# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'A Amoroso' 'Santiago Alvarez' 'Peter G Edwards' 'James C. Knight' 'Neha Singh' _publ_contact_author_name 'A Amoroso' _publ_contact_author_email AMOROSOAJ@CF.AC.UK _publ_section_title ; A Novel Bipyridine-based Hexadentate Tripodal Framework with a Strong Preference for Trigonal Prismatic Co-ordination Geometries ; # Attachment '1.cif' data_platon_1 _database_code_depnum_ccdc_archive 'CCDC 755781' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common aja0718 _chemical_melting_point ? _chemical_formula_moiety 'C31 H22 Mn N6 O, 2(Cl O4), H2 O' _chemical_formula_sum 'C31 H24 Cl2 Mn N6 O10' _chemical_formula_weight 766.40 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5618(2) _cell_length_b 15.9279(3) _cell_length_c 19.0219(5) _cell_angle_alpha 92.0290(10) _cell_angle_beta 103.4120(10) _cell_angle_gamma 98.5920(10) _cell_volume 3360.25(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27666 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1564 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 0.885 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54886 _diffrn_reflns_av_R_equivalents 0.1954 _diffrn_reflns_av_sigmaI/netI 0.1929 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.54 _reflns_number_total 15338 _reflns_number_gt 7306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0680P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15338 _refine_ls_number_parameters 903 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1621 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.1885 _refine_ls_wR_factor_gt 0.1613 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 C1 C 1.1011(4) 0.0686(3) 0.8584(2) 0.0230(10) Uani 1 1 d . . . C2 C 1.0352(4) -0.0056(3) 0.8909(2) 0.0214(10) Uani 1 1 d . . . C3 C 1.0938(4) -0.0456(3) 0.9491(2) 0.0270(11) Uani 1 1 d . . . H3 H 1.1762 -0.0260 0.9717 0.032 Uiso 1 1 calc R . . C4 C 1.0308(4) -0.1144(3) 0.9738(2) 0.0308(12) Uani 1 1 d . . . H4 H 1.0710 -0.1444 1.0119 0.037 Uiso 1 1 calc R . . C5 C 0.9093(4) -0.1395(3) 0.9432(2) 0.0284(11) Uani 1 1 d . . . H5 H 0.8650 -0.1870 0.9593 0.034 Uiso 1 1 calc R . . C6 C 0.8533(4) -0.0933(3) 0.8880(2) 0.0232(10) Uani 1 1 d . . . C7 C 0.7224(4) -0.1084(3) 0.8569(2) 0.0223(10) Uani 1 1 d . . . C8 C 0.6419(4) -0.1499(3) 0.8925(3) 0.0355(12) Uani 1 1 d . . . H8 H 0.6706 -0.1724 0.9377 0.043 Uiso 1 1 calc R . . C9 C 0.5196(4) -0.1588(3) 0.8625(3) 0.0394(13) Uani 1 1 d . . . H9 H 0.4631 -0.1879 0.8860 0.047 Uiso 1 1 calc R . . C10 C 0.4818(5) -0.1240(3) 0.7968(3) 0.0413(14) Uani 1 1 d . . . H10 H 0.3983 -0.1286 0.7747 0.050 Uiso 1 1 calc R . . C11 C 0.5660(4) -0.0828(3) 0.7642(3) 0.0331(12) Uani 1 1 d . . . H11 H 0.5388 -0.0587 0.7195 0.040 Uiso 1 1 calc R . . C12 C 1.1159(4) 0.0378(3) 0.7833(2) 0.0255(11) Uani 1 1 d . . . C13 C 1.2271(4) 0.0479(3) 0.7671(3) 0.0310(12) Uani 1 1 d . . . H13 H 1.2977 0.0732 0.8021 0.037 Uiso 1 1 calc R . . C14 C 1.2328(5) 0.0199(3) 0.6985(3) 0.0461(14) Uani 1 1 d . . . H14 H 1.3078 0.0271 0.6853 0.055 Uiso 1 1 calc R . . C15 C 1.1281(5) -0.0187(3) 0.6489(3) 0.0408(13) Uani 1 1 d . . . H15 H 1.1306 -0.0375 0.6014 0.049 Uiso 1 1 calc R . . C16 C 1.0212(4) -0.0291(3) 0.6698(3) 0.0298(11) Uani 1 1 d . . . C17 C 0.9077(4) -0.0765(3) 0.6224(2) 0.0299(11) Uani 1 1 d . . . C18 C 0.9061(5) -0.1262(3) 0.5599(3) 0.0421(14) Uani 1 1 d . . . H18 H 0.9779 -0.1275 0.5440 0.051 Uiso 1 1 calc R . . C19 C 0.7979(5) -0.1736(3) 0.5216(3) 0.0473(15) Uani 1 1 d . . . H19 H 0.7952 -0.2083 0.4794 0.057 Uiso 1 1 calc R . . C20 C 0.6945(5) -0.1701(3) 0.5450(3) 0.0408(14) Uani 1 1 d . . . H20 H 0.6194 -0.2017 0.5193 0.049 Uiso 1 1 calc R . . C21 C 0.7032(4) -0.1193(3) 0.6070(3) 0.0336(12) Uani 1 1 d . . . H21 H 0.6316 -0.1168 0.6229 0.040 Uiso 1 1 calc R . . C22 C 1.0335(4) 0.1449(3) 0.8485(2) 0.0206(10) Uani 1 1 d . . . C23 C 1.0871(4) 0.2251(3) 0.8836(2) 0.0246(11) Uani 1 1 d . . . H23 H 1.1658 0.2333 0.9145 0.030 Uiso 1 1 calc R . . C24 C 1.0227(4) 0.2914(3) 0.8721(2) 0.0286(11) Uani 1 1 d . . . H24 H 1.0568 0.3461 0.8957 0.034 Uiso 1 1 calc R . . C25 C 0.9087(4) 0.2790(3) 0.8264(2) 0.0241(10) Uani 1 1 d . . . H25 H 0.8634 0.3244 0.8185 0.029 Uiso 1 1 calc R . . C26 C 0.8622(4) 0.1989(3) 0.7925(2) 0.0192(10) Uani 1 1 d . . . C27 C 0.7433(4) 0.1794(3) 0.7391(2) 0.0217(10) Uani 1 1 d . . . C28 C 0.6666(4) 0.2378(3) 0.7226(2) 0.0304(12) Uani 1 1 d . . . H28 H 0.6862 0.2925 0.7480 0.036 Uiso 1 1 calc R . . C29 C 0.5603(4) 0.2173(3) 0.6688(3) 0.0359(13) Uani 1 1 d . . . H29 H 0.5060 0.2569 0.6579 0.043 Uiso 1 1 calc R . . C30 C 0.5358(4) 0.1383(3) 0.6319(2) 0.0338(12) Uani 1 1 d . . . H30 H 0.4650 0.1228 0.5940 0.041 Uiso 1 1 calc R . . C31 C 0.6156(4) 0.0820(3) 0.6508(2) 0.0297(11) Uani 1 1 d . . . H31 H 0.5978 0.0274 0.6255 0.036 Uiso 1 1 calc R . . C32 C -0.1317(4) 0.4423(3) 0.6402(2) 0.0221(10) Uani 1 1 d . . . C33 C -0.0739(4) 0.3615(3) 0.6451(2) 0.0200(10) Uani 1 1 d . . . C34 C -0.1326(4) 0.2854(3) 0.6072(2) 0.0248(11) Uani 1 1 d . . . H34 H -0.2110 0.2814 0.5763 0.030 Uiso 1 1 calc R . . C35 C -0.0740(4) 0.2144(3) 0.6154(2) 0.0294(12) Uani 1 1 d . . . H35 H -0.1119 0.1611 0.5904 0.035 Uiso 1 1 calc R . . C36 C 0.0398(4) 0.2234(3) 0.6604(2) 0.0285(11) Uani 1 1 d . . . H36 H 0.0810 0.1759 0.6665 0.034 Uiso 1 1 calc R . . C37 C 0.0940(4) 0.3005(3) 0.6964(2) 0.0210(10) Uani 1 1 d . . . C38 C 0.2143(4) 0.3141(3) 0.7484(2) 0.0211(10) Uani 1 1 d . . . C39 C 0.2925(4) 0.2563(3) 0.7512(2) 0.0299(12) Uani 1 1 d . . . H39 H 0.2719 0.2073 0.7181 0.036 Uiso 1 1 calc R . . C40 C 0.4014(4) 0.2697(3) 0.8028(3) 0.0363(13) Uani 1 1 d . . . H40 H 0.4559 0.2302 0.8057 0.044 Uiso 1 1 calc R . . C41 C 0.4288(4) 0.3415(3) 0.8496(3) 0.0344(13) Uani 1 1 d . . . H41 H 0.5021 0.3520 0.8860 0.041 Uiso 1 1 calc R . . C42 C 0.3483(4) 0.3979(3) 0.8428(2) 0.0283(11) Uani 1 1 d . . . H42 H 0.3677 0.4473 0.8755 0.034 Uiso 1 1 calc R . . C43 C -0.1480(4) 0.4677(3) 0.7159(2) 0.0228(10) Uani 1 1 d . . . C44 C -0.2616(4) 0.4590(3) 0.7293(2) 0.0262(11) Uani 1 1 d . . . H44 H -0.3311 0.4394 0.6915 0.031 Uiso 1 1 calc R . . C45 C -0.2726(4) 0.4792(3) 0.7982(2) 0.0300(12) Uani 1 1 d . . . H45 H -0.3496 0.4727 0.8088 0.036 Uiso 1 1 calc R . . C46 C -0.1680(4) 0.5094(3) 0.8525(2) 0.0285(11) Uani 1 1 d . . . H46 H -0.1733 0.5228 0.9006 0.034 Uiso 1 1 calc R . . C47 C -0.0583(4) 0.5195(3) 0.8352(2) 0.0218(10) Uani 1 1 d . . . C48 C 0.0557(4) 0.5576(3) 0.8870(2) 0.0254(11) Uani 1 1 d . . . C49 C 0.0562(4) 0.6006(3) 0.9522(2) 0.0352(12) Uani 1 1 d . . . H49 H -0.0171 0.6020 0.9664 0.042 Uiso 1 1 calc R . . C50 C 0.1629(5) 0.6407(3) 0.9955(3) 0.0412(14) Uani 1 1 d . . . H50 H 0.1643 0.6720 1.0392 0.049 Uiso 1 1 calc R . . C51 C 0.2685(5) 0.6353(3) 0.9751(2) 0.0367(13) Uani 1 1 d . . . H51 H 0.3439 0.6617 1.0049 0.044 Uiso 1 1 calc R . . C52 C 0.2622(4) 0.5905(3) 0.9103(2) 0.0325(12) Uani 1 1 d . . . H52 H 0.3351 0.5862 0.8965 0.039 Uiso 1 1 calc R . . C53 C -0.0552(4) 0.5136(3) 0.6102(2) 0.0213(10) Uani 1 1 d . . . C54 C -0.1023(4) 0.5487(3) 0.5461(2) 0.0248(11) Uani 1 1 d . . . H54 H -0.1815 0.5274 0.5184 0.030 Uiso 1 1 calc R . . C55 C -0.0328(4) 0.6144(3) 0.5235(2) 0.0264(11) Uani 1 1 d . . . H55 H -0.0652 0.6412 0.4812 0.032 Uiso 1 1 calc R . . C56 C 0.0850(4) 0.6421(3) 0.5622(2) 0.0276(11) Uani 1 1 d . . . H56 H 0.1346 0.6873 0.5467 0.033 Uiso 1 1 calc R . . C57 C 0.1282(4) 0.6018(3) 0.6240(2) 0.0214(10) Uani 1 1 d . . . C58 C 0.2558(4) 0.6230(3) 0.6663(2) 0.0237(11) Uani 1 1 d . . . C59 C 0.3408(4) 0.6802(3) 0.6447(3) 0.0357(13) Uani 1 1 d . . . H59 H 0.3174 0.7111 0.6033 0.043 Uiso 1 1 calc R . . C60 C 0.4598(4) 0.6926(3) 0.6833(3) 0.0442(14) Uani 1 1 d . . . H60 H 0.5189 0.7312 0.6684 0.053 Uiso 1 1 calc R . . C61 C 0.4909(4) 0.6483(3) 0.7432(3) 0.0356(13) Uani 1 1 d . . . H61 H 0.5718 0.6560 0.7712 0.043 Uiso 1 1 calc R . . C62 C 0.4034(4) 0.5928(3) 0.7619(2) 0.0300(11) Uani 1 1 d . . . H62 H 0.4264 0.5617 0.8032 0.036 Uiso 1 1 calc R . . N1 N 0.9168(3) -0.0303(2) 0.86081(17) 0.0208(8) Uani 1 1 d . . . N2 N 0.6848(3) -0.0752(2) 0.79247(18) 0.0244(9) Uani 1 1 d . . . N3 N 1.0137(3) 0.0012(2) 0.73550(19) 0.0243(9) Uani 1 1 d . . . N4 N 0.8058(3) -0.0735(2) 0.64625(19) 0.0288(9) Uani 1 1 d . . . N5 N 0.9233(3) 0.1335(2) 0.80398(17) 0.0196(8) Uani 1 1 d . . . N6 N 0.7170(3) 0.1009(2) 0.70327(18) 0.0247(9) Uani 1 1 d . . . N7 N 0.0377(3) 0.3685(2) 0.68976(17) 0.0198(8) Uani 1 1 d . . . N8 N 0.2441(3) 0.3868(2) 0.79243(18) 0.0227(9) Uani 1 1 d . . . N9 N -0.0478(3) 0.4969(2) 0.76794(17) 0.0188(8) Uani 1 1 d . . . N10 N 0.1591(3) 0.5534(2) 0.86644(19) 0.0262(9) Uani 1 1 d . . . N11 N 0.0576(3) 0.5404(2) 0.64857(17) 0.0189(8) Uani 1 1 d . . . N12 N 0.2857(3) 0.5787(2) 0.72571(18) 0.0264(9) Uani 1 1 d . . . O1 O 1.2146(3) 0.10000(19) 0.90478(16) 0.0320(8) Uani 1 1 d . . . H1 H 1.2524 0.0594 0.9160 0.048 Uiso 1 1 calc R . . O2 O -0.2458(2) 0.41970(19) 0.59179(15) 0.0265(7) Uani 1 1 d . . . H2 H -0.2781 0.4634 0.5837 0.040 Uiso 1 1 calc R . . O3 O 0.6115(4) 0.1319(3) 0.9748(2) 0.0819(15) Uani 1 1 d . . . O4 O 0.5290(3) 0.0936(2) 0.8496(2) 0.0638(13) Uani 1 1 d . . . O5 O 0.7318(3) 0.0921(2) 0.89828(18) 0.0454(10) Uani 1 1 d . . . O6 O 0.6576(3) 0.2221(2) 0.88798(17) 0.0414(9) Uani 1 1 d . . . O7 O 0.3998(4) 0.3246(3) 0.0118(2) 0.0707(13) Uani 1 1 d . . . O8 O 0.2802(4) 0.3352(2) 0.09455(19) 0.0565(11) Uani 1 1 d . . . O9 O 0.2472(3) 0.4101(2) -0.00959(18) 0.0540(11) Uani 1 1 d . . . O10 O 0.4208(3) 0.4517(2) 0.0832(2) 0.0581(11) Uani 1 1 d . . . O11 O 0.7046(5) 0.0503(3) 0.5037(3) 0.1071(19) Uani 1 1 d . . . O12 O 0.7868(3) 0.1579(2) 0.4462(2) 0.0628(11) Uani 1 1 d . . . O13 O 0.6144(4) 0.1710(3) 0.4837(2) 0.0630(12) Uani 1 1 d . . . O14 O 0.6073(4) 0.0752(3) 0.3874(2) 0.0788(14) Uani 1 1 d . . . O15 O 0.3793(5) 0.3533(3) 0.5575(2) 0.0902(16) Uani 1 1 d . . . O16 O 0.4489(3) 0.4088(2) 0.67835(17) 0.0432(9) Uani 1 1 d . . . O17 O 0.2456(3) 0.4050(3) 0.61876(19) 0.0723(14) Uani 1 1 d . . . O18 O 0.3900(3) 0.4965(2) 0.5840(2) 0.0604(12) Uani 1 1 d . . . O19 O 0.6356(3) 0.5575(2) 0.58376(18) 0.0412(9) Uani 1 1 d . . . H19A H 0.5837 0.5116 0.5714 0.049 Uiso 1 1 d . . . H19B H 0.5935 0.5983 0.5828 0.049 Uiso 1 1 d . . . O20 O 0.3625(3) 0.9838(2) 0.9204(2) 0.0520(10) Uani 1 1 d . . . H20A H 0.4006 1.0333 0.9398 0.062 Uiso 1 1 d . . . H20B H 0.4073 0.9661 0.8945 0.062 Uiso 1 1 d . . . Cl1 Cl 0.63270(10) 0.13358(8) 0.90249(6) 0.0338(3) Uani 1 1 d . . . Cl2 Cl 0.33836(11) 0.38017(8) 0.04450(6) 0.0311(3) Uani 1 1 d . . . Cl3 Cl 0.67356(11) 0.11100(8) 0.45609(6) 0.0350(3) Uani 1 1 d . . . Cl4 Cl 0.36540(10) 0.41331(8) 0.61045(6) 0.0328(3) Uani 1 1 d . . . Mn1 Mn 0.82817(6) 0.00499(4) 0.75148(3) 0.02212(19) Uani 1 1 d . . . Mn2 Mn 0.13852(6) 0.49016(4) 0.75397(3) 0.02015(18) 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 C1 0.021(2) 0.018(2) 0.028(3) 0.005(2) 0.0059(19) -0.004(2) C2 0.022(2) 0.021(2) 0.023(2) 0.003(2) 0.0089(19) 0.005(2) C3 0.024(3) 0.029(3) 0.027(3) 0.001(2) 0.004(2) 0.003(2) C4 0.032(3) 0.030(3) 0.030(3) 0.009(2) 0.004(2) 0.007(2) C5 0.034(3) 0.025(3) 0.028(3) 0.006(2) 0.011(2) 0.005(2) C6 0.034(3) 0.016(2) 0.021(2) 0.003(2) 0.008(2) 0.004(2) C7 0.025(3) 0.017(2) 0.022(2) -0.001(2) 0.0022(19) 0.000(2) C8 0.039(3) 0.030(3) 0.035(3) 0.004(2) 0.009(2) -0.003(2) C9 0.028(3) 0.035(3) 0.058(4) 0.012(3) 0.016(3) 0.001(2) C10 0.030(3) 0.039(3) 0.055(4) 0.008(3) 0.009(3) 0.007(3) C11 0.023(3) 0.031(3) 0.041(3) 0.001(2) -0.001(2) 0.005(2) C12 0.031(3) 0.018(2) 0.029(3) 0.006(2) 0.007(2) 0.007(2) C13 0.029(3) 0.026(3) 0.041(3) 0.004(2) 0.012(2) 0.007(2) C14 0.046(4) 0.039(3) 0.061(4) 0.000(3) 0.025(3) 0.012(3) C15 0.042(3) 0.041(3) 0.043(3) -0.007(3) 0.018(3) 0.009(3) C16 0.036(3) 0.022(3) 0.035(3) 0.002(2) 0.012(2) 0.010(2) C17 0.035(3) 0.024(3) 0.031(3) 0.003(2) 0.006(2) 0.008(2) C18 0.051(4) 0.051(4) 0.029(3) -0.007(3) 0.015(3) 0.016(3) C19 0.056(4) 0.046(4) 0.034(3) -0.017(3) 0.000(3) 0.013(3) C20 0.046(3) 0.041(3) 0.029(3) -0.007(3) -0.004(3) 0.011(3) C21 0.031(3) 0.034(3) 0.036(3) 0.004(2) 0.007(2) 0.008(2) C22 0.022(2) 0.019(2) 0.022(2) 0.003(2) 0.0089(19) -0.002(2) C23 0.026(3) 0.025(3) 0.021(2) 0.005(2) 0.0062(19) -0.004(2) C24 0.035(3) 0.023(3) 0.029(3) -0.002(2) 0.016(2) -0.004(2) C25 0.027(3) 0.021(3) 0.025(2) 0.001(2) 0.009(2) 0.005(2) C26 0.021(2) 0.025(3) 0.016(2) 0.005(2) 0.0121(18) 0.003(2) C27 0.025(2) 0.017(2) 0.025(2) 0.003(2) 0.0112(19) 0.001(2) C28 0.038(3) 0.024(3) 0.032(3) 0.004(2) 0.011(2) 0.009(2) C29 0.037(3) 0.039(3) 0.036(3) 0.015(3) 0.009(2) 0.015(3) C30 0.034(3) 0.044(3) 0.022(3) 0.004(2) 0.003(2) 0.010(3) C31 0.038(3) 0.030(3) 0.020(2) 0.000(2) 0.004(2) 0.006(2) C32 0.016(2) 0.030(3) 0.019(2) -0.001(2) 0.0037(18) 0.001(2) C33 0.017(2) 0.027(3) 0.015(2) 0.000(2) 0.0018(18) 0.004(2) C34 0.027(3) 0.027(3) 0.018(2) 0.002(2) 0.0037(19) 0.000(2) C35 0.038(3) 0.023(3) 0.024(3) 0.001(2) 0.006(2) -0.004(2) C36 0.034(3) 0.023(3) 0.032(3) 0.003(2) 0.015(2) 0.004(2) C37 0.028(3) 0.019(2) 0.019(2) 0.003(2) 0.0102(19) 0.004(2) C38 0.026(3) 0.023(3) 0.016(2) 0.005(2) 0.0104(19) 0.004(2) C39 0.039(3) 0.023(3) 0.031(3) 0.007(2) 0.012(2) 0.010(2) C40 0.039(3) 0.034(3) 0.041(3) 0.021(3) 0.011(3) 0.018(3) C41 0.036(3) 0.042(3) 0.027(3) 0.010(3) 0.006(2) 0.013(3) C42 0.029(3) 0.033(3) 0.018(2) 0.004(2) 0.000(2) 0.000(2) C43 0.023(2) 0.018(2) 0.030(3) 0.006(2) 0.008(2) 0.006(2) C44 0.020(2) 0.028(3) 0.030(3) 0.001(2) 0.006(2) 0.001(2) C45 0.032(3) 0.030(3) 0.034(3) 0.005(2) 0.016(2) 0.009(2) C46 0.036(3) 0.027(3) 0.028(3) 0.002(2) 0.016(2) 0.010(2) C47 0.021(2) 0.023(3) 0.023(2) 0.000(2) 0.0080(19) 0.006(2) C48 0.029(3) 0.025(3) 0.022(2) 0.005(2) 0.004(2) 0.005(2) C49 0.036(3) 0.044(3) 0.026(3) -0.004(2) 0.009(2) 0.004(3) C50 0.048(4) 0.048(3) 0.023(3) -0.008(2) 0.005(2) 0.001(3) C51 0.039(3) 0.038(3) 0.027(3) -0.005(2) 0.001(2) -0.001(3) C52 0.029(3) 0.037(3) 0.027(3) -0.004(2) 0.000(2) 0.004(2) C53 0.022(2) 0.022(2) 0.022(2) 0.001(2) 0.0071(19) 0.006(2) C54 0.022(2) 0.031(3) 0.018(2) -0.003(2) -0.0005(19) 0.006(2) C55 0.027(3) 0.030(3) 0.021(2) 0.010(2) 0.001(2) 0.007(2) C56 0.035(3) 0.023(3) 0.028(3) 0.007(2) 0.012(2) 0.007(2) C57 0.024(2) 0.020(2) 0.021(2) -0.001(2) 0.0060(19) 0.006(2) C58 0.026(3) 0.019(2) 0.024(2) 0.004(2) 0.004(2) -0.001(2) C59 0.031(3) 0.032(3) 0.040(3) 0.013(2) 0.002(2) 0.000(2) C60 0.034(3) 0.040(3) 0.049(3) 0.012(3) -0.002(3) -0.005(3) C61 0.025(3) 0.029(3) 0.044(3) -0.006(2) 0.000(2) -0.008(2) C62 0.025(3) 0.036(3) 0.025(3) -0.001(2) -0.001(2) 0.004(2) N1 0.019(2) 0.018(2) 0.023(2) -0.0003(16) 0.0023(16) 0.0012(16) N2 0.022(2) 0.028(2) 0.021(2) -0.0006(17) 0.0017(16) 0.0023(17) N3 0.033(2) 0.015(2) 0.026(2) 0.0022(17) 0.0062(18) 0.0061(18) N4 0.034(2) 0.024(2) 0.027(2) -0.0011(18) 0.0017(18) 0.0067(19) N5 0.020(2) 0.020(2) 0.0197(19) 0.0024(16) 0.0062(15) 0.0011(17) N6 0.025(2) 0.029(2) 0.020(2) -0.0006(17) 0.0037(16) 0.0079(18) N7 0.022(2) 0.017(2) 0.0190(19) 0.0008(16) 0.0060(16) -0.0010(17) N8 0.023(2) 0.024(2) 0.021(2) 0.0067(17) 0.0044(16) 0.0045(17) N9 0.023(2) 0.017(2) 0.0193(19) 0.0003(16) 0.0070(16) 0.0074(16) N10 0.022(2) 0.025(2) 0.029(2) -0.0027(18) 0.0011(17) 0.0062(18) N11 0.020(2) 0.017(2) 0.0199(19) 0.0006(16) 0.0058(15) 0.0009(16) N12 0.024(2) 0.029(2) 0.023(2) -0.0006(17) 0.0019(16) -0.0003(18) O1 0.0217(17) 0.0288(19) 0.0394(19) 0.0036(16) -0.0023(15) -0.0003(15) O2 0.0196(17) 0.0300(18) 0.0231(17) -0.0002(15) -0.0049(13) -0.0011(14) O3 0.116(4) 0.098(4) 0.064(3) 0.049(3) 0.061(3) 0.048(3) O4 0.026(2) 0.037(2) 0.111(3) -0.012(2) -0.014(2) 0.0000(18) O5 0.033(2) 0.049(2) 0.058(2) 0.0092(19) 0.0069(17) 0.0231(19) O6 0.044(2) 0.030(2) 0.044(2) -0.0033(17) 0.0038(17) 0.0004(17) O7 0.114(4) 0.062(3) 0.066(3) 0.011(2) 0.057(3) 0.054(3) O8 0.084(3) 0.043(2) 0.063(3) 0.021(2) 0.048(2) 0.022(2) O9 0.052(2) 0.064(3) 0.036(2) 0.0061(19) -0.0102(18) 0.013(2) O10 0.045(2) 0.059(3) 0.055(2) -0.004(2) -0.0042(19) -0.012(2) O11 0.161(5) 0.074(4) 0.094(4) 0.045(3) 0.025(4) 0.045(4) O12 0.045(2) 0.050(3) 0.093(3) -0.012(2) 0.024(2) -0.003(2) O13 0.080(3) 0.057(3) 0.067(3) -0.001(2) 0.039(2) 0.025(2) O14 0.053(3) 0.118(4) 0.048(3) -0.050(3) -0.012(2) 0.009(3) O15 0.125(4) 0.063(3) 0.075(3) -0.028(3) -0.001(3) 0.039(3) O16 0.032(2) 0.055(2) 0.036(2) 0.0094(18) -0.0057(16) 0.0058(18) O17 0.021(2) 0.141(4) 0.049(2) 0.040(3) 0.0011(17) -0.001(2) O18 0.054(3) 0.067(3) 0.064(3) 0.034(2) 0.017(2) 0.008(2) O19 0.033(2) 0.038(2) 0.051(2) 0.0067(18) 0.0070(17) 0.0079(17) O20 0.037(2) 0.048(2) 0.077(3) 0.016(2) 0.0186(19) 0.0161(19) Cl1 0.0293(7) 0.0385(8) 0.0362(7) 0.0127(6) 0.0093(5) 0.0085(6) Cl2 0.0367(7) 0.0307(7) 0.0255(6) 0.0014(5) 0.0069(5) 0.0053(6) Cl3 0.0398(8) 0.0343(7) 0.0272(7) -0.0040(6) 0.0028(5) 0.0043(6) Cl4 0.0242(6) 0.0432(8) 0.0289(7) 0.0048(6) 0.0032(5) 0.0035(6) Mn1 0.0244(4) 0.0191(4) 0.0215(4) 0.0005(3) 0.0028(3) 0.0034(3) Mn2 0.0205(4) 0.0215(4) 0.0175(4) 0.0005(3) 0.0029(3) 0.0031(3) _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 C1 O1 1.410(5) . ? C1 C22 1.535(6) . ? C1 C2 1.537(6) . ? C1 C12 1.550(6) . ? C2 N1 1.347(5) . ? C2 C3 1.386(5) . ? C3 C4 1.382(6) . ? C3 H3 0.9500 . ? C4 C5 1.381(6) . ? C4 H4 0.9500 . ? C5 C6 1.394(5) . ? C5 H5 0.9500 . ? C6 N1 1.343(5) . ? C6 C7 1.471(6) . ? C7 N2 1.356(5) . ? C7 C8 1.380(6) . ? C8 C9 1.380(6) . ? C8 H8 0.9500 . ? C9 C10 1.388(6) . ? C9 H9 0.9500 . ? C10 C11 1.372(6) . ? C10 H10 0.9500 . ? C11 N2 1.339(5) . ? C11 H11 0.9500 . ? C12 N3 1.349(5) . ? C12 C13 1.378(6) . ? C13 C14 1.383(7) . ? C13 H13 0.9500 . ? C14 C15 1.393(7) . ? C14 H14 0.9500 . ? C15 C16 1.373(6) . ? C15 H15 0.9500 . ? C16 N3 1.350(6) . ? C16 C17 1.487(6) . ? C17 N4 1.363(6) . ? C17 C18 1.399(6) . ? C18 C19 1.385(7) . ? C18 H18 0.9500 . ? C19 C20 1.376(7) . ? C19 H19 0.9500 . ? C20 C21 1.382(6) . ? C20 H20 0.9500 . ? C21 N4 1.337(6) . ? C21 H21 0.9500 . ? C22 N5 1.339(5) . ? C22 C23 1.403(6) . ? C23 C24 1.377(6) . ? C23 H23 0.9500 . ? C24 C25 1.382(6) . ? C24 H24 0.9500 . ? C25 C26 1.381(6) . ? C25 H25 0.9500 . ? C26 N5 1.340(5) . ? C26 C27 1.489(6) . ? C27 N6 1.360(5) . ? C27 C28 1.375(6) . ? C28 C29 1.391(6) . ? C28 H28 0.9500 . ? C29 C30 1.378(7) . ? C29 H29 0.9500 . ? C30 C31 1.379(6) . ? C30 H30 0.9500 . ? C31 N6 1.338(5) . ? C31 H31 0.9500 . ? C32 O2 1.410(5) . ? C32 C33 1.533(6) . ? C32 C53 1.541(6) . ? C32 C43 1.544(6) . ? C33 N7 1.357(5) . ? C33 C34 1.384(6) . ? C34 C35 1.397(6) . ? C34 H34 0.9500 . ? C35 C36 1.377(6) . ? C35 H35 0.9500 . ? C36 C37 1.372(6) . ? C36 H36 0.9500 . ? C37 N7 1.339(5) . ? C37 C38 1.489(6) . ? C38 N8 1.355(5) . ? C38 C39 1.379(6) . ? C39 C40 1.387(6) . ? C39 H39 0.9500 . ? C40 C41 1.374(7) . ? C40 H40 0.9500 . ? C41 C42 1.376(6) . ? C41 H41 0.9500 . ? C42 N8 1.338(5) . ? C42 H42 0.9500 . ? C43 N9 1.346(5) . ? C43 C44 1.383(6) . ? C44 C45 1.377(6) . ? C44 H44 0.9500 . ? C45 C46 1.404(6) . ? C45 H45 0.9500 . ? C46 C47 1.371(6) . ? C46 H46 0.9500 . ? C47 N9 1.355(5) . ? C47 C48 1.480(6) . ? C48 N10 1.351(5) . ? C48 C49 1.394(6) . ? C49 C50 1.365(7) . ? C49 H49 0.9500 . ? C50 C51 1.377(7) . ? C50 H50 0.9500 . ? C51 C52 1.384(6) . ? C51 H51 0.9500 . ? C52 N10 1.326(5) . ? C52 H52 0.9500 . ? C53 N11 1.336(5) . ? C53 C54 1.389(5) . ? C54 C55 1.366(6) . ? C54 H54 0.9500 . ? C55 C56 1.386(6) . ? C55 H55 0.9500 . ? C56 C57 1.386(5) . ? C56 H56 0.9500 . ? C57 N11 1.346(5) . ? C57 C58 1.490(6) . ? C58 N12 1.358(5) . ? C58 C59 1.382(6) . ? C59 C60 1.382(6) . ? C59 H59 0.9500 . ? C60 C61 1.369(6) . ? C60 H60 0.9500 . ? C61 C62 1.360(6) . ? C61 H61 0.9500 . ? C62 N12 1.356(5) . ? C62 H62 0.9500 . ? N1 Mn1 2.227(3) . ? N2 Mn1 2.242(4) . ? N3 Mn1 2.245(4) . ? N4 Mn1 2.263(4) . ? N5 Mn1 2.252(3) . ? N6 Mn1 2.229(3) . ? N7 Mn2 2.259(3) . ? N8 Mn2 2.238(3) . ? N9 Mn2 2.249(3) . ? N10 Mn2 2.278(4) . ? N11 Mn2 2.236(3) . ? N12 Mn2 2.221(4) . ? O1 H1 0.8400 . ? O2 H2 0.8400 . ? O3 Cl1 1.452(4) . ? O4 Cl1 1.423(4) . ? O5 Cl1 1.421(3) . ? O6 Cl1 1.446(3) . ? O7 Cl2 1.425(4) . ? O8 Cl2 1.440(3) . ? O9 Cl2 1.442(3) . ? O10 Cl2 1.428(4) . ? O11 Cl3 1.378(4) . ? O12 Cl3 1.463(4) . ? O13 Cl3 1.408(4) . ? O14 Cl3 1.404(4) . ? O15 Cl4 1.417(4) . ? O16 Cl4 1.433(3) . ? O17 Cl4 1.417(4) . ? O18 Cl4 1.446(4) . ? O19 H19A 0.8605 . ? O19 H19B 0.8649 . ? O20 H20A 0.8665 . ? O20 H20B 0.8627 . ? 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 O1 C1 C22 105.6(3) . . ? O1 C1 C2 110.6(3) . . ? C22 C1 C2 112.8(3) . . ? O1 C1 C12 110.3(4) . . ? C22 C1 C12 108.2(3) . . ? C2 C1 C12 109.2(3) . . ? N1 C2 C3 120.8(4) . . ? N1 C2 C1 117.3(3) . . ? C3 C2 C1 122.0(4) . . ? C4 C3 C2 119.2(4) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 118.4(4) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? N1 C6 C5 121.3(4) . . ? N1 C6 C7 115.7(3) . . ? C5 C6 C7 123.0(4) . . ? N2 C7 C8 121.7(4) . . ? N2 C7 C6 115.9(4) . . ? C8 C7 C6 122.4(4) . . ? C7 C8 C9 120.0(4) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C10 118.0(5) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? C11 C10 C9 119.4(5) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? N2 C11 C10 122.9(4) . . ? N2 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? N3 C12 C13 122.8(4) . . ? N3 C12 C1 115.8(4) . . ? C13 C12 C1 121.4(4) . . ? C12 C13 C14 118.0(5) . . ? C12 C13 H13 121.0 . . ? C14 C13 H13 121.0 . . ? C13 C14 C15 119.7(5) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 118.9(5) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? N3 C16 C15 121.8(5) . . ? N3 C16 C17 116.1(4) . . ? C15 C16 C17 122.1(5) . . ? N4 C17 C18 121.7(4) . . ? N4 C17 C16 115.8(4) . . ? C18 C17 C16 122.3(5) . . ? C19 C18 C17 118.8(5) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C20 C19 C18 119.7(5) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 118.0(5) . . ? C19 C20 H20 121.0 . . ? C21 C20 H20 121.0 . . ? N4 C21 C20 124.3(5) . . ? N4 C21 H21 117.9 . . ? C20 C21 H21 117.9 . . ? N5 C22 C23 120.9(4) . . ? N5 C22 C1 118.2(4) . . ? C23 C22 C1 120.9(4) . . ? C24 C23 C22 118.4(4) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C23 C24 C25 120.4(4) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 118.3(4) . . ? C26 C25 H25 120.9 . . ? C24 C25 H25 120.9 . . ? N5 C26 C25 121.9(4) . . ? N5 C26 C27 115.2(4) . . ? C25 C26 C27 122.9(4) . . ? N6 C27 C28 120.8(4) . . ? N6 C27 C26 116.0(4) . . ? C28 C27 C26 123.1(4) . . ? C27 C28 C29 120.3(5) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 118.5(4) . . ? C30 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? C29 C30 C31 118.8(4) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? N6 C31 C30 122.9(5) . . ? N6 C31 H31 118.5 . . ? C30 C31 H31 118.5 . . ? O2 C32 C33 105.9(3) . . ? O2 C32 C53 109.8(3) . . ? C33 C32 C53 110.5(3) . . ? O2 C32 C43 109.3(3) . . ? C33 C32 C43 108.3(3) . . ? C53 C32 C43 112.8(4) . . ? N7 C33 C34 121.8(4) . . ? N7 C33 C32 116.0(4) . . ? C34 C33 C32 122.1(4) . . ? C33 C34 C35 118.4(4) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? C36 C35 C34 118.7(4) . . ? C36 C35 H35 120.7 . . ? C34 C35 H35 120.7 . . ? C37 C36 C35 120.4(4) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? N7 C37 C36 121.3(4) . . ? N7 C37 C38 115.1(4) . . ? C36 C37 C38 123.5(4) . . ? N8 C38 C39 121.4(4) . . ? N8 C38 C37 116.8(4) . . ? C39 C38 C37 121.8(4) . . ? C38 C39 C40 119.7(5) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C41 C40 C39 118.6(4) . . ? C41 C40 H40 120.7 . . ? C39 C40 H40 120.7 . . ? C40 C41 C42 118.8(4) . . ? C40 C41 H41 120.6 . . ? C42 C41 H41 120.6 . . ? N8 C42 C41 123.3(5) . . ? N8 C42 H42 118.4 . . ? C41 C42 H42 118.4 . . ? N9 C43 C44 121.9(4) . . ? N9 C43 C32 117.4(4) . . ? C44 C43 C32 120.7(4) . . ? C45 C44 C43 119.1(4) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C44 C45 C46 118.9(4) . . ? C44 C45 H45 120.6 . . ? C46 C45 H45 120.6 . . ? C47 C46 C45 119.2(4) . . ? C47 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? N9 C47 C46 121.6(4) . . ? N9 C47 C48 115.2(4) . . ? C46 C47 C48 123.2(4) . . ? N10 C48 C49 121.2(4) . . ? N10 C48 C47 117.1(4) . . ? C49 C48 C47 121.5(4) . . ? C50 C49 C48 119.4(5) . . ? C50 C49 H49 120.3 . . ? C48 C49 H49 120.3 . . ? C49 C50 C51 119.3(5) . . ? C49 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C50 C51 C52 118.5(5) . . ? C50 C51 H51 120.8 . . ? C52 C51 H51 120.8 . . ? N10 C52 C51 123.1(5) . . ? N10 C52 H52 118.5 . . ? C51 C52 H52 118.5 . . ? N11 C53 C54 121.5(4) . . ? N11 C53 C32 117.4(3) . . ? C54 C53 C32 121.1(4) . . ? C55 C54 C53 118.9(4) . . ? C55 C54 H54 120.6 . . ? C53 C54 H54 120.6 . . ? C54 C55 C56 120.2(4) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C55 C56 C57 117.9(4) . . ? C55 C56 H56 121.0 . . ? C57 C56 H56 121.0 . . ? N11 C57 C56 121.9(4) . . ? N11 C57 C58 116.3(3) . . ? C56 C57 C58 121.9(4) . . ? N12 C58 C59 121.6(4) . . ? N12 C58 C57 115.6(4) . . ? C59 C58 C57 122.7(4) . . ? C60 C59 C58 120.0(4) . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C61 C60 C59 118.9(5) . . ? C61 C60 H60 120.6 . . ? C59 C60 H60 120.6 . . ? C62 C61 C60 118.5(4) . . ? C62 C61 H61 120.8 . . ? C60 C61 H61 120.8 . . ? N12 C62 C61 124.7(4) . . ? N12 C62 H62 117.6 . . ? C61 C62 H62 117.6 . . ? C6 N1 C2 120.2(3) . . ? C6 N1 Mn1 115.6(3) . . ? C2 N1 Mn1 122.5(3) . . ? C11 N2 C7 118.0(4) . . ? C11 N2 Mn1 125.5(3) . . ? C7 N2 Mn1 115.8(3) . . ? C12 N3 C16 118.6(4) . . ? C12 N3 Mn1 123.8(3) . . ? C16 N3 Mn1 116.9(3) . . ? C21 N4 C17 117.3(4) . . ? C21 N4 Mn1 126.1(3) . . ? C17 N4 Mn1 116.6(3) . . ? C22 N5 C26 120.2(4) . . ? C22 N5 Mn1 122.5(3) . . ? C26 N5 Mn1 117.2(3) . . ? C31 N6 C27 118.7(4) . . ? C31 N6 Mn1 124.0(3) . . ? C27 N6 Mn1 116.1(3) . . ? C37 N7 C33 119.3(4) . . ? C37 N7 Mn2 116.8(3) . . ? C33 N7 Mn2 123.8(3) . . ? C42 N8 C38 118.0(4) . . ? C42 N8 Mn2 125.0(3) . . ? C38 N8 Mn2 114.8(2) . . ? C43 N9 C47 119.2(4) . . ? C43 N9 Mn2 122.7(3) . . ? C47 N9 Mn2 117.3(3) . . ? C52 N10 C48 118.4(4) . . ? C52 N10 Mn2 125.4(3) . . ? C48 N10 Mn2 116.0(3) . . ? C53 N11 C57 119.4(3) . . ? C53 N11 Mn2 123.8(3) . . ? C57 N11 Mn2 116.8(3) . . ? C62 N12 C58 116.3(4) . . ? C62 N12 Mn2 126.4(3) . . ? C58 N12 Mn2 117.3(3) . . ? C1 O1 H1 109.5 . . ? C32 O2 H2 109.5 . . ? H19A O19 H19B 105.4 . . ? H20A O20 H20B 105.1 . . ? O5 Cl1 O4 109.1(2) . . ? O5 Cl1 O6 110.4(2) . . ? O4 Cl1 O6 108.5(2) . . ? O5 Cl1 O3 110.7(2) . . ? O4 Cl1 O3 111.2(3) . . ? O6 Cl1 O3 106.9(2) . . ? O7 Cl2 O10 110.7(3) . . ? O7 Cl2 O8 109.6(2) . . ? O10 Cl2 O8 108.6(2) . . ? O7 Cl2 O9 110.7(2) . . ? O10 Cl2 O9 109.0(2) . . ? O8 Cl2 O9 108.2(2) . . ? O11 Cl3 O14 112.6(3) . . ? O11 Cl3 O13 113.0(3) . . ? O14 Cl3 O13 111.2(3) . . ? O11 Cl3 O12 106.2(3) . . ? O14 Cl3 O12 106.8(3) . . ? O13 Cl3 O12 106.6(2) . . ? O15 Cl4 O17 112.8(3) . . ? O15 Cl4 O16 110.8(2) . . ? O17 Cl4 O16 111.1(2) . . ? O15 Cl4 O18 106.7(3) . . ? O17 Cl4 O18 105.6(2) . . ? O16 Cl4 O18 109.5(2) . . ? N1 Mn1 N6 138.54(13) . . ? N1 Mn1 N2 73.46(12) . . ? N6 Mn1 N2 96.95(13) . . ? N1 Mn1 N3 80.48(12) . . ? N6 Mn1 N3 122.57(13) . . ? N2 Mn1 N3 139.73(12) . . ? N1 Mn1 N5 79.28(12) . . ? N6 Mn1 N5 72.80(13) . . ? N2 Mn1 N5 123.26(13) . . ? N3 Mn1 N5 79.85(13) . . ? N1 Mn1 N4 125.15(12) . . ? N6 Mn1 N4 95.78(13) . . ? N2 Mn1 N4 97.64(14) . . ? N3 Mn1 N4 72.96(14) . . ? N5 Mn1 N4 138.17(13) . . ? N12 Mn2 N11 73.68(12) . . ? N12 Mn2 N8 97.87(13) . . ? N11 Mn2 N8 137.89(13) . . ? N12 Mn2 N9 136.37(12) . . ? N11 Mn2 N9 79.71(12) . . ? N8 Mn2 N9 124.63(12) . . ? N12 Mn2 N7 126.15(13) . . ? N11 Mn2 N7 79.18(12) . . ? N8 Mn2 N7 73.16(12) . . ? N9 Mn2 N7 80.30(13) . . ? N12 Mn2 N10 96.07(14) . . ? N11 Mn2 N10 126.21(12) . . ? N8 Mn2 N10 95.35(12) . . ? N9 Mn2 N10 72.71(13) . . ? N7 Mn2 N10 136.97(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 166.4(4) . . . . ? C22 C1 C2 N1 48.3(5) . . . . ? C12 C1 C2 N1 -72.0(5) . . . . ? O1 C1 C2 C3 -13.1(6) . . . . ? C22 C1 C2 C3 -131.2(4) . . . . ? C12 C1 C2 C3 108.5(5) . . . . ? N1 C2 C3 C4 3.3(7) . . . . ? C1 C2 C3 C4 -177.2(4) . . . . ? C2 C3 C4 C5 -3.6(7) . . . . ? C3 C4 C5 C6 -0.6(7) . . . . ? C4 C5 C6 N1 5.4(7) . . . . ? C4 C5 C6 C7 -173.3(4) . . . . ? N1 C6 C7 N2 17.6(6) . . . . ? C5 C6 C7 N2 -163.6(4) . . . . ? N1 C6 C7 C8 -159.1(4) . . . . ? C5 C6 C7 C8 19.7(7) . . . . ? N2 C7 C8 C9 0.3(7) . . . . ? C6 C7 C8 C9 176.9(5) . . . . ? C7 C8 C9 C10 -0.8(8) . . . . ? C8 C9 C10 C11 0.3(8) . . . . ? C9 C10 C11 N2 0.7(8) . . . . ? O1 C1 C12 N3 175.9(3) . . . . ? C22 C1 C12 N3 -69.1(4) . . . . ? C2 C1 C12 N3 54.1(4) . . . . ? O1 C1 C12 C13 -4.3(5) . . . . ? C22 C1 C12 C13 110.8(4) . . . . ? C2 C1 C12 C13 -126.1(4) . . . . ? N3 C12 C13 C14 0.8(6) . . . . ? C1 C12 C13 C14 -179.0(4) . . . . ? C12 C13 C14 C15 -1.4(7) . . . . ? C13 C14 C15 C16 -0.8(7) . . . . ? C14 C15 C16 N3 3.7(7) . . . . ? C14 C15 C16 C17 -174.4(4) . . . . ? N3 C16 C17 N4 9.1(6) . . . . ? C15 C16 C17 N4 -172.7(4) . . . . ? N3 C16 C17 C18 -166.4(4) . . . . ? C15 C16 C17 C18 11.8(7) . . . . ? N4 C17 C18 C19 -0.1(7) . . . . ? C16 C17 C18 C19 175.2(4) . . . . ? C17 C18 C19 C20 0.8(7) . . . . ? C18 C19 C20 C21 -0.6(7) . . . . ? C19 C20 C21 N4 -0.4(7) . . . . ? O1 C1 C22 N5 177.4(3) . . . . ? C2 C1 C22 N5 -61.6(5) . . . . ? C12 C1 C22 N5 59.3(5) . . . . ? O1 C1 C22 C23 -0.9(5) . . . . ? C2 C1 C22 C23 120.1(4) . . . . ? C12 C1 C22 C23 -118.9(4) . . . . ? N5 C22 C23 C24 1.1(6) . . . . ? C1 C22 C23 C24 179.3(4) . . . . ? C22 C23 C24 C25 -0.7(6) . . . . ? C23 C24 C25 C26 -0.5(6) . . . . ? C24 C25 C26 N5 1.4(6) . . . . ? C24 C25 C26 C27 -176.5(4) . . . . ? N5 C26 C27 N6 -6.5(5) . . . . ? C25 C26 C27 N6 171.6(4) . . . . ? N5 C26 C27 C28 177.6(4) . . . . ? C25 C26 C27 C28 -4.4(6) . . . . ? N6 C27 C28 C29 0.1(7) . . . . ? C26 C27 C28 C29 175.9(4) . . . . ? C27 C28 C29 C30 -1.4(7) . . . . ? C28 C29 C30 C31 1.7(7) . . . . ? C29 C30 C31 N6 -0.6(7) . . . . ? O2 C32 C33 N7 -179.5(3) . . . . ? C53 C32 C33 N7 61.6(5) . . . . ? C43 C32 C33 N7 -62.4(5) . . . . ? O2 C32 C33 C34 -0.6(5) . . . . ? C53 C32 C33 C34 -119.4(4) . . . . ? C43 C32 C33 C34 116.6(4) . . . . ? N7 C33 C34 C35 -0.4(6) . . . . ? C32 C33 C34 C35 -179.3(4) . . . . ? C33 C34 C35 C36 -0.4(6) . . . . ? C34 C35 C36 C37 0.1(6) . . . . ? C35 C36 C37 N7 1.0(6) . . . . ? C35 C36 C37 C38 177.1(4) . . . . ? N7 C37 C38 N8 11.6(5) . . . . ? C36 C37 C38 N8 -164.7(4) . . . . ? N7 C37 C38 C39 -167.7(4) . . . . ? C36 C37 C38 C39 16.0(6) . . . . ? N8 C38 C39 C40 3.6(6) . . . . ? C37 C38 C39 C40 -177.1(4) . . . . ? C38 C39 C40 C41 -0.5(7) . . . . ? C39 C40 C41 C42 -1.1(7) . . . . ? C40 C41 C42 N8 -0.3(7) . . . . ? O2 C32 C43 N9 -175.5(3) . . . . ? C33 C32 C43 N9 69.6(5) . . . . ? C53 C32 C43 N9 -53.0(5) . . . . ? O2 C32 C43 C44 5.5(5) . . . . ? C33 C32 C43 C44 -109.4(4) . . . . ? C53 C32 C43 C44 128.0(4) . . . . ? N9 C43 C44 C45 -1.4(6) . . . . ? C32 C43 C44 C45 177.5(4) . . . . ? C43 C44 C45 C46 1.2(6) . . . . ? C44 C45 C46 C47 1.1(6) . . . . ? C45 C46 C47 N9 -3.4(6) . . . . ? C45 C46 C47 C48 174.8(4) . . . . ? N9 C47 C48 N10 -10.4(5) . . . . ? C46 C47 C48 N10 171.3(4) . . . . ? N9 C47 C48 C49 165.7(4) . . . . ? C46 C47 C48 C49 -12.6(6) . . . . ? N10 C48 C49 C50 1.3(7) . . . . ? C47 C48 C49 C50 -174.6(4) . . . . ? C48 C49 C50 C51 -2.3(7) . . . . ? C49 C50 C51 C52 1.3(7) . . . . ? C50 C51 C52 N10 0.8(7) . . . . ? O2 C32 C53 N11 -177.7(4) . . . . ? C33 C32 C53 N11 -61.3(5) . . . . ? C43 C32 C53 N11 60.1(5) . . . . ? O2 C32 C53 C54 2.7(6) . . . . ? C33 C32 C53 C54 119.1(4) . . . . ? C43 C32 C53 C54 -119.5(4) . . . . ? N11 C53 C54 C55 -2.6(7) . . . . ? C32 C53 C54 C55 177.0(4) . . . . ? C53 C54 C55 C56 3.5(7) . . . . ? C54 C55 C56 C57 -0.7(7) . . . . ? C55 C56 C57 N11 -3.1(7) . . . . ? C55 C56 C57 C58 175.8(4) . . . . ? N11 C57 C58 N12 -1.1(6) . . . . ? C56 C57 C58 N12 179.9(4) . . . . ? N11 C57 C58 C59 175.2(4) . . . . ? C56 C57 C58 C59 -3.8(7) . . . . ? N12 C58 C59 C60 0.9(8) . . . . ? C57 C58 C59 C60 -175.2(5) . . . . ? C58 C59 C60 C61 -0.8(8) . . . . ? C59 C60 C61 C62 0.9(8) . . . . ? C60 C61 C62 N12 -1.0(8) . . . . ? C5 C6 N1 C2 -5.8(6) . . . . ? C7 C6 N1 C2 173.0(4) . . . . ? C5 C6 N1 Mn1 159.7(3) . . . . ? C7 C6 N1 Mn1 -21.5(5) . . . . ? C3 C2 N1 C6 1.3(6) . . . . ? C1 C2 N1 C6 -178.1(4) . . . . ? C3 C2 N1 Mn1 -163.1(3) . . . . ? C1 C2 N1 Mn1 17.4(5) . . . . ? C10 C11 N2 C7 -1.3(7) . . . . ? C10 C11 N2 Mn1 -171.4(4) . . . . ? C8 C7 N2 C11 0.7(6) . . . . ? C6 C7 N2 C11 -176.0(4) . . . . ? C8 C7 N2 Mn1 171.8(3) . . . . ? C6 C7 N2 Mn1 -4.9(5) . . . . ? C13 C12 N3 C16 1.9(6) . . . . ? C1 C12 N3 C16 -178.2(3) . . . . ? C13 C12 N3 Mn1 -168.2(3) . . . . ? C1 C12 N3 Mn1 11.6(5) . . . . ? C15 C16 N3 C12 -4.2(6) . . . . ? C17 C16 N3 C12 173.9(4) . . . . ? C15 C16 N3 Mn1 166.6(3) . . . . ? C17 C16 N3 Mn1 -15.2(5) . . . . ? C20 C21 N4 C17 1.1(6) . . . . ? C20 C21 N4 Mn1 -176.4(3) . . . . ? C18 C17 N4 C21 -0.8(6) . . . . ? C16 C17 N4 C21 -176.4(4) . . . . ? C18 C17 N4 Mn1 176.9(3) . . . . ? C16 C17 N4 Mn1 1.3(5) . . . . ? C23 C22 N5 C26 -0.3(6) . . . . ? C1 C22 N5 C26 -178.5(3) . . . . ? C23 C22 N5 Mn1 -176.2(3) . . . . ? C1 C22 N5 Mn1 5.5(5) . . . . ? C25 C26 N5 C22 -1.0(6) . . . . ? C27 C26 N5 C22 177.0(4) . . . . ? C25 C26 N5 Mn1 175.1(3) . . . . ? C27 C26 N5 Mn1 -6.8(4) . . . . ? C30 C31 N6 C27 -0.7(6) . . . . ? C30 C31 N6 Mn1 166.6(3) . . . . ? C28 C27 N6 C31 1.0(6) . . . . ? C26 C27 N6 C31 -175.1(4) . . . . ? C28 C27 N6 Mn1 -167.3(3) . . . . ? C26 C27 N6 Mn1 16.6(5) . . . . ? C36 C37 N7 C33 -1.8(6) . . . . ? C38 C37 N7 C33 -178.2(3) . . . . ? C36 C37 N7 Mn2 179.1(3) . . . . ? C38 C37 N7 Mn2 2.7(4) . . . . ? C34 C33 N7 C37 1.5(6) . . . . ? C32 C33 N7 C37 -179.6(3) . . . . ? C34 C33 N7 Mn2 -179.5(3) . . . . ? C32 C33 N7 Mn2 -0.5(5) . . . . ? C41 C42 N8 C38 3.3(6) . . . . ? C41 C42 N8 Mn2 -159.1(3) . . . . ? C39 C38 N8 C42 -4.9(6) . . . . ? C37 C38 N8 C42 175.8(3) . . . . ? C39 C38 N8 Mn2 159.3(3) . . . . ? C37 C38 N8 Mn2 -20.0(4) . . . . ? C44 C43 N9 C47 -0.8(6) . . . . ? C32 C43 N9 C47 -179.7(3) . . . . ? C44 C43 N9 Mn2 168.9(3) . . . . ? C32 C43 N9 Mn2 -10.1(5) . . . . ? C46 C47 N9 C43 3.2(6) . . . . ? C48 C47 N9 C43 -175.1(4) . . . . ? C46 C47 N9 Mn2 -167.0(3) . . . . ? C48 C47 N9 Mn2 14.7(5) . . . . ? C51 C52 N10 C48 -1.8(6) . . . . ? C51 C52 N10 Mn2 173.4(3) . . . . ? C49 C48 N10 C52 0.7(6) . . . . ? C47 C48 N10 C52 176.8(4) . . . . ? C49 C48 N10 Mn2 -175.0(3) . . . . ? C47 C48 N10 Mn2 1.1(5) . . . . ? C54 C53 N11 C57 -1.2(6) . . . . ? C32 C53 N11 C57 179.2(4) . . . . ? C54 C53 N11 Mn2 178.0(3) . . . . ? C32 C53 N11 Mn2 -1.6(5) . . . . ? C56 C57 N11 C53 4.1(6) . . . . ? C58 C57 N11 C53 -174.9(4) . . . . ? C56 C57 N11 Mn2 -175.2(3) . . . . ? C58 C57 N11 Mn2 5.9(5) . . . . ? C61 C62 N12 C58 0.9(7) . . . . ? C61 C62 N12 Mn2 -179.3(4) . . . . ? C59 C58 N12 C62 -0.8(7) . . . . ? C57 C58 N12 C62 175.5(4) . . . . ? C59 C58 N12 Mn2 179.4(4) . . . . ? C57 C58 N12 Mn2 -4.3(5) . . . . ? C6 N1 Mn1 N6 95.7(3) . . . . ? C2 N1 Mn1 N6 -99.2(4) . . . . ? C6 N1 Mn1 N2 14.1(3) . . . . ? C2 N1 Mn1 N2 179.2(4) . . . . ? C6 N1 Mn1 N3 -134.9(3) . . . . ? C2 N1 Mn1 N3 30.2(3) . . . . ? C6 N1 Mn1 N5 143.8(3) . . . . ? C2 N1 Mn1 N5 -51.1(3) . . . . ? C6 N1 Mn1 N4 -73.6(3) . . . . ? C2 N1 Mn1 N4 91.5(4) . . . . ? C31 N6 Mn1 N1 -132.5(3) . . . . ? C27 N6 Mn1 N1 35.1(4) . . . . ? C31 N6 Mn1 N2 -59.7(4) . . . . ? C27 N6 Mn1 N2 107.9(3) . . . . ? C31 N6 Mn1 N3 112.2(3) . . . . ? C27 N6 Mn1 N3 -80.2(3) . . . . ? C31 N6 Mn1 N5 177.6(4) . . . . ? C27 N6 Mn1 N5 -14.8(3) . . . . ? C31 N6 Mn1 N4 38.8(4) . . . . ? C27 N6 Mn1 N4 -153.6(3) . . . . ? C11 N2 Mn1 N1 166.0(4) . . . . ? C7 N2 Mn1 N1 -4.4(3) . . . . ? C11 N2 Mn1 N6 27.3(4) . . . . ? C7 N2 Mn1 N6 -143.1(3) . . . . ? C11 N2 Mn1 N3 -142.2(4) . . . . ? C7 N2 Mn1 N3 47.5(4) . . . . ? C11 N2 Mn1 N5 101.2(4) . . . . ? C7 N2 Mn1 N5 -69.1(3) . . . . ? C11 N2 Mn1 N4 -69.6(4) . . . . ? C7 N2 Mn1 N4 120.1(3) . . . . ? C12 N3 Mn1 N1 -46.5(3) . . . . ? C16 N3 Mn1 N1 143.2(3) . . . . ? C12 N3 Mn1 N6 96.2(3) . . . . ? C16 N3 Mn1 N6 -74.2(3) . . . . ? C12 N3 Mn1 N2 -96.3(4) . . . . ? C16 N3 Mn1 N2 93.3(3) . . . . ? C12 N3 Mn1 N5 34.2(3) . . . . ? C16 N3 Mn1 N5 -136.1(3) . . . . ? C12 N3 Mn1 N4 -177.9(3) . . . . ? C16 N3 Mn1 N4 11.8(3) . . . . ? C22 N5 Mn1 N1 38.5(3) . . . . ? C26 N5 Mn1 N1 -137.6(3) . . . . ? C22 N5 Mn1 N6 -172.5(3) . . . . ? C26 N5 Mn1 N6 11.4(3) . . . . ? C22 N5 Mn1 N2 100.4(3) . . . . ? C26 N5 Mn1 N2 -75.7(3) . . . . ? C22 N5 Mn1 N3 -43.6(3) . . . . ? C26 N5 Mn1 N3 140.3(3) . . . . ? C22 N5 Mn1 N4 -93.3(3) . . . . ? C26 N5 Mn1 N4 90.6(3) . . . . ? C21 N4 Mn1 N1 106.1(3) . . . . ? C17 N4 Mn1 N1 -71.3(3) . . . . ? C21 N4 Mn1 N6 -66.8(4) . . . . ? C17 N4 Mn1 N6 115.7(3) . . . . ? C21 N4 Mn1 N2 31.0(4) . . . . ? C17 N4 Mn1 N2 -146.4(3) . . . . ? C21 N4 Mn1 N3 170.8(4) . . . . ? C17 N4 Mn1 N3 -6.6(3) . . . . ? C21 N4 Mn1 N5 -137.4(3) . . . . ? C17 N4 Mn1 N5 45.1(4) . . . . ? C62 N12 Mn2 N11 -174.3(4) . . . . ? C58 N12 Mn2 N11 5.4(3) . . . . ? C62 N12 Mn2 N8 -36.6(4) . . . . ? C58 N12 Mn2 N8 143.1(3) . . . . ? C62 N12 Mn2 N9 130.9(4) . . . . ? C58 N12 Mn2 N9 -49.3(4) . . . . ? C62 N12 Mn2 N7 -111.5(4) . . . . ? C58 N12 Mn2 N7 68.3(3) . . . . ? C62 N12 Mn2 N10 59.7(4) . . . . ? C58 N12 Mn2 N10 -120.6(3) . . . . ? C53 N11 Mn2 N12 174.8(4) . . . . ? C57 N11 Mn2 N12 -6.0(3) . . . . ? C53 N11 Mn2 N8 91.2(4) . . . . ? C57 N11 Mn2 N8 -89.6(3) . . . . ? C53 N11 Mn2 N9 -40.1(3) . . . . ? C57 N11 Mn2 N9 139.1(3) . . . . ? C53 N11 Mn2 N7 41.8(3) . . . . ? C57 N11 Mn2 N7 -139.0(3) . . . . ? C53 N11 Mn2 N10 -99.7(3) . . . . ? C57 N11 Mn2 N10 79.5(3) . . . . ? C42 N8 Mn2 N12 53.1(4) . . . . ? C38 N8 Mn2 N12 -109.9(3) . . . . ? C42 N8 Mn2 N11 127.4(3) . . . . ? C38 N8 Mn2 N11 -35.5(4) . . . . ? C42 N8 Mn2 N9 -116.5(3) . . . . ? C38 N8 Mn2 N9 80.6(3) . . . . ? C42 N8 Mn2 N7 178.5(4) . . . . ? C38 N8 Mn2 N7 15.6(3) . . . . ? C42 N8 Mn2 N10 -43.9(4) . . . . ? C38 N8 Mn2 N10 153.2(3) . . . . ? C43 N9 Mn2 N12 99.2(3) . . . . ? C47 N9 Mn2 N12 -91.0(3) . . . . ? C43 N9 Mn2 N11 46.4(3) . . . . ? C47 N9 Mn2 N11 -143.8(3) . . . . ? C43 N9 Mn2 N8 -95.9(3) . . . . ? C47 N9 Mn2 N8 73.9(3) . . . . ? C43 N9 Mn2 N7 -34.3(3) . . . . ? C47 N9 Mn2 N7 135.5(3) . . . . ? C43 N9 Mn2 N10 179.6(3) . . . . ? C47 N9 Mn2 N10 -10.6(3) . . . . ? C37 N7 Mn2 N12 77.9(3) . . . . ? C33 N7 Mn2 N12 -101.2(3) . . . . ? C37 N7 Mn2 N11 138.3(3) . . . . ? C33 N7 Mn2 N11 -40.8(3) . . . . ? C37 N7 Mn2 N8 -9.6(3) . . . . ? C33 N7 Mn2 N8 171.4(3) . . . . ? C37 N7 Mn2 N9 -140.4(3) . . . . ? C33 N7 Mn2 N9 40.5(3) . . . . ? C37 N7 Mn2 N10 -89.1(3) . . . . ? C33 N7 Mn2 N10 91.8(3) . . . . ? C52 N10 Mn2 N12 -33.9(4) . . . . ? C48 N10 Mn2 N12 141.5(3) . . . . ? C52 N10 Mn2 N11 -108.1(4) . . . . ? C48 N10 Mn2 N11 67.3(3) . . . . ? C52 N10 Mn2 N8 64.7(4) . . . . ? C48 N10 Mn2 N8 -120.0(3) . . . . ? C52 N10 Mn2 N9 -170.7(4) . . . . ? C48 N10 Mn2 N9 4.7(3) . . . . ? C52 N10 Mn2 N7 135.6(3) . . . . ? C48 N10 Mn2 N7 -49.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.603 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.111 # Attachment '2.cif' data_aja0711 _database_code_depnum_ccdc_archive 'CCDC 755782' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common aja0711 _chemical_melting_point ? _chemical_formula_moiety '2(C31 H22 Fe N6 O), C2 H3 N, 4(Cl O4)' _chemical_formula_sum 'C64 H47 Cl4 Fe2 N13 O18' _chemical_formula_weight 1539.65 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.4113(3) _cell_length_b 13.4325(3) _cell_length_c 20.8164(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.8420(10) _cell_angle_gamma 90.00 _cell_volume 3174.21(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19049 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1572 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7887 _exptl_absorpt_correction_T_max 0.8202 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36044 _diffrn_reflns_av_R_equivalents 0.1471 _diffrn_reflns_av_sigmaI/netI 0.1290 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.45 _reflns_number_total 7223 _reflns_number_gt 3548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0878P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7223 _refine_ls_number_parameters 469 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1634 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1891 _refine_ls_wR_factor_gt 0.1543 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 C1 C 0.3041(4) 0.2378(4) -0.0412(2) 0.0470(12) Uani 1 1 d . . . C2 C 0.1860(4) 0.2706(3) -0.0179(2) 0.0456(11) Uani 1 1 d . . . C3 C 0.1098(5) 0.3335(4) -0.0548(3) 0.0631(15) Uani 1 1 d . . . H3 H 0.1269 0.3538 -0.0965 0.076 Uiso 1 1 calc R . . C4 C 0.0103(5) 0.3658(5) -0.0305(3) 0.0728(17) Uani 1 1 d . . . H4 H -0.0409 0.4111 -0.0545 0.087 Uiso 1 1 calc R . . C5 C -0.0165(4) 0.3322(4) 0.0299(3) 0.0623(15) Uani 1 1 d . . . H5 H -0.0853 0.3543 0.0478 0.075 Uiso 1 1 calc R . . C6 C 0.0600(4) 0.2659(4) 0.0625(2) 0.0448(11) Uani 1 1 d . . . C7 C 0.0354(4) 0.2148(4) 0.1230(2) 0.0432(11) Uani 1 1 d . . . C8 C -0.0683(4) 0.2288(4) 0.1509(3) 0.0637(15) Uani 1 1 d . . . H8 H -0.1239 0.2768 0.1337 0.076 Uiso 1 1 calc R . . C9 C -0.0902(5) 0.1729(4) 0.2034(3) 0.0664(16) Uani 1 1 d . . . H9 H -0.1613 0.1816 0.2228 0.080 Uiso 1 1 calc R . . C10 C -0.0083(4) 0.1041(4) 0.2276(3) 0.0611(15) Uani 1 1 d . . . H10 H -0.0218 0.0639 0.2637 0.073 Uiso 1 1 calc R . . C11 C 0.0940(4) 0.0952(4) 0.1982(2) 0.0508(12) Uani 1 1 d . . . H11 H 0.1506 0.0476 0.2150 0.061 Uiso 1 1 calc R . . C12 C 0.3148(4) 0.1235(4) -0.0413(2) 0.0431(11) Uani 1 1 d . . . C13 C 0.3262(4) 0.0713(4) -0.0971(2) 0.0531(13) Uani 1 1 d . . . H13 H 0.3254 0.1047 -0.1374 0.064 Uiso 1 1 calc R . . C14 C 0.3390(5) -0.0306(4) -0.0933(3) 0.0631(15) Uani 1 1 d . . . H14 H 0.3456 -0.0687 -0.1312 0.076 Uiso 1 1 calc R . . C15 C 0.3421(4) -0.0768(4) -0.0341(2) 0.0584(13) Uani 1 1 d . . . H15 H 0.3519 -0.1469 -0.0307 0.070 Uiso 1 1 calc R . . C16 C 0.3308(4) -0.0203(3) 0.0202(2) 0.0403(11) Uani 1 1 d . . . C17 C 0.3442(4) -0.0602(3) 0.0868(2) 0.0414(11) Uani 1 1 d . . . C18 C 0.3579(4) -0.1606(4) 0.1006(3) 0.0567(13) Uani 1 1 d . . . H18 H 0.3488 -0.2084 0.0668 0.068 Uiso 1 1 calc R . . C19 C 0.3846(4) -0.1907(4) 0.1635(3) 0.0631(15) Uani 1 1 d . . . H19 H 0.3973 -0.2592 0.1732 0.076 Uiso 1 1 calc R . . C20 C 0.3929(4) -0.1220(4) 0.2120(3) 0.0568(13) Uani 1 1 d . . . H20 H 0.4120 -0.1413 0.2557 0.068 Uiso 1 1 calc R . . C21 C 0.3727(4) -0.0229(4) 0.1956(2) 0.0489(12) Uani 1 1 d . . . H21 H 0.3773 0.0253 0.2291 0.059 Uiso 1 1 calc R . . C22 C 0.4060(4) 0.2825(3) 0.0030(2) 0.0457(12) Uani 1 1 d . . . C23 C 0.4900(4) 0.3437(3) -0.0202(3) 0.0554(13) Uani 1 1 d . . . H23 H 0.4864 0.3595 -0.0649 0.066 Uiso 1 1 calc R . . C24 C 0.5782(5) 0.3807(4) 0.0227(3) 0.0689(16) Uani 1 1 d . . . H24 H 0.6383 0.4208 0.0076 0.083 Uiso 1 1 calc R . . C25 C 0.5803(4) 0.3604(4) 0.0870(3) 0.0580(14) Uani 1 1 d . . . H25 H 0.6409 0.3867 0.1169 0.070 Uiso 1 1 calc R . . C26 C 0.4925(4) 0.3005(3) 0.1085(2) 0.0448(11) Uani 1 1 d . . . C27 C 0.4772(4) 0.2840(3) 0.1772(2) 0.0445(11) Uani 1 1 d . . . C28 C 0.5501(4) 0.3266(4) 0.2259(3) 0.0588(14) Uani 1 1 d . . . H28 H 0.6179 0.3627 0.2165 0.071 Uiso 1 1 calc R . . C29 C 0.5237(5) 0.3165(4) 0.2889(3) 0.0734(17) Uani 1 1 d . . . H29 H 0.5726 0.3464 0.3232 0.088 Uiso 1 1 calc R . . C30 C 0.4261(5) 0.2629(4) 0.3014(2) 0.0657(15) Uani 1 1 d . . . H30 H 0.4052 0.2555 0.3442 0.079 Uiso 1 1 calc R . . C31 C 0.3605(4) 0.2208(4) 0.2503(2) 0.0504(12) Uani 1 1 d . . . H31 H 0.2937 0.1828 0.2588 0.061 Uiso 1 1 calc R . . C32 C 0.488(4) 0.443(3) 0.4451(10) 0.146(16) Uani 0.50 1 d PD . . H32A H 0.4507 0.3795 0.4542 0.218 Uiso 0.50 1 calc PR . . H32B H 0.5653 0.4307 0.4305 0.218 Uiso 0.50 1 calc PR . . H32C H 0.4381 0.4783 0.4112 0.218 Uiso 0.50 1 calc PR . . C33 C 0.5000 0.5000 0.5000 0.19(2) Uani 1 2 d SD . . N1 N 0.1624(3) 0.2385(3) 0.03975(16) 0.0395(9) Uani 1 1 d . . . N2 N 0.1182(3) 0.1494(3) 0.14787(18) 0.0426(9) Uani 1 1 d . . . N3 N 0.3154(3) 0.0788(3) 0.01581(16) 0.0404(9) Uani 1 1 d . . . N4 N 0.3469(3) 0.0078(3) 0.13446(17) 0.0420(9) Uani 1 1 d . . . N5 N 0.4097(3) 0.2607(3) 0.06619(17) 0.0395(9) Uani 1 1 d . . . N6 N 0.3835(3) 0.2289(3) 0.18893(17) 0.0420(9) Uani 1 1 d . . . N7 N 0.490(5) 0.450(3) 0.4570(15) 0.20(3) Uani 0.50 1 d PD . . O1 O 0.3114(3) 0.2654(3) -0.10616(15) 0.0667(10) Uani 1 1 d . . . H1 H 0.2959 0.3262 -0.1108 0.100 Uiso 1 1 calc R . . O2 O 0.7747(3) 0.0468(3) 0.3341(2) 0.0835(12) Uani 1 1 d . . . O3 O 0.6291(4) 0.0897(4) 0.2540(3) 0.130(2) Uani 1 1 d . . . O4 O 0.6951(4) -0.0709(4) 0.2591(2) 0.1156(18) Uani 1 1 d . . . O5 O 0.5806(5) -0.0081(5) 0.3337(3) 0.142(2) Uani 1 1 d . . . O6 O 0.2425(4) 0.4745(4) 0.0616(2) 0.1076(16) Uani 1 1 d . . . O7 O 0.2303(6) 0.5998(5) 0.1332(4) 0.197(4) Uani 1 1 d . . . O8 O 0.4007(4) 0.5201(4) 0.1317(2) 0.1145(17) Uani 1 1 d . . . O9 O 0.2491(7) 0.4403(6) 0.1680(3) 0.197(3) Uani 1 1 d . . . Cl1 Cl 0.67069(11) 0.01319(10) 0.29521(6) 0.0554(4) Uani 1 1 d . . . Cl2 Cl 0.27612(11) 0.50940(11) 0.12348(7) 0.0600(4) Uani 1 1 d . . . Fe1 Fe 0.28816(5) 0.15912(5) 0.10471(3) 0.0363(2) 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 C1 0.066(3) 0.041(3) 0.034(3) 0.003(2) 0.007(2) 0.005(2) C2 0.059(3) 0.039(3) 0.037(3) 0.000(2) -0.001(2) 0.007(2) C3 0.081(4) 0.061(4) 0.047(3) 0.014(3) 0.002(3) 0.012(3) C4 0.066(4) 0.080(4) 0.068(4) 0.010(3) -0.015(3) 0.020(3) C5 0.048(3) 0.065(4) 0.073(4) 0.001(3) -0.001(3) 0.019(3) C6 0.045(3) 0.044(3) 