# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2123 data_COMPOUND(1) #------------------------------------------------------------------------------ _audit_creation_date 'Wed Oct 27 09:30:47 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 5.1224(9) _cell_length_b 17.356(2) _cell_length_c 8.934(1) _cell_angle_alpha 90 _cell_angle_beta 100.53(1) _cell_angle_gamma 90 _cell_volume 780.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 22.4 _cell_measurement_theta_max 39.4 #------------------------------------------------------------------------------ _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' #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'clear' _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.060 _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_meas ? _chemical_formula_weight 186.10 _chemical_formula_analytical ? _chemical_formula_sum 'C3 H11 N2 O5 P ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 392.00 _exptl_absorpt_coefficient_mu 0.334 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 295.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.42 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 0 2 0 4 1 -1 1 2 _diffrn_reflns_number 2584 _reflns_number_total 2353 _reflns_number_observed 1405 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 3.30 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 29.97 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.06341 _diffrn_orient_matrix_UB_12 0.02425 _diffrn_orient_matrix_UB_13 0.10168 _diffrn_orient_matrix_UB_21 0.01989 _diffrn_orient_matrix_UB_22 0.05047 _diffrn_orient_matrix_UB_23 -0.05074 _diffrn_orient_matrix_UB_31 -0.18711 _diffrn_orient_matrix_UB_32 0.01358 _diffrn_orient_matrix_UB_33 0.00698 #------------------------------------------------------------------------------ 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 12 0.003 0.002 'International Tables' H 0 44 0.000 0.000 'International Tables' N 0 8 0.006 0.003 'International Tables' O 0 20 0.011 0.006 'International Tables' P 0 4 0.102 0.094 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom P(1) 0.72295(10) 0.21978(3) 0.73140(5) 0.0187(1) Uij ? ? O(1) -0.0630(3) 0.45428(9) 0.7034(2) 0.0322(4) Uij ? ? O(2) 0.3589(3) 0.44637(10) 0.8249(2) 0.0333(4) Uij ? ? O(3) 0.6175(3) 0.15611(8) 0.8169(1) 0.0266(3) Uij ? ? O(4) 0.9373(3) 0.26908(10) 0.8378(2) 0.0305(4) Uij ? ? O(5) 0.8391(3) 0.19561(8) 0.5967(1) 0.0271(4) Uij ? ? N(1) 0.4991(3) 0.35757(9) 0.6007(2) 0.0194(4) Uij ? ? N(2) 0.2193(4) 0.4307(1) 1.1153(2) 0.0258(4) Uij ? ? C(1) 0.1777(4) 0.4381(1) 0.7127(2) 0.0221(4) Uij ? ? C(2) 0.2570(4) 0.4069(1) 0.5676(2) 0.0233(5) Uij ? ? C(3) 0.4450(4) 0.2841(1) 0.6737(3) 0.0271(5) Uij ? ? H(1) 0.393(5) 0.409(1) 1.181(3) 0.055(8) Uij ? ? H(2) 0.267(5) 0.444(1) 1.035(3) 0.045(8) Uij ? ? H(3) 0.075(5) 0.396(2) 1.108(3) 0.054(8) Uij ? ? H(4) 0.155(6) 0.482(2) 1.169(3) 0.071(9) Uij ? ? H(5) 0.125(4) 0.378(1) 0.510(2) 0.027(6) Uij ? ? H(6) 0.289(5) 0.452(1) 0.506(3) 0.048(7) Uij ? ? H(9) 0.643(4) 0.389(1) 0.662(3) 0.033(6) Uij ? ? H(10) 0.560(4) 0.351(1) 0.517(3) 0.032(6) Uij ? ? H(11) 0.360(5) 0.295(2) 0.752(3) 0.054(8) Uij ? ? H(12) 0.324(4) 0.258(1) 0.608(3) 0.036(6) Uij ? ? H(13) 0.920(7) 0.285(2) 0.904(4) 0.11(1) Uij ? ? 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 P(1) 0.0209(2) 0.0210(2) 0.0152(2) 0.0003(2) 0.0058(1) -0.0001(2) O(1) 0.0238(7) 0.0298(8) 0.0448(9) 0.0021(6) 0.0111(7) -0.0113(7) O(2) 0.0303(8) 0.0462(9) 0.0234(7) -0.0020(7) 0.0046(6) -0.0103(7) O(3) 0.0366(8) 0.0248(7) 0.0196(6) -0.0042(6) 0.0085(6) 0.0026(6) O(4) 0.0274(7) 0.0435(10) 0.0216(7) -0.0118(6) 0.0072(5) -0.0087(6) O(5) 0.0355(8) 0.0314(8) 0.0163(6) 0.0082(6) 0.0102(5) 0.0007(6) N(1) 0.0200(7) 0.0213(7) 0.0175(7) 0.0022(6) 0.0054(6) -0.0026(6) N(2) 0.0290(9) 0.0224(9) 0.0265(8) -0.0015(7) 0.0065(7) -0.0029(7) C(1) 0.0243(8) 0.0192(9) 0.0246(8) 0.0000(7) 0.0095(7) -0.0042(8) C(2) 0.0213(9) 0.028(1) 0.0205(8) 0.0087(8) 0.0022(7) -0.0014(8) C(3) 0.0216(9) 0.0239(9) 0.038(1) 0.0010(7) 0.0122(8) 0.0063(9) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 89.18620 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1405 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0388 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0498 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.709 _refine_ls_shift/esd_max 0.3440 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.31 _refine_diff_density_max 0.33 #------------------------------------------------------------------------------ _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 P(1) O(3) 1.499(2) ? ? yes P(1) O(4) 1.569(2) ? ? yes P(1) O(5) 1.497(2) ? ? yes P(1) C(3) 1.808(3) ? ? yes O(1) C(1) 1.252(3) ? ? yes O(2) C(1) 1.244(3) ? ? yes N(1) C(2) 1.492(3) ? ? yes N(1) C(3) 1.482(3) ? ? yes C(1) C(2) 1.527(4) ? ? 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(3) P(1) O(4) 111.8(1) ? ? ? yes O(3) P(1) O(5) 115.9(1) ? ? ? yes O(3) P(1) C(3) 105.2(1) ? ? ? yes O(4) P(1) O(5) 107.6(1) ? ? ? yes O(4) P(1) C(3) 105.3(1) ? ? ? yes O(5) P(1) C(3) 110.6(1) ? ? ? yes C(2) N(1) C(3) 111.5(2) ? ? ? yes O(1) C(1) O(2) 127.5(2) ? ? ? yes O(1) C(1) C(2) 115.7(2) ? ? ? yes O(2) C(1) C(2) 116.8(2) ? ? ? yes N(1) C(2) C(1) 112.1(2) ? ? ? yes P(1) C(3) N(1) 117.1(2) ? ? ? yes #===END #------------------------------------------------------------------------------ data_COMPOUND(3) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H16 N2 Na2 O11 P2' _chemical_formula_weight 400.13 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.1850(10) _cell_length_b 9.288(2) _cell_length_c 10.7940(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.428(7) _cell_angle_gamma 90.00 _cell_volume 1519.