# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 182/1298 data_Mn(N3)2(pyrazine) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H4 Mn N8' _chemical_formula_weight 219.09 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 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 16.3458(17) _cell_length_b 7.3848(5) _cell_length_c 6.8236(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.032(4) _cell_angle_gamma 90.00 _cell_volume 763.53(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200(0.1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Thin plate' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 1.690 _exptl_absorpt_correction_type SCALEPACK _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(0.1) _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 Diffractometer' _diffrn_measurement_method 'Phi plus OMega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1230 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 31.95 _reflns_number_total 1230 _reflns_number_gt 928 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN' _computing_data_reduction 'DENZO-SMN' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _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^)+(0.1355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 1230 _refine_ls_number_parameters 118 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1823 _refine_ls_wR_factor_gt 0.1659 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.6812(2) -0.00364(6) 0.2467(5) 0.0164(3) Uani 1 1 d . . . N1 N 0.7792(9) -0.0050(8) 0.083(2) 0.021(2) Uani 1 1 d . . . N2 N 0.8479(7) 0.0376(13) 0.1560(18) 0.037(3) Uani 1 1 d . . . N3 N 0.9229(10) 0.0870(13) 0.232(3) 0.053(3) Uani 1 1 d . . . N4 N 0.5887(9) -0.0005(8) 0.4118(19) 0.019(2) Uani 1 1 d . . . N5 N 0.5087(6) 0.0389(12) 0.3334(15) 0.0250(16) Uani 1 1 d . . . N6 N 0.4366(10) 0.073(2) 0.262(3) 0.080(4) Uani 1 1 d . . . N7 N 0.6820(9) 0.3077(5) 0.251(2) 0.0185(8) Uani 1 1 d . . . N8 N 0.6838(9) 0.6853(5) 0.251(3) 0.0183(9) Uani 1 1 d . . . C1 C 0.7578(5) 0.4020(15) 0.3447(13) 0.0166(17) Uani 1 1 d . . . H1 H 0.8118 0.3386 0.4110 0.020 Uiso 1 1 calc R . . C2 C 0.7576(5) 0.5930(13) 0.3450(13) 0.0151(16) Uani 1 1 d . . . H2 H 0.8114 0.6565 0.4136 0.018 Uiso 1 1 calc R . . C3 C 0.6094(8) 0.584(2) 0.1468(18) 0.032(3) Uani 1 1 d . . . H3 H 0.5554 0.6445 0.0722 0.038 Uiso 1 1 calc R . . C4 C 0.6102(7) 0.402(2) 0.1465(18) 0.028(2) Uani 1 1 d . . . H4 H 0.5573 0.3387 0.0683 0.034 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 Mn 0.0175(4) 0.0151(4) 0.0166(4) -0.0002(6) 0.0063(2) -0.0006(5) N1 0.014(4) 0.023(6) 0.024(5) 0.005(2) 0.003(3) 0.000(2) N2 0.050(7) 0.033(4) 0.033(5) 0.006(4) 0.020(4) 0.018(5) N3 0.027(5) 0.055(6) 0.063(7) -0.006(4) 0.003(4) -0.018(4) N4 0.021(5) 0.026(6) 0.012(4) 0.0048(19) 0.008(3) 0.0024(19) N5 0.007(3) 0.050(4) 0.017(3) 0.003(4) 0.003(2) 0.011(3) N6 0.022(5) 0.174(12) 0.040(7) 0.004(8) 0.008(4) 0.010(7) N7 0.0234(16) 0.0153(17) 0.0157(16) -0.003(4) 0.0059(13) 0.008(4) N8 0.0198(17) 0.0176(18) 0.0187(17) 0.005(4) 0.0084(14) -0.007(4) C1 0.015(3) 0.011(4) 0.020(4) -0.003(3) 0.003(3) -0.009(3) C2 0.016(4) 0.004(3) 0.024(4) -0.002(3) 0.006(3) 0.003(2) C3 0.019(4) 0.047(7) 0.027(5) 0.003(5) 0.006(4) 0.012(4) C4 0.021(4) 0.033(5) 0.028(5) -0.005(5) 