Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Murray, Keith' 'Batten, S.' 'Jensen, Paul' 'Moubaraki, Boujemaa' _publ_contact_author_name 'Prof Keith Murray' _publ_contact_author_address ; School of Chemistry Monash University School of Chemistry PO Box 23 Monash University Vic 3800 AUSTRALIA ; _publ_contact_author_email 'KEITH.S.MURRAY@SCI.MONASH.EDU.AU' _publ_section_title ; Syntheses, crystal structures, and magnetic properties of first row transition metal coordination polymers containing dicyanamide and 4,4'bipyridine ; data_1_123 _database_code_CSD 172403 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Fe(dca)2(4,4'-bipy) _chemical_formula_sum 'C14 H8 Fe N8' _chemical_formula_weight 344.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Fe' 'Fe' 0.3463 0.8444 '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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.6367(2) _cell_length_b 16.8457(4) _cell_length_c 11.5033(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.010(2) _cell_angle_gamma 90.00 _cell_volume 1673.63(6) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 25078 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.30 _exptl_crystal_description Prismatic _exptl_crystal_colour Orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.911 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_T_max 0.931 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _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 25078 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7574 _reflns_number_gt 6697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett and Johnson, 1996)' _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^)+(0.0292P)^2^+0.3461P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 7574 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.11215(3) 0.5000 0.01596(13) Uani 1 1 d . . . Fe2 Fe 0.67420(4) 0.61050(3) 0.49969(13) 0.01615(13) Uani 1 1 d . . . N1 N 0.5550(4) 0.23632(17) 0.4915(4) 0.0264(7) Uani 1 1 d . . . N2 N 0.7281(7) 0.3465(3) 0.4422(6) 0.107(3) Uani 1 1 d . . . N3 N 0.7069(4) 0.48566(15) 0.4949(4) 0.0255(7) Uani 1 1 d . . . N4 N 0.4692(4) -0.01336(16) 0.4995(4) 0.0271(8) Uani 1 1 d . . . N5 N 0.4518(5) -0.1545(2) 0.4546(4) 0.0613(16) Uani 1 1 d . . . N6 N 0.6317(4) -0.26341(17) 0.4949(4) 0.0306(8) Uani 1 1 d . . . N7 N 0.2561(4) 0.1313(2) 0.5031(6) 0.0257(8) Uani 1 1 d . . . N8 N 0.0033(5) 0.1248(4) 0.5966(4) 0.094(2) Uani 1 1 d . . . N9 N -0.2530(4) 0.0976(2) 0.5122(5) 0.0291(10) Uani 1 1 d . . . N10 N 0.4272(4) 0.5954(2) 0.5032(5) 0.0313(8) Uani 1 1 d . . . N11 N 0.1860(4) 0.6662(2) 0.5497(4) 0.0606(14) Uani 1 1 d . . . N12 N -0.0820(4) 0.6330(2) 0.5036(5) 0.0256(7) Uani 1 1 d . . . N13 N 0.4968(7) 0.1116(2) 0.3104(4) 0.0226(11) Uani 1 1 d . . . N14 N 0.4930(7) 0.1148(2) -0.3069(4) 0.0205(10) Uani 1 1 d . . . N15 N 0.6685(7) 0.6118(2) 0.3110(4) 0.0231(11) Uani 1 1 d . . . N16 N 0.6712(7) 0.6105(2) -0.3102(4) 0.0242(12) Uani 1 1 d . . . C1 C 0.6321(6) 0.2899(2) 0.4720(4) 0.0394(14) Uani 1 1 d . . . C2 C 0.7089(5) 0.4190(3) 0.4724(4) 0.0357(13) Uani 1 1 d . . . C3 C 0.4698(5) -0.0794(2) 0.4809(5) 0.0333(12) Uani 1 1 d . . . C4 C 0.5557(6) -0.2089(2) 0.4783(5) 0.0358(13) Uani 1 1 d . . . C5 C 0.1332(6) 0.1294(3) 0.5410(4) 0.0388(13) Uani 1 1 d . . . C6 C -0.1299(7) 0.1118(3) 0.5438(5) 0.0370(15) Uani 1 1 d . . . C7 C 0.3090(7) 0.6244(3) 0.5244(5) 0.0347(17) Uani 1 1 d . . . C8 C 0.0456(4) 0.6435(3) 0.5205(5) 0.0340(14) Uani 1 1 d . . . C9 C 0.6134(5) 0.1412(3) 0.2468(4) 0.0287(10) Uani 1 1 d . . . H9 H 0.7016 0.1612 0.2863 0.034 Uiso 1 1 calc R . . C10 C 0.6119(5) 0.1440(3) 0.1267(4) 0.0302(11) Uani 1 1 d . . . H10 H 0.6987 0.1654 0.0867 0.036 Uiso 1 1 calc R . . C11 C 0.4867(9) 0.1164(3) 0.0636(5) 0.0233(15) Uani 1 1 d . . . C12 C 0.4823(10) 0.1164(3) -0.0659(5) 0.0249(16) Uani 1 1 d . . . C13 C 0.5852(6) 0.1661(3) -0.1270(4) 0.0304(12) Uani 1 1 d . . . H13 H 0.6532 0.2009 -0.0867 0.036 Uiso 1 1 calc R . . C14 C 0.5847(5) 0.1629(3) -0.2466(4) 0.0266(10) Uani 1 1 d . . . H14 H 0.6532 0.1968 -0.2880 0.032 Uiso 1 1 calc R . . C15 C 0.3930(6) 0.0686(3) -0.2494(4) 0.0295(10) Uani 1 1 d . . . H15 H 0.3258 0.0348 -0.2921 0.035 Uiso 1 1 calc R . . C16 C 0.3850(6) 0.0687(3) -0.1297(4) 0.0325(12) Uani 1 1 d . . . H16 H 0.3120 0.0357 -0.0912 0.039 Uiso 1 1 calc R . . C17 C 0.3661(6) 0.0844(3) 0.1290(4) 0.0316(11) Uani 1 1 d . . . H17 H 0.2782 0.0625 0.0911 0.038 Uiso 1 1 calc R . . C18 C 0.3742(5) 0.0844(3) 0.2485(4) 0.0286(9) Uani 1 1 d . . . H18 H 0.2882 0.0641 0.2905 0.034 Uiso 1 1 calc R . . C19 C 0.7535(5) 0.6618(3) 0.2475(4) 0.0295(12) Uani 1 1 d . . . H19 H 0.8187 0.6980 0.2876 0.035 Uiso 1 1 calc R . . C20 C 0.7533(6) 0.6644(3) 0.1275(4) 0.0297(12) Uani 1 1 d . . . H20 H 0.8163 0.7020 0.0880 0.036 Uiso 1 1 calc R . . C21 C 0.6607(9) 0.6120(3) 0.0641(5) 0.0215(15) Uani 1 1 d . . . C22 C 0.6619(9) 0.6133(3) -0.0651(5) 0.0196(15) Uani 1 1 d . . . C23 C 0.7282(6) 0.6738(3) -0.1300(4) 0.0321(12) Uani 1 1 d . . . H23 H 0.7728 0.7180 -0.0912 0.039 Uiso 1 1 calc R . . C24 C 0.7306(6) 0.6708(3) -0.2476(4) 0.0285(11) Uani 1 1 d . . . H24 H 0.7768 0.7137 -0.2884 0.034 Uiso 1 1 calc R . . C25 C 0.6036(6) 0.5514(2) -0.2494(4) 0.0308(11) Uani 1 1 d . . . H25 H 0.5588 0.5084 -0.2910 0.037 Uiso 1 1 calc R . . C26 C 0.5966(6) 0.5505(3) -0.1294(4) 0.0293(12) Uani 1 1 d . . . H26 H 0.5479 0.5076 -0.0903 0.035 Uiso 1 1 calc R . . C27 C 0.5699(6) 0.5612(3) 0.1283(4) 0.0263(11) Uani 1 1 d . . . H27 H 0.5021 0.5252 0.0904 0.032 Uiso 1 1 calc R . . C28 C 0.5780(5) 0.5630(2) 0.2477(4) 0.0245(10) Uani 1 1 d . . . H28 H 0.5144 0.5267 0.2891 0.029 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0151(3) 0.0170(3) 0.0157(3) -0.0010(3) -0.0002(6) 0.00013(19) Fe2 0.0164(3) 0.0163(3) 0.0158(3) 0.0007(3) 0.0000(6) 0.00025(19) N1 0.0296(18) 0.0193(15) 0.0304(17) -0.0021(17) 0.004(2) -0.0036(13) N2 0.101(5) 0.029(2) 0.191(7) -0.028(3) 0.090(5) -0.031(3) N3 0.031(2) 0.0187(16) 0.0272(15) -0.0020(18) -0.001(2) -0.0022(14) N4 0.030(2) 0.0211(17) 0.0301(15) 0.000(2) 0.001(2) 0.0014(14) N5 0.032(2) 0.0220(19) 0.130(5) -0.011(2) -0.035(3) 0.0024(17) N6 0.039(2) 0.0238(15) 0.0286(16) 0.0018(19) -0.001(3) 0.0044(14) N7 0.0143(19) 0.0326(19) 0.0302(19) 0.001(3) 0.005(2) 0.0030(17) N8 0.015(2) 0.221(7) 0.046(3) -0.033(3) 0.0053(18) -0.019(3) N9 0.0133(19) 0.041(2) 0.033(3) -0.0060(19) 0.0009(18) 0.0049(15) N10 0.020(2) 0.0410(19) 0.0331(18) 0.002(3) 0.002(3) -0.0021(16) N11 0.0202(17) 0.044(2) 0.118(4) -0.042(2) -0.0126(19) 0.0006(17) N12 0.026(2) 0.0224(16) 0.0285(18) 0.005(2) 0.003(2) 0.0029(17) N13 0.015(2) 0.028(2) 0.026(3) 0.0009(17) -0.005(3) -0.0054(14) N14 0.030(2) 0.023(2) 0.009(2) -0.0026(15) 0.001(2) -0.0053(14) N15 0.022(2) 0.019(2) 0.027(3) -0.0004(16) -0.007(3) -0.0059(14) N16 0.030(3) 0.024(2) 0.018(3) 0.0012(16) -0.002(3) -0.0024(15) C1 0.038(3) 0.021(2) 0.059(4) -0.0075(18) 0.022(2) 0.0013(19) C2 0.029(3) 0.025(2) 0.052(4) -0.0035(19) 0.015(2) -0.005(2) C3 0.028(2) 0.020(2) 0.052(4) -0.004(2) -0.005(2) 0.0024(18) C4 0.033(2) 0.020(2) 0.054(4) -0.0052(19) -0.007(2) 0.0001(18) C5 0.029(3) 0.069(3) 0.019(2) -0.0097(19) -0.0057(17) -0.004(2) C6 0.013(2) 0.056(4) 0.043(3) -0.0118(19) 0.008(2) -0.0011(19) C7 0.017(2) 0.043(2) 0.044(5) -0.002(2) -0.0080(19) -0.0095(18) C8 0.018(2) 0.0185(17) 0.065(4) -0.011(2) -0.001(2) -0.0019(13) C9 0.029(2) 0.042(2) 0.015(2) -0.0028(17) -0.0036(17) -0.0100(19) C10 0.024(2) 0.044(3) 0.022(3) 0.0018(18) 0.0025(17) -0.019(2) C11 0.017(3) 0.038(3) 0.014(4) 0.0002(19) 0.005(2) -0.006(2) C12 0.025(4) 0.021(3) 0.028(4) 0.0018(19) 0.009(3) -0.002(2) C13 0.039(3) 0.032(2) 0.020(2) -0.0027(16) -0.0005(17) -0.0099(19) C14 0.024(2) 0.035(2) 0.020(2) 0.0033(16) -0.0009(16) -0.0091(17) C15 0.036(2) 0.036(2) 0.017(2) -0.0012(16) 0.0009(18) -0.015(2) C16 0.041(3) 0.037(2) 0.020(3) 0.0009(16) 0.0011(18) -0.021(2) C17 0.027(2) 0.045(3) 0.022(3) 0.0024(17) -0.0013(17) -0.015(2) C18 0.025(2) 0.038(2) 0.023(2) -0.0017(18) 0.0037(17) -0.0137(19) C19 0.037(3) 0.034(3) 0.018(3) 0.0016(17) -0.0048(18) -0.0148(18) C20 0.032(2) 0.038(3) 0.020(3) -0.0003(17) 0.0063(17) -0.0188(19) C21 0.024(3) 0.025(3) 0.015(4) -0.0022(16) 0.003(2) -0.0044(19) C22 0.026(4) 0.018(3) 0.015(4) -0.0036(15) 0.007(2) -0.0032(18) C23 0.046(3) 0.024(2) 0.027(3) 0.0020(17) 0.002(2) -0.014(2) C24 0.037(2) 0.025(2) 0.023(3) 0.0018(17) -0.0056(18) -0.0137(17) C25 0.050(3) 0.022(2) 0.021(2) 0.0003(16) 0.001(2) -0.0084(18) C26 0.043(3) 0.027(2) 0.018(2) -0.0001(15) 0.0043(18) -0.0144(19) C27 0.029(2) 0.028(2) 0.022(2) 0.0015(15) -0.0006(16) -0.0113(18) C28 0.026(2) 0.028(2) 0.019(2) 0.0035(15) 0.0007(16) -0.0147(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N4 2.131(3) . ? Fe1 N7 2.132(3) . ? Fe1 N1 2.147(3) . ? Fe1 N9 2.152(4) 1_655 ? Fe1 N13 2.182(5) . ? Fe1 N14 2.222(4) 1_556 ? Fe2 N3 2.123(3) . ? Fe2 N12 2.140(3) 1_655 ? Fe2 N10 2.149(4) . ? Fe2 N6 2.156(3) 1_565 ? Fe2 N15 2.171(5) . ? Fe2 N16 2.187(5) 1_556 ? N1 C1 1.143(5) . ? N2 C2 1.281(6) . ? N2 C1 1.311(6) . ? N3 C2 1.152(5) . ? N4 C3 1.132(5) . ? N5 C3 1.311(5) . ? N5 C4 1.312(5) . ? N6 C4 1.144(5) . ? N6 Fe2 2.156(3) 1_545 ? N7 C5 1.148(6) . ? N8 C5 1.294(7) . ? N8 C6 1.319(7) . ? N9 C6 1.149(7) . ? N9 Fe1 2.152(4) 1_455 ? N10 C7 1.158(7) . ? N11 C7 1.308(7) . ? N11 C8 1.315(5) . ? N12 C8 1.133(5) . ? N12 Fe2 2.140(3) 1_455 ? N13 C9 1.340(7) . ? N13 C18 1.355(7) . ? N14 C14 1.329(6) . ? N14 C15 1.338(6) . ? N14 Fe1 2.222(4) 1_554 ? N15 C19 1.335(6) . ? N15 C28 1.348(6) . ? N16 C24 1.346(6) . ? N16 C25 1.349(6) . ? N16 Fe2 2.187(5) 1_554 ? C9 C10 1.382(6) . ? C10 C11 1.383(8) . ? C11 C17 1.394(8) . ? C11 C12 1.490(6) . ? C12 C16 1.375(8) . ? C12 C13 1.409(8) . ? C13 C14 1.377(7) . ? C15 C16 1.378(7) . ? C17 C18 1.377(7) . ? C19 C20 1.381(7) . ? C20 C21 1.397(8) . ? C21 C27 1.376(7) . ? C21 C22 1.487(5) . ? C22 C23 1.387(7) . ? C22 C26 1.408(7) . ? C23 C24 1.354(7) . ? C25 C26 1.382(7) . ? C27 C28 1.375(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N7 91.56(13) . . ? N4 Fe1 N1 173.72(14) . . ? N7 Fe1 N1 94.12(13) . . ? N4 Fe1 N9 90.60(13) . 1_655 ? N7 Fe1 N9 174.81(19) . 1_655 ? N1 Fe1 N9 83.97(12) . 1_655 ? N4 Fe1 N13 89.53(17) . . ? N7 Fe1 N13 90.3(2) . . ? N1 Fe1 N13 87.76(16) . . ? N9 Fe1 N13 94.4(2) 1_655 . ? N4 Fe1 N14 91.08(17) . 1_556 ? N7 Fe1 N14 87.3(2) . 1_556 ? N1 Fe1 N14 91.86(17) . 1_556 ? N9 Fe1 N14 87.9(2) 1_655 1_556 ? N13 Fe1 N14 177.55(14) . 1_556 ? N3 Fe2 N12 92.57(12) . 1_655 ? N3 Fe2 N10 90.86(13) . . ? N12 Fe2 N10 175.93(16) 1_655 . ? N3 Fe2 N6 176.35(17) . 1_565 ? N12 Fe2 N6 89.64(13) 1_655 1_565 ? N10 Fe2 N6 87.04(12) . 1_565 ? N3 Fe2 N15 89.27(16) . . ? N12 Fe2 N15 92.4(2) 1_655 . ? N10 Fe2 N15 89.8(2) . . ? N6 Fe2 N15 87.73(16) 1_565 . ? N3 Fe2 N16 91.56(16) . 1_556 ? N12 Fe2 N16 89.5(2) 1_655 1_556 ? N10 Fe2 N16 88.3(2) . 1_556 ? N6 Fe2 N16 91.37(16) 1_565 1_556 ? N15 Fe2 N16 177.94(15) . 1_556 ? C1 N1 Fe1 155.0(3) . . ? C2 N2 C1 122.8(5) . . ? C2 N3 Fe2 166.7(4) . . ? C3 N4 Fe1 167.0(4) . . ? C3 N5 C4 123.1(4) . . ? C4 N6 Fe2 153.1(4) . 1_545 ? C5 N7 Fe1 156.3(5) . . ? C5 N8 C6 122.6(5) . . ? C6 N9 Fe1 156.1(4) . 1_455 ? C7 N10 Fe2 146.0(4) . . ? C7 N11 C8 122.4(4) . . ? C8 N12 Fe2 171.3(5) . 1_455 ? C9 N13 C18 115.2(5) . . ? C9 N13 Fe1 122.3(4) . . ? C18 N13 Fe1 122.4(4) . . ? C14 N14 C15 118.8(5) . . ? C14 N14 Fe1 121.2(4) . 1_554 ? C15 N14 Fe1 120.1(4) . 1_554 ? C19 N15 C28 114.1(5) . . ? C19 N15 Fe2 122.8(3) . . ? C28 N15 Fe2 123.2(4) . . ? C24 N16 C25 116.4(5) . . ? C24 N16 Fe2 122.0(3) . 1_554 ? C25 N16 Fe2 121.5(3) . 1_554 ? N1 C1 N2 174.1(5) . . ? N3 C2 N2 172.8(5) . . ? N4 C3 N5 172.5(5) . . ? N6 C4 N5 171.0(5) . . ? N7 C5 N8 172.5(6) . . ? N9 C6 N8 170.9(6) . . ? N10 C7 N11 172.2(6) . . ? N12 C8 N11 170.5(5) . . ? N13 C9 C10 123.5(5) . . ? C9 C10 C11 121.3(5) . . ? C10 C11 C17 115.5(5) . . ? C10 C11 C12 123.0(7) . . ? C17 C11 C12 121.4(7) . . ? C16 C12 C13 117.8(5) . . ? C16 C12 C11 123.3(7) . . ? C13 C12 C11 118.8(7) . . ? C14 C13 C12 118.3(5) . . ? N14 C14 C13 123.2(5) . . ? N14 C15 C16 121.8(5) . . ? C12 C16 C15 120.2(5) . . ? C18 C17 C11 120.1(5) . . ? N13 C18 C17 124.4(5) . . ? N15 C19 C20 124.6(5) . . ? C19 C20 C21 120.1(5) . . ? C27 C21 C20 116.1(5) . . ? C27 C21 C22 123.4(6) . . ? C20 C21 C22 120.6(6) . . ? C23 C22 C26 115.8(5) . . ? C23 C22 C21 123.5(6) . . ? C26 C22 C21 120.8(6) . . ? C24 C23 C22 121.1(5) . . ? N16 C24 C23 123.8(5) . . ? N16 C25 C26 123.0(4) . . ? C25 C26 C22 119.9(4) . . ? C28 C27 C21 119.6(5) . . ? N15 C28 C27 125.6(4) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.465 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.058 #=END data_1_293 _database_code_CSD 172404 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Fe(dca)2(4,4'-bipy) _chemical_formula_sum 'C14 H8 Fe N8' _chemical_formula_weight 344.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Fe' 'Fe' 0.3463 0.8444 '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' '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pmn2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' _cell_length_a 11.5198(2) _cell_length_b 17.0112(4) _cell_length_c 8.6659(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1698.22(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25510 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 28.26 _exptl_crystal_description Prismatic _exptl_crystal_colour Orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius KappaCCD' _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 25510 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.26 _reflns_number_total 4219 _reflns_number_gt 3131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett and Johnson, 1996)' _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^)+(0.0546P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.490(16) _refine_ls_number_reflns 4219 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Fe1 Fe 0.5000 0.11206(4) 0.5000 0.0329(3) Uani 1 2 d S . . Fe2 Fe 0.5000 0.61139(4) 0.65004(6) 0.0330(3) Uani 1 2 d S . . N1 N 0.5000 0.2374(3) 0.5447(7) 0.0559(15) Uani 1 2 d S . . N2 N 0.4449(10) 0.3490(5) 0.6953(16) 0.164(6) Uani 0.50 1 d P . . N3 N 0.5000 0.4863(2) 0.6757(8) 0.0556(15) Uani 1 2 d S . . N4 N 0.5000 -0.0121(3) 0.4777(8) 0.0579(15) Uani 1 2 d S . . N5 N 0.4466(11) -0.1499(4) 0.4620(9) 0.146(7) Uani 0.50 1 d P . . N6 N 0.5000 -0.2641(3) 0.6170(7) 0.0616(15) Uani 1 2 d S . . N7 N 0.5000 0.1283(3) 0.2583(6) 0.0507(14) Uani 1 2 d S . . N8 N 0.5740(10) 0.1427(10) 0.0013(12) 0.197(7) Uani 0.50 1 d P . . N9 N 0.5000 0.1036(3) -0.2512(8) 0.0609(18) Uani 1 2 d S . . N10 N 0.5000 0.6005(3) 0.4032(7) 0.0634(18) Uani 1 2 d S . . N11 N 0.5541(10) 0.6588(5) 0.1598(9) 0.137(6) Uani 0.50 1 d P . . N12 N 0.5000 0.6287(3) -0.1032(7) 0.0529(15) Uani 1 2 d S . . N13 N 0.3087(2) 0.11282(16) 0.4957(5) 0.0474(9) Uani 1 1 d . . . N15 N 0.3083(2) 0.61190(15) 0.6470(5) 0.0466(9) Uani 1 1 d . . . C1 C 0.4734(9) 0.2930(4) 0.6114(12) 0.065(5) Uani 0.50 1 d P . . C2 C 0.4736(7) 0.4212(4) 0.6743(12) 0.065(4) Uani 0.50 1 d P . . C3 C 0.4775(19) -0.0772(4) 0.4767(9) 0.058(6) Uani 0.50 1 d P . . C4 C 0.4762(13) -0.2083(4) 0.5527(11) 0.060(5) Uani 0.50 1 d P . . C5 C 0.5295(6) 0.1336(6) 0.1376(11) 0.066(3) Uani 0.50 1 d P . . C6 C 0.5312(7) 0.1206(5) -0.1269(11) 0.070(4) Uani 0.50 1 d P . . C7 C 0.524(2) 0.6235(5) 0.2892(13) 0.071(8) Uani 0.50 1 d P . . C8 C 0.520(4) 0.6387(5) 0.0248(9) 0.071(10) Uani 0.50 1 d P . . C9 C 0.2463(3) 0.1536(2) 0.5963(4) 0.0690(11) Uani 1 1 d . . . H9 H 0.2854 0.1825 0.6710 0.083 Uiso 1 1 calc R . . C10 C 0.1272(2) 0.1554(2) 0.5961(4) 0.0735(12) Uani 1 1 d . . . H10 H 0.0883 0.1851 0.6700 0.088 Uiso 1 1 calc R . . C11 C 0.0651(4) 0.1144(2) 0.4890(6) 0.0498(11) Uani 1 1 d . . . C17 C 0.1286(2) 0.0732(2) 0.3811(4) 0.0691(10) Uani 1 1 d . . . H17 H 0.0912 0.0451 0.3036 0.083 Uiso 1 1 calc R . . C18 C 0.2490(2) 0.0741(2) 0.3893(4) 0.0674(10) Uani 1 1 d . . . H18 H 0.2903 0.0457 0.3157 0.081 Uiso 1 1 calc R . . C19 C 0.2468(2) 0.6649(2) 0.7233(5) 0.0666(10) Uani 1 1 d . . . H19 H 0.2867 0.7028 0.7797 0.080 Uiso 1 1 calc R . . C20 C 0.1283(2) 0.6675(2) 0.7242(5) 0.0659(10) Uani 1 1 d . . . H20 H 0.0904 0.7058 0.7819 0.079 Uiso 1 1 calc R . . C21 C 0.0640(3) 0.61353(18) 0.6402(6) 0.0445(10) Uani 1 1 d . . . C27 C 0.1289(2) 0.55961(19) 0.5570(4) 0.0592(9) Uani 1 1 d . . . H27 H 0.0913 0.5226 0.4959 0.071 Uiso 1 1 calc R . . C28 C 0.2479(2) 0.5601(2) 0.5636(5) 0.0612(9) Uani 1 1 d . . . H28 H 0.2884 0.5226 0.5072 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0325(4) 0.0368(6) 0.0294(6) 0.0005(3) 0.000 0.000 Fe2 0.0300(4) 0.0346(5) 0.0345(7) 0.0004(3) 0.000 0.000 N1 0.060(3) 0.033(3) 0.074(4) -0.001(3) 0.000 0.000 N2 0.185(11) 0.055(5) 0.253(14) -0.045(7) 0.145(10) -0.020(6) N3 0.059(2) 0.035(3) 0.072(4) -0.012(3) 0.000 0.000 N4 0.064(3) 0.040(3) 0.069(4) -0.011(3) 0.000 0.000 N5 0.31(2) 0.037(4) 0.086(5) 0.015(4) -0.117(8) -0.044(7) N6 0.064(3) 0.049(3) 0.072(4) 0.012(3) 0.000 0.000 N7 0.064(3) 0.067(4) 0.021(3) 