Supplementary Material (ESI) 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 'Andrea Bencini' 'Carmen Anda' 'Carla Bazzicalupi' 'Antonio Bianchi' 'Patrizia Fornasari' 'Claudia Giorgi' ; C.Lodeiro ; 'A Jorge Parola' 'F. Pina' 'Barbara Valtancoli' _publ_contact_author_name 'Prof Andrea Bencini' _publ_contact_author_address ; Department of Chemistry Universitą di Firenze Via della Lastruccia 3 Sesto Fiorentino - Firenze 50019 ITALY ; _publ_contact_author_email ANDREA.BENCINI@UNIFI.IT _publ_section_title ; Cu(II) and Ni(II) Complexes with Dipyridine-Containing Macrocyclic Polyamines with Different Binding units. ; data_[CuL1](ClO4)2 _database_code_CSD 199214 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (C20 H31 N7 Cu 2+)2, (Cl O4 -1)4 ; _chemical_formula_sum 'C40 H62 Cl4 Cu2 N14 O16' _chemical_formula_weight 1263.92 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' Cu Cu 0.3201 1.2651 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.245(5) _cell_length_b 18.438(7) _cell_length_c 20.233(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.26(3) _cell_angle_gamma 90.00 _cell_volume 5212(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6 _cell_measurement_theta_max 12 _exptl_crystal_description prismatic _exptl_crystal_colour blue _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ENRAF NONIUS CAD4' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6583 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.2099 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 24.01 _reflns_number_total 6361 _reflns_number_gt 2775 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ENRAF NONIUS CAD4' _computing_cell_refinement 'ENRAF NONIUS CAD4' _computing_data_reduction 'ENRAF NONIUS CAD4' _computing_structure_solution 'SIR97(Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 Ver. 1.01\b (Farrugia, 1997)' _computing_publication_material 'PARST93 (Nardelli, 1993)' _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^)+(0.1369P)^2^+0.0000P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6361 _refine_ls_number_parameters 687 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2377 _refine_ls_R_factor_gt 0.0882 _refine_ls_wR_factor_ref 0.2892 _refine_ls_wR_factor_gt 0.2225 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.002 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 Cu1 Cu 0.75204(12) 0.44801(9) 0.34938(9) 0.0548(6) Uani 1 1 d . . . Cu2 Cu 0.30719(12) 0.14290(9) 0.41403(9) 0.0558(6) Uani 1 1 d . . . N1 N 0.6051(8) 0.4660(6) 0.3479(6) 0.048(3) Uani 1 1 d . . . N2 N 0.7011(12) 0.5382(9) 0.2596(6) 0.083(4) Uani 1 1 d . . . H2C H 0.7334 0.5317 0.2199 0.050 Uiso 1 1 d . . . N3 N 0.7935(10) 0.5437(7) 0.3955(6) 0.073(4) Uani 1 1 d . . . H3C H 0.7891 0.5396 0.4396 0.050 Uiso 1 1 calc R . . N4 N 0.8801(9) 0.4493(8) 0.3242(6) 0.075(4) Uani 1 1 d . . . H4C H 0.9180 0.4218 0.3560 0.050 Uiso 1 1 calc R . . N5 N 0.7360(8) 0.3540(6) 0.2959(5) 0.052(3) Uani 1 1 d . . . H5C H 0.6756 0.3544 0.2708 0.050 Uiso 1 1 calc R . . N6 N 0.8921(11) 0.3305(10) 0.4136(9) 0.099(5) Uani 1 1 d . . . N7 N 0.7205(10) 0.3920(6) 0.4467(6) 0.060(3) Uani 1 1 d . . . N8 N 0.1734(8) 0.1052(8) 0.4199(6) 0.064(4) Uani 1 1 d . . . N9 N 0.2471(13) 0.2345(7) 0.4799(8) 0.088(5) Uani 1 1 d . . . H9C H 0.2666 0.2796 0.4702 0.050 Uiso 1 1 calc R . . N10 N 0.3614(9) 0.1060(7) 0.5097(6) 0.067(4) Uani 1 1 d . . . H10C H 0.3546 0.0569 0.5094 0.050 Uiso 1 1 calc R . . N11 N 0.4359(9) 0.1852(7) 0.4192(7) 0.069(3) Uani 1 1 d . . . H11C H 0.4692 0.1528 0.3988 0.050 Uiso 1 1 calc R . . N12 N 0.2807(10) 0.1964(8) 0.3224(7) 0.077(4) Uani 1 1 d . . . H12C H 0.2204 0.2147 0.3174 0.050 Uiso 1 1 calc R . . N13 N 0.4405(11) 0.0933(10) 0.3057(8) 0.088(4) Uani 1 1 d . . . N14 N 0.2909(9) 0.0223(6) 0.3612(5) 0.057(3) Uani 1 1 d . . . Cl1 Cl 0.6952(4) 0.0794(3) 0.4123(3) 0.0953(15) Uani 1 1 d . . . O11 O 0.6280(14) 0.0505(9) 0.4471(10) 0.179(8) Uani 1 1 d . . . O12 O 0.7526(18) 0.1180(17) 0.4573(11) 0.264(14) Uani 1 1 d . . . O13 O 0.6588(14) 0.1112(15) 0.3514(12) 0.262(15) Uani 1 1 d . . . O14 O 0.745(2) 0.0271(13) 0.3919(17) 0.290(17) Uani 1 1 d . . . Cl2 Cl 0.5335(4) 0.2866(3) 0.1630(3) 0.0896(14) Uani 1 1 d . . . O21 O 0.4452(13) 0.2704(11) 0.1308(13) 0.253(13) Uani 1 1 d . . . O22 O 0.5955(17) 0.2372(12) 0.1710(15) 0.293(17) Uani 1 1 d . . . O23 O 0.5241(13) 0.3224(15) 0.2190(10) 0.236(12) Uani 1 1 d . . . O24 O 0.574(2) 0.3430(16) 0.1321(15) 0.293(15) Uani 1 1 d . . . Cl3 Cl 0.1756(5) 0.4325(3) 0.4152(3) 0.0985(16) Uani 1 1 d . . . O31 O 0.2629(10) 0.4096(8) 0.4595(8) 0.132(5) Uani 1 1 d . . . O32 O 0.1817(18) 0.4996(10) 0.4072(19) 0.33(2) Uani 1 1 d . . . O33 O 0.0960(13) 0.4143(16) 0.4377(13) 0.271(16) Uani 1 1 d . . . O34 O 0.170(2) 0.404(2) 0.3567(11) 0.33(2) Uani 1 1 d . . . C1 C 0.5664(13) 0.4418(8) 0.3995(8) 0.069(5) Uani 1 1 d . . . C2 C 0.4701(14) 0.4553(12) 0.3992(13) 0.106(7) Uani 1 1 d . . . H2 H 0.4440 0.4427 0.4364 0.050 Uiso 1 1 calc R . . C3 C 0.4156(16) 0.4861(13) 0.3459(18) 0.141(12) Uani 1 1 d . . . H3 H 0.3500 0.4902 0.3435 0.050 Uiso 1 1 calc R . . C4 C 