Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'A. L. Balch' 'A.de Bettencourt-Dias' 'Hon Man Lee' 'Marylin Olmstead' 'David Pham' _publ_contact_author_name 'Prof A L Balch' _publ_contact_author_address ; Department of Chemistry University of California Davis CA 95616 USA ; _publ_contact_author_email ALBALCH@UCDAVIS.EDU _publ_section_title ; Interactions of Metalloporphyrins as Donors with the Electron Acceptors: C60, Tetracyanoquinomethane (TCNQ) and Trinitrofluorenylidenemalonitrile ; data_hml66a _database_code_CSD 198536 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common C!60$$.!Pt(OEP)$.!2(C!6$H!6$) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H56 N4 Pt' _chemical_formula_weight 1604.66 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' Pt Pt -1.7033 8.3905 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.1778(19) _cell_length_b 14.4430(14) _cell_length_c 17.1813(17) _cell_angle_alpha 87.679(7) _cell_angle_beta 75.728(6) _cell_angle_gamma 75.512(6) _cell_volume 3300.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8096 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 31.4 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 2.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3531 _exptl_absorpt_correction_T_max 0.5892 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43336 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 31.50 _reflns_number_total 19865 _reflns_number_gt 18705 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT/SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5, XP (Sheldrick, 1994)' _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^)+(0.0308P)^2^+1.4918P] 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 19865 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0537 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.010 _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 Pt1 Pt 0.467536(4) 1.084845(4) 0.388197(3) 0.01028(2) Uani 1 1 d . . . N1 N 0.41679(9) 1.02010(9) 0.31109(7) 0.0125(2) Uani 1 1 d . . . N3 N 0.51899(9) 1.15056(9) 0.46452(7) 0.0108(2) Uani 1 1 d . . . N2 N 0.34647(9) 1.19616(9) 0.40078(7) 0.0121(2) Uani 1 1 d . . . N4 N 0.58962(9) 0.97431(9) 0.37453(7) 0.0117(2) Uani 1 1 d . . . C5 C 0.60315(11) 1.11370(10) 0.49259(8) 0.0120(2) Uani 1 1 d . . . C6 C 0.74047(11) 0.87441(10) 0.38714(9) 0.0137(3) Uani 1 1 d . . . C7 C 0.66430(11) 0.96167(10) 0.41473(9) 0.0120(2) Uani 1 1 d . . . C8 C 0.26442(11) 1.20258(11) 0.36958(9) 0.0136(3) Uani 1 1 d . . . C9 C 0.19371(11) 1.29436(11) 0.39113(9) 0.0144(3) Uani 1 1 d . . . C10 C 0.31773(12) 0.98482(11) 0.23341(9) 0.0159(3) Uani 1 1 d . . . C11 C 0.61588(11) 1.18236(11) 0.54540(8) 0.0127(2) Uani 1 1 d . . . C12 C 0.53944(11) 1.26231(11) 0.54771(9) 0.0134(3) Uani 1 1 d . . . C13 C 0.09228(12) 1.32307(12) 0.37354(10) 0.0176(3) Uani 1 1 d . . . H13A H 0.0975 1.3010 0.3185 0.021 Uiso 1 1 calc R . . H13B H 0.0689 1.3937 0.3756 0.021 Uiso 1 1 calc R . . C14 C 0.25376(11) 1.13351(11) 0.32119(9) 0.0153(3) Uani 1 1 d . . . H14A H 0.1916 1.1445 0.3065 0.018 Uiso 1 1 calc R . . C15 C 0.32514(11) 1.04983(11) 0.29213(9) 0.0140(3) Uani 1 1 d . . . C16 C 0.70035(12) 1.16584(12) 0.58657(9) 0.0158(3) Uani 1 1 d . . . H16A H 0.7102 1.1008 0.6089 0.019 Uiso 1 1 calc R . . H16B H 0.6812 1.2122 0.6321 0.019 Uiso 1 1 calc R . . C17 C 0.66863(11) 1.02475(11) 0.47130(9) 0.0130(3) Uani 1 1 d . . . H17A H 0.7213 1.0054 0.4981 0.016 Uiso 1 1 calc R . . C18 C 0.47867(11) 1.24153(11) 0.49710(8) 0.0125(2) Uani 1 1 d . . . C19 C 0.83368(11) 0.83946(11) 0.41706(10) 0.0168(3) Uani 1 1 d . . . H19A H 0.8614 0.7705 0.4035 0.020 Uiso 1 1 calc R . . H19B H 0.8157 0.8468 0.4763 0.020 Uiso 1 1 calc R . . C20 C 0.46755(11) 0.93850(11) 0.26543(9) 0.0142(3) Uani 1 1 d . . . C21 C 0.79756(14) 1.37555(13) 1.31994(10) 0.0218(3) Uani 1 1 d . . . C22 C 0.61660(11) 0.89766(11) 0.32159(9) 0.0135(3) Uani 1 1 d . . . C23 C 0.40721(12) 0.91714(11) 0.21511(9) 0.0158(3) Uani 1 1 d . . . C24 C 0.23548(11) 1.34479(11) 0.43285(9) 0.0144(3) Uani 1 1 d . . . C25 C 0.33001(11) 1.28194(10) 0.44019(9) 0.0126(2) Uani 1 1 d . . . C26 C 0.52136(12) 1.35511(11) 0.59140(9) 0.0168(3) Uani 1 1 d . . . H26A H 0.5301 1.3416 0.6465 0.020 Uiso 1 1 calc R . . H26B H 0.4510 1.3915 0.5959 0.020 Uiso 1 1 calc R . . C27 C 0.22771(13) 0.99238(13) 0.20038(10) 0.0198(3) Uani 1 1 d . . . H27A H 0.2495 0.9591 0.1473 0.024 Uiso 1 1 calc R . . H27B H 0.1976 1.0606 0.1924 0.024 Uiso 1 1 calc R . . C28 C 0.56085(11) 0.88274(11) 0.26995(9) 0.0154(3) Uani 1 1 d . . . H28A H 0.5892 0.8291 0.2341 0.018 Uiso 1 1 calc R . . C29 C 0.73605(16) 1.22020(15) 0.95424(10) 0.0281(4) Uani 1 1 d . . . C30 C 0.71147(11) 0.83503(11) 0.32879(9) 0.0149(3) Uani 1 1 d . . . C31 C 0.91497(12) 0.89272(13) 0.38176(11) 0.0212(3) Uani 1 1 d . . . H31A H 0.9745 0.8655 0.4023 0.032 Uiso 1 1 calc R . . H31B H 0.8894 0.9606 0.3974 0.032 Uiso 1 1 calc R . . H31C H 0.9330 0.8861 0.3231 0.032 Uiso 1 1 calc R . . C32 C 0.39239(11) 1.30316(11) 0.48398(9) 0.0139(3) Uani 1 1 d . . . H32A H 0.3742 1.3657 0.5071 0.017 Uiso 1 1 calc R . . C33 C 0.57265(13) 1.20455(14) 1.25861(10) 0.0227(3) Uani 1 1 d . . . C34 C 0.19363(12) 1.44492(11) 0.46662(10) 0.0181(3) Uani 1 1 d . . . H34A H 0.1477 1.4812 0.4347 0.022 Uiso 1 1 calc R . . H34B H 0.2495 1.4763 0.4610 0.022 Uiso 1 1 calc R . . C35 C 0.01497(13) 1.28121(14) 0.43327(11) 0.0237(3) Uani 1 1 d . . . H35A H -0.0500 1.3009 0.4192 0.036 Uiso 1 1 calc R . . H35B H 0.0078 1.3047 0.4877 0.036 Uiso 1 1 calc R . . H35C H 0.0376 1.2112 0.4312 0.036 Uiso 1 1 calc R . . C36 C 0.61525(14) 1.32091(14) 1.33573(10) 0.0232(3) Uani 1 1 d . . . C37 C 0.80018(12) 1.17576(13) 0.53113(10) 0.0209(3) Uani 1 1 d . . . H37A H 0.8517 1.1646 0.5617 0.031 Uiso 1 1 calc R . . H37B H 0.7915 1.2403 0.5095 0.031 Uiso 1 1 calc R . . H37C H 0.8210 1.1287 0.4868 0.031 Uiso 1 1 calc R . . C38 C 0.76596(13) 0.74641(12) 0.27879(10) 0.0202(3) Uani 1 1 d . . . H38A H 0.7164 0.7189 0.2623 0.024 Uiso 1 1 calc R . . H38B H 0.8009 0.6987 0.3119 0.024 Uiso 1 1 calc R . . C39 C 0.44002(13) 0.83703(12) 0.15420(10) 0.0196(3) Uani 1 1 d . . . H39A H 0.5135 0.8252 0.1319 0.024 Uiso 1 1 calc R . . H39B H 0.4072 0.8572 0.1095 0.024 Uiso 1 1 calc R . . C40 C 0.95710(13) 1.22224(14) 1.24229(12) 0.0255(4) Uani 1 1 d . . . C41 C 0.72477(17) 1.54783(13) 1.10930(12) 0.0290(4) Uani 1 1 d . . . C42 C 0.65911(17) 1.52305(13) 1.06478(13) 0.0309(4) Uani 1 1 d . . . C43 C 0.87347(15) 1.07306(12) 1.20968(12) 0.0273(4) Uani 1 1 d . . . C44 C 0.80839(15) 1.04783(12) 1.16520(12) 0.0269(4) Uani 1 1 d . . . C45 C 0.79330(14) 1.28190(13) 1.33654(10) 0.0224(3) Uani 1 1 d . . . C46 C 0.66240(14) 1.13431(13) 1.26771(10) 0.0233(3) Uani 1 1 d . . . C47 C 0.61957(13) 1.41879(13) 1.31782(10) 0.0236(3) Uani 1 1 d . . . C48 C 0.68555(15) 1.11801(13) 1.05713(11) 0.0249(3) Uani 1 1 d . . . C49 C 0.70017(14) 1.25379(13) 1.34500(9) 0.0224(3) Uani 1 1 d . . . C50 C 0.83229(14) 1.12719(13) 1.28046(11) 0.0252(4) Uani 1 1 d . . . C51 C 0.64186(14) 1.11394(13) 1.13873(11) 0.0234(3) Uani 1 1 d . . . C52 C 0.96128(13) 1.32061(14) 1.22402(11) 0.0244(3) Uani 1 1 d . . . C53 C 0.73953(15) 1.50914(12) 1.24681(11) 0.0241(3) Uani 1 1 d . . . C54 C 0.87495(14) 1.20359(13) 1.29702(11) 0.0246(3) Uani 1 1 d . . . C55 C 0.97662(15) 1.14105(16) 1.01174(13) 0.0330(4) Uani 1 1 d . . . C56 C 0.52601(13) 1.27119(14) 1.13519(11) 0.0244(3) Uani 1 1 d . . . C57 C 0.67916(15) 1.54339(12) 1.19421(12) 0.0268(4) Uani 1 1 d . . . C58 C 0.72435(14) 1.15837(13) 1.31027(10) 0.0238(3) Uani 1 1 d . . . C59 C 1.00034(13) 1.16635(14) 1.16786(13) 0.0287(4) Uani 1 1 d . . . C60 C 0.50172(13) 1.36630(14) 1.16991(12) 0.0261(4) Uani 1 1 d . . . C61 C 0.57586(15) 1.37404(14) 1.03167(12) 0.0289(4) Uani 1 1 d . . . C62 C 0.88378(14) 1.39537(13) 1.26201(11) 0.0226(3) Uani 1 1 d . . . C63 C 0.76340(15) 0.51267(14) 0.76887(12) 0.0293(4) Uani 1 1 d . . . H63A H 0.7128 0.5680 0.7911 0.035 Uiso 1 1 calc R . . C64 C 0.64958(15) 1.20079(14) 1.01209(11) 0.0256(4) Uani 1 1 d . . . C65 C 0.13646(15) 1.44972(14) 0.55522(11) 0.0279(4) Uani 1 1 d . . . H65A H 0.1104 1.5167 0.5735 0.042 Uiso 1 1 calc R . . H65B H 0.1820 1.4160 0.5875 0.042 Uiso 1 1 calc R . . H65C H 0.0805 1.4195 0.5613 0.042 Uiso 1 1 calc R . . C66 C 0.41596(16) 0.74363(13) 0.18682(11) 0.0276(4) Uani 1 1 d . . . H66A H 0.4416 0.6943 0.1440 0.041 Uiso 1 1 calc R . . H66B H 0.3430 0.7535 0.2061 0.041 Uiso 1 1 calc R . . H66C H 0.4477 0.7231 0.2313 0.041 Uiso 1 1 calc R . . C67 C 0.57151(14) 1.27532(14) 1.04995(11) 0.0261(4) Uani 1 1 d . . . C68 C 0.54958(13) 1.29601(14) 1.29146(10) 0.0238(3) Uani 1 1 d . . . C69 C 0.89122(15) 1.48232(14) 1.13528(12) 0.0267(4) Uani 1 1 d . . . C70 C 0.56061(13) 1.19205(13) 1.17845(11) 0.0228(3) Uani 1 1 d . . . C71 C 0.84767(14) 1.47812(13) 1.21689(11) 0.0239(3) Uani 1 1 d . . . C72 C 0.84240(15) 0.76442(14) 0.20410(11) 0.0287(4) Uani 1 1 d . . . H72A H 0.8764 0.7040 0.1743 0.043 Uiso 1 1 calc R . . H72B H 0.8920 0.7913 0.2200 0.043 Uiso 1 1 calc R . . H72C H 0.8080 0.8096 0.1699 0.043 Uiso 1 1 calc R . . C73 C 0.55665(13) 1.45438(13) 1.26273(11) 0.0260(4) Uani 1 1 d . . . C74 C 0.95924(14) 1.09323(13) 1.15219(13) 0.0296(4) Uani 1 1 d . . . C75 C 0.51373(12) 1.37800(14) 1.24661(11) 0.0252(3) Uani 1 1 d . . . C76 C 0.53202(14) 1.42973(14) 1.10658(12) 0.0290(4) Uani 1 1 d . . . C77 C 0.26466(13) 1.22806(13) 0.97996(12) 0.0257(3) Uani 1 1 d . . . H77A H 0.2277 1.2619 0.9440 0.031 Uiso 1 1 calc R . . C78 C 0.91809(17) 1.27433(17) 0.93821(11) 0.0334(4) Uani 1 1 d . . . C79 C 0.58578(14) 1.51530(13) 1.20226(12) 0.0273(4) Uani 1 1 d . . . C80 C 0.79383(15) 1.08638(13) 1.02734(11) 0.0277(4) Uani 1 1 d . . . C81 C 0.57348(15) 1.50304(13) 1.12213(13) 0.0299(4) Uani 1 1 d . . . C82 C 0.93543(15) 0.42457(16) 0.73859(12) 0.0308(4) Uani 1 1 d . . . H82A H 1.0031 0.4191 0.7402 0.037 Uiso 1 1 calc R . . C83 C 0.31437(14) 1.13260(14) 0.96452(12) 0.0266(4) Uani 1 1 d . . . H83A H 0.3103 1.1007 0.9187 0.032 Uiso 1 1 calc R . . C84 C 1.00695(13) 1.32481(15) 1.13889(12) 0.0276(4) Uani 1 1 d . . . C85 C 0.85362(15) 1.05248(13) 1.08045(12) 0.0287(4) Uani 1 1 d . . . C86 C 1.01939(14) 1.21739(16) 1.02784(12) 0.0321(4) Uani 1 1 d . . . C87 C 0.70876(14) 1.44590(13) 1.31031(10) 0.0224(3) Uani 1 1 d . . . C88 C 0.94717(14) 1.08091(14) 1.07224(13) 0.0304(4) Uani 1 1 d . . . C89 C 0.97269(14) 1.40400(15) 1.09549(12) 0.0284(4) Uani 1 1 d . . . C90 C 0.59126(16) 1.41652(14) 0.55047(13) 0.0320(4) Uani 1 1 d . . . H90A H 0.5749 1.4766 0.5811 0.048 Uiso 1 1 calc R . . H90B H 0.5830 1.4304 0.4959 0.048 Uiso 1 1 calc R . . H90C H 0.6610 1.3822 0.5480 0.048 Uiso 1 1 calc R . . C91 C 0.82482(16) 1.14971(15) 0.96398(11) 0.0301(4) Uani 1 1 d . . . C92 C 0.70479(15) 1.07809(12) 1.19368(11) 0.0243(3) Uani 1 1 d . . . C93 C 0.87091(17) 1.46179(15) 1.00611(11) 0.0316(4) Uani 1 1 d . . . C94 C 0.26874(14) 1.27423(14) 1.04781(13) 0.0285(4) Uani 1 1 d . . . H94A H 0.2339 1.3395 1.0586 0.034 Uiso 1 1 calc R . . C95 C 0.32352(15) 1.22525(15) 1.09980(12) 0.0297(4) Uani 1 1 d . . . H95A H 0.3255 1.2567 1.1467 0.036 Uiso 1 1 calc R . . C96 C 0.37015(16) 1.08366(14) 1.01612(14) 0.0309(4) Uani 1 1 d . . . H96A H 0.4046 1.0183 1.0053 0.037 Uiso 1 1 calc R . . C97 C 0.96039(16) 1.39125(17) 1.01532(12) 0.0322(4) Uani 1 1 d . . . C98 C 0.81198(17) 0.36008(16) 0.70163(13) 0.0335(4) Uani 1 1 d . . . H98A H 0.7950 0.3105 0.6775 0.040 Uiso 1 1 calc R . . C99 C 0.73845(15) 0.44034(15) 0.73457(13) 0.0316(4) Uani 1 1 d . . . H99A H 0.6706 0.4457 0.7336 0.038 Uiso 1 1 calc R . . C100 C 0.65770(17) 1.39279(15) 0.97704(12) 0.0316(4) Uani 1 1 d . . . C101 C 0.70052(18) 1.46918(15) 0.99355(12) 0.0324(4) Uani 1 1 d . . . C102 C 1.03082(13) 1.22943(16) 1.10438(13) 0.0300(4) Uani 1 1 d . . . C103 C 0.98360(15) 1.29981(17) 0.98275(11) 0.0331(4) Uani 1 1 d . . . C104 C 0.86176(15) 0.50488(14) 0.77095(11) 0.0264(4) Uani 1 1 d . . . H10D H 0.8788 0.5548 0.7946 0.032 Uiso 1 1 calc R . . C105 C 0.73946(17) 1.31448(16) 0.93721(10) 0.0309(4) Uani 1 1 d . . . C106 C 0.82800(17) 1.51814(13) 1.08045(12) 0.0291(4) Uani 1 1 d . . . C107 C 0.14786(14) 0.94915(15) 0.25559(13) 