Supplementary Material for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Thorsten Glaser' 'Maik Heidemeier' 'Thomas Lugger' _publ_contact_author_name 'Dr Thorsten Glaser' _publ_contact_author_address ; Institut fur Anorganische und Analytische Chemie Universitat Munster Wilhelm-Klemm-Str. 8 Muenster 48149 GERMANY ; _publ_contact_author_email TGLASER@UNI-MUENSTER.DE _publ_section_title ; The novel triplesalen ligand bridges three NiII-salen subunits in a meta-phenylene linkage ; data_sad _database_code_CSD 196942 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49.50 H53 Cl3 N6 Ni3 O6' _chemical_formula_weight 1110.46 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.4321(10) _cell_length_b 12.7252(5) _cell_length_c 30.8525(11) _cell_angle_alpha 90.00 _cell_angle_beta 110.7210(10) _cell_angle_gamma 90.00 _cell_volume 9706.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent plates' _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4600 _exptl_absorpt_coefficient_mu 1.373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8522 _exptl_absorpt_correction_T_max 0.9730 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.759783 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38565 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8551 _reflns_number_gt 6771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+21.2482P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8551 _refine_ls_number_parameters 614 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.205 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.417497(19) -0.05269(4) 0.237075(15) 0.02351(13) Uani 1 1 d . . . C101 C 0.40858(15) -0.2571(3) 0.19767(13) 0.0287(8) Uani 1 1 d . . . C106 C 0.39699(16) -0.3218(3) 0.15825(13) 0.0334(9) Uani 1 1 d . . . H106 H 0.3816 -0.2915 0.1283 0.040 Uiso 1 1 calc R . . C105 C 0.40754(16) -0.4279(3) 0.16232(14) 0.0359(10) Uani 1 1 d . . . H105 H 0.4000 -0.4692 0.1351 0.043 Uiso 1 1 calc R . . C104 C 0.42907(15) -0.4760(3) 0.20545(13) 0.0303(9) Uani 1 1 d . . . H104 H 0.4358 -0.5495 0.2079 0.036 Uiso 1 1 calc R . . C103 C 0.44027(14) -0.4152(3) 0.24427(13) 0.0275(8) Uani 1 1 d . . . H103 H 0.4543 -0.4475 0.2739 0.033 Uiso 1 1 calc R . . C102 C 0.43154(14) -0.3062(3) 0.24143(12) 0.0252(8) Uani 1 1 d . . . C17 C 0.44903(15) -0.2458(3) 0.28339(13) 0.0278(8) Uani 1 1 d . . . H17 H 0.4634 -0.2833 0.3117 0.033 Uiso 1 1 calc R . . C14 C 0.46483(15) -0.0923(3) 0.33237(12) 0.0263(8) Uani 1 1 d . . . C13 C 0.48239(15) 0.0168(3) 0.32268(12) 0.0261(8) Uani 1 1 d . . . H13A H 0.4850 0.0648 0.3486 0.031 Uiso 1 1 calc R . . H13B H 0.5184 0.0128 0.3196 0.031 Uiso 1 1 calc R . . C16 C 0.51269(17) -0.1463(3) 0.36891(13) 0.0352(10) Uani 1 1 d . . . H16A H 0.5007 -0.2126 0.3782 0.053 Uiso 1 1 calc R . . H16B H 0.5272 -0.1004 0.3960 0.053 Uiso 1 1 calc R . . H16C H 0.5409 -0.1604 0.3560 0.053 Uiso 1 1 calc R . . C15 C 0.41571(16) -0.0891(3) 0.34733(13) 0.0325(9) Uani 1 1 d . . . H15A H 0.3855 -0.0551 0.3231 