#------------------------------------------------------------------------------ #$Date: 2016-08-07 11:22:46 +0300 (Sun, 07 Aug 2016) $ #$Revision: 185227 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/51/7225191.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7225191 loop_ _publ_author_name 'Beldon, Patrick J.' 'Henke, Sebastian' 'Monserrat, Bartomeu' 'Tominaka, Satoshi' 'Stock, Norbert' 'Cheetham, Anthony K.' _publ_section_title ; Transition metal coordination complexes of chrysazin ; _journal_issue 27 _journal_name_full CrystEngComm _journal_page_first 5121 _journal_paper_doi 10.1039/C5CE00792E _journal_volume 18 _journal_year 2016 _chemical_formula_moiety 'C76 H64 N4 Ni6 O28, 4(C3 H7 N O)' _chemical_formula_sum 'C88 H92 N8 Ni6 O32' _chemical_formula_weight 2125.95 _chemical_name_systematic 'tetra(acetato)-tetra(chrysazinato)-tetra(N,N-dimethylformamide)-hexa-nickel(II) bis(N,N-dimethylformamide) solvate' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2015-08-17 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _audit_update_record ; 2016-04-20 deposited with the CCDC. 2016-05-11 downloaded from the CCDC. ; _cell_angle_alpha 95.504(3) _cell_angle_beta 97.873(4) _cell_angle_gamma 95.172(4) _cell_formula_units_Z 1 _cell_length_a 9.7302(6) _cell_length_b 13.4388(5) _cell_length_c 17.0848(7) _cell_measurement_reflns_used 5065 _cell_measurement_temperature 200.00(14) _cell_measurement_theta_max 70.9260 _cell_measurement_theta_min 4.6070 _cell_volume 2190.67(18) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 200.00(14) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1183 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.8595 _diffrn_measured_fraction_theta_max 0.8311 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0645062000 _diffrn_orient_matrix_UB_12 0.0358257000 _diffrn_orient_matrix_UB_13 0.0866883000 _diffrn_orient_matrix_UB_21 0.0535171000 _diffrn_orient_matrix_UB_22 0.1016696000 _diffrn_orient_matrix_UB_23 -0.0253853000 _diffrn_orient_matrix_UB_31 -0.1371323000 _diffrn_orient_matrix_UB_32 0.0423122000 _diffrn_orient_matrix_UB_33 0.0151042000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_unetI/netI 0.0411 _diffrn_reflns_Laue_measured_fraction_full 0.854 _diffrn_reflns_Laue_measured_fraction_max 0.831 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 12949 _diffrn_reflns_point_group_measured_fraction_full 0.854 _diffrn_reflns_point_group_measured_fraction_max 0.831 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.309 _diffrn_reflns_theta_min 3.322 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.175 _exptl_absorpt_correction_T_max 0.933 _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.611 _exptl_crystal_F_000 1100 _exptl_crystal_size_max 0.2686 _exptl_crystal_size_mid 0.1263 _exptl_crystal_size_min 0.0446 _refine_diff_density_max 0.861 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.097 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 623 _refine_ls_number_reflns 7058 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0598 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+3.2535P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1660 _refine_ls_wR_factor_ref 0.1810 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5763 _reflns_number_total 7058 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5ce00792e2.cif _cod_data_source_block NiChrys-2 _cod_depositor_comments 'Adding full bibliography for 7225182--7225192.cif.' _cod_original_cell_volume 2190.66(18) _cod_database_code 7225191 _shelxl_version_number 2014/6 _chemical_oxdiff_formula 'Ni6 C88 H92 O32 N8' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 85.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C42-O16 = C42-O17 1.25 with sigma of 0.01 3. Others Fixed Sof: O16(0.5) O17(0.5) H42A(0.5) H42(0.5) 4.