# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Berthold Kersting' _publ_contact_author_email B.KERSTING@UNI-LEIPZIG.DE _publ_section_title ; The first binucleating amino-thiophenolate macrocycles with pendant hydroxyethyl groups ; loop_ _publ_author_name 'Berthold Kersting' 'Mathias Gressenbuch' # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 721405' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H80 N6 O6 S2' _chemical_formula_weight 877.28 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.8791(12) _cell_length_b 10.6841(9) _cell_length_c 22.6377(14) _cell_angle_alpha 90.00 _cell_angle_beta 96.938(5) _cell_angle_gamma 90.00 _cell_volume 4772.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.164 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9525 _exptl_absorpt_correction_T_max 0.9680 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19591 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 29.30 _reflns_number_total 6413 _reflns_number_gt 4009 _reflns_threshold_expression >2sigma(I) _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^)+(0.0642P)^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 6413 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1258 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 _computing_data_collection 'STOE X-Area' _computing_cell_refinement 'STOE X-Area' _computing_data_reduction 'STOE X-Area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material ? 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 S1 S 0.55529(3) 0.24905(5) 0.17035(2) 0.04846(15) Uani 1 1 d . . . C1 C 0.54090(9) 0.41315(17) 0.16113(7) 0.0352(4) Uani 1 1 d . . . C2 C 0.48375(8) 0.45570(16) 0.12319(7) 0.0320(4) Uani 1 1 d . . . C3 C 0.47297(8) 0.58337(16) 0.11787(7) 0.0321(3) Uani 1 1 d . . . H3B H 0.4342 0.6126 0.0931 0.039 Uiso 1 1 calc R . . C4 C 0.51708(9) 0.67078(16) 0.14756(8) 0.0339(4) Uani 1 1 d . . . C5 C 0.57258(9) 0.62705(18) 0.18440(8) 0.0382(4) Uani 1 1 d . . . H5 H 0.6024 0.6855 0.2055 0.046 Uiso 1 1 calc R . . C6 C 0.58596(9) 0.49982(18) 0.19138(8) 0.0371(4) Uani 1 1 d . C . C7 C 0.50363(10) 0.81075(17) 0.13609(8) 0.0409(4) Uani 1 1 d . . . C8 C 0.43198(11) 0.8438(2) 0.14898(11) 0.0527(5) Uani 1 1 d . . . H8A H 0.4248 0.9342 0.1443 0.079 Uiso 1 1 calc R . . H8B H 0.4263 0.8193 0.1898 0.079 Uiso 1 1 calc R . . H8C H 0.3989 0.7991 0.1211 0.079 Uiso 1 1 calc R . . C9 C 0.50989(12) 0.8386(2) 0.07042(9) 0.0528(5) Uani 1 1 d . . . H9A H 0.4755 0.7909 0.0451 0.079 Uiso 1 1 calc R . . H9B H 0.5551 0.8145 0.0614 0.079 Uiso 1 1 calc R . . H9C H 0.5030 0.9283 0.0628 0.079 Uiso 1 1 calc R . . C10 C 0.55419(13) 0.8936(2) 0.17457(10) 0.0583(6) Uani 1 1 d . . . H10A H 0.6004 0.8706 0.1680 0.061(7) Uiso 1 1 calc R . . H10B H 0.5486 0.8816 0.2166 0.091 Uiso 1 1 calc R . . H10C H 0.5460 0.9815 0.1637 0.091 Uiso 1 1 calc R . . C11 C 0.64894(11) 0.4603(2) 0.23194(9) 0.0507(5) Uani 1 1 d . . . H11A H 0.6709 0.3894 0.2136 0.061 Uiso 1 1 calc R A 1 H11B H 0.6357 0.4316 0.2705 0.061 Uiso 1 1 calc R A 1 C12 C 0.74655(9) 0.5368(2) 0.29620(8) 0.0479(5) Uani 1 1 d . . . H12A H 0.7910 0.5784 0.2956 0.058 Uiso 1 1 calc R B 1 H12B H 0.7538 0.4451 0.2976 0.044(6) Uiso 1 1 calc R B 1 C13 C 0.71358(9) 0.57965(17) 0.35023(8) 0.0363(4) Uani 1 1 d . C . H13A H 0.7176 0.6719 0.3533 0.044 Uiso 1 1 calc R . . H13B H 0.6647 0.5591 0.3433 0.044 Uiso 1 1 calc R . . C14 C 0.72668(9) 0.38979(16) 0.41033(8) 0.0355(4) Uani 1 1 d . C . H14A H 0.7697 0.3424 0.4173 0.043 Uiso 1 1 calc R . . H14B H 0.7025 0.3622 0.3717 0.043 Uiso 1 1 calc R . . C15 C 0.68373(9) 0.36056(16) 0.45942(8) 0.0378(4) Uani 1 1 d . . . H15A H 0.6744 0.2696 0.4600 0.045 Uiso 1 1 calc R . . H15B H 0.7087 0.3839 0.4984 0.045 Uiso 1 1 calc R . . C16 C 0.56531(9) 0.36595(17) 0.41272(8) 0.0377(4) Uani 1 1 d . . . H16C H 0.5396 0.3134 0.4382 0.045 Uiso 1 1 calc R . . H16D H 0.5855 0.3097 0.3849 0.045 Uiso 1 1 calc R . . N1A N 0.70050(18) 0.5710(3) 0.24297(16) 0.0298(7) Uani 0.686(5) 1 d P C 1 C17A C 0.73429(14) 0.6069(2) 0.19136(11) 0.0332(7) Uani 0.686(5) 1 d P C 1 H17A H 0.7598 0.6851 0.2014 0.040 Uiso 0.686(5) 1 calc PR C 1 H17B H 0.6988 0.6264 0.1581 0.040 Uiso 0.686(5) 1 calc PR C 1 C18A C 0.78214(18) 0.5138(3) 0.16932(13) 0.0454(9) Uani 0.686(5) 1 d P C 1 H18A H 0.8179 0.4881 0.2013 0.054 Uiso 0.686(5) 1 calc PR C 1 H18B H 0.7579 0.4386 0.1524 0.054 Uiso 0.686(5) 1 calc PR C 1 O1A O 0.8099(6) 0.5866(10) 0.1236(4) 0.088(3) Uani 0.686(5) 1 d P C 1 N1B N 0.7010(4) 0.5187(7) 0.2374(3) 0.0304(15) Uani 0.314(5) 1 d P C 2 C17B C 0.7385(3) 0.5020(5) 0.1864(3) 0.0356(17) Uani 0.314(5) 1 d P C 2 H17C H 0.7060 0.4838 0.1507 0.043 Uiso 0.314(5) 1 calc PR C 2 H17D H 0.7688 0.4286 0.1937 0.043 Uiso 0.314(5) 1 calc PR C 2 C18B C 0.7795(5) 0.6117(8) 0.1740(4) 0.062(2) Uani 0.314(5) 1 d P C 2 H18C H 0.8127 0.6315 0.2089 0.074 Uiso 0.314(5) 1 calc PR C 2 H18D H 0.7500 0.6855 0.1647 0.074 Uiso 0.314(5) 1 calc PR C 2 O1B O 0.8155(9) 0.5775(15) 0.1213(6) 0.044(3) Uani 0.314(5) 1 d P C 2 C19 C 0.81418(9) 0.55500(17) 0.42083(8) 0.0368(4) Uani 1 1 d . C . H19A H 0.8203 0.6459 0.4150 0.044 Uiso 1 1 calc R . . H19B H 0.8395 0.5105 0.3921 0.044 Uiso 1 1 calc R . . C20 C 0.84452(10) 0.52087(19) 0.48323(8) 0.0422(4) Uani 1 1 d . . . H20A H 0.8413 0.4291 0.4884 