0.049 Uiso 1 1 calc R . . H15B H 0.4246 -0.0492 0.3762 0.049 Uiso 1 1 calc R . . H15C H 0.4054 -0.1609 0.3522 0.049 Uiso 1 1 calc R . . N12 N 0.44686(12) -0.1453(2) 0.28582(10) 0.0247(7) Uani 1 1 d . . . N11 N 0.44205(11) 0.0566(2) 0.27934(9) 0.0214(6) Uani 1 1 d . . . O12 O 0.39810(11) -0.1564(2) 0.19204(8) 0.0324(6) Uani 1 1 d . . . O11 O 0.38796(10) 0.03904(19) 0.18894(8) 0.0268(6) Uani 1 1 d . . . Ni2 Ni 0.223064(18) 0.24082(4) 0.066119(15) 0.02209(12) Uani 1 1 d . . . C301 C 0.43968(15) 0.5222(3) 0.37771(12) 0.0267(8) Uani 1 1 d . . . C306 C 0.49021(17) 0.5042(3) 0.41311(13) 0.0385(10) Uani 1 1 d . . . H306 H 0.5125 0.4485 0.4098 0.046 Uiso 1 1 calc R . . C305 C 0.50764(18) 0.5655(4) 0.45215(14) 0.0439(11) Uani 1 1 d . . . H305 H 0.5416 0.5512 0.4756 0.053 Uiso 1 1 calc R . . C304 C 0.47618(17) 0.6491(3) 0.45804(13) 0.0380(10) Uani 1 1 d . . . H304 H 0.4885 0.6913 0.4852 0.046 Uiso 1 1 calc R . . C303 C 0.42745(16) 0.6686(3) 0.42403(13) 0.0320(9) Uani 1 1 d . . . H303 H 0.4059 0.7250 0.4278 0.038 Uiso 1 1 calc R . . C302 C 0.40846(15) 0.6071(3) 0.38356(12) 0.0269(8) Uani 1 1 d . . . C37 C 0.35797(15) 0.6349(3) 0.34838(12) 0.0260(8) Uani 1 1 d . . . H37 H 0.3378 0.6901 0.3552 0.031 Uiso 1 1 calc R . . C34 C 0.28487(14) 0.6281(3) 0.27445(12) 0.0268(8) Uani 1 1 d . . . C33 C 0.28823(14) 0.6013(3) 0.22740(12) 0.0244(8) Uani 1 1 d . . . H33A H 0.2516 0.6021 0.2034 0.029 Uiso 1 1 calc R . . H33B H 0.3105 0.6544 0.2190 0.029 Uiso 1 1 calc R . . C35 C 0.23991(16) 0.5645(3) 0.28290(14) 0.0370(10) Uani 1 1 d . . . H35A H 0.2459 0.4894 0.2796 0.056 Uiso 1 1 calc R . . H35B H 0.2048 0.5850 0.2602 0.056 Uiso 1 1 calc R . . H35C H 0.2404 0.5784 0.3143 0.056 Uiso 1 1 calc R . . C36 C 0.27603(17) 0.7457(3) 0.27674(13) 0.0360(10) Uani 1 1 d . . . H36A H 0.2723 0.7631 0.3064 0.054 Uiso 1 1 calc R . . H36B H 0.2430 0.7663 0.2513 0.054 Uiso 1 1 calc R . . H36C H 0.3070 0.7836 0.2740 0.054 Uiso 1 1 calc R . . N32 N 0.33781(11) 0.5911(2) 0.30831(10) 0.0232(7) Uani 1 1 d . . . N31 N 0.31259(11) 0.4964(2) 0.22958(9) 0.0199(6) Uani 1 1 d . . . O32 O 0.42383(10) 0.4582(2) 0.34202(8) 0.0281(6) Uani 1 1 d . . . O31 O 0.38610(10) 0.34893(19) 0.27102(8) 0.0247(6) Uani 1 1 d . . . Ni3 Ni 0.364119(18) 0.47374(4) 0.287713(15) 0.02215(12) Uani 1 1 d . . . C201 C 0.13279(14) 0.3757(3) 0.02615(12) 0.0242(8) Uani 1 1 d . . . C206 C 0.10727(15) 0.4733(3) 0.02573(13) 0.0306(9) Uani 1 1 d . . . H206 H 0.1240 0.5234 0.0493 0.037 Uiso 1 1 calc R . . C205 C 0.05868(16) 0.4968(3) -0.00823(13) 0.0329(9) Uani 1 1 d . . . H205 H 0.0424 0.5633 -0.0080 0.040 Uiso 1 1 calc R . . C204 C 0.03258(15) 0.4244(3) -0.04335(13) 0.0329(9) Uani 1 1 d . . . H204 H -0.0015 0.4409 -0.0662 0.039 Uiso 1 1 calc R . . C203 C 0.05652(15) 0.3307(3) -0.04422(12) 0.0304(9) Uani 1 1 d . . . H203 H 0.0390 0.2818 -0.0681 0.036 Uiso 1 1 calc R . . C202 C 0.10724(15) 0.3039(3) -0.01034(12) 0.0257(8) Uani 1 1 d . . . C27 C 0.13075(14) 0.2047(3) -0.01322(12) 0.0255(8) Uani 1 1 d . . . H27 H 0.1110 0.1593 -0.0378 0.031 Uiso 1 1 calc R . . C23 C 0.25714(15) 0.0716(3) 0.02880(12) 0.0269(8) Uani 1 1 d . . . H23A H 0.2736 0.0008 0.0354 0.032 Uiso 1 1 calc R . . H23B H 0.2697 0.1063 0.0057 0.032 Uiso 1 1 calc R . . C24 C 0.19541(15) 0.0633(3) 0.01020(12) 0.0253(8) Uani 1 1 d . . . C26 C 0.17641(17) 0.0235(3) -0.03964(13) 0.0362(10) Uani 1 1 d . . . H26A H 0.1378 0.0066 -0.0500 0.054 Uiso 1 1 calc R . . H26B H 0.1968 -0.0398 -0.0413 0.054 Uiso 1 1 calc R . . H26C H 0.1824 0.0779 -0.0597 0.054 Uiso 1 1 calc R . . C25 C 0.17638(16) -0.0087(3) 0.04091(13) 0.0328(9) Uani 1 1 d . . . H25A H 0.1918 0.0151 0.0731 0.049 Uiso 1 1 calc R . . H25B H 0.1883 -0.0808 0.0386 0.049 Uiso 1 1 calc R . . H25C H 0.1368 -0.0068 0.0307 0.049 Uiso 1 1 calc R . . N22 N 0.17670(11) 0.1715(2) 0.01493(9) 0.0230(6) Uani 1 1 d . . . N21 N 0.27279(11) 0.1345(2) 0.07176(9) 0.0210(6) Uani 1 1 d . . . O22 O 0.17783(10) 0.3553(2) 0.06017(8) 0.0283(6) Uani 1 1 d . . . O21 O 0.26742(10) 0.3083(2) 0.11723(9) 0.0326(6) Uani 1 1 d . . . C1 C 0.37365(14) 0.1357(3) 0.19005(11) 0.0206(7) Uani 1 1 d . . . C2 C 0.39326(13) 0.1986(3) 0.23056(11) 0.0206(7) Uani 1 1 d . . . C3 C 0.36994(13) 0.3003(3) 0.23155(11) 0.0200(7) Uani 1 1 d . . . C4 C 0.32966(13) 0.3417(3) 0.19133(11) 0.0200(7) Uani 1 1 d . . . C5 C 0.30986(13) 0.2761(3) 0.15068(11) 0.0216(7) Uani 1 1 d . . . C6 C 0.33478(13) 0.1783(3) 0.14827(11) 0.0196(7) Uani 1 1 d . . . C11 C 0.43559(13) 0.1570(3) 0.27180(11) 0.0212(7) Uani 1 1 d . . . C12 C 0.47538(14) 0.2312(3) 0.30522(12) 0.0263(8) Uani 1 1 d . . . H12A H 0.4664 0.2384 0.3333 0.039 Uiso 1 1 calc R . . H12B H 0.4734 0.3001 0.2906 0.039 Uiso 1 1 calc R . . H12C H 0.5121 0.2030 0.3134 0.039 Uiso 1 1 calc R . . C31 C 0.30605(14) 0.4453(3) 0.19114(11) 0.0212(7) Uani 1 1 d . . . C32 C 0.27609(15) 0.5009(3) 0.14602(12) 0.0275(8) Uani 1 1 d . . . H32A H 0.2373 0.4869 0.1369 0.041 Uiso 1 1 calc R . . H32B H 0.2890 0.4752 0.1219 0.041 Uiso 1 1 calc R . . H32C H 0.2825 0.5768 0.1500 0.041 Uiso 1 1 calc R . . C21 C 0.31926(14) 0.1190(3) 0.10542(12) 0.0219(8) Uani 1 1 d . . . C22 C 0.35859(15) 0.0421(3) 0.09743(12) 0.0288(9) Uani 1 1 d . . . H22A H 0.3500 -0.0291 0.1048 0.043 Uiso 1 1 calc R . . H22B H 0.3955 0.0603 0.1174 0.043 Uiso 1 1 calc R . . H22C H 0.3557 0.0451 0.0649 0.043 Uiso 1 1 calc R . . C400 C 0.13110(18) 0.7748(3) 0.12852(14) 0.0402(10) Uani 1 1 d . . . H400 H 0.1124 0.8176 0.1455 0.048 Uiso 1 1 calc R . . Cl42 Cl 0.19646(5) 0.82461(11) 0.14122(4) 0.0578(3) Uani 1 1 d . . . Cl41 Cl 0.13411(5) 0.64437(9) 0.14725(5) 0.0540(3) Uani 1 1 d . . . Cl43 Cl 0.09364(6) 0.78241(12) 0.06889(4) 0.0637(4) Uani 1 1 d . . . C80 C 0.2837(5) 0.7697(9) 0.0396(4) 0.053(3) Uiso 0.50 1 d P . . C81 C 0.2127(4) 0.6880(8) 0.0438(4) 0.051(2) Uiso 0.50 1 d P . . C82 C 0.3004(7) 0.8014(13) -0.0053(7) 0.099(5) Uiso 0.50 1 d P . . C83 C 0.2707(6) 0.7444(11) 0.0614(5) 0.080(4) Uiso 0.50 1 d P . . C85 C 0.2376(8) 0.7307(13) 0.0249(6) 0.096(4) Uiso 0.50 1 d P . . C86 C 0.3470(8) 0.8004(15) 0.0333(7) 0.129(6) Uiso 0.50 1 d P . . C87 C 0.2969(6) 0.7770(10) 0.0230(5) 0.065(3) Uiso 0.50 1 d P . . 