# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Nirmalendu Ray Chaudhuri' 'Sudipta Dalai' 'Partha Sarathi Mukherjee' 'Ennio Zangrando' _publ_contact_author_name 'Prof Nirmalendu Ray Chaudhuri' _publ_contact_author_address ; Department of Chemistry Indian Association for the Cultivation of Science Jadavpur Calcutta 700 032 INDIA ; _publ_contact_author_email 'ICNRC@MAHENDRA.IACS.RES.IN' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Synthesis, crystal structure and magnetic property of two new dicyanamide bridged 2D and 1D complexes of Mn(II) ; data_complex1 _database_code_CSD 190860 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(4-cyanopyridine)-bis(dicyanamide)-manganese(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C6 H4 N2) 2(N3 C2 1-) (Mn 2+)' _chemical_formula_sum 'C16 H8 Mn N10' _chemical_formula_weight 395.26 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' _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+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 9.479(4) _cell_length_b 12.308(5) _cell_length_c 14.402(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1680.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'no colour' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4276 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 28.81 _reflns_number_total 2179 _reflns_number_gt 1801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'Shelxl-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.64.02 (Farrugia, 1999)' _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^)+(0.0692P)^2^+0.2108P] 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 SHELXL _refine_ls_extinction_coef 0.032(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2179 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Mn Mn 0.7500 -0.2500 -0.14980(2) 0.03990(16) Uani 1 2 d S . . N1 N 0.60343(15) -0.16964(11) -0.03808(10) 0.0459(3) Uani 1 1 d . . . C1 C 0.65825(18) -0.13273(14) 0.04155(12) 0.0479(4) Uani 1 1 d . . . H1 H 0.7555 -0.1234 0.0449 0.057 Uiso 1 1 calc R . . C2 C 0.57885(19) -0.10770(16) 0.11895(14) 0.0496(4) Uani 1 1 d . . . H2 H 0.6214 -0.0839 0.1734 0.059 Uiso 1 1 calc R . . C3 C 0.43387(19) -0.11914(14) 0.11299(13) 0.0467(4) Uani 1 1 d . . . C4 C 0.37440(19) -0.14809(16) 0.02878(14) 0.0548(4) Uani 1 1 d . . . H4 H 0.2770 -0.1499 0.0214 0.066 Uiso 1 1 calc R . . C5 C 0.4628(2) -0.17428(16) -0.04415(14) 0.0545(4) Uani 1 1 d . . . H5 H 0.4226 -0.1962 -0.1000 0.065 Uiso 1 1 calc R . . N2 N 0.2805(2) -0.10118(18) 0.26095(15) 0.0715(5) Uani 1 1 d . . . C6 C 0.34739(19) -0.10659(16) 0.19539(15) 0.0554(4) Uani 1 1 d . . . N3 N 0.49771(19) -0.07373(14) -0.38039(11) 0.0569(4) Uani 1 1 d . . . N4 N 0.61221(17) -0.17464(12) -0.25485(10) 0.0510(4) Uani 1 1 d . . . N5 N 0.88266(17) -0.10458(13) -0.13112(12) 0.0519(4) Uani 1 1 d . . . C7 C 0.55625(17) -0.12275(14) -0.31052(12) 0.0442(4) Uani 1 1 d . . . C8 C 0.93898(18) -0.02153(14) -0.12947(12) 0.0449(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn 0.0412(2) 0.0344(2) 0.0441(2) 0.000 0.000 -0.00193(11) N1 0.0443(7) 0.0436(7) 0.0496(8) -0.0022(6) -0.0010(6) -0.0026(5) C1 0.0422(8) 0.0506(9) 0.0508(9) -0.0026(7) -0.0030(7) -0.0023(6) C2 