# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1588 data_winsom _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ; [Ni9(chp)3(Hchp)(OH)6(Me3NCH2CO2)9(CO3)Cl].[Ni(chp)3]4.0.5Cl.(chp.Hchp)1.5. 8.5EtOAc ; _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C193.50 H240.50 Cl22.50 N30 Ni13 O65' _chemical_formula_weight 5587.51 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 30.603(2) _cell_length_b 30.603(2) _cell_length_c 46.202(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 37473.1(53) _cell_formula_units_Z 6 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 71 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description 'plate developed in (001)' _exptl_crystal_colour Green _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method ? _exptl_crystal_F_000 17268 _exptl_absorpt_coefficient_mu 3.919 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.135 _exptl_absorpt_correction_T_max 0.729 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; Stoe Stadi-4 diffractometer with Oxford Cryosystems variable temperature device. ; _diffrn_measurement_method Omega-theta _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 10611 _diffrn_reflns_av_R_equivalents 0.2318 _diffrn_reflns_av_sigmaI/netI 0.1599 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 56.00 _reflns_number_total 10473 _reflns_number_observed 4829 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution DIRDIF _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. The diffuse solvent in the cell was treated in the manner described by van der Sluis and Spek. The solvent region accounts for 2453.9 e per cell, corresponding to 2.8EtOAc per asymmetric unit, or 8.5EtOAc per formula unit. Treating the solvent in this way was superior to modelling with partially-occupied EtOAc disordered over several orientations, which converged to R1=10.5% with a relatively high residual density of 1.6e in the solvent region. The final cycle of the 'squeeze' procedure output follows: PLATON(V-160797)-Run for: winsom in R-3 DATE 14-Jun-97 Cycle = 8, R(F) = 0.23, Nref(Hemi) = 35603, R(F > 4 SIGF) = 0.12 Nref = 16042 Density Maxima in Enhanced (Full) Difference Map x y z (e/A^3) Shortest Contacts within 0.359 0.328 0.383 5.78 void 0.805 0.547 0.441 5.38 void 0.452 0.048 0.309 4.37 void 1.000 1.001 0.766 4.16 void O2 3.15; O2 3.17; O2 3.19; 0.131 0.962 0.113 3.98 void 0.225 0.978 0.043 3.37 void 0.322 0.584 0.199 3.33 Cl3 0.06; C63 1.75; N13 2.62; C53 2.68; 0.436 0.572 0.777 3.24 void 0.147 0.891 0.626 3.13 C61 1.73; N11 2.59; C51 2.66; 0.093 0.813 0.920 3.12 void 0.717 0.641 0.508 3.00 Cl6 0.11; C66 1.79; N16 2.59; C56 2.71; 0.203 0.625 0.534 2.95 C32 1.89; C42 2.25; C22 3.17; 0.374 0.430 0.716 2.84 void VOID # gridpnts Electron-Count (e-) ======================================== A 376049 768.5 B 4098 8.9 C 4093 8.5 D 4067 7.7 E 376090 767.4 F 4052 8.4 G 4087 9.2 H 4075 7.8 I 4036 8.4 J 4019 7.6 K 4037 8.8 L 376055 767.7 M 4006 7.5 N 4002 8.2 O 4025 9.0 P 4107 9.1 Q 4093 8.6 R 4080 7.8 S 4066 8.3 T 4070 9.0 U 4072 7.6 Total (Positive) Electron Count/Cell = 2453.9 :: Fo-scale =0.150963E+02 - SinT/L-Min = 0.20 :: Omitted Outliers H K L Fo Fc Sig Del/Sig - [Abs(Fo-Abs(Fc))> 100.Sig] 0 -2 2 235.81 646.52 3.87 106.24 -2 2 2 235.81 642.86 3.87 105.30 2 0 2 235.81 643.44 3.87 105.45 Cycle = 9, R(F) = 0.23, Nref(Hemi) = 35603, R(F > 4 SIGF) = 0.12 Nref = 16054 SQUEEZE Statistics on the Difference Map Phasing =============================================================================== FcMod = Average contribution to Fc from discrete model FcSolv = Average contribution to Fc from solvent region FcTot = Average Fc total ( = model + solvent contrib.) DelMS = Average Phase difference between model and solvent contrib. DelMT = Average Phase difference between model and combined contrib. N = Number of reflections in Sin(Theta)/Lambda range R(Mod) = SIGMA(ABS(ABS(FcMod) - Fo)) / SIGMA(Fo) R(Tot) = SIGMA(ABS(ABS(FcTot) - Fo)) / SIGMA(Fo) SinT/L N R(Mod) R(Tot) =============================================================================== 0.05 579.44 246.89 553.54 452.20 110.09 30.66 31. 0.583 0.432 0.10 383.82 181.98 400.25 440.00 89.31 25.25 100. 0.384 0.143 0.15 388.60 107.61 410.46 448.99 83.24 17.81 232. 0.264 0.129 0.20 281.15 63.82 284.40 299.94 94.43 14.68 407. 0.248 0.152 0.25 271.89 41.85 276.24 296.44 87.81 9.18 632. 0.188 0.131 0.30 226.03 27.58 229.26 240.79 85.75 8.80 914. 0.170 0.130 0.35 177.15 24.07 180.78 184.22 85.45 9.53 1238. 0.193 0.157 0.40 138.29 22.70 141.70 141.82 88.26 10.46 1628. 0.258 0.209 0.45 105.22 21.10 109.08 107.71 86.81 12.83 2079. 0.311 0.252 0.50 94.35 20.44 97.60 92.13 87.94 13.99 2603. 0.359 0.285 0.55 78.47 17.03 80.93 74.06 89.70 13.57 2233. 0.416 0.337 N: Potential solvent area Vol = 10736.6 Ang^3 N: Electron Count / Cell = 2453.9 - To be included in D(calc), F000 & Mol.Wght. Although data were collected to 120\% Rsigma for reflections above 112\% rose above 0.6. These were therefore omitted from the refinement. The following is the final Shelxl res file (which the referee may find convenient): TITL winsom in R-3 -after Platon CELL 1.54184 30.6029 30.6029 46.2024 90.0000 90.0000 120.0000 ZERR 6 0.0020 0.0020 0.0050 0.0000 0.0000 0.0000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC C H N O CL NI UNIT 1161 1443 180 390 135 78 TEMP -53 OMIT -4 112 OMIT -1 2 0 OMIT 0 0 3 OMIT 0 1 5 OMIT 0 1 2 OMIT -2 2 2 OMIT 0 2 1 OMIT 0 1 8 L.S. 4 SIMU DELU FMAP 2 PLAN -10 ACTA WGHT 0.104900 FVAR 0.07666 NI1 6 1.10253 1.01100 0.30376 11.00000 0.02608 0.02538 = 0.03470 0.00070 0.00158 0.01259 NI2 6 1.00801 0.90545 0.30174 11.00000 0.02584 0.02526 = 0.03131 -0.00209 -0.00204 0.01332 NI3 6 0.90646 0.84151 0.25012 11.00000 0.03767 0.03935 = 0.04185 -0.01366 -0.01079 0.02284 O1 4 1.12239 1.07099 0.33104 11.00000 0.02841 0.03054 = 0.03545 0.00384 0.00790 0.01623 AFIX 3 H1 2 1.10390 1.06135 0.34940 11.00000 -1.20000 AFIX 0 O2 4 0.95761 0.90176 0.27326 11.00000 0.03423 0.03127 = 0.02962 -0.00151 0.00142 0.02089 AFIX 13 H2 2 0.97100 0.93335 0.26193 11.00000 -1.20000 AFIX 0 O10 4 1.02709 0.97828 0.31367 11.00000 0.02526 0.02603 = 0.03697 0.00142 -0.00231 0.01072 C10 1 1.00000 1.00000 0.31416 10.33333 0.03075 0.03075 = 0.01401 0.00000 0.00000 0.01538 CL 5 1.00000 1.00000 0.23446 10.33333 0.05701 0.05701 = 0.06845 0.00000 0.00000 0.02851 N11 3 0.87473 0.78238 0.32847 11.00000 0.03023 0.03079 = 0.05459 0.00579 0.00646 0.00469 AFIX 43 H11 2 0.89987 0.81044 0.33490 11.00000 -1.20000 AFIX 0 C21 1 0.85137 0.78123 0.30343 11.00000 0.04686 0.03246 = 0.05536 -0.00141 -0.00227 0.01383 C31 1 0.80945 0.73558 0.29421 11.00000 0.15382 0.04779 = 0.17891 0.03632 -0.10989 -0.02643 AFIX 43 H31 2 0.78991 0.73557 0.27851 11.00000 -1.20000 AFIX 0 C41 1 0.79733 0.69229 0.30767 11.00000 0.21093 0.04721 = 0.20098 0.04250 -0.14240 -0.04326 AFIX 43 H41 2 0.77459 0.66120 0.29911 11.00000 -1.20000 AFIX 0 C51 1 0.81876 0.69374 0.33452 11.00000 0.11795 0.03183 = 0.13440 0.02665 -0.05283 0.00473 AFIX 43 H51 2 0.80681 0.66489 0.34625 11.00000 -1.20000 AFIX 0 C61 1 0.85839 0.73972 0.34295 11.00000 0.06324 0.03579 = 0.06365 0.00078 -0.00903 0.02149 O21 4 0.86766 0.82351 0.28936 11.00000 0.04579 0.02729 = 0.05640 -0.00238 -0.00660 0.01590 CL1 5 0.89028 0.74333 0.37468 11.00000 0.08174 0.05834 = 0.06593 0.01790 -0.00208 0.01897 SAME 0.01 N11 > CL1 N12 3 0.86243 0.79399 0.21257 11.00000 0.06384 0.07565 = 0.09429 -0.03849 -0.02758 