# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Xiao-Jun Zhao' _publ_contact_author_email 'xiaojun zhao15@yahoo.com.cn' _publ_section_title ; CoII, MnII and CuII-directed coordination polymers with mixed tetrazolate-dicarboxylate heterobridges exhibiting spin-canted, spin-frustrated antiferromagnetism and slight spin-flop transition ; loop_ _publ_author_name 'En-Cui Yang' 'Zhong-Yi Liu' 'Xiao-Yun Wu' 'Hong Chang' 'En-Chan Wang' ; Xiao-Jun Zhao ; # Attachment '- 2.cif' data_91106a _database_code_depnum_ccdc_archive 'CCDC 779502' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9.50 H11 Mn2 N6 O9' _chemical_formula_weight 463.12 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6921(11) _cell_length_b 10.1758(16) _cell_length_c 12.444(2) _cell_angle_alpha 74.805(2) _cell_angle_beta 74.955(2) _cell_angle_gamma 88.679(2) _cell_volume 788.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3781 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.950 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 1.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7109 _exptl_absorpt_correction_T_max 0.7319 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4041 _diffrn_reflns_av_R_equivalents 0.0110 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2756 _reflns_number_gt 2588 _reflns_threshold_expression >2sigma(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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0409P)^2^+0.9256P] 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 2756 _refine_ls_number_parameters 262 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.068 _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 Mn1 Mn 0.27982(6) 0.41612(4) 0.54051(3) 0.02394(13) Uani 1 1 d D . . Mn2 Mn 0.65744(5) 0.44085(4) 0.25617(3) 0.02123(12) Uani 1 1 d . . . O1 O 0.6592(3) 0.7035(2) 0.29991(17) 0.0443(5) Uani 1 1 d . . . O2 O 0.6936(3) 0.63994(19) 0.13913(18) 0.0379(5) Uani 1 1 d . . . O3 O 0.6670(4) 1.2056(2) 0.2737(2) 0.0581(7) Uani 1 1 d . . . O4 O 0.7165(4) 1.3502(2) 0.1066(2) 0.0498(6) Uani 1 1 d . . . O5 O 0.8118(5) 1.1909(3) -0.2362(2) 0.0640(7) Uani 1 1 d . . . O6 O 0.8472(5) 0.9799(3) -0.2287(2) 0.0673(8) Uani 1 1 d . . . O7 O 0.5832(3) 0.40304(17) 0.43907(14) 0.0237(4) Uani 1 1 d . . . H7' H 0.6469 0.3205 0.4736 0.028 Uiso 1 1 calc R . . O8 O 0.1364(6) 0.2275(3) 0.5405(2) 0.0859(10) Uani 1 1 d . . . H8A H 0.2081 0.2028 0.4826 0.129 Uiso 1 1 d RD . . H8B H 0.0094 0.2413 0.5437 0.129 Uiso 1 1 d RD . . N1 N 0.9919(3) 0.4700(2) 0.26316(18) 0.0272(5) Uani 1 1 d . . . N2 N 1.0088(3) 0.5045(2) 0.35817(18) 0.0270(5) Uani 1 1 d . . . N3 N 1.1980(3) 0.4927(2) 0.36635(18) 0.0268(5) Uani 1 1 d . . . N4 N 1.3140(3) 0.4514(2) 0.27635(18) 0.0261(5) Uani 1 1 d . . . N5 N 1.2365(4) 0.3942(3) 0.1173(2) 0.0383(6) Uani 1 1 d . . . H5" H 1.1612 0.4180 0.0655 0.046 Uiso 1 1 d R . . H5' H 1.3738 0.4062 0.0846 0.046 Uiso 1 1 d R . . N6 N 0.8124(4) 1.0723(3) -0.1826(2) 0.0377(6) Uani 1 1 d . . . C1 C 1.1833(4) 0.4392(3) 0.2143(2) 0.0247(5) Uani 1 1 d . . . C2 C 0.7072(4) 0.8753(2) 0.1242(2) 0.0244(5) Uani 1 1 d . . . C3 C 0.6905(4) 0.9802(3) 0.1774(2) 0.0296(6) Uani 1 1 d . . . H3 H 0.6641 0.9601 0.2573 0.036 Uiso 1 1 calc R . . C4 C 0.7130(4) 1.1158(3) 0.1121(2) 0.0296(6) Uani 1 1 d . . . C5 C 0.7513(4) 1.1460(3) -0.0060(2) 0.0300(6) Uani 1 1 d . . . H5 H 0.7648 1.2361 -0.0504 0.036 Uiso 1 1 calc R . . C6 C 0.7692(4) 1.0403(3) -0.0568(2) 0.0260(5) Uani 1 1 d . . . C7 C 0.7482(4) 0.9051(3) 0.0050(2) 0.0248(5) Uani 1 1 d . . . H7 H 0.7613 0.8359 -0.0321 0.030 Uiso 1 1 calc R . . C8 C 0.6849(4) 0.7281(3) 0.1933(2) 0.0297(6) Uani 1 1 d . . . C9 C 0.6990(4) 1.2314(3) 0.1673(3) 0.0374(7) Uani 1 1 d . . . O9 O 0.848(3) 0.1522(16) 0.4553(13) 0.083(5) Uani 0.25 1 d P A 1 O9' O 0.776(2) 0.1707(14) 0.5280(15) 0.085(5) Uani 0.25 1 d P B 2 C10 C 0.272(2) 0.0852(13) 0.4058(11) 0.110(4) Uani 0.50 1 d PDU . . O10 O 0.425(2) 0.0347(16) 0.4802(15) 0.211(6) Uani 0.50 1 d PDU . . 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 Mn1 0.0223(2) 0.0302(2) 0.0216(2) -0.01153(16) -0.00486(15) -0.00010(15) Mn2 0.0213(2) 0.0229(2) 0.0219(2) -0.01007(15) -0.00579(15) 0.00187(14) O1 0.0514(13) 0.0450(12) 0.0294(11) 0.0006(9) -0.0098(9) 0.0119(10) O2 0.0475(12) 0.0224(9) 0.0445(12) -0.0077(9) -0.0145(10) 0.0009(8) O3 0.091(2) 0.0458(13) 0.0488(15) -0.0303(11) -0.0212(13) 0.0121(13) O4 0.0681(16) 0.0279(11) 0.0585(14) -0.0235(10) -0.0135(12) 0.0054(10) O5 0.093(2) 0.0467(15) 0.0359(13) 0.0075(11) -0.0065(13) 0.0012(13) O6 0.114(2) 0.0577(16) 0.0316(13) -0.0219(11) -0.0119(13) 0.0060(15) O7 0.0235(9) 0.0248(9) 0.0236(9) -0.0094(7) -0.0050(7) 0.0032(7) O8 0.129(3) 0.0675(18) 0.0586(18) -0.0115(14) -0.0206(18) -0.0517(19) N1 0.0238(11) 0.0377(12) 0.0253(11) -0.0151(9) -0.0087(9) 0.0041(9) N2 0.0217(11) 0.0386(12) 0.0255(11) -0.0151(9) -0.0080(9) 0.0035(9) N3 0.0218(11) 