# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Giovanni De Munno' _publ_contact_author_address ; Dipartimento di Chimica Universita della Calabria 87030 Arcavacata di Rende Cosenza ITALY ; _publ_contact_author_email DEMUNNO@UNICAL.IT _publ_contact_letter ; Dear Sir/Madam I am sending the cif file of the paper B511009B: "The counter-ion as useful tool to get complexes of cytosine with alkali metal ions" The compounds have been identified in the paper with numbers 1-3. (in this cif file they have been called data_(1)-data_(3)). For further comunications or informations contact me at this E-mail address: demunno@unical.it Yours sincerely Giovanni De Munno ; _publ_section_title ; The counter-ion as useful tool to get complexes of cytosine with alkali metal ions ; loop_ _publ_author_name _publ_author_address 'Donatella Armentano' ; Dipartimento di Chimica Universita della Calabria, Via P. Bucci 14/c I-87030 Arcavacata di Rende, Cosenza Italy ; 'G.De Munno' ; Dipartimento di Chimica Universita della Calabria, Via P. Bucci 14/c I-87030 Arcavacata di Rende, Cosenza Italy ; 'Rachele Rossi' ; Dipartimento di Chimica Universita della Calabria, Via P. Bucci 14/c I-87030 Arcavacata di Rende, Cosenza Italy ; # 5. CHEMICAL DATA data_1 _database_code_depnum_ccdc_archive 'CCDC 271107' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H11 B F4 N6 O2' _chemical_formula_weight 310.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2263(16) _cell_length_b 8.5046(17) _cell_length_c 9.812(2) _cell_angle_alpha 111.91(3) _cell_angle_beta 90.79(3) _cell_angle_gamma 102.23(3) _cell_volume 619.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1235 _cell_measurement_theta_min 4.42 _cell_measurement_theta_max 28.08 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 316 _exptl_absorpt_coefficient_mu 0.160 _exptl_absorpt_correction_type none _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 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4275 _diffrn_reflns_av_R_equivalents 0.0149 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 28.17 _reflns_number_total 2795 _reflns_number_gt 1974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius X8 APEX' _computing_cell_refinement 'Bruker-Nonius X8 APEX' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1484P)^2^+0.1501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2795 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.2620 _refine_ls_wR_factor_gt 0.2534 _refine_ls_goodness_of_fit_ref 1.242 _refine_ls_restrained_S_all 1.242 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.0056(3) 0.6381(3) -0.2546(3) 0.0393(6) Uani 1 1 d . . . H1 H 0.0292 0.5535 -0.2365 0.047 Uiso 1 1 calc R . . C2 C 0.0855(3) 0.8050(3) -0.1671(3) 0.0354(6) Uani 1 1 d . . . O2 O 0.1864(3) 0.8393(2) -0.0604(2) 0.0466(6) Uani 1 1 d . . . N3 N 0.0448(3) 0.9332(3) -0.2034(2) 0.0352(5) Uani 1 1 d . . . H3 H 0.098(4) 1.030(4) -0.159(4) 0.043(8) Uiso 1 1 d . . . C4 C -0.0696(3) 0.9041(3) -0.3158(3) 0.0365(6) Uani 1 1 d . . . N4 N -0.1002(3) 1.0375(3) -0.3382(3) 0.0465(6) Uani 1 1 d . . . H4A H -0.0481 1.1416 -0.2819 0.056 Uiso 1 1 calc R . . H4B H -0.1725 1.0214 -0.4091 0.056 Uiso 1 1 calc R . . C5 C -0.1505(4) 0.7274(3) -0.4029(3) 0.0416(7) Uani 1 1 d . . . H5 H -0.2299 0.7004 -0.4816 0.050 Uiso 1 1 calc R . . C6 C -0.1095(3) 0.6014(3) -0.3687(3) 0.0406(7) Uani 1 1 d . . . H6 H -0.1614 0.4856 -0.4249 0.049 Uiso 1 1 calc R . . N11 N 0.2627(3) 0.5788(3) 0.0280(3) 0.0404(6) Uani 1 1 d . . . H11 H 0.2375 0.6622 0.0092 0.049 Uiso 1 1 calc R . . C21 C 0.1886(3) 0.4102(3) -0.0626(3) 0.0358(6) Uani 1 1 d . . . O21 O 0.0857(3) 0.3818(2) -0.1686(2) 0.0484(6) Uani 1 1 d . . . N31 N 0.2296(3) 0.2783(3) -0.0342(2) 0.0353(5) Uani 1 1 d . . . C41 C 0.3446(3) 0.3157(3) 0.0785(3) 0.0359(6) Uani 1 1 d . . . N41 N 0.3891(3) 0.1850(3) 0.0984(3) 0.0488(7) Uani 1 1 d . . . H41A H 0.3447 0.0794 0.0399 0.059 Uiso 1 1 calc R . . H41B H 0.4626 0.2054 0.1698 0.059 Uiso 1 1 calc R . . C51 C 0.4188(4) 0.4913(3) 0.1757(3) 0.0398(6) Uani 1 1 d . . . H51 H 0.4950 0.5161 0.2561 0.048 Uiso 1 1 calc R . . C61 C 0.3734(4) 0.6190(3) 0.1455(3) 0.0415(7) Uani 1 1 d . . . H61 H 0.4185 0.7351 0.2057 0.050 Uiso 1 1 calc R . . B1 B 0.5946(4) 0.1722(4) 0.4110(4) 0.0437(8) Uani 1 1 d . . . F1 F 0.4667(3) 0.1735(3) 0.5002(3) 0.0706(7) Uani 1 1 d . . . F2 F 0.6209(3) 0.3208(2) 0.3771(2) 0.0657(6) Uani 1 1 d . . . F3 F 0.5521(3) 0.0290(2) 0.2810(2) 