Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Abu-Youssef, Morsy A. M.' 'Escuer, Albert' 'Goher, Mohamed A. S.' 'Mautner, Franz A.' 'Vicente, Ramon' _publ_contact_author_name 'Dr Albert Escuer' _publ_contact_author_address ; Dr Albert Escuer Inorganic Chemistry University of Barcelona Martí Franqués 1-11 Barcelona Barcelona 08028 SPAIN ; _publ_contact_author_email 'ALBERT.ESCUER@QI.UB.ES' _publ_section_title ; [M (N3)2 (L)]n : building 3-D MII-azido networks with new topologies ; data_mnpydz _database_code_CSD 172083 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Mn2(pyridazine)2(N3)4]n' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H8 Mn2 N16' _chemical_formula_weight 438.18 _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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 14.620(4) _cell_length_b 8.551(2) _cell_length_c 13.214(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1652.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature -185(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 15.6 _exptl_crystal_description irregular _exptl_crystal_colour 'transparent yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method ? _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 1.562 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature -185(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: 1.00 deg.' _diffrn_standards_number '2 (2 0 0; 0 0 -2)' _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '80 min' _diffrn_standards_decay_% 3 _diffrn_reflns_number 2633 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 29.70 _reflns_number_total 2459 _reflns_number_observed 2132 _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 20 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^)+(0.0398P)^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 noref _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 0.01(4) _refine_ls_number_reflns 2439 _refine_ls_number_parameters 235 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_obs 0.0477 _refine_ls_wR_factor_all 0.2340 _refine_ls_wR_factor_obs 0.0995 _refine_ls_goodness_of_fit_all 1.076 _refine_ls_goodness_of_fit_obs 1.086 _refine_ls_restrained_S_all 2.363 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max 0.000 _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 0.35449(5) 0.04355(9) 0.73628(7) 0.0091(2) Uani 1 d . . Mn2 Mn 0.24315(5) -0.31930(9) 0.80301(7) 0.0100(2) Uani 1 d . . N41 N 0.3347(4) -0.1368(6) 0.8518(4) 0.0157(11) Uani 1 d . . N42 N 0.3767(3) -0.1233(6) 0.9285(4) 0.0156(11) Uani 1 d . . N43 N 0.4162(5) -0.1083(8) 1.0023(4) 0.032(2) Uani 1 d . . N31 N 0.3328(4) -0.5009(6) 0.8572(5) 