# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2031 data_ns168a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Mn(terpy)(N(CN)2)(NO3)]n' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H11 Mn N7 O3' _chemical_formula_weight 416.27 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.825(3) _cell_length_b 13.928(4) _cell_length_c 14.650(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.05(3) _cell_angle_gamma 90.00 _cell_volume 1790.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 53 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 11.8 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 1.53(3) _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'suspension method' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type 'none (mu.x = 0.24)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'mod. STOE 4-circle diffractometer' _diffrn_measurement_method 'Omega-scan; delta Omega: 1.25 deg.' _diffrn_standards_number '3 (-2 -1 6; 0 -2 -16; -2 -2 0)' _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '1 h' _diffrn_standards_decay_% 6 _diffrn_reflns_number 4467 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 26.50 _reflns_number_total 3718 _reflns_number_observed 2760 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _computing_publication_material 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 58 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0904P)^2^+0.1193P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3660 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_obs 0.0553 _refine_ls_wR_factor_all 0.1712 _refine_ls_wR_factor_obs 0.1436 _refine_ls_goodness_of_fit_all 1.060 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.106 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.22511(6) 0.25907(4) 0.94703(3) 0.0363(2) Uani 1 d . . N1 N 0.2232(4) 0.4247(2) 1.0496(2) 0.0537(8) Uani 1 d . . O1 O 0.1209(4) 0.3619(2) 1.0451(2) 0.0631(8) Uani 1 d . . O2 O 0.3321(4) 0.4081(3) 1.0031(2) 0.0682(9) Uani 1 d . . O3 O 0.2178(5) 0.4947(3) 1.0973(3) 0.0976(13) Uani 1 d . . N2 N 0.3519(4) 0.1848(3) 1.0633(2) 0.0553(9) Uani 1 d . . C1 C 0.4126(4) 0.1459(3) 1.1247(2) 0.0426(8) Uani 1 d . . N3 N 0.4793(5) 0.0922(3) 1.1895(2) 0.0678(12) Uani 1 d . . C2 C 0.0450(4) 0.3693(3) 0.7644(2) 0.0411(8) Uani 1 d . . N4 N 0.1045(4) 0.3428(2) 0.8327(2) 0.0484(8) Uani 1 d . . N5 N 0.0090(3) 0.1711(2) 0.9691(2) 0.0460(7) Uani 1 d . . C3 C -0.0730(5) 0.1836(3) 1.0392(3) 0.0593(11) Uani 1 d . . H3 H -0.0431(5) 0.2315(3) 1.0816(3) 0.071 Uiso 1 calc R . C4 C -0.1998(5) 0.1299(4) 1.0526(4) 0.0744(14) Uani 1 d . . H4 H -0.2535(5) 0.1406(4) 1.1030(4) 0.089 Uiso 1 calc R . C5 C -0.2439(6) 0.0606(4) 0.9899(4) 0.0766(15) Uani 1 d . . H5 H -0.3298(6) 0.0237(4) 0.9964(4) 0.092 Uiso 1 calc R . C6 C -0.1614(5) 0.0456(3) 0.9171(4) 0.0633(12) Uani 1 d . . H6 H -0.1902(5) -0.0020(3) 0.8742(4) 0.076 Uiso 1 calc R . C7 C -0.0348(4) 0.1018(3) 0.9080(3) 0.0474(9) Uani 1 d . . C8 C 0.0620(4) 0.0905(3) 0.8324(3) 0.0478(9) Uani 1 d . . N6 N 0.1968(3) 0.1363(2) 0.8447(2) 0.0419(7) Uani 1 d . . C9 C 0.0192(6) 0.0401(3) 0.7531(3) 0.0666(13) Uani 1 d . . H9 H -0.0750(6) 0.0095(3) 0.7447(3) 0.080 Uiso 1 calc R . C10 C 0.1179(7) 0.0356(4) 0.6865(3) 0.0769(15) Uani 1 d . . H10 H 0.0904(7) 0.0022(4) 0.6323(3) 0.092 Uiso 1 calc R . C11 C 0.2556(6) 0.0800(3) 0.6999(3) 0.0631(12) Uani 1 d . . H11 H 0.3237(6) 0.0762(3) 0.6557(3) 0.076 Uiso 1 calc R . C12 C 0.2932(5) 0.1311(3) 0.7803(2) 0.0452(9) Uani 1 d . . C13 C 0.4381(4) 0.1855(3) 0.8013(2) 0.0446(8) Uani 1 d . . C14 C 0.5629(5) 0.1714(3) 0.7546(3) 0.0557(10) Uani 1 d . . H14 H 0.5604(5) 0.1256(3) 0.7083(3) 0.067 Uiso 1 calc R . C15 C 0.6927(6) 0.2257(4) 0.7771(4) 0.0667(13) Uani 1 d . . H15 H 0.7783(6) 0.2172(4) 0.7460(4) 0.080 Uiso 1 calc R . C16 C 0.6931(5) 0.2924(3) 0.8460(3) 0.0611(11) Uani 1 d . . H16 H 0.7783(5) 0.3305(3) 0.8619(3) 0.073 Uiso 1 calc R . C17 C 0.5653(4) 0.3018(3) 0.8911(3) 0.0509(9) Uani 1 d . . H17 H 0.5671(4) 0.3462(3) 0.9387(3) 0.061 Uiso 1 calc R . N7 N 0.4378(4) 0.2502(2) 0.8702(2) 0.0429(7) Uani 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 Mn1 0.0376(3) 0.0419(3) 0.0290(3) -0.0018(2) 0.0009(2) -0.0044(2) N1 0.067(2) 0.049(2) 0.044(2) -0.008(2) 0.005(2) -0.005(2) O1 0.075(2) 0.064(2) 0.054(2) -0.0114(14) 0.0214(15) -0.020(2) O2 0.063(2) 0.079(2) 0.064(2) -0.004(2) 0.017(2) -0.011(2) O3 0.115(3) 0.063(2) 0.113(3) -0.042(2) 0.004(3) -0.001(2) N2 0.055(2) 0.067(2) 0.042(2) 0.004(2) -0.005(2) -0.006(2) C1 0.040(2) 0.050(2) 0.037(2) -0.006(2) 0.002(2) -0.006(2) N3 0.100(3) 0.046(2) 0.050(2) -0.002(2) -0.029(2) 0.001(2) C2 0.042(2) 0.040(2) 0.041(2) -0.008(2) 0.000(2) -0.0005(15) N4 0.050(2) 0.052(2) 0.041(2) 0.0004(15) -0.0039(14) 0.0020(15) N5 0.041(2) 0.050(2) 0.047(2) 0.0006(15) 0.0036(14) -0.0089(14) C3 0.054(2) 0.065(3) 0.062(3) -0.004(2) 0.016(2) -0.011(2) C4 0.058(3) 0.082(3) 0.087(4) 0.006(3) 0.025(3) -0.015(2) C5 0.055(3) 0.070(3) 0.106(4) 0.011(3) 0.010(3) -0.021(2) C6 0.054(2) 0.052(2) 0.083(3) -0.001(2) 0.000(2) -0.017(2) C7 0.044(2) 0.039(2) 0.056(2) 0.004(2) -0.009(2) -0.007(2) C8 0.052(2) 0.041(2) 0.048(2) -0.006(2) -0.006(2) -0.002(2) N6 0.046(2) 0.040(2) 0.038(2) -0.0032(13) -0.0034(13) 0.0008(13) C9 0.071(3) 0.058(3) 0.067(3) -0.021(2) -0.012(2) -0.009(2) C10 0.102(4) 0.068(3) 0.057(3) -0.034(2) -0.009(3) -0.001(3) C11 0.084(3) 0.058(3) 0.047(2) -0.016(2) 0.005(2) 0.013(2) C12 0.058(2) 0.040(2) 0.037(2) -0.004(2) 0.001(2) 0.009(2) C13 0.055(2) 0.043(2) 0.036(2) 0.005(2) 0.007(2) 0.009(2) C14 0.070(3) 0.058(2) 0.044(2) 0.004(2) 0.026(2) 0.012(2) C15 0.062(3) 0.067(3) 0.077(3) 0.018(2) 0.038(2) 0.011(2) C16 0.047(2) 0.058(3) 0.081(3) 0.012(2) 0.018(2) 0.000(2) C17 