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.402 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2817 _diffrn_reflns_av_R_equivalents 0.0104 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 24.96 _reflns_number_total 2660 _reflns_number_gt 2376 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+1.0275P] 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 SHELXL _refine_ls_extinction_coef 0.0066(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2660 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0698 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.36377(5) 0.06422(8) 0.66637(7) 0.02138(18) Uani 1 1 d . . . Na2 Na 0.15004(5) 0.06775(8) 0.66746(6) 0.02143(18) Uani 1 1 d . . . P1 P 0.47442(3) 0.21405(5) 0.40576(4) 0.01400(13) Uani 1 1 d . . . N1 N 0.42065(10) 0.07086(18) 0.18687(13) 0.0159(3) Uani 1 1 d . . . O1 O 0.26740(8) 0.23858(14) 0.16453(12) 0.0233(3) Uani 1 1 d . . . O2 O 0.20491(9) 0.09355(17) 0.02041(14) 0.0351(4) Uani 1 1 d . . . O3 O 0.45920(8) 0.35659(14) 0.34224(12) 0.0212(3) Uani 1 1 d . . . O4 O 0.45193(9) 0.20247(14) 0.53835(11) 0.0229(3) Uani 1 1 d . . . O5 O 0.57163(9) 0.16077(15) 0.38972(13) 0.0226(3) Uani 1 1 d . . . C1 C 0.26619(12) 0.1298(2) 0.09861(16) 0.0191(4) Uani 1 1 d . . . C2 C 0.34175(12) 0.0211(2) 0.10975(19) 0.0218(4) Uani 1 1 d . . . C3 C 0.40756(12) 0.0795(2) 0.32294(16) 0.0172(4) Uani 1 1 d . . . P1' P 0.96410(3) -0.19119(5) 0.63212(4) 0.01570(13) Uani 1 1 d . . . N1' N 0.90949(10) 0.08939(17) 0.63000(15) 0.0181(3) Uani 1 1 d . . . O1' O 0.68787(8) 0.22517(15) 0.56233(13) 0.0277(3) Uani 1 1 d . . . O2' O 0.75932(8) 0.04079(15) 0.48266(12) 0.0249(3) Uani 1 1 d . . . O3' O 1.05294(8) -0.12489(14) 0.61823(12) 0.0211(3) Uani 1 1 d . . . O4' O 0.95613(8) -0.31881(14) 0.71505(12) 0.0222(3) Uani 1 1 d . . . O5' O 0.92254(9) -0.22327(15) 0.49741(11) 0.0227(3) Uani 1 1 d . . . O6 O 0.26417(10) -0.02372(17) 0.80657(13) 0.0255(3) Uani 1 1 d . . . C1' C 0.75505(11) 0.1462(2) 0.55144(16) 0.0181(4) Uani 1 1 d . . . C2' C 0.83549(12) 0.1923(2) 0.63387(19) 0.0234(4) Uani 1 1 d . . . C3' C 0.89329(12) -0.0519(2) 0.68985(18) 0.0210(4) Uani 1 1 d . . . H2A H 0.3244(15) -0.069(3) 0.142(2) 0.032(6) Uiso 1 1 d . . . H2B H 0.3586(15) 0.002(3) 0.033(2) 0.030(6) Uiso 1 1 d . . . H3A H 0.4183(13) -0.016(2) 0.3560(19) 0.023(5) Uiso 1 1 d . . . H3B H 0.3486(15) 0.108(2) 0.333(2) 0.028(6) Uiso 1 1 d . . . H2'A H 0.8550(15) 0.287(3) 0.602(2) 0.036(6) Uiso 1 1 d . . . H2'B H 0.8228(15) 0.200(2) 0.718(2) 0.033(6) Uiso 1 1 d . . . H3'A H 0.8337(15) -0.080(2) 0.6738(19) 0.025(5) Uiso 1 1 d . . . H3'B H 0.9050(14) -0.036(2) 0.780(2) 0.029(6) Uiso 1 1 d . . . H4 H 0.4637(16) 0.005(3) 0.176(2) 0.031(6) Uiso 1 1 d . . . H5 H 0.4356(14) 0.153(3) 0.152(2) 0.026(6) Uiso 1 1 d . . . H6 H 0.6068(19) 0.185(3) 0.442(3) 0.057(9) Uiso 1 1 d . . . H7 H 0.2843(17) -0.104(3) 0.833(3) 0.046(8) Uiso 1 1 d . . . H8 H 0.251(2) 0.021(4) 0.868(3) 0.069(11) Uiso 1 1 d . . . H4' H 0.9211(14) 0.079(2) 0.553(2) 0.022(5) Uiso 1 1 d . . . H5' H 0.9580(15) 0.127(2) 0.672(2) 0.027(6) Uiso 1 1 d . . . H6' H 0.880(2) -0.286(3) 0.495(3) 0.068(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0192(4) 0.0209(4) 0.0243(4) 0.0000(3) 0.0030(3) 0.0004(3) Na2 0.0177(4) 0.0244(4) 0.0220(4) -0.0021(3) 0.0001(3) 0.0007(3) P1 0.0139(2) 0.0152(2) 0.0129(2) -0.00083(17) 0.00045(16) -0.00032(16) N1 0.0143(7) 0.0174(8) 0.0156(7) -0.0016(6) -0.0013(6) 0.0019(6) O1 0.0203(6) 0.0195(7) 0.0298(7) -0.0031(6) 0.0000(5) 0.0023(5) O2 0.0257(8) 0.0445(9) 0.0331(8) -0.0149(7) -0.0144(6) 0.0134(7) O3 0.0201(6) 0.0182(7) 0.0250(7) 0.0040(5) -0.0020(5) -0.0021(5) O4 0.0287(7) 0.0247(7) 0.0156(6) -0.0026(5) 0.0047(5) -0.0029(6) O5 0.0141(6) 0.0290(7) 0.0242(7) -0.0069(6) -0.0027(5) 0.0031(5) C1 0.0177(9) 0.0223(10) 0.0174(9) 0.0008(7) 0.0013(7) 0.0024(7) C2 0.0200(9) 0.0225(10) 0.0220(10) -0.0063(8) -0.0069(8) 0.0030(8) C3 0.0179(9) 0.0195(10) 0.0141(8) 0.0007(7) -0.0002(7) -0.0030(7) P1' 0.0138(2) 0.0185(2) 0.0146(2) 0.00252(17) -0.00067(17) -0.00073(17) N1' 0.0141(8) 0.0204(8) 0.0195(8) -0.0034(6) -0.0020(6) 0.0012(6) O1' 0.0172(7) 0.0261(7) 0.0388(8) -0.0100(6) -0.0068(6) 0.0056(6) O2' 0.0196(7) 0.0288(8) 0.0258(7) -0.0100(6) -0.0016(5) 0.0010(6) O3' 0.0159(6) 0.0247(7) 0.0227(7) -0.0007(5) 0.0006(5) -0.0034(5) O4' 0.0201(7) 0.0252(7) 0.0209(7) 0.0079(5) -0.0013(5) -0.0005(5) O5' 0.0250(7) 0.0261(7) 0.0163(6) 0.0020(5) -0.0033(5) -0.0070(6) O6 0.0296(8) 0.0252(8) 0.0213(7) 0.0046(6) -0.0012(6) -0.0017(6) C1' 0.0152(9) 0.0208(9) 0.0181(9) 0.0013(8) -0.0012(7) -0.0014(7) C2' 0.0177(9) 0.0249(11) 0.0270(11) -0.0067(8) -0.0039(8) 0.0037(8) C3' 0.0173(9) 0.0255(10) 0.0204(9) 0.0022(8) 0.0036(7) 0.0009(8) _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 Na1 O1 2.3438(15) 4_566 ? Na1 O6 2.3491(16) . ? Na1 O4 2.3605(15) . ? Na1 O5 2.4014(16) 3_656 ? Na1 O3 2.4323(15) 4_566 ? Na1 O2' 2.5831(14) 3_656 ? Na1 Na2 3.2463(10) . ? Na2 O4' 2.3583(14) 2_656 ? Na2 O3' 2.3587(15) 1_455 ? Na2 O6 2.3809(16) . ? Na2 O2' 2.4090(15) 3_656 ? Na2 O5' 2.4967(15) 3_656 ? Na2 O1 2.5336(15) 4_566 ? Na2 H8 2.61(3) . ? P1 O4 1.4950(13) . ? P1 O3 1.5024(13) . ? P1 O5 1.5762(13) . ? P1 C3 1.8119(18) . ? N1 C2 1.491(2) . ? N1 C3 1.496(2) . ? N1 H4 0.91(3) . ? N1 H5 0.89(2) . ? O1 C1 