# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_publication _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'A. K. Cheetham' _publ_contact_author_email cheetham@mrl.ucsb.edu _publ_section_title ; A thermally stable nanoporous nickel 5-sulfoisophthalate; crystal structure and adsorption properties ; loop_ _publ_author_name 'Anthony K. Cheetham' 'Dae Sung Kim' 'R.Le Toquin' P.M.Forster data_datat _database_code_depnum_ccdc_archive 'CCDC 241102' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H19 Na1 Ni3 O21 S2' _chemical_formula_weight 810.52 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' 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 9.833(2) _cell_length_b 11.107(2) _cell_length_c 12.615(3) _cell_angle_alpha 74.884(3) _cell_angle_beta 89.323(4) _cell_angle_gamma 69.755(3) _cell_volume 1243.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 200 _exptl_crystal_size_mid 180 _exptl_crystal_size_min 150 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 1.268 _exptl_absorpt_correction_type MULTISCAN _exptl_absorpt_correction_T_min 1.000000 _exptl_absorpt_correction_T_max 0.814177 _exptl_absorpt_process_details SADABS _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 'BRUKER SMART CCD' _diffrn_measurement_method '/F AND/W SCANS' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9959 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.30 _reflns_number_total 5513 _reflns_number_gt 4633 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.0' _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^)+(0.0530P)^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 5513 _refine_ls_number_parameters 415 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.83359(4) 0.32953(3) 0.70160(3) 0.00846(9) Uani 1 1 d . . . Ni2 Ni 0.62788(4) 0.35678(3) 0.51825(3) 0.00802(9) Uani 1 1 d . . . Ni3 Ni 0.70039(4) 0.11460(3) 0.78541(3) 0.00855(9) Uani 1 1 d . . . S1 S 0.72900(7) 0.46190(6) 0.27268(5) 0.01033(14) Uani 1 1 d . . . S2 S 0.39947(7) 0.04415(6) 0.81110(5) 0.00971(14) Uani 1 1 d . . . Na1 Na 0.44021(13) 0.24284(12) 0.97106(9) 0.0212(3) Uani 1 1 d . . . O1 O 1.08890(19) -0.12295(17) 0.24432(15) 0.0097(4) Uani 1 1 d . . . O2 O 0.9945(2) -0.07138(18) 0.39740(15) 0.0142(4) Uani 1 1 d . . . O3 O 0.8091(2) 0.34273(18) -0.14101(15) 0.0132(4) Uani 1 1 d . . . O4 O 0.6965(2) 0.19519(18) -0.08385(15) 