0.044(2) 0.049(2) 0.061(2) -0.002(2) 0.009(2) -0.002(2) N7 0.043(2) 0.047(2) 0.039(2) -0.0014(13) 0.0066(13) 0.0009(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 Mn1 N2 2.196(3) . yes Mn1 N4 2.218(3) . yes Mn1 N6 2.271(3) . yes Mn1 O1 2.289(3) . yes Mn1 N7 2.291(3) . yes Mn1 N5 2.318(3) . yes Mn1 O2 2.390(3) . yes N1 O3 1.203(5) . yes N1 O1 1.253(4) . yes N1 O2 1.257(5) . yes N2 C1 1.134(5) . yes C1 N3 1.300(5) . yes N3 C2 1.302(5) 4_666 yes C2 N4 1.141(4) . yes C2 N3 1.302(5) 4_565 yes N5 C3 1.328(5) . ? N5 C7 1.345(5) . ? C3 C4 1.378(6) . ? C3 H3 0.93 . ? C4 C5 1.361(7) . ? C4 H4 0.93 . ? C5 C6 1.369(7) . ? C5 H5 0.93 . ? C6 C7 1.382(6) . ? C6 H6 0.93 . ? C7 C8 1.477(6) . ? C8 N6 1.345(5) . ? C8 C9 1.375(5) . ? N6 C12 1.337(5) . ? C9 C10 1.377(7) . ? C9 H9 0.93 . ? C10 C11 1.360(7) . ? C10 H10 0.93 . ? C11 C12 1.387(5) . ? C11 H11 0.93 . ? C12 C13 1.490(5) . ? C13 N7 1.353(5) . ? C13 C14 1.371(6) . ? C14 C15 1.384(7) . ? C14 H14 0.93 . ? C15 C16 1.372(7) . ? C15 H15 0.93 . ? C16 C17 1.372(6) . ? C16 H16 0.93 . ? C17 N7 1.344(5) . ? C17 H17 0.93 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mn1 N4 176.31(13) . . yes N2 Mn1 N6 99.71(12) . . yes N4 Mn1 N6 83.51(12) . . yes N2 Mn1 O1 90.78(13) . . yes N4 Mn1 O1 87.26(12) . . yes N6 Mn1 O1 149.57(11) . . yes N2 Mn1 N7 88.77(13) . . yes N4 Mn1 N7 90.60(12) . . yes N6 Mn1 N7 70.96(11) . . yes O1 Mn1 N7 138.25(11) . . yes N2 Mn1 N5 90.11(12) . . yes N4 Mn1 N5 92.70(12) . . yes N6 Mn1 N5 70.08(12) . . yes O1 Mn1 N5 81.51(11) . . yes N7 Mn1 N5 140.23(12) . . yes N2 Mn1 O2 89.55(13) . . yes N4 Mn1 O2 86.76(12) . . yes N6 Mn1 O2 153.27(12) . . yes O1 Mn1 O2 53.91(11) . . yes N7 Mn1 O2 84.34(11) . . yes N5 Mn1 O2 135.41(12) . . yes O3 N1 O1 121.6(4) . . yes O3 N1 O2 122.8(4) . . yes O1 N1 O2 115.5(3) . . yes N1 O1 Mn1 97.8(2) . . yes N1 O2 Mn1 92.8(2) . . yes C1 N2 Mn1 177.5(3) . . yes N2 C1 N3 173.3(4) . . yes C2 N3 C1 120.4(4) 4_666 . yes N4 C2 N3 174.5(4) . 4_565 yes C2 N4 Mn1 166.3(3) . . yes C3 N5 C7 117.8(3) . . ? C3 N5 Mn1 124.2(3) . . ? C7 N5 Mn1 118.0(3) . . ? N5 C3 C4 123.8(4) . . ? N5 C3 H3 118.1(2) . . ? C4 C3 H3 118.1(3) . . ? C5 C4 C3 117.9(5) . . ? C5 C4 H4 121.1(3) . . ? C3 C4 H4 121.1(3) . . ? C4 C5 C6 119.8(4) . . ? C4 C5 H5 120.1(3) . . ? C6 C5 H5 120.1(3) . . ? C5 C6 C7 119.3(4) . . ? C5 C6 H6 120.3(3) . . ? C7 C6 H6 120.3(3) . . ? N5 C7 C6 121.4(4) . . ? N5 C7 C8 115.3(3) . . ? C6 C7 C8 123.3(4) . . ? N6 C8 C9 121.1(4) . . ? N6 C8 C7 115.0(3) . . ? C9 C8 C7 123.9(4) . . ? C12 N6 C8 120.0(3) . . ? C12 N6 Mn1 118.2(2) . . ? C8 N6 Mn1 118.7(3) . . ? C10 C9 C8 118.9(4) . . ? C10 C9 H9 120.6(3) . . ? C8 C9 H9 120.6(3) . . ? C11 C10 C9 120.0(4) . . ? C11 C10 H10 120.0(3) . . ? C9 C10 H10 120.0(3) . . ? C10 C11 C12 119.1(4) . . ? C10 C11 H11 120.5(3) . . ? C12 C11 H11 120.5(3) . . ? N6 C12 C11 121.0(4) . . ? N6 