# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1991 # Syntheses, structures and multinuclear NMR (^45^Sc, ^89^Y, ^31^P) # studies of Ph~3~PO, Ph~2~MePO and Me~3~PO complexes of scandium # and yttrium nitrates # L. Deakin, W. Levason, M. C. Popham, G. Reid and M. Webster # Department of Chemistry, University of Southampton, Southampton, UK SO17 1BJ # J. Chem. Soc., Dalton Trans. Paper reference no. B001669L ############################################################################## ### CIF submission form for molecular structure report ### ### Version: 7 October 1991 ### ############################################################################## #============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof W Levason' _publ_contact_author_address ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; _publ_contact_author_phone '023 80 593792' _publ_contact_author_fax '023 80 593781' _publ_contact_author_email 'wxl@soton.ac.uk' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; Please note that this file contains seven CIFs edited into one file and it accompanies a paper submitted to J. Chem. Soc., Dalton Trans. (ref. B001669L). ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Syntheses, structures and multinuclear NMR (^45^Sc, ^89^Y, ^31^P) studies of Ph~3~PO, Ph~2~MePO and Me~3~PO complexes of scandium and yttrium nitrates ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Deakin, Lucy' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Levason, William' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Popham, Michael C.' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Reid, Gillian' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Webster, Michael' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; #============================================================================== data_Ascpo_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(nitrato-O,O')bis(triphenylphosphineoxide)scandium(III) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 N3 O11 P2 Sc' _chemical_formula_weight 787.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sc' 'Sc' 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'Pn' _symmetry_Int_Tables_number 7 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 10.249(5) _cell_length_b 10.628(4) _cell_length_c 17.289(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.76(3) _cell_angle_gamma 90.00 _cell_volume 1850.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? # 0.9055 _exptl_absorpt_correction_T_max ? # 0.9659 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2706 _diffrn_reflns_av_R_equivalents 0.2002 _diffrn_reflns_av_sigmaI/netI 0.1177 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2704 _reflns_number_gt 1707 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+2.4000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(9) _refine_ls_number_reflns 2704 _refine_ls_number_parameters 284 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1546 _refine_ls_wR_factor_gt 0.1268 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc Sc 0.34435(18) 0.69170(18) 0.34083(11) 0.0281(5) Uani 1 d . . . P1 P 0.5226(3) 0.7599(3) 0.18945(16) 0.0304(7) Uani 1 d . . . P2 P 0.5366(3) 0.9038(3) 0.47554(16) 0.0300(7) Uani 1 d . . . O1 O 0.4413(8) 0.7515(7) 0.2527(4) 0.0392(19) Uani 1 d . . . O2 O 0.4532(7) 0.8140(7) 0.4188(4) 0.0336(18) Uani 1 d . . . O3 O 0.0252(8) 0.8159(9) 0.2042(5) 0.066(3) Uani 1 d . . . O4 O 0.2076(7) 0.8548(7) 0.2873(4) 0.0381(19) Uani 1 d . . . O5 O 0.1634(8) 0.6656(7) 0.2509(4) 0.045(2) Uani 1 d . . . O6 O 0.1531(10) 0.6082(10) 0.5111(6) 0.082(3) Uani 1 d . . . O7 O 0.1856(8) 0.7314(8) 0.4153(5) 0.053(2) Uani 1 d . . . O8 O 0.3047(11) 0.5699(8) 0.4401(6) 0.073(3) Uani 1 d . . . O9 O 0.5337(10) 0.3807(8) 0.3221(6) 0.073(3) Uani 1 d . . . O10 O 0.5243(7) 0.5655(7) 0.3761(4) 0.0387(19) Uani 1 d . . . O11 O 0.3584(8) 0.5015(7) 0.2910(4) 0.046(2) Uani 1 d . . . N1 N 0.1277(10) 0.7803(9) 0.2456(6) 0.042(2) Uiso 1 d . . . N2 N 0.2097(11) 0.6336(10) 0.4577(6) 0.049(3) Uiso 1 d . . . N3 N 0.4745(9) 0.4767(10) 0.3299(6) 0.039(2) Uiso 1 d . . . C1 C 0.5652(10) 0.9207(10) 0.1761(6) 0.031(3) Uiso 1 d . . . C2 C 0.4831(12) 1.0135(11) 0.1954(7) 0.045(3) Uiso 1 d . . . H2 H 0.4060 0.9903 0.2152 0.069(7) Uiso 1 calc R . . C3 C 0.5106(12) 1.1405(11) 0.1866(7) 0.047(3) Uiso 1 d . . . H3 H 0.4533 1.2040 0.1999 0.069(7) Uiso 1 calc R . . C4 C 0.6228(13) 1.1713(13) 0.1582(7) 0.053(3) Uiso 1 d . . . H4 H 0.6428 1.2577 0.1522 0.069(7) Uiso 1 calc R . . C5 C 0.7054(12) 1.0840(11) 0.1386(7) 0.049(3) Uiso 1 d . . . H5 H 0.7818 1.1085 0.1185 0.069(7) Uiso 1 calc R . . C6 C 0.6776(12) 0.9545(11) 0.1482(7) 0.046(3) Uiso 1 d . . . H6 H 0.7361 0.8918 0.1355 0.069(7) Uiso 1 calc R . . C7 C 0.4343(11) 0.6992(10) 0.0964(6) 0.032(3) Uiso 1 d . . . C8 C 0.4353(13) 0.7572(12) 0.0276(7) 0.052(3) Uiso 1 d . . . H8 H 0.4788 0.8360 0.0268 0.069(7) Uiso 1 calc R . . C9 C 0.3729(14) 0.7024(13) -0.0423(8) 0.062(4) Uiso 1 d . . . H9 H 0.3793 0.7416 -0.0909 0.069(7) Uiso 1 calc R . . C10 C 0.3039(13) 0.5955(12) -0.0428(8) 0.053(3) Uiso 1 d . . . H10 H 0.2577 0.5615 -0.0910 0.069(7) Uiso 1 calc R . . C11 C 0.3005(16) 0.5374(16) 0.0245(9) 0.081(5) Uiso 1 d . . . H11 H 0.2552 0.4594 0.0240 0.069(7) Uiso 1 calc R . . C12 C 0.3636(14) 0.5898(13) 0.0971(9) 0.068(4) Uiso 1 d . . . H12 H 0.3571 0.5500 0.1454 0.069(7) Uiso 1 calc R . . C13 C 0.6721(10) 0.6684(10) 0.2146(6) 0.031(3) Uiso 1 d . . . C14 C 0.7071(12) 0.5769(12) 0.1666(8) 0.050(3) Uiso 1 d . . . H14 H 0.6529 0.5611 0.1167 0.069(7) Uiso 1 calc R . . C15 C 0.8207(14) 0.5081(14) 0.1908(8) 0.062(4) Uiso 1 d . . . H15 H 0.8471 0.4474 0.1564 0.069(7) Uiso 1 calc R . . C16 C 0.8957(12) 0.5260(12) 0.2632(7) 0.049(3) Uiso 1 d . . . H16 H 0.9718 0.4749 0.2796 0.069(7) Uiso 1 calc R . . C17 C 0.8648(13) 0.6150(11) 0.3131(8) 0.049(3) Uiso 1 d . . . H17 H 0.9195 0.6274 0.3633 0.069(7) Uiso 1 calc R . . C18 C 0.7513(13) 0.6881(12) 0.2894(7) 0.047(3) Uiso 1 d . . . H18 H 0.7275 0.7507 0.3234 0.069(7) Uiso 1 calc R . . C19 C 0.5682(10) 0.8352(10) 0.5715(6) 0.030(3) Uiso 1 d . . . C20 C 0.5735(11) 0.7063(10) 0.5795(6) 0.034(3) Uiso 1 d . . . H20 H 0.5515 0.6543 0.5342 0.069(7) Uiso 1 calc R . . C21 C 0.6106(12) 0.6526(12) 0.6528(7) 0.045(3) Uiso 1 d . . . H21 H 0.6132 0.5635 0.6574 0.069(7) Uiso 1 calc R . . C22 C 0.6444(12) 0.7260(11) 0.7205(7) 0.047(3) Uiso 1 d . . . H22 H 0.6696 0.6879 0.7708 0.069(7) Uiso 1 calc R . . C23 C 0.6402(12) 0.8531(12) 0.7128(8) 0.048(3) Uiso 1 d . . . H23 H 0.6647 0.9043 0.7582 0.069(7) Uiso 1 calc R . . C24 C 0.6006(11) 0.9102(11) 0.6391(6) 0.037(3) Uiso 1 d . . . H24 H 0.5957 0.9992 0.6350 0.069(7) Uiso 1 calc R . . C25 C 0.6956(11) 0.9334(10) 0.4487(6) 0.034(3) Uiso 1 d . . . C26 C 0.6995(12) 1.0040(11) 0.3821(7) 0.041(3) Uiso 1 d . . . H26 H 0.6210 1.0448 0.3561 0.069(7) Uiso 1 calc R . . C27 C 0.8147(12) 1.0165(12) 0.3528(8) 0.052(3) Uiso 1 d . . . H27 H 0.8177 1.0675 0.3080 0.069(7) Uiso 1 calc R . . C28 C 0.9255(13) 0.9527(12) 0.3903(7) 0.054(3) Uiso 1 d . . . H28 H 1.0051 0.9583 0.3698 0.069(7) Uiso 1 calc R . . C29 C 0.9248(14) 0.8837(12) 0.4542(7) 0.055(4) Uiso 1 d . . . H29 H 1.0033 0.8414 0.4787 0.069(7) Uiso 1 calc R . . C30 C 0.8101(12) 0.8729(11) 0.4853(7) 0.042(3) Uiso 1 d . . . H30 H 0.8101 0.8242 0.5314 0.069(7) Uiso 1 calc R . . C31 C 0.4521(10) 1.0492(10) 0.4763(6) 0.030(2) Uiso 1 d . . . C32 C 0.3147(12) 1.0494(11) 0.4506(6) 0.041(3) Uiso 1 d . . . H32 H 0.2691 0.9738 0.4332 0.069(7) Uiso 1 calc R . . C33 C 0.2447(14) 1.1633(12) 0.4507(7) 0.051(3) Uiso 1 d . . . H33 H 0.1513 1.1639 0.4327 0.069(7) Uiso 1 calc R . . C34 C 0.3067(13) 1.2702(13) 0.4755(7) 0.053(3) Uiso 1 d . . . H34 H 0.2561 1.3452 0.4751 0.069(7) Uiso 1 calc R . . C35 C 0.4416(14) 1.2750(14) 0.5017(8) 0.068(4) Uiso 1 d . . . H35 H 0.4844 1.3519 0.5193 0.069(7) Uiso 1 calc R . . C36 C 0.5163(13) 1.1607(11) 0.5016(7) 0.051(3) Uiso 1 d . . . H36 H 0.6099 1.1614 0.5190 0.069(7) Uiso 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 Sc 0.0288(11) 0.0278(11) 0.0272(10) 0.0008(10) 0.0036(9) -0.0004(10) P1 0.0314(16) 0.0317(16) 0.0289(14) -0.0046(13) 0.0078(13) -0.0049(14) P2 0.0323(16) 0.0285(15) 0.0293(15) -0.0049(13) 0.0058(13) 0.0000(14) O1 0.047(4) 0.036(5) 0.036(5) -0.002(4) 0.011(4) -0.004(4) O2 0.036(5) 0.026(4) 0.037(4) -0.006(3) 0.005(4) -0.006(4) O3 0.033(5) 0.079(7) 0.073(6) 0.030(5) -0.021(5) 0.000(5) O4 0.043(5) 0.031(4) 0.037(4) 0.008(4) 0.001(4) 0.006(4) O5 0.044(5) 0.040(5) 0.047(5) -0.003(4) -0.005(4) -0.002(4) O6 0.096(8) 0.092(8) 0.076(6) 0.032(6) 0.064(6) 0.023(6) O7 0.056(5) 0.052(6) 0.055(5) 0.017(4) 0.022(5) 0.018(5) O8 0.105(8) 0.032(5) 0.096(7) 0.018(5) 0.057(6) 0.016(5) O9 0.075(7) 0.040(5) 0.096(7) -0.028(5) -0.009(6) 0.027(6) O10 0.029(4) 0.037(5) 0.046(4) -0.008(4) -0.005(4) 0.001(4) O11 0.052(5) 0.030(5) 0.049(5) -0.008(4) -0.008(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc O2 2.047(7) . ? Sc O1 2.068(7) . ? Sc O5 2.205(8) . ? Sc O11 2.213(8) . ? Sc O8 2.246(9) . ? Sc O10 2.270(7) . ? Sc O7 2.294(8) . ? Sc O4 2.311(7) . ? P1 O1 1.497(8) . ? P1 C1 1.790(10) . ? P1 C13 1.798(11) . ? P1 C7 1.811(11) . ? P2 O2 1.513(7) . ? P2 C31 1.773(11) . ? P2 C19 1.786(10) . ? P2 C25 1.803(11) . ? O3 N1 1.216(12) . ? O4 N1 1.264(12) . ? O5 N1 1.271(12) . ? O6 N2 1.210(12) . ? O7 N2 1.270(12) . ? O8 N2 1.268(13) . ? O9 N3 1.208(11) . ? O10 N3 1.280(11) . ? O11 N3 1.280(11) . ? C1 C2 1.377(15) . ? C1 C6 1.377(15) . ? C2 C3 1.394(16) . ? C3 C4 1.372(17) . ? C4 C5 1.341(16) . ? C5 C6 1.422(16) . ? C7 C8 1.342(15) . ? C7 C12 1.371(17) . ? C8 C9 1.385(17) . ? C9 C10 1.338(17) . ? C10 C11 1.322(19) . ? C11 C12 1.414(19) . ? C13 C14 1.368(16) . ? C13 C18 1.408(16) . ? C14 C15 1.372(17) . ? C15 C16 1.355(16) . ? C16 C17 1.357(16) . ? C17 C18 1.395(18) . ? C19 C20 1.377(14) . ? C19 C24 1.402(15) . ? C20 C21 1.378(15) . ? C21 C22 1.395(16) . ? C22 C23 1.357(16) . ? C23 C24 1.400(16) . ? C25 C26 1.381(15) . ? C25 C30 1.384(15) . ? C26 C27 1.376(16) . ? C27 C28 1.376(17) . ? C28 C29 1.327(17) . ? C29 C30 1.385(16) . ? C31 C36 1.386(15) . ? C31 C32 1.395(15) . ? C32 C33 1.406(17) . ? C33 C34 1.333(17) . ? C34 C35 1.373(18) . ? C35 C36 1.436(18) . ? 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 O2 Sc O1 90.7(3) . . ? O2 Sc O5 145.9(3) . . ? O1 Sc O5 88.6(3) . . ? O2 Sc O11 140.3(3) . . ? O1 Sc O11 85.3(3) . . ? O5 Sc O11 73.6(3) . . ? O2 Sc O8 91.0(3) . . ? O1 Sc O8 156.9(3) . . ? O5 Sc O8 102.6(4) . . ? O11 Sc O8 78.8(3) . . ? O2 Sc O10 83.3(3) . . ? O1 Sc O10 84.4(3) . . ? O5 Sc O10 130.5(3) . . ? O11 Sc O10 57.1(3) . . ? O8 Sc O10 73.0(3) . . ? O2 Sc O7 82.5(3) . . ? O1 Sc O7 147.7(3) . . ? O5 Sc O7 80.1(3) . . ? O11 Sc O7 119.4(3) . . ? O8 Sc O7 55.2(3) . . ? O10 Sc O7 125.7(3) . . ? O2 Sc O4 90.1(3) . . ? O1 Sc O4 79.2(3) . . ? O5 Sc O4 56.2(3) . . ? O11 Sc O4 127.4(3) . . ? O8 Sc O4 123.7(3) . . ? O10 Sc O4 162.3(3) . . ? O7 Sc O4 69.3(3) . . ? O1 P1 C1 109.5(5) . . ? O1 P1 C13 110.9(5) . . ? C1 P1 C13 109.3(5) . . ? O1 P1 C7 112.0(5) . . ? C1 P1 C7 108.6(5) . . ? C13 P1 C7 106.5(5) . . ? O2 P2 C31 109.6(5) . . ? O2 P2 C19 109.1(5) . . ? C31 P2 C19 110.6(5) . . ? O2 P2 C25 111.9(5) . . ? C31 P2 C25 108.4(5) . . ? C19 P2 C25 107.1(5) . . ? P1 O1 Sc 165.1(5) . . ? P2 O2 Sc 178.5(5) . . ? N1 O4 Sc 92.2(6) . . ? N1 O5 Sc 97.1(6) . . ? N2 O7 Sc 95.2(7) . . ? N2 O8 Sc 97.6(7) . . ? N3 O10 Sc 93.3(6) . . ? N3 O11 Sc 96.0(6) . . ? O3 N1 O4 122.5(10) . . ? O3 N1 O5 123.1(10) . . ? O4 N1 O5 114.4(9) . . ? O6 N2 O8 124.3(11) . . ? O6 N2 O7 123.7(11) . . ? O8 N2 O7 112.0(10) . . ? O9 N3 O11 123.6(10) . . ? O9 N3 O10 122.8(9) . . ? O11 N3 O10 113.6(9) . . ? C2 C1 C6 119.2(10) . . ? C2 C1 P1 118.5(8) . . ? C6 C1 P1 122.3(9) . . ? C1 C2 C3 121.5(11) . . ? C4 C3 C2 118.1(12) . . ? C5 C4 C3 122.4(12) . . ? C4 C5 C6 119.4(12) . . ? C1 C6 C5 119.5(12) . . ? C8 C7 C12 119.2(11) . . ? C8 C7 P1 122.6(9) . . ? C12 C7 P1 118.1(9) . . ? C7 C8 C9 120.1(12) . . ? C10 C9 C8 121.3(13) . . ? C11 C10 C9 119.5(14) . . ? C10 C11 C12 120.9(16) . . ? C7 C12 C11 118.8(14) . . ? C14 C13 C18 119.4(11) . . ? C14 C13 P1 123.1(9) . . ? C18 C13 P1 117.4(8) . . ? C13 C14 C15 119.8(12) . . ? C16 C15 C14 120.6(14) . . ? C15 C16 C17 121.8(13) . . ? C16 C17 C18 118.8(13) . . ? C17 C18 C13 119.6(11) . . ? C20 C19 C24 118.9(10) . . ? C20 C19 P2 119.7(8) . . ? C24 C19 P2 121.1(8) . . ? C19 C20 C21 120.2(10) . . ? C20 C21 C22 121.5(11) . . ? C23 C22 C21 118.4(12) . . ? C22 C23 C24 121.3(12) . . ? C23 C24 C19 119.7(11) . . ? C26 C25 C30 118.6(10) . . ? C26 C25 P2 118.5(9) . . ? C30 C25 P2 122.1(8) . . ? C27 C26 C25 121.3(12) . . ? C26 C27 C28 117.9(12) . . ? C29 C28 C27 122.2(13) . . ? C28 C29 C30 120.4(13) . . ? C25 C30 C29 119.6(11) . . ? C36 C31 C32 119.4(11) . . ? C36 C31 P2 122.9(9) . . ? C32 C31 P2 117.7(9) . . ? C31 C32 C33 119.1(11) . . ? C34 C33 C32 121.4(12) . . ? C33 C34 C35 121.8(14) . . ? C34 C35 C36 118.2(14) . . ? C31 C36 C35 120.1(12) . . ? _diffrn_measured_fraction_theta_max 0.776 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.776 _refine_diff_density_max 0.499 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.085 #===END #===================================================== data_Bwlyppo _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(nitrato-O,O')tris(triphenylphosphineoxide)yttrium(III) dichloromethane solvate ; _chemical_name_common ? _chemical_formula_moiety 'C54 H45 N3 O12 P3 Y, 1.78(C H2 Cl2)' _chemical_formula_sum 'C55.78 H48.56 Cl3.57 N3 O12 P3 Y' _chemical_formula_weight 1261.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 /n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.118(2) _cell_length_b 19.342(3) _cell_length_c 27.244(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.569(16) _cell_angle_gamma 90.00 _cell_volume 5839.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2580 _exptl_absorpt_coefficient_mu 1.306 _exptl_absorpt_correction_type empirical # psi-scan _exptl_absorpt_correction_T_min 0.765 # 0.5910 _exptl_absorpt_correction_T_max 1.000 # 0.8282 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10823 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.1577 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10255 _reflns_number_gt 4523 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+13.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10255 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1926 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.2206 _refine_ls_wR_factor_gt 0.1708 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.077 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.61466(6) 0.24975(4) 0.13218(2) 0.02239(19) Uani 1 d . . . P1 P 0.28125(17) 0.25614(11) 0.11790(7) 0.0288(5) Uani 1 d . . . P2 P 0.62690(17) 0.30144(10) -0.00046(7) 0.0249(5) Uani 1 d . . . P3 P 0.59530(18) 0.29592(10) 0.26460(7) 0.0266(5) Uani 1 d . . . O1 O 0.4141(4) 0.2664(2) 0.11383(18) 0.0294(13) Uani 1 d . . . O2 O 0.6279(4) 0.2848(3) 0.05275(17) 0.0302(13) Uani 1 d . . . O3 O 0.5787(4) 0.2754(3) 0.21149(17) 0.0282(12) Uani 1 d . . . O4 O 0.4859(6) 0.0532(3) 0.1153(2) 0.0563(18) Uani 1 d . . . O5 O 0.5556(5) 0.1467(3) 0.0843(2) 0.0428(15) Uani 1 d . . . O6 O 0.5463(5) 0.1386(3) 0.1619(2) 0.0448(16) Uani 1 d . . . O7 O 0.7410(5) 0.4487(3) 0.1450(2) 0.0462(16) Uani 1 d . . . O8 O 0.7683(4) 0.3369(3) 0.14425(18) 0.0285(12) Uani 1 d . . . O9 O 0.5878(4) 0.3783(3) 0.13506(18) 0.0294(12) Uani 1 d . . . O10 O 0.9511(5) 0.1625(4) 0.1542(2) 0.0590(19) Uani 1 d . . . O11 O 0.7845(5) 0.1974(3) 0.1828(2) 0.0402(14) Uani 1 d . . . O12 O 0.8039(5) 0.2005(3) 0.1050(2) 0.0436(15) Uani 1 d . . . N1 N 0.5280(6) 0.1110(4) 0.1203(3) 0.0397(17) Uani 1 d . . . N2 N 0.6997(6) 0.3895(3) 0.1415(2) 0.0311(16) Uani 1 d . . . N3 N 0.8493(6) 0.1860(4) 0.1476(3) 0.0403(18) Uani 1 d . . . C1 C 0.2116(7) 0.2253(4) 0.0604(3) 0.0325(19) Uiso 1 d . . . C2 C 0.0871(8) 0.2248(5) 0.0495(3) 0.044(2) Uiso 1 d . . . H2 H 0.0356 0.2415 0.0731 0.054(4) Uiso 1 calc R . . C3 C 0.0374(8) 0.2000(5) 0.0039(3) 0.049(2) Uiso 1 d . . . H3 H -0.0475 0.2010 -0.0037 0.054(4) Uiso 1 calc R . . C4 C 0.1101(8) 0.1748(5) -0.0291(3) 0.049(2) Uiso 1 d . . . H4 H 0.0760 0.1576 -0.0598 0.054(4) Uiso 1 calc R . . C5 C 0.2364(9) 0.1736(5) -0.0186(4) 0.054(3) Uiso 1 d . . . H5 H 0.2873 0.1560 -0.0420 0.054(4) Uiso 1 calc R . . C6 C 0.2844(8) 0.1982(5) 0.0254(3) 0.048(2) Uiso 1 d . . . H6 H 0.3693 0.1969 0.0327 0.054(4) Uiso 1 calc R . . C7 C 0.2116(7) 0.3376(4) 0.1315(3) 0.0280(18) Uiso 1 d . . . C8 C 0.0934(7) 0.3418(4) 0.1445(3) 0.036(2) Uiso 1 d . . . H8 H 0.0486 0.3009 0.1492 0.054(4) Uiso 1 calc R . . C9 C 0.0413(7) 0.4062(4) 0.1506(3) 0.0339(19) Uiso 1 d . . . H9 H -0.0397 0.4094 0.1593 0.054(4) Uiso 1 calc R . . C10 C 0.1079(7) 0.4663(5) 0.1441(3) 0.041(2) Uiso 1 d . . . H10 H 0.0715 0.5103 0.1473 0.054(4) Uiso 1 calc R . . C11 C 0.2264(7) 0.4617(5) 0.1329(3) 0.041(2) Uiso 1 d . . . H11 H 0.2726 0.5025 0.1296 0.054(4) Uiso 1 calc R . . C12 C 0.2781(7) 0.3975(4) 0.1263(3) 0.0325(19) Uiso 1 d . . . H12 H 0.3594 0.3945 0.1182 0.054(4) Uiso 1 calc R . . C13 C 0.2537(7) 0.1940(4) 0.1646(3) 0.0284(18) Uiso 1 d . . . C14 C 0.2658(8) 0.2131(5) 0.2137(3) 0.046(2) Uiso 1 d . . . H14 H 0.2727 0.2605 0.2225 0.054(4) Uiso 1 calc R . . C15 C 0.2680(8) 0.1628(5) 0.2500(4) 0.054(3) Uiso 1 d . . . H15 H 0.2799 0.1759 0.2836 0.054(4) Uiso 1 calc R . . C16 C 0.2529(8) 0.0929(5) 0.2376(4) 0.054(3) Uiso 1 d . . . H16 H 0.2528 0.0584 0.2624 0.054(4) Uiso 1 calc R . . C17 C 0.2381(9) 0.0757(6) 0.1883(4) 0.059(3) Uiso 1 d . . . H17 H 0.2274 0.0284 0.1795 0.054(4) Uiso 1 calc R . . C18 C 0.2383(8) 0.1249(5) 0.1512(3) 0.048(2) Uiso 1 d . . . H18 H 0.2281 0.1118 0.1176 0.054(4) Uiso 1 calc R . . C19 C 0.5197(6) 0.3691(4) -0.0173(3) 0.0267(18) Uiso 1 d . . . C20 C 0.4215(6) 0.3743(4) 0.0111(3) 0.0293(18) Uiso 1 d . . . H20 H 0.4129 0.3430 0.0375 0.054(4) Uiso 1 calc R . . C21 C 0.3350(7) 0.4264(4) 0.0005(3) 0.040(2) Uiso 1 d . . . H21 H 0.2661 0.4298 0.0189 0.054(4) Uiso 1 calc R . . C22 C 0.3515(7) 0.4728(4) -0.0372(3) 0.0344(19) Uiso 1 d . . . H22 H 0.2946 0.5088 -0.0438 0.054(4) Uiso 1 calc R . . C23 C 0.4473(7) 0.4677(4) -0.0649(3) 0.037(2) Uiso 1 d . . . H23 H 0.4568 0.4997 -0.0908 0.054(4) Uiso 1 calc R . . C24 C 0.5323(7) 0.4148(4) -0.0551(3) 0.0341(19) Uiso 1 d . . . H24 H 0.5989 0.4107 -0.0747 0.054(4) Uiso 1 calc R . . C25 C 0.5868(7) 0.2275(4) -0.0380(3) 0.0310(19) Uiso 1 d . . . C26 C 0.6319(8) 0.1633(5) -0.0217(3) 0.045(2) Uiso 1 d . . . H26 H 0.6841 0.1593 0.0075 0.054(4) Uiso 1 calc R . . C27 C 0.5977(8) 0.1049(5) -0.0500(3) 0.055(3) Uiso 1 d . . . H27 H 0.6264 0.0607 -0.0393 0.054(4) Uiso 1 calc R . . C28 C 0.5237(8) 0.1100(5) -0.0925(3) 0.050(2) Uiso 1 d . . . H28 H 0.5005 0.0695 -0.1106 0.054(4) Uiso 1 calc R . . C29 C 0.4833(8) 0.1734(5) -0.1090(3) 0.046(2) Uiso 1 d . . . H29 H 0.4343 0.1771 -0.1391 0.054(4) Uiso 1 calc R . . C30 C 0.5141(7) 0.2329(4) -0.0815(3) 0.034(2) Uiso 1 d . . . H30 H 0.4853 0.2769 -0.0927 0.054(4) Uiso 1 calc R . . C31 C 0.7724(7) 0.3314(4) -0.0162(3) 0.0290(18) Uiso 1 d . . . C32 C 0.8082(7) 0.3292(4) -0.0644(3) 0.035(2) Uiso 1 d . . . H32 H 0.7569 0.3084 -0.0898 0.054(4) Uiso 1 calc R . . C33 C 0.9165(8) 0.3568(5) -0.0753(3) 0.044(2) Uiso 1 d . . . H33 H 0.9407 0.3544 -0.1079 0.054(4) Uiso 1 calc R . . C34 C 0.9903(8) 0.3879(5) -0.0387(3) 0.045(2) Uiso 1 d . . . H34 H 1.0636 0.4088 -0.0466 0.054(4) Uiso 1 calc R . . C35 C 0.9590(8) 0.3892(5) 0.0094(3) 0.043(2) Uiso 1 d . . . H35 H 1.0119 0.4091 0.0346 0.054(4) Uiso 1 calc R . . C36 C 0.8495(7) 0.3611(4) 0.0203(3) 0.036(2) Uiso 1 d . . . H36 H 0.8270 0.3623 0.0533 0.054(4) Uiso 1 calc R . . C37 C 0.7078(7) 0.3616(4) 0.2752(3) 0.0263(17) Uiso 1 d . . . C38 C 0.6878(9) 0.4238(5) 0.2984(3) 0.052(2) Uiso 1 d . . . H38 H 0.6112 0.4328 0.3103 0.054(4) Uiso 1 calc R . . C39 C 0.7790(9) 0.4736(6) 0.3045(4) 0.059(3) Uiso 1 d . . . H39 H 0.7646 0.5162 0.3204 0.054(4) Uiso 1 calc R . . C40 C 0.8883(9) 0.4603(5) 0.2876(3) 0.055(3) Uiso 1 d . . . H40 H 0.9501 0.4943 0.2915 0.054(4) Uiso 1 calc R . . C41 C 0.9105(8) 0.4006(5) 0.2656(3) 0.048(2) Uiso 1 d . . . H41 H 0.9878 0.3928 0.2540 0.054(4) Uiso 1 calc R . . C42 C 0.8223(7) 0.3491(5) 0.2591(3) 0.039(2) Uiso 1 d . . . H42 H 0.8398 0.3064 0.2441 0.054(4) Uiso 1 calc R . . C43 C 0.4573(6) 0.3286(4) 0.2851(3) 0.0275(18) Uiso 1 d . . . C44 C 0.4109(7) 0.3096(4) 0.3288(3) 0.036(2) Uiso 1 d . . . H44 H 0.4542 0.2777 0.3501 0.054(4) Uiso 1 calc R . . C45 C 0.3027(8) 0.3362(5) 0.3421(3) 0.048(2) Uiso 1 d . . . H45 H 0.2741 0.3243 0.3729 0.054(4) Uiso 1 calc R . . C46 C 0.2360(8) 0.3802(5) 0.3103(3) 0.043(2) Uiso 1 d . . . H46 H 0.1599 0.3969 0.3188 0.054(4) Uiso 1 calc R . . C47 C 0.2807(8) 0.4000(5) 0.2660(3) 0.043(2) Uiso 1 d . . . H47 H 0.2357 0.4305 0.2443 0.054(4) Uiso 1 calc R . . C48 C 0.3909(7) 0.3749(4) 0.2540(3) 0.0340(19) Uiso 1 d . . . H48 H 0.4222 0.3892 0.2242 0.054(4) Uiso 1 calc R . . C49 C 0.6378(7) 0.2228(4) 0.3026(3) 0.0285(18) Uiso 1 d . . . C50 C 0.6149(7) 0.1568(4) 0.2838(3) 0.0314(19) Uiso 1 d . . . H50 H 0.5791 0.1510 0.2512 0.054(4) Uiso 1 calc R . . C51 C 0.6451(7) 0.0988(4) 0.3133(3) 0.038(2) Uiso 1 d . . . H51 H 0.6309 0.0535 0.3007 0.054(4) Uiso 1 calc R . . C52 C 0.6955(7) 0.1085(4) 0.3605(3) 0.036(2) Uiso 1 d . . . H52 H 0.7144 0.0693 0.3807 0.054(4) Uiso 1 calc R . . C53 C 0.7190(7) 0.1731(4) 0.3792(3) 0.0343(19) Uiso 1 d . . . H53 H 0.7549 0.1784 0.4118 0.054(4) Uiso 1 calc R . . C54 C 0.6906(7) 0.2311(4) 0.3505(3) 0.0302(19) Uiso 1 d . . . H54 H 0.7069 0.2761 0.3633 0.054(4) Uiso 1 calc R . . Cl1S Cl 0.9851(3) 0.03875(17) 0.29947(11) 0.078 Uiso 0.962(4) d P . . Cl2S Cl 0.9961(3) 0.18769(19) 0.30374(13) 0.090 Uiso 0.962(4) d P . . Cl3S Cl 0.8117(5) 0.0205(3) 0.06597(19) 0.125 Uiso 0.822(5) d P . . Cl4S Cl 1.0605(5) -0.0200(3) 0.0873(2) 0.131 Uiso 0.822(5) d P . . C55S C 0.9488(9) 0.1167(6) 0.2670(4) 0.057 Uiso 0.962(4) d P . . C56S C 0.9619(16) 0.0403(10) 0.0628(6) 0.109 Uiso 0.822(5) d P . . 