# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Jan Janczak' 'Ryszard Kubiak' _publ_contact_author_name 'Jan Janczak' _publ_contact_author_email J.JANCZAK@INT.PAN.WROC.PL _publ_section_title ; Pyrazine control of the supramolecular chemistry of iron(II) and cobalt(II) phthalocyanines ; # Attachment 'CO_Comp_II.cif' data_Co_Comp_II _database_code_depnum_ccdc_archive 'CCDC 767377' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H36 Co2 N18, 2(C36 H20 Co N10), 3(C4 H4 N2)' _chemical_formula_sum 'C152 H88 Co4 N44' _chemical_formula_weight 2766.38 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' Co Co 0.3494 0.9721 '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 11.9041(18) _cell_length_b 14.8949(22) _cell_length_c 18.2861(27) _cell_angle_alpha 103.601(11) _cell_angle_beta 90.669(10) _cell_angle_gamma 98.660(11) _cell_volume 3111.7(8) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1523 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.16 _exptl_crystal_description paralellepiped _exptl_crystal_colour violet _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 1.47 _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method floatation _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8162 _exptl_absorpt_correction_T_max 0.8772 _exptl_absorpt_process_details ; Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'KUMA KM-4 with area CCD detector' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33858 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.2365 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 28.18 _reflns_number_total 13968 _reflns_number_gt 7517 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Oxford Diffraction Poland (2006). CrysAlis CCD, Version 171.32.6 ; _computing_cell_refinement ; Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6 ; _computing_data_reduction ; Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular Structure Visualisation, University of Bonn, Germany ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0010P)^2^] 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 13968 _refine_ls_number_parameters 901 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1850 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0465 _refine_ls_wR_factor_gt 0.0397 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 Co1 Co 0.71063(3) 0.49777(3) 0.43575(2) 0.04462(13) Uani 1 1 d . . . N1 N 0.63940(18) 0.50435(19) 0.52991(12) 0.0398(6) Uani 1 1 d . . . N2 N 0.5878(2) 0.33862(19) 0.52667(16) 0.0468(7) Uani 1 1 d . . . N3 N 0.67997(19) 0.36278(16) 0.41354(15) 0.0426(7) Uani 1 1 d . . . N4 N 0.7588(2) 0.32324(19) 0.29076(14) 0.0482(7) Uani 1 1 d . . . N5 N 0.76469(18) 0.49070(19) 0.33658(13) 0.0426(7) Uani 1 1 d . . . N6 N 0.80368(19) 0.65654(18) 0.33744(15) 0.0448(7) Uani 1 1 d . . . N7 N 0.72582(18) 0.63185(15) 0.45424(14) 0.0394(6) Uani 1 1 d . . . N8 N 0.6563(2) 0.67217(19) 0.58023(14) 0.0497(7) Uani 1 1 d . . . C1 C 0.6260(3) 0.5839(3) 0.58369(19) 0.0434(9) Uani 1 1 d . . . C2 C 0.5704(2) 0.5595(3) 0.6488(2) 0.0455(9) Uani 1 1 d . . . C3 C 0.5411(3) 0.6134(2) 0.7167(2) 0.0602(10) Uani 1 1 d . . . H3 H 0.5549 0.6784 0.7274 0.072 Uiso 1 1 calc R . . C4 C 0.4902(3) 0.5658(3) 0.76810(18) 0.0695(11) Uani 1 1 d . . . H4 H 0.4689 0.5995 0.8140 0.083 Uiso 1 1 calc R . . C5 C 0.4707(3) 0.4674(3) 0.7512(2) 0.0646(10) Uani 1 1 d . . . H5 H 0.4380 0.4374 0.7868 0.077 Uiso 1 1 calc R . . C6 C 0.4986(3) 0.4138(2) 0.6832(2) 0.0555(10) Uani 1 1 d . . . H6 H 0.4839 0.3488 0.6720 0.067 Uiso 1 1 calc R . . C7 C 0.5500(2) 0.4619(3) 0.63228(19) 0.0445(9) Uani 1 1 d . . . C8 C 0.5929(2) 0.4283(3) 0.55861(18) 0.0404(8) Uani 1 1 d . . . C9 C 0.6281(3) 0.3080(2) 0.4593(2) 0.0464(9) Uani 1 1 d . . . C10 C 0.6258(3) 0.2102(3) 0.42407(19) 0.0476(9) Uani 1 1 d . . . C11 C 0.5814(3) 0.1284(3) 0.44612(18) 0.0612(10) Uani 1 1 d . . . H11 H 0.5428 0.1314 0.4904 0.073 Uiso 1 1 calc R . . C12 C 0.5961(3) 0.0446(3) 0.4012(2) 0.0735(12) Uani 1 1 d . . . H12 H 0.5676 -0.0101 0.4154 0.088 Uiso 1 1 calc R . . C13 C 0.6536(3) 0.0387(2) 0.3338(2) 0.0733(11) Uani 1 1 d . . . H13 H 0.6630 -0.0194 0.3042 0.088 Uiso 1 1 calc R . . C14 C 0.6967(2) 0.1202(3) 0.31154(18) 0.0607(10) Uani 1 1 d . . . H14 H 0.7347 0.1174 0.2671 0.073 Uiso 1 1 calc R . . C15 C 0.6811(3) 0.2062(2) 0.3580(2) 0.0451(9) Uani 1 1 d . . . C16 C 0.7119(3) 0.3022(2) 0.3506(2) 0.0441(9) Uani 1 1 d . . . C17 C 0.7787(2) 0.4106(3) 0.2838(2) 0.0450(9) Uani 1 1 d . . . C18 C 0.8230(2) 0.4358(3) 0.2166(2) 0.0488(9) Uani 1 1 d . . . C19 C 0.8511(3) 0.3807(2) 0.1482(2) 0.0728(11) Uani 1 1 d . . . H19 H 0.8447 0.3161 0.1398 0.087 Uiso 1 1 calc R . . C20 C 0.8892(3) 0.4275(3) 0.0934(2) 0.0905(13) Uani 1 1 d . . . H20 H 0.9077 0.3933 0.0470 0.109 Uiso 1 1 calc R . . C21 C 0.9004(3) 0.5266(3) 0.1069(2) 0.0861(12) Uani 1 1 d . . . H21 H 0.9264 0.5559 0.0693 0.103 Uiso 1 1 calc R . . C22 C 0.8733(3) 0.5799(2) 0.1751(2) 0.0682(11) Uani 1 1 d . . . H22 H 0.8810 0.6447 0.1842 0.082 Uiso 1 1 calc R . . C23 C 0.8339(2) 0.5330(3) 0.22948(19) 0.0493(9) Uani 1 1 d . . . C24 C 0.7989(2) 0.5658(3) 0.30490(19) 0.0440(8) Uani 1 1 d . . . C25 C 0.7711(2) 0.6861(2) 0.40634(19) 0.0423(8) Uani 1 1 d . . . C26 C 0.7792(3) 0.7838(2) 0.44320(18) 0.0467(9) Uani 1 1 d . . . C27 C 0.8228(3) 0.8644(3) 0.41995(18) 0.0626(10) Uani 1 1 d . . . H27 H 0.8518 0.8608 0.3725 0.075 Uiso 1 1 calc R . . C28 C 0.8212(3) 0.9500(2) 0.4702(2) 0.0760(12) Uani 1 1 d . . . H28 H 0.8501 1.0047 0.4560 0.091 Uiso 1 1 calc R . . C29 C 0.7774(3) 0.9564(2) 0.5416(2) 0.0786(12) Uani 1 1 d . . . H29 H 0.7780 1.0149 0.5739 0.094 Uiso 1 1 calc R . . C30 C 0.7333(3) 0.8768(3) 0.56485(18) 0.0640(10) Uani 1 1 d . . . H30 H 0.7031 0.8805 0.6119 0.077 Uiso 1 1 calc R . . C31 C 0.7362(3) 0.7904(2) 0.5141(2) 0.0473(9) Uani 1 1 d . . . C32 C 0.7033(2) 0.6934(2) 0.5195(2) 0.0447(9) Uani 1 1 d . . . N9 N 0.8865(2) 0.50278(18) 0.47795(14) 0.0538(7) Uani 1 1 d . . . C33 C 0.9750(4) 0.5487(2) 0.45223(19) 0.0754(11) Uani 1 1 d . . . H33 H 0.9627 0.5844 0.4183 0.090 Uiso 1 1 calc R . . C34 C 0.9132(3) 0.4548(2) 0.5253(2) 0.0733(11) Uani 1 1 d . . . H34 H 0.8542 0.4209 0.5452 0.088 Uiso 1 1 calc R . . Co1B Co 0.95254(4) 0.98040(3) 0.84791(2) 0.04757(13) Uani 1 1 d . . . N1B N 0.8005(2) 0.92727(16) 0.86371(14) 0.0454(7) Uani 1 1 d . . . N2B N 0.6909(2) 0.99771(18) 0.78568(14) 0.0524(8) Uani 1 1 d . . . N3B N 0.8928(2) 1.05461(16) 0.78785(12) 0.0440(7) Uani 1 1 d . . . N4B N 1.0675(2) 1.14795(16) 0.76319(13) 0.0478(7) Uani 1 1 d . . . N5B N 1.10334(19) 1.04446(15) 0.84366(13) 0.0422(7) Uani 1 1 d . . . N6B N 1.2121(2) 0.97428(18) 0.92211(14) 0.0471(7) Uani 1 1 d . . . N7B N 1.0100(2) 0.91800(15) 0.91861(12) 0.0423(7) Uani 1 1 d . . . N8B N 0.8331(2) 0.83220(16) 0.95049(14) 0.0459(7) Uani 1 1 d . . . C1B C 0.7669(3) 0.8647(2) 0.90800(17) 0.0450(9) Uani 1 1 d . . . C2B C 0.6438(3) 0.8382(2) 0.90250(18) 0.0451(9) Uani 1 1 d . . . C3B C 0.5713(3) 0.7794(2) 0.93616(17) 0.0564(9) Uani 1 1 d . . . H3B H 0.5988 0.7482 0.9693 0.068 Uiso 1 1 calc R . . C4B C 0.4567(3) 0.7696(2) 0.91796(19) 0.0652(11) Uani 1 1 d . . . H4B H 0.4054 0.7311 0.9396 0.078 Uiso 1 1 calc R . . C5B C 0.4158(3) 0.8158(2) 0.8680(2) 0.0657(10) Uani 1 1 d . . . H5B H 0.3380 0.8072 0.8567 0.079 Uiso 1 1 calc R . . C6B C 0.4888(3) 0.8745(2) 0.83468(17) 0.0601(10) Uani 1 1 d . . . H6B H 0.4613 0.9051 0.8010 0.072 Uiso 1 1 calc R . . C7B C 0.6033(3) 0.8858(2) 0.85330(18) 0.0496(9) Uani 1 1 d . . . C8B C 0.7018(3) 0.9407(2) 0.83048(18) 0.0470(9) Uani 1 1 d . . . C9B C 0.7809(3) 1.0508(2) 0.76757(16) 0.0447(9) Uani 1 1 d . . . C10B C 0.7709(3) 1.1171(2) 0.72041(17) 