C12 C13 115.0(3) . . ? C11 C12 C13 124.0(4) . . ? N7 C13 C14 122.2(4) . . ? N7 C13 C12 115.0(3) . . ? C14 C13 C12 122.8(4) . . ? C13 C14 C15 119.4(4) . . ? C13 C14 H14 120.3(3) . . ? C15 C14 H14 120.3(3) . . ? C16 C15 C14 118.9(4) . . ? C16 C15 H15 120.5(3) . . ? C14 C15 H15 120.5(3) . . ? C15 C16 C17 118.7(4) . . ? C15 C16 H16 120.6(3) . . ? C17 C16 H16 120.6(3) . . ? N7 C17 C16 123.4(4) . . ? N7 C17 H17 118.3(2) . . ? C16 C17 H17 118.3(3) . . ? C17 N7 C13 117.3(3) . . ? C17 N7 Mn1 124.7(3) . . ? C13 N7 Mn1 118.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 N1 O1 Mn1 -178.4(4) . . . . ? O2 N1 O1 Mn1 0.0(4) . . . . ? N2 Mn1 O1 N1 88.9(2) . . . . ? N4 Mn1 O1 N1 -88.0(2) . . . . ? N6 Mn1 O1 N1 -160.2(2) . . . . ? N7 Mn1 O1 N1 -0.2(3) . . . . ? N5 Mn1 O1 N1 178.9(2) . . . . ? O2 Mn1 O1 N1 0.0(2) . . . . ? O3 N1 O2 Mn1 178.3(4) . . . . ? O1 N1 O2 Mn1 0.0(3) . . . . ? N2 Mn1 O2 N1 -91.3(2) . . . . ? N4 Mn1 O2 N1 89.0(2) . . . . ? N6 Mn1 O2 N1 157.6(2) . . . . ? O1 Mn1 O2 N1 0.0(2) . . . . ? N7 Mn1 O2 N1 179.9(2) . . . . ? N5 Mn1 O2 N1 -1.6(3) . . . . ? N4 Mn1 N2 C1 112.0(75) . . . . ? N6 Mn1 N2 C1 -97.2(77) . . . . ? O1 Mn1 N2 C1 54.1(77) . . . . ? N7 Mn1 N2 C1 -167.7(77) . . . . ? N5 Mn1 N2 C1 -27.4(77) . . . . ? O2 Mn1 N2 C1 108.0(77) . . . . ? Mn1 N2 C1 N3 89.9(87) . . . . ? N2 C1 N3 C2 175.9(35) . . . 4_666 ? N3 C2 N4 Mn1 -162.5(36) 4_565 . . . ? N2 Mn1 N4 C2 145.7(19) . . . . ? N6 Mn1 N4 C2 -5.3(13) . . . . ? O1 Mn1 N4 C2 -156.2(13) . . . . ? N7 Mn1 N4 C2 65.5(13) . . . . ? N5 Mn1 N4 C2 -74.9(13) . . . . ? O2 Mn1 N4 C2 149.8(13) . . . . ? N2 Mn1 N5 C3 71.4(3) . . . . ? N4 Mn1 N5 C3 -106.2(3) . . . . ? N6 Mn1 N5 C3 171.7(4) . . . . ? O1 Mn1 N5 C3 -19.4(3) . . . . ? N7 Mn1 N5 C3 159.6(3) . . . . ? O2 Mn1 N5 C3 -18.1(4) . . . . ? N2 Mn1 N5 C7 -107.4(3) . . . . ? N4 Mn1 N5 C7 75.0(3) . . . . ? N6 Mn1 N5 C7 -7.1(3) . . . . ? O1 Mn1 N5 C7 161.8(3) . . . . ? N7 Mn1 N5 C7 -19.2(4) . . . . ? O2 Mn1 N5 C7 163.1(2) . . . . ? C7 N5 C3 C4 0.0(7) . . . . ? Mn1 N5 C3 C4 -178.8(4) . . . . ? N5 C3 C4 C5 -0.6(8) . . . . ? C3 C4 C5 C6 0.9(8) . . . . ? C4 C5 C6 C7 -0.6(8) . . . . ? C3 N5 C7 C6 0.3(6) . . . . ? Mn1 N5 C7 C6 179.2(3) . . . . ? C3 N5 C7 C8 -179.2(4) . . . . ? Mn1 N5 C7 C8 -0.3(4) . . . . ? C5 C6 C7 N5 0.0(7) . . . . ? C5 C6 C7 C8 179.5(4) . . . . ? N5 C7 C8 N6 13.2(5) . . . . ? C6 C7 C8 N6 -166.4(4) . . . . ? N5 C7 C8 C9 -164.8(4) . . . . ? C6 C7 C8 C9 15.7(6) . . . . ? C9 C8 N6 C12 -1.7(6) . . . . ? C7 C8 N6 C12 -179.8(3) . . . . ? C9 C8 N6 Mn1 157.8(3) . . . . ? C7 C8 N6 Mn1 -20.3(4) . . . . ? N2 Mn1 N6 C12 -98.7(3) . . . . ? N4 Mn1 N6 C12 79.4(3) . . . . ? O1 Mn1 N6 C12 152.7(3) . . . . ? N7 Mn1 N6 C12 -13.5(2) . . . . ? N5 Mn1 N6 C12 174.7(3) . . . . ? O2 Mn1 N6 C12 10.1(4) . . . . ? N2 Mn1 N6 C8 101.4(3) . . . . ? N4 Mn1 N6 C8 -80.4(3) . . . . ? O1 Mn1 N6 C8 -7.2(4) . . . . ? N7 