0.044(3) -0.005(2) -0.001(2) 0.001(2) C7 0.039(3) 0.043(3) 0.048(3) -0.014(2) 0.004(2) -0.002(2) C8 0.056(3) 0.071(4) 0.066(4) -0.004(3) 0.014(3) 0.009(3) C9 0.056(3) 0.073(4) 0.074(4) -0.009(3) 0.026(3) -0.001(3) C10 0.059(3) 0.069(4) 0.058(3) -0.003(3) 0.018(3) -0.016(3) C11 0.053(3) 0.050(3) 0.050(3) 0.008(3) 0.005(2) -0.006(2) C12 0.056(3) 0.043(3) 0.031(3) 0.004(2) 0.006(2) 0.004(2) C13 0.076(3) 0.051(3) 0.033(3) -0.002(2) 0.009(2) 0.005(3) C14 0.083(4) 0.062(4) 0.046(3) -0.013(3) 0.012(3) 0.004(3) C15 0.085(4) 0.042(3) 0.048(3) -0.007(3) 0.008(3) 0.002(3) C16 0.047(3) 0.036(3) 0.039(3) -0.002(2) 0.005(2) 0.003(2) C17 0.046(3) 0.036(3) 0.043(3) -0.003(2) 0.008(2) 0.002(2) C18 0.082(4) 0.032(3) 0.057(3) -0.002(3) 0.016(3) 0.008(3) C19 0.084(4) 0.036(3) 0.071(4) 0.013(3) 0.021(3) 0.012(3) C20 0.068(3) 0.051(3) 0.051(3) 0.018(3) 0.008(3) 0.013(3) C21 0.053(3) 0.047(3) 0.045(3) 0.007(2) 0.000(2) 0.001(2) C22 0.058(3) 0.036(3) 0.046(3) 0.005(2) 0.019(2) 0.008(2) C23 0.072(3) 0.036(3) 0.063(3) 0.005(3) 0.028(3) 0.000(3) C24 0.079(4) 0.044(3) 0.091(5) -0.002(3) 0.044(4) -0.012(3) C25 0.052(3) 0.046(3) 0.078(4) -0.013(3) 0.018(3) -0.012(2) C26 0.045(3) 0.033(3) 0.058(3) -0.004(2) 0.012(2) 0.008(2) C27 0.042(3) 0.039(3) 0.051(3) -0.004(2) 0.003(2) -0.004(2) C28 0.056(3) 0.058(4) 0.061(4) 0.000(3) 0.000(3) -0.011(3) C29 0.081(4) 0.068(4) 0.065(4) -0.011(3) -0.022(3) -0.017(3) C30 0.081(4) 0.072(4) 0.041(3) -0.003(3) -0.009(3) -0.010(3) C31 0.054(3) 0.047(3) 0.049(3) -0.001(3) 0.002(2) -0.003(2) C32 0.26(4) 0.11(3) 0.070(14) 0.032(16) 0.030(18) 0.04(3) C33 0.097(13) 0.18(3) 0.29(5) 0.16(4) 0.04(3) 0.06(2) N1 0.049(2) 0.035(2) 0.033(2) -0.0029(17) -0.0004(17) 0.0051(17) N2 0.037(2) 0.049(3) 0.042(2) -0.0019(19) 0.0008(17) -0.0021(18) N3 0.052(2) 0.034(2) 0.036(2) -0.0017(18) 0.0073(17) 0.0039(17) N4 0.049(2) 0.041(2) 0.037(2) 0.0010(19) 0.0070(17) 0.0047(17) N5 0.047(2) 0.029(2) 0.042(2) -0.0002(18) 0.0069(18) -0.0023(16) N6 0.050(2) 0.040(2) 0.037(2) -0.0030(18) 0.0040(17) -0.0030(18) N7 0.15(3) 0.21(5) 0.24(5) 0.01(4) -0.01(3) 0.11(3) O1 0.107(3) 0.056(2) 0.0389(19) 0.0112(17) 0.0163(18) 0.018(2) O2 0.076(2) 0.077(3) 0.093(3) -0.023(2) -0.014(2) 0.004(2) O3 0.123(4) 0.090(4) 0.167(5) 0.041(4) -0.039(3) 0.022(3) O4 0.101(3) 0.119(4) 0.119(4) -0.070(3) -0.024(3) 0.047(3) O5 0.160(5) 0.170(5) 0.108(4) -0.055(4) 0.073(4) -0.088(4) O6 0.146(4) 0.114(4) 0.064(3) -0.037(3) 0.018(3) -0.046(3) O7 0.177(5) 0.142(6) 0.250(8) -0.129(6) -0.085(5) 0.099(5) O8 0.084(3) 0.140(5) 0.116(4) 0.006(3) -0.009(3) 0.007(3) O9 0.211(6) 0.244(8) 0.147(6) 0.098(6) 0.075(5) -0.026(6) Cl1 0.0612(8) 0.0550(9) 0.0506(8) -0.0078(7) 0.0085(6) 0.0076(6) Cl2 0.0658(9) 0.0631(9) 0.0521(8) -0.0059(7) 0.0108(6) 0.0121(7) Fe1 0.0416(4) 0.0334(4) 0.0338(4) -0.0005(3) 0.0031(3) 0.0013(3) _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 C1 O1 1.413(5) . ? C1 C22 1.531(6) . ? C1 C12 1.540(7) . ? C1 C2 1.542(6) . ? C2 N1 1.329(5) . ? C2 C3 1.387(6) . ? C3 C4 1.360(7) . ? C3 H3 0.9500 . ? C4 C5 1.399(8) . ? C4 H4 0.9500 . ? C5 C6 1.377(6) . ? C5 H5 0.9500 . ? C6 N1 1.355(5) . ? C6 C7 1.486(6) . ? C7 N2 1.354(6) . ? C7 C8 1.382(6) . ? C8 C9 1.370(7) . ? C8 H8 0.9500 . ? C9 C10 1.373(7) . ? C9 H9 0.9500 . ? C10 C11 1.377(7) . ? C10 H10 0.9500 . ? C11 N2 1.327(5) . ? C11 H11 0.9500 . ? C12 N3 1.331(5) . ? C12 C13 1.375(6) . ? C13 C14 1.379(7) . ? C13 H13 0.9500 . ? C14 C15 1.378(7) . ? C14 H14 0.9500 . ? C15 C16 1.379(6) . ? C15 H15 0.9500 . ? C16 N3 1.344(5) . ? C16 C17 1.480(6) . ? C17 N4 1.347(5) . ? C17 C18 1.384(6) . ? C18 C19 1.375(7) . ? C18 H18 0.9500 . ? C19 C20 1.365(7) . ? C19 H19 0.9500 . ? C20 C21 1.387(6) . ? C20 H20 0.9500 . ? C21 N4 1.342(5) . ? C21 H21 0.9500 . ? C22 N5 1.344(5) . ? C22 C23 1.386(6) . ? C23 C24 1.370(8) . ? C23 H23 0.9500 . ? C24 C25 1.366(8) . ? C24 H24 0.9500 . ? C25 C26 1.393(6) . ? C25 H25 0.9500 . ? C26 N5 1.337(5) . ? C26 C27 1.475(6) . ? C27 N6 1.343(5) . ? C27 C28 1.370(6) . ? C28 C29 1.381(7) . ? C28 H28 0.9500 . ? C29 C30 1.373(7) . ? C29 H29 0.9500 . ? C30 C31 1.361(6) . ? C30 H30 0.9500 . ? C31 N6 1.333(5) . ? C31 H31 0.9500 . ? C32 C33 1.37(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N7 1.111(17) 3_666 ? C33 N7 1.111(17) . ? C33 C32 1.37(3) 3_666 ? N1 Fe1 2.152(3) . ? N2 Fe1 2.223(4) . ? N3 Fe1 2.192(3) . ? N4 Fe1 2.209(4) . ? N5 Fe1 2.157(3) . ? N6 Fe1 2.179(3) . ? O1 H1 0.8400 . ? O2 Cl1 1.439(4) . ? O3 Cl1 1.391(4) . ? O4 Cl1 1.401(4) . ? O5 Cl1 1.397(5) . ? O6 Cl2 1.387(4) . ? O7 Cl2 1.345(5) . ? O8 Cl2 1.421(5) . ? O9 Cl2 1.369(6) . ? 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 O1 C1 C22 110.9(4) . . ? O1 C1 C12 104.4(4) . . ? C22 C1 C12 109.6(4) . . ? O1 C1 C2 111.4(4) . . ? C22 C1 C2 109.5(4) . . ? C12 C1 C2 110.9(4) . . ? N1 C2 C3 121.6(4) . . ? N1 C2 C1 117.1(4) . . ? C3 C2 C1 121.3(4) . . ? C4 C3 C2 119.3(5) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.9(5) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 117.8(5) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.1 . . ? N1 C6 C5 122.0(4) . . ? N1 C6 C7 114.5(4) . . ? C5 C6 C7 123.5(4) . . ? N2 C7 C8 121.4(5) . . ? N2 C7 C6 116.1(4) . . ? C8 C7 C6 122.5(4) . . ? C9 C8 C7 119.6(5) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 119.3(5) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C9 C10 C11 118.1(5) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? N2 C11 C10 123.8(5) . . ? N2 C11 H11 118.1 . . ? C10 C11 H11 118.1 . . ? N3 C12 C13 122.2(4) . . ? N3 C12 C1 116.2(4) . . ? C13 C12 C1 121.6(4) . . ? C12 C13 C14 118.4(5) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 119.5(5) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 119.3(5) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? N3 C16 C15 120.8(4) . . ? N3 C16 C17 115.0(4) . . ? C15 C16 C17 123.9(4) . . ? N4 C17 C18 121.0(4) . . ? N4 C17 C16 115.9(4) . . ? C18 C17 C16 123.1(4) . . ? C19 C18 C17 119.6(5) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C18 119.9(5) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 118.0(5) . . ? C19 C20 H20 121.0 . . ? C21 C20 H20 121.0 . . ? N4 C21 C20 123.0(5) . . ? N4 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? N5 C22 C23 121.1(5) . . ? N5 C22 C1 116.7(4) . . ? C23 C22 C1 122.2(4) . . ? C24 C23 C22 118.4(5) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C25 C24 C23 120.3(5) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.3(5) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? N5 C26 C25 120.2(5) . . ? N5 C26 C27 115.7(4) . . ? C25 C26 C27 123.9(4) . . ? N6 C27 C28 122.1(4) . . ? N6 C27 C26 115.7(4) . . ? C28 C27 C26 122.1(4) . . ? C27 C28 C29 119.1(5) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C30 C29 C28 119.5(5) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C31 C30 C29 117.5(5) . . ? C31 C30 H30 121.3 . . ? C29 C30 H30 121.3 . . ? N6 C31 C30 124.7(5) . . ? N6 C31 H31 117.7 . . ? C30 C31 H31 117.7 . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C32 C33 C32 180.000(12) 3_666 . ? C2 N1 C6 119.3(4) . . ? C2 N1 Fe1 123.0(3) . . ? C6 N1 Fe1 117.3(3) . . ? C11 N2 C7 117.7(4) . . ? C11 N2 Fe1 127.7(3) . . ? C7 N2 Fe1 114.2(3) . . ? C12 N3 C16 119.7(4) . . ? C12 N3 Fe1 122.9(3) . . ? C16 N3 Fe1 117.3(3) . . ? C21 N4 C17 118.4(4) . . ? C21 N4 Fe1 125.5(3) . . ? C17 N4 Fe1 115.8(3) . . ? C26 N5 C22 120.5(4) . . ? C26 N5 Fe1 116.5(3) . . ? C22 N5 Fe1 123.0(3) . . ? C31 N6 C27 117.2(4) . . ? C31 N6 Fe1 127.2(3) . . ? C27 N6 Fe1 115.7(3) . . ? C1 O1 H1 109.5 . . ? O3 Cl1 O5 106.3(4) . . ? O3 Cl1 O4 109.8(3) . . ? O5 Cl1 O4 110.0(3) . . ? O3 Cl1 O2 109.0(3) . . ? O5 Cl1 O2 110.8(3) . . ? O4 Cl1 O2 110.9(2) . . ? O7 Cl2 O9 113.0(5) . . ? O7 Cl2 O6 111.7(4) . . ? O9 Cl2 O6 109.9(4) . . ? O7 Cl2 O8 106.9(4) . . ? O9 Cl2 O8 106.2(4) . . ? O6 Cl2 O8 108.9(3) . . ? N1 Fe1 N5 82.31(13) . . ? N1 Fe1 N6 122.60(13) . . ? N5 Fe1 N6 74.91(14) . . ? N1 Fe1 N3 81.73(13) . . ? N5 Fe1 N3 81.13(13) . . ? N6 Fe1 N3 142.12(13) . . ? N1 Fe1 N4 142.74(13) . . ? N5 Fe1 N4 119.88(13) . . ? N6 Fe1 N4 93.33(13) . . ? N3 Fe1 N4 73.66(13) . . ? N1 Fe1 N2 74.30(14) . . ? N5 Fe1 N2 143.89(14) . . ? N6 Fe1 N2 94.87(13) . . ? N3 Fe1 N2 121.12(13) . . ? N4 Fe1 N2 94.86(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 172.1(4) . . . . ? C22 C1 C2 N1 -64.9(5) . . . . ? C12 C1 C2 N1 56.3(5) . . . . ? O1 C1 C2 C3 -10.0(6) . . . . ? C22 C1 C2 C3 113.1(5) . . . . ? C12 C1 C2 C3 -125.8(5) . . . . ? N1 C2 C3 C4 2.2(8) . . . . ? C1 C2 C3 C4 -175.7(5) . . . . ? C2 C3 C4 C5 -2.6(9) . . . . ? C3 C4 C5 C6 -0.5(8) . . . . ? C4 C5 C6 N1 4.4(7) . . . . ? C4 C5 C6 C7 -172.3(5) . . . . ? N1 C6 C7 N2 1.0(6) . . . . ? C5 C6 C7 N2 178.0(4) . . . . ? N1 C6 C7 C8 -175.9(4) . . . . ? C5 C6 C7 C8 1.1(7) . . . . ? N2 C7 C8 C9 -2.5(7) . . . . ? C6 C7 C8 C9 174.3(4) . . . . ? C7 C8 C9 C10 0.3(8) . . . . ? C8 C9 C10 C11 0.8(8) . . . . ? C9 C10 C11 N2 0.1(8) . . . . ? O1 C1 C12 N3 177.2(4) . . . . ? C22 C1 C12 N3 58.4(5) . . . . ? C2 C1 C12 N3 -62.7(5) . . . . ? O1 C1 C12 C13 -1.1(5) . . . . ? C22 C1 C12 C13 -119.9(5) . . . . ? C2 C1 C12 C13 119.0(4) . . . . ? N3 C12 C13 C14 -0.2(7) . . . . ? C1 C12 C13 C14 178.1(4) . . . . ? C12 C13 C14 C15 -1.2(7) . . . . ? C13 C14 C15 C16 0.9(7) . . . . ? C14 C15 C16 N3 0.8(7) . . . . ? C14 C15 C16 C17 -173.9(4) . . . . ? N3 C16 C17 N4 -4.0(5) . . . . ? C15 C16 C17 N4 170.9(4) . . . . ? N3 C16 C17 C18 178.3(4) . . . . ? C15 C16 C17 C18 -6.7(7) . . . . ? N4 C17 C18 C19 -5.7(7) . . . . ? C16 C17 C18 C19 171.8(4) . . . . ? C17 C18 C19 C20 2.6(8) . . . . ? C18 C19 C20 C21 0.5(8) . . . . ? C19 C20 C21 N4 -0.8(7) . . . . ? O1 C1 C22 N5 -179.3(4) . . . . ? C12 C1 C22 N5 -64.6(5) . . . . ? C2 C1 C22 N5 57.3(5) . . . . ? O1 C1 C22 C23 1.6(6) . . . . ? C12 C1 C22 C23 116.3(5) . . . . ? C2 C1 C22 C23 -121.7(5) . . . . ? N5 C22 C23 C24 0.8(7) . . . . ? C1 C22 C23 C24 179.9(4) . . . . ? C22 C23 C24 C25 -2.3(8) . . . . ? C23 C24 C25 C26 0.8(8) . . . . ? C24 C25 C26 N5 2.3(7) . . . . ? C24 C25 C26 C27 -171.9(5) . . . . ? N5 C26 C27 N6 1.6(6) . . . . ? C25 C26 C27 N6 176.0(4) . . . . ? N5 C26 C27 C28 -175.0(4) . . . . ? C25 C26 C27 C28 -0.5(7) . . . . ? N6 C27 C28 C29 -2.9(8) . . . . ? C26 C27 C28 C29 173.4(5) . . . . ? C27 C28 C29 C30 0.9(8) . . . . ? C28 C29 C30 C31 0.9(8) . . . . ? C29 C30 C31 N6 -0.9(8) . . . . ? C3 C2 N1 C6 1.6(7) . . . . ? C1 C2 N1 C6 179.6(4) . . . . ? C3 C2 N1 Fe1 -170.6(4) . . . . ? C1 C2 N1 Fe1 7.3(6) . . . . ? C5 C6 N1 C2 -5.0(7) . . . . ? C7 C6 N1 C2 172.0(4) . . . . ? C5 C6 N1 Fe1 167.7(4) . . . . ? C7 C6 N1 Fe1 -15.3(5) . . . . ? C10 C11 N2 C7 -2.2(7) . . . . ? C10 C11 N2 Fe1 170.3(4) . . . . ? C8 C7 N2 C11 3.3(6) . . . . ? C6 C7 N2 C11 -173.6(4) . . . . ? C8 C7 N2 Fe1 -170.1(4) . . . . ? C6 C7 N2 Fe1 12.9(5) . . . . ? C13 C12 N3 C16 1.8(6) . . . . ? C1 C12 N3 C16 -176.5(4) . . . . ? C13 C12 N3 Fe1 -176.7(3) . . . . ? C1 C12 N3 Fe1 5.0(5) . . . . ? C15 C16 N3 C12 -2.2(6) . . . . ? C17 C16 N3 C12 173.0(4) . . . . ? C15 C16 N3 Fe1 176.5(3) . . . . ? C17 C16 N3 Fe1 -8.4(5) . . . . ? C20 C21 N4 C17 -2.2(6) . . . . ? C20 C21 N4 Fe1 170.6(3) . . . . ? C18 C17 N4 C21 5.4(6) . . . . ? C16 C17 N4 C21 -172.3(4) . . . . ? C18 C17 N4 Fe1 -168.0(3) . . . . ? C16 C17 N4 Fe1 14.3(5) . . . . ? C25 C26 N5 C22 -3.8(6) . . . . ? C27 C26 N5 C22 170.8(4) . . . . ? C25 C26 N5 Fe1 174.8(3) . . . . ? C27 C26 N5 Fe1 -10.6(5) . . . . ? C23 C22 N5 C26 2.3(6) . . . . ? C1 C22 N5 C26 -176.8(4) . . . . ? C23 C22 N5 Fe1 -176.2(3) . . . . ? C1 C22 N5 Fe1 4.7(5) . . . . ? C30 C31 N6 C27 -1.0(7) . . . . ? C30 C31 N6 Fe1 177.2(4) . . . . ? C28 C27 N6 C31 2.9(7) . . . . ? C26 C27 N6 C31 -173.7(4) . . . . ? C28 C27 N6 Fe1 -175.4(4) . . . . ? C26 C27 N6 Fe1 8.0(5) . . . . ? C2 N1 Fe1 N5 36.8(3) . . . . ? C6 N1 Fe1 N5 -135.6(3) . . . . ? C2 N1 Fe1 N6 103.4(3) . . . . ? C6 N1 Fe1 N6 -69.0(3) . . . . ? C2 N1 Fe1 N3 -45.3(3) . . . . ? C6 N1 Fe1 N3 142.3(3) . . . . ? C2 N1 Fe1 N4 -93.9(4) . . . . ? C6 N1 Fe1 N4 93.7(4) . . . . ? C2 N1 Fe1 N2 -171.0(4) . . . . ? C6 N1 Fe1 N2 16.7(3) . . . . ? C26 N5 Fe1 N1 137.9(3) . . . . ? C22 N5 Fe1 N1 -43.6(3) . . . . ? C26 N5 Fe1 N6 11.1(3) . . . . ? C22 N5 Fe1 N6 -170.4(4) . . . . ? C26 N5 Fe1 N3 -139.3(3) . . . . ? C22 N5 Fe1 N3 39.2(3) . . . . ? C26 N5 Fe1 N4 -74.0(3) . . . . ? C22 N5 Fe1 N4 104.5(3) . . . . ? C26 N5 Fe1 N2 88.3(4) . . . . ? C22 N5 Fe1 N2 -93.1(4) . . . . ? C31 N6 Fe1 N1 101.5(4) . . . . ? C27 N6 Fe1 N1 -80.4(3) . . . . ? C31 N6 Fe1 N5 171.8(4) . . . . ? C27 N6 Fe1 N5 -10.1(3) . . . . ? C31 N6 Fe1 N3 -135.6(4) . . . . ? C27 N6 Fe1 N3 42.6(4) . . . . ? C31 N6 Fe1 N4 -68.2(4) . . . . ? C27 N6 Fe1 N4 110.0(3) . . . . ? C31 N6 Fe1 N2 27.0(4) . . . . ? C27 N6 Fe1 N2 -154.8(3) . . . . ? C12 N3 Fe1 N1 38.6(3) . . . . ? C16 N3 Fe1 N1 -140.0(3) . . . . ? C12 N3 Fe1 N5 -44.8(3) . . . . ? C16 N3 Fe1 N5 136.6(3) . . . . ? C12 N3 Fe1 N6 -95.8(4) . . . . ? C16 N3 Fe1 N6 85.6(4) . . . . ? C12 N3 Fe1 N4 -169.6(3) . . . . ? C16 N3 Fe1 N4 11.8(3) . . . . ? C12 N3 Fe1 N2 104.6(3) . . . . ? C16 N3 Fe1 N2 -74.0(3) . . . . ? C21 N4 Fe1 N1 -136.0(3) . . . . ? C17 N4 Fe1 N1 36.9(4) . . . . ? C21 N4 Fe1 N5 104.0(4) . . . . ? C17 N4 Fe1 N5 -83.1(3) . . . . ? C21 N4 Fe1 N6 29.5(4) . . . . ? C17 N4 Fe1 N6 -157.6(3) . . . . ? C21 N4 Fe1 N3 173.3(4) . . . . ? C17 N4 Fe1 N3 -13.8(3) . . . . ? C21 N4 Fe1 N2 -65.7(4) . . . . ? C17 N4 Fe1 N2 107.2(3) . . . . ? C11 N2 Fe1 N1 171.8(4) . . . . ? C7 N2 Fe1 N1 -15.5(3) . . . . ? C11 N2 Fe1 N5 -136.6(4) . . . . ? C7 N2 Fe1 N5 36.1(4) . . . . ? C11 N2 Fe1 N6 -65.7(4) . . . . ? C7 N2 Fe1 N6 107.0(3) . . . . ? C11 N2 Fe1 N3 101.9(4) . . . . ? C7 N2 Fe1 N3 -85.4(3) . . . . ? C11 N2 Fe1 N4 28.1(4) . . . . ? C7 N2 Fe1 N4 -159.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.613 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.118 # Attachment '3.cif' data_aja0708 _database_code_depnum_ccdc_archive 'CCDC 755783' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common aja0708 _chemical_melting_point ? _chemical_formula_moiety '2(C31 H22 Co N6 O), C2 H3 N, 4(Cl O4)' _chemical_formula_sum 'C64 H47 Cl4 Co2 N13 O18' _chemical_formula_weight 1545.81 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 _symmetry_space_group_name_Hall '-P 2yn' 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 11.4027(3) _cell_length_b 13.4301(3) _cell_length_c 20.7683(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.7710(10) _cell_angle_gamma 90.00 _cell_volume 3164.32(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16717 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7720 _exptl_absorpt_correction_T_max 0.8055 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25479 _diffrn_reflns_av_R_equivalents 0.1033 _diffrn_reflns_av_sigmaI/netI 0.1035 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7227 _reflns_number_gt 3979 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0753P)^2^+1.3677P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7227 _refine_ls_number_parameters 469 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1343 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1792 _refine_ls_wR_factor_gt 0.1500 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.013 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 C1 C 0.6966(4) 0.2374(3) 0.04234(19) 0.0448(11) Uani 1 1 d . . . C2 C 0.8131(4) 0.2713(3) 0.01834(19) 0.0405(10) Uani 1 1 d . . . C3 C 0.8904(5) 0.3335(4) 0.0545(2) 0.0598(14) Uani 1 1 d . . . H3 H 0.8747 0.3543 0.0964 0.072 Uiso 1 1 calc R . . C4 C 0.9905(5) 0.3648(4) 0.0288(3) 0.0668(15) Uani 1 1 d . . . H4 H 1.0427 0.4102 0.0521 0.080 Uiso 1 1 calc R . . C5 C 1.0151(4) 0.3300(4) -0.0311(2) 0.0564(13) Uani 1 1 d . . . H5 H 1.0843 0.3507 -0.0493 0.068 Uiso 1 1 calc R . . C6 C 0.9373(4) 0.2647(3) -0.0637(2) 0.0411(10) Uani 1 1 d . . . C7 C 0.9608(4) 0.2122(3) -0.1237(2) 0.0412(10) Uani 1 1 d . . . C8 C 1.0629(4) 0.2271(4) -0.1535(2) 0.0569(13) Uani 1 1 d . . . H8 H 1.1174 0.2774 -0.1385 0.068 Uiso 1 1 calc R . . C9 C 1.0844(5) 0.1677(4) -0.2055(3) 0.0636(15) Uani 1 1 d . . . H9 H 1.1546 0.1757 -0.2261 0.076 Uiso 1 1 calc R . . C10 C 1.0028(4) 0.0969(4) -0.2268(2) 0.0566(13) Uani 1 1 d . . . H10 H 1.0159 0.0549 -0.2621 0.068 Uiso 1 1 calc R . . C11 C 0.9008(4) 0.0876(4) -0.1960(2) 0.0477(11) Uani 1 1 d . . . H11 H 0.8444 0.0388 -0.2113 0.057 Uiso 1 1 calc R . . C12 C 0.6873(4) 0.1238(3) 0.0420(2) 0.0427(11) Uani 1 1 d . . . C13 C 0.6758(4) 0.0699(4) 0.0978(2) 0.0511(12) Uani 1 1 d . . . H13 H 0.6763 0.1024 0.1385 0.061 Uiso 1 1 calc R . . C14 C 0.6637(5) -0.0324(4) 0.0931(2) 0.0609(14) Uani 1 1 d . . . H14 H 0.6582 -0.0712 0.1309 0.073 Uiso 1 1 calc R . . C15 C 0.6594(5) -0.0779(4) 0.0335(2) 0.0559(13) Uani 1 1 d . . . H15 H 0.6496 -0.1480 0.0296 0.067 Uiso 1 1 calc R . . C16 C 0.6698(4) -0.0197(3) -0.0203(2) 0.0405(10) Uani 1 1 d . . . C17 C 0.6560(4) -0.0582(3) -0.0878(2) 0.0393(10) Uani 1 1 d . . . C18 C 0.6400(5) -0.1584(3) -0.1024(2) 0.0549(13) Uani 1 1 d . . . H18 H 0.6479 -0.2068 -0.0689 0.066 Uiso 1 1 calc R . . C19 C 0.6127(5) -0.1870(4) -0.1658(3) 0.0618(14) Uani 1 1 d . . . H19 H 0.6004 -0.2553 -0.1764 0.074 Uiso 1 1 calc R . . C20 C 0.6033(4) -0.1166(4) -0.2131(2) 0.0540(12) Uani 1 1 d . . . H20 H 0.5826 -0.1344 -0.2571 0.065 Uiso 1 1 calc R . . C21 C 0.6249(4) -0.0183(3) -0.1956(2) 0.0454(11) Uani 1 1 d . . . H21 H 0.6202 0.0306 -0.2288 0.054 Uiso 1 1 calc R . . C22 C 0.5927(4) 0.2807(3) -0.0023(2) 0.0436(11) Uani 1 1 d . . . C23 C 0.5092(5) 0.3432(3) 0.0203(3) 0.0536(13) Uani 1 1 d . . . H23 H 0.5132 0.3607 0.0648 0.064 Uiso 1 1 calc R . . C24 C 0.4210(5) 0.3791(4) -0.0229(3) 0.0612(14) Uani 1 1 d . . . H24 H 0.3609 0.4198 -0.0083 0.073 Uiso 1 1 calc R . . C25 C 0.4192(4) 0.3565(4) -0.0871(3) 0.0567(13) Uani 1 1 d . . . H25 H 0.3582 0.3816 -0.1173 0.068 Uiso 1 1 calc R . . C26 C 0.5063(4) 0.2970(3) -0.1078(2) 0.0395(10) Uani 1 1 d . . . C27 C 0.5240(4) 0.2793(3) -0.1764(2) 0.0428(11) Uani 1 1 d . . . C28 C 0.4516(4) 0.3208(4) -0.2268(2) 0.0569(13) Uani 1 1 d . . . H28 H 0.3826 0.3560 -0.2183 0.068 Uiso 1 1 calc R . . C29 C 0.4796(5) 0.3110(4) -0.2889(3) 0.0684(16) Uani 1 1 d . . . H29 H 0.4302 0.3389 -0.3239 0.082 Uiso 1 1 calc R . . C30 C 0.5808(5) 0.2601(4) -0.3001(2) 0.0576(13) Uani 1 1 d . . . H30 H 0.6036 0.2534 -0.3426 0.069 Uiso 1 1 calc R . . C31 C 0.6471(4) 0.2195(3) -0.2480(2) 0.0452(11) Uani 1 1 d . . . H31 H 0.7159 0.1834 -0.2559 0.054 Uiso 1 1 calc R . . C32 C 0.511(6) 0.440(4) 0.5552(14) 0.138(17) Uani 0.50 1 d PD . . H32A H 0.4382 0.4437 0.5767 0.208 Uiso 0.50 1 calc PR . . H32B H 0.5774 0.4630 0.5850 0.208 Uiso 0.50 1 calc PR . . H32C H 0.5244 0.3708 0.5427 0.208 Uiso 0.50 1 calc PR . . C33 C 0.5000 0.5000 0.5000 0.17(2) Uani 1 2 d SD . . N1 N 0.8358(3) 0.2385(2) -0.03996(15) 0.0379(8) Uani 1 1 d . . . N2 N 0.8785(3) 0.1442(3) -0.14587(16) 0.0391(8) Uani 1 1 d . . . N3 N 0.6864(3) 0.0789(3) -0.01583(15) 0.0370(8) Uani 1 1 d . . . N4 N 0.6518(3) 0.0115(2) -0.13452(16) 0.0366(8) Uani 1 1 d . . . N5 N 0.5899(3) 0.2578(2) -0.06499(16) 0.0372(8) Uani 1 1 d . . . N6 N 0.6212(3) 0.2274(3) -0.18693(16) 0.0389(8) Uani 1 1 d . . . N7 N 0.510(6) 0.448(3) 0.5427(14) 0.17(3) Uani 0.50 1 d PD . . O1 O 0.6891(4) 0.2653(3) 0.10744(14) 0.0619(10) Uani 1 1 d . . . H1 H 0.6967 0.3273 0.1111 0.093 Uiso 1 1 calc R . . O2 O 0.9136(6) 0.5115(5) 0.1643(3) 0.149(3) Uani 1 1 d . . . O3 O 0.8687(5) 0.4125(4) 0.2446(3) 0.130(2) Uani 1 1 d . . . O4 O 0.8003(4) 0.5717(4) 0.2402(2) 0.1177(19) Uani 1 1 d . . . O5 O 0.7214(3) 0.4540(3) 0.16479(19) 0.0795(12) Uani 1 1 d . . . O6 O 0.4025(4) 0.4833(5) 0.1301(2) 0.1211(18) Uani 1 1 d . . . O7 O 0.2485(8) 0.5527(7) 0.1694(3) 0.214(4) Uani 1 1 d . . . O8 O 0.2385(6) 0.3961(5) 0.1304(4) 0.190(3) Uani 1 1 d . . . O9 O 0.2436(5) 0.5265(3) 0.0618(2) 0.1056(16) Uani 1 1 d . . . Cl1 Cl 0.82524(11) 0.48839(9) 0.20354(6) 0.0524(3) Uani 1 1 d . . . Cl2 Cl 0.27678(12) 0.48994(10) 0.12330(6) 0.0564(3) Uani 1 1 d . . . Co1 Co 0.71124(5) 0.15938(4) -0.10237(2) 0.0341(2) 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 C1 0.065(3) 0.039(3) 0.031(2) -0.0046(19) 0.006(2) -0.004(2) C2 0.050(3) 0.039(2) 0.032(2) -0.0004(19) 0.003(2) -0.006(2) C3 0.074(4) 0.054(3) 0.049(3) -0.015(2) -0.005(3) -0.007(3) C4 0.063(4) 0.069(4) 0.065(4) -0.014(3) -0.013(3) -0.015(3) C5 0.046(3) 0.059(3) 0.062(3) -0.001(3) -0.001(2) -0.016(3) C6 0.040(2) 0.038(2) 0.044(2) 0.001(2) -0.001(2) -0.003(2) C7 0.041(2) 0.035(2) 0.047(3) 0.007(2) -0.001(2) -0.002(2) C8 0.043(3) 0.062(3) 0.067(3) 0.008(3) 0.012(3) -0.009(2) C9 0.053(3) 0.074(4) 0.068(4) 0.005(3) 0.026(3) 0.003(3) C10 0.057(3) 0.064(3) 0.050(3) -0.001(3) 0.011(3) 0.014(3) C11 0.049(3) 0.048(3) 0.047(3) -0.002(2) 0.011(2) 0.005(2) C12 0.051(3) 0.038(2) 0.040(2) -0.002(2) 0.011(2) -0.005(2) C13 0.067(3) 0.053(3) 0.035(2) 0.004(2) 0.011(2) -0.004(3) C14 0.084(4) 0.053(3) 0.047(3) 0.015(2) 0.010(3) -0.002(3) C15 0.083(4) 0.037(3) 0.049(3) 0.010(2) 0.008(3) -0.004(3) C16 0.043(2) 0.037(3) 0.042(2) 0.006(2) 0.008(2) -0.001(2) C17 0.044(2) 0.035(2) 0.040(2) 0.001(2) 0.010(2) -0.006(2) C18 0.074(3) 0.032(3) 0.061(3) -0.003(2) 0.017(3) -0.003(2) C19 0.079(4) 0.041(3) 0.067(3) -0.014(3) 0.014(3) -0.008(3) C20 0.063(3) 0.049(3) 0.050(3) -0.016(2) 0.005(2) -0.010(3) C21 0.048(3) 0.044(3) 0.042(3) 0.000(2) 0.001(2) -0.003(2) C22 0.054(3) 0.038(3) 0.042(3) -0.005(2) 0.019(2) -0.007(2) C23 0.072(3) 0.032(2) 0.062(3) -0.005(2) 0.033(3) -0.004(2) C24 0.065(3) 0.043(3) 0.081(4) 0.005(3) 0.035(3) 0.010(3) C25 0.055(3) 0.049(3) 0.069(3) 0.012(3) 0.017(3) 0.011(2) C26 0.044(2) 0.028(2) 0.048(3) 0.004(2) 0.013(2) -0.003(2) C27 0.041(2) 0.031(2) 0.055(3) 0.001(2) -0.001(2) 0.001(2) C28 0.050(3) 0.058(3) 0.062(3) 0.003(3) -0.002(2) 0.011(2) C29 0.077(4) 0.072(4) 0.052(3) 0.010(3) -0.014(3) 0.016(3) C30 0.069(3) 0.060(3) 0.041(3) 0.001(2) -0.003(2) 0.002(3) C31 0.051(3) 0.044(3) 0.040(2) 0.004(2) 0.000(2) 0.005(2) C32 0.17(4) 0.13(3) 0.12(2) -0.018(19) 0.05(2) -0.04(3) C33 0.085(12) 0.17(4) 0.24(5) -0.13(4) 0.03(2) -0.066(17) N1 0.046(2) 0.035(2) 0.0322(19) 0.0016(15) 0.0006(16) -0.0060(16) N2 0.039(2) 0.041(2) 0.0386(19) 0.0006(16) 0.0063(16) 0.0036(17) N3 0.047(2) 0.032(2) 0.0320(18) 0.0010(15) 0.0066(16) -0.0005(16) N4 0.0391(19) 0.0341(19) 0.0375(19) -0.0011(16) 0.0079(16) -0.0057(16) N5 0.043(2) 0.0293(18) 0.040(2) 0.0007(16) 0.0066(16) -0.0004(16) N6 0.042(2) 0.038(2) 0.037(2) 0.0003(16) 0.0034(16) 0.0005(17) N7 0.19(4) 0.17(6) 0.14(4) -0.02(3) -0.02(3) -0.10(4) O1 0.099(3) 0.053(2) 0.0366(17) -0.0093(15) 0.0191(18) -0.016(2) O2 0.175(5) 0.179(6) 0.105(4) -0.056(4) 0.070(4) -0.106(5) O3 0.114(4) 0.089(3) 0.176(5) 0.042(4) -0.043(4) 0.016(3) O4 0.095(3) 