# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/ data_CRYSTALS_cif _audit_creation_date 99-03-22 _audit_creation_method CRYSTALS # FA2 IPDS 10-May-98 0.71073 #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\REF.CIF # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS _publ_contact_author ; Pascal G. Lacroix Laboratoire de chimie de coordination 205, route de Narbonne 31077 Toulouse, France ; _publ_contact_author_phone ' (33) (0)5 61 33 31 36 ' _publ_contact_author_fax ' (33) (0)5 61 55 30 03 ' _publ_contact_author_email ' pascal@lcc-toulouse .fr ' _publ_requested_journal ' J. Mater. Chem. ' _publ_requested_coeditor_name ' Doctor McCann ' _publ_contact_letter ; ; #************************************************ # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, crystal structure, solid state NLO and magnetic properties in a novel class of chiral bis(salicylaldiminato)nickel(II) Schiff-base complexes. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Averseng Frederic' ; 205 route de Narbonne 31077 Toulouse, France ; 'Malfant Isabelle' ; 205 route de Narbonne 31077 Toulouse, France ; 'Lacroix Pascal G.' ; 205 route de Narbonne 31077 Toulouse, France ; 'Dahan Francoise' ; 205 route de Narbonne 31077 Toulouse, France ; 'Nakatani Keitaro' ; PPSM, Ecole normale superieure de Cachan avenue du president Wilson 94235 Cachan, France ; #============================================================================== # 4. TEXT _publ_section_references # Add your own references - in alphabetic order ; Carruthers, J.R. and Watkin, D.J. (1979), (Chebychev Weighting) Acta Cryst, A35, 698-699 North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), (Psi correction), Acta Cryst, A24, 351-359 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin, D.J., Prout, C.K. Carruthers, R.J. & Betteridge, P. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; #========================================================================== # NOW THE GOODIES TO BE ENTERED BY HAND #========================================================================== # ligand H2L3 _chemical_melting_point ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' stoe-ipds ' _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary Direct_Methods _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle ; #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ; _cell_length_a '12.432 (1)' _cell_angle_alpha 90 _cell_length_b '12.893 (1)' _cell_angle_beta 90 _cell_length_c '22.148 (2)' _cell_angle_gamma 90 _cell_volume 3550.01 _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,-y+1/2,-z' '-x,y+1/2,-z+1/2' '-x+1/2,-y,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C42 H42 O2 N4 ' _chemical_formula_moiety ' C42 H42 O2 N4 ' _chemical_compound_source ; ; _chemical_formula_weight 634.82 _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 24.2 _cell_measurement_temperature 160 _cell_formula_units_Z 4.00 _exptl_crystal_description ' diamond ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.17 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.31 _exptl_crystal_density_diffrn 1.19 _exptl_crystal_density_meas none _exptl_crystal_F_000 1352.23 _exptl_absorpt_coefficient_mu 0.07 _exptl_absorpt_correction_type none _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 0 _diffrn_reflns_number 5672 _reflns_number_total 0 _diffrn_reflns_av_R_equivalents 0.00 _reflns_number_observed 2637 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 24.37 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _reflns_observed_criterion >2.00\s(I) _refine_diff_density_min -0.61 _refine_diff_density_max 0.82 _refine_ls_number_reflns 2637 _refine_ls_number_parameters 434 _refine_ls_R_factor_obs 0.0913 _refine_ls_wR_factor_obs 0.0800 _refine_ls_goodness_of_fit_obs 1.1412 _refine_ls_shift/esd_max 0.038602 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method 2\q/\w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type O1 0.3370(4) 0.3692(4) 0.4735(2) 0.0496 1.0000 Uani O2 0.6403(5) 0.0797(5) 0.2785(2) 0.0756 1.0000 Uani N1 0.3728(5) 0.3175(4) 0.3633(2) 0.0401 1.0000 Uani N2 0.5759(6) 0.1077(4) 0.3875(3) 0.0454 1.0000 Uani N3 0.3010(5) 0.7227(5) 0.5255(3) 0.0549 1.0000 Uani N4 0.9916(7) 0.1978(9) 0.2246(4) 0.1154 1.0000 Uani C1 0.3442(6) 0.4663(5) 0.4561(3) 0.0452 1.0000 Uani C2 0.3244(7) 0.5426(6) 0.4991(3) 0.0533 1.0000 Uani C3 0.3296(7) 0.6486(5) 0.4830(3) 0.0537 1.0000 Uani C4 0.3558(7) 0.6749(5) 0.4235(3) 0.0497 1.0000 Uani C5 0.3738(7) 0.5979(5) 0.3813(3) 0.0483 1.0000 Uani C6 0.3690(7) 0.4952(6) 0.3948(3) 0.0511 1.0000 Uani C7 0.3807(7) 0.4148(6) 0.3490(3) 0.0464 1.0000 Uani C8 0.2885(9) 0.8317(5) 0.5083(4) 0.0714 1.0000 Uani C9 0.1859(9) 0.8559(8) 0.4735(5) 0.0910 1.0000 Uani C10 0.2608(9) 0.6937(6) 0.5846(4) 0.0715 1.0000 Uani C11 0.1398(9) 0.6583(6) 0.5828(4) 0.0763 1.0000 Uani C21 0.7360(6) 0.1195(7) 0.2960(3) 0.0541 1.0000 Uani C22 0.8135(7) 0.1321(8) 0.2528(3) 0.0800 1.0000 Uani C23 0.9164(7) 0.1754(9) 0.2678(3) 0.0790 1.0000 Uani C24 0.9383(7) 0.188(1) 0.3283(4) 0.0848 1.0000 Uani C25 0.8604(8) 0.1707(7) 0.3714(4) 0.0682 1.0000 Uani C26 0.7535(7) 0.1386(6) 0.3553(3) 0.0454 1.0000 Uani C27 0.6710(7) 0.1338(5) 0.4009(3) 0.0410 1.0000 Uani C28 1.0984(9) 0.242(1) 0.2390(5) 0.1135 1.0000 Uani C29 1.105(1) 0.359(1) 0.2535(7) 0.1464 1.0000 Uani C30 0.954(1) 0.212(1) 0.1599(6) 0.1092 1.0000 Uani C31 0.971(1) 0.111(2) 0.1284(9) 0.1817 1.0000 Uani C41 0.3748(6) 0.2382(5) 0.3202(3) 0.0437 1.0000 Uani C42 0.3785(7) 0.2547(5) 0.2560(3) 0.0525 1.0000 Uani C43 0.3808(7) 0.1713(5) 0.2176(3) 0.0522 1.0000 Uani C44 0.3738(6) 0.0704(5) 0.2401(3) 0.0386 1.0000 Uani C45 0.3713(7) -0.0181(5) 0.1987(3) 0.0516 1.0000 Uani C46 0.3663(8) -0.1157(7) 0.2185(3) 0.0645 1.0000 Uani C47 0.3666(8) -0.1323(6) 0.2834(3) 0.0639 1.0000 Uani C48 0.3704(8) -0.0531(6) 0.3233(3) 0.0644 1.0000 Uani C49 0.3713(6) 0.0530(5) 0.3019(3) 0.0409 1.0000 Uani C50 0.3748(6) 0.1356(5) 0.3425(3) 0.0409 1.0000 Uani C51 0.4923(6) 0.1081(5) 0.4313(3) 0.0429 1.0000 Uani C52 0.5134(6) 0.0971(6) 0.4932(3) 0.0454 1.0000 Uani C53 0.4299(7) 0.0996(6) 0.5323(3) 0.0537 1.0000 Uani C54 0.3219(6) 0.1102(5) 0.5123(3) 0.0446 1.0000 Uani C55 0.2333(6) 0.1143(6) 0.5536(3) 0.0507 1.0000 Uani C56 0.1306(8) 0.1269(6) 0.5326(4) 0.0647 1.0000 Uani C57 0.1137(6) 0.1363(6) 0.4704(3) 0.0518 1.0000 Uani C58 0.1941(7) 0.1348(6) 0.4300(3) 0.0501 1.0000 Uani C59 0.3033(6) 0.1212(5) 0.4492(3) 0.0408 1.0000 Uani C60 0.3912(6) 0.1195(5) 0.4080(3) 0.0358 1.0000 Uani H11 0.4041 0.3349 0.4665 0.0531 1.0000 Uiso H12 0.5815 0.1257 0.2894 0.0500 1.0000 Uiso H21 0.3069 0.5227 0.5408 0.0609 1.0000 Uiso H41 0.3587 0.7484 0.4113 0.0564 1.0000 Uiso H51 0.3916 0.6190 0.3394 0.0474 1.0000 Uiso H71 0.3966 0.4343 0.3068 0.0526 1.0000 Uiso H81 0.2874 0.8735 0.5457 0.0664 1.0000 Uiso H82 0.3504 0.8518 0.4831 0.0664 1.0000 Uiso H91 0.1840 0.9317 0.4636 0.1010 1.0000 Uiso H92 0.1221 0.8381 0.4975 0.1010 1.0000 Uiso H93 0.1850 0.8165 0.4349 0.1010 1.0000 Uiso H101 0.2672 0.7543 0.6124 0.0754 1.0000 Uiso H102 0.3049 0.6359 0.6011 0.0754 1.0000 Uiso H111 0.1154 0.6398 0.6239 0.0913 1.0000 Uiso H112 0.0951 0.7161 0.5671 0.0913 1.0000 Uiso H113 0.1328 0.5977 0.5558 0.0913 1.0000 Uiso H221 0.7968 0.1126 0.2109 0.0724 1.0000 Uiso H241 1.0124 0.2096 0.3413 0.0826 1.0000 Uiso H251 0.8784 0.1827 0.4145 0.0786 1.0000 Uiso H271 0.6884 0.1503 0.4435 0.0465 1.0000 Uiso H281 1.1267 0.2044 0.2739 0.1123 1.0000 Uiso H282 1.1444 0.2301 0.2031 0.1123 1.0000 Uiso H291 1.1821 0.3753 0.2616 0.1673 1.0000 Uiso H292 1.0619 0.3727 0.2895 0.1673 1.0000 Uiso H293 1.0797 0.3984 0.2187 0.1673 1.0000 Uiso H301 0.9979 0.2653 0.1406 0.1284 1.0000 Uiso H302 0.8778 0.2313 0.1604 