0.4558(14) 0.5117(12) 0.2947(13) 0.112(7) Uani 1 1 d . . . H4 H 0.4193 0.5375 0.2592 0.050 Uiso 1 1 calc R . . C5 C 0.5507(12) 0.4990(9) 0.2964(8) 0.071(5) Uani 1 1 d . . . C6 C 0.5986(15) 0.5228(12) 0.2408(8) 0.105(7) Uani 1 1 d . . . H6A H 0.5893 0.4854 0.2064 0.050 Uiso 1 1 calc R . . H6B H 0.5666 0.5662 0.2207 0.050 Uiso 1 1 calc R . . C7 C 0.7192(15) 0.6082(12) 0.2889(12) 0.114(8) Uani 1 1 d . . . H7A H 0.6664 0.6403 0.2711 0.050 Uiso 1 1 calc R . . H7B H 0.7769 0.6280 0.2772 0.050 Uiso 1 1 calc R . . C8 C 0.7314(14) 0.6038(9) 0.3662(10) 0.095(6) Uani 1 1 d . . . H8A H 0.7583 0.6491 0.3858 0.050 Uiso 1 1 calc R . . H8B H 0.6690 0.5979 0.3779 0.050 Uiso 1 1 calc R . . C9 C 0.8964(13) 0.5539(11) 0.3925(9) 0.092(6) Uani 1 1 d . . . H9A H 0.9356 0.5325 0.4323 0.050 Uiso 1 1 calc R . . H9B H 0.9105 0.6054 0.3928 0.050 Uiso 1 1 calc R . . C10 C 0.9222(11) 0.5203(10) 0.3312(10) 0.083(5) Uani 1 1 d . . . H10A H 0.8977 0.5495 0.2917 0.050 Uiso 1 1 calc R . . H10B H 0.9912 0.5169 0.3363 0.050 Uiso 1 1 calc R . . C11 C 0.8754(13) 0.4102(10) 0.2619(9) 0.085(5) Uani 1 1 d . . . H11A H 0.9366 0.3868 0.2627 0.050 Uiso 1 1 calc R . . H11B H 0.8653 0.4447 0.2250 0.050 Uiso 1 1 calc R . . C12 C 0.8005(14) 0.3557(11) 0.2489(9) 0.102(6) Uani 1 1 d . . . H12A H 0.7630 0.3638 0.2040 0.050 Uiso 1 1 calc R . . H12B H 0.8304 0.3084 0.2489 0.050 Uiso 1 1 calc R . . C13 C 0.7457(12) 0.2874(9) 0.3339(9) 0.079(5) Uani 1 1 d . . . H13A H 0.7286 0.2475 0.3027 0.050 Uiso 1 1 calc R . . H13B H 0.6997 0.2880 0.3636 0.050 Uiso 1 1 calc R . . C14 C 0.8455(17) 0.2719(12) 0.3769(11) 0.118(8) Uani 1 1 d . . . H14A H 0.8392 0.2333 0.4083 0.050 Uiso 1 1 calc R . . H14B H 0.8862 0.2539 0.3473 0.050 Uiso 1 1 calc R . . C15 C 0.8781(15) 0.3328(13) 0.4800(12) 0.129(9) Uani 1 1 d . . . H15A H 0.9234 0.3674 0.5043 0.050 Uiso 1 1 calc R . . H15B H 0.8950 0.2856 0.5000 0.050 Uiso 1 1 calc R . . C16 C 0.7791(15) 0.3524(11) 0.4930(8) 0.084(5) Uani 1 1 d . . . C17 C 0.7512(18) 0.3283(13) 0.5509(10) 0.109(7) Uani 1 1 d . . . H17 H 0.7929 0.3014 0.5827 0.050 Uiso 1 1 calc R . . C18 C 0.665(2) 0.3439(13) 0.5600(11) 0.128(9) Uani 1 1 d . . . H18 H 0.6476 0.3283 0.5996 0.050 Uiso 1 1 calc R . . C19 C 0.5982(14) 0.3829(10) 0.5134(11) 0.090(6) Uani 1 1 d . . . H19 H 0.5366 0.3925 0.5199 0.050 Uiso 1 1 calc R . . C20 C 0.6320(14) 0.4063(8) 0.4558(8) 0.070(5) Uani 1 1 d . . . C21 C 0.1474(11) 0.0376(10) 0.4057(7) 0.059(4) Uani 1 1 d . . . C22 C 0.0593(14) 0.0120(13) 0.4152(8) 0.092(6) Uani 1 1 d . . . H22 H 0.0425 -0.0363 0.4064 0.050 Uiso 1 1 calc R . . C23 C -0.0015(14) 0.0576(17) 0.4374(10) 0.105(8) Uani 1 1 d . . . H23 H -0.0615 0.0412 0.4423 0.050 Uiso 1 1 calc R . . C24 C 0.0243(14) 0.1284(15) 0.4529(10) 0.102(7) Uani 1 1 d . . . H24 H -0.0166 0.1602 0.4690 0.050 Uiso 1 1 calc R . . C25 C 0.1158(13) 0.1508(13) 0.4434(9) 0.090(6) Uani 1 1 d . . . C26 C 0.1455(19) 0.2263(13) 0.4588(13) 0.132(9) Uani 1 1 d . . . H26A H 0.1240 0.2558 0.4191 0.050 Uiso 1 1 calc R . . H26B H 0.1145 0.2441 0.4942 0.050 Uiso 1 1 calc R . . C27 C 0.2880(16) 0.2137(11) 0.5489(10) 0.111(7) Uani 1 1 d . . . H27A H 0.2442 0.2281 0.5777 0.050 Uiso 1 1 calc R . . H27B H 0.3472 0.2402 0.5635 0.050 Uiso 1 1 calc R . . C28 C 0.3079(13) 0.1353(9) 0.5584(8) 0.078(5) Uani 1 1 d . . . H28A H 0.3443 0.1272 0.6036 0.050 Uiso 1 1 calc R . . H28B H 0.2478 0.1094 0.5542 0.050 Uiso 1 1 calc R . . C29 C 0.4633(13) 0.1220(9) 0.5248(8) 0.086(6) Uani 1 1 d . . . H29A H 0.4984 0.0815 0.5111 0.050 Uiso 1 1 calc R . . H29B H 0.4840 0.1285 0.5730 0.050 Uiso 1 1 calc R . . C30 C 0.4847(12) 0.1883(10) 0.4895(9) 0.091(6) Uani 1 1 d . . . H30A H 0.4636 0.2307 0.5109 0.050 Uiso 1 1 calc R . . H30B H 0.5532 0.1923 0.4920 0.050 Uiso 1 1 calc R . . C31 C 0.428(2) 0.2484(12) 0.3800(12) 0.137(9) Uani 1 1 d . . . H31A H 0.4832 0.2497 0.3581 0.050 Uiso 1 1 calc R . . H31B H 0.4343 0.2895 0.4104 0.050 Uiso 1 1 calc R . . C32 C 0.3452(17) 0.2591(11) 0.3297(11) 0.112(7) Uani 1 1 d . . . H32A H 0.3640 0.2685 0.2869 0.050 Uiso 1 1 calc R . . H32B H 0.3113 0.3015 0.3411 0.050 Uiso 1 1 calc R . . C33 C 0.2820(15) 0.1524(12) 0.2619(9) 0.112(8) Uani 1 1 d . . . H33A H 0.2528 0.1807 0.2228 0.050 Uiso 1 1 calc R . . H33B H 0.2417 0.1103 0.2636 0.050 Uiso 1 1 calc R . . C34 C 0.3755(18) 0.1267(13) 0.2508(11) 0.116(8) Uani 1 1 d . . . H34A H 0.3636 0.0921 0.2140 0.050 Uiso 1 1 calc R . . H34B H 0.4082 0.1677 0.2356 0.050 Uiso 1 1 calc R . . C35 C 0.4293(13) 0.0151(12) 0.3066(9) 0.094(6) Uani 1 1 d . . . H35A H 0.4880 -0.0044 0.3331 0.050 Uiso 1 1 calc R . . H35B H 0.4256 -0.0017 0.2608 0.050 Uiso 1 1 calc R . . C36 C 0.3482(12) -0.0196(10) 0.3321(8) 0.067(4) Uani 1 1 d . . . C37 C 0.3349(18) -0.0920(12) 0.3207(10) 0.103(7) Uani 1 1 d . . . H37 H 0.3741 -0.1183 0.2977 0.050 Uiso 1 1 calc R . . C38 C 0.2614(19) -0.1246(12) 0.3445(11) 0.110(7) Uani 1 1 d . . . H38 H 0.2531 -0.1746 0.3404 0.050 Uiso 1 1 calc R . . C39 C 0.2013(18) -0.0851(14) 0.3738(12) 0.125(8) Uani 1 1 d . . . H39 H 0.1508 -0.1071 0.3891 0.050 Uiso 1 1 calc R . . C40 C 0.2165(12) -0.0099(10) 0.3806(7) 0.067(5) Uani 1 1 