0.0756(7) Uani 1 1 d . . . F4 F 0.7405(2) 0.1756(3) 0.4850(2) 0.0609(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0429(13) 0.0242(10) 0.0472(13) 0.0116(9) -0.0053(10) 0.0054(9) C2 0.0381(14) 0.0265(11) 0.0389(13) 0.0111(9) -0.0044(11) 0.0051(9) O2 0.0551(13) 0.0295(9) 0.0510(12) 0.0149(8) -0.0190(10) 0.0040(8) N3 0.0373(12) 0.0245(10) 0.0402(12) 0.0112(9) -0.0077(10) 0.0031(9) C4 0.0368(14) 0.0314(12) 0.0386(14) 0.0111(10) -0.0022(11) 0.0068(10) N4 0.0517(15) 0.0371(12) 0.0487(14) 0.0154(10) -0.0151(11) 0.0094(10) C5 0.0397(15) 0.0348(13) 0.0414(14) 0.0077(11) -0.0103(12) 0.0046(10) C6 0.0398(15) 0.0276(12) 0.0443(15) 0.0057(10) -0.0031(12) 0.0026(10) N11 0.0458(13) 0.0245(10) 0.0496(13) 0.0134(9) -0.0030(10) 0.0074(9) C21 0.0355(13) 0.0269(11) 0.0428(14) 0.0124(10) -0.0034(11) 0.0048(9) O21 0.0532(13) 0.0308(9) 0.0583(13) 0.0171(8) -0.0180(10) 0.0057(8) N31 0.0387(12) 0.0243(10) 0.0406(12) 0.0120(8) -0.0046(10) 0.0040(8) C41 0.0380(14) 0.0292(12) 0.0374(13) 0.0131(10) -0.0017(11) 0.0013(10) N41 0.0591(16) 0.0318(11) 0.0518(14) 0.0160(10) -0.0203(12) 0.0050(10) C51 0.0423(15) 0.0336(13) 0.0370(14) 0.0112(10) -0.0061(12) 0.0005(11) C61 0.0433(15) 0.0294(12) 0.0439(15) 0.0097(10) -0.0002(12) 0.0008(10) B1 0.0470(18) 0.0363(15) 0.0442(17) 0.0163(12) -0.0127(15) 0.0020(13) F1 0.0619(13) 0.0778(14) 0.0825(15) 0.0384(12) 0.0074(11) 0.0241(11) F2 0.0793(14) 0.0421(10) 0.0726(13) 0.0302(9) -0.0298(11) -0.0048(9) F3 0.1124(19) 0.0398(10) 0.0564(12) 0.0095(8) -0.0216(12) -0.0008(11) F4 0.0499(11) 0.0589(12) 0.0798(14) 0.0360(10) -0.0145(10) 0.0088(9) _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 N1 C6 1.354(4) . ? N1 C2 1.365(3) . ? C2 O2 1.231(3) . ? C2 N3 1.367(3) . ? N3 C4 1.353(3) . ? C4 N4 1.306(3) . ? C4 C5 1.426(4) . ? C5 C6 1.340(4) . ? N11 C61 1.349(4) . ? N11 C21 1.371(3) . ? C21 O21 1.249(3) . ? C21 N31 1.357(3) . ? N31 C41 1.341(3) . ? C41 N41 1.320(4) . ? C41 C51 1.430(3) . ? C51 C61 1.348(4) . ? B1 F3 1.371(4) . ? B1 F1 1.377(4) . ? B1 F4 1.383(4) . ? B1 F2 1.398(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 N1 C2 122.1(2) . . ? O2 C2 N1 122.3(2) . . ? O2 C2 N3 121.6(2) . . ? N1 C2 N3 116.0(2) . . ? C4 N3 C2 124.3(2) . . ? N4 C4 N3 118.8(2) . . ? N4 C4 C5 123.8(3) . . ? N3 C4 C5 117.4(2) . . ? C6 C5 C4 118.4(2) . . ? C5 C6 N1 121.7(2) . . ? C61 N11 C21 122.7(2) . . ? O21 C21 N31 121.7(2) . . ? O21 C21 N11 119.5(2) . . ? N31 C21 N11 118.8(2) . . ? C41 N31 C21 119.4(2) . . ? N41 C41 N31 118.1(2) . . ? N41 C41 C51 119.9(3) . . ? N31 C41 C51 122.0(2) . . ? C61 C51 C41 117.0(3) . . ? C51 C61 N11 120.1(2) . . ? F3 B1 F1 109.9(3) . . ? F3 B1 F4 111.7(3) . . ? F1 B1 F4 109.6(3) . . ? F3 B1 F2 107.9(2) . . ? F1 B1 F2 109.5(3) . . ? F4 B1 F2 108.2(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O21 0.86 1.95 2.804(3) 172 . N11 H11 O2 0.86 1.98 2.840(3) 173 . N3 H3 N31 0.80(3) 2.05(3) 2.843(3) 177(3) 1_565 N4 H4A O21 0.86 1.98 2.842(3) 174 1_565 N41 H41A O2 0.86 2.04 2.878(3) 164 1_545 N41 H41B F2 0.86 2.17 3.002(3) 164 . N41 H41B F3 0.86 2.38 3.038(4) 134 . N4 H4B F4 0.86 2.17 2.866(3) 138 1_464 N4 H4B F1 0.86 2.56 3.207(4) 133 2_565 _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 28.17 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.530 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.088 #==END data_2 _database_code_depnum_ccdc_archive 'CCDC 271108' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H23 Cl3 N9 Na3 O19' _chemical_formula_weight 772.71 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' Na Na 0.0362 0.0249 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.014(3) _cell_length_b 11.025(3) _cell_length_c 14.399(3) _cell_angle_alpha 78.36(2) _cell_angle_beta 84.60(2) _cell_angle_gamma 75.62(2) _cell_volume 1506.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 15 _cell_measurement_theta_max 30 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.442 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8607 _exptl_absorpt_correction_T_max 0.9247 _exptl_absorpt_process_details psi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ' R3m/V automatic four-circle diffractometer ' _diffrn_measurement_method omega/2-theta-scans _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.6 _diffrn_reflns_number 6988 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.06 _reflns_number_total 6603 _reflns_number_gt 3354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker P3' _computing_cell_refinement 'Bruker P3' _computing_data_reduction XDISK _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1275P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6603 _refine_ls_number_parameters 439 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1280 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.2173 _refine_ls_wR_factor_gt 0.1888 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.66091(17) 1.05777(15) 0.01779(12) 0.0395(4) Uani 1 1 d . . . Na2 Na 0.99269(17) 1.13903(15) 0.03884(11) 0.0360(4) Uani 1 1 d . . . Na3 Na 0.68889(17) 0.78818(16) -0.07600(12) 0.0390(4) Uani 1 1 d . . . O1W O 0.8945(3) 0.8174(3) -0.1615(2) 0.0408(7) Uani 1 1 d D . . H1W H 0.901(5) 0.896(3) -0.198(3) 0.060 Uiso 1 1 d D . . H2W H 0.935(5) 0.762(3) -0.200(3) 0.060 Uiso 1 1 d D . . O2W O 0.7873(3) 1.1118(3) 0.1285(2) 0.0398(7) Uani 1 1 d D . . H3W H 0.799(5) 1.035(3) 0.170(3) 0.060 Uiso 1 1 d D . . H4W H 0.749(5) 1.174(3) 0.164(3) 0.060 Uiso 1 1 d D . . O3W O 0.5065(3) 1.2594(3) -0.0122(2) 0.0442(8) Uani 1 1 d D . . H5W H 0.506(5) 1.253(5) -0.073(2) 0.060 Uiso 1 1 d D . . H6W H 0.545(5) 1.324(4) -0.008(3) 0.060 Uiso 1 1 d D . . O4W O 0.6014(5) 0.7634(4) -0.2146(3) 0.0714(12) Uani 1 1 d D . . H7W H 0.660(4) 0.739(5) -0.269(3) 0.060 Uiso 1 1 d D . . H8W H 0.518(3) 0.747(5) -0.227(3) 0.060 Uiso 1 1 d D . . N1 N 0.5511(4) 1.0386(4) -0.2707(3) 0.0435(9) Uani 1 1 d . . . H1 H 0.5638 0.9577 -0.2668 0.052 Uiso 1 1 calc R . . C2 C 0.5456(4) 1.0848(4) -0.1889(3) 0.0335(9) Uani 1 1 d . . . O2 O 0.5585(3) 1.0100(3) -0.1106(2) 0.0386(7) Uani 1 1 d . . . N3 N 0.5243(4) 1.2113(4) -0.1952(3) 0.0395(9) Uani 1 1 d . . . C4 C 0.5099(5) 1.2885(5) -0.2801(4) 0.0511(13) Uani 1 1 d . . . N4 N 0.4880(5) 1.4135(4) -0.2819(4) 0.0731(15) Uani 1 1 d . . . H4B H 0.4836 1.4414 -0.2299 0.088 Uiso 1 1 calc R . . H4A H 0.4782 1.4660 -0.3352 0.088 Uiso 1 1 calc R . . C5 C 0.5166(6) 1.2419(6) -0.3636(4) 0.0600(15) Uani 1 1 d . . . H5 H 0.5069 1.2966 -0.4221 0.072 Uiso 1 1 calc R . . C6 C 0.5377(5) 1.1133(6) -0.3570(4) 0.0583(15) Uani 1 1 d . . . H6 H 0.5427 1.0782 -0.4111 0.070 Uiso 1 1 calc R . . N11 N 0.8499(4) 1.2633(3) -0.2006(3) 0.0380(8) Uani 1 1 d . . . H11 H 0.8427 1.3058 -0.1557 0.046 Uiso 1 1 calc R . . C21 C 0.8748(4) 1.1335(4) -0.1779(3) 0.0297(9) Uani 1 1 d . . . O21 O 0.8866(3) 1.0801(3) -0.0927(2) 0.0367(7) Uani 1 1 d . . . N31 N 0.8851(3) 1.0680(3) -0.2485(2) 0.0324(8) Uani 1 1 d . . . C41 C 0.8733(4) 1.1307(4) -0.3384(3) 0.0367(10) Uani 1 1 d . . . N41 N 0.8858(5) 1.0628(4) -0.4064(3) 0.0535(11) Uani 1 1 d . . . H41B H 0.9010 0.9811 -0.3921 0.064 Uiso 1 1 calc R . . H41A H 0.8787 1.1005 -0.4648 0.064 Uiso 1 1 calc R . . C51 C 0.8474(5) 1.2656(5) -0.3618(3) 0.0453(11) Uani 1 1 d . . . H51 H 0.8388 1.3085 -0.4243 0.054 Uiso 1 1 calc R . . C61 C 0.8362(5) 1.3275(4) -0.2907(3) 0.0422(11) Uani 1 1 d . . . H61 H 0.8187 1.4160 -0.3029 0.051 Uiso 1 1 calc R . . N12 N 0.8271(4) 0.6598(3) 0.1632(2) 0.0374(8) Uani 1 1 d . . . H12 H 0.8332 0.6180 0.1180 0.045 Uiso 1 1 calc R . . C22 C 0.8033(4) 0.7893(4) 0.1416(3) 0.0299(9) Uani 1 1 d . . . O22 O 0.7917(3) 0.8445(3) 0.05605(19) 0.0351(7) Uani 1 1 d . . . N32 N 0.7948(3) 0.8553(3) 0.2117(2) 0.0327(8) Uani 1 1 d . . . C42 C 0.8080(4) 0.7919(4) 0.3010(3) 0.0364(10) Uani 1 1 d . . . N42 N 0.7985(4) 0.8605(4) 0.3691(3) 0.0517(11) Uani 1 1 d . . . H42B H 0.7845 0.9421 0.3545 0.062 Uiso 1 1 calc R . . H42A H 0.8065 0.8230 0.4274 0.062 Uiso 1 1 calc R . . C52 C 0.8337(5) 0.6570(4) 0.3249(3) 0.0442(11) Uani 1 1 d . . . H52 H 0.8444 0.6140 0.3873 0.053 Uiso 1 1 calc R . . C62 C 0.8415(5) 0.5953(4) 0.2530(3) 0.0459(11) Uani 1 1 d . . . H62 H 0.8571 0.5069 0.2651 0.055 Uiso 1 1 calc R . . Cl1 Cl 0.77630(14) 0.45690(10) -0.00600(9) 0.0504(3) Uani 1 1 d . . . O3 O 0.8191(4) 0.5729(3) -0.0239(3) 0.0539(9) Uani 1 1 d . . . O4 O 0.7315(10) 0.4313(5) 0.0882(4) 0.173(4) Uani 1 1 d . . . O5 O 0.6682(5) 0.4676(5) -0.0686(5) 0.122(2) Uani 1 1 d . . . O6 O 0.8863(4) 0.3559(3) -0.0280(3) 0.0641(11) Uani 1 1 d . . . Cl2 Cl 0.87670(19) 0.68196(14) -0.38771(10) 0.0700(5) Uani 1 1 d . . . O7 O 0.9805(13) 0.6169(8) -0.4379(5) 0.231(6) Uani 1 1 d . . . O8 O 0.8779(6) 0.6371(4) -0.2922(3) 0.1021(19) Uani 1 1 d . . . O9 O 0.7754(13) 0.6358(10) -0.4196(8) 0.243(6) Uani 1 1 d . . . O10 O 0.8294(10) 0.8102(5) -0.4128(5) 0.163(3) Uani 1 1 d . . . Cl3 Cl 0.31908(19) 0.77189(15) -0.36489(10) 0.0716(5) Uani 1 1 d . . . O11 O 