data_NimmBTC _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety "C18 H6 Ni3 O18, Na O5, 2(O)" _chemical_formula_sum 'C18 H6 Na Ni3 O25' _chemical_formula_weight 821.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' -0.0020 0.0020 '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' -0.0041 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.1906 1.3024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M "P b c a" _symmetry_space_group_name_Hall "-P 2ac 2ab" loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.430(4) _cell_length_b 18.800(5) _cell_length_c 21.356(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5794(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description hexagon _exptl_crystal_colour green _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.883 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 2.583 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type ? _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 5459 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 33.52 _reflns_number_total 5459 _reflns_number_gt 4486 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.2000P)^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 SHELXL _refine_ls_extinction_coef 0.0000(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5459 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1578 _refine_ls_R_factor_gt 0.1382 _refine_ls_wR_factor_ref 0.3608 _refine_ls_wR_factor_gt 0.3387 _refine_ls_goodness_of_fit_ref 1.508 _refine_ls_restrained_S_all 1.508 _refine_ls_shift/su_max 0.788 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.19986(11) 0.03722(9) 0.12232(7) 0.0027(5) Uiso 1 1 d . . . Ni2 Ni 0.03775(10) 0.03382(9) 0.20985(7) 0.0018(5) Uiso 1 1 d . . . Ni3 Ni 0.06375(9) 0.14663(9) 0.09325(7) 0.0018(5) Uiso 1 1 d . . . Na4 Na 0.0892(4) -0.2066(3) 0.1270(2) 0.0140(12) Uiso 1 1 d . . . O2 O 0.0383(6) -0.1094(5) 0.2211(4) 0.0088(19) Uiso 1 1 d . . . O3 O 0.0303(5) 0.1815(5) 0.1866(4) 0.0052(18) Uiso 1 1 d . . . O4 O 0.2138(6) -0.1082(5) 0.1255(4) 0.0050(19) Uiso 1 1 d . . . O5 O 0.1723(6) 0.1848(5) 0.1175(4) 0.0092(19) Uiso 1 1 d . . . O6 O -0.0562(5) 0.0216(5) 0.1641(4) 0.0065(19) Uiso 1 1 d . . . O7 O 0.0856(6) 0.2138(5) -0.2286(4) 0.0087(19) Uiso 1 1 d . . . O8 O 0.4149(6) 0.1654(6) -0.0700(4) 0.011(2) Uiso 1 1 d . . . O9 O -0.0436(5) 0.1140(5) 0.0803(4) 0.0046(18) Uiso 1 1 d . . . O10 O 0.0927(6) 0.0280(5) 0.1299(4) 0.0021(19) Uiso 1 1 d . . . O11 O -0.2775(5) 0.1994(5) -0.0296(4) 0.0049(18) Uiso 1 1 d . . . O13 O -0.0224(6) 0.0566(5) 0.2894(4) 