d . . . Cl4 Cl 0.0203(7) 0.2274(5) 0.2069(9) 0.234(7) Uani 1 1 d . . . O41 O 0.0356(13) 0.2169(14) 0.2890(8) 0.194(11) Uani 1 1 d . . . O42 O 0.004(4) 0.167(3) 0.160(3) 0.52(4) Uani 1 1 d . . . O43 O 0.109(3) 0.2519(18) 0.207(3) 0.52(4) Uani 1 1 d . . . O44 O -0.036(3) 0.272(3) 0.192(2) 0.55(4) Uani 1 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 Cu1 0.0580(11) 0.0545(11) 0.0543(11) -0.0062(9) 0.0171(9) -0.0090(10) Cu2 0.0573(11) 0.0554(11) 0.0529(11) 0.0064(9) 0.0063(8) 0.0046(9) N1 0.053(7) 0.048(7) 0.041(7) -0.015(6) 0.008(6) -0.003(6) N2 0.104(13) 0.104(12) 0.049(8) 0.027(8) 0.033(8) 0.044(10) N3 0.095(11) 0.070(9) 0.060(8) -0.019(7) 0.033(8) -0.005(9) N4 0.078(9) 0.084(10) 0.065(9) -0.002(8) 0.021(7) -0.014(8) N5 0.065(8) 0.046(7) 0.047(7) 0.001(6) 0.016(6) -0.003(6) N6 0.082(11) 0.128(15) 0.074(11) 0.020(11) -0.016(9) 0.010(10) N7 0.071(9) 0.062(8) 0.049(8) 0.006(7) 0.015(7) -0.019(7) N8 0.048(8) 0.074(10) 0.074(9) 0.020(8) 0.022(7) 0.022(8) N9 0.112(13) 0.044(8) 0.119(14) 0.018(8) 0.046(11) 0.039(9) N10 0.064(9) 0.076(9) 0.058(8) 0.013(7) 0.001(7) 0.017(7) N11 0.068(9) 0.065(9) 0.073(9) -0.003(8) 0.012(7) -0.009(7) N12 0.070(9) 0.094(11) 0.063(10) 0.036(8) 0.004(7) 0.018(8) N13 0.089(11) 0.096(13) 0.077(11) -0.017(10) 0.011(9) -0.007(10) N14 0.077(9) 0.054(8) 0.033(7) -0.003(6) -0.009(6) -0.004(7) Cl1 0.090(4) 0.091(4) 0.106(4) 0.013(3) 0.021(3) -0.007(3) O11 0.213(18) 0.147(14) 0.229(19) 0.074(14) 0.171(17) 0.047(13) O12 0.24(2) 0.39(4) 0.150(18) -0.11(2) 0.013(17) -0.13(3) O13 0.162(18) 0.37(3) 0.22(2) 0.23(2) -0.042(16) -0.042(19) O14 0.37(4) 0.17(2) 0.41(4) 0.00(2) 0.28(4) 0.00(2) Cl2 0.073(3) 0.089(3) 0.103(4) -0.014(3) 0.007(3) 0.006(3) O21 0.138(16) 0.20(2) 0.35(3) -0.13(2) -0.130(18) -0.006(14) O22 0.22(2) 0.20(2) 0.40(4) -0.11(2) -0.08(2) 0.15(2) O23 0.138(15) 0.40(3) 0.171(17) -0.16(2) 0.031(13) 0.032(18) O24 0.32(3) 0.27(3) 0.33(3) 0.14(3) 0.16(3) 0.01(3) Cl3 0.130(5) 0.085(4) 0.084(4) 0.006(3) 0.031(3) 0.001(3) O31 0.097(10) 0.155(13) 0.143(13) 0.042(11) 0.022(10) 0.033(10) O32 0.24(3) 0.061(12) 0.60(6) 0.02(2) -0.12(3) -0.009(14) O33 0.099(13) 0.42(4) 0.31(3) 0.23(3) 0.070(16) 0.039(18) O34 0.33(4) 0.54(6) 0.107(16) -0.12(2) 0.000(19) 0.10(3) C1 0.105(15) 0.042(9) 0.063(11) -0.013(9) 0.022(11) -0.014(10) C2 0.054(13) 0.113(17) 0.17(2) -0.037(16) 0.058(14) -0.003(12) C3 0.034(13) 0.114(19) 0.27(4) 0.00(2) 0.031(19) 0.010(13) C4 0.048(14) 0.115(18) 0.15(2) 0.004(15) -0.024(13) 0.019(12) C5 0.068(12) 0.078(12) 0.060(11) -0.015(10) -0.004(10) 0.008(10) C6 0.125(19) 0.137(19) 0.048(11) 0.012(11) 0.003(12) 0.041(15) C7 0.103(16) 0.099(17) 0.16(2) 0.055(16) 0.064(16) 0.034(13) C8 0.119(17) 0.054(11) 0.137(18) -0.022(12) 0.085(14) 0.002(11) C9 0.089(15) 0.095(14) 0.081(13) -0.004(12) -0.010(11) -0.026(12) C10 0.050(10) 0.090(14) 0.106(15) 0.012(11) 0.006(10) -0.007(10) C11 0.089(14) 0.094(13) 0.080(13) -0.009(11) 0.036(11) 0.015(11) C12 0.106(15) 0.130(17) 0.073(12) -0.057(12) 0.027(11) -0.031(14) C13 0.087(14) 0.062(11) 0.094(13) -0.018(10) 0.029(11) 0.007(10) C14 0.15(2) 0.103(18) 0.102(16) 0.019(14) 0.028(16) 0.071(17) C15 0.107(19) 0.122(19) 0.13(2) 0.048(16) -0.060(16) -0.003(14) C16 0.113(17) 0.102(14) 0.036(10) 0.000(10) 0.012(10) -0.006(13) C17 0.113(18) 0.14(2) 0.061(14) 0.017(13) -0.009(13) -0.023(16) C18 0.20(3) 0.12(2) 0.069(15) 0.028(14) 0.046(19) -0.04(2) C19 0.093(15) 0.084(13) 0.105(16) -0.018(12) 0.051(13) -0.026(11) C20 0.105(15) 0.055(10) 0.056(11) -0.017(9) 0.034(11) -0.029(10) C21 0.048(10) 0.082(13) 0.044(9) 0.014(9) 0.005(7) 0.006(9) C22 0.064(13) 0.141(18) 0.063(12) 0.027(12) -0.009(10) -0.030(13) C23 0.055(12) 0.19(3) 0.073(13) 0.064(17) 0.021(10) 0.005(17) C24 0.075(15) 0.16(2) 0.085(14) 0.057(16) 0.053(11) 0.043(15) C25 0.070(13) 0.114(17) 0.095(14) 0.041(13) 0.037(11) 0.035(13) C26 0.15(3) 0.11(2) 0.15(2) 0.037(17) 0.074(19) 0.058(18) C27 0.15(2) 0.102(17) 0.089(16) -0.017(13) 0.045(15) 0.011(14) C28 0.098(13) 0.078(13) 0.067(11) 0.004(9) 0.037(10) 0.026(10) C29 0.115(17) 0.071(13) 0.059(11) 0.003(10) -0.016(11) 0.018(11) C30 0.074(12) 0.099(15) 0.090(14) -0.027(12) -0.009(11) 0.010(11) C31 0.19(3) 0.12(2) 0.104(18) 0.013(16) 0.034(19) -0.059(19) C32 0.17(2) 0.076(14) 0.094(16) 0.053(13) 0.028(16) 0.004(15) C33 0.114(18) 0.132(19) 0.062(13) 0.031(13) -0.049(12) -0.037(15) C34 0.13(2) 0.127(19) 0.100(18) -0.041(15) 0.048(16) -0.031(17) C35 0.087(14) 0.130(19) 0.063(12) -0.021(12) 0.007(10) 0.016(13) C36 0.067(11) 0.068(12) 0.066(11) -0.029(9) 0.009(9) 0.004(9) C37 0.13(2) 0.087(17) 0.079(14) -0.024(12) -0.002(13) 0.028(14) C38 0.15(2) 0.068(14) 0.112(18) -0.032(13) 0.032(16) -0.021(16) C39 0.14(2) 0.12(2) 0.113(19) -0.009(16) 0.004(16) -0.063(18) C40 0.071(11) 0.086(13) 0.045(9) 0.002(9) 0.010(8) -0.027(11) Cl4 0.123(7) 0.103(6) 0.51(2) -0.011(9) 0.150(11) -0.003(5) O41 0.135(15) 0.37(3) 0.086(11) 0.051(15) 0.034(10) 0.043(17) O42 0.50(7) 0.30(5) 0.80(11) -0.17(6) 0.22(7) -0.13(5) O43 0.28(4) 0.22(3) 0.95(12) 0.14(5) -0.12(6) -0.05(3) O44 0.44(6) 0.57(7) 0.54(7) 0.01(5) -0.15(5) 