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 0.0278(3) 0.0224(3) 0.0167(2) 0.00022(19) 0.00333(19) 0.00304(19) C101 0.027(2) 0.028(2) 0.028(2) -0.0021(16) 0.0051(16) -0.0031(16) C106 0.038(2) 0.029(2) 0.026(2) -0.0028(17) 0.0032(17) -0.0027(18) C105 0.038(2) 0.034(2) 0.030(2) -0.0098(18) 0.0047(18) -0.0104(19) C104 0.028(2) 0.021(2) 0.042(2) -0.0022(17) 0.0129(18) -0.0039(16) C103 0.0191(18) 0.028(2) 0.035(2) 0.0057(17) 0.0085(16) -0.0023(15) C102 0.0212(18) 0.028(2) 0.0265(19) 0.0007(16) 0.0088(15) -0.0003(15) C17 0.026(2) 0.031(2) 0.0256(19) 0.0050(16) 0.0089(16) 0.0049(16) C14 0.033(2) 0.026(2) 0.0170(17) 0.0027(15) 0.0046(16) 0.0055(16) C13 0.0256(19) 0.031(2) 0.0161(17) 0.0002(15) 0.0006(15) 0.0048(16) C16 0.045(2) 0.033(2) 0.0199(19) -0.0002(17) 0.0018(18) 0.0074(19) C15 0.042(2) 0.030(2) 0.026(2) -0.0004(17) 0.0134(18) 0.0004(18) N12 0.0277(16) 0.0235(17) 0.0200(15) 0.0018(13) 0.0048(13) 0.0034(13) N11 0.0221(15) 0.0244(16) 0.0155(14) 0.0005(12) 0.0037(12) 0.0024(12) O12 0.0437(16) 0.0249(15) 0.0208(13) -0.0002(11) 0.0017(12) 0.0021(12) O11 0.0350(15) 0.0246(14) 0.0176(12) -0.0002(10) 0.0054(11) 0.0052(11) Ni2 0.0221(2) 0.0215(2) 0.0172(2) -0.00279(18) 0.00017(18) 0.00184(19) C301 0.031(2) 0.028(2) 0.0195(18) 0.0001(16) 0.0058(16) -0.0021(16) C306 0.035(2) 0.042(3) 0.029(2) -0.0049(19) 0.0006(18) 0.0067(19) C305 0.039(2) 0.052(3) 0.028(2) -0.006(2) -0.0046(19) -0.001(2) C304 0.045(3) 0.039(2) 0.021(2) -0.0066(18) 0.0015(18) -0.003(2) C303 0.040(2) 0.031(2) 0.0245(19) -0.0030(17) 0.0106(17) 0.0013(18) C302 0.033(2) 0.028(2) 0.0179(18) 0.0006(15) 0.0069(16) -0.0017(16) C37 0.030(2) 0.025(2) 0.0253(19) -0.0022(16) 0.0129(16) 0.0021(16) C34 0.0229(19) 0.031(2) 0.0246(19) -0.0015(16) 0.0055(15) 0.0082(16) C33 0.0222(18) 0.026(2) 0.0216(18) -0.0012(15) 0.0030(15) 0.0036(15) C35 0.027(2) 0.047(3) 0.039(2) 0.000(2) 0.0136(18) 0.0070(19) C36 0.039(2) 0.038(2) 0.027(2) -0.0047(18) 0.0057(18) 0.0146(19) N32 0.0226(16) 0.0256(16) 0.0202(15) -0.0006(13) 0.0061(13) 0.0039(13) N31 0.0155(14) 0.0232(16) 0.0179(14) -0.0015(12) 0.0020(12) 0.0028(12) O32 0.0276(14) 0.0299(15) 0.0193(12) -0.0041(11) -0.0008(11) 0.0072(11) O31 0.0284(13) 0.0236(13) 0.0167(12) -0.0039(10) 0.0011(10) 0.0042(11) Ni3 0.0217(2) 0.0242(3) 0.0174(2) -0.00261(19) 0.00310(19) 0.00260(19) C201 0.0246(19) 0.027(2) 0.0204(18) 0.0035(15) 0.0077(15) 0.0001(15) C206 0.030(2) 0.032(2) 0.026(2) 0.0000(17) 0.0063(17) 0.0020(17) C205 0.031(2) 0.035(2) 0.032(2) 0.0061(18) 0.0098(18) 0.0095(17) C204 0.026(2) 0.043(2) 0.025(2) 0.0106(18) 0.0040(17) 0.0059(18) C203 0.026(2) 0.040(2) 0.0205(18) 0.0003(17) 0.0025(16) -0.0017(18) C202 0.027(2) 0.029(2) 0.0190(18) 0.0045(15) 0.0052(15) -0.0009(16) C27 0.0253(19) 0.031(2) 0.0165(17) -0.0025(15) 0.0023(15) -0.0042(16) C23 0.030(2) 0.028(2) 0.0215(18) -0.0046(16) 