0.1284 1.0000 Uiso H311 0.9442 0.1171 0.0865 0.2124 1.0000 Uiso H312 1.0454 0.0899 0.1296 0.2124 1.0000 Uiso H313 0.9253 0.0559 0.1494 0.2124 1.0000 Uiso H421 0.3791 0.3264 0.2402 0.0532 1.0000 Uiso H431 0.3875 0.1831 0.1735 0.0536 1.0000 Uiso H451 0.3735 -0.0055 0.1544 0.0606 1.0000 Uiso H461 0.3617 -0.1755 0.1904 0.0721 1.0000 Uiso H471 0.3657 -0.2041 0.2989 0.0664 1.0000 Uiso H481 0.3736 -0.0678 0.3668 0.0718 1.0000 Uiso H521 0.5865 0.0896 0.5086 0.0512 1.0000 Uiso H531 0.4447 0.0926 0.5757 0.0520 1.0000 Uiso H551 0.2450 0.1069 0.5979 0.0583 1.0000 Uiso H561 0.0684 0.1293 0.5613 0.0740 1.0000 Uiso H571 0.0379 0.1442 0.4557 0.0609 1.0000 Uiso H581 0.1780 0.1435 0.3864 0.0562 1.0000 Uiso 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 O1 0.080(4) 0.038(3) 0.031(2) 0.001(2) 0.011(2) 0.002(3) O2 0.067(4) 0.112(5) 0.048(3) -0.027(3) 0.010(3) 0.002(4) N1 0.059(4) 0.040(4) 0.021(3) -0.004(2) -0.001(3) 0.007(3) N2 0.056(4) 0.045(4) 0.034(3) -0.001(3) -0.006(3) -0.013(3) N3 0.075(5) 0.041(4) 0.049(4) -0.004(3) 0.010(3) -0.001(3) N4 0.076(6) 0.19(1) 0.076(6) 0.007(7) 0.011(5) -0.039(7) C1 0.061(6) 0.049(5) 0.026(4) -0.002(3) -0.010(3) 0.000(4) C2 0.078(6) 0.045(4) 0.037(4) -0.001(3) 0.001(4) 0.018(4) C3 0.076(6) 0.044(5) 0.041(4) -0.019(3) 0.008(4) -0.007(4) C4 0.075(6) 0.034(4) 0.040(4) 0.007(3) 0.012(4) 0.006(4) C5 0.082(6) 0.025(4) 0.037(4) 0.004(3) 0.006(4) -0.010(4) C6 0.068(5) 0.056(5) 0.029(4) -0.002(3) 0.008(4) -0.009(4) C7 0.069(5) 0.041(5) 0.029(3) -0.005(3) -0.003(4) -0.004(4) C8 0.123(8) 0.021(4) 0.070(6) -0.010(4) 0.020(6) -0.008(4) C9 0.083(7) 0.063(6) 0.127(9) 0.021(6) 0.016(7) 0.035(6) C10 0.126(9) 0.042(4) 0.046(5) -0.011(4) 0.015(5) 0.003(5) C11 0.090(8) 0.049(5) 0.090(7) -0.018(4) 0.006(6) -0.019(5) C21 0.036(5) 0.076(5) 0.050(5) -0.004(4) -0.002(4) -0.005(4) C22 0.068(6) 0.155(9) 0.018(4) -0.013(5) 0.012(4) -0.037(7) C23 0.056(6) 0.155(9) 0.026(4) -0.009(5) 0.022(4) -0.012(6) C24 0.043(6) 0.16(1) 0.054(6) 0.012(6) 0.012(5) -0.018(6) C25 0.069(7) 0.086(6) 0.050(5) 0.001(4) -0.015(5) -0.003(5) C26 0.062(5) 0.047(4) 0.027(4) 0.001(3) 0.002(4) 0.001(4) C27 0.058(5) 0.038(4) 0.028(4) -0.012(3) -0.002(3) 0.019(4) C28 0.058(7) 0.21(2) 0.069(7) 0.008(8) 0.001(5) -0.027(8) C29 0.21(2) 0.11(1) 0.12(1) -0.012(9) 0.01(1) -0.05(1) C30 0.13(1) 0.11(1) 0.087(8) 0.024(7) 0.041(7) -0.010(8) C31 0.14(1) 0.23(2) 0.18(2) -0.14(2) 0.04(1) -0.00(1) C41 0.058(5) 0.042(4) 0.031(4) 0.009(3) 0.010(3) 0.007(4) C42 0.082(6) 0.054(4) 0.021(3) 0.000(3) 0.006(4) -0.003(4) C43 0.080(6) 0.051(5) 0.025(3) -0.002(3) 0.004(4) -0.005(4) C44 0.049(4) 0.029(4) 0.038(4) 0.005(3) -0.002(3) -0.010(3) C45 0.068(5) 0.045(5) 0.042(4) -0.008(3) 0.003(4) -0.001(4) C46 0.091(6) 0.069(6) 0.034(4) 0.000(4) -0.007(4) 0.008(5) C47 0.113(7) 0.033(4) 0.047(4) -0.005(3) -0.006(5) -0.003(4) C48 0.097(7) 0.047(5) 0.049(5) -0.001(4) -0.000(5) -0.018(5) C49 0.048(4) 0.038(4) 0.037(4) 0.003(3) 0.004(4) 0.008(3) C50 0.046(4) 0.048(4) 0.029(3) -0.003(3) -0.001(3) 0.001(4) C51 0.051(5) 0.042(4) 0.035(4) 0.004(3) 0.017(4) 0.011(4) C52 0.059(5) 0.055(4) 0.022(4) 0.001(3) -0.004(3) -0.000(4) C53 0.074(6) 0.063(5) 0.024(4) 0.008(3) -0.001(4) -0.015(4) C54 0.054(5) 0.054(5) 0.026(4) -0.001(3) 0.005(4) 0.002(4) C55 0.053(5) 0.062(5) 0.037(4) 0.009(3) 0.015(4) -0.002(4) C56 0.066(6) 0.056(5) 0.073(6) 0.007(4) 0.016(5) 0.015(5) C57 0.064(5) 0.059(5) 0.032(4) 0.008(3) -0.002(4) -0.001(4) C58 0.071(6) 0.044(4) 0.035(4) 0.009(3) 0.006(4) 0.011(4) C59 0.059(5) 0.041(4) 0.022(3) 0.011(3) -0.002(4) -0.004(4) C60 0.050(5) 0.033(4) 0.025(3) 0.008(2) -0.004(3) 0.008(3) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 . C1 . 1.313(8) yes O1 . H11 . 0.957(5) no O2 . C21 . 1.352(9) yes O2 . H12 . 0.973(6) no N1 . C7 . 1.298(9) yes N1 . C41 . 1.399(8) yes N2 . C27 . 1.265(9) yes N2 . C51 . 1.423(9) yes N3 . C3 . 1.387(9) yes N3 . C8 . 1.46(1) yes N3 . C10 . 1.45(1) yes N4 . C23 . 1.37(1) yes N4 . C28 . 1.48(1) yes N4 . C30 . 1.52(2) yes C1 . C2 . 1.39(1) yes C1 . C6 . 1.441(9) yes C2 . C3 . 1.41(1) yes C2 . H21 . 0.981(7) no C3 . C4 . 1.40(1) yes C4 . C5 . 1.38(1) yes C4 . H41 . 0.985(7) no C5 . C6 . 1.36(1) yes C5 . H51 . 0.992(6) no C6 . C7 . 1.46(1) yes C7 . H71 . 0.989(7) no C8 . C9 . 1.52(2) yes C8 . H81 . 0.989(8) no C8 . H82 . 0.984(9) no C9 . H91 . 1.00(1) no C9 . H92 . 0.98(1) no C9 . H93 . 0.99(1) no C10 . C11 . 1.57(1) yes C10 . H101 . 0.999(8) no C10 . H102 . 0.994(9) no C11 . H111 . 0.99(1) no C11 . H112 . 0.99(1) no C11 . H113 . 0.988(8) no C21 . C22 . 1.37(1) yes C21 . C26 . 1.36(1) yes C22 . C23 . 1.44(1) yes C22 . H221 . 0.985(7) no C23 . C24 . 1.38(1) yes C24 . C25 . 1.38(1) yes C24 . H241 . 1.006(9) no C25 . C26 . 1.44(1) yes C25 . H251 . 0.994(8) no C26 . C27 . 1.44(1) yes C27 . H271 . 0.991(6) no C28 . C29 . 1.54(2) yes C28 . H281 . 0.98(1) no C28 . H282 . 0.99(1) no C29 . H291 . 1.00(2) no C29 . H292 . 0.97(2) no C29 . H293 . 0.97(2) no C30 . C31 . 1.49(2) yes C30 . H301 . 0.98(1) no C30 . H302 . 0.98(1) no C31 . H311 . 0.99(2) no C31 . H312 . 0.96(2) no C31 . H313 . 1.02(2) no C41 . C42 . 1.439(9) yes C41 . C50 . 1.412(9) yes C42 . C43 . 1.37(1) yes C42 . H421 . 0.988(7) no C43 . C44 . 1.395(9) yes C43 . H431 . 0.993(7) no C44 . C45 . 1.47(1) yes C44 . C49 . 1.386(9) yes C45 . C46 . 1.33(1) yes C45 . H451 . 0.994(7) no C46 . C47 . 1.45(1) yes C46 . H461 . 0.992(8) no C47 . C48 . 1.35(1) yes C47 . H471 . 0.987(7) no C48 . C49 . 1.45(1) yes C48 . H481 . 0.983(8) no C49 . C50 . 1.40(1) yes C50 . C60 . 1.480(9) yes C51 . C52 . 1.402(9) yes C51 . C60 . 1.37(1) yes C52 . C53 . 1.35(1) yes C52 . H521 . 0.976(8) no C53 . C54 . 1.42(1) yes C53 . H531 . 0.982(7) no C54 . C55 . 1.43(1) yes C54 . C59 . 1.423(9) yes C55 . C56 . 1.37(1) yes C55 . H551 . 0.997(7) no C56 . C57 . 1.40(1) yes C56 . H561 . 1.001(8) no C57 . C58 . 1.34(1) yes C57 . H571 . 1.001(8) no C58 . C59 . 1.43(1) yes C58 . H581 . 0.994(7) no C59 . C60 . 1.42(1) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . O1 . H11 . 109.5(5) no C21 . O2 . H12 . 110.9(6) no C7 . N1 . C41 . 122.7(5) yes C27 . N2 . C51 . 121.4(6) yes C3 . N3 . C8 . 120.7(6) yes C3 . N3 . C10 . 121.6(6) yes C8 . N3 . C10 . 116.5(6) yes C23 . N4 . C28 . 122.9(9) yes C23 . N4 . C30 . 118.2(9) yes C28 . N4 . C30 . 115.8(9) yes O1 . C1 . C2 . 117.5(6) yes O1 . C1 . C6 . 122.5(6) yes C2 . C1 . C6 . 120.0(6) yes C1 . C2 . C3 . 120.1(6) yes C1 . C2 . H21 . 119.8(7) no C3 . C2 . H21 . 120.1(7) no N3 . C3 . C2 . 118.8(7) yes N3 . C3 . C4 . 122.2(7) yes C2 . C3 . C4 . 118.9(6) yes C3 . C4 . C5 . 120.1(6) yes C3 . C4 . H41 . 119.9(7) no C5 . C4 . H41 . 120.0(7) no C4 . C5 . C6 . 122.9(6) yes C4 . C5 . H51 . 118.2(6) no C6 . C5 . H51 . 118.9(6) no C1 . C6 . C5 . 118.0(6) yes C1 . C6 . C7 . 119.6(6) yes C5 . C6 . C7 . 122.3(6) yes N1 . C7 . C6 . 120.7(6) yes N1 . C7 . H71 . 119.4(6) no C6 . C7 . H71 . 119.9(7) no N3 . C8 . C9 . 114.6(8) yes N3 . C8 . H81 . 107.8(8) no C9 . C8 . H81 . 107.6(9) no N3 . C8 . H82 . 108.5(8) no C9 . C8 . H82 . 108.3(9) no H81 . C8 . H82 . 110.0(9) no C8 . C9 . H91 . 109.2(10) no C8 . C9 . H92 . 110.7(10) no H91 . C9 . H92 . 109.1(9) no C8 . C9 . H93 . 109.8(8) no H91 . C9 . H93 . 108.2(10) no H92 . C9 . H93 . 109.8(12) no N3 . C10 . C11 . 112.4(8) yes N3 . C10 . H101 . 109.1(7) no C11 . C10 . H101 . 108.6(8) no N3 . C10 . H102 . 109.5(8) no C11 . C10 . H102 . 108.7(8) no H101 . C10 . H102 . 108.4(9) no C10 . C11 . H111 . 109.9(8) no C10 . C11 . H112 . 109.1(7) no H111 . C11 . H112 . 109.4(10) no C10 . C11 . H113 . 109.2(9) no H111 . C11 . H113 . 109.8(8) no H112 . C11 . H113 . 109.4(9) no O2 . C21 . C22 . 117.7(7) yes O2 . C21 . C26 . 119.3(7) yes C22 . C21 . C26 . 122.9(7) yes C21 . C22 . C23 . 120.9(7) yes C21 . C22 . H221 . 