1.235(2) . ? O1 Na1 2.3438(15) 4_565 ? O1 Na2 2.5336(15) 4_565 ? O2 C1 1.264(2) . ? O3 Na1 2.4322(14) 4_565 ? O5 Na1 2.4014(16) 3_656 ? O5 H6 0.79(3) . ? C1 C2 1.528(3) . ? C2 H2A 0.95(2) . ? C2 H2B 0.90(2) . ? C3 H3A 0.97(2) . ? C3 H3B 0.95(2) . ? P1' O4' 1.4947(13) . ? P1' O3' 1.4986(13) . ? P1' O5' 1.5785(13) . ? P1' C3' 1.8163(19) . ? N1' C2' 1.478(2) . ? N1' C3' 1.489(2) . ? N1' H4' 0.87(2) . ? N1' H5' 0.91(2) . ? O1' C1' 1.268(2) . ? O2' C1' 1.233(2) . ? O2' Na2 2.4090(15) 3_656 ? O2' Na1 2.5832(14) 3_656 ? O3' Na2 2.3588(15) 1_655 ? O4' Na2 2.3583(14) 2_646 ? O5' Na2 2.4967(15) 3_656 ? O5' H6' 0.87(3) . ? O6 H7 0.85(3) . ? O6 H8 0.82(4) . ? C1' C2' 1.529(2) . ? C2' H2'A 0.99(3) . ? C2' H2'B 0.94(2) . ? C3' H3'A 0.95(2) . ? C3' H3'B 0.99(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Na1 O6 81.46(6) 4_566 . ? O1 Na1 O4 86.88(5) 4_566 . ? O6 Na1 O4 167.37(6) . . ? O1 Na1 O5 160.42(6) 4_566 3_656 ? O6 Na1 O5 98.53(6) . 3_656 ? O4 Na1 O5 94.09(5) . 3_656 ? O1 Na1 O3 96.48(5) 4_566 4_566 ? O6 Na1 O3 88.79(5) . 4_566 ? O4 Na1 O3 87.71(5) . 4_566 ? O5 Na1 O3 103.10(5) 3_656 4_566 ? O1 Na1 O2' 82.05(5) 4_566 3_656 ? O6 Na1 O2' 78.47(5) . 3_656 ? O4 Na1 O2' 104.80(5) . 3_656 ? O5 Na1 O2' 78.80(5) 3_656 3_656 ? O3 Na1 O2' 167.26(5) 4_566 3_656 ? O1 Na1 Na2 50.82(4) 4_566 . ? O6 Na1 Na2 47.07(4) . . ? O4 Na1 Na2 126.78(4) . . ? O5 Na1 Na2 115.67(4) 3_656 . ? O3 Na1 Na2 122.91(4) 4_566 . ? O2' Na1 Na2 47.14(3) 3_656 . ? O4' Na2 O3' 91.25(5) 2_656 1_455 ? O4' Na2 O6 108.39(6) 2_656 . ? O3' Na2 O6 107.04(6) 1_455 . ? O4' Na2 O2' 170.10(5) 2_656 3_656 ? O3' Na2 O2' 84.58(5) 1_455 3_656 ? O6 Na2 O2' 81.45(5) . 3_656 ? O4' Na2 O5' 80.68(5) 2_656 3_656 ? O3' Na2 O5' 92.00(5) 1_455 3_656 ? O6 Na2 O5' 158.37(6) . 3_656 ? O2' Na2 O5' 90.47(5) 3_656 3_656 ? O4' Na2 O1 101.16(5) 2_656 4_566 ? O3' Na2 O1 165.10(5) 1_455 4_566 ? O6 Na2 O1 77.01(5) . 4_566 ? O2' Na2 O1 81.84(5) 3_656 4_566 ? O5' Na2 O1 82.02(5) 3_656 4_566 ? O4' Na2 Na1 136.24(4) 2_656 . ? O3' Na2 Na1 127.09(4) 1_455 . ? O6 Na2 Na1 46.25(4) . . ? O2' Na2 Na1 51.81(3) 3_656 . ? O5' Na2 Na1 113.71(4) 3_656 . ? O1 Na2 Na1 45.82(3) 4_566 . ? O4' Na2 H8 90.8(8) 2_656 . ? O3' Na2 H8 113.0(7) 1_455 . ? O6 Na2 H8 18.1(8) . . ? O2' Na2 H8 99.1(8) 3_656 . ? O5' Na2 H8 153.9(8) 3_656 . ? O1 Na2 H8 75.4(7) 4_566 . ? Na1 Na2 H8 57.6(7) . . ? O4 P1 O3 117.55(8) . . ? O4 P1 O5 110.58(8) . . ? O3 P1 O5 110.24(8) . . ? O4 P1 C3 105.63(8) . . ? O3 P1 C3 108.44(8) . . ? O5 P1 C3 103.30(8) . . ? C2 N1 C3 114.54(15) . . ? C2 N1 H4 106.1(14) . . ? C3 N1 H4 107.7(14) . . ? C2 N1 H5 104.3(14) . . ? C3 N1 H5 115.0(14) . . ? H4 N1 H5 109(2) . . ? C1 O1 Na1 129.18(12) . 4_565 ? C1 O1 Na2 126.98(12) . 4_565 ? Na1 O1 Na2 83.36(5) 4_565 4_565 ? P1 O3 Na1 133.70(7) . 4_565 ? P1 O4 Na1 140.32(8) . . ? P1 O5 Na1 134.45(8) . 3_656 ? P1 O5 H6 115(2) . . ? Na1 O5 H6 99(2) 3_656 . ? O1 C1 O2 126.00(17) . . ? O1 C1 C2 120.66(16) . . ? O2 C1 C2 113.31(16) . . ? N1 C2 C1 114.46(16) . . ? N1 C2 H2A 107.6(14) . . ? C1 C2 H2A 112.8(14) . . ? N1 C2 H2B 108.3(14) . . ? C1 C2 H2B 108.1(15) . . ? H2A C2 H2B 105(2) . . ? N1 C3 P1 114.70(12) . . ? N1 C3 H3A 106.5(12) . . ? P1 C3 H3A 112.0(12) . . ? N1 C3 H3B 108.2(13) . . ? P1 C3 H3B 104.8(13) . . ? H3A C3 H3B 110.7(18) . . ? O4' P1' O3' 119.44(7) . . ? O4' P1' O5' 111.09(8) . . ? O3' P1' O5' 107.35(7) . . ? O4' P1' C3' 106.78(8) . . ? O3' P1' C3' 107.24(8) . . ? O5' P1' C3' 103.78(8) . . ? C2' N1' C3' 114.32(15) . . ? C2' N1' H4' 107.5(14) . . ? C3' N1' H4' 111.4(14) . . ? C2' N1' H5' 109.3(14) . . ? C3' N1' H5' 106.1(14) . . ? H4' N1' H5' 108.2(19) . . ? C1' O2' Na2 142.20(12) . 3_656 ? C1' O2' Na1 127.79(12) . 3_656 ? Na2 O2' Na1 81.05(4) 3_656 3_656 ? P1' O3' Na2 147.51(8) . 1_655 ? P1' O4' Na2 139.36(8) . 2_646 ? P1' O5' Na2 133.04(8) . 3_656 ? P1' O5' H6' 114(2) . . ? Na2 O5' H6' 94(2) 3_656 . ? Na1 O6 Na2 86.68(5) . . ? Na1 O6 H7 106.7(18) . . ? Na2 O6 H7 139.3(18) . . ? Na1 O6 H8 123(2) . . ? Na2 O6 H8 97(2) . . ? H7 O6 H8 106(3) . . ? O2' C1' O1' 125.94(16) . . ? O2' C1' C2' 120.26(16) . . ? O1' C1' C2' 113.81(16) . . ? N1' C2' C1' 112.65(16) . . ? N1' C2' H2'A 108.6(14) . . ? C1' C2' H2'A 107.0(14) . . ? N1' C2' H2'B 106.2(14) . . ? C1' C2' H2'B 112.3(14) . . ? H2'A C2' H2'B 110.1(19) . . ? N1' C3' P1' 111.24(12) . . ? N1' C3' H3'A 110.3(13) . . ? P1' C3' H3'A 108.4(13) . . ? N1' C3' H3'B 105.8(13) . . ? P1' C3' H3'B 111.5(13) . . ? H3'A C3' H3'B 109.5(18) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Na1 Na2 O4' -51.35(7) 4_566 . . 2_656 ? O6 Na1 Na2 O4' 68.41(8) . . . 2_656 ? O4 Na1 Na2 O4' -97.18(8) . . . 2_656 ? O5 Na1 Na2 O4' 145.56(7) 3_656 . . 2_656 ? O3 Na1 Na2 O4' 17.93(9) 4_566 . . 2_656 ? O2' Na1 Na2 O4' -172.19(8) 3_656 . . 2_656 ? O1 Na1 Na2 O3' 162.66(7) 4_566 . . 1_455 ? O6 Na1 Na2 O3' -77.58(8) . . . 1_455 ? O4 Na1 Na2 O3' 116.83(7) . . . 1_455 ? O5 Na1 Na2 O3' -0.43(7) 3_656 . . 1_455 ? O3 Na1 Na2 O3' -128.06(6) 4_566 . . 1_455 ? O2' Na1 Na2 O3' 41.83(7) 3_656 . . 1_455 ? O1 Na1 Na2 O6 -119.76(7) 4_566 . . . ? O4 Na1 Na2 O6 -165.59(8) . . . . ? O5 Na1 Na2 O6 77.15(7) 3_656 . . . ? O3 Na1 Na2 O6 -50.48(7) 4_566 . . . ? O2' Na1 Na2 O6 119.40(8) 3_656 . . . ? O1 Na1 Na2 O2' 120.84(7) 4_566 . . 3_656 ? O6 Na1 Na2 O2' -119.40(8) . . . 3_656 ? O4 Na1 Na2 O2' 75.01(7) . . . 3_656 ? O5 Na1 Na2 O2' -42.25(6) 3_656 . . 3_656 ? O3 Na1 Na2 O2' -169.89(7) 4_566 . . 3_656 ? O1 Na1 Na2 O5' 50.34(6) 4_566 . . 3_656 ? O6 Na1 Na2 O5' 170.10(7) . . . 3_656 ? O4 Na1 Na2 O5' 4.51(7) . . . 