0.126(4) 0.124(4) -0.077(3) -0.027(3) 0.050(3) O5 0.076(3) 0.070(3) 0.088(3) -0.017(2) -0.015(2) 0.003(2) O6 0.084(3) 0.161(5) 0.117(4) -0.010(3) 0.000(3) 0.000(3) O7 0.278(9) 0.249(9) 0.131(5) -0.064(6) 0.097(6) 0.062(7) O8 0.186(6) 0.118(5) 0.245(7) 0.108(5) -0.081(5) -0.091(5) O9 0.148(4) 0.105(3) 0.066(3) 0.039(2) 0.016(3) 0.043(3) Cl1 0.0588(7) 0.0502(7) 0.0488(7) -0.0055(6) 0.0079(6) 0.0070(6) Cl2 0.0640(8) 0.0544(8) 0.0517(7) 0.0062(6) 0.0107(6) -0.0086(6) Co1 0.0392(3) 0.0314(3) 0.0318(3) 0.0006(2) 0.0035(2) -0.0014(3) _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 C1 O1 1.414(5) . ? C1 C12 1.529(6) . ? C1 C2 1.534(6) . ? C1 C22 1.543(6) . ? C2 N1 1.338(5) . ? C2 C3 1.380(6) . ? C3 C4 1.373(7) . ? C3 H3 0.9500 . ? C4 C5 1.383(7) . ? C4 H4 0.9500 . ? C5 C6 1.376(6) . ? C5 H5 0.9500 . ? C6 N1 1.349(5) . ? C6 C7 1.480(6) . ? C7 N2 1.357(5) . ? C7 C8 1.387(6) . ? C8 C9 1.383(7) . ? C8 H8 0.9500 . ? C9 C10 1.372(7) . ? C9 H9 0.9500 . ? C10 C11 1.388(6) . ? C10 H10 0.9500 . ? C11 N2 1.335(5) . ? C11 H11 0.9500 . ? C12 N3 1.344(5) . ? C12 C13 1.384(6) . ? C13 C14 1.384(7) . ? C13 H13 0.9500 . ? C14 C15 1.376(7) . ? C14 H14 0.9500 . ? C15 C16 1.379(6) . ? C15 H15 0.9500 . ? C16 N3 1.339(5) . ? C16 C17 1.487(6) . ? C17 N4 1.345(5) . ? C17 C18 1.387(6) . ? C18 C19 1.376(7) . ? C18 H18 0.9500 . ? C19 C20 1.360(7) . ? C19 H19 0.9500 . ? C20 C21 1.384(6) . ? C20 H20 0.9500 . ? C21 N4 1.337(5) . ? C21 H21 0.9500 . ? C22 N5 1.335(5) . ? C22 C23 1.385(6) . ? C23 C24 1.367(7) . ? C23 H23 0.9500 . ? C24 C25 1.366(7) . ? C24 H24 0.9500 . ? C25 C26 1.377(6) . ? C25 H25 0.9500 . ? C26 N5 1.344(5) . ? C26 C27 1.478(6) . ? C27 N6 1.346(5) . ? C27 C28 1.383(6) . ? C28 C29 1.366(7) . ? C28 H28 0.9500 . ? C29 C30 1.381(7) . ? C29 H29 0.9500 . ? C30 C31 1.369(6) . ? C30 H30 0.9500 . ? C31 N6 1.336(5) . ? C31 H31 0.9500 . ? C32 C33 1.40(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N7 1.127(18) 3_666 ? C33 N7 1.127(18) . ? C33 C32 1.40(4) 3_666 ? N1 Co1 2.111(3) . ? N2 Co1 2.200(3) . ? N3 Co1 2.141(3) . ? N4 Co1 2.181(3) . ? N5 Co1 2.116(3) . ? N6 Co1 2.147(3) . ? O1 H1 0.8400 . ? O2 Cl1 1.392(5) . ? O3 Cl1 1.388(4) . ? O4 Cl1 1.398(4) . ? O5 Cl1 1.439(4) . ? O6 Cl2 1.429(5) . ? O7 Cl2 1.339(6) . ? O8 Cl2 1.347(5) . ? O9 Cl2 1.385(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 O1 C1 C12 104.9(3) . . ? O1 C1 C2 111.7(3) . . ? C12 C1 C2 110.9(4) . . ? O1 C1 C22 110.9(4) . . ? C12 C1 C22 108.9(4) . . ? C2 C1 C22 109.3(3) . . ? N1 C2 C3 121.3(4) . . ? N1 C2 C1 116.7(4) . . ? C3 C2 C1 122.0(4) . . ? C4 C3 C2 119.0(5) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.9(5) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 118.6(5) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N1 C6 C5 121.4(4) . . ? N1 C6 C7 114.7(4) . . ? C5 C6 C7 123.7(4) . . ? N2 C7 C8 121.9(4) . . ? N2 C7 C6 115.3(4) . . ? C8 C7 C6 122.7(4) . . ? C9 C8 C7 119.3(5) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C8 118.8(5) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 119.2(5) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? N2 C11 C10 122.8(4) . . ? N2 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? N3 C12 C13 121.4(4) . . ? N3 C12 C1 116.5(4) . . ? C13 C12 C1 122.1(4) . . ? C14 C13 C12 118.5(4) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C15 C14 C13 119.9(4) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 118.6(4) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? N3 C16 C15 121.8(4) . . ? N3 C16 C17 114.2(4) . . ? C15 C16 C17 123.9(4) . . ? N4 C17 C18 121.5(4) . . ? N4 C17 C16 115.5(4) . . ? C18 C17 C16 122.8(4) . . ? C19 C18 C17 119.5(5) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C20 C19 C18 119.4(4) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 118.3(4) . . ? C19 C20 H20 120.9 . . ? C21 C20 H20 120.9 . . ? N4 C21 C20 123.5(4) . . ? N4 C21 H21 118.2 . . ? C20 C21 H21 118.2 . . ? N5 C22 C23 121.3(4) . . ? N5 C22 C1 116.1(4) . . ? C23 C22 C1 122.5(4) . . ? C24 C23 C22 118.5(5) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C25 C24 C23 120.0(5) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 119.6(5) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? N5 C26 C25 120.4(4) . . ? N5 C26 C27 114.8(4) . . ? C25 C26 C27 124.5(4) . . ? N6 C27 C28 121.7(4) . . ? N6 C27 C26 115.7(4) . . ? C28 C27 C26 122.4(4) . . ? C29 C28 C27 119.9(5) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 119.0(5) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C31 C30 C29 118.0(5) . . ? C31 C30 H30 121.0 . . ? C29 C30 H30 121.0 . . ? N6 C31 C30 124.1(4) . . ? N6 C31 H31 117.9 . . ? C30 C31 H31 117.9 . . ? C33 C32 H32A 108.8 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N7 C33 N7 180.0(19) 3_666 . ? C32 C33 C32 180.000(16) 3_666 . ? C2 N1 C6 119.7(4) . . ? C2 N1 Co1 122.8(3) . . ? C6 N1 Co1 117.1(3) . . ? C11 N2 C7 117.9(4) . . ? C11 N2 Co1 127.9(3) . . ? C7 N2 Co1 113.4(3) . . ? C16 N3 C12 119.7(4) . . ? C16 N3 Co1 118.1(3) . . ? C12 N3 Co1 122.3(3) . . ? C21 N4 C17 117.7(4) . . ? C21 N4 Co1 126.7(3) . . ? C17 N4 Co1 115.2(3) . . ? C22 N5 C26 120.1(4) . . ? C22 N5 Co1 123.3(3) . . ? C26 N5 Co1 116.6(3) . . ? C31 N6 C27 117.4(4) . . ? C31 N6 Co1 127.6(3) . . ? C27 N6 Co1 115.0(3) . . ? C1 O1 H1 109.5 . . ? O3 Cl1 O2 106.7(4) . . ? O3 Cl1 O4 109.5(3) . . ? O2 Cl1 O4 109.8(4) . . ? O3 Cl1 O5 109.3(3) . . ? O2 Cl1 O5 110.3(3) . . ? O4 Cl1 O5 111.1(2) . . ? O7 Cl2 O8 114.0(5) . . ? O7 Cl2 O9 111.9(4) . . ? O8 Cl2 O9 111.8(4) . . ? O7 Cl2 O6 106.3(5) . . ? O8 Cl2 O6 105.3(4) . . ? O9 Cl2 O6 107.0(3) . . ? N1 Co1 N5 83.38(13) . . ? N1 Co1 N3 82.90(13) . . ? N5 Co1 N3 82.01(13) . . ? N1 Co1 N6 121.66(13) . . ? N5 Co1 N6 75.98(13) . . ? N3 Co1 N6 143.99(13) . . ? N1 Co1 N4 144.61(13) . . ? N5 Co1 N4 119.13(12) . . ? N3 Co1 N4 74.56(12) . . ? N6 Co1 N4 91.66(13) . . ? N1 Co1 N2 74.99(13) . . ? N5 Co1 N2 146.48(13) . . ? N3 Co1 N2 119.44(13) . . ? N6 Co1 N2 93.81(13) . . ? N4 Co1 N2 92.61(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 172.1(4) . . . . ? C12 C1 C2 N1 55.4(5) . . . . ? C22 C1 C2 N1 -64.7(5) . . . . ? O1 C1 C2 C3 -8.5(6) . . . . ? C12 C1 C2 C3 -125.2(5) . . . . ? C22 C1 C2 C3 114.6(5) . . . . ? N1 C2 C3 C4 2.3(7) . . . . ? C1 C2 C3 C4 -177.0(4) . . . . ? C2 C3 C4 C5 -3.1(8) . . . . ? C3 C4 C5 C6 0.4(8) . . . . ? C4 C5 C6 N1 3.4(7) . . . . ? C4 C5 C6 C7 -171.8(4) . . . . ? N1 C6 C7 N2 -1.1(5) . . . . ? C5 C6 C7 N2 174.5(4) . . . . ? N1 C6 C7 C8 -177.6(4) . . . . ? C5 C6 C7 C8 -2.0(7) . . . . ? N2 C7 C8 C9 -3.2(7) . . . . ? C6 C7 C8 C9 173.1(4) . . . . ? C7 C8 C9 C10 1.3(7) . . . . ? C8 C9 C10 C11 0.5(7) . . . . ? C9 C10 C11 N2 -0.5(7) . . . . ? O1 C1 C12 N3 176.8(4) . . . . ? C2 C1 C12 N3 -62.4(5) . . . . ? C22 C1 C12 N3 58.0(5) . . . . ? O1 C1 C12 C13 -0.8(6) . . . . ? C2 C1 C12 C13 120.0(4) . . . . ? C22 C1 C12 C13 -119.7(5) . . . . ? N3 C12 C13 C14 0.2(7) . . . . ? C1 C12 C13 C14 177.7(5) . . . . ? C12 C13 C14 C15 -2.0(8) . . . . ? C13 C14 C15 C16 1.2(8) . . . . ? C14 C15 C16 N3 1.5(7) . . . . ? C14 C15 C16 C17 -174.3(5) . . . . ? N3 C16 C17 N4 -5.5(5) . . . . ? C15 C16 C17 N4 170.6(4) . . . . ? N3 C16 C17 C18 178.9(4) . . . . ? C15 C16 C17 C18 -5.0(7) . . . . ? N4 C17 C18 C19 -3.7(7) . . . . ? C16 C17 C18 C19 171.6(4) . . . . ? C17 C18 C19 C20 0.9(8) . . . . ? C18 C19 C20 C21 1.6(8) . . . . ? C19 C20 C21 N4 -1.5(7) . . . . ? O1 C1 C22 N5 -179.1(3) . . . . ? C12 C1 C22 N5 -64.1(5) . . . . ? C2 C1 C22 N5 57.3(5) . . . . ? O1 C1 C22 C23 3.5(6) . . . . ? C12 C1 C22 C23 118.6(4) . . . . ? C2 C1 C22 C23 -120.1(4) . . . . ? N5 C22 C23 C24 1.9(7) . . . . ? C1 C22 C23 C24 179.1(4) . . . . ? C22 C23 C24 C25 -2.6(7) . . . . ? C23 C24 C25 C26 0.3(7) . . . . ? C24 C25 C26 N5 2.8(7) . . . . ? C24 C25 C26 C27 -170.7(4) . . . . ? N5 C26 C27 N6 -0.5(5) . . . . ? C25 C26 C27 N6 173.3(4) . . . . ? N5 C26 C27 C28 -174.9(4) . . . . ? C25 C26 C27 C28 -1.1(7) . . . . ? N6 C27 C28 C29 -1.3(7) . . . . ? C26 C27 C28 C29 172.8(5) . . . . ? C27 C28 C29 C30 -0.4(8) . . . . ? C28 C29 C30 C31 1.5(8) . . . . ? C29 C30 C31 N6 -1.1(7) . . . . ? C3 C2 N1 C6 1.4(6) . . . . ? C1 C2 N1 C6 -179.3(4) . . . . ? C3 C2 N1 Co1 -171.6(3) . . . . ? C1 C2 N1 Co1 7.7(5) . . . . ? C5 C6 N1 C2 -4.3(6) . . . . ? C7 C6 N1 C2 171.3(4) . . . . ? C5 C6 N1 Co1 169.1(3) . . . . ? C7 C6 N1 Co1 -15.3(4) . . . . ? C10 C11 N2 C7 -1.3(6) . . . . ? C10 C11 N2 Co1 168.1(3) . . . . ? C8 C7 N2 C11 3.2(6) . . . . ? C6 C7 N2 C11 -173.4(4) . . . . ? C8 C7 N2 Co1 -167.7(3) . . . . ? C6 C7 N2 Co1 15.7(4) . . . . ? C15 C16 N3 C12 -3.4(6) . . . . ? C17 C16 N3 C12 172.8(4) . . . . ? C15 C16 N3 Co1 176.5(4) . . . . ? C17 C16 N3 Co1 -7.3(5) . . . . ? C13 C12 N3 C16 2.5(6) . . . . ? C1 C12 N3 C16 -175.2(4) . . . . ? C13 C12 N3 Co1 -177.3(3) . . . . ? C1 C12 N3 Co1 5.0(5) . . . . ? C20 C21 N4 C17 -1.2(6) . . . . ? C20 C21 N4 Co1 170.8(3) . . . . ? C18 C17 N4 C21 3.8(6) . . . . ? C16 C17 N4 C21 -171.8(4) . . . . ? C18 C17 N4 Co1 -169.1(4) . . . . ? C16 C17 N4 Co1 15.2(5) . . . . ? C23 C22 N5 C26 1.2(6) . . . . ? C1 C22 N5 C26 -176.2(4) . . . . ? C23 C22 N5 Co1 -178.0(3) . . . . ? C1 C22 N5 Co1 4.6(5) . . . . ? C25 C26 N5 C22 -3.6(6) . . . . ? C27 C26 N5 C22 170.5(4) . . . . ? C25 C26 N5 Co1 175.7(3) . . . . ? C27 C26 N5 Co1 -10.3(4) . . . . ? C30 C31 N6 C27 -0.5(6) . . . . ? C30 C31 N6 Co1 175.6(3) . . . . ? C28 C27 N6 C31 1.7(6) . . . . ? C26 C27 N6 C31 -172.7(4) . . . . ? C28 C27 N6 Co1 -174.9(3) . . . . ? C26 C27 N6 Co1 10.7(4) . . . . ? C2 N1 Co1 N5 36.8(3) . . . . ? C6 N1 Co1 N5 -136.4(3) . . . . ? C2 N1 Co1 N3 -45.9(3) . . . . ? C6 N1 Co1 N3 140.9(3) . . . . ? C2 N1 Co1 N6 105.8(3) . . . . ? C6 N1 Co1 N6 -67.3(3) . . . . ? C2 N1 Co1 N4 -96.2(4) . . . . ? C6 N1 Co1 N4 90.6(3) . . . . ? C2 N1 Co1 N2 -169.0(3) . . . . ? C6 N1 Co1 N2 17.8(3) . . . . ? C22 N5 Co1 N1 -43.8(3) . . . . ? C26 N5 Co1 N1 137.0(3) . . . . ? C22 N5 Co1 N3 40.0(3) . . . . ? C26 N5 Co1 N3 -139.3(3) . . . . ? C22 N5 Co1 N6 -168.8(3) . . . . ? C26 N5 Co1 N6 12.0(3) . . . . ? C22 N5 Co1 N4 107.3(3) . . . . ? C26 N5 Co1 N4 -72.0(3) . . . . ? C22 N5 Co1 N2 -93.4(4) . . . . ? C26 N5 Co1 N2 87.4(3) . . . . ? C16 N3 Co1 N1 -140.9(3) . . . . ? C12 N3 Co1 N1 38.9(3) . . . . ? C16 N3 Co1 N5 134.8(3) . . . . ? C12 N3 Co1 N5 -45.4(3) . . . . ? C16 N3 Co1 N6 82.3(4) . . . . ? C12 N3 Co1 N6 -97.9(4) . . . . ? C16 N3 Co1 N4 11.5(3) . . . . ? C12 N3 Co1 N4 -168.7(3) . . . . ? C16 N3 Co1 N2 -72.7(3) . . . . ? C12 N3 Co1 N2 107.2(3) . . . . ? C31 N6 Co1 N1 98.9(4) . . . . ? C27 N6 Co1 N1 -85.0(3) . . . . ? C31 N6 Co1 N5 171.8(4) . . . . ? C27 N6 Co1 N5 -12.1(3) . . . . ? C31 N6 Co1 N3 -134.2(3) . . . . ? C27 N6 Co1 N3 42.0(4) . . . . ? C31 N6 Co1 N4 -68.6(4) . . . . ? C27 N6 Co1 N4 107.6(3) . . . . ? C31 N6 Co1 N2 24.2(4) . . . . ? C27 N6 Co1 N2 -159.7(3) . . . . ? C21 N4 Co1 N1 -134.0(3) . . . . ? C17 N4 Co1 N1 38.2(4) . . . . ? C21 N4 Co1 N5 102.2(3) . . . . ? C17 N4 Co1 N5 -85.7(3) . . . . ? C21 N4 Co1 N3 173.6(4) . . . . ? C17 N4 Co1 N3 -14.3(3) . . . . ? C21 N4 Co1 N6 27.3(4) . . . . ? C17 N4 Co1 N6 -160.5(3) . . . . ? C21 N4 Co1 N2 -66.6(3) . . . . ? C17 N4 Co1 N2 105.6(3) . . . . ? C11 N2 Co1 N1 172.5(4) . . . . ? C7 N2 Co1 N1 -17.7(3) . . . . ? C11 N2 Co1 N5 -135.9(3) . . . . ? C7 N2 Co1 N5 33.9(4) . . . . ? C11 N2 Co1 N3 99.8(4) . . . . ? C7 N2 Co1 N3 -90.4(3) . . . . ? C11 N2 Co1 N6 -65.7(4) . . . . ? C7 N2 Co1 N6 104.0(3) . . . . ? C11 N2 Co1 N4 26.1(4) . . . . ? C7 N2 Co1 N4 -164.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.835 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.081 # Attachment '4.cif' data_aja0710 _database_code_depnum_ccdc_archive 'CCDC 755784' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common aja0710 _chemical_melting_point ? _chemical_formula_moiety '2(C31 H22 N6 Ni O), C2 H3 N, 4(Cl O4)' _chemical_formula_sum 'C64 H47 Cl4 N13 Ni2 O18' _chemical_formula_weight 1545.33 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' 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 11.4636(2) _cell_length_b 13.4293(2) _cell_length_c 20.7077(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.0130(10) _cell_angle_gamma 90.00 _cell_volume 3175.72(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23666 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7558 _exptl_absorpt_correction_T_max 0.7912 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43216 _diffrn_reflns_av_R_equivalents 0.1449 _diffrn_reflns_av_sigmaI/netI 0.1012 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.53 _reflns_number_total 7268 _reflns_number_gt 4025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1642P)^2^+2.8768P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0041(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7268 _refine_ls_number_parameters 439 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1553 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2884 _refine_ls_wR_factor_gt 0.2425 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.031 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 C1 C 0.6996(6) 0.2367(5) 1.0454(3) 0.0444(15) Uani 1 1 d . . . C2 C 0.8128(6) 0.2744(5) 1.0183(3) 0.0436(14) Uani 1 1 d . . . C3 C 0.8942(7) 0.3341(5) 1.0539(4) 0.0560(18) Uani 1 1 d . . . H3 H 0.8827 0.3527 1.0971 0.067 Uiso 1 1 calc R . . C4 C 0.9903(7) 0.3653(6) 1.0257(4) 0.064(2) Uani 1 1 d . . . H4 H 1.0419 0.4120 1.0476 0.076 Uiso 1 1 calc R . . C5 C 1.0138(6) 0.3299(5) 0.9659(4) 0.0602(19) Uani 1 1 d . . . H5 H 1.0834 0.3479 0.9470 0.072 Uiso 1 1 calc R . . C6 C 0.9305(5) 0.2659(4) 0.9338(3) 0.0430(14) Uani 1 1 d . . . C7 C 0.9535(5) 0.2083(4) 0.8751(3) 0.0419(14) Uani 1 1 d . . . C8 C 1.0492(6) 0.2237(6) 0.8404(4) 0.0571(18) Uani 1 1 d . . . H8 H 1.1003 0.2782 0.8507 0.068 Uiso 1 1 calc R . . C9 C 1.0703(7) 0.1598(6) 0.7908(4) 0.068(2) Uani 1 1 d . . . H9 H 1.1372 0.1680 0.7673 0.082 Uiso 1 1 calc R . . C10 C 0.9922(6) 0.0837(6) 0.7761(4) 0.0601(19) Uani 1 1 d . . . H10 H 1.0049 0.0382 0.7423 0.072 Uiso 1 1 calc R . . C11 C 0.8955(6) 0.0740(5) 0.8106(3) 0.0519(17) Uani 1 1 d . . . H11 H 0.8420 0.0215 0.7993 0.062 Uiso 1 1 calc R . . C12 C 0.6937(5) 0.1223(5) 1.0451(3) 0.0446(15) Uani 1 1 d . . . C13 C 0.6835(6) 0.0682(5) 1.1009(3) 0.0518(17) Uani 1 1 d . . . H13 H 0.6846 0.1002 1.1419 0.062 Uiso 1 1 calc R . . C14 C 0.6713(7) -0.0362(5) 1.0955(4) 0.0580(18) Uani 1 1 d . . . H14 H 0.6682 -0.0765 1.1330 0.070 Uiso 1 1 calc R . . C15 C 0.6640(6) -0.0781(5) 1.0347(3) 0.0548(17) Uani 1 1 d . . . H15 H 0.6514 -0.1477 1.0297 0.066 Uiso 1 1 calc R . . C16 C 0.6751(5) -0.0192(4) 0.9811(3) 0.0405(14) Uani 1 1 d . . . C17 C 0.6536(5) -0.0537(4) 0.9130(3) 0.0407(14) Uani 1 1 d . . . C18 C 0.6403(6) -0.1535(5) 0.8962(4) 0.0539(18) Uani 1 1 d . . . H18 H 0.6551 -0.2041 0.9280 0.065 Uiso 1 1 calc R . . C19 C 0.6050(6) -0.1784(5) 0.8320(4) 0.0555(18) Uani 1 1 d . . . H19 H 0.5941 -0.2462 0.8196 0.067 Uiso 1 1 calc R . . C20 C 0.5865(6) -0.1051(5) 0.7877(3) 0.0514(16) Uani 1 1 d . . . H20 H 0.5603 -0.1201 0.7440 0.062 Uiso 1 1 calc R . . C21 C 0.6068(5) -0.0068(5) 0.8074(3) 0.0437(14) Uani 1 1 d . . . H21 H 0.5962 0.0444 0.7758 0.052 Uiso 1 1 calc R . . C22 C 0.5947(6) 0.2775(4) 1.0022(3) 0.0437(15) Uani 1 1 d . . . C23 C 0.5122(7) 0.3412(5) 1.0238(4) 0.0554(18) Uani 1 1 d . . . H23 H 0.5164 0.3605 1.0681 0.066 Uiso 1 1 calc R . . C24 C 0.4235(7) 0.3769(6) 0.9807(4) 0.062(2) Uani 1 1 d . . . H24 H 0.3629 0.4169 0.9956 0.075 Uiso 1 1 calc R . . C25 C 0.4237(6) 0.3539(5) 0.9161(4) 0.0550(18) Uani 1 1 d . . . H25 H 0.3649 0.3800 0.8855 0.066 Uiso 1 1 calc R . . C26 C 0.5112(5) 0.2918(4) 0.8957(3) 0.0411(14) Uani 1 1 d . . . C27 C 0.5328(5) 0.2760(4) 0.8275(3) 0.0392(13) Uani 1 1 d . . . C28 C 0.4571(6) 0.3091(5) 0.7765(4) 0.0549(17) Uani 1 1 d . . . H28 H 0.3837 0.3372 0.7844 0.066 Uiso 1 1 calc R . . C29 C 0.4889(7) 0.3011(6) 0.7135(4) 0.066(2) Uani 1 1 d . . . H29 H 0.4385 0.3241 0.6777 0.079 Uiso 1 1 calc R . . C30 C 0.5952(7) 0.2591(5) 0.7044(3) 0.0589(18) Uani 1 1 d . . . H30 H 0.6207 0.2534 0.6621 0.071 Uiso 1 1 calc R . . C31 C 0.6647(6) 0.2253(5) 0.7580(3) 0.0473(15) Uani 1 1 d . . . H31 H 0.7375 0.1952 0.7510 0.057 Uiso 1 1 calc R . . C32 C 0.991(5) -0.064(4) 0.9545(18) 0.14(3) Uiso 0.50 1 d PD . . H32A H 0.9445 -0.0357 0.9168 0.210 Uiso 0.50 1 calc PR . . H32B H 0.9514 -0.1236 0.9692 0.210 Uiso 0.50 1 calc PR . . H32C H 1.0687 -0.0818 0.9425 0.210 Uiso 0.50 1 calc PR . . C33 C 1.0000 0.0000 1.0000 0.181(15) Uiso 1 2 d SD . . N1 N 0.8304(4) 0.2431(3) 0.9591(2) 0.0386(11) Uani 1 1 d . . . N2 N 0.8733(4) 0.1343(4) 0.8591(3) 0.0416(12) Uani 1 1 d . . . N3 N 0.6957(4) 0.0788(3) 0.9869(2) 0.0369(11) Uani 1 1 d . . . N4 N 0.6401(4) 0.0190(4) 0.8680(2) 0.0391(11) Uani 1 1 d . . . N5 N 0.5902(4) 0.2507(3) 0.9392(2) 0.0376(11) Uani 1 1 d . . . N6 N 0.6360(4) 0.2322(4) 0.8187(2) 0.0411(12) Uani 1 1 d . . . N7 N 0.986(3) -0.0574(19) 0.9607(10) 0.14(2) Uani 0.50 1 d PD . . O1 O 0.6937(5) 0.2640(4) 1.1101(2) 0.0600(13) Uani 1 1 d . . . H1 H 0.6977 0.3263 1.1134 0.090 Uiso 1 1 calc R . . O2 O 0.5997(8) 0.5106(10) 0.8695(6) 0.177(5) Uani 1 1 d . . . O3 O 0.7340(9) 0.6166(5) 0.8792(5) 0.152(4) Uani 1 1 d . . . O4 O 0.7573(8) 0.4723(6) 0.9346(4) 0.126(3) Uani 1 1 d . . . O5 O 0.7479(13) 0.4661(12) 0.8259(8) 0.224(6) Uiso 1 1 d . . . O6 O 0.4022(9) -0.0181(8) 0.6598(5) 0.157(4) Uiso 1 1 d . . . O7 O 0.3551(7) 0.0846(7) 0.7389(4) 0.129(3) Uiso 1 1 d . . . O8 O 0.2066(5) 0.0436(4) 0.6622(3) 0.0738(15) Uani 1 1 d . . . O9 O 0.2889(7) -0.0745(6) 0.7368(4) 0.113(2) Uiso 1 1 d . . . Cl1 Cl 0.72548(16) 0.51568(13) 0.87520(9) 0.0578(5) Uani 1 1 d . . . Cl2 Cl 0.31062(15) 0.00886(12) 0.69961(8) 0.0510(5) Uani 1 1 d . . . Ni1 Ni 0.71160(6) 0.15877(5) 0.90251(3) 0.0348(3) 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 C1 0.061(4) 0.042(4) 0.030(3) -0.004(3) 0.005(3) -0.004(3) C2 0.062(4) 0.035(3) 0.032(3) -0.001(3) -0.002(3) -0.002(3) C3 0.067(5) 0.047(4) 0.052(4) -0.011(3) -0.006(3) -0.002(3) C4 0.063(5) 0.057(5) 0.067(5) -0.012(4) -0.012(4) -0.016(4) C5 0.054(4) 0.058(5) 0.066(5) -0.006(4) -0.005(3) -0.013(3) C6 0.046(3) 0.037(3) 0.045(4) 0.002(3) -0.004(3) -0.004(3) C7 0.039(3) 0.034(3) 0.051(4) 0.013(3) -0.002(3) 0.004(3) C8 0.056(4) 0.054(4) 0.063(5) 0.005(4) 0.015(3) -0.008(3) C9 0.061(5) 0.073(6) 0.074(6) 0.014(4) 0.019(4) 0.010(4) C10 0.060(4) 0.067(5) 0.056(4) -0.004(4) 0.015(3) 0.014(4) C11 0.059(4) 0.053(4) 0.045(4) -0.001(3) 0.008(3) 0.014(3) C12 0.054(4) 0.039(3) 0.040(4) 0.002(3) 0.001(3) 0.000(3) C13 0.069(4) 0.057(4) 0.030(3) 0.004(3) 0.005(3) -0.004(3) C14 0.081(5) 0.050(4) 0.044(4) 0.015(3) 0.008(3) -0.001(4) C15 0.074(4) 0.038(4) 0.052(4) 0.012(3) 0.006(3) -0.006(3) C16 0.047(3) 0.031(3) 0.044(4) 0.002(3) 0.006(3) -0.005(3) C17 0.042(3) 0.033(3) 0.048(4) 0.000(3) 0.005(3) -0.007(3) C18 0.073(5) 0.031(3) 0.060(5) 0.006(3) 0.020(4) -0.001(3) C19 0.065(4) 0.039(4) 0.064(5) -0.015(3) 0.018(4) -0.011(3) C20 0.056(4) 0.046(4) 0.052(4) -0.017(3) 0.003(3) -0.010(3) C21 0.051(4) 0.039(3) 0.040(4) 0.000(3) 0.000(3) -0.002(3) C22 0.059(4) 0.031(3) 0.043(4) -0.002(3) 0.016(3) 0.000(3) C23 0.076(5) 0.039(4) 0.054(4) -0.004(3) 0.026(4) -0.002(3) C24 0.063(4) 0.052(4) 0.077(6) 0.005(4) 0.035(4) 0.018(4) C25 0.055(4) 0.043(4) 0.069(5) 0.011(3) 0.015(3) 0.015(3) C26 0.042(3) 0.031(3) 0.051(4) 0.013(3) 0.006(3) -0.001(2) C27 0.044(3) 0.030(3) 0.044(4) 0.008(3) 0.006(3) -0.001(3) C28 0.048(4) 0.053(4) 0.062(5) -0.003(4) -0.004(3) 0.006(3) C29 0.073(5) 0.066(5) 0.055(5) 0.003(4) -0.025(4) 0.006(4) C30 0.081(5) 0.058(4) 0.038(4) 0.000(3) 0.003(3) 0.005(4) C31 0.056(4) 0.045(4) 0.041(4) 0.003(3) 0.006(3) 0.004(3) N1 0.049(3) 0.032(3) 0.035(3) 0.004(2) 0.001(2) -0.003(2) N2 0.047(3) 0.036(3) 0.043(3) 0.002(2) 0.004(2) 0.003(2) N3 0.051(3) 0.031(3) 0.029(3) 0.003(2) 0.007(2) 0.000(2) N4 0.044(3) 0.033(3) 0.040(3) 0.002(2) 0.001(2) -0.003(2) N5 0.046(3) 0.028(2) 0.039(3) -0.002(2) 0.011(2) 0.001(2) N6 0.048(3) 0.037(3) 0.038(3) 0.005(2) 0.006(2) -0.002(2) N7 0.118(18) 0.16(3) 0.15(3) 0.08(2) -0.017(12) 0.085(18) O1 0.091(4) 0.053(3) 0.037(3) -0.006(2) 0.012(2) -0.006(3) O2 0.107(6) 0.233(12) 0.183(11) -0.002(8) -0.029(6) -0.046(7) O3 0.210(9) 0.053(4) 0.199(10) 0.038(5) 0.044(8) 0.006(5) O4 0.191(8) 0.106(6) 0.080(5) 0.047(4) 0.016(5) 0.060(5) O8 0.076(3) 0.066(4) 0.075(4) 0.014(3) -0.015(3) -0.004(3) Cl1 0.0725(12) 0.0493(10) 0.0523(11) 0.0036(8) 0.0104(8) -0.0075(8) Cl2 0.0620(10) 0.0447(9) 0.0464(10) 0.0041(7) 0.0064(8) -0.0072(7) Ni1 0.0427(5) 0.0286(4) 0.0332(5) 0.0019(3) 0.0032(3) 0.0004(3) _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 C1 O1 1.397(7) . ? C1 C22 1.535(9) . ? C1 C12 1.539(9) . ? C1 C2 1.543(9) . ? C2 N1 1.328(7) . ? C2 C3 1.391(9) . ? C3 C4 1.357(11) . ? C3 H3 0.9500 . ? C4 C5 1.375(11) . ? C4 H4 0.9500 . ? C5 C6 1.408(9) . ? C5 H5 0.9500 . ? C6 N1 1.338(8) . ? C6 C7 1.483(9) . ? C7 N2 1.375(8) . ? C7 C8 1.379(9) . ? C8 C9 1.376(11) . ? C8 H8 0.9500 . ? C9 C10 1.375(11) . ? C9 H9 0.9500 . ? C10 C11 1.376(10) . ? C10 H10 0.9500 . ? C11 N2 1.331(8) . ? C11 H11 0.9500 . ? C12 N3 1.341(8) . ? C12 C13 1.379(9) . ? C13 C14 1.412(10) . ? C13 H13 0.9500 . ? C14 C15 1.374(10) . ? C14 H14 0.9500 . ? C15 C16 1.378(9) . ? C15 H15 0.9500 . ? C16 N3 1.342(7) . ? C16 C17 1.485(9) . ? C17 N4 1.350(8) . ? C17 C18 1.390(9) . ? C18 C19 1.398(10) . ? C18 H18 0.9500 . ? C19 C20 1.349(10) . ? C19 H19 0.9500 . ? C20 C21 1.396(9) . ? C20 H20 0.9500 . ? C21 N4 1.324(8) . ? C21 H21 0.9500 . ? C22 N5 1.350(8) . ? C22 C23 1.379(9) . ? C23 C24 1.379(11) . ? C23 H23 0.9500 . ? C24 C25 1.374(11) . ? C24 H24 0.9500 . ? C25 C26 1.398(9) . ? C25 H25 0.9500 . ? C26 N5 1.339(8) . ? C26 C27 1.469(9) . ? C27 N6 1.348(8) . ? C27 C28 1.381(9) . ? C28 C29 1.389(11) . ? C28 H28 0.9500 . ? C29 C30 1.370(10) . ? C29 H29 0.9500 . ? C30 C31 1.386(9) . ? C30 H30 0.9500 . ? C31 N6 1.330(8) . ? C31 H31 0.9500 . ? C32 C33 1.27(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N7 1.122(18) 3_757 ? C33 N7 1.122(18) . ? C33 C32 1.27(3) 3_757 ? N1 Ni1 2.057(5) . ? N2 Ni1 2.155(5) . ? N3 Ni1 2.072(4) . ? N4 Ni1 2.145(5) . ? N5 Ni1 2.055(4) . ? N6 Ni1 2.115(5) . ? O1 H1 0.8400 . ? O2 Cl1 1.438(9) . ? O3 Cl1 1.361(8) . ? O4 Cl1 1.381(7) . ? O5 Cl1 1.264(16) . ? O6 Cl2 1.437(10) . ? O7 Cl2 1.373(9) . ? O8 Cl2 1.442(5) . ? O9 Cl2 1.394(8) . ? 