.022(2) -0.041(3) N1 0.047(3) 0.041(3) 0.031(3) -0.005(2) 0.003(2) -0.004(2) N2 0.038(3) 0.030(2) 0.032(3) -0.003(2) -0.002(2) -0.008(2) N3 0.027(3) 0.053(3) 0.048(3) -0.019(2) -0.011(2) -0.017(2) N5 0.041(3) 0.040(3) 0.040(3) 0.004(2) -0.018(3) -0.017(3) N4 0.030(3) 0.037(3) 0.048(3) -0.017(2) -0.005(2) -0.013(2) C1 0.031(3) 0.033(3) 0.038(3) -0.008(3) -0.002(3) 0.000(3) C2 0.035(3) 0.032(3) 0.030(3) -0.008(3) 0.001(2) -0.008(3) C3 0.041(4) 0.048(4) 0.037(3) -0.013(3) 0.010(3) -0.015(3) C4 0.056(5) 0.051(4) 0.060(4) -0.015(3) -0.005(4) -0.012(4) C5 0.056(5) 0.059(5) 0.060(5) -0.026(4) 0.003(4) 0.000(4) C6 0.053(4) 0.061(4) 0.056(4) -0.017(3) -0.010(3) -0.016(4) C7 0.037(4) 0.057(4) 0.029(3) -0.007(3) 0.001(3) -0.026(3) C8 0.048(4) 0.078(5) 0.062(5) -0.011(4) -0.006(3) -0.031(4) C9 0.045(4) 0.080(5) 0.076(5) -0.010(4) -0.018(4) -0.020(4) C10 0.039(4) 0.102(6) 0.081(6) -0.040(5) -0.007(4) -0.022(4) C11 0.075(6) 0.144(8) 0.088(6) -0.019(5) -0.008(5) -0.078(5) C12 0.071(5) 0.087(5) 0.060(5) -0.009(4) -0.007(4) -0.049(4) C13 0.062(4) 0.047(4) 0.029(3) -0.003(3) -0.013(3) -0.025(3) C14 0.094(5) 0.046(4) 0.052(4) -0.003(3) -0.032(4) -0.027(4) C15 0.167(8) 0.063(5) 0.078(6) -0.001(5) -0.081(6) -0.023(5) C16 0.164(9) 0.089(6) 0.048(5) 0.000(5) -0.053(5) -0.057(6) C17 0.110(7) 0.088(6) 0.042(4) -0.016(4) -0.019(4) -0.040(5) C18 0.079(5) 0.078(5) 0.035(4) -0.014(4) -0.008(3) -0.028(4) C19 0.043(4) 0.032(3) 0.036(3) -0.012(3) 0.000(3) -0.013(3) C20 0.044(4) 0.027(3) 0.038(3) -0.012(3) -0.004(3) -0.013(3) C21 0.087(5) 0.043(4) 0.038(4) -0.009(3) -0.004(3) -0.032(4) C22 0.092(5) 0.053(4) 0.059(5) -0.018(4) -0.003(4) -0.050(4) C23 0.088(5) 0.067(5) 0.074(5) -0.034(4) -0.015(4) -0.044(4) C24 0.060(4) 0.046(4) 0.050(4) -0.017(3) -0.009(3) -0.025(3) C25 0.038(4) 0.034(4) 0.033(3) 0.006(3) -0.002(3) 0.001(3) C26 0.046(4) 0.059(4) 0.037(4) -0.001(3) -0.004(3) -0.012(4) C27 0.039(4) 0.097(6) 0.052(4) -0.012(4) -0.007(3) 0.010(4) C28 0.051(6) 0.093(7) 0.060(5) 0.004(5) 0.011(4) 0.021(5) C29 0.072(6) 0.045(5) 0.067(5) -0.001(4) 0.014(5) 0.019(4) C30 0.075(5) 0.041(4) 0.051(4) -0.005(3) -0.001(4) -0.005(4) C31 0.126(6) 0.065(5) 0.049(5) 0.004(4) -0.023(4) -0.059(5) C32 0.163(9) 0.176(9) 0.072(6) -0.024(6) -0.018(6) -0.094(7) C33 0.138(7) 0.193(9) 0.050(5) -0.003(5) 0.021(5) -0.105(7) C34 0.131(7) 0.095(6) 0.053(5) 0.008(4) -0.017(5) -0.043(6) C35 0.127(7) 0.146(8) 0.191(10) 0.109(7) -0.118(7) -0.086(6) C36 0.215(10) 0.118(7) 0.101(7) -0.004(6) -0.047(6) -0.114(7) C37 0.054(4) 0.035(3) 0.035(3) -0.001(3) -0.006(3) -0.016(3) C38 0.052(4) 0.053(4) 0.041(4) -0.005(3) -0.006(3) -0.013(3) C39 0.072(5) 0.031(3) 0.052(4) 0.002(3) -0.011(3) -0.002(3) C40 0.050(4) 0.046(4) 0.040(4) -0.009(3) -0.005(3) -0.018(3) C41 0.076(5) 0.074(5) 0.062(4) -0.024(4) 0.012(3) -0.045(4) C42 0.045(4) 0.042(3) 0.042(4) -0.007(3) 0.006(3) -0.015(3) C43 0.029(3) 0.033(3) 0.032(3) -0.003(2) -0.002(2) -0.014(3) C44 0.029(3) 0.029(3) 0.043(3) -0.002(3) -0.003(3) -0.016(3) C45 0.049(4) 0.037(3) 0.041(4) 0.003(3) -0.008(3) -0.020(3) C46 0.056(4) 0.040(3) 0.047(4) 0.006(3) -0.004(3) -0.029(3) C47 0.047(4) 0.045(4) 0.064(4) -0.003(3) -0.012(3) -0.032(3) C48 0.046(4) 0.045(4) 0.042(4) -0.003(3) -0.012(3) -0.027(3) C49 0.042(3) 0.033(3) 0.035(3) -0.009(3) -0.015(3) -0.018(3) C50 0.042(4) 0.040(3) 0.046(4) -0.009(3) -0.013(3) -0.019(3) C51 0.045(4) 0.036(3) 0.051(4) -0.015(3) -0.020(3) -0.012(3) C52 0.031(3) 0.057(4) 0.049(4) -0.016(3) -0.011(3) -0.010(3) C53 0.049(4) 0.055(4) 0.038(4) -0.001(3) -0.009(3) -0.025(3) C54 0.036(3) 0.034(3) 0.041(4) -0.004(3) -0.016(3) -0.013(3) C55 0.032(3) 0.028(3) 0.041(3) 0.003(3) -0.010(3) -0.018(3) C56 0.041(4) 0.047(4) 0.049(4) -0.003(3) -0.014(3) -0.011(3) C57 0.047(4) 0.056(4) 0.056(4) 0.011(4) -0.023(4) -0.014(3) C58 0.062(5) 0.081(5) 0.053(5) 0.015(4) -0.031(4) -0.041(4) C59 0.059(5) 0.061(4) 0.050(4) -0.002(3) -0.023(4) -0.023(4) C60 0.046(4) 0.040(3) 0.053(4) -0.002(3) -0.015(3) -0.022(3) C61 0.023(3) 0.030(3) 0.037(3) -0.006(2) -0.010(2) -0.010(2) C62 0.028(3) 0.035(3) 0.028(3) -0.008(2) -0.005(2) -0.015(3) C63 0.034(3) 0.040(3) 0.040(3) -0.003(3) -0.007(3) -0.019(3) C64 0.031(3) 0.029(3) 0.047(4) -0.013(3) 0.000(3) -0.010(3) C65 0.042(4) 0.025(3) 0.054(4) -0.012(3) -0.013(3) -0.010(3) C66 0.031(3) 0.034(3) 0.046(4) -0.004(3) -0.012(3) -0.015(3) C67 0.025(3) 0.022(3) 0.046(4) -0.012(2) 0.000(3) -0.005(2) C68 0.035(3) 0.036(3) 0.047(4) -0.013(3) 0.002(3) -0.014(3) C69 0.043(4) 0.044(4) 0.042(4) -0.018(3) -0.008(3) -0.009(3) C70 0.039(4) 0.037(3) 0.039(4) -0.005(3) 0.000(3) -0.011(3) C71 0.031(3) 0.036(3) 0.049(4) -0.007(3) 0.003(3) -0.015(3) C72 0.030(3) 0.028(3) 0.047(4) -0.006(3) -0.005(3) -0.010(3) C73 0.056(4) 0.070(4) 0.058(4) -0.014(4) -0.018(3) -0.033(4) C74 0.117(6) 0.087(6) 0.122(7) -0.037(5) -0.046(5) -0.054(5) C75 0.054(4) 0.128(6) 0.053(4) -0.005(4) -0.018(3) -0.047(4) C76 0.045(4) 0.097(5) 0.079(5) -0.054(4) -0.012(4) -0.024(4) C77 0.034(4) 0.075(5) 0.175(8) -0.054(5) -0.016(5) -0.009(4) C78 0.050(4) 0.156(7) 0.050(4) -0.032(5) -0.005(3) -0.038(5) C79 0.063(4) 0.050(4) 0.049(4) 0.006(3) -0.025(3) -0.038(3) C80 0.043(4) 0.044(4) 0.102(5) -0.014(4) -0.028(4) -0.012(3) C81 0.103(6) 0.140(7) 0.059(5) 0.014(5) -0.037(4) -0.089(5) C82 0.034(4) 0.158(7) 0.117(6) -0.108(6) 0.032(4) -0.060(4) C83 0.145(7) 0.102(6) 0.080(6) -0.036(5) -0.009(5) -0.067(6) C84 0.037(4) 0.202(9) 0.186(9) -0.167(7) 0.019(5) -0.043(5) N1S 0.080(5) 0.104(5) 0.116(6) -0.031(5) -0.003(4) -0.057(4) C2S 0.077(5) 0.084(6) 0.083(6) -0.019(5) 0.009(4) -0.051(5) C1S 0.119(7) 0.067(5) 0.109(7) -0.023(5) 0.007(5) -0.052(5) N1NI 0.067(5) 0.046(4) 0.101(5) 0.010(3) -0.018(4) -0.031(4) O1NI 0.068(4) 0.077(4) 0.141(5) 0.006(3) 0.007(3) -0.037(3) O2NI 0.070(4) 0.051(3) 0.185(6) 0.009(3) -0.003(4) -0.019(3) O3NI 0.105(4) 0.079(4) 0.233(7) -0.033(4) -0.062(4) -0.034(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y1 O6 2.261(3) . ? Y1 O1 2.283(3) . ? Y1 O3 2.314(3) . ? Y1 O5 2.319(3) . ? Y1 O4 2.330(3) . ? Y1 O2 2.335(3) . ? Y1 O7 2.431(3) . ? Y1 O8 2.485(3) . ? Y1 N5 2.879(4) . ? P1 O1 1.502(3) . ? P1 N1 1.637(4) . ? P1 C7 1.799(5) . ? P1 C1 1.827(5) . ? P2 O2 1.493(3) . ? P2 C19 1.811(5) . ? P2 C13 1.811(5) . ? P2 C2 1.818(5) . ? P3 O3 1.498(3) . ? P3 N2 1.631(4) . ? P3 C25 1.797(5) . ? P3 C20 1.818(5) . ? P4 O4 1.507(3) . ? P4 N3 1.639(4) . ? P4 C49 1.798(5) . ? P4 C43 1.824(5) . ? P5 O5 1.489(3) . ? P5 C55 1.813(5) . ? P5 C61 1.815(5) . ? P5 C44 1.830(4) . ? P6 O6 1.498(3) . ? P6 N4 1.631(4) . ? P6 C67 1.793(5) . ? P6 C62 1.805(5) . ? O8 N5 1.282(4) . ? O7 N5 1.258(5) . ? O9 N5 1.225(5) . ? N1 C31 1.459(7) . ? N1 C34 1.507(8) . ? N2 C40 1.491(6) . ? N2 C37 1.494(6) . ? N3 C73 1.479(6) . ? N3 C76 1.491(7) . ? N4 C79 1.487(6) . ? N4 C82 1.566(7) . ? C1 C6 1.383(6) . ? C1 C2 1.409(6) . ? C2 C3 1.392(6) . ? C3 C4 1.374(7) . ? C3 H3 0.95 . ? C4 C5 1.355(7) . ? C4 H4 0.95 . ? C5 C6 1.388(7) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C12 1.356(6) . ? C7 C8 1.388(7) . ? C8 C9 1.406(7) . ? C8 H8 0.95 . ? C9 C10 1.336(7) . ? C9 H9 0.95 . ? C10 C11 1.387(8) . ? C10 H10 0.95 . ? C11 C12 1.402(7) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C14 1.366(7) . ? C13 C18 1.395(7) . ? C14 C15 1.405(8) . ? C14 H14 0.95 . ? C15 C16 1.384(9) . ? C15 H15 0.95 . ? C16 C17 1.335(8) . ? C16 H16 0.95 . ? C17 C18 1.366(7) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? C19 C24 1.402(6) . ? C19 C20 1.415(6) . ? C20 C21 1.392(6) . ? C21 C22 1.386(7) . ? C21 H21 0.95 . ? C22 C23 1.367(7) . ? C22 H22 0.95 . ? C23 C24 1.365(7) . ? C23 H23 0.95 . ? C24 H24 0.95 . ? C25 C26 1.374(7) . ? C25 C30 1.412(7) . ? C26 C27 1.384(7) . ? C26 H26 0.95 . ? C27 C28 1.368(9) . ? C27 H27 0.95 . ? C28 C29 1.382(9) . ? C28 H28 0.95 . ? C29 C30 1.375(8) . ? C29 H29 0.95 . ? C30 H30 0.95 . ? C31 C32 