0.0211(12) Uani 1 d . . N32 N 0.3284(3) -0.6387(6) 0.8508(4) 0.0147(10) Uani 1 d . . N33 N 0.3258(4) -0.7751(6) 0.8480(4) 0.0194(12) Uani 1 d . . N21 N 0.3568(4) 0.2074(6) 0.6111(4) 0.0164(11) Uani 1 d . . N22 N 0.1489(3) -0.3034(6) 1.0223(4) 0.0146(10) Uani 1 d . . N23 N 0.1512(4) -0.3115(7) 0.9342(4) 0.0238(13) Uani 1 d . . N11 N 0.5013(3) 0.0546(6) 0.7619(4) 0.0187(11) Uani 1 d . . N12 N 0.5758(3) 0.0201(5) 0.7469(5) 0.0123(9) Uani 1 d . . N13 N 0.1531(3) -0.4890(5) 0.7307(6) 0.0203(11) Uani 1 d . . N1 N 0.3683(3) -0.1671(6) 0.6261(4) 0.0112(10) Uani 1 d . . N2 N 0.3110(3) -0.2894(6) 0.6404(4) 0.0110(9) Uani 1 d . . C1 C 0.3004(4) -0.3957(7) 0.5696(5) 0.0171(12) Uani 1 d . . H1 H 0.2580(4) -0.4752(7) 0.5795(5) 0.021 Uiso 1 calc R . C2 C 0.3513(5) -0.3930(8) 0.4789(5) 0.0204(13) Uani 1 d . . H2 H 0.3438(5) -0.4705(8) 0.4302(5) 0.024 Uiso 1 calc R . C3 C 0.4116(5) -0.2742(7) 0.4649(5) 0.0189(13) Uani 1 d . . H3 H 0.4476(5) -0.2683(7) 0.4070(5) 0.023 Uiso 1 calc R . C4 C 0.4174(4) -0.1611(7) 0.5410(5) 0.0160(12) Uani 1 d . . H4 H 0.4573(4) -0.0777(7) 0.5319(5) 0.019 Uiso 1 calc R . N3 N 0.1541(3) -0.1159(5) 0.7454(5) 0.0120(9) Uani 1 d . . N4 N 0.1972(3) 0.0099(5) 0.7056(4) 0.0103(9) Uani 1 d . . C5 C 0.1493(4) 0.1209(7) 0.6625(5) 0.0141(11) Uani 1 d . . H5 H 0.1802(4) 0.2051(7) 0.6339(5) 0.017 Uiso 1 calc R . C6 C 0.0530(4) 0.1185(7) 0.6574(5) 0.0176(12) Uani 1 d . . H6 H 0.0202(4) 0.1979(7) 0.6258(5) 0.021 Uiso 1 calc R . C7 C 0.0102(4) -0.0066(7) 0.7014(5) 0.0188(12) Uani 1 d . . H7 H -0.0533(4) -0.0132(7) 0.7029(5) 0.023 Uiso 1 calc R . C8 C 0.0637(4) -0.1226(6) 0.7436(6) 0.0164(11) Uani 1 d . . H8 H 0.0350(4) -0.2092(6) 0.7719(6) 0.020 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0099(3) 0.0088(3) 0.0086(3) 0.0017(4) -0.0017(4) -0.0002(3) Mn2 0.0124(4) 0.0092(3) 0.0084(3) 0.0002(4) 0.0010(4) -0.0006(3) N41 0.021(3) 0.018(3) 0.008(2) -0.001(2) -0.001(2) -0.004(2) N42 0.013(2) 0.017(3) 0.017(2) 0.007(2) -0.001(2) -0.006(2) N43 0.044(4) 0.041(4) 0.013(3) 0.010(3) -0.014(3) -0.019(3) N31 0.023(3) 0.014(2) 0.026(3) -0.003(2) -0.005(3) 0.001(2) N32 0.015(2) 0.020(2) 0.009(2) 0.003(2) -0.001(2) 0.003(2) N33 0.029(3) 0.013(2) 0.016(3) -0.001(2) 0.010(2) 0.005(2) N21 0.017(2) 0.016(3) 0.016(3) 0.006(2) -0.001(2) -0.006(2) N22 0.014(2) 0.014(2) 0.016(2) 0.004(2) 0.008(2) 0.000(2) N23 0.030(3) 0.029(3) 0.013(3) 0.007(2) 0.009(2) 0.003(3) N11 0.015(2) 0.019(2) 0.021(3) -0.002(2) 0.000(2) -0.001(2) N12 0.017(2) 0.009(2) 0.012(2) -0.001(2) -0.003(2) 0.001(2) N13 0.022(2) 0.017(2) 0.021(3) -0.005(3) 0.005(3) -0.005(2) N1 0.009(2) 0.013(2) 0.011(2) 0.001(2) 0.000(2) -0.002(2) N2 0.010(2) 0.013(2) 0.010(2) -0.003(2) 