0.0069(16) 0.0028(16) C24 0.027(2) 0.0245(19) 0.0204(18) -0.0042(15) 0.0040(15) 0.0009(15) C26 0.039(2) 0.036(2) 0.028(2) -0.0105(18) 0.0051(18) 0.0034(19) C25 0.035(2) 0.026(2) 0.033(2) 0.0008(17) 0.0062(18) -0.0040(17) N22 0.0234(16) 0.0256(16) 0.0177(14) -0.0016(13) 0.0042(13) -0.0024(13) N21 0.0245(16) 0.0201(15) 0.0165(14) -0.0031(12) 0.0048(12) 0.0002(12) O22 0.0265(14) 0.0256(14) 0.0245(13) -0.0053(11) -0.0011(11) 0.0050(11) O21 0.0291(14) 0.0278(15) 0.0274(14) -0.0089(11) -0.0067(11) 0.0073(11) C1 0.0214(18) 0.0219(19) 0.0195(17) 0.0012(14) 0.0084(14) 0.0012(15) C2 0.0187(17) 0.0255(19) 0.0176(17) 0.0020(14) 0.0063(14) -0.0020(15) C3 0.0194(18) 0.0216(18) 0.0199(18) -0.0021(14) 0.0081(14) -0.0037(14) C4 0.0181(17) 0.0221(18) 0.0183(17) 0.0002(14) 0.0047(14) 0.0008(14) C5 0.0178(17) 0.0238(19) 0.0196(17) 0.0026(15) 0.0023(14) -0.0007(14) C6 0.0205(17) 0.0210(18) 0.0154(16) -0.0016(14) 0.0039(14) -0.0014(14) C11 0.0185(17) 0.027(2) 0.0199(17) -0.0017(15) 0.0089(14) -0.0016(15) C12 0.0209(18) 0.027(2) 0.0261(19) -0.0024(16) 0.0023(15) -0.0006(15) C31 0.0194(17) 0.0247(19) 0.0180(17) -0.0028(15) 0.0048(14) -0.0034(14) C32 0.031(2) 0.026(2) 0.0212(18) 0.0002(16) 0.0042(16) 0.0041(16) C21 0.0256(19) 0.0187(18) 0.0208(18) 0.0037(14) 0.0074(15) 0.0000(15) C22 0.032(2) 0.034(2) 0.0174(17) -0.0014(16) 0.0052(16) 0.0033(17) C400 0.049(3) 0.032(2) 0.036(2) 0.0013(19) 0.011(2) 0.001(2) Cl42 0.0601(8) 0.0640(8) 0.0409(6) 0.0077(6) 0.0077(6) -0.0211(6) Cl41 0.0620(8) 0.0377(6) 0.0659(8) 0.0129(6) 0.0270(6) 0.0012(6) Cl43 0.0602(8) 0.0735(9) 0.0415(7) 0.0086(6) -0.0014(6) -0.0062(7) _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 O11 1.832(2) . ? Ni1 N12 1.851(3) . ? Ni1 O12 1.852(3) . ? Ni1 N11 1.859(3) . ? C101 O12 1.310(4) . ? C101 C106 1.410(5) . ? C101 C102 1.415(5) . ? C106 C105 1.375(6) . ? C106 H106 0.9500 . ? C105 C104 1.391(5) . ? C105 H105 0.9500 . ? C104 C103 1.368(5) . ? C104 H104 0.9500 . ? C103 C102 1.404(5) . ? C103 H103 0.9500 . ? C102 C17 1.434(5) . ? C17 N12 1.284(5) . ? C17 H17 0.9500 . ? C14 N12 1.504(4) . ? C14 C15 1.525(5) . ? C14 C13 1.526(5) . ? C14 C16 1.528(5) . ? C13 N11 1.474(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N11 C11 1.299(4) . ? O11 C1 1.291(4) . ? Ni2 O21 1.814(2) . ? Ni2 N22 1.845(3) . ? Ni2 N21 1.851(3) . ? Ni2 O22 1.852(2) . ? C301 O32 1.314(4) . ? C301 C302 1.409(5) . ? C301 C306 1.413(5) . ? C306 C305 1.371(6) . ? C306 H306 0.9500 . ? C305 C304 1.400(6) . ? C305 H305 0.9500 . ? C304 C303 1.366(5) . ? C304 H304 0.9500 . ? C303 C302 1.407(5) . ? C303 H303 0.9500 . ? C302 C37 1.435(5) . ? C37 N32 1.287(4) . ? C37 H37 0.9500 . ? C34 N32 1.495(4) . ? C34 C36 1.520(5) . ? C34 C33 1.524(5) . ? C34 C35 1.535(5) . ? C33 N31 1.474(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? N32 Ni3 1.852(3) . ? N31 C31 1.309(4) . ? N31 Ni3 1.851(3) . ? O32 Ni3 1.862(2) . ? O31 C3 1.296(4) . ? O31 Ni3 1.827(2) . ? C201 O22 1.305(4) . ? C201 C206 1.411(5) . ? C201 C202 