118.7(8) no C23 . C22 . H221 . 120.4(7) no N4 . C23 . C22 . 122.0(8) yes N4 . C23 . C24 . 121.4(9) yes C22 . C23 . C24 . 116.4(7) yes C23 . C24 . C25 . 121.2(8) yes C23 . C24 . H241 . 119.4(8) no C25 . C24 . H241 . 119.4(9) no C24 . C25 . C26 . 121.6(7) yes C24 . C25 . H251 . 118.9(9) no C26 . C25 . H251 . 119.4(9) no C21 . C26 . C25 . 116.2(7) yes C21 . C26 . C27 . 123.9(7) yes C25 . C26 . C27 . 119.8(6) yes N2 . C27 . C26 . 120.8(6) yes N2 . C27 . H271 . 119.0(7) no C26 . C27 . H271 . 120.2(8) no N4 . C28 . C29 . 118.0(12) yes N4 . C28 . H281 . 107.3(11) no C29 . C28 . H281 . 107.8(12) no N4 . C28 . H282 . 106.4(10) no C29 . C28 . H282 . 107.1(12) no H281 . C28 . H282 . 110.2(13) no C28 . C29 . H291 . 106.8(14) no C28 . C29 . H292 . 108.4(12) no H291 . C29 . H292 . 110.1(14) no C28 . C29 . H293 . 108.9(12) no H291 . C29 . H293 . 110.1(14) no H292 . C29 . H293 . 112.4(18) no N4 . C30 . C31 . 107.2(13) yes N4 . C30 . H301 . 108.7(12) no C31 . C30 . H301 . 109.1(13) no N4 . C30 . H302 . 108.6(10) no C31 . C30 . H302 . 111.8(14) no H301 . C30 . H302 . 111.4(13) no C30 . C31 . H311 . 109.0(20) no C30 . C31 . H312 . 112.1(14) no H311 . C31 . H312 . 111.8(14) no C30 . C31 . H313 . 108.2(12) no H311 . C31 . H313 . 106.9(15) no H312 . C31 . H313 . 108.6(23) no N1 . C41 . C42 . 124.5(6) yes N1 . C41 . C50 . 116.5(6) yes C42 . C41 . C50 . 119.0(6) yes C41 . C42 . C43 . 119.8(6) yes C41 . C42 . H421 . 119.2(6) no C43 . C42 . H421 . 121.0(6) no C42 . C43 . C44 . 120.6(6) yes C42 . C43 . H431 . 119.4(7) no C44 . C43 . H431 . 120.0(6) no C43 . C44 . C45 . 120.2(6) yes C43 . C44 . C49 . 120.3(6) yes C45 . C44 . C49 . 119.4(6) yes C44 . C45 . C46 . 122.0(7) yes C44 . C45 . H451 . 119.3(6) no C46 . C45 . H451 . 118.7(7) no C45 . C46 . C47 . 117.7(7) yes C45 . C46 . H461 . 121.9(7) no C47 . C46 . H461 . 120.3(8) no C46 . C47 . C48 . 122.3(7) yes C46 . C47 . H471 . 118.9(7) no C48 . C47 . H471 . 118.8(7) no C47 . C48 . C49 . 120.0(7) yes C47 . C48 . H481 . 119.7(7) no C49 . C48 . H481 . 120.3(7) no C44 . C49 . C48 . 118.5(6) yes C44 . C49 . C50 . 120.8(6) yes C48 . C49 . C50 . 120.6(6) yes C41 . C50 . C49 . 119.3(6) yes C41 . C50 . C60 . 118.3(6) yes C49 . C50 . C60 . 122.0(6) yes N2 . C51 . C52 . 122.0(7) yes N2 . C51 . C60 . 114.5(6) yes C52 . C51 . C60 . 123.5(7) yes C51 . C52 . C53 . 118.7(7) yes C51 . C52 . H521 . 121.7(7) no C53 . C52 . H521 . 119.5(7) no C52 . C53 . C54 . 121.8(6) yes C52 . C53 . H531 . 118.8(8) no C54 . C53 . H531 . 119.4(8) no C53 . C54 . C55 . 122.1(6) yes C53 . C54 . C59 . 118.0(6) yes C55 . C54 . C59 . 119.8(7) yes C54 . C55 . C56 . 120.4(7) yes C54 . C55 . H551 . 120.8(8) no C56 . C55 . H551 . 118.8(7) no C55 . C56 . C57 . 119.0(7) yes C55 . C56 . H561 . 120.5(8) no C57 . C56 . H561 . 120.5(9) no C56 . C57 . C58 . 122.9(8) yes C56 . C57 . H571 . 118.1(7) no C58 . C57 . H571 . 119.0(7) no C57 . C58 . C59 . 120.6(7) yes C57 . C58 . H581 . 119.8(8) no C59 . C58 . H581 . 119.5(7) no C54 . C59 . C58 . 117.2(6) yes C54 . C59 . C60 . 120.2(6) yes C58 . C59 . C60 . 122.6(6) yes C50 . C60 . C51 . 120.8(6) yes C50 . C60 . C59 . 121.4(6) yes C51 . C60 . C59 . 117.7(6) yes #========================END # complex NiL2 data_(NiL2) _audit_creation_method SHELXL _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H40 N4 Ni O2' _chemical_formula_weight 619.43 _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' 0.0033 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a '13.660(2)' _cell_length_b '10.601(2)' _cell_length_c '12.340(2)' _cell_angle_alpha 90.00 _cell_angle_beta '112.086(11)' _cell_angle_gamma 90.00 _cell_volume '1655.7(4)' _cell_formula_units_Z 2 _cell_measurement_temperature '293(2)' _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.332 _cell_measurement_theta_max 15.890 _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method ? _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.9071 _exptl_absorpt_correction_T_max 0.9993 _exptl_special_details ; ? ; _diffrn_ambient_temperature '293(2)' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4 Enraf-Nonius' _diffrn_measurement_method \w/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -0.5 _diffrn_reflns_number 6127 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 24.97 _reflns_number_total 5842 _reflns_number_observed 4749 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4-EXPRESS' _computing_cell_refinement 'CAD4-EXPRESS' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'cameron' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.6234P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.015(13) _refine_ls_number_reflns 5842 _refine_ls_number_parameters 388 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_obs 0.0352 _refine_ls_wR_factor_all 0.0632 _refine_ls_wR_factor_obs 0.0568 _refine_ls_goodness_of_fit_all 1.076 _refine_ls_goodness_of_fit_obs 1.115 _refine_ls_restrained_S_all 1.076 _refine_ls_restrained_S_obs 1.115 _refine_ls_shift/esd_max 0.000 _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 Ni Ni 0.47071(3) 0.50028(4) 0.35405(3) 0.03749(10) Uani 1 d . . O1 O 0.4695(2) 0.3792(2) 0.2453(2) 0.0421(5) Uani 1 d . . C1 C 0.3901(2) 0.3409(3) 0.1536(3) 0.0369(7) Uani 1 d . . C2 C 0.4079(3) 0.2513(3) 0.0793(3) 0.0461(8) Uani 1 d . . H2 H 0.4760(3) 0.2201(3) 0.0988(3) 0.051 Uiso 1 calc R . C3 C 0.3292(3) 0.2067(3) -0.0219(3) 0.0448(8) Uani 1 d . . C4 C 0.2254(3) 0.2510(3) -0.0481(3) 0.0531(8) Uani 1 d . . H4 H 0.1701(3) 0.2206(3) -0.1131(3) 0.058 Uiso 1 calc R . C5 C 0.2067(3) 0.3400(3) 0.0237(3) 0.0501(8) Uani 1 d . . H5 H 0.1380(3) 0.3695(3) 0.0039(3) 0.055 Uiso 1 calc R . C6 C 0.2856(3) 0.3882(3) 0.1246(3) 0.0433(8) Uani 1 d . . C7 C 0.2612(2) 0.4808(3) 0.1937(3) 0.0430(8) Uani 1 d . . H7 H 0.1911(2) 0.5067(3) 0.1692(3) 0.047 Uiso 1 calc R . O2 O 0.6142(2) 0.4723(2) 0.4143(2) 0.0476(6) Uani 1 d . . C8 C 0.6884(3) 0.5380(3) 0.4982(3) 0.0433(8) Uani 1 d . . C9 C 0.7929(2) 0.5139(4) 0.5193(3) 0.0527(8) Uani 1 d . . H9 H 0.8095(2) 0.4506(4) 0.4768(3) 0.058 Uiso 1 calc R . C10 C 0.8760(3) 0.5820(4) 0.6033(3) 0.0591(9) Uani 1 d . . C11 C 0.8458(3) 0.6757(4) 0.6688(3) 0.0585(9) Uani 1 d . . H11 H 0.8975(3) 0.7233(4) 0.7249(3) 0.064 Uiso 1 calc R . C12 C 0.7447(3) 0.6953(3) 0.6501(3) 0.0518(9) Uani 1 d . . H12 H 0.7284(3) 0.7539(3) 0.6968(3) 0.057 Uiso 1 calc R . C13 C 0.6613(3) 0.6325(3) 0.5641(3) 0.0461(8) Uani 1 d . . C14 C 0.5573(3) 0.6610(3) 0.5476(3) 0.0431(8) Uani 1 d . . H14 H 0.5471(3) 0.7178(3) 0.5998(3) 0.047 Uiso 1 calc R . N1 N 0.3274(2) 0.5323(2) 0.2876(2) 0.0412(7) Uani 1 d . . C15 C 0.2877(3) 0.6338(3) 0.3431(3) 0.0468(8) Uani 1 d . . H15 H 0.2206(3) 0.6070(3) 0.3474(3) 0.051 Uiso 1 calc R . C17 C 0.2691(3) 0.7542(3) 0.2690(3) 0.0520(8) Uani 1 d . . C18 C 0.1668(3) 0.7905(4) 0.2013(4) 0.0687(11) Uani 1 d . . H18 H 0.1097(3) 0.7439(4) 0.2033(4) 0.076 Uiso 1 calc R . C19 C 0.1497(4) 0.8965(4) 0.1306(4) 0.0760(12) Uani 1 d . . H19 H 0.0814(4) 0.9183(4) 0.0818(4) 0.084 Uiso 1 calc R . C20 C 0.2331(4) 0.9687(4) 0.1326(4) 0.0771(13) Uani 1 d . . H20 H 0.2208(4) 1.0422(4) 0.0883(4) 0.085 Uiso 1 calc R . C21 C 0.3343(3) 0.9342(4) 0.1989(4) 0.0657(10) Uani 1 d . . H21 H 0.3909(3) 0.9824(4) 0.1981(4) 0.072 Uiso 1 calc R . C22 C 0.3515(3) 0.8283(4) 0.2663(4) 0.0610(10) Uani 1 d . . H22 H 0.4205(3) 0.8052(4) 0.3117(4) 0.067 Uiso 1 calc R . N2 N 0.4734(2) 0.6161(2) 0.4669(2) 0.0420(6) Uani 1 d . . C16 C 0.3692(3) 0.6531(3) 0.4678(3) 0.0456(8) Uani 1 d . . H16 H 0.3713(3) 0.7429(3) 0.4875(3) 0.050 Uiso 1 calc R . C23 C 0.3478(3) 0.5767(4) 0.5622(3) 0.0449(9) Uani 1 d . . C24 C 0.3309(3) 0.4467(4) 0.5505(4) 0.0566(10) Uani 1 d . . H24 H 0.3273(3) 0.4053(4) 0.4827(4) 0.062 Uiso 1 calc R . C25 C 0.3195(3) 0.3807(4) 