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 0.0244(3) 0.0215(3) 0.0208(3) 0.0002(4) -0.0005(2) 0.0014(4) P1 0.0258(10) 0.0287(12) 0.0314(11) 0.0023(10) -0.0006(8) -0.0020(10) P2 0.0294(11) 0.0251(11) 0.0198(10) 0.0016(9) 0.0001(8) 0.0021(9) P3 0.0317(11) 0.0247(12) 0.0235(11) -0.0004(9) 0.0023(9) 0.0002(9) O1 0.025(3) 0.026(3) 0.036(3) 0.001(2) -0.001(2) 0.000(2) O2 0.034(3) 0.032(3) 0.024(3) 0.003(2) 0.000(2) -0.003(3) O3 0.032(3) 0.029(3) 0.023(3) -0.001(2) -0.001(2) 0.004(2) O4 0.072(5) 0.020(4) 0.075(5) -0.005(3) -0.003(4) -0.009(3) O5 0.057(4) 0.030(3) 0.042(4) -0.010(3) 0.011(3) -0.003(3) O6 0.068(4) 0.030(3) 0.035(3) 0.005(3) -0.006(3) -0.014(3) O7 0.046(4) 0.023(3) 0.068(4) 0.001(3) -0.009(3) -0.006(3) O8 0.024(3) 0.027(3) 0.033(3) -0.002(2) -0.004(2) 0.001(2) O9 0.024(3) 0.026(3) 0.037(3) 0.001(2) -0.006(2) -0.004(2) O10 0.033(4) 0.092(5) 0.051(4) 0.012(4) 0.001(3) 0.034(4) O11 0.033(3) 0.052(4) 0.036(3) 0.012(3) 0.005(3) 0.016(3) O12 0.045(4) 0.054(4) 0.030(3) -0.007(3) -0.006(3) 0.019(3) N1 0.049(5) 0.022(4) 0.046(5) 0.002(4) -0.006(4) 0.000(4) N2 0.035(4) 0.025(4) 0.031(4) 0.003(3) -0.008(3) -0.001(3) N3 0.035(4) 0.043(5) 0.043(5) 0.002(4) 0.002(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O1 2.269(5) . ? Y1 O3 2.283(5) . ? Y1 O2 2.284(5) . ? Y1 O8 2.403(5) . ? Y1 O6 2.441(5) . ? Y1 O5 2.443(5) . ? Y1 O11 2.465(5) . ? Y1 O12 2.476(5) . ? Y1 O9 2.506(5) . ? Y1 N1 2.862(7) . ? Y1 N2 2.869(7) . ? Y1 N3 2.886(7) . ? P1 O1 1.503(5) . ? P1 C1 1.793(8) . ? P1 C13 1.794(8) . ? P1 C7 1.807(8) . ? P2 O2 1.484(5) . ? P2 C25 1.793(8) . ? P2 C31 1.802(8) . ? P2 C19 1.804(8) . ? P3 O3 1.498(5) . ? P3 C37 1.789(8) . ? P3 C43 1.789(7) . ? P3 C49 1.795(8) . ? O4 N1 1.215(8) . ? O5 N1 1.259(8) . ? O6 N1 1.254(8) . ? O7 N2 1.235(8) . ? O8 N2 1.271(8) . ? O9 N2 1.262(8) . ? O10 N3 1.220(8) . ? O11 N3 1.264(8) . ? O12 N3 1.259(8) . ? C1 C2 1.392(11) . ? C1 C6 1.400(11) . ? C2 C3 1.404(12) . ? C3 C4 1.348(12) . ? C4 C5 1.410(12) . ? C5 C6 1.360(12) . ? C7 C12 1.387(10) . ? C7 C8 1.390(10) . ? C8 C9 1.389(11) . ? C9 C10 1.397(11) . ? C10 C11 1.379(11) . ? C11 C12 1.386(11) . ? C13 C14 1.382(11) . ? C13 C18 1.392(11) . ? C14 C15 1.386(12) . ? C15 C16 1.400(13) . ? C16 C17 1.380(13) . ? C17 C18 1.389(13) . ? C19 C24 1.372(10) . ? C19 C20 1.393(10) . ? C20 C21 1.407(11) . ? C21 C22 1.387(11) . ? C22 C23 1.357(11) . ? C23 C24 1.403(11) . ? C25 C30 1.385(10) . ? C25 C26 1.398(11) . ? C26 C27 1.402(12) . ? C27 C28 1.369(12) . ? C28 C29 1.370(12) . ? C29 C30 1.400(11) . ? C31 C36 1.386(10) . ? C31 C32 1.403(10) . ? C32 C33 1.371(11) . ? C33 C34 1.378(11) . ? C34 C35 1.382(11) . ? C35 C36 1.387(11) . ? C37 C38 1.386(11) . ? C37 C42 1.399(10) . ? C38 C39 1.399(13) . ? C39 C40 1.358(12) . ? C40 C41 1.335(12) . ? C41 C42 1.398(12) . ? C43 C44 1.385(10) . ? C43 C48 1.402(10) . ? C44 C45 1.383(11) . ? C45 C46 1.386(11) . ? C46 C47 1.395(11) . ? C47 C48 1.382(11) . ? C49 C50 1.392(11) . ? C49 C54 1.395(10) . ? C50 C51 1.404(11) . ? C51 C52 1.376(10) . ? C52 C53 1.367(11) . ? C53 C54 1.389(10) . ? Cl1S C55S 1.778(11) . ? Cl2S C55S 1.755(11) . ? Cl3S C56S 1.722(18) . ? Cl4S C56S 1.700(18) . ? 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 Y1 O3 86.24(18) . . ? O1 Y1 O2 83.42(18) . . ? O3 Y1 O2 149.49(18) . . ? O1 Y1 O8 127.28(17) . . ? O3 Y1 O8 83.93(17) . . ? O2 Y1 O8 79.78(17) . . ? O1 Y1 O6 82.64(19) . . ? O3 Y1 O6 78.16(19) . . ? O2 Y1 O6 128.43(19) . . ? O8 Y1 O6 144.01(18) . . ? O1 Y1 O5 77.32(19) . . ? O3 Y1 O5 128.53(19) . . ? O2 Y1 O5 76.76(19) . . ? O8 Y1 O5 143.41(18) . . ? O6 Y1 O5 51.76(19) . . ? O1 Y1 O11 151.29(18) . . ? O3 Y1 O11 75.16(18) . . ? O2 Y1 O11 123.22(18) . . ? O8 Y1 O11 72.97(18) . . ? O6 Y1 O11 72.4(2) . . ? O5 Y1 O11 97.2(2) . . ? O1 Y1 O12 146.36(18) . . ? O3 Y1 O12 125.71(17) . . ? O2 Y1 O12 73.18(18) . . ? O8 Y1 O12 72.48(18) . . ? O6 Y1 O12 93.1(2) . . ? O5 Y1 O12 74.06(19) . . ? O11 Y1 O12 51.54(18) . . ? O1 Y1 O9 75.43(16) . . ? O3 Y1 O9 74.00(17) . . ? O2 Y1 O9 75.63(17) . . ? O8 Y1 O9 52.07(16) . . ? O6 Y1 O9 145.36(19) . . ? O5 Y1 O9 142.96(18) . . ? O11 Y1 O9 118.54(18) . . ? O12 Y1 O9 119.82(18) . . ? O1 Y1 N1 78.01(19) . . ? O3 Y1 N1 103.2(2) . . ? O2 Y1 N1 102.6(2) . . ? O8 Y1 N1 154.49(19) . . ? O6 Y1 N1 25.84(18) . . ? O5 Y1 N1 25.95(18) . . ? O11 Y1 N1 85.1(2) . . ? O12 Y1 N1 83.8(2) . . ? O9 Y1 N1 153.41(18) . . ? O1 Y1 N2 101.35(18) . . ? O3 Y1 N2 78.03(18) . . ? O2 Y1 N2 76.02(18) . . ? O8 Y1 N2 26.02(16) . . ? O6 Y1 N2 155.52(19) . . ? O5 Y1 N2 152.71(19) . . ? O11 Y1 N2 96.02(19) . . ? O12 Y1 N2 96.1(2) . . ? O9 Y1 N2 26.05(16) . . ? N1 Y1 N2 178.57(19) . . ? O1 Y1 N3 162.52(19) . . ? O3 Y1 N3 100.35(19) . . ? O2 Y1 N3 98.01(19) . . ? O8 Y1 N3 69.86(19) . . ? O6 Y1 N3 82.9(2) . . ? O5 Y1 N3 86.0(2) . . ? O11 Y1 N3 25.82(17) . . ? O12 Y1 N3 25.74(17) . . ? O9 Y1 N3 121.89(18) . . ? N1 Y1 N3 84.7(2) . . ? N2 Y1 N3 95.87(19) . . ? O1 P1 C1 109.7(3) . . ? O1 P1 C13 111.4(3) . . ? C1 P1 C13 108.1(4) . . ? O1 P1 C7 109.8(3) . . ? C1 P1 C7 107.9(4) . . ? C13 P1 C7 109.8(3) . . ? O2 P2 C25 111.5(3) . . ? O2 P2 C31 111.4(3) . . ? C25 P2 C31 107.9(4) . . ? O2 P2 C19 111.1(3) . . ? C25 P2 C19 107.7(4) . . ? C31 P2 C19 107.0(4) . . ? O3 P3 C37 112.0(3) . . ? O3 P3 C43 110.6(3) . . ? C37 P3 C43 107.7(4) . . ? O3 P3 C49 110.8(3) . . ? C37 P3 C49 108.5(3) . . ? C43 P3 C49 106.9(4) . . ? P1 O1 Y1 156.8(3) . . ? P2 O2 Y1 173.7(3) . . ? P3 O3 Y1 162.6(3) . . ? N1 O5 Y1 95.9(4) . . ? N1 O6 Y1 96.2(4) . . ? N2 O8 Y1 97.9(4) . . ? N2 O9 Y1 93.3(4) . . ? N3 O11 Y1 96.0(4) . . ? N3 O12 Y1 95.6(4) . . ? O4 N1 O6 121.8(8) . . ? O4 N1 O5 122.2(7) . . ? O6 N1 O5 116.0(7) . . ? O4 N1 Y1 177.0(6) . . ? O6 N1 Y1 58.0(4) . . ? O5 N1 Y1 58.1(4) . . ? O7 N2 O9 121.9(7) . . ? O7 N2 O8 121.4(6) . . ? O9 N2 O8 116.7(6) . . ? O7 N2 Y1 177.3(5) . . ? O9 N2 Y1 60.7(4) . . ? O8 N2 Y1 56.1(3) . . ? O10 N3 O12 121.2(7) . . ? O10 N3 O11 122.1(7) . . ? O12 N3 O11 116.7(6) . . ? O10 N3 Y1 176.6(6) . . ? O12 N3 Y1 58.6(4) . . ? O11 N3 Y1 58.2(4) . . ? C2 C1 C6 118.1(8) . . ? C2 C1 P1 122.7(6) . . ? C6 C1 P1 119.1(6) . . ? C1 C2 C3 120.4(8) . . ? C4 C3 C2 120.0(9) . . ? C3 C4 C5 120.7(9) . . ? C6 C5 C4 119.2(9) . . ? C5 C6 C1 121.7(9) . . ? C12 C7 C8 119.9(7) . . ? C12 C7 P1 117.9(6) . . ? C8 C7 P1 122.2(6) . . ? C9 C8 C7 119.7(8) . . ? C8 C9 C10 119.9(8) . . ? C11 C10 C9 120.1(8) . . ? C10 C11 C12 119.9(8) . . ? C11 C12 C7 120.4(7) . . ? C14 C13 C18 120.6(8) . . ? C14 C13 P1 119.9(6) . . ? C18 C13 P1 118.8(6) . . ? C13 C14 C15 119.9(9) . . ? C14 C15 C16 120.6(9) . . ? C17 C16 C15 118.1(10) . . ? C16 C17 C18 122.3(10) . . ? C17 C18 C13 118.4(9) . . ? C24 C19 C20 120.1(7) . . ? C24 C19 P2 123.6(6) . . ? C20 C19 P2 116.2(6) . . ? C19 C20 C21 119.4(7) . . ? C22 C21 C20 119.1(8) . . ? C23 C22 C21 121.5(8) . . ? C22 C23 C24 119.5(8) . . ? C19 C24 C23 120.4(7) . . ? C30 C25 C26 120.6(8) . . ? C30 C25 P2 121.9(6) . . ? C26 C25 P2 117.5(6) . . ? C25 C26 C27 117.8(8) . . ? C28 C27 C26 121.7(10) . . ? C27 C28 C29 120.1(10) . . ? C28 C29 C30 120.0(9) . . ? C25 C30 C29 119.8(8) . . ? C36 C31 C32 118.7(7) . . ? C36 C31 P2 118.5(6) . . ? C32 C31 P2 122.7(6) . . ? C33 C32 C31 120.7(8) . . ? C32 C33 C34 119.7(8) . . ? C33 C34 C35 120.9(9) . . ? C34 C35 C36 119.3(8) . . ? C31 C36 C35 120.7(8) . . ? C38 C37 C42 118.3(8) . . ? C38 C37 P3 123.7(6) . . ? C42 C37 P3 118.0(6) . . ? C37 C38 C39 120.7(9) . . ? C40 C39 C38 119.3(10) . . ? C41 C40 C39 121.3(10) . . ? C40 C41 C42 121.3(9) . . ? C41 C42 C37 119.0(8) . . ? C44 C43 C48 118.4(7) . . ? C44 C43 P3 124.2(6) . . ? C48 C43 P3 117.4(6) . . ? C45 C44 C43 121.1(8) . . ? C44 C45 C46 120.0(9) . . ? C45 C46 C47 119.8(8) . . ? C48 C47 C46 119.6(8) . . ? C47 C48 C43 121.0(8) . . ? C50 C49 C54 120.1(7) . . ? C50 C49 P3 118.6(6) . . ? C54 C49 P3 121.3(6) . . ? C49 C50 C51 119.5(7) . . ? C52 C51 C50 119.2(8) . . ? C53 C52 C51 121.6(8) . . ? C52 C53 C54 120.0(8) . . ? C53 C54 C49 119.6(7) . . ? Cl2S C55S Cl1S 109.5(6) . . ? Cl4S C56S Cl3S 115.2(11) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.484 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.115 #===END #===================================================== data_Clev99_1 #------------------------------------------------------------------------------ _audit_creation_date '1999-08-31' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 20.111(1) _cell_length_b 10.8636(4) _cell_length_c 20.648(1) _cell_angle_alpha 90 _cell_angle_beta 106.830(2) _cell_angle_gamma 90 _cell_volume 4318.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 923.58 _chemical_formula_analytical ? _chemical_name_systematic ; tris(nitrato-O,O')tris(diphenylmethylphosphineoxide)yttrium(III) ; _chemical_formula_sum 'C39 H39 N3 O12 P3 Y ' _chemical_formula_moiety 'C39 H39 N3 O12 P3 Y ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1896.00 _exptl_absorpt_coefficient_mu 1.526 _exptl_absorpt_correction_type 'multi-scan' # SORTAV _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius ccd diffractometer' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 # loop_ # _diffrn_standard_refln_index_h # _diffrn_standard_refln_index_k # _diffrn_standard_refln_index_l # ? ? ? _diffrn_reflns_number 68129 _reflns_number_total 8832 _reflns_number_gt 4609 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.43 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H 0 156 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; C 0 156 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 12 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 48 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 12 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Y 0 4 -2.951 3.542 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Y(1) 0.27237(3) 0.24480(5) 0.03699(3) 0.0214(1) 1.000 . Uani d ? P(1) 0.26761(9) 0.5818(1) 0.01892(9) 0.0324(5) 1.000 . Uani d ? P(2) 0.18354(8) 0.3261(1) 0.16464(9) 0.0310(5) 1.000 . Uani d ? P(3) 0.2812(1) 0.2116(1) -0.1375(1) 0.0478(7) 1.000 . Uani d ? O(1) 0.2660(2) 0.4448(3) 0.0060(2) 0.034(1) 1.000 . Uani d ? O(2) 0.2047(2) 0.3039(3) 0.1010(2) 0.034(1) 1.000 . Uani d ? O(3) 0.2947(2) 0.2128(3) -0.0624(2) 0.044(2) 1.000 . Uani d ? O(4) 0.4619(3) 0.3695(5) 0.1522(3) 0.096(2) 1.000 . Uani d ? O(5) 0.3537(2) 0.3296(4) 0.1403(2) 0.050(2) 1.000 . Uani d ? O(6) 0.3963(2) 0.2906(3) 0.0586(2) 0.045(2) 1.000 . Uani d ? O(7) 0.3383(2) -0.0907(4) 0.1277(2) 0.052(2) 1.000 . Uani d ? O(8) 0.3326(2) 0.0445(3) 0.0482(3) 0.054(2) 1.000 . Uani d ? O(9) 0.2892(2) 0.0878(4) 0.1282(2) 0.052(2) 1.000 . Uani d ? O(10) 0.0805(2) 0.1216(4) -0.0711(3) 0.085(2) 1.000 . Uani d ? O(11) 0.1833(2) 0.0907(3) -0.0015(2) 0.038(1) 1.000 . Uani d ? O(12) 0.1567(2) 0.2698(3) -0.0478(2) 0.044(1) 1.000 . Uani d ? N(1) 0.4059(3) 0.3309(5) 0.1175(3) 0.048(2) 1.000 . Uani d ? N(2) 0.3209(3) 0.0112(5) 0.1021(3) 0.039(2) 1.000 . Uani d ? N(3) 0.1379(3) 0.1591(4) -0.0416(3) 0.047(2) 1.000 . Uani d ? C(1) 0.2888(3) 0.6179(5) 0.1063(3) 0.042(2) 1.000 . Uani d ? C(2) 0.3319(3) 0.6519(5) -0.0139(3) 0.035(2) 1.000 . Uani d ? C(3) 0.3328(3) 0.7768(5) -0.0262(4) 0.052(3) 1.000 . Uani d ? C(4) 0.3848(4) 0.8286(6) -0.0500(4) 0.061(3) 1.000 . Uani d ? C(5) 0.4351(3) 0.7551(7) -0.0615(4) 0.063(3) 1.000 . Uani d ? C(6) 0.4364(4) 0.6303(6) -0.0486(4) 0.070(3) 1.000 . Uani d ? C(7) 0.3851(3) 0.5789(5) -0.0248(4) 0.051(3) 1.000 . Uani d ? C(8) 0.1855(3) 0.6508(5) -0.0205(3) 0.029(2) 1.000 . Uani d ? C(9) 0.1355(3) 0.5841(5) -0.0690(3) 0.034(2) 1.000 . Uani d ? C(10) 0.0710(3) 0.6351(5) -0.1000(3) 0.044(2) 1.000 . Uani d ? C(11) 0.0547(3) 0.7520(6) -0.0823(3) 0.045(2) 1.000 . Uani d ? C(12) 0.1026(4) 0.8181(5) -0.0338(4) 0.042(2) 1.000 . Uani d ? C(13) 0.1680(3) 0.7678(5) -0.0025(3) 0.036(2) 1.000 . Uani d ? C(14) 0.2546(3) 0.3460(5) 0.2383(3) 0.040(2) 1.000 . Uani d ? C(15) 0.1332(3) 0.1980(5) 0.1803(3) 0.028(2) 1.000 . Uani d ? C(16) 0.1233(3) 0.0964(5) 0.1376(3) 0.039(2) 1.000 . Uani d ? C(17) 0.0829(3) -0.0015(5) 0.1477(4) 0.044(2) 1.000 . Uani d ? C(18) 0.0541(3) 0.0013(5) 0.2006(4) 0.045(2) 1.000 . Uani d ? C(19) 0.0642(3) 0.1012(6) 0.2439(3) 0.041(2) 1.000 . Uani d ? C(20) 0.1033(3) 0.2006(5) 0.2328(3) 0.037(2) 1.000 . Uani d ? C(21) 0.1297(3) 0.4610(5) 0.1549(3) 0.025(2) 1.000 . Uani d ? C(22) 0.1220(3) 0.5268(5) 0.2095(3) 0.039(2) 1.000 . Uani d ? C(23) 0.0763(4) 0.6271(5) 0.1983(4) 0.050(3) 1.000 . Uani d ? C(24) 0.0401(3) 0.6600(5) 0.1340(4) 0.043(2) 1.000 . Uani d ? C(25) 0.0484(3) 0.5951(5) 0.0788(3) 0.041(2) 1.000 . Uani d ? C(26) 0.0936(3) 0.4960(5) 0.0894(3) 0.034(2) 1.000 . Uani d ? C(27) 0.2551(4) 0.3612(6) -0.1741(4) 0.073(3) 1.000 . Uani d ? C(28) 0.3596(4) 0.1649(6) -0.1576(4) 0.047(3) 1.000 . Uani d ? C(29) 0.4236(4) 0.1857(7) -0.1104(4) 0.069(3) 1.000 . Uani d ? C(30) 0.4839(4) 0.1504(9) -0.1239(5) 0.094(4) 1.000 . Uani d ? C(31) 0.4802(4) 0.0899(8) -0.1830(5) 0.084(4) 1.000 . Uani d ? C(32) 0.4168(5) 0.0646(8) -0.2298(5) 0.086(4) 1.000 . Uani d ? C(33) 0.3567(4) 0.1043(7) -0.2172(4) 0.066(3) 1.000 . Uani d ? C(34) 0.2140(4) 0.1032(6) -0.1774(4) 0.048(3) 1.000 . Uani d ? C(35) 0.1638(5) 0.1231(7) -0.2375(5) 0.082(4) 1.000 . Uani d ? C(36) 0.1147(5) 0.031(1) -0.2648(5) 0.099(4) 1.000 . Uani d ? C(37) 0.1194(5) -0.079(1) -0.2311(6) 0.099(5) 1.000 . Uani d ? C(38) 0.1691(5) -0.1006(7) -0.1722(5) 0.082(4) 1.000 . Uani d ? C(39) 0.2153(4) -0.0095(7) -0.1458(4) 0.067(3) 1.000 . Uani d ? H(1) 0.2548 0.5838 0.1248 0.050 1.000 . Uiso c ? H(2) 0.3331 0.5845 0.1290 0.050 1.000 . Uiso c ? H(3) 0.2900 0.7048 0.1118 0.050 1.000 . Uiso c ? H(4) 0.2977 0.8280 -0.0183 0.062 1.000 . Uiso c ? H(5) 0.3851 0.9147 -0.0582 0.074 1.000 . Uiso c ? H(6) 0.4699 0.7903 -0.0787 0.076 1.000 . Uiso c ? H(7) 0.4722 0.5802 -0.0561 0.084 1.000 . Uiso c ? H(8) 0.3859 0.4931 -0.0157 0.062 1.000 . Uiso c ? H(9) 0.1459 0.5033 -0.0809 0.041 1.000 . Uiso c ? H(10) 0.0377 0.5897 -0.1336 0.053 1.000 . Uiso c ? H(11) 0.0103 0.7864 -0.1037 0.053 1.000 . Uiso c ? H(12) 0.0913 0.8980 -0.0216 0.051 1.000 . Uiso c ? H(13) 0.2009 0.8135 0.0312 0.044 1.000 . Uiso c ? H(14) 0.2815 0.4146 0.2324 0.048 1.000 . Uiso c ? H(15) 0.2826 0.2740 0.2459 0.048 1.000 . Uiso c ? H(16) 0.2377 0.3600 0.2761 0.048 1.000 . Uiso c ? H(17) 0.1441 0.0938 0.1018 0.047 1.000 . Uiso c ? H(18) 0.0752 -0.0704 0.1181 0.052 1.000 . Uiso c ? H(19) 0.0269 -0.0663 0.2074 0.054 1.000 . Uiso c ? H(20) 0.0447 0.1021 0.2807 0.050 1.000 . Uiso c ? H(21) 0.1095 0.2707 0.2614 0.044 1.000 . Uiso c ? H(22) 0.1474 0.5041 0.2543 0.047 1.000 . Uiso c ? H(23) 0.0706 0.6725 0.2357 0.061 1.000 . Uiso c ? H(24) 0.0089 0.7277 0.1268 0.051 1.000 . Uiso c ? H(25) 0.0233 0.6186 0.0341 0.049 1.000 . Uiso c ? H(26) 0.0999 0.4519 0.0518 0.040 1.000 . Uiso c ? H(27) 0.2135 0.3858 -0.1647 0.088 1.000 . Uiso c ? H(28) 0.2907 0.4194 -0.1552 0.088 1.000 . Uiso c ? H(29) 0.2473 0.3574 -0.2217 0.088 1.000 . Uiso c ? H(30) 0.4257 0.2245 -0.0686 0.083 1.000 . Uiso c ? H(31) 0.5277 0.1678 -0.0925 0.113 1.000 . Uiso c ? H(32) 0.5218 0.0649 -0.1922 0.100 1.000 . Uiso c ? H(33) 0.4148 0.0204 -0.2700 0.103 1.000 . Uiso c ? H(34) 0.3130 0.0899 -0.2495 0.079 1.000 . Uiso c ? H(35) 0.1622 0.1992 -0.2606 0.099 1.000 . Uiso c ? H(36) 0.0789 0.0448 -0.3058 0.118 1.000 . Uiso c ? H(37) 0.0867 -0.1424 -0.2498 0.119 1.000 . Uiso c ? H(38) 0.1717 -0.1777 -0.1498 0.098 1.000 . Uiso c ? H(39) 0.2498 -0.0236 -0.1040 0.080 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Y(1) 0.0223(3) 0.0176(3) 0.0247(3) -0.0004(3) 0.0076(2) -0.0004(3) P(1) 0.033(1) 0.0262(9) 0.038(1) -0.0024(7) 0.0090(9) 0.0006(7) P(2) 0.026(1) 0.030(1) 0.037(1) 0.0003(7) 0.0084(9) -0.0003(7) P(3) 0.053(1) 0.049(1) 0.044(1) 0.0039(9) 0.019(1) 0.0060(9) O(1) 0.035(3) 0.020(2) 0.048(3) -0.001(2) 0.011(2) 0.001(2) O(2) 0.036(3) 0.030(2) 0.042(3) 0.000(2) 0.023(2) -0.006(2) O(3) 0.055(3) 0.054(3) 0.026(3) -0.004(2) 0.017(2) -0.001(2) O(4) 0.037(4) 0.166(6) 0.087(5) -0.031(3) 0.020(4) -0.076(4) O(5) 0.031(3) 0.078(3) 0.043(4) -0.011(2) 0.015(3) -0.007(2) O(6) 0.034(3) 0.058(3) 0.045(3) 0.000(2) 0.014(3) -0.018(2) O(7) 0.073(4) 0.026(3) 0.056(4) 0.007(2) 0.015(3) 0.010(2) O(8) 0.077(4) 0.040(3) 0.064(4) 0.019(2) 0.048(3) 0.018(2) O(9) 0.073(4) 0.046(3) 0.038(3) 0.023(2) 0.018(3) 0.003(2) O(10) 0.032(3) 0.050(3) 0.138(6) -0.010(2) -0.030(4) 0.017(3) O(11) 0.030(3) 0.029(2) 0.046(3) 0.005(2) -0.002(2) 0.005(2) O(12) 0.043(3) 0.024(3) 0.057(3) -0.006(2) 0.001(2) 0.005(2) N(1) 0.034(4) 0.057(4) 0.052(5) -0.004(3) 0.009(4) -0.017(3) N(2) 0.042(4) 0.035(4) 0.038(4) -0.001(3) 0.008(3) -0.001(3) N(3) 0.034(4) 0.032(3) 0.064(5) -0.002(3) -0.005(4) 0.000(3) C(1) 0.046(5) 0.036(4) 0.040(5) -0.004(3) 0.006(4) -0.003(3) C(2) 0.032(4) 0.031(4) 0.041(5) -0.006(3) 0.010(4) 