0.0301(4) Uani 1 1 d . . . H10A H 0.0891 0.9593 0.2330 0.045 Uiso 1 1 calc R . . H10B H 0.1278 0.9801 0.3089 0.045 Uiso 1 1 calc R . . H10C H 0.1755 0.8804 0.2602 0.045 Uiso 1 1 calc R . . C108 C 0.37577(16) 1.12997(15) 1.08339(13) 0.0320(4) Uani 1 1 d . . . H10F H 0.4151 1.0969 1.1181 0.038 Uiso 1 1 calc R . . C109 C 0.91078(16) 0.35228(15) 0.70393(13) 0.0351(5) Uani 1 1 d . . . H10E H 0.9615 0.2971 0.6816 0.042 Uiso 1 1 calc R . . C110 C 0.91417(16) 1.17661(16) 0.95589(11) 0.0327(4) Uani 1 1 d . . . C111 C 0.83321(18) 1.34189(17) 0.92889(10) 0.0340(5) Uani 1 1 d . . . C112 C 0.80837(18) 1.43783(16) 0.96393(11) 0.0337(5) 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 Pt1 0.00988(3) 0.01049(3) 0.01083(3) -0.00037(2) -0.00223(2) -0.00337(2) N1 0.0120(5) 0.0130(6) 0.0134(5) -0.0012(4) -0.0032(4) -0.0046(4) N3 0.0098(5) 0.0117(5) 0.0115(5) -0.0005(4) -0.0023(4) -0.0035(4) N2 0.0113(5) 0.0122(5) 0.0134(5) 0.0001(4) -0.0035(4) -0.0036(4) N4 0.0121(5) 0.0115(5) 0.0121(5) -0.0006(4) -0.0028(4) -0.0041(4) C5 0.0120(6) 0.0127(6) 0.0120(6) -0.0002(5) -0.0030(5) -0.0040(5) C6 0.0127(6) 0.0113(6) 0.0161(6) 0.0006(5) -0.0019(5) -0.0029(5) C7 0.0109(6) 0.0115(6) 0.0134(6) 0.0014(5) -0.0021(5) -0.0037(5) C8 0.0118(6) 0.0149(6) 0.0142(6) 0.0018(5) -0.0040(5) -0.0033(5) C9 0.0130(6) 0.0137(6) 0.0165(6) 0.0022(5) -0.0048(5) -0.0022(5) C10 0.0180(7) 0.0174(7) 0.0153(6) -0.0001(5) -0.0063(5) -0.0075(6) C11 0.0122(6) 0.0155(6) 0.0113(6) -0.0010(5) -0.0022(5) -0.0054(5) C12 0.0129(6) 0.0158(7) 0.0124(6) -0.0024(5) -0.0022(5) -0.0054(5) C13 0.0152(7) 0.0173(7) 0.0219(7) 0.0027(6) -0.0086(6) -0.0031(5) C14 0.0141(6) 0.0168(7) 0.0168(6) 0.0001(5) -0.0063(5) -0.0045(5) C15 0.0145(6) 0.0161(7) 0.0134(6) 0.0005(5) -0.0052(5) -0.0059(5) C16 0.0169(7) 0.0196(7) 0.0130(6) -0.0011(5) -0.0063(5) -0.0056(6) C17 0.0121(6) 0.0143(6) 0.0132(6) 0.0016(5) -0.0041(5) -0.0034(5) C18 0.0118(6) 0.0134(6) 0.0119(6) -0.0016(5) -0.0011(5) -0.0039(5) C19 0.0143(6) 0.0149(7) 0.0204(7) 0.0024(5) -0.0052(5) -0.0015(5) C20 0.0153(6) 0.0153(7) 0.0133(6) -0.0013(5) -0.0029(5) -0.0066(5) C21 0.0270(8) 0.0278(8) 0.0148(7) -0.0027(6) -0.0094(6) -0.0098(7) C22 0.0130(6) 0.0123(6) 0.0144(6) -0.0019(5) -0.0011(5) -0.0037(5) C23 0.0181(7) 0.0172(7) 0.0143(6) -0.0021(5) -0.0052(5) -0.0070(6) C24 0.0124(6) 0.0128(6) 0.0171(6) 0.0012(5) -0.0034(5) -0.0019(5) C25 0.0110(6) 0.0121(6) 0.0140(6) 0.0000(5) -0.0021(5) -0.0023(5) C26 0.0188(7) 0.0167(7) 0.0154(6) -0.0041(5) -0.0037(5) -0.0054(6) C27 0.0199(7) 0.0233(8) 0.0204(7) -0.0008(6) -0.0100(6) -0.0077(6) C28 0.0149(6) 0.0148(7) 0.0161(6) -0.0034(5) -0.0016(5) -0.0045(5) C29 0.0381(10) 0.0380(10) 0.0142(7) -0.0063(7) -0.0084(7) -0.0173(8) C30 0.0132(6) 0.0129(6) 0.0173(6) -0.0001(5) -0.0016(5) -0.0031(5) C31 0.0144(7) 0.0228(8) 0.0274(8) 0.0020(6) -0.0066(6) -0.0051(6) C32 0.0130(6) 0.0122(6) 0.0159(6) -0.0016(5) -0.0023(5) -0.0029(5) C33 0.0184(7) 0.0314(9) 0.0200(7) 0.0010(6) 0.0014(6) -0.0153(7) C34 0.0162(7) 0.0122(6) 0.0251(8) -0.0001(6) -0.0058(6) -0.0013(5) C35 0.0165(7) 0.0281(9) 0.0291(8) 0.0060(7) -0.0089(6) -0.0074(6) C36 0.0231(8) 0.0324(9) 0.0118(6) -0.0043(6) 0.0035(6) -0.0098(7) C37 0.0153(7) 0.0270(8) 0.0218(7) 0.0000(6) -0.0061(6) -0.0061(6) C38 0.0191(7) 0.0148(7) 0.0246(8) -0.0054(6) -0.0043(6) -0.0007(6) C39 0.0206(7) 0.0228(8) 0.0168(7) -0.0067(6) -0.0050(6) -0.0062(6) C40 0.0201(8) 0.0278(9) 0.0322(9) 0.0022(7) -0.0164(7) -0.0027(7) C41 0.0457(11) 0.0122(7) 0.0354(10) 0.0076(7) -0.0189(9) -0.0107(7) C42 0.0460(11) 0.0166(8) 0.0364(10) 0.0123(7) -0.0243(9) -0.0073(8) C43 0.0288(9) 0.0135(7) 0.0387(10) 0.0049(7) -0.0136(8) 0.0012(6) C44 0.0335(9) 0.0094(7) 0.0375(10) 0.0014(6) -0.0096(8) -0.0041(6) C45 0.0284(8) 0.0287(9) 0.0137(7) 0.0034(6) -0.0106(6) -0.0088(7) C46 0.0293(9) 0.0215(8) 0.0222(8) 0.0087(6) -0.0039(7) -0.0154(7) C47 0.0232(8) 0.0254(8) 0.0172(7) -0.0119(6) 0.0008(6) -0.0007(7) C48 0.0328(9) 0.0216(8) 0.0255(8) -0.0072(6) -0.0076(7) -0.0146(7) C49 0.0288(8) 0.0292(9) 0.0112(6) 0.0041(6) -0.0033(6) -0.0126(7) C50 0.0308(9) 0.0187(8) 0.0285(8) 0.0107(7) -0.0147(7) -0.0047(7) C51 0.0286(8) 0.0201(8) 0.0274(8) -0.0009(6) -0.0069(7) -0.0162(7) C52 0.0187(7) 0.0319(9) 0.0287(8) -0.0003(7) -0.0121(7) -0.0112(7) C53 0.0343(9) 0.0134(7) 0.0266(8) -0.0075(6) -0.0093(7) -0.0066(6) C54 0.0283(9) 0.0255(8) 0.0247(8) 0.0068(7) -0.0177(7) -0.0050(7) C55 0.0215(8) 0.0358(11) 0.0324(10) -0.0186(8) 0.0074(7) -0.0009(7) C56 0.0144(7) 0.0337(9) 0.0289(8) -0.0024(7) -0.0084(6) -0.0094(7) C57 0.0368(10) 0.0088(7) 0.0349(9) -0.0041(6) -0.0120(8) -0.0017(6) C58 0.0316(9) 0.0239(8) 0.0191(7) 0.0112(6) -0.0078(7) -0.0127(7) C59 0.0142(7) 0.0283(9) 0.0407(10) -0.0027(8) -0.0095(7) 0.0032(6) C60 0.0127(7) 0.0308(9) 0.0340(9) -0.0029(7) -0.0086(7) -0.0008(6) C61 0.0334(10) 0.0303(9) 0.0311(9) 0.0053(7) -0.0243(8) -0.0071(8) C62 0.0273(8) 0.0251(8) 0.0235(8) -0.0011(6) -0.0135(7) -0.0138(7) C63 0.0263(9) 0.0224(9) 0.0345(10) -0.0024(7) -0.0031(8) -0.0017(7) C64 0.0330(9) 0.0312(9) 0.0208(8) -0.0046(7) -0.0129(7) -0.0158(8) C65 0.0309(9) 0.0209(8) 0.0256(8) -0.0064(7) 0.0000(7) -0.0009(7) C66 0.0436(11) 0.0156(7) 0.0231(8) -0.0031(6) -0.0124(8) -0.0019(7) C67 0.0266(8) 0.0336(10) 0.0262(8) 0.0003(7) -0.0168(7) -0.0122(7) C68 0.0164(7) 0.0337(9) 0.0187(7) -0.0044(7) 0.0043(6) -0.0094(7) C69 0.0347(10) 0.0241(9) 0.0299(9) 0.0040(7) -0.0096(7) -0.0221(8) C70 0.0203(7) 0.0269(9) 0.0260(8) -0.0015(7) -0.0047(6) -0.0151(7) C71 0.0328(9) 0.0188(8) 0.0273(8) -0.0021(6) -0.0118(7) -0.0146(7) C72 0.0301(9) 0.0282(9) 0.0200(8) -0.0084(7) 0.0009(7) 0.0011(7) C73 0.0194(8) 0.0233(8) 0.0289(9) -0.0116(7) -0.0024(7) 0.0048(6) C74 0.0212(8) 0.0179(8) 0.0438(11) -0.0049(7) -0.0087(8) 0.0077(6) C75 0.0116(7) 0.0294(9) 0.0295(9) -0.0084(7) 0.0008(6) -0.0002(6) C76 0.0231(8) 0.0269(9) 0.0381(10) 0.0019(8) -0.0190(8) 0.0027(7) C77 0.0202(8) 0.0243(8) 0.0337(9) 0.0071(7) -0.0075(7) -0.0080(7) C78 0.0380(11) 0.0484(12) 0.0132(7) -0.0065(7) 0.0071(7) -0.0215(10) C79 0.0274(9) 0.0148(7) 0.0359(10) -0.0068(7) -0.0105(8) 0.0060(6) C80 0.0353(10) 0.0196(8) 0.0273(8) -0.0143(7) -0.0020(7) -0.0086(7) C81 0.0313(9) 0.0168(8) 0.0409(11) 0.0014(7) -0.0203(8) 0.0067(7) C82 0.0208(8) 0.0388(11) 0.0316(9) 0.0074(8) -0.0049(7) -0.0075(8) C83 0.0275(9) 0.0243(9) 0.0305(9) 0.0034(7) -0.0072(7) -0.0110(7) C84 0.0148(7) 0.0385(10) 0.0329(9) -0.0028(8) -0.0040(7) -0.0137(7) C85 0.0318(9) 0.0131(7) 0.0370(10) -0.0119(7) -0.0040(8) -0.0007(7) C86 0.0158(8) 0.0415(11) 0.0320(9) -0.0123(8) 0.0087(7) -0.0066(7) C87 0.0282(8) 0.0212(8) 0.0179(7) -0.0097(6) -0.0047(6) -0.0055(7) C88 0.0226(8) 0.0210(8) 0.0397(10) -0.0141(8) -0.0007(8) 0.0044(7) C89 0.0248(8) 0.0354(10) 0.0310(9) 0.0013(8) -0.0029(7) -0.0223(8) C90 0.0348(10) 0.0207(8) 0.0362(10) -0.0112(7) 0.0091(8) -0.0150(8) C91 0.0371(10) 0.0331(10) 0.0185(8) -0.0149(7) 0.0007(7) -0.0109(8) C92 0.0318(9) 0.0138(7) 0.0306(9) 0.0034(6) -0.0071(7) -0.0126(7) C93 0.0469(12) 0.0323(10) 0.0231(8) 0.0121(7) -0.0066(8) -0.0273(9) C94 0.0185(8) 0.0234(9) 0.0425(11) -0.0009(8) -0.0027(7) -0.0079(7) C95 0.0280(9) 0.0333(10) 0.0332(9) 0.0000(8) -0.0065(8) -0.0181(8) C96 0.0315(10) 0.0190(8) 0.0461(11) 0.0063(8) -0.0150(9) -0.0087(7) C97 0.0330(10) 0.0443(12) 0.0235(8) 0.0048(8) 0.0032(7) -0.0278(9) C98 0.0398(11) 0.0294(10) 0.0329(10) -0.0039(8) -0.0060(8) -0.0139(9) C99 0.0238(9) 0.0334(10) 0.0402(11) 0.0016(8) -0.0102(8) -0.0091(8) C100 0.0475(12) 0.0333(10) 0.0238(8) 0.0102(7) -0.0248(8) -0.0136(9) C101 0.0508(12) 0.0285(9) 0.0271(9) 0.0161(7) -0.0224(9) -0.0161(9) C102 0.0111(7) 0.0372(10) 0.0385(10) -0.0061(8) -0.0004(7) -0.0046(7) C103 0.0271(9) 0.0493(12) 0.0208(8) -0.0043(8) 0.0100(7) -0.0207(9) C104 0.0327(9) 0.0294(9) 0.0211(8) 0.0035(7) -0.0067(7) -0.0155(8) C105 0.0460(11) 0.0410(11) 0.0124(7) 0.0035(7) -0.0124(7) -0.0186(9) C106 0.0460(11) 0.0205(8) 0.0294(9) 0.0099(7) -0.0132(8) -0.0214(8) C107 0.0228(8) 0.0341(10) 0.0400(10) 0.0108(8) -0.0147(8) -0.0134(7) C108 0.0360(10) 0.0300(10) 0.0390(11) 0.0140(8) -0.0184(9) -0.0179(8) C109 0.0304(10) 0.0278(10) 0.0359(10) -0.0025(8) 0.0037(8) 0.0022(8) C110 0.0332(10) 0.0394(11) 0.0195(8) -0.0162(8) 0.0084(7) -0.0103(9) C111 0.0503(12) 0.0475(12) 0.0096(7) 0.0056(7) -0.0037(7) -0.0266(10) C112 0.0542(13) 0.0376(11) 0.0183(8) 0.0152(7) -0.0117(8) -0.0271(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 Pt1 N2 2.0105(13) . ? Pt1 N4 2.0117(13) . ? Pt1 N1 2.0136(12) . ? Pt1 N3 2.0178(12) . ? N1 C20 1.3763(19) . ? N1 C15 1.3773(18) . ? N3 C5 1.3729(18) . ? N3 C18 1.3756(19) . ? N2 C25 1.3760(19) . ? N2 C8 1.3778(18) . ? N4 C7 1.3731(18) . ? N4 C22 1.3774(19) . ? C5 C17 1.386(2) . ? C5 C11 1.443(2) . ? C6 C30 1.365(2) . ? C6 C7 1.447(2) . ? C6 C19 1.499(2) . ? C7 C17 1.381(2) . ? C8 C14 1.384(2) . ? C8 C9 1.446(2) . ? C9 C24 1.365(2) . ? C9 C13 1.496(2) . ? C10 C23 1.368(2) . ? C10 C15 1.445(2) . ? C10 C27 1.498(2) . ? C11 C12 1.366(2) . ? C11 C16 1.501(2) . ? C12 C18 1.452(2) . ? C12 C26 1.497(2) . ? C13 C35 1.532(2) . ? C14 C15 1.386(2) . ? C16 C37 1.535(2) . ? C18 C32 1.384(2) . ? C19 C31 1.533(2) . ? C20 C28 1.385(2) . ? C20 C23 1.447(2) . ? C21 C45 1.384(3) . ? C21 C87 1.447(3) . ? C21 C62 1.456(3) . ? C22 C28 1.380(2) . ? C22 C30 1.451(2) . ? C23 C39 1.496(2) . ? C24 C25 1.450(2) . ? C24 C34 1.500(2) . ? C25 C32 1.387(2) . ? C26 C90 1.520(2) . ? C27 C107 1.532(3) . ? C29 C105 1.391(3) . ? C29 C91 1.448(3) . ? C29 C64 1.455(3) . ? C30 C38 1.497(2) . ? C33 C68 1.387(3) . ? C33 C70 1.453(2) . ? C33 C46 1.453(3) . ? C34 C65 1.533(2) . ? C36 C49 1.383(3) . ? C36 C47 1.448(3) . ? C36 C68 1.454(3) . ? C38 C72 1.522(3) . ? C39 C66 1.525(3) . ? C40 C54 1.382(3) . ? C40 C59 1.453(3) . ? C40 C52 1.455(3) . ? C41 C106 1.385(3) . ? C41 C57 1.449(3) . ? C41 C42 1.456(3) . ? C42 C101 1.394(3) . ? C42 C81 1.446(3) . ? C43 C50 1.389(3) . ? C43 C74 1.449(3) . ? C43 C44 1.451(3) . ? C44 C92 1.389(3) . ? C44 C85 1.445(3) . ? C45 C49 1.449(3) . ? C45 C54 1.449(3) . ? C46 C58 1.385(3) . ? C46 C92 1.449(3) . ? C47 C87 1.390(3) . ? C47 C73 1.450(3) . ? C48 C51 1.391(3) . ? C48 C64 1.450(3) . ? C48 C80 1.452(3) . ? C49 C58 1.450(3) . ? C50 C58 1.447(3) . ? C50 C54 1.452(3) . ? C51 C70 1.446(3) . ? C51 C92 1.449(3) . ? C52 C62 1.382(3) . ? C52 C84 1.452(3) . ? C53 C57 1.388(3) . ? C53 C87 1.449(3) . ? C53 C71 1.450(3) . ? C55 C88 1.380(3) . ? C55 C86 1.450(3) . ? C55 C110 1.456(3) . ? C56 C70 1.389(3) . ? C56 C60 1.446(3) . ? C56 C67 1.453(3) . ? C57 C79 1.453(3) . ? C59 C74 1.391(3) . ? C59 C102 1.446(3) . ? C60 C75 1.392(3) . ? C60 C76 1.447(3) . ? C61 C100 1.379(3) . ? C61 C76 1.459(3) . ? C61 C67 1.461(3) . ? C62 C71 1.451(3) . ? C63 C99 1.379(3) . ? C63 C104 1.380(3) . ? C64 C67 1.383(3) . ? C68 C75 1.440(3) . ? C69 C71 1.391(3) . ? C69 C89 1.449(3) . ? C69 C106 1.450(3) . ? C73 C79 1.386(3) . ? C73 C75 1.452(3) . ? C74 C88 1.449(3) . ? C76 C81 1.396(3) . ? C77 C83 1.385(3) . ? C77 C94 1.386(3) . ? C78 C111 1.386(3) . ? C78 C110 1.443(3) . ? C78 C103 1.459(3) . ? C79 C81 1.453(3) . ? C80 C85 1.389(3) . ? C80 C91 1.449(3) . ? C82 C109 1.379(3) . ? C82 C104 1.380(3) . ? C83 C96 1.388(3) . ? C84 C89 1.390(3) . ? C84 C102 1.448(3) . ? C85 C88 1.457(3) . ? C86 C102 1.387(3) . ? C86 C103 1.446(3) . ? C89 C97 1.455(3) . ? C91 C110 1.389(3) . ? C93 C112 1.386(3) . ? C93 C97 1.453(3) . ? C93 C106 1.455(3) . ? C94 C95 1.385(3) . ? C95 C108 1.393(3) . ? C96 C108 1.387(3) . ? C97 C103 1.385(3) . ? C98 C99 1.381(3) . ? C98 C109 1.387(3) . ? C100 C105 1.451(3) . ? C100 C101 1.453(3) . ? C101 C112 1.446(3) . ? C105 C111 1.452(3) . ? C111 C112 1.458(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 N2 Pt1 N4 179.30(5) . . ? N2 Pt1 N1 90.21(5) . . ? N4 Pt1 N1 89.83(5) . . ? N2 Pt1 N3 89.71(5) . . ? N4 Pt1 N3 90.25(5) . . ? N1 Pt1 N3 179.40(5) . . ? C20 N1 C15 106.23(12) . . ? C20 N1 Pt1 126.91(10) . . ? C15 N1 Pt1 126.85(10) . . ? C5 N3 C18 106.39(12) . . ? C5 N3 Pt1 126.46(10) . . ? C18 N3 Pt1 127.13(10) . . ? C25 N2 C8 106.23(12) . . ? C25 N2 Pt1 127.11(10) . . ? C8 N2 Pt1 126.64(10) . . ? C7 N4 C22 106.22(12) . . ? C7 N4 Pt1 126.69(10) . . ? C22 N4 Pt1 127.06(10) . . ? N3 C5 C17 125.10(13) . . ? N3 C5 C11 