# This journal is © Deutsche Bunsen-Gesellschaft für Physikalische Chemie, # Kemisk Forening, Koninklijke Nederlandse Chemische Vereniging, Norsk Kjemisk Selskap, # Real Sociedad Espanola de Quimica, The Royal Society of Chemistry, Società Chimica # Italiana 2000, Suomen Kemian Seura-Kemiska Sallskopet i Finland and # Svenska Kemistsamfundet # CCDC Number: 1326/10 data_trien _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Ni 2+), C20 H26 N6, H2 O, (Cl O4 1-)2' _chemical_formula_sum 'C20 H28 Cl2 N6 Ni O9' _chemical_formula_weight 626.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorombic' _symmetry_space_group_name_H-M 'P B C A' 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' '-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 15.043(4) _cell_length_b 15.370(3) _cell_length_c 21.872(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5057(2) _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 23 _exptl_crystal_description prismatic _exptl_crystal_colour blue _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 3.612 _exptl_absorpt_correction_type 'empiric(psi-scan)' _exptl_absorpt_correction_T_min 0.1830 _exptl_absorpt_correction_T_max 0.3758 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\q/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3839 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 59.99 _reflns_number_total 3083 _reflns_number_gt 2952 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P4' _computing_cell_refinement 'Siemens P4' _computing_data_reduction 'Siemens P4' _computing_structure_solution 'Sir97(Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3(L.J.Farrugia, 1997)' _computing_publication_material 'Parst97( Nardelli, 1997)' _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^)+(0.1167P)^2^+13.7184P] 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 ? _refine_ls_number_reflns 3083 _refine_ls_number_parameters 383 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1936 _refine_ls_wR_factor_gt 0.1902 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.093 _refine_ls_shift/su_mean 0.005 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 Ni Ni 0.46125(6) 0.23642(5) 0.62632(4) 0.0385(3) Uani 1 1 d . . . O1 O 0.5937(3) 0.2402(4) 0.6004(3) 0.0582(12) Uani 1 1 d D . . N1 N 0.4511(3) 0.3803(3) 0.5932(2) 0.0440(11) Uani 1 1 d . . . C1 C 0.4775(4) 0.4565(4) 0.6156(3) 0.0596(17) Uani 1 1 d . . . C2 C 0.5417(6) 0.4603(5) 0.6668(4) 0.082(2) Uani 1 1 d . . . H2A H 0.5728 0.5155 0.6649 0.099 Uiso 1 1 calc R . . H2B H 0.5088 0.4590 0.7049 0.099 Uiso 1 1 calc R . . N6 N 0.6072(4) 0.3911(4) 0.6681(3) 0.0676(16) Uani 1 1 d . . . H6 H 0.662(4) 0.408(4) 0.656(3) 0.052(17) Uiso 1 1 d . . . C3 C 0.6191(6) 0.3514(7) 0.7289(4) 0.095(3) Uani 1 1 d . . . H3A H 0.6373 0.3960 0.7576 0.114 Uiso 1 1 calc R . . H3B H 0.6662 0.3085 0.7267 0.114 Uiso 1 1 calc R . . C4 C 0.5353(10) 0.3083(9) 0.7521(4) 0.153(6) Uani 1 1 d . . . H4A H 0.5451 0.2909 0.7941 