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 O1 C1 C22 111.3(5) . . ? O1 C1 C12 105.1(5) . . ? C22 C1 C12 108.8(5) . . ? O1 C1 C2 112.0(5) . . ? C22 C1 C2 108.2(5) . . ? C12 C1 C2 111.4(5) . . ? N1 C2 C3 121.5(6) . . ? N1 C2 C1 115.6(5) . . ? C3 C2 C1 122.9(6) . . ? C4 C3 C2 118.8(7) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 120.7(7) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 117.3(7) . . ? C4 C5 H5 121.4 . . ? C6 C5 H5 121.4 . . ? N1 C6 C5 121.6(6) . . ? N1 C6 C7 115.0(5) . . ? C5 C6 C7 122.9(6) . . ? N2 C7 C8 121.9(6) . . ? N2 C7 C6 114.3(5) . . ? C8 C7 C6 123.8(6) . . ? C9 C8 C7 119.7(7) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 118.4(7) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C11 C10 C9 119.6(7) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? N2 C11 C10 123.3(7) . . ? N2 C11 H11 118.3 . . ? C10 C11 H11 118.4 . . ? N3 C12 C13 122.3(6) . . ? N3 C12 C1 115.7(5) . . ? C13 C12 C1 122.0(6) . . ? C12 C13 C14 118.1(6) . . ? C12 C13 H13 120.9 . . ? C14 C13 H13 121.0 . . ? C15 C14 C13 118.5(6) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 120.0(6) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? N3 C16 C15 121.3(6) . . ? N3 C16 C17 113.8(5) . . ? C15 C16 C17 124.6(6) . . ? N4 C17 C18 121.5(6) . . ? N4 C17 C16 115.5(5) . . ? C18 C17 C16 122.9(6) . . ? C17 C18 C19 119.0(6) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C20 C19 C18 119.2(6) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 118.6(7) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? N4 C21 C20 123.5(6) . . ? N4 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? N5 C22 C23 120.6(6) . . ? N5 C22 C1 115.4(5) . . ? C23 C22 C1 123.9(6) . . ? C22 C23 C24 119.6(7) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 119.2(6) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 119.4(7) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? N5 C26 C25 120.2(6) . . ? N5 C26 C27 115.2(5) . . ? C25 C26 C27 124.2(6) . . ? N6 C27 C28 122.4(6) . . ? N6 C27 C26 114.7(5) . . ? C28 C27 C26 122.8(6) . . ? C27 C28 C29 119.7(6) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 118.0(7) . . ? C30 C29 H29 121.0 . . ? C28 C29 H29 121.0 . . ? C29 C30 C31 118.7(7) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? N6 C31 C30 124.2(6) . . ? N6 C31 H31 117.9 . . ? C30 C31 H31 117.9 . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.8 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.1 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N7 C33 N7 180.000(15) 3_757 . ? C32 C33 C32 180.000(18) . 3_757 ? C2 N1 C6 119.6(5) . . ? C2 N1 Ni1 123.7(4) . . ? C6 N1 Ni1 116.7(4) . . ? C11 N2 C7 117.0(6) . . ? C11 N2 Ni1 129.5(5) . . ? C7 N2 Ni1 111.7(4) . . ? C12 N3 C16 119.3(5) . . ? C12 N3 Ni1 122.8(4) . . ? C16 N3 Ni1 117.5(4) . . ? C21 N4 C17 118.1(5) . . ? C21 N4 Ni1 127.9(4) . . ? C17 N4 Ni1 112.6(4) . . ? C26 N5 C22 120.4(5) . . ? C26 N5 Ni1 116.1(4) . . ? C22 N5 Ni1 123.2(4) . . ? C31 N6 C27 116.9(5) . . ? C31 N6 Ni1 128.7(4) . . ? C27 N6 Ni1 113.2(4) . . ? C1 O1 H1 109.5 . . ? O5 Cl1 O3 123.7(8) . . ? O5 Cl1 O4 116.2(8) . . ? O3 Cl1 O4 110.7(6) . . ? O5 Cl1 O2 100.5(8) . . ? O3 Cl1 O2 96.8(7) . . ? O4 Cl1 O2 103.8(6) . . ? O7 Cl2 O9 110.0(5) . . ? O7 Cl2 O6 106.0(6) . . ? O9 Cl2 O6 106.8(6) . . ? O7 Cl2 O8 109.0(4) . . ? O9 Cl2 O8 112.2(4) . . ? O6 Cl2 O8 112.7(5) . . ? N5 Ni1 N1 84.0(2) . . ? N5 Ni1 N3 83.53(19) . . ? N1 Ni1 N3 84.66(19) . . ? N5 Ni1 N6 77.34(19) . . ? N1 Ni1 N6 114.51(19) . . ? N3 Ni1 N6 150.87(19) . . ? N5 Ni1 N4 113.41(18) . . ? N1 Ni1 N4 152.38(19) . . ? N3 Ni1 N4 76.64(19) . . ? N6 Ni1 N4 90.96(19) . . ? N5 Ni1 N2 151.76(19) . . ? N1 Ni1 N2 76.8(2) . . ? N3 Ni1 N2 114.53(19) . . ? N6 Ni1 N2 91.97(19) . . ? N4 Ni1 N2 92.57(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 173.6(5) . . . . ? C22 C1 C2 N1 -63.4(7) . . . . ? C12 C1 C2 N1 56.2(7) . . . . ? O1 C1 C2 C3 -3.9(9) . . . . ? C22 C1 C2 C3 119.1(6) . . . . ? C12 C1 C2 C3 -121.3(7) . . . . ? N1 C2 C3 C4 3.8(10) . . . . ? C1 C2 C3 C4 -178.8(6) . . . . ? C2 C3 C4 C5 -7.1(11) . . . . ? C3 C4 C5 C6 4.1(11) . . . . ? C4 C5 C6 N1 2.4(10) . . . . ? C4 C5 C6 C7 -168.8(7) . . . . ? N1 C6 C7 N2 -5.4(8) . . . . ? C5 C6 C7 N2 166.4(6) . . . . ? N1 C6 C7 C8 177.2(6) . . . . ? C5 C6 C7 C8 -11.1(10) . . . . ? N2 C7 C8 C9 -4.3(10) . . . . ? C6 C7 C8 C9 173.0(6) . . . . ? C7 C8 C9 C10 2.0(11) . . . . ? C8 C9 C10 C11 0.5(11) . . . . ? C9 C10 C11 N2 -1.0(11) . . . . ? O1 C1 C12 N3 178.7(5) . . . . ? C22 C1 C12 N3 59.5(7) . . . . ? C2 C1 C12 N3 -59.7(7) . . . . ? O1 C1 C12 C13 0.6(8) . . . . ? C22 C1 C12 C13 -118.7(7) . . . . ? C2 C1 C12 C13 122.1(6) . . . . ? N3 C12 C13 C14 -1.9(10) . . . . ? C1 C12 C13 C14 176.1(6) . . . . ? C12 C13 C14 C15 -3.4(10) . . . . ? C13 C14 C15 C16 3.5(11) . . . . ? C14 C15 C16 N3 1.6(10) . . . . ? C14 C15 C16 C17 -171.7(6) . . . . ? N3 C16 C17 N4 -9.7(7) . . . . ? C15 C16 C17 N4 164.0(6) . . . . ? N3 C16 C17 C18 174.4(6) . . . . ? C15 C16 C17 C18 -11.9(10) . . . . ? N4 C17 C18 C19 -4.1(9) . . . . ? C16 C17 C18 C19 171.5(6) . . . . ? C17 C18 C19 C20 1.1(10) . . . . ? C18 C19 C20 C21 1.9(10) . . . . ? C19 C20 C21 N4 -2.1(10) . . . . ? O1 C1 C22 N5 -177.0(5) . . . . ? C12 C1 C22 N5 -61.6(7) . . . . ? C2 C1 C22 N5 59.5(7) . . . . ? O1 C1 C22 C23 6.2(8) . . . . ? C12 C1 C22 C23 121.5(6) . . . . ? C2 C1 C22 C23 -117.3(6) . . . . ? N5 C22 C23 C24 0.8(10) . . . . ? C1 C22 C23 C24 177.5(6) . . . . ? C22 C23 C24 C25 -4.6(11) . . . . ? C23 C24 C25 C26 2.4(11) . . . . ? C24 C25 C26 N5 3.7(10) . . . . ? C24 C25 C26 C27 -168.9(6) . . . . ? N5 C26 C27 N6 -7.3(7) . . . . ? C25 C26 C27 N6 165.7(6) . . . . ? N5 C26 C27 C28 176.8(6) . . . . ? C25 C26 C27 C28 -10.2(10) . . . . ? N6 C27 C28 C29 -2.5(10) . . . . ? C26 C27 C28 C29 173.1(6) . . . . ? C27 C28 C29 C30 0.6(11) . . . . ? C28 C29 C30 C31 1.1(11) . . . . ? C29 C30 C31 N6 -1.1(11) . . . . ? C3 C2 N1 C6 2.6(9) . . . . ? C1 C2 N1 C6 -174.9(5) . . . . ? C3 C2 N1 Ni1 -177.8(5) . . . . ? C1 C2 N1 Ni1 4.6(7) . . . . ? C5 C6 N1 C2 -5.7(9) . . . . ? C7 C6 N1 C2 166.2(5) . . . . ? C5 C6 N1 Ni1 174.7(5) . . . . ? C7 C6 N1 Ni1 -13.5(7) . . . . ? C10 C11 N2 C7 -1.1(10) . . . . ? C10 C11 N2 Ni1 162.1(5) . . . . ? C8 C7 N2 C11 3.8(9) . . . . ? C6 C7 N2 C11 -173.7(5) . . . . ? C8 C7 N2 Ni1 -162.4(5) . . . . ? C6 C7 N2 Ni1 20.1(6) . . . . ? C13 C12 N3 C16 7.1(9) . . . . ? C1 C12 N3 C16 -171.1(5) . . . . ? C13 C12 N3 Ni1 -179.8(5) . . . . ? C1 C12 N3 Ni1 2.1(7) . . . . ? C15 C16 N3 C12 -6.9(9) . . . . ? C17 C16 N3 C12 167.1(5) . . . . ? C15 C16 N3 Ni1 179.6(5) . . . . ? C17 C16 N3 Ni1 -6.4(6) . . . . ? C20 C21 N4 C17 -0.8(9) . . . . ? C20 C21 N4 Ni1 164.9(5) . . . . ? C18 C17 N4 C21 3.9(8) . . . . ? C16 C17 N4 C21 -172.0(5) . . . . ? C18 C17 N4 Ni1 -163.9(5) . . . . ? C16 C17 N4 Ni1 20.2(6) . . . . ? C25 C26 N5 C22 -7.6(8) . . . . ? C27 C26 N5 C22 165.6(5) . . . . ? C25 C26 N5 Ni1 178.8(5) . . . . ? C27 C26 N5 Ni1 -8.0(6) . . . . ? C23 C22 N5 C26 5.4(9) . . . . ? C1 C22 N5 C26 -171.6(5) . . . . ? C23 C22 N5 Ni1 178.5(4) . . . . ? C1 C22 N5 Ni1 1.6(7) . . . . ? C30 C31 N6 C27 -0.6(9) . . . . ? C30 C31 N6 Ni1 165.5(5) . . . . ? C28 C27 N6 C31 2.5(9) . . . . ? C26 C27 N6 C31 -173.5(5) . . . . ? C28 C27 N6 Ni1 -165.8(5) . . . . ? C26 C27 N6 Ni1 18.2(6) . . . . ? C26 N5 Ni1 N1 130.3(4) . . . . ? C22 N5 Ni1 N1 -43.1(5) . . . . ? C26 N5 Ni1 N3 -144.4(4) . . . . ? C22 N5 Ni1 N3 42.2(5) . . . . ? C26 N5 Ni1 N6 13.5(4) . . . . ? C22 N5 Ni1 N6 -160.0(5) . . . . ? C26 N5 Ni1 N4 -72.0(4) . . . . ? C22 N5 Ni1 N4 114.5(5) . . . . ? C26 N5 Ni1 N2 83.4(6) . . . . ? C22 N5 Ni1 N2 -90.0(6) . . . . ? C2 N1 Ni1 N5 39.8(5) . . . . ? C6 N1 Ni1 N5 -140.6(4) . . . . ? C2 N1 Ni1 N3 -44.2(5) . . . . ? C6 N1 Ni1 N3 135.4(4) . . . . ? C2 N1 Ni1 N6 112.9(5) . . . . ? C6 N1 Ni1 N6 -67.5(5) . . . . ? C2 N1 Ni1 N4 -91.5(6) . . . . ? C6 N1 Ni1 N4 88.1(6) . . . . ? C2 N1 Ni1 N2 -161.0(5) . . . . ? C6 N1 Ni1 N2 18.6(4) . . . . ? C12 N3 Ni1 N5 -44.3(5) . . . . ? C16 N3 Ni1 N5 129.0(4) . . . . ? C12 N3 Ni1 N1 40.2(5) . . . . ? C16 N3 Ni1 N1 -146.5(4) . . . . ? C12 N3 Ni1 N6 -93.2(6) . . . . ? C16 N3 Ni1 N6 80.0(6) . . . . ? C12 N3 Ni1 N4 -160.2(5) . . . . ? C16 N3 Ni1 N4 13.0(4) . . . . ? C12 N3 Ni1 N2 113.1(5) . . . . ? C16 N3 Ni1 N2 -73.7(5) . . . . ? C31 N6 Ni1 N5 176.3(6) . . . . ? C27 N6 Ni1 N5 -17.2(4) . . . . ? C31 N6 Ni1 N1 99.0(6) . . . . ? C27 N6 Ni1 N1 -94.4(4) . . . . ? C31 N6 Ni1 N3 -133.5(5) . . . . ? C27 N6 Ni1 N3 33.0(6) . . . . ? C31 N6 Ni1 N4 -69.9(5) . . . . ? C27 N6 Ni1 N4 96.6(4) . . . . ? C31 N6 Ni1 N2 22.7(5) . . . . ? C27 N6 Ni1 N2 -170.8(4) . . . . ? C21 N4 Ni1 N5 99.1(5) . . . . ? C17 N4 Ni1 N5 -94.5(4) . . . . ? C21 N4 Ni1 N1 -135.4(5) . . . . ? C17 N4 Ni1 N1 30.9(6) . . . . ? C21 N4 Ni1 N3 175.9(5) . . . . ? C17 N4 Ni1 N3 -17.8(4) . . . . ? C21 N4 Ni1 N6 22.5(5) . . . . ? C17 N4 Ni1 N6 -171.2(4) . . . . ? C21 N4 Ni1 N2 -69.5(5) . . . . ? C17 N4 Ni1 N2 96.8(4) . . . . ? C11 N2 Ni1 N5 -136.4(6) . . . . ? C7 N2 Ni1 N5 27.6(7) . . . . ? C11 N2 Ni1 N1 175.4(6) . . . . ? C7 N2 Ni1 N1 -20.6(4) . . . . ? C11 N2 Ni1 N3 97.6(6) . . . . ? C7 N2 Ni1 N3 -98.4(4) . . . . ? C11 N2 Ni1 N6 -69.9(6) . . . . ? C7 N2 Ni1 N6 94.1(4) . . . . ? C11 N2 Ni1 N4 21.1(6) . . . . ? C7 N2 Ni1 N4 -174.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.710 _refine_diff_density_min -1.000 _refine_diff_density_rms 0.132 # Attachment '5.cif' data_aja0716 _database_code_depnum_ccdc_archive 'CCDC 755785' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H22 Cu N6 O, C2 H3 N, 2(Cl O4)' _chemical_formula_sum 'C33 H25 Cl2 Cu N7 O9' _chemical_formula_weight 798.04 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 20.7459(4) _cell_length_b 12.2533(3) _cell_length_c 26.2774(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.3110(10) _cell_angle_gamma 90.00 _cell_volume 6591.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 66276 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3256 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6537 _exptl_absorpt_correction_T_max 0.8277 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27917 _diffrn_reflns_av_R_equivalents 0.0953 _diffrn_reflns_av_sigmaI/netI 0.0910 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.43 _reflns_number_total 7489 _reflns_number_gt 4441 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0753P)^2^+8.5659P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7489 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1203 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1732 _refine_ls_wR_factor_gt 0.1510 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 C1 C 0.0570(2) 0.4044(3) 0.11963(16) 0.0389(10) Uani 1 1 d . . . C2 C 0.08515(19) 0.3856(3) 0.07003(15) 0.0356(9) Uani 1 1 d . . . C3 C 0.0833(2) 0.4647(4) 0.03281(16) 0.0435(11) Uani 1 1 d . . . H3 H 0.0643 0.5338 0.0372 0.052 Uiso 1 1 calc R . . C4 C 0.1096(2) 0.4420(4) -0.01120(17) 0.0508(12) Uani 1 1 d . . . H4 H 0.1091 0.4960 -0.0372 0.061 Uiso 1 1 calc R . . C5 C 0.1363(2) 0.3422(4) -0.01716(16) 0.0488(12) Uani 1 1 d . . . H5 H 0.1545 0.3261 -0.0472 0.059 Uiso 1 1 calc R . . C6 C 0.1365(2) 0.2643(3) 0.02119(15) 0.0381(10) Uani 1 1 d . . . C7 C 0.1625(2) 0.1525(3) 0.01932(15) 0.0387(10) Uani 1 1 d . . . C8 C 0.1945(2) 0.1156(4) -0.02007(16) 0.0507(12) Uani 1 1 d . . . H8 H 0.1996 0.1626 -0.0479 0.061 Uiso 1 1 calc R . . C9 C 0.2184(2) 0.0122(4) -0.01854(17) 0.0516(12) Uani 1 1 d . . . H9 H 0.2403 -0.0136 -0.0453 0.062 Uiso 1 1 calc R . . C10 C 0.2107(2) -0.0549(4) 0.02197(17) 0.0520(12) Uani 1 1 d . . . H10 H 0.2265 -0.1278 0.0235 0.062 Uiso 1 1 calc R . . C11 C 0.1795(2) -0.0143(4) 0.06031(16) 0.0448(11) Uani 1 1 d . . . H11 H 0.1751 -0.0600 0.0887 0.054 Uiso 1 1 calc R . . C12 C 0.1049(2) 0.3751(3) 0.16769(15) 0.0362(9) Uani 1 1 d . . . C13 C 0.1269(2) 0.4476(4) 0.20716(17) 0.0450(11) Uani 1 1 d . . . H13 H 0.1153 0.5226 0.2040 0.054 Uiso 1 1 calc R . . C14 C 0.1657(2) 0.4093(4) 0.25112(17) 0.0484(12) Uani 1 1 d . . . H14 H 0.1825 0.4587 0.2779 0.058 Uiso 1 1 calc R . . C15 C 0.1803(2) 0.2997(4) 0.25637(17) 0.0427(10) Uani 1 1 d . . . H15 H 0.2056 0.2721 0.2871 0.051 Uiso 1 1 calc R . . C16 C 0.15717(19) 0.2308(3) 0.21580(15) 0.0368(10) Uani 1 1 d . . . C17 C 0.16075(19) 0.1102(3) 0.21754(14) 0.0340(9) Uani 1 1 d . . . C18 C 0.1855(2) 0.0527(4) 0.26155(15) 0.0401(10) Uani 1 1 d . . . H18 H 0.2061 0.0900 0.2915 0.048 Uiso 1 1 calc R . . C19 C 0.1800(2) -0.0600(4) 0.26147(17) 0.0490(12) Uani 1 1 d . . . H19 H 0.1973 -0.1011 0.2912 0.059 Uiso 1 1 calc R . . C20 C 0.1491(2) -0.1115(4) 0.21762(17) 0.0447(11) Uani 1 1 d . . . H20 H 0.1436 -0.1884 0.2170 0.054 Uiso 1 1 calc R . . C21 C 0.1261(2) -0.0494(3) 0.17462(16) 0.0395(10) Uani 1 1 d . . . H21 H 0.1056 -0.0856 0.1443 0.047 Uiso 1 1 calc R . . C22 C -0.0054(2) 0.3330(3) 0.11806(16) 0.0407(10) Uani 1 1 d . . . C23 C -0.0648(2) 0.3764(4) 0.12417(16) 0.0447(11) Uani 1 1 d . . . H23 H -0.0688 0.4524 0.1301 0.054 Uiso 1 1 calc R . . C24 C -0.1180(2) 0.3102(4) 0.12166(17) 0.0496(12) Uani 1 1 d . . . H24 H -0.1595 0.3392 0.1253 0.060 Uiso 1 1 calc R . . C25 C -0.1101(2) 0.1996(5) 0.11377(17) 0.0535(12) Uani 1 1 d . . . H25 H -0.1464 0.1516 0.1118 0.064 Uiso 1 1 calc R . . C26 C -0.0482(2) 0.1588(4) 0.10873(16) 0.0429(11) Uani 1 1 d . . . C27 C -0.0364(2) 0.0418(4) 0.09910(17) 0.0492(12) Uani 1 1 d . . . C28 C -0.0692(3) -0.0376(5) 0.1210(2) 0.0785(17) Uani 1 1 d . . . H28 H -0.1003 -0.0203 0.1427 0.094 Uiso 1 1 calc R . . C29 C -0.0545(4) -0.1467(6) 0.1099(4) 0.106(3) Uani 1 1 d . . . H29 H -0.0752 -0.2048 0.1249 0.127 Uiso 1 1 calc R . . C30 C -0.0113(3) -0.1687(5) 0.0781(3) 0.0803(19) Uani 1 1 d . . . H30 H -0.0022 -0.2419 0.0696 0.096 Uiso 1 1 calc R . . C31 C 0.0186(3) -0.0848(5) 0.0586(2) 0.0754(17) Uani 1 1 d . . . H31 H 0.0488 -0.1009 0.0360 0.090 Uiso 1 1 calc R . . C34 C 0.0000 0.6312(11) 0.2500 0.114(4) Uani 1 2 d S . . C35 C 0.0000 0.7484(13) 0.2500 0.102(3) Uani 1 2 d S . . C36 C 0.0000 1.0952(10) 0.2500 0.083(3) Uani 1 2 d S . . C37 C 0.0000 1.2113(12) 0.2500 0.083(3) Uani 1 2 d S . . N1 N 0.11100(16) 0.2871(3) 0.06408(12) 0.0339(8) Uani 1 1 d . . . N2 N 0.15489(18) 0.0879(3) 0.05933(12) 0.0403(8) Uani 1 1 d . . . N3 N 0.12256(16) 0.2702(3) 0.17200(12) 0.0350(8) Uani 1 1 d . . . N4 N 0.13163(16) 0.0596(3) 0.17373(12) 0.0353(8) Uani 1 1 d . . . N5 N 0.00339(16) 0.2253(3) 0.11037(12) 0.0386(8) Uani 1 1 d . . . N6 N 0.0082(2) 0.0204(3) 0.06916(16) 0.0617(11) Uani 1 1 d . . . N7 N 0.0000 0.8439(11) 0.2500 0.146(4) Uani 1 2 d S . . N8 N 0.0000 1.3089(10) 0.2500 0.104(3) Uani 1 2 d S . . O1 O 0.03484(14) 0.5134(2) 0.12195(12) 0.0482(8) Uani 1 1 d . . . H1 H 0.0665 0.5563 0.1224 0.072 Uiso 1 1 calc R . . O2 O 0.12348(16) 0.6834(3) 0.12402(15) 0.0677(10) Uani 1 1 d . . . O3 O 0.21302(17) 0.5717(3) 0.12157(12) 0.0602(9) Uani 1 1 d . . . O4 O 0.1758(2) 0.6853(3) 0.05191(12) 0.0686(11) Uani 1 1 d . . . O5 O 0.22605(15) 0.7618(3) 0.12951(12) 0.0557(9) Uani 1 1 d . . . O6 O -0.2247(2) -0.4452(3) 0.14701(15) 0.0983(14) Uani 1 1 d . . . O7 O -0.2206(3) -0.2604(3) 0.12933(16) 0.0987(15) Uani 1 1 d . . . O8 O -0.1794(2) -0.3275(3) 0.21175(12) 0.0675(10) Uani 1 1 d . . . O9 O -0.1271(2) -0.3704(4) 0.14211(16) 0.0928(14) Uani 1 1 d . . . Cl1 Cl 0.18515(5) 0.67545(8) 0.10652(4) 0.0409(3) Uani 1 1 d . . . Cl2 Cl -0.18742(6) -0.34577(9) 0.15747(4) 0.0457(3) Uani 1 1 d . . . Cu1 Cu 0.11114(2) 0.16342(4) 0.113443(17) 0.03483(17) Uani 1 1 d . . . H34A H -0.0188 0.6024 0.2796 0.052 Uiso 0.50 1 d P . . H34B H 0.0449 0.6024 0.2524 0.052 Uiso 0.50 1 d P . . H34C H -0.0262 0.6024 0.2180 0.052 Uiso 0.50 1 d P . . H36A H -0.0058 1.0674 0.2144 0.052 Uiso 0.50 1 d P . . H36B H -0.0359 1.0674 0.2668 0.052 Uiso 0.50 1 d P . . H36C H 0.0417 1.0674 0.2688 0.052 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 C1 0.041(3) 0.029(2) 0.047(2) 0.0017(19) 0.010(2) 0.0022(19) C2 0.033(2) 0.038(2) 0.036(2) 0.0033(19) 0.0047(18) -0.0049(19) C3 0.042(3) 0.039(2) 0.048(3) 0.005(2) 0.003(2) -0.006(2) C4 0.066(3) 0.046(3) 0.039(3) 0.011(2) 0.004(2) -0.008(2) C5 0.065(3) 0.050(3) 0.033(2) 0.006(2) 0.012(2) -0.008(2) C6 0.042(3) 0.044(3) 0.028(2) 0.0020(18) 0.0035(19) -0.009(2) C7 0.046(3) 0.043(3) 0.028(2) -0.0016(18) 0.0068(19) -0.008(2) C8 0.067(3) 0.054(3) 0.033(2) -0.005(2) 0.017(2) -0.010(3) C9 0.064(3) 0.056(3) 0.038(2) -0.012(2) 0.018(2) -0.005(3) C10 0.065(3) 0.046(3) 0.048(3) -0.009(2) 0.016(2) 0.002(2) C11 0.062(3) 0.042(3) 0.033(2) -0.0002(19) 0.012(2) 0.000(2) C12 0.037(2) 0.035(2) 0.039(2) -0.0013(19) 0.014(2) -0.0010(19) C13 0.048(3) 0.038(2) 0.052(3) -0.005(2) 0.019(2) -0.003(2) C14 0.053(3) 0.049(3) 0.044(3) -0.014(2) 0.009(2) -0.012(2) C15 0.035(2) 0.054(3) 0.038(2) -0.004(2) 0.002(2) -0.006(2) C16 0.030(2) 0.050(3) 0.031(2) -0.0027(19) 0.0082(19) 0.0007(19) C17 0.032(2) 0.040(2) 0.031(2) 0.0012(18) 0.0084(18) 0.0036(18) C18 0.039(2) 0.054(3) 0.028(2) -0.0045(19) 0.0059(19) 0.006(2) C19 0.056(3) 0.060(3) 0.034(2) 0.014(2) 0.014(2) 0.016(2) C20 0.051(3) 0.041(2) 0.044(3) 0.006(2) 0.015(2) 0.005(2) C21 0.044(3) 0.042(2) 0.034(2) 0.0038(19) 0.008(2) -0.003(2) C22 0.044(3) 0.045(3) 0.034(2) 0.007(2) 0.008(2) 0.000(2) C23 0.044(3) 0.053(3) 0.037(2) 0.008(2) 0.008(2) 0.003(2) C24 0.042(3) 0.066(3) 0.042(3) 0.009(2) 0.008(2) 0.004(2) C25 0.039(3) 0.076(4) 0.044(3) 0.004(2) 0.002(2) -0.011(2) C26 0.044(3) 0.051(3) 0.031(2) 0.009(2) -0.0009(19) -0.008(2) C27 0.044(3) 0.055(3) 0.044(3) 0.009(2) -0.007(2) -0.011(2) C28 0.071(4) 0.067(4) 0.095(4) 0.016(3) 0.005(3) -0.026(3) C29 0.095(6) 0.073(5) 0.137(7) 0.031(4) -0.021(5) -0.036(4) C30 0.078(5) 0.047(3) 0.102(5) -0.005(3) -0.029(4) -0.010(3) C31 0.094(5) 0.049(3) 0.074(4) -0.009(3) -0.014(3) 0.004(3) C34 0.083(7) 0.144(11) 0.115(9) 0.000 0.020(6) 0.000 C35 0.056(6) 0.122(9) 0.125(9) 0.000 0.007(6) 0.000 C36 0.056(5) 0.135(9) 0.064(5) 0.000 0.024(4) 0.000 C37 0.060(6) 0.137(9) 0.057(5) 0.000 0.020(4) 0.000 N1 0.038(2) 0.0353(19) 0.0289(17) 0.0059(14) 0.0073(15) -0.0011(16) N2 0.050(2) 0.042(2) 0.0297(18) -0.0054(16) 0.0075(16) -0.0019(17) N3 0.036(2) 0.041(2) 0.0288(18) 0.0008(15) 0.0086(15) -0.0022(16) N4 0.041(2) 0.039(2) 0.0268(17) 0.0027(15) 0.0081(15) 0.0021(16) N5 0.035(2) 0.047(2) 0.0331(18) 0.0058(16) 0.0045(15) -0.0047(17) N6 0.073(3) 0.053(3) 0.055(3) 0.004(2) 0.001(2) -0.001(2) N7 0.097(8) 0.166(11) 0.183(11) 0.000 0.046(8) 0.000 N8 0.091(6) 0.145(8) 0.080(6) 0.000 0.025(5) 0.000 O1 0.0456(18) 0.0380(17) 0.063(2) 0.0010(15) 0.0134(17) 0.0036(14) O2 0.047(2) 0.055(2) 0.104(3) -0.0168(19) 0.023(2) -0.0044(16) O3 0.081(3) 0.057(2) 0.0439(18) 0.0052(15) 0.0154(18) 0.0225(18) O4 0.111(3) 0.052(2) 0.0364(18) 0.0044(15) -0.0072(19) -0.014(2) O5 0.0475(19) 0.068(2) 0.0522(19) -0.0177(16) 0.0098(16) -0.0155(17) O6 0.120(4) 0.090(3) 0.072(3) 0.004(2) -0.025(3) -0.039(3) O7 0.157(4) 0.069(3) 0.075(3) 0.026(2) 0.032(3) 0.045(3) O8 0.108(3) 0.055(2) 0.0415(18) -0.0103(15) 0.019(2) 0.001(2) O9 0.098(3) 0.106(3) 0.087(3) 0.020(3) 0.051(3) 0.020(3) Cl1 0.0446(6) 0.0411(6) 0.0364(5) -0.0036(5) 0.0041(5) 0.0005(5) Cl2 0.0504(7) 0.0540(7) 0.0352(5) 0.0018(5) 0.0148(5) 0.0000(6) Cu1 0.0436(3) 0.0352(3) 0.0265(3) 0.0019(2) 0.0080(2) -0.0002(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. ; 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 C1 O1 1.416(5) . ? C1 C12 1.518(6) . ? C1 C2 1.530(5) . ? C1 C22 1.558(6) . ? C2 N1 1.340(5) . ? C2 C3 1.373(6) . ? C3 C4 1.385(6) . ? C3 H3 0.9500 . ? C4 C5 1.361(6) . ? C4 H4 0.9500 . ? C5 C6 1.388(6) . ? C5 H5 0.9500 . ? C6 N1 1.349(5) . ? C6 C7 1.476(6) . ? C7 N2 1.346(5) . ? C7 C8 1.392(6) . ? C8 C9 1.359(6) . ? C8 H8 0.9500 . ? C9 C10 1.375(6) . ? C9 H9 0.9500 . ? C10 C11 1.375(6) . ? C10 H10 0.9500 . ? C11 N2 1.351(5) . ? C11 H11 0.9500 . ? C12 N3 1.337(5) . ? C12 C13 1.385(6) . ? C13 C14 1.380(6) . ? C13 H13 0.9500 . ? C14 C15 1.379(6) . ? C14 H14 0.9500 . ? C15 C16 1.383(6) . ? C15 H15 0.9500 . ? C16 N3 1.344(5) . ? C16 C17 1.480(6) . ? C17 N4 1.360(5) . ? C17 C18 1.380(6) . ? C18 C19 1.386(6) . ? C18 H18 0.9500 . ? C19 C20 1.378(6) . ? C19 H19 0.9500 . ? C20 C21 1.381(6) . ? C20 H20 0.9500 . ? C21 N4 1.341(5) . ? C21 H21 0.9500 . ? C22 N5 1.352(5) . ? C22 C23 1.376(6) . ? C23 C24 1.362(6) . ? C23 H23 0.9500 . ? C24 C25 1.384(7) . ? C24 H24 0.9500 . ? C25 C26 1.404(6) . ? C25 H25 0.9500 . ? C26 N5 1.340(5) . ? C26 C27 1.484(6) . ? C27 N6 1.335(6) . ? C27 C28 1.366(7) . ? C28 C29 1.412(9) . ? C28 H28 0.9500 . ? C29 C30 1.349(10) . ? C29 H29 0.9500 . ? C30 C31 1.344(8) . ? C30 H30 0.9500 . ? C31 N6 1.344(6) . ? C31 H31 0.9500 . ? C34 C35 1.436(17) . ? C34 H34A 0.989(5) . ? C34 H34B 0.989(5) . ? C34 H34C 0.989(5) . ? C35 N7 1.171(14) . ? C36 C37 1.422(16) . ? C36 H36A 0.985(4) . ? C36 H36B 0.985(4) . ? C36 H36C 0.985(4) . ? C37 N8 1.196(13) . ? N1 Cu1 1.995(3) . ? N2 Cu1 2.030(3) . ? N3 Cu1 2.005(3) . ? N4 Cu1 2.023(3) . ? N5 Cu1 2.350(3) . ? N6 Cu1 2.860(4) . ? O1 H1 0.8400 . ? O2 Cl1 1.431(3) . ? O3 Cl1 1.425(3) . ? O4 Cl1 1.422(3) . ? O5 Cl1 1.428(3) . ? O6 Cl2 1.445(4) . ? O7 Cl2 1.397(4) . ? O8 Cl2 1.426(3) . ? O9 Cl2 1.408(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 O1 C1 C12 111.1(3) . . ? O1 C1 C2 110.5(3) . . ? C12 C1 C2 112.6(3) . . ? O1 C1 C22 104.9(3) . . ? C12 C1 C22 108.6(3) . . ? C2 C1 C22 108.9(3) . . ? N1 C2 C3 121.2(4) . . ? N1 C2 C1 116.8(3) . . ? C3 C2 C1 122.0(4) . . ? C2 C3 C4 119.0(4) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 119.2(4) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? N1 C6 C5 120.6(4) . . ? N1 C6 C7 114.5(3) . . ? C5 C6 C7 124.9(4) . . ? N2 C7 C8 121.3(4) . . ? N2 C7 C6 115.5(3) . . ? C8 C7 C6 123.2(4) . . ? C9 C8 C7 119.8(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.5(4) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 C11 118.6(4) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? N2 C11 C10 122.9(4) . . ? N2 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? N3 C12 C13 120.0(4) . . ? N3 C12 C1 115.6(3) . . ? C13 C12 C1 124.3(4) . . ? C14 C13 C12 119.1(4) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C15 C14 C13 120.3(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 118.3(4) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? N3 C16 C15 120.8(4) . . ? N3 C16 C17 113.7(3) . . ? C15 C16 C17 125.2(4) . . ? N4 C17 C18 122.1(4) . . ? N4 C17 C16 114.6(3) . . ? C18 C17 C16 123.0(4) . . ? C17 C18 C19 119.2(4) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C20 C19 C18 119.0(4) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 119.0(4) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? N4 C21 C20 122.9(4) . . ? N4 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? N5 C22 C23 122.7(4) . . ? N5 C22 C1 114.9(4) . . ? C23 C22 C1 122.4(4) . . ? C24 C23 C22 119.9(5) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 118.4(5) . . ? C23 C24 H24 120.8 . . ? C25 C24 H24 120.8 . . ? C24 C25 C26 119.7(4) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? N5 C26 C25 