# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1821 data_FebipyMndca _audit_creation_method SHELXL-97 _chemical_name_systematic ; Iron(II) tris(2,2'-bipyridine) Bis(manganese(II) tris(dicyanamide)) ; _chemical_name_common Fe(bipy)3[Mn(dca)3]2 _chemical_melting_point ? _chemical_formula_moiety Fe(bipy)3[Mn(dca)3]2 _chemical_formula_sum 'C42 H24 Fe Mn2 N24' _chemical_formula_weight 1030.58 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' 'Mn' 'Mn' 0.3368 0.7283 '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 Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 28.7821(7) _cell_length_b 12.5280(3) _cell_length_c 23.7374(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8559.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour 'dark red ' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4160 _exptl_absorpt_coefficient_mu 0.981 _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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28565 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 28.31 _reflns_number_total 5287 _reflns_number_gt 4323 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0256P)^2^+10.9750P] 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(16) _refine_ls_number_reflns 5287 _refine_ls_number_parameters 313 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 0.2500 0.2500 0.99960(2) 0.01246(11) Uani 1 2 d S . . Mn1 Mn 0.2500 -0.2500 0.83350(2) 0.02034(14) Uani 1 2 d S . . Mn2 Mn 0.2500 -0.2500 1.150887(19) 0.01825(15) Uani 1 2 d S . . N1 N 0.20407(9) -0.3178(2) 0.90032(10) 0.0311(6) Uani 1 1 d . . . N2 N 0.17897(8) -0.38795(19) 0.99182(10) 0.0293(5) Uani 1 1 d . . . N3 N 0.20821(8) -0.32412(19) 1.08327(10) 0.0266(6) Uani 1 1 d . . . N4 N 0.20640(8) -0.1024(2) 0.83372(11) 0.0318(6) Uani 1 1 d . . . N5 N 0.16941(9) 0.0401(3) 0.77932(13) 0.0543(9) Uani 1 1 d . . . N6 N 0.20765(8) 0.1658(2) 0.71627(9) 0.0256(6) Uani 1 1 d . . . N7 N 0.29165(9) -0.1694(2) 0.76783(10) 0.0304(6) Uani 1 1 d . . . N8 N 0.33298(8) -0.0346(2) 0.71219(10) 0.0330(6) Uani 1 1 d . . . N9 N 0.29801(9) 0.1142(2) 0.66034(11) 0.0363(7) Uani 1 1 d . . . N10 N 0.21071(7) 0.12224(16) 1.00497(9) 0.0154(5) Uani 1 1 d . . . N11 N 0.29157(7) 0.20082(17) 1.06024(8) 0.0142(5) Uani 1 1 d . . . N12 N 0.28740(7) 0.19399(17) 0.93699(9) 0.0160(5) Uani 1 1 d . . . C1 C 0.19327(9) -0.3474(2) 0.94437(11) 0.0216(6) Uani 1 1 d . . . C2 C 0.19588(9) -0.3506(2) 1.03908(11) 0.0195(6) Uani 1 1 d . . . C3 C 0.19127(10) -0.0340(2) 0.80729(12) 0.0288(7) Uani 1 1 d . . . C4 C 0.19176(9) 0.1051(2) 0.74673(13) 0.0264(6) Uani 1 1 d . . . C5 C 0.30829(9) -0.1039(2) 0.74063(12) 0.0234(6) Uani 1 1 d . . . C6 C 0.31241(10) 0.0432(2) 0.68554(11) 0.0252(6) Uani 1 1 d . . . C7 C 0.18037(9) 0.1223(2) 1.04922(10) 0.0150(5) Uani 1 1 d . . . C8 C 0.15366(9) 0.0340(2) 1.06244(10) 0.0198(6) Uani 1 1 d . . . H8 H 0.1322 0.0364 1.0928 0.024 Uiso 1 1 calc R . . C9 C 0.15869(9) -0.0580(2) 1.03063(11) 0.0216(6) Uani 1 1 d . . . H9 H 0.1418 -0.1206 1.0402 0.026 Uiso 1 1 calc R . . C10 C 0.18831(9) -0.0582(2) 0.98502(11) 0.0229(6) Uani 1 1 d . . . H10 H 0.1915 -0.1200 0.9621 0.027 Uiso 1 1 calc R . . C11 C 0.21341(9) 0.0336(2) 0.97322(10) 0.0188(5) Uani 1 1 d . . . H11 H 0.2334 0.0338 0.9414 0.023 Uiso 1 1 calc R . . C12 C 0.32037(8) 0.27689(18) 1.08145(10) 0.0150(5) Uani 1 1 d . . . C13 C 0.34730(9) 0.2596(2) 1.12884(10) 0.0212(6) Uani 1 1 d . . . H13 H 0.3667 0.3146 1.1432 0.025 Uiso 1 1 calc R . . C14 C 0.34567(9) 0.1608(2) 1.15516(10) 0.0245(6) Uani 1 1 d . . . H14 H 0.3637 0.1476 1.1880 0.029 Uiso 1 1 calc R . . C15 C 0.31754(9) 0.0821(2) 1.13307(11) 0.0232(6) Uani 1 1 d . . . H15 H 0.3164 0.0135 1.1500 0.028 Uiso 1 1 calc R . . C16 C 0.29104(9) 0.1048(2) 1.08586(10) 0.0188(5) Uani 1 1 d . . . H16 H 0.2717 0.0503 1.0709 0.023 Uiso 1 1 calc R . . C17 C 0.27135(8) 0.2170(2) 0.88465(10) 0.0188(5) Uani 1 1 d . . . C18 C 0.29292(9) 0.1785(2) 0.83666(11) 0.0240(6) Uani 1 1 d . . . H18 H 0.2808 0.1949 0.8005 0.029 Uiso 1 1 calc R . . C19 C 0.33191(10) 0.1166(2) 0.84168(11) 0.0266(6) Uani 1 1 d . . . H19 H 0.3468 0.0893 0.8090 0.032 Uiso 1 1 calc R . . C20 C 0.34934(9) 0.0941(2) 0.89453(11) 0.0235(6) Uani 1 1 d . . . H20 H 0.3766 0.0520 0.8987 0.028 Uiso 1 1 calc R . . C21 C 0.32637(9) 0.1341(2) 0.94145(11) 0.0193(6) Uani 1 1 d . . . H21 H 0.3384 0.1190 0.9779 0.023 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 0.0130(2) 0.0135(2) 0.0109(3) 0.000 0.000 0.0001(2) Mn1 0.0244(3) 0.0208(3) 0.0158(3) 0.000 0.000 -0.0010(3) Mn2 0.0241(3) 0.0162(3) 0.0145(3) 0.000 0.000 0.0007(2) N1 0.0445(15) 0.0270(15) 0.0219(13) -0.0011(10) 0.0034(12) -0.0079(12) N2 0.0362(13) 0.0345(14) 0.0172(11) 0.0010(11) -0.0003(12) -0.0143(11) N3 0.0345(14) 0.0253(14) 0.0199(12) 0.0002(10) -0.0006(11) -0.0083(11) N4 0.0300(13) 0.0289(14) 0.0365(14) 0.0034(12) 0.0104(12) 0.0048(11) N5 0.0257(14) 0.071(2) 0.066(2) 0.0455(18) 0.0136(15) 0.0078(15) N6 0.0284(13) 0.0309(15) 0.0176(12) 0.0011(10) 0.0005(11) -0.0018(11) N7 0.0277(13) 0.0350(15) 0.0285(13) 0.0065(11) 0.0030(11) 0.0024(11) N8 0.0261(13) 0.0322(15) 0.0406(14) 0.0119(12) 0.0068(12) 0.0065(11) N9 0.0434(16) 0.0306(16) 0.0350(15) 0.0090(11) 0.0137(12) 0.0170(12) N10 0.0152(10) 0.0156(11) 0.0153(11) 0.0004(8) -0.0040(9) 0.0004(8) N11 0.0140(10) 0.0162(11) 0.0123(10) -0.0021(8) 0.0015(8) 0.0004(9) N12 0.0148(10) 0.0155(12) 0.0177(11) 0.0010(8) 0.0005(9) -0.0010(9) C1 0.0222(14) 0.0189(15) 0.0237(15) -0.0045(11) 0.0012(12) -0.0030(11) C2 0.0176(13) 0.0154(14) 0.0255(15) 0.0033(11) 0.0075(11) 0.0000(11) C3 0.0211(14) 0.0341(18) 0.0313(15) 0.0038(13) 0.0122(13) -0.0026(13) C4 0.0224(13) 0.0353(16) 0.0216(13) 0.0016(14) 0.0017(14) 0.0027(12) C5 0.0208(13) 0.0279(15) 0.0215(13) 0.0008(13) 0.0021(13) 0.0089(12) C6 0.0288(15) 0.0247(16) 0.0221(14) -0.0015(12) 0.0062(13) 0.0085(13) C7 0.0123(12) 0.0167(14) 0.0160(12) 0.0005(9) -0.0028(10) 0.0001(10) C8 0.0176(13) 0.0235(14) 0.0184(13) 0.0029(10) -0.0035(11) -0.0029(11) C9 0.0204(13) 0.0170(15) 0.0274(14) 0.0026(11) -0.0083(12) -0.0042(11) C10 0.0257(13) 0.0164(14) 0.0267(15) -0.0039(11) -0.0100(12) 0.0024(11) C11 0.0173(13) 0.0221(14) 0.0172(12) -0.0031(10) -0.0057(10) 0.0022(11) C12 0.0155(11) 0.0171(12) 0.0125(11) -0.0006(9) 0.0030(10) -0.0002(10) C13 0.0188(13) 0.0269(15) 0.0179(12) -0.0047(11) -0.0011(11) -0.0030(11) C14 0.0273(14) 0.0313(17) 0.0148(13) 0.0042(10) -0.0047(11) 0.0001(12) C15 0.0287(15) 0.0196(14) 0.0212(14) 0.0080(11) -0.0052(12) 0.0023(12) C16 0.0194(12) 0.0187(14) 0.0184(13) -0.0002(10) -0.0006(11) -0.0011(11) C17 0.0203(13) 0.0193(13) 0.0167(12) -0.0017(10) -0.0002(11) -0.0018(10) C18 0.0246(14) 0.0312(16) 0.0162(13) -0.0009(11) 0.0019(11) 0.0017(12) C19 0.0281(14) 0.0305(17) 0.0212(14) -0.0047(11) 0.0044(12) 0.0014(13) C20 0.0169(12) 0.0282(16) 0.0254(13) -0.0024(12) 0.0032(12) 0.0030(11) C21 0.0174(13) 0.0213(15) 0.0192(13) -0.0026(10) -0.0013(11) 0.0001(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 Fe1 N10 1.964(2) . ? Fe1 N10 1.964(2) 14 ? Fe1 N12 1.965(2) . ? Fe1 N12 1.965(2) 14 ? Fe1 N11 1.970(2) 14 ? Fe1 N11 1.971(2) . ? Mn1 N7 2.210(2) 14_545 ? Mn1 N7 2.210(3) . ? Mn1 N1 2.233(2) . ? Mn1 N1 2.233(3) 14_545 ? Mn1 N4 2.234(2) . ? Mn1 N4 2.234(2) 14_545 ? Mn2 N9 2.203(3) 10 ? Mn2 N9 2.203(3) 5_545 ? Mn2 N3 2.210(2) . ? Mn2 N3 2.210(2) 14_545 ? Mn2 N6 2.238(2) 5_545 ? Mn2 N6 2.238(2) 10 ? N1 C1 1.152(3) . ? N2 C1 1.302(4) . ? N2 C2 1.309(4) . ? N3 C2 1.156(3) . ? N4 C3 1.149(4) . ? N5 C4 1.294(4) . ? N5 C3 1.303(4) . ? N6 C4 1.145(4) . ? N6 Mn2 2.238(2) 5_554 ? N7 C5 1.149(3) . ? N8 C6 1.305(4) . ? N8 C5 1.309(4) . ? N9 C6 1.149(4) . ? N9 Mn2 2.203(3) 5_554 ? N10 C11 1.345(3) . ? N10 C7 1.366(3) . ? N11 C16 1.348(3) . ? N11 C12 1.360(3) . ? N12 C21 1.353(3) . ? N12 C17 1.357(3) . ? C7 C8 1.383(3) . ? C7 C12 1.477(3) 14 ? C8 C9 1.385(4) . ? C9 C10 1.378(4) . ? C10 C11 1.386(4) . ? C12 C13 1.383(3) . ? C12 C7 1.477(3) 14 ? C13 C14 1.387(4) . ? C14 C15 1.379(4) . ? C15 C16 1.385(4) . ? C17 C18 1.384(3) . ? C17 C17 1.481(5) 14 ? C18 C19 1.370(4) . ? C19 C20 1.380(4) . ? C20 C21 1.389(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 N10 Fe1 N10 172.56(12) . 14 ? N10 Fe1 N12 94.21(8) . . ? N10 Fe1 N12 91.41(8) 14 . ? N10 Fe1 N12 91.42(8) . 14 ? N10 Fe1 N12 94.21(8) 14 14 ? N12 Fe1 N12 81.69(13) . 14 ? N10 Fe1 N11 81.83(9) . 14 ? N10 Fe1 N11 92.71(8) 14 14 ? N12 Fe1 N11 175.50(9) . 14 ? N12 Fe1 N11 96.22(8) 14 14 ? N10 Fe1 N11 92.72(8) . . ? N10 Fe1 N11 81.82(9) 14 . ? N12 Fe1 N11 96.22(8) . . ? N12 Fe1 N11 175.50(9) 14 . ? N11 Fe1 N11 86.14(12) 14 . ? N7 Mn1 N7 90.31(13) 14_545 . ? N7 Mn1 N1 90.35(8) 14_545 . ? N7 Mn1 N1 174.77(10) . . ? N7 Mn1 N1 174.77(9) 14_545 14_545 ? N7 Mn1 N1 90.35(8) . 