0.000(2) -0.002(2) C1 0.015(3) 0.017(3) 0.020(3) -0.002(3) -0.002(2) -0.003(2) C2 0.029(3) 0.021(3) 0.011(3) 0.002(3) 0.003(3) -0.001(3) C3 0.026(3) 0.020(3) 0.011(3) 0.003(3) 0.008(3) -0.001(3) C4 0.017(3) 0.017(3) 0.014(3) 0.002(2) 0.004(2) -0.005(2) N3 0.015(2) 0.010(2) 0.011(2) -0.001(2) 0.000(2) 0.002(2) N4 0.010(2) 0.009(2) 0.012(2) 0.000(2) -0.004(2) -0.002(2) C5 0.012(2) 0.015(3) 0.015(3) 0.001(2) 0.000(2) 0.002(2) C6 0.016(3) 0.021(3) 0.017(3) 0.000(3) -0.003(3) 0.005(2) C7 0.014(3) 0.024(3) 0.018(3) -0.006(3) -0.003(2) -0.003(2) C8 0.014(2) 0.015(2) 0.020(3) 0.004(3) 0.006(3) -0.003(2) _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 N21 2.168(5) . yes Mn1 N11 2.174(5) . yes Mn1 N33 2.182(6) 1_565 yes Mn1 N41 2.189(6) . yes Mn1 N1 2.325(5) . yes Mn1 N4 2.353(4) . yes Mn2 N31 2.154(5) . yes Mn2 N41 2.155(5) . yes Mn2 N13 2.180(5) . yes Mn2 N23 2.195(5) . yes Mn2 N3 2.302(4) . yes Mn2 N2 2.380(5) . yes N41 N42 1.190(8) . yes N42 N43 1.142(8) . yes N31 N32 1.183(7) . yes N32 N33 1.167(7) . yes N33 Mn1 2.182(6) 1_545 yes N21 N22 1.180(8) 3_554 yes N22 N23 1.167(8) . yes N22 N21 1.180(8) 3_545 yes N11 N12 1.146(6) . yes N12 N13 1.181(6) 4_545 yes N13 N12 1.181(6) 4_445 yes N1 C4 1.334(8) . ? N1 N2 1.354(7) . ? N2 C1 1.314(8) . ? C1 C2 1.410(9) . ? C1 H1 0.93 . ? C2 C3 1.358(9) . ? C2 H2 0.93 . ? C3 C4 1.397(9) . ? C3 H3 0.93 . ? C4 H4 0.93 . ? N3 C8 1.323(7) . ? N3 N4 1.353(6) . ? N4 C5 1.310(7) . ? C5 C6 1.410(8) . ? C5 H5 0.93 . ? C6 C7 1.369(9) . ? C6 H6 0.93 . ? C7 C8 1.381(9) . ? C7 H7 0.93 . ? C8 H8 0.93 . ? Mn1 Mn2 3.613(1) . yes Mn1 Mn2 5.754(2) 1_565 yes Mn1 Mn2 6.016(2) 3_554 yes Mn1 Mn2 6.062(2) 4_545 yes Mn1 Mn2 7.713(2) 3_555 ? 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 N21 Mn1 N11 94.3(2) . . yes N21 Mn1 N33 93.4(2) . 1_565 yes N11 Mn1 N33 93.1(2) . 1_565 yes N21 Mn1 N41 171.6(2) . . yes N11 Mn1 N41 93.0(2) . . yes N33 Mn1 N41 90.2(2) 1_565 . yes N21 Mn1 N1 91.2(2) . . yes N11 Mn1 N1 92.6(2) . . yes N33 Mn1 N1 172.4(2) 1_565 . yes N41 Mn1 N1 84.4(2) . . yes N21 Mn1 N4 87.9(2) . . yes N11 Mn1 N4 175.4(2) . . yes N33 Mn1 N4 90.9(2) 1_565 . yes N41 Mn1 N4 84.5(2) . . yes N1 Mn1 N4 83.2(2) . . yes N31 Mn2 N41 92.6(2) . . yes N31 Mn2 N13 91.9(2) . . yes N41 Mn2 N13 171.3(2) . . yes N31 Mn2 N23 97.6(2) . . yes N41 Mn2 N23 97.0(2) . . yes N13 Mn2 N23 89.8(2) . . yes N31 Mn2 N3 176.8(2) . . yes N41 Mn2 N3 84.4(2) . . yes N13 Mn2 N3 91.0(2) . . yes N23 Mn2 N3 83.8(2) . . yes N31 Mn2 N2 97.1(2) . . yes N41 Mn2 N2 86.2(2) . . yes N13 Mn2 N2 85.8(2) . . yes N23 Mn2 N2 164.8(2) . . yes N3 Mn2 N2 81.7(2) . . yes N42 N41 Mn2 130.2(4) . . yes N42 N41 Mn1 117.2(4) . . yes Mn2 N41 Mn1 112.6(2) . . yes N43 N42 N41 179.0(7) . . yes N32 N31 Mn2 131.4(5) . . yes N33 N32 N31 177.4(7) . . yes N32 N33 Mn1 136.5(5) . 