0.0122(4) Uani 1 1 d . . . O5 O 0.6566(2) 0.58371(18) 0.18694(16) 0.0175(4) Uani 1 1 d . . . O6 O 0.8547(2) 0.46576(18) 0.33336(15) 0.0137(4) Uani 1 1 d . . . O7 O 0.6256(2) 0.42434(18) 0.34759(15) 0.0127(4) Uani 1 1 d . . . O8 O 0.3389(2) -0.17373(17) 0.49632(15) 0.0121(4) Uani 1 1 d . . . O9 O 0.2905(2) -0.01707(17) 0.33076(15) 0.0117(4) Uani 1 1 d . . . O10 O 0.2307(2) 0.46750(18) 0.35527(15) 0.0125(4) Uani 1 1 d . . . O11 O 0.40128(19) 0.44433(17) 0.48457(15) 0.0092(4) Uani 1 1 d . . . O12 O 0.4940(2) 0.11527(18) 0.83246(15) 0.0115(4) Uani 1 1 d . . . O13 O 0.4676(2) -0.09991(18) 0.84972(15) 0.0146(4) Uani 1 1 d . . . O14 O 0.2591(2) 0.09684(19) 0.85514(15) 0.0139(4) Uani 1 1 d . . . O1W O 1.0446(2) 0.31927(19) 0.71535(17) 0.0161(4) Uani 1 1 d D . . H1WA H 1.104(3) 0.258(3) 0.761(2) 0.019 Uiso 1 1 d D . . H1WB H 1.079(3) 0.376(3) 0.698(3) 0.019 Uiso 1 1 d D . . O2W O 0.8510(2) 0.31307(18) 0.53969(16) 0.0112(4) Uani 1 1 d D . . H2WA H 0.884(3) 0.352(3) 0.492(2) 0.013 Uiso 1 1 d D . . H2WB H 0.900(3) 0.2335(19) 0.549(3) 0.013 Uiso 1 1 d D . . O3W O 0.7889(2) -0.05872(19) 0.91029(17) 0.0148(4) Uani 1 1 d D . . H3WA H 0.796(4) -0.131(2) 0.906(3) 0.018 Uiso 1 1 d D . . H3WB H 0.766(4) -0.046(3) 0.9689(19) 0.018 Uiso 1 1 d D . . O4W O 0.1943(3) 0.3186(2) 1.0188(2) 0.0374(6) Uani 1 1 d . . . O5W O 0.4273(4) 0.3812(4) 1.1253(4) 0.0821(12) Uani 1 1 d . . . O6W O 0.0456(3) 0.4864(3) 1.1368(3) 0.0420(7) Uani 1 1 d D . . H6WA H 0.087(4) 0.543(4) 1.135(4) 0.050 Uiso 1 1 d D . . H6WB H 0.043(5) 0.447(4) 1.2041(19) 0.050 Uiso 1 1 d D . . O1H O 0.6390(2) 0.30381(17) 0.68288(15) 0.0090(4) Uani 1 1 d D . . H1OH H 0.574(3) 0.357(2) 0.700(3) 0.011 Uiso 1 1 d D . . C1 C 0.9246(3) 0.0969(3) 0.2280(2) 0.0098(5) Uani 1 1 d . . . C2 C 0.8884(3) 0.1191(3) 0.1162(2) 0.0106(5) Uani 1 1 d . . . H2 H 0.9171 0.0480 0.0850 0.013 Uiso 1 1 calc R . . C3 C 0.8091(3) 0.2477(3) 0.0508(2) 0.0101(5) Uani 1 1 d . . . C4 C 0.7662(3) 0.3554(2) 0.0971(2) 0.0109(5) Uani 1 1 d . . . H4 H 0.7173 0.4418 0.0536 0.013 Uiso 1 1 calc R . . C5 C 0.7984(3) 0.3302(2) 0.2099(2) 0.0105(5) Uani 1 1 d . . . C6 C 0.8755(3) 0.2027(3) 0.2763(2) 0.0112(5) Uani 1 1 d . . . H6 H 0.8943 0.1879 0.3516 0.013 Uiso 1 1 calc R . . C7 C 1.0081(3) -0.0415(3) 0.2965(2) 0.0111(5) Uani 1 1 d . . . C8 C 0.7680(3) 0.2644(3) -0.0674(2) 0.0104(5) Uani 1 1 d . . . C9 C 0.3177(3) 0.0444(3) 0.4955(2) 