# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Euan Brechin' 'Guillem Aromi' 'E. McInnes' 'S. Parsons' 'Wolfgang Wernsdorfer' _publ_contact_author_name 'Euan Brechin' _publ_contact_author_address ; Department of Chemistry University of Edinburgh West Mains Raod Edinburgh EH9 3JJ UNITED KINGDOM ; _publ_contact_author_email EBRECHIN@STAFFMAIL.ED.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Synthesis, structure and magnetic properties of a decametallic Ni single-molecule magnet ; data_eb0532 _database_code_depnum_ccdc_archive 'CCDC 278999' _audit_creation_method SHELXL-97 _chemical_compound_source 'Euan Brechin reaction EKB33' _exptl_crystal_recrystallization_method ; Slow evaporation of MeOH/CH2Cl2 solution. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ni10(acac)6(N3)10(tmp)(OMe)(MeOH)5(H2O)].H2O.MeOH' _chemical_formula_sum 'C43 H84 N30 Ni10 O24' _chemical_formula_weight 1992.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8253(6) _cell_length_b 14.5088(8) _cell_length_c 24.9691(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.851(4) _cell_angle_gamma 90.00 _cell_volume 3919.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5174 _cell_measurement_theta_min 2 _cell_measurement_theta_max 24 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 2.430 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_T_max 0.760 _exptl_absorpt_process_details 'Sadabs v 2.10' _exptl_special_details ; Data collection strategy optimised with COSMO. Oxford Cryosystems LT device. ; _diffrn_ambient_temperature 150(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 Apex CCD' _diffrn_measurement_method 'Omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72251 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6897 _reflns_number_gt 5255 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Dirdif _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'XCIF, PLATON' _refine_special_details ; Ligands: 1. Part weight tmp ABC: Part weight azise (AB) and MeO-(C) 2-4 acac 5-8 N3 9 MeOH (1-3 part of complex; 4 solvent) 10 H2O of solvation. The structure is disordered about an inversion centre. The tmp (#1) is half-occupied; the symmetry-related position appears to be occupied by 2 azides and an MeO- (these carry the labels A, B and C). The 1,2 and 1,3 distances in the C(CH2O)3 moiety of the tmp were restrained to have 3-fold symmetry. Azides A and B were restrained to be geometrically similar. The occupancies were fixed at 0.5 after competitive refinement. Azide #7 is disordered over two orientations. N17-N27-N37 is present when methanol of solvation C49-O49 is present. When the latter is absent the orientation of the azide follws N17-N27'-N37'. This was inferred from the unfavorably short N37'...O49 interaction. All occupancies were fixed at 0.5, and the two axides were restrained to be geometrically similar. The C-atom of MeOH #3 (C39-O39) makes a short contact to what appears to be water of crystallisation #10. The MeOH site is therefore presumably 50% water (present when 0110 is present) and 50% MeOH. No attempt was made to place the 9 part weight H-atoms incorporated in the part-weight H2O and MeOH groups described above. The H-atoms H19 and H29 were selected on the basis of their favorable H-bonding contacts. ADPs were refined only for full-weight atoms. All a bit messy. The .res file is included below after the checkcif output. Checkcif output: 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 8.21 Ratio 220_ALERT_2_A Large Non-Solvent N Ueq(max)/Ueq(min) ... 9.20 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 10.00 Ratio 241_ALERT_2_B Check High Ueq as Compared to Neighbors for N3A 241_ALERT_2_B Check High Ueq as Compared to Neighbors for N3B 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for O19 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for O29 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for N27 241_ALERT_2_C Check High Ueq as Compared to Neighbors for Ni3 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1A 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C21 Terminal C-atoms of MeO- and N-atoms of axide have high thermal motion, though this is not unusual for these ligands. 430_ALERT_2_A Short Inter D...A Contact O49 .. N37' .. 2.21 Ang. 432_ALERT_2_A Short Inter X...Y Contact O110 .. C39 .. 2.05 Ang. 430_ALERT_2_C Short Inter D...A Contact O49 .. O110 .. 2.87 Ang. 432_ALERT_2_C Short Inter X...Y Contact O110 .. C29 .. 2.96 Ang. See discussion of disorder above. 041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? 068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? Part weight H's not placed. See above. 