1.421(5) . ? C206 C205 1.373(5) . ? C206 H206 0.9500 . ? C205 C204 1.403(6) . ? C205 H205 0.9500 . ? C204 C203 1.355(6) . ? C204 H204 0.9500 . ? C203 C202 1.419(5) . ? C203 H203 0.9500 . ? C202 C27 1.424(5) . ? C27 N22 1.289(4) . ? C27 H27 0.9500 . ? C23 N21 1.477(4) . ? C23 C24 1.530(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N22 1.488(5) . ? C24 C26 1.526(5) . ? C24 C25 1.526(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? N21 C21 1.313(4) . ? O21 C5 1.293(4) . ? C1 C2 1.419(5) . ? C1 C6 1.440(5) . ? C2 C3 1.438(5) . ? C2 C11 1.464(5) . ? C3 C4 1.420(5) . ? C4 C5 1.442(5) . ? C4 C31 1.458(5) . ? C5 C6 1.422(5) . ? C6 C21 1.450(5) . ? C11 C12 1.514(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C31 C32 1.512(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C21 C22 1.510(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C400 Cl42 1.750(5) . ? C400 Cl41 1.750(4) . ? C400 Cl43 1.756(4) . ? C400 H400 1.0000 . ? C80 C87 0.719(15) . ? C80 C83 0.917(15) . ? C80 C85 1.24(2) . ? C80 C82 1.65(2) . ? C80 C86 1.79(2) . ? C80 C85 1.866(19) 7_565 ? C81 C85 1.157(18) . ? C81 C82 1.12(2) 7_565 ? C81 C83 1.603(18) . ? C82 C87 0.963(18) . ? C82 C85 1.05(2) 7_565 ? C82 C81 1.12(2) 7_565 ? C82 C86 1.38(2) . ? C83 C85 1.17(2) . ? C83 C87 1.62(2) . ? C85 C82 1.05(2) 7_565 ? C85 C87 1.44(2) 7_565 ? C85 C87 1.70(2) . ? C85 C80 1.866(19) 7_565 ? C85 C85 1.94(3) 7_565 ? C86 C87 1.28(2) . ? C87 C85 1.44(2) 7_565 ? 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 O11 Ni1 N12 179.56(13) . . ? O11 Ni1 O12 85.43(11) . . ? N12 Ni1 O12 94.65(12) . . ? O11 Ni1 N11 92.00(11) . . ? N12 Ni1 N11 87.96(13) . . ? O12 Ni1 N11 173.89(13) . . ? O12 C101 C106 119.1(3) . . ? O12 C101 C102 123.9(3) . . ? C106 C101 C102 117.0(3) . . ? C105 C106 C101 121.3(4) . . ? C105 C106 H106 119.4 . . ? C101 C106 H106 119.4 . . ? C106 C105 C104 121.4(4) . . ? C106 C105 H105 119.3 . . ? C104 C105 H105 119.3 . . ? C103 C104 C105 118.5(4) . . ? C103 C104 H104 120.8 . . ? C105 C104 H104 120.8 . . ? C104 C103 C102 121.7(4) . . ? C104 C103 H103 119.2 . . ? C102 C103 H103 119.2 . . ? C103 C102 C101 120.1(3) . . ? C103 C102 C17 118.7(3) . . ? C101 C102 C17 121.2(3) . . ? N12 C17 C102 125.4(3) . . ? N12 C17 H17 117.3 . . ? C102 C17 H17 117.3 . . ? N12 C14 C15 106.6(3) . . ? N12 C14 C13 103.7(3) . . ? C15 C14 C13 112.7(3) . . ? N12 C14 C16 113.7(3) . . ? C15 C14 C16 111.1(3) . . ? C13 C14 C16 108.9(3) . . ? N11 C13 C14 108.5(3) . . ? N11 C13 H13A 110.0 . . ? C14 C13 H13A 110.0 . . ? N11 C13 H13B 110.0 . . ? C14 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 N12 C14 119.8(3) . . ? C17 N12 Ni1 127.0(3) . . ? C14 N12 Ni1 113.0(2) . . ? C11 N11 C13 120.5(3) . . ? C11 N11 Ni1 128.2(2) . . ? C13 N11 Ni1 109.9(2) . . ? C101 O12 Ni1 127.5(2) . . ? C1 O11 Ni1 129.1(2) . . ? O21 Ni2 N22 178.50(13) . . ? O21 Ni2 N21 92.60(11) . . ? N22 Ni2 N21 88.04(12) . . ? O21 Ni2 O22 84.82(11) . . ? N22 Ni2 O22 94.64(12) . . ? N21 Ni2 O22 175.03(12) . . ? O32 C301 