0.1932(8) 0.8558(7) -0.3743(6) 0.163(3) Uani 1 1 d . . . O12 O 0.4138(9) 0.8541(7) -0.4017(5) 0.158(3) Uani 1 1 d . . . O13 O 0.3486(6) 0.7183(5) -0.2704(3) 0.1003(17) Uani 1 1 d . . . O14 O 0.3348(8) 0.6767(6) -0.4164(4) 0.133(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0389(10) 0.0334(9) 0.0453(10) -0.0102(7) -0.0123(8) -0.0008(7) Na2 0.0339(9) 0.0344(9) 0.0385(9) -0.0074(7) -0.0046(7) -0.0042(7) Na3 0.0364(10) 0.0373(9) 0.0431(10) -0.0084(7) -0.0058(8) -0.0064(7) O1W 0.055(2) 0.0331(16) 0.0374(17) -0.0123(13) 0.0014(15) -0.0132(15) O2W 0.0450(19) 0.0384(17) 0.0380(17) -0.0132(13) -0.0018(14) -0.0082(15) O3W 0.0448(19) 0.0343(17) 0.056(2) -0.0135(15) 0.0030(16) -0.0112(14) O4W 0.070(3) 0.078(3) 0.071(3) -0.033(2) -0.021(2) -0.003(2) N1 0.041(2) 0.053(2) 0.037(2) -0.0100(18) -0.0032(17) -0.0098(18) C2 0.024(2) 0.039(2) 0.035(2) -0.0073(19) -0.0005(17) -0.0034(18) O2 0.0443(18) 0.0340(16) 0.0356(16) -0.0054(13) -0.0066(13) -0.0047(13) N3 0.032(2) 0.042(2) 0.039(2) 0.0006(16) -0.0009(16) -0.0071(16) C4 0.035(3) 0.053(3) 0.058(3) 0.008(2) -0.001(2) -0.013(2) N4 0.072(3) 0.050(3) 0.088(4) 0.023(3) -0.011(3) -0.023(2) C5 0.054(3) 0.083(4) 0.036(3) 0.013(3) -0.006(2) -0.021(3) C6 0.041(3) 0.099(5) 0.033(3) -0.009(3) 0.003(2) -0.017(3) N11 0.043(2) 0.0292(18) 0.043(2) -0.0083(16) -0.0060(17) -0.0084(16) C21 0.029(2) 0.028(2) 0.033(2) -0.0078(17) -0.0052(17) -0.0064(17) O21 0.0440(18) 0.0344(16) 0.0310(16) -0.0084(12) -0.0027(13) -0.0057(13) N31 0.0328(19) 0.0301(18) 0.0348(19) -0.0063(15) -0.0013(15) -0.0080(15) C41 0.032(2) 0.044(2) 0.035(2) -0.0102(19) 0.0010(18) -0.0093(19) N41 0.068(3) 0.058(3) 0.035(2) -0.0117(19) -0.005(2) -0.012(2) C51 0.050(3) 0.047(3) 0.035(2) 0.003(2) -0.008(2) -0.011(2) C61 0.044(3) 0.025(2) 0.053(3) 0.005(2) -0.009(2) -0.0074(19) N12 0.046(2) 0.0296(18) 0.036(2) -0.0071(15) -0.0059(16) -0.0047(16) C22 0.022(2) 0.031(2) 0.035(2) -0.0070(17) -0.0010(16) -0.0034(16) O22 0.0380(17) 0.0330(15) 0.0310(15) -0.0050(12) -0.0019(13) -0.0028(13) N32 0.0294(19) 0.0336(18) 0.0358(19) -0.0096(15) -0.0046(15) -0.0051(15) C42 0.030(2) 0.042(2) 0.038(2) -0.0068(19) -0.0029(18) -0.0101(19) N42 0.062(3) 0.060(3) 0.036(2) -0.0129(19) -0.0045(19) -0.017(2) C52 0.046(3) 0.044(3) 0.038(3) 0.005(2) -0.009(2) -0.010(2) C62 0.046(3) 0.032(2) 0.052(3) 0.002(2) -0.008(2) -0.001(2) Cl1 0.0592(8) 0.0288(5) 0.0634(8) -0.0149(5) 0.0106(6) -0.0105(5) O3 0.055(2) 0.0319(17) 0.076(2) -0.0131(16) -0.0098(18) -0.0086(15) O4 0.326(10) 0.072(3) 0.102(4) -0.025(3) 0.115(6) -0.051(5) O5 0.078(3) 0.070(3) 0.233(7) -0.049(4) -0.057(4) -0.013(3) O6 0.078(3) 0.0303(17) 0.079(3) -0.0209(17) -0.017(2) 0.0092(17) Cl2 0.1066(13) 0.0495(8) 0.0476(8) 0.0020(6) -0.0094(8) -0.0132(8) O7 0.349(15) 0.168(8) 0.098(5) -0.019(5) 0.098(7) 0.042(9) O8 0.173(5) 0.064(3) 0.043(2) -0.010(2) -0.006(3) 0.021(3) O9 0.283(14) 0.193(9) 0.286(13) 0.020(8) -0.160(11) -0.114(9) O10 0.310(10) 0.055(3) 0.113(5) 0.010(3) -0.075(6) -0.018(5) Cl3 0.1058(13) 0.0623(9) 0.0416(7) -0.0094(6) -0.0248(8) -0.0026(9) O11 0.135(6) 0.121(5) 0.205(8) -0.020(5) -0.058(5) 0.033(5) O12 0.217(8) 0.146(6) 0.127(5) 0.025(4) -0.041(5) -0.101(6) O13 0.133(4) 0.106(4) 0.054(3) 0.003(3) -0.020(3) -0.022(3) O14 0.227(7) 0.107(4) 0.077(4) -0.047(3) 0.005(4) -0.041(5) _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 O3W 2.356(4) . ? Na1 O22 2.373(3) . ? Na1 O2W 2.373(3) . ? Na1 O2 2.401(3) . ? Na1 O2 2.652(4) 2_675 ? Na1 O21 2.672(4) . ? Na2 O1W 2.370(3) 2_775 ? Na2 O2W 2.374(4) . ? Na2 O6 2.403(4) 1_565 ? Na2 O21 2.422(3) 2_775 ? Na2 O22 2.470(3) 2_775 ? Na2 O21 2.521(3) . ? Na3 O3W 2.343(4) 2_675 ? Na3 O4W 2.344(4) . ? Na3 O1W 2.356(4) . ? Na3 O3 2.413(4) . ? Na3 O2 2.446(3) . ? Na3 O22 2.495(3) . ? O1W Na2 2.370(3) 2_775 ? O3W Na3 2.343(4) 2_675 ? N1 C6 1.343(6) . ? N1 C2 1.366(5) . ? C2 O2 1.251(5) . ? C2 N3 1.343(6) . ? O2 Na1 2.652(4) 2_675 ? N3 C4 1.339(6) . ? C4 N4 1.336(7) . ? C4 C5 1.389(8) . ? C5 C6 1.365(8) . ? N11 C61 1.347(5) . ? N11 C21 1.366(5) . ? C21 O21 1.251(5) . ? C21 N31 1.344(5) . ? O21 Na2 2.422(3) 2_775 ? N31 C41 1.340(5) . ? C41 N41 1.327(6) . ? C41 C51 1.419(6) . ? C51 C61 1.322(7) . ? N12 C62 1.347(6) . ? N12 C22 1.363(5) . ? C22 O22 1.261(5) . ? C22 N32 1.343(5) . ? O22 Na2 2.470(3) 2_775 ? N32 C42 1.335(5) . ? C42 N42 1.337(6) . ? C42 C52 1.420(6) . ? C52 C62 1.335(7) . ? Cl1 O4 1.383(5) . ? Cl1 O3 1.415(3) . ? Cl1 O6 1.422(4) . ? Cl1 O5 1.441(5) . ? O6 Na2 2.403(4) 1_545 ? Cl2 O7 1.347(7) . ? Cl2 O10 1.359(5) . ? Cl2 O8 1.365(4) . ? Cl2 O9 1.392(9) . ? Cl3 O11 1.366(7) . ? Cl3 O14 1.373(5) . ? Cl3 O13 1.397(4) . ? Cl3 O12 1.464(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3W Na1 O22 172.74(13) . . ? O3W Na1 O2W 94.85(13) . . ? O22 Na1 O2W 88.34(12) . . ? O3W Na1 O2 86.17(12) . . ? O22 Na1 O2 91.61(11) . . ? O2W Na1 O2 171.82(14) . . ? O3W Na1 O2 82.72(11) . 