1_545 yes N22 N21 Mn1 135.0(5) 3_554 . yes N23 N22 N21 177.3(7) . 3_545 yes N22 N23 Mn2 143.8(5) . . yes N12 N11 Mn1 154.2(5) . . yes N11 N12 N13 178.0(6) . 4_545 yes N12 N13 Mn2 130.4(5) 4_445 . yes C4 N1 N2 118.7(5) . . ? C4 N1 Mn1 123.0(4) . . ? N2 N1 Mn1 117.2(4) . . ? C1 N2 N1 120.5(5) . . ? C1 N2 Mn2 121.4(4) . . ? N1 N2 Mn2 117.9(4) . . ? N2 C1 C2 122.2(6) . . ? N2 C1 H1 118.9(3) . . ? C2 C1 H1 118.9(4) . . ? C3 C2 C1 118.0(6) . . ? C3 C2 H2 121.0(4) . . ? C1 C2 H2 121.0(4) . . ? C2 C3 C4 117.3(6) . . ? C2 C3 H3 121.4(4) . . ? C4 C3 H3 121.4(4) . . ? N1 C4 C3 123.2(5) . . ? N1 C4 H4 118.4(3) . . ? C3 C4 H4 118.4(4) . . ? C8 N3 N4 119.5(5) . . ? C8 N3 Mn2 122.6(4) . . ? N4 N3 Mn2 117.8(3) . . ? C5 N4 N3 119.8(5) . . ? C5 N4 Mn1 120.6(4) . . ? N3 N4 Mn1 119.0(3) . . ? N4 C5 C6 122.9(6) . . ? N4 C5 H5 118.5(3) . . ? C6 C5 H5 118.5(4) . . ? C7 C6 C5 116.6(6) . . ? C7 C6 H6 121.7(4) . . ? C5 C6 H6 121.7(4) . . ? C6 C7 C8 118.3(5) . . ? C6 C7 H7 120.8(4) . . ? C8 C7 H7 120.8(3) . . ? N3 C8 C7 122.8(5) . . ? N3 C8 H8 118.6(3) . . ? C7 C8 H8 118.6(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 N31 Mn2 N41 N42 -43.3(6) . . . . ? N13 Mn2 N41 N42 -164.2(11) . . . . ? N23 Mn2 N41 N42 54.7(6) . . . . ? N3 Mn2 N41 N42 137.7(6) . . . . ? N2 Mn2 N41 N42 -140.2(6) . . . . ? N31 Mn2 N41 Mn1 134.1(3) . . . . ? N13 Mn2 N41 Mn1 13.2(15) . . . . ? N23 Mn2 N41 Mn1 -127.9(3) . . . . ? N3 Mn2 N41 Mn1 -44.9(3) . . . . ? N2 Mn2 N41 Mn1 37.1(2) . . . . ? N21 Mn1 N41 N42 -167.7(13) . . . . ? N11 Mn1 N41 N42 41.0(5) . . . . ? N33 Mn1 N41 N42 -52.0(5) 1_565 . . . ? N1 Mn1 N41 N42 133.4(5) . . . . ? N4 Mn1 N41 N42 -142.9(5) . . . . ? N21 Mn1 N41 Mn2 14.6(16) . . . . ? N11 Mn1 N41 Mn2 -136.7(3) . . . . ? N33 Mn1 N41 Mn2 130.3(3) 1_565 . . . ? N1 Mn1 N41 Mn2 -44.3(3) . . . . ? N4 Mn1 N41 Mn2 39.4(2) . . . . ? Mn2 N41 N42 N43 -117.5(355) . . . . ? Mn1 N41 N42 N43 65.2(358) . . . . ? N41 Mn2 N31 N32 -175.2(7) . . . . ? N13 Mn2 N31 N32 -2.7(7) . . . . ? N23 Mn2 N31 N32 87.4(7) . . . . ? N3 Mn2 N31 N32 -157.1(37) . . . . ? N2 Mn2 N31 N32 -88.7(7) . . . . ? Mn2 N31 N32 N33 -150.4(142) . . . . ? N31 N32 N33 Mn1 -132.0(142) . . . 1_545 ? N11 Mn1 N21 N22 104.3(7) . . . 3_554 ? N33 Mn1 N21 N22 -162.3(6) 1_565 . . 3_554 ? N41 Mn1 N21 N22 -46.9(18) . . . 3_554 ? N1 Mn1 N21 N22 11.6(7) . . . 3_554 ? N4 Mn1 N21 N22 -71.6(7) . . . 