0.0378(12) 0.0247(11) -0.0144(9) -0.0068(9) 0.0034(9) N4 0.0208(10) 0.0363(12) 0.0239(11) -0.0126(9) -0.0060(8) 0.0029(9) N5 0.0373(13) 0.0562(16) 0.0293(13) -0.0228(11) -0.0118(10) 0.0102(11) N6 0.0360(13) 0.0436(15) 0.0297(13) -0.0052(11) -0.0064(10) -0.0011(11) C1 0.0264(13) 0.0268(13) 0.0212(12) -0.0076(10) -0.0058(10) 0.0018(10) C2 0.0231(12) 0.0233(12) 0.0274(13) -0.0073(10) -0.0074(10) 0.0024(9) C3 0.0294(14) 0.0348(14) 0.0282(14) -0.0143(11) -0.0081(11) 0.0063(11) C4 0.0280(13) 0.0271(13) 0.0400(15) -0.0183(12) -0.0104(11) 0.0050(10) C5 0.0280(14) 0.0225(13) 0.0396(15) -0.0079(11) -0.0094(11) 0.0018(10) C6 0.0232(12) 0.0293(13) 0.0256(13) -0.0080(10) -0.0056(10) 0.0008(10) C7 0.0239(12) 0.0254(13) 0.0293(13) -0.0134(10) -0.0080(10) 0.0024(10) C8 0.0241(13) 0.0292(14) 0.0334(15) -0.0045(11) -0.0071(11) 0.0036(10) C9 0.0321(15) 0.0417(17) 0.0484(18) -0.0269(14) -0.0134(13) 0.0081(12) O9 0.124(13) 0.079(9) 0.068(9) -0.004(8) -0.079(10) -0.011(8) O9' 0.096(11) 0.064(8) 0.103(12) 0.019(8) -0.079(10) 0.000(7) C10 0.121(8) 0.107(7) 0.108(7) -0.046(6) -0.026(6) -0.015(6) O10 0.227(11) 0.188(10) 0.220(10) -0.067(8) -0.049(8) 0.023(8) _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 Mn1 O7 2.1164(17) . ? Mn1 O8 2.165(2) . ? Mn1 O1 2.173(2) 2_666 ? Mn1 O7 2.1759(17) 2_666 ? Mn1 N2 2.274(2) 2_666 ? Mn1 N3 2.306(2) 1_455 ? Mn1 Mn1 3.2253(9) 2_666 ? Mn2 O7 2.1303(17) . ? Mn2 O2 2.139(2) . ? Mn2 O4 2.230(2) 1_545 ? Mn2 N4 2.249(2) 1_455 ? Mn2 N1 2.291(2) . ? Mn2 O3 2.347(2) 1_545 ? Mn2 C9 2.625(3) 1_545 ? O1 C8 1.249(3) . ? O1 Mn1 2.173(2) 2_666 ? O2 C8 1.248(3) . ? O3 C9 1.242(4) . ? O3 Mn2 2.347(2) 1_565 ? O4 C9 1.235(4) . ? O4 Mn2 2.230(2) 1_565 ? O5 N6 1.217(3) . ? O6 N6 1.213(4) . ? O7 Mn1 2.1759(17) 2_666 ? O7 H7' 0.9800 . ? O8 H8A 0.8499 . ? O8 H8B 0.8506 . ? N1 C1 1.336(3) . ? N1 N2 1.350(3) . ? N2 N3 1.296(3) . ? N2 Mn1 2.274(2) 2_666 ? N3 N4 1.347(3) . ? N3 Mn1 2.306(2) 1_655 ? N4 C1 1.336(3) . ? N4 Mn2 2.249(2) 1_655 ? N5 C1 1.361(3) . ? N5 H5" 0.8999 . ? N5 H5' 0.8999 . ? N6 C6 1.464(3) . ? C2 C3 1.385(4) . ? C2 C7 1.386(4) . ? C2 C8 1.509(4) . ? C3 C4 1.395(4) . ? C3 H3 0.9300 . ? C4 C5 1.375(4) . ? C4 C9 1.500(4) . ? C5 C6 1.373(4) . ? C5 H5 0.9300 . ? C6 C7 1.379(4) . ? C7 H7 0.9300 . ? C9 Mn2 2.625(3) 1_565 ? C10 O10 1.547(9) . ? O10 O10 1.33(2) 2_656 ? 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 O7 Mn1 O8 100.44(11) . . ? O7 Mn1 O1 94.08(7) . 2_666 ? O8 Mn1 O1 84.40(11) . 2_666 ? O7 Mn1 O7 82.59(7) . 2_666 ? O8 Mn1 O7 173.72(9) . 2_666 ? O1 Mn1 O7 89.92(8) 2_666 2_666 ? O7 Mn1 N2 162.55(8) . 2_666 ? O8 Mn1 N2 96.74(12) . 2_666 ? O1 Mn1 N2 90.59(8) 2_666 2_666 ? O7 Mn1 N2 80.62(7) 2_666 2_666 ? O7 Mn1 N3 85.14(7) . 1_455 ? O8 Mn1 N3 82.31(10) . 1_455 ? O1 Mn1 N3 166.31(8) 2_666 1_455 ? O7 Mn1 N3 103.51(7) 2_666 1_455 ? N2 Mn1 N3 94.20(8) 2_666 1_455 ? O7 Mn1 Mn1 41.99(5) . 2_666 ? O8 Mn1 Mn1 142.14(11) . 2_666 ? O1 Mn1 Mn1 92.63(6) 2_666 2_666 ? O7 Mn1 Mn1 40.60(4) 2_666 2_666 ? N2 Mn1 Mn1 121.07(6) 2_666 2_666 ? N3 Mn1 Mn1 95.86(5) 1_455 2_666 ? O7 Mn2 O2 124.08(7) . . ? O7 Mn2 O4 146.46(8) . 1_545 ? O2 Mn2 O4 89.43(8) . 1_545 ? O7 Mn2 N4 85.94(7) . 1_455 ? O2 Mn2 N4 88.02(8) . 1_455 ? O4 Mn2 N4 94.59(8) 1_545 1_455 ? O7 Mn2 N1 84.96(7) . . ? O2 Mn2 N1 87.51(8) . . ? O4 Mn2 N1 99.40(8) 1_545 . ? N4 Mn2 N1 165.27(8) 1_455 . ? O7 Mn2 O3 90.32(8) . 1_545 ? O2 Mn2 O3 145.60(8) . 1_545 ? O4 Mn2 O3 56.20(8) 1_545 1_545 ? N4 Mn2 O3 95.43(9) 1_455 1_545 ? N1 Mn2 O3 96.19(9) . 1_545 ? O7 Mn2 C9 118.48(9) . 1_545 ? O2 Mn2 C9 117.43(9) . 1_545 ? O4 Mn2 C9 28.00(9) 1_545 1_545 ? N4 Mn2 C9 95.11(8) 1_455 1_545 ? N1 Mn2 C9 99.41(8) . 1_545 ? O3 Mn2 C9 28.22(9) 1_545 1_545 ? C8 O1 Mn1 150.74(19) . 2_666 ? C8 O2 Mn2 109.76(18) . . ? C9 O3 Mn2 88.44(19) . 1_565 ? C9 O4 Mn2 94.07(19) . 1_565 ? Mn1 O7 Mn2 122.71(8) . . ? Mn1 O7 Mn1 97.41(7) . 2_666 ? Mn2 O7 Mn1 102.04(7) . 2_666 ? Mn1 O7 H7' 111.0 . . ? Mn2 O7 H7' 111.0 . . ? Mn1 O7 H7' 111.0 2_666 . ? Mn1 O8 H8A 107.4 . . ? Mn1 O8 H8B 107.4 . . ? H8A O8 H8B 117.2 . . ? C1 N1 N2 104.5(2) . . ? C1 N1 Mn2 139.68(17) . . ? N2 N1 Mn2 114.21(15) . . ? N3 N2 N1 109.88(19) . . ? N3 N2 Mn1 133.79(16) . 2_666 ? N1 N2 Mn1 116.14(15) . 2_666 ? N2 N3 N4 109.47(19) . . ? N2 N3 Mn1 122.85(16) . 1_655 ? N4 N3 Mn1 117.34(15) . 1_655 ? C1 N4 N3 104.95(19) . . ? C1 N4 Mn2 136.57(17) . 1_655 ? N3 N4 Mn2 118.12(15) . 1_655 ? C1 N5 H5" 119.0 . . ? C1 N5 H5' 111.0 . . ? H5" N5 H5' 112.9 . . ? O6 N6 O5 123.0(3) . . ? O6 N6 C6 118.7(2) . . ? O5 N6 C6 118.3(3) . . ? N4 C1 N1 111.2(2) . . ? N4 C1 N5 124.2(2) . . ? N1 C1 N5 124.6(2) . . ? C3 C2 C7 119.8(2) . . ? C3 C2 C8 121.2(2) . . ? C7 C2 C8 119.0(2) . . ? C2 C3 C4 120.4(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.0(2) . . ? C5 C4 C9 118.4(3) . . ? C3 C4 C9 121.6(3) . . ? C6 C5 C4 118.4(2) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 C7 123.1(2) . . ? C5 C6 N6 118.5(2) . . ? C7 C6 N6 118.4(2) . . ? C6 C7 C2 118.2(2) . . ? C6 C7 H7 120.9 . . ? C2 C7 H7 120.9 . . ? O2 C8 O1 125.0(3) . . ? O2 C8 C2 117.1(2) . . ? O1 C8 C2 117.9(2) . . ? O4 C9 O3 121.3(3) . . ? O4 C9 C4 119.6(3) . . ? O3 C9 C4 119.1(3) . . ? O4 C9 Mn2 57.94(15) . 