14_545 ? N1 Mn1 N1 89.47(13) . 14_545 ? N7 Mn1 N4 94.30(9) 14_545 . ? N7 Mn1 N4 85.89(9) . . ? N1 Mn1 N4 88.88(9) . . ? N1 Mn1 N4 90.92(10) 14_545 . ? N7 Mn1 N4 85.90(9) 14_545 14_545 ? N7 Mn1 N4 94.30(9) . 14_545 ? N1 Mn1 N4 90.92(10) . 14_545 ? N1 Mn1 N4 88.88(9) 14_545 14_545 ? N4 Mn1 N4 179.72(14) . 14_545 ? N9 Mn2 N9 168.30(13) 10 5_545 ? N9 Mn2 N3 93.28(9) 10 . ? N9 Mn2 N3 95.21(10) 5_545 . ? N9 Mn2 N3 95.21(10) 10 14_545 ? N9 Mn2 N3 93.27(9) 5_545 14_545 ? N3 Mn2 N3 86.86(12) . 14_545 ? N9 Mn2 N6 87.22(10) 10 5_545 ? N9 Mn2 N6 84.67(9) 5_545 5_545 ? N3 Mn2 N6 90.54(8) . 5_545 ? N3 Mn2 N6 176.53(9) 14_545 5_545 ? N9 Mn2 N6 84.67(9) 10 10 ? N9 Mn2 N6 87.22(10) 5_545 10 ? N3 Mn2 N6 176.53(9) . 10 ? N3 Mn2 N6 90.54(8) 14_545 10 ? N6 Mn2 N6 92.15(12) 5_545 10 ? C1 N1 Mn1 158.0(2) . . ? C1 N2 C2 119.0(2) . . ? C2 N3 Mn2 161.2(2) . . ? C3 N4 Mn1 146.1(2) . . ? C4 N5 C3 120.8(2) . . ? C4 N6 Mn2 165.7(2) . 5_554 ? C5 N7 Mn1 161.5(2) . . ? C6 N8 C5 120.0(2) . . ? C6 N9 Mn2 151.3(2) . 5_554 ? C11 N10 C7 117.9(2) . . ? C11 N10 Fe1 127.13(18) . . ? C7 N10 Fe1 114.70(16) . . ? C16 N11 C12 117.7(2) . . ? C16 N11 Fe1 126.99(17) . . ? C12 N11 Fe1 114.93(16) . . ? C21 N12 C17 118.1(2) . . ? C21 N12 Fe1 126.36(18) . . ? C17 N12 Fe1 115.49(16) . . ? N1 C1 N2 174.7(3) . . ? N3 C2 N2 173.8(3) . . ? N4 C3 N5 173.4(3) . . ? N6 C4 N5 173.7(3) . . ? N7 C5 N8 171.7(3) . . ? N9 C6 N8 174.1(3) . . ? N10 C7 C8 122.0(2) . . ? N10 C7 C12 114.0(2) . 14 ? C8 C7 C12 124.0(2) . 14 ? C7 C8 C9 118.9(2) . . ? C10 C9 C8 119.7(2) . . ? C9 C10 C11 118.7(2) . . ? N10 C11 C10 122.8(2) . . ? N11 C12 C13 122.2(2) . . ? N11 C12 C7 113.5(2) . 14 ? C13 C12 C7 124.3(2) . 14 ? C12 C13 C14 119.2(2) . . ? C15 C14 C13 119.1(2) . . ? C14 C15 C16 119.0(2) . . ? N11 C16 C15 122.8(2) . . ? N12 C17 C18 121.8(2) . . ? N12 C17 C17 113.66(14) . 14 ? C18 C17 C17 124.53(15) . 14 ? C19 C18 C17 119.6(2) . . ? C18 C19 C20 119.5(3) . . ? C19 C20 C21 118.8(2) . . ? N12 C21 C20 122.1(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.366 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.068 _publ_contact_author ; Prof. K.S. Murray Department of Chemistry PO Box 23 Monash University 3800 AUSTRALIA ; _publ_contact_author_phone ' +61 3 9905 4512 ' _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_email 'Keith.S.Murray@sci.monash.edu.au ' loop_ _publ_author_name _publ_author_address 'Batten, Stuart R.' ; Department of Chemistry PO Box 23 Monash University 3800 Australia ; 'Jensen, Paul' ; Department of Chemistry PO Box 23 Monash University 3800 Australia ; 'Moubaraki, Boujemaa' ; Department of Chemistry PO Box 23 Monash University 3800 Australia ; 'Murray, Keith S.' ; Department of Chemistry PO Box 23 Monash University 3800 Australia ; _publ_section_title ; Anionic metal dicyanamide networks with paramagnetic countercations ; #=END data_FebipyFedca _audit_creation_method SHELXL-97 _chemical_name_systematic ; Iron(II) tris(2,2'-bipyridine) Bis(iron(II) tris(dicyanamide)) ; _chemical_name_common Fe(bipy)3[Fe(dca)3]2 _chemical_melting_point ? _chemical_formula_moiety Fe(bipy)3[Fe(dca)3]2 _chemical_formula_sum 'C42 H24 Fe3 N24' _chemical_formula_weight 1032.40 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 Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 28.8799(6) _cell_length_b 12.4011(3) _cell_length_c 23.5140(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8421.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description acicular _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4176 _exptl_absorpt_coefficient_mu 1.087 _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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28083 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 28.25 _reflns_number_total 4983 _reflns_number_gt 4407 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0281P)^2^+6.9241P] 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 0.010(12) _refine_ls_number_reflns 4983 _refine_ls_number_parameters 313 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0608 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.2500 0.2500 1.000010(16) 0.01213(9) Uani 1 2 d S . . Fe2 Fe 0.2500 -0.2500 0.83314(2) 0.01964(11) Uani 1 2 d S . . Fe3 Fe 0.2500 -0.2500 1.150652(14) 0.01741(12) Uani 1 2 d S . . N1 N 0.20676(7) -0.31819(16) 0.89977(8) 0.0289(5) Uani 1 1 d . . . N2 N 0.17846(6) -0.38326(15) 0.99201(8) 0.0272(4) Uani 1 1 d . . . N3 N 0.20909(7) -0.32063(15) 1.08392(8) 0.0239(4) Uani 1 1 d . . . N4 N 0.20754(7) -0.10534(15) 0.83159(9) 0.0288(4) Uani 1 1 d . . . N5 N 0.16998(7) 0.0406(2) 0.77827(11) 0.0465(6) Uani 1 1 d . . . N6 N 0.20803(7) 0.16955(16) 0.71531(8) 0.0235(4) Uani 1 1 d . . . N7 N 0.29063(7) -0.17169(16) 0.76896(8) 0.0275(4) Uani 1 1 d . . . N8 N 0.33058(7) -0.03756(17) 0.70977(9) 0.0315(5) Uani 1 1 d . . . N9 N 0.29425(7) 0.11345(17) 0.65892(8) 0.0306(5) Uani 1 1 d . . . N10 N 0.21061(6) 0.12139(13) 1.00537(7) 0.0140(4) Uani 1 1 d . . . N11 N 0.29152(6) 0.20003(14) 1.06104(7) 0.0142(4) Uani 1 1 d . . . N12 N 0.28739(6) 0.19323(13) 0.93704(7) 0.0152(4) Uani 1 1 d . . . C1 C 0.19447(7) -0.34595(17) 0.94400(9) 0.0212(5) Uani 1 1 d . . . C2 C 0.19612(7) -0.34673(17) 1.03936(9) 0.0183(4) Uani 1 1 d . . . C3 C 0.19223(8) -0.0345(2) 0.80589(10) 0.0258(5) Uani 1 1 d . . . C4 C 0.19235(7) 0.10766(17) 0.74563(10) 0.0241(5) Uani 1 1 d . . . C5 C 0.30676(7) -0.10645(17) 0.73999(10) 0.0217(4) Uani 1 1 d . . . C6 C 0.30932(8) 0.04134(19) 0.68395(9) 0.0239(5) Uani 1 1 d . . . C7 C 0.17984(7) 0.12241(16) 1.04902(8) 0.0158(4) Uani 1 1 d . . . C8 C 0.15235(7) 0.03340(17) 1.06199(8) 0.0199(4) Uani 1 1 d . . . H8 H 0.1305 0.0365 1.0921 0.024 Uiso 1 1 calc R . . C9 C 0.15754(8) -0.06005(17) 1.02994(9) 0.0216(4) Uani 1 1 d . . . H9 H 0.1404 -0.1230 1.0392 0.026 Uiso 1 1 calc R . . C10 C 0.18778(7) -0.06035(16) 0.98458(8) 0.0211(4) Uani 1 1 d . . . H10 H 0.1909 -0.1226 0.9614 0.025 Uiso 1 1 calc R . . C11 C 0.21362(8) 0.03167(16) 0.97327(8) 0.0184(4) Uani 1 1 d . . . H11 H 0.2342 0.0313 0.9417 0.022 Uiso 1 1 calc R . . C12 C 0.32115(7) 0.27603(15) 1.08145(8) 0.0160(4) Uani 1 1 d . . . C13 C 0.34882(7) 0.25702(17) 1.12856(8) 0.0205(4) Uani 1 1 d . . . H13 H 0.3687 0.3119 1.1425 0.025 Uiso 1 1 calc R . . C14 C 0.34721(8) 0.15743(19) 1.15515(8) 0.0245(5) Uani 1 1 d . . . H14 H 0.3659 0.1432 1.1876 0.029 Uiso 1 1 calc R . . C15 C 0.31793(8) 0.07892(17) 1.13370(9) 0.0233(5) Uani 1 1 d . . . H15 H 0.3165 0.0096 1.1508 0.028 Uiso 1 1 calc R . . C16 C 0.29082(7) 0.10319(16) 1.08703(8) 0.0195(4) Uani 1 1 d . . . H16 H 0.2707 0.0491 1.0726 0.023 Uiso 1 1 calc R . . C17 C 0.27129(7) 0.21653(16) 0.88415(8) 0.0172(4) Uani 1 1 d . . . C18 C 0.29274(8) 0.17743(18) 0.83548(9) 0.0229(5) Uani 1 1 d . . . H18 H 0.2804 0.1936 0.7990 0.028 Uiso 1 1 calc R . . C19 C 0.33190(8) 0.11524(18) 0.84049(9) 0.0249(5) Uani 1 1 d . . . H19 H 0.3469 0.0879 0.8076 0.030 Uiso 1 1 calc R . . C20 C 0.34931(7) 0.09289(18) 0.89422(9) 0.0233(5) Uani 1 1 d . . . H20 H 0.3765 0.0506 0.8987 0.028 Uiso 1 1 calc R . . C21 C 0.32623(7) 0.13342(17) 0.94122(8) 0.0192(4) Uani 1 1 d . . . H21 H 0.3383 0.1184 0.9780 0.023 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 0.01442(19) 0.01193(18) 0.0100(2) 0.000 0.000 0.00007(16) Fe2 0.0256(2) 0.0182(2) 0.0151(3) 0.000 0.000 -0.00151(19) Fe3 0.0243(3) 0.0143(2) 0.0136(3) 0.000 0.000 0.00088(17) N1 0.0428(13) 0.0260(11) 0.0178(11) -0.0004(8) 0.0046(8) -0.0072(9) N2 0.0324(11) 0.0332(10) 0.0159(9) 0.0008(8) 0.0001(8) -0.0132(8) N3 0.0329(11) 0.0214(10) 0.0174(10) -0.0002(7) 0.0014(8) -0.0066(8) N4 0.0283(10) 0.0246(10) 0.0334(11) 0.0030(9) 0.0089(8) 0.0023(8) N5 0.0243(12) 0.0578(16) 0.0575(15) 0.0349(13) 0.0102(10) 0.0056(11) N6 0.0259(11) 0.0276(11) 0.0169(10) 0.0017(8) 0.0003(7) -0.0027(8) N7 0.0246(11) 0.0304(11) 0.0275(11) 0.0067(8) 0.0034(8) 0.0035(9) N8 0.0272(11) 0.0288(11) 0.0384(12) 0.0136(9) 0.0069(9) 0.0086(9) N9 0.0369(13) 0.0273(12) 0.0276(11) 0.0061(8) 0.0082(9) 0.0100(9) N10 0.0159(8) 0.0139(8) 0.0122(9) 0.0003(6) -0.0038(6) 0.0007(7) N11 0.0162(9) 0.0152(9) 0.0112(9) -0.0018(6) 0.0013(6) -0.0006(7) N12 0.0156(9) 0.0121(9) 0.0181(9) 0.0002(6) 0.0000(7) -0.0004(7) C1 0.0248(12) 0.0164(11) 0.0226(13) -0.0041(8) -0.0009(9) -0.0033(9) C2 0.0193(11) 0.0143(11) 0.0213(12) 0.0022(8) 0.0045(8) -0.0013(9) C3 0.0234(12) 0.0277(13) 0.0264(12) 0.0004(9) 0.0076(9) -0.0027(10) C4 0.0223(11) 0.0304(12) 0.0197(11) -0.0001(10) 0.0004(9) 0.0025(9) C5 0.0209(11) 0.0237(11) 0.0207(11) 0.0024(9) 0.0028(9) 0.0074(9) C6 0.0274(12) 0.0248(12) 