110.23(13) . . ? C17 C5 C11 124.64(13) . . ? C30 C6 C7 106.69(13) . . ? C30 C6 C19 128.65(14) . . ? C7 C6 C19 124.62(14) . . ? N4 C7 C17 125.12(13) . . ? N4 C7 C6 110.35(13) . . ? C17 C7 C6 124.48(13) . . ? N2 C8 C14 124.97(14) . . ? N2 C8 C9 109.98(13) . . ? C14 C8 C9 124.96(14) . . ? C24 C9 C8 107.00(13) . . ? C24 C9 C13 128.19(14) . . ? C8 C9 C13 124.73(14) . . ? C23 C10 C15 106.87(13) . . ? C23 C10 C27 127.87(14) . . ? C15 C10 C27 125.27(14) . . ? C12 C11 C5 106.88(12) . . ? C12 C11 C16 128.61(14) . . ? C5 C11 C16 124.50(13) . . ? C11 C12 C18 106.64(13) . . ? C11 C12 C26 127.76(13) . . ? C18 C12 C26 125.58(13) . . ? C9 C13 C35 112.09(13) . . ? C8 C14 C15 126.21(14) . . ? N1 C15 C14 124.58(14) . . ? N1 C15 C10 110.05(13) . . ? C14 C15 C10 125.23(14) . . ? C11 C16 C37 113.65(12) . . ? C7 C17 C5 125.98(13) . . ? N3 C18 C32 124.72(13) . . ? N3 C18 C12 109.85(12) . . ? C32 C18 C12 125.42(14) . . ? C6 C19 C31 113.31(13) . . ? N1 C20 C28 124.71(14) . . ? N1 C20 C23 110.15(13) . . ? C28 C20 C23 125.08(14) . . ? C45 C21 C87 119.95(16) . . ? C45 C21 C62 119.90(17) . . ? C87 C21 C62 107.89(15) . . ? N4 C22 C28 124.72(14) . . ? N4 C22 C30 109.96(13) . . ? C28 C22 C30 125.33(14) . . ? C10 C23 C20 106.64(13) . . ? C10 C23 C39 128.06(14) . . ? C20 C23 C39 125.29(14) . . ? C9 C24 C25 106.60(13) . . ? C9 C24 C34 128.10(14) . . ? C25 C24 C34 125.29(14) . . ? N2 C25 C32 124.80(13) . . ? N2 C25 C24 110.11(13) . . ? C32 C25 C24 125.02(14) . . ? C12 C26 C90 113.28(13) . . ? C10 C27 C107 112.68(14) . . ? C22 C28 C20 126.22(14) . . ? C105 C29 C91 120.59(19) . . ? C105 C29 C64 119.41(19) . . ? C91 C29 C64 108.03(17) . . ? C6 C30 C22 106.77(13) . . ? C6 C30 C38 128.11(14) . . ? C22 C30 C38 125.10(14) . . ? C18 C32 C25 125.97(14) . . ? C68 C33 C70 119.50(17) . . ? C68 C33 C46 120.24(16) . . ? C70 C33 C46 107.83(16) . . ? C24 C34 C65 113.39(14) . . ? C49 C36 C47 120.05(17) . . ? C49 C36 C68 120.17(17) . . ? C47 C36 C68 107.88(16) . . ? C30 C38 C72 113.09(14) . . ? C23 C39 C66 114.34(14) . . ? C54 C40 C59 120.28(18) . . ? C54 C40 C52 119.93(17) . . ? C59 C40 C52 107.41(17) . . ? C106 C41 C57 120.40(17) . . ? C106 C41 C42 119.82(19) . . ? C57 C41 C42 107.95(18) . . ? C101 C42 C81 120.00(19) . . ? C101 C42 C41 119.8(2) . . ? C81 C42 C41 108.08(18) . . ? C50 C43 C74 119.72(18) . . ? C50 C43 C44 120.11(18) . . ? C74 C43 C44 108.01(18) . . ? C92 C44 C85 119.85(18) . . ? C92 C44 C43 119.73(18) . . ? C85 C44 C43 108.12(18) . . ? C21 C45 C49 120.43(16) . . ? C21 C45 C54 120.15(17) . . ? C49 C45 C54 107.89(16) . . ? C58 C46 C92 120.53(17) . . ? C58 C46 C33 119.88(17) . . ? C92 C46 C33 107.98(16) . . ? C87 C47 C36 120.25(17) . . ? C87 C47 C73 120.20(17) . . ? C36 C47 C73 107.99(16) . . ? C51 C48 C64 119.88(17) . . ? C51 C48 C80 119.98(17) . . ? C64 C48 C80 108.11(17) . . ? C36 C49 C45 119.68(17) . . ? C36 C49 C58 120.13(16) . . ? C45 C49 C58 107.99(16) . . ? C43 C50 C58 120.13(17) . . ? C43 C50 C54 120.26(18) . . ? C58 C50 C54 107.73(16) . . ? C48 C51 C70 120.01(17) . . ? C48 C51 C92 119.77(17) . . ? C70 C51 C92 108.24(16) . . ? C62 C52 C84 120.05(17) . . ? C62 C52 C40 120.09(17) . . ? C84 C52 C40 108.15(17) . . ? C57 C53 C87 119.83(17) . . ? C57 C53 C71 120.13(17) . . ? C87 C53 C71 108.18(16) . . ? C40 C54 C45 120.05(17) . . ? C40 C54 C50 119.85(18) . . ? C45 C54 C50 108.17(16) . . ? C88 C55 C86 120.2(2) . . ? C88 C55 C110 120.12(19) . . ? C86 C55 C110 107.7(2) . . ? C70 C56 C60 120.06(16) . . ? C70 C56 C67 119.92(17) . . ? C60 C56 C67 108.27(17) . . ? C53 C57 C41 119.66(19) . . ? C53 C57 C79 120.18(18) . . ? C41 C57 C79 107.95(17) . . ? C46 C58 C50 119.66(17) . . ? C46 C58 C49 120.00(17) . . ? C50 C58 C49 108.21(16) . . ? C74 C59 C102 119.90(19) . . ? C74 C59 C40 119.69(19) . . ? C102 C59 C40 108.43(18) . . ? C75 C60 C56 119.61(17) . . ? C75 C60 C76 120.22(18) . . ? C56 C60 C76 108.02(17) . . ? C100 C61 C76 120.62(19) . . ? C100 C61 C67 120.07(19) . . ? C76 C61 C67 107.10(17) . . ? C52 C62 C71 120.09(17) . . ? C52 C62 C21 119.88(17) . . ? C71 C62 C21 107.96(16) . . ? C99 C63 C104 120.15(18) . . ? C67 C64 C48 120.14(17) . . ? C67 C64 C29 120.36(18) . . ? C48 C64 C29 107.77(17) . . ? C64 C67 C56 119.99(17) . . ? C64 C67 C61 119.79(18) . . ? C56 C67 C61 108.07(17) . . ? C33 C68 C75 120.32(16) . . ? C33 C68 C36 119.58(17) . . ? C75 C68 C36 108.10(16) . . ? C71 C69 C89 119.90(18) . . ? C71 C69 C106 119.71(19) . . ? C89 C69 C106 108.34(17) . . ? C56 C70 C51 120.05(16) . . ? C56 C70 C33 120.16(17) . . ? C51 C70 C33 107.99(16) . . ? C69 C71 C53 120.06(17) . . ? C69 C71 C62 120.00(18) . . ? C53 C71 C62 107.84(16) . . ? C79 C73 C47 119.87(18) . . ? C79 C73 C75 120.40(17) . . ? C47 C73 C75 107.84(17) . . ? C59 C74 C88 119.7(2) . . ? C59 C74 C43 120.19(19) . . ? C88 C74 C43 108.06(18) . . ? C60 C75 C68 120.35(17) . . ? C60 C75 C73 119.59(18) . . ? C68 C75 C73 108.19(16) . . ? C81 C76 C60 120.13(18) . . ? C81 C76 C61 119.17(19) . . ? C60 C76 C61 108.54(17) . . ? C83 C77 C94 120.12(18) . . ? C111 C78 C110 120.5(2) . . ? C111 C78 C103 119.7(2) . . ? C110 C78 C103 108.0(2) . . ? C73 C79 C57 119.96(17) . . ? C73 C79 C81 120.07(18) . . ? C57 C79 C81 108.04(18) . . ? C85 C80 C91 119.86(19) . . ? C85 C80 C48 119.88(18) . . ? C91 C80 C48 107.97(18) . . ? C76 C81 C42 120.29(19) . . ? C76 C81 C79 119.60(19) . . ? C42 C81 C79 107.98(18) . . ? C109 C82 C104 120.01(19) . . ? C77 C83 C96 119.94(19) . . ? C89 C84 C102 120.15(18) . . ? C89 C84 C52 120.03(18) . . ? C102 C84 C52 107.96(18) . . ? C80 C85 C44 120.25(18) . . ? C80 C85 C88 119.81(19) . . ? C44 C85 C88 107.93(18) . . ? C102 C86 C103 120.08(19) . . ? C102 C86 C55 119.6(2) . . ? C103 C86 C55 108.33(19) . . ? C47 C87 C21 119.63(17) . . ? C47 C87 C53 119.96(16) . . ? C21 C87 C53 108.12(16) . . ? C55 C88 C74 120.28(19) . . ? C55 C88 C85 120.2(2) . . ? C74 C88 C85 107.88(18) . . ? C84 C89 C69 119.93(18) . . ? C84 C89 C97 120.04(19) . . ? C69 C89 C97 107.96(18) . . ? C110 C91 C29 119.6(2) . . ? C110 C91 C80 120.4(2) . . ? C29 C91 C80 108.12(18) . . ? C44 C92 C51 120.27(17) . . ? C44 C92 C46 119.83(17) . . ? C51 C92 C46 107.95(16) . . ? C112 C93 C97 119.9(2) . . ? C112 C93 C106 120.0(2) . . ? C97 C93 C106 108.11(17) . . ? C95 C94 C77 120.02(18) . . ? C94 C95 C108 120.05(19) . . ? C108 C96 C83 120.15(19) . . ? C103 C97 C93 120.59(19) . . ? C103 C97 C89 119.4(2) . . ? C93 C97 C89 107.83(19) . . ? C99 C98 C109 119.7(2) . . ? C63 C99 C98 120.10(19) . . ? C61 C100 C105 120.08(19) . . ? C61 C100 C101 119.9(2) . . ? C105 C100 C101 108.10(19) . . ? C42 C101 C112 120.15(19) . . ? C42 C101 C100 120.0(2) . . ? C112 C101 C100 107.75(19) . . ? C86 C102 C59 120.34(19) . . ? C86 C102 C84 119.8(2) . . ? C59 C102 C84 108.06(17) . . ? C97 C103 C86 120.56(19) . . ? C97 C103 C78 119.7(2) . . ? C86 C103 C78 107.77(19) . . ? C63 C104 C82 119.98(19) . . ? C29 C105 C100 120.29(19) . . ? C29 C105 C111 119.4(2) . . ? C100 C105 C111 108.25(19) . . ? C41 C106 C69 120.04(18) . . ? C41 C106 C93 120.18(18) . . ? C69 C106 C93 107.75(19) . . ? C96 C108 C95 119.69(18) . . ? C82 C109 C98 120.09(19) . . ? C91 C110 C78 120.1(2) . . ? C91 C110 C55 119.6(2) . . ? C78 C110 C55 108.12(19) . . ? C78 C111 C105 119.9(2) . . ? C78 C111 C112 120.53(19) . . ? C105 C111 C112 107.4(2) . . ? C93 C112 C101 120.0(2) . . ? C93 C112 C111 119.6(2) . . ? C101 C112 C111 108.55(18) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 0.864 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.075 #===END data_ab011 _database_code_CSD 198537 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TCNQ$.!Cu(OEP) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H48 Cu N8' _chemical_formula_weight 800.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.0673(6) _cell_length_b 25.567(2) _cell_length_c 11.0938(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.018(4) _cell_angle_gamma 90.00 _cell_volume 1999.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 6327 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 31.5 _exptl_crystal_description needle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 842 _exptl_absorpt_coefficient_mu 0.592 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7290 _exptl_absorpt_correction_T_max 0.9164 _exptl_absorpt_process_details 'SADABS 2.0' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 frames remeasured' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 27755 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 31.50 _reflns_number_total 6376 _reflns_number_gt 5514 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.03, XP (Sheldrick, 1994)' _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^)+(0.0523P)^2^+0.6200P] 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 6376 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Cu1 Cu 0.5000 0.0000 0.5000 0.01114(6) Uani 1 2 d S . . N1 N 0.56122(13) 0.06699(3) 0.58755(8) 0.01296(17) Uani 1 1 d . . . N2 N 0.39552(13) 0.03965(3) 0.35416(8) 0.01287(17) Uani 1 1 d . . . N3 N -0.04579(18) 0.18174(5) 0.42378(12) 0.0305(3) Uani 1 1 d . . . N4 N -0.24400(16) 0.07326(5) 0.13495(11) 0.0272(2) Uani 1 1 d . . . C1 C 0.64646(15) 0.07347(4) 0.70217(10) 0.01408(19) Uani 1 1 d . . . C2 C 0.66576(16) 0.12866(4) 0.73127(10) 0.0155(2) Uani 1 1 d . . . C3 C 0.58986(16) 0.15536(4) 0.63297(10) 0.0155(2) Uani 1 1 d . . . C4 C 0.52589(15) 0.11664(4) 0.54457(10) 0.01375(19) Uani 1 1 d . . . C5 C 0.44446(15) 0.12879(4) 0.43049(10) 0.01462(19) Uani 1 1 d . . . H5 H 0.4273 0.1648 0.4117 0.018 Uiso 1 1 calc R . . C6 C 0.38603(15) 0.09314(4) 0.34178(10) 0.01340(19) Uani 1 1 d . . . C7 C 0.30500(15) 0.10746(4) 0.22313(10) 0.01454(19) Uani 1 1 d . . . C8 C 0.26490(15) 0.06168(4) 0.16282(10) 0.01473(19) Uani 1 1 d . . . C9 C 0.32012(15) 0.01981(4) 0.24579(10) 0.01348(18) Uani 1 1 d . . . C10 C 0.29819(15) -0.03317(4) 0.22005(10) 0.01471(19) Uani 1 1 d . . . H10 H 0.2407 -0.0424 0.1430 0.018 Uiso 1 1 calc R . . C11 C 0.76055(19) 0.15168(5) 0.84454(11) 0.0208(2) Uani 1 1 d . . . H11A H 0.7569 0.1260 0.9111 0.025 Uiso 1 1 calc R . . H11B H 0.6900 0.1832 0.8675 0.025 Uiso 1 1 calc R . . C12 C 0.9673(2) 0.16659(6) 0.82772(13) 0.0287(3) Uani 1 1 d . . . H12A H 1.0391 0.1352 0.8092 0.043 Uiso 1 1 calc R . . H12B H 1.0234 0.1825 0.9022 0.043 Uiso 1 1 calc R . . H12C H 0.9714 0.1916 0.7610 0.043 Uiso 1 1 calc R . . C13 C 0.57214(17) 0.21347(4) 0.61686(11) 0.0187(2) Uani 1 1 d . . . H13A H 0.6055 0.2227 0.5343 0.022 Uiso 1 1 calc R . . H13B H 0.6644 0.2309 0.6749 0.022 Uiso 1 1 calc R . . C14 C 0.3733(2) 0.23425(5) 0.63570(15) 0.0290(3) Uani 1 1 d . . . H14A H 0.2809 0.2170 0.5789 0.044 Uiso 1 1 calc R . . H14B H 0.3699 0.2721 0.6216 0.044 Uiso 1 1 calc R . . H14C H 0.3418 0.2269 0.7187 0.044 Uiso 1 1 calc R . . C15 C 0.28003(16) 0.16236(4) 0.17737(11) 0.0174(2) Uani 1 1 d . . . H15A H 0.2250 0.1839 0.2403 0.021 Uiso 1 1 calc R . . H15B H 0.1890 0.1622 0.1054 0.021 Uiso 1 1 calc R . . C16 C 0.46680(18) 0.18752(5) 0.14362(12) 0.0221(2) Uani 1 1 d . . . H16A H 0.5532 0.1910 0.2162 0.033 Uiso 1 1 calc R . . H16B H 0.4406 0.2222 0.1087 0.033 Uiso 1 1 calc R . . H16C H 0.5256 0.1654 0.0844 0.033 Uiso 1 1 calc R . . C17 C 0.18696(17) 0.05551(5) 0.03418(10) 0.0184(2) Uani 1 1 d . . . H17A H 0.0796 0.0800 0.0185 0.022 Uiso 1 1 calc R . . H17B H 0.1375 0.0195 0.0223 0.022 Uiso 1 1 calc R . . C18 C 0.33495(19) 0.06591(6) -0.05635(12) 0.0278(3) Uani 1 1 d . . . H18A H 0.3816 0.1019 -0.0467 0.042 Uiso 1 1 calc R . . H18B H 0.2775 0.0611 -0.1386 0.042 Uiso 1 1 calc R . . H18C H 0.4409 0.0415 -0.0420 0.042 Uiso 1 1 calc R . . C19 C 0.08527(17) 0.00895(5) 0.61650(11) 0.0185(2) Uani 1 1 d . . . H19 H 0.1436 0.0143 0.6953 0.022 Uiso 1 1 calc R . . C20 C 0.03569(17) 0.05075(5) 0.54712(11) 0.0187(2) Uani 1 1 d . . . H20 H 0.0583 0.0850 0.5779 0.022 Uiso 1 1 calc R . . C21 C -0.05149(16) 0.04387(5) 0.42645(10) 0.0170(2) Uani 1 1 d . . . C22 C -0.10044(16) 0.08625(5) 0.35385(11) 0.0191(2) Uani 1 1 d . . . C23 C -0.07015(18) 0.13916(5) 0.39346(12) 0.0225(2) Uani 1 1 d . . . C24 C -0.18197(17) 0.07936(5) 0.23229(11) 0.0215(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 Cu1 0.01181(9) 0.00976(9) 0.01180(9) 0.00010(6) 0.00047(6) -0.00006(6) N1 