0.0480(9) 0.0505(10) 0.0501(9) -0.0052(7) -0.0034(7) 0.0013(7) C3 0.0471(9) 0.0375(8) 0.0554(10) -0.0016(7) 0.0039(7) 0.0026(6) C4 0.0420(8) 0.0568(10) 0.0656(11) -0.0107(8) -0.0034(7) -0.0011(7) C5 0.0478(9) 0.0593(11) 0.0565(10) -0.0086(8) -0.0054(7) -0.0033(7) N2 0.0619(10) 0.0800(13) 0.0725(12) -0.0113(10) 0.0140(9) 0.0016(9) C6 0.0515(9) 0.0505(10) 0.0640(11) -0.0058(8) 0.0039(8) 0.0034(8) N3 0.0721(11) 0.0533(9) 0.0453(7) -0.0053(7) -0.0046(7) 0.0249(8) N4 0.0543(8) 0.0449(8) 0.0538(8) 0.0007(6) -0.0052(6) 0.0065(6) N5 0.0550(8) 0.0459(8) 0.0547(8) 0.0009(6) 0.0015(7) -0.0124(6) C7 0.0439(8) 0.0405(8) 0.0483(8) -0.0073(7) 0.0007(6) 0.0064(6) C8 0.0470(8) 0.0468(9) 0.0409(8) 0.0002(7) 0.0013(6) -0.0064(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 Mn N4 2.2034(15) . ? Mn N4 2.2034(15) 2_645 ? Mn N5 2.2039(16) 2_645 ? Mn N5 2.2039(16) . ? Mn N1 2.3447(15) 2_645 ? Mn N1 2.3447(15) . ? N1 C5 1.337(2) . ? N1 C1 1.339(2) . ? C1 C2 1.380(3) . ? C2 C3 1.384(3) . ? C3 C4 1.384(3) . ? C3 C6 1.451(3) . ? C4 C5 1.382(3) . ? N2 C6 1.139(3) . ? N3 C7 1.298(2) . ? N3 C8 1.306(2) 3_454 ? N4 C7 1.154(2) . ? N5 C8 1.153(2) . ? C8 N3 1.306(2) 3_554 ? 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 Mn N4 93.28(8) . 2_645 ? N4 Mn N5 95.02(6) . 2_645 ? N4 Mn N5 94.60(6) 2_645 2_645 ? N4 Mn N5 94.60(6) . . ? N4 Mn N5 95.02(6) 2_645 . ? N5 Mn N5 165.97(9) 2_645 . ? N4 Mn N1 179.94(6) . 2_645 ? N4 Mn N1 86.69(6) 2_645 2_645 ? N5 Mn N1 84.94(6) 2_645 2_645 ? N5 Mn N1 85.45(6) . 2_645 ? N4 Mn N1 86.69(6) . . ? N4 Mn N1 179.94(6) 2_645 . ? N5 Mn N1 85.45(6) 2_645 . ? N5 Mn N1 84.94(6) . . ? N1 Mn N1 93.33(8) 2_645 . ? C5 N1 C1 117.23(15) . . ? C5 N1 Mn 121.86(12) . . ? C1 N1 Mn 120.07(11) . . ? N1 C1 C2 123.79(16) . . ? C1 C2 C3 117.95(17) . . ? C4 C3 C2 119.01(17) . . ? C4 C3 C6 120.94(17) . . ? C2 C3 C6 119.97(17) . . ? C5 C4 C3 118.64(17) . . ? N1 C5 C4 123.01(17) . . ? N2 C6 C3 177.1(2) . . ? C7 N3 C8 121.03(16) . 3_454 ? C7 N4 Mn 169.21(15) . . ? C8 N5 Mn 170.51(16) . . ? N4 C7 N3 172.90(18) . . ? N5 C8 N3 174.5(2) . 3_554 ? 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 N4 Mn N1 C5 46.15(15) . . . . ? N4 Mn N1 C5 106(100) 2_645 . . . ? N5 Mn N1 C5 -49.15(15) 2_645 . . . ? N5 Mn N1 C5 141.07(15) . . . . ? N1 Mn N1 C5 -133.80(16) 2_645 . . . ? N4 Mn N1 C1 -144.62(13) . . . . ? N4 Mn N1 C1 -85(100) 2_645 . . . ? N5 Mn N1 C1 120.07(13) 2_645 . . . ? N5 Mn N1 C1 -49.70(13) . . . . ? N1 Mn N1 C1 35.43(11) 2_645 . . . ? C5 N1 C1 C2 5.2(3) . . . . ? Mn N1 C1 C2 -164.51(14) . . . . ? N1 C1 C2 C3 -1.5(3) . . . . ? C1 C2 C3 C4 -4.1(3) . . . . ? C1 C2 C3 C6 172.56(17) . . . . ? C2 C3 C4 C5 5.9(3) . . . . ? C6 C3 C4 C5 -170.76(18) . . . . ? C1 N1 C5 C4 -3.3(3) . . . . ? Mn N1 C5 C4 166.26(15) . . . . ? C3 C4 C5 N1 -2.2(3) . . . . ? C4 C3 C6 N2 92(4) . . . . ? C2 C3 C6 N2 -85(4) . . . . ? N4 Mn N4 C7 -81.4(8) 2_645 . . . ? N5 Mn N4 C7 -176.4(8) 2_645 . . . ? N5 Mn N4 C7 13.9(8) . . . . ? N1 Mn N4 C7 -142(100) 2_645 . . . ? N1 Mn N4 C7 98.5(8) . . . . ? N4 Mn N5 C8 5.6(10) . . . . ? N4 Mn N5 C8 99.3(10) 2_645 . . . ? N5 Mn N5 C8 -127.6(10) 2_645 . . . ? N1 Mn N5 C8 -174.4(10) 2_645 . . . ? N1 Mn N5 C8 -80.7(10) . . . . ? Mn N4 C7 N3 106.7(16) . . . . ? C8 N3 C7 N4 -177.0(15) 3_454 . . . ? Mn N5 C8 N3 105(2) . . . 