1.424(8) . ? C31 C33 1.524(8) . ? C31 H31 1 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 C36 1.472(8) . ? C34 C35 1.510(8) . ? C34 H34 1 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 C39 1.507(6) . ? C37 C38 1.513(6) . ? C37 H37 1 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 C42 1.510(7) . ? C40 C41 1.554(6) . ? C40 H40 1 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 C48 1.385(6) . ? C43 C44 1.418(6) . ? C44 C45 1.393(6) . ? C45 C46 1.391(6) . ? C45 H45 0.95 . ? C46 C47 1.372(6) . ? C46 H46 0.95 . ? C47 C48 1.374(6) . ? C47 H47 0.95 . ? C48 H48 0.95 . ? C49 C54 1.380(6) . ? C49 C50 1.387(6) . ? C50 C51 1.381(7) . ? C50 H50 0.95 . ? C51 C52 1.380(6) . ? C51 H51 0.95 . ? C52 C53 1.374(7) . ? C52 H52 0.95 . ? C53 C54 1.395(7) . ? C53 H53 0.95 . ? C54 H54 0.95 . ? C55 C60 1.377(7) . ? C55 C56 1.380(6) . ? C56 C57 1.378(7) . ? C56 H56 0.95 . ? C57 C58 1.365(8) . ? C57 H57 0.95 . ? C58 C59 1.361(7) . ? C58 H58 0.95 . ? C59 C60 1.385(6) . ? C59 H59 0.95 . ? C60 H60 0.95 . ? C61 C66 1.390(6) . ? C61 C62 1.408(6) . ? C62 C63 1.417(6) . ? C63 C64 1.367(6) . ? C63 H63 0.95 . ? C64 C65 1.363(6) . ? C64 H64 0.95 . ? C65 C66 1.395(6) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? C67 C72 1.382(6) . ? C67 C68 1.425(6) . ? C68 C69 1.371(6) . ? C68 H68 0.95 . ? C69 C70 1.383(6) . ? C69 H69 0.95 . ? C70 C71 1.372(6) . ? C70 H70 0.95 . ? C71 C72 1.392(6) . ? C71 H71 0.95 . ? C72 H72 0.95 . ? C73 C74 1.471(7) . ? C73 C75 1.523(7) . ? C73 H73 1 . ? C74 H74A 0.98 . ? C74 H74B 0.98 . ? C74 H74C 0.98 . ? C75 H75A 0.98 . ? C75 H75B 0.98 . ? C75 H75C 0.98 . ? C76 C77 1.484(8) . ? C76 C78 1.517(8) . ? C76 H76 1 . ? C77 H77A 0.98 . ? C77 H77B 0.98 . ? C77 H77C 0.98 . ? C78 H78A 0.98 . ? C78 H78B 0.98 . ? C78 H78C 0.98 . ? C79 C81 1.506(7) . ? C79 C80 1.541(7) . ? C79 H79 1 . ? C80 H80A 0.98 . ? C80 H80B 0.98 . ? C80 H80C 0.98 . ? C81 H81A 0.98 . ? C81 H81B 0.98 . ? C81 H81C 0.98 . ? C82 C83 1.480(7) . ? C82 C84 1.518(8) . ? C82 H82 1 . ? C83 H83A 0.98 . ? C83 H83B 0.98 . ? C83 H83C 0.98 . ? C84 H84A 0.98 . ? C84 H84B 0.98 . ? C84 H84C 0.98 . ? N1S C2S 1.133(8) . ? C2S C1S 1.451(8) . ? C1S H1S 0.98 . ? C1S H2S 0.98 . ? C1S H3S 0.98 . ? N1NI O1NI 1.220(5) . ? N1NI O3NI 1.221(6) . ? N1NI O2NI 1.235(6) . ? N2NI O6NI 1.2193 . ? N2NI O4NI 1.2207 . ? N2NI O5NI 1.2336 . ? 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 O6 Y1 O1 161.87(10) . . ? O6 Y1 O3 90.60(10) . . ? O1 Y1 O3 97.79(11) . . ? O6 Y1 O5 73.64(10) . . ? O1 Y1 O5 89.73(10) . . ? O3 Y1 O5 139.47(10) . . ? O6 Y1 O4 92.47(10) . . ? O1 Y1 O4 88.97(11) . . ? O3 Y1 O4 147.76(10) . . ? O5 Y1 O4 71.60(10) . . ? O6 Y1 O2 94.71(10) . . ? O1 Y1 O2 73.05(10) . . ? O3 Y1 O2 71.40(10) . . ? O5 Y1 O2 72.98(10) . . ? O4 Y1 O2 140.10(10) . . ? O6 Y1 O7 126.19(11) . . ? O1 Y1 O7 71.72(11) . . ? O3 Y1 O7 75.15(10) . . ? O5 Y1 O7 143.89(10) . . ? O4 Y1 O7 77.22(10) . . ? O2 Y1 O7 126.64(11) . . ? O6 Y1 O8 74.52(11) . . ? O1 Y1 O8 122.89(11) . . ? O3 Y1 O8 78.04(10) . . ? O5 Y1 O8 129.66(11) . . ? O4 Y1 O8 71.93(10) . . ? O2 Y1 O8 147.50(10) . . ? O7 Y1 O8 51.93(10) . . ? O6 Y1 N5 100.87(12) . . ? O1 Y1 N5 96.70(12) . . ? O3 Y1 N5 76.70(11) . . ? O5 Y1 N5 142.07(11) . . ? O4 Y1 N5 71.20(11) . . ? O2 Y1 N5 144.50(12) . . ? O7 Y1 N5 25.66(11) . . ? O8 Y1 N5 26.37(10) . . ? O1 P1 N1 112.6(2) . . ? O1 P1 C7 108.3(2) . . ? N1 P1 C7 109.4(2) . . ? O1 P1 C1 113.3(2) . . ? N1 P1 C1 108.8(2) . . ? C7 P1 C1 104.1(2) . . ? O2 P2 C19 114.4(2) . . ? O2 P2 C13 109.1(2) . . ? C19 P2 C13 105.1(2) . . ? O2 P2 C2 117.8(2) . . ? C19 P2 C2 105.1(2) . . ? C13 P2 C2 104.2(2) . . ? O3 P3 N2 118.0(2) . . ? O3 P3 C25 109.5(2) . . ? N2 P3 C25 107.0(2) . . ? O3 P3 C20 108.9(2) . . ? N2 P3 C20 104.3(2) . . ? C25 P3 C20 108.7(3) . . ? O4 P4 N3 114.49(19) . . ? O4 P4 C49 110.8(2) . . ? N3 P4 C49 108.2(2) . . ? O4 P4 C43 108.9(2) . . ? N3 P4 C43 107.3(2) . . ? C49 P4 C43 106.8(2) . . ? O5 P5 C55 108.0(2) . . ? O5 P5 C61 119.5(2) . . ? C55 P5 C61 103.5(2) . . ? O5 P5 C44 112.2(2) . . ? C55 P5 C44 107.0(2) . . ? C61 P5 C44 105.7(2) . . ? O6 P6 N4 114.1(2) . . ? O6 P6 C67 106.75(19) . . ? N4 P6 C67 110.2(2) . . ? O6 P6 C62 113.40(19) . . ? N4 P6 C62 106.8(2) . . ? C67 P6 C62 105.2(2) . . ? P1 O1 Y1 154.45(19) . . ? P2 O2 Y1 138.95(18) . . ? P3 O3 Y1 172.95(18) . . ? P4 O4 Y1 166.39(19) . . ? P5 O5 Y1 140.38(18) . . ? P6 O6 Y1 156.60(18) . . ? N5 O8 Y1 94.2(3) . . ? N5 O7 Y1 97.5(3) . . ? C31 N1 C34 121.8(5) . . ? C31 N1 P1 119.0(4) . . ? C34 N1 P1 119.0(4) . . ? C40 N2 C37 112.9(4) . . ? C40 N2 P3 117.4(3) . . ? C37 N2 P3 123.9(3) . . ? C73 N3 C76 114.0(4) . . ? C73 N3 P4 129.4(4) . . ? C76 N3 P4 115.4(4) . . ? O9 N5 O7 122.3(5) . . ? O9 N5 O8 121.8(5) . . ? O7 N5 O8 115.9(4) . . ? O9 N5 Y1 174.3(3) . . ? O7 N5 Y1 56.8(2) . . ? O8 N5 Y1 59.4(2) . . ? C79 N4 C82 124.3(4) . . ? C79 N4 P6 123.9(3) . . ? C82 N4 P6 111.6(3) . . ? C6 C1 C2 117.8(5) . . ? C6 C1 P1 114.9(4) . . ? C2 C1 P1 127.3(4) . . ? C3 C2 C1 118.3(5) . . ? C3 C2 P2 113.6(4) . . ? C1 C2 P2 127.9(4) . . ? C4 C3 C2 123.0(5) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C5 C4 C3 118.4(6) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C6 120.5(6) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 122.0(6) . . ? C1 C6 H6 119 . . ? C5 C6 H6 119 . . ? C12 C7 C8 118.8(5) . . ? C12 C7 P1 123.2(4) . . ? C8 C7 P1 117.9(4) . . ? C7 C8 C9 120.5(5) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 119.9(6) . . ? C10 C9 H9 120 . . ? C8 C9 H9 120 . . ? C9 C10 C11 120.3(6) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 119.6(6) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C7 C12 C11 120.6(6) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C18 119.6(5) . . ? C14 C13 P2 117.2(4) . . ? C18 C13 P2 123.1(5) . . ? C13 C14 C15 119.2(6) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 119.7(7) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 120.2(7) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 121.3(7) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C13 120.0(6) . . ? C17 C18 H18 120 . . ? C13 C18 H18 120 . . ? C24 C19 C20 117.7(5) . . ? C24 C19 P2 116.2(4) . . ? C20 C19 P2 125.9(4) . . ? C21 C20 C19 118.7(5) . . ? C21 C20 P3 117.1(4) . . ? C19 C20 P3 124.2(4) . . ? C22 C21 C20 122.0(5) . . ? C22 C21 H21 119 . . ? C20 C21 H21 119 . . ? C23 C22 C21 118.7(5) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C24 C23 C22 121.0(6) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C19 121.7(5) . . ? C23 C24 H24 119.1 . . ? C19 C24 H24 119.1 . . ? C26 C25 C30 118.1(5) . . ? C26 C25 P3 120.8(5) . . ? C30 C25 P3 121.1(5) . . ? C25 C26 C27 121.9(6) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C28 C27 C26 119.2(7) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C29 120.5(8) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C30 C29 C28 120.3(8) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C25 119.9(7) . . ? C29 C30 H30 120 . . ? C25 C30 H30 120 . . ? C32 C31 N1 119.4(6) . . ? C32 C31 C33 108.0(6) . . ? N1 C31 C33 114.9(5) . . ? C32 C31 H31 104.3 . . ? N1 C31 H31 104.3 . . ? C33 C31 H31 104.3 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C34 N1 108.9(6) . . ? C36 C34 C35 119.0(6) . . ? N1 C34 C35 112.0(7) . . ? C36 C34 H34 105.3 . . ? N1 C34 H34 105.3 . . ? C35 C34 H34 105.3 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N2 C37 C39 114.5(4) . . ? N2 C37 C38 113.7(4) . . ? C39 C37 C38 113.4(4) . . ? N2 C37 H37 104.6 . . ? C39 C37 H37 104.6 . . ? C38 C37 H37 104.6 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N2 C40 C42 113.3(4) . . ? N2 C40 C41 111.0(4) . . ? C42 C40 C41 110.4(4) . . ? N2 C40 H40 107.3 . . ? C42 C40 H40 107.3 . . ? C41 C40 H40 107.3 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 C44 117.5(4) . . ? C48 C43 P4 117.0(4) . . ? C44 C43 P4 125.5(4) . . ? C45 C44 C43 