0.04791 C22 1 0.90180 0.82946 0.19650 11.00000 0.10917 0.09836 = 0.06416 -0.01886 -0.00227 0.06820 C32 1 0.89784 0.82983 0.16658 11.00000 0.14313 0.13129 = 0.07179 -0.03367 -0.03183 0.09771 AFIX 43 H32 2 0.92469 0.85533 0.15596 11.00000 -1.20000 AFIX 0 C42 1 0.85712 0.79514 0.15235 11.00000 0.14355 0.17499 = 0.09473 -0.02287 -0.03013 0.10180 C52 1 0.81746 0.75656 0.16833 11.00000 0.10918 0.16336 = 0.11895 -0.07108 -0.03603 0.09189 AFIX 43 H52 2 0.78880 0.73027 0.15934 11.00000 -1.20000 AFIX 0 C62 1 0.82321 0.75967 0.19804 11.00000 0.07468 0.12308 = 0.09150 -0.03456 -0.03488 0.07591 O22 4 0.94047 0.86386 0.21164 11.00000 0.08730 0.09323 = 0.04795 -0.01312 0.00043 0.06530 CL2 5 0.77516 0.71383 0.21928 11.00000 0.09780 0.09520 = 0.17890 -0.04378 -0.02711 0.03052 O1A 4 1.11799 0.97640 0.33581 11.00000 0.03611 0.03356 = 0.03824 0.00286 -0.00418 0.02075 O2A 4 1.04926 0.89964 0.33413 11.00000 0.02942 0.03342 = 0.04556 0.00153 -0.00676 0.01612 C1A 1 1.09043 0.93195 0.34443 11.00000 0.02458 0.03936 = 0.02921 0.00287 0.00133 0.01864 C2A 1 1.10764 0.91232 0.36932 11.00000 0.04234 0.03547 = 0.03475 -0.00012 -0.00694 0.02040 AFIX 23 H2A1 2 1.08074 0.89886 0.38387 11.00000 -1.20000 H2A2 2 1.11074 0.88387 0.36212 11.00000 -1.20000 AFIX 0 N3A 3 1.15619 0.94798 0.38445 11.00000 0.03491 0.04548 = 0.04144 -0.00089 -0.01139 0.02323 C4A 1 1.19974 0.96864 0.36355 11.00000 0.03646 0.04485 = 0.05917 -0.00415 -0.01074 0.01629 AFIX 33 H4A1 2 1.20168 0.94095 0.35465 11.00000 -1.50000 H4A2 2 1.23088 0.99018 0.37385 11.00000 -1.50000 H4A3 2 1.19473 0.98809 0.34869 11.00000 -1.50000 AFIX 0 C5A 1 1.15336 0.99040 0.39795 11.00000 0.06287 0.05454 = 0.05338 -0.02831 -0.01533 0.02766 AFIX 33 H5A1 2 1.14780 1.00947 0.38307 11.00000 -1.50000 H5A2 2 1.18474 1.01227 0.40794 11.00000 -1.50000 H5A3 2 1.12567 0.97725 0.41167 11.00000 -1.50000 AFIX 0 C6A 1 1.16469 0.91846 0.40736 11.00000 0.06759 0.06889 = 0.06126 0.00865 -0.02894 0.03877 AFIX 33 H6A1 2 1.16650 0.89068 0.39848 11.00000 -1.50000 H6A2 2 1.13700 0.90529 0.42108 11.00000 -1.50000 H6A3 2 1.19609 0.94025 0.41736 11.00000 -1.50000 AFIX 0 SAME 0.01 O1A > C6A O1B 4 0.86796 0.87951 0.23852 11.00000 0.03998 0.04356 = 0.03733 -0.01029 -0.00622 0.02409 O2B 4 0.87442 0.92622 0.27708 11.00000 0.03008 0.03863 = 0.03635 -0.00748 -0.00799 0.01964 C1B 1 0.86376 0.91320 0.25115 11.00000 0.02894 0.03960 = 0.03751 0.00153 0.00130 0.01751 C2B 1 0.84211 0.94077 0.23496 11.00000 0.03088 0.04084 = 0.04223 -0.00473 -0.01051 0.02101 AFIX 23 H2B1 2 0.86518 0.97703 0.23756 11.00000 -1.20000 H2B2 2 0.81018 0.93273 0.24428 11.00000 -1.20000 AFIX 0 N3B 3 0.83217 0.93101 0.20292 11.00000 0.05091 0.05943 = 0.04223 -0.00037 -0.01732 0.03157 C4B 1 0.79326 0.87707 0.19762 11.00000 0.08047 0.06241 = 0.06770 -0.03042 -0.03190 0.03179 AFIX 33 H4B1 2 0.76275 0.86895 0.20821 11.00000 -1.50000 H4B2 2 0.80601 0.85540 0.20411 11.00000 -1.50000 H4B3 2 0.78577 0.87189 0.17709 11.00000 -1.50000 AFIX 0 C5B 1 0.87888 0.94423 0.18703 11.00000 0.06618 0.11060 = 0.04231 0.00185 -0.00528 0.05267 AFIX 33 H5B1 2 0.90373 0.97925 0.19070 11.00000 -1.50000 H5B2 2 0.87174 0.93935 0.16645 11.00000 -1.50000 H5B3 2 0.89194 0.92278 0.19345 11.00000 -1.50000 AFIX 0 C6B 1 0.81149 0.96383 0.19269 11.00000 0.08943 0.08349 = 0.06457 0.00386 -0.01968 0.05933 AFIX 33 H6B1 2 0.78075 0.95513 0.20319 11.00000 -1.50000 H6B2 2 0.80421 0.95851 0.17214 11.00000 -1.50000 H6B3 2 0.83621 0.99897 0.19614 11.00000 -1.50000 AFIX 0 SAME 0.01 O1A > C6A O1C 4 0.99689 0.83729 0.29062 11.00000 0.04634 0.03090 = 0.04558 -0.00873 -0.00925 0.01894 O2C 4 0.93304 0.79430 0.25972 11.00000 0.06723 0.04454 = 0.06863 -0.03763 -0.03266 0.03772 C1C 1 0.96608 0.79908 0.27701 11.00000 0.04334 0.03080 = 0.04507 -0.00434 -0.00188 0.02241 C2C 1 0.96594 0.75020 0.28281 11.00000 0.06649 0.04125 = 0.06617 -0.00816 -0.00723 0.03163 AFIX 23 H2C1 2 0.93341 0.72651 0.29161 11.00000 -1.20000 H2C2 2 0.96742 0.73599 0.26407 11.00000 -1.20000 AFIX 0 N3C 3 1.00678 0.75171 0.30167 11.00000 0.07044 0.04229 = 0.05166 -0.00184 0.00584 0.03949 C4C 1 0.99909 0.69882 0.30362 11.00000 0.12245 0.05213 = 0.08549 -0.01529 -0.02736 0.06212 AFIX 33 H4C1 2 0.96565 0.67603 0.31114 11.00000 -1.50000 H4C2 2 1.02423 0.69891 0.31644 11.00000 -1.50000 H4C3 2 1.00248 0.68771 0.28451 11.00000 -1.50000 AFIX 0 C5C 1 1.05751 0.78573 0.29024 11.00000 0.06645 0.09180 = 0.10252 0.03412 0.02011 0.05214 AFIX 33 H5C1 2 1.06031 0.77513 0.27087 11.00000 -1.50000 H5C2 2 1.08246 0.78463 0.30270 11.00000 -1.50000 H5C3 2 1.06328 0.81990 0.28960 11.00000 -1.50000 AFIX 0 C6C 1 1.00161 0.76729 0.33155 11.00000 0.11893 0.06033 = 0.04681 0.00682 0.00914 0.05887 AFIX 33 H6C1 2 0.96794 0.74453 0.33879 11.00000 -1.50000 H6C2 2 1.00721 0.80141 0.33109 11.00000 -1.50000 H6C3 2 1.02631 0.76605 0.34416 11.00000 -1.50000 AFIX 0 NI4 6 1.00000 1.00000 0.39931 10.33333 0.03324 0.03324 = 0.03118 0.00000 0.00000 0.01662 SAME 0.01 N11 > CL1 N13 3 1.04901 1.06591 0.42094 11.00000 0.04121 0.02676 = 0.03219 -0.00087 -0.00495 0.01859 C23 1 1.08643 1.07450 0.40189 11.00000 0.03984 0.03427 = 0.03828 0.00616 0.00294 0.00533 C33 1 1.13576 1.11281 0.40747 11.00000 0.04180 0.05654 = 0.05709 0.00537 0.00915 0.00180 AFIX 43 H33 2 1.16123 1.12001 0.39379 11.00000 -1.20000 AFIX 0 C43 1 1.14726 1.13950 0.43216 11.00000 0.05433 0.06085 = 0.06219 -0.00450 -0.01304 0.00954 AFIX 43 H43 2 1.18096 1.16350 0.43639 11.00000 -1.20000 AFIX 0 C53 1 1.10887 1.13139 0.45149 11.00000 0.07140 0.05012 = 0.05392 -0.01891 -0.01818 0.01607 AFIX 43 H53 2 1.11549 1.15011 0.46868 11.00000 -1.20000 AFIX 0 C63 1 1.06071 1.09445 0.44405 11.00000 0.06101 0.03551 = 0.03719 0.00518 0.00407 0.02310 O23 4 1.07168 1.04400 0.37979 11.00000 0.04874 0.04625 = 0.03917 -0.00024 0.01243 0.02236 CL3 5 1.01076 1.08038 0.46732 11.00000 0.07792 0.08304 = 0.05577 -0.01962 0.00652 0.03955 NI5 6 1.03769 0.70342 0.21159 11.00000 0.05246 0.06757 = 0.04873 -0.01621 -0.00595 0.03382 SAME 0.01 N11 > CL1 N14 3 1.10909 0.73478 0.19571 11.00000 0.05340 0.06621 = 0.05874 -0.00455 -0.00063 0.02584 C24 1 1.12262 0.78011 0.20803 11.00000 0.07084 0.05981 = 0.05517 -0.00011 -0.01484 0.03418 C34 1 1.17149 0.82086 0.20450 11.00000 0.07112 0.05930 = 0.10235 0.01737 -0.01161 0.02654 AFIX 43 H34 2 1.17998 0.85254 0.21224 11.00000 -1.20000 AFIX 0 C44 1 1.20626 0.81509 0.19019 11.00000 0.07421 0.07981 = 0.10462 0.02944 0.00270 0.02640 AFIX 43 H44 2 1.23921 0.84249 0.18809 11.00000 -1.20000 AFIX 0 C54 1 1.19336 0.76806 0.17835 11.00000 0.06834 0.10646 = 0.10340 0.01594 0.02050 0.03898 AFIX 43 H54 2 1.21711 0.76269 0.16845 11.00000 -1.20000 AFIX 0 C64 1 1.14405 0.72993 0.18194 11.00000 0.06521 0.10509 = 0.07927 -0.02164 0.00055 0.04123 O24 4 1.08621 0.78099 0.22206 11.00000 0.08104 0.06537 = 0.08042 -0.01701 -0.02340 0.04815 CL4 5 1.12474 0.66972 0.16883 11.00000 0.08859 0.13836 = 0.18271 -0.07643 0.02992 0.04746 SAME 0.01 N11 > CL1 N15 3 1.00304 0.71875 0.17900 11.00000 0.09895 0.07297 = 0.09659 -0.03750 -0.04482 0.06035 C25 1 0.96495 0.71144 0.19689 11.00000 0.07909 0.07719 = 0.15996 -0.05859 -0.04852 0.05756 C35 1 0.92571 0.71853 0.18681 11.00000 0.12818 0.13619 = 0.26722 -0.07204 -0.08353 0.10569 AFIX 43 H35 2 0.89985 0.71427 0.19949 11.00000 -1.20000 AFIX 0 C45 1 0.92495 0.73142 0.15906 11.00000 0.16458 0.12151 = 0.31800 -0.03566 -0.13297 0.10723 AFIX 43 H45 2 0.89876 0.73636 0.15232 11.00000 -1.20000 AFIX 0 C55 1 0.96358 0.73742 0.14027 11.00000 0.17630 0.11724 = 0.20635 -0.00887 -0.13110 0.06155 