121.2(4) . . ? N5 C26 C27 116.1(4) . . ? C25 C26 C27 122.6(4) . . ? N6 C27 C28 123.3(5) . . ? N6 C27 C26 116.1(4) . . ? C28 C27 C26 120.6(5) . . ? C27 C28 C29 116.6(6) . . ? C27 C28 H28 121.7 . . ? C29 C28 H28 121.7 . . ? C30 C29 C28 120.4(6) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 118.5(6) . . ? C31 C30 H30 120.7 . . ? C29 C30 H30 120.7 . . ? C30 C31 N6 123.7(6) . . ? C30 C31 H31 118.1 . . ? N6 C31 H31 118.1 . . ? C35 C34 H34A 110.9(8) . . ? C35 C34 H34B 110.9(7) . . ? H34A C34 H34B 108.0(8) . . ? C35 C34 H34C 110.9(8) . . ? H34A C34 H34C 108.0(8) . . ? H34B C34 H34C 108.0(8) . . ? N7 C35 C34 180.000(7) . . ? C37 C36 H36A 110.2(7) . . ? C37 C36 H36B 110.2(7) . . ? H36A C36 H36B 108.7(7) . . ? C37 C36 H36C 110.2(7) . . ? H36A C36 H36C 108.7(7) . . ? H36B C36 H36C 108.7(7) . . ? N8 C37 C36 180.000(8) . . ? C2 N1 C6 120.2(3) . . ? C2 N1 Cu1 124.5(2) . . ? C6 N1 Cu1 115.2(3) . . ? C7 N2 C11 117.9(3) . . ? C7 N2 Cu1 113.7(3) . . ? C11 N2 Cu1 128.3(3) . . ? C12 N3 C16 121.3(3) . . ? C12 N3 Cu1 124.5(3) . . ? C16 N3 Cu1 113.8(3) . . ? C21 N4 C17 117.8(3) . . ? C21 N4 Cu1 129.2(3) . . ? C17 N4 Cu1 112.6(3) . . ? C26 N5 C22 118.1(4) . . ? C26 N5 Cu1 123.8(3) . . ? C22 N5 Cu1 117.4(3) . . ? C27 N6 C31 117.4(5) . . ? C27 N6 Cu1 100.6(3) . . ? C31 N6 Cu1 122.6(4) . . ? C1 O1 H1 109.5 . . ? O4 Cl1 O3 109.8(2) . . ? O4 Cl1 O5 109.8(2) . . ? O3 Cl1 O5 110.9(2) . . ? O4 Cl1 O2 109.6(2) . . ? O3 Cl1 O2 108.3(2) . . ? O5 Cl1 O2 108.3(2) . . ? O7 Cl2 O9 113.2(3) . . ? O7 Cl2 O8 112.3(2) . . ? O9 Cl2 O8 110.8(3) . . ? O7 Cl2 O6 109.1(3) . . ? O9 Cl2 O6 103.8(3) . . ? O8 Cl2 O6 107.2(2) . . ? N1 Cu1 N3 89.47(13) . . ? N1 Cu1 N4 164.87(14) . . ? N3 Cu1 N4 79.97(13) . . ? N1 Cu1 N2 81.05(13) . . ? N3 Cu1 N2 145.56(14) . . ? N4 Cu1 N2 101.59(13) . . ? N1 Cu1 N5 80.28(12) . . ? N3 Cu1 N5 79.01(13) . . ? N4 Cu1 N5 107.94(12) . . ? N2 Cu1 N5 130.83(13) . . ? N1 Cu1 N6 106.17(12) . . ? N3 Cu1 N6 134.43(13) . . ? N4 Cu1 N6 88.95(13) . . ? N2 Cu1 N6 79.90(13) . . ? N5 Cu1 N6 62.62(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 176.7(3) . . . . ? C12 C1 C2 N1 51.8(5) . . . . ? C22 C1 C2 N1 -68.6(4) . . . . ? O1 C1 C2 C3 -4.3(6) . . . . ? C12 C1 C2 C3 -129.2(4) . . . . ? C22 C1 C2 C3 110.4(4) . . . . ? N1 C2 C3 C4 -0.9(6) . . . . ? C1 C2 C3 C4 -179.9(4) . . . . ? C2 C3 C4 C5 0.5(7) . . . . ? C3 C4 C5 C6 0.1(7) . . . . ? C4 C5 C6 N1 -0.4(7) . . . . ? C4 C5 C6 C7 178.8(4) . . . . ? N1 C6 C7 N2 2.6(5) . . . . ? C5 C6 C7 N2 -176.7(4) . . . . ? N1 C6 C7 C8 -175.7(4) . . . . ? C5 C6 C7 C8 5.0(7) . . . . ? N2 C7 C8 C9 0.3(7) . . . . ? C6 C7 C8 C9 178.6(4) . . . . ? C7 C8 C9 C10 0.0(7) . . . . ? C8 C9 C10 C11 -0.9(7) . . . . ? C9 C10 C11 N2 1.5(7) . . . . ? O1 C1 C12 N3 172.3(3) . . . . ? C2 C1 C12 N3 -63.2(4) . . . . ? C22 C1 C12 N3 57.4(4) . . . . ? O1 C1 C12 C13 -3.5(5) . . . . ? C2 C1 C12 C13 121.0(4) . . . . ? C22 C1 C12 C13 -118.4(4) . . . . ? N3 C12 C13 C14 -1.5(6) . . . . ? C1 C12 C13 C14 174.1(4) . . . . ? C12 C13 C14 C15 -2.5(6) . . . . ? C13 C14 C15 C16 2.5(6) . . . . ? C14 C15 C16 N3 1.4(6) . . . . ? C14 C15 C16 C17 -171.5(4) . . . . ? N3 C16 C17 N4 3.4(5) . . . . ? C15 C16 C17 N4 176.7(4) . . . . ? N3 C16 C17 C18 -170.3(4) . . . . ? C15 C16 C17 C18 3.1(6) . . . . ? N4 C17 C18 C19 -0.7(6) . . . . ? C16 C17 C18 C19 172.5(4) . . . . ? C17 C18 C19 C20 -1.0(6) . . . . ? C18 C19 C20 C21 1.9(7) . . . . ? C19 C20 C21 N4 -1.1(7) . . . . ? O1 C1 C22 N5 173.5(3) . . . . ? C12 C1 C22 N5 -67.7(4) . . . . ? C2 C1 C22 N5 55.2(4) . . . . ? O1 C1 C22 C23 -6.7(5) . . . . ? C12 C1 C22 C23 112.2(4) . . . . ? C2 C1 C22 C23 -125.0(4) . . . . ? N5 C22 C23 C24 -1.2(6) . . . . ? C1 C22 C23 C24 179.0(4) . . . . ? C22 C23 C24 C25 1.0(6) . . . . ? C23 C24 C25 C26 0.2(7) . . . . ? C24 C25 C26 N5 -1.4(7) . . . . ? C24 C25 C26 C27 -178.7(4) . . . . ? N5 C26 C27 N6 -32.2(6) . . . . ? C25 C26 C27 N6 145.2(4) . . . . ? N5 C26 C27 C28 146.5(5) . . . . ? C25 C26 C27 C28 -36.1(7) . . . . ? N6 C27 C28 C29 -1.0(8) . . . . ? C26 C27 C28 C29 -179.6(5) . . . . ? C27 C28 C29 C30 -1.6(10) . . . . ? C28 C29 C30 C31 1.9(10) . . . . ? C29 C30 C31 N6 0.4(9) . . . . ? C3 C2 N1 C6 0.7(6) . . . . ? C1 C2 N1 C6 179.6(4) . . . . ? C3 C2 N1 Cu1 -175.9(3) . . . . ? C1 C2 N1 Cu1 3.0(5) . . . . ? C5 C6 N1 C2 0.0(6) . . . . ? C7 C6 N1 C2 -179.3(3) . . . . ? C5 C6 N1 Cu1 176.9(3) . . . . ? C7 C6 N1 Cu1 -2.4(5) . . . . ? C8 C7 N2 C11 0.2(6) . . . . ? C6 C7 N2 C11 -178.2(4) . . . . ? C8 C7 N2 Cu1 176.8(3) . . . . ? C6 C7 N2 Cu1 -1.6(5) . . . . ? C10 C11 N2 C7 -1.2(7) . . . . ? C10 C11 N2 Cu1 -177.2(4) . . . . ? C13 C12 N3 C16 5.5(6) . . . . ? C1 C12 N3 C16 -170.5(3) . . . . ? C13 C12 N3 Cu1 -166.4(3) . . . . ? C1 C12 N3 Cu1 17.7(5) . . . . ? C15 C16 N3 C12 -5.5(6) . . . . ? C17 C16 N3 C12 168.2(3) . . . . ? C15 C16 N3 Cu1 167.2(3) . . . . ? C17 C16 N3 Cu1 -19.2(4) . . . . ? C20 C21 N4 C17 -0.5(6) . . . . ? C20 C21 N4 Cu1 172.3(3) . . . . ? C18 C17 N4 C21 1.4(6) . . . . ? C16 C17 N4 C21 -172.3(3) . . . . ? C18 C17 N4 Cu1 -172.5(3) . . . . ? C16 C17 N4 Cu1 13.8(4) . . . . ? C25 C26 N5 C22 1.3(6) . . . . ? C27 C26 N5 C22 178.7(4) . . . . ? C25 C26 N5 Cu1 171.5(3) . . . . ? C27 C26 N5 Cu1 -11.0(5) . . . . ? C23 C22 N5 C26 0.0(6) . . . . ? C1 C22 N5 C26 179.8(3) . . . . ? C23 C22 N5 Cu1 -170.9(3) . . . . ? C1 C22 N5 Cu1 9.0(4) . . . . ? C28 C27 N6 C31 3.2(7) . . . . ? C26 C27 N6 C31 -178.1(4) . . . . ? C28 C27 N6 Cu1 -132.3(4) . . . . ? C26 C27 N6 Cu1 46.3(4) . . . . ? C30 C31 N6 C27 -2.9(8) . . . . ? C30 C31 N6 Cu1 122.3(6) . . . . ? C2 N1 Cu1 N3 -35.3(3) . . . . ? C6 N1 Cu1 N3 148.0(3) . . . . ? C2 N1 Cu1 N4 -80.7(6) . . . . ? C6 N1 Cu1 N4 102.6(5) . . . . ? C2 N1 Cu1 N2 178.0(3) . . . . ? C6 N1 Cu1 N2 1.2(3) . . . . ? C2 N1 Cu1 N5 43.7(3) . . . . ? C6 N1 Cu1 N5 -133.1(3) . . . . ? C2 N1 Cu1 N6 101.3(3) . . . . ? C6 N1 Cu1 N6 -75.5(3) . . . . ? C12 N3 Cu1 N1 24.1(3) . . . . ? C16 N3 Cu1 N1 -148.2(3) . . . . ? C12 N3 Cu1 N4 -166.7(3) . . . . ? C16 N3 Cu1 N4 20.9(3) . . . . ? C12 N3 Cu1 N2 97.4(4) . . . . ? C16 N3 Cu1 N2 -75.0(4) . . . . ? C12 N3 Cu1 N5 -56.1(3) . . . . ? C16 N3 Cu1 N5 131.5(3) . . . . ? C12 N3 Cu1 N6 -88.3(3) . . . . ? C16 N3 Cu1 N6 99.4(3) . . . . ? C21 N4 Cu1 N1 -145.4(5) . . . . ? C17 N4 Cu1 N1 27.7(6) . . . . ? C21 N4 Cu1 N3 168.3(4) . . . . ? C17 N4 Cu1 N3 -18.6(3) . . . . ? C21 N4 Cu1 N2 -46.7(4) . . . . ? C17 N4 Cu1 N2 126.3(3) . . . . ? C21 N4 Cu1 N5 93.4(4) . . . . ? C17 N4 Cu1 N5 -93.5(3) . . . . ? C21 N4 Cu1 N6 32.7(4) . . . . ? C17 N4 Cu1 N6 -154.2(3) . . . . ? C7 N2 Cu1 N1 0.3(3) . . . . ? C11 N2 Cu1 N1 176.4(4) . . . . ? C7 N2 Cu1 N3 -75.5(4) . . . . ? C11 N2 Cu1 N3 100.7(4) . . . . ? C7 N2 Cu1 N4 -164.6(3) . . . . ? C11 N2 Cu1 N4 11.5(4) . . . . ? C7 N2 Cu1 N5 69.0(3) . . . . ? C11 N2 Cu1 N5 -114.8(4) . . . . ? C7 N2 Cu1 N6 108.6(3) . . . . ? C11 N2 Cu1 N6 -75.3(4) . . . . ? C26 N5 Cu1 N1 138.9(3) . . . . ? C22 N5 Cu1 N1 -50.8(3) . . . . ? C26 N5 Cu1 N3 -129.7(3) . . . . ? C22 N5 Cu1 N3 40.5(3) . . . . ? C26 N5 Cu1 N4 -54.2(3) . . . . ? C22 N5 Cu1 N4 116.1(3) . . . . ? C26 N5 Cu1 N2 69.8(3) . . . . ? C22 N5 Cu1 N2 -119.9(3) . . . . ? C26 N5 Cu1 N6 24.9(3) . . . . ? C22 N5 Cu1 N6 -164.8(3) . . . . ? C27 N6 Cu1 N1 -105.7(3) . . . . ? C31 N6 Cu1 N1 121.9(4) . . . . ? C27 N6 Cu1 N3 0.0(4) . . . . ? C31 N6 Cu1 N3 -132.4(4) . . . . ? C27 N6 Cu1 N4 74.8(3) . . . . ? C31 N6 Cu1 N4 -57.6(4) . . . . ? C27 N6 Cu1 N2 176.8(3) . . . . ? C31 N6 Cu1 N2 44.4(4) . . . . ? C27 N6 Cu1 N5 -36.1(3) . . . . ? C31 N6 Cu1 N5 -168.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.886 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.087 # Attachment '6.cif' data_platon_6 _database_code_depnum_ccdc_archive 'CCDC 755786' #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common aja0715 _chemical_melting_point ? _chemical_formula_moiety 'C31 H22 N6 O Zn, 2(Cl O4)' _chemical_formula_sum 'C31 H22 Cl2 N6 O9 Zn' _chemical_formula_weight 758.82 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.1983(3) _cell_length_b 13.3434(3) _cell_length_c 20.7361(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.7470(10) _cell_angle_gamma 90.00 _cell_volume 3082.89(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14101 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 1.038 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.653 _exptl_absorpt_correction_T_max 0.688 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22524 _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_sigmaI/netI 0.1204 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7051 _reflns_number_gt 4117 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0547P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7051 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 C1 C 0.3007(3) 0.2375(3) -0.04263(19) 0.0278(9) Uani 1 1 d . . . C2 C 0.3112(3) 0.1230(3) -0.04262(19) 0.0268(9) Uani 1 1 d . . . C3 C 0.3235(3) 0.0698(3) -0.0992(2) 0.0320(10) Uani 1 1 d . . . H3 H 0.3232 0.1035 -0.1396 0.038 Uiso 1 1 calc R . . C4 C 0.3364(4) -0.0332(3) -0.0956(2) 0.0359(11) Uani 1 1 d . . . H4 H 0.3429 -0.0715 -0.1337 0.043 Uiso 1 1 calc R . . C5 C 0.3397(4) -0.0798(3) -0.0360(2) 0.0320(10) Uani 1 1 d . . . H5 H 0.3498 -0.1504 -0.0328 0.038 Uiso 1 1 calc R . . C6 C 0.3282(3) -0.0232(3) 0.01928(19) 0.0252(9) Uani 1 1 d . . . C7 C 0.3415(3) -0.0625(3) 0.08605(19) 0.0234(9) Uani 1 1 d . . . C8 C 0.3571(4) -0.1641(3) 0.0998(2) 0.0338(11) Uani 1 1 d . . . H8 H 0.3500 -0.2120 0.0658 0.041 Uiso 1 1 calc R . . C9 C 0.3831(4) -0.1946(3) 0.1633(2) 0.0358(11) Uani 1 1 d . . . H9 H 0.3941 -0.2637 0.1733 0.043 Uiso 1 1 calc R . . C10 C 0.3928(3) -0.1246(3) 0.2116(2) 0.0329(10) Uani 1 1 d . . . H10A H 0.4131 -0.1434 0.2555 0.039 Uiso 1 1 calc R . . C11 C 0.3722(3) -0.0253(3) 0.1946(2) 0.0260(9) Uani 1 1 d . . . H11 H 0.3772 0.0231 0.2284 0.031 Uiso 1 1 calc R . . C12 C 0.4054(3) 0.2820(2) 0.00161(19) 0.0233(9) Uani 1 1 d . . . C13 C 0.4898(4) 0.3451(3) -0.0217(2) 0.0320(10) Uani 1 1 d . . . H13 H 0.4852 0.3627 -0.0663 0.038 Uiso 1 1 calc R . . C14 C 0.5799(4) 0.3812(3) 0.0217(2) 0.0374(11) Uani 1 1 d . . . H14 H 0.6404 0.4225 0.0066 0.045 Uiso 1 1 calc R . . C15 C 0.5849(4) 0.3593(3) 0.0860(2) 0.0340(11) Uani 1 1 d . . . H15 H 0.6479 0.3845 0.1157 0.041 Uiso 1 1 calc R . . C16 C 0.4947(3) 0.2987(3) 0.1073(2) 0.0240(9) Uani 1 1 d . . . C17 C 0.4781(3) 0.2818(3) 0.1760(2) 0.0260(9) Uani 1 1 d . . . C18 C 0.5514(4) 0.3262(3) 0.2258(2) 0.0359(11) Uani 1 1 d . . . H18 H 0.6199 0.3635 0.2164 0.043 Uiso 1 1 calc R . . C19 C 0.5248(4) 0.3162(3) 0.2887(2) 0.0401(11) Uani 1 1 d . . . H19 H 0.5747 0.3459 0.3233 0.048 Uiso 1 1 calc R . . C20 C 0.4246(4) 0.2623(3) 0.3007(2) 0.0362(10) Uani 1 1 d . . . H20 H 0.4025 0.2553 0.3435 0.043 Uiso 1 1 calc R . . C21 C 0.3572(3) 0.2188(3) 0.2487(2) 0.0310(10) Uani 1 1 d . . . H21 H 0.2889 0.1806 0.2572 0.037 Uiso 1 1 calc R . . C22 C 0.1818(3) 0.2712(3) -0.01787(19) 0.0268(9) Uani 1 1 d . . . C23 C 0.1023(4) 0.3345(3) -0.0542(2) 0.0366(11) Uani 1 1 d . . . H23 H 0.1177 0.3549 -0.0964 0.044 Uiso 1 1 calc R . . C24 C 0.0004(4) 0.3671(3) -0.0277(2) 0.0401(11) Uani 1 1 d . . . H24 H -0.0530 0.4128 -0.0509 0.048 Uiso 1 1 calc R . . C25 C -0.0229(4) 0.3329(3) 0.0323(2) 0.0380(11) Uani 1 1 d . . . H25 H -0.0922 0.3549 0.0511 0.046 Uiso 1 1 calc R . . C26 C 0.0560(3) 0.2659(3) 0.06494(19) 0.0254(9) Uani 1 1 d . . . C27 C 0.0326(3) 0.2145(2) 0.12530(18) 0.0235(9) Uani 1 1 d . . . C28 C -0.0720(3) 0.2289(3) 0.1549(2) 0.0321(10) Uani 1 1 d . . . H28 H -0.1283 0.2783 0.1386 0.038 Uiso 1 1 calc R . . C29 C -0.0941(4) 0.1722(3) 0.2072(2) 0.0352(11) Uani 1 1 d . . . H29 H -0.1649 0.1824 0.2281 0.042 Uiso 1 1 calc R . . C30 C -0.0120(3) 0.0997(3) 0.2293(2) 0.0313(10) Uani 1 1 d . . . H30 H -0.0270 0.0572 0.2644 0.038 Uiso 1 1 calc R . . C31 C 0.0914(3) 0.0902(3) 0.19988(19) 0.0295(9) Uani 1 1 d . . . H31 H 0.1489 0.0417 0.2161 0.035 Uiso 1 1 calc R . . N1 N 0.3114(3) 0.0774(2) 0.01460(15) 0.0234(7) Uani 1 1 d . . . N2 N 0.3458(3) 0.0070(2) 0.13396(15) 0.0223(7) Uani 1 1 d . . . N3 N 0.4101(3) 0.2589(2) 0.06468(16) 0.0227(7) Uani 1 1 d . . . N4 N 0.3816(3) 0.2270(2) 0.18778(15) 0.0236(7) Uani 1 1 d . . . N5 N 0.1587(3) 0.2385(2) 0.04062(14) 0.0211(7) Uani 1 1 d . . . N6 N 0.1152(3) 0.1467(2) 0.14884(15) 0.0240(7) Uani 1 1 d . . . O1 O 0.3067(3) 0.26559(19) -0.10752(12) 0.0373(7) Uani 1 1 d . . . H1 H 0.2905 0.3268 -0.1119 0.056 Uiso 1 1 calc R . . O2 O 0.2383(3) 0.4707(2) 0.06230(15) 0.0501(9) Uani 1 1 d . . . O3 O 0.2523(3) 0.4338(3) 0.17147(19) 0.0995(16) Uani 1 1 d . . . O4 O 0.4095(3) 0.5169(2) 0.13016(16) 0.0518(9) Uani 1 1 d . . . O5 O 0.2309(3) 0.5991(3) 0.1372(2) 0.0934(15) Uani 1 1 d . . . O6 O -0.1262(3) 0.5912(2) 0.24924(16) 0.0543(9) Uani 1 1 d . . . O7 O -0.1879(3) 0.4240(2) 0.23939(15) 0.0488(8) Uani 1 1 d . . . O8 O -0.2685(3) 0.54333(19) 0.16435(15) 0.0422(8) Uani 1 1 d . . . O9 O -0.0677(3) 0.4916(2) 0.16516(16) 0.0566(10) Uani 1 1 d . . . Cl02 Cl 0.28119(9) 0.50518(7) 0.12520(5) 0.0331(3) Uani 1 1 d . . . Cl03 Cl -0.16163(9) 0.51218(7) 0.20486(5) 0.0298(2) Uani 1 1 d . . . Zn1 Zn 0.28681(4) 0.15701(3) 0.10499(2) 0.02117(14) 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 C1 0.036(2) 0.029(2) 0.019(2) 0.0066(18) 0.0053(19) 0.0075(18) C2 0.030(2) 0.027(2) 0.024(2) 0.0042(18) 0.0003(18) 0.0059(18) C3 0.036(2) 0.035(2) 0.026(3) -0.0026(19) 0.007(2) 0.0058(19) C4 0.045(3) 0.038(2) 0.025(3) -0.013(2) 0.007(2) 0.004(2) C5 0.046(3) 0.025(2) 0.026(3) -0.0077(19) 0.006(2) 0.0058(19) C6 0.029(2) 0.027(2) 0.020(2) -0.0010(17) 0.0059(18) 0.0033(17) C7 0.025(2) 0.0232(19) 0.023(2) -0.0025(17) 0.0047(17) -0.0016(17) C8 0.041(3) 0.022(2) 0.040(3) -0.001(2) 0.011(2) 0.0045(19) C9 0.043(3) 0.028(2) 0.037(3) 0.010(2) 0.010(2) 0.008(2) C10 0.034(2) 0.031(2) 0.034(3) 0.009(2) 0.001(2) 0.0065(19) C11 0.024(2) 0.029(2) 0.025(3) 0.0021(18) 0.0020(18) -0.0006(17) C12 0.027(2) 0.0206(19) 0.024(2) 0.0035(17) 0.0087(18) 0.0104(17) C13 0.046(3) 0.0203(19) 0.033(3) 0.0041(19) 0.017(2) 0.006(2) C14 0.039(3) 0.029(2) 0.049(3) -0.003(2) 0.023(2) -0.008(2) C15 0.031(2) 0.027(2) 0.045(3) -0.011(2) 0.012(2) -0.0047(18) C16 0.022(2) 0.0167(17) 0.033(3) -0.0038(18) 0.0026(18) 0.0020(17) C17 0.020(2) 0.024(2) 0.034(3) -0.0033(18) 0.0017(18) 0.0014(17) C18 0.030(2) 0.037(2) 0.041(3) -0.001(2) 0.001(2) -0.004(2) C19 0.037(2) 0.039(2) 0.042(3) -0.010(2) -0.008(2) -0.016(2) C20 0.041(3) 0.044(2) 0.022(3) 0.000(2) -0.004(2) -0.003(2) C21 0.028(2) 0.029(2) 0.035(3) -0.001(2) -0.003(2) 0.0004(18) C22 0.037(2) 0.0208(19) 0.022(2) -0.0007(17) -0.0013(19) 0.0013(18) C23 0.044(3) 0.041(2) 0.025(3) 0.007(2) 0.002(2) 0.008(2) C24 0.042(3) 0.037(2) 0.039(3) 0.008(2) -0.008(2) 0.013(2) C25 0.037(2) 0.041(2) 0.037(3) 0.008(2) 0.007(2) 0.014(2) C26 0.025(2) 0.0237(19) 0.027(2) -0.0043(18) 0.0001(18) 0.0022(17) C27 0.025(2) 0.0191(18) 0.026(2) -0.0060(17) -0.0013(18) 0.0008(17) C28 0.026(2) 0.033(2) 0.037(3) -0.004(2) 0.0024(19) 0.0046(18) C29 0.030(2) 0.039(2) 0.039(3) -0.006(2) 0.010(2) -0.006(2) C30 0.034(2) 0.032(2) 0.029(3) -0.0002(19) 0.007(2) -0.009(2) C31 0.027(2) 0.031(2) 0.030(3) 0.0041(19) -0.0014(19) -0.0001(18) N1 0.0302(18) 0.0224(15) 0.0174(19) -0.0008(14) 0.0014(14) 0.0047(14) N2 0.0242(16) 0.0223(15) 0.0202(19) 0.0026(14) 0.0014(14) 0.0030(14) N3 0.0263(17) 0.0170(15) 0.026(2) 0.0019(14) 0.0091(15) 0.0050(14) N4 0.0255(17) 0.0242(16) 0.021(2) 0.0010(14) 0.0019(15) 0.0015(14) N5 0.0275(17) 0.0187(15) 0.0161(18) 0.0001(13) -0.0031(14) 0.0029(13) N6 0.0223(17) 0.0255(16) 0.024(2) 0.0014(14) -0.0005(14) -0.0045(14) O1 0.062(2) 0.0328(15) 0.0182(16) 0.0106(13) 0.0114(14) 0.0129(15) O2 0.063(2) 0.0563(19) 0.032(2) -0.0235(16) 0.0075(17) -0.0148(17) O3 0.064(3) 0.158(4) 0.079(3) 0.075(3) 0.018(2) -0.007(3) O4 0.0370(17) 0.066(2) 0.053(2) 0.0069(17) 0.0056(16) -0.0008(16) O5 0.083(3) 0.068(2) 0.118(4) -0.064(2) -0.045(2) 0.045(2) O6 0.054(2) 0.0492(18) 0.058(2) -0.0217(17) -0.0039(17) -0.0119(16) O7 0.0429(18) 0.0526(18) 0.049(2) 0.0255(16) -0.0033(15) -0.0155(15) O8 0.0408(17) 0.0369(16) 0.047(2) 0.0100(15) -0.0069(15) -0.0015(14) O9 0.063(2) 0.065(2) 0.046(2) 0.0177(17) 0.0295(18) 0.0277(18) Cl02 0.0370(6) 0.0337(5) 0.0292(6) -0.0016(5) 0.0058(5) 0.0073(5) Cl03 0.0307(5) 0.0307(5) 0.0280(6) 0.0023(4) 0.0040(5) -0.0028(4) Zn1 0.0233(2) 0.0199(2) 0.0203(3) 0.00023(19) 0.00197(19) 0.00105(19) _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 C1 O1 1.405(4) . ? C1 C2 1.533(5) . ? C1 C12 1.533(5) . ? C1 C22 1.542(5) . ? C2 N1 1.333(4) . ? C2 C3 1.390(5) . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.380(5) . ? C4 H4 0.9500 . ? C5 C6 1.390(5) . ? C5 H5 0.9500 . ? C6 N1 1.357(4) . ? C6 C7 1.474(5) . ? C7 N2 1.356(4) . ? C7 C8 1.392(5) . ? C8 C9 1.381(6) . ? C8 H8 0.9500 . ? C9 C10 1.366(6) . ? C9 H9 0.9500 . ? C10 C11 1.385(5) . ? C10 H10A 0.9500 . ? C11 N2 1.334(5) . ? C11 H11 0.9500 . ? C12 N3 1.339(4) . ? C12 C13 1.389(5) . ? C13 C14 1.371(6) . ? C13 H13 0.9500 . ? C14 C15 1.360(6) . ? C14 H14 0.9500 . ? C15 C16 1.399(5) . ? C15 H15 0.9500 . ? C16 N3 1.339(5) . ? C16 C17 1.472(5) . ? C17 N4 1.348(4) . ? C17 C18 1.387(5) . ? C18 C19 1.373(6) . ? C18 H18 0.9500 . ? C19 C20 1.376(5) . ? C19 H19 0.9500 . ? C20 C21 1.381(5) . ? C20 H20 0.9500 . ? C21 N4 1.323(5) . ? C21 H21 0.9500 . ? C22 N5 1.339(4) . ? C22 C23 1.392(5) . ? C23 C24 1.384(5) . ? C23 H23 0.9500 . ? C24 C25 1.375(6) . ? C24 H24 0.9500 . ? C25 C26 1.385(5) . ? C25 H25 0.9500 . ? C26 N5 1.351(4) . ? C26 C27 1.473(5) . ? C27 N6 1.349(4) . ? C27 C28 1.389(5) . ? C28 C29 1.367(5) . ? C28 H28 0.9500 . ? C29 C30 1.381(5) . ? C29 H29 0.9500 . ? C30 C31 1.368(5) . ? C30 H30 0.9500 . ? C31 N6 1.348(4) . ? C31 H31 0.9500 . ? N1 Zn1 2.196(3) . ? N2 Zn1 2.174(3) . ? N3 Zn1 2.164(3) . ? N4 Zn1 2.140(3) . ? N5 Zn1 2.154(3) . ? N6 Zn1 2.211(3) . ? O1 H1 0.8400 . ? O2 Cl02 1.421(3) . ? O3 Cl02 1.412(3) . ? O4 Cl02 1.439(3) . ? O5 Cl02 1.406(3) . ? O6 Cl03 1.429(3) . ? O7 Cl03 1.424(3) . ? O8 Cl03 1.452(3) . ? O9 Cl03 1.426(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 O1 C1 C2 104.8(3) . . ? O1 C1 C12 111.3(3) . . ? C2 C1 C12 109.4(3) . . ? O1 C1 C22 111.5(3) . . ? C2 C1 C22 111.1(3) . . ? C12 C1 C22 108.8(3) . . ? N1 C2 C3 121.8(3) . . ? N1 C2 C1 116.7(3) . . ? C3 C2 C1 121.5(3) . . ? C4 C3 C2 118.7(4) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C5 C4 C3 119.3(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 119.8(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? N1 C6 C5 120.2(3) . . ? N1 C6 C7 114.8(3) . . ? C5 C6 C7 124.9(3) . . ? N2 C7 C8 121.4(4) . . ? N2 C7 C6 115.9(3) . . ? C8 C7 C6 122.5(3) . . ? C9 C8 C7 119.5(4) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 119.4(4) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 117.9(4) . . ? C9 C10 H10A 121.0 . . ? C11 C10 H10A 121.0 . . ? N2 C11 C10 124.4(4) . . ? N2 C11 H11 117.8 . . ? C10 C11 H11 117.8 . . ? N3 C12 C13 121.2(4) . . ? N3 C12 C1 116.6(3) . . ? C13 C12 C1 122.2(4) . . ? C14 C13 C12 117.8(4) . . ? C14 C13 H13 121.1 . . ? C12 C13 H13 121.1 . . ? C15 C14 C13 121.6(4) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C16 118.2(4) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? N3 C16 C15 120.5(4) . . ? N3 C16 C17 115.3(3) . . ? C15 C16 C17 123.9(4) . . ? N4 C17 C18 121.5(4) . . ? N4 C17 C16 116.1(3) . . ? C18 C17 C16 122.2(3) . . ? C19 C18 C17 119.8(4) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 118.7(4) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C19 C20 C21 118.1(4) . . ? C19 C20 H20 121.0 . . ? C21 C20 H20 121.0 . . ? N4 C21 C20 124.2(4) . . ? N4 C21 H21 117.9 . . ? C20 C21 H21 117.9 . . ? N5 C22 C23 121.1(3) . . ? N5 C22 C1 117.3(3) . . ? C23 C22 C1 121.6(3) . . ? C24 C23 C22 119.0(4) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C25 C24 C23 119.5(4) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 119.2(4) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? N5 C26 C25 121.1(3) . . ? N5 C26 C27 114.9(3) . . ? C25 C26 C27 123.8(3) . . ? N6 C27 C28 120.7(3) . . ? N6 C27 C26 116.4(3) . . ? C28 C27 C26 122.7(3) . . ? C29 C28 C27 120.2(4) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 118.9(4) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C31 C30 C29 118.8(4) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? N6 C31 C30 122.8(4) . . ? N6 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? C2 N1 C6 120.2(3) . . ? C2 N1 Zn1 123.3(2) . . ? C6 N1 Zn1 116.5(2) . . ? C11 N2 C7 117.3(3) . . ? C11 N2 Zn1 126.2(2) . . ? C7 N2 Zn1 116.1(2) . . ? C16 N3 C12 120.6(3) . . ? C16 N3 Zn1 115.6(2) . . ? C12 N3 Zn1 123.9(3) . . ? C21 N4 C17 117.7(3) . . ? C21 N4 Zn1 126.6(3) . . ? C17 N4 Zn1 115.7(3) . . ? C22 N5 C26 119.9(3) . . ? C22 N5 Zn1 123.3(2) . . ? C26 N5 Zn1 116.4(2) . . ? C31 N6 C27 118.5(3) . . ? C31 N6 Zn1 127.3(2) . . ? C27 N6 Zn1 113.7(2) . . ? C1 O1 H1 109.5 . . ? O5 Cl02 O3 110.9(3) . . ? O5 Cl02 O2 110.3(2) . . ? O3 Cl02 O2 109.0(2) . . ? O5 Cl02 O4 107.8(2) . . ? O3 Cl02 O4 108.7(2) . . ? O2 Cl02 O4 110.12(19) . . ? O7 Cl03 O9 109.41(18) . . ? O7 Cl03 O6 110.1(2) . . ? O9 Cl03 O6 109.9(2) . . ? O7 Cl03 O8 109.13(17) . . ? O9 Cl03 O8 109.51(19) . . ? O6 Cl03 O8 108.73(18) . . ? N4 Zn1 N5 121.54(11) . . ? N4 Zn1 N3 75.62(12) . . ? N5 Zn1 N3 81.64(11) . . ? N4 Zn1 N2 93.86(11) . . ? N5 Zn1 N2 143.26(11) . . ? N3 Zn1 N2 119.80(10) . . ? N4 Zn1 N1 143.25(11) . . ? N5 Zn1 N1 81.26(11) . . ? N3 Zn1 N1 80.49(11) . . ? N2 Zn1 N1 74.31(11) . . ? N4 Zn1 N6 94.51(11) . . ? N5 Zn1 N6 74.56(11) . . ? N3 Zn1 N6 144.31(10) . . ? N2 Zn1 N6 94.70(10) . . ? N1 Zn1 N6 120.64(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 178.1(3) . . . . ? C12 C1 C2 N1 58.7(4) . . . . ? C22 C1 C2 N1 -61.4(5) . . . . ? O1 C1 C2 C3 0.0(5) . . . . ? C12 C1 C2 C3 -119.4(4) . . . . ? C22 C1 C2 C3 120.6(4) . . . . ? N1 C2 C3 C4 0.0(6) . . . . ? C1 C2 C3 C4 178.0(4) . . . . ? C2 C3 C4 C5 -1.7(6) . . . . ? C3 C4 C5 C6 1.0(6) . . . . ? C4 C5 C6 N1 1.3(6) . . . . ? C4 C5 C6 C7 -174.0(4) . . . . ? N1 C6 C7 N2 -5.6(5) . . . . ? C5 C6 C7 N2 170.0(3) . . . . ? N1 C6 C7 C8 178.8(3) . . . . ? C5 C6 C7 C8 -5.7(6) . . . . ? N2 C7 C8 C9 -3.0(6) . . . . ? C6 C7 C8 C9 172.4(3) . . . . ? C7 C8 C9 C10 0.1(6) . . . . ? C8 C9 C10 C11 2.0(6) . . . . ? C9 C10 C11 N2 -1.4(6) . . . . ? O1 C1 C12 N3 -179.0(3) . . . . ? C2 C1 C12 N3 -63.7(4) . . . . ? C22 C1 C12 N3 57.8(4) . . . . ? O1 C1 C12 C13 2.6(4) . . . . ? C2 C1 C12 C13 117.9(3) . . . . ? C22 C1 C12 C13 -120.6(3) . . . . ? N3 C12 C13 C14 1.5(5) . . . . ? C1 C12 C13 C14 179.9(3) . . . . ? C12 C13 C14 C15 -2.4(5) . . . . ? C13 C14 C15 C16 -0.2(5) . . . . ? C14 C15 C16 N3 3.8(5) . . . . ? C14 C15 C16 C17 -170.2(3) . . . . ? N3 C16 C17 N4 1.2(4) . . . . ? C15 C16 C17 N4 175.5(3) . . . . ? N3 C16 C17 C18 -173.7(3) . . . . ? C15 C16 C17 C18 0.5(5) . . . . ? N4 C17 C18 C19 -1.3(6) . . . . ? C16 C17 C18 C19 173.4(3) . . . . ? C17 C18 C19 C20 -0.4(6) . . . . ? C18 C19 C20 C21 1.5(6) . . . . ? C19 C20 C21 N4 -1.2(6) . . . . ? O1 C1 C22 N5 172.1(3) . . . . ? C2 C1 C22 N5 55.6(5) . . . . ? C12 C1 C22 N5 -64.8(4) . . . . ? O1 C1 C22 C23 -9.0(5) . . . . ? C2 C1 C22 C23 -125.5(4) . . . . ? C12 C1 C22 C23 114.1(4) . . . . ? N5 C22 C23 C24 2.8(6) . . . . ? C1 C22 C23 C24 -176.1(4) . . . . ? C22 C23 C24 C25 -3.0(6) . . . . ? C23 C24 C25 C26 -0.4(6) . . . . ? C24 C25 C26 N5 4.1(6) . . . . ? C24 C25 C26 C27 -171.9(4) . . . . ? N5 C26 C27 N6 -0.2(5) . . . . ? C25 C26 C27 N6 176.0(4) . . . . ? N5 C26 C27 C28 -176.0(3) . . . . ? C25 C26 C27 C28 0.2(6) . . . . ? N6 C27 C28 C29 -1.9(6) . . . . ? C26 C27 C28 C29 173.7(4) . . . . ? C27 C28 C29 C30 -1.0(6) . . . . ? C28 C29 C30 C31 2.9(6) . . . . ? C29 C30 C31 N6 -2.0(6) . . . . ? C3 C2 N1 C6 2.3(5) . . . . ? C1 C2 N1 C6 -175.7(3) . . . . ? C3 C2 N1 Zn1 -178.1(3) . . . . ? C1 C2 N1 Zn1 3.9(4) . . . . ? C5 C6 N1 C2 -3.0(5) . . . . ? C7 C6 N1 C2 172.8(3) . . . . ? C5 C6 N1 Zn1 177.4(3) . . . . ? C7 C6 N1 Zn1 -6.8(4) . . . . ? C10 C11 N2 C7 -1.4(5) . . . . ? C10 C11 N2 Zn1 170.3(3) . . . . ? C8 C7 N2 C11 3.6(5) . . . . ? C6 C7 N2 C11 -172.1(3) . . . . ? C8 C7 N2 Zn1 -168.9(3) . . . . ? C6 C7 N2 Zn1 15.4(4) . . . . ? C15 C16 N3 C12 -4.7(5) . . . . ? C17 C16 N3 C12 169.7(3) . . . . ? C15 C16 N3 Zn1 175.0(2) . . . . ? C17 C16 N3 Zn1 -10.6(4) . . . . ? C13 C12 N3 C16 2.0(5) . . . . ? C1 C12 N3 C16 -176.4(3) . . . . ? C13 C12 N3 Zn1 -177.6(2) . . . . ? C1 C12 N3 Zn1 3.9(4) . . . . ? C20 C21 N4 C17 -0.4(5) . . . . ? C20 C21 N4 Zn1 177.1(3) . . . . ? C18 C17 N4 C21 1.7(5) . . . . ? C16 C17 N4 C21 -173.3(3) . . . . ? C18 C17 N4 Zn1 -176.2(3) . . . . ? C16 C17 N4 Zn1 8.8(4) . . . . ? C23 C22 N5 C26 0.8(5) . . . . ? C1 C22 N5 C26 179.8(3) . . . . ? C23 C22 N5 Zn1 -171.6(3) . . . . ? C1 C22 N5 Zn1 7.4(4) . . . . ? C25 C26 N5 C22 -4.3(5) . . . . ? C27 C26 N5 C22 172.0(3) . . . . ? C25 C26 N5 Zn1 168.6(3) . . . . ? C27 C26 N5 Zn1 -15.1(4) . . . . ? C30 C31 N6 C27 -1.0(6) . . . . ? C30 C31 N6 Zn1 170.3(3) . . . . ? C28 C27 N6 C31 2.9(5) . . . . ? C26 C27 N6 C31 -173.0(3) . . . . ? C28 C27 N6 Zn1 -169.5(3) . . . . ? C26 C27 N6 Zn1 14.7(4) . . . . ? C21 N4 Zn1 N5 101.2(3) . . . . ? C17 N4 Zn1 N5 -81.2(3) . . . . ? C21 N4 Zn1 N3 171.7(3) . . . . ? C17 N4 Zn1 N3 -10.7(2) . . . . ? C21 N4 Zn1 N2 -68.5(3) . . . . ? C17 N4 Zn1 N2 109.1(2) . . . . ? C21 N4 Zn1 N1 -137.2(3) . . . . ? C17 N4 Zn1 N1 40.4(3) . . . . ? C21 N4 Zn1 N6 26.5(3) . . . . ? C17 N4 Zn1 N6 -155.9(2) . . . . ? C22 N5 Zn1 N4 104.0(3) . . . . ? C26 N5 Zn1 N4 -68.7(3) . . . . ? C22 N5 Zn1 N3 36.6(3) . . . . ? C26 N5 Zn1 N3 -136.1(3) . . . . ? C22 N5 Zn1 N2 -93.4(3) . . . . ? C26 N5 Zn1 N2 93.9(3) . . . . ? C22 N5 Zn1 N1 -45.0(3) . . . . ? C26 N5 Zn1 N1 142.4(3) . . . . ? C22 N5 Zn1 N6 -170.3(3) . . . . ? C26 N5 Zn1 N6 17.1(2) . . . . ? C16 N3 Zn1 N4 11.5(2) . . . . ? C12 N3 Zn1 N4 -168.9(3) . . . . ? C16 N3 Zn1 N5 137.2(2) . . . . ? C12 N3 Zn1 N5 -43.2(2) . . . . ? C16 N3 Zn1 N2 -74.7(3) . . . . ? C12 N3 Zn1 N2 105.0(3) . . . . ? C16 N3 Zn1 N1 -140.4(2) . . . . ? C12 N3 Zn1 N1 39.3(2) . . . . ? C16 N3 Zn1 N6 88.9(3) . . . . ? C12 N3 Zn1 N6 -91.4(3) . . . . ? C11 N2 Zn1 N4 29.6(3) . . . . ? C7 N2 Zn1 N4 -158.7(2) . . . . ? C11 N2 Zn1 N5 -135.6(3) . . . . ? C7 N2 Zn1 N5 36.1(3) . . . . ? C11 N2 Zn1 N3 105.2(3) . . . . ? C7 N2 Zn1 N3 -83.0(3) . . . . ? C11 N2 Zn1 N1 174.2(3) . . . . ? C7 N2 Zn1 N1 -14.1(2) . . . . ? C11 N2 Zn1 N6 -65.3(3) . . . . ? C7 N2 Zn1 N6 106.5(2) . . . . ? C2 N1 Zn1 N4 -93.6(3) . . . . ? C6 N1 Zn1 N4 86.0(3) . . . . ? C2 N1 Zn1 N5 39.2(3) . . . . ? C6 N1 Zn1 N5 -141.3(3) . . . . ? C2 N1 Zn1 N3 -43.8(3) . . . . ? C6 N1 Zn1 N3 135.8(3) . . . . ? C2 N1 Zn1 N2 -168.6(3) . . . . ? C6 N1 Zn1 N2 11.0(2) . . . . ? C2 N1 Zn1 N6 105.3(3) . . . . ? C6 N1 Zn1 N6 -75.1(3) . . . . ? C31 N6 Zn1 N4 -66.8(3) . . . . ? C27 N6 Zn1 N4 104.8(3) . . . . ? C31 N6 Zn1 N5 171.7(3) . . . . ? C27 N6 Zn1 N5 -16.7(2) . . . . ? C31 N6 Zn1 N3 -138.3(3) . . . . ? C27 N6 Zn1 N3 33.3(4) . . . . ? C31 N6 Zn1 N2 27.5(3) . . . . ? C27 N6 Zn1 N2 -161.0(2) . . . . ? C31 N6 Zn1 N1 102.0(3) . . . . ? C27 N6 Zn1 N1 -86.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.434 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.105 # Attachment '7.cif' data_aja0706 _database_code_depnum_ccdc_archive 'CCDC 755787' #TrackingRef '7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common aja0706 _chemical_melting_point ? _chemical_formula_moiety 'C31 H22 Cd N6 O, 2(C H4 O), 2(Cl O4)' _chemical_formula_sum 'C33 H30 Cd Cl2 N6 O11' _chemical_formula_weight 869.94 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' Cd Cd -0.8075 1.2024 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.7638(3) _cell_length_b 15.4130(3) _cell_length_c 15.9828(4) _cell_angle_alpha 109.1960(10) _cell_angle_beta 94.1520(10) _cell_angle_gamma 95.3900(10) _cell_volume 3398.85(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 59689 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.872 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6599 _exptl_absorpt_correction_T_max 0.8313 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55061 _diffrn_reflns_av_R_equivalents 0.1097 _diffrn_reflns_av_sigmaI/netI 0.0943 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.83 _reflns_number_total 15553 _reflns_number_gt 10533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0320P)^2^+5.7005P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15553 _refine_ls_number_parameters 965 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1276 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 C1 C 0.9920(3) 0.3946(3) 0.7487(3) 0.0366(11) Uani 1 1 d . . . C2 C 1.0980(3) 0.4085(3) 0.7681(3) 0.0317(10) Uani 1 1 d . . . C3 C 1.1500(3) 0.4739(3) 0.7435(3) 0.0360(11) Uani 1 1 d . . . H3 H 1.1224 0.5091 0.7140 0.043 Uiso 1 1 calc R . . C4 C 1.2439(3) 0.4855(3) 0.7636(3) 0.0401(11) Uani 1 1 d . . . H4 H 1.2802 0.5288 0.7475 0.048 Uiso 1 1 calc R . . C5 C 1.2842(3) 0.4331(3) 0.8077(3) 0.0390(11) Uani 1 1 d . . . H5 H 1.3473 0.4413 0.8224 0.047 Uiso 1 1 calc R . . C6 C 1.2286(3) 0.3682(3) 0.8295(3) 0.0286(9) Uani 1 1 d . . . C7 C 1.2657(3) 0.3081(3) 0.8767(3) 0.0313(10) Uani 1 1 d . . . C8 C 1.3597(3) 0.3086(4) 0.8933(3) 0.0459(13) Uani 1 1 d . . . H8 H 1.4006 0.3466 0.8749 0.055 Uiso 1 1 calc R . . C9 C 1.3914(3) 0.2522(4) 0.9371(4) 0.0526(14) Uani 1 1 d . . . H9 H 1.4539 0.2497 0.9465 0.063 Uiso 1 1 calc R . . C10 C 1.3297(3) 0.1995(4) 0.9669(3) 0.0461(13) Uani 1 1 d . . . H10 H 1.3496 0.1630 0.9990 0.055 Uiso 1 1 calc R . . C11 C 1.2380(3) 0.2022(3) 0.9481(3) 0.0414(12) Uani 1 1 d . . . H11 H 1.1963 0.1661 0.9677 0.050 Uiso 1 1 calc R . . C12 C 0.9486(3) 0.4149(3) 0.8369(3) 0.0341(10) Uani 1 1 d . . . C13 C 0.8992(3) 0.4887(4) 0.8665(4) 0.0463(13) Uani 1 1 d . . . H13 H 0.8931 0.5286 0.8343 0.056 Uiso 1 1 calc R . . C14 C 0.8593(3) 0.5025(3) 0.9439(4) 0.0466(13) Uani 1 1 d . . . H14 H 0.8241 0.5507 0.9633 0.056 Uiso 1 1 calc R . . C15 C 0.8714(3) 0.4448(3) 0.9929(3) 0.0399(11) Uani 1 1 d . . . H15 H 0.8451 0.4539 1.0458 0.048 Uiso 1 1 calc R . . C16 C 0.9239(3) 0.3727(3) 0.9617(3) 0.0330(10) Uani 1 1 d . . . C17 C 0.9415(3) 0.3077(3) 1.0099(3) 0.0340(10) Uani 1 1 d . . . C18 C 0.9089(4) 0.3165(3) 1.0911(3) 0.0457(12) Uani 1 1 d . . . H18 H 0.8746 0.3642 1.1164 0.055 Uiso 1 1 calc R . . C19 C 0.9269(4) 0.2548(4) 1.1347(3) 0.0517(14) Uani 1 1 d . . . H19 H 0.9053 0.2610 1.1893 0.062 Uiso 1 1 calc R . . C20 C 0.9770(3) 0.1845(3) 1.0959(3) 0.0440(12) Uani 1 1 d . . . H20 H 0.9899 0.1416 1.1232 0.053 Uiso 1 1 calc R . . C21 C 1.0078(3) 0.1794(3) 1.0148(3) 0.0390(11) Uani 1 1 d . . . H21 H 1.0412 0.1314 0.9878 0.047 Uiso 1 1 calc R . . C22 C 0.9541(3) 0.2967(3) 0.6848(3) 0.0339(10) Uani 1 1 d . . . C23 C 0.8937(3) 0.2847(4) 0.6106(3) 0.0437(12) Uani 1 1 d . . . H23 H 0.8746 0.3357 0.5987 0.052 Uiso 1 1 calc R . . C24 C 0.8622(3) 0.1960(4) 0.5543(3) 0.0474(13) Uani 1 1 d . . . H24 H 0.8214 0.1866 0.5041 0.057 Uiso 1 1 calc R . . C25 C 0.8917(3) 0.1216(4) 0.5731(3) 0.0433(12) Uani 1 1 d . . . H25 H 0.8714 0.0615 0.5355 0.052 Uiso 1 1 calc R . . C26 C 0.9523(3) 0.1377(3) 0.6494(3) 0.0355(11) Uani 1 1 d . . . C27 C 0.9866(3) 0.0607(3) 0.6744(3) 0.0343(10) Uani 1 1 d . . . C28 C 0.9772(3) -0.0286(3) 0.6138(3) 0.0438(12) Uani 1 1 d . . . H28 H 0.9472 -0.0422 0.5569 0.053 Uiso 1 1 calc R . . C29 C 1.0130(4) -0.0971(4) 0.6387(4) 0.0498(14) Uani 1 1 d . . . H29 H 1.0084 -0.1570 0.5982 0.060 Uiso 1 1 calc R . . C30 C 1.0551(3) -0.0766(3) 0.7226(3) 0.0422(12) Uani 1 1 d . . . H30 H 1.0791 -0.1221 0.7407 0.051 Uiso 1 1 calc R . . C31 C 1.0611(3) 0.0135(3) 0.7803(3) 0.0378(11) Uani 1 1 d . . . H31 H 1.0891 0.0275 0.8380 0.045 Uiso 1 1 calc R . . C32 C 0.4369(3) 0.8734(3) 0.5897(4) 0.0425(12) Uani 1 1 d . . . C33 C 0.5415(3) 0.8890(3) 0.6126(3) 0.0389(11) Uani 1 1 d . . . C34 C 0.5942(4) 0.9623(4) 0.6009(4) 0.0507(13) Uani 1 1 d . . . H34 H 0.5674 1.0023 0.5769 0.061 Uiso 1 1 calc R . . C35 C 0.6879(4) 0.9750(4) 0.6258(4) 0.0548(14) Uani 1 1 d . . . H35 H 0.7243 1.0247 0.6196 0.066 Uiso 1 1 calc R . . C36 C 0.7265(4) 0.9145(3) 0.6592(4) 0.0490(13) Uani 1 1 d . . . H36 H 0.7891 0.9229 0.6766 0.059 Uiso 1 1 calc R . . C37 C 0.6710(3) 0.8402(3) 0.6669(3) 0.0413(12) Uani 1 1 d . . . C38 C 0.7068(3) 0.7702(3) 0.7001(3) 0.0446(12) Uani 1 1 d . . . C39 C 0.7991(4) 0.7571(4) 0.7005(4) 0.0624(16) Uani 1 1 d . . . H39 H 0.8396 0.7920 0.6785 0.075 Uiso 1 1 calc R . . C40 C 0.8292(5) 0.6925(5) 0.7334(5) 0.083(2) Uani 1 1 d . . . H40 H 0.8902 0.6821 0.7330 0.099 Uiso 1 1 calc R . . C41 C 0.7681(5) 0.6426(5) 0.7675(5) 0.089(2) Uani 1 1 d . . . H41 H 0.7880 0.6003 0.7927 0.107 Uiso 1 1 calc R . . C42 C 0.6762(4) 0.6569(4) 0.7634(4) 0.0673(17) Uani 1 1 d . . . H42 H 0.6348 0.6228 0.7854 0.081 Uiso 1 1 calc R . . C43 C 0.3874(3) 0.8916(3) 0.6739(4) 0.0432(12) Uani 1 1 d . . . C44 C 0.3303(4) 0.9625(3) 0.6965(4) 0.0578(16) Uani 1 1 d . . . H44 H 0.3198 0.9974 0.6600 0.069 Uiso 1 1 calc R . . C45 C 0.2909(4) 0.9778(5) 0.7742(6) 0.082(2) Uani 1 1 d . . . H45 H 0.2549 1.0257 0.7922 0.099 Uiso 1 1 calc R . . C46 C 0.3037(4) 0.9239(5) 0.8252(5) 0.074(2) Uani 1 1 d . . . H46 H 0.2764 0.9344 0.8777 0.089 Uiso 1 1 calc R . . C47 C 0.3581(3) 0.8529(4) 0.7982(4) 0.0503(14) Uani 1 1 d . . . C48 C 0.3712(4) 0.7874(4) 0.8473(3) 0.0572(16) Uani 1 1 d . . . C49 C 0.3237(4) 0.7900(5) 0.9216(4) 0.081(2) Uani 1 1 d . . . H49 H 0.2838 0.8335 0.9428 0.097 Uiso 1 1 calc R . . C50 C 0.3397(6) 0.7233(6) 0.9621(5) 0.089(2) Uani 1 1 d U . . H50 H 0.3086 0.7223 1.0104 0.107 Uiso 1 1 calc R . . C51 C 0.3968(5) 0.6631(6) 0.9340(5) 0.086(2) Uani 1 1 d U . . H51 H 0.4076 0.6202 0.9618 0.103 Uiso 1 1 calc R . . C52 C 0.4407(5) 0.6657(4) 0.8611(4) 0.0714(19) Uani 1 1 d . . . H52 H 0.4808 0.6223 0.8402 0.086 Uiso 1 1 calc R . . C53 C 0.3690(3) 0.7625(4) 0.4367(3) 0.0453(12) Uani 1 1 d . . . H53 H 0.3647 0.8128 0.4173 0.054 Uiso 1 1 calc R . . C54 C 0.3399(4) 0.6749(4) 0.3809(3) 0.0481(13) Uani 1 1 d . . . H54 H 0.3169 0.6650 0.3224 0.058 Uiso 1 1 calc R . . C55 C 0.3441(3) 0.6004(4) 0.4104(3) 0.0448(12) Uani 1 1 d . . . H55 H 0.3222 0.5405 0.3733 0.054 Uiso 1 1 calc R . . C56 C 0.3827(3) 0.6182(3) 0.4987(3) 0.0332(10) Uani 1 1 d . . . C57 C 0.3908(3) 0.5431(3) 0.5364(3) 0.0356(11) Uani 1 1 d . . . C58 C 0.3432(4) 0.4552(3) 0.4968(3) 0.0445(12) Uani 1 1 d . . . H58 H 0.3037 0.4419 0.4450 0.053 Uiso 1 1 calc R . . C59 C 0.3542(4) 0.3880(4) 0.5339(4) 0.0505(13) Uani 1 1 d . . . H59 H 0.3214 0.3295 0.5078 0.061 Uiso 1 1 calc R . . C60 C 0.4133(4) 0.4068(3) 0.6092(4) 0.0489(13) Uani 1 1 d . . . H60 H 0.4229 0.3615 0.6343 0.059 Uiso 1 1 calc R . . C61 C 0.4586(3) 0.4961(3) 0.6469(4) 0.0457(12) Uani 1 1 d . . . H61 H 0.4984 0.5100 0.6986 0.055 Uiso 1 1 calc R . . C62 C 0.7623(4) 0.2014(4) 0.7938(4) 0.0605(15) Uani 1 1 d . . . H62D H 0.7676 0.2566 0.8451 0.091 Uiso 1 1 calc R . . H62E H 0.7056 0.1639 0.7907 0.091 Uiso 1 1 calc R . . H62F H 0.7634 0.2179 0.7409 0.091 Uiso 1 1 calc R . . C63 C 0.0894(5) 0.3868(5) 0.5101(5) 0.0777(19) Uani 1 1 d . . . H62A H 0.1048 0.4056 0.4607 0.116 Uiso 1 1 calc R . . H62B H 0.0685 0.3217 0.4891 0.116 Uiso 1 1 calc R . . H62C H 0.1424 0.3996 0.5527 0.116 Uiso 1 1 calc R . . C64 C 0.4829(5) 0.1701(5) 0.7145(5) 0.091(2) Uani 1 1 d . . . H63A H 0.5046 0.2329 0.7207 0.136 Uiso 1 1 calc R . . H63B H 0.5321 0.1417 0.7331 0.136 Uiso 1 1 calc R . . H63C H 0.4340 0.1696 0.7508 0.136 Uiso 1 1 calc R . . C65 C 0.5524(7) 0.0200(7) 0.8779(9) 0.177(6) Uani 1 1 d . . . H64A H 0.5381 0.0585 0.9349 0.265 Uiso 1 1 calc R . . H64B H 0.5034 0.0152 0.8331 0.265 Uiso 1 1 calc R . . H64C H 0.6080 0.0469 0.8638 0.265 Uiso 1 1 calc R . . C73 C 0.4051(3) 0.7755(3) 0.5228(3) 0.0362(11) Uani 1 1 d . . . N1 N 1.1367(2) 0.3567(2) 0.8101(2) 0.0297(8) Uani 1 1 d . . . N2 N 1.2051(2) 0.2542(2) 0.9027(2) 0.0322(8) Uani 1 1 d . . . N3 N 0.9613(2) 0.3587(2) 0.8843(2) 0.0308(8) Uani 1 1 d . . . N4 N 0.9921(2) 0.2400(2) 0.9732(2) 0.0332(8) Uani 1 1 d . . . N5 N 0.9814(2) 0.2241(3) 0.7043(2) 0.0316(8) Uani 1 1 d . . . N6 N 1.0286(2) 0.0818(2) 0.7570(2) 0.0321(8) Uani 1 1 d . . . N7 N 0.5794(3) 0.8287(3) 0.6442(3) 0.0367(9) Uani 1 1 d . . . N8 N 0.6462(3) 0.7178(3) 0.7292(3) 0.0468(11) Uani 1 1 d . . . N9 N 0.4004(3) 0.8399(3) 0.7241(3) 0.0379(9) Uani 1 1 d . . . N10 N 0.4298(3) 0.7258(3) 0.8186(3) 0.0505(11) Uani 1 1 d . . . N11 N 0.4125(2) 0.7036(2) 0.5521(2) 0.0319(8) Uani 1 1 d . . . N12 N 0.4476(3) 0.5629(3) 0.6125(2) 0.0360(9) Uani 1 1 d . . . O1 O 0.9646(2) 0.4619(2) 0.7128(2) 0.0443(8) Uani 1 1 d . . . H1 H 0.9786 0.4495 0.6618 0.066 Uiso 1 1 calc R . . O2 O 0.4117(3) 0.9335(2) 0.5437(3) 0.0611(11) Uani 1 1 d . . . H2 H 0.4267 0.9875 0.5760 0.092 Uiso 1 1 calc R . . O3 O 0.5187(3) 0.4598(5) 0.8356(5) 0.152(3) Uani 1 1 d . . . O4 O 0.6084(5) 0.3566(3) 0.8596(4) 0.124(2) Uani 1 1 d . . . O5 O 0.6276(4) 0.4986(4) 0.9589(3) 0.1093(19) Uani 1 1 d . . . O6 O 0.6691(3) 0.4787(4) 0.8182(3) 0.0901(15) Uani 1 1 d . . . O7 O 0.7789(3) 0.0653(3) 0.9279(3) 0.0630(11) Uani 1 1 d . . . O8 O 0.7502(3) -0.0962(3) 0.8913(3) 0.0670(11) Uani 1 1 d . . . O9 O 0.8923(3) -0.0265(3) 0.8753(3) 0.0729(12) Uani 1 1 d . . . O10 O 0.8482(3) -0.0078(2) 1.0179(2) 0.0573(10) Uani 1 1 d . . . O11 O 0.2042(4) 0.1677(4) 0.6941(3) 0.0985(16) Uani 1 1 d . . . O12 O 0.1453(4) 0.1973(4) 0.5673(4) 0.115(2) Uani 1 1 d . . . O13 O 0.2221(3) 0.0696(3) 0.5567(3) 0.0765(13) Uani 1 1 d . . . O14 O 0.3027(3) 0.2149(3) 0.6056(4) 0.1056(19) Uani 1 1 d . . . O15 O 0.0841(3) 0.6659(4) 0.6505(3) 0.109(2) Uani 1 1 d . . . O16 O 0.1746(3) 0.6097(3) 0.5384(2) 0.0627(11) Uani 1 1 d . . . O17 O 0.2390(3) 0.6527(3) 0.6862(3) 0.0780(14) Uani 1 1 d . . . O18 O 0.1994(3) 0.7642(3) 0.6269(3) 0.0808(14) Uani 1 1 d . . . O19 O 0.8365(3) 0.1508(3) 0.8005(3) 0.0679(12) Uani 1 1 d . . . H19A H 0.8255 0.1205 0.8331 0.102 Uiso 1 1 calc R . . O20 O 0.0196(3) 0.4360(3) 0.5506(3) 0.0671(11) Uani 1 1 d . . . H20A H -0.0244 0.4279 0.5134 0.101 Uiso 1 1 calc R . . O21 O 0.4510(3) 0.1208(3) 0.6252(3) 0.0668(11) Uani 1 1 d . . . H21A H 0.4143 0.1491 0.6071 0.100 Uiso 1 1 calc R . . O22 O 0.5631(5) -0.0663(7) 0.8806(8) 0.198(4) Uani 1 1 d . . . H22 H 0.6178 -0.0716 0.8856 0.297 Uiso 1 1 calc R . . Cd1 Cd 1.05229(2) 0.23680(2) 0.84227(2) 0.02823(9) Uani 1 1 d . . . Cd2 Cd 0.49126(2) 0.72126(2) 0.69015(2) 0.03265(10) Uani 1 1 d . . . Cl1 Cl 0.60451(8) 0.44968(8) 0.86858(8) 0.0423(3) Uani 1 1 d . . . Cl2 Cl 0.81826(8) -0.01620(8) 0.92813(8) 0.0410(3) Uani 1 1 d . . . Cl3 Cl 0.21740(9) 0.16403(8) 0.60525(9) 0.0480(3) Uani 1 1 d . . . Cl4 Cl 0.17459(8) 0.67273(8) 0.62632(7) 0.0388(3) 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 C1 0.030(3) 0.041(3) 0.043(3) 0.022(2) -0.005(2) 0.004(2) C2 0.026(2) 0.034(2) 0.032(2) 0.0087(19) -0.0003(19) 0.000(2) C3 0.033(3) 0.038(3) 0.038(3) 0.015(2) -0.001(2) 0.003(2) C4 0.035(3) 0.039(3) 0.050(3) 0.020(2) 0.008(2) -0.003(2) C5 0.026(3) 0.040(3) 0.048(3) 0.013(2) 0.003(2) -0.001(2) C6 0.021(2) 0.030(2) 0.030(2) 0.0050(18) 0.0022(18) -0.0005(18) C7 0.026(2) 0.034(2) 0.031(2) 0.0075(19) 0.0005(19) 0.003(2) C8 0.022(3) 0.062(3) 0.058(3) 0.028(3) 0.000(2) 0.000(2) C9 0.026(3) 0.073(4) 0.063(4) 0.031(3) -0.007(2) 0.006(3) C10 0.035(3) 0.052(3) 0.053(3) 0.023(3) -0.005(2) 0.006(2) C11 0.031(3) 0.053(3) 0.045(3) 0.024(2) 0.003(2) 0.003(2) C12 0.019(2) 0.036(2) 0.048(3) 0.016(2) -0.002(2) 0.0036(19) C13 0.031(3) 0.052(3) 0.061(3) 0.024(3) 0.001(2) 0.014(2) C14 0.033(3) 0.044(3) 0.060(3) 0.010(3) 0.003(3) 0.015(2) C15 0.025(3) 0.047(3) 0.046(3) 0.012(2) 0.006(2) 0.010(2) C16 0.020(2) 0.033(2) 0.041(3) 0.008(2) -0.0002(19) -0.0018(19) C17 0.027(2) 0.033(2) 0.034(2) 0.003(2) 0.002(2) -0.003(2) C18 0.048(3) 0.045(3) 0.040(3) 0.008(2) 0.014(2) 0.007(3) C19 0.068(4) 0.053(3) 0.036(3) 0.015(2) 0.018(3) 0.010(3) C20 0.043(3) 0.046(3) 0.043(3) 0.017(2) 0.001(2) 0.002(2) C21 0.033(3) 0.044(3) 0.039(3) 0.013(2) 0.007(2) 0.008(2) C22 0.023(2) 0.049(3) 0.032(2) 0.018(2) 0.0011(19) -0.001(2) C23 0.029(3) 0.065(3) 0.042(3) 0.028(3) -0.002(2) -0.001(2) C24 0.032(3) 0.080(4) 0.033(3) 0.027(3) -0.003(2) -0.003(3) C25 0.033(3) 0.056(3) 0.034(3) 0.009(2) 0.001(2) -0.011(2) C26 0.019(2) 0.052(3) 0.031(2) 0.011(2) 0.0043(19) -0.002(2) C27 0.027(2) 0.041(3) 0.029(2) 0.005(2) 0.0060(19) -0.005(2) C28 0.040(3) 0.041(3) 0.040(3) 0.003(2) 0.004(2) -0.006(2) C29 0.046(3) 0.040(3) 0.052(3) 0.000(2) 0.018(3) -0.004(3) C30 0.039(3) 0.034(3) 0.053(3) 0.010(2) 0.017(2) 0.006(2) C31 0.030(3) 0.041(3) 0.040(3) 0.009(2) 0.008(2) 0.005(2) C32 0.038(3) 0.036(3) 0.062(3) 0.027(2) 0.001(2) 0.007(2) C33 0.036(3) 0.040(3) 0.043(3) 0.017(2) 0.007(2) 0.003(2) C34 0.047(3) 0.049(3) 0.059(3) 0.026(3) 0.007(3) -0.007(3) C35 0.046(3) 0.054(3) 0.066(4) 0.024(3) 0.015(3) -0.006(3) C36 0.030(3) 0.048(3) 0.061(3) 0.008(3) 0.015(3) -0.005(2) C37 0.035(3) 0.042(3) 0.039(3) 0.003(2) 0.009(2) 0.004(2) C38 0.034(3) 0.042(3) 0.042(3) -0.003(2) -0.005(2) 0.000(2) C39 0.034(3) 0.059(4) 0.079(4) 0.006(3) -0.009(3) 0.008(3) C40 0.043(4) 0.068(4) 0.112(6) 0.005(4) -0.036(4) 0.012(3) C41 0.066(5) 0.074(5) 0.123(7) 0.037(5) -0.043(4) 0.015(4) C42 0.054(4) 0.067(4) 0.083(5) 0.035(4) -0.021(3) 0.008(3) C43 0.027(3) 0.032(3) 0.065(3) 0.011(2) 0.001(2) -0.001(2) C44 0.034(3) 0.035(3) 0.092(5) 0.008(3) -0.008(3) -0.001(2) C45 0.032(4) 0.057(4) 0.122(7) -0.017(4) 0.013(4) 0.001(3) C46 0.034(3) 0.071(4) 0.077(5) -0.026(4) 0.015(3) -0.012(3) C47 0.026(3) 0.053(3) 0.050(3) -0.010(3) 0.013(2) -0.011(2) C48 0.050(4) 0.067(4) 0.035(3) -0.001(3) 0.008(3) -0.029(3) C49 0.052(4) 0.103(5) 0.051(4) -0.016(4) 0.013(3) -0.033(4) C50 0.089(4) 0.110(4) 0.061(3) 0.031(3) 0.010(3) -0.036(3) C51 0.094(4) 0.096(4) 0.063(3) 0.035(3) -0.005(3) -0.028(3) C52 0.096(5) 0.079(4) 0.031(3) 0.024(3) -0.010(3) -0.038(4) C53 0.043(3) 0.048(3) 0.049(3) 0.022(3) -0.001(2) 0.009(2) C54 0.050(3) 0.059(3) 0.040(3) 0.021(3) 0.002(2) 0.016(3) C55 0.041(3) 0.045(3) 0.040(3) 0.003(2) 0.004(2) 0.004(2) C56 0.026(2) 0.040(3) 0.036(2) 0.015(2) 0.008(2) 0.006(2) C57 0.028(2) 0.035(2) 0.036(3) 0.001(2) 0.010(2) 0.001(2) C58 0.044(3) 0.039(3) 0.045(3) 0.009(2) 0.005(2) -0.004(2) C59 0.048(3) 0.037(3) 0.056(3) 0.002(2) 0.010(3) -0.001(2) C60 0.047(3) 0.040(3) 0.068(4) 0.028(3) 0.017(3) 0.007(3) C61 0.039(3) 0.041(3) 0.057(3) 0.019(3) 0.002(2) 0.002(2) C62 0.047(4) 0.064(4) 0.062(4) 0.011(3) 0.005(3) 0.007(3) C63 0.084(5) 0.071(4) 0.076(5) 0.025(4) -0.002(4) 0.009(4) C64 0.084(5) 0.070(5) 0.093(6) 0.000(4) -0.005(4) 0.002(4) C65 0.078(7) 0.089(7) 0.300(17) 0.001(9) -0.065(8) 0.003(6) C73 0.029(3) 0.045(3) 0.042(3) 0.026(2) 0.005(2) 0.004(2) N1 0.025(2) 0.0306(19) 0.033(2) 0.0102(16) 0.0020(16) 0.0000(16) N2 0.025(2) 0.040(2) 0.031(2) 0.0127(17) -0.0006(16) -0.0007(17) N3 0.0239(19) 0.031(2) 0.036(2) 0.0116(16) 0.0001(16) 0.0022(16) N4 0.027(2) 0.036(2) 0.034(2) 0.0095(17) 0.0033(16) 0.0023(17) N5 0.0213(19) 0.041(2) 0.032(2) 0.0126(17) 0.0039(15) 0.0012(17) N6 0.024(2) 0.034(2) 0.036(2) 0.0080(17) 0.0052(16) 0.0045(16) N7 0.025(2) 0.043(2) 0.043(2) 0.0162(18) 0.0059(17) 0.0001(18) N8 0.043(3) 0.045(2) 0.046(2) 0.010(2) -0.013(2) 0.010(2) N9 0.026(2) 0.034(2) 0.047(2) 0.0062(18) 0.0033(18) -0.0001(17) N10 0.055(3) 0.059(3) 0.031(2) 0.014(2) 0.002(2) -0.017(2) N11 0.024(2) 0.037(2) 0.034(2) 0.0114(17) 0.0044(16) 0.0011(17) N12 0.032(2) 0.036(2) 0.038(2) 0.0120(17) 0.0026(17) 0.0017(18) O1 0.0338(19) 0.055(2) 0.054(2) 0.0315(18) 0.0019(17) 0.0097(17) O2 0.068(3) 0.043(2) 0.077(3) 0.034(2) -0.015(2) -0.001(2) O3 0.031(3) 0.272(8) 0.249(8) 0.219(7) 0.006(4) 0.017(4) O4 0.214(7) 0.054(3) 0.102(4) 0.027(3) -0.012(4) 0.023(4) O5 0.150(5) 0.093(4) 0.061(3) -0.003(3) 0.033(3) -0.009(4) O6 0.060(3) 0.144(4) 0.068(3) 0.048(3) 0.013(2) -0.021(3) O7 0.060(3) 0.057(2) 0.084(3) 0.033(2) 0.012(2) 0.027(2) O8 0.079(3) 0.055(2) 0.054(2) 0.0122(19) -0.009(2) -0.019(2) O9 0.065(3) 0.085(3) 0.087(3) 0.042(3) 0.038(2) 0.031(2) O10 0.069(3) 0.057(2) 0.045(2) 0.0197(18) -0.0019(19) -0.001(2) O11 0.108(4) 0.117(4) 0.053(3) 0.003(3) 0.014(3) 0.022(3) O12 0.084(4) 0.121(4) 0.154(5) 0.062(4) -0.014(4) 0.043(3) O13 0.100(4) 0.045(2) 0.067(3) -0.002(2) 0.001(2) 0.002(2) O14 0.055(3) 0.073(3) 0.202(6) 0.076(4) -0.005(3) -0.017(2) O15 0.057(3) 0.180(5) 0.056(3) 0.003(3) 0.018(2) -0.033(3) O16 0.057(3) 0.069(3) 0.046(2) -0.0020(19) 0.0039(19) 0.012(2) O17 0.103(4) 0.061(3) 0.071(3) 0.041(2) -0.043(3) -0.016(2) O18 0.084(3) 0.043(2) 0.113(4) 0.037(2) -0.038(3) -0.010(2) O19 0.057(3) 0.085(3) 0.081(3) 0.050(3) 0.017(2) 0.012(2) O20 0.053(3) 0.095(3) 0.064(3) 0.044(2) -0.001(2) 0.002(2) O21 0.056(3) 0.043(2) 0.091(3) 0.010(2) 0.002(2) 0.0061(19) O22 0.088(5) 0.232(10) 0.292(11) 0.146(9) -0.058(7) -0.043(6) Cd1 0.02193(17) 0.03124(18) 0.03012(17) 0.00903(13) 0.00101(13) 0.00273(13) Cd2 0.0318(2) 0.03475(19) 0.03200(18) 0.01307(15) 0.00123(14) 0.00224(15) Cl1 0.0360(7) 0.0452(7) 0.0491(7) 0.0221(6) 0.0006(6) 0.0022(5) Cl2 0.0402(7) 0.0405(6) 0.0436(7) 0.0153(5) 0.0052(5) 0.0071(5) Cl3 0.0373(7) 0.0369(7) 0.0588(8) 0.0034(6) -0.0004(6) 0.0014(6) Cl4 0.0375(7) 0.0397(6) 0.0343(6) 0.0101(5) -0.0021(5) -0.0060(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.415(5) . ? C1 C12 1.541(6) . ? C1 C22 1.543(6) . ? C1 C2 1.555(6) . ? C2 N1 1.339(5) . ? C2 C3 1.386(6) . ? C3 C4 1.382(6) . ? C3 H3 0.9300 . ? C4 C5 1.380(6) . ? C4 H4 0.9300 . ? C5 C6 