1_565 ? O3 C9 Mn2 63.35(16) . 1_565 ? C4 C9 Mn2 176.2(2) . 1_565 ? O10 O10 C10 161(2) 2_656 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Mn2 O2 C8 6.5(2) . . . . ? O4 Mn2 O2 C8 -175.18(19) 1_545 . . . ? N4 Mn2 O2 C8 90.21(18) 1_455 . . . ? N1 Mn2 O2 C8 -75.74(18) . . . . ? O3 Mn2 O2 C8 -173.06(18) 1_545 . . . ? C9 Mn2 O2 C8 -175.05(17) 1_545 . . . ? O8 Mn1 O7 Mn2 76.08(12) . . . . ? O1 Mn1 O7 Mn2 161.12(10) 2_666 . . . ? O7 Mn1 O7 Mn2 -109.49(11) 2_666 . . . ? N2 Mn1 O7 Mn2 -93.7(2) 2_666 . . . ? N3 Mn1 O7 Mn2 -5.17(10) 1_455 . . . ? Mn1 Mn1 O7 Mn2 -109.49(11) 2_666 . . . ? O8 Mn1 O7 Mn1 -174.43(10) . . . 2_666 ? O1 Mn1 O7 Mn1 -89.39(8) 2_666 . . 2_666 ? O7 Mn1 O7 Mn1 0.0 2_666 . . 2_666 ? N2 Mn1 O7 Mn1 15.8(3) 2_666 . . 2_666 ? N3 Mn1 O7 Mn1 104.32(8) 1_455 . . 2_666 ? O2 Mn2 O7 Mn1 77.49(12) . . . . ? O4 Mn2 O7 Mn1 -99.54(15) 1_545 . . . ? N4 Mn2 O7 Mn1 -7.36(10) 1_455 . . . ? N1 Mn2 O7 Mn1 161.04(10) . . . . ? O3 Mn2 O7 Mn1 -102.78(11) 1_545 . . . ? C9 Mn2 O7 Mn1 -100.98(11) 1_545 . . . ? O2 Mn2 O7 Mn1 -29.60(11) . . . 2_666 ? O4 Mn2 O7 Mn1 153.37(12) 1_545 . . 2_666 ? N4 Mn2 O7 Mn1 -114.44(8) 1_455 . . 2_666 ? N1 Mn2 O7 Mn1 53.95(8) . . . 2_666 ? O3 Mn2 O7 Mn1 150.14(9) 1_545 . . 2_666 ? C9 Mn2 O7 Mn1 151.94(8) 1_545 . . 2_666 ? O7 Mn2 N1 C1 139.2(3) . . . . ? O2 Mn2 N1 C1 -96.3(3) . . . . ? O4 Mn2 N1 C1 -7.3(3) 1_545 . . . ? N4 Mn2 N1 C1 -168.7(3) 1_455 . . . ? O3 Mn2 N1 C1 49.4(3) 1_545 . . . ? C9 Mn2 N1 C1 21.1(3) 1_545 . . . ? O7 Mn2 N1 N2 -23.53(17) . . . . ? O2 Mn2 N1 N2 101.00(18) . . . . ? O4 Mn2 N1 N2 -169.99(17) 1_545 . . . ? N4 Mn2 N1 N2 28.5(4) 1_455 . . . ? O3 Mn2 N1 N2 -113.30(18) 1_545 . . . ? C9 Mn2 N1 N2 -141.60(18) 1_545 . . . ? C1 N1 N2 N3 -1.0(3) . . . . ? Mn2 N1 N2 N3 167.53(16) . . . . ? C1 N1 N2 Mn1 174.55(16) . . . 2_666 ? Mn2 N1 N2 Mn1 -16.9(2) . . . 2_666 ? N1 N2 N3 N4 0.7(3) . . . . ? Mn1 N2 N3 N4 -173.78(18) 2_666 . . . ? N1 N2 N3 Mn1 -143.20(17) . . . 1_655 ? Mn1 N2 N3 Mn1 42.3(3) 2_666 . . 1_655 ? N2 N3 N4 C1 -0.1(3) . . . . ? Mn1 N3 N4 C1 146.05(16) 1_655 . . . ? N2 N3 N4 Mn2 174.16(16) . . . 1_655 ? Mn1 N3 N4 Mn2 -39.7(2) 1_655 . . 1_655 ? N3 N4 C1 N1 -0.6(3) . . . . ? Mn2 N4 C1 N1 -173.19(18) 1_655 . . . ? N3 N4 C1 N5 -177.4(2) . . . . ? Mn2 N4 C1 N5 10.0(4) 1_655 . . . ? N2 N1 C1 N4 1.0(3) . . . . ? Mn2 N1 C1 N4 -162.8(2) . . . . ? N2 N1 C1 N5 177.8(2) . . . . ? Mn2 N1 C1 N5 14.0(4) . . . . ? C7 C2 C3 C4 0.5(4) . . . . ? C8 C2 C3 C4 179.5(2) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C2 C3 C4 C9 -179.0(2) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C9 C4 C5 C6 178.4(2) . . . . ? C4 C5 C6 C7 0.7(4) . . . . ? C4 C5 C6 N6 -179.3(2) . . . . ? O6 N6 C6 C5 173.3(3) . . . . ? O5 N6 C6 C5 -6.7(4) . . . . ? O6 N6 C6 C7 -6.7(4) . . . . ? O5 N6 C6 C7 173.3(3) . . . . ? C5 C6 C7 C2 0.0(4) . . . . ? N6 C6 C7 C2 -180.0(2) . . . . ? C3 C2 C7 C6 -0.6(4) . . . . ? C8 C2 C7 C6 -179.7(2) . . . . ? Mn2 O2 C8 O1 0.1(3) . . . . ? Mn2 O2 C8 C2 -179.89(17) . . . . ? Mn1 O1 C8 O2 40.1(6) 2_666 . . . ? Mn1 O1 C8 C2 -140.0(3) 2_666 . . . ? C3 C2 C8 O2 177.1(2) . . . . ? C7 C2 C8 O2 -3.9(4) . . . . ? C3 C2 C8 O1 -2.8(4) . . . . ? C7 C2 C8 O1 176.2(2) . . . . ? Mn2 O4 C9 O3 -2.2(3) 1_565 . . . ? Mn2 O4 C9 C4 176.7(2) 1_565 . . . ? Mn2 O3 C9 O4 2.1(3) 1_565 . . . ? Mn2 O3 C9 C4 -176.8(2) 1_565 . . . ? C5 C4 C9 O4 1.9(4) . . . . ? C3 C4 C9 O4 -178.8(3) . . . . ? C5 C4 C9 O3 -179.1(3) . . . . ? C3 C4 C9 O3 0.1(4) . . . . ? C5 C4 C9 Mn2 50(4) . . . 1_565 ? C3 C4 C9 Mn2 -130(3) . . . 1_565 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.480 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.065 # Attachment '- 3.cif' data_n100810a _database_code_depnum_ccdc_archive 'CCDC 794789' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 Cu8 N24 O40' _chemical_formula_weight 1965.30 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.4021(3) _cell_length_b 14.9295(6) _cell_length_c 15.8901(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1518.78(11) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6572 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 28.27 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 2.874 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6724 _exptl_absorpt_correction_T_max 0.7620 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7715 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2672 _reflns_number_gt 2622 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0397P)^2^+1.4494P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.554(14) _refine_ls_number_reflns 2672 