3_656 ? O5 Na1 Na2 O5' -112.75(6) 3_656 . . 3_656 ? O3 Na1 Na2 O5' 119.62(6) 4_566 . . 3_656 ? O2' Na1 Na2 O5' -70.50(6) 3_656 . . 3_656 ? O6 Na1 Na2 O1 119.76(7) . . . 4_566 ? O4 Na1 Na2 O1 -45.83(7) . . . 4_566 ? O5 Na1 Na2 O1 -163.09(7) 3_656 . . 4_566 ? O3 Na1 Na2 O1 69.28(6) 4_566 . . 4_566 ? O2' Na1 Na2 O1 -120.84(7) 3_656 . . 4_566 ? O4 P1 O3 Na1 -116.88(10) . . . 4_565 ? O5 P1 O3 Na1 115.16(10) . . . 4_565 ? C3 P1 O3 Na1 2.74(13) . . . 4_565 ? O3 P1 O4 Na1 123.61(12) . . . . ? O5 P1 O4 Na1 -108.59(13) . . . . ? C3 P1 O4 Na1 2.52(15) . . . . ? O1 Na1 O4 P1 -104.14(13) 4_566 . . . ? O6 Na1 O4 P1 -126.7(2) . . . . ? O5 Na1 O4 P1 56.26(13) 3_656 . . . ? O3 Na1 O4 P1 159.24(13) 4_566 . . . ? O2' Na1 O4 P1 -23.21(14) 3_656 . . . ? Na2 Na1 O4 P1 -70.30(14) . . . . ? O4 P1 O5 Na1 94.52(12) . . . 3_656 ? O3 P1 O5 Na1 -133.78(10) . . . 3_656 ? C3 P1 O5 Na1 -18.09(13) . . . 3_656 ? Na1 O1 C1 O2 -116.22(19) 4_565 . . . ? Na2 O1 C1 O2 -0.9(3) 4_565 . . . ? Na1 O1 C1 C2 65.9(2) 4_565 . . . ? Na2 O1 C1 C2 -178.79(13) 4_565 . . . ? C3 N1 C2 C1 70.7(2) . . . . ? O1 C1 C2 N1 -10.5(3) . . . . ? O2 C1 C2 N1 171.39(17) . . . . ? C2 N1 C3 P1 -151.09(13) . . . . ? O4 P1 C3 N1 -179.20(13) . . . . ? O3 P1 C3 N1 53.95(15) . . . . ? O5 P1 C3 N1 -63.02(15) . . . . ? O4' P1' O3' Na2 -105.38(15) . . . 1_655 ? O5' P1' O3' Na2 127.10(14) . . . 1_655 ? C3' P1' O3' Na2 16.11(17) . . . 1_655 ? O3' P1' O4' Na2 154.71(10) . . . 2_646 ? O5' P1' O4' Na2 -79.52(13) . . . 2_646 ? C3' P1' O4' Na2 32.99(14) . . . 2_646 ? O4' P1' O5' Na2 150.25(9) . . . 3_656 ? O3' P1' O5' Na2 -77.51(11) . . . 3_656 ? C3' P1' O5' Na2 35.84(12) . . . 3_656 ? O1 Na1 O6 Na2 42.88(5) 4_566 . . . ? O4 Na1 O6 Na2 65.7(3) . . . . ? O5 Na1 O6 Na2 -117.31(6) 3_656 . . . ? O3 Na1 O6 Na2 139.62(5) 4_566 . . . ? O2' Na1 O6 Na2 -40.68(5) 3_656 . . . ? O4' Na2 O6 Na1 -137.33(5) 2_656 . . . ? O3' Na2 O6 Na1 125.43(5) 1_455 . . . ? O2' Na2 O6 Na1 43.83(5) 3_656 . . . ? O5' Na2 O6 Na1 -25.28(18) 3_656 . . . ? O1 Na2 O6 Na1 -39.71(5) 4_566 . . . ? Na2 O2' C1' O1' 132.64(18) 3_656 . . . ? Na1 O2' C1' O1' -0.1(3) 3_656 . . . ? Na2 O2' C1' C2' -47.4(3) 3_656 . . . ? Na1 O2' C1' C2' 179.88(13) 3_656 . . . ? C3' N1' C2' C1' -69.1(2) . . . . ? O2' C1' C2' N1' -6.4(3) . . . . ? O1' C1' C2' N1' 173.54(16) . . . . ? C2' N1' C3' P1' 158.10(13) . . . . ? O4' P1' C3' N1' 168.74(12) . . . . ? O3' P1' C3' N1' 39.61(15) . . . . ? O5' P1' C3' N1' -73.82(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.390 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.050 #===END #------------------------------------------------------------------------------ data_compound(4) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H9 N Na O6 P' _chemical_formula_weight 209.07 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.1210(4) _cell_length_b 11.2074(7) _cell_length_c 9.6687(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.602(6) _cell_angle_gamma 90.00 _cell_volume 762.96(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 0.409 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1453 _diffrn_reflns_av_R_equivalents 0.0135 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 24.96 _reflns_number_total 1340 _reflns_number_gt 1311 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.5224P] 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 SHELXL _refine_ls_extinction_coef 0.047(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1340 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na Na 0.13574(8) 0.87675(5) -0.00804(6) 0.02097(19) Uani 1 1 d . . . N1 N 0.42964(18) 0.49419(12) 0.25352(13) 0.0175(3) Uani 1 1 d . . . P1 P 0.33882(5) 0.34018(3) 0.45705(4) 0.01419(15) Uani 1 1 d . . . O1 O 0.09152(16) 0.60481(11) 0.24420(11) 0.0264(3) Uani 1 1 d . . . O2 O 0.07625(16) 0.66144(10) 0.02144(12) 0.0238(3) Uani 1 1 d . . . O3 O 0.27675(16) 0.20502(10) 0.44650(12) 0.0209(3) Uani 1 1 d . . . O4 O 0.54057(14) 0.34634(10) 0.52838(11) 0.0210(3) Uani 1 1 d . . . O5 O 0.19541(15) 0.41520(9) 0.51450(11) 0.0207(3) Uani 1 1 d . . . O6 O 0.80664(17) 0.41999(13) 0.24235(14) 0.0293(3) Uani 1 1 d . . . C1 C 0.1565(2) 0.61147(13) 0.13255(15) 0.0177(3) Uani 1 1 d . . . C2 C 0.3484(2) 0.55632(15) 0.12219(16) 0.0190(3) Uani 1 1 d . . . C3 C 0.3377(2) 0.37657(14) 0.27362(15) 0.0189(3) Uani 1 1 d . . . H2A H 0.335(3) 0.4998(18) 0.050(2) 0.026(5) Uiso 1 1 d . . . H2B H 0.431(3) 0.6143(18) 0.1044(19) 0.025(5) Uiso 1 1 d . . . H3A H 0.214(3) 0.3795(17) 0.231(2) 0.025(5) Uiso 1 1 d . . . H3B H 0.403(3) 0.3131(19) 0.231(2) 0.027(5) Uiso 1 1 d . . . H4 H 0.557(3) 0.4801(17) 0.252(2) 0.026(5) Uiso 1 1 d . . . H5 H 0.421(3) 0.5443(19) 0.328(2) 0.028(5) Uiso 1 1 d . . . H6 H 0.166(4) 0.197(2) 0.446(2) 0.043(6) Uiso 1 1 d . . . H7 H 0.878(4) 0.483(3) 0.250(3) 0.062(8) Uiso 1 1 d . . . H8 H 0.833(4) 0.385(3) 0.182(3) 0.055(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na 0.0184(3) 0.0205(3) 0.0246(3) 0.0019(2) 0.0047(2) -0.0008(2) N1 0.0143(6) 0.0202(7) 0.0180(6) 0.0011(5) 0.0023(5) 0.0014(5) P1 0.0136(2) 0.0144(2) 0.0146(2) 0.00001(13) 0.00217(15) -0.00020(13) O1 0.0224(6) 0.0391(7) 0.0188(6) 0.0029(5) 0.0064(4) 0.0067(5) O2 0.0237(6) 0.0262(6) 0.0212(6) 0.0063(4) 0.0028(4) 0.0063(5) O3 0.0172(6) 0.0161(6) 0.0296(6) -0.0001(4) 0.0040(4) -0.0009(4) O4 0.0156(6) 0.0253(6) 0.0214(6) -0.0004(4) 0.0000(4) -0.0019(4) O5 0.0203(5) 0.0191(6) 0.0242(6) -0.0018(4) 0.0077(4) 0.0009(4) O6 0.0246(6) 0.0364(7) 0.0279(7) -0.0083(6) 0.0079(5) -0.0008(6) C1 0.0176(7) 0.0149(7) 0.0203(8) -0.0002(6) 