0.184 Uiso 1 1 calc R . . H4B H 0.4881 0.3513 0.7521 0.184 Uiso 1 1 calc R . . N5 N 0.5049(4) 0.2336(4) 0.7185(2) 0.0620(14) Uani 1 1 d . . . H5 H 0.5500 0.1942 0.7200 0.074 Uiso 1 1 calc R . . C5 C 0.4316(6) 0.1957(6) 0.7538(3) 0.086(2) Uani 1 1 d . . . H5A H 0.4401 0.2078 0.7969 0.103 Uiso 1 1 calc R . . H5B H 0.4310 0.1331 0.7483 0.103 Uiso 1 1 calc R . . C6 C 0.3458(5) 0.2326(4) 0.7334(3) 0.0624(17) Uani 1 1 d . . . H6A H 0.2974 0.2010 0.7527 0.075 Uiso 1 1 calc R . . H6B H 0.3419 0.2929 0.7462 0.075 Uiso 1 1 calc R . . N4 N 0.3361(3) 0.2276(3) 0.6663(2) 0.0475(11) Uani 1 1 d . . . H4 H 0.3026 0.2734 0.6535 0.057 Uiso 1 1 calc R . . C7 C 0.2936(4) 0.1454(4) 0.6447(3) 0.0625(17) Uani 1 1 d . . . H7A H 0.2717 0.1534 0.6033 0.075 Uiso 1 1 calc R . . H7B H 0.2433 0.1315 0.6707 0.075 Uiso 1 1 calc R . . C8 C 0.3591(5) 0.0714(4) 0.6458(4) 0.075(2) Uani 1 1 d . . . H8A H 0.3701 0.0544 0.6878 0.090 Uiso 1 1 calc R . . H8B H 0.3341 0.0218 0.6245 0.090 Uiso 1 1 calc R . . N3 N 0.4441(4) 0.0966(3) 0.6165(3) 0.0625(15) Uani 1 1 d . . . H3 H 0.4900 0.0684 0.6351 0.075 Uiso 1 1 calc R . . C9 C 0.4453(6) 0.0782(5) 0.5513(4) 0.082(2) Uani 1 1 d . . . H9A H 0.4131 0.0246 0.5435 0.099 Uiso 1 1 calc R . . H9B H 0.5062 0.0699 0.5380 0.099 Uiso 1 1 calc R . . C10 C 0.4040(5) 0.1506(5) 0.5151(3) 0.0644(18) Uani 1 1 d . . . N2 N 0.4145(3) 0.2280(3) 0.5405(2) 0.0489(12) Uani 1 1 d . . . C11 C 0.3618(6) 0.1417(7) 0.4587(4) 0.088(3) Uani 1 1 d . . . H11 H 0.3570 0.0873 0.4403 0.106 Uiso 1 1 calc R . . C12 C 0.3279(5) 0.2132(8) 0.4308(3) 0.092(3) Uani 1 1 d . . . H12 H 0.2982 0.2073 0.3938 0.111 Uiso 1 1 calc R . . C13 C 0.3368(4) 0.2948(6) 0.4568(3) 0.075(2) Uani 1 1 d . . . C14 C 0.3828(4) 0.2996(4) 0.5124(3) 0.0511(15) Uani 1 1 d . . . C15 C 0.4003(4) 0.3809(4) 0.5420(3) 0.0502(15) Uani 1 1 d . . . C16 C 0.3677(5) 0.4575(5) 0.5142(4) 0.073(2) Uani 1 1 d . . . C17 C 0.3916(6) 0.5351(6) 0.5422(5) 0.096(3) Uani 1 1 d . . . H17 H 0.3693 0.5873 0.5273 0.115 Uiso 1 1 calc R . . C18 C 0.4460(6) 0.5355(4) 0.5900(5) 0.085(3) Uani 1 1 d . . . H18 H 0.4637 0.5883 0.6069 0.103 Uiso 1 1 calc R . . C19 C 0.3178(6) 0.4501(9) 0.4580(5) 0.107(4) Uani 1 1 d . . . H19 H 0.2951 0.5002 0.4399 0.128 Uiso 1 1 calc R . . C20 C 0.3036(6) 0.3734(9) 0.4315(4) 0.103(3) Uani 1 1 d . . . H20 H 0.2709 0.3712 0.3955 0.123 Uiso 1 1 calc R . . Cl1 Cl 0.33517(11) 0.50913(10) 0.78712(7) 0.0585(5) Uani 1 1 d . . . O11 O 0.3245(5) 0.4643(5) 0.7296(3) 0.116(2) Uani 1 1 d . . . O12 O 0.3144(9) 0.4518(9) 0.8311(4) 0.219(6) Uani 1 1 d . . . O13 O 0.4096(10) 0.5437(11) 0.7838(7) 0.353(13) Uani 1 1 d . . . O14 O 0.2618(9) 0.5610(8) 0.7927(4) 0.223(7) Uani 1 1 d . . . Cl2 Cl 0.12324(12) 0.31045(12) 0.57458(8) 0.0721(5) Uani 1 1 d . . . O21 O 0.1994(5) 0.3380(5) 0.6050(4) 0.120(2) Uani 1 1 d . . . O22A O 0.1390(19) 0.316(5) 0.5183(10) 0.38(4) Uani 0.50 1 d P . . O22B O 0.1488(19) 0.2466(9) 0.5292(8) 0.146(10) Uani 0.50 1 d P . . O23A O 0.0989(18) 0.2440(9) 