# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Chun-Hua Yan' 'En-Qing Gao' 'Zhe-Ming Wang' _publ_contact_author_address ; State Key Lab of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Lab on Rare Earth Materials and Bioinorganic Chemistry, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, China ; _publ_contact_author_email chyan@chem.pku.edu.cn _publ_contact_author_fax 86-(10)-62754179 _publ_contact_author_phone 86-(10)-62754179 # SUBMISSION DETAILS _publ_contact_author_name 'Prof. Chun-Hua Yan' _publ_section_title ; >From Manganese(II)-Azido Layers to a Novel Three-Dimensional Molecular Magnet: Spin Canting and Metamagnetism ; data_Yan _database_code_CSD 205051 ## Crystallographic Data _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 Mn N10' _chemical_formula_weight 377.29 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.5610(7) _cell_length_b 8.5159(4) _cell_length_c 8.2206(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.093(2) _cell_angle_gamma 90.00 _cell_volume 849.01(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20161 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description Prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 0.890 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _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 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 13835 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 27.43 _reflns_number_total 1890 _reflns_number_gt 1383 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0564P)^2^+0.6440P] 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 0.082(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1890 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Mn1 Mn 0.5000 0.5000 0.0000 0.0341(2) Uani 1 2 d S . . N1 N 0.64413(19) 0.3291(3) 0.0772(3) 0.0394(6) Uani 1 1 d . . . N2 N 0.9626(2) 0.0556(4) 0.4545(4) 0.0584(8) Uani 1 1 d . . . N3 N 0.5571(3) 0.6064(4) 0.2503(4) 0.0686(9) Uani 1 1 d . . . N4 N 0.5814(2) 0.7215(3) 0.3259(3) 0.0464(6) Uani 1 1 d . . . N5 N 0.6070(3) 0.8309(4) 0.4122(5) 0.0682(9) Uani 1 1 d . . . C1 C 0.7390(3) 0.3749(4) 0.1848(4) 0.0502(8) Uani 1 1 d . . . H1A H 0.7513 0.4819 0.2039 0.060 Uiso 1 1 calc R . . C2 C 0.8189(2) 0.2717(4) 0.2677(5) 0.0517(8) Uani 1 1 d . . . H2A H 0.8830 0.3093 0.3418 0.062 Uiso 1 1 calc R . . C3 C 0.8039(2) 0.1117(3) 0.2410(4) 0.0403(7) Uani 1 1 d . . . C4 C 0.7078(3) 0.0646(4) 0.1262(4) 0.0439(7) Uani 1 1 d . . . H4A H 0.6949 -0.0414 0.1013 0.053 Uiso 1 1 calc R . . C5 C 0.6312(2) 0.1758(3) 0.0487(4) 0.0421(7) Uani 1 1 d . . . H5A H 0.5670 0.1415 -0.0275 0.051 Uiso 1 1 calc R . . C6 C 0.8858(2) -0.0032(4) 0.3375(4) 0.0447(7) Uani 1 1 d . . . C7 C 0.8720(3) -0.1733(4) 0.2931(6) 0.0699(11) Uani 1 1 d . . . H7A H 0.9307 -0.2322 0.3657 0.105 Uiso 1 1 calc R . . H7B H 0.8740 -0.1877 0.1781 0.105 Uiso 1 1 calc R . . H7C H 0.8025 -0.2095 0.3069 0.105 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 Mn1 0.0360(4) 0.0268(3) 0.0351(3) 0.0012(2) 0.0011(2) 0.0062(2) N1 0.0364(13) 0.0335(13) 0.0449(13) 0.0020(10) 0.0043(10) 0.0076(10) N2 0.0500(16) 0.0481(15) 0.0612(17) -0.0007(13) -0.0142(14) 0.0186(13) N3 0.081(2) 0.0598(19) 0.0514(17) -0.0190(14) -0.0071(15) 0.0201(16) N4 0.0433(14) 0.0487(16) 0.0432(14) -0.0009(12) 0.0045(11) 0.0126(12) N5 0.0535(18) 0.0531(18) 0.099(3) -0.0273(17) 0.0209(17) -0.0048(15) C1 0.0408(17) 0.0319(16) 0.069(2) 0.0001(14) -0.0023(15) 0.0037(13) C2 0.0334(15) 0.0435(18) 0.067(2) -0.0029(15) -0.0070(14) 0.0058(13) C3 0.0367(15) 0.0385(15) 0.0421(15) 0.0020(12) 0.0039(12) 0.0106(12) C4 0.0463(17) 0.0342(15) 0.0441(16) -0.0010(13) -0.0006(13) 0.0075(13) C5 0.0379(16) 0.0393(16) 0.0417(15) -0.0021(12) -0.0028(12) 0.0086(12) C6 0.0376(15) 0.0458(17) 0.0466(16) 0.0017(13) 0.0033(13) 0.0121(14) C7 0.061(2) 0.050(2) 0.082(3) -0.0011(18) -0.012(2) 0.0197(18) _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 N3 2.191(3) . ? Mn1 N3 2.191(3) 3_665 ? Mn1 N5 2.215(3) 2_645 ? Mn1 N5 2.215(3) 4_575 ? Mn1 N1 2.281(2) 3_665 ? Mn1 N1 2.281(2) . ? N1 C5 1.329(4) . ? N1 C1 1.344(4) . ? N2 C6 1.274(4) . ? N2 N2 1.405(5) 3_756 ? N3 N4 1.158(4) . ? N4 N5 1.165(4) . ? N5 Mn1 2.215(3) 2_655 ? C1 C2 1.374(4) . ? C2 C3 1.385(4) . ? C3 C4 1.384(4) . ? C3 C6 1.490(4) . ? C4 C5 1.382(4) . ? C6 C7 1.493(5) . ? 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 N3 Mn1 N3 180.0 . 3_665 ? N3 Mn1 N5 92.33(15) . 2_645 ? N3 Mn1 N5 87.67(15) 3_665 2_645 ? N3 Mn1 N5 87.67(15) . 4_575 ? N3 Mn1 N5 92.33(15) 3_665 4_575 ? N5 Mn1 N5 180.00(18) 2_645 4_575 ? N3 Mn1 N1 92.25(10) . 3_665 ? N3 Mn1 N1 87.75(10) 3_665 3_665 ? N5 Mn1 N1 90.03(10) 2_645 3_665 ? N5 Mn1 N1 89.97(10) 4_575 3_665 ? N3 Mn1 N1 87.75(10) . . ? N3 Mn1 N1 92.25(10) 3_665 . ? N5 Mn1 N1 89.97(10) 2_645 . ? N5 Mn1 N1 90.03(10) 4_575 . ? N1 Mn1 N1 180.00(9) 3_665 . ? C5 N1 C1 116.6(2) . . ? C5 N1 Mn1 121.74(19) . . ? C1 N1 Mn1 120.11(19) . . ? C6 N2 N2 114.0(4) . 3_756 ? N4 N3 Mn1 146.1(3) . . ? N3 N4 N5 175.2(4) . . ? N4 N5 Mn1 128.6(3) . 2_655 ? N1 C1 C2 123.3(3) . . ? C1 C2 C3 119.9(3) . . ? C4 C3 C2 116.9(3) . . ? C4 C3 C6 122.1(3) . . ? C2 C3 C6 121.0(3) . . ? C5 C4 C3 119.6(3) . . ? N1 C5 C4 123.6(3) . . ? N2 C6 C3 115.2(3) . . ? N2 C6 C7 125.6(3) . . ? C3 C6 C7 119.2(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.972 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.061