0.004(3) C(3) 0.050(5) 0.029(4) 0.087(6) 0.005(3) 0.039(4) 0.009(3) C(4) 0.054(6) 0.038(4) 0.103(7) 0.002(4) 0.041(5) 0.019(4) C(5) 0.054(5) 0.054(5) 0.100(7) -0.003(4) 0.051(5) 0.013(5) C(6) 0.058(6) 0.054(5) 0.121(8) 0.007(4) 0.062(6) 0.006(4) C(7) 0.047(5) 0.035(4) 0.083(6) 0.006(3) 0.036(5) 0.005(4) C(8) 0.025(4) 0.025(3) 0.038(5) 0.001(3) 0.013(3) 0.003(3) C(9) 0.041(4) 0.024(3) 0.037(5) -0.001(3) 0.009(4) 0.000(3) C(10) 0.032(5) 0.048(4) 0.045(5) -0.006(3) 0.001(4) 0.003(3) C(11) 0.029(4) 0.044(4) 0.060(5) 0.005(4) 0.011(4) 0.011(4) C(12) 0.042(5) 0.027(4) 0.059(6) 0.001(3) 0.016(4) 0.006(3) C(13) 0.033(4) 0.031(4) 0.043(4) -0.008(3) 0.007(3) -0.005(3) C(14) 0.031(4) 0.049(4) 0.038(5) -0.002(3) 0.008(4) 0.007(3) C(15) 0.020(4) 0.031(3) 0.032(4) -0.001(3) 0.006(3) 0.000(3) C(16) 0.037(4) 0.028(4) 0.055(5) 0.000(3) 0.018(4) 0.003(3) C(17) 0.045(5) 0.027(4) 0.061(6) -0.004(3) 0.020(4) -0.005(3) C(18) 0.044(5) 0.035(4) 0.052(6) -0.007(3) 0.009(4) 0.009(3) C(19) 0.039(5) 0.047(4) 0.035(5) -0.011(3) 0.007(4) 0.008(3) C(20) 0.036(5) 0.036(4) 0.036(5) -0.003(3) 0.006(4) 0.001(3) C(21) 0.022(4) 0.028(3) 0.024(4) 0.001(3) 0.004(3) 0.005(3) C(22) 0.045(5) 0.037(4) 0.032(5) 0.004(3) 0.006(4) 0.001(3) C(23) 0.054(5) 0.044(5) 0.053(6) 0.000(3) 0.016(5) -0.010(4) C(24) 0.036(5) 0.025(4) 0.063(6) 0.006(3) 0.007(4) 0.003(3) C(25) 0.041(4) 0.037(4) 0.038(5) -0.002(3) 0.003(4) 0.009(3) C(26) 0.032(4) 0.036(4) 0.037(5) 0.000(3) 0.017(4) 0.000(3) C(27) 0.102(7) 0.053(5) 0.076(7) 0.024(4) 0.046(6) 0.023(4) C(28) 0.042(5) 0.058(5) 0.048(6) 0.006(3) 0.025(4) 0.007(4) C(29) 0.049(6) 0.115(7) 0.044(6) 0.008(5) 0.015(5) -0.012(4) C(30) 0.045(6) 0.151(9) 0.085(9) 0.011(5) 0.016(6) -0.019(7) C(31) 0.053(7) 0.126(8) 0.080(8) 0.005(5) 0.033(6) -0.008(6) C(32) 0.068(7) 0.132(8) 0.066(7) -0.003(6) 0.034(6) -0.021(6) C(33) 0.061(6) 0.095(6) 0.055(6) 0.002(5) 0.038(5) -0.012(5) C(34) 0.044(5) 0.060(5) 0.036(5) 0.000(4) 0.006(4) -0.006(4) C(35) 0.070(7) 0.091(7) 0.076(8) 0.025(5) 0.006(6) -0.016(5) C(36) 0.054(7) 0.14(1) 0.074(8) 0.041(6) -0.033(6) -0.040(7) C(37) 0.054(7) 0.13(1) 0.11(1) 0.005(7) 0.028(7) -0.041(8) C(38) 0.093(8) 0.099(7) 0.069(8) -0.043(6) 0.047(6) -0.019(6) C(39) 0.071(6) 0.083(6) 0.046(6) -0.024(5) 0.018(5) -0.002(5) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4609 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0422 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.497 _refine_ls_shift/su_max 0.0130 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.83 _refine_diff_density_max 0.88 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y(1) O(1) 2.258(3) . . yes Y(1) O(2) 2.248(4) . . yes Y(1) O(3) 2.252(4) . . yes Y(1) O(5) 2.461(4) . . yes Y(1) O(6) 2.453(4) . . yes Y(1) O(8) 2.469(4) . . yes Y(1) O(9) 2.491(4) . . yes Y(1) O(11) 2.413(4) . . yes Y(1) O(12) 2.488(4) . . yes P(1) O(1) 1.510(3) . . yes P(1) C(1) 1.773(7) . . yes P(1) C(2) 1.793(6) . . yes P(1) C(8) 1.782(6) . . yes P(2) O(2) 1.513(4) . . yes P(2) C(14) 1.773(6) . . yes P(2) C(15) 1.803(6) . . yes P(2) C(21) 1.798(5) . . yes P(3) O(3) 1.494(4) . . yes P(3) C(27) 1.805(6) . . yes P(3) C(28) 1.815(7) . . yes P(3) C(34) 1.802(7) . . yes O(4) N(1) 1.221(6) . . yes O(5) N(1) 1.267(7) . . yes O(6) N(1) 1.255(7) . . yes O(7) N(2) 1.232(5) . . yes O(8) N(2) 1.255(6) . . yes O(9) N(2) 1.262(6) . . yes O(10) N(3) 1.209(6) . . yes O(11) N(3) 1.278(5) . . yes O(12) N(3) 1.278(5) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(1) H(3) 0.95 . . no C(2) C(3) 1.382(7) . . yes C(2) C(7) 1.401(8) . . yes C(3) C(4) 1.397(9) . . yes C(3) H(4) 0.95 . . no C(4) C(5) 1.363(9) . . yes C(4) H(5) 0.95 . . no C(5) C(6) 1.381(8) . . yes C(5) H(6) 0.95 . . no C(6) C(7) 1.384(9) . . yes C(6) H(7) 0.95 . . no C(7) H(8) 0.95 . . no C(8) C(9) 1.399(7) . . yes C(8) C(13) 1.396(7) . . yes C(9) C(10) 1.385(8) . . yes C(9) H(9) 0.95 . . no C(10) C(11) 1.388(8) . . yes C(10) H(10) 0.95 . . no C(11) C(12) 1.374(8) . . yes C(11) H(11) 0.95 . . no C(12) C(13) 1.398(8) . . yes C(12) H(12) 0.95 . . no C(13) H(13) 0.95 . . no C(14) H(14) 0.95 . . no C(14) H(15) 0.95 . . no C(14) H(16) 0.95 . . no C(15) C(16) 1.390(7) . . yes C(15) C(20) 1.385(8) . . yes C(16) C(17) 1.391(8) . . yes C(16) H(17) 0.95 . . no C(17) C(18) 1.377(9) . . yes C(17) H(18) 0.95 . . no C(18) C(19) 1.385(8) . . yes C(18) H(19) 0.95 . . no C(19) C(20) 1.394(7) . . yes C(19) H(20) 0.95 . . no C(20) H(21) 0.95 . . no C(21) C(22) 1.382(8) . . yes C(21) C(26) 1.391(7) . . yes C(22) C(23) 1.400(8) . . yes C(22) H(22) 0.95 . . no C(23) C(24) 1.365(9) . . yes C(23) H(23) 0.95 . . no C(24) C(25) 1.391(9) . . yes C(24) H(24) 0.95 . . no C(25) C(26) 1.384(7) . . yes C(25) H(25) 0.95 . . no C(26) H(26) 0.95 . . no C(27) H(27) 0.95 . . no C(27) H(28) 0.95 . . no C(27) H(29) 0.95 . . no C(28) C(29) 1.389(9) . . yes C(28) C(33) 1.382(9) . . yes C(29) C(30) 1.38(1) . . yes C(29) H(30) 0.95 . . no C(30) C(31) 1.37(1) . . yes C(30) H(31) 0.95 . . no C(31) C(32) 1.39(1) . . yes C(31) H(32) 0.95 . . no C(32) C(33) 1.38(1) . . yes C(32) H(33) 0.95 . . no C(33) H(34) 0.95 . . no C(34) C(35) 1.37(1) . . yes C(34) C(39) 1.384(9) . . yes C(35) C(36) 1.40(1) . . yes C(35) H(35) 0.95 . . no C(36) C(37) 1.38(1) . . yes C(36) H(36) 0.95 . . no C(37) C(38) 1.35(1) . . yes C(37) H(37) 0.95 . . no C(38) C(39) 1.360(9) . . yes C(38) H(38) 0.95 . . no C(39) H(39) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Y(1) O(2) 84.1(1) . . . yes O(1) Y(1) O(3) 84.2(1) . . . yes O(1) Y(1) O(5) 81.6(1) . . . yes O(1) Y(1) O(6) 80.1(1) . . . yes O(1) Y(1) O(8) 149.4(1) . . . yes O(1) Y(1) O(9) 149.0(1) . . . yes O(1) Y(1) O(11) 126.8(1) . . . yes O(1) Y(1) O(12) 74.4(1) . . . yes O(2) Y(1) O(3) 153.5(1) . . . yes O(2) Y(1) O(5) 75.3(2) . . . yes O(2) Y(1) O(6) 126.3(1) . . . yes O(2) Y(1) O(8) 124.1(1) . . . yes O(2) Y(1) O(9) 74.0(1) . . . yes O(2) Y(1) O(11) 82.7(1) . . . yes O(2) Y(1) O(12) 77.4(1) . . . yes O(3) Y(1) O(5) 126.2(2) . . . yes O(3) Y(1) O(6) 74.7(2) . . . yes O(3) Y(1) O(8) 74.2(1) . . . yes O(3) Y(1) O(9) 124.4(1) . . . yes O(3) Y(1) O(11) 85.3(1) . . . yes O(3) Y(1) O(12) 76.6(1) . . . yes O(5) Y(1) O(6) 51.7(1) . . . yes O(5) Y(1) O(8) 93.6(2) . . . yes O(5) Y(1) O(9) 71.9(1) . . . yes O(5) Y(1) O(11) 142.1(1) . . . yes O(5) Y(1) O(12) 145.1(1) . . . yes O(6) Y(1) O(8) 73.5(1) . . . yes O(6) Y(1) O(9) 95.3(2) . . . yes O(6) Y(1) O(11) 145.0(1) . . . yes O(6) Y(1) O(12) 143.1(1) . . . yes O(8) Y(1) O(9) 50.9(1) . . . yes O(8) Y(1) O(11) 73.6(1) . . . yes O(8) Y(1) O(12) 119.7(1) . . . yes O(9) Y(1) O(11) 72.5(1) . . . yes O(9) Y(1) O(12) 120.1(1) . . . yes O(11) Y(1) O(12) 52.4(1) . . . yes O(1) P(1) C(1) 112.6(2) . . . yes O(1) P(1) C(2) 109.4(3) . . . yes O(1) P(1) C(8) 111.4(2) . . . yes C(1) P(1) C(2) 107.6(3) . . . yes C(1) P(1) C(8) 106.8(3) . . . yes C(2) P(1) C(8) 108.9(3) . . . yes O(2) P(2) C(14) 113.9(3) . . . yes O(2) P(2) C(15) 110.2(3) . . . yes O(2) P(2) C(21) 110.1(3) . . . yes C(14) P(2) C(15) 107.2(3) . . . yes C(14) P(2) C(21) 107.8(3) . . . yes C(15) P(2) C(21) 107.3(3) . . . yes O(3) P(3) C(27) 111.7(3) . . . yes O(3) P(3) C(28) 109.3(3) . . . yes O(3) P(3) C(34) 111.5(3) . . . yes C(27) P(3) C(28) 108.8(3) . . . yes C(27) P(3) C(34) 108.0(4) . . . yes C(28) P(3) C(34) 107.4(3) . . . yes Y(1) O(1) P(1) 154.3(3) . . . yes Y(1) O(2) P(2) 157.9(2) . . . yes Y(1) O(3) P(3) 157.3(3) . . . yes Y(1) O(5) N(1) 95.5(4) . . . yes Y(1) O(6) N(1) 96.3(4) . . . yes Y(1) O(8) N(2) 97.2(4) . . . yes Y(1) O(9) N(2) 95.9(4) . . . yes Y(1) O(11) N(3) 97.6(3) . . . yes Y(1) O(12) N(3) 94.0(3) . . . yes O(4) N(1) O(5) 120.6(6) . . . yes O(4) N(1) O(6) 123.0(7) . . . yes O(5) N(1) O(6) 116.4(6) . . . yes O(7) N(2) O(8) 122.5(6) . . . yes O(7) N(2) O(9) 121.6(6) . . . yes O(8) N(2) O(9) 115.9(5) . . . yes O(10) N(3) O(11) 121.9(5) . . . yes O(10) N(3) O(12) 122.3(5) . . . yes O(11) N(3) O(12) 115.8(5) . . . yes P(1) C(1) H(1) 109.5 . . . no P(1) C(1) H(2) 109.5 . . . no P(1) C(1) H(3) 109.5 . . . no H(1) C(1) H(2) 109.5 . . . no H(1) C(1) H(3) 109.5 . . . no H(2) C(1) H(3) 109.5 . . . no P(1) C(2) C(3) 122.5(5) . . . yes P(1) C(2) C(7) 119.2(5) . . . yes C(3) C(2) C(7) 118.3(6) . . . yes C(2) C(3) C(4) 120.9(6) . . . yes C(2) C(3) H(4) 119.6 . . . no C(4) C(3) H(4) 119.6 . . . no C(3) C(4) C(5) 119.6(6) . . . yes C(3) C(4) H(5) 120.2 . . . no C(5) C(4) H(5) 120.2 . . . no C(4) C(5) C(6) 121.0(6) . . . yes C(4) C(5) H(6) 119.5 . . . no C(6) C(5) H(6) 119.5 . . . no C(5) C(6) C(7) 119.4(6) . . . yes C(5) C(6) H(7) 120.3 . . . no C(7) C(6) H(7) 120.3 . . . no C(2) C(7) C(6) 120.8(6) . . . yes C(2) C(7) H(8) 119.6 . . . no C(6) C(7) H(8) 119.6 . . . no P(1) C(8) C(9) 119.2(4) . . . yes P(1) C(8) C(13) 122.2(4) . . . yes C(9) C(8) C(13) 118.6(5) . . . yes C(8) C(9) C(10) 120.4(5) . . . yes C(8) C(9) H(9) 119.8 . . . no C(10) C(9) H(9) 119.8 . . . no C(9) C(10) C(11) 120.4(5) . . . yes C(9) C(10) H(10) 119.8 . . . no C(11) C(10) H(10) 119.8 . . . no C(10) C(11) C(12) 120.0(5) . . . yes C(10) C(11) H(11) 120.0 . . . no C(12) C(11) H(11) 120.0 . . . no C(11) C(12) C(13) 120.1(6) . . . yes C(11) C(12) H(12) 120.0 . . . no C(13) C(12) H(12) 120.0 . . . no C(8) C(13) C(12) 120.5(5) . . . yes C(8) C(13) H(13) 119.7 . . . no C(12) C(13) H(13) 119.7 . . . no P(2) C(14) H(14) 109.5 . . . no P(2) C(14) H(15) 109.5 . . . no P(2) C(14) H(16) 109.5 . . . no H(14) C(14) H(15) 109.5 . . . no H(14) C(14) H(16) 109.5 . . . no H(15) C(14) H(16) 109.5 . . . no P(2) C(15) C(16) 119.0(5) . . . yes P(2) C(15) C(20) 121.2(4) . . . yes C(16) C(15) C(20) 119.8(5) . . . yes C(15) C(16) C(17) 119.7(6) . . . yes C(15) C(16) H(17) 120.1 . . . no C(17) C(16) H(17) 120.1 . . . no C(16) C(17) C(18) 120.0(6) . . . yes C(16) C(17) H(18) 120.0 . . . no C(18) C(17) H(18) 120.0 . . . no C(17) C(18) C(19) 120.9(6) . . . yes C(17) C(18) H(19) 119.6 . . . no C(19) C(18) H(19) 119.6 . . . no C(18) C(19) C(20) 119.0(6) . . . yes C(18) C(19) H(20) 120.5 . . . no C(20) C(19) H(20) 120.5 . . . no C(15) C(20) C(19) 120.5(6) . . . yes C(15) C(20) H(21) 119.7 . . . no C(19) C(20) H(21) 119.7 . . . no P(2) C(21) C(22) 122.5(5) . . . yes P(2) C(21) C(26) 117.4(5) . . . yes C(22) C(21) C(26) 120.1(5) . . . yes C(21) C(22) C(23) 119.4(6) . . . yes C(21) C(22) H(22) 120.3 . . . no C(23) C(22) H(22) 120.3 . . . no C(22) C(23) C(24) 120.3(6) . . . yes C(22) C(23) H(23) 119.9 . . . no C(24) C(23) H(23) 119.9 . . . no C(23) C(24) C(25) 120.5(6) . . . yes C(23) C(24) H(24) 119.8 . . . no C(25) C(24) H(24) 119.7 . . . no C(24) C(25) C(26) 119.6(6) . . . yes C(24) C(25) H(25) 120.2 . . . no C(26) C(25) H(25) 120.2 . . . no C(21) C(26) C(25) 120.0(6) . . . yes C(21) C(26) H(26) 120.0 . . . no C(25) C(26) H(26) 120.0 . . . no P(3) C(27) H(27) 109.5 . . . no P(3) C(27) H(28) 109.5 . . . no P(3) C(27) H(29) 109.5 . . . no H(27) C(27) H(28) 109.4 . . . no H(27) C(27) H(29) 109.4 . . . no H(28) C(27) H(29) 109.5 . . . no P(3) C(28) C(29) 119.0(6) . . . yes P(3) C(28) C(33) 121.4(6) . . . yes C(29) C(28) C(33) 119.5(7) . . . yes C(28) C(29) C(30) 120.3(8) . . . yes C(28) C(29) H(30) 119.8 . . . no C(30) C(29) H(30) 119.8 . . . no C(29) C(30) C(31) 119.4(8) . . . yes C(29) C(30) H(31) 120.3 . . . no C(31) C(30) H(31) 120.3 . . . no C(30) C(31) C(32) 121.2(8) . . . yes C(30) C(31) H(32) 119.4 . . . no C(32) C(31) H(32) 119.4 . . . no C(31) C(32) C(33) 119.1(8) . . . yes C(31) C(32) H(33) 120.5 . . . no C(33) C(32) H(33) 120.4 . . . no C(28) C(33) C(32) 120.3(8) . . . yes C(28) C(33) H(34) 119.8 . . . no C(32) C(33) H(34) 119.8 . . . no P(3) C(34) C(35) 124.6(6) . . . yes P(3) C(34) C(39) 117.0(6) . . . yes C(35) C(34) C(39) 118.3(7) . . . yes C(34) C(35) C(36) 120.0(8) . . . yes C(34) C(35) H(35) 120.0 . . . no C(36) C(35) H(35) 120.0 . . . no C(35) C(36) C(37) 118.7(9) . . . yes C(35) C(36) H(36) 120.7 . . . no C(37) C(36) H(36) 120.6 . . . no C(36) C(37) C(38) 122(1) . . . yes C(36) C(37) H(37) 119.1 . . . no C(38) C(37) H(37) 119.0 . . . no C(37) C(38) C(39) 118.6(9) . . . yes C(37) C(38) H(38) 120.8 . . . no C(39) C(38) H(38) 120.7 . . . no C(34) C(39) C(38) 122.5(8) . . . yes C(34) C(39) H(39) 118.7 . . . no C(38) C(39) H(39) 118.8 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(4) C(36) 3.239(9) . 4 no O(4) C(6) 3.36(1) . 3_665 no O(4) C(19) 3.444(8) . 2 no O(4) C(5) 3.446(9) . 3_665 no O(4) C(18) 3.457(9) . 2 no O(6) C(5) 3.409(8) . 3_665 no O(6) C(6) 3.535(8) . 3_665 no O(7) C(1) 3.310(7) . 1_545 no O(7) C(3) 3.462(8) . 1_545 no O(7) C(22) 3.465(8) . 2_545 no O(7) C(31) 3.50(1) . 3_655 no O(7) C(20) 3.586(7) . 2_545 no O(8) C(3) 3.290(7) . 1_545 no O(8) C(4) 3.457(9) . 1_545 no O(9) C(22) 3.375(8) . 2_545 no O(10) C(24) 3.372(7) . 3_565 no O(10) C(12) 3.386(7) . 1_545 no O(10) C(17) 3.463(8) . 3 no O(10) C(18) 3.473(8) . 3 no O(11) C(12) 3.350(7) . 1_545 no O(11) C(13) 3.521(7) . 1_545 no C(1) C(20) 3.519(9) . 2 no C(10) C(25) 3.580(9) . 3_565 no C(12) C(38) 3.60(1) . 1_565 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Y(1) O(1) P(1) C(1) . . . . 4.4(6) no Y(1) O(1) P(1) C(2) . . . . 124.0(5) no Y(1) O(1) P(1) C(8) . . . . -115.6(5) no Y(1) O(2) P(2) C(14) . . . . 25.5(6) no Y(1) O(2) P(2) C(15) . . . . -95.0(6) no Y(1) O(2) P(2) C(21) . . . . 146.7(5) no Y(1) O(3) P(3) C(27) . . . . 54.3(7) no Y(1) O(3) P(3) C(28) . . . . 174.8(6) no Y(1) O(3) P(3) C(34) . . . . -66.7(7) no Y(1) O(5) N(1) O(4) . . . . 179.0(6) no Y(1) O(5) N(1) O(6) . . . . -1.3(6) no Y(1) O(6) N(1) O(4) . . . . -179.0(6) no Y(1) O(6) N(1) O(5) . . . . 1.3(6) no Y(1) O(8) N(2) O(7) . . . . 176.0(5) no Y(1) O(8) N(2) O(9) . . . . -3.0(6) no Y(1) O(9) N(2) O(7) . . . . -176.0(5) no Y(1) O(9) N(2) O(8) . . . . 2.9(6) no Y(1) O(11) N(3) O(10) . . . . -176.1(6) no Y(1) O(11) N(3) O(12) . . . . 3.2(6) no Y(1) O(12) N(3) O(10) . . . . 176.2(6) no Y(1) O(12) N(3) O(11) . . . . -3.1(6) no P(1) O(1) Y(1) O(2) . . . . 44.5(5) no P(1) O(1) Y(1) O(3) . . . . -159.4(5) no P(1) O(1) Y(1) O(5) . . . . -31.5(5) no P(1) O(1) Y(1) O(6) . . . . -84.0(5) no P(1) O(1) Y(1) O(8) . . . . -114.5(6) no P(1) O(1) Y(1) O(9) . . . . -0.2(7) no P(1) O(1) Y(1) O(11) . . . . 120.8(5) no P(1) O(1) Y(1) O(12) . . . . 122.9(6) no P(1) C(2) C(3) C(4) . . . . 178.2(6) no P(1) C(2) C(7) C(6) . . . . -178.6(6) no P(1) C(8) C(9) C(10) . . . . 179.4(5) no P(1) C(8) C(13) C(12) . . . . -179.0(5) no P(2) O(2) Y(1) O(1) . . . . -118.9(6) no P(2) O(2) Y(1) O(3) . . . . 176.7(5) no P(2) O(2) Y(1) O(5) . . . . -36.0(6) no P(2) O(2) Y(1) O(6) . . . . -45.8(6) no P(2) O(2) Y(1) O(8) . . . . 48.4(6) no P(2) O(2) Y(1) O(9) . . . . 39.0(6) no P(2) O(2) Y(1) O(11) . . . . 112.8(6) no P(2) O(2) Y(1) O(12) . . . . 165.9(6) no P(2) C(15) C(16) C(17) . . . . -178.0(5) no P(2) C(15) C(20) C(19) . . . . 179.6(4) no P(2) C(21) C(22) C(23) . . . . -176.6(5) no P(2) C(21) C(26) C(25) . . . . 176.5(5) no P(3) O(3) Y(1) O(1) . . . . -63.4(6) no P(3) O(3) Y(1) O(2) . . . . 1.0(8) no P(3) O(3) Y(1) O(5) . . . . -138.6(6) no P(3) O(3) Y(1) O(6) . . . . -144.7(6) no P(3) O(3) Y(1) O(8) . . . . 138.5(6) no P(3) O(3) Y(1) O(9) . . . . 129.3(6) no P(3) O(3) Y(1) O(11) . . . . 64.3(6) no P(3) O(3) Y(1) O(12) . . . . 11.9(6) no P(3) C(28) C(29) C(30) . . . . 179.5(7) no P(3) C(28) C(33) C(32) . . . . -176.9(6) no P(3) C(34) C(35) C(36) . . . . 178.6(7) no P(3) C(34) C(39) C(38) . . . . -177.4(7) no O(1) Y(1) O(5) N(1) . . . . -83.2(3) no O(1) Y(1) O(6) N(1) . . . . 86.4(4) no O(1) Y(1) O(8) N(2) . . . . 144.6(3) no O(1) Y(1) O(9) N(2) . . . . -145.0(3) no O(1) Y(1) O(11) N(3) . . . . 0.7(4) no O(1) Y(1) O(12) N(3) . . . . -176.0(4) no O(1) P(1) C(2) C(3) . . . . 162.1(5) no O(1) P(1) C(2) C(7) . . . . -20.8(6) no O(1) P(1) C(8) C(9) . . . . -14.0(6) no O(1) P(1) C(8) C(13) . . . . 163.4(5) no O(2) Y(1) O(5) N(1) . . . . -169.3(4) no O(2) Y(1) O(6) N(1) . . . . 11.3(4) no O(2) Y(1) O(8) N(2) . . . . -9.9(4) no O(2) Y(1) O(9) N(2) . . . . 168.3(4) no O(2) Y(1) O(11) N(3) . . . . 77.7(4) no O(2) Y(1) O(12) N(3) . . . . -88.6(4) no O(2) P(2) C(15) C(16) . . . . 3.6(5) no O(2) P(2) C(15) C(20) . . . . -175.0(5) no O(2) P(2) C(21) C(22) . . . . -157.7(5) no O(2) P(2) C(21) C(26) . . . . 24.2(5) no O(3) Y(1) O(5) N(1) . . . . -6.7(4) no O(3) Y(1) O(6) N(1) . . . . 173.1(4) no O(3) Y(1) O(8) N(2) . . . . -168.5(4) no O(3) Y(1) O(9) N(2) . . . . 9.7(4) no O(3) Y(1) O(11) N(3) . . . . -78.5(4) no O(3) Y(1) O(12) N(3) . . . . 96.3(4) no O(3) P(3) C(28) C(29) . . . . -26.1(6) no O(3) P(3) C(28) C(33) . . . . 150.9(6) no O(3) P(3) C(34) C(35) . . . . 140.9(7) no O(3) P(3) C(34) C(39) . . . . -41.5(7) no O(5) Y(1) O(6) N(1) . . . . -0.7(3) no O(5) Y(1) O(8) N(2) . . . . 64.9(4) no O(5) Y(1) O(9) N(2) . . . . -112.2(4) no O(5) Y(1) O(11) N(3) . . . . 132.3(4) no O(5) Y(1) O(12) N(3) . . . . -127.8(4) no O(6) Y(1) O(5) N(1) . . . . 0.7(3) no O(6) Y(1) O(8) N(2) . . . . 113.1(4) no O(6) Y(1) O(9) N(2) . . . . -65.4(3) no O(6) Y(1) O(11) N(3) . . . . -133.2(4) no O(6) Y(1) O(12) N(3) . . . . 136.1(3) no O(8) Y(1) O(5) N(1) . . . . 66.4(4) no O(8) Y(1) O(6) N(1) . . . . -109.3(4) no O(8) Y(1) O(9) N(2) . . . . -1.7(3) no O(8) Y(1) O(11) N(3) . . . . -153.4(4) no O(8) Y(1) O(12) N(3) . . . . 33.6(4) no O(9) Y(1) O(5) N(1) . . . . 113.2(4) no O(9) Y(1) O(6) N(1) . . . . -62.7(4) no O(9) Y(1) O(8) N(2) . . . . 1.7(3) no O(9) Y(1) O(11) N(3) . . . . 153.1(4) no O(9) Y(1) O(12) N(3) . . . . -25.9(4) no O(11) Y(1) O(5) N(1) . . . . 134.1(3) no O(11) Y(1) O(6) N(1) . . . . -129.5(4) no O(11) Y(1) O(8) N(2) . . . . -78.8(4) no O(11) Y(1) O(9) N(2) . . . . 81.0(3) no O(11) Y(1) O(12) N(3) . . . . 1.9(3) no O(12) Y(1) O(5) N(1) . . . . -129.7(4) no O(12) Y(1) O(6) N(1) . . . . 132.9(4) no O(12) Y(1) O(8) N(2) . . . . -104.6(4) no O(12) Y(1) O(9) N(2) . . . . 103.8(3) no O(12) Y(1) O(11) N(3) . . . . -1.9(3) no C(1) P(1) C(2) C(3) . . . . -75.2(6) no C(1) P(1) C(2) C(7) . . . . 101.8(6) no C(1) P(1) C(8) C(9) . . . . -137.3(5) no C(1) P(1) C(8) C(13) . . . . 40.0(6) no C(2) P(1) C(8) C(9) . . . . 106.7(5) no C(2) P(1) C(8) C(13) . . . . -75.9(6) no C(2) C(3) C(4) C(5) . . . . 0(1) no C(2) C(7) C(6) C(5) . . . . 0(1) no C(3) C(2) P(1) C(8) . . . . 40.2(6) no C(3) C(2) C(7) C(6) . . . . -1(1) no C(3) C(4) C(5) C(6) . . . . -1(1) no C(4) C(3) C(2) C(7) . . . . 1(1) no C(4) C(5) C(6) C(7) . . . . 1(1) no C(7) C(2) P(1) C(8) . . . . -142.7(5) no C(8) C(9) C(10) C(11) . . . . -1(1) no C(8) C(13) C(12) C(11) . . . . 1(1) no C(9) C(8) C(13) C(12) . . . . -1.6(9) no C(9) C(10) C(11) C(12) . . . . 0(1) no C(10) C(9) C(8) C(13) . . . . 2.0(9) no C(10) C(11) C(12) C(13) . . . . 0(1) no C(14) P(2) C(15) C(16) . . . . -120.9(5) no C(14) P(2) C(15) C(20) . . . . 60.5(6) no C(14) P(2) C(21) C(22) . . . . -32.9(6) no C(14) P(2) C(21) C(26) . . . . 149.0(5) no C(15) P(2) C(21) C(22) . . . . 82.2(6) no C(15) P(2) C(21) C(26) . . . . -95.8(5) no C(15) C(16) C(17) C(18) . . . . -1(1) no C(15) C(20) C(19) C(18) . . . . -2(1) no C(16) C(15) P(2) C(21) . . . . 123.5(5) no C(16) C(15) C(20) C(19) . . . . 1.0(9) no C(16) C(17) C(18) C(19) . . . . 1(1) no C(17) C(16) C(15) C(20) . . . . 0.6(9) no C(17) C(18) C(19) C(20) . . . . 1(1) no C(20) C(15) P(2) C(21) . . . . -55.1(6) no C(21) C(22) C(23) C(24) . . . . 0(1) no C(21) C(26) C(25) C(24) . . . . 0.7(9) no C(22) C(21) C(26) C(25) . . . . -1.6(9) no C(22) C(23) C(24) C(25) . . . . -1(1) no C(23) C(22) C(21) C(26) . . . . 