118.9(4) . . ? C45 C44 P5 116.9(4) . . ? C43 C44 P5 124.2(4) . . ? C46 C45 C44 121.8(5) . . ? C46 C45 H45 119.1 . . ? C44 C45 H45 119.1 . . ? C47 C46 C45 118.8(5) . . ? C47 C46 H46 120.6 . . ? C45 C46 H46 120.6 . . ? C46 C47 C48 120.1(5) . . ? C46 C47 H47 120 . . ? C48 C47 H47 120 . . ? C47 C48 C43 122.8(5) . . ? C47 C48 H48 118.6 . . ? C43 C48 H48 118.6 . . ? C54 C49 C50 119.6(5) . . ? C54 C49 P4 117.5(4) . . ? C50 C49 P4 122.9(4) . . ? C51 C50 C49 120.5(5) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C52 C51 C50 119.7(5) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C53 C52 C51 120.4(5) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C52 C53 C54 120.0(5) . . ? C52 C53 H53 120 . . ? C54 C53 H53 120 . . ? C49 C54 C53 119.8(5) . . ? C49 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C60 C55 C56 119.1(5) . . ? C60 C55 P5 117.0(4) . . ? C56 C55 P5 123.9(4) . . ? C57 C56 C55 120.1(6) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C58 C57 C56 120.1(6) . . ? C58 C57 H57 119.9 . . ? C56 C57 H57 119.9 . . ? C59 C58 C57 120.5(5) . . ? C59 C58 H58 119.7 . . ? C57 C58 H58 119.7 . . ? C58 C59 C60 119.7(6) . . ? C58 C59 H59 120.1 . . ? C60 C59 H59 120.1 . . ? C55 C60 C59 120.4(5) . . ? C55 C60 H60 119.8 . . ? C59 C60 H60 119.8 . . ? C66 C61 C62 118.5(5) . . ? C66 C61 P5 113.9(4) . . ? C62 C61 P5 127.1(4) . . ? C61 C62 C63 116.9(4) . . ? C61 C62 P6 128.0(4) . . ? C63 C62 P6 115.0(3) . . ? C64 C63 C62 123.1(5) . . ? C64 C63 H63 118.4 . . ? C62 C63 H63 118.4 . . ? C65 C64 C63 119.9(5) . . ? C65 C64 H64 120.1 . . ? C63 C64 H64 120.1 . . ? C64 C65 C66 118.7(5) . . ? C64 C65 H65 120.7 . . ? C66 C65 H65 120.7 . . ? C61 C66 C65 122.9(5) . . ? C61 C66 H66 118.6 . . ? C65 C66 H66 118.6 . . ? C72 C67 C68 118.1(5) . . ? C72 C67 P6 124.2(4) . . ? C68 C67 P6 117.7(4) . . ? C69 C68 C67 119.6(5) . . ? C69 C68 H68 120.2 . . ? C67 C68 H68 120.2 . . ? C68 C69 C70 121.1(5) . . ? C68 C69 H69 119.4 . . ? C70 C69 H69 119.4 . . ? C71 C70 C69 120.2(5) . . ? C71 C70 H70 119.9 . . ? C69 C70 H70 119.9 . . ? C70 C71 C72 119.4(5) . . ? C70 C71 H71 120.3 . . ? C72 C71 H71 120.3 . . ? C67 C72 C71 121.6(5) . . ? C67 C72 H72 119.2 . . ? C71 C72 H72 119.2 . . ? C74 C73 N3 116.3(5) . . ? C74 C73 C75 113.8(6) . . ? N3 C73 C75 115.3(5) . . ? C74 C73 H73 103 . . ? N3 C73 H73 103 . . ? C75 C73 H73 103 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C77 C76 N3 113.4(6) . . ? C77 C76 C78 111.0(5) . . ? N3 C76 C78 112.5(5) . . ? C77 C76 H76 106.4 . . ? N3 C76 H76 106.4 . . ? C78 C76 H76 106.4 . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C76 C78 H78A 109.5 . . ? C76 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C76 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N4 C79 C81 114.4(5) . . ? N4 C79 C80 111.9(4) . . ? C81 C79 C80 110.7(4) . . ? N4 C79 H79 106.4 . . ? C81 C79 H79 106.4 . . ? C80 C79 H79 106.4 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C84 116.2(5) . . ? C83 C82 N4 113.4(5) . . ? C84 C82 N4 109.5(6) . . ? C83 C82 H82 105.6 . . ? C84 C82 H82 105.6 . . ? N4 C82 H82 105.6 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? N1S C2S C1S 179.8(10) . . ? C2S C1S H1S 109.5 . . ? C2S C1S H2S 109.5 . . ? H1S C1S H2S 109.5 . . ? C2S C1S H3S 109.5 . . ? H1S C1S H3S 109.5 . . ? H2S C1S H3S 109.5 . . ? O1NI N1NI O3NI 118.5(6) . . ? O1NI N1NI O2NI 121.2(6) . . ? O3NI N1NI O2NI 119.6(6) . . ? O6NI N2NI O4NI 118.5 . . ? O6NI N2NI O5NI 121.2 . . ? O4NI N2NI O5NI 119.5 . . ? # END of CIF # END of CIF # Attachment '- complex12_AG24_P21c_CCDC806041.cif' data_ag24 _database_code_depnum_ccdc_archive 'CCDC 806041' #TrackingRef '- complex12_AG24_P21c_CCDC806041.cif' _audit_creation_date 2010-11-28T19:49:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C44 H54 N6 O12 P3 Y' _chemical_formula_moiety 'C42 H51 N5 O12 P3 Y, C2 H3 N' _chemical_formula_weight 1040.75 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.5641(7) _cell_length_b 20.9926(8) _cell_length_c 24.1037(8) _cell_angle_alpha 90 _cell_angle_beta 119.372(2) _cell_angle_gamma 90 _cell_volume 9508.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2081 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 17.59 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.201 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4320 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.395 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_reflns_av_R_equivalents 0.0912 _diffrn_reflns_av_unetI/netI 0.1699 _diffrn_reflns_number 49562 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 24.46 _diffrn_reflns_theta_full 24.46 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 15665 _reflns_number_gt 7722 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution SUPERFLIP _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0099P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 15665 _refine_ls_number_parameters 1189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0968 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 0.825 _refine_ls_restrained_S_all 0.825 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.501 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.071 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y1 Y 0.57324(2) 0.19679(2) 0.26851(2) 0.01428(12) Uani 1 1 d . . . Y2 Y 0.07312(2) 0.29227(2) 0.26573(2) 0.01540(12) Uani 1 1 d . . . P1 P 0.50558(6) 0.31198(6) 0.34743(6) 0.0151(3) Uani 1 1 d . . . P2 P 0.50919(6) 0.14558(6) 0.36746(6) 0.0142(3) Uani 1 1 d . . . P3 P 0.70885(6) 0.16066(6) 0.43255(6) 0.0146(3) Uani 1 1 d . . . P4 P 0.22084(6) 0.32386(6) 0.42734(6) 0.0161(3) Uani 1 1 d . . . P5 P 0.02981(6) 0.34924(6) 0.37796(6) 0.0165(3) Uani 1 1 d . . . P6 P 0.00790(6) 0.18375(6) 0.35021(6) 0.0158(3) Uani 1 1 d . . . O1 O 0.55353(13) 0.27105(13) 0.33278(13) 0.0147(8) Uani 1 1 d . . . O2 O 0.52854(13) 0.13448(13) 0.31636(13) 0.0128(7) Uani 1 1 d . . . O3 O 0.66745(13) 0.17420(13) 0.36280(13) 0.0136(8) Uani 1 1 d . . . O4 O 0.17595(13) 0.30551(14) 0.35870(13) 0.0178(8) Uani 1 1 d . . . O5 O 0.04178(14) 0.35459(14) 0.32193(13) 0.0151(8) Uani 1 1 d . . . O6 O 0.05351(13) 0.22011(14) 0.32936(13) 0.0149(8) Uani 1 1 d . . . O1N1 O 0.60258(15) 0.08522(15) 0.25572(14) 0.0202(8) Uani 1 1 d . . . O2N1 O 0.64070(15) 0.16016(15) 0.21917(14) 0.0232(8) Uani 1 1 d . . . O3N1 O 0.65908(16) 0.06062(16) 0.20442(15) 0.0305(9) Uani 1 1 d . . . O1N2 O 0.65588(15) 0.28097(14) 0.28173(14) 0.0182(8) Uani 1 1 d . . . O2N2 O 0.56467(15) 0.27373(15) 0.18801(14) 0.0217(8) Uani 1 1 d . . . O3N2 O 0.65362(15) 0.33538(15) 0.20334(15) 0.0252(9) Uani 1 1 d . . . O2N3 O 0.44584(15) 0.22173(15) 0.21320(14) 0.0195(8) Uani 1 1 d . . . O1N3 O 0.47883(15) 0.14715(15) 0.17125(14) 0.0232(9) Uani 1 1 d . . . O3N3 O 0.36654(15) 0.15591(16) 0.14457(14) 0.0310(10) Uani 1 1 d . . . O1N4 O 0.14535(14) 0.20399(14) 0.27014(14) 0.0186(8) Uani 1 1 d . . . O2N4 O 0.04962(14) 0.21642(15) 0.17921(13) 0.0209(8) Uani 1 1 d . . . O3N4 O 0.13400(15) 0.15238(15) 0.18641(15) 0.0241(9) Uani 1 1 d . . . O1N5 O 0.13446(16) 0.32622(15) 0.20930(14) 0.0231(8) Uani 1 1 d . . . O2N5 O 0.10878(15) 0.40215(15) 0.25482(14) 0.0212(8) Uani 1 1 d . . . O3N5 O 0.15998(16) 0.42466(16) 0.19809(16) 0.0317(9) Uani 1 1 d . . . O1N6 O -0.05668(15) 0.27714(16) 0.21693(14) 0.0223(8) Uani 1 1 d . . . O2N6 O -0.02289(15) 0.34950(15) 0.17380(14) 0.0260(9) Uani 1 1 d . . . O3N6 O -0.13342(16) 0.34779(17) 0.15356(15) 0.0336(10) Uani 1 1 d . . . N1N1 N 0.6346(2) 0.1002(2) 0.22547(19) 0.0228(10) Uani 1 1 d . . . N1N2 N 0.62614(19) 0.29870(18) 0.22455(19) 0.0189(10) Uani 1 1 d . . . N1N3 N 0.4287(2) 0.17509(19) 0.17598(18) 0.0208(10) Uani 1 1 d . . . N1N4 N 0.11087(19) 0.18949(19) 0.21173(19) 0.0204(10) Uani 1 1 d . . . N1N5 N 0.1351(2) 0.3861(2) 0.22012(19) 0.0224(11) Uani 1 1 d . . . N1N6 N -0.0729(2) 0.3249(2) 0.18084(19) 