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C26(H26), C27(H27), C28(H28), C33(H33), C36(H36), C39(H39), C42(H42A), C42(H42) 4.b Idealised Me refined as rotating group: C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B, H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A, H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C) ; _shelx_res_file ; TITL NiChrys-1 in P-1 CELL 1.54184 9.730214 13.438767 17.084755 95.5039 97.8727 95.1723 ZERR 1 0.000557 0.000463 0.000732 0.0032 0.0043 0.0037 LATT 1 SFAC C H N O Ni UNIT 88 92 8 32 6 DFIX 1.25 0.01 C42 O16 C42 O17 L.S. 4 0 0 PLAN 20 fmap 2 53 acta OMIT -3 -2 1 OMIT 5 0 16 REM C:/Users/pjb76/Desktop/Dropbox/Research%20outlines/Cambridge/Chrysazi REM n%20high-throughput/Chrysazin%20paper/CIFs/Post-review/NiChrys-2/NiChrys-2 REM .hkl WGHT 0.103400 3.253500 FVAR 2.53111 NI1 5 0.665098 -0.006157 0.019439 11.00000 0.02592 0.02232 = 0.03815 0.00332 0.00734 0.00323 NI2 5 0.541060 0.136928 0.121608 11.00000 0.02576 0.02285 = 0.03676 0.00425 0.00825 0.00496 NI3 5 0.387206 0.265597 0.225722 11.00000 0.03106 0.02613 = 0.03960 0.00211 0.00909 0.00497 O1 4 0.785890 -0.108409 0.049306 11.00000 0.02724 0.02823 = 0.04426 0.00451 0.01055 0.00656 O2 4 0.633901 0.013237 0.135209 11.00000 0.03259 0.02435 = 0.03124 0.00539 0.00551 0.00926 O3 4 0.537322 0.161158 0.235860 11.00000 0.03600 0.02825 = 0.03474 0.00465 0.00565 0.00947 O4 4 0.728493 -0.203691 0.379067 11.00000 0.15431 0.07328 = 0.07027 0.04184 0.05181 0.06665 O5 4 0.520105 0.106963 0.003723 11.00000 0.02097 0.02031 = 0.03777 0.00636 0.00521 0.00052 O6 4 0.445035 0.260475 0.112378 11.00000 0.03109 0.02698 = 0.03471 0.00578 0.00922 0.00866 O7 4 0.261594 0.363668 0.189058 11.00000 0.03277 0.03298 = 0.04677 0.00611 0.01361 0.01119 O8 4 0.369488 0.488924 -0.127207 11.00000 0.06676 0.04360 = 0.06328 0.02535 0.02346 0.02332 O9 4 0.817157 0.106701 0.037482 11.00000 0.02788 0.02641 = 0.04787 -0.00018 0.00839 -0.00023 O10 4 0.734011 0.213343 0.125365 11.00000 0.02595 0.02984 = 0.04915 0.00048 0.00991 0.00201 O11 4 0.341263 0.053326 0.099662 11.00000 0.02469 0.02378 = 0.03952 0.00383 0.00782 0.00155 O12 4 0.241529 0.146810 0.186994 11.00000 0.02831 0.03161 = 0.04891 -0.00292 0.01351 0.00166 O13 4 0.535391 0.375939 0.278836 11.00000 0.03392 0.03409 = 0.05173 -0.00356 0.00831 -0.00164 O14 4 0.301098 0.271434 0.330592 11.00000 0.03936 0.04231 = 0.04419 0.00624 0.01372 0.01047 O15 4 0.913791 0.429672 0.568188 11.00000 0.07258 0.50680 = 0.25781 -0.11605 0.00114 0.06162 PART 1 O16 4 0.865130 0.210144 0.558024 10.50000 0.16425 0.14639 = 0.27826 0.05696 0.03975 0.01226 PART 0 PART 2 O17 4 0.979552 0.072843 0.531434 10.50000 0.14321 0.17264 = 0.15581 -0.04400 0.04616 0.02144 PART 0 N1 3 0.753035 0.454701 0.290138 11.00000 0.03930 0.03930 = 0.05422 -0.00229 0.01056 -0.00192 N2 3 0.094969 0.269707 0.380287 11.00000 0.04686 0.06608 = 0.04873 0.01037 0.01796 0.01499 N3 3 0.680418 0.405664 0.575450 11.00000 0.09657 0.09721 = 0.09801 -0.01912 0.01070 0.02965 N4 3 0.837399 0.077318 0.623762 11.00000 0.08879 0.06679 = 0.06620 0.00710 0.02190 0.00113 C1 1 0.811384 -0.143496 0.116932 11.00000 0.03107 0.02520 = 0.04298 0.00351 0.00181 0.00136 C2 1 0.902016 -0.221022 0.120080 11.00000 0.03594 0.03348 = 0.05352 0.00553 0.01162 0.01105 AFIX 43 H2 2 0.940067 -0.240760 0.074719 11.00000 -1.20000 AFIX 0 C3 1 0.935694 -0.267822 0.186811 11.00000 0.04218 0.03768 = 0.05843 0.01020 0.00659 0.01652 AFIX 43 H3 2 0.996842 -0.317151 0.186369 11.00000 -1.20000 AFIX 0 C4 1 0.878597 -0.241684 0.255190 11.00000 0.05776 0.04163 = 0.04881 0.01501 0.00637 0.01761 AFIX 43 H4 2 0.899045 -0.274885 0.300012 11.00000 -1.20000 AFIX 0 C5 1 0.791909 -0.166655 0.256253 11.00000 0.04661 0.03333 = 0.04702 0.00740 0.00668 0.01033 C6 1 0.757112 -0.112547 0.189318 11.00000 0.03168 0.02594 = 0.04589 0.00818 0.00540 0.00484 C7 1 0.673996 -0.029481 0.196888 11.00000 0.02815 0.02469 = 0.04226 0.00493 0.00536 -0.00026 C8 1 0.636960 0.008742 0.274099 11.00000 0.03300 0.03540 = 0.03747 0.00817 0.00589 0.00806 C9 1 0.666881 -0.048497 0.339944 11.00000 0.05870 0.04480 = 0.04319 0.01431 0.01112 0.01731 C10 1 0.728598 -0.144817 0.328509 11.00000 0.07293 0.04890 = 0.05105 0.01967 0.01686 0.02502 C11 1 0.573554 0.099835 0.289216 11.00000 0.03243 0.03174 = 0.03759 0.00633 0.00412 0.00387 C12 1 0.549977 0.128260 0.367164 11.00000 0.05885 0.04643 = 0.04069 0.00527 0.01212 0.02015 AFIX 43 H12 2 0.509503 0.187368 0.377326 11.00000 -1.20000 AFIX 0 C13 1 0.583853 0.072953 0.428639 11.00000 