0.0142(4) 0.0106(4) 0.0140(4) 0.0002(3) 0.0005(3) -0.0006(3) N2 0.0138(4) 0.0113(4) 0.0135(4) 0.0005(3) 0.0006(3) 0.0002(3) N3 0.0286(6) 0.0274(6) 0.0359(6) 0.0007(5) 0.0055(5) 0.0006(5) N4 0.0205(5) 0.0373(6) 0.0235(5) 0.0052(5) 0.0006(4) 0.0039(4) C1 0.0147(5) 0.0132(4) 0.0144(4) -0.0007(4) 0.0017(4) -0.0016(4) C2 0.0173(5) 0.0137(4) 0.0155(5) -0.0027(4) 0.0019(4) -0.0026(4) C3 0.0162(5) 0.0123(4) 0.0180(5) -0.0023(4) 0.0018(4) -0.0014(4) C4 0.0138(4) 0.0112(4) 0.0164(5) -0.0007(4) 0.0020(4) -0.0004(3) C5 0.0155(5) 0.0109(4) 0.0175(5) 0.0011(4) 0.0012(4) 0.0005(3) C6 0.0128(4) 0.0122(4) 0.0153(4) 0.0019(4) 0.0014(4) 0.0007(3) C7 0.0127(4) 0.0151(5) 0.0157(5) 0.0033(4) 0.0004(4) 0.0006(4) C8 0.0130(4) 0.0159(5) 0.0152(5) 0.0027(4) -0.0002(4) -0.0008(4) C9 0.0132(4) 0.0141(4) 0.0131(4) 0.0009(4) 0.0009(3) -0.0004(4) C10 0.0156(5) 0.0147(4) 0.0138(4) -0.0003(4) 0.0011(4) -0.0020(4) C11 0.0288(6) 0.0167(5) 0.0164(5) -0.0028(4) -0.0014(4) -0.0041(4) C12 0.0280(7) 0.0302(7) 0.0264(6) 0.0030(5) -0.0087(5) -0.0084(5) C13 0.0205(5) 0.0114(4) 0.0240(5) -0.0020(4) 0.0004(4) -0.0006(4) C14 0.0247(6) 0.0181(5) 0.0443(8) -0.0054(5) 0.0028(6) 0.0040(5) C15 0.0178(5) 0.0148(5) 0.0195(5) 0.0050(4) 0.0007(4) 0.0020(4) C16 0.0228(6) 0.0165(5) 0.0275(6) 0.0050(4) 0.0056(5) -0.0011(4) C17 0.0182(5) 0.0208(5) 0.0156(5) 0.0029(4) -0.0030(4) -0.0022(4) C18 0.0229(6) 0.0449(8) 0.0158(5) -0.0038(5) 0.0023(4) 0.0015(5) C19 0.0170(5) 0.0238(5) 0.0147(5) -0.0012(4) 0.0004(4) -0.0018(4) C20 0.0174(5) 0.0226(5) 0.0160(5) -0.0017(4) 0.0015(4) -0.0017(4) C21 0.0133(5) 0.0222(5) 0.0157(5) 0.0002(4) 0.0025(4) -0.0005(4) C22 0.0145(5) 0.0244(5) 0.0188(5) 0.0021(4) 0.0033(4) 0.0007(4) C23 0.0181(5) 0.0265(6) 0.0233(6) 0.0042(5) 0.0038(4) 0.0019(4) C24 0.0155(5) 0.0269(6) 0.0222(6) 0.0054(5) 0.0028(4) 0.0034(4) _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 Cu1 N1 2.0013(9) . ? Cu1 N1 2.0013(9) 3_656 ? Cu1 N2 2.0058(9) 3_656 ? Cu1 N2 2.0058(9) . ? N1 C4 1.3725(13) . ? N1 C1 1.3784(14) . ? N2 C6 1.3757(13) . ? N2 C9 1.3773(14) . ? N3 C23 1.1489(18) . ? N4 C24 1.1473(17) . ? C1 C10 1.3827(15) 3_656 ? C1 C2 1.4516(15) . ? C2 C3 1.3643(16) . ? C2 C11 1.5022(16) . ? C3 C4 1.4436(15) . ? C3 C13 1.5006(15) . ? C4 C5 1.3883(15) . ? C5 C6 1.3829(15) . ? C6 C7 1.4452(15) . ? C7 C8 1.3680(15) . ? C7 C15 1.4989(15) . ? C8 C9 1.4473(15) . ? C8 C17 1.5016(15) . ? C9 C10 1.3907(15) . ? C10 C1 1.3827(15) 3_656 ? C11 C12 1.5339(19) . ? C13 C14 1.5304(18) . ? C15 C16 1.5381(17) . ? C17 C18 1.5233(17) . ? C19 C20 1.3488(17) . ? C19 C21 1.4463(16) 3_556 ? C20 C21 1.4447(16) . ? C21 C22 1.3797(17) . ? C21 C19 1.4463(16) 3_556 ? C22 C23 1.4337(18) . ? C22 C24 1.4396(17) . ? 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 Cu1 N1 180.00(3) . 3_656 ? N1 Cu1 N2 89.21(4) . 3_656 ? N1 Cu1 N2 90.79(4) 3_656 3_656 ? N1 Cu1 N2 90.79(4) . . ? N1 Cu1 N2 89.21(4) 3_656 . ? N2 Cu1 N2 180.0 3_656 . ? C4 N1 C1 105.45(9) . . ? C4 N1 Cu1 126.51(7) . . ? C1 N1 Cu1 128.04(7) . . ? C6 N2 C9 105.41(9) . . ? C6 N2 Cu1 126.56(7) . . ? C9 N2 Cu1 128.02(7) . . ? N1 C1 C10 124.91(10) . 3_656 ? N1 C1 C2 110.50(9) . . ? C10 C1 C2 124.57(10) 3_656 . ? C3 C2 C1 106.44(9) . . ? C3 C2 C11 126.86(10) . . ? C1 C2 C11 126.61(10) . . ? C2 C3 C4 106.66(9) . . ? C2 C3 C13 127.99(10) . . ? C4 C3 C13 125.35(10) . . ? N1 C4 C5 125.26(10) . . ? N1 C4 C3 110.95(10) . . ? C5 C4 C3 123.77(10) . . ? C6 C5 C4 125.83(10) . . ? N2 C6 C5 125.02(10) . . ? N2 C6 C7 110.86(9) . . ? C5 C6 C7 124.11(10) . . ? C8 C7 C6 106.50(9) . . ? C8 C7 C15 128.33(10) . . ? C6 C7 C15 125.12(10) . . ? C7 C8 C9 106.52(9) . . ? C7 C8 C17 127.17(10) . . ? C9 C8 C17 126.26(10) . . ? N2 C9 C10 124.66(10) . . ? N2 C9 C8 110.69(9) . . ? C10 C9 C8 124.65(10) . . ? C1 C10 C9 125.11(10) 3_656 . ? C2 C11 C12 111.62(10) . . ? C3 C13 C14 113.41(10) . . ? C7 C15 C16 113.04(9) . . ? C8 C17 C18 112.65(10) . . ? C20 C19 C21 121.43(11) . 3_556 ? C19 C20 C21 120.61(11) . . ? C22 C21 C20 121.23(11) . . ? C22 C21 C19 120.81(11) . 3_556 ? C20 C21 C19 117.96(10) . 3_556 ? C21 C22 C23 122.42(11) . . ? C21 C22 C24 121.21(12) . . ? C23 C22 C24 116.35(11) . . ? N3 C23 C22 179.18(14) . . ? N4 C24 C22 178.67(14) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.522 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.060 #===END data_ab026 _database_code_CSD 198538 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TCNQ$.!H2OEP _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H50 N8' _chemical_formula_weight 738.96 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.0582(7) _cell_length_b 25.645(2) _cell_length_c 11.0904(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.752(4) _cell_angle_gamma 90.00 _cell_volume 2003.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 903 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 31.2 _exptl_crystal_description needle _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9619 _exptl_absorpt_correction_T_max 0.9912 _exptl_absorpt_process_details 'SADABS 2.0 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18788 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.039 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 31.49 _reflns_number_total 6215 _reflns_number_gt 4498 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5, XP (Sheldrick, 1994)' _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^)+(0.0689P)^2^+0.3215P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6215 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 N1 N 0.56425(13) 0.06743(4) 0.59481(8) 0.01615(18) Uani 1 1 d . . . H1 H 0.5393 0.0376 0.5580 0.019 Uiso 0.50 1 calc PR . . N2 N 0.38914(13) 0.03940(4) 0.34997(8) 0.01587(18) Uani 1 1 d . . . H2 H 0.4335 0.0209 0.4124 0.019 Uiso 0.50 1 calc PR . . N3 N -0.05057(17) 0.18098(5) 0.42408(12) 0.0342(3) Uani 1 1 d . . . N4 N -0.25148(16) 0.07260(5) 0.13673(11) 0.0310(3) Uani 1 1 d . . . C1 C 0.64944(16) 0.07365(4) 0.70882(10) 0.0166(2) Uani 1 1 d . . . C2 C 0.66662(16) 0.12886(4) 0.73582(10) 0.0183(2) Uani 1 1 d . . . C3 C 0.58867(16) 0.15501(4) 0.63696(10) 0.0173(2) Uani 1 1 d . . . C4 C 0.52507(15) 0.11609(4) 0.54862(10) 0.0162(2) Uani 1 1 d . . . C5 C 0.44230(15) 0.12726(4) 0.43403(10) 0.0165(2) Uani 1 1 d . . . H5 H 0.4247 0.1632 0.4159 0.020 Uiso 1 1 calc R . . C6 C 0.38202(15) 0.09276(4) 0.34270(10) 0.0155(2) Uani 1 1 d . . . C7 C 0.30076(15) 0.10825(4) 0.22455(10) 0.0165(2) Uani 1 1 d . . . C8 C 0.25890(15) 0.06324(4) 0.16166(10) 0.0171(2) Uani 1 1 d . . . C9 C 0.31402(15) 0.02037(4) 0.24167(10) 0.0162(2) Uani 1 1 d . . . C10 C 0.29385(16) -0.03265(4) 0.21501(10) 0.0173(2) Uani 1 1 d . . . H10 H 0.2362 -0.0415 0.1379 0.021 Uiso 1 1 calc R . . C11 C 0.76050(19) 0.15263(5) 0.84831(11) 0.0237(3) Uani 1 1 d . . . H11A H 0.7591 0.1272 0.9154 0.028 Uiso 1 1 calc R . . H11B H 0.6877 0.1837 0.8711 0.028 Uiso 1 1 calc R . . C12 C 0.9659(2) 0.16853(6) 0.83013(13) 0.0310(3) Uani 1 1 d . . . H12A H 1.0401 0.1375 0.8120 0.046 Uiso 1 1 calc R . . H12B H 1.0212 0.1850 0.9040 0.046 Uiso 1 1 calc R . . H12C H 0.9679 0.1932 0.7627 0.046 Uiso 1 1 calc R . . C13 C 0.56972(17) 0.21282(4) 0.62018(11) 0.0216(2) Uani 1 1 d . . . H13A H 0.6038 0.2220 0.5376 0.026 Uiso 1 1 calc R . . H13B H 0.6610 0.2305 0.6781 0.026 Uiso 1 1 calc R . . C14 C 0.36985(19) 0.23321(5) 0.63852(15) 0.0329(3) Uani 1 1 d . . . H14A H 0.2782 0.2156 0.5821 0.049 Uiso 1 1 calc R . . H14B H 0.3654 0.2709 0.6235 0.049 Uiso 1 1 calc R . . H14C H 0.3379 0.2262 0.7217 0.049 Uiso 1 1 calc R . . C15 C 0.27732(17) 0.16336(4) 0.18136(11) 0.0201(2) Uani 1 1 d . . . H15A H 0.2252 0.1846 0.2460 0.024 Uiso 1 1 calc R . . H15B H 0.1844 0.1641 0.1106 0.024 Uiso 1 1 calc R . . C16 C 0.46400(18) 0.18785(5) 0.14611(12) 0.0256(3) Uani 1 1 d . . . H16A H 0.5516 0.1910 0.2180 0.038 Uiso 1 1 calc R . . H16B H 0.4386 0.2225 0.1114 0.038 Uiso 1 1 calc R . . H16C H 0.5212 0.1657 0.0864 0.038 Uiso 1 1 calc R . . C17 C 0.18008(17) 0.05850(5) 0.03319(10) 0.0224(2) Uani 1 1 d . . . H17A H 0.0783 0.0847 0.0181 0.027 Uiso 1 1 calc R . . H17B H 0.1225 0.0235 0.0211 0.027 Uiso 1 1 calc R . . C18 C 0.3294(2) 0.06629(7) -0.05771(12) 0.0351(3) Uani 1 1 d . . . H18A H 0.3869 0.1009 -0.0463 0.053 Uiso 1 1 calc R . . H18B H 0.2699 0.0635 -0.1398 0.053 Uiso 1 1 calc R . . H18C H 0.4278 0.0395 -0.0456 0.053 Uiso 1 1 calc R . . C19 C 0.09056(17) 0.00915(5) 0.61476(11) 0.0219(2) Uani 1 1 d . . . H19 H 0.1526 0.0147 0.6923 0.026 Uiso 1 1 calc R . . C20 C 0.03724(17) 0.05061(5) 0.54587(11) 0.0220(2) Uani 1 1 d . . . H20 H 0.0608 0.0849 0.5759 0.026 Uiso 1 1 calc R . . C21 C -0.05515(16) 0.04353(5) 0.42721(10) 0.0199(2) Uani 1 1 d . . . C22 C -0.10638(16) 0.08575(5) 0.35459(11) 0.0222(2) Uani 1 1 d . . . C23 C -0.07565(18) 0.13851(5) 0.39390(12) 0.0255(3) Uani 1 1 d . . . C24 C -0.18884(17) 0.07870(5) 0.23390(11) 0.0247(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 N1 0.0183(4) 0.0136(4) 0.0166(4) 0.0007(3) 0.0010(3) 0.0003(3) N2 0.0171(4) 0.0132(4) 0.0173(4) 0.0004(3) 0.0007(3) -0.0005(3) N3 0.0322(6) 0.0298(6) 0.0412(7) 0.0018(5) 0.0069(5) 0.0006(5) N4 0.0226(5) 0.0427(7) 0.0273(6) 0.0085(5) -0.0005(4) 0.0032(5) C1 0.0183(5) 0.0152(5) 0.0166(5) -0.0019(4) 0.0023(4) -0.0019(4) C2 0.0219(5) 0.0148(5) 0.0182(5) -0.0024(4) 0.0031(4) -0.0028(4) C3 0.0194(5) 0.0128(5) 0.0198(5) -0.0017(4) 0.0025(4) -0.0012(4) C4 0.0165(5) 0.0137(5) 0.0186(5) 0.0003(4) 0.0023(4) -0.0010(4) C5 0.0171(5) 0.0128(4) 0.0196(5) 0.0014(4) 0.0016(4) 0.0007(4) C6 0.0135(5) 0.0151(5) 0.0179(5) 0.0018(4) 0.0019(4) 0.0003(4) C7 0.0152(5) 0.0158(5) 0.0183(5) 0.0039(4) 0.0004(4) 0.0005(4) C8 0.0154(5) 0.0183(5) 0.0175(5) 0.0038(4) -0.0004(4) -0.0017(4) C9 0.0155(5) 0.0160(5) 0.0171(5) 0.0018(4) 0.0009(4) -0.0011(4) C10 0.0197(5) 0.0171(5) 0.0149(5) -0.0002(4) 0.0000(4) -0.0030(4) C11 0.0347(7) 0.0176(5) 0.0185(5) -0.0027(4) -0.0013(5) -0.0047(4) C12 0.0337(7) 0.0289(7) 0.0289(7) 0.0048(5) -0.0093(5) -0.0091(5) C13 0.0248(6) 0.0127(5) 0.0270(6) -0.0015(4) 0.0009(5) -0.0006(4) C14 0.0289(7) 0.0201(6) 0.0497(9) -0.0066(6) 0.0029(6) 0.0041(5) C15 0.0219(5) 0.0162(5) 0.0221(5) 0.0061(4) 0.0005(4) 0.0016(4) C16 0.0274(6) 0.0178(5) 0.0323(7) 0.0048(5) 0.0075(5) -0.0011(4) C17 0.0249(6) 0.0227(6) 0.0185(5) 0.0047(4) -0.0055(4) -0.0042(4) C18 0.0303(7) 0.0573(10) 0.0176(6) -0.0063(6) -0.0004(5) 0.0092(6) C19 0.0204(5) 0.0283(6) 0.0169(5) -0.0002(4) -0.0001(4) -0.0027(4) C20 0.0216(6) 0.0236(6) 0.0209(5) -0.0007(5) 0.0020(4) -0.0027(4) C21 0.0158(5) 0.0248(6) 0.0193(5) 0.0011(4) 0.0029(4) -0.0007(4) C22 0.0179(5) 0.0274(6) 0.0217(6) 0.0034(5) 0.0033(4) 0.0011(4) C23 0.0214(6) 0.0291(6) 0.0265(6) 0.0048(5) 0.0055(5) 0.0016(5) C24 0.0180(5) 0.0304(6) 0.0257(6) 0.0073(5) 0.0030(4) 0.0032(4) _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 N1 C4 1.3702(14) . ? N1 C1 1.3735(14) . ? N2 C6 1.3715(14) . ? N2 C9 1.3706(14) . ? N3 C23 1.1497(18) . ? N4 C24 1.1484(17) . ? C1 C10 1.3912(15) 3_656 ? C1 C2 1.4505(15) . ? C2 C3 1.3695(16) . ? C2 C11 1.5029(16) . ? C3 C4 1.4491(15) . ? C3 C13 1.4991(15) . ? C4 C5 1.3933(15) . ? C5 C6 1.3904(15) . ? C6 C7 1.4510(15) . ? C7 C8 1.3706(15) . ? C7 C15 1.4980(15) . ? C8 C9 1.4498(15) . ? C8 C17 1.5002(15) . ? C9 C10 1.3968(15) . ? C10 C1 1.3912(15) 3_656 ? C11 C12 1.5323(19) . ? C13 C14 1.5305(18) . ? C15 C16 1.5333(17) . ? C17 C18 1.5188(19) . ? C19 C20 1.3484(17) . ? C19 C21 1.4454(17) 3_556 ? C20 C21 1.4414(16) . ? C21 C22 1.3833(17) . ? C21 C19 1.4454(17) 3_556 ? C22 C23 1.4336(19) . ? C22 C24 1.4356(17) . ? 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 C4 N1 C1 107.69(9) . . ? C6 N2 C9 107.05(9) . . ? N1 C1 C10 124.22(10) . 3_656 ? N1 C1 C2 109.21(9) . . ? C10 C1 C2 126.56(10) 3_656 . ? C3 C2 C1 106.79(9) . . ? C3 C2 C11 126.74(10) . . ? C1 C2 C11 126.41(10) . . ? C2 C3 C4 107.13(10) . . ? C2 C3 C13 127.70(10) . . ? C4 C3 C13 125.18(10) . . ? N1 C4 C5 126.20(10) . . ? N1 C4 C3 109.18(9) . . ? C5 C4 C3 124.60(10) . . ? C6 C5 C4 128.58(10) . . ? N2 C6 C5 125.72(10) . . ? N2 C6 C7 109.69(9) . . ? C5 C6 C7 124.59(10) . . ? C8 C7 C6 106.76(9) . . ? C8 C7 C15 128.04(10) . . ? C6 C7 C15 125.16(10) . . ? C7 C8 C9 106.67(9) . . ? C7 C8 C17 127.28(10) . . ? C9 C8 C17 125.99(10) . . ? N2 C9 C10 124.08(10) . . ? N2 C9 C8 109.83(9) . . ? C10 C9 C8 126.09(10) . . ? C1 C10 C9 125.87(10) 3_656 . ? C2 C11 C12 111.61(11) . . ? C3 C13 C14 113.38(10) . . ? C7 C15 C16 112.91(9) . . ? C8 C17 C18 112.91(10) . . ? C20 C19 C21 121.24(11) . 