0.6417(4) 0.0605(11) Uani 1 d . . H25 H 0.3093(3) 0.2939(4) 0.6356(4) 0.067 Uiso 1 calc R . C26 C 0.3229(4) 0.4415(5) 0.7409(4) 0.0646(12) Uani 1 d . . H26 H 0.3186(4) 0.3958(5) 0.8032(4) 0.071 Uiso 1 calc R . C27 C 0.3328(3) 0.5702(5) 0.7478(4) 0.0619(12) Uani 1 d . . H27 H 0.3295(3) 0.6123(5) 0.8125(4) 0.068 Uiso 1 calc R . C28 C 0.3475(3) 0.6377(4) 0.6596(3) 0.0502(9) Uani 1 d . . H28 H 0.3572(3) 0.7246(4) 0.6664(3) 0.055 Uiso 1 calc R . N3 N 0.3517(3) 0.1203(3) -0.0923(3) 0.0610(8) Uani 1 d . . C29 C 0.4567(3) 0.0685(4) -0.0600(3) 0.0659(11) Uani 1 d . . H29A H 0.4521(3) -0.0113(4) -0.1001(3) 0.072 Uiso 1 calc R . H29B H 0.4852(3) 0.0516(4) 0.0234(3) 0.072 Uiso 1 calc R . C30 C 0.5322(4) 0.1541(4) -0.0888(4) 0.0782(13) Uani 1 d . . H30A H 0.6002(4) 0.1144(4) -0.0652(4) 0.086 Uiso 1 calc R . H30B H 0.5387(4) 0.2326(4) -0.0479(4) 0.086 Uiso 1 calc R . H30C H 0.5056(4) 0.1696(4) -0.1715(4) 0.086 Uiso 1 calc R . C31 C 0.2731(4) 0.0764(4) -0.2015(4) 0.0730(13) Uani 1 d . . H31A H 0.3064(4) 0.0625(4) -0.2574(4) 0.080 Uiso 1 calc R . H31B H 0.2196(4) 0.1411(4) -0.2329(4) 0.080 Uiso 1 calc R . C32 C 0.2210(5) -0.0438(5) -0.1864(5) 0.111(2) Uani 1 d . . H32A H 0.1697(5) -0.0695(5) -0.2606(5) 0.122 Uiso 1 calc R . H32B H 0.1868(5) -0.0300(5) -0.1323(5) 0.122 Uiso 1 calc R . H32C H 0.2735(5) -0.1085(5) -0.1568(5) 0.122 Uiso 1 calc R . N4 N 0.9808(3) 0.5618(4) 0.6224(3) 0.0772(11) Uani 1 d . . C33 C 1.0645(3) 0.6458(4) 0.7006(4) 0.0783(13) Uani 1 d . . H33A H 1.0376(3) 0.7313(4) 0.6934(4) 0.086 Uiso 1 calc R . H33B H 1.1242(3) 0.6456(4) 0.6761(4) 0.086 Uiso 1 calc R . C34 C 1.1010(4) 0.6058(5) 0.8255(5) 0.099(2) Uani 1 d . . H34A H 1.1549(4) 0.6625(5) 0.8729(5) 0.109 Uiso 1 calc R . H34B H 1.1290(4) 0.5218(5) 0.8334(5) 0.109 Uiso 1 calc R . H34C H 1.0425(4) 0.6074(5) 0.8506(5) 0.109 Uiso 1 calc R . C35 C 1.0118(4) 0.4671(5) 0.5557(5) 0.104(2) Uani 1 d . . H35A H 1.0823(4) 0.4870(5) 0.5594(5) 0.114 Uiso 1 calc R . H35B H 0.9643(4) 0.4729(5) 0.4744(5) 0.114 Uiso 1 calc R . C36 C 1.0113(5) 0.3354(7) 0.5951(6) 0.136(3) Uani 1 d . . H36A H 1.0325(5) 0.2799(7) 0.5465(6) 0.150 Uiso 1 calc R . H36B H 0.9414(5) 0.3134(7) 0.5896(6) 0.150 Uiso 1 calc R . H36C H 1.0596(5) 0.3274(7) 0.6748(6) 0.150 Uiso 1 calc R . 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 Ni 0.0491(2) 0.0270(2) 0.0414(2) -0.0017(2) 0.02277(14) 0.0017(2) O1 0.0480(14) 0.0326(12) 0.0448(13) -0.0063(10) 0.0164(11) 0.0026(10) C1 0.040(2) 0.035(2) 0.036(2) 0.0013(13) 0.0138(14) -0.0022(13) C2 0.052(2) 0.039(2) 0.046(2) -0.0024(15) 0.018(2) 0.000(2) C3 0.054(2) 0.040(2) 0.043(2) -0.0032(14) 0.020(2) -0.0084(15) C4 0.054(2) 0.053(2) 0.048(2) 0.000(2) 0.015(2) -0.001(2) C5 0.049(2) 0.050(2) 0.049(2) 0.001(2) 0.017(2) 0.001(2) C6 0.048(2) 0.036(2) 0.047(2) 0.0005(14) 0.020(2) -0.0015(14) C7 0.045(2) 0.040(2) 0.048(2) 0.007(2) 0.0208(14) 0.001(2) O2 0.0538(13) 0.037(2) 0.0525(13) -0.0119(10) 0.0202(11) 0.0050(10) C8 0.049(2) 0.040(2) 0.038(2) 0.0000(12) 0.013(2) -0.0004(13) C9 0.052(2) 0.053(2) 0.049(2) -0.007(2) 0.0146(14) 0.000(2) C10 0.059(2) 0.061(2) 0.055(2) -0.006(2) 0.020(2) -0.004(2) C11 0.052(2) 0.061(2) 0.058(2) -0.012(2) 0.015(2) -0.004(2) C12 0.050(2) 0.047(2) 0.058(2) -0.006(2) 0.020(2) 0.000(2) C13 0.049(2) 0.038(2) 0.049(2) -0.004(2) 0.016(2) -0.0012(15) C14 0.049(2) 0.039(2) 0.044(2) -0.0059(14) 0.019(2) -0.0043(15) N1 0.0458(14) 0.038(2) 0.0451(14) 0.0059(11) 0.0224(12) 0.0065(11) C15 0.055(2) 0.040(2) 0.057(2) 0.004(2) 0.034(2) 0.0085(15) C17 0.061(2) 0.046(2) 0.055(2) -0.002(2) 0.028(2) 0.006(2) C18 0.061(3) 0.066(3) 0.080(3) 0.013(2) 0.028(2) 0.012(2) C19 0.068(3) 0.078(3) 0.075(3) 0.011(2) 0.019(2) 0.018(2) C20 0.082(3) 0.078(4) 0.073(3) 0.006(2) 0.032(2) 0.009(2) C21 0.069(3) 0.062(2) 0.073(3) 0.009(2) 0.034(2) 0.005(2) C22 0.068(2) 0.052(2) 0.067(2) 0.003(2) 0.030(2) 0.003(2) N2 0.057(2) 0.0304(14) 0.050(2) 0.0022(12) 0.0324(14) 0.0016(12) C16 0.060(2) 0.033(2) 0.055(2) -0.0021(14) 0.035(2) 0.0055(15) C23 0.044(2) 0.048(2) 0.046(2) 0.001(2) 0.020(2) 0.000(2) C24 0.063(3) 0.053(2) 0.059(2) 0.001(2) 0.028(2) -0.002(2) C25 0.062(3) 0.049(2) 0.072(3) 0.005(2) 0.027(2) -0.005(2) C26 0.065(3) 0.071(3) 0.060(3) 0.012(2) 0.026(2) 0.002(2) C27 0.059(3) 0.079(4) 0.047(3) 0.001(2) 0.020(2) -0.002(2) C28 0.053(2) 0.054(2) 0.050(2) -0.005(2) 0.028(2) -0.007(2) N3 0.080(2) 0.050(2) 0.050(2) -0.0129(15) 0.022(2) -0.006(2) C29 0.084(3) 0.051(2) 0.058(2) -0.022(2) 0.020(2) 0.006(2) C30 0.084(3) 0.086(3) 0.074(3) -0.032(2) 0.040(2) -0.002(3) C31 0.093(3) 0.066(3) 0.051(2) -0.012(2) 0.016(2) -0.012(2) C32 0.134(5) 0.082(4) 0.090(4) -0.018(3) 0.013(3) -0.050(3) N4 0.045(2) 0.089(3) 0.082(2) -0.026(2) 0.006(2) 0.011(2) C33 0.066(3) 0.072(3) 0.083(3) 0.005(3) 0.012(2) -0.015(2) C34 0.087(4) 0.093(4) 0.107(4) 0.006(3) 0.022(3) -0.005(3) C35 0.058(3) 0.102(5) 0.123(4) -0.029(3) 0.003(3) 0.013(3) C36 0.133(6) 0.146(7) 0.104(5) -0.024(5) 0.015(4) 0.027(5) _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 Ni O2 1.840(2) . ? Ni N2 1.846(3) . ? Ni N1 1.848(3) . ? Ni O1 1.853(2) . ? O1 C1 1.303(4) . ? C1 C2 1.403(4) . ? C1 C6 1.426(4) . ? C2 C3 1.388(5) . ? C3 N3 1.375(4) . ? C3 C4 1.411(5) . ? C4 C5 1.382(5) . ? C5 C6 1.402(5) . ? C6 C7 1.420(4) . ? C7 N1 1.293(4) . ? O2 C8 1.339(4) . ? C8 C9 1.376(4) . ? C8 C13 1.424(4) . ? C9 C10 1.414(5) . ? C10 N4 1.378(5) . ? C10 C11 1.437(5) . ? C11 C12 1.328(5) . ? C12 C13 1.399(5) . ? C13 C14 1.390(5) . ? C14 N2 1.294(4) . ? N1 C15 1.483(4) . ? C15 C17 1.534(5) . ? C15 C16 1.536(5) . ? C17 C22 1.382(5) . ? C17 C18 1.387(5) . ? C18 C19 1.388(6) . ? C19 C20 1.365(6) . ? C20 C21 1.365(6) . ? C21 C22 1.364(5) . ? N2 C16 1.480(4) . ? C16 C23 1.535(5) . ? C23 C28 1.366(5) . ? C23 C24 1.396(5) . ? C24 C25 1.382(6) . ? C25 C26 1.368(6) . ? C26 C27 1.370(5) . ? C27 C28 1.379(6) . ? N3 C29 1.445(5) . ? N3 C31 1.448(5) . ? C29 C30 1.513(6) . ? C31 C32 1.504(6) . ? N4 C35 1.458(6) . ? N4 C33 1.483(5) . ? C33 C34 1.492(6) . ? C35 C36 1.479(9) . ? 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 O2 Ni N2 94.95(11) . . ? O2 Ni N1 177.30(11) . . ? N2 Ni N1 85.96(12) . . ? O2 Ni O1 84.22(9) . . ? N2 Ni O1 177.78(11) . . ? N1 Ni O1 94.96(10) . . ? C1 O1 Ni 128.5(2) . . ? O1 C1 C2 119.1(3) . . ? O1 C1 C6 122.4(3) . . ? C2 C1 C6 118.5(3) . . ? C3 C2 C1 123.5(3) . . ? N3 C3 C2 120.9(3) . . ? N3 C3 C4 121.4(3) . . ? C2 C3 C4 117.7(3) . . ? C5 C4 C3 119.5(3) . . ? C4 C5 C6 123.5(3) . . ? C5 C6 C7 120.6(3) . . ? C5 C6 C1 117.3(3) . . ? C7 C6 C1 122.1(3) . . ? N1 C7 C6 126.0(3) . . ? C8 O2 Ni 127.6(2) . . ? O2 C8 C9 118.7(3) . . ? O2 C8 C13 121.6(3) . . ? C9 C8 C13 119.8(3) . . ? C8 C9 C10 122.3(4) . . ? N4 C10 C9 122.9(3) . . ? N4 C10 C11 120.7(3) . . ? C9 C10 C11 116.4(3) . . ? C12 C11 C10 120.7(3) . . ? C11 C12 C13 123.7(3) . . ? C14 C13 C12 120.2(3) . . ? C14 C13 C8 122.7(3) . . ? C12 C13 C8 117.1(3) . . ? N2 C14 C13 126.4(3) . . ? C7 N1 C15 117.8(3) . . ? C7 N1 Ni 126.0(2) . . ? C15 N1 Ni 116.0(2) . . ? N1 C15 C17 109.6(2) . . ? N1 C15 C16 107.8(3) . . ? C17 C15 C16 112.4(3) . . ? C22 C17 C18 118.3(4) . . ? C22 C17 C15 122.2(3) . . ? C18 C17 C15 119.5(3) . . ? C17 C18 C19 119.7(4) . . ? C20 C19 C18 120.1(4) . . ? C21 C20 C19 120.7(4) . . ? C22 C21 C20 119.3(4) . . ? C21 C22 C17 121.8(4) . . ? C14 N2 C16 118.2(3) . . ? C14 N2 Ni 125.9(2) . . ? C16 N2 Ni 115.8(2) . . ? N2 C16 C23 108.9(3) . . ? N2 C16 C15 107.1(2) . . ? C23 C16 C15 114.6(3) . . ? C28 C23 C24 120.2(4) . . ? C28 C23 C16 118.9(3) . . ? C24 C23 C16 120.9(4) . . ? C25 C24 C23 118.7(4) . . ? C26 C25 C24 120.9(4) . . ? C25 C26 C27 119.6(5) . . ? C26 C27 C28 120.5(5) . . ? C23 C28 C27 119.9(4) . . ? C3 N3 C29 120.9(3) . . ? C3 N3 C31 122.6(4) . . ? C29 N3 C31 116.5(3) . . ? N3 C29 C30 113.6(3) . . ? N3 C31 C32 112.1(4) . . ? C10 N4 C35 120.9(4) . . ? C10 N4 C33 121.0(4) . . ? C35 N4 C33 117.7(4) . . ? N4 C33 C34 112.2(4) . . ? N4 C35 C36 115.3(6) . . ? _refine_diff_density_max 0.176 _refine_diff_density_min -0.163 _refine_diff_density_rms 0.038 #========================END # complex (NiL3)2Ni(AcO)2(H2O) data_fatri _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_formula_sum 'C88 H88 N8 Ni3 O9' _chemical_formula_weight 1577.