0.0458(9) Uani 1 1 d . . . C11B C 0.6774(3) 1.1395(2) 0.68595(18) 0.0593(10) Uani 1 1 d . . . H11B H 0.6037 1.1125 0.6925 0.071 Uiso 1 1 calc R . . C12B C 0.6979(3) 1.2036(2) 0.64148(17) 0.0670(11) Uani 1 1 d . . . H12B H 0.6372 1.2202 0.6179 0.080 Uiso 1 1 calc R . . C13B C 0.8085(4) 1.2429(2) 0.63200(19) 0.0728(12) Uani 1 1 d . . . H13B H 0.8203 1.2843 0.6009 0.087 Uiso 1 1 calc R . . C14B C 0.9017(3) 1.2229(2) 0.66716(19) 0.0640(10) Uani 1 1 d . . . H14B H 0.9752 1.2504 0.6608 0.077 Uiso 1 1 calc R . . C15B C 0.8809(3) 1.1594(2) 0.71279(17) 0.0453(9) Uani 1 1 d . . . C16B C 0.9568(3) 1.1207(2) 0.75647(17) 0.0474(9) Uani 1 1 d . . . C17B C 1.1346(3) 1.1140(2) 0.80441(17) 0.0414(8) Uani 1 1 d . . . C18B C 1.2560(3) 1.1452(2) 0.81402(17) 0.0462(9) Uani 1 1 d . . . C19B C 1.3275(3) 1.2106(2) 0.78494(17) 0.0583(10) Uani 1 1 d . . . H19B H 1.2986 1.2456 0.7554 0.070 Uiso 1 1 calc R . . C20B C 1.4426(3) 1.2207(2) 0.80207(19) 0.0700(11) Uani 1 1 d . . . H20B H 1.4929 1.2633 0.7837 0.084 Uiso 1 1 calc R . . C21B C 1.4848(3) 1.1671(2) 0.84725(19) 0.0695(11) Uani 1 1 d . . . H21B H 1.5628 1.1748 0.8576 0.083 Uiso 1 1 calc R . . C22B C 1.4136(3) 1.1036(2) 0.87636(17) 0.0596(10) Uani 1 1 d . . . H22B H 1.4418 1.0691 0.9066 0.071 Uiso 1 1 calc R . . C23B C 1.2987(3) 1.0935(2) 0.85886(18) 0.0450(9) Uani 1 1 d . . . C24B C 1.2021(3) 1.0325(2) 0.87763(18) 0.0452(9) Uani 1 1 d . . . C25B C 1.1225(3) 0.9224(2) 0.94164(18) 0.0433(9) Uani 1 1 d . . . C26B C 1.1293(3) 0.8625(2) 0.99281(17) 0.0437(9) Uani 1 1 d . . . C27B C 1.2216(3) 0.8419(2) 1.02968(16) 0.0498(9) Uani 1 1 d . . . H27B H 1.2957 0.8689 1.0241 0.060 Uiso 1 1 calc R . . C28B C 1.1982(3) 0.7794(2) 1.07512(16) 0.0572(9) Uani 1 1 d . . . H28B H 1.2581 0.7632 1.0997 0.069 Uiso 1 1 calc R . . C29B C 1.0865(3) 0.7404(2) 1.08484(16) 0.0570(10) Uani 1 1 d . . . H29B H 1.0735 0.6993 1.1162 0.068 Uiso 1 1 calc R . . C30B C 0.9956(3) 0.7618(2) 1.04870(17) 0.0519(9) Uani 1 1 d . . . H30B H 0.9212 0.7364 1.0555 0.062 Uiso 1 1 calc R . . C31B C 1.0189(3) 0.8233(2) 1.00137(17) 0.0436(9) Uani 1 1 d . . . C32B C 0.9457(3) 0.8579(2) 0.95493(16) 0.0421(8) Uani 1 1 d . . . N9B N 0.9686(2) 0.8676(2) 0.74630(16) 0.0620(8) Uani 1 1 d . . . C33B C 1.0005(3) 0.8861(3) 0.6820(3) 0.0761(12) Uani 1 1 d . . . H33B H 1.0191 0.9482 0.6795 0.091 Uiso 1 1 calc R . . C34B C 1.0073(3) 0.8157(4) 0.6178(2) 0.0927(13) Uani 1 1 d . . . H34B H 1.0304 0.8328 0.5739 0.111 Uiso 1 1 calc R . . N10B N 0.9825(3) 0.7257(3) 0.6161(2) 0.0999(12) Uani 1 1 d . . . C35B C 0.9499(4) 0.7097(3) 0.6811(3) 0.1011(18) Uani 1 1 d . . . H35B H 0.9304 0.6476 0.6836 0.125 Uiso 1 1 calc R . . C36B C 0.9423(3) 0.7785(3) 0.7465(2) 0.0904(15) Uani 1 1 d . . . H36B H 0.9185 0.7615 0.7904 0.109 Uiso 1 1 calc R . . N1C N 0.7572(5) 0.4461(7) 0.8736(6) 0.121(2) Uani 1 1 d . . . C1C C 0.7677(6) 0.5369(9) 0.8993(4) 0.120(3) Uani 1 1 d . . . H1C H 0.7543 0.5622 0.9493 0.143 Uiso 1 1 calc R . . C2C C 0.7965(8) 0.5905(7) 0.8553(8) 0.123(4) Uani 1 1 d . . . H2C H 0.8001 0.6542 0.8763 0.145 Uiso 1 1 calc R . . N2C N 0.8213(7) 0.5681(8) 0.7856(6) 0.128(4) Uani 1 1 d . . . C3C C 0.8135(6) 0.4778(9) 0.7633(4) 0.129(3) Uani 1 1 d . . . H3C H 0.8330 0.4534 0.7143 0.154 Uiso 1 1 calc R . . C4C C 0.7797(6) 0.4175(4) 0.8051(6) 0.122(2) Uani 1 1 d . . . H4C H 0.7725 0.3536 0.7839 0.148 Uiso 1 1 calc R . . N1D N 0.4146(6) 0.5251(13) -0.0362(6) 0.122(2) Uani 1 1 d . . . C1D C 0.4838(11) 0.5884(5) 0.0126(7) 0.126(2) Uani 1 1 d . . . H1D H 0.4728 0.6505 0.0215 0.150 Uiso 1 1 calc R . . C2D C 0.5653(10) 0.5687(9) 0.0482(4) 0.124(2) Uani 1 1 d . . . H2D H 0.6121 0.6161 0.0823 0.147 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0444(3) 0.0458(3) 0.0441(3) 0.0092(2) 0.0026(2) 0.0076(2) N1 0.0407(16) 0.0388(18) 0.0402(18) 0.0085(16) 0.0019(14) 0.0092(14) N2 0.0547(19) 0.0402(19) 0.044(2) 0.0091(17) -0.0011(16) 0.0066(15) N3 0.0438(16) 0.0415(18) 0.0419(18) 0.0097(16) -0.0009(14) 0.0057(14) N4 0.0544(19) 0.0401(19) 0.047(2) 0.0061(17) 0.0085(15) 0.0050(15) N5 0.0454(16) 0.0370(18) 0.0466(19) 0.0100(16) 0.0080(14) 0.0099(14) N6 0.0504(18) 0.0411(19) 0.0422(19) 0.0078(16) 0.0109(15) 0.0073(15) N7 0.0447(16) 0.0410(18) 0.0328(17) 0.0075(15) 0.0033(14) 0.0095(13) N8 0.0556(19) 0.049(2) 0.044(2) 0.0103(17) 0.0026(15) 0.0106(16) C1 0.045(2) 0.041(3) 0.044(3) 0.009(2) -0.0043(19) 0.008(2) C2 0.051(2) 0.046(3) 0.040(2) 0.007(2) 0.0018(19) 0.0122(19) C3 0.069(3) 0.059(3) 0.051(3) 0.006(2) 0.013(2) 0.014(2) C4 0.083(3) 0.076(3) 0.047(3) 0.008(2) 0.013(2) 0.016(2) C5 0.066(3) 0.080(3) 0.052(3) 0.025(2) 0.008(2) 0.012(2) C6 0.061(2) 0.060(3) 0.047(2) 0.016(2) 0.008(2) 0.011(2) C7 0.045(2) 0.051(3) 0.039(2) 0.014(2) -0.0004(19) 0.0067(19) C8 0.039(2) 0.049(3) 0.033(2) 0.006(2) -0.0022(17) 0.0087(19) C9 0.046(2) 0.046(3) 0.044(2) 0.011(2) -0.007(2) -0.0006(19) C10 0.057(2) 0.041(3) 0.042(2) 0.005(2) -0.0005(19) 0.003(2) C11 0.077(3) 0.048(3) 0.055(3) 0.009(2) 0.004(2) 0.004(2) C12 0.103(3) 0.046(3) 0.067(3) 0.015(3) -0.003(3) -0.003(2) C13 0.096(3) 0.046(3) 0.077(3) 0.012(2) -0.005(3) 0.012(2) C14 0.068(2) 0.055(3) 0.057(3) 0.001(2) -0.006(2) 0.007(2) C15 0.050(2) 0.039(2) 0.042(2) -0.001(2) -0.0069(19) 0.008(2) C16 0.044(2) 0.040(3) 0.046(3) 0.005(2) 0.0023(19) 0.0060(19) C17 0.036(2) 0.046(3) 0.051(3) 0.007(2) 0.0105(18) 0.0060(19) C18 0.054(2) 0.042(3) 0.041(2) -0.004(2) 0.0187(19) 0.0010(19) C19 0.076(3) 0.061(2) 0.063(3) -0.012(2) 0.024(2) -0.006(2) C20 0.119(3) 0.071(3) 0.062(3) -0.008(3) 0.040(2) -0.009(3) C21 0.113(3) 0.074(3) 0.065(3) 0.017(3) 0.033(3) -0.010(3) C22 0.088(3) 0.060(3) 0.050(3) 0.005(2) 0.021(2) 0.000(2) C23 0.052(2) 0.052(3) 0.039(2) 0.005(2) 0.0114(19) 0.0035(19) C24 0.040(2) 0.042(2) 0.045(2) 0.001(2) 0.0017(18) 0.0058(19) C25 0.046(2) 0.041(2) 0.039(2) 0.006(2) 0.0022(19) 0.0124(18) C26 0.060(2) 0.044(2) 0.040(2) 0.015(2) 0.0101(19) 0.0126(19) C27 0.090(3) 0.053(3) 0.047(2) 0.011(2) 0.010(2) 0.015(2) C28 0.115(3) 0.039(3) 0.074(3) 0.013(2) 0.016(3) 0.010(2) C29 0.123(3) 0.045(3) 0.066(3) 0.008(2) 0.027(3) 0.014(2) C30 0.086(3) 0.060(3) 0.048(2) 0.011(2) 0.015(2) 0.020(2) C31 0.057(2) 0.038(3) 0.049(3) 0.012(2) 0.000(2) 0.010(2) C32 0.041(2) 0.048(3) 0.045(3) 0.009(2) 0.0036(19) 0.0118(19) N9 0.060(2) 0.0583(17) 0.0575(18) 0.0358(14) 0.0023(16) 0.0154(16) C33 0.049(3) 0.098(3) 0.099(3) 0.080(2) -0.013(3) 0.002(2) C34 0.058(3) 0.093(3) 0.080(3) 0.070(2) -0.001(2) -0.009(2) Co1B 0.0451(3) 0.0494(3) 0.0500(3) 0.0154(2) 0.0032(2) 0.0077(2) N1B 0.0351(17) 0.0508(18) 0.0516(18) 0.0115(15) -0.0009(15) 0.0073(14) N2B 0.0497(19) 0.0495(19) 0.059(2) 0.0165(16) 0.0050(17) 0.0057(16) N3B 0.0392(18) 0.0511(18) 0.0440(17) 0.0139(14) 0.0045(15) 0.0101(15) N4B 0.0425(18) 0.0534(18) 0.0501(19) 0.0158(15) 0.0035(16) 0.0103(16) N5B 0.0376(18) 0.0450(17) 0.0460(17) 0.0106(14) 0.0046(14) 0.0058(14) N6B 0.0443(18) 0.052(2) 0.0467(19) 0.0163(16) 0.0016(15) 0.0066(16) N7B 0.0420(18) 0.0469(17) 0.0394(17) 0.0125(14) 0.0016(15) 0.0084(14) N8B 0.0396(19) 0.0486(18) 0.0503(19) 0.0125(15) 0.0009(16) 0.0089(16) C1B 0.041(3) 0.045(2) 0.049(2) 0.0102(18) 0.003(2) 0.009(2) C2B 0.031(2) 0.048(2) 0.055(2) 0.0089(19) 0.0056(19) 0.0053(19) C3B 0.048(2) 0.056(2) 0.067(3) 0.019(2) 0.006(2) 0.007(2) C4B 0.051(3) 0.063(3) 0.086(3) 0.028(2) 0.016(2) 0.005(2) C5B 0.044(2) 0.063(3) 0.088(3) 0.017(2) 0.001(2) 0.003(2) C6B 0.055(3) 0.056(2) 0.074(3) 0.024(2) 0.002(2) 0.011(2) C7B 0.039(2) 0.047(2) 0.064(3) 0.016(2) -0.003(2) 0.006(2) C8B 0.040(3) 0.048(2) 0.050(2) 0.0103(18) 0.006(2) 0.002(2) C9B 0.046(2) 0.046(2) 0.043(2) 0.0074(18) 0.001(2) 0.015(2) C10B 0.047(2) 0.049(2) 0.046(2) 0.0160(18) 0.001(2) 0.016(2) C11B 