0.051 Uiso 1 1 calc R . . H20B H 0.8932 0.5436 0.4884 0.051 Uiso 1 1 calc R . . C21 C 0.59926(10) 0.4837(2) 0.50477(8) 0.0424(4) Uani 1 1 d . . . H21A H 0.5987 0.4173 0.5352 0.051 Uiso 1 1 calc R . . H21B H 0.5528 0.5177 0.4963 0.051 Uiso 1 1 calc R . . C22 C 0.64694(10) 0.5872(2) 0.52898(8) 0.0453(4) Uani 1 1 d . . . H22A H 0.6253 0.6365 0.5586 0.054 Uiso 1 1 calc R . . H22B H 0.6889 0.5497 0.5496 0.054 Uiso 1 1 calc R . . C23 C 0.53752(11) 0.22828(18) 0.24743(9) 0.0483(5) Uani 1 1 d . . . H23A H 0.5574 0.1481 0.2630 0.058 Uiso 1 1 calc R . . H23B H 0.5595 0.2966 0.2722 0.058 Uiso 1 1 calc R . . N2 N 0.74191(7) 0.52500(13) 0.40725(6) 0.0304(3) Uani 1 1 d . . . N3 N 0.61975(7) 0.42936(13) 0.45025(6) 0.0342(3) Uani 1 1 d . . . O2 O 0.81223(7) 0.58118(14) 0.52795(6) 0.0468(3) Uani 1 1 d . . . O3 O 0.66395(7) 0.66845(12) 0.48314(6) 0.0417(3) Uani 1 1 d . . . H1 H 0.8113(18) 0.521(3) 0.0934(17) 0.102(12) Uiso 1 1 d . . . H2 H 0.8160(15) 0.673(3) 0.5242(13) 0.088(9) Uiso 1 1 d . . . H3 H 0.6886(13) 0.621(2) 0.4591(12) 0.069(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 S1 0.0611(3) 0.0493(3) 0.0343(2) -0.0041(2) 0.0032(2) 0.0254(2) C1 0.0343(9) 0.0451(9) 0.0271(8) -0.0005(7) 0.0067(7) 0.0087(7) C2 0.0283(8) 0.0423(9) 0.0257(8) -0.0023(7) 0.0046(7) 0.0018(7) C3 0.0256(8) 0.0429(9) 0.0273(8) 0.0033(7) 0.0008(6) 0.0005(7) C4 0.0290(8) 0.0439(9) 0.0290(8) 0.0060(7) 0.0039(7) -0.0039(7) C5 0.0294(9) 0.0545(11) 0.0297(9) 0.0022(7) -0.0007(7) -0.0085(8) C6 0.0282(8) 0.0576(11) 0.0249(8) 0.0022(7) 0.0008(7) 0.0047(8) C7 0.0417(10) 0.0426(10) 0.0364(10) 0.0058(8) -0.0037(8) -0.0091(8) C8 0.0531(13) 0.0456(11) 0.0583(13) -0.0068(10) 0.0024(11) 0.0011(9) C9 0.0631(14) 0.0508(11) 0.0424(11) 0.0130(9) -0.0014(10) -0.0087(10) C10 0.0631(15) 0.0562(12) 0.0507(13) 0.0067(10) -0.0126(11) -0.0250(11) C11 0.0408(11) 0.0709(14) 0.0376(10) -0.0016(10) -0.0075(8) 0.0137(10) C12 0.0268(9) 0.0895(16) 0.0268(9) 0.0057(9) 0.0005(7) 0.0034(9) C13 0.0304(8) 0.0449(9) 0.0333(9) 0.0064(7) 0.0024(7) 0.0031(7) C14 0.0381(10) 0.0357(8) 0.0316(9) -0.0024(7) -0.0001(7) 0.0052(7) C15 0.0402(10) 0.0370(9) 0.0342(9) 0.0079(7) -0.0041(8) 0.0000(7) C16 0.0389(10) 0.0385(9) 0.0347(9) 0.0059(7) -0.0001(8) -0.0070(7) N1A 0.0259(12) 0.0372(17) 0.0258(13) 0.0013(14) 0.0010(9) -0.0052(14) C17A 0.0356(15) 0.0372(14) 0.0264(12) 0.0038(10) 0.0026(11) 0.0010(10) C18A 0.057(2) 0.0483(19) 0.0321(14) 0.0031(12) 0.0108(14) 0.0092(14) O1A 0.099(5) 0.108(5) 0.067(4) -0.002(3) 0.048(3) 0.008(4) N1B 0.024(3) 0.040(4) 0.023(3) 0.000(3) -0.0086(19) -0.007(3) C17B 0.037(3) 0.041(3) 0.028(3) -0.001(2) 0.002(3) 0.001(2) C18B 0.080(6) 0.052(5) 0.058(5) -0.009(3) 0.030(4) -0.015(4) O1B 0.057(5) 0.053(5) 0.025(4) 0.011(4) 0.023(4) 0.011(4) C19 0.0304(8) 0.0477(10) 0.0322(9) -0.0053(7) 0.0036(7) 0.0008(7) C20 0.0414(10) 0.0470(10) 0.0363(10) -0.0063(8) -0.0025(8) 0.0050(8) C21 0.0371(10) 0.0604(11) 0.0309(9) 0.0048(8) 0.0098(8) -0.0072(8) C22 0.0410(10) 0.0637(12) 0.0319(9) -0.0053(9) 0.0072(8) -0.0031(9) C23 0.0663(13) 0.0411(10) 0.0367(10) 0.0035(8) 0.0026(10) 0.0164(9) N2 0.0296(7) 0.0343(7) 0.0271(7) 0.0003(5) 0.0023(6) 0.0015(6) N3 0.0315(7) 0.0421(8) 0.0283(7) 0.0058(6) 0.0003(6) -0.0019(6) O2 0.0557(9) 0.0517(8) 0.0321(7) -0.0056(6) 0.0015(6) 0.0049(7) O3 0.0404(7) 0.0450(7) 0.0408(7) -0.0078(6) 0.0099(6) -0.0010(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 S1 C1 1.7847(18) . ? S1 C23 1.835(2) . ? C1 C6 1.407(3) . ? C1 C2 1.414(2) . ? C2 C3 1.384(2) . ? C2 C16 1.530(2) 2_655 ? C3 C4 1.397(2) . ? C4 C5 1.381(3) . ? C4 C7 1.536(3) . ? C5 C6 1.390(3) . ? C6 C11 1.520(3) . ? C7 C8 1.529(3) . ? C7 C10 1.530(3) . ? C7 C9 1.536(3) . ? C11 N1B 1.202(8) . ? C11 N1A 1.565(4) . ? C12 N1A 1.469(4) . ? C12 C13 1.526(3) . ? C12 N1B 1.529(8) . ? C13 N2 1.466(2) . ? C14 N2 1.479(2) . ? C14 C15 1.514(2) . ? C15 N3 1.462(2) . ? C16 N3 1.459(2) . ? C16 C2 1.530(2) 2_655 ? N1A C17A 1.467(4) . ? C17A C18A 1.503(4) . ? C18A O1A 1.457(10) . ? N1B C17B 1.461(10) . ? C17B C18B 1.472(10) . ? C18B O1B 1.510(19) . ? C19 N2 1.468(2) . ? C19 C20 1.512(3) . ? C20 O2 1.418(2) . ? C21 N3 1.465(2) . ? C21 C22 1.516(3) . ? C22 O3 1.424(2) . ? C23 C23 1.510(4) 2_655 ? 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 C1 S1 C23 100.57(8) . . ? C6 C1 C2 120.10(16) . . ? C6 C1 S1 120.40(14) . . ? C2 C1 S1 119.50(14) . . ? C3 C2 C1 118.32(16) . . ? C3 C2 C16 119.31(15) . 2_655 ? C1 C2 C16 122.36(15) . 2_655 ? C2 C3 C4 122.39(16) . . ? C5 C4 C3 118.26(16) . . ? C5 C4 C7 122.78(16) . . ? C3 C4 C7 118.91(16) . . ? C4 C5 C6 121.81(17) . . ? C5 C6 C1 119.10(16) . . ? C5 C6 C11 118.20(17) . . ? C1 C6 C11 122.71(18) . . ? C8 C7 C10 108.71(18) . . ? C8 C7 C9 109.03(18) . . ? C10 C7 C9 108.33(16) . . ? C8 C7 C4 109.86(15) . . ? C10 C7 C4 112.21(17) . . ? C9 C7 C4 108.64(16) . . ? N1B C11 C6 123.6(4) . . ? N1B C11 N1A 18.5(4) . . ? C6 C11 N1A 111.2(2) . . ? N1A C12 C13 107.31(19) . . ? N1A C12 N1B 21.9(2) . . ? C13 C12 N1B 117.9(3) . . ? N2 C13 C12 115.45(15) . . ? N2 C14 C15 111.90(14) . . ? N3 C15 C14 110.49(14) . . ? N3 C16 C2 113.50(14) . 