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a '12.9998(10)' _cell_length_b '16.1021(16)' _cell_length_c '36.377(3)' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume '7614.7(11)' _cell_formula_units_Z 4 _cell_measurement_temperature 180 _cell_measurement_reflns_used 28880 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 20.99 _exptl_crystal_description 'elongated plate' _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 0.800 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180 _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 'stoe ipds' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28880 _diffrn_reflns_av_R_equivalents 0.1229 _diffrn_reflns_av_sigmaI/netI 0.0884 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 20.99 _reflns_number_total 8073 _reflns_number_gt 5977 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ipds-stoe' _computing_cell_refinement 'ipds-stoe' _computing_data_reduction 'ipds-stoe' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'cameron' _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^)+(0.1329P)^2^+5.4227P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 8073 _refine_ls_number_parameters 974 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.2080 _refine_ls_wR_factor_gt 0.1862 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.017 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 Ni1 Ni 0.24177(11) 0.28168(8) 0.85635(5) 0.0606(5) Uani 1 d . . . O101 O 0.2624(6) 0.1618(4) 0.8439(3) 0.071(3) Uani 1 d . . . O102 O 0.1503(5) 0.2293(4) 0.8939(2) 0.0564(19) Uani 1 d . . . N101 N 0.3322(8) 0.3125(6) 0.8137(3) 0.062(3) Uani 1 d . . . N102 N 0.2763(7) 0.3780(5) 0.8897(3) 0.057(2) Uani 1 d . . . N103 N 0.4521(8) -0.0827(6) 0.8145(3) 0.074(3) Uani 1 d . . . N104 N -0.1298(8) 0.2477(6) 0.9785(3) 0.070(3) Uani 1 d . . . C101 C 0.3325(9) 0.1263(7) 0.8239(4) 0.064(3) Uani 1 d . . . C102 C 0.3522(10) 0.0421(8) 0.8270(4) 0.072(4) Uani 1 d . . . H102 H 0.3098 0.0117 0.8426 0.087 Uiso 1 calc R . . C103 C 0.4314(9) -0.0024(8) 0.8084(4) 0.067(3) Uani 1 d . . . C104 C 0.4899(9) 0.0485(8) 0.7837(4) 0.073(4) Uani 1 d . . . H104 H 0.5434 0.0248 0.7704 0.087 Uiso 1 calc R . . C105 C 0.4689(10) 0.1303(7) 0.7795(4) 0.069(3) Uani 1 d . . . H105 H 0.5065 0.1598 0.7621 0.083 Uiso 1 calc R . . C106 C 0.3950(8) 0.1725(6) 0.7994(3) 0.054(3) Uani 1 d . . . C107 C 0.3809(10) 0.2614(8) 0.7943(4) 0.069(4) Uani 1 d . . . H107 H 0.4126 0.2837 0.7736 0.083 Uiso 1 calc R . . C108 C 0.5353(12) -0.1222(9) 0.7975(4) 0.091(4) Uani 1 d . . . H10A H 0.5862 -0.0804 0.7914 0.110 Uiso 1 calc R . . H10B H 0.5114 -0.1463 0.7746 0.110 Uiso 1 calc R . . C109 C 0.5866(15) -0.1883(11) 0.8191(6) 0.141(8) Uani 1 d . . . H10C H 0.6459 -0.2079 0.8060 0.212 Uiso 1 calc R . . H10D H 0.5395 -0.2334 0.8229 0.212 Uiso 1 calc R . . H10E H 0.6076 -0.1663 0.8425 0.212 Uiso 1 calc R . . C110 C 0.3771(11) -0.1369(8) 0.8317(5) 0.085(4) Uani 1 d . . . H11A H 0.3087 -0.1158 0.8265 0.102 Uiso 1 calc R . . H11B H 0.3824 -0.1916 0.8208 0.102 Uiso 1 calc R . . C111 C 0.3888(13) -0.1444(9) 0.8703(5) 0.098(5) Uani 1 d . . . H11C H 0.3238 -0.1585 0.8811 0.148 Uiso 1 calc R . . H11D H 0.4124 -0.0925 0.8802 0.148 Uiso 1 calc R . . H11E H 0.4381 -0.1871 0.8756 0.148 Uiso 1 calc R . . C121 C 0.1003(9) 0.2704(7) 0.9202(3) 0.058(3) Uani 1 d . . . C122 C 0.0169(9) 0.2369(7) 0.9368(4) 0.061(3) Uani 1 d . . . H122 H -0.0039 0.1838 0.9300 0.074 Uiso 1 calc R . . C123 C -0.0395(10) 0.2787(8) 0.9639(4) 0.077(4) Uani 1 d . . . C124 C -0.0004(10) 0.3557(7) 0.9776(4) 0.073(4) Uani 1 d . . . H124 H -0.0328 0.3829 0.9969 0.087 Uiso 1 calc R . . C125 C 0.0851(10) 0.3882(7) 0.9618(4) 0.066(3) Uani 1 d . . . H125 H 0.1117 0.4373 0.9714 0.080 Uiso 1 calc R . . C126 C 0.1351(9) 0.3522(7) 0.9320(4) 0.064(3) Uani 1 d . . . C127 C 0.2220(9) 0.3956(7) 0.9176(4) 0.060(3) Uani 1 d . . . H127 H 0.2412 0.4432 0.9303 0.072 Uiso 1 calc R . . C128 C -0.1773(11) 0.1748(7) 0.9608(5) 0.087(5) Uani 1 d . . . H12A H -0.1639 0.1769 0.9346 0.105 Uiso 1 calc R . . H12B H -0.2513 0.1773 0.9643 0.105 Uiso 1 calc R . . C129 C -0.1374(12) 0.0934(8) 0.9760(5) 0.091(5) Uani 1 d . . . H12C H -0.1718 0.0480 0.9641 0.137 Uiso 1 calc R . . H12D H -0.1503 0.0910 1.0020 0.137 Uiso 1 calc R . . H12E H -0.0647 0.0895 0.9717 0.137 Uiso 1 calc R . . C130 C -0.1876(10) 0.2867(8) 1.0080(4) 0.077(4) Uani 1 d . . . H13A H -0.1399 0.3158 1.0239 0.092 Uiso 1 calc R . . H13B H -0.2203 0.2435 1.0225 0.092 Uiso 1 calc R . . C131 C -0.2694(11) 0.3471(10) 0.9954(5) 0.100(5) Uani 1 d . . . H13C H -0.3100 0.3643 1.0161 0.149 Uiso 1 calc R . . H13D H -0.3129 0.3207 0.9775 0.149 Uiso 1 calc R . . H13E H -0.2371 0.3948 0.9845 0.149 Uiso 1 calc R . . C141 C 0.3058(9) 0.3938(7) 0.7991(4) 0.060(3) Uani 1 d . . . C142 C 0.2511(10) 0.3942(8) 0.7663(4) 0.074(4) Uani 1 d . . . H142 H 0.2409 0.3455 0.7530 0.089 Uiso 1 calc R . . C143 C 0.2121(9) 0.4687(9) 0.7538(4) 0.075(4) Uani 1 d . . . H143 H 0.1782 0.4709 0.7313 0.091 Uiso 1 calc R . . C144 C 0.2232(9) 0.5409(7) 0.7747(4) 0.066(3) Uani 1 d . . . C145 C 0.1773(9) 0.6171(9) 0.7620(5) 0.088(5) Uani 1 d . . . H145 H 0.1437 0.6203 0.7395 0.105 Uiso 1 calc R . . C146 C 0.1856(12) 0.6847(10) 0.7848(6) 0.097(5) Uani 1 d . . . H146 H 0.1566 0.7345 0.7771 0.116 Uiso 1 calc R . . C147 C 0.2334(11) 0.6831(8) 0.8178(6) 0.096(5) Uani 1 d . . . H147 H 0.2334 0.7301 0.8326 0.116 Uiso 1 calc R . . C148 C 0.2816(9) 0.6128(7) 0.8293(4) 0.075(4) Uani 1 d . . . H148 H 0.3170 0.6128 0.8515 0.090 Uiso 1 calc R . . C149 C 0.2780(9) 0.5392(7) 0.8076(4) 0.069(4) Uani 1 d . . . C150 C 0.3224(9) 0.4629(7) 0.8197(4) 0.066(3) Uani 1 d . . . C151 C 0.3716(9) 0.4263(7) 0.8850(4) 0.065(3) Uani 1 d . . . C152 C 0.4347(10) 0.4334(7) 0.9158(4) 0.074(4) Uani 1 d . . . H152 H 0.4165 0.4071 0.9376 0.089 Uiso 1 calc R . . C153 C 0.5261(10) 0.4802(8) 0.9139(5) 0.077(4) Uani 1 d . . . H153 H 0.5677 0.4876 0.9345 0.092 Uiso 1 calc R . . C154 C 0.5514(8) 0.5152(7) 0.8802(4) 0.063(3) Uani 1 d . . . C155 C 0.6481(9) 0.5594(7) 0.8772(5) 0.075(4) Uani 1 d . . . H155 H 0.6888 0.5667 0.8980 0.090 Uiso 1 calc R . . C156 C 0.6806(11) 0.5908(8) 0.8439(5) 0.082(5) Uani 1 d . . . H156 H 0.7442 0.6169 0.8419 0.098 Uiso 1 calc R . . C157 C 0.6178(10) 0.5830(7) 0.8136(5) 0.080(4) Uani 1 d . . . H157 H 0.6386 0.6058 0.7913 0.096 Uiso 1 calc R . . C158 C 0.5241(9) 0.5418(7) 0.8157(4) 0.067(3) Uani 1 d . . . H158 H 0.4829 0.5374 0.7949 0.081 Uiso 1 calc R . . C159 C 0.4908(8) 0.5067(6) 0.8490(4) 0.067(4) Uani 1 d . . . C160 C 0.3936(9) 0.4618(7) 0.8521(4) 0.067(3) Uani 1 d . . . Ni2 Ni 0.03042(12) -0.02803(9) 0.88471(6) 0.0754(6) Uani 1 d . . . O201 O 0.1477(5) 0.0427(4) 0.9006(2) 0.064(2) Uani 1 d . . . O202 O -0.0292(6) 0.0871(4) 0.8802(2) 0.058(2) Uani 1 d . . . N201 N -0.1013(7) -0.0792(5) 0.8678(3) 0.065(3) Uani 1 d . . . N202 N 0.0341(8) -0.0901(5) 0.9345(3) 0.064(3) Uani 1 d . . . N203 N 0.5007(7) 0.0699(6) 0.9309(3) 0.072(3) Uani 1 d . . . N204 N -0.2512(8) 0.3053(6) 0.8403(3) 0.081(3) Uani 1 d . . . C201 C 0.2253(9) 0.0182(6) 0.9208(4) 0.061(3) Uani 1 d . . . C202 C 0.3191(9) 0.0590(6) 0.9175(4) 0.064(3) Uani 1 d . . . H202 H 0.3251 0.1042 0.9017 0.077 Uiso 1 calc R . . C203 C 0.4035(9) 0.0328(7) 0.9375(4) 0.070(4) Uani 1 d . . . C204 C 