0.08294 0.06684 = 0.04033 0.00996 0.01795 0.03597 AFIX 43 H13 2 0.569445 0.095790 0.479704 11.00000 -1.20000 AFIX 0 C14 1 0.639976 -0.017647 0.414803 11.00000 0.08837 0.06565 = 0.04451 0.01993 0.01793 0.03818 AFIX 43 H14 2 0.659153 -0.057077 0.456021 11.00000 -1.20000 AFIX 0 C15 1 0.526859 0.186692 -0.040201 11.00000 0.02300 0.02656 = 0.03760 0.00694 0.00454 0.00362 C16 1 0.593838 0.176043 -0.107525 11.00000 0.03624 0.02911 = 0.04097 0.00443 0.01327 0.00717 AFIX 43 H16 2 0.640937 0.119729 -0.116316 11.00000 -1.20000 AFIX 0 C17 1 0.592223 0.245754 -0.160740 11.00000 0.04243 0.03512 = 0.04858 0.00961 0.01954 0.00463 AFIX 43 H17 2 0.639346 0.237239 -0.204341 11.00000 -1.20000 AFIX 0 C18 1 0.519949 0.329516 -0.149588 11.00000 0.04833 0.03136 = 0.04451 0.01337 0.01283 0.00699 AFIX 43 H18 2 0.513937 0.375251 -0.187152 11.00000 -1.20000 AFIX 0 C19 1 0.457371 0.344036 -0.082341 11.00000 0.03359 0.02376 = 0.04581 0.00700 0.00838 0.00310 C20 1 0.464386 0.276566 -0.023023 11.00000 0.02835 0.02362 = 0.04193 0.00739 0.00716 -0.00077 C21 1 0.409382 0.305773 0.051937 11.00000 0.02677 0.02288 = 0.03659 0.00528 0.00553 -0.00160 C22 1 0.323174 0.386461 0.057875 11.00000 0.03047 0.02247 = 0.04228 0.00549 0.00427 0.00213 C23 1 0.303299 0.447777 -0.006020 11.00000 0.03823 0.02452 = 0.04571 0.00476 0.00478 0.00379 C24 1 0.377350 0.432461 -0.075169 11.00000 0.04009 0.02904 = 0.04877 0.01169 0.00851 0.00597 C25 1 0.255761 0.409005 0.126977 11.00000 0.02862 0.02493 = 0.04424 0.00077 0.00647 0.00256 C26 1 0.169588 0.490653 0.124052 11.00000 0.03701 0.03013 = 0.05709 0.00394 0.01308 0.00943 AFIX 43 H26 2 0.122900 0.505916 0.166955 11.00000 -1.20000 AFIX 0 C27 1 0.152951 0.546498 0.061942 11.00000 0.04575 0.03234 = 0.06149 0.00814 0.01046 0.01721 AFIX 43 H27 2 0.095519 0.598159 0.062959 11.00000 -1.20000 AFIX 0 C28 1 0.221966 0.526543 -0.003584 11.00000 0.04648 0.03288 = 0.05516 0.01295 0.00807 0.01164 AFIX 43 H28 2 0.213013 0.566241 -0.045317 11.00000 -1.20000 AFIX 0 C29 1 0.825657 0.186215 0.084186 11.00000 0.02818 0.02600 = 0.04344 0.00845 0.00443 0.00314 C30 1 0.959437 0.255149 0.091137 11.00000 0.03112 0.03103 = 0.05859 0.00326 0.00892 0.00095 AFIX 137 H30A 2 0.993790 0.275832 0.146223 11.00000 -1.50000 H30B 2 0.941732 0.313240 0.064243 11.00000 -1.50000 H30C 2 1.027735 0.220146 0.067358 11.00000 -1.50000 AFIX 0 C31 1 0.236963 0.073583 0.135526 11.00000 0.03117 0.02408 = 0.04196 0.00616 0.01097 0.00533 C32 1 0.104629 0.005671 0.114704 11.00000 0.03126 0.03719 = 0.06359 -0.00472 0.01478 -0.00042 AFIX 137 H32A 2 0.049929 0.012734 0.157216 11.00000 -1.50000 H32B 2 0.125633 -0.062671 0.106623 11.00000 -1.50000 H32C 2 0.053020 0.023174 0.066852 11.00000 -1.50000 AFIX 0 C33 1 0.651549 0.386270 0.257244 11.00000 0.04026 0.03111 = 0.04539 0.00430 0.01286 0.00487 AFIX 43 H33 2 0.668130 0.342549 0.214783 11.00000 -1.20000 AFIX 0 C34 1 0.880815 0.467834 0.255527 11.00000 0.04425 0.05723 = 0.08280 0.00619 0.02013 -0.00622 AFIX 137 H34A 2 0.881602 0.527364 0.228631 11.00000 -1.50000 H34B 2 0.885684 0.410540 0.218243 11.00000 -1.50000 H34C 2 0.959637 0.474280 0.296825 11.00000 -1.50000 AFIX 0 C35 1 0.730535 0.530964 0.351477 11.00000 0.07126 0.08035 = 0.11029 -0.04897 0.03853 -0.02397 AFIX 137 H35A 2 0.816633 0.551666 0.386217 11.00000 -1.50000 H35B 2 0.662204 0.504031 0.381490 11.00000 -1.50000 H35C 2 0.697839 0.587792 0.327418 11.00000 -1.50000 AFIX 0 C36 1 0.171441 0.261924 0.322214 11.00000 0.04065 0.04123 = 0.04734 0.00701 0.01516 0.01216 AFIX 43 H36 2 0.124230 0.248144 0.270614 11.00000 -1.20000 AFIX 0 C37 1 -0.055762 0.252098 0.365156 11.00000 0.04761 0.10699 = 0.07833 0.02388 0.02912 0.02175 AFIX 137 H37A 2 -0.086408 0.196860 0.392430 11.00000 -1.50000 H37B 2 -0.085868 0.236414 0.309071 11.00000 -1.50000 H37C 2 -0.094968 0.311341 0.383932 11.00000 -1.50000 AFIX 0 C38 1 0.161094 0.294658 0.461578 11.00000 0.08575 0.20305 = 0.04313 0.00148 0.01825 0.01422 AFIX 137 H38A 2 0.161217 0.234912 0.488199 11.00000 -1.50000 H38B 2 0.110653 0.342419 0.488195 11.00000 -1.50000 H38C 2 0.255403 0.323242 0.462423 11.00000 -1.50000 AFIX 0 C39 1 0.796685 0.398525 0.539444 11.00000 0.12938 0.28138 = 0.15743 -0.01374 0.03558 