2_655 ? C17A N1A C12 114.7(3) . . ? C17A N1A C11 115.1(3) . . ? C12 N1A C11 105.9(2) . . ? N1A C17A C18A 117.4(2) . . ? O1A C18A C17A 101.1(5) . . ? C11 N1B C17B 111.7(6) . . ? C11 N1B C12 124.6(6) . . ? C17B N1B C12 113.5(6) . . ? N1B C17B C18B 113.6(6) . . ? C17B C18B O1B 106.5(8) . . ? N2 C19 C20 114.39(15) . . ? O2 C20 C19 113.19(15) . . ? N3 C21 C22 111.60(14) . . ? O3 C22 C21 111.99(15) . . ? C23 C23 S1 112.25(19) 2_655 . ? C13 N2 C19 111.08(13) . . ? C13 N2 C14 111.81(14) . . ? C19 N2 C14 113.83(14) . . ? C16 N3 C15 114.86(14) . . ? C16 N3 C21 114.34(14) . . ? C15 N3 C21 113.89(14) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 29.30 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.348 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.042 #===END # Attachment '6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 721406' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H76 N6 O4 S2' _chemical_formula_weight 817.23 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.449(2) _cell_length_b 19.417(3) _cell_length_c 18.976(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.98(2) _cell_angle_gamma 90.00 _cell_volume 4584.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.163 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9528 _exptl_absorpt_correction_T_max 0.9682 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19229 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 29.29 _reflns_number_total 6174 _reflns_number_gt 4497 _reflns_threshold_expression >2sigma(I) _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^)+(0.0727P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6174 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _computing_data_collection 'STOE X-Area' _computing_cell_refinement 'STOE X-Area' _computing_data_reduction 'STOE X-Area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material ? 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 S1 S 0.63330(3) 0.046849(18) 0.674985(19) 0.02433(10) Uani 1 1 d . . . O1 O 0.51252(12) -0.24678(9) 0.44138(9) 0.0610(4) Uani 1 1 d . . . H1 H 0.5180 -0.2870 0.4256 0.091 Uiso 1 1 calc R . . O2 O 0.00056(10) -0.11048(8) 0.57909(8) 0.0498(4) Uani 1 1 d . . . H2 H 0.0671 -0.1086 0.5735 0.075 Uiso 1 1 calc R . . N1 N 0.50486(10) -0.14195(7) 0.55986(6) 0.0263(3) Uani 1 1 d . . . N2 N 0.20741(10) -0.10427(7) 0.52638(6) 0.0275(3) Uani 1 1 d . . . N3 N 0.15176(10) -0.01293(7) 0.64121(6) 0.0252(3) Uani 1 1 d . . . C1 C 0.66596(11) -0.03976(7) 0.69878(7) 0.0205(3) Uani 1 1 d . . . C2 C 0.74608(11) -0.05291(7) 0.75075(7) 0.0207(3) Uani 1 1 d . . . C4 C 0.72184(11) -0.17629(7) 0.73408(7) 0.0211(3) Uani 1 1 d . . . C3 C 0.77313(11) -0.12097(7) 0.76645(7) 0.0216(3) Uani 1 1 d . . . H3 H 0.8289 -0.1297 0.8007 0.026 Uiso 1 1 calc R . . C5 C 0.64124(12) -0.16203(7) 0.68289(7) 0.0245(3) Uani 1 1 d . . . H5 H 0.6037 -0.1993 0.6609 0.029 Uiso 1 1 calc R . . C6 C 0.61450(12) -0.09518(8) 0.66327(7) 0.0241(3) Uani 1 1 d . . . C7 C 0.75079(12) -0.25120(7) 0.75172(8) 0.0242(3) Uani 1 1 d . . . C8 C 0.65232(14) -0.28757(9) 0.78069(10) 0.0357(4) Uani 1 1 d . . . H8A H 0.6719 -0.3346 0.7949 0.054 Uiso 1 1 calc R . . H8B H 0.5949 -0.2892 0.7441 0.054 Uiso 1 1 calc R . . H8C H 0.6273 -0.2622 0.8216 0.054 Uiso 1 1 calc R . . C9 C 0.84373(13) -0.25651(9) 0.80641(9) 0.0336(3) Uani 1 1 d . . . H9A H 0.8602 -0.3051 0.8155 0.050 Uiso 1 1 calc R . . H9B H 0.8232 -0.2343 0.8503 0.050 Uiso 1 1 calc R . . H9C H 0.9073 -0.2335 0.7884 0.050 Uiso 1 1 calc R . . C10 C 0.78409(16) -0.28819(9) 0.68442(9) 0.0388(4) Uani 1 1 d . . . H10A H 0.8470 -0.2652 0.6655 0.058 Uiso 1 1 calc R . . H10B H 0.7246 -0.2868 0.6493 0.058 Uiso 1 1 calc R . . H10C H 0.8020 -0.3362 0.6955 0.058 Uiso 1 1 calc R . . C11 C 0.53278(15) -0.08212(9) 0.60373(9) 0.0361(4) Uani 1 1 d . . . H11A H 0.4662 -0.0643 0.6242 0.043 Uiso 1 1 calc R . . H11B H 0.5611 -0.0456 0.5730 0.043 Uiso 1 1 calc R . . C12 C 0.59446(13) -0.16133(11) 0.51527(9) 0.0376(4) Uani 1 1 d . . . H12A H 0.6630 -0.1517 0.5414 0.045 Uiso 1 1 calc R . . H12B H 0.5920 -0.1320 0.4725 0.045 Uiso 1 1 calc R . . C13 C 0.59322(16) -0.23531(12) 0.49309(10) 0.0487(5) Uani 1 1 d . . . H13A H 0.6639 -0.2477 0.4743 0.058 Uiso 1 1 calc R . . H13B H 0.5806 -0.2649 0.5345 0.058 Uiso 1 1 calc R . . C14 C 0.40811(12) -0.12580(9) 0.51628(7) 0.0280(3) Uani 1 1 d . . . H14A H 0.4042 -0.1569 0.4750 0.034 Uiso 1 1 calc R . . H14B H 0.4129 -0.0779 0.4987 0.034 Uiso 1 1 calc R . . C15 C 0.30641(12) -0.13385(8) 0.55826(7) 0.0269(3) Uani 1 1 d . . . H15A H 0.2942 -0.1836 0.5661 0.032 Uiso 1 1 calc R . . H15B H 0.3194 -0.1123 0.6051 0.032 Uiso 1 1 calc R . . C16 C 0.17749(13) -0.13767(11) 0.45910(8) 0.0373(4) Uani 1 1 d . . . H16A H 0.2322 -0.1278 0.4246 0.056 Uiso 1 1 calc R . . H16B H 0.1078 -0.1200 0.4417 0.056 Uiso 1 1 calc R . . H16C H 0.1725 -0.1876 0.4661 0.056 Uiso 1 1 calc R . . C17 C 0.20963(13) -0.02904(9) 0.51831(8) 0.0308(3) Uani 1 1 d . . . H17A H 0.1412 -0.0138 0.4951 0.037 Uiso 1 1 calc R . . H17B H 0.2686 -0.0165 0.4870 0.037 Uiso 1 1 calc R . . C18 C 0.22550(12) 0.00914(8) 0.58787(8) 0.0295(3) Uani 1 1 d . . . H18A H 0.3002 0.0019 0.6060 0.035 Uiso 1 1 calc R . . H18B H 0.2157 0.0591 0.5794 0.035 Uiso 1 1 calc R . . C19 C 0.03864(12) 0.00325(9) 0.62551(9) 0.0326(3) Uani 1 1 d . . . H19A H 0.0306 0.0229 0.5775 0.039 Uiso 1 1 calc R . . H19B H 0.0136 0.0379 0.6594 0.039 Uiso 1 1 calc R . . C20 C -0.02867(13) -0.06113(10) 