0.3951(10) -0.0355(7) 0.9622(4) 0.073(4) Uani 1 d . . . H204 H 0.4524 -0.0557 0.9745 0.087 Uiso 1 calc R . . C205 C 0.3020(10) -0.0698(7) 0.9670(4) 0.069(4) Uani 1 d . . . H205 H 0.2943 -0.1098 0.9853 0.083 Uiso 1 calc R . . C206 C 0.2163(9) -0.0482(7) 0.9460(4) 0.072(4) Uani 1 d . . . C207 C 0.1206(12) -0.0928(7) 0.9538(4) 0.079(4) Uani 1 d . . . H207 H 0.1205 -0.1268 0.9744 0.095 Uiso 1 calc R . . C208 C 0.5986(10) 0.0324(8) 0.9445(4) 0.086(4) Uani 1 d . . . H20A H 0.5883 0.0098 0.9689 0.103 Uiso 1 calc R . . H20B H 0.6516 0.0746 0.9458 0.103 Uiso 1 calc R . . C209 C 0.6330(11) -0.0379(9) 0.9179(5) 0.104(5) Uani 1 d . . . H20C H 0.6902 -0.0672 0.9284 0.156 Uiso 1 calc R . . H20D H 0.6531 -0.0141 0.8948 0.156 Uiso 1 calc R . . H20E H 0.5769 -0.0757 0.9141 0.156 Uiso 1 calc R . . C210 C 0.5164(9) 0.1288(8) 0.9011(4) 0.075(4) Uani 1 d . . . H21A H 0.4724 0.1133 0.8807 0.090 Uiso 1 calc R . . H21B H 0.5872 0.1246 0.8928 0.090 Uiso 1 calc R . . C211 C 0.4938(13) 0.2207(9) 0.9117(5) 0.108(5) Uani 1 d . . . H21C H 0.5200 0.2569 0.8929 0.163 Uiso 1 calc R . . H21D H 0.5265 0.2334 0.9347 0.163 Uiso 1 calc R . . H21E H 0.4209 0.2286 0.9140 0.163 Uiso 1 calc R . . C221 C -0.1172(9) 0.1092(7) 0.8633(3) 0.059(3) Uani 1 d . . . C222 C -0.1404(9) 0.1928(6) 0.8617(4) 0.067(3) Uani 1 d . . . H222 H -0.0965 0.2309 0.8728 0.080 Uiso 1 calc R . . C223 C -0.2310(9) 0.2220(7) 0.8433(4) 0.064(3) Uani 1 d . . . C224 C -0.2980(10) 0.1624(8) 0.8275(4) 0.071(4) Uani 1 d . . . H224 H -0.3564 0.1790 0.8147 0.085 Uiso 1 calc R . . C225 C -0.2745(9) 0.0787(7) 0.8314(4) 0.066(3) Uani 1 d . . . H225 H -0.3189 0.0400 0.8210 0.079 Uiso 1 calc R . . C226 C -0.1876(8) 0.0492(7) 0.8501(4) 0.059(3) Uani 1 d . . . C227 C -0.1732(9) -0.0405(7) 0.8515(4) 0.066(4) Uani 1 d . . . H227 H -0.2217 -0.0727 0.8393 0.079 Uiso 1 calc R . . C228 C -0.1858(9) 0.3672(7) 0.8583(4) 0.069(4) Uani 1 d . . . H22A H -0.1962 0.4211 0.8470 0.082 Uiso 1 calc R . . H22B H -0.1140 0.3521 0.8554 0.082 Uiso 1 calc R . . C229 C -0.2130(11) 0.3717(9) 0.8996(4) 0.088(4) Uani 1 d . . . H22C H -0.1729 0.4145 0.9111 0.132 Uiso 1 calc R . . H22D H -0.1982 0.3193 0.9110 0.132 Uiso 1 calc R . . H22E H -0.2848 0.3842 0.9023 0.132 Uiso 1 calc R . . C230 C -0.3421(9) 0.3366(8) 0.8215(5) 0.077(4) Uani 1 d . . . H23A H -0.3607 0.3894 0.8324 0.093 Uiso 1 calc R . . H23B H -0.3984 0.2984 0.8261 0.093 Uiso 1 calc R . . C231 C -0.3333(13) 0.3481(10) 0.7820(6) 0.108(6) Uani 1 d . . . H23C H -0.3929 0.3769 0.7730 0.163 Uiso 1 calc R . . H23D H -0.3283 0.2950 0.7701 0.163 Uiso 1 calc R . . H23E H -0.2728 0.3802 0.7766 0.163 Uiso 1 calc R . . C241 C -0.0939(8) -0.1679(7) 0.8627(5) 0.066(4) Uani 1 d . . . C242 C -0.0835(9) -0.2026(8) 0.8289(5) 0.073(4) Uani 1 d . . . H242 H -0.0930 -0.1698 0.8082 0.088 Uiso 1 calc R . . C243 C -0.0594(9) -0.2841(8) 0.8247(4) 0.073(4) Uani 1 d . . . H243 H -0.0512 -0.3070 0.8015 0.087 Uiso 1 calc R . . C244 C -0.0471(9) -0.3335(8) 0.8567(5) 0.076(4) Uani 1 d . . . C245 C -0.0152(10) -0.4196(8) 0.8558(6) 0.086(4) Uani 1 d . . . H245 H 0.0007 -0.4437 0.8333 0.103 Uiso 1 calc R . . C246 C -0.0080(11) -0.4652(9) 0.8859(7) 0.097(5) Uani 1 d . . . H246 H 0.0117 -0.5205 0.8836 0.117 Uiso 1 calc R . . C247 C -0.0280(10) -0.4353(9) 0.9195(6) 0.090(5) Uani 1 d . . . H247 H -0.0215 -0.4692 0.9401 0.108 Uiso 1 calc R . . C248 C -0.0587(9) -0.3523(7) 0.9233(5) 0.076(4) Uani 1 d . . . H248 H -0.0736 -0.3308 0.9464 0.091 Uiso 1 calc R . . C249 C -0.0669(8) -0.3010(8) 0.8915(5) 0.069(4) Uani 1 d . . . C250 C -0.0923(8) -0.2141(7) 0.8952(4) 0.061(3) Uani 1 d . . . C251 C -0.0543(9) -0.1237(7) 0.9518(4) 0.067(3) Uani 1 d . . . C252 C -0.0773(11) -0.1018(8) 0.9878(4) 0.075(4) Uani 1 d . . . H252 H -0.0305 -0.0701 1.0010 0.091 Uiso 1 calc R . . C253 C -0.1671(11) -0.1259(8) 1.0042(4) 0.080(4) Uani 1 d . . . H253 H -0.1802 -0.1106 1.0284 0.096 Uiso 1 calc R . . C254 C -0.2390(10) -0.1730(7) 0.9851(5) 0.077(4) Uani 1 d . . . C255 C -0.3376(11) -0.1901(8) 1.0006(5) 0.087(4) Uani 1 d . . . H255 H -0.3543 -0.1715 1.0241 0.104 Uiso 1 calc R . . C256 C -0.4066(12) -0.2341(9) 0.9806(6) 0.101(6) Uani 1 d . . . H256 H -0.4715 -0.2440 0.9904 0.121 Uiso 1 calc R . . C257 C -0.3839(12) -0.2650(9) 0.9460(6) 0.099(5) Uani 1 d . . . H257 H -0.4326 -0.2963 0.9334 0.119 Uiso 1 calc R . . C258 C -0.2879(10) -0.2490(8) 0.9299(5) 0.089(5) Uani 1 d . . . H258 H -0.2729 -0.2700 0.9067 0.107 Uiso 1 calc R . . C259 C -0.2142(10) -0.2013(7) 0.9489(5) 0.071(4) Uani 1 d . . . C260 C -0.1176(8) -0.1788(7) 0.9326(4) 0.065(3) Uani 1 d . . . Ni3 Ni 0.11520(11) 0.12852(8) 0.86140(5) 0.0602(5) Uani 1 d . . . O301 O 0.1190(6) 0.3251(4) 0.8305(2) 0.064(2) Uani 1 d . . . O302 O 0.0561(6) 0.1977(5) 0.8201(2) 0.071(2) Uani 1 d . . . C301 C 0.0594(10) 0.2766(8) 0.8141(4) 0.074(4) Uani 1 d . . . C302 C -0.0110(10) 0.3078(8) 0.7840(4) 0.079(4) Uani 1 d . . . H30A H -0.0782 0.2841 0.7872 0.118 Uiso 1 calc R . . H30B H 0.0161 0.2918 0.7605 0.118 Uiso 1 calc R . . H30C H -0.0156 0.3672 0.7853 0.118 Uiso 1 calc R . . O401 O 0.0929(8) 0.0261(6) 0.8300(3) 0.091(3) Uani 1 d D . . O402 O 0.1184(12) -0.0892(7) 0.7952(4) 0.130(4) Uani 1 d . . . C401 C 0.1061(12) -0.0099(11) 0.8011(5) 0.150(9) Uani 1 d D . . C402 C 0.1216(18) 0.0443(13) 0.7644(5) 0.142(8) Uani 1 d D . . H40A H 0.1445 0.0088 0.7448 0.213 Uiso 1 calc R . . H40B H 0.1722 0.0866 0.7688 0.213 Uiso 1 calc R . . H40C H 0.0575 0.0697 0.7577 0.213 Uiso 1 calc R . . O501 O 0.1247(7) -0.1219(10) 0.8624(4) 0.139(5) Uani 1 d . . . H50A H 0.0902 -0.1511 0.8398 0.167 Uiso 1 d . . . H50B H 0.1345 -0.1717 0.8833 0.167 Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0543(9) 0.0335(7) 0.0939(12) 0.0016(8) 0.0034(8) -0.0026(6) O101 0.054(5) 0.031(4) 0.130(8) -0.001(4) 0.025(5) 0.001(4) O102 0.055(4) 0.036(4) 0.078(6) -0.004(4) 0.008(4) -0.006(3) N101 0.064(6) 0.044(6) 0.078(7) -0.007(5) -0.003(6) 0.003(5) N102 0.050(5) 0.039(5) 0.081(7) -0.003(5) -0.006(6) -0.006(4) N103 0.054(6) 0.038(6) 0.131(10) -0.013(6) 0.005(6) 0.020(5) N104 0.065(7) 0.056(6) 0.088(8) -0.009(5) 0.006(6) -0.003(5) C101 0.056(7) 0.041(7) 0.097(10) -0.008(7) -0.010(7) 0.003(6) C102 0.069(8) 0.053(8) 0.095(11) -0.001(7) 0.007(7) -0.013(7) C103 0.049(7) 0.070(9) 0.081(9) -0.007(7) -0.005(7) 0.004(7) C104 0.052(7) 0.070(9) 0.096(11) -0.009(7) 0.005(7) -0.003(7) C105 0.060(7) 0.047(7) 0.100(10) -0.005(7) 0.002(7) -0.005(6) C106 0.042(6) 0.033(6) 0.088(9) -0.003(6) 0.013(6) -0.014(5) C107 0.049(7) 0.072(9) 0.087(10) 0.006(8) -0.015(7) -0.010(7) C108 0.092(10) 0.066(9) 0.116(12) -0.020(9) 0.008(9) 0.010(9) C109 0.139(16) 0.092(12) 0.19(2) 0.038(13) 0.062(15) 0.057(12) C110 0.077(9) 0.054(8) 0.123(14) 0.005(8) 0.006(9) 0.001(7) C111 0.101(11) 0.082(10) 0.112(15) 0.003(9) 0.008(10) 0.024(9) C121 0.055(7) 0.043(6) 0.075(8) 0.009(6) -0.007(7) 0.001(6) C122 0.054(7) 0.044(6) 0.087(9) -0.004(6) 0.003(7) -0.001(6) C123 0.068(8) 0.053(7) 0.109(11) -0.001(8) 0.006(8) -0.012(7) C124 0.073(9) 0.045(7) 0.100(10) -0.023(7) 0.016(8) 0.008(6) C125 0.072(9) 0.052(7) 0.075(9) -0.008(6) 0.014(7) -0.002(6) C126 0.066(8) 0.046(7) 0.079(9) 0.004(6) 0.001(7) -0.006(6) C127 0.048(7) 0.044(7) 0.088(10) 0.001(6) 0.001(7) 0.007(5) C128 0.087(10) 0.036(7) 0.140(14) -0.011(8) -0.006(9) -0.015(7) C129 0.102(11) 0.053(8) 0.119(12) 0.015(7) 0.000(10) -0.010(7) C130 0.072(8) 0.064(8) 0.095(10) -0.007(8) 0.016(8) -0.013(7) C131 0.071(9) 0.098(11) 0.130(14) -0.040(10) 0.021(9) 0.004(9) C141 0.054(7) 0.054(8) 0.072(9) 0.007(7) 0.006(7) 0.001(6) C142 0.068(8) 0.060(8) 0.093(11) 0.006(7) 0.005(8) -0.010(7) C143 0.052(7) 0.081(10) 0.094(10) 0.010(9) -0.009(7) 0.001(7) C144 0.043(7) 0.047(7) 0.107(11) 0.008(7) -0.004(7) -0.013(6) C145 0.049(8) 0.061(9) 0.152(15) 0.024(10) -0.005(8) 