0.010(2) Uiso 1 1 d . . . O14 O 0.1990(6) 0.0418(5) 0.0283(4) 0.0072(19) Uiso 1 1 d . . . O15 O 0.1473(7) -0.2863(5) 0.0437(5) 0.016(2) Uiso 1 1 d . . . O16 O 0.1841(6) 0.2004(5) -0.2862(5) 0.017(2) Uiso 1 1 d . . . O17 O 0.4149(6) 0.2028(5) -0.1725(4) 0.010(2) Uiso 1 1 d . . . O18 O 0.1434(7) -0.2950(6) 0.2038(5) 0.022(2) Uiso 1 1 d . . . O19 O -0.3785(6) 0.1655(5) 0.0229(4) 0.011(2) Uiso 1 1 d . . . O20 O -0.3771(6) 0.0575(5) 0.2342(4) 0.0108(19) Uiso 1 1 d . . . O21 O -0.2755(6) 0.0403(5) 0.2865(4) 0.010(2) Uiso 1 1 d . . . O22 O 0.0456(5) 0.2786(5) 0.0699(4) 0.0054(18) Uiso 1 1 d . . . C24 C -0.3110(8) 0.1676(8) 0.0187(6) 0.008(3) Uiso 1 1 d . . . O25 O 0.1008(5) 0.1199(5) 0.0024(4) 0.0074(19) Uiso 1 1 d . . . C26 C 0.2703(8) 0.1185(8) -0.0731(6) 0.009(3) Uiso 1 1 d . . . H26 H 0.3088 0.0980 -0.0419 0.011 Uiso 1 1 calc R . . C27 C -0.2701(7) 0.0746(7) 0.1792(6) 0.002(2) Uiso 1 1 d . . . C28 C -0.1595(8) 0.0868(8) 0.1225(6) 0.004(3) Uiso 1 1 d . . . O29 O 0.3081(6) 0.0663(5) 0.1141(5) 0.017(2) Uiso 1 1 d . . . C30 C -0.3062(8) 0.1062(8) 0.1263(5) 0.004(3) Uiso 1 1 d . . . H30 H -0.3716 0.1116 0.1282 0.005 Uiso 1 1 calc R . . C31 C -0.2696(7) 0.1315(8) 0.0721(6) 0.005(2) Uiso 1 1 d . . . C32 C -0.1964(8) 0.0642(7) 0.1773(6) 0.006(3) Uiso 1 1 d . . . H32 H -0.1620 0.0420 0.2099 0.007 Uiso 1 1 calc R . . C33 C -0.0804(8) 0.0713(8) 0.1219(6) 0.004(3) Uiso 1 1 d . . . C34 C 0.3070(8) 0.1541(7) -0.1254(5) 0.005(3) Uiso 1 1 d . . . O35 O -0.0178(10) -0.3007(7) 0.1284(6) 0.041(4) Uiso 1 1 d . . . C36 C 0.1517(7) 0.1950(7) -0.2340(6) 0.005(2) Uiso 1 1 d . . . C37 C 0.1922(8) 0.1708(8) -0.1773(6) 0.007(3) Uiso 1 1 d . . . C39 C 0.1577(8) 0.1462(8) -0.1220(6) 0.006(3) Uiso 1 1 d . . . H39 H 0.0924 0.1513 -0.1188 0.007 Uiso 1 1 calc R . . C40 C 0.1964(7) 0.1158(7) -0.0705(5) 0.001(2) Uiso 1 1 d . . . C41 C 0.2666(8) 0.1746(8) -0.1777(6) 0.008(3) Uiso 1 1 d . . . H41 H 0.3004 0.1913 -0.2129 0.009 Uiso 1 1 calc R . . C42 C -0.3106(7) 0.0555(8) 0.2374(6) 0.005(3) Uiso 1 1 d . . . O44 O 0.0362(6) -0.1113(5) 0.0514(4) 0.0080(19) Uiso 1 1 d . . . C45 C -0.1962(8) 0.1216(7) 0.0696(6) 0.008(3) Uiso 1 1 d . . . H45 H -0.1594 0.1351 0.0348 0.010 Uiso 1 1 calc R . . C46 C 0.3841(8) 0.1752(8) -0.1238(6) 0.008(3) Uiso 1 1 d . . . O1W O 0.0996(8) 0.4240(7) 0.1450(6) 0.031(3) Uiso 1 1 d . . . C11X C 0.1622(7) 0.0877(7) -0.0081(6) 0.001(2) Uiso 1 1 d . . . _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 O10 1.565(8) . ? Ni1 O29 1.664(9) . ? Ni1 O21 1.980(9) 6_656 ? Ni1 O14 2.010(9) . ? Ni1 Ni3 2.911(2) . ? Ni1 Ni2 