0.63029(9) 0.0394(4) Uani 1 1 d . . . H20A H -0.0189 -0.0813 0.6780 0.047 Uiso 1 1 calc R . . H20B H -0.1055 -0.0491 0.6230 0.047 Uiso 1 1 calc R . . C21 C 0.18910(13) 0.00439(8) 0.71315(8) 0.0284(3) Uani 1 1 d . . . H21A H 0.1260 0.0149 0.7416 0.034 Uiso 1 1 calc R . . H21B H 0.2340 0.0464 0.7117 0.034 Uiso 1 1 calc R . . C22 C 0.49951(12) 0.05634(8) 0.70990(8) 0.0275(3) Uani 1 1 d . . . H22A H 0.4675 0.1000 0.6923 0.033 Uiso 1 1 calc R . . H22B H 0.4534 0.0181 0.6921 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.02737(17) 0.01806(16) 0.02747(17) 0.00551(14) -0.00045(12) 0.00102(13) O1 0.0449(8) 0.0736(11) 0.0635(10) -0.0252(8) -0.0132(7) 0.0033(8) O2 0.0336(7) 0.0620(9) 0.0542(8) -0.0219(7) 0.0074(6) -0.0129(6) N1 0.0272(6) 0.0282(6) 0.0228(6) -0.0018(5) -0.0082(5) 0.0011(5) N2 0.0256(6) 0.0339(7) 0.0228(6) -0.0034(5) -0.0022(5) -0.0005(5) N3 0.0254(6) 0.0263(7) 0.0234(6) 0.0000(5) -0.0063(5) 0.0048(5) C1 0.0228(6) 0.0169(6) 0.0218(6) 0.0017(5) -0.0013(5) 0.0009(5) C2 0.0231(6) 0.0196(6) 0.0193(6) 0.0010(5) -0.0009(5) -0.0009(5) C4 0.0232(6) 0.0193(6) 0.0206(6) 0.0005(5) -0.0012(5) 0.0019(5) C3 0.0220(6) 0.0224(7) 0.0201(6) 0.0020(5) -0.0038(5) 0.0011(5) C5 0.0289(7) 0.0182(6) 0.0259(7) -0.0013(5) -0.0079(5) 0.0003(5) C6 0.0262(7) 0.0206(7) 0.0248(6) -0.0004(5) -0.0071(5) 0.0011(5) C7 0.0274(7) 0.0183(6) 0.0265(7) 0.0014(5) -0.0037(5) 0.0033(5) C8 0.0353(8) 0.0292(8) 0.0424(9) 0.0107(7) -0.0031(7) -0.0011(7) C9 0.0323(8) 0.0254(8) 0.0423(9) 0.0044(7) -0.0107(7) 0.0064(6) C10 0.0519(10) 0.0285(8) 0.0362(9) -0.0029(7) 0.0020(8) 0.0136(8) C11 0.0448(9) 0.0228(8) 0.0390(9) -0.0001(7) -0.0233(7) 0.0038(7) C12 0.0250(7) 0.0583(12) 0.0291(8) 0.0009(7) -0.0056(6) -0.0017(7) C13 0.0392(9) 0.0659(14) 0.0405(10) -0.0200(9) -0.0068(8) 0.0132(9) C14 0.0272(7) 0.0361(8) 0.0202(6) 0.0002(6) -0.0059(5) 0.0002(6) C15 0.0313(7) 0.0285(8) 0.0208(6) 0.0005(6) -0.0022(5) 0.0005(6) C16 0.0300(8) 0.0537(11) 0.0280(8) -0.0109(7) -0.0044(6) 0.0002(7) C17 0.0296(7) 0.0364(9) 0.0260(7) 0.0052(6) -0.0021(6) 0.0052(6) C18 0.0282(7) 0.0267(8) 0.0333(8) 0.0029(6) -0.0027(6) 0.0023(6) C19 0.0269(7) 0.0423(9) 0.0283(7) 0.0006(7) -0.0041(6) 0.0097(7) C20 0.0277(8) 0.0552(12) 0.0353(9) -0.0058(8) 0.0017(6) -0.0003(7) C21 0.0356(8) 0.0223(7) 0.0267(7) -0.0025(6) -0.0088(6) 0.0078(6) C22 0.0265(7) 0.0256(7) 0.0303(7) 0.0014(6) -0.0025(5) 0.0052(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 S1 C1 1.7846(14) . ? S1 C22 1.8230(16) . ? O1 C13 1.398(2) . ? O2 C20 1.421(2) . ? N1 C11 1.464(2) . ? N1 C14 1.4711(19) . ? N1 C12 1.472(2) . ? N2 C16 1.468(2) . ? N2 C17 1.469(2) . ? N2 C15 1.471(2) . ? N3 C18 1.454(2) . ? N3 C19 1.4634(19) . ? N3 C21 1.4657(19) . ? C1 C2 1.4017(19) . ? C1 C6 1.412(2) . ? C2 C3 1.3935(19) . ? C2 C21 1.523(2) 2_656 ? C4 C3 1.383(2) . ? C4 C5 1.3999(19) . ? C4 C7 1.5329(19) . ? C5 C6 1.388(2) . ? C6 C11 1.515(2) . ? C7 C9 1.531(2) . ? C7 C8 1.533(2) . ? C7 C10 1.535(2) . ? C12 C13 1.497(3) . ? C14 C15 1.527(2) . ? C17 C18 1.521(2) . ? C19 C20 1.509(3) . ? C21 C2 1.523(2) 2_656 ? C22 C22 1.521(3) 2_656 ? 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 C1 S1 C22 101.91(7) . . ? C11 N1 C14 108.91(12) . . ? C11 N1 C12 111.11(13) . . ? C14 N1 C12 110.69(12) . . ? C16 N2 C17 110.71(13) . . ? C16 N2 C15 111.65(13) . . ? C17 N2 C15 114.37(12) . . ? C18 N3 C19 114.91(12) . . ? C18 N3 C21 113.15(12) . . ? C19 N3 C21 114.36(12) . . ? C2 C1 C6 119.81(12) . . ? C2 C1 S1 120.00(10) . . ? C6 C1 S1 120.13(10) . . ? C3 C2 C1 118.95(12) . . ? C3 C2 C21 118.44(12) . 2_656 ? C1 C2 C21 122.45(12) . 2_656 ? C3 C4 C5 117.63(13) . . ? C3 C4 C7 122.59(12) . . ? C5 C4 C7 119.78(12) . . ? C4 C3 C2 122.50(13) . . ? C6 C5 C4 122.05(13) . . ? C5 C6 C1 118.97(13) . . ? C5 C6 C11 120.35(13) . . ? C1 C6 C11 120.67(13) . . ? C9 C7 C8 108.71(13) . . ? C9 C7 C4 112.24(12) . . ? C8 C7 C4 109.31(12) . . ? C9 C7 C10 108.24(13) . . ? C8 C7 C10 108.98(14) . . ? C4 C7 C10 109.30(12) . . ? N1 C11 C6 115.54(13) . . ? N1 C12 C13 113.98(15) . . ? O1 C13 C12 110.51(17) . . ? N1 C14 C15 111.25(12) . . ? N2 C15 C14 116.33(12) . . ? N2 C17 C18 113.36(12) . . ? N3 C18 C17 113.22(13) . . ? N3 C19 C20 110.02(14) . . ? O2 C20 C19 111.20(14) . . ? N3 C21 C2 113.41(12) . 2_656 ? C22 C22 S1 112.81(14) 2_656 . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 29.29 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.842 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.050 #===END # Attachment '7n.