0.0020(6) -0.0011(6) C2 0.0188(7) 0.0207(8) 0.0182(8) 0.0048(6) 0.0055(6) 0.0008(6) C3 0.0212(8) 0.0188(8) 0.0164(7) 0.0000(6) 0.0021(6) 0.0004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na O4 2.3671(12) 2_655 ? Na O5 2.3742(12) 4_575 ? Na O1 2.3780(13) 4_575 ? Na O5 2.3888(12) 2 ? Na O2 2.4739(13) . ? Na O6 2.5860(15) 2_655 ? Na Na 3.3886(12) 3_575 ? N1 C2 1.4874(19) . ? N1 C3 1.497(2) . ? N1 H4 0.92(2) . ? N1 H5 0.92(2) . ? P1 O5 1.4926(11) . ? P1 O4 1.4993(11) . ? P1 O3 1.5771(11) . ? P1 C3 1.8186(15) . ? O1 C1 1.2385(19) . ? O1 Na 2.3780(13) 4_576 ? O2 C1 1.2691(19) . ? O3 H6 0.79(2) . ? O4 Na 2.3672(12) 2_645 ? O5 Na 2.3742(12) 4_576 ? O5 Na 2.3888(12) 2_545 ? O6 Na 2.5860(15) 2_645 ? O6 H7 0.87(3) . ? O6 H8 0.75(3) . ? C1 C2 1.517(2) . ? C2 H2A 0.94(2) . ? C2 H2B 0.91(2) . ? C3 H3A 0.92(2) . ? C3 H3B 0.98(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Na O5 89.19(4) 2_655 4_575 ? O4 Na O1 84.99(4) 2_655 4_575 ? O5 Na O1 90.12(4) 4_575 4_575 ? O4 Na O5 173.46(5) 2_655 2 ? O5 Na O5 89.29(4) 4_575 2 ? O1 Na O5 88.66(4) 4_575 2 ? O4 Na O2 93.14(4) 2_655 . ? O5 Na O2 168.17(5) 4_575 . ? O1 Na O2 101.63(5) 4_575 . ? O5 Na O2 89.63(4) 2 . ? O4 Na O6 95.61(4) 2_655 2_655 ? O5 Na O6 74.05(5) 4_575 2_655 ? O1 Na O6 164.13(5) 4_575 2_655 ? O5 Na O6 90.09(4) 2 2_655 ? O2 Na O6 94.17(5) . 2_655 ? O4 Na Na 133.67(4) 2_655 3_575 ? O5 Na Na 44.82(3) 4_575 3_575 ? O1 Na Na 89.14(4) 4_575 3_575 ? O5 Na Na 44.47(3) 2 3_575 ? O2 Na Na 132.94(4) . 3_575 ? O6 Na Na 78.96(4) 2_655 3_575 ? C2 N1 C3 113.65(12) . . ? C2 N1 H4 108.7(12) . . ? C3 N1 H4 107.6(12) . . ? C2 N1 H5 108.4(12) . . ? C3 N1 H5 110.7(12) . . ? H4 N1 H5 107.6(17) . . ? O5 P1 O4 117.69(6) . . ? O5 P1 O3 111.37(6) . . ? O4 P1 O3 108.30(6) . . ? O5 P1 C3 109.46(7) . . ? O4 P1 C3 107.61(7) . . ? O3 P1 C3 101.07(7) . . ? C1 O1 Na 149.58(10) . 4_576 ? C1 O2 Na 117.70(10) . . ? P1 O3 H6 112.1(18) . . ? P1 O4 Na 147.82(7) . 2_645 ? P1 O5 Na 129.94(6) . 4_576 ? P1 O5 Na 128.05(6) . 2_545 ? Na O5 Na 90.71(4) 4_576 2_545 ? Na O6 H7 93.7(19) 2_645 . ? Na O6 H8 131(2) 2_645 . ? H7 O6 H8 106(3) . . ? O1 C1 O2 125.79(14) . . ? O1 C1 C2 119.39(13) . . ? O2 C1 C2 114.82(13) . . ? N1 C2 C1 111.93(12) . . ? N1 C2 H2A 107.6(12) . . ? C1 C2 H2A 109.5(12) . . ? N1 C2 H2B 108.4(12) . . ? C1 C2 H2B 109.7(12) . . ? H2A C2 H2B 109.7(16) . . ? N1 C3 P1 112.69(10) . . ? N1 C3 H3A 108.7(12) . . ? P1 C3 H3A 107.9(12) . . ? N1 C3 H3B 109.9(11) . . ? P1 C3 H3B 108.3(11) . . ? H3A C3 H3B 109.2(16) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Na O2 C1 67.43(11) 2_655 . . . ? O5 Na O2 C1 -33.7(3) 4_575 . . . ? O1 Na O2 C1 152.96(10) 4_575 . . . ? O5 Na O2 C1 -118.49(11) 2 . . . ? O6 Na O2 C1 -28.43(11) 2_655 . . . ? Na Na O2 C1 -107.22(11) 3_575 . . . ? O5 P1 O4 Na -127.24(12) . . . 2_645 ? O3 P1 O4 Na 105.39(13) . . . 2_645 ? C3 P1 O4 Na -3.10(15) . . . 2_645 ? O4 P1 O5 Na 76.78(10) . . . 4_576 ? O3 P1 O5 Na -157.34(7) . . . 4_576 ? C3 P1 O5 Na -46.44(10) . . . 4_576 ? O4 P1 O5 Na -150.71(7) . . . 2_545 ? O3 P1 O5 Na -24.83(10) . . . 2_545 ? C3 P1 O5 Na 86.08(9) . . . 2_545 ? Na O1 C1 O2 -133.96(17) 4_576 . . . ? Na O1 C1 C2 46.1(3) 4_576 . . . ? Na O2 C1 O1 88.40(17) . . . . ? Na O2 C1 C2 -91.65(14) . . . . ? C3 N1 C2 C1 75.30(17) . . . . ? O1 C1 C2 N1 2.8(2) . . . . ? O2 C1 C2 N1 -177.13(13) . . . . ? C2 N1 C3 P1 -149.38(11) . . . . ? O5 P1 C3 N1 74.05(12) . . . . ? O4 P1 C3 N1 -54.95(12) . . . . ? O3 P1 C3 N1 -168.38(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.253 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.052 #------------------------------------------------------------------------------ #===END data_compound(6) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H24 N Na2 O14 P' _chemical_formula_weight 375.18 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.3650(10) _cell_length_b 7.186(2) _cell_length_c 17.816(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.040(10) _cell_angle_gamma 90.00 _cell_volume 812.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 0.287 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1712 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 24.96 _reflns_number_total 1564 _reflns_number_gt 1464 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(12) _refine_ls_number_reflns 1564 _refine_ls_number_parameters 270 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0640 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.658 _refine_ls_shift/su_mean 0.044 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.71477(16) 0.89594(16) 0.33015(6) 0.0295(3) Uani 1 1 d . . . Na2 Na 0.5098(2) 0.62823(16) -0.00070(8) 0.0327(3) Uani 1 1 d . . . P1 P 0.09179(9) 0.42201(9) 0.21719(3) 0.01826(16) Uani 1 1 d . . . O1 O 0.7353(3) 0.5993(3) 0.39564(12) 0.0369(5) Uani 1 1 d . . . O2 O 0.7602(3) 0.4090(4) 0.49499(10) 0.0403(5) Uani 1 1 d . . . O3 O 0.2061(3) 0.2594(3) 0.18452(12) 0.0299(5) Uani 1 1 d . . . O4 O 0.1840(3) 0.6074(3) 0.19370(11) 0.0285(5) Uani 1 1 d . . . O5 O -0.1444(2) 0.4118(3) 0.20306(9) 0.0282(4) Uani 1 1 d . . . O6 O 0.1811(4) 0.7075(4) 0.04705(14) 0.0324(5) Uani 1 1 d . . . O7 O 0.3310(4) 0.3904(4) -0.07987(13) 0.0434(6) Uani 1 1 d . . . O8 O 0.4552(3) 0.8790(3) -0.08844(11) 0.0291(5) Uani 1 1 d . . . O9 O 0.8557(4) 0.5865(3) -0.05018(14) 0.0367(5) Uani 1 1 d . . . O10 O 0.5974(4) 0.7244(3) 0.21663(12) 0.0311(5) Uani 1 1 d . . . O11 O 0.5923(4) 1.1815(3) 0.27070(13) 0.0328(5) Uani 1 1 d . . . O12 O 1.0311(4) 0.9325(4) 0.25373(13) 0.0379(5) Uani 1 1 