0.002(3) 0.000 0.000 N8 0.155(9) 0.40(2) 0.038(5) -0.019(8) 0.011(6) -0.155(10) N9 0.068(3) 0.069(4) 0.045(5) 0.009(3) 0.000 0.000 N10 0.069(3) 0.096(5) 0.025(4) -0.011(3) 0.000 0.000 N11 0.286(16) 0.095(5) 0.030(4) -0.001(3) -0.009(6) -0.121(7) N12 0.055(3) 0.059(4) 0.045(5) 0.005(3) 0.000 0.000 N13 0.0307(13) 0.060(2) 0.051(2) -0.0146(13) -0.003(3) 0.0019(14) N15 0.0374(14) 0.0510(18) 0.051(2) -0.0122(13) -0.003(3) -0.0026(13) C1 0.075(13) 0.038(4) 0.083(6) -0.003(4) 0.023(5) 0.000(4) C2 0.051(11) 0.043(5) 0.101(7) -0.017(5) 0.016(4) -0.005(4) C3 0.086(19) 0.044(4) 0.045(4) 0.001(4) -0.019(6) 0.006(5) C4 0.069(15) 0.031(4) 0.081(6) 0.006(4) -0.017(5) -0.010(4) C5 0.044(8) 0.118(7) 0.036(5) -0.006(5) -0.008(3) -0.022(4) C6 0.049(9) 0.145(10) 0.017(4) 0.007(5) 0.004(3) -0.022(4) C7 0.10(2) 0.067(5) 0.050(6) -0.020(4) -0.008(6) -0.012(6) C8 0.12(3) 0.053(4) 0.034(5) -0.008(3) 0.007(6) -0.031(11) C9 0.0355(17) 0.100(3) 0.071(2) -0.043(2) -0.0029(15) -0.0026(15) C10 0.0370(19) 0.106(3) 0.078(3) -0.050(2) 0.0025(16) 0.0054(16) C11 0.041(2) 0.062(3) 0.046(2) -0.0117(16) -0.001(2) 0.0025(18) C17 0.0357(16) 0.100(3) 0.072(2) -0.043(2) -0.0026(15) -0.0031(16) C18 0.0377(17) 0.096(3) 0.069(2) -0.043(2) 0.0006(14) -0.0012(16) C19 0.0352(16) 0.073(2) 0.092(3) -0.045(2) -0.0004(16) -0.0004(15) C20 0.0355(16) 0.071(2) 0.092(3) -0.044(2) 0.0022(16) -0.0009(14) C21 0.0264(16) 0.050(2) 0.057(3) -0.0090(14) -0.001(2) -0.0008(15) C27 0.0377(16) 0.065(2) 0.075(2) -0.0286(18) -0.0033(14) -0.0007(13) C28 0.0306(16) 0.071(2) 0.081(2) -0.034(2) 0.0003(15) 0.0034(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N7 2.113(5) . ? Fe1 N4 2.121(5) . ? Fe1 N9 2.161(7) 1_556 ? Fe1 N1 2.167(5) . ? Fe1 N13 2.204(3) 4_655 ? Fe1 N13 2.204(3) . ? Fe2 N6 2.137(5) 1_565 ? Fe2 N3 2.140(4) . ? Fe2 N10 2.147(6) . ? Fe2 N12 2.159(6) 1_556 ? Fe2 N15 2.209(3) . ? Fe2 N15 2.209(3) 4_655 ? N1 C1 1.150(9) 4_655 ? N1 C1 1.150(9) . ? N2 C1 1.243(11) . ? N2 N2 1.27(2) 4_655 ? N2 C2 1.286(10) . ? N2 C1 1.525(12) 4_655 ? N2 C2 1.558(11) 4_655 ? N3 C2 1.148(8) . ? N3 C2 1.148(8) 4_655 ? N4 C3 1.137(9) . ? N4 C3 1.137(9) 4_655 ? N5 N5 1.23(2) 4_655 ? N5 C3 1.293(11) . ? N5 C4 1.312(10) . ? N5 C3 1.520(16) 4_655 ? N5 C4 1.548(14) 4_655 ? N6 C4 1.134(9) 4_655 ? N6 C4 1.135(9) . ? N6 Fe2 2.137(5) 1_545 ? N7 C5 1.104(10) . ? N7 C5 1.104(10) 4_655 ? N8 C6 1.273(12) . ? N8 C5 1.297(12) . ? N8 C5 1.685(11) 4_655 ? N8 C6 1.687(12) 4_655 ? N8 N8 1.71(2) 4_655 ? N9 C6 1.172(11) 4_655 ? N9 C6 1.172(11) . ? N9 Fe1 2.161(7) 1_554 ? N10 C7 1.097(13) . ? N10 C7 1.097(13) 4_655 ? N11 N11 1.25(2) 4_655 ? N11 C8 1.280(16) . ? N11 C7 1.320(14) . ? N11 C8 1.49(3) 4_655 ? N11 C7 1.56(2) 4_655 ? N12 C8 1.146(12) 4_655 ? N12 C8 1.146(12) . ? N12 Fe2 2.159(6) 1_554 ? N13 C9 1.325(5) . ? N13 C18 1.326(5) . ? N15 C19 1.324(4) . ? N15 C28 1.335(5) . ? C1 C1 0.61(2) 4_655 ? C1 N2 1.525(12) 4_655 ? C2 C2 0.609(16) 4_655 ? C2 N2 1.558(11) 4_655 ? C3 C3 0.52(4) 4_655 ? C3 N5 1.520(16) 4_655 ? C4 C4 0.55(3) 4_655 ? C4 N5 1.548(14) 4_655 ? C5 C5 0.679(13) 4_655 ? C5 N8 1.685(11) 4_655 ? C6 C6 0.718(15) 4_655 ? C6 N8 1.687(12) 4_655 ? C7 C7 0.54(6) 4_655 ? C7 N11 1.56(2) 4_655 ? C8 C8 0.47(8) 4_655 ? C8 N11 1.49(3) 4_655 ? C9 C10 1.372(4) . ? C10 C11 1.364(5) . ? C11 C17 1.380(5) . ? C11 C11 1.499(9) 4 ? C17 C18 1.389(4) . ? C19 C20 1.365(4) . ? C20 C21 1.386(5) . ? C21 C27 1.385(5) . ? C21 C21 1.475(8) 4 ? C27 C28 1.372(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 N7 Fe1 N4 92.3(2) . . ? N7 Fe1 N9 176.3(2) . 1_556 ? N4 Fe1 N9 91.4(2) . 1_556 ? N7 Fe1 N1 92.8(2) . . ? N4 Fe1 N1 174.9(3) . . ? N9 Fe1 N1 83.52(19) 1_556 . ? N7 Fe1 N13 89.00(12) . 4_655 ? N4 Fe1 N13 90.25(7) . 4_655 ? N9 Fe1 N13 90.99(12) 1_556 4_655 ? N1 Fe1 N13 89.84(7) . 4_655 ? N7 Fe1 N13 89.00(12) . . ? N4 Fe1 N13 90.25(7) . . ? N9 Fe1 N13 90.99(12) 1_556 . ? N1 Fe1 N13 89.84(7) . . ? N13 Fe1 N13 178.0(2) 4_655 . ? N6 Fe2 N3 178.3(3) 1_565 . ? N6 Fe2 N10 87.2(2) 1_565 . ? N3 Fe2 N10 91.0(2) . . ? N6 Fe2 N12 89.9(2) 1_565 1_556 ? N3 Fe2 N12 91.9(2) . 1_556 ? N10 Fe2 N12 177.1(2) . 1_556 ? N6 Fe2 N15 89.69(7) 1_565 . ? N3 Fe2 N15 90.30(7) . . ? N10 Fe2 N15 89.34(12) . . ? N12 Fe2 N15 90.64(12) 1_556 . ? N6 Fe2 N15 89.69(7) 1_565 4_655 ? N3 Fe2 N15 90.29(7) . 4_655 ? N10 Fe2 N15 89.34(12) . 4_655 ? N12 Fe2 N15 90.64(12) 1_556 4_655 ? N15 Fe2 N15 178.6(2) . 4_655 ? C1 N1 C1 30.9(11) 4_655 . ? C1 N1 Fe1 154.0(6) 4_655 . ? C1 N1 Fe1 154.0(6) . . ? C1 N2 N2 74.7(7) . 4_655 ? C1 N2 C2 125.6(10) . . ? N2 N2 C2 75.1(6) 4_655 . ? C1 N2 C1 22.8(8) . 4_655 ? N2 N2 C1 51.8(6) 4_655 4_655 ? C2 N2 C1 111.8(8) . 4_655 ? C1 N2 C2 112.2(9) . 4_655 ? N2 N2 C2 52.9(5) 4_655 4_655 ? C2 N2 C2 22.2(6) . 4_655 ? C1 N2 C2 93.7(7) 4_655 4_655 ? C2 N3 C2 30.8(8) . 4_655 ? C2 N3 Fe2 163.3(5) . . ? C2 N3 Fe2 163.3(5) 4_655 . ? C3 N4 C3 26(2) . 4_655 ? C3 N4 Fe1 166.0(10) . . ? C3 N4 Fe1 166.0(10) 4_655 . ? N5 N5 C3 74.0(11) 4_655 . ? N5 N5 C4 74.9(8) 4_655 . ? C3 N5 C4 126.4(10) . . ? N5 N5 C3 54.9(8) 4_655 4_655 ? C3 N5 C3 19.2(16) . 4_655 ? C4 N5 C3 114.6(10) . 4_655 ? N5 N5 C4 54.9(7) 4_655 4_655 ? C3 N5 C4 113.9(11) . 4_655 ? C4 N5 C4 20.0(11) . 4_655 ? C3 N5 C4 98.5(10) 4_655 4_655 ? C4 N6 C4 28.0(15) 4_655 . ? C4 N6 Fe2 153.5(7) 4_655 1_545 ? C4 N6 Fe2 153.6(7) . 1_545 ? C5 N7 C5 35.9(7) . 4_655 ? C5 N7 Fe1 161.9(4) . . ? C5 N7 Fe1 161.9(4) 4_655 . ? C6 N8 C5 127.3(9) . . ? C6 N8 C5 108.1(7) . 4_655 ? C5 N8 C5 21.7(5) . 4_655 ? C6 N8 C6 23.1(6) . 4_655 ? C5 N8 C6 106.8(7) . 4_655 ? C5 N8 C6 86.1(6) 4_655 4_655 ? C6 N8 N8 67.2(6) . 4_655 ? C5 N8 N8 66.7(6) . 4_655 ? C5 N8 N8 45.0(5) 4_655 4_655 ? C6 N8 N8 44.1(5) 4_655 4_655 ? C6 N9 C6 35.7(8) 4_655 . ? C6 N9 Fe1 154.3(5) 4_655 1_554 ? C6 N9 Fe1 154.3(5) . 1_554 ? C7 N10 C7 29(3) . 4_655 ? C7 N10 Fe2 150.1(9) . . ? C7 N10 Fe2 150.1(9) 4_655 . ? N11 N11 C8 72.2(18) 4_655 . ? N11 N11 C7 74.6(12) 4_655 . ? C8 N11 C7 124.9(14) . . ? N11 N11 C8 54.9(14) 4_655 4_655 ? C8 N11 C8 17(3) . 4_655 ? C7 N11 C8 114.1(14) . 4_655 ? N11 N11 C7 54.9(10) 4_655 4_655 ? C8 N11 C7 112.3(16) . 4_655 ? C7 N11 C7 20(2) . 4_655 ? C8 N11 C7 98.4(15) 4_655 4_655 ? C8 N12 C8 23(4) 4_655 . ? C8 N12 Fe2 168(2) 4_655 1_554 ? C8 N12 Fe2 168(2) . 1_554 ? C9 N13 C18 115.9(3) . . ? C9 N13 Fe1 122.3(3) . . ? C18 N13 Fe1 121.8(2) . . ? C19 N15 C28 116.2(3) . . ? C19 N15 Fe2 122.1(2) . . ? C28 N15 Fe2 121.7(2) . . ? C1 C1 N1 74.5(5) 4_655 . ? C1 C1 N2 105.3(8) 4_655 . ? N1 C1 N2 174.4(12) . . ? C1 C1 N2 51.8(6) 4_655 4_655 ? N1 C1 N2 126.1(10) . 4_655 ? N2 C1 N2 53.5(11) . 4_655 ? C2 C2 N3 74.6(4) 4_655 . ? C2 C2 N2 104.9(6) 4_655 . ? N3 C2 N2 171.2(11) . . ? C2 C2 N2 52.9(5) 4_655 4_655 ? N3 C2 N2 126.8(7) . 4_655 ? N2 C2 N2 52.0(10) . 4_655 ? C3 C3 N4 76.8(11) 4_655 . ? C3 C3 N5 106.0(11) 4_655 . ? N4 C3 N5 174.0(12) . . ? C3 C3 N5 54.9(8) 4_655 4_655 ? N4 C3 N5 131.4(18) . 4_655 ? N5 C3 N5 51.1(11) . 4_655 ? C4 C4 N6 76.0(7) 4_655 . ? C4 C4 N5 105.1(8) 4_655 . ? N6 C4 N5 172.2(9) . . ? C4 C4 N5 54.9(7) 4_655 4_655 ? N6 C4 N5 130.4(13) . 4_655 ? N5 C4 N5 50.1(10) . 4_655 ? C5 C5 N7 72.1(4) 4_655 . ? C5 C5 N8 113.3(6) 4_655 . ? N7 C5 N8 174.2(8) . . ? C5 C5 N8 45.0(5) 4_655 4_655 ? N7 C5 N8 117.0(6) . 4_655 ? N8 C5 N8 68.3(10) . 4_655 ? C6 C6 N9 72.2(4) 4_655 . ? C6 C6 N8 112.8(6) 4_655 . ? N9 C6 N8 173.9(9) . . ? C6 C6 N8 44.1(5) 4_655 4_655 ? N9 C6 N8 116.1(7) . 4_655 ? N8 C6 N8 68.8(10) . 4_655 ? C7 C7 N10 75.6(14) 4_655 . ? C7 C7 N11 105.4(12) 4_655 . ? N10 C7 N11 173.4(11) . . ? C7 C7 N11 54.9(10) 4_655 4_655 ? N10 C7 N11 130(2) . 4_655 ? N11 C7 N11 50.6(11) . 4_655 ? C8 C8 N12 78(2) 4_655 . ? C8 C8 N11 107.8(18) 4_655 . ? N12 C8 N11 170(2) . . ? C8 C8 N11 54.9(14) 4_655 4_655 ? N12 C8 N11 133(3) . 4_655 ? N11 C8 N11 52.8(11) . 4_655 ? N13 C9 C10 123.6(3) . . ? C11 C10 C9 120.9(3) . . ? C10 C11 C17 116.3(4) . . ? C10 C11 C11 121.7(2) . 4 ? C17 C11 C11 122.1(2) . 4 ? C11 C17 C18 119.3(3) . . ? N13 C18 C17 124.0(3) . . ? N15 C19 C20 124.0(3) . . ? C19 C20 C21 120.6(3) . . ? C27 C21 C20 115.1(3) . . ? C27 C21 C21 122.6(2) . 4 ? C20 C21 C21 122.3(2) . 4 ? C28 C27 C21 120.9(3) . . ? N15 C28 C27 123.2(3) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.430 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.055 #=END data_2 _database_code_CSD 172405 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Co(dca)2(4,4'-bipy) _chemical_formula_sum 'C14 H8 Co N8' _chemical_formula_weight 347.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 '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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.5824(3) _cell_length_b 16.7687(7) _cell_length_c 11.4092(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.068(3) _cell_angle_gamma 90.00 _cell_volume 1641.96(11) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 11937 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 30.03 _exptl_crystal_description Acicular _exptl_crystal_colour Pink _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method Phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11937 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.1410 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7735 _reflns_number_gt 4881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett and Johnson, 1996)' _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^)+(0.0000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 7735 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1218 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.11247(6) 0.5000 0.0153(3) Uani 1 1 d . . . Co2 Co 0.66793(10) 0.61055(6) 0.49933(17) 0.0152(3) Uani 1 1 d . . . N1 N 0.5545(8) 0.2357(4) 0.4913(7) 0.0237(17) Uani 1 1 d . . . N2 N 0.7256(11) 0.3473(5) 0.4424(10) 0.079(4) Uani 1 1 d . . . N3 N 0.6973(8) 0.4858(4) 0.4946(7) 0.0223(18) Uani 1 1 d . . . N4 N 0.4672(8) -0.0104(4) 0.5004(8) 0.0244(18) Uani 1 1 d . . . N5 N 0.4535(9) -0.1536(5) 0.4504(8) 0.051(3) Uani 1 1 d . . . N6 N 0.6289(8) -0.2652(4) 0.4944(7) 0.0241(17) Uani 1 1 d . . . N7 N 0.2582(7) 0.1299(4) 0.5024(8) 0.0215(17) Uani 1 1 d . . . N8 N -0.0001(9) 0.1275(7) 0.5934(6) 0.087(4) Uani 1 1 d . . . N9 N -0.2549(9) 0.0980(4) 0.5112(8) 0.027(2) Uani 1 1 d . . . N10 N 0.4241(9) 0.5962(4) 0.5024(9) 0.0280(19) Uani 1 1 d . . . N11 N 0.1783(9) 0.6647(4) 0.5517(7) 0.052(2) Uani 1 1 d . . . N12 N -0.0889(8) 0.6324(4) 0.5021(8) 0.0259(18) Uani 1 1 d . . . N13 N 0.4976(10) 0.1110(5) 0.3132(7) 0.021(2) Uani 1 1 d . . . N14 N 0.4961(10) 0.1149(5) -0.3103(7) 0.020(2) Uani 1 1 d . . . N15 N 0.6647(10) 0.6116(4) 0.3107(6) 0.017(2) Uani 1 1 d . . . N16 N 0.6660(10) 0.6112(5) -0.3120(7) 0.023(2) Uani 1 1 d . . . C1 C 0.6293(11) 0.2907(5) 0.4726(7) 0.032(3) Uani 1 1 d . . . C2 C 0.7027(11) 0.4189(5) 0.4707(7) 0.029(2) Uani 1 1 d . . . C3 C 0.4691(10) -0.0768(5) 0.4804(8) 0.028(2) Uani 1 1 d . . . C4 C 0.5550(10) -0.2095(5) 0.4762(7) 0.025(2) Uani 1 1 d . . . C5 C 0.1345(9) 0.1303(6) 0.5401(7) 0.0314(16) Uani 1 1 d . . . C6 C -0.1309(11) 0.1127(5) 0.5438(8) 0.0314(16) Uani 1 1 d . . . C7 C 0.3048(13) 0.6254(5) 0.5236(9) 0.032(3) Uani 1 1 d . . . C8 C 0.0392(11) 0.6429(5) 0.5240(7) 0.027(2) Uani 1 1 d . . . C9 C 0.6142(9) 0.1410(5) 0.2490(7) 0.0234(18) Uani 1 1 d . . . H9 H 0.7024 0.1616 0.2893 0.028 Uiso 1 1 calc R . . C10 C 0.6146(9) 0.1441(5) 0.1282(6) 0.0239(19) Uani 1 1 d . . . H10 H 0.7024 0.1649 0.0878 0.029 Uiso 1 1 calc R . . C11 C 0.4855(14) 0.1166(7) 0.0650(9) 0.024(3) Uani 1 1 d . . . C12 C 0.4844(13) 0.1158(6) -0.0666(8) 0.020(3) Uani 1 1 d . . . C13 C 0.5835(10) 0.1669(5) -0.1275(7) 0.0238(15) Uani 1 1 d . . . H13 H 0.6493 0.2030 -0.0867 0.029 Uiso 1 1 calc R . . C14 C 0.5841(9) 0.1638(5) -0.2481(7) 0.0238(15) Uani 1 1 d . . . H14 H 0.6518 0.1989 -0.2890 0.029 Uiso 1 1 calc R . . C15 C 0.3955(10) 0.0674(4) -0.2501(7) 0.021(2) Uani 1 1 d . . . H15 H 0.3280 0.0330 -0.2926 0.025 Uiso 1 1 calc R . . C16 C 0.3885(11) 0.0677(5) -0.1292(7) 0.027(2) Uani 1 1 d . . . H16 H 0.3164 0.0341 -0.0899 0.033 Uiso 1 1 calc R . . C17 C 0.3645(10) 0.0838(5) 0.1326(7) 0.026(2) Uani 1 1 d . . . H17 H 0.2762 0.0609 0.0951 0.031 Uiso 1 1 calc R . . C18 C 0.3740(10) 0.0848(5) 0.2524(7) 0.024(2) Uani 1 1 d . . . H18 H 0.2871 0.0656 0.2954 0.029 Uiso 1 1 calc R . . C19 C 0.7510(10) 0.6628(5) 0.2495(8) 0.026(2) Uani 1 1 d . . . H19 H 0.8147 0.6996 0.2907 0.032 Uiso 1 1 calc R . . C20 C 0.7516(11) 0.6643(6) 0.1271(7) 0.026(2) Uani 1 1 d . . . H20 H 0.8168 0.7008 0.0865 0.031 Uiso 1 1 calc R . . C21 C 0.6554(12) 0.6118(6) 0.0647(9) 0.020(3) Uani 1 1 d . . . C22 C 0.6569(13) 0.6142(6) -0.0663(9) 0.020(3) Uani 1 1 d . . . C23 C 0.7225(11) 0.6745(6) -0.1324(7) 0.025(2) Uani 1 1 d . . . H23 H 0.7663 0.7195 -0.0940 0.031 Uiso 1 1 calc R . . C24 C 0.7256(10) 0.6705(5) -0.2505(8) 0.025(2) Uani 1 1 d . . . H24 H 0.7735 0.7131 -0.2920 0.030 Uiso 1 1 calc R . . C25 C 0.5977(10) 0.5511(4) -0.2500(7) 0.024(2) Uani 1 1 d . . . H25 H 0.5513 0.5080 -0.2912 0.029 Uiso 1 1 calc R . . C26 C 0.5940(10) 0.5512(5) -0.1307(7) 0.023(2) Uani 1 1 d . . . H26 H 0.5478 0.5075 -0.0906 0.028 Uiso 1 1 calc R . . C27 C 0.5614(10) 0.5619(5) 0.1303(7) 0.023(2) Uani 1 1 d . . . H27 H 0.4910 0.5266 0.0924 0.028 Uiso 1 1 calc R . . C28 C 0.5705(10) 0.5636(4) 0.2511(7) 0.022(2) Uani 1 1 d . . . H28 H 0.5054 0.5284 0.2941 0.026 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 0.0149(7) 0.0159(7) 0.0152(6) -0.0003(7) 0.0011(7) 0.0011(4) Co2 0.0157(7) 0.0157(7) 0.0144(6) 0.0007(7) 0.0021(7) 0.0006(4) N1 0.035(5) 0.013(4) 0.023(3) 0.000(4) 0.002(4) 0.002(3) N2 0.094(8) 0.016(5) 0.127(9) -0.006(6) 0.064(6) -0.010(5) N3 0.027(5) 0.018(4) 0.021(3) -0.003(4) -0.005(4) -0.007(3) N4 0.022(5) 0.025(4) 0.026(3) -0.007(5) 0.003(4) -0.002(3) N5 0.020(4) 0.025(5) 0.109(7) -0.018(5) -0.035(4) 0.011(4) N6 0.019(4) 0.028(4) 0.025(3) -0.003(4) -0.005(4) 0.006(3) N7 0.009(4) 0.026(4) 0.030(4) 0.003(5) -0.009(4) -0.004(4) N8 0.018(4) 0.206(11) 0.037(4) -0.044(6) 0.005(4) -0.011(6) N9 0.020(5) 0.035(5) 0.025(4) -0.001(4) -0.003(4) 0.011(4) N10 0.019(5) 0.036(5) 0.029(4) -0.008(5) 0.001(5) 0.003(3) N11 0.017(4) 0.036(4) 0.104(7) -0.038(4) -0.010(4) 0.006(4) N12 0.025(5) 0.029(4) 0.024(4) 0.007(5) -0.002(5) -0.003(4) N13 0.021(5) 0.019(5) 0.022(5) 0.002(4) 0.005(5) -0.004(3) N14 0.023(5) 0.013(4) 0.025(5) 0.008(4) 0.003(5) -0.001(3) N15 0.018(5) 0.022(5) 0.011(4) 0.002(4) 0.003(4) -0.003(3) N16 0.022(6) 0.024(5) 0.024(5) -0.006(4) -0.002(5) 0.000(3) C1 0.034(6) 0.021(5) 0.042(6) -0.002(4) 0.024(5) 0.006(4) C2 0.029(6) 0.015(5) 0.042(6) -0.003(4) 0.017(4) -0.015(4) C3 0.018(5) 0.025(5) 0.040(6) -0.006(5) -0.002(4) -0.004(4) C4 0.027(5) 0.016(4) 0.031(6) -0.005(4) -0.004(4) 0.001(4) C5 0.006(3) 0.061(4) 0.026(3) -0.010(3) -0.005(2) -0.002(3) C6 0.006(3) 0.061(4) 0.026(3) -0.010(3) -0.005(2) -0.002(3) C7 0.033(5) 0.024(5) 0.038(7) -0.004(4) -0.016(4) -0.021(4) C8 0.040(6) 0.018(4) 0.025(6) -0.009(3) -0.001(3) -0.007(4) C9 0.014(4) 0.040(5) 0.016(3) 0.002(3) -0.005(3) -0.011(3) C10 0.012(4) 0.039(5) 0.020(4) 0.004(3) 0.000(3) -0.009(3) C11 0.024(6) 0.030(7) 0.018(6) 0.005(5) -0.001(4) 0.005(5) C12 0.022(6) 0.023(6) 0.017(6) -0.004(4) 0.005(4) -0.013(4) C13 0.024(4) 0.023(3) 0.024(3) 0.004(2) 0.006(2) -0.008(3) C14 0.024(4) 0.023(3) 0.024(3) 0.004(2) 0.006(2) -0.008(3) C15 0.023(5) 0.016(4) 0.024(4) 0.002(3) -0.002(3) -0.013(4) C16 0.034(6) 0.028(5) 0.020(5) 0.008(3) -0.002(4) -0.013(4) C17 0.015(4) 0.042(6) 0.021(4) 0.001(4) -0.006(3) -0.014(4) C18 0.025(5) 0.029(5) 0.018(4) -0.005(3) 0.007(3) 0.003(4) C19 0.031(6) 0.024(5) 0.025(5) 0.001(4) -0.001(4) -0.019(4) C20 0.031(5) 0.037(6) 0.010(4) -0.008(4) 0.001(3) -0.012(4) C21 0.017(6) 0.025(6) 0.018(6) -0.009(4) -0.008(4) -0.001(4) C22 0.022(6) 0.020(6) 0.018(6) -0.002(4) -0.004(4) -0.002(4) C23 0.031(5) 0.023(5) 0.022(5) 0.000(3) -0.002(4) -0.008(4) C24 0.028(5) 0.023(5) 0.023(5) 0.005(4) 0.000(4) -0.009(4) C25 0.030(5) 0.011(4) 0.032(5) 0.007(3) 0.003(4) 0.000(3) C26 0.025(5) 0.025(5) 0.019(4) 0.011(3) 0.005(3) -0.004(4) C27 0.015(4) 0.028(5) 0.027(5) 0.005(3) -0.002(3) -0.006(4) C28 0.027(5) 0.024(5) 0.014(4) 0.004(3) 0.008(3) -0.008(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 Co1 N4 2.080(7) . ? Co1 N7 2.096(6) . ? Co1 N9 2.121(8) 1_655 ? Co1 N1 2.122(6) . ? Co1 N13 2.131(8) . ? Co1 N14 2.164(8) 1_556 ? Co2 N10 2.107(8) . ? Co2 N3 2.108(6) . ? Co2 N6 2.111(6) 1_565 ? Co2 N12 2.119(7) 1_655 ? Co2 N15 2.152(8) . ? Co2 N16 2.152(8) 1_556 ? N1 C1 1.144(9) . ? N2 C2 1.260(10) . ? N2 C1 1.304(10) . ? N3 C2 1.155(9) . ? N4 C3 1.136(10) . ? N5 C4 1.313(9) . ? N5 C3 1.340(10) . ? N6 C4 1.148(9) . ? N6 Co2 2.111(6) 1_545 ? N7 C5 1.146(10) . ? N8 C6 1.280(11) . ? N8 C5 1.308(11) . ? N9 C6 1.154(11) . ? N9 Co1 2.121(8) 1_455 ? N10 C7 1.161(12) . ? N11 C8 1.288(10) . ? N11 C7 1.310(12) . ? N12 C8 1.141(10) . ? N12 Co2 2.119(7) 1_455 ? N13 C9 1.339(10) . ? N13 C18 1.341(12) . ? N14 C14 1.321(11) . ? N14 C15 1.361(10) . ? N14 Co1 2.165(8) 1_554 ? N15 C28 1.328(11) . ? N15 C19 1.332(10) . ? N16 C24 1.320(10) . ? N16 C25 1.364(10) . ? N16 Co2 2.152(8) 1_554 ? C9 C10 1.380(9) . ? C10 C11 1.399(12) . ? C11 C17 1.406(13) . ? C11 C12 1.502(11) . ? C12 C16 1.356(12) . ? C12 C13 1.394(12) . ? C13 C14 1.377(10) . ? C15 C16 1.380(11) . ? C17 C18 1.369(11) . ? C19 C20 1.396(11) . ? C20 C21 1.401(12) . ? C21 C27 1.383(12) . ? C21 C22 1.495(11) . ? C22 C23 1.381(13) . ? C22 C26 1.395(12) . ? C23 C24 1.350(11) . ? C25 C26 1.362(11) . ? C27 C28 1.381(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N7 90.2(3) . . ? N4 Co1 N9 91.2(3) . 