0.0101(5) Uani 1 1 d . . . C10 C 0.3032(3) 0.1750(2) 0.4374(2) 0.0098(5) Uani 1 1 d . . . H10 H 0.2791 0.2047 0.3616 0.012 Uiso 1 1 calc R . . C11 C 0.3251(3) 0.2603(2) 0.4943(2) 0.0092(5) Uani 1 1 d . . . C12 C 0.3564(3) 0.2176(2) 0.6083(2) 0.0100(5) Uani 1 1 d . . . H12 H 0.3713 0.2744 0.6459 0.012 Uiso 1 1 calc R . . C13 C 0.3653(3) 0.0890(3) 0.6658(2) 0.0098(5) Uani 1 1 d . . . C14 C 0.3477(3) 0.0018(2) 0.6098(2) 0.0095(5) Uani 1 1 d . . . H14 H 0.3559 -0.0844 0.6484 0.011 Uiso 1 1 calc R . . C15 C 0.3134(3) -0.0568(3) 0.4348(2) 0.0104(5) Uani 1 1 d . . . C16 C 0.3184(3) 0.4005(2) 0.4382(2) 0.0096(5) 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 Ni1 0.00985(17) 0.00735(16) 0.00738(17) -0.00074(12) -0.00092(12) -0.00297(13) Ni2 0.00984(17) 0.00637(16) 0.00711(17) -0.00130(12) -0.00074(12) -0.00233(12) Ni3 0.01066(17) 0.00773(16) 0.00727(17) -0.00172(13) -0.00001(12) -0.00349(13) S1 0.0147(3) 0.0073(3) 0.0076(3) -0.0019(2) 0.0007(2) -0.0023(2) S2 0.0111(3) 0.0092(3) 0.0083(3) -0.0011(2) -0.0005(2) -0.0040(2) Na1 0.0232(6) 0.0215(6) 0.0134(6) 0.0033(5) -0.0020(5) -0.0072(5) O1 0.0083(9) 0.0089(8) 0.0110(9) -0.0026(7) 0.0012(7) -0.0018(7) O2 0.0163(10) 0.0111(9) 0.0105(9) -0.0012(8) 0.0001(8) -0.0002(8) O3 0.0208(10) 0.0117(9) 0.0087(9) -0.0018(7) 0.0015(8) -0.0084(8) O4 0.0148(10) 0.0137(9) 0.0104(9) -0.0046(8) 0.0007(7) -0.0068(8) O5 0.0269(11) 0.0094(9) 0.0099(10) -0.0009(8) -0.0011(8) 0.0000(8) O6 0.0188(10) 0.0140(9) 0.0105(9) -0.0035(8) 0.0018(8) -0.0085(8) O7 0.0131(9) 0.0143(9) 0.0095(9) -0.0033(8) 0.0006(7) -0.0033(8) O8 0.0171(10) 0.0087(9) 0.0113(9) -0.0030(7) 0.0006(8) -0.0052(8) O9 0.0153(10) 0.0099(9) 0.0101(9) -0.0035(7) 0.0002(7) -0.0043(8) O10 0.0171(10) 0.0094(9) 0.0098(9) 0.0003(7) -0.0043(8) -0.0052(8) O11 0.0109(9) 0.0075(8) 0.0095(9) -0.0027(7) 0.0009(7) -0.0032(7) O12 0.0132(9) 0.0127(9) 0.0097(9) -0.0035(7) -0.0007(7) -0.0055(8) O13 0.0195(10) 0.0095(9) 0.0117(10) -0.0005(7) -0.0003(8) -0.0032(8) O14 0.0130(10) 0.0166(9) 0.0108(9) -0.0013(8) 0.0015(7) -0.0053(8) O1W 0.0125(10) 0.0121(10) 0.0213(11) 0.0017(8) -0.0027(8) -0.0056(8) O2W 0.0121(9) 0.0077(9) 0.0113(10) -0.0008(8) 0.0027(7) -0.0019(7) O3W 0.0190(10) 0.0112(9) 0.0119(10) -0.0019(8) 0.0018(8) -0.0035(8) O4W 0.0519(17) 0.0186(12) 0.0394(15) -0.0075(11) 0.0248(13) -0.0108(11) O5W 0.075(3) 0.054(2) 0.105(3) -0.010(2) -0.022(2) -0.015(2) O6W 