1.4(9) no C(23) C(24) C(25) C(26) . . . . 0(1) no C(27) P(3) C(28) C(29) . . . . 96.2(6) no C(27) P(3) C(28) C(33) . . . . -86.9(7) no C(27) P(3) C(34) C(35) . . . . 17.8(8) no C(27) P(3) C(34) C(39) . . . . -164.6(6) no C(28) P(3) C(34) C(35) . . . . -99.4(7) no C(28) P(3) C(34) C(39) . . . . 78.2(7) no C(28) C(29) C(30) C(31) . . . . -3(1) no C(28) C(33) C(32) C(31) . . . . -2(1) no C(29) C(28) P(3) C(34) . . . . -147.2(6) no C(29) C(28) C(33) C(32) . . . . 0(1) no C(29) C(30) C(31) C(32) . . . . 1(2) no C(30) C(29) C(28) C(33) . . . . 2(1) no C(30) C(31) C(32) C(33) . . . . 2(2) no C(33) C(28) P(3) C(34) . . . . 29.8(7) no C(34) C(35) C(36) C(37) . . . . -2(1) no C(34) C(39) C(38) C(37) . . . . -1(1) no C(35) C(34) C(39) C(38) . . . . 0(1) no C(35) C(36) C(37) C(38) . . . . 1(2) no C(36) C(35) C(34) C(39) . . . . 1(1) no C(36) C(37) C(38) C(39) . . . . 0(2) no #===END #===================================================== data_Elev99_6a _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(nitrato-O,O')tetrakis(diphenylmethylphosphineoxide)scandium(III) nitrate dichloromethane solvate ; _chemical_name_common ? _chemical_formula_moiety 'C52 H52 N2 O10 P4 Sc, N O3, 1.3(C H2 Cl2)' _chemical_formula_sum 'C53.30 H54.60 Cl2.60 N3 O13 P4 Sc' _chemical_formula_weight 1206.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sc' 'Sc' 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 /n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 13.712(5) _cell_length_b 23.412(4) _cell_length_c 18.650(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.40(2) _cell_angle_gamma 90.00 _cell_volume 5923(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2498 _exptl_absorpt_coefficient_mu 0.411 _exptl_absorpt_correction_type empirical # psi-scan _exptl_absorpt_correction_T_min 0.796 # 0.8207 _exptl_absorpt_correction_T_max 1.000 # 0.9222 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed fine-focus tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10865 _diffrn_reflns_av_R_equivalents 0.0881 _diffrn_reflns_av_sigmaI/netI 0.1679 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.04 _reflns_number_total 10398 _reflns_number_gt 4535 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+1.3000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10398 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2183 _refine_ls_R_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.3322 _refine_ls_wR_factor_gt 0.2460 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc Sc 0.76482(12) 0.03184(7) 0.24243(9) 0.0233(4) Uani 1 d . . . P1 P 0.96579(17) -0.05330(10) 0.20484(12) 0.0272(6) Uani 1 d . . . P2 P 0.83652(17) 0.15439(9) 0.15129(12) 0.0250(5) Uani 1 d . . . P3 P 0.51959(17) 0.06526(10) 0.16545(12) 0.0269(5) Uani 1 d . . . P4 P 0.67497(18) -0.06613(10) 0.36259(12) 0.0277(5) Uani 1 d . . . O1 O 0.8920(4) -0.0160(3) 0.2334(3) 0.0310(14) Uani 1 d . . . O2 O 0.8211(4) 0.1070(3) 0.2029(3) 0.0316(15) Uani 1 d . . . O3 O 0.6182(4) 0.0561(3) 0.2108(3) 0.0313(14) Uani 1 d . . . O4 O 0.7270(4) -0.0224(3) 0.3229(3) 0.0325(15) Uani 1 d . . . O5 O 0.8440(6) 0.1238(3) 0.4192(4) 0.057(2) Uani 1 d . . . O6 O 0.7332(4) 0.0976(3) 0.3286(3) 0.0332(15) Uani 1 d . . . O7 O 0.8767(4) 0.0606(3) 0.3411(3) 0.0323(15) Uani 1 d . . . O8 O 0.6833(5) -0.0553(3) 0.0572(3) 0.0418(17) Uani 1 d . . . O9 O 0.7495(5) 0.0181(3) 0.1154(3) 0.0336(15) Uani 1 d . . . O10 O 0.6964(5) -0.0511(3) 0.1751(3) 0.0346(15) Uani 1 d . . . O11 O 0.8868(5) 0.2539(3) 0.9664(3) 0.0434(17) Uani 1 d . . . O12 O 0.7562(5) 0.2211(3) 0.9008(4) 0.052(2) Uani 1 d . . . O13 O 0.8976(6) 0.1851(4) 0.8907(4) 0.062(2) Uani 1 d . . . N1 N 0.8194(6) 0.0952(3) 0.3653(4) 0.0319(18) Uiso 1 d . . . N2 N 0.7090(5) -0.0307(3) 0.1145(4) 0.0293(17) Uiso 1 d . . . N3 N 0.8486(6) 0.2201(3) 0.9192(4) 0.0333(18) Uiso 1 d . . . C1 C 0.9121(8) -0.1095(4) 0.1477(5) 0.043(3) Uiso 1 d . . . C2 C 1.0415(7) -0.0859(4) 0.2803(5) 0.028(2) Uiso 1 d . . . C3 C 1.0330(8) -0.0648(5) 0.3490(5) 0.044(3) Uiso 1 d . . . H3 H 0.9902 -0.0337 0.3545 0.075(6) Uiso 1 calc R . . C4 C 1.0891(8) -0.0904(4) 0.4105(6) 0.045(3) Uiso 1 d . . . H4 H 1.0828 -0.0774 0.4578 0.075(6) Uiso 1 calc R . . C5 C 1.1527(7) -0.1342(4) 0.4013(5) 0.041(2) Uiso 1 d . . . H5 H 1.1904 -0.1512 0.4426 0.075(6) Uiso 1 calc R . . C6 C 1.1630(7) -0.1541(4) 0.3327(5) 0.037(2) Uiso 1 d . . . H6 H 1.2086 -0.1837 0.3272 0.075(6) Uiso 1 calc R . . C7 C 1.1065(7) -0.1305(4) 0.2723(5) 0.035(2) Uiso 1 d . . . H7 H 1.1119 -0.1448 0.2253 0.075(6) Uiso 1 calc R . . C8 C 1.0426(6) -0.0116(4) 0.1544(5) 0.028(2) Uiso 1 d . . . C9 C 1.0818(7) -0.0321(4) 0.0940(5) 0.039(2) Uiso 1 d . . . H9 H 1.0703 -0.0705 0.0784 0.075(6) Uiso 1 calc R . . C10 C 1.1375(8) 0.0041(5) 0.0572(6) 0.051(3) Uiso 1 d . . . H10 H 1.1631 -0.0094 0.0156 0.075(6) Uiso 1 calc R . . C11 C 1.1556(8) 0.0584(5) 0.0802(6) 0.050(3) Uiso 1 d . . . H11 H 1.1946 0.0823 0.0546 0.075(6) Uiso 1 calc R . . C12 C 1.1192(8) 0.0801(5) 0.1395(6) 0.053(3) Uiso 1 d . . . H12 H 1.1329 0.1185 0.1542 0.075(6) Uiso 1 calc R . . C13 C 1.0615(8) 0.0453(5) 0.1783(6) 0.047(3) Uiso 1 d . . . H13 H 1.0359 0.0595 0.2194 0.075(6) Uiso 1 calc R . . C14 C 0.8523(7) 0.1285(4) 0.0630(5) 0.031(2) Uiso 1 d . . . C15 C 0.9448(6) 0.1950(4) 0.1874(4) 0.0262(19) Uiso 1 d . . . C16 C 0.9792(7) 0.1928(4) 0.2617(5) 0.035(2) Uiso 1 d . . . H16 H 0.9491 0.1678 0.2920 0.075(6) Uiso 1 calc R . . C17 C 1.0568(7) 0.2270(4) 0.2911(5) 0.038(2) Uiso 1 d . . . H17 H 1.0802 0.2252 0.3416 0.075(6) Uiso 1 calc R . . C18 C 1.1009(7) 0.2639(4) 0.2473(5) 0.037(2) Uiso 1 d . . . H18 H 1.1534 0.2878 0.2682 0.075(6) Uiso 1 calc R . . C19 C 1.0693(7) 0.2662(4) 0.1736(5) 0.037(2) Uiso 1 d . . . H19 H 1.1014 0.2908 0.1441 0.075(6) Uiso 1 calc R . . C20 C 0.9907(7) 0.2325(4) 0.1423(5) 0.031(2) Uiso 1 d . . . H20 H 0.9681 0.2345 0.0917 0.075(6) Uiso 1 calc R . . C21 C 0.7322(7) 0.2034(4) 0.1423(5) 0.029(2) Uiso 1 d . . . C22 C 0.6785(7) 0.2060(4) 0.1978(5) 0.036(2) Uiso 1 d . . . H22 H 0.6944 0.1817 0.2387 0.075(6) Uiso 1 calc R . . C23 C 0.6014(8) 0.2437(4) 0.1954(6) 0.043(3) Uiso 1 d . . . H23 H 0.5623 0.2447 0.2335 0.075(6) Uiso 1 calc R . . C24 C 0.5806(8) 0.2814(5) 0.1349(6) 0.050(3) Uiso 1 d . . . H24 H 0.5280 0.3081 0.1328 0.075(6) Uiso 1 calc R . . C25 C 0.6353(7) 0.2791(4) 0.0812(5) 0.041(2) Uiso 1 d . . . H25 H 0.6217 0.3043 0.0411 0.075(6) Uiso 1 calc R . . C26 C 0.7128(7) 0.2395(4) 0.0836(5) 0.036(2) Uiso 1 d . . . H26 H 0.7513 0.2376 0.0453 0.075(6) Uiso 1 calc R . . C27 C 0.5325(7) 0.0850(4) 0.0737(5) 0.039(2) Uiso 1 d . . . C28 C 0.4536(6) 0.1215(4) 0.2016(5) 0.029(2) Uiso 1 d . . . C29 C 0.3742(7) 0.1484(4) 0.1616(5) 0.036(2) Uiso 1 d . . . H29 H 0.3563 0.1388 0.1119 0.075(6) Uiso 1 calc R . . C30 C 0.3197(8) 0.1892(5) 0.1928(6) 0.046(3) Uiso 1 d . . . H30 H 0.2659 0.2079 0.1644 0.075(6) Uiso 1 calc R . . C31 C 0.3442(8) 0.2023(4) 0.2649(5) 0.040(2) Uiso 1 d . . . H31 H 0.3067 0.2299 0.2863 0.075(6) Uiso 1 calc R . . C32 C 0.4231(7) 0.1757(4) 0.3070(5) 0.039(2) Uiso 1 d . . . H32 H 0.4384 0.1845 0.3571 0.075(6) Uiso 1 calc R . . C33 C 0.4801(7) 0.1357(4) 0.2756(5) 0.032(2) Uiso 1 d . . . H33 H 0.5358 0.1183 0.3035 0.075(6) Uiso 1 calc R . . C34 C 0.4409(7) 0.0033(4) 0.1621(5) 0.029(2) Uiso 1 d . . . C35 C 0.4475(8) -0.0403(4) 0.1138(6) 0.043(3) Uiso 1 d . . . H35 H 0.4951 -0.0378 0.0817 0.075(6) Uiso 1 calc R . . C36 C 0.3877(8) -0.0874(5) 0.1105(6) 0.053(3) Uiso 1 d . . . H36 H 0.3929 -0.1166 0.0760 0.075(6) Uiso 1 calc R . . C37 C 0.3193(8) -0.0919(5) 0.1583(5) 0.046(3) Uiso 1 d . . . H37 H 0.2767 -0.1241 0.1561 0.075(6) Uiso 1 calc R . . C38 C 0.3137(8) -0.0495(5) 0.2088(6) 0.051(3) Uiso 1 d . . . H38 H 0.2690 -0.0527 0.2430 0.075(6) Uiso 1 calc R . . C39 C 0.3735(8) -0.0025(4) 0.2090(6) 0.043(3) Uiso 1 d . . . H39 H 0.3680 0.0271 0.2430 0.075(6) Uiso 1 calc R . . C40 C 0.6586(7) -0.1326(4) 0.3132(5) 0.040(2) Uiso 1 d . . . C41 C 0.7478(6) -0.0812(4) 0.4476(4) 0.0256(19) Uiso 1 d . . . C42 C 0.8351(7) -0.0511(4) 0.4677(5) 0.038(2) Uiso 1 d . . . H42 H 0.8552 -0.0229 0.4362 0.075(6) Uiso 1 calc R . . C43 C 0.8938(8) -0.0623(4) 0.5351(6) 0.045(3) Uiso 1 d . . . H43 H 0.9534 -0.0419 0.5488 0.075(6) Uiso 1 calc R . . C44 C 0.8641(8) -0.1033(5) 0.5809(6) 0.045(3) Uiso 1 d . . . H44 H 0.9046 -0.1119 0.6254 0.075(6) Uiso 1 calc R . . C45 C 0.7749(7) -0.1321(4) 0.5619(5) 0.042(2) Uiso 1 d . . . H45 H 0.7534 -0.1590 0.5944 0.075(6) Uiso 1 calc R . . C46 C 0.7173(7) -0.1214(4) 0.4954(5) 0.035(2) Uiso 1 d . . . H46 H 0.6570 -0.1413 0.4824 0.075(6) Uiso 1 calc R . . C47 C 0.5564(6) -0.0409(4) 0.3805(5) 0.028(2) Uiso 1 d . . . C48 C 0.4775(8) -0.0770(5) 0.3791(5) 0.043(3) Uiso 1 d . . . H48 H 0.4837 -0.1163 0.3681 0.075(6) Uiso 1 calc R . . C49 C 0.3875(8) -0.0549(5) 0.3941(6) 0.050(3) Uiso 1 d . . . H49 H 0.3317 -0.0794 0.3908 0.075(6) Uiso 1 calc R . . C50 C 0.3784(8) 0.0012(4) 0.4134(5) 0.041(3) Uiso 1 d . . . H50 H 0.3179 0.0152 0.4258 0.075(6) Uiso 1 calc R . . C51 C 0.4581(7) 0.0367(4) 0.4146(5) 0.040(2) Uiso 1 d . . . H51 H 0.4516 0.0759 0.4261 0.075(6) Uiso 1 calc R . . C52 C 0.5482(7) 0.0167(4) 0.3993(5) 0.035(2) Uiso 1 d . . . H52 H 0.6033 0.0416 0.4015 0.075(6) Uiso 1 calc R . . C53S C 0.6195(10) 0.2366(6) 0.4460(7) 0.031(3) Uiso 0.65 d P . . C54S C 0.8961(11) 0.3185(6) 0.3864(7) 0.034(3) Uiso 0.65 d P . . Cl1S Cl 0.5989(2) 0.16976(14) 0.48707(18) 0.0286(8) Uani 0.65 d P . . Cl2S Cl 0.6818(3) 0.28401(18) 0.5090(2) 0.0523(12) Uani 0.65 d P . . Cl3S Cl 0.8026(2) 0.27801(13) 0.33470(16) 0.0242(7) Uani 0.65 d P . . Cl4S Cl 0.9531(3) 0.28087(17) 0.4629(2) 0.0466(10) Uani 0.65 d P . . 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 Sc 0.0211(9) 0.0230(9) 0.0265(9) 0.0022(7) 0.0051(7) 0.0004(7) P1 0.0231(12) 0.0279(13) 0.0311(13) -0.0026(10) 0.0056(10) 0.0007(10) P2 0.0247(12) 0.0232(12) 0.0278(12) 0.0009(9) 0.0060(10) -0.0027(9) P3 0.0235(12) 0.0284(13) 0.0287(12) -0.0014(10) 0.0034(10) 0.0024(10) P4 0.0306(13) 0.0249(12) 0.0288(12) 0.0026(10) 0.0078(10) -0.0008(10) O1 0.021(3) 0.033(3) 0.039(4) -0.002(3) 0.004(3) 0.005(3) O2 0.034(4) 0.030(3) 0.033(3) -0.004(3) 0.011(3) -0.003(3) O3 0.020(3) 0.037(4) 0.037(4) -0.004(3) 0.004(3) 0.004(3) O4 0.026(3) 0.044(4) 0.027(3) 0.009(3) 0.004(3) -0.001(3) O5 0.070(5) 0.060(5) 0.037(4) -0.022(4) -0.001(4) -0.004(4) O6 0.028(3) 0.041(4) 0.031(3) 0.004(3) 0.008(3) 0.002(3) O7 0.028(3) 0.033(4) 0.034(3) -0.002(3) 0.000(3) 0.001(3) O8 0.042(4) 0.046(4) 0.035(4) -0.015(3) -0.002(3) -0.005(3) O9 0.037(4) 0.030(4) 0.035(4) -0.001(3) 0.007(3) -0.004(3) O10 0.037(4) 0.032(4) 0.036(4) 0.004(3) 0.008(3) -0.003(3) O11 0.047(4) 0.044(4) 0.039(4) -0.013(3) 0.007(3) -0.016(3) O12 0.038(4) 0.052(5) 0.065(5) 0.000(4) -0.001(4) -0.004(4) O13 0.061(5) 0.061(5) 0.068(5) -0.006(4) 0.028(4) 0.021(4) Cl1S 0.0207(16) 0.0292(18) 0.0351(19) 0.0066(14) 0.0011(14) 0.0035(14) Cl2S 0.071(3) 0.052(3) 0.033(2) -0.0053(18) 0.006(2) -0.038(2) Cl3S 0.0234(17) 0.0271(17) 0.0231(16) -0.0019(13) 0.0064(13) -0.0031(13) Cl4S 0.055(3) 0.044(2) 0.036(2) 0.0023(17) -0.0089(18) 0.0096(19) _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 Sc O4 2.088(6) . ? Sc O3 2.090(6) . ? Sc O2 2.097(6) . ? Sc O1 2.099(6) . ? Sc O6 2.311(6) . ? Sc O7 2.317(6) . ? Sc O9 2.370(6) . ? Sc O10 2.425(6) . ? Sc N1 2.740(8) . ? Sc N2 2.809(7) . ? P1 O1 1.493(6) . ? P1 C1 1.782(10) . ? P1 C2 1.794(9) . ? P1 C8 1.800(9) . ? P2 O2 1.505(6) . ? P2 C14 1.798(9) . ? P2 C15 1.809(9) . ? P2 C21 1.822(9) . ? P3 O3 1.502(6) . ? P3 C28 1.786(9) . ? P3 C34 1.805(9) . ? P3 C27 1.807(10) . ? P4 O4 1.504(6) . ? P4 C41 1.782(9) . ? P4 C40 1.805(10) . ? P4 C47 1.807(9) . ? O5 N1 1.214(9) . ? O6 N1 1.277(9) . ? O7 N1 1.257(9) . ? O8 N2 1.219(9) . ? O9 N2 1.269(9) . ? O10 N2 1.261(9) . ? O11 N3 1.242(9) . ? O12 N3 1.263(10) . ? O13 N3 1.228(10) . ? C2 C3 1.393(13) . ? C2 C7 1.395(13) . ? C3 C4 1.418(14) . ? C4 C5 1.372(14) . ? C5 C6 1.388(13) . ? C6 C7 1.385(13) . ? C8 C9 1.402(13) . ? C8 C13 1.416(13) . ? C9 C10 1.387(14) . ? C10 C11 1.355(15) . ? C11 C12 1.374(15) . ? C12 C13 1.407(15) . ? C15 C16 1.398(12) . ? C15 C20 1.424(12) . ? C16 C17 1.379(13) . ? C17 C18 1.388(13) . ? C18 C19 1.380(13) . ? C19 C20 1.393(13) . ? C21 C22 1.357(12) . ? C21 C26 1.377(13) . ? C22 C23 1.372(14) . ? C23 C24 1.428(14) . ? C24 C25 1.337(14) . ? C25 C26 1.406(13) . ? C28 C29 1.378(12) . ? C28 C33 1.414(12) . ? C29 C30 1.393(14) . ? C30 C31 1.371(14) . ? C31 C32 1.388(13) . ? C32 C33 1.402(13) . ? C34 C39 1.368(13) . ? C34 C35 1.373(13) . ? C35 C36 1.369(15) . ? C36 C37 1.387(15) . ? C37 C38 1.381(15) . ? C38 C39 1.371(15) . ? C41 C42 1.393(13) . ? C41 C46 1.401(12) . ? C42 C43 1.414(14) . ? C43 C44 1.385(14) . ? C44 C45 1.396(14) . ? C45 C46 1.392(13) . ? C47 C48 1.369(13) . ? C47 C52 1.400(13) . ? C48 C49 1.403(15) . ? C49 C50 1.374(14) . ? C50 C51 1.371(14) . ? C51 C52 1.390(13) . ? C53S Cl2S 1.746(14) . ? C53S Cl1S 1.783(14) . ? C54S Cl4S 1.759(14) . ? C54S Cl3S 1.763(14) . ? 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 O4 Sc O3 92.2(2) . . ? O4 Sc O2 154.8(2) . . ? O3 Sc O2 93.5(2) . . ? O4 Sc O1 91.7(2) . . ? O3 Sc O1 154.0(2) . . ? O2 Sc O1 93.8(2) . . ? O4 Sc O6 79.3(2) . . ? O3 Sc O6 75.2(2) . . ? O2 Sc O6 78.6(2) . . ? O1 Sc O6 130.8(2) . . ? O4 Sc O7 79.1(2) . . ? O3 Sc O7 130.0(2) . . ? O2 Sc O7 78.5(2) . . ? O1 Sc O7 76.0(2) . . ? O6 Sc O7 54.8(2) . . ? O4 Sc O9 129.9(2) . . ? O3 Sc O9 79.3(2) . . ? O2 Sc O9 75.3(2) . . ? O1 Sc O9 78.5(2) . . ? O6 Sc O9 141.9(2) . . ? O7 Sc O9 141.7(2) . . ? O4 Sc O10 76.6(2) . . ? O3 Sc O10 77.8(2) . . ? O2 Sc O10 128.6(2) . . ? O1 Sc O10 78.1(2) . . ? O6 Sc O10 142.7(2) . . ? O7 Sc O10 143.6(2) . . ? O9 Sc O10 53.3(2) . . ? O4 Sc N1 78.1(2) . . ? O3 Sc N1 102.9(2) . . ? O2 Sc N1 76.7(2) . . ? O1 Sc N1 103.1(2) . . ? O6 Sc N1 27.7(2) . . ? O7 Sc N1 27.2(2) . . ? O9 Sc N1 152.0(2) . . ? O10 Sc N1 154.7(2) . . ? O4 Sc N2 103.2(2) . . ? O3 Sc N2 76.8(2) . . ? O2 Sc N2 102.0(2) . . ? O1 Sc N2 77.3(2) . . ? O6 Sc N2 151.9(2) . . ? O7 Sc N2 153.2(2) . . ? O9 Sc N2 26.7(2) . . ? O10 Sc N2 26.6(2) . . ? N1 Sc N2 178.6(2) . . ? O1 P1 C1 113.8(4) . . ? O1 P1 C2 108.3(4) . . ? C1 P1 C2 107.2(4) . . ? O1 P1 C8 110.3(4) . . ? C1 P1 C8 108.0(4) . . ? C2 P1 C8 109.0(4) . . ? O2 P2 C14 112.6(4) . . ? O2 P2 C15 109.5(4) . . ? C14 P2 C15 108.4(4) . . ? O2 P2 C21 110.0(4) . . ? C14 P2 C21 109.0(4) . . ? C15 P2 C21 107.1(4) . . ? O3 P3 C28 110.9(4) . . ? O3 P3 C34 112.9(4) . . ? C28 P3 C34 105.8(4) . . ? O3 P3 C27 111.5(4) . . ? C28 P3 C27 107.1(4) . . ? C34 P3 C27 108.3(4) . . ? O4 P4 C41 109.2(4) . . ? O4 P4 C40 111.6(4) . . ? C41 P4 C40 107.2(4) . . ? O4 P4 C47 111.9(4) . . ? C41 P4 C47 107.7(4) . . ? C40 P4 C47 109.2(4) . . ? P1 O1 Sc 162.7(4) . . ? P2 O2 Sc 159.6(4) . . ? P3 O3 Sc 161.3(4) . . ? P4 O4 Sc 162.4(4) . . ? N1 O6 Sc 95.2(5) . . ? N1 O7 Sc 95.5(5) . . ? N2 O9 Sc 96.3(5) . . ? N2 O10 Sc 93.9(5) . . ? O5 N1 O7 122.7(8) . . ? O5 N1 O6 122.9(8) . . ? O7 N1 O6 114.4(7) . . ? O5 N1 Sc 179.2(6) . . ? O7 N1 Sc 57.3(4) . . ? O6 N1 Sc 57.1(4) . . ? O8 N2 O10 123.1(8) . . ? O8 N2 O9 120.4(7) . . ? O10 N2 O9 116.5(7) . . ? O8 N2 Sc 176.7(6) . . ? O10 N2 Sc 59.5(4) . . ? O9 N2 Sc 57.0(4) . . ? O13 N3 O11 122.1(8) . . ? O13 N3 O12 119.0(8) . . ? O11 N3 O12 118.9(8) . . ? C3 C2 C7 120.3(8) . . ? C3 C2 P1 117.0(7) . . ? C7 C2 P1 122.7(7) . . ? C2 C3 C4 119.0(10) . . ? C5 C4 C3 119.6(10) . . ? C4 C5 C6 121.2(10) . . ? C7 C6 C5 119.8(9) . . ? C6 C7 C2 120.0(9) . . ? C9 C8 C13 120.1(9) . . ? C9 C8 P1 123.8(7) . . ? C13 C8 P1 116.1(7) . . ? C10 C9 C8 119.4(10) . . ? C11 C10 C9 120.4(11) . . ? C10 C11 C12 122.1(11) . . ? C11 C12 C13 119.8(11) . . ? C12 C13 C8 118.3(10) . . ? C16 C15 C20 119.6(8) . . ? C16 C15 P2 119.3(7) . . ? C20 C15 P2 120.9(6) . . ? C17 C16 C15 120.1(9) . . ? C16 C17 C18 120.3(9) . . ? C19 C18 C17 120.7(9) . . ? C18 C19 C20 120.5(9) . . ? C19 C20 C15 118.8(8) . . ? C22 C21 C26 121.0(9) . . ? C22 C21 P2 117.7(7) . . ? C26 C21 P2 121.1(7) . . ? C21 C22 C23 120.3(9) . . ? C22 C23 C24 119.2(10) . . ? C25 C24 C23 119.8(10) . . ? C24 C25 C26 120.4(10) . . ? C21 C26 C25 119.2(9) . . ? C29 C28 C33 119.5(8) . . ? C29 C28 P3 122.4(7) . . ? C33 C28 P3 117.9(7) . . ? C28 C29 C30 121.1(9) . . ? C31 C30 C29 119.5(10) . . ? C30 C31 C32 121.0(10) . . ? C31 C32 C33 119.9(9) . . ? C32 C33 C28 119.0(9) . . ? C39 C34 C35 117.4(9) . . ? C39 C34 P3 120.9(7) . . ? C35 C34 P3 121.6(7) . . ? C36 C35 C34 122.1(10) . . ? C35 C36 C37 119.3(11) . . ? C38 C37 C36 119.6(11) . . ? C39 C38 C37 119.0(11) . . ? C34 C39 C38 122.5(10) . . ? C42 C41 C46 119.6(8) . . ? C42 C41 P4 119.1(7) . . ? C46 C41 P4 121.2(7) . . ? C41 C42 C43 120.0(9) . . ? C44 C43 C42 119.8(10) . . ? C43 C44 C45 120.2(10) . . ? C46 C45 C44 120.1(10) . . ? C45 C46 C41 120.3(9) . . ? C48 C47 C52 120.5(9) . . ? C48 C47 P4 121.6(7) . . ? C52 C47 P4 117.9(7) . . ? C47 C48 C49 119.0(10) . . ? C50 C49 C48 121.4(11) . . ? C51 C50 C49 118.7(10) . . ? C50 C51 C52 121.6(10) . . ? C51 C52 C47 118.8(9) . . ? Cl2S C53S Cl1S 111.2(7) . . ? Cl4S C54S Cl3S 112.1(8) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.497 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.148 #===END #===================================================== data_G99bp003 #------------------------------------------------------------------------------ _audit_creation_date '1999-10-28' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 16.975(2) _cell_length_b 10.745(2) _cell_length_c 22.024(3) _cell_angle_alpha 90 _cell_angle_beta 105.877(8) _cell_angle_gamma 90 _cell_volume 3863.