AFIX 43 H55 2 0.96292 0.74402 0.12045 11.00000 -1.20000 AFIX 0 C65 1 1.00248 0.73319 0.15220 11.00000 0.12933 0.07922 = 0.11859 -0.02822 -0.08806 0.04753 O25 4 0.96890 0.69831 0.22336 11.00000 0.07383 0.12810 = 0.13099 -0.04532 0.00076 0.06650 CL5 5 1.05198 0.73960 0.13077 11.00000 0.23680 0.23609 = 0.08121 0.02754 -0.01715 0.12106 N16 3 1.01248 0.62716 0.20897 11.00000 0.05022 0.06379 = 0.05120 -0.01233 -0.01416 0.02920 C26 1 1.02790 0.62639 0.23694 11.00000 0.04905 0.06244 = 0.06081 -0.00247 -0.01646 0.00812 C36 1 1.02668 0.58245 0.24891 11.00000 0.12984 0.07855 = 0.07209 0.00985 -0.04211 0.02547 AFIX 43 H36 2 1.04067 0.58242 0.26701 11.00000 -1.20000 AFIX 0 C46 1 1.00360 0.54112 0.23178 11.00000 0.17014 0.07446 = 0.09321 0.00866 -0.03381 0.05713 AFIX 43 H46 2 0.99936 0.51062 0.23917 11.00000 -1.20000 AFIX 0 C56 1 0.98538 0.54051 0.20355 11.00000 0.11065 0.05737 = 0.08728 -0.00053 -0.02829 0.02392 AFIX 43 H56 2 0.96990 0.51129 0.19203 11.00000 -1.20000 AFIX 0 C66 1 0.99181 0.58352 0.19491 11.00000 0.06079 0.05803 = 0.06005 -0.00663 -0.01278 0.01941 O26 4 1.04936 0.67018 0.24816 11.00000 0.05259 0.07455 = 0.05725 -0.00809 -0.01753 0.01228 CL6 5 0.97132 0.58729 0.15984 11.00000 0.11687 0.10620 = 0.07139 -0.03430 -0.04276 0.07632 SAME 0.01 N11 > CL1 N17 3 0.00957 0.55426 0.04231 11.00000 0.04546 0.05765 = 0.06093 0.01290 -0.01412 0.00870 C27 1 -0.03722 0.51890 0.03301 11.00000 0.05092 0.06290 = 0.06800 -0.00053 -0.01603 0.01688 C37 1 -0.08031 0.51245 0.04747 11.00000 0.05188 0.08574 = 0.07967 0.01667 -0.00081 0.02624 AFIX 43 H37 2 -0.11239 0.48753 0.04109 11.00000 -1.20000 AFIX 0 C47 1 -0.07650 0.54120 0.07020 11.00000 0.05345 0.10151 = 0.06710 0.02809 0.00803 0.03553 AFIX 43 H47 2 -0.10565 0.53755 0.07925 11.00000 -1.20000 AFIX 0 C57 1 -0.02861 0.57677 0.08037 11.00000 0.07148 0.09894 = 0.06927 0.01747 -0.00932 0.03932 AFIX 43 H57 2 -0.02444 0.59621 0.09698 11.00000 -1.20000 AFIX 0 C67 1 0.01213 0.58189 0.06484 11.00000 0.04683 0.08752 = 0.05929 0.00334 -0.02073 0.01287 O27 4 -0.03902 0.49357 0.00991 11.00000 0.04782 0.07977 = 0.08604 -0.01773 -0.02179 0.02162 AFIX 83 H27 2 -0.00990 0.50252 0.00445 10.50000 -1.50000 AFIX 0 CL7 5 0.07280 0.62561 0.07640 11.00000 0.06074 0.11314 = 0.09452 -0.03630 -0.02325 0.01900 CL8 5 0.00000 0.00000 0.14867 10.16667 0.12007 0.12007 = 0.19774 0.00000 0.00000 0.06003 HKLF 4 100 0 1 0 1 0 0 0 0 -1 END WGHT 0.1046 0.0000 Q1 1 0.9100 0.8632 0.1357 11.00000 0.05 0.61 Q2 1 -0.0109 0.0300 0.1354 11.00000 0.05 0.57 Q3 1 0.8567 0.7899 0.2261 11.00000 0.05 0.51 Q4 1 0.9549 0.8933 0.2358 11.00000 0.05 0.50 Q5 1 0.0000 0.0000 0.1231 10.33333 0.05 0.43 Q6 1 0.0612 0.6512 0.0762 11.00000 0.05 0.43 Q7 1 0.8200 0.7726 0.1394 11.00000 0.05 0.43 Q8 1 0.8607 0.8173 0.1862 11.00000 0.05 0.41 Q9 1 1.0000 1.0000 0.2036 10.33333 0.05 0.39 Q10 1 0.8944 0.8233 0.1804 11.00000 0.05 0.39 Finally, here is a check on the space group: - This Search is on ALL NON-H Chemical Types - Number of Input Atoms Included in Search = 90 - Number of Excluded Disordered Input Atoms = 2 - The Structure implies the following Symmetry Elements subject to the Criteria: 1.00 Deg., (metric) 1.00 Ang. (distances) and 1.00 Ang. (inv. and transl.) Symm. Input Reduced (Ang) (Deg) (Ang) Input Cell Elem Cell Row Cell Row d Type Dot Angle Max. dev. x y z -------------------------------------------------------------------------------- 3 [ 0 0 1] [-1-1-1] 46.202 3 3 0.00 0.759 through 0 0 0 C2C -C1C [-1 0 1] 30.603 2 2 0 Metric [ 0 1-1] 30.603 2 2 0 Metric [ 1-1 0] 30.603 2 2 0 Metric -1 ====================================== 0.759 at 0 1/2 1/2 C2C -C1C Reduced->Convent Input->Reduced T = Input->Convent: a' = T a -------------------------------------------------------------------------------- ( -1 1 0 ) ( 0.67 0.33 0.33 ) ( -1 0 0 ) Det(T) ( 1 0 -1 ) X ( -0.33 0.33 0.33 ) = ( 1 1 0 ) = ( -1 -1 -1 ) ( -0.33 -0.67 0.33 ) ( 0 0 -1 ) 1.000 Cell Lattice a b c alpha beta gamma Volume CrystalSystem Laue -------------------------------------------------------------------------------- Input hR 30.603 30.603 46.202 90.00 90.00 120.00 37473 Trigonal -3 Reduced P 23.438 23.438 23.438 81.51 81.51 81.51 12491 Convent hR 30.603 30.603 46.202 90.00 90.00 120.00 37473 Trigonal -3 :: Lattice Features Metrical Symmetry not Supported by Contents. :: *** No Obvious Extra Crystallographic Symmetry was Detected *** ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1049P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment Riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10466 _refine_ls_number_parameters 796 _refine_ls_number_restraints 1025 _refine_ls_R_factor_all 0.1569 _refine_ls_R_factor_obs 0.0794 _refine_ls_wR_factor_all 0.2245 _refine_ls_wR_factor_obs 0.1824 _refine_ls_goodness_of_fit_all 0.886 _refine_ls_goodness_of_fit_obs 1.161 _refine_ls_restrained_S_all 0.927 _refine_ls_restrained_S_obs 1.100 _refine_ls_shift/esd_max -0.010 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 1.10253(5) 1.01100(5) 0.30376(3) 0.0288(4) Uani 1 d U . Ni2 Ni 1.00801(5) 0.90545(5) 0.30174(3) 0.0272(3) Uani 1 d U . Ni3 Ni 0.90646(5) 0.84151(6) 0.25012(3) 0.0380(4) Uani 1 d U . O1 O 1.1224(2) 1.0710(2) 0.33104(13) 0.0308(14) Uani 1 d U . H1 H 1.1039(2) 1.0614(2) 0.34940(13) 0.037 Uiso 1 d R . O2 O 0.9576(2) 0.9018(2) 0.27326(12) 0.0297(13) Uani 1 d U . H2 H 0.9710(2) 0.9334(2) 0.26193(12) 0.036 Uiso 1 calc R . O10 O 1.0271(2) 0.9783(2) 0.31367(12) 0.0304(13) Uani 1 d U . C10 C 1.0000 1.0000 0.3142(3) 0.025(3) Uani 1 d SU . Cl Cl 1.0000 1.0000 0.23446(11) 0.0608(13) Uani 1 d S . N11 N 0.8747(2) 0.7824(2) 0.32847(13) 0.043(2) Uani 1 d DU . H11 H 0.8999(2) 0.8104(2) 0.33490(13) 0.052 Uiso 1 calc R . C21 C 0.8514(3) 0.7812(3) 0.3034(2) 0.048(2) Uani 1 d DU . C31 C 0.8094(5) 0.7356(3) 0.2942(3) 0.161(8) Uani 1 d DU . H31 H 0.7899(5) 0.7356(3) 0.2785(3) 0.193 Uiso 1 calc R . C41 C 0.7973(7) 0.6923(3) 0.3077(3) 0.201(11) Uani 1 d DU . H41 H 0.7746(7) 0.6612(3) 0.2991(3) 0.241 Uiso 1 calc R . C51 C 0.8188(4) 0.6937(3) 0.3345(3) 0.109(6) Uani 1 d DU . H51 H 0.8068(4) 0.6649(3) 0.3462(3) 0.131 Uiso 1 calc R . C61 C 0.8584(3) 0.7397(3) 0.3430(2) 0.056(3) Uani 1 d DU . O21 O 0.8677(2) 0.8235(2) 0.28936(13) 0.0442(15) Uani 1 d DU . Cl1 Cl 0.89028(11) 0.74333(11) 0.37468(7) 0.0758(9) Uani 1 d DU . N12 N 0.8624(2) 0.7940(3) 0.2126(2) 0.072(2) Uani 1 d DU . C22 C 0.9018(3) 0.8295(4) 0.1965(2) 0.083(3) Uani 1 d DU . C32 C 0.8978(4) 0.8298(4) 0.1666(2) 0.102(4) Uani 1 d DU . H32 H 0.9247(4) 0.8553(4) 0.1560(2) 0.123 Uiso 1 calc R . C42 C 0.8571(5) 0.7951(5) 0.1524(2) 0.128(5) Uani 1 d DU . C52 C 0.8175(4) 0.7566(5) 0.1683(2) 0.120(5) Uani 1 d DU . H52 H 0.7888(4) 0.7303(5) 0.1593(2) 0.144 Uiso 1 calc R . C62 C 0.8232(3) 0.7597(4) 0.1980(2) 0.085(3) Uani 1 d DU . O22 O 0.9405(2) 0.8639(3) 0.21164(14) 0.067(2) Uani 1 d DU . Cl2 Cl 0.77516(15) 0.71383(14) 0.21928(12) 0.132(2) Uani 1 d DU . O1A O 1.1180(2) 0.9764(2) 0.33581(12) 0.0345(14) Uani 1 d DU . O2A O 1.0493(2) 0.8996(2) 0.33413(13) 0.0359(14) Uani 1 d DU . C1A C 1.0904(3) 0.9319(3) 0.3444(2) 0.030(2) Uani 1 d DU . C2A C 1.1076(3) 0.9123(3) 0.3693(2) 0.037(2) Uani 1 d DU . H2A1 H 1.0807(3) 0.8989(3) 0.3839(2) 0.045 Uiso 1 calc R . H2A2 H 1.1107(3) 0.8839(3) 0.3621(2) 0.045 Uiso 1 calc R . N3A N 1.1562(2) 0.9480(2) 0.38445(14) 0.039(2) Uani 1 d DU . C4A C 1.1997(3) 0.9686(3) 0.3636(2) 0.049(2) Uani 1 d DU . H4A1 H 1.2017(3) 0.9409(3) 0.3546(2) 0.073 Uiso 1 calc R . H4A2 H 1.2309(3) 