060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.12 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay etc. The crystal was a rather irregular shape, having been cleaved from a larger block; this precluded integration methods for correcting for absorption. 301_ALERT_3_C Main Residue Disorder ......................... 17.00 Perc. 302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. 309_ALERT_2_C Single Bonded Oxygen (C-O .GT. 1.3 Ang) ........ O49 341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 12 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 3 779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 42.50 Deg. N27 -N17 -N27' 1.555 1.555 1.555 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C42 H75 N30 Ni10 O22 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C O 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C22 796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O12 797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N16 911_ALERT_3_C # Missing FCF Refl. Between TH(Min) & STH/L=0.6 3 Noted but no action taken. Data were weak above 50 deg in 2theta. Data set statistics: #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 0.999 4104 4101 3 23.01 0.550 0.999 5456 5453 3 25.00 0.595 1.000 6900 6897 3 #----------------------------------------------------------- ACTA Min. Res. ---- Final res file: #TITL EB0532 in P21/n solved dirdif CELL 0.71073 10.82530 14.50880 24.96910 90.0000 91.8510 90.0000 ZERR 2.000 0.00060 0.00080 0.00130 0.0000 0.0040 0.0000 LATT +1 SYMM 1/2-X , 1/2+Y , 1/2-Z SFAC C H N O NI UNIT 86 168 60 48 20 REM 9 PART-WEIGHT H PER FORMULA UNIT NOT PLACED. TEMP -123 ACTA OMIT -3 50 OMIT -1 0 5 OMIT 0 0 4 OMIT -2 0 2 L.S. 6 BOND $H HTAB FMAP 2 PLAN 10 WGHT 0.085900 18.985798 FVAR 0.15110 NI1 5 -0.551111 0.531591 1.161076 11.00000 0.05940 0.04388 = 0.02570 0.00527 -0.01244 -0.01025 NI2 5 -0.401890 0.714741 1.139696 11.00000 0.05978 0.04149 = 0.02650 -0.00377 -0.00932 -0.00942 NI3 5 -0.468190 0.571198 1.045112 11.00000 0.09803 0.05703 = 0.02251 -0.00488 -0.00116 -0.04119 NI4 5 -0.324066 0.751931 1.020148 11.00000 0.04983 0.03048 = 0.03031 0.00099 -0.00924 -0.00408 NI5 5 -0.395355 0.613567 0.928159 11.00000 0.07017 0.04897 = 0.02447 0.00128 -0.00398 -0.02313 PART 1 10.5 SAME 0.01 C11 C41 O41 C21 O21 C31 O31 C51 C61 C11 1 -0.251994 0.453368 0.997459 10.50000 0.02925 C21 1 -0.229024 0.556123 1.012965 10.50000 0.01910 AFIX 23 H21A 2 -0.202923 0.559384 1.051285 10.50000 -1.20000 H21B 2 -0.160522 0.580428 0.991755 10.50000 -1.20000 AFIX 0 O21 4 -0.335087 0.613161 1.004176 10.50000 0.02966 C31 1 -0.350722 0.408930 1.033006 10.50000 0.03190 AFIX 23 H31A 2 -0.354867 0.342303 1.024583 10.50000 -1.20000 H31B 2 -0.322156 0.414805 1.070918 10.50000 -1.20000 AFIX 0 O31 4 -0.471686 0.445446 1.028023 10.50000 0.02811 C41 1 -0.285589 0.442477 0.937051 10.50000 0.04135 AFIX 23 H41A 2 -0.218093 0.469576 0.916347 10.50000 -1.20000 H41B 2 -0.289006 0.375853 0.928568 10.50000 -1.20000 AFIX 0 O41 4 -0.398163 0.483076 0.919265 10.50000 0.03306 C51 1 -0.130945 0.399426 1.007100 10.50000 0.03888 AFIX 23 H51A 2 -0.145967 0.335232 0.995131 10.50000 -1.20000 H51B 2 -0.068779 0.425918 0.983284 10.50000 -1.20000 AFIX 0 C61 1 -0.073919 0.395374 1.062228 10.50000 0.04635 AFIX 33 H61A 2 0.000941 0.357418 1.061950 10.50000 -1.50000 H61B 2 -0.132811 0.368228 1.086710 10.50000 -1.50000 H61C 2 -0.052417 0.457812 1.074248 10.50000 -1.50000 AFIX 0 PART 2 10.5 N1A 3 -0.358499 0.462582 0.914945 10.50000 0.02472 N2A 3 -0.256643 0.422972 0.921303 10.50000 0.05020 N3A 3 -0.163503 0.389151 0.919804 10.50000 0.09641 SAME N1A > N3A N1B 3 -0.425043 0.416484 1.032697 10.50000 0.03100 N2B 3 -0.332952 0.371167 1.046487 10.50000 0.04341 N3B 3 -0.248271 0.328959 1.059143 10.50000 0.07670 O1C 4 -0.293508 0.607872 1.004290 10.50000 0.04388 C1C 1 -0.180013 0.571321 1.016430 10.50000 0.04564 AFIX 33 H1C1 2 -0.180391 0.505423 1.007811 10.50000 -1.50000 H1C2 2 -0.160516 0.579617 1.054727 10.50000 -1.50000 H1C3 2 -0.117546 0.602649 0.995479 10.50000 -1.50000 AFIX 0 PART 0 O12 4 -0.715199 0.503527 1.191259 11.00000 0.05703 0.05682 = 0.05105 0.01864 -0.00932 -0.01104 C22 1 -0.789549 0.563692 1.209545 11.00000 0.04347 0.06641 = 0.07128 0.02473 -0.01317 0.00386 C32 1 -0.766462 0.659362 1.213338 11.00000 0.04546 0.06464 = 0.06175 0.01751 -0.00581 0.00825 AFIX 43 H32 2 -0.825162 0.695276 1.231623 11.00000 -1.20000 AFIX 0 C42 1 -0.664833 0.706671 1.192635 11.00000 0.04993 0.06135 = 0.03450 0.00563 -0.02294 -0.00508 O52 4 -0.576413 0.669543 1.168007 11.00000 0.05077 0.05081 = 0.03172 0.00157 -0.00497 -0.00289 C62 1 -0.910521 0.529779 1.227631 11.00000 0.05777 0.08338 = 0.16405 0.04378 0.01427 0.00492 AFIX 137 H62A 2 -0.945070 0.485883 1.201345 11.00000 -1.50000 