0.0246(11) Uani 1 1 d . . . N1 N -0.03723(17) 0.12235(17) 0.30707(16) 0.0151(10) Uani 1 1 d . . . N2 N 0.25567(17) 0.39546(17) 0.44387(16) 0.0138(9) Uani 1 1 d . . . N3 N 0.75451(17) 0.09408(17) 0.45456(16) 0.0128(9) Uani 1 1 d . . . N4 N 0.47015(17) 0.37599(17) 0.30365(16) 0.0131(9) Uani 1 1 d . . . C1 C 0.4308(2) 0.2640(2) 0.3381(2) 0.0152(11) Uani 1 1 d . . . C2 C 0.4319(2) 0.1980(2) 0.34283(19) 0.0130(11) Uani 1 1 d . . . C3 C 0.3678(2) 0.1661(2) 0.32682(19) 0.0167(12) Uani 1 1 d . . . H3 H 0.3677 0.1209 0.3289 0.02 Uiso 1 1 calc R . . C4 C 0.3051(2) 0.1989(2) 0.3081(2) 0.0189(12) Uani 1 1 d . . . H4 H 0.262 0.1764 0.2956 0.023 Uiso 1 1 calc R . . C5 C 0.3055(2) 0.2640(2) 0.3078(2) 0.0217(13) Uani 1 1 d . . . H5 H 0.263 0.2868 0.2971 0.026 Uiso 1 1 calc R . . C6 C 0.3677(2) 0.2970(2) 0.3229(2) 0.0198(12) Uani 1 1 d . . . H6 H 0.3676 0.3422 0.323 0.024 Uiso 1 1 calc R . . C7 C 0.6555(2) 0.1671(2) 0.4726(2) 0.0160(12) Uani 1 1 d . . . C8 C 0.5793(2) 0.17258(19) 0.4445(2) 0.0105(11) Uani 1 1 d . . . C9 C 0.5527(2) 0.1920(2) 0.4844(2) 0.0149(11) Uani 1 1 d . . . H9 H 0.5028 0.1978 0.4664 0.018 Uiso 1 1 calc R . . C10 C 0.5957(2) 0.2033(2) 0.5489(2) 0.0189(12) Uani 1 1 d . . . H10 H 0.5754 0.2168 0.5741 0.023 Uiso 1 1 calc R . . C11 C 0.6688(2) 0.1948(2) 0.5764(2) 0.0203(12) Uani 1 1 d . . . H11 H 0.6989 0.2002 0.6209 0.024 Uiso 1 1 calc R . . C12 C 0.6966(2) 0.1783(2) 0.5374(2) 0.0157(12) Uani 1 1 d . . . H12 H 0.7467 0.1743 0.5562 0.019 Uiso 1 1 calc R . . C13 C 0.5505(2) 0.3362(2) 0.4294(2) 0.0148(11) Uani 1 1 d . . . C14 C 0.6248(2) 0.3359(2) 0.4645(2) 0.0181(12) Uani 1 1 d . . . H14 H 0.6514 0.3241 0.4442 0.022 Uiso 1 1 calc R . . C15 C 0.6603(2) 0.3523(2) 0.5282(2) 0.0242(13) Uani 1 1 d . . . H15 H 0.7108 0.3518 0.551 0.029 Uiso 1 1 calc R . . C16 C 0.6232(2) 0.3692(2) 0.5590(2) 0.0280(14) Uani 1 1 d . . . H16 H 0.6475 0.3811 0.6027 0.034 Uiso 1 1 calc R . . C17 C 0.5492(2) 0.3684(2) 0.5245(2) 0.0278(14) Uani 1 1 d . . . H17 H 0.5229 0.3793 0.5453 0.033 Uiso 1 1 calc R . . C18 C 0.5133(2) 0.3524(2) 0.4612(2) 0.0201(12) Uani 1 1 d . . . H18 H 0.4628 0.3524 0.4389 0.024 Uiso 1 1 calc R . . C19 C 0.7740(2) 0.2231(2) 0.4675(2) 0.0125(11) Uani 1 1 d . . . C20 C 0.8386(2) 0.2158(2) 0.5232(2) 0.0193(12) Uani 1 1 d . . . H20 H 0.8512 0.1754 0.5436 0.023 Uiso 1 1 calc R . . C21 C 0.8847(2) 0.2668(2) 0.5493(2) 0.0269(13) Uani 1 1 d . . . H21 H 0.9291 0.2613 0.587 0.032 Uiso 1 1 calc R . . C22 C 0.8656(2) 0.3260(2) 0.5200(2) 0.0308(14) Uani 1 1 d . . . H22 H 0.8964 0.3614 0.5384 0.037 Uiso 1 1 calc R . . C23 C 0.8019(2) 0.3336(2) 0.4643(2) 0.0244(13) Uani 1 1 d . . . H23 H 0.7891 0.3741 0.4442 0.029 Uiso 1 1 calc R . . C24 C 0.7570(2) 0.2825(2) 0.4378(2) 0.0197(12) Uani 1 1 d . . . H24 H 0.7139 0.2877 0.3988 0.024 Uiso 1 1 calc R . . C25 C 0.4793(2) 0.0697(2) 0.3815(2) 0.0145(11) Uani 1 1 d . . . C26 C 0.4664(2) 0.0218(2) 0.3384(2) 0.0206(12) Uani 1 1 d . . . H26 H 0.479 0.0276 0.3061 0.025 Uiso 1 1 calc R . . C27 C 0.4354(2) -0.0346(2) 0.3414(2) 0.0260(13) Uani 1 1 d . . . H27 H 0.4272 -0.0675 0.3114 0.031 Uiso 1 1 calc R . . C28 C 0.4159(2) -0.0436(2) 0.3879(2) 0.0240(13) Uani 1 1 d . . . H28 H 0.3939 -0.0822 0.3896 0.029 Uiso 1 1 calc R . . C29 C 0.4290(2) 0.0037(2) 0.4313(2) 0.0219(12) Uani 1 1 d . . . H29 H 0.416 -0.002 0.4633 0.026 Uiso 1 1 calc R . . C30 C 0.4610(2) 0.0599(2) 0.4286(2) 0.0205(12) Uani 1 1 d . . . H30 H 0.4706 0.0922 0.4594 0.025 Uiso 1 1 calc R . . C31 C 0.5070(2) 0.4392(2) 0.3160(2) 0.0221(13) Uani 1 1 d . . . H31 H 0.4811 0.464 0.2755 0.026 Uiso 1 1 calc R . . C32 C 0.4134(2) 0.3669(2) 0.2359(2) 0.0169(12) Uani 1 1 d . . . H32 H 0.3943 0.3227 0.232 0.02 Uiso 1 1 calc R . . C33 C 0.8104(2) 0.0886(2) 0.4349(2) 0.0197(12) Uani 1 1 d . . . H33 H 0.823 0.1329 0.4287 0.024 Uiso 1 1 calc R . . C34 C 0.7311(2) 0.0322(2) 0.4677(2) 0.0166(12) Uani 1 1 d . . . H34 H 0.7576 -0.0013 0.4583 0.02 Uiso 1 1 calc R . . C35 C 0.5840(2) 0.4345(2) 0.3302(2) 0.0326(15) Uani 1 1 d . . . H35A H 0.586 0.4099 0.2966 0.049 Uiso 1 1 calc R . . H35B H 0.6127 0.4132 0.3713 0.049 Uiso 1 1 calc R . . H35C H 0.6029 0.4774 0.332 0.049 Uiso 1 1 calc R . . C36 C 0.5016(2) 0.4784(2) 0.3670(2) 0.0301(14) Uani 1 1 d . . . H36A H 0.4517 0.4811 0.3567 0.045 Uiso 1 1 calc R . . H36B H 0.5201 0.5214 0.3685 0.045 Uiso 1 1 calc R . . H36C H 0.5295 0.4579 0.4086 0.045 Uiso 1 1 calc R . . C37 C 0.4416(2) 0.3726(2) 0.1890(2) 0.0242(13) Uani 1 1 d . . . H37A H 0.4808 0.3425 0.2008 0.036 Uiso 1 1 calc R . . H37B H 0.4588 0.4161 0.1901 0.036 Uiso 1 1 calc R . . H37C H 0.4033 0.363 0.1459 0.036 Uiso 1 1 calc R . . C38 C 0.3511(2) 0.4133(2) 0.2162(2) 0.0281(14) Uani 1 1 d . . . H38A H 0.3321 0.4091 0.2456 0.042 Uiso 1 1 calc R . . H38B H 0.3136 0.4034 0.1728 0.042 Uiso 1 1 calc R . . H38C H 0.3677 0.457 0.2177 0.042 Uiso 1 1 calc R . . C39 C 0.8786(2) 0.0581(2) 0.4882(2) 0.0280(14) Uani 1 1 d . . . H39A H 0.8944 0.0821 0.5278 0.042 Uiso 1 1 calc R . . H39B H 0.9159 0.0589 0.4762 0.042 Uiso 1 1 calc R . . H39C H 0.8688 0.0139 0.4946 0.042 Uiso 1 1 calc R . . C40 C 0.7843(2) 0.0536(2) 0.3719(2) 0.0292(14) Uani 1 1 d . . . H40A H 0.7414 0.0747 0.3389 0.044 Uiso 1 1 calc R . . H40B H 0.7731 0.0094 0.3766 0.044 Uiso 1 1 calc R . . H40C H 0.8214 0.0544 0.3597 0.044 Uiso 1 1 calc R . . C41 C 0.7522(2) 0.0235(2) 0.5374(2) 0.0294(14) Uani 1 1 d . . . H41A H 0.8031 0.032 0.564 0.044 Uiso 1 1 calc R . . H41B H 0.742 -0.0203 0.5444 0.044 Uiso 1 1 calc R . . H41C H 0.725 0.0532 0.5486 0.044 Uiso 1 1 calc R . . C42 C 0.6518(2) 0.0180(2) 0.4237(2) 0.0249(13) Uani 1 1 d . . . H42A H 0.6403 0.0231 0.3793 0.037 Uiso 1 1 calc R . . H42B H 0.6231 0.0477 0.4331 0.037 Uiso 1 1 calc R . . H42C H 0.6415 -0.0258 0.4308 0.037 Uiso 1 1 calc R . . C43 C 0.1745(2) 0.3148(2) 0.4740(2) 0.0177(12) Uani 1 1 d . . . C44 C 0.1002(2) 0.3172(2) 0.4518(2) 0.0149(11) Uani 1 1 d . . . C45 C 0.0767(2) 0.3033(2) 0.4949(2) 0.0179(12) Uani 1 1 d . . . H45 H 0.027 0.3041 0.4803 0.021 Uiso 1 1 calc R . . C46 C 0.1221(2) 0.2886(2) 0.5576(2) 0.0219(13) Uani 1 1 d . . . H46 H 0.1038 0.2785 0.5853 0.026 Uiso 1 1 calc R . . C47 C 0.1943(2) 0.2886(2) 0.5798(2) 0.0216(12) Uani 1 1 d . . . H47 H 0.2267 0.2803 0.6235 0.026 Uiso 1 1 calc R . . C48 C 0.2192(2) 0.3009(2) 0.5373(2) 0.0187(12) Uani 1 1 d . . . H48 H 0.269 0.2996 0.5526 0.022 Uiso 1 1 calc R . . C49 C -0.0587(2) 0.2378(2) 0.3508(2) 0.0152(12) Uani 1 1 d . . . C50 C -0.0502(2) 0.3035(2) 0.3600(2) 0.0134(11) Uani 1 1 d . . . C51 C -0.1071(2) 0.3395(2) 0.35630(19) 0.0180(12) Uani 1 1 d . . . H51 H -0.1016 0.3841 0.3637 0.022 Uiso 1 1 calc R . . C52 C -0.1713(2) 0.3106(2) 0.3419(2) 0.0214(12) Uani 1 1 d . . . H52 H -0.2105 0.3359 0.3364 0.026 Uiso 1 1 calc R . . C53 C -0.1780(2) 0.2464(2) 0.3357(2) 0.0198(12) Uani 1 1 d . . . H53 H -0.2213 0.2267 0.3275 0.024 Uiso 1 1 calc R . . C54 C -0.1218(2) 0.2092(2) 0.3413(2) 0.0197(12) Uani 1 1 d . . . H54 H -0.1263 0.1641 0.3386 0.024 Uiso 1 1 calc R . . C55 C 0.2938(2) 0.2678(2) 0.4620(2) 0.0130(11) Uani 1 1 d . . . C56 C 0.3589(2) 0.2819(2) 0.5164(2) 0.0184(12) Uani 1 1 d . . . H56 H 0.3673 0.3234 0.5343 0.022 Uiso 1 1 calc R . . C57 C 0.4107(2) 0.2354(2) 0.5440(2) 0.0217(12) Uani 1 1 d . . . H57 H 0.4544 0.245 0.5812 0.026 Uiso 1 1 calc R . . C58 C 0.3992(2) 0.1758(2) 0.5180(2) 0.0223(13) Uani 1 1 d . . . H58 H 0.4349 0.144 0.5376 0.027 Uiso 1 1 calc R . . C59 C 0.3357(2) 0.1610(2) 0.4632(2) 0.0223(12) Uani 1 1 d . . . H59 H 0.328 0.1196 0.4451 0.027 Uiso 1 1 calc R . . C60 C 0.2840(2) 0.2075(2) 0.4354(2) 0.0156(11) Uani 1 1 d . . . H60 H 0.2411 0.198 0.3975 0.019 Uiso 1 1 calc R . . C61 C 0.0612(2) 0.1572(2) 0.4311(2) 0.0152(11) Uani 1 1 d . . . C62 C 0.1346(2) 0.1544(2) 0.4579(2) 0.0201(12) Uani 1 1 d . . . H62 H 0.1564 0.1652 0.4332 0.024 Uiso 1 1 calc R . . C63 C 0.1762(2) 0.1356(2) 0.5209(2) 0.0247(13) Uani 