1_655 ? N7 Co1 N9 175.6(4) . 1_655 ? N4 Co1 N1 174.4(3) . . ? N7 Co1 N1 94.8(3) . . ? N9 Co1 N1 84.0(2) 1_655 . ? N4 Co1 N13 89.4(3) . . ? N7 Co1 N13 90.4(4) . . ? N9 Co1 N13 93.9(3) 1_655 . ? N1 Co1 N13 88.1(3) . . ? N4 Co1 N14 90.8(3) . 1_556 ? N7 Co1 N14 88.1(3) . 1_556 ? N9 Co1 N14 87.6(3) 1_655 1_556 ? N1 Co1 N14 91.8(3) . 1_556 ? N13 Co1 N14 178.5(3) . 1_556 ? N10 Co2 N3 90.3(3) . . ? N10 Co2 N6 87.5(2) . 1_565 ? N3 Co2 N6 176.3(3) . 1_565 ? N10 Co2 N12 176.2(3) . 1_655 ? N3 Co2 N12 93.1(3) . 1_655 ? N6 Co2 N12 89.2(3) 1_565 1_655 ? N10 Co2 N15 90.3(4) . . ? N3 Co2 N15 89.1(3) . . ? N6 Co2 N15 87.9(3) 1_565 . ? N12 Co2 N15 91.4(3) 1_655 . ? N10 Co2 N16 88.6(3) . 1_556 ? N3 Co2 N16 91.8(3) . 1_556 ? N6 Co2 N16 91.2(3) 1_565 1_556 ? N12 Co2 N16 89.6(3) 1_655 1_556 ? N15 Co2 N16 178.6(3) . 1_556 ? C1 N1 Co1 156.6(7) . . ? C2 N2 C1 121.7(9) . . ? C2 N3 Co2 167.0(8) . . ? C3 N4 Co1 165.4(8) . . ? C4 N5 C3 124.2(8) . . ? C4 N6 Co2 153.6(7) . 1_545 ? C5 N7 Co1 157.4(8) . . ? C6 N8 C5 125.2(8) . . ? C6 N9 Co1 155.4(8) . 1_455 ? C7 N10 Co2 146.2(7) . . ? C8 N11 C7 124.4(8) . . ? C8 N12 Co2 168.2(8) . 1_455 ? C9 N13 C18 115.5(8) . . ? C9 N13 Co1 122.4(6) . . ? C18 N13 Co1 121.9(6) . . ? C14 N14 C15 117.0(8) . . ? C14 N14 Co1 122.6(6) . 1_554 ? C15 N14 Co1 120.3(6) . 1_554 ? C28 N15 C19 117.4(8) . . ? C28 N15 Co2 121.0(6) . . ? C19 N15 Co2 121.6(6) . . ? C24 N16 C25 116.5(8) . . ? C24 N16 Co2 122.1(6) . 1_554 ? C25 N16 Co2 121.3(6) . 1_554 ? N1 C1 N2 172.4(10) . . ? N3 C2 N2 173.1(10) . . ? N4 C3 N5 172.7(10) . . ? N6 C4 N5 171.1(10) . . ? N7 C5 N8 173.8(10) . . ? N9 C6 N8 172.5(11) . . ? N10 C7 N11 174.1(10) . . ? N12 C8 N11 172.2(10) . . ? N13 C9 C10 124.3(8) . . ? C9 C10 C11 120.0(8) . . ? C10 C11 C17 115.6(8) . . ? C10 C11 C12 121.5(10) . . ? C17 C11 C12 122.7(10) . . ? C16 C12 C13 118.2(9) . . ? C16 C12 C11 122.4(10) . . ? C13 C12 C11 119.3(10) . . ? C14 C13 C12 118.6(8) . . ? N14 C14 C13 123.9(8) . . ? N14 C15 C16 122.1(8) . . ? C12 C16 C15 120.1(8) . . ? C18 C17 C11 119.9(9) . . ? N13 C18 C17 124.6(9) . . ? N15 C19 C20 122.6(9) . . ? C19 C20 C21 119.6(9) . . ? C27 C21 C20 116.7(9) . . ? C27 C21 C22 124.2(10) . . ? C20 C21 C22 119.1(10) . . ? C23 C22 C26 115.1(9) . . ? C23 C22 C21 124.6(10) . . ? C26 C22 C21 120.2(10) . . ? C24 C23 C22 121.1(9) . . ? N16 C24 C23 124.1(9) . . ? C26 C25 N16 121.9(8) . . ? C25 C26 C22 121.1(8) . . ? C28 C27 C21 119.7(8) . . ? N15 C28 C27 123.9(8) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.467 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.101 #=END data_4 _database_code_CSD 172406 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Mn(dca)2(4,4'-bipy)(H2O).0.5MeOH _chemical_formula_sum 'C29 H24 Mn2 N16 O3' _chemical_formula_weight 754.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mn' 'Mn' 0.3368 0.7283 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 22.5468(3) _cell_length_b 22.5468(3) _cell_length_c 13.4343(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6829.44(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 87307 _cell_measurement_theta_min 1.28 _cell_measurement_theta_max 30.03 _exptl_crystal_description Prismatic _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.833 _exptl_absorpt_correction_T_max 0.868 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius KappaCCD' _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 87307 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 30.03 _reflns_number_total 18370 _reflns_number_gt 10512 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett and Johnson, 1996)' _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^)+(0.0562P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.002(13) _refine_ls_number_reflns 18370 _refine_ls_number_parameters 900 _refine_ls_number_restraints 563 _refine_ls_R_factor_all 0.1148 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.094 _refine_ls_shift/su_mean 0.016 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 0.14063(7) 0.15384(6) -0.0033 0.0341(4) Uani 1 1 d . . . Mn2 Mn 0.35982(7) 0.34488(6) 0.01474(9) 0.0355(4) Uani 1 1 d . . . Mn3 Mn 0.14104(7) 0.34629(6) 0.51383(14) 0.0368(4) Uani 1 1 d . . . Mn4 Mn 0.36017(7) 0.15473(6) 0.49718(16) 0.0346(4) Uani 1 1 d . . . O1 O 0.1926(2) 0.2377(2) -0.0373(4) 0.0461(12) Uani 1 1 d . . . O2 O 0.3079(2) 0.26228(19) 0.0342(5) 0.0602(15) Uani 1 1 d . . . O3 O 0.1940(2) 0.26357(19) 0.5350(5) 0.0576(14) Uani 1 1 d . . . O4 O 0.3095(2) 0.23869(18) 0.4643(4) 0.0441(12) Uani 1 1 d . . . O5 O 0.2821(2) 0.2531(3) 0.2614(6) 0.084(2) Uani 1 1 d D . . O6 O 0.2129(3) 0.2551(5) -0.2398(8) 0.127(3) Uani 1 1 d D . . N1 N 0.0907(3) 0.1989(3) 0.1170(4) 0.0491(19) Uani 1 1 d D . . N2 N 0.0427(3) 0.2569(5) 0.2478(7) 0.088(3) Uani 1 1 d D . . N3 N 0.0890(3) 0.3053(3) 0.3914(5) 0.059(2) Uani 1 1 d D . . N4 N 0.1997(3) 0.1135(3) 0.1091(5) 0.063(2) Uani 1 1 d D . . N5 N 0.2593(4) 0.0647(4) 0.2358(7) 0.110(4) Uani 1 1 d D . . N6 N 0.3089(3) 0.1110(3) 0.3775(5) 0.058(2) Uani 1 1 d D . . N7 N 0.0784(3) 0.1875(3) -0.1189(5) 0.053(2) Uani 1 1 d D . . N8 N 0.0282(3) 0.2468(4) -0.2472(7) 0.080(3) Uani 1 1 d D . . N9 N 0.0826(4) 0.3061(3) -0.3717(5) 0.061(2) Uani 1 1 d D . . N10 N 0.1911(3) 0.1071(4) -0.1220(5) 0.0558(19) Uani 1 1 d D . . N11 N 0.2476(4) 0.0657(4) -0.2565(6) 0.110(5) Uani 1 1 d D . . N12 N 0.2999(4) 0.1133(4) -0.3917(5) 0.064(2) Uani 1 1 d D . . N13 N 0.3083(3) 0.3891(3) 0.1320(5) 0.062(2) Uani 1 1 d D . . N14 N 0.2433(5) 0.4307(5) 0.2572(7) 0.140(5) Uani 1 1 d D . . N15 N 0.1980(3) 0.3873(4) 0.4023(5) 0.057(2) Uani 1 1 d D . . N16 N 0.4174(4) 0.3057(3) 0.1319(5) 0.056(2) Uani 1 1 d D . . N17 N 0.4682(3) 0.2465(5) 0.2541(8) 0.107(4) Uani 1 1 d D . . N18 N 0.4245(3) 0.1908(3) 0.3880(5) 0.055(2) Uani 1 1 d D . . N19 N 0.3051(3) 0.3876(4) -0.0967(5) 0.063(2) Uani 1 1 d D . . N20 N 0.2442(5) 0.4317(4) -0.2270(7) 0.133(5) Uani 1 1 d D . . N21 N 0.1927(3) 0.3899(4) -0.3684(5) 0.064(2) Uani 1 1 d D . . N22 N 0.4123(3) 0.3023(4) -0.1067(5) 0.063(2) Uani 1 1 d D . . N23 N 0.4562(4) 0.2413(5) -0.2356(8) 0.120(5) Uani 1 1 d D . . N24 N 0.4077(4) 0.1988(3) -0.3796(5) 0.054(2) Uani 1 1 d D . . N25 N 0.0759(2) 0.0763(3) 0.0099(5) 0.0300(16) Uani 1 1 d D . . N26 N -0.1266(3) -0.1648(3) 0.0080(7) 0.061(3) Uani 1 1 d D . . N27 N 0.4264(3) 0.4203(3) 0.0110(5) 0.0332(17) Uani 1 1 d D . . N28 N 0.6321(3) 0.6576(3) 0.0071(7) 0.057(3) Uani 1 1 d D . . N29 N 0.0753(3) 0.4217(3) 0.5087(5) 0.0375(18) Uani 1 1 d D . . N30 N -0.1277(3) 0.6627(3) 0.5023(7) 0.058(3) Uani 1 1 d D . . N31 N 0.4255(3) 0.0792(3) 0.5086(5) 0.0376(18) Uani 1 1 d D . . N32 N 0.6300(3) -0.1610(3) 0.5071(7) 0.067(3) Uani 1 1 d D . . C1 C 0.0709(4) 0.2248(4) 0.1825(6) 0.054(2) Uani 1 1 d D . . C2 C 0.0694(4) 0.2795(4) 0.3244(6) 0.055(2) Uani 1 1 d D . . C3 C 0.2254(4) 0.0948(4) 0.1745(6) 0.058(2) Uani 1 1 d D . . C4 C 0.2817(4) 0.0933(4) 0.3132(6) 0.059(3) Uani 1 1 d D . . C5 C 0.0600(4) 0.2156(4) -0.1835(6) 0.048(2) Uani 1 1 d D . . C6 C 0.0603(4) 0.2756(4) -0.3150(6) 0.061(3) Uani 1 1 d D . . C7 C 0.2163(4) 0.0921(4) -0.1897(6) 0.051(2) Uani 1 1 d D . . C8 C 0.2721(4) 0.0946(4) -0.3299(6) 0.059(3) Uani 1 1 d D . . C9 C 0.2792(4) 0.4069(4) 0.1956(6) 0.061(3) Uani 1 1 d D . . C10 C 0.2242(4) 0.4052(4) 0.3377(6) 0.059(3) Uani 1 1 d D . . C11 C 0.4411(4) 0.2803(4) 0.1929(6) 0.049(2) Uani 1 1 d D . . C12 C 0.4430(3) 0.2188(4) 0.3244(6) 0.042(2) Uani 1 1 d D . . C13 C 0.2787(4) 0.4069(4) -0.1633(6) 0.061(3) Uani 1 1 d D . . C14 C 0.2192(4) 0.4079(4) -0.3020(6) 0.064(3) Uani 1 1 d D . . C15 C 0.4304(4) 0.2764(4) -0.1721(7) 0.066(3) Uani 1 1 d D . . C16 C 0.4280(4) 0.2231(4) -0.3132(6) 0.057(3) Uani 1 1 d D . . C17 C 0.0944(3) 0.0212(3) 0.0082(6) 0.039(2) Uani 1 1 d D . . H17 H 0.1351 0.0141 0.0067 0.046 Uiso 1 1 calc R . . C18 C 0.0561(3) -0.0268(3) 0.0084(5) 0.037(2) Uani 1 1 d D . . H18 H 0.0710 -0.0652 0.0087 0.044 Uiso 1 1 calc R . . C19 C -0.0049(3) -0.0173(3) 0.0083(5) 0.043(2) Uani 1 1 d D . . C20 C -0.0478(3) -0.0676(3) 0.0102(6) 0.035(2) Uani 1 1 d D . . C21 C -0.0296(3) -0.1237(4) 0.0108(6) 0.059(3) Uani 1 1 d D . . H21 H 0.0109 -0.1311 0.0138 0.070 Uiso 1 1 calc R . . C22 C -0.0684(3) -0.1722(2) 0.0073(6) 0.052(2) Uani 1 1 d D . . H22 H -0.0529 -0.2104 0.0044 0.062 Uiso 1 1 calc R . . C23 C -0.1452(3) -0.1079(4) 0.0018(9) 0.081(4) Uani 1 1 d D . . H23 H -0.1857 -0.1011 -0.0048 0.097 Uiso 1 1 calc R . . C24 C -0.1080(3) -0.0589(3) 0.0045(7) 0.060(3) Uani 1 1 d D . . H24 H -0.1236 -0.0208 0.0026 0.071 Uiso 1 1 calc R . . C25 C -0.0248(3) 0.0422(3) 0.0093(5) 0.035(2) Uani 1 1 d D . . H25 H -0.0649 0.0516 0.0101 0.041 Uiso 1 1 calc R . . C26 C 0.0189(3) 0.0862(3) 0.0090(6) 0.041(2) Uani 1 1 d D . . H26 H 0.0064 0.1255 0.0080 0.049 Uiso 1 1 calc R . . C27 C 0.4081(3) 0.4764(3) 0.0124(6) 0.037(2) Uani 1 1 d D . . H27 H 0.3676 0.4843 0.0139 0.044 Uiso 1 1 calc R . . C28 C 0.4483(3) 0.5241(3) 0.0116(5) 0.044(2) Uani 1 1 d D . . H28 H 0.4341 0.5629 0.0122 0.053 Uiso 1 1 calc R . . C29 C 0.5083(3) 0.5139(3) 0.0100(5) 0.035(2) Uani 1 1 d D . . C30 C 0.5503(3) 0.5633(3) 0.0134(6) 0.044(2) Uani 1 1 d D . . C31 C 0.5311(3) 0.6225(3) 0.0108(6) 0.056(3) Uani 1 1 d D . . H31 H 0.4909 0.6318 0.0123 0.067 Uiso 1 1 calc R . . C32 C 0.5739(4) 0.6665(3) 0.0059(7) 0.070(3) Uani 1 1 d D . . H32 H 0.5608 0.7055 0.0013 0.085 Uiso 1 1 calc R . . C33 C 0.6498(4) 0.6024(4) 0.0086(9) 0.078(4) Uani 1 1 d D . . H33 H 0.6903 0.5949 0.0078 0.093 Uiso 1 1 calc R . . C34 C 0.6110(3) 0.5539(3) 0.0112(7) 0.059(3) Uani 1 1 d D . . H34 H 0.6259 0.5154 0.0115 0.071 Uiso 1 1 calc R . . C35 C 0.5267(3) 0.4555(3) 0.0095(5) 0.0308(18) Uani 1 1 d D . . H35 H 0.5669 0.4465 0.0103 0.037 Uiso 1 1 calc R . . C36 C 0.4854(3) 0.4108(3) 0.0078(6) 0.046(2) Uani 1 1 d D . . H36 H 0.4989 0.3719 0.0043 0.055 Uiso 1 1 calc R . . C37 C 0.0939(3) 0.4799(3) 0.5125(6) 0.044(2) Uani 1 1 d D . . H37 H 0.1344 0.4878 0.5153 0.053 Uiso 1 1 calc R . . C38 C 0.0553(3) 0.5264(3) 0.5124(5) 0.039(2) Uani 1 1 d D . . H38 H 0.0700 0.5650 0.5122 0.047 Uiso 1 1 calc R . . C39 C -0.0055(3) 0.5173(2) 0.5127(5) 0.0292(19) Uani 1 1 d D . . C40 C -0.0480(3) 0.5684(3) 0.5085(5) 0.041(2) Uani 1 1 d D . . C41 C -0.0279(3) 0.6263(3) 0.5025(6) 0.057(3) Uani 1 1 d D . . H41 H 0.0123 0.6350 0.4998 0.068 Uiso 1 1 calc R . . C42 C -0.0692(4) 0.6695(3) 0.5007(7) 0.073(3) Uani 1 1 d D . . H42 H -0.0552 0.7083 0.4981 0.088 Uiso 1 1 calc R . . C43 C -0.1474(3) 0.6078(3) 0.5135(7) 0.060(3) Uani 1 1 d D . . H43 H -0.1879 0.6010 0.5191 0.072 Uiso 1 1 calc R . . C44 C -0.1088(4) 0.5604(3) 0.5172(7) 0.065(3) Uani 1 1 d D . . H44 H -0.1239 0.5223 0.5256 0.077 Uiso 1 1 calc R . . C45 C -0.0235(3) 0.4588(3) 0.5095(6) 0.044(2) Uani 1 1 d D . . H45 H -0.0638 0.4502 0.5068 0.053 Uiso 1 1 calc R . . C46 C 0.0169(3) 0.4128(3) 0.5103(6) 0.035(2) Uani 1 1 d D . . H46 H 0.0027 0.3741 0.5120 0.042 Uiso 1 1 calc R . . C47 C 0.4852(3) 0.0892(3) 0.5142(5) 0.0309(19) Uani 1 1 d D . . H47 H 0.4987 0.1281 0.5173 0.037 Uiso 1 1 calc R . . C48 C 0.5259(3) 0.0442(3) 0.5155(5) 0.044(2) Uani 1 1 d D . . H48 H 0.5662 0.0529 0.5190 0.053 Uiso 1 1 calc R . . C49 C 0.5072(3) -0.0147(3) 0.5116(5) 0.0307(19) Uani 1 1 d D . . C50 C 0.5508(3) -0.0647(3) 0.5101(5) 0.034(2) Uani 1 1 d D . . C51 C 0.6116(3) -0.0577(3) 0.5017(6) 0.056(3) Uani 1 1 d D . . H51 H 0.6273 -0.0198 0.4955 0.067 Uiso 1 1 calc R . . C52 C 0.6481(3) -0.1045(3) 0.5024(7) 0.060(3) Uani 1 1 d D . . H52 H 0.6887 -0.0973 0.4994 0.072 Uiso 1 1 calc R . . C53 C 0.5718(4) -0.1691(3) 0.5200(8) 0.070(3) Uani 1 1 d D . . H53 H 0.5576 -0.2075 0.5283 0.084 Uiso 1 1 calc R . . C54 C 0.5327(3) -0.1235(3) 0.5214(6) 0.059(3) Uani 1 1 d D . . H54 H 0.4926 -0.1316 0.5302 0.071 Uiso 1 1 calc R . . C55 C 0.4452(3) -0.0241(3) 0.5064(5) 0.037(2) Uani 1 1 d D . . H55 H 0.4301 -0.0624 0.5031 0.044 Uiso 1 1 calc R . . C56 C 0.4087(3) 0.0225(3) 0.5063(6) 0.037(2) Uani 1 1 d D . . H56 H 0.3682 0.0148 0.5045 0.044 Uiso 1 1 calc R . . C57 C 0.2216(2) 0.2509(4) 0.2516(9) 0.068(3) Uani 1 1 d D . . H57A H 0.2047 0.2318 0.3088 0.102 Uiso 1 1 calc R . . H57B H 0.2115 0.2289 0.1928 0.102 Uiso 1 1 calc R . . H57C H 0.2062 0.2905 0.2463 0.102 Uiso 1 1 calc R . . C58 C 0.2734(4) 0.2482(5) -0.2564(9) 0.107(4) Uani 1 1 d D . . H58A H 0.2902 0.2854 -0.2768 0.161 Uiso 1 1 calc R . . H58B H 0.2795 0.2192 -0.3078 0.161 Uiso 1 1 calc R . . H58C H 0.2923 0.2351 -0.1962 0.161 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 Mn1 0.0357(7) 0.0354(7) 0.0312(8) -0.0007(4) -0.0003(5) -0.0012(7) Mn2 0.0378(8) 0.0324(7) 0.0364(9) -0.0016(5) -0.0019(5) -0.0007(6) Mn3 0.0369(7) 0.0323(7) 0.0413(9) -0.0022(5) -0.0005(5) 0.0029(6) Mn4 0.0341(7) 0.0370(7) 0.0328(7) 0.0002(4) 0.0002(4) 0.0018(7) O1 0.042(3) 0.052(3) 0.044(2) 0.000(2) 0.0055(18) 0.007(2) O2 0.033(3) 0.038(3) 0.111(4) -0.009(3) -0.008(3) -0.003(2) O3 0.043(3) 0.031(3) 0.099(4) -0.015(3) 0.010(3) -0.005(2) O4 0.042(3) 0.038(3) 0.052(3) 0.007(2) -0.0019(19) 0.015(2) O5 0.049(3) 0.146(6) 0.058(4) 0.048(3) 0.013(3) 0.008(4) O6 0.079(5) 0.181(9) 0.120(7) 0.024(5) 0.000(6) -0.014(7) N1 0.057(4) 0.055(5) 0.035(3) -0.008(3) -0.002(3) 0.001(3) N2 0.054(5) 0.152(8) 0.059(5) -0.061(5) -0.006(4) 0.025(5) N3 0.061(5) 0.058(5) 0.058(5) -0.022(3) 0.001(3) 0.009(4) N4 0.061(5) 0.061(5) 0.068(4) -0.011(3) -0.030(3) 0.021(4) N5 0.151(9) 0.070(6) 0.109(6) -0.040(5) -0.095(7) 0.057(5) N6 0.086(5) 0.042(4) 0.044(3) -0.001(3) -0.018(3) -0.003(3) N7 0.050(4) 0.059(5) 0.049(4) 0.022(3) -0.012(3) 0.001(3) N8 0.071(5) 0.096(6) 0.073(5) 0.053(4) 0.000(5) 0.000(5) N9 0.078(5) 0.049(5) 0.055(4) 0.020(3) 0.019(3) 0.006(4) N10 0.058(4) 0.056(4) 0.054(4) -0.012(3) 0.018(3) -0.002(3) N11 0.182(11) 0.048(6) 0.101(7) 0.020(4) 0.102(7) 0.038(5) N12 0.062(5) 0.076(5) 0.055(4) -0.002(3) 0.014(3) -0.001(4) N13 0.064(5) 0.053(5) 0.070(5) 0.006(3) 0.027(4) 0.004(4) N14 0.206(12) 0.087(8) 0.128(9) 0.040(6) 0.124(9) 0.072(7) N15 0.056(5) 0.055(4) 0.059(4) -0.001(3) 0.017(3) -0.003(3) N16 0.059(5) 0.056(5) 0.054(4) 0.017(3) -0.007(3) -0.003(4) N17 0.034(4) 0.171(10) 0.116(7) 0.098(6) 0.038(4) 0.037(5) N18 0.058(4) 0.057(4) 0.051(4) 0.021(3) -0.001(3) 0.014(4) N19 0.063(4) 0.073(5) 0.052(4) -0.008(3) -0.033(3) 0.013(4) N20 0.229(13) 0.047(5) 0.122(8) -0.032(5) -0.128(8) 0.071(6) N21 0.061(5) 0.069(5) 0.062(4) 0.004(3) -0.031(4) 0.007(4) N22 0.060(4) 0.069(5) 0.060(5) -0.025(4) -0.003(3) 0.020(4) N23 0.096(7) 0.162(9) 0.102(8) -0.093(7) -0.045(6) 0.070(6) N24 0.066(5) 0.047(4) 0.049(4) -0.017(3) -0.007(3) 0.008(3) N25 0.023(4) 0.031(4) 0.035(4) 0.003(3) 0.004(3) -0.006(3) N26 0.064(7) 0.044(5) 0.073(6) -0.001(4) 0.009(4) -0.020(5) N27 0.026(4) 0.044(4) 0.029(4) 0.001(3) -0.003(3) -0.005(3) N28 0.064(6) 0.047(5) 0.060(5) -0.003(4) -0.003(4) -0.022(5) N29 0.047(5) 0.031(4) 0.034(4) 0.007(3) -0.001(3) -0.002(4) N30 0.053(6) 0.033(5) 0.087(6) 0.001(4) -0.005(5) 0.010(4) N31 0.048(5) 0.026(4) 0.039(4) 0.000(3) 0.000(4) -0.001(4) N32 0.052(6) 0.052(6) 0.097(7) 0.012(5) 0.004(5) 0.024(5) C1 0.045(5) 0.063(6) 0.055(5) -0.023(5) 0.000(4) -0.002(4) C2 0.046(5) 0.067(6) 0.053(5) -0.016(4) 0.004(4) -0.007(5) C3 0.050(5) 0.049(5) 0.076(6) -0.013(4) -0.029(5) 0.002(4) C4 0.073(6) 0.055(6) 0.048(5) 0.003(4) -0.031(4) 0.005(5) C5 0.054(5) 0.045(5) 0.046(5) 0.007(4) -0.002(4) -0.012(4) C6 0.075(6) 0.070(7) 0.039(5) 0.009(4) -0.002(4) 0.027(5) C7 0.059(5) 0.042(5) 0.051(5) -0.006(3) 0.027(4) -0.004(4) C8 0.066(6) 0.059(6) 0.053(5) -0.004(4) 0.016(4) 0.000(5) C9 0.069(6) 0.032(5) 0.082(6) 0.013(4) 0.022(5) 0.005(4) C10 0.081(7) 0.040(5) 0.057(5) -0.007(4) 0.031(5) 0.000(5) C11 0.034(4) 0.041(4) 0.072(5) 0.023(4) -0.003(3) -0.003(3) C12 0.031(4) 0.046(5) 0.051(5) 0.014(4) -0.005(3) -0.001(3) C13 0.081(7) 0.029(4) 0.075(6) -0.017(4) -0.024(5) 0.003(4) C14 0.080(7) 0.043(5) 0.070(6) 0.000(4) -0.027(5) 0.018(5) C15 0.060(6) 0.070(7) 0.069(6) -0.036(5) -0.014(5) 0.005(5) C16 0.057(5) 0.076(6) 0.039(4) -0.015(4) 0.010(4) 0.028(5) C17 0.033(5) 0.047(5) 0.036(5) 0.000(4) 0.002(3) -0.020(4) C18 0.034(5) 0.036(5) 0.041(5) -0.005(4) 0.002(4) -0.001(4) C19 0.060(6) 0.053(6) 0.017(4) -0.008(4) 0.002(4) -0.001(5) C20 0.035(5) 0.027(4) 0.044(5) 0.005(3) -0.006(4) 0.007(4) C21 0.027(4) 0.060(6) 0.089(7) -0.005(5) -0.007(4) -0.005(4) C22 0.046(6) 0.013(3) 0.096(7) 0.000(3) 0.004(4) -0.005(4) C23 0.042(6) 0.083(8) 0.116(9) 0.010(7) 0.009(5) -0.029(6) C24 0.038(5) 0.031(5) 0.109(7) -0.006(4) -0.002(4) -0.019(4) C25 0.051(5) 0.030(4) 0.022(4) 0.000(3) -0.004(4) 0.016(4) C26 0.070(7) 0.023(4) 0.030(5) -0.001(3) 0.005(4) 0.002(4) C27 0.033(5) 