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0630 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 0.73662(6) 0.59122(2) 0.13476(2) 0.00787(10) Uani 1 1 d . . . Cu2 Cu 0.48552(6) 0.75625(3) 0.00532(2) 0.00946(11) Uani 1 1 d . . . O1 O 0.7303(4) 0.51612(13) 0.02999(12) 0.0114(4) Uani 1 1 d . . . O2 O 0.7183(4) 0.43064(14) 0.14261(13) 0.0174(5) Uani 1 1 d . . . O3 O 0.7593(4) 0.38054(13) -0.24842(12) 0.0125(4) Uani 1 1 d . . . O4 O 0.7205(4) 0.23279(15) -0.26952(13) 0.0168(5) Uani 1 1 d . . . O5 O 0.7285(5) 0.04329(13) -0.01274(14) 0.0212(5) Uani 1 1 d . . . O6 O 0.7136(4) 0.10436(15) 0.11086(14) 0.0206(6) Uani 1 1 d . . . O7 O 0.7392(4) 0.72320(13) 0.06122(12) 0.0101(4) Uani 1 1 d . . . H7' H 0.7537 0.7522 0.1069 0.015 Uiso 1 1 d R . . O8 O 0.4525(5) 0.87712(17) 0.09435(15) 0.0243(6) Uani 1 1 d . . . H8A H 0.3971 0.9194 0.0663 0.036 Uiso 1 1 d R . . H8B H 0.3559 0.8578 0.1263 0.036 Uiso 1 1 d R . . N1 N 0.4120(4) 0.60458(18) 0.13083(17) 0.0093(6) Uani 1 1 d . . . N2 N 0.3385(4) 0.66478(18) 0.07557(18) 0.0103(6) Uani 1 1 d . . . N3 N 0.1373(4) 0.66360(17) 0.07478(18) 0.0100(6) Uani 1 1 d . . . N4 N 0.0660(4) 0.60319(18) 0.12961(18) 0.0089(5) Uani 1 1 d . . . N5 N 0.2391(5) 0.49900(16) 0.22060(16) 0.0148(5) Uani 1 1 d . . . H5' H 0.3495 0.4826 0.2521 0.018 Uiso 1 1 d R . . H5" H 0.1179 0.4976 0.2493 0.018 Uiso 1 1 d R . . N6 N 0.7211(4) 0.10925(17) 0.03389(16) 0.0122(6) Uani 1 1 d . . . C1 C 0.2385(6) 0.56703(19) 0.16400(18) 0.0102(6) Uani 1 1 d . . . C2 C 0.7238(5) 0.35729(19) 0.00957(19) 0.0100(6) Uani 1 1 d . . . C3 C 0.7276(5) 0.36510(19) -0.07768(18) 0.0103(6) Uani 1 1 d . . . H3 H 0.7296 0.4228 -0.1028 0.012 Uiso 1 1 calc R . . C4 C 0.7286(5) 0.28884(19) -0.12883(19) 0.0110(6) Uani 1 1 d . . . C5 C 0.7251(5) 0.20452(19) -0.09276(19) 0.0108(6) Uani 1 1 d . . . H5D H 0.7251 0.1522 -0.1267 0.013 Uiso 1 1 calc R . . C6 C 0.7214(5) 0.19840(19) -0.00557(19) 0.0098(6) Uani 1 1 d . . . C7 C 0.7209(5) 0.2730(2) 0.04663(19) 0.0112(6) Uani 1 1 d . . . H7 H 0.7186 0.2666 0.1061 0.013 Uiso 1 1 calc R . . C8 C 0.7249(5) 0.43905(19) 0.06494(18) 0.0101(6) Uani 1 1 d . . . C9 C 0.7361(5) 0.29964(19) -0.22407(18) 0.0106(6) Uani 1 1 d . . . O9 O 0.0637(5) 0.4074(2) 0.3924(2) 0.0418(8) Uani 1 1 d . . . H9A H 0.1953 0.4133 0.3881 0.063 Uiso 1 1 d R . . H9B H 0.0262 0.4476 0.4272 0.063 Uiso 1 1 d R . . O10 O 0.7690(5) 0.31106(19) 0.27596(17) 0.0361(7) Uani 1 1 d . . . H10A H 0.8497 0.3554 0.2842 0.054 Uiso 1 1 d R . . H10B H 0.7027 0.3236 0.2311 0.054 Uiso 1 1 d 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 Cu1 0.00756(17) 0.00860(17) 0.00747(17) -0.00090(13) -0.00013(16) -0.00022(16) Cu2 0.0071(2) 0.01037(18) 0.01091(18) 0.00314(14) 0.00001(13) -0.00008(13) O1 0.0115(11) 0.0100(10) 0.0129(10) -0.0003(8) 0.0000(10) -0.0003(10) O2 0.0305(14) 0.0129(10) 0.0088(11) -0.0013(9) -0.0007(11) 0.0015(10) O3 0.0167(11) 0.0125(10) 0.0082(10) 0.0029(8) 0.0005(10) -0.0003(10) O4 0.0277(14) 0.0135(10) 0.0093(10) -0.0008(9) -0.0006(10) -0.0039(11) O5 0.0384(15) 0.0073(10) 0.0179(11) -0.0027(9) -0.0021(13) 0.0023(11) O6 0.0374(16) 0.0149(11) 0.0095(12) 0.0023(8) 0.0015(11) 0.0026(12) O7 0.0084(10) 0.0117(9) 0.0102(10) 0.0007(8) 0.0008(10) 0.0011(10) O8 0.0376(17) 0.0190(12) 0.0163(13) 0.0041(10) 0.0046(12) 0.0092(12) N1 0.0117(13) 0.0096(14) 0.0066(12) 0.0022(11) -0.0023(11) 0.0020(10) N2 0.0095(13) 0.0097(13) 0.0116(15) 0.0017(11) -0.0007(11) 0.0008(10) N3 0.0101(14) 0.0078(13) 0.0121(14) 0.0001(11) -0.0021(12) 0.0013(11) N4 0.0104(13) 0.0075(13) 0.0086(12) 0.0000(11) -0.0010(11) -0.0010(10) N5 0.0132(13) 0.0161(12) 0.0152(13) 0.0076(10) -0.0019(14) -0.0012(14) N6 0.0104(14) 0.0129(13) 0.0135(14) 0.0013(10) 0.0004(11) 0.0012(11) C1 0.0120(15) 0.0094(13) 0.0092(13) -0.0042(11) -0.0001(14) -0.0020(14) C2 0.0061(15) 0.0109(13) 0.0131(14) -0.0004(12) -0.0009(13) 0.0018(13) C3 0.0073(15) 0.0113(14) 0.0122(14) 0.0018(11) -0.0003(13) 0.0029(13) C4 0.0066(14) 0.0149(14) 0.0116(14) 0.0001(12) -0.0009(15) 0.0014(13) C5 0.0086(15) 0.0095(13) 0.0143(15) -0.0020(11) -0.0020(14) 0.0006(13) C6 0.0075(15) 0.0090(13) 0.0131(15) 0.0024(12) 0.0009(14) 0.0016(12) C7 0.0066(16) 0.0171(15) 0.0097(14) 0.0001(12) 0.0004(13) 0.0000(13) C8 0.0068(15) 0.0117(14) 0.0117(15) -0.0004(12) -0.0019(14) 0.0010(13) C9 0.0056(13) 0.0151(14) 0.0112(14) 0.0010(12) 0.0019(14) 0.0035(14) O9 0.0384(18) 0.0407(19) 0.0463(18) -0.0131(15) -0.0091(14) 0.0023(16) O10 0.0372(17) 0.0424(16) 0.0289(14) 0.0055(12) 0.0003(16) 0.0030(16) _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 O3 1.9038(19) 2_665 ? Cu1 O1 2.007(2) . ? Cu1 N1 2.089(3) . ? Cu1 N4 2.118(3) 1_655 ? Cu1 O7 2.291(2) . ? Cu1 O2 2.403(2) . ? Cu1 C8 2.529(3) . ? Cu2 O7 1.916(2) . ? Cu2 O7 1.923(2) 3_465 ? Cu2 N3 1.999(3) 3_565 ? Cu2 N2 1.999(3) . ? Cu2 O8 2.303(3) . ? O1 C8 1.278(4) . ? O2 C8 1.241(4) . ? O3 C9 1.277(4) . ? O3 Cu1 1.9039(19) 2_664 ? O4 C9 1.236(4) . ? O5 N6 1.233(3) . ? O6 N6 1.226(3) . ? O7 Cu2 1.923(2) 3_565 ? O7 H7' 0.8498 . ? O8 H8A 0.8500 . ? O8 H8B 0.8500 . ? N1 N2 1.342(4) . ? N1 C1 1.351(4) . ? N2 N3 1.289(4) . ? N3 N4 1.334(4) . ? N3 Cu2 1.999(3) 3_465 ? N4 C1 1.346(4) . ? N4 Cu1 2.118(3) 1_455 ? N5 C1 1.357(4) . ? N5 H5' 0.9000 . ? N5 H5" 0.9000 . ? N6 C6 1.471(4) . ? C2 C7 1.389(4) . ? C2 C3 1.391(4) . ? C2 C8 1.505(4) . ? C3 C4 1.399(4) . ? C3 H3 0.9500 . ? C4 C5 1.383(4) . ? C4 C9 1.523(4) . ? C5 C6 1.389(4) . ? C5 H5D 0.9500 . ? C6 C7 1.389(4) . ? C7 H7 0.9500 . ? O9 H9A 0.8499 . ? O9 H9B 0.8499 . ? O10 H10A 0.8502 . ? O10 H10B 0.8502 . ? 