0.9902(3) 0.3739(2) 0.073 Uiso 1 calc R . H4A3 H 1.1947(3) 0.9881(3) 0.3487(2) 0.073 Uiso 1 calc R . C5A C 1.1534(3) 0.9904(3) 0.3979(2) 0.058(3) Uani 1 d DU . H5A1 H 1.1478(3) 1.0095(3) 0.3831(2) 0.087 Uiso 1 calc R . H5A2 H 1.1847(3) 1.0123(3) 0.4079(2) 0.087 Uiso 1 calc R . H5A3 H 1.1257(3) 0.9773(3) 0.4117(2) 0.087 Uiso 1 calc R . C6A C 1.1647(4) 0.9185(3) 0.4074(2) 0.064(3) Uani 1 d DU . H6A1 H 1.1665(4) 0.8907(3) 0.3985(2) 0.096 Uiso 1 calc R . H6A2 H 1.1370(4) 0.9053(3) 0.4211(2) 0.096 Uiso 1 calc R . H6A3 H 1.1961(4) 0.9403(3) 0.4174(2) 0.096 Uiso 1 calc R . O1B O 0.8680(2) 0.8795(2) 0.23852(12) 0.0389(15) Uani 1 d DU . O2B O 0.8744(2) 0.9262(2) 0.27708(11) 0.0339(14) Uani 1 d DU . C1B C 0.8638(3) 0.9132(3) 0.2512(2) 0.035(2) Uani 1 d DU . C2B C 0.8421(3) 0.9408(3) 0.23496(14) 0.037(2) Uani 1 d DU . H2B1 H 0.8652(3) 0.9770(3) 0.23756(14) 0.044 Uiso 1 calc R . H2B2 H 0.8102(3) 0.9327(3) 0.24428(14) 0.044 Uiso 1 calc R . N3B N 0.8322(3) 0.9310(3) 0.20292(14) 0.049(2) Uani 1 d DU . C4B C 0.7933(3) 0.8771(3) 0.1976(2) 0.072(3) Uani 1 d DU . H4B1 H 0.7628(3) 0.8689(3) 0.2082(2) 0.108 Uiso 1 calc R . H4B2 H 0.8060(3) 0.8554(3) 0.2041(2) 0.108 Uiso 1 calc R . H4B3 H 0.7858(3) 0.8719(3) 0.1771(2) 0.108 Uiso 1 calc R . C5B C 0.8789(3) 0.9442(4) 0.1870(2) 0.069(3) Uani 1 d DU . H5B1 H 0.9037(3) 0.9792(4) 0.1907(2) 0.104 Uiso 1 calc R . H5B2 H 0.8717(3) 0.9394(4) 0.1665(2) 0.104 Uiso 1 calc R . H5B3 H 0.8919(3) 0.9228(4) 0.1935(2) 0.104 Uiso 1 calc R . C6B C 0.8115(4) 0.9638(4) 0.1927(2) 0.072(3) Uani 1 d DU . H6B1 H 0.7808(4) 0.9551(4) 0.2032(2) 0.108 Uiso 1 calc R . H6B2 H 0.8042(4) 0.9585(4) 0.1721(2) 0.108 Uiso 1 calc R . H6B3 H 0.8362(4) 0.9990(4) 0.1961(2) 0.108 Uiso 1 calc R . O1C O 0.9969(2) 0.8373(2) 0.29062(13) 0.041(2) Uani 1 d DU . O2C O 0.9330(2) 0.7943(2) 0.25972(14) 0.056(2) Uani 1 d DU . C1C C 0.9661(3) 0.7991(3) 0.2770(2) 0.038(2) Uani 1 d DU . C2C C 0.9659(3) 0.7502(3) 0.2828(2) 0.056(3) Uani 1 d DU . H2C1 H 0.9334(3) 0.7265(3) 0.2916(2) 0.067 Uiso 1 calc R . H2C2 H 0.9674(3) 0.7360(3) 0.2641(2) 0.067 Uiso 1 calc R . N3C N 1.0068(3) 0.7517(2) 0.3017(2) 0.050(2) Uani 1 d DU . C4C C 0.9991(4) 0.6988(3) 0.3036(2) 0.078(4) Uani 1 d DU . H4C1 H 0.9656(4) 0.6760(3) 0.3111(2) 0.118 Uiso 1 calc R . H4C2 H 1.0242(4) 0.6989(3) 0.3164(2) 0.118 Uiso 1 calc R . H4C3 H 1.0025(4) 0.6877(3) 0.2845(2) 0.118 Uiso 1 calc R . C5C C 1.0575(3) 0.7857(4) 0.2902(2) 0.081(4) Uani 1 d DU . H5C1 H 1.0603(3) 0.7751(4) 0.2709(2) 0.122 Uiso 1 calc R . H5C2 H 1.0825(3) 0.7846(4) 0.3027(2) 0.122 Uiso 1 calc R . H5C3 H 1.0633(3) 0.8199(4) 0.2896(2) 0.122 Uiso 1 calc R . C6C C 1.0016(4) 0.7673(4) 0.3315(2) 0.069(3) Uani 1 d DU . H6C1 H 0.9679(4) 0.7445(4) 0.3388(2) 0.104 Uiso 1 calc R . H6C2 H 1.0072(4) 0.8014(4) 0.3311(2) 0.104 Uiso 1 calc R . H6C3 H 1.0263(4) 0.7661(4) 0.3442(2) 0.104 Uiso 1 calc R . Ni4 Ni 1.0000 1.0000 0.39931(6) 0.0326(6) Uani 1 d SU . N13 N 1.0490(2) 1.0659(2) 0.42094(12) 0.033(2) Uani 1 d DU . C23 C 1.0864(3) 1.0745(3) 0.4019(2) 0.043(2) Uani 1 d DU . C33 C 1.1358(3) 1.1128(3) 0.4075(2) 0.062(3) Uani 1 d DU . H33 H 1.1612(3) 1.1200(3) 0.3938(2) 0.074 Uiso 1 calc R . C43 C 1.1473(3) 1.1395(4) 0.4322(2) 0.068(3) Uani 1 d DU . H43 H 1.1810(3) 1.1635(4) 0.4364(2) 0.081 Uiso 1 calc R . C53 C 1.1089(3) 1.1314(3) 0.4515(2) 0.065(3) Uani 1 d DU . H53 H 1.1155(3) 1.1501(3) 0.4687(2) 0.078 Uiso 1 calc R . C63 C 1.0607(3) 1.0944(3) 0.4440(2) 0.045(2) Uani 1 d DU . O23 O 1.0717(2) 1.0440(2) 0.37979(12) 0.045(2) Uani 1 d DU . Cl3 Cl 1.01076(11) 1.08038(12) 0.46732(6) 0.0725(9) Uani 1 d DU . Ni5 Ni 1.03769(6) 0.70342(7) 0.21159(4) 0.0546(5) Uani 1 d U . N14 N 1.1091(2) 0.7348(2) 0.1957(2) 0.061(2) Uani 1 d DU . C24 C 1.1226(3) 0.7801(3) 0.2080(2) 0.061(2) Uani 1 d DU . C34 C 1.1715(3) 0.8209(3) 0.2045(3) 0.080(4) Uani 1 d DU . H34 H 1.1800(3) 0.8525(3) 0.2122(3) 0.096 Uiso 1 calc R . C44 C 1.2063(3) 0.8151(3) 0.1902(3) 0.092(4) Uani 1 d DU . H44 H 1.2392(3) 0.8425(3) 0.1881(3) 0.110 Uiso 1 calc R . C54 C 1.1934(3) 0.7681(3) 0.1784(3) 0.095(4) Uani 1 d DU . H54 H 1.2171(3) 0.7627(3) 0.1685(3) 0.114 Uiso 1 calc R . C64 C 1.1441(3) 0.7299(3) 0.1819(3) 0.084(4) Uani 1 d DU . O24 O 1.0862(2) 0.7810(2) 0.2221(2) 0.070(2) Uani 1 d DU . Cl4 Cl 1.12474(14) 0.6697(2) 0.16883(12) 0.141(2) Uani 1 d DU . N15 N 1.0030(3) 0.7188(4) 0.1790(2) 0.082(2) Uani 1 d DU . C25 C 0.9650(4) 0.7114(5) 0.1969(2) 0.097(3) Uani 1 d DU . C35 C 0.9257(5) 0.7185(7) 0.1868(3) 0.160(6) Uani 1 d DU . H35 H 0.8999(5) 0.7143(7) 0.1995(3) 0.192 Uiso 1 calc R . C45 C 0.9250(6) 0.7314(8) 0.1591(3) 0.185(7) Uani 1 d DU . H45 H 0.8988(6) 0.7364(8) 0.1523(3) 0.223 Uiso 1 calc R . C55 C 0.9636(5) 0.7374(7) 0.1403(2) 0.172(6) Uani 1 d DU . H55 H 0.9629(5) 0.7440(7) 0.1205(2) 0.206 Uiso 1 calc R . C65 C 1.0025(4) 0.7332(5) 0.1522(2) 0.111(4) Uani 1 d DU . O25 O 0.9689(3) 0.6983(4) 0.2234(2) 0.104(3) Uani 1 d DU . Cl5 Cl 1.0520(2) 0.7396(2) 0.13077(10) 0.183(2) Uani 1 d DU . N16 N 1.0125(3) 0.6272(3) 0.2090(2) 0.055(2) Uani 1 d U . C26 C 1.0279(4) 0.6264(5) 0.2369(3) 0.066(3) Uani 1 d U . C36 C 1.0267(6) 0.5824(5) 0.2489(3) 0.105(5) Uani 1 d U . H36 H 1.0407(6) 0.5824(5) 0.2670(3) 0.126 Uiso 1 calc R . C46 C 1.0036(6) 0.5411(5) 0.2318(3) 0.114(5) Uani 1 d U . H46 H 0.9994(6) 0.5106(5) 0.2392(3) 0.137 Uiso 1 calc R . C56 C 0.9854(5) 0.5405(5) 0.2035(3) 0.093(4) Uani 1 d U . H56 H 0.9699(5) 0.5113(5) 0.1920(3) 0.112 Uiso 1 calc R . C66 C 0.9918(4) 0.5835(4) 0.1949(3) 0.064(3) Uani 1 d U . O26 O 1.0494(3) 0.6702(3) 0.2482(2) 0.070(2) Uani 1 d U . Cl6 Cl 0.97132(14) 0.58729(13) 0.15984(7) 0.0890(11) Uani 1 d U . N17 N 0.0096(2) 0.5543(3) 0.0423(2) 0.062(2) Uani 1 d DU . C27 C -0.0372(3) 0.5189(4) 0.0330(2) 0.066(3) Uani 1 d DU . C37 C -0.0803(3) 0.5124(4) 0.0475(2) 0.076(3) Uani 1 d DU . H37 H -0.1124(3) 0.4875(4) 0.0411(2) 0.091 Uiso 1 calc R . C47 C -0.0765(3) 0.5412(4) 0.0702(2) 0.075(3) Uani 1 d DU . H47 H -0.1057(3) 0.5376(4) 0.0792(2) 0.091 Uiso 1 calc R . C57 C -0.0286(3) 0.5768(4) 0.0804(2) 0.081(3) Uani 1 d DU . H57 H -0.0244(3) 0.5962(4) 0.0970(2) 0.098 Uiso 1 calc R . C67 C 0.0121(3) 0.5819(4) 0.0648(2) 0.074(3) Uani 1 d DU . O27 O -0.0390(2) 0.4936(3) 0.0099(2) 0.076(2) Uani 1 d DU . H27 H -0.0099(2) 0.5025(3) 0.0044(2) 0.114 Uiso 0.50 calc PR . Cl7 Cl 0.07280(11) 0.62561(14) 0.07640(8) 0.1003(12) Uani 1 d DU . Cl8 Cl 0.0000 0.0000 0.1487(5) 0.146(7) Uani 0.50 d SP . 