0.033(5) 0.045(5) 0.002(4) 0.004(3) -0.009(4) C28 0.054(6) 0.024(5) 0.054(6) 0.010(4) -0.004(4) -0.001(4) C29 0.042(5) 0.041(5) 0.022(4) 0.003(3) 0.004(3) -0.005(4) C30 0.053(6) 0.043(5) 0.036(4) 0.002(4) -0.001(4) 0.013(4) C31 0.030(4) 0.032(5) 0.106(6) -0.003(5) -0.002(4) -0.014(4) C32 0.084(8) 0.032(5) 0.095(6) 0.000(4) -0.008(5) -0.014(5) C33 0.047(7) 0.072(8) 0.115(10) -0.003(6) -0.002(5) -0.008(6) C34 0.045(6) 0.034(5) 0.099(7) -0.007(4) 0.019(4) -0.016(4) C35 0.031(4) 0.015(3) 0.047(4) -0.004(3) 0.002(4) 0.009(3) C36 0.047(6) 0.044(6) 0.047(5) -0.001(4) 0.002(4) 0.001(5) C37 0.049(5) 0.034(5) 0.049(5) -0.003(4) 0.004(4) -0.020(4) C38 0.038(5) 0.024(4) 0.056(5) -0.010(4) -0.002(4) 0.000(4) C39 0.026(4) 0.016(3) 0.045(5) -0.004(3) 0.006(3) 0.000(3) C40 0.050(6) 0.049(5) 0.024(4) 0.000(3) -0.002(4) 0.024(4) C41 0.072(7) 0.022(4) 0.076(7) 0.003(4) 0.001(4) 0.005(4) C42 0.070(8) 0.067(7) 0.084(7) -0.003(5) 0.000(5) 0.005(6) C43 0.052(6) 0.028(4) 0.101(7) 0.013(4) 0.002(5) -0.004(4) C44 0.059(7) 0.058(6) 0.077(6) 0.011(5) 0.014(4) -0.009(5) C45 0.025(4) 0.044(5) 0.064(6) 0.003(5) -0.003(4) 0.008(4) C46 0.031(5) 0.029(5) 0.044(5) 0.004(3) 0.000(3) -0.004(4) C47 0.026(4) 0.031(4) 0.035(4) -0.005(3) -0.001(3) -0.005(3) C48 0.037(5) 0.061(6) 0.034(4) 0.010(4) 0.001(4) 0.015(4) C49 0.031(5) 0.031(5) 0.031(4) 0.003(3) 0.000(3) 0.005(4) C50 0.042(5) 0.028(4) 0.031(4) -0.005(3) -0.006(3) 0.022(3) C51 0.041(6) 0.043(5) 0.082(7) 0.000(4) -0.009(4) -0.015(4) C52 0.037(6) 0.046(5) 0.097(8) -0.014(5) -0.009(4) 0.011(5) C53 0.058(7) 0.046(6) 0.107(7) 0.007(5) 0.019(5) 0.017(5) C54 0.064(6) 0.051(6) 0.063(5) 0.015(4) 0.009(4) -0.013(5) C55 0.039(5) 0.041(5) 0.030(4) 0.004(4) -0.001(3) -0.006(4) C56 0.028(5) 0.042(5) 0.040(5) 0.003(4) -0.006(3) -0.010(4) C57 0.025(3) 0.098(7) 0.081(6) -0.047(4) -0.001(5) -0.003(4) C58 0.174(11) 0.109(10) 0.038(6) -0.005(5) 0.011(6) -0.012(9) _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 N4 2.210(6) . ? Mn1 N1 2.217(6) . ? Mn1 N10 2.224(6) . ? Mn1 N7 2.227(6) . ? Mn1 O1 2.270(5) . ? Mn1 N25 2.285(5) . ? Mn2 N19 2.166(6) . ? Mn2 N13 2.196(6) . ? Mn2 O2 2.215(5) . ? Mn2 N16 2.223(7) . ? Mn2 N22 2.232(6) . ? Mn2 N27 2.270(6) . ? Mn3 N15 2.180(6) . ? Mn3 N21 2.197(6) 1_556 ? Mn3 N9 2.219(7) 1_556 ? Mn3 N3 2.221(6) . ? Mn3 O3 2.233(5) . ? Mn3 N29 2.257(6) . ? Mn4 N24 2.208(6) 1_556 ? Mn4 N6 2.213(6) . ? Mn4 N18 2.217(6) . ? Mn4 N12 2.224(7) 1_556 ? Mn4 O4 2.254(4) . ? Mn4 N31 2.257(6) . ? O5 C57 1.372(8) . ? O6 C58 1.391(10) . ? N1 C1 1.145(7) . ? N2 C2 1.297(8) . ? N2 C1 1.305(8) . ? N3 C2 1.159(7) . ? N4 C3 1.134(7) . ? N5 C3 1.312(8) . ? N5 C4 1.325(8) . ? N6 C4 1.131(7) . ? N7 C5 1.151(7) . ? N8 C5 1.320(8) . ? N8 C6 1.333(8) . ? N9 C6 1.142(7) . ? N9 Mn3 2.219(6) 1_554 ? N10 C7 1.125(7) . ? N11 C7 1.287(7) . ? N11 C8 1.304(8) . ? N12 C8 1.123(7) . ? N12 Mn4 2.224(7) 1_554 ? N13 C9 1.152(7) . ? N14 C9 1.275(8) . ? N14 C10 1.297(8) . ? N15 C10 1.124(7) . ? N16 C11 1.134(7) . ? N17 C12 1.266(8) . ? N17 C11 1.276(8) . ? N18 C12 1.142(7) . ? N19 C13 1.160(7) . ? N20 C14 1.273(8) . ? N20 C13 1.284(8) . ? N21 C14 1.148(7) . ? N21 Mn3 2.197(6) 1_554 ? N22 C15 1.132(7) . ? N23 C16 1.288(8) . ? N23 C15 1.300(8) . ? N24 C16 1.143(7) . ? N24 Mn4 2.208(6) 1_554 ? N25 C26 1.304(7) . ? N25 C17 1.311(7) . ? N26 C22 1.322(8) . ? N26 C23 1.353(8) . ? N27 C27 1.330(7) . ? N27 C36 1.348(8) . ? N28 C33 1.308(8) . ? N28 C32 1.327(8) . ? N29 C46 1.332(7) . ? N29 C37 1.381(7) . ? N30 C43 1.324(7) . ? N30 C42 1.329(8) . ? N31 C56 1.334(7) . ? N31 C47 1.367(7) . ? N32 C53 1.337(8) . ? N32 C52 1.338(7) . ? C17 C18 1.386(8) . ? C18 C19 1.391(8) . ? C19 C25 1.413(8) . ? C19 C20 1.491(8) . ? C20 C21 1.329(8) . ? C20 C24 1.375(8) . ? C21 C22 1.401(7) . ? C23 C24 1.387(8) . ? C25 C26 1.398(8) . ? C27 C28 1.408(8) . ? C28 C29 1.372(8) . ? C29 C35 1.381(7) . ? C29 C30 1.463(8) . ? C30 C34 1.384(8) . ? C30 C31 1.403(8) . ? C31 C32 1.387(8) . ? C33 C34 1.400(8) . ? C35 C36 1.372(8) . ? C37 C38 1.363(8) . ? C38 C39 1.387(7) . ? C39 C45 1.380(8) . ? C39 C40 1.498(7) . ? C40 C41 1.385(8) . ? C40 C44 1.388(8) . ? C41 C42 1.348(8) . ? C43 C44 1.378(8) . ? C45 C46 1.380(8) . ? C47 C48 1.368(8) . ? C48 C49 1.394(8) . ? C49 C55 1.414(8) . ? C49 C50 1.497(7) . ? C50 C51 1.383(8) . ? C50 C54 1.395(8) . ? C51 C52 1.339(8) . ? C53 C54 1.353(8) . ? C55 C56 1.334(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 N4 Mn1 N1 89.8(2) . . ? N4 Mn1 N10 89.2(3) . . ? N1 Mn1 N10 178.9(3) . . ? N4 Mn1 N7 175.6(3) . . ? N1 Mn1 N7 91.8(3) . . ? N10 Mn1 N7 89.1(3) . . ? N4 Mn1 O1 99.8(3) . . ? N1 Mn1 O1 91.6(2) . . ? N10 Mn1 O1 89.2(2) . . ? N7 Mn1 O1 84.3(2) . . ? N4 Mn1 N25 91.0(3) . . ? N1 Mn1 N25 88.2(3) . . ? N10 Mn1 N25 91.2(3) . . ? N7 Mn1 N25 85.0(2) . . ? O1 Mn1 N25 169.3(2) . . ? N19 Mn2 N13 89.6(3) . . ? N19 Mn2 O2 98.9(3) . . ? N13 Mn2 O2 91.0(3) . . ? N19 Mn2 N16 177.0(3) . . ? N13 Mn2 N16 88.9(3) . . ? O2 Mn2 N16 83.7(3) . . ? N19 Mn2 N22 89.3(3) . . ? N13 Mn2 N22 178.4(3) . . ? O2 Mn2 N22 90.3(3) . . ? N16 Mn2 N22 92.1(3) . . ? N19 Mn2 N27 91.6(3) . . ? N13 Mn2 N27 91.4(3) . . ? O2 Mn2 N27 169.2(2) . . ? N16 Mn2 N27 85.8(3) . . ? N22 Mn2 N27 87.5(3) . . ? N15 Mn3 N21 89.6(3) . 1_556 ? N15 Mn3 N9 179.0(3) . 1_556 ? N21 Mn3 N9 89.9(3) 1_556 1_556 ? N15 Mn3 N3 88.8(3) . . ? N21 Mn3 N3 177.9(3) 1_556 . ? N9 Mn3 N3 91.7(3) 1_556 . ? N15 Mn3 O3 97.3(2) . . ? N21 Mn3 O3 89.9(3) 1_556 . ? N9 Mn3 O3 83.6(3) 1_556 . ? N3 Mn3 O3 91.7(2) . . ? N15 Mn3 N29 92.7(3) . . ? N21 Mn3 N29 91.9(3) 1_556 . ? N9 Mn3 N29 86.5(3) 1_556 . ? N3 Mn3 N29 86.7(3) . . ? O3 Mn3 N29 169.9(2) . . ? N24 Mn4 N6 177.5(3) 1_556 . ? N24 Mn4 N18 90.8(3) 1_556 . ? N6 Mn4 N18 91.4(3) . . ? N24 Mn4 N12 89.0(3) 1_556 1_556 ? N6 Mn4 N12 88.9(3) . 1_556 ? N18 Mn4 N12 176.0(3) . 1_556 ? N24 Mn4 O4 90.8(2) 1_556 . ? N6 Mn4 O4 88.1(2) . . ? N18 Mn4 O4 83.9(2) . . ? N12 Mn4 O4 100.0(3) 1_556 . ? N24 Mn4 N31 88.4(3) 1_556 . ? N6 Mn4 N31 93.1(3) . . ? N18 Mn4 N31 84.0(3) . . ? N12 Mn4 N31 92.1(3) 1_556 . ? O4 Mn4 N31 167.8(2) . . ? C1 N1 Mn1 172.2(8) . . ? C2 N2 C1 121.7(7) . . ? C2 N3 Mn3 170.0(8) . . ? C3 N4 Mn1 172.3(8) . . ? C3 N5 C4 117.6(8) . . ? C4 N6 Mn4 174.1(7) . . ? C5 N7 Mn1 160.2(7) . . ? C5 N8 C6 114.0(7) . . ? C6 N9 Mn3 165.8(8) . 1_554 ? C7 N10 Mn1 168.8(8) . . ? C7 N11 C8 121.9(8) . . ? C8 N12 Mn4 174.4(8) . 1_554 ? C9 N13 Mn2 173.4(8) . . ? C9 N14 C10 124.4(9) . . ? C10 N15 Mn3 172.8(8) . . ? C11 N16 Mn2 171.0(8) . . ? C12 N17 C11 124.1(7) . . ? C12 N18 Mn4 159.6(7) . . ? C13 N19 Mn2 173.1(8) . . ? C14 N20 C13 127.8(9) . . ? C14 N21 Mn3 173.7(8) . 1_554 ? C15 N22 Mn2 168.8(8) . . ? C16 N23 C15 120.3(8) . . ? C16 N24 Mn4 174.6(8) . 1_554 ? C26 N25 C17 118.5(5) . . ? C26 N25 Mn1 119.8(5) . . ? C17 N25 Mn1 121.3(4) . . ? C22 N26 C23 115.3(6) . . ? C27 N27 C36 117.3(6) . . ? C27 N27 Mn2 120.4(4) . . ? C36 N27 Mn2 122.3(5) . . ? C33 N28 C32 116.4(6) . . ? C46 N29 C37 116.3(6) . . ? C46 N29 Mn3 122.4(5) . . ? C37 N29 Mn3 121.0(5) . . ? C43 N30 C42 116.3(6) . . ? C56 N31 C47 116.0(5) . . ? C56 N31 Mn4 122.4(5) . . ? C47 N31 Mn4 121.5(4) . . ? C53 N32 C52 115.8(6) . . ? N1 C1 N2 171.6(11) . . ? N3 C2 N2 172.1(12) . . ? N4 C3 N5 167.5(11) . . ? N6 C4 N5 168.0(12) . . ? N7 C5 N8 167.9(10) . . ? N9 C6 N8 171.1(11) . . ? N10 C7 N11 168.6(10) . . ? N12 C8 N11 169.4(12) . . ? N13 C9 N14 172.3(11) . . ? N15 C10 N14 167.4(12) . . ? N16 C11 N17 173.2(13) . . ? N18 C12 N17 174.2(10) . . ? N19 C13 N20 171.2(12) . . ? N21 C14 N20 174.1(13) . . ? N22 C15 N23 170.0(13) . . ? N24 C16 N23 169.3(12) . . ? N25 C17 C18 122.7(6) . . ? C17 C18 C19 119.7(6) . . ? C18 C19 C25 117.4(6) . . ? C18 C19 C20 121.5(7) . . ? C25 C19 C20 121.1(7) . . ? C21 C20 C24 116.1(6) . . ? C21 C20 C19 121.6(7) . . ? C24 C20 C19 122.1(6) . . ? C20 C21 C22 123.4(6) . . ? N26 C22 C21 121.3(6) . . ? N26 C23 C24 124.4(7) . . ? C20 C24 C23 119.1(7) . . ? C26 C25 C19 116.8(6) . . ? N25 C26 C25 124.9(6) . . ? N27 C27 C28 121.7(6) . . ? C29 C28 C27 120.5(6) . . ? C28 C29 C35 117.1(5) . . ? C28 C29 C30 120.7(7) . . ? C35 C29 C30 122.1(7) . . ? C34 C30 C31 116.8(6) . . ? C34 C30 C29 121.5(7) . . ? C31 C30 C29 121.5(7) . . ? C32 C31 C30 117.8(6) . . ? N28 C32 C31 125.4(7) . . ? N28 C33 C34 123.6(7) . . ? C30 C34 C33 119.8(7) . . ? C36 C35 C29 119.9(6) . . ? N27 C36 C35 123.5(6) . . ? C38 C37 N29 122.5(6) . . ? C37 C38 C39 121.2(6) . . ? C45 C39 C38 115.6(5) . . ? C45 C39 C40 123.0(6) . . ? C38 C39 C40 121.2(6) . . ? C41 C40 C44 116.8(6) . . ? C41 C40 C39 121.2(7) . . ? C44 C40 C39 121.9(7) . . ? C42 C41 C40 117.3(7) . . ? N30 C42 C41 126.9(7) . . ? N30 C43 C44 121.2(6) . . ? C43 C44 C40 121.3(6) . . ? C46 C45 C39 121.7(6) . . ? N29 C46 C45 122.6(6) . . ? N31 C47 C48 122.6(6) . . ? C47 C48 C49 120.2(6) . . ? C48 C49 C55 116.4(5) . . ? C48 C49 C50 121.3(6) . . ? C55 C49 C50 122.3(6) . . ? C51 C50 C54 114.0(5) . . ? C51 C50 C49 124.4(7) . . ? C54 C50 C49 121.5(7) . . ? C52 C51 C50 121.3(6) . . ? N32 C52 C51 124.2(6) . . ? N32 C53 C54 122.5(7) . . ? C53 C54 C50 122.0(6) . . ? C56 C55 C49 119.4(6) . . ? C55 C56 N31 125.4(6) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.361 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.071 #=END data_5 _database_code_CSD 172407 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Fe(dca)2(4,4'-bipy)(H2O).0.5MeOH _chemical_formula_sum 'C29 H24 Fe2 N16 O3' _chemical_formula_weight 756.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Fe' 'Fe' 0.3463 0.8444 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 22.3171(4) _cell_length_b 22.3171(4) _cell_length_c 13.2602(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6604.28(17) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 60593 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 28.27 _exptl_crystal_description Acicular _exptl_crystal_colour Orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.938 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.935 _exptl_absorpt_correction_T_max 0.952 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method Phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60593 _diffrn_reflns_av_R_equivalents 0.0990 _diffrn_reflns_av_sigmaI/netI 0.1167 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.27 _reflns_number_total 15206 _reflns_number_gt 10154 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett and Johnson, 1996)' _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 w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+16.0245P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(2) _refine_ls_number_reflns 15206 _refine_ls_number_parameters 417 _refine_ls_number_restraints 663 _refine_ls_R_factor_all 0.1239 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.14213(7) 0.15338(7) -0.0033 0.0078(4) Uani 1 d . . . Fe2 Fe 0.35957(8) 0.34394(8) 0.01849(12) 0.0159(5) Uani 1 d . . . Fe3 Fe 0.14001(8) 0.34489(8) 0.51681(18) 0.0133(4) Uani 1 d . . . Fe4 Fe 0.36091(7) 0.15587(7) 0.49777(19) 0.0095(4) Uani 1 d . . . O1 O 0.1930(3) 0.2364(3) -0.0357(4) 0.0163(14) Uiso 1 d . . . O2 O 0.3068(3) 0.2633(3) 0.0417(5) 0.0203(15) Uiso 1 d . . . O3 O 0.1923(3) 0.2645(3) 0.5414(5) 0.0185(15) Uiso 1 d . . . O4 O 0.3072(3) 0.2361(3) 0.4664(5) 0.0188(15) Uiso 1 d . . . O5 O 0.2834(4) 0.2446(4) 0.2569(9) 0.048(3) Uiso 1 d D . . O6 O 0.2172(3) 0.2614(3) -0.2375(5) 0.0207(17) Uiso 1 d D . . N1 N 0.0931(4) 0.1983(3) 0.1150(5) 0.0135(19) Uiso 1 d DU . . N2 N 0.0439(4) 0.2606(3) 0.2449(5) 0.021(2) Uiso 1 d DU . . N3 N 0.0921(4) 0.3048(4) 0.3934(6) 0.020(2) Uiso 1 d DU . . N4 N 0.2002(4) 0.1160(4) 0.1062(6) 0.023(2) Uiso 1 d DU . . N5 N 0.2625(4) 0.0663(4) 0.2306(6) 0.036(3) Uiso 1 d DU . . N6 N 0.3120(4) 0.1112(4) 0.3774(5) 0.0175(19) Uiso 1 d DU . . N7 N 0.0812(4) 0.1876(4) -0.1188(6) 0.021(2) Uiso 1 d DU . . N8 N 0.0267(3) 0.2473(4) -0.2486(6) 0.019(2) Uiso 1 d DU . . N9 N 0.0795(4) 0.3073(4) -0.3734(6) 0.018(2) Uiso 1 d DU . . N10 N 0.1918(4) 0.1089(4) -0.1203(5) 0.0200(19) Uiso 1 d DU . . N11 N 0.2335(4) 0.0669(3) -0.2758(5) 0.0234(19) Uiso 1 d DU . . N12 N 0.3002(4) 0.1165(4) -0.3960(5) 0.0191(19) Uiso 1 d DU . . N13 N 0.3107(4) 0.3875(4) 0.1336(5) 0.021(2) Uiso 1 d DU . . N14 N 0.2461(3) 0.4350(3) 0.2615(5) 0.0118(19) Uiso 1 d DU . . N15 N 0.1988(4) 0.3860(4) 0.4074(6) 0.022(2) Uiso 1 d DU . . N16 N 0.4180(4) 0.3077(4) 0.1332(6) 0.024(2) Uiso 1 d DU . . N17 N 0.4732(4) 0.2406(4) 0.2483(6) 0.034(3) Uiso 1 d DU . . N18 N 0.4221(3) 0.1923(3) 0.3918(5) 0.0132(18) Uiso 1 d DU . . N19 N 0.3039(4) 0.3828(3) -0.0922(5) 0.0195(19) Uiso 1 d DU . . N20 N 0.2462(4) 0.4346(4) -0.2269(6) 0.034(3) Uiso 1 d DU . . N21 N 0.1903(4) 0.3886(4) -0.3643(5) 0.019(2) Uiso 1 d DU . . N22 N 0.4106(4) 0.2994(4) -0.1000(6) 0.027(2) Uiso 1 d DU . . N23 N 0.4601(3) 0.2426(4) -0.2368(6) 0.020(2) Uiso 1 d DU . . N24 N 0.4076(4) 0.1993(4) -0.3817(6) 0.018(2) Uiso 1 d DU . . N25 N 0.0786(3) 0.0791(3) 0.0089(7) 0.012(2) Uiso 1 d DU . . N26 N -0.1274(4) -0.1644(4) 0.0000(8) 0.021(2) Uiso 1 d DU . . N27 N 0.4262(3) 0.4173(3) 0.0097(7) 0.011(2) Uiso 1 d DU . . N28 N 0.6300(4) 0.6621(4) 0.0042(8) 0.022(3) Uiso 1 d DU . . N29 N 0.0782(4) 0.4206(3) 0.5081(7) 0.016(2) Uiso 1 d DU . . N30 N -0.1273(4) 0.6633(4) 0.5030(8) 0.018(2) Uiso 1 d DU . . N31 N 0.4229(3) 0.0811(3) 0.5086(7) 0.011(2) Uiso 1 d DU . . N32 N 0.6318(4) -0.1596(4) 0.5089(9) 0.033(3) Uiso 1 d DU . . C1 C 0.0710(4) 0.2282(4) 0.1765(6) 0.020(2) Uiso 1 d DU . . C2 C 0.0734(5) 0.2797(4) 0.3248(6) 0.023(2) Uiso 1 d DU . . C3 C 0.2301(4) 0.0941(4) 0.1664(6) 0.020(2) Uiso 1 d DU . . C4 C 0.2872(4) 0.0930(4) 0.3083(5) 0.0114(19) Uiso 1 d DU . . C5 C 0.0580(4) 0.2145(3) -0.1825(5) 0.0074(13) Uiso 1 d DU . . C6 C 0.0586(4) 0.2780(4) -0.3129(5) 0.0074(13) Uiso 1 d DU . . C7 C 0.2135(4) 0.0917(4) -0.1926(5) 0.017(2) Uiso 1 d DU . . C8 C 0.2714(4) 0.0963(4) -0.3332(6) 0.019(2) Uiso 1 d DU . . C9 C 0.2798(4) 0.4078(4) 0.1960(6) 0.022(2) Uiso 1 d DU . . C10 C 0.2220(4) 0.4061(4) 0.3375(6) 0.021(2) Uiso 1 d DU . . C11 C 0.4433(5) 0.2769(4) 0.1898(7) 0.027(3) Uiso 1 d DU . . C12 C 0.4452(5) 0.2197(5) 0.3293(7) 0.029(3) Uiso 1 d DU . . C13 C 0.2755(4) 0.4039(4) -0.1565(6) 0.019(2) Uiso 1 d DU . . C14 C 0.2180(4) 0.4060(4) -0.2981(6) 0.023(2) Uiso 1 d DU . . C15 C 0.4315(4) 0.2754(3) -0.1697(5) 0.0074(19) Uiso 1 d DU . . C16 C 0.4282(5) 0.2203(4) -0.3114(6) 0.021(2) Uiso 1 d DU . . C17 C 0.0977(4) 0.0224(4) 0.0078(7) 0.011(2) Uiso 1 d DU . . H17 H 0.1396 0.0148 0.0081 0.013 Uiso 1 calc R . . C18 C 0.0583(4) -0.0264(4) 0.0064(6) 0.011(2) Uiso 1 d DU . . H18 H 0.0734 -0.0662 0.0050 0.013 Uiso 1 calc R . . C19 C -0.0028(3) -0.0162(3) 0.0070(6) 0.005(2) Uiso 1 d DU . . C20 C -0.0463(4) -0.0686(4) 0.0074(8) 0.021(3) Uiso 1 d DU . . C21 C -0.0265(4) -0.1267(4) 0.0098(6) 0.017(3) Uiso 1 d DU . . H21 H 0.0152 -0.1352 0.0128 0.020 Uiso 1 calc R . . C22 C -0.0685(4) -0.1730(4) 0.0079(8) 0.031(3) Uiso 1 d DU . . H22 H -0.0543 -0.2131 0.0126 0.037 Uiso 1 calc R . . C23 C -0.1477(4) -0.1079(4) -0.0025(8) 0.027(3) Uiso 1 d DU . . H23 H -0.1894 -0.1006 -0.0101 0.032 Uiso 1 calc R . . C24 C -0.1077(4) -0.0594(4) 0.0060(8) 0.032(3) Uiso 1 d DU . . H24 H -0.1231 -0.0197 0.0108 0.039 Uiso 1 calc R . . C25 C -0.0225(4) 0.0425(4) 0.0082(6) 0.0071(17) Uiso 1 d DU . . H25 H -0.0642 0.0511 0.0086 0.009 Uiso 1 calc R . . C26 C 0.0194(3) 0.0891(3) 0.0089(7) 0.0071(17) Uiso 1 d DU . . H26 H 0.0053 0.1293 0.0094 0.009 Uiso 1 calc R . . C27 C 0.4069(4) 0.4744(4) 0.0110(7) 0.0105(17) Uiso 1 d DU . . H27 H 0.3651 0.4820 0.0128 0.013 Uiso 1 calc R . . C28 C 0.4469(4) 0.5232(3) 0.0099(6) 0.0105(17) Uiso 1 d DU . . H28 H 0.4318 0.5629 0.0103 0.013 Uiso 1 calc R . . C29 C 0.5073(4) 0.5135(3) 0.0082(7) 0.011(3) Uiso 1 d DU . . C30 C 0.5513(4) 0.5640(4) 0.0101(7) 0.014(3) Uiso 1 d DU . . C31 C 0.5301(4) 0.6227(4) 0.0108(7) 0.021(3) Uiso 1 d DU . . H31 H 0.4883 0.6305 0.0126 0.025 Uiso 1 calc R . . C32 C 0.5707(4) 0.6699(4) 0.0086(8) 0.025(3) Uiso 1 d DU . . H32 H 0.5556 0.7096 0.0104 0.030 Uiso 1 calc R . . C33 C 0.6498(4) 0.6054(4) 0.0058(7) 0.022(3) Uiso 1 d DU . . H33 H 0.6916 0.5984 -0.0002 0.027 Uiso 1 calc R . . C34 C 0.6121(4) 0.5565(4) 0.0157(7) 0.021(3) Uiso 1 d DU . . H34 H 0.6284 0.5177 0.0263 0.025 Uiso 1 calc R . . C35 C 0.5275(4) 0.4545(4) 0.0079(7) 0.011(2) Uiso 1 d DU . . H35 H 0.5693 0.4461 0.0081 0.013 Uiso 1 calc R . . C36 C 0.4856(3) 0.4075(3) 0.0073(7) 0.008(2) Uiso 1 d DU . . H36 H 0.4997 0.3673 0.0052 0.009 Uiso 1 calc R . . C37 C 0.0969(4) 0.4778(4) 0.5132(7) 0.016(3) Uiso 1 d DU . . H37 H 0.1387 0.4852 0.5164 0.020 Uiso 1 calc R . . C38 C 0.0593(4) 0.5257(4) 0.5140(6) 0.017(3) Uiso 1 d DU . . H38 H 0.0750 0.5652 0.5179 0.021 Uiso 1 calc R . . C39 C -0.0035(4) 0.5164(4) 0.5090(7) 0.017(3) Uiso 1 d DU . . C40 C -0.0459(3) 0.5669(3) 0.5073(6) 0.007(2) Uiso 1 d DU . . C41 C -0.0272(4) 0.6256(4) 0.4995(6) 0.015(3) Uiso 1 d DU . . H41 H 0.0144 0.6342 0.4954 0.019 Uiso 1 calc R . . C42 C -0.0675(4) 0.6714(4) 0.4976(7) 0.019(3) Uiso 1 d DU . . H42 H -0.0526 0.7112 0.4921 0.023 Uiso 1 calc R . . C43 C -0.1455(4) 0.6073(4) 