2_675 ? O22 Na1 O2 90.10(11) . 2_675 ? O2W Na1 O2 107.63(12) . 2_675 ? O2 Na1 O2 80.56(12) . 2_675 ? O3W Na1 O21 105.69(12) . . ? O22 Na1 O21 81.21(11) . . ? O2W Na1 O21 81.66(11) . . ? O2 Na1 O21 90.25(11) . . ? O2 Na1 O21 167.19(11) 2_675 . ? O1W Na2 O2W 97.20(12) 2_775 . ? O1W Na2 O6 97.38(13) 2_775 1_565 ? O2W Na2 O6 91.74(14) . 1_565 ? O1W Na2 O21 84.62(11) 2_775 2_775 ? O2W Na2 O21 92.94(12) . 2_775 ? O6 Na2 O21 174.65(14) 1_565 2_775 ? O1W Na2 O22 84.44(11) 2_775 2_775 ? O2W Na2 O22 176.87(12) . 2_775 ? O6 Na2 O22 90.69(13) 1_565 2_775 ? O21 Na2 O22 84.55(11) 2_775 2_775 ? O1W Na2 O21 176.08(12) 2_775 . ? O2W Na2 O21 84.91(11) . . ? O6 Na2 O21 85.83(12) 1_565 . ? O21 Na2 O21 91.99(11) 2_775 . ? O22 Na2 O21 93.30(11) 2_775 . ? O3W Na3 O4W 90.27(16) 2_675 . ? O3W Na3 O1W 175.11(13) 2_675 . ? O4W Na3 O1W 89.91(16) . . ? O3W Na3 O3 90.39(13) 2_675 . ? O4W Na3 O3 99.71(15) . . ? O1W Na3 O3 84.76(13) . . ? O3W Na3 O2 87.64(12) 2_675 . ? O4W Na3 O2 86.45(14) . . ? O1W Na3 O2 97.25(12) . . ? O3 Na3 O2 173.54(13) . . ? O3W Na3 O22 96.19(12) 2_675 . ? O4W Na3 O22 171.09(16) . . ? O1W Na3 O22 84.18(11) . . ? O3 Na3 O22 86.41(12) . . ? O2 Na3 O22 87.69(11) . . ? Na3 O1W Na2 98.73(12) . 2_775 ? Na1 O2W Na2 102.51(12) . . ? Na3 O3W Na1 99.81(13) 2_675 . ? C6 N1 C2 123.3(5) . . ? O2 C2 N3 121.7(4) . . ? O2 C2 N1 120.1(4) . . ? N3 C2 N1 118.2(4) . . ? C2 O2 Na1 120.7(3) . . ? C2 O2 Na3 128.5(3) . . ? Na1 O2 Na3 90.61(11) . . ? C2 O2 Na1 120.0(3) . 2_675 ? Na1 O2 Na1 99.44(12) . 2_675 ? Na3 O2 Na1 89.62(11) . 2_675 ? C4 N3 C2 120.0(4) . . ? N4 C4 N3 117.3(5) . . ? N4 C4 C5 120.7(5) . . ? N3 C4 C5 122.0(5) . . ? C6 C5 C4 117.9(5) . . ? N1 C6 C5 118.6(5) . . ? C61 N11 C21 122.6(4) . . ? O21 C21 N31 122.5(4) . . ? O21 C21 N11 119.3(4) . . ? N31 C21 N11 118.3(4) . . ? C21 O21 Na2 124.7(3) . 2_775 ? C21 O21 Na2 129.5(3) . . ? Na2 O21 Na2 88.01(11) 2_775 . ? C21 O21 Na1 119.7(3) . . ? Na2 O21 Na1 93.72(11) 2_775 . ? Na2 O21 Na1 90.90(10) . . ? C41 N31 C21 119.6(3) . . ? N41 C41 N31 118.0(4) . . ? N41 C41 C51 120.1(4) . . ? N31 C41 C51 121.9(4) . . ? C61 C51 C41 117.1(4) . . ? C51 C61 N11 120.5(4) . . ? C62 N12 C22 122.1(4) . . ? O22 C22 N32 121.4(4) . . ? O22 C22 N12 119.2(4) . . ? N32 C22 N12 119.3(4) . . ? C22 O22 Na1 120.1(2) . . ? C22 O22 Na2 117.0(2) . 2_775 ? Na1 O22 Na2 100.41(12) . 2_775 ? C22 O22 Na3 129.6(3) . . ? Na1 O22 Na3 90.08(11) . . ? Na2 O22 Na3 92.50(11) 2_775 . ? C42 N32 C22 118.9(4) . . ? N32 C42 N42 117.3(4) . . ? N32 C42 C52 122.7(4) . . ? N42 C42 C52 120.0(4) . . ? C62 C52 C42 116.4(4) . . ? C52 C62 N12 120.6(4) . . ? O4 Cl1 O3 109.3(3) . . ? O4 Cl1 O6 110.7(4) . . ? O3 Cl1 O6 110.4(2) . . ? O4 Cl1 O5 111.3(5) . . ? O3 Cl1 O5 108.9(3) . . ? O6 Cl1 O5 106.2(3) . . ? Cl1 O3 Na3 129.9(2) . . ? Cl1 O6 Na2 139.2(3) . 1_545 ? O7 Cl2 O10 121.4(5) . . ? O7 Cl2 O8 114.1(4) . . ? O10 Cl2 O8 114.6(3) . . ? O7 Cl2 O9 94.4(8) . . ? O10 Cl2 O9 102.5(6) . . ? O8 Cl2 O9 105.1(6) . . ? O11 Cl3 O14 112.8(5) . . ? O11 Cl3 O13 113.0(4) . . ? O14 Cl3 O13 109.6(4) . . ? O11 Cl3 O12 102.2(5) . . ? O14 Cl3 O12 110.9(5) . . ? O13 Cl3 O12 108.0(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2W O8 0.90(3) 2.30(4) 3.041(6) 140(4) . O1W H1W N31 0.93(3) 1.87(3) 2.777(5) 167(4) . O2W H3W N32 0.92(3) 1.96(3) 2.825(5) 156(4) . O2W H4W O13 0.93(3) 2.13(3) 3.049(6) 167(4) 2_675 O3W H5W N3 0.90(3) 1.88(3) 2.772(5) 171(5) . O3W H6W O5 0.90(3) 2.24(4) 3.065(6) 152(4) 1_565 O4W H7W O8 0.97(3) 2.22(4) 2.997(7) 136(4) . O4W H8W O13 0.94(3) 1.97(3) 2.910(7) 173(4) . N1 H1 O4W 0.86 2.07 2.906(6) 163 . N11 H11 O6 0.86 2.13 2.955(5) 159 1_565 N12 H12 O3 0.86 2.22 3.050(5) 161 . N41 H41B O10 0.86 2.26 2.996(8) 144 . N42 H42A O10 0.86 2.31 3.109(7) 155 1_556 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.981 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.091 #==END data_3 _database_code_depnum_ccdc_archive 'CCDC 271109' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H21 Cl3 N9 Na3 O18' _chemical_formula_weight 754.70 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' Na Na 0.0362 0.0249 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9433(12) _cell_length_b 10.9857(15) _cell_length_c 14.691(2) _cell_angle_alpha 75.706(7) _cell_angle_beta 70.487(5) _cell_angle_gamma 73.880(5) _cell_volume 1431.