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 0.0261(8) 0.0254(8) 0.0347(8) 0.0007(7) 0.0016(7) 0.0126(7) Ni2 0.0258(8) 0.0253(8) 0.0313(8) -0.0021(7) -0.0020(7) 0.0133(7) Ni3 0.0377(9) 0.0393(9) 0.0419(9) -0.0137(8) -0.0108(8) 0.0228(8) O1 0.028(3) 0.031(3) 0.035(3) 0.004(3) 0.008(3) 0.016(3) O2 0.034(3) 0.031(3) 0.030(3) -0.002(3) 0.001(3) 0.021(3) O10 0.025(3) 0.026(3) 0.037(3) 0.001(3) -0.002(3) 0.011(2) C10 0.031(4) 0.031(4) 0.014(7) 0.000 0.000 0.015(2) Cl 0.057(2) 0.057(2) 0.068(3) 0.000 0.000 0.0285(9) N11 0.030(4) 0.031(4) 0.055(5) 0.006(4) 0.006(4) 0.005(3) C21 0.047(6) 0.032(5) 0.055(6) -0.001(4) -0.002(5) 0.014(4) C31 0.154(14) 0.048(7) 0.179(16) 0.036(9) -0.110(12) -0.026(8) C41 0.211(17) 0.047(7) 0.201(17) 0.042(10) -0.142(14) -0.043(10) C51 0.118(11) 0.032(5) 0.134(12) 0.027(7) -0.053(9) 0.005(6) C61 0.063(7) 0.036(5) 0.064(7) 0.001(5) -0.009(5) 0.021(5) O21 0.046(4) 0.027(3) 0.056(4) -0.002(3) -0.007(3) 0.016(3) Cl1 0.082(2) 0.058(2) 0.066(2) 0.018(2) -0.002(2) 0.019(2) N12 0.064(5) 0.076(6) 0.094(6) -0.038(5) -0.028(4) 0.048(4) C22 0.109(9) 0.098(9) 0.064(5) -0.019(5) -0.002(5) 0.068(6) C32 0.143(11) 0.131(12) 0.072(5) -0.034(7) -0.032(7) 0.098(9) C42 0.144(14) 0.175(17) 0.095(9) -0.023(9) -0.030(7) 0.102(11) C52 0.109(11) 0.163(14) 0.119(7) -0.071(9) -0.036(7) 0.092(9) C62 0.075(7) 0.123(9) 0.091(7) -0.035(6) -0.035(6) 0.076(5) O22 0.087(5) 0.093(6) 0.048(4) -0.013(4) 0.000(4) 0.065(4) Cl2 0.098(3) 0.095(3) 0.179(5) -0.044(3) -0.027(3) 0.031(2) O1A 0.036(3) 0.034(3) 0.038(4) 0.003(3) -0.004(3) 0.021(3) O2A 0.029(3) 0.033(3) 0.046(4) 0.002(3) -0.007(3) 0.016(3) C1A 0.025(4) 0.039(5) 0.029(5) 0.003(4) 0.001(4) 0.019(4) C2A 0.042(5) 0.035(5) 0.035(5) 0.000(4) -0.007(4) 0.020(4) N3A 0.035(4) 0.045(5) 0.041(5) -0.001(4) -0.011(3) 0.023(4) C4A 0.036(5) 0.045(6) 0.059(6) -0.004(5) -0.011(5) 0.016(5) C5A 0.063(7) 0.055(6) 0.053(7) -0.028(5) -0.015(6) 0.028(6) C6A 0.068(7) 0.069(7) 0.061(7) 0.009(6) -0.029(6) 0.039(6) O1B 0.040(4) 0.044(4) 0.037(4) -0.010(3) -0.006(3) 0.024(3) O2B 0.030(3) 0.039(4) 0.036(3) -0.007(3) -0.008(3) 0.020(3) C1B 0.029(5) 0.040(5) 0.038(5) 0.002(4) 0.001(4) 0.018(4) C2B 0.031(5) 0.041(5) 0.042(4) -0.005(4) -0.011(4) 0.021(4) N3B 0.051(5) 0.059(5) 0.042(4) 0.000(4) -0.017(4) 0.032(4) C4B 0.080(7) 0.062(6) 0.068(8) -0.030(6) -0.032(7) 0.032(5) C5B 0.066(6) 0.111(10) 0.042(6) 0.002(7) -0.005(5) 0.053(7) C6B 0.089(9) 0.083(7) 0.065(8) 0.004(7) -0.020(7) 0.059(7) O1C 0.046(4) 0.031(3) 0.046(4) -0.009(3) -0.009(3) 0.019(3) O2C 0.067(5) 0.045(4) 0.069(5) -0.038(3) -0.033(4) 0.038(4) C1C 0.043(5) 0.031(4) 0.045(6) -0.004(4) -0.002(4) 0.022(4) C2C 0.066(6) 0.041(5) 0.066(7) -0.008(5) -0.007(6) 0.032(5) N3C 0.070(5) 0.042(5) 0.052(5) -0.002(4) 0.006(4) 0.039(4) C4C 0.122(10) 0.052(6) 0.085(9) -0.015(6) -0.027(8) 0.062(7) C5C 0.066(6) 0.092(8) 0.103(10) 0.034(9) 0.020(7) 0.052(6) C6C 0.119(10) 0.060(7) 0.047(6) 0.007(6) 0.009(6) 0.059(8) Ni4 0.0332(9) 0.0332(9) 0.0312(14) 0.000 0.000 0.0166(4) N13 0.041(4) 0.027(4) 0.032(4) -0.001(3) -0.005(3) 0.019(3) C23 0.040(5) 0.034(5) 0.038(5) 0.006(4) 0.003(4) 0.005(4) C33 0.042(5) 0.057(7) 0.057(6) 0.005(5) 0.009(5) 0.002(4) C43 0.054(6) 0.061(7) 0.062(7) -0.004(6) -0.013(5) 0.010(6) C53 0.071(6) 0.050(6) 0.054(7) -0.019(6) -0.018(5) 0.016(5) C63 0.061(5) 0.036(5) 0.037(5) 0.005(4) 0.004(4) 0.023(4) O23 0.049(4) 0.046(4) 0.039(4) 0.000(3) 0.012(3) 0.022(3) Cl3 0.078(2) 0.083(2) 0.056(2) -0.020(2) 0.007(2) 0.040(2) Ni5 0.0525(11) 0.0676(12) 0.0487(11) -0.0162(10) -0.0059(9) 0.0338(10) N14 0.053(4) 0.066(5) 0.059(6) -0.005(4) -0.001(4) 0.026(4) C24 0.071(4) 0.060(5) 0.055(7) 0.000(5) -0.015(5) 0.034(4) C34 0.071(6) 0.059(6) 0.102(11) 0.017(7) -0.012(7) 0.027(5) C44 0.074(8) 0.080(7) 0.105(12) 0.029(8) 0.003(7) 0.026(7) C54 0.068(7) 0.106(8) 0.103(11) 0.016(9) 0.021(8) 0.039(6) C64 0.065(6) 0.105(7) 0.079(9) -0.022(8) 0.001(7) 0.041(6) O24 0.081(4) 0.065(4) 0.080(6) -0.017(4) -0.023(4) 0.048(4) Cl4 0.089(3) 0.138(4) 0.183(5) -0.076(4) 0.030(3) 0.047(3) N15 0.099(6) 0.073(6) 0.097(6) -0.037(5) -0.045(5) 0.060(6) C25 0.079(6) 0.077(8) 0.160(9) -0.059(9) -0.049(7) 0.058(7) C35 0.128(11) 0.136(14) 0.267(16) -0.072(15) -0.084(12) 0.106(11) C45 0.165(14) 0.122(14) 0.318(20) -0.036(18) -0.133(13) 0.107(15) C55 0.176(15) 0.117(13) 0.206(15) -0.009(14) -0.131(10) 0.062(15) C65 0.129(10) 0.079(9) 0.119(8) -0.028(9) -0.088(6) 0.048(9) O25 0.074(4) 0.128(8) 0.131(7) -0.045(7) 0.001(6) 0.067(5) Cl5 0.237(6) 0.236(6) 0.081(3) 0.028(4) -0.017(4) 0.121(6) N16 0.050(5) 0.064(4) 0.051(5) -0.012(4) -0.014(4) 0.029(4) C26 0.049(6) 0.062(5) 0.061(6) -0.002(4) -0.016(6) 0.008(5) C36 0.130(12) 0.079(7) 0.072(9) 0.010(6) -0.042(9) 0.025(9) C46 0.170(15) 0.074(8) 0.093(10) 0.009(7) -0.034(10) 0.057(10) C56 0.111(11) 0.057(6) 0.087(9) -0.001(7) -0.028(9) 0.024(8) C66 0.061(7) 0.058(5) 0.060(6) -0.007(5) -0.013(6) 0.019(6) O26 0.053(4) 0.075(4) 0.057(4) -0.008(3) -0.018(4) 0.012(4) Cl6 0.117(3) 0.106(3) 0.071(2) -0.034(2) -0.043(2) 0.076(2) N17 0.045(5) 0.058(6) 0.061(6) 0.013(4) -0.014(4) 0.009(4) C27 0.051(6) 0.063(7) 0.068(7) -0.001(6) -0.016(5) 0.017(6) C37 0.052(6) 0.086(9) 0.080(8) 0.017(6) -0.001(6) 0.026(6) C47 0.053(6) 0.102(10) 0.067(8) 0.028(6) 0.008(6) 0.036(6) C57 0.071(6) 0.099(9) 0.069(8) 0.017(7) -0.009(6) 0.039(7) C67 0.047(5) 0.088(9) 0.059(7) 0.003(6) -0.021(5) 0.013(6) O27 0.048(4) 0.080(6) 0.086(6) -0.018(5) -0.022(4) 0.022(4) Cl7 0.061(2) 0.113(3) 0.095(3) -0.036(2) -0.023(2) 0.019(2) Cl8 0.120(7) 0.120(7) 0.198(20) 0.000 0.000 0.060(4) _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 O1A 2.010(5) . ? Ni1 O2 2.017(5) 2_765 ? Ni1 O1 2.053(6) . ? Ni1 O10 2.057(5) . ? Ni1 O2B 2.073(5) 2_765 ? Ni1 O21 2.073(5) 2_765 ? Ni1 Ni2 2.933(2) 2_765 ? Ni1 Ni3 2.996(2) 2_765 ? Ni2 O2 1.987(5) . ? Ni2 O1C 2.005(5) . ? Ni2 O2A 2.022(5) . ? Ni2 O10 2.076(5) . ? Ni2 O1 2.077(6) 3_675 ? Ni2 O2B 2.104(5) 2_765 ? Ni2 Ni1 2.933(2) 3_675 ? Ni3 O22 2.000(7) . ? Ni3 O2 2.026(6) . ? Ni3 O2C 2.030(6) . ? Ni3 O21 2.085(6) . ? Ni3 O1B 2.097(5) . ? Ni3 N12 2.232(7) . ? Ni3 C22 2.498(8) . ? Ni3 Ni1 2.996(2) 3_675 ? O1 Ni2 2.077(6) 2_765 ? O2 Ni1 2.017(5) 3_675 ? O10 C10 1.296(5) . ? C10 O10 1.296(5) 2_765 ? C10 O10 1.296(5) 3_675 ? N11 C61 1.323(7) . ? N11 C21 1.351(7) . ? C21 O21 1.304(7) . ? C21 C31 1.410(8) . ? C31 C41 1.337(9) . ? C41 C51 1.394(9) . ? C51 C61 1.377(8) . ? C61 Cl1 1.734(7) . ? O21 Ni1 2.073(5) 3_675 ? N12 C62 1.317(7) . ? N12 C22 1.369(8) . ? C22 O22 1.324(7) . ? C22 C32 1.388(8) . ? C32 C42 1.338(9) . ? C42 C52 1.407(9) . ? C52 C62 1.381(8) . ? C62 Cl2 1.741(7) . ? O1A C1A 1.254(7) . ? O2A C1A 1.243(7) . ? C1A C2A 1.509(8) . ? C2A N3A 1.505(7) . ? N3A C5A 1.481(8) . ? N3A C6A 1.497(8) . ? N3A C4A 1.505(8) . ? O1B C1B 1.246(7) . ? O2B C1B 1.253(7) . ? O2B Ni1 2.073(5) 3_675 ? O2B Ni2 2.104(5) 3_675 ? C1B C2B 1.507(8) . ? C2B N3B 1.511(8) . ? N3B C5B 1.473(8) . ? N3B C4B 1.496(8) . ? N3B C6B 1.506(8) . ? O1C C1C 1.245(7) . ? O2C C1C 1.238(7) . ? C1C C2C 1.518(8) . ? C2C N3C 1.505(8) . ? N3C C5C 1.469(8) . ? N3C C6C 1.495(8) . ? N3C C4C 1.517(8) . ? Ni4 N13 2.072(6) . ? Ni4 N13 2.072(6) 2_765 ? Ni4 N13 2.072(6) 3_675 ? Ni4 O23 2.118(6) 3_675 ? Ni4 O23 2.118(6) 2_765 ? Ni4 O23 2.118(6) . ? Ni4 C23 2.486(7) . ? Ni4 C23 2.486(7) 3_675 ? Ni4 C23 2.486(7) 2_765 ? N13 C63 1.311(7) . ? N13 C23 1.362(7) . ? C23 O23 1.302(7) . ? C23 C33 1.397(8) . ? C33 C43 1.344(9) . ? C43 C53 1.396(9) . ? C53 C63 1.379(8) . ? C63 Cl3 1.738(6) . ? Ni5 N15 2.027(7) . ? Ni5 N14 2.034(7) . ? Ni5 N16 2.063(9) . ? Ni5 O26 2.093(8) . ? Ni5 O25 2.103(7) . ? Ni5 O24 2.133(7) . ? Ni5 C25 2.454(9) . ? Ni5 C24 2.488(8) . ? Ni5 C26 2.513(13) . ? N14 C64 1.315(7) . ? N14 C24 1.359(7) . ? C24 O24 1.301(7) . ? C24 C34 1.398(8) . ? C34 C44 1.338(9) . ? C44 C54 1.399(9) . ? C54 C64 1.380(8) . ? C64 Cl4 1.739(7) . ? N15 C65 1.317(8) . ? N15 C25 1.353(8) . ? C25 O25 1.312(7) . ? C25 C35 1.402(8) . ? C35 C45 1.345(9) . ? C45 C55 1.403(10) . ? C55 C65 1.375(8) . ? C65 Cl5 1.737(7) . ? N16 C66 1.327(13) . ? N16 C26 1.380(14) . ? C26 O26 1.271(12) . ? C26 C36 1.44(2) . ? C36 C46 1.35(2) . ? C46 C56 1.42(2) . ? C56 C66 1.29(2) . ? C66 Cl6 1.762(12) . ? N17 C67 1.318(7) . ? N17 C27 1.363(7) . ? C27 O27 1.304(7) . ? C27 C37 1.401(8) . ? C37 C47 1.337(9) . ? C47 C57 1.399(9) . ? C57 C67 1.378(8) . ? C67 Cl7 1.743(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 O1A Ni1 O2 170.4(2) . 2_765 ? O1A Ni1 O1 88.6(2) . . ? O2 Ni1 O1 84.9(2) 2_765 . ? O1A Ni1 O10 94.7(2) . . ? O2 Ni1 O10 92.7(2) 2_765 . ? O1 Ni1 O10 93.3(2) . . ? O1A Ni1 O2B 93.0(2) . 