0.006(4) -0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn N4 2.198(12) . ? Mn N4 2.217(12) 2_554 ? Mn N1 2.255(14) 2 ? Mn N1 2.270(14) . ? Mn N8 2.298(4) 1_545 ? Mn N7 2.299(4) . ? N1 N2 1.091(18) . ? N1 Mn 2.255(14) 2_554 ? N2 N3 1.195(16) . ? N4 N5 1.248(17) . ? N4 Mn 2.217(12) 2 ? N5 N6 1.123(13) . ? N7 C4 1.32(2) . ? N7 C1 1.355(17) . ? N8 C2 1.323(17) . ? N8 C3 1.38(2) . ? N8 Mn 2.298(4) 1_565 ? C1 C2 1.411(19) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 C4 1.34(3) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? 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 101.2(5) . 2_554 ? N4 Mn N1 80.8(4) . 2 ? N4 Mn N1 176.8(4) 2_554 2 ? N4 Mn N1 178.7(6) . . ? N4 Mn N1 80.1(4) 2_554 . ? N1 Mn N1 97.9(5) 2 . ? N4 Mn N8 91.0(4) . 1_545 ? N4 Mn N8 91.7(4) 2_554 1_545 ? N1 Mn N8 90.7(4) 2 1_545 ? N1 Mn N8 89.4(4) . 1_545 ? N4 Mn N7 89.1(4) . . ? N4 Mn N7 89.9(4) 2_554 . ? N1 Mn N7 87.7(4) 2 . ? N1 Mn N7 90.6(4) . . ? N8 Mn N7 178.4(7) 1_545 . ? N2 N1 Mn 132.3(12) . 2_554 ? N2 N1 Mn 124.8(12) . . ? Mn N1 Mn 97.9(5) 2_554 . ? N1 N2 N3 178.5(14) . . ? N5 N4 Mn 126.5(9) . . ? N5 N4 Mn 129.7(10) . 2 ? Mn N4 Mn 101.2(5) . 2 ? N6 N5 N4 179.4(13) . . ? C4 N7 C1 117.1(5) . . ? C4 N7 Mn 121.3(9) . . ? C1 N7 Mn 121.3(8) . . ? C2 N8 C3 115.9(5) . . ? C2 N8 Mn 122.0(8) . 1_565 ? C3 N8 Mn 121.9(8) . 1_565 ? N7 C1 C2 120.9(7) . . ? N7 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? N8 C2 C1 121.1(7) . . ? N8 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 N8 122.6(8) . . ? C4 C3 H3 118.7 . . ? N8 C3 H3 118.7 . . ? N7 C4 C3 122.2(8) . . ? N7 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? 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 N2 -5(9) . . . . ? N4 Mn N1 N2 158.4(8) 2_554 . . . ? N1 Mn N1 N2 -19.2(8) 2 . . . ? N8 Mn N1 N2 -109.8(10) 1_545 . . . ? N7 Mn N1 N2 68.6(9) . . . . ? N4 Mn N1 Mn -163(8) . . . 2_554 ? N4 Mn N1 Mn 0.8(3) 2_554 . . 2_554 ? N1 Mn N1 Mn -176.7(3) 2 . . 2_554 ? N8 Mn N1 Mn 92.7(4) 1_545 . . 2_554 ? N7 Mn N1 Mn -89.0(4) . . . 2_554 ? Mn N1 N2 N3 22(52) 2_554 . . . ? Mn N1 N2 N3 -127(52) . . . . ? N4 Mn N4 N5 -15.4(7) 2_554 . . . ? N1 Mn N4 N5 162.1(7) 2 . . . ? N1 Mn N4 N5 148(9) . . . . ? N8 Mn N4 N5 -107.4(9) 1_545 . . . ? N7 Mn N4 N5 74.3(8) . . . . ? N4 Mn N4 Mn -178.4(3) 2_554 . . 2 ? N1 Mn N4 Mn -0.9(3) 2 . . 2 ? N1 Mn N4 Mn -15(8) . . . 2 ? N8 Mn N4 Mn 89.7(4) 1_545 . . 2 ? N7 Mn N4 Mn -88.7(4) . . . 2 ? Mn N4 N5 N6 58(100) . . . . ? Mn N4 N5 N6 -144(100) 2 . . . ? N4 Mn N7 C4 -64.9(12) . . . . ? N4 Mn N7 C4 36.3(13) 2_554 . . . ? N1 Mn N7 C4 -145.7(13) 2 . . . ? N1 Mn N7 C4 116.4(13) . . . . ? N8 Mn N7 C4 -157(21) 1_545 . . . ? N4 Mn N7 C1 121.4(12) . . . . ? N4 Mn N7 C1 -137.4(12) 2_554 . . . ? N1 Mn N7 C1 40.6(12) 2 . . . ? N1 Mn N7 C1 -57.3(12) . . . . ? N8 Mn N7 C1 29(23) 1_545 . . . ? C4 N7 C1 C2 5(2) . . . . ? Mn N7 C1 C2 179.4(6) . . . . ? C3 N8 C2 C1 -2.9(19) . . . . ? Mn N8 C2 C1 -179.6(6) 1_565 . . . ? N7 C1 C2 N8 -1.1(11) . . . . ? C2 N8 C3 C4 3(2) . . . . ? Mn N8 C3 C4 179.4(7) 1_565 . . . ? C1 N7 C4 C3 -6(2) . . . . ? Mn N7 C4 C3 -179.8(7) . . . . ? N8 C3 C4 N7 1.9(13) . . . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 31.95 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 3.935 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.214