0.41(6) _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 = -0.05452(0.00007) m2 = 0.49601(0.00005) m3 = -0.86660(0.00000) D = -2.22870(0.00118) Atom d s d/s (d/s)**2 N1 * 0.1128 0.0002 472.223 222994.203 N3 * -0.1310 0.0002 -548.414 300758.000 N4 * 0.1473 0.0002 616.910 380577.688 N5 * -0.1291 0.0002 -540.718 292376.313 Cu1 -0.1906 0.0002 -798.070 636915.188 #=========== Sum((d/s)**2) for starred atoms ********** Chi-squared at 95% for 1 degrees of freedom: 3.84 The group of atoms deviates significantly from planarity Plane 2 m1 = 0.33157(0.00010) m2 = -0.84663(0.00003) m3 = -0.41626(0.00009) D = -4.83332(0.00087) Atom d s d/s (d/s)**2 N8 * -0.0083 0.0003 -25.109 630.455 N10 * 0.0098 0.0003 29.938 896.297 N11 * -0.0108 0.0003 -32.801 1075.908 N12 * 0.0092 0.0003 27.972 782.416 Cu2 0.0910 0.0003 276.939 76694.992 #=========== Sum((d/s)**2) for starred atoms 3385.076 Chi-squared at 95% for 1 degrees of freedom: 3.84 The group of atoms deviates significantly from planarity Plane 3 m1 = -0.12633(0.00011) m2 = -0.87909(0.00004) m3 = -0.45960(0.00012) D = -11.63923(0.00062) Atom d s d/s (d/s)**2 C1 * 0.0129 0.0003 41.342 1709.199 C2 * -0.0262 0.0003 -83.951 7047.743 C3 * 0.0277 0.0003 89.005 7921.978 C4 * -0.0159 0.0003 -51.099 2611.125 C5 * 0.0032 0.0003 10.206 104.173 N1 * -0.0017 0.0003 -5.504 30.299 #=========== Sum((d/s)**2) for starred atoms 19424.516 Chi-squared at 95% for 3 degrees of freedom: 7.81 The group of atoms deviates significantly from planarity Plane 4 m1 = -0.25184(0.00013) m2 = -0.84543(0.00005) m3 = -0.47098(0.00011) D = -12.41243(0.00099) Atom d s d/s (d/s)**2 N7 * -0.0126 0.0003 -39.878 1590.293 C16 * 0.0108 0.0003 33.936 1151.659 C17 * 0.0022 0.0003 7.080 50.131 C18 * -0.0125 0.0003 -39.430 1554.702 C19 * 0.0098 0.0003 31.046 963.874 C20 * 0.0023 0.0003 7.245 52.497 #=========== Sum((d/s)**2) for starred atoms 5363.155 Chi-squared at 95% for 3 degrees of freedom: 7.81 The group of atoms deviates significantly from planarity Plane 5 m1 = -0.21967(0.00008) m2 = 0.26730(0.00009) m3 = -0.93824(0.00001) D = -7.48377(0.00047) Atom d s d/s (d/s)**2 N8 * 0.0057 0.0002 25.112 630.626 C21 * 0.0056 0.0002 24.741 612.121 C22 * -0.0146 0.0002 -64.312 4136.034 C23 * 0.0124 0.0002 54.517 2972.093 C24 * -0.0011 0.0002 -4.961 24.608 C25 * -0.0080 0.0002 -35.098 1231.842 #=========== Sum((d/s)**2) for starred atoms 9607.323 Chi-squared at 95% for 3 degrees of freedom: 7.81 The group of atoms deviates significantly from planarity Plane 6 m1 = -0.41924(0.00009) m2 = 0.16401(0.00010) m3 = -0.89294(0.00002) D = -7.46128(0.00012) Atom d s d/s (d/s)**2 N14 * -0.0086 0.0003 -32.659 1066.578 C36 * -0.0162 0.0003 -61.752 3813.327 C37 * 0.0286 0.0003 108.966 11873.653 C38 * -0.0176 0.0003 -66.978 4485.989 C39 * -0.0062 0.0003 -23.456 550.203 C40 * 0.0199 0.0003 75.878 5757.517 #=========== Sum((d/s)**2) for starred atoms 27547.268 Chi-squared at 95% for 3 degrees of freedom: 7.81 The group of atoms deviates significantly from planarity 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 = -0.15097(0.00025) X0 = 9.14710(0.00032) m2 = 0.67433(0.00011) Y0 = 9.09159(0.00024) m3 = -0.72283(0.00011) Z0 = 6.04216(0.00014) Atom d s d/s (d/s)**2 Cu1 * 0.0000 0.0005 0.001 0.000 N2 * 0.0000 0.0005 0.001 0.000 #=========== Sum((d/s)**2) for starred atoms 0.000 Line 2 m1 = -0.35574(0.00023) X0 = 8.91597(0.00032) m2 = -0.44106(0.00017) Y0 = 7.74359(0.00024) m3 = 0.82396(0.00011) Z0 = 7.89892(0.00014) Atom d s d/s (d/s)**2 Cu1 * 0.0000 0.0005 0.001 0.000 N7 * 0.0000 0.0005 0.001 0.000 #=========== Sum((d/s)**2) for starred atoms 0.000 Line 3 m1 = -0.46479(0.00021) X0 = 2.17975(0.00032) m2 = 0.69928(0.00014) Y0 = 3.47759(0.00024) m3 = 0.54311(0.00012) Z0 = 8.87006(0.00014) Atom d s d/s (d/s)**2 Cu2 * 0.0000 0.0005 0.000 0.000 N9 * 0.0000 0.0005 0.000 0.000 #=========== Sum((d/s)**2) for starred atoms 0.000 Line 4 m1 = -0.01052(0.00027) X0 = 2.72687(0.00032) m2 = -0.90448(0.00004) Y0 = 1.52224(0.00024) m3 = -0.42639(0.00012) Z0 = 7.69106(0.00014) Atom d s d/s (d/s)**2 Cu2 * 0.0000 0.0005 0.001 0.000 N14 * 0.0000 0.0005 0.001 0.000 #=========== Sum((d/s)**2) for starred atoms 0.000 Dihedral angles formed by LSQ-planes Plane - plane angle (s.u.) angle (s.u.) 1 2 85.57( 0.00) 94.43( 0.00) 1 3 88.23( 0.01) 91.77( 0.01) 1 4 89.85( 0.01) 90.15( 0.01) 1 5 16.74( 0.01) 163.26( 0.01) 1 6 28.59( 0.01) 151.41( 0.01) 2 3 26.66( 0.01) 153.34( 0.01) 2 4 34.07( 0.01) 145.93( 0.01) 2 5 84.75( 0.01) 95.25( 0.01) 2 6 84.62( 0.01) 95.38( 0.01) 3 4 7.48( 0.01) 172.52( 0.01) 3 5 77.06( 0.01) 102.94( 0.01) 3 6 71.39( 0.01) 108.61( 0.01) 4 5 74.26( 0.01) 105.74( 0.01) 4 6 67.20( 0.01) 112.80( 0.01) 5 6 13.16( 0.01) 166.84( 0.01) Angles formed by LSQ-lines Line - line angle (s.u.) angle (s.u.) 1 2 32.93( 0.02) 147.07( 0.02) 1 3 81.42( 0.01) 98.58( 0.01) 1 4 72.54( 0.01) 107.46( 0.01) 2 3 72.28( 0.01) 107.72( 0.01) 2 4 87.06( 0.01) 92.94( 0.01) 3 4 30.78( 0.02) 149.22( 0.02) Angles formed by lines and normals to planes Line - plane angle (s.u.) angle (s.u.) 1 1 14.28( 0.01) 165.72( 0.01) 1 2 71.33( 0.01) 108.67( 0.01) 1 3 76.02( 