0.0487(17) 0.0460(17) 0.0552(19) -0.0319(15) 0.0266(15) -0.0335(14) O1H 0.0093(9) 0.0077(8) 0.0099(9) -0.0039(7) 0.0005(7) -0.0019(7) C1 0.0096(12) 0.0108(12) 0.0087(12) -0.0026(10) 0.0005(10) -0.0035(10) C2 0.0099(12) 0.0093(12) 0.0132(13) -0.0046(10) 0.0019(10) -0.0031(10) C3 0.0097(12) 0.0115(12) 0.0094(13) -0.0026(10) 0.0005(10) -0.0045(10) C4 0.0131(13) 0.0067(12) 0.0103(13) -0.0007(10) 0.0009(10) -0.0016(10) C5 0.0133(13) 0.0095(12) 0.0104(13) -0.0048(10) 0.0033(10) -0.0045(10) C6 0.0117(13) 0.0128(12) 0.0080(13) -0.0026(10) -0.0001(10) -0.0034(10) C7 0.0100(12) 0.0110(12) 0.0124(13) -0.0018(10) -0.0016(10) -0.0048(10) C8 0.0102(12) 0.0091(12) 0.0101(13) -0.0043(10) 0.0007(10) -0.0002(10) C9 0.0090(12) 0.0115(12) 0.0109(13) -0.0044(10) 0.0004(10) -0.0039(10) C10 0.0093(12) 0.0102(12) 0.0094(12) -0.0029(10) 0.0003(10) -0.0028(10) C11 0.0095(12) 0.0072(11) 0.0097(13) -0.0013(10) 0.0007(10) -0.0023(9) C12 0.0094(12) 0.0094(12) 0.0114(13) -0.0044(10) -0.0002(10) -0.0024(10) C13 0.0095(12) 0.0109(12) 0.0080(12) -0.0016(10) 0.0003(10) -0.0029(10) C14 0.0096(12) 0.0068(11) 0.0110(13) -0.0016(10) 0.0007(10) -0.0022(9) C15 0.0073(12) 0.0112(12) 0.0134(13) -0.0044(10) 0.0021(10) -0.0034(10) C16 0.0098(12) 0.0085(12) 0.0099(13) -0.0024(10) 0.0025(10) -0.0025(10) _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 Ni1 O3 2.0340(19) 1_556 ? Ni1 O10 2.0439(18) 2_666 ? Ni1 O1W 2.045(2) . ? Ni1 O1H 2.0552(18) . ? Ni1 O1 2.0729(18) 2_756 ? Ni1 O2W 2.097(2) . ? Ni1 Ni2 2.9756(7) . ? Ni2 O1H 1.9986(19) . ? Ni2 O8 2.0020(18) 2_656 ? Ni2 O2W 2.081(2) . ? Ni2 O7 2.0846(19) . ? Ni2 O11 2.0971(19) . ? Ni2 O11 2.1177(18) 2_666 ? Ni3 O9 2.0216(19) 2_656 ? Ni3 O1H 2.0437(18) . ? Ni3 O3W 2.058(2) . ? Ni3 O4 2.0658(19) 1_556 ? Ni3 O12 2.1053(19) . ? Ni3 O1 2.1303(18) 2_756 ? S1 O5 1.4476(19) . ? S1 O7 1.4713(19) . ? S1 O6 1.480(2) . ? S1 C5 1.769(3) . ? S2 O13 1.4511(19) . ? S2 O14 1.466(2) . ? S2 O12 1.4787(18) . ? S2 C13 1.773(3) . ? Na1 O5 2.316(2) 2_666 ? Na1 O13 2.374(2) 2_657 ? Na1 O4W 2.396(3) . ? Na1 O12 2.469(2) . ? Na1 O4 2.517(2) 1_556 ? Na1 O5W 2.754(4) . ? O1 C7 1.298(3) . ? O1 Ni1 2.0729(18) 2_756 ? O1 Ni3 2.1303(18) 2_756 ? O2 C7 1.247(3) . ? O3 C8 1.263(3) . ? O3 Ni1 2.0340(19) 1_554 ? O4 C8 1.261(3) . ? O4 Ni3 2.0658(19) 1_554 ? O4 Na1 2.517(2) 1_554 ? O5 Na1 2.316(2) 2_666 ? O8 C15 1.267(3) . ? O8 Ni2 2.0020(18) 2_656 ? O9 