H62B 2 -0.967306 0.581893 1.231078 11.00000 -1.50000 H62C 2 -0.899132 0.499150 1.262421 11.00000 -1.50000 AFIX 0 C72 1 -0.663735 0.808815 1.201176 11.00000 0.07219 0.06472 = 0.06005 -0.00874 -0.00088 -0.00588 AFIX 137 H72A 2 -0.588003 0.826427 1.221178 11.00000 -1.50000 H72B 2 -0.735805 0.826708 1.221546 11.00000 -1.50000 H72C 2 -0.666680 0.840167 1.166394 11.00000 -1.50000 AFIX 0 O13 4 -0.343257 0.699423 1.216506 11.00000 0.05903 0.04352 = 0.03027 -0.00651 -0.01491 -0.00405 C23 1 -0.321924 0.765738 1.249363 11.00000 0.05100 0.05236 = 0.03164 -0.01212 -0.00725 -0.00278 C33 1 -0.325578 0.859240 1.236155 11.00000 0.06234 0.04731 = 0.03706 -0.01398 -0.00804 -0.00521 AFIX 43 H33 2 -0.302462 0.901393 1.263816 11.00000 -1.20000 AFIX 0 C43 1 -0.359645 0.897005 1.186579 11.00000 0.04775 0.04933 = 0.03928 -0.01436 -0.00178 -0.00252 O53 4 -0.403519 0.851588 1.146073 11.00000 0.05931 0.04617 = 0.03384 -0.00505 -0.00752 -0.00710 C63 1 -0.290350 0.737848 1.306037 11.00000 0.08668 0.05468 = 0.03833 -0.01557 -0.01109 0.00200 AFIX 137 H63A 2 -0.354869 0.696956 1.319070 11.00000 -1.50000 H63B 2 -0.284703 0.792903 1.328723 11.00000 -1.50000 H63C 2 -0.210859 0.705472 1.307330 11.00000 -1.50000 AFIX 0 C73 1 -0.348243 0.997528 1.178150 11.00000 0.07608 0.04578 = 0.05898 -0.01119 -0.00883 -0.01207 AFIX 137 H73A 2 -0.282402 1.009628 1.153052 11.00000 -1.50000 H73B 2 -0.328154 1.027706 1.212448 11.00000 -1.50000 H73C 2 -0.426621 1.021845 1.163365 11.00000 -1.50000 AFIX 0 O14 4 -0.239704 0.736137 1.093716 11.00000 0.05212 0.03036 = 0.03501 -0.00148 -0.00900 -0.00172 C24 1 -0.125582 0.755128 1.104013 11.00000 0.04577 0.03958 = 0.04977 -0.00964 -0.01470 0.00597 C34 1 -0.043830 0.786640 1.067149 11.00000 0.04517 0.06533 = 0.05460 -0.01251 -0.01001 -0.00039 AFIX 43 H34 2 0.038023 0.797765 1.080451 11.00000 -1.20000 AFIX 0 C44 1 -0.065498 0.804276 1.013033 11.00000 0.04276 0.06222 = 0.05811 0.00312 -0.00728 0.00031 O54 4 -0.166868 0.788654 0.987232 11.00000 0.05127 0.05383 = 0.04117 0.00003 -0.00248 -0.00349 C64 1 -0.080526 0.740741 1.161146 11.00000 0.05837 0.07183 = 0.04553 -0.00326 -0.01885 0.00212 AFIX 137 H64A 2 -0.124009 0.783020 1.184659 11.00000 -1.50000 H64B 2 0.008500 0.752838 1.164080 11.00000 -1.50000 H64C 2 -0.096774 0.677009 1.171849 11.00000 -1.50000 AFIX 0 C74 1 0.037929 0.845913 0.980614 11.00000 0.05908 0.08744 = 0.06724 0.01125 -0.00230 -0.00733 AFIX 137 H74A 2 0.065298 0.800765 0.954322 11.00000 -1.50000 H74B 2 0.107551 0.862503 1.004771 11.00000 -1.50000 H74C 2 0.007309 0.901191 0.961946 11.00000 -1.50000 AFIX 0 N15 3 -0.388610 0.573235 1.124674 11.00000 0.05750 0.03806 = 0.02305 -0.00208 -0.00982 -0.01098 N25 3 -0.293369 0.537124 1.140642 11.00000 0.08439 0.05678 = 0.02582 0.00252 -0.01618 -0.02043 N35 3 -0.205804 0.505850 1.156279 11.00000 0.10257 0.07867 = 0.04547 0.01077 -0.01794 -0.01614 N16 3 -0.481354 0.714574 1.062412 11.00000 0.03986 0.04226 = 0.02622 0.00149 -0.00857 -0.00138 N26 3 -0.573611 0.763002 1.055773 11.00000 0.07261 0.06123 = 0.03594 -0.01029 0.00098 -0.01934 N36 3 -0.655991 0.807462 1.052247 11.00000 0.08333 0.08894 = 0.08396 -0.01509 -0.00360 -0.01079 REM DISORDERED AZIDE. N17-N27-N37 PRESENT WITH C49-O49 MEOH OF SOLVATION SAME 0.01 N17 N27' N37' N17 3 -0.416040 0.750892 0.946490 11.00000 0.06763 0.04248 = 0.03399 0.00762 -0.00818 -0.00760 PART 1 N27 3 -0.502258 0.788999 0.929596 10.50000 0.03406 N37 3 -0.582446 0.832056 0.913573 10.50000 0.05325 PART 2 N27' 3 -0.437773 0.817569 0.921783 10.50000 0.10210 N37' 3 -0.418176 0.880882 0.895719 10.50000 0.23004 PART 0 N18 3 -0.488467 0.606476 0.853603 11.00000 0.07009 0.05437 = 0.02876 0.00179 -0.00579 -0.01426 N28 3 -0.483868 0.665361 0.819771 11.00000 0.06010 0.06264 = 0.03521 0.00397 -0.00479 -0.01159 N38 3 -0.480165 0.719450 0.787444 11.00000 0.11612 0.08186 = 0.06023 0.04115 -0.00107 -0.02215 O19 4 -0.365275 0.889255 1.040085 11.00000 0.07675 0.03454 = 0.04239 -0.00123 -0.00113 -0.00243 AFIX 3 H19 2 -0.356374 0.891551 1.079648 11.00000 -1.20000 AFIX 0 C19 1 -0.311607 0.968853 1.022552 11.00000 0.32235 0.04363 = 0.11028 -0.00552 0.09156 -0.02511 AFIX 33 H19A 2 -0.350564 1.022004 1.039375 11.00000 -1.50000 H19B 2 -0.322744 0.973315 0.983532 11.00000 -1.50000 H19C 2 -0.223148 0.968144 1.032216 11.00000 -1.50000 AFIX 0 O29 4 -0.454200 0.533231 1.234609 11.00000 0.07139 0.05237 = 0.02848 0.00677 -0.01010 -0.01079 AFIX 3 H29 2 -0.426369 0.597710 1.239777 11.00000 -1.20000 AFIX 0 C29 1 -0.499806 0.505661 1.283882 11.00000 0.09929 0.20302 = 0.06518 0.04738 -0.02422 -0.05119 AFIX 33 H29A 2 -0.435057 0.512818 1.311917 11.00000 -1.50000 H29B 2 -0.525249 0.440906 1.281768 11.00000 -1.50000 H29C 2 -0.571066 0.543945 1.292482 11.00000 -1.50000 AFIX 0 REM O39 FULL OCC, C39 