0.01) 103.98( 0.01) 1 4 78.95( 0.01) 101.05( 0.01) 1 5 26.92( 0.01) 153.08( 0.01) 1 6 34.98( 0.01) 145.02( 0.01) 2 1 24.02( 0.01) 155.98( 0.01) 2 2 84.98( 0.01) 95.02( 0.01) 2 3 86.91( 0.01) 93.09( 0.01) 2 4 85.73( 0.01) 94.27( 0.01) 2 5 35.63( 0.01) 144.37( 0.01) 2 6 48.78( 0.01) 131.22( 0.01) 3 1 84.35( 0.01) 95.65( 0.01) 3 2 13.54( 0.01) 166.46( 0.01) 3 3 36.33( 0.01) 143.67( 0.01) 3 4 43.12( 0.01) 136.88( 0.01) 3 5 77.26( 0.01) 102.74( 0.01) 3 6 79.90( 0.01) 100.10( 0.01) 4 1 85.49( 0.01) 94.51( 0.01) 4 2 19.99( 0.02) 160.01( 0.02) 4 3 7.06( 0.02) 172.94( 0.02) 4 4 14.50( 0.02) 165.50( 0.02) 4 5 80.76( 0.01) 99.24( 0.01) 4 6 76.30( 0.01) 103.70( 0.01) ; 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 Cu1 N4 1.988(12) . ? Cu1 N3 2.030(12) . ? Cu1 N5 2.032(11) . ? Cu1 N1 2.113(11) . ? Cu1 N7 2.344(12) . ? Cu1 N2 2.465(13) . ? Cu2 N11 1.976(12) . ? Cu2 N10 2.054(11) . ? Cu2 N8 2.053(12) . ? Cu2 N12 2.069(12) . ? Cu2 N9 2.409(13) . ? Cu2 N14 2.459(11) . ? N1 C5 1.321(18) . ? N1 C1 1.347(17) . ? N2 C7 1.42(2) . ? N2 C6 1.46(2) . ? N3 C8 1.47(2) . ? N3 C9 1.491(19) . ? N4 C10 1.436(19) . ? N4 C11 1.441(18) . ? N5 C12 1.447(18) . ? N5 C13 1.441(18) . ? N6 C15 1.40(2) . ? N6 C14 1.40(2) . ? N7 C20 1.336(19) . ? N7 C16 1.34(2) . ? N8 C21 1.317(18) . ? N8 C25 1.33(2) . ? N9 C26 1.43(2) . ? N9 C27 1.46(2) . ? N10 C29 1.455(19) . ? N10 C28 1.462(17) . ? N11 C31 1.40(2) . ? N11 C30 1.457(19) . ? N12 C33 1.47(2) . ? N12 C32 1.47(2) . ? N13 C34 1.44(2) . ? N13 C35 1.45(2) . ? N14 C40 1.339(17) . ? N14 C36 1.340(18) . ? Cl1 O14 1.31(2) . ? Cl1 O12 1.31(2) . ? Cl1 O13 1.372(16) . ? Cl1 O11 1.399(14) . ? Cl2 O22 1.257(17) . ? Cl2 O21 1.332(15) . ? Cl2 O23 1.340(16) . ? Cl2 O24 1.39(2) . ? Cl3 O32 1.253(18) . ? Cl3 O34 1.28(2) . ? Cl3 O33 1.344(17) . ? Cl3 O31 1.447(14) . ? C1 C2 1.39(2) . ? C1 C20 1.48(2) . ? C2 C3 1.33(3) . ? C3 C4 1.36(3) . ? C4 C5 1.37(2) . ? C5 C6 1.49(2) . ? C7 C8 1.54(3) . ? C9 C10 1.49(2) . ? C11 C12 1.45(2) . ? C13 C14 1.54(2) . ? C15 C16 1.53(3) . ? C16 C17 1.38(2) . ? C17 C18 1.31(3) . ? C18 C19 1.40(3) . ? C19 C20 1.41(2) . ? C21 C22 1.39(2) . ? C21 C40 1.48(2) . ? C22 C23 1.35(3) . ? C23 C24 1.37(3) . ? C24 C25 1.41(2) . ? C25 C26 1.47(3) . ? C27 C28 1.48(2) . ? C29 C30 1.48(2) . ? C31 C32 1.42(3) . ? C33 C34 1.47(2) . ? C35 C36 1.50(2) . ? C36 C37 1.36(2) . ? C37 C38 1.37(3) . ? C38 C39 1.35(3) . ? C39 C40 1.41(2) . ? Cl4 O44 1.15(3) . ? Cl4 O43 1.34(4) . ? Cl4 O42 1.45(5) . ? Cl4 O41 1.65(2) . ? 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 N4 Cu1 N3 84.7(5) . . ? N4 Cu1 N5 83.5(5) . . ? N3 Cu1 N5 168.2(5) . . ? N4 Cu1 N1 161.9(5) . . ? N3 Cu1 N1 93.9(5) . . ? N5 Cu1 N1 96.8(4) . . ? N4 Cu1 N7 123.8(5) . . ? N3 Cu1 N7 94.8(5) . . ? N5 Cu1 N7 92.9(4) . . ? N1 Cu1 N7 74.3(5) . . ? N4 Cu1 N2 87.5(5) . . ? N3 Cu1 N2 76.7(6) . . ? N5 Cu1 N2 101.4(5) . . ? N1 Cu1 N2 74.7(5) . . ? N7 Cu1 N2 147.1(5) . . ? N11 Cu2 N10 84.7(5) . . ? N11 Cu2 N8 172.9(6) . . ? N10 Cu2 N8 90.9(5) . . ? N11 Cu2 N12 82.2(6) . . ? N10 Cu2 N12 166.3(6) . . ? N8 Cu2 N12 101.8(5) . . ? N11 Cu2 N9 96.9(6) . . ? N10 Cu2 N9 79.6(5) . . ? N8 Cu2 N9 76.8(6) . . ? N12 Cu2 N9 98.0(6) . . ? N11 Cu2 N14 112.8(5) . . ? N10 Cu2 N14 95.5(5) . . ? N8 Cu2 N14 73.1(5) . . ? N12 Cu2 N14 93.2(5) . . ? N9 Cu2 N14 149.4(5) . . ? C5 N1 C1 119.9(14) . . ? C5 N1 Cu1 120.7(10) . . ? C1 N1 Cu1 119.4(11) . . ? C7 N2 C6 112.0(15) . . ? C7 N2 Cu1 107.5(11) . . ? C6 N2 Cu1 101.4(11) . . ? C8 N3 C9 114.1(13) . . ? C8 N3 Cu1 111.8(11) . . ? C9 N3 Cu1 106.9(10) . . ? C10 N4 C11 119.3(14) . . ? C10 N4 Cu1 111.9(10) . . ? C11 N4 Cu1 109.3(10) . . ? C12 N5 C13 111.3(13) . . ? C12 N5 Cu1 108.2(9) . . ? C13 N5 Cu1 117.0(9) . . ? C15 N6 C14 113.1(19) . . ? C20 N7 C16 119.2(14) . . ? C20 N7 Cu1 111.7(11) . . ? C16 N7 Cu1 129.1(11) . . ? C21 N8 C25 120.7(16) . . ? C21 N8 Cu2 122.2(10) . . ? C25 N8 Cu2 117.0(14) . . ? C26 N9 C27 116.6(17) . . ? C26 N9 Cu2 102.1(13) . . ? C27 N9 Cu2 103.1(10) . . ? C29 N10 C28 114.4(14) . . ? C29 N10 Cu2 107.8(10) . . ? C28 N10 Cu2 111.3(9) . . ? C31 N11 C30 119.2(16) . . ? C31 N11 Cu2 109.4(13) . . ? C30 N11 Cu2 109.2(10) . . ? C33 N12 C32 114.1(15) . . ? C33 N12 Cu2 116.9(11) . . ? C32 N12 Cu2 106.5(11) . . ? C34 N13 C35 112.3(16) . . ? C40 N14 C36 117.3(14) . . ? C40 N14 Cu2 106.6(10) . . ? C36 N14 Cu2 134.2(11) . . ? O14 Cl1 O12 108(2) . . ? O14 Cl1 O13 99(2) . . ? O12 Cl1 O13 117.8(18) . . ? O14 Cl1 O11 110.2(12) . . ? O12 Cl1 O11 104.6(14) . . ? O13 Cl1 O11 116.1(12) . . ? O22 Cl2 O21 118.2(14) . . ? O22 Cl2 O23 115.6(16) . . ? O21 Cl2 O23 106.5(14) . . ? O22 Cl2 O24 105.0(19) . . ? O21 Cl2 O24 112.2(18) . . ? O23 Cl2 O24 97.4(18) . . ? O32 Cl3 O34 106(2) . . ? O32 Cl3 O33 112.0(19) . . ? O34 Cl3 O33 108(2) . . ? O32 Cl3 O31 107.1(14) . . ? O34 Cl3 O31 110.2(15) . . ? O33 Cl3 O31 113.4(11) . . ? N1 C1 C2 119.3(18) . . ? N1 C1 C20 116.8(15) . . ? C2 C1 C20 123.7(18) . . ? C3 C2 C1 120(2) . . ? C2 C3 C4 120(2) . . ? C5 C4 C3 119(2) . . ? N1 C5 C4 121.6(17) . . ? N1 C5 C6 116.6(15) . . ? C4 C5 C6 121.8(19) . . ? N2 C6 C5 116.2(14) . . ? N2 C7 C8 110.5(15) . . ? N3 