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 877.57 _chemical_formula_analytical ? _chemical_name_systematic ; tris(nitrato-O,O')bis(triphenylphosphineoxide)ethanolyttrium(III) ; _chemical_formula_sum 'C38 H36 N3 O12 P2 Y ' _chemical_formula_moiety 'C38 H36 N3 O12 P2 Y ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1800.00 _exptl_absorpt_coefficient_mu 1.661 _exptl_absorpt_correction_type multi-scan # SORTAV _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'ccd' _diffrn_measurement_device_type 'Nonius ccd' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 19560 _reflns_number_total 6286 _reflns_number_gt 1765 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.25230 _diffrn_reflns_av_sigmaI/netI 0.470 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 24.10 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 152 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Y 0 4 -2.951 3.542 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 12 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 48 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 144 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Y(1) 0.06560(14) 0.1543(2) 0.37793(13) 0.0275(8) 1.000 . Uani d ? P(1) 0.0164(4) -0.0966(7) 0.2555(4) 0.036(3) 1.000 . Uani d ? P(2) 0.2560(4) -0.0120(7) 0.4645(3) 0.033(2) 1.000 . Uani d ? O(1) 0.0320(9) 0.0135(15) 0.2993(8) 0.040(6) 1.000 . Uani d ? O(2) 0.1731(8) 0.0330(14) 0.4277(7) 0.033(6) 1.000 . Uani d ? O(3) 0.2727(9) 0.3086(15) 0.3500(8) 0.044(6) 1.000 . Uani d ? O(4) 0.1639(9) 0.1902(15) 0.3168(8) 0.044(6) 1.000 . Uani d ? O(5) 0.1757(9) 0.3016(14) 0.4002(8) 0.043(6) 1.000 . Uani d ? O(6) -0.1257(9) -0.036(2) 0.4157(8) 0.044(6) 1.000 . Uani d ? O(7) -0.0784(8) 0.1193(14) 0.3713(7) 0.030(5) 1.000 . Uani d ? O(8) 0.0057(8) -0.0142(14) 0.4272(7) 0.028(5) 1.000 . Uani d ? O(9) -0.0651(10) 0.4636(15) 0.2954(9) 0.053(7) 1.000 . Uani d ? O(10) 0.0003(8) 0.3592(14) 0.3807(9) 0.040(6) 1.000 . Uani d ? O(11) -0.0039(10) 0.2841(15) 0.2883(8) 0.046(6) 1.000 . Uani d ? O(12) 0.0784(9) 0.2102(15) 0.4855(7) 0.041(6) 1.000 . Uani d ? N(1) 0.2047(12) 0.268(2) 0.3526(10) 0.027(6) 1.000 . Uiso d ? N(2) -0.0698(13) 0.019(2) 0.4046(10) 0.035(6) 1.000 . Uiso d ? N(3) -0.0245(14) 0.375(2) 0.3204(13) 0.045(7) 1.000 . Uiso d ? C(1) -0.0874(12) -0.147(2) 0.2387(10) 0.029(6) 1.000 . Uiso d ? C(2) -0.1465(13) -0.061(2) 0.2372(12) 0.036(7) 1.000 . Uiso d ? C(3) -0.2307(14) -0.089(2) 0.2220(12) 0.044(8) 1.000 . Uiso d ? C(4) -0.250(2) -0.217(3) 0.2093(14) 0.057(9) 1.000 . Uiso d ? C(5) -0.1930(14) -0.302(2) 0.2099(12) 0.041(8) 1.000 . Uiso d ? C(6) -0.1112(13) -0.271(2) 0.2246(11) 0.024(6) 1.000 . Uiso d ? C(7) 0.0353(13) -0.063(2) 0.1813(12) 0.031(7) 1.000 . Uiso d ? C(8) 0.0185(13) -0.148(3) 0.1316(12) 0.038(7) 1.000 . Uiso d ? C(9) 0.0389(14) -0.118(3) 0.0772(12) 0.046(8) 1.000 . Uiso d ? C(10) 0.0751(13) -0.002(2) 0.0714(12) 0.037(7) 1.000 . Uiso d ? C(11) 0.0912(13) 0.086(2) 0.1184(12) 0.034(7) 1.000 . Uiso d ? C(12) 0.0705(13) 0.057(2) 0.1746(12) 0.034(7) 1.000 . Uiso d ? C(13) 0.0800(14) -0.227(2) 0.2852(12) 0.039(7) 1.000 . Uiso d ? C(14) 0.1413(14) -0.264(2) 0.2611(12) 0.033(7) 1.000 . Uiso d ? C(15) 0.1950(14) -0.354(3) 0.2912(12) 0.044(7) 1.000 . Uiso d ? C(16) 0.1868(14) -0.412(3) 0.3456(13) 0.044(8) 1.000 . Uiso d ? C(17) 0.1252(13) -0.373(2) 0.3711(11) 0.033(7) 1.000 . Uiso d ? C(18) 0.0709(13) -0.280(2) 0.3408(12) 0.033(7) 1.000 . Uiso d ? C(19) 0.3233(12) -0.030(2) 0.4147(11) 0.017(6) 1.000 . Uiso d ? C(20) 0.2898(14) -0.071(2) 0.3551(13) 0.040(8) 1.000 . Uiso d ? C(21) 0.3346(13) -0.094(2) 0.3129(12) 0.035(7) 1.000 . Uiso d ? C(22) 0.4194(13) -0.072(2) 0.3356(12) 0.029(7) 1.000 . Uiso d ? C(23) 0.4573(14) -0.024(3) 0.3922(13) 0.048(8) 1.000 . Uiso d ? C(24) 0.4072(14) -0.006(2) 0.4328(12) 0.045(8) 1.000 . Uiso d ? C(25) 0.3065(13) 0.089(2) 0.5281(12) 0.032(7) 1.000 . Uiso d ? C(26) 0.3350(14) 0.206(3) 0.5157(13) 0.044(8) 1.000 . Uiso d ? C(27) 0.3722(15) 0.287(3) 0.5637(14) 0.051(8) 1.000 . Uiso d ? C(28) 0.3790(13) 0.248(2) 0.6245(11) 0.030(7) 1.000 . Uiso d ? C(29) 0.3490(14) 0.136(3) 0.6386(12) 0.047(8) 1.000 . Uiso d ? C(30) 0.3150(14) 0.055(2) 0.5893(13) 0.036(7) 1.000 . Uiso d ? C(31) 0.2485(13) -0.163(2) 0.4998(11) 0.031(6) 1.000 . Uiso d ? C(32) 0.1735(14) -0.198(2) 0.5079(12) 0.039(8) 1.000 . Uiso d ? C(33) 0.1677(15) -0.307(3) 0.5381(13) 0.052(8) 1.000 . Uiso d ? C(34) 0.2345(14) -0.383(2) 0.5574(12) 0.040(8) 1.000 . Uiso d ? C(35) 0.3080(14) -0.353(3) 0.5479(12) 0.042(7) 1.000 . Uiso d ? C(36) 0.3154(14) -0.238(3) 0.5162(12) 0.043(8) 1.000 . Uiso d ? C(37) 0.113(2) 0.325(3) 0.5191(14) 0.067(9) 1.000 . Uiso d ? C(38) 0.077(2) 0.348(3) 0.5707(14) 0.069(9) 1.000 . Uiso d ? H(1) -0.1301 0.0225 0.2469 0.043 1.000 . Uiso c ? H(2) -0.2714 -0.0275 0.2204 0.053 1.000 . Uiso c ? H(3) -0.3055 -0.2420 0.2000 0.068 1.000 . Uiso c ? H(4) -0.2090 -0.3856 0.1998 0.050 1.000 . Uiso c ? H(5) -0.0712 -0.3328 0.2253 0.029 1.000 . Uiso c ? H(6) -0.0067 -0.2258 0.1352 0.046 1.000 . Uiso c ? H(7) 0.0286 -0.1750 0.0431 0.056 1.000 . Uiso c ? H(8) 0.0889 0.0160 0.0334 0.044 1.000 . Uiso c ? H(9) 0.1155 0.1632 0.1132 0.041 1.000 . Uiso c ? H(10) 0.0797 0.1161 0.2079 0.040 1.000 . Uiso c ? H(11) 0.1472 -0.2273 0.2234 0.040 1.000 . Uiso c ? H(12) 0.2389 -0.3775 0.2745 0.053 1.000 . Uiso c ? H(13) 0.2227 -0.4776 0.3647 0.053 1.000 . Uiso c ? H(14) 0.1199 -0.4083 0.4093 0.040 1.000 . Uiso c ? H(15) 0.0282 -0.2527 0.3578 0.039 1.000 . Uiso c ? H(16) 0.2323 -0.0843 0.3417 0.047 1.000 . Uiso c ? H(17) 0.3101 -0.1227 0.2713 0.042 1.000 . Uiso c ? H(18) 0.4524 -0.0920 0.3084 0.035 1.000 . Uiso c ? H(19) 0.5140 -0.0044 0.4041 0.058 1.000 . Uiso c ? H(20) 0.4316 0.0234 0.4743 0.055 1.000 . Uiso c ? H(21) 0.3286 0.2303 0.4731 0.053 1.000 . Uiso c ? H(22) 0.3922 0.3661 0.5553 0.062 1.000 . Uiso c ? H(23) 0.4056 0.3009 0.6584 0.036 1.000 . Uiso c ? H(24) 0.3516 0.1141 0.6809 0.056 1.000 . Uiso c ? H(25) 0.2974 -0.0257 0.5982 0.043 1.000 . Uiso c ? H(26) 0.1267 -0.1468 0.4926 0.047 1.000 . Uiso c ? H(27) 0.1172 -0.3300 0.5457 0.062 1.000 . Uiso c ? H(28) 0.2294 -0.4591 0.5781 0.048 1.000 . Uiso c ? H(29) 0.3537 -0.4074 0.5618 0.050 1.000 . Uiso c ? H(30) 0.3651 -0.2157 0.5072 0.052 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Y(1) 0.0244(13) 0.0268(15) 0.034(2) -0.001(2) 0.0126(12) 0.002(2) P(1) 0.032(4) 0.042(5) 0.038(6) -0.005(4) 0.016(4) 0.002(4) P(2) 0.023(4) 0.040(5) 0.037(5) -0.001(4) 0.008(4) 0.002(4) O(1) 0.046(10) 0.047(13) 0.037(13) 0.000(10) 0.027(10) -0.006(11) O(2) 0.027(9) 0.036(11) 0.033(12) 0.000(9) 0.005(9) 0.006(10) O(3) 0.022(9) 0.059(14) 0.052(14) -0.012(9) 0.015(9) 0.002(10) O(4) 0.042(10) 0.041(13) 0.054(14) -0.031(10) 0.024(10) -0.020(10) O(5) 0.046(11) 0.039(12) 0.042(14) -0.003(10) 0.011(10) -0.001(10) O(6) 0.021(9) 0.056(13) 0.057(14) 0.005(10) 0.017(10) -0.001(11) O(7) 0.025(9) 0.038(12) 0.030(11) -0.005(9) 0.013(8) 0.014(10) O(8) 0.023(9) 0.050(13) 0.010(11) -0.007(9) 0.000(8) 0.010(9) O(9) 0.074(13) 0.026(12) 0.049(14) 0.035(11) 0.003(11) 0.003(11) O(10) 0.025(9) 0.017(11) 0.073(15) 0.011(9) 0.006(10) 0.023(11) O(11) 0.069(13) 0.031(12) 0.039(13) -0.003(11) 0.014(11) 0.009(10) O(12) 0.043(10) 0.039(12) 0.040(13) -0.002(10) 0.008(10) -0.021(10) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1765 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0969 _refine_ls_wR_factor_all 0.0954 _refine_ls_wR_factor_ref 0.0954 _refine_ls_goodness_of_fit_all 1.361 _refine_ls_goodness_of_fit_ref 1.361 _refine_ls_shift/su_max 0.0290 _refine_ls_shift/su_mean 0.0060 _refine_diff_density_min -0.76 _refine_diff_density_max 0.78 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y(1) O(1) 2.25(2) . . yes Y(1) O(2) 2.266(15) . . yes Y(1) O(4) 2.444(14) . . yes Y(1) O(5) 2.394(15) . . yes Y(1) O(7) 2.438(13) . . yes Y(1) O(8) 2.469(14) . . yes Y(1) O(10) 2.473(15) . . yes Y(1) O(11) 2.44(2) . . yes Y(1) O(12) 2.40(2) . . yes P(1) O(1) 1.50(2) . . yes P(1) C(1) 1.78(2) . . yes P(1) C(7) 1.79(2) . . yes P(1) C(13) 1.78(3) . . yes P(2) O(2) 1.500(15) . . yes P(2) C(19) 1.80(2) . . yes P(2) C(25) 1.80(3) . . yes P(2) C(31) 1.82(2) . . yes O(3) N(1) 1.25(2) . . yes O(4) N(1) 1.22(2) . . yes O(5) N(1) 1.33(2) . . yes O(6) N(2) 1.20(2) . . yes O(7) N(2) 1.29(2) . . yes O(8) N(2) 1.29(2) . . yes O(9) N(3) 1.21(2) . . yes O(10) N(3) 1.29(2) . . yes O(11) N(3) 1.31(2) . . yes O(12) C(37) 1.47(3) . . yes C(1) C(2) 1.36(3) . . yes C(1) C(6) 1.39(3) . . yes C(2) C(3) 1.41(3) . . yes C(2) H(1) 0.95 . . no C(3) C(4) 1.42(3) . . yes C(3) H(2) 0.95 . . no C(4) C(5) 1.33(3) . . yes C(4) H(3) 0.95 . . no C(5) C(6) 1.38(3) . . yes C(5) H(4) 0.95 . . no C(6) H(5) 0.95 . . no C(7) C(8) 1.40(3) . . yes C(7) C(12) 1.44(3) . . yes C(8) C(9) 1.38(3) . . yes C(8) H(6) 0.95 . . no C(9) C(10) 1.40(3) . . yes C(9) H(7) 0.95 . . no C(10) C(11) 1.37(3) . . yes C(10) H(8) 0.95 . . no C(11) C(12) 1.41(3) . . yes C(11) H(9) 0.95 . . no C(12) H(10) 0.95 . . no C(13) C(14) 1.35(3) . . yes C(13) C(18) 1.39(3) . . yes C(14) C(15) 1.37(3) . . yes C(14) H(11) 0.95 . . no C(15) C(16) 1.39(3) . . yes C(15) H(12) 0.95 . . no C(16) C(17) 1.38(3) . . yes C(16) H(13) 0.95 . . no C(17) C(18) 1.40(3) . . yes C(17) H(14) 0.95 . . no C(18) H(15) 0.95 . . no C(19) C(20) 1.35(3) . . yes C(19) C(24) 1.39(3) . . yes C(20) C(21) 1.38(3) . . yes C(20) H(16) 0.95 . . no C(21) C(22) 1.41(3) . . yes C(21) H(17) 0.95 . . no C(22) C(23) 1.34(3) . . yes C(22) H(18) 0.95 . . no C(23) C(24) 1.40(3) . . yes C(23) H(19) 0.95 . . no C(24) H(20) 0.95 . . no C(25) C(26) 1.40(3) . . yes C(25) C(30) 1.37(3) . . yes C(26) C(27) 1.38(3) . . yes C(26) H(21) 0.95 . . no C(27) C(28) 1.38(3) . . yes C(27) H(22) 0.95 . . no C(28) C(29) 1.38(3) . . yes C(28) H(23) 0.95 . . no C(29) C(30) 1.39(3) . . yes C(29) H(24) 0.95 . . no C(30) H(25) 0.95 . . no C(31) C(32) 1.39(3) . . yes C(31) C(36) 1.36(3) . . yes C(32) C(33) 1.36(3) . . yes C(32) H(26) 0.95 . . no C(33) C(34) 1.37(3) . . yes C(33) H(27) 0.95 . . no C(34) C(35) 1.36(3) . . yes C(34) H(28) 0.95 . . no C(35) C(36) 1.44(3) . . yes C(35) H(29) 0.95 . . no C(36) H(30) 0.95 . . no C(37) C(38) 1.46(3) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Y(1) O(2) 89.2(6) . . . yes O(1) Y(1) O(4) 75.5(5) . . . yes O(1) Y(1) O(5) 128.3(6) . . . yes O(1) Y(1) O(7) 79.2(5) . . . yes O(1) Y(1) O(8) 78.3(5) . . . yes O(1) Y(1) O(10) 126.6(6) . . . yes O(1) Y(1) O(11) 78.3(6) . . . yes O(1) Y(1) O(12) 149.8(6) . . . yes O(2) Y(1) O(4) 77.1(5) . . . yes O(2) Y(1) O(5) 78.5(5) . . . yes O(2) Y(1) O(7) 127.0(5) . . . yes O(2) Y(1) O(8) 74.9(5) . . . yes O(2) Y(1) O(10) 143.8(6) . . . yes O(2) Y(1) O(11) 150.1(5) . . . yes O(2) Y(1) O(12) 79.8(5) . . . yes O(4) Y(1) O(5) 52.9(6) . . . yes O(4) Y(1) O(7) 144.7(5) . . . yes O(4) Y(1) O(8) 141.6(5) . . . yes O(4) Y(1) O(10) 104.6(5) . . . yes O(4) Y(1) O(11) 73.5(6) . . . yes O(4) Y(1) O(12) 127.9(5) . . . yes O(5) Y(1) O(7) 145.9(5) . . . yes O(5) Y(1) O(8) 141.9(5) . . . yes O(5) Y(1) O(10) 74.7(5) . . . yes O(5) Y(1) O(11) 88.0(5) . . . yes O(5) Y(1) O(12) 77.2(6) . . . yes O(7) Y(1) O(8) 52.1(5) . . . yes O(7) Y(1) O(10) 72.0(5) . . . yes O(7) Y(1) O(11) 77.6(5) . . . yes O(7) Y(1) O(12) 85.2(5) . . . yes O(8) Y(1) O(10) 113.6(5) . . . yes O(8) Y(1) O(11) 127.5(5) . . . yes O(8) Y(1) O(12) 71.7(5) . . . yes O(10) Y(1) O(11) 52.5(6) . . . yes O(10) Y(1) O(12) 70.9(6) . . . yes O(11) Y(1) O(12) 123.3(6) . . . yes O(1) P(1) C(1) 111.3(10) . . . yes O(1) P(1) C(7) 112.5(11) . . . yes O(1) P(1) C(13) 113.7(11) . . . yes C(1) P(1) C(7) 106.7(11) . . . yes C(1) P(1) C(13) 107.4(12) . . . yes C(7) P(1) C(13) 104.7(11) . . . yes O(2) P(2) C(19) 111.2(10) . . . yes O(2) P(2) C(25) 113.8(11) . . . yes O(2) P(2) C(31) 110.8(10) . . . yes C(19) P(2) C(25) 106.9(10) . . . yes C(19) P(2) C(31) 107.3(10) . . . yes C(25) P(2) C(31) 106.4(12) . . . yes Y(1) O(1) P(1) 170.0(11) . . . yes Y(1) O(2) P(2) 163.7(10) . . . yes Y(1) O(4) N(1) 96.0(14) . . . yes Y(1) O(5) N(1) 95.4(14) . . . yes Y(1) O(7) N(2) 98.0(13) . . . yes Y(1) O(8) N(2) 96.3(13) . . . yes Y(1) O(10) N(3) 96.7(16) . . . yes Y(1) O(11) N(3) 97.6(15) . . . yes Y(1) O(12) C(37) 128.3(15) . . . yes O(3) N(1) O(4) 125.2(22) . . . yes O(3) N(1) O(5) 119.1(21) . . . yes O(4) N(1) O(5) 115.5(20) . . . yes O(6) N(2) O(7) 123.9(21) . . . yes O(6) N(2) O(8) 122.6(22) . . . yes O(7) N(2) O(8) 113.5(20) . . . yes O(9) N(3) O(10) 123.9(25) . . . yes O(9) N(3) O(11) 122.9(26) . . . yes O(10) N(3) O(11) 113.2(23) . . . yes P(1) C(1) C(2) 118.7(19) . . . yes P(1) C(1) C(6) 123.0(17) . . . yes C(2) C(1) C(6) 118.3(21) . . . yes C(1) C(2) C(3) 123.8(23) . . . yes C(1) C(2) H(1) 118.1 . . . no C(3) C(2) H(1) 118.1 . . . no C(2) C(3) C(4) 114.5(24) . . . yes C(2) C(3) H(2) 122.7 . . . no C(4) C(3) H(2) 122.7 . . . no C(3) C(4) C(5) 122.5(25) . . . yes C(3) C(4) H(3) 118.8 . . . no C(5) C(4) H(3) 118.7 . . . no C(4) C(5) C(6) 121.2(24) . . . yes C(4) C(5) H(4) 119.4 . . . no C(6) C(5) H(4) 119.3 . . . no C(1) C(6) C(5) 119.6(21) . . . yes C(1) C(6) H(5) 120.2 . . . no C(5) C(6) H(5) 120.2 . . . no P(1) C(7) C(8) 122.3(19) . . . yes P(1) C(7) C(12) 117.2(19) . . . yes C(8) C(7) C(12) 120.5(23) . . . yes C(7) C(8) C(9) 118.6(25) . . . yes C(7) C(8) H(6) 120.7 . . . no C(9) C(8) H(6) 120.7 . . . no C(8) C(9) C(10) 120.7(25) . . . yes C(8) C(9) H(7) 119.6 . . . no C(10) C(9) H(7) 119.6 . . . no C(9) C(10) C(11) 122.8(24) . . . yes C(9) C(10) H(8) 118.7 . . . no C(11) C(10) H(8) 118.6 . . . no C(10) C(11) C(12) 117.7(23) . . . yes C(10) C(11) H(9) 121.2 . . . no C(12) C(11) H(9) 121.1 . . . no C(7) C(12) C(11) 119.6(23) . . . yes C(7) C(12) H(10) 120.2 . . . no C(11) C(12) H(10) 120.2 . . . no P(1) C(13) C(14) 122.6(21) . . . yes P(1) C(13) C(18) 116.1(18) . . . yes C(14) C(13) C(18) 120.7(24) . . . yes C(13) C(14) C(15) 119.9(24) . . . yes C(13) C(14) H(11) 120.1 . . . no C(15) C(14) H(11) 120.0 . . . no C(14) C(15) C(16) 121.5(22) . . . yes C(14) C(15) H(12) 119.2 . . . no C(16) C(15) H(12) 119.2 . . . no C(15) C(16) C(17) 118.5(24) . . . yes C(15) C(16) H(13) 120.7 . . . no C(17) C(16) H(13) 120.8 . . . no C(16) C(17) C(18) 119.8(24) . . . yes C(16) C(17) H(14) 120.1 . . . no C(18) C(17) H(14) 120.1 . . . no C(13) C(18) C(17) 119.4(21) . . . yes C(13) C(18) H(15) 120.3 . . . no C(17) C(18) H(15) 120.3 . . . no P(2) C(19) C(20) 117.2(17) . . . yes P(2) C(19) C(24) 125.3(19) . . . yes C(20) C(19) C(24) 117.4(21) . . . yes C(19) C(20) C(21) 123.4(22) . . . yes C(19) C(20) H(16) 118.3 . . . no C(21) C(20) H(16) 118.3 . . . no C(20) C(21) C(22) 115.5(23) . . . yes C(20) C(21) H(17) 122.3 . . . no C(22) C(21) H(17) 122.2 . . . no C(21) C(22) C(23) 125.4(23) . . . yes C(21) C(22) H(18) 117.3 . . . no C(23) C(22) H(18) 117.3 . . . no C(22) C(23) C(24) 115.2(23) . . . yes C(22) C(23) H(19) 122.4 . . . no C(24) C(23) H(19) 122.5 . . . no C(19) C(24) C(23) 122.9(25) . . . yes C(19) C(24) H(20) 118.5 . . . no C(23) C(24) H(20) 118.5 . . . no P(2) C(25) C(26) 120.6(20) . . . yes P(2) C(25) C(30) 120.1(21) . . . yes C(26) C(25) C(30) 119.3(25) . . . yes C(25) C(26) C(27) 121.7(26) . . . yes C(25) C(26) H(21) 119.1 . . . no C(27) C(26) H(21) 119.1 . . . no C(26) C(27) C(28) 116.7(25) . . . yes C(26) C(27) H(22) 121.7 . . . no C(28) C(27) H(22) 121.7 . . . no C(27) C(28) C(29) 123.3(24) . . . yes C(27) C(28) H(23) 118.3 . . . no C(29) C(28) H(23) 118.3 . . . no C(28) C(29) C(30) 118.3(25) . . . yes C(28) C(29) H(24) 120.8 . . . no C(30) C(29) H(24) 120.9 . . . no C(25) C(30) C(29) 120.5(25) . . . yes C(25) C(30) H(25) 119.7 . . . no C(29) C(30) H(25) 119.7 . . . no P(2) C(31) C(32) 118.1(19) . . . yes P(2) C(31) C(36) 119.6(17) . . . yes C(32) C(31) C(36) 122.3(24) . . . yes C(31) C(32) C(33) 119.3(24) . . . yes C(31) C(32) H(26) 120.3 . . . no C(33) C(32) H(26) 120.4 . . . no C(32) C(33) C(34) 120.0(23) . . . yes C(32) C(33) H(27) 120.0 . . . no C(34) C(33) H(27) 120.0 . . . no C(33) C(34) C(35) 121.9(24) . . . yes C(33) C(34) H(28) 119.0 . . . no C(35) C(34) H(28) 119.1 . . . no C(34) C(35) C(36) 118.8(24) . . . yes C(34) C(35) H(29) 120.6 . . . no C(36) C(35) H(29) 120.6 . . . no C(31) C(36) C(35) 117.5(21) . . . yes C(31) C(36) H(30) 121.2 . . . no C(35) C(36) H(30) 121.2 . . . no O(12) C(37) C(38) 109.4(23) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(3) C(9) 3.26(3) . 2 no O(3) C(14) 3.27(3) . 2 no O(3) C(16) 3.33(3) . 1_565 no O(3) C(10) 3.37(3) . 2 no O(3) C(8) 3.49(3) . 2 no O(5) C(16) 3.33(3) . 1_565 no O(6) O(12) 2.81(2) . 3_556 no O(6) C(30) 3.19(3) . 3_556 no O(6) C(32) 3.25(3) . 3_556 no O(6) C(37) 3.40(3) . 3_556 no O(6) C(38) 3.44(4) . 3_556 no O(6) O(8) 3.54(2) . 3_556 no O(7) C(4) 3.45(3) . 2_455 no O(7) C(33) 3.46(3) . 3_556 no O(7) C(32) 3.57(3) . 3_556 no O(8) O(8) 3.28(3) . 3_556 no O(8) O(12) 3.42(2) . 3_556 no O(8) N(2) 3.56(3) . 3_556 no O(9) C(6) 3.24(3) . 1_565 no O(9) C(3) 3.43(3) . 2_455 no O(9) C(5) 3.52(3) . 1_565 no O(9) C(29) 3.53(3) . 4_454 no O(9) C(18) 3.56(3) . 1_565 no O(12) N(2) 3.49(3) . 3_556 no N(1) C(16) 3.45(3) . 1_565 no N(2) C(32) 3.52(3) . 3_556 no C(3) C(34) 3.52(4) . 4_444 no C(4) C(34) 3.45(4) . 4_444 no C(8) C(35) 3.54(3) . 4_444 no C(9) C(10) 3.56(4) . 3 no C(10) C(10) 3.47(5) . 3 no C(15) C(21) 3.39(4) . 2_545 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Y(1) O(1) P(1) C(1) . . . . 102.1(55) no Y(1) O(1) P(1) C(7) . . . . -138.2(52) no Y(1) O(1) P(1) C(13) . . . . -19.4(58) no Y(1) O(2) P(2) C(19) . . . . -85.5(37) no Y(1) O(2) P(2) C(25) . . . . 35.4(39) no Y(1) O(2) P(2) C(31) . . . . 155.3(33) no Y(1) O(4) N(1) O(3) . . . . 169.2(19) no Y(1) O(4) N(1) O(5) . . . . -5.3(20) no Y(1) O(5) N(1) O(3) . . . . -169.5(17) no Y(1) O(5) N(1) O(4) . . . . 5.4(20) no Y(1) O(7) N(2) O(6) . . . . 179.8(20) no Y(1) O(7) N(2) O(8) . . . . 2.1(20) no Y(1) O(8) N(2) O(6) . . . . -179.8(20) no Y(1) O(8) N(2) O(7) . . . . -2.1(20) no Y(1) O(10) N(3) O(9) . . . . 176.6(21) no Y(1) O(10) N(3) O(11) . . . . -1.1(19) no Y(1) O(11) N(3) O(9) . . . . -176.6(20) no Y(1) O(11) N(3) O(10) . . . . 1.1(20) no Y(1) O(12) C(37) C(38) . . . . 153.9(18) no P(1) O(1) Y(1) O(2) . . . . 28.5(55) no P(1) O(1) Y(1) O(4) . . . . 105.4(55) no P(1) O(1) Y(1) O(5) . . . . 103.2(54) no P(1) O(1) Y(1) O(7) . . . . -99.4(55) no P(1) O(1) Y(1) O(8) . . . . -46.2(54) no P(1) O(1) Y(1) O(10) . . . . -157.1(52) no P(1) O(1) Y(1) O(11) . . . . -178.8(55) no P(1) O(1) Y(1) O(12) . . . . -39.4(60) no P(1) C(1) C(2) C(3) . . . . 177.4(20) no P(1) C(1) C(6) C(5) . . . . -177.6(18) no P(1) C(7) C(8) C(9) . . . . -176.6(18) no P(1) C(7) C(12) C(11) . . . . 176.3(17) no P(1) C(13) C(14) C(15) . . . . 171.1(19) no P(1) C(13) C(18) C(17) . . . . -172.3(18) no P(2) O(2) Y(1) O(1) . . . . 140.0(36) no P(2) O(2) Y(1) O(4) . . . . 64.7(35) no P(2) O(2) Y(1) O(5) . . . . 10.5(35) no P(2) O(2) Y(1) O(7) . . . . -144.3(33) no P(2) O(2) Y(1) O(8) . . . . -141.9(36) no P(2) O(2) Y(1) O(10) . . . . -32.4(40) no P(2) O(2) Y(1) O(11) . . . . 75.4(39) no P(2) O(2) Y(1) O(12) . . . . -68.3(35) no P(2) C(19) C(20) C(21) . . . . -176.8(21) no P(2) C(19) C(24) C(23) . . . . 178.4(20) no P(2) C(25) C(26) C(27) . . . . 178.3(19) no P(2) C(25) C(30) C(29) . . . . -175.7(18) no P(2) C(31) C(32) C(33) . . . . -175.5(20) no P(2) C(31) C(36) C(35) . . . . 175.9(19) no O(1) Y(1) O(4) N(1) . . . . -174.5(14) no O(1) Y(1) O(5) N(1) . . . . -0.5(15) no O(1) Y(1) O(7) N(2) . . . . 82.3(13) no O(1) Y(1) O(8) N(2) . . . . -84.0(13) no O(1) Y(1) O(10) N(3) . . . . -26.6(14) no O(1) Y(1) O(11) N(3) . . . . 157.3(13) no O(1) Y(1) O(12) C(37) . . . . 174.2(16) no O(1) P(1) C(1) C(2) . . . . 31.8(22) no O(1) P(1) C(1) C(6) . . . . -150.7(19) no O(1) P(1) C(7) C(8) . . . . -174.7(18) no O(1) P(1) C(7) C(12) . . . . 6.3(20) no O(1) P(1) C(13) C(14) . . . . -108.6(22) no O(1) P(1) C(13) C(18) . . . . 62.5(22) no O(2) Y(1) O(4) N(1) . . . . -82.0(13) no O(2) Y(1) O(5) N(1) . . . . 79.3(12) no O(2) Y(1) O(7) N(2) . . . . 1.6(16) no O(2) Y(1) O(8) N(2) . . . . -176.3(14) no O(2) Y(1) O(10) N(3) . . . . 143.9(12) no O(2) Y(1) O(11) N(3) . . . . -135.6(13) no O(2) Y(1) O(12) C(37) . . . . 103.9(18) no O(2) P(2) C(19) C(20) . . . . -36.2(22) no O(2) P(2) C(19) C(24) . . . . 144.8(21) no O(2) P(2) C(25) C(26) . . . . -69.4(20) no O(2) P(2) C(25) C(30) . . . . 108.4(20) no O(2) P(2) C(31) C(32) . . . . -21.2(22) no O(2) P(2) C(31) C(36) . . . . 157.7(19) no O(4) Y(1) O(5) N(1) . . . . -3.1(11) no O(4) Y(1) O(7) N(2) . . . . 126.9(13) no O(4) Y(1) O(8) N(2) . . . . -131.8(13) no O(4) Y(1) O(10) N(3) . . . . 56.0(13) no O(4) Y(1) O(11) N(3) . . . . -124.6(13) no O(4) Y(1) O(12) C(37) . . . . 39.2(20) no O(5) Y(1) O(4) N(1) . . . . 3.3(12) no O(5) Y(1) O(7) N(2) . . . . -130.3(14) no O(5) Y(1) O(8) N(2) . . . . 136.3(13) no O(5) Y(1) O(10) N(3) . . . . 100.2(13) no O(5) Y(1) O(11) N(3) . . . . -72.9(13) no O(5) Y(1) O(12) C(37) . . . . 23.4(18) no O(7) Y(1) O(4) N(1) . . . . 140.0(13) no O(7) Y(1) O(5) N(1) . . . . -138.1(12) no O(7) Y(1) O(8) N(2) . . . . 1.3(12) no O(7) Y(1) O(10) N(3) . . . . -87.3(13) no O(7) Y(1) O(11) N(3) . . . . 