0.10597 AFIX 43 H39 2 0.783754 0.366531 0.487848 11.00000 -1.20000 AFIX 0 C40 1 0.548924 0.361243 0.531126 11.00000 0.11058 0.26416 = 0.17247 -0.08843 -0.00242 -0.03685 AFIX 137 H40A 2 0.504834 0.314919 0.561770 11.00000 -1.50000 H40B 2 0.564667 0.326125 0.482046 11.00000 -1.50000 H40C 2 0.489680 0.413094 0.520035 11.00000 -1.50000 AFIX 0 C41 1 0.688283 0.451652 0.654653 11.00000 0.15188 0.15359 = 0.10271 -0.02875 0.02144 0.06467 AFIX 137 H41A 2 0.748090 0.417235 0.689923 11.00000 -1.50000 H41B 2 0.596677 0.447974 0.669800 11.00000 -1.50000 H41C 2 0.725393 0.520797 0.657714 11.00000 -1.50000 AFIX 0 C42 1 0.898269 0.121910 0.568723 11.00000 0.12003 0.08421 = 0.09377 0.00707 0.03455 -0.00583 PART 2 AFIX 43 H42A 2 0.881671 0.186699 0.558081 10.50000 -1.20000 AFIX 43 PART 0 PART 1 H42 2 0.960442 0.090882 0.540182 10.50000 -1.20000 AFIX 0 PART 0 C43 1 0.751707 0.128308 0.671764 11.00000 0.10422 0.17655 = 0.11137 -0.03143 0.04136 0.01393 AFIX 137 H43A 2 0.746396 0.195377 0.657494 11.00000 -1.50000 H43B 2 0.791047 0.131054 0.726714 11.00000 -1.50000 H43C 2 0.659796 0.092934 0.663509 11.00000 -1.50000 AFIX 0 C44 1 0.870773 -0.022230 0.637136 11.00000 0.20047 0.07790 = 0.13135 0.03197 0.04771 0.03790 AFIX 137 H44A 2 0.919210 -0.048274 0.595613 11.00000 -1.50000 H44B 2 0.786330 -0.065062 0.637211 11.00000 -1.50000 H44C 2 0.929079 -0.019871 0.687520 11.00000 -1.50000 AFIX 0 HKLF 4 REM NiChrys-1 in P-1 REM R1 = 0.0598 for 5763 Fo > 4sig(Fo) and 0.0719 for all 7058 data REM 623 parameters refined using 2 restraints END WGHT 0.1034 3.2535 REM Highest difference peak 0.861, deepest hole -0.541, 1-sigma level 0.097 Q1 1 0.5311 0.1209 0.0592 11.00000 0.05 0.86 Q2 1 0.3481 0.0266 0.0439 11.00000 0.05 0.72 Q3 1 0.6868 0.1999 0.6512 11.00000 0.05 0.70 Q4 1 0.5575 0.1514 0.1914 11.00000 0.05 0.67 Q5 1 0.1987 0.1412 0.0816 11.00000 0.05 0.55 Q6 1 0.7285 0.0010 0.2011 11.00000 0.05 0.54 Q7 1 0.6841 0.0011 0.0915 11.00000 0.05 0.54 Q8 1 -0.0518 0.1353 0.3377 11.00000 0.05 0.53 Q9 1 0.5551 0.4652 0.5378 11.00000 0.05 0.52 Q10 1 -0.1823 0.2670 0.4212 11.00000 0.05 0.52 Q11 1 0.9877 0.2783 0.0166 11.00000 0.05 0.52 Q12 1 0.0861 -0.0042 0.2262 11.00000 0.05 0.49 Q13 1 0.3917 0.2797 0.1538 11.00000 0.05 0.48 Q14 1 0.5072 0.0847 -0.0423 11.00000 0.05 0.45 Q15 1 0.8120 -0.1468 0.3987 11.00000 0.05 0.41 Q16 1 0.7346 0.2627 0.2614 11.00000 0.05 0.38 Q17 1 0.6033 0.3999 0.3635 11.00000 0.05 0.38 Q18 1 0.3804 0.0587 0.1554 11.00000 0.05 0.36 Q19 1 0.4386 0.4670 0.4414 11.00000 0.05 0.36 Q20 1 0.3647 0.0615 0.1383 11.00000 0.05 0.36 ; _shelx_res_checksum 71694 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.66510(7) -0.00616(4) 0.01944(4) 0.0285(2) Uani 1 1 d . . . . . Ni2 Ni 0.54106(7) 0.13693(4) 0.12161(4) 0.0279(2) Uani 1 1 d . . . . . Ni3 Ni 0.38721(7) 0.26560(5) 0.22572(4) 0.0319(2) Uani 1 1 d . . . . . O1 O 0.7859(3) -0.1084(2) 0.04931(17) 0.0325(6) Uani 1 1 d . . . . . O2 O 0.6339(3) 0.01324(18) 0.13521(15) 0.0288(6) Uani 1 1 d . . . . . O3 O 0.5373(3) 0.1612(2) 0.23586(16) 0.0325(6) Uani 1 1 d . . . . . O4 O 0.7285(6) -0.2037(3) 0.3791(3) 0.0904(17) Uani 1 1 d . . . . . O5 O 0.5201(3) 0.10696(18) 0.00372(16) 0.0262(6) Uani 1 1 d . . . . . O6 O 0.4450(3) 0.26047(19) 0.11238(16) 0.0300(6) Uani 1 1 d . . . . . O7 O 0.2616(3) 0.3637(2) 0.18906(18) 0.0362(7) Uani 1 1 d . . . . . O8 O 0.3695(4) 0.4889(2) -0.1272(2) 0.0542(9) Uani 1 1 d . . . . . O9 O 0.8172(3) 0.1067(2) 0.03748(17) 0.0343(6) Uani 1 1 d . . . . . O10 O 0.7340(3) 0.2133(2) 0.12536(18) 0.0349(6) Uani 1 1 d . . . . . O11 O 0.3413(3) 0.05333(18) 0.09966(16) 0.0291(6) Uani 1 1 d . . . . . O12 O 0.2415(3) 0.1468(2) 0.18699(18) 0.0361(7) Uani 1 1 d . . . . . O13 O 0.5354(3) 0.3759(2) 0.27884(18) 0.0406(7) Uani 1 1 d . . . . . O14 O 0.3011(3) 0.2714(2) 0.33059(18) 0.0408(7) Uani 1 1 d . . . . . O15 O 0.9138(9) 0.4297(13) 0.5682(8) 0.290(9) Uani 1 1 d . . . . . O16 O 0.8651(19) 0.2101(11) 0.5580(13) 0.194(8) Uani 0.5 1 d D . P A 1 O17 O 0.9796(15) 0.0728(13) 0.5314(10) 0.159(6) Uani 0.5 1 d D . P A 2 N1 N 0.7530(4) 0.4547(3) 0.2901(2) 0.0448(9) Uani 1 1 d . . . . . N2 N 0.0950(5) 0.2697(3) 0.3803(2) 0.0520(10) Uani 1 1 d . . . . . N3 N 0.6804(8) 