1 1 d . . . H63 H 0.2263 0.1326 0.5386 0.03 Uiso 1 1 calc R . . C64 C 0.1459(2) 0.1213(2) 0.5584(2) 0.0272(14) Uani 1 1 d . . . H64 H 0.1747 0.1094 0.6017 0.033 Uiso 1 1 calc R . . C65 C 0.0725(2) 0.1246(2) 0.5314(2) 0.0253(13) Uani 1 1 d . . . H65 H 0.0507 0.1142 0.5562 0.03 Uiso 1 1 calc R . . C66 C 0.0310(2) 0.1429(2) 0.4691(2) 0.0198(12) Uani 1 1 d . . . H66 H -0.0191 0.1458 0.4516 0.024 Uiso 1 1 calc R . . C67 C 0.0163(2) 0.4297(2) 0.3948(2) 0.0151(11) Uani 1 1 d . . . C68 C -0.0256(2) 0.4677(2) 0.3422(2) 0.0185(12) Uani 1 1 d . . . H68 H -0.0455 0.4502 0.3006 0.022 Uiso 1 1 calc R . . C69 C -0.0386(2) 0.5298(2) 0.3497(2) 0.0229(13) Uani 1 1 d . . . H69 H -0.0694 0.5543 0.3134 0.028 Uiso 1 1 calc R . . C70 C -0.0075(2) 0.5578(2) 0.4093(2) 0.0241(13) Uani 1 1 d . . . H70 H -0.0171 0.6009 0.4144 0.029 Uiso 1 1 calc R . . C71 C 0.0380(2) 0.5213(2) 0.4615(2) 0.0244(13) Uani 1 1 d . . . H71 H 0.0619 0.5404 0.5025 0.029 Uiso 1 1 calc R . . C72 C 0.0492(2) 0.4577(2) 0.4548(2) 0.0195(12) Uani 1 1 d . . . H72 H 0.0794 0.433 0.4912 0.023 Uiso 1 1 calc R . . C73 C 0.2197(2) 0.4470(2) 0.4602(2) 0.0213(13) Uani 1 1 d . . . H73 H 0.178 0.4261 0.4601 0.026 Uiso 1 1 calc R . . C74 C 0.3109(2) 0.4102(2) 0.4249(2) 0.0207(12) Uani 1 1 d . . . H74 H 0.3332 0.3684 0.4251 0.025 Uiso 1 1 calc R . . C75 C -0.0078(2) 0.0560(2) 0.3159(2) 0.0214(13) Uani 1 1 d . . . H75 H -0.0391 0.0334 0.275 0.026 Uiso 1 1 calc R . . C76 C -0.0973(2) 0.1356(2) 0.2414(2) 0.0181(12) Uani 1 1 d . . . H76 H -0.1114 0.1812 0.24 0.022 Uiso 1 1 calc R . . C77 C 0.2649(2) 0.4731(2) 0.5273(2) 0.0304(14) Uani 1 1 d . . . H77A H 0.2832 0.4377 0.5576 0.046 Uiso 1 1 calc R . . H77B H 0.2357 0.501 0.5379 0.046 Uiso 1 1 calc R . . H77C H 0.3048 0.4975 0.5295 0.046 Uiso 1 1 calc R . . C78 C 0.1884(2) 0.5006(2) 0.4116(2) 0.0271(13) Uani 1 1 d . . . H78A H 0.1586 0.4826 0.3691 0.041 Uiso 1 1 calc R . . H78B H 0.2271 0.5255 0.4119 0.041 Uiso 1 1 calc R . . H78C H 0.1595 0.5284 0.4225 0.041 Uiso 1 1 calc R . . C79 C 0.3714(2) 0.4516(2) 0.4738(2) 0.0258(13) Uani 1 1 d . . . H79A H 0.3895 0.4332 0.5163 0.039 Uiso 1 1 calc R . . H79B H 0.3536 0.4947 0.4731 0.039 Uiso 1 1 calc R . . H79C H 0.4098 0.4534 0.4632 0.039 Uiso 1 1 calc R . . C80 C 0.2822(2) 0.4367(2) 0.3580(2) 0.0288(14) Uani 1 1 d . . . H80A H 0.2444 0.4088 0.3275 0.043 Uiso 1 1 calc R . . H80B H 0.3207 0.4389 0.3476 0.043 Uiso 1 1 calc R . . H80C H 0.2629 0.4795 0.3558 0.043 Uiso 1 1 calc R . . C81 C 0.0673(2) 0.0532(2) 0.3242(2) 0.0361(15) Uani 1 1 d . . . H81A H 0.0686 0.0776 0.29 0.054 Uiso 1 1 calc R . . H81B H 0.0801 0.0088 0.3223 0.054 Uiso 1 1 calc R . . H81C H 0.1013 0.0716 0.3655 0.054 Uiso 1 1 calc R . . C82 C -0.0129(2) 0.0181(2) 0.3669(2) 0.0306(14) Uani 1 1 d . . . H82A H -0.0616 0.0201 0.3598 0.046 Uiso 1 1 calc R . . H82B H 0.02 0.0359 0.4088 0.046 Uiso 1 1 calc R . . H82C H -0.0002 -0.0264 0.3651 0.046 Uiso 1 1 calc R . . C83 C -0.0761(2) 0.1261(2) 0.1903(2) 0.0243(13) Uani 1 1 d . . . H83A H -0.0351 0.1531 0.1996 0.036 Uiso 1 1 calc R . . H83B H -0.1161 0.1377 0.1487 0.036 Uiso 1 1 calc R . . H83C H -0.0635 0.0813 0.1896 0.036 Uiso 1 1 calc R . . C84 C -0.1621(2) 0.0944(2) 0.2272(2) 0.0278(13) Uani 1 1 d . . . H84A H -0.1758 0.1016 0.2599 0.042 Uiso 1 1 calc R . . H84B H -0.1502 0.0494 0.2271 0.042 Uiso 1 1 calc R . . H84C H -0.2019 0.1059 0.1854 0.042 Uiso 1 1 calc R . . N1S2 N 0.1835(2) -0.0272(2) 0.1262(2) 0.0469(14) Uani 1 1 d . . . C1S2 C 0.2672(2) 0.0659(2) 0.1883(2) 0.0371(15) Uani 1 1 d . . . H1S2 H 0.2459 0.0909 0.209 0.056 Uiso 1 1 calc R . . H2S2 H 0.2747 0.0932 0.1592 0.056 Uiso 1 1 calc R . . H3S2 H 0.313 0.0486 0.2208 0.056 Uiso 1 1 calc R . . C2S2 C 0.2198(3) 0.0138(3) 0.1528(2) 0.0295(14) Uani 1 1 d . . . N1S1 N 0.7517(2) -0.0528(2) 0.6710(2) 0.0439(13) Uani 1 1 d . . . C1S1 C 0.7827(2) 0.0632(2) 0.7107(2) 0.0351(15) Uani 1 1 d . . . H1S1 H 0.8047 0.0844 0.6885 0.053 Uiso 1 1 calc R . . H2S1 H 0.8158 0.0634 0.7566 0.053 Uiso 1 1 calc R . . H3S1 H 0.739 0.0858 0.7019 0.053 Uiso 1 1 calc R . . C2S1 C 0.7656(3) -0.0021(3) 0.6886(2) 0.0289(14) 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 Y1 0.0098(2) 0.0180(3) 0.0145(3) 0.0003(2) 0.0055(2) -0.0004(2) Y2 0.0099(2) 0.0213(3) 0.0145(3) 0.0000(2) 0.0055(2) 0.0002(2) P1 0.0123(6) 0.0158(8) 0.0169(8) -0.0016(6) 0.0070(6) -0.0009(6) P2 0.0095(6) 0.0172(8) 0.0151(8) 0.0006(6) 0.0056(6) -0.0008(6) P3 0.0094(6) 0.0167(8) 0.0161(8) 0.0005(6) 0.0050(6) -0.0006(6) P4 0.0112(6) 0.0191(8) 0.0177(8) -0.0002(6) 0.0070(6) -0.0001(6) P5 0.0116(6) 0.0178(8) 0.0213(8) -0.0017(6) 0.0090(6) -0.0005(6) P6 0.0129(6) 0.0167(8) 0.0181(8) 0.0001(6) 0.0077(6) 0.0011(6) O1 0.0123(16) 0.0136(19) 0.019(2) -0.0012(15) 0.0083(15) -0.0019(15) O2 0.0064(15) 0.020(2) 0.0104(18) -0.0004(14) 0.0026(14) -0.0010(14) O3 0.0090(15) 0.0175(19) 0.0140(19) 0.0036(14) 0.0054(14) 0.0025(14) O4 0.0092(15) 0.023(2) 0.018(2) -0.0032(15) 0.0042(14) -0.0016(15) O5 0.0137(16) 0.0191(19) 0.0152(19) 0.0019(15) 0.0091(14) -0.0020(15) O6 0.0092(16) 0.0164(19) 0.0191(19) 0.0032(15) 0.0071(15) 0.0035(15) O1N1 0.0179(18) 0.028(2) 0.020(2) 0.0049(16) 0.0131(16) 0.0039(16) O2N1 0.0287(19) 0.019(2) 0.032(2) -0.0023(17) 0.0229(17) -0.0005(17) O3N1 0.033(2) 0.031(2) 0.036(2) -0.0092(18) 0.0231(19) 0.0057(18) O1N2 0.0181(17) 0.019(2) 0.015(2) 0.0046(16) 0.0066(15) 0.0042(16) O2N2 0.0113(17) 0.031(2) 0.019(2) -0.0002(17) 0.0047(15) -0.0033(16) O3N2 0.0256(19) 0.025(2) 0.034(2) 0.0099(17) 0.0217(17) -0.0023(17) O2N3 0.0173(18) 0.021(2) 0.017(2) -0.0020(17) 0.0057(16) -0.0013(16) O1N3 0.0156(17) 0.028(2) 0.022(2) -0.0045(17) 0.0064(16) 0.0043(17) O3N3 0.0085(17) 0.047(3) 0.023(2) 0.0008(18) -0.0037(16) -0.0118(18) O1N4 0.0133(16) 0.026(2) 0.012(2) -0.0004(16) 0.0023(15) 0.0016(16) O2N4 0.0123(17) 0.028(2) 0.019(2) 0.0018(16) 0.0053(15) 0.0038(16) O3N4 0.0233(18) 0.023(2) 0.035(2) -0.0094(17) 0.0215(17) -0.0008(17) O1N5 0.0266(19) 0.021(2) 0.026(2) 0.0005(17) 0.0163(17) 0.0000(17) O2N5 0.0198(18) 0.033(2) 0.016(2) -0.0030(16) 0.0133(16) 0.0000(17) O3N5 0.031(2) 0.032(2) 0.039(2) 0.0083(19) 0.0228(19) -0.0038(18) O1N6 0.0151(18) 0.027(2) 0.022(2) 0.0029(18) 0.0067(16) -0.0006(17) O2N6 0.0181(18) 0.031(2) 0.029(2) 0.0058(17) 0.0108(17) -0.0015(18) O3N6 0.0150(18) 0.046(3) 0.029(2) -0.0007(19) 0.0028(17) 0.0186(19) N1N1 0.018(2) 0.026(3) 0.020(3) -0.005(2) 0.005(2) -0.001(2) N1N2 0.015(2) 0.018(3) 0.026(3) 0.001(2) 0.012(2) 0.006(2) N1N3 0.023(2) 0.018(3) 0.018(3) 0.002(2) 0.008(2) 0.001(2) N1N4 0.015(2) 0.025(3) 0.019(3) 0.002(2) 0.007(2) -0.007(2) N1N5 0.013(2) 0.032(3) 0.016(3) 0.009(2) 0.002(2) 0.000(2) N1N6 0.026(3) 0.028(3) 0.016(3) -0.006(2) 0.007(2) 0.004(2) N1 0.013(2) 0.014(2) 0.015(2) -0.0020(18) 0.0042(18) 0.0032(18) N2 0.012(2) 0.015(2) 0.020(2) -0.0019(18) 0.0125(18) -0.0006(18) N3 0.0092(19) 0.014(2) 0.018(2) 0.0009(18) 0.0087(18) -0.0007(18) N4 0.0092(19) 0.014(2) 0.011(2) 0.0011(18) 0.0010(18) 0.0006(18) C1 0.014(2) 0.014(3) 0.021(3) 0.000(2) 0.011(2) -0.004(2) C2 0.015(2) 0.016(3) 0.009(3) 0.001(2) 0.007(2) 0.003(2) C3 0.016(2) 0.014(3) 0.022(3) 0.001(2) 0.011(2) 0.001(2) C4 0.014(2) 0.023(3) 0.021(3) 0.007(2) 0.009(2) -0.001(2) C5 0.008(2) 0.034(4) 0.021(3) 0.003(3) 0.005(2) 0.007(2) C6 0.018(3) 0.021(3) 0.023(3) 0.003(2) 0.012(2) 0.001(2) C7 0.013(2) 0.023(3) 0.010(3) 0.001(2) 0.004(2) 0.003(2) C8 0.011(2) 0.004(3) 0.016(3) 0.001(2) 0.007(2) 0.001(2) C9 0.012(2) 0.013(3) 0.019(3) 0.002(2) 0.007(2) -0.001(2) C10 0.023(3) 0.018(3) 0.022(3) 0.001(2) 0.016(2) 0.000(2) C11 0.018(3) 0.027(3) 0.009(3) -0.001(2) 0.001(2) -0.004(2) C12 0.009(2) 0.016(3) 0.020(3) 0.005(2) 0.005(2) 0.002(2) C13 0.015(2) 0.012(3) 0.016(3) 0.001(2) 0.007(2) 0.000(2) C14 0.019(3) 0.015(3) 0.023(3) 0.000(2) 0.012(2) 0.003(2) C15 0.020(3) 0.026(3) 0.020(3) -0.004(3) 0.005(2) 0.001(3) C16 0.032(3) 0.025(3) 0.018(3) -0.002(3) 