3_554 ? N21 N22 N23 Mn2 154.1(148) 3_545 . . . ? N31 Mn2 N23 N22 49.8(9) . . . . ? N41 Mn2 N23 N22 -43.8(9) . . . . ? N13 Mn2 N23 N22 141.7(9) . . . . ? N3 Mn2 N23 N22 -127.4(9) . . . . ? N2 Mn2 N23 N22 -145.2(8) . . . . ? N21 Mn1 N11 N12 -83.7(11) . . . . ? N33 Mn1 N11 N12 -177.3(11) 1_565 . . . ? N41 Mn1 N11 N12 92.3(11) . . . . ? N1 Mn1 N11 N12 7.8(11) . . . . ? N4 Mn1 N11 N12 34.3(32) . . . . ? Mn1 N11 N12 N13 119.1(207) . . . 4_545 ? N31 Mn2 N13 N12 116.4(7) . . . 4_445 ? N41 Mn2 N13 N12 -122.6(13) . . . 4_445 ? N23 Mn2 N13 N12 18.8(7) . . . 4_445 ? N3 Mn2 N13 N12 -64.9(7) . . . 4_445 ? N2 Mn2 N13 N12 -146.6(7) . . . 4_445 ? N21 Mn1 N1 C4 34.9(5) . . . . ? N11 Mn1 N1 C4 -59.5(5) . . . . ? N33 Mn1 N1 C4 162.6(14) 1_565 . . . ? N41 Mn1 N1 C4 -152.2(5) . . . . ? N4 Mn1 N1 C4 122.6(5) . . . . ? N21 Mn1 N1 N2 -133.0(4) . . . . ? N11 Mn1 N1 N2 132.6(4) . . . . ? N33 Mn1 N1 N2 -5.3(17) 1_565 . . . ? N41 Mn1 N1 N2 39.9(4) . . . . ? N4 Mn1 N1 N2 -45.3(4) . . . . ? C4 N1 N2 C1 -3.5(8) . . . . ? Mn1 N1 N2 C1 164.9(4) . . . . ? C4 N1 N2 Mn2 170.2(4) . . . . ? Mn1 N1 N2 Mn2 -21.4(5) . . . . ? N31 Mn2 N2 C1 72.5(5) . . . . ? N41 Mn2 N2 C1 164.6(5) . . . . ? N13 Mn2 N2 C1 -18.9(5) . . . . ? N23 Mn2 N2 C1 -92.5(9) . . . . ? N3 Mn2 N2 C1 -110.5(5) . . . . ? N31 Mn2 N2 N1 -101.1(4) . . . . ? N41 Mn2 N2 N1 -9.0(4) . . . . ? N13 Mn2 N2 N1 167.5(4) . . . . ? N23 Mn2 N2 N1 93.9(8) . . . . ? N3 Mn2 N2 N1 75.9(4) . . . . ? N1 N2 C1 C2 3.8(9) . . . . ? Mn2 N2 C1 C2 -169.7(5) . . . . ? N2 C1 C2 C3 -1.3(10) . . . . ? C1 C2 C3 C4 -1.2(10) . . . . ? N2 N1 C4 C3 0.9(9) . . . . ? Mn1 N1 C4 C3 -166.8(5) . . . . ? C2 C3 C4 N1 1.4(10) . . . . ? N31 Mn2 N3 C8 -166.0(38) . . . . ? N41 Mn2 N3 C8 -147.8(6) . . . . ? N13 Mn2 N3 C8 39.6(6) . . . . ? N23 Mn2 N3 C8 -50.1(6) . . . . ? N2 Mn2 N3 C8 125.3(6) . . . . ? N31 Mn2 N3 N4 18.8(43) . . . . ? N41 Mn2 N3 N4 37.0(5) . . . . ? N13 Mn2 N3 N4 -135.6(5) . . . . ? N23 Mn2 N3 N4 134.8(5) . . . . ? N2 Mn2 N3 N4 -49.9(4) . . . . ? C8 N3 N4 C5 -2.4(9) . . . . ? Mn2 N3 N4 C5 172.9(4) . . . . ? C8 N3 N4 Mn1 168.6(5) . . . . ? Mn2 N3 N4 Mn1 -16.1(6) . . . . ? N21 Mn1 N4 C5 -26.0(5) . . . . ? N11 Mn1 N4 C5 -144.2(23) . . . . ? N33 Mn1 N4 C5 67.3(5) 1_565 . . . ? N41 Mn1 N4 C5 157.5(5) . . . . ? N1 Mn1 N4 C5 -117.6(5) . . . . ? N21 Mn1 N4 N3 163.1(4) . . . . ? N11 Mn1 N4 N3 44.9(27) . . . . ? N33 Mn1 N4 N3 -103.5(4) 1_565 . . . ? N41 Mn1 N4 N3 -13.4(4) . . . . ? N1 Mn1 N4 N3 71.6(4) . . . . ? N3 N4 C5 C6 1.7(9) . . . . ? Mn1 N4 C5 C6 -169.1(5) . . . . ? N4 C5 C6 C7 0.8(10) . . . . ? C5 C6 C7 C8 -2.4(9) . . . . ? N4 N3 C8 C7 0.7(11) . . . . ? Mn2 N3 C8 C7 -174.4(5) . . . . ? C6 C7 C8 N3 1.8(11) . . . . ? _refine_diff_density_max 0.667 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.123 data_mnpymx _database_code_CSD 172084 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Mn(pyrimidine)(N3)2]n' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H4 Mn N8' _chemical_formula_weight 219.09 _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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 7.647(3) _cell_length_b 12.300(4) _cell_length_c 8.734(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.47(3) _cell_angle_gamma 90.00 _cell_volume 821.