0.4057(5) 0.5755(4) 0.098(2) Uani 1 1 d . . . . . N4 N 0.8374(6) 0.0773(4) 0.6238(3) 0.0734(14) Uani 1 1 d . . . . . C1 C 0.8114(4) -0.1435(3) 0.1169(3) 0.0335(9) Uani 1 1 d . . . . . C2 C 0.9020(5) -0.2210(3) 0.1201(3) 0.0400(10) Uani 1 1 d . . . . . H2 H 0.9401 -0.2408 0.0747 0.048 Uiso 1 1 calc R U . . . C3 C 0.9357(5) -0.2678(3) 0.1868(3) 0.0451(11) Uani 1 1 d . . . . . H3 H 0.9968 -0.3172 0.1864 0.054 Uiso 1 1 calc R U . . . C4 C 0.8786(6) -0.2417(4) 0.2552(3) 0.0481(12) Uani 1 1 d . . . . . H4 H 0.8990 -0.2749 0.3000 0.058 Uiso 1 1 calc R U . . . C5 C 0.7919(5) -0.1667(3) 0.2563(3) 0.0418(10) Uani 1 1 d . . . . . C6 C 0.7571(4) -0.1125(3) 0.1893(3) 0.0341(9) Uani 1 1 d . . . . . C7 C 0.6740(4) -0.0295(3) 0.1969(3) 0.0318(9) Uani 1 1 d . . . . . C8 C 0.6370(4) 0.0087(3) 0.2741(3) 0.0347(9) Uani 1 1 d . . . . . C9 C 0.6669(6) -0.0485(4) 0.3399(3) 0.0472(12) Uani 1 1 d . . . . . C10 C 0.7286(6) -0.1448(4) 0.3285(3) 0.0548(13) Uani 1 1 d . . . . . C11 C 0.5736(4) 0.0998(3) 0.2892(3) 0.0338(9) Uani 1 1 d . . . . . C12 C 0.5500(5) 0.1283(4) 0.3672(3) 0.0473(12) Uani 1 1 d . . . . . H12 H 0.5095 0.1874 0.3773 0.057 Uiso 1 1 calc R U . . . C13 C 0.5839(7) 0.0730(4) 0.4286(3) 0.0605(15) Uani 1 1 d . . . . . H13 H 0.5694 0.0958 0.4797 0.073 Uiso 1 1 calc R U . . . C14 C 0.6400(7) -0.0176(4) 0.4148(3) 0.0626(16) Uani 1 1 d . . . . . H14 H 0.6592 -0.0571 0.4560 0.075 Uiso 1 1 calc R U . . . C15 C 0.5269(4) 0.1867(3) -0.0402(2) 0.0288(8) Uani 1 1 d . . . . . C16 C 0.5938(4) 0.1760(3) -0.1075(2) 0.0345(9) Uani 1 1 d . . . . . H16 H 0.6409 0.1197 -0.1163 0.041 Uiso 1 1 calc R U . . . C17 C 0.5922(5) 0.2458(3) -0.1607(3) 0.0405(10) Uani 1 1 d . . . . . H17 H 0.6393 0.2372 -0.2043 0.049 Uiso 1 1 calc R U . . . C18 C 0.5199(5) 0.3295(3) -0.1496(3) 0.0401(10) Uani 1 1 d . . . . . H18 H 0.5139 0.3753 -0.1872 0.048 Uiso 1 1 calc R U . . . C19 C 0.4574(4) 0.3440(3) -0.0823(3) 0.0339(9) Uani 1 1 d . . . . . C20 C 0.4644(4) 0.2766(3) -0.0230(2) 0.0311(9) Uani 1 1 d . . . . . C21 C 0.4094(4) 0.3058(3) 0.0519(2) 0.0288(8) Uani 1 1 d . . . . . C22 C 0.3232(4) 0.3865(3) 0.0579(3) 0.0318(9) Uani 1 1 d . . . . . C23 C 0.3033(5) 0.4478(3) -0.0060(3) 0.0362(9) Uani 1 1 d . . . . . C24 C 0.3773(5) 0.4325(3) -0.0752(3) 0.0385(10) Uani 1 1 d . . . . . C25 C 0.2558(4) 0.4090(3) 0.1270(3) 0.0327(9) Uani 1 1 d . . . . . C26 C 0.1696(5) 0.4907(3) 0.1241(3) 0.0405(10) Uani 1 1 d . . . . . H26 H 0.1229 0.5059 0.1670 0.049 Uiso 1 1 calc R U . . . C27 C 0.1530(5) 0.5465(3) 0.0619(3) 0.0453(11) Uani 1 1 d . . . . . H27 H 0.0955 0.5982 0.0630 0.054 Uiso 1 1 calc R U . . . C28 C 0.2220(5) 0.5265(3) -0.0036(3) 0.0438(11) Uani 1 1 d . . . . . H28 H 0.2130 0.5662 -0.0453 0.053 Uiso 1 1 calc R U . . . C29 C 0.8257(4) 0.1862(3) 0.0842(3) 0.0323(9) Uani 1 1 d . . . . . C30 C 0.9594(4) 0.2551(3) 0.0911(3) 0.0403(10) Uani 1 1 d . . . . . H30A H 0.9938 0.2758 0.1462 0.060 Uiso 1 1 calc R U . . . H30B H 0.9417 0.3132 0.0642 0.060 Uiso 1 1 calc R U . . . H30C H 1.0277 0.2201 0.0674 0.060 Uiso 1 1 calc R U . . . C31 C 0.2370(4) 0.0736(3) 0.1355(2) 0.0316(9) Uani 1 1 d . . . . . C32 C 0.1046(5) 0.0057(3) 0.1147(3) 0.0442(11) Uani 1 1 d . . . . . H32A H 0.0499 0.0127 0.1572 0.066 Uiso 1 1 calc R U . . . H32B H 0.1256 -0.0627 0.1066 0.066 Uiso 1 1 calc R U . . . H32C H 0.0530 0.0232 0.0669 0.066 Uiso 1 1 calc R U . . . C33 C 0.6515(5) 0.3863(3) 0.2572(3) 0.0382(10) Uani 1 1 d . . . . . H33 H 0.6681 0.3425 0.2148 0.046 Uiso 1 1 calc R U . . . C34 C 0.8808(6) 0.4678(4) 0.2555(4) 0.0612(15) Uani 1 1 d . . . . . H34A H 0.8816 0.5274 0.2286 0.092 Uiso 1 1 calc R U . . . H34B H 0.8857 0.4105 0.2182 0.092 Uiso 1 1 calc R U . . . H34C H 0.9596 0.4743 0.2968 0.092 Uiso 1 1 calc R U . . . C35 C 0.7305(7) 0.5310(5) 0.3515(4) 0.091(2) Uani 1 1 d . . . . . H35A H 0.8166 0.5517 0.3862 0.136 Uiso 1 1 calc R U . . . H35B H 0.6622 0.5040 0.3815 0.136 Uiso 1 1 calc R U . . . H35C H 0.6978 0.5878 0.3274 0.136 Uiso 1 1 calc R U . . . C36 C 0.1714(5) 0.2619(3) 0.3222(3) 0.0416(11) Uani 1 1 d . . . . . H36 H 0.1242 0.2481 0.2706 0.050 Uiso 1 1 calc R U . . . C37 C -0.0558(6) 0.2521(6) 0.3652(4) 0.0740(18) Uani 1 1 d . . . . . H37A H -0.0864 0.1969 0.3924 