0.6126(15) 0.186(14) Uani 0.50 1 d P . . O23B O 0.0494(15) 0.261(2) 0.5986(14) 0.172(12) Uani 0.50 1 d P . . O24A O 0.0567(7) 0.3744(9) 0.5950(7) 0.091(4) Uani 0.50 1 d P . . O24B O 0.0904(19) 0.3721(11) 0.5378(15) 0.208(15) Uani 0.50 1 d P . . H101 H 0.616(6) 0.230(6) 0.572(3) 0.10(3) Uiso 1 1 d D . . H102 H 0.605(5) 0.283(3) 0.613(3) 0.05(2) Uiso 1 1 d 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 Ni 0.0390(6) 0.0371(5) 0.0395(5) 0.0010(4) 0.0010(4) 0.0047(4) O1 0.043(2) 0.065(3) 0.067(3) -0.007(3) 0.007(2) 0.009(2) N1 0.045(3) 0.036(2) 0.051(3) 0.004(2) 0.010(2) 0.004(2) C1 0.057(4) 0.046(4) 0.076(4) -0.007(3) 0.018(3) 0.001(3) C2 0.085(6) 0.072(5) 0.090(5) -0.035(4) 0.010(4) -0.008(4) N6 0.046(3) 0.087(4) 0.070(4) -0.019(3) 0.007(3) -0.016(3) C3 0.076(5) 0.140(8) 0.070(5) -0.008(5) -0.025(4) -0.030(6) C4 0.220(15) 0.190(12) 0.050(5) 0.000(6) -0.018(6) -0.115(11) N5 0.061(3) 0.080(4) 0.045(3) 0.014(3) -0.008(3) 0.005(3) C5 0.096(6) 0.111(6) 0.051(4) 0.021(4) 0.000(4) 0.011(5) C6 0.065(4) 0.057(4) 0.065(4) -0.003(3) 0.023(3) 0.002(3) N4 0.044(3) 0.040(2) 0.059(3) 0.010(2) 0.006(2) 0.006(2) C7 0.056(4) 0.062(4) 0.069(4) 0.003(3) 0.010(3) -0.015(3) C8 0.097(6) 0.043(3) 0.085(5) 0.004(3) 0.024(4) -0.013(4) N3 0.070(4) 0.035(3) 0.083(4) 0.001(2) 0.012(3) 0.007(2) C9 0.105(6) 0.049(4) 0.093(5) -0.021(4) 0.032(5) -0.008(4) C10 0.062(4) 0.072(4) 0.059(4) -0.021(3) 0.013(3) -0.020(4) N2 0.054(3) 0.054(3) 0.039(2) -0.005(2) 0.003(2) -0.007(2) C11 0.077(6) 0.121(7) 0.067(5) -0.045(5) 0.017(4) -0.042(5) C12 0.060(5) 0.172(10) 0.045(4) -0.021(5) 0.000(3) -0.033(6) C13 0.046(4) 0.132(7) 0.047(4) 0.023(5) -0.001(3) -0.014(4) C14 0.036(3) 0.074(4) 0.043(3) 0.012(3) 0.003(2) -0.007(3) C15 0.038(3) 0.061(4) 0.052(3) 0.025(3) 0.009(3) 0.009(3) C16 0.056(4) 0.075(5) 0.088(5) 0.043(4) 0.020(4) 0.019(4) C17 0.079(6) 0.064(5) 0.144(9) 0.053(6) 0.040(6) 0.030(5) C18 0.089(6) 0.037(4) 0.131(8) 0.006(4) 0.039(6) 0.011(4) C19 0.056(5) 0.165(10) 0.100(7) 0.091(8) 0.013(5) 0.037(6) C20 0.059(5) 0.182(11) 0.067(5) 0.049(7) -0.006(4) 0.007(7) Cl1 0.0564(9) 0.0538(9) 0.0653(9) 0.0052(7) 0.0052(7) 0.0023(7) O11 0.116(5) 0.134(6) 0.097(4) -0.041(4) -0.003(4) -0.003(4) O12 0.255(13) 0.263(13) 0.139(8) 0.112(8) -0.038(8) -0.023(10) O13 0.260(14) 0.44(2) 0.361(18) -0.283(17) 0.193(14) -0.290(16) O14 0.291(14) 0.262(12) 0.116(6) -0.028(7) -0.014(7) 0.207(12) Cl2 0.0646(11) 0.0790(12) 0.0726(11) 0.0093(9) -0.0135(9) -0.0002(10) O21 0.095(5) 0.123(5) 0.142(6) -0.021(4) -0.061(4) 0.022(4) O22A 0.14(2) 0.96(11) 0.056(11) -0.06(3) 0.046(13) -0.17(4) O22B 0.29(3) 0.069(7) 0.073(10) -0.027(7) -0.009(13) -0.046(10) O23A 0.19(2) 0.036(6) 0.33(4) 0.027(11) 0.12(2) -0.027(10) O23B 0.109(15) 0.23(3) 0.177(19) -0.042(18) 0.076(14) -0.033(15) O24A 0.059(6) 0.098(9) 0.115(9) 0.019(8) -0.021(7) 0.005(6) O24B 0.23(3) 0.092(11) 0.30(3) 0.093(17) -0.20(3) -0.036(14) _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. Weighted least-squares planes through the starred atoms (Nardelli, Musatti, Domiano & Andreetti Ric.Sci.