1/2 OCC. SITE IS 50:50 MEOH/H2O. REM MEOH (IE C39) IS PRESENT WHEN WATER OF SOLVATION #10 IS ABSENT REM 1 H PER FORMULA UNIT OF MEOH NOT PLACED REM 2 H PER FORMULA UNIT OF H2O NOT PLACED O39 4 -0.229544 0.635714 0.887831 11.00000 0.05592 0.07950 = 0.07219 0.03379 0.00197 -0.00950 PART 1 C39 1 -0.192631 0.715014 0.861735 10.50000 0.06518 AFIX 33 H39A 2 -0.111423 0.704885 0.846516 10.50000 -1.50000 H39B 2 -0.187456 0.766188 0.887326 10.50000 -1.50000 H39C 2 -0.252941 0.729984 0.832929 10.50000 -1.50000 AFIX 0 PART 0 REM MEOH #4 NO ATTEMPT TO PLACE H'S HERE (4 MISSING PER FORM. UNIT) REM THIS IS PRESENT WHEN N17-N2-N37 IS PRESENT PART 1 O49 4 -0.264387 0.964158 0.865509 10.50000 0.07557 C49 1 -0.147373 1.018264 0.899158 10.50000 0.11321 REM WATER OF CRYSTALLISATION. 2H PER FORM UNIT NOT PLACED. PART 2 O110 4 -0.093327 0.824516 0.834197 10.50000 0.06965 PART 0 HKLF 4 REM EB0532 in P21/n solved dirdif REM R1 = 0.0758 for 5255 Fo > 4sig(Fo) and 0.1000 for all 6897 data REM 476 parameters refined using 24 restraints END WGHT 0.0860 18.9612 REM Highest difference peak 1.333, deepest hole -1.025, 1-sigma level 0.125 Q1 1 -0.0998 0.5445 1.0311 11.00000 0.05 1.33 Q2 1 -0.2238 0.8470 0.8673 11.00000 0.05 1.32 Q3 1 -0.3093 0.9151 0.8425 11.00000 0.05 1.22 Q4 1 -0.0933 0.6186 0.8926 11.00000 0.05 1.21 Q5 1 -0.5428 0.5612 1.0468 11.00000 0.05 0.91 Q6 1 -0.3966 0.5820 1.0304 11.00000 0.05 0.81 Q7 1 -0.2278 0.9879 0.8793 11.00000 0.05 0.76 Q8 1 -0.4395 0.5352 1.0336 11.00000 0.05 0.70 Q9 1 -0.1876 0.9355 0.8882 11.00000 0.05 0.68 Q10 1 -0.4973 0.6053 1.0639 11.00000 0.05 0.65 ; _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^)+(0.0859P)^2^+18.9858P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6897 _refine_ls_number_parameters 476 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2012 _refine_ls_wR_factor_gt 0.1863 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.003 _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 -0.55111(10) 0.53159(7) 1.16108(4) 0.0433(3) Uani 1 1 d . . . Ni2 Ni -0.40189(10) 0.71474(7) 1.13970(4) 0.0428(3) Uani 1 1 d . . . Ni3 Ni -0.46819(12) 0.57120(8) 1.04511(4) 0.0593(4) Uani 1 1 d . . . Ni4 Ni -0.32407(9) 0.75193(6) 1.02015(3) 0.0371(3) Uani 1 1 d . . . Ni5 Ni -0.39536(10) 0.61357(7) 0.92816(4) 0.0480(3) Uani 1 1 d . . . C11 C -0.2520(11) 0.4534(6) 0.9975(3) 0.029(3) Uiso 0.50 1 d PD A 1 C21 C -0.2290(11) 0.5561(7) 1.0130(4) 0.019(3) Uiso 0.50 1 d PD A 1 H21A H -0.2029 0.5594 1.0513 0.023 Uiso 0.50 1 calc PR A 1 H21B H -0.1605 0.5804 0.9918 0.023 Uiso 0.50 1 calc PR A 1 O21 O -0.3351(10) 0.6132(6) 1.0042(4) 0.030(3) Uiso 0.50 1 d PD A 1 C31 C -0.3507(11) 0.4089(9) 1.0330(5) 0.032(3) Uiso 0.50 1 d PD A 1 H31A H -0.3549 0.3423 1.0246 0.038 Uiso 0.50 1 calc PR A 1 H31B H -0.3222 0.4148 1.0709 0.038 Uiso 0.50 1 calc PR A 1 O31 O -0.4717(8) 0.4454(6) 1.0280(3) 0.028(2) Uiso 0.50 1 d PD . 1 C41 C -0.2856(12) 0.4425(10) 0.9371(5) 0.041(4) Uiso 0.50 1 d PD A 1 H41A H -0.2181 0.4696 0.9163 0.050 Uiso 0.50 1 calc PR A 1 H41B H -0.2890 0.3759 0.9286 0.050 Uiso 0.50 1 calc PR A 1 O41 O -0.3982(9) 0.4831(7) 0.9193(4) 0.033(3) Uiso 0.50 1 d PD . 1 C51 C -0.1309(12) 0.3994(9) 1.0071(5) 0.039(3) Uiso 0.50 1 d PD A 1 H51A H -0.1460 0.3352 0.9951 0.047 Uiso 0.50 1 calc PR A 1 H51B H -0.0688 0.4259 0.9833 0.047 Uiso 0.50 1 calc PR A 1 C61 C -0.0739(14) 0.3954(11) 1.0622(6) 0.046(4) Uiso 0.50 1 d P A 1 H61A H 0.0009 0.3574 1.0620 0.070 Uiso 0.50 1 calc PR A 1 H61B H -0.1328 0.3682 1.0867 0.070 Uiso 0.50 1 calc PR A 1 H61C H -0.0524 0.4578 1.0742 0.070 Uiso 0.50 1 calc PR A 1 N1A N -0.3585(11) 0.4626(8) 0.9149(4) 0.025(3) Uiso 0.50 1 d PD . 2 N2A N -0.2566(13) 0.4230(10) 0.9213(6) 0.050(4) Uiso 0.50 1 d PD B 2 N3A N -0.1635(18) 0.3892(14) 0.9198(8) 0.096(6) Uiso 0.50 1 d PD B 2 N1B N -0.4250(13) 0.4165(8) 1.0327(4) 0.031(3) Uiso 0.50 1 d PD . 2 N2B N -0.3330(12) 0.3712(10) 1.0465(5) 0.043(3) Uiso 0.50 1 d PD C 2 N3B N -0.2483(15) 0.3290(12) 1.0591(7) 0.077(5) Uiso 0.50 1 d PD C 2 O1C O -0.2935(13) 0.6079(9) 1.0043(5) 0.044(4) Uiso 0.50 1 d P A 2 C1C C -0.1800(16) 0.5713(12) 1.0164(7) 0.046(4) Uiso 0.50 1 d P A 2 H1C1 H -0.1804 0.5054 1.0078 0.068 Uiso 0.50 1 calc PR A 2 H1C2 H -0.1605 0.5796 1.0547 0.068 Uiso 0.50 1 calc PR A 2 H1C3 H -0.1175 0.6026 0.9955 0.068 Uiso 0.50 1 calc PR A 2 O12 O -0.7152(5) 0.5035(4) 1.1913(2) 0.0552(15) Uani 1 1 d . . . C22 C -0.7895(8) 0.5637(7) 1.2095(4) 0.061(2) Uani 1 1 d . . . C32 C -0.7665(8) 0.6594(7) 1.2133(4) 0.057(2) Uani 1 1 d . . . H32 H -0.8252 0.6953 1.2316 0.069 Uiso 1 1 calc R . . C42 C -0.6648(8) 0.7067(6) 1.1926(3) 0.049(2) Uani 1 1 d . . . O52 O -0.5764(5) 0.6695(4) 1.16801(19) 0.0446(12) Uani 1 1 d . . . C62 C -0.9105(9) 0.5298(8) 1.2276(6) 0.102(4) Uani 