0.111 Uiso 1 1 calc R U . . . H37B H -0.0859 0.2364 0.3091 0.111 Uiso 1 1 calc R U . . . H37C H -0.0950 0.3113 0.3839 0.111 Uiso 1 1 calc R U . . . C38 C 0.1611(8) 0.2947(8) 0.4616(4) 0.111(3) Uani 1 1 d . . . . . H38A H 0.1612 0.2349 0.4882 0.166 Uiso 1 1 calc R U . . . H38B H 0.1107 0.3424 0.4882 0.166 Uiso 1 1 calc R U . . . H38C H 0.2554 0.3232 0.4624 0.166 Uiso 1 1 calc R U . . . C39 C 0.7967(16) 0.3985(13) 0.5394(8) 0.185(7) Uani 1 1 d . . . . . H39 H 0.7838 0.3665 0.4878 0.222 Uiso 1 1 calc R U . . . C40 C 0.5489(12) 0.3612(11) 0.5311(7) 0.195(7) Uani 1 1 d . . . . . H40A H 0.5048 0.3149 0.5618 0.293 Uiso 1 1 calc R U . . . H40B H 0.5647 0.3261 0.4820 0.293 Uiso 1 1 calc R U . . . H40C H 0.4897 0.4131 0.5200 0.293 Uiso 1 1 calc R U . . . C41 C 0.6883(12) 0.4517(8) 0.6547(5) 0.136(4) Uani 1 1 d . . . . . H41A H 0.7481 0.4172 0.6899 0.203 Uiso 1 1 calc R U . . . H41B H 0.5967 0.4480 0.6698 0.203 Uiso 1 1 calc R U . . . H41C H 0.7254 0.5208 0.6577 0.203 Uiso 1 1 calc R U . . . C42 C 0.8983(10) 0.1219(7) 0.5687(5) 0.099(3) Uani 1 1 d D . . . . H42A H 0.8817 0.1867 0.5581 0.119 Uiso 0.5 1 calc R U P A 2 H42 H 0.9604 0.0909 0.5402 0.119 Uiso 0.5 1 calc R U P A 1 C43 C 0.7517(10) 0.1283(8) 0.6718(6) 0.131(4) Uani 1 1 d . . . . . H43A H 0.7464 0.1954 0.6575 0.197 Uiso 1 1 calc R U . . . H43B H 0.7910 0.1311 0.7267 0.197 Uiso 1 1 calc R U . . . H43C H 0.6598 0.0929 0.6635 0.197 Uiso 1 1 calc R U . . . C44 C 0.8708(12) -0.0222(6) 0.6371(6) 0.132(4) Uani 1 1 d . . . . . H44A H 0.9192 -0.0483 0.5956 0.197 Uiso 1 1 calc R U . . . H44B H 0.7863 -0.0651 0.6372 0.197 Uiso 1 1 calc R U . . . H44C H 0.9291 -0.0199 0.6875 0.197 Uiso 1 1 calc R U . . . 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 0.0259(4) 0.0223(3) 0.0381(4) 0.0033(3) 0.0073(3) 0.0032(2) Ni2 0.0258(4) 0.0228(3) 0.0368(4) 0.0043(3) 0.0082(3) 0.0050(3) Ni3 0.0311(4) 0.0261(4) 0.0396(4) 0.0021(3) 0.0091(3) 0.0050(3) O1 0.0272(15) 0.0282(14) 0.0443(17) 0.0045(12) 0.0105(12) 0.0066(11) O2 0.0326(16) 0.0244(13) 0.0312(15) 0.0054(11) 0.0055(11) 0.0093(11) O3 0.0360(17) 0.0283(14) 0.0347(15) 0.0046(11) 0.0057(12) 0.0095(11) O4 0.154(5) 0.073(3) 0.070(3) 0.042(2) 0.052(3) 0.067(3) O5 0.0210(14) 0.0203(12) 0.0378(15) 0.0064(10) 0.0052(11) 0.0005(9) O6 0.0311(16) 0.0270(13) 0.0347(15) 0.0058(11) 0.0092(12) 0.0087(11) O7 0.0328(17) 0.0330(15) 0.0468(18) 0.0061(13) 0.0136(13) 0.0112(12) O8 0.067(2) 0.0436(19) 0.063(2) 0.0253(17) 0.0235(18) 0.0233(17) O9 0.0279(16) 0.0264(14) 0.0479(17) -0.0002(12) 0.0084(12) -0.0002(11) O10 0.0259(16) 0.0298(14) 0.0491(17) 0.0005(12) 0.0099(13) 0.0020(11) O11 0.0247(15) 0.0238(13) 0.0395(15) 0.0038(11) 0.0078(12) 0.0016(10) O12 0.0283(16) 0.0316(15) 0.0489(17) -0.0029(13) 0.0135(13) 0.0017(11) O13 0.0339(18) 0.0341(16) 0.0517(19) -0.0036(13) 0.0083(14) -0.0016(12) O14 0.039(2) 0.0423(17) 0.0442(18) 0.0062(13) 0.0137(14) 0.0105(13) O15 0.073(6) 0.51(2) 0.258(13) -0.116(13) 0.001(7) 0.062(9) O16 0.164(17) 0.146(15) 0.28(2) 0.057(15) 0.040(15) 0.012(13) O17 0.143(13) 0.173(15) 0.156(13) -0.044(11) 0.046(10) 0.021(11) N1 0.039(2) 0.039(2) 0.054(2) -0.0023(17) 0.0106(18) -0.0019(16) N2 0.047(3) 0.066(3) 0.049(2) 0.010(2) 0.0180(19) 0.015(2) N3 0.097(5) 0.097(5) 0.098(5) -0.019(4) 0.011(4) 0.030(4) N4 0.089(4) 0.067(3) 0.066(3) 0.007(3) 0.022(3) 0.001(3) C1 0.031(2) 0.0252(19) 0.043(2) 0.0035(17) 0.0018(18) 0.0014(16) C2 0.036(3) 0.033(2) 0.054(3) 0.0055(19) 0.012(2) 0.0111(18) C3 0.042(3) 0.038(2) 0.058(3) 0.010(2) 0.007(2) 0.017(2) C4 0.058(3) 0.042(3) 0.049(3) 0.015(2) 0.006(2) 0.018(2) C5 0.047(3) 0.033(2) 0.047(3) 0.0074(19) 0.007(2) 0.0103(19) C6 0.032(2) 0.0259(19) 0.046(2) 0.0082(17) 0.0054(18) 0.0048(16) C7 0.028(2) 0.0247(19) 0.042(2) 0.0049(17) 0.0054(17) -0.0003(15) C8 0.033(2) 0.035(2) 0.037(2) 0.0082(18) 0.0059(18) 0.0081(17) C9 0.059(3) 0.045(3) 0.043(3) 0.014(2) 0.011(2) 0.017(2) C10 0.073(4) 0.049(3) 0.051(3) 0.020(2) 0.017(3) 0.025(3) C11 0.032(2) 0.032(2) 0.038(2) 0.0063(17) 0.0041(17) 0.0039(16) C12 0.059(3) 0.046(3) 0.041(3) 0.005(2) 0.012(2) 0.020(2) C13 0.083(4) 0.067(3) 0.040(3) 0.010(2) 0.018(3) 0.036(3) C14 0.088(5) 0.066(3) 0.045(3) 0.020(3) 0.018(3) 0.038(3) C15 0.023(2) 