3_556 ? C19 C20 C21 120.72(11) . . ? C22 C21 C20 121.23(11) . . ? C22 C21 C19 120.73(11) . 3_556 ? C20 C21 C19 118.04(10) . 3_556 ? C21 C22 C23 122.21(11) . . ? C21 C22 C24 121.25(12) . . ? C23 C22 C24 116.52(11) . . ? N3 C23 C22 179.21(14) . . ? N4 C24 C22 178.63(14) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 31.49 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.436 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.049 #===END data_ab028 _database_code_CSD 198539 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TNFM$.!Co(OEP) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H48 Co N9 O6' _chemical_formula_weight 953.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2190(10) _cell_length_b 22.5632(17) _cell_length_c 15.0954(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.873(2) _cell_angle_gamma 90.00 _cell_volume 4406.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 91(2) _cell_measurement_reflns_used 4158 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 30.4 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 0.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7124 _exptl_absorpt_correction_T_max 0.9602 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 91(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41106 _diffrn_reflns_av_R_equivalents 0.10 _diffrn_reflns_av_sigmaI/netI 0.10 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10084 _reflns_number_gt 4933 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5, XP (Sheldrick, 1994)' _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. There is disorder in the position of the nitro group N5, O1, O2. The atoms were split into two groups and their occupancies refined to 0.592(3):0.408(3) for sets A:B. ; _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^)+(0.0661P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10084 _refine_ls_number_parameters 652 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1277 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1390 _refine_ls_wR_factor_gt 0.1138 _refine_ls_goodness_of_fit_ref 0.895 _refine_ls_restrained_S_all 0.895 _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 Co1 Co 0.5000 0.5000 0.5000 0.01449(15) Uani 1 2 d S . . N1 N 0.5004(2) 0.41309(11) 0.48857(17) 0.0144(6) Uani 1 1 d . . . N2 N 0.4661(2) 0.50825(11) 0.36729(17) 0.0171(6) Uani 1 1 d . . . C1 C 0.5196(3) 0.37095(14) 0.5568(2) 0.0190(8) Uani 1 1 d . . . C2 C 0.5129(2) 0.31151(14) 0.5187(2) 0.0212(8) Uani 1 1 d . . . C3 C 0.4909(2) 0.31778(14) 0.4276(2) 0.0189(7) Uani 1 1 d . . . C4 C 0.4825(2) 0.38068(14) 0.4094(2) 0.0172(7) Uani 1 1 d . . . C5 C 0.4604(2) 0.40393(14) 0.3240(2) 0.0183(8) Uani 1 1 d . . . H5 H 0.4491 0.3768 0.2748 0.022 Uiso 1 1 calc R . . C6 C 0.4532(3) 0.46358(14) 0.3034(2) 0.0190(7) Uani 1 1 d . . . C7 C 0.4311(3) 0.48707(15) 0.2127(2) 0.0208(8) Uani 1 1 d . . . C8 C 0.4311(3) 0.54702(15) 0.2207(2) 0.0218(8) Uani 1 1 d . . . C9 C 0.4533(2) 0.55991(14) 0.3164(2) 0.0183(7) Uani 1 1 d . . . C10 C 0.4603(2) 0.61653(14) 0.3525(2) 0.0187(8) Uani 1 1 d . . . H10 H 0.4504 0.6490 0.3114 0.022 Uiso 1 1 calc R . . C11 C 0.5267(3) 0.25513(14) 0.5730(2) 0.0246(8) Uani 1 1 d . . . H11A H 0.5739 0.2628 0.6319 0.029 Uiso 1 1 calc R . . H11B H 0.5598 0.2251 0.5405 0.029 Uiso 1 1 calc R . . C12 C 0.4259(3) 0.23016(15) 0.5903(3) 0.0331(9) Uani 1 1 d . . . H12A H 0.3929 0.2595 0.6230 0.050 Uiso 1 1 calc R . . H12B H 0.4400 0.1939 0.6265 0.050 Uiso 1 1 calc R . . H12C H 0.3798 0.2209 0.5323 0.050 Uiso 1 1 calc R . . C13 C 0.4721(3) 0.27062(14) 0.3566(2) 0.0263(8) Uani 1 1 d . . . H13A H 0.5064 0.2335 0.3819 0.032 Uiso 1 1 calc R . . H13B H 0.5032 0.2829 0.3051 0.032 Uiso 1 1 calc R . . C14 C 0.3569(3) 0.25887(16) 0.3224(2) 0.0318(9) Uani 1 1 d . . . H14A H 0.3261 0.2460 0.3730 0.048 Uiso 1 1 calc R . . H14B H 0.3477 0.2278 0.2761 0.048 Uiso 1 1 calc R . . H14C H 0.3229 0.2953 0.2962 0.048 Uiso 1 1 calc R . . C15 C 0.4105(3) 0.45071(16) 0.1281(2) 0.0296(9) Uani 1 1 d . . . H15A H 0.4597 0.4171 0.1352 0.035 Uiso 1 1 calc R . . H15B H 0.4225 0.4753 0.0770 0.035 Uiso 1 1 calc R . . C16 C 0.2998(3) 0.42646(19) 0.1056(3) 0.0457(11) Uani 1 1 d . . . H16A H 0.2865 0.4034 0.1570 0.068 Uiso 1 1 calc R . . H16B H 0.2914 0.4010 0.0520 0.068 Uiso 1 1 calc R . . H16C H 0.2509 0.4595 0.0934 0.068 Uiso 1 1 calc R . . C17 C 0.4161(3) 0.59154(15) 0.1444(2) 0.0279(9) Uani 1 1 d . . . H17A H 0.3908 0.6292 0.1654 0.033 Uiso 1 1 calc R . . H17B H 0.3627 0.5766 0.0934 0.033 Uiso 1 1 calc R . . C18 C 0.5156(3) 0.60333(16) 0.1110(3) 0.0351(9) Uani 1 1 d . . . H18A H 0.5664 0.6221 0.1594 0.053 Uiso 1 1 calc R . . H18B H 0.5009 0.6297 0.0583 0.053 Uiso 1 1 calc R . . H18C H 0.5435 0.5658 0.0938 0.053 Uiso 1 1 calc R . . O1A O 0.3239(3) 0.53657(19) 0.8383(3) 0.0342(12) Uani 0.592(4) 1 d PD A 1 O2A O 0.3589(4) 0.6178(2) 0.7771(4) 0.0353(13) Uani 0.592(4) 1 d PD A 1 N5A N 0.3256(4) 0.5666(2) 0.7697(3) 0.0249(12) Uani 0.592(4) 1 d PD A 1 O1B O 0.2885(5) 0.7382(3) 0.7480(4) 0.044(2) Uani 0.408(4) 1 d PD A 2 O2B O 0.3475(6) 0.6498(4) 0.7570(5) 0.041(2) Uani 0.408(4) 1 d PD A 2 N5B N 0.2996(5) 0.6904(3) 0.7116(5) 0.0225(17) Uani 0.408(4) 1 d PD A 2 O3 O 0.29971(19) 0.35808(10) 0.67082(16) 0.0298(6) Uani 1 1 d . . . O4 O 0.2621(2) 0.35753(11) 0.52335(17) 0.0322(7) Uani 1 1 d . . . O5 O 0.1842(3) 0.80315(12) 0.35946(19) 0.0582(9) Uani 1 1 d . . . O6 O 0.2415(3) 0.84555(12) 0.4865(2) 0.0653(11) Uani 1 1 d . . . N6 N 0.2792(2) 0.38335(12) 0.5974(2) 0.0259(7) Uani 1 1 d . . . N7 N 0.1982(2) 0.45613(14) 0.2900(2) 0.0324(8) Uani 1 1 d . A . N8 N 0.1828(3) 0.63922(13) 0.2155(2) 0.0359(8) Uani 1 1 d . A . N9 N 0.2190(2) 0.80147(13) 0.4403(2) 0.0339(8) Uani 1 1 d . . . C37 C 0.2672(3) 0.68766(15) 0.6219(2) 0.0283(8) Uani 1 1 d . . . C38 C 0.2616(2) 0.63496(15) 0.5723(2) 0.0231(8) Uani 1 1 d . A . C39 C 0.2712(2) 0.57069(14) 0.5967(2) 0.0200(7) Uani 1 1 d . . . C40 C 0.2930(3) 0.54010(15) 0.6783(2) 0.0249(8) Uani 1 1 d . A . C41 C 0.2945(3) 0.47808(15) 0.6785(2) 0.0228(8) Uani 1 1 d . . . H41 H 0.3089 0.4568 0.7340 0.027 Uiso 1 1 calc R A . C42 C 0.2748(3) 0.44849(15) 0.5971(2) 0.0238(8) Uani 1 1 d . A . C43 C 0.2546(2) 0.47661(16) 0.5130(2) 0.0244(8) Uani 1 1 d . . . H43 H 0.2427 0.4549 0.4580 0.029 Uiso 1 1 calc R A . C44 C 0.2527(3) 0.53792(16) 0.5142(2) 0.0247(8) Uani 1 1 d . A . C45 C 0.2322(2) 0.57882(15) 0.4372(2) 0.0215(7) Uani 1 1 d . . . C46 C 0.2394(2) 0.63930(14) 0.4758(2) 0.0215(8) Uani 1 1 d . A . C47 C 0.2246(2) 0.69336(14) 0.4321(2) 0.0243(8) Uani 1 1 d . . . H47 H 0.2091 0.6960 0.3679 0.029 Uiso 1 1 calc R A . C48 C 0.2332(2) 0.74323(15) 0.4858(2) 0.0279(9) Uani 1 1 d . A . C49 C 0.2533(3) 0.74144(15) 0.5790(2) 0.0283(8) Uani 1 1 d . A . H49 H 0.2573 0.7771 0.6132 0.034 Uiso 1 1 calc R . . C50 C 0.2124(3) 0.56425(15) 0.3474(2) 0.0236(8) Uani 1 1 d . A . C51 C 0.2048(3) 0.50349(17) 0.3155(2) 0.0254(8) Uani 1 1 d . . . C52 C 0.1952(3) 0.60676(16) 0.2753(2) 0.0277(8) Uani 1 1 d . . . Co2 Co 0.0000 0.5000 0.5000 0.01284(15) Uani 1 2 d S . . N3 N -0.0024(2) 0.41345(11) 0.48443(17) 0.0157(6) Uani 1 1 d . . . N4 N 0.03078(19) 0.48955(11) 0.63213(16) 0.0140(6) Uani 1 1 d . . . C19 C -0.0185(2) 0.38231(13) 0.4043(2) 0.0165(7) Uani 1 1 d . . . C20 C -0.0100(2) 0.31902(14) 0.4200(2) 0.0170(7) Uani 1 1 d . . . C21 C 0.0099(2) 0.31129(13) 0.5113(2) 0.0172(7) Uani 1 1 d . . . C22 C 0.0152(2) 0.36970(13) 0.5504(2) 0.0150(7) Uani 1 1 d . . . C23 C 0.0348(2) 0.38109(13) 0.6423(2) 0.0163(7) Uani 1 1 d . . . H23 H 0.0437 0.3480 0.6821 0.020 Uiso 1 1 calc R . . C24 C 0.0424(2) 0.43701(14) 0.6807(2) 0.0161(7) Uani 1 1 d . . . C25 C 0.0659(2) 0.44739(13) 0.7771(2) 0.0165(7) Uani 1 1 d . . . C26 C 0.0714(2) 0.50746(14) 0.7879(2) 0.0184(7) Uani 1 1 d . . . C27 C 0.0486(2) 0.53283(13) 0.6983(2) 0.0151(7) Uani 1 1 d . . . C28 C 0.0423(2) 0.59304(13) 0.6809(2) 0.0176(7) Uani 1 1 d . . . H28 H 0.0554 0.6192 0.7313 0.021 Uiso 1 1 calc R . . C29 C -0.0131(3) 0.27333(14) 0.3476(2) 0.0223(8) Uani 1 1 d . . . H29A H -0.0697 0.2826 0.2955 0.027 Uiso 1 1 calc R . . H29B H -0.0269 0.2339 0.3712 0.027 Uiso 1 1 calc R . . C30 C 0.0905(3) 0.27225(15) 0.3166(2) 0.0314(9) Uani 1 1 d . . . H30A H 0.1023 0.3108 0.2905 0.047 Uiso 1 1 calc R . . H30B H 0.0889 0.2412 0.2709 0.047 Uiso 1 1 calc R . . H30C H 0.1466 0.2641 0.3687 0.047 Uiso 1 1 calc R . . C31 C 0.0273(3) 0.25386(14) 0.5618(2) 0.0210(8) Uani 1 1 d . . . H31A H -0.0130 0.2225 0.5244 0.025 Uiso 1 1 calc R . . H31B H 0.0003 0.2575 0.6181 0.025 Uiso 1 1 calc R . . C32 C 0.1402(3) 0.23460(15) 0.5866(2) 0.0280(8) Uani 1 1 d . . . H32A H 0.1684 0.2321 0.5315 0.042 Uiso 1 1 calc R . . H32B H 0.1449 0.1957 0.6160 0.042 Uiso 1 1 calc R . . H32C H 0.1798 0.2636 0.6280 0.042 Uiso 1 1 calc R . . C33 C 0.0865(3) 0.40073(14) 0.8490(2) 0.0207(8) Uani 1 1 d . . . H33A H 0.0384 0.3672 0.8312 0.025 Uiso 1 1 calc R . . H33B H 0.0734 0.4173 0.9063 0.025 Uiso 1 1 calc R . . C34 C 0.1981(3) 0.37794(15) 0.8645(2) 0.0257(8) Uani 1 1 d . . . H34A H 0.2119 0.3623 0.8076 0.039 Uiso 1 1 calc R . . H34B H 0.2077 0.3464 0.9101 0.039 Uiso 1 1 calc R . . H34C H 0.2459 0.4105 0.8858 0.039 Uiso 1 1 calc R . . C35 C 0.0962(3) 0.54223(15) 0.8747(2) 0.0256(8) Uani 1 1 d . . . H35A H 0.1400 0.5765 0.8664 0.031 Uiso 1 1 calc R . . H35B H 0.1365 0.5168 0.9228 0.031 Uiso 1 1 calc R . . C36 C -0.0002(3) 0.56481(18) 0.9059(2) 0.0402(10) Uani 1 1 d . . . H36A H -0.0412 0.5896 0.8583 0.060 Uiso 1 1 calc R . . H36B H 0.0208 0.5883 0.9612 0.060 Uiso 1 1 calc R . . H36C H -0.0419 0.5310 0.9180 0.060 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 0.0148(3) 0.0127(3) 0.0162(3) -0.0013(3) 0.0035(3) -0.0011(3) N1 0.0091(14) 0.0155(14) 0.0198(15) -0.0015(12) 0.0063(12) 0.0001(11) N2 0.0172(15) 0.0154(14) 0.0190(15) -0.0013(13) 0.0045(12) 0.0006(12) C1 0.0162(18) 0.0144(17) 0.0276(19) 0.0027(16) 0.0072(16) -0.0002(14) C2 0.0149(18) 0.0145(17) 0.035(2) -0.0006(15) 0.0067(17) -0.0004(14) C3 0.0137(18) 0.0151(17) 0.0284(19) -0.0034(15) 0.0055(16) -0.0027(13) C4 0.0125(18) 0.0165(17) 0.0240(19) -0.0041(15) 0.0071(16) -0.0004(13) C5 0.0169(19) 0.0190(18) 0.0193(18) -0.0070(15) 0.0041(15) -0.0025(14) C6 0.0139(18) 0.0226(18) 0.0210(18) -0.0055(15) 0.0045(15) -0.0017(14) C7 0.0154(18) 0.030(2) 0.0172(18) -0.0017(15) 0.0030(15) -0.0002(14) C8 0.022(2) 0.0254(19) 0.0192(18) 0.0019(16) 0.0068(16) 0.0010(15) C9 0.0125(18) 0.0218(18) 0.0209(18) 0.0013(16) 0.0038(15) -0.0007(14) C10 0.0162(18) 0.0192(18) 0.0210(18) 0.0058(15) 0.0042(16) 0.0014(14) C11 0.025(2) 0.0151(17) 0.034(2) 0.0020(16) 0.0067(17) 0.0015(14) C12 0.035(2) 0.0250(19) 0.042(2) 0.0106(17) 0.0139(19) 0.0000(16) C13 0.028(2) 0.0172(17) 0.034(2) -0.0055(16) 0.0067(17) -0.0003(15) C14 0.033(2) 0.0273(19) 0.035(2) -0.0115(17) 0.0061(18) -0.0107(16) C15 0.040(2) 0.029(2) 0.0185(19) -0.0014(16) 0.0053(18) -0.0003(17) C16 0.045(3) 0.056(3) 0.031(2) -0.016(2) -0.002(2) -0.008(2) C17 0.035(2) 0.027(2) 0.0210(19) 0.0045(16) 0.0039(18) 0.0030(16) C18 0.048(3) 0.028(2) 0.033(2) 0.0070(17) 0.016(2) 0.0049(18) O1A 0.035(3) 0.042(3) 0.029(2) -0.002(2) 0.014(2) 0.002(2) O2A 0.040(3) 0.026(3) 0.038(3) -0.006(3) 0.005(2) 0.001(3) N5A 0.021(3) 0.028(3) 0.029(3) 0.003(2) 0.013(2) 0.002(2) O1B 0.051(5) 0.038(4) 0.035(4) -0.009(3) -0.008(3) 0.014(3) O2B 0.051(5) 0.042(5) 0.030(4) -0.010(4) 0.005(4) 0.002(5) N5B 0.026(4) 0.016(3) 0.027(4) -0.004(3) 0.008(3) 0.003(3) O3 0.0352(15) 0.0251(13) 0.0301(14) 0.0098(11) 0.0091(12) 0.0047(11) O4 0.0373(17) 0.0270(14) 0.0314(15) 0.0009(12) 0.0049(14) -0.0004(12) O5 0.089(3) 0.0311(16) 0.0415(17) 0.0103(14) -0.0178(18) -0.0121(16) O6 0.097(3) 0.0185(14) 0.065(2) -0.0020(15) -0.020(2) -0.0042(16) N6 0.0208(16) 0.0252(16) 0.0336(18) 0.0060(15) 0.0099(14) 0.0011(13) N7 0.0347(19) 0.0301(18) 0.0311(18) -0.0013(15) 0.0041(15) 0.0008(15) N8 0.041(2) 0.0311(17) 0.0370(19) 0.0100(16) 0.0120(17) 0.0044(15) N9 