d . . . O13 O 0.8819(5) 1.0553(4) 0.43317(16) 0.0498(7) Uani 1 1 d . . . O14 O 0.3569(4) 0.8559(4) 0.36249(14) 0.0360(5) Uani 1 1 d . . . N1 N 0.3664(4) 0.4612(4) 0.34300(13) 0.0238(5) Uani 1 1 d . . . C1 C 0.6645(4) 0.4830(4) 0.43857(15) 0.0261(6) Uani 1 1 d . . . C2 C 0.4395(4) 0.4128(5) 0.42107(14) 0.0311(6) Uani 1 1 d . . . H2A H 0.4352 0.2789 0.4276 0.037 Uiso 1 1 calc R . . H2B H 0.3469 0.4687 0.4557 0.037 Uiso 1 1 calc R . . C3 C 0.1433(3) 0.4094(5) 0.31949(13) 0.0230(5) Uani 1 1 d . . . H3A H 0.0484 0.4929 0.3433 0.028 Uiso 1 1 calc R . . H3B H 0.1159 0.2840 0.3364 0.028 Uiso 1 1 calc R . . H6A H 0.179(6) 0.663(7) 0.089(3) 0.051(13) Uiso 1 1 d . . . H6B H 0.165(7) 0.816(7) 0.047(2) 0.057(15) Uiso 1 1 d . . . H7A H 0.357(7) 0.371(9) -0.122(3) 0.068(14) Uiso 1 1 d . . . H7B H 0.206(11) 0.409(15) -0.095(4) 0.15(3) Uiso 1 1 d . . . H8A H 0.547(5) 0.859(5) -0.1192(19) 0.032(9) Uiso 1 1 d . . . H8B H 0.344(5) 0.878(5) -0.1205(18) 0.028(8) Uiso 1 1 d . . . H9A H 0.958(8) 0.631(9) -0.016(3) 0.078(15) Uiso 1 1 d . . . H9B H 0.858(7) 0.637(8) -0.101(3) 0.073(14) Uiso 1 1 d . . . H10A H 0.473(7) 0.702(6) 0.200(2) 0.059(13) Uiso 1 1 d . . . H10B H 0.685(8) 0.624(9) 0.211(3) 0.080(16) Uiso 1 1 d . . . H11A H 0.500(5) 1.173(5) 0.242(2) 0.027(10) Uiso 1 1 d . . . H11B H 0.698(8) 1.250(7) 0.247(3) 0.071(14) Uiso 1 1 d . . . H12A H 1.064(5) 0.848(6) 0.2369(19) 0.018(9) Uiso 1 1 d . . . H13A H 0.988(8) 0.998(7) 0.455(3) 0.074(15) Uiso 1 1 d . . . H13B H 0.860(6) 1.145(7) 0.452(2) 0.037(11) Uiso 1 1 d . . . H14A H 0.252(5) 0.882(5) 0.3372(18) 0.026(8) Uiso 1 1 d . . . H14B H 0.339(7) 0.870(9) 0.406(3) 0.077(16) Uiso 1 1 d . . . H1B H 0.460(5) 0.410(6) 0.3160(18) 0.034(8) Uiso 1 1 d . . . H1A H 0.383(5) 0.589(6) 0.3395(18) 0.033(9) Uiso 1 1 d . . . H12B H 1.113(15) 1.023(16) 0.223(5) 0.22(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0304(5) 0.0272(6) 0.0305(5) 0.0000(5) -0.0005(4) -0.0008(5) Na2 0.0393(6) 0.0274(6) 0.0317(5) 0.0041(5) 0.0048(4) 0.0029(6) P1 0.0175(3) 0.0194(3) 0.0176(3) -0.0003(3) -0.0011(2) -0.0006(3) O1 0.0308(10) 0.0389(13) 0.0405(12) 0.0106(10) -0.0014(9) -0.0016(10) O2 0.0364(10) 0.0533(14) 0.0294(9) 0.0070(12) -0.0116(8) -0.0020(13) O3 0.0330(11) 0.0292(12) 0.0267(11) -0.0077(9) -0.0033(9) 0.0082(9) O4 0.0324(11) 0.0249(11) 0.0280(10) 0.0031(9) 0.0011(9) -0.0083(9) O5 0.0207(8) 0.0340(11) 0.0294(9) 0.0040(10) -0.0022(6) -0.0024(10) O6 0.0424(13) 0.0288(13) 0.0259(13) 0.0024(10) 0.0018(10) -0.0020(11) O7 0.0457(12) 0.0505(15) 0.0335(11) -0.0111(12) -0.0003(9) 0.0049(13) O8 0.0323(10) 0.0322(12) 0.0224(9) 0.0017(9) -0.0019(8) 0.0012(9) O9 0.0483(14) 0.0309(13) 0.0302(12) 0.0038(10) -0.0035(10) -0.0065(10) O10 0.0301(11) 0.0302(11) 0.0329(12) -0.0033(10) 0.0006(9) -0.0027(10) O11 0.0269(11) 0.0342(13) 0.0372(13) 0.0075(10) 0.0018(10) 0.0009(10) O12 0.0435(12) 0.0275(13) 0.0434(12) -0.0041(13) 0.0084(9) 0.0057(12) O13 0.0518(15) 0.0424(15) 0.0516(15) -0.0107(14) -0.0220(12) 0.0127(13) O14 0.0343(11) 0.0424(13) 0.0311(12) -0.0006(11) 0.0011(10) 0.0062(10) N1 0.0216(11) 0.0288(15) 0.0207(11) 0.0022(10) -0.0011(9) -0.0003(10) C1 0.0291(14) 0.0272(14) 0.0215(13) -0.0035(11) -0.0011(11) 0.0033(11) C2 0.0313(13) 0.0399(16) 0.0215(12) 0.0090(15) -0.0023(10) -0.0022(16) C3 0.0206(11) 0.0271(13) 0.0210(11) 0.0020(13) 0.0007(9) 0.0003(13) _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 Na1 O13 2.353(3) . ? Na1 O14 2.406(2) . ? Na1 O11 2.413(2) . ? Na1 O1 2.429(3) . ? Na1 O10 2.440(2) . ? Na1 O12 2.523(3) . ? Na2 O6 2.383(3) . ? Na2 O8 2.395(2) . ? Na2 O8 2.394(2) 2_645 ? Na2 O9 2.447(3) . ? Na2 O7 2.445(3) . ? Na2 O7 2.536(3) 2_655 ? Na2 Na2 3.5953(10) 2_645 ? Na2 Na2 3.5953(10) 2_655 ? P1 O5 1.5087(17) . ? P1 O3 1.514(2) . ? P1 O4 1.526(2) . ? P1 C3 1.831(2) . ? O1 C1 1.239(4) . ? O2 C1 1.256(3) . ? O6 H6A 0.81(5) . ? O6 H6B 0.79(5) . ? O7 Na2 2.536(3) 2_645 ? O7 H7A 0.79(5) . ? O7 H7B 0.83(7) . ? O8 Na2 2.394(2) 2_655 ? O8 H8A 0.84(4) . ? O8 H8B 0.88(3) . ? O9 H9A 0.91(5) . ? O9 H9B 0.98(5) . ? O10 H10A 0.84(4) . ? O10 H10B 0.92(6) . ? O11 H11A 0.75(4) . ? O11 H11B 0.95(5) . ? O12 H12A 0.72(4) . ? O12 H12B 1.02(10) . ? O13 H13A 0.86(5) . ? O13 H13B 0.74(5) . ? O14 H14A 0.80(3) . ? O14 H14B 0.80(5) . ? N1 C2 1.477(3) . ? N1 C3 1.499(3) . ? N1 H1B 0.87(4) . ? N1 H1A 0.92(4) . ? C1 C2 1.530(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? 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 O13 Na1 O14 104.78(10) . . ? O13 Na1 O11 92.45(10) . . ? O14 Na1 O11 85.68(9) . . ? O13 Na1 O1 92.67(10) . . ? O14 Na1 O1 78.45(8) . . ? O11 Na1 O1 164.09(9) . . ? O13 Na1 O10 170.93(11) . . ? O14 Na1 O10 84.16(9) . . ? O11 Na1 O10 89.73(9) . . ? O1 Na1 O10 87.57(9) . . ? O13 Na1 O12 92.06(10) . . ? O14 Na1 O12 161.24(9) . . ? O11 Na1 O12 85.41(9) . . ? O1 Na1 O12 109.44(9) . . ? O10 Na1 O12 79.32(8) . . ? O6 Na2 O8 87.84(9) . . ? O6 Na2 O8 89.14(10) . 2_645 ? O8 Na2 O8 176.89(7) . 2_645 ? O6 Na2 O9 173.22(10) . . ? O8 Na2 O9 87.15(9) . . ? O8 Na2 O9 95.92(9) 2_645 . ? O6 Na2 O7 89.32(9) . . ? O8 Na2 O7 96.26(10) . . ? O8 Na2 O7 82.97(9) 2_645 . ? O9 Na2 O7 95.77(9) . . ? O6 Na2 O7 86.92(9) . 2_655 ? O8 Na2 O7 81.05(8) . 2_655 ? O8 Na2 O7 99.53(10) 2_645 2_655 ? O9 Na2 O7 87.78(10) . 2_655 ? O7 Na2 O7 175.45(9) . 2_655 ? O6 Na2 Na2 101.80(9) . 2_645 ? O8 Na2 Na2 138.85(9) . 2_645 ? O8 Na2 Na2 41.35(5) 2_645 2_645 ? O9 Na2 Na2 84.98(7) . 2_645 ? O7 Na2 Na2 44.81(7) . 2_645 ? O7 Na2 Na2 138.69(9) 2_655 2_645 ? O6 Na2 Na2 74.15(8) . 2_655 ? O8 Na2 Na2 41.33(6) . 