Mn1 N6 C8 -173.3(3) . . . . ? N5 Mn1 N6 C8 14.8(3) . . . . ? O2 Mn1 N6 C8 -149.8(3) . . . . ? N6 C8 C9 C10 1.1(7) . . . . ? C7 C8 C9 C10 178.9(4) . . . . ? C8 C9 C10 C11 0.4(8) . . . . ? C9 C10 C11 C12 -1.3(7) . . . . ? C8 N6 C12 C11 0.8(5) . . . . ? Mn1 N6 C12 C11 -158.8(3) . . . . ? C8 N6 C12 C13 179.5(3) . . . . ? Mn1 N6 C12 C13 19.9(4) . . . . ? C10 C11 C12 N6 0.7(6) . . . . ? C10 C11 C12 C13 -177.8(4) . . . . ? N6 C12 C13 N7 -15.1(5) . . . . ? C11 C12 C13 N7 163.4(4) . . . . ? N6 C12 C13 C14 164.8(3) . . . . ? C11 C12 C13 C14 -16.6(6) . . . . ? N7 C13 C14 C15 -1.1(6) . . . . ? C12 C13 C14 C15 179.0(4) . . . . ? C13 C14 C15 C16 0.2(7) . . . . ? C14 C15 C16 C17 1.0(7) . . . . ? C15 C16 C17 N7 -1.4(7) . . . . ? C16 C17 N7 C13 0.5(6) . . . . ? C16 C17 N7 Mn1 177.5(3) . . . . ? C14 C13 N7 C17 0.8(5) . . . . ? C12 C13 N7 C17 -179.3(3) . . . . ? C14 C13 N7 Mn1 -176.5(3) . . . . ? C12 C13 N7 Mn1 3.4(4) . . . . ? N2 Mn1 N7 C17 -71.7(3) . . . . ? N4 Mn1 N7 C17 104.7(3) . . . . ? N6 Mn1 N7 C17 -172.4(3) . . . . ? O1 Mn1 N7 C17 18.2(4) . . . . ? N5 Mn1 N7 C17 -160.4(3) . . . . ? O2 Mn1 N7 C17 18.0(3) . . . . ? N2 Mn1 N7 C13 105.4(3) . . . . ? N4 Mn1 N7 C13 -78.3(3) . . . . ? N6 Mn1 N7 C13 4.7(2) . . . . ? O1 Mn1 N7 C13 -164.8(2) . . . . ? N5 Mn1 N7 C13 16.7(3) . . . . ? O2 Mn1 N7 C13 -165.0(3) . . . . ? _refine_diff_density_max 0.666 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.098 #===END data_ac01a1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Mn(terpy)(N(CN)2)(H2O)](N(CN)2)' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H13 Mn N9 O' _chemical_formula_weight 438.32 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 7.574(2) _cell_length_b 8.795(3) _cell_length_c 14.948(6) _cell_angle_alpha 78.16(3) _cell_angle_beta 79.73(3) _cell_angle_gamma 81.80(2) _cell_volume 953.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.6 _exptl_crystal_description prism _exptl_crystal_colour 'transparent yellow' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 1.53(3) _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'suspension method' _exptl_crystal_F_000 446 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type 'none (mu.x = 0.24)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'mod. STOE 4-circle diffractometer' _diffrn_measurement_method 'Omega-scan, delta Omega: 1.25 deg.' _diffrn_standards_number '2 (0 0 4; 1 0 2)' _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '1 h' _diffrn_standards_decay_% 5 _diffrn_reflns_number 4419 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 26.50 _reflns_number_total 3950 _reflns_number_observed 3568 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _computing_publication_material 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 54 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0447P)^2^+0.2601P] 