1 1 d . . . H62A H -0.9451 0.4859 1.2013 0.152 Uiso 1 1 calc R . . H62B H -0.9673 0.5819 1.2311 0.152 Uiso 1 1 calc R . . H62C H -0.8991 0.4991 1.2624 0.152 Uiso 1 1 calc R . . C72 C -0.6637(9) 0.8088(7) 1.2012(4) 0.066(3) Uani 1 1 d . . . H72A H -0.5880 0.8264 1.2212 0.099 Uiso 1 1 calc R . . H72B H -0.7358 0.8267 1.2215 0.099 Uiso 1 1 calc R . . H72C H -0.6667 0.8402 1.1664 0.099 Uiso 1 1 calc R . . O13 O -0.3433(5) 0.6994(4) 1.21651(19) 0.0446(13) Uani 1 1 d . . . C23 C -0.3219(7) 0.7657(6) 1.2494(3) 0.0452(19) Uani 1 1 d . . . C33 C -0.3256(8) 0.8592(6) 1.2362(3) 0.049(2) Uani 1 1 d . . . H33 H -0.3025 0.9014 1.2638 0.059 Uiso 1 1 calc R . . C43 C -0.3596(7) 0.8970(6) 1.1866(3) 0.0455(19) Uani 1 1 d . . . O53 O -0.4035(5) 0.8516(4) 1.14607(19) 0.0466(13) Uani 1 1 d . . . C63 C -0.2904(9) 0.7378(6) 1.3060(3) 0.060(2) Uani 1 1 d . . . H63A H -0.3549 0.6970 1.3191 0.090 Uiso 1 1 calc R . . H63B H -0.2847 0.7929 1.3287 0.090 Uiso 1 1 calc R . . H63C H -0.2109 0.7055 1.3073 0.090 Uiso 1 1 calc R . . C73 C -0.3482(9) 0.9975(6) 1.1781(4) 0.061(2) Uani 1 1 d . . . H73A H -0.2824 1.0096 1.1531 0.091 Uiso 1 1 calc R . . H73B H -0.3282 1.0277 1.2124 0.091 Uiso 1 1 calc R . . H73C H -0.4266 1.0218 1.1634 0.091 Uiso 1 1 calc R . . O14 O -0.2397(5) 0.7361(3) 1.09372(19) 0.0394(12) Uani 1 1 d . A . C24 C -0.1256(7) 0.7551(5) 1.1040(3) 0.0454(19) Uani 1 1 d . . . C34 C -0.0438(8) 0.7866(6) 1.0671(3) 0.055(2) Uani 1 1 d . A . H34 H 0.0380 0.7978 1.0805 0.066 Uiso 1 1 calc R . . C44 C -0.0655(7) 0.8043(6) 1.0130(4) 0.055(2) Uani 1 1 d . . . O54 O -0.1669(5) 0.7887(4) 0.9872(2) 0.0488(13) Uani 1 1 d . A . C64 C -0.0805(8) 0.7407(7) 1.1611(3) 0.059(2) Uani 1 1 d . A . H64A H -0.1240 0.7830 1.1847 0.089 Uiso 1 1 calc R . . H64B H 0.0085 0.7528 1.1641 0.089 Uiso 1 1 calc R . . H64C H -0.0968 0.6770 1.1718 0.089 Uiso 1 1 calc R . . C74 C 0.0379(9) 0.8459(8) 0.9806(4) 0.071(3) Uani 1 1 d . A . H74A H 0.0653 0.8008 0.9543 0.107 Uiso 1 1 calc R . . H74B H 0.1076 0.8625 1.0048 0.107 Uiso 1 1 calc R . . H74C H 0.0073 0.9012 0.9619 0.107 Uiso 1 1 calc R . . N15 N -0.3886(6) 0.5732(4) 1.1247(2) 0.0398(14) Uani 1 1 d . A . N25 N -0.2934(8) 0.5371(5) 1.1406(3) 0.056(2) Uani 1 1 d . . . N35 N -0.2058(9) 0.5059(6) 1.1563(3) 0.076(2) Uani 1 1 d . A . N16 N -0.4814(6) 0.7146(4) 1.0624(2) 0.0363(13) Uani 1 1 d . A . N26 N -0.5736(8) 0.7630(6) 1.0558(3) 0.057(2) Uani 1 1 d . . . N36 N -0.6560(10) 0.8075(7) 1.0522(4) 0.086(3) Uani 1 1 d . A . N17 N -0.4160(7) 0.7509(5) 0.9465(2) 0.0482(16) Uani 1 1 d D A . N27 N -0.5023(10) 0.7890(8) 0.9296(5) 0.034(3) Uiso 0.50 1 d PD A 1 N37 N -0.5824(12) 0.8321(10) 0.9136(5) 0.053(3) Uiso 0.50 1 d PD A 1 N27' N -0.438(2) 0.8176(12) 0.9218(8) 0.102(7) Uiso 0.50 1 d PD A 2 N37' N -0.418(4) 0.881(2) 0.8957(16) 0.230(18) Uiso 0.50 1 d PD A 2 N18 N -0.4885(7) 0.6065(5) 0.8536(2) 0.0512(17) Uani 1 1 d . . . N28 N -0.4839(6) 0.6654(5) 0.8198(3) 0.0528(17) Uani 1 1 d . . . N38 N -0.4802(9) 0.7195(6) 0.7874(3) 0.086(3) Uani 1 1 d . A . O19 O -0.3653(5) 0.8893(4) 1.0401(2) 0.0513(14) Uani 1 1 d . A . H19 H -0.3564 0.8916 1.0796 0.062 Uiso 1 1 d R . . C19 C -0.3116(19) 0.9689(8) 1.0226(6) 0.157(8) Uani 1 1 d . . . H19A H -0.3506 1.0220 1.0394 0.235 Uiso 1 1 calc R A . H19B H -0.3227 0.9733 0.9835 0.235 Uiso 1 1 calc R . . H19C H -0.2231 0.9681 1.0322 0.235 Uiso 1 1 calc R . . O29 O -0.4542(5) 0.5332(4) 1.23461(19) 0.0510(14) Uani 1 1 d . . . H29 H -0.4264 0.5977 1.2398 0.061 Uiso 1 1 d R . . C29 C -0.4998(12) 0.5057(12) 1.2839(5) 0.123(6) Uani 1 1 d . . . H29A H -0.4351 0.5128 1.3119 0.185 Uiso 1 1 calc R . . H29B H -0.5252 0.4409 1.2818 0.185 Uiso 1 1 calc R . . H29C H -0.5711 0.5439 1.2925 0.185 Uiso 1 1 calc R . . O39 O -0.2295(6) 0.6357(5) 0.8878(3) 0.0692(18) Uani 1 1 d . A . C39 C -0.1926(18) 0.7150(13) 0.8617(8) 0.065(5) Uiso 0.50 1 d P A 1 H39A H -0.1114 0.7049 0.8465 0.098 Uiso 0.50 1 calc PR A 1 H39B H -0.1875 0.7662 0.8873 0.098 Uiso 0.50 1 calc PR A 1 H39C H -0.2529 0.7300 0.8329 0.098 Uiso 0.50 1 calc PR A 1 O49 O -0.2644(13) 0.9642(10) 0.8655(6) 0.076(4) Uiso 0.50 1 d P D 1 C49 C -0.147(3) 1.018(2) 0.8992(12) 0.113(9) Uiso 0.50 1 d P D 1 O110 O -0.0933(12) 0.8245(9) 0.8342(5) 0.070(3) Uiso 0.50 1 d P E 2 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 0.0594(6) 0.0439(6) 0.0257(5) 0.0053(4) -0.0124(4) -0.0103(5) Ni2 0.0598(6) 0.0415(6) 0.0265(5) -0.0038(4) -0.0093(4) -0.0094(5) Ni3 0.0980(9) 0.0570(7) 0.0225(5) -0.0049(5) -0.0012(5) -0.0412(6) Ni4 0.0498(6) 0.0305(5) 0.0303(5) 0.0010(4) -0.0092(4) -0.0041(4) Ni5 0.0702(7) 0.0490(6) 0.0245(5) 0.0013(4) -0.0040(4) -0.0231(5) O12 0.057(4) 0.057(4) 0.051(3) 0.019(3) -0.009(3) -0.011(3) C22 0.043(5) 0.066(6) 0.071(6) 0.025(5) -0.013(4) 0.004(4) C32 0.045(5) 