2_765 ? O2 Ni1 O2B 94.2(2) 2_765 2_765 ? O1 Ni1 O2B 173.3(2) . 2_765 ? O10 Ni1 O2B 80.1(2) . 2_765 ? O1A Ni1 O21 90.4(2) . 2_765 ? O2 Ni1 O21 82.5(2) 2_765 2_765 ? O1 Ni1 O21 89.8(2) . 2_765 ? O10 Ni1 O21 174.1(2) . 2_765 ? O2B Ni1 O21 96.7(2) 2_765 2_765 ? O1A Ni1 Ni2 132.9(2) . 2_765 ? O2 Ni1 Ni2 42.5(2) 2_765 2_765 ? O1 Ni1 Ni2 45.1(2) . 2_765 ? O10 Ni1 Ni2 82.12(15) . 2_765 ? O2B Ni1 Ni2 131.9(2) 2_765 2_765 ? O21 Ni1 Ni2 96.6(2) 2_765 2_765 ? O1A Ni1 Ni3 132.8(2) . 2_765 ? O2 Ni1 Ni3 42.3(2) 2_765 2_765 ? O1 Ni1 Ni3 100.6(2) . 2_765 ? O10 Ni1 Ni3 130.2(2) . 2_765 ? O2B Ni1 Ni3 83.09(15) 2_765 2_765 ? O21 Ni1 Ni3 44.1(2) 2_765 2_765 ? Ni2 Ni1 Ni3 75.22(5) 2_765 2_765 ? O2 Ni2 O1C 92.7(2) . . ? O2 Ni2 O2A 170.4(2) . . ? O1C Ni2 O2A 83.5(2) . . ? O2 Ni2 O10 91.7(2) . . ? O1C Ni2 O10 174.3(2) . . ? O2A Ni2 O10 92.6(2) . . ? O2 Ni2 O1 85.0(2) . 3_675 ? O1C Ni2 O1 94.7(2) . 3_675 ? O2A Ni2 O1 86.5(2) . 3_675 ? O10 Ni2 O1 89.2(2) . 3_675 ? O2 Ni2 O2B 98.7(2) . 2_765 ? O1C Ni2 O2B 96.9(2) . 2_765 ? O2A Ni2 O2B 90.6(2) . 2_765 ? O10 Ni2 O2B 78.9(2) . 2_765 ? O1 Ni2 O2B 167.6(2) 3_675 2_765 ? O2 Ni2 Ni1 43.3(2) . 3_675 ? O1C Ni2 Ni1 107.0(2) . 3_675 ? O2A Ni2 Ni1 129.6(2) . 3_675 ? O10 Ni2 Ni1 78.69(15) . 3_675 ? O1 Ni2 Ni1 44.4(2) 3_675 3_675 ? O2B Ni2 Ni1 134.4(2) 2_765 3_675 ? O22 Ni3 O2 97.2(2) . . ? O22 Ni3 O2C 96.5(3) . . ? O2 Ni3 O2C 97.5(2) . . ? O22 Ni3 O21 173.5(3) . . ? O2 Ni3 O21 82.0(2) . . ? O2C Ni3 O21 90.0(3) . . ? O22 Ni3 O1B 85.6(3) . . ? O2 Ni3 O1B 91.3(2) . . ? O2C Ni3 O1B 170.6(2) . . ? O21 Ni3 O1B 88.0(2) . . ? O22 Ni3 N12 64.7(2) . . ? O2 Ni3 N12 160.6(3) . . ? O2C Ni3 N12 91.8(3) . . ? O21 Ni3 N12 115.2(2) . . ? O1B Ni3 N12 80.7(3) . . ? O22 Ni3 C22 31.8(2) . . ? O2 Ni3 C22 128.2(3) . . ? O2C Ni3 C22 97.2(4) . . ? O21 Ni3 C22 147.2(3) . . ? O1B Ni3 C22 79.8(3) . . ? N12 Ni3 C22 33.0(2) . . ? O22 Ni3 Ni1 133.0(2) . 3_675 ? O2 Ni3 Ni1 42.07(15) . 3_675 ? O2C Ni3 Ni1 109.0(2) . 3_675 ? O21 Ni3 Ni1 43.76(15) . 3_675 ? O1B Ni3 Ni1 75.6(2) . 3_675 ? N12 Ni3 Ni1 148.1(2) . 3_675 ? C22 Ni3 Ni1 152.7(3) . 3_675 ? Ni1 O1 Ni2 90.5(2) . 2_765 ? Ni2 O2 Ni1 94.2(2) . 3_675 ? Ni2 O2 Ni3 128.7(3) . . ? Ni1 O2 Ni3 95.6(2) 3_675 . ? C10 O10 Ni1 127.2(4) . . ? C10 O10 Ni2 130.3(4) . . ? Ni1 O10 Ni2 96.2(2) . . ? O10 C10 O10 119.97(5) . 2_765 ? O10 C10 O10 119.97(5) . 3_675 ? O10 C10 O10 119.97(5) 2_765 3_675 ? C61 N11 C21 118.3(5) . . ? O21 C21 N11 117.8(6) . . ? O21 C21 C31 122.7(6) . . ? N11 C21 C31 119.5(6) . . ? C41 C31 C21 120.4(7) . . ? C31 C41 C51 119.3(8) . . ? C61 C51 C41 116.4(7) . . ? N11 C61 C51 124.8(6) . . ? N11 C61 Cl1 116.2(5) . . ? C51 C61 Cl1 119.0(6) . . ? C21 O21 Ni1 130.2(5) . 3_675 ? C21 O21 Ni3 125.5(6) . . ? Ni1 O21 Ni3 92.2(2) 3_675 . ? C62 N12 C22 116.5(6) . . ? C62 N12 Ni3 158.2(6) . . ? C22 N12 Ni3 84.2(4) . . ? O22 C22 N12 115.3(6) . . ? O22 C22 C32 124.5(7) . . ? N12 C22 C32 120.1(7) . . ? O22 C22 Ni3 52.9(4) . . ? N12 C22 Ni3 62.7(4) . . ? C32 C22 Ni3 170.1(11) . . ? C42 C32 C22 122.2(8) . . ? C32 C42 C52 118.6(7) . . ? C62 C52 C42 115.9(7) . . ? N12 C62 C52 126.6(7) . . ? N12 C62 Cl2 114.9(6) . . ? C52 C62 Cl2 118.5(6) . . ? C22 O22 Ni3 95.3(5) . . ? C1A O1A Ni1 126.7(5) . . ? C1A O2A Ni2 129.9(5) . . ? O2A C1A O1A 127.3(6) . . ? O2A C1A C2A 113.1(6) . . ? O1A C1A C2A 119.6(6) . . ? N3A C2A C1A 118.7(5) . . ? C5A N3A C6A 109.6(6) . . ? C5A N3A C4A 109.2(6) . . ? C6A N3A C4A 108.8(6) . . ? C5A N3A C2A 111.2(5) . . ? C6A N3A C2A 107.3(5) . . ? C4A N3A C2A 110.6(5) . . ? C1B O1B Ni3 131.2(5) . . ? C1B O2B Ni1 122.7(5) . 3_675 ? C1B O2B Ni2 137.0(5) . 3_675 ? Ni1 O2B Ni2 94.9(2) 3_675 3_675 ? O1B C1B O2B 126.4(7) . . ? O1B C1B C2B 119.1(6) . . ? O2B C1B C2B 114.5(6) . . ? C1B C2B N3B 118.5(5) . . ? C5B N3B C4B 110.4(6) . . ? C5B N3B C6B 109.5(6) . . ? C4B N3B C6B 108.4(6) . . ? C5B N3B C2B 111.3(6) . . ? C4B N3B C2B 110.5(6) . . ? C6B N3B C2B 106.6(6) . . ? C1C O1C Ni2 139.6(5) . . ? C1C O2C Ni3 130.6(5) . . ? O2C C1C O1C 128.8(6) . . ? O2C C1C C2C 113.4(6) . . ? O1C C1C C2C 117.7(6) . . ? N3C C2C C1C 118.6(5) . . ? C5C N3C C6C 110.4(7) . . ? C5C N3C C2C 112.4(6) . . ? C6C N3C C2C 109.0(6) . . ? C5C N3C C4C 108.8(6) . . ? C6C N3C C4C 107.5(6) . . ? C2C N3C C4C 108.5(6) . . ? N13 Ni4 N13 98.7(2) . 2_765 ? N13 Ni4 N13 98.7(2) . 3_675 ? N13 Ni4 N13 98.7(2) 2_765 3_675 ? N13 Ni4 O23 159.0(2) . 3_675 ? N13 Ni4 O23 96.4(2) 2_765 3_675 ? N13 Ni4 O23 64.6(2) 3_675 3_675 ? N13 Ni4 O23 96.4(2) . 2_765 ? N13 Ni4 O23 64.6(2) 2_765 2_765 ? N13 Ni4 O23 159.0(2) 3_675 2_765 ? O23 Ni4 O23 103.2(2) 3_675 2_765 ? N13 Ni4 O23 64.6(2) . . ? N13 Ni4 O23 159.0(2) 2_765 . ? N13 Ni4 O23 96.4(2) 3_675 . ? O23 Ni4 O23 103.2(2) 3_675 . ? O23 Ni4 O23 103.2(2) 2_765 . ? N13 Ni4 C23 33.2(2) . . ? N13 Ni4 C23 131.5(3) 2_765 . ? N13 Ni4 C23 96.0(3) 3_675 . ? O23 Ni4 C23 131.4(2) 3_675 . ? O23 Ni4 C23 104.6(3) 2_765 . ? O23 Ni4 C23 31.6(2) . . ? N13 Ni4 C23 131.5(3) . 3_675 ? N13 Ni4 C23 96.0(3) 2_765 3_675 ? N13 Ni4 C23 33.2(2) 3_675 3_675 ? O23 Ni4 C23 31.6(2) 3_675 3_675 ? O23 Ni4 C23 131.4(2) 2_765 3_675 ? O23 Ni4 C23 104.6(3) . 3_675 ? C23 Ni4 C23 119.77(3) . 3_675 ? N13 Ni4 C23 96.0(3) . 2_765 ? N13 Ni4 C23 33.2(2) 2_765 2_765 ? N13 Ni4 C23 131.5(3) 3_675 2_765 ? O23 Ni4 C23 104.6(3) 3_675 2_765 ? O23 Ni4 C23 31.6(2) 2_765 2_765 ? O23 Ni4 C23 131.4(2) . 2_765 ? C23 Ni4 C23 119.77(3) . 2_765 ? C23 Ni4 C23 119.77(3) 3_675 2_765 ? C63 N13 C23 118.4(5) . . ? C63 N13 Ni4 149.9(5) . . ? C23 N13 Ni4 90.3(4) . . ? O23 C23 N13 114.3(5) . . ? O23 C23 C33 126.0(6) . . ? N13 C23 C33 119.6(6) . . ? O23 C23 Ni4 58.4(3) . . ? N13 C23 Ni4 56.5(3) . . ? C33 C23 Ni4 170.7(7) . . ? C43 C33 C23 120.8(7) . . ? C33 C43 C53 119.6(7) . . ? C63 C53 C43 116.5(6) . . ? N13 C63 C53 125.0(6) . . ? N13 C63 Cl3 115.2(5) . . ? C53 C63 Cl3 119.7(5) . . ? C23 O23 Ni4 90.0(4) . . ? N15 Ni5 N14 100.7(3) . . ? N15 Ni5 N16 106.0(4) . . ? N14 Ni5 N16 102.6(3) . . ? N15 Ni5 O26 161.5(3) . . ? N14 Ni5 O26 96.7(3) . . ? N16 Ni5 O26 63.6(3) . . ? N15 Ni5 O25 65.8(3) . . ? N14 Ni5 O25 158.1(3) . . ? N16 Ni5 O25 97.9(4) . . ? O26 Ni5 O25 99.4(3) . . ? N15 Ni5 O24 93.7(3) . . ? N14 Ni5 O24 64.6(2) . . ? N16 Ni5 O24 158.6(3) . . ? O26 Ni5 O24 99.5(3) . . ? O25 Ni5 O24 97.9(3) . . ? N15 Ni5 C25 33.5(2) . . ? N14 Ni5 C25 131.9(4) . . ? N16 Ni5 C25 104.6(4) . . ? O26 Ni5 C25 131.0(3) . . ? O25 Ni5 C25 32.3(2) . . ? O24 Ni5 C25 96.5(4) . . ? N15 Ni5 C24 98.8(4) . . ? N14 Ni5 C24 33.1(2) . . ? N16 Ni5 C24 133.4(3) . . ? O26 Ni5 C24 99.2(3) . . ? O25 Ni5 C24 128.5(3) . . ? O24 Ni5 C24 31.5(2) . . ? C25 Ni5 C24 117.4(4) . . ? N15 Ni5 C26 137.1(4) . . ? N14 Ni5 C26 101.9(4) . . ? N16 Ni5 C26 33.3(3) . . ? O26 Ni5 C26 30.3(3) . . ? O25 Ni5 C26 99.5(4) . . ? O24 Ni5 C26 128.9(3) . . ? C25 Ni5 C26 122.3(4) . . ? C24 Ni5 C26 119.6(3) . . ? C64 N14 C24 117.9(6) . . ? C64 N14 Ni5 149.8(5) . . ? C24 N14 Ni5 92.1(4) . . ? O24 C24 N14 113.8(6) . . ? O24 C24 C34 125.8(7) . . ? N14 C24 C34 120.4(6) . . ? O24 C24 Ni5 59.0(4) . . ? N14 C24 Ni5 54.8(3) . . ? C34 C24 Ni5 175.2(6) . . ? C44 C34 C24 120.5(7) . . ? C34 C44 C54 119.7(7) . . ? C64 C54 C44 116.7(7) . . ? N14 C64 C54 124.7(7) . . ? N14 C64 Cl4 115.1(5) . . ? C54 C64 Cl4 120.2(6) . . ? C24 O24 Ni5 89.5(4) . . ? C65 N15 C25 118.4(6) . . ? C65 N15 Ni5 150.7(5) . . ? C25 N15 Ni5 90.9(4) . . ? O25 C25 N15 114.6(6) . . ? O25 C25 C35 125.0(7) . . ? N15 C25 C35 120.3(7) . . ? O25 C25 Ni5 59.0(4) . . ? N15 C25 Ni5 55.7(4) . . ? C35 C25 Ni5 175.6(7) . . ? C45 C35 C25 