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4544 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 21.96 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.460 _exptl_absorpt_correction_type none _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 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13832 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 22.15 _reflns_number_total 3364 _reflns_number_gt 2569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius X8 APEX' _computing_cell_refinement 'Bruker-Nonius X8 APEX' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1312P)^2^+5.8969P] 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 3364 _refine_ls_number_parameters 424 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2434 _refine_ls_wR_factor_gt 0.2286 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na -0.3456(3) 0.5512(3) 0.0247(2) 0.0431(8) Uani 1 1 d . . . Na2 Na -0.0284(3) 0.6387(3) 0.0414(2) 0.0405(8) Uani 1 1 d . . . Na3 Na -0.2746(4) 0.2862(3) -0.0884(2) 0.0526(9) Uani 1 1 d . . . O1W O -0.0373(6) 0.3135(5) -0.1680(4) 0.0443(14) Uani 1 1 d D . . H1W H -0.029(9) 0.393(4) -0.210(5) 0.060 Uiso 1 1 d D . . H2W H 0.032(8) 0.254(5) -0.207(5) 0.060 Uiso 1 1 d D . . O2W O -0.2633(6) 0.6040(5) 0.1410(4) 0.0448(14) Uani 1 1 d D . . H3W H -0.273(9) 0.524(4) 0.182(5) 0.060 Uiso 1 1 d D . . H4W H -0.310(9) 0.665(5) 0.185(4) 0.060 Uiso 1 1 d D . . O3W O -0.4934(6) 0.7561(5) 0.0070(4) 0.0454(14) Uani 1 1 d D . . H5W H -0.470(9) 0.831(5) 0.014(5) 0.060 Uiso 1 1 d D . . H6W H -0.473(9) 0.762(7) -0.061(3) 0.060 Uiso 1 1 d D . . N1 N -0.3553(7) 0.5583(6) -0.2778(5) 0.0404(16) Uani 1 1 d . . . H1 H -0.3405 0.4778 -0.2795 0.048 Uiso 1 1 calc R . . C2 C -0.3903(8) 0.5950(7) -0.1903(6) 0.0338(19) Uani 1 1 d . . . O2 O -0.3985(6) 0.5117(5) -0.1144(4) 0.0421(14) Uani 1 1 d . . . N3 N -0.4170(7) 0.7226(6) -0.1870(5) 0.0386(16) Uani 1 1 d . . . C4 C -0.4059(9) 0.8078(7) -0.2704(5) 0.0375(19) Uani 1 1 d . . . N4 N -0.4328(8) 0.9310(6) -0.2643(6) 0.055(2) Uani 1 1 d . . . H4B H -0.4565 0.9538 -0.2081 0.067 Uiso 1 1 calc R . . H4A H -0.4266 0.9883 -0.3166 0.067 Uiso 1 1 calc R . . C5 C -0.3665(10) 0.7694(9) -0.3616(6) 0.050(2) Uani 1 1 d . . . H5 H -0.3574 0.8293 -0.4192 0.061 Uiso 1 1 calc R . . C6 C -0.3423(9) 0.6428(8) -0.3632(6) 0.045(2) Uani 1 1 d . . . H6 H -0.3170 0.6139 -0.4224 0.055 Uiso 1 1 calc R . . N11 N -0.0888(7) 0.7647(6) -0.2048(5) 0.0412(17) Uani 1 1 d . . . H11 H -0.1164 0.8092 -0.1586 0.049 Uiso 1 1 calc R . . C21 C -0.0682(8) 0.6346(7) -0.1796(6) 0.0316(18) Uani 1 1 d . . . O21 O -0.0889(6) 0.5827(5) -0.0911(4) 0.0406(14) Uani 1 1 d . . . N31 N -0.0251(7) 0.5644(6) -0.2520(4) 0.0365(16) Uani 1 1 d . . . C41 C -0.0020(8) 0.6250(7) -0.3454(6) 0.0361(19) Uani 1 1 d . . . N41 N 0.0431(8) 0.5517(7) -0.4143(5) 0.0518(19) Uani 1 1 d . . . H41B H 0.0562 0.4695 -0.3981 0.062 Uiso 1 1 calc R . . H41A H 0.0592 0.5867 -0.4751 0.062 Uiso 1 1 calc R . . C51 C -0.0235(9) 0.7598(7) -0.3708(6) 0.043(2) Uani 1 1 d . . . H51 H -0.0071 0.8003 -0.4359 0.051 Uiso 1 1 calc R . . C61 C -0.0686(9) 0.8278(7) -0.2974(6) 0.042(2) Uani 1 1 d . . . H61 H -0.0855 0.9171 -0.3106 0.050 Uiso 1 1 calc R . . N12 N -0.2113(7) 0.1494(6) 0.1714(5) 0.0435(17) Uani 1 1 d . . . H12 H -0.1820 0.1088 0.1228 0.052 Uiso 1 1 calc R . . C22 C -0.2374(8) 0.2819(6) 0.1530(6) 0.0318(18) Uani 1 1 d . . . O22 O -0.2198(6) 0.3377(5) 0.0658(4) 0.0412(14) Uani 1 1 d . . . N32 N -0.2770(7) 0.3451(6) 0.2275(5) 0.0377(16) Uani 1 1 d . . . C42 C -0.2965(9) 0.2782(8) 0.3200(6) 0.041(2) Uani 1 1 d . . . N42 N -0.3389(8) 0.3443(7) 0.3925(5) 0.0502(19) Uani 1 1 d . . . H42B H -0.3531 0.4268 0.3800 0.060 Uiso 1 1 calc R . . H42A H -0.3522 0.3047 0.4521 0.060 Uiso 1 1 calc R . . C52 C -0.2734(9) 0.1419(8) 0.3390(6) 0.046(2) Uani 1 1 d . . . H52 H -0.2882 0.0967 0.4028 0.055 Uiso 1 1 calc R . . C62 C -0.2303(9) 0.0809(8) 0.2633(6) 0.045(2) Uani 1 1 d . . . H62 H -0.2131 -0.0083 0.2734 0.054 Uiso 1 1 calc R . . Cl1 Cl -0.2308(3) -0.03814(18) -0.00846(15) 0.0476(7) Uani 1 1 d . . . O3 O -0.1758(8) 0.0720(5) -0.0207(5) 0.069(2) Uani 1 1 d . . . O4 O -0.3318(13) -0.0557(8) 0.0822(6) 