C15 1.267(3) . ? O9 Ni3 2.0216(19) 2_656 ? O10 C16 1.250(3) . ? O10 Ni1 2.0439(18) 2_666 ? O11 C16 1.295(3) . ? O11 Ni2 2.1177(18) 2_666 ? O13 Na1 2.374(2) 2_657 ? C1 C2 1.394(4) . ? C1 C6 1.399(4) . ? C1 C7 1.495(3) . ? C2 C3 1.400(4) . ? C3 C4 1.400(4) . ? C3 C8 1.496(4) . ? C4 C5 1.395(4) . ? C5 C6 1.391(4) . ? C9 C14 1.395(4) . ? C9 C10 1.402(3) . ? C9 C15 1.528(4) . ? C10 C11 1.401(4) . ? C11 C12 1.393(4) . ? C11 C16 1.512(3) . ? C12 C13 1.396(3) . ? C13 C14 1.393(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 O3 Ni1 O10 90.47(8) 1_556 2_666 ? O3 Ni1 O1W 90.84(8) 1_556 . ? O10 Ni1 O1W 89.25(8) 2_666 . ? O3 Ni1 O1H 94.45(8) 1_556 . ? O10 Ni1 O1H 100.45(7) 2_666 . ? O1W Ni1 O1H 168.88(8) . . ? O3 Ni1 O1 91.11(7) 1_556 2_756 ? O10 Ni1 O1 176.49(7) 2_666 2_756 ? O1W Ni1 O1 87.60(7) . 2_756 ? O1H Ni1 O1 82.54(7) . 2_756 ? O3 Ni1 O2W 177.47(7) 1_556 . ? O10 Ni1 O2W 90.46(7) 2_666 . ? O1W Ni1 O2W 91.52(8) . . ? O1H Ni1 O2W 83.06(7) . . ? O1 Ni1 O2W 88.09(7) 2_756 . ? O3 Ni1 Ni2 133.43(6) 1_556 . ? O10 Ni1 Ni2 84.39(5) 2_666 . ? O1W Ni1 Ni2 135.14(6) . . ? O1H Ni1 Ni2 42.04(5) . . ? O1 Ni1 Ni2 96.77(5) 2_756 . ? O2W Ni1 Ni2 44.36(5) . . ? O1H Ni2 O8 95.14(7) . 2_656 ? O1H Ni2 O2W 84.88(8) . . ? O8 Ni2 O2W 90.93(8) 2_656 . ? O1H Ni2 O7 174.71(7) . . ? O8 Ni2 O7 89.17(8) 2_656 . ? O2W Ni2 O7 92.01(7) . . ? O1H Ni2 O11 99.20(7) . . ? O8 Ni2 O11 100.54(7) 2_656 . ? O2W Ni2 O11 167.37(7) . . ? O7 Ni2 O11 82.97(7) . . ? O1H Ni2 O11 90.93(7) . 2_666 ? O8 Ni2 O11 173.66(7) 2_656 2_666 ? O2W Ni2 O11 87.76(7) . 2_666 ? O7 Ni2 O11 84.67(7) . 2_666 ? O11 Ni2 O11 80.26(7) . 2_666 ? O1H Ni2 Ni1 43.52(5) . . ? O8 Ni2 Ni1 107.72(6) 2_656 . ? O2W Ni2 Ni1 44.81(5) . . ? O7 Ni2 Ni1 132.03(5) . . ? O11 Ni2 Ni1 133.82(5) . . ? O11 Ni2 Ni1 75.56(5) 2_666 . ? O9 Ni3 O1H 97.97(7) 2_656 . ? O9 Ni3 O3W 93.50(8) 2_656 . ? O1H Ni3 O3W 166.23(8) . . ? O9 Ni3 O4 174.02(7) 2_656 1_556 ? O1H Ni3 O4 88.00(7) . 1_556 ? O3W Ni3 O4 80.62(8) . 1_556 ? O9 Ni3 O12 95.84(7) 2_656 . ? O1H Ni3 O12 98.74(7) . . ? O3W Ni3 O12 87.60(8) . . ? O4 Ni3 O12 82.91(7) 1_556 . ? O9 Ni3 O1 91.40(7) 2_656 2_756 ? O1H Ni3 O1 81.41(7) . 2_756 ? O3W Ni3 O1 90.74(7) . 2_756 ? O4 Ni3 O1 89.76(7) 1_556 2_756 ? O12 Ni3 O1 172.65(7) . 