0.0266(19) 0.038(2) 0.0069(16) 0.0045(16) 0.0036(14) C16 0.036(2) 0.029(2) 0.041(2) 0.0044(17) 0.0133(18) 0.0072(17) C17 0.042(3) 0.035(2) 0.049(3) 0.0096(19) 0.020(2) 0.0046(19) C18 0.048(3) 0.031(2) 0.045(3) 0.0134(18) 0.013(2) 0.0070(18) C19 0.034(2) 0.0238(19) 0.046(2) 0.0070(17) 0.0084(18) 0.0031(16) C20 0.028(2) 0.0236(19) 0.042(2) 0.0074(16) 0.0072(17) -0.0008(15) C21 0.027(2) 0.0229(18) 0.037(2) 0.0053(16) 0.0055(16) -0.0016(15) C22 0.030(2) 0.0225(18) 0.042(2) 0.0055(16) 0.0043(17) 0.0021(15) C23 0.038(2) 0.0245(19) 0.046(3) 0.0048(17) 0.0048(19) 0.0038(16) C24 0.040(3) 0.029(2) 0.049(3) 0.0117(19) 0.009(2) 0.0060(17) C25 0.029(2) 0.0249(19) 0.044(2) 0.0008(17) 0.0065(17) 0.0026(15) C26 0.037(3) 0.030(2) 0.057(3) 0.0039(19) 0.013(2) 0.0094(18) C27 0.046(3) 0.032(2) 0.061(3) 0.008(2) 0.010(2) 0.0172(19) C28 0.046(3) 0.033(2) 0.055(3) 0.013(2) 0.008(2) 0.0116(19) C29 0.028(2) 0.0260(19) 0.043(2) 0.0084(17) 0.0044(18) 0.0031(15) C30 0.031(2) 0.031(2) 0.059(3) 0.0033(19) 0.009(2) 0.0010(17) C31 0.031(2) 0.0241(19) 0.042(2) 0.0062(17) 0.0110(18) 0.0053(15) C32 0.031(3) 0.037(2) 0.064(3) -0.005(2) 0.015(2) -0.0004(18) C33 0.040(3) 0.031(2) 0.045(3) 0.0043(18) 0.013(2) 0.0049(18) C34 0.044(3) 0.057(3) 0.083(4) 0.006(3) 0.020(3) -0.006(2) C35 0.071(4) 0.080(5) 0.110(5) -0.049(4) 0.039(4) -0.024(3) C36 0.041(3) 0.041(2) 0.047(3) 0.007(2) 0.015(2) 0.0122(19) C37 0.048(4) 0.107(5) 0.078(4) 0.024(4) 0.029(3) 0.022(3) C38 0.086(6) 0.203(10) 0.043(4) 0.001(5) 0.018(3) 0.014(6) C39 0.129(11) 0.281(19) 0.157(12) -0.014(11) 0.036(10) 0.106(12) C40 0.111(9) 0.264(17) 0.172(12) -0.088(11) -0.002(8) -0.037(10) C41 0.152(10) 0.154(9) 0.103(7) -0.029(6) 0.021(6) 0.065(8) C42 0.120(7) 0.084(6) 0.094(6) 0.007(5) 0.035(5) -0.006(5) C43 0.104(7) 0.177(10) 0.111(7) -0.031(7) 0.041(6) 0.014(7) C44 0.200(11) 0.078(6) 0.131(8) 0.032(5) 0.048(8) 0.038(6) 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' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 9 -3 0.0498 -0.0053 8.9967 -2.9690 0.0646 0.9898 0.3365 0 0 11 0.0445 -0.0009 0.0054 10.9964 0.9534 -0.2786 0.1664 0 -9 3 0.0766 0.0053 -8.9967 2.9690 -0.0646 -0.9898 -0.3365 6 0 -4 0.1114 5.9931 -0.0152 -4.0050 0.0389 0.4209 -0.8830 0 -1 -11 0.0068 0.0015 -1.0052 -10.9998 -0.9895 0.1771 -0.2089 1 4 8 0.0232 0.9957 4.0009 8.0097 0.9019 0.2567 0.1537 3 -7 4 0.1276 3.0003 -7.0032 3.9722 0.2870 -0.6523 -0.6478 -6 -1 -3 0.1090 -5.9919 -0.9881 -2.9960 -0.6816 -0.3451 0.7346 -1 -2 11 0.0434 -0.9985 -1.9920 10.9908 0.8170 -0.5350 0.2186 -1 1 11 0.0405 -1.0003 1.0074 11.0008 0.9252 -0.2304 0.3460 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 O1 Ni1 Ni2 129.01(9) . . O1 Ni1 O2 87.40(11) . . O1 Ni1 O5 94.64(11) . 2_655 O1 Ni1 O5 171.28(11) . . O1 Ni1 O9 95.21(12) . . O1 Ni1 O11 91.22(11) . 2_655 O2 Ni1 Ni2 42.52(7) . . O2 Ni1 O5 84.08(10) . . O2 Ni1 O5 87.94(11) . 2_655 O2 Ni1 O11 166.25(11) . 2_655 O5 Ni1 Ni2 92.68(7) 2_655 . O5 Ni1 Ni2 42.99(7) . . O5 Ni1 O5 83.23(10) 2_655 . O9 Ni1 Ni2 80.47(8) . . O9 Ni1 O2 91.71(11) . . O9 Ni1 O5 170.12(11) . 2_655 O9 Ni1 O5 86.91(10) . . O9 Ni1 O11 102.05(11) . 2_655 O11 Ni1 Ni2 139.59(8) 2_655 . O11 Ni1 O5 96.61(10) 2_655 . O11 Ni1 O5 78.52(10) 2_655 2_655 O2 Ni2 Ni1 44.07(8) . . O2 Ni2 O5 90.54(11) . . O2 Ni2 O6 177.56(11) . . O2 Ni2 O10 88.28(11) . . O2 Ni2 O11 91.39(11) . . O3 Ni2 Ni1 134.94(8) . . O3 Ni2 O2 91.32(11) . . O3 Ni2 O5 173.03(11) . . O3 Ni2 O6 86.41(11) . . O3 Ni2 O10 95.11(12) . . O3 Ni2 O11 93.23(11) . . O5 Ni2 Ni1 48.07(7) . . O5 Ni2 O10 91.66(11) . . O5 Ni2 O11 80.01(10) . . O6 Ni2 Ni1 138.29(8) . . O6 Ni2 O5 91.61(11) . . O6 Ni2 O10 92.82(11) . . O6 Ni2 O11 87.84(11) . . O10 Ni2 Ni1 80.24(8) . . O10 Ni2 O11 171.66(11) . . O11 Ni2 Ni1 93.75(7) . . O6 Ni3 O3 79.85(11) . . O7 Ni3 O3 165.30(12) . . O7 Ni3 O6 85.46(11) . . O7 Ni3 O12 93.00(12) . . O7 Ni3 O13 91.93(13) . . O7 Ni3 O14 88.32(12) . . O12 Ni3 O3 87.47(11) . . O12 Ni3 O6 89.46(11) . . O12 Ni3 O14 85.68(12) . . O13 Ni3 O3 89.32(12) . . O13 Ni3 O6 97.08(12) . . O13 Ni3 O12 172.10(13) . . O13 Ni3 O14 88.30(13) . . O14 Ni3 O3 106.36(12) . . O14 Ni3 O6 171.90(12) . . C1 O1 Ni1 129.0(3) . . Ni2 O2 Ni1 93.41(11) . . C7 O2 Ni1 134.0(2) . . C7 O2 Ni2 132.0(2) . . Ni2 O3 Ni3 94.88(12) . . C11 O3 Ni2 126.1(2) . . C11 O3 Ni3 133.6(3) . . Ni1 O5 Ni1 96.77(10) 2_655 . Ni2 O5 Ni1 101.37(11) . 