76.0(13) no O(7) Y(1) O(12) C(37) . . . . -127.2(18) no O(8) Y(1) O(4) N(1) . . . . -126.0(13) no O(8) Y(1) O(5) N(1) . . . . 125.7(12) no O(8) Y(1) O(7) N(2) . . . . -1.3(12) no O(8) Y(1) O(10) N(3) . . . . -119.4(12) no O(8) Y(1) O(11) N(3) . . . . 92.0(13) no O(8) Y(1) O(12) C(37) . . . . -178.8(18) no O(10) Y(1) O(4) N(1) . . . . 60.8(14) no O(10) Y(1) O(5) N(1) . . . . -125.4(13) no O(10) Y(1) O(7) N(2) . . . . -143.2(14) no O(10) Y(1) O(8) N(2) . . . . 41.1(14) no O(10) Y(1) O(11) N(3) . . . . -0.7(12) no O(10) Y(1) O(12) C(37) . . . . -54.6(18) no O(11) Y(1) O(4) N(1) . . . . 103.6(14) no O(11) Y(1) O(5) N(1) . . . . -73.9(12) no O(11) Y(1) O(7) N(2) . . . . 162.5(14) no O(11) Y(1) O(8) N(2) . . . . -18.7(15) no O(11) Y(1) O(10) N(3) . . . . 0.7(12) no O(11) Y(1) O(12) C(37) . . . . -55.5(19) no O(12) Y(1) O(4) N(1) . . . . -16.1(16) no O(12) Y(1) O(5) N(1) . . . . 161.3(12) no O(12) Y(1) O(7) N(2) . . . . -71.8(13) no O(12) Y(1) O(8) N(2) . . . . 99.6(13) no O(12) Y(1) O(10) N(3) . . . . -178.4(13) no O(12) Y(1) O(11) N(3) . . . . 0.3(15) no C(1) P(1) C(7) C(8) . . . . -52.3(22) no C(1) P(1) C(7) C(12) . . . . 128.7(18) no C(1) P(1) C(13) C(14) . . . . 127.8(22) no C(1) P(1) C(13) C(18) . . . . -61.2(22) no C(1) C(2) C(3) C(4) . . . . 1.2(40) no C(1) C(6) C(5) C(4) . . . . -0.6(39) no C(2) C(1) P(1) C(7) . . . . -91.3(21) no C(2) C(1) P(1) C(13) . . . . 156.8(20) no C(2) C(1) C(6) C(5) . . . . 0.0(35) no C(2) C(3) C(4) C(5) . . . . -1.9(43) no C(3) C(2) C(1) C(6) . . . . -0.3(38) no C(3) C(4) C(5) C(6) . . . . 1.7(45) no C(6) C(1) P(1) C(7) . . . . 86.3(22) no C(6) C(1) P(1) C(13) . . . . -25.6(23) no C(7) P(1) C(13) C(14) . . . . 14.6(24) no C(7) P(1) C(13) C(18) . . . . -174.3(20) no C(7) C(8) C(9) C(10) . . . . -0.8(36) no C(7) C(12) C(11) C(10) . . . . 1.4(34) no C(8) C(7) P(1) C(13) . . . . 61.4(21) no C(8) C(7) C(12) C(11) . . . . -2.8(34) no C(8) C(9) C(10) C(11) . . . . -0.6(38) no C(9) C(8) C(7) C(12) . . . . 2.4(35) no C(9) C(10) C(11) C(12) . . . . 0.3(37) no C(12) C(7) P(1) C(13) . . . . -117.6(18) no C(13) C(14) C(15) C(16) . . . . 1.8(39) no C(13) C(18) C(17) C(16) . . . . -0.6(37) no C(14) C(13) C(18) C(17) . . . . -1.0(38) no C(14) C(15) C(16) C(17) . . . . -3.3(40) no C(15) C(14) C(13) C(18) . . . . 0.4(39) no C(15) C(16) C(17) C(18) . . . . 2.6(38) no C(19) P(2) C(25) C(26) . . . . 53.9(21) no C(19) P(2) C(25) C(30) . . . . -128.4(19) no C(19) P(2) C(31) C(32) . . . . -142.7(19) no C(19) P(2) C(31) C(36) . . . . 36.2(24) no C(19) C(20) C(21) C(22) . . . . -0.2(40) no C(19) C(24) C(23) C(22) . . . . -3.1(42) no C(20) C(19) P(2) C(25) . . . . -161.1(19) no C(20) C(19) P(2) C(31) . . . . 85.1(21) no C(20) C(19) C(24) C(23) . . . . -0.5(40) no C(20) C(21) C(22) C(23) . . . . -4.0(41) no C(21) C(20) C(19) C(24) . . . . 2.2(39) no C(21) C(22) C(23) C(24) . . . . 5.4(42) no C(24) C(19) P(2) C(25) . . . . 20.0(24) no C(24) C(19) P(2) C(31) . . . . -93.9(22) no C(25) P(2) C(31) C(32) . . . . 103.1(20) no C(25) P(2) C(31) C(36) . . . . -78.0(22) no C(25) C(26) C(27) C(28) . . . . -0.7(37) no C(25) C(30) C(29) C(28) . . . . -4.4(36) no C(26) C(25) P(2) C(31) . . . . 168.3(18) no C(26) C(25) C(30) C(29) . . . . 2.1(35) no C(26) C(27) C(28) C(29) . . . . -1.7(36) no C(27) C(26) C(25) C(30) . . . . 0.5(36) no C(27) C(28) C(29) C(30) . . . . 4.3(36) no C(30) C(25) P(2) C(31) . . . . -13.9(22) no C(31) C(32) C(33) C(34) . . . . -3.1(40) no C(31) C(36) C(35) C(34) . . . . 2.6(38) no C(32) C(31) C(36) C(35) . . . . -5.2(38) no C(32) C(33) C(34) C(35) . . . . 0.6(42) no C(33) C(32) C(31) C(36) . . . . 5.6(39) no C(33) C(34) C(35) C(36) . . . . -0.3(40) no #===END #===================================================== data_Ilev99_11 #------------------------------------------------------------------------------ _audit_creation_date '2000-02-04' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 14.578(10) _cell_length_b 15.39(2) _cell_length_c 10.57(2) _cell_angle_alpha 100.0(1) _cell_angle_beta 93.0(1) _cell_angle_gamma 96.91(9) _cell_volume 2312(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 24.9 _cell_measurement_theta_max 25.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.90 _exptl_crystal_size_min 0.70 _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 551.15 _chemical_formula_analytical ? _chemical_name_systematic ; tris(nitrato-O,O')tris(trimethylphosphineoxide)yttrium(III) ; _chemical_formula_sum 'C9 H27 N3 O12 P3 Y ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1128.00 _exptl_absorpt_coefficient_mu 2.794 _exptl_absorpt_correction_type empirical # psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.478 _exptl_special_details ; The scan width was (1.42+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.03 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -2 -3 4 3 -2 5 2 -1 _diffrn_reflns_number 8495 _reflns_number_total 8145 _reflns_number_gt 5513 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.09279 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.05560 _diffrn_orient_matrix_UB_12 0.03700 _diffrn_orient_matrix_UB_13 -0.02322 _diffrn_orient_matrix_UB_21 0.04047 _diffrn_orient_matrix_UB_22 -0.02548 _diffrn_orient_matrix_UB_23 0.05956 _diffrn_orient_matrix_UB_31 0.00854 _diffrn_orient_matrix_UB_32 -0.04908 _diffrn_orient_matrix_UB_33 -0.07211 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 36 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 108 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 12 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 48 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 12 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Y 0 4 -2.951 3.542 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Y(1) 0.29957(7) 0.73567(7) 0.0247(1) 0.0214(3) 1.000 . Uani d ? Y(2) 0.20171(7) 0.22621(7) 0.4756(1) 0.0210(3) 1.000 . Uani d ? P(1) 0.1054(2) 0.8367(2) 0.1712(3) 0.025(1) 1.000 . Uani d ? P(2) 0.1460(2) 0.7180(2) -0.2544(3) 0.027(1) 1.000 . Uani d ? P(3) 0.1947(2) 0.5283(2) 0.1016(3) 0.027(1) 1.000 . Uani d ? P(4) 0.3580(2) 0.4173(2) 0.6478(3) 0.031(1) 1.000 . Uani d ? P(5) 0.3983(2) 0.1425(2) 0.3241(3) 0.024(1) 1.000 . Uani d ? P(6) 0.2695(2) 0.1096(2) 0.7243(3) 0.0260(9) 1.000 . Uani d ? O(1) 0.1605(4) 0.7763(4) 0.0845(6) 0.021(2) 1.000 . Uani d ? O(2) 0.2357(4) 0.7139(5) -0.1817(7) 0.027(2) 1.000 . Uani d ? O(3) 0.2269(5) 0.5972(5) 0.0237(7) 0.027(2) 1.000 . Uani d ? O(4) 0.3217(4) 0.3329(5) 0.5565(7) 0.029(2) 1.000 . Uani d ? O(5) 0.3171(4) 0.1494(5) 0.4063(7) 0.024(2) 1.000 . Uani d ? O(6) 0.2205(4) 0.1727(4) 0.6599(7) 0.026(2) 1.000 . Uani d ? O(7) 0.5299(6) 0.6113(6) -0.0528(9) 0.072(4) 1.000 . Uani d ? O(8) 0.3954(5) 0.6427(5) -0.1164(8) 0.034(3) 1.000 . Uani d ? O(9) 0.4448(5) 0.6829(5) 0.0820(8) 0.037(3) 1.000 . Uani d ? O(10) 0.3844(6) 0.8147(6) 0.4099(8) 0.060(3) 1.000 . Uani d ? O(11) 0.3081(5) 0.7149(5) 0.2562(7) 0.034(3) 1.000 . Uani d ? O(12) 0.3696(5) 0.8420(5) 0.2153(7) 0.032(3) 1.000 . Uani d ? O(13) 0.4043(5) 0.9611(5) -0.1077(8) 0.043(3) 1.000 . Uani d ? O(14) 0.4199(5) 0.8320(5) -0.0580(7) 0.030(3) 1.000 . Uani d ? O(15) 0.2954(5) 0.8919(5) -0.0136(7) 0.025(2) 1.000 . Uani d ? O(16) -0.0242(5) 0.0349(5) 0.3867(7) 0.035(3) 1.000 . Uani d ? O(17) 0.1260(5) 0.0705(5) 0.4111(7) 0.027(2) 1.000 . Uani d ? O(18) 0.0364(5) 0.1699(5) 0.4808(7) 0.031(3) 1.000 . Uani d ? O(19) 0.0628(6) 0.4406(6) 0.5980(9) 0.062(4) 1.000 . Uani d ? O(20) 0.1191(5) 0.3523(5) 0.4449(8) 0.038(3) 1.000 . Uani d ? O(21) 0.1303(5) 0.3299(5) 0.6400(8) 0.035(3) 1.000 . Uani d ? O(22) 0.1790(6) 0.2604(5) 0.0954(8) 0.047(3) 1.000 . Uani d ? O(23) 0.1311(5) 0.1942(6) 0.2503(7) 0.040(3) 1.000 . Uani d ? O(24) 0.2534(5) 0.2923(5) 0.2844(7) 0.030(3) 1.000 . Uani d ? N(1) 0.4591(7) 0.6442(7) -0.029(1) 0.038(4) 1.000 . Uani d ? N(2) 0.3554(7) 0.7925(7) 0.297(1) 0.039(4) 1.000 . Uani d ? N(3) 0.3737(7) 0.8956(6) -0.0604(9) 0.027(3) 1.000 . Uani d ? N(4) 0.0444(6) 0.0904(7) 0.4267(9) 0.028(3) 1.000 . Uani d ? N(5) 0.1035(6) 0.3779(7) 0.561(1) 0.038(4) 1.000 . Uani d ? N(6) 0.1885(7) 0.2501(7) 0.207(1) 0.035(4) 1.000 . Uani d ? C(1) 0.1551(7) 0.8626(7) 0.335(1) 0.030(3) 1.000 . Uiso d ? C(2) 0.0955(7) 0.9402(8) 0.117(1) 0.037(3) 1.000 . Uiso d ? C(3) -0.0123(7) 0.7862(7) 0.176(1) 0.032(3) 1.000 . Uiso d ? C(4) 0.1106(7) 0.8275(8) -0.227(1) 0.040(3) 1.000 . Uiso d ? C(5) 0.0505(7) 0.6470(8) -0.207(1) 0.039(3) 1.000 . Uiso d ? C(6) 0.1549(8) 0.6843(8) -0.429(1) 0.046(4) 1.000 . Uiso d ? C(7) 0.1262(7) 0.5685(7) 0.235(1) 0.035(3) 1.000 . Uiso d ? C(8) 0.1207(7) 0.4364(7) -0.002(1) 0.026(3) 1.000 . Uiso d ? C(9) 0.2905(7) 0.4857(7) 0.169(1) 0.036(3) 1.000 . Uiso d ? C(10) 0.3149(8) 0.5114(8) 0.596(1) 0.041(3) 1.000 . Uiso d ? C(11) 0.3252(8) 0.4170(9) 0.812(1) 0.052(4) 1.000 . Uiso d ? C(12) 0.4853(7) 0.4346(8) 0.657(1) 0.039(3) 1.000 . Uiso d ? C(13) 0.4751(7) 0.2474(7) 0.347(1) 0.029(3) 1.000 . Uiso d ? C(14) 0.3619(7) 0.1137(7) 0.154(1) 0.030(3) 1.000 . Uiso d ? C(15) 0.4639(7) 0.0595(7) 0.364(1) 0.024(3) 1.000 . Uiso d ? C(16) 0.2785(7) 0.0076(7) 0.616(1) 0.027(3) 1.000 . Uiso d ? C(17) 0.2085(7) 0.0802(7) 0.857(1) 0.031(3) 1.000 . Uiso d ? C(18) 0.3864(7) 0.1574(8) 0.785(1) 0.035(3) 1.000 . Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Y(1) 0.0224(6) 0.0185(7) 0.0222(7) 0.0003(5) -0.0046(5) 0.0044(5) Y(2) 0.0219(6) 0.0205(7) 0.0194(7) 0.0008(5) -0.0043(5) 0.0036(5) P(1) 0.027(2) 0.023(2) 0.025(2) 0.002(1) 0.000(1) 0.006(1) P(2) 0.029(2) 0.029(2) 0.024(2) 0.003(1) -0.008(1) 0.007(2) P(3) 0.027(2) 0.019(2) 0.033(2) -0.003(1) -0.003(1) 0.006(2) P(4) 0.033(2) 0.028(2) 0.028(2) -0.004(2) -0.005(2) 0.001(2) P(5) 0.023(2) 0.025(2) 0.024(2) 0.001(1) -0.001(1) 0.002(1) P(6) 0.027(2) 0.024(2) 0.026(2) 0.002(1) -0.004(1) 0.007(1) O(1) 0.022(4) 0.020(5) 0.022(5) -0.004(3) -0.001(3) 0.007(4) O(2) 0.026(4) 0.029(5) 0.026(5) 0.003(4) -0.008(4) 0.006(4) O(3) 0.037(5) 0.018(5) 0.023(5) -0.008(4) -0.008(4) 0.006(4) O(4) 0.026(4) 0.022(5) 0.031(5) -0.007(3) -0.006(4) -0.007(4) O(5) 0.019(4) 0.025(5) 0.029(5) -0.001(3) -0.003(4) 0.010(4) O(6) 0.035(5) 0.019(5) 0.022(5) 0.005(4) -0.005(4) 0.002(4) O(7) 0.052(6) 0.089(9) 0.070(8) 0.048(6) -0.017(5) -0.017(6) O(8) 0.027(5) 0.031(5) 0.044(6) 0.007(4) -0.006(4) 0.005(4) O(9) 0.031(5) 0.040(6) 0.033(6) 0.009(4) -0.010(4) -0.011(4) O(10) 0.080(7) 0.059(7) 0.027(6) -0.011(5) -0.027(5) -0.007(5) O(11) 0.047(5) 0.024(5) 0.028(5) -0.009(4) -0.016(4) 0.008(4) O(12) 0.040(5) 0.025(5) 0.026(5) -0.009(4) -0.007(4) 0.007(4) O(13) 0.054(6) 0.033(6) 0.046(6) 0.002(5) 0.016(5) 0.020(5) O(14) 0.028(5) 0.020(5) 0.041(6) 0.001(4) 0.001(4) 0.007(4) O(15) 0.022(4) 0.021(5) 0.036(5) 0.002(3) 0.007(4) 0.011(4) O(16) 0.025(5) 0.030(5) 0.044(6) -0.010(4) -0.012(4) 0.005(4) O(17) 0.026(4) 0.019(5) 0.035(5) 0.002(4) -0.004(4) 0.004(4) O(18) 0.024(4) 0.030(5) 0.035(5) 0.000(4) -0.002(4) 0.002(4) O(19) 0.067(7) 0.045(7) 0.078(8) 0.034(5) 0.006(6) 0.000(6) O(20) 0.041(5) 0.038(6) 0.038(6) 0.015(4) -0.001(4) 0.011(5) O(21) 0.038(5) 0.028(6) 0.039(6) 0.005(4) 0.003(4) 0.002(4) O(22) 0.080(7) 0.043(6) 0.020(5) 0.006(5) -0.007(5) 0.014(5) O(23) 0.048(6) 0.053(7) 0.015(5) 0.001(5) -0.014(4) 0.008(4) O(24) 0.040(5) 0.024(5) 0.026(5) -0.005(4) -0.004(4) 0.012(4) N(1) 0.030(7) 0.031(7) 0.054(9) 0.011(5) -0.004(6) 0.005(6) N(2) 0.034(7) 0.046(8) 0.032(8) 0.005(6) -0.006(6) -0.002(6) N(3) 0.037(6) 0.019(6) 0.020(6) 0.003(5) -0.009(5) 0.000(5) N(4) 0.031(6) 0.034(7) 0.020(6) -0.001(5) -0.004(5) 0.012(5) N(5) 0.027(6) 0.032(8) 0.056(9) 0.009(5) 0.001(6) 0.006(7) N(6) 0.047(7) 0.030(7) 0.032(7) 0.008(5) 0.000(6) 0.014(6) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5513 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_all 0.0624 _refine_ls_wR_factor_ref 0.0624 _refine_ls_goodness_of_fit_all 5.688 _refine_ls_goodness_of_fit_ref 5.688 _refine_ls_shift/su_max 0.0350 _refine_ls_shift/su_mean 0.0070 _refine_diff_density_min -0.90 _refine_diff_density_max 1.31 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y(1) O(1) 2.281(7) . . yes Y(1) O(2) 2.279(7) . . yes Y(1) O(3) 2.261(7) . . yes Y(1) O(8) 2.487(7) . . yes Y(1) O(9) 2.441(7) . . yes Y(1) O(11) 2.520(8) . . yes Y(1) O(12) 2.453(7) . . yes Y(1) O(14) 2.454(7) . . yes Y(1) O(15) 2.515(7) . . yes Y(2) O(4) 2.270(6) . . yes Y(2) O(5) 2.251(7) . . yes Y(2) O(6) 2.258(7) . . yes Y(2) O(17) 2.479(7) . . yes Y(2) O(18) 2.468(7) . . yes Y(2) O(20) 2.463(8) . . yes Y(2) O(21) 2.506(8) . . yes Y(2) O(23) 2.486(7) . . yes Y(2) O(24) 2.525(7) . . yes P(1) O(1) 1.521(7) . . yes P(1) C(1) 1.80(1) . . yes P(1) C(2) 1.80(1) . . yes P(1) C(3) 1.80(1) . . yes P(2) O(2) 1.495(7) . . yes P(2) C(4) 1.80(1) . . yes P(2) C(5) 1.81(1) . . yes P(2) C(6) 1.84(1) . . yes P(3) O(3) 1.499(7) . . yes P(3) C(7) 1.83(1) . . yes P(3) C(8) 1.83(1) . . yes P(3) C(9) 1.78(1) . . yes P(4) O(4) 1.498(7) . . yes P(4) C(10) 1.80(1) . . yes P(4) C(11) 1.83(1) . . yes P(4) C(12) 1.84(1) . . yes P(5) O(5) 1.509(7) . . yes P(5) C(13) 1.82(1) . . yes P(5) C(14) 1.81(1) . . yes P(5) C(15) 1.78(1) . . yes P(6) O(6) 1.505(7) . . yes P(6) C(16) 1.80(1) . . yes P(6) C(17) 1.80(1) . . yes P(6) C(18) 1.81(1) . . yes O(7) N(1) 1.22(1) . . yes O(8) N(1) 1.27(1) . . yes O(9) N(1) 1.26(1) . . yes O(10) N(2) 1.22(1) . . yes O(11) N(2) 1.30(1) . . yes O(12) N(2) 1.26(1) . . yes O(13) N(3) 1.25(1) . . yes O(14) N(3) 1.26(1) . . yes O(15) N(3) 1.27(1) . . yes O(16) N(4) 1.24(1) . . yes O(17) N(4) 1.27(1) . . yes O(18) N(4) 1.28(1) . . yes O(19) N(5) 1.21(1) . . yes O(20) N(5) 1.27(1) . . yes O(21) N(5) 1.28(1) . . yes O(22) N(6) 1.22(1) . . yes O(23) N(6) 1.29(1) . . yes O(24) N(6) 1.26(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Y(1) O(2) 86.0(2) . . . yes O(1) Y(1) O(3) 82.9(2) . . . yes O(1) Y(1) O(8) 152.1(2) . . . yes O(1) Y(1) O(9) 148.7(3) . . . yes O(1) Y(1) O(11) 79.6(2) . . . yes O(1) Y(1) O(12) 86.6(2) . . . yes O(1) Y(1) O(14) 124.5(2) . . . yes O(1) Y(1) O(15) 72.7(2) . . . yes O(2) Y(1) O(3) 84.3(2) . . . yes O(2) Y(1) O(8) 71.6(3) . . . yes O(2) Y(1) O(9) 122.9(3) . . . yes O(2) Y(1) O(11) 155.3(2) . . . yes O(2) Y(1) O(12) 147.5(3) . . . yes O(2) Y(1) O(14) 83.0(2) . . . yes O(2) Y(1) O(15) 77.3(2) . . . yes O(3) Y(1) O(8) 78.5(3) . . . yes O(3) Y(1) O(9) 88.2(3) . . . yes O(3) Y(1) O(11) 74.2(2) . . . yes O(3) Y(1) O(12) 126.0(3) . . . yes O(3) Y(1) O(14) 148.6(3) . . . yes O(3) Y(1) O(15) 150.2(2) . . . yes O(8) Y(1) O(9) 51.5(2) . . . yes O(8) Y(1) O(11) 114.4(3) . . . yes O(8) Y(1) O(12) 121.2(2) . . . yes O(8) Y(1) O(14) 70.3(2) . . . yes O(8) Y(1) O(15) 116.5(2) . . . yes O(9) Y(1) O(11) 69.1(3) . . . yes O(9) Y(1) O(12) 74.6(3) . . . yes O(9) Y(1) O(14) 75.1(3) . . . yes O(9) Y(1) O(15) 121.5(2) . . . yes O(11) Y(1) O(12) 51.9(2) . . . yes O(11) Y(1) O(14) 121.7(2) . . . yes O(11) Y(1) O(15) 116.6(2) . . . yes O(12) Y(1) O(14) 75.4(3) . . . yes O(12) Y(1) O(15) 70.3(2) . . . yes O(14) Y(1) O(15) 51.8(2) . . . yes O(4) Y(2) O(5) 82.5(2) . . . yes O(4) Y(2) O(6) 86.8(3) . . . yes O(4) Y(2) O(17) 154.2(2) . . . yes O(4) Y(2) O(18) 147.4(3) . . . yes O(4) Y(2) O(20) 84.6(3) . . . yes O(4) Y(2) O(21) 76.7(2) . . . yes O(4) Y(2) O(23) 126.0(3) . . . yes O(4) Y(2) O(24) 75.0(2) . . . yes O(5) Y(2) O(6) 86.1(2) . . . yes O(5) Y(2) O(17) 75.7(2) . . . yes O(5) Y(2) O(18) 128.2(2) . . . yes O(5) Y(2) O(20) 144.0(3) . . . yes O(5) Y(2) O(21) 152.8(2) . . . yes O(5) Y(2) O(23) 88.3(3) . . . yes O(5) Y(2) O(24) 76.1(2) . . . yes O(6) Y(2) O(17) 78.2(2) . . . yes O(6) Y(2) O(18) 84.9(2) . . . yes O(6) Y(2) O(20) 126.6(3) . . . yes O(6) Y(2) O(21) 75.5(3) . . . yes O(6) Y(2) O(23) 145.6(3) . . . yes O(6) Y(2) O(24) 155.9(2) . . . yes O(17) Y(2) O(18) 52.5(2) . . . yes O(17) Y(2) O(20) 121.2(2) . . . yes O(17) Y(2) O(21) 118.6(2) . . . yes O(17) Y(2) O(23) 67.6(3) . . . yes O(17) Y(2) O(24) 112.1(2) . . . yes O(18) Y(2) O(20) 75.4(3) . . . yes O(18) Y(2) O(21) 70.7(2) . . . yes O(18) Y(2) O(23) 72.2(3) . . . yes O(18) Y(2) O(24) 118.9(2) . . . yes O(20) Y(2) O(21) 51.3(3) . . . yes O(20) Y(2) O(23) 72.6(3) . . . yes O(20) Y(2) O(24) 68.1(3) . . . yes O(21) Y(2) O(23) 118.2(3) . . . yes O(21) Y(2) O(24) 114.4(3) . . . yes O(23) Y(2) O(24) 51.2(2) . . . yes O(1) P(1) C(1) 112.1(5) . . . yes O(1) P(1) C(2) 112.8(5) . . . yes O(1) P(1) C(3) 111.8(4) . . . yes C(1) P(1) C(2) 107.9(5) . . . yes C(1) P(1) C(3) 106.8(5) . . . yes C(2) P(1) C(3) 105.1(5) . . . yes O(2) P(2) C(4) 112.9(5) . . . yes O(2) P(2) C(5) 112.3(5) . . . yes O(2) P(2) C(6) 110.4(5) . . . yes C(4) P(2) C(5) 104.5(5) . . . yes C(4) P(2) C(6) 107.9(6) . . . yes C(5) P(2) C(6) 108.4(5) . . . yes O(3) P(3) C(7) 114.1(5) . . . yes O(3) P(3) C(8) 109.4(5) . . . yes O(3) P(3) C(9) 110.9(5) . . . yes C(7) P(3) C(8) 106.4(5) . . . yes C(7) P(3) C(9) 107.1(5) . . . yes C(8) P(3) C(9) 108.6(5) . . . yes O(4) P(4) C(10) 110.7(5) . . . yes O(4) P(4) C(11) 113.2(5) . . . yes O(4) P(4) C(12) 110.1(5) . . . yes C(10) P(4) C(11) 107.2(6) . . . yes C(10) P(4) C(12) 108.9(5) . . . yes C(11) P(4) C(12) 106.6(5) . . . yes O(5) P(5) C(13) 111.6(4) . . . yes O(5) P(5) C(14) 112.0(4) . . . yes O(5) P(5) C(15) 110.4(5) . . . yes C(13) P(5) C(14) 106.8(5) . . . yes C(13) P(5) C(15) 108.1(5) . . . yes C(14) P(5) C(15) 107.8(5) . . . yes O(6) P(6) C(16) 112.3(5) . . . yes O(6) P(6) C(17) 110.9(5) . . . yes O(6) P(6) C(18) 111.7(5) . . . yes C(16) P(6) C(17) 106.9(5) . . . yes C(16) P(6) C(18) 106.6(5) . . . yes C(17) P(6) C(18) 108.1(5) . . . yes Y(1) O(1) P(1) 149.9(4) . . . yes Y(1) O(2) P(2) 140.2(4) . . . yes Y(1) O(3) P(3) 147.0(4) . . . yes Y(2) O(4) P(4) 149.3(4) . . . yes Y(2) O(5) P(5) 147.8(4) . . . yes Y(2) O(6) P(6) 144.5(4) . . . yes Y(1) O(8) N(1) 95.2(7) . . . yes Y(1) O(9) N(1) 97.6(6) . . . yes Y(1) O(11) N(2) 93.4(7) . . . yes Y(1) O(12) N(2) 97.6(6) . . . yes Y(1) O(14) N(3) 96.2(6) . . . yes Y(1) O(15) N(3) 93.0(6) . . . yes Y(2) O(17) N(4) 94.3(6) . . . yes Y(2) O(18) N(4) 94.6(6) . . . yes Y(2) O(20) N(5) 98.0(7) . . . yes Y(2) O(21) N(5) 95.5(7) . . . yes Y(2) O(23) N(6) 96.5(6) . . . yes Y(2) O(24) N(6) 95.5(6) . . . yes O(7) N(1) O(8) 122(1) . . . yes O(7) N(1) O(9) 123(1) . . . yes O(8) N(1) O(9) 115.5(9) . . . yes O(10) N(2) O(11) 120(1) . . . yes O(10) N(2) O(12) 123(1) . . . yes O(11) N(2) O(12) 117(1) . . . yes O(13) N(3) O(14) 121(1) . . . yes O(13) N(3) O(15) 121(1) . . . yes O(14) N(3) O(15) 119(1) . . . yes O(16) N(4) O(17) 121(1) . . . yes O(16) N(4) O(18) 121.7(9) . . . yes O(17) N(4) O(18) 117.7(9) . . . yes O(19) N(5) O(20) 124(1) . . . yes O(19) N(5) O(21) 121(1) . . . yes O(20) N(5) O(21) 115(1) . . . yes O(22) N(6) O(23) 121(1) . . . yes O(22) N(6) O(24) 123(1) . . . yes O(23) N(6) O(24) 117(1) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(7) C(11) 3.34(2) . 2_666 no O(7) C(9) 3.35(1) . 2_665 no O(8) C(10) 3.41(1) . 1_554 no O(8) C(11) 3.44(1) . 1_554 no O(9) C(18) 3.33(1) . 2_666 no O(10) C(15) 3.34(1) . 2_666 no O(10) C(13) 3.53(1) . 2_666 no O(12) C(15) 3.52(1) . 1_565 no O(12) C(18) 3.56(1) . 2_666 no O(13) C(15) 3.39(1) . 2_665 no O(13) C(14) 3.44(1) . 1_565 no O(13) C(18) 3.44(1) . 1_564 no O(13) O(13) 3.46(2) . 2_675 no O(13) C(16) 3.58(1) . 1_564 no O(14) C(14) 3.44(1) . 2_665 no O(14) C(13) 3.58(1) . 2_665 no O(15) C(14) 3.56(1) . 1_565 no O(16) O(16) 2.88(2) . 2_556 no O(16) N(4) 2.99(1) . 2_556 no O(16) O(17) 3.22(1) . 2_556 no O(16) C(4) 3.25(1) . 2_565 no O(17) C(1) 3.25(1) . 1_545 no O(17) C(2) 3.37(1) . 