0.005(3) 0.001(3) C17 0.035(3) 0.030(3) 0.030(4) -0.002(3) 0.024(3) 0.008(3) C18 0.016(3) 0.023(3) 0.022(3) -0.004(2) 0.011(2) 0.002(2) C19 0.015(2) 0.015(3) 0.013(3) 0.000(2) 0.011(2) 0.000(2) C20 0.017(3) 0.022(3) 0.024(3) 0.000(2) 0.014(2) -0.002(2) C21 0.023(3) 0.037(4) 0.022(3) -0.002(3) 0.011(3) -0.010(3) C22 0.031(3) 0.034(4) 0.030(4) -0.014(3) 0.017(3) -0.025(3) C23 0.029(3) 0.025(3) 0.026(3) -0.004(3) 0.019(3) -0.006(3) C24 0.017(3) 0.029(3) 0.017(3) -0.008(2) 0.011(2) -0.005(2) C25 0.010(2) 0.022(3) 0.011(3) 0.003(2) 0.004(2) 0.006(2) C26 0.021(3) 0.020(3) 0.031(3) 0.000(3) 0.021(3) -0.003(2) C27 0.023(3) 0.021(3) 0.038(4) -0.006(3) 0.018(3) -0.003(2) C28 0.019(3) 0.020(3) 0.028(3) 0.005(3) 0.008(3) -0.004(2) C29 0.015(3) 0.030(3) 0.021(3) 0.007(3) 0.009(2) -0.001(2) C30 0.017(3) 0.019(3) 0.019(3) 0.000(2) 0.004(2) -0.001(2) C31 0.018(3) 0.022(3) 0.018(3) 0.004(2) 0.003(2) -0.003(2) C32 0.015(3) 0.016(3) 0.019(3) -0.001(2) 0.009(2) -0.001(2) C33 0.017(3) 0.024(3) 0.024(3) 0.005(2) 0.014(2) 0.002(2) C34 0.010(2) 0.014(3) 0.025(3) 0.003(2) 0.009(2) 0.002(2) C35 0.022(3) 0.038(4) 0.034(4) 0.006(3) 0.010(3) -0.014(3) C36 0.030(3) 0.020(3) 0.027(4) 0.000(3) 0.004(3) -0.003(3) C37 0.023(3) 0.026(3) 0.023(3) 0.005(2) 0.010(2) 0.005(2) C38 0.023(3) 0.027(3) 0.037(4) 0.001(3) 0.017(3) 0.001(3) C39 0.014(3) 0.030(3) 0.042(4) 0.002(3) 0.015(3) 0.006(2) C40 0.024(3) 0.037(4) 0.030(4) 0.001(3) 0.016(3) 0.008(3) C41 0.030(3) 0.025(3) 0.034(4) 0.010(3) 0.016(3) 0.002(3) C42 0.017(3) 0.025(3) 0.032(3) -0.004(2) 0.011(2) -0.007(2) C43 0.014(2) 0.018(3) 0.019(3) -0.001(2) 0.007(2) 0.000(2) C44 0.015(2) 0.016(3) 0.013(3) 0.002(2) 0.005(2) 0.001(2) C45 0.014(2) 0.017(3) 0.024(3) 0.000(2) 0.011(2) -0.001(2) C46 0.026(3) 0.022(3) 0.023(3) -0.004(2) 0.016(3) -0.005(3) C47 0.017(3) 0.027(3) 0.014(3) -0.004(2) 0.003(2) -0.004(2) C48 0.011(2) 0.023(3) 0.023(3) 0.002(2) 0.009(2) 0.001(2) C49 0.016(3) 0.014(3) 0.017(3) -0.002(2) 0.009(2) -0.002(2) C50 0.011(2) 0.016(3) 0.013(3) -0.001(2) 0.006(2) -0.003(2) C51 0.024(3) 0.011(3) 0.022(3) 0.001(2) 0.013(2) 0.000(2) C52 0.017(3) 0.020(3) 0.030(3) 0.009(2) 0.013(2) 0.006(2) C53 0.007(2) 0.030(3) 0.022(3) 0.002(2) 0.006(2) -0.002(2) C54 0.024(3) 0.014(3) 0.027(3) 0.000(2) 0.017(2) -0.001(2) C55 0.012(2) 0.018(3) 0.012(3) 0.004(2) 0.009(2) 0.001(2) C56 0.018(3) 0.023(3) 0.019(3) -0.002(2) 0.012(2) -0.001(2) C57 0.013(3) 0.031(3) 0.019(3) 0.000(3) 0.006(2) 0.002(3) C58 0.021(3) 0.029(3) 0.021(3) 0.007(2) 0.014(3) 0.011(3) C59 0.028(3) 0.021(3) 0.030(3) 0.005(3) 0.024(3) 0.003(3) C60 0.016(2) 0.022(3) 0.017(3) 0.003(2) 0.013(2) 0.001(2) C61 0.013(2) 0.019(3) 0.008(3) 0.002(2) 0.001(2) 0.002(2) C62 0.020(3) 0.022(3) 0.018(3) -0.002(2) 0.009(2) 0.003(2) C63 0.014(3) 0.028(3) 0.025(3) 0.003(3) 0.004(2) 0.002(2) C64 0.033(3) 0.025(3) 0.014(3) 0.000(2) 0.004(3) -0.003(3) C65 0.027(3) 0.026(3) 0.020(3) 0.007(3) 0.009(3) -0.004(3) C66 0.012(2) 0.019(3) 0.024(3) 0.002(2) 0.005(2) 0.000(2) C67 0.012(2) 0.022(3) 0.016(3) -0.003(2) 0.011(2) -0.002(2) C68 0.021(3) 0.014(3) 0.026(3) -0.004(2) 0.016(3) -0.005(2) C69 0.018(3) 0.027(3) 0.029(3) 0.005(3) 0.015(3) 0.005(3) C70 0.022(3) 0.021(3) 0.037(4) 0.000(3) 0.020(3) 0.001(2) C71 0.021(3) 0.028(3) 0.033(3) -0.013(3) 0.020(3) -0.008(3) C72 0.013(3) 0.024(3) 0.027(3) 0.000(2) 0.014(2) 0.001(2) C73 0.016(3) 0.021(3) 0.028(3) 0.001(3) 0.012(2) -0.004(2) C74 0.017(3) 0.021(3) 0.028(3) 0.000(3) 0.015(2) -0.001(2) C75 0.019(3) 0.019(3) 0.024(3) -0.006(2) 0.008(2) 0.001(2) C76 0.014(2) 0.022(3) 0.018(3) 0.001(2) 0.007(2) 0.002(2) C77 0.034(3) 0.027(3) 0.034(4) -0.006(3) 0.019(3) 0.003(3) C78 0.026(3) 0.024(3) 0.035(3) 0.002(3) 0.017(3) 0.006(3) C79 0.016(3) 0.031(3) 0.027(3) -0.006(3) 0.008(2) -0.007(2) C80 0.026(3) 0.034(4) 0.030(3) -0.001(3) 0.016(3) -0.005(3) C81 0.026(3) 0.036(4) 0.043(4) -0.011(3) 0.015(3) 0.011(3) C82 0.032(3) 0.022(3) 0.029(4) 0.003(3) 0.008(3) 0.002(3) C83 0.017(3) 0.028(3) 0.027(3) -0.001(3) 0.010(2) -0.001(2) C84 0.023(3) 0.033(3) 0.023(3) -0.005(3) 0.008(2) -0.001(3) N1S2 0.056(3) 0.041(3) 0.058(4) -0.008(3) 0.039(3) -0.018(3) C1S2 0.037(3) 0.038(4) 0.042(4) -0.010(3) 0.023(3) -0.008(3) C2S2 0.037(3) 0.033(4) 0.035(4) 0.000(3) 0.030(3) -0.003(3) N1S1 0.044(3) 0.040(3) 0.046(3) 0.002(3) 0.021(3) -0.004(3) C1S1 0.026(3) 0.041(4) 0.037(4) -0.006(3) 0.014(3) -0.006(3) C2S1 0.024(3) 0.032(4) 0.025(3) 0.008(3) 0.007(3) -0.001(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Y1 O3 2.233(3) . ? Y1 O2 2.250(3) . ? Y1 O1 2.378(3) . ? Y1 O2N1 2.412(3) . ? Y1 O1N2 2.417(3) . ? Y1 O2N3 2.451(3) . ? Y1 O1N3 2.459(3) . ? Y1 O2N2 2.461(3) . ? Y1 O1N1 2.484(3) . ? Y1 N1N3 2.842(4) . ? Y1 N1N2 2.861(4) . ? Y1 N1N1 2.878(4) . ? Y2 O5 2.214(3) . ? Y2 O4 2.268(3) . ? Y2 O6 2.337(3) . ? Y2 O1N4 2.389(3) . ? Y2 O1N5 2.423(3) . ? Y2 O1N6 2.468(3) . ? Y2 O2N4 2.471(3) . ? Y2 O2N6 2.478(3) . ? Y2 O2N5 2.486(3) . ? Y2 N1N4 2.837(4) . ? Y2 N1N6 2.872(4) . ? Y2 N1N5 2.884(4) . ? P1 O1 1.513(3) . ? P1 N4 1.647(4) . ? P1 C13 1.796(4) . ? P1 C1 1.818(4) . ? P2 O2 1.500(3) . ? P2 C25 1.811(5) . ? P2 C8 1.817(4) . ? P2 C2 1.836(4) . ? P3 O3 1.494(3) . ? P3 N3 1.641(4) . ? P3 C19 1.800(4) . ? P3 C7 1.834(4) . ? P4 O4 1.501(3) . ? P4 N2 1.640(4) . ? P4 C55 1.808(4) . ? P4 C43 1.844(5) . ? P5 O5 1.499(3) . ? P5 C67 1.793(5) . ? P5 C44 1.809(4) . ? P5 C50 1.832(4) . ? P6 O6 1.513(3) . ? P6 N1 1.642(4) . ? P6 C61 1.799(4) . ? P6 C49 1.835(4) . ? O1N1 N1N1 1.265(5) . ? O2N1 N1N1 1.282(5) . ? O3N1 N1N1 1.221(4) . ? O1N2 N1N2 1.258(4) . ? O2N2 N1N2 1.289(4) . ? O3N2 N1N2 1.226(4) . ? O2N3 N1N3 1.255(4) . ? O1N3 N1N3 1.284(4) . ? O3N3 N1N3 1.239(4) . ? O1N4 N1N4 1.265(4) . ? O2N4 N1N4 1.289(4) . ? O3N4 N1N4 1.236(4) . ? O1N5 N1N5 1.283(5) . ? O2N5 N1N5 1.266(5) . ? O3N5 N1N5 1.226(4) . ? O1N6 N1N6 1.259(5) . ? O2N6 N1N6 1.279(4) . ? O3N6 N1N6 1.235(4) . ? N1 C76 1.499(5) . ? N1 C75 1.501(5) . ? N2 C73 1.493(5) . ? N2 C74 1.502(5) . ? N3 C34 1.484(5) . ? N3 C33 1.501(5) . ? N4 C32 1.497(5) . ? N4 C31 1.500(5) . ? C1 C2 1.391(6) . ? C1 C6 1.406(5) . ? C2 C3 1.407(5) . ? C3 C4 1.383(5) . ? C3 H3 0.95 . ? C4 C5 1.365(6) . ? C4 H4 0.95 . ? C5 C6 1.391(5) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C12 1.386(5) . ? C7 C8 1.443(5) . ? C8 C9 1.400(6) . ? C9 C10 1.386(5) . ? C9 H9 0.95 . ? C10 C11 1.388(5) . ? C10 H10 0.95 . ? C11 C12 1.384(6) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C18 1.395(6) . ? C13 C14 1.398(5) . ? C14 C15 1.382(6) . ? C14 H14 0.95 . ? C15 C16 1.378(6) . ? C15 H15 0.95 . ? C16 C17 1.392(6) . ? C16 H16 0.95 . ? C17 C18 1.371(6) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? C19 C20 1.390(5) . ? C19 C24 1.395(6) . ? C20 C21 1.384(6) . ? C20 H20 0.95 . ? C21 C22 1.389(6) . ? C21 H21 0.95 . ? C22 C23 1.381(6) . ? C22 H22 0.95 . ? C23 C24 1.375(6) . ? C23 H23 0.95 . ? C24 H24 0.95 . ? C25 C26 1.373(6) . ? C25 C30 1.388(6) . ? C26 C27 1.379(6) . ? C26 H26 0.95 . ? C27 C28 1.390(6) . ? C27 H27 0.95 . ? C28 C29 1.367(6) . ? C28 H28 0.95 . ? C29 C30 1.385(6) . ? C29 H29 0.95 . ? C30 H30 0.95 . ? C31 C35 1.526(6) . ? C31 C36 1.531(6) . ? C31 H31 1 . ? C32 C37 1.528(6) . ? C32 C38 1.536(5) . ? C32 H32 1 . ? C33 C40 1.523(6) . ? C33 C39 1.538(5) . ? C33 H33 1 . ? C34 C41 1.519(6) . ? C34 C42 1.535(5) . ? C34 H34 1 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 C48 1.379(5) . ? C43 C44 1.419(5) . ? C44 C45 1.394(6) . ? C45 C46 1.372(6) . ? C45 H45 0.95 . ? C46 C47 1.377(5) . ? C46 H46 0.95 . ? C47 C48 1.394(6) . ? C47 H47 0.95 . ? C48 H48 0.95 . ? C49 C50 1.395(6) . ? C49 C54 1.400(5) . ? C50 C51 1.405(5) . ? C51 C52 1.390(5) . ? C51 H51 0.95 . ? C52 C53 1.356(6) . ? C52 H52 0.95 . ? C53 C54 1.393(6) . ? C53 H53 0.95 . ? C54 H54 0.95 . ? C55 C60 1.388(6) . ? C55 C56 1.403(5) . ? C56 C57 1.383(5) . ? C56 H56 0.95 . ? C57 C58 1.368(6) . ? C57 