2_655 ? O8 Na2 Na2 138.14(9) 2_645 2_655 ? O9 Na2 Na2 99.08(8) . 2_655 ? O7 Na2 Na2 133.43(9) . 2_655 ? O7 Na2 Na2 42.81(6) 2_655 2_655 ? Na2 Na2 Na2 175.88(9) 2_645 2_655 ? O5 P1 O3 113.48(12) . . ? O5 P1 O4 113.26(12) . . ? O3 P1 O4 111.33(11) . . ? O5 P1 C3 105.66(10) . . ? O3 P1 C3 106.70(13) . . ? O4 P1 C3 105.71(13) . . ? C1 O1 Na1 151.53(19) . . ? Na2 O6 H6A 108(3) . . ? Na2 O6 H6B 111(3) . . ? H6A O6 H6B 113(5) . . ? Na2 O7 Na2 92.38(8) . 2_645 ? Na2 O7 H7A 123(4) . . ? Na2 O7 H7A 108(4) 2_645 . ? Na2 O7 H7B 118(7) . . ? Na2 O7 H7B 129(7) 2_645 . ? H7A O7 H7B 90(5) . . ? Na2 O8 Na2 97.32(7) . 2_655 ? Na2 O8 H8A 103(2) . . ? Na2 O8 H8A 122(2) 2_655 . ? Na2 O8 H8B 120(2) . . ? Na2 O8 H8B 118(2) 2_655 . ? H8A O8 H8B 98(3) . . ? Na2 O9 H9A 109(3) . . ? Na2 O9 H9B 111(3) . . ? H9A O9 H9B 116(5) . . ? Na1 O10 H10A 128(3) . . ? Na1 O10 H10B 109(3) . . ? H10A O10 H10B 112(5) . . ? Na1 O11 H11A 116(3) . . ? Na1 O11 H11B 115(3) . . ? H11A O11 H11B 106(4) . . ? Na1 O12 H12A 114(3) . . ? Na1 O12 H12B 145(6) . . ? H12A O12 H12B 98(6) . . ? Na1 O13 H13A 115(3) . . ? Na1 O13 H13B 133(3) . . ? H13A O13 H13B 112(4) . . ? Na1 O14 H14A 127(2) . . ? Na1 O14 H14B 115(3) . . ? H14A O14 H14B 111(4) . . ? C2 N1 C3 115.7(2) . . ? C2 N1 H1B 104(2) . . ? C3 N1 H1B 114(2) . . ? C2 N1 H1A 105(2) . . ? C3 N1 H1A 110(2) . . ? H1B N1 H1A 107(3) . . ? O1 C1 O2 127.1(3) . . ? O1 C1 C2 118.2(2) . . ? O2 C1 C2 114.7(3) . . ? N1 C2 C1 110.0(2) . . ? N1 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N1 C3 P1 111.43(16) . . ? N1 C3 H3A 109.3 . . ? P1 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? P1 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O13 Na1 O1 C1 86.4(4) . . . . ? O14 Na1 O1 C1 -18.2(4) . . . . ? O11 Na1 O1 C1 -22.2(6) . . . . ? O10 Na1 O1 C1 -102.7(4) . . . . ? O12 Na1 O1 C1 179.5(4) . . . . ? O6 Na2 O7 Na2 -107.59(10) . . . 2_645 ? O8 Na2 O7 Na2 164.66(10) . . . 2_645 ? O8 Na2 O7 Na2 -18.37(7) 2_645 . . 2_645 ? O9 Na2 O7 Na2 76.91(9) . . . 2_645 ? O7 Na2 O7 Na2 -141.9(11) 2_655 . . 2_645 ? Na2 Na2 O7 Na2 -174.79(12) 2_655 . . 2_645 ? O6 Na2 O8 Na2 68.21(9) . . . 2_655 ? O8 Na2 O8 Na2 81.9(18) 2_645 . . 2_655 ? O9 Na2 O8 Na2 -107.21(10) . . . 2_655 ? O7 Na2 O8 Na2 157.29(10) . . . 2_655 ? O7 Na2 O8 Na2 -19.01(7) 2_655 . . 2_655 ? Na2 Na2 O8 Na2 173.75(13) 2_645 . . 2_655 ? Na1 O1 C1 O2 -127.7(4) . . . . ? Na1 O1 C1 C2 54.9(5) . . . . ? C3 N1 C2 C1 -176.9(2) . . . . ? O1 C1 C2 N1 15.5(4) . . . . ? O2 C1 C2 N1 -162.3(3) . . . . ? C2 N1 C3 P1 -165.8(2) . . . . ? O5 P1 C3 N1 -167.1(2) . . . . ? O3 P1 C3 N1 71.9(2) . . . . ? O4 P1 C3 N1 -46.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.195 _refine_diff_density_min -0.178 _refine_diff_density_rms 0.040 #===END #------------------------------------------------------------------------------ data_compound(7) #------------------------------------------------------------------------------ _audit_creation_date 'Mon Nov 15 16:42:39 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 5.400(2) _cell_length_b 17.168(3) _cell_length_c 5.010(2) _cell_angle_alpha 94.49(2) _cell_angle_beta 115.75(2) _cell_angle_gamma 81.95(2) _cell_volume 414.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 24.1 _cell_measurement_theta_max 29.1 #------------------------------------------------------------------------------ _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' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'pale-brownprismatic' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.080 _exptl_crystal_density_diffrn 3.061 _exptl_crystal_density_meas ? _chemical_formula_weight 382.79 _chemical_formula_analytical ? _chemical_formula_sum 'C3 H6 Ag2 N O5 P ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 360.00 _exptl_absorpt_coefficient_mu 4.888 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.914 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 295.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.12 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -3 1 -1 0 2 0 -5 1 _diffrn_reflns_number 2100 _reflns_number_total 1902 _reflns_number_observed 1297 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 2.04 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.10692 _diffrn_orient_matrix_UB_12 -0.02376 _diffrn_orient_matrix_UB_13 0.08668 _diffrn_orient_matrix_UB_21 0.09075 _diffrn_orient_matrix_UB_22 -0.05352 _diffrn_orient_matrix_UB_23 -0.02141 _diffrn_orient_matrix_UB_31 0.15230 _diffrn_orient_matrix_UB_32 0.00577 _diffrn_orient_matrix_UB_33 0.20288 #------------------------------------------------------------------------------ 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 6 0.003 0.002 'International Tables' H 0 10 0.000 0.000 'International Tables' Ag 0 4 -0.897 1.101 'International Tables' N 0 2 0.006 0.003 'International Tables' P 0 2 0.102 0.094 'International Tables' O 0 10 0.011 0.006 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ag(1) 0.1117(6) 0.0520(2) 0.3499(6) 0.0344(8) Uij ? ? Ag(2) 0.5000 0.0000 1.0000 0.097(3) Uij ? ? Ag(3) 0.915(3) -0.5515(4) 0.245(2) 0.115(4) Uij ? ? P(1) 0.296(2) -0.1332(5) 0.371(2) 0.024(2) Uij ? ? O(1) 0.80(1) -0.354(4) 0.42(1) 0.06(2) Uij ? ? O(1') 0.93(1) -0.331(3) 0.49(1) 0.03(1) Uij ? ? O(2) 0.69(1) -0.427(4) 0.09(1) 0.08(2) Uij ? ? O(2') 1.03(1) -0.409(4) 0.20(1) 0.07(2) Uij ? ? O(3) 0.255(5) -0.059(1) 0.179(5) 0.035(7) Uij ? ? O(4) -0.049(5) 0.146(1) 0.588(5) 0.038(8) Uij ? ? O(5) 0.446(4) 0.134(1) 0.340(4) 0.032(7) Uij ? ? N(3) 0.582(6) -0.224(1) 0.091(6) 0.028(8) Uij ? ? C(1) 0.71(2) -0.364(4) 0.18(2) 0.03(2) Uij ? ? C(1') 0.91(2) -0.341(6) 0.30(2) 0.06(2) Uij ? ? C(2) 0.60(1) -0.303(3) -0.06(1) 0.01(1) Uij ? ? C(2') 0.71(1) -0.301(4) 0.00(1) 0.02(2) Uij ? ? C(4) 0.340(7) -0.224(2) 0.163(7) 0.03(1) Uij ? ? H(1) 0.3621 -0.2679 0.2700 0.0427 Uij ? ? H(2) 0.1818 -0.2243 -0.0247 0.0427 Uij ? ? H(3) 0.4775 -0.3139 -0.1944 0.0000 Uij ? ? 