1_545 no O(18) C(4) 3.35(1) . 2_565 no O(18) C(1) 3.52(1) . 2_566 no O(19) C(7) 3.35(1) . 2_566 no O(19) C(5) 3.51(1) . 1_556 no O(19) O(19) 3.56(2) . 2_566 no O(20) C(5) 3.44(1) . 2_565 no O(21) C(3) 3.28(1) . 2_566 no O(22) C(8) 3.25(1) . . no O(22) C(17) 3.49(1) . 1_554 no O(22) C(3) 3.57(1) . 2_565 no O(22) C(9) 3.58(1) . . no O(23) C(4) 3.49(1) . 2_565 no O(24) C(9) 3.40(1) . . no N(4) C(4) 3.50(1) . 2_565 no N(4) N(4) 3.56(2) . 2_556 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Y(1) O(1) P(1) C(1) . . . . -39(1) no Y(1) O(1) P(1) C(2) . . . . 83.3(9) no Y(1) O(1) P(1) C(3) . . . . -158.6(8) no Y(1) O(2) P(2) C(4) . . . . 61.2(8) no Y(1) O(2) P(2) C(5) . . . . -56.7(8) no Y(1) O(2) P(2) C(6) . . . . -177.9(7) no Y(1) O(3) P(3) C(7) . . . . 51.7(9) no Y(1) O(3) P(3) C(8) . . . . 170.7(7) no Y(1) O(3) P(3) C(9) . . . . -69.5(9) no Y(1) O(8) N(1) O(7) . . . . -175(1) no Y(1) O(8) N(1) O(9) . . . . 4(1) no Y(1) O(9) N(1) O(7) . . . . 175(1) no Y(1) O(9) N(1) O(8) . . . . -4(1) no Y(1) O(11) N(2) O(10) . . . . -175(1) no Y(1) O(11) N(2) O(12) . . . . 5(1) no Y(1) O(12) N(2) O(10) . . . . 175(1) no Y(1) O(12) N(2) O(11) . . . . -5(1) no Y(1) O(14) N(3) O(13) . . . . -173.9(8) no Y(1) O(14) N(3) O(15) . . . . 6.1(9) no Y(1) O(15) N(3) O(13) . . . . 174.1(8) no Y(1) O(15) N(3) O(14) . . . . -6.0(9) no Y(2) O(4) P(4) C(10) . . . . -72(1) no Y(2) O(4) P(4) C(11) . . . . 48(1) no Y(2) O(4) P(4) C(12) . . . . 167.2(9) no Y(2) O(5) P(5) C(13) . . . . 47.5(9) no Y(2) O(5) P(5) C(14) . . . . -72.1(9) no Y(2) O(5) P(5) C(15) . . . . 167.7(7) no Y(2) O(6) P(6) C(16) . . . . -38.3(9) no Y(2) O(6) P(6) C(17) . . . . -157.9(7) no Y(2) O(6) P(6) C(18) . . . . 81.5(8) no Y(2) O(17) N(4) O(16) . . . . 168.6(8) no Y(2) O(17) N(4) O(18) . . . . -9.2(9) no Y(2) O(18) N(4) O(16) . . . . -168.5(9) no Y(2) O(18) N(4) O(17) . . . . 9.2(9) no Y(2) O(20) N(5) O(19) . . . . -180(1) no Y(2) O(20) N(5) O(21) . . . . -3(1) no Y(2) O(21) N(5) O(19) . . . . 180(1) no Y(2) O(21) N(5) O(20) . . . . 3(1) no Y(2) O(23) N(6) O(22) . . . . -177.5(9) no Y(2) O(23) N(6) O(24) . . . . 3(1) no Y(2) O(24) N(6) O(22) . . . . 178(1) no Y(2) O(24) N(6) O(23) . . . . -2(1) no P(1) O(1) Y(1) O(2) . . . . -140.6(9) no P(1) O(1) Y(1) O(3) . . . . 134.7(9) no P(1) O(1) Y(1) O(8) . . . . -177.0(7) no P(1) O(1) Y(1) O(9) . . . . 60(1) no P(1) O(1) Y(1) O(11) . . . . 59.6(9) no P(1) O(1) Y(1) O(12) . . . . 7.7(9) no P(1) O(1) Y(1) O(14) . . . . -61.9(9) no P(1) O(1) Y(1) O(15) . . . . -62.7(8) no P(2) O(2) Y(1) O(1) . . . . -2.5(7) no P(2) O(2) Y(1) O(3) . . . . 80.8(7) no P(2) O(2) Y(1) O(8) . . . . 160.5(7) no P(2) O(2) Y(1) O(9) . . . . 164.8(6) no P(2) O(2) Y(1) O(11) . . . . 52(1) no P(2) O(2) Y(1) O(12) . . . . -79.8(8) no P(2) O(2) Y(1) O(14) . . . . -128.0(7) no P(2) O(2) Y(1) O(15) . . . . -75.6(7) no P(3) O(3) Y(1) O(1) . . . . -78.8(8) no P(3) O(3) Y(1) O(2) . . . . -165.5(8) no P(3) O(3) Y(1) O(8) . . . . 122.1(8) no P(3) O(3) Y(1) O(9) . . . . 71.1(8) no P(3) O(3) Y(1) O(11) . . . . 2.4(8) no P(3) O(3) Y(1) O(12) . . . . 2(1) no P(3) O(3) Y(1) O(14) . . . . 128.0(8) no P(3) O(3) Y(1) O(15) . . . . -113.7(8) no P(4) O(4) Y(2) O(5) . . . . -162(1) no P(4) O(4) Y(2) O(6) . . . . -75.5(9) no P(4) O(4) Y(2) O(17) . . . . -129.5(8) no P(4) O(4) Y(2) O(18) . . . . 0(1) no P(4) O(4) Y(2) O(20) . . . . 51.8(9) no P(4) O(4) Y(2) O(21) . . . . 0.4(9) no P(4) O(4) Y(2) O(23) . . . . 115.7(9) no P(4) O(4) Y(2) O(24) . . . . 121(1) no P(5) O(5) Y(2) O(4) . . . . -61.8(8) no P(5) O(5) Y(2) O(6) . . . . -149.1(8) no P(5) O(5) Y(2) O(17) . . . . 132.2(8) no P(5) O(5) Y(2) O(18) . . . . 130.6(7) no P(5) O(5) Y(2) O(20) . . . . 8(1) no P(5) O(5) Y(2) O(21) . . . . -102.0(9) no P(5) O(5) Y(2) O(23) . . . . 64.9(8) no P(5) O(5) Y(2) O(24) . . . . 14.6(7) no P(6) O(6) Y(2) O(4) . . . . -90.0(7) no P(6) O(6) Y(2) O(5) . . . . -7.3(7) no P(6) O(6) Y(2) O(17) . . . . 68.9(7) no P(6) O(6) Y(2) O(18) . . . . 121.6(7) no P(6) O(6) Y(2) O(20) . . . . -170.9(6) no P(6) O(6) Y(2) O(21) . . . . -167.1(8) no P(6) O(6) Y(2) O(23) . . . . 73.9(9) no P(6) O(6) Y(2) O(24) . . . . -49(1) no O(1) Y(1) O(8) N(1) . . . . -148.6(6) no O(1) Y(1) O(9) N(1) . . . . 152.4(6) no O(1) Y(1) O(11) N(2) . . . . -96.5(6) no O(1) Y(1) O(12) N(2) . . . . 82.2(7) no O(1) Y(1) O(14) N(3) . . . . -4.4(7) no O(1) Y(1) O(15) N(3) . . . . -177.4(6) no O(2) Y(1) O(8) N(1) . . . . 172.7(7) no O(2) Y(1) O(9) N(1) . . . . -2.7(8) no O(2) Y(1) O(11) N(2) . . . . -152.0(6) no O(2) Y(1) O(12) N(2) . . . . 159.4(6) no O(2) Y(1) O(14) N(3) . . . . 75.9(6) no O(2) Y(1) O(15) N(3) . . . . -87.6(6) no O(3) Y(1) O(8) N(1) . . . . -99.5(7) no O(3) Y(1) O(9) N(1) . . . . 79.3(7) no O(3) Y(1) O(11) N(2) . . . . 178.0(7) no O(3) Y(1) O(12) N(2) . . . . 3.5(8) no O(3) Y(1) O(14) N(3) . . . . 142.7(6) no O(3) Y(1) O(15) N(3) . . . . -140.9(6) no O(4) Y(2) O(17) N(4) . . . . 153.6(6) no O(4) Y(2) O(18) N(4) . . . . -160.2(6) no O(4) Y(2) O(20) N(5) . . . . -75.4(6) no O(4) Y(2) O(21) N(5) . . . . 92.0(6) no O(4) Y(2) O(23) N(6) . . . . 4.6(8) no O(4) Y(2) O(24) N(6) . . . . -173.5(7) no O(5) Y(2) O(17) N(4) . . . . -173.1(6) no O(5) Y(2) O(18) N(4) . . . . -3.3(7) no O(5) Y(2) O(20) N(5) . . . . -144.8(6) no O(5) Y(2) O(21) N(5) . . . . 133.2(7) no O(5) Y(2) O(23) N(6) . . . . -74.9(7) no O(5) Y(2) O(24) N(6) . . . . 100.7(6) no O(6) Y(2) O(17) N(4) . . . . 97.9(6) no O(6) Y(2) O(18) N(4) . . . . -84.3(6) no O(6) Y(2) O(20) N(5) . . . . 6.6(8) no O(6) Y(2) O(21) N(5) . . . . -177.8(7) no O(6) Y(2) O(23) N(6) . . . . -155.4(6) no O(6) Y(2) O(24) N(6) . . . . 144.1(6) no O(8) Y(1) O(9) N(1) . . . . 2.6(6) no O(8) Y(1) O(11) N(2) . . . . 108.9(6) no O(8) Y(1) O(12) N(2) . . . . -95.2(7) no O(8) Y(1) O(14) N(3) . . . . 148.8(6) no O(8) Y(1) O(15) N(3) . . . . -25.9(6) no O(9) Y(1) O(8) N(1) . . . . -2.6(6) no O(9) Y(1) O(11) N(2) . . . . 83.8(6) no O(9) Y(1) O(12) N(2) . . . . -72.5(7) no O(9) Y(1) O(14) N(3) . . . . -157.3(6) no O(9) Y(1) O(15) N(3) . . . . 33.4(6) no O(11) Y(1) O(8) N(1) . . . . -33.0(7) no O(11) Y(1) O(9) N(1) . . . . 153.0(7) no O(11) Y(1) O(12) N(2) . . . . 2.7(6) no O(11) Y(1) O(14) N(3) . . . . -104.0(6) no O(11) Y(1) O(15) N(3) . . . . 114.1(6) no O(12) Y(1) O(8) N(1) . . . . 25.8(7) no O(12) Y(1) O(9) N(1) . . . . -152.4(7) no O(12) Y(1) O(11) N(2) . . . . -2.6(6) no O(12) Y(1) O(14) N(3) . . . . -79.7(6) no O(12) Y(1) O(15) N(3) . . . . 90.0(6) no O(14) Y(1) O(8) N(1) . . . . 83.7(6) no O(14) Y(1) O(9) N(1) . . . . -73.9(7) no O(14) Y(1) O(11) N(2) . . . . 27.8(7) no O(14) Y(1) O(12) N(2) . . . . -150.8(7) no O(14) Y(1) O(15) N(3) . . . . 3.4(5) no O(15) Y(1) O(8) N(1) . . . . 107.8(6) no O(15) Y(1) O(9) N(1) . . . . -97.9(7) no O(15) Y(1) O(11) N(2) . . . . -31.9(7) no O(15) Y(1) O(12) N(2) . . . . 155.1(7) no O(15) Y(1) O(14) N(3) . . . . -3.5(5) no O(17) Y(2) O(18) N(4) . . . . -5.3(5) no O(17) Y(2) O(20) N(5) . . . . 105.2(6) no O(17) Y(2) O(21) N(5) . . . . -110.3(6) no O(17) Y(2) O(23) N(6) . . . . -150.1(7) no O(17) Y(2) O(24) N(6) . . . . 32.7(7) no O(18) Y(2) O(17) N(4) . . . . 5.3(5) no O(18) Y(2) O(20) N(5) . . . . 78.6(6) no O(18) Y(2) O(21) N(5) . . . . -88.2(6) no O(18) Y(2) O(23) N(6) . . . . 153.9(7) no O(18) Y(2) O(24) N(6) . . . . -25.5(7) no O(20) Y(2) O(17) N(4) . . . . -27.9(7) no O(20) Y(2) O(18) N(4) . . . . 145.8(6) no O(20) Y(2) O(21) N(5) . . . . -1.8(6) no O(20) Y(2) O(23) N(6) . . . . 74.1(7) no O(20) Y(2) O(24) N(6) . . . . -83.4(6) no O(21) Y(2) O(17) N(4) . . . . 31.9(6) no O(21) Y(2) O(18) N(4) . . . . -160.7(6) no O(21) Y(2) O(20) N(5) . . . . 1.8(6) no O(21) Y(2) O(23) N(6) . . . . 98.4(7) no O(21) Y(2) O(24) N(6) . . . . -106.0(6) no O(23) Y(2) O(17) N(4) . . . . -79.0(6) no O(23) Y(2) O(18) N(4) . . . . 69.7(6) no O(23) Y(2) O(20) N(5) . . . . 154.1(7) no O(23) Y(2) O(21) N(5) . . . . -31.9(7) no O(23) Y(2) O(24) N(6) . . . . 1.5(6) no O(24) Y(2) O(17) N(4) . . . . -104.9(6) no O(24) Y(2) O(18) N(4) . . . . 91.5(6) no O(24) Y(2) O(20) N(5) . . . . -151.5(7) no O(24) Y(2) O(21) N(5) . . . . 25.5(7) no O(24) Y(2) O(23) N(6) . . . . -1.4(6) no #===END #===================================================== data_Jlev99_12 #------------------------------------------------------------------------------ _audit_creation_date '2000-02-04' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 11.170(6) _cell_length_b 11.411(4) _cell_length_c 41.504(6) _cell_angle_alpha 90 _cell_angle_beta 93.48(3) _cell_angle_gamma 90 _cell_volume 5280(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 7.0 _cell_measurement_theta_max 9.8 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1109.79 _chemical_formula_analytical ? _chemical_name_systematic ; tris(nitrato-O,O')tris(triphenylphosphineoxide)yttrium(III) ; _chemical_formula_sum 'C54 H45 N3 O12 P3 Y ' _chemical_formula_moiety 'C54 H45 N3 O12 P3 Y ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2280.00 _exptl_absorpt_coefficient_mu 1.261 _exptl_absorpt_correction_type empirical # psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.798 _exptl_special_details ; The scan width was (0.94+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.08 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 -1 10 -1 -4 10 0 -4 6 _diffrn_reflns_number 10349 _reflns_number_total 9809 _reflns_number_gt 2941 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.07796 _diffrn_reflns_av_sigmaI/netI 0.260 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01803 _diffrn_orient_matrix_UB_12 -0.03222 _diffrn_orient_matrix_UB_13 0.02158 _diffrn_orient_matrix_UB_21 -0.05067 _diffrn_orient_matrix_UB_22 0.07017 _diffrn_orient_matrix_UB_23 0.00397 _diffrn_orient_matrix_UB_31 -0.07178 _diffrn_orient_matrix_UB_32 -0.04144 _diffrn_orient_matrix_UB_33 -0.01006 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 216 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 180 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 12 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 48 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 12 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Y 0 4 -2.951 3.542 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Y(1) 0.2622(2) 0.3397(2) 0.13674(5) 0.0269(5) 1.000 . Uani d ? P(1) 0.5964(5) 0.3635(4) 0.1398(1) 0.030(2) 1.000 . Uani d ? P(2) 0.2460(5) 0.6051(4) 0.1891(1) 0.030(2) 1.000 . Uani d ? P(3) 0.2835(6) 0.1949(4) 0.0577(1) 0.042(2) 1.000 . Uani d ? O(1) 0.464(1) 0.376(1) 0.1396(3) 0.038(5) 1.000 . Uani d ? O(2) 0.248(1) 0.494(1) 0.1696(3) 0.038(5) 1.000 . Uani d ? O(3) 0.300(1) 0.264(1) 0.0883(3) 0.043(5) 1.000 . Uani d ? O(4) -0.075(1) 0.198(1) 0.1438(3) 0.053(5) 1.000 . Uani d ? O(5) 0.066(1) 0.323(1) 0.1614(3) 0.042(5) 1.000 . Uani d ? O(6) 0.105(1) 0.195(1) 0.1266(3) 0.042(5) 1.000 . Uani d ? O(7) 0.398(2) 0.088(1) 0.1995(4) 0.081(7) 1.000 . Uani d ? O(8) 0.350(1) 0.147(1) 0.1508(3) 0.044(5) 1.000 . Uani d ? O(9) 0.313(1) 0.259(1) 0.1904(3) 0.043(5) 1.000 . Uani d ? O(10) 0.141(1) 0.562(1) 0.0645(4) 0.065(6) 1.000 . Uani d ? O(11) 0.107(1) 0.435(1) 0.1021(3) 0.034(4) 1.000 . Uani d ? O(12) 0.284(1) 0.508(1) 0.0991(3) 0.034(4) 1.000 . Uani d ? N(1) 0.025(2) 0.236(2) 0.1439(4) 0.039(5) 1.000 . Uiso d ? N(2) 0.353(2) 0.162(2) 0.1811(5) 0.048(5) 1.000 . Uiso d ? N(3) 0.176(2) 0.505(1) 0.0877(4) 0.035(5) 1.000 . Uiso d ? C(1) 0.664(2) 0.402(1) 0.1793(4) 0.025(5) 1.000 . Uiso d ? C(2) 0.593(2) 0.415(2) 0.2048(5) 0.035(5) 1.000 . Uiso d ? C(3) 0.634(2) 0.450(2) 0.2341(5) 0.039(6) 1.000 . Uiso d ? C(4) 0.753(2) 0.476(2) 0.2379(5) 0.039(6) 1.000 . Uiso d ? C(5) 0.830(2) 0.468(2) 0.2130(5) 0.050(6) 1.000 . Uiso d ? C(6) 0.787(2) 0.429(2) 0.1827(5) 0.043(6) 1.000 . Uiso d ? C(7) 0.656(2) 0.458(2) 0.1104(4) 0.025(5) 1.000 . Uiso d ? C(8) 0.584(2) 0.546(2) 0.0974(4) 0.030(5) 1.000 . Uiso d ? C(9) 0.627(2) 0.629(2) 0.0773(5) 0.053(7) 1.000 . Uiso d ? C(10) 0.746(2) 0.624(2) 0.0700(5) 0.051(6) 1.000 . Uiso d ? C(11) 0.819(2) 0.533(2) 0.0824(6) 0.063(7) 1.000 . Uiso d ? C(12) 0.777(2) 0.449(2) 0.1023(5) 0.045(6) 1.000 . Uiso d ? C(13) 0.641(2) 0.217(2) 0.1313(5) 0.031(5) 1.000 . Uiso d ? C(14) 0.654(2) 0.183(2) 0.0994(6) 0.063(7) 1.000 . Uiso d ? C(15) 0.686(3) 0.065(3) 0.0917(7) 0.10(1) 1.000 . Uiso d ? C(16) 0.693(2) -0.013(2) 0.1180(6) 0.056(7) 1.000 . Uiso d ? C(17) 0.681(2) 0.020(2) 0.1482(5) 0.052(7) 1.000 . Uiso d ? C(18) 0.655(2) 0.134(2) 0.1561(5) 0.038(6) 1.000 . Uiso d ? C(19) 0.182(2) 0.579(2) 0.2268(4) 0.031(5) 1.000 . Uiso d ? C(20) 0.167(2) 0.466(2) 0.2376(5) 0.037(6) 1.000 . Uiso d ? C(21) 0.114(2) 0.445(2) 0.2664(5) 0.049(6) 1.000 . Uiso d ? C(22) 0.077(2) 0.536(2) 0.2850(5) 0.060(7) 1.000 . Uiso d ? C(23) 0.089(2) 0.654(2) 0.2744(5) 0.053(6) 1.000 . Uiso d ? C(24) 0.145(2) 0.673(2) 0.2449(5) 0.050(6) 1.000 . Uiso d ? C(25) 0.156(2) 0.715(2) 0.1679(4) 0.027(5) 1.000 . Uiso d ? C(26) 0.051(2) 0.684(2) 0.1522(5) 0.045(6) 1.000 . Uiso d ? C(27) -0.021(2) 0.770(2) 0.1363(6) 0.067(8) 1.000 . Uiso d ? C(28) 0.015(2) 0.884(2) 0.1360(5) 0.042(6) 1.000 . Uiso d ? C(29) 0.124(2) 0.916(2) 0.1508(5) 0.040(6) 1.000 . Uiso d ? C(30) 0.194(2) 0.833(2) 0.1676(5) 0.042(6) 1.000 . Uiso d ? C(31) 0.395(2) 0.662(2) 0.1964(4) 0.028(5) 1.000 . Uiso d ? C(32) 0.446(2) 0.697(2) 0.2266(5) 0.037(6) 1.000 . Uiso d ? C(33) 0.561(2) 0.737(2) 0.2288(5) 0.044(6) 1.000 . Uiso d ? C(34) 0.630(2) 0.745(2) 0.2029(5) 0.042(6) 1.000 . Uiso d ? C(35) 0.580(2) 0.709(2) 0.1730(5) 0.043(6) 1.000 . Uiso d ? C(36) 0.463(2) 0.671(2) 0.1694(4) 0.032(5) 1.000 . Uiso d ? C(37) 0.406(2) 0.229(2) 0.0327(5) 0.042(6) 1.000 . Uiso d ? C(38) 0.463(2) 0.337(2) 0.0375(5) 0.041(5) 1.000 . Uiso d ? C(39) 0.557(2) 0.366(2) 0.0183(5) 0.051(6) 1.000 . Uiso d ? C(40) 0.589(2) 0.291(2) -0.0055(6) 0.063(7) 1.000 . Uiso d ? C(41) 0.524(2) 0.185(2) -0.0110(6) 0.071(8) 1.000 . Uiso d ? C(42) 0.435(2) 0.156(2) 0.0085(6) 0.064(7) 1.000 . Uiso d ? C(43) 0.136(2) 0.235(2) 0.0388(5) 0.105 1.000 G Uiso d ? C(44) 0.138(1) 0.304(2) 0.0110(5) 0.105 1.000 G Uiso d ? C(45) 0.030(2) 0.346(1) -0.0035(4) 0.105 1.000 G Uiso d ? C(46) -0.0876 0.3193 0.0170 0.076 1.000 G Uiso c ? C(47) -0.0707 0.2448 0.0435 0.076 1.000 G Uiso c ? C(48) 0.0438 0.2035 0.0528 0.076 1.000 G Uiso c ? C(49) 0.281(2) 0.039(2) 0.0660(5) 0.045(6) 1.000 . Uiso d ? C(50) 0.203(2) -0.035(2) 0.0514(5) 0.055(7) 1.000 . Uiso d ? C(51) 0.213(2) -0.160(2) 0.0616(6) 0.073(8) 1.000 . Uiso d ? C(52) 0.297(2) -0.189(2) 0.0833(6) 0.067(8) 1.000 . Uiso d ? C(53) 0.380(2) -0.120(2) 0.0985(6) 0.079(9) 1.000 . Uiso d ? C(54) 0.369(2) 0.001(2) 0.0893(6) 0.063(7) 1.000 . Uiso d ? H(1) 0.5102 0.3990 0.2015 0.042 1.000 . Uiso c ? H(2) 0.5832 0.4552 0.2515 0.046 1.000 . Uiso c ? H(3) 0.7846 0.5021 0.2585 0.047 1.000 . Uiso c ? H(4) 0.9121 0.4881 0.2166 0.060 1.000 . Uiso c ? H(5) 0.8380 0.4217 0.1654 0.052 1.000 . Uiso c ? H(6) 0.5017 0.5494 0.1024 0.036 1.000 . Uiso c ? H(7) 0.5763 0.6890 0.0685 0.064 1.000 . Uiso c ? H(8) 0.7786 0.6819 0.0567 0.062 1.000 . Uiso c ? H(9) 0.9002 0.5300 0.0768 0.075 1.000 . Uiso c ? H(10) 0.8265 0.3863 0.1102 0.053 1.000 . Uiso c ? H(11) 0.6418 0.2392 0.0826 0.075 1.000 . Uiso c ? H(12) 0.7013 0.0419 0.0704 0.120 1.000 . Uiso c ? H(13) 0.7069 -0.0940 0.1138 0.067 1.000 . Uiso c ? H(14) 0.6899 -0.0368 0.1649 0.062 1.000 . Uiso c ? H(15) 0.6465 0.1561 0.1780 0.045 1.000 . Uiso c ? H(16) 0.1936 0.4017 0.2252 0.045 1.000 . Uiso c ? H(17) 0.1028 0.3668 0.2734 0.059 1.000 . Uiso c ? H(18) 0.0423 0.5207 0.3050 0.071 1.000 . Uiso c ? H(19) 0.0617 0.7175 0.2866 0.064 1.000 . Uiso c ? H(20) 0.1566 0.7507 0.2376 0.061 1.000 . Uiso c ? H(21) 0.0260 0.6045 0.1520 0.054 1.000 . Uiso c ? H(22) -0.0948 0.7482 0.1256 0.080 1.000 . Uiso c ? H(23) -0.0358 0.9413 0.1257 0.051 1.000 . Uiso c ? H(24) 0.1509 0.9945 0.1494 0.048 1.000 . Uiso c ? H(25) 0.2663 0.8556 0.1790 0.051 1.000 . Uiso c ? H(26) 0.4002 0.6935 0.2451 0.044 1.000 . Uiso c ? H(27) 0.5947 0.7594 0.2494 0.053 1.000 . Uiso c ? H(28) 0.7093 0.7740 0.2052 0.050 1.000 . Uiso c ? H(29) 0.6276 0.7114 0.1548 0.052 1.000 . Uiso c ? H(30) 0.4290 0.6512 0.1486 0.038 1.000 . Uiso c ? H(31) 0.4381 0.3894 0.0536 0.049 1.000 . Uiso c ? H(32) 0.5988 0.4375 0.0217 0.062 1.000 . Uiso c ? H(33) 0.6542 0.3095 -0.0182 0.076 1.000 . Uiso c ? H(34) 0.5429 0.1348 -0.0283 0.085 1.000 . Uiso c ? H(35) 0.3933 0.0842 0.0051 0.077 1.000 . Uiso c ? H(41) 0.1452 -0.0100 0.0352 0.065 1.000 . Uiso c ? H(42) 0.1587 -0.2165 0.0526 0.087 1.000 . Uiso c ? H(43) 0.3008 -0.2702 0.0889 0.081 1.000 . Uiso c ? H(44) 0.4396 -0.1488 0.1140 0.095 1.000 . Uiso c ? H(45) 0.4234 0.0563 0.0992 0.076 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Y(1) 0.029(1) 0.0144(9) 0.038(1) -0.001(1) 0.0009(9) 0.002(1) P(1) 0.027(3) 0.024(3) 0.040(4) 0.001(3) -0.002(3) 0.005(3) P(2) 0.037(4) 0.021(3) 0.031(3) -0.001(3) -0.002(3) -0.002(3) P(3) 0.058(4) 0.024(3) 0.042(4) -0.011(3) -0.009(3) 0.008(3) O(1) 0.032(9) 0.033(9) 0.052(9) -0.003(7) 0.017(8) 0.014(7) O(2) 0.05(1) 0.029(8) 0.035(9) -0.002(8) 0.003(8) -0.004(7) O(3) 0.07(1) 0.023(8) 0.04(1) -0.009(8) 0.015(8) -0.002(7) O(4) 0.020(8) 0.06(1) 0.08(1) -0.022(8) 0.010(8) -0.013(9) O(5) 0.042(9) 0.051(9) 0.033(9) -0.007(8) 0.005(7) -0.007(8) O(6) 0.06(1) 0.011(7) 0.06(1) -0.010(7) 0.015(9) -0.006(7) O(7) 0.11(2) 0.05(1) 0.08(1) 0.04(1) 0.01(1) 0.04(1) O(8) 0.05(1) 0.021(8) 0.06(1) 0.010(8) 0.008(8) 0.008(8) O(9) 0.05(1) 0.035(9) 0.04(1) 0.020(8) 0.011(8) -0.003(7) O(10) 0.10(1) 0.038(9) 0.06(1) -0.004(9) -0.03(1) 0.030(8) O(11) 0.032(9) 0.022(8) 0.048(9) -0.009(7) -0.010(7) -0.001(7) O(12) 0.040(9) 0.017(7) 0.043(9) 0.007(7) -0.014(7) 0.010(7) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2941 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0868 _refine_ls_wR_factor_all 0.0947 _refine_ls_wR_factor_ref 0.0947 _refine_ls_goodness_of_fit_all 2.695 _refine_ls_goodness_of_fit_ref 2.695 _refine_ls_shift/su_max 0.0890 _refine_ls_shift/su_mean 0.0180 _refine_diff_density_min -0.69 _refine_diff_density_max 2.16 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y(1) O(1) 2.29(1) . . yes Y(1) O(2) 2.24(1) . . yes Y(1) O(3) 2.25(1) . . yes Y(1) O(5) 2.48(1) . . yes Y(1) O(6) 2.43(1) . . yes Y(1) O(8) 2.46(1) . . yes Y(1) O(9) 2.45(1) . . yes Y(1) O(11) 2.44(1) . . yes Y(1) O(12) 2.49(1) . . yes P(1) O(1) 1.48(1) . . yes P(1) C(1) 1.82(2) . . yes P(1) C(7) 1.79(2) . . yes P(1) C(13) 1.79(2) . . yes P(2) O(2) 1.50(1) . . yes P(2) C(19) 1.78(2) . . yes P(2) C(25) 1.80(2) . . yes P(2) C(31) 1.80(2) . . yes P(3) O(3) 1.50(1) . . yes P(3) C(37) 1.81(2) . . yes P(3) C(49) 1.81(2) . . yes P(3) C(43) 1.84(2) . . yes O(4) N(1) 1.20(2) . . yes O(5) N(1) 1.29(2) . . yes O(6) N(1) 1.26(2) . . yes O(7) N(2) 1.23(3) . . yes O(8) N(2) 1.27(2) . . yes O(9) N(2) 1.27(2) . . yes O(10) N(3) 1.21(2) . . yes O(11) N(3) 1.28(2) . . yes O(12) N(3) 1.27(2) . . yes C(1) C(2) 1.37(3) . . yes C(1) C(6) 1.41(3) . . yes C(2) C(3) 1.33(3) . . yes C(2) H(1) 0.95 . . no C(3) C(4) 1.36(3) . . yes C(3) H(2) 0.95 . . no C(4) C(5) 1.39(3) . . yes C(4) H(3) 0.95 . . no C(5) C(6) 1.39(3) . . yes C(5) H(4) 0.95 . . no C(6) H(5) 0.95 . . no C(7) C(8) 1.38(3) . . yes C(7) C(12) 1.42(3) . . yes C(8) C(9) 1.37(3) . . yes C(8) H(6) 0.95 . . no C(9) C(10) 1.39(3) . . yes C(9) H(7) 0.95 . . no C(10) C(11) 1.39(3) . . yes C(10) H(8) 0.95 . . no C(11) C(12) 1.37(3) . . yes C(11) H(9) 0.95 . . no C(12) H(10) 