0.0195(11) -0.0014(9) 0.0066(9) 0.0037(10) C7 0.0161(11) 0.0158(10) 0.0156(10) 0.0011(7) -0.0037(7) -0.0010(8) C8 0.0172(11) 0.0236(11) 0.0188(11) 0.0029(7) -0.0035(7) -0.0024(9) C9 0.0213(11) 0.0151(11) 0.0283(12) 0.0010(8) -0.0075(8) -0.0043(9) C10 0.0262(11) 0.0146(10) 0.0226(12) -0.0044(8) -0.0075(8) 0.0037(8) C11 0.0189(11) 0.0184(10) 0.0177(10) -0.0044(7) -0.0047(8) 0.0032(9) C12 0.0170(10) 0.0171(10) 0.0139(9) -0.0012(7) 0.0030(7) 0.0009(8) C13 0.0186(11) 0.0239(11) 0.0191(11) -0.0030(8) -0.0024(7) -0.0042(9) C14 0.0278(12) 0.0286(13) 0.0173(11) 0.0047(8) -0.0061(8) -0.0002(10) C15 0.0305(13) 0.0204(11) 0.0190(11) 0.0060(8) -0.0059(9) 0.0008(10) C16 0.0224(11) 0.0165(10) 0.0195(11) 0.0007(8) -0.0021(8) -0.0002(9) C17 0.0199(11) 0.0169(10) 0.0150(11) 0.0007(7) -0.0008(8) -0.0023(8) C18 0.0248(11) 0.0297(12) 0.0143(11) -0.0010(8) 0.0011(8) 0.0007(10) C19 0.0274(12) 0.0295(13) 0.0179(12) -0.0048(8) 0.0045(8) 0.0011(10) C20 0.0195(11) 0.0258(12) 0.0245(11) -0.0014(9) 0.0017(8) 0.0042(9) C21 0.0171(11) 0.0215(11) 0.0190(10) -0.0007(8) -0.0007(8) 0.0004(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N10 1.9630(17) 14 ? Fe1 N10 1.9631(16) . ? Fe1 N12 1.9632(18) 14 ? Fe1 N12 1.9633(18) . ? Fe1 N11 1.9700(17) . ? Fe1 N11 1.9701(17) 14 ? Fe2 N7 2.144(2) 14_545 ? Fe2 N7 2.144(2) . ? Fe2 N4 2.1732(19) . ? Fe2 N4 2.1732(19) 14_545 ? Fe2 N1 2.1745(19) . ? Fe2 N1 2.1746(19) 14_545 ? Fe3 N9 2.130(2) 5_545 ? Fe3 N9 2.130(2) 10 ? Fe3 N3 2.151(2) 14_545 ? Fe3 N3 2.1507(19) . ? Fe3 N6 2.1854(19) 5_545 ? Fe3 N6 2.1855(19) 10 ? N1 C1 1.152(3) . ? N2 C1 1.305(3) . ? N2 C2 1.306(3) . ? N3 C2 1.159(3) . ? N4 C3 1.154(3) . ? N5 C4 1.303(3) . ? N5 C3 1.305(3) . ? N6 C4 1.141(3) . ? N6 Fe3 2.1853(19) 5_554 ? N7 C5 1.156(3) . ? N8 C6 1.305(3) . ? N8 C5 1.307(3) . ? N9 C6 1.156(3) . ? N9 Fe3 2.130(2) 5_554 ? N10 C11 1.347(2) . ? N10 C7 1.358(3) . ? N11 C16 1.348(3) . ? N11 C12 1.360(3) . ? N12 C21 1.348(3) . ? N12 C17 1.359(3) . ? C7 C8 1.393(3) . ? C7 C12 1.473(3) 14 ? C8 C9 1.390(3) . ? C9 C10 1.378(3) . ? C10 C11 1.389(3) . ? C12 C13 1.386(3) . ? C12 C7 1.473(3) 14 ? C13 C14 1.385(3) . ? C14 C15 1.385(3) . ? C15 C16 1.381(3) . ? C17 C18 1.389(3) . ? C17 C17 1.484(4) 14 ? C18 C19 1.374(3) . ? C19 C20 1.388(3) . ? C20 C21 1.385(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N10 Fe1 N10 172.63(9) 14 . ? N10 Fe1 N12 94.34(7) 14 14 ? N10 Fe1 N12 91.21(7) . 14 ? N10 Fe1 N12 91.21(7) 14 . ? N10 Fe1 N12 94.35(7) . . ? N12 Fe1 N12 82.08(10) 14 . ? N10 Fe1 N11 81.73(7) 14 . ? N10 Fe1 N11 92.88(7) . . ? N12 Fe1 N11 175.54(7) 14 . ? N12 Fe1 N11 95.84(6) . . ? N10 Fe1 N11 92.88(7) 14 14 ? N10 Fe1 N11 81.72(7) . 14 ? N12 Fe1 N11 95.84(6) 14 14 ? N12 Fe1 N11 175.54(7) . 14 ? N11 Fe1 N11 86.49(10) . 14 ? N7 Fe2 N7 90.54(11) 14_545 . ? N7 Fe2 N4 93.05(8) 14_545 . ? N7 Fe2 N4 85.59(7) . . ? N7 Fe2 N4 85.60(7) 14_545 14_545 ? N7 Fe2 N4 93.05(8) . 14_545 ? N4 Fe2 N4 178.08(11) . 14_545 ? N7 Fe2 N1 90.95(7) 14_545 . ? N7 Fe2 N1 175.91(8) . . ? N4 Fe2 N1 90.52(8) . . ? N4 Fe2 N1 90.86(8) 14_545 . ? N7 Fe2 N1 175.91(8) 14_545 14_545 ? N7 Fe2 N1 90.95(7) . 14_545 ? N4 Fe2 N1 90.86(8) . 14_545 ? N4 Fe2 N1 90.52(8) 14_545 14_545 ? N1 Fe2 N1 87.82(10) . 14_545 ? N9 Fe3 N9 169.52(11) 5_545 10 ? N9 Fe3 N3 93.49(7) 5_545 14_545 ? N9 Fe3 N3 94.15(8) 10 14_545 ? N9 Fe3 N3 94.15(8) 5_545 . ? N9 Fe3 N3 93.48(7) 10 . ? N3 Fe3 N3 86.29(10) 14_545 . ? N9 Fe3 N6 84.62(7) 5_545 5_545 ? N9 Fe3 N6 88.09(8) 10 5_545 ? N3 Fe3 N6 176.56(7) 14_545 5_545 ? N3 Fe3 N6 90.98(7) . 5_545 ? N9 Fe3 N6 88.09(8) 5_545 10 ? N9 Fe3 N6 84.63(7) 10 10 ? N3 Fe3 N6 90.97(7) 14_545 10 ? N3 Fe3 N6 176.56(8) . 10 ? N6 Fe3 N6 91.83(10) 5_545 10 ? C1 N1 Fe2 160.72(19) . . ? C1 N2 C2 118.44(17) . . ? C2 N3 Fe3 161.99(17) . . ? C3 N4 Fe2 148.55(18) . . ? C4 N5 C3 120.3(2) . . ? C4 N6 Fe3 164.09(18) . 5_554 ? C5 N7 Fe2 162.28(18) . . ? C6 N8 C5 119.7(2) . . ? C6 N9 Fe3 152.56(18) . 5_554 ? C11 N10 C7 118.26(17) . . ? C11 N10 Fe1 126.70(14) . . ? C7 N10 Fe1 114.85(13) . . ? C16 N11 C12 117.81(18) . . ? C16 N11 Fe1 126.98(14) . . ? C12 N11 Fe1 114.96(13) . . ? C21 N12 C17 117.94(17) . . ? C21 N12 Fe1 126.86(14) . . ? C17 N12 Fe1 115.20(13) . . ? N1 C1 N2 175.3(2) . . ? N3 C2 N2 173.8(2) . . ? N4 C3 N5 173.0(3) . . ? N6 C4 N5 173.7(2) . . ? N7 C5 N8 172.0(2) . . ? N9 C6 N8 173.9(2) . . ? N10 C7 C8 122.07(18) . . ? N10 C7 C12 114.34(17) . 