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 Ag(1) 0.047(2) 0.030(2) 0.034(2) -0.010(1) 0.024(1) -0.008(1) Ag(2) 0.151(7) 0.093(5) 0.088(5) -0.050(5) 0.079(5) -0.007(4) Ag(3) 0.23(1) 0.026(4) 0.048(5) 0.029(5) 0.034(6) 0.023(3) P(1) 0.025(5) 0.033(5) 0.018(4) -0.004(4) 0.012(4) 0.003(3) O(3) 0.05(2) 0.04(1) 0.03(1) 0.00(1) 0.02(1) 0.00(1) O(4) 0.03(2) 0.06(2) 0.04(1) -0.02(1) 0.03(1) -0.01(1) O(5) 0.03(1) 0.05(2) 0.02(1) -0.01(1) 0.00(1) 0.01(1) N(3) 0.04(2) 0.02(1) 0.04(2) 0.00(1) 0.03(1) -0.01(1) C(4) 0.04(2) 0.04(2) 0.04(2) -0.03(2) 0.02(2) -0.02(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _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 1297 _refine_ls_number_parameters 112 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.1389 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1507 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 9.633 _refine_ls_shift/esd_max 2.2290 _refine_ls_shift/esd_mean ? _refine_diff_density_min -3.91 _refine_diff_density_max 8.25 #------------------------------------------------------------------------------ _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 Ag(1) Ag(1) 3.083(5) ? ? yes Ag(1) O(3) 2.21(2) ? ? yes Ag(1) O(4) 2.23(2) ? ? yes Ag(2) O(3) 2.27(2) ? ? yes Ag(2) O(3) 2.27(2) ? ? yes Ag(3) Ag(3) 2.87(2) ? ? yes Ag(3) O(1) 2.30(6) ? ? yes Ag(3) O(1') 2.36(5) ? ? yes Ag(3) O(2) 2.32(7) ? ? yes Ag(3) O(2') 2.42(7) ? ? yes P(1) O(3) 1.59(2) ? ? yes P(1) O(4) 1.48(2) ? ? yes P(1) O(5) 1.51(2) ? ? yes P(1) C(4) 1.86(3) ? ? yes O(1) O(1') 0.81(7) ? ? yes O(1) C(1) 1.11(8) ? ? yes O(1) C(1') 1.1(1) ? ? yes O(1') C(1) 1.63(9) ? ? yes O(1') C(1') 0.87(10) ? ? yes O(2) O(2') 1.71(8) ? ? yes O(2) C(1) 1.13(9) ? ? yes O(2') C(1) 1.74(9) ? ? yes O(2') C(1') 1.4(1) ? ? yes N(3) C(2) 1.52(6) ? ? yes N(3) C(2') 1.51(7) ? ? yes N(3) C(4) 1.50(4) ? ? yes C(1) C(1') 1.1(1) ? ? yes C(1) C(2) 1.50(9) ? ? yes C(1) C(2') 1.44(9) ? ? yes C(1') C(2') 1.6(1) ? ? yes C(2) C(2') 0.50(8) ? ? 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 Ag(1) Ag(1) O(3) 86.1(6) ? ? ? yes Ag(1) Ag(1) O(4) 81.0(6) ? ? ? yes O(3) Ag(1) O(4) 166.8(8) ? ? ? yes O(3) Ag(2) O(3) 180.0000(1) ? ? ? yes Ag(3) Ag(3) O(1) 83(1) ? ? ? yes Ag(3) Ag(3) O(1') 95(1) ? ? ? yes Ag(3) Ag(3) O(2) 72(1) ? ? ? yes Ag(3) Ag(3) O(2') 144(1) ? ? ? yes O(1) Ag(3) O(1') 20(1) ? ? ? yes O(1) Ag(3) O(2) 156(2) ? ? ? yes O(1) Ag(3) O(2') 103(2) ? ? ? yes O(1') Ag(3) O(2) 160(2) ? ? ? yes O(1') Ag(3) O(2') 102(2) ? ? ? yes O(2) Ag(3) O(2') 95(2) ? ? ? yes O(3) P(1) O(4) 114(1) ? ? ? yes O(3) P(1) O(5) 112(1) ? ? ? yes O(3) P(1) C(4) 108(1) ? ? ? yes O(4) P(1) O(5) 112(1) ? ? ? yes O(4) P(1) C(4) 101(1) ? ? ? yes O(5) P(1) C(4) 106(1) ? ? ? yes Ag(3) O(1) O(1') 84(6) ? ? ? yes Ag(3) O(1) C(1) 123(5) ? ? ? yes Ag(3) O(1) C(1') 105(7) ? ? ? yes O(1') O(1) C(1) 114(8) ? ? ? yes O(1') O(1) C(1') 53(6) ? ? ? yes C(1) O(1) C(1') 61(7) ? ? ? yes Ag(3) O(1') O(1) 75(6) ? ? ? yes Ag(3) O(1') C(1) 98(3) ? ? ? yes Ag(3) O(1') C(1') 109(7) ? ? ? yes O(1) O(1') C(1) 38(5) ? ? ? yes O(1) O(1') C(1') 77(8) ? ? ? yes C(1) O(1') C(1') 39(7) ? ? ? yes Ag(3) O(2) O(2') 80(3) ? ? ? yes Ag(3) O(2) C(1) 137(6) ? ? ? yes O(2') O(2) C(1) 72(5) ? ? ? yes Ag(3) O(2') O(2) 98(3) ? ? ? yes Ag(3) O(2') C(1) 119(4) ? ? ? yes Ag(3) O(2') C(1') 136(5) ? ? ? yes O(2) O(2') C(1) 38(3) ? ? ? yes O(2) O(2') C(1') 77(5) ? ? ? yes C(1) O(2') C(1') 39(4) ? ? ? yes Ag(1) O(3) Ag(2) 93.9(9) ? ? ? yes Ag(1) O(3) P(1) 113(1) ? ? ? yes Ag(2) O(3) P(1) 138(1) ? ? ? yes Ag(1) O(4) P(1) 117(1) ? ? ? yes C(2) N(3) C(2') 19(3) ? ? ? yes C(2) N(3) C(4) 104(3) ? ? ? yes C(2') N(3) C(4) 119(3) ? ? ? yes O(1) C(1) O(1') 26(3) ? ? ? yes O(1) C(1) O(2) 118(8) ? ? ? yes O(1) C(1) O(2') 90(6) ? ? ? yes O(1) C(1) C(1') 56(6) ? ? ? yes O(1) C(1) C(2) 127(7) ? ? ? yes O(1) C(1) C(2') 115(7) ? ? ? yes O(1') C(1) O(2) 128(7) ? ? ? yes O(1') C(1) O(2') 74(4) ? ? ? yes O(1') C(1) C(1') 30(5) ? ? ? yes O(1') C(1) C(2) 110(5) ? ? ? yes O(1') C(1) C(2') 93(5) ? ? ? yes O(2) C(1) O(2') 69(5) ? ? ? yes O(2) C(1) C(1') 121(9) ? ? ? yes O(2) C(1) C(2) 114(7) ? ? ? yes O(2) C(1) C(2') 121(7) ? ? ? yes O(2') C(1) C(1') 53(6) ? ? ? yes O(2') C(1) C(2) 107(5) ? ? ? yes O(2') C(1) C(2') 92(5) ? ? ? yes C(1') C(1) C(2) 94(7) ? ? ? yes C(1') C(1) C(2') 74(7) ? ? ? yes C(2) C(1) C(2') 19(3) ? ? ? yes O(1) C(1') O(1') 48(6) ? ? ? yes O(1) C(1') O(2') 113(9) ? ? ? yes O(1) C(1') C(1) 61(7) ? ? ? yes O(1) C(1') C(2') 110(9) ? ? ? yes O(1') C(1') O(2') 126(10) ? ? ? yes O(1') C(1') C(1) 110(11) ? ? ? yes O(1') C(1') C(2') 131(10) ? ? ? yes O(2') C(1') C(1) 87(8) ? ? ? yes O(2') C(1') C(2') 101(7) ? ? ? yes C(1) C(1') C(2') 62(6) ? ? ? yes N(3) C(2) C(1) 107(4) ? ? ? yes N(3) C(2) C(2') 80(11) ? ? ? yes C(1) C(2) C(2') 73(11) ? ? ? yes N(3) C(2') C(1) 110(5) ? ? ? yes N(3) C(2') C(1') 105(5) ? ? ? yes N(3) C(2') C(2) 80(11) ? ? ? yes C(1) C(2') C(1') 43(4) ? ? ? yes C(1) C(2') C(2) 86(12) ? ? ? yes C(1') C(2') C(2) 129(13) ? ? ? yes P(1) C(4) N(3) 110(1) ? ? ? yes #------------------------------------------------------------------------------ #===END