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 14.2 _exptl_crystal_description prism _exptl_crystal_colour 'transparent green' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method ? _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 1.571 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.336 _exptl_absorpt_correction_T_max 1.000 _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: 1.10 deg.' _diffrn_standards_number '3 (-1 0 -1; -1 -1 -2; 0 0 -4)' _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '1 h' _diffrn_standards_decay_% 28 _diffrn_reflns_number 1169 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 26.48 _reflns_number_total 901 _reflns_number_observed 761 _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 4 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^)+(0.0668P)^2^+1.8411P] 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 897 _refine_ls_number_parameters 66 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_obs 0.0501 _refine_ls_wR_factor_all 0.1401 _refine_ls_wR_factor_obs 0.1279 _refine_ls_goodness_of_fit_all 1.066 _refine_ls_goodness_of_fit_obs 1.075 _refine_ls_restrained_S_all 1.076 _refine_ls_restrained_S_obs 1.075 _refine_ls_shift/esd_max 0.000 _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 0.2500 0.2500 0.7500 0.0387(3) Uani 1 d S . N1 N 0.0799(4) 0.0958(3) 0.7558(4) 0.0452(8) Uani 1 d . . C1 C -0.0948(5) 0.0945(3) 0.7628(5) 0.0529(10) Uani 1 d . . H1 H -0.1549(5) 0.1602(3) 0.7655(5) 0.063 Uiso 1 calc R . C2 C -0.1869(8) 0.0000 0.7662(9) 0.060(2) Uani 1 d S . H2 H -0.3083(8) 0.0000 0.7706(9) 0.072 Uiso 1 calc SR . C3 C 0.1567(7) 0.0000 0.7521(7) 0.0469(13) Uani 1 d S . H3 H 0.2780(7) 0.0000 0.7461(7) 0.056 Uiso 1 calc SR . N2 N 0.1471(5) 0.3097(4) 0.9671(4) 0.0597(10) Uani 1 d . . N3 N 0.0000 0.3092(4) 1.0000 0.0476(11) Uani 1 d S . N4 N 0.0350(4) 0.3368(3) 0.6313(4) 0.0529(9) Uani 1 d . . N5 N 0.0000 0.3366(4) 0.5000 0.0453(10) Uani 1 d S . 