0.5121(7) 0.023(3) Uiso 1 d DU . . H43 H -0.1873 0.6004 0.5193 0.027 Uiso 1 calc R . . C44 C -0.1082(4) 0.5581(4) 0.5119(7) 0.025(3) Uiso 1 d DU . . H44 H -0.1244 0.5188 0.5150 0.030 Uiso 1 calc R . . C45 C -0.0220(4) 0.4568(4) 0.5055(7) 0.017(2) Uiso 1 d DU . . H45 H -0.0636 0.4477 0.5028 0.020 Uiso 1 calc R . . C46 C 0.0185(4) 0.4114(4) 0.5059(8) 0.019(2) Uiso 1 d DU . . H46 H 0.0042 0.3713 0.5046 0.023 Uiso 1 calc R . . C47 C 0.4826(4) 0.0921(4) 0.5152(8) 0.021(3) Uiso 1 d DU . . H47 H 0.4959 0.1325 0.5197 0.025 Uiso 1 calc R . . C48 C 0.5239(4) 0.0477(4) 0.5158(6) 0.018(3) Uiso 1 d DU . . H48 H 0.5650 0.0580 0.5212 0.021 Uiso 1 calc R . . C49 C 0.5082(4) -0.0124(4) 0.5086(7) 0.015(3) Uiso 1 d DU . . C50 C 0.5501(3) -0.0629(4) 0.5084(7) 0.012(2) Uiso 1 d DU . . C51 C 0.6116(3) -0.0551(3) 0.4915(6) 0.0078(19) Uiso 1 d DU . . H51 H 0.6270 -0.0161 0.4788 0.009 Uiso 1 calc R . . C52 C 0.6493(4) -0.1028(4) 0.4931(7) 0.028(3) Uiso 1 d DU . . H52 H 0.6908 -0.0956 0.4824 0.034 Uiso 1 calc R . . C53 C 0.5730(4) -0.1684(4) 0.5221(7) 0.022(3) Uiso 1 d DU . . H53 H 0.5588 -0.2084 0.5280 0.027 Uiso 1 calc R . . C54 C 0.5324(4) -0.1225(4) 0.5275(8) 0.025(3) Uiso 1 d DU . . H54 H 0.4918 -0.1309 0.5443 0.031 Uiso 1 calc R . . C55 C 0.4445(4) -0.0224(4) 0.5043(7) 0.014(2) Uiso 1 d DU . . H55 H 0.4295 -0.0623 0.5021 0.017 Uiso 1 calc R . . C56 C 0.4064(4) 0.0235(4) 0.5034(7) 0.017(2) Uiso 1 d DU . . H56 H 0.3648 0.0148 0.4987 0.020 Uiso 1 calc R . . C57 C 0.2210(4) 0.2529(6) 0.2507(12) 0.031(3) Uiso 1 d D . . H57A H 0.2103 0.2916 0.2807 0.047 Uiso 1 calc R . . H57B H 0.2007 0.2207 0.2874 0.047 Uiso 1 calc R . . H57C H 0.2086 0.2523 0.1798 0.047 Uiso 1 calc R . . C58 C 0.2790(5) 0.2557(7) -0.2433(13) 0.054(5) Uiso 1 d D . . H58A H 0.2980 0.2902 -0.2106 0.081 Uiso 1 calc R . . H58B H 0.2913 0.2541 -0.3142 0.081 Uiso 1 calc R . . H58C H 0.2915 0.2188 -0.2092 0.081 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0072(8) 0.0078(8) 0.0085(8) -0.0023(5) 0.0003(6) -0.0015(6) Fe2 0.0161(10) 0.0160(10) 0.0158(10) -0.0017(6) 0.0023(6) -0.0006(7) Fe3 0.0121(9) 0.0091(9) 0.0188(10) 0.0006(6) 0.0030(6) -0.0013(7) Fe4 0.0082(8) 0.0084(8) 0.0120(9) 0.0016(5) 0.0021(6) 0.0006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N4 2.117(7) . ? Fe1 N10 2.150(7) . ? Fe1 N1 2.159(7) . ? Fe1 N7 2.187(7) . ? Fe1 N25 2.188(7) . ? Fe1 O1 2.214(7) . ? Fe2 N19 2.109(7) . ? Fe2 N13 2.113(7) . ? Fe2 N16 2.161(8) . ? Fe2 O2 2.173(7) . ? Fe2 N22 2.180(8) . ? Fe2 N27 2.215(7) . ? Fe3 N3 2.150(7) . ? Fe3 N9 2.155(7) 1_556 ? Fe3 N15 2.160(7) . ? Fe3 O3 2.165(7) . ? Fe3 N21 2.167(7) 1_556 ? Fe3 N29 2.183(7) . ? Fe4 N18 2.121(7) . ? Fe4 N24 2.140(7) 1_556 ? Fe4 N12 2.143(7) 1_556 ? Fe4 N31 2.172(7) . ? Fe4 N6 2.175(7) . ? Fe4 O4 2.195(6) . ? O5 C57 1.406(10) . ? O6 C58 1.387(11) . ? N1 C1 1.164(8) . ? N2 C1 1.309(8) . ? N2 C2 1.318(8) . ? N3 C2 1.148(8) . ? N4 C3 1.150(8) . ? N5 C3 1.277(8) . ? N5 C4 1.312(8) . ? N6 C4 1.145(8) . ? N7 C5 1.158(8) . ? N8 C6 1.305(8) . ? N8 C5 1.338(8) . ? N9 C6 1.136(8) . ? N9 Fe3 2.155(7) 1_554 ? N10 C7 1.140(8) . ? N11 C7 1.312(8) . ? N11 C8 1.314(8) . ? N12 C8 1.144(8) . ? N12 Fe4 2.143(7) 1_554 ? N13 C9 1.169(8) . ? N14 C9 1.299(8) . ? N14 C10 1.312(8) . ? N15 C10 1.153(8) . ? N16 C11 1.163(9) . ? N17 C11 1.305(9) . ? N17 C12 1.326(9) . ? N18 C12 1.153(8) . ? N19 C13 1.162(8) . ? N20 C14 1.304(8) . ? N20 C13 1.329(8) . ? N21 C14 1.141(8) . ? N21 Fe3 2.167(7) 1_554 ? N22 C15 1.167(8) . ? N23 C15 1.315(8) . ? N23 C16 1.317(8) . ? N24 C16 1.140(8) . ? N24 Fe4 2.140(7) 1_554 ? N25 C17 1.336(8) . ? N25 C26 1.340(8) . ? N26 C22 1.333(9) . ? N26 C23 1.340(9) . ? N27 C36 1.343(8) . ? N27 C27 1.345(8) . ? N28 C32 1.336(9) . ? N28 C33 1.340(9) . ? N29 C37 1.346(9) . ? N29 C46 1.349(9) . ? N30 C43 1.320(9) . ? N30 C42 1.349(9) . ? N31 C56 1.339(9) . ? N31 C47 1.358(9) . ? N32 C53 1.338(9) . ? N32 C52 1.342(9) . ? C17 C18 1.400(9) . ? C18 C19 1.383(9) . ? C19 C25 1.381(8) . ? C19 C20 1.521(9) . ? C20 C21 1.370(9) . ? C20 C24 1.386(9) . ? C21 C22 1.397(9) . ? C23 C24 1.408(10) . ? C25 C26 1.398(9) . ? C27 C28 1.407(9) . ? C28 C29 1.366(9) . ? C29 C35 1.392(9) . ? C29 C30 1.495(9) . ? C30 C34 1.369(9) . ? C30 C31 1.394(9) . ? C31 C32 1.389(9) . ? C33 C34 1.383(9) . ? C35 C36 1.407(9) . ? C37 C38 1.358(9) . ? C38 C39 1.418(9) . ? C39 C45 1.396(9) . ? C39 C40 1.471(8) . ? C40 C41 1.378(9) . ? C40 C44 1.406(9) . ? C41 C42 1.362(9) . ? C43 C44 1.377(9) . ? C45 C46 1.359(10) . ? C47 C48 1.352(9) . ? C48 C49 1.389(9) . ? C49 C55 1.440(9) . ? C49 C50 1.467(9) . ? C50 C51 1.402(9) . ? C50 C54 1.410(9) . ? C51 C52 1.358(9) . ? C53 C54 1.371(9) . ? C55 C56 1.332(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N10 89.8(3) . . ? N4 Fe1 N1 89.7(3) . . ? N10 Fe1 N1 179.4(3) . . ? N4 Fe1 N7 177.3(3) . . ? N10 Fe1 N7 88.7(3) . . ? N1 Fe1 N7 91.8(3) . . ? N4 Fe1 N25 92.7(3) . . ? N10 Fe1 N25 92.1(3) . . ? N1 Fe1 N25 88.3(3) . . ? N7 Fe1 N25 85.0(3) . . ? N4 Fe1 O1 98.6(3) . . ? N10 Fe1 O1 89.0(3) . . ? N1 Fe1 O1 90.7(3) . . ? N7 Fe1 O1 83.7(3) . . ? N25 Fe1 O1 168.7(3) . . ? N19 Fe2 N13 90.5(3) . . ? N19 Fe2 N16 177.7(3) . . ? N13 Fe2 N16 88.6(3) . . ? N19 Fe2 O2 96.9(3) . . ? N13 Fe2 O2 89.9(3) . . ? N16 Fe2 O2 85.3(3) . . ? N19 Fe2 N22 89.6(3) . . ? N13 Fe2 N22 179.6(4) . . ? N16 Fe2 N22 91.2(3) . . ? O2 Fe2 N22 90.4(3) . . ? N19 Fe2 N27 93.1(3) . . ? N13 Fe2 N27 92.6(3) . . ? N16 Fe2 N27 84.7(3) . . ? O2 Fe2 N27 169.6(3) . . ? N22 Fe2 N27 87.0(3) . . ? N3 Fe3 N9 92.3(3) . 1_556 ? N3 Fe3 N15 88.2(3) . . ? N9 Fe3 N15 177.7(3) 1_556 . ? N3 Fe3 O3 92.2(3) . . ? N9 Fe3 O3 85.1(3) 1_556 . ? N15 Fe3 O3 97.2(3) . . ? N3 Fe3 N21 177.0(3) . 1_556 ? N9 Fe3 N21 90.5(3) 1_556 1_556 ? N15 Fe3 N21 89.0(3) . 1_556 ? O3 Fe3 N21 89.1(3) . 1_556 ? N3 Fe3 N29 88.2(3) . . ? N9 Fe3 N29 86.6(3) 1_556 . ? N15 Fe3 N29 91.1(3) . . ? O3 Fe3 N29 171.7(3) . . ? N21 Fe3 N29 91.0(3) 1_556 . ? N18 Fe4 N24 90.4(3) . 1_556 ? N18 Fe4 N12 178.3(3) . 1_556 ? N24 Fe4 N12 90.2(3) 1_556 1_556 ? N18 Fe4 N31 85.9(3) . . ? N24 Fe4 N31 89.3(3) 1_556 . ? N12 Fe4 N31 92.6(3) 1_556 . ? N18 Fe4 N6 90.7(3) . . ? N24 Fe4 N6 178.9(3) 1_556 . ? N12 Fe4 N6 88.7(3) 1_556 . ? N31 Fe4 N6 90.9(3) . . ? N18 Fe4 O4 85.0(3) . . ? N24 Fe4 O4 92.2(3) 1_556 . ? N12 Fe4 O4 96.5(3) 1_556 . ? N31 Fe4 O4 170.8(3) . . ? N6 Fe4 O4 87.7(3) . . ? C1 N1 Fe1 172.0(7) . . ? C1 N2 C2 120.2(8) . . ? C2 N3 Fe3 171.1(8) . . ? C3 N4 Fe1 177.3(8) . . ? C3 N5 C4 122.8(9) . . ? C4 N6 Fe4 172.9(7) . . ? C5 N7 Fe1 165.9(8) . . ? C6 N8 C5 115.5(7) . . ? C6 N9 Fe3 163.5(8) . 1_554 ? C7 N10 Fe1 168.7(7) . . ? C7 N11 C8 119.7(8) . . ? C8 N12 Fe4 174.1(8) . 1_554 ? C9 N13 Fe2 174.1(8) . . ? C9 N14 C10 121.4(8) . . ? C10 N15 Fe3 167.9(8) . . ? C11 N16 Fe2 165.4(8) . . ? C11 N17 C12 117.4(9) . . ? C12 N18 Fe4 165.6(8) . . ? C13 N19 Fe2 176.7(7) . . ? C14 N20 C13 119.6(9) . . ? C14 N21 Fe3 173.1(8) . 1_554 ? C15 N22 Fe2 171.9(8) . . ? C15 N23 C16 117.2(7) . . ? C16 N24 Fe4 173.2(9) . 1_554 ? C17 N25 C26 118.3(6) . . ? C17 N25 Fe1 120.6(6) . . ? C26 N25 Fe1 120.8(5) . . ? C22 N26 C23 118.1(7) . . ? C36 N27 C27 118.1(6) . . ? C36 N27 Fe2 122.9(5) . . ? C27 N27 Fe2 119.0(5) . . ? C32 N28 C33 116.6(7) . . ? C37 N29 C46 116.8(7) . . ? C37 N29 Fe3 122.5(6) . . ? C46 N29 Fe3 120.5(6) . . ? C43 N30 C42 115.8(7) . . ? C56 N31 C47 116.6(7) . . ? C56 N31 Fe4 124.0(6) . . ? C47 N31 Fe4 119.4(6) . . ? C53 N32 C52 116.5(7) . . ? N1 C1 N2 177.4(11) . . ? N3 C2 N2 167.6(11) . . ? N4 C3 N5 176.2(10) . . ? N6 C4 N5 173.2(9) . . ? N7 C5 N8 173.7(9) . . ? N9 C6 N8 171.2(10) . . ? N10 C7 N11 173.2(10) . . ? N12 C8 N11 168.4(10) . . ? N13 C9 N14 174.9(10) . . ? N15 C10 N14 173.4(10) . . ? N16 C11 N17 176.3(11) . . ? N18 C12 N17 168.4(12) . . ? N19 C13 N20 172.7(10) . . ? N21 C14 N20 170.4(11) . . ? N22 C15 N23 170.1(9) . . ? N24 C16 N23 171.0(11) . . ? N25 C17 C18 122.4(7) . . ? C19 C18 C17 119.4(6) . . ? C25 C19 C18 118.0(6) . . ? C25 C19 C20 121.8(7) . . ? C18 C19 C20 120.2(7) . . ? C21 C20 C24 117.5(7) . . ? C21 C20 C19 121.4(8) . . ? C24 C20 C19 121.1(8) . . ? C20 C21 C22 118.9(7) . . ? N26 C22 C21 123.8(8) . . ? N26 C23 C24 120.6(7) . . ? C20 C24 C23 120.8(8) . . ? C19 C25 C26 119.6(6) . . ? N25 C26 C25 122.3(7) . . ? N27 C27 C28 122.0(7) . . ? C29 C28 C27 120.3(7) . . ? C28 C29 C35 118.0(6) . . ? C28 C29 C30 122.0(7) . . ? C35 C29 C30 120.0(7) . . ? C34 C30 C31 116.8(7) . . ? C34 C30 C29 124.1(8) . . ? C31 C30 C29 119.1(7) . . ? C32 C31 C30 119.4(7) . . ? N28 C32 C31 123.3(7) . . ? N28 C33 C34 123.0(7) . . ? C30 C34 C33 120.1(7) . . ? C29 C35 C36 119.3(6) . . ? N27 C36 C35 122.3(7) . . ? N29 C37 C38 123.8(7) . . ? C37 C38 C39 119.7(7) . . ? C45 C39 C38 115.7(6) . . ? C45 C39 C40 122.7(8) . . ? C38 C39 C40 121.7(8) . . ? C41 C40 C44 115.8(6) . . ? C41 C40 C39 122.3(8) . . ? C44 C40 C39 121.9(8) . . ? C42 C41 C40 121.0(7) . . ? N30 C42 C41 123.4(7) . . ? N30 C43 C44 124.7(7) . . ? C43 C44 C40 119.1(7) . . ? C46 C45 C39 120.9(7) . . ? N29 C46 C45 123.0(8) . . ? C48 C47 N31 122.4(7) . . ? C47 C48 C49 122.3(7) . . ? C48 C49 C55 113.7(6) . . ? C48 C49 C50 125.6(8) . . ? C55 C49 C50 120.6(8) . . ? C51 C50 C54 115.0(6) . . ? C51 C50 C49 121.9(7) . . ? C54 C50 C49 123.1(8) . . ? C52 C51 C50 120.4(7) . . ? N32 C52 C51 124.2(8) . . ? N32 C53 C54 123.1(7) . . ? C53 C54 C50 120.6(7) . . ? C56 C55 C49 120.7(7) . . ? C55 C56 N31 124.2(7) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.722 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.111 #=END data_6 _database_code_CSD 172408 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Co(dca)2(4,4'-bipy)(H2O).0.5MeOH _chemical_formula_sum 'C29 H24 Co2 N16 O3' _chemical_formula_weight 762.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 22.2246(2) _cell_length_b 22.2246(2) _cell_length_c 13.1576(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6498.97(10) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 62963 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 28.28 _exptl_crystal_description Prismatic _exptl_crystal_colour Red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 1.081 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.697 _exptl_absorpt_correction_T_max 0.755 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method Phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62963 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.28 _reflns_number_total 16005 _reflns_number_gt 13230 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett and Johnson, 1996)' _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^)+(0.0398P)^2^+0.8410P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(8) _refine_ls_number_reflns 16005 _refine_ls_number_parameters 846 _refine_ls_number_restraints 1035 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.005 _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 0.14147(3) 0.15397(4) -0.0033 0.01107(19) Uani 1 1 d . . . Co2 Co 0.36075(3) 0.34355(4) 0.02006(6) 0.01086(19) Uani 1 1 d . . . Co3 Co 0.13994(4) 0.34541(4) 0.51829(8) 0.01165(19) Uani 1 1 d . . . Co4 Co 0.36076(4) 0.15533(4) 0.49838(9) 0.01221(19) Uani 1 1 d . . . O1 O 0.19326(12) 0.23302(12) -0.0303(2) 0.0170(6) Uani 1 1 d . . . O2 O 0.30735(11) 0.26280(11) 0.0470(2) 0.0148(6) Uani 1 1 d . . . O3 O 0.19248(12) 0.26359(11) 0.5442(2) 0.0168(6) Uani 1 1 d . . . O4 O 0.30765(12) 0.23428(12) 0.4716(2) 0.0154(6) Uani 1 1 d . . . O5 O 0.28461(17) 0.2382(2) 0.2496(3) 0.0292(12) Uani 1 1 d D . . O6 O 0.21621(18) 0.2393(2) -0.2546(4) 0.0339(12) Uani 1 1 d D . . N1 N 0.0920(2) 0.1970(2) 0.1123(3) 0.0180(10) Uani 1 1 d D . . N2 N 0.0453(2) 0.2596(2) 0.2461(4) 0.0309(15) Uani 1 1 d D . . N3 N 0.09419(19) 0.3031(2) 0.3957(3) 0.0165(10) Uani 1 1 d D . . N4 N 0.19997(18) 0.11800(19) 0.1049(3) 0.0216(10) Uani 1 1 d D . . N5 N 0.2631(2) 0.0674(2) 0.2322(4) 0.0374(14) Uani 1 1 d D . . N6 N 0.31324(18) 0.11132(18) 0.3801(3) 0.0184(9) Uani 1 1 d D . . N7 N 0.08388(19) 0.1893(2) -0.1173(3) 0.0196(10) Uani 1 1 d D . . N8 N 0.0284(2) 0.2437(3) -0.2504(4) 0.0279(14) Uani 1 1 d D . . N9 N 0.0797(2) 0.3076(2) -0.3744(3) 0.0171(10) Uani 1 1 d D . . N10 N 0.1910(2) 0.10931(19) -0.1195(3) 0.0193(9) Uani 1 1 d D . . N11 N 0.2369(2) 0.0659(2) -0.2728(4) 0.0324(13) Uani 1 1 d D . . N12 N 0.30066(19) 0.11697(19) -0.3964(3) 0.0198(10) Uani 1 1 d D . . N13 N 0.31160(19) 0.38522(19) 0.1362(3) 0.0205(10) Uani 1 1 d D . . N14 N 0.2452(2) 0.4320(3) 0.2633(4) 0.0377(16) Uani 1 1 d D . . N15 N 0.19787(19) 0.38542(19) 0.4118(3) 0.0178(9) Uani 1 1 d D . . N16 N 0.4202(2) 0.30847(19) 0.1281(3) 0.0161(10) Uani 1 1 d D . . N17 N 0.4746(2) 0.2476(3) 0.2566(5) 0.0310(15) Uani 1 1 d D . . N18 N 0.41977(19) 0.1937(2) 0.3914(3) 0.0189(10) Uani 1 1 d D . . N19 N 0.30295(18) 0.38168(18) -0.0886(3) 0.0170(9) Uani 1 1 d D . . N20 N 0.2498(2) 0.4325(3) -0.2285(4) 0.0460(19) Uani 1 1 d D . . N21 N 0.18953(18) 0.38656(17) -0.3633(3) 0.0171(9) Uani 1 1 d D . . N22 N 0.40665(18) 0.2996(2) -0.0986(3) 0.0175(10) Uani 1 1 d D . . N23 N 0.4582(2) 0.2495(3) -0.2416(4) 0.0304(13) Uani 1 1 d D . . N24 N 0.4083(2) 0.1978(2) -0.3805(3) 0.0170(10) Uani 1 1 d D . . N25 N 0.07974(19) 0.07997(18) 0.0054(3) 0.0120(9) Uani 1 1 d D . . N26 N -0.1276(2) -0.1639(2) -0.0023(4) 0.0163(11) Uani 1 1 d D . . N27 N 0.4241(2) 0.41660(19) 0.0076(3) 0.0120(9) Uani 1 1 d D . . N28 N 0.6298(2) 0.6609(2) 0.0028(4) 0.0193(13) Uani 1 1 d D . . N29 N 0.07989(18) 0.41962(19) 0.5079(3) 0.0130(9) Uani 1 1 d D . . N30 N -0.1251(2) 0.6649(2) 0.5017(4) 0.0271(14) Uani 1 1 d D . . N31 N 0.42231(18) 0.08274(19) 0.5074(3) 0.0130(9) Uani 1 1 d D . . N32 N 0.6307(2) -0.1605(3) 0.5055(5) 0.0328(16) Uani 1 1 d D . . C1 C 0.0715(2) 0.2270(2) 0.1785(3) 0.0157(11) Uani 1 1 d D . . C2 C 0.0741(2) 0.2810(2) 0.3249(4) 0.0188(12) Uani 1 1 d D . . C3 C 0.2298(2) 0.0958(2) 0.1671(3) 0.0187(11) Uani 1 1 d D . . C4 C 0.2882(2) 0.0934(2) 0.3091(3) 0.0177(11) Uani 1 1 d D . . C5 C 0.0593(2) 0.2154(2) -0.1815(4) 0.0127(10) Uani 1 1 d D . . C6 C 0.0589(3) 0.2782(3) -0.3145(4) 0.0225(13) Uani 1 1 d D . . C7 C 0.2139(2) 0.0927(2) -0.1917(3) 0.0167(11) Uani 1 1 d D . . C8 C 0.2708(2) 0.0967(2) -0.3366(3) 0.0223(12) Uani 1 1 d D . . C9 C 0.2792(2) 0.4053(2) 0.1977(3) 0.0195(11) Uani 1 1 d D . . C10 C 0.2217(2) 0.4050(2) 0.3407(3) 0.0212(12) Uani 1 1 d D . . C11 C 0.4437(2) 0.2783(2) 0.1890(3) 0.0142(11) Uani 1 1 d D . . C12 C 0.4437(2) 0.2204(2) 0.3274(4) 0.0168(12) Uani 1 1 d D . . C13 C 0.2772(2) 0.4024(2) -0.1562(3) 0.0184(11) Uani 1 1 d D . . C14 C 0.2177(2) 0.4043(2) -0.2979(4) 0.0245(12) Uani 1 1 d D . . C15 C 0.4284(2) 0.2758(2) -0.1675(4) 0.0166(11) Uani 1 1 d D . . C16 C 0.4285(2) 0.2227(3) -0.3129(4) 0.0219(13) Uani 1 1 d D . . C17 C 0.0987(2) 0.0218(2) 0.0045(4) 0.0163(11) Uani 1 1 d DU . . H17 H 0.1407 0.0140 0.0035 0.020 Uiso 1 1 calc R . . C18 C 0.0596(3) -0.0260(2) 0.0048(4) 0.0208(13) Uani 1 1 d DU . . H18 H 0.0750 -0.0659 0.0048 0.025 Uiso 1 1 calc R . . C19 C -0.0025(2) -0.0167(2) 0.0053(4) 0.0152(10) Uani 1 1 d DU . . C20 C -0.0456(2) -0.0677(2) 0.0033(4) 0.0152(10) Uani 1 1 d DU . . C21 C -0.0260(2) -0.1267(2) 0.0075(4) 0.0201(9) Uani 1 1 d DU . . H21 H 0.0157 -0.1354 0.0121 0.024 Uiso 1 1 calc R . . C22 C -0.0678(2) -0.1734(2) 0.0048(4) 0.0201(9) Uani 1 1 d DU . . H22 H -0.0536 -0.2137 0.0081 0.024 Uiso 1 1 calc R . . C23 C -0.1462(2) -0.1073(3) -0.0047(5) 0.0278(16) Uani 1 1 d DU . . H23 H -0.1883 -0.0997 -0.0085 0.033 Uiso 1 1 calc R . . C24 C -0.1069(3) -0.0578(2) -0.0018(5) 0.0242(15) Uani 1 1 d DU . . H24 H -0.1222 -0.0179 -0.0034 0.029 Uiso 1 1 calc R . . C25 C -0.0219(2) 0.0442(2) 0.0063(4) 0.0141(10) Uani 1 1 d DU . . H25 H -0.0635 0.0538 0.0068 0.017 Uiso 1 1 calc R . . C26 C 0.0213(2) 0.0896(2) 0.0065(4) 0.0141(10) Uani 1 1 d DU . . H26 H 0.0077 0.1301 0.0076 0.017 Uiso 1 1 calc R . . C27 C 0.4058(2) 0.4736(2) 0.0086(4) 0.0174(12) Uani 1 1 d DU . . H27 H 0.3638 0.4816 0.0101 0.021 Uiso 1 1 calc R . . C28 C 0.4455(2) 0.5218(2) 0.0073(4) 0.0161(12) Uani 1 1 d DU . . H28 H 0.4303 0.5618 0.0071 0.019 Uiso 1 1 calc R . . C29 C 0.5070(2) 0.5124(2) 0.0065(4) 0.0142(11) Uani 1 1 d DU . . C30 C 0.5498(2) 0.5639(2) 0.0057(4) 0.0173(12) Uani 1 1 d DU . . C31 C 0.5298(2) 0.6233(2) 0.0079(4) 0.0221(10) Uani 1 1 d DU . . H31 H 0.4878 0.6315 0.0099 0.027 Uiso 1 1 calc R . . C32 C 0.5704(2) 0.6699(2) 0.0070(4) 0.0221(10) Uani 1 1 d DU . . H32 H 0.5557 0.7100 0.0096 0.027 Uiso 1 1 calc R . . C33 C 0.6500(2) 0.6041(3) 0.0050(5) 0.0283(15) Uani 1 1 d DU . . H33 H 0.6922 0.5974 0.0059 0.034 Uiso 1 1 calc R . . C34 C 0.6115(2) 0.5540(2) 0.0060(5) 0.0208(14) Uani 1 1 d DU . . H34 H 0.6273 0.5143 0.0069 0.025 Uiso 1 1 calc R . . C35 C 0.5260(2) 0.4518(2) 0.0051(4) 0.0132(13) Uani 1 1 d DU . . H35 H 0.5675 0.4418 0.0041 0.016 Uiso 1 1 calc R . . C36 C 0.4822(2) 0.4072(2) 0.0052(4) 0.0124(13) Uani 1 1 d DU . . H36 H 0.4956 0.3666 0.0033 0.015 Uiso 1 1 calc R . . C37 C 0.0992(2) 0.4761(2) 0.5126(4) 0.0100(9) Uani 1 1 d DU . . H37 H 0.1412 0.4833 0.5171 0.012 Uiso 1 1 calc R . . C38 C 0.0604(2) 0.5249(2) 0.5112(3) 0.0100(9) Uani 