120.2(8) . . ? C35 C45 C55 119.4(7) . . ? C65 C55 C45 116.9(7) . . ? N15 C65 C55 124.4(7) . . ? N15 C65 Cl5 114.6(6) . . ? C55 C65 Cl5 120.5(6) . . ? C25 O25 Ni5 88.7(5) . . ? C66 N16 C26 115.9(10) . . ? C66 N16 Ni5 152.6(8) . . ? C26 N16 Ni5 91.5(7) . . ? O26 C26 N16 111.4(11) . . ? O26 C26 C36 126.0(12) . . ? N16 C26 C36 121.8(12) . . ? O26 C26 Ni5 56.3(6) . . ? N16 C26 Ni5 55.2(6) . . ? C36 C26 Ni5 172.9(10) . . ? C46 C36 C26 114.0(12) . . ? C36 C46 C56 124.7(13) . . ? C66 C56 C46 114.4(14) . . ? C56 C66 N16 128.8(13) . . ? C56 C66 Cl6 118.2(10) . . ? N16 C66 Cl6 113.0(9) . . ? C26 O26 Ni5 93.4(7) . . ? C67 N17 C27 117.4(6) . . ? O27 C27 N17 116.5(6) . . ? O27 C27 C37 123.3(7) . . ? N17 C27 C37 120.2(6) . . ? C47 C37 C27 121.0(7) . . ? C37 C47 C57 119.2(7) . . ? C67 C57 C47 116.7(7) . . ? N17 C67 C57 125.3(6) . . ? N17 C67 Cl7 115.7(5) . . ? C57 C67 Cl7 118.9(6) . . ? _refine_diff_density_max 0.608 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.096 data_rh_co4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ; [Co10(OH)6(tpa)6(mhp)6(Hmhp)3(HCO3)3].MeOH.2H2O ; _chemical_formula_sum 'C178 H164 Co10 N9 O39' _chemical_formula_weight 3642.48 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' 'Co' 'Co' 0.3494 0.9721 '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 Rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 19.054(3) _cell_length_b 19.054(3) _cell_length_c 81.851(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 25737(7) _cell_formula_units_Z 6 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11262 _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_type 'Psi Scans' _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.768 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9949 _diffrn_reflns_av_R_equivalents 0.1312 _diffrn_reflns_av_sigmaI/netI 0.1088 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 78 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 20.06 _reflns_number_total 2679 _reflns_number_gt 1620 _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 w=1/[\s^2^(Fo^2^)+(0.1187P)^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 2679 _refine_ls_number_parameters 355 _refine_ls_number_restraints 360 _refine_ls_R_factor_all 0.1299 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.2127 _refine_ls_wR_factor_gt 0.1790 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.008 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.77591(10) 0.32789(10) 0.04693(2) 0.0255(6) Uani 1 d U . . Co2 Co 0.6667 0.3333 0.0833 0.0198(10) Uani 1 d SU . . Co3 Co 0.82884(11) 0.3333 0.0833 0.0229(7) Uani 1 d SU . . O1V O 0.7201(4) 0.2919(4) 0.07030(8) 0.0193(17) Uani 1 d U . . H1V H 0.6890 0.2320 0.0708 0.023 Uiso 1 calc R . . O1A O 0.8287(5) 0.2577(5) 0.04671(10) 0.039(2) Uani 1 d U . . O2A O 0.8637(5) 0.2581(5) 0.07301(10) 0.036(2) Uani 1 d U . . C1A C 0.8606(7) 0.2382(7) 0.05828(16) 0.028(3) Uani 1 d U . . C2A C 0.9036(7) 0.1914(7) 0.05257(15) 0.029(2) Uani 1 d U . . C3A C 0.9912(7) 0.2550(8) 0.04792(14) 0.031(3) Uani 1 d DU . . C4A C 1.0498(8) 0.2315(9) 0.04618(15) 0.052(4) Uani 1 d DU . . H4A H 1.0365 0.1780 0.0486 0.063 Uiso 1 calc R . . C5A C 1.1276(9) 0.2870(11) 0.04085(18) 0.079(5) Uani 1 d DU . . H5A H 1.1660 0.2700 0.0397 0.095 Uiso 1 calc R . . C6A C 1.1493(10) 0.3641(11) 0.0373(2) 0.076(5) Uani 1 d DU . . H6A H 1.2022 0.4008 0.0337 0.091 Uiso 1 calc R . . C7A C 1.0942(9) 0.3872(9) 0.03888(18) 0.059(4) Uani 1 d DU . . H7A H 1.1092 0.4412 0.0365 0.071 Uiso 1 calc R . . C8A C 1.0160(8) 0.3346(9) 0.04388(17) 0.050(4) Uani 1 d DU . . H8A H 0.9787 0.3531 0.0446 0.061 Uiso 1 calc R . . C9A C 0.9065(7) 0.1392(8) 0.06666(15) 0.030(3) Uani 1 d DU . . C10A C 0.8769(7) 0.0567(8) 0.06480(17) 0.047(4) Uani 1 d DU . . H10A H 0.8509 0.0322 0.0549 0.056 Uiso 1 calc R . . C11A C 0.8834(9) 0.0096(9) 0.07631(18) 0.064(4) Uani 1 d DU . . H11A H 0.8629 -0.0461 0.0746 0.077 Uiso 1 calc R . . C12A C 0.9217(9) 0.0470(10) 0.0908(2) 0.064(4) Uani 1 d DU . . H12A H 0.9272 0.0166 0.0993 0.077 Uiso 1 calc R . . C13A C 0.9516(10) 0.1291(10) 0.09278(19) 0.059(4) Uani 1 d DU . . H13A H 0.9764 0.1536 0.1027 0.071 Uiso 1 calc R . . C14A C 0.9463(8) 0.1759(9) 0.08068(16) 0.044(3) Uani 1 d DU . . H14A H 0.9698 0.2322 0.0820 0.053 Uiso 1 calc R . . C15A C 0.8594(8) 0.1422(7) 0.03732(15) 0.031(3) Uani 1 d DU . . C16A C 0.7767(8) 0.0892(7) 0.03870(16) 0.041(3) Uani 1 d DU . . H16A H 0.7500 0.0870 0.0485 0.049 Uiso 1 calc R . . C17A C 0.7331(9) 0.0396(8) 0.02573(18) 0.054(4) Uani 1 d DU . . H17A H 0.6771 0.0036 0.0269 0.064 Uiso 1 calc R . . C18A C 0.7695(10) 0.0425(9) 0.01177(19) 0.060(4) Uani 1 d DU . . H18A H 0.7399 0.0085 0.0030 0.072 Uiso 1 calc R . . C19A C 0.8507(10) 0.0956(9) 0.01024(19) 0.061(4) Uani 1 d DU . . H19A H 0.8766 0.0987 0.0003 0.073 Uiso 1 calc R . . C20A C 0.8959(9) 0.1452(8) 0.02319(17) 0.048(4) Uani 1 d DU . . H20A H 0.9519 0.1806 0.0220 0.057 Uiso 1 calc R . . N1P N 0.5605(6) 0.1742(6) 0.02297(12) 0.032(3) Uani 1 d U . . C2P C 0.6390(8) 0.2018(8) 0.02544(15) 0.028(3) Uani 1 d U . . C3P C 0.6856(8) 0.1868(8) 0.01492(16) 0.046(4) Uani 1 d U . . H3P H 0.7414 0.2087 0.0167 0.055 Uiso 1 calc R . . C4P C 0.6483(10) 0.1389(10) 0.00170(19) 0.069(5) Uani 1 d U . . H4P H 0.6786 0.1261 -0.0055 0.082 Uiso 1 calc R . . C5P C 0.5666(9) 0.1086(10) -0.00132(18) 0.061(4) Uani 1 d U . . H5P H 0.5416 0.0759 -0.0105 0.073 Uiso 1 calc R . . C6P C 0.5227(9) 0.1275(9) 0.00946(18) 0.049(4) Uani 1 d U . . C1MP C 0.4333(8) 0.0981(10) 0.00750(19) 0.071(5) Uani 1 d U . . H1M1 H 0.4151 0.1185 0.0164 0.107 Uiso 1 calc R . . H1M2 H 0.4032 0.0393 0.0076 0.107 Uiso 1 calc R . . H1M3 H 0.4242 0.1176 -0.0028 0.107 Uiso 1 calc R . . O2P O 0.6649(5) 0.2420(5) 0.03911(10) 0.030(2) Uani 1 d U . . N1Q N 0.9485(6) 0.5523(6) 0.07223(12) 0.031(5) Uiso 0.50 d PDU A -1 H1Q H 0.9199 0.5457 0.0810 0.037 Uiso 0.50 calc PR A -1 C2Q C 0.9248(6) 0.4898(6) 0.06099(12) 0.045(4) Uani 1 d RDU . . C3Q C 0.9715(6) 0.5009(6) 0.04714(12) 0.056(9) Uiso 0.50 d PRDU A -1 H3Q H 0.9552 0.4583 0.0396 0.067 Uiso 0.50 calc PR A -1 C4Q C 1.0456(16) 0.5781(16) 0.0442(3) 0.042(7) Uiso 0.50 d PDU A -1 H4Q H 1.0780 0.5855 0.0349 0.050 Uiso 0.50 calc PR A -1 C5Q C 1.0663(18) 0.6388(18) 0.0552(4) 0.055(8) Uiso 0.50 d PDU A -1 H5Q H 1.1124 0.6897 0.0533 0.066 Uiso 0.50 calc PR A -1 C6Q C 1.0197(14) 0.6265(13) 0.0692(3) 0.032(6) Uiso 0.50 d PDU A -1 C1MQ C 1.0372(14) 0.6874(13) 0.0822(3) 0.039(7) Uiso 0.50 d PDU A -1 H1M4 H 0.9959 0.6638 0.0906 0.058 Uiso 0.50 calc PR A -1 H1M5 H 1.0374 0.7342 0.0776 0.058 Uiso 0.50 calc PR A -1 H1M6 H 1.0899 0.7038 0.0870 0.058 Uiso 0.50 calc PR A -1 O2Q O 0.8723(5) 0.4161(5) 0.06264(10) 0.045(2) Uani 1 d DU . . O1Q O 0.8872(11) 0.5209(10) 0.0698(2) 0.056(5) Uiso 0.50 d PDU A 2 O3Q O 0.9760(11) 0.5265(13) 0.0518(3) 0.096(8) Uiso 0.50 d PDU A 2 H3Q1 H 0.9946 0.4980 0.0484 0.144 Uiso 0.50 d PR A 2 O1S O 0.318(5) 0.594(4) 0.0271(9) 0.079(19) Uiso 0.17 d PDU B -1 H1S H 0.3461 0.5745 0.0302 0.119 Uiso 0.17 d PR B -1 C1S C 0.380(6) 0.675(4) 0.0271(13) 0.09(3) Uiso 0.17 d PDU B -1 H1S1 H 0.3506 0.7021 0.0299 0.141 Uiso 0.17 d PR B -1 H1S2 H 0.3967 0.6851 0.0157 0.141 Uiso 0.17 d PR B -1 H1S3 H 0.4281 0.6952 0.0339 0.141 Uiso 0.17 d PR B -1 O1W O 1.0000 0.0000 0.0195(10) 0.074(19) Uiso 0.25 d SPU C 1 O1X O 1.0000 0.0000 0.0326(9) 0.060(19) Uiso 0.25 d SPU D 2 O1Y O 1.0000 0.0000 0.0000 0.057(13) Uiso 0.50 d SPU E 3 O1Z O 0.3333 0.6667 0.0164(9) 0.068(19) Uiso 0.25 d SPU F 4 