0.052(2) 0.066(3) 0.059(3) 0.011(2) 0.000(2) 0.012(2) C12B 0.085(3) 0.064(3) 0.057(3) 0.022(2) -0.011(2) 0.019(2) C13B 0.074(3) 0.070(3) 0.084(3) 0.038(2) -0.005(3) 0.013(3) C14B 0.061(3) 0.066(3) 0.071(3) 0.032(2) 0.006(2) 0.005(2) C15B 0.040(2) 0.052(2) 0.046(2) 0.0133(18) 0.0022(19) 0.0118(19) C16B 0.048(2) 0.051(2) 0.042(2) 0.0086(19) 0.006(2) 0.010(2) C17B 0.030(2) 0.049(2) 0.043(2) 0.0056(18) -0.0002(18) 0.0088(18) C18B 0.045(2) 0.049(2) 0.041(2) 0.0083(18) 0.0023(19) 0.003(2) C19B 0.053(3) 0.050(2) 0.072(3) 0.019(2) 0.011(2) 0.004(2) C20B 0.064(3) 0.064(3) 0.083(3) 0.027(2) 0.013(2) -0.005(2) C21B 0.037(2) 0.076(3) 0.094(3) 0.024(2) -0.001(2) -0.002(2) C22B 0.053(3) 0.060(2) 0.068(3) 0.015(2) -0.001(2) 0.000(2) C23B 0.038(2) 0.045(2) 0.049(2) 0.0073(19) 0.006(2) 0.002(2) C24B 0.045(2) 0.043(2) 0.044(2) 0.0019(19) 0.004(2) 0.009(2) C25B 0.038(2) 0.045(2) 0.045(2) 0.0055(19) 0.003(2) 0.009(2) C26B 0.047(2) 0.044(2) 0.041(2) 0.0100(18) -0.001(2) 0.008(2) C27B 0.050(2) 0.055(2) 0.046(2) 0.0163(18) 0.0035(19) 0.0044(19) C28B 0.062(3) 0.064(3) 0.049(2) 0.017(2) -0.006(2) 0.012(2) C29B 0.062(3) 0.057(2) 0.053(2) 0.0145(19) 0.005(2) 0.004(2) C30B 0.054(2) 0.050(2) 0.052(2) 0.0085(19) 0.000(2) 0.012(2) C31B 0.050(3) 0.041(2) 0.041(2) 0.0080(18) 0.007(2) 0.011(2) C32B 0.052(2) 0.044(2) 0.032(2) 0.0075(17) 0.001(2) 0.014(2) N9B 0.0628(18) 0.061(2) 0.062(2) 0.0055(19) 0.0030(17) 0.0019(16) C33B 0.097(3) 0.061(3) 0.062(3) -0.002(3) 0.016(3) 0.012(2) C34B 0.100(3) 0.096(3) 0.066(3) -0.010(3) 0.017(3) 0.009(3) N10B 0.120(3) 0.080(3) 0.085(3) -0.012(3) 0.013(2) 0.017(2) C35B 0.102(5) 0.086(4) 0.107(4) 0.010(4) 0.037(4) 0.010(3) C36B 0.099(4) 0.074(3) 0.086(3) -0.002(3) 0.026(3) 0.007(3) N1C 0.125(5) 0.125(7) 0.142(6) 0.050(5) 0.033(5) 0.067(5) C1C 0.114(7) 0.116(7) 0.117(7) -0.030(6) 0.040(5) 0.060(7) C2C 0.125(8) 0.097(6) 0.145(13) 0.033(8) 0.005(10) -0.006(5) N2C 0.109(6) 0.108(8) 0.160(10) 0.038(9) 0.001(7) -0.014(6) C3C 0.135(7) 0.130(8) 0.121(6) 0.036(7) 0.013(5) 0.026(7) C4C 0.148(6) 0.095(5) 0.125(7) 0.016(6) -0.010(6) 0.048(5) N1D 0.113(7) 0.119(8) 0.134(7) 0.039(6) 0.024(6) 0.007(8) C1D 0.131(7) 0.095(5) 0.143(7) 0.028(6) -0.006(5) 0.011(6) C2D 0.127(10) 0.115(9) 0.118(6) -0.014(5) -0.005(6) 0.001(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 Co1 N5 1.916(2) . y Co1 N1 1.917(2) . y Co1 N7 1.926(2) . y Co1 N3 1.932(2) . y Co1 N9 2.207(2) . y N1 C1 1.382(3) . ? N1 C8 1.401(3) . ? N2 C8 1.318(3) . ? N2 C9 1.331(3) . ? N3 C16 1.382(3) . ? N3 C9 1.388(3) . ? N4 C16 1.316(3) . ? N4 C17 1.323(3) . ? N5 C17 1.380(3) . ? N5 C24 1.387(3) . ? N6 C25 1.317(3) . ? N6 C24 1.335(3) . ? N7 C32 1.379(3) . ? N7 C25 1.386(3) . ? N8 C1 1.327(3) . ? N8 C32 1.331(3) . ? C1 C2 1.461(4) . ? C2 C3 1.390(3) . ? C2 C7 1.396(3) . ? C3 C4 1.397(4) . ? C3 H3 0.9300 . ? C4 C5 1.408(4) . ? C4 H4 0.9300 . ? C5 C6 1.384(4) . ? C5 H5 0.9300 . ? C6 C7 1.397(4) . ? C6 H6 0.9300 . ? C7 C8 1.450(4) . ? C9 C10 1.443(4) . ? C10 C15 1.376(4) . ? C10 C11 1.403(4) . ? C11 C12 1.360(4) . ? C11 H11 0.9300 . ? C12 C13 1.408(4) . ? C12 H12 0.9300 . ? C13 C14 1.397(4) . ? C13 H13 0.9300 . ? C14 C15 1.400(4) . ? C14 H14 0.9300 . ? C15 C16 1.460(4) . ? C17 C18 1.451(4) . ? C18 C23 1.396(3) . ? C18 C19 1.399(4) . ? C19 C20 1.392(4) . ? C19 H19 0.9300 . ? C20 C21 1.423(4) . ? C20 H20 0.9300 . ? C21 C22 1.381(4) . ? C21 H21 0.9300 . ? C22 C23 1.392(4) . ? C22 H22 0.9300 . ? C23 C24 1.440(4) . ? C25 C26 1.442(3) . ? C26 C31 1.387(4) . ? C26 C27 1.395(4) . ? C27 C28 1.388(4) . ? C27 H27 0.9300 . ? C28 C29 1.399(4) . ? C28 H28 0.9300 . ? C29 C30 1.384(4) . ? C29 H29 0.9300 . ? C30 C31 1.405(3) . ? C30 H30 0.9300 . ? C31 C32 1.466(4) . ? N9 C34 1.310(3) . ? N9 C33 1.321(3) . ? C33 C34 1.401(4) 2_766 ? C33 H33 0.9300 . ? C34 C33 1.401(4) 2_766 ? C34 H34 0.9300 . ? Co1B N5B 1.913(2) . y Co1B N1B 1.917(2) . y Co1B N3B 1.930(2) . y Co1B N7B 1.933(2) . y Co1B N9B 2.225(3) . y N1B C8B 1.379(3) . ? N1B C1B 1.391(3) . ? N2B C9B 1.327(3) . ? N2B C8B 1.329(3) . ? N3B C9B 1.367(3) . ? N3B C16B 1.389(3) . ? N4B C16B 1.314(3) . ? N4B C17B 1.323(3) . ? N5B C24B 1.378(3) . ? N5B C17B 1.403(3) . ? N6B C25B 1.323(3) . ? N6B C24B 1.338(3) . ? N7B C32B 1.383(3) . ? N7B C25B 1.387(3) . ? N8B C1B 1.318(3) . ? N8B C32B 1.333(3) . ? C1B C2B 1.454(4) . ? C2B C3B 1.389(3) . ? C2B C7B 1.392(4) . ? C3B C4B 1.379(3) . ? C3B H3B 0.9300 . ? C4B C5B 1.389(4) . ? C4B H4B 0.9300 . ? C5B C6B 1.388(4) . ? C5B H5B 0.9300 . ? C6B C7B 1.377(4) . ? C6B H6B 0.9300 . ? C7B C8B 1.450(4) . ? C9B C10B 1.472(4) . ? C10B C15B 1.388(4) . ? C10B C11B 1.394(4) . ? C11B C12B 1.389(4) . ? C11B H11B 0.9300 . ? C12B C13B 1.389(4) . ? C12B H12B 0.9300 . ? C13B C14B 1.380(4) . ? C13B H13B 0.9300 . ? C14B C15B 1.399(4) . ? C14B H14B 0.9300 . ? C15B C16B 1.463(4) . ? C17B C18B 1.445(4) . ? C18B C23B 1.388(4) . ? C18B C19B 1.400(4) . ? C19B C20B 1.380(4) . ? C19B H19B 0.9300 . ? C20B C21B 1.412(4) . ? C20B H20B 0.9300 . ? C21B C22B 1.379(4) . ? C21B H21B 0.9300 . ? C22B C23B 1.378(4) . ? C22B H22B 0.9300 . ? C23B C24B 1.452(4) . ? C25B C26B 1.446(4) . ? C26B C31B 1.382(4) . ? C26B C27B 1.392(3) . ? C27B C28B 1.388(3) . ? C27B H27B 0.9300 . ? C28B C29B 1.399(3) . ? C28B H28B 0.9300 . ? C29B C30B 1.378(3) . ? C29B H29B 0.9300 . ? C30B C31B 1.402(4) . ? C30B H30B 0.9300 . ? C31B C32B 1.439(4) . ? N9B C33B 1.316(4) . ? N9B C36B 1.319(4) . ? C33B C34B 1.390(4) . ? C33B H33B 0.9300 . ? C34B N10B 1.322(4) . ? C34B H34B 0.9300 . ? N10B C35B 1.318(4) . ? C35B C36B 1.394(4) . ? C35B H35B 0.9300 . ? C36B H36B 0.9300 . ? N1C C4C 1.270(15) . ? N1C C1C 1.309(16) . ? C1C C2C 1.276(18) . ? C1C H1C 0.9300 . ? C2C N2C 1.288(19) . ? C2C H2C 0.9300 . ? N2C C3C 1.298(18) . ? C3C C4C 1.332(17) . ? C3C H3C 0.9300 . ? C4C H4C 0.9300 . ? N1D C1D 1.310(17) . ? N1D C2D 1.420(17) 2_665 ? C1D C2D 1.269(17) . ? C1D H1D 0.9300 . ? C2D N1D 1.420(17) 2_665 ? C2D H2D 0.9300 . ? 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 N5 Co1 N1 173.38(9) . . y N5 Co1 N7 90.56(11) . . y N1 Co1 N7 89.07(11) . . y N5 Co1 N3 89.54(12) . . y N1 Co1 N3 90.17(11) . . y N7 Co1 N3 174.27(9) . . y N5 Co1 N9 89.25(10) . . y N1 Co1 N9 97.37(10) . . y N7 Co1 N9 92.98(9) . . y N3 Co1 N9 92.75(9) . . y C1 N1 C8 106.3(3) . . ? C1 N1 Co1 127.4(2) . . ? C8 N1 Co1 126.3(2) . . ? C8 N2 C9 122.6(3) . . ? C16 N3 C9 106.7(3) . . ? C16 N3 Co1 126.2(2) . . ? C9 N3 Co1 127.0(2) . . ? C16 N4 C17 121.4(3) . . ? C17 N5 C24 107.2(3) . . ? C17 N5 Co1 126.6(2) . . ? C24 N5 Co1 126.1(2) . . ? C25 N6 C24 122.2(3) . . ? C32 N7 C25 106.4(3) . . ? C32 N7 Co1 127.2(2) . . ? C25 N7 Co1 126.2(2) . . ? C1 N8 C32 121.1(3) . . ? N8 C1 N1 127.4(3) . . ? N8 C1 C2 121.7(3) . . ? N1 C1 C2 110.8(3) . . ? C3 C2 C7 121.7(3) . . ? C3 C2 C1 132.6(3) . . ? C7 C2 C1 105.7(3) . . ? C2 C3 C4 117.2(3) . . ? C2 C3 H3 121.4 . . ? C4 C3 H3 121.4 . . ? C3 C4 C5 120.7(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 122.1(3) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 116.9(3) . . ? C5 C6 H6 121.6 . . ? C7 C6 H6 121.6 . . ? C2 C7 C6 121.5(3) . . ? C2 C7 C8 107.4(3) . . ? C6 C7 C8 131.1(3) . . ? N2 C8 N1 127.5(3) . . ? N2 C8 C7 122.8(3) . . ? N1 C8 C7 109.7(3) . . ? N2 C9 N3 126.4(3) . . ? N2 C9 C10 123.5(3) . . ? N3 C9 C10 110.1(3) . . ? C15 C10 C11 121.1(3) . . ? C15 C10 C9 106.7(3) . . ? C11 C10 C9 132.2(4) . . ? C12 C11 C10 118.4(3) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? C11 C12 C13 121.6(4) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C14 C13 C12 120.0(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 118.1(3) . . ? C13 C14 H14 120.9 . . ? C15 C14 H14 120.9 . . ? C10 C15 C14 120.8(3) . . ? C10 C15 C16 