1 1 d DU . . H38 H 0.0761 0.5647 0.5133 0.012 Uiso 1 1 calc R . . C39 C -0.0016(2) 0.51573(19) 0.5067(4) 0.0110(10) Uani 1 1 d DU . . C40 C -0.0445(2) 0.5670(2) 0.5060(4) 0.0133(11) Uani 1 1 d DU . . C41 C -0.0251(2) 0.6252(2) 0.4974(4) 0.0193(11) Uani 1 1 d DU . . H41 H 0.0168 0.6334 0.4939 0.023 Uiso 1 1 calc R . . C42 C -0.0653(2) 0.6720(2) 0.4937(4) 0.0222(11) Uani 1 1 d DU . . H42 H -0.0500 0.7116 0.4850 0.027 Uiso 1 1 calc R . . C43 C -0.1448(2) 0.6082(2) 0.5082(4) 0.0223(14) Uani 1 1 d DU . . H43 H -0.1871 0.6016 0.5090 0.027 Uiso 1 1 calc R . . C44 C -0.1078(2) 0.5590(2) 0.5138(5) 0.0213(14) Uani 1 1 d DU . . H44 H -0.1242 0.5200 0.5229 0.026 Uiso 1 1 calc R . . C45 C -0.0212(2) 0.4569(2) 0.5003(4) 0.0123(11) Uani 1 1 d DU . . H45 H -0.0631 0.4488 0.4957 0.015 Uiso 1 1 calc R . . C46 C 0.0190(2) 0.4099(2) 0.5006(4) 0.0154(12) Uani 1 1 d DU . . H46 H 0.0044 0.3698 0.4957 0.018 Uiso 1 1 calc R . . C47 C 0.4835(2) 0.0930(2) 0.5105(4) 0.0139(13) Uani 1 1 d DU . . H47 H 0.4978 0.1332 0.5127 0.017 Uiso 1 1 calc R . . C48 C 0.5240(2) 0.0466(2) 0.5106(4) 0.0164(13) Uani 1 1 d DU . . H48 H 0.5659 0.0553 0.5131 0.020 Uiso 1 1 calc R . . C49 C 0.5052(2) -0.0122(2) 0.5073(4) 0.0115(9) Uani 1 1 d DU . . C50 C 0.5490(2) -0.0626(2) 0.5072(4) 0.0115(9) Uani 1 1 d DU . . C51 C 0.6111(2) -0.0552(2) 0.4914(4) 0.0181(12) Uani 1 1 d DU . . H51 H 0.6270 -0.0159 0.4815 0.022 Uiso 1 1 calc R . . C52 C 0.6490(2) -0.1036(2) 0.4900(4) 0.0193(12) Uani 1 1 d DU . . H52 H 0.6905 -0.0967 0.4774 0.023 Uiso 1 1 calc R . . C53 C 0.5708(2) -0.1680(2) 0.5174(4) 0.0235(12) Uani 1 1 d DU . . H53 H 0.5560 -0.2080 0.5235 0.028 Uiso 1 1 calc R . . C54 C 0.5302(2) -0.1221(2) 0.5214(4) 0.0206(11) Uani 1 1 d DU . . H54 H 0.4889 -0.1305 0.5338 0.025 Uiso 1 1 calc R . . C55 C 0.4428(2) -0.0231(2) 0.5026(4) 0.0118(9) Uani 1 1 d DU . . H55 H 0.4277 -0.0630 0.4985 0.014 Uiso 1 1 calc R . . C56 C 0.4041(2) 0.0253(2) 0.5040(4) 0.0118(9) Uani 1 1 d DU . . H56 H 0.3621 0.0175 0.5024 0.014 Uiso 1 1 calc R . . C57 C 0.2217(2) 0.2432(3) 0.2681(6) 0.0290(18) Uani 1 1 d D . . H57A H 0.2135 0.2808 0.3043 0.043 Uiso 1 1 calc R . . H57B H 0.2084 0.2090 0.3096 0.043 Uiso 1 1 calc R . . H57C H 0.2000 0.2431 0.2033 0.043 Uiso 1 1 calc R . . C58 C 0.2782(3) 0.2439(3) -0.2357(5) 0.0312(18) Uani 1 1 d D . . H58A H 0.2853 0.2738 -0.1823 0.047 Uiso 1 1 calc R . . H58B H 0.2989 0.2563 -0.2980 0.047 Uiso 1 1 calc R . . H58C H 0.2937 0.2047 -0.2135 0.047 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 0.0118(4) 0.0109(4) 0.0105(4) 0.0004(2) -0.0007(3) 0.0005(4) Co2 0.0115(4) 0.0106(4) 0.0105(4) -0.0007(3) -0.0004(2) 0.0004(4) Co3 0.0120(4) 0.0124(4) 0.0105(4) -0.0009(3) 0.0000(3) 0.0012(4) Co4 0.0129(4) 0.0135(4) 0.0102(4) -0.0004(2) -0.0002(2) 0.0012(4) O1 0.0185(16) 0.0121(15) 0.0203(16) 0.0005(14) -0.0014(12) 0.0050(12) O2 0.0114(14) 0.0122(15) 0.0206(16) -0.0016(13) -0.0018(11) -0.0007(12) O3 0.0135(15) 0.0142(16) 0.0228(17) -0.0003(14) 0.0027(12) 0.0042(12) O4 0.0129(15) 0.0151(15) 0.0183(15) -0.0001(13) -0.0008(11) -0.0008(12) O5 0.017(2) 0.047(3) 0.024(2) 0.0063(18) 0.0053(15) 0.0009(19) O6 0.022(2) 0.054(3) 0.025(2) 0.0134(19) 0.0090(16) -0.003(2) N1 0.017(2) 0.022(2) 0.016(2) -0.0031(16) -0.0018(15) 0.0005(16) N2 0.025(3) 0.037(3) 0.031(3) -0.016(2) -0.006(2) 0.0132(19) N3 0.020(2) 0.018(2) 0.0117(18) -0.0032(15) -0.0003(15) 0.0010(16) N4 0.019(2) 0.022(2) 0.024(2) 0.0034(17) -0.0037(17) 0.0028(16) N5 0.058(3) 0.020(2) 0.035(3) -0.002(2) -0.031(3) 0.011(2) N6 0.021(2) 0.0129(19) 0.022(2) -0.0017(16) -0.0032(18) 0.0022(16) N7 0.019(2) 0.019(2) 0.020(2) 0.0042(17) -0.0027(16) -0.0001(16) N8 0.016(2) 0.046(3) 0.021(3) 0.022(2) -0.0020(19) 0.005(2) N9 0.019(2) 0.016(2) 0.0165(19) 0.0040(16) 0.0088(16) -0.0013(17) N10 0.026(2) 0.021(2) 0.0118(18) 0.0023(16) 0.0005(17) 0.0024(16) N11 0.052(3) 0.014(2) 0.031(3) -0.009(2) 0.025(3) -0.009(2) N12 0.021(2) 0.021(2) 0.017(2) -0.0047(16) 0.0088(17) -0.0043(16) N13 0.022(2) 0.023(2) 0.017(2) -0.0002(16) 0.0047(17) 0.0027(17) N14 0.058(4) 0.021(3) 0.034(3) 0.010(2) 0.030(3) 0.012(2) N15 0.018(2) 0.022(2) 0.0133(18) -0.0038(15) 0.0055(16) -0.0001(15) N16 0.019(2) 0.014(2) 0.0150(19) 0.0033(16) 0.0031(15) -0.0045(16) N17 0.016(3) 0.042(3) 0.035(3) 0.0235(17) 0.004(2) 0.006(2) N18 0.013(2) 0.024(2) 0.020(2) 0.0038(17) 0.0000(16) 0.0061(16) N19 0.020(2) 0.016(2) 0.0151(19) 0.0005(15) -0.0033(16) 0.0035(15) N20 0.076(5) 0.019(3) 0.043(3) -0.005(3) -0.045(3) 0.002(2) N21 0.018(2) 0.0139(19) 0.019(2) -0.0033(16) -0.0115(17) 0.0034(16) N22 0.014(2) 0.025(2) 0.0132(19) -0.0046(17) 0.0029(15) 0.0012(16) N23 0.015(2) 0.056(3) 0.020(2) -0.0232(18) 0.009(2) -0.004(2) N24 0.016(2) 0.011(2) 0.024(2) -0.0058(16) 0.0009(16) 0.0037(16) N25 0.019(2) 0.009(2) 0.0072(16) -0.0002(7) -0.0004(8) 0.0015(18) N26 0.018(3) 0.015(3) 0.016(2) -0.0011(18) 0.0013(19) -0.007(2) N27 0.019(2) 0.009(2) 0.0072(16) -0.0002(7) -0.0004(8) 0.0015(18) N28 0.018(3) 0.011(3) 0.029(3) -0.001(2) -0.003(2) -0.003(2) N29 0.010(2) 0.016(2) 0.0137(18) -0.0003(7) -0.0031(7) 0.0019(17) N30 0.032(3) 0.020(3) 0.029(3) -0.002(2) -0.008(2) 0.004(2) N31 0.010(2) 0.016(2) 0.0137(18) -0.0003(7) -0.0031(7) 0.0019(17) N32 0.037(4) 0.033(4) 0.029(3) -0.002(2) 0.004(3) 0.019(3) C1 0.023(3) 0.010(2) 0.013(2) -0.0040(17) -0.0017(18) -0.0057(19) C2 0.016(3) 0.021(3) 0.019(2) -0.0022(18) 0.0007(18) 0.0065(19) C3 0.016(3) 0.016(2) 0.025(3) -0.0075(19) -0.005(2) 0.0027(18) C4 0.025(3) 0.015(2) 0.014(2) 0.0013(18) -0.0039(19) 0.0075(19) C5 0.009(2) 0.012(2) 0.017(2) 0.0049(17) 0.0007(16) -0.0015(16) C6 0.019(3) 0.024(3) 0.024(3) -0.009(2) -0.004(2) 0.013(2) C7 0.020(3) 0.010(2) 0.021(3) 0.0011(18) 0.006(2) -0.0006(18) C8 0.029(3) 0.019(2) 0.019(2) -0.0048(19) 0.002(2) 0.005(2) C9 0.024(3) 0.013(2) 0.022(2) -0.0017(18) 0.0111(19) -0.0045(18) C10 0.028(3) 0.017(2) 0.019(2) -0.0057(19) 0.011(2) 0.002(2) C11 0.009(3) 0.015(3) 0.019(2) 0.0086(19) 0.0024(17) -0.0003(18) C12 0.017(3) 0.019(3) 0.014(2) 0.0028(19) -0.0017(19) 0.0056(19) C13 0.024(3) 0.011(2) 0.021(2) -0.0032(19) -0.006(2) 0.0022(19) C14 0.027(3) 0.017(3) 0.030(3) 0.007(2) -0.003(2) 0.006(2) C15 0.007(2) 0.022(3) 0.021(2) -0.006(2) -0.0046(18) 0.0033(18) C16 0.016(3) 0.027(3) 0.023(3) 0.000(2) 0.010(2) 0.004(2) C17 0.017(3) 0.019(3) 0.013(2) -0.0018(19) 0.0001(19) 0.004(2) C18 0.030(3) 0.009(3) 0.024(3) -0.0036(19) 0.000(2) 0.000(2) C19 0.019(3) 0.016(3) 0.0111(18) 0.0001(15) -0.0020(15) -0.005(2) C20 0.019(3) 0.016(3) 0.0111(18) 0.0001(15) -0.0020(15) -0.005(2) C21 0.027(2) 0.009(2) 0.0246(18) 0.0048(14) -0.0028(15) -0.0043(14) C22 0.027(2) 0.009(2) 0.0246(18) 0.0048(14) -0.0028(15) -0.0043(14) C23 0.016(3) 0.033(4) 0.035(3) -0.005(2) 0.005(2) -0.006(3) C24 0.031(4) 0.014(3) 0.028(3) -0.004(2) 0.003(2) -0.008(2) C25 0.022(3) 0.006(2) 0.0136(18) 0.0004(14) -0.0018(15) 0.0017(16) C26 0.022(3) 0.006(2) 0.0136(18) 0.0004(14) -0.0018(15) 0.0017(16) C27 0.012(3) 0.026(3) 0.014(2) 0.001(2) 0.0004(19) 0.000(2) C28 0.020(3) 0.010(3) 0.018(3) 0.0038(18) -0.001(2) 0.0012(19) C29 0.015(3) 0.019(3) 0.008(2) 0.0012(18) 0.0054(17) -0.002(2) C30 0.017(3) 0.023(3) 0.012(2) -0.0008(18) 0.0047(19) -0.008(2) C31 0.018(2) 0.014(2) 0.034(2) -0.0037(15) -0.0030(16) -0.0012(14) C32 0.018(2) 0.014(2) 0.034(2) -0.0037(15) -0.0030(16) -0.0012(14) C33 0.016(3) 0.034(4) 0.036(3) 0.001(2) -0.003(2) -0.007(3) C34 0.015(3) 0.014(3) 0.033(3) 0.003(2) 0.004(2) -0.005(2) C35 0.017(3) 0.011(3) 0.012(3) -0.0011(17) 0.0009(18) 0.006(2) C36 0.020(3) 0.007(3) 0.011(3) -0.0013(17) 0.0026(19) -0.001(2) C37 0.010(2) 0.009(2) 0.0118(19) -0.0006(13) -0.0010(13) -0.0017(15) C38 0.010(2) 0.009(2) 0.0118(19) -0.0006(13) -0.0010(13) -0.0017(15) C39 0.014(3) 0.006(2) 0.013(2) 0.0000(17) 0.0029(17) -0.0011(19) C40 0.016(3) 0.014(3) 0.010(2) -0.0015(17) 0.0032(18) 0.001(2) C41 0.010(2) 0.025(3) 0.023(2) 0.005(2) 0.0022(18) 0.0007(18) C42 0.021(3) 0.023(3) 0.022(2) 0.002(2) 0.003(2) 0.0013(18) C43 0.017(3) 0.010(3) 0.040(3) 0.000(2) -0.006(2) 0.001(2) C44 0.012(3) 0.018(3) 0.034(3) -0.001(2) -0.003(2) -0.006(2) C45 0.005(2) 0.021(3) 0.011(2) -0.0014(18) -0.0003(17) -0.0003(18) C46 0.010(3) 0.022(3) 0.014(2) 0.001(2) 0.0001(19) -0.002(2) C47 0.008(3) 0.019(3) 0.015(3) -0.001(2) 0.0006(18) -0.005(2) C48 0.005(3) 0.023(3) 0.020(3) 0.008(2) 0.0002(18) 0.000(2) C49 0.017(2) 0.009(2) 0.0084(18) -0.0007(13) -0.0019(13) -0.0010(18) C50 0.017(2) 0.009(2) 0.0084(18) -0.0007(13) -0.0019(13) -0.0010(18) C51 0.019(3) 0.014(3) 0.021(2) -0.0022(19) -0.0036(19) -0.005(2) C52 0.018(3) 0.014(3) 0.026(2) -0.0009(19) 0.000(2) 0.000(2) C53 0.023(3) 0.019(3) 0.029(3) -0.005(2) 0.004(2) 0.0054(19) C54 0.020(3) 0.025(3) 0.016(2) -0.002(2) 0.0084(18) -0.0013(19) C55 0.011(2) 0.010(2) 0.014(2) 0.0022(14) -0.0024(14) -0.0038(15) C56 0.011(2) 0.010(2) 0.014(2) 0.0022(14) -0.0024(14) -0.0038(15) C57 0.026(4) 0.032(4) 0.029(4) -0.005(2) -0.006(2) -0.009(3) C58 0.032(4) 0.046(4) 0.016(3) -0.007(2) -0.013(2) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 2.087(4) . ? Co1 N1 2.106(4) . ? Co1 N7 2.122(4) . ? Co1 N10 2.129(4) . ? Co1 O1 2.130(3) . ? Co1 N25 2.145(4) . ? Co2 N16 2.092(4) . ? Co2 N13 2.095(4) . ? Co2 N19 2.100(4) . ? Co2 N22 2.105(4) . ? Co2 N27 2.155(4) . ? Co2 O2 2.181(3) . ? Co3 N15 2.100(4) . ? Co3 N21 2.116(4) 1_556 ? Co3 N9 2.119(4) 1_556 ? Co3 N3 2.126(4) . ? Co3 N29 2.126(4) . ? Co3 O3 2.188(3) . ? Co4 N12 2.104(4) 1_556 ? Co4 N18 2.105(4) . ? Co4 N31 2.118(4) . ? Co4 N6 2.120(4) . ? Co4 N24 2.133(4) 1_556 ? Co4 O4 2.144(3) . ? O5 C57 1.423(8) . ? O6 C58 1.404(8) . ? N1 C1 1.188(5) . ? N2 C1 1.286(6) . ? N2 C2 1.308(6) . ? N3 C2 1.144(5) . ? N4 C3 1.163(5) . ? N5 C4 1.292(6) . ? N5 C3 1.296(5) . ? N6 C4 1.158(5) . ? N7 C5 1.162(5) . ? N8 C5 1.299(6) . ? N8 C6 1.326(6) . ? N9 C6 1.124(6) . ? N9 Co3 2.119(4) 1_554 ? N10 C7 1.140(5) . ? N11 C8 1.319(6) . ? N11 C7 1.323(5) . ? N12 C8 1.124(5) . ? N12 Co4 2.104(4) 1_554 ? N13 C9 1.172(5) . ? N14 C9 1.291(6) . ? N14 C10 1.291(6) . ? N15 C10 1.161(5) . ? N16 C11 1.168(5) . ? N17 C12 1.305(6) . ? N17 C11 1.314(6) . ? N18 C12 1.160(5) . ? N19 C13 1.153(5) . ? N20 C13 1.312(6) . ? N20 C14 1.318(6) . ? N21 C14 1.135(5) . ? N21 Co3 2.116(4) 1_554 ? N22 C15 1.156(5) . ? N23 C16 1.293(6) . ? N23 C15 1.315(6) . ? N24 C16 1.139(6) . ? N24 Co4 2.133(4) 1_554 ? N25 C26 1.317(6) . ? N25 C17 1.359(6) . ? N26 C23 1.325(6) . ? N26 C22 1.349(6) . ? N27 C36 1.309(6) . ? N27 C27 1.331(6) . ? N28 C32 1.337(6) . ? N28 C33 1.340(6) . ? N29 C37 1.327(5) . ? N29 C46 1.374(6) . ? N30 C43 1.337(6) . ? N30 C42 1.341(6) . ? N31 C56 1.340(6) . ? N31 C47 1.379(6) . ? N32 C52 1.343(6) . ? N32 C53 1.350(6) . ? C17 C18 1.374(7) . ? C18 C19 1.394(7) . ? C19 C25 1.421(6) . ? C19 C20 1.485(6) . ? C20 C24 1.380(7) . ? C20 C21 1.384(6) . ? C21 C22 1.392(6) . ? C23 C24 1.406(6) . ? C25 C26 1.392(6) . ? C27 C28 1.389(7) . ? C28 C29 1.382(6) . ? C29 C35 1.410(6) . ? C29 C30 1.489(6) . ? C30 C34 1.388(6) . ? C30 C31 1.394(6) . ? C31 C32 1.375(6) . ? C33 C34 1.404(6) . ? C35 C36 1.388(6) . ? C37 C38 1.387(6) . ? C38 C39 1.394(6) . ? C39 C45 1.380(6) . ? C39 C40 1.485(5) . ? C40 C41 1.368(6) . ? C40 C44 1.421(6) . ? C41 C42 1.371(6) . ? C43 C44 1.370(6) . ? C45 C46 1.376(6) . ? C47 C48 1.369(6) . ? C48 C49 1.373(6) . ? C49 C55 1.410(6) . ? C49 C50 1.485(6) . ? C50 C54 1.398(6) . ? C50 C51 1.406(6) . ? C51 C52 1.366(6) . ? C53 C54 1.364(6) . ? C55 C56 1.376(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N1 90.34(15) . . ? N4 Co1 N7 178.07(18) . . ? N1 Co1 N7 91.57(17) . . ? N4 Co1 N10 89.39(15) . . ? N1 Co1 N10 179.19(18) . . ? N7 Co1 N10 88.70(16) . . ? N4 Co1 O1 95.34(14) . . ? N1 Co1 O1 91.60(15) . . ? N7 Co1 O1 84.42(14) . . ? N10 Co1 O1 89.19(14) . . ? N4 Co1 N25 93.92(17) . . ? N1 Co1 N25 88.60(17) . . ? N7 Co1 N25 86.33(17) . . ? N10 Co1 N25 90.65(16) . . ? O1 Co1 N25 170.74(14) . . ? N16 Co2 N13 89.91(16) . . ? N16 Co2 N19 177.88(17) . . ? N13 Co2 N19 89.97(14) . . ? N16 Co2 N22 91.40(16) . . ? N13 Co2 N22 177.45(18) . . ? N19 Co2 N22 88.79(15) . . ? N16 Co2 N27 85.37(17) . . ? N13 Co2 N27 93.61(17) . . ? N19 Co2 N27 92.53(16) . . ? N22 Co2 N27 88.68(17) . . ? N16 Co2 O2 85.81(14) . . ? N13 Co2 O2 87.80(14) . . ? N19 Co2 O2 96.30(13) . . ? N22 Co2 O2 90.11(14) . . ? N27 Co2 O2 171.06(15) . . ? N15 Co3 N21 89.36(15) . 1_556 ? N15 Co3 N9 178.09(18) . 1_556 ? N21 Co3 N9 90.58(16) 1_556 1_556 ? N15 Co3 N3 88.55(16) . . ? N21 Co3 N3 177.18(18) 1_556 . ? N9 Co3 N3 91.57(18) 1_556 . ? N15 Co3 N29 90.76(17) . . ? N21 Co3 N29 92.24(16) 1_556 . ? N9 Co3 N29 87.34(18) 1_556 . ? N3 Co3 N29 89.67(17) . . ? N15 Co3 O3 97.40(14) . . ? N21 Co3 O3 88.08(13) 1_556 . ? N9 Co3 O3 84.50(15) 1_556 . ? N3 Co3 O3 90.32(15) . . ? N29 Co3 O3 171.84(15) . . ? N12 Co4 N18 179.08(18) 1_556 . ? N12 Co4 N31 93.70(17) 1_556 . ? N18 Co4 N31 86.79(17) . . ? N12 Co4 N6 88.84(15) 1_556 . ? N18 Co4 N6 90.38(17) . . ? N31 Co4 N6 90.66(16) . . ? N12 Co4 N24 90.14(15) 1_556 1_556 ? N18 Co4 N24 90.65(18) . 1_556 ? N31 Co4 N24 88.60(17) . 1_556 ? N6 Co4 N24 178.70(18) . 1_556 ? N12 Co4 O4 95.18(14) 1_556 . ? N18 Co4 O4 84.32(14) . . ? N31 Co4 O4 171.11(14) . . ? N6 Co4 O4 89.01(13) . . ? N24 Co4 O4 91.89(15) 1_556 . ? C1 N1 Co1 169.9(5) . . ? C1 N2 C2 122.1(5) . . ? C2 N3 Co3 173.9(5) . . ? C3 N4 Co1 176.0(4) . . ? C4 N5 C3 123.1(5) . . ? C4 N6 Co4 172.0(4) . . ? C5 N7 Co1 169.3(4) . . ? C5 N8 C6 116.9(5) . . ? C6 N9 Co3 163.3(5) . 1_554 ? C7 N10 Co1 168.7(4) . . ? C8 N11 C7 120.0(5) . . ? C8 N12 Co4 176.5(4) . 1_554 ? C9 N13 Co2 173.2(4) . . ? C9 N14 C10 123.4(5) . . ? C10 N15 Co3 167.7(4) . . ? C11 N16 Co2 164.3(4) . . ? C12 N17 C11 116.6(5) . . ? C12 N18 Co4 168.3(4) . . ? C13 N19 Co2 171.5(4) . . ? C13 N20 C14 120.8(5) . . ? C14 N21 Co3 174.7(4) . 1_554 ? C15 N22 Co2 175.5(4) . . ? C16 N23 C15 119.0(5) . . ? C16 N24 Co4 173.4(5) . 1_554 ? C26 N25 C17 117.4(4) . . ? C26 N25 Co1 120.5(3) . . ? C17 N25 Co1 122.0(4) . . ? C23 N26 C22 117.3(4) . . ? C36 N27 C27 117.0(4) . . ? C36 N27 Co2 121.8(3) . . ? C27 N27 Co2 121.1(4) . . ? C32 N28 C33 118.0(4) . . ? C37 N29 C46 118.0(4) . . ? C37 N29 Co3 121.9(3) . . ? C46 N29 Co3 120.0(3) . . ? C43 N30 C42 116.2(5) . . ? C56 N31 C47 117.1(4) . . ? C56 N31 Co4 121.9(3) . . ? C47 N31 Co4 120.8(3) . . ? C52 N32 C53 115.7(5) . . ? N1 C1 N2 175.4(6) . . ? N3 C2 N2 173.1(6) . . ? N4 C3 N5 175.6(5) . . ? N6 C4 N5 173.4(6) . . ? N7 C5 N8 176.1(6) . . ? N9 C6 N8 173.2(7) . . ? N10 C7 N11 171.8(6) . . ? N12 C8 N11 172.3(6) . . ? N13 C9 N14 175.1(6) . . ? N15 C10 N14 174.0(6) . . ? N16 C11 N17 174.6(6) . . ? N18 C12 N17 175.2(6) . . ? N19 C13 N20 172.9(6) . . ? N21 C14 N20 171.8(6) . . ? N22 C15 N23 174.5(6) . . ? N24 C16 N23 172.4(6) . . ? N25 C17 C18 122.7(5) . . ? C17 C18 C19 120.7(5) . . ? C18 C19 C25 116.2(4) . . ? C18 C19 C20 121.7(5) . . ? C25 C19 C20 122.1(5) . . ? C24 C20 C21 117.7(5) . . ? C24 C20 C19 121.1(5) . . ? C21 C20 C19 121.3(5) . . ? C20 C21 C22 119.7(5) . . ? N26 C22 C21 122.8(5) . . ? N26 C23 C24 123.2(5) . . ? C20 C24 C23 119.3(5) . . ? C26 C25 C19 118.8(5) . . ? N25 C26 C25 124.2(5) . . ? N27 C27 C28 122.6(5) . . ? C29 C28 C27 120.8(5) . . ? C28 C29 C35 116.2(4) . . ? C28 C29 C30 121.0(5) . . ? C35 C29 C30 122.8(5) . . ? C34 C30 C31 117.8(5) . . ? C34 C30 C29 120.7(5) . . ? C31 C30 C29 121.5(5) . . ? C32 C31 C30 120.3(5) . . ? N28 C32 C31 122.4(5) . . ? N28 C33 C34 123.0(5) . . ? C30 C34 C33 118.4(5) . . ? C36 C35 C29 118.1(4) . . ? N27 C36 C35 125.3(5) . . ? N29 C37 C38 122.6(4) . . ? C37 C38 C39 120.0(4) . . ? C45 C39 C38 117.0(4) . . ? C45 C39 C40 121.6(4) . . ? C38 C39 C40 121.4(4) . . ? C41 C40 C44 115.8(4) . . ? C41 C40 C39 121.7(5) . . ? C44 C40 C39 122.6(5) . . ? C40 C41 C42 121.0(4) . . ? N30 C42 C41 123.6(5) . . ? N30 C43 C44 123.9(5) . . ? C43 C44 C40 119.5(5) . . ? C46 C45 C39 121.0(4) . . ? N29 C46 C45 121.4(5) . . ? C48 C47 N31 121.6(5) . . ? C47 C48 C49 121.1(5) . . ? C48 C49 C55 117.7(4) . . ? C48 C49 C50 121.3(4) . . ? C55 C49 C50 121.1(4) . . ? C54 C50 C51 115.2(4) . . ? C54 C50 C49 121.1(5) . . ? C51 C50 C49 123.7(5) . . ? C52 C51 C50 120.9(4) . . ? N32 C52 C51 123.5(5) . . ? N32 C53 C54 124.4(5) . . ? C53 C54 C50 120.2(5) . . ? C56 C55 C49 118.7(4) . . ? N31 C56 C55 123.8(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.523 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.069 #=END data_7 _database_code_CSD 172409 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Co(dca)2(4,4'-bipy).0.5H2O.0.5MeOH _chemical_formula_sum 'C14.50 H11 Co N8 O' _chemical_formula_weight 372.