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 721407' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H176 N12 Na4 Ni2 O22 S4' _chemical_formula_weight 2188.10 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 12.049(2) _cell_length_b 17.177(2) _cell_length_c 17.654(2) _cell_angle_alpha 67.639(10) _cell_angle_beta 71.354(12) _cell_angle_gamma 71.855(12) _cell_volume 3125.7(8) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8970 _exptl_absorpt_correction_T_max 0.9363 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23060 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.1266 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.53 _reflns_number_total 10719 _reflns_number_gt 5665 _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^)+(0.0981P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10719 _refine_ls_number_parameters 615 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1135 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1951 _refine_ls_wR_factor_gt 0.1779 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.002 _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 Ni Ni 0.22611(5) 0.27448(4) 0.99056(4) 0.0392(2) Uani 1 1 d . . . Na1 Na 0.81504(17) 0.00833(13) 0.81089(11) 0.0472(5) Uani 1 1 d . . . Na2 Na 0.58940(19) -0.06604(14) 0.86106(12) 0.0512(5) Uani 1 1 d . . . S1 S 0.42684(11) 0.20936(8) 0.98810(8) 0.0431(3) Uani 1 1 d . . . S2 S 0.56607(13) 0.14002(9) 0.71249(8) 0.0501(4) Uani 1 1 d . . . O1 O 0.6895(3) -0.0410(2) 0.94560(19) 0.0430(9) Uani 1 1 d . . . H1 H 0.7295 -0.0874 0.9720 0.064 Uiso 1 1 calc R . . O2 O 0.9844(5) -0.0973(3) 0.8633(3) 0.0840(15) Uani 1 1 d . . . H2 H 0.9586 -0.1345 0.9077 0.126 Uiso 1 1 calc R . . O3 O 0.7822(4) -0.1251(2) 0.8024(2) 0.0576(11) Uani 1 1 d . . . H3 H 0.7924 -0.1768 0.8330 0.086 Uiso 1 1 calc R . . O4 O 0.3831(9) 0.2491(6) 0.5465(5) 0.173(3) Uani 1 1 d . . . H4 H 0.4217 0.2088 0.5808 0.260 Uiso 1 1 d R . . O5 O 0.1618(3) 0.1805(2) 0.9915(2) 0.0461(9) Uani 1 1 d . . . O6 O 0.1235(3) 0.2746(2) 1.1038(2) 0.0501(10) Uani 1 1 d . . . N1 N 0.7657(3) 0.1187(3) 0.8944(2) 0.0393(10) Uani 1 1 d . . . N2 N 0.9866(4) 0.0819(3) 0.7638(3) 0.0491(11) Uani 1 1 d . . . N3 N 0.9018(4) 0.0092(3) 0.6617(3) 0.0520(12) Uani 1 1 d . . . N4 N 0.4284(4) 0.3278(3) 0.6528(2) 0.0549(13) Uani 1 1 d . . . N5 N 0.2096(4) 0.3308(3) 0.8630(3) 0.0447(11) Uani 1 1 d . . . N6 N 0.2439(4) 0.3972(3) 0.9779(2) 0.0448(11) Uani 1 1 d . . . C1 C 0.5134(4) 0.2883(3) 0.9299(3) 0.0403(12) Uani 1 1 d . . . C2 C 0.6232(4) 0.2703(3) 0.8718(3) 0.0402(12) Uani 1 1 d . . . C3 C 0.6828(5) 0.3352(3) 0.8230(3) 0.0461(13) Uani 1 1 d . . . H3B H 0.7557 0.3225 0.7840 0.055 Uiso 1 1 calc R . . C4 C 0.6421(5) 0.4189(4) 0.8275(3) 0.0490(14) Uani 1 1 d . . . C5 C 0.5366(5) 0.4354(4) 0.8854(3) 0.0501(14) Uani 1 1 d . . . H5B H 0.5078 0.4916 0.8909 0.060 Uiso 1 1 calc R . . C6 C 0.4710(4) 0.3726(3) 0.9359(3) 0.0428(13) Uani 1 1 d . . . C7 C 0.6711(4) 0.1845(3) 0.8538(3) 0.0411(12) Uani 1 1 d . . . H7A H 0.6020 0.1576 0.8692 0.049 Uiso 1 1 calc R . . H7B H 0.7022 0.1973 0.7922 0.049 Uiso 1 1 calc R . . C8 C 0.7229(5) 0.0723(3) 0.9835(3) 0.0441(13) Uani 1 1 d . . . H8A H 0.6792 0.1146 1.0142 0.053 Uiso 1 1 calc R . . H8B H 0.7928 0.0365 1.0078 0.053 Uiso 1 1 calc R . . C9 C 0.6413(5) 0.0154(3) 0.9954(3) 0.0457(13) Uani 1 1 d . . . H9B H 0.6235 -0.0195 1.0554 0.055 Uiso 1 1 calc R . . H9C H 0.5645 0.0525 0.9815 0.055 Uiso 1 1 calc R . . C10 C 0.8743(5) 0.1492(4) 0.8794(3) 0.0471(13) Uani 1 1 d . . . H10B H 0.9245 0.1070 0.9185 0.056 Uiso 1 1 calc R . . H10C H 0.8514 0.2049 0.8909 0.056 Uiso 1 1 calc R . . C11 C 0.9474(5) 0.1608(4) 0.7881(3) 0.0512(14) Uani 1 1 d . . . H11A H 0.8981 0.2056 0.7497 0.061 Uiso 1 1 calc R . . H11B H 1.0191 0.1820 0.7804 0.061 Uiso 1 1 calc R . . C12 C 1.0852(5) 0.0194(4) 0.8023(4) 0.0589(16) Uani 1 1 d . . . H12A H 1.1276 0.0507 0.8170 0.071 Uiso 1 1 calc R . . H12B H 1.1435 -0.0075 0.7604 0.071 Uiso 1 1 calc R . . C13 C 1.0421(7) -0.0516(4) 0.8813(5) 0.079(2) Uani 1 1 d . . . H13A H 1.1116 -0.0910 0.9043 0.095 Uiso 1 1 calc R . . H13B H 0.9868 -0.0254 0.9246 0.095 Uiso 1 1 calc R . . C14 C 1.0184(5) 0.1044(4) 0.6718(3) 0.0587(16) Uani 1 1 d . . . H14A H 1.0988 0.1183 0.6507 0.070 Uiso 1 1 calc R . . H14B H 0.9605 0.1570 0.6487 0.070 Uiso 1 1 calc R . . C15 C 1.0200(5) 0.0343(4) 0.6382(3) 0.0592(16) Uani 1 1 d . . . H15A H 1.0461 0.0545 0.5760 0.071 Uiso 1 1 calc R . . H15B H 1.0804 -0.0176 0.6593 0.071 Uiso 1 1 calc R . . C16 C 0.9223(6) -0.0825(4) 0.6684(3) 0.0594(16) Uani 1 1 d . . . H16A H 0.9894 -0.1160 0.6964 0.071 Uiso 1 1 calc R . . H16B H 0.9468 -0.0874 0.6110 0.071 Uiso 1 1 calc R . . C17 C 0.8139(6) -0.1217(4) 0.7165(3) 0.0640(17) Uani 1 1 d . . . H17A H 0.7453 -0.0871 0.6903 0.077 Uiso 1 1 calc R . . H17B H 0.8315 -0.1808 0.7132 0.077 Uiso 1 1 calc R . . C18 C 0.8256(6) 0.0618(4) 0.5997(3) 0.0579(16) Uani 1 1 d . . . H18A H 0.7521 0.0389 0.6177 0.069 Uiso 1 1 calc R . . H18B H 0.8698 0.0534 0.5445 0.069 Uiso 1 1 calc R . . C19 C 0.7881(5) 0.1579(4) 0.5875(3) 0.0500(14) Uani 1 1 d . . . C20 C 0.6806(5) 0.1975(4) 0.6323(3) 0.0487(14) Uani 1 1 d . . . C21 C 0.6549(5) 0.2864(4) 0.6155(3) 0.0511(14) Uani 1 1 d . . . C22 C 0.7359(5) 0.3345(4) 0.5570(3) 0.0582(16) Uani 1 1 d . . . H22 H 0.7191 0.3948 0.5480 0.070 Uiso 1 1 calc R . . C23 C 0.8423(6) 0.2961(4) 0.5105(3) 0.0630(18) Uani 1 1 d . A . C24 C 0.8635(6) 0.2086(4) 0.5262(3) 0.0633(18) Uani 1 1 d . . . H24 H 0.9332 0.1819 0.4934 0.076 Uiso 1 1 calc R . . C25 C 0.5407(5) 0.3348(4) 0.6632(3) 0.0576(16) Uani 1 1 d . . . H25A H 0.5405 0.3120 0.7239 0.069 Uiso 1 1 calc R . . H25B H 0.5435 0.3965 0.6435 0.069 Uiso 1 1 calc R . . C26 C 0.4168(13) 0.3668(9) 0.5660(7) 0.173(3) Uani 1 1 d . . . H26A H 0.4957 0.3536 0.5279 0.208 Uiso 1 1 calc R . . H26B H 0.3914 0.4302 0.5530 0.208 Uiso 1 1 calc R . . C27 C 0.3269(14) 0.3340(9) 0.5509(8) 0.173(3) Uani 1 1 d . . . H27A H 0.2543 0.3328 0.5975 0.208 Uiso 1 1 calc R . . H27B H 0.3030 0.3716 0.4976 0.208 Uiso 1 1 calc R . . C28 