14 ? C8 C7 C12 123.58(18) . 14 ? C9 C8 C7 118.71(19) . . ? C10 C9 C8 119.3(2) . . ? C9 C10 C11 119.09(19) . . ? N10 C11 C10 122.44(19) . . ? N11 C12 C13 121.79(18) . . ? N11 C12 C7 113.42(17) . 14 ? C13 C12 C7 124.78(18) . 14 ? C14 C13 C12 119.55(19) . . ? C15 C14 C13 118.87(19) . . ? C16 C15 C14 118.8(2) . . ? N11 C16 C15 123.1(2) . . ? N12 C17 C18 121.81(18) . . ? N12 C17 C17 113.74(11) . 14 ? C18 C17 C17 124.42(12) . 14 ? C19 C18 C17 119.51(19) . . ? C18 C19 C20 119.24(19) . . ? C21 C20 C19 118.7(2) . . ? N12 C21 C20 122.80(19) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.245 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.053 _publ_contact_author ; Prof. K.S. Murray Department of Chemistry PO Box 23 Monash University 3800 AUSTRALIA ; _publ_contact_author_phone ' +61 3 9905 4512 ' _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_email 'Keith.S.Murray@sci.monash.edu.au ' loop_ _publ_author_name _publ_author_address 'Batten, Stuart R.' ; Department of Chemistry PO Box 23 Monash University 3800 Australia ; 'Jensen, Paul' ; Department of Chemistry PO Box 23 Monash University 3800 Australia ; 'Moubaraki, Boujemaa' ; Department of Chemistry PO Box 23 Monash University 3800 Australia ; 'Murray, Keith S.' ; Department of Chemistry PO Box 23 Monash University 3800 Australia ; _publ_section_title ; Anionic metal dicyanamide networks with paramagnetic countercations ; #=END data_NibipyMndca _audit_creation_method SHELXL-97 _chemical_name_systematic ; Nickel(II) tris(2,2'-bipyridine) Bis(manganese(II) tris(dicyanamide)) ; _chemical_name_common Ni(bipy)3[Mn(dca)3]2 _chemical_melting_point ? _chemical_formula_moiety Ni(bipy)3[Mn(dca)3]2 _chemical_formula_sum 'C42 H24 Mn2 N24 Ni' _chemical_formula_weight 1033.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 28.8625(5) _cell_length_b 12.5231(2) _cell_length_c 23.9239(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8647.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prismatic _exptl_crystal_colour 'Pale orange/pink' _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4176 _exptl_absorpt_coefficient_mu 1.071 _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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28783 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 28.25 _reflns_number_total 5323 _reflns_number_gt 4791 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0261P)^2^+6.6069P] 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 0.011(9) _refine_ls_number_reflns 5323 _refine_ls_number_parameters 313 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0564 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.0000 0.000000(12) 0.01427(7) Uani 1 2 d S . . Mn1 Mn 0.0000 0.5000 0.165884(16) 0.01971(10) Uani 1 2 d S . . Mn2 Mn 0.0000 0.5000 -0.150636(14) 0.01834(10) Uani 1 2 d S . . N1 N 0.04587(6) 0.56666(14) 0.09897(7) 0.0301(4) Uani 1 1 d . . . N2 N 0.07015(6) 0.63760(13) 0.00808(7) 0.0284(4) Uani 1 1 d . . . N3 N 0.04163(6) 0.57303(13) -0.08275(7) 0.0268(4) Uani 1 1 d . . . N4 N 0.04286(6) 0.35091(13) 0.16659(8) 0.0321(4) Uani 1 1 d . . . N5 N 0.08030(6) 0.20828(18) 0.22027(10) 0.0526(6) Uani 1 1 d . . . N6 N 0.04287(6) 0.08408(14) 0.28477(7) 0.0273(4) Uani 1 1 d . . . N7 N -0.04167(6) 0.42003(14) 0.23119(7) 0.0302(4) Uani 1 1 d . . . N8 N -0.08218(6) 0.28553(14) 0.28735(7) 0.0313(4) Uani 1 1 d . . . N9 N -0.04700(7) 0.13693(14) 0.33931(7) 0.0364(5) Uani 1 1 d . . . N10 N 0.04211(5) 0.13329(11) -0.00836(6) 0.0170(3) Uani 1 1 d . . . N11 N -0.04483(5) 0.04994(11) -0.06309(6) 0.0167(3) Uani 1 1 d . . . N12 N -0.03808(5) 0.05843(11) 0.06666(6) 0.0181(3) Uani 1 1 d . . . C1 C 0.05641(6) 0.59678(14) 0.05545(7) 0.0214(4) Uani 1 1 d . . . C2 C 0.05371(6) 0.59978(14) -0.03868(8) 0.0203(4) Uani 1 1 d . . . C3 C 0.05799(7) 0.28244(16) 0.19261(8) 0.0287(4) Uani 1 1 d . . . C4 C 0.05837(6) 0.14413(15) 0.25382(9) 0.0256(4) Uani 1 1 d . . . C5 C -0.05790(6) 0.35447(14) 0.25879(9) 0.0242(4) Uani 1 1 d . . . C6 C -0.06145(7) 0.20775(16) 0.31396(8) 0.0271(4) Uani 1 1 d . . . C7 C 0.07177(6) 0.12979(13) -0.05197(7) 0.0173(4) Uani 1 1 d . . . C8 C 0.09889(6) 0.21746(14) -0.06666(7) 0.0215(4) Uani 1 1 d . . . H8 H 0.1203 0.2131 -0.0968 0.026 Uiso 1 1 calc R . . C9 C 