(1965),15(II-A),807). Equation of the plane: m1*X+m2*Y+m3*Z=d Plane 1 m1 = .94273( .00060) m2 = -.06093( .00157) m3 = -.32795( .00165) D = 1.78681( .02785) Atom d s d/s (d/s)**2 N1 * -.0007 .0045 -.151 .023 N2 * .0009 .0045 .204 .042 N3 * -.0014 .0061 -.230 .053 N5 * .0009 .0059 .153 .023 Ni1 .0404 .0009 44.392 1970.636 ============ Sum((d/s)**2) for starred atoms .141 Chi-squared at 95% for 1 degrees of freedom: 3.84 The group of atoms does not deviate significantly from planarity Plane 2 m1 = .85113( .00085) m2 = .07537( .00148) m3 = -.51952( .00131) D = -.52222( .01914) Atom d s d/s (d/s)**2 N1 * -.0020 .0045 -.446 .199 N2 * -.0482 .0045 -10.764 115.873 C18 * .1489 .0096 15.559 242.083 C17 * -.0050 .0096 -.520 .270 C19 * -.0916 .0096 -9.529 90.794 C20 * -.0611 .0090 -6.803 46.274 C11 * .1065 .0090 11.887 141.290 C12 * .0724 .0073 9.894 97.901 ============ Sum((d/s)**2) for starred atoms 734.684 Chi-squared at 95% for 5 degrees of freedom: 11.10 The group of atoms deviates significantly from planarity Plane 3 m1 = .29950( .00254) m2 = .62951( .00199) m3 = -.71695( .00161) D = -6.73194( .03382) Atom d s d/s (d/s)**2 N3 * .0000 .0058 .000 .000 N4 * .0000 .0045 .000 .000 N5 * .0000 .0053 .000 .000 ============ Sum((d/s)**2) for starred atoms .000 Weighted least-squares lines through the starred atoms (Schoemaker,Waser,Marsh & Bergman,Acta Cryst.(1959).12,600) m1,m2,m3 are the direction cosines referred to the X,Y,Z orthogonal axes. X0,Y0,Z0 are the coordinates of the centroid of the set of atoms. Equation of the line: (X-X0)/m1=(Y-Y0)/m2=(Z-Z0)/m3 Line 1 m1 = -.90501( .00088) X0 = 5.99727( .00230) m2 = -.06517( .00225) Y0 = 3.56599( .00234) m3 = .42036( .00189) Z0 = 14.13609( .00223) Atom d s d/s (d/s)**2 Ni1 * .0000 .0012 .003 .000 N4 * .0000 .0064 .001 .000 ============ Sum((d/s)**2) for starred atoms .000 Line 2 m1 = .96144( .00085) X0 = 7.93481( .00230) m2 = .02804( .00295) Y0 = 3.66282( .00310) m3 = -.27357( .00299) Z0 = 13.41541( .00331) Atom d s d/s (d/s)**2 Ni1 * .0000 .0012 .004 .000 O1 * .0000 .0089 .000 .000 ============ Sum((d/s)**2) for starred atoms .000 Dihedral angles formed by LSQ-planes Plane - plane angle (s.u.) angle (s.u.) 1 2 14.50( .11) 165.50( .11) 1 3 61.37( .16) 118.63( .16) 2 3 47.56( .16) 132.44( .16) Angles formed by LSQ-lines Line - line angle (s.u.) angle (s.u.) 1 2 9.27( .18) 170.73( .18) Angles formed by lines and normals to planes Line - plane angle (s.u.) angle (s.u.) 1 1 9.22( .15) 170.78( .15) 1 2 6.50( .13) 173.50( .13) 1 3 52.16( .18) 127.84( .18) 2 1 6.07( .19) 173.93( .19) 2 2 15.73( .18) 164.27( .18) 2 3 59.89( .21) 120.11( .21) ; 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 N2 2.008(5) . ? Ni O1 2.071(5) . ? Ni N4 2.081(5) . ? Ni N5 2.122(5) . ? Ni N3 2.175(5) . ? Ni N1 2.333(4) . ? O1 H101 0.73(5) . ? O1 H102 0.74(5) . ? N1 C1 1.329(8) . ? N1 C15 1.355(8) . ? C1 C18 