0.0288(18) 0.0234(17) 0.046(2) 0.0033(16) -0.0010(16) -0.0011(13) C37 0.0180(19) 0.0255(19) 0.038(2) -0.0017(17) -0.0013(17) -0.0010(15) C38 0.0135(17) 0.0254(18) 0.031(2) 0.0024(16) 0.0055(15) 0.0001(14) C39 0.0105(16) 0.0220(17) 0.0291(18) 0.0016(16) 0.0079(15) 0.0015(13) C40 0.0210(19) 0.0237(19) 0.031(2) 0.0038(16) 0.0085(17) 0.0021(15) C41 0.0198(19) 0.0245(19) 0.0262(19) 0.0055(16) 0.0097(16) 0.0027(14) C42 0.0179(18) 0.0267(19) 0.0289(19) 0.0051(17) 0.0094(16) 0.0009(14) C43 0.0153(18) 0.0255(17) 0.032(2) 0.0055(16) 0.0049(17) -0.0013(14) C44 0.0159(18) 0.0260(18) 0.032(2) 0.0052(16) 0.0044(16) 0.0004(15) C45 0.0131(17) 0.0210(17) 0.0322(19) 0.0066(16) 0.0084(15) 0.0004(13) C46 0.0133(18) 0.0217(17) 0.031(2) 0.0003(15) 0.0076(17) -0.0012(14) C47 0.0159(18) 0.0256(18) 0.0320(19) 0.0037(16) 0.0062(15) -0.0027(14) C48 0.018(2) 0.0190(17) 0.045(2) 0.0082(16) 0.0010(17) -0.0001(13) C49 0.0212(19) 0.0223(18) 0.039(2) -0.0045(17) 0.0000(17) -0.0022(14) C50 0.0183(18) 0.0232(18) 0.031(2) 0.0048(16) 0.0085(16) -0.0009(14) C51 0.0208(18) 0.030(2) 0.0255(19) 0.0042(18) 0.0042(15) 0.0025(16) C52 0.023(2) 0.0262(19) 0.034(2) 0.0011(17) 0.0066(17) -0.0003(15) Co2 0.0137(3) 0.0117(3) 0.0131(3) -0.0001(3) 0.0028(3) -0.0001(3) N3 0.0144(15) 0.0148(14) 0.0186(15) 0.0003(12) 0.0049(13) -0.0018(11) N4 0.0161(15) 0.0135(14) 0.0131(14) -0.0012(11) 0.0043(12) -0.0018(11) C19 0.0159(19) 0.0136(16) 0.0207(18) -0.0014(15) 0.0051(15) 0.0005(13) C20 0.0159(18) 0.0145(17) 0.0203(18) -0.0031(14) 0.0031(15) 0.0000(13) C21 0.0156(18) 0.0116(15) 0.0249(19) -0.0014(15) 0.0051(15) 0.0008(14) C22 0.0107(17) 0.0139(16) 0.0204(18) 0.0010(14) 0.0034(15) 0.0006(13) C23 0.0148(18) 0.0139(16) 0.0217(18) 0.0024(15) 0.0072(15) 0.0004(13) C24 0.0151(18) 0.0177(17) 0.0159(17) 0.0029(15) 0.0039(14) 0.0016(14) C25 0.0141(17) 0.0186(17) 0.0173(17) 0.0000(14) 0.0046(14) -0.0005(13) C26 0.0193(18) 0.0201(18) 0.0156(17) 0.0014(15) 0.0032(15) 0.0023(14) C27 0.0138(17) 0.0176(17) 0.0145(17) -0.0040(14) 0.0048(14) 0.0018(13) C28 0.0181(19) 0.0169(17) 0.0178(18) -0.0036(15) 0.0041(15) 0.0003(14) C29 0.030(2) 0.0142(16) 0.0200(18) -0.0052(14) -0.0022(16) 0.0012(14) C30 0.039(2) 0.0259(19) 0.030(2) -0.0067(16) 0.0089(18) 0.0072(16) C31 0.0235(19) 0.0154(17) 0.0228(18) 0.0004(15) 0.0020(16) 0.0011(14) C32 0.029(2) 0.0225(18) 0.033(2) 0.0043(16) 0.0082(17) 0.0081(15) C33 0.027(2) 0.0186(17) 0.0157(17) 0.0024(14) 0.0035(16) -0.0010(14) C34 0.029(2) 0.0269(18) 0.0201(17) 0.0055(15) 0.0020(16) 0.0023(15) C35 0.042(2) 0.0204(17) 0.0136(17) -0.0025(15) 0.0045(17) 0.0018(16) C36 0.053(3) 0.042(2) 0.027(2) -0.0064(19) 0.012(2) 0.013(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 Co1 N1 1.969(2) . ? Co1 N1 1.969(2) 3_666 ? Co1 N2 1.970(3) . ? Co1 N2 1.970(3) 3_666 ? N1 C4 1.379(4) . ? N1 C1 1.386(4) . ? N2 C6 1.382(4) . ? N2 C9 1.387(4) . ? C1 C10 1.371(5) 3_666 ? C1 C2 1.454(4) . ? C2 C3 1.353(5) . ? C2 C11 1.504(4) . ? C3 C4 1.446(4) . ? C3 C13 1.495(4) . ? C4 C5 1.367(5) . ? C5 C6 1.380(4) . ? C6 C7 1.441(5) . ? C7 C8 1.358(5) . ? C7 C15 1.495(4) . ? C8 C9 1.444(4) . ? C8 C17 1.510(4) . ? C9 C10 1.384(4) . ? C10 C1 1.371(5) 3_666 ? C11 C12 1.518(5) . ? C13 C14 1.528(5) . ? C15 C16 1.532(5) . ? C17 C18 1.526(5) . ? O1A N5A 1.242(6) . ? O2A N5A 1.234(6) . ? N5A C40 1.483(6) . ? O1B N5B 1.233(8) . ? O2B N5B 1.237(9) . ? N5B C37 1.335(7) . ? O3 N6 1.226(3) . ? O4 N6 1.239(4) . ? O5 N9 1.213(4) . ? O6 N9 1.216(4) . ? N6 C42 1.471(4) . ? N7 C51 1.134(4) . ? N8 C52 1.147(4) . ? N9 C48 1.477(4) . ? C37 C49 1.370(5) . ? C37 C38 1.399(5) . ? C38 C46 1.429(5) . ? C38 C39 1.495(4) . ? C39 C40 1.390(5) . ? C39 C44 1.426(5) . ? C40 C41 1.400(5) . ? C41 C42 1.375(5) . ? C42 C43 1.395(5) . ? C43 C44 1.384(5) . ? C44 C45 1.465(5) . ? C45 C50 1.366(5) . ? C45 C46 1.479(5) . ? C46 C47 1.381(4) . ? C47 C48 1.378(5) . ? C48 C49 1.378(5) . ? C50 C52 1.434(5) . ? C50 C51 1.450(5) . ? Co2 N3 1.966(2) . ? Co2 N3 1.966(2) 3_566 ? Co2 N4 1.966(2) 3_566 ? Co2 N4 1.966(2) . ? N3 C19 1.377(4) . ? N3 C22 1.387(4) . ? N4 C27 1.382(4) . ? N4 C24 1.386(4) . ? C19 C28 1.378(4) 3_566 ? C19 C20 1.448(4) . ? C20 C21 1.361(4) . ? C20 C29 1.496(4) . ? C21 C22 1.440(4) . ? C21 C31 1.497(4) . ? C22 C23 1.382(4) . ? C23 C24 1.383(4) . ? C24 C25 1.444(4) . ? C25 C26 1.365(4) . ? C25 C33 1.496(4) . ? C26 C27 1.443(4) . ? C26 C35 1.504(4) . ? C27 C28 1.383(4) . ? C28 C19 1.378(4) 3_566 ? C29 C30 1.537(5) . ? C31 C32 1.525(4) . ? C33 C34 1.533(5) . ? C35 C36 1.533(5) . ? 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 Co1 N1 180.00(15) . 3_666 ? N1 Co1 N2 90.53(10) . . ? N1 Co1 N2 89.47(10) 3_666 . ? N1 Co1 N2 89.47(10) . 3_666 ? N1 Co1 N2 90.53(10) 3_666 3_666 ? N2 Co1 N2 180.000(1) . 3_666 ? C4 N1 C1 104.6(2) . . ? C4 N1 Co1 126.9(2) . . ? C1 N1 Co1 128.4(2) . . ? C6 N2 C9 104.0(3) . . ? C6 N2 Co1 127.7(2) . . ? C9 N2 Co1 128.3(2) . . ? C10 C1 N1 124.7(3) 3_666 . ? C10 C1 C2 124.6(3) 3_666 . ? N1 C1 C2 110.6(3) . . ? C3 C2 C1 106.7(3) . . ? C3 C2 C11 128.2(3) . . ? C1 C2 C11 125.0(3) . . ? C2 C3 C4 106.7(3) . . ? C2 C3 C13 128.6(3) . . ? C4 C3 C13 124.6(3) . . ? C5 C4 N1 125.4(3) . . ? C5 C4 C3 123.3(3) . . ? N1 C4 C3 111.3(3) . . ? C4 C5 C6 125.3(3) . . ? C5 C6 N2 124.1(3) . . ? C5 C6 C7 124.3(3) . . ? N2 C6 C7 111.5(3) . . ? C8 C7 C6 106.6(3) . . ? C8 C7 C15 128.2(3) . . ? C6 C7 C15 125.1(3) . . ? C7 C8 C9 106.6(3) . . ? C7 C8 C17 126.7(3) . . ? C9 C8 C17 126.6(3) . . ? C10 C9 N2 124.5(3) . . ? C10 C9 C8 124.3(3) . . ? N2 C9 C8 111.2(3) . . ? C1 C10 C9 124.5(3) 3_666 . ? C2 C11 C12 113.2(3) . . ? C3 C13 C14 111.9(3) . . ? C7 C15 C16 112.5(3) . . ? C8 C17 C18 112.4(3) . . ? O2A N5A O1A 120.2(5) . . ? O2A N5A C40 119.5(5) . . ? O1A N5A C40 120.3(4) . . ? O2B N5B O1B 119.7(7) . . ? O2B N5B C37 123.2(6) . . ? O1B N5B C37 116.7(6) . . ? O3 N6 O4 124.2(3) . . ? O3 N6 C42 117.9(3) . . ? O4 N6 C42 117.9(3) . . ? O5 N9 O6 123.3(3) . . ? O5 N9 C48 118.8(3) . . ? O6 N9 C48 118.0(3) . . ? N5B C37 C49 114.9(4) . . ? N5B C37 C38 123.6(4) . . ? C49 C37 C38 120.9(3) . . ? C37 C38 C46 117.7(3) . . ? C37 C38 C39 134.5(3) . . ? C46 C38 C39 107.9(3) . . ? C40 C39 C44 118.9(3) . . ? C40 C39 C38 133.8(3) . . ? C44 C39 C38 107.3(3) . . ? C39 C40 C41 120.0(3) . . ? C39 C40 N5A 126.3(3) . . ? C41 C40 N5A 113.5(4) . . ? C42 C41 C40 118.9(3) . . ? C41 C42 C43 123.9(3) . . ? C41 C42 N6 118.9(3) . . ? C43 C42 N6 117.2(3) . . ? C44 C43 C42 116.3(3) . . ? C43 C44 C39 121.9(3) . . ? C43 C44 C45 128.4(4) . . ? C39 C44 C45 109.7(3) . . ? C50 C45 C44 127.0(3) . . ? C50 C45 C46 126.6(3) . . ? C44 C45 C46 106.4(3) . . ? C47 C46 C38 121.8(3) . . ? C47 C46 C45 129.4(3) . . ? C38 C46 C45 108.7(3) . . ? C48 C47 C46 117.0(3) . . ? C49 C48 C47 123.5(3) . . ? C49 C48 N9 118.7(3) . . ? C47 C48 N9 117.8(3) . . ? C37 C49 C48 119.1(3) . . ? C45 C50 C52 124.1(3) . . ? C45 C50 C51 122.9(3) . . ? C52 C50 C51 113.0(3) . . ? N7 C51 C50 179.4(4) . . ? N8 C52 C50 177.4(4) . . ? N3 Co2 N3 180.00(15) . 3_566 ? N3 Co2 N4 90.17(10) . 3_566 ? N3 Co2 N4 89.83(10) 3_566 3_566 ? N3 Co2 N4 89.83(10) . . ? N3 Co2 N4 90.17(10) 3_566 . ? N4 Co2 N4 180.000(1) 3_566 . ? C19 N3 C22 103.9(2) . . ? C19 N3 Co2 127.4(2) . . ? C22 N3 Co2 128.7(2) . . ? C27 N4 C24 103.8(2) . . ? C27 N4 Co2 128.1(2) . . ? C24 N4 Co2 128.1(2) . . ? N3 C19 C28 125.4(3) . 3_566 ? N3 C19 C20 111.5(3) . . ? C28 C19 C20 123.1(3) 3_566 . ? C21 C20 C19 106.5(3) . . ? C21 C20 C29 128.5(3) . . ? C19 C20 C29 124.8(3) . . ? C20 C21 C22 106.3(3) . . ? C20 C21 C31 127.2(3) . . ? C22 C21 C31 126.5(3) . . ? C23 C22 N3 123.9(3) . . ? C23 C22 C21 124.4(3) . . ? N3 C22 C21 111.7(3) . . ? C22 C23 C24 124.9(3) . . ? C23 C24 N4 124.6(3) . . ? C23 C24 C25 123.5(3) . . ? N4 C24 C25 111.8(3) . . ? C26 C25 C24 106.1(3) . . ? C26 C25 C33 127.9(3) . . ? C24 C25 C33 125.9(3) . . ? C25 C26 C27 106.6(3) . . ? C25 C26 C35 128.2(3) . . ? C27 C26 C35 125.2(3) . . ? N4 C27 C28 124.2(3) . . ? N4 C27 C26 111.7(3) . . ? C28 C27 C26 124.1(3) . . ? C19 C28 C27 124.5(3) 3_566 . ? C20 C29 C30 109.9(3) . . ? C21 C31 C32 114.3(3) . . ? C25 C33 C34 111.9(3) . . ? C26 C35 C36 113.3(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.512 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.074 #===END data_dp07 _database_code_CSD 213236 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2{Zn(OEP)}.TCNQ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H92 N12 Zn2' _chemical_formula_weight 1400.44 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' 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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.241(8) _cell_length_b 14.168(7) _cell_length_c 21.651(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.31(2) _cell_angle_gamma 90.00 _cell_volume 3448(4) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 996 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 20 _exptl_crystal_description rod _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6542 _exptl_absorpt_correction_T_max 0.9251 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44485 _diffrn_reflns_av_R_equivalents 0.097 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8404 _reflns_number_gt 7871 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART 5.054 (Bruker, 2002)' _computing_cell_refinement 'SAINT 6.22 (Bruker, 2002)' _computing_data_reduction 'SAINT 6.22 (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0451P)^2^+1.8093P] 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 8404 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _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 Zn1 Zn 0.30604(2) 0.455031(15) 0.492239(12) 0.01032(6) Uani 1 1 d . . . N1 N 0.21456(15) 0.33093(11) 0.49261(8) 0.0103(3) Uani 1 1 d . . . N2 N 0.33256(17) 0.44372(12) 0.58469(8) 0.0107(4) Uani 1 1 d . . . N3 N 0.38609(16) 0.58412(11) 0.49302(9) 0.0109(3) Uani 1 1 d . . . N4 N 0.26270(17) 0.47319(12) 0.40141(9) 0.0105(4) Uani 1 1 d . . . C1 C 0.1995(2) 0.27166(14) 0.54198(9) 0.0111(4) Uani 1 1 d . . . C2 C 0.1409(2) 0.18588(15) 0.52252(10) 0.0122(4) Uani 1 1 d . . . C3 C 0.1179(2) 0.19534(15) 0.46073(10) 0.0117(4) Uani 1 1 d . . . C4 C 0.1639(2) 0.28662(15) 0.44265(10) 0.0117(4) Uani 1 1 d . . . C5 C 0.15556(19) 0.32584(15) 0.38372(10) 0.0116(4) Uani 1 1 d . . . H5A H 0.1150 0.2894 0.3534 0.014 Uiso 1 1 calc R . . C6 C 0.2000(2) 0.41240(14) 0.36458(9) 0.0111(4) Uani 1 1 d . . . C7 C 0.1885(2) 0.45016(15) 0.30265(9) 0.0131(4) Uani 1 1 d . . . C8 C 0.2488(2) 0.53326(16) 0.30208(10) 0.0131(4) Uani 1 1 d . . . C9 C 0.2934(2) 0.54792(14) 0.36459(9) 0.0117(4) Uani 1 1 d . . . C10 C 0.3567(2) 0.62663(15) 0.38465(10) 0.0116(4) Uani 1 1 d . . . H10A H 0.3729 0.6734 0.3544 0.014 Uiso 1 1 calc R . . C11 C 0.3989(2) 0.64450(15) 0.44407(10) 0.0111(4) Uani 1 1 d . . . C12 C 0.46266(19) 0.72790(16) 0.46337(10) 0.0114(4) Uani 1 1 d . . . C13 C 0.4894(2) 0.71711(15) 0.52470(10) 0.0108(4) Uani 1 1 d . . . C14 C 0.4398(2) 0.62634(15) 0.54239(10) 0.0115(4) Uani 1 1 d . . . C15 C 0.4431(2) 0.59010(15) 0.60209(10) 0.0120(4) Uani 1 1 d . . . H15A H 0.4860 0.6255 0.6321 0.014 Uiso 1 1 calc R . . C16 C 0.3898(2) 0.50694(15) 0.62215(9) 0.0105(4) Uani 1 1 d . . . C17 C 0.3854(2) 0.47649(16) 0.68607(10) 0.0132(4) Uani 1 1 d . . . C18 C 0.3241(2) 0.39388(14) 0.68659(9) 0.0129(4) Uani 1 1 d . . . C19 C 0.2929(2) 0.37343(14) 0.62271(9) 0.0109(4) Uani 1 1 d . . . C20 C 0.23286(19) 0.29308(15) 0.60263(10) 0.0124(4) Uani 1 1 d . . . H20A H 0.2125 0.2481 0.6334 0.015 Uiso 1 1 calc R . . C21 C 0.1124(2) 0.10293(15) 0.56303(10) 0.0144(4) Uani 1 1 d . . . H21A H 0.0501 0.0645 0.5426 0.017 Uiso 1 1 calc R . . H21B H 0.0795 0.1264 0.6025 0.017 Uiso 1 1 calc R . . C22 C 0.2194(2) 0.03996(16) 0.57710(11) 0.0185(5) Uani 1 1 d . . . H22A H 0.1930 -0.0160 0.5998 0.028 Uiso 1 1 calc R . . H22B H 0.2772 0.0750 0.6022 0.028 Uiso 1 1 calc R . . H22C H 0.2566 0.0205 0.5383 0.028 Uiso 1 1 calc R . . C23 C 0.0616(2) 0.12459(16) 0.41818(11) 0.0153(4) Uani 1 1 d . . . H23A H 0.0288 0.1579 0.3817 0.018 Uiso 1 1 calc R . . H23B H -0.0055 0.0937 0.4397 0.018 Uiso 1 1 calc R . . C24 C 0.1486(3) 0.04913(18) 0.39656(13) 0.0234(5) Uani 1 1 d . . . H24A H 0.1089 0.0074 0.3668 