0.004(7) C146 0.076(10) 0.063(10) 0.151(17) 0.033(11) -0.014(11) -0.008(8) C147 0.063(9) 0.045(8) 0.182(18) 0.022(9) -0.028(11) 0.001(7) C148 0.057(8) 0.052(8) 0.117(12) 0.003(8) -0.016(7) -0.001(6) C149 0.052(7) 0.045(8) 0.112(12) 0.012(7) -0.014(8) 0.005(6) C150 0.065(8) 0.036(7) 0.097(10) -0.001(7) 0.006(7) -0.006(6) C151 0.056(8) 0.051(7) 0.087(11) -0.020(7) 0.004(8) -0.006(6) C152 0.077(9) 0.048(7) 0.099(12) -0.012(7) 0.000(8) 0.006(7) C153 0.065(8) 0.057(8) 0.109(12) 0.001(8) -0.017(8) -0.011(7) C154 0.045(7) 0.035(6) 0.109(11) -0.023(7) -0.012(8) 0.004(5) C155 0.044(7) 0.041(7) 0.140(14) -0.011(8) -0.003(8) 0.009(6) C156 0.051(8) 0.059(8) 0.136(15) 0.001(9) -0.011(10) -0.009(6) C157 0.059(8) 0.044(7) 0.136(14) 0.015(7) 0.013(9) -0.003(6) C158 0.054(7) 0.048(7) 0.100(11) 0.007(7) 0.000(7) 0.001(6) C159 0.040(7) 0.030(6) 0.130(13) 0.010(7) -0.007(8) -0.003(5) C160 0.063(8) 0.046(6) 0.091(11) 0.006(7) 0.002(8) 0.008(6) Ni2 0.0566(9) 0.0386(8) 0.1309(16) 0.0163(9) -0.0176(10) -0.0063(7) O201 0.048(4) 0.027(4) 0.117(7) 0.010(4) -0.014(5) -0.005(3) O202 0.051(5) 0.028(3) 0.095(6) 0.001(4) -0.003(4) -0.002(3) N201 0.041(5) 0.036(5) 0.119(9) 0.012(5) -0.002(6) -0.007(4) N202 0.067(7) 0.037(5) 0.088(8) 0.011(5) -0.011(6) -0.012(5) N203 0.053(6) 0.048(6) 0.115(9) 0.002(6) -0.017(6) -0.002(5) N204 0.063(6) 0.051(6) 0.128(10) -0.002(6) -0.012(7) 0.016(5) C201 0.062(8) 0.030(6) 0.092(9) 0.016(6) -0.010(7) -0.003(6) C202 0.054(8) 0.031(6) 0.108(11) 0.000(6) -0.011(7) -0.003(6) C203 0.064(9) 0.040(7) 0.104(11) -0.013(7) -0.008(8) -0.007(6) C204 0.059(8) 0.053(7) 0.106(11) 0.021(7) -0.012(7) -0.006(7) C205 0.072(9) 0.047(7) 0.087(10) -0.006(6) -0.017(7) -0.004(7) C206 0.059(8) 0.045(7) 0.112(11) 0.001(7) -0.010(8) -0.005(6) C207 0.089(11) 0.028(6) 0.120(12) 0.001(6) 0.006(10) 0.008(7) C208 0.066(8) 0.057(8) 0.135(13) 0.021(8) 0.006(8) 0.009(7) C209 0.074(9) 0.074(9) 0.164(16) 0.011(10) 0.023(10) 0.022(8) C210 0.041(6) 0.067(8) 0.118(12) -0.003(8) 0.004(7) 0.006(6) C211 0.109(12) 0.067(9) 0.149(15) 0.018(10) -0.005(11) 0.001(9) C221 0.051(7) 0.049(7) 0.076(8) 0.005(6) 0.005(7) 0.008(6) C222 0.062(8) 0.037(7) 0.102(10) -0.005(6) 0.005(8) 0.007(5) C223 0.057(7) 0.041(7) 0.095(10) 0.000(6) -0.007(7) 0.005(6) C224 0.055(7) 0.065(9) 0.093(11) 0.003(7) -0.006(7) 0.009(6) C225 0.056(8) 0.044(7) 0.098(10) -0.001(6) -0.010(7) -0.008(6) C226 0.044(6) 0.044(7) 0.089(10) 0.012(6) -0.003(6) -0.001(5) C227 0.051(7) 0.036(6) 0.112(11) -0.001(7) 0.005(7) -0.011(6) C228 0.064(7) 0.035(6) 0.106(12) -0.003(7) -0.012(8) 0.009(5) C229 0.084(9) 0.060(8) 0.119(13) -0.006(8) -0.015(9) 0.012(7) C230 0.049(7) 0.052(7) 0.131(15) 0.010(8) -0.005(8) 0.005(6) C231 0.090(11) 0.082(11) 0.153(19) 0.008(11) -0.035(11) 0.003(9) C241 0.050(7) 0.040(7) 0.108(12) 0.013(8) 0.004(7) -0.002(5) C242 0.063(8) 0.055(9) 0.101(12) 0.011(8) 0.007(7) -0.011(6) C243 0.074(8) 0.042(7) 0.102(11) -0.003(7) 0.003(7) 0.004(6) C244 0.056(7) 0.051(8) 0.120(13) -0.012(9) -0.001(9) -0.007(6) C245 0.077(9) 0.039(8) 0.142(15) -0.016(9) -0.006(10) -0.006(6) C246 0.088(10) 0.031(7) 0.174(19) 0.003(12) -0.009(12) 0.005(7) C247 0.063(8) 0.047(9) 0.161(18) 0.017(10) -0.016(10) 0.008(7) C248 0.070(8) 0.038(7) 0.119(12) -0.004(8) -0.006(8) -0.019(6) C249 0.039(6) 0.058(8) 0.111(12) 0.011(9) -0.010(7) -0.006(6) C250 0.042(6) 0.039(6) 0.100(11) -0.003(7) -0.009(6) -0.005(5) C251 0.057(8) 0.047(7) 0.097(11) -0.003(7) 0.015(7) 0.005(7) C252 0.073(9) 0.067(8) 0.087(11) 0.003(7) -0.001(8) -0.003(7) C253 0.084(10) 0.057(8) 0.098(11) 0.022(8) 0.009(9) 0.001(8) C254 0.055(8) 0.045(7) 0.130(14) 0.020(8) 0.004(9) -0.001(7) C255 0.075(9) 0.062(9) 0.124(13) 0.001(8) 0.013(9) -0.010(8) C256 0.076(10) 0.053(8) 0.175(19) 0.020(10) 0.025(12) 0.015(8) C257 0.068(10) 0.054(8) 0.174(18) -0.002(10) 0.003(11) -0.016(7) C258 0.055(8) 0.055(8) 0.157(15) -0.002(9) 0.027(9) 0.000(7) C259 0.058(9) 0.041(7) 0.112(12) 0.020(7) -0.007(8) -0.002(6) C260 0.037(6) 0.049(6) 0.111(11) 0.014(7) -0.002(7) 0.004(6) Ni3 0.0540(8) 0.0340(7) 0.0926(12) -0.0004(8) 0.0044(8) -0.0027(6) O301 0.045(4) 0.043(4) 0.102(6) 0.007(4) -0.016(5) 0.010(4) O302 0.073(5) 0.044(5) 0.096(7) 0.012(4) -0.007(5) -0.003(4) C301 0.060(8) 0.043(8) 0.120(12) -0.004(8) 0.000(8) -0.005(7) C302 0.056(8) 0.077(9) 0.103(11) 0.015(8) -0.012(7) 0.007(7) O401 0.119(8) 0.047(5) 0.107(8) -0.031(5) -0.019(6) 0.017(5) O402 0.171(12) 0.068(7) 0.150(11) -0.021(7) 0.002(10) -0.001(8) C401 0.061(10) 0.092(14) 0.30(3) -0.080(18) 0.004(14) 0.010(9) C402 0.165(19) 0.137(16) 0.124(16) 0.037(13) 0.061(15) -0.004(15) O501 0.068(6) 0.221(14) 0.128(9) -0.074(10) 0.031(7) -0.042(8) _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 O301 1.980(7) . ? Ni1 O102 1.998(7) . ? Ni1 O101 2.002(7) . ? Ni1 N101 2.008(11) . ? Ni1 N102 2.020(9) . ? Ni1 Ni3 2.9703(18) . ? O101 C101 1.297(14) . ? O101 Ni3 2.087(8) . ? O102 C121 1.330(14) . ? O102 Ni3 2.060(7) . ? N101 C107 1.256(16) . ? N101 C141 1.454(16) . ? N102 C127 1.266(15) . ? N102 C151 1.473(15) . ? N103 C103 1.339(16) . ? N103 C108 1.400(17) . ? N103 C110 1.450(17) . ? N104 C123 1.382(16) . ? N104 C130 1.452(16) . ? N104 C128 1.474(16) . ? C101 C102 1.385(18) . ? C101 C106 1.419(17) . ? C102 C103 1.424(18) . ? C103 C104 1.434(18) . ? C104 C105 1.354(18) . ? C105 C106 1.382(17) . ? C106 C107 1.456(17) . ? C108 C109 1.48(2) . ? C110 C111 1.41(2) . ? C121 C122 1.355(16) . ? C121 C126 1.458(16) . ? C122 C123 1.400(18) . ? C123 C124 1.429(18) . ? C124 C125 1.356(17) . ? C125 C126 1.393(17) . ? C126 C127 1.427(17) . ? C128 C129 1.516(18) . ? C130 C131 1.51(2) . ? C141 C150 1.359(18) . ? C141 C142 1.390(18) . ? C142 C143 1.379(19) . ? C143 C144 1.395(19) . ? C144 C149 1.394(18) . ? C144 C145 1.440(18) . ? C145 C146 1.37(2) . ? C146 C147 1.35(2) . ? C147 C148 1.360(18) . ? C148 C149 1.425(19) . ? C149 C150 1.425(17) . ? C150 C160 1.501(19) . ? C151 C160 1.356(18) . ? C151 C152 1.394(19) . ? C152 C153 1.409(18) . ? C153 C154 1.391(19) . ? C154 C159 1.388(18) . ? C154 C155 1.448(17) . ? C155 C156 1.38(2) . ? C156 C157 1.38(2) . ? C157 C158 1.390(18) . ? C158 C159 1.404(18) . ? C159 C160 1.460(17) . ? Ni2 O201 1.989(7) . ? Ni2 N201 1.997(9) . ? Ni2 O202 2.015(6) . ? Ni2 N202 2.068(10) . ? Ni2 O501 2.108(13) . ? Ni2 O401 2.321(12) . ? Ni2 Ni3 2.8789(19) . ? O201 C201 1.308(13) . ? O201 Ni3 2.032(8) . ? O202 C221 1.348(13) . ? O202 Ni3 2.107(7) . ? N201 C227 1.270(15) . ? N201 C241 1.445(15) . ? N202 C207 1.327(18) . ? N202 C251 1.418(16) . ? N203 C203 1.419(16) . ? N203 C210 1.454(18) . ? N203 C208 1.493(16) . ? N204 C223 1.372(15) . ? N204 C230 1.457(17) . ? N204 C228 1.464(16) . ? C201 C202 1.390(16) . ? C201 C206 1.414(18) . ? C202 C203 1.383(17) . ? C203 C204 1.423(18) . ? C204 C205 1.342(17) . ? C205 C206 1.395(18) . ? C206 C207 1.464(19) . ? C208 C209 1.55(2) . ? C210 C211 1.56(2) . ? C221 C222 1.381(15) . ? C221 C226 1.414(16) . ? C222 C223 1.434(17) . ? C223 C224 1.417(17) . ? C224 C225 1.389(17) . ? C225 C226 1.402(16) . ? C226 C227 1.457(16) . ? C228 C229 1.54(2) . ? C230 C231 1.45(2) . ? C241 C242 1.357(19) . ? C241 C250 1.396(19) . ? C242 C243 1.358(18) . ? C243 C244 1.42(2) . ? C244 C249 1.40(2) . ? C244 C245 1.448(19) . ? C245 C246 1.32(2) . ? C246 C247 1.34(2) . ? C247 C248 1.403(19) . ? C248 C249 1.424(19) . ? C249 C250 1.444(18) . ? C250 C260 1.511(19) . ? C251 C252 1.386(19) . ? C251 C260 1.397(18) . ? C252 C253 1.368(19) . ? C253 C254 1.39(2) . ? C254 C255 1.43(2) . ? C254 C259 1.43(2) . ? C255 C256 1.36(2) . ? C256 C257 1.38(2) . ? C257 C258 1.40(2) . ? C258 C259 1.409(19) . ? C259 C260 1.435(18) . ? Ni3 O302 2.022(8) . ? Ni3 O401 2.028(9) . ? O301 C301 1.251(15) . ? O302 C301 1.289(15) . ? C301 C302 1.512(19) . ? O401 C401 1.210(15) . ? O402 C401 1.31(2) . ? C401 C402 1.608(17) . ? 