1.418(11) . ? C1 C2 1.482(10) . ? C2 N6 1.449(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? N6 C3 1.472(10) . ? N6 H6 0.91(7) . ? C3 C4 1.512(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N5 1.437(11) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? N5 C5 1.467(10) . ? N5 H5 0.9100 . ? C5 C6 1.479(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N4 1.476(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? N4 C7 1.493(8) . ? N4 H4 0.9100 . ? C7 C8 1.505(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N3 1.483(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? N3 C9 1.455(9) . ? N3 H3 0.9100 . ? C9 C10 1.501(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.323(8) . ? C10 C11 1.394(11) . ? N2 C14 1.348(8) . ? C11 C12 1.356(13) . ? C11 H11 0.9300 . ? C12 C13 1.382(13) . ? C12 H12 0.9300 . ? C13 C14 1.401(9) . ? C13 C20 1.419(14) . ? C14 C15 1.433(9) . ? C15 C16 1.414(8) . ? C16 C17 1.387(13) . ? C16 C19 1.444(14) . ? C17 C18 1.328(13) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.332(15) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? Cl1 O13 1.242(9) . ? Cl1 O12 1.341(9) . ? Cl1 O14 1.366(9) . ? Cl1 O11 1.444(6) . ? Cl2 O22A 1.26(2) . ? Cl2 O24B 1.337(13) . ? Cl2 O21 1.390(6) . ? Cl2 O23A 1.368(19) . ? Cl2 O23B 1.45(2) . ? Cl2 O22B 1.449(16) . ? Cl2 O24A 1.473(13) . ? O22A O22B 1.11(7) . ? O22A O24B 1.20(5) . ? O23A O23B 0.84(4) . ? O23B O24A 1.75(3) . ? O24A O24B 1.35(4) . ? 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 N2 Ni O1 94.8(2) . . ? N2 Ni N4 94.1(2) . . ? O1 Ni N4 170.7(2) . . ? N2 Ni N5 174.6(2) . . ? O1 Ni N5 87.9(2) . . ? N4 Ni N5 83.0(2) . . ? N2 Ni N3 78.6(2) . . ? O1 Ni N3 96.6(2) . . ? N4 Ni N3 82.53(19) . . ? N5 Ni N3 96.3(2) . . ? N2 Ni N1 75.39(18) . . ? O1 Ni N1 87.22(18) . . ? N4 Ni N1 97.64(16) . . ? N5 Ni N1 109.6(2) . . ? N3 Ni N1 154.0(2) . . ? Ni O1 H101 133(8) . . ? Ni O1 H102 99(6) . . ? H101 O1 H102 113(9) . . ? C1 N1 C15 117.8(5) . . ? C1 N1 Ni 134.5(4) . . ? C15 N1 Ni 107.4(4) . . ? N1 C1 C18 120.6(7) . . ? N1 C1 C2 120.5(6) . . ? C18 C1 C2 118.9(7) . . ? N6 C2 C1 115.4(6) . . ? N6 C2 H2A 108.4 . . ? C1 C2 H2A 108.4 . . ? N6 C2 H2B 108.4 . . ? C1 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? C2 N6 C3 113.8(7) . . ? C2 N6 H6 114(4) . . ? C3 N6 H6 105(4) . . ? N6 C3 C4 112.5(7) . . ? N6 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N6 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N5 C4 C3 116.3(9) . . ? N5 C4 H4A 108.2 . . ? C3 C4 H4A 108.2 . . ? N5 C4 H4B 108.2 . . ? C3 C4 H4B 108.2 . . ? H4A C4 H4B 107.4 . . ? C4 N5 C5 106.7(7) . . ? C4 N5 Ni 124.6(5) . . ? C5 N5 Ni 106.0(4) . . ? C4 N5 H5 106.1 . . ? C5 N5 H5 106.1 . . ? Ni N5 H5 106.1 . . ? N5 C5 C6 110.2(6) . . ? N5 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? N5 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? N4 C6 C5 111.4(5) . . ? N4 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N4 