H57 0.95 . ? C58 C59 1.394(6) . ? C58 H58 0.95 . ? C59 C60 1.382(5) . ? C59 H59 0.95 . ? C60 H60 0.95 . ? C61 C62 1.387(5) . ? C61 C66 1.391(6) . ? C62 C63 1.390(6) . ? C62 H62 0.95 . ? C63 C64 1.382(6) . ? C63 H63 0.95 . ? C64 C65 1.387(6) . ? C64 H64 0.95 . ? C65 C66 1.373(6) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? C67 C68 1.391(6) . ? C67 C72 1.392(6) . ? C68 C69 1.365(6) . ? C68 H68 0.95 . ? C69 C70 1.382(6) . ? C69 H69 0.95 . ? C70 C71 1.386(6) . ? C70 H70 0.95 . ? C71 C72 1.380(6) . ? C71 H71 0.95 . ? C72 H72 0.95 . ? C73 C78 1.523(6) . ? C73 C77 1.523(5) . ? C73 H73 1 . ? C74 C80 1.522(6) . ? C74 C79 1.528(5) . ? C74 H74 1 . ? C75 C82 1.512(6) . ? C75 C81 1.534(5) . ? C75 H75 1 . ? C76 C83 1.523(6) . ? C76 C84 1.532(5) . ? C76 H76 1 . ? C77 H77A 0.98 . ? C77 H77B 0.98 . ? C77 H77C 0.98 . ? C78 H78A 0.98 . ? C78 H78B 0.98 . ? C78 H78C 0.98 . ? C79 H79A 0.98 . ? C79 H79B 0.98 . ? C79 H79C 0.98 . ? C80 H80A 0.98 . ? C80 H80B 0.98 . ? C80 H80C 0.98 . ? C81 H81A 0.98 . ? C81 H81B 0.98 . ? C81 H81C 0.98 . ? C82 H82A 0.98 . ? C82 H82B 0.98 . ? C82 H82C 0.98 . ? C83 H83A 0.98 . ? C83 H83B 0.98 . ? C83 H83C 0.98 . ? C84 H84A 0.98 . ? C84 H84B 0.98 . ? C84 H84C 0.98 . ? N1S2 C2S2 1.128(6) . ? C1S2 C2S2 1.454(6) . ? C1S2 H1S2 0.98 . ? C1S2 H2S2 0.98 . ? C1S2 H3S2 0.98 . ? N1S1 C2S1 1.131(6) . ? C1S1 C2S1 1.449(6) . ? C1S1 H1S1 0.98 . ? C1S1 H2S1 0.98 . ? C1S1 H3S1 0.98 . ? 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 O3 Y1 O2 76.08(9) . . ? O3 Y1 O1 80.81(9) . . ? O2 Y1 O1 77.81(10) . . ? O3 Y1 O2N1 88.08(10) . . ? O2 Y1 O2N1 125.52(11) . . ? O1 Y1 O2N1 150.89(10) . . ? O3 Y1 O1N2 77.13(10) . . ? O2 Y1 O1N2 146.20(10) . . ? O1 Y1 O1N2 77.91(10) . . ? O2N1 Y1 O1N2 73.39(10) . . ? O3 Y1 O2N3 144.72(10) . . ? O2 Y1 O2N3 75.83(10) . . ? O1 Y1 O2N3 72.75(9) . . ? O2N1 Y1 O2N3 125.89(10) . . ? O1N2 Y1 O2N3 118.21(10) . . ? O3 Y1 O1N3 142.64(10) . . ? O2 Y1 O1N3 83.09(10) . . ? O1 Y1 O1N3 124.74(10) . . ? O2N1 Y1 O1N3 79.19(10) . . ? O1N2 Y1 O1N3 130.37(10) . . ? O2N3 Y1 O1N3 52.32(10) . . ? O3 Y1 O2N2 128.37(10) . . ? O2 Y1 O2N2 154.23(9) . . ? O1 Y1 O2N2 96.61(10) . . ? O2N1 Y1 O2N2 69.56(10) . . ? O1N2 Y1 O2N2 52.38(9) . . ? O2N3 Y1 O2N2 78.48(10) . . ? O1N3 Y1 O2N2 79.61(10) . . ? O3 Y1 O1N1 76.48(10) . . ? O2 Y1 O1N1 73.42(10) . . ? O1 Y1 O1N1 146.77(10) . . ? O2N1 Y1 O1N1 52.15(10) . . ? O1N2 Y1 O1N1 119.30(10) . . ? O2N3 Y1 O1N1 114.82(10) . . ? O1N3 Y1 O1N1 67.93(10) . . ? O2N2 Y1 O1N1 116.50(10) . . ? O3 Y1 N1N3 149.83(11) . . ? O2 Y1 N1N3 74.23(10) . . ? O1 Y1 N1N3 97.96(11) . . ? O2N1 Y1 N1N3 104.87(11) . . ? O1N2 Y1 N1N3 132.42(11) . . ? O2N3 Y1 N1N3 26.11(10) . . ? O1N3 Y1 N1N3 26.79(10) . . ? O2N2 Y1 N1N3 81.79(10) . . ? O1N1 Y1 N1N3 89.98(11) . . ? O3 Y1 N1N2 101.93(10) . . ? O2 Y1 N1N2 166.79(11) . . ? O1 Y1 N1N2 88.98(10) . . ? O2N1 Y1 N1N2 67.01(11) . . ? O1N2 Y1 N1N2 25.86(9) . . ? O2N3 Y1 N1N2 100.54(10) . . ? O1N3 Y1 N1N2 104.95(11) . . ? O2N2 Y1 N1N2 26.70(9) . . ? O1N1 Y1 N1N2 119.14(10) . . ? N1N3 Y1 N1N2 108.20(11) . . ? O3 Y1 N1N1 82.40(10) . . ? O2 Y1 N1N1 99.40(12) . . ? O1 Y1 N1N1 163.16(10) . . ? O2N1 Y1 N1N1 26.21(10) . . ? O1N2 Y1 N1N1 97.08(11) . . ? O2N3 Y1 N1N1 123.04(11) . . ? O1N3 Y1 N1N1 70.71(10) . . ? O2N2 Y1 N1N1 92.77(11) . . ? O1N1 Y1 N1N1 25.98(10) . . ? N1N3 Y1 N1N1 97.20(11) . . ? N1N2 Y1 N1N1 93.22(11) . . ? O5 Y2 O4 76.52(10) . . ? O5 Y2 O6 76.92(10) . . ? O4 Y2 O6 80.49(10) . . ? O5 Y2 O1N4 144.99(10) . . ? O4 Y2 O1N4 75.58(10) . . ? O6 Y2 O1N4 77.99(10) . . ? O5 Y2 O1N5 125.74(11) . . ? O4 Y2 O1N5 88.87(10) . . ? O6 Y2 O1N5 152.04(10) . . ? O1N4 Y2 O1N5 74.32(10) . . ? O5 Y2 O1N6 75.66(10) . . ? O4 Y2 O1N6 144.84(10) . . ? O6 Y2 O1N6 72.62(10) . . ? O1N4 Y2 O1N6 118.93(10) . . ? O1N5 Y2 O1N6 125.04(10) . . ? O5 Y2 O2N4 154.09(9) . . ? O4 Y2 O2N4 127.55(10) . . ? O6 Y2 O2N4 96.20(10) . . ? O1N4 Y2 O2N4 52.92(9) . . ? O1N5 Y2 O2N4 70.02(10) . . ? O1N6 Y2 O2N4 78.44(10) . . ? O5 Y2 O2N6 83.61(10) . . ? O4 Y2 O2N6 143.85(11) . . ? O6 Y2 O2N6 124.08(10) . . ? O1N4 Y2 O2N6 131.03(10) . . ? O1N5 Y2 O2N6 78.59(10) . . ? O1N6 Y2 O2N6 51.77(10) . . ? O2N4 Y2 O2N6 79.76(10) . . ? O5 Y2 O2N5 73.71(10) . . ? O4 Y2 O2N5 77.73(10) . . ? O6 Y2 O2N5 146.70(10) . . ? O1N4 Y2 O2N5 119.71(10) . . ? O1N5 Y2 O2N5 52.08(10) . . ? O1N6 Y2 O2N5 113.98(10) . . ? O2N4 Y2 O2N5 117.05(10) . . ? O2N6 Y2 O2N5 67.77(10) . . ? O5 Y2 N1N4 166.50(11) . . ? O4 Y2 N1N4 100.67(10) . . ? O6 Y2 N1N4 89.60(11) . . ? O1N4 Y2 N1N4 26.27(9) . . ? O1N5 Y2 N1N4 66.91(11) . . ? O1N6 Y2 N1N4 101.36(10) . . ? O2N4 Y2 N1N4 27.00(9) . . ? O2N6 Y2 N1N4 105.09(11) . . ? O2N5 Y2 N1N4 118.94(10) . . ? O5 Y2 N1N6 74.82(10) . . ? O4 Y2 N1N6 150.90(11) . . ? O6 Y2 N1N6 97.71(11) . . ? O1N4 Y2 N1N6 132.81(11) . . ? O1N5 Y2 N1N6 103.85(11) . . ? O1N6 Y2 N1N6 25.89(10) . . ? O2N4 Y2 N1N6 81.55(10) . . ? O2N6 Y2 N1N6 26.37(10) . . ? O2N5 Y2 N1N6 89.49(11) . . ? N1N4 Y2 N1N6 108.39(11) . . ? O5 Y2 N1N5 99.63(12) . . ? O4 Y2 N1N5 83.20(10) . . ? O6 Y2 N1N5 163.69(10) . . ? O1N4 Y2 N1N5 97.63(11) . . ? O1N5 Y2 N1N5 26.17(10) . . ? O1N6 Y2 N1N5 122.39(11) . . ? O2N4 Y2 N1N5 93.44(11) . . ? O2N6 Y2 N1N5 70.62(10) . . ? O2N5 Y2 N1N5 25.92(10) . . ? N1N4 Y2 N1N5 93.08(12) . . ? N1N6 Y2 N1N5 96.70(12) . . ? O1 P1 N4 117.98(18) . . ? O1 P1 C13 110.89(18) . . ? N4 P1 C13 107.7(2) . . ? O1 P1 C1 108.80(19) . . ? N4 P1 C1 105.53(19) . . ? C13 P1 C1 105.1(2) . . ? O2 P2 C25 106.54(19) . . ? O2 P2 C8 117.44(18) . . ? C25 P2 C8 106.09(19) . . ? O2 P2 C2 113.70(18) . . ? C25 P2 C2 103.7(2) . . ? C8 P2 C2 108.2(2) . . ? O3 P3 N3 117.29(18) . . ? O3 P3 C19 106.67(19) . . ? N3 P3 C19 105.19(19) . . ? O3 P3 C7 113.31(18) . . ? N3 P3 C7 108.9(2) . . ? C19 P3 C7 104.3(2) . . ? O4 P4 N2 118.30(18) . . ? O4 P4 C55 106.69(19) . . ? N2 P4 C55 107.02(19) . . ? O4 P4 C43 113.34(18) . . ? N2 P4 C43 105.5(2) . . ? C55 P4 C43 105.1(2) . . ? O5 P5 C67 104.59(19) . . ? O5 P5 C44 118.82(19) . . ? C67 P5 C44 106.2(2) . . ? O5 P5 C50 112.64(19) . . ? C67 P5 C50 108.0(2) . . ? C44 P5 C50 106.1(2) . . ? O6 P6 N1 117.75(19) . . ? O6 P6 C61 110.06(18) . . ? N1 P6 C61 107.9(2) . . ? O6 P6 C49 109.20(19) . . ? N1 P6 C49 105.50(19) . . ? C61 P6 C49 105.7(2) . . ? P1 O1 Y1 152.25(16) . . ? P2 O2 Y1 133.82(17) . . ? P3 O3 Y1 158.24(17) . . ? P4 O4 Y2 155.57(17) . . ? P5 O5 Y2 138.28(18) . . ? P6 O6 Y2 154.37(16) . . ? N1N1 O1N1 Y1 94.6(3) . . ? N1N1 O2N1 Y1 97.6(3) . . ? N1N2 O1N2 Y1 97.2(2) . . ? N1N2 O2N2 Y1 94.2(2) . . ? N1N3 O2N3 Y1 94.6(2) . . ? N1N3 O1N3 Y1 93.5(2) . . ? N1N4 O1N4 Y2 97.0(2) . . ? N1N4 O2N4 Y2 92.6(2) . . ? N1N5 O1N5 Y2 97.4(3) . . ? N1N5 O2N5 Y2 94.9(3) . . ? N1N6 O1N6 Y2 95.3(3) . . ? N1N6 O2N6 Y2 94.3(3) . . ? O3N1 N1N1 O1N1 122.7(4) . . ? O3N1 N1N1 O2N1 121.9(4) . . ? O1N1 N1N1 O2N1 115.4(4) . . ? O3N1 N1N1 Y1 176.9(3) . . ? O1N1 N1N1 Y1 59.4(2) . . ? O2N1 N1N1 Y1 56.2(2) . . ? O3N2 N1N2 O1N2 123.5(4) . . ? O3N2 N1N2 O2N2 121.1(4) . . ? O1N2 N1N2 O2N2 115.4(4) . . ? O3N2 N1N2 Y1 170.5(3) . . ? O1N2 N1N2 Y1 57.0(2) . . ? O2N2 N1N2 Y1 59.1(2) . . ? O3N3 N1N3 O2N3 122.8(4) . . ? O3N3 N1N3 O1N3 120.2(4) . . ? O2N3 N1N3 O1N3 117.0(4) . . ? O3N3 N1N3 Y1 166.6(3) . . ? O2N3 N1N3 Y1 59.2(2) . . ? O1N3 N1N3 Y1 59.7(2) . . ? O3N4 N1N4 O1N4 122.8(4) . . ? O3N4 N1N4 O2N4 121.2(4) . . ? O1N4 N1N4 O2N4 116.0(4) . . ? O3N4 N1N4 Y2 169.1(3) . . ? O1N4 N1N4 Y2 56.7(2) . . ? O2N4 N1N4 Y2 60.4(2) . . ? O3N5 N1N5 O2N5 123.0(4) . . ? O3N5 N1N5 O1N5 121.5(4) . . ? O2N5 N1N5 O1N5 115.5(4) . . ? O3N5 N1N5 Y2 177.1(3) . . ? O2N5 N1N5 Y2 59.2(2) . . ? O1N5 N1N5 Y2 56.4(2) . . ? O3N6 N1N6 O1N6 122.7(4) . . ? O3N6 N1N6 O2N6 120.8(4) . . ? O1N6 N1N6 O2N6 116.5(4) . . ? O3N6 N1N6 Y2 167.2(3) . . ? O1N6 N1N6 Y2 58.8(2) . . ? O2N6 N1N6 Y2 59.4(2) . . ? C76 N1 C75 114.0(3) . . ? C76 N1 P6 117.4(3) . . ? C75 N1 P6 124.1(3) . . ? C73 N2 C74 121.5(4) . . ? C73 N2 P4 