C 0.3260(5) 0.3668(4) 0.7086(3) 0.0581(16) Uani 1 1 d . . . H28A H 0.2505 0.3669 0.6975 0.070 Uiso 1 1 calc R . . H28B H 0.3290 0.4274 0.6966 0.070 Uiso 1 1 calc R . . C29 C 0.3266(4) 0.3176(3) 0.8010(3) 0.0451(13) Uani 1 1 d . . . H29A H 0.3540 0.2553 0.8074 0.054 Uiso 1 1 calc R . . H29B H 0.3865 0.3343 0.8159 0.054 Uiso 1 1 calc R . . C30 C 0.1241(5) 0.2863(4) 0.8607(4) 0.0548(15) Uani 1 1 d . . . H30A H 0.1285 0.2929 0.8017 0.066 Uiso 1 1 calc R . . H30B H 0.0413 0.3124 0.8856 0.066 Uiso 1 1 calc R . . C31 C 0.1545(5) 0.1902(4) 0.9104(4) 0.0569(15) Uani 1 1 d . . . H31A H 0.0918 0.1619 0.9146 0.068 Uiso 1 1 calc R . . H31B H 0.2321 0.1622 0.8806 0.068 Uiso 1 1 calc R . . C32 C 0.1571(5) 0.4226(3) 0.8588(3) 0.0519(15) Uani 1 1 d . . . H32A H 0.0732 0.4284 0.8922 0.062 Uiso 1 1 calc R . . H32B H 0.1562 0.4583 0.7997 0.062 Uiso 1 1 calc R . . C33 C 0.2299(5) 0.4550(4) 0.8929(3) 0.0527(15) Uani 1 1 d . . . H33A H 0.3100 0.4577 0.8545 0.063 Uiso 1 1 calc R . . H33B H 0.1888 0.5139 0.8955 0.063 Uiso 1 1 calc R . . C34 C 0.1384(5) 0.4223(4) 1.0445(3) 0.0509(14) Uani 1 1 d . . . H34A H 0.0639 0.4417 1.0238 0.061 Uiso 1 1 calc R . . H34B H 0.1495 0.4706 1.0569 0.061 Uiso 1 1 calc R . . C35 C 0.1276(5) 0.3452(4) 1.1244(3) 0.0541(15) Uani 1 1 d . . . H35A H 0.1973 0.3304 1.1492 0.065 Uiso 1 1 calc R . . H35B H 0.0538 0.3597 1.1662 0.065 Uiso 1 1 calc R . . C36 C 0.3570(5) 0.3970(4) 0.9967(3) 0.0466(13) Uani 1 1 d . . . H36A H 0.3616 0.3564 1.0537 0.056 Uiso 1 1 calc R . . H36B H 0.3518 0.4553 0.9977 0.056 Uiso 1 1 calc R . . C37 C 0.7140(5) 0.4882(4) 0.7695(4) 0.0589(16) Uani 1 1 d . . . C38 C 0.6556(8) 0.5754(5) 0.7827(5) 0.100(3) Uani 1 1 d . . . H38A H 0.7095 0.6153 0.7498 0.150 Uiso 1 1 calc R . . H38B H 0.6395 0.5692 0.8425 0.150 Uiso 1 1 calc R . . H38C H 0.5799 0.5982 0.7642 0.150 Uiso 1 1 calc R . . C39 C 0.8397(7) 0.4620(6) 0.7882(6) 0.109(3) Uani 1 1 d . . . H39A H 0.8818 0.4065 0.7787 0.163 Uiso 1 1 calc R . . H39B H 0.8314 0.4568 0.8469 0.163 Uiso 1 1 calc R . . H39C H 0.8855 0.5060 0.7508 0.163 Uiso 1 1 calc R . . C40 C 0.7323(9) 0.4936(6) 0.6786(4) 0.109(3) Uani 1 1 d . . . H40A H 0.7786 0.4382 0.6705 0.163 Uiso 1 1 calc R . . H40B H 0.7759 0.5390 0.6414 0.163 Uiso 1 1 calc R . . H40C H 0.6541 0.5072 0.6653 0.163 Uiso 1 1 calc R . . C41 C 0.9338(6) 0.3502(4) 0.4482(4) 0.072(2) Uani 1 1 d D . . C42A C 0.8728(16) 0.4346(11) 0.3963(11) 0.135(7) Uani 0.542(17) 1 d PD A 1 H42A H 0.8131 0.4659 0.4334 0.203 Uiso 0.542(17) 1 calc PR A 1 H42B H 0.8329 0.4243 0.3616 0.203 Uiso 0.542(17) 1 calc PR A 1 H42C H 0.9324 0.4691 0.3597 0.203 Uiso 0.542(17) 1 calc PR A 1 C43A C 1.0331(15) 0.3023(11) 0.3936(11) 0.135(7) Uani 0.542(17) 1 d PD A 1 H43A H 0.9980 0.2788 0.3663 0.203 Uiso 0.542(17) 1 calc PR A 1 H43B H 1.0835 0.2550 0.4286 0.203 Uiso 0.542(17) 1 calc PR A 1 H43C H 1.0821 0.3420 0.3507 0.203 Uiso 0.542(17) 1 calc PR A 1 C44A C 0.9956(15) 0.3686(12) 0.5039(10) 0.135(7) Uani 0.542(17) 1 d PD A 1 H44A H 1.0676 0.3905 0.4686 0.203 Uiso 0.542(17) 1 calc PR A 1 H44B H 1.0183 0.3151 0.5480 0.203 Uiso 0.542(17) 1 calc PR A 1 H44C H 0.9396 0.4117 0.5298 0.203 Uiso 0.542(17) 1 calc PR A 1 C42B C 0.895(2) 0.4467(12) 0.4381(13) 0.129(5) Uani 0.458(17) 1 d PD A 2 H42D H 0.9358 0.4790 0.3825 0.193 Uiso 0.458(17) 1 calc PR A 2 H42E H 0.9165 0.4576 0.4817 0.193 Uiso 0.458(17) 1 calc PR A 2 H42F H 0.8081 0.4654 0.4436 0.193 Uiso 0.458(17) 1 calc PR A 2 C43B C 0.955(2) 0.3410(13) 0.3606(11) 0.129(5) Uani 0.46 1 d PD A 2 H43D H 0.8874 0.3231 0.3580 0.193 Uiso 0.458(17) 1 calc PR A 2 H43E H 1.0291 0.2975 0.3510 0.193 Uiso 0.458(17) 1 calc PR A 2 H43F H 0.9637 0.3965 0.3172 0.193 Uiso 0.458(17) 1 calc PR A 2 C44B C 1.0521(17) 0.3147(14) 0.4762(12) 0.129(5) Uani 0.46 1 d PD A 2 H44D H 1.1094 0.3507 0.4385 0.193 Uiso 0.458(17) 1 calc PR A 2 H44E H 1.0846 0.2554 0.4741 0.193 Uiso 0.458(17) 1 calc PR A 2 H44F H 1.0383 0.3151 0.5339 0.193 Uiso 0.458(17) 1 calc PR A 2 O7 O 0.6400(3) 0.0597(2) 0.7623(2) 0.0495(9) Uani 1 1 d . . . O8 O 0.5130(4) 0.1150(3) 0.6601(3) 0.0804(14) Uani 1 1 d . . . O9 O 0.4550(6) -0.0472(4) 0.7841(4) 0.1123(19) Uiso 1 1 d . . . H9 H 0.4721 -0.0004 0.7482 0.168 Uiso 1 1 d R . . C45 C 0.4208(13) -0.1073(9) 0.7626(9) 0.161(5) Uiso 1 1 d . . . H45A H 0.4215 -0.0855 0.7019 0.193 Uiso 1 1 calc R . . H45B H 0.3381 -0.1132 0.7946 0.193 Uiso 1 1 calc R . . C46 C 0.5010(13) -0.1898(9) 0.7813(8) 0.173(5) Uiso 1 1 d . . . H46A H 0.5730 -0.1898 0.7353 0.260 Uiso 1 1 calc R . . H46B H 0.4612 -0.2344 0.7876 0.260 Uiso 1 1 calc R . . H46C H 0.5239 -0.2016 0.8338 0.260 Uiso 1 1 calc R . . O10 O -0.0945(7) 0.3413(5) 1.0616(7) 0.162(4) Uani 1 1 d . . . H10 H -0.0482 0.3117 1.0942 0.244 Uiso 1 1 calc R . . C47 C -0.1692(10) 0.2944(7) 1.0671(10) 0.157(5) Uani 1 1 d . . . H47A H -0.1862 0.2568 1.1262 0.188 Uiso 1 1 calc R . . H47B H -0.1239 0.2559 1.0324 0.188 Uiso 1 1 calc R . . C48 C -0.2765(11) 0.3323(8) 1.0453(9) 0.167(5) Uani 1 1 d . . . H48A H -0.3312 0.3599 1.0870 0.250 Uiso 1 1 calc R . . H48B H -0.3109 0.2885 1.0435 0.250 Uiso 1 1 calc R . . H48C H -0.2647 0.3759 0.9898 0.250 Uiso 1 1 calc R . . O11A O 0.650(2) 0.3461(17) 0.3345(15) 0.152(8) Uiso 0.33 1 d P . . O11B O 0.665(2) 0.2465(17) 0.3746(15) 0.153(8) Uiso 0.33 1 d P . . O11C O 