0.95 . . no C(13) C(14) 1.39(3) . . yes C(13) C(18) 1.40(3) . . yes C(14) C(15) 1.43(4) . . yes C(14) H(11) 0.95 . . no C(15) C(16) 1.41(4) . . yes C(15) H(12) 0.95 . . no C(16) C(17) 1.33(3) . . yes C(16) H(13) 0.95 . . no C(17) C(18) 1.38(3) . . yes C(17) H(14) 0.95 . . no C(18) H(15) 0.95 . . no C(19) C(20) 1.38(3) . . yes C(19) C(24) 1.39(3) . . yes C(20) C(21) 1.39(3) . . yes C(20) H(16) 0.95 . . no C(21) C(22) 1.37(3) . . yes C(21) H(17) 0.95 . . no C(22) C(23) 1.42(3) . . yes C(22) H(18) 0.95 . . no C(23) C(24) 1.42(3) . . yes C(23) H(19) 0.95 . . no C(24) H(20) 0.95 . . no C(25) C(26) 1.35(3) . . yes C(25) C(30) 1.41(3) . . yes C(26) C(27) 1.41(3) . . yes C(26) H(21) 0.95 . . no C(27) C(28) 1.36(3) . . yes C(27) H(22) 0.95 . . no C(28) C(29) 1.38(3) . . yes C(28) H(23) 0.95 . . no C(29) C(30) 1.39(3) . . yes C(29) H(24) 0.95 . . no C(30) H(25) 0.95 . . no C(31) C(32) 1.40(3) . . yes C(31) C(36) 1.39(3) . . yes C(32) C(33) 1.36(3) . . yes C(32) H(26) 0.95 . . no C(33) C(34) 1.36(3) . . yes C(33) H(27) 0.95 . . no C(34) C(35) 1.39(3) . . yes C(34) H(28) 0.95 . . no C(35) C(36) 1.38(3) . . yes C(35) H(29) 0.95 . . no C(36) H(30) 0.95 . . no C(37) C(38) 1.39(3) . . yes C(37) C(42) 1.37(3) . . yes C(38) C(39) 1.40(3) . . yes C(38) H(31) 0.95 . . no C(39) C(40) 1.37(3) . . yes C(39) H(32) 0.95 . . no C(40) C(41) 1.42(3) . . yes C(40) H(33) 0.95 . . no C(41) C(42) 1.36(3) . . yes C(41) H(34) 0.95 . . no C(42) H(35) 0.95 . . no C(49) C(50) 1.33(3) . . yes C(49) C(54) 1.41(3) . . yes C(50) C(51) 1.48(3) . . yes C(50) H(41) 0.95 . . no C(51) C(52) 1.31(3) . . yes C(51) H(42) 0.95 . . no C(52) C(53) 1.34(4) . . yes C(52) H(43) 0.95 . . no C(53) C(54) 1.44(3) . . yes C(53) H(44) 0.95 . . no C(54) H(45) 0.95 . . no C(43) C(44) 1.39(3) . . yes C(43) C(57) 1.39(3) . . yes C(44) C(45) 1.39(3) . . yes C(45) C(55) 1.39(3) . . yes C(55) C(56) 1.39(3) . . yes C(56) C(57) 1.39(3) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Y(1) O(2) 86.1(4) . . . yes O(1) Y(1) O(3) 82.9(5) . . . yes O(1) Y(1) O(5) 152.2(4) . . . yes O(1) Y(1) O(6) 146.4(4) . . . yes O(1) Y(1) O(8) 77.0(4) . . . yes O(1) Y(1) O(9) 81.2(4) . . . yes O(1) Y(1) O(11) 127.8(4) . . . yes O(1) Y(1) O(12) 76.0(4) . . . yes O(2) Y(1) O(3) 150.4(4) . . . yes O(2) Y(1) O(5) 73.4(4) . . . yes O(2) Y(1) O(6) 124.2(5) . . . yes O(2) Y(1) O(8) 126.9(4) . . . yes O(2) Y(1) O(9) 76.3(4) . . . yes O(2) Y(1) O(11) 86.1(4) . . . yes O(2) Y(1) O(12) 77.8(4) . . . yes O(3) Y(1) O(5) 123.9(4) . . . yes O(3) Y(1) O(6) 76.1(5) . . . yes O(3) Y(1) O(8) 77.0(4) . . . yes O(3) Y(1) O(9) 128.5(4) . . . yes O(3) Y(1) O(11) 79.2(4) . . . yes O(3) Y(1) O(12) 72.8(4) . . . yes O(5) Y(1) O(6) 50.9(4) . . . yes O(5) Y(1) O(8) 100.3(4) . . . yes O(5) Y(1) O(9) 75.9(4) . . . yes O(5) Y(1) O(11) 70.4(4) . . . yes O(5) Y(1) O(12) 116.3(4) . . . yes O(6) Y(1) O(8) 73.0(4) . . . yes O(6) Y(1) O(9) 91.6(4) . . . yes O(6) Y(1) O(11) 73.7(4) . . . yes O(6) Y(1) O(12) 120.8(4) . . . yes O(8) Y(1) O(9) 51.8(4) . . . yes O(8) Y(1) O(11) 142.7(4) . . . yes O(8) Y(1) O(12) 141.4(4) . . . yes O(9) Y(1) O(11) 145.2(4) . . . yes O(9) Y(1) O(12) 146.4(4) . . . yes O(11) Y(1) O(12) 51.9(4) . . . yes O(1) P(1) C(1) 109.9(8) . . . yes O(1) P(1) C(7) 110.4(8) . . . yes O(1) P(1) C(13) 112.3(8) . . . yes C(1) P(1) C(7) 108.4(8) . . . yes C(1) P(1) C(13) 107.4(8) . . . yes C(7) P(1) C(13) 108.3(9) . . . yes O(2) P(2) C(19) 110.6(8) . . . yes O(2) P(2) C(25) 110.3(8) . . . yes O(2) P(2) C(31) 110.6(8) . . . yes C(19) P(2) C(25) 107.7(9) . . . yes C(19) P(2) C(31) 109.4(9) . . . yes C(25) P(2) C(31) 108.2(9) . . . yes O(3) P(3) C(37) 108.1(9) . . . yes O(3) P(3) C(49) 111.0(9) . . . yes O(3) P(3) C(43) 107.1(9) . . . yes C(37) P(3) C(49) 110(1) . . . yes C(37) P(3) C(43) 112.9(9) . . . yes C(49) P(3) C(43) 107.6(9) . . . yes Y(1) O(1) P(1) 163.7(8) . . . yes Y(1) O(2) P(2) 173.9(8) . . . yes Y(1) O(3) P(3) 159.7(9) . . . yes Y(1) O(5) N(1) 97(1) . . . yes Y(1) O(6) N(1) 100(1) . . . yes Y(1) O(8) N(2) 96(1) . . . yes Y(1) O(9) N(2) 97(1) . . . yes Y(1) O(11) N(3) 97(1) . . . yes Y(1) O(12) N(3) 95(1) . . . yes O(4) N(1) O(5) 125(2) . . . yes O(4) N(1) O(6) 124(2) . . . yes O(5) N(1) O(6) 111(2) . . . yes O(7) N(2) O(8) 121(2) . . . yes O(7) N(2) O(9) 124(2) . . . yes O(8) N(2) O(9) 115(2) . . . yes O(10) N(3) O(11) 122(2) . . . yes O(10) N(3) O(12) 122(2) . . . yes O(11) N(3) O(12) 115(2) . . . yes P(1) C(1) C(2) 120(1) . . . yes P(1) C(1) C(6) 120(1) . . . yes C(2) C(1) C(6) 120(2) . . . yes C(1) C(2) C(3) 124(2) . . . yes C(1) C(2) H(1) 118.2 . . . no C(3) C(2) H(1) 118.0 . . . no C(2) C(3) C(4) 117(2) . . . yes C(2) C(3) H(2) 121.7 . . . no C(4) C(3) H(2) 121.6 . . . no C(3) C(4) C(5) 123(2) . . . yes C(3) C(4) H(3) 118.6 . . . no C(5) C(4) H(3) 118.7 . . . no C(4) C(5) C(6) 120(2) . . . yes C(4) C(5) H(4) 119.9 . . . no C(6) C(5) H(4) 119.9 . . . no C(1) C(6) C(5) 116(2) . . . yes C(1) C(6) H(5) 121.9 . . . no C(5) C(6) H(5) 121.9 . . . no P(1) C(7) C(8) 119(1) . . . yes P(1) C(7) C(12) 121(1) . . . yes C(8) C(7) C(12) 120(2) . . . yes C(7) C(8) C(9) 121(2) . . . yes C(7) C(8) H(6) 119.3 . . . no C(9) C(8) H(6) 119.4 . . . no C(8) C(9) C(10) 119(2) . . . yes C(8) C(9) H(7) 120.3 . . . no C(10) C(9) H(7) 120.5 . . . no C(9) C(10) C(11) 120(2) . . . yes C(9) C(10) H(8) 120.1 . . . no C(11) C(10) H(8) 120.1 . . . no C(10) C(11) C(12) 122(2) . . . yes C(10) C(11) H(9) 119.0 . . . no C(12) C(11) H(9) 119.0 . . . no C(7) C(12) C(11) 117(2) . . . yes C(7) C(12) H(10) 121.4 . . . no C(11) C(12) H(10) 121.4 . . . no P(1) C(13) C(14) 119(2) . . . yes P(1) C(13) C(18) 120(2) . . . yes C(14) C(13) C(18) 120(2) . . . yes C(13) C(14) C(15) 121(2) . . . yes C(13) C(14) H(11) 119.7 . . . no C(15) C(14) H(11) 119.7 . . . no C(14) C(15) C(16) 115(2) . . . yes C(14) C(15) H(12) 122.2 . . . no C(16) C(15) H(12) 122.3 . . . no C(15) C(16) C(17) 123(2) . . . yes C(15) C(16) H(13) 118.5 . . . no C(17) C(16) H(13) 118.5 . . . no C(16) C(17) C(18) 122(2) . . . yes C(16) C(17) H(14) 119.0 . . . no C(18) C(17) H(14) 118.9 . . . no C(13) C(18) C(17) 118(2) . . . yes C(13) C(18) H(15) 120.8 . . . no C(17) C(18) H(15) 120.8 . . . no P(2) C(19) C(20) 120(2) . . . yes P(2) C(19) C(24) 120(2) . . . yes C(20) C(19) C(24) 120(2) . . . yes C(19) C(20) C(21) 120(2) . . . yes C(19) C(20) H(16) 119.9 . . . no C(21) C(20) H(16) 120.0 . . . no C(20) C(21) C(22) 121(2) . . . yes C(20) C(21) H(17) 119.3 . . . no C(22) C(21) H(17) 119.4 . . . no C(21) C(22) C(23) 120(2) . . . yes C(21) C(22) H(18) 120.1 . . . no C(23) C(22) H(18) 120.0 . . . no C(22) C(23) C(24) 118(2) . . . yes C(22) C(23) H(19) 121.0 . . . no C(24) C(23) H(19) 120.9 . . . no C(19) C(24) C(23) 120(2) . . . yes C(19) C(24) H(20) 119.7 . . . no C(23) C(24) H(20) 119.9 . . . no P(2) C(25) C(26) 120(1) . . . yes P(2) C(25) C(30) 121(1) . . . yes C(26) C(25) C(30) 119(2) . . . yes C(25) C(26) C(27) 120(2) . . . yes C(25) C(26) H(21) 120.1 . . . no C(27) C(26) H(21) 120.0 . . . no C(26) C(27) C(28) 121(2) . . . yes C(26) C(27) H(22) 119.5 . . . no C(28) C(27) H(22) 119.5 . . . no C(27) C(28) C(29) 120(2) . . . yes C(27) C(28) H(23) 120.0 . . . no C(29) C(28) H(23) 120.1 . . . no C(28) C(29) C(30) 120(2) . . . yes C(28) C(29) H(24) 120.1 . . . no C(30) C(29) H(24) 120.1 . . . no C(25) C(30) C(29) 120(2) . . . yes C(25) C(30) H(25) 120.0 . . . no C(29) C(30) H(25) 120.1 . . . no P(2) C(31) C(32) 125(1) . . . yes P(2) C(31) C(36) 116(1) . . . yes C(32) C(31) C(36) 119(2) . . . yes C(31) C(32) C(33) 119(2) . . . yes C(31) C(32) H(26) 120.5 . . . no C(33) C(32) H(26) 120.7 . . . no C(32) C(33) C(34) 123(2) . . . yes C(32) C(33) H(27) 118.3 . . . no C(34) C(33) H(27) 118.4 . . . no C(33) C(34) C(35) 118(2) . . . yes C(33) C(34) H(28) 121.0 . . . no C(35) C(34) H(28) 120.9 . . . no C(34) C(35) C(36) 121(2) . . . yes C(34) C(35) H(29) 119.5 . . . no C(36) C(35) H(29) 119.5 . . . no C(31) C(36) C(35) 120(2) . . . yes C(31) C(36) H(30) 120.2 . . . no C(35) C(36) H(30) 120.2 . . . no P(3) C(37) C(38) 118(2) . . . yes P(3) C(37) C(42) 121(2) . . . yes C(38) C(37) C(42) 121(2) . . . yes C(37) C(38) C(39) 119(2) . . . yes C(37) C(38) H(31) 120.7 . . . no C(39) C(38) H(31) 120.6 . . . no C(38) C(39) C(40) 120(2) . . . yes C(38) C(39) H(32) 119.8 . . . no C(40) C(39) H(32) 120.0 . . . no C(39) C(40) C(41) 120(2) . . . yes C(39) C(40) H(33) 120.1 . . . no C(41) C(40) H(33) 120.1 . . . no C(40) C(41) C(42) 120(2) . . . yes C(40) C(41) H(34) 120.2 . . . no C(42) C(41) H(34) 120.3 . . . no C(37) C(42) C(41) 121(2) . . . yes C(37) C(42) H(35) 119.7 . . . no C(41) C(42) H(35) 119.7 . . . no P(3) C(49) C(50) 124(2) . . . yes P(3) C(49) C(54) 115(2) . . . yes C(50) C(49) C(54) 121(2) . . . yes C(49) C(50) C(51) 117(2) . . . yes C(49) C(50) H(41) 121.7 . . . no C(51) C(50) H(41) 121.7 . . . no C(50) C(51) C(52) 119(2) . . . yes C(50) C(51) H(42) 120.7 . . . no C(52) C(51) H(42) 120.5 . . . no C(51) C(52) C(53) 128(2) . . . yes C(51) C(52) H(43) 115.9 . . . no C(53) C(52) H(43) 115.9 . . . no C(52) C(53) C(54) 113(2) . . . yes C(52) C(53) H(44) 123.3 . . . no C(54) C(53) H(44) 123.4 . . . no C(49) C(54) C(53) 122(2) . . . yes C(49) C(54) H(45) 119.2 . . . no C(53) C(54) H(45) 119.1 . . . no P(3) C(43) C(44) 116(1) . . . yes P(3) C(43) C(57) 124(2) . . . yes C(44) C(43) C(57) 120(2) . . . yes C(43) C(44) C(45) 120(2) . . . yes C(44) C(45) C(55) 120(2) . . . yes C(45) C(55) C(56) 120(2) . . . yes C(55) C(56) C(57) 120(2) . . . yes C(43) C(57) C(56) 120(2) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag P(3) C(43) 1.84(2) . . no P(3) C(44) 2.75(2) . . no P(3) C(57) 2.86(3) . . no O(3) C(43) 2.69(2) . . no O(3) C(57) 3.37(3) . . no O(4) C(18) 3.18(2) . 1_455 no O(4) C(13) 3.19(2) . 1_455 no O(4) C(17) 3.42(3) . 1_455 no O(4) C(23) 3.45(3) . 2_545 no O(4) C(14) 3.45(3) . 1_455 no O(4) C(22) 3.49(3) . 2_545 no O(4) C(6) 3.50(2) . 1_455 no O(5) C(6) 3.51(2) . 1_455 no O(6) C(57) 3.16(2) . . no O(6) C(29) 3.34(2) . 1_545 no O(7) C(3) 3.21(3) . 2_645 no O(7) C(4) 3.42(3) . 2_645 no O(7) C(33) 3.44(3) . 2_645 no O(9) C(33) 3.57(2) . 2_645 no O(10) C(45) 3.25(2) . 3_565 no O(10) C(51) 3.28(3) . 1_565 no O(10) C(52) 3.39(3) . 1_565 no O(10) C(55) 3.40(2) . 3_565 no O(11) C(57) 3.39(2) . . no O(11) C(11) 3.46(3) . 1_455 no O(11) C(43) 3.51(2) . . no O(12) C(52) 3.52(3) . 1_565 no C(3) C(32) 3.46(3) . 2_645 no C(37) C(43) 3.03(3) . . no C(37) C(44) 3.19(3) . . no C(49) C(43) 2.94(3) . . no C(49) C(57) 3.45(3) . . no C(50) C(43) 3.21(3) . . no C(50) C(57) 3.42(3) . . no C(45) C(45) 3.59(3) . 3_565 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Y(1) O(1) P(1) C(1) . . . . -117(3) no Y(1) O(1) P(1) C(7) . . . . 123(3) no Y(1) O(1) P(1) C(13) . . . . 2(3) no Y(1) O(2) P(2) C(19) . . . . -172(7) no Y(1) O(2) P(2) C(25) . . . . 69(8) no Y(1) O(2) P(2) C(31) . . . . -51(8) no Y(1) O(3) P(3) C(37) . . . . 174(2) no Y(1) O(3) P(3) C(49) . . . . -65(3) no Y(1) O(3) P(3) C(43) . . . . 52(2) no Y(1) O(5) N(1) O(4) . . . . -172(2) no Y(1) O(5) N(1) O(6) . . . . 7(2) no Y(1) O(6) N(1) O(4) . . . . 172(2) no Y(1) O(6) N(1) O(5) . . . . -8(2) no Y(1) O(8) N(2) O(7) . . . . -176(2) no Y(1) O(8) N(2) O(9) . . . . 1(2) no Y(1) O(9) N(2) O(7) . . . . 176(2) no Y(1) O(9) N(2) O(8) . . . . -1(2) no Y(1) O(11) N(3) O(10) . . . . 170(2) no Y(1) O(11) N(3) O(12) . . . . -8(2) no Y(1) O(12) N(3) O(10) . . . . -170(2) no Y(1) O(12) N(3) O(11) . . . . 8(2) no P(1) O(1) Y(1) O(2) . . . . 152(3) no P(1) O(1) Y(1) O(3) . . . . -55(3) no P(1) O(1) Y(1) O(5) . . . . 110(3) no P(1) O(1) Y(1) O(6) . . . . -4(3) no P(1) O(1) Y(1) O(8) . . . . 23(3) no P(1) O(1) Y(1) O(9) . . . . 75(3) no P(1) O(1) Y(1) O(11) . . . . -126(3) no P(1) O(1) Y(1) O(12) . . . . -129(3) no P(1) C(1) C(2) C(3) . . . . -176(2) no P(1) C(1) C(6) C(5) . . . . 175(1) no P(1) C(7) C(8) C(9) . . . . 173(2) no P(1) C(7) C(12) C(11) . . . . -173(2) no P(1) C(13) C(14) C(15) . . . . -178(2) no P(1) C(13) C(18) C(17) . . . . 175(2) no P(2) O(2) Y(1) O(1) . . . . 51(8) no P(2) O(2) Y(1) O(3) . . . . -17(8) no P(2) O(2) Y(1) O(5) . . . . -148(8) no P(2) O(2) Y(1) O(6) . . . . -145(8) no P(2) O(2) Y(1) O(8) . . . . 121(8) no P(2) O(2) Y(1) O(9) . . . . 133(8) no P(2) O(2) Y(1) O(11) . . . . -77(8) no P(2) O(2) Y(1) O(12) . . . . -26(8) no P(2) C(19) C(20) C(21) . . . . -178(2) no P(2) C(19) C(24) C(23) . . . . 178(2) no P(2) C(25) C(26) C(27) . . . . 178(2) no P(2) C(25) C(30) C(29) . . . . 179(2) no P(2) C(31) C(32) C(33) . . . . 179(2) no P(2) C(31) C(36) C(35) . . . . -177(2) no P(3) O(3) Y(1) O(1) . . . . 163(2) no P(3) O(3) Y(1) O(2) . . . . -128(2) no P(3) O(3) Y(1) O(5) . . . . -9(3) no P(3) O(3) Y(1) O(6) . . . . 10(2) no P(3) O(3) Y(1) O(8) . . . . 85(2) no P(3) O(3) Y(1) O(9) . . . . 90(2) no P(3) O(3) Y(1) O(11) . . . . -66(2) no P(3) O(3) Y(1) O(12) . . . . -119(2) no P(3) C(37) C(38) C(39) . . . . -180(2) no P(3) C(37) C(42) C(41) . . . . 177(2) no P(3) C(49) C(50) C(51) . . . . -179(2) no P(3) C(49) C(54) C(53) . . . . -180(2) no P(3) C(43) C(44) C(45) . . . . -175(1) no P(3) C(43) C(57) C(56) . . . . 174(2) no O(1) Y(1) O(5) N(1) . . . . -144(1) no O(1) Y(1) O(6) N(1) . . . . 152(1) no O(1) Y(1) O(8) N(2) . . . . 89(1) no O(1) Y(1) O(9) N(2) . . . . -80(1) no O(1) Y(1) O(11) N(3) . . . . 0(1) no O(1) Y(1) O(12) N(3) . . . . 171(1) no O(1) P(1) C(1) C(2) . . . . 12(2) no O(1) P(1) C(1) C(6) . . . . -162(1) no O(1) P(1) C(7) C(8) . . . . 14(2) no O(1) P(1) C(7) C(12) . . . . -170(1) no O(1) P(1) C(13) C(14) . . . . 90(2) no O(1) P(1) C(13) C(18) . . . . -86(2) no O(2) Y(1) O(5) N(1) . . . . 172(1) no O(2) Y(1) O(6) N(1) . . . . 1(1) no O(2) Y(1) O(8) N(2) . . . . 14(1) no O(2) Y(1) O(9) N(2) . . . . -168(1) no O(2) Y(1) O(11) N(3) . . . . 82(1) no O(2) Y(1) O(12) N(3) . . . . -100(1) no O(2) P(2) C(19) C(20) . . . . 15(2) no O(2) P(2) C(19) C(24) . . . . -164(2) no O(2) P(2) C(25) C(26) . . . . 42(2) no O(2) P(2) C(25) C(30) . . . . -139(2) no O(2) P(2) C(31) C(32) . . . . -131(2) no O(2) P(2) C(31) C(36) . . . . 49(2) no O(3) Y(1) O(5) N(1) . . . . 19(1) no O(3) Y(1) O(6) N(1) . . . . -155(1) no O(3) Y(1) O(8) N(2) . . . . 174(1) no O(3) Y(1) O(9) N(2) . . . . -6(1) no O(3) Y(1) O(11) N(3) . . . . -72(1) no O(3) Y(1) O(12) N(3) . . . . 85(1) no O(3) P(3) C(37) C(38) . . . . -25(2) no O(3) P(3) C(37) C(42) . . . . 160(2) no O(3) P(3) C(49) C(50) . . . . 137(2) no O(3) P(3) C(49) C(54) . . . . -44(2) no O(3) P(3) C(43) C(44) . . . . 108(2) no O(3) P(3) C(43) C(57) . . . . -66(2) no O(5) Y(1) O(6) N(1) . . . . 5(1) no O(5) Y(1) O(8) N(2) . . . . -63(1) no O(5) Y(1) O(9) N(2) . . . . 116(1) no O(5) Y(1) O(11) N(3) . . . . 156(1) no O(5) Y(1) O(12) N(3) . . . . -35(1) no O(6) Y(1) O(5) N(1) . . . . -4.6(9) no O(6) Y(1) O(8) N(2) . . . . -107(1) no O(6) Y(1) O(9) N(2) . . . . 67(1) no O(6) Y(1) O(11) N(3) . . . . -150(1) no O(6) Y(1) O(12) N(3) . . . . 23(1) no O(8) Y(1) O(5) N(1) . . . . -63(1) no O(8) Y(1) O(6) N(1) . . . . 124(1) no O(8) Y(1) O(9) N(2) . . . . 0(1) no O(8) Y(1) O(11) N(3) . . . . -123(1) no O(8) Y(1) O(12) N(3) . . . . 125(1) no O(9) Y(1) O(5) N(1) . . . . -109(1) no O(9) Y(1) O(6) N(1) . . . . 75(1) no O(9) Y(1) O(8) N(2) . . . . 0(1) no O(9) Y(1) O(11) N(3) . . . . 141(1) no O(9) Y(1) O(12) N(3) . . . . -140(1) no O(11) Y(1) O(5) N(1) . . . . 80(1) no O(11) Y(1) O(6) N(1) . . . . -73(1) no O(11) Y(1) O(8) N(2) . . . . -134(1) no O(11) Y(1) O(9) N(2) . . . . 130(1) no O(11) Y(1) O(12) N(3) . . . . -4.9(9) no O(12) Y(1) O(5) N(1) . . . . 105(1) no O(12) Y(1) O(6) N(1) . . . . -96(1) no O(12) Y(1) O(8) N(2) . . . . 135(1) no O(12) Y(1) O(9) N(2) . . . . -127(1) no O(12) Y(1) O(11) N(3) . . . . 4.9(9) no C(1) P(1) C(7) C(8) . . . . -106(2) no C(1) P(1) C(7) C(12) . . . . 70(2) no C(1) P(1) C(13) C(14) . . . . -149(2) no C(1) P(1) C(13) C(18) . . . . 35(2) no C(1) C(2) C(3) C(4) . . . . 2(3) no C(1) C(6) C(5) C(4) . . . . 1(3) no C(2) C(1) P(1) C(7) . . . . 133(2) no C(2) C(1) P(1) C(13) . . . . -110(2) no C(2) C(1) C(6) C(5) . . . . 1(3) no C(2) C(3) C(4) C(5) . . . . -1(3) no C(3) C(2) C(1) C(6) . . . . -2(3) no C(3) C(4) C(5) C(6) . . . . 0(3) no C(6) C(1) P(1) C(7) . . . . -41(2) no C(6) C(1) P(1) C(13) . . . . 76(2) no C(7) P(1) C(13) C(14) . . . . -32(2) no C(7) P(1) C(13) C(18) . . . . 152(2) no C(7) C(8) C(9) C(10) . . . . 0(3) no C(7) C(12) C(11) C(10) . . . . -1(3) no C(8) C(7) P(1) C(13) . . . . 138(2) no C(8) C(7) C(12) C(11) . . . . 3(3) no C(8) C(9) C(10) C(11) . . . . 2(3) no C(9) C(8) C(7) C(12) . . . . -3(3) no C(9) C(10) C(11) C(12) . . . . -1(3) no C(12) C(7) P(1) C(13) . . . . -46(2) no C(13) C(14) C(15) C(16) . . . . 5(4) no C(13) C(18) C(17) C(16) . . . . 0(3) no C(14) C(13) C(18) C(17) . . . . 0(3) no C(14) C(15) C(16) C(17) . . . . -5(4) no C(15) C(14) C(13) C(18) . . . . -2(3) no C(15) C(16) C(17) C(18) . . . . 3(4) no C(19) P(2) C(25) C(26) . . . . -79(2) no C(19) P(2) C(25) C(30) . . . . 100(2) no C(19) P(2) C(31) C(32) . . . . -9(2) no C(19) P(2) C(31) C(36) . . . . 171(1) no C(19) C(20) C(21) C(22) . . . . -1(3) no C(19) C(24) C(23) C(22) . . . . 2(3) no C(20) C(19) P(2) C(25) . . . . 135(2) no C(20) C(19) P(2) C(31) . . . . -108(2) no C(20) C(19) C(24) C(23) . . . . -1(3) no C(20) C(21) C(22) C(23) . . . . 2(3) no C(21) C(20) C(19) C(24) . . . . 1(3) no C(21) C(22) C(23) C(24) . . . . -2(3) no C(24) C(19) P(2) C(25) . . . . -44(2) no C(24) C(19) P(2) C(31) . . . . 74(2) no C(25) P(2) C(31) C(32) . . . . 108(2) no C(25) P(2) C(31) C(36) . . . . -72(2) no C(25) C(26) C(27) C(28) . . . . 1(3) no C(25) C(30) C(29) C(28) . . . . 4(3) no C(26) C(25) P(2) C(31) . . . . 163(2) no C(26) C(25) C(30) C(29) . . . . -1(3) no C(26) C(27) C(28) C(29) . . . . 2(3) no C(27) C(26) C(25) C(30) . . . . -1(3) no C(27) C(28) C(29) C(30) . . . . -4(3) no C(30) C(25) P(2) C(31) . . . . -18(2) no C(31) C(32) C(33) C(34) . . . . 0(3) no C(31) C(36) C(35) C(34) . . . . -3(3) no C(32) C(31) C(36) C(35) . . . . 3(3) no C(32) C(33) C(34) C(35) . . . . -1(3) no C(33) C(32) C(31) C(36) . . . . -1(3) no C(33) C(34) C(35) C(36) . . . . 2(3) no C(37) P(3) C(49) C(50) . . . . -103(2) no C(37) P(3) C(49) C(54) . . . . 76(2) no C(37) P(3) C(43) C(44) . . . . -10(2) no C(37) P(3) C(43) C(57) . . . . 175(2) no C(37) C(38) C(39) C(40) . . . . 2(3) no C(37) C(42) C(41) C(40) . . . . 2(4) no C(38) C(37) P(3) C(49) . . . . -146(2) no C(38) C(37) P(3) C(43) . . . . 93(2) no C(38) C(37) C(42) C(41) . . . . 2(3) no C(38) C(39) C(40) C(41) . . . . 2(3) no C(39) C(38) C(37) C(42) . . . . -4(3) no C(39) C(40) C(41) C(42) . . . . -4(4) no C(42) C(37) P(3) C(49) . . . . 38(2) no C(42) C(37) P(3) C(43) . . . . -82(2) no C(49) P(3) C(43) C(44) . . . . -132(2) no C(49) P(3) C(43) C(57) . . . . 53(2) no C(49) C(50) C(51) C(52) . . . . -2(3) no C(49) C(54) C(53) C(52) . . . . -1(4) no C(50) C(49) P(3) C(43) . . . . 20(2) no C(50) C(49) C(54) C(53) . . . . 0(4) no C(50) C(51) C(52) C(53) . . . . 1(4) no C(51) C(50) C(49) C(54) . . . . 2(3) no C(51) C(52) C(53) C(54) . . . . 1(4) no C(54) C(49) P(3) C(43) . . . . -160(2) no C(43) C(44) C(45) C(55) . . . . 0(3) no C(43) C(57) C(56) C(55) . . . . 0(3) no C(44) C(43) C(57) C(56) . . . . 0(3) no C(44) C(45) C(55) C(56) . . . . 0(3) no C(45) C(44) C(43) C(57) . . . . 0(3) no C(45) C(55) C(56) C(57) . . . . 0(3) no #===END #======= end of file ==============