0.035 Uiso 1 1 calc R . . H24B H 0.1760 0.0121 0.4321 0.035 Uiso 1 1 calc R . . H24C H 0.2170 0.0794 0.3768 0.035 Uiso 1 1 calc R . . C25 C 0.1180(2) 0.40586(16) 0.25111(10) 0.0159(4) Uani 1 1 d . . . H25A H 0.1366 0.3376 0.2494 0.019 Uiso 1 1 calc R . . H25B H 0.1426 0.4344 0.2114 0.019 Uiso 1 1 calc R . . C26 C -0.0153(2) 0.41826(19) 0.25859(12) 0.0210(5) Uani 1 1 d . . . H26A H -0.0567 0.3889 0.2236 0.031 Uiso 1 1 calc R . . H26B H -0.0345 0.4857 0.2599 0.031 Uiso 1 1 calc R . . H26C H -0.0407 0.3882 0.2971 0.031 Uiso 1 1 calc R . . C27 C 0.2682(2) 0.59746(17) 0.24759(10) 0.0186(5) Uani 1 1 d . . . H27A H 0.2938 0.5588 0.2120 0.022 Uiso 1 1 calc R . . H27B H 0.3338 0.6416 0.2577 0.022 Uiso 1 1 calc R . . C28 C 0.1598(3) 0.6544(2) 0.22865(12) 0.0294(6) Uani 1 1 d . . . H28A H 0.1794 0.6940 0.1930 0.044 Uiso 1 1 calc R . . H28B H 0.1351 0.6945 0.2631 0.044 Uiso 1 1 calc R . . H28C H 0.0948 0.6114 0.2176 0.044 Uiso 1 1 calc R . . C29 C 0.4887(2) 0.81216(16) 0.42398(10) 0.0135(4) Uani 1 1 d . . . H29A H 0.5010 0.7912 0.3809 0.016 Uiso 1 1 calc R . . H29B H 0.5633 0.8420 0.4386 0.016 Uiso 1 1 calc R . . C30 C 0.3884(3) 0.88534(18) 0.42529(12) 0.0249(5) Uani 1 1 d . . . H30A H 0.4104 0.9397 0.3999 0.037 Uiso 1 1 calc R . . H30B H 0.3754 0.9060 0.4679 0.037 Uiso 1 1 calc R . . H30C H 0.3151 0.8571 0.4089 0.037 Uiso 1 1 calc R . . C31 C 0.5529(2) 0.78361(15) 0.56700(10) 0.0136(4) Uani 1 1 d . . . H31A H 0.6046 0.8252 0.5420 0.016 Uiso 1 1 calc R . . H31B H 0.6048 0.7467 0.5950 0.016 Uiso 1 1 calc R . . C32 C 0.4705(2) 0.84514(17) 0.60593(12) 0.0200(5) Uani 1 1 d . . . H32A H 0.5182 0.8890 0.6308 0.030 Uiso 1 1 calc R . . H32B H 0.4233 0.8049 0.6333 0.030 Uiso 1 1 calc R . . H32C H 0.4171 0.8809 0.5787 0.030 Uiso 1 1 calc R . . C33 C 0.4337(2) 0.53233(16) 0.73945(10) 0.0154(4) Uani 1 1 d . . . H33A H 0.5122 0.5588 0.7282 0.018 Uiso 1 1 calc R . . H33B H 0.4454 0.4899 0.7753 0.018 Uiso 1 1 calc R . . C34 C 0.3500(2) 0.61278(18) 0.75751(12) 0.0215(5) Uani 1 1 d . . . H34A H 0.3850 0.6485 0.7919 0.032 Uiso 1 1 calc R . . H34B H 0.2732 0.5866 0.7702 0.032 Uiso 1 1 calc R . . H34C H 0.3381 0.6548 0.7221 0.032 Uiso 1 1 calc R . . C35 C 0.2932(2) 0.33456(15) 0.74138(9) 0.0160(4) Uani 1 1 d . . . H35A H 0.2104 0.3117 0.7366 0.019 Uiso 1 1 calc R . . H35B H 0.2967 0.3743 0.7789 0.019 Uiso 1 1 calc R . . C36 C 0.3753(2) 0.24984(19) 0.75020(11) 0.0186(4) Uani 1 1 d . . . H36A H 0.3508 0.2143 0.7868 0.028 Uiso 1 1 calc R . . H36B H 0.4574 0.2718 0.7557 0.028 Uiso 1 1 calc R . . H36C H 0.3705 0.2090 0.7138 0.028 Uiso 1 1 calc R . . N5 N 0.2020(2) 0.77169(16) 0.56378(12) 0.0316(5) Uani 1 1 d . . . N6 N 0.0899(2) 0.75843(18) 0.37104(12) 0.0330(6) Uani 1 1 d . . . C38 C 0.0083(2) 0.46298(17) 0.56010(11) 0.0171(5) Uani 1 1 d . . . H38A H 0.0123 0.4373 0.6006 0.021 Uiso 1 1 calc R . . C37 C 0.0589(2) 0.54675(17) 0.54885(11) 0.0174(5) Uani 1 1 d . . . H37A H 0.0997 0.5788 0.5811 0.021 Uiso 1 1 calc R . . C39 C 0.0522(2) 0.58898(16) 0.48799(12) 0.0171(4) Uani 1 1 d . . . C40 C 0.1012(2) 0.67599(17) 0.47698(11) 0.0188(5) Uani 1 1 d . . . C41 C 0.1582(2) 0.72919(18) 0.52490(12) 0.0218(5) Uani 1 1 d . . . C42 C 0.0954(2) 0.72091(18) 0.41763(13) 0.0237(5) 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 Zn1 0.01362(11) 0.00776(10) 0.00955(10) 0.00001(8) -0.00153(10) -0.00080(9) N1 0.0138(8) 0.0068(7) 0.0104(7) -0.0001(6) -0.0011(7) 0.0003(6) N2 0.0127(9) 0.0060(8) 0.0135(8) -0.0008(6) -0.0007(6) -0.0010(7) N3 0.0144(8) 0.0084(7) 0.0100(8) 0.0006(7) -0.0006(7) 0.0018(6) N4 0.0127(9) 0.0056(8) 0.0131(8) -0.0002(6) 0.0003(7) -0.0013(6) C1 0.0124(10) 0.0072(9) 0.0136(9) -0.0001(7) 0.0002(9) 0.0002(9) C2 0.0107(10) 0.0099(10) 0.0159(11) 0.0001(7) 0.0001(8) -0.0004(8) C3 0.0104(10) 0.0095(10) 0.0150(10) -0.0017(8) -0.0020(8) -0.0009(8) C4 0.0128(11) 0.0109(10) 0.0115(9) -0.0010(7) 0.0001(7) 0.0008(8) C5 0.0133(10) 0.0108(10) 0.0107(9) -0.0017(7) -0.0024(7) 0.0011(8) C6 0.0131(10) 0.0097(9) 0.0105(8) -0.0020(7) -0.0012(8) 0.0016(9) C7 0.0162(10) 0.0122(9) 0.0109(8) -0.0006(7) -0.0006(9) 0.0025(9) C8 0.0164(11) 0.0129(10) 0.0099(9) -0.0008(8) -0.0011(8) 0.0023(8) C9 0.0122(10) 0.0130(9) 0.0098(8) 0.0012(7) 0.0000(8) 0.0017(8) C10 0.0135(10) 0.0103(9) 0.0109(9) 0.0015(7) 0.0010(8) 0.0010(8) C11 0.0120(10) 0.0066(9) 0.0148(10) 0.0002(7) 0.0018(8) 0.0009(8) C12 0.0097(10) 0.0099(10) 0.0145(10) 0.0006(8) 0.0017(8) 0.0012(8) C13 0.0120(10) 0.0069(9) 0.0136(10) 0.0002(7) 0.0015(7) 0.0005(8) C14 0.0112(10) 0.0090(9) 0.0143(10) -0.0001(8) -0.0006(8) -0.0005(8) C15 0.0132(10) 0.0105(10) 0.0121(9) -0.0015(8) -0.0017(8) -0.0007(8) C16 0.0127(10) 0.0077(9) 0.0110(9) 0.0002(7) -0.0022(8) 0.0012(8) C17 0.0158(10) 0.0110(10) 0.0126(10) 0.0019(8) -0.0014(8) 0.0005(8) C18 0.0178(11) 0.0097(9) 0.0113(9) -0.0004(7) -0.0012(8) 0.0020(8) C19 0.0138(10) 0.0087(9) 0.0103(8) 0.0003(7) 0.0001(8) 0.0015(8) C20 0.0138(10) 0.0111(10) 0.0122(9) 0.0021(8) 0.0004(8) -0.0002(8) C21 0.0182(11) 0.0081(10) 0.0169(10) 0.0021(8) -0.0020(8) -0.0029(8) C22 0.0209(13) 0.0136(10) 0.0211(11) 0.0030(8) 0.0000(9) 0.0023(9) C23 0.0198(11) 0.0106(10) 0.0156(10) -0.0015(8) -0.0040(9) -0.0044(9) C24 0.0263(13) 0.0205(12) 0.0235(12) -0.0085(10) 0.0037(10) -0.0023(10) C25 0.0240(12) 0.0127(10) 0.0109(9) -0.0008(8) -0.0032(9) -0.0006(9) C26 0.0200(12) 0.0240(13) 0.0190(11) -0.0017(10) -0.0072(9) -0.0008(10) C27 0.0282(13) 0.0174(11) 0.0101(9) 0.0026(8) -0.0018(9) -0.0050(9) C28 0.0442(18) 0.0237(13) 0.0201(12) 0.0093(10) -0.0034(11) 0.0061(12) C29 0.0165(11) 0.0118(10) 0.0121(10) 0.0022(8) 0.0008(8) -0.0014(8) C30 0.0371(15) 0.0157(12) 0.0221(12) 0.0051(9) 0.0051(11) 0.0073(11) C31 0.0147(11) 0.0107(10) 0.0154(10) 0.0007(8) -0.0028(8) -0.0036(8) C32 0.0232(13) 0.0167(12) 0.0201(11) -0.0072(9) -0.0038(10) 0.0014(9) C33 0.0201(12) 0.0150(10) 0.0110(9) 0.0013(8) -0.0031(8) -0.0020(9) C34 0.0244(13) 0.0228(12) 0.0174(11) -0.0084(9) -0.0003(9) -0.0004(10) C35 0.0223(12) 0.0152(10) 0.0104(9) 0.0017(7) -0.0006(9) -0.0027(9) C36 0.0215(11) 0.0187(10) 0.0157(11) 0.0056(9) -0.0017(9) -0.0016(11) N5 0.0209(11) 0.0269(12) 0.0471(14) -0.0133(10) -0.0015(11) -0.0005(10) N6 0.0327(14) 0.0301(13) 0.0362(14) 0.0061(11) 0.0115(11) 0.0101(11) C38 0.0172(11) 0.0173(11) 0.0169(11) -0.0023(9) -0.0019(9) 0.0059(9) C37 0.0149(11) 0.0200(12) 0.0173(11) -0.0057(9) -0.0040(9) 0.0044(9) C39 0.0151(10) 0.0154(10) 0.0208(10) -0.0032(9) 0.0008(9) 0.0045(8) C40 0.0150(11) 0.0175(11) 0.0238(12) -0.0030(9) 0.0001(9) 0.0049(9) C41 0.0167(11) 0.0159(11) 0.0329(14) -0.0024(10) 0.0026(10) 0.0029(9) C42 0.0200(13) 0.0199(12) 0.0313(14) -0.0009(10) 0.0067(10) 0.0048(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 Zn1 N2 2.028(2) . ? Zn1 N1 2.0370(18) . ? Zn1 N3 2.0384(19) . ? Zn1 N4 2.040(2) . ? N1 C1 1.370(3) . ? N1 C4 1.372(3) . ? N2 C16 1.367(3) . ? N2 C19 1.368(3) . ? N3 C14 1.363(3) . ? N3 C11 1.370(3) . ? N4 C6 1.367(3) . ? N4 C9 1.371(3) . ? C1 C20 1.397(3) . ? C1 C2 1.444(3) . ? C2 C3 1.368(3) . ? C2 C21 1.502(3) . ? C3 C4 1.448(3) . ? C3 C23 1.499(3) . ? C4 C5 1.394(3) . ? C5 C6 1.388(3) . ? C6 C7 1.449(3) . ? C7 C8 1.359(3) . ? C7 C25 1.502(3) . ? C8 C9 1.455(3) . ? C8 C27 1.506(3) . ? C9 C10 1.391(3) . ? C10 C11 1.392(3) . ? C11 C12 1.443(3) . ? C12 C13 1.368(3) . ? C12 C29 1.497(3) . ? C13 C14 1.454(3) . ? C13 C31 1.493(3) . ? C14 C15 1.391(3) . ? C15 C16 1.392(3) . ? C16 C17 1.451(3) . ? C17 C18 1.358(3) . ? C17 C33 1.500(3) . ? C18 C19 1.454(3) . ? C18 C35 1.496(3) . ? C19 C20 1.392(3) . ? C21 C22 1.526(3) . ? C23 C24 1.525(4) . ? C25 C26 1.518(4) . ? C27 C28 1.516(4) . ? C29 C30 1.532(3) . ? C31 C32 1.529(3) . ? C33 C34 1.530(4) . ? C35 C36 1.526(3) . ? N5 C41 1.144(4) . ? N6 C42 1.142(4) . ? C38 C37 1.339(4) . ? C38 C39 1.443(3) 3_566 ? C37 C39 1.449(3) . ? C39 C40 1.372(3) . ? C39 C38 1.443(3) 3_566 ? C40 C41 1.431(3) . ? C40 C42 1.435(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N1 89.96(7) . . ? N2 Zn1 N3 90.02(7) . . ? N1 Zn1 N3 175.81(7) . . ? N2 Zn1 N4 173.93(8) . . ? N1 Zn1 N4 89.70(7) . . ? N3 Zn1 N4 89.88(7) . . ? C1 N1 C4 106.39(17) . . ? C1 N1 Zn1 126.63(14) . . ? C4 N1 Zn1 126.81(15) . . ? C16 N2 C19 105.89(18) . . ? C16 N2 Zn1 126.86(14) . . ? C19 N2 Zn1 127.20(14) . . ? C14 N3 C11 106.54(17) . . ? C14 N3 Zn1 126.43(15) . . ? C11 N3 Zn1 127.02(15) . . ? C6 N4 C9 106.15(18) . . ? C6 N4 Zn1 127.06(14) . . ? C9 N4 Zn1 126.77(14) . . ? N1 C1 C20 124.49(19) . . ? N1 C1 C2 110.26(18) . . ? C20 C1 C2 125.22(19) . . ? C3 C2 C1 106.65(19) . . ? C3 C2 C21 127.4(2) . . ? C1 C2 C21 125.92(19) . . ? C2 C3 C4 106.6(2) . . ? C2 C3 C23 127.8(2) . . ? C4 C3 C23 125.6(2) . . ? N1 C4 C5 124.4(2) . . ? N1 C4 C3 110.06(18) . . ? C5 C4 C3 125.5(2) . . ? C6 C5 C4 127.0(2) . . ? N4 C6 C5 124.59(19) . . ? N4 C6 C7 110.52(18) . . ? C5 C6 C7 124.88(19) . . ? C8 C7 C6 106.63(19) . . ? C8 C7 C25 128.06(19) . . ? C6 C7 C25 125.3(2) . . ? C7 C8 C9 106.53(19) . . ? C7 C8 C27 127.2(2) . . ? C9 C8 C27 126.3(2) . . ? N4 C9 C10 124.59(19) . . ? N4 C9 C8 110.13(19) . . ? C10 C9 C8 125.27(19) . . ? C9 C10 C11 127.3(2) . . ? N3 C11 C10 124.4(2) . . ? N3 C11 C12 109.97(19) . . ? C10 C11 C12 125.7(2) . . ? C13 C12 C11 107.2(2) . . ? C13 C12 C29 126.8(2) . . ? C11 C12 C29 125.9(2) . . ? C12 C13 C14 105.8(2) . . ? C12 C13 C31 128.8(2) . . ? C14 C13 C31 125.40(19) . . ? N3 C14 C15 125.2(2) . . ? N3 C14 C13 110.51(18) . . ? C15 C14 C13 124.2(2) . . ? C14 C15 C16 126.3(2) . . ? N2 C16 C15 124.85(19) . . ? N2 C16 C17 110.65(19) . . ? C15 C16 C17 124.49(19) . . ? C18 C17 C16 106.50(19) . . ? C18 C17 C33 129.0(2) . . ? C16 C17 C33 124.3(2) . . ? C17 C18 C19 106.47(18) . . ? C17 C18 C35 127.6(2) . . ? C19 C18 C35 125.91(19) . . ? N2 C19 C20 124.49(19) . . ? N2 C19 C18 110.46(18) . . ? C20 C19 C18 125.04(19) . . ? C19 C20 C1 126.8(2) . . ? C2 C21 C22 113.8(2) . . ? C3 C23 C24 112.8(2) . . ? C7 C25 C26 112.9(2) . . ? C8 C27 C28 114.4(2) . . ? C12 C29 C30 112.5(2) . . ? C13 C31 C32 114.2(2) . . ? C17 C33 C34 111.7(2) . . ? C18 C35 C36 113.5(2) . . ? C37 C38 C39 121.3(2) . 3_566 ? C38 C37 C39 120.8(2) . . ? C40 C39 C38 121.4(2) . 3_566 ? C40 C39 C37 120.7(2) . . ? C38 C39 C37 117.9(2) 3_566 . ? C39 C40 C41 121.7(2) . . ? C39 C40 C42 122.5(2) . . ? C41 C40 C42 115.7(2) . . ? N5 C41 C40 178.9(3) . . ? N6 C42 C40 178.5(3) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.460 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.095 #===END data_dp08d _database_code_CSD 213237 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2{Cu(OEP)}.TCNQ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H92 Cu2 N12' _chemical_formula_weight 1396.