3_554 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.81 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.431 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.069 ############################ END ##################################### data_Complex_2 _database_code_CSD 190861 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (1,2-bis(4-pyridyl)ethane)-bis(dicyanamide)-manganese(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C12 H12 N2) 2(N3 C2 1-) (Mn 2+)' _chemical_formula_sum 'C16 H12 Mn N8' _chemical_formula_weight 371.28 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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'I2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 13.078(4) _cell_length_b 9.695(3) _cell_length_c 14.592(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.74(2) _cell_angle_gamma 90.00 _cell_volume 1780.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'no colour' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4297 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 29.05 _reflns_number_total 2214 _reflns_number_gt 1712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'Shelxl-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.64.02 (Farrugia, 1999)' _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^)+(0.0634P)^2^+0.5529P] 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 SHELXL _refine_ls_extinction_coef 0.017(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1712 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Mn Mn 0.2500 0.2500 0.7500 0.0601(2) Uani 1 2 d S . . N1 N 0.26204(16) 0.4687(2) 0.69876(13) 0.0690(5) Uani 1 1 d . . . C1 C 0.3552(2) 0.5261(3) 0.70091(19) 0.0809(7) Uani 1 1 d . . . H1 H 0.4167 0.4812 0.7348 0.097 Uiso 1 1 calc R . . C2 C 0.3657(2) 0.6475(3) 0.65606(19) 0.0813(7) Uani 1 1 d . . . H2 H 0.4329 0.6821 0.6595 0.098 Uiso 1 1 calc R . . C3 C 0.2772(2) 0.7177(2) 0.60625(19) 0.0680(6) Uani 1 1 d . . . C4 C 0.1804(2) 0.6624(3) 0.6082(2) 0.0877(8) Uani 1 1 d . . . H4 H 0.1178 0.7085 0.5787 0.105 Uiso 1 1 calc R . . C5 C 0.1768(2) 0.5388(3) 0.6540(2) 0.0844(7) Uani 1 1 d . . . H5 H 0.1106 0.5030 0.6533 0.101 Uiso 1 1 calc R . . C6 C 0.2849(3) 0.8476(2) 0.55122(19) 0.0798(7) Uani 1 1 d . . . H6A H 0.3583 0.8602 0.5505 0.096 Uiso 1 1 calc R . . H6B H 0.2654 0.9257 0.5844 0.096 Uiso 1 1 calc R . . N2 N 0.3735(2) 0.2990(3) 0.88415(14) 0.0784(6) Uani 1 1 d . . . N3 N 0.45068(18) 0.1375(3) 0.54986(13) 0.0794(6) Uani 1 1 d . . . N4 N 0.37471(18) 0.1855(3) 0.68148(14) 0.0741(6) Uani 1 1 d . . . C7 C 0.40537(17) 0.3258(2) 0.96256(15) 0.0595(5) Uani 1 1 d . . . C8 C 0.40691(16) 0.1673(2) 0.61683(14) 0.0576(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn 0.0764(4) 0.0672(4) 0.0404(3) -0.00030(17) 0.0225(2) -0.0018(2) N1 0.0778(12) 0.0697(11) 0.0626(10) 0.0067(9) 0.0245(9) 0.0002(9) C1 0.0765(15) 0.0803(16) 0.0789(15) 0.0120(13) 0.0092(12) -0.0066(12) C2 0.0766(16) 0.0741(15) 0.0892(17) 0.0038(13) 0.0156(14) -0.0136(12) C3 0.0855(16) 0.0528(11) 0.0697(14) -0.0089(10) 0.0280(13) -0.0027(10) C4 0.0804(16) 0.0801(17) 0.109(2) 0.0220(15) 0.0364(15) 0.0179(13) C5 