2.995(2) . ? Ni2 O6 1.687(8) . ? Ni2 O20 1.770(9) 6_656 ? Ni2 O10 1.885(8) . ? Ni2 O13 1.955(9) . ? Ni2 C42 2.495(11) 6_656 ? Ni3 O9 1.689(8) . ? Ni3 O5 1.799(9) . ? Ni3 O25 2.073(9) . ? Ni3 O3 2.153(9) . ? Ni3 O10 2.401(9) . ? Na4 O35 2.348(15) . ? Na4 O18 2.462(12) . ? Na4 O15 2.472(12) . ? Na4 O44 2.532(11) . ? Na4 O4 2.581(10) . ? Na4 O2 2.814(10) . ? O6 C33 1.344(17) . ? O7 C36 1.023(13) . ? O8 C46 1.245(16) . ? O9 C33 1.310(16) . ? O11 C24 1.285(16) . ? O14 C11X 1.275(15) . ? O16 C36 1.212(16) . ? O17 C46 1.244(16) . ? O19 C24 0.979(14) . ? O20 C42 0.963(13) . ? O20 Ni2 1.770(9) 6_556 ? O21 C42 1.199(15) . ? O21 Ni1 1.980(9) 6_556 ? C24 C31 1.456(18) . ? O25 C11X 1.098(14) . ? C26 C40 1.068(15) . ? C26 C34 1.406(18) . ? C26 C39 2.000(18) . ? C27 C32 1.082(15) . ? C27 C30 1.380(17) . ? C27 C42 1.420(17) . ? C27 C28 2.015(16) . ? C28 C33 1.179(16) . ? C28 C32 1.354(18) . ? C28 C45 1.409(18) . ? C30 C31 1.357(17) . ? C30 C45 2.016(17) . ? C31 C45 1.076(16) . ? C34 C46 1.182(17) . ? C34 C41 1.318(17) . ? C34 C37 2.018(17) . ? C36 C37 1.420(18) . ? C37 C41 1.075(16) . ? C37 C39 1.362(18) . ? C39 C40 1.359(17) . ? C40 C11X 1.517(17) . ? C42 Ni2 2.495(11) 6_556 ? 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 O10 Ni1 O29 167.2(5) . . ? O10 Ni1 O21 94.5(4) . 6_656 ? O29 Ni1 O21 85.7(4) . 6_656 ? O10 Ni1 O14 95.9(4) . . ? O29 Ni1 O14 83.5(4) . . ? O21 Ni1 O14 169.2(4) 6_656 . ? O10 Ni1 Ni3 55.5(3) . . ? O29 Ni1 Ni3 112.3(4) . . ? O21 Ni1 Ni3 108.1(3) 6_656 . ? O14 Ni1 Ni3 75.6(3) . . ? O10 Ni1 Ni2 32.9(3) . . ? O29 Ni1 Ni2 143.7(4) . . ? O21 Ni1 Ni2 61.8(3) 6_656 . ? O14 Ni1 Ni2 128.3(3) . . ? Ni3 Ni1 Ni2 67.74(6) . . ? O6 Ni2 O20 169.4(4) . 6_656 ? O6 Ni2 O10 78.8(4) . . ? O20 Ni2 O10 109.5(4) 6_656 . ? O6 Ni2 O13 100.2(4) . . ? O20 Ni2 O13 70.5(4) 6_656 . ? O10 Ni2 O13 170.5(4) . . ? O6 Ni2 C42 171.4(4) . 6_656 ? O20 Ni2 C42 17.4(4) 6_656 6_656 ? O10 Ni2 C42 92.8(4) . 6_656 ? O13 Ni2 C42 87.8(4) . 6_656 ? O6 Ni2 Ni1 105.6(3) . . ? O20 Ni2 Ni1 82.7(3) 6_656 . ? O10 Ni2 Ni1 26.8(2) . . ? O13 Ni2 Ni1 152.2(3) . . ? C42 Ni2 Ni1 66.0(3) 6_656 . ? O9 Ni3 O5 172.1(4) . . ? O9 Ni3 O25 89.7(4) . . ? O5 Ni3 O25 98.1(4) . . ? O9 Ni3 O3 93.2(4) . . ? O5 Ni3 O3 78.9(4) . . ? O25 Ni3 O3 175.9(3) . . ? O9 Ni3 O10 82.9(4) . . ? O5 Ni3 O10 97.2(4) . . ? O25 Ni3 O10 92.0(3) . . ? O3 Ni3 O10 91.1(3) . . ? O9 Ni3 Ni1 113.4(3) . . ? O5 Ni3 Ni1 68.5(3) . . ? O25 Ni3 Ni1 81.6(2) . . ? O3 Ni3 Ni1 99.7(2) . . ? O10 Ni3 Ni1 32.5(2) . . ? O35 Na4 O18 72.1(4) . . ? O35 Na4 O15 77.1(4) . . ? O18 Na4 O15 87.9(4) . . ? O35 Na4 O44 