1.383(6) . ? C5 H5 0.9300 . ? C6 N1 1.352(5) . ? C6 C7 1.490(6) . ? C7 N2 1.343(5) . ? C7 C8 1.393(6) . ? C8 C9 1.377(7) . ? C8 H8 0.9300 . ? C9 C10 1.377(7) . ? C9 H9 0.9300 . ? C10 C11 1.373(6) . ? C10 H10 0.9300 . ? C11 N2 1.345(6) . ? C11 H11 0.9300 . ? C12 N3 1.341(5) . ? C12 C13 1.379(6) . ? C13 C14 1.370(7) . ? C13 H13 0.9300 . ? C14 C15 1.381(7) . ? C14 H14 0.9300 . ? C15 C16 1.392(6) . ? C15 H15 0.9300 . ? C16 N3 1.351(6) . ? C16 C17 1.482(6) . ? C17 N4 1.341(5) . ? C17 C18 1.386(6) . ? C18 C19 1.384(7) . ? C18 H18 0.9300 . ? C19 C20 1.372(7) . ? C19 H19 0.9300 . ? C20 C21 1.386(6) . ? C20 H20 0.9300 . ? C21 N4 1.339(6) . ? C21 H21 0.9300 . ? C22 N5 1.345(5) . ? C22 C23 1.380(6) . ? C23 C24 1.380(7) . ? C23 H23 0.9300 . ? C24 C25 1.377(7) . ? C24 H24 0.9300 . ? C25 C26 1.397(6) . ? C25 H25 0.9300 . ? C26 N5 1.341(6) . ? C26 C27 1.490(6) . ? C27 N6 1.339(5) . ? C27 C28 1.385(6) . ? C28 C29 1.379(7) . ? C28 H28 0.9300 . ? C29 C30 1.360(7) . ? C29 H29 0.9300 . ? C30 C31 1.382(6) . ? C30 H30 0.9300 . ? C31 N6 1.343(6) . ? C31 H31 0.9300 . ? C32 O2 1.418(5) . ? C32 C43 1.535(7) . ? C32 C33 1.538(7) . ? C32 C73 1.541(7) . ? C33 N7 1.340(6) . ? C33 C34 1.382(6) . ? C34 C35 1.388(7) . ? C34 H34 0.9300 . ? C35 C36 1.365(7) . ? C35 H35 0.9300 . ? C36 C37 1.389(7) . ? C36 H36 0.9300 . ? C37 N7 1.354(6) . ? C37 C38 1.473(7) . ? C38 N8 1.357(7) . ? C38 C39 1.397(7) . ? C39 C40 1.363(9) . ? C39 H39 0.9300 . ? C40 C41 1.386(10) . ? C40 H40 0.9300 . ? C41 C42 1.395(9) . ? C41 H41 0.9300 . ? C42 N8 1.325(6) . ? C42 H42 0.9300 . ? C43 N9 1.321(6) . ? C43 C44 1.412(7) . ? C44 C45 1.368(9) . ? C44 H44 0.9300 . ? C45 C46 1.359(10) . ? C45 H45 0.9300 . ? C46 C47 1.390(8) . ? C46 H46 0.9300 . ? C47 N9 1.344(6) . ? C47 C48 1.486(8) . ? C48 N10 1.335(7) . ? C48 C49 1.414(8) . ? C49 C50 1.411(10) . ? C49 H49 0.9300 . ? C50 C51 1.304(10) . ? C50 H50 0.9300 . ? C51 C52 1.384(9) . ? C51 H51 0.9300 . ? C52 N10 1.331(7) . ? C52 H52 0.9300 . ? C53 C54 1.359(7) . ? C53 C73 1.382(6) . ? C53 H53 0.9300 . ? C54 C55 1.382(7) . ? C54 H54 0.9300 . ? C55 C56 1.410(6) . ? C55 H55 0.9300 . ? C56 N11 1.325(6) . ? C56 C57 1.481(6) . ? C57 N12 1.355(6) . ? C57 C58 1.386(6) . ? C58 C59 1.368(7) . ? C58 H58 0.9300 . ? C59 C60 1.366(7) . ? C59 H59 0.9300 . ? C60 C61 1.388(7) . ? C60 H60 0.9300 . ? C61 N12 1.334(6) . ? C61 H61 0.9300 . ? C62 O19 1.421(6) . ? C62 H62D 0.9600 . ? C62 H62E 0.9600 . ? C62 H62F 0.9600 . ? C63 O20 1.406(7) . ? C63 H62A 0.9600 . ? C63 H62B 0.9600 . ? C63 H62C 0.9600 . ? C64 O21 1.399(7) . ? C64 H63A 0.9600 . ? C64 H63B 0.9600 . ? C64 H63C 0.9600 . ? C65 O22 1.369(11) . ? C65 H64A 0.9600 . ? C65 H64B 0.9600 . ? C65 H64C 0.9600 . ? C73 N11 1.348(5) . ? N1 Cd1 2.349(3) . ? N2 Cd1 2.344(4) . ? N3 Cd1 2.358(3) . ? N4 Cd1 2.320(4) . ? N5 Cd1 2.311(3) . ? N6 Cd1 2.307(4) . ? N7 Cd2 2.347(4) . ? N8 Cd2 2.337(4) . ? N9 Cd2 2.314(4) . ? N10 Cd2 2.287(4) . ? N11 Cd2 2.338(4) . ? N12 Cd2 2.347(4) . ? O1 H1 0.8200 . ? O2 H2 0.8200 . ? O3 Cl1 1.378(4) . ? O4 Cl1 1.401(5) . ? O5 Cl1 1.391(5) . ? O6 Cl1 1.424(4) . ? O7 Cl2 1.433(3) . ? O8 Cl2 1.442(4) . ? O9 Cl2 1.419(4) . ? O10 Cl2 1.431(4) . ? O11 Cl3 1.431(5) . ? O12 Cl3 1.406(5) . ? O13 Cl3 1.418(4) . ? O14 Cl3 1.418(4) . ? O15 Cl4 1.421(4) . ? O16 Cl4 1.422(4) . ? O17 Cl4 1.425(4) . ? O18 Cl4 1.420(4) . ? O19 H19A 0.8200 . ? O20 H20A 0.8200 . ? O21 H21A 0.8200 . ? O22 H22 0.8200 . ? 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 O1 C1 C12 104.9(4) . . ? O1 C1 C22 109.9(4) . . ? C12 C1 C22 110.0(4) . . ? O1 C1 C2 109.3(4) . . ? C12 C1 C2 109.7(4) . . ? C22 C1 C2 112.7(4) . . ? N1 C2 C3 121.7(4) . . ? N1 C2 C1 118.2(4) . . ? C3 C2 C1 120.2(4) . . ? C4 C3 C2 118.4(4) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C5 C4 C3 120.2(4) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 118.5(4) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? N1 C6 C5 121.4(4) . . ? N1 C6 C7 116.1(4) . . ? C5 C6 C7 122.5(4) . . ? N2 C7 C8 121.7(4) . . ? N2 C7 C6 117.4(4) . . ? C8 C7 C6 120.9(4) . . ? C9 C8 C7 119.2(5) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C8 119.3(5) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 118.3(5) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? N2 C11 C10 123.5(5) . . ? N2 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? N3 C12 C13 121.2(4) . . ? N3 C12 C1 117.7(4) . . ? C13 C12 C1 121.1(4) . . ? C14 C13 C12 119.3(5) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 120.0(4) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 118.6(5) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? N3 C16 C15 120.7(4) . . ? N3 C16 C17 116.6(4) . . ? C15 C16 C17 122.7(4) . . ? N4 C17 C18 120.4(4) . . ? N4 C17 C16 117.7(4) . . ? C18 C17 C16 121.9(4) . . ? C19 C18 C17 120.5(5) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 118.9(5) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 117.9(5) . . ? C19 C20 H20 121.1 . . ? C21 C20 H20 121.1 . . ? N4 C21 C20 123.4(4) . . ? N4 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? N5 C22 C23 121.6(4) . . ? N5 C22 C1 117.7(4) . . ? C23 C22 C1 120.7(4) . . ? C22 C23 C24 119.0(5) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 119.5(4) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 119.1(5) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? N5 C26 C25 120.9(4) . . ? N5 C26 C27 116.9(4) . . ? C25 C26 C27 122.2(4) . . ? N6 C27 C28 121.6(4) . . ? N6 C27 C26 117.3(4) . . ? C28 C27 C26 121.1(4) . . ? C29 C28 C27 119.2(5) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C30 C29 C28 119.8(5) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 118.2(5) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? N6 C31 C30 123.2(5) . . ? N6 C31 H31 118.4 . . ? C30 C31 H31 118.4 . . ? O2 C32 C43 109.6(4) . . ? O2 C32 C33 109.0(4) . . ? C43 C32 C33 111.5(4) . . ? O2 C32 C73 104.3(4) . . ? C43 C32 C73 111.2(4) . . ? C33 C32 C73 111.1(4) . . ? N7 C33 C34 121.4(5) . . ? N7 C33 C32 117.4(4) . . ? C34 C33 C32 121.2(4) . . ? C33 C34 C35 118.8(5) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? C36 C35 C34 119.9(5) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 119.1(5) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? N7 C37 C36 121.0(5) . . ? N7 C37 C38 116.0(4) . . ? C36 C37 C38 122.9(5) . . ? N8 C38 C39 121.2(5) . . ? N8 C38 C37 117.3(4) . . ? C39 C38 C37 121.5(5) . . ? C40 C39 C38 119.3(6) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 119.4(6) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C40 C41 C42 118.8(6) . . ? C40 C41 H41 120.6 . . ? C42 C41 H41 120.6 . . ? N8 C42 C41 121.9(6) . . ? N8 C42 H42 119.0 . . ? C41 C42 H42 119.0 . . ? N9 C43 C44 121.5(5) . . ? N9 C43 C32 118.3(4) . . ? C44 C43 C32 120.3(5) . . ? C45 C44 C43 117.6(6) . . ? C45 C44 H44 121.2 . . ? C43 C44 H44 121.2 . . ? C46 C45 C44 120.7(6) . . ? C46 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? C45 C46 C47 119.3(6) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 120.3 . . ? N9 C47 C46 120.4(6) . . ? N9 C47 C48 116.9(5) . . ? C46 C47 C48 122.7(6) . . ? N10 C48 C49 121.1(6) . . ? N10 C48 C47 117.4(4) . . ? C49 C48 C47 121.4(6) . . ? C50 C49 C48 116.8(7) . . ? C50 C49 H49 121.6 . . ? C48 C49 H49 121.6 . . ? C51 C50 C49 122.0(7) . . ? C51 C50 H50 119.0 . . ? C49 C50 H50 119.0 . . ? C50 C51 C52 117.4(7) . . ? C50 C51 H51 121.3 . . ? C52 C51 H51 121.3 . . ? N10 C52 C51 124.8(7) . . ? N10 C52 H52 117.6 . . ? C51 C52 H52 117.6 . . ? C54 C53 C73 118.8(5) . . ? C54 C53 H53 120.6 . . ? C73 C53 H53 120.6 . . ? C53 C54 C55 120.6(5) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C54 C55 C56 117.8(5) . . ? C54 C55 H55 121.1 . . ? C56 C55 H55 121.1 . . ? N11 C56 C55 121.2(4) . . ? N11 C56 C57 116.8(4) . . ? C55 C56 C57 122.0(4) . . ? N12 C57 C58 120.1(4) . . ? N12 C57 C56 117.4(4) . . ? C58 C57 C56 122.5(4) . . ? C59 C58 C57 120.1(5) . . ? C59 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? C60 C59 C58 120.1(5) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C59 C60 C61 117.6(5) . . ? C59 C60 H60 121.2 . . ? C61 C60 H60 121.2 . . ? N12 C61 C60 123.1(5) . . ? N12 C61 H61 118.4 . . ? C60 C61 H61 118.4 . . ? O19 C62 H62D 109.5 . . ? O19 C62 H62E 109.5 . . ? H62D C62 H62E 109.5 . . ? O19 C62 H62F 109.5 . . ? H62D C62 H62F 109.5 . . ? H62E C62 H62F 109.5 . . ? O20 C63 H62A 109.5 . . ? O20 C63 H62B 109.5 . . ? H62A C63 H62B 109.5 . . ? O20 C63 H62C 109.5 . . ? H62A C63 H62C 109.5 . . ? H62B C63 H62C 109.5 . . ? O21 C64 H63A 109.5 . . ? O21 C64 H63B 109.5 . . ? H63A C64 H63B 109.5 . . ? O21 C64 H63C 109.5 . . ? H63A C64 H63C 109.5 . . ? H63B C64 H63C 109.5 . . ? O22 C65 H64A 109.5 . . ? O22 C65 H64B 109.5 . . ? H64A C65 H64B 109.5 . . ? O22 C65 H64C 109.5 . . ? H64A C65 H64C 109.5 . . ? H64B C65 H64C 109.5 . . ? N11 C73 C53 121.6(4) . . ? N11 C73 C32 117.3(4) . . ? C53 C73 C32 121.1(4) . . ? C2 N1 C6 119.7(4) . . ? C2 N1 Cd1 122.6(3) . . ? C6 N1 Cd1 117.5(3) . . ? C7 N2 C11 117.8(4) . . ? C7 N2 Cd1 116.8(3) . . ? C11 N2 Cd1 124.3(3) . . ? C12 N3 C16 120.1(4) . . ? C12 N3 Cd1 123.0(3) . . ? C16 N3 Cd1 116.8(3) . . ? C21 N4 C17 118.9(4) . . ? C21 N4 Cd1 123.2(3) . . ? C17 N4 Cd1 117.9(3) . . ? C26 N5 C22 119.9(4) . . ? C26 N5 Cd1 115.8(3) . . ? C22 N5 Cd1 123.1(3) . . ? C27 N6 C31 118.1(4) . . ? C27 N6 Cd1 116.2(3) . . ? C31 N6 Cd1 125.3(3) . . ? C33 N7 C37 119.7(4) . . ? C33 N7 Cd2 122.1(3) . . ? C37 N7 Cd2 116.9(3) . . ? C42 N8 C38 119.3(5) . . ? C42 N8 Cd2 123.3(4) . . ? C38 N8 Cd2 116.4(3) . . ? C43 N9 C47 120.4(4) . . ? C43 N9 Cd2 123.4(3) . . ? C47 N9 Cd2 116.2(3) . . ? C52 N10 C48 117.9(5) . . ? C52 N10 Cd2 124.7(4) . . ? C48 N10 Cd2 117.0(3) . . ? C56 N11 C73 120.0(4) . . ? C56 N11 Cd2 117.4(3) . . ? C73 N11 Cd2 122.3(3) . . ? C61 N12 C57 118.9(4) . . ? C61 N12 Cd2 124.3(3) . . ? C57 N12 Cd2 115.1(3) . . ? C1 O1 H1 109.5 . . ? C32 O2 H2 109.5 . . ? C62 O19 H19A 109.5 . . ? C63 O20 H20A 109.5 . . ? C64 O21 H21A 109.5 . . ? C65 O22 H22 109.5 . . ? N6 Cd1 N5 72.32(13) . . ? N6 Cd1 N4 103.22(13) . . ? N5 Cd1 N4 131.04(12) . . ? N6 Cd1 N2 101.80(12) . . ? N5 Cd1 N2 134.31(12) . . ? N4 Cd1 N2 94.63(12) . . ? N6 Cd1 N1 127.23(12) . . ? N5 Cd1 N1 77.88(12) . . ? N4 Cd1 N1 128.99(12) . . ? N2 Cd1 N1 70.45(12) . . ? N6 Cd1 N3 136.12(12) . . ? N5 Cd1 N3 79.88(12) . . ? N4 Cd1 N3 70.82(12) . . ? N2 Cd1 N3 121.81(12) . . ? N1 Cd1 N3 76.77(12) . . ? N10 Cd2 N9 72.23(16) . . ? N10 Cd2 N8 101.84(16) . . ? N9 Cd2 N8 132.07(14) . . ? N10 Cd2 N11 127.38(14) . . ? N9 Cd2 N11 76.79(13) . . ? N8 Cd2 N11 130.27(14) . . ? N10 Cd2 N7 134.78(14) . . ? N9 Cd2 N7 80.53(13) . . ? N8 Cd2 N7 70.95(14) . . ? N11 Cd2 N7 77.87(13) . . ? N10 Cd2 N12 96.93(14) . . ? N9 Cd2 N12 128.54(13) . . ? N8 Cd2 N12 99.25(14) . . ? N11 Cd2 N12 71.11(13) . . ? N7 Cd2 N12 128.15(13) . . ? O3 Cl1 O5 114.3(4) . . ? O3 Cl1 O4 109.5(4) . . ? O5 Cl1 O4 105.3(3) . . ? O3 Cl1 O6 107.6(3) . . ? O5 Cl1 O6 109.9(3) . . ? O4 Cl1 O6 110.2(4) . . ? O9 Cl2 O10 111.2(3) . . ? O9 Cl2 O7 108.9(2) . . ? O10 Cl2 O7 109.2(2) . . ? O9 Cl2 O8 109.4(3) . . ? O10 Cl2 O8 108.5(2) . . ? O7 Cl2 O8 109.6(3) . . ? O12 Cl3 O14 110.9(3) . . ? O12 Cl3 O13 111.0(3) . . ? O14 Cl3 O13 107.9(3) . . ? O12 Cl3 O11 111.5(3) . . ? O14 Cl3 O11 109.6(4) . . ? O13 Cl3 O11 105.7(3) . . ? O18 Cl4 O15 108.5(3) . . ? O18 Cl4 O16 109.0(3) . . ? O15 Cl4 O16 108.0(3) . . ? O18 Cl4 O17 109.1(2) . . ? O15 Cl4 O17 112.0(3) . . ? O16 Cl4 O17 110.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 173.9(4) . . . . ? C12 C1 C2 N1 59.4(5) . . . . ? C22 C1 C2 N1 -63.5(5) . . . . ? O1 C1 C2 C3 -5.0(6) . . . . ? C12 C1 C2 C3 -119.5(4) . . . . ? C22 C1 C2 C3 117.5(4) . . . . ? N1 C2 C3 C4 -0.4(7) . . . . ? C1 C2 C3 C4 178.6(4) . . . . ? C2 C3 C4 C5 -0.3(7) . . . . ? C3 C4 C5 C6 1.1(7) . . . . ? C4 C5 C6 N1 -1.3(7) . . . . ? C4 C5 C6 C7 179.8(4) . . . . ? N1 C6 C7 N2 -5.6(6) . . . . ? C5 C6 C7 N2 173.4(4) . . . . ? N1 C6 C7 C8 174.6(4) . . . . ? C5 C6 C7 C8 -6.4(7) . . . . ? N2 C7 C8 C9 0.2(7) . . . . ? C6 C7 C8 C9 180.0(5) . . . . ? C7 C8 C9 C10 -2.7(8) . . . . ? C8 C9 C10 C11 2.9(8) . . . . ? C9 C10 C11 N2 -0.6(8) . . . . ? O1 C1 C12 N3 177.9(4) . . . . ? C22 C1 C12 N3 59.8(5) . . . . ? C2 C1 C12 N3 -64.8(5) . . . . ? O1 C1 C12 C13 -2.7(6) . . . . ? C22 C1 C12 C13 -120.8(5) . . . . ? C2 C1 C12 C13 114.6(5) . . . . ? N3 C12 C13 C14 -2.7(7) . . . . ? C1 C12 C13 C14 177.9(4) . . . . ? C12 C13 C14 C15 2.3(8) . . . . ? C13 C14 C15 C16 -0.5(7) . . . . ? C14 C15 C16 N3 -0.9(7) . . . . ? C14 C15 C16 C17 179.5(4) . . . . ? N3 C16 C17 N4 -0.5(6) . . . . ? C15 C16 C17 N4 179.2(4) . . . . ? N3 C16 C17 C18 178.3(4) . . . . ? C15 C16 C17 C18 -2.0(7) . . . . ? N4 C17 C18 C19 -0.9(8) . . . . ? C16 C17 C18 C19 -179.7(5) . . . . ? C17 C18 C19 C20 -0.5(8) . . . . ? C18 C19 C20 C21 0.5(8) . . . . ? C19 C20 C21 N4 0.8(8) . . . . ? O1 C1 C22 N5 173.3(4) . . . . ? C12 C1 C22 N5 -71.6(5) . . . . ? C2 C1 C22 N5 51.2(5) . . . . ? O1 C1 C22 C23 -7.1(6) . . . . ? C12 C1 C22 C23 107.9(5) . . . . ? C2 C1 C22 C23 -129.3(4) . . . . ? N5 C22 C23 C24 -1.3(7) . . . . ? C1 C22 C23 C24 179.2(4) . . . . ? C22 C23 C24 C25 -0.1(7) . . . . ? C23 C24 C25 C26 0.5(7) . . . . ? C24 C25 C26 N5 0.5(7) . . . . ? C24 C25 C26 C27 179.5(4) . . . . ? N5 C26 C27 N6 12.7(6) . . . . ? C25 C26 C27 N6 -166.4(4) . . . . ? N5 C26 C27 C28 -165.8(4) . . . . ? C25 C26 C27 C28 15.1(7) . . . . ? N6 C27 C28 C29 -0.9(7) . . . . ? C26 C27 C28 C29 177.6(4) . . . . ? C27 C28 C29 C30 1.4(7) . . . . ? C28 C29 C30 C31 -0.6(7) . . . . ? C29 C30 C31 N6 -0.9(7) . . . . ? O2 C32 C33 N7 -170.2(4) . . . . ? C43 C32 C33 N7 68.8(5) . . . . ? C73 C32 C33 N7 -55.8(6) . . . . ? O2 C32 C33 C34 9.8(7) . . . . ? C43 C32 C33 C34 -111.2(5) . . . . ? C73 C32 C33 C34 124.2(5) . . . . ? N7 C33 C34 C35 -2.4(8) . . . . ? C32 C33 C34 C35 177.7(5) . . . . ? C33 C34 C35 C36 1.4(8) . . . . ? C34 C35 C36 C37 0.7(8) . . . . ? C35 C36 C37 N7 -2.0(7) . . . . ? C35 C36 C37 C38 178.5(5) . . . . ? N7 C37 C38 N8 -18.4(6) . . . . ? C36 C37 C38 N8 161.2(5) . . . . ? N7 C37 C38 C39 160.6(5) . . . . ? C36 C37 C38 C39 -19.8(7) . . . . ? N8 C38 C39 C40 -2.2(8) . . . . ? C37 C38 C39 C40 178.8(5) . . . . ? C38 C39 C40 C41 -1.3(10) . . . . ? C39 C40 C41 C42 2.9(11) . . . . ? C40 C41 C42 N8 -1.1(11) . . . . ? O2 C32 C43 N9 177.9(4) . . . . ? C33 C32 C43 N9 -61.3(5) . . . . ? C73 C32 C43 N9 63.2(5) . . . . ? O2 C32 C43 C44 -2.5(6) . . . . ? C33 C32 C43 C44 118.3(5) . . . . ? C73 C32 C43 C44 -117.2(5) . . . . ? N9 C43 C44 C45 2.1(8) . . . . ? C32 C43 C44 C45 -177.5(5) . . . . ? C43 C44 C45 C46 -2.7(9) . . . . ? C44 C45 C46 C47 0.5(9) . . . . ? C45 C46 C47 N9 2.5(8) . . . . ? C45 C46 C47 C48 -176.4(5) . . . . ? N9 C47 C48 N10 5.4(7) . . . . ? C46 C47 C48 N10 -175.7(5) . . . . ? N9 C47 C48 C49 -174.6(5) . . . . ? C46 C47 C48 C49 4.4(8) . . . . ? N10 C48 C49 C50 -1.4(8) . . . . ? C47 C48 C49 C50 178.6(5) . . . . ? C48 C49 C50 C51 1.3(10) . . . . ? C49 C50 C51 C52 -1.1(11) . . . . ? C50 C51 C52 N10 1.0(10) . . . . ? C73 C53 C54 C55 1.7(8) . . . . ? C53 C54 C55 C56 -2.4(8) . . . . ? C54 C55 C56 N11 1.1(7) . . . . ? C54 C55 C56 C57 -179.6(4) . . . . ? N11 C56 C57 N12 -16.3(6) . . . . ? C55 C56 C57 N12 164.4(4) . . . . ? N11 C56 C57 C58 163.8(4) . . . . ? C55 C56 C57 C58 -15.5(7) . . . . ? N12 C57 C58 C59 -0.8(7) . . . . ? C56 C57 C58 C59 179.1(4) . . . . ? C57 C58 C59 C60 -1.1(8) . . . . ? C58 C59 C60 C61 1.8(8) . . . . ? C59 C60 C61 N12 -0.8(8) . . . . ? C54 C53 C73 N11 0.5(7) . . . . ? C54 C53 C73 C32 -178.4(5) . . . . ? O2 C32 C73 N11 -173.7(4) . . . . ? C43 C32 C73 N11 -55.8(5) . . . . ? C33 C32 C73 N11 69.0(5) . . . . ? O2 C32 C73 C53 5.2(6) . . . . ? C43 C32 C73 C53 123.2(5) . . . . ? C33 C32 C73 C53 -112.1(5) . . . . ? C3 C2 N1 C6 0.1(6) . . . . ? C1 C2 N1 C6 -178.8(4) . . . . ? C3 C2 N1 Cd1 -174.7(3) . . . . ? C1 C2 N1 Cd1 6.3(5) . . . . ? C5 C6 N1 C2 0.7(6) . . . . ? C7 C6 N1 C2 179.7(4) . . . . ? C5 C6 N1 Cd1 175.9(3) . . . . ? C7 C6 N1 Cd1 -5.2(5) . . . . ? C8 C7 N2 C11 2.1(7) . . . . ? C6 C7 N2 C11 -177.7(4) . . . . ? C8 C7 N2 Cd1 -166.7(4) . . . . ? C6 C7 N2 Cd1 13.5(5) . . . . ? C10 C11 N2 C7 -1.9(7) . . . . ? C10 C11 N2 Cd1 166.0(4) . . . . ? C13 C12 N3 C16 1.3(6) . . . . ? C1 C12 N3 C16 -179.3(4) . . . . ? C13 C12 N3 Cd1 -176.2(3) . . . . ? C1 C12 N3 Cd1 3.2(5) . . . . ? C15 C16 N3 C12 0.5(6) . . . . ? C17 C16 N3 C12 -179.8(4) . . . . ? C15 C16 N3 Cd1 178.2(3) . . . . ? C17 C16 N3 Cd1 -2.1(5) . . . . ? C20 C21 N4 C17 -2.2(7) . . . . ? C20 C21 N4 Cd1 175.7(4) . . . . ? C18 C17 N4 C21 2.2(7) . . . . ? C16 C17 N4 C21 -179.0(4) . . . . ? C18 C17 N4 Cd1 -175.8(3) . . . . ? C16 C17 N4 Cd1 3.0(5) . . . . ? C25 C26 N5 C22 -1.9(6) . . . . ? C27 C26 N5 C22 179.0(4) . . . . ? C25 C26 N5 Cd1 165.9(3) . . . . ? C27 C26 N5 Cd1 -13.2(5) . . . . ? C23 C22 N5 C26 2.3(6) . . . . ? C1 C22 N5 C26 -178.1(4) . . . . ? C23 C22 N5 Cd1 -164.5(3) . . . . ? C1 C22 N5 Cd1 15.0(5) . . . . ? C28 C27 N6 C31 -0.5(6) . . . . ? C26 C27 N6 C31 -179.0(4) . . . . ? C28 C27 N6 Cd1 173.0(3) . . . . ? C26 C27 N6 Cd1 -5.4(5) . . . . ? C30 C31 N6 C27 1.4(7) . . . . ? C30 C31 N6 Cd1 -171.5(3) . . . . ? C34 C33 N7 C37 1.2(7) . . . . ? C32 C33 N7 C37 -178.9(4) . . . . ? C34 C33 N7 Cd2 168.2(4) . . . . ? C32 C33 N7 Cd2 -11.8(6) . . . . ? C36 C37 N7 C33 1.0(7) . . . . ? C38 C37 N7 C33 -179.4(4) . . . . ? C36 C37 N7 Cd2 -166.7(4) . . . . ? C38 C37 N7 Cd2 12.9(5) . . . . ? C41 C42 N8 C38 -2.4(9) . . . . ? C41 C42 N8 Cd2 165.3(5) . . . . ? C39 C38 N8 C42 4.0(7) . . . . ? C37 C38 N8 C42 -176.9(5) . . . . ? C39 C38 N8 Cd2 -164.5(4) . . . . ? C37 C38 N8 Cd2 14.5(5) . . . . ? C44 C43 N9 C47 0.8(7) . . . . ? C32 C43 N9 C47 -179.6(4) . . . . ? C44 C43 N9 Cd2 179.0(3) . . . . ? C32 C43 N9 Cd2 -1.4(6) . . . . ? C46 C47 N9 C43 -3.1(7) . . . . ? C48 C47 N9 C43 175.8(4) . . . . ? C46 C47 N9 Cd2 178.5(4) . . . . ? C48 C47 N9 Cd2 -2.6(5) . . . . ? C51 C52 N10 C48 -1.1(8) . . . . ? C51 C52 N10 Cd2 -173.7(5) . . . . ? C49 C48 N10 C52 1.3(8) . . . . ? C47 C48 N10 C52 -178.7(5) . . . . ? C49 C48 N10 Cd2 174.5(4) . . . . ? C47 C48 N10 Cd2 -5.5(6) . . . . ? C55 C56 N11 C73 0.9(6) . . . . ? C57 C56 N11 C73 -178.3(4) . . . . ? C55 C56 N11 Cd2 -172.5(3) . . . . ? C57 C56 N11 Cd2 8.2(5) . . . . ? C53 C73 N11 C56 -1.8(7) . . . . ? C32 C73 N11 C56 177.2(4) . . . . ? C53 C73 N11 Cd2 171.4(3) . . . . ? C32 C73 N11 Cd2 -9.7(5) . . . . ? C60 C61 N12 C57 -1.0(7) . . . . ? C60 C61 N12 Cd2 163.7(4) . . . . ? C58 C57 N12 C61 1.8(6) . . . . ? C56 C57 N12 C61 -178.1(4) . . . . ? C58 C57 N12 Cd2 -164.3(3) . . . . ? C56 C57 N12 Cd2 15.8(5) . . . . ? C27 N6 Cd1 N5 -0.9(3) . . . . ? C31 N6 Cd1 N5 172.2(4) . . . . ? C27 N6 Cd1 N4 128.4(3) . . . . ? C31 N6 Cd1 N4 -58.6(4) . . . . ? C27 N6 Cd1 N2 -133.9(3) . . . . ? C31 N6 Cd1 N2 39.1(4) . . . . ? C27 N6 Cd1 N1 -59.6(3) . . . . ? C31 N6 Cd1 N1 113.4(3) . . . . ? C27 N6 Cd1 N3 52.4(4) . . . . ? C31 N6 Cd1 N3 -134.5(3) . . . . ? C26 N5 Cd1 N6 7.7(3) . . . . ? C22 N5 Cd1 N6 175.1(3) . . . . ? C26 N5 Cd1 N4 -84.6(3) . . . . ? C22 N5 Cd1 N4 82.7(4) . . . . ? C26 N5 Cd1 N2 97.1(3) . . . . ? C22 N5 Cd1 N2 -95.6(3) . . . . ? C26 N5 Cd1 N1 143.6(3) . . . . ? C22 N5 Cd1 N1 -49.1(3) . . . . ? C26 N5 Cd1 N3 -137.9(3) . . . . ? C22 N5 Cd1 N3 29.4(3) . . . . ? C21 N4 Cd1 N6 44.5(4) . . . . ? C17 N4 Cd1 N6 -137.6(3) . . . . ? C21 N4 Cd1 N5 122.4(3) . . . . ? C17 N4 Cd1 N5 -59.6(4) . . . . ? C21 N4 Cd1 N2 -58.8(4) . . . . ? C17 N4 Cd1 N2 119.2(3) . . . . ? C21 N4 Cd1 N1 -127.3(3) . . . . ? C17 N4 Cd1 N1 50.6(4) . . . . ? C21 N4 Cd1 N3 179.1(4) . . . . ? C17 N4 Cd1 N3 -3.0(3) . . . . ? C7 N2 Cd1 N6 113.9(3) . . . . ? C11 N2 Cd1 N6 -54.1(4) . . . . ? C7 N2 Cd1 N5 37.2(4) . . . . ? C11 N2 Cd1 N5 -130.8(3) . . . . ? C7 N2 Cd1 N4 -141.6(3) . . . . ? C11 N2 Cd1 N4 50.5(4) . . . . ? C7 N2 Cd1 N1 -11.7(3) . . . . ? C11 N2 Cd1 N1 -179.6(4) . . . . ? C7 N2 Cd1 N3 -71.3(3) . . . . ? C11 N2 Cd1 N3 120.8(4) . . . . ? C2 N1 Cd1 N6 93.5(3) . . . . ? C6 N1 Cd1 N6 -81.5(3) . . . . ? C2 N1 Cd1 N5 37.1(3) . . . . ? C6 N1 Cd1 N5 -137.9(3) . . . . ? C2 N1 Cd1 N4 -96.5(3) . . . . ? C6 N1 Cd1 N4 88.5(3) . . . . ? C2 N1 Cd1 N2 -176.3(4) . . . . ? C6 N1 Cd1 N2 8.7(3) . . . . ? C2 N1 Cd1 N3 -45.2(3) . . . . ? C6 N1 Cd1 N3 139.8(3) . . . . ? C12 N3 Cd1 N6 -90.4(4) . . . . ? C16 N3 Cd1 N6 91.9(3) . . . . ? C12 N3 Cd1 N5 -39.5(3) . . . . ? C16 N3 Cd1 N5 142.8(3) . . . . ? C12 N3 Cd1 N4 -179.7(4) . . . . ? C16 N3 Cd1 N4 2.7(3) . . . . ? C12 N3 Cd1 N2 96.9(3) . . . . ? C16 N3 Cd1 N2 -80.7(3) . . . . ? C12 N3 Cd1 N1 40.3(3) . . . . ? C16 N3 Cd1 N1 -137.4(3) . . . . ? C52 N10 Cd2 N9 175.8(5) . . . . ? C48 N10 Cd2 N9 3.1(3) . . . . ? C52 N10 Cd2 N8 -53.6(4) . . . . ? C48 N10 Cd2 N8 133.8(4) . . . . ? C52 N10 Cd2 N11 118.9(4) . . . . ? C48 N10 Cd2 N11 -53.8(4) . . . . ? C52 N10 Cd2 N7 -128.4(4) . . . . ? C48 N10 Cd2 N7 58.9(4) . . . . ? C52 N10 Cd2 N12 47.5(4) . . . . ? C48 N10 Cd2 N12 -125.2(4) . . . . ? C43 N9 Cd2 N10 -178.4(4) . . . . ? C47 N9 Cd2 N10 -0.1(3) . . . . ? C43 N9 Cd2 N8 91.5(4) . . . . ? C47 N9 Cd2 N8 -90.2(4) . . . . ? C43 N9 Cd2 N11 -41.5(4) . . . . ? C47 N9 Cd2 N11 136.8(3) . . . . ? C43 N9 Cd2 N7 38.1(4) . . . . ? C47 N9 Cd2 N7 -143.6(3) . . . . ? C43 N9 Cd2 N12 -93.8(4) . . . . ? C47 N9 Cd2 N12 84.5(4) . . . . ? C42 N8 Cd2 N10 52.7(5) . . . . ? C38 N8 Cd2 N10 -139.3(3) . . . . ? C42 N8 Cd2 N9 129.3(4) . . . . ? C38 N8 Cd2 N9 -62.6(4) . . . . ? C42 N8 Cd2 N11 -119.5(4) . . . . ? C38 N8 Cd2 N11 48.6(4) . . . . ? C42 N8 Cd2 N7 -173.8(5) . . . . ? C38 N8 Cd2 N7 -5.7(3) . . . . ? C42 N8 Cd2 N12 -46.5(5) . . . . ? C38 N8 Cd2 N12 121.6(3) . . . . ? C56 N11 Cd2 N10 -84.4(3) . . . . ? C73 N11 Cd2 N10 102.3(4) . . . . ? C56 N11 Cd2 N9 -139.4(3) . . . . ? C73 N11 Cd2 N9 47.3(3) . . . . ? C56 N11 Cd2 N8 85.9(3) . . . . ? C73 N11 Cd2 N8 -87.4(4) . . . . ? C56 N11 Cd2 N7 137.7(3) . . . . ? C73 N11 Cd2 N7 -35.7(3) . . . . ? C56 N11 Cd2 N12 -0.2(3) . . . . ? C73 N11 Cd2 N12 -173.5(4) . . . . ? C33 N7 Cd2 N10 -83.7(4) . . . . ? C37 N7 Cd2 N10 83.7(4) . . . . ? C33 N7 Cd2 N9 -30.7(4) . . . . ? C37 N7 Cd2 N9 136.7(3) . . . . ? C33 N7 Cd2 N8 -171.6(4) . . . . ? C37 N7 Cd2 N8 -4.2(3) . . . . ? C33 N7 Cd2 N11 47.7(4) . . . . ? C37 N7 Cd2 N11 -144.9(3) . . . . ? C33 N7 Cd2 N12 101.6(4) . . . . ? C37 N7 Cd2 N12 -91.1(3) . . . . ? C61 N12 Cd2 N10 -46.5(4) . . . . ? C57 N12 Cd2 N10 118.8(3) . . . . ? C61 N12 Cd2 N9 -119.3(4) . . . . ? C57 N12 Cd2 N9 46.0(4) . . . . ? C61 N12 Cd2 N8 56.7(4) . . . . ? C57 N12 Cd2 N8 -138.0(3) . . . . ? C61 N12 Cd2 N11 -173.7(4) . . . . ? C57 N12 Cd2 N11 -8.5(3) . . . . ? C61 N12 Cd2 N7 129.7(4) . . . . ? C57 N12 Cd2 N7 -65.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.755 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.098