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.343(2) _cell_length_b 14.142(4) _cell_length_c 21.723(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.02(2) _cell_angle_gamma 90.00 _cell_volume 3484.0(18) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 993 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 20 _exptl_crystal_description rod _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7272 _exptl_absorpt_correction_T_max 0.8804 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47174 _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _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 1.80 _diffrn_reflns_theta_max 25.36 _reflns_number_total 6239 _reflns_number_gt 5746 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.054 (Bruker, 2002)' _computing_cell_refinement 'SAINT 6.22 (Bruker, 2002)' _computing_data_reduction 'SAINT 6.22 (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0000P)^2^+26.0728P] 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 6239 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1637 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.206 _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 Cu1 Cu 0.29989(5) 0.45690(4) 0.49287(2) 0.01051(16) Uani 1 1 d . . . N1 N 0.2140(3) 0.3320(3) 0.49222(16) 0.0111(7) Uani 1 1 d . . . N2 N 0.3288(3) 0.4444(3) 0.58366(17) 0.0129(8) Uani 1 1 d . . . N3 N 0.3825(3) 0.5822(3) 0.49330(17) 0.0120(8) Uani 1 1 d . . . N4 N 0.2620(3) 0.4731(3) 0.40268(17) 0.0124(8) Uani 1 1 d . . . C1 C 0.1991(4) 0.2729(3) 0.5417(2) 0.0121(9) Uani 1 1 d . . . C2 C 0.1410(4) 0.1863(3) 0.5222(2) 0.0149(9) Uani 1 1 d . . . C3 C 0.1192(4) 0.1951(3) 0.4601(2) 0.0143(9) Uani 1 1 d . . . C4 C 0.1639(4) 0.2866(3) 0.4425(2) 0.0125(9) Uani 1 1 d . . . C5 C 0.1548(4) 0.3252(3) 0.3838(2) 0.0149(9) Uani 1 1 d . . . H5A H 0.1150 0.2884 0.3533 0.018 Uiso 1 1 calc R . . C6 C 0.1983(4) 0.4121(3) 0.3653(2) 0.0122(9) Uani 1 1 d . . . C7 C 0.1879(4) 0.4494(3) 0.3033(2) 0.0153(9) Uani 1 1 d . . . C8 C 0.2486(4) 0.5332(3) 0.3027(2) 0.0152(9) Uani 1 1 d . . . C9 C 0.2932(4) 0.5471(3) 0.3655(2) 0.0133(9) Uani 1 1 d . . . C10 C 0.3566(4) 0.6256(3) 0.3850(2) 0.0139(9) Uani 1 1 d . . . H10A H 0.3737 0.6721 0.3549 0.017 Uiso 1 1 calc R . . C11 C 0.3973(4) 0.6424(3) 0.4447(2) 0.0138(9) Uani 1 1 d . . . C12 C 0.4622(4) 0.7260(3) 0.4643(2) 0.0140(9) Uani 1 1 d . . . C13 C 0.4877(4) 0.7159(3) 0.5252(2) 0.0134(9) Uani 1 1 d . . . C14 C 0.4377(4) 0.6256(3) 0.5431(2) 0.0141(9) Uani 1 1 d . . . C15 C 0.4411(4) 0.5905(3) 0.6024(2) 0.0143(9) Uani 1 1 d . . . H15A H 0.4834 0.6262 0.6325 0.017 Uiso 1 1 calc R . . C16 C 0.3878(4) 0.5073(3) 0.6217(2) 0.0153(9) Uani 1 1 d . . . C17 C 0.3839(4) 0.4771(3) 0.6853(2) 0.0151(9) Uani 1 1 d . . . C18 C 0.3219(4) 0.3944(3) 0.6858(2) 0.0150(9) Uani 1 1 d . . . C19 C 0.2904(4) 0.3739(3) 0.6218(2) 0.0142(9) Uani 1 1 d . . . C20 C 0.2308(4) 0.2935(3) 0.6020(2) 0.0137(9) Uani 1 1 d . . . H20A H 0.2099 0.2487 0.6326 0.016 Uiso 1 1 calc R . . C21 C 0.1140(4) 0.1031(3) 0.5627(2) 0.0181(10) Uani 1 1 d . . . H21A H 0.0522 0.0643 0.5422 0.022 Uiso 1 1 calc R . . H21B H 0.0817 0.1268 0.6018 0.022 Uiso 1 1 calc R . . C22 C 0.2206(4) 0.0398(3) 0.5775(2) 0.0203(10) Uani 1 1 d . . . H22A H 0.1944 -0.0167 0.5994 0.031 Uiso 1 1 calc R . . H22B H 0.2773 0.0747 0.6035 0.031 Uiso 1 1 calc R . . H22C H 0.2583 0.0211 0.5391 0.031 Uiso 1 1 calc R . . C23 C 0.0634(4) 0.1240(3) 0.4172(2) 0.0197(10) Uani 1 1 d . . . H23A H 0.0316 0.1571 0.3804 0.024 Uiso 1 1 calc R . . H23B H -0.0033 0.0932 0.4381 0.024 Uiso 1 1 calc R . . C24 C 0.1506(5) 0.0481(4) 0.3969(2) 0.0261(11) Uani 1 1 d . . . H24A H 0.1125 0.0070 0.3662 0.039 Uiso 1 1 calc R . . H24B H 0.1755 0.0103 0.4326 0.039 Uiso 1 1 calc R . . H24C H 0.2196 0.0784 0.3789 0.039 Uiso 1 1 calc R . . C25 C 0.1167(4) 0.4056(4) 0.2517(2) 0.0190(10) Uani 1 1 d . . . H25A H 0.1346 0.3371 0.2500 0.023 Uiso 1 1 calc R . . H25B H 0.1407 0.4341 0.2123 0.023 Uiso 1 1 calc R . . C26 C -0.0166(4) 0.4186(4) 0.2588(2) 0.0251(11) Uani 1 1 d . . . H26A H -0.0584 0.3858 0.2252 0.038 Uiso 1 1 calc R . . H26B H -0.0358 0.4861 0.2574 0.038 Uiso 1 1 calc R . . H26C H -0.0408 0.3922 0.2983 0.038 Uiso 1 1 calc R . . C27 C 0.2686(5) 0.5973(4) 0.2487(2) 0.0221(11) Uani 1 1 d . . . H27A H 0.2920 0.5584 0.2131 0.027 Uiso 1 1 calc R . . H27B H 0.3349 0.6404 0.2589 0.027 Uiso 1 1 calc R . . C28 C 0.1615(6) 0.6563(4) 0.2302(3) 0.0327(13) Uani 1 1 d . . . H28A H 0.1780 0.6911 0.1923 0.049 Uiso 1 1 calc R . . H28B H 0.1439 0.7012 0.2631 0.049 Uiso 1 1 calc R . . H28C H 0.0935 0.6146 0.2232 0.049 Uiso 1 1 calc R . . C29 C 0.4899(4) 0.8100(3) 0.4242(2) 0.0179(10) Uani 1 1 d . . . H29A H 0.5008 0.7882 0.3814 0.021 Uiso 1 1 calc R . . H29B H 0.5649 0.8388 0.4387 0.021 Uiso 1 1 calc R . . C30 C 0.3924(5) 0.8849(4) 0.4250(2) 0.0269(12) Uani 1 1 d . . . H30A H 0.4157 0.9393 0.4000 0.040 Uiso 1 1 calc R . . H30B H 0.3798 0.9056 0.4675 0.040 Uiso 1 1 calc R . . H30C H 0.3191 0.8579 0.4081 0.040 Uiso 1 1 calc R . . C31 C 0.5537(4) 0.7820(3) 0.5679(2) 0.0155(9) Uani 1 1 d . . . H31A H 0.6053 0.8232 0.5432 0.019 Uiso 1 1 calc R . . H31B H 0.6048 0.7443 0.5960 0.019 Uiso 1 1 calc R . . C32 C 0.4727(4) 0.8441(4) 0.6062(2) 0.0224(11) Uani 1 1 d . . . H32A H 0.5204 0.8859 0.6325 0.034 Uiso 1 1 calc R . . H32B H 0.4232 0.8039 0.6319 0.034 Uiso 1 1 calc R . . H32C H 0.4224 0.8822 0.5787 0.034 Uiso 1 1 calc R . . C33 C 0.4330(4) 0.5326(3) 0.7387(2) 0.0180(10) Uani 1 1 d . . . H33A H 0.5108 0.5588 0.7277 0.022 Uiso 1 1 calc R . . H33B H 0.4451 0.4898 0.7744 0.022 Uiso 1 1 calc R . . C34 C 0.3512(5) 0.6134(4) 0.7570(2) 0.0238(11) Uani 1 1 d . . . H34A H 0.3871 0.6488 0.7914 0.036 Uiso 1 1 calc R . . H34B H 0.2753 0.5875 0.7697 0.036 Uiso 1 1 calc R . . H34C H 0.3389 0.6558 0.7218 0.036 Uiso 1 1 calc R . . C35 C 0.2914(4) 0.3348(3) 0.7405(2) 0.0174(10) Uani 1 1 d . . . H35A H 0.2093 0.3120 0.7354 0.021 Uiso 1 1 calc R . . H35B H 0.2953 0.3746 0.7780 0.021 Uiso 1 1 calc R . . C36 C 0.3735(4) 0.2493(4) 0.7494(2) 0.0223(11) Uani 1 1 d . . . H36A H 0.3480 0.2123 0.7849 0.034 Uiso 1 1 calc R . . H36B H 0.4544 0.2714 0.7566 0.034 Uiso 1 1 calc R . . H36C H 0.3704 0.2097 0.7124 0.034 Uiso 1 1 calc R . . N5 N 0.2015(4) 0.7726(3) 0.5655(3) 0.0344(12) Uani 1 1 d . . . N6 N 0.0914(4) 0.7598(4) 0.3722(3) 0.0377(12) Uani 1 1 d . . . C37 C 0.0072(4) 0.4627(3) 0.5603(2) 0.0188(10) Uani 1 1 d . . . H37A H 0.0106 0.4368 0.6007 0.023 Uiso 1 1 calc R . . C38 C 0.0574(4) 0.5469(4) 0.5495(2) 0.0202(10) Uani 1 1 d . . . H38A H 0.0970 0.5791 0.5822 0.024 Uiso 1 1 calc R . . C39 C 0.0524(4) 0.5896(3) 0.4891(2) 0.0173(10) Uani 1 1 d . . . C40 C 0.1008(4) 0.6761(4) 0.4781(2) 0.0221(11) Uani 1 1 d . . . C41 C 0.1584(5) 0.7294(4) 0.5266(3) 0.0262(12) Uani 1 1 d . . . C42 C 0.0957(5) 0.7218(4) 0.4184(3) 0.0254(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0143(3) 0.0074(3) 0.0098(3) -0.0001(2) -0.00066(19) -0.0004(2) N1 0.0149(18) 0.0099(18) 0.0083(18) -0.0016(14) 0.0002(14) 0.0007(14) N2 0.0156(19) 0.0092(18) 0.0138(19) -0.0009(15) -0.0016(14) -0.0015(15) N3 0.0136(18) 0.0085(18) 0.0138(19) 0.0031(15) 0.0001(14) -0.0002(14) N4 0.0150(19) 0.0099(18) 0.0122(19) -0.0002(15) -0.0015(14) -0.0002(14) C1 0.012(2) 0.011(2) 0.013(2) 0.0026(17) 0.0015(16) 0.0003(17) C2 0.013(2) 0.012(2) 0.020(2) -0.0014(18) -0.0004(17) 0.0010(17) C3 0.013(2) 0.011(2) 0.019(2) -0.0003(18) -0.0012(17) 0.0009(17) C4 0.010(2) 0.012(2) 0.016(2) -0.0034(18) 0.0004(17) 0.0014(17) C5 0.011(2) 0.017(2) 0.016(2) -0.0062(18) -0.0017(17) 0.0006(18) C6 0.013(2) 0.013(2) 0.011(2) -0.0026(17) -0.0002(16) 0.0033(17) C7 0.018(2) 0.014(2) 0.014(2) -0.0011(18) 0.0002(18) 0.0027(18) C8 0.021(2) 0.015(2) 0.010(2) -0.0014(18) 0.0000(17) -0.0008(18) C9 0.016(2) 0.015(2) 0.008(2) 0.0027(17) -0.0008(16) 0.0005(18) C10 0.013(2) 0.016(2) 0.013(2) 0.0021(18) 0.0015(17) -0.0010(17) C11 0.012(2) 0.012(2) 0.017(2) -0.0007(18) 0.0033(17) 0.0001(17) C12 0.013(2) 0.013(2) 0.017(2) 0.0000(18) 0.0018(17) 0.0008(17) C13 0.012(2) 0.011(2) 0.018(2) -0.0034(18) 0.0018(17) 0.0012(17) C14 0.012(2) 0.012(2) 0.018(2) -0.0014(18) -0.0007(17) 0.0016(17) C15 0.010(2) 0.015(2) 0.019(2) -0.0044(19) -0.0008(17) 0.0022(17) C16 0.012(2) 0.015(2) 0.019(2) 0.0012(19) 0.0009(17) 0.0016(18) C17 0.015(2) 0.013(2) 0.017(2) -0.0008(18) -0.0005(17) 0.0019(17) C18 0.014(2) 0.016(2) 0.015(2) -0.0012(18) -0.0004(17) 0.0006(18) C19 0.015(2) 0.012(2) 0.016(2) -0.0002(18) 0.0004(17) 0.0026(17) C20 0.016(2) 0.010(2) 0.015(2) 0.0030(18) 0.0010(17) -0.0002(17) C21 0.019(2) 0.014(2) 0.021(2) 0.0021(19) -0.0023(19) -0.0048(19) C22 0.027(3) 0.012(2) 0.022(3) 0.0013(19) -0.001(2) 0.000(2) C23 0.021(2) 0.013(2) 0.025(3) -0.001(2) -0.005(2) -0.0035(19) C24 0.035(3) 0.021(3) 0.023(3) -0.008(2) 0.004(2) -0.003(2) C25 0.025(3) 0.018(2) 0.014(2) -0.0002(19) -0.0034(19) -0.002(2) C26 0.026(3) 0.031(3) 0.018(3) 0.001(2) -0.008(2) -0.002(2) C27 0.032(3) 0.022(3) 0.012(2) 0.002(2) -0.002(2) -0.006(2) C28 0.051(4) 0.028(3) 0.019(3) 0.010(2) -0.003(2) 0.005(3) C29 0.017(2) 0.017(2) 0.020(2) -0.0004(19) -0.0014(18) -0.0040(19) C30 0.040(3) 0.020(3) 0.022(3) 0.008(2) 0.005(2) 0.008(2) C31 0.015(2) 0.013(2) 0.018(2) 0.0017(19) -0.0028(18) -0.0043(18) C32 0.023(3) 0.022(3) 0.022(3) -0.006(2) -0.002(2) 0.001(2) C33 0.022(2) 0.019(2) 0.013(2) 0.0004(19) -0.0024(18) -0.0024(19) C34 0.029(3) 0.024(3) 0.018(2) -0.006(2) -0.001(2) -0.002(2) C35 0.024(2) 0.016(2) 0.013(2) -0.0011(18) 0.0006(18) -0.0022(19) C36 0.024(3) 0.019(3) 0.024(3) 0.008(2) -0.001(2) -0.002(2) N5 0.026(2) 0.027(3) 0.050(3) -0.014(2) -0.001(2) -0.001(2) N6 0.035(3) 0.031(3) 0.047(3) 0.007(2) 0.014(2) 0.008(2) C37 0.018(2) 0.020(2) 0.018(2) -0.004(2) -0.0001(18) 0.0072(19) C38 0.017(2) 0.022(3) 0.021(2) -0.010(2) -0.0020(19) 0.004(2) C39 0.018(2) 0.017(2) 0.017(2) -0.0061(19) 0.0009(18) 0.0059(19) C40 0.013(2) 0.025(3) 0.029(3) -0.005(2) 0.0024(19) 0.004(2) C41 0.020(3) 0.020(3) 0.039(3) -0.005(2) 0.002(2) 0.004(2) C42 0.022(3) 0.024(3) 0.030(3) 0.005(2) 0.007(2) 0.004(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 Cu1 N2 2.001(4) . ? Cu1 N3 2.005(4) . ? Cu1 N4 2.011(4) . ? Cu1 N1 2.017(4) . ? N1 C4 1.372(6) . ? N1 C1 1.375(6) . ? N2 C19 1.373(6) . ? N2 C16 1.379(6) . ? N3 C11 1.369(6) . ? N3 C14 1.383(6) . ? N4 C9 1.373(6) . ? N4 C6 1.379(6) . ? C1 C20 1.384(6) . ? C1 C2 1.450(6) . ? C2 C3 1.373(7) . ? C2 C21 1.504(6) . ? C3 C4 1.443(6) . ? C3 C23 1.503(6) . ? C4 C5 1.389(7) . ? C5 C6 1.387(7) . ? C6 C7 1.450(6) . ? C7 C8 1.371(7) . ? C7 C25 1.503(6) . ? C8 C9 1.460(6) . ? C8 C27 1.503(6) . ? C9 C10 1.384(6) . ? C10 C11 1.390(6) . ? C11 C12 1.452(6) . ? C12 C13 1.359(6) . ? C12 C29 1.508(6) . ? C13 C14 1.452(6) . ? C13 C31 1.507(6) . ? C14 C15 1.381(7) . ? C15 C16 1.392(7) . ? C16 C17 1.447(7) . ? C17 C18 1.365(7) . ? C17 C33 1.500(6) . ? C18 C19 1.458(6) . ? C18 C35 1.502(6) . ? C19 C20 1.388(6) . ? C21 C22 1.534(7) . ? C23 C24 1.529(7) . ? C25 C26 1.533(7) . ? C27 C28 1.523(8) . ? C29 C30 1.533(7) . ? C31 C32 1.528(7) . ? C33 C34 1.529(7) . ? C35 C36 1.536(7) . ? N5 C41 1.146(7) . ? N6 C42 1.138(7) . ? C37 C38 1.342(7) . ? C37 C39 1.461(7) 3_566 ? C38 C39 1.444(7) . ? C39 C40 1.364(7) . ? C39 C37 1.461(7) 3_566 ? C40 C41 1.442(7) . ? C40 C42 1.450(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 N2 Cu1 N3 90.28(15) . . ? N2 Cu1 N4 176.73(15) . . ? N3 Cu1 N4 89.76(15) . . ? N2 Cu1 N1 90.02(15) . . ? N3 Cu1 N1 178.98(15) . . ? N4 Cu1 N1 89.89(15) . . ? C4 N1 C1 106.0(4) . . ? C4 N1 Cu1 127.5(3) . . ? C1 N1 Cu1 126.4(3) . . ? C19 N2 C16 105.2(4) . . ? C19 N2 Cu1 127.6(3) . . ? C16 N2 Cu1 127.1(3) . . ? C11 N3 C14 105.5(4) . . ? C11 N3 Cu1 127.6(3) . . ? C14 N3 Cu1 126.9(3) . . ? C9 N4 C6 105.6(4) . . ? C9 N4 Cu1 127.4(3) . . ? C6 N4 Cu1 127.1(3) . . ? N1 C1 C20 125.3(4) . . ? N1 C1 C2 110.3(4) . . ? C20 C1 C2 124.3(4) . . ? C3 C2 C1 106.5(4) . . ? C3 C2 C21 127.7(4) . . ? C1 C2 C21 125.8(4) . . ? C2 C3 C4 106.5(4) . . ? C2 C3 C23 127.9(4) . . ? C4 C3 C23 125.6(4) . . ? N1 C4 C5 124.2(4) . . ? N1 C4 C3 110.7(4) . . ? C5 C4 C3 125.1(4) . . ? C6 C5 C4 126.4(4) . . ? N4 C6 C5 124.7(4) . . ? N4 C6 C7 110.7(4) . . ? C5 C6 C7 124.6(4) . . ? C8 C7 C6 106.9(4) . . ? C8 C7 C25 127.8(4) . . ? C6 C7 C25 125.2(4) . . ? C7 C8 C9 105.9(4) . . ? C7 C8 C27 127.7(4) . . ? C9 C8 C27 126.4(4) . . ? N4 C9 C10 124.7(4) . . ? N4 C9 C8 111.0(4) . . ? C10 C9 C8 124.3(4) . . ? C9 C10 C11 125.8(4) . . ? N3 C11 C10 124.8(4) . . ? N3 C11 C12 110.4(4) . . ? C10 C11 C12 124.8(4) . . ? C13 C12 C11 107.3(4) . . ? C13 C12 C29 127.1(4) . . ? C11 C12 C29 125.6(4) . . ? C12 C13 C14 106.0(4) . . ? C12 C13 C31 129.0(4) . . ? C14 C13 C31 125.0(4) . . ? C15 C14 N3 125.1(4) . . ? C15 C14 C13 124.1(4) . . ? N3 C14 C13 110.8(4) . . ? C14 C15 C16 125.5(4) . . ? N2 C16 C15 124.9(4) . . ? N2 C16 C17 111.1(4) . . ? C15 C16 C17 123.9(4) . . ? C18 C17 C16 106.5(4) . . ? C18 C17 C33 128.8(4) . . ? C16 C17 C33 124.5(4) . . ? C17 C18 C19 106.3(4) . . ? C17 C18 C35 127.8(4) . . ? C19 C18 C35 125.9(4) . . ? N2 C19 C20 124.5(4) . . ? N2 C19 C18 110.9(4) . . ? C20 C19 C18 124.6(4) . . ? C1 C20 C19 125.7(4) . . ? C2 C21 C22 114.3(4) . . ? C3 C23 C24 112.4(4) . . ? C7 C25 C26 113.2(4) . . ? C8 C27 C28 113.9(4) . . ? C12 C29 C30 112.3(4) . . ? C13 C31 C32 113.2(4) . . ? C17 C33 C34 111.9(4) . . ? C18 C35 C36 113.2(4) . . ? C38 C37 C39 120.8(5) . 3_566 ? C37 C38 C39 121.4(5) . . ? C40 C39 C38 121.6(5) . . ? C40 C39 C37 120.5(5) . 3_566 ? C38 C39 C37 117.8(4) . 3_566 ? C39 C40 C41 121.3(5) . . ? C39 C40 C42 123.1(5) . . ? C41 C40 C42 115.5(5) . . ? N5 C41 C40 178.3(6) . . ? N6 C42 C40 178.3(6) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.124 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.110