0.09401(7) 0.31160(14) -0.03627(8) 0.0251(4) Uani 1 1 d . . . H9 H 0.1111 0.3734 -0.0465 0.030 Uiso 1 1 calc R . . C10 C 0.06422(6) 0.31467(14) 0.00883(8) 0.0244(4) Uani 1 1 d . . . H10 H 0.0610 0.3777 0.0305 0.029 Uiso 1 1 calc R . . C11 C 0.03904(6) 0.22336(13) 0.02172(7) 0.0212(4) Uani 1 1 d . . . H11 H 0.0188 0.2248 0.0531 0.025 Uiso 1 1 calc R . . C12 C -0.07287(6) -0.02721(13) -0.08354(7) 0.0169(3) Uani 1 1 d . . . C13 C -0.09962(6) -0.01094(14) -0.13090(7) 0.0226(4) Uani 1 1 d . . . H13 H -0.1186 -0.0666 -0.1451 0.027 Uiso 1 1 calc R . . C14 C -0.09830(7) 0.08760(16) -0.15732(7) 0.0271(4) Uani 1 1 d . . . H14 H -0.1163 0.1001 -0.1899 0.033 Uiso 1 1 calc R . . C15 C -0.07052(7) 0.16747(15) -0.13564(8) 0.0263(4) Uani 1 1 d . . . H15 H -0.0694 0.2360 -0.1526 0.032 Uiso 1 1 calc R . . C16 C -0.04437(6) 0.14519(14) -0.08860(7) 0.0211(4) Uani 1 1 d . . . H16 H -0.0252 0.1999 -0.0737 0.025 Uiso 1 1 calc R . . C17 C -0.02130(6) 0.03405(13) 0.11790(7) 0.0189(3) Uani 1 1 d . . . C18 C -0.04216(6) 0.07157(15) 0.16628(8) 0.0251(4) Uani 1 1 d . . . H18 H -0.0296 0.0546 0.2019 0.030 Uiso 1 1 calc R . . C19 C -0.08147(7) 0.13413(15) 0.16187(8) 0.0272(4) Uani 1 1 d . . . H19 H -0.0963 0.1603 0.1946 0.033 Uiso 1 1 calc R . . C20 C -0.09903(6) 0.15843(15) 0.10971(8) 0.0246(4) Uani 1 1 d . . . H20 H -0.1260 0.2012 0.1059 0.029 Uiso 1 1 calc R . . C21 C -0.07630(6) 0.11889(14) 0.06313(8) 0.0209(4) Uani 1 1 d . . . H21 H -0.0883 0.1353 0.0272 0.025 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 Ni1 0.01618(14) 0.01348(14) 0.01314(16) 0.000 0.000 0.00050(12) Mn1 0.02526(19) 0.01820(18) 0.0157(2) 0.000 0.000 -0.00082(15) Mn2 0.0257(2) 0.01480(19) 0.01453(19) 0.000 0.000 0.00067(14) N1 0.0426(10) 0.0285(9) 0.0191(9) -0.0007(7) 0.0044(8) -0.0085(8) N2 0.0381(9) 0.0298(8) 0.0173(7) 0.0006(7) 0.0001(8) -0.0143(7) N3 0.0353(9) 0.0249(9) 0.0203(8) -0.0007(7) 0.0006(7) -0.0068(7) N4 0.0314(8) 0.0243(9) 0.0405(10) 0.0055(8) 0.0095(8) 0.0041(7) N5 0.0283(10) 0.0630(14) 0.0664(15) 0.0437(12) 0.0137(10) 0.0071(10) N6 0.0317(9) 0.0294(9) 0.0209(8) 0.0033(7) 0.0009(7) -0.0046(7) N7 0.0287(8) 0.0353(10) 0.0265(9) 0.0071(7) 0.0038(7) 0.0024(7) N8 0.0282(9) 0.0289(9) 0.0369(9) 0.0108(7) 0.0057(8) 0.0089(7) N9 0.0466(11) 0.0303(10) 0.0324(10) 0.0077(7) 0.0112(8) 0.0158(8) N10 0.0175(7) 0.0145(7) 0.0190(8) -0.0014(5) -0.0037(6) 0.0009(6) N11 0.0169(7) 0.0175(7) 0.0156(7) -0.0010(6) 0.0006(6) 0.0006(6) N12 0.0181(7) 0.0179(7) 0.0183(8) -0.0007(6) 0.0007(6) -0.0007(6) C1 0.0240(9) 0.0154(9) 0.0248(10) -0.0034(7) -0.0001(8) -0.0028(7) C2 0.0220(9) 0.0151(9) 0.0238(10) 0.0033(7) 0.0052(7) -0.0016(7) C3 0.0241(9) 0.0290(11) 0.0330(10) 0.0026(8) 0.0129(8) -0.0018(8) C4 0.0234(9) 0.0305(10) 0.0229(9) -0.0014(8) 0.0001(9) 0.0023(7) C5 0.0241(9) 0.0270(9) 0.0214(9) 0.0011(8) 0.0021(9) 0.0080(7) C6 0.0317(10) 0.0259(10) 0.0237(9) 0.0006(8) 0.0086(9) 0.0079(8) C7 0.0183(8) 0.0160(8) 0.0175(8) 0.0010(6) -0.0050(7) 0.0004(6) C8 0.0202(8) 0.0214(9) 0.0228(9) 0.0035(7) -0.0035(7) -0.0031(7) C9 0.0254(9) 0.0168(9) 0.0330(10) 0.0035(7) -0.0116(8) -0.0032(7) C10 0.0272(9) 0.0171(8) 0.0288(10) -0.0057(8) -0.0089(9) 0.0026(7) C11 0.0208(9) 0.0194(8) 0.0235(9) -0.0043(7) -0.0064(8) 0.0040(7) C12 0.0179(8) 0.0185(8) 0.0144(8) -0.0009(6) 0.0034(7) 0.0014(6) C13 0.0221(9) 0.0259(9) 0.0199(9) -0.0026(7) -0.0002(8) -0.0040(7) C14 0.0305(10) 0.0309(11) 0.0200(10) 0.0041(7) -0.0056(8) -0.0001(8) C15 0.0341(10) 0.0208(9) 0.0241(9) 0.0066(7) -0.0043(9) 0.0012(8) C16 0.0251(9) 0.0167(8) 0.0215(10) 0.0013(7) -0.0016(7) -0.0004(7) C17 0.0217(9) 0.0174(8) 0.0176(8) 0.0008(6) 0.0006(7) -0.0017(7) C18 0.0279(9) 0.0305(10) 0.0170(8) -0.0003(7) 0.0010(8) 0.0005(8) C19 0.0287(9) 0.0305(11) 0.0225(10) -0.0063(7) 0.0048(8) 0.0018(8) C20 0.0215(9) 0.0249(10) 0.0273(10) -0.0015(8) 0.0020(8) 0.0035(7) C21 0.0179(9) 0.0235(10) 0.0213(8) -0.0008(7) -0.0008(7) 0.0008(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 Ni1 N12 2.0703(15) 2 ? Ni1 N12 2.0704(15) . ? Ni1 N10 2.0744(14) 2 ? Ni1 N10 2.0744(14) . ? Ni1 N11 2.0842(14) . ? Ni1 N11 2.0843(14) 2 ? Mn1 N7 2.2115(17) 2_565 ? Mn1 N7 2.2115(17) . ? Mn1 N1 2.2389(17) . ? Mn1 N1 2.2389(17) 2_565 ? Mn1 N4 2.2398(16) . ? Mn1 N4 2.2398(16) 2_565 ? Mn2 N9 2.1996(17) 6_554 ? Mn2 N9 2.1996(17) 5_554 ? Mn2 N3 2.2175(17) 2_565 ? Mn2 N3 2.2176(17) . ? Mn2 N6 2.2422(17) 5_554 ? Mn2 N6 2.2422(17) 6_554 ? N1 C1 1.148(2) . ? N2 C2 1.304(2) . ? N2 C1 1.305(2) . ? N3 C2 1.160(2) . ? N4 C3 1.146(3) . ? N5 C4 1.300(3) . ? N5 C3 1.310(3) . ? N6 C4 1.146(2) . ? N6 Mn2 2.2421(17) 5_545 ? N7 C5 1.153(2) . ? N8 C5 1.305(3) . ? N8 C6 1.308(3) . ? N9 C6 1.153(3) . ? N9 Mn2 2.1997(17) 5_545 ? N10 C11 1.341(2) . ? N10 C7 1.351(2) . ? N11 C16 1.340(2) . ? N11 C12 1.352(2) . ? N12 C21 1.341(2) . ? N12 C17 1.353(2) . ? C7 C8 1.393(2) . ? C7 C12 1.491(2) 2 ? C8 C9 1.392(3) . ? C9 C10 1.380(3) . ? C10 C11 1.390(3) . ? C12 C13 1.386(2) . ? C12 C7 1.490(2) 2 ? C13 C14 1.387(3) . ? C14 C15 1.383(3) . ? C15 C16 1.383(3) . ? C17 C18 1.387(3) . ? C17 C17 1.496(3) 2 ? C18 C19 1.383(3) . ? C19 C20 1.381(3) . ? C20 C21 1.385(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Ni1 N12 79.25(8) 2 . ? N12 Ni1 N10 95.79(6) 2 2 ? N12 Ni1 N10 92.73(5) . 2 ? N12 Ni1 N10 92.73(5) 2 . ? N12 Ni1 N10 95.79(6) . . ? N10 Ni1 N10 168.94(8) 2 . ? N12 Ni1 N11 173.45(6) 2 . ? N12 Ni1 N11 97.02(5) . . ? N10 Ni1 N11 78.93(6) 2 . ? N10 Ni1 N11 93.01(5) . . ? N12 Ni1 N11 97.02(5) 2 2 ? N12 Ni1 N11 173.45(6) . 2 ? N10 Ni1 N11 93.00(5) 2 2 ? N10 Ni1 N11 78.93(6) . 2 ? N11 Ni1 N11 87.19(8) . 2 ? N7 Mn1 N7 90.10(9) 2_565 . ? N7 Mn1 N1 90.84(6) 2_565 . ? N7 Mn1 N1 174.65(7) . . ? N7 Mn1 N1 174.65(6) 2_565 2_565 ? N7 Mn1 N1 90.84(6) . 2_565 ? N1 Mn1 N1 88.71(9) . 2_565 ? N7 Mn1 N4 94.12(7) 2_565 . ? N7 Mn1 N4 85.27(6) . . ? N1 Mn1 N4 89.40(7) . . ? N1 Mn1 N4 91.21(7) 2_565 . ? N7 Mn1 N4 85.27(6) 2_565 2_565 ? N7 Mn1 N4 94.12(7) . 2_565 ? N1 Mn1 N4 91.21(7) . 2_565 ? N1 Mn1 N4 89.41(7) 2_565 2_565 ? N4 Mn1 N4 179.14(10) . 2_565 ? N9 Mn2 N9 167.44(9) 6_554 5_554 ? N9 Mn2 N3 95.32(7) 6_554 2_565 ? N9 Mn2 N3 93.87(6) 5_554 2_565 ? N9 Mn2 N3 93.87(6) 6_554 . ? N9 Mn2 N3 95.32(7) 5_554 . ? N3 Mn2 N3 85.83(8) 2_565 . ? N9 Mn2 N6 87.15(7) 6_554 5_554 ? N9 Mn2 N6 84.20(6) 5_554 5_554 ? N3 Mn2 N6 175.86(6) 2_565 5_554 ? N3 Mn2 N6 90.69(6) . 5_554 ? N9 Mn2 N6 84.19(6) 6_554 6_554 ? N9 Mn2 N6 87.16(7) 5_554 6_554 ? N3 Mn2 N6 90.69(6) 2_565 6_554 ? N3 Mn2 N6 175.85(6) . 6_554 ? N6 Mn2 N6 92.87(9) 5_554 6_554 ? C1 N1 Mn1 158.03(17) . . ? C2 N2 C1 119.48(15) . . ? C2 N3 Mn2 161.38(15) . . ? C3 N4 Mn1 146.95(17) . . ? C4 N5 C3 120.71(18) . . ? C4 N6 Mn2 165.61(16) . 5_545 ? C5 N7 Mn1 161.44(16) . . ? C5 N8 C6 120.09(17) . . ? C6 N9 Mn2 151.71(16) . 5_545 ? C11 N10 C7 118.94(15) . . ? C11 N10 Ni1 125.90(12) . . ? C7 N10 Ni1 114.82(11) . . ? C16 N11 C12 118.52(15) . . ? C16 N11 Ni1 126.22(12) . . ? C12 N11 Ni1 114.78(11) . . ? C21 N12 C17 118.62(15) . . ? C21 N12 Ni1 126.01(12) . . ? C17 N12 Ni1 115.36(11) . . ? N1 C1 N2 175.2(2) . . ? N3 C2 N2 173.68(19) . . ? N4 C3 N5 172.9(2) . . ? N6 C4 N5 173.8(2) . . ? N7 C5 N8 171.5(2) . . ? N9 C6 N8 173.9(2) . . ? N10 C7 C8 121.70(16) . . ? N10 C7 C12 115.65(15) . 2 ? C8 C7 C12 122.65(16) . 2 ? C9 C8 C7 118.60(17) . . ? C10 C9 C8 119.67(17) . . ? C9 C10 C11 118.45(16) . . ? N10 C11 C10 122.58(17) . . ? N11 C12 C13 121.60(15) . . ? N11 C12 C7 114.84(15) . 2 ? C13 C12 C7 123.55(15) . 2 ? C12 C13 C14 119.21(17) . . ? C15 C14 C13 119.24(17) . . ? C14 C15 C16 118.39(17) . . ? N11 C16 C15 123.00(17) . . ? N12 C17 C18 121.63(16) . . ? N12 C17 C17 115.00(10) . 2 ? C18 C17 C17 123.36(11) . 2 ? C19 C18 C17 118.98(17) . . ? C20 C19 C18 119.68(18) . . ? C19 C20 C21 118.33(17) . . ? N12 C21 C20 122.76(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.264 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.048 _publ_contact_author ; Prof. K.S. Murray Department of Chemistry PO Box 23 Monash University 3800 AUSTRALIA ; _publ_contact_author_phone ' +61 3 9905 4512 ' _publ_contact_author_fax ' +61 3 9905 4597 ' _publ_contact_author_email ' Keith.S.Murray@sci.monash.edu.au ' loop_ _publ_author_name _publ_author_address 'Batten, Stuart R.' ; Department of Chemistry PO Box 23 Monash University 3800 Australia ; 'Jensen, Paul' ; Department of Chemistry PO Box 23 Monash University 3800 Australia ; 'Moubaraki, Boujemaa' ; Department of Chemistry PO Box 23 Monash University 3800 Australia ; 'Murray, Keith S.' ; Department of Chemistry PO Box 23 Monash University 3800 Australia ; _publ_section_title ; Anionic metal dicyanamide networks with paramagnetic countercations ; #=END