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 O3 Cu1 O1 158.84(8) 2_665 . ? O3 Cu1 N1 91.24(11) 2_665 . ? O1 Cu1 N1 90.49(10) . . ? O3 Cu1 N4 90.31(11) 2_665 1_655 ? O1 Cu1 N4 92.01(10) . 1_655 ? N1 Cu1 N4 168.95(9) . 1_655 ? O3 Cu1 O7 107.86(8) 2_665 . ? O1 Cu1 O7 93.30(8) . . ? N1 Cu1 O7 84.83(10) . . ? N4 Cu1 O7 84.28(10) 1_655 . ? O3 Cu1 O2 99.85(8) 2_665 . ? O1 Cu1 O2 59.00(7) . . ? N1 Cu1 O2 92.76(10) . . ? N4 Cu1 O2 97.76(9) 1_655 . ? O7 Cu1 O2 152.22(7) . . ? O3 Cu1 C8 128.83(9) 2_665 . ? O1 Cu1 C8 30.01(9) . . ? N1 Cu1 C8 92.48(10) . . ? N4 Cu1 C8 95.07(10) 1_655 . ? O7 Cu1 C8 123.30(8) . . ? O2 Cu1 C8 29.00(8) . . ? O7 Cu2 O7 172.34(4) . 3_465 ? O7 Cu2 N3 92.14(10) . 3_565 ? O7 Cu2 N3 87.30(11) 3_465 3_565 ? O7 Cu2 N2 87.95(11) . . ? O7 Cu2 N2 91.73(10) 3_465 . ? N3 Cu2 N2 173.34(13) 3_565 . ? O7 Cu2 O8 89.70(9) . . ? O7 Cu2 O8 97.91(9) 3_465 . ? N3 Cu2 O8 88.09(10) 3_565 . ? N2 Cu2 O8 98.57(10) . . ? C8 O1 Cu1 98.22(17) . . ? C8 O2 Cu1 81.13(17) . . ? C9 O3 Cu1 120.43(18) . 2_664 ? Cu2 O7 Cu2 113.52(10) . 3_565 ? Cu2 O7 Cu1 116.86(11) . . ? Cu2 O7 Cu1 115.07(11) 3_565 . ? Cu2 O7 H7' 110.9 . . ? Cu2 O7 H7' 107.4 3_565 . ? Cu1 O7 H7' 90.1 . . ? Cu2 O8 H8A 107.4 . . ? Cu2 O8 H8B 99.7 . . ? H8A O8 H8B 105.2 . . ? N2 N1 C1 104.2(3) . . ? N2 N1 Cu1 115.6(2) . . ? C1 N1 Cu1 140.0(2) . . ? N3 N2 N1 110.4(3) . . ? N3 N2 Cu2 118.3(2) . . ? N1 N2 Cu2 131.1(2) . . ? N2 N3 N4 110.2(3) . . ? N2 N3 Cu2 118.9(2) . 3_465 ? N4 N3 Cu2 130.8(2) . 3_465 ? N3 N4 C1 104.8(2) . . ? N3 N4 Cu1 115.02(19) . 1_455 ? C1 N4 Cu1 140.2(2) . 1_455 ? C1 N5 H5' 125.1 . . ? C1 N5 H5" 110.5 . . ? H5' N5 H5" 112.9 . . ? O6 N6 O5 123.6(3) . . ? O6 N6 C6 118.6(3) . . ? O5 N6 C6 117.8(2) . . ? N4 C1 N1 110.5(2) . . ? N4 C1 N5 124.9(3) . . ? N1 C1 N5 124.5(3) . . ? C7 C2 C3 119.9(3) . . ? C7 C2 C8 119.1(3) . . ? C3 C2 C8 121.0(3) . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 C9 120.6(3) . . ? C3 C4 C9 119.4(3) . . ? C4 C5 C6 118.3(3) . . ? C4 C5 H5D 120.9 . . ? C6 C5 H5D 120.9 . . ? C5 C6 C7 122.9(3) . . ? C5 C6 N6 119.0(3) . . ? C7 C6 N6 118.1(3) . . ? C6 C7 C2 118.2(3) . . ? C6 C7 H7 120.9 . . ? C2 C7 H7 120.9 . . ? O2 C8 O1 121.6(3) . . ? O2 C8 C2 119.9(3) . . ? O1 C8 C2 118.5(3) . . ? O2 C8 Cu1 69.86(16) . . ? O1 C8 Cu1 51.77(14) . . ? C2 C8 Cu1 170.1(2) . . ? O4 C9 O3 126.6(3) . . ? O4 C9 C4 119.5(3) . . ? O3 C9 C4 113.9(2) . . ? H9A O9 H9B 105.0 . . ? H10A O10 H10B 105.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cu1 O1 C8 0.6(4) 2_665 . . . ? N1 Cu1 O1 C8 -94.1(2) . . . . ? N4 Cu1 O1 C8 96.7(2) 1_655 . . . ? O7 Cu1 O1 C8 -179.0(2) . . . . ? O2 Cu1 O1 C8 -1.18(19) . . . . ? O3 Cu1 O2 C8 -178.1(2) 2_665 . . . ? O1 Cu1 O2 C8 1.22(19) . . . . ? N1 Cu1 O2 C8 90.1(2) . . . . ? N4 Cu1 O2 C8 -86.5(2) 1_655 . . . ? O7 Cu1 O2 C8 6.0(3) . . . . ? O7 Cu2 O7 Cu2 65.3(6) 3_465 . . 3_565 ? N3 Cu2 O7 Cu2 -20.37(12) 3_565 . . 3_565 ? N2 Cu2 O7 Cu2 152.97(13) . . . 3_565 ? O8 Cu2 O7 Cu2 -108.45(11) . . . 3_565 ? O7 Cu2 O7 Cu1 -72.3(6) 3_465 . . . ? N3 Cu2 O7 Cu1 -157.96(12) 3_565 . . . ? N2 Cu2 O7 Cu1 15.38(12) . . . . ? O8 Cu2 O7 Cu1 113.96(11) . . . . ? O3 Cu1 O7 Cu2 -108.41(13) 2_665 . . . ? O1 Cu1 O7 Cu2 71.42(12) . . . . ? N1 Cu1 O7 Cu2 -18.77(12) . . . . ? N4 Cu1 O7 Cu2 163.12(12) 1_655 . . . ? O2 Cu1 O7 Cu2 67.3(2) . . . . ? C8 Cu1 O7 Cu2 70.80(14) . . . . ? O3 Cu1 O7 Cu2 114.65(12) 2_665 . . 3_565 ? O1 Cu1 O7 Cu2 -65.52(12) . . . 3_565 ? N1 Cu1 O7 Cu2 -155.71(12) . . . 3_565 ? N4 Cu1 O7 Cu2 26.18(12) 1_655 . . 3_565 ? O2 Cu1 O7 Cu2 -69.6(2) . . . 3_565 ? C8 Cu1 O7 Cu2 -66.14(15) . . . 3_565 ? O3 Cu1 N1 N2 122.6(2) 2_665 . . . ? O1 Cu1 N1 N2 -78.5(2) . . . . ? N4 Cu1 N1 N2 24.6(6) 1_655 . . . ? O7 Cu1 N1 N2 14.7(2) . . . . ? O2 Cu1 N1 N2 -137.5(2) . . . . ? C8 Cu1 N1 N2 -108.5(2) . . . . ? O3 Cu1 N1 C1 -62.8(3) 2_665 . . . ? O1 Cu1 N1 C1 96.1(3) . . . . ? N4 Cu1 N1 C1 -160.7(4) 1_655 . . . ? O7 Cu1 N1 C1 -170.6(3) . . . . ? O2 Cu1 N1 C1 37.2(3) . . . . ? C8 Cu1 N1 C1 66.2(3) . . . . ? C1 N1 N2 N3 -0.4(4) . . . . ? Cu1 N1 N2 N3 176.1(2) . . . . ? C1 N1 N2 Cu2 174.7(2) . . . . ? Cu1 N1 N2 Cu2 -8.8(4) . . . . ? O7 Cu2 N2 N3 169.8(3) . . . . ? O7 Cu2 N2 N3 -17.9(3) 3_465 . . . ? N3 Cu2 N2 N3 -99.4(11) 3_565 . . . ? O8 Cu2 N2 N3 80.4(3) . . . . ? O7 Cu2 N2 N1 -5.0(3) . . . . ? O7 Cu2 N2 N1 167.3(3) 3_465 . . . ? N3 Cu2 N2 N1 85.8(12) 3_565 . . . ? O8 Cu2 N2 N1 -94.4(3) . . . . ? N1 N2 N3 N4 0.4(4) . . . . ? Cu2 N2 N3 N4 -175.41(18) . . . . ? N1 N2 N3 Cu2 -177.74(18) . . . 