C302 123.7(3) . . ? O32 C301 C306 118.8(3) . . ? C302 C301 C306 117.5(3) . . ? C305 C306 C301 121.2(4) . . ? C305 C306 H306 119.4 . . ? C301 C306 H306 119.4 . . ? C306 C305 C304 121.0(4) . . ? C306 C305 H305 119.5 . . ? C304 C305 H305 119.5 . . ? C303 C304 C305 118.7(4) . . ? C303 C304 H304 120.6 . . ? C305 C304 H304 120.7 . . ? C304 C303 C302 121.6(4) . . ? C304 C303 H303 119.2 . . ? C302 C303 H303 119.2 . . ? C303 C302 C301 119.9(3) . . ? C303 C302 C37 118.6(3) . . ? C301 C302 C37 121.5(3) . . ? N32 C37 C302 125.3(3) . . ? N32 C37 H37 117.3 . . ? C302 C37 H37 117.3 . . ? N32 C34 C36 113.5(3) . . ? N32 C34 C33 103.9(3) . . ? C36 C34 C33 109.0(3) . . ? N32 C34 C35 107.7(3) . . ? C36 C34 C35 111.8(3) . . ? C33 C34 C35 110.7(3) . . ? N31 C33 C34 109.3(3) . . ? N31 C33 H33A 109.8 . . ? C34 C33 H33A 109.8 . . ? N31 C33 H33B 109.8 . . ? C34 C33 H33B 109.8 . . ? H33A C33 H33B 108.3 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C37 N32 C34 120.1(3) . . ? C37 N32 Ni3 126.9(3) . . ? C34 N32 Ni3 112.7(2) . . ? C31 N31 C33 119.5(3) . . ? C31 N31 Ni3 128.1(2) . . ? C33 N31 Ni3 110.2(2) . . ? C301 O32 Ni3 127.3(2) . . ? C3 O31 Ni3 130.4(2) . . ? O31 Ni3 N31 93.48(11) . . ? O31 Ni3 N32 173.34(12) . . ? N31 Ni3 N32 88.28(12) . . ? O31 Ni3 O32 84.74(10) . . ? N31 Ni3 O32 170.91(12) . . ? N32 Ni3 O32 94.51(12) . . ? O22 C201 C206 118.7(3) . . ? O22 C201 C202 123.5(3) . . ? C206 C201 C202 117.8(3) . . ? C205 C206 C201 120.9(4) . . ? C205 C206 H206 119.5 . . ? C201 C206 H206 119.5 . . ? C206 C205 C204 121.2(4) . . ? C206 C205 H205 119.4 . . ? C204 C205 H205 119.4 . . ? C203 C204 C205 119.2(3) . . ? C203 C204 H204 120.4 . . ? C205 C204 H204 120.4 . . ? C204 C203 C202 121.5(4) . . ? C204 C203 H203 119.2 . . ? C202 C203 H203 119.2 . . ? C203 C202 C201 119.3(3) . . ? C203 C202 C27 119.1(3) . . ? C201 C202 C27 121.6(3) . . ? N22 C27 C202 125.2(3) . . ? N22 C27 H27 117.4 . . ? C202 C27 H27 117.4 . . ? N21 C23 C24 107.3(3) . . ? N21 C23 H23A 110.3 . . ? C24 C23 H23A 110.3 . . ? N21 C23 H23B 110.3 . . ? C24 C23 H23B 110.3 . . ? H23A C23 H23B 108.5 . . ? N22 C24 C26 113.8(3) . . ? N22 C24 C25 107.5(3) . . ? C26 C24 C25 111.3(3) . . ? N22 C24 C23 104.3(3) . . ? C26 C24 C23 109.2(3) . . ? C25 C24 C23 110.6(3) . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 N22 C24 120.2(3) . . ? C27 N22 Ni2 127.1(3) . . ? C24 N22 Ni2 112.5(2) . . ? C21 N21 C23 121.0(3) . . ? C21 N21 Ni2 128.2(2) . . ? C23 N21 Ni2 110.3(2) . . ? C201 O22 Ni2 127.6(2) . . ? C5 O21 Ni2 130.9(2) . . ? O11 C1 C2 122.8(3) . . ? O11 C1 C6 117.3(3) . . ? C2 C1 C6 119.9(3) . . ? C1 C2 C3 120.1(3) . . ? C1 C2 C11 119.3(3) . . ? C3 C2 C11 120.6(3) . . ? O31 C3 C4 122.7(3) . . ? O31 C3 C2 116.6(3) . . ? C4 C3 C2 120.6(3) . . ? C3 C4 C5 118.4(3) . . ? C3 C4 C31 121.8(3) . . ? C5 C4 C31 119.8(3) . . ? O21 C5 C6 121.5(3) . . ? O21 C5 C4 117.2(3) . . ? C6 C5 C4 121.3(3) . . ? C5 C6 C1 118.7(3) . . ? C5 C6 C21 121.1(3) . . ? C1 C6 C21 120.1(3) . . ? N11 C11 C2 121.5(3) . . ? N11 