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 3896 _refine_ls_number_parameters 278 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_obs 0.0372 _refine_ls_wR_factor_all 0.1933 _refine_ls_wR_factor_obs 0.0947 _refine_ls_goodness_of_fit_all 1.073 _refine_ls_goodness_of_fit_obs 1.079 _refine_ls_restrained_S_all 2.086 _refine_ls_restrained_S_obs 1.079 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.32682(4) 0.38983(3) 0.81741(2) 0.03218(11) Uani 1 d . . O1 O 0.5992(2) 0.2707(2) 0.77330(13) 0.0506(4) Uani 1 d D . N1 N 0.3334(2) 0.5607(2) 0.67940(11) 0.0364(4) Uani 1 d . . C1 C 0.3933(3) 0.7015(2) 0.6639(2) 0.0447(5) Uani 1 d . . H1 H 0.4277(3) 0.7348(2) 0.7127(2) 0.054 Uiso 1 calc R . C2 C 0.4058(3) 0.7987(3) 0.5790(2) 0.0543(6) Uani 1 d . . H2 H 0.4492(3) 0.8952(3) 0.5705(2) 0.065 Uiso 1 calc R . C3 C 0.3535(4) 0.7512(3) 0.5071(2) 0.0586(6) Uani 1 d . . H3 H 0.3608(4) 0.8153(3) 0.4490(2) 0.070 Uiso 1 calc R . C4 C 0.2898(3) 0.6076(3) 0.5214(2) 0.0516(6) Uani 1 d . . H4 H 0.2529(3) 0.5739(3) 0.4734(2) 0.062 Uiso 1 calc R . C5 C 0.2815(3) 0.5139(2) 0.60892(13) 0.0376(4) Uani 1 d . . N2 N 0.2283(2) 0.2788(2) 0.71675(11) 0.0354(4) Uani 1 d . . C6 C 0.2188(3) 0.3561(2) 0.63080(14) 0.0384(4) Uani 1 d . . C7 C 0.1547(3) 0.2919(3) 0.5671(2) 0.0516(6) Uani 1 d . . H7 H 0.1498(3) 0.3466(3) 0.5072(2) 0.062 Uiso 1 calc R . C8 C 0.0988(4) 0.1454(3) 0.5949(2) 0.0593(7) Uani 1 d . . H8 H 0.0533(4) 0.1005(3) 0.5539(2) 0.071 Uiso 1 calc R . C9 C 0.1099(3) 0.0648(3) 0.6832(2) 0.0541(6) Uani 1 d . . H9 H 0.0730(3) -0.0347(3) 0.7023(2) 0.065 Uiso 1 calc R . C10 C 0.1772(3) 0.1347(2) 0.7434(2) 0.0399(4) Uani 1 d . . C11 C 0.2009(3) 0.0576(2) 0.8390(2) 0.0415(5) Uani 1 d . . C12 C 0.1703(4) -0.0965(3) 0.8740(2) 0.0597(7) Uani 1 d . . H12 H 0.1322(4) -0.1556(3) 0.8376(2) 0.072 Uiso 1 calc R . C13 C 0.1968(4) -0.1613(3) 0.9632(2) 0.0679(8) Uani 1 d . . H13 H 0.1777(4) -0.2649(3) 0.9875(2) 0.081 Uiso 1 calc R . C14 C 0.2515(4) -0.0720(3) 1.0157(2) 0.0637(7) Uani 1 d . . H14 H 0.2693(4) -0.1135(3) 1.0763(2) 0.076 Uiso 1 calc R . C15 C 0.2799(3) 0.0814(3) 0.9771(2) 0.0508(5) Uani 1 d . . H15 H 0.3167(3) 0.1420(3) 1.0130(2) 0.061 Uiso 1 calc R . N3 N 0.2566(2) 0.1459(2) 0.89036(12) 0.0399(4) Uani 1 d . . N4 N 0.4858(2) 0.5157(2) 0.87795(13) 0.0478(4) Uani 1 d . . C16 C 0.6160(3) 0.5532(2) 0.89134(13) 0.0373(4) Uani 1 d . . N5 N 0.7528(2) 0.6073(2) 0.91034(15) 0.0519(5) Uani 1 d . . C17 C -0.0831(3) 0.5457(2) 0.88920(13) 0.0353(4) Uani 1 d . . N6 N 0.0667(2) 0.5009(2) 0.87472(13) 0.0438(4) Uani 1 d . . N7 N 0.8220(3) 0.5049(2) 0.67967(14) 0.0518(5) Uani 1 d . . C18 C 0.8373(3) 0.6337(3) 0.67617(15) 0.0421(5) Uani 1 d . . N8 N 0.8705(3) 0.7777(3) 0.6659(2) 0.0691(7) Uani 1 d . . C19 C 0.7449(4) 0.8834(3) 0.6918(2) 0.0541(6) Uani 1 d . . N9 N 0.6472(4) 0.9880(3) 0.7096(2) 0.0794(8) Uani 1 d . . H5 H 0.6755(36) 0.3306(30) 0.7426(20) 0.083(7) Uiso 1 d D . H6 H 0.6122(42) 0.1889(25) 0.7523(20) 0.083(7) Uiso 1 d 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 Mn1 0.0337(2) 0.0296(2) 0.0360(2) -0.00726(11) -0.00931(12) -0.00623(11) O1 0.0422(9) 0.0372(8) 0.0731(11) -0.0186(8) -0.0005(8) -0.0048(7) N1 0.0380(9) 0.0332(8) 0.0383(9) -0.0045(7) -0.0076(7) -0.0052(7) C1 0.0460(12) 0.0372(11) 0.0507(12) -0.0037(9) -0.0100(9) -0.0074(9) C2 0.0563(14) 0.0364(11) 0.0630(15) 0.0051(10) -0.0059(11) -0.0058(10) C3 0.065(2) 0.0540(14) 0.0472(13) 0.0106(11) -0.0090(11) -0.0022(12) C4 0.0555(14) 0.0571(14) 0.0393(11) -0.0029(10) -0.0126(10) 0.0013(11) C5 0.0363(10) 0.0409(10) 0.0353(10) -0.0080(8) -0.0078(8) 0.0017(8) N2 0.0362(9) 0.0332(8) 0.0404(9) -0.0108(7) -0.0091(7) -0.0059(6) C6 0.0361(10) 0.0427(11) 0.0390(10) -0.0136(8) -0.0091(8) -0.0002(8) C7 0.0549(14) 0.0604(14) 0.0475(12) -0.0227(11) -0.0176(10) -0.0017(11) C8 0.062(2) 0.063(2) 0.068(2) -0.0330(13) -0.0263(13) -0.0063(12) C9 0.0538(14) 0.0440(12) 0.075(2) -0.0242(12) -0.0168(12) -0.0114(10) C10 0.0379(10) 0.0347(10) 0.0515(12) -0.0145(9) -0.0078(9) -0.0073(8) C11 0.0387(11) 0.0313(10) 0.0544(12) -0.0081(9) -0.0033(9) -0.0083(8) C12 0.067(2) 0.0351(11) 0.075(2) -0.0072(11) -0.0027(13) -0.0161(11) C13 0.078(2) 0.0363(12) 0.080(2) 0.0048(12) -0.001(2) -0.0140(12) C14 0.067(2) 0.0537(15) 0.059(2) 0.0118(12) -0.0068(13) -0.0032(12) C15 0.0560(14) 0.0454(12) 0.0478(12) 0.0001(10) -0.0098(10) -0.0047(10) N3 0.0407(9) 0.0339(8) 0.0448(9) -0.0045(7) -0.0068(7) -0.0072(7) N4 0.0369(10) 0.0641(12) 0.0517(11) -0.0269(9) -0.0090(8) -0.0099(8) C16 0.0360(10) 0.0425(10) 0.0365(10) -0.0163(8) -0.0056(8) -0.0016(8) N5 0.0329(9) 0.0612(12) 0.0736(13) -0.0386(10) -0.0104(9) -0.0043(8) C17 0.0391(11) 0.0364(10) 0.0351(9) -0.0094(8) -0.0102(8) -0.0101(8) N6 0.0360(10) 0.0513(10) 0.0479(10) -0.0161(8) -0.0100(8) -0.0030(8) N7 0.0515(11) 0.0447(11) 0.0600(12) -0.0161(9) -0.0024(9) -0.0060(8) C18 0.0422(11) 0.0434(12) 0.0420(11) -0.0116(9) -0.0052(9) -0.0051(9) N8 0.0621(14) 0.0450(11) 0.101(2) -0.0239(12) 0.0048(13) -0.0167(10) C19 0.0624(15) 0.0374(12) 0.067(2) -0.0111(11) -0.0110(12) -0.0168(11) N9 0.084(2) 0.0400(12) 0.118(2) -0.0260(13) -0.010(2) -0.0076(12) _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 2.162(2) . yes Mn1 N6 2.182(2) . yes Mn1 N2 2.233(2) . yes Mn1 O1 2.230(2) . yes Mn1 N3 2.288(2) . yes Mn1 N1 2.287(2) . yes O1 H5 0.85(2) . yes O1 H6 0.83(2) . yes N1 C1 1.341(3) . ? N1 C5 1.344(3) . ? C1 C2 1.373(3) . ? C1 H1 0.93 . ? C2 C3 1.368(4) . ? C2 H2 0.93 . ? C3 C4 1.378(4) . ? C3 H3 0.93 . ? C4 C5 1.392(3) . ? C4 H4 0.93 . ? C5 C6 1.485(3) . ? N2 C6 1.334(3) . ? N2 C10 1.339(3) . ? C6 C7 1.387(3) . ? C7 C8 1.373(4) . ? C7 H7 0.93 . ? C8 C9 1.375(4) . ? C8 H8 0.93 . ? C9 C10 1.388(3) . ? C9 H9 0.93 . ? C10 C11 