107.1(3) . . ? C14 C15 C16 132.0(4) . . ? N4 C16 N3 127.7(3) . . ? N4 C16 C15 123.1(3) . . ? N3 C16 C15 109.2(3) . . ? N4 C17 N5 127.8(3) . . ? N4 C17 C18 123.0(3) . . ? N5 C17 C18 109.2(3) . . ? C23 C18 C19 121.6(3) . . ? C23 C18 C17 107.2(3) . . ? C19 C18 C17 131.2(3) . . ? C20 C19 C18 116.7(3) . . ? C20 C19 H19 121.7 . . ? C18 C19 H19 121.7 . . ? C19 C20 C21 121.5(3) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C22 C21 C20 121.0(3) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 117.5(3) . . ? C21 C22 H22 121.3 . . ? C23 C22 H22 121.3 . . ? C22 C23 C18 121.7(3) . . ? C22 C23 C24 132.0(4) . . ? C18 C23 C24 106.3(3) . . ? N6 C24 N5 127.3(3) . . ? N6 C24 C23 122.5(3) . . ? N5 C24 C23 110.1(3) . . ? N6 C25 N7 127.3(3) . . ? N6 C25 C26 122.9(3) . . ? N7 C25 C26 109.8(3) . . ? C31 C26 C27 120.5(3) . . ? C31 C26 C25 108.0(3) . . ? C27 C26 C25 131.4(3) . . ? C28 C27 C26 117.6(3) . . ? C28 C27 H27 121.2 . . ? C26 C27 H27 121.2 . . ? C27 C28 C29 121.8(3) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C30 C29 C28 121.0(3) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 117.0(3) . . ? C29 C30 H30 121.5 . . ? C31 C30 H30 121.5 . . ? C26 C31 C30 122.2(3) . . ? C26 C31 C32 105.0(3) . . ? C30 C31 C32 132.8(4) . . ? N8 C32 N7 127.2(3) . . ? N8 C32 C31 122.0(3) . . ? N7 C32 C31 110.7(3) . . ? C34 N9 C33 114.2(3) . . ? C34 N9 Co1 123.4(3) . . ? C33 N9 Co1 122.2(3) . . ? N9 C33 C34 121.8(3) . 2_766 ? N9 C33 H33 119.1 . . ? C34 C33 H33 119.1 2_766 . ? N9 C34 C33 124.0(3) . 2_766 ? N9 C34 H34 118.0 . . ? C33 C34 H34 118.0 2_766 . ? N5B Co1B N1B 172.92(10) . . y N5B Co1B N3B 90.70(11) . . y N1B Co1B N3B 89.81(11) . . y N5B Co1B N7B 89.09(11) . . y N1B Co1B N7B 89.55(11) . . y N3B Co1B N7B 173.03(10) . . y N5B Co1B N9B 93.54(10) . . y N1B Co1B N9B 93.50(10) . . y N3B Co1B N9B 91.72(11) . . y N7B Co1B N9B 95.25(10) . . y C8B N1B C1B 105.9(3) . . ? C8B N1B Co1B 126.5(2) . . ? C1B N1B Co1B 127.6(2) . . ? C9B N2B C8B 121.1(3) . . ? C9B N3B C16B 107.8(3) . . ? C9B N3B Co1B 126.5(2) . . ? C16B N3B Co1B 125.7(2) . . ? C16B N4B C17B 122.1(3) . . ? C24B N5B C17B 106.2(3) . . ? C24B N5B Co1B 127.9(2) . . ? C17B N5B Co1B 125.9(2) . . ? C25B N6B C24B 122.0(3) . . ? C32B N7B C25B 106.5(3) . . ? C32B N7B Co1B 126.1(2) . . ? C25B N7B Co1B 127.4(2) . . ? C1B N8B C32B 121.3(3) . . ? N8B C1B N1B 127.1(3) . . ? N8B C1B C2B 122.4(3) . . ? N1B C1B C2B 110.5(3) . . ? C3B C2B C7B 122.0(3) . . ? C3B C2B C1B 131.9(3) . . ? C7B C2B C1B 106.1(3) . . ? C4B C3B C2B 116.7(3) . . ? C4B C3B H3B 121.6 . . ? C2B C3B H3B 121.6 . . ? C3B C4B C5B 121.6(3) . . ? C3B C4B H4B 119.2 . . ? C5B C4B H4B 119.2 . . ? C6B C5B C4B 121.4(3) . . ? C6B C5B H5B 119.3 . . ? C4B C5B H5B 119.3 . . ? C7B C6B C5B 117.5(3) . . ? C7B C6B H6B 121.2 . . ? C5B C6B H6B 121.2 . . ? C6B C7B C2B 120.8(3) . . ? C6B C7B C8B 132.6(4) . . ? C2B C7B C8B 106.6(3) . . ? N2B C8B N1B 127.8(3) . . ? N2B C8B C7B 121.3(3) . . ? N1B C8B C7B 110.9(3) . . ? N2B C9B N3B 128.0(3) . . ? N2B C9B C10B 122.3(3) . . ? N3B C9B C10B 109.8(3) . . ? C15B C10B C11B 121.4(3) . . ? C15B C10B C9B 106.4(3) . . ? C11B C10B C9B 132.2(3) . . ? C12B C11B C10B 117.8(3) . . ? C12B C11B H11B 121.1 . . ? C10B C11B H11B 121.1 . . ? C13B C12B C11B 120.4(3) . . ? C13B C12B H12B 119.8 . . ? C11B C12B H12B 119.8 . . ? C14B C13B C12B 122.4(4) . . ? C14B C13B H13B 118.8 . . ? C12B C13B H13B 118.8 . . ? C13B C14B C15B 117.3(3) . . ? C13B C14B H14B 121.4 . . ? C15B C14B H14B 121.4 . . ? C10B C15B C14B 120.7(3) . . ? C10B C15B C16B 106.9(3) . . ? C14B C15B C16B 132.3(3) . . ? N4B C16B N3B 128.0(3) . . ? N4B C16B C15B 122.8(3) . . ? N3B C16B C15B 109.2(3) . . ? N4B C17B N5B 127.5(3) . . ? N4B C17B C18B 122.7(3) . . ? N5B C17B C18B 109.8(3) . . ? C23B C18B C19B 121.6(3) . . ? C23B C18B C17B 106.8(3) . . ? C19B C18B C17B 131.5(3) . . ? C20B C19B C18B 117.0(3) . . ? C20B C19B H19B 121.5 . . ? C18B C19B H19B 121.5 . . ? C19B C20B C21B 120.7(3) . . ? C19B C20B H20B 119.7 . . ? C21B C20B H20B 119.7 . . ? C22B C21B C20B 121.8(3) . . ? C22B C21B H21B 119.1 . . ? C20B C21B H21B 119.1 . . ? C23B C22B C21B 117.3(3) . . ? C23B C22B H22B 121.4 . . ? C21B C22B H22B 121.4 . . ? C22B C23B C18B 121.6(3) . . ? C22B C23B C24B 131.7(3) . . ? C18B C23B C24B 106.7(3) . . ? N6B C24B N5B 126.8(3) . . ? N6B C24B C23B 122.8(3) . . ? N5B C24B C23B 110.4(3) . . ? N6B C25B N7B 126.5(3) . . ? N6B C25B C26B 123.6(3) . . ? N7B C25B C26B 109.8(3) . . ? C31B C26B C27B 121.7(3) . . ? C31B C26B C25B 106.5(3) . . ? C27B C26B C25B 131.8(3) . . ? C28B C27B C26B 117.1(3) . . ? C28B C27B H27B 121.5 . . ? C26B C27B H27B 121.5 . . ? C27B C28B C29B 121.5(3) . . ? C27B C28B H28B 119.2 . . ? C29B C28B H28B 119.2 . . ? C30B C29B C28B 121.0(3) . . ? C30B C29B H29B 119.5 . . ? C28B C29B H29B 119.5 . . ? C29B C30B C31B 117.7(3) . . ? C29B C30B H30B 121.2 . . ? C31B C30B H30B 121.2 . . ? C26B C31B C30B 121.0(3) . . ? C26B C31B C32B 107.3(3) . . ? C30B C31B C32B 131.8(3) . . ? N8B C32B N7B 128.3(3) . . ? N8B C32B C31B 121.9(3) . . ? N7B C32B C31B 109.9(3) . . ? C33B N9B C36B 116.4(3) . . ? C33B N9B Co1B 121.9(3) . . ? C36B N9B Co1B 121.6(3) . . ? N9B C33B C34B 122.1(4) . . ? N9B C33B H33B 119.0 . . ? C34B C33B H33B 119.0 . . ? N10B C34B C33B 123.2(4) . . ? N10B C34B H34B 118.4 . . ? C33B C34B H34B 118.4 . . ? C35B N10B C34B 113.2(4) . . ? N10B C35B C36B 125.1(4) . . ? N10B C35B H35B 117.4 . . ? C36B C35B H35B 117.4 . . ? N9B C36B C35B 120.0(4) . . ? N9B C36B H36B 120.0 . . ? C35B C36B H36B 120.0 . . ? C4C N1C C1C 116.1(7) . . ? C2C C1C N1C 119.7(9) . . ? C2C C1C H1C 120.2 . . ? N1C C1C H1C 120.2 . . ? C1C C2C N2C 128.5(12) . . ? C1C C2C H2C 115.7 . . ? N2C C2C H2C 115.7 . . ? C2C N2C C3C 109.7(10) . . ? N2C C3C C4C 125.1(9) . . ? N2C C3C H3C 117.5 . . ? C4C C3C H3C 117.5 . . ? N1C C4C C3C 120.9(7) . . ? N1C C4C H4C 119.6 . . ? C3C C4C H4C 119.6 . . ? C1D N1D C2D 116.7(6) . 2_665 ? C2D C1D N1D 122.8(7) . . ? C2D C1D H1D 118.6 . . ? N1D C1D H1D 118.6 . . ? C1D C2D N1D 120.5(7) . 2_665 ? C1D C2D H2D 119.8 . . ? N1D C2D H2D 119.8 2_665 . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.474 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.044 # Attachment 'CO_Comp_III.cif' data_Co_Comp_III _database_code_depnum_ccdc_archive 'CCDC 767378' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H36 Co2 N18, C40 H24 Co N12' _chemical_formula_sum 'C108 H60 Co3 N30' _chemical_formula_weight 1954.65 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' Co Co 0.3494 0.9721 '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 11.597(2) _cell_length_b 13.436(3) _cell_length_c 14.524(3) _cell_angle_alpha 103.62(2) _cell_angle_beta 98.36(1) _cell_angle_gamma 94.92(1) _cell_volume 2159.1(8) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1276 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 28.18 _exptl_crystal_description paralellepiped _exptl_crystal_colour violet _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas 1.50 _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method floatation _exptl_crystal_F_000 999 _exptl_absorpt_coefficient_mu 0.644 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.778 _exptl_absorpt_correction_T_max 0.854 _exptl_absorpt_process_details ; Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'KUMA KM-4 with area CCD detector' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24306 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.1129 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 28.18 _reflns_number_total 9493 _reflns_number_gt 5697 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Oxford Diffraction Poland (2006). CrysAlis CCD, Version 171.32.6 ; _computing_cell_refinement ; Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6 ; _computing_data_reduction ; Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular Structure Visualisation, University of Bonn, Germany ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0074P)^2^] 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 9493 _refine_ls_number_parameters 637 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0986 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0480 _refine_ls_wR_factor_gt 0.0449 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 Co1 Co 0.0000 0.0000 0.0000 0.03555(13) Uani 1 2 d S . . N1 N -0.06965(14) -0.08846(11) 0.06866(11) 0.0318(4) Uani 1 1 d . . . N2 N 0.10326(16) -0.13036(12) 0.15934(11) 0.0324(5) Uani 1 1 d . . . N3 N 0.15280(13) -0.01583(11) 0.06106(11) 0.0315(4) Uani 1 1 d . . . N4 N 0.27564(14) 0.09208(13) -0.00784(13) 0.0366(5) Uani 1 1 d . . . C1 C -0.1880(2) -0.11853(15) 0.06138(14) 0.0320(6) Uani 1 1 d . . . C2 C -0.20560(19) -0.18768(14) 0.12282(14) 0.0305(6) Uani 1 1 d . . . C3 C -0.30630(19) -0.23857(15) 0.14029(14) 0.0387(6) Uani 1 1 d . . . H3 H -0.3807 -0.2300 0.1117 0.046 Uiso 1 1 calc R . . C4 C -0.2916(2) -0.30271(15) 0.20198(15) 0.0438(6) Uani 1 1 d . . . H4 H -0.3574 -0.3370 0.2160 0.053 Uiso 1 1 calc R . . C5 C -0.1803(2) -0.31678(15) 0.24341(15) 0.0451(7) Uani 1 1 d . . . H5 H -0.1733 -0.3617 0.2833 0.054 Uiso 1 1 calc R . . C6 C -0.07957(19) -0.26551(15) 0.22675(14) 0.0395(6) Uani 1 1 d . . . H6 H -0.0052 -0.2745 0.2551 0.047 Uiso 1 1 calc R . . C7 C -0.09438(18) -0.20011(14) 0.16582(14) 0.0300(5) Uani 1 1 d . . . C8 C -0.01139(19) -0.13689(15) 0.13149(14) 0.0312(5) Uani 1 1 d . . . C9 C 0.17834(19) -0.07302(15) 0.12667(14) 0.0310(5) Uani 1 1 d . . . C10 C 0.30402(18) -0.06313(15) 0.15787(14) 0.0288(5) Uani 1 1 d . . . C11 C 0.3731(2) -0.10692(15) 0.22107(14) 0.0359(6) Uani 1 1 d . . . H11 H 0.3398 -0.1508 0.2536 0.043 Uiso 1 1 calc R . . C12 C 0.4935(2) -0.08175(16) 0.23295(15) 0.0424(6) Uani 1 1 d . . . H12 H 0.5425 -0.1093 0.2745 0.051 Uiso 1 1 calc R . . C13 C 0.54264(19) -0.01620(16) 0.18419(15) 0.0449(6) Uani 1 1 d . . . H13 H 0.6239 -0.0009 0.1939 0.054 Uiso 1 1 calc R . . C14 C 0.47407(19) 0.02685(16) 0.12167(15) 0.0433(6) Uani 1 1 d . . . H14 H 0.5075 0.0711 0.0896 0.052 Uiso 1 1 calc R . . C15 C 0.35374(19) 0.00160(15) 0.10870(15) 0.0321(6) Uani 1 1 d . . . C16 C 0.25858(19) 0.03064(15) 0.04935(14) 0.0318(5) Uani 1 1 d . . . N5 N 0.00015(16) 0.14889(15) 0.13061(15) 0.0483(5) Uani 1 1 d . . . C17 C -0.0217(2) 0.2403(2) 0.1163(2) 0.0677(8) Uani 1 1 d . . . H17 H -0.0404 0.2467 0.0536 0.081 Uiso 1 1 calc R . . C18 C -0.0175(2) 0.3256(2) 0.1918(3) 0.0701(9) Uani 1 1 d . . . H18 H -0.0340 0.3876 0.1780 0.085 Uiso 1 1 calc R . . N6 N 0.0089(2) 0.3234(2) 0.2820(2) 0.0760(8) Uani 1 1 d . . . C19 C 0.0297(3) 0.2322(3) 0.2954(2) 0.0636(12) Uani 1 1 d . . . H19 H 0.0478 0.2256 0.3580 0.076 Uiso 1 1 calc R . . C20 C 0.0259(3) 0.1470(2) 0.2207(2) 0.0677(10) Uani 1 1 d . . . H20 H 0.0423 0.0851 0.2348 0.079 Uiso 1 1 calc R . . Co1B Co 0.29954(2) 0.59114(2) 0.50201(2) 0.02964(9) Uani 1 1 d . . . N1B N 0.25841(13) 0.72766(12) 0.51032(12) 0.0297(4) Uani 1 1 d . . . N2B N 0.27010(14) 0.79131(13) 0.68216(13) 0.0354(5) Uani 1 1 d . . . N3B N 0.33353(13) 0.62161(12) 0.63975(11) 0.0288(4) Uani 1 1 d . . . N4B N 0.40959(14) 0.46551(13) 0.66289(13) 0.0329(5) Uani 1 1 d . . . N5B N 0.35692(13) 0.46003(11) 0.49434(12) 0.0274(4) Uani 1 1 d . . . N6B N 0.32927(14) 0.39028(13) 0.32193(12) 0.0356(5) Uani 1 1 d . . . N7B N 0.27996(13) 0.56474(12) 0.36468(11) 0.0282(4) Uani 1 1 d . . . N8B N 0.21829(14) 0.72558(13) 0.34242(13) 0.0342(5) Uani 1 1 d . . . C1B C 0.22789(17) 0.77029(16) 0.43518(16) 0.0316(5) Uani 1 1 d . . . C2B C 0.20162(17) 0.87451(16) 0.46958(16) 0.0344(6) Uani 1 1 d . . . C3B C 0.17062(19) 0.94947(18) 0.42225(17) 0.0519(7) Uani 1 1 d . . . H3B H 0.1620 0.9367 0.3557 0.062 Uiso 1 1 calc R . . C4B C 0.1532(2) 1.0431(2) 0.4777(2) 0.0692(8) Uani 1 1 d . . . H4B H 0.1339 1.0952 0.4482 0.083 Uiso 1 1 calc R . . C5B C 0.1637(2) 1.06153(18) 0.5767(2) 0.0636(8) Uani 1 1 d . . . H5B H 0.1506 1.1256 0.6121 0.076 Uiso 1 1 calc R . . C6B C 0.19318(18) 0.98664(17) 0.62416(16) 0.0505(7) Uani 1 1 d . . . H6B H 0.1991 0.9989 0.6905 0.061 Uiso 1 1 calc R . . C7B C 0.21353(17) 0.89279(16) 0.56891(16) 0.0343(6) Uani 1 1 d . . . C8B C 0.24956(17) 0.79999(16) 0.59279(17) 0.0323(6) Uani 1 1 d . . . C9B C 0.31157(17) 0.70869(17) 0.70320(16) 0.0318(6) Uani 1 1 d . . . C10B C 0.34108(17) 0.69963(16) 0.80116(16) 0.0328(6) Uani 1 1 d . . . C11B C 0.33169(18) 0.76381(16) 0.88907(16) 0.0424(6) Uani 1 1 d . . . H11B H 0.3006 0.8259 0.8929 0.051 Uiso 1 1 calc R . . C12B C 0.3703(2) 0.73185(19) 0.97054(16) 0.0548(7) Uani 1 1 d . . . H12B H 0.3641 0.7727 1.0305 0.066 Uiso 1 1 calc R . . C13B C 0.4189(2) 0.63846(19) 0.96460(17) 0.0534(7) Uani 1 1 d . . . H13B H 0.4451 0.6189 1.0206 0.064 Uiso 1 1 calc R . . C14B C 0.42806(18) 0.57637(17) 0.87749(17) 0.0453(6) Uani 1 1 d . . . H14B H 0.4609 0.5150 0.8733 0.054 Uiso 1 1 calc R . . C15B C 0.38701(18) 0.60733(16) 0.79578(16) 0.0333(6) Uani 1 1 d . . . C16B C 0.37967(17) 0.55938(17) 0.69407(15) 0.0303(5) Uani 1 1 d . . . C17B C 0.39821(17) 0.42091(15) 0.57024(16) 0.0287(5) Uani 1 1 d . . . C18B C 0.42874(17) 0.31754(16) 0.53495(16) 0.0303(5) Uani 1 1 d . . . C19B C 0.47243(17) 0.24684(17) 0.58282(16) 0.0396(6) Uani 1 1 d . . . H19B H 0.4891 0.2620 0.6496 0.048 Uiso 1 1 calc R . . C20B C 0.48979(19) 0.15318(17) 0.52654(19) 0.0482(7) Uani 1 1 d . . . H20B H 0.5182 0.1037 0.5560 0.058 Uiso 1 1 calc R . . C21B C 0.46583(19) 0.13093(16) 0.42663(18) 0.0494(7) Uani 1 1 d . . . H21B H 0.4793 0.0672 0.3910 0.059 Uiso 1 1 calc R . . C22B C 0.42247(18) 0.20124(16) 0.37911(16) 0.0440(6) Uani 1 1 d . . . H22B H 0.4062 0.1861 0.3123 0.053 Uiso 1 1 calc R . . C23B C 0.40419(17) 0.29555(16) 0.43556(16) 0.0336(6) Uani 1 1 d . . . C24B C 0.35987(17) 0.38541(16) 0.41171(16) 0.0302(6) Uani 1 1 d . . . C25B C 0.29171(17) 0.47442(17) 0.30138(15) 0.0313(6) Uani 1 1 d . . . C26B C 0.25764(17) 0.48156(16) 0.20305(16) 0.0328(6) Uani 1 1 d . . . C27B C 0.24938(19) 0.41178(17) 0.11491(17) 0.0469(6) Uani 1 1 d . . . H27B H 0.2724 0.3464 0.1105 0.056 Uiso 1 1 calc R . . C28B C 0.2061(2) 0.44205(19) 0.03423(16) 0.0554(7) Uani 1 1 d . . . H28B H 0.1987 0.3961 -0.0258 0.067 Uiso 1 1 calc R . . C29B C 0.1727(2) 0.54086(19) 0.04060(17) 0.0564(7) Uani 1 1 d . . . H29B H 0.1436 0.5597 -0.0152 0.068 Uiso 1 1 calc R . . C30B C 0.18246(19) 0.61003(17) 0.12797(16) 0.0460(6) Uani 1 1 d . . . H30B H 0.1613 0.6760 0.1324 0.055 Uiso 1 1 calc R . . C31B C 0.22478(17) 0.57914(16) 0.20968(15) 0.0332(6) Uani 1 1 d . . . C32B C 0.24146(17) 0.62971(16) 0.31096(15) 0.0306(5) Uani 1 1 d . . . N9B N 0.11721(14) 0.53323(12) 0.49820(11) 0.0314(4) Uani 1 1 d . . . C33B C 0.0275(2) 0.56644(17) 0.45097(16) 0.0487(7) Uani 1 1 d . . . H33B H 0.0429 0.6135 0.4151 0.058 Uiso 1 1 calc R . . C34B C 0.0879(2) 0.46676(17) 0.54649(16) 0.0471(7) Uani 1 1 d . . . H34B H 0.1474 0.4408 0.5805 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0307(3) 0.0380(3) 0.0443(3) 0.0217(2) 0.0071(2) 0.0061(2) N1 0.0293(12) 0.0332(11) 0.0366(11) 0.0154(9) 0.0063(9) 0.0048(9) N2 0.0328(12) 0.0340(11) 0.0335(11) 0.0144(9) 0.0056(10) 0.0043(10) N3 0.0274(12) 0.0348(11) 0.0374(11) 0.0193(9) 0.0051(9) 0.0049(9) N4 0.0292(12) 0.0379(11) 0.0467(12) 0.0181(10) 0.0060(10) 0.0053(9) C1 0.0333(16) 0.0294(13) 0.0383(14) 0.0142(11) 0.0107(12) 0.0075(12) C2 0.0304(15) 0.0280(13) 0.0353(14) 0.0098(11) 0.0105(12) 0.0028(11) C3 0.0369(15) 0.0349(14) 