0.0743(15) 0.0856(17) 0.1020(19) 0.0211(15) 0.0390(14) 0.0050(13) C6 0.1048(19) 0.0471(11) 0.0907(17) -0.0083(11) 0.0319(15) -0.0052(11) N2 0.0910(15) 0.0970(15) 0.0471(10) -0.0047(10) 0.0188(10) -0.0084(12) N3 0.0763(13) 0.1153(17) 0.0497(10) 0.0081(10) 0.0225(9) 0.0190(12) N4 0.0847(13) 0.0889(14) 0.0549(10) -0.0040(10) 0.0293(10) 0.0027(11) C7 0.0601(11) 0.0714(13) 0.0505(11) 0.0028(9) 0.0209(9) 0.0060(9) C8 0.0616(12) 0.0642(12) 0.0475(10) 0.0014(8) 0.0157(9) -0.0022(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 Mn N4 2.222(2) 7_556 ? Mn N4 2.222(2) . ? Mn N2 2.225(2) 7_556 ? Mn N2 2.225(2) . ? Mn N1 2.267(2) . ? Mn N1 2.267(2) 7_556 ? N1 C5 1.318(3) . ? N1 C1 1.332(3) . ? C1 C2 1.372(4) . ? C2 C3 1.369(4) . ? C3 C4 1.382(4) . ? C3 C6 1.512(4) . ? C4 C5 1.379(4) . ? C6 C6 1.526(6) 2_556 ? N2 C7 1.137(3) . ? N3 C8 1.292(3) . ? N3 C7 1.300(3) 8_554 ? N4 C8 1.146(3) . ? C7 N3 1.300(3) 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 Mn N4 180.0 7_556 . ? N4 Mn N2 90.54(9) 7_556 7_556 ? N4 Mn N2 89.46(9) . 7_556 ? N4 Mn N2 89.46(9) 7_556 . ? N4 Mn N2 90.54(9) . . ? N2 Mn N2 180.0 7_556 . ? N4 Mn N1 90.59(8) 7_556 . ? N4 Mn N1 89.41(8) . . ? N2 Mn N1 90.47(9) 7_556 . ? N2 Mn N1 89.53(9) . . ? N4 Mn N1 89.41(8) 7_556 7_556 ? N4 Mn N1 90.59(8) . 7_556 ? N2 Mn N1 89.53(9) 7_556 7_556 ? N2 Mn N1 90.47(9) . 7_556 ? N1 Mn N1 180.00(4) . 7_556 ? C5 N1 C1 116.2(2) . . ? C5 N1 Mn 121.37(17) . . ? C1 N1 Mn 121.85(17) . . ? N1 C1 C2 123.8(3) . . ? C3 C2 C1 120.1(3) . . ? C2 C3 C4 116.3(2) . . ? C2 C3 C6 121.8(2) . . ? C4 C3 C6 121.9(3) . . ? C5 C4 C3 120.0(3) . . ? N1 C5 C4 123.6(2) . . ? C3 C6 C6 114.31(19) . 2_556 ? C7 N2 Mn 156.2(2) . . ? C8 N3 C7 120.1(2) . 8_554 ? C8 N4 Mn 153.14(19) . . ? N2 C7 N3 173.7(3) . 8 ? N4 C8 N3 173.6(2) . . ? 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 N4 Mn N1 C5 -49.6(2) 7_556 . . . ? N4 Mn N1 C5 130.4(2) . . . . ? N2 Mn N1 C5 41.0(2) 7_556 . . . ? N2 Mn N1 C5 -139.0(2) . . . . ? N1 Mn N1 C5 129(100) 7_556 . . . ? N4 Mn N1 C1 139.4(2) 7_556 . . . ? N4 Mn N1 C1 -40.6(2) . . . . ? N2 Mn N1 C1 -130.1(2) 7_556 . . . ? N2 Mn N1 C1 49.9(2) . . . . ? N1 Mn N1 C1 -42(100) 7_556 . . . ? C5 N1 C1 C2 -3.3(4) . . . . ? Mn N1 C1 C2 168.2(2) . . . . ? N1 C1 C2 C3 0.7(5) . . . . ? C1 C2 C3 C4 2.8(4) . . . . ? C1 C2 C3 C6 -176.5(2) . . . . ? C2 C3 C4 C5 -3.6(4) . . . . ? C6 C3 C4 C5 175.7(3) . . . . ? C1 N1 C5 C4 2.3(4) . . . . ? Mn N1 C5 C4 -169.2(2) . . . . ? C3 C4 C5 N1 1.1(5) . . . . ? C2 C3 C6 C6 130.1(3) . . . 2_556 ? C4 C3 C6 C6 -49.2(4) . . . 2_556 ? N4 Mn N2 C7 11.7(6) 7_556 . . . ? N4 Mn N2 C7 -168.3(6) . . . . ? N2 Mn N2 C7 -167(100) 7_556 . . . ? N1 Mn N2 C7 102.3(6) . . . . ? N1 Mn N2 C7 -77.7(6) 7_556 . . . ? N4 Mn N4 C8 -4(100) 7_556 . . . ? N2 Mn N4 C8 25.7(5) 7_556 . . . ? N2 Mn N4 C8 -154.3(5) . . . . ? N1 Mn N4 C8 -64.8(5) . . . . ? N1 Mn N4 C8 115.2(5) 7_556 . . . ? Mn N2 C7 N3 -155(2) . . . 8 ? Mn N4 C8 N3 -158(2) . . . . ? C7 N3 C8 N4 168(2) 8_554 . . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 29.05 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.392 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.051 ########################### END ########################