0.065(6) 0.062(5) 0.018(5) -0.006(4) 0.008(4) C42 0.050(5) 0.061(5) 0.034(4) 0.006(4) -0.023(4) -0.005(4) O52 0.051(3) 0.051(3) 0.032(3) 0.002(2) -0.005(2) -0.003(3) C62 0.058(7) 0.083(8) 0.164(13) 0.044(8) 0.014(7) 0.005(6) C72 0.072(6) 0.065(6) 0.060(6) -0.009(5) -0.001(5) -0.006(5) O13 0.059(3) 0.044(3) 0.030(3) -0.007(2) -0.015(2) -0.004(2) C23 0.051(5) 0.052(5) 0.032(4) -0.012(4) -0.007(3) -0.003(4) C33 0.062(5) 0.047(5) 0.037(4) -0.014(4) -0.008(4) -0.005(4) C43 0.048(5) 0.049(5) 0.039(4) -0.014(4) -0.002(3) -0.003(4) O53 0.059(3) 0.046(3) 0.034(3) -0.005(2) -0.008(2) -0.007(3) C63 0.087(7) 0.055(5) 0.038(4) -0.016(4) -0.011(4) 0.002(5) C73 0.076(6) 0.046(5) 0.059(5) -0.011(4) -0.009(5) -0.012(4) O14 0.052(3) 0.030(3) 0.035(3) -0.001(2) -0.009(2) -0.002(2) C24 0.046(5) 0.040(4) 0.050(5) -0.010(4) -0.015(4) 0.006(4) C34 0.045(5) 0.065(6) 0.055(5) -0.013(4) -0.010(4) 0.000(4) C44 0.043(5) 0.062(6) 0.058(5) 0.003(4) -0.007(4) 0.000(4) O54 0.051(3) 0.054(3) 0.041(3) 0.000(3) -0.002(2) -0.003(3) C64 0.058(5) 0.072(6) 0.046(5) -0.003(4) -0.019(4) 0.002(5) C74 0.059(6) 0.087(8) 0.067(6) 0.011(5) -0.002(5) -0.007(5) N15 0.057(4) 0.038(4) 0.023(3) -0.002(3) -0.010(3) -0.011(3) N25 0.084(6) 0.057(5) 0.026(3) 0.003(3) -0.016(4) -0.020(4) N35 0.103(7) 0.079(6) 0.045(5) 0.011(4) -0.018(5) -0.016(5) N16 0.040(3) 0.042(4) 0.026(3) 0.001(3) -0.009(2) -0.001(3) N26 0.073(6) 0.061(5) 0.036(4) -0.010(4) 0.001(4) -0.019(4) N36 0.083(7) 0.089(7) 0.084(7) -0.015(6) -0.004(5) -0.011(6) N17 0.068(4) 0.042(4) 0.034(3) 0.008(3) -0.008(3) -0.008(3) N18 0.070(5) 0.054(4) 0.029(3) 0.002(3) -0.006(3) -0.014(4) N28 0.060(4) 0.063(5) 0.035(4) 0.004(4) -0.005(3) -0.012(4) N38 0.116(8) 0.082(6) 0.060(5) 0.041(5) -0.001(5) -0.022(5) O19 0.077(4) 0.035(3) 0.042(3) -0.001(2) -0.001(3) -0.002(3) C19 0.32(2) 0.044(7) 0.110(11) -0.006(7) 0.092(14) -0.025(10) O29 0.071(4) 0.052(3) 0.028(3) 0.007(2) -0.010(2) -0.011(3) C29 0.099(9) 0.203(17) 0.065(7) 0.047(9) -0.024(7) -0.051(10) O39 0.056(4) 0.079(5) 0.072(4) 0.034(4) 0.002(3) -0.010(3) _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 O12 1.994(6) . ? Ni1 O52 2.028(6) . ? Ni1 O41 2.074(9) 3_467 ? Ni1 N18 2.083(7) 3_467 ? Ni1 O29 2.085(5) . ? Ni1 N15 2.095(6) . ? Ni1 N1A 2.109(11) 3_467 ? Ni2 O53 1.992(5) . ? Ni2 O13 2.013(5) . ? Ni2 N16 2.087(6) . ? Ni2 N15 2.093(6) . ? Ni2 O52 2.141(5) . ? Ni2 O14 2.151(5) . ? Ni3 O31 1.874(9) . ? Ni3 O21 1.894(11) . ? Ni3 O41 1.894(10) 3_467 ? Ni3 O31 1.934(9) 3_467 ? Ni3 N16 2.130(6) . ? Ni3 N15 2.140(6) . ? Ni3 N1A 2.208(12) 3_467 ? Ni3 N1B 2.236(12) 3_467 ? Ni3 O1C 2.241(13) . ? Ni3 N1B 2.316(12) . ? Ni4 O54 1.986(5) . ? Ni4 O14 2.038(5) . ? Ni4 O21 2.055(9) . ? Ni4 N17 2.063(6) . ? Ni4 N16 2.103(6) . ? Ni4 O19 2.105(5) . ? Ni4 O1C 2.155(13) . ? Ni5 O41 1.906(10) . ? Ni5 O21 1.987(10) . ? Ni5 O31 2.026(8) 3_467 ? Ni5 N17 2.058(7) . ? Ni5 N18 2.091(6) . ? Ni5 O39 2.111(6) . ? Ni5 O1C 2.168(13) . ? Ni5 N1B 2.247(13) 3_467 ? Ni5 N1A 2.253(12) . ? C11 C51 1.539(19) . ? C11 C41 1.548(11) . ? C11 C31 1.551(11) . ? C11 C21 1.558(10) . ? C21 O21 1.427(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C31 O31 1.414(12) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? O31 Ni3 1.934(9) 3_467 ? O31 Ni5 2.026(8) 3_467 ? C41 O41 1.412(12) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? O41 Ni3 1.894(10) 3_467 ? O41 Ni1 2.074(9) 3_467 ? C51 C61 1.491(19) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? N1A N2A 1.249(17) . ? N1A Ni1 2.109(11) 3_467 ? N1A Ni3 2.208(12) 3_467 ? N2A N3A 1.123(17) . ? N1B N2B 1.234(16) . ? N1B Ni3 2.236(12) 3_467 ? N1B Ni5 2.247(13) 3_467 ? N2B N3B 1.139(17) . ? O1C C1C 1.36(2) . ? C1C H1C1 0.9800 . ? C1C H1C2 0.9800 . ? C1C H1C3 0.9800 . ? O12 C22 1.281(11) . ? C22 C32 1.413(13) . ? C22 C62 1.483(13) . ? C32 C42 1.409(12) . ? C32 H32 0.9500 . ? C42 O52 1.274(10) . ? C42 C72 1.497(12) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? O13 C23 1.281(9) . ? C23 C33 1.396(11) . ? C23 C63 1.501(11) . ? C33 C43 1.393(11) . ? C33 H33 0.9500 . ? C43 O53 1.285(9) . ? C43 C73 1.479(12) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? O14 C24 1.284(9) . ? C24 C34 1.376(12) . ? C24 C64 1.507(11) . ? C34 C44 1.388(12) . ? C34 H34 0.9500 . ? C44 O54 1.275(9) . ? C44 C74 1.527(12) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? N15 N25 1.212(10) . ? N25 N35 1.110(11) . ? N16 N26 1.228(11) . ? N26 N36 1.102(11) . ? N17 N27 1.153(11) . ? N17 N27' 1.167(13) . ? N27 N37 1.132(15) . ? N27' N37' 1.149(17) . ? N18 N28 1.204(9) . ? N18 Ni1 2.083(7) 3_467 ? N28 N38 1.127(10) . ? O19 C19 1.371(13) . ? O19 H19 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O29 C29 1.399(12) . ? O29 H29 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? O39 C39 1.39(2) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? O49 C49 1.69(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Ni1 O52 92.6(2) . . ? O12 Ni1 O41 97.7(3) . 