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 Co1 0.0251(10) 0.0315(11) 0.0234(10) -0.0011(8) 0.0005(8) 0.0167(9) Co2 0.0188(14) 0.0188(14) 0.022(2) 0.000 0.000 0.0094(7) Co3 0.0197(10) 0.0265(14) 0.0247(15) -0.0024(12) -0.0012(6) 0.0133(7) O1V 0.022(4) 0.016(4) 0.018(4) 0.000(3) 0.003(3) 0.007(3) O1A 0.042(6) 0.062(6) 0.033(5) -0.007(5) -0.004(4) 0.041(5) O2A 0.048(6) 0.063(6) 0.022(5) -0.007(5) 0.004(5) 0.045(5) C1A 0.030(7) 0.034(7) 0.030(6) -0.011(6) -0.007(6) 0.025(6) C2A 0.033(5) 0.033(6) 0.035(6) -0.003(5) 0.005(5) 0.027(4) C3A 0.036(5) 0.042(6) 0.019(7) -0.005(5) 0.001(5) 0.022(5) C4A 0.039(7) 0.067(9) 0.062(10) 0.002(8) 0.004(7) 0.034(6) C5A 0.041(8) 0.104(11) 0.104(13) 0.024(11) 0.022(9) 0.045(9) C6A 0.049(9) 0.089(10) 0.079(12) 0.017(10) 0.021(9) 0.026(8) C7A 0.055(9) 0.054(9) 0.051(10) 0.011(8) 0.020(8) 0.013(6) C8A 0.045(7) 0.046(7) 0.056(10) 0.003(7) 0.014(7) 0.020(6) C9A 0.033(7) 0.036(6) 0.037(6) 0.000(5) 0.004(5) 0.029(6) C10A 0.060(9) 0.038(6) 0.041(8) 0.006(6) -0.002(7) 0.024(7) C11A 0.091(12) 0.029(7) 0.065(10) 0.015(6) -0.006(9) 0.026(8) C12A 0.075(11) 0.066(8) 0.065(9) 0.017(8) -0.004(8) 0.046(9) C13A 0.078(11) 0.076(8) 0.040(8) -0.007(7) -0.007(8) 0.051(9) C14A 0.068(10) 0.056(8) 0.029(7) -0.006(6) -0.001(7) 0.046(8) C15A 0.038(6) 0.038(7) 0.032(6) -0.001(5) 0.003(5) 0.031(5) C16A 0.044(6) 0.055(9) 0.030(7) -0.009(6) 0.009(6) 0.029(6) C17A 0.059(8) 0.045(9) 0.056(9) -0.021(7) -0.010(6) 0.026(7) C18A 0.070(8) 0.062(10) 0.055(8) -0.039(8) -0.021(8) 0.038(8) C19A 0.076(9) 0.080(11) 0.044(8) -0.027(8) 0.000(7) 0.052(8) C20A 0.050(8) 0.057(9) 0.046(7) -0.018(7) 0.007(6) 0.034(7) N1P 0.027(5) 0.040(7) 0.025(6) -0.005(5) -0.007(4) 0.014(5) C2P 0.035(6) 0.038(8) 0.019(6) -0.006(5) -0.002(5) 0.024(6) C3P 0.034(7) 0.062(10) 0.035(8) -0.013(6) 0.009(6) 0.018(7) C4P 0.066(8) 0.093(12) 0.061(10) -0.040(8) -0.004(8) 0.050(10) C5P 0.063(8) 0.073(11) 0.047(9) -0.022(8) -0.015(7) 0.034(9) C6P 0.045(7) 0.057(9) 0.043(9) -0.010(7) -0.015(6) 0.024(7) C1MP 0.042(7) 0.083(12) 0.068(12) -0.035(10) -0.023(8) 0.016(9) O2P 0.024(4) 0.036(5) 0.030(5) -0.012(4) -0.007(4) 0.016(4) C2Q 0.075(9) 0.029(6) 0.039(8) -0.002(6) 0.000(7) 0.032(6) O2Q 0.029(5) 0.056(5) 0.027(5) 0.005(4) -0.001(4) 0.003(4) _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 Co1 O2P 2.025(8) . ? Co1 O1A 2.036(8) . ? Co1 O2P 2.103(8) 2_655 ? Co1 O1V 2.128(7) . ? Co1 O2Q 2.183(8) . ? Co1 N1P 2.220(10) 2_655 ? Co2 O1V 1.898(7) . ? Co2 O1V 1.898(7) 3_665 ? Co2 O1V 1.898(7) 2_655 ? Co2 O1V 1.898(7) 17_554 ? Co2 O1V 1.898(7) 18_654 ? Co2 O1V 1.897(7) 16_544 ? Co3 O2A 2.040(8) . ? Co3 O2A 2.040(8) 17_554 ? Co3 O1V 2.102(7) . ? Co3 O1V 2.102(7) 17_554 ? Co3 O2Q 2.176(8) . ? Co3 O2Q 2.176(8) 17_554 ? O1A C1A 1.276(14) . ? O2A C1A 1.256(14) . ? C1A C2A 1.555(16) . ? C2A C15A 1.536(17) . ? C2A C9A 1.541(17) . ? C2A C3A 1.542(17) . ? C3A C8A 1.385(18) . ? C3A C4A 1.402(18) . ? C4A C5A 1.39(2) . ? C5A C6A 1.34(2) . ? C6A C7A 1.33(2) . ? C7A C8A 1.378(19) . ? C9A C14A 1.361(17) . ? C9A C10A 1.389(18) . ? C10A C11A 1.349(18) . ? C11A C12A 1.39(2) . ? C12A C13A 1.38(2) . ? C13A C14A 1.370(19) . ? C15A C20A 1.336(17) . ? C15A C16A 1.388(17) . ? C16A C17A 1.388(18) . ? C17A C18A 1.32(2) . ? C18A C19A 1.37(2) . ? C19A C20A 1.395(18) . ? N1P C2P 1.330(15) . ? N1P C6P 1.376(16) . ? N1P Co1 2.220(10) 3_665 ? C2P O2P 1.305(13) . ? C2P C3P 1.365(17) . ? C3P C4P 1.365(19) . ? C4P C5P 1.385(19) . ? C5P C6P 1.38(2) . ? C6P C1MP 1.512(19) . ? O2P Co1 2.103(8) 3_665 ? N1Q C2Q 1.3899 . ? N1Q C6Q 1.41(3) . ? C2Q O3Q 1.152(14) . ? C2Q O2Q 1.259(11) . ? C2Q O1Q 1.347(14) . ? C2Q C3Q 1.3900 . ? C3Q C4Q 1.46(3) . ? C4Q C5Q 1.36(4) . ? C5Q C6Q 1.40(4) . ? C6Q C1MQ 1.484(10) . ? O1S C1S 1.40(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2P Co1 O1A 97.2(3) . . ? O2P Co1 O2P 92.7(4) . 2_655 ? O1A Co1 O2P 155.3(3) . 2_655 ? O2P Co1 O1V 82.7(3) . . ? O1A Co1 O1V 97.3(3) . . ? O2P Co1 O1V 106.3(3) 2_655 . ? O2P Co1 O2Q 161.0(3) . . ? O1A Co1 O2Q 90.5(3) . . ? O2P Co1 O2Q 87.3(3) 2_655 . ? O1V Co1 O2Q 79.1(3) . . ? O2P Co1 N1P 97.9(4) . 2_655 ? O1A Co1 N1P 95.3(4) . 2_655 ? O2P Co1 N1P 60.8(3) 2_655 2_655 ? O1V Co1 N1P 167.1(3) . 2_655 ? O2Q Co1 N1P 98.6(3) . 2_655 ? O1V Co2 O1V 91.5(3) . 3_665 ? O1V Co2 O1V 91.5(3) . 2_655 ? O1V Co2 O1V 91.5(3) 3_665 2_655 ? O1V Co2 O1V 83.8(4) . 17_554 ? O1V Co2 O1V 173.1(4) 3_665 17_554 ? O1V Co2 O1V 93.7(4) 2_655 17_554 ? O1V Co2 O1V 93.7(4) . 18_654 ? O1V Co2 O1V 83.8(4) 3_665 18_654 ? O1V Co2 O1V 173.1(4) 2_655 18_654 ? O1V Co2 O1V 91.5(3) 17_554 18_654 ? O1V Co2 O1V 173.1(4) . 16_544 ? O1V Co2 O1V 93.7(4) 3_665 16_544 ? O1V Co2 O1V 83.8(4) 2_655 16_544 ? O1V Co2 O1V 91.5(3) 17_554 16_544 ? O1V Co2 O1V 91.5(3) 18_654 16_544 ? O2A Co3 O2A 94.8(5) . 17_554 ? O2A Co3 O1V 97.6(3) . . ? O2A Co3 O1V 161.5(3) 17_554 . ? O2A Co3 O1V 161.5(3) . 17_554 ? O2A Co3 O1V 97.6(3) 17_554 17_554 ? O1V Co3 O1V 74.1(4) . 17_554 ? O2A Co3 O2Q 92.7(3) . . ? O2A Co3 O2Q 85.9(3) 17_554 . ? O1V Co3 O2Q 79.9(3) . . ? O1V Co3 O2Q 101.9(3) 17_554 . ? O2A Co3 O2Q 85.9(3) . 17_554 ? O2A Co3 O2Q 92.7(3) 17_554 17_554 ? O1V Co3 O2Q 101.9(3) . 17_554 ? O1V Co3 O2Q 79.9(3) 17_554 17_554 ? O2Q Co3 O2Q 177.9(5) . 17_554 ? Co2 O1V Co3 101.0(3) . . ? Co2 O1V Co1 131.1(4) . . ? Co3 O1V Co1 95.5(3) . . ? C1A O1A Co1 130.4(8) . . ? C1A O2A Co3 128.8(8) . . ? O2A C1A O1A 125.5(11) . . ? O2A C1A C2A 120.2(11) . . ? O1A C1A C2A 114.1(11) . . ? C15A C2A C9A 113.5(10) . . ? C15A C2A C3A 109.1(10) . . ? C9A C2A C3A 108.5(10) . . ? C15A C2A C1A 108.0(10) . . ? C9A C2A C1A 110.1(10) . . ? C3A C2A C1A 107.4(10) . . ? C8A C3A C4A 115.8(13) . . ? C8A C3A C2A 124.1(11) . . ? C4A C3A C2A 119.8(12) . . ? C5A C4A C3A 120.3(15) . . ? C6A C5A C4A 121.9(16) . . ? C7A C6A C5A 118.4(16) . . ? C6A C7A C8A 122.3(16) . . ? C7A C8A C3A 121.3(14) . . ? C14A C9A C10A 118.7(13) . . ? C14A C9A C2A 119.4(12) . . ? C10A C9A C2A 121.6(12) . . ? C11A C10A C9A 123.9(14) . . ? C10A C11A C12A 117.1(14) . . ? C13A C12A C11A 119.5(15) . . ? C14A C13A C12A 122.1(15) . . ? C9A C14A C13A 118.6(14) . . ? C20A C15A C16A 118.6(13) . . ? C20A C15A C2A 124.3(12) . . ? C16A C15A C2A 117.1(11) . . ? C15A C16A C17A 120.6(13) . . ? C18A C17A C16A 120.6(15) . . ? C17A C18A C19A 119.1(14) . . ? C18A C19A C20A 121.3(15) . . ? C15A C20A C19A 119.8(14) . . ? C2P N1P C6P 120.0(11) . . ? C2P N1P Co1 90.3(7) . 3_665 ? C6P N1P Co1 149.3(9) . 3_665 ? O2P C2P N1P 112.5(10) . . ? O2P C2P C3P 124.6(12) . . ? N1P C2P C3P 122.8(12) . . ? C4P C3P C2P 117.6(13) . . ? C3P C4P C5P 121.4(14) . . ? C6P C5P C4P 118.6(14) . . ? N1P C6P C5P 119.5(13) . . ? N1P C6P C1MP 117.0(13) . . ? C5P C6P C1MP 123.6(13) . . ? C2P O2P Co1 132.9(8) . . ? C2P O2P Co1 96.3(7) . 3_665 ? Co1 O2P Co1 127.2(4) . 3_665 ? C2Q N1Q C6Q 118.8(10) . . ? O3Q C2Q O2Q 134.9(15) . . ? O3Q C2Q O1Q 124.1(15) . . ? O2Q C2Q O1Q 97.6(9) . . ? O3Q C2Q N1Q 95.7(13) . . ? O2Q C2Q N1Q 128.4(6) . . ? O1Q C2Q N1Q 44.3(8) . . ? O3Q C2Q C3Q 24.6(13) . . ? O2Q C2Q C3Q 110.4(6) . . ? O1Q C2Q C3Q 144.2(8) . . ? N1Q C2Q C3Q 120.0 . . ? C2Q C3Q C4Q 120.8(11) . . ? C5Q C4Q C3Q 118(2) . . ? C4Q C5Q C6Q 121(3) . . ? C5Q C6Q N1Q 122(2) . . ? C5Q C6Q C1MQ 126(2) . . ? N1Q C6Q C1MQ 112.7(18) . . ? C2Q O2Q Co3 134.0(7) . . ? C2Q O2Q Co1 133.5(7) . . ? Co3 O2Q Co1 91.8(3) . . ? _diffrn_measured_fraction_theta_max 0.295 _diffrn_reflns_theta_full 20.06 _diffrn_measured_fraction_theta_full 0.295 _refine_diff_density_max 0.814 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.108