C8 C7 112.9(13) . . ? N3 C9 C10 112.7(13) . . ? N4 C10 C9 107.1(14) . . ? N4 C11 C12 114.3(14) . . ? N5 C12 C11 115.7(13) . . ? N5 C13 C14 116.1(15) . . ? N6 C14 C13 116.4(15) . . ? N6 C15 C16 118.8(15) . . ? N7 C16 C17 122(2) . . ? N7 C16 C15 118.6(15) . . ? C17 C16 C15 120(2) . . ? C18 C17 C16 119(2) . . ? C17 C18 C19 123(2) . . ? C18 C19 C20 114.5(19) . . ? N7 C20 C19 122.4(18) . . ? N7 C20 C1 116.9(14) . . ? C19 C20 C1 120.4(18) . . ? N8 C21 C22 121.0(16) . . ? N8 C21 C40 117.2(14) . . ? C22 C21 C40 121.8(18) . . ? C23 C22 C21 119(2) . . ? C22 C23 C24 121(2) . . ? C23 C24 C25 117(2) . . ? N8 C25 C24 121(2) . . ? N8 C25 C26 120.2(18) . . ? C24 C25 C26 119(2) . . ? N9 C26 C25 113.3(18) . . ? N9 C27 C28 114.4(15) . . ? N10 C28 C27 112.8(14) . . ? N10 C29 C30 111.0(14) . . ? N11 C30 C29 109.6(14) . . ? N11 C31 C32 118.8(18) . . ? C31 C32 N12 112.4(16) . . ? N12 C33 C34 117.6(15) . . ? N13 C34 C33 119.1(17) . . ? N13 C35 C36 121.5(15) . . ? N14 C36 C37 124.2(18) . . ? N14 C36 C35 118.9(16) . . ? C37 C36 C35 116.9(19) . . ? C36 C37 C38 117(2) . . ? C39 C38 C37 121(2) . . ? C38 C39 C40 119(2) . . ? N14 C40 C39 121.5(19) . . ? N14 C40 C21 117.2(15) . . ? C39 C40 C21 121.2(19) . . ? O44 Cl4 O43 111(3) . . ? O44 Cl4 O42 111(4) . . ? O43 Cl4 O42 107(3) . . ? O44 Cl4 O41 108(3) . . ? O43 Cl4 O41 95(3) . . ? O42 Cl4 O41 123(3) . . ? _diffrn_measured_fraction_theta_max 0.775 _diffrn_reflns_theta_full 24.01 _diffrn_measured_fraction_theta_full 0.775 _refine_diff_density_max 0.640 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.106 #===END data_[NiL1](ClO4)2 _database_code_CSD 199215 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (C20 H31 N7 Ni 2+), (Cl O4 -1)2 ; _chemical_formula_sum 'C20 H31 Cl2 N7 Ni O8' _chemical_formula_weight 627.13 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7484(6) _cell_length_b 11.2278(6) _cell_length_c 19.6420(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.359(2) _cell_angle_gamma 90.00 _cell_volume 2579.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 35 _cell_measurement_theta_min 20 _cell_measurement_theta_max 40 _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 3.520 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 0.70 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'crossed Gobels mirrors' _diffrn_measurement_device_type 'Bruker CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7612 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 53.19 _reflns_number_total 2762 _reflns_number_gt 2355 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart\Bruker CCD' _computing_cell_refinement 'Saint\Bruker CCD' _computing_data_reduction 'Saint\Bruker CCD' _computing_structure_solution 'SIR97 (Altomare 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 Ver. 1.01\b (Farrugia, 1997)' _computing_publication_material 'PARST93 (Nardelli, 1993)' _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^)+(0.0748P)^2^+9.3136P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2762 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.1852 _refine_ls_wR_factor_gt 0.1772 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.003 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 0.29043(10) 0.26097(11) 0.09856(6) 0.0369(5) Uani 1 1 d . . . N7 N 0.2153(5) 0.2077(6) -0.0099(3) 0.0365(16) Uani 1 1 d . . . C16 C 0.2106(6) 0.1043(8) -0.0426(4) 0.042(2) Uani 1 1 d . . . C17 C 0.1649(7) 0.0931(9) -0.1096(5) 0.058(2) Uani 1 1 d . . . H17 H 0.1649 0.0192 -0.1310 0.069 Uiso 1 1 calc R . . C18 C 0.1200(8) 0.1891(11) -0.1446(5) 0.067(3) Uani 1 1 d . . . H18 H 0.0892 0.1824 -0.1898 0.080 Uiso 1 1 calc R . . C19 C 0.1216(7) 0.2976(10) -0.1106(5) 0.059(3) Uani 1 1 d . . . H19 H 0.0906 0.3651 -0.1327 0.071 Uiso 1 1 calc R . . C20 C 0.1698(6) 0.3048(8) -0.0435(4) 0.043(2) Uani 1 1 d . . . N1 N 0.2056(5) 0.4087(5) 0.0616(3) 0.0390(16) Uani 1 1 d . . . C1 C 0.1710(6) 0.4175(7) -0.0049(5) 0.044(2) Uani 1 1 d . . . C2 C 0.1375(8) 0.5258(9) -0.0338(5) 0.071(3) Uani 1 1 d . . . H2 H 0.1149 0.5317 -0.0804 0.086 Uiso 1 1 calc R . . C3 C 0.1385(9) 0.6238(9) 0.0074(7) 0.084(4) Uani 1 1 d . . . H3 H 0.1156 0.6970 -0.0113 0.101 Uiso 1 1 calc R . . C4 C 0.1725(8) 0.6160(8) 0.0760(6) 0.066(3) Uani 1 1 d . . . H4 H 0.1730 0.6823 0.1044 0.079 Uiso 1 1 calc R . . C5 C 0.2062(7) 0.5045(7) 0.1012(5) 0.050(2) Uani 1 1 d . . . C6 C 0.2457(8) 0.4823(8) 0.1740(5) 0.061(3) Uani 1 1 d . . . H6A H 0.2713 0.5564 0.1958 0.073 Uiso 1 1 calc R . . H6B H 0.1831 0.4514 0.1976 0.073 Uiso 1 1 calc R . . N2 N 0.3398(6) 0.3962(6) 0.1783(3) 0.0491(18) Uani 1 1 d . . . H2A H 0.3463 0.3611 0.2202 0.059 Uiso 1 1 calc R . . C7 C 0.4498(8) 0.4475(8) 0.1646(4) 0.057(2) Uani 1 1 d . . . H7A H 0.5102 0.4085 0.1934 0.068 Uiso 1 1 calc R . . H7B H 0.4506 0.5313 0.1765 0.068 Uiso 1 1 calc R . . C8 C 0.4738(7) 0.4345(8) 0.0900(5) 0.057(3) Uani 1 1 d . . . H8A H 0.4265 0.4898 0.0619 0.069 Uiso 1 1 calc R . . H8B H 0.5533 0.4532 0.0853 0.069 Uiso 1 1 calc R . . N3 N 0.4490(5) 0.3115(6) 0.0668(3) 0.0466(18) Uani 1 1 d . . . H3A H 0.4426 0.3115 0.0203 0.056 Uiso 