3_467 ? O52 Ni1 O41 98.7(3) . 3_467 ? O12 Ni1 N18 93.5(3) . 3_467 ? O52 Ni1 N18 173.2(2) . 3_467 ? O41 Ni1 N18 77.3(3) 3_467 3_467 ? O12 Ni1 O29 95.7(2) . . ? O52 Ni1 O29 88.8(2) . . ? O41 Ni1 O29 164.4(3) 3_467 . ? N18 Ni1 O29 93.8(2) 3_467 . ? O12 Ni1 N15 173.6(3) . . ? O52 Ni1 N15 82.5(2) . . ? O41 Ni1 N15 79.0(3) 3_467 . ? N18 Ni1 N15 91.2(3) 3_467 . ? O29 Ni1 N15 88.5(2) . . ? O12 Ni1 N1A 87.4(4) . 3_467 ? O52 Ni1 N1A 88.7(4) . 3_467 ? O41 Ni1 N1A 14.7(3) 3_467 3_467 ? N18 Ni1 N1A 88.4(4) 3_467 3_467 ? O29 Ni1 N1A 176.1(3) . 3_467 ? N15 Ni1 N1A 88.3(4) . 3_467 ? O53 Ni2 O13 92.1(2) . . ? O53 Ni2 N16 94.0(2) . . ? O13 Ni2 N16 171.3(2) . . ? O53 Ni2 N15 173.2(2) . . ? O13 Ni2 N15 92.4(2) . . ? N16 Ni2 N15 82.1(2) . . ? O53 Ni2 O52 105.6(2) . . ? O13 Ni2 O52 84.6(2) . . ? N16 Ni2 O52 87.9(2) . . ? N15 Ni2 O52 79.9(2) . . ? O53 Ni2 O14 84.7(2) . . ? O13 Ni2 O14 106.7(2) . . ? N16 Ni2 O14 80.0(2) . . ? N15 Ni2 O14 89.1(2) . . ? O52 Ni2 O14 164.67(19) . . ? O31 Ni3 O21 101.6(4) . . ? O31 Ni3 O41 72.1(4) . 3_467 ? O21 Ni3 O41 173.3(4) . 3_467 ? O31 Ni3 O31 70.1(5) . 3_467 ? O21 Ni3 O31 76.7(4) . 3_467 ? O41 Ni3 O31 98.8(4) 3_467 3_467 ? O31 Ni3 N16 174.8(3) . . ? O21 Ni3 N16 81.5(3) . . ? O41 Ni3 N16 104.7(4) 3_467 . ? O31 Ni3 N16 106.9(3) 3_467 . ? O31 Ni3 N15 103.3(3) . . ? O21 Ni3 N15 101.9(4) . . ? O41 Ni3 N15 82.0(3) 3_467 . ? O31 Ni3 N15 172.5(3) 3_467 . ? N16 Ni3 N15 80.0(2) . . ? O31 Ni3 N1A 82.8(4) . 3_467 ? O21 Ni3 N1A 170.9(4) . 3_467 ? O41 Ni3 N1A 12.2(4) 3_467 3_467 ? O31 Ni3 N1A 97.7(4) 3_467 3_467 ? N16 Ni3 N1A 93.5(4) . 3_467 ? N15 Ni3 N1A 84.6(3) . 3_467 ? O31 Ni3 N1B 82.8(5) . 3_467 ? O21 Ni3 N1B 83.5(4) . 3_467 ? O41 Ni3 N1B 93.4(4) 3_467 3_467 ? O31 Ni3 N1B 16.4(3) 3_467 3_467 ? N16 Ni3 N1B 93.6(3) . 3_467 ? N15 Ni3 N1B 170.8(4) . 3_467 ? N1A Ni3 N1B 89.3(5) 3_467 3_467 ? O31 Ni3 O1C 98.0(4) . . ? O21 Ni3 O1C 8.3(5) . . ? O41 Ni3 O1C 168.8(5) 3_467 . ? O31 Ni3 O1C 82.1(4) 3_467 . ? N16 Ni3 O1C 85.6(4) . . ? N15 Ni3 O1C 95.7(4) . . ? N1A Ni3 O1C 179.0(5) 3_467 . ? N1B Ni3 O1C 90.3(5) 3_467 . ? O31 Ni3 N1B 13.7(4) . . ? O21 Ni3 N1B 94.5(4) . . ? O41 Ni3 N1B 79.6(5) 3_467 . ? O31 Ni3 N1B 79.4(5) 3_467 . ? N16 Ni3 N1B 171.4(4) . . ? N15 Ni3 N1B 93.5(3) . . ? N1A Ni3 N1B 91.3(5) 3_467 . ? N1B Ni3 N1B 93.6(4) 3_467 . ? O1C Ni3 N1B 89.6(5) . . ? O54 Ni4 O14 92.2(2) . . ? O54 Ni4 O21 103.2(3) . . ? O14 Ni4 O21 94.9(3) . . ? O54 Ni4 N17 91.6(2) . . ? O14 Ni4 N17 172.8(2) . . ? O21 Ni4 N17 78.3(3) . . ? O54 Ni4 N16 174.3(2) . . ? O14 Ni4 N16 82.3(2) . . ? O21 Ni4 N16 78.6(3) . . ? N17 Ni4 N16 94.0(2) . . ? O54 Ni4 O19 92.0(2) . . ? O14 Ni4 O19 89.2(2) . . ? O21 Ni4 O19 164.1(4) . . ? N17 Ni4 O19 96.8(2) . . ? N16 Ni4 O19 86.8(2) . . ? O54 Ni4 O1C 92.6(4) . . ? O14 Ni4 O1C 89.4(4) . . ? O21 Ni4 O1C 12.2(4) . . ? N17 Ni4 O1C 84.4(4) . . ? N16 Ni4 O1C 88.5(4) . . ? O19 Ni4 O1C 175.2(4) . . ? O41 Ni5 O21 96.4(4) . . ? O41 Ni5 O31 68.5(4) . 3_467 ? O21 Ni5 O31 72.5(4) . 3_467 ? O41 Ni5 N17 170.4(4) . . ? O21 Ni5 N17 79.9(3) . . ? O31 Ni5 N17 101.8(3) 3_467 . ? O41 Ni5 N18 80.9(3) . . ? O21 Ni5 N18 169.9(4) . . ? O31 Ni5 N18 97.4(3) 3_467 . ? N17 Ni5 N18 101.1(3) . . ? O41 Ni5 O39 96.1(4) . . ? O21 Ni5 O39 101.4(4) . . ? O31 Ni5 O39 162.2(3) 3_467 . ? N17 Ni5 O39 93.4(3) . . ? N18 Ni5 O39 88.6(3) . . ? O41 Ni5 O1C 94.0(4) . . ? O21 Ni5 O1C 11.6(4) . . ? O31 Ni5 O1C 82.0(4) 3_467 . ? N17 Ni5 O1C 84.1(4) . . ? N18 Ni5 O1C 174.7(4) . . ? O39 Ni5 O1C 90.5(4) . . ? O41 Ni5 N1B 81.2(4) . 3_467 ? O21 Ni5 N1B 81.1(4) . 3_467 ? O31 Ni5 N1B 16.9(3) 3_467 3_467 ? N17 Ni5 N1B 89.4(4) . 3_467 ? N18 Ni5 N1B 88.8(4) . 3_467 ? O39 Ni5 N1B 176.5(4) . 3_467 ? O1C Ni5 N1B 91.9(5) . 3_467 ? O41 Ni5 N1A 11.3(4) . . ? O21 Ni5 N1A 94.7(4) . . ? O31 Ni5 N1A 78.5(4) 3_467 . ? N17 Ni5 N1A 174.2(3) . . ? N18 Ni5 N1A 84.5(3) . . ? O39 Ni5 N1A 85.5(4) . . ? O1C Ni5 N1A 90.2(5) . . ? N1B Ni5 N1A 92.0(4) 3_467 . ? C51 C11 C41 105.8(8) . . ? C51 C11 C31 107.3(8) . . ? C41 C11 C31 111.7(8) . . ? C51 C11 C21 108.6(8) . . ? C41 C11 C21 111.7(8) . . ? C31 C11 C21 111.3(8) . . ? O21 C21 C11 113.3(9) . . ? O21 C21 H21A 108.9 . . ? C11 C21 H21A 108.9 . . ? O21 C21 H21B 108.9 . . ? C11 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 O21 Ni3 110.7(7) . . ? C21 O21 Ni5 112.7(7) . . ? Ni3 O21 Ni5 106.5(5) . . ? C21 O21 Ni4 119.8(7) . . ? Ni3 O21 Ni4 104.5(4) . . ? Ni5 O21 Ni4 101.4(4) . . ? O31 C31 C11 116.5(10) . . ? O31 C31 H31A 108.2 . . ? C11 C31 H31A 108.2 . . ? O31 C31 H31B 108.2 . . ? C11 C31 H31B 108.2 . . ? H31A C31 H31B 107.3 . . ? C31 O31 Ni3 109.4(7) . . ? C31 O31 Ni3 108.6(7) . 