C11 C12 118.4(3) . . ? C2 C11 C12 119.9(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N31 C31 C4 121.7(3) . . ? N31 C31 C32 117.4(3) . . ? C4 C31 C32 120.7(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N21 C21 C6 121.8(3) . . ? N21 C21 C22 118.3(3) . . ? C6 C21 C22 119.8(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Cl42 C400 Cl41 110.1(2) . . ? Cl42 C400 Cl43 111.1(2) . . ? Cl41 C400 Cl43 110.0(2) . . ? Cl42 C400 H400 108.5 . . ? Cl41 C400 H400 108.5 . . ? Cl43 C400 H400 108.5 . . ? C87 C80 C83 166(2) . . ? C87 C80 C85 117(2) . . ? C83 C80 C85 63.4(14) . . ? C87 C80 C82 13.8(15) . . ? C83 C80 C82 170.7(16) . . ? C85 C80 C82 108.2(12) . . ? C87 C80 C86 35.9(15) . . ? C83 C80 C86 139.7(16) . . ? C85 C80 C86 151.6(15) . . ? C82 C80 C86 47.0(10) . . ? C87 C80 C85 44.2(15) . 7_565 ? C83 C80 C85 137.0(16) . 7_565 ? C85 C80 C85 74.0(12) . 7_565 ? C82 C80 C85 34.2(7) . 7_565 ? C86 C80 C85 80.1(11) . 7_565 ? C85 C81 C82 55.1(12) . 7_565 ? C85 C81 C83 46.7(11) . . ? C82 C81 C83 101.9(13) 7_565 . ? C87 C82 C85 91(2) . 7_565 ? C87 C82 C81 155(2) . 7_565 ? C85 C82 C81 64.2(15) 7_565 7_565 ? C87 C82 C86 63.5(16) . . ? C85 C82 C86 151(2) 7_565 . ? C81 C82 C86 140(2) 7_565 . ? C87 C82 C80 10.3(11) . . ? C85 C82 C80 84.4(15) 7_565 . ? C81 C82 C80 147.9(17) 7_565 . ? C86 C82 C80 72.1(14) . . ? C80 C83 C85 72.1(15) . . ? C80 C83 C87 6.2(11) . . ? C85 C83 C87 72.7(12) . . ? C80 C83 C81 118.1(15) . . ? C85 C83 C81 46.1(10) . . ? C87 C83 C81 118.1(11) . . ? C82 C85 C81 60.7(16) 7_565 . ? C82 C85 C83 148(2) 7_565 . ? C81 C85 C83 87.1(15) . . ? C82 C85 C80 167(2) 7_565 . ? C81 C85 C80 131.6(18) . . ? C83 C85 C80 44.5(10) . . ? C82 C85 C87 41.9(12) 7_565 7_565 ? C81 C85 C87 102.6(17) . 7_565 ? C83 C85 C87 170.3(19) . 7_565 ? C80 C85 C87 125.7(15) . 7_565 ? C82 C85 C87 145.1(18) 7_565 . ? C81 C85 C87 151.4(17) . . ? C83 C85 C87 66.1(13) . . ? C80 C85 C87 22.2(8) . . ? C87 C85 C87 104.3(12) 7_565 . ? C82 C85 C80 61.4(14) 7_565 7_565 ? C81 C85 C80 121.6(16) . 7_565 ? C83 C85 C80 150.3(16) . 7_565 ? C80 C85 C80 106.0(12) . 7_565 ? C87 C85 C80 20.4(7) 7_565 7_565 ? C87 C85 C80 84.2(9) . 7_565 ? C82 C85 C85 99.5(18) 7_565 7_565 ? C81 C85 C85 159(2) . 7_565 ? C83 C85 C85 112.3(18) . 7_565 ? C80 C85 C85 67.9(12) . 7_565 ? C87 C85 C85 58.1(10) 7_565 7_565 ? C87 C85 C85 46.1(9) . 7_565 ? C80 C85 C85 38.2(7) 7_565 7_565 ? C87 C86 C82 42.2(10) . . ? C87 C86 C80 19.2(9) . . ? C82 C86 C80 60.9(12) . . ? C80 C87 C82 156(3) . . ? C80 C87 C86 125(2) . . ? C82 C87 C86 74.3(18) . . ? C80 C87 C85 115(2) . 7_565 ? C82 C87 C85 47.0(13) . 7_565 ? C86 C87 C85 119.6(18) . 7_565 ? C80 C87 C83 7.9(14) . . ? C82 C87 C83 161.3(18) . . ? C86 C87 C83 123.3(15) . . ? C85 C87 C83 116.9(13) 7_565 . ? C80 C87 C85 40.9(14) . . ? C82 C87 C85 122.0(17) . . ? C86 C87 C85 163.4(17) . . ? C85 C87 C85 75.7(12) 7_565 . ? C83 C87 C85 41.2(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.400 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.082