1 1 calc R . . C9 C 0.5339(7) 0.2219(8) 0.0902(5) 0.063(3) Uani 1 1 d . . . H9A H 0.6086 0.2592 0.0969 0.075 Uiso 1 1 calc R . . H9B H 0.5368 0.1613 0.0553 0.075 Uiso 1 1 calc R . . C10 C 0.5076(7) 0.1638(8) 0.1561(5) 0.062(3) Uani 1 1 d . . . H10A H 0.5541 0.0931 0.1648 0.074 Uiso 1 1 calc R . . H10B H 0.5231 0.2184 0.1941 0.074 Uiso 1 1 calc R . . N4 N 0.3867(5) 0.1323(6) 0.1480(4) 0.0503(19) Uani 1 1 d . . . H4A H 0.3825 0.0696 0.1185 0.060 Uiso 1 1 calc R . . C11 C 0.3354(8) 0.0872(9) 0.2093(5) 0.068(3) Uani 1 1 d . . . H11A H 0.3805 0.1149 0.2501 0.081 Uiso 1 1 calc R . . H11B H 0.3374 0.0008 0.2094 0.081 Uiso 1 1 calc R . . C12 C 0.2141(9) 0.1282(9) 0.2108(5) 0.069(3) Uani 1 1 d . . . H12A H 0.1689 0.0620 0.2251 0.083 Uiso 1 1 calc R . . H12B H 0.2123 0.1902 0.2451 0.083 Uiso 1 1 calc R . . N5 N 0.1598(5) 0.1744(5) 0.1455(3) 0.0412(16) Uani 1 1 d . . . H5 H 0.1118 0.2332 0.1570 0.049 Uiso 1 1 calc R . . C13 C 0.0868(7) 0.0880(8) 0.1046(5) 0.058(2) Uani 1 1 d . . . H13A H 0.0609 0.1251 0.0613 0.069 Uiso 1 1 calc R . . H13B H 0.0197 0.0723 0.1285 0.069 Uiso 1 1 calc R . . C14 C 0.1413(8) -0.0287(8) 0.0901(5) 0.067(3) Uani 1 1 d . . . H14A H 0.1491 -0.0747 0.1321 0.081 Uiso 1 1 calc R . . H14B H 0.0896 -0.0720 0.0575 0.081 Uiso 1 1 calc R . . N6 N 0.2514(6) -0.0232(6) 0.0637(4) 0.0504(18) Uani 1 1 d . . . H6A' H 0.2903 0.0375 0.0847 0.060 Uiso 1 1 calc R . . H6B' H 0.2893 -0.0906 0.0763 0.060 Uiso 0.00 1 calc PR . . C15 C 0.2559(8) -0.0086(8) -0.0093(5) 0.064(3) Uani 1 1 d . . . H15A H 0.2144 -0.0745 -0.0319 0.076 Uiso 1 1 calc R . . H15B H 0.3351 -0.0165 -0.0188 0.076 Uiso 1 1 calc R . . Cl1 Cl 0.48324(17) 0.20170(18) -0.12257(11) 0.0485(6) Uani 1 1 d . . . O11 O 0.4139(10) 0.1617(10) -0.1787(5) 0.155(4) Uani 1 1 d . . . O12 O 0.5899(7) 0.2275(8) -0.1423(7) 0.174(5) Uani 1 1 d . . . O13 O 0.4255(7) 0.2995(6) -0.0984(4) 0.103(3) Uani 1 1 d . . . O14 O 0.4890(6) 0.1066(6) -0.0750(4) 0.092(2) Uani 1 1 d . . . Cl2 Cl -0.13339(19) 0.2810(2) 0.20261(13) 0.0633(7) Uani 1 1 d . . . O21 O -0.0358(6) 0.3490(7) 0.1916(4) 0.094(2) Uani 1 1 d . . . O22 O -0.2278(10) 0.3666(14) 0.1976(9) 0.147(6) Uani 0.75 1 d P . . O23 O -0.1690(8) 0.2150(8) 0.1459(5) 0.099(4) Uani 0.75 1 d P . . O24 O -0.0842(13) 0.1825(14) 0.2451(8) 0.151(6) Uani 0.75 1 d P . . O25 O -0.168(3) 0.293(2) 0.2644(12) 0.247(14) Uani 0.75 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 0.0361(7) 0.0432(8) 0.0306(8) 0.0068(6) -0.0004(6) 0.0026(6) N7 0.028(3) 0.042(4) 0.040(4) -0.008(3) 0.004(3) -0.005(3) C16 0.038(4) 0.058(6) 0.030(5) -0.012(4) 0.001(4) -0.011(4) C17 0.049(5) 0.074(7) 0.051(7) -0.009(5) 0.007(5) -0.017(5) C18 0.058(6) 0.117(10) 0.023(6) -0.018(6) -0.011(5) -0.015(6) C19 0.041(5) 0.106(8) 0.030(6) 0.013(5) -0.005(4) -0.007(5) C20 0.030(4) 0.055(6) 0.043(6) 0.010(4) 0.002(4) -0.005(4) N1 0.049(4) 0.030(4) 0.038(5) 0.004(3) 0.006(3) 0.004(3) C1 0.037(5) 0.043(5) 0.050(6) 0.012(4) 0.002(4) 0.002(4) C2 0.087(7) 0.059(7) 0.063(7) 0.019(6) -0.017(6) 0.015(6) C3 0.087(8) 0.044(7) 0.118(11) 0.031(7) -0.012(7) 0.011(6) C4 0.073(7) 0.035(6) 0.092(9) 0.003(5) 0.014(6) 0.007(5) C5 0.060(6) 0.036(6) 0.056(7) 0.004(5) 0.015(5) 0.002(4) C6 0.088(7) 0.040(5) 0.057(7) -0.017(4) 0.019(5) 0.010(5) N2 0.074(5) 0.047(4) 0.026(4) -0.003(3) 0.005(3) 0.004(4) C7 0.072(6) 0.044(5) 0.051(7) -0.015(4) -0.011(5) -0.009(5) C8 0.054(5) 0.053(6) 0.067(7) -0.002(5) 0.015(5) -0.021(5) N3 0.037(4) 0.064(5) 0.039(4) -0.010(3) 0.002(3) -0.003(4) C9 0.050(5) 0.072(7) 0.067(8) -0.026(5) 0.013(5) 0.000(5) C10 0.047(5) 0.051(6) 0.080(8) -0.014(5) -0.033(5) 0.013(5) N4 0.048(4) 0.041(4) 0.058(5) 0.001(4) -0.011(4) 0.005(3) C11 0.085(7) 0.074(7) 0.041(6) 0.017(5) -0.013(5) 0.003(6) C12 0.096(8) 0.070(7) 0.044(7) 0.022(5) 0.017(5) -0.005(6) N5 0.046(4) 0.035(4) 0.044(5) 0.007(3) 0.013(3) 0.006(3) C13 0.044(5) 0.056(6) 0.077(7) -0.002(5) 0.023(5) -0.005(5) C14 0.084(7) 0.042(6) 0.080(8) -0.007(5) 0.030(6) -0.008(5) N6 0.057(4) 0.050(5) 0.043(5) -0.016(3) 0.000(4) 0.002(4) C15 0.065(6) 0.043(6) 0.082(9) -0.022(5) 0.006(5) 0.006(5) Cl1 0.0525(13) 0.0486(14) 0.0451(15) 0.0026(10) 0.0078(10) 0.0035(10) O11 0.197(10) 0.180(10) 0.075(6) -0.031(6) -0.055(7) 0.017(8) O12 0.087(6) 0.118(8) 0.332(16) 0.082(9) 0.103(8) 0.023(6) O13 0.134(7) 0.062(5) 0.122(7) -0.003(4) 0.060(5) 0.017(5) O14 0.111(6) 0.085(5) 0.083(5) 0.038(4) 0.021(4) 0.013(4) Cl2 0.0565(14) 0.0738(18) 0.0594(18) -0.0135(13) 0.0049(12) -0.0091(13) O21 0.072(5) 0.103(6) 0.105(6) 0.026(5) -0.006(4) -0.017(4) O22 0.087(8) 0.160(13) 0.196(16) -0.084(12) 0.023(9) 0.031(8) O23 0.097(7) 0.091(7) 0.102(8) -0.075(6) -0.033(6) 0.011(6) O24 0.158(12) 0.156(12) 0.130(12) 0.081(11) -0.022(10) -0.061(11) O25 0.36(3) 0.25(3) 0.164(18) -0.081(18) 0.18(2) -0.12(2) _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 = -.13471( .00200) m2 = -.52508( .00196) m3 = -.84033( .00121) D = -3.68741( .00670) Atom d s d/s (d/s)**2 N1 * -.0445 .0058 -7.680 58.983 N3 * .0591 .0061 9.659 93.298 N4 * -.1002 .0075 -13.341 177.991 N5 * .0512 .0058 8.833 78.014 Ni1 .0939 .0012 78.823 6213.108 #=========== Sum((d/s)**2) for starred atoms 408.286 Chi-squared at 95% for 1 degrees of freedom: 3.84 The group of atoms deviates significantly from planarity Plane 2 m1 = .94628( .00182) m2 = .23151( .00355) m3 = -.22573( .00502) D = 2.98163( .01012) Atom d s d/s (d/s)**2 N7 * .0127 .0059 2.135 4.559 N1 * -.0125 .0059 -2.117 4.481 C20 * -.0341 .0072 -4.708 22.165 C1 * .0348 .0073 4.758 22.640 #=========== Sum((d/s)**2) for starred atoms 53.845 Chi-squared at 95% for 1 degrees of freedom: 3.84 The group of atoms deviates significantly from planarity Plane 3 m1 = .92574( .00111) m2 = .19728( .00324) m3 = -.32261( .00307) D = 2.87352( .00620) Atom d s d/s (d/s)**2 N7 * .0074 .0059 1.251 1.565 C16 * -.0109 .0072 -1.501 2.252 C17 * .0038 .0085 .445 .198 C18 * .0084 .0096 .871 .758 C19 * -.0062 .0086 -.719 .517 C20 * -.0033 .0072 -.456 .208 #=========== Sum((d/s)**2) for starred atoms 5.497 Chi-squared at 95% for 3 degrees of freedom: 7.81 The group of atoms does not deviate significantly from planarity Plane 4 m1 = .96313( .00096) m2 = .19149( .00343) m3 = -.18896( .00335) D = 2.86550( .01773) Atom d s d/s (d/s)**2 N1 * .0031 .0059 .532 .283 C1 * -.0062 .0072 -.855 .730 C2 * .0055 .0095 .575 .331 C3 * .0024 .0108 .225 .050 C4 * -.0044 .0095 -.458 .210 C5 * -.0004 .0083 -.051 .003 #=========== Sum((d/s)**2) for starred atoms 1.607 Chi-squared at 95% for 3 degrees of freedom: 7.81 The group of atoms does not deviate significantly from planarity Dihedral angles formed by LSQ-planes Plane - plane angle (s.u.) angle (s.u.) 1 2 86.60( .29) 93.40( .29) 1 3 87.55( .21) 92.45( .21) 1 4 85.90( .22) 94.10( .22) 2 3 6.01( .31) 173.99( .31) 2 4 3.26( .31) 176.74( .31) 3 4 7.97( .25) 172.03( .25) ; 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 N1 2.034(6) . ? Ni1 N4 2.026(6) . ? Ni1 N5 2.101(6) . ? Ni1 N3 2.097(6) . ? Ni1 N2 2.219(6) . ? Ni1 N7 2.308(6) . ? N7 C16 1.326(9) . ? N7 C20 1.358(10) . ? C16 C17 1.380(12) . ? C16 C15 1.500(12) . ? C17 C18 1.358(13) . ? C18 C19 1.389(13) . ? C19 C20 1.388(11) . ? C20 C1 1.474(12) . ? N1 C1 1.336(10) . ? N1 C5 1.327(10) . ? C1 C2 1.383(12) . ? C2 C3 1.366(14) . ? C3 C4 1.373(14) . ? C4 C5 1.389(12) . ? C5 C6 1.483(12) . ? C6 N2 1.466(10) . ? N2 C7 1.462(10) . ? C7 C8 1.524(12) . ? C8 N3 1.475(10) . ? N3 C9 1.461(11) . ? C9 C10 1.506(13) . ? C10 N4 1.458(10) . ? N4 C11 1.485(11) . ? C11 C12 1.501(13) . ? C12 N5 1.473(10) . ? N5 C13 1.481(10) . ? C13 C14 1.498(12) . ? C14 N6 1.439(11) . ? N6 C15 1.451(11) . ? Cl1 O12 1.376(8) . ? Cl1 O11 1.383(8) . ? Cl1 O13 1.396(7) . ? Cl1 O14 1.416(6) . ? Cl2 O25 1.323(16) . ? Cl2 O23 1.370(8) . ? Cl2 O21 1.410(7) . ? Cl2 O22 1.464(13) . ? Cl2 O24 1.472(13) . ? O22 O25 1.65(3) . ? O24 O25 1.65(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N4 170.3(3) . . ? N1 Ni1 N5 100.4(2) . . ? N4 Ni1 N5 81.8(3) . . ? N1 Ni1 N3 95.3(3) . . ? N4 Ni1 N3 82.2(3) . . ? N5 Ni1 N3 164.0(2) . . ? N1 Ni1 N2 77.3(3) . . ? N4 Ni1 N2 93.0(3) . . ? N5 Ni1 N2 99.2(3) . . ? N3 Ni1 N2 81.0(3) . . ? N1 Ni1 N7 75.5(2) . . ? N4 Ni1 N7 113.9(3) . . ? N5 Ni1 N7 93.0(2) . . ? N3 Ni1 N7 94.0(2) . . ? N2 Ni1 N7 151.8(2) . . ? C16 N7 C20 118.1(7) . . ? C16 N7 Ni1 132.0(5) . . ? C20 N7 Ni1 109.9(5) . . ? N7 C16 C17 122.4(8) . . ? N7 C16 C15 122.1(7) . . ? C17 C16 C15 115.4(8) . . ? C18 C17 C16 120.6(9) . . ? C17 C18 C19 117.7(9) . . ? C20 C19 C18 119.6(9) . . ? N7 C20 C19 121.5(8) . . ? N7 C20 C1 117.1(7) . . ? C19 C20 C1 121.4(8) . . ? C1 N1 C5 119.8(7) . . ? C1 N1 Ni1 120.3(5) . . ? C5 N1 Ni1 118.5(6) . . ? N1 C1 C2 121.1(8) . . ? N1 C1 C20 115.2(7) . . ? C2 C1 C20 123.7(9) . . ? C3 C2 C1 118.6(10) . . ? C4 C3 C2 121.1(9) . . ? C3 C4 C5 117.0(9) . . ? N1 C5 C4 122.5(9) . . ? N1 C5 C6 114.4(7) . . ? C4 C5 C6 123.2(8) . . ? N2 C6 C5 109.4(7) . . ? C6 N2 C7 113.9(7) . . ? C6 N2 Ni1 105.4(5) . . ? C7 N2 Ni1 108.5(5) . . ? N2 C7 C8 112.7(6) . . ? N3 C8 C7 109.7(7) . . ? C9 N3 C8 116.0(6) . . ? C9 N3 Ni1 108.6(5) . . ? C8 N3 Ni1 108.5(5) . . ? N3 C9 C10 112.3(7) . . ? N4 C10 C9 106.8(7) . . ? C10 N4 C11 117.4(7) . . ? C10 N4 Ni1 111.9(5) . . ? C11 N4 Ni1 112.4(5) . . ? N4 C11 C12 111.7(7) . . ? N5 C12 C11 115.2(7) . . ? C13 N5 C12 115.1(7) . . ? C13 N5 Ni1 118.3(5) . . ? C12 N5 Ni1 105.7(5) . . ? N5 C13 C14 116.1(7) . . ? N6 C14 C13 116.5(7) . . ? C15 N6 C14 118.5(7) . . ? N6 C15 C16 118.8(7) . . ? O12 Cl1 O11 109.2(8) . . ? O12 Cl1 O13 114.5(6) . . ? O11 Cl1 O13 104.9(6) . . ? O12 Cl1 O14 110.8(5) . . ? O11 Cl1 O14 105.6(6) . . ? O13 Cl1 O14 111.3(5) . . ? O25 Cl2 O23 134.6(11) . . ? O25 Cl2 O21 114.4(10) . . ? O23 Cl2 O21 111.0(6) . . ? O25 Cl2 O22 72.5(14) . . ? O23 Cl2 O22 97.4(7) . . ? O21 Cl2 O22 104.9(7) . . ? O25 Cl2 O24 72.0(14) . . ? O23 Cl2 O24 97.4(8) . . ? O21 Cl2 O24 102.2(6) . . ? O22 Cl2 O24 141.8(9) . . ? Cl2 O22 O25 49.8(8) . . ? Cl2 O24 O25 49.8(9) . . ? Cl2 O25 O24 58.2(10) . . ? Cl2 O25 O22 57.7(11) . . ? O24 O25 O22 114.4(13) . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 53.19 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.625 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.078 #===END