3_467 ? Ni3 O31 Ni3 109.9(5) . 3_467 ? C31 O31 Ni5 117.8(7) . 3_467 ? Ni3 O31 Ni5 107.3(4) . 3_467 ? Ni3 O31 Ni5 103.5(4) 3_467 3_467 ? O41 C41 C11 115.9(10) . . ? O41 C41 H41A 108.3 . . ? C11 C41 H41A 108.3 . . ? O41 C41 H41B 108.3 . . ? C11 C41 H41B 108.3 . . ? H41A C41 H41B 107.4 . . ? C41 O41 Ni3 110.1(8) . 3_467 ? C41 O41 Ni5 111.5(8) . . ? Ni3 O41 Ni5 111.6(5) 3_467 . ? C41 O41 Ni1 117.4(8) . 3_467 ? Ni3 O41 Ni1 103.2(4) 3_467 3_467 ? Ni5 O41 Ni1 102.6(4) . 3_467 ? C61 C51 C11 119.3(10) . . ? C61 C51 H51A 107.5 . . ? C11 C51 H51A 107.5 . . ? C61 C51 H51B 107.5 . . ? C11 C51 H51B 107.5 . . ? H51A C51 H51B 107.0 . . ? C51 C61 H61A 109.5 . . ? C51 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C51 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N2A N1A Ni1 121.0(10) . 3_467 ? N2A N1A Ni3 126.9(10) . 3_467 ? Ni1 N1A Ni3 92.2(5) 3_467 3_467 ? N2A N1A Ni5 126.1(10) . . ? Ni1 N1A Ni5 90.8(4) 3_467 . ? Ni3 N1A Ni5 89.6(5) 3_467 . ? N3A N2A N1A 171(2) . . ? N2B N1B Ni3 132.5(10) . 3_467 ? N2B N1B Ni5 118.6(9) . 3_467 ? Ni3 N1B Ni5 87.9(5) 3_467 3_467 ? N2B N1B Ni3 130.1(10) . . ? Ni3 N1B Ni3 86.4(4) 3_467 . ? Ni5 N1B Ni3 87.1(5) 3_467 . ? N3B N2B N1B 179.7(19) . . ? C1C O1C Ni4 118.6(11) . . ? C1C O1C Ni5 129.7(10) . . ? Ni4 O1C Ni5 92.7(5) . . ? C1C O1C Ni3 125.0(11) . . ? Ni4 O1C Ni3 90.6(5) . . ? Ni5 O1C Ni3 89.7(5) . . ? O1C C1C H1C1 109.5 . . ? O1C C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? O1C C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? C22 O12 Ni1 125.0(6) . . ? O12 C22 C32 125.5(8) . . ? O12 C22 C62 117.0(9) . . ? C32 C22 C62 117.5(9) . . ? C42 C32 C22 126.3(9) . . ? C42 C32 H32 116.8 . . ? C22 C32 H32 116.8 . . ? O52 C42 C32 125.4(8) . . ? O52 C42 C72 119.0(8) . . ? C32 C42 C72 115.6(8) . . ? C42 O52 Ni1 124.3(5) . . ? C42 O52 Ni2 135.6(5) . . ? Ni1 O52 Ni2 98.7(2) . . ? C22 C62 H62A 109.5 . . ? C22 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C22 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C42 C72 H72A 109.5 . . ? C42 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C42 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C23 O13 Ni2 124.9(5) . . ? O13 C23 C33 125.1(7) . . ? O13 C23 C63 115.6(7) . . ? C33 C23 C63 119.2(7) . . ? C43 C33 C23 126.6(7) . . ? C43 C33 H33 116.7 . . ? C23 C33 H33 116.7 . . ? O53 C43 C33 125.3(8) . . ? O53 C43 C73 115.1(7) . . ? C33 C43 C73 119.6(7) . . ? C43 O53 Ni2 124.7(5) . . ? C23 C63 H63A 109.5 . . ? C23 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C23 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C43 C73 H73A 109.5 . . ? C43 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C43 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C24 O14 Ni4 123.8(5) . . ? C24 O14 Ni2 136.1(5) . . ? Ni4 O14 Ni2 98.5(2) . . ? O14 C24 C34 125.0(7) . . ? O14 C24 C64 116.1(7) . . ? C34 C24 C64 118.9(7) . . ? C24 C34 C44 128.4(8) . . ? C24 C34 H34 115.8 . . ? C44 C34 H34 115.8 . . ? O54 C44 C34 125.1(8) . . ? O54 C44 C74 115.9(8) . . ? C34 C44 C74 119.0(8) . . ? C44 O54 Ni4 125.0(5) . . ? C24 C64 H64A 109.5 . . ? C24 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C24 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C44 C74 H74A 109.5 . . ? C44 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C44 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N25 N15 Ni2 115.3(5) . . ? N25 N15 Ni1 116.7(5) . . ? Ni2 N15 Ni1 98.1(3) . . ? N25 N15 Ni3 127.7(5) . . ? Ni2 N15 Ni3 98.7(3) . . ? Ni1 N15 Ni3 94.6(3) . . ? N35 N25 N15 178.1(9) . . ? N26 N16 Ni2 115.7(5) . . ? N26 N16 Ni4 116.9(5) . . ? Ni2 N16 Ni4 98.5(2) . . ? N26 N16 Ni3 126.2(5) . . ? Ni2 N16 Ni3 99.2(3) . . ? Ni4 N16 Ni3 95.1(3) . . ? N36 N26 N16 176.8(9) . . ? N27 N17 N27' 42.5(11) . . ? N27 N17 Ni5 118.4(8) . . ? N27' N17 Ni5 134.9(12) . . ? N27 N17 Ni4 133.2(8) . . ? N27' N17 Ni4 123.3(13) . . ? Ni5 N17 Ni4 98.8(3) . . ? N37 N27 N17 175.1(15) . . ? N37' N27' N17 157(3) . . ? N28 N18 Ni1 123.1(6) . 3_467 ? N28 N18 Ni5 124.1(5) . . ? Ni1 N18 Ni5 96.2(3) 3_467 . ? N38 N28 N18 178.8(9) . . ? C19 O19 Ni4 128.8(7) . . ? C19 O19 H19 105.2 . . ? Ni4 O19 H19 104.7 . . ? O19 C19 H19A 109.5 . . ? O19 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O19 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C29 O29 Ni1 126.1(6) . . ? C29 O29 H29 105.7 . . ? Ni1 O29 H29 105.5 . . ? O29 C29 H29A 109.5 . . ? O29 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O29 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C39 O39 Ni5 127.8(9) . . ? O39 C39 H39A 109.5 . . ? O39 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O39 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.333 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.125