0.327(3) 0.099(2) 0.4848(18) 0.190(11) Uiso 0.33 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0359(3) 0.0320(4) 0.0402(3) -0.0090(3) -0.0025(2) -0.0038(3) Na1 0.0453(11) 0.0449(13) 0.0413(10) -0.0122(9) 0.0004(8) -0.0085(9) Na2 0.0556(12) 0.0447(13) 0.0465(11) -0.0097(9) -0.0049(9) -0.0147(10) S1 0.0356(6) 0.0318(7) 0.0475(7) -0.0044(5) -0.0023(5) -0.0056(5) S2 0.0530(8) 0.0467(9) 0.0426(7) -0.0067(6) -0.0097(6) -0.0106(6) O1 0.046(2) 0.033(2) 0.0421(18) -0.0096(15) -0.0050(15) -0.0054(15) O2 0.071(3) 0.069(4) 0.095(3) -0.005(3) -0.023(3) -0.015(3) O3 0.074(3) 0.039(2) 0.0413(19) -0.0114(16) 0.0016(18) -0.004(2) O4 0.231(7) 0.167(6) 0.140(4) -0.054(4) -0.129(5) 0.029(5) O5 0.0430(19) 0.042(2) 0.048(2) -0.0108(16) -0.0073(15) -0.0082(16) O6 0.051(2) 0.040(2) 0.0478(19) -0.0146(17) 0.0016(16) -0.0074(16) N1 0.035(2) 0.034(2) 0.043(2) -0.0103(18) -0.0025(17) -0.0080(17) N2 0.046(2) 0.041(3) 0.051(2) -0.016(2) 0.0011(19) -0.008(2) N3 0.058(3) 0.044(3) 0.042(2) -0.013(2) 0.002(2) -0.009(2) N4 0.060(3) 0.056(3) 0.036(2) -0.010(2) -0.014(2) 0.002(2) N5 0.042(2) 0.032(3) 0.052(2) -0.0090(19) -0.0099(19) -0.0022(18) N6 0.044(2) 0.035(3) 0.042(2) -0.0110(18) -0.0034(18) 0.0013(19) C1 0.040(3) 0.039(3) 0.037(2) -0.007(2) -0.009(2) -0.008(2) C2 0.040(3) 0.037(3) 0.037(2) -0.008(2) -0.007(2) -0.005(2) C3 0.044(3) 0.036(3) 0.047(3) -0.006(2) -0.001(2) -0.013(2) C4 0.044(3) 0.045(4) 0.050(3) -0.007(2) -0.006(2) -0.014(2) C5 0.056(3) 0.036(3) 0.054(3) -0.010(2) -0.011(3) -0.010(2) C6 0.041(3) 0.038(3) 0.043(3) -0.012(2) -0.005(2) -0.005(2) C7 0.037(3) 0.042(3) 0.038(2) -0.012(2) -0.001(2) -0.007(2) C8 0.044(3) 0.041(3) 0.041(3) -0.014(2) -0.006(2) -0.003(2) C9 0.042(3) 0.039(3) 0.045(3) -0.009(2) -0.003(2) -0.005(2) C10 0.045(3) 0.039(3) 0.059(3) -0.018(2) -0.011(2) -0.009(2) C11 0.040(3) 0.049(4) 0.059(3) -0.015(3) -0.003(2) -0.013(2) C12 0.042(3) 0.058(4) 0.068(4) -0.020(3) -0.008(3) -0.004(3) C13 0.085(5) 0.047(4) 0.114(6) -0.012(4) -0.061(4) -0.003(4) C14 0.057(3) 0.057(4) 0.050(3) -0.011(3) 0.004(3) -0.022(3) C15 0.062(4) 0.052(4) 0.049(3) -0.019(3) 0.011(3) -0.013(3) C16 0.071(4) 0.044(4) 0.048(3) -0.018(3) 0.005(3) -0.007(3) C17 0.085(4) 0.049(4) 0.048(3) -0.012(3) -0.006(3) -0.015(3) C18 0.069(4) 0.054(4) 0.039(3) -0.017(3) -0.002(3) -0.006(3) C19 0.062(3) 0.046(4) 0.033(3) -0.010(2) -0.004(2) -0.010(3) C20 0.059(3) 0.043(3) 0.033(2) -0.010(2) -0.006(2) -0.003(3) C21 0.056(3) 0.045(4) 0.038(3) -0.007(2) -0.003(2) -0.007(3) C22 0.068(4) 0.046(4) 0.037(3) -0.005(2) 0.004(3) -0.006(3) C23 0.065(4) 0.054(4) 0.041(3) -0.002(3) 0.003(3) -0.006(3) C24 0.068(4) 0.052(4) 0.044(3) -0.010(3) 0.009(3) -0.005(3) C25 0.064(4) 0.049(4) 0.043(3) -0.012(2) -0.002(3) -0.004(3) C26 0.231(7) 0.167(6) 0.140(4) -0.054(4) -0.129(5) 0.029(5) C27 0.231(7) 0.167(6) 0.140(4) -0.054(4) -0.129(5) 0.029(5) C28 0.053(3) 0.058(4) 0.045(3) -0.007(3) -0.013(2) 0.002(3) C29 0.041(3) 0.039(3) 0.043(3) -0.011(2) -0.006(2) 0.001(2) C30 0.052(3) 0.048(4) 0.062(3) -0.009(3) -0.022(3) -0.008(3) C31 0.055(3) 0.053(4) 0.062(4) -0.013(3) -0.018(3) -0.013(3) C32 0.050(3) 0.036(3) 0.055(3) -0.008(2) -0.012(2) 0.003(2) C33 0.054(3) 0.034(3) 0.052(3) -0.007(2) -0.003(2) -0.002(2) C34 0.043(3) 0.039(3) 0.058(3) -0.020(2) 0.002(2) 0.000(2) C35 0.051(3) 0.047(4) 0.048(3) -0.019(3) 0.007(2) -0.003(3) C36 0.053(3) 0.033(3) 0.051(3) -0.017(2) -0.005(2) -0.008(2) C37 0.063(4) 0.043(4) 0.062(3) -0.008(3) -0.002(3) -0.021(3) C38 0.122(7) 0.058(5) 0.107(6) -0.027(4) 0.015(5) -0.042(5) C39 0.078(5) 0.108(7) 0.131(7) 0.005(6) -0.028(5) -0.055(5) C40 0.165(9) 0.090(6) 0.063(4) -0.003(4) 0.009(5) -0.079(6) C41 0.071(4) 0.054(4) 0.059(4) -0.002(3) 0.012(3) -0.017(3) C42A 0.103(8) 0.096(8) 0.132(10) -0.006(7) 0.052(7) -0.039(6) C43A 0.103(8) 0.096(8) 0.132(10) -0.006(7) 0.052(7) -0.039(6) C44A 0.103(8) 0.096(8) 0.132(10) -0.006(7) 0.052(7) -0.039(6) C42B 0.117(10) 0.094(9) 0.124(10) -0.011(8) 0.045(8) -0.058(8) C43B 0.117(10) 0.094(9) 0.124(10) -0.011(8) 0.045(8) -0.058(8) C44B 0.117(10) 0.094(9) 0.124(10) -0.011(8) 0.045(8) -0.058(8) O7 0.050(2) 0.044(2) 0.0434(19) -0.0045(16) -0.0077(15) -0.0114(17) O8 0.091(3) 0.083(4) 0.080(3) -0.019(3) -0.040(3) -0.022(3) O10 0.096(5) 0.103(6) 0.314(12) -0.098(7) -0.071(6) 0.010(4) C47 0.091(7) 0.084(8) 0.288(16) -0.032(9) -0.066(9) -0.019(6) C48 0.133(10) 0.136(11) 0.224(14) -0.014(10) -0.067(10) -0.047(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 Ni O6 1.986(3) . ? Ni O5 1.989(4) . ? Ni N6 2.105(5) . ? Ni N5 2.135(4) . ? Ni S1 2.3210(14) . ? Na1 O7 2.320(4) . ? Na1 N3 2.500(5) . ? Na1 N2 2.508(5) . ? Na1 N1 2.643(5) . ? Na1 C13 3.088(7) . ? Na1 Na2 3.094(3) . ? Na2 O7 2.313(4) . ? Na2 S1 2.858(2) 2_657 ? S1 C1 1.765(5) . ? S1 Na2 2.858(2) 2_657 ? S2 O7 1.511(4) . ? S2 O8 1.516(5) . ? S2 C20 1.849(6) . ? O1 C9 1.422(6) . ? O2 C13 1.368(8) . ? O3 C17 1.423(7) . ? O4 C27 1.424(14) . ? O5 C31 1.405(7) . ? O6 C35 1.411(7) . ? N1 C10 1.468(7) . ? N1 C8 1.469(6) . ? N1 C7 1.481(6) . ? N2 C14 1.467(7) . ? N2 C11 1.470(7) . ? N2 C12 1.480(7) . ? N3 C16 1.480(8) . ? N3 C18 1.494(7) . ? N3 C15 1.501(8) . ? N4 C26 1.454(10) . ? N4 C28 1.467(7) . ? N4 C25 1.468(8) . ? N5 C30 1.480(7) . ? N5 C32 1.487(7) . ? N5 C29 1.497(6) . ? N6 C33 1.479(6) . ? N6 C36 