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 11.6750(4) _cell_length_b 19.4612(5) _cell_length_c 7.3249(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1664.29(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 15388 _cell_measurement_theta_min 3.45 _cell_measurement_theta_max 30.50 _exptl_crystal_description Prismatic _exptl_crystal_colour Orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.051 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.693 _exptl_absorpt_correction_T_max 0.859 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _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 15388 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 30.50 _reflns_number_total 2518 _reflns_number_gt 1714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett and Johnson, 1996)' _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^)+(0.0591P)^2^+0.2295P] 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 2518 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1089 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.0000 0.0000 0.0000 0.01822(12) Uani 1 2 d S . . C8 C -0.2500 0.2500 0.7631(10) 0.0563(18) Uiso 0.50 2 d SP . . O1 O -0.1480(14) 0.2604(8) 0.810(3) 0.073(4) Uiso 0.14 1 d P . . O2 O -0.1504(16) 0.2460(8) 0.703(3) 0.078(4) Uiso 0.13 1 d P . . O3 O -0.1977(15) 0.2482(10) 0.574(3) 0.093(6) Uiso 0.13 1 d P . . O4 O -0.199(2) 0.2469(15) 0.443(5) 0.108(9) Uiso 0.10 1 d P . . N1 N -0.09216(12) 0.04346(7) 0.21945(18) 0.0255(3) Uani 1 1 d . . . N2 N -0.1280(2) 0.10058(9) 0.51320(18) 0.0425(5) Uani 1 1 d . . . N3 N -0.11674(12) 0.04147(7) 0.80810(19) 0.0261(3) Uani 1 1 d . . . N4 N 0.09431(12) 0.09386(7) -0.01946(16) 0.0219(3) Uani 1 1 d . . . C1 C -0.10849(15) 0.06750(8) 0.3607(2) 0.0252(4) Uani 1 1 d . . . C2 C -0.12130(15) 0.06679(8) 0.6665(2) 0.0252(4) Uani 1 1 d . . . C3 C 0.20713(15) 0.09432(9) -0.0509(2) 0.0260(4) Uani 1 1 d . . . H3 H 0.2420(16) 0.0496(9) -0.069(3) 0.031 Uiso 1 1 d . . . C4 C 0.27102(16) 0.15427(8) -0.0587(3) 0.0270(4) Uani 1 1 d . . . H4 H 0.3484(18) 0.1508(8) -0.080(3) 0.032 Uiso 1 1 d . . . C5 C 0.21720(15) 0.21732(8) -0.0321(2) 0.0223(3) Uani 1 1 d . . . C6 C 0.09988(16) 0.21658(9) -0.0008(2) 0.0270(4) Uani 1 1 d . . . H6 H 0.058(2) 0.2587(11) 0.017(2) 0.032 Uiso 1 1 d . . . C7 C 0.04224(17) 0.15442(10) 0.0034(2) 0.0275(4) Uani 1 1 d . . . H7 H -0.034(2) 0.1531(12) 0.026(2) 0.033 Uiso 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 Co1 0.02326(18) 0.01706(19) 0.01435(17) 0.00050(10) -0.00016(12) -0.00917(10) N1 0.0325(8) 0.0254(7) 0.0187(7) 0.0000(6) 0.0024(6) -0.0070(6) N2 0.0819(14) 0.0261(9) 0.0196(8) -0.0013(6) -0.0005(7) 0.0116(8) N3 0.0300(8) 0.0280(7) 0.0205(7) -0.0004(6) -0.0039(6) -0.0044(6) N4 0.0263(7) 0.0192(7) 0.0201(7) -0.0005(5) 0.0003(5) -0.0085(5) C1 0.0336(9) 0.0203(8) 0.0216(8) 0.0019(6) -0.0038(7) -0.0032(6) C2 0.0311(9) 0.0220(8) 0.0224(8) -0.0046(7) -0.0018(7) 0.0000(7) C3 0.0298(9) 0.0206(8) 0.0276(8) -0.0042(7) 0.0061(7) -0.0088(7) C4 0.0278(9) 0.0226(8) 0.0307(9) -0.0037(7) 0.0072(7) -0.0094(7) C5 0.0301(9) 0.0190(8) 0.0177(7) 0.0007(6) -0.0005(6) -0.0096(7) C6 0.0281(9) 0.0183(8) 0.0345(10) 0.0013(6) -0.0013(7) -0.0070(7) C7 0.0248(8) 0.0234(9) 0.0343(10) 0.0026(7) -0.0011(7) -0.0080(7) _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 2.1112(14) . ? Co1 N1 2.1112(14) 5 ? Co1 N3 2.1177(14) 5_556 ? Co1 N3 2.1178(14) 1_554 ? Co1 N4 2.1376(13) . ? Co1 N4 2.1377(13) 5 ? C8 O2 1.246(18) 2_455 ? C8 O2 1.246(18) . ? C8 O1 1.256(15) . ? C8 O1 1.256(15) 2_455 ? C8 O4 1.45(3) 7_566 ? C8 O4 1.45(3) 8_556 ? C8 O3 1.52(2) . ? C8 O3 1.52(2) 2_455 ? O1 O2 0.83(2) . ? O1 O4 1.15(3) 7_566 ? O2 O3 1.10(2) . ? O3 O4 0.95(3) . ? O3 O3 1.22(3) 2_455 ? O3 O4 1.54(3) 2_455 ? O4 O1 1.15(3) 7_565 ? O4 O4 1.20(5) 2_455 ? O4 C8 1.45(3) 7_565 ? O4 O3 1.54(3) 2_455 ? N1 C1 1.151(2) . ? N2 C2 1.304(2) . ? N2 C1 1.309(2) . ? N3 C2 1.149(2) . ? N3 Co1 2.1177(14) 1_556 ? N4 C7 1.337(2) . ? N4 C3 1.337(2) . ? C3 C4 1.386(2) . ? C4 C5 1.392(2) . ? C5 C6 1.389(2) . ? C5 C5 1.485(3) 2 ? C6 C7 1.384(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.0 . 5 ? N1 Co1 N3 88.59(6) . 5_556 ? N1 Co1 N3 91.42(6) 5 5_556 ? N1 Co1 N3 91.42(6) . 1_554 ? N1 Co1 N3 88.58(6) 5 1_554 ? N3 Co1 N3 180.0 5_556 1_554 ? N1 Co1 N4 88.33(5) . . ? N1 Co1 N4 91.67(5) 5 . ? N3 Co1 N4 92.20(5) 5_556 . ? N3 Co1 N4 87.80(5) 1_554 . ? N1 Co1 N4 91.67(5) . 5 ? N1 Co1 N4 88.33(5) 5 5 ? N3 Co1 N4 87.80(5) 5_556 5 ? N3 Co1 N4 92.20(5) 1_554 5 ? N4 Co1 N4 180.0 . 5 ? O2 C8 O2 139(2) 2_455 . ? O2 C8 O1 166.3(13) 2_455 . ? O2 C8 O1 39.0(10) . . ? O2 C8 O1 39.0(10) 2_455 2_455 ? O2 C8 O1 166.3(13) . 2_455 ? O1 C8 O1 148.2(19) . 2_455 ? O2 C8 O4 134.7(19) 2_455 7_566 ? O2 C8 O4 86.7(14) . 7_566 ? O1 C8 O4 49.8(11) . 7_566 ? O1 C8 O4 98.4(19) 2_455 7_566 ? O2 C8 O4 86.7(14) 2_455 8_556 ? O2 C8 O4 134.7(19) . 8_556 ? O1 C8 O4 98.4(19) . 8_556 ? O1 C8 O4 49.8(11) 2_455 8_556 ? O4 C8 O4 49(2) 7_566 8_556 ? O2 C8 O3 93.1(17) 2_455 . ? O2 C8 O3 45.5(9) . . ? O1 C8 O3 82.7(10) . . ? O1 C8 O3 129.0(14) 2_455 . ? O4 C8 O3 132.0(13) 7_566 . ? O4 C8 O3 176.3(15) 8_556 . ? O2 C8 O3 45.5(9) 2_455 2_455 ? O2 C8 O3 93.1(17) . 2_455 ? O1 C8 O3 129.0(14) . 2_455 ? O1 C8 O3 82.7(10) 2_455 2_455 ? O4 C8 O3 176.3(15) 7_566 2_455 ? O4 C8 O3 132.0(13) 8_556 2_455 ? O3 C8 O3 47.6(16) . 2_455 ? O2 O1 O4 138(3) . 7_566 ? O2 O1 C8 69.9(16) . . ? O4 O1 C8 73.9(17) 7_566 . ? O1 O2 O3 145(3) . . ? O1 O2 C8 71.2(16) . . ? O3 O2 C8 80.4(17) . . ? O4 O3 O2 150(3) . . ? O4 O3 O3 89.2(19) . 2_455 ? O2 O3 O3 120.3(13) . 2_455 ? O4 O3 C8 155(2) . . ? O2 O3 C8 54.1(13) . . ? O3 O3 C8 66.2(8) 2_455 . ? O4 O3 O4 51(2) . 2_455 ? O2 O3 O4 159(2) . 2_455 ? O3 O3 O4 38.3(12) 2_455 2_455 ? C8 O3 O4 104.5(16) . 2_455 ? O3 O4 O1 147(3) . 7_565 ? O3 O4 O4 90.8(19) . 2_455 ? O1 O4 O4 121.7(15) 7_565 2_455 ? O3 O4 C8 156(3) . 7_565 ? O1 O4 C8 56.3(16) 7_565 7_565 ? O4 O4 C8 65.6(12) 2_455 7_565 ? O3 O4 O3 53(2) . 2_455 ? O1 O4 O3 159(2) 7_565 2_455 ? O4 O4 O3 38.3(12) 2_455 2_455 ? C8 O4 O3 103.9(18) 7_565 2_455 ? C1 N1 Co1 158.65(14) . . ? C2 N2 C1 118.44(17) . . ? C2 N3 Co1 142.38(14) . 1_556 ? C7 N4 C3 117.62(14) . . ? C7 N4 Co1 120.72(12) . . ? C3 N4 Co1 121.64(11) . . ? N1 C1 N2 174.42(18) . . ? N3 C2 N2 175.00(18) . . ? N4 C3 C4 122.89(16) . . ? C3 C4 C5 119.55(16) . . ? C6 C5 C4 117.33(14) . . ? C6 C5 C5 121.2(2) . 2 ? C4 C5 C5 121.5(2) . 2 ? C7 C6 C5 119.48(17) . . ? N4 C7 C6 123.13(17) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.520 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.097 #=END data_8 _database_code_CSD 172410 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Cu(dca)2(4,4'-bipy)(H2O) _chemical_formula_sum 'C14 H10 Cu N8 O' _chemical_formula_weight 369.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 7.3887(4) _cell_length_b 11.9610(6) _cell_length_c 18.7679(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1658.64(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11369 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 30.03 _exptl_crystal_description Prismatic _exptl_crystal_colour Blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 1.335 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.866 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method Phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11369 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 30.03 _reflns_number_total 4235 _reflns_number_gt 3130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett and Johnson, 1996)' _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^)+(0.0592P)^2^+0.2925P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.53(2) _refine_ls_number_reflns 4235 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.25939(5) 0.03927(3) 0.0000 0.02938(13) Uani 1 1 d . . . N1 N 0.0737(5) -0.0684(3) 0.03484(18) 0.0381(7) Uani 1 1 d . . . N2 N -0.2202(6) -0.1467(5) 0.0662(4) 0.094(2) Uani 1 1 d . . . N3 N -0.5049(5) -0.0458(3) 0.05002(19) 0.0379(7) Uani 1 1 d . . . N4 N 0.3799(5) 0.1687(3) -0.04583(18) 0.0381(7) Uani 1 1 d . . . N5 N 0.4449(6) 0.3659(3) -0.0660(2) 0.0669(12) Uani 1 1 d . . . N6 N 0.2517(6) 0.5038(5) -0.1262(3) 0.0685(14) Uani 1 1 d . . . N7 N 0.2180(4) 0.1325(3) 0.09025(17) 0.0320(7) Uani 1 1 d . . . N8 N 0.2211(4) 0.4517(2) 0.40798(17) 0.0304(7) Uani 1 1 d . . . C1 C -0.0679(5) -0.1004(3) 0.0483(2) 0.0394(9) Uani 1 1 d . . . C2 C -0.3689(6) -0.0882(3) 0.0559(2) 0.0389(9) Uani 1 1 d . . . C3 C 0.4014(5) 0.2610(3) -0.0590(2) 0.0408(9) Uani 1 1 d . . . C4 C 0.3374(7) 0.4349(4) -0.0997(3) 0.0534(11) Uani 1 1 d . . . C5 C 0.2370(4) 0.0830(3) 0.1538(2) 0.0323(8) Uani 1 1 d . . . H5 H 0.2550 0.0044 0.1553 0.039 Uiso 1 1 calc R . . C6 C 0.2314(4) 0.1418(3) 0.2180(2) 0.0314(8) Uani 1 1 d . . . H6 H 0.2478 0.1041 0.2621 0.038 Uiso 1 1 calc R . . C7 C 0.2011(5) 0.2576(3) 0.21635(19) 0.0288(7) Uani 1 1 d . . . C8 C 0.2033(5) 0.3248(3) 0.2835(2) 0.0303(8) Uani 1 1 d . . . C9 C 0.1772(5) 0.2763(3) 0.3492(2) 0.0342(8) Uani 1 1 d . . . H9 H 0.1520 0.1987 0.3527 0.041 Uiso 1 1 calc R . . C10 C 0.1880(6) 0.3416(3) 0.4104(2) 0.0336(8) Uani 1 1 d . . . H10 H 0.1714 0.3069 0.4554 0.040 Uiso 1 1 calc R . . C11 C 0.2448(5) 0.4993(4) 0.3450(2) 0.0403(10) Uani 1 1 d . . . H11 H 0.2672 0.5774 0.3428 0.048 Uiso 1 1 calc R . . C12 C 0.2377(5) 0.4384(4) 0.2819(2) 0.0382(10) Uani 1 1 d . . . H12 H 0.2567 0.4749 0.2376 0.046 Uiso 1 1 calc R . . C13 C 0.1751(5) 0.3071(3) 0.1502(2) 0.0329(8) Uani 1 1 d . . . H13 H 0.1521 0.3851 0.1470 0.039 Uiso 1 1 calc R . . C14 C 0.1825(5) 0.2433(3) 0.0892(2) 0.0322(8) Uani 1 1 d . . . H14 H 0.1617 0.2786 0.0446 0.039 Uiso 1 1 calc R . . O1 O 0.3854(5) -0.2093(3) 0.2390(2) 0.147(8) Uiso 0.26 1 d PR . . O2 O 0.2596(5) -0.2109(3) 0.2007(2) 0.158(12) Uiso 0.26 1 d PR . . O3 O 0.4571(5) -0.3070(3) 0.2539(2) 0.18(2) Uiso 0.14 1 d PR . . O4 O 0.4937(5) -0.2391(3) 0.2248(2) 0.16(2) Uiso 0.11 1 d PR . . O5 O 0.2874(5) -0.2837(3) 0.2319(2) 0.19(3) Uiso 0.11 1 d PR . . O6 O 0.4089(5) -0.3277(3) 0.2292(2) 0.17(2) Uiso 0.12 1 d PR . . 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 0.0435(2) 0.0251(2) 0.01958(18) -0.0057(2) 0.0010(2) -0.00126(15) N1 0.043(2) 0.0386(17) 0.0321(17) -0.0086(14) -0.0020(13) 0.0023(15) N2 0.039(3) 0.060(3) 0.183(7) 0.057(4) 0.005(3) 0.0001(19) N3 0.0399(19) 0.0431(19) 0.0308(17) -0.0030(14) 0.0016(13) 0.0001(15) N4 0.061(2) 0.0269(17) 0.0262(16) -0.0032(13) 0.0024(15) -0.0063(15) N5 0.078(3) 0.039(2) 0.084(3) 0.020(2) -0.023(2) -0.021(2) N6 0.091(4) 0.047(2) 0.068(4) 0.021(3) -0.003(2) -0.006(2) N7 0.0431(17) 0.0321(18) 0.0209(14) -0.0037(13) -0.0032(12) -0.0013(13) N8 0.0443(18) 0.0293(17) 0.0176(15) -0.0076(11) -0.0017(12) 0.0019(12) C1 0.036(2) 0.031(2) 0.051(3) 0.0021(18) -0.0027(18) 0.0026(16) C2 0.035(2) 0.035(2) 0.047(2) 0.0020(18) 0.0005(17) -0.0041(17) C3 0.049(2) 0.045(2) 0.028(2) 0.0010(17) -0.0010(16) -0.0006(18) C4 0.069(3) 0.041(2) 0.051(3) 0.014(2) -0.004(2) -0.008(2) C5 0.047(2) 0.023(2) 0.0263(18) -0.0045(15) 0.0026(15) 0.0011(14) C6 0.044(2) 0.028(2) 0.0220(17) -0.0045(15) 0.0010(14) 0.0020(14) C7 0.0369(18) 0.0282(18) 0.0212(17) -0.0032(14) 0.0011(13) 0.0013(14) C8 0.0333(18) 0.031(2) 0.0267(18) -0.0062(16) -0.0023(14) 0.0009(15) C9 0.048(2) 0.0290(19) 0.0255(18) -0.0063(15) 0.0008(15) 0.0008(16) C10 0.052(2) 0.0282(18) 0.0206(18) 0.0003(14) -0.0004(15) 0.0033(16) C11 0.070(3) 0.029(2) 0.0213(19) -0.0042(17) 0.0098(17) -0.0061(16) C12 0.064(3) 0.029(2) 0.0217(19) -0.0052(15) 0.0042(17) -0.0049(16) C13 0.043(2) 0.0258(18) 0.0299(19) -0.0035(15) -0.0044(16) 0.0077(16) C14 0.043(2) 0.0303(19) 0.0231(17) -0.0045(15) -0.0025(15) 0.0020(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 N4 1.983(3) . ? Cu1 N1 1.992(4) . ? Cu1 N8 2.025(3) 4_544 ? Cu1 N7 2.051(3) . ? Cu1 N3 2.225(4) 1_655 ? N1 C1 1.143(5) . ? N2 C1 1.299(6) . ? N2 C2 1.317(7) . ? N3 C2 1.130(5) . ? N3 Cu1 2.225(4) 1_455 ? N4 C3 1.143(5) . ? N5 C3 1.301(5) . ? N5 C4 1.309(6) . ? N6 C4 1.152(7) . ? N7 C5 1.339(5) . ? N7 C14 1.352(5) . ? N8 C11 1.324(6) . ? N8 C10 1.341(5) . ? N8 Cu1 2.025(3) 4 ? C5 C6 1.397(5) . ? C6 C7 1.403(5) . ? C7 C13 1.388(5) . ? C7 C8 1.494(5) . ? C8 C9 1.376(5) . ? C8 C12 1.382(6) . ? C9 C10 1.391(5) . ? C11 C12 1.391(6) . ? C13 C14 1.376(5) . ? O1 O4 0.9154 . ? O1 O5 1.1555 . ? O1 O2 1.1752 . ? O1 O3 1.3132 . ? O1 O6 1.4389 . ? O2 O5 1.0688 . ? O2 O4 1.8192 . ? O3 O6 0.6346 . ? O3 O4 1.0149 . ? O3 O5 1.3495 . ? O4 O6 1.2341 . ? O4 O5 1.6203 . ? O5 O6 1.0417 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N1 163.09(14) . . ? N4 Cu1 N8 90.10(13) . 4_544 ? N1 Cu1 N8 89.70(13) . 4_544 ? N4 Cu1 N7 90.03(13) . . ? N1 Cu1 N7 88.73(13) . . ? N8 Cu1 N7 175.05(13) 4_544 . ? N4 Cu1 N3 100.88(13) . 1_655 ? N1 Cu1 N3 96.01(13) . 1_655 ? N8 Cu1 N3 93.87(12) 4_544 1_655 ? N7 Cu1 N3 90.97(13) . 1_655 ? C1 N1 Cu1 156.9(3) . . ? C1 N2 C2 117.3(5) . . ? C2 N3 Cu1 160.4(3) . 1_455 ? C3 N4 Cu1 155.7(3) . . ? C3 N5 C4 120.4(4) . . ? C5 N7 C14 117.8(3) . . ? C5 N7 Cu1 118.7(3) . . ? C14 N7 Cu1 123.4(3) . . ? C11 N8 C10 118.4(3) . . ? C11 N8 Cu1 122.0(3) . 4 ? C10 N8 Cu1 119.5(3) . 4 ? N1 C1 N2 173.7(5) . . ? N3 C2 N2 173.6(5) . . ? N4 C3 N5 170.9(5) . . ? N6 C4 N5 173.4(6) . . ? N7 C5 C6 122.9(4) . . ? C5 C6 C7 118.9(4) . . ? C13 C7 C6 117.5(3) . . ? C13 C7 C8 121.7(3) . . ? C6 C7 C8 120.7(3) . . ? C9 C8 C12 117.3(3) . . ? C9 C8 C7 121.8(3) . . ? C12 C8 C7 120.8(4) . . ? C8 C9 C10 119.7(3) . . ? N8 C10 C9 122.3(3) . . ? N8 C11 C12 122.0(4) . . ? C8 C12 C11 120.2(4) . . ? C14 C13 C7 120.1(3) . . ? N7 C14 C13 122.6(3) . . ? O4 O1 O5 102.3 . . ? O4 O1 O2 120.4 . . ? O5 O1 O2 54.6 . . ? O4 O1 O3 50.4 . . ? O5 O1 O3 65.9 . . ? O2 O1 O3 115.7 . . ? O4 O1 O6 58.3 . . ? O5 O1 O6 45.7 . . ? O2 O1 O6 90.1 . . ? O3 O1 O6 26.2 . . ? O5 O2 O1 61.8 . . ? O5 O2 O4 62.0 . . ? O1 O2 O4 25.7 . . ? O6 O3 O4 94.0 . . ? O6 O3 O1 88.0 . . ? O4 O3 O1 44.0 . . ? O6 O3 O5 48.3 . . ? O4 O3 O5 85.3 . . ? O1 O3 O5 51.4 . . ? O1 O4 O3 85.6 . . ? O1 O4 O6 82.6 . . ? O3 O4 O6 30.9 . . ? O1 O4 O5 44.2 . . ? O3 O4 O5 56.1 . . ? O6 O4 O5 40.0 . . ? O1 O4 O2 33.8 . . ? O3 O4 O2 91.7 . . ? O6 O4 O2 72.1 . . ? O5 O4 O2 35.6 . . ? O6 O5 O2 123.4 . . ? O6 O5 O1 81.6 . . ? O2 O5 O1 63.6 . . ? O6 O5 O3 27.1 . . ? O2 O5 O3 120.9 . . ? O1 O5 O3 62.7 . . ? O6 O5 O4 49.6 . . ? O2 O5 O4 82.4 . . ? O1 O5 O4 33.5 . . ? O3 O5 O4 38.6 . . ? O3 O6 O5 104.6 . . ? O3 O6 O4 55.1 . . ? O5 O6 O4 90.4 . . ? O3 O6 O1 65.8 . . ? O5 O6 O1 52.6 . . ? O4 O6 O1 39.1 . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.395 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.074 #=END data_9 _database_code_CSD 172411 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Cu(dca)2(4,4'-bipy).MeOH _chemical_formula_sum 'C15 H12 Cu N8 O' _chemical_formula_weight 383.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.6253(2) _cell_length_b 12.5777(3) _cell_length_c 14.8959(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.421(1) _cell_angle_gamma 90.00 _cell_volume 1613.12(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23470 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 30.02 _exptl_crystal_description Prismatic _exptl_crystal_colour Blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.832 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method Phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23470 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 30.02 _reflns_number_total 4456 _reflns_number_gt 3741 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett and Johnson, 1996)' _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^)+(0.0426P)^2^+0.8821P] 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 4456 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.15156(2) 0.205528(16) 0.079734(13) 0.01872(8) Uani 1 1 d . . . O1 O 0.2951(2) 0.09502(14) -0.47094(12) 0.0503(4) Uani 1 1 d . . . H1 H 0.304(3) 0.073(2) -0.412(2) 0.060 Uiso 1 1 d . . . N1 N 0.03922(19) 0.30278(13) 0.15727(11) 0.0276(3) Uani 1 1 d . . . N2 N -0.0990(2) 0.45093(18) 0.22089(14) 0.0525(6) Uani 1 1 d . . . N3 N -0.0541(2) 0.55705(14) 0.35702(12) 0.0326(4) Uani 1 1 d . . . N4 N 0.27261(17) 0.13419(13) -0.01035(10) 0.0262(3) Uani 1 1 d . . . N5 N 0.3749(2) 0.01239(13) -0.12001(11) 0.0318(4) Uani 1 1 d . . . N6 N 0.3339(3) 0.02462(15) -0.28514(12) 0.0437(5) Uani 1 1 d . . . N7 N 0.33995(17) 0.21080(11) 0.16842(9) 0.0193(3) Uani 1 1 d . . . N8 N 0.97336(17) 0.27900(11) 0.48605(9) 0.0201(3) Uani 1 1 d . . . C1 C -0.0176(2) 0.37402(16) 0.19098(12) 0.0274(4) Uani 1 1 d . . . C2 C -0.0665(2) 0.50313(14) 0.29490(12) 0.0251(4) Uani 1 1 d . . . C3 C 0.3148(2) 0.07897(14) -0.06569(11) 0.0225(3) Uani 1 1 d . . . C4 C 0.3489(2) 0.02333(14) -0.20810(13) 0.0283(4) Uani 1 1 d . . . C5 C 0.3230(2) 0.20228(14) 0.25714(11) 0.0225(3) Uani 1 1 d . . . H5 H 0.2226 0.1875 0.2770 0.027 Uiso 1 1 calc R . . C6 C 0.4448(2) 0.21406(14) 0.32087(12) 0.0226(3) Uani 1 1 d . . . H6 H 0.4280 0.2070 0.3830 0.027 Uiso 1 1 calc R . . C7 C 0.5926(2) 0.23637(14) 0.29289(11) 0.0210(3) Uani 1 1 d . . . C8 C 0.7258(2) 0.25151(14) 0.35914(11) 0.0207(3) Uani 1 1 d . . . C9 C 0.7150(2) 0.31943(16) 0.43185(13) 0.0277(4) Uani 1 1 d . . . H9 H 0.6216 0.3576 0.4394 0.033 Uiso 1 1 calc R . . C10 C 0.8399(2) 0.33149(16) 0.49319(13) 0.0274(4) Uani 1 1 d . . . H10 H 0.8308 0.3788 0.5423 0.033 Uiso 1 1 calc R . . C11 C 0.9846(2) 0.21291(16) 0.41610(13) 0.0276(4) Uani 1 1 d . . . H11 H 1.0788 0.1748 0.4110 0.033 Uiso 1 1 calc R . . C12 C 0.8658(2) 0.19783(15) 0.35131(13) 0.0282(4) Uani 