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 O301 Ni1 O102 89.7(3) . . ? O301 Ni1 O101 109.9(4) . . ? O102 Ni1 O101 80.1(3) . . ? O301 Ni1 N101 91.0(4) . . ? O102 Ni1 N101 168.7(4) . . ? O101 Ni1 N101 89.1(4) . . ? O301 Ni1 N102 101.2(3) . . ? O102 Ni1 N102 92.6(4) . . ? O101 Ni1 N102 147.9(4) . . ? N101 Ni1 N102 98.3(4) . . ? O301 Ni1 Ni3 82.9(2) . . ? O102 Ni1 Ni3 43.8(2) . . ? O101 Ni1 Ni3 44.5(2) . . ? N101 Ni1 Ni3 125.2(3) . . ? N102 Ni1 Ni3 136.3(3) . . ? C101 O101 Ni1 130.2(7) . . ? C101 O101 Ni3 134.6(7) . . ? Ni1 O101 Ni3 93.2(3) . . ? C121 O102 Ni1 124.9(6) . . ? C121 O102 Ni3 134.0(7) . . ? Ni1 O102 Ni3 94.1(3) . . ? C107 N101 C141 120.1(11) . . ? C107 N101 Ni1 124.6(9) . . ? C141 N101 Ni1 111.6(8) . . ? C127 N102 C151 116.4(10) . . ? C127 N102 Ni1 121.9(8) . . ? C151 N102 Ni1 121.5(8) . . ? C103 N103 C108 121.4(12) . . ? C103 N103 C110 121.1(10) . . ? C108 N103 C110 116.0(10) . . ? C123 N104 C130 124.6(10) . . ? C123 N104 C128 118.5(11) . . ? C130 N104 C128 116.7(11) . . ? O101 C101 C102 121.1(12) . . ? O101 C101 C106 121.6(10) . . ? C102 C101 C106 117.3(12) . . ? C101 C102 C103 126.1(12) . . ? N103 C103 C102 123.5(12) . . ? N103 C103 C104 123.3(12) . . ? C102 C103 C104 113.1(11) . . ? C105 C104 C103 121.4(12) . . ? C104 C105 C106 124.0(12) . . ? C105 C106 C101 118.1(10) . . ? C105 C106 C107 120.4(11) . . ? C101 C106 C107 121.6(11) . . ? N101 C107 C106 129.5(13) . . ? N103 C108 C109 116.0(14) . . ? C111 C110 N103 114.0(14) . . ? O102 C121 C122 121.0(10) . . ? O102 C121 C126 120.6(10) . . ? C122 C121 C126 118.4(12) . . ? C121 C122 C123 122.9(11) . . ? N104 C123 C122 122.7(11) . . ? N104 C123 C124 118.9(12) . . ? C122 C123 C124 118.4(12) . . ? C125 C124 C123 118.6(12) . . ? C124 C125 C126 123.5(12) . . ? C125 C126 C127 116.8(11) . . ? C125 C126 C121 117.5(11) . . ? C127 C126 C121 125.4(12) . . ? N102 C127 C126 128.7(11) . . ? N104 C128 C129 112.7(12) . . ? N104 C130 C131 114.7(12) . . ? C150 C141 C142 123.4(11) . . ? C150 C141 N101 119.9(12) . . ? C142 C141 N101 116.1(11) . . ? C143 C142 C141 118.3(12) . . ? C142 C143 C144 120.6(13) . . ? C143 C144 C149 120.2(12) . . ? C143 C144 C145 119.5(14) . . ? C149 C144 C145 120.2(13) . . ? C146 C145 C144 116.8(15) . . ? C147 C146 C145 123.8(15) . . ? C146 C147 C148 120.1(16) . . ? C147 C148 C149 120.4(14) . . ? C144 C149 C148 118.4(11) . . ? C144 C149 C150 119.2(12) . . ? C148 C149 C150 122.2(13) . . ? C141 C150 C149 118.2(12) . . ? C141 C150 C160 121.4(11) . . ? C149 C150 C160 120.1(11) . . ? C160 C151 C152 123.5(12) . . ? C160 C151 N102 120.2(12) . . ? C152 C151 N102 116.4(13) . . ? C151 C152 C153 120.0(14) . . ? C154 C153 C152 117.3(13) . . ? C159 C154 C153 123.2(11) . . ? C159 C154 C155 118.8(14) . . ? C153 C154 C155 118.0(13) . . ? C156 C155 C154 120.6(14) . . ? C155 C156 C157 119.3(13) . . ? C156 C157 C158 121.2(14) . . ? C157 C158 C159 120.7(13) . . ? C154 C159 C158 119.3(11) . . ? C154 C159 C160 118.4(13) . . ? C158 C159 C160 122.3(13) . . ? C151 C160 C159 117.4(13) . . ? C151 C160 C150 124.7(12) . . ? C159 C160 C150 117.8(12) . . ? O201 Ni2 N201 169.4(3) . . ? O201 Ni2 O202 78.0(3) . . ? N201 Ni2 O202 91.4(3) . . ? O201 Ni2 N202 90.2(4) . . ? N201 Ni2 N202 95.1(4) . . ? O202 Ni2 N202 121.6(4) . . ? O201 Ni2 O501 94.4(4) . . ? N201 Ni2 O501 94.9(4) . . ? O202 Ni2 O501 148.4(5) . . ? N202 Ni2 O501 88.7(5) . . ? O201 Ni2 O401 76.5(4) . . ? N201 Ni2 O401 101.0(4) . . ? O202 Ni2 O401 73.7(3) . . ? N202 Ni2 O401 157.6(4) . . ? O501 Ni2 O401 74.7(5) . . ? O201 Ni2 Ni3 44.9(2) . . ? N201 Ni2 Ni3 126.8(3) . . ? O202 Ni2 Ni3 47.0(2) . . ? N202 Ni2 Ni3 132.2(3) . . ? O501 Ni2 Ni3 107.0(4) . . ? O401 Ni2 Ni3 44.3(2) . . ? C201 O201 Ni2 125.6(6) . . ? C201 O201 Ni3 139.4(6) . . ? Ni2 O201 Ni3 91.4(3) . . ? C221 O202 Ni2 127.4(6) . . ? C221 O202 Ni3 121.6(7) . . ? Ni2 O202 Ni3 88.6(3) . . ? C227 N201 C241 118.3(11) . . ? C227 N201 Ni2 124.9(7) . . ? C241 N201 Ni2 113.0(7) . . ? C207 N202 C251 116.0(11) . . ? C207 N202 Ni2 119.9(9) . . ? C251 N202 Ni2 123.7(8) . . ? C203 N203 C210 121.8(10) . . ? C203 N203 C208 122.2(10) . . ? C210 N203 C208 113.0(10) . . ? C223 N204 C230 122.0(11) . . ? C223 N204 C228 121.4(10) . . ? C230 N204 C228 116.5(9) . . ? O201 C201 C202 119.1(10) . . ? O201 C201 C206 121.8(10) . . ? C202 C201 C206 119.1(11) . . ? C203 C202 C201 120.4(11) . . ? C202 C203 N203 119.3(11) . . ? C202 C203 C204 120.4(11) . . ? N203 C203 C204 120.1(11) . . ? C205 C204 C203 118.1(12) . . ? C204 C205 C206 123.0(12) . . ? C205 C206 C201 118.6(11) . . ? C205 C206 C207 116.8(12) . . ? C201 C206 C207 124.5(12) . . ? N202 C207 C206 127.1(13) . . ? N203 C208 C209 109.5(13) . . ? N203 C210 C211 114.1(12) . . ? O202 C221 C222 117.5(11) . . ? O202 C221 C226 121.5(9) . . ? C222 C221 C226 120.7(11) . . ? C221 C222 C223 121.2(11) . . ? N204 C223 C224 120.9(11) . . ? N204 C223 C222 120.9(11) . . ? C224 C223 C222 118.2(10) . . ? C225 C224 C223 118.7(12) . . ? C224 C225 C226 123.8(11) . . ? C225 C226 C221 117.0(9) . . ? C225 C226 C227 117.2(11) . . ? C221 C226 C227 125.6(11) . . ? N201 C227 C226 126.7(11) . . ? N204 C228 C229 109.4(11) . . ? N204 C230 C231 116.5(13) . . ? C242 C241 C250 123.0(10) . . ? C242 C241 N201 122.0(13) . . ? C250 C241 N201 114.8(13) . . ? C241 C242 C243 121.5(14) . . ? C242 C243 C244 118.5(14) . . ? C249 C244 C243 120.9(11) . . ? C249 C244 C245 115.5(16) . . ? C243 C244 C245 123.5(16) . . ? C246 C245 C244 122.3(17) . . ? C247 C246 C245 122.8(14) . . ? C246 C247 C248 119.2(16) . . ? C247 C248 C249 119.5(16) . . ? C244 C249 C248 120.5(12) . . ? C244 C249 C250 119.3(13) . . ? C248 C249 C250 120.2(14) . . ? C241 C250 C249 116.2(13) . . ? C241 C250 C260 123.9(10) . . ? C249 C250 C260 119.9(12) . . ? C252 C251 C260 120.4(12) . . ? C252 C251 N202 119.8(12) . . ? C260 C251 N202 119.7(12) . . ? C253 C252 C251 121.5(14) . . ? C252 C253 C254 120.8(15) . . ? C253 C254 C255 120.9(16) . . ? C253 C254 C259 118.8(13) . . ? C255 C254 C259 120.2(14) . . ? C256 C255 C254 118.9(16) . . ? C255 C256 C257 122.4(15) . . ? C256 C257 C258 120.2(15) . . ? C257 C258 C259 120.1(16) . . ? C258 C259 C260 122.1(14) . . ? C258 C259 C254 118.1(12) . . ? C260 C259 C254 119.7(12) . . ? C251 C260 C259 118.0(13) . . ? C251 C260 C250 124.2(11) . . ? C259 C260 C250 117.8(12) . . ? O302 Ni3 O401 88.6(4) . . ? O302 Ni3 O201 167.4(3) . . ? O401 Ni3 O201 82.7(4) . . ? O302 Ni3 O102 94.4(3) . . ? O401 Ni3 O102 175.2(4) . . ? O201 Ni3 O102 95.0(3) . . ? O302 Ni3 O101 88.8(3) . . ? O401 Ni3 O101 99.6(4) . . ? O201 Ni3 O101 101.5(3) . . ? O102 Ni3 O101 76.7(3) . . ? O302 Ni3 O202 94.4(3) . . ? O401 Ni3 O202 78.3(4) . . ? O201 Ni3 O202 75.0(3) . . ? O102 Ni3 O202 105.1(3) . . ? O101 Ni3 O202 176.1(3) . . ? O302 Ni3 Ni2 123.8(2) . . ? O401 Ni3 Ni2 53.1(3) . . ? O201 Ni3 Ni2 43.7(2) . . ? O102 Ni3 Ni2 127.3(2) . . ? O101 Ni3 Ni2 131.7(2) . . ? O202 Ni3 Ni2 44.41(18) . . ? O302 Ni3 Ni1 73.0(2) . . ? O401 Ni3 Ni1 136.0(3) . . ? O201 Ni3 Ni1 119.6(2) . . ? O102 Ni3 Ni1 42.1(2) . . ? O101 Ni3 Ni1 42.3(2) . . ? O202 Ni3 Ni1 140.97(19) . . ? Ni2 Ni3 Ni1 163.19(8) . . ? C301 O301 Ni1 120.4(7) . . ? C301 O302 Ni3 131.0(9) . . ? O301 C301 O302 123.7(13) . . ? O301 C301 C302 120.8(11) . . ? O302 C301 C302 115.4(12) . . ? C401 O401 Ni3 149.0(12) . . ? C401 O401 Ni2 127.9(11) . . ? Ni3 O401 Ni2 82.6(4) . . ? O401 C401 O402 128.9(18) . . ? O401 C401 C402 118.6(16) . . ? O402 C401 C402 112.2(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O501 H50A O402 1.049(11) 1.939(13) 2.50(2) 110.2(9) . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 20.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.034 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.083