0.136(4) Uani 1 1 d . . . O5 O -0.3019(9) -0.0210(7) -0.0823(6) 0.089(2) Uani 1 1 d . . . O6 O -0.1135(8) -0.1471(5) -0.0227(5) 0.0670(19) Uani 1 1 d . . . Cl2 Cl -0.1895(3) 0.2220(2) -0.32657(17) 0.0611(8) Uani 1 1 d . . . O7 O -0.0725(10) 0.1340(8) -0.2902(8) 0.108(3) Uani 1 1 d . . . O8 O -0.3045(8) 0.2611(7) -0.2441(5) 0.074(2) Uani 1 1 d . . . O9 O -0.2323(11) 0.1578(8) -0.3809(7) 0.105(3) Uani 1 1 d . . . O10 O -0.1371(13) 0.3324(8) -0.3816(6) 0.127(4) Uani 1 1 d . . . Cl3 Cl -0.3661(3) 0.7475(2) 0.37224(15) 0.0543(7) Uani 1 1 d . . . O11 O -0.4073(9) 0.6278(6) 0.4066(6) 0.092(3) Uani 1 1 d . . . O12 O -0.4691(8) 0.8403(6) 0.4274(4) 0.0651(18) Uani 1 1 d . . . O13 O -0.3602(12) 0.7887(7) 0.2732(5) 0.110(3) Uani 1 1 d . . . O14 O -0.2247(9) 0.7352(9) 0.3839(7) 0.108(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.055(2) 0.0355(17) 0.0448(19) -0.0102(14) -0.0230(16) -0.0055(15) Na2 0.051(2) 0.0370(17) 0.0389(18) -0.0054(14) -0.0209(15) -0.0094(14) Na3 0.055(2) 0.0415(18) 0.058(2) 0.0020(16) -0.0196(17) -0.0109(16) O1W 0.060(4) 0.035(3) 0.039(3) -0.007(2) -0.011(3) -0.014(3) O2W 0.064(4) 0.035(3) 0.035(3) -0.004(2) -0.013(3) -0.011(3) O3W 0.054(4) 0.035(3) 0.048(3) -0.007(3) -0.014(3) -0.011(3) N1 0.055(5) 0.035(4) 0.036(4) -0.006(3) -0.018(3) -0.010(3) C2 0.033(5) 0.035(5) 0.035(5) -0.002(4) -0.014(4) -0.009(3) O2 0.061(4) 0.028(3) 0.040(3) 0.004(3) -0.022(3) -0.012(3) N3 0.051(5) 0.030(4) 0.039(4) 0.001(3) -0.017(3) -0.014(3) C4 0.039(5) 0.039(5) 0.031(5) 0.003(4) -0.011(4) -0.009(4) N4 0.078(6) 0.033(4) 0.053(5) 0.002(3) -0.021(4) -0.014(4) C5 0.061(6) 0.054(6) 0.038(5) 0.007(4) -0.020(4) -0.020(5) C6 0.044(6) 0.056(6) 0.038(5) -0.015(5) -0.013(4) -0.007(4) N11 0.059(5) 0.033(4) 0.037(4) -0.011(3) -0.016(3) -0.012(3) C21 0.036(5) 0.024(4) 0.035(5) -0.001(4) -0.010(4) -0.010(3) O21 0.054(4) 0.038(3) 0.031(3) -0.005(3) -0.015(3) -0.008(3) N31 0.050(5) 0.033(3) 0.030(4) -0.003(3) -0.013(3) -0.016(3) C41 0.040(5) 0.041(5) 0.033(5) -0.006(4) -0.009(4) -0.018(4) N41 0.081(6) 0.048(4) 0.028(4) -0.008(3) -0.012(4) -0.019(4) C51 0.058(6) 0.035(5) 0.035(5) 0.006(4) -0.015(4) -0.018(4) C61 0.057(6) 0.028(4) 0.045(6) -0.002(4) -0.020(4) -0.013(4) N12 0.056(5) 0.031(4) 0.047(5) -0.009(3) -0.015(3) -0.011(3) C22 0.041(5) 0.020(4) 0.038(5) -0.004(4) -0.012(4) -0.011(3) O22 0.053(4) 0.033(3) 0.038(4) -0.004(3) -0.014(3) -0.010(3) N32 0.040(4) 0.036(4) 0.039(4) -0.006(3) -0.010(3) -0.013(3) C42 0.037(5) 0.042(5) 0.049(6) -0.007(4) -0.010(4) -0.016(4) N42 0.066(5) 0.050(4) 0.036(4) -0.009(3) -0.007(3) -0.022(4) C52 0.052(6) 0.044(5) 0.041(5) 0.003(4) -0.018(4) -0.013(4) C62 0.059(6) 0.028(4) 0.051(6) -0.004(4) -0.017(4) -0.015(4) Cl1 0.0668(16) 0.0275(11) 0.0447(13) -0.0074(9) -0.0100(11) -0.0103(10) O3 0.095(5) 0.025(3) 0.106(5) -0.008(3) -0.054(4) -0.015(3) O4 0.187(11) 0.089(6) 0.065(6) -0.008(5) 0.049(6) -0.028(6) O5 0.110(6) 0.083(5) 0.107(6) -0.022(4) -0.075(5) -0.015(4) O6 0.082(5) 0.034(3) 0.087(5) -0.020(3) -0.036(4) 0.008(3) Cl2 0.086(2) 0.0440(13) 0.0533(15) -0.0139(11) -0.0083(13) -0.0230(13) O7 0.104(7) 0.079(5) 0.146(8) -0.036(5) -0.050(6) 0.006(5) O8 0.081(5) 0.080(5) 0.060(4) -0.018(4) -0.010(4) -0.021(4) O9 0.143(8) 0.097(6) 0.103(6) -0.042(5) -0.049(6) -0.028(6) O10 0.215(11) 0.080(6) 0.068(5) -0.006(5) 0.010(6) -0.071(7) Cl3 0.0758(19) 0.0399(13) 0.0385(13) -0.0027(10) -0.0122(11) -0.0070(11) O11 0.118(7) 0.047(4) 0.094(6) -0.011(4) -0.003(5) -0.028(4) O12 0.091(5) 0.045(4) 0.047(4) -0.013(3) -0.014(3) 0.002(3) O13 0.209(10) 0.064(5) 0.026(4) -0.011(3) -0.029(5) 0.014(5) O14 0.074(6) 0.110(7) 0.145(8) -0.037(6) -0.040(6) -0.004(5) _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 O3W 2.329(6) . ? Na1 O22 2.367(6) . ? Na1 O2W 2.370(6) . ? Na1 O2 2.433(6) . ? Na1 O21 2.614(6) . ? Na1 O2 2.641(6) 2_465 ? Na2 O6 2.339(6) 1_565 ? Na2 O1W 2.377(6) 2_565 ? Na2 O2W 2.383(6) . ? Na2 O21 2.435(6) 2_565 ? Na2 O21 2.472(6) . ? Na2 O22 2.489(6) 2_565 ? Na3 O1W 2.324(7) . ? Na3 O3W 2.334(6) 2_465 ? Na3 O3 2.389(6) . ? Na3 O2 2.440(6) . ? Na3 O8 2.491(8) . ? Na3 O22 2.716(6) . ? O1W Na2 2.377(6) 2_565 ? O3W Na3 2.334(6) 2_465 ? N1 C2 1.347(10) . ? N1 C6 1.356(10) . ? C2 O2 1.250(9) . ? C2 N3 1.363(10) . ? O2 Na1 2.641(6) 2_465 ? N3 C4 1.339(9) . ? C4 N4 1.325(10) . ? C4 C5 1.401(12) . ? C5 C6 1.348(12) . ? N11 C61 1.341(10) . ? N11 C21 1.359(9) . ? C21 O21 1.256(9) . ? C21 N31 1.351(10) . ? O21 Na2 2.435(6) 2_565 ? N31 C41 1.342(9) . ? C41 N41 1.332(10) . ? C41 C51 1.408(11) . ? C51 C61 1.346(11) . ? N12 C62 1.353(10) . ? N12 C22 1.379(9) . ? C22 O22 1.253(9) . ? C22 N32 1.331(10) . ? O22 Na2 2.489(6) 2_565 ? N32 C42 1.355(10) . ? C42 N42 1.322(11) . ? C42 C52 1.421(11) . ? C52 C62 1.326(12) . ? Cl1 O4 1.381(8) . ? Cl1 O3 1.410(6) . ? Cl1 O6 1.422(6) . ? Cl1 O5 1.432(7) . ? O6 Na2 2.339(6) 1_545 ? Cl2 O10 1.407(8) . ? Cl2 O9 1.409(8) . ? Cl2 O8 1.421(7) . ? Cl2 O7 1.453(9) . ? Cl3 O13 1.400(7) . ? Cl3 O11 1.409(7) . ? Cl3 O12 1.421(6) . ? Cl3 O14 1.438(8) . ? 