1 1 d . . . H12 H 0.8791 0.1515 0.3020 0.034 Uiso 1 1 calc R . . C13 C 0.6102(2) 0.24337(16) 0.20086(12) 0.0252(4) Uani 1 1 d . . . H13 H 0.7096 0.2570 0.1790 0.030 Uiso 1 1 calc R . . C14 C 0.4825(2) 0.23045(15) 0.14137(12) 0.0244(4) Uani 1 1 d . . . H14 H 0.4963 0.2357 0.0787 0.029 Uiso 1 1 calc R . . C15 C 0.2875(5) -0.0028(2) -0.51791(19) 0.0716(9) Uani 1 1 d . . . H15A H 0.3637 -0.0523 -0.4900 0.107 Uiso 1 1 calc R . . H15B H 0.3106 0.0091 -0.5808 0.107 Uiso 1 1 calc R . . H15C H 0.1831 -0.0329 -0.5155 0.107 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 Cu1 0.01496(13) 0.02613(12) 0.01448(11) -0.00192(7) -0.00413(7) 0.00096(7) O1 0.0702(12) 0.0459(10) 0.0334(8) 0.0022(7) -0.0090(8) 0.0045(8) N1 0.0218(8) 0.0376(9) 0.0228(7) -0.0078(6) -0.0047(6) 0.0033(6) N2 0.0471(12) 0.0624(13) 0.0447(11) -0.0300(10) -0.0241(9) 0.0287(10) N3 0.0306(9) 0.0337(9) 0.0327(9) -0.0104(7) -0.0056(7) 0.0061(7) N4 0.0205(7) 0.0369(8) 0.0208(7) -0.0033(6) -0.0038(6) 0.0029(6) N5 0.0387(9) 0.0318(8) 0.0248(8) -0.0040(6) 0.0014(7) 0.0083(7) N6 0.0662(13) 0.0347(10) 0.0294(9) -0.0054(7) -0.0027(8) 0.0083(9) N7 0.0166(7) 0.0245(7) 0.0162(6) -0.0015(5) -0.0043(5) -0.0003(5) N8 0.0166(7) 0.0269(7) 0.0162(6) 0.0000(5) -0.0039(5) -0.0010(5) C1 0.0233(9) 0.0348(10) 0.0231(8) -0.0059(7) -0.0072(7) 0.0011(7) C2 0.0210(9) 0.0263(9) 0.0277(9) 0.0001(7) -0.0021(7) 0.0039(7) C3 0.0188(8) 0.0272(8) 0.0208(8) 0.0020(6) -0.0034(6) -0.0016(6) C4 0.0331(10) 0.0227(8) 0.0289(9) -0.0056(7) 0.0003(7) 0.0012(7) C5 0.0194(9) 0.0297(9) 0.0180(8) 0.0003(6) -0.0015(6) -0.0010(6) C6 0.0222(9) 0.0285(9) 0.0167(7) -0.0004(6) -0.0035(6) 0.0011(6) C7 0.0193(8) 0.0237(8) 0.0193(8) -0.0026(6) -0.0056(6) 0.0016(6) C8 0.0193(9) 0.0247(8) 0.0174(7) 0.0008(6) -0.0040(6) -0.0006(6) C9 0.0205(9) 0.0352(10) 0.0264(9) -0.0092(7) -0.0060(7) 0.0073(7) C10 0.0217(9) 0.0342(9) 0.0254(9) -0.0085(7) -0.0063(7) 0.0047(7) C11 0.0191(9) 0.0392(10) 0.0239(9) -0.0063(7) -0.0035(7) 0.0066(7) C12 0.0223(9) 0.0380(10) 0.0236(9) -0.0105(7) -0.0047(7) 0.0047(7) C13 0.0185(9) 0.0358(10) 0.0210(8) -0.0010(7) -0.0021(6) -0.0026(7) C14 0.0204(9) 0.0348(9) 0.0175(8) 0.0004(7) -0.0016(6) -0.0022(7) C15 0.114(3) 0.0578(17) 0.0412(14) -0.0013(13) -0.0097(16) -0.0220(18) _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 N4 1.9654(15) . ? Cu1 N1 1.9755(16) . ? Cu1 N8 2.0229(14) 4_465 ? Cu1 N7 2.0332(14) . ? Cu1 N3 2.2750(16) 2_545 ? O1 C15 1.415(3) . ? N1 C1 1.151(2) . ? N2 C1 1.290(3) . ? N2 C2 1.299(2) . ? N3 C2 1.147(2) . ? N3 Cu1 2.2751(16) 2 ? N4 C3 1.153(2) . ? N5 C3 1.294(2) . ? N5 C4 1.325(2) . ? N6 C4 1.147(3) . ? N7 C14 1.340(2) . ? N7 C5 1.343(2) . ? N8 C10 1.336(2) . ? N8 C11 1.341(2) . ? N8 Cu1 2.0229(14) 4_666 ? C5 C6 1.381(2) . ? C6 C7 1.394(2) . ? C7 C13 1.391(2) . ? C7 C8 1.481(2) . ? C8 C9 1.387(2) . ? C8 C12 1.395(3) . ? C9 C10 1.379(2) . ? C11 C12 1.378(3) . ? C13 C14 1.382(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N1 168.78(7) . . ? N4 Cu1 N8 89.18(6) . 4_465 ? N1 Cu1 N8 87.98(6) . 4_465 ? N4 Cu1 N7 91.26(6) . . ? N1 Cu1 N7 90.04(6) . . ? N8 Cu1 N7 171.90(6) 4_465 . ? N4 Cu1 N3 97.60(7) . 2_545 ? N1 Cu1 N3 93.44(7) . 2_545 ? N8 Cu1 N3 94.62(6) 4_465 2_545 ? N7 Cu1 N3 93.34(6) . 2_545 ? C1 N1 Cu1 166.82(17) . . ? C1 N2 C2 125.29(18) . . ? C2 N3 Cu1 143.16(15) . 2 ? C3 N4 Cu1 165.03(15) . . ? C3 N5 C4 120.10(17) . . ? C14 N7 C5 117.84(15) . . ? C14 N7 Cu1 121.52(11) . . ? C5 N7 Cu1 120.47(12) . . ? C10 N8 C11 118.09(15) . . ? C10 N8 Cu1 121.33(12) . 4_666 ? C11 N8 Cu1 120.55(12) . 4_666 ? N1 C1 N2 171.5(2) . . ? N3 C2 N2 171.2(2) . . ? N4 C3 N5 172.67(19) . . ? N6 C4 N5 173.9(2) . . ? N7 C5 C6 123.01(16) . . ? C5 C6 C7 119.21(16) . . ? C13 C7 C6 117.59(15) . . ? C13 C7 C8 121.51(16) . . ? C6 C7 C8 120.90(15) . . ? C9 C8 C12 117.54(16) . . ? C9 C8 C7 120.93(16) . . ? C12 C8 C7 121.53(16) . . ? C10 C9 C8 119.92(17) . . ? N8 C10 C9 122.38(17) . . ? N8 C11 C12 122.95(17) . . ? C11 C12 C8 119.10(16) . . ? C14 C13 C7 119.66(16) . . ? N7 C14 C13 122.67(16) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.430 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.066 #=END data_10 _database_code_CSD 172412 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Cu(dca)2(4,4'-bipy).2H2O _chemical_formula_sum 'C14 H12 Cu N8 O2' _chemical_formula_weight 387.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.3713(5) _cell_length_b 13.0693(6) _cell_length_c 15.0030(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.033(3) _cell_angle_gamma 90.00 _cell_volume 1640.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14570 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 28.29 _exptl_crystal_description Prismatic _exptl_crystal_colour Blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 1.358 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.879 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _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 14570 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3955 _reflns_number_gt 2906 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett and Johnson, 1996)' _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^)+(0.0525P)^2^+0.9713P] 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 3955 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.16215(4) 0.20777(3) 0.09232(2) 0.02820(13) Uani 1 1 d . . . O1 O 0.3279(3) 0.10262(18) -0.45108(15) 0.0500(6) Uani 1 1 d . . . O2 O 0.3342(3) -0.0669(2) -0.56223(18) 0.0632(7) Uani 1 1 d . . . N1 N 0.0453(3) 0.30175(19) 0.16889(16) 0.0342(5) Uani 1 1 d . . . N2 N -0.1121(3) 0.4457(2) 0.22156(18) 0.0499(7) Uani 1 1 d . . . N3 N -0.0553(3) 0.5640(2) 0.34629(17) 0.0421(6) Uani 1 1 d . . . N4 N 0.2838(3) 0.1341(2) 0.00357(16) 0.0358(5) Uani 1 1 d . . . N5 N 0.3819(3) 0.0159(2) -0.10882(16) 0.0421(6) Uani 1 1 d . . . N6 N 0.3279(4) 0.0293(2) -0.27066(19) 0.0542(8) Uani 1 1 d . . . N7 N 0.3496(3) 0.20591(16) 0.18185(14) 0.0267(5) Uani 1 1 d . . . N8 N 0.9852(3) 0.27129(17) 0.49891(15) 0.0295(5) Uani 1 1 d . . . C1 C -0.0210(3) 0.3714(2) 0.19717(19) 0.0348(6) Uani 1 1 d . . . C2 C -0.0741(3) 0.5060(2) 0.2891(2) 0.0353(6) Uani 1 1 d . . . C3 C 0.3246(3) 0.0803(2) -0.05224(19) 0.0317(6) Uani 1 1 d . . . C4 C 0.3503(4) 0.0271(2) -0.1949(2) 0.0372(7) Uani 1 1 d . . . C5 C 0.3252(3) 0.2050(2) 0.27000(18) 0.0305(6) Uani 1 1 d . . . H5 H 0.2190 0.1978 0.2894 0.037 Uiso 1 1 calc R . . C6 C 0.4481(3) 0.2142(2) 0.33362(19) 0.0315(6) Uani 1 1 d . . . H6 H 0.4258 0.2137 0.3953 0.038 Uiso 1 1 calc R . . C7 C 0.6047(3) 0.2243(2) 0.30646(18) 0.0298(6) Uani 1 1 d . . . C8 C 0.7373(3) 0.2405(2) 0.37191(18) 0.0303(6) Uani 1 1 d . . . C9 C 0.7359(4) 0.3214(2) 0.4312(2) 0.0416(7) Uani 1 1 d . . . H9 H 0.6489 0.3681 0.4297 0.050 Uiso 1 1 calc R . . C10 C 0.8602(3) 0.3345(2) 0.4924(2) 0.0404(7) Uani 1 1 d . . . H10 H 0.8570 0.3913 0.5319 0.049 Uiso 1 1 calc R . . C11 C 0.9883(3) 0.1921(2) 0.4419(2) 0.0384(7) Uani 1 1 d . . . H11 H 1.0761 0.1462 0.4460 0.046 Uiso 1 1 calc R . . C12 C 0.8694(3) 0.1747(2) 0.3775(2) 0.0387(7) Uani 1 1 d . . . H12 H 0.8770 0.1187 0.3375 0.046 Uiso 1 1 calc R . . C13 C 0.6297(3) 0.2219(2) 0.21501(19) 0.0321(6) Uani 1 1 d . . . H13 H 0.7351 0.2262 0.1938 0.039 Uiso 1 1 calc R . . C14 C 0.5004(3) 0.2132(2) 0.15537(18) 0.0303(6) Uani 1 1 d . . . H14 H 0.5193 0.2124 0.0933 0.036 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 Cu1 0.0280(2) 0.0342(2) 0.02197(18) -0.00191(14) -0.00611(12) 0.00203(13) O1 0.0536(13) 0.0563(15) 0.0395(13) 0.0014(11) -0.0055(10) 0.0036(11) O2 0.0542(15) 0.084(2) 0.0509(15) -0.0152(14) -0.0063(11) -0.0032(13) N1 0.0309(12) 0.0410(14) 0.0301(13) -0.0062(11) -0.0074(10) 0.0051(10) N2 0.0453(15) 0.0555(17) 0.0475(16) -0.0231(13) -0.0184(12) 0.0179(13) N3 0.0457(15) 0.0416(15) 0.0384(15) -0.0092(12) -0.0070(11) 0.0080(12) N4 0.0335(12) 0.0452(14) 0.0283(13) -0.0026(11) -0.0057(9) 0.0049(11) N5 0.0551(16) 0.0403(15) 0.0306(14) -0.0053(11) -0.0029(11) 0.0104(12) N6 0.086(2) 0.0420(16) 0.0336(16) -0.0068(12) -0.0049(14) 0.0115(15) N7 0.0295(12) 0.0285(11) 0.0218(11) 0.0004(9) -0.0049(8) 0.0006(9) N8 0.0288(12) 0.0365(13) 0.0227(11) 0.0007(9) -0.0050(9) -0.0024(9) C1 0.0315(15) 0.0437(17) 0.0285(15) -0.0019(13) -0.0079(11) -0.0046(13) C2 0.0334(15) 0.0356(16) 0.0363(16) -0.0023(13) -0.0075(12) 0.0068(12) C3 0.0301(14) 0.0362(16) 0.0282(15) 0.0026(13) -0.0070(11) -0.0008(12) C4 0.0460(17) 0.0306(15) 0.0347(17) -0.0048(12) -0.0002(13) 0.0035(12) C5 0.0292(14) 0.0367(15) 0.0253(14) 0.0001(11) -0.0032(10) -0.0017(11) C6 0.0312(14) 0.0386(16) 0.0244(13) -0.0003(12) -0.0049(11) -0.0004(11) C7 0.0335(15) 0.0285(14) 0.0269(14) -0.0009(11) -0.0072(11) -0.0002(11) C8 0.0295(14) 0.0364(15) 0.0247(14) 0.0018(11) -0.0045(11) -0.0020(11) C9 0.0365(16) 0.0421(17) 0.0451(19) -0.0112(14) -0.0144(13) 0.0104(13) C10 0.0398(17) 0.0409(17) 0.0394(17) -0.0127(14) -0.0142(13) 0.0065(13) C11 0.0356(16) 0.0425(17) 0.0362(17) -0.0055(13) -0.0109(12) 0.0100(12) C12 0.0368(16) 0.0419(17) 0.0367(16) -0.0130(13) -0.0095(12) 0.0074(13) C13 0.0296(14) 0.0395(16) 0.0269(14) -0.0005(12) -0.0032(11) -0.0014(11) C14 0.0317(14) 0.0343(15) 0.0247(13) -0.0004(11) -0.0026(11) 0.0000(11) _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 N4 1.958(2) . ? Cu1 N1 1.966(2) . ? Cu1 N8 2.021(2) 4_465 ? Cu1 N7 2.029(2) . ? Cu1 N3 2.289(3) 2_545 ? N1 C1 1.155(4) . ? N2 C1 1.296(4) . ? N2 C2 1.314(4) . ? N3 C2 1.151(4) . ? N3 Cu1 2.289(3) 2 ? N4 C3 1.155(4) . ? N5 C3 1.299(4) . ? N5 C4 1.317(4) . ? N6 C4 1.146(4) . ? N7 C14 1.341(4) . ? N7 C5 1.345(3) . ? N8 C10 1.335(4) . ? N8 C11 1.343(4) . ? N8 Cu1 2.021(2) 4_666 ? C5 C6 1.383(4) . ? C6 C7 1.393(4) . ? C7 C13 1.396(4) . ? C7 C8 1.470(4) . ? C8 C9 1.383(4) . ? C8 C12 1.401(4) . ? C9 C10 1.373(4) . ? C11 C12 1.381(4) . ? C13 C14 1.384(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 N4 Cu1 N1 170.48(11) . . ? N4 Cu1 N8 88.90(9) . 4_465 ? N1 Cu1 N8 87.31(9) . 4_465 ? N4 Cu1 N7 92.05(9) . . ? N1 Cu1 N7 90.56(9) . . ? N8 Cu1 N7 172.32(9) 4_465 . ? N4 Cu1 N3 95.15(10) . 2_545 ? N1 Cu1 N3 93.92(10) . 2_545 ? N8 Cu1 N3 95.91(9) 4_465 2_545 ? N7 Cu1 N3 91.59(9) . 2_545 ? C1 N1 Cu1 164.3(2) . . ? C1 N2 C2 122.6(3) . . ? C2 N3 Cu1 142.7(2) . 2 ? C3 N4 Cu1 165.3(2) . . ? C3 N5 C4 120.2(3) . . ? C14 N7 C5 118.0(2) . . ? C14 N7 Cu1 121.16(18) . . ? C5 N7 Cu1 120.68(18) . . ? C10 N8 C11 117.6(2) . . ? C10 N8 Cu1 121.36(19) . 4_666 ? C11 N8 Cu1 121.07(18) . 4_666 ? N1 C1 N2 172.0(3) . . ? N3 C2 N2 172.9(3) . . ? N4 C3 N5 173.9(3) . . ? N6 C4 N5 174.6(3) . . ? N7 C5 C6 122.9(3) . . ? C5 C6 C7 119.4(3) . . ? C6 C7 C13 117.4(2) . . ? C6 C7 C8 120.9(2) . . ? C13 C7 C8 121.6(2) . . ? C9 C8 C12 117.1(3) . . ? C9 C8 C7 121.1(3) . . ? C12 C8 C7 121.8(3) . . ? C10 C9 C8 120.2(3) . . ? N8 C10 C9 123.0(3) . . ? N8 C11 C12 122.9(3) . . ? C11 C12 C8 119.2(3) . . ? C14 C13 C7 119.8(3) . . ? N7 C14 C13 122.5(3) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.646 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.077 #=END data_11 _database_code_CSD 172413 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Fe(dca)2(H2O)2(4,4'-bipy)2 _chemical_formula_sum 'C24 H20 Fe N10 O2' _chemical_formula_weight 536.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Fe' 'Fe' 0.3463 0.8444 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 8.1365(1) _cell_length_b 8.6926(1) _cell_length_c 9.7297(2) _cell_angle_alpha 102.531(1) _cell_angle_beta 107.798(1) _cell_angle_gamma 97.420(1) _cell_volume 625.31(2) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 10573 _cell_measurement_theta_min 3.74 _cell_measurement_theta_max 28.28 _exptl_crystal_description Prismatic _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.058 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 276 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _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 10573 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3031 _reflns_number_gt 2743 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett and Johnson, 1996)' _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^)+(0.0229P)^2^+0.4004P] 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 3031 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Fe1 Fe 0.0000 0.0000 0.0000 0.01559(9) Uani 1 2 d S . . O1 O 0.02851(16) 0.19169(13) -0.09292(12) 0.0222(2) Uani 1 1 d . . . H1 H -0.061(3) 0.223(3) -0.142(3) 0.045(6) Uiso 1 1 d . . . H2 H 0.116(3) 0.219(3) -0.119(3) 0.052(7) Uiso 1 1 d . . . N1 N -0.28023(16) -0.03536(15) -0.10634(14) 0.0228(3) Uani 1 1 d . . . N2 N -0.56981(19) 0.0095(2) -0.24231(18) 0.0396(4) Uani 1 1 d . . . N3 N -0.6930(2) 0.2510(2) -0.1954(2) 0.0418(4) Uani 1 1 d . . . N4 N -0.02369(16) 0.17398(14) 0.19520(13) 0.0185(2) Uani 1 1 d . . . N5 N -0.23988(18) 0.30979(16) -0.24970(16) 0.0290(3) Uani 1 1 d . . . C1 C -0.41422(19) -0.00530(17) -0.16369(16) 0.0218(3) Uani 1 1 d . . . C2 C -0.6278(2) 0.1411(2) -0.21071(19) 0.0300(4) Uani 1 1 d . . . C3 C -0.1128(2) 0.29124(17) 0.17417(16) 0.0214(3) Uani 1 1 d . . . H3 H -0.1835 0.2856 0.0747 0.026 Uiso 1 1 calc R . . C4 C -0.1079(2) 0.41995(17) 0.28863(16) 0.0209(3) Uani 1 1 d . . . H4 H -0.1725 0.5004 0.2668 0.025 Uiso 1 1 calc R . . C5 C -0.00719(19) 0.43070(16) 0.43637(15) 0.0175(3) Uani 1 1 d . . . C6 C 0.0798(2) 0.30515(18) 0.45902(16) 0.0223(3) Uani 1 1 d . . . H6 H 0.1464 0.3043 0.5578 0.027 Uiso 1 1 calc R . . C7 C 0.0688(2) 0.18207(17) 0.33754(16) 0.0212(3) Uani 1 1 d . . . H7 H 0.1302 0.0987 0.3560 0.025 Uiso 1 1 calc R . . C8 C -0.3095(3) 0.2410(2) -0.3963(2) 0.0408(5) Uani 1 1 d . . . H8 H -0.2881 0.1380 -0.4340 0.049 Uiso 1 1 calc R . . C9 C -0.4115(3) 0.3108(2) -0.4973(2) 0.0412(5) Uani 1 1 d . . . H9 H -0.4569 0.2565 -0.6013 0.049 Uiso 1 1 calc R . . C10 C -0.44744(19) 0.45975(17) -0.44683(17) 0.0226(3) Uani 1 1 d . . . C11 C -0.3777(2) 0.53063(19) -0.29347(18) 0.0286(3) Uani 1 1 d . . . H11 H -0.3997 0.6321 -0.2523 0.034 Uiso 1 1 calc R . . C12 C -0.2756(2) 0.4523(2) -0.20057(19) 0.0320(4) Uani 1 1 d . . . H12 H -0.2284 0.5034 -0.0959 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02012(15) 0.01474(15) 0.01152(14) 0.00119(10) 0.00404(11) 0.00990(11) O1 0.0242(6) 0.0242(5) 0.0243(5) 0.0120(4) 0.0098(5) 0.0136(4) N1 0.0225(6) 0.0204(6) 0.0215(6) 0.0003(5) 0.0036(5) 0.0092(5) N2 0.0224(7) 0.0454(9) 0.0363(8) -0.0052(7) -0.0027(6) 0.0159(6) N3 0.0362(8) 0.0561(10) 0.0581(10) 0.0378(9) 0.0272(8) 0.0305(8) N4 0.0241(6) 0.0168(6) 0.0149(6) 0.0013(4) 0.0069(5) 0.0099(5) N5 0.0255(7) 0.0249(7) 0.0338(7) 0.0135(6) 0.0013(6) 0.0085(5) C1 0.0223(7) 0.0199(7) 0.0197(7) -0.0013(5) 0.0063(6) 0.0062(6) C2 0.0214(7) 0.0470(10) 0.0292(8) 0.0195(7) 0.0093(7) 0.0160(7) C3 0.0278(7) 0.0212(7) 0.0142(6) 0.0015(5) 0.0046(6) 0.0135(6) C4 0.0274(7) 0.0202(7) 0.0163(7) 0.0032(5) 0.0067(6) 0.0142(6) C5 0.0235(7) 0.0165(7) 0.0139(6) 0.0013(5) 0.0084(6) 0.0088(5) C6 0.0329(8) 0.0216(7) 0.0135(6) 0.0032(5) 0.0068(6) 0.0154(6) C7 0.0321(8) 0.0180(7) 0.0159(6) 0.0038(5) 0.0080(6) 0.0152(6) C8 0.0500(11) 0.0274(9) 0.0384(10) 0.0070(7) 0.0008(9) 0.0239(8) C9 0.0557(12) 0.0265(9) 0.0285(9) 0.0006(7) -0.0048(8) 0.0231(8) C10 0.0219(7) 0.0171(7) 0.0265(7) 0.0068(6) 0.0031(6) 0.0070(6) C11 0.0383(9) 0.0199(7) 0.0264(8) 0.0068(6) 0.0068(7) 0.0124(7) C12 0.0386(9) 0.0264(8) 0.0258(8) 0.0085(6) 0.0019(7) 0.0092(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 2.0807(11) 2 ? Fe1 O1 2.0808(11) . ? Fe1 N1 2.1453(12) 2 ? Fe1 N1 2.1453(12) . ? Fe1 N4 2.2325(11) 2 ? Fe1 N4 2.2325(11) . ? N1 C1 1.1547(19) . ? N2 C1 1.303(2) . ? N2 C2 1.305(2) . ? N3 C2 1.155(2) . ? N4 C7 1.3402(18) . ? N4 C3 1.3405(18) . ? N5 C8 1.327(2) . ? N5 C12 1.330(2) . ? C3 C4 1.3835(19) . ? C4 C5 1.3957(19) . ? C5 C6 1.3961(19) . ? C5 C5 1.492(2) 2_566 ? C6 C7 1.3827(19) . ? C8 C9 1.383(2) . ? C9 C10 1.383(2) . ? C10 C11 1.386(2) . ? C10 C10 1.490(3) 2_464 ? C11 C12 1.387(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O1 180.0 2 . ? O1 Fe1 N1 88.06(5) 2 2 ? O1 Fe1 N1 91.94(5) . 2 ? O1 Fe1 N1 91.94(5) 2 . ? O1 Fe1 N1 88.06(5) . . ? N1 Fe1 N1 180.0 2 . ? O1 Fe1 N4 87.82(4) 2 2 ? O1 Fe1 N4 92.18(4) . 2 ? N1 Fe1 N4 87.89(4) 2 2 ? N1 Fe1 N4 92.11(4) . 2 ? O1 Fe1 N4 92.18(4) 2 . ? O1 Fe1 N4 87.82(4) . . ? N1 Fe1 N4 92.11(4) 2 . ? N1 Fe1 N4 87.89(4) . . ? N4 Fe1 N4 180.00(4) 2 . ? C1 N1 Fe1 158.47(12) . . ? C1 N2 C2 121.73(15) . . ? C7 N4 C3 116.41(12) . . ? C7 N4 Fe1 122.50(9) . . ? C3 N4 Fe1 120.42(9) . . ? C8 N5 C12 116.53(14) . . ? N1 C1 N2 171.99(16) . . ? N3 C2 N2 173.32(19) . . ? N4 C3 C4 123.95(13) . . ? C3 C4 C5 119.52(13) . . ? C4 C5 C6 116.56(12) . . ? C4 C5 C5 121.79(15) . 2_566 ? C6 C5 C5 121.65(15) . 2_566 ? C7 C6 C5 119.89(13) . . ? N4 C7 C6 123.59(13) . . ? N5 C8 C9 123.65(16) . . ? C10 C9 C8 119.98(16) . . ? C9 C10 C11 116.53(14) . . ? C9 C10 C10 121.27(18) . 2_464 ? C11 C10 C10 122.19(17) . 2_464 ? C10 C11 C12 119.55(15) . . ? N5 C12 C11 123.73(16) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.278 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.051 #=END OF CIF