2_756 ? O5 S1 O7 111.48(12) . . ? O5 S1 O6 113.25(11) . . ? O7 S1 O6 111.90(11) . . ? O5 S1 C5 108.15(12) . . ? O7 S1 C5 104.96(11) . . ? O6 S1 C5 106.57(12) . . ? O13 S2 O14 113.59(11) . . ? O13 S2 O12 113.23(11) . . ? O14 S2 O12 108.93(11) . . ? O13 S2 C13 108.16(12) . . ? O14 S2 C13 106.74(12) . . ? O12 S2 C13 105.68(11) . . ? O5 Na1 O13 168.48(9) 2_666 2_657 ? O5 Na1 O4W 82.24(9) 2_666 . ? O13 Na1 O4W 93.89(9) 2_657 . ? O5 Na1 O12 80.58(7) 2_666 . ? O13 Na1 O12 110.73(8) 2_657 . ? O4W Na1 O12 117.56(9) . . ? O5 Na1 O4 93.03(8) 2_666 1_556 ? O13 Na1 O4 89.58(7) 2_657 1_556 ? O4W Na1 O4 172.33(9) . 1_556 ? O12 Na1 O4 67.25(7) . 1_556 ? O5 Na1 O5W 101.10(10) 2_666 . ? O13 Na1 O5W 67.38(10) 2_657 . ? O4W Na1 O5W 71.80(11) . . ? O12 Na1 O5W 170.63(11) . . ? O4 Na1 O5W 103.40(10) 1_556 . ? C7 O1 Ni1 126.40(15) . 2_756 ? C7 O1 Ni3 116.62(15) . 2_756 ? Ni1 O1 Ni3 93.32(7) 2_756 2_756 ? C8 O3 Ni1 124.05(17) . 1_554 ? C8 O4 Ni3 127.99(17) . 1_554 ? C8 O4 Na1 120.21(17) . 1_554 ? Ni3 O4 Na1 104.09(8) 1_554 1_554 ? S1 O5 Na1 170.05(13) . 2_666 ? S1 O7 Ni2 134.27(12) . . ? C15 O8 Ni2 138.87(18) . 2_656 ? C15 O9 Ni3 132.45(16) . 2_656 ? C16 O10 Ni1 123.20(16) . 2_666 ? C16 O11 Ni2 126.55(16) . . ? C16 O11 Ni2 128.97(16) . 2_666 ? Ni2 O11 Ni2 99.74(7) . 2_666 ? S2 O12 Ni3 133.68(12) . . ? S2 O12 Na1 121.12(11) . . ? Ni3 O12 Na1 104.52(8) . . ? S2 O13 Na1 130.95(12) . 2_657 ? Ni2 O2W Ni1 90.83(7) . . ? Ni2 O1H Ni3 127.14(9) . . ? Ni2 O1H Ni1 94.44(7) . . ? Ni3 O1H Ni1 96.47(8) . . ? C2 C1 C6 119.8(2) . . ? C2 C1 C7 119.5(2) . . ? C6 C1 C7 120.5(2) . . ? C1 C2 C3 120.5(2) . . ? C4 C3 C2 120.1(2) . . ? C4 C3 C8 121.9(2) . . ? C2 C3 C8 118.0(2) . . ? C5 C4 C3 118.5(2) . . ? C6 C5 C4 122.0(2) . . ? C6 C5 S1 118.7(2) . . ? C4 C5 S1 119.20(19) . . ? C5 C6 C1 119.0(2) . . ? O2 C7 O1 124.8(2) . . ? O2 C7 C1 119.0(2) . . ? O1 C7 C1 116.2(2) . . ? O4 C8 O3 125.9(3) . . ? O4 C8 C3 115.6(2) . . ? O3 C8 C3 118.5(2) . . ? C14 C9 C10 120.2(2) . . ? C14 C9 C15 118.7(2) . . ? C10 C9 C15 120.9(2) . . ? C11 C10 C9 119.4(2) . . ? C12 C11 C10 120.4(2) . . ? C12 C11 C16 116.3(2) . . ? C10 C11 C16 123.3(2) . . ? C11 C12 C13 119.5(2) . . ? C14 C13 C12 120.6(2) . . ? C14 C13 S2 122.60(19) . . ? C12 C13 S2 116.8(2) . . ? C13 C14 C9 119.7(2) . . ? O9 C15 O8 127.6(2) . . ? O9 C15 C9 117.7(2) . . ? O8 C15 C9 114.6(2) . . ? O10 C16 O11 124.8(2) . . ? O10 C16 C11 119.2(2) . . ? O11 C16 C11 116.0(2) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.799 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.104