3_465 ? Cu2 N2 N3 Cu2 6.5(4) . . . 3_465 ? N2 N3 N4 C1 -0.2(4) . . . . ? Cu2 N3 N4 C1 177.6(2) 3_465 . . . ? N2 N3 N4 Cu1 -179.1(2) . . . 1_455 ? Cu2 N3 N4 Cu1 -1.2(3) 3_465 . . 1_455 ? N3 N4 C1 N1 0.0(3) . . . . ? Cu1 N4 C1 N1 178.3(3) 1_455 . . . ? N3 N4 C1 N5 -176.6(3) . . . . ? Cu1 N4 C1 N5 1.7(5) 1_455 . . . ? N2 N1 C1 N4 0.2(3) . . . . ? Cu1 N1 C1 N4 -174.8(3) . . . . ? N2 N1 C1 N5 176.9(3) . . . . ? Cu1 N1 C1 N5 1.8(5) . . . . ? C7 C2 C3 C4 0.0(5) . . . . ? C8 C2 C3 C4 179.4(3) . . . . ? C2 C3 C4 C5 0.2(5) . . . . ? C2 C3 C4 C9 -179.1(3) . . . . ? C3 C4 C5 C6 -0.3(5) . . . . ? C9 C4 C5 C6 179.1(3) . . . . ? C4 C5 C6 C7 0.1(5) . . . . ? C4 C5 C6 N6 -179.0(3) . . . . ? O6 N6 C6 C5 -178.6(3) . . . . ? O5 N6 C6 C5 1.5(4) . . . . ? O6 N6 C6 C7 2.3(4) . . . . ? O5 N6 C6 C7 -177.6(3) . . . . ? C5 C6 C7 C2 0.1(5) . . . . ? N6 C6 C7 C2 179.2(3) . . . . ? C3 C2 C7 C6 -0.2(5) . . . . ? C8 C2 C7 C6 -179.5(3) . . . . ? Cu1 O2 C8 O1 -1.9(3) . . . . ? Cu1 O2 C8 C2 178.9(3) . . . . ? Cu1 O1 C8 O2 2.3(4) . . . . ? Cu1 O1 C8 C2 -178.5(2) . . . . ? C7 C2 C8 O2 -1.7(5) . . . . ? C3 C2 C8 O2 178.9(3) . . . . ? C7 C2 C8 O1 179.1(3) . . . . ? C3 C2 C8 O1 -0.3(5) . . . . ? C7 C2 C8 Cu1 172.3(12) . . . . ? C3 C2 C8 Cu1 -7.0(15) . . . . ? O3 Cu1 C8 O2 2.4(3) 2_665 . . . ? O1 Cu1 C8 O2 -177.9(3) . . . . ? N1 Cu1 C8 O2 -91.2(2) . . . . ? N4 Cu1 C8 O2 96.9(2) 1_655 . . . ? O7 Cu1 C8 O2 -176.66(18) . . . . ? O3 Cu1 C8 O1 -179.7(2) 2_665 . . . ? N1 Cu1 C8 O1 86.7(2) . . . . ? N4 Cu1 C8 O1 -85.2(2) 1_655 . . . ? O7 Cu1 C8 O1 1.2(2) . . . . ? O2 Cu1 C8 O1 177.9(3) . . . . ? O3 Cu1 C8 C2 -172.1(13) 2_665 . . . ? O1 Cu1 C8 C2 7.6(13) . . . . ? N1 Cu1 C8 C2 94.3(13) . . . . ? N4 Cu1 C8 C2 -77.7(13) 1_655 . . . ? O7 Cu1 C8 C2 8.8(14) . . . . ? O2 Cu1 C8 C2 -174.5(15) . . . . ? Cu1 O3 C9 O4 2.2(5) 2_664 . . . ? Cu1 O3 C9 C4 -178.0(2) 2_664 . . . ? C5 C4 C9 O4 6.3(5) . . . . ? C3 C4 C9 O4 -174.4(3) . . . . ? C5 C4 C9 O3 -173.5(3) . . . . ? C3 C4 C9 O3 5.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.879 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.096 # Attachment '- 1.cif' data_90217c _database_code_depnum_ccdc_archive 'CCDC 826949' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H11 Co2 N6 O9.50' _chemical_formula_weight 473.10 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5160(4) _cell_length_b 10.1804(7) _cell_length_c 12.0390(8) _cell_angle_alpha 102.9130(10) _cell_angle_beta 105.2700(10) _cell_angle_gamma 93.2140(10) _cell_volume 745.30(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3900 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description BLOCK _exptl_crystal_colour RED _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 474 _exptl_absorpt_coefficient_mu 2.296 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6087 _exptl_absorpt_correction_T_max 0.6320 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3774 _diffrn_reflns_av_R_equivalents 0.0079 _diffrn_reflns_av_sigmaI/netI 0.0136 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2591 _reflns_number_gt 2458 _reflns_threshold_expression >2sigma(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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0239P)^2^+1.5171P] 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 2591 _refine_ls_number_parameters 254 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.68179(6) 0.92563(4) 0.96389(3) 0.01618(11) Uani 1 1 d . . . Co2 Co 0.42338(6) 1.04906(4) 0.75910(3) 0.01731(11) Uani 1 1 d . . . O1 O 0.3418(3) 0.8682(2) 0.62804(19) 0.0284(5) Uani 1 1 d . . . O2 O 0.4409(3) 0.8180(2) 0.80175(18) 0.0317(5) Uani 1 1 d . . . O3 O 0.5157(18) 0.3202(15) 0.8077(7) 0.034(5) Uani 0.192(16) 1 d PDU A 1 O3' O 0.4036(13) 0.3341(5) 0.8180(3) 0.082(2) Uani 0.808(16) 1 d PDU A 2 O4 O 0.3708(4) 0.1765(3) 0.6520(3) 0.0520(8) Uani 1 1 d . . . O5 O 0.0957(5) 0.2960(3) 0.2742(2) 0.0530(7) Uani 1 1 d . . . O6 O 0.1112(5) 0.5049(3) 0.2659(2) 0.0507(7) Uani 1 1 d . . . O7 O 0.5283(3) 1.09472(18) 0.93916(16) 0.0170(4) Uani 1 1 d D . . H7' H 0.6127 1.1682 0.9700 0.026 Uiso 1 1 d RD . . O8 O 0.7798(6) 0.7366(3) 0.9754(3) 0.0691(10) Uani 1 1 d . . . H8A H 0.7837 0.7230 1.0523 0.104 Uiso 1 1 d R . . H8B H 0.9202 0.7333 0.9644 0.104 Uiso 1 1 d R . . N1 N 0.7597(4) 1.0281(2) 0.7642(2) 0.0203(5) Uani 1 1 d . . . N2 N 0.8686(4) 0.9921(2) 0.8626(2) 0.0183(5) Uani 1 1 d . . . N3 N 1.0720(4) 1.0002(2) 0.87049(19) 0.0186(5) Uani 1 1 d . . . N4 N 1.1036(4) 1.0387(2) 0.7756(2) 0.0194(5) Uani 1 1 d . . . N5 N 0.8722(5) 1.0942(4) 0.6090(2) 0.0420(8) Uani 1 1 d . . . H5A H 0.9770 1.1105 0.5812 0.050 Uiso 1 1 calc R . . H5B H 0.7437 1.1029 0.5715 0.050 Uiso 1 