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C6 N4 C7 113.7(5) . . ? C6 N4 Ni 109.0(4) . . ? C7 N4 Ni 108.0(4) . . ? C6 N4 H4 108.7 . . ? C7 N4 H4 108.7 . . ? Ni N4 H4 108.7 . . ? N4 C7 C8 110.7(6) . . ? N4 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N4 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N3 C8 C7 111.1(5) . . ? N3 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? N3 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C9 N3 C8 112.6(6) . . ? C9 N3 Ni 106.7(4) . . ? C8 N3 Ni 108.5(4) . . ? C9 N3 H3 109.7 . . ? C8 N3 H3 109.7 . . ? Ni N3 H3 109.7 . . ? N3 C9 C10 111.6(5) . . ? N3 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N3 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? N2 C10 C11 121.0(8) . . ? N2 C10 C9 113.3(6) . . ? C11 C10 C9 125.6(7) . . ? C10 N2 C14 119.9(5) . . ? C10 N2 Ni 119.5(4) . . ? C14 N2 Ni 119.9(4) . . ? C12 C11 C10 119.3(8) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C13 121.0(7) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C14 116.9(8) . . ? C12 C13 C20 125.3(8) . . ? C14 C13 C20 117.8(9) . . ? N2 C14 C13 121.9(7) . . ? N2 C14 C15 116.1(5) . . ? C13 C14 C15 122.0(6) . . ? N1 C15 C16 123.8(6) . . ? N1 C15 C14 118.2(5) . . ? C16 C15 C14 117.9(6) . . ? C17 C16 C15 115.8(7) . . ? C17 C16 C19 125.3(8) . . ? C15 C16 C19 118.7(8) . . ? C18 C17 C16 120.8(7) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C1 120.8(8) . . ? C17 C18 H18 119.6 . . ? C1 C18 H18 119.6 . . ? C20 C19 C16 121.6(8) . . ? C20 C19 H19 119.2 . . ? C16 C19 H19 119.2 . . ? C19 C20 C13 121.9(8) . . ? C19 C20 H20 119.1 . . ? C13 C20 H20 119.1 . . ? O13 Cl1 O12 122.3(12) . . ? O13 Cl1 O14 118.9(11) . . ? O12 Cl1 O14 97.5(8) . . ? O13 Cl1 O11 104.7(6) . . ? O12 Cl1 O11 106.6(7) . . ? O14 Cl1 O11 105.4(5) . . ? O22A Cl2 O24B 55(3) . . ? O22A Cl2 O21 107.0(14) . . ? O24B Cl2 O21 112.1(9) . . ? O22A Cl2 O23A 134(3) . . ? O24B Cl2 O23A 142.8(18) . . ? O21 Cl2 O23A 99.1(15) . . ? O22A Cl2 O23B 123(2) . . ? O24B Cl2 O23B 108.0(18) . . ? O21 Cl2 O23B 128.2(14) . . ? O23A Cl2 O23B 34.8(16) . . ? O22A Cl2 O22B 48(3) . . ? O24B Cl2 O22B 99.6(18) . . ? O21 Cl2 O22B 108.4(11) . . ? O23A Cl2 O22B 88.9(12) . . ? O23B Cl2 O22B 95.5(14) . . ? O22A Cl2 O24A 112(3) . . ? O24B Cl2 O24A 57.2(16) . . ? O21 Cl2 O24A 102.2(6) . . ? O23A Cl2 O24A 97.6(11) . . ? O23B Cl2 O24A 73.8(12) . . ? O22B Cl2 O24A 147.3(12) . . ? O22B O22A O24B 134(3) . . ? O22B O22A Cl2 75(3) . . ? O24B O22A Cl2 65.8(16) . . ? O22A O22B Cl2 57.0(14) . . ? O23B O23A Cl2 78(3) . . ? O23A O23B Cl2 67(2) . . ? O23A O23B O24A 105(3) . . ? Cl2 O23B O24A 53.8(10) . . ? O24B O24A Cl2 56.3(9) . . ? O24B O24A O23B 92.2(15) . . ? Cl2 O24A O23B 52.4(8) . . ? O22A O24B Cl2 59.0(19) . . ? O22A O24B O24A 125(3) . . ? Cl2 O24B O24A 66.4(12) . . ? _diffrn_measured_fraction_theta_max 0.821 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.821 _refine_diff_density_max 0.818 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.089 #====END