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 O3W Na1 O22 171.6(2) . . ? O3W Na1 O2W 90.6(2) . . ? O22 Na1 O2W 86.5(2) . . ? O3W Na1 O2 88.8(2) . . ? O22 Na1 O2 95.2(2) . . ? O2W Na1 O2 170.8(2) . . ? O3W Na1 O21 103.6(2) . . ? O22 Na1 O21 83.9(2) . . ? O2W Na1 O21 82.88(19) . . ? O2 Na1 O21 88.3(2) . . ? O3W Na1 O2 81.8(2) . 2_465 ? O22 Na1 O2 91.65(19) . 2_465 ? O2W Na1 O2 108.6(2) . 2_465 ? O2 Na1 O2 80.5(2) . 2_465 ? O21 Na1 O2 167.5(2) . 2_465 ? O6 Na2 O1W 95.5(2) 1_565 2_565 ? O6 Na2 O2W 94.9(2) 1_565 . ? O1W Na2 O2W 95.4(2) 2_565 . ? O6 Na2 O21 172.7(3) 1_565 2_565 ? O1W Na2 O21 85.70(19) 2_565 2_565 ? O2W Na2 O21 92.2(2) . 2_565 ? O6 Na2 O21 86.1(2) 1_565 . ? O1W Na2 O21 178.0(2) 2_565 . ? O2W Na2 O21 85.7(2) . . ? O21 Na2 O21 92.56(19) 2_565 . ? O6 Na2 O22 87.6(2) 1_565 2_565 ? O1W Na2 O22 86.8(2) 2_565 2_565 ? O2W Na2 O22 176.6(2) . 2_565 ? O21 Na2 O22 85.3(2) 2_565 2_565 ? O21 Na2 O22 92.0(2) . 2_565 ? O1W Na3 O3W 176.1(2) . 2_465 ? O1W Na3 O3 88.5(2) . . ? O3W Na3 O3 87.8(2) 2_465 . ? O1W Na3 O2 97.7(2) . . ? O3W Na3 O2 86.1(2) 2_465 . ? O3 Na3 O2 165.5(3) . . ? O1W Na3 O8 90.9(2) . . ? O3W Na3 O8 88.8(2) 2_465 . ? O3 Na3 O8 103.5(3) . . ? O2 Na3 O8 89.5(2) . . ? O1W Na3 O22 82.7(2) . . ? O3W Na3 O22 97.8(2) 2_465 . ? O3 Na3 O22 81.1(2) . . ? O2 Na3 O22 86.71(19) . . ? O8 Na3 O22 172.1(2) . . ? Na3 O1W Na2 101.7(2) . 2_565 ? Na1 O2W Na2 100.0(2) . . ? Na1 O3W Na3 101.5(2) . 2_465 ? C2 N1 C6 122.8(7) . . ? O2 C2 N1 119.5(7) . . ? O2 C2 N3 121.7(7) . . ? N1 C2 N3 118.8(7) . . ? C2 O2 Na1 119.4(5) . . ? C2 O2 Na3 131.3(5) . . ? Na1 O2 Na3 91.6(2) . . ? C2 O2 Na1 117.0(4) . 2_465 ? Na1 O2 Na1 99.5(2) . 2_465 ? Na3 O2 Na1 90.54(19) . 2_465 ? C4 N3 C2 119.4(7) . . ? N4 C4 N3 117.7(7) . . ? N4 C4 C5 120.6(7) . . ? N3 C4 C5 121.8(7) . . ? C6 C5 C4 118.0(8) . . ? C5 C6 N1 119.3(8) . . ? C61 N11 C21 124.0(7) . . ? O21 C21 N31 121.8(6) . . ? O21 C21 N11 120.1(7) . . ? N31 C21 N11 118.2(7) . . ? C21 O21 Na2 122.1(5) . 2_565 ? C21 O21 Na2 129.6(4) . . ? Na2 O21 Na2 87.44(19) 2_565 . ? C21 O21 Na1 122.9(5) . . ? Na2 O21 Na1 92.9(2) 2_565 . ? Na2 O21 Na1 91.38(19) . . ? C41 N31 C21 119.1(6) . . ? N41 C41 N31 117.0(7) . . ? N41 C41 C51 120.7(7) . . ? N31 C41 C51 122.3(7) . . ? C61 C51 C41 117.5(7) . . ? N11 C61 C51 118.9(7) . . ? C62 N12 C22 122.3(7) . . ? O22 C22 N32 122.6(6) . . ? O22 C22 N12 118.1(7) . . ? N32 C22 N12 119.2(7) . . ? C22 O22 Na1 121.7(5) . . ? C22 O22 Na2 120.3(5) . 2_565 ? Na1 O22 Na2 97.8(2) . 2_565 ? C22 O22 Na3 132.0(4) . . ? Na1 O22 Na3 86.50(19) . . ? Na2 O22 Na3 88.79(19) 2_565 . ? C22 N32 C42 119.3(6) . . ? N42 C42 N32 117.7(7) . . ? N42 C42 C52 121.0(8) . . ? N32 C42 C52 121.4(7) . . ? C62 C52 C42 118.2(8) . . ? C52 C62 N12 119.6(7) . . ? O4 Cl1 O3 110.4(5) . . ? O4 Cl1 O6 112.2(5) . . ? O3 Cl1 O6 109.8(4) . . ? O4 Cl1 O5 108.4(7) . . ? O3 Cl1 O5 109.1(4) . . ? O6 Cl1 O5 106.8(4) . . ? Cl1 O3 Na3 126.2(4) . . ? Cl1 O6 Na2 144.7(5) . 1_545 ? O10 Cl2 O9 113.8(6) . . ? O10 Cl2 O8 106.9(5) . . ? O9 Cl2 O8 112.7(5) . . ? O10 Cl2 O7 107.5(7) . . ? O9 Cl2 O7 108.2(5) . . ? O8 Cl2 O7 107.4(5) . . ? Cl2 O8 Na3 125.8(4) . . ? O13 Cl3 O11 110.4(5) . . ? O13 Cl3 O12 109.1(4) . . ? O11 Cl3 O12 109.7(4) . . ? O13 Cl3 O14 109.3(6) . . ? O11 Cl3 O14 109.3(5) . . ? O12 Cl3 O14 109.0(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W N31 0.94(3) 1.84(3) 2.746(8) 161(7) . O2W H3W N32 0.94(3) 1.92(3) 2.835(8) 163(6) . O2W H4W O13 0.95(3) 1.96(4) 2.902(8) 167(8) . O3W H6W N3 0.94(3) 1.87(3) 2.784(9) 164(7) . N1 H1 O8 0.86 2.26 3.100(9) 166 . N11 H11 O6 0.86 2.18 2.978(9) 155 1_565 N12 H12 O3 0.86 2.22 3.027(10) 156 . N41 H41A O10 0.86 2.05 2.896(10) 169 2_564 N42 H42B O11 0.86 2.22 3.042(10) 159 . _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 22.15 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.818 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.135 #==END