0.0468(15) 0.0116(12) 0.0125(12) 0.0057(12) C4 0.0492(18) 0.0405(15) 0.0443(15) 0.0132(13) 0.0174(13) -0.0032(13) C5 0.0590(18) 0.0368(16) 0.0452(16) 0.0199(13) 0.0147(15) 0.0018(14) C6 0.0445(16) 0.0417(14) 0.0356(15) 0.0161(12) 0.0054(12) 0.0073(12) C7 0.0349(15) 0.0274(12) 0.0304(13) 0.0085(11) 0.0116(11) 0.0051(11) C8 0.0321(15) 0.0331(13) 0.0318(14) 0.0140(11) 0.0057(12) 0.0064(12) C9 0.0333(15) 0.0295(13) 0.0317(13) 0.0100(11) 0.0060(11) 0.0057(11) C10 0.0290(15) 0.0296(13) 0.0282(13) 0.0078(11) 0.0038(11) 0.0057(11) C11 0.0399(16) 0.0370(14) 0.0324(14) 0.0086(12) 0.0080(12) 0.0102(12) C12 0.0382(17) 0.0511(16) 0.0377(15) 0.0104(13) 0.0008(13) 0.0159(13) C13 0.0304(15) 0.0573(16) 0.0483(15) 0.0180(14) 0.0021(12) 0.0085(13) C14 0.0359(16) 0.0506(16) 0.0477(16) 0.0212(13) 0.0082(13) 0.0020(13) C15 0.0270(15) 0.0333(14) 0.0365(14) 0.0097(12) 0.0038(12) 0.0068(11) C16 0.0319(15) 0.0301(13) 0.0361(14) 0.0134(12) 0.0053(12) 0.0047(11) N5 0.0483(13) 0.0505(14) 0.0498(15) 0.0102(12) 0.0151(11) 0.0122(11) C17 0.0780(17) 0.0620(18) 0.0680(18) 0.0222(19) 0.0121(17) 0.0214(17) C18 0.0760(18) 0.0620(18) 0.0720(19) 0.005(2) 0.009(2) 0.0201(17) N6 0.0745(19) 0.0710(18) 0.0750(17) 0.0071(17) 0.0149(16) 0.0124(15) C19 0.0700(23) 0.0720(23) 0.0510(18) 0.0090(19) 0.014(2) 0.030(3) C20 0.0760(23) 0.0620(22) 0.0610(18) 0.0098(19) 0.011(2) 0.017(2) Co1B 0.0316(2) 0.02881(18) 0.02931(18) 0.00773(14) 0.00632(15) 0.00485(15) N1B 0.0319(11) 0.0298(11) 0.0288(11) 0.0083(10) 0.0070(9) 0.0061(9) N2B 0.0380(12) 0.0325(12) 0.0346(12) 0.0051(10) 0.0059(10) 0.0080(9) N3B 0.0296(11) 0.0277(11) 0.0280(11) 0.0045(9) 0.0049(9) 0.0053(9) N4B 0.0336(12) 0.0308(12) 0.0338(12) 0.0076(10) 0.0056(10) 0.0040(9) N5B 0.0300(11) 0.0246(10) 0.0282(11) 0.0074(9) 0.0053(9) 0.0034(8) N6B 0.0399(12) 0.0322(12) 0.0343(12) 0.0052(10) 0.0080(10) 0.0077(9) N7B 0.0336(12) 0.0265(11) 0.0251(11) 0.0069(9) 0.0055(9) 0.0052(9) N8B 0.0381(12) 0.0309(12) 0.0352(12) 0.0096(10) 0.0082(10) 0.0065(9) C1B 0.0338(14) 0.0284(14) 0.0317(15) 0.0070(13) 0.0039(12) 0.0040(11) C2B 0.0347(15) 0.0288(14) 0.0394(16) 0.0076(12) 0.0042(12) 0.0083(11) C3B 0.0690(19) 0.0395(16) 0.0458(17) 0.0083(14) 0.0032(14) 0.0177(14) C4B 0.0800(18) 0.0586(18) 0.0700(17) 0.0138(17) 0.0036(18) 0.0355(16) C5B 0.0740(18) 0.0544(17) 0.0560(18) 0.0007(16) 0.0002(16) 0.0307(15) C6B 0.0621(18) 0.0433(16) 0.0398(16) 0.0002(14) 0.0020(13) 0.0207(14) C7B 0.0365(15) 0.0313(14) 0.0337(15) 0.0053(13) 0.0034(12) 0.0100(11) C8B 0.0315(15) 0.0329(14) 0.0315(15) 0.0045(13) 0.0065(12) 0.0067(11) C9B 0.0313(14) 0.0314(14) 0.0311(15) 0.0066(13) 0.0048(11) 0.0006(11) C10B 0.0368(15) 0.0321(15) 0.0261(15) 0.0026(12) 0.0051(12) 0.0005(11) C11B 0.0523(17) 0.0388(15) 0.0328(15) 0.0013(13) 0.0091(13) 0.0052(12) C12B 0.0670(17) 0.0526(18) 0.0370(16) 0.0015(14) 0.0095(14) -0.0024(15) C13B 0.0720(18) 0.0484(18) 0.0378(16) 0.0104(14) 0.0052(14) 0.0022(15) C14B 0.0521(17) 0.0395(16) 0.0401(17) 0.0074(14) -0.0001(14) 0.0028(13) C15B 0.0345(15) 0.0346(15) 0.0280(15) 0.0049(12) 0.0037(12) 0.0001(11) C16B 0.0270(14) 0.0297(14) 0.0316(15) 0.0053(13) 0.0024(11) 0.0007(11) C17B 0.0273(13) 0.0309(14) 0.0274(14) 0.0057(12) 0.0064(11) 0.0029(10) C18B 0.0320(14) 0.0266(13) 0.0349(15) 0.0095(12) 0.0103(11) 0.0057(11) C19B 0.0406(16) 0.0360(15) 0.0458(16) 0.0130(13) 0.0111(12) 0.0108(12) C20B 0.0589(18) 0.0332(15) 0.0613(19) 0.0212(14) 0.0170(15) 0.0168(13) C21B 0.0701(19) 0.0308(15) 0.0520(18) 0.0112(14) 0.0181(15) 0.0172(13) C22B 0.0565(17) 0.0335(15) 0.0402(15) 0.0023(13) 0.0128(13) 0.0082(12) C23B 0.0335(14) 0.0279(14) 0.0389(15) 0.0059(13) 0.0084(12) 0.0043(11) C24B 0.0319(15) 0.0269(14) 0.0313(15) 0.0052(13) 0.0075(12) 0.0029(11) C25B 0.0327(15) 0.0342(15) 0.0289(15) 0.0088(13) 0.0093(11) 0.0050(11) C26B 0.0400(15) 0.0318(15) 0.0261(14) 0.0048(12) 0.0076(12) 0.0062(12) C27B 0.0679(18) 0.0371(15) 0.0382(16) 0.0096(14) 0.0121(14) 0.0154(13) C28B 0.0730(18) 0.0526(18) 0.0366(15) 0.0038(14) 0.0111(14) 0.0142(15) C29B 0.0740(18) 0.0547(19) 0.0401(16) 0.0087(15) 0.0064(14) 0.0186(16) C30B 0.0653(18) 0.0411(16) 0.0365(16) 0.0140(14) 0.0121(14) 0.0151(13) C31B 0.0410(15) 0.0326(14) 0.0273(14) 0.0073(12) 0.0098(12) 0.0049(11) C32B 0.0338(14) 0.0298(14) 0.0286(14) 0.0077(12) 0.0068(11) 0.0035(11) N9B 0.0315(12) 0.0345(11) 0.0306(11) 0.0137(9) 0.0045(9) 0.0031(9) C33B 0.0389(17) 0.0608(17) 0.0605(18) 0.0442(15) 0.0095(14) 0.0016(14) C34B 0.0349(16) 0.0564(17) 0.0600(18) 0.0379(15) 0.0027(13) 0.0075(13) _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 Co1 N3 1.9152(16) 2 y Co1 N3 1.9152(16) . y Co1 N1 1.9202(16) . y Co1 N1 1.9203(16) 2 y Co1 N5 2.411(2) 2 y Co1 N5 2.411(2) . y N1 C8 1.374(2) . ? N1 C1 1.379(2) . ? N2 C8 1.321(2) . ? N2 C9 1.324(2) . ? N3 C9 1.374(2) . ? N3 C16 1.379(2) . ? N4 C1 1.313(2) 2 ? N4 C16 1.324(2) . ? C1 N4 1.313(2) 2 ? C1 C2 1.453(2) . ? C2 C3 1.388(2) . ? C2 C7 1.390(2) . ? C3 C4 1.385(2) . ? C3 H3 0.9300 . ? C4 C5 1.390(3) . ? C4 H4 0.9300 . ? C5 C6 1.386(3) . ? C5 H5 0.9300 . ? C6 C7 1.390(2) . ? C6 H6 0.9300 . ? C7 C8 1.447(2) . ? C9 C10 1.447(2) . ? C10 C15 1.388(2) . ? C10 C11 1.397(2) . ? C11 C12 1.384(2) . ? C11 H11 0.9300 . ? C12 C13 1.388(3) . ? C12 H12 0.9300 . ? C13 C14 1.381(2) . ? C13 H13 0.9300 . ? C14 C15 1.382(2) . ? C14 H14 0.9300 . ? C15 C16 1.438(3) . ? N5 C20 1.306(3) . ? N5 C17 1.332(3) . ? C17 C18 1.380(3) . ? C17 H17 0.9300 . ? C18 N6 1.309(3) . ? C18 H18 0.9300 . ? N6 C19 1.321(3) . ? C19 C20 1.372(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? Co1B N1B 1.9155(16) . y Co1B N7B 1.9176(16) . y Co1B N3B 1.9189(16) . y Co1B N5B 1.9206(16) . y Co1B N9B 2.1778(17) . y N1B C1B 1.364(2) . ? N1B C8B 1.376(2) . ? N2B C8B 1.320(2) . ? N2B C9B 1.329(2) . ? N3B C16B 1.368(2) . ? N3B C9B 1.376(2) . ? N4B C17B 1.320(2) . ? N4B C16B 1.330(2) . ? N5B C17B 1.372(2) . ? N5B C24B 1.378(2) . ? N6B C24B 1.319(2) . ? N6B C25B 1.328(2) . ? N7B C32B 1.362(2) . ? N7B C25B 1.370(2) . ? N8B C1B 1.324(2) . ? N8B C32B 1.326(2) . ? C1B C2B 1.446(3) . ? C2B C7B 1.389(3) . ? C2B C3B 1.390(3) . ? C3B C4B 1.373(3) . ? C3B H3B 0.9300 . ? C4B C5B 1.385(3) . ? C4B H4B 0.9300 . ? C5B C6B 1.387(3) . ? C5B H5B 0.9300 . ? C6B C7B 1.385(3) . ? C6B H6B 0.9300 . ? C7B C8B 1.449(3) . ? C9B C10B 1.450(3) . ? C10B C15B 1.381(2) . ? C10B C11B 1.387(3) . ? C11B C12B 1.380(3) . ? C11B H11B 0.9300 . ? C12B C13B 1.409(3) . ? C12B H12B 0.9300 . ? C13B C14B 1.366(3) . ? C13B H13B 0.9300 . ? C14B C15B 1.382(3) . ? C14B H14B 0.9300 . ? C15B C16B 1.453(3) . ? C17B C18B 1.456(2) . ? C18B C23B 1.385(3) . ? C18B C19B 1.391(2) . ? C19B C20B 1.378(3) . ? C19B H19B 0.9300 . ? C20B C21B 1.392(3) . ? C20B H20B 0.9300 . ? C21B C22B 1.382(2) . ? C21B H21B 0.9300 . ? C22B C23B 1.389(3) . ? C22B H22B 0.9300 . ? C23B C24B 1.447(3) . ? C25B C26B 1.453(3) . ? C26B C31B 1.382(2) . ? C26B C27B 1.382(3) . ? C27B C28B 1.371(3) . ? C27B H27B 0.9300 . ? C28B C29B 1.401(3) . ? C28B H28B 0.9300 . ? C29B C30B 1.368(3) . ? C29B H29B 0.9300 . ? C30B C31B 1.385(3) . ? C30B H30B 0.9300 . ? C31B C32B 1.445(3) . ? N9B C34B 1.310(2) . ? N9B C33B 1.329(2) . ? C33B C34B 1.383(3) 2_566 ? C33B H33B 0.9300 . ? C34B C33B 1.383(3) 2_566 ? C34B H34B 0.9300 . ? 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 N3 Co1 N3 180.00(11) 2 . y N3 Co1 N1 90.27(7) 2 . y N3 Co1 N1 89.73(7) . . y N3 Co1 N1 89.73(7) 2 2 y N3 Co1 N1 90.27(7) . 2 y N1 Co1 N1 180.00(11) . 2 y N3 Co1 N5 88.21(7) 2 2 y N3 Co1 N5 91.79(7) . 2 y N1 Co1 N5 89.20(7) . 