110.0(4) . . ? O18 Na4 O44 177.3(4) . . ? O15 Na4 O44 94.1(4) . . ? O35 Na4 O4 177.0(5) . . ? O18 Na4 O4 105.8(4) . . ? O15 Na4 O4 100.9(3) . . ? O44 Na4 O4 72.2(3) . . ? O35 Na4 O2 107.9(4) . . ? O18 Na4 O2 92.6(4) . . ? O15 Na4 O2 174.9(4) . . ? O44 Na4 O2 85.2(3) . . ? O4 Na4 O2 74.0(3) . . ? C33 O6 Ni2 120.2(8) . . ? C33 O9 Ni3 118.8(8) . . ? Ni1 O10 Ni2 120.2(5) . . ? Ni1 O10 Ni3 92.0(4) . . ? Ni2 O10 Ni3 99.7(4) . . ? C11X O14 Ni1 129.8(8) . . ? C42 O20 Ni2 129.3(11) . 6_556 ? C42 O21 Ni1 142.3(9) . 6_556 ? O19 C24 O11 117.7(13) . . ? O19 C24 C31 108.5(13) . . ? O11 C24 C31 133.7(11) . . ? C11X O25 Ni3 122.3(9) . . ? C40 C26 C34 116.0(14) . . ? C40 C26 C39 39.6(9) . . ? C34 C26 C39 76.5(8) . . ? C32 C27 C30 114.8(13) . . ? C32 C27 C42 113.1(12) . . ? C30 C27 C42 132.1(10) . . ? C32 C27 C28 38.8(9) . . ? C30 C27 C28 76.0(8) . . ? C42 C27 C28 151.7(9) . . ? C33 C28 C32 108.2(12) . . ? C33 C28 C45 118.0(12) . . ? C32 C28 C45 133.7(11) . . ? C33 C28 C27 138.2(12) . . ? C32 C28 C27 30.0(7) . . ? C45 C28 C27 103.7(9) . . ? C31 C30 C27 134.6(12) . . ? C31 C30 C45 29.8(7) . . ? C27 C30 C45 104.8(9) . . ? C45 C31 C30 111.4(13) . . ? C45 C31 C24 116.5(13) . . ? C30 C31 C24 132.2(11) . . ? C27 C32 C28 111.2(13) . . ? C28 C33 O9 104.4(12) . . ? C28 C33 O6 114.6(12) . . ? O9 C33 O6 140.9(11) . . ? C46 C34 C41 110.1(13) . . ? C46 C34 C26 119.5(12) . . ? C41 C34 C26 130.2(12) . . ? C46 C34 C37 137.4(12) . . ? C41 C34 C37 29.0(7) . . ? C26 C34 C37 101.6(9) . . ? O7 C36 O16 115.7(13) . . ? O7 C36 C37 113.5(12) . . ? O16 C36 C37 130.7(11) . . ? C41 C37 C39 113.2(14) . . ? C41 C37 C36 112.5(13) . . ? C39 C37 C36 134.2(11) . . ? C41 C37 C34 36.4(9) . . ? C39 C37 C34 76.7(8) . . ? C36 C37 C34 148.9(10) . . ? C40 C39 C37 134.0(12) . . ? C40 C39 C26 30.0(7) . . ? C37 C39 C26 104.2(9) . . ? C26 C40 C39 110.4(13) . . ? C26 C40 C11X 112.7(12) . . ? C39 C40 C11X 136.4(10) . . ? C37 C41 C34 114.6(14) . . ? O20 C42 O21 119.5(14) . . ? O20 C42 C27 109.8(13) . . ? O21 C42 C27 130.7(11) . . ? O20 C42 Ni2 33.3(8) . 6_556 ? O21 C42 Ni2 86.4(8) . 6_556 ? C27 C42 Ni2 142.9(8) . 6_556 ? C31 C45 C28 114.2(13) . . ? C31 C45 C30 38.8(9) . . ? C28 C45 C30 75.4(8) . . ? C34 C46 O17 116.9(13) . . ? C34 C46 O8 108.2(12) . . ? O17 C46 O8 134.9(12) . . ? O25 C11X O14 125.7(12) . . ? O25 C11X C40 104.5(11) . . ? O14 C11X C40 129.5(10) . . ? _diffrn_measured_fraction_theta_max 0.477 _diffrn_reflns_theta_full 33.52 _diffrn_measured_fraction_theta_full 0.477 _refine_diff_density_max 6.993 _refine_diff_density_min -3.630 _refine_diff_density_rms 0.444