1.501(7) . ? N6 C34 1.507(6) . ? C1 C6 1.412(7) . ? C1 C2 1.419(7) . ? C2 C3 1.368(7) . ? C2 C7 1.523(7) . ? C3 C4 1.392(8) . ? C4 C5 1.380(7) . ? C4 C37 1.538(8) . ? C5 C6 1.390(7) . ? C6 C36 1.502(7) . ? C8 C9 1.509(8) . ? C10 C11 1.539(7) . ? C12 C13 1.529(9) . ? C14 C15 1.525(9) . ? C16 C17 1.511(9) . ? C18 C19 1.517(8) . ? C19 C24 1.380(8) . ? C19 C20 1.404(7) . ? C20 C21 1.391(8) . ? C21 C22 1.383(8) . ? C21 C25 1.539(8) . ? C22 C23 1.402(8) . ? C23 C24 1.375(9) . ? C23 C41 1.540(8) . ? C26 C27 1.498(18) . ? C28 C29 1.526(7) . ? C30 C31 1.534(8) . ? C32 C33 1.529(9) . ? C34 C35 1.525(7) . ? C37 C38 1.515(10) . ? C37 C40 1.518(10) . ? C37 C39 1.545(10) . ? C41 C42A 1.498(16) . ? C41 C43A 1.513(15) . ? C41 C44B 1.525(18) . ? C41 C42B 1.532(19) . ? C41 C43B 1.546(18) . ? C41 C44A 1.572(16) . ? O9 C45 1.429(14) . ? C45 C46 1.430(17) . ? O10 C47 1.344(12) . ? C47 C48 1.359(14) . ? O11A O11B 1.56(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ni O5 91.78(15) . . ? O6 Ni N6 85.75(16) . . ? O5 Ni N6 161.96(15) . . ? O6 Ni N5 137.56(15) . . ? O5 Ni N5 85.03(16) . . ? N6 Ni N5 84.80(17) . . ? O6 Ni S1 114.82(11) . . ? O5 Ni S1 102.14(11) . . ? N6 Ni S1 95.08(12) . . ? N5 Ni S1 107.19(12) . . ? O7 Na1 N3 80.63(15) . . ? O7 Na1 N2 126.90(15) . . ? N3 Na1 N2 76.15(17) . . ? O7 Na1 N1 96.58(15) . . ? N3 Na1 N1 136.08(16) . . ? N2 Na1 N1 70.90(15) . . ? O7 Na1 C13 176.5(2) . . ? N3 Na1 C13 102.0(2) . . ? N2 Na1 C13 52.12(17) . . ? N1 Na1 C13 79.89(19) . . ? O7 Na1 Na2 48.01(10) . . ? N3 Na1 Na2 103.10(14) . . ? N2 Na1 Na2 174.69(13) . . ? N1 Na1 Na2 107.04(11) . . ? C13 Na1 Na2 132.84(15) . . ? O7 Na2 S1 160.41(14) . 2_657 ? O7 Na2 Na1 48.21(10) . . ? S1 Na2 Na1 114.76(8) 2_657 . ? C1 S1 Ni 108.69(17) . . ? C1 S1 Na2 140.13(17) . 2_657 ? Ni S1 Na2 101.72(6) . 2_657 ? O7 S2 O8 108.7(3) . . ? O7 S2 C20 103.2(2) . . ? O8 S2 C20 102.6(3) . . ? C31 O5 Ni 111.3(3) . . ? C35 O6 Ni 111.2(3) . . ? C10 N1 C8 112.4(4) . . ? C10 N1 C7 114.3(4) . . ? C8 N1 C7 114.5(4) . . ? C10 N1 Na1 109.1(3) . . ? C8 N1 Na1 106.5(3) . . ? C7 N1 Na1 98.8(3) . . ? C14 N2 C11 109.6(4) . . ? C14 N2 C12 112.2(4) . . ? C11 N2 C12 112.5(5) . . ? C14 N2 Na1 105.0(3) . . ? C11 N2 Na1 109.9(3) . . ? C12 N2 Na1 107.4(3) . . ? C16 N3 C18 108.0(5) . . ? C16 N3 C15 109.8(4) . . ? C18 N3 C15 113.2(4) . . ? C16 N3 Na1 102.9(3) . . ? C18 N3 Na1 117.4(3) . . ? C15 N3 Na1 104.9(3) . . ? C26 N4 C28 110.7(6) . . ? C26 N4 C25 112.3(7) . . ? C28 N4 C25 109.8(5) . . ? C30 N5 C32 113.5(4) . . ? C30 N5 C29 112.1(5) . . ? C32 N5 C29 113.7(4) . . ? C30 N5 Ni 102.4(3) . . ? C32 N5 Ni 101.1(3) . . ? C29 N5 Ni 113.0(3) . . ? C33 N6 C36 112.6(4) . . ? C33 N6 C34 110.8(4) . . ? C36 N6 C34 108.8(4) . . ? C33 N6 Ni 108.2(3) . . ? C36 N6 Ni 114.2(3) . . ? C34 N6 Ni 101.7(3) . . ? C6 C1 C2 118.3(5) . . ? C6 C1 S1 120.6(4) . . ? C2 C1 S1 121.0(4) . . ? C3 C2 C1 119.2(5) . . ? C3 C2 C7 117.6(4) . . ? C1 C2 C7 122.8(5) . . ? C2 C3 C4 123.4(5) . . ? C5 C4 C3 117.1(5) . . ? C5 C4 C37 122.9(5) . . ? C3 C4 C37 120.0(5) . . ? C4 C5 C6 122.2(5) . . ? C5 C6 C1 119.8(5) . . ? C5 C6 C36 118.2(5) . . ? C1 C6 C36 121.9(5) . . ? N1 C7 C2 119.8(4) . . ? N1 C8 C9 112.3(4) . . ? O1 C9 C8 114.1(4) . . ? N1 C10 C11 111.2(4) . . ? N2 C11 C10 114.2(4) . . ? N2 C12 C13 113.2(5) . . ? O2 C13 C12 110.7(6) . . ? O2 C13 Na1 49.6(3) . . ? C12 C13 Na1 82.9(3) . . ? N2 C14 C15 114.8(5) . . ? N3 C15 C14 114.7(5) . . ? N3 C16 C17 113.9(5) . . ? O3 C17 C16 111.4(6) . . ? N3 C18 C19 116.2(5) . . ? C24 C19 C20 119.0(6) . . ? C24 C19 C18 116.9(5) . . ? C20 C19 C18 124.1(5) . . ? C21 C20 C19 119.2(5) . . ? C21 C20 S2 116.2(4) . . ? C19 C20 S2 124.6(4) . . ? C22 C21 C20 120.2(5) . . ? C22 C21 C25 117.2(5) . . ? C20 C21 C25 122.6(5) . . ? C21 C22 C23 121.2(6) . . ? C24 C23 C22 117.3(5) . . ? C24 C23 C41 122.1(5) . . ? C22 C23 C41 120.4(6) . . ? C23 C24 C19 122.9(5) . . ? N4 C25 C21 114.3(5) . . ? N4 C26 C27 111.1(11) . . ? O4 C27 C26 106.8(11) . . ? N4 C28 C29 111.4(4) . . ? N5 C29 C28 116.2(4) . . ? N5 C30 C31 109.8(4) . . ? O5 C31 C30 110.0(5) . . ? N5 C32 C33 110.7(4) . . ? N6 C33 C32 110.7(5) . . ? N6 C34 C35 109.8(4) . . ? O6 C35 C34 108.8(5) . . ? N6 C36 C6 115.4(4) . . ? C38 C37 C40 111.3(6) . . ? C38 C37 C4 112.6(5) . . ? C40 C37 C4 109.3(6) . . ? C38 C37 C39 106.7(7) . . ? C40 C37 C39 107.1(7) . . ? C4 C37 C39 109.6(5) . . ? C42A C41 C43A 111.5(8) . . ? C42A C41 C44B 136.3(11) . . ? C43A C41 C44B 65.5(9) . . ? C42A C41 C42B 37.3(10) . . ? C43A C41 C42B 130.0(10) . . ? C44B C41 C42B 108.5(9) . . ? C42A C41 C23 111.2(9) . . ? C43A C41 C23 113.3(8) . . ? C44B C41 C23 109.1(8) . . ? C42B C41 C23 115.1(9) . . ? C42A C41 C43B 73.9(9) . . ? C43A C41 C43B 44.2(9) . . ? C44B C41 C43B 108.5(9) . . ? C42B C41 C43B 107.1(9) . . ? C23 C41 C43B 108.2(9) . . ? C42A C41 C44A 108.4(10) . . ? C43A C41 C44A 106.3(9) . . ? C44B C41 C44A 43.2(9) . . ? C42B C41 C44A 71.9(10) . . ? C23 C41 C44A 105.8(7) . . ? C43B C41 C44A 142.1(10) . . ? S2 O7 Na2 131.6(2) . . ? S2 O7 Na1 142.7(2) . . ? Na2 O7 Na1 83.78(13) . . ? O9 C45 C46 110.7(12) . . ? O10 C47 C48 121.6(10) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 25.53 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 1.013 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.094 #===END