1 calc R . . N6 N 0.1371(4) 0.4174(3) 0.3211(2) 0.0318(6) Uani 1 1 d . . . C1 C 0.9093(4) 1.0547(3) 0.7119(2) 0.0202(6) Uani 1 1 d . . . C2 C 0.3327(4) 0.6358(3) 0.6289(3) 0.0206(6) Uani 1 1 d . . . C3 C 0.3705(5) 0.5382(3) 0.6930(3) 0.0268(7) Uani 1 1 d . . . H3 H 0.4205 0.5649 0.7755 0.032 Uiso 1 1 calc R . . C4 C 0.3348(5) 0.4008(3) 0.6361(3) 0.0303(7) Uani 1 1 d . A . C5 C 0.2588(5) 0.3606(3) 0.5134(3) 0.0281(7) Uani 1 1 d . . . H5 H 0.2346 0.2691 0.4739 0.034 Uiso 1 1 calc R . . C6 C 0.2200(4) 0.4593(3) 0.4511(3) 0.0226(6) Uani 1 1 d . . . C7 C 0.2559(4) 0.5963(3) 0.5052(3) 0.0201(6) Uani 1 1 d . . . H7 H 0.2297 0.6604 0.4606 0.024 Uiso 1 1 calc R . . C8 C 0.3754(4) 0.7837(3) 0.6902(3) 0.0220(6) Uani 1 1 d . . . C9 C 0.3803(6) 0.2974(4) 0.7094(3) 0.0508(11) Uani 1 1 d D . . O9 O 0.1718(7) 0.6645(5) -0.0202(4) 0.1210(17) Uani 1 1 d DU . . H9A H 0.2115 0.5954 -0.0597 0.182 Uiso 1 1 d RD . . H9B H 0.1397 0.6565 0.0422 0.182 Uiso 1 1 d RD . . O10 O 0.3656(17) 0.4655(8) 0.9899(8) 0.104(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0156(2) 0.0199(2) 0.01448(19) 0.00671(14) 0.00420(14) 0.00415(14) Co2 0.0166(2) 0.0214(2) 0.01425(19) 0.00572(15) 0.00379(14) 0.00274(15) O1 0.0336(12) 0.0189(10) 0.0299(11) 0.0063(9) 0.0039(9) 0.0028(9) O2 0.0289(12) 0.0372(13) 0.0221(11) -0.0011(9) 0.0045(9) -0.0045(10) O3 0.023(6) 0.046(6) 0.044(6) 0.022(4) 0.013(4) 0.019(4) O3' 0.104(5) 0.069(3) 0.062(3) 0.051(2) -0.019(2) -0.015(3) O4 0.0487(16) 0.0397(16) 0.095(2) 0.0465(16) 0.0388(16) 0.0211(12) O5 0.0685(19) 0.0317(14) 0.0436(15) -0.0130(12) 0.0110(14) -0.0044(13) O6 0.0699(19) 0.0467(16) 0.0275(13) 0.0087(12) 0.0010(12) 0.0052(14) O7 0.0178(9) 0.0166(9) 0.0165(9) 0.0055(7) 0.0034(7) 0.0006(7) O8 0.082(2) 0.0370(16) 0.063(2) -0.0013(14) -0.0161(17) 0.0310(15) N1 0.0169(12) 0.0288(13) 0.0164(11) 0.0094(10) 0.0034(9) 0.0034(10) N2 0.0152(11) 0.0247(12) 0.0158(11) 0.0073(9) 0.0032(9) 0.0042(9) N3 0.0153(11) 0.0251(13) 0.0164(11) 0.0073(9) 0.0047(9) 0.0025(9) N4 0.0161(11) 0.0283(13) 0.0153(11) 0.0084(10) 0.0043(9) 0.0024(9) N5 0.0254(14) 0.080(2) 0.0288(15) 0.0336(15) 0.0042(12) 0.0046(14) N6 0.0267(14) 0.0321(16) 0.0308(15) -0.0012(12) 0.0067(11) 0.0006(11) C1 0.0183(14) 0.0260(15) 0.0163(13) 0.0069(11) 0.0036(11) 0.0016(11) C2 0.0170(14) 0.0210(14) 0.0235(14) 0.0062(11) 0.0049(11) 0.0018(11) C3 0.0256(16) 0.0300(16) 0.0256(15) 0.0134(13) 0.0038(12) 0.0007(12) C4 0.0234(16) 0.0267(16) 0.0430(19) 0.0205(14) 0.0038(14) 0.0016(12) C5 0.0218(15) 0.0171(15) 0.0451(19) 0.0071(13) 0.0092(14) 0.0025(12) C6 0.0175(14) 0.0225(15) 0.0259(15) 0.0025(12) 0.0060(12) 0.0018(11) C7 0.0183(14) 0.0199(14) 0.0235(14) 0.0094(11) 0.0047(11) 0.0031(11) C8 0.0158(14) 0.0228(15) 0.0248(16) 0.0021(12) 0.0051(11) 0.0000(11) C9 0.040(2) 0.039(2) 0.075(3) 0.040(2) -0.001(2) -0.0034(17) O9 0.090(3) 0.133(3) 0.108(3) -0.030(3) 0.032(2) -0.018(3) O10 0.156(9) 0.070(5) 0.086(6) 0.024(4) 0.035(6) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O7 2.0484(19) 2_677 ? Co1 O7 2.0779(18) . ? Co1 O8 2.084(3) . ? Co1 N2 2.118(2) . ? Co1 N3 2.151(2) 2_777 ? Co1 O2 2.171(2) . ? Co2 O4 2.007(2) 1_565 ? Co2 O7 2.0288(18) . ? Co2 O1 2.077(2) . ? Co2 N4 2.143(2) 1_455 ? Co2 N1 2.200(2) . ? O1 C8 1.253(4) . ? O2 C8 1.257(4) . ? O3 C9 1.2393(11) . ? O3' C9 1.2418(11) . ? O4 C9 1.259(5) . ? O4 Co2 2.007(2) 1_545 ? O5 N6 1.220(4) . ? O6 N6 1.219(4) . ? O7 Co1 2.0484(18) 2_677 ? O7 H7' 0.8499 . ? O8 H8A 0.9600 . ? O8 H8B 0.9600 . ? N1 C1 1.338(4) . ? N1 N2 1.350(3) . ? N2 N3 1.300(3) . ? N3 N4 1.348(3) . ? N3 Co1 2.151(2) 2_777 ? N4 C1 1.336(4) . ? N4 Co2 2.143(2) 1_655 ? N5 C1 1.352(4) . ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? N6 C6 1.467(4) . ? C2 C3 1.384(4) . ? C2 C7 1.395(4) . ? C2 C8 1.496(4) . ? C3 C4 1.389(5) . ? C3 H3 0.9300 . ? C4 C5 1.385(5) . ? C4 C9 1.512(4) . ? C5 C6 1.379(4) . ? C5 H5 0.9300 . ? C6 C7 1.379(4) . ? C7 H7 0.9300 . ? O9 H9A 0.8507 . ? O9 H9B 0.8504 . ? O10 O10 1.78(2) 2_667 ? 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 O7 Co1 O7 82.94(7) 2_677 . ? O7 Co1 O8 91.22(13) 2_677 . ? O7 Co1 O8 169.52(11) . . ? O7 Co1 N2 166.05(8) 2_677 . ? O7 Co1 N2 83.23(8) . . ? O8 Co1 N2 102.73(13) . . ? O7 Co1 N3 87.76(8) 2_677 2_777 ? O7 Co1 N3 103.94(8) . 2_777 ? O8 Co1 N3 84.45(10) . 2_777 ? N2 Co1 N3 93.76(9) . 2_777 ? O7 Co1 O2 90.39(8) 2_677 . ? O7 Co1 O2 84.96(8) . . ? O8 Co1 O2 86.39(10) . . ? N2 Co1 O2 90.25(9) . . ? N3 Co1 O2 170.61(9) 2_777 . ? O4 Co2 O7 128.49(11) 1_565 . ? O4 Co2 O1 97.79(11) 1_565 . ? O7 Co2 O1 133.71(8) . . ? O4 Co2 N4 94.10(10) 1_565 1_455 ? O7 Co2 N4 87.36(8) . 1_455 ? O1 Co2 N4 90.30(9) . 1_455 ? O4 Co2 N1 97.78(10) 1_565 . ? O7 Co2 N1 85.93(8) . . ? O1 Co2 N1 87.24(9) . . ? N4 Co2 N1 168.08(9) 1_455 . ? C8 O1 Co2 100.74(18) . . ? C8 O2 Co1 149.9(2) . . ? C9 O4 Co2 111.8(3) . 1_545 ? Co2 O7 Co1 120.23(9) . 