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 0.0389(5) 0.0383(5) 0.0389(5) 0.0004(3) 0.0005(3) -0.0001(3) N1 0.042(2) 0.038(2) 0.056(2) 0.0001(14) 0.0010(13) 0.0008(13) C1 0.045(2) 0.041(2) 0.073(3) -0.002(2) 0.001(2) 0.003(2) C2 0.035(3) 0.050(3) 0.094(5) 0.000 0.004(3) 0.000 C3 0.038(3) 0.043(3) 0.059(3) 0.000 0.003(2) 0.000 N2 0.054(2) 0.078(3) 0.047(2) -0.011(2) 0.007(2) -0.002(2) N3 0.059(3) 0.045(3) 0.039(2) 0.000 -0.001(2) 0.000 N4 0.050(2) 0.055(2) 0.053(2) -0.003(2) -0.0103(15) 0.008(2) N5 0.037(2) 0.042(2) 0.056(3) 0.000 -0.006(2) 0.000 _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 2.198(4) 7_556 yes Mn1 N2 2.198(4) . yes Mn1 N4 2.198(3) 7_556 yes Mn1 N4 2.198(3) . yes Mn1 N1 2.301(3) . yes Mn1 N1 2.301(3) 7_556 yes N1 C3 1.318(4) . yes N1 C1 1.339(5) . yes C1 C2 1.360(5) . yes C1 H1 0.93 . ? C2 C1 1.360(5) 6 yes C2 H2 0.93 . ? C3 N1 1.318(4) 6 yes C3 H3 0.93 . ? N2 N3 1.168(4) . yes N3 N2 1.168(4) 2_557 yes N4 N5 1.171(4) . yes N5 N4 1.171(4) 2_556 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 N2 Mn1 N2 180.0 7_556 . yes N2 Mn1 N4 87.97(14) 7_556 7_556 yes N2 Mn1 N4 92.03(14) . 7_556 yes N2 Mn1 N4 92.03(14) 7_556 . yes N2 Mn1 N4 87.97(14) . . yes N4 Mn1 N4 180.0 7_556 . yes N2 Mn1 N1 87.65(13) 7_556 . yes N2 Mn1 N1 92.35(13) . . yes N4 Mn1 N1 90.32(13) 7_556 . yes N4 Mn1 N1 89.68(13) . . yes N2 Mn1 N1 92.35(13) 7_556 7_556 yes N2 Mn1 N1 87.65(13) . 7_556 yes N4 Mn1 N1 89.68(13) 7_556 7_556 yes N4 Mn1 N1 90.32(13) . 7_556 yes N1 Mn1 N1 180.0 . 7_556 yes C3 N1 C1 115.9(4) . . ? C3 N1 Mn1 118.9(3) . . ? C1 N1 Mn1 125.2(3) . . ? N1 C1 C2 122.0(4) . . ? N1 C1 H1 119.0(2) . . ? C2 C1 H1 119.0(3) . . ? C1 C2 C1 117.5(5) . 6 ? C1 C2 H2 121.3(3) . . ? C1 C2 H2 121.3(3) 6 . ? N1 C3 N1 126.9(5) 6 . ? N1 C3 H3 116.6(2) 6 . ? N1 C3 H3 116.6(2) . . ? N3 N2 Mn1 125.4(3) . . yes N2 N3 N2 179.5(7) 2_557 . yes N5 N4 Mn1 127.6(3) . . yes N4 N5 N4 179.7(6) . 2_556 yes 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 N2 Mn1 N1 C3 57.5(4) 7_556 . . . ? N2 Mn1 N1 C3 -122.5(4) . . . . ? N4 Mn1 N1 C3 -30.5(4) 7_556 . . . ? N4 Mn1 N1 C3 149.5(4) . . . . ? N1 Mn1 N1 C3 -5.6(1000) 7_556 . . . ? N2 Mn1 N1 C1 -122.5(4) 7_556 . . . ? N2 Mn1 N1 C1 57.5(4) . . . . ? N4 Mn1 N1 C1 149.5(3) 7_556 . . . ? N4 Mn1 N1 C1 -30.5(3) . . . . ? N1 Mn1 N1 C1 174.4(1000) 7_556 . . . ? C3 N1 C1 C2 0.1(7) . . . . ? Mn1 N1 C1 C2 -179.9(5) . . . . ? N1 C1 C2 C1 0.3(10) . . . 6 ? C1 N1 C3 N1 -0.6(9) . . . 6 ? Mn1 N1 C3 N1 179.4(4) . . . 6 ? N2 Mn1 N2 N3 88.7(1000) 7_556 . . . ? N4 Mn1 N2 N3 -134.9(5) 7_556 . . . ? N4 Mn1 N2 N3 45.1(5) . . . . ? N1 Mn1 N2 N3 -44.5(5) . . . . ? N1 Mn1 N2 N3 135.5(5) 7_556 . . . ? Mn1 N2 N3 N2 -114.4(4) . . . 2_557 ? N2 Mn1 N4 N5 4.3(4) 7_556 . . . ? N2 Mn1 N4 N5 -175.7(4) . . . . ? N4 Mn1 N4 N5 93.1(1000) 7_556 . . . ? N1 Mn1 N4 N5 -83.3(4) . . . . ? N1 Mn1 N4 N5 96.7(4) 7_556 . . . ? Mn1 N4 N5 N4 -128.0(6) . . . 2_556 ? _refine_diff_density_max 0.420 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.089