2 y N1 Co1 N5 90.80(7) 2 2 y N3 Co1 N5 91.79(7) 2 . y N3 Co1 N5 88.21(7) . . y N1 Co1 N5 90.80(7) . . y N1 Co1 N5 89.20(7) 2 . y N5 Co1 N5 180.00(13) 2 . y C8 N1 C1 106.91(16) . . ? C8 N1 Co1 126.75(14) . . ? C1 N1 Co1 126.30(13) . . ? C8 N2 C9 121.56(18) . . ? C9 N3 C16 106.77(16) . . ? C9 N3 Co1 126.90(14) . . ? C16 N3 Co1 126.31(13) . . ? C1 N4 C16 122.11(18) 2 . ? N4 C1 N1 127.56(19) 2 . ? N4 C1 C2 122.6(2) 2 . ? N1 C1 C2 109.86(18) . . ? C3 C2 C7 121.41(19) . . ? C3 C2 C1 132.1(2) . . ? C7 C2 C1 106.46(19) . . ? C4 C3 C2 117.3(2) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C3 C4 C5 121.2(2) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 121.6(2) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 117.1(2) . . ? C5 C6 H6 121.4 . . ? C7 C6 H6 121.4 . . ? C6 C7 C2 121.3(2) . . ? C6 C7 C8 132.3(2) . . ? C2 C7 C8 106.44(18) . . ? N2 C8 N1 127.54(19) . . ? N2 C8 C7 122.15(18) . . ? N1 C8 C7 110.31(18) . . ? N2 C9 N3 127.5(2) . . ? N2 C9 C10 122.36(19) . . ? N3 C9 C10 110.15(18) . . ? C15 C10 C11 121.6(2) . . ? C15 C10 C9 106.19(18) . . ? C11 C10 C9 132.2(2) . . ? C12 C11 C10 116.7(2) . . ? C12 C11 H11 121.6 . . ? C10 C11 H11 121.6 . . ? C11 C12 C13 121.3(2) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C14 C13 C12 121.8(2) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 117.4(2) . . ? C13 C14 H14 121.3 . . ? C15 C14 H14 121.3 . . ? C14 C15 C10 121.1(2) . . ? C14 C15 C16 131.9(2) . . ? C10 C15 C16 106.94(19) . . ? N4 C16 N3 127.43(19) . . ? N4 C16 C15 122.62(19) . . ? N3 C16 C15 109.94(18) . . ? C20 N5 C17 115.0(2) . . ? C20 N5 Co1 122.51(18) . . ? C17 N5 Co1 122.46(18) . . ? N5 C17 C18 121.8(3) . . ? N5 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? N6 C18 C17 123.0(3) . . ? N6 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? C18 N6 C19 114.7(3) . . ? N6 C19 C20 122.7(3) . . ? N6 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? N5 C20 C19 122.8(3) . . ? N5 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? N1B Co1B N7B 90.38(8) . . ? N1B Co1B N3B 89.76(8) . . ? N7B Co1B N3B 174.91(7) . . ? N1B Co1B N5B 174.19(7) . . ? N7B Co1B N5B 89.46(7) . . ? N3B Co1B N5B 89.88(8) . . ? N1B Co1B N9B 90.62(7) . . ? N7B Co1B N9B 92.72(7) . . ? N3B Co1B N9B 92.36(7) . . ? N5B Co1B N9B 95.18(7) . . ? C1B N1B C8B 106.90(17) . . ? C1B N1B Co1B 126.45(15) . . ? C8B N1B Co1B 126.61(14) . . ? C8B N2B C9B 121.43(19) . . ? C16B N3B C9B 106.59(17) . . ? C16B N3B Co1B 126.81(14) . . ? C9B N3B Co1B 126.54(14) . . ? C17B N4B C16B 121.56(18) . . ? C17B N5B C24B 106.82(17) . . ? C17B N5B Co1B 126.52(14) . . ? C24B N5B Co1B 126.60(14) . . ? C24B N6B C25B 121.24(18) . . ? C32B N7B C25B 106.75(17) . . ? C32B N7B Co1B 126.14(14) . . ? C25B N7B Co1B 126.88(14) . . ? C1B N8B C32B 122.11(18) . . ? N8B C1B N1B 127.25(19) . . ? N8B C1B C2B 122.18(19) . . ? N1B C1B C2B 110.53(19) . . ? C7B C2B C3B 121.6(2) . . ? C7B C2B C1B 106.23(19) . . ? C3B C2B C1B 132.2(2) . . ? C4B C3B C2B 117.3(2) . . ? C4B C3B H3B 121.3 . . ? C2B C3B H3B 121.3 . . ? C3B C4B C5B 121.4(2) . . ? C3B C4B H4B 119.3 . . ? C5B C4B H4B 119.3 . . ? C4B C5B C6B 121.5(2) . . ? C4B C5B H5B 119.3 . . ? C6B C5B H5B 119.3 . . ? C7B C6B C5B 117.4(2) . . ? C7B C6B H6B 121.3 . . ? C5B C6B H6B 121.3 . . ? C6B C7B C2B 120.7(2) . . ? C6B C7B C8B 132.9(2) . . ? C2B C7B C8B 106.35(19) . . ? N2B C8B N1B 127.66(19) . . ? N2B C8B C7B 122.4(2) . . ? N1B C8B C7B 109.94(19) . . ? N2B C9B N3B 127.3(2) . . ? N2B C9B C10B 122.6(2) . . ? N3B C9B C10B 110.10(19) . . ? C15B C10B C11B 121.1(2) . . ? C15B C10B C9B 106.6(2) . . ? C11B C10B C9B 132.3(2) . . ? C12B C11B C10B 117.3(2) . . ? C12B C11B H11B 121.3 . . ? C10B C11B H11B 121.3 . . ? C11B C12B C13B 121.2(2) . . ? C11B C12B H12B 119.4 . . ? C13B C12B H12B 119.4 . . ? C14B C13B C12B 120.7(2) . . ? C14B C13B H13B 119.7 . . ? C12B C13B H13B 119.7 . . ? C13B C14B C15B 118.1(2) . . ? C13B C14B H14B 121.0 . . ? C15B C14B H14B 121.0 . . ? C10B C15B C14B 121.5(2) . . ? C10B C15B C16B 106.2(2) . . ? C14B C15B C16B 132.3(2) . . ? N4B C16B N3B 127.4(2) . . ? N4B C16B C15B 122.00(19) . . ? N3B C16B C15B 110.48(18) . . ? N4B C17B N5B 127.75(19) . . ? N4B C17B C18B 122.24(19) . . ? N5B C17B C18B 110.01(18) . . ? C23B C18B C19B 121.9(2) . . ? C23B C18B C17B 106.42(18) . . ? C19B C18B C17B 131.7(2) . . ? C20B C19B C18B 116.8(2) . . ? C20B C19B H19B 121.6 . . ? C18B C19B H19B 121.6 . . ? C19B C20B C21B 121.5(2) . . ? C19B C20B H20B 119.2 . . ? C21B C20B H20B 119.2 . . ? C22B C21B C20B 121.6(2) . . ? C22B C21B H21B 119.2 . . ? C20B C21B H21B 119.2 . . ? C21B C22B C23B 117.0(2) . . ? C21B C22B H22B 121.5 . . ? C23B C22B H22B 121.5 . . ? C18B C23B C22B 121.1(2) . . ? C18B C23B C24B 106.53(19) . . ? C22B C23B C24B 132.3(2) . . ? N6B C24B N5B 127.72(19) . . ? N6B C24B C23B 122.1(2) . . ? N5B C24B C23B 110.21(19) . . ? N6B C25B N7B 127.55(19) . . ? N6B C25B C26B 122.2(2) . . ? N7B C25B C26B 110.24(18) . . ? C31B C26B C27B 121.2(2) . . ? C31B C26B C25B 105.9(2) . . ? C27B C26B C25B 132.8(2) . . ? C28B C27B C26B 117.8(2) . . ? C28B C27B H27B 121.1 . . ? C26B C27B H27B 121.1 . . ? C27B C28B C29B 121.2(2) . . ? C27B C28B H28B 119.4 . . ? C29B C28B H28B 119.4 . . ? C30B C29B C28B 120.7(2) . . ? C30B C29B H29B 119.6 . . ? C28B C29B H29B 119.6 . . ? C29B C30B C31B 118.2(2) . . ? C29B C30B H30B 120.9 . . ? C31B C30B H30B 120.9 . . ? C26B C31B C30B 120.9(2) . . ? C26B C31B C32B 106.54(19) . . ? C30B C31B C32B 132.5(2) . . ? N8B C32B N7B 127.48(19) . . ? N8B C32B C31B 121.99(19) . . ? N7B C32B C31B 110.51(18) . . ? C34B N9B C33B 115.10(17) . . ? C34B N9B Co1B 122.16(15) . . ? C33B N9B Co1B 122.65(15) . . ? N9B C33B C34B 122.04(19) . 2_566 ? N9B C33B H33B 119.0 . . ? C34B C33B H33B 119.0 2_566 . ? N9B C34B C33B 122.86(19) . 2_566 ? N9B C34B H34B 118.6 . . ? C33B C34B H34B 118.6 2_566 . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.535 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.047 # Attachment 'Fe_Comp_I.cif' data_Fe_Comp_I _database_code_depnum_ccdc_archive 'CCDC 767379' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H24 Fe N12' _chemical_formula_sum 'C40 H24 Fe N12' _chemical_formula_weight 728.56 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' 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/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5301(19) _cell_length_b 19.6721(37) _cell_length_c 9.1369(18) _cell_angle_alpha 90.00 _cell_angle_beta 111.26(1) _cell_angle_gamma 90.00 _cell_volume 1596.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1625 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.73 _exptl_crystal_description paralellepiped _exptl_crystal_colour violet _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 1.51 _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method floatation _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.526 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8713 _exptl_absorpt_correction_T_max 0.9127 _exptl_absorpt_process_details ; Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'KUMA KM-4 with area CCD detector' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17887 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.73 _reflns_number_total 3533 _reflns_number_gt 2086 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Oxford Diffraction Poland (2006). CrysAlis CCD, Version 171.32.6 ; _computing_cell_refinement ; Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6 ; _computing_data_reduction ; Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular Structure Visualisation, University of Bonn, Germany ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^] 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 3533 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Fe1 Fe 0.5000 0.5000 0.5000 0.02685(12) Uani 1 2 d S . . N1 N 0.44851(16) 