2_655 Ni2 O5 Ni1 88.95(10) . . C15 O5 Ni1 128.7(2) . . C15 O5 Ni1 117.3(2) . 2_655 C15 O5 Ni2 117.6(2) . . Ni2 O6 Ni3 94.89(11) . . C21 O6 Ni2 130.3(2) . . C21 O6 Ni3 133.4(2) . . C25 O7 Ni3 129.8(3) . . C29 O9 Ni1 127.4(3) . . C29 O10 Ni2 124.8(3) . . Ni1 O11 Ni2 99.08(11) 2_655 . C31 O11 Ni1 126.9(3) . 2_655 C31 O11 Ni2 124.9(2) . . C31 O12 Ni3 132.4(3) . . C33 O13 Ni3 121.4(3) . . C36 O14 Ni3 115.4(3) . . C33 N1 C34 120.5(4) . . C33 N1 C35 120.7(4) . . C35 N1 C34 117.7(4) . . C36 N2 C37 121.7(5) . . C36 N2 C38 120.2(5) . . C38 N2 C37 118.1(5) . . C39 N3 C40 117.4(10) . . C39 N3 C41 121.7(10) . . C41 N3 C40 120.8(9) . . C42 N4 C43 121.9(8) . . C42 N4 C44 117.3(7) . . C43 N4 C44 120.6(7) . . O1 C1 C2 116.1(4) . . O1 C1 C6 126.8(4) . . C2 C1 C6 117.1(4) . . C3 C2 C1 123.0(4) . . C2 C3 C4 120.1(4) . . C5 C4 C3 119.7(4) . . C4 C5 C6 122.7(4) . . C4 C5 C10 117.8(4) . . C6 C5 C10 119.4(4) . . C5 C6 C1 117.3(4) . . C5 C6 C7 119.5(4) . . C7 C6 C1 123.2(4) . . O2 C7 C6 119.1(4) . . O2 C7 C8 119.2(4) . . C6 C7 C8 121.6(4) . . C9 C8 C7 118.0(4) . . C9 C8 C11 116.9(4) . . C11 C8 C7 125.1(4) . . C8 C9 C10 120.1(4) . . C14 C9 C8 122.3(4) . . C14 C9 C10 117.6(4) . . O4 C10 C5 121.2(4) . . O4 C10 C9 120.4(5) . . C5 C10 C9 118.4(4) . . O3 C11 C8 125.4(4) . . O3 C11 C12 116.4(4) . . C12 C11 C8 118.2(4) . . C13 C12 C11 122.9(4) . . C12 C13 C14 119.9(5) . . C9 C14 C13 119.6(5) . . O5 C15 C16 117.2(3) . . O5 C15 C20 123.6(3) . . C16 C15 C20 119.1(4) . . C17 C16 C15 122.1(4) . . C16 C17 C18 119.9(4) . . C19 C18 C17 119.4(4) . . C18 C19 C20 122.4(4) . . C18 C19 C24 116.9(4) . . C20 C19 C24 120.7(4) . . C15 C20 C21 125.3(4) . . C19 C20 C15 116.6(4) . . C19 C20 C21 118.1(3) . . O6 C21 C20 118.7(3) . . O6 C21 C22 120.1(4) . . C22 C21 C20 121.2(4) . . C21 C22 C25 122.2(4) . . C23 C22 C21 119.4(4) . . C23 C22 C25 118.4(4) . . C22 C23 C24 120.5(4) . . C28 C23 C22 122.0(4) . . C28 C23 C24 117.3(4) . . O8 C24 C19 120.2(4) . . O8 C24 C23 121.2(4) . . C23 C24 C19 118.5(4) . . O7 C25 C22 127.4(4) . . O7 C25 C26 116.4(4) . . C26 C25 C22 116.2(4) . . C27 C26 C25 123.4(4) . . C26 C27 C28 120.2(4) . . C23 C28 C27 119.7(4) . . O9 C29 O10 126.5(4) . . O9 C29 C30 115.9(4) . . O10 C29 C30 117.5(4) . . O11 C31 C32 118.2(3) . . O12 C31 O11 123.4(4) . . O12 C31 C32 118.3(4) . . O13 C33 N1 124.5(4) . . O14 C36 N2 125.6(5) . . O15 C39 N3 126.0(14) . . O16 C42 N4 115.5(12) . . O17 C42 N4 117.9(12) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 Ni2 2.9245(9) . Ni1 O1 1.947(3) . Ni1 O2 2.038(3) . Ni1 O5 2.122(2) 2_655 Ni1 O5 2.176(3) . Ni1 O9 1.991(3) . Ni1 O11 2.063(3) 2_655 Ni2 O2 1.980(3) . Ni2 O3 1.954(3) . Ni2 O5 1.994(3) . Ni2 O6 1.986(3) . Ni2 O10 2.047(3) . Ni2 O11 2.123(3) . Ni3 O3 2.117(3) . Ni3 O6 2.086(3) . Ni3 O7 1.965(3) . Ni3 O12 2.032(3) . Ni3 O13 2.025(3) . Ni3 O14 2.077(3) . O1 C1 1.291(5) . O2 C7 1.279(5) . O3 C11 1.320(5) . O4 C10 1.226(6) . O5 Ni1 2.122(2) 2_655 O5 C15 1.368(4) . O6 C21 1.272(5) . O7 C25 1.270(5) . O8 C24 1.222(5) . O9 C29 1.260(5) . O10 C29 1.267(5) . O11 Ni1 2.063(3) 2_655 O11 C31 1.291(5) . O12 C31 1.249(5) . O13 C33 1.236(5) . O14 C36 1.244(6) . O15 C39 1.198(16) . O16 C42 1.280(9) . O17 C42 1.272(9) . N1 C33 1.312(6) . N1 C34 1.452(6) . N1 C35 1.447(7) . N2 C36 1.321(6) . N2 C37 1.448(7) . N2 C38 1.443(8) . N3 C39 1.366(13) . N3 C40 1.441(11) . N3 C41 1.422(10) . N4 C42 1.338(9) . N4 C43 1.421(9) . N4 C44 1.437(9) . C1 C2 1.425(6) . C1 C6 1.450(6) . C2 C3 1.369(7) . C3 C4 1.390(7) . C4 C5 1.372(6) . C5 C6 1.431(6) . C5 C10 1.470(7) . C6 C7 1.442(5) . C7 C8 1.472(6) . C8 C9 1.435(6) . C8 C11 1.437(6) . C9 C10 1.483(6) . C9 C14 1.373(7) . C11 C12 1.405(6) . C12 C13 1.365(7) . C13 C14 1.392(7) . C15 C16 1.400(5) . C15 C20 1.424(5) . C16 C17 1.366(6) . C17 C18 1.391(6) . C18 C19 1.378(6) . C19 C20 1.422(6) . C19 C24 1.483(5) . C20 C21 1.487(5) . C21 C22 1.434(5) . C22 C23 1.432(6) . C22 C25 1.447(6) . C23 C24 1.473(6) . C23 C28 1.378(6) . C25 C26 1.440(6) . C26 C27 1.358(7) . C27 C28 1.399(7) . C29 C30 1.512(5) . C31 C32 1.489(6) .