2_677 ? Co2 O7 Co1 100.21(8) . . ? Co1 O7 Co1 97.06(7) 2_677 . ? Co2 O7 H7' 114.0 . . ? Co1 O7 H7' 111.0 2_677 . ? Co1 O7 H7' 112.1 . . ? Co1 O8 H8A 109.4 . . ? Co1 O8 H8B 109.3 . . ? H8A O8 H8B 109.5 . . ? C1 N1 N2 104.5(2) . . ? C1 N1 Co2 142.43(19) . . ? N2 N1 Co2 112.28(16) . . ? N3 N2 N1 110.1(2) . . ? N3 N2 Co1 133.65(17) . . ? N1 N2 Co1 116.18(16) . . ? N2 N3 N4 109.1(2) . . ? N2 N3 Co1 123.06(17) . 2_777 ? N4 N3 Co1 116.69(17) . 2_777 ? C1 N4 N3 105.3(2) . . ? C1 N4 Co2 137.18(19) . 1_655 ? N3 N4 Co2 117.46(17) . 1_655 ? C1 N5 H5A 120.0 . . ? C1 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? O6 N6 O5 123.5(3) . . ? O6 N6 C6 118.7(3) . . ? O5 N6 C6 117.8(3) . . ? N4 C1 N1 111.0(2) . . ? N4 C1 N5 123.8(3) . . ? N1 C1 N5 125.2(3) . . ? C3 C2 C7 119.8(3) . . ? C3 C2 C8 120.9(3) . . ? C7 C2 C8 119.3(3) . . ? C2 C3 C4 121.0(3) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.6(3) . . ? C5 C4 C9 121.0(3) . . ? C3 C4 C9 119.4(3) . . ? C6 C5 C4 118.5(3) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C7 C6 C5 123.0(3) . . ? C7 C6 N6 118.1(3) . . ? C5 C6 N6 118.8(3) . . ? C6 C7 C2 118.0(3) . . ? C6 C7 H7 121.0 . . ? C2 C7 H7 121.0 . . ? O1 C8 O2 122.8(3) . . ? O1 C8 C2 118.5(3) . . ? O2 C8 C2 118.7(3) . . ? O3 C9 O3' 37.0(6) . . ? O3 C9 O4 110.9(8) . . ? O3' C9 O4 124.9(4) . . ? O3 C9 C4 123.9(8) . . ? O3' C9 C4 118.8(4) . . ? O4 C9 C4 115.9(3) . . ? H9A O9 H9B 117.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Co2 O1 C8 178.88(18) 1_565 . . . ? O7 Co2 O1 C8 -0.3(2) . . . . ? N4 Co2 O1 C8 -86.94(18) 1_455 . . . ? N1 Co2 O1 C8 81.40(18) . . . . ? O7 Co1 O2 C8 166.1(4) 2_677 . . . ? O7 Co1 O2 C8 83.2(4) . . . . ? O8 Co1 O2 C8 -102.7(4) . . . . ? N2 Co1 O2 C8 0.0(4) . . . . ? N3 Co1 O2 C8 -115.3(6) 2_777 . . . ? O4 Co2 O7 Co1 104.14(13) 1_565 . . 2_677 ? O1 Co2 O7 Co1 -76.90(14) . . . 2_677 ? N4 Co2 O7 Co1 11.00(11) 1_455 . . 2_677 ? N1 Co2 O7 Co1 -159.15(11) . . . 2_677 ? O4 Co2 O7 Co1 -151.42(10) 1_565 . . . ? O1 Co2 O7 Co1 27.55(14) . . . . ? N4 Co2 O7 Co1 115.44(9) 1_455 . . . ? N1 Co2 O7 Co1 -54.70(9) . . . . ? O7 Co1 O7 Co2 -122.54(10) 2_677 . . . ? O8 Co1 O7 Co2 -66.0(6) . . . . ? N2 Co1 O7 Co2 59.34(9) . . . . ? N3 Co1 O7 Co2 151.55(8) 2_777 . . . ? O2 Co1 O7 Co2 -31.51(8) . . . . ? O7 Co1 O7 Co1 0.0 2_677 . . 2_677 ? O8 Co1 O7 Co1 56.6(6) . . . 2_677 ? N2 Co1 O7 Co1 -178.12(9) . . . 2_677 ? N3 Co1 O7 Co1 -85.91(8) 2_777 . . 2_677 ? O2 Co1 O7 Co1 91.02(8) . . . 2_677 ? O4 Co2 N1 C1 -12.0(3) 1_565 . . . ? O7 Co2 N1 C1 -140.3(3) . . . . ? O1 Co2 N1 C1 85.5(3) . . . . ? N4 Co2 N1 C1 163.8(4) 1_455 . . . ? O4 Co2 N1 N2 155.9(2) 1_565 . . . ? O7 Co2 N1 N2 27.56(18) . . . . ? O1 Co2 N1 N2 -106.63(19) . . . . ? N4 Co2 N1 N2 -28.4(5) 1_455 . . . ? C1 N1 N2 N3 1.6(3) . . . . ? Co2 N1 N2 N3 -170.78(17) . . . . ? C1 N1 N2 Co1 -175.08(18) . . . . ? Co2 N1 N2 Co1 12.5(2) . . . . ? O7 Co1 N2 N3 130.9(3) 2_677 . . . ? O7 Co1 N2 N3 138.7(3) . . . . ? O8 Co1 N2 N3 -50.0(3) . . . . ? N3 Co1 N2 N3 35.1(3) 2_777 . . . ? O2 Co1 N2 N3 -136.4(3) . . . . ? O7 Co1 N2 N1 -53.3(4) 2_677 . . . ? O7 Co1 N2 N1 -45.59(19) . . . . ? O8 Co1 N2 N1 125.7(2) . . . . ? N3 Co1 N2 N1 -149.19(19) 2_777 . . . ? O2 Co1 N2 N1 39.30(19) . . . . ? N1 N2 N3 N4 -1.5(3) . . . . ? Co1 N2 N3 N4 174.41(19) . . . . ? N1 N2 N3 Co1 140.90(19) . . . 2_777 ? Co1 N2 N3 Co1 -43.2(3) . . . 2_777 ? N2 N3 N4 C1 0.7(3) . . . . ? Co1 N3 N4 C1 -144.35(19) 2_777 . . . ? N2 N3 N4 Co2 -176.42(17) . . . 1_655 ? Co1 N3 N4 Co2 38.5(2) 2_777 . . 1_655 ? N3 N4 C1 N1 0.3(3) . . . . ? Co2 N4 C1 N1 176.6(2) 1_655 . . . ? N3 N4 C1 N5 179.6(3) . . . . ? Co2 N4 C1 N5 -4.1(5) 1_655 . . . ? N2 N1 C1 N4 -1.1(3) . . . . ? Co2 N1 C1 N4 167.3(2) . . . . ? N2 N1 C1 N5 179.6(3) . . . . ? Co2 N1 C1 N5 -12.0(5) . . . . ? C7 C2 C3 C4 0.6(5) . . . . ? C8 C2 C3 C4 -178.8(3) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? C2 C3 C4 C9 179.3(3) . . . . ? C3 C4 C5 C6 -0.2(5) . . . . ? C9 C4 C5 C6 180.0(3) . . . . ? C4 C5 C6 C7 0.8(4) . . . . ? C4 C5 C6 N6 -179.3(3) . . . . ? O6 N6 C6 C7 2.8(4) . . . . ? O5 N6 C6 C7 -176.5(3) . . . . ? O6 N6 C6 C5 -177.0(3) . . . . ? O5 N6 C6 C5 3.6(4) . . . . ? C5 C6 C7 C2 -0.7(4) . . . . ? N6 C6 C7 C2 179.4(2) . . . . ? C3 C2 C7 C6 0.0(4) . . . . ? C8 C2 C7 C6 179.4(3) . . . . ? Co2 O1 C8 O2 0.2(3) . . . . ? Co2 O1 C8 C2 179.3(2) . . . . ? Co1 O2 C8 O1 -59.6(5) . . . . ? Co1 O2 C8 C2 121.3(4) . . . . ? C3 C2 C8 O1 178.9(3) . . . . ? C7 C2 C8 O1 -0.4(4) . . . . ? C3 C2 C8 O2 -2.0(4) . . . . ? C7 C2 C8 O2 178.7(3) . . . . ? Co2 O4 C9 O3 34.2(9) 1_545 . . . ? Co2 O4 C9 O3' -5.0(7) 1_545 . . . ? Co2 O4 C9 C4 -177.8(2) 1_545 . . . ? C5 C4 C9 O3 152.0(9) . . . . ? C3 C4 C9 O3 -27.8(10) . . . . ? C5 C4 C9 O3' -164.8(5) . . . . ? C3 C4 C9 O3' 15.4(6) . . . . ? C5 C4 C9 O4 8.5(5) . . . . ? C3 C4 C9 O4 -171.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.662 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.069