0.55818(7) 0.64335(16) 0.0267(4) Uani 1 1 d . . . N2 N 0.23044(17) 0.61613(7) 0.46211(18) 0.0297(4) Uani 1 1 d . . . N3 N 0.33265(16) 0.53587(7) 0.32552(16) 0.0270(4) Uani 1 1 d . . . N4 N 0.35854(18) 0.47308(8) 0.10856(17) 0.0320(4) Uani 1 1 d . . . C1 C 0.5239(2) 0.56268(9) 0.8034(2) 0.0286(4) Uani 1 1 d . . . C2 C 0.4544(2) 0.61481(9) 0.8672(2) 0.0308(5) Uani 1 1 d . . . C3 C 0.4892(2) 0.64005(10) 1.0186(2) 0.0418(5) Uani 1 1 d . . . H3 H 0.5698 0.6230 1.1027 0.050 Uiso 1 1 calc R . . C4 C 0.3996(3) 0.69121(10) 1.0390(3) 0.0469(6) Uani 1 1 d . . . H4 H 0.4201 0.7088 1.1390 0.056 Uiso 1 1 calc R . . C5 C 0.2788(2) 0.71735(10) 0.9139(2) 0.0436(6) Uani 1 1 d . . . H5 H 0.2210 0.7522 0.9318 0.052 Uiso 1 1 calc R . . C6 C 0.2441(2) 0.69233(9) 0.7642(2) 0.0361(5) Uani 1 1 d . . . H6 H 0.1635 0.7095 0.6803 0.043 Uiso 1 1 calc R . . C7 C 0.3338(2) 0.64057(9) 0.7429(2) 0.0297(5) Uani 1 1 d . . . C8 C 0.3313(2) 0.60399(9) 0.6037(2) 0.0274(4) Uani 1 1 d . . . C9 C 0.23295(19) 0.58504(9) 0.3334(2) 0.0273(4) Uani 1 1 d . . . C10 C 0.1264(2) 0.60057(9) 0.1772(2) 0.0295(5) Uani 1 1 d . . . C11 C 0.0076(2) 0.64587(10) 0.1224(2) 0.0389(5) Uani 1 1 d . . . H11 H -0.0181 0.6739 0.1908 0.047 Uiso 1 1 calc R . . C12 C -0.0710(2) 0.64796(11) -0.0369(3) 0.0469(6) Uani 1 1 d . . . H12 H -0.1514 0.6779 -0.0768 0.056 Uiso 1 1 calc R . . C13 C -0.0329(2) 0.60633(11) -0.1390(2) 0.0460(6) Uani 1 1 d . . . H13 H -0.0884 0.6089 -0.2461 0.055 Uiso 1 1 calc R . . C14 C 0.0849(2) 0.56137(10) -0.0854(2) 0.0385(5) Uani 1 1 d . . . H14 H 0.1100 0.5334 -0.1543 0.046 Uiso 1 1 calc R . . C15 C 0.1648(2) 0.55903(9) 0.0742(2) 0.0300(5) Uani 1 1 d . . . C16 C 0.2940(2) 0.51913(9) 0.1698(2) 0.0285(5) Uani 1 1 d . . . N5 N 0.36760(17) 0.42625(7) 0.53246(16) 0.0280(4) Uani 1 1 d . . . C17 C 0.2370(2) 0.43916(10) 0.5515(2) 0.0362(5) Uani 1 1 d . . . H17 H 0.2058 0.4841 0.5495 0.043 Uiso 1 1 calc R . . C18 C 0.1479(2) 0.38841(11) 0.5740(2) 0.0469(6) Uani 1 1 d . . . H18 H 0.0592 0.4006 0.5877 0.056 Uiso 1 1 calc R . . N6 N 0.1818(2) 0.32308(9) 0.5773(2) 0.0555(5) Uani 1 1 d . . . C19 C 0.3106(3) 0.31084(11) 0.5581(2) 0.0537(6) Uani 1 1 d . . . H19 H 0.3405 0.2658 0.5591 0.064 Uiso 1 1 calc R . . C20 C 0.4028(2) 0.36044(10) 0.5367(2) 0.0381(5) Uani 1 1 d . . . H20 H 0.4921 0.3478 0.5248 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0269(2) 0.0256(2) 0.0302(2) -0.0002(2) 0.01294(18) 0.0009(2) N1 0.0294(10) 0.0237(9) 0.0300(10) 0.0011(7) 0.0142(8) 0.0010(7) N2 0.0305(10) 0.0277(9) 0.0340(10) 0.0012(8) 0.0155(8) 0.0020(7) N3 0.0276(9) 0.0262(9) 0.0291(10) -0.0004(7) 0.0126(8) -0.0007(7) N4 0.0328(10) 0.0322(9) 0.0327(10) 0.0004(8) 0.0138(8) 0.0031(8) C1 0.0327(12) 0.0272(11) 0.0299(11) -0.0015(9) 0.0160(10) -0.0015(9) C2 0.0384(13) 0.0273(11) 0.0325(12) -0.0018(10) 0.0199(11) 0.0009(9) C3 0.0499(14) 0.0395(12) 0.0363(14) -0.0015(11) 0.0159(11) 0.0050(12) C4 0.0652(17) 0.0399(13) 0.0417(14) -0.0120(11) 0.0267(13) 0.0017(12) C5 0.0596(16) 0.0300(12) 0.0513(15) -0.0029(11) 0.0322(13) 0.0071(11) C6 0.0455(14) 0.0285(11) 0.0395(13) 0.0034(10) 0.0217(11) 0.0057(10) C7 0.0368(13) 0.0256(11) 0.0338(12) -0.0010(9) 0.0214(11) -0.0007(9) C8 0.0295(12) 0.0241(11) 0.0332(12) 0.0019(9) 0.0167(10) -0.0006(9) C9 0.0267(12) 0.0233(10) 0.0346(12) -0.0001(9) 0.0144(10) -0.0007(9) C10 0.0290(12) 0.0263(11) 0.0335(12) 0.0026(9) 0.0117(10) -0.0008(9) C11 0.0356(13) 0.0370(12) 0.0442(14) 0.0026(10) 0.0145(11) 0.0055(10) C12 0.0395(14) 0.0447(14) 0.0492(15) 0.0094(11) 0.0074(12) 0.0128(11) C13 0.0447(15) 0.0484(14) 0.0355(13) 0.0056(11) 0.0033(11) 0.0036(12) C14 0.0411(14) 0.0389(13) 0.0345(13) -0.0011(10) 0.0126(11) -0.0027(10) C15 0.0273(12) 0.0287(11) 0.0338(12) 0.0041(10) 0.0110(10) -0.0011(9) C16 0.0290(12) 0.0282(12) 0.0295(11) 0.0007(9) 0.0121(10) -0.0026(9) N5 0.0281(10) 0.0296(9) 0.0284(9) -0.0006(7) 0.0126(8) 0.0020(7) C17 0.0352(13) 0.0356(12) 0.0417(12) -0.0024(10) 0.0188(10) -0.0001(10) C18 0.0385(14) 0.0516(15) 0.0608(15) 0.0022(12) 0.0304(12) -0.0055(11) N6 0.0529(14) 0.0417(12) 0.0838(15) 0.0034(11) 0.0389(12) -0.0082(10) C19 0.0609(17) 0.0323(13) 0.0785(18) 0.0024(12) 0.0378(15) -0.0052(12) C20 0.0401(13) 0.0306(12) 0.0495(14) -0.0008(10) 0.0234(11) 0.0002(10) _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 Fe1 N1 1.9318(14) . y Fe1 N1 1.9318(14) 3_666 y Fe1 N3 1.9337(16) 3_666 y Fe1 N3 1.9337(16) . y Fe1 N5 2.0141(15) 3_666 y Fe1 N5 2.0141(15) . y N1 C8 1.377(2) . ? N1 C1 1.379(2) . ? N2 C8 1.324(2) . ? N2 C9 1.334(2) . ? N3 C16 1.374(2) . ? N3 C9 1.376(2) . ? N4 C1 1.320(2) 3_666 ? N4 C16 1.327(2) . ? C1 N4 1.320(2) 3_666 ? C1 C2 1.453(2) . ? C2 C7 1.386(2) . ? C2 C3 1.392(2) . ? C3 C4 1.375(3) . ? C3 H3 0.9300 . ? C4 C5 1.393(3) . ? C4 H4 0.9300 . ? C5 C6 1.376(2) . ? C5 H5 0.9300 . ? C6 C7 1.387(2) . ? C6 H6 0.9300 . ? C7 C8 1.454(2) . ? C9 C10 1.452(2) . ? C10 C11 1.384(2) . ? C10 C15 1.392(2) . ? C11 C12 1.375(3) . ? C11 H11 0.9300 . ? C12 C13 1.385(3) . ? C12 H12 0.9300 . ? C13 C14 1.373(3) . ? C13 H13 0.9300 . ? C14 C15 1.379(2) . ? C14 H14 0.9300 . ? C15 C16 1.454(2) . ? N5 C20 1.334(2) . ? N5 C17 1.342(2) . ? C17 C18 1.374(3) . ? C17 H17 0.9300 . ? C18 N6 1.323(3) . ? C18 H18 0.9300 . ? N6 C19 1.323(3) . ? C19 C20 1.374(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 180.0 . 3_666 y N1 Fe1 N3 89.63(6) . 3_666 y N1 Fe1 N3 90.37(6) 3_666 3_666 y N1 Fe1 N3 90.37(6) . . y N1 Fe1 N3 89.63(6) 3_666 . y N3 Fe1 N3 180.0 3_666 . y N1 Fe1 N5 89.99(6) . 3_666 y N1 Fe1 N5 90.01(6) 3_666 3_666 y N3 Fe1 N5 90.62(6) 3_666 3_666 y N3 Fe1 N5 89.38(6) . 3_666 y N1 Fe1 N5 90.01(6) . . y N1 Fe1 N5 89.99(6) 3_666 . y N3 Fe1 N5 89.38(6) 3_666 . y N3 Fe1 N5 90.62(6) . . y N5 Fe1 N5 180.0 3_666 . y C8 N1 C1 107.35(14) . . ? C8 N1 Fe1 126.18(12) . . ? C1 N1 Fe1 126.46(12) . . ? C8 N2 C9 122.69(16) . . ? C16 N3 C9 106.96(15) . . ? C16 N3 Fe1 126.68(12) . . ? C9 N3 Fe1 126.32(12) . . ? C1 N4 C16 121.82(16) 3_666 . ? N4 C1 N1 127.81(16) 3_666 . ? N4 C1 C2 122.76(17) 3_666 . ? N1 C1 C2 109.43(16) . . ? C7 C2 C3 120.79(18) . . ? C7 C2 C1 107.02(16) . . ? C3 C2 C1 132.19(18) . . ? C4 C3 C2 117.3(2) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C3 C4 C5 121.86(19) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 120.84(19) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 117.61(19) . . ? C5 C6 H6 121.2 . . ? C7 C6 H6 121.2 . . ? C2 C7 C6 121.55(17) . . ? C2 C7 C8 106.33(16) . . ? C6 C7 C8 132.10(18) . . ? N2 C8 N1 127.40(16) . . ? N2 C8 C7 122.74(17) . . ? N1 C8 C7 109.84(16) . . ? N2 C9 N3 127.01(17) . . ? N2 C9 C10 122.71(16) . . ? N3 C9 C10 110.28(15) . . ? C11 C10 C15 120.95(18) . . ? C11 C10 C9 132.81(18) . . ? C15 C10 C9 106.23(16) . . ? C12 C11 C10 117.56(19) . . ? C12 C11 H11 121.2 . . ? C10 C11 H11 121.2 . . ? C11 C12 C13 121.33(19) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C14 C13 C12 121.38(19) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 117.74(19) . . ? C13 C14 H14 121.1 . . ? C15 C14 H14 121.1 . . ? C14 C15 C10 121.03(17) . . ? C14 C15 C16 132.50(18) . . ? C10 C15 C16 106.47(16) . . ? N4 C16 N3 127.51(17) . . ? N4 C16 C15 122.42(16) . . ? N3 C16 C15 110.06(16) . . ? C20 N5 C17 114.53(16) . . ? C20 N5 Fe1 122.61(13) . . ? C17 N5 Fe1 122.87(12) . . ? N5 C17 C18 122.31(18) . . ? N5 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? N6 C18 C17 123.4(2) . . ? N6 C18 H18 118.3 . . ? C17 C18 H18 118.3 . . ? C18 N6 C19 113.86(19) . . ? N6 C19 C20 124.2(2) . . ? N6 C19 H19 117.9 . . ? C20 C19 H19 117.9 . . ? N5 C20 C19 121.75(19) . . ? N5 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.575 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.048