1.480(3) . ? C11 N3 1.351(3) . ? C11 C12 1.385(3) . ? C12 C13 1.376(4) . ? C12 H12 0.93 . ? C13 C14 1.366(4) . ? C13 H13 0.93 . ? C14 C15 1.385(3) . ? C14 H14 0.93 . ? C15 N3 1.336(3) . ? C15 H15 0.93 . ? N4 C16 1.145(3) . yes C16 N5 1.297(3) . yes N5 C17 1.294(3) 1_655 yes C17 N6 1.145(3) . yes C17 N5 1.294(3) 1_455 yes N7 C18 1.144(3) . yes C18 N8 1.299(3) . yes N8 C19 1.298(3) . yes C19 N9 1.140(3) . yes O1 N7 2.831(3) . yes O1 N9 2.795(3) 1_545 yes H5 N7 2.00(2) . yes H6 N9 1.97(2) 1_545 yes 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 N6 95.05(7) . . yes N4 Mn1 N2 162.08(7) . . yes N6 Mn1 N2 97.80(7) . . yes N4 Mn1 O1 81.41(7) . . yes N6 Mn1 O1 174.23(7) . . yes N2 Mn1 O1 86.67(7) . . yes N4 Mn1 N3 120.14(8) . . yes N6 Mn1 N3 92.40(7) . . yes N2 Mn1 N3 71.81(7) . . yes O1 Mn1 N3 85.51(7) . . yes N4 Mn1 N1 95.82(8) . . yes N6 Mn1 N1 92.64(7) . . yes N2 Mn1 N1 71.22(7) . . yes O1 Mn1 N1 92.25(7) . . yes N3 Mn1 N1 143.03(7) . . yes Mn1 O1 H5 115.2(21) . . ? Mn1 O1 H6 121.8(22) . . ? H5 O1 H6 109.7(25) . . yes C1 N1 C5 118.4(2) . . ? C1 N1 Mn1 123.76(14) . . ? C5 N1 Mn1 117.81(13) . . ? N1 C1 C2 122.9(2) . . ? N1 C1 H1 118.57(12) . . ? C2 C1 H1 118.57(15) . . ? C3 C2 C1 118.9(2) . . ? C3 C2 H2 120.55(14) . . ? C1 C2 H2 120.55(15) . . ? C2 C3 C4 119.4(2) . . ? C2 C3 H3 120.30(14) . . ? C4 C3 H3 120.30(14) . . ? C3 C4 C5 119.0(2) . . ? C3 C4 H4 120.50(14) . . ? C5 C4 H4 120.50(14) . . ? N1 C5 C4 121.5(2) . . ? N1 C5 C6 115.4(2) . . ? C4 C5 C6 123.1(2) . . ? C6 N2 C10 120.2(2) . . ? C6 N2 Mn1 120.22(13) . . ? C10 N2 Mn1 119.60(14) . . ? N2 C6 C7 121.7(2) . . ? N2 C6 C5 115.3(2) . . ? C7 C6 C5 123.0(2) . . ? C8 C7 C6 118.2(2) . . ? C8 C7 H7 120.90(14) . . ? C6 C7 H7 120.90(14) . . ? C7 C8 C9 120.2(2) . . ? C7 C8 H8 119.88(14) . . ? C9 C8 H8 119.88(14) . . ? C8 C9 C10 118.8(2) . . ? C8 C9 H9 120.59(14) . . ? C10 C9 H9 120.59(14) . . ? N2 C10 C9 120.8(2) . . ? N2 C10 C11 115.5(2) . . ? C9 C10 C11 123.7(2) . . ? N3 C11 C12 121.5(2) . . ? N3 C11 C10 116.0(2) . . ? C12 C11 C10 122.5(2) . . ? C13 C12 C11 119.4(3) . . ? C13 C12 H12 120.3(2) . . ? C11 C12 H12 120.3(2) . . ? C14 C13 C12 119.3(2) . . ? C14 C13 H13 120.4(2) . . ? C12 C13 H13 120.4(2) . . ? C13 C14 C15 118.8(3) . . ? C13 C14 H14 120.6(2) . . ? C15 C14 H14 120.6(2) . . ? N3 C15 C14 122.8(2) . . ? N3 C15 H15 118.61(13) . . ? C14 C15 H15 118.6(2) . . ? C15 N3 C11 118.2(2) . . ? C15 N3 Mn1 124.7(2) . . ? C11 N3 Mn1 116.85(14) . . ? C16 N4 Mn1 155.6(2) . . ? N4 C16 N5 174.0(2) . . yes C17 N5 C16 121.9(2) 1_655 . yes N6 C17 N5 173.6(2) . 1_455 yes C17 N6 Mn1 164.0(2) . . yes N7 C18 N8 173.8(3) . . yes C19 N8 C18 120.5(2) . . yes N9 C19 N8 172.4(3) . . yes N7 O1 N9 118.14(9) . 1_545 yes O1 H5 N7 169(3) . . yes O1 H6 N9 177(3) . 1_545 yes _refine_diff_density_max 0.286 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.054 #===END