119.5(3) . . ? C74 N2 P4 116.9(3) . . ? C34 N3 C33 114.3(3) . . ? C34 N3 P3 127.0(3) . . ? C33 N3 P3 114.3(3) . . ? C32 N4 C31 113.6(3) . . ? C32 N4 P1 118.0(3) . . ? C31 N4 P1 124.1(3) . . ? C2 C1 C6 119.1(4) . . ? C2 C1 P1 124.4(3) . . ? C6 C1 P1 116.5(3) . . ? C1 C2 C3 118.5(4) . . ? C1 C2 P2 126.8(3) . . ? C3 C2 P2 114.6(3) . . ? C4 C3 C2 121.6(4) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.6(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.6(4) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C12 C7 C8 117.8(4) . . ? C12 C7 P3 112.8(3) . . ? C8 C7 P3 128.5(3) . . ? C9 C8 C7 117.2(4) . . ? C9 C8 P2 112.1(3) . . ? C7 C8 P2 129.8(3) . . ? C10 C9 C8 123.0(4) . . ? C10 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? C9 C10 C11 119.6(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 118.4(4) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? C11 C12 C7 123.9(4) . . ? C11 C12 H12 118 . . ? C7 C12 H12 118 . . ? C18 C13 C14 117.8(4) . . ? C18 C13 P1 121.9(3) . . ? C14 C13 P1 120.2(4) . . ? C15 C14 C13 121.1(4) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 120.8(4) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 118.2(5) . . ? C15 C16 H16 120.9 . . ? C17 C16 H16 120.9 . . ? C18 C17 C16 121.6(5) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C13 120.5(4) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C20 C19 C24 118.8(4) . . ? C20 C19 P3 123.7(4) . . ? C24 C19 P3 117.5(3) . . ? C21 C20 C19 120.6(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 119.6(4) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.3(5) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 119.9(5) . . ? C24 C23 H23 120 . . ? C22 C23 H23 120 . . ? C23 C24 C19 120.8(4) . . ? C23 C24 H24 119.6 . . ? C19 C24 H24 119.6 . . ? C26 C25 C30 118.4(4) . . ? C26 C25 P2 117.5(4) . . ? C30 C25 P2 123.6(4) . . ? C25 C26 C27 121.0(5) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C28 120.2(5) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 119.2(5) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C30 120.3(5) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C25 120.8(4) . . ? C29 C30 H30 119.6 . . ? C25 C30 H30 119.6 . . ? N4 C31 C35 113.6(4) . . ? N4 C31 C36 113.2(4) . . ? C35 C31 C36 111.0(4) . . ? N4 C31 H31 106.1 . . ? C35 C31 H31 106.1 . . ? C36 C31 H31 106.1 . . ? N4 C32 C37 112.9(3) . . ? N4 C32 C38 112.2(4) . . ? C37 C32 C38 109.1(4) . . ? N4 C32 H32 107.4 . . ? C37 C32 H32 107.4 . . ? C38 C32 H32 107.4 . . ? N3 C33 C40 112.9(4) . . ? N3 C33 C39 110.8(4) . . ? C40 C33 C39 111.6(4) . . ? N3 C33 H33 107.1 . . ? C40 C33 H33 107.1 . . ? C39 C33 H33 107.1 . . ? N3 C34 C41 113.2(4) . . ? N3 C34 C42 113.7(4) . . ? C41 C34 C42 111.6(4) . . ? N3 C34 H34 105.8 . . ? C41 C34 H34 105.8 . . ? C42 C34 H34 105.8 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C32 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C33 C39 H39A 109.5 . . ? C33 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C33 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C33 C40 H40A 109.5 . . ? C33 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C33 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C34 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C34 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C34 C42 H42A 109.5 . . ? C34 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C34 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 C44 118.1(4) . . ? C48 C43 P4 113.8(3) . . ? C44 C43 P4 128.0(3) . . ? C45 C44 C43 117.9(4) . . ? C45 C44 P5 112.0(3) . . ? C43 C44 P5 129.2(4) . . ? C46 C45 C44 122.9(4) . . ? C46 C45 H45 118.5 . . ? C44 C45 H45 118.5 . . ? C45 C46 C47 119.3(4) . . ? C45 C46 H46 120.4 . . ? C47 C46 H46 120.4 . . ? C46 C47 C48 118.9(4) . . ? C46 C47 H47 120.6 . . ? C48 C47 H47 120.6 . . ? C43 C48 C47 122.8(4) . . ? C43 C48 H48 118.6 . . ? C47 C48 H48 118.6 . . ? C50 C49 C54 119.4(4) . . ? C50 C49 P6 124.9(3) . . ? C54 C49 P6 115.8(3) . . ? C49 C50 C51 118.7(4) . . ? C49 C50 P5 126.2(3) . . ? C51 C50 P5 115.1(3) . . ? C52 C51 C50 120.8(4) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C53 C52 C51 120.0(4) . . ? C53 C52 H52 120 . . ? C51 C52 H52 120 . . ? C52 C53 C54 120.5(4) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C53 C54 C49 120.4(4) . . ? C53 C54 H54 119.8 . . ? C49 C54 H54 119.8 . . ? C60 C55 C56 118.6(4) . . ? C60 C55 P4 118.6(3) . . ? C56 C55 P4 122.7(4) . . ? C57 C56 C55 120.2(4) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C58 C57 C56 120.2(4) . . ? C58 C57 H57 119.9 . . ? C56 C57 H57 119.9 . . ? C57 C58 C59 120.6(4) . . ? C57 C58 H58 119.7 . . ? C59 C58 H58 119.7 . . ? C60 C59 C58 119.1(4) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.4 . . ? C59 C60 C55 121.1(4) . . ? C59 C60 H60 119.5 . . ? C55 C60 H60 119.5 . . ? C62 C61 C66 118.7(4) . . ? C62 C61 P6 119.6(4) . . ? C66 C61 P6 121.6(3) . . ? C61 C62 C63 119.9(4) . . ? C61 C62 H62 120 . . ? C63 C62 H62 120 . . ? C64 C63 C62 121.1(4) . . ? C64 C63 H63 119.4 . . ? C62 C63 H63 119.4 . . ? C63 C64 C65 118.7(5) . . ? C63 C64 H64 120.7 . . ? C65 C64 H64 120.7 . . ? C66 C65 C64 120.5(5) . . ? C66 C65 H65 119.7 . . ? C64 C65 H65 119.7 . . ? C65 C66 C61 121.1(4) . . ? C65 C66 H66 119.5 . . ? C61 C66 H66 119.4 . . ? C68 C67 C72 118.4(4) . . ? C68 C67 P5 116.1(3) . . ? C72 C67 P5 125.2(4) . . ? C69 C68 C67 120.8(5) . . ? C69 C68 H68 119.6 . . ? C67 C68 H68 119.6 . . ? C68 C69 C70 121.1(5) . . ? C68 C69 H69 119.4 . . ? C70 C69 H69 119.4 . . ? C69 C70 C71 118.4(5) . . ? C69 C70 H70 120.8 . . ? C71 C70 H70 120.8 . . ? C72 C71 C70 120.9(5) . . ? C72 C71 H71 119.5 . . ? C70 C71 H71 119.5 . . ? C71 C72 C67 120.1(4) . . ? C71 C72 H72 119.9 . . ? C67 C72 H72 119.9 . . ? N2 C73 C78 115.1(4) . . ? N2 C73 C77 113.3(4) . . ? C78 C73 C77 111.2(4) . . ? N2 C73 H73 105.4 . . ? C78 C73 H73 105.4 . . ? C77 C73 H73 105.4 . . ? N2 C74 C80 115.2(3) . . ? N2 C74 C79 112.8(4) . . ? C80 C74 C79 111.0(4) . . ? N2 C74 H74 105.6 . . ? C80 C74 H74 105.6 . . ? C79 C74 H74 105.6 . . ? N1 C75 C82 114.2(4) . . ? N1 C75 C81 113.5(4) . . ? C82 C75 C81 111.5(4) . . ? N1 C75 H75 105.6 . . ? C82 C75 H75 105.6 . . ? C81 C75 H75 105.6 . . ? N1 C76 C83 112.5(4) . . ? N1 C76 C84 110.7(4) . . ? C83 C76 C84 110.3(4) . . ? N1 C76 H76 107.7 . . ? C83 C76 H76 107.7 . . ? C84 C76 H76 107.7 . . ? C73 C77 H77A 109.5 . . ? C73 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C73 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C73 C78 H78A 109.5 . . ? C73 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C73 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C74 C79 H79A 109.5 . . ? C74 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C74 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C74 C80 H80A 109.5 . . ? C74 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C74 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C75 C81 H81A 109.5 . . ? C75 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C75 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C75 C82 H82A 109.5 . . ? C75 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C75 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C76 C83 H83A 109.5 . . ? C76 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C76 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C76 C84 H84A 109.5 . . ? C76 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C76 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C2S2 C1S2 H1S2 109.5 . . ? C2S2 C1S2 H2S2 109.5 . . ? H1S2 C1S2 H2S2 109.5 . . ? C2S2 C1S2 H3S2 109.5 . . ? H1S2 C1S2 H3S2 109.5 . . ? H2S2 C1S2 H3S2 109.5 . . ? N1S2 C2S2 C1S2 178.7(6) . . ? C2S1 C1S1 H1S1 109.5 . . ? C2